# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\rechne\sar15 #TrackingRef 'SH12a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 I N3' _chemical_formula_weight 377.22 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 0.0000 0.0000 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3307(6) _cell_length_b 18.6233(13) _cell_length_c 9.6719(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.796(3) _cell_angle_gamma 90.00 _cell_volume 1525.72(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 2.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.686 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II duo' _diffrn_measurement_method 'omega psi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32385 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0119 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 30.61 _reflns_number_total 4690 _reflns_number_gt 4336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Kappa Apex II suite, 2008' _computing_cell_refinement 'Bruker Kappa Apex II suite, 2008' _computing_data_reduction 'Bruker Kappa Apex II suite, 2008' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+0.8713P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4690 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0158 _refine_ls_wR_factor_ref 0.0389 _refine_ls_wR_factor_gt 0.0382 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.21786(15) 0.50215(7) 1.44783(14) 0.0180(2) Uani 1 1 d . . . H1 H 0.2204 0.5017 1.5471 0.022 Uiso 1 1 calc R . . C2 C 0.30576(14) 0.54542(6) 1.39692(14) 0.0163(2) Uani 1 1 d . . . C16 C 0.01315(17) 0.40664(7) 1.32538(16) 0.0224(2) Uani 1 1 d . . . H16C H 0.0389 0.3897 1.4290 0.027 Uiso 1 1 calc R . . H16B H 0.0164 0.3661 1.2620 0.027 Uiso 1 1 calc R . . H16A H -0.0928 0.4277 1.2824 0.027 Uiso 1 1 calc R . . C3 C 0.42531(15) 0.59838(6) 1.48585(14) 0.0168(2) Uani 1 1 d . . . C4 C 0.45709(18) 0.60511(8) 1.64033(16) 0.0261(3) Uani 1 1 d . . . H4 H 0.4026 0.5755 1.6824 0.031 Uiso 1 1 calc R . . C5 C 0.5668(2) 0.65437(9) 1.73247(17) 0.0318(3) Uani 1 1 d . . . H5 H 0.5880 0.6579 1.8372 0.038 Uiso 1 1 calc R . . C6 C 0.64567(17) 0.69840(8) 1.67194(17) 0.0259(3) Uani 1 1 d . . . H6 H 0.7187 0.7332 1.7340 0.031 Uiso 1 1 calc R . . C7 C 0.61724(15) 0.69121(7) 1.52047(16) 0.0231(3) Uani 1 1 d . . . H7 H 0.6730 0.7207 1.4794 0.028 Uiso 1 1 calc R . . C8 C 0.50845(15) 0.64164(7) 1.42723(15) 0.0205(2) Uani 1 1 d . . . H8 H 0.4907 0.6372 1.3234 0.025 Uiso 1 1 calc R . . C9 C 0.30576(16) 0.55023(7) 1.12908(14) 0.0203(2) Uani 1 1 d . . . H9A H 0.2712 0.5147 1.0452 0.024 Uiso 1 1 calc R . . H9B H 0.4224 0.5533 1.1722 0.024 Uiso 1 1 calc R . . C10 C 0.23642(15) 0.62266(7) 1.06567(14) 0.0178(2) Uani 1 1 d . . . C11 C 0.10232(16) 0.64922(7) 1.07573(15) 0.0221(2) Uani 1 1 d . . . H11 H 0.0535 0.6226 1.1281 0.027 Uiso 1 1 calc R . . C12 C 0.03929(18) 0.71476(8) 1.00916(17) 0.0280(3) Uani 1 1 d . . . H12 H -0.0510 0.7334 1.0186 0.034 Uiso 1 1 calc R . . C13 C 0.10709(18) 0.75311(8) 0.92921(17) 0.0310(3) Uani 1 1 d . . . H13 H 0.0627 0.7975 0.8825 0.037 Uiso 1 1 calc R . . C14 C 0.23993(17) 0.72620(8) 0.91801(18) 0.0309(3) Uani 1 1 d . . . H14 H 0.2861 0.7520 0.8622 0.037 Uiso 1 1 calc R . . C15 C 0.30617(15) 0.66185(8) 0.98766(16) 0.0246(3) Uani 1 1 d . . . H15 H 0.3994 0.6445 0.9821 0.030 Uiso 1 1 calc R . . N3 N 0.12795(13) 0.46079(6) 1.32931(12) 0.0181(2) Uani 1 1 d . . . N2 N 0.14907(14) 0.47407(6) 1.20567(13) 0.0201(2) Uani 1 1 d . . . N1 N 0.25830(13) 0.52526(6) 1.24775(12) 0.01774(19) Uani 1 1 d . . . I1 I 0.232871(9) 0.412091(4) 0.796580(9) 0.01876(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0211(6) 0.0170(5) 0.0162(5) 0.0008(4) 0.0080(4) 0.0004(4) C2 0.0201(5) 0.0141(5) 0.0151(5) 0.0013(4) 0.0079(4) 0.0036(4) C16 0.0245(6) 0.0190(6) 0.0231(6) -0.0004(5) 0.0095(5) -0.0048(5) C3 0.0187(5) 0.0142(5) 0.0174(5) 0.0011(4) 0.0074(4) 0.0026(4) C4 0.0343(7) 0.0263(6) 0.0203(6) -0.0016(5) 0.0139(6) -0.0080(6) C5 0.0407(8) 0.0340(8) 0.0209(6) -0.0055(6) 0.0130(6) -0.0112(6) C6 0.0241(6) 0.0237(6) 0.0254(6) -0.0021(5) 0.0061(5) -0.0040(5) C7 0.0176(6) 0.0248(6) 0.0253(6) 0.0042(5) 0.0075(5) -0.0010(5) C8 0.0188(5) 0.0239(6) 0.0193(6) 0.0021(5) 0.0086(5) 0.0005(5) C9 0.0294(6) 0.0191(6) 0.0173(6) 0.0003(4) 0.0146(5) 0.0010(5) C10 0.0197(5) 0.0179(5) 0.0138(5) -0.0007(4) 0.0050(4) -0.0029(4) C11 0.0241(6) 0.0254(6) 0.0171(6) -0.0009(5) 0.0088(5) 0.0001(5) C12 0.0273(7) 0.0283(7) 0.0233(6) -0.0029(5) 0.0055(5) 0.0059(5) C13 0.0317(7) 0.0206(6) 0.0274(7) 0.0037(5) -0.0007(6) -0.0007(5) C14 0.0251(7) 0.0292(7) 0.0307(7) 0.0104(6) 0.0042(6) -0.0099(5) C15 0.0167(6) 0.0290(7) 0.0253(6) 0.0056(5) 0.0060(5) -0.0041(5) N3 0.0214(5) 0.0154(5) 0.0182(5) 0.0012(4) 0.0089(4) 0.0005(4) N2 0.0273(5) 0.0155(5) 0.0192(5) -0.0007(4) 0.0114(4) -0.0008(4) N1 0.0249(5) 0.0144(4) 0.0164(5) -0.0002(4) 0.0111(4) 0.0005(4) I1 0.02049(4) 0.02040(4) 0.01757(4) 0.00086(3) 0.01013(3) 0.00144(3) _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_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N3 1.3434(16) . ? C1 C2 1.3795(17) . ? C2 N1 1.3721(16) . ? C2 C3 1.4671(17) . ? C16 N3 1.4600(16) . ? C3 C8 1.3933(17) . ? C3 C4 1.4016(18) . ? C4 C5 1.385(2) . ? C5 C6 1.385(2) . ? C6 C7 1.382(2) . ? C7 C8 1.3886(19) . ? C9 N1 1.4684(16) . ? C9 C10 1.5103(18) . ? C10 C11 1.3863(18) . ? C10 C15 1.3920(18) . ? C11 C12 1.390(2) . ? C12 C13 1.385(2) . ? C13 C14 1.383(2) . ? C14 C15 1.387(2) . ? N3 N2 1.3144(15) . ? N2 N1 1.3287(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 C1 C2 106.40(11) . . ? N1 C2 C1 103.74(11) . . ? N1 C2 C3 129.13(11) . . ? C1 C2 C3 127.10(11) . . ? C8 C3 C4 118.50(12) . . ? C8 C3 C2 124.50(11) . . ? C4 C3 C2 117.00(11) . . ? C5 C4 C3 120.92(13) . . ? C4 C5 C6 120.05(14) . . ? C7 C6 C5 119.42(13) . . ? C6 C7 C8 121.07(13) . . ? C7 C8 C3 120.02(12) . . ? N1 C9 C10 112.45(10) . . ? C11 C10 C15 119.46(12) . . ? C11 C10 C9 122.40(11) . . ? C15 C10 C9 118.06(12) . . ? C10 C11 C12 119.99(13) . . ? C13 C12 C11 120.51(14) . . ? C14 C13 C12 119.42(13) . . ? C13 C14 C15 120.45(14) . . ? C14 C15 C10 120.14(13) . . ? N2 N3 C1 112.96(11) . . ? N2 N3 C16 119.64(11) . . ? C1 N3 C16 127.38(11) . . ? N3 N2 N1 104.17(10) . . ? N2 N1 C2 112.72(10) . . ? N2 N1 C9 115.59(10) . . ? C2 N1 C9 131.69(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.525 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.059 _database_code_depnum_ccdc_archive 'CCDC 846888' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sar250m #TrackingRef 'SH36.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H56 Cl4 N12 O Pd2' _chemical_formula_weight 1315.77 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 0.0000 0.0000 '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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4987(18) _cell_length_b 14.889(2) _cell_length_c 14.0557(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.797(3) _cell_angle_gamma 90.00 _cell_volume 2798.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5871 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.650 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'Blessing, 1955' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart AXS' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36889 _diffrn_reflns_av_R_equivalents 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0099 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6416 _reflns_number_gt 5871 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+2.8680P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6416 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.688612(10) 0.128082(9) 0.978796(9) 0.01977(5) Uani 1 1 d . . . Cl2 Cl 0.65684(4) 0.12638(3) 1.13996(3) 0.02966(11) Uani 1 1 d . . . Cl1 Cl 0.78890(4) -0.00350(3) 1.00066(4) 0.03225(11) Uani 1 1 d . . . N1 N 0.72151(12) 0.16881(10) 0.69098(11) 0.0225(3) Uani 1 1 d . . . N1A N 0.51667(11) 0.35430(10) 0.89787(11) 0.0213(3) Uani 1 1 d . . . N2 N 0.81658(12) 0.16925(12) 0.72893(11) 0.0261(3) Uani 1 1 d . . . N3A N 0.49727(12) 0.22828(10) 0.95655(11) 0.0229(3) Uani 1 1 d . . . C17 C 0.59728(13) 0.23129(12) 0.95096(12) 0.0208(3) Uani 1 1 d . . . C1 C 0.71910(14) 0.14240(12) 0.84507(13) 0.0211(3) Uani 1 1 d . . . N2A N 0.44667(12) 0.30115(11) 0.92499(11) 0.0244(3) Uani 1 1 d . . . C9 C 0.69962(13) 0.17522(13) 0.58739(13) 0.0228(4) Uani 1 1 d . . . C19 C 0.70088(13) 0.35455(12) 0.88223(13) 0.0204(3) Uani 1 1 d . . . N3 N 0.81295(12) 0.15320(11) 0.82127(11) 0.0249(3) Uani 1 1 d . . . C21 C 0.88040(15) 0.37072(13) 0.91563(16) 0.0311(4) Uani 1 1 d . . . H21 H 0.9395 0.3645 0.9576 0.037 Uiso 1 1 calc R . . C5 C 0.38825(15) 0.09506(14) 0.75661(15) 0.0302(4) Uani 1 1 d . . . H5 H 0.3500 0.0501 0.7798 0.036 Uiso 1 1 calc R . . C8 C 0.50165(14) 0.22782(12) 0.68404(12) 0.0224(3) Uani 1 1 d . . . H8 H 0.5394 0.2717 0.6586 0.027 Uiso 1 1 calc R . . C2 C 0.65876(14) 0.15349(12) 0.75777(12) 0.0208(3) Uani 1 1 d . . . C4 C 0.49175(14) 0.08981(13) 0.77209(13) 0.0249(4) Uani 1 1 d . . . H4 H 0.5229 0.0420 0.8067 0.030 Uiso 1 1 calc R . . C24 C 0.70291(14) 0.39268(12) 0.79172(13) 0.0214(3) Uani 1 1 d . . . H24 H 0.6436 0.4015 0.7507 0.026 Uiso 1 1 calc R . . C3 C 0.54920(13) 0.15606(12) 0.73585(12) 0.0212(3) Uani 1 1 d . . . C30 C 0.54026(14) 0.51609(13) 0.89979(13) 0.0252(4) Uani 1 1 d . . . H30 H 0.5961 0.5093 0.9458 0.030 Uiso 1 1 calc R . . C23 C 0.79370(15) 0.41753(13) 0.76301(14) 0.0262(4) Uani 1 1 d . . . H23 H 0.7951 0.4423 0.7025 0.031 Uiso 1 1 calc R . . C26 C 0.40356(14) 0.44966(14) 0.79276(14) 0.0279(4) Uani 1 1 d . . . H26 H 0.3683 0.3990 0.7689 0.033 Uiso 1 1 calc R . . C20 C 0.79004(15) 0.34520(13) 0.94435(14) 0.0261(4) Uani 1 1 d . . . H20 H 0.7890 0.3217 1.0055 0.031 Uiso 1 1 calc R . . C25 C 0.48660(14) 0.44210(12) 0.86212(13) 0.0232(4) Uani 1 1 d . . . C13 C 0.67026(17) 0.10075(15) 0.43652(15) 0.0339(4) Uani 1 1 d . . . H13 H 0.6626 0.0482 0.4006 0.041 Uiso 1 1 calc R . . C28 C 0.42602(17) 0.60979(15) 0.79766(16) 0.0336(5) Uani 1 1 d . . . H28 H 0.4051 0.6667 0.7762 0.040 Uiso 1 1 calc R . . C11 C 0.67412(15) 0.26197(14) 0.44336(14) 0.0281(4) Uani 1 1 d . . . H11 H 0.6682 0.3172 0.4123 0.034 Uiso 1 1 calc R . . C7 C 0.39806(14) 0.23345(13) 0.67066(13) 0.0257(4) Uani 1 1 d . . . H7 H 0.3665 0.2818 0.6374 0.031 Uiso 1 1 calc R . . C12 C 0.66366(15) 0.18349(15) 0.39044(14) 0.0299(4) Uani 1 1 d . . . H12 H 0.6522 0.1861 0.3237 0.036 Uiso 1 1 calc R . . C10 C 0.69351(15) 0.25832(13) 0.54323(13) 0.0263(4) Uani 1 1 d . . . H10 H 0.7022 0.3107 0.5794 0.032 Uiso 1 1 calc R . . C18 C 0.60949(13) 0.31574(12) 0.91174(12) 0.0203(3) Uani 1 1 d . . . C29 C 0.50855(16) 0.60075(14) 0.86717(14) 0.0291(4) Uani 1 1 d . . . H29 H 0.5429 0.6515 0.8921 0.035 Uiso 1 1 calc R . . C22 C 0.88243(15) 0.40543(14) 0.82456(16) 0.0317(4) Uani 1 1 d . . . H22 H 0.9431 0.4207 0.8045 0.038 Uiso 1 1 calc R . . C16 C 0.90986(15) 0.14945(16) 0.88319(15) 0.0315(4) Uani 1 1 d . . . H16B H 0.9389 0.0910 0.8786 0.047 Uiso 1 1 calc R . . H16C H 0.9001 0.1607 0.9485 0.047 Uiso 1 1 calc R . . H16A H 0.9538 0.1942 0.8629 0.047 Uiso 1 1 calc R . . C14 C 0.68819(16) 0.09629(14) 0.53555(15) 0.0300(4) Uani 1 1 d . . . H14 H 0.6925 0.0411 0.5667 0.036 Uiso 1 1 calc R . . C31 C 0.43993(15) 0.15552(14) 0.99427(15) 0.0291(4) Uani 1 1 d . . . H31C H 0.4437 0.1615 1.0627 0.044 Uiso 1 1 calc R . . H31A H 0.4674 0.0986 0.9792 0.044 Uiso 1 1 calc R . . H31B H 0.3713 0.1590 0.9655 0.044 Uiso 1 1 calc R . . C27 C 0.37461(16) 0.53484(15) 0.76002(15) 0.0329(4) Uani 1 1 d . . . H27 H 0.3202 0.5415 0.7124 0.040 Uiso 1 1 calc R . . C6 C 0.34180(15) 0.16713(15) 0.70670(15) 0.0301(4) Uani 1 1 d . . . H6 H 0.2724 0.1710 0.6974 0.036 Uiso 1 1 calc R . . O100 O 0.9792(3) -0.0723(2) 0.9041(2) 0.0370(7) Uani 0.50 1 d P . . H100 H 0.917(4) -0.056(3) 0.949(3) 0.124(16) Uiso 1 1 d . . . H101 H 1.041(4) -0.078(4) 0.938(4) 0.139(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02413(8) 0.01842(8) 0.01647(7) 0.00170(4) 0.00165(5) 0.00035(5) Cl2 0.0385(3) 0.0333(2) 0.0175(2) 0.00253(16) 0.00473(18) -0.00104(19) Cl1 0.0425(3) 0.0238(2) 0.0295(2) 0.00442(18) 0.0014(2) 0.00856(19) N1 0.0239(7) 0.0223(7) 0.0215(7) 0.0000(6) 0.0040(6) 0.0023(6) N1A 0.0220(7) 0.0228(7) 0.0192(7) -0.0012(6) 0.0030(6) 0.0004(6) N2 0.0233(8) 0.0318(9) 0.0237(8) 0.0016(6) 0.0053(6) 0.0042(6) N3A 0.0245(7) 0.0233(7) 0.0215(7) 0.0000(6) 0.0050(6) -0.0010(6) C17 0.0224(8) 0.0233(8) 0.0168(7) -0.0015(6) 0.0030(6) -0.0015(7) C1 0.0222(8) 0.0176(8) 0.0233(8) 0.0012(6) 0.0020(7) 0.0022(6) N2A 0.0252(8) 0.0244(8) 0.0241(8) -0.0007(6) 0.0046(6) -0.0003(6) C9 0.0239(9) 0.0260(9) 0.0189(8) -0.0012(7) 0.0049(7) 0.0016(7) C19 0.0224(8) 0.0177(8) 0.0207(8) -0.0007(6) 0.0017(6) 0.0000(6) N3 0.0231(8) 0.0294(8) 0.0220(7) 0.0017(6) 0.0027(6) 0.0047(6) C21 0.0235(9) 0.0264(10) 0.0411(11) 0.0074(8) -0.0043(8) -0.0015(7) C5 0.0300(10) 0.0302(10) 0.0310(10) -0.0032(8) 0.0060(8) -0.0083(8) C8 0.0250(9) 0.0230(9) 0.0187(8) -0.0023(7) 0.0012(6) -0.0025(7) C2 0.0258(9) 0.0183(8) 0.0190(8) -0.0007(6) 0.0051(7) 0.0014(7) C4 0.0311(10) 0.0206(8) 0.0231(9) -0.0016(7) 0.0037(7) -0.0009(7) C24 0.0245(8) 0.0196(8) 0.0197(8) -0.0011(6) 0.0011(7) 0.0006(7) C3 0.0228(8) 0.0223(8) 0.0184(8) -0.0042(7) 0.0025(6) -0.0003(7) C30 0.0276(9) 0.0272(9) 0.0219(8) -0.0016(7) 0.0070(7) 0.0003(7) C23 0.0323(10) 0.0202(9) 0.0271(9) 0.0020(7) 0.0074(8) -0.0017(7) C26 0.0264(9) 0.0314(10) 0.0258(9) -0.0033(8) 0.0039(7) 0.0042(8) C20 0.0279(9) 0.0227(9) 0.0259(9) 0.0055(7) -0.0029(7) -0.0014(7) C25 0.0268(9) 0.0233(9) 0.0205(8) 0.0005(7) 0.0071(7) 0.0054(7) C13 0.0406(11) 0.0312(10) 0.0294(10) -0.0113(8) 0.0029(9) 0.0019(9) C28 0.0377(11) 0.0312(10) 0.0349(11) 0.0083(9) 0.0154(9) 0.0114(9) C11 0.0333(10) 0.0283(10) 0.0238(9) 0.0024(7) 0.0072(7) -0.0020(8) C7 0.0263(9) 0.0273(9) 0.0219(8) -0.0026(7) -0.0025(7) 0.0009(7) C12 0.0321(10) 0.0382(11) 0.0197(8) -0.0026(8) 0.0042(7) 0.0002(8) C10 0.0326(10) 0.0231(9) 0.0237(9) -0.0022(7) 0.0059(7) -0.0020(7) C18 0.0229(8) 0.0212(8) 0.0167(8) -0.0014(6) 0.0019(6) 0.0009(7) C29 0.0367(11) 0.0250(9) 0.0288(10) -0.0009(8) 0.0160(8) 0.0002(8) C22 0.0260(9) 0.0256(9) 0.0443(12) 0.0058(8) 0.0075(8) -0.0037(8) C16 0.0224(9) 0.0424(11) 0.0287(10) 0.0031(9) 0.0004(8) 0.0041(8) C14 0.0380(11) 0.0220(9) 0.0298(10) -0.0004(8) 0.0039(8) 0.0023(8) C31 0.0263(9) 0.0308(10) 0.0318(10) 0.0034(8) 0.0093(8) -0.0045(8) C27 0.0302(10) 0.0385(11) 0.0304(10) 0.0032(8) 0.0051(8) 0.0124(9) C6 0.0221(9) 0.0374(11) 0.0299(10) -0.0049(8) 0.0001(7) -0.0030(8) O100 0.0335(16) 0.0362(16) 0.0404(17) -0.0047(13) 0.0014(13) 0.0022(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C17 1.9757(18) . ? Pd1 C1 1.9894(19) . ? Pd1 Cl2 2.3620(6) . ? Pd1 Cl1 2.3775(5) . ? N1 N2 1.321(2) . ? N1 C2 1.366(2) . ? N1 C9 1.449(2) . ? N1A N2A 1.327(2) . ? N1A C18 1.368(2) . ? N1A C25 1.439(2) . ? N2 N3 1.327(2) . ? N3A N2A 1.326(2) . ? N3A C17 1.364(2) . ? N3A C31 1.471(2) . ? C17 C18 1.392(2) . ? C1 N3 1.363(2) . ? C1 C2 1.388(2) . ? C9 C14 1.380(3) . ? C9 C10 1.382(3) . ? C19 C20 1.395(2) . ? C19 C24 1.397(2) . ? C19 C18 1.472(2) . ? N3 C16 1.471(2) . ? C21 C22 1.384(3) . ? C21 C20 1.389(3) . ? C5 C6 1.385(3) . ? C5 C4 1.387(3) . ? C8 C7 1.388(3) . ? C8 C3 1.399(3) . ? C2 C3 1.470(2) . ? C4 C3 1.393(3) . ? C24 C23 1.391(3) . ? C30 C25 1.384(3) . ? C30 C29 1.389(3) . ? C23 C22 1.391(3) . ? C26 C25 1.387(3) . ? C26 C27 1.387(3) . ? C13 C14 1.382(3) . ? C13 C12 1.389(3) . ? C28 C27 1.381(3) . ? C28 C29 1.385(3) . ? C11 C12 1.382(3) . ? C11 C10 1.394(3) . ? C7 C6 1.383(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 C1 86.16(7) . . ? C17 Pd1 Cl2 90.50(5) . . ? C1 Pd1 Cl2 174.26(5) . . ? C17 Pd1 Cl1 174.62(5) . . ? C1 Pd1 Cl1 91.33(5) . . ? Cl2 Pd1 Cl1 92.376(18) . . ? N2 N1 C2 112.46(15) . . ? N2 N1 C9 117.38(15) . . ? C2 N1 C9 129.83(16) . . ? N2A N1A C18 112.51(15) . . ? N2A N1A C25 117.63(15) . . ? C18 N1A C25 129.84(16) . . ? N1 N2 N3 103.37(15) . . ? N2A N3A C17 115.01(15) . . ? N2A N3A C31 116.79(15) . . ? C17 N3A C31 128.19(16) . . ? N3A C17 C18 102.94(15) . . ? N3A C17 Pd1 123.99(13) . . ? C18 C17 Pd1 132.60(14) . . ? N3 C1 C2 102.86(16) . . ? N3 C1 Pd1 124.25(13) . . ? C2 C1 Pd1 132.56(14) . . ? N3A N2A N1A 103.27(14) . . ? C14 C9 C10 121.98(17) . . ? C14 C9 N1 117.86(17) . . ? C10 C9 N1 120.13(16) . . ? C20 C19 C24 119.27(17) . . ? C20 C19 C18 118.00(16) . . ? C24 C19 C18 122.47(16) . . ? N2 N3 C1 114.84(15) . . ? N2 N3 C16 115.95(16) . . ? C1 N3 C16 129.21(16) . . ? C22 C21 C20 119.96(19) . . ? C6 C5 C4 120.03(19) . . ? C7 C8 C3 119.95(17) . . ? N1 C2 C1 106.46(16) . . ? N1 C2 C3 123.48(16) . . ? C1 C2 C3 129.92(16) . . ? C5 C4 C3 120.11(18) . . ? C23 C24 C19 119.94(17) . . ? C4 C3 C8 119.49(17) . . ? C4 C3 C2 119.94(17) . . ? C8 C3 C2 120.43(16) . . ? C25 C30 C29 118.32(18) . . ? C22 C23 C24 120.22(18) . . ? C25 C26 C27 118.16(19) . . ? C21 C20 C19 120.54(18) . . ? C30 C25 C26 122.38(18) . . ? C30 C25 N1A 118.78(16) . . ? C26 C25 N1A 118.82(17) . . ? C14 C13 C12 120.25(19) . . ? C27 C28 C29 120.39(19) . . ? C12 C11 C10 120.04(18) . . ? C6 C7 C8 120.03(18) . . ? C11 C12 C13 120.23(18) . . ? C9 C10 C11 118.62(17) . . ? N1A C18 C17 106.28(16) . . ? N1A C18 C19 125.55(16) . . ? C17 C18 C19 127.97(16) . . ? C28 C29 C30 120.2(2) . . ? C21 C22 C23 120.00(19) . . ? C9 C14 C13 118.86(19) . . ? C28 C27 C26 120.49(19) . . ? C7 C6 C5 120.35(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.042 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.066 _database_code_depnum_ccdc_archive 'CCDC 929861' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\rechne\sar32 #TrackingRef 'SH18a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 Cl2 N6 Pd' _chemical_formula_weight 675.92 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 0.0000 0.0000 '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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 16.427(3) _cell_length_b 8.2599(12) _cell_length_c 12.1501(17) _cell_angle_alpha 90.00 _cell_angle_beta 116.214(7) _cell_angle_gamma 90.00 _cell_volume 1479.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1868 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5635 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II duo' _diffrn_measurement_method 'Omega psi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4408 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.18 _reflns_number_total 2328 _reflns_number_gt 1868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Kappa Apex II suite, 2008' _computing_cell_refinement 'Bruker Kappa Apex II suite, 2008' _computing_data_reduction 'Bruker Kappa Apex II suite, 2008' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+18.2510P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(9) _refine_ls_number_reflns 2328 _refine_ls_number_parameters 187 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0927(8) 0.4979(15) 0.5740(11) 0.023(3) Uani 1 1 d U . . C2 C 0.0976(7) 0.6177(13) 0.6570(9) 0.022(2) Uani 1 1 d . . . C3 C 0.0317(7) 0.6693(14) 0.7052(9) 0.024(2) Uani 1 1 d . . . C4 C 0.0159(8) 0.5695(15) 0.7848(11) 0.035(3) Uani 1 1 d . . . H4 H 0.0471 0.4693 0.8106 0.042 Uiso 1 1 calc R . . C5 C -0.0473(9) 0.6194(16) 0.8270(11) 0.041(3) Uani 1 1 d . . . H5 H -0.0596 0.5507 0.8805 0.049 Uiso 1 1 calc R . . C6 C -0.0907(8) 0.7622(16) 0.7933(11) 0.043(4) Uani 1 1 d . . . H6 H -0.1312 0.7960 0.8254 0.051 Uiso 1 1 calc R . . C7 C -0.0757(7) 0.8597(17) 0.7111(11) 0.039(4) Uani 1 1 d . . . H7 H -0.1079 0.9587 0.6840 0.047 Uiso 1 1 calc R . . C8 C -0.0137(6) 0.812(2) 0.6686(9) 0.030(3) Uani 1 1 d . . . H8 H -0.0027 0.8802 0.6134 0.036 Uiso 1 1 calc R . . C9 C 0.2183(6) 0.827(2) 0.7741(8) 0.026(2) Uani 1 1 d . . . H9A H 0.1702 0.8977 0.7759 0.031 Uiso 1 1 calc R . . H9B H 0.2565 0.8944 0.7476 0.031 Uiso 1 1 calc R . . C10 C 0.2758(7) 0.7654(12) 0.9010(9) 0.025(3) Uani 1 1 d . . . C11 C 0.3568(7) 0.6814(15) 0.9283(11) 0.034(3) Uani 1 1 d . . . H11 H 0.3744 0.6606 0.8650 0.040 Uiso 1 1 calc R . . C12 C 0.4108(7) 0.6289(14) 1.0458(11) 0.033(3) Uani 1 1 d . . . H12 H 0.4650 0.5709 1.0625 0.039 Uiso 1 1 calc R . . C13 C 0.3873(9) 0.6597(15) 1.1395(12) 0.036(3) Uani 1 1 d . . . H13 H 0.4257 0.6257 1.2207 0.043 Uiso 1 1 calc R . . C14 C 0.3064(9) 0.7413(15) 1.1141(11) 0.038(3) Uani 1 1 d . . . H14 H 0.2891 0.7611 1.1778 0.045 Uiso 1 1 calc R . . C15 C 0.2521(8) 0.7926(15) 0.9969(10) 0.036(3) Uani 1 1 d . . . H15 H 0.1972 0.8478 0.9805 0.043 Uiso 1 1 calc R . . C16 C 0.1966(8) 0.4367(16) 0.4776(11) 0.037(3) Uani 1 1 d . . . H16A H 0.2448 0.4981 0.4698 0.056 Uiso 1 1 calc R . . H16B H 0.1446 0.4263 0.3967 0.056 Uiso 1 1 calc R . . H16C H 0.2191 0.3288 0.5104 0.056 Uiso 1 1 calc R . . N1 N 0.1765(6) 0.6997(10) 0.6849(8) 0.023(2) Uani 1 1 d . . . N2 N 0.2196(6) 0.6421(10) 0.6248(8) 0.026(2) Uani 1 1 d . . . N3 N 0.1688(6) 0.5207(10) 0.5597(8) 0.024(2) Uani 1 1 d . . . Cl1 Cl 0.1147(2) 0.1235(3) 0.5722(3) 0.0278(8) Uani 1 1 d . . . Pd1 Pd 0.0000 0.32505(13) 0.5000 0.0289(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(6) 0.029(6) 0.013(6) 0.009(4) -0.002(5) 0.013(5) C2 0.025(6) 0.027(6) 0.015(6) -0.006(5) 0.008(5) 0.000(5) C3 0.027(6) 0.035(7) 0.011(6) -0.008(5) 0.009(5) -0.005(5) C4 0.037(7) 0.037(8) 0.040(8) 0.001(6) 0.026(7) 0.005(6) C5 0.046(8) 0.055(8) 0.037(8) -0.008(7) 0.031(7) -0.006(7) C6 0.025(7) 0.066(11) 0.041(8) -0.018(6) 0.018(6) -0.004(6) C7 0.023(6) 0.045(11) 0.049(7) -0.009(6) 0.016(6) 0.001(6) C8 0.030(5) 0.029(6) 0.037(6) -0.016(8) 0.021(5) -0.011(8) C9 0.030(5) 0.024(5) 0.024(5) 0.013(8) 0.012(4) 0.013(8) C10 0.028(6) 0.026(6) 0.018(6) -0.001(4) 0.009(5) -0.002(4) C11 0.022(6) 0.050(8) 0.033(8) 0.014(6) 0.016(6) 0.017(6) C12 0.021(6) 0.045(7) 0.032(7) 0.005(6) 0.012(6) 0.005(6) C13 0.038(7) 0.037(7) 0.029(7) 0.002(6) 0.012(6) -0.005(6) C14 0.046(9) 0.043(7) 0.032(8) -0.003(6) 0.024(7) 0.001(6) C15 0.033(6) 0.042(10) 0.033(6) 0.000(6) 0.017(5) 0.012(6) C16 0.032(7) 0.061(9) 0.027(7) -0.016(6) 0.019(6) -0.006(7) N1 0.027(5) 0.013(4) 0.033(6) 0.003(4) 0.018(5) 0.004(4) N2 0.038(6) 0.021(5) 0.030(5) 0.005(4) 0.023(5) 0.005(4) N3 0.027(5) 0.024(5) 0.022(5) -0.003(4) 0.012(4) 0.004(4) Cl1 0.0294(18) 0.0274(17) 0.0276(18) 0.0041(13) 0.0134(15) 0.0036(14) Pd1 0.0279(7) 0.0366(7) 0.0244(7) 0.000 0.0135(6) 0.000 _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_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N3 1.349(13) . ? C1 C2 1.390(16) . ? C1 Pd1 1.989(13) . ? C2 N1 1.365(13) . ? C2 C3 1.503(13) . ? C3 C8 1.362(19) . ? C3 C4 1.380(15) . ? C4 C5 1.408(15) . ? C5 C6 1.345(17) . ? C6 C7 1.387(17) . ? C7 C8 1.387(14) . ? C9 N1 1.449(18) . ? C9 C10 1.498(14) . ? C10 C15 1.400(14) . ? C10 C11 1.403(14) . ? C11 C12 1.376(15) . ? C12 C13 1.378(16) . ? C13 C14 1.397(17) . ? C14 C15 1.371(17) . ? C16 N3 1.444(13) . ? N1 N2 1.310(11) . ? N2 N3 1.321(12) . ? Cl1 Pd1 2.373(3) . ? Pd1 C1 1.989(13) 2_556 ? Pd1 Cl1 2.373(3) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 C1 C2 103.5(11) . . ? N3 C1 Pd1 127.6(9) . . ? C2 C1 Pd1 128.8(8) . . ? N1 C2 C1 106.1(9) . . ? N1 C2 C3 122.1(9) . . ? C1 C2 C3 131.6(10) . . ? C8 C3 C4 120.2(9) . . ? C8 C3 C2 120.2(10) . . ? C4 C3 C2 119.6(10) . . ? C3 C4 C5 118.5(11) . . ? C6 C5 C4 121.5(11) . . ? C5 C6 C7 119.3(11) . . ? C6 C7 C8 119.9(13) . . ? C3 C8 C7 120.5(12) . . ? N1 C9 C10 113.4(13) . . ? C15 C10 C11 117.7(10) . . ? C15 C10 C9 121.5(10) . . ? C11 C10 C9 120.8(9) . . ? C12 C11 C10 120.7(10) . . ? C11 C12 C13 120.7(11) . . ? C12 C13 C14 119.5(12) . . ? C15 C14 C13 119.8(11) . . ? C14 C15 C10 121.5(11) . . ? N2 N1 C2 111.6(8) . . ? N2 N1 C9 119.1(8) . . ? C2 N1 C9 129.1(8) . . ? N1 N2 N3 104.8(8) . . ? N2 N3 C1 113.8(9) . . ? N2 N3 C16 118.1(9) . . ? C1 N3 C16 127.9(10) . . ? C1 Pd1 C1 88.3(7) . 2_556 ? C1 Pd1 Cl1 174.3(4) . 2_556 ? C1 Pd1 Cl1 90.7(3) 2_556 2_556 ? C1 Pd1 Cl1 90.7(3) . . ? C1 Pd1 Cl1 174.3(4) 2_556 . ? Cl1 Pd1 Cl1 90.86(16) 2_556 . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.521 _refine_diff_density_min -2.666 _refine_diff_density_rms 0.169 _database_code_depnum_ccdc_archive 'CCDC 846894' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pd #TrackingRef 'SH24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Cl2 N6 Pd' _chemical_formula_weight 732.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.7893(14) _cell_length_b 15.1436(9) _cell_length_c 19.3799(11) _cell_angle_alpha 90.00 _cell_angle_beta 113.010(2) _cell_angle_gamma 90.00 _cell_volume 6696.4(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 6.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3698 _exptl_absorpt_correction_T_max 0.5756 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38116 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 66.54 _reflns_number_total 10976 _reflns_number_gt 9820 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+52.7814P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10976 _refine_ls_number_parameters 822 _refine_ls_number_restraints 815 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2356 _refine_ls_wR_factor_gt 0.2283 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.010 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.37113(3) 0.75509(7) 0.22088(4) 0.0226(2) Uani 1 1 d U . . Cl1 Cl 0.46224(10) 0.75088(13) 0.32066(14) 0.0187(5) Uani 1 1 d U . . Cl2 Cl 0.27792(11) 0.75591(19) 0.12119(15) 0.0315(7) Uani 1 1 d U . . Pd2 Pd 0.13016(8) 0.2393(3) 0.34755(9) 0.0176(4) Uani 0.883(17) 1 d PU A 1 Cl3 Cl 0.03994(11) 0.25029(14) 0.35768(15) 0.0215(5) Uani 1 1 d U A 1 Cl4 Cl 0.22098(12) 0.23917(17) 0.33929(15) 0.0295(6) Uani 1 1 d U A 1 Pd2' Pd 0.1274(5) 0.275(3) 0.3458(6) 0.022(4) Uani 0.117(17) 1 d PU A 2 N1 N 0.2981(4) 0.7688(7) 0.3845(6) 0.042(2) Uani 1 1 d U . . N2 N 0.3028(4) 0.8615(7) 0.3751(6) 0.050(2) Uani 1 1 d U . . N3 N 0.3229(4) 0.8667(6) 0.3221(5) 0.0351(18) Uani 1 1 d U . . N4 N 0.4430(4) 0.7237(7) 0.0585(5) 0.0389(19) Uani 1 1 d U . . N5 N 0.4331(4) 0.6393(6) 0.0719(6) 0.042(2) Uani 1 1 d U . . N6 N 0.4134(4) 0.6431(6) 0.1247(5) 0.0408(19) Uani 1 1 d U . . N7 N 0.0581(4) 0.2743(7) 0.1123(6) 0.0382(19) Uani 1 1 d U . . N8 N 0.0687(4) 0.3633(6) 0.1391(6) 0.046(2) Uani 1 1 d U . . N9 N 0.0875(4) 0.3556(6) 0.2089(5) 0.0381(18) Uani 1 1 d U A . N10 N 0.2006(4) 0.2171(7) 0.5819(5) 0.0380(18) Uani 1 1 d U . . N11 N 0.1939(4) 0.1282(6) 0.5663(5) 0.043(2) Uani 1 1 d U . . N12 N 0.1764(4) 0.1280(6) 0.4966(5) 0.0333(17) Uani 1 1 d U A . C1 C 0.3338(4) 0.7847(8) 0.2946(6) 0.035(2) Uani 1 1 d U . . C2 C 0.3183(5) 0.7315(8) 0.3386(7) 0.038(2) Uani 1 1 d U . . C3 C 0.3214(4) 0.6293(7) 0.3344(7) 0.036(2) Uani 1 1 d U . . C4 C 0.3447(5) 0.5815(8) 0.4033(7) 0.043(2) Uani 1 1 d U . . H4A H 0.3576 0.6120 0.4498 0.052 Uiso 1 1 calc R . . C5 C 0.3486(6) 0.4870(8) 0.4018(8) 0.053(3) Uani 1 1 d U . . H5A H 0.3647 0.4535 0.4467 0.064 Uiso 1 1 calc R . . C6 C 0.3281(6) 0.4473(9) 0.3325(8) 0.059(3) Uani 1 1 d U . . H6A H 0.3303 0.3848 0.3300 0.071 Uiso 1 1 calc R . . C7 C 0.3043(7) 0.4947(9) 0.2659(9) 0.061(3) Uani 1 1 d U . . H7A H 0.2898 0.4660 0.2185 0.073 Uiso 1 1 calc R . . C8 C 0.3028(6) 0.5854(8) 0.2720(7) 0.048(2) Uani 1 1 d U . . H8A H 0.2868 0.6184 0.2268 0.058 Uiso 1 1 calc R . . C9 C 0.2683(5) 0.7482(7) 0.4314(7) 0.031(2) Uani 1 1 d U . . H9A H 0.2806 0.7901 0.4740 0.037 Uiso 1 1 calc R . . H9B H 0.2796 0.6881 0.4520 0.037 Uiso 1 1 calc R . . C10 C 0.2043(5) 0.7524(5) 0.3915(7) 0.0227(19) Uani 1 1 d U . . C11 C 0.1693(5) 0.7780(8) 0.4283(7) 0.038(2) Uani 1 1 d U . . H11A H 0.1875 0.7944 0.4795 0.046 Uiso 1 1 calc R . . C12 C 0.1083(5) 0.7809(8) 0.3938(7) 0.040(2) Uani 1 1 d U . . H12A H 0.0858 0.7977 0.4218 0.048 Uiso 1 1 calc R . . C13 C 0.0806(5) 0.7594(7) 0.3186(8) 0.037(2) Uani 1 1 d U . . H13A H 0.0390 0.7583 0.2952 0.044 Uiso 1 1 calc R . . C14 C 0.1140(6) 0.7395(8) 0.2784(10) 0.041(3) Uani 1 1 d U . . H14A H 0.0957 0.7280 0.2261 0.050 Uiso 1 1 calc R . . C15 C 0.1725(5) 0.7363(8) 0.3132(8) 0.035(2) Uani 1 1 d U . . H15A H 0.1944 0.7225 0.2838 0.042 Uiso 1 1 calc R . . C16 C 0.3312(5) 0.9585(9) 0.2962(7) 0.047(3) Uani 1 1 d U . . H16A H 0.3265 1.0011 0.3329 0.057 Uiso 1 1 calc R . . C17 C 0.2875(7) 0.9785(10) 0.2264(10) 0.074(4) Uani 1 1 d U . . H17A H 0.2489 0.9711 0.2286 0.111 Uiso 1 1 calc R . . H17B H 0.2909 0.9388 0.1884 0.111 Uiso 1 1 calc R . . H17C H 0.2920 1.0398 0.2133 0.111 Uiso 1 1 calc R . . C18 C 0.3945(6) 0.9685(8) 0.3018(8) 0.057(3) Uani 1 1 d U . . H18A H 0.4000 1.0278 0.2854 0.085 Uiso 1 1 calc R . . H18B H 0.4021 0.9244 0.2696 0.085 Uiso 1 1 calc R . . H18C H 0.4218 0.9595 0.3538 0.085 Uiso 1 1 calc R . . C19 C 0.4073(5) 0.7324(8) 0.1466(6) 0.034(2) Uani 1 1 d U . . C20 C 0.4285(5) 0.7798(8) 0.1041(6) 0.035(2) Uani 1 1 d U . . C21 C 0.4347(6) 0.8751(8) 0.1021(8) 0.049(3) Uani 1 1 d U . . C22 C 0.4879(5) 0.9142(8) 0.1121(7) 0.045(2) Uani 1 1 d U . . H22A H 0.5201 0.8780 0.1151 0.055 Uiso 1 1 calc R . . C23 C 0.4951(6) 1.0076(9) 0.1180(8) 0.056(3) Uani 1 1 d U . . H23A H 0.5311 1.0339 0.1224 0.067 Uiso 1 1 calc R . . C24 C 0.4490(7) 1.0595(9) 0.1173(8) 0.061(3) Uani 1 1 d U . . H24A H 0.4531 1.1219 0.1208 0.073 Uiso 1 1 calc R . . C25 C 0.3963(7) 1.0201(9) 0.1115(9) 0.061(3) Uani 1 1 d U . . H25A H 0.3647 1.0561 0.1108 0.073 Uiso 1 1 calc R . . C26 C 0.3897(6) 0.9291(8) 0.1065(9) 0.058(3) Uani 1 1 d U . . H26A H 0.3547 0.9030 0.1062 0.069 Uiso 1 1 calc R . . C27 C 0.4602(5) 0.7446(7) -0.0068(7) 0.032(2) Uani 1 1 d U . . H27A H 0.4327 0.7154 -0.0528 0.038 Uiso 1 1 calc R . . H27B H 0.4581 0.8091 -0.0156 0.038 Uiso 1 1 calc R . . C28 C 0.5219(4) 0.7120(8) 0.0110(6) 0.0318(19) Uani 1 1 d U . . C29 C 0.5356(5) 0.6209(8) 0.0143(6) 0.041(2) Uani 1 1 d U . . H29A H 0.5055 0.5785 0.0060 0.049 Uiso 1 1 calc R . . C30 C 0.5922(5) 0.5928(8) 0.0295(7) 0.046(2) Uani 1 1 d U . . H30A H 0.6010 0.5315 0.0324 0.055 Uiso 1 1 calc R . . C31 C 0.6366(5) 0.6559(8) 0.0407(6) 0.043(2) Uani 1 1 d U . . H31A H 0.6754 0.6359 0.0519 0.051 Uiso 1 1 calc R . . C32 C 0.6256(6) 0.7475(7) 0.0359(7) 0.031(2) Uani 1 1 d U . . H32A H 0.6550 0.7905 0.0420 0.037 Uiso 1 1 calc R . . C33 C 0.5681(4) 0.7687(8) 0.0215(6) 0.033(2) Uani 1 1 d U . . H33A H 0.5591 0.8300 0.0184 0.039 Uiso 1 1 calc R . . C34 C 0.3987(5) 0.5618(8) 0.1525(7) 0.045(2) Uani 1 1 d U . . H34A H 0.3931 0.5767 0.1996 0.054 Uiso 1 1 calc R . . C35 C 0.3427(6) 0.5249(9) 0.0995(8) 0.055(3) Uani 1 1 d U . . H35A H 0.3117 0.5693 0.0888 0.082 Uiso 1 1 calc R . . H35B H 0.3325 0.4726 0.1218 0.082 Uiso 1 1 calc R . . H35C H 0.3466 0.5083 0.0528 0.082 Uiso 1 1 calc R . . C36 C 0.4491(6) 0.4967(8) 0.1737(8) 0.052(3) Uani 1 1 d U . . H36A H 0.4848 0.5244 0.2095 0.078 Uiso 1 1 calc R . . H36B H 0.4553 0.4793 0.1286 0.078 Uiso 1 1 calc R . . H36C H 0.4397 0.4443 0.1966 0.078 Uiso 1 1 calc R . . C37 C 0.0933(6) 0.2683(8) 0.2375(7) 0.037(2) Uani 1 1 d U . . C38 C 0.0723(5) 0.2232(8) 0.1726(7) 0.0368(19) Uani 1 1 d U A . C39 C 0.0653(5) 0.1261(8) 0.1650(8) 0.045(2) Uani 1 1 d U . . C40 C 0.0098(6) 0.0867(8) 0.1199(7) 0.049(2) Uani 1 1 d U A . H40A H -0.0220 0.1232 0.0902 0.059 Uiso 1 1 calc R . . C41 C 0.0025(7) -0.0040(8) 0.1196(8) 0.055(3) Uani 1 1 d U . . H41A H -0.0337 -0.0298 0.0881 0.066 Uiso 1 1 calc R A . C42 C 0.0485(6) -0.0578(8) 0.1659(8) 0.057(3) Uani 1 1 d U A . H42A H 0.0428 -0.1197 0.1677 0.069 Uiso 1 1 calc R . . C43 C 0.1017(7) -0.0205(8) 0.2086(8) 0.057(3) Uani 1 1 d U . . H43A H 0.1335 -0.0575 0.2376 0.069 Uiso 1 1 calc R A . C44 C 0.1101(6) 0.0717(7) 0.2102(7) 0.046(2) Uani 1 1 d U A . H44A H 0.1464 0.0965 0.2423 0.056 Uiso 1 1 calc R . . C45 C 0.0392(6) 0.2587(8) 0.0324(8) 0.038(3) Uani 1 1 d U . . H45A H 0.0421 0.1947 0.0240 0.045 Uiso 1 1 calc R . . H45B H 0.0663 0.2897 0.0142 0.045 Uiso 1 1 calc R . . C46 C -0.0239(5) 0.2893(8) -0.0145(6) 0.039(2) Uani 1 1 d U . . C47 C -0.0632(6) 0.2300(8) -0.0454(8) 0.043(2) Uani 1 1 d U . . H47A H -0.0525 0.1694 -0.0383 0.052 Uiso 1 1 calc R . . C48 C -0.1213(6) 0.2525(8) -0.0889(8) 0.035(2) Uani 1 1 d U . . H48A H -0.1495 0.2078 -0.1119 0.042 Uiso 1 1 calc R . . C49 C -0.1381(5) 0.3447(9) -0.0989(7) 0.048(3) Uani 1 1 d U . . H49A H -0.1773 0.3623 -0.1273 0.058 Uiso 1 1 calc R . . C50 C -0.0938(5) 0.4065(8) -0.0647(7) 0.046(2) Uani 1 1 d U . . H50A H -0.1030 0.4677 -0.0700 0.056 Uiso 1 1 calc R . . C51 C -0.0376(5) 0.3804(8) -0.0237(7) 0.044(2) Uani 1 1 d U . . H51A H -0.0078 0.4233 -0.0015 0.053 Uiso 1 1 calc R . . C52 C 0.1036(6) 0.4399(8) 0.2568(8) 0.054(3) Uani 1 1 d U . . H52A H 0.1087 0.4238 0.3091 0.065 Uiso 1 1 calc R A . C53 C 0.1613(6) 0.4731(8) 0.2588(8) 0.058(3) Uani 1 1 d U A . H53A H 0.1720 0.5273 0.2887 0.087 Uiso 1 1 calc R . . H53B H 0.1579 0.4855 0.2076 0.087 Uiso 1 1 calc R . . H53C H 0.1915 0.4282 0.2814 0.087 Uiso 1 1 calc R . . C54 C 0.0536(6) 0.5031(8) 0.2267(7) 0.052(3) Uani 1 1 d U A . H54A H 0.0633 0.5575 0.2565 0.078 Uiso 1 1 calc R . . H54B H 0.0184 0.4764 0.2294 0.078 Uiso 1 1 calc R . . H54C H 0.0462 0.5170 0.1743 0.078 Uiso 1 1 calc R . . C55 C 0.1670(4) 0.2068(7) 0.4593(6) 0.0303(18) Uani 1 1 d U . . C56 C 0.1848(5) 0.2624(7) 0.5179(6) 0.0273(19) Uani 1 1 d U A . C57 C 0.1835(5) 0.3643(7) 0.5130(7) 0.036(2) Uani 1 1 d U . . C58 C 0.2112(6) 0.4059(8) 0.4748(8) 0.057(3) Uani 1 1 d U A . H58A H 0.2308 0.3721 0.4503 0.068 Uiso 1 1 calc R . . C59 C 0.2116(8) 0.4981(9) 0.4707(9) 0.070(3) Uani 1 1 d U . . H59A H 0.2305 0.5268 0.4426 0.084 Uiso 1 1 calc R A . C60 C 0.1840(8) 0.5475(10) 0.5083(9) 0.075(3) Uani 1 1 d U A . H60A H 0.1823 0.6100 0.5042 0.090 Uiso 1 1 calc R . . C61 C 0.1591(7) 0.5046(8) 0.5515(8) 0.059(3) Uani 1 1 d U . . H61A H 0.1413 0.5372 0.5789 0.071 Uiso 1 1 calc R A . C62 C 0.1604(6) 0.4094(9) 0.5542(8) 0.058(3) Uani 1 1 d U A . H62A H 0.1450 0.3789 0.5853 0.070 Uiso 1 1 calc R . . C63 C 0.2313(6) 0.2438(8) 0.6604(7) 0.038(2) Uani 1 1 d U . . H63A H 0.2220 0.2011 0.6929 0.046 Uiso 1 1 calc R . . H63B H 0.2166 0.3024 0.6677 0.046 Uiso 1 1 calc R . . C64 C 0.2983(5) 0.2486(7) 0.6849(7) 0.026(2) Uani 1 1 d U . . C65 C 0.3242(5) 0.2283(8) 0.6375(7) 0.037(2) Uani 1 1 d U . . H65A H 0.3016 0.2087 0.5879 0.044 Uiso 1 1 calc R . . C66 C 0.3861(6) 0.2368(8) 0.6632(9) 0.036(3) Uani 1 1 d U . . H66A H 0.4049 0.2276 0.6294 0.043 Uiso 1 1 calc R . . C67 C 0.4182(6) 0.2579(8) 0.7348(7) 0.038(3) Uani 1 1 d U . . H67A H 0.4597 0.2553 0.7535 0.045 Uiso 1 1 calc R . . C68 C 0.3901(5) 0.2841(9) 0.7827(7) 0.046(3) Uani 1 1 d U . . H68A H 0.4122 0.3074 0.8311 0.056 Uiso 1 1 calc R . . C69 C 0.3289(5) 0.2749(10) 0.7574(7) 0.044(3) Uani 1 1 d U . . H69A H 0.3093 0.2866 0.7898 0.053 Uiso 1 1 calc R . . C70 C 0.1641(5) 0.0362(8) 0.4588(7) 0.045(2) Uani 1 1 d U . . H70A H 0.1708 -0.0088 0.4991 0.054 Uiso 1 1 calc R A . C71 C 0.2067(6) 0.0176(8) 0.4229(8) 0.053(3) Uani 1 1 d U A . H71A H 0.2468 0.0243 0.4602 0.080 Uiso 1 1 calc R . . H71B H 0.2000 0.0593 0.3817 0.080 Uiso 1 1 calc R . . H71C H 0.2009 -0.0428 0.4033 0.080 Uiso 1 1 calc R . . C72 C 0.0996(6) 0.0276(9) 0.4025(8) 0.054(3) Uani 1 1 d U A . H72A H 0.0931 -0.0314 0.3800 0.082 Uiso 1 1 calc R . . H72B H 0.0914 0.0723 0.3631 0.082 Uiso 1 1 calc R . . H72C H 0.0734 0.0366 0.4289 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0124(4) 0.0421(5) 0.0158(5) -0.0003(3) 0.0083(4) -0.0004(2) Cl1 0.0059(10) 0.0415(13) 0.0073(11) -0.0018(7) 0.0010(10) 0.0020(7) Cl2 0.0072(11) 0.0714(19) 0.0119(13) -0.0022(9) -0.0006(10) -0.0009(9) Pd2 0.0171(5) 0.0228(12) 0.0138(5) 0.0030(5) 0.0068(4) 0.0019(5) Cl3 0.0116(11) 0.0438(14) 0.0118(12) 0.0042(8) 0.0075(11) 0.0031(7) Cl4 0.0197(12) 0.0526(14) 0.0194(14) 0.0058(9) 0.0112(12) -0.0007(9) Pd2' 0.022(3) 0.039(10) 0.004(3) 0.004(4) 0.006(2) 0.009(5) N1 0.027(4) 0.070(5) 0.033(5) -0.002(4) 0.016(4) 0.005(4) N2 0.046(5) 0.059(5) 0.051(5) -0.005(4) 0.027(4) -0.002(4) N3 0.027(4) 0.041(4) 0.041(4) -0.007(3) 0.017(3) 0.004(3) N4 0.040(5) 0.064(5) 0.024(4) -0.001(4) 0.025(4) 0.003(4) N5 0.039(4) 0.044(4) 0.052(5) -0.017(4) 0.026(4) -0.005(4) N6 0.040(4) 0.046(4) 0.041(4) -0.002(4) 0.021(4) -0.004(4) N7 0.024(4) 0.058(5) 0.035(4) 0.001(4) 0.014(4) -0.005(4) N8 0.045(5) 0.031(4) 0.051(5) 0.011(4) 0.008(4) -0.002(4) N9 0.052(5) 0.034(4) 0.038(4) 0.004(3) 0.028(4) 0.001(3) N10 0.034(4) 0.052(4) 0.029(4) -0.001(4) 0.014(3) -0.003(4) N11 0.048(5) 0.041(4) 0.042(4) 0.003(4) 0.020(4) 0.009(4) N12 0.035(4) 0.031(4) 0.042(4) 0.012(3) 0.024(3) 0.007(3) C1 0.025(4) 0.043(5) 0.038(5) 0.004(4) 0.013(4) 0.007(4) C2 0.023(5) 0.068(5) 0.029(5) -0.006(4) 0.017(4) 0.003(4) C3 0.022(4) 0.036(4) 0.044(5) 0.001(4) 0.008(4) -0.004(4) C4 0.039(5) 0.046(5) 0.046(5) -0.003(4) 0.019(4) 0.009(4) C5 0.049(6) 0.042(5) 0.071(6) 0.000(5) 0.025(5) 0.001(5) C6 0.070(7) 0.042(5) 0.075(7) -0.007(5) 0.040(6) -0.008(5) C7 0.076(7) 0.048(6) 0.070(6) -0.013(5) 0.039(6) -0.012(6) C8 0.058(6) 0.048(5) 0.054(6) 0.000(4) 0.037(5) -0.006(5) C9 0.026(5) 0.042(5) 0.028(6) 0.003(4) 0.014(4) 0.004(4) C10 0.026(4) 0.016(4) 0.030(5) 0.000(3) 0.015(4) -0.002(3) C11 0.036(5) 0.037(5) 0.044(5) 0.009(5) 0.019(4) 0.004(4) C12 0.038(5) 0.054(6) 0.041(5) 0.006(5) 0.029(5) 0.009(5) C13 0.022(5) 0.044(5) 0.050(6) 0.005(5) 0.020(5) -0.004(4) C14 0.030(5) 0.056(6) 0.043(6) -0.009(5) 0.020(5) -0.003(4) C15 0.023(5) 0.054(6) 0.034(5) -0.004(4) 0.017(4) -0.003(4) C16 0.053(6) 0.045(5) 0.053(6) -0.001(5) 0.031(5) 0.004(5) C17 0.064(8) 0.051(8) 0.104(11) 0.021(8) 0.028(7) 0.013(7) C18 0.067(7) 0.041(7) 0.073(8) -0.012(6) 0.039(7) -0.022(6) C19 0.018(4) 0.065(5) 0.025(5) -0.005(4) 0.014(4) -0.003(4) C20 0.034(5) 0.053(4) 0.029(4) -0.004(4) 0.022(4) -0.001(4) C21 0.048(5) 0.037(4) 0.060(6) 0.017(5) 0.018(5) 0.010(4) C22 0.053(5) 0.042(5) 0.055(6) 0.003(5) 0.035(5) -0.003(4) C23 0.070(6) 0.044(6) 0.066(7) 0.001(5) 0.041(6) -0.008(5) C24 0.078(7) 0.045(6) 0.066(7) -0.001(6) 0.036(6) -0.002(5) C25 0.075(7) 0.045(5) 0.077(7) 0.004(6) 0.046(6) 0.009(5) C26 0.053(6) 0.043(5) 0.086(7) 0.017(6) 0.037(6) 0.004(5) C27 0.020(5) 0.067(6) 0.013(5) 0.001(4) 0.013(4) 0.008(4) C28 0.025(4) 0.052(5) 0.022(4) -0.003(4) 0.013(3) -0.001(4) C29 0.040(5) 0.044(5) 0.042(5) -0.006(4) 0.018(4) 0.002(4) C30 0.046(5) 0.045(5) 0.049(6) -0.002(5) 0.021(5) 0.004(4) C31 0.033(5) 0.057(5) 0.041(5) -0.002(5) 0.017(4) 0.008(4) C32 0.021(5) 0.050(5) 0.024(6) 0.001(4) 0.012(5) 0.005(4) C33 0.014(4) 0.066(6) 0.022(5) -0.004(4) 0.012(4) -0.002(4) C34 0.045(5) 0.038(5) 0.058(6) -0.007(5) 0.028(5) -0.004(4) C35 0.057(6) 0.051(7) 0.070(8) -0.012(6) 0.039(6) -0.012(6) C36 0.058(7) 0.035(6) 0.069(8) -0.008(6) 0.032(6) -0.011(5) C37 0.039(5) 0.049(5) 0.033(4) 0.006(4) 0.023(4) -0.002(4) C38 0.028(4) 0.051(4) 0.038(4) 0.005(4) 0.020(4) 0.006(4) C39 0.038(5) 0.037(4) 0.066(6) -0.001(4) 0.027(5) 0.006(4) C40 0.062(6) 0.039(5) 0.054(6) -0.003(5) 0.031(5) -0.003(5) C41 0.075(6) 0.038(5) 0.057(6) -0.009(5) 0.031(5) -0.009(5) C42 0.081(7) 0.035(5) 0.065(7) -0.004(5) 0.038(6) -0.001(5) C43 0.083(7) 0.030(5) 0.059(7) 0.003(5) 0.029(6) 0.011(5) C44 0.057(6) 0.030(5) 0.060(6) -0.001(4) 0.031(5) 0.005(4) C45 0.030(5) 0.053(6) 0.038(5) -0.001(4) 0.023(5) 0.004(4) C46 0.047(5) 0.047(5) 0.033(5) 0.005(4) 0.028(4) 0.012(4) C47 0.056(6) 0.042(5) 0.037(6) 0.001(5) 0.024(5) 0.008(4) C48 0.037(5) 0.052(5) 0.019(6) 0.001(4) 0.014(5) -0.004(4) C49 0.046(5) 0.059(6) 0.044(6) 0.011(5) 0.021(5) 0.006(4) C50 0.050(5) 0.046(5) 0.049(6) 0.011(5) 0.027(5) 0.007(4) C51 0.047(5) 0.045(5) 0.043(6) 0.014(4) 0.022(4) 0.003(4) C52 0.065(6) 0.039(5) 0.058(6) -0.002(5) 0.024(6) -0.007(5) C53 0.069(7) 0.037(6) 0.066(8) 0.006(6) 0.023(7) -0.014(6) C54 0.072(7) 0.034(5) 0.053(7) -0.005(5) 0.027(6) 0.002(5) C55 0.025(4) 0.030(4) 0.035(4) 0.006(4) 0.012(4) 0.001(4) C56 0.020(4) 0.053(4) 0.013(4) -0.003(3) 0.011(4) 0.000(4) C57 0.035(5) 0.031(4) 0.048(5) -0.013(4) 0.023(4) -0.014(4) C58 0.077(7) 0.041(5) 0.060(7) -0.011(5) 0.035(6) -0.020(5) C59 0.102(8) 0.042(6) 0.077(8) -0.012(5) 0.047(6) -0.032(6) C60 0.103(9) 0.052(6) 0.078(8) -0.017(6) 0.045(7) -0.022(6) C61 0.087(8) 0.038(5) 0.061(7) -0.015(5) 0.037(6) -0.009(5) C62 0.074(7) 0.047(5) 0.057(7) -0.020(5) 0.029(6) -0.020(5) C63 0.037(5) 0.067(6) 0.020(5) 0.005(4) 0.021(5) -0.003(4) C64 0.025(4) 0.042(5) 0.018(5) 0.000(3) 0.016(4) -0.006(4) C65 0.027(5) 0.058(6) 0.026(5) -0.011(5) 0.013(4) -0.010(5) C66 0.025(5) 0.059(7) 0.029(5) -0.002(4) 0.016(5) -0.004(4) C67 0.025(5) 0.064(7) 0.021(5) 0.004(4) 0.005(4) -0.006(4) C68 0.035(5) 0.065(7) 0.033(5) -0.005(5) 0.007(4) -0.003(5) C69 0.036(5) 0.078(7) 0.022(5) -0.003(5) 0.017(4) -0.005(5) C70 0.054(6) 0.039(5) 0.048(6) 0.002(4) 0.025(5) -0.001(5) C71 0.062(7) 0.040(6) 0.064(8) -0.001(6) 0.030(7) 0.002(6) C72 0.059(6) 0.046(7) 0.059(8) -0.002(6) 0.024(6) -0.005(6) _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_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C19 2.001(10) . ? Pd1 C1 2.033(10) . ? Pd1 Cl1 2.330(3) . ? Pd1 Cl2 2.363(3) . ? Pd2 C37 2.014(12) . ? Pd2 C55 2.054(10) . ? Pd2 Cl4 2.319(3) . ? Pd2 Cl3 2.326(3) . ? Pd2' C37 1.935(16) . ? Pd2' C55 2.27(2) . ? N1 C2 1.309(15) . ? N1 C9 1.411(15) . ? N1 N2 1.426(15) . ? N2 N3 1.308(13) . ? N3 C1 1.418(14) . ? N3 C16 1.519(16) . ? N4 N5 1.345(14) . ? N4 C20 1.371(14) . ? N4 C27 1.517(13) . ? N5 N6 1.296(13) . ? N6 C19 1.444(15) . ? N6 C34 1.446(15) . ? N7 C38 1.330(15) . ? N7 N8 1.431(14) . ? N7 C45 1.451(17) . ? N8 N9 1.253(14) . ? N9 C37 1.419(14) . ? N9 C52 1.536(15) . ? N10 C56 1.337(15) . ? N10 N11 1.375(14) . ? N10 C63 1.466(16) . ? N11 N12 1.247(13) . ? N12 C55 1.367(13) . ? N12 C70 1.546(15) . ? C1 C2 1.334(17) . ? C2 C3 1.552(17) . ? C3 C8 1.297(17) . ? C3 C4 1.427(16) . ? C4 C5 1.435(16) . ? C4 H4A 0.9500 . ? C5 C6 1.375(19) . ? C5 H5A 0.9500 . ? C6 C7 1.39(2) . ? C6 H6A 0.9500 . ? C7 C8 1.381(18) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C10 1.470(16) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.376(16) . ? C10 C15 1.432(18) . ? C11 C12 1.395(17) . ? C11 H11A 0.9500 . ? C12 C13 1.385(19) . ? C12 H12A 0.9500 . ? C13 C14 1.375(19) . ? C13 H13A 0.9500 . ? C14 C15 1.339(19) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.40(2) . ? C16 C18 1.539(17) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.345(15) . ? C20 C21 1.453(17) . ? C21 C22 1.389(17) . ? C21 C26 1.414(18) . ? C22 C23 1.425(17) . ? C22 H22A 0.9500 . ? C23 C24 1.382(19) . ? C23 H23A 0.9500 . ? C24 C25 1.40(2) . ? C24 H24A 0.9500 . ? C25 C26 1.386(18) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.514(14) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C33 1.381(16) . ? C28 C29 1.417(16) . ? C29 C30 1.383(16) . ? C29 H29A 0.9500 . ? C30 C31 1.409(17) . ? C30 H30A 0.9500 . ? C31 C32 1.410(15) . ? C31 H31A 0.9500 . ? C32 C33 1.380(16) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.477(17) . ? C34 C36 1.517(17) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.344(17) . ? C38 C39 1.481(17) . ? C39 C44 1.384(18) . ? C39 C40 1.441(18) . ? C40 C41 1.385(17) . ? C40 H40A 0.9500 . ? C41 C42 1.40(2) . ? C41 H41A 0.9500 . ? C42 C43 1.38(2) . ? C42 H42A 0.9500 . ? C43 C44 1.410(16) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.541(17) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.288(19) . ? C46 C51 1.416(16) . ? C47 C48 1.40(2) . ? C47 H47A 0.9500 . ? C48 C49 1.448(17) . ? C48 H48A 0.9500 . ? C49 C50 1.396(18) . ? C49 H49A 0.9500 . ? C50 C51 1.364(16) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C54 1.493(18) . ? C52 C53 1.502(18) . ? C52 H52A 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.343(15) . ? C56 C57 1.545(15) . ? C57 C62 1.338(17) . ? C57 C58 1.346(16) . ? C58 C59 1.398(18) . ? C58 H58A 0.9500 . ? C59 C60 1.40(2) . ? C59 H59A 0.9500 . ? C60 C61 1.38(2) . ? C60 H60A 0.9500 . ? C61 C62 1.442(18) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? C63 C64 1.541(17) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.346(16) . ? C64 C69 1.370(17) . ? C65 C66 1.422(17) . ? C65 H65A 0.9500 . ? C66 C67 1.34(2) . ? C66 H66A 0.9500 . ? C67 C68 1.417(18) . ? C67 H67A 0.9500 . ? C68 C69 1.406(17) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 C71 1.500(17) . ? C70 C72 1.550(17) . ? C70 H70A 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Pd1 C1 177.1(5) . . ? C19 Pd1 Cl1 91.7(3) . . ? C1 Pd1 Cl1 89.0(3) . . ? C19 Pd1 Cl2 89.0(3) . . ? C1 Pd1 Cl2 90.3(3) . . ? Cl1 Pd1 Cl2 178.39(9) . . ? C37 Pd2 C55 178.7(5) . . ? C37 Pd2 Cl4 88.7(3) . . ? C55 Pd2 Cl4 91.7(3) . . ? C37 Pd2 Cl3 91.2(4) . . ? C55 Pd2 Cl3 88.5(3) . . ? Cl4 Pd2 Cl3 175.8(2) . . ? C37 Pd2' C55 150(2) . . ? C2 N1 C9 141.1(11) . . ? C2 N1 N2 105.4(10) . . ? C9 N1 N2 113.0(9) . . ? N3 N2 N1 103.6(9) . . ? N2 N3 C1 115.4(10) . . ? N2 N3 C16 117.2(9) . . ? C1 N3 C16 127.4(9) . . ? N5 N4 C20 110.6(9) . . ? N5 N4 C27 119.4(9) . . ? C20 N4 C27 129.6(10) . . ? N6 N5 N4 105.3(8) . . ? N5 N6 C19 112.8(9) . . ? N5 N6 C34 119.0(10) . . ? C19 N6 C34 128.1(9) . . ? C38 N7 N8 106.4(10) . . ? C38 N7 C45 135.0(11) . . ? N8 N7 C45 118.6(10) . . ? N9 N8 N7 104.0(8) . . ? N8 N9 C37 116.5(9) . . ? N8 N9 C52 118.3(9) . . ? C37 N9 C52 125.2(10) . . ? C56 N10 N11 109.4(9) . . ? C56 N10 C63 131.8(10) . . ? N11 N10 C63 117.8(9) . . ? N12 N11 N10 101.6(9) . . ? N11 N12 C55 119.1(10) . . ? N11 N12 C70 115.9(9) . . ? C55 N12 C70 125.0(9) . . ? C2 C1 N3 98.3(9) . . ? C2 C1 Pd1 129.8(9) . . ? N3 C1 Pd1 131.5(8) . . ? N1 C2 C1 117.1(12) . . ? N1 C2 C3 120.4(11) . . ? C1 C2 C3 122.5(10) . . ? C8 C3 C4 118.6(11) . . ? C8 C3 C2 123.6(11) . . ? C4 C3 C2 117.9(10) . . ? C3 C4 C5 119.6(11) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C4 117.0(13) . . ? C6 C5 H5A 121.5 . . ? C4 C5 H5A 121.5 . . ? C5 C6 C7 122.8(13) . . ? C5 C6 H6A 118.6 . . ? C7 C6 H6A 118.6 . . ? C8 C7 C6 116.7(14) . . ? C8 C7 H7A 121.6 . . ? C6 C7 H7A 121.6 . . ? C3 C8 C7 125.3(14) . . ? C3 C8 H8A 117.3 . . ? C7 C8 H8A 117.3 . . ? N1 C9 C10 112.3(11) . . ? N1 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C15 113.6(10) . . ? C11 C10 C9 120.6(12) . . ? C15 C10 C9 125.7(11) . . ? C10 C11 C12 123.2(12) . . ? C10 C11 H11A 118.4 . . ? C12 C11 H11A 118.4 . . ? C13 C12 C11 119.6(10) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C14 C13 C12 119.2(12) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C15 C14 C13 119.8(15) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C10 124.5(12) . . ? C14 C15 H15A 117.8 . . ? C10 C15 H15A 117.8 . . ? C17 C16 N3 111.4(12) . . ? C17 C16 C18 115.5(12) . . ? N3 C16 C18 109.4(9) . . ? C17 C16 H16A 106.7 . . ? N3 C16 H16A 106.7 . . ? C18 C16 H16A 106.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N6 102.1(9) . . ? C20 C19 Pd1 137.9(9) . . ? N6 C19 Pd1 120.0(8) . . ? C19 C20 N4 109.1(11) . . ? C19 C20 C21 128.1(11) . . ? N4 C20 C21 122.8(11) . . ? C22 C21 C26 118.3(12) . . ? C22 C21 C20 121.6(11) . . ? C26 C21 C20 118.7(11) . . ? C21 C22 C23 121.0(12) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C24 C23 C22 119.2(12) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 120.0(12) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 120.7(13) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C21 120.3(12) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C28 C27 N4 109.3(9) . . ? C28 C27 H27A 109.8 . . ? N4 C27 H27A 109.8 . . ? C28 C27 H27B 109.8 . . ? N4 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? C33 C28 C29 115.4(10) . . ? C33 C28 C27 122.5(11) . . ? C29 C28 C27 122.0(10) . . ? C30 C29 C28 121.0(11) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C31 119.3(11) . . ? C29 C30 H30A 120.3 . . ? C31 C30 H30A 120.3 . . ? C30 C31 C32 122.6(10) . . ? C30 C31 H31A 118.7 . . ? C32 C31 H31A 118.7 . . ? C33 C32 C31 113.6(11) . . ? C33 C32 H32A 123.2 . . ? C31 C32 H32A 123.2 . . ? C32 C33 C28 128.1(12) . . ? C32 C33 H33A 116.0 . . ? C28 C33 H33A 116.0 . . ? N6 C34 C35 111.7(11) . . ? N6 C34 C36 110.7(9) . . ? C35 C34 C36 113.2(11) . . ? N6 C34 H34A 107.0 . . ? C35 C34 H34A 107.0 . . ? C36 C34 H34A 107.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N9 99.5(10) . . ? C38 C37 Pd2' 152.3(15) . . ? N9 C37 Pd2' 108.2(15) . . ? C38 C37 Pd2 136.9(9) . . ? N9 C37 Pd2 123.5(9) . . ? Pd2' C37 Pd2 15.5(11) . . ? N7 C38 C37 113.5(11) . . ? N7 C38 C39 120.7(11) . . ? C37 C38 C39 125.7(11) . . ? C44 C39 C40 118.5(11) . . ? C44 C39 C38 119.7(12) . . ? C40 C39 C38 121.2(11) . . ? C41 C40 C39 120.3(13) . . ? C41 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C40 C41 C42 120.1(14) . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 119.9 . . ? C43 C42 C41 119.7(12) . . ? C43 C42 H42A 120.2 . . ? C41 C42 H42A 120.2 . . ? C42 C43 C44 121.1(13) . . ? C42 C43 H43A 119.4 . . ? C44 C43 H43A 119.4 . . ? C39 C44 C43 120.1(13) . . ? C39 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? N7 C45 C46 114.3(10) . . ? N7 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? N7 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C47 C46 C51 121.3(12) . . ? C47 C46 C45 118.2(11) . . ? C51 C46 C45 120.4(11) . . ? C46 C47 C48 121.6(12) . . ? C46 C47 H47A 119.2 . . ? C48 C47 H47A 119.2 . . ? C47 C48 C49 119.4(12) . . ? C47 C48 H48A 120.3 . . ? C49 C48 H48A 120.3 . . ? C50 C49 C48 116.8(11) . . ? C50 C49 H49A 121.6 . . ? C48 C49 H49A 121.6 . . ? C51 C50 C49 121.1(12) . . ? C51 C50 H50A 119.5 . . ? C49 C50 H50A 119.5 . . ? C50 C51 C46 119.7(12) . . ? C50 C51 H51A 120.1 . . ? C46 C51 H51A 120.1 . . ? C54 C52 C53 115.6(11) . . ? C54 C52 N9 108.5(11) . . ? C53 C52 N9 108.3(11) . . ? C54 C52 H52A 108.1 . . ? C53 C52 H52A 108.1 . . ? N9 C52 H52A 108.1 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N12 99.7(9) . . ? C56 C55 Pd2 127.2(8) . . ? N12 C55 Pd2 132.9(8) . . ? C56 C55 Pd2' 114.2(12) . . ? N12 C55 Pd2' 145.7(12) . . ? Pd2 C55 Pd2' 13.1(8) . . ? N10 C56 C55 110.1(10) . . ? N10 C56 C57 124.2(10) . . ? C55 C56 C57 125.6(10) . . ? C62 C57 C58 121.1(11) . . ? C62 C57 C56 118.5(10) . . ? C58 C57 C56 119.9(10) . . ? C57 C58 C59 121.0(13) . . ? C57 C58 H58A 119.5 . . ? C59 C58 H58A 119.5 . . ? C60 C59 C58 119.2(14) . . ? C60 C59 H59A 120.4 . . ? C58 C59 H59A 120.4 . . ? C61 C60 C59 119.4(14) . . ? C61 C60 H60A 120.3 . . ? C59 C60 H60A 120.3 . . ? C60 C61 C62 118.9(13) . . ? C60 C61 H61A 120.6 . . ? C62 C61 H61A 120.6 . . ? C57 C62 C61 119.9(12) . . ? C57 C62 H62A 120.1 . . ? C61 C62 H62A 120.1 . . ? N10 C63 C64 113.0(10) . . ? N10 C63 H63A 109.0 . . ? C64 C63 H63A 109.0 . . ? N10 C63 H63B 109.0 . . ? C64 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? C65 C64 C69 123.1(11) . . ? C65 C64 C63 121.6(11) . . ? C69 C64 C63 115.3(10) . . ? C64 C65 C66 118.5(12) . . ? C64 C65 H65A 120.7 . . ? C66 C65 H65A 120.7 . . ? C67 C66 C65 120.4(12) . . ? C67 C66 H66A 119.8 . . ? C65 C66 H66A 119.8 . . ? C66 C67 C68 120.0(11) . . ? C66 C67 H67A 120.0 . . ? C68 C67 H67A 120.0 . . ? C69 C68 C67 118.8(11) . . ? C69 C68 H68A 120.6 . . ? C67 C68 H68A 120.6 . . ? C64 C69 C68 118.4(11) . . ? C64 C69 H69A 120.8 . . ? C68 C69 H69A 120.8 . . ? C71 C70 N12 110.2(9) . . ? C71 C70 C72 112.2(11) . . ? N12 C70 C72 111.5(10) . . ? C71 C70 H70A 107.6 . . ? N12 C70 H70A 107.6 . . ? C72 C70 H70A 107.6 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 66.54 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 3.104 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.201 _database_code_depnum_ccdc_archive 'CCDC 892296'