ANEXO A4 – CIFs das ESTRUTURAS ESTUDADAS - USP€¦ · 180 Johnson, C.K. (1965). ORTEP. Report ORNL-3794. Oak Ridge National

175

ANEXO A4 – CIFs das ESTRUTURAS ESTUDADAS

A4,1-[Cu{Pd(CN)4}(pn)]n (porPd)

#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#

data_global

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date 2009-09-03

_audit_creation_method 'WinGX routine CIF_UPDATE'

_audit_conform_dict_name cif_core.dic

_audit_conform_dict_version 2.3

_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic

_audit_update_record ?

#------------------ SUBMISSION DETAILS --------------------------------------#

# Name and address of author for correspondence

_publ_contact_author_name 'Farrugia, Louis J.'

_publ_contact_author_address

;

Department of Chemistry

University of Glasgow

Glasgow G12 8QQ

Scotland UK

;

_publ_contact_author_email [email protected]

176

_publ_contact_author_fax '44(141)3304888'

_publ_contact_author_phone '44(141)3305137'

_publ_requested_journal 'Acta Crystallographica Section C'

_publ_requested_coeditor_name ?

_publ_contact_letter # Include date of submission

;

Date of submission ?

Please consider this CIF submission for publication as a

Regular Structural Paper in Acta Crystallographica C.

;

_publ_requested_category ?

#------------------ PROCESSING SUMMARY (JOURNAL OFFICE ONLY) --------------

--#

_journal_date_recd_electronic ?

_journal_date_to_coeditor ?

_journal_date_from_coeditor ?

_journal_date_accepted ?

_journal_date_printers_first ?

_journal_date_printers_final ?

_journal_date_proofs_out ?

_journal_date_proofs_in ?

_journal_coeditor_name ?

_journal_coeditor_code ?

_journal_coeditor_notes ?

_journal_techeditor_code ?

_journal_techeditor_notes ?

_journal_coden_ASTM ?

_journal_name_full ?

_journal_year ?

177

_journal_volume ?

_journal_issue ?

_journal_page_first ?

_journal_page_last ?

_journal_suppl_publ_number ?

_journal_suppl_publ_pages ?

#------------------ TITLE AND AUTHOR LIST------------------------------------#

_publ_section_title

;

?

;

_publ_section_title_footnote

;

?

;

loop_

_publ_author_name

_publ_author_address

'Farrugia, Louis J.'

;



Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#

_publ_section_synopsis

178

;

# Insert blank lines between paragraphs

?

;

_publ_section_abstract

;


?

;

_publ_section_comment

;


?

;

_publ_section_exptl_prep

;

?

;

_publ_section_exptl_refinement

;

?

;

# Insert blank lines between references

_publ_section_references

;

Allen, F.H., Kennard, O. & Taylor, R. (1983).

Acc. Chem. Res. 16, 146-153.

179

Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A.

(1993) J. Appl. Cryst. 26, 343-350.

Altomare, A. Burla, M. C., Camalli, M., Cascarano, G. L.,

Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G.

& Spagna, R. (1999) J. Appl. Cryst. 32, 115-119.

Blessing, R. H. (1995) Acta Cryst., A51, 33-38.

Blessing, R. H. (1987) Cryst. Rev. 1, 3-58.

Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397.

Beurskens, P.T., Beurskens, G., de Gelder, R.,

Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M.

(1999) The DIRDIF-99 program system,

Technical Report of the Crystallography Laboratory,

University of Nijmegen, The Netherlands.

Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358.

Enraf-Nonius (1994). CAD4Express Software. Enraf-Nonius, Delft,

The Netherlands.

Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565.

Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838.

Flack, H.D. (1983). Acta Cryst. A39, 876-881.

Harms, K. & Wocadlo, S. (1995) XCAD-4. Program for Processing CAD-4

Diffractometer Data. University of Marburg, Germany.

180

Johnson, C.K. (1965). ORTEP. Report ORNL-3794. Oak Ridge National

Laboratory, Tennessee, USA.

Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580

LePage, Y. (1987). J. Appl. Cryst. 20, 264-269.

North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst,

A24, 351-359

Orpen, A. G., Brammer, L., Allen, F. H., Kennard, O., Watson, D. G.,

& Taylor, R. (1992). International Tables for Crystallography,

Volume C.

Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure

refinement. University of G\"ottingen, Germany.



Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3,

edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189.

Oxford University Press.

Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution.

University of G\"ottingen, Germany.

Spek, A.L. (1990). Acta Cryst. A46, C34

Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr.

34, 824-828


181

35, 281.

Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166.

Wilson, A.J.C. (1992) Ed. International Tables for Crystallography,

Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands.

;

_publ_section_figure_captions

;

Figure 1. View of (I) (50% probability displacement ellipsoids)

;

_publ_section_acknowledgements

;

?

;

_publ_section_table_legends

;

Table 1. Fractional atomic coordinates and equivalent

isotropic displacement parameters (\%A^2^)

Table 2. Selected geometric parameters (\%A ,\% )

;

#------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_cupnpdcn2

_audit_creation_date 2009-09-03T15:46:36-00:00


#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety 'C7 H8 Cu1 N6 Pd1'

182

_chemical_formula_sum 'C7 H8 Cu N6 Pd'

_chemical_formula_weight 346.13

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting orthorhombic

_symmetry_space_group_name_H-M 'P b c a'

loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

'-x+1/2, -y, z+1/2'

'x+1/2, -y+1/2, -z'

'-x, y+1/2, -z+1/2'

'-x, -y, -z'

'x-1/2, y, -z-1/2'

'-x-1/2, y-1/2, z'

'x, -y-1/2, z-1/2'

_cell_length_a 9.6731(11)

_cell_length_b 12.365(3)

_cell_length_c 19.2427(19)

_cell_angle_alpha 90

_cell_angle_beta 90

_cell_angle_gamma 90

_cell_volume 2301.5(6)

_cell_formula_units_Z 8

_cell_measurement_temperature 293(2)

_cell_measurement_reflns_used 20

_cell_measurement_theta_min 11.58

_cell_measurement_theta_max 18.5

#------------------ CRYSTAL INFORMATION -------------------------------------#

183

_exptl_crystal_description prism

_exptl_crystal_colour colorless

_exptl_crystal_size_max 0.15

_exptl_crystal_size_mid 0.13

_exptl_crystal_size_min 0.1

_exptl_crystal_density_diffrn 1.998

_exptl_crystal_density_method 'not measured'

_exptl_crystal_F_000 1336

_exptl_absorpt_coefficient_mu 3.387

_exptl_absorpt_correction_type psi-scan

_exptl_absorpt_correction_T_min 0.6593

_exptl_absorpt_correction_T_max 0.7039

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength 0.71073

_diffrn_radiation_type MoK\a

_diffrn_radiation_probe x-ray

_diffrn_measurement_device_type 'Enraf Nonius TurboCAD4'

_diffrn_measurement_device '\k-geometry diffractometer'

_diffrn_measurement_method 'non-profiled omega/2theta scans'

_diffrn_standards_number 3

_diffrn_standards_interval_time 120

_diffrn_standards_decay_% 3

loop_

_diffrn_standard_refln_index_h

_diffrn_standard_refln_index_k

_diffrn_standard_refln_index_l

5 0 -6

3 -4 7

3 4 7

_diffrn_reflns_number 3447

184

_diffrn_reflns_av_R_equivalents 0.0425

_diffrn_reflns_limit_h_min -3

_diffrn_reflns_limit_h_max 13

_diffrn_reflns_limit_k_min -17

_diffrn_reflns_limit_k_max 2

_diffrn_reflns_limit_l_min -27

_diffrn_reflns_limit_l_max 4

_diffrn_reflns_theta_min 2.12

_diffrn_reflns_theta_max 29.98

_diffrn_reflns_theta_full 29.98

_diffrn_measured_fraction_theta_max

0.984

_diffrn_measured_fraction_theta_full

0.984

_reflns_number_total 3291

_reflns_number_gt 1970

_reflns_threshold_expression >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)'

_computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)'

_computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)'

_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)'

_computing_publication_material

'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type full

185

_refine_ls_weighting_scheme calc

_refine_ls_weighting_details

'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'

_refine_ls_hydrogen_treatment mixed

_refine_ls_extinction_method SHELXL

_refine_ls_extinction_expression

Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^

_refine_ls_extinction_coef 0.00181(18)

_refine_ls_number_reflns 3291

_refine_ls_number_parameters 137

_refine_ls_number_restraints 0

_refine_ls_R_factor_gt 0.0374

_refine_ls_wR_factor_ref 0.1027

_refine_ls_goodness_of_fit_ref 1.034

_refine_ls_restrained_S_all 1.034

_refine_ls_shift/su_max 0.022

_refine_diff_density_max 1.05

_refine_diff_density_min -1.085

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL

PARAMETERS --------#

loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source

C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

186

loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_group

_atom_site_disorder_assembly

Pd Pd 0.76547(4) 0.58384(3) 0.362977(19) 0.02529(12) Uani 1 d . . .

Cu Cu 1.15907(6) 0.31797(5) 0.36481(3) 0.02612(15) Uani 1 d . . .

N3 N 0.7988(5) 0.7149(4) 0.2244(3) 0.0427(12) Uani 1 d . . .

N4 N 0.5020(5) 0.7240(4) 0.3899(2) 0.0392(11) Uani 1 d . . .

N2 N 0.7370(6) 0.4812(4) 0.5109(2) 0.0462(13) Uani 1 d . . .

N1 N 1.0201(5) 0.4331(3) 0.3378(2) 0.0362(11) Uani 1 d . . .

N5 N 1.2755(4) 0.2508(3) 0.4403(2) 0.0321(10) Uani 1 d . . .

HAN5 H 1.2763 0.2963 0.4768 0.039 Uiso 1 calc R . .

HBN5 H 1.2336 0.1895 0.4542 0.039 Uiso 1 calc R . .

N6 N 1.3122(4) 0.4221(3) 0.3432(2) 0.0347(10) Uani 1 d . . .

HAN6 H 1.291 0.4558 0.3031 0.042 Uiso 1 calc R . .

HBN6 H 1.3132 0.4728 0.3768 0.042 Uiso 1 calc R . .

C3 C 0.7848(5) 0.6635(4) 0.2727(3) 0.0311(11) Uani 1 d . . .

C4 C 0.5987(6) 0.6732(4) 0.3826(3) 0.0326(12) Uani 1 d . . .

C2 C 0.7494(5) 0.5148(4) 0.4563(3) 0.0321(11) Uani 1 d . . .

C1 C 0.9284(5) 0.4904(4) 0.3445(3) 0.0301(11) Uani 1 d . . .

C5 C 1.4203(5) 0.2244(4) 0.4226(3) 0.0419(14) Uani 1 d . . .

H5A H 1.4218 0.1745 0.3837 0.05 Uiso 1 calc R . .

H5B H 1.4639 0.1891 0.4619 0.05 Uiso 1 calc R . .

187

C6 C 1.5009(6) 0.3248(4) 0.4039(3) 0.0446(15) Uani 1 d . . .

H6A H 1.5978 0.3059 0.3995 0.054 Uiso 1 calc R . .

H6B H 1.4926 0.3765 0.4416 0.054 Uiso 1 calc R . .

C7 C 1.4534(6) 0.3787(5) 0.3366(3) 0.0461(15) Uani 1 d . . .

H7A H 1.5164 0.437 0.325 0.055 Uiso 1 calc R . .

H7B H 1.456 0.3263 0.2991 0.055 Uiso 1 calc R . .

loop_

_atom_site_aniso_label

_atom_site_aniso_U_11






Pd 0.02384(19) 0.02486(18) 0.02716(19) 0.00455(17) 0.00025(17) 0.00330(15)

Cu 0.0227(3) 0.0264(3) 0.0293(3) -0.0004(3) -0.0007(3) -0.0006(2)

N3 0.046(3) 0.043(3) 0.039(3) 0.008(2) 0.002(2) 0.002(2)

N4 0.035(3) 0.040(3) 0.042(3) 0.007(2) 0.002(2) 0.005(2)

N2 0.072(4) 0.034(3) 0.033(2) 0.005(2) 0.009(3) 0.004(2)

N1 0.037(3) 0.031(3) 0.040(3) 0.000(2) 0.004(2) 0.005(2)

N5 0.035(2) 0.026(2) 0.035(2) 0.0026(19) -0.0044(19) 0.0008(19)

N6 0.036(2) 0.033(2) 0.035(2) 0.0028(19) -0.002(2) -0.006(2)

C3 0.030(3) 0.034(3) 0.029(2) 0.006(2) 0.001(2) 0.004(2)

C4 0.030(3) 0.037(3) 0.032(3) 0.006(2) 0.001(2) 0.006(2)

C2 0.033(3) 0.029(2) 0.035(3) 0.001(2) 0.001(3) 0.003(2)

C1 0.030(3) 0.028(3) 0.032(3) 0.001(2) -0.001(2) 0.004(2)

C5 0.033(3) 0.043(3) 0.049(4) 0.001(3) -0.012(3) 0.006(3)

C6 0.024(3) 0.054(4) 0.055(4) -0.014(3) -0.003(3) -0.001(3)

C7 0.033(3) 0.051(4) 0.055(4) -0.008(3) 0.010(3) -0.011(3)

#------------------ MOLECULAR GEOMETRY --------------------------------------#

188

_geom_special_details

;

All esds (except the esd in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell esds are taken

into account individually in the estimation of esds in distances, angles

and torsion angles; correlations between esds in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell esds is used for estimating esds involving l.s. planes.

;

loop_

_geom_bond_atom_site_label_1


_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag

Pd C1 1.987(5) . ?

Pd C4 1.992(5) . ?

Pd C2 1.994(5) . ?

Pd C3 2.006(5) . ?

Cu N4 2.003(5) 7_755 ?

Cu N6 2.007(4) . ?

Cu N5 2.016(4) . ?

Cu N1 2.026(4) . ?

Cu N3 2.176(5) 4_745 ?

N3 C3 1.134(6) . ?

N3 Cu 2.176(5) 4_755 ?

N4 C4 1.135(7) . ?

N4 Cu 2.003(5) 7_765 ?

N2 C2 1.135(6) . ?

N1 C1 1.142(6) . ?

N5 C5 1.478(7) . ?

N5 HAN5 0.9 . ?

189

N5 HBN5 0.9 . ?

N6 C7 1.473(7) . ?

N6 HAN6 0.9 . ?

N6 HBN6 0.9 . ?

C5 C6 1.508(7) . ?

C5 H5A 0.97 . ?

C5 H5B 0.97 . ?

C6 C7 1.527(8) . ?

C6 H6A 0.97 . ?

C6 H6B 0.97 . ?

C7 H7A 0.97 . ?

C7 H7B 0.97 . ?

loop_

_geom_angle_atom_site_label_1



_geom_angle

_geom_angle_site_symmetry_1


_geom_angle_publ_flag

C1 Pd C4 178.1(2) . . ?

C1 Pd C2 88.5(2) . . ?

C4 Pd C2 90.2(2) . . ?

C1 Pd C3 93.2(2) . . ?

C4 Pd C3 88.1(2) . . ?

C2 Pd C3 175.8(2) . . ?

N4 Cu N6 175.34(19) 7_755 . ?

N4 Cu N5 91.25(18) 7_755 . ?

N6 Cu N5 90.07(17) . . ?

N4 Cu N1 87.33(19) 7_755 . ?

N6 Cu N1 89.16(17) . . ?

N5 Cu N1 147.66(18) . . ?

190

N4 Cu N3 89.81(18) 7_755 4_745 ?

N6 Cu N3 94.26(18) . 4_745 ?

N5 Cu N3 102.81(18) . 4_745 ?

N1 Cu N3 109.48(19) . 4_745 ?

C3 N3 Cu 175.4(5) . 4_755 ?

C4 N4 Cu 158.7(5) . 7_765 ?

C1 N1 Cu 157.2(5) . . ?

C5 N5 Cu 117.1(3) . . ?

C5 N5 HAN5 108 . . ?

Cu N5 HAN5 108 . . ?

C5 N5 HBN5 108 . . ?

Cu N5 HBN5 108 . . ?

HAN5 N5 HBN5 107.3 . . ?

C7 N6 Cu 117.9(3) . . ?

C7 N6 HAN6 107.8 . . ?

Cu N6 HAN6 107.8 . . ?

C7 N6 HBN6 107.8 . . ?

Cu N6 HBN6 107.8 . . ?

HAN6 N6 HBN6 107.2 . . ?

N3 C3 Pd 175.0(5) . . ?

N4 C4 Pd 176.2(5) . . ?

N2 C2 Pd 175.8(5) . . ?

N1 C1 Pd 175.5(5) . . ?

N5 C5 C6 111.3(4) . . ?

N5 C5 H5A 109.4 . . ?

C6 C5 H5A 109.4 . . ?

N5 C5 H5B 109.4 . . ?

C6 C5 H5B 109.4 . . ?

H5A C5 H5B 108 . . ?

C5 C6 C7 114.0(5) . . ?

C5 C6 H6A 108.8 . . ?

C7 C6 H6A 108.8 . . ?

C5 C6 H6B 108.8 . . ?

191

C7 C6 H6B 108.8 . . ?

H6A C6 H6B 107.7 . . ?

N6 C7 C6 111.4(5) . . ?

N6 C7 H7A 109.3 . . ?

C6 C7 H7A 109.4 . . ?

N6 C7 H7B 109.4 . . ?

C6 C7 H7B 109.4 . . ?

H7A C7 H7B 108 . . ?

loop_

_geom_torsion_atom_site_label_1




_geom_torsion

_geom_torsion_site_symmetry_1




_geom_torsion_publ_flag

N4 Cu N1 C1 53.7(11) 7_755 . . . ?

N6 Cu N1 C1 -123.2(11) . . . . ?

N5 Cu N1 C1 -34.4(13) . . . . ?

N3 Cu N1 C1 142.6(11) 4_745 . . . ?

N4 Cu N5 C5 137.4(4) 7_755 . . . ?

N6 Cu N5 C5 -47.1(4) . . . . ?

N1 Cu N5 C5 -135.6(4) . . . . ?

N3 Cu N5 C5 47.3(4) 4_745 . . . ?

N4 Cu N6 C7 153(2) 7_755 . . . ?

N5 Cu N6 C7 46.6(4) . . . . ?

N1 Cu N6 C7 -165.7(4) . . . . ?

N3 Cu N6 C7 -56.2(4) 4_745 . . . ?

Cu N3 C3 Pd 44(10) 4_755 . . . ?

192

C1 Pd C3 N3 -109(6) . . . . ?

C4 Pd C3 N3 72(6) . . . . ?

C2 Pd C3 N3 5(8) . . . . ?

Cu N4 C4 Pd -15(9) 7_765 . . . ?

C1 Pd C4 N4 -101(9) . . . . ?

C2 Pd C4 N4 -149(8) . . . . ?

C3 Pd C4 N4 35(8) . . . . ?

C1 Pd C2 N2 149(7) . . . . ?

C4 Pd C2 N2 -33(7) . . . . ?

C3 Pd C2 N2 34(9) . . . . ?

Cu N1 C1 Pd -10(7) . . . . ?

C4 Pd C1 N1 -40(11) . . . . ?

C2 Pd C1 N1 8(6) . . . . ?

C3 Pd C1 N1 -176(6) . . . . ?

Cu N5 C5 C6 62.2(5) . . . . ?

N5 C5 C6 C7 -66.9(6) . . . . ?

Cu N6 C7 C6 -60.5(6) . . . . ?

C5 C6 C7 N6 65.9(6) . . . . ?

A4,2-Pd C16 H22 N2 Cl2 (cyPd1)

data_umc8

_audit_creation_method SHELXL-97

_chemical_name_systematic

;

?

;

_chemical_name_common ?

_chemical_melting_point ?

_chemical_formula_moiety ?

_chemical_formula_sum

193

'C16 H22 Cl2 N2 Pd'


loop_

_atom_type_symbol





'C' 'C' 0.0033 0.0016

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

'H' 'H' 0.0000 0.0000


'N' 'N' 0.0061 0.0033


'Cl' 'Cl' 0.1484 0.1585


'Pd' 'Pd' -0.9988 1.0072


_symmetry_cell_setting ?

_symmetry_space_group_name_H-M ?

loop_


'x, y, z'

'-x, y+1/2, -z+1/2'

'-x, -y, -z'

'x, -y-1/2, z-1/2'




194

_cell_angle_alpha 90.00

_cell_angle_beta 103.049(18)

_cell_angle_gamma 90.00




_cell_measurement_reflns_used ?

_cell_measurement_theta_min ?

_cell_measurement_theta_max ?

_exptl_crystal_description ?

_exptl_crystal_colour ?

_exptl_crystal_size_max ?

_exptl_crystal_size_mid ?

_exptl_crystal_size_min ?

_exptl_crystal_density_meas ?





_exptl_absorpt_correction_type ?

_exptl_absorpt_correction_T_min ?

_exptl_absorpt_correction_T_max ?

_exptl_absorpt_process_details ?

_exptl_special_details

;

?

;

_diffrn_ambient_temperature 293(2)



195

_diffrn_radiation_source 'fine-focus sealed tube'

_diffrn_radiation_monochromator graphite

_diffrn_measurement_device_type ?

_diffrn_measurement_method ?

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time ?

_diffrn_standards_decay_% ?



_diffrn_reflns_av_sigmaI/netI 0.1522












_computing_data_collection ?

_computing_cell_refinement ?

_computing_data_reduction ?

_computing_structure_solution ?


_computing_molecular_graphics ?

_computing_publication_material ?

_refine_special_details

196

;

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F^2^, conventional R-factors R are based

on F, with F set to zero for negative F^2^. The threshold expression of

F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F^2^ are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

;






_atom_sites_solution_primary direct

_atom_sites_solution_secondary difmap

_atom_sites_solution_hydrogens geom


_refine_ls_extinction_method none

_refine_ls_extinction_coef ?




_refine_ls_R_factor_all 0.2748



_refine_ls_wR_factor_gt 0.2069




_refine_ls_shift/su_mean 0.000

197

loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type


_atom_site_symmetry_multiplicity





Pd Pd 0.2294(2) 0.18968(4) 0.02495(13) 0.0359(3) Uani 1 1 d . . .

Cl1 Cl 0.4916(8) 0.25262(15) 0.0427(5) 0.0524(11) Uani 1 1 d . . .

Cl2 Cl -0.3920(9) 0.10780(18) -0.1490(5) 0.0653(14) Uani 1 1 d . . .

N1 N 0.495(2) 0.1516(5) 0.2845(14) 0.044(3) Uani 1 1 d . . .

N2 N 0.030(2) 0.2140(5) -0.1489(14) 0.044(3) Uani 1 1 d . . .

C1 C 0.398(3) 0.1648(5) 0.1873(14) 0.039(4) Uani 1 1 d . . .

C2 C 0.628(3) 0.1350(7) 0.406(2) 0.060(5) Uani 1 1 d . . .

H2A H 0.6550 0.1607 0.4669 0.071 Uiso 1 1 calc R . .

H2B H 0.7714 0.1243 0.3929 0.071 Uiso 1 1 calc R . .

C3 C 0.516(3) 0.0953(7) 0.4608(18) 0.060(5) Uani 1 1 d . . .

H3A H 0.5048 0.0688 0.4024 0.072 Uiso 1 1 calc R . .

H3B H 0.6128 0.0860 0.5421 0.072 Uiso 1 1 calc R . .

C4 C 0.295(4) 0.1039(10) 0.484(3) 0.105(11) Uani 1 1 d . . .

H4A H 0.1912 0.1098 0.4019 0.126 Uiso 1 1 calc R . .

H4B H 0.2999 0.1317 0.5371 0.126 Uiso 1 1 calc R . .

C5 C 0.215(5) 0.0635(11) 0.549(2) 0.121(12) Uani 1 1 d . . .

H5A H 0.2575 0.0348 0.5132 0.181 Uiso 1 1 calc R . .

H5B H 0.0557 0.0649 0.5349 0.181 Uiso 1 1 calc R . .

H5C H 0.2810 0.0647 0.6395 0.181 Uiso 1 1 calc R . .

198

C6 C -0.194(3) 0.1919(6) -0.1641(15) 0.045(4) Uani 1 1 d . . .

H6A H -0.2914 0.2121 -0.1278 0.055 Uiso 1 1 calc R . .

H6B H -0.2615 0.1871 -0.2550 0.055 Uiso 1 1 calc R . .

C7 C -0.163(3) 0.1463(6) -0.0951(17) 0.043(4) Uani 1 1 d . . .

C8 C 0.014(3) 0.1359(5) 0.0002(14) 0.036(3) Uani 1 1 d . . .

C9 C 0.040(3) 0.0917(5) 0.0722(14) 0.037(3) Uani 1 1 d . . .

C10 C 0.220(3) 0.0620(6) 0.0679(17) 0.049(4) Uani 1 1 d . . .

H10 H 0.3263 0.0712 0.0229 0.059 Uiso 1 1 calc R . .

C11 C 0.240(4) 0.0196(6) 0.129(2) 0.062(5) Uani 1 1 d . . .

H11 H 0.3575 -0.0003 0.1235 0.074 Uiso 1 1 calc R . .

C12 C 0.092(4) 0.0062(6) 0.199(2) 0.065(6) Uani 1 1 d . . .

H12 H 0.1096 -0.0223 0.2427 0.079 Uiso 1 1 calc R . .

C13 C -0.085(4) 0.0347(7) 0.205(2) 0.063(5) Uani 1 1 d . . .

H13 H -0.1897 0.0252 0.2512 0.075 Uiso 1 1 calc R . .

C14 C -0.107(3) 0.0774(7) 0.144(2) 0.058(5) Uani 1 1 d . . .

H14 H -0.2246 0.0970 0.1507 0.070 Uiso 1 1 calc R . .

C15 C 0.000(4) 0.2668(6) -0.155(3) 0.090(9) Uani 1 1 d . . .

H15A H 0.1436 0.2817 -0.1305 0.135 Uiso 1 1 calc R . .

H15B H -0.0909 0.2762 -0.0971 0.135 Uiso 1 1 calc R . .

H15C H -0.0709 0.2758 -0.2417 0.135 Uiso 1 1 calc R . .

C16 C 0.130(3) 0.1983(8) -0.2562(19) 0.070(6) Uani 1 1 d . . .

H16A H 0.1452 0.1647 -0.2537 0.105 Uiso 1 1 calc R . .

H16B H 0.2749 0.2124 -0.2473 0.105 Uiso 1 1 calc R . .

H16C H 0.0357 0.2075 -0.3371 0.105 Uiso 1 1 calc R . .

loop_








199

Pd 0.0434(6) 0.0299(5) 0.0361(6) 0.0008(6) 0.0126(4) 0.0007(6)

Cl1 0.056(3) 0.045(2) 0.057(3) -0.004(2) 0.015(2) -0.010(2)

Cl2 0.056(3) 0.059(3) 0.073(3) 0.012(2) -0.001(3) -0.015(2)

N1 0.052(9) 0.038(7) 0.042(8) 0.008(6) 0.008(7) -0.002(6)

N2 0.043(8) 0.044(7) 0.049(9) 0.008(6) 0.016(7) -0.012(6)

C1 0.055(10) 0.038(8) 0.025(8) 0.002(6) 0.010(7) -0.005(7)

C2 0.049(11) 0.058(11) 0.069(14) 0.015(10) 0.006(10) 0.009(9)

C3 0.074(14) 0.057(11) 0.043(11) 0.017(9) -0.003(10) -0.002(10)

C4 0.052(14) 0.14(2) 0.12(2) 0.08(2) 0.009(14) -0.013(15)

C5 0.13(3) 0.16(3) 0.066(19) 0.015(18) -0.008(17) -0.06(2)

C6 0.059(10) 0.044(8) 0.036(8) -0.007(8) 0.015(7) 0.005(9)

C7 0.038(9) 0.043(8) 0.049(10) -0.007(7) 0.011(8) -0.009(7)

C8 0.059(10) 0.031(7) 0.022(7) 0.002(5) 0.015(7) -0.004(7)

C9 0.048(10) 0.037(7) 0.022(7) 0.000(6) -0.003(6) -0.013(7)

C10 0.061(12) 0.041(9) 0.049(10) 0.005(8) 0.020(9) 0.005(8)

C11 0.070(14) 0.033(9) 0.075(15) 0.001(9) 0.003(11) 0.006(9)

C12 0.092(17) 0.037(9) 0.059(13) 0.007(9) -0.001(12) -0.018(10)

C13 0.071(14) 0.057(12) 0.065(14) 0.011(10) 0.026(11) -0.017(11)

C14 0.054(12) 0.055(11) 0.067(13) -0.001(10) 0.016(10) -0.007(9)

C15 0.077(16) 0.033(9) 0.17(3) 0.027(13) 0.040(17) -0.011(10)

C16 0.057(12) 0.107(18) 0.055(12) 0.015(12) 0.032(10) 0.017(12)


;







;

loop_

200



_geom_bond_distance



Pd C1 1.934(16) . ?

Pd C8 2.000(15) . ?

Pd N2 2.089(14) . ?

Pd Cl1 2.390(4) . ?

Cl2 C7 1.774(16) . ?

N1 C1 1.135(19) . ?

N1 C2 1.44(2) . ?

N2 C16 1.48(2) . ?

N2 C6 1.49(2) . ?

N2 C15 1.51(2) . ?

C2 C3 1.51(2) . ?

C3 C4 1.45(3) . ?

C4 C5 1.48(3) . ?

C6 C7 1.48(2) . ?

C7 C8 1.34(2) . ?

C8 C9 1.464(19) . ?

C9 C14 1.37(2) . ?

C9 C10 1.40(2) . ?

C10 C11 1.37(2) . ?

C11 C12 1.35(3) . ?

C12 C13 1.37(3) . ?

C13 C14 1.37(3) . ?

loop_




_geom_angle

201




C1 Pd C8 92.4(6) . . ?

C1 Pd N2 176.4(6) . . ?

C8 Pd N2 84.3(6) . . ?

C1 Pd Cl1 89.4(5) . . ?

C8 Pd Cl1 176.6(4) . . ?

N2 Pd Cl1 94.0(4) . . ?

C1 N1 C2 177.4(18) . . ?

C16 N2 C6 108.8(14) . . ?

C16 N2 C15 109.6(16) . . ?

C6 N2 C15 108.2(14) . . ?

C16 N2 Pd 108.5(11) . . ?

C6 N2 Pd 107.4(9) . . ?

C15 N2 Pd 114.2(14) . . ?

N1 C1 Pd 177.7(15) . . ?

N1 C2 C3 112.1(16) . . ?

C4 C3 C2 117.7(18) . . ?

C3 C4 C5 112(2) . . ?

C7 C6 N2 107.6(14) . . ?

C8 C7 C6 123.9(14) . . ?

C8 C7 Cl2 123.9(13) . . ?

C6 C7 Cl2 112.2(12) . . ?

C7 C8 C9 123.8(14) . . ?

C7 C8 Pd 109.3(11) . . ?

C9 C8 Pd 126.9(12) . . ?

C14 C9 C10 117.6(16) . . ?

C14 C9 C8 122.7(16) . . ?

C10 C9 C8 119.7(15) . . ?

C11 C10 C9 120.4(18) . . ?

C12 C11 C10 120.7(19) . . ?

C11 C12 C13 120.1(18) . . ?

202

C12 C13 C14 119.6(19) . . ?

C9 C14 C13 121.6(19) . . ?

_diffrn_measured_fraction_theta_max 0.998


_diffrn_measured_fraction_theta_full 0.998



_refine_diff_density_rms 0.322

A4,3- C26H44N10P2Pd2 (cyPd2) #\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE

# Created on 2010-03-02 at 09:57:01

# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic

# Dictionary vers : 2.3

# Request file : c:\wingx\files\cifdoc.dat

# CIF files read : ad2 struct


data_global

#------------------ AUDIT DETAILS -------------------------------------------#





203







;



Glasgow G12 8QQ

Scotland UK

;







;




;



--#

204
















_journal_year ?

_journal_volume ?

_journal_issue ?






_publ_section_title

;

?

;


;

?

205

;

loop_

_publ_author_name



;



Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#


;


?

;


;


?

;


;


?

;


206

;

?

;


;

?

;



;


Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.











207




The Netherlands.











A24, 351-359



Volume C.



208










34, 824-828


35, 281.




;


;


;


;

?

;


;

209




;


data_ad2




_chemical_formula_moiety 'C46 H44 N10 P2 Pd2'

_chemical_formula_sum 'C46 H44 N10 P2 Pd2'



_symmetry_cell_setting triclinic

_symmetry_space_group_name_H-M 'P -1'

loop_


'x, y, z'

'-x, -y, -z'




_cell_angle_alpha 70.74(2)


210

_cell_angle_gamma 70.06(2)





_cell_measurement_theta_min 0

_cell_measurement_theta_max 0



_exptl_crystal_colour yellow








_exptl_absorpt_correction_type none












211






0.999


0.999



















Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^



212












loop_

_atom_type_symbol








P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type

213






Pd1 Pd 0.13622(4) 0.81074(4) 0.24752(3) 0.03853(15) Uani 1 d . . .

Pd2 Pd 0.38256(4) 0.76472(4) 0.15421(3) 0.03903(16) Uani 1 d . . .

N1 N 0.5024(6) 0.8427(6) 0.1702(5) 0.075(2) Uani 1 d . . .

N2 N 0.4744(6) 0.9339(7) 0.1764(5) 0.081(2) Uani 1 d . . .

N3 N 0.4577(10) 1.0257(10) 0.1827(10) 0.185(6) Uani 1 d . . .

N1A N 0.1550(8) 0.6679(6) 0.3494(4) 0.077(2) Uani 1 d . . .

N2A N 0.1497(6) 0.5810(6) 0.3543(4) 0.0673(18) Uani 1 d . . .

N3A N 0.1495(12) 0.4834(8) 0.3662(5) 0.143(4) Uani 1 d . . .

P1 P 0.10371(16) 0.91391(14) 0.33404(10) 0.0422(4) Uani 1 d . . .

P2 P 0.54904(15) 0.58742(14) 0.19852(10) 0.0412(4) Uani 1 d . . .

C1A C 0.2372(6) 0.8577(5) 0.4053(4) 0.0450(15) Uani 1 d . . .

C2A C 0.2334(7) 0.8881(6) 0.4733(4) 0.061(2) Uani 1 d . . .

H2A H 0.1596 0.9359 0.4851 0.08 Uiso 1 calc R . .

C3A C 0.3399(9) 0.8476(8) 0.5244(5) 0.077(2) Uani 1 d . . .

H3A H 0.3364 0.8667 0.571 0.1 Uiso 1 calc R . .

C4A C 0.4506(8) 0.7794(8) 0.5068(6) 0.081(3) Uani 1 d . . .

H4A H 0.522 0.754 0.5405 0.105 Uiso 1 calc R . .

C5A C 0.4544(8) 0.7499(8) 0.4400(6) 0.079(2) Uani 1 d . . .

H5A H 0.5286 0.7026 0.4282 0.103 Uiso 1 calc R . .

C6A C 0.3499(7) 0.7889(7) 0.3892(5) 0.065(2) Uani 1 d . . .

H6A H 0.3548 0.7688 0.3429 0.085 Uiso 1 calc R . .

C7A C -0.0268(7) 0.8918(6) 0.3863(4) 0.0531(18) Uani 1 d . . .

C8A C -0.0127(7) 0.8069(7) 0.4617(5) 0.068(2) Uani 1 d . . .

H8A H 0.0642 0.7672 0.491 0.089 Uiso 1 calc R . .

C9A C -0.1131(10) 0.7812(9) 0.4936(6) 0.087(3) Uani 1 d . . .

H9A H -0.1041 0.7251 0.5449 0.113 Uiso 1 calc R . .

C10A C -0.2258(10) 0.8376(10) 0.4502(7) 0.091(3) Uani 1 d . . .

H10A H -0.2929 0.8186 0.4717 0.119 Uiso 1 calc R . .

214

C11A C -0.2401(9) 0.9215(10) 0.3757(7) 0.092(3) Uani 1 d . . .

H11A H -0.3169 0.9598 0.3462 0.119 Uiso 1 calc R . .

C12A C -0.1422(8) 0.9490(8) 0.3445(5) 0.074(2) Uani 1 d . . .

H12A H -0.153 1.0077 0.294 0.096 Uiso 1 calc R . .

C13A C 0.0751(6) 1.0762(5) 0.2989(4) 0.0453(16) Uani 1 d . . .

C14A C 0.1555(7) 1.1164(6) 0.2474(4) 0.0551(18) Uani 1 d . . .

H14A H 0.2132 1.064 0.2266 0.072 Uiso 1 calc R . .

C15A C 0.1480(8) 1.2350(7) 0.2277(5) 0.070(2) Uani 1 d . . .

H15A H 0.201 1.2627 0.1931 0.09 Uiso 1 calc R . .

C16A C 0.0638(9) 1.3127(7) 0.2583(6) 0.077(3) Uani 1 d . . .

H16A H 0.0597 1.3924 0.2446 0.101 Uiso 1 calc R . .

C17A C -0.0136(8) 1.2731(6) 0.3087(5) 0.075(3) Uani 1 d . . .

H17A H -0.0697 1.3256 0.3302 0.097 Uiso 1 calc R . .

C18A C -0.0100(7) 1.1560(6) 0.3284(4) 0.0583(19) Uani 1 d . . .

H18A H -0.0653 1.1306 0.3618 0.076 Uiso 1 calc R . .

C1B C 0.5161(6) 0.4491(5) 0.2189(4) 0.0495(17) Uani 1 d . . .

C2B C 0.4179(6) 0.4376(6) 0.2622(4) 0.0538(18) Uani 1 d . . .

H2B H 0.3701 0.5007 0.2786 0.07 Uiso 1 calc R . .

C3B C 0.3899(7) 0.3340(7) 0.2811(5) 0.068(2) Uani 1 d . . .

H3B H 0.3246 0.3267 0.311 0.089 Uiso 1 calc R . .

C4B C 0.4589(9) 0.2417(7) 0.2558(6) 0.079(3) Uani 1 d . . .

H4B H 0.4404 0.1715 0.2685 0.103 Uiso 1 calc R . .

C5B C 0.5537(9) 0.2522(7) 0.2122(6) 0.085(3) Uani 1 d . . .

H5B H 0.5987 0.1899 0.1942 0.11 Uiso 1 calc R . .

C6B C 0.5848(7) 0.3553(6) 0.1941(5) 0.065(2) Uani 1 d . . .

H6B H 0.6516 0.3608 0.1654 0.085 Uiso 1 calc R . .

C7B C 0.6399(6) 0.5619(5) 0.2885(4) 0.0447(15) Uani 1 d . . .

C8B C 0.6356(7) 0.4783(7) 0.3621(5) 0.065(2) Uani 1 d . . .

H8B H 0.5855 0.433 0.3658 0.084 Uiso 1 calc R . .

C9B C 0.7059(8) 0.4618(7) 0.4304(5) 0.072(2) Uani 1 d . . .

H9B H 0.7004 0.4069 0.4794 0.093 Uiso 1 calc R . .

C10B C 0.7815(7) 0.5239(8) 0.4267(5) 0.072(2) Uani 1 d . . .

H10B H 0.8299 0.5096 0.4725 0.094 Uiso 1 calc R . .

215

C11B C 0.7872(7) 0.6089(7) 0.3547(5) 0.067(2) Uani 1 d . . .

H11B H 0.8377 0.6535 0.352 0.087 Uiso 1 calc R . .

C12B C 0.7160(6) 0.6268(6) 0.2862(4) 0.0549(18) Uani 1 d . . .

H12B H 0.7199 0.6837 0.2377 0.071 Uiso 1 calc R . .

C13B C 0.6571(5) 0.5917(6) 0.1234(4) 0.0407(15) Uani 1 d . . .

C14B C 0.6234(6) 0.6833(6) 0.0500(4) 0.0529(18) Uani 1 d . . .

H14B H 0.5445 0.7411 0.039 0.069 Uiso 1 calc R . .

C15B C 0.7041(8) 0.6907(7) -0.0070(5) 0.068(2) Uani 1 d . . .

H15B H 0.6799 0.7537 -0.056 0.088 Uiso 1 calc R . .

C16B C 0.8198(8) 0.6064(8) 0.0076(5) 0.070(2) Uani 1 d . . .

H16B H 0.8746 0.6119 -0.0312 0.091 Uiso 1 calc R . .

C17B C 0.8545(7) 0.5136(8) 0.0799(5) 0.065(2) Uani 1 d . . .

H17B H 0.9326 0.4546 0.0896 0.084 Uiso 1 calc R . .

C18B C 0.7752(6) 0.5069(7) 0.1380(4) 0.0555(18) Uani 1 d . . .

H18B H 0.8007 0.4451 0.1875 0.072 Uiso 1 calc R . .

N1P N 0.2633(4) 0.6888(4) 0.1354(3) 0.0356(11) Uani 1 d . . .

N2P N 0.1623(4) 0.7069(4) 0.1761(3) 0.0354(11) Uani 1 d . . .

N3P N 0.2404(5) 0.9273(4) 0.1101(3) 0.0451(13) Uani 1 d . . .

N4P N 0.1330(5) 0.9460(4) 0.1464(3) 0.0420(12) Uani 1 d . . .

C1P C 0.0880(5) 0.6613(5) 0.1520(4) 0.0383(14) Uani 1 d . . .

C2P C 0.1414(6) 0.6111(6) 0.0966(4) 0.0503(17) Uani 1 d . . .

H5P H 0.1104 0.5709 0.0713 0.065 Uiso 1 calc R . .

C3P C 0.2503(6) 0.6319(5) 0.0858(4) 0.0410(14) Uani 1 d . . .

C4P C 0.3453(6) 0.6025(7) 0.0293(4) 0.063(2) Uani 1 d . . .

H41 H 0.3937 0.6532 0.0218 0.081 Uiso 1 calc R . .

H42 H 0.3049 0.6165 -0.0215 0.081 Uiso 1 calc R . .

H43 H 0.3978 0.5191 0.0517 0.081 Uiso 1 calc R . .

C5P C -0.0339(6) 0.6727(6) 0.1842(4) 0.0523(17) Uani 1 d . . .

H51 H -0.0233 0.6085 0.2345 0.068 Uiso 1 calc R . .

H52 H -0.0883 0.6675 0.1467 0.068 Uiso 1 calc R . .

H53 H -0.0684 0.7493 0.1919 0.068 Uiso 1 calc R . .

C6P C 0.0472(6) 1.0459(6) 0.0979(4) 0.0531(18) Uani 1 d . . .

C7P C 0.0984(7) 1.0935(7) 0.0304(4) 0.066(2) Uani 1 d . . .

216

H7P H 0.0593 1.1637 -0.0128 0.085 Uiso 1 calc R . .

C8P C 0.2178(6) 1.0177(6) 0.0388(4) 0.0504(17) Uani 1 d . . .

C9P C 0.3167(7) 1.0198(7) -0.0165(5) 0.073(2) Uani 1 d . . .

H91 H 0.3803 1.0359 0.0063 0.096 Uiso 1 calc R . .

H92 H 0.2826 1.0819 -0.0675 0.096 Uiso 1 calc R . .

H93 H 0.3505 0.9427 -0.0238 0.096 Uiso 1 calc R . .

C10P C -0.0820(7) 1.0905(7) 0.1191(5) 0.075(2) Uani 1 d . . .

H101 H -0.1029 1.0229 0.1519 0.097 Uiso 1 calc R . .

H102 H -0.1376 1.1325 0.0709 0.097 Uiso 1 calc R . .

H103 H -0.0883 1.1445 0.1481 0.097 Uiso 1 calc R . .

loop_








Pd1 0.0496(3) 0.0336(3) 0.0363(3) -0.0163(2) 0.0119(2) -0.0158(2)

Pd2 0.0392(3) 0.0398(3) 0.0436(3) -0.0176(2) 0.0092(2) -0.0177(2)

N1 0.056(4) 0.047(4) 0.130(6) -0.035(4) -0.011(4) -0.020(3)

N2 0.076(5) 0.074(5) 0.119(6) -0.056(5) 0.015(4) -0.036(4)

N3 0.130(9) 0.159(10) 0.373(19) -0.198(12) 0.073(10) -0.081(8)

N1A 0.160(7) 0.044(4) 0.042(4) -0.018(3) 0.027(4) -0.051(4)

N2A 0.100(5) 0.062(4) 0.041(4) -0.012(3) 0.021(3) -0.036(4)

N3A 0.281(14) 0.082(6) 0.080(6) -0.014(5) 0.021(7) -0.096(8)

P1 0.0545(10) 0.0365(9) 0.0397(9) -0.0189(7) 0.0148(8) -0.0159(8)

P2 0.0408(9) 0.0384(9) 0.0492(10) -0.0196(8) 0.0127(8) -0.0159(7)

C1A 0.055(4) 0.040(4) 0.040(4) -0.014(3) 0.007(3) -0.016(3)

C2A 0.069(5) 0.061(5) 0.056(5) -0.029(4) 0.003(4) -0.015(4)

C3A 0.102(7) 0.089(6) 0.056(5) -0.027(5) 0.009(5) -0.051(6)

C4A 0.071(6) 0.094(7) 0.078(7) -0.023(5) 0.000(5) -0.036(5)

217

C5A 0.054(5) 0.086(6) 0.092(7) -0.030(6) 0.012(5) -0.018(5)

C6A 0.064(5) 0.071(5) 0.066(5) -0.036(4) 0.015(4) -0.021(4)

C7A 0.064(5) 0.056(4) 0.055(4) -0.033(4) 0.028(4) -0.026(4)

C8A 0.066(5) 0.086(6) 0.066(5) -0.030(5) 0.023(4) -0.039(5)

C9A 0.109(8) 0.110(8) 0.065(6) -0.027(5) 0.027(6) -0.072(7)

C10A 0.088(7) 0.122(8) 0.105(8) -0.060(7) 0.045(6) -0.067(7)

C11A 0.071(6) 0.118(8) 0.095(8) -0.041(7) 0.017(6) -0.041(6)

C12A 0.065(5) 0.093(6) 0.068(6) -0.028(5) 0.013(5) -0.032(5)

C13A 0.059(4) 0.039(3) 0.040(4) -0.018(3) 0.000(3) -0.016(3)

C14A 0.067(5) 0.054(4) 0.054(4) -0.021(4) 0.006(4) -0.031(4)

C15A 0.082(6) 0.061(5) 0.068(6) -0.011(4) -0.015(4) -0.037(5)

C16A 0.102(7) 0.037(4) 0.081(6) -0.012(4) -0.030(5) -0.017(5)

C17A 0.097(7) 0.035(4) 0.075(6) -0.030(4) -0.011(5) 0.010(4)

C18A 0.070(5) 0.045(4) 0.054(4) -0.023(3) 0.006(4) -0.007(4)

C1B 0.057(4) 0.034(3) 0.057(4) -0.010(3) 0.000(3) -0.020(3)

C2B 0.048(4) 0.051(4) 0.062(5) -0.013(4) 0.001(3) -0.023(3)

C3B 0.066(5) 0.063(5) 0.078(6) -0.010(4) 0.002(4) -0.038(4)

C4B 0.085(6) 0.053(5) 0.102(7) -0.014(5) -0.011(6) -0.038(5)

C5B 0.104(7) 0.045(5) 0.115(8) -0.040(5) 0.004(6) -0.026(5)

C6B 0.074(5) 0.050(4) 0.075(5) -0.028(4) 0.010(4) -0.020(4)

C7B 0.039(4) 0.040(3) 0.058(4) -0.025(3) 0.016(3) -0.012(3)

C8B 0.080(6) 0.061(5) 0.055(5) -0.011(4) 0.002(4) -0.035(4)

C9B 0.093(6) 0.061(5) 0.054(5) -0.004(4) 0.003(5) -0.033(5)

C10B 0.064(5) 0.096(6) 0.060(5) -0.039(5) 0.005(4) -0.021(5)

C11B 0.062(5) 0.084(6) 0.074(6) -0.039(5) 0.014(4) -0.037(4)

C12B 0.054(4) 0.070(5) 0.054(4) -0.026(4) 0.018(4) -0.034(4)

C13B 0.037(4) 0.047(4) 0.048(4) -0.028(3) 0.013(3) -0.017(3)

C14B 0.047(4) 0.047(4) 0.056(4) -0.016(4) 0.022(3) -0.008(3)

C15B 0.082(6) 0.057(5) 0.063(5) -0.017(4) 0.030(4) -0.028(4)

C16B 0.073(6) 0.099(7) 0.073(6) -0.055(5) 0.043(5) -0.050(5)

C17B 0.044(4) 0.106(7) 0.070(5) -0.058(5) 0.025(4) -0.033(4)

C18B 0.042(4) 0.071(5) 0.057(5) -0.034(4) 0.002(3) -0.011(4)

N1P 0.032(3) 0.039(3) 0.039(3) -0.019(2) 0.008(2) -0.012(2)

218

N2P 0.040(3) 0.041(3) 0.037(3) -0.022(2) 0.013(2) -0.021(2)

N3P 0.052(3) 0.046(3) 0.044(3) -0.017(3) 0.020(3) -0.024(3)

N4P 0.048(3) 0.037(3) 0.042(3) -0.015(2) 0.008(3) -0.015(2)

C1P 0.036(3) 0.042(3) 0.042(4) -0.016(3) 0.006(3) -0.017(3)

C2P 0.050(4) 0.054(4) 0.061(5) -0.037(4) 0.002(3) -0.018(3)

C3P 0.042(4) 0.048(4) 0.040(4) -0.025(3) 0.006(3) -0.014(3)

C4P 0.051(4) 0.084(5) 0.066(5) -0.050(4) 0.010(4) -0.016(4)

C5P 0.045(4) 0.057(4) 0.065(5) -0.029(4) 0.013(3) -0.023(3)

C6P 0.044(4) 0.047(4) 0.055(5) -0.012(3) 0.002(3) -0.005(3)

C7P 0.068(5) 0.050(4) 0.053(5) 0.003(4) 0.003(4) -0.010(4)

C8P 0.058(5) 0.039(4) 0.049(4) -0.007(3) 0.014(3) -0.019(3)

C9P 0.074(5) 0.060(5) 0.063(5) 0.005(4) 0.020(4) -0.021(4)

C10P 0.052(5) 0.075(5) 0.062(5) -0.001(4) 0.007(4) -0.001(4)



;







;

loop_



_geom_bond_distance



Pd1 N4P 2.011(5) . ?

219

Pd1 N1A 2.033(6) . ?

Pd1 N2P 2.046(4) . ?

Pd1 P1 2.2619(17) . ?

Pd1 Pd2 3.2550(8) . ?

Pd2 N1P 2.018(5) . ?

Pd2 N1 2.026(6) . ?

Pd2 N3P 2.049(5) . ?

Pd2 P2 2.2974(18) . ?

N1 N2 1.117(8) . ?

N2 N3 1.141(10) . ?

N1A N2A 1.085(8) . ?

N2A N3A 1.170(9) . ?

P1 C1A 1.805(7) . ?

P1 C7A 1.816(7) . ?

P1 C13A 1.826(6) . ?

P2 C7B 1.810(7) . ?

P2 C13B 1.814(6) . ?

P2 C1B 1.819(6) . ?

C1A C2A 1.377(9) . ?

C1A C6A 1.386(9) . ?

C2A C3A 1.389(11) . ?

C2A H2A 0.93 . ?

C3A C4A 1.377(12) . ?

C3A H3A 0.93 . ?

C4A C5A 1.349(12) . ?

C4A H4A 0.93 . ?

C5A C6A 1.372(11) . ?

C5A H5A 0.93 . ?

C6A H6A 0.93 . ?

C7A C12A 1.379(10) . ?

C7A C8A 1.379(10) . ?

C8A C9A 1.378(11) . ?

C8A H8A 0.93 . ?

220

C9A C10A 1.365(12) . ?

C9A H9A 0.93 . ?

C10A C11A 1.362(13) . ?

C10A H10A 0.93 . ?

C11A C12A 1.357(12) . ?

C11A H11A 0.93 . ?

C12A H12A 0.93 . ?

C13A C18A 1.380(9) . ?

C13A C14A 1.395(9) . ?

C14A C15A 1.381(9) . ?

C14A H14A 0.93 . ?

C15A C16A 1.371(12) . ?

C15A H15A 0.93 . ?

C16A C17A 1.354(12) . ?

C16A H16A 0.93 . ?

C17A C18A 1.376(10) . ?

C17A H17A 0.93 . ?

C18A H18A 0.93 . ?

C1B C6B 1.377(9) . ?

C1B C2B 1.386(9) . ?

C2B C3B 1.376(9) . ?

C2B H2B 0.93 . ?

C3B C4B 1.370(11) . ?

C3B H3B 0.93 . ?

C4B C5B 1.352(12) . ?

C4B H4B 0.93 . ?

C5B C6B 1.392(10) . ?

C5B H5B 0.93 . ?

C6B H6B 0.93 . ?

C7B C12B 1.382(9) . ?

C7B C8B 1.391(9) . ?

C8B C9B 1.393(10) . ?

C8B H8B 0.93 . ?

221

C9B C10B 1.347(11) . ?

C9B H9B 0.93 . ?

C10B C11B 1.383(11) . ?

C10B H10B 0.93 . ?

C11B C12B 1.398(10) . ?

C11B H11B 0.93 . ?

C12B H12B 0.93 . ?

C13B C14B 1.376(9) . ?

C13B C18B 1.386(8) . ?

C14B C15B 1.368(9) . ?

C14B H14B 0.93 . ?

C15B C16B 1.364(11) . ?

C15B H15B 0.93 . ?

C16B C17B 1.371(11) . ?

C16B H16B 0.93 . ?

C17B C18B 1.371(10) . ?

C17B H17B 0.93 . ?

C18B H18B 0.93 . ?

N1P C3P 1.340(7) . ?

N1P N2P 1.358(6) . ?

N2P C1P 1.331(7) . ?

N3P C8P 1.348(8) . ?

N3P N4P 1.377(7) . ?

N4P C6P 1.332(8) . ?

C1P C2P 1.364(8) . ?

C1P C5P 1.497(8) . ?

C2P C3P 1.375(9) . ?

C2P H5P 0.93 . ?

C3P C4P 1.511(9) . ?

C4P H41 0.96 . ?

C4P H42 0.96 . ?

C4P H43 0.96 . ?

C5P H51 0.96 . ?

222

C5P H52 0.96 . ?

C5P H53 0.96 . ?

C6P C7P 1.374(9) . ?

C6P C10P 1.503(9) . ?

C7P C8P 1.367(9) . ?

C7P H7P 0.93 . ?

C8P C9P 1.497(9) . ?

C9P H91 0.96 . ?

C9P H92 0.96 . ?

C9P H93 0.96 . ?

C10P H101 0.96 . ?

C10P H102 0.96 . ?

C10P H103 0.96 . ?

loop_




_geom_angle




N4P Pd1 N1A 175.2(3) . . ?

N4P Pd1 N2P 85.74(19) . . ?

N1A Pd1 N2P 92.8(2) . . ?

N4P Pd1 P1 98.66(14) . . ?

N1A Pd1 P1 82.91(17) . . ?

N2P Pd1 P1 175.45(13) . . ?

N4P Pd1 Pd2 64.09(14) . . ?

N1A Pd1 Pd2 111.2(2) . . ?

N2P Pd1 Pd2 60.82(13) . . ?

P1 Pd1 Pd2 122.19(5) . . ?

N1P Pd2 N1 178.7(3) . . ?

223

N1P Pd2 N3P 86.48(19) . . ?

N1 Pd2 N3P 93.1(2) . . ?

N1P Pd2 P2 95.70(13) . . ?

N1 Pd2 P2 84.70(18) . . ?

N3P Pd2 P2 176.62(14) . . ?

N1P Pd2 Pd1 63.52(13) . . ?

N1 Pd2 Pd1 117.3(2) . . ?

N3P Pd2 Pd1 60.75(13) . . ?

P2 Pd2 Pd1 122.55(5) . . ?

N2 N1 Pd2 124.1(6) . . ?

N1 N2 N3 173.3(9) . . ?

N2A N1A Pd1 127.5(6) . . ?

N1A N2A N3A 174.0(9) . . ?

C1A P1 C7A 109.9(3) . . ?

C1A P1 C13A 100.8(3) . . ?

C7A P1 C13A 106.9(3) . . ?

C1A P1 Pd1 110.7(2) . . ?

C7A P1 Pd1 107.0(2) . . ?

C13A P1 Pd1 121.2(2) . . ?

C7B P2 C13B 103.2(3) . . ?

C7B P2 C1B 104.3(3) . . ?

C13B P2 C1B 108.0(3) . . ?

C7B P2 Pd2 116.2(2) . . ?

C13B P2 Pd2 108.3(2) . . ?

C1B P2 Pd2 115.9(2) . . ?

C2A C1A C6A 117.9(7) . . ?

C2A C1A P1 122.1(5) . . ?

C6A C1A P1 119.9(5) . . ?

C1A C2A C3A 120.1(7) . . ?

C1A C2A H2A 120 . . ?

C3A C2A H2A 120 . . ?

C4A C3A C2A 120.7(8) . . ?

C4A C3A H3A 119.7 . . ?

224

C2A C3A H3A 119.6 . . ?

C5A C4A C3A 119.2(8) . . ?

C5A C4A H4A 120.4 . . ?

C3A C4A H4A 120.4 . . ?

C4A C5A C6A 120.7(8) . . ?

C4A C5A H5A 119.7 . . ?

C6A C5A H5A 119.7 . . ?

C5A C6A C1A 121.4(7) . . ?

C5A C6A H6A 119.3 . . ?

C1A C6A H6A 119.3 . . ?

C12A C7A C8A 118.6(7) . . ?

C12A C7A P1 118.5(6) . . ?

C8A C7A P1 122.2(6) . . ?

C9A C8A C7A 119.7(8) . . ?

C9A C8A H8A 120.1 . . ?

C7A C8A H8A 120.1 . . ?

C10A C9A C8A 120.3(9) . . ?

C10A C9A H9A 119.8 . . ?

C8A C9A H9A 119.9 . . ?

C11A C10A C9A 120.2(9) . . ?

C11A C10A H10A 119.9 . . ?

C9A C10A H10A 120 . . ?

C12A C11A C10A 119.8(10) . . ?

C12A C11A H11A 120.1 . . ?

C10A C11A H11A 120.1 . . ?

C11A C12A C7A 121.3(9) . . ?

C11A C12A H12A 119.3 . . ?

C7A C12A H12A 119.4 . . ?

C18A C13A C14A 119.2(6) . . ?

C18A C13A P1 123.4(5) . . ?

C14A C13A P1 116.8(5) . . ?

C15A C14A C13A 119.0(7) . . ?

C15A C14A H14A 120.5 . . ?

225

C13A C14A H14A 120.5 . . ?

C16A C15A C14A 121.0(8) . . ?

C16A C15A H15A 119.5 . . ?

C14A C15A H15A 119.5 . . ?

C17A C16A C15A 119.8(7) . . ?

C17A C16A H16A 120.1 . . ?

C15A C16A H16A 120.1 . . ?

C16A C17A C18A 120.7(7) . . ?

C16A C17A H17A 119.7 . . ?

C18A C17A H17A 119.7 . . ?

C17A C18A C13A 120.3(8) . . ?

C17A C18A H18A 119.9 . . ?

C13A C18A H18A 119.9 . . ?

C6B C1B C2B 118.7(6) . . ?

C6B C1B P2 123.2(6) . . ?

C2B C1B P2 118.1(5) . . ?

C3B C2B C1B 121.0(7) . . ?

C3B C2B H2B 119.5 . . ?

C1B C2B H2B 119.5 . . ?

C4B C3B C2B 119.6(8) . . ?

C4B C3B H3B 120.2 . . ?

C2B C3B H3B 120.2 . . ?

C5B C4B C3B 120.3(7) . . ?

C5B C4B H4B 119.8 . . ?

C3B C4B H4B 119.9 . . ?

C4B C5B C6B 120.7(8) . . ?

C4B C5B H5B 119.6 . . ?

C6B C5B H5B 119.6 . . ?

C1B C6B C5B 119.7(8) . . ?

C1B C6B H6B 120.2 . . ?

C5B C6B H6B 120.1 . . ?

C12B C7B C8B 117.6(7) . . ?

C12B C7B P2 120.5(5) . . ?

226

C8B C7B P2 121.9(5) . . ?

C7B C8B C9B 120.5(7) . . ?

C7B C8B H8B 119.8 . . ?

C9B C8B H8B 119.8 . . ?

C10B C9B C8B 121.2(8) . . ?

C10B C9B H9B 119.4 . . ?

C8B C9B H9B 119.4 . . ?

C9B C10B C11B 120.0(8) . . ?

C9B C10B H10B 120 . . ?

C11B C10B H10B 120 . . ?

C10B C11B C12B 119.1(7) . . ?

C10B C11B H11B 120.5 . . ?

C12B C11B H11B 120.4 . . ?

C7B C12B C11B 121.6(7) . . ?

C7B C12B H12B 119.2 . . ?

C11B C12B H12B 119.2 . . ?

C14B C13B C18B 118.2(6) . . ?

C14B C13B P2 119.7(5) . . ?

C18B C13B P2 122.1(5) . . ?

C15B C14B C13B 121.0(7) . . ?

C15B C14B H14B 119.5 . . ?

C13B C14B H14B 119.5 . . ?

C16B C15B C14B 120.5(7) . . ?

C16B C15B H15B 119.7 . . ?

C14B C15B H15B 119.8 . . ?

C15B C16B C17B 119.3(7) . . ?

C15B C16B H16B 120.4 . . ?

C17B C16B H16B 120.3 . . ?

C18B C17B C16B 120.5(7) . . ?

C18B C17B H17B 119.7 . . ?

C16B C17B H17B 119.8 . . ?

C17B C18B C13B 120.4(7) . . ?

C17B C18B H18B 119.8 . . ?

227

C13B C18B H18B 119.8 . . ?

C3P N1P N2P 108.0(4) . . ?

C3P N1P Pd2 136.0(4) . . ?

N2P N1P Pd2 115.6(3) . . ?

C1P N2P N1P 108.3(4) . . ?

C1P N2P Pd1 131.1(4) . . ?

N1P N2P Pd1 120.0(3) . . ?

C8P N3P N4P 107.3(5) . . ?

C8P N3P Pd2 131.0(4) . . ?

N4P N3P Pd2 120.0(4) . . ?

C6P N4P N3P 108.5(5) . . ?

C6P N4P Pd1 135.9(5) . . ?

N3P N4P Pd1 115.0(4) . . ?

N2P C1P C2P 109.0(5) . . ?

N2P C1P C5P 120.5(5) . . ?

C2P C1P C5P 130.5(6) . . ?

C1P C2P C3P 106.2(5) . . ?

C1P C2P H5P 126.9 . . ?

C3P C2P H5P 126.9 . . ?

N1P C3P C2P 108.4(5) . . ?

N1P C3P C4P 121.3(6) . . ?

C2P C3P C4P 130.3(6) . . ?

C3P C4P H41 109.5 . . ?

C3P C4P H42 109.5 . . ?

H41 C4P H42 109.5 . . ?

C3P C4P H43 109.5 . . ?

H41 C4P H43 109.5 . . ?

H42 C4P H43 109.5 . . ?

C1P C5P H51 109.5 . . ?

C1P C5P H52 109.5 . . ?

H51 C5P H52 109.5 . . ?

C1P C5P H53 109.5 . . ?

H51 C5P H53 109.5 . . ?

228

H52 C5P H53 109.5 . . ?

N4P C6P C7P 108.6(6) . . ?

N4P C6P C10P 122.0(6) . . ?

C7P C6P C10P 129.4(6) . . ?

C8P C7P C6P 106.9(6) . . ?

C8P C7P H7P 126.6 . . ?

C6P C7P H7P 126.6 . . ?

N3P C8P C7P 108.7(6) . . ?

N3P C8P C9P 119.9(6) . . ?

C7P C8P C9P 131.3(6) . . ?

C8P C9P H91 109.5 . . ?

C8P C9P H92 109.5 . . ?

H91 C9P H92 109.5 . . ?

C8P C9P H93 109.5 . . ?

H91 C9P H93 109.5 . . ?

H92 C9P H93 109.5 . . ?

C6P C10P H101 109.5 . . ?

C6P C10P H102 109.5 . . ?

H101 C10P H102 109.5 . . ?

C6P C10P H103 109.4 . . ?

H101 C10P H103 109.5 . . ?

H102 C10P H103 109.5 . . ?

loop_





_geom_torsion





229


N4P Pd1 Pd2 N1P -99.3(2) . . . . ?

N1A Pd1 Pd2 N1P 81.9(2) . . . . ?

N2P Pd1 Pd2 N1P 0.9(2) . . . . ?

P1 Pd1 Pd2 N1P 176.91(16) . . . . ?

N4P Pd1 Pd2 N1 79.5(3) . . . . ?

N1A Pd1 Pd2 N1 -99.3(3) . . . . ?

N2P Pd1 Pd2 N1 179.7(3) . . . . ?

P1 Pd1 Pd2 N1 -4.3(2) . . . . ?

N4P Pd1 Pd2 N3P 2.3(2) . . . . ?

N1A Pd1 Pd2 N3P -176.6(3) . . . . ?

N2P Pd1 Pd2 N3P 102.4(2) . . . . ?

P1 Pd1 Pd2 N3P -81.54(17) . . . . ?

N4P Pd1 Pd2 P2 -178.56(16) . . . . ?

N1A Pd1 Pd2 P2 2.6(2) . . . . ?

N2P Pd1 Pd2 P2 -78.38(16) . . . . ?

P1 Pd1 Pd2 P2 97.65(8) . . . . ?

N1P Pd2 N1 N2 92(10) . . . . ?

N3P Pd2 N1 N2 22.1(9) . . . . ?

P2 Pd2 N1 N2 -160.5(9) . . . . ?

Pd1 Pd2 N1 N2 -36.4(9) . . . . ?

Pd2 N1 N2 N3 -175(10) . . . . ?

N4P Pd1 N1A N2A -89(3) . . . . ?

N2P Pd1 N1A N2A -16.7(9) . . . . ?

P1 Pd1 N1A N2A 161.8(9) . . . . ?

Pd2 Pd1 N1A N2A -76.4(9) . . . . ?

Pd1 N1A N2A N3A 160(9) . . . . ?

N4P Pd1 P1 C1A -113.9(3) . . . . ?

N1A Pd1 P1 C1A 61.5(3) . . . . ?

N2P Pd1 P1 C1A 81.3(18) . . . . ?

Pd2 Pd1 P1 C1A -49.1(2) . . . . ?

N4P Pd1 P1 C7A 126.4(3) . . . . ?

N1A Pd1 P1 C7A -58.2(4) . . . . ?

230

N2P Pd1 P1 C7A -38.4(18) . . . . ?

Pd2 Pd1 P1 C7A -168.9(3) . . . . ?

N4P Pd1 P1 C13A 3.7(3) . . . . ?

N1A Pd1 P1 C13A 179.0(4) . . . . ?

N2P Pd1 P1 C13A -161.2(18) . . . . ?

Pd2 Pd1 P1 C13A 68.4(3) . . . . ?

N1P Pd2 P2 C7B -133.6(3) . . . . ?

N1 Pd2 P2 C7B 47.7(3) . . . . ?

N3P Pd2 P2 C7B 96(3) . . . . ?

Pd1 Pd2 P2 C7B -71.5(2) . . . . ?

N1P Pd2 P2 C13B 110.8(2) . . . . ?

N1 Pd2 P2 C13B -67.9(3) . . . . ?

N3P Pd2 P2 C13B -19(3) . . . . ?

Pd1 Pd2 P2 C13B 172.9(2) . . . . ?

N1P Pd2 P2 C1B -10.6(3) . . . . ?

N1 Pd2 P2 C1B 170.7(4) . . . . ?

N3P Pd2 P2 C1B -141(3) . . . . ?

Pd1 Pd2 P2 C1B 51.5(3) . . . . ?

C7A P1 C1A C2A -49.1(6) . . . . ?

C13A P1 C1A C2A 63.5(6) . . . . ?

Pd1 P1 C1A C2A -167.1(5) . . . . ?

C7A P1 C1A C6A 135.9(6) . . . . ?

C13A P1 C1A C6A -111.6(6) . . . . ?

Pd1 P1 C1A C6A 17.8(6) . . . . ?

C6A C1A C2A C3A -1.6(11) . . . . ?

P1 C1A C2A C3A -176.8(6) . . . . ?

C1A C2A C3A C4A 1.7(12) . . . . ?

C2A C3A C4A C5A -1.5(13) . . . . ?

C3A C4A C5A C6A 1.2(14) . . . . ?

C4A C5A C6A C1A -1.2(13) . . . . ?

C2A C1A C6A C5A 1.4(11) . . . . ?

P1 C1A C6A C5A 176.6(6) . . . . ?

C1A P1 C7A C12A 167.9(6) . . . . ?

231

C13A P1 C7A C12A 59.3(7) . . . . ?

Pd1 P1 C7A C12A -71.9(6) . . . . ?

C1A P1 C7A C8A -21.8(7) . . . . ?

C13A P1 C7A C8A -130.3(6) . . . . ?

Pd1 P1 C7A C8A 98.5(6) . . . . ?

C12A C7A C8A C9A 0.0(11) . . . . ?

P1 C7A C8A C9A -170.3(6) . . . . ?

C7A C8A C9A C10A 1.2(13) . . . . ?

C8A C9A C10A C11A -1.3(15) . . . . ?

C9A C10A C11A C12A 0.0(15) . . . . ?

C10A C11A C12A C7A 1.4(14) . . . . ?

C8A C7A C12A C11A -1.4(12) . . . . ?

P1 C7A C12A C11A 169.3(7) . . . . ?

C1A P1 C13A C18A -97.7(6) . . . . ?

C7A P1 C13A C18A 17.2(7) . . . . ?

Pd1 P1 C13A C18A 140.0(5) . . . . ?

C1A P1 C13A C14A 73.8(6) . . . . ?

C7A P1 C13A C14A -171.3(5) . . . . ?

Pd1 P1 C13A C14A -48.5(6) . . . . ?

C18A C13A C14A C15A 0.4(10) . . . . ?

P1 C13A C14A C15A -171.5(5) . . . . ?

C13A C14A C15A C16A 0.4(11) . . . . ?

C14A C15A C16A C17A 0.0(12) . . . . ?

C15A C16A C17A C18A -1.2(13) . . . . ?

C16A C17A C18A C13A 1.9(12) . . . . ?

C14A C13A C18A C17A -1.5(11) . . . . ?

P1 C13A C18A C17A 169.8(6) . . . . ?

C7B P2 C1B C6B -96.0(6) . . . . ?

C13B P2 C1B C6B 13.4(7) . . . . ?

Pd2 P2 C1B C6B 135.0(6) . . . . ?

C7B P2 C1B C2B 83.3(6) . . . . ?

C13B P2 C1B C2B -167.3(5) . . . . ?

Pd2 P2 C1B C2B -45.7(6) . . . . ?

232

C6B C1B C2B C3B 0.8(11) . . . . ?

P2 C1B C2B C3B -178.5(6) . . . . ?

C1B C2B C3B C4B -1.1(12) . . . . ?

C2B C3B C4B C5B -0.1(13) . . . . ?

C3B C4B C5B C6B 1.6(14) . . . . ?

C2B C1B C6B C5B 0.6(11) . . . . ?

P2 C1B C6B C5B 179.9(6) . . . . ?

C4B C5B C6B C1B -1.8(14) . . . . ?

C13B P2 C7B C12B 45.1(6) . . . . ?

C1B P2 C7B C12B 157.9(5) . . . . ?

Pd2 P2 C7B C12B -73.3(5) . . . . ?

C13B P2 C7B C8B -135.4(6) . . . . ?

C1B P2 C7B C8B -22.7(6) . . . . ?

Pd2 P2 C7B C8B 106.2(5) . . . . ?

C12B C7B C8B C9B 0.1(11) . . . . ?

P2 C7B C8B C9B -179.3(6) . . . . ?

C7B C8B C9B C10B -1.6(13) . . . . ?

C8B C9B C10B C11B 2.3(13) . . . . ?

C9B C10B C11B C12B -1.6(12) . . . . ?

C8B C7B C12B C11B 0.5(10) . . . . ?

P2 C7B C12B C11B -180.0(5) . . . . ?

C10B C11B C12B C7B 0.2(11) . . . . ?

C7B P2 C13B C14B -132.5(5) . . . . ?

C1B P2 C13B C14B 117.4(6) . . . . ?

Pd2 P2 C13B C14B -8.8(6) . . . . ?

C7B P2 C13B C18B 45.7(6) . . . . ?

C1B P2 C13B C18B -64.4(6) . . . . ?

Pd2 P2 C13B C18B 169.4(5) . . . . ?

C18B C13B C14B C15B -0.1(10) . . . . ?

P2 C13B C14B C15B 178.2(6) . . . . ?

C13B C14B C15B C16B 0.6(12) . . . . ?

C14B C15B C16B C17B 0.3(12) . . . . ?

C15B C16B C17B C18B -1.7(11) . . . . ?

233

C16B C17B C18B C13B 2.3(11) . . . . ?

C14B C13B C18B C17B -1.4(10) . . . . ?

P2 C13B C18B C17B -179.5(5) . . . . ?

N1 Pd2 N1P C3P 42(10) . . . . ?

N3P Pd2 N1P C3P 111.8(6) . . . . ?

P2 Pd2 N1P C3P -65.6(6) . . . . ?

Pd1 Pd2 N1P C3P 170.7(6) . . . . ?

N1 Pd2 N1P N2P -130(9) . . . . ?

N3P Pd2 N1P N2P -60.2(4) . . . . ?

P2 Pd2 N1P N2P 122.4(4) . . . . ?

Pd1 Pd2 N1P N2P -1.3(3) . . . . ?

C3P N1P N2P C1P 0.2(6) . . . . ?

Pd2 N1P N2P C1P 174.4(4) . . . . ?

C3P N1P N2P Pd1 -172.1(4) . . . . ?

Pd2 N1P N2P Pd1 2.1(5) . . . . ?

N4P Pd1 N2P C1P -109.0(5) . . . . ?

N1A Pd1 N2P C1P 75.6(6) . . . . ?

P1 Pd1 N2P C1P 56(2) . . . . ?

Pd2 Pd1 N2P C1P -171.6(6) . . . . ?

N4P Pd1 N2P N1P 61.3(4) . . . . ?

N1A Pd1 N2P N1P -114.1(5) . . . . ?

P1 Pd1 N2P N1P -133.8(16) . . . . ?

Pd2 Pd1 N2P N1P -1.3(3) . . . . ?

N1P Pd2 N3P C8P -105.2(6) . . . . ?

N1 Pd2 N3P C8P 73.5(6) . . . . ?

P2 Pd2 N3P C8P 25(3) . . . . ?

Pd1 Pd2 N3P C8P -166.7(6) . . . . ?

N1P Pd2 N3P N4P 58.0(4) . . . . ?

N1 Pd2 N3P N4P -123.2(5) . . . . ?

P2 Pd2 N3P N4P -172(2) . . . . ?

Pd1 Pd2 N3P N4P -3.4(4) . . . . ?

C8P N3P N4P C6P -0.1(7) . . . . ?

Pd2 N3P N4P C6P -167.0(4) . . . . ?

234

C8P N3P N4P Pd1 172.2(4) . . . . ?

Pd2 N3P N4P Pd1 5.3(5) . . . . ?

N1A Pd1 N4P C6P 18E1(10) . . . . ?

N2P Pd1 N4P C6P 106.7(6) . . . . ?

P1 Pd1 N4P C6P -72.1(6) . . . . ?

Pd2 Pd1 N4P C6P 166.3(7) . . . . ?

N1A Pd1 N4P N3P 10(3) . . . . ?

N2P Pd1 N4P N3P -62.8(4) . . . . ?

P1 Pd1 N4P N3P 118.4(4) . . . . ?

Pd2 Pd1 N4P N3P -3.2(3) . . . . ?

N1P N2P C1P C2P 1.2(7) . . . . ?

Pd1 N2P C1P C2P 172.3(4) . . . . ?

N1P N2P C1P C5P -177.4(5) . . . . ?

Pd1 N2P C1P C5P -6.3(9) . . . . ?

N2P C1P C2P C3P -2.1(7) . . . . ?

C5P C1P C2P C3P 176.3(6) . . . . ?

N2P N1P C3P C2P -1.5(7) . . . . ?

Pd2 N1P C3P C2P -173.9(4) . . . . ?

N2P N1P C3P C4P 177.6(6) . . . . ?

Pd2 N1P C3P C4P 5.2(10) . . . . ?

C1P C2P C3P N1P 2.2(7) . . . . ?

C1P C2P C3P C4P -176.9(7) . . . . ?

N3P N4P C6P C7P -0.6(8) . . . . ?

Pd1 N4P C6P C7P -170.6(5) . . . . ?

N3P N4P C6P C10P 178.8(6) . . . . ?

Pd1 N4P C6P C10P 8.8(11) . . . . ?

N4P C6P C7P C8P 1.1(9) . . . . ?

C10P C6P C7P C8P -178.3(8) . . . . ?

N4P N3P C8P C7P 0.8(7) . . . . ?

Pd2 N3P C8P C7P 165.6(5) . . . . ?

N4P N3P C8P C9P -177.7(6) . . . . ?

Pd2 N3P C8P C9P -12.8(10) . . . . ?

C6P C7P C8P N3P -1.1(9) . . . . ?

235

C6P C7P C8P C9P 177.1(8) . . . . ?

A4.4, C24H30N6Pd2 (cyPd3)

#\#CIF_1.1


# Created on 2010-03-02 at 10:52:19





# CIF files read : chuck02 struct


data_global

#------------------ AUDIT DETAILS -------------------------------------------#









236



;



Glasgow G12 8QQ

Scotland UK

;







;




;



--#








237









_journal_year ?

_journal_volume ?

_journal_issue ?






_publ_section_title

;

?

;


;

?

;

loop_

_publ_author_name



;

238



Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#


;


?

;


;


?

;


;


?

;


;

?

;


;

?

239

;



;


Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.














The Netherlands.

240











A24, 351-359



Volume C.








241





34, 824-828


35, 281.




;


;


;


;

?

;


;




;


242

data_chuck02




_chemical_formula_moiety 'C24 H30 N6 Pd2'

_chemical_formula_sum 'C24 H30 N6 Pd2'



_symmetry_cell_setting monoclinic

_symmetry_space_group_name_H-M 'P 1 21/c 1'

loop_


'x, y, z'

'-x, y+1/2, -z+1/2'

'-x, -y, -z'

'x, -y-1/2, z-1/2'





_cell_angle_beta 106.51






243
























_diffrn_reflns_limit_l_min 0






244

0.997


0.997



















Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^








245


_refine_ls_shift/su_max 0





loop_

_atom_type_symbol









loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type






Pd2 Pd 0.35586(3) -0.00521(4) 0.30491(3) 0.0374(3) Uani 1 d . . .

246

Pd1 Pd 0.15970(3) -0.03659(4) 0.15018(3) 0.0370(3) Uani 1 d . . .

N2 N 0.3625(4) 0.0014(4) 0.1700(3) 0.0407(13) Uani 1 d . . .

N1 N 0.2782(3) -0.0250(4) 0.1083(3) 0.0418(12) Uani 1 d . . .

N3 N 0.0360(3) -0.0316(4) 0.1925(3) 0.0447(13) Uani 1 d . . .

C1 C 0.2938(5) -0.0332(6) 0.0296(5) 0.0547(17) Uani 1 d . . .

H1 H 0.2475 -0.0514 -0.0235 0.066 Uiso 1 calc R . .

C2 C 0.3885(5) -0.0110(6) 0.0377(5) 0.0587(19) Uani 1 d . . .

H2 H 0.4188 -0.0103 -0.0073 0.07 Uiso 1 calc R . .

C3 C 0.4288(5) 0.0099(5) 0.1267(5) 0.0472(17) Uani 1 d . . .

H3 H 0.4932 0.0276 0.1531 0.057 Uiso 1 calc R . .

C4 C 0.1064(4) 0.1156(5) 0.0922(3) 0.0414(15) Uani 1 d . . .

C5 C 0.1523(5) 0.2061(6) 0.0592(4) 0.0554(17) Uani 1 d . . .

H5 H 0.2165 0.1972 0.0612 0.066 Uiso 1 calc R . .

C6 C 0.1033(7) 0.3102(7) 0.0232(4) 0.078(2) Uani 1 d . . .

H6 H 0.1353 0.3711 0.0029 0.094 Uiso 1 calc R . .

C7 C 0.0081(7) 0.3220(8) 0.0180(5) 0.080(2) Uani 1 d . . .

H7 H -0.0252 0.3897 -0.0084 0.096 Uiso 1 calc R . .

C8 C -0.0381(5) 0.2365(7) 0.0508(5) 0.070(2) Uani 1 d . . .

H8 H -0.1024 0.247 0.048 0.085 Uiso 1 calc R . .

C9 C 0.0094(4) 0.1328(6) 0.0886(4) 0.0473(16) Uani 1 d . . .

C10 C -0.0369(4) 0.0351(6) 0.1253(4) 0.0513(18) Uani 1 d . . .

H101 H -0.0838 0.0683 0.1522 0.062 Uiso 1 calc R . .

H102 H -0.0701 -0.0182 0.0776 0.062 Uiso 1 calc R . .

C11 C 0.0620(5) 0.0344(6) 0.2794(4) 0.0570(18) Uani 1 d . . .

H111 H 0.0811 0.1143 0.2703 0.068 Uiso 1 calc R . .

H112 H 0.1141 -0.0059 0.3212 0.068 Uiso 1 calc R . .

H113 H 0.0074 0.0369 0.3025 0.068 Uiso 1 calc R . .

C12 C -0.0029(4) -0.1487(6) 0.2071(4) 0.0654(19) Uani 1 d . . .

H121 H -0.061 -0.1376 0.2238 0.079 Uiso 1 calc R . .

H122 H 0.0433 -0.1902 0.2538 0.079 Uiso 1 calc R . .

H123 H -0.0163 -0.1947 0.1531 0.079 Uiso 1 calc R . .

N1A N 0.3070(3) -0.1747(4) 0.2827(3) 0.0381(12) Uani 1 d . . .

N2A N 0.2209(3) -0.1926(4) 0.2216(3) 0.0378(12) Uani 1 d . . .

247

N3A N 0.4009(3) 0.1703(4) 0.3383(3) 0.0507(14) Uani 1 d . . .

C1A C 0.3377(4) -0.2773(6) 0.3233(4) 0.0489(17) Uani 1 d . . .

H1A H 0.3944 -0.2878 0.3688 0.059 Uiso 1 calc R . .

C2A C 0.2717(5) -0.3668(6) 0.2869(4) 0.0529(16) Uani 1 d . . .

H2A H 0.275 -0.4475 0.3015 0.063 Uiso 1 calc R . .

C3A C 0.2005(4) -0.3080(6) 0.2244(4) 0.0503(16) Uani 1 d . . .

H3A H 0.1453 -0.3442 0.1886 0.06 Uiso 1 calc R . .

C4A C 0.3429(4) -0.0053(5) 0.4271(4) 0.0397(16) Uani 1 d . . .

C5A C 0.2934(4) -0.0843(6) 0.4663(4) 0.0510(16) Uani 1 d . . .

H5A H 0.2606 -0.148 0.4331 0.061 Uiso 1 calc R . .

C6A C 0.2916(5) -0.0704(7) 0.5534(5) 0.0667(19) Uani 1 d . . .

H6A H 0.2584 -0.1246 0.5788 0.08 Uiso 1 calc R . .

C7A C 0.3389(5) 0.0236(8) 0.6021(5) 0.074(2) Uani 1 d . . .

H7A H 0.3376 0.0329 0.6608 0.088 Uiso 1 calc R . .

C8A C 0.3883(5) 0.1049(6) 0.5662(4) 0.0641(18) Uani 1 d . . .

H8A H 0.4199 0.1687 0.6001 0.077 Uiso 1 calc R . .

C9A C 0.3906(4) 0.0907(6) 0.4793(4) 0.0466(16) Uani 1 d . . .

C10A C 0.4462(4) 0.1706(5) 0.4375(4) 0.0538(17) Uani 1 d . . .

H1A1 H 0.5122 0.1431 0.4511 0.065 Uiso 1 calc R . .

H1A2 H 0.4465 0.2511 0.4607 0.065 Uiso 1 calc R . .

C11A C 0.3151(5) 0.2477(6) 0.3158(5) 0.082(2) Uani 1 d . . .

H11A H 0.3338 0.3284 0.3332 0.098 Uiso 1 calc R . .

H21A H 0.2708 0.2203 0.347 0.098 Uiso 1 calc R . .

H31A H 0.2848 0.2447 0.2527 0.098 Uiso 1 calc R . .

C12A C 0.4714(6) 0.2156(6) 0.2929(4) 0.079(2) Uani 1 d . . .

H12A H 0.4421 0.217 0.2296 0.095 Uiso 1 calc R . .

H22A H 0.5264 0.1639 0.3064 0.095 Uiso 1 calc R . .

H32A H 0.4911 0.2949 0.3136 0.095 Uiso 1 calc R . .

loop_




248





Pd2 0.0455(4) 0.0353(4) 0.0264(4) 0.0025(2) 0.0023(3) -0.0014(2)

Pd1 0.0368(4) 0.0437(4) 0.0290(4) -0.0007(2) 0.0068(3) 0.0007(2)

N2 0.043(3) 0.047(3) 0.031(3) 0.003(2) 0.010(3) -0.001(2)

N1 0.041(3) 0.056(3) 0.026(3) -0.001(2) 0.005(3) -0.001(2)

N3 0.042(3) 0.048(3) 0.041(3) 0.003(3) 0.006(2) 0.004(3)

C1 0.043(5) 0.084(5) 0.034(5) -0.002(3) 0.006(3) 0.000(3)

C2 0.056(5) 0.085(5) 0.044(5) 0.008(4) 0.028(4) 0.006(4)

C3 0.041(4) 0.050(4) 0.050(5) 0.009(3) 0.014(4) 0.001(3)

C4 0.045(4) 0.049(4) 0.023(3) 0.000(3) -0.002(3) 0.000(3)

C5 0.057(4) 0.059(5) 0.041(4) 0.001(4) -0.001(3) 0.000(4)

C6 0.101(7) 0.058(6) 0.061(5) 0.009(4) -0.003(4) -0.012(5)

C7 0.098(7) 0.061(5) 0.058(5) 0.011(4) -0.014(5) 0.018(5)

C8 0.070(5) 0.073(6) 0.053(5) -0.001(4) -0.008(4) 0.019(5)

C9 0.048(4) 0.054(5) 0.030(3) -0.003(3) -0.004(3) 0.009(4)

C10 0.041(4) 0.068(5) 0.042(4) -0.010(4) 0.008(3) 0.007(4)

C11 0.066(4) 0.065(4) 0.040(4) -0.012(4) 0.014(3) 0.008(4)

C12 0.060(4) 0.070(5) 0.072(5) 0.004(4) 0.028(4) -0.002(4)

N1A 0.044(3) 0.035(3) 0.030(3) 0.002(3) 0.003(2) 0.002(3)

N2A 0.041(3) 0.038(4) 0.035(3) -0.004(2) 0.011(3) -0.003(2)

N3A 0.065(3) 0.037(3) 0.038(3) 0.000(2) -0.004(3) -0.010(3)

C1A 0.058(4) 0.049(5) 0.037(4) 0.010(4) 0.010(3) 0.013(4)

C2A 0.073(4) 0.031(4) 0.061(4) -0.004(4) 0.028(4) -0.002(4)

C3A 0.050(4) 0.050(5) 0.050(4) -0.009(4) 0.014(3) -0.004(4)

C4A 0.037(4) 0.048(4) 0.029(4) 0.001(3) 0.003(3) 0.002(3)

C5A 0.053(4) 0.055(4) 0.042(5) -0.006(3) 0.008(3) 0.000(4)

C6A 0.078(5) 0.085(6) 0.045(5) -0.006(4) 0.030(4) -0.004(4)

C7A 0.085(6) 0.103(6) 0.039(4) -0.017(5) 0.027(4) -0.002(5)

C8A 0.081(5) 0.065(5) 0.043(5) -0.013(4) 0.012(4) -0.006(4)

C9A 0.056(4) 0.047(4) 0.030(4) -0.003(3) 0.002(3) -0.001(3)

249

C10A 0.071(4) 0.044(4) 0.035(4) -0.009(3) -0.003(3) -0.004(4)

C11A 0.110(6) 0.040(4) 0.070(5) 0.006(4) -0.014(4) 0.018(4)

C12A 0.124(6) 0.050(4) 0.053(4) 0.005(4) 0.010(4) -0.035(4)



;







;

loop_



_geom_bond_distance



Pd2 C4A 1.972(6) . ?

Pd2 N1A 2.020(5) . ?

Pd2 N3A 2.089(5) . ?

Pd2 N2 2.140(5) . ?

Pd2 Pd1 3.1896(10) . ?

Pd1 C4 1.981(6) . ?

Pd1 N1 2.011(5) . ?

Pd1 N3 2.085(5) . ?

Pd1 N2A 2.126(5) . ?

N2 C3 1.329(7) . ?

N2 N1 1.358(6) . ?

250

N1 C1 1.317(7) . ?

N3 C10 1.466(8) . ?

N3 C12 1.470(7) . ?

N3 C11 1.497(8) . ?

C1 C2 1.367(8) . ?

C1 H1 0.93 . ?

C2 C3 1.368(9) . ?

C2 H2 0.93 . ?

C3 H3 0.93 . ?

C4 C5 1.389(8) . ?

C4 C9 1.406(7) . ?

C5 C6 1.397(9) . ?

C5 H5 0.93 . ?

C6 C7 1.368(9) . ?

C6 H6 0.93 . ?

C7 C8 1.350(10) . ?

C7 H7 0.93 . ?

C8 C9 1.394(9) . ?

C8 H8 0.93 . ?

C9 C10 1.481(8) . ?

C10 H101 0.97 . ?

C10 H102 0.97 . ?

C11 H111 0.96 . ?

C11 H112 0.96 . ?

C11 H113 0.96 . ?

C12 H121 0.96 . ?

C12 H122 0.96 . ?

C12 H123 0.96 . ?

N1A C1A 1.327(7) . ?

N1A N2A 1.355(6) . ?

N2A C3A 1.329(7) . ?

N3A C11A 1.475(7) . ?

N3A C12A 1.491(8) . ?

251

N3A C10A 1.503(7) . ?

C1A C2A 1.392(8) . ?

C1A H1A 0.93 . ?

C2A C3A 1.372(8) . ?

C2A H2A 0.93 . ?

C3A H3A 0.93 . ?

C4A C5A 1.387(8) . ?

C4A C9A 1.408(8) . ?

C5A C6A 1.379(8) . ?

C5A H5A 0.93 . ?

C6A C7A 1.364(10) . ?

C6A H6A 0.93 . ?

C7A C8A 1.373(9) . ?

C7A H7A 0.93 . ?

C8A C9A 1.376(8) . ?

C8A H8A 0.93 . ?

C9A C10A 1.477(8) . ?

C10A H1A1 0.97 . ?

C10A H1A2 0.97 . ?

C11A H11A 0.96 . ?

C11A H21A 0.96 . ?

C11A H31A 0.96 . ?

C12A H12A 0.96 . ?

C12A H22A 0.96 . ?

C12A H32A 0.96 . ?

loop_




_geom_angle



252


C4A Pd2 N1A 92.3(2) . . ?

C4A Pd2 N3A 82.4(2) . . ?

N1A Pd2 N3A 174.49(17) . . ?

C4A Pd2 N2 176.6(2) . . ?

N1A Pd2 N2 88.55(17) . . ?

N3A Pd2 N2 96.63(17) . . ?

C4A Pd2 Pd1 115.10(17) . . ?

N1A Pd2 Pd1 64.65(13) . . ?

N3A Pd2 Pd1 116.21(12) . . ?

N2 Pd2 Pd1 62.40(14) . . ?

C4 Pd1 N1 93.2(2) . . ?

C4 Pd1 N3 82.1(2) . . ?

N1 Pd1 N3 174.74(19) . . ?

C4 Pd1 N2A 175.65(19) . . ?

N1 Pd1 N2A 87.41(17) . . ?

N3 Pd1 N2A 97.18(17) . . ?

C4 Pd1 Pd2 113.64(16) . . ?

N1 Pd1 Pd2 65.01(14) . . ?

N3 Pd1 Pd2 114.87(13) . . ?

N2A Pd1 Pd2 62.75(13) . . ?

C3 N2 N1 106.9(5) . . ?

C3 N2 Pd2 138.3(4) . . ?

N1 N2 Pd2 114.1(4) . . ?

C1 N1 N2 108.6(5) . . ?

C1 N1 Pd1 133.6(4) . . ?

N2 N1 Pd1 117.7(4) . . ?

C10 N3 C12 109.5(5) . . ?

C10 N3 C11 110.1(5) . . ?

C12 N3 C11 107.9(5) . . ?

C10 N3 Pd1 107.3(4) . . ?

C12 N3 Pd1 115.4(4) . . ?

C11 N3 Pd1 106.5(4) . . ?

253

N1 C1 C2 109.6(6) . . ?

N1 C1 H1 125.2 . . ?

C2 C1 H1 125.2 . . ?

C1 C2 C3 104.7(6) . . ?

C1 C2 H2 127.6 . . ?

C3 C2 H2 127.6 . . ?

N2 C3 C2 110.1(6) . . ?

N2 C3 H3 125 . . ?

C2 C3 H3 125 . . ?

C5 C4 C9 117.8(5) . . ?

C5 C4 Pd1 129.0(4) . . ?

C9 C4 Pd1 113.1(4) . . ?

C4 C5 C6 120.9(6) . . ?

C4 C5 H5 119.5 . . ?

C6 C5 H5 119.5 . . ?

C7 C6 C5 119.6(7) . . ?

C7 C6 H6 120.2 . . ?

C5 C6 H6 120.2 . . ?

C8 C7 C6 120.8(7) . . ?

C8 C7 H7 119.6 . . ?

C6 C7 H7 119.6 . . ?

C7 C8 C9 120.8(7) . . ?

C7 C8 H8 119.6 . . ?

C9 C8 H8 119.6 . . ?

C8 C9 C4 120.0(6) . . ?

C8 C9 C10 123.7(6) . . ?

C4 C9 C10 116.3(5) . . ?

N3 C10 C9 109.8(5) . . ?

N3 C10 H101 109.7 . . ?

C9 C10 H101 109.7 . . ?

N3 C10 H102 109.7 . . ?

C9 C10 H102 109.7 . . ?

H101 C10 H102 108.2 . . ?

254

N3 C11 H111 109.5 . . ?

N3 C11 H112 109.5 . . ?

H111 C11 H112 109.5 . . ?

N3 C11 H113 109.5 . . ?

H111 C11 H113 109.5 . . ?

H112 C11 H113 109.5 . . ?

N3 C12 H121 109.5 . . ?

N3 C12 H122 109.5 . . ?

H121 C12 H122 109.5 . . ?

N3 C12 H123 109.5 . . ?

H121 C12 H123 109.5 . . ?

H122 C12 H123 109.5 . . ?

C1A N1A N2A 109.1(4) . . ?

C1A N1A Pd2 132.6(4) . . ?

N2A N1A Pd2 117.9(4) . . ?

C3A N2A N1A 106.9(4) . . ?

C3A N2A Pd1 138.7(4) . . ?

N1A N2A Pd1 114.4(4) . . ?

C11A N3A C12A 109.6(5) . . ?

C11A N3A C10A 109.7(5) . . ?

C12A N3A C10A 109.3(5) . . ?

C11A N3A Pd2 108.0(4) . . ?

C12A N3A Pd2 114.1(4) . . ?

C10A N3A Pd2 105.9(3) . . ?

N1A C1A C2A 109.2(5) . . ?

N1A C1A H1A 125.4 . . ?

C2A C1A H1A 125.4 . . ?

C3A C2A C1A 103.8(5) . . ?

C3A C2A H2A 128.1 . . ?

C1A C2A H2A 128.1 . . ?

N2A C3A C2A 111.1(5) . . ?

N2A C3A H3A 124.4 . . ?

C2A C3A H3A 124.4 . . ?

255

C5A C4A C9A 117.4(5) . . ?

C5A C4A Pd2 129.3(5) . . ?

C9A C4A Pd2 113.3(4) . . ?

C6A C5A C4A 121.5(6) . . ?

C6A C5A H5A 119.2 . . ?

C4A C5A H5A 119.2 . . ?

C7A C6A C5A 119.3(6) . . ?

C7A C6A H6A 120.3 . . ?

C5A C6A H6A 120.3 . . ?

C6A C7A C8A 121.5(6) . . ?

C6A C7A H7A 119.3 . . ?

C8A C7A H7A 119.3 . . ?

C7A C8A C9A 119.3(6) . . ?

C7A C8A H8A 120.4 . . ?

C9A C8A H8A 120.4 . . ?

C8A C9A C4A 121.0(6) . . ?

C8A C9A C10A 122.5(6) . . ?

C4A C9A C10A 116.5(5) . . ?

C9A C10A N3A 108.7(5) . . ?

C9A C10A H1A1 109.9 . . ?

N3A C10A H1A1 109.9 . . ?

C9A C10A H1A2 109.9 . . ?

N3A C10A H1A2 109.9 . . ?

H1A1 C10A H1A2 108.3 . . ?

N3A C11A H11A 109.5 . . ?

N3A C11A H21A 109.5 . . ?

H11A C11A H21A 109.5 . . ?

N3A C11A H31A 109.5 . . ?

H11A C11A H31A 109.5 . . ?

H21A C11A H31A 109.5 . . ?

N3A C12A H12A 109.5 . . ?

N3A C12A H22A 109.5 . . ?

H12A C12A H22A 109.5 . . ?

256

N3A C12A H32A 109.5 . . ?

H12A C12A H32A 109.5 . . ?

H22A C12A H32A 109.5 . . ?

loop_





_geom_torsion






C4A Pd2 Pd1 C4 99.8(3) . . . . ?

N1A Pd2 Pd1 C4 179.9(2) . . . . ?

N3A Pd2 Pd1 C4 5.9(2) . . . . ?

N2 Pd2 Pd1 C4 -77.7(2) . . . . ?

C4A Pd2 Pd1 N1 -178.1(2) . . . . ?

N1A Pd2 Pd1 N1 -98.04(19) . . . . ?

N3A Pd2 Pd1 N1 88.0(2) . . . . ?

N2 Pd2 Pd1 N1 4.4(2) . . . . ?

C4A Pd2 Pd1 N3 7.7(2) . . . . ?

N1A Pd2 Pd1 N3 87.75(19) . . . . ?

N3A Pd2 Pd1 N3 -86.2(2) . . . . ?

N2 Pd2 Pd1 N3 -169.77(19) . . . . ?

C4A Pd2 Pd1 N2A -77.5(2) . . . . ?

N1A Pd2 Pd1 N2A 2.57(17) . . . . ?

N3A Pd2 Pd1 N2A -171.39(19) . . . . ?

N2 Pd2 Pd1 N2A 105.04(17) . . . . ?

C4A Pd2 N2 C3 141(4) . . . . ?

N1A Pd2 N2 C3 -113.8(6) . . . . ?

257

N3A Pd2 N2 C3 68.0(6) . . . . ?

Pd1 Pd2 N2 C3 -175.8(6) . . . . ?

C4A Pd2 N2 N1 -50(4) . . . . ?

N1A Pd2 N2 N1 55.4(4) . . . . ?

N3A Pd2 N2 N1 -122.7(4) . . . . ?

Pd1 Pd2 N2 N1 -6.5(3) . . . . ?

C3 N2 N1 C1 0.5(6) . . . . ?

Pd2 N2 N1 C1 -172.0(4) . . . . ?

C3 N2 N1 Pd1 -177.1(3) . . . . ?

Pd2 N2 N1 Pd1 10.4(5) . . . . ?

C4 Pd1 N1 C1 -69.2(6) . . . . ?

N3 Pd1 N1 C1 -94(2) . . . . ?

N2A Pd1 N1 C1 115.1(6) . . . . ?

Pd2 Pd1 N1 C1 176.2(6) . . . . ?

C4 Pd1 N1 N2 107.7(4) . . . . ?

N3 Pd1 N1 N2 83(2) . . . . ?

N2A Pd1 N1 N2 -68.0(4) . . . . ?

Pd2 Pd1 N1 N2 -7.0(3) . . . . ?

C4 Pd1 N3 C10 28.2(4) . . . . ?

N1 Pd1 N3 C10 53(2) . . . . ?

N2A Pd1 N3 C10 -156.2(4) . . . . ?

Pd2 Pd1 N3 C10 140.6(3) . . . . ?

C4 Pd1 N3 C12 150.6(4) . . . . ?

N1 Pd1 N3 C12 175.5(19) . . . . ?

N2A Pd1 N3 C12 -33.8(4) . . . . ?

Pd2 Pd1 N3 C12 -97.0(4) . . . . ?

C4 Pd1 N3 C11 -89.7(4) . . . . ?

N1 Pd1 N3 C11 -65(2) . . . . ?

N2A Pd1 N3 C11 86.0(4) . . . . ?

Pd2 Pd1 N3 C11 22.7(4) . . . . ?

N2 N1 C1 C2 -0.7(7) . . . . ?

Pd1 N1 C1 C2 176.4(4) . . . . ?

N1 C1 C2 C3 0.6(7) . . . . ?

258

N1 N2 C3 C2 -0.2(6) . . . . ?

Pd2 N2 C3 C2 169.6(4) . . . . ?

C1 C2 C3 N2 -0.2(7) . . . . ?

N1 Pd1 C4 C5 -15.4(5) . . . . ?

N3 Pd1 C4 C5 162.3(5) . . . . ?

N2A Pd1 C4 C5 82(3) . . . . ?

Pd2 Pd1 C4 C5 48.6(5) . . . . ?

N1 Pd1 C4 C9 167.3(4) . . . . ?

N3 Pd1 C4 C9 -14.9(4) . . . . ?

N2A Pd1 C4 C9 -95(3) . . . . ?

Pd2 Pd1 C4 C9 -128.6(3) . . . . ?

C9 C4 C5 C6 -0.4(8) . . . . ?

Pd1 C4 C5 C6 -177.5(4) . . . . ?

C4 C5 C6 C7 -1.8(10) . . . . ?

C5 C6 C7 C8 2.9(11) . . . . ?

C6 C7 C8 C9 -1.6(11) . . . . ?

C7 C8 C9 C4 -0.6(9) . . . . ?

C7 C8 C9 C10 -179.7(6) . . . . ?

C5 C4 C9 C8 1.6(8) . . . . ?

Pd1 C4 C9 C8 179.2(4) . . . . ?

C5 C4 C9 C10 -179.3(5) . . . . ?

Pd1 C4 C9 C10 -1.7(6) . . . . ?

C12 N3 C10 C9 -161.5(5) . . . . ?

C11 N3 C10 C9 80.0(6) . . . . ?

Pd1 N3 C10 C9 -35.5(5) . . . . ?

C8 C9 C10 N3 -155.1(6) . . . . ?

C4 C9 C10 N3 25.8(7) . . . . ?

C4A Pd2 N1A C1A -58.9(5) . . . . ?

N3A Pd2 N1A C1A -75(2) . . . . ?

N2 Pd2 N1A C1A 124.4(5) . . . . ?

Pd1 Pd2 N1A C1A -175.7(5) . . . . ?

C4A Pd2 N1A N2A 112.7(3) . . . . ?

N3A Pd2 N1A N2A 96.2(18) . . . . ?

259

N2 Pd2 N1A N2A -64.0(3) . . . . ?

Pd1 Pd2 N1A N2A -4.1(3) . . . . ?

C1A N1A N2A C3A -1.1(5) . . . . ?

Pd2 N1A N2A C3A -174.6(3) . . . . ?

C1A N1A N2A Pd1 179.5(3) . . . . ?

Pd2 N1A N2A Pd1 6.0(4) . . . . ?

C4 Pd1 N2A C3A 143(3) . . . . ?

N1 Pd1 N2A C3A -119.7(5) . . . . ?

N3 Pd1 N2A C3A 62.9(5) . . . . ?

Pd2 Pd1 N2A C3A 177.2(6) . . . . ?

C4 Pd1 N2A N1A -38(3) . . . . ?

N1 Pd1 N2A N1A 59.3(3) . . . . ?

N3 Pd1 N2A N1A -118.1(3) . . . . ?

Pd2 Pd1 N2A N1A -3.8(2) . . . . ?

C4A Pd2 N3A C11A -87.9(4) . . . . ?

N1A Pd2 N3A C11A -71.3(19) . . . . ?

N2 Pd2 N3A C11A 88.8(4) . . . . ?

Pd1 Pd2 N3A C11A 26.4(4) . . . . ?

C4A Pd2 N3A C12A 149.9(4) . . . . ?

N1A Pd2 N3A C12A 166.6(17) . . . . ?

N2 Pd2 N3A C12A -33.3(4) . . . . ?

Pd1 Pd2 N3A C12A -95.8(4) . . . . ?

C4A Pd2 N3A C10A 29.6(4) . . . . ?

N1A Pd2 N3A C10A 46(2) . . . . ?

N2 Pd2 N3A C10A -153.7(4) . . . . ?

Pd1 Pd2 N3A C10A 143.9(3) . . . . ?

N2A N1A C1A C2A 1.5(6) . . . . ?

Pd2 N1A C1A C2A 173.7(4) . . . . ?

N1A C1A C2A C3A -1.2(6) . . . . ?

N1A N2A C3A C2A 0.4(6) . . . . ?

Pd1 N2A C3A C2A 179.4(4) . . . . ?

C1A C2A C3A N2A 0.5(6) . . . . ?

N1A Pd2 C4A C5A -14.7(5) . . . . ?

260

N3A Pd2 C4A C5A 163.7(6) . . . . ?

N2 Pd2 C4A C5A 90(4) . . . . ?

Pd1 Pd2 C4A C5A 48.2(6) . . . . ?

N1A Pd2 C4A C9A 166.3(4) . . . . ?

N3A Pd2 C4A C9A -15.3(4) . . . . ?

N2 Pd2 C4A C9A -89(4) . . . . ?

Pd1 Pd2 C4A C9A -130.7(4) . . . . ?

C9A C4A C5A C6A -0.7(9) . . . . ?

Pd2 C4A C5A C6A -179.7(5) . . . . ?

C4A C5A C6A C7A 0.5(10) . . . . ?

C5A C6A C7A C8A 0.0(11) . . . . ?

C6A C7A C8A C9A -0.4(11) . . . . ?

C7A C8A C9A C4A 0.1(10) . . . . ?

C7A C8A C9A C10A -176.8(6) . . . . ?

C5A C4A C9A C8A 0.4(8) . . . . ?

Pd2 C4A C9A C8A 179.5(5) . . . . ?

C5A C4A C9A C10A 177.5(5) . . . . ?

Pd2 C4A C9A C10A -3.4(7) . . . . ?

C8A C9A C10A N3A -154.2(5) . . . . ?

C4A C9A C10A N3A 28.8(7) . . . . ?

C11A N3A C10A C9A 78.4(6) . . . . ?

C12A N3A C10A C9A -161.4(5) . . . . ?

Pd2 N3A C10A C9A -37.9(5) . . . . ?

A4,5. C40H56N2P2SPdCl3 (cyPd4) #\#CIF_1.1


# Created on 2010-03-02 at 11:44:22



261



# CIF files read : mau5 shelxa


data_global

#------------------ AUDIT DETAILS -------------------------------------------#











;



Glasgow G12 8QQ

Scotland UK

;




262




;




;



--#
















_journal_year ?

_journal_volume ?

_journal_issue ?


263





_publ_section_title

;

?

;


;

?

;

loop_

_publ_author_name



;



Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#


;


?

264

;


;


?

;


;


?

;


;

?

;


;

?

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;


Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.

265














The Netherlands.








266




A24, 351-359



Volume C.












34, 824-828


35, 281.


267



;


;


;


;

?

;


;




;


data_mau5




_chemical_formula_sum 'C40 H56 Cl3 N2 P2 Pd S'



268

loop_


'x, y, z'

'-x+1/2, y+1/2, -z+1/2'

'-x, -y, -z'

'x-1/2, -y-1/2, z-1/2'















_exptl_absorpt_correction_type refdelf







269












0.998


0.998
















270











loop_

_atom_type_symbol









S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


271

_atom_site_adp_type






C1CL C 0.849(3) 0.2788(9) -0.0263(6) 0.087(8) Uani 0.5 d P . .

H H 0.8319 0.3101 0.0071 0.113 Uiso 0.5 calc PR . .

Cl1 Cl 0.9374(7) 0.3396(3) -0.0739(2) 0.0898(18) Uani 0.5 d P . .

Cl2 Cl 0.6946(6) 0.2496(4) -0.0587(2) 0.0893(16) Uani 0.5 d P . .

Cl3 Cl 0.9416(10) 0.1977(4) -0.0092(4) 0.133(3) Uani 0.5 d P . .

Pd Pd 0.54668(5) 0.26097(3) 0.16827(2) 0.03897(16) Uani 1 d . . .

S S 0.7113(2) 0.33911(12) 0.12024(9) 0.0580(5) Uani 1 d . . .

C C 0.8586(10) 0.3003(6) 0.1417(4) 0.072(3) Uani 1 d . . .

N N 0.9594(10) 0.2775(8) 0.1584(7) 0.131(5) Uani 1 d . . .

P1 P 0.5158(2) 0.36290(11) 0.23438(8) 0.0451(4) Uani 1 d . . .

P2 P 0.39319(17) 0.17755(10) 0.20353(7) 0.0411(4) Uani 1 d . . .

C1P C 0.3594(8) 0.3619(5) 0.2723(3) 0.0575(19) Uani 1 d . . .

H1C1 H 0.3742 0.3925 0.3062 0.075 Uiso 1 calc R . .

H2C1 H 0.2917 0.3901 0.2501 0.075 Uiso 1 calc R . .

C2P C 0.3036(9) 0.2807(5) 0.2876(3) 0.0568(19) Uani 1 d . . .

H1C2 H 0.2283 0.2888 0.3112 0.074 Uiso 1 calc R . .

H2C2 H 0.3716 0.2512 0.3088 0.074 Uiso 1 calc R . .

C3P C 0.2574(8) 0.2294(5) 0.2378(3) 0.0546(18) Uani 1 d . . .

H1C3 H 0.2108 0.2638 0.211 0.071 Uiso 1 calc R . .

H2C3 H 0.194 0.1896 0.2502 0.071 Uiso 1 calc R . .

C1 C 0.6530(8) 0.3568(4) 0.2860(3) 0.0523(18) Uani 1 d . . .

C2 C 0.6343(13) 0.3281(7) 0.3398(4) 0.088(3) Uani 1 d . . .

H2 H 0.5483 0.3157 0.3505 0.114 Uiso 1 calc R . .

C3 C 0.7419(17) 0.3175(8) 0.3777(5) 0.115(5) Uani 1 d . . .

H3 H 0.7289 0.2982 0.4133 0.149 Uiso 1 calc R . .

C4 C 0.8724(16) 0.3376(7) 0.3599(7) 0.115(6) Uani 1 d . . .

H4 H 0.9459 0.3302 0.3841 0.15 Uiso 1 calc R . .

272

C5 C 0.8920(12) 0.3686(8) 0.3062(6) 0.098(4) Uani 1 d . . .

H5 H 0.9768 0.3829 0.2949 0.127 Uiso 1 calc R . .

C6 C 0.7792(10) 0.3772(6) 0.2706(4) 0.075(3) Uani 1 d . . .

H6 H 0.7904 0.3974 0.2351 0.097 Uiso 1 calc R . .

C7 C 0.5143(8) 0.4662(4) 0.2116(3) 0.0472(16) Uani 1 d . . .

C8 C 0.5492(8) 0.5301(5) 0.2466(4) 0.061(2) Uani 1 d . . .

H8 H 0.582 0.5195 0.2824 0.079 Uiso 1 calc R . .

C9 C 0.5359(9) 0.6102(5) 0.2288(5) 0.070(2) Uani 1 d . . .

H9 H 0.5582 0.6523 0.2528 0.091 Uiso 1 calc R . .

C10 C 0.4897(10) 0.6258(6) 0.1760(5) 0.077(3) Uani 1 d . . .

H10 H 0.4824 0.6786 0.1635 0.1 Uiso 1 calc R . .

C11 C 0.4540(11) 0.5630(6) 0.1411(4) 0.075(3) Uani 1 d . . .

H11 H 0.4206 0.5739 0.1055 0.097 Uiso 1 calc R . .

C12 C 0.4674(10) 0.4847(5) 0.1586(4) 0.065(2) Uani 1 d . . .

H12 H 0.4443 0.4431 0.1342 0.084 Uiso 1 calc R . .

C13 C 0.4605(7) 0.1105(4) 0.2573(3) 0.0463(15) Uani 1 d . . .

C14 C 0.5885(8) 0.1216(5) 0.2797(3) 0.0545(18) Uani 1 d . . .

H14 H 0.643 0.1616 0.2658 0.071 Uiso 1 calc R . .

C15 C 0.6360(9) 0.0729(6) 0.3231(4) 0.070(2) Uani 1 d . . .

H15 H 0.7212 0.0817 0.3386 0.091 Uiso 1 calc R . .

C16 C 0.5590(10) 0.0130(6) 0.3427(4) 0.068(2) Uani 1 d . . .

H16 H 0.5923 -0.0201 0.371 0.088 Uiso 1 calc R . .

C17 C 0.4286(11) 0.0006(6) 0.3203(4) 0.074(3) Uani 1 d . . .

H17 H 0.376 -0.0405 0.334 0.096 Uiso 1 calc R . .

C18 C 0.3782(9) 0.0496(5) 0.2779(3) 0.0575(19) Uani 1 d . . .

H18 H 0.2917 0.0423 0.2634 0.075 Uiso 1 calc R . .

C19 C 0.3020(7) 0.1097(5) 0.1559(3) 0.0492(16) Uani 1 d . . .

C20 C 0.1774(9) 0.1319(6) 0.1344(4) 0.069(2) Uani 1 d . . .

H20 H 0.1406 0.1815 0.143 0.09 Uiso 1 calc R . .

C21 C 0.1073(12) 0.0776(8) 0.0989(4) 0.087(3) Uani 1 d . . .

H21 H 0.0232 0.0915 0.0842 0.113 Uiso 1 calc R . .

C22 C 0.1617(13) 0.0054(8) 0.0862(4) 0.090(4) Uani 1 d . . .

H22 H 0.1138 -0.0303 0.0634 0.117 Uiso 1 calc R . .

273

C23 C 0.2864(12) -0.0154(6) 0.1067(4) 0.079(3) Uani 1 d . . .

H23 H 0.3239 -0.0643 0.0966 0.103 Uiso 1 calc R . .

C24 C 0.3570(9) 0.0358(5) 0.1421(4) 0.0581(19) Uani 1 d . . .

H24 H 0.4408 0.0209 0.1566 0.076 Uiso 1 calc R . .

N1B N 0.4088(8) 0.2787(5) 0.0698(3) 0.0613(17) Uani 1 d . . .

C1B C 0.5959(6) 0.1665(4) 0.1193(3) 0.0414(14) Uani 1 d . . .

C2B C 0.6887(8) 0.1086(4) 0.1373(3) 0.0533(17) Uani 1 d . . .

H2B H 0.7282 0.1131 0.1726 0.069 Uiso 1 calc R . .

C3B C 0.7234(8) 0.0450(5) 0.1043(4) 0.061(2) Uani 1 d . . .

H3B H 0.7851 0.0073 0.1178 0.079 Uiso 1 calc R . .

C4B C 0.6685(10) 0.0363(5) 0.0519(4) 0.069(2) Uani 1 d . . .

H4B H 0.6915 -0.0072 0.0299 0.09 Uiso 1 calc R . .

C5B C 0.5777(9) 0.0938(5) 0.0324(4) 0.064(2) Uani 1 d . . .

H5B H 0.5411 0.0895 -0.0034 0.083 Uiso 1 calc R . .

C6B C 0.5408(8) 0.1580(4) 0.0658(3) 0.0504(16) Uani 1 d . . .

C7B C 0.4504(9) 0.2177(6) 0.0433(3) 0.061(2) Uani 1 d . . .

H7B H 0.4198 0.2114 0.0068 0.079 Uiso 1 calc R . .

C8B C 0.3374(10) 0.3421(7) 0.0428(4) 0.071(2) Uani 1 d . . .

C9B C 0.3943(15) 0.3863(8) 0.0029(5) 0.114(5) Uani 1 d . . .

H9B H 0.4815 0.3763 -0.0074 0.148 Uiso 1 calc R . .

C10B C 0.3160(15) 0.4489(8) -0.0229(6) 0.110(4) Uani 1 d . . .

H10B H 0.3459 0.4716 -0.0554 0.143 Uiso 1 calc R . .

C11B C 0.2066(15) 0.4755(9) -0.0033(5) 0.111(5) Uani 1 d . . .

H11B H 0.1655 0.5217 -0.0174 0.145 Uiso 1 calc R . .

C12B C 0.1511(13) 0.4314(11) 0.0407(5) 0.119(6) Uani 1 d . . .

H12B H 0.0708 0.4486 0.0549 0.155 Uiso 1 calc R . .

C13B C 0.2112(10) 0.3653(8) 0.0624(4) 0.085(3) Uani 1 d . . .

H13B H 0.1706 0.3355 0.0897 0.11 Uiso 1 calc R . .

loop_




274





C1CL 0.20(3) 0.029(7) 0.030(7) -0.008(5) 0.029(10) 0.003(10)

Cl1 0.143(5) 0.059(3) 0.069(3) -0.001(2) 0.022(3) -0.043(3)

Cl2 0.092(4) 0.092(4) 0.085(3) 0.023(3) 0.021(3) -0.007(3)

Cl3 0.171(8) 0.082(4) 0.143(6) 0.035(4) -0.028(6) 0.022(5)

Pd 0.0410(3) 0.0331(2) 0.0431(3) 0.0006(2) 0.00498(18) -0.0005(2)

S 0.0557(11) 0.0497(10) 0.0689(12) 0.0110(9) 0.0068(9) -0.0091(8)

C 0.060(5) 0.055(5) 0.102(7) -0.009(5) 0.025(5) -0.001(4)

N 0.049(5) 0.126(10) 0.220(15) -0.001(9) 0.024(7) 0.023(6)

P1 0.0537(10) 0.0360(9) 0.0459(9) -0.0026(7) 0.0058(8) 0.0024(7)

P2 0.0399(9) 0.0370(8) 0.0468(9) 0.0037(7) 0.0049(7) -0.0019(6)

C1P 0.060(5) 0.053(4) 0.060(4) -0.008(4) 0.014(4) 0.004(4)

C2P 0.066(5) 0.047(4) 0.059(4) -0.003(3) 0.022(4) -0.001(3)

C3P 0.050(4) 0.049(4) 0.066(5) 0.000(3) 0.013(3) 0.000(3)

C1 0.065(5) 0.043(4) 0.048(4) -0.006(3) -0.011(3) 0.008(3)

C2 0.102(8) 0.084(7) 0.076(6) 0.006(5) -0.018(6) -0.023(6)

C3 0.159(14) 0.096(9) 0.086(8) 0.020(7) -0.057(9) -0.013(9)

C4 0.131(12) 0.071(7) 0.138(12) -0.013(7) -0.078(10) 0.020(7)

C5 0.083(8) 0.098(9) 0.111(9) -0.041(7) -0.028(7) 0.017(6)

C6 0.072(6) 0.082(6) 0.069(6) -0.014(5) -0.008(5) 0.019(5)

C7 0.058(4) 0.033(3) 0.052(4) -0.002(3) 0.009(3) 0.006(3)

C8 0.056(5) 0.058(5) 0.068(5) -0.008(4) 0.000(4) 0.008(4)

C9 0.060(5) 0.039(4) 0.112(8) -0.009(4) 0.009(5) 0.002(4)

C10 0.069(6) 0.047(5) 0.117(9) 0.012(5) 0.029(6) 0.012(4)

C11 0.089(7) 0.064(6) 0.072(6) 0.024(5) 0.010(5) 0.022(5)

C12 0.082(6) 0.044(4) 0.067(5) 0.001(4) 0.004(4) 0.004(4)

C13 0.048(4) 0.046(4) 0.045(4) 0.003(3) 0.000(3) 0.002(3)

C14 0.053(4) 0.055(4) 0.055(4) 0.010(3) 0.004(3) -0.001(3)

C15 0.057(5) 0.084(7) 0.069(5) 0.016(5) 0.009(4) 0.011(5)

C16 0.077(6) 0.075(6) 0.051(4) 0.011(4) -0.002(4) 0.022(5)

275

C17 0.101(8) 0.057(5) 0.065(5) 0.023(4) 0.012(5) -0.004(5)

C18 0.059(5) 0.050(4) 0.063(5) 0.015(4) 0.000(4) -0.005(3)

C19 0.046(4) 0.053(4) 0.049(4) 0.003(3) 0.004(3) -0.006(3)

C20 0.054(5) 0.079(6) 0.073(6) 0.007(5) -0.006(4) -0.005(4)

C21 0.079(7) 0.103(9) 0.078(7) 0.002(6) -0.023(5) -0.025(6)

C22 0.097(8) 0.104(9) 0.068(6) -0.008(6) -0.008(6) -0.053(7)

C23 0.097(8) 0.068(6) 0.074(6) -0.017(5) 0.018(5) -0.027(5)

C24 0.054(4) 0.048(4) 0.072(5) -0.007(4) 0.001(4) -0.011(3)

N1B 0.070(5) 0.065(4) 0.049(4) -0.008(3) 0.000(3) 0.009(3)

C1B 0.040(3) 0.030(3) 0.055(4) -0.002(3) 0.009(3) -0.003(2)

C2B 0.057(4) 0.044(4) 0.059(4) 0.000(3) 0.004(3) 0.006(3)

C3B 0.053(5) 0.049(4) 0.082(6) -0.002(4) 0.017(4) 0.004(3)

C4B 0.086(6) 0.045(4) 0.078(6) -0.016(4) 0.025(5) -0.001(4)

C5B 0.076(6) 0.063(5) 0.053(4) -0.016(4) 0.010(4) -0.005(4)

C6B 0.062(4) 0.044(4) 0.046(4) -0.003(3) 0.013(3) -0.007(3)

C7B 0.061(5) 0.076(6) 0.045(4) -0.006(4) 0.001(3) -0.011(4)

C8B 0.073(6) 0.088(7) 0.050(4) -0.009(4) -0.008(4) 0.019(5)

C9B 0.138(11) 0.098(9) 0.110(9) 0.055(7) 0.064(8) 0.052(8)

C10B 0.108(10) 0.104(10) 0.118(10) 0.027(8) 0.004(8) 0.034(8)

C11B 0.123(11) 0.122(11) 0.088(9) -0.016(8) -0.015(8) 0.058(9)

C12B 0.088(8) 0.188(16) 0.082(8) -0.022(9) 0.001(7) 0.063(10)

C13B 0.062(6) 0.134(10) 0.058(5) 0.003(6) 0.007(4) 0.033(6)



;






276


;

loop_



_geom_bond_distance



C1CL Cl3 1.68(2) . ?

C1CL Cl2 1.77(3) . ?

C1CL Cl1 1.786(19) . ?

Pd C1B 2.035(6) . ?

Pd P2 2.2562(17) . ?

Pd P1 2.3541(18) . ?

Pd S 2.423(2) . ?

S C 1.673(10) . ?

C N 1.136(14) . ?

P1 C7 1.801(7) . ?

P1 C1 1.824(8) . ?

P1 C1P 1.840(8) . ?

P2 C13 1.821(7) . ?

P2 C19 1.829(8) . ?

P2 C3P 1.831(8) . ?

C1P C2P 1.510(11) . ?

C2P C3P 1.530(11) . ?

C1 C6 1.371(13) . ?

C1 C2 1.402(13) . ?

C2 C3 1.399(16) . ?

C3 C4 1.43(2) . ?

C4 C5 1.42(2) . ?

C5 C6 1.401(14) . ?

C7 C12 1.381(11) . ?

C7 C8 1.394(11) . ?

277

C8 C9 1.402(12) . ?

C9 C10 1.366(15) . ?

C10 C11 1.378(15) . ?

C11 C12 1.373(12) . ?

C13 C14 1.384(10) . ?

C13 C18 1.405(10) . ?

C14 C15 1.392(11) . ?

C15 C16 1.355(13) . ?

C16 C17 1.408(14) . ?

C17 C18 1.388(11) . ?

C19 C20 1.382(11) . ?

C19 C24 1.390(11) . ?

C20 C21 1.412(14) . ?

C21 C22 1.355(17) . ?

C22 C23 1.369(17) . ?

C23 C24 1.381(12) . ?

N1B C7B 1.276(11) . ?

N1B C8B 1.417(12) . ?

C1B C2B 1.394(10) . ?

C1B C6B 1.395(10) . ?

C2B C3B 1.375(11) . ?

C3B C4B 1.367(13) . ?

C4B C5B 1.388(13) . ?

C5B C6B 1.393(11) . ?

C6B C7B 1.435(12) . ?

C8B C9B 1.351(14) . ?

C8B C13B 1.417(13) . ?

C9B C10B 1.431(16) . ?

C10B C11B 1.285(18) . ?

C11B C12B 1.42(2) . ?

C12B C13B 1.347(18) . ?

278

loop_




_geom_angle




Cl3 C1CL Cl2 110.7(10) . . ?

Cl3 C1CL Cl1 109.3(14) . . ?

Cl2 C1CL Cl1 108.3(10) . . ?

C1B Pd P2 85.86(18) . . ?

C1B Pd P1 171.2(2) . . ?

P2 Pd P1 94.46(7) . . ?

C1B Pd S 87.27(18) . . ?

P2 Pd S 172.66(7) . . ?

P1 Pd S 92.72(7) . . ?

C S Pd 104.5(3) . . ?

N C S 176.0(11) . . ?

C7 P1 C1 105.1(4) . . ?

C7 P1 C1P 99.4(4) . . ?

C1 P1 C1P 106.9(4) . . ?

C7 P1 Pd 118.5(2) . . ?

C1 P1 Pd 108.1(2) . . ?

C1P P1 Pd 117.8(3) . . ?

C13 P2 C19 103.6(3) . . ?

C13 P2 C3P 103.0(4) . . ?

C19 P2 C3P 102.3(4) . . ?

C13 P2 Pd 113.9(2) . . ?

C19 P2 Pd 118.1(2) . . ?

C3P P2 Pd 114.0(3) . . ?

C2P C1P P1 117.2(6) . . ?

C1P C2P C3P 114.2(7) . . ?

279

C2P C3P P2 114.1(6) . . ?

C6 C1 C2 119.4(8) . . ?

C6 C1 P1 118.5(6) . . ?

C2 C1 P1 122.0(7) . . ?

C3 C2 C1 121.6(12) . . ?

C2 C3 C4 117.6(12) . . ?

C5 C4 C3 121.2(11) . . ?

C6 C5 C4 117.7(13) . . ?

C1 C6 C5 122.4(11) . . ?

C12 C7 C8 117.6(7) . . ?

C12 C7 P1 119.6(6) . . ?

C8 C7 P1 122.7(6) . . ?

C7 C8 C9 121.1(9) . . ?

C10 C9 C8 119.4(9) . . ?

C9 C10 C11 119.9(9) . . ?

C12 C11 C10 120.6(9) . . ?

C11 C12 C7 121.4(9) . . ?

C14 C13 C18 120.2(7) . . ?

C14 C13 P2 120.7(6) . . ?

C18 C13 P2 119.1(6) . . ?

C13 C14 C15 120.2(8) . . ?

C16 C15 C14 120.4(9) . . ?

C15 C16 C17 120.2(8) . . ?

C18 C17 C16 120.3(9) . . ?

C17 C18 C13 118.7(8) . . ?

C20 C19 C24 120.2(8) . . ?

C20 C19 P2 119.7(7) . . ?

C24 C19 P2 120.1(6) . . ?

C19 C20 C21 118.7(10) . . ?

C22 C21 C20 120.5(10) . . ?

C21 C22 C23 120.6(10) . . ?

C22 C23 C24 120.5(11) . . ?

C23 C24 C19 119.6(9) . . ?

280

C7B N1B C8B 121.8(7) . . ?

C2B C1B C6B 117.1(7) . . ?

C2B C1B Pd 121.5(5) . . ?

C6B C1B Pd 121.4(5) . . ?

C3B C2B C1B 121.9(8) . . ?

C4B C3B C2B 121.0(8) . . ?

C3B C4B C5B 118.5(8) . . ?

C4B C5B C6B 120.9(8) . . ?

C5B C6B C1B 120.6(8) . . ?

C5B C6B C7B 119.1(7) . . ?

C1B C6B C7B 120.2(7) . . ?

N1B C7B C6B 124.8(7) . . ?

C9B C8B C13B 119.5(10) . . ?

C9B C8B N1B 120.9(9) . . ?

C13B C8B N1B 119.2(9) . . ?

C8B C9B C10B 117.9(12) . . ?

C11B C10B C9B 123.2(14) . . ?

C10B C11B C12B 117.3(13) . . ?

C13B C12B C11B 122.0(11) . . ?

C12B C13B C8B 118.8(12) . . ?

A4,6- C36H34N6Pd2 (cyPd5) #\#CIF_1.1


# Created on 2010-03-02 at 14:49:24





# CIF files read : m26 struct

281


data_global

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Glasgow G12 8QQ

Scotland UK

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Glasgow G12 8QQ

Scotland UK

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284

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Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.




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The Netherlands.










286


A24, 351-359



Volume C.












34, 824-828


35, 281.




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data_m26








_symmetry_cell_setting triclinic

_symmetry_space_group_name_H-M 'P -1'

288

loop_


'x, y, z'

'-x, -y, -z'




_cell_angle_alpha 101.319(12)


_cell_angle_gamma 105.416(11)



















289
















0.998


0.998












290



















loop_

_atom_type_symbol









loop_

_atom_site_label

291


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type






Pd1 Pd 0.33056(4) 0.09336(3) 0.65348(2) 0.05085(12) Uani 1 d . . .

Pd2 Pd 0.21674(4) 0.09463(3) 0.84709(3) 0.05373(13) Uani 1 d . . .

N1 N 0.3896(4) -0.0107(3) 0.7321(3) 0.0547(10) Uani 1 d . . .

N2 N 0.3315(4) -0.0210(3) 0.8104(3) 0.0543(10) Uani 1 d . . .

N3 N 0.0299(5) -0.0287(5) 0.8350(3) 0.0730(13) Uani 1 d . . .

C3 C 0.3835(6) -0.0926(5) 0.8529(4) 0.0632(13) Uani 1 d . . .

C4 C 0.4763(7) -0.1284(5) 0.8018(4) 0.0767(17) Uani 1 d . . .

H4 H 0.5264 -0.179 0.8154 0.092 Uiso 1 calc R . .

C5 C 0.4786(6) -0.0738(5) 0.7270(4) 0.0668(14) Uani 1 d . . .

C6 C 0.3373(7) -0.1230(6) 0.9403(4) 0.0854(19) Uani 1 d . . .

H61 H 0.2943 -0.0667 0.9679 0.111 Uiso 1 calc R . .

H62 H 0.4154 -0.1207 0.9863 0.111 Uiso 1 calc R . .

H63 H 0.2726 -0.2011 0.9229 0.111 Uiso 1 calc R . .

C7 C 0.5607(7) -0.0749(7) 0.6498(5) 0.091(2) Uani 1 d . . .

H71 H 0.5072 -0.1336 0.5929 0.119 Uiso 1 calc R . .

H72 H 0.6433 -0.0935 0.6711 0.119 Uiso 1 calc R . .

H73 H 0.5845 0.0017 0.6359 0.119 Uiso 1 calc R . .

C8 C 0.0000(6) -0.1528(6) 0.8088(4) 0.0802(18) Uani 1 d . . .

C9 C 0.0402(7) -0.2035(6) 0.7284(5) 0.0821(18) Uani 1 d . . .

H9 H 0.0863 -0.1551 0.6932 0.098 Uiso 1 calc R . .

C10 C 0.0134(8) -0.3244(7) 0.6990(6) 0.105(2) Uani 1 d . . .

H10 H 0.0393 -0.3582 0.644 0.126 Uiso 1 calc R . .

292

C11 C -0.0521(11) -0.3932(8) 0.7528(9) 0.139(4) Uani 1 d . . .

H11 H -0.0695 -0.4749 0.7346 0.167 Uiso 1 calc R . .

C12 C -0.0938(10) -0.3432(8) 0.8351(8) 0.143(4) Uani 1 d . . .

H12 H -0.138 -0.3916 0.871 0.172 Uiso 1 calc R . .

C13 C -0.0692(8) -0.2242(8) 0.8619(5) 0.114(3) Uani 1 d . . .

H13 H -0.0985 -0.1906 0.9154 0.136 Uiso 1 calc R . .

C14 C -0.0668(7) 0.0195(8) 0.8518(4) 0.094(2) Uani 1 d . . .

H14 H -0.1557 -0.027 0.8497 0.113 Uiso 1 calc R . .

C15 C -0.0315(7) 0.1466(7) 0.8736(4) 0.0811(18) Uani 1 d . . .

C16 C 0.1076(6) 0.2058(6) 0.8767(4) 0.0690(15) Uani 1 d . . .

C17 C 0.1448(7) 0.3278(6) 0.8936(4) 0.0807(18) Uani 1 d . . .

H17 H 0.2356 0.3697 0.8958 0.097 Uiso 1 calc R . .

C18 C 0.0512(10) 0.3889(8) 0.9073(5) 0.111(3) Uani 1 d . . .

H18 H 0.0791 0.4711 0.9186 0.133 Uiso 1 calc R . .

C19 C -0.0853(11) 0.3281(11) 0.9043(6) 0.133(4) Uani 1 d . . .

H19 H -0.1484 0.3697 0.914 0.159 Uiso 1 calc R . .

C20 C -0.1259(8) 0.2092(10) 0.8875(5) 0.110(3) Uani 1 d . . .

H20 H -0.2173 0.1687 0.8852 0.132 Uiso 1 calc R . .

N1A N 0.4338(4) 0.2331(3) 0.7742(3) 0.0575(10) Uani 1 d . . .

N2A N 0.3902(4) 0.2269(3) 0.8575(3) 0.0548(10) Uani 1 d . . .

N3A N 0.2541(4) 0.1851(4) 0.5644(3) 0.0601(10) Uani 1 d . . .

C3A C 0.4760(6) 0.3134(5) 0.9295(4) 0.0669(15) Uani 1 d . . .

C5A C 0.5498(5) 0.3241(5) 0.7946(5) 0.0686(15) Uani 1 d . . .

C4A C 0.5779(6) 0.3769(5) 0.8900(5) 0.0803(18) Uani 1 d . . .

H4A H 0.6515 0.4431 0.9227 0.096 Uiso 1 calc R . .

C6A C 0.4564(7) 0.3268(6) 1.0296(4) 0.087(2) Uani 1 d . . .

H61A H 0.3654 0.2797 1.0302 0.113 Uiso 1 calc R . .

H62A H 0.468 0.4086 1.058 0.113 Uiso 1 calc R . .

H63A H 0.5232 0.3009 1.0658 0.113 Uiso 1 calc R . .

C7A C 0.6223(7) 0.3529(7) 0.7167(6) 0.106(2) Uani 1 d . . .

H71A H 0.6073 0.4231 0.7016 0.138 Uiso 1 calc R . .

H72A H 0.5872 0.288 0.6607 0.138 Uiso 1 calc R . .

H73A H 0.7191 0.3663 0.7376 0.138 Uiso 1 calc R . .

293

C8A C 0.2769(6) 0.3106(5) 0.5824(5) 0.0697(15) Uani 1 d . . .

C9A C 0.2719(6) 0.3739(5) 0.6707(5) 0.0780(17) Uani 1 d . . .

H9A H 0.255 0.3349 0.7191 0.094 Uiso 1 calc R . .

C10A C 0.2917(8) 0.4943(6) 0.6887(6) 0.100(2) Uani 1 d . . .

H10A H 0.2861 0.5361 0.7483 0.121 Uiso 1 calc R . .

C11A C 0.3192(10) 0.5507(7) 0.6192(9) 0.130(3) Uani 1 d . . .

H11A H 0.3345 0.6322 0.6319 0.156 Uiso 1 calc R . .

C12A C 0.3252(10) 0.4896(8) 0.5284(8) 0.126(3) Uani 1 d . . .

H12A H 0.3432 0.53 0.481 0.151 Uiso 1 calc R . .

C13A C 0.3043(8) 0.3690(6) 0.5095(6) 0.097(2) Uani 1 d . . .

H13A H 0.3084 0.3271 0.4495 0.116 Uiso 1 calc R . .

C14A C 0.1764(5) 0.1174(5) 0.4853(4) 0.0643(14) Uani 1 d . . .

H14A H 0.1332 0.1486 0.4405 0.077 Uiso 1 calc R . .

C15A C 0.1577(5) -0.0081(5) 0.4675(3) 0.0613(13) Uani 1 d . . .

C16A C 0.2280(5) -0.0421(4) 0.5427(3) 0.0555(12) Uani 1 d . . .

C17A C 0.2131(6) -0.1616(5) 0.5282(4) 0.0711(15) Uani 1 d . . .

H17A H 0.2559 -0.1882 0.5766 0.085 Uiso 1 calc R . .

C18A C 0.1364(7) -0.2437(6) 0.4442(4) 0.0794(17) Uani 1 d . . .

H18A H 0.1293 -0.3236 0.4367 0.095 Uiso 1 calc R . .

C19A C 0.0711(6) -0.2067(6) 0.3721(4) 0.0843(19) Uani 1 d . . .

H19A H 0.0206 -0.2612 0.3155 0.101 Uiso 1 calc R . .

C20A C 0.0807(6) -0.0891(6) 0.3841(4) 0.0708(15) Uani 1 d . . .

H20A H 0.0353 -0.0639 0.3359 0.085 Uiso 1 calc R . .

loop_








Pd1 0.0478(2) 0.0558(2) 0.0485(2) 0.01727(17) 0.01308(16) 0.01006(17)

294

Pd2 0.0520(2) 0.0628(3) 0.0464(2) 0.01335(17) 0.01334(17) 0.01571(19)

N1 0.055(2) 0.056(2) 0.052(2) 0.0147(18) 0.0104(19) 0.014(2)

N2 0.057(2) 0.056(2) 0.049(2) 0.0142(18) 0.0139(19) 0.0143(19)

N3 0.056(3) 0.096(4) 0.058(3) 0.021(3) 0.019(2) 0.003(3)

C3 0.072(4) 0.063(3) 0.060(3) 0.022(3) 0.014(3) 0.024(3)

C4 0.089(4) 0.080(4) 0.079(4) 0.030(3) 0.022(3) 0.044(4)

C5 0.061(3) 0.078(4) 0.072(4) 0.024(3) 0.020(3) 0.031(3)

C6 0.104(5) 0.103(5) 0.078(4) 0.050(4) 0.038(4) 0.047(4)

C7 0.087(5) 0.121(6) 0.086(4) 0.032(4) 0.041(4) 0.047(4)

C8 0.064(4) 0.092(5) 0.068(4) 0.036(3) 0.006(3) -0.012(3)

C9 0.075(4) 0.079(4) 0.079(4) 0.028(3) 0.011(3) -0.002(3)

C10 0.099(5) 0.086(5) 0.101(5) 0.011(4) 0.010(4) -0.005(4)

C11 0.142(8) 0.083(6) 0.158(9) 0.041(6) 0.012(7) -0.020(5)

C12 0.151(9) 0.107(7) 0.133(8) 0.059(6) 0.023(7) -0.044(6)

C13 0.105(6) 0.118(6) 0.083(5) 0.032(4) 0.019(4) -0.028(5)

C14 0.054(4) 0.159(7) 0.066(4) 0.041(4) 0.016(3) 0.016(4)

C15 0.068(4) 0.127(6) 0.059(3) 0.022(4) 0.022(3) 0.042(4)

C16 0.070(4) 0.101(5) 0.042(3) 0.011(3) 0.013(2) 0.040(3)

C17 0.089(5) 0.098(5) 0.061(3) 0.000(3) 0.012(3) 0.054(4)

C18 0.132(7) 0.136(7) 0.075(4) -0.006(4) 0.001(5) 0.093(6)

C19 0.136(8) 0.216(11) 0.074(5) 0.002(6) 0.015(5) 0.126(9)

C20 0.086(5) 0.200(10) 0.063(4) 0.019(5) 0.029(4) 0.077(6)

N1A 0.049(2) 0.053(2) 0.062(3) 0.0127(19) 0.0051(19) 0.0063(19)

N2A 0.052(2) 0.050(2) 0.055(2) 0.0081(19) 0.0007(19) 0.0114(19)

N3A 0.057(3) 0.068(3) 0.062(3) 0.026(2) 0.021(2) 0.018(2)

C3A 0.069(4) 0.063(3) 0.067(3) 0.002(3) -0.009(3) 0.038(3)

C5A 0.048(3) 0.059(3) 0.091(4) 0.020(3) 0.005(3) 0.006(3)

C4A 0.054(3) 0.056(3) 0.109(5) -0.003(3) -0.009(3) 0.010(3)

C6A 0.099(5) 0.087(4) 0.068(4) -0.002(3) -0.010(3) 0.047(4)

C7A 0.068(4) 0.106(5) 0.128(6) 0.039(5) 0.026(4) -0.010(4)

C8A 0.060(3) 0.069(4) 0.085(4) 0.032(3) 0.015(3) 0.018(3)

C9A 0.072(4) 0.069(4) 0.086(4) 0.017(3) 0.003(3) 0.018(3)

C10A 0.114(6) 0.072(5) 0.113(6) 0.015(4) 0.012(5) 0.036(4)

295

C11A 0.135(8) 0.061(5) 0.194(11) 0.041(6) 0.024(7) 0.026(5)

C12A 0.143(8) 0.099(6) 0.155(9) 0.069(6) 0.042(7) 0.038(6)

C13A 0.110(6) 0.091(5) 0.115(6) 0.055(4) 0.047(5) 0.037(4)

C14A 0.059(3) 0.086(4) 0.056(3) 0.030(3) 0.015(3) 0.023(3)

C15A 0.053(3) 0.087(4) 0.046(3) 0.017(3) 0.018(2) 0.020(3)

C16A 0.055(3) 0.062(3) 0.047(3) 0.012(2) 0.019(2) 0.011(2)

C17A 0.080(4) 0.065(4) 0.061(3) 0.010(3) 0.018(3) 0.013(3)

C18A 0.082(4) 0.071(4) 0.071(4) 0.000(3) 0.017(3) 0.011(3)

C19A 0.070(4) 0.097(5) 0.059(4) -0.010(3) 0.013(3) 0.000(4)

C20A 0.065(4) 0.098(5) 0.044(3) 0.010(3) 0.011(2) 0.020(3)



;







;

loop_



_geom_bond_distance



Pd1 C16A 1.985(5) . ?

Pd1 N1 2.005(4) . ?

Pd1 N3A 2.063(4) . ?

Pd1 N1A 2.098(4) . ?

296

Pd1 Pd2 3.1921(7) . ?

Pd2 C16 1.989(6) . ?

Pd2 N2A 2.018(4) . ?

Pd2 N3 2.056(5) . ?

Pd2 N2 2.094(4) . ?

N1 C5 1.339(6) . ?

N1 N2 1.368(5) . ?

N2 C3 1.334(6) . ?

N3 C14 1.308(8) . ?

N3 C8 1.407(8) . ?

C3 C4 1.394(8) . ?

C3 C6 1.493(8) . ?

C4 C5 1.376(8) . ?

C5 C7 1.495(8) . ?

C8 C9 1.378(9) . ?

C8 C13 1.390(8) . ?

C9 C10 1.376(9) . ?

C10 C11 1.364(11) . ?

C11 C12 1.405(13) . ?

C12 C13 1.356(12) . ?

C14 C15 1.437(10) . ?

C15 C20 1.394(10) . ?

C15 C16 1.410(9) . ?

C16 C17 1.381(8) . ?

C17 C18 1.373(9) . ?

C18 C19 1.391(13) . ?

C19 C20 1.344(12) . ?

N1A C5A 1.340(6) . ?

N1A N2A 1.355(6) . ?

N2A C3A 1.335(6) . ?

N3A C14A 1.284(6) . ?

N3A C8A 1.433(7) . ?

C3A C4A 1.389(9) . ?

297

C3A C6A 1.479(8) . ?

C5A C4A 1.359(9) . ?

C5A C7A 1.486(9) . ?

C8A C9A 1.372(8) . ?

C8A C13A 1.402(8) . ?

C9A C10A 1.378(9) . ?

C10A C11A 1.345(12) . ?

C11A C12A 1.397(13) . ?

C12A C13A 1.379(10) . ?

C14A C15A 1.440(8) . ?

C15A C20A 1.379(7) . ?

C15A C16A 1.411(7) . ?

C16A C17A 1.379(7) . ?

C17A C18A 1.389(7) . ?

C18A C19A 1.374(9) . ?

C19A C20A 1.371(8) . ?

loop_




_geom_angle




C16A Pd1 N1 93.33(19) . . ?

C16A Pd1 N3A 81.2(2) . . ?

N1 Pd1 N3A 174.13(17) . . ?

C16A Pd1 N1A 177.60(18) . . ?

N1 Pd1 N1A 85.37(16) . . ?

N3A Pd1 N1A 100.06(17) . . ?

C16A Pd1 Pd2 115.73(13) . . ?

N1 Pd1 Pd2 64.89(12) . . ?

298

N3A Pd1 Pd2 115.67(12) . . ?

N1A Pd1 Pd2 61.89(12) . . ?

C16 Pd2 N2A 93.1(2) . . ?

C16 Pd2 N3 81.7(2) . . ?

N2A Pd2 N3 174.53(19) . . ?

C16 Pd2 N2 177.68(18) . . ?

N2A Pd2 N2 86.22(16) . . ?

N3 Pd2 N2 98.89(19) . . ?

C16 Pd2 Pd1 115.61(16) . . ?

N2A Pd2 Pd1 65.02(12) . . ?

N3 Pd2 Pd1 115.66(13) . . ?

N2 Pd2 Pd1 62.10(11) . . ?

C5 N1 N2 109.6(4) . . ?

C5 N1 Pd1 134.1(4) . . ?

N2 N1 Pd1 116.3(3) . . ?

C3 N2 N1 107.3(4) . . ?

C3 N2 Pd2 135.6(4) . . ?

N1 N2 Pd2 116.1(3) . . ?

C14 N3 C8 120.5(6) . . ?

C14 N3 Pd2 112.8(5) . . ?

C8 N3 Pd2 126.6(4) . . ?

N2 C3 C4 109.0(5) . . ?

N2 C3 C6 119.9(5) . . ?

C4 C3 C6 131.1(5) . . ?

C5 C4 C3 106.2(5) . . ?

N1 C5 C4 107.9(5) . . ?

N1 C5 C7 120.9(5) . . ?

C4 C5 C7 131.2(6) . . ?

C9 C8 C13 119.9(7) . . ?

C9 C8 N3 118.7(5) . . ?

C13 C8 N3 121.4(7) . . ?

C10 C9 C8 121.3(6) . . ?

C11 C10 C9 118.2(8) . . ?

299

C10 C11 C12 121.4(9) . . ?

C13 C12 C11 119.7(8) . . ?

C12 C13 C8 119.5(8) . . ?

N3 C14 C15 117.9(6) . . ?

C20 C15 C16 121.1(8) . . ?

C20 C15 C14 123.9(7) . . ?

C16 C15 C14 114.9(6) . . ?

C17 C16 C15 116.8(6) . . ?

C17 C16 Pd2 130.4(5) . . ?

C15 C16 Pd2 112.6(5) . . ?

C18 C17 C16 121.8(8) . . ?

C17 C18 C19 120.1(9) . . ?

C20 C19 C18 120.0(8) . . ?

C19 C20 C15 120.2(8) . . ?

C5A N1A N2A 107.5(4) . . ?

C5A N1A Pd1 134.7(4) . . ?

N2A N1A Pd1 117.0(3) . . ?

C3A N2A N1A 109.8(4) . . ?

C3A N2A Pd2 134.5(4) . . ?

N1A N2A Pd2 115.7(3) . . ?

C14A N3A C8A 119.4(5) . . ?

C14A N3A Pd1 113.1(4) . . ?

C8A N3A Pd1 127.5(4) . . ?

N2A C3A C4A 106.7(5) . . ?

N2A C3A C6A 121.9(6) . . ?

C4A C3A C6A 131.3(6) . . ?

N1A C5A C4A 108.8(6) . . ?

N1A C5A C7A 119.9(6) . . ?

C4A C5A C7A 131.3(6) . . ?

C5A C4A C3A 107.2(5) . . ?

C9A C8A C13A 119.8(6) . . ?

C9A C8A N3A 120.3(5) . . ?

C13A C8A N3A 119.9(6) . . ?

300

C8A C9A C10A 121.0(7) . . ?

C11A C10A C9A 119.4(8) . . ?

C10A C11A C12A 121.4(8) . . ?

C13A C12A C11A 119.5(8) . . ?

C12A C13A C8A 118.9(8) . . ?

N3A C14A C15A 118.5(5) . . ?

C20A C15A C16A 122.1(5) . . ?

C20A C15A C14A 123.8(5) . . ?

C16A C15A C14A 114.1(5) . . ?

C17A C16A C15A 115.9(5) . . ?

C17A C16A Pd1 131.0(4) . . ?

C15A C16A Pd1 113.1(4) . . ?

C16A C17A C18A 122.5(6) . . ?

C19A C18A C17A 119.8(6) . . ?

C20A C19A C18A 119.8(5) . . ?

C19A C20A C15A 119.9(6) . . ?

A4,7- C32H26N6Pd2 (cyPd6) #\#CIF_1.1


# Created on 2010-03-02 at 15:21:57





# CIF files read : mau3ad struct


data_global

301

#------------------ AUDIT DETAILS -------------------------------------------#











;



Glasgow G12 8QQ

Scotland UK

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302


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--#
















_journal_year ?

_journal_volume ?

_journal_issue ?






_publ_section_title

303

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loop_

_publ_author_name



;



Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#


;


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;


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;

304


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?

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;

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Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.






305









The Netherlands.











A24, 351-359

306



Volume C.












34, 824-828


35, 281.




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307

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;


data_mau3ad









_symmetry_space_group_name_H-M 'P 1 21/n 1'

loop_


'x, y, z'

308

'-x+1/2, y+1/2, -z+1/2'

'-x, -y, -z'

'x-1/2, -y-1/2, z-1/2'


























309





_diffrn_reflns_limit_h_min 0










0.96


0.96













310







Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^














loop_

_atom_type_symbol









311

loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type






Pd1 Pd 0.73709(4) 0.19886(5) 0.35932(2) 0.04832(17) Uani 1 d . . .

Pd2 Pd 0.46945(4) 0.14688(5) 0.34789(3) 0.04984(17) Uani 1 d . . .

N1 N 0.6239(5) 0.3332(5) 0.3581(3) 0.0533(14) Uani 1 d . . .

N2 N 0.5134(5) 0.3103(5) 0.3483(3) 0.0543(14) Uani 1 d . . .

N1A N 0.6522(5) 0.1530(5) 0.2706(3) 0.0557(14) Uani 1 d . . .

N2A N 0.5417(5) 0.1328(5) 0.2617(3) 0.0568(15) Uani 1 d . . .

C2 C 0.6355(7) 0.4469(7) 0.3559(3) 0.0615(19) Uani 1 d . . .

H2 H 0.7032 0.4851 0.362 0.08 Uiso 1 calc R . .

C3 C 0.5339(8) 0.4981(7) 0.3433(4) 0.069(2) Uani 1 d . . .

H3 H 0.5182 0.5756 0.3387 0.09 Uiso 1 calc R . .

C4 C 0.4602(7) 0.4097(7) 0.3389(3) 0.065(2) Uani 1 d . . .

H4 H 0.3832 0.4178 0.3306 0.085 Uiso 1 calc R . .

C2A C 0.6814(7) 0.1447(7) 0.2114(4) 0.068(2) Uani 1 d . . .

H2A H 0.7532 0.1546 0.2035 0.088 Uiso 1 calc R . .

C3A C 0.5902(7) 0.1194(7) 0.1640(4) 0.072(2) Uani 1 d . . .

H3A H 0.5877 0.1083 0.119 0.094 Uiso 1 calc R . .

C4A C 0.5037(7) 0.1140(6) 0.1977(4) 0.064(2) Uani 1 d . . .

H4A H 0.4299 0.0995 0.1788 0.083 Uiso 1 calc R . .

N3 N 0.8343(5) 0.2410(5) 0.4469(3) 0.0515(14) Uani 1 d . . .

N3A N 0.4181(4) -0.0174(5) 0.3543(3) 0.0533(14) Uani 1 d . . .

312

C5 C 0.8530(6) 0.0810(6) 0.3619(3) 0.0522(17) Uani 1 d . . .

C6 C 0.8613(6) -0.0101(6) 0.3195(3) 0.0560(17) Uani 1 d . . .

H6 H 0.8029 -0.0257 0.2848 0.073 Uiso 1 calc R . .

C7 C 0.9571(7) -0.0781(7) 0.3287(4) 0.070(2) Uani 1 d . . .

H7 H 0.962 -0.1373 0.2993 0.09 Uiso 1 calc R . .

C8 C 1.0436(7) -0.0590(7) 0.3800(4) 0.072(2) Uani 1 d . . .

H8 H 1.1066 -0.1049 0.3853 0.093 Uiso 1 calc R . .

C9 C 1.0370(7) 0.0282(7) 0.4236(4) 0.068(2) Uani 1 d . . .

H9 H 1.0948 0.0414 0.459 0.089 Uiso 1 calc R . .

C10 C 0.9424(6) 0.0967(6) 0.4140(3) 0.0531(17) Uani 1 d . . .

C11 C 0.9266(6) 0.1854(7) 0.4596(3) 0.0575(18) Uani 1 d . . .

H11 H 0.9805 0.2018 0.4965 0.075 Uiso 1 calc R . .

C12 C 0.8092(6) 0.3293(6) 0.4908(3) 0.0521(17) Uani 1 d . . .

C13 C 0.8845(7) 0.4136(8) 0.5113(4) 0.078(2) Uani 1 d . . .

H13 H 0.9529 0.4132 0.4976 0.102 Uiso 1 calc R . .

C14 C 0.8599(8) 0.4995(8) 0.5522(5) 0.095(3) Uani 1 d . . .

H14 H 0.9111 0.5572 0.5657 0.124 Uiso 1 calc R . .

C15 C 0.7599(9) 0.4991(8) 0.5727(4) 0.086(3) Uani 1 d . . .

H15 H 0.7424 0.5565 0.6002 0.112 Uiso 1 calc R . .

C16 C 0.6855(8) 0.4130(9) 0.5523(4) 0.086(3) Uani 1 d . . .

H16 H 0.6177 0.412 0.5667 0.111 Uiso 1 calc R . .

C17 C 0.7095(7) 0.3278(7) 0.5109(4) 0.071(2) Uani 1 d . . .

H17 H 0.6582 0.2703 0.4969 0.092 Uiso 1 calc R . .

C18 C 0.4103(5) 0.1581(6) 0.4325(3) 0.0505(16) Uani 1 d . . .

C19 C 0.4071(6) 0.2504(7) 0.4731(4) 0.065(2) Uani 1 d . . .

H19 H 0.4346 0.3205 0.4624 0.085 Uiso 1 calc R . .

C20 C 0.3620(7) 0.2385(8) 0.5311(4) 0.077(2) Uani 1 d . . .

H20 H 0.3584 0.3017 0.5579 0.1 Uiso 1 calc R . .

C21 C 0.3233(7) 0.1349(9) 0.5485(4) 0.080(3) Uani 1 d . . .

H21 H 0.2937 0.1284 0.5868 0.104 Uiso 1 calc R . .

C22 C 0.3283(6) 0.0422(8) 0.5097(4) 0.070(2) Uani 1 d . . .

H22 H 0.3031 -0.0281 0.5218 0.091 Uiso 1 calc R . .

C23 C 0.3720(6) 0.0526(7) 0.4510(3) 0.0582(18) Uani 1 d . . .

313

C24 C 0.3778(6) -0.0406(7) 0.4063(4) 0.0615(19) Uani 1 d . . .

H24 H 0.3537 -0.1134 0.4145 0.08 Uiso 1 calc R . .

C25 C 0.4176(6) -0.1054(6) 0.3054(4) 0.0606(19) Uani 1 d . . .

C26 C 0.3219(7) -0.1664(7) 0.2831(4) 0.078(2) Uani 1 d . . .

H26 H 0.258 -0.1509 0.2999 0.101 Uiso 1 calc R . .

C27 C 0.3202(9) -0.2506(9) 0.2360(5) 0.100(3) Uani 1 d . . .

H27 H 0.2552 -0.2915 0.2213 0.13 Uiso 1 calc R . .

C28 C 0.4143(10) -0.2741(9) 0.2107(5) 0.101(3) Uani 1 d . . .

H28 H 0.4133 -0.3304 0.1788 0.131 Uiso 1 calc R . .

C29 C 0.5084(8) -0.2145(8) 0.2329(4) 0.084(3) Uani 1 d . . .

H29 H 0.5724 -0.2313 0.2163 0.109 Uiso 1 calc R . .

C30 C 0.5120(6) -0.1284(7) 0.2799(4) 0.065(2) Uani 1 d . . .

H30 H 0.577 -0.0872 0.2939 0.084 Uiso 1 calc R . .

loop_








Pd1 0.0508(3) 0.0479(3) 0.0493(3) -0.0016(2) 0.0172(2) -0.0004(3)

Pd2 0.0482(3) 0.0477(3) 0.0562(3) -0.0045(3) 0.0165(2) 0.0010(2)

N1 0.060(4) 0.048(4) 0.055(3) 0.005(3) 0.018(3) -0.007(3)

N2 0.061(4) 0.046(3) 0.059(3) -0.004(3) 0.021(3) 0.000(3)

N1A 0.057(3) 0.059(4) 0.053(3) -0.010(3) 0.014(3) 0.001(3)

N2A 0.055(4) 0.060(4) 0.056(4) -0.009(3) 0.012(3) -0.004(3)

C2 0.077(5) 0.053(5) 0.056(4) -0.002(4) 0.016(4) -0.012(4)

C3 0.109(7) 0.039(4) 0.066(5) 0.007(4) 0.031(5) 0.003(5)

C4 0.072(5) 0.064(5) 0.062(5) 0.006(4) 0.019(4) 0.027(4)

C2A 0.075(5) 0.079(6) 0.055(4) -0.008(4) 0.027(4) 0.004(4)

C3A 0.088(6) 0.079(6) 0.052(5) -0.008(4) 0.018(4) 0.006(5)

314

C4A 0.070(5) 0.057(5) 0.063(5) -0.010(4) 0.009(4) 0.000(4)

N3 0.052(3) 0.055(3) 0.049(3) -0.005(3) 0.013(3) -0.005(3)

N3A 0.052(3) 0.045(3) 0.065(4) -0.011(3) 0.017(3) 0.000(3)

C5 0.064(4) 0.045(4) 0.053(4) 0.002(3) 0.025(3) 0.003(3)

C6 0.067(5) 0.050(4) 0.056(4) -0.001(3) 0.024(4) -0.001(4)

C7 0.091(6) 0.055(5) 0.071(5) 0.009(4) 0.039(5) 0.018(4)

C8 0.076(5) 0.072(6) 0.074(5) 0.021(5) 0.032(5) 0.024(4)

C9 0.071(5) 0.071(5) 0.062(5) 0.010(4) 0.010(4) 0.012(4)

C10 0.054(4) 0.052(4) 0.054(4) 0.009(3) 0.013(3) 0.009(3)

C11 0.046(4) 0.070(5) 0.055(4) 0.009(4) 0.007(3) -0.002(4)

C12 0.059(4) 0.059(5) 0.038(3) 0.004(3) 0.009(3) 0.001(3)

C13 0.072(5) 0.081(6) 0.090(6) -0.033(5) 0.036(5) -0.014(5)

C14 0.100(7) 0.086(7) 0.104(7) -0.037(6) 0.028(6) -0.012(6)

C15 0.111(8) 0.081(7) 0.068(5) -0.019(5) 0.022(5) 0.020(6)

C16 0.091(6) 0.097(7) 0.077(6) -0.021(5) 0.035(5) 0.021(6)

C17 0.075(5) 0.073(6) 0.070(5) -0.002(4) 0.031(4) -0.005(4)

C18 0.039(3) 0.057(4) 0.056(4) 0.002(3) 0.011(3) 0.001(3)

C19 0.065(5) 0.065(5) 0.070(5) -0.002(4) 0.023(4) 0.004(4)

C20 0.078(6) 0.086(6) 0.068(5) -0.015(5) 0.020(4) 0.008(5)

C21 0.082(6) 0.101(8) 0.062(5) -0.009(5) 0.025(4) -0.003(5)

C22 0.071(5) 0.079(6) 0.062(5) 0.012(4) 0.016(4) 0.001(4)

C23 0.053(4) 0.062(5) 0.060(4) -0.002(4) 0.011(3) 0.004(4)

C24 0.063(5) 0.053(5) 0.069(5) 0.003(4) 0.012(4) -0.005(4)

C25 0.059(4) 0.053(4) 0.069(5) -0.011(4) 0.010(4) 0.001(4)

C26 0.081(6) 0.061(5) 0.096(6) -0.024(5) 0.025(5) -0.007(4)

C27 0.092(7) 0.087(7) 0.118(8) -0.030(6) 0.014(6) -0.020(6)

C28 0.121(9) 0.078(7) 0.096(7) -0.028(6) 0.002(7) 0.005(7)

C29 0.097(7) 0.081(7) 0.077(6) -0.009(5) 0.027(5) 0.031(6)

C30 0.065(5) 0.062(5) 0.071(5) 0.000(4) 0.021(4) 0.015(4)


315


;







;

loop_



_geom_bond_distance



Pd1 C5 1.974(7) . ?

Pd1 N1A 2.001(5) . ?

Pd1 N3 2.030(5) . ?

Pd1 N1 2.096(6) . ?

Pd2 N2 1.991(6) . ?

Pd2 C18 2.011(7) . ?

Pd2 N3A 2.039(6) . ?

Pd2 N2A 2.129(6) . ?

N1 C2 1.342(9) . ?

N1 N2 1.357(7) . ?

N2 C4 1.332(9) . ?

N1A C2A 1.335(8) . ?

N1A N2A 1.352(7) . ?

N2A C4A 1.334(8) . ?

C2 C3 1.362(11) . ?

C2 H2 0.93 . ?

C3 C4 1.367(11) . ?

C3 H3 0.93 . ?

316

C4 H4 0.93 . ?

C2A C3A 1.373(10) . ?

C2A H2A 0.93 . ?

C3A C4A 1.369(10) . ?

C3A H3A 0.93 . ?

C4A H4A 0.93 . ?

N3 C11 1.288(8) . ?

N3 C12 1.444(8) . ?

N3A C24 1.287(8) . ?

N3A C25 1.443(8) . ?

C5 C10 1.394(9) . ?

C5 C6 1.397(9) . ?

C6 C7 1.401(10) . ?

C6 H6 0.93 . ?

C7 C8 1.369(11) . ?

C7 H7 0.93 . ?

C8 C9 1.374(11) . ?

C8 H8 0.93 . ?

C9 C10 1.393(10) . ?

C9 H9 0.93 . ?

C10 C11 1.438(10) . ?

C11 H11 0.93 . ?

C12 C17 1.358(10) . ?

C12 C13 1.365(10) . ?

C13 C14 1.383(11) . ?

C13 H13 0.93 . ?

C14 C15 1.366(12) . ?

C14 H14 0.93 . ?

C15 C16 1.373(12) . ?

C15 H15 0.93 . ?

C16 C17 1.381(11) . ?

C16 H16 0.93 . ?

C17 H17 0.93 . ?

317

C18 C19 1.372(10) . ?

C18 C23 1.402(10) . ?

C19 C20 1.411(10) . ?

C19 H19 0.93 . ?

C20 C21 1.377(12) . ?

C20 H20 0.93 . ?

C21 C22 1.357(11) . ?

C21 H21 0.93 . ?

C22 C23 1.414(10) . ?

C22 H22 0.93 . ?

C23 C24 1.439(10) . ?

C24 H24 0.93 . ?

C25 C26 1.376(10) . ?

C25 C30 1.381(10) . ?

C26 C27 1.383(12) . ?

C26 H26 0.93 . ?

C27 C28 1.377(13) . ?

C27 H27 0.93 . ?

C28 C29 1.353(13) . ?

C28 H28 0.93 . ?

C29 C30 1.394(11) . ?

C29 H29 0.93 . ?

C30 H30 0.93 . ?

loop_




_geom_angle




C5 Pd1 N1A 94.9(3) . . ?

318

C5 Pd1 N3 81.1(3) . . ?

N1A Pd1 N3 175.4(2) . . ?

C5 Pd1 N1 175.6(3) . . ?

N1A Pd1 N1 87.8(2) . . ?

N3 Pd1 N1 96.0(2) . . ?

N2 Pd2 C18 94.2(3) . . ?

N2 Pd2 N3A 175.0(2) . . ?

C18 Pd2 N3A 80.9(3) . . ?

N2 Pd2 N2A 85.7(2) . . ?

C18 Pd2 N2A 176.5(2) . . ?

N3A Pd2 N2A 99.3(2) . . ?

C2 N1 N2 107.5(6) . . ?

C2 N1 Pd1 132.4(5) . . ?

N2 N1 Pd1 119.4(4) . . ?

C4 N2 N1 107.2(6) . . ?

C4 N2 Pd2 135.9(6) . . ?

N1 N2 Pd2 116.9(4) . . ?

C2A N1A N2A 107.1(6) . . ?

C2A N1A Pd1 132.2(5) . . ?

N2A N1A Pd1 120.5(4) . . ?

C4A N2A N1A 108.7(6) . . ?

C4A N2A Pd2 135.6(5) . . ?

N1A N2A Pd2 115.6(4) . . ?

N1 C2 C3 110.3(7) . . ?

N1 C2 H2 124.8 . . ?

C3 C2 H2 124.8 . . ?

C2 C3 C4 104.2(7) . . ?

C2 C3 H3 127.9 . . ?

C4 C3 H3 127.9 . . ?

N2 C4 C3 110.9(7) . . ?

N2 C4 H4 124.6 . . ?

C3 C4 H4 124.6 . . ?

N1A C2A C3A 110.2(7) . . ?

319

N1A C2A H2A 124.9 . . ?

C3A C2A H2A 124.9 . . ?

C4A C3A C2A 104.6(7) . . ?

C4A C3A H3A 127.7 . . ?

C2A C3A H3A 127.7 . . ?

N2A C4A C3A 109.4(7) . . ?

N2A C4A H4A 125.3 . . ?

C3A C4A H4A 125.3 . . ?

C11 N3 C12 121.1(6) . . ?

C11 N3 Pd1 113.9(5) . . ?

C12 N3 Pd1 124.9(4) . . ?

C24 N3A C25 118.4(6) . . ?

C24 N3A Pd2 115.1(5) . . ?

C25 N3A Pd2 126.4(5) . . ?

C10 C5 C6 116.4(6) . . ?

C10 C5 Pd1 112.7(5) . . ?

C6 C5 Pd1 130.8(5) . . ?

C5 C6 C7 120.5(7) . . ?

C5 C6 H6 119.8 . . ?

C7 C6 H6 119.8 . . ?

C8 C7 C6 121.3(7) . . ?

C8 C7 H7 119.4 . . ?

C6 C7 H7 119.4 . . ?

C7 C8 C9 119.7(7) . . ?

C7 C8 H8 120.1 . . ?

C9 C8 H8 120.1 . . ?

C8 C9 C10 119.0(7) . . ?

C8 C9 H9 120.5 . . ?

C10 C9 H9 120.5 . . ?

C9 C10 C5 123.1(7) . . ?

C9 C10 C11 122.2(7) . . ?

C5 C10 C11 114.6(6) . . ?

N3 C11 C10 116.9(6) . . ?

320

N3 C11 H11 121.6 . . ?

C10 C11 H11 121.6 . . ?

C17 C12 C13 120.5(7) . . ?

C17 C12 N3 119.2(7) . . ?

C13 C12 N3 120.2(6) . . ?

C12 C13 C14 120.4(8) . . ?

C12 C13 H13 119.8 . . ?

C14 C13 H13 119.8 . . ?

C15 C14 C13 119.6(9) . . ?

C15 C14 H14 120.2 . . ?

C13 C14 H14 120.2 . . ?

C14 C15 C16 119.3(8) . . ?

C14 C15 H15 120.4 . . ?

C16 C15 H15 120.4 . . ?

C15 C16 C17 121.1(8) . . ?

C15 C16 H16 119.4 . . ?

C17 C16 H16 119.4 . . ?

C12 C17 C16 119.0(8) . . ?

C12 C17 H17 120.5 . . ?

C16 C17 H17 120.5 . . ?

C19 C18 C23 118.9(6) . . ?

C19 C18 Pd2 129.4(6) . . ?

C23 C18 Pd2 111.7(5) . . ?

C18 C19 C20 119.8(8) . . ?

C18 C19 H19 120.1 . . ?

C20 C19 H19 120.1 . . ?

C21 C20 C19 121.0(8) . . ?

C21 C20 H20 119.5 . . ?

C19 C20 H20 119.5 . . ?

C22 C21 C20 120.0(8) . . ?

C22 C21 H21 120 . . ?

C20 C21 H21 120 . . ?

C21 C22 C23 119.9(8) . . ?

321

C21 C22 H22 120.1 . . ?

C23 C22 H22 120.1 . . ?

C18 C23 C22 120.4(7) . . ?

C18 C23 C24 116.0(6) . . ?

C22 C23 C24 123.5(7) . . ?

N3A C24 C23 116.3(7) . . ?

N3A C24 H24 121.9 . . ?

C23 C24 H24 121.9 . . ?

C26 C25 C30 119.4(7) . . ?

C26 C25 N3A 119.9(7) . . ?

C30 C25 N3A 120.6(7) . . ?

C25 C26 C27 120.5(8) . . ?

C25 C26 H26 119.7 . . ?

C27 C26 H26 119.7 . . ?

C28 C27 C26 120.2(9) . . ?

C28 C27 H27 119.9 . . ?

C26 C27 H27 119.9 . . ?

C29 C28 C27 119.3(9) . . ?

C29 C28 H28 120.4 . . ?

C27 C28 H28 120.4 . . ?

C28 C29 C30 121.6(9) . . ?

C28 C29 H29 119.2 . . ?

C30 C29 H29 119.2 . . ?

C25 C30 C29 119.0(8) . . ?

C25 C30 H30 120.5 . . ?

C29 C30 H30 120.5 . . ?

loop_





_geom_torsion

322






C5 Pd1 N1 C2 14(3) . . . . ?

N1A Pd1 N1 C2 -114.1(6) . . . . ?

N3 Pd1 N1 C2 63.3(6) . . . . ?

C5 Pd1 N1 N2 -18E1(4) . . . . ?

N1A Pd1 N1 N2 54.5(5) . . . . ?

N3 Pd1 N1 N2 -128.1(5) . . . . ?

C2 N1 N2 C4 1.3(7) . . . . ?

Pd1 N1 N2 C4 -170.0(4) . . . . ?

C2 N1 N2 Pd2 179.3(4) . . . . ?

Pd1 N1 N2 Pd2 8.1(6) . . . . ?

C18 Pd2 N2 C4 -70.7(7) . . . . ?

N3A Pd2 N2 C4 -64(3) . . . . ?

N2A Pd2 N2 C4 112.7(7) . . . . ?

C18 Pd2 N2 N1 111.9(5) . . . . ?

N3A Pd2 N2 N1 119(3) . . . . ?

N2A Pd2 N2 N1 -64.6(5) . . . . ?

C5 Pd1 N1A C2A -57.6(7) . . . . ?

N3 Pd1 N1A C2A -27(3) . . . . ?

N1 Pd1 N1A C2A 118.9(7) . . . . ?

C5 Pd1 N1A N2A 128.4(5) . . . . ?

N3 Pd1 N1A N2A 159(3) . . . . ?

N1 Pd1 N1A N2A -55.1(5) . . . . ?

C2A N1A N2A C4A -0.9(8) . . . . ?

Pd1 N1A N2A C4A 174.5(5) . . . . ?

C2A N1A N2A Pd2 -177.6(5) . . . . ?

Pd1 N1A N2A Pd2 -2.3(7) . . . . ?

N2 Pd2 N2A C4A -112.0(7) . . . . ?

C18 Pd2 N2A C4A 159(4) . . . . ?

323

N3A Pd2 N2A C4A 67.7(7) . . . . ?

N2 Pd2 N2A N1A 63.6(5) . . . . ?

C18 Pd2 N2A N1A -25(5) . . . . ?

N3A Pd2 N2A N1A -116.7(5) . . . . ?

N2 N1 C2 C3 -1.3(8) . . . . ?

Pd1 N1 C2 C3 168.3(5) . . . . ?

N1 C2 C3 C4 0.8(8) . . . . ?

N1 N2 C4 C3 -0.8(8) . . . . ?

Pd2 N2 C4 C3 -178.3(5) . . . . ?

C2 C3 C4 N2 0.0(8) . . . . ?

N2A N1A C2A C3A 0.2(9) . . . . ?

Pd1 N1A C2A C3A -174.4(5) . . . . ?

N1A C2A C3A C4A 0.6(10) . . . . ?

N1A N2A C4A C3A 1.3(9) . . . . ?

Pd2 N2A C4A C3A 177.1(6) . . . . ?

C2A C3A C4A N2A -1.2(9) . . . . ?

C5 Pd1 N3 C11 7.3(5) . . . . ?

N1A Pd1 N3 C11 -23(3) . . . . ?

N1 Pd1 N3 C11 -169.2(5) . . . . ?

C5 Pd1 N3 C12 -176.3(5) . . . . ?

N1A Pd1 N3 C12 153(3) . . . . ?

N1 Pd1 N3 C12 7.1(5) . . . . ?

N2 Pd2 N3A C24 -9(3) . . . . ?

C18 Pd2 N3A C24 -2.2(5) . . . . ?

N2A Pd2 N3A C24 174.3(5) . . . . ?

N2 Pd2 N3A C25 167(3) . . . . ?

C18 Pd2 N3A C25 174.3(6) . . . . ?

N2A Pd2 N3A C25 -9.2(6) . . . . ?

N1A Pd1 C5 C10 169.9(5) . . . . ?

N3 Pd1 C5 C10 -7.8(5) . . . . ?

N1 Pd1 C5 C10 42(3) . . . . ?

N1A Pd1 C5 C6 -7.1(6) . . . . ?

N3 Pd1 C5 C6 175.2(6) . . . . ?

324

N1 Pd1 C5 C6 -135(3) . . . . ?

C10 C5 C6 C7 -2.1(9) . . . . ?

Pd1 C5 C6 C7 174.9(5) . . . . ?

C5 C6 C7 C8 1.5(11) . . . . ?

C6 C7 C8 C9 0.1(12) . . . . ?

C7 C8 C9 C10 -0.9(11) . . . . ?

C8 C9 C10 C5 0.1(11) . . . . ?

C8 C9 C10 C11 176.4(7) . . . . ?

C6 C5 C10 C9 1.4(10) . . . . ?

Pd1 C5 C10 C9 -176.2(6) . . . . ?

C6 C5 C10 C11 -175.2(6) . . . . ?

Pd1 C5 C10 C11 7.3(8) . . . . ?

C12 N3 C11 C10 178.1(6) . . . . ?

Pd1 N3 C11 C10 -5.4(8) . . . . ?

C9 C10 C11 N3 -177.8(7) . . . . ?

C5 C10 C11 N3 -1.2(9) . . . . ?

C11 N3 C12 C17 -130.2(7) . . . . ?

Pd1 N3 C12 C17 53.7(8) . . . . ?

C11 N3 C12 C13 50.3(10) . . . . ?

Pd1 N3 C12 C13 -125.8(7) . . . . ?

C17 C12 C13 C14 -0.8(13) . . . . ?

N3 C12 C13 C14 178.7(8) . . . . ?

C12 C13 C14 C15 0.7(15) . . . . ?

C13 C14 C15 C16 0.1(15) . . . . ?

C14 C15 C16 C17 -0.8(15) . . . . ?

C13 C12 C17 C16 0.1(12) . . . . ?

N3 C12 C17 C16 -179.5(7) . . . . ?

C15 C16 C17 C12 0.7(14) . . . . ?

N2 Pd2 C18 C19 -0.9(7) . . . . ?

N3A Pd2 C18 C19 179.7(7) . . . . ?

N2A Pd2 C18 C19 87(4) . . . . ?

N2 Pd2 C18 C23 -178.3(5) . . . . ?

N3A Pd2 C18 C23 2.3(5) . . . . ?

325

N2A Pd2 C18 C23 -90(4) . . . . ?

C23 C18 C19 C20 -2.3(11) . . . . ?

Pd2 C18 C19 C20 -179.5(6) . . . . ?

C18 C19 C20 C21 1.5(12) . . . . ?

C19 C20 C21 C22 0.1(13) . . . . ?

C20 C21 C22 C23 -0.8(13) . . . . ?

C19 C18 C23 C22 1.5(10) . . . . ?

Pd2 C18 C23 C22 179.2(5) . . . . ?

C19 C18 C23 C24 -180.0(6) . . . . ?

Pd2 C18 C23 C24 -2.2(8) . . . . ?

C21 C22 C23 C18 0.0(11) . . . . ?

C21 C22 C23 C24 -178.4(7) . . . . ?

C25 N3A C24 C23 -175.2(6) . . . . ?

Pd2 N3A C24 C23 1.6(8) . . . . ?

C18 C23 C24 N3A 0.4(10) . . . . ?

C22 C23 C24 N3A 178.9(7) . . . . ?

C24 N3A C25 C26 48.6(10) . . . . ?

Pd2 N3A C25 C26 -127.8(7) . . . . ?

C24 N3A C25 C30 -132.1(8) . . . . ?

Pd2 N3A C25 C30 51.5(9) . . . . ?

C30 C25 C26 C27 0.4(13) . . . . ?

N3A C25 C26 C27 179.7(8) . . . . ?

C25 C26 C27 C28 -0.1(16) . . . . ?

C26 C27 C28 C29 0.4(17) . . . . ?

C27 C28 C29 C30 -1.0(16) . . . . ?

C26 C25 C30 C29 -1.0(12) . . . . ?

N3A C25 C30 C29 179.7(7) . . . . ?

C28 C29 C30 C25 1.4(13) . . . . ?

326

A4,8. C36H38N4P2Pd (cyPd7) #\#CIF_1.1


# Created on 2010-03-04 at 10:37:45





# CIF files read : maurod struct


data_global

#------------------ AUDIT DETAILS -------------------------------------------#











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327


Glasgow G12 8QQ

Scotland UK

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328





_journal_year ?

_journal_volume ?

_journal_issue ?






_publ_section_title

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_publ_author_name



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Glasgow G12 8QQ

Scotland UK

329

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#------------------ TEXT ----------------------------------------------------#


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330


;


Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.














The Netherlands.



331









A24, 351-359



Volume C.











332


34, 824-828


35, 281.




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data_maurod


333



_chemical_formula_moiety 'C36 H38 N4 P2 Pd1'

_chemical_formula_sum 'C36 H38 N4 P2 Pd'




_symmetry_space_group_name_H-M 'P 1 21/c 1'

loop_


'x, y, z'

'-x, y+1/2, -z+1/2'

'-x, -y, -z'

'x, -y-1/2, z-1/2'














334



























0.999


0.999


335


















Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^












336



loop_

_atom_type_symbol










loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type






Pd Pd 0.29258(2) 0.262468(16) 0.688977(11) 0.03494(12) Uani 1 d . . .

P1 P 0.30673(8) 0.36116(5) 0.76962(4) 0.03485(19) Uani 1 d . . .

P2 P 0.10685(8) 0.19483(5) 0.71794(4) 0.0364(2) Uani 1 d . . .

N1 N 0.4848(3) 0.31397(19) 0.66282(14) 0.0449(7) Uani 1 d . . .

337

N2 N 0.5067(4) 0.3251(3) 0.6139(2) 0.0711(10) Uani 1 d . . .

N3 N 0.5402(7) 0.3402(5) 0.5640(3) 0.133(3) Uani 1 d . . .

N4 N 0.1083(6) 0.3178(3) 0.48920(18) 0.0841(13) Uani 1 d . . .

C1 C 0.1639(4) 0.3676(2) 0.81975(16) 0.0415(7) Uani 1 d . . .

H11 H 0.2001 0.3875 0.8601 0.054 Uiso 1 calc R . .

H12 H 0.0987 0.4092 0.8027 0.054 Uiso 1 calc R . .

C2 C 0.0862(4) 0.2855(2) 0.82842(16) 0.0449(8) Uani 1 d . . .

H21 H 0.0236 0.2936 0.8605 0.058 Uiso 1 calc R . .

H22 H 0.1519 0.2425 0.8426 0.058 Uiso 1 calc R . .

C3 C 0.0037(4) 0.2543(2) 0.76981(18) 0.0433(8) Uani 1 d . . .

H31 H -0.0369 0.3023 0.7476 0.056 Uiso 1 calc R . .

H32 H -0.0709 0.2189 0.7816 0.056 Uiso 1 calc R . .

C4 C 0.2916(3) 0.1851(2) 0.61377(15) 0.0404(7) Uani 1 d . . .

C5 C 0.3662(4) 0.1112(2) 0.61771(19) 0.0510(9) Uani 1 d . . .

H5 H 0.4054 0.0936 0.6561 0.066 Uiso 1 calc R . .

C6 C 0.3840(5) 0.0626(3) 0.5658(2) 0.0622(11) Uani 1 d . . .

H6 H 0.4352 0.0133 0.5693 0.081 Uiso 1 calc R . .

C7 C 0.3243(5) 0.0887(3) 0.5087(2) 0.0668(12) Uani 1 d . . .

H7 H 0.3375 0.0576 0.4734 0.087 Uiso 1 calc R . .

C8 C 0.2462(5) 0.1599(3) 0.50441(18) 0.0626(11) Uani 1 d . . .

H8 H 0.2038 0.1758 0.4662 0.081 Uiso 1 calc R . .

C9 C 0.2289(4) 0.2096(3) 0.55634(16) 0.0490(8) Uani 1 d . . .

C10 C 0.1387(7) 0.2867(4) 0.5504(2) 0.0847(17) Uani 1 d . . .

H101 H 0.0524 0.2741 0.5679 0.11 Uiso 1 calc R . .

H102 H 0.1834 0.3312 0.5752 0.11 Uiso 1 calc R . .

C11 C -0.0177(12) 0.3650(7) 0.4810(5) 0.205(6) Uani 1 d . . .

H111 H -0.0103 0.4143 0.5066 0.266 Uiso 1 calc R . .

H112 H -0.0928 0.3309 0.4926 0.266 Uiso 1 calc R . .

H113 H -0.034 0.3813 0.4384 0.266 Uiso 1 calc R . .

C12 C 0.2226(12) 0.3689(6) 0.4737(4) 0.165(4) Uani 1 d . . .

H121 H 0.2198 0.422 0.4947 0.214 Uiso 1 calc R . .

H122 H 0.2169 0.3782 0.4298 0.214 Uiso 1 calc R . .

H123 H 0.3075 0.3407 0.4863 0.214 Uiso 1 calc R . .

338

C1B C 0.1513(3) 0.1020(2) 0.76439(15) 0.0382(7) Uani 1 d . . .

C2B C 0.2867(4) 0.0871(2) 0.78705(17) 0.0476(8) Uani 1 d . . .

H2B H 0.3567 0.1225 0.7761 0.062 Uiso 1 calc R . .

C3B C 0.3176(4) 0.0189(3) 0.8263(2) 0.0580(10) Uani 1 d . . .

H3B H 0.4083 0.0095 0.8416 0.075 Uiso 1 calc R . .

C4B C 0.2170(5) -0.0337(3) 0.8425(2) 0.0585(10) Uani 1 d . . .

H4B H 0.2388 -0.0789 0.8686 0.076 Uiso 1 calc R . .

C5B C 0.0810(4) -0.0199(3) 0.81972(19) 0.0561(10) Uani 1 d . . .

H5B H 0.0119 -0.0561 0.8305 0.073 Uiso 1 calc R . .

C6B C 0.0487(4) 0.0475(2) 0.78126(18) 0.0478(8) Uani 1 d . . .

H6B H -0.0424 0.0567 0.7664 0.062 Uiso 1 calc R . .

C7B C -0.0197(4) 0.1579(2) 0.65790(16) 0.0467(8) Uani 1 d . . .

C8B C 0.0066(5) 0.0839(3) 0.62674(18) 0.0578(10) Uani 1 d . . .

H8B H 0.0846 0.0522 0.6384 0.075 Uiso 1 calc R . .

C9B C -0.0862(6) 0.0576(3) 0.5774(2) 0.0747(14) Uani 1 d . . .

H9B H -0.0698 0.0086 0.5558 0.097 Uiso 1 calc R . .

C10B C -0.2042(6) 0.1066(4) 0.5612(2) 0.0845(17) Uani 1 d . . .

H10B H -0.2658 0.0896 0.5286 0.11 Uiso 1 calc R . .

C11B C -0.2291(6) 0.1773(4) 0.5919(2) 0.0822(16) Uani 1 d . . .

H11B H -0.308 0.2086 0.581 0.107 Uiso 1 calc R . .

C12B C -0.1372(5) 0.2035(3) 0.6397(2) 0.0653(11) Uani 1 d . . .

H12B H -0.1546 0.2532 0.6602 0.085 Uiso 1 calc R . .

C1A C 0.3171(3) 0.4688(2) 0.74132(16) 0.0401(7) Uani 1 d . . .

C2A C 0.2968(4) 0.4857(3) 0.67882(18) 0.0514(9) Uani 1 d . . .

H2A H 0.279 0.4419 0.6509 0.067 Uiso 1 calc R . .

C3A C 0.3029(5) 0.5679(3) 0.6575(2) 0.0705(13) Uani 1 d . . .

H3A H 0.2875 0.5792 0.6155 0.092 Uiso 1 calc R . .

C4A C 0.3316(5) 0.6320(3) 0.6984(3) 0.0696(14) Uani 1 d . . .

H4A H 0.3375 0.6868 0.6838 0.09 Uiso 1 calc R . .

C5A C 0.3514(4) 0.6168(3) 0.7594(3) 0.0619(11) Uani 1 d . . .

H5A H 0.3705 0.661 0.7868 0.08 Uiso 1 calc R . .

C6A C 0.3434(4) 0.5352(2) 0.7817(2) 0.0501(9) Uani 1 d . . .

H6A H 0.3558 0.5252 0.824 0.065 Uiso 1 calc R . .

339

C7A C 0.4619(3) 0.3493(2) 0.82214(15) 0.0404(7) Uani 1 d . . .

C8A C 0.4610(5) 0.3071(3) 0.87745(17) 0.0595(10) Uani 1 d . . .

H8A H 0.3792 0.2844 0.8893 0.077 Uiso 1 calc R . .

C9A C 0.5825(6) 0.2982(4) 0.9160(2) 0.0781(15) Uani 1 d . . .

H9A H 0.581 0.271 0.9539 0.101 Uiso 1 calc R . .

C10A C 0.7031(5) 0.3297(3) 0.8979(2) 0.0729(14) Uani 1 d . . .

H10A H 0.784 0.3233 0.9234 0.095 Uiso 1 calc R . .

C11A C 0.7062(4) 0.3706(3) 0.8426(2) 0.0643(11) Uani 1 d . . .

H11A H 0.7891 0.3917 0.8307 0.084 Uiso 1 calc R . .

C12A C 0.5863(4) 0.3808(2) 0.80428(19) 0.0523(9) Uani 1 d . . .

H12A H 0.5889 0.4085 0.7667 0.068 Uiso 1 calc R . .

loop_








Pd 0.03654(17) 0.03490(17) 0.03382(16) -0.00537(9) 0.00561(10) -0.00539(9)

P1 0.0366(4) 0.0337(4) 0.0342(4) -0.0042(3) 0.0031(3) -0.0025(3)

P2 0.0340(4) 0.0363(4) 0.0388(4) -0.0015(3) 0.0016(3) -0.0050(3)

N1 0.0485(17) 0.0466(17) 0.0412(16) -0.0129(13) 0.0135(13) -0.0169(13)

N2 0.058(2) 0.065(2) 0.091(3) -0.011(2) 0.016(2) -0.0134(18)

N3 0.131(5) 0.187(7) 0.086(4) 0.020(4) 0.042(4) -0.047(5)

N4 0.129(4) 0.066(3) 0.054(2) 0.0133(19) -0.013(2) 0.010(3)

C1 0.0435(18) 0.0403(17) 0.0415(17) -0.0051(14) 0.0087(14) 0.0015(14)

C2 0.0464(19) 0.0482(19) 0.0419(18) -0.0012(15) 0.0145(15) -0.0006(15)

C3 0.0340(16) 0.0446(19) 0.052(2) -0.0012(15) 0.0068(15) -0.0005(14)

C4 0.0418(17) 0.0392(17) 0.0411(17) -0.0081(14) 0.0081(14) -0.0060(14)

C5 0.047(2) 0.049(2) 0.057(2) -0.0063(17) 0.0025(17) 0.0026(16)

C6 0.068(3) 0.045(2) 0.075(3) -0.016(2) 0.018(2) 0.0052(19)

340

C7 0.090(3) 0.058(2) 0.056(2) -0.024(2) 0.024(2) -0.010(2)

C8 0.088(3) 0.061(3) 0.0396(19) -0.0066(18) 0.0090(19) -0.005(2)

C9 0.062(2) 0.0473(19) 0.0384(18) -0.0012(15) 0.0084(16) 0.0007(17)

C10 0.127(5) 0.079(3) 0.048(2) 0.012(2) 0.008(3) 0.042(3)

C11 0.235(13) 0.189(11) 0.176(10) 0.037(8) -0.073(9) 0.095(10)

C12 0.246(12) 0.112(6) 0.143(7) 0.042(6) 0.060(8) -0.022(7)

C1B 0.0359(16) 0.0385(17) 0.0398(16) -0.0026(13) 0.0010(13) -0.0019(13)

C2B 0.0369(17) 0.053(2) 0.053(2) 0.0006(17) 0.0053(15) 0.0007(15)

C3B 0.042(2) 0.065(3) 0.066(3) 0.003(2) -0.0035(18) 0.0136(18)

C4B 0.065(3) 0.050(2) 0.060(2) 0.0090(18) 0.0011(19) 0.0115(19)

C5B 0.055(2) 0.046(2) 0.067(2) 0.0087(18) 0.0037(19) -0.0085(17)

C6B 0.0396(18) 0.0457(19) 0.057(2) 0.0071(16) -0.0032(15) -0.0054(15)

C7B 0.0458(19) 0.052(2) 0.0414(18) 0.0051(15) -0.0033(14) -0.0152(16)

C8B 0.065(2) 0.059(2) 0.048(2) -0.0021(18) -0.0004(18) -0.021(2)

C9B 0.100(4) 0.072(3) 0.052(2) -0.009(2) 0.007(2) -0.039(3)

C10B 0.087(4) 0.101(4) 0.060(3) 0.019(3) -0.028(3) -0.031(3)

C11B 0.082(3) 0.082(4) 0.076(3) 0.013(3) -0.032(3) -0.009(3)

C12B 0.062(3) 0.067(3) 0.064(3) 0.010(2) -0.013(2) -0.004(2)

C1A 0.0336(16) 0.0392(17) 0.0473(18) 0.0021(14) 0.0021(13) -0.0003(13)

C2A 0.048(2) 0.052(2) 0.053(2) 0.0066(17) 0.0026(17) 0.0039(16)

C3A 0.059(3) 0.076(3) 0.078(3) 0.033(3) 0.012(2) 0.012(2)

C4A 0.047(2) 0.043(2) 0.119(4) 0.023(3) 0.014(2) 0.0053(18)

C5A 0.043(2) 0.040(2) 0.103(4) -0.003(2) 0.007(2) -0.0006(16)

C6A 0.0428(19) 0.0390(18) 0.067(2) -0.0059(17) -0.0016(17) -0.0028(15)

C7A 0.0408(17) 0.0383(17) 0.0415(17) -0.0105(13) -0.0004(14) 0.0051(13)

C8A 0.060(2) 0.078(3) 0.041(2) 0.0041(19) 0.0019(17) 0.008(2)

C9A 0.091(4) 0.098(4) 0.042(2) -0.003(2) -0.012(2) 0.026(3)

C10A 0.060(3) 0.087(3) 0.068(3) -0.025(3) -0.021(2) 0.020(2)

C11A 0.046(2) 0.064(3) 0.081(3) -0.017(2) -0.007(2) 0.0053(19)

C12A 0.047(2) 0.046(2) 0.063(2) -0.0024(17) -0.0011(17) 0.0011(16)


341


;







;

loop_



_geom_bond_distance



Pd C4 2.043(3) . ?

Pd N1 2.160(3) . ?

Pd P2 2.2378(8) . ?

Pd P1 2.3463(8) . ?

P1 C1A 1.825(3) . ?

P1 C7A 1.827(3) . ?

P1 C1 1.836(3) . ?

P2 C7B 1.816(3) . ?

P2 C1B 1.820(3) . ?

P2 C3 1.831(4) . ?

N1 N2 1.113(5) . ?

N2 N3 1.181(6) . ?

N4 C10 1.426(6) . ?

N4 C11 1.437(10) . ?

N4 C12 1.441(10) . ?

C1 C2 1.528(5) . ?

C1 H11 0.97 . ?

342

C1 H12 0.97 . ?

C2 C3 1.530(5) . ?

C2 H21 0.97 . ?

C2 H22 0.97 . ?

C3 H31 0.97 . ?

C3 H32 0.97 . ?

C4 C5 1.381(5) . ?

C4 C9 1.397(5) . ?

C5 C6 1.388(5) . ?

C5 H5 0.93 . ?

C6 C7 1.389(7) . ?

C6 H6 0.93 . ?

C7 C8 1.364(7) . ?

C7 H7 0.93 . ?

C8 C9 1.397(5) . ?

C8 H8 0.93 . ?

C9 C10 1.509(6) . ?

C10 H101 0.97 . ?

C10 H102 0.97 . ?

C11 H111 0.96 . ?

C11 H112 0.96 . ?

C11 H113 0.96 . ?

C12 H121 0.96 . ?

C12 H122 0.96 . ?

C12 H123 0.96 . ?

C1B C2B 1.390(5) . ?

C1B C6B 1.394(5) . ?

C2B C3B 1.397(6) . ?

C2B H2B 0.93 . ?

C3B C4B 1.356(6) . ?

C3B H3B 0.93 . ?

C4B C5B 1.393(6) . ?

C4B H4B 0.93 . ?

343

C5B C6B 1.379(5) . ?

C5B H5B 0.93 . ?

C6B H6B 0.93 . ?

C7B C12B 1.386(6) . ?

C7B C8B 1.391(6) . ?

C8B C9B 1.407(6) . ?

C8B H8B 0.93 . ?

C9B C10B 1.410(8) . ?

C9B H9B 0.93 . ?

C10B C11B 1.339(8) . ?

C10B H10B 0.93 . ?

C11B C12B 1.377(6) . ?

C11B H11B 0.93 . ?

C12B H12B 0.93 . ?

C1A C2A 1.380(5) . ?

C1A C6A 1.383(5) . ?

C2A C3A 1.390(6) . ?

C2A H2A 0.93 . ?

C3A C4A 1.364(8) . ?

C3A H3A 0.93 . ?

C4A C5A 1.345(7) . ?

C4A H4A 0.93 . ?

C5A C6A 1.388(6) . ?

C5A H5A 0.93 . ?

C6A H6A 0.93 . ?

C7A C8A 1.375(5) . ?

C7A C12A 1.394(5) . ?

C8A C9A 1.400(6) . ?

C8A H8A 0.93 . ?

C9A C10A 1.364(8) . ?

C9A H9A 0.93 . ?

C10A C11A 1.366(7) . ?

C10A H10A 0.93 . ?

344

C11A C12A 1.387(6) . ?

C11A H11A 0.93 . ?

C12A H12A 0.93 . ?

loop_




_geom_angle




C4 Pd N1 88.09(12) . . ?

C4 Pd P2 89.03(10) . . ?

N1 Pd P2 173.25(9) . . ?

C4 Pd P1 174.08(10) . . ?

N1 Pd P1 86.69(8) . . ?

P2 Pd P1 96.46(3) . . ?

C1A P1 C7A 103.94(16) . . ?

C1A P1 C1 102.25(16) . . ?

C7A P1 C1 105.33(16) . . ?

C1A P1 Pd 112.26(11) . . ?

C7A P1 Pd 113.05(10) . . ?

C1 P1 Pd 118.50(11) . . ?

C7B P2 C1B 104.54(16) . . ?

C7B P2 C3 103.53(18) . . ?

C1B P2 C3 101.34(16) . . ?

C7B P2 Pd 118.10(12) . . ?

C1B P2 Pd 112.61(11) . . ?

C3 P2 Pd 114.84(12) . . ?

N2 N1 Pd 123.2(3) . . ?

N1 N2 N3 174.4(5) . . ?

C10 N4 C11 114.0(6) . . ?

345

C10 N4 C12 107.9(6) . . ?

C11 N4 C12 110.1(7) . . ?

C2 C1 P1 115.6(2) . . ?

C2 C1 H11 108.4 . . ?

P1 C1 H11 108.4 . . ?

C2 C1 H12 108.4 . . ?

P1 C1 H12 108.4 . . ?

H11 C1 H12 107.4 . . ?

C1 C2 C3 114.0(3) . . ?

C1 C2 H21 108.7 . . ?

C3 C2 H21 108.7 . . ?

C1 C2 H22 108.7 . . ?

C3 C2 H22 108.7 . . ?

H21 C2 H22 107.6 . . ?

C2 C3 P2 113.7(2) . . ?

C2 C3 H31 108.8 . . ?

P2 C3 H31 108.8 . . ?

C2 C3 H32 108.8 . . ?

P2 C3 H32 108.8 . . ?

H31 C3 H32 107.7 . . ?

C5 C4 C9 118.8(3) . . ?

C5 C4 Pd 119.7(3) . . ?

C9 C4 Pd 121.2(3) . . ?

C4 C5 C6 121.6(4) . . ?

C4 C5 H5 119.2 . . ?

C6 C5 H5 119.2 . . ?

C5 C6 C7 119.1(4) . . ?

C5 C6 H6 120.4 . . ?

C7 C6 H6 120.4 . . ?

C8 C7 C6 120.0(4) . . ?

C8 C7 H7 120 . . ?

C6 C7 H7 120 . . ?

C7 C8 C9 121.2(4) . . ?

346

C7 C8 H8 119.4 . . ?

C9 C8 H8 119.4 . . ?

C8 C9 C4 119.3(4) . . ?

C8 C9 C10 119.9(4) . . ?

C4 C9 C10 120.8(3) . . ?

N4 C10 C9 115.9(4) . . ?

N4 C10 H101 108.3 . . ?

C9 C10 H101 108.3 . . ?

N4 C10 H102 108.3 . . ?

C9 C10 H102 108.3 . . ?

H101 C10 H102 107.4 . . ?

N4 C11 H111 109.5 . . ?

N4 C11 H112 109.5 . . ?

H111 C11 H112 109.5 . . ?

N4 C11 H113 109.5 . . ?

H111 C11 H113 109.5 . . ?

H112 C11 H113 109.5 . . ?

N4 C12 H121 109.5 . . ?

N4 C12 H122 109.5 . . ?

H121 C12 H122 109.5 . . ?

N4 C12 H123 109.5 . . ?

H121 C12 H123 109.5 . . ?

H122 C12 H123 109.5 . . ?

C2B C1B C6B 118.8(3) . . ?

C2B C1B P2 120.6(3) . . ?

C6B C1B P2 120.5(3) . . ?

C1B C2B C3B 119.9(4) . . ?

C1B C2B H2B 120 . . ?

C3B C2B H2B 120 . . ?

C4B C3B C2B 120.9(4) . . ?

C4B C3B H3B 119.6 . . ?

C2B C3B H3B 119.6 . . ?

C3B C4B C5B 119.8(4) . . ?

347

C3B C4B H4B 120.1 . . ?

C5B C4B H4B 120.1 . . ?

C6B C5B C4B 120.1(4) . . ?

C6B C5B H5B 120 . . ?

C4B C5B H5B 120 . . ?

C5B C6B C1B 120.6(3) . . ?

C5B C6B H6B 119.7 . . ?

C1B C6B H6B 119.7 . . ?

C12B C7B C8B 119.0(4) . . ?

C12B C7B P2 122.1(3) . . ?

C8B C7B P2 118.8(3) . . ?

C7B C8B C9B 119.3(5) . . ?

C7B C8B H8B 120.4 . . ?

C9B C8B H8B 120.4 . . ?

C8B C9B C10B 119.1(5) . . ?

C8B C9B H9B 120.5 . . ?

C10B C9B H9B 120.5 . . ?

C11B C10B C9B 121.1(4) . . ?

C11B C10B H10B 119.4 . . ?

C9B C10B H10B 119.4 . . ?

C10B C11B C12B 119.7(5) . . ?

C10B C11B H11B 120.1 . . ?

C12B C11B H11B 120.1 . . ?

C11B C12B C7B 121.8(5) . . ?

C11B C12B H12B 119.1 . . ?

C7B C12B H12B 119.1 . . ?

C2A C1A C6A 118.5(4) . . ?

C2A C1A P1 120.4(3) . . ?

C6A C1A P1 121.1(3) . . ?

C1A C2A C3A 120.2(4) . . ?

C1A C2A H2A 119.9 . . ?

C3A C2A H2A 119.9 . . ?

C4A C3A C2A 120.0(4) . . ?

348

C4A C3A H3A 120 . . ?

C2A C3A H3A 120 . . ?

C5A C4A C3A 120.7(4) . . ?

C5A C4A H4A 119.7 . . ?

C3A C4A H4A 119.7 . . ?

C4A C5A C6A 120.2(4) . . ?

C4A C5A H5A 119.9 . . ?

C6A C5A H5A 119.9 . . ?

C1A C6A C5A 120.5(4) . . ?

C1A C6A H6A 119.8 . . ?

C5A C6A H6A 119.8 . . ?

C8A C7A C12A 119.0(3) . . ?

C8A C7A P1 122.1(3) . . ?

C12A C7A P1 118.9(3) . . ?

C7A C8A C9A 120.4(4) . . ?

C7A C8A H8A 119.8 . . ?

C9A C8A H8A 119.8 . . ?

C10A C9A C8A 119.8(5) . . ?

C10A C9A H9A 120.1 . . ?

C8A C9A H9A 120.1 . . ?

C9A C10A C11A 120.5(4) . . ?

C9A C10A H10A 119.7 . . ?

C11A C10A H10A 119.7 . . ?

C10A C11A C12A 120.3(4) . . ?

C10A C11A H11A 119.8 . . ?

C12A C11A H11A 119.8 . . ?

C11A C12A C7A 120.0(4) . . ?

C11A C12A H12A 120 . . ?

C7A C12A H12A 120 . . ?

loop_



349



_geom_torsion






C4 Pd P1 C1A 29.4(10) . . . . ?

N1 Pd P1 C1A 57.59(14) . . . . ?

P2 Pd P1 C1A -128.40(12) . . . . ?

C4 Pd P1 C7A -87.8(10) . . . . ?

N1 Pd P1 C7A -59.61(16) . . . . ?

P2 Pd P1 C7A 114.40(13) . . . . ?

C4 Pd P1 C1 148.3(10) . . . . ?

N1 Pd P1 C1 176.48(16) . . . . ?

P2 Pd P1 C1 -9.51(14) . . . . ?

C4 Pd P2 C7B -35.45(18) . . . . ?

N1 Pd P2 C7B -100.2(7) . . . . ?

P1 Pd P2 C7B 142.31(15) . . . . ?

C4 Pd P2 C1B 86.59(15) . . . . ?

N1 Pd P2 C1B 21.9(7) . . . . ?

P1 Pd P2 C1B -95.64(12) . . . . ?

C4 Pd P2 C3 -158.10(17) . . . . ?

N1 Pd P2 C3 137.2(7) . . . . ?

P1 Pd P2 C3 19.66(14) . . . . ?

C4 Pd N1 N2 38.1(4) . . . . ?

P2 Pd N1 N2 102.9(8) . . . . ?

P1 Pd N1 N2 -139.1(4) . . . . ?

Pd N1 N2 N3 174(6) . . . . ?

C1A P1 C1 C2 154.1(3) . . . . ?

C7A P1 C1 C2 -97.5(3) . . . . ?

Pd P1 C1 C2 30.1(3) . . . . ?

350

P1 C1 C2 C3 -67.6(4) . . . . ?

C1 C2 C3 P2 83.2(3) . . . . ?

C7B P2 C3 C2 174.5(3) . . . . ?

C1B P2 C3 C2 66.4(3) . . . . ?

Pd P2 C3 C2 -55.3(3) . . . . ?

N1 Pd C4 C5 82.9(3) . . . . ?

P2 Pd C4 C5 -91.0(3) . . . . ?

P1 Pd C4 C5 111.1(10) . . . . ?

N1 Pd C4 C9 -90.2(3) . . . . ?

P2 Pd C4 C9 95.9(3) . . . . ?

P1 Pd C4 C9 -62.0(11) . . . . ?

C9 C4 C5 C6 2.3(6) . . . . ?

Pd C4 C5 C6 -171.0(3) . . . . ?

C4 C5 C6 C7 -0.5(6) . . . . ?

C5 C6 C7 C8 -1.8(7) . . . . ?

C6 C7 C8 C9 2.4(7) . . . . ?

C7 C8 C9 C4 -0.7(7) . . . . ?

C7 C8 C9 C10 -178.3(5) . . . . ?

C5 C4 C9 C8 -1.6(6) . . . . ?

Pd C4 C9 C8 171.5(3) . . . . ?

C5 C4 C9 C10 176.0(5) . . . . ?

Pd C4 C9 C10 -10.8(6) . . . . ?

C11 N4 C10 C9 154.8(7) . . . . ?

C12 N4 C10 C9 -82.6(7) . . . . ?

C8 C9 C10 N4 -17.5(8) . . . . ?

C4 C9 C10 N4 165.0(5) . . . . ?

C7B P2 C1B C2B 140.2(3) . . . . ?

C3 P2 C1B C2B -112.5(3) . . . . ?

Pd P2 C1B C2B 10.7(3) . . . . ?

C7B P2 C1B C6B -44.1(3) . . . . ?

C3 P2 C1B C6B 63.3(3) . . . . ?

Pd P2 C1B C6B -173.5(3) . . . . ?

C6B C1B C2B C3B -0.5(5) . . . . ?

351

P2 C1B C2B C3B 175.3(3) . . . . ?

C1B C2B C3B C4B 0.5(6) . . . . ?

C2B C3B C4B C5B 0.0(7) . . . . ?

C3B C4B C5B C6B -0.4(7) . . . . ?

C4B C5B C6B C1B 0.4(6) . . . . ?

C2B C1B C6B C5B 0.0(6) . . . . ?

P2 C1B C6B C5B -175.8(3) . . . . ?

C1B P2 C7B C12B 137.4(3) . . . . ?

C3 P2 C7B C12B 31.7(4) . . . . ?

Pd P2 C7B C12B -96.5(3) . . . . ?

C1B P2 C7B C8B -46.6(3) . . . . ?

C3 P2 C7B C8B -152.3(3) . . . . ?

Pd P2 C7B C8B 79.5(3) . . . . ?

C12B C7B C8B C9B 0.3(6) . . . . ?

P2 C7B C8B C9B -175.8(3) . . . . ?

C7B C8B C9B C10B -0.6(6) . . . . ?

C8B C9B C10B C11B 0.0(8) . . . . ?

C9B C10B C11B C12B 0.9(8) . . . . ?

C10B C11B C12B C7B -1.1(8) . . . . ?

C8B C7B C12B C11B 0.5(7) . . . . ?

P2 C7B C12B C11B 176.5(4) . . . . ?

C7A P1 C1A C2A 131.6(3) . . . . ?

C1 P1 C1A C2A -119.0(3) . . . . ?

Pd P1 C1A C2A 9.1(3) . . . . ?

C7A P1 C1A C6A -49.3(3) . . . . ?

C1 P1 C1A C6A 60.1(3) . . . . ?

Pd P1 C1A C6A -171.8(2) . . . . ?

C6A C1A C2A C3A 0.0(6) . . . . ?

P1 C1A C2A C3A 179.1(3) . . . . ?

C1A C2A C3A C4A 1.2(6) . . . . ?

C2A C3A C4A C5A -1.3(7) . . . . ?

C3A C4A C5A C6A 0.2(7) . . . . ?

C2A C1A C6A C5A -1.1(5) . . . . ?

352

P1 C1A C6A C5A 179.8(3) . . . . ?

C4A C5A C6A C1A 1.0(6) . . . . ?

C1A P1 C7A C8A 139.8(3) . . . . ?

C1 P1 C7A C8A 32.6(4) . . . . ?

Pd P1 C7A C8A -98.2(3) . . . . ?

C1A P1 C7A C12A -43.2(3) . . . . ?

C1 P1 C7A C12A -150.3(3) . . . . ?

Pd P1 C7A C12A 78.8(3) . . . . ?

C12A C7A C8A C9A 2.0(6) . . . . ?

P1 C7A C8A C9A 179.0(4) . . . . ?

C7A C8A C9A C10A -1.7(8) . . . . ?

C8A C9A C10A C11A 0.6(8) . . . . ?

C9A C10A C11A C12A 0.2(7) . . . . ?

C10A C11A C12A C7A 0.1(6) . . . . ?

C8A C7A C12A C11A -1.2(6) . . . . ?

P1 C7A C12A C11A -178.3(3) . . . . ?

A4.9-{[Pd(CH2 – N(CH3)2) (Cl)C=C(Ph)] (µ-Cl)]}2 (cyPd8)

#\#CIF_1.1


# Created on 2009-10-02 at 10:28:16





# CIF files read : umc4 dreduc psi_scan shelxa struct


353

data_global

#------------------ AUDIT DETAILS -------------------------------------------#











;



Glasgow G12 8QQ

Scotland UK

;







;


354



;



--#
















_journal_year ?

_journal_volume ?

_journal_issue ?






355

_publ_section_title

;

?

;


;

?

;

loop_

_publ_author_name



;



Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#


;


?

;


;


?

356

;


;


?

;


;

?

;


;

?

;



;


Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.





357










The Netherlands.











358

A24, 351-359



Volume C.












34, 824-828


35, 281.




;


359

;


;


;

?

;


;




;


data_umc4




_chemical_formula_moiety 'C23 H26 Cl6 N5 Pd2'

_chemical_formula_sum 'C23 H26 Cl6 N5 Pd2'




_symmetry_space_group_name_H-M 'P 21/c'

loop_

360


'x, y, z'

'-x, y+1/2, -z+1/2'

'-x, -y, -z'

'x, -y-1/2, z-1/2'


























361







_diffrn_measurement_method 'non-profiled omega scans'




loop_




-6 3 -5

-4 3 8

-6 -5 -2





_diffrn_reflns_limit_k_min 0








0.998

362


0.998






















Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^






363









loop_

_atom_type_symbol










loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type




364



Pd1 Pd 0.38911(5) -0.04132(7) 0.24279(4) 0.0485(2) Uani 1 d . . .

Pd2 Pd 0.25719(5) 0.05516(7) 0.35954(4) 0.0501(2) Uani 1 d . . .

Cl1 Cl 0.41202(18) 0.0001(3) 0.38488(15) 0.0748(9) Uani 1 d . . .

Cl2 Cl 0.4213(2) -0.2278(3) 0.01762(17) 0.0852(9) Uani 1 d . . .

Cl3 Cl -0.00890(19) 0.1563(3) 0.41486(18) 0.0915(11) Uani 1 d . . .

Cl4 Cl -0.2546(3) 0.1445(4) 0.1462(2) 0.1469(17) Uani 1 d . . .

Cl5 Cl -0.2227(3) 0.2343(3) 0.3010(2) 0.1321(15) Uani 1 d . . .

Cl6 Cl -0.1910(3) -0.0041(3) 0.2713(2) 0.1053(12) Uani 1 d . . .

N1 N 0.2862(5) 0.0721(8) 0.2457(5) 0.060(2) Uani 1 d . . .

N2 N 0.2663(6) 0.1513(10) 0.2046(6) 0.072(3) Uani 1 d . . .

N3 N 0.2447(7) 0.2284(10) 0.1646(7) 0.099(4) Uani 1 d . . .

N4 N 0.4898(5) -0.1627(7) 0.2455(5) 0.056(2) Uani 1 d . . .

N5 N 0.2299(6) 0.0226(7) 0.4726(4) 0.057(2) Uani 1 d . . .

C C -0.1853(8) 0.1367(10) 0.2347(7) 0.083(4) Uani 1 d . . .

C1A C 0.3283(7) -0.0013(8) 0.0671(5) 0.050(2) Uani 1 d . . .

C2A C 0.3730(8) 0.0716(9) 0.0220(6) 0.074(3) Uani 1 d . . .

H2A H 0.4337 0.0744 0.0312 0.088 Uiso 1 calc R . .

C3A C 0.3298(12) 0.1406(12) -0.0364(7) 0.108(5) Uani 1 d . . .

H3A H 0.361 0.1926 -0.0639 0.13 Uiso 1 calc R . .

C4A C 0.2403(13) 0.1321(13) -0.0539(8) 0.113(6) Uani 1 d . . .

H4A H 0.2109 0.1731 -0.0961 0.136 Uiso 1 calc R . .

C5A C 0.1954(9) 0.0620(13) -0.0079(9) 0.102(4) Uani 1 d . . .

H5A H 0.1348 0.0583 -0.0182 0.122 Uiso 1 calc R . .

C6A C 0.2374(8) -0.0027(11) 0.0528(7) 0.083(4) Uani 1 d . . .

H6A H 0.2053 -0.0475 0.0843 0.099 Uiso 1 calc R . .

C7A C 0.3765(6) -0.0734(8) 0.1278(5) 0.047(2) Uani 1 d . . .

C8A C 0.4188(7) -0.1674(9) 0.1122(6) 0.061(3) Uani 1 d . . .

C9A C 0.4695(7) -0.2400(10) 0.1764(6) 0.076(3) Uani 1 d . . .

H9A1 H 0.4347 -0.3059 0.1897 0.092 Uiso 1 calc R . .

H9A2 H 0.5229 -0.2692 0.159 0.092 Uiso 1 calc R . .

C10A C 0.5018(8) -0.2349(10) 0.3184(6) 0.086(4) Uani 1 d . . .

365

H10A H 0.5418 -0.2973 0.312 0.129 Uiso 1 calc R . .

H10B H 0.4465 -0.2667 0.328 0.129 Uiso 1 calc R . .

H10C H 0.5249 -0.1873 0.3623 0.129 Uiso 1 calc R . .

C11A C 0.5708(7) -0.0976(10) 0.2401(7) 0.081(4) Uani 1 d . . .

H11A H 0.6191 -0.1509 0.2426 0.122 Uiso 1 calc R . .

H11B H 0.5804 -0.0434 0.2831 0.122 Uiso 1 calc R . .

H11C H 0.5659 -0.0559 0.191 0.122 Uiso 1 calc R . .

C1B C 0.0852(6) 0.1206(9) 0.2626(6) 0.053(3) Uani 1 d . . .

C2B C 0.0656(6) 0.0273(10) 0.2119(6) 0.069(3) Uani 1 d . . .

H2B H 0.0822 -0.0477 0.228 0.083 Uiso 1 calc R . .

C3B C 0.0206(8) 0.0460(15) 0.1359(7) 0.100(4) Uani 1 d . . .

H3B H 0.0082 -0.0162 0.1015 0.12 Uiso 1 calc R . .

C4B C -0.0045(9) 0.1559(17) 0.1134(7) 0.101(5) Uani 1 d . . .

H4B H -0.036 0.1687 0.0641 0.121 Uiso 1 calc R . .

C5B C 0.0168(8) 0.2483(13) 0.1638(9) 0.091(4) Uani 1 d . . .

H5B H 0.0015 0.3235 0.1471 0.109 Uiso 1 calc R . .

C6B C 0.0602(7) 0.2315(11) 0.2384(7) 0.077(3) Uani 1 d . . .

H6B H 0.0725 0.2945 0.2722 0.092 Uiso 1 calc R . .

C7B C 0.1329(6) 0.1005(8) 0.3425(5) 0.050(2) Uani 1 d . . .

C8B C 0.0994(6) 0.1115(9) 0.4091(6) 0.059(3) Uani 1 d . . .

C9B C 0.1528(6) 0.0934(10) 0.4877(5) 0.067(3) Uani 1 d . . .

H9B1 H 0.1714 0.1677 0.5112 0.081 Uiso 1 calc R . .

H9B2 H 0.1189 0.0526 0.5233 0.081 Uiso 1 calc R . .

C10B C 0.2071(8) -0.1033(10) 0.4775(6) 0.082(4) Uani 1 d . . .

H10D H 0.2538 -0.1498 0.4619 0.123 Uiso 1 calc R . .

H10E H 0.1543 -0.1189 0.4431 0.123 Uiso 1 calc R . .

H10F H 0.1986 -0.1221 0.5307 0.123 Uiso 1 calc R . .

C11B C 0.3025(7) 0.0505(10) 0.5352(6) 0.081(3) Uani 1 d . . .

H11D H 0.3194 0.1305 0.5304 0.121 Uiso 1 calc R . .

H11E H 0.3515 0.0009 0.5297 0.121 Uiso 1 calc R . .

H11F H 0.2835 0.0383 0.5859 0.121 Uiso 1 calc R . .

loop_

366








Pd1 0.0485(5) 0.0511(5) 0.0462(4) 0.0059(4) 0.0070(3) 0.0040(4)

Pd2 0.0520(5) 0.0593(5) 0.0397(4) -0.0009(4) 0.0082(3) -0.0015(4)

Cl1 0.0704(18) 0.098(2) 0.0569(15) 0.0035(15) 0.0094(14) -0.0007(16)

Cl2 0.097(2) 0.084(2) 0.0742(19) -0.0228(17) 0.0074(16) 0.0028(19)

Cl3 0.0606(18) 0.135(3) 0.083(2) -0.008(2) 0.0249(16) 0.008(2)

Cl4 0.206(5) 0.143(4) 0.088(3) 0.020(3) 0.005(3) 0.023(4)

Cl5 0.145(4) 0.103(3) 0.146(3) -0.039(3) 0.005(3) 0.045(3)

Cl6 0.134(3) 0.075(2) 0.108(3) 0.0149(19) 0.022(2) 0.009(2)

N1 0.063(6) 0.064(6) 0.054(5) 0.010(5) 0.010(4) 0.018(5)

N2 0.078(7) 0.065(7) 0.076(7) 0.006(6) 0.014(6) -0.001(6)

N3 0.099(9) 0.084(8) 0.115(9) 0.027(7) 0.022(7) -0.001(7)

N4 0.061(6) 0.053(5) 0.051(5) 0.010(4) -0.004(4) 0.009(5)

N5 0.076(6) 0.058(6) 0.039(4) 0.003(4) 0.011(4) -0.001(5)

C 0.108(10) 0.057(8) 0.083(8) 0.008(7) 0.014(7) 0.013(7)

C1A 0.064(7) 0.046(6) 0.040(5) -0.004(4) 0.009(5) -0.003(5)

C2A 0.099(9) 0.072(8) 0.051(6) 0.012(6) 0.014(6) -0.002(7)

C3A 0.185(17) 0.086(10) 0.055(8) 0.026(7) 0.021(10) 0.015(12)

C4A 0.181(18) 0.092(12) 0.055(8) -0.007(8) -0.030(10) 0.052(13)

C5A 0.077(9) 0.128(13) 0.094(10) 0.014(10) -0.013(8) 0.015(10)

C6A 0.078(9) 0.093(10) 0.071(8) 0.009(7) -0.014(7) -0.003(7)

C7A 0.037(5) 0.049(7) 0.055(6) 0.009(5) 0.004(4) 0.001(5)

C8A 0.066(7) 0.063(8) 0.053(6) 0.000(6) 0.002(5) -0.010(6)

C9A 0.072(8) 0.080(9) 0.074(8) -0.006(7) 0.001(6) 0.010(7)

C10A 0.109(10) 0.079(9) 0.072(8) 0.022(7) 0.022(7) 0.044(8)

C11A 0.051(7) 0.096(10) 0.095(9) -0.005(7) 0.003(6) 0.007(7)

C1B 0.055(6) 0.050(7) 0.056(6) 0.006(5) 0.013(5) -0.005(5)

367

C2B 0.061(7) 0.080(9) 0.061(6) -0.007(6) -0.008(5) -0.003(6)

C3B 0.076(9) 0.147(14) 0.072(8) -0.024(10) -0.018(7) -0.015(10)

C4B 0.086(10) 0.159(16) 0.055(8) 0.016(10) -0.004(7) 0.022(11)

C5B 0.078(9) 0.097(11) 0.098(10) 0.032(9) 0.010(8) 0.000(8)

C6B 0.075(8) 0.072(9) 0.080(9) 0.013(7) -0.002(7) -0.014(7)

C7B 0.053(6) 0.055(6) 0.044(5) 0.001(5) 0.010(5) 0.000(5)

C8B 0.058(7) 0.057(7) 0.066(7) -0.006(6) 0.019(5) -0.008(5)

C9B 0.065(7) 0.090(9) 0.049(6) -0.011(6) 0.018(5) 0.003(6)

C10B 0.100(10) 0.074(9) 0.072(8) 0.012(7) 0.019(7) 0.011(7)

C11B 0.080(8) 0.108(10) 0.051(6) 0.002(7) -0.007(6) 0.014(8)



;







;

loop_



_geom_bond_distance



Pd1 C7A 1.985(9) . ?

Pd1 N1 2.058(8) . ?

Pd1 N4 2.082(8) . ?

Pd1 Cl1 2.457(3) . ?

368

Pd1 Pd2 3.2178(12) . ?

Pd2 C7B 1.972(9) . ?

Pd2 N1 2.059(8) . ?

Pd2 N5 2.062(7) . ?

Pd2 Cl1 2.455(3) . ?

Cl2 C8A 1.764(10) . ?

Cl3 C8B 1.761(10) . ?

Cl4 C 1.743(12) . ?

Cl5 C 1.743(12) . ?

Cl6 C 1.739(11) . ?

N1 N2 1.166(11) . ?

N2 N3 1.142(11) . ?

N4 C11A 1.467(12) . ?

N4 C9A 1.479(11) . ?

N4 C10A 1.490(11) . ?

N5 C11B 1.485(12) . ?

N5 C9B 1.489(12) . ?

N5 C10B 1.491(12) . ?

C1A C2A 1.379(13) . ?

C1A C6A 1.392(13) . ?

C1A C7A 1.456(12) . ?

C2A C3A 1.378(15) . ?

C2A H2A 0.93 . ?

C3A C4A 1.380(19) . ?

C3A H3A 0.93 . ?

C4A C5A 1.370(18) . ?

C4A H4A 0.93 . ?

C5A C6A 1.372(16) . ?

C5A H5A 0.93 . ?

C6A H6A 0.93 . ?

C7A C8A 1.305(12) . ?

C8A C9A 1.515(13) . ?

C9A H9A1 0.97 . ?

369

C9A H9A2 0.97 . ?

C10A H10A 0.96 . ?

C10A H10B 0.96 . ?

C10A H10C 0.96 . ?

C11A H11A 0.96 . ?

C11A H11B 0.96 . ?

C11A H11C 0.96 . ?

C1B C6B 1.378(13) . ?

C1B C2B 1.387(13) . ?

C1B C7B 1.487(12) . ?

C2B C3B 1.410(14) . ?

C2B H2B 0.93 . ?

C3B C4B 1.360(18) . ?

C3B H3B 0.93 . ?

C4B C5B 1.381(17) . ?

C4B H4B 0.93 . ?

C5B C6B 1.378(15) . ?

C5B H5B 0.93 . ?

C6B H6B 0.93 . ?

C7B C8B 1.312(12) . ?

C8B C9B 1.502(12) . ?

C9B H9B1 0.97 . ?

C9B H9B2 0.97 . ?

C10B H10D 0.96 . ?

C10B H10E 0.96 . ?

C10B H10F 0.96 . ?

C11B H11D 0.96 . ?

C11B H11E 0.96 . ?

C11B H11F 0.96 . ?

loop_



370


_geom_angle




C7A Pd1 N1 99.2(3) . . ?

C7A Pd1 N4 83.0(3) . . ?

N1 Pd1 N4 176.2(3) . . ?

C7A Pd1 Cl1 177.3(3) . . ?

N1 Pd1 Cl1 82.5(2) . . ?

N4 Pd1 Cl1 95.3(2) . . ?

C7A Pd1 Pd2 133.3(3) . . ?

N1 Pd1 Pd2 38.6(2) . . ?

N4 Pd1 Pd2 138.1(2) . . ?

Cl1 Pd1 Pd2 49.04(7) . . ?

C7B Pd2 N1 99.0(3) . . ?

C7B Pd2 N5 83.0(3) . . ?

N1 Pd2 N5 175.0(3) . . ?

C7B Pd2 Cl1 178.3(3) . . ?

N1 Pd2 Cl1 82.6(2) . . ?

N5 Pd2 Cl1 95.5(2) . . ?

C7B Pd2 Pd1 132.6(3) . . ?

N1 Pd2 Pd1 38.6(2) . . ?

N5 Pd2 Pd1 137.5(2) . . ?

Cl1 Pd2 Pd1 49.10(6) . . ?

Pd2 Cl1 Pd1 81.85(9) . . ?

N2 N1 Pd1 128.5(8) . . ?

N2 N1 Pd2 124.9(7) . . ?

Pd1 N1 Pd2 102.8(4) . . ?

N3 N2 N1 178.2(13) . . ?

C11A N4 C9A 110.7(9) . . ?

C11A N4 C10A 108.5(8) . . ?

C9A N4 C10A 109.1(8) . . ?

371

C11A N4 Pd1 107.2(6) . . ?

C9A N4 Pd1 107.5(6) . . ?

C10A N4 Pd1 113.9(6) . . ?

C11B N5 C9B 107.6(8) . . ?

C11B N5 C10B 109.3(8) . . ?

C9B N5 C10B 108.7(8) . . ?

C11B N5 Pd2 114.4(6) . . ?

C9B N5 Pd2 109.0(6) . . ?

C10B N5 Pd2 107.8(6) . . ?

Cl6 C Cl4 107.9(7) . . ?

Cl6 C Cl5 109.1(6) . . ?

Cl4 C Cl5 108.4(6) . . ?

C2A C1A C6A 118.0(10) . . ?

C2A C1A C7A 119.9(10) . . ?

C6A C1A C7A 122.1(9) . . ?

C3A C2A C1A 121.6(12) . . ?

C3A C2A H2A 119.2 . . ?

C1A C2A H2A 119.2 . . ?

C2A C3A C4A 119.8(14) . . ?

C2A C3A H3A 120.1 . . ?

C4A C3A H3A 120.1 . . ?

C5A C4A C3A 118.7(13) . . ?

C5A C4A H4A 120.7 . . ?

C3A C4A H4A 120.7 . . ?

C4A C5A C6A 121.8(13) . . ?

C4A C5A H5A 119.1 . . ?

C6A C5A H5A 119.1 . . ?

C5A C6A C1A 119.8(12) . . ?

C5A C6A H6A 120.1 . . ?

C1A C6A H6A 120.1 . . ?

C8A C7A C1A 123.2(9) . . ?

C8A C7A Pd1 111.4(7) . . ?

C1A C7A Pd1 125.4(7) . . ?

372

C7A C8A C9A 122.2(9) . . ?

C7A C8A Cl2 125.5(8) . . ?

C9A C8A Cl2 112.3(8) . . ?

N4 C9A C8A 106.7(8) . . ?

N4 C9A H9A1 110.4 . . ?

C8A C9A H9A1 110.4 . . ?

N4 C9A H9A2 110.4 . . ?

C8A C9A H9A2 110.4 . . ?

H9A1 C9A H9A2 108.6 . . ?

N4 C10A H10A 109.5 . . ?

N4 C10A H10B 109.5 . . ?

H10A C10A H10B 109.5 . . ?

N4 C10A H10C 109.5 . . ?

H10A C10A H10C 109.5 . . ?

H10B C10A H10C 109.5 . . ?

N4 C11A H11A 109.5 . . ?

N4 C11A H11B 109.5 . . ?

H11A C11A H11B 109.5 . . ?

N4 C11A H11C 109.5 . . ?

H11A C11A H11C 109.5 . . ?

H11B C11A H11C 109.5 . . ?

C6B C1B C2B 119.6(10) . . ?

C6B C1B C7B 120.5(10) . . ?

C2B C1B C7B 119.9(9) . . ?

C1B C2B C3B 120.1(12) . . ?

C1B C2B H2B 119.9 . . ?

C3B C2B H2B 119.9 . . ?

C4B C3B C2B 119.5(13) . . ?

C4B C3B H3B 120.2 . . ?

C2B C3B H3B 120.2 . . ?

C3B C4B C5B 119.8(12) . . ?

C3B C4B H4B 120.1 . . ?

C5B C4B H4B 120.1 . . ?

373

C6B C5B C4B 121.4(13) . . ?

C6B C5B H5B 119.3 . . ?

C4B C5B H5B 119.3 . . ?

C1B C6B C5B 119.5(12) . . ?

C1B C6B H6B 120.2 . . ?

C5B C6B H6B 120.2 . . ?

C8B C7B C1B 125.3(9) . . ?

C8B C7B Pd2 112.2(7) . . ?

C1B C7B Pd2 122.5(6) . . ?

C7B C8B C9B 122.1(9) . . ?

C7B C8B Cl3 123.7(8) . . ?

C9B C8B Cl3 114.1(7) . . ?

N5 C9B C8B 106.2(7) . . ?

N5 C9B H9B1 110.5 . . ?

C8B C9B H9B1 110.5 . . ?

N5 C9B H9B2 110.5 . . ?

C8B C9B H9B2 110.5 . . ?

H9B1 C9B H9B2 108.7 . . ?

N5 C10B H10D 109.5 . . ?

N5 C10B H10E 109.5 . . ?

H10D C10B H10E 109.5 . . ?

N5 C10B H10F 109.5 . . ?

H10D C10B H10F 109.5 . . ?

H10E C10B H10F 109.5 . . ?

N5 C11B H11D 109.5 . . ?

N5 C11B H11E 109.5 . . ?

H11D C11B H11E 109.5 . . ?

N5 C11B H11F 109.5 . . ?

H11D C11B H11F 109.5 . . ?

H11E C11B H11F 109.5 . . ?

loop_


374




_geom_torsion






C7A Pd1 Pd2 C7B 1.7(5) . . . . ?

N1 Pd1 Pd2 C7B 35.8(5) . . . . ?

N4 Pd1 Pd2 C7B -141.4(5) . . . . ?

Cl1 Pd1 Pd2 C7B -180.0(4) . . . . ?

C7A Pd1 Pd2 N1 -34.1(5) . . . . ?

N4 Pd1 Pd2 N1 -177.2(5) . . . . ?

Cl1 Pd1 Pd2 N1 144.2(4) . . . . ?

C7A Pd1 Pd2 N5 141.0(5) . . . . ?

N1 Pd1 Pd2 N5 175.1(5) . . . . ?

N4 Pd1 Pd2 N5 -2.1(5) . . . . ?

Cl1 Pd1 Pd2 N5 -40.7(4) . . . . ?

C7A Pd1 Pd2 Cl1 -178.3(4) . . . . ?

N1 Pd1 Pd2 Cl1 -144.2(4) . . . . ?

N4 Pd1 Pd2 Cl1 38.6(4) . . . . ?

C7B Pd2 Cl1 Pd1 18E1(10) . . . . ?

N1 Pd2 Cl1 Pd1 -21.6(3) . . . . ?

N5 Pd2 Cl1 Pd1 153.7(2) . . . . ?

C7A Pd1 Cl1 Pd2 153(6) . . . . ?

N1 Pd1 Cl1 Pd2 21.6(3) . . . . ?

N4 Pd1 Cl1 Pd2 -155.3(2) . . . . ?

C7A Pd1 N1 N2 -45.8(10) . . . . ?

N4 Pd1 N1 N2 -172(5) . . . . ?

Cl1 Pd1 N1 N2 132.2(10) . . . . ?

Pd2 Pd1 N1 N2 158.7(12) . . . . ?

375

C7A Pd1 N1 Pd2 155.6(4) . . . . ?

N4 Pd1 N1 Pd2 29(5) . . . . ?

Cl1 Pd1 N1 Pd2 -26.5(3) . . . . ?

C7B Pd2 N1 N2 46.2(10) . . . . ?

N5 Pd2 N1 N2 159(3) . . . . ?

Cl1 Pd2 N1 N2 -133.2(10) . . . . ?

Pd1 Pd2 N1 N2 -159.7(12) . . . . ?

C7B Pd2 N1 Pd1 -154.1(4) . . . . ?

N5 Pd2 N1 Pd1 -41(4) . . . . ?

Cl1 Pd2 N1 Pd1 26.5(3) . . . . ?

Pd1 N1 N2 N3 15E1(4) . . . . ?

Pd2 N1 N2 N3 -5E1(4) . . . . ?

C7A Pd1 N4 C11A 92.9(7) . . . . ?

N1 Pd1 N4 C11A -140(5) . . . . ?

Cl1 Pd1 N4 C11A -85.0(6) . . . . ?

Pd2 Pd1 N4 C11A -113.2(6) . . . . ?

C7A Pd1 N4 C9A -26.1(7) . . . . ?

N1 Pd1 N4 C9A 101(5) . . . . ?

Cl1 Pd1 N4 C9A 156.0(6) . . . . ?

Pd2 Pd1 N4 C9A 127.8(6) . . . . ?

C7A Pd1 N4 C10A -147.1(8) . . . . ?

N1 Pd1 N4 C10A -20(5) . . . . ?

Cl1 Pd1 N4 C10A 35.0(7) . . . . ?

Pd2 Pd1 N4 C10A 6.8(9) . . . . ?

C7B Pd2 N5 C11B -144.0(8) . . . . ?

N1 Pd2 N5 C11B 102(4) . . . . ?

Cl1 Pd2 N5 C11B 35.2(7) . . . . ?

Pd1 Pd2 N5 C11B 64.9(8) . . . . ?

C7B Pd2 N5 C9B -23.5(7) . . . . ?

N1 Pd2 N5 C9B -137(4) . . . . ?

Cl1 Pd2 N5 C9B 155.7(6) . . . . ?

Pd1 Pd2 N5 C9B -174.6(5) . . . . ?

C7B Pd2 N5 C10B 94.3(7) . . . . ?

376

N1 Pd2 N5 C10B -19(4) . . . . ?

Cl1 Pd2 N5 C10B -86.5(7) . . . . ?

Pd1 Pd2 N5 C10B -56.8(8) . . . . ?

C6A C1A C2A C3A -0.8(16) . . . . ?

C7A C1A C2A C3A 179.5(10) . . . . ?

C1A C2A C3A C4A -4.0(19) . . . . ?

C2A C3A C4A C5A 6(2) . . . . ?

C3A C4A C5A C6A -2(2) . . . . ?

C4A C5A C6A C1A -2(2) . . . . ?

C2A C1A C6A C5A 3.9(17) . . . . ?

C7A C1A C6A C5A -176.4(11) . . . . ?

C2A C1A C7A C8A -75.5(13) . . . . ?

C6A C1A C7A C8A 104.8(12) . . . . ?

C2A C1A C7A Pd1 103.0(10) . . . . ?

C6A C1A C7A Pd1 -76.8(12) . . . . ?

N1 Pd1 C7A C8A -162.4(7) . . . . ?

N4 Pd1 C7A C8A 14.5(7) . . . . ?

Cl1 Pd1 C7A C8A 67(6) . . . . ?

Pd2 Pd1 C7A C8A -141.6(6) . . . . ?

N1 Pd1 C7A C1A 19.0(8) . . . . ?

N4 Pd1 C7A C1A -164.1(8) . . . . ?

Cl1 Pd1 C7A C1A -112(6) . . . . ?

Pd2 Pd1 C7A C1A 39.8(9) . . . . ?

C1A C7A C8A C9A 179.1(9) . . . . ?

Pd1 C7A C8A C9A 0.5(12) . . . . ?

C1A C7A C8A Cl2 -3.3(15) . . . . ?

Pd1 C7A C8A Cl2 178.1(6) . . . . ?

C11A N4 C9A C8A -86.1(10) . . . . ?

C10A N4 C9A C8A 154.5(8) . . . . ?

Pd1 N4 C9A C8A 30.6(9) . . . . ?

C7A C8A C9A N4 -22.3(14) . . . . ?

Cl2 C8A C9A N4 159.8(7) . . . . ?

C6B C1B C2B C3B 0.2(16) . . . . ?

377

C7B C1B C2B C3B -179.8(10) . . . . ?

C1B C2B C3B C4B -1.0(18) . . . . ?

C2B C3B C4B C5B 2(2) . . . . ?

C3B C4B C5B C6B -3(2) . . . . ?

C2B C1B C6B C5B -0.6(16) . . . . ?

C7B C1B C6B C5B 179.3(10) . . . . ?

C4B C5B C6B C1B 1.9(18) . . . . ?

C6B C1B C7B C8B 69.4(14) . . . . ?

C2B C1B C7B C8B -110.7(12) . . . . ?

C6B C1B C7B Pd2 -109.8(10) . . . . ?

C2B C1B C7B Pd2 70.2(11) . . . . ?

N1 Pd2 C7B C8B -172.0(8) . . . . ?

N5 Pd2 C7B C8B 12.7(8) . . . . ?

Cl1 Pd2 C7B C8B -13(10) . . . . ?

Pd1 Pd2 C7B C8B 166.3(6) . . . . ?

N1 Pd2 C7B C1B 7.2(8) . . . . ?

N5 Pd2 C7B C1B -168.1(8) . . . . ?

Cl1 Pd2 C7B C1B 166(9) . . . . ?

Pd1 Pd2 C7B C1B -14.5(10) . . . . ?

C1B C7B C8B C9B -177.9(9) . . . . ?

Pd2 C7B C8B C9B 1.3(13) . . . . ?

C1B C7B C8B Cl3 -1.7(15) . . . . ?

Pd2 C7B C8B Cl3 177.5(5) . . . . ?

C11B N5 C9B C8B 152.5(8) . . . . ?

C10B N5 C9B C8B -89.3(9) . . . . ?

Pd2 N5 C9B C8B 28.0(9) . . . . ?

C7B C8B C9B N5 -20.6(14) . . . . ?

Cl3 C8B C9B N5 162.9(7) . . . . ?

378

A4.10 - {[Pd (C2, N-dmpa) (Cl) (C1-benzonitrila)]} (cyPd9)

#\#CIF_1.1


# Created on 2009-11-10 at 11:01:21




# Request file : c:\wingx\files\archive.dat

# CIF files read : umca5 dreduc psi_scan struct

#

# CCDC ELECTRONIC DATA DEPOSITION FORM (CIF)

#

# This electronic data deposition form can be used:

#

# (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or

# (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC

#

# A comprehensive archive of CIF resources is maintained by the IUCr

# at its Chester office. This can be accessed

# by anonymous ftp to ftp.iucr.org

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# If data items in this form are not available or not applicable

# then ignore these items

# A few items specific to CCDC input are indicated by _ccdc_

#

# Submission and help information is provided at the end of this form

#-------------------------------------------------------------------------

#1 Global data block identification for start of deposition

379

data_global

#

#-------------------------------------------------------------------------

#2 Person making the deposition

#

_publ_contact_author 'Farrugia, Louis J.'


#-------------------------------------------------------------------------

#3 Publication details

#

# Provide these details if the structure has been published,

# accepted or submitted for publication

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# The CCDC journal deposition number, eg. 182/357,

# should be included only if it has been assigned by the journal

#

loop_

_publ_author_name


_journal_name_full 'private communication'

_journal_volume ?



_journal_year ?

_ccdc_journal_depnumber ?

#

#-------------------------------------------------------------------------

#4 Chemical and physical data

#

380

# Note that the units for melting point are Kelvin

# The compound_id is the identifier for the compound in the published

# paper, eg. 4a, II, etc.

# Provide a brief description of any significant biological activity,

# eg. antimalarial activity

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_ccdc_compound_id ?

_ccdc_biological_activity ?

_ccdc_polymorph ?

_ccdc_chemdiag_type ?

_ccdc_chemdiag_records

;

?

;

#

#-------------------------------------------------------------------------

#5 Other data relating to the structure determination and refinement

#

# Record the radiation type if not X-rays, eg. neutron

# Record the temperature of the data collection (Kelvin)

# if not room-temperature

# Record R_squared if this is the only reliability factor given by

# your refinement program

# Describe briefly any disorder, eg. t-Butyl C31-33 disordered over

# two sites with occupancies 0.6 and 0.4

# Under ccdc_comments record any other important information

_ccdc_temp_data_collection ?

_ccdc_ls_R_squared ?

381

_ccdc_disorder ?

_ccdc_comments

;

?

;

#-------------------------------------------------------------------------

#6 Include your "standard" CIF file here

# It should contain the following data items:

# unit cell parameters and volume, z value, space group symbol,

# R-factor(s), atomic coordinates with standard deviations,

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data_umca5



382

#----------------------------------------------------------------------------#

# CHEMICAL INFORMATION #

#----------------------------------------------------------------------------#

_chemical_name_systematic

;

?

;


_chemical_formula_sum 'C19 H20 Cl2 N2 Pd'


_chemical_compound_source 'synthesis as described'

_chemical_absolute_configuration rm

#----------------------------------------------------------------------------#

# UNIT CELL INFORMATION #

#----------------------------------------------------------------------------#

_symmetry_cell_setting orthorhombic

_symmetry_space_group_name_H-M 'P 21 21 21'

_symmetry_space_group_name_Hall 'P 2ac 2ab'

_symmetry_Int_Tables_number 19

loop_


'x, y, z'

'-x+1/2, -y, z+1/2'

'x+1/2, -y+1/2, -z'

'-x, y+1/2, -z+1/2'





383

_cell_angle_beta 90








_cell_measurement_wavelength 0.71073

#----------------------------------------------------------------------------#

# CRYSTAL INFORMATION #

#----------------------------------------------------------------------------#









_exptl_special_details

;

?

;

#----------------------------------------------------------------------------#

# ABSORPTION CORRECTION #

#----------------------------------------------------------------------------#



384

_exptl_absorpt_process_details

;

North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351

Number of psi-scan sets used was 7

Theta correction was applied.

Averaged transmission function was used.

Fourier smoothing - Window value 5

;



#----------------------------------------------------------------------------#

# DATA COLLECTION #

#----------------------------------------------------------------------------#

_diffrn_source 'Enraf Nonius FR590'

_diffrn_ambient_temperature 293(2)



_diffrn_radiation_monochromator graphite


_diffrn_detector 'scintillation LiI'

_diffrn_detector_dtime 1.195

_diffrn_orient_matrix_type

;

x-axis points to radiation source

the matrix is specified in reciprocal space

;

_diffrn_orient_matrix_ub_11 -0.026059

_diffrn_orient_matrix_ub_12 0.061572




385




_diffrn_orient_matrix_ub_33 0.005369







loop_




-2 -4 -9

2 -5 -1

2 1 -12


_diffrn_reflns_av_unetI/netI 0.0711












0.999


386

0.999




#----------------------------------------------------------------------------#

# COMPUTER PROGRAMS USED #

#----------------------------------------------------------------------------#









#----------------------------------------------------------------------------#

# REFINEMENT INFORMATION #

#----------------------------------------------------------------------------#

_refine_special_details

;

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F^2^, conventional R-factors R are based

on F, with F set to zero for negative F^2^. The threshold expression of

F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F^2^ are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

;


387





_atom_sites_solution_primary direct

_atom_sites_solution_secondary difmap

_atom_sites_solution_hydrogens geom






_refine_ls_R_factor_all 0.0889



_refine_ls_wR_factor_gt 0.0735




_refine_ls_shift/su_mean 0

_refine_ls_abs_structure_details

'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack -0.10(5)



_refine_diff_density_rms 0.115

#----------------------------------------------------------------------------#

# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS

#

#----------------------------------------------------------------------------#

loop_

388

_atom_type_symbol










loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type


_atom_site_symmetry_multiplicity





Pd Pd 0.69686(7) 0.16518(3) 0.302106(14) 0.03070(10) Uani 1 1 d . . .

Cl2 Cl 0.1519(3) 0.35670(17) 0.37641(6) 0.0620(5) Uani 1 1 d . . .

Cl1 Cl 0.9388(3) 0.12674(13) 0.23683(5) 0.0460(4) Uani 1 1 d . . .

N1 N 0.8930(8) -0.0511(5) 0.35545(17) 0.0431(12) Uani 1 1 d . . .

N2 N 0.5455(7) 0.3051(4) 0.26423(14) 0.0334(11) Uani 1 1 d . . .

C1 C 0.8197(11) 0.0332(5) 0.33799(18) 0.0372(12) Uani 1 1 d . . .

C2 C 0.9748(11) -0.1613(6) 0.3763(2) 0.0583(18) Uani 1 1 d . . .

H2A H 1.0796 -0.1417 0.4009 0.07 Uiso 1 1 calc R . .

389

H2B H 1.0462 -0.2078 0.3513 0.07 Uiso 1 1 calc R . .

C3 C 0.7990(12) -0.2368(5) 0.39855(19) 0.0419(13) Uani 1 1 d . . .

C4 C 0.6529(13) -0.1880(6) 0.4297(2) 0.062(2) Uani 1 1 d . . .

H4 H 0.6605 -0.1065 0.4374 0.074 Uiso 1 1 calc R . .

C5 C 0.4953(16) -0.2582(8) 0.4496(3) 0.083(3) Uani 1 1 d . . .

H5 H 0.3973 -0.2248 0.4711 0.1 Uiso 1 1 calc R . .

C6 C 0.4832(18) -0.3770(8) 0.4377(3) 0.086(3) Uani 1 1 d . . .

H6 H 0.375 -0.4243 0.4508 0.104 Uiso 1 1 calc R . .

C7 C 0.6277(17) -0.4276(7) 0.4068(3) 0.081(3) Uani 1 1 d . . .

H7 H 0.6187 -0.509 0.3991 0.097 Uiso 1 1 calc R . .

C8 C 0.7869(14) -0.3574(6) 0.3870(2) 0.0606(19) Uani 1 1 d . . .

H8 H 0.8861 -0.3913 0.366 0.073 Uiso 1 1 calc R . .

C9 C 0.4928(9) 0.2111(5) 0.35500(18) 0.0327(13) Uani 1 1 d . . .

C10 C 0.4967(9) 0.1640(6) 0.40535(18) 0.0362(12) Uani 1 1 d . . .

C11 C 0.6696(11) 0.1800(6) 0.43592(19) 0.0459(15) Uani 1 1 d . . .

H11 H 0.7914 0.2192 0.4247 0.055 Uiso 1 1 calc R . .

C12 C 0.6626(11) 0.1380(6) 0.4832(2) 0.0514(17) Uani 1 1 d . . .

H12 H 0.7781 0.1516 0.5037 0.062 Uiso 1 1 calc R . .

C13 C 0.4894(13) 0.0777(6) 0.4998(2) 0.0549(19) Uani 1 1 d . . .

H13 H 0.4884 0.0485 0.5314 0.066 Uiso 1 1 calc R . .

C14 C 0.3175(13) 0.0593(6) 0.4709(2) 0.0539(16) Uani 1 1 d . . .

H14 H 0.1981 0.0185 0.4825 0.065 Uiso 1 1 calc R . .

C15 C 0.3224(12) 0.1027(5) 0.42352(19) 0.0465(15) Uani 1 1 d . . .

H15 H 0.2048 0.0898 0.4036 0.056 Uiso 1 1 calc R . .

C16 C 0.3522(9) 0.2918(5) 0.3400(2) 0.0389(14) Uani 1 1 d . . .

C17 C 0.3425(9) 0.3378(6) 0.28876(18) 0.0447(14) Uani 1 1 d . . .

H17A H 0.2223 0.3018 0.2719 0.054 Uiso 1 1 calc R . .

H17B H 0.3241 0.4246 0.2887 0.054 Uiso 1 1 calc R . .

C18 C 0.6951(13) 0.4089(5) 0.2648(2) 0.0583(17) Uani 1 1 d . . .

H18A H 0.6368 0.4734 0.2458 0.087 Uiso 1 1 calc R . .

H18B H 0.8302 0.3846 0.2515 0.087 Uiso 1 1 calc R . .

H18C H 0.715 0.4357 0.2975 0.087 Uiso 1 1 calc R . .

C19 C 0.4971(12) 0.2744(6) 0.21326(19) 0.0567(19) Uani 1 1 d . . .

390

H19A H 0.4009 0.207 0.2123 0.085 Uiso 1 1 calc R . .

H19B H 0.6273 0.2538 0.1968 0.085 Uiso 1 1 calc R . .

H19C H 0.432 0.3424 0.1977 0.085 Uiso 1 1 calc R . .

loop_








Pd 0.02738(17) 0.02941(17) 0.03529(17) 0.00212(19) -0.0021(2) -0.0004(2)

Cl2 0.0516(11) 0.0677(12) 0.0668(9) 0.0015(9) 0.0198(8) 0.0149(9)

Cl1 0.0409(9) 0.0448(8) 0.0522(8) -0.0005(7) 0.0091(7) 0.0054(7)

N1 0.041(3) 0.037(3) 0.051(3) 0.008(2) -0.009(3) -0.001(2)

N2 0.028(2) 0.034(2) 0.038(2) 0.004(2) -0.002(2) 0.001(2)

C1 0.037(3) 0.037(3) 0.037(3) -0.001(2) -0.003(3) -0.010(3)

C2 0.058(4) 0.043(3) 0.074(4) 0.017(4) -0.010(4) 0.014(4)

C3 0.048(3) 0.033(3) 0.045(3) 0.012(2) -0.007(4) -0.002(3)

C4 0.073(6) 0.050(4) 0.063(4) 0.002(3) 0.011(4) 0.004(4)

C5 0.068(6) 0.096(7) 0.086(6) 0.027(5) 0.021(5) 0.018(6)

C6 0.084(7) 0.074(6) 0.101(7) 0.040(5) 0.001(6) -0.017(6)

C7 0.108(9) 0.047(4) 0.087(6) 0.015(4) -0.018(6) -0.018(5)

C8 0.081(5) 0.052(4) 0.048(3) -0.002(3) -0.011(4) 0.004(5)

C9 0.030(3) 0.032(3) 0.036(3) 0.001(2) -0.001(2) -0.005(2)

C10 0.035(3) 0.036(3) 0.038(3) 0.001(3) 0.000(2) -0.005(3)

C11 0.040(4) 0.052(4) 0.046(3) -0.001(3) -0.004(3) -0.008(4)

C12 0.051(4) 0.061(4) 0.042(3) -0.002(3) -0.014(3) 0.006(4)

C13 0.076(5) 0.056(4) 0.033(3) 0.005(3) 0.010(4) -0.001(4)

C14 0.053(4) 0.058(4) 0.051(3) 0.012(3) 0.008(4) -0.016(4)

C15 0.038(4) 0.054(4) 0.048(3) 0.005(3) -0.001(3) -0.012(4)

C16 0.031(3) 0.041(3) 0.045(3) -0.005(3) 0.002(3) -0.003(3)

391

C17 0.034(3) 0.048(3) 0.051(3) 0.003(3) 0.004(2) 0.011(3)

C18 0.051(4) 0.035(3) 0.089(5) 0.015(3) -0.010(5) -0.006(4)

C19 0.058(5) 0.070(5) 0.043(3) 0.012(3) -0.010(3) 0.006(4)

#----------------------------------------------------------------------------#

# MOLECULAR GEOMETRY #

#----------------------------------------------------------------------------#


;







;

loop_



_geom_bond_distance



Pd C1 1.928(6) . ?

Pd C9 2.006(5) . ?

Pd N2 2.098(4) . ?

Pd Cl1 2.3929(15) . ?

Cl2 C16 1.761(6) . ?

N1 C1 1.148(7) . ?

N1 C2 1.445(7) . ?

N2 C19 1.481(7) . ?

N2 C18 1.483(8) . ?

392

N2 C17 1.484(7) . ?

C2 C3 1.513(9) . ?

C2 H2A 0.97 . ?

C2 H2B 0.97 . ?

C3 C4 1.367(9) . ?

C3 C8 1.377(8) . ?

C4 C5 1.371(11) . ?

C4 H4 0.93 . ?

C5 C6 1.360(11) . ?

C5 H5 0.93 . ?

C6 C7 1.364(12) . ?

C6 H6 0.93 . ?

C7 C8 1.377(11) . ?

C7 H7 0.93 . ?

C8 H8 0.93 . ?

C9 C16 1.323(8) . ?

C9 C10 1.487(7) . ?

C10 C15 1.379(8) . ?

C10 C11 1.384(8) . ?

C11 C12 1.389(8) . ?

C11 H11 0.93 . ?

C12 C13 1.353(9) . ?

C12 H12 0.93 . ?

C13 C14 1.355(10) . ?

C13 H13 0.93 . ?

C14 C15 1.395(7) . ?

C14 H14 0.93 . ?

C15 H15 0.93 . ?

C16 C17 1.505(8) . ?

C17 H17A 0.97 . ?

C17 H17B 0.97 . ?

C18 H18A 0.96 . ?

C18 H18B 0.96 . ?

393

C18 H18C 0.96 . ?

C19 H19A 0.96 . ?

C19 H19B 0.96 . ?

C19 H19C 0.96 . ?

loop_




_geom_angle




C1 Pd C9 94.1(2) . . ?

C1 Pd N2 176.6(2) . . ?

C9 Pd N2 83.6(2) . . ?

C1 Pd Cl1 90.04(18) . . ?

C9 Pd Cl1 175.43(16) . . ?

N2 Pd Cl1 92.35(12) . . ?

C1 N1 C2 176.6(6) . . ?

C19 N2 C18 108.5(5) . . ?

C19 N2 C17 108.4(5) . . ?

C18 N2 C17 110.2(5) . . ?

C19 N2 Pd 113.4(3) . . ?

C18 N2 Pd 106.5(3) . . ?

C17 N2 Pd 109.8(3) . . ?

N1 C1 Pd 173.8(5) . . ?

N1 C2 C3 111.9(5) . . ?

N1 C2 H2A 109.2 . . ?

C3 C2 H2A 109.2 . . ?

N1 C2 H2B 109.2 . . ?

C3 C2 H2B 109.2 . . ?

H2A C2 H2B 107.9 . . ?

394

C4 C3 C8 119.6(7) . . ?

C4 C3 C2 121.5(6) . . ?

C8 C3 C2 118.9(7) . . ?

C3 C4 C5 120.5(7) . . ?

C3 C4 H4 119.7 . . ?

C5 C4 H4 119.7 . . ?

C6 C5 C4 119.6(9) . . ?

C6 C5 H5 120.2 . . ?

C4 C5 H5 120.2 . . ?

C5 C6 C7 120.8(9) . . ?

C5 C6 H6 119.6 . . ?

C7 C6 H6 119.6 . . ?

C6 C7 C8 119.7(8) . . ?

C6 C7 H7 120.2 . . ?

C8 C7 H7 120.2 . . ?

C3 C8 C7 119.8(8) . . ?

C3 C8 H8 120.1 . . ?

C7 C8 H8 120.1 . . ?

C16 C9 C10 122.9(5) . . ?

C16 C9 Pd 111.5(4) . . ?

C10 C9 Pd 125.6(4) . . ?

C15 C10 C11 117.3(5) . . ?

C15 C10 C9 120.1(5) . . ?

C11 C10 C9 122.6(5) . . ?

C10 C11 C12 120.5(6) . . ?

C10 C11 H11 119.8 . . ?

C12 C11 H11 119.8 . . ?

C13 C12 C11 120.7(6) . . ?

C13 C12 H12 119.7 . . ?

C11 C12 H12 119.7 . . ?

C12 C13 C14 120.6(6) . . ?

C12 C13 H13 119.7 . . ?

C14 C13 H13 119.7 . . ?

395

C13 C14 C15 119.0(7) . . ?

C13 C14 H14 120.5 . . ?

C15 C14 H14 120.5 . . ?

C10 C15 C14 122.0(7) . . ?

C10 C15 H15 119 . . ?

C14 C15 H15 119 . . ?

C9 C16 C17 123.5(5) . . ?

C9 C16 Cl2 124.7(4) . . ?

C17 C16 Cl2 111.8(4) . . ?

N2 C17 C16 108.2(4) . . ?

N2 C17 H17A 110.1 . . ?

C16 C17 H17A 110.1 . . ?

N2 C17 H17B 110.1 . . ?

C16 C17 H17B 110.1 . . ?

H17A C17 H17B 108.4 . . ?

N2 C18 H18A 109.5 . . ?

N2 C18 H18B 109.5 . . ?

H18A C18 H18B 109.5 . . ?

N2 C18 H18C 109.5 . . ?

H18A C18 H18C 109.5 . . ?

H18B C18 H18C 109.5 . . ?

N2 C19 H19A 109.5 . . ?

N2 C19 H19B 109.5 . . ?

H19A C19 H19B 109.5 . . ?

N2 C19 H19C 109.5 . . ?

H19A C19 H19C 109.5 . . ?

H19B C19 H19C 109.5 . . ?

396

A4,11 - {[Pd(C2, N-dmba)(N3)]2(µ-dppe)} (cyPd10)

#\#CIF_1.1


# Created on 2009-06-13 at 09:48:35





# CIF files read : umca1 dreduc psi_scan shelxa struct


data_global

#------------------ AUDIT DETAILS -------------------------------------------#









_publ_contact_author_name 'Gambardella,M.T.P'


;

397

Instituto de Qu\´imica de S\~ao Carlos-USP,

Universidade de S\~ao Paulo,

Av. Trabalhador S\~aocarlense, 400,

Caixa Postal 780, 13560-970,

S\~ao Carlos - SP- Brazil.

;







;




;

_publ_requested_category FM


--#










398







_journal_year ?

_journal_volume ?

_journal_issue ?






_publ_section_title

;

?

;


;

?

;

loop_

_publ_author_name



;



399

Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#


;


?

;


;


?

;


;


?

;


;

?

;


;

?

;

400



;


Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.














The Netherlands.


401










A24, 351-359



Volume C.










402



34, 824-828


35, 281.




;


;


;


;

?

;


;




;


data_umca1

403





_chemical_formula_sum 'C23 H26 N4 P Pd'


_chemical_absolute_configuration unk



_symmetry_space_group_name_H-M 'P 21'

loop_


'x, y, z'

'-x, y+1/2, -z'













404
























loop_




2 -8 4

-3 -10 1

-4 4 4

405





_diffrn_reflns_limit_k_min 0








0.999


0.999














406
















_refine_ls_abs_structure_details

'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack 0.03(3)





loop_

_atom_type_symbol








407



loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type






Pd1 Pd 0.59841(7) 0.33138(2) 0.36670(4) 0.04250(14) Uani 1 d . . .

Pd2 Pd 0.93500(7) 0.06422(2) 0.16765(4) 0.04446(15) Uani 1 d . . .

P1 P 0.7051(2) 0.24570(8) 0.42169(14) 0.0371(4) Uani 1 d . . .

P2 P 0.8055(2) 0.14533(8) 0.10930(14) 0.0360(4) Uani 1 d . . .

N1A N 0.6779(11) 0.3257(4) 0.2058(6) 0.097(3) Uani 1 d . . .

N2A N 0.6250(11) 0.3336(5) 0.1175(7) 0.081(3) Uani 1 d . . .

N3A1 N 0.543(2) 0.3330(12) 0.0164(13) 0.106(8) Uani 0.54 d P . .

N3A2 N 0.639(3) 0.3614(11) 0.027(2) 0.109(9) Uani 0.46 d P . .

N4A N 0.4922(8) 0.4133(3) 0.3267(5) 0.0509(16) Uani 1 d . . .

N1B N 0.9159(9) 0.0544(4) 0.4202(6) 0.061(2) Uani 1 d . . .

N2B N 0.8995(13) 0.0759(4) 0.3403(7) 0.117(4) Uani 1 d . . .

N3B1 N 0.963(6) 0.044(2) 0.518(3) 0.23(3) Uani 0.52 d P . .

N3B2 N 0.901(6) 0.0266(12) 0.498(3) 0.141(18) Uani 0.48 d P . .

N4B N 1.0886(9) -0.0088(3) 0.2062(5) 0.065(2) Uani 1 d . . .

C1A C 0.8736(8) 0.2497(3) 0.5451(6) 0.0417(17) Uani 1 d . . .

C2A C 0.9885(10) 0.2895(4) 0.5377(6) 0.055(2) Uani 1 d . . .

H2A H 0.9752 0.3135 0.4733 0.066 Uiso 1 calc R . .

408

C3A C 1.1253(11) 0.2946(4) 0.6249(8) 0.071(3) Uani 1 d . . .

H3A H 1.2042 0.3214 0.6187 0.085 Uiso 1 calc R . .

C4A C 1.1418(11) 0.2598(4) 0.7199(7) 0.067(2) Uani 1 d . . .

H4A H 1.2327 0.2632 0.7788 0.081 Uiso 1 calc R . .

C5A C 1.0300(10) 0.2208(4) 0.7303(7) 0.063(2) Uani 1 d . . .

H5A H 1.0429 0.198 0.7965 0.076 Uiso 1 calc R . .

C6A C 0.8937(10) 0.2144(4) 0.6414(6) 0.053(2) Uani 1 d . . .

H6A H 0.8175 0.1866 0.6471 0.064 Uiso 1 calc R . .

C7A C 0.5612(9) 0.1937(3) 0.4550(5) 0.0401(17) Uani 1 d . . .

C8A C 0.4026(9) 0.2086(4) 0.4543(6) 0.052(2) Uani 1 d . . .

H8A H 0.3701 0.2461 0.4414 0.062 Uiso 1 calc R . .

C9A C 0.2930(10) 0.1683(4) 0.4725(8) 0.062(2) Uani 1 d . . .

H9A H 0.1863 0.1786 0.472 0.075 Uiso 1 calc R . .

C10A C 0.3395(11) 0.1126(4) 0.4915(7) 0.069(3) Uani 1 d . . .

H10A H 0.2646 0.0856 0.5044 0.082 Uiso 1 calc R . .

C11A C 0.4936(13) 0.0974(4) 0.4915(8) 0.069(3) Uani 1 d . . .

H11A H 0.5245 0.0598 0.5043 0.082 Uiso 1 calc R . .

C12A C 0.6062(10) 0.1372(4) 0.4725(6) 0.056(2) Uani 1 d . . .

H12A H 0.7119 0.1262 0.4713 0.067 Uiso 1 calc R . .

C13A C 0.5367(9) 0.3483(3) 0.5235(6) 0.0423(19) Uani 1 d . . .

C14A C 0.5930(9) 0.3237(4) 0.6333(6) 0.050(2) Uani 1 d . . .

H14A H 0.6588 0.2918 0.6397 0.061 Uiso 1 calc R . .

C15A C 0.5498(10) 0.3474(4) 0.7323(6) 0.061(3) Uani 1 d . . .

H15A H 0.5872 0.3305 0.8046 0.073 Uiso 1 calc R . .

C16A C 0.4558(10) 0.3937(4) 0.7275(7) 0.056(2) Uani 1 d . . .

H16A H 0.4307 0.4091 0.7953 0.067 Uiso 1 calc R . .

C17A C 0.3979(10) 0.4176(4) 0.6204(8) 0.062(2) Uani 1 d . . .

H17A H 0.3319 0.4494 0.6161 0.075 Uiso 1 calc R . .

C18A C 0.4357(9) 0.3954(3) 0.5176(6) 0.0470(18) Uani 1 d . . .

C19A C 0.3631(10) 0.4188(3) 0.3970(7) 0.056(2) Uani 1 d . . .

H19A H 0.3341 0.4587 0.4032 0.067 Uiso 1 calc R . .

C20A C 0.2129(10) 0.3842(4) 0.3477(8) 0.077(3) Uani 1 d . . .

H20A H 0.168 0.3971 0.2703 0.115 Uiso 1 calc R . .

409

H20B H 0.1344 0.3886 0.397 0.115 Uiso 1 calc R . .

H20C H 0.2417 0.345 0.3449 0.115 Uiso 1 calc R . .

C21A C 0.6208(12) 0.4569(4) 0.3655(8) 0.086(3) Uani 1 d . . .

H21A H 0.7121 0.4493 0.3296 0.128 Uiso 1 calc R . .

H21B H 0.6537 0.4554 0.449 0.128 Uiso 1 calc R . .

H21C H 0.5788 0.4938 0.3428 0.128 Uiso 1 calc R . .

C22A C 0.4253(13) 0.4255(4) 0.2021(7) 0.088(4) Uani 1 d . . .

H22A H 0.3664 0.3932 0.1669 0.132 Uiso 1 calc R . .

H22B H 0.512 0.4338 0.1619 0.132 Uiso 1 calc R . .

H22C H 0.354 0.4575 0.1968 0.132 Uiso 1 calc R . .

C23A C 0.8093(9) 0.2088(3) 0.3171(6) 0.0408(17) Uani 1 d . . .

H23A H 0.8806 0.2355 0.2892 0.049 Uiso 1 calc R . .

H23B H 0.8762 0.1791 0.3588 0.049 Uiso 1 calc R . .

C1B C 0.6404(8) 0.1381(3) -0.0143(5) 0.0378(16) Uani 1 d . . .

C2B C 0.6116(10) 0.1705(4) -0.1133(6) 0.057(2) Uani 1 d . . .

H2B H 0.6825 0.1998 -0.1212 0.068 Uiso 1 calc R . .

C3B C 0.4828(12) 0.1612(5) -0.2004(7) 0.076(3) Uani 1 d . . .

H3B H 0.4672 0.1839 -0.2668 0.091 Uiso 1 calc R . .

C4B C 0.3750(10) 0.1184(5) -0.1914(8) 0.072(3) Uani 1 d . . .

H4B H 0.2863 0.1122 -0.2509 0.086 Uiso 1 calc R . .

C5B C 0.4004(11) 0.0859(5) -0.0949(8) 0.079(3) Uani 1 d . . .

H5B H 0.3281 0.0569 -0.0881 0.095 Uiso 1 calc R . .

C6B C 0.5313(10) 0.0946(4) -0.0061(7) 0.062(2) Uani 1 d . . .

H6B H 0.547 0.0713 0.0596 0.074 Uiso 1 calc R . .

C7B C 0.9470(10) 0.1970(3) 0.0743(6) 0.0432(18) Uani 1 d . . .

C8B C 0.9017(12) 0.2524(4) 0.0446(7) 0.066(2) Uani 1 d . . .

H8B H 0.7936 0.2626 0.0368 0.08 Uiso 1 calc R . .

C9B C 1.0106(16) 0.2917(5) 0.0267(9) 0.086(3) Uani 1 d . . .

H9B H 0.9767 0.3284 0.0061 0.103 Uiso 1 calc R . .

C10B C 1.1736(14) 0.2777(5) 0.0390(9) 0.084(3) Uani 1 d . . .

H10B H 1.2484 0.3049 0.0267 0.1 Uiso 1 calc R . .

C11B C 1.2228(12) 0.2235(5) 0.0693(9) 0.086(3) Uani 1 d . . .

H11B H 1.3312 0.2135 0.0777 0.103 Uiso 1 calc R . .

410

C12B C 1.1103(11) 0.1843(4) 0.0869(8) 0.064(2) Uani 1 d . . .

H12B H 1.1444 0.1477 0.1082 0.076 Uiso 1 calc R . .

C13B C 0.9663(9) 0.0448(3) 0.0042(6) 0.0427(19) Uani 1 d . . .

C14B C 0.9420(9) 0.0765(4) -0.0980(6) 0.048(2) Uani 1 d . . .

H14B H 0.9085 0.1139 -0.0954 0.058 Uiso 1 calc R . .

C15B C 0.9655(9) 0.0547(4) -0.2026(6) 0.051(2) Uani 1 d . . .

H15B H 0.943 0.0767 -0.2699 0.061 Uiso 1 calc R . .

C16B C 1.0212(11) 0.0013(4) -0.2085(7) 0.060(2) Uani 1 d . . .

H16B H 1.0368 -0.0131 -0.2798 0.072 Uiso 1 calc R . .

C17B C 1.0551(10) -0.0321(4) -0.1089(6) 0.053(2) Uani 1 d . . .

H17B H 1.0978 -0.0682 -0.1118 0.063 Uiso 1 calc R . .

C18B C 1.0237(10) -0.0101(3) -0.0035(6) 0.0487(19) Uani 1 d . . .

C19B C 1.0395(10) -0.0464(3) 0.1035(6) 0.055(2) Uani 1 d . . .

H19B H 1.1242 -0.0746 0.1022 0.066 Uiso 1 calc R . .

C20B C 0.8830(13) -0.0761(4) 0.1086(8) 0.082(3) Uani 1 d . . .

H20D H 0.8995 -0.1022 0.1729 0.122 Uiso 1 calc R . .

H20E H 0.8469 -0.0963 0.0369 0.122 Uiso 1 calc R . .

H20F H 0.803 -0.0487 0.1194 0.122 Uiso 1 calc R . .

C21B C 1.0888(14) -0.0386(4) 0.3176(8) 0.101(5) Uani 1 d . . .

H21D H 0.9796 -0.0466 0.3253 0.152 Uiso 1 calc R . .

H21E H 1.1395 -0.0153 0.3816 0.152 Uiso 1 calc R . .

H21F H 1.1476 -0.0735 0.3184 0.152 Uiso 1 calc R . .

C22B C 1.2586(11) 0.0130(4) 0.2084(8) 0.090(3) Uani 1 d . . .

H22D H 1.2898 0.0376 0.2744 0.136 Uiso 1 calc R . .

H22E H 1.2614 0.0335 0.1376 0.136 Uiso 1 calc R . .

H22F H 1.3321 -0.0184 0.2145 0.136 Uiso 1 calc R . .

C23B C 0.6996(9) 0.1826(3) 0.2119(5) 0.0408(18) Uani 1 d . . .

H23C H 0.6335 0.2123 0.1696 0.049 Uiso 1 calc R . .

H23D H 0.6275 0.1561 0.2397 0.049 Uiso 1 calc R . .

loop_



411






Pd1 0.0524(3) 0.0406(3) 0.0368(3) 0.0010(2) 0.0144(2) 0.0083(3)

Pd2 0.0544(3) 0.0427(3) 0.0363(3) 0.0003(2) 0.0087(2) 0.0164(3)

P1 0.0409(11) 0.0390(11) 0.0324(9) -0.0013(7) 0.0093(8) 0.0021(9)

P2 0.0378(10) 0.0355(10) 0.0354(9) -0.0012(7) 0.0087(8) 0.0066(8)

N1A 0.159(8) 0.086(6) 0.058(4) 0.035(5) 0.055(5) 0.085(6)

N2A 0.106(6) 0.083(6) 0.068(5) 0.014(5) 0.049(5) 0.050(6)

N3A1 0.088(14) 0.19(2) 0.038(8) 0.032(13) 0.017(8) 0.010(16)

N3A2 0.14(2) 0.098(19) 0.114(19) -0.013(14) 0.077(18) 0.019(16)

N4A 0.060(4) 0.040(4) 0.057(4) 0.002(3) 0.024(3) 0.014(3)

N1B 0.075(5) 0.063(6) 0.049(4) -0.011(4) 0.021(4) 0.018(4)

N2B 0.194(10) 0.114(9) 0.051(4) 0.025(5) 0.044(5) 0.108(8)

N3B1 0.22(4) 0.43(7) 0.046(13) -0.02(2) 0.044(17) 0.17(4)

N3B2 0.31(5) 0.075(14) 0.051(15) 0.044(12) 0.06(2) 0.07(2)

N4B 0.086(6) 0.060(5) 0.046(4) 0.001(3) 0.006(4) 0.037(4)

C1A 0.037(4) 0.049(5) 0.041(4) -0.006(3) 0.011(3) -0.004(4)

C2A 0.052(5) 0.065(5) 0.043(4) 0.003(3) -0.002(4) -0.012(4)

C3A 0.049(5) 0.071(6) 0.089(7) -0.008(5) 0.005(5) -0.021(5)

C4A 0.051(5) 0.082(7) 0.062(5) -0.005(5) -0.007(4) 0.004(5)

C5A 0.044(5) 0.083(6) 0.058(5) 0.014(5) -0.003(4) 0.004(5)

C6A 0.053(5) 0.063(6) 0.044(4) 0.010(4) 0.009(4) -0.020(4)

C7A 0.037(4) 0.048(5) 0.036(4) -0.002(3) 0.008(3) -0.002(4)

C8A 0.034(4) 0.055(5) 0.064(5) -0.004(4) 0.006(4) 0.002(4)

C9A 0.029(5) 0.064(6) 0.090(6) 0.001(5) 0.001(4) -0.010(4)

C10A 0.066(6) 0.062(6) 0.081(6) -0.004(4) 0.019(5) -0.034(5)

C11A 0.080(7) 0.043(6) 0.087(6) 0.012(5) 0.026(5) -0.011(6)

C12A 0.056(5) 0.053(6) 0.061(5) 0.007(4) 0.017(4) 0.001(4)

C13A 0.048(5) 0.037(5) 0.045(4) -0.007(3) 0.018(3) -0.005(3)

C14A 0.047(4) 0.059(6) 0.049(4) -0.010(4) 0.018(3) 0.000(4)

412

C15A 0.049(5) 0.095(8) 0.041(4) -0.014(4) 0.018(4) -0.017(5)

C16A 0.044(5) 0.076(6) 0.053(5) -0.030(4) 0.022(4) -0.012(4)

C17A 0.056(5) 0.052(5) 0.088(6) -0.023(5) 0.035(5) -0.003(4)

C18A 0.044(4) 0.036(4) 0.065(4) -0.014(3) 0.020(4) -0.005(3)

C19A 0.062(5) 0.039(4) 0.074(5) 0.004(4) 0.028(4) 0.012(4)

C20A 0.051(5) 0.081(7) 0.093(6) 0.016(5) -0.001(5) 0.003(5)

C21A 0.098(8) 0.050(6) 0.124(9) -0.001(5) 0.062(7) -0.020(6)

C22A 0.139(10) 0.069(6) 0.054(5) 0.016(5) 0.014(6) 0.037(7)

C23A 0.034(4) 0.045(5) 0.046(4) 0.001(3) 0.012(3) 0.003(3)

C1B 0.034(4) 0.046(4) 0.034(3) -0.004(3) 0.005(3) 0.007(3)

C2B 0.049(5) 0.070(6) 0.048(5) 0.007(4) 0.001(4) 0.006(4)

C3B 0.067(7) 0.107(8) 0.049(5) 0.019(5) -0.001(5) 0.004(6)

C4B 0.037(5) 0.114(9) 0.060(5) -0.010(5) -0.004(4) 0.004(6)

C5B 0.053(6) 0.107(9) 0.074(6) -0.008(6) 0.002(5) -0.011(5)

C6B 0.052(5) 0.073(6) 0.059(5) -0.006(4) 0.005(4) -0.006(5)

C7B 0.051(5) 0.038(4) 0.044(4) -0.007(3) 0.019(4) -0.004(4)

C8B 0.080(7) 0.049(6) 0.080(6) 0.000(4) 0.039(5) 0.002(5)

C9B 0.101(9) 0.052(6) 0.115(9) 0.002(5) 0.047(7) 0.004(7)

C10B 0.089(8) 0.066(7) 0.102(7) -0.004(6) 0.032(6) -0.033(6)

C11B 0.046(6) 0.091(8) 0.119(8) -0.004(7) 0.012(6) -0.016(6)

C12B 0.046(5) 0.059(6) 0.084(6) 0.007(4) 0.010(5) -0.009(5)

C13B 0.037(4) 0.051(5) 0.042(4) -0.010(3) 0.013(3) 0.003(3)

C14B 0.046(4) 0.056(6) 0.044(4) -0.008(4) 0.013(3) 0.011(4)

C15B 0.045(4) 0.063(6) 0.048(4) -0.011(4) 0.018(3) -0.004(4)

C16B 0.070(6) 0.068(6) 0.047(4) -0.018(4) 0.021(4) -0.008(5)

C17B 0.054(5) 0.047(5) 0.060(5) -0.014(4) 0.017(4) 0.002(4)

C18B 0.049(5) 0.045(5) 0.053(4) -0.004(3) 0.014(4) 0.000(4)

C19B 0.063(6) 0.041(4) 0.064(5) -0.009(4) 0.017(4) 0.012(4)

C20B 0.099(8) 0.060(6) 0.093(7) 0.013(5) 0.040(6) 0.004(6)

C21B 0.164(12) 0.087(8) 0.061(6) 0.020(5) 0.039(6) 0.082(8)

C22B 0.067(7) 0.093(8) 0.096(7) -0.022(6) -0.020(6) 0.036(6)

C23B 0.036(4) 0.048(5) 0.039(4) -0.011(3) 0.008(3) 0.012(3)

413



;







;

loop_



_geom_bond_distance



Pd1 C13A 2.032(7) . ?

Pd1 N1A 2.111(6) . ?

Pd1 N4A 2.147(6) . ?

Pd1 P1 2.2583(19) . ?

Pd2 C13B 2.023(7) . ?

Pd2 N2B 2.107(7) . ?

Pd2 N4B 2.153(6) . ?

Pd2 P2 2.2466(19) . ?

P1 C7A 1.820(7) . ?

P1 C1A 1.822(7) . ?

P1 C23A 1.849(7) . ?

P2 C7B 1.808(8) . ?

P2 C1B 1.811(6) . ?

P2 C23B 1.845(6) . ?

N1A N2A 1.057(9) . ?

414

N2A N3A1 1.248(17) . ?

N2A N3A2 1.27(3) . ?

N3A1 N3A2 1.04(3) . ?

N4A C22A 1.483(9) . ?

N4A C19A 1.485(9) . ?

N4A C21A 1.501(11) . ?

N1B N2B 1.047(10) . ?

N1B N3B2 1.14(2) . ?

N1B N3B1 1.16(4) . ?

N3B1 N3B2 0.68(9) . ?

N4B C21B 1.477(10) . ?

N4B C19B 1.484(9) . ?

N4B C22B 1.519(12) . ?

C1A C2A 1.364(10) . ?

C1A C6A 1.382(10) . ?

C2A C3A 1.390(10) . ?

C2A H2A 0.93 . ?

C3A C4A 1.365(13) . ?

C3A H3A 0.93 . ?

C4A C5A 1.340(12) . ?

C4A H4A 0.93 . ?

C5A C6A 1.401(10) . ?

C5A H5A 0.93 . ?

C6A H6A 0.93 . ?

C7A C8A 1.381(10) . ?

C7A C12A 1.392(11) . ?

C8A C9A 1.371(11) . ?

C8A H8A 0.93 . ?

C9A C10A 1.379(12) . ?

C9A H9A 0.93 . ?

C10A C11A 1.348(13) . ?

C10A H10A 0.93 . ?

C11A C12A 1.383(11) . ?

415

C11A H11A 0.93 . ?

C12A H12A 0.93 . ?

C13A C18A 1.393(10) . ?

C13A C14A 1.402(10) . ?

C14A C15A 1.391(10) . ?

C14A H14A 0.93 . ?

C15A C16A 1.346(12) . ?

C15A H15A 0.93 . ?

C16A C17A 1.372(12) . ?

C16A H16A 0.93 . ?

C17A C18A 1.398(10) . ?

C17A H17A 0.93 . ?

C18A C19A 1.526(10) . ?

C19A C20A 1.525(11) . ?

C19A H19A 0.98 . ?

C20A H20A 0.96 . ?

C20A H20B 0.96 . ?

C20A H20C 0.96 . ?

C21A H21A 0.96 . ?

C21A H21B 0.96 . ?

C21A H21C 0.96 . ?

C22A H22A 0.96 . ?

C22A H22B 0.96 . ?

C22A H22C 0.96 . ?

C23A C23B 1.520(8) . ?

C23A H23A 0.97 . ?

C23A H23B 0.97 . ?

C1B C2B 1.368(10) . ?

C1B C6B 1.395(10) . ?

C2B C3B 1.356(11) . ?

C2B H2B 0.93 . ?

C3B C4B 1.376(14) . ?

C3B H3B 0.93 . ?

416

C4B C5B 1.345(13) . ?

C4B H4B 0.93 . ?

C5B C6B 1.378(11) . ?

C5B H5B 0.93 . ?

C6B H6B 0.93 . ?

C7B C8B 1.388(11) . ?

C7B C12B 1.389(11) . ?

C8B C9B 1.350(13) . ?

C8B H8B 0.93 . ?

C9B C10B 1.393(14) . ?

C9B H9B 0.93 . ?

C10B C11B 1.372(15) . ?

C10B H10B 0.93 . ?

C11B C12B 1.369(12) . ?

C11B H11B 0.93 . ?

C12B H12B 0.93 . ?

C13B C14B 1.388(10) . ?

C13B C18B 1.394(10) . ?

C14B C15B 1.372(9) . ?

C14B H14B 0.93 . ?

C15B C16B 1.352(12) . ?

C15B H15B 0.93 . ?

C16B C17B 1.388(11) . ?

C16B H16B 0.93 . ?

C17B C18B 1.403(10) . ?

C17B H17B 0.93 . ?

C18B C19B 1.497(10) . ?

C19B C20B 1.505(13) . ?

C19B H19B 0.98 . ?

C20B H20D 0.96 . ?

C20B H20E 0.96 . ?

C20B H20F 0.96 . ?

C21B H21D 0.96 . ?

417

C21B H21E 0.96 . ?

C21B H21F 0.96 . ?

C22B H22D 0.96 . ?

C22B H22E 0.96 . ?

C22B H22F 0.96 . ?

C23B H23C 0.97 . ?

C23B H23D 0.97 . ?

loop_




_geom_angle




C13A Pd1 N1A 171.6(4) . . ?

C13A Pd1 N4A 81.4(3) . . ?

N1A Pd1 N4A 93.1(3) . . ?

C13A Pd1 P1 94.5(2) . . ?

N1A Pd1 P1 91.0(2) . . ?

N4A Pd1 P1 175.82(17) . . ?

C13B Pd2 N2B 174.4(4) . . ?

C13B Pd2 N4B 80.4(3) . . ?

N2B Pd2 N4B 95.4(3) . . ?

C13B Pd2 P2 92.9(2) . . ?

N2B Pd2 P2 91.6(2) . . ?

N4B Pd2 P2 170.2(2) . . ?

C7A P1 C1A 108.6(3) . . ?

C7A P1 C23A 103.9(3) . . ?

C1A P1 C23A 98.5(3) . . ?

C7A P1 Pd1 114.9(3) . . ?

C1A P1 Pd1 112.7(3) . . ?

418

C23A P1 Pd1 116.7(2) . . ?

C7B P2 C1B 109.0(3) . . ?

C7B P2 C23B 104.1(3) . . ?

C1B P2 C23B 99.6(3) . . ?

C7B P2 Pd2 110.0(3) . . ?

C1B P2 Pd2 114.6(2) . . ?

C23B P2 Pd2 118.6(2) . . ?

N2A N1A Pd1 134.9(7) . . ?

N1A N2A N3A1 166.4(18) . . ?

N1A N2A N3A2 145(2) . . ?

N3A1 N2A N3A2 48.8(14) . . ?

N3A2 N3A1 N2A 67(2) . . ?

N3A1 N3A2 N2A 64.5(18) . . ?

C22A N4A C19A 109.9(7) . . ?

C22A N4A C21A 106.3(7) . . ?

C19A N4A C21A 109.7(6) . . ?

C22A N4A Pd1 116.9(5) . . ?

C19A N4A Pd1 106.1(4) . . ?

C21A N4A Pd1 107.8(5) . . ?

N2B N1B N3B2 165(3) . . ?

N2B N1B N3B1 160(3) . . ?

N3B2 N1B N3B1 34(4) . . ?

N1B N2B Pd2 140.0(8) . . ?

N3B2 N3B1 N1B 71(5) . . ?

N3B1 N3B2 N1B 74(5) . . ?

C21B N4B C19B 112.1(7) . . ?

C21B N4B C22B 107.6(7) . . ?

C19B N4B C22B 109.5(7) . . ?

C21B N4B Pd2 117.8(5) . . ?

C19B N4B Pd2 104.3(4) . . ?

C22B N4B Pd2 105.1(5) . . ?

C2A C1A C6A 119.2(7) . . ?

C2A C1A P1 116.3(5) . . ?

419

C6A C1A P1 124.4(6) . . ?

C1A C2A C3A 120.9(8) . . ?

C1A C2A H2A 119.5 . . ?

C3A C2A H2A 119.5 . . ?

C4A C3A C2A 118.9(9) . . ?

C4A C3A H3A 120.6 . . ?

C2A C3A H3A 120.6 . . ?

C5A C4A C3A 121.5(8) . . ?

C5A C4A H4A 119.2 . . ?

C3A C4A H4A 119.2 . . ?

C4A C5A C6A 119.9(8) . . ?

C4A C5A H5A 120 . . ?

C6A C5A H5A 120 . . ?

C1A C6A C5A 119.5(7) . . ?

C1A C6A H6A 120.3 . . ?

C5A C6A H6A 120.3 . . ?

C8A C7A C12A 118.9(7) . . ?

C8A C7A P1 120.6(6) . . ?

C12A C7A P1 120.3(6) . . ?

C9A C8A C7A 120.0(8) . . ?

C9A C8A H8A 120 . . ?

C7A C8A H8A 120 . . ?

C8A C9A C10A 120.6(8) . . ?

C8A C9A H9A 119.7 . . ?

C10A C9A H9A 119.7 . . ?

C11A C10A C9A 120.0(8) . . ?

C11A C10A H10A 120 . . ?

C9A C10A H10A 120 . . ?

C10A C11A C12A 120.6(9) . . ?

C10A C11A H11A 119.7 . . ?

C12A C11A H11A 119.7 . . ?

C11A C12A C7A 119.9(8) . . ?

C11A C12A H12A 120 . . ?

420

C7A C12A H12A 120 . . ?

C18A C13A C14A 118.3(7) . . ?

C18A C13A Pd1 111.8(5) . . ?

C14A C13A Pd1 129.6(6) . . ?

C15A C14A C13A 119.5(8) . . ?

C15A C14A H14A 120.3 . . ?

C13A C14A H14A 120.3 . . ?

C16A C15A C14A 122.5(8) . . ?

C16A C15A H15A 118.8 . . ?

C14A C15A H15A 118.8 . . ?

C15A C16A C17A 118.5(7) . . ?

C15A C16A H16A 120.7 . . ?

C17A C16A H16A 120.7 . . ?

C16A C17A C18A 121.6(8) . . ?

C16A C17A H17A 119.2 . . ?

C18A C17A H17A 119.2 . . ?

C13A C18A C17A 119.6(7) . . ?

C13A C18A C19A 118.0(6) . . ?

C17A C18A C19A 122.4(7) . . ?

N4A C19A C20A 112.9(7) . . ?

N4A C19A C18A 105.6(6) . . ?

C20A C19A C18A 108.1(6) . . ?

N4A C19A H19A 110 . . ?

C20A C19A H19A 110 . . ?

C18A C19A H19A 110 . . ?

C19A C20A H20A 109.5 . . ?

C19A C20A H20B 109.5 . . ?

H20A C20A H20B 109.5 . . ?

C19A C20A H20C 109.5 . . ?

H20A C20A H20C 109.5 . . ?

H20B C20A H20C 109.5 . . ?

N4A C21A H21A 109.5 . . ?

N4A C21A H21B 109.5 . . ?

421

H21A C21A H21B 109.5 . . ?

N4A C21A H21C 109.5 . . ?

H21A C21A H21C 109.5 . . ?

H21B C21A H21C 109.5 . . ?

N4A C22A H22A 109.5 . . ?

N4A C22A H22B 109.5 . . ?

H22A C22A H22B 109.5 . . ?

N4A C22A H22C 109.5 . . ?

H22A C22A H22C 109.5 . . ?

H22B C22A H22C 109.5 . . ?

C23B C23A P1 115.5(4) . . ?

C23B C23A H23A 108.4 . . ?

P1 C23A H23A 108.4 . . ?

C23B C23A H23B 108.4 . . ?

P1 C23A H23B 108.4 . . ?

H23A C23A H23B 107.5 . . ?

C2B C1B C6B 117.2(7) . . ?

C2B C1B P2 127.2(6) . . ?

C6B C1B P2 115.6(5) . . ?

C3B C2B C1B 121.9(9) . . ?

C3B C2B H2B 119 . . ?

C1B C2B H2B 119 . . ?

C2B C3B C4B 120.6(8) . . ?

C2B C3B H3B 119.7 . . ?

C4B C3B H3B 119.7 . . ?

C5B C4B C3B 118.8(8) . . ?

C5B C4B H4B 120.6 . . ?

C3B C4B H4B 120.6 . . ?

C4B C5B C6B 121.3(9) . . ?

C4B C5B H5B 119.3 . . ?

C6B C5B H5B 119.3 . . ?

C5B C6B C1B 120.2(8) . . ?

C5B C6B H6B 119.9 . . ?

422

C1B C6B H6B 119.9 . . ?

C8B C7B C12B 116.9(8) . . ?

C8B C7B P2 122.1(7) . . ?

C12B C7B P2 120.8(6) . . ?

C9B C8B C7B 121.6(10) . . ?

C9B C8B H8B 119.2 . . ?

C7B C8B H8B 119.2 . . ?

C8B C9B C10B 120.4(10) . . ?

C8B C9B H9B 119.8 . . ?

C10B C9B H9B 119.8 . . ?

C11B C10B C9B 119.5(9) . . ?

C11B C10B H10B 120.2 . . ?

C9B C10B H10B 120.2 . . ?

C12B C11B C10B 119.1(10) . . ?

C12B C11B H11B 120.5 . . ?

C10B C11B H11B 120.5 . . ?

C11B C12B C7B 122.5(9) . . ?

C11B C12B H12B 118.7 . . ?

C7B C12B H12B 118.7 . . ?

C14B C13B C18B 116.4(6) . . ?

C14B C13B Pd2 131.3(6) . . ?

C18B C13B Pd2 112.3(5) . . ?

C15B C14B C13B 122.4(8) . . ?

C15B C14B H14B 118.8 . . ?

C13B C14B H14B 118.8 . . ?

C16B C15B C14B 120.4(8) . . ?

C16B C15B H15B 119.8 . . ?

C14B C15B H15B 119.8 . . ?

C15B C16B C17B 120.4(7) . . ?

C15B C16B H16B 119.8 . . ?

C17B C16B H16B 119.8 . . ?

C16B C17B C18B 118.5(8) . . ?

C16B C17B H17B 120.7 . . ?

423

C18B C17B H17B 120.7 . . ?

C13B C18B C17B 121.7(7) . . ?

C13B C18B C19B 117.2(7) . . ?

C17B C18B C19B 120.9(7) . . ?

N4B C19B C18B 107.2(6) . . ?

N4B C19B C20B 111.1(7) . . ?

C18B C19B C20B 111.1(7) . . ?

N4B C19B H19B 109.2 . . ?

C18B C19B H19B 109.2 . . ?

C20B C19B H19B 109.2 . . ?

C19B C20B H20D 109.5 . . ?

C19B C20B H20E 109.5 . . ?

H20D C20B H20E 109.5 . . ?

C19B C20B H20F 109.5 . . ?

H20D C20B H20F 109.5 . . ?

H20E C20B H20F 109.5 . . ?

N4B C21B H21D 109.5 . . ?

N4B C21B H21E 109.5 . . ?

H21D C21B H21E 109.5 . . ?

N4B C21B H21F 109.5 . . ?

H21D C21B H21F 109.5 . . ?

H21E C21B H21F 109.5 . . ?

N4B C22B H22D 109.5 . . ?

N4B C22B H22E 109.5 . . ?

H22D C22B H22E 109.5 . . ?

N4B C22B H22F 109.5 . . ?

H22D C22B H22F 109.5 . . ?

H22E C22B H22F 109.5 . . ?

C23A C23B P2 114.9(4) . . ?

C23A C23B H23C 108.5 . . ?

P2 C23B H23C 108.5 . . ?

C23A C23B H23D 108.5 . . ?

P2 C23B H23D 108.5 . . ?

424

H23C C23B H23D 107.5 . . ?

A4,12 - {[Pd(CH2-N(CH3)2 (Cl)C=C(Ph)]2} (µ-Cl) (µ-N3) (cyPd11)

#\#CIF_1.1


# Created on 2009-10-02 at 12:02:11





# CIF files read : umc7 dreduc psi_scan shelxa struct


data_global

#------------------ AUDIT DETAILS -------------------------------------------#









425



;



Glasgow G12 8QQ

Scotland UK

;







;




;



--#








426









_journal_year ?

_journal_volume ?

_journal_issue ?






_publ_section_title

;

?

;


;

?

;

loop_

_publ_author_name



;

427



Glasgow G12 8QQ

Scotland UK

;

#------------------ TEXT ----------------------------------------------------#


;


?

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;


?

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;


?

;


;

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428

;



;


Acc. Chem. Res. 16, 146-153.


(1993) J. Appl. Cryst. 26, 343-350.














The Netherlands.

429











A24, 351-359



Volume C.








430





34, 824-828


35, 281.




;


;


;


;

?

;


;




;


431

data_umc7





_chemical_formula_sum 'C22 H26 Cl4 N2 Pd2'




_symmetry_space_group_name_H-M 'P 21/a'

loop_


'x, y, z'

'-x+1/2, y+1/2, -z'

'-x, -y, -z'

'x-1/2, -y-1/2, z'











432






















_diffrn_measurement_method 'non-profiled omega/2theta scans'




loop_




433

-2 -4 4

-7 1 2

-2 -4 -8













1


1













434










Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^














loop_

_atom_type_symbol





435






loop_

_atom_site_label


_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z


_atom_site_adp_type






Pd1 Pd 0.621784(17) 0.40325(2) 0.093583(16) 0.03152(7) Uani 1 d . . .

Cl1 Cl 0.54319(7) 0.66308(9) 0.06923(6) 0.04742(19) Uani 1 d . . .

Cl2 Cl 0.96060(7) 0.32964(12) 0.36352(7) 0.0569(2) Uani 1 d . . .

N1 N 0.6922(2) 0.1739(3) 0.1176(2) 0.0376(5) Uani 1 d . . .

C1 C 0.7650(3) 0.5993(3) 0.2914(2) 0.0388(6) Uani 1 d . . .

C2 C 0.8598(3) 0.7029(4) 0.3105(3) 0.0504(8) Uani 1 d . . .

H2 H 0.9163 0.6834 0.2778 0.06 Uiso 1 calc R . .

C3 C 0.8707(3) 0.8356(5) 0.3782(3) 0.0619(10) Uani 1 d . . .

H3 H 0.9352 0.9031 0.3915 0.074 Uiso 1 calc R . .

C4 C 0.7882(4) 0.8667(5) 0.4248(3) 0.0702(12) Uani 1 d . . .

H4 H 0.7966 0.9552 0.4703 0.084 Uiso 1 calc R . .

C5 C 0.6912(4) 0.7682(5) 0.4055(3) 0.0642(10) Uani 1 d . . .

H5 H 0.6344 0.791 0.4372 0.077 Uiso 1 calc R . .

C6 C 0.6794(3) 0.6347(4) 0.3381(3) 0.0495(8) Uani 1 d . . .

436

H6 H 0.614 0.5688 0.3243 0.059 Uiso 1 calc R . .

C7 C 0.7564(2) 0.4517(4) 0.2259(2) 0.0360(6) Uani 1 d . . .

C8 C 0.8343(2) 0.3342(4) 0.2489(2) 0.0400(6) Uani 1 d . . .

C9 C 0.8199(2) 0.1901(4) 0.1782(3) 0.0460(7) Uani 1 d . . .

H9A H 0.8485 0.0947 0.2216 0.055 Uiso 1 calc R . .

H9B H 0.8634 0.2034 0.1281 0.055 Uiso 1 calc R . .

C10 C 0.6763(3) 0.0830(4) 0.0161(3) 0.0530(8) Uani 1 d . . .

H10A H 0.7185 -0.0168 0.0326 0.08 Uiso 1 calc R . .

H10B H 0.7055 0.1457 -0.0314 0.08 Uiso 1 calc R . .

H10C H 0.5948 0.0612 -0.0187 0.08 Uiso 1 calc R . .

C11 C 0.6353(3) 0.0841(4) 0.1857(3) 0.0513(8) Uani 1 d . . .

H11A H 0.6662 -0.0232 0.1979 0.077 Uiso 1 calc R . .

H11B H 0.5525 0.0795 0.1492 0.077 Uiso 1 calc R . .

H11C H 0.6504 0.1381 0.2539 0.077 Uiso 1 calc R . .

loop_








Pd1 0.03323(11) 0.02638(10) 0.03348(11) 0.00018(9) 0.00878(8) 0.00022(9)

Cl1 0.0512(4) 0.0287(3) 0.0483(4) -0.0051(3) -0.0031(3) 0.0045(3)

Cl2 0.0401(4) 0.0705(6) 0.0500(4) 0.0067(4) 0.0007(3) 0.0064(4)

N1 0.0387(12) 0.0296(12) 0.0450(13) -0.0015(10) 0.0141(10) 0.0032(10)

C1 0.0432(15) 0.0383(14) 0.0289(12) 0.0030(11) 0.0036(11) 0.0032(12)

C2 0.0490(17) 0.0429(17) 0.0513(18) 0.0011(14) 0.0053(14) -0.0037(14)

C3 0.065(2) 0.0443(19) 0.059(2) -0.0039(16) -0.0039(19) -0.0088(17)

C4 0.095(3) 0.051(2) 0.0447(19) -0.0125(16) -0.005(2) 0.010(2)

C5 0.085(3) 0.064(2) 0.0435(18) -0.0021(17) 0.0210(18) 0.021(2)

C6 0.0572(19) 0.0504(19) 0.0422(16) 0.0008(14) 0.0178(15) 0.0032(15)

437

C7 0.0354(13) 0.0372(14) 0.0346(13) 0.0032(11) 0.0100(11) -0.0008(11)

C8 0.0328(13) 0.0456(16) 0.0384(14) 0.0043(12) 0.0072(11) 0.0001(12)

C9 0.0373(15) 0.0442(17) 0.0563(18) 0.0025(14) 0.0151(14) 0.0083(13)

C10 0.0572(19) 0.0438(18) 0.0580(19) -0.0134(15) 0.0185(16) 0.0079(15)

C11 0.0541(19) 0.0401(17) 0.062(2) 0.0107(15) 0.0222(16) 0.0004(14)



;







;

loop_



_geom_bond_distance



Pd1 C7 1.993(3) . ?

Pd1 N1 2.068(2) . ?

Pd1 Cl1 2.3378(7) . ?

Pd1 Cl1 2.4597(8) 3_665 ?

Cl1 Pd1 2.4597(8) 3_665 ?

Cl2 C8 1.758(3) . ?

N1 C10 1.483(4) . ?

N1 C11 1.489(4) . ?

N1 C9 1.496(4) . ?

438

C1 C2 1.390(4) . ?

C1 C6 1.392(4) . ?

C1 C7 1.479(4) . ?

C2 C3 1.391(5) . ?

C2 H2 0.93 . ?

C3 C4 1.352(6) . ?

C3 H3 0.93 . ?

C4 C5 1.384(6) . ?

C4 H4 0.93 . ?

C5 C6 1.393(5) . ?

C5 H5 0.93 . ?

C6 H6 0.93 . ?

C7 C8 1.321(4) . ?

C8 C9 1.487(4) . ?

C9 H9A 0.97 . ?

C9 H9B 0.97 . ?

C10 H10A 0.96 . ?

C10 H10B 0.96 . ?

C10 H10C 0.96 . ?

C11 H11A 0.96 . ?

C11 H11B 0.96 . ?

C11 H11C 0.96 . ?

loop_




_geom_angle




C7 Pd1 N1 82.76(11) . . ?

C7 Pd1 Cl1 96.51(9) . . ?

439

N1 Pd1 Cl1 179.13(7) . . ?

C7 Pd1 Cl1 178.70(8) . 3_665 ?

N1 Pd1 Cl1 95.94(7) . 3_665 ?

Cl1 Pd1 Cl1 84.79(3) . 3_665 ?

Pd1 Cl1 Pd1 95.21(3) . 3_665 ?

C10 N1 C11 109.1(2) . . ?

C10 N1 C9 109.3(2) . . ?

C11 N1 C9 109.1(2) . . ?

C10 N1 Pd1 113.93(19) . . ?

C11 N1 Pd1 107.74(18) . . ?

C9 N1 Pd1 107.54(17) . . ?

C2 C1 C6 118.6(3) . . ?

C2 C1 C7 121.1(3) . . ?

C6 C1 C7 120.3(3) . . ?

C1 C2 C3 120.5(3) . . ?

C1 C2 H2 119.8 . . ?

C3 C2 H2 119.8 . . ?

C4 C3 C2 120.3(4) . . ?

C4 C3 H3 119.8 . . ?

C2 C3 H3 119.8 . . ?

C3 C4 C5 120.7(3) . . ?

C3 C4 H4 119.6 . . ?

C5 C4 H4 119.6 . . ?

C4 C5 C6 119.5(4) . . ?

C4 C5 H5 120.2 . . ?

C6 C5 H5 120.2 . . ?

C1 C6 C5 120.4(3) . . ?

C1 C6 H6 119.8 . . ?

C5 C6 H6 119.8 . . ?

C8 C7 C1 124.7(3) . . ?

C8 C7 Pd1 111.7(2) . . ?

C1 C7 Pd1 123.5(2) . . ?

C7 C8 C9 121.5(3) . . ?

440

C7 C8 Cl2 124.6(2) . . ?

C9 C8 Cl2 113.9(2) . . ?

C8 C9 N1 107.0(2) . . ?

C8 C9 H9A 110.3 . . ?

N1 C9 H9A 110.3 . . ?

C8 C9 H9B 110.3 . . ?

N1 C9 H9B 110.3 . . ?

H9A C9 H9B 108.6 . . ?

N1 C10 H10A 109.5 . . ?

N1 C10 H10B 109.5 . . ?

H10A C10 H10B 109.5 . . ?

N1 C10 H10C 109.5 . . ?

H10A C10 H10C 109.5 . . ?

H10B C10 H10C 109.5 . . ?

N1 C11 H11A 109.5 . . ?

N1 C11 H11B 109.5 . . ?

H11A C11 H11B 109.5 . . ?

N1 C11 H11C 109.5 . . ?

H11A C11 H11C 109.5 . . ?

H11B C11 H11C 109.5 . . ?

loop_





_geom_torsion






C7 Pd1 Cl1 Pd1 -179.85(8) . . . 3_665 ?

441

N1 Pd1 Cl1 Pd1 -147(4) . . . 3_665 ?

Cl1 Pd1 Cl1 Pd1 0 3_665 . . 3_665 ?

C7 Pd1 N1 C10 -147.0(2) . . . . ?

Cl1 Pd1 N1 C10 -18E1(10) . . . . ?

Cl1 Pd1 N1 C10 33.1(2) 3_665 . . . ?

C7 Pd1 N1 C11 91.7(2) . . . . ?

Cl1 Pd1 N1 C11 59(4) . . . . ?

Cl1 Pd1 N1 C11 -88.15(19) 3_665 . . . ?

C7 Pd1 N1 C9 -25.80(19) . . . . ?

Cl1 Pd1 N1 C9 -58(4) . . . . ?

Cl1 Pd1 N1 C9 154.33(18) 3_665 . . . ?

C6 C1 C2 C3 2.4(5) . . . . ?

C7 C1 C2 C3 -175.6(3) . . . . ?

C1 C2 C3 C4 -1.1(5) . . . . ?

C2 C3 C4 C5 -0.5(6) . . . . ?

C3 C4 C5 C6 0.7(6) . . . . ?

C2 C1 C6 C5 -2.2(5) . . . . ?

C7 C1 C6 C5 175.9(3) . . . . ?

C4 C5 C6 C1 0.7(5) . . . . ?

C2 C1 C7 C8 59.0(4) . . . . ?

C6 C1 C7 C8 -119.0(3) . . . . ?

C2 C1 C7 Pd1 -123.1(3) . . . . ?

C6 C1 C7 Pd1 58.9(3) . . . . ?

N1 Pd1 C7 C8 13.6(2) . . . . ?

Cl1 Pd1 C7 C8 -166.9(2) . . . . ?

Cl1 Pd1 C7 C8 20(4) 3_665 . . . ?

N1 Pd1 C7 C1 -164.6(2) . . . . ?

Cl1 Pd1 C7 C1 14.9(2) . . . . ?

Cl1 Pd1 C7 C1 -159(3) 3_665 . . . ?

C1 C7 C8 C9 -179.4(3) . . . . ?

Pd1 C7 C8 C9 2.5(4) . . . . ?

C1 C7 C8 Cl2 1.6(4) . . . . ?

Pd1 C7 C8 Cl2 -176.53(16) . . . . ?

442

C7 C8 C9 N1 -24.1(4) . . . . ?

Cl2 C8 C9 N1 155.1(2) . . . . ?

C10 N1 C9 C8 155.8(2) . . . . ?

C11 N1 C9 C8 -84.9(3) . . . . ?

Pd1 N1 C9 C8 31.7(3) . . . . ?

Documents

ANEXO A4 – CIFs das ESTRUTURAS ESTUDADAS - USP€¦ · 180 Johnson, C.K. (1965). ORTEP. Report ORNL-3794. Oak Ridge National