# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1924 data_Complex1 #(97ab5) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H36 Cl2 N2 O2 P2 Pd' _chemical_formula_weight 695.85 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 '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' 'P' 'P' 0.1023 0.0942 '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 P21/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 10.456(2) _cell_length_b 7.5530(10) _cell_length_c 19.935(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.641(13) _cell_angle_gamma 90.00 _cell_volume 1547.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method ? _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 396(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6352 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.95 _reflns_number_total 2395 _reflns_number_observed 1992 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2395 _refine_ls_number_parameters 183 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_obs 0.0383 _refine_ls_wR_factor_all 0.1098 _refine_ls_wR_factor_obs 0.1084 _refine_ls_goodness_of_fit_all 1.146 _refine_ls_goodness_of_fit_obs 1.250 _refine_ls_restrained_S_all 1.146 _refine_ls_restrained_S_obs 1.250 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.5000 0.0108(2) Uani 1 d S . P1 P -0.17096(9) 0.16750(13) 0.44220(5) 0.0134(3) Uani 1 d . . Cl1 Cl 0.10103(10) -0.00004(11) 0.40704(5) 0.0193(3) Uani 1 d . . N1 N -0.2263(3) 0.3065(4) 0.4935(2) 0.0185(8) Uani 1 d D . H1 H -0.2281(43) 0.2645(53) 0.5365(15) 0.030(13) Uiso 1 d D . O1 O -0.3172(3) 0.5094(3) 0.5910(2) 0.0269(8) Uani 1 d . . C1 C -0.2977(4) 0.0155(4) 0.4031(2) 0.0168(9) Uani 1 d . . C2 C -0.2689(4) -0.1132(5) 0.3576(2) 0.0228(10) Uani 1 d . . H2 H -0.1860(4) -0.1190(5) 0.3471(2) 0.027 Uiso 1 calc R . C3 C -0.3642(4) -0.2324(5) 0.3284(2) 0.0291(11) Uani 1 d . . H3 H -0.3456(4) -0.3167(5) 0.2976(2) 0.035 Uiso 1 calc R . C4 C -0.4859(4) -0.2258(6) 0.3448(3) 0.0338(12) Uani 1 d . . H4 H -0.5493(4) -0.3058(6) 0.3249(3) 0.041 Uiso 1 calc R . C5 C -0.5150(4) -0.1015(6) 0.3905(3) 0.0338(12) Uani 1 d . . H5 H -0.5974(4) -0.0981(6) 0.4018(3) 0.041 Uiso 1 calc R . C6 C -0.4203(4) 0.0179(5) 0.4194(2) 0.0251(11) Uani 1 d . . H6 H -0.4397(4) 0.1013(5) 0.4503(2) 0.030 Uiso 1 calc R . C7 C -0.1403(4) 0.3081(4) 0.3731(2) 0.0134(9) Uani 1 d . . C8 C -0.0511(4) 0.4460(5) 0.3896(2) 0.0208(10) Uani 1 d . . H8 H -0.0116(4) 0.4641(5) 0.4349(2) 0.025 Uiso 1 calc R . C9 C -0.0213(4) 0.5557(6) 0.3393(2) 0.0237(10) Uani 1 d . . H9 H 0.0366(4) 0.6490(6) 0.3509(2) 0.028 Uiso 1 calc R . C10 C -0.0772(4) 0.5274(5) 0.2719(2) 0.0237(10) Uani 1 d . . H10 H -0.0550(4) 0.5992(5) 0.2379(2) 0.028 Uiso 1 calc R . C11 C -0.1657(4) 0.3928(5) 0.2552(2) 0.0241(10) Uani 1 d . . H11 H -0.2044(4) 0.3747(5) 0.2099(2) 0.029 Uiso 1 calc R . C12 C -0.1978(4) 0.2837(5) 0.3055(2) 0.0202(10) Uani 1 d . . H12 H -0.2584(4) 0.1936(5) 0.2938(2) 0.024 Uiso 1 calc R . C13 C -0.3212(4) 0.4489(5) 0.4746(2) 0.0243(10) Uani 1 d . . H13A H -0.4087(4) 0.4016(5) 0.4695(2) 0.029 Uiso 1 calc R . H13B H -0.3107(4) 0.5000(5) 0.4313(2) 0.029 Uiso 1 calc R . C14 C -0.3011(4) 0.5902(5) 0.5294(2) 0.0235(10) Uani 1 d . . H14A H -0.2145(4) 0.6403(5) 0.5340(2) 0.028 Uiso 1 calc R . H14B H -0.3642(4) 0.6846(5) 0.5175(2) 0.028 Uiso 1 calc R . C15 C -0.2983(5) 0.6297(6) 0.6467(3) 0.0368(12) Uani 1 d . . H15A H -0.3027(30) 0.5668(9) 0.6881(3) 0.055 Uiso 1 calc R . H15B H -0.3650(18) 0.7187(24) 0.6391(8) 0.055 Uiso 1 calc R . H15C H -0.2146(13) 0.6849(31) 0.6505(10) 0.055 Uiso 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 0.0120(3) 0.0115(3) 0.0088(3) 0.0010(2) 0.0019(2) 0.0003(2) P1 0.0134(5) 0.0147(5) 0.0118(6) 0.0011(4) 0.0018(4) 0.0009(4) Cl1 0.0244(6) 0.0198(6) 0.0157(6) 0.0041(4) 0.0088(5) 0.0046(4) N1 0.022(2) 0.018(2) 0.015(2) 0.0017(15) 0.004(2) 0.0085(14) O1 0.041(2) 0.017(2) 0.024(2) -0.0033(13) 0.012(2) -0.0051(12) C1 0.017(2) 0.016(2) 0.016(2) 0.007(2) -0.002(2) 0.000(2) C2 0.019(2) 0.019(2) 0.030(3) 0.002(2) 0.004(2) 0.000(2) C3 0.039(3) 0.019(2) 0.027(3) -0.001(2) 0.000(2) -0.004(2) C4 0.031(3) 0.027(3) 0.038(3) 0.007(2) -0.008(2) -0.014(2) C5 0.019(2) 0.039(3) 0.043(3) 0.006(2) 0.004(2) -0.009(2) C6 0.022(2) 0.026(3) 0.027(3) 0.004(2) 0.001(2) 0.000(2) C7 0.014(2) 0.013(2) 0.014(2) 0.001(2) 0.003(2) 0.004(2) C8 0.022(2) 0.023(2) 0.016(2) 0.000(2) -0.001(2) -0.003(2) C9 0.027(2) 0.018(2) 0.026(3) 0.002(2) 0.005(2) -0.007(2) C10 0.028(3) 0.022(2) 0.023(3) 0.008(2) 0.008(2) 0.002(2) C11 0.027(2) 0.033(3) 0.011(2) 0.002(2) 0.001(2) -0.001(2) C12 0.021(2) 0.017(2) 0.021(3) 0.000(2) 0.002(2) -0.004(2) C13 0.024(2) 0.024(2) 0.024(3) 0.002(2) 0.001(2) 0.011(2) C14 0.024(2) 0.017(2) 0.031(3) 0.003(2) 0.011(2) 0.005(2) C15 0.051(3) 0.028(3) 0.033(3) -0.009(2) 0.014(3) -0.005(2) _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 Cl1 2.2963(10) 3_556 ? Pd1 Cl1 2.2963(10) . ? Pd1 P1 2.3158(10) . ? Pd1 P1 2.3158(10) 3_556 ? P1 N1 1.643(3) . ? P1 C7 1.815(4) . ? P1 C1 1.817(4) . ? N1 C13 1.464(5) . ? O1 C14 1.410(5) . ? O1 C15 1.420(5) . ? C1 C6 1.379(6) . ? C1 C2 1.400(6) . ? C2 C3 1.389(6) . ? C3 C4 1.371(6) . ? C4 C5 1.381(7) . ? C5 C6 1.383(6) . ? C7 C12 1.381(6) . ? C7 C8 1.397(5) . ? C8 C9 1.380(6) . ? C9 C10 1.379(6) . ? C10 C11 1.375(6) . ? C11 C12 1.386(6) . ? C13 C14 1.513(6) . ? 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 Cl1 Pd1 Cl1 180.0 3_556 . ? Cl1 Pd1 P1 88.49(4) 3_556 . ? Cl1 Pd1 P1 91.51(4) . . ? Cl1 Pd1 P1 91.51(4) 3_556 3_556 ? Cl1 Pd1 P1 88.49(4) . 3_556 ? P1 Pd1 P1 180.0 . 3_556 ? N1 P1 C7 103.3(2) . . ? N1 P1 C1 110.9(2) . . ? C7 P1 C1 105.1(2) . . ? N1 P1 Pd1 111.59(13) . . ? C7 P1 Pd1 117.98(12) . . ? C1 P1 Pd1 107.65(12) . . ? C13 N1 P1 127.6(3) . . ? C14 O1 C15 112.5(3) . . ? C6 C1 C2 118.8(4) . . ? C6 C1 P1 121.8(3) . . ? C2 C1 P1 119.3(3) . . ? C3 C2 C1 119.9(4) . . ? C4 C3 C2 120.1(4) . . ? C3 C4 C5 120.6(4) . . ? C4 C5 C6 119.3(4) . . ? C1 C6 C5 121.2(4) . . ? C12 C7 C8 118.8(4) . . ? C12 C7 P1 123.8(3) . . ? C8 C7 P1 117.4(3) . . ? C9 C8 C7 120.4(4) . . ? C10 C9 C8 120.2(4) . . ? C11 C10 C9 119.7(4) . . ? C10 C11 C12 120.4(4) . . ? C7 C12 C11 120.4(4) . . ? N1 C13 C14 109.6(3) . . ? O1 C14 C13 107.5(3) . . ? _refine_diff_density_max 0.830 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.157 #===end data_Complex2 #(98ab2) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H40 Cl2 N2 O4 P2 Pd' _chemical_formula_weight 755.90 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 (no.2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.396(2) _cell_length_b 10.146(2) _cell_length_c 10.849(3) _cell_angle_alpha 94.97(2) _cell_angle_beta 111.01(2) _cell_angle_gamma 94.71(2) _cell_volume 853.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method ? _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3413 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2981 _reflns_number_observed 2589 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+0.1009P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2973 _refine_ls_number_parameters 202 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_obs 0.0518 _refine_ls_wR_factor_all 0.1459 _refine_ls_wR_factor_obs 0.1298 _refine_ls_goodness_of_fit_all 1.223 _refine_ls_goodness_of_fit_obs 1.292 _refine_ls_restrained_S_all 1.351 _refine_ls_restrained_S_obs 1.292 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.0000 0.0327(2) Uani 1 d S . P1 P -0.22461(13) -0.16937(10) -0.10983(10) 0.0329(3) Uani 1 d . . N1 N -0.4053(5) -0.1083(4) -0.1848(4) 0.0438(9) Uani 1 d D . H1 H -0.4072(52) -0.0221(27) -0.1687(39) 0.028(10) Uiso 1 d D . Cl1 Cl 0.18808(15) -0.15456(12) 0.01112(14) 0.0585(4) Uani 1 d . . O1 O -0.6280(5) 0.0224(3) -0.3912(3) 0.0565(9) Uani 1 d . . O2 O -0.7614(4) -0.1879(3) -0.5019(3) 0.0491(8) Uani 1 d . . C1 C -0.2633(5) -0.2794(4) 0.0038(4) 0.0370(9) Uani 1 d . . C2 C -0.1499(6) -0.3706(5) 0.0567(5) 0.0519(12) Uani 1 d . . H2 H -0.0537(6) -0.3771(5) 0.0341(5) 0.062 Uiso 1 calc R . C3 C -0.1821(7) -0.4514(6) 0.1436(6) 0.067(2) Uani 1 d . . H3 H -0.1075(7) -0.5132(6) 0.1787(6) 0.081 Uiso 1 calc R . C4 C -0.3233(8) -0.4414(6) 0.1786(5) 0.067(2) Uani 1 d . . H4 H -0.3439(8) -0.4965(6) 0.2368(5) 0.081 Uiso 1 calc R . C5 C -0.4328(7) -0.3505(6) 0.1279(5) 0.0608(14) Uani 1 d . . H5 H -0.5272(7) -0.3430(6) 0.1527(5) 0.073 Uiso 1 calc R . C6 C -0.4040(6) -0.2690(5) 0.0394(5) 0.0471(11) Uani 1 d . . H6 H -0.4795(6) -0.2078(5) 0.0045(5) 0.057 Uiso 1 calc R . C7 C -0.1994(5) -0.2858(4) -0.2379(4) 0.0368(9) Uani 1 d . . C8 C -0.1061(6) -0.2412(5) -0.3129(5) 0.0496(11) Uani 1 d . . H8 H -0.0496(6) -0.1549(5) -0.2932(5) 0.059 Uiso 1 calc R . C9 C -0.0980(8) -0.3255(6) -0.4161(5) 0.0646(15) Uani 1 d . . H9 H -0.0347(8) -0.2957(6) -0.4653(5) 0.078 Uiso 1 calc R . C10 C -0.1809(7) -0.4518(6) -0.4475(5) 0.0622(14) Uani 1 d . . H10 H -0.1749(7) -0.5075(6) -0.5181(5) 0.075 Uiso 1 calc R . C11 C -0.2733(7) -0.4966(5) -0.3744(5) 0.0600(13) Uani 1 d . . H11 H -0.3301(7) -0.5829(5) -0.3953(5) 0.072 Uiso 1 calc R . C12 C -0.2821(6) -0.4139(5) -0.2703(5) 0.0482(11) Uani 1 d . . H12 H -0.3448(6) -0.4450(5) -0.2211(5) 0.058 Uiso 1 calc R . C13 C -0.5636(5) -0.1778(5) -0.2848(4) 0.0447(10) Uani 1 d . . H13A H -0.6560(5) -0.1752(5) -0.2512(4) 0.054 Uiso 1 calc R . H13B H -0.5491(5) -0.2705(5) -0.3028(4) 0.054 Uiso 1 calc R . C14 C -0.6101(6) -0.1149(5) -0.4111(4) 0.0442(10) Uani 1 d . . H14 H -0.5187(6) -0.1233(5) -0.4465(4) 0.053 Uiso 1 calc R . C15 C -0.8036(8) -0.1548(6) -0.6360(5) 0.073(2) Uani 1 d . . H15A H -0.9075(34) -0.2084(34) -0.6938(10) 0.110 Uiso 1 calc R . H15B H -0.7116(28) -0.1717(44) -0.6658(18) 0.110 Uiso 1 calc R . H15C H -0.8197(59) -0.0623(13) -0.6374(10) 0.110 Uiso 1 calc R . C16 C -0.7630(8) 0.0493(6) -0.3488(7) 0.079(2) Uani 1 d . . H16A H -0.7617(39) 0.1440(6) -0.3324(47) 0.118 Uiso 1 calc R . H16B H -0.7488(36) 0.0107(42) -0.2683(27) 0.118 Uiso 1 calc R . H16C H -0.8706(9) 0.0118(43) -0.4165(21) 0.118 Uiso 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 0.0257(3) 0.0332(3) 0.0381(3) 0.0031(2) 0.0106(2) 0.0033(2) P1 0.0282(6) 0.0331(6) 0.0362(6) 0.0037(4) 0.0111(4) 0.0022(4) N1 0.032(2) 0.036(2) 0.053(2) 0.004(2) 0.005(2) 0.002(2) Cl1 0.0337(6) 0.0456(7) 0.0841(9) -0.0084(6) 0.0095(6) 0.0118(5) O1 0.057(2) 0.042(2) 0.057(2) 0.0098(15) 0.005(2) 0.001(2) O2 0.047(2) 0.048(2) 0.042(2) 0.0011(13) 0.0076(14) -0.0044(15) C1 0.035(2) 0.040(2) 0.032(2) 0.001(2) 0.009(2) -0.001(2) C2 0.042(3) 0.060(3) 0.051(3) 0.020(2) 0.011(2) 0.005(2) C3 0.055(3) 0.069(4) 0.065(3) 0.027(3) 0.003(3) 0.000(3) C4 0.065(3) 0.083(4) 0.044(3) 0.021(3) 0.012(2) -0.022(3) C5 0.063(3) 0.072(4) 0.054(3) 0.009(3) 0.033(3) -0.009(3) C6 0.045(3) 0.048(3) 0.051(3) 0.003(2) 0.022(2) 0.001(2) C7 0.034(2) 0.040(2) 0.035(2) 0.004(2) 0.012(2) 0.003(2) C8 0.054(3) 0.053(3) 0.049(3) 0.013(2) 0.026(2) 0.009(2) C9 0.072(4) 0.086(4) 0.056(3) 0.019(3) 0.041(3) 0.024(3) C10 0.064(3) 0.075(4) 0.045(3) -0.005(2) 0.018(2) 0.020(3) C11 0.054(3) 0.051(3) 0.062(3) -0.012(2) 0.012(3) 0.004(2) C12 0.047(3) 0.044(3) 0.052(3) -0.002(2) 0.020(2) 0.002(2) C13 0.029(2) 0.047(3) 0.050(2) 0.010(2) 0.005(2) 0.001(2) C14 0.039(2) 0.046(3) 0.042(2) 0.004(2) 0.010(2) 0.000(2) C15 0.082(4) 0.073(4) 0.049(3) 0.010(3) 0.005(3) 0.002(3) C16 0.074(4) 0.064(4) 0.082(4) -0.009(3) 0.011(3) 0.024(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 Pd1 Cl1 2.2957(12) . ? Pd1 Cl1 2.2957(12) 2 ? Pd1 P1 2.3304(12) . ? Pd1 P1 2.3304(12) 2 ? P1 N1 1.644(4) . ? P1 C1 1.827(4) . ? P1 C7 1.827(4) . ? N1 C13 1.456(6) . ? O1 C16 1.405(7) . ? O1 C14 1.419(6) . ? O2 C14 1.398(5) . ? O2 C15 1.445(6) . ? C1 C6 1.378(6) . ? C1 C2 1.391(6) . ? C2 C3 1.383(7) . ? C3 C4 1.377(9) . ? C4 C5 1.365(8) . ? C5 C6 1.391(7) . ? C7 C12 1.376(6) . ? C7 C8 1.394(6) . ? C8 C9 1.374(7) . ? C9 C10 1.360(8) . ? C10 C11 1.373(8) . ? C11 C12 1.376(7) . ? C13 C14 1.499(6) . ? 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 Cl1 Pd1 Cl1 180.0 . 2 ? Cl1 Pd1 P1 88.23(4) . . ? Cl1 Pd1 P1 91.77(4) 2 . ? Cl1 Pd1 P1 91.77(4) . 2 ? Cl1 Pd1 P1 88.23(4) 2 2 ? P1 Pd1 P1 180.0 . 2 ? N1 P1 C1 107.3(2) . . ? N1 P1 C7 105.1(2) . . ? C1 P1 C7 102.8(2) . . ? N1 P1 Pd1 111.31(14) . . ? C1 P1 Pd1 112.17(13) . . ? C7 P1 Pd1 117.34(14) . . ? C13 N1 P1 127.9(3) . . ? C16 O1 C14 114.8(4) . . ? C14 O2 C15 113.2(4) . . ? C6 C1 C2 120.1(4) . . ? C6 C1 P1 119.3(3) . . ? C2 C1 P1 120.6(3) . . ? C3 C2 C1 119.1(5) . . ? C4 C3 C2 120.7(5) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 120.3(5) . . ? C1 C6 C5 119.8(5) . . ? C12 C7 C8 118.6(4) . . ? C12 C7 P1 121.7(3) . . ? C8 C7 P1 119.5(3) . . ? C9 C8 C7 119.7(5) . . ? C10 C9 C8 121.2(5) . . ? C9 C10 C11 119.6(5) . . ? C10 C11 C12 120.0(5) . . ? C7 C12 C11 120.9(5) . . ? N1 C13 C14 110.8(4) . . ? O2 C14 O1 111.9(4) . . ? O2 C14 C13 107.2(4) . . ? O1 C14 C13 112.5(4) . . ? _refine_diff_density_max 1.250 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.211 data_98ab2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H40 Cl2 N2 O4 P2 Pd' _chemical_formula_weight 755.90 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 (no.2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.396(2) _cell_length_b 10.146(2) _cell_length_c 10.849(3) _cell_angle_alpha 94.97(2) _cell_angle_beta 111.01(2) _cell_angle_gamma 94.71(2) _cell_volume 853.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method ? _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3413 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2981 _reflns_number_observed 2589 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+0.1009P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2973 _refine_ls_number_parameters 202 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_obs 0.0518 _refine_ls_wR_factor_all 0.1459 _refine_ls_wR_factor_obs 0.1298 _refine_ls_goodness_of_fit_all 1.223 _refine_ls_goodness_of_fit_obs 1.292 _refine_ls_restrained_S_all 1.351 _refine_ls_restrained_S_obs 1.292 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.0000 0.0327(2) Uani 1 d S . P1 P -0.22461(13) -0.16937(10) -0.10983(10) 0.0329(3) Uani 1 d . . N1 N -0.4053(5) -0.1083(4) -0.1848(4) 0.0438(9) Uani 1 d D . H1 H -0.4072(52) -0.0221(27) -0.1687(39) 0.028(10) Uiso 1 d D . Cl1 Cl 0.18808(15) -0.15456(12) 0.01112(14) 0.0585(4) Uani 1 d . . O1 O -0.6280(5) 0.0224(3) -0.3912(3) 0.0565(9) Uani 1 d . . O2 O -0.7614(4) -0.1879(3) -0.5019(3) 0.0491(8) Uani 1 d . . C1 C -0.2633(5) -0.2794(4) 0.0038(4) 0.0370(9) Uani 1 d . . C2 C -0.1499(6) -0.3706(5) 0.0567(5) 0.0519(12) Uani 1 d . . H2 H -0.0537(6) -0.3771(5) 0.0341(5) 0.062 Uiso 1 calc R . C3 C -0.1821(7) -0.4514(6) 0.1436(6) 0.067(2) Uani 1 d . . H3 H -0.1075(7) -0.5132(6) 0.1787(6) 0.081 Uiso 1 calc R . C4 C -0.3233(8) -0.4414(6) 0.1786(5) 0.067(2) Uani 1 d . . H4 H -0.3439(8) -0.4965(6) 0.2368(5) 0.081 Uiso 1 calc R . C5 C -0.4328(7) -0.3505(6) 0.1279(5) 0.0608(14) Uani 1 d . . H5 H -0.5272(7) -0.3430(6) 0.1527(5) 0.073 Uiso 1 calc R . C6 C -0.4040(6) -0.2690(5) 0.0394(5) 0.0471(11) Uani 1 d . . H6 H -0.4795(6) -0.2078(5) 0.0045(5) 0.057 Uiso 1 calc R . C7 C -0.1994(5) -0.2858(4) -0.2379(4) 0.0368(9) Uani 1 d . . C8 C -0.1061(6) -0.2412(5) -0.3129(5) 0.0496(11) Uani 1 d . . H8 H -0.0496(6) -0.1549(5) -0.2932(5) 0.059 Uiso 1 calc R . C9 C -0.0980(8) -0.3255(6) -0.4161(5) 0.0646(15) Uani 1 d . . H9 H -0.0347(8) -0.2957(6) -0.4653(5) 0.078 Uiso 1 calc R . C10 C -0.1809(7) -0.4518(6) -0.4475(5) 0.0622(14) Uani 1 d . . H10 H -0.1749(7) -0.5075(6) -0.5181(5) 0.075 Uiso 1 calc R . C11 C -0.2733(7) -0.4966(5) -0.3744(5) 0.0600(13) Uani 1 d . . H11 H -0.3301(7) -0.5829(5) -0.3953(5) 0.072 Uiso 1 calc R . C12 C -0.2821(6) -0.4139(5) -0.2703(5) 0.0482(11) Uani 1 d . . H12 H -0.3448(6) -0.4450(5) -0.2211(5) 0.058 Uiso 1 calc R . C13 C -0.5636(5) -0.1778(5) -0.2848(4) 0.0447(10) Uani 1 d . . H13A H -0.6560(5) -0.1752(5) -0.2512(4) 0.054 Uiso 1 calc R . H13B H -0.5491(5) -0.2705(5) -0.3028(4) 0.054 Uiso 1 calc R . C14 C -0.6101(6) -0.1149(5) -0.4111(4) 0.0442(10) Uani 1 d . . H14 H -0.5187(6) -0.1233(5) -0.4465(4) 0.053 Uiso 1 calc R . C15 C -0.8036(8) -0.1548(6) -0.6360(5) 0.073(2) Uani 1 d . . H15A H -0.9075(34) -0.2084(34) -0.6938(10) 0.110 Uiso 1 calc R . H15B H -0.7116(28) -0.1717(44) -0.6658(18) 0.110 Uiso 1 calc R . H15C H -0.8197(59) -0.0623(13) -0.6374(10) 0.110 Uiso 1 calc R . C16 C -0.7630(8) 0.0493(6) -0.3488(7) 0.079(2) Uani 1 d . . H16A H -0.7617(39) 0.1440(6) -0.3324(47) 0.118 Uiso 1 calc R . H16B H -0.7488(36) 0.0107(42) -0.2683(27) 0.118 Uiso 1 calc R . H16C H -0.8706(9) 0.0118(43) -0.4165(21) 0.118 Uiso 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 0.0257(3) 0.0332(3) 0.0381(3) 0.0031(2) 0.0106(2) 0.0033(2) P1 0.0282(6) 0.0331(6) 0.0362(6) 0.0037(4) 0.0111(4) 0.0022(4) N1 0.032(2) 0.036(2) 0.053(2) 0.004(2) 0.005(2) 0.002(2) Cl1 0.0337(6) 0.0456(7) 0.0841(9) -0.0084(6) 0.0095(6) 0.0118(5) O1 0.057(2) 0.042(2) 0.057(2) 0.0098(15) 0.005(2) 0.001(2) O2 0.047(2) 0.048(2) 0.042(2) 0.0011(13) 0.0076(14) -0.0044(15) C1 0.035(2) 0.040(2) 0.032(2) 0.001(2) 0.009(2) -0.001(2) C2 0.042(3) 0.060(3) 0.051(3) 0.020(2) 0.011(2) 0.005(2) C3 0.055(3) 0.069(4) 0.065(3) 0.027(3) 0.003(3) 0.000(3) C4 0.065(3) 0.083(4) 0.044(3) 0.021(3) 0.012(2) -0.022(3) C5 0.063(3) 0.072(4) 0.054(3) 0.009(3) 0.033(3) -0.009(3) C6 0.045(3) 0.048(3) 0.051(3) 0.003(2) 0.022(2) 0.001(2) C7 0.034(2) 0.040(2) 0.035(2) 0.004(2) 0.012(2) 0.003(2) C8 0.054(3) 0.053(3) 0.049(3) 0.013(2) 0.026(2) 0.009(2) C9 0.072(4) 0.086(4) 0.056(3) 0.019(3) 0.041(3) 0.024(3) C10 0.064(3) 0.075(4) 0.045(3) -0.005(2) 0.018(2) 0.020(3) C11 0.054(3) 0.051(3) 0.062(3) -0.012(2) 0.012(3) 0.004(2) C12 0.047(3) 0.044(3) 0.052(3) -0.002(2) 0.020(2) 0.002(2) C13 0.029(2) 0.047(3) 0.050(2) 0.010(2) 0.005(2) 0.001(2) C14 0.039(2) 0.046(3) 0.042(2) 0.004(2) 0.010(2) 0.000(2) C15 0.082(4) 0.073(4) 0.049(3) 0.010(3) 0.005(3) 0.002(3) C16 0.074(4) 0.064(4) 0.082(4) -0.009(3) 0.011(3) 0.024(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 Pd1 Cl1 2.2957(12) . ? Pd1 Cl1 2.2957(12) 2 ? Pd1 P1 2.3304(12) . ? Pd1 P1 2.3304(12) 2 ? P1 N1 1.644(4) . ? P1 C1 1.827(4) . ? P1 C7 1.827(4) . ? N1 C13 1.456(6) . ? O1 C16 1.405(7) . ? O1 C14 1.419(6) . ? O2 C14 1.398(5) . ? O2 C15 1.445(6) . ? C1 C6 1.378(6) . ? C1 C2 1.391(6) . ? C2 C3 1.383(7) . ? C3 C4 1.377(9) . ? C4 C5 1.365(8) . ? C5 C6 1.391(7) . ? C7 C12 1.376(6) . ? C7 C8 1.394(6) . ? C8 C9 1.374(7) . ? C9 C10 1.360(8) . ? C10 C11 1.373(8) . ? C11 C12 1.376(7) . ? C13 C14 1.499(6) . ? 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 Cl1 Pd1 Cl1 180.0 . 2 ? Cl1 Pd1 P1 88.23(4) . . ? Cl1 Pd1 P1 91.77(4) 2 . ? Cl1 Pd1 P1 91.77(4) . 2 ? Cl1 Pd1 P1 88.23(4) 2 2 ? P1 Pd1 P1 180.0 . 2 ? N1 P1 C1 107.3(2) . . ? N1 P1 C7 105.1(2) . . ? C1 P1 C7 102.8(2) . . ? N1 P1 Pd1 111.31(14) . . ? C1 P1 Pd1 112.17(13) . . ? C7 P1 Pd1 117.34(14) . . ? C13 N1 P1 127.9(3) . . ? C16 O1 C14 114.8(4) . . ? C14 O2 C15 113.2(4) . . ? C6 C1 C2 120.1(4) . . ? C6 C1 P1 119.3(3) . . ? C2 C1 P1 120.6(3) . . ? C3 C2 C1 119.1(5) . . ? C4 C3 C2 120.7(5) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 120.3(5) . . ? C1 C6 C5 119.8(5) . . ? C12 C7 C8 118.6(4) . . ? C12 C7 P1 121.7(3) . . ? C8 C7 P1 119.5(3) . . ? C9 C8 C7 119.7(5) . . ? C10 C9 C8 121.2(5) . . ? C9 C10 C11 119.6(5) . . ? C10 C11 C12 120.0(5) . . ? C7 C12 C11 120.9(5) . . ? N1 C13 C14 110.8(4) . . ? O2 C14 O1 111.9(4) . . ? O2 C14 C13 107.2(4) . . ? O1 C14 C13 112.5(4) . . ? _refine_diff_density_max 1.250 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.211 #===end data_Complex14 #(98ab5) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H36 Br N3 O4 P2 Pt' _chemical_formula_weight 839.56 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.576(2) _cell_length_b 24.119(5) _cell_length_c 14.306(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.09(2) _cell_angle_gamma 90.00 _cell_volume 3190.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method ? _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 5.790 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5596 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.97 _reflns_number_total 5596 _reflns_number_observed 4518 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+3.1962P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5587 _refine_ls_number_parameters 381 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_obs 0.0325 _refine_ls_wR_factor_all 0.0949 _refine_ls_wR_factor_obs 0.0887 _refine_ls_goodness_of_fit_all 1.091 _refine_ls_goodness_of_fit_obs 1.181 _refine_ls_restrained_S_all 1.129 _refine_ls_restrained_S_obs 1.184 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.20889(2) 0.129670(9) 0.216519(14) 0.03068(11) Uani 1 d . . Br1 Br 0.45094(7) 0.08451(3) 0.25843(5) 0.0544(2) Uani 1 d . . P1 P -0.0065(2) 0.17298(6) 0.16619(10) 0.0334(3) Uani 1 d . . P2 P 0.1421(2) 0.08083(6) 0.33335(10) 0.0341(3) Uani 1 d . . N1 N -0.1413(5) 0.1283(2) 0.1520(4) 0.0412(12) Uani 1 d D . H1A H -0.0948(63) 0.0923(16) 0.1592(45) 0.048(18) Uiso 1 d D . N2 N 0.2868(6) 0.0649(2) 0.4220(4) 0.0464(13) Uani 1 d D . H2A H 0.3664(58) 0.0508(30) 0.3984(50) 0.074(23) Uiso 1 d D . N3 N 0.2894(6) 0.1692(3) 0.1064(3) 0.054(2) Uani 1 d D . O1 O 0.2751(7) 0.1409(3) 0.0335(4) 0.094(2) Uani 1 d D . O2 O 0.3430(6) 0.2152(3) 0.1261(5) 0.103(3) Uani 1 d D . O3 O -0.2943(6) 0.0724(2) -0.0215(4) 0.0699(15) Uani 1 d . . O4 O 0.5309(6) 0.0618(3) 0.5792(4) 0.074(2) Uani 1 d . . C1 C -0.0315(6) 0.2278(2) 0.2460(4) 0.0382(13) Uani 1 d . . C2 C -0.1620(7) 0.2354(3) 0.2701(5) 0.056(2) Uani 1 d . . H2 H -0.2387(7) 0.2111(3) 0.2472(5) 0.067 Uiso 1 calc R . C3 C -0.1760(8) 0.2801(3) 0.3290(7) 0.071(2) Uani 1 d . . H3 H -0.2625(8) 0.2852(3) 0.3460(7) 0.085 Uiso 1 calc R . C4 C -0.0646(9) 0.3162(3) 0.3621(6) 0.070(2) Uani 1 d . . H4 H -0.0764(9) 0.3463(3) 0.4000(6) 0.084 Uiso 1 calc R . C5 C 0.0648(8) 0.3081(3) 0.3397(5) 0.057(2) Uani 1 d . . H5 H 0.1414(8) 0.3324(3) 0.3632(5) 0.068 Uiso 1 calc R . C6 C 0.0810(7) 0.2639(3) 0.2821(5) 0.048(2) Uani 1 d . . H6 H 0.1691(7) 0.2584(3) 0.2676(5) 0.057 Uiso 1 calc R . C7 C -0.0301(6) 0.2071(2) 0.0501(4) 0.0382(13) Uani 1 d . . C8 C -0.0456(7) 0.1754(3) -0.0321(4) 0.048(2) Uani 1 d . . H8 H -0.0515(7) 0.1370(3) -0.0281(4) 0.057 Uiso 1 calc R . C9 C -0.0525(7) 0.2000(3) -0.1206(5) 0.057(2) Uani 1 d . . H9 H -0.0629(7) 0.1782(3) -0.1756(5) 0.069 Uiso 1 calc R . C10 C -0.0441(7) 0.2568(4) -0.1272(6) 0.062(2) Uani 1 d . . H10 H -0.0465(7) 0.2733(4) -0.1864(6) 0.074 Uiso 1 calc R . C11 C -0.0320(7) 0.2891(3) -0.0463(6) 0.059(2) Uani 1 d . . H11 H -0.0295(7) 0.3275(3) -0.0516(6) 0.071 Uiso 1 calc R . C12 C -0.0237(7) 0.2654(3) 0.0417(5) 0.0465(15) Uani 1 d . . H12 H -0.0138(7) 0.2876(3) 0.0962(5) 0.056 Uiso 1 calc R . C13 C -0.2941(7) 0.1369(3) 0.1007(5) 0.048(2) Uani 1 d . . H13A H -0.3011(7) 0.1658(3) 0.0524(5) 0.058 Uiso 1 calc R . H13B H -0.3469(7) 0.1491(3) 0.1463(5) 0.058 Uiso 1 calc R . C14 C -0.3599(7) 0.0853(3) 0.0528(5) 0.054(2) Uani 1 d . . H14A H -0.3452(7) 0.0553(3) 0.0995(5) 0.064 Uiso 1 calc R . H14B H -0.4631(7) 0.0904(3) 0.0262(5) 0.064 Uiso 1 calc R . C15 C -0.3510(11) 0.0244(4) -0.0724(7) 0.093(3) Uani 1 d . . H15A H -0.2917(46) 0.0138(18) -0.1141(40) 0.139 Uiso 1 calc R . H15B H -0.4476(30) 0.0316(9) -0.1106(41) 0.139 Uiso 1 calc R . H15C H -0.3525(74) -0.0050(9) -0.0274(7) 0.139 Uiso 1 calc R . C16 C 0.0277(7) 0.1147(2) 0.3993(4) 0.0389(13) Uani 1 d . . C17 C 0.0872(7) 0.1579(3) 0.4606(4) 0.0428(14) Uani 1 d . . H17 H 0.1831(7) 0.1678(3) 0.4669(4) 0.051 Uiso 1 calc R . C18 C 0.0083(8) 0.1864(3) 0.5122(5) 0.058(2) Uani 1 d . . H18 H 0.0494(8) 0.2158(3) 0.5521(5) 0.070 Uiso 1 calc R . C19 C -0.1332(8) 0.1709(3) 0.5041(6) 0.065(2) Uani 1 d . . H19 H -0.1871(8) 0.1895(3) 0.5397(6) 0.078 Uiso 1 calc R . C20 C -0.1953(8) 0.1279(3) 0.4437(6) 0.060(2) Uani 1 d . . H20 H -0.2907(8) 0.1178(3) 0.4387(6) 0.072 Uiso 1 calc R . C21 C -0.1170(6) 0.1002(3) 0.3911(4) 0.0438(14) Uani 1 d . . H21 H -0.1597(6) 0.0716(3) 0.3497(4) 0.053 Uiso 1 calc R . C22 C 0.0454(6) 0.0184(2) 0.2813(5) 0.0418(14) Uani 1 d . . C23 C 0.0259(8) 0.0074(3) 0.1823(5) 0.054(2) Uani 1 d . . H23 H 0.0644(8) 0.0318(3) 0.1453(5) 0.065 Uiso 1 calc R . C24 C -0.0489(10) -0.0387(3) 0.1385(6) 0.074(2) Uani 1 d . . H24 H -0.0635(10) -0.0445(3) 0.0724(6) 0.089 Uiso 1 calc R . C25 C -0.1011(9) -0.0756(3) 0.1931(8) 0.080(3) Uani 1 d . . H25 H -0.1529(9) -0.1065(3) 0.1642(8) 0.096 Uiso 1 calc R . C26 C -0.0769(9) -0.0671(3) 0.2909(7) 0.075(2) Uani 1 d . . H26 H -0.1096(9) -0.0933(3) 0.3280(7) 0.089 Uiso 1 calc R . C27 C -0.0048(8) -0.0203(3) 0.3359(6) 0.060(2) Uani 1 d . . H27 H 0.0096(8) -0.0152(3) 0.4021(6) 0.072 Uiso 1 calc R . C28 C 0.2878(8) 0.0375(3) 0.5143(5) 0.053(2) Uani 1 d . . H28A H 0.3116(8) -0.0014(3) 0.5107(5) 0.064 Uiso 1 calc R . H28B H 0.1921(8) 0.0398(3) 0.5251(5) 0.064 Uiso 1 calc R . C29 C 0.3941(8) 0.0636(4) 0.5967(5) 0.066(2) Uani 1 d . . H29A H 0.3668(8) 0.1018(4) 0.6040(5) 0.079 Uiso 1 calc R . H29B H 0.3957(8) 0.0440(4) 0.6561(5) 0.079 Uiso 1 calc R . C30 C 0.6425(9) 0.0847(4) 0.6546(6) 0.082(3) Uani 1 d . . H30A H 0.7329(16) 0.0821(26) 0.6376(23) 0.124 Uiso 1 calc R . H30B H 0.6490(50) 0.0645(18) 0.7134(13) 0.124 Uiso 1 calc R . H30C H 0.6213(38) 0.1229(9) 0.6639(34) 0.124 Uiso 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 Pt1 0.03110(14) 0.03001(14) 0.03095(14) 0.00156(9) 0.00812(9) 0.00058(9) Br1 0.0446(4) 0.0667(5) 0.0534(4) 0.0078(3) 0.0154(3) 0.0103(3) P1 0.0328(7) 0.0307(7) 0.0354(8) 0.0029(6) 0.0064(6) 0.0010(6) P2 0.0356(8) 0.0317(8) 0.0361(8) 0.0044(6) 0.0113(6) 0.0021(6) N1 0.038(3) 0.035(3) 0.047(3) 0.005(2) 0.005(2) 0.000(2) N2 0.042(3) 0.058(3) 0.041(3) 0.015(3) 0.013(2) 0.008(3) N3 0.035(3) 0.103(5) 0.020(3) 0.006(3) 0.000(2) 0.053(3) O1 0.086(4) 0.142(6) 0.064(4) 0.022(4) 0.037(3) 0.021(4) O2 0.069(4) 0.172(8) 0.074(4) 0.068(5) 0.029(3) 0.027(5) O3 0.071(3) 0.075(4) 0.066(3) -0.017(3) 0.020(3) -0.027(3) O4 0.055(3) 0.109(5) 0.056(3) -0.006(3) 0.010(2) 0.018(3) C1 0.045(3) 0.028(3) 0.040(3) 0.002(2) 0.008(3) 0.009(3) C2 0.043(4) 0.055(4) 0.075(5) -0.012(4) 0.024(3) -0.004(3) C3 0.058(4) 0.057(5) 0.109(6) -0.022(5) 0.040(4) 0.005(4) C4 0.081(6) 0.055(5) 0.078(5) -0.027(4) 0.029(5) -0.001(4) C5 0.058(4) 0.048(4) 0.060(4) -0.013(3) 0.010(4) -0.011(3) C6 0.039(3) 0.055(4) 0.046(4) -0.007(3) 0.005(3) 0.002(3) C7 0.032(3) 0.038(3) 0.043(3) 0.009(3) 0.007(3) 0.003(3) C8 0.052(4) 0.046(4) 0.043(4) 0.007(3) 0.008(3) 0.006(3) C9 0.054(4) 0.074(5) 0.042(4) 0.007(4) 0.009(3) 0.012(4) C10 0.039(4) 0.082(6) 0.059(5) 0.035(4) 0.004(3) 0.009(4) C11 0.045(4) 0.050(4) 0.078(5) 0.023(4) 0.009(4) -0.001(3) C12 0.042(3) 0.039(3) 0.054(4) 0.009(3) 0.006(3) 0.001(3) C13 0.036(3) 0.052(4) 0.054(4) -0.003(3) 0.007(3) -0.006(3) C14 0.043(4) 0.059(4) 0.056(4) -0.002(3) 0.007(3) -0.015(3) C15 0.099(7) 0.086(7) 0.090(6) -0.031(5) 0.018(6) -0.040(6) C16 0.044(3) 0.039(3) 0.034(3) 0.002(3) 0.010(3) 0.004(3) C17 0.044(3) 0.037(3) 0.047(3) -0.001(3) 0.012(3) -0.004(3) C18 0.066(5) 0.052(4) 0.058(4) -0.012(3) 0.017(4) -0.001(4) C19 0.071(5) 0.066(5) 0.068(5) -0.014(4) 0.033(4) 0.014(4) C20 0.048(4) 0.067(5) 0.069(5) -0.011(4) 0.023(4) 0.002(4) C21 0.039(3) 0.044(4) 0.049(3) -0.004(3) 0.013(3) -0.001(3) C22 0.044(3) 0.033(3) 0.052(4) -0.001(3) 0.020(3) 0.006(3) C23 0.072(5) 0.033(3) 0.058(4) -0.007(3) 0.017(4) -0.005(3) C24 0.107(7) 0.041(4) 0.078(5) -0.023(4) 0.029(5) -0.011(4) C25 0.076(6) 0.044(5) 0.122(8) -0.023(5) 0.030(6) -0.009(4) C26 0.079(6) 0.040(4) 0.114(7) 0.002(5) 0.042(5) -0.012(4) C27 0.066(5) 0.044(4) 0.079(5) 0.002(4) 0.035(4) -0.003(3) C28 0.059(4) 0.056(4) 0.045(4) 0.019(3) 0.017(3) 0.015(3) C29 0.061(5) 0.095(6) 0.043(4) 0.014(4) 0.018(3) 0.026(4) C30 0.078(6) 0.092(7) 0.066(5) -0.009(5) -0.001(5) 0.009(5) _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 Pt1 N3 2.150(6) . ? Pt1 P1 2.2564(15) . ? Pt1 P2 2.2684(14) . ? Pt1 Br1 2.4889(8) . ? P1 N1 1.653(5) . ? P1 C1 1.803(6) . ? P1 C7 1.814(6) . ? P2 N2 1.661(5) . ? P2 C16 1.816(6) . ? P2 C22 1.822(6) . ? N1 C13 1.471(8) . ? N2 C28 1.475(8) . ? N3 O1 1.2235(14) . ? N3 O2 1.2246(10) . ? O3 C15 1.399(9) . ? O3 C14 1.403(8) . ? O4 C29 1.396(8) . ? O4 C30 1.418(10) . ? C1 C6 1.376(9) . ? C1 C2 1.392(8) . ? C2 C3 1.395(10) . ? C3 C4 1.363(11) . ? C4 C5 1.373(10) . ? C5 C6 1.381(9) . ? C7 C8 1.380(9) . ? C7 C12 1.413(8) . ? C8 C9 1.384(9) . ? C9 C10 1.376(11) . ? C10 C11 1.376(11) . ? C11 C12 1.367(9) . ? C13 C14 1.480(9) . ? C16 C17 1.386(8) . ? C16 C21 1.404(8) . ? C17 C18 1.371(9) . ? C18 C19 1.381(10) . ? C19 C20 1.381(10) . ? C20 C21 1.368(9) . ? C22 C27 1.381(9) . ? C22 C23 1.405(9) . ? C23 C24 1.382(10) . ? C24 C25 1.362(12) . ? C25 C26 1.372(13) . ? C26 C27 1.390(11) . ? C28 C29 1.483(10) . ? 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 Pt1 P1 91.91(12) . . ? N3 Pt1 P2 173.86(13) . . ? P1 Pt1 P2 93.78(5) . . ? N3 Pt1 Br1 83.19(12) . . ? P1 Pt1 Br1 174.96(4) . . ? P2 Pt1 Br1 91.07(4) . . ? N1 P1 C1 109.2(3) . . ? N1 P1 C7 106.0(3) . . ? C1 P1 C7 103.9(3) . . ? N1 P1 Pt1 110.9(2) . . ? C1 P1 Pt1 113.5(2) . . ? C7 P1 Pt1 112.8(2) . . ? N2 P2 C16 101.8(3) . . ? N2 P2 C22 110.8(3) . . ? C16 P2 C22 105.8(3) . . ? N2 P2 Pt1 110.1(2) . . ? C16 P2 Pt1 118.2(2) . . ? C22 P2 Pt1 109.8(2) . . ? C13 N1 P1 127.8(4) . . ? C28 N2 P2 126.6(4) . . ? O1 N3 O2 130.4(7) . . ? O1 N3 Pt1 113.3(5) . . ? O2 N3 Pt1 116.3(4) . . ? C15 O3 C14 112.9(6) . . ? C29 O4 C30 114.1(6) . . ? C6 C1 C2 119.3(6) . . ? C6 C1 P1 118.8(4) . . ? C2 C1 P1 121.9(5) . . ? C1 C2 C3 119.0(7) . . ? C4 C3 C2 120.9(7) . . ? C3 C4 C5 120.0(7) . . ? C4 C5 C6 119.8(7) . . ? C1 C6 C5 120.9(6) . . ? C8 C7 C12 118.5(6) . . ? C8 C7 P1 119.2(5) . . ? C12 C7 P1 122.1(5) . . ? C7 C8 C9 120.6(6) . . ? C10 C9 C8 120.1(7) . . ? C11 C10 C9 120.0(7) . . ? C12 C11 C10 120.6(7) . . ? C11 C12 C7 120.1(7) . . ? N1 C13 C14 111.1(6) . . ? O3 C14 C13 108.4(5) . . ? C17 C16 C21 118.4(5) . . ? C17 C16 P2 117.6(5) . . ? C21 C16 P2 124.1(5) . . ? C18 C17 C16 121.6(6) . . ? C17 C18 C19 119.1(7) . . ? C18 C19 C20 120.6(6) . . ? C21 C20 C19 120.2(7) . . ? C20 C21 C16 120.2(6) . . ? C27 C22 C23 117.8(6) . . ? C27 C22 P2 122.9(5) . . ? C23 C22 P2 119.2(5) . . ? C24 C23 C22 121.8(7) . . ? C25 C24 C23 119.3(8) . . ? C24 C25 C26 119.9(8) . . ? C25 C26 C27 121.6(8) . . ? C22 C27 C26 119.5(7) . . ? N2 C28 C29 111.4(6) . . ? O4 C29 C28 109.0(6) . . ? _refine_diff_density_max 2.234 _refine_diff_density_min -1.754 _refine_diff_density_rms 0.115 #===end data_complex16 #(98ab1) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H30 Cl N2 O P Pd' _chemical_formula_weight 535.32 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 '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' 'P' 'P' 0.1023 0.0942 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.070(2) _cell_length_b 17.080(3) _cell_length_c 18.899(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4541.7(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method ? _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3785 _diffrn_reflns_av_R_equivalents 0.0020 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.06 _reflns_number_total 3715 _reflns_number_observed 2499 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3715 _refine_ls_number_parameters 277 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_obs 0.0534 _refine_ls_wR_factor_all 0.1446 _refine_ls_wR_factor_obs 0.1366 _refine_ls_goodness_of_fit_all 1.104 _refine_ls_goodness_of_fit_obs 1.296 _refine_ls_restrained_S_all 1.104 _refine_ls_restrained_S_obs 1.295 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.20322(3) 0.13707(2) 0.09754(2) 0.0343(2) Uani 1 d . . Cl1 Cl 0.09762(13) 0.23338(9) 0.05396(9) 0.0504(5) Uani 1 d . . P1 P 0.09827(12) 0.09585(9) 0.17903(8) 0.0355(4) Uani 1 d . . N1 N 0.0113(4) 0.1570(3) 0.1873(3) 0.0440(14) Uani 1 d D . H1 H -0.0064(43) 0.1938(28) 0.1498(23) 0.053 Uiso 1 d D . N2 N 0.3192(4) 0.1814(3) 0.0361(3) 0.0409(13) Uani 1 d . . O1 O -0.1518(5) 0.2600(4) 0.2007(3) 0.090(2) Uani 1 d . . C1 C 0.0410(5) 0.0048(3) 0.1637(3) 0.0385(15) Uani 1 d . . C2 C 0.0321(5) -0.0206(4) 0.0947(4) 0.054(2) Uani 1 d . . H2 H 0.0576(5) 0.0089(4) 0.0580(4) 0.065 Uiso 1 calc R . C3 C -0.0125(6) -0.0867(4) 0.0808(4) 0.059(2) Uani 1 d . . H3 H -0.0190(6) -0.1040(4) 0.0344(4) 0.070 Uiso 1 calc R . C4 C -0.0492(5) -0.1297(4) 0.1355(4) 0.056(2) Uani 1 d . . H4 H -0.0801(5) -0.1767(4) 0.1260(4) 0.067 Uiso 1 calc R . C5 C -0.0409(5) -0.1049(4) 0.2028(4) 0.056(2) Uani 1 d . . H5 H -0.0667(5) -0.1344(4) 0.2394(4) 0.067 Uiso 1 calc R . C6 C 0.0038(5) -0.0385(4) 0.2171(4) 0.049(2) Uani 1 d . . H6 H 0.0097(5) -0.0216(4) 0.2637(4) 0.059 Uiso 1 calc R . C7 C 0.1440(5) 0.0881(3) 0.2685(3) 0.0370(15) Uani 1 d . . C8 C 0.1278(5) 0.1458(4) 0.3164(3) 0.048(2) Uani 1 d . . H8 H 0.0922(5) 0.1893(4) 0.3030(3) 0.057 Uiso 1 calc R . C9 C 0.1632(6) 0.1417(4) 0.3857(4) 0.055(2) Uani 1 d . . H9 H 0.1490(6) 0.1812(4) 0.4179(4) 0.066 Uiso 1 calc R . C10 C 0.2169(5) 0.0814(5) 0.4055(4) 0.054(2) Uani 1 d . . H10 H 0.2407(5) 0.0787(5) 0.4513(4) 0.065 Uiso 1 calc R . C11 C 0.2362(5) 0.0250(4) 0.3590(4) 0.050(2) Uani 1 d . . H11 H 0.2742(5) -0.0169(4) 0.3726(4) 0.061 Uiso 1 calc R . C12 C 0.2001(5) 0.0279(4) 0.2903(3) 0.044(2) Uani 1 d . . H12 H 0.2147(5) -0.0121(4) 0.2588(3) 0.053 Uiso 1 calc R . C13 C 0.2938(4) 0.0513(4) 0.1091(3) 0.0355(14) Uani 1 d . . C14 C 0.2738(5) -0.0242(4) 0.1240(3) 0.044(2) Uani 1 d . . H14 H 0.2127(5) -0.0388(4) 0.1374(3) 0.053 Uiso 1 calc R . C15 C 0.3443(6) -0.0785(4) 0.1190(3) 0.048(2) Uani 1 d . . H15 H 0.3300(6) -0.1306(4) 0.1285(3) 0.058 Uiso 1 calc R . C16 C 0.4345(5) -0.0595(4) 0.1008(4) 0.054(2) Uani 1 d . . H16 H 0.4810(5) -0.0983(4) 0.0998(4) 0.064 Uiso 1 calc R . C17 C 0.4575(5) 0.0134(4) 0.0844(3) 0.052(2) Uani 1 d . . H17 H 0.5190(5) 0.0266(4) 0.0709(3) 0.062 Uiso 1 calc R . C18 C 0.3870(5) 0.0685(4) 0.0880(3) 0.043(2) Uani 1 d . . C19 C -0.0780(5) 0.1407(4) 0.2249(4) 0.046(2) Uani 1 d . . H19A H -0.0654(5) 0.1062(4) 0.2645(4) 0.056 Uiso 1 calc R . H19B H -0.1216(5) 0.1142(4) 0.1932(4) 0.056 Uiso 1 calc R . C20 C -0.1238(6) 0.2152(5) 0.2517(5) 0.084(3) Uani 1 d . . H20A H -0.1779(6) 0.2018(5) 0.2812(5) 0.101 Uiso 1 calc R . H20B H -0.0785(6) 0.2434(5) 0.2808(5) 0.101 Uiso 1 calc R . C21 C -0.2017(7) 0.3213(5) 0.2282(6) 0.105(4) Uani 1 d . . H21A H -0.2053(47) 0.3626(18) 0.1939(16) 0.158 Uiso 1 calc R . H21B H -0.1702(31) 0.3402(29) 0.2699(24) 0.158 Uiso 1 calc R . H21C H -0.2647(19) 0.3043(12) 0.2402(38) 0.158 Uiso 1 calc R . C22 C 0.4067(5) 0.1471(4) 0.0681(4) 0.044(2) Uani 1 d . . H22A H 0.4583(5) 0.1482(4) 0.0341(4) 0.053 Uiso 1 calc R . H22B H 0.4256(5) 0.1772(4) 0.1092(4) 0.053 Uiso 1 calc R . C23 C 0.3096(5) 0.1552(5) -0.0390(4) 0.059(2) Uani 1 d . . H23A H 0.2513(17) 0.1751(23) -0.0584(9) 0.089 Uiso 1 calc R . H23B H 0.3090(34) 0.0991(5) -0.0408(4) 0.089 Uiso 1 calc R . H23C H 0.3622(19) 0.1747(23) -0.0661(6) 0.089 Uiso 1 calc R . C24 C 0.3286(5) 0.2639(4) 0.0359(5) 0.062(2) Uani 1 d . . H24A H 0.2724(16) 0.2869(4) 0.0161(26) 0.093 Uiso 1 calc R . H24B H 0.3827(22) 0.2784(4) 0.0079(23) 0.093 Uiso 1 calc R . H24C H 0.3371(37) 0.2822(5) 0.0835(5) 0.093 Uiso 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 0.0426(3) 0.0269(3) 0.0335(3) 0.0009(2) 0.0001(2) -0.0032(2) Cl1 0.0572(10) 0.0368(8) 0.0572(11) 0.0113(8) -0.0001(10) 0.0019(8) P1 0.0431(10) 0.0285(8) 0.0350(9) -0.0004(7) 0.0003(8) -0.0039(7) N1 0.055(3) 0.034(3) 0.043(3) 0.008(2) 0.007(3) 0.006(3) N2 0.049(3) 0.039(3) 0.035(3) -0.001(2) 0.003(3) -0.007(3) O1 0.106(5) 0.083(4) 0.081(4) 0.003(4) 0.016(4) 0.023(4) C1 0.046(4) 0.035(3) 0.034(4) -0.006(3) -0.006(3) -0.002(3) C2 0.072(5) 0.040(4) 0.050(4) 0.003(3) -0.015(4) 0.002(4) C3 0.077(6) 0.046(4) 0.053(5) -0.014(4) -0.016(4) 0.000(4) C4 0.056(5) 0.037(4) 0.074(6) -0.004(4) -0.011(4) -0.002(3) C5 0.062(5) 0.045(4) 0.060(5) 0.005(4) 0.000(4) -0.019(4) C6 0.061(5) 0.038(4) 0.048(4) -0.002(3) -0.001(4) -0.012(3) C7 0.044(4) 0.031(3) 0.036(4) -0.001(3) 0.002(3) -0.007(3) C8 0.057(4) 0.037(4) 0.049(4) -0.009(3) -0.009(4) -0.003(3) C9 0.064(5) 0.051(4) 0.050(4) -0.017(4) -0.002(4) -0.004(4) C10 0.060(5) 0.061(5) 0.042(4) 0.002(4) -0.010(4) -0.012(4) C11 0.057(5) 0.046(4) 0.048(4) 0.010(3) -0.006(4) -0.003(3) C12 0.056(4) 0.038(3) 0.039(4) 0.001(3) 0.000(3) -0.006(3) C13 0.038(4) 0.040(3) 0.029(3) -0.002(3) 0.006(3) 0.006(3) C14 0.053(4) 0.038(4) 0.042(4) -0.002(3) 0.005(3) 0.000(3) C15 0.066(5) 0.035(4) 0.044(4) -0.004(3) 0.001(4) 0.007(4) C16 0.055(5) 0.052(4) 0.053(4) -0.006(4) -0.001(4) 0.023(4) C17 0.047(4) 0.061(5) 0.046(5) -0.005(4) 0.008(3) 0.009(4) C18 0.052(4) 0.046(4) 0.033(4) -0.004(3) -0.009(3) -0.001(3) C19 0.044(4) 0.043(4) 0.052(4) -0.003(3) 0.005(3) -0.006(3) C20 0.056(5) 0.128(8) 0.068(5) 0.057(6) 0.031(4) 0.050(5) C21 0.129(9) 0.057(5) 0.130(10) -0.016(6) 0.021(7) 0.046(6) C22 0.038(4) 0.048(4) 0.045(4) 0.001(3) -0.007(3) -0.009(3) C23 0.062(5) 0.078(5) 0.038(4) 0.000(4) 0.001(4) -0.002(4) C24 0.066(5) 0.037(4) 0.084(6) 0.012(4) 0.003(5) -0.015(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 Pd1 C13 1.955(6) . ? Pd1 N2 2.141(5) . ? Pd1 P1 2.247(2) . ? Pd1 Cl1 2.365(2) . ? P1 N1 1.616(6) . ? P1 C1 1.775(6) . ? P1 C7 1.814(6) . ? N1 C19 1.470(8) . ? N2 C24 1.414(8) . ? N2 C22 1.491(8) . ? N2 C23 1.496(8) . ? O1 C20 1.293(9) . ? O1 C21 1.363(9) . ? C1 C6 1.356(9) . ? C1 C2 1.380(9) . ? C2 C3 1.319(9) . ? C3 C4 1.368(10) . ? C4 C5 1.347(10) . ? C5 C6 1.324(9) . ? C7 C8 1.358(8) . ? C7 C12 1.360(9) . ? C8 C9 1.402(9) . ? C9 C10 1.330(10) . ? C10 C11 1.332(10) . ? C11 C12 1.395(9) . ? C13 C14 1.349(9) . ? C13 C18 1.401(9) . ? C14 C15 1.362(9) . ? C15 C16 1.355(10) . ? C16 C17 1.323(10) . ? C17 C18 1.370(9) . ? C18 C22 1.422(8) . ? C19 C20 1.513(10) . ? 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 C13 Pd1 N2 80.1(2) . . ? C13 Pd1 P1 96.7(2) . . ? N2 Pd1 P1 169.53(14) . . ? C13 Pd1 Cl1 166.0(2) . . ? N2 Pd1 Cl1 92.53(15) . . ? P1 Pd1 Cl1 92.51(6) . . ? N1 P1 C1 103.8(3) . . ? N1 P1 C7 103.0(3) . . ? C1 P1 C7 104.4(3) . . ? N1 P1 Pd1 111.2(2) . . ? C1 P1 Pd1 117.4(2) . . ? C7 P1 Pd1 115.4(2) . . ? C19 N1 P1 124.9(4) . . ? C24 N2 C22 108.4(5) . . ? C24 N2 C23 107.6(6) . . ? C22 N2 C23 110.0(5) . . ? C24 N2 Pd1 115.2(4) . . ? C22 N2 Pd1 105.7(4) . . ? C23 N2 Pd1 109.9(4) . . ? C20 O1 C21 109.1(7) . . ? C6 C1 C2 119.8(6) . . ? C6 C1 P1 122.1(5) . . ? C2 C1 P1 118.1(5) . . ? C3 C2 C1 120.0(7) . . ? C2 C3 C4 119.2(7) . . ? C5 C4 C3 120.8(7) . . ? C6 C5 C4 120.2(7) . . ? C5 C6 C1 119.9(7) . . ? C8 C7 C12 116.3(6) . . ? C8 C7 P1 120.6(5) . . ? C12 C7 P1 122.9(5) . . ? C7 C8 C9 121.8(6) . . ? C10 C9 C8 120.3(7) . . ? C9 C10 C11 119.3(7) . . ? C10 C11 C12 120.9(7) . . ? C7 C12 C11 121.4(6) . . ? C14 C13 C18 117.1(6) . . ? C14 C13 Pd1 127.1(5) . . ? C18 C13 Pd1 114.9(5) . . ? C13 C14 C15 119.0(7) . . ? C16 C15 C14 122.5(7) . . ? C17 C16 C15 120.9(7) . . ? C16 C17 C18 117.2(7) . . ? C17 C18 C13 123.2(6) . . ? C17 C18 C22 119.6(7) . . ? C13 C18 C22 117.1(6) . . ? N1 C19 C20 111.5(5) . . ? O1 C20 C19 112.2(7) . . ? C18 C22 N2 108.5(5) . . ? _refine_diff_density_max 1.382 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.217 #===end data_complex18 #(pd) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H32 Cl N2 O P Pd' _chemical_formula_weight 549.35 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 P21/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 16.835(2) _cell_length_b 8.3350(9) _cell_length_c 19.590(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.922(2) _cell_angle_gamma 90.00 _cell_volume 2550.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14866 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5207 _reflns_number_observed 3775 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5207 _refine_ls_number_parameters 287 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_obs 0.0392 _refine_ls_wR_factor_all 0.1028 _refine_ls_wR_factor_obs 0.0942 _refine_ls_goodness_of_fit_all 0.906 _refine_ls_goodness_of_fit_obs 0.985 _refine_ls_restrained_S_all 0.907 _refine_ls_restrained_S_obs 0.986 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.17691(2) 0.45891(3) 0.372659(14) 0.04071(11) Uani 1 d . . P1 P 0.28970(5) 0.31410(10) 0.37312(5) 0.0371(2) Uani 1 d . . Cl1 Cl 0.22971(8) 0.4482(2) 0.50392(6) 0.0869(4) Uani 1 d . . C17 C 0.1272(2) 0.5048(4) 0.2627(2) 0.0444(8) Uani 1 d . . N2 N 0.0717(2) 0.6073(4) 0.3720(2) 0.0492(7) Uani 1 d . . C2 C 0.2190(2) 0.0496(4) 0.2887(2) 0.0455(8) Uani 1 d . . H2 H 0.1871(2) 0.0432(4) 0.3185(2) 0.055 Uiso 1 calc R . C1 C 0.2785(2) 0.1721(4) 0.2999(2) 0.0383(7) Uani 1 d . . C3 C 0.2066(2) -0.0630(4) 0.2337(2) 0.0544(9) Uani 1 d . . H3 H 0.1667(2) -0.1447(4) 0.2269(2) 0.065 Uiso 1 calc R . C4 C 0.2526(3) -0.0547(5) 0.1896(2) 0.0612(11) Uani 1 d . . H4 H 0.2437(3) -0.1298(5) 0.1524(2) 0.073 Uiso 1 calc R . C6 C 0.3253(3) 0.1771(5) 0.2553(2) 0.0561(10) Uani 1 d . . H6 H 0.3661(3) 0.2571(5) 0.2623(2) 0.067 Uiso 1 calc R . C5 C 0.3121(3) 0.0642(5) 0.2000(2) 0.0704(12) Uani 1 d . . H5 H 0.3438(3) 0.0693(5) 0.1700(2) 0.084 Uiso 1 calc R . C7 C 0.3764(2) 0.4463(4) 0.3748(2) 0.0410(8) Uani 1 d . . N1 N 0.3210(2) 0.1934(4) 0.4449(2) 0.0466(7) Uani 1 d D . H1 H 0.3101(20) 0.2272(40) 0.4799(14) 0.038(10) Uiso 1 d D . C13 C 0.3832(2) 0.0637(4) 0.4614(2) 0.0474(8) Uani 1 d . . H13A H 0.4350(2) 0.0965(4) 0.5014(2) 0.057 Uiso 1 calc R . H13B H 0.3977(2) 0.0444(4) 0.4186(2) 0.057 Uiso 1 calc R . C8 C 0.3598(2) 0.6028(4) 0.3499(2) 0.0505(9) Uani 1 d . . H8 H 0.3036(2) 0.6397(4) 0.3311(2) 0.061 Uiso 1 calc R . C22 C 0.0486(2) 0.5841(4) 0.2413(2) 0.0507(9) Uani 1 d . . C14 C 0.3512(3) -0.0907(5) 0.4824(2) 0.0582(10) Uani 1 d . . H14A H 0.2983(3) -0.1211(5) 0.4430(2) 0.070 Uiso 1 calc R . H14B H 0.3929(3) -0.1746(5) 0.4870(2) 0.070 Uiso 1 calc R . C18 C 0.1618(3) 0.4835(4) 0.2101(2) 0.0555(10) Uani 1 d . . H18 H 0.2143(3) 0.4315(4) 0.2229(2) 0.067 Uiso 1 calc R . C12 C 0.4613(2) 0.3961(5) 0.4026(2) 0.0631(11) Uani 1 d . . H12 H 0.4742(2) 0.2909(5) 0.4187(2) 0.076 Uiso 1 calc R . C23 C 0.0072(2) 0.5984(5) 0.2964(2) 0.0599(10) Uani 1 d . . H23A H -0.0282(2) 0.6941(5) 0.2862(2) 0.072 Uiso 1 calc R . H23B H -0.0296(2) 0.5064(5) 0.2922(2) 0.072 Uiso 1 calc R . C9 C 0.4258(3) 0.7056(5) 0.3526(2) 0.0596(10) Uani 1 d . . H9 H 0.4137(3) 0.8100(5) 0.3350(2) 0.071 Uiso 1 calc R . O1 O 0.4159(3) -0.0486(4) 0.6093(2) 0.0872(10) Uani 1 d . . C10 C 0.5087(3) 0.6526(5) 0.3812(2) 0.0589(10) Uani 1 d . . H10 H 0.5531(3) 0.7213(5) 0.3833(2) 0.071 Uiso 1 calc R . C21 C 0.0083(2) 0.6408(5) 0.1706(2) 0.0621(11) Uani 1 d . . H21 H -0.0434(2) 0.6956(5) 0.1580(2) 0.075 Uiso 1 calc R . C20 C 0.0439(3) 0.6168(5) 0.1185(2) 0.0699(12) Uani 1 d . . H20 H 0.0164(3) 0.6538(5) 0.0706(2) 0.084 Uiso 1 calc R . C19 C 0.1209(3) 0.5372(5) 0.1385(2) 0.0702(12) Uani 1 d . . H19 H 0.1455(3) 0.5194(5) 0.1039(2) 0.084 Uiso 1 calc R . C25 C 0.1074(3) 0.7725(5) 0.3887(3) 0.0727(12) Uani 1 d . . H25A H 0.1313(17) 0.8036(14) 0.3532(10) 0.109 Uiso 1 calc R . H25B H 0.1514(13) 0.7746(9) 0.4371(7) 0.109 Uiso 1 calc R . H25C H 0.0626(5) 0.8458(7) 0.3867(16) 0.109 Uiso 1 calc R . C24 C 0.0317(3) 0.5669(5) 0.4252(3) 0.0718(13) Uani 1 d . . H24A H -0.0182(12) 0.6325(27) 0.4159(11) 0.108 Uiso 1 calc R . H24B H 0.0718(8) 0.5861(37) 0.4743(3) 0.108 Uiso 1 calc R . H24C H 0.0153(19) 0.4558(11) 0.4200(12) 0.108 Uiso 1 calc R . C11 C 0.5263(3) 0.4997(6) 0.4066(3) 0.0694(12) Uani 1 d . . H11 H 0.5828(3) 0.4650(6) 0.4269(3) 0.083 Uiso 1 calc R . C15 C 0.3357(3) -0.0814(6) 0.5522(3) 0.0751(13) Uani 1 d . . H15A H 0.2951(3) 0.0034(6) 0.5493(3) 0.090 Uiso 1 calc R . H15B H 0.3127(3) -0.1821(6) 0.5615(3) 0.090 Uiso 1 calc R . C16 C 0.4153(5) -0.0653(8) 0.6794(3) 0.124(3) Uani 1 d . . H16A H 0.3689(22) -0.0041(52) 0.6833(10) 0.186 Uiso 1 calc R . H16B H 0.4686(15) -0.0270(60) 0.7148(4) 0.186 Uiso 1 calc R . H16C H 0.4081(35) -0.1764(11) 0.6887(11) 0.186 Uiso 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 0.0363(2) 0.0362(2) 0.0492(2) 0.00065(12) 0.01555(12) 0.00341(11) P1 0.0347(4) 0.0331(4) 0.0421(5) 0.0025(4) 0.0128(4) 0.0028(3) Cl1 0.0854(8) 0.1250(11) 0.0498(6) -0.0038(6) 0.0246(6) 0.0458(8) C17 0.040(2) 0.030(2) 0.056(2) 0.0091(15) 0.009(2) -0.0012(13) N2 0.0400(15) 0.035(2) 0.076(2) 0.0005(15) 0.025(2) 0.0026(13) C2 0.038(2) 0.047(2) 0.050(2) -0.001(2) 0.015(2) -0.001(2) C1 0.037(2) 0.033(2) 0.043(2) 0.0054(14) 0.0129(15) 0.0051(13) C3 0.048(2) 0.044(2) 0.063(2) -0.005(2) 0.011(2) -0.004(2) C4 0.069(3) 0.055(3) 0.057(2) -0.015(2) 0.021(2) 0.004(2) C6 0.065(2) 0.048(2) 0.067(3) -0.005(2) 0.037(2) -0.008(2) C5 0.086(3) 0.072(3) 0.069(3) -0.014(2) 0.047(3) -0.012(2) C7 0.039(2) 0.041(2) 0.043(2) -0.0057(15) 0.0143(15) -0.0032(14) N1 0.056(2) 0.043(2) 0.044(2) 0.0057(14) 0.023(2) 0.0129(14) C13 0.044(2) 0.045(2) 0.048(2) 0.009(2) 0.012(2) 0.007(2) C8 0.049(2) 0.037(2) 0.069(2) -0.003(2) 0.025(2) -0.001(2) C22 0.043(2) 0.033(2) 0.066(2) 0.006(2) 0.010(2) -0.0031(15) C14 0.059(2) 0.045(2) 0.061(2) 0.006(2) 0.011(2) -0.002(2) C18 0.061(2) 0.044(2) 0.056(2) 0.005(2) 0.014(2) 0.005(2) C12 0.041(2) 0.057(2) 0.087(3) 0.022(2) 0.019(2) 0.005(2) C23 0.041(2) 0.044(2) 0.086(3) 0.009(2) 0.014(2) 0.005(2) C9 0.073(3) 0.038(2) 0.075(3) -0.007(2) 0.036(2) -0.008(2) O1 0.120(3) 0.085(2) 0.057(2) 0.007(2) 0.033(2) -0.014(2) C10 0.059(2) 0.058(3) 0.066(3) -0.016(2) 0.029(2) -0.024(2) C21 0.052(2) 0.040(2) 0.075(3) 0.013(2) 0.000(2) 0.001(2) C20 0.077(3) 0.046(2) 0.061(3) 0.009(2) -0.005(2) -0.004(2) C19 0.089(3) 0.056(3) 0.057(3) 0.006(2) 0.018(2) 0.000(2) C25 0.071(3) 0.039(2) 0.111(4) -0.010(2) 0.038(3) -0.001(2) C24 0.066(3) 0.070(3) 0.094(3) -0.001(2) 0.047(3) 0.008(2) C11 0.039(2) 0.077(3) 0.087(3) 0.010(2) 0.018(2) -0.009(2) C15 0.089(3) 0.060(3) 0.080(3) 0.017(2) 0.035(3) -0.007(2) C16 0.188(7) 0.120(6) 0.071(4) 0.001(3) 0.056(4) -0.018(5) _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 C17 2.034(4) . ? Pd1 N2 2.156(3) . ? Pd1 P1 2.2472(8) . ? Pd1 Cl1 2.3882(11) . ? P1 N1 1.648(3) . ? P1 C1 1.815(3) . ? P1 C7 1.820(3) . ? C17 C18 1.372(5) . ? C17 C22 1.396(5) . ? N2 C23 1.475(5) . ? N2 C24 1.476(5) . ? N2 C25 1.490(5) . ? C2 C3 1.384(5) . ? C2 C1 1.389(5) . ? C1 C6 1.378(4) . ? C3 C4 1.361(5) . ? C4 C5 1.369(6) . ? C6 C5 1.389(5) . ? C7 C8 1.384(5) . ? C7 C12 1.390(5) . ? N1 C13 1.455(4) . ? C13 C14 1.510(5) . ? C8 C9 1.389(5) . ? C22 C21 1.379(5) . ? C22 C23 1.493(5) . ? C14 C15 1.487(6) . ? C18 C19 1.386(5) . ? C12 C11 1.373(5) . ? C9 C10 1.368(6) . ? O1 C16 1.383(6) . ? O1 C15 1.421(6) . ? C10 C11 1.361(6) . ? C21 C20 1.378(6) . ? C20 C19 1.377(6) . ? 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 N2 82.72(13) . . ? C17 Pd1 P1 96.80(10) . . ? N2 Pd1 P1 177.49(8) . . ? C17 Pd1 Cl1 170.91(10) . . ? N2 Pd1 Cl1 90.16(9) . . ? P1 Pd1 Cl1 90.07(3) . . ? N1 P1 C1 100.53(15) . . ? N1 P1 C7 110.8(2) . . ? C1 P1 C7 104.82(14) . . ? N1 P1 Pd1 109.37(11) . . ? C1 P1 Pd1 120.57(10) . . ? C7 P1 Pd1 110.23(11) . . ? C18 C17 C22 117.2(3) . . ? C18 C17 Pd1 130.4(3) . . ? C22 C17 Pd1 112.1(3) . . ? C23 N2 C24 109.8(3) . . ? C23 N2 C25 110.7(3) . . ? C24 N2 C25 108.0(3) . . ? C23 N2 Pd1 105.8(2) . . ? C24 N2 Pd1 117.1(2) . . ? C25 N2 Pd1 105.4(2) . . ? C3 C2 C1 120.7(3) . . ? C6 C1 C2 118.2(3) . . ? C6 C1 P1 124.4(3) . . ? C2 C1 P1 117.4(2) . . ? C4 C3 C2 120.2(3) . . ? C3 C4 C5 120.1(4) . . ? C1 C6 C5 120.7(4) . . ? C4 C5 C6 120.1(4) . . ? C8 C7 C12 117.7(3) . . ? C8 C7 P1 120.6(3) . . ? C12 C7 P1 121.7(3) . . ? C13 N1 P1 128.1(2) . . ? N1 C13 C14 113.2(3) . . ? C7 C8 C9 121.0(3) . . ? C21 C22 C17 121.4(4) . . ? C21 C22 C23 120.7(3) . . ? C17 C22 C23 117.8(3) . . ? C15 C14 C13 114.1(3) . . ? C17 C18 C19 121.9(4) . . ? C11 C12 C7 120.9(4) . . ? N2 C23 C22 111.2(3) . . ? C10 C9 C8 119.7(4) . . ? C16 O1 C15 114.0(4) . . ? C11 C10 C9 120.1(4) . . ? C22 C21 C20 120.5(4) . . ? C19 C20 C21 118.9(4) . . ? C20 C19 C18 120.2(4) . . ? C10 C11 C12 120.6(4) . . ? O1 C15 C14 107.1(4) . . ? _refine_diff_density_max 0.841 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.086 #===end data_Complex30 #(98ab4) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C43 H46 Cl2 N2 O2 P2 Pt2' _chemical_formula_weight 1145.84 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.877(5) _cell_length_b 20.984(7) _cell_length_c 15.345(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.09(3) _cell_angle_gamma 90.00 _cell_volume 4271.1(25) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method ? _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 6.781 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6620 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2245 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 23.98 _reflns_number_total 6620 _reflns_number_observed 3521 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6614 _refine_ls_number_parameters 482 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1541 _refine_ls_R_factor_obs 0.0715 _refine_ls_wR_factor_all 0.1776 _refine_ls_wR_factor_obs 0.1449 _refine_ls_goodness_of_fit_all 0.951 _refine_ls_goodness_of_fit_obs 1.189 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.186 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.12639(5) 0.11084(4) 0.01812(5) 0.0338(2) Uani 1 d . . Pt2 Pt 0.28289(5) 0.26449(4) 0.16800(5) 0.0343(2) Uani 1 d . . P1 P 0.0691(3) 0.2057(2) 0.0400(3) 0.0311(12) Uani 1 d . . P2 P 0.3233(3) 0.1620(3) 0.1796(3) 0.0329(12) Uani 1 d . . Cl1 Cl 0.7361(11) 0.1028(10) 0.2973(10) 0.296(11) Uani 1 d . . Cl2 Cl 0.7687(13) 0.0959(8) 0.4805(11) 0.283(9) Uani 1 d . . N1 N 0.1849(10) 0.0182(7) -0.0012(10) 0.037(4) Uani 1 d . . N2 N 0.2400(12) 0.3632(8) 0.1645(11) 0.045(4) Uani 1 d . . O1 O 0.2330(8) 0.1149(6) 0.1489(8) 0.035(3) Uani 1 d . . O2 O 0.1295(8) 0.2401(6) 0.1269(8) 0.044(4) Uani 1 d . . C1 C 0.0711(14) 0.2629(10) -0.0542(12) 0.042(5) Uani 1 d . . C2 C 0.0048(15) 0.3142(11) -0.0779(16) 0.072(8) Uani 1 d . . H2 H -0.0501(15) 0.3184(11) -0.0552(16) 0.086 Uiso 1 calc R . C3 C 0.0257(15) 0.3604(12) -0.1393(15) 0.063(7) Uani 1 d . . H3 H -0.0128(15) 0.3972(12) -0.1550(15) 0.075 Uiso 1 calc R . C4 C 0.1070(16) 0.3477(14) -0.1750(15) 0.079(9) Uani 1 d . . H4 H 0.1188(16) 0.3764(14) -0.2169(15) 0.095 Uiso 1 calc R . C5 C 0.1697(14) 0.2956(10) -0.1516(13) 0.049(4) Uani 1 d U . H5 H 0.2226(14) 0.2893(10) -0.1764(13) 0.059 Uiso 1 calc R . C6 C 0.1510(13) 0.2532(10) -0.0901(12) 0.048(4) Uani 1 d U . H6 H 0.1923(13) 0.2177(10) -0.0723(12) 0.057 Uiso 1 calc R . C7 C -0.0545(13) 0.2054(11) 0.0524(14) 0.053(6) Uani 1 d U . C8 C -0.1424(13) 0.1957(10) -0.0220(14) 0.050(5) Uani 1 d U . H8 H -0.1366(13) 0.1879(10) -0.0799(14) 0.060 Uiso 1 calc R . C9 C -0.2400(14) 0.1977(11) -0.0081(15) 0.061(7) Uani 1 d U . H9 H -0.2978(14) 0.1919(11) -0.0569(15) 0.073 Uiso 1 calc R . C10 C -0.2474(15) 0.2082(11) 0.0764(15) 0.066(7) Uani 1 d U . H10 H -0.3102(15) 0.2084(11) 0.0868(15) 0.079 Uiso 1 calc R . C11 C -0.1647(15) 0.2180(14) 0.1442(15) 0.088(10) Uani 1 d U . H11 H -0.1703(15) 0.2234(14) 0.2027(15) 0.106 Uiso 1 calc R . C12 C -0.0729(15) 0.2205(13) 0.1321(15) 0.075(8) Uani 1 d U . H12 H -0.0189(15) 0.2333(13) 0.1809(15) 0.090 Uiso 1 calc R . C13 C 0.0294(13) 0.0913(10) -0.1037(13) 0.041(6) Uani 1 d . . C14 C -0.0281(12) 0.1285(10) -0.1709(13) 0.040(5) Uani 1 d . . H14 H -0.0294(12) 0.1719(10) -0.1593(13) 0.048 Uiso 1 calc R . C15 C -0.0865(14) 0.1065(13) -0.2572(13) 0.062(7) Uani 1 d . . H15 H -0.1232(14) 0.1340(13) -0.3023(13) 0.074 Uiso 1 calc R . C16 C -0.0852(18) 0.0414(14) -0.2701(19) 0.083(10) Uani 1 d . . H16 H -0.1259(18) 0.0253(14) -0.3250(19) 0.099 Uiso 1 calc R . C17 C -0.0261(17) -0.0034(14) -0.2054(15) 0.072(8) Uani 1 d . . H17 H -0.0255(17) -0.0470(14) -0.2157(15) 0.086 Uiso 1 calc R . C18 C 0.0284(14) 0.0253(12) -0.1283(14) 0.050(6) Uani 1 d . . C19 C 0.0901(13) -0.0188(10) -0.0637(13) 0.050(6) Uani 1 d . . H19A H 0.1121(13) -0.0531(10) -0.0956(13) 0.060 Uiso 1 calc R . H19B H 0.0515(13) -0.0370(10) -0.0264(13) 0.060 Uiso 1 calc R . C20 C 0.2313(15) -0.0180(10) 0.0816(12) 0.059(6) Uani 1 d . . H20A H 0.1796(16) -0.0377(51) 0.1025(51) 0.088 Uiso 1 calc R . H20B H 0.2705(78) 0.0101(14) 0.1279(30) 0.088 Uiso 1 calc R . H20C H 0.2742(77) -0.0504(40) 0.0689(24) 0.088 Uiso 1 calc R . C21 C 0.2526(12) 0.0213(9) -0.0541(13) 0.046(6) Uani 1 d . . H21A H 0.2205(33) 0.0420(50) -0.1110(36) 0.069 Uiso 1 calc R . H21B H 0.2720(66) -0.0211(9) -0.0656(65) 0.069 Uiso 1 calc R . H21C H 0.3114(41) 0.0450(46) -0.0217(37) 0.069 Uiso 1 calc R . C22 C 0.3832(14) 0.1381(11) 0.2957(12) 0.036(5) Uani 1 d . . C23 C 0.3621(15) 0.0819(14) 0.3264(15) 0.070(8) Uani 1 d . . H23 H 0.3158(15) 0.0566(14) 0.2846(15) 0.084 Uiso 1 calc R . C24 C 0.4007(19) 0.0569(14) 0.4124(17) 0.085(9) Uani 1 d . . H24 H 0.3891(19) 0.0156(14) 0.4290(17) 0.102 Uiso 1 calc R . C25 C 0.4584(20) 0.1010(17) 0.4702(17) 0.095(12) Uani 1 d . . H25 H 0.4864(20) 0.0893(17) 0.5309(17) 0.114 Uiso 1 calc R . C26 C 0.4778(21) 0.1606(15) 0.4453(21) 0.097(10) Uani 1 d . . H26 H 0.5174(21) 0.1892(15) 0.4870(21) 0.116 Uiso 1 calc R . C27 C 0.4363(15) 0.1762(13) 0.3562(14) 0.065(8) Uani 1 d . . H27 H 0.4470(15) 0.2171(13) 0.3379(14) 0.078 Uiso 1 calc R . C28 C 0.4099(13) 0.1408(9) 0.1151(12) 0.039(5) Uani 1 d . . C29 C 0.4092(13) 0.1726(9) 0.0369(13) 0.039(5) Uani 1 d . . H29 H 0.3707(13) 0.2094(9) 0.0209(13) 0.047 Uiso 1 calc R . C30 C 0.4642(14) 0.1512(10) -0.0178(13) 0.045(6) Uani 1 d . . H30 H 0.4601(14) 0.1728(10) -0.0717(13) 0.054 Uiso 1 calc R . C31 C 0.5236(14) 0.1001(10) 0.0043(14) 0.048(6) Uani 1 d . . H31 H 0.5596(14) 0.0853(10) -0.0341(14) 0.058 Uiso 1 calc R . C32 C 0.5305(14) 0.0685(10) 0.0891(14) 0.055(6) Uani 1 d . . H32 H 0.5727(14) 0.0334(10) 0.1064(14) 0.066 Uiso 1 calc R . C33 C 0.4772(13) 0.0889(10) 0.1432(13) 0.048(6) Uani 1 d . . H33 H 0.4841(13) 0.0691(10) 0.1990(13) 0.058 Uiso 1 calc R . C34 C 0.4230(14) 0.3015(11) 0.2082(13) 0.052(6) Uani 1 d . . C35 C 0.5176(15) 0.2755(11) 0.2040(13) 0.059(7) Uani 1 d . . H35 H 0.5209(15) 0.2328(11) 0.1890(13) 0.071 Uiso 1 calc R . C36 C 0.6005(15) 0.3112(13) 0.2210(17) 0.066(7) Uani 1 d . . H36 H 0.6590(15) 0.2917(13) 0.2166(17) 0.079 Uiso 1 calc R . C37 C 0.6058(20) 0.3701(16) 0.2428(17) 0.082(9) Uani 1 d . . H37 H 0.6667(20) 0.3918(16) 0.2546(17) 0.098 Uiso 1 calc R . C38 C 0.5210(21) 0.4010(12) 0.2488(15) 0.086(9) Uani 1 d . . H38 H 0.5226(21) 0.4443(12) 0.2620(15) 0.103 Uiso 1 calc R . C39 C 0.4266(15) 0.3639(12) 0.2339(16) 0.062(7) Uani 1 d . . C40 C 0.3264(16) 0.3938(10) 0.2370(15) 0.061(7) Uani 1 d . . H40A H 0.3174(16) 0.3872(10) 0.2967(15) 0.073 Uiso 1 calc R . H40B H 0.3274(16) 0.4393(10) 0.2262(15) 0.073 Uiso 1 calc R . C41 C 0.2347(14) 0.3902(10) 0.0778(13) 0.054(6) Uani 1 d . . H41A H 0.3002(25) 0.3888(55) 0.0687(38) 0.081 Uiso 1 calc R . H41B H 0.2125(88) 0.4336(19) 0.0759(32) 0.081 Uiso 1 calc R . H41C H 0.1880(71) 0.3662(36) 0.0307(13) 0.081 Uiso 1 calc R . C42 C 0.1446(14) 0.3737(11) 0.1811(16) 0.071(8) Uani 1 d . . H42A H 0.1469(40) 0.3571(64) 0.2400(47) 0.106 Uiso 1 calc R . H42B H 0.0924(22) 0.3524(60) 0.1351(62) 0.106 Uiso 1 calc R . H42C H 0.1306(53) 0.4185(12) 0.1792(100) 0.106 Uiso 1 calc R . C43 C 0.7092(30) 0.1245(26) 0.3770(31) 0.234(31) Uani 1 d . . H43A H 0.6379(30) 0.1160(26) 0.3658(31) 0.280 Uiso 1 calc R . H43B H 0.7173(30) 0.1704(26) 0.3799(31) 0.280 Uiso 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 Pt1 0.0346(4) 0.0320(5) 0.0359(5) 0.0005(4) 0.0119(3) 0.0007(4) Pt2 0.0344(4) 0.0353(5) 0.0323(4) -0.0027(4) 0.0082(3) 0.0017(4) P1 0.030(3) 0.033(3) 0.030(3) 0.001(3) 0.009(2) 0.004(2) P2 0.038(3) 0.034(3) 0.028(3) 0.001(3) 0.010(2) 0.003(2) Cl1 0.228(15) 0.485(31) 0.143(12) 0.069(16) 0.006(11) -0.151(16) Cl2 0.341(21) 0.279(22) 0.198(15) 0.001(14) 0.030(14) -0.085(16) N1 0.040(9) 0.031(10) 0.044(10) 0.015(9) 0.016(8) 0.009(8) N2 0.061(11) 0.031(10) 0.039(11) -0.002(9) 0.010(9) 0.019(9) O1 0.025(6) 0.035(8) 0.040(8) -0.003(7) -0.002(6) 0.012(6) O2 0.032(7) 0.064(10) 0.040(8) -0.002(8) 0.016(6) 0.009(7) C1 0.045(12) 0.052(14) 0.025(11) 0.001(11) 0.004(9) -0.013(11) C2 0.048(14) 0.049(16) 0.092(20) -0.001(15) -0.021(13) 0.029(13) C3 0.037(13) 0.060(17) 0.077(18) 0.034(15) -0.006(12) 0.012(12) C4 0.047(15) 0.116(25) 0.052(16) 0.050(16) -0.020(12) -0.016(15) C5 0.046(9) 0.059(11) 0.046(9) 0.034(8) 0.020(7) 0.016(8) C6 0.045(9) 0.057(12) 0.046(9) 0.035(8) 0.021(7) 0.015(8) C7 0.021(8) 0.075(17) 0.061(11) -0.011(13) 0.009(9) -0.018(11) C8 0.047(9) 0.047(14) 0.066(10) -0.023(13) 0.030(9) -0.016(11) C9 0.030(8) 0.079(19) 0.066(10) -0.037(14) 0.002(11) -0.018(12) C10 0.041(9) 0.084(19) 0.070(11) -0.021(16) 0.011(11) 0.005(13) C11 0.037(10) 0.171(30) 0.055(11) -0.044(18) 0.010(10) -0.014(16) C12 0.038(9) 0.142(27) 0.055(10) 0.006(17) 0.029(10) 0.009(14) C13 0.023(10) 0.057(16) 0.036(12) -0.024(11) -0.003(9) -0.008(10) C14 0.023(10) 0.050(15) 0.045(13) -0.022(11) 0.008(9) -0.013(10) C15 0.043(13) 0.115(24) 0.025(12) -0.008(15) 0.006(10) 0.007(14) C16 0.080(19) 0.090(23) 0.094(22) -0.075(20) 0.049(17) -0.050(17) C17 0.065(17) 0.097(23) 0.041(15) -0.011(16) -0.006(12) -0.014(16) C18 0.044(13) 0.066(18) 0.037(13) 0.009(13) 0.008(10) -0.013(12) C19 0.044(13) 0.043(15) 0.060(15) -0.018(13) 0.010(11) -0.011(11) C20 0.088(17) 0.039(15) 0.044(13) -0.004(12) 0.013(12) -0.010(13) C21 0.042(12) 0.027(12) 0.071(15) 0.004(11) 0.021(11) 0.029(10) C22 0.033(11) 0.057(15) 0.021(11) -0.002(11) 0.012(9) -0.007(11) C23 0.042(14) 0.124(26) 0.043(15) 0.027(16) 0.009(11) 0.015(15) C24 0.111(24) 0.083(24) 0.059(19) 0.000(18) 0.024(17) 0.015(18) C25 0.086(22) 0.165(36) 0.039(16) 0.022(21) 0.028(15) 0.091(23) C26 0.116(25) 0.065(22) 0.105(28) -0.013(20) 0.024(21) -0.006(19) C27 0.056(15) 0.099(23) 0.027(13) 0.032(15) -0.008(12) 0.009(15) C28 0.038(11) 0.030(12) 0.041(12) 0.008(10) -0.002(9) 0.000(10) C29 0.056(13) 0.023(12) 0.051(13) -0.001(11) 0.035(11) -0.013(10) C30 0.056(14) 0.042(15) 0.028(12) -0.010(11) -0.003(10) -0.029(11) C31 0.049(13) 0.048(16) 0.060(15) -0.006(12) 0.033(12) -0.003(11) C32 0.053(14) 0.047(16) 0.062(16) 0.012(13) 0.015(12) 0.005(11) C33 0.049(13) 0.060(16) 0.046(13) 0.015(12) 0.029(11) 0.026(11) C34 0.040(13) 0.069(18) 0.038(13) -0.023(12) -0.001(10) -0.028(12) C35 0.040(13) 0.067(18) 0.054(14) -0.017(13) -0.012(11) 0.012(13) C36 0.025(13) 0.074(20) 0.084(19) 0.001(17) -0.007(12) -0.015(13) C37 0.076(20) 0.107(28) 0.060(17) -0.037(18) 0.016(15) 0.006(19) C38 0.146(26) 0.041(18) 0.046(15) -0.004(13) -0.009(17) -0.054(18) C39 0.047(14) 0.055(17) 0.085(18) -0.013(15) 0.022(13) -0.037(13) C40 0.080(17) 0.039(15) 0.067(16) -0.012(13) 0.027(14) 0.021(13) C41 0.059(14) 0.051(15) 0.040(13) 0.000(13) -0.003(11) 0.012(12) C42 0.052(14) 0.064(19) 0.104(20) -0.011(16) 0.035(14) 0.011(13) C43 0.158(40) 0.356(82) 0.189(48) 0.194(57) 0.054(37) 0.062(41) _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 Pt1 C13 2.00(2) . ? Pt1 O1 2.116(11) . ? Pt1 N1 2.160(15) . ? Pt1 P1 2.205(5) . ? Pt2 C34 2.01(2) . ? Pt2 O2 2.098(11) . ? Pt2 N2 2.15(2) . ? Pt2 P2 2.217(5) . ? P1 O2 1.531(13) . ? P1 C7 1.78(2) . ? P1 C1 1.89(2) . ? P2 O1 1.556(12) . ? P2 C22 1.80(2) . ? P2 C28 1.82(2) . ? Cl1 C43 1.45(5) . ? Cl2 C43 1.67(4) . ? N1 C21 1.41(2) . ? N1 C20 1.46(2) . ? N1 C19 1.58(2) . ? N2 C41 1.43(2) . ? N2 C42 1.44(2) . ? N2 C40 1.52(2) . ? C1 C6 1.39(2) . ? C1 C2 1.39(3) . ? C2 C3 1.44(3) . ? C3 C4 1.42(3) . ? C4 C5 1.38(3) . ? C5 C6 1.38(2) . ? C7 C12 1.36(3) . ? C7 C8 1.42(2) . ? C8 C9 1.43(2) . ? C9 C10 1.35(3) . ? C10 C11 1.32(2) . ? C11 C12 1.34(2) . ? C13 C14 1.35(3) . ? C13 C18 1.43(3) . ? C14 C15 1.41(2) . ? C15 C16 1.38(3) . ? C16 C17 1.44(3) . ? C17 C18 1.34(3) . ? C18 C19 1.44(3) . ? C22 C27 1.28(3) . ? C22 C23 1.33(3) . ? C23 C24 1.37(3) . ? C24 C25 1.37(4) . ? C25 C26 1.36(4) . ? C26 C27 1.36(3) . ? C28 C29 1.37(2) . ? C28 C33 1.42(2) . ? C29 C30 1.37(2) . ? C30 C31 1.34(3) . ? C31 C32 1.44(3) . ? C32 C33 1.34(2) . ? C34 C39 1.36(3) . ? C34 C35 1.44(3) . ? C35 C36 1.33(3) . ? C36 C37 1.28(3) . ? C37 C38 1.37(3) . ? C38 C39 1.48(3) . ? C39 C40 1.54(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 C13 Pt1 O1 170.4(7) . . ? C13 Pt1 N1 82.1(7) . . ? O1 Pt1 N1 88.9(5) . . ? C13 Pt1 P1 98.9(6) . . ? O1 Pt1 P1 90.1(3) . . ? N1 Pt1 P1 179.0(4) . . ? C34 Pt2 O2 171.3(8) . . ? C34 Pt2 N2 82.6(8) . . ? O2 Pt2 N2 88.8(6) . . ? C34 Pt2 P2 98.7(7) . . ? O2 Pt2 P2 89.9(4) . . ? N2 Pt2 P2 176.2(4) . . ? O2 P1 C7 101.9(8) . . ? O2 P1 C1 103.9(8) . . ? C7 P1 C1 108.4(10) . . ? O2 P1 Pt1 115.4(5) . . ? C7 P1 Pt1 114.5(8) . . ? C1 P1 Pt1 111.7(7) . . ? O1 P2 C22 102.6(8) . . ? O1 P2 C28 106.4(8) . . ? C22 P2 C28 106.4(8) . . ? O1 P2 Pt2 115.5(5) . . ? C22 P2 Pt2 112.4(7) . . ? C28 P2 Pt2 112.6(7) . . ? C21 N1 C20 109.0(15) . . ? C21 N1 C19 104.4(15) . . ? C20 N1 C19 110.3(15) . . ? C21 N1 Pt1 112.3(11) . . ? C20 N1 Pt1 115.9(12) . . ? C19 N1 Pt1 104.2(10) . . ? C41 N2 C42 107.9(16) . . ? C41 N2 C40 109.2(16) . . ? C42 N2 C40 112.1(16) . . ? C41 N2 Pt2 110.1(12) . . ? C42 N2 Pt2 113.9(13) . . ? C40 N2 Pt2 103.6(11) . . ? P2 O1 Pt1 126.1(7) . . ? P1 O2 Pt2 128.6(7) . . ? C6 C1 C2 123.5(20) . . ? C6 C1 P1 113.8(15) . . ? C2 C1 P1 122.3(17) . . ? C1 C2 C3 116.5(22) . . ? C4 C3 C2 117.6(21) . . ? C5 C4 C3 124.2(22) . . ? C6 C5 C4 117.4(19) . . ? C5 C6 C1 120.7(19) . . ? C12 C7 C8 114.4(17) . . ? C12 C7 P1 122.5(16) . . ? C8 C7 P1 122.8(16) . . ? C7 C8 C9 120.2(19) . . ? C10 C9 C8 119.4(19) . . ? C11 C10 C9 119.3(21) . . ? C10 C11 C12 122.6(23) . . ? C11 C12 C7 123.6(22) . . ? C14 C13 C18 113.5(17) . . ? C14 C13 Pt1 132.8(16) . . ? C18 C13 Pt1 113.4(15) . . ? C13 C14 C15 125.1(21) . . ? C16 C15 C14 115.4(23) . . ? C15 C16 C17 125.2(24) . . ? C18 C17 C16 112.0(25) . . ? C17 C18 C13 128.5(22) . . ? C17 C18 C19 112.7(23) . . ? C13 C18 C19 118.7(19) . . ? C18 C19 N1 108.8(17) . . ? C27 C22 C23 115.8(20) . . ? C27 C22 P2 122.9(18) . . ? C23 C22 P2 120.7(17) . . ? C22 C23 C24 127.8(26) . . ? C25 C24 C23 110.7(28) . . ? C26 C25 C24 124.6(27) . . ? C25 C26 C27 116.4(29) . . ? C22 C27 C26 124.2(26) . . ? C29 C28 C33 118.4(18) . . ? C29 C28 P2 121.4(14) . . ? C33 C28 P2 120.2(14) . . ? C30 C29 C28 121.1(19) . . ? C31 C30 C29 121.5(20) . . ? C30 C31 C32 118.2(19) . . ? C33 C32 C31 120.9(20) . . ? C32 C33 C28 119.5(19) . . ? C39 C34 C35 114.9(18) . . ? C39 C34 Pt2 114.1(16) . . ? C35 C34 Pt2 130.6(17) . . ? C36 C35 C34 121.6(22) . . ? C37 C36 C35 125.1(27) . . ? C36 C37 C38 119.5(29) . . ? C37 C38 C39 118.5(25) . . ? C34 C39 C38 120.3(22) . . ? C34 C39 C40 116.4(18) . . ? C38 C39 C40 123.1(23) . . ? N2 C40 C39 109.3(17) . . ? Cl1 C43 Cl2 120.8(32) . . ? _refine_diff_density_max 0.982 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.239