# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2050 data_1 #----------------------------------------------------------------------- _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 15.577(1) _cell_length_b 12.190(3) _cell_length_c 8.139(1) _cell_angle_alpha 90 _cell_angle_beta 105.156(8) _cell_angle_gamma 90 _cell_volume 1491.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 30.8 _cell_measurement_theta_max 35.4 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ; _exptl_crystal_description 'block' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 278.29 _chemical_formula_analytical 'C17 H15 N2 P ' _chemical_formula_sum 'C17 H15 N2 P ' _chemical_formula_moiety 'C17 H15 N2 P ' _chemical_formula_structural 'C17 H15 N2 P ' _chemical_compound_source - _exptl_crystal_F_000 584.00 _exptl_absorpt_coefficient_mu 1.541 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.772 _exptl_special_details ; The scan width was (0.79+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.79 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -5 1 3 -5 -3 2 -5 -4 2 _diffrn_reflns_number 2449 _reflns_number_total 2357 _reflns_number_gt 1429 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.17051 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 60.08 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05152 _diffrn_orient_matrix_UB_12 -0.04364 _diffrn_orient_matrix_UB_13 0.01623 _diffrn_orient_matrix_UB_21 0.03830 _diffrn_orient_matrix_UB_22 -0.06701 _diffrn_orient_matrix_UB_23 0.02328 _diffrn_orient_matrix_UB_31 0.01739 _diffrn_orient_matrix_UB_32 0.01828 _diffrn_orient_matrix_UB_33 0.12409 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 68 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 60 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom P(1) 0.67792(6) -0.1510(1) 0.2688(1) 0.0662(3) 1.000 . Uani d ? N(1) 0.5076(2) 0.0910(3) 0.1878(4) 0.066(1) 1.000 . Uani d ? N(2) 0.5944(2) -0.0603(3) 0.1864(4) 0.068(1) 1.000 . Uani d ? C(2) 0.5697(2) 0.0238(4) 0.2767(5) 0.059(1) 1.000 . Uani d ? C(3) 0.6078(2) 0.0397(4) 0.4530(5) 0.074(1) 1.000 . Uani d ? C(4) 0.5799(3) 0.1258(4) 0.5309(5) 0.083(2) 1.000 . Uani d ? C(5) 0.5165(2) 0.1968(4) 0.4403(5) 0.077(1) 1.000 . Uani d ? C(6) 0.4827(2) 0.1748(4) 0.2701(5) 0.077(1) 1.000 . Uani d ? C(7) 0.6202(2) -0.2796(4) 0.2771(5) 0.067(1) 1.000 . Uani d ? C(8) 0.5388(3) -0.3086(4) 0.1682(5) 0.081(2) 1.000 . Uani d ? C(9) 0.4994(3) -0.4062(5) 0.1854(7) 0.100(2) 1.000 . Uani d ? C(10) 0.5366(4) -0.4784(5) 0.3092(7) 0.103(2) 1.000 . Uani d ? C(11) 0.6170(4) -0.4525(5) 0.4239(7) 0.100(2) 1.000 . Uani d ? C(12) 0.6577(3) -0.3545(4) 0.4078(5) 0.085(2) 1.000 . Uani d ? C(13) 0.7202(2) -0.1721(4) 0.0814(5) 0.063(1) 1.000 . Uani d ? C(14) 0.7467(3) -0.2710(5) 0.0383(6) 0.098(2) 1.000 . Uani d ? C(15) 0.7873(4) -0.2816(5) -0.0962(7) 0.122(3) 1.000 . Uani d ? C(16) 0.7996(3) -0.1933(5) -0.1855(6) 0.097(2) 1.000 . Uani d ? C(17) 0.7726(3) -0.0950(5) -0.1477(7) 0.099(2) 1.000 . Uani d ? C(18) 0.7329(3) -0.0836(4) -0.0140(7) 0.090(2) 1.000 . Uani d ? H(2n) 0.5633 -0.0519 0.0532 0.085 1.000 . Uiso c ? H(3) 0.6520 -0.0090 0.5155 0.089 1.000 . Uiso c ? H(4) 0.6046 0.1373 0.6493 0.100 1.000 . Uiso c ? H(5) 0.4970 0.2581 0.4929 0.092 1.000 . Uiso c ? H(6) 0.4383 0.2229 0.2064 0.092 1.000 . Uiso c ? H(8) 0.5102 -0.2595 0.0802 0.097 1.000 . Uiso c ? H(9) 0.4440 -0.4238 0.1080 0.120 1.000 . Uiso c ? H(10) 0.5081 -0.5462 0.3179 0.123 1.000 . Uiso c ? H(11) 0.6437 -0.5020 0.5127 0.120 1.000 . Uiso c ? H(12) 0.7125 -0.3369 0.4868 0.102 1.000 . Uiso c ? H(14) 0.7380 -0.3344 0.0999 0.117 1.000 . Uiso c ? H(15) 0.8060 -0.3518 -0.1241 0.147 1.000 . Uiso c ? H(16) 0.8275 -0.2007 -0.2755 0.117 1.000 . Uiso c ? H(17) 0.7803 -0.0326 -0.2123 0.119 1.000 . Uiso c ? H(18) 0.7142 -0.0130 0.0120 0.108 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P(1) 0.0280(5) 0.1109(9) 0.0551(6) 0.0105(6) 0.0026(4) -0.0007(7) N(1) 0.037(2) 0.109(3) 0.050(2) 0.016(2) 0.007(1) -0.004(2) N(2) 0.036(2) 0.109(3) 0.053(2) 0.017(2) 0.001(1) -0.004(2) C(2) 0.021(2) 0.099(3) 0.058(2) -0.005(2) 0.011(2) -0.002(2) C(3) 0.033(2) 0.133(4) 0.052(2) 0.008(2) 0.000(2) -0.011(3) C(4) 0.048(2) 0.142(5) 0.056(3) -0.002(3) 0.009(2) -0.019(3) C(5) 0.049(2) 0.115(4) 0.071(3) 0.000(2) 0.023(2) -0.013(3) C(6) 0.044(2) 0.115(4) 0.069(3) 0.013(2) 0.012(2) 0.000(3) C(7) 0.043(2) 0.107(3) 0.055(2) 0.013(2) 0.021(2) 0.005(2) C(8) 0.056(3) 0.126(4) 0.059(3) -0.011(3) 0.010(2) 0.006(3) C(9) 0.073(3) 0.138(5) 0.089(4) -0.019(4) 0.024(3) 0.003(4) C(10) 0.099(4) 0.116(4) 0.116(5) -0.003(4) 0.068(4) 0.003(4) C(11) 0.094(4) 0.119(5) 0.107(4) 0.033(4) 0.061(4) 0.036(4) C(12) 0.053(3) 0.134(4) 0.072(3) 0.029(3) 0.025(2) 0.017(3) C(13) 0.027(2) 0.101(3) 0.062(2) 0.007(2) 0.013(2) -0.001(2) C(14) 0.097(4) 0.112(4) 0.103(4) 0.028(3) 0.059(3) 0.019(3) C(15) 0.141(5) 0.130(5) 0.130(5) 0.024(4) 0.095(4) 0.006(4) C(16) 0.066(3) 0.151(5) 0.086(3) 0.002(3) 0.039(3) 0.006(4) C(17) 0.064(3) 0.139(5) 0.103(4) 0.005(3) 0.040(3) 0.020(4) C(18) 0.068(3) 0.105(4) 0.110(4) 0.007(3) 0.047(3) 0.009(3) #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.0000136(2) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1429 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_all 0.0394 _refine_ls_wR_factor_ref 0.0394 _refine_ls_goodness_of_fit_all 2.645 _refine_ls_goodness_of_fit_ref 2.645 _refine_ls_shift/esd_max 0.0180 _refine_ls_shift/esd_mean 0.0160 _refine_diff_density_min -0.23 _refine_diff_density_max 0.18 #----------------------------------------------------------------------- _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P(1) N(2) 1.705(3) . . yes P(1) C(7) 1.817(4) . . yes P(1) C(13) 1.831(4) . . yes N(1) C(2) 1.329(4) . . yes N(1) C(6) 1.334(5) . . yes N(2) C(2) 1.374(5) . . yes N(2) H(2n) 1.07 . . no C(2) C(3) 1.415(5) . . yes C(3) C(4) 1.355(6) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.374(5) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.373(5) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.389(5) . . yes C(7) C(12) 1.408(5) . . yes C(8) C(9) 1.362(6) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.349(7) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.389(7) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.374(7) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) C(14) 1.350(6) . . yes C(13) C(18) 1.373(6) . . yes C(14) C(15) 1.405(6) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.340(7) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.332(7) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.393(6) . . yes C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(2) P(1) C(7) 103.9(2) . . . yes N(2) P(1) C(13) 99.6(2) . . . yes C(7) P(1) C(13) 101.5(2) . . . yes C(2) N(1) C(6) 117.7(3) . . . yes P(1) N(2) C(2) 124.4(2) . . . yes P(1) N(2) H(2n) 123.9 . . . no C(2) N(2) H(2n) 110.8 . . . no N(1) C(2) N(2) 115.7(3) . . . yes N(1) C(2) C(3) 121.4(4) . . . yes N(2) C(2) C(3) 122.9(4) . . . yes C(2) C(3) C(4) 118.7(4) . . . yes C(2) C(3) H(3) 120.7 . . . no C(4) C(3) H(3) 120.7 . . . no C(3) C(4) C(5) 120.7(4) . . . yes C(3) C(4) H(4) 119.6 . . . no C(5) C(4) H(4) 119.7 . . . no C(4) C(5) C(6) 116.8(4) . . . yes C(4) C(5) H(5) 121.6 . . . no C(6) C(5) H(5) 121.6 . . . no N(1) C(6) C(5) 124.8(4) . . . yes N(1) C(6) H(6) 117.6 . . . no C(5) C(6) H(6) 117.6 . . . no P(1) C(7) C(8) 125.0(4) . . . yes P(1) C(7) C(12) 118.4(3) . . . yes C(8) C(7) C(12) 116.5(4) . . . yes C(7) C(8) C(9) 121.2(5) . . . yes C(7) C(8) H(8) 119.4 . . . no C(9) C(8) H(8) 119.4 . . . no C(8) C(9) C(10) 121.9(5) . . . yes C(8) C(9) H(9) 119.0 . . . no C(10) C(9) H(9) 119.0 . . . no C(9) C(10) C(11) 119.3(5) . . . yes C(9) C(10) H(10) 120.4 . . . no C(11) C(10) H(10) 120.3 . . . no C(10) C(11) C(12) 119.4(5) . . . yes C(10) C(11) H(11) 120.3 . . . no C(12) C(11) H(11) 120.3 . . . no C(7) C(12) C(11) 121.7(5) . . . yes C(7) C(12) H(12) 119.2 . . . no C(11) C(12) H(12) 119.1 . . . no P(1) C(13) C(14) 122.9(4) . . . yes P(1) C(13) C(18) 119.8(4) . . . yes C(14) C(13) C(18) 117.1(4) . . . yes C(13) C(14) C(15) 121.0(5) . . . yes C(13) C(14) H(14) 119.5 . . . no C(15) C(14) H(14) 119.5 . . . no C(14) C(15) C(16) 120.4(5) . . . yes C(14) C(15) H(15) 119.8 . . . no C(16) C(15) H(15) 119.8 . . . no C(15) C(16) C(17) 119.9(5) . . . yes C(15) C(16) H(16) 120.0 . . . no C(17) C(16) H(16) 120.0 . . . no C(16) C(17) C(18) 120.1(5) . . . yes C(16) C(17) H(17) 120.0 . . . no C(18) C(17) H(17) 120.0 . . . no C(13) C(18) C(17) 121.5(5) . . . yes C(13) C(18) H(18) 119.2 . . . no C(17) C(18) H(18) 119.2 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(1) N(2) 3.067(4) . 3_655 no C(3) C(4) 3.583(6) . 3_656 no #----------------------------------------------------------------------- loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(2)' 'H(2n)' 'N(1)' '1.07' '2.04' '2.289(4)' '160.0' '3_655' #---END data_5 #----------------------------------------------------------------------- _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 11.994(4) _cell_length_b 15.236(3) _cell_length_c 9.839(3) _cell_angle_alpha 94.12(2) _cell_angle_beta 113.79(2) _cell_angle_gamma 90.39(2) _cell_volume 1639.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 34.2 _cell_measurement_theta_max 37.4 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 831.59 _chemical_formula_analytical 'C34 H31 Cl2 N4 O0.50 P2 Pt ' _chemical_formula_sum 'C34 H31 Cl2 N4 O0.50 P2 Pt ' _chemical_formula_moiety 'C34 H30 Cl2 N4 P2 Pt(H2 O)0.5 ' _chemical_formula_structural 'C34 H31 Cl2 N4 O0.50 P2 Pt ' _chemical_compound_source - _exptl_crystal_F_000 818.00 _exptl_absorpt_coefficient_mu 10.376 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.902 _exptl_special_details ; The scan width was (1.26+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.10 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 3 3 -1 -3 4 -2 6 2 _diffrn_reflns_number 5151 _reflns_number_total 4878 _reflns_number_gt 3943 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.24970 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 60.20 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05111 _diffrn_orient_matrix_UB_12 0.02242 _diffrn_orient_matrix_UB_13 0.05303 _diffrn_orient_matrix_UB_21 -0.01470 _diffrn_orient_matrix_UB_22 -0.06158 _diffrn_orient_matrix_UB_23 0.01961 _diffrn_orient_matrix_UB_31 0.07407 _diffrn_orient_matrix_UB_32 0.00642 _diffrn_orient_matrix_UB_33 0.09604 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 68 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 62 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 2 -5.233 6.925 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 1 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.12552(3) 0.23662(2) 0.21939(4) 0.02684(9) 1.000 . Uani d ? Cl(1) 0.1978(2) 0.2162(2) 0.4743(2) 0.0453(6) 1.000 . Uani d ? Cl(2) 0.6825(2) 0.2646(2) 0.6342(3) 0.0616(8) 1.000 . Uani d ? P(1) 0.0379(2) 0.2442(1) -0.0255(2) 0.0296(6) 1.000 . Uani d ? P(21) 0.3213(2) 0.2294(1) 0.2488(2) 0.0281(6) 1.000 . Uani d ? O(1) 0.292(2) -0.033(1) 0.035(2) 0.127(8) 0.500 . Uani d ? N(1) -0.0546(5) 0.2498(4) 0.2017(7) 0.024(2) 1.000 . Uani d ? N(2) -0.1074(6) 0.2632(5) -0.0504(7) 0.037(2) 1.000 . Uani d ? N(21) 0.2745(7) 0.4097(5) 0.3392(9) 0.051(3) 1.000 . Uani d ? N(22) 0.4126(6) 0.2988(4) 0.3929(7) 0.037(2) 1.000 . Uani d ? C(2) -0.1422(7) 0.2583(5) 0.065(1) 0.038(3) 1.000 . Uani d ? C(3) -0.2655(8) 0.2649(7) 0.042(1) 0.051(3) 1.000 . Uani d ? C(4) -0.2958(8) 0.2618(7) 0.161(1) 0.054(3) 1.000 . Uani d ? C(5) -0.2078(9) 0.2540(7) 0.300(1) 0.052(3) 1.000 . Uani d ? C(6) -0.0912(8) 0.2471(6) 0.314(1) 0.044(3) 1.000 . Uani d ? C(7) 0.0262(8) 0.1433(5) -0.1393(9) 0.036(2) 1.000 . Uani d ? C(8) -0.0559(9) 0.1359(7) -0.289(1) 0.052(3) 1.000 . Uani d ? C(9) -0.0685(9) 0.0555(8) -0.375(1) 0.059(3) 1.000 . Uani d ? C(10) -0.001(1) -0.0137(7) -0.311(1) 0.064(4) 1.000 . Uani d ? C(11) 0.077(1) -0.0067(6) -0.165(1) 0.065(4) 1.000 . Uani d ? C(12) 0.0900(9) 0.0712(6) -0.078(1) 0.051(3) 1.000 . Uani d ? C(13) 0.0761(7) 0.3347(5) -0.1115(9) 0.032(2) 1.000 . Uani d ? C(14) 0.0915(9) 0.3259(6) -0.241(1) 0.048(3) 1.000 . Uani d ? C(15) 0.117(1) 0.4001(8) -0.301(1) 0.066(4) 1.000 . Uani d ? C(16) 0.128(1) 0.4801(7) -0.229(1) 0.069(4) 1.000 . Uani d ? C(17) 0.122(1) 0.4893(6) -0.094(1) 0.062(4) 1.000 . Uani d ? C(18) 0.0949(9) 0.4165(6) -0.034(1) 0.048(3) 1.000 . Uani d ? C(22) 0.3755(8) 0.3771(6) 0.4366(9) 0.036(2) 1.000 . Uani d ? C(23) 0.4421(8) 0.4196(7) 0.578(1) 0.046(3) 1.000 . Uani d ? C(24) 0.399(1) 0.4953(7) 0.615(1) 0.059(4) 1.000 . Uani d ? C(25) 0.293(1) 0.5289(7) 0.518(1) 0.066(4) 1.000 . Uani d ? C(26) 0.236(1) 0.4836(7) 0.381(1) 0.067(4) 1.000 . Uani d ? C(27) 0.3536(7) 0.2549(6) 0.0909(9) 0.035(2) 1.000 . Uani d ? C(28) 0.3807(8) 0.3405(6) 0.073(1) 0.041(3) 1.000 . Uani d ? C(29) 0.4043(9) 0.3587(7) -0.049(1) 0.060(3) 1.000 . Uani d ? C(30) 0.401(1) 0.2922(8) -0.152(1) 0.063(4) 1.000 . Uani d ? C(31) 0.374(1) 0.2071(7) -0.136(1) 0.058(3) 1.000 . Uani d ? C(32) 0.3517(8) 0.1881(6) -0.015(1) 0.045(3) 1.000 . Uani d ? C(33) 0.3849(7) 0.1231(5) 0.2896(8) 0.033(2) 1.000 . Uani d ? C(34) 0.5041(8) 0.1080(6) 0.304(1) 0.047(3) 1.000 . Uani d ? C(35) 0.5473(9) 0.0250(7) 0.320(1) 0.058(3) 1.000 . Uani d ? C(36) 0.472(1) -0.0459(7) 0.322(1) 0.062(4) 1.000 . Uani d ? C(37) 0.3576(9) -0.0323(6) 0.306(1) 0.048(3) 1.000 . Uani d ? C(38) 0.3131(8) 0.0511(6) 0.293(1) 0.042(3) 1.000 . Uani d ? H(2) -0.1650 0.2610 -0.1534 0.050 1.000 . Uiso c ? H(3) -0.3265 0.2714 -0.0549 0.061 1.000 . Uiso c ? H(4) -0.3787 0.2651 0.1473 0.065 1.000 . Uiso c ? H(5) -0.2276 0.2535 0.3838 0.063 1.000 . Uiso c ? H(6) -0.0307 0.2398 0.4107 0.052 1.000 . Uiso c ? H(8) -0.1028 0.1845 -0.3320 0.063 1.000 . Uiso c ? H(9) -0.1240 0.0495 -0.4765 0.070 1.000 . Uiso c ? H(10) -0.0077 -0.0674 -0.3701 0.076 1.000 . Uiso c ? H(11) 0.1223 -0.0558 -0.1225 0.077 1.000 . Uiso c ? H(12) 0.1432 0.0748 0.0248 0.061 1.000 . Uiso c ? H(14) 0.0850 0.2693 -0.2918 0.058 1.000 . Uiso c ? H(15) 0.1256 0.3940 -0.3925 0.079 1.000 . Uiso c ? H(16) 0.1412 0.5307 -0.2725 0.082 1.000 . Uiso c ? H(17) 0.1369 0.5456 -0.0410 0.075 1.000 . Uiso c ? H(18) 0.0891 0.4231 0.0599 0.057 1.000 . Uiso c ? H(22) 0.4917 0.2827 0.4417 0.050 1.000 . Uiso c ? H(23) 0.5150 0.3963 0.6455 0.056 1.000 . Uiso c ? H(24) 0.4422 0.5257 0.7100 0.071 1.000 . Uiso c ? H(25) 0.2607 0.5809 0.5444 0.079 1.000 . Uiso c ? H(26) 0.1644 0.5070 0.3113 0.080 1.000 . Uiso c ? H(28) 0.3833 0.3867 0.1445 0.049 1.000 . Uiso c ? H(29) 0.4226 0.4176 -0.0613 0.072 1.000 . Uiso c ? H(30) 0.4173 0.3052 -0.2354 0.076 1.000 . Uiso c ? H(31) 0.3711 0.1614 -0.2084 0.069 1.000 . Uiso c ? H(32) 0.3347 0.1289 -0.0035 0.054 1.000 . Uiso c ? H(34) 0.5549 0.1556 0.3018 0.057 1.000 . Uiso c ? H(35) 0.6283 0.0152 0.3305 0.069 1.000 . Uiso c ? H(36) 0.5032 -0.1034 0.3346 0.074 1.000 . Uiso c ? H(37) 0.3064 -0.0808 0.3030 0.058 1.000 . Uiso c ? H(38) 0.2327 0.0599 0.2861 0.050 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0221(2) 0.0328(2) 0.0255(2) -0.0091(1) 0.0109(1) -0.0056(1) Cl(1) 0.040(1) 0.066(2) 0.028(1) -0.010(1) 0.014(1) 0.000(1) Cl(2) 0.045(1) 0.063(2) 0.055(2) -0.008(1) -0.002(1) 0.008(1) P(1) 0.024(1) 0.037(1) 0.027(1) -0.0090(9) 0.0111(9) -0.0043(9) P(21) 0.025(1) 0.031(1) 0.027(1) -0.0074(9) 0.0093(9) -0.0009(9) O(1) 0.09(1) 0.22(2) 0.06(1) -0.10(1) 0.02(1) 0.02(1) N(1) 0.025(4) 0.021(3) 0.024(3) -0.001(3) 0.008(3) -0.008(3) N(2) 0.028(4) 0.052(5) 0.029(4) -0.006(3) 0.011(3) -0.002(3) N(21) 0.055(5) 0.041(5) 0.049(5) 0.001(4) 0.016(4) -0.011(4) N(22) 0.029(4) 0.040(4) 0.034(4) -0.013(3) 0.007(3) -0.007(3) C(2) 0.025(4) 0.030(5) 0.057(6) -0.010(4) 0.017(4) -0.006(4) C(3) 0.032(5) 0.065(7) 0.057(6) -0.002(5) 0.020(5) 0.006(5) C(4) 0.028(5) 0.079(8) 0.065(7) -0.001(5) 0.028(5) 0.006(6) C(5) 0.048(6) 0.056(7) 0.070(7) 0.005(5) 0.040(6) 0.015(5) C(6) 0.038(5) 0.048(6) 0.050(6) -0.005(4) 0.025(5) 0.002(5) C(7) 0.036(5) 0.036(5) 0.034(5) -0.018(4) 0.016(4) -0.011(4) C(8) 0.052(6) 0.066(7) 0.040(5) -0.023(5) 0.023(5) -0.012(5) C(9) 0.052(6) 0.077(8) 0.045(6) -0.026(6) 0.023(5) -0.023(6) C(10) 0.074(8) 0.053(7) 0.066(8) -0.026(6) 0.034(6) -0.022(6) C(11) 0.074(8) 0.038(6) 0.082(8) -0.014(6) 0.034(7) -0.005(6) C(12) 0.051(6) 0.049(6) 0.052(6) -0.014(5) 0.021(5) -0.010(5) C(13) 0.026(4) 0.039(5) 0.034(5) -0.008(4) 0.016(4) 0.003(4) C(14) 0.054(6) 0.051(6) 0.044(5) -0.015(5) 0.026(5) -0.003(5) C(15) 0.090(9) 0.072(8) 0.055(7) -0.015(7) 0.049(7) 0.007(6) C(16) 0.085(9) 0.043(7) 0.11(1) -0.003(6) 0.065(8) 0.021(6) C(17) 0.072(8) 0.032(6) 0.099(9) -0.001(5) 0.051(7) 0.005(6) C(18) 0.056(6) 0.034(5) 0.063(6) -0.007(5) 0.035(5) -0.002(5) C(22) 0.034(5) 0.036(5) 0.038(5) -0.022(4) 0.015(4) -0.007(4) C(23) 0.047(6) 0.057(6) 0.038(5) -0.025(5) 0.022(4) -0.004(5) C(24) 0.078(8) 0.058(7) 0.045(6) -0.041(6) 0.035(6) -0.021(5) C(25) 0.10(1) 0.038(6) 0.076(8) -0.019(6) 0.055(8) -0.012(6) C(26) 0.064(7) 0.051(7) 0.075(8) 0.003(6) 0.018(6) 0.000(6) C(27) 0.026(4) 0.043(5) 0.037(5) -0.009(4) 0.017(4) -0.002(4) C(28) 0.033(5) 0.045(5) 0.044(5) -0.008(4) 0.015(4) 0.002(4) C(29) 0.044(6) 0.071(7) 0.064(7) -0.020(5) 0.018(5) 0.028(6) C(30) 0.056(7) 0.099(9) 0.043(6) -0.011(6) 0.028(5) 0.017(6) C(31) 0.064(7) 0.076(8) 0.036(6) 0.004(6) 0.024(5) 0.001(5) C(32) 0.040(5) 0.059(6) 0.037(5) -0.008(5) 0.017(4) -0.003(5) C(33) 0.036(5) 0.035(5) 0.028(4) -0.010(4) 0.014(4) -0.004(4) C(34) 0.038(5) 0.048(6) 0.064(7) 0.002(5) 0.028(5) 0.009(5) C(35) 0.039(6) 0.067(7) 0.073(7) 0.011(5) 0.029(5) 0.005(6) C(36) 0.088(9) 0.042(6) 0.063(7) 0.019(6) 0.039(7) 0.012(5) C(37) 0.056(6) 0.042(6) 0.050(6) -0.008(5) 0.025(5) 0.007(5) C(38) 0.042(5) 0.041(5) 0.046(5) -0.006(4) 0.022(4) 0.005(4) #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 3943 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all - _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_all - _refine_ls_wR_factor_ref 0.0403 _refine_ls_goodness_of_fit_all - _refine_ls_goodness_of_fit_ref 1.997 _refine_ls_shift/esd_max 0.0120 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -1.09 _refine_diff_density_max 1.68 #----------------------------------------------------------------------- _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) Cl(1) 2.345(2) . . yes Pt(1) P(1) 2.219(2) . . yes Pt(1) P(21) 2.252(2) . . yes Pt(1) N(1) 2.109(6) . . yes P(1) N(2) 1.689(7) . . yes P(1) C(7) 1.806(8) . . yes P(1) C(13) 1.816(8) . . yes P(21) N(22) 1.686(6) . . yes P(21) C(27) 1.811(8) . . yes P(21) C(33) 1.797(9) . . yes N(1) C(2) 1.35(1) . . yes N(1) C(6) 1.35(1) . . yes N(2) C(2) 1.36(1) . . yes N(2) H(2) 0.97 . . no N(21) C(22) 1.33(1) . . yes N(21) C(26) 1.32(1) . . yes N(22) C(22) 1.38(1) . . yes N(22) H(22) 0.92 . . no C(2) C(3) 1.41(1) . . yes C(3) C(4) 1.37(1) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.36(1) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.35(1) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.40(1) . . yes C(7) C(12) 1.38(1) . . yes C(8) C(9) 1.41(1) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.36(1) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.36(1) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.38(1) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) C(14) 1.36(1) . . yes C(13) C(18) 1.38(1) . . yes C(14) C(15) 1.39(1) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.34(1) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.35(2) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.39(1) . . yes C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(22) C(23) 1.40(1) . . yes C(23) C(24) 1.35(1) . . yes C(23) H(23) 0.95 . . no C(24) C(25) 1.37(2) . . yes C(24) H(24) 0.95 . . no C(25) C(26) 1.37(1) . . yes C(25) H(25) 0.95 . . no C(26) H(26) 0.95 . . no C(27) C(28) 1.38(1) . . yes C(27) C(32) 1.40(1) . . yes C(28) C(29) 1.39(1) . . yes C(28) H(28) 0.95 . . no C(29) C(30) 1.37(2) . . yes C(29) H(29) 0.95 . . no C(30) C(31) 1.37(1) . . yes C(30) H(30) 0.95 . . no C(31) C(32) 1.37(1) . . yes C(31) H(31) 0.95 . . no C(32) H(32) 0.95 . . no C(33) C(34) 1.40(1) . . yes C(33) C(38) 1.40(1) . . yes C(34) C(35) 1.37(1) . . yes C(34) H(34) 0.95 . . no C(35) C(36) 1.41(1) . . yes C(35) H(35) 0.95 . . no C(36) C(37) 1.34(1) . . yes C(36) H(36) 0.95 . . no C(37) C(38) 1.38(1) . . yes C(37) H(37) 0.95 . . no C(38) H(38) 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Pt(1) P(1) 172.79(7) . . . yes Cl(1) Pt(1) P(21) 86.20(8) . . . yes Cl(1) Pt(1) N(1) 92.0(2) . . . yes P(1) Pt(1) P(21) 99.18(8) . . . yes P(1) Pt(1) N(1) 82.9(2) . . . yes P(21) Pt(1) N(1) 176.5(2) . . . yes Pt(1) P(1) N(2) 101.0(2) . . . yes Pt(1) P(1) C(7) 116.5(3) . . . yes Pt(1) P(1) C(13) 120.7(3) . . . yes N(2) P(1) C(7) 104.2(4) . . . yes N(2) P(1) C(13) 102.9(4) . . . yes C(7) P(1) C(13) 108.8(4) . . . yes Pt(1) P(21) N(22) 111.1(3) . . . yes Pt(1) P(21) C(27) 116.5(3) . . . yes Pt(1) P(21) C(33) 114.5(3) . . . yes N(22) P(21) C(27) 105.8(4) . . . yes N(22) P(21) C(33) 104.9(4) . . . yes C(27) P(21) C(33) 103.0(4) . . . yes Pt(1) N(1) C(2) 117.3(5) . . . yes Pt(1) N(1) C(6) 125.9(5) . . . yes C(2) N(1) C(6) 116.8(7) . . . yes P(1) N(2) C(2) 120.2(6) . . . yes P(1) N(2) H(2) 114.7 . . . no C(2) N(2) H(2) 122.9 . . . no C(22) N(21) C(26) 117.8(8) . . . yes P(21) N(22) C(22) 123.7(6) . . . yes P(21) N(22) H(22) 116.5 . . . no C(22) N(22) H(22) 119.8 . . . no N(1) C(2) N(2) 118.0(7) . . . yes N(1) C(2) C(3) 121.1(9) . . . yes N(2) C(2) C(3) 120.8(8) . . . yes C(2) C(3) C(4) 118.8(9) . . . yes C(2) C(3) H(3) 120.6 . . . no C(4) C(3) H(3) 120.6 . . . no C(3) C(4) C(5) 120.2(9) . . . yes C(3) C(4) H(4) 119.9 . . . no C(5) C(4) H(4) 119.9 . . . no C(4) C(5) C(6) 118.2(9) . . . yes C(4) C(5) H(5) 120.9 . . . no C(6) C(5) H(5) 120.9 . . . no N(1) C(6) C(5) 124.8(9) . . . yes N(1) C(6) H(6) 117.6 . . . no C(5) C(6) H(6) 117.6 . . . no P(1) C(7) C(8) 119.7(7) . . . yes P(1) C(7) C(12) 120.8(7) . . . yes C(8) C(7) C(12) 119.4(8) . . . yes C(7) C(8) C(9) 119(1) . . . yes C(7) C(8) H(8) 120.4 . . . no C(9) C(8) H(8) 120.4 . . . no C(8) C(9) C(10) 120(1) . . . yes C(8) C(9) H(9) 120.1 . . . no C(10) C(9) H(9) 120.1 . . . no C(9) C(10) C(11) 121(1) . . . yes C(9) C(10) H(10) 119.6 . . . no C(11) C(10) H(10) 119.7 . . . no C(10) C(11) C(12) 121(1) . . . yes C(10) C(11) H(11) 119.6 . . . no C(12) C(11) H(11) 119.6 . . . no C(7) C(12) C(11) 120.1(9) . . . yes C(7) C(12) H(12) 119.9 . . . no C(11) C(12) H(12) 119.9 . . . no P(1) C(13) C(14) 124.4(7) . . . yes P(1) C(13) C(18) 116.1(6) . . . yes C(14) C(13) C(18) 119.4(8) . . . yes C(13) C(14) C(15) 119.9(9) . . . yes C(13) C(14) H(14) 120.1 . . . no C(15) C(14) H(14) 120.0 . . . no C(14) C(15) C(16) 120(1) . . . yes C(14) C(15) H(15) 119.8 . . . no C(16) C(15) H(15) 119.8 . . . no C(15) C(16) C(17) 121(1) . . . yes C(15) C(16) H(16) 119.8 . . . no C(17) C(16) H(16) 119.7 . . . no C(16) C(17) C(18) 120(1) . . . yes C(16) C(17) H(17) 119.8 . . . no C(18) C(17) H(17) 119.9 . . . no C(13) C(18) C(17) 119.2(9) . . . yes C(13) C(18) H(18) 120.4 . . . no C(17) C(18) H(18) 120.4 . . . no N(21) C(22) N(22) 117.1(7) . . . yes N(21) C(22) C(23) 122.2(9) . . . yes N(22) C(22) C(23) 120.7(9) . . . yes C(22) C(23) C(24) 117.5(9) . . . yes C(22) C(23) H(23) 121.2 . . . no C(24) C(23) H(23) 121.2 . . . no C(23) C(24) C(25) 121.3(9) . . . yes C(23) C(24) H(24) 119.3 . . . no C(25) C(24) H(24) 119.4 . . . no C(24) C(25) C(26) 117(1) . . . yes C(24) C(25) H(25) 121.7 . . . no C(26) C(25) H(25) 121.6 . . . no N(21) C(26) C(25) 124(1) . . . yes N(21) C(26) H(26) 117.8 . . . no C(25) C(26) H(26) 117.8 . . . no P(21) C(27) C(28) 120.8(7) . . . yes P(21) C(27) C(32) 120.6(7) . . . yes C(28) C(27) C(32) 118.7(8) . . . yes C(27) C(28) C(29) 119.9(9) . . . yes C(27) C(28) H(28) 120.1 . . . no C(29) C(28) H(28) 120.1 . . . no C(28) C(29) C(30) 120.3(9) . . . yes C(28) C(29) H(29) 119.8 . . . no C(30) C(29) H(29) 119.9 . . . no C(29) C(30) C(31) 120.5(9) . . . yes C(29) C(30) H(30) 119.8 . . . no C(31) C(30) H(30) 119.8 . . . no C(30) C(31) C(32) 120(1) . . . yes C(30) C(31) H(31) 120.1 . . . no C(32) C(31) H(31) 120.1 . . . no C(27) C(32) C(31) 120.9(9) . . . yes C(27) C(32) H(32) 119.6 . . . no C(31) C(32) H(32) 119.6 . . . no P(21) C(33) C(34) 120.6(6) . . . yes P(21) C(33) C(38) 121.0(7) . . . yes C(34) C(33) C(38) 118.1(9) . . . yes C(33) C(34) C(35) 120.1(9) . . . yes C(33) C(34) H(34) 120.0 . . . no C(35) C(34) H(34) 120.0 . . . no C(34) C(35) C(36) 120.3(9) . . . yes C(34) C(35) H(35) 119.8 . . . no C(36) C(35) H(35) 119.9 . . . no C(35) C(36) C(37) 120(1) . . . yes C(35) C(36) H(36) 120.0 . . . no C(37) C(36) H(36) 120.0 . . . no C(36) C(37) C(38) 120.7(9) . . . yes C(36) C(37) H(37) 119.6 . . . no C(38) C(37) H(37) 119.7 . . . no C(33) C(38) C(37) 120.8(9) . . . yes C(33) C(38) H(38) 119.6 . . . no C(37) C(38) H(38) 119.6 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(31) 3.57(1) . 1_556 no Cl(1) C(30) 3.59(1) . 1_556 no Cl(2) N(2) 3.111(7) . 1_656 no Cl(2) N(22) 3.223(7) . . no Cl(2) C(8) 3.56(1) . 1_656 no O(1) C(37) 2.46(2) . . no O(1) C(11) 2.60(2) . . no O(1) C(38) 2.68(2) . . no O(1) C(12) 2.79(3) . . no O(1) C(36) 2.80(2) . . no O(1) C(33) 3.17(2) . . no O(1) C(35) 3.27(2) . . no O(1) C(34) 3.43(2) . . no O(1) C(3) 3.54(2) . 2 no O(1) C(32) 3.55(2) . . no C(9) C(10) 3.53(1) . 2_554 no C(17) C(18) 3.59(1) . 2_565 no C(22) C(24) 3.54(1) . 2_666 no C(23) C(24) 3.49(1) . 2_666 no C(23) C(23) 3.54(2) . 2_666 no C(23) C(30) 3.58(1) . 1_556 no C(35) C(37) 3.38(1) . 2_656 no C(36) C(36) 3.48(2) . 2_656 no C(36) C(37) 3.51(1) . 2_656 no #----------------------------------------------------------------------- loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(2)' 'H(2)' 'Cl(2)' '0.97' '2.16' '3.111(7)' '169.1' '1_454' 'N(22)' 'H(22)' 'Cl(2)' '0.92' '2.34' '3.223(7)' '160.6' '.' #---END data_11 #----------------------------------------------------------------------- _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 10.526(2) _cell_length_b 12.720(2) _cell_length_c 22.094(1) _cell_angle_alpha 90 _cell_angle_beta 97.980(8) _cell_angle_gamma 90 _cell_volume 2929.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 35.5 _cell_measurement_theta_max 37.5 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 749.66 _chemical_formula_analytical 'C34 H28 N4 P2 Pt ' _chemical_formula_sum 'C34 H28 N4 P2 Pt ' _chemical_formula_moiety 'C34 H28 N4 P2 Pt ' _chemical_formula_structural 'C34 H28 N4 P2 Pt ' _chemical_compound_source - _exptl_crystal_F_000 1472.00 _exptl_absorpt_coefficient_mu 9.889 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.789 _exptl_special_details ; The scan width was (0.94+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.41 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 1 6 -4 0 6 -3 1 8 _diffrn_reflns_number 4877 _reflns_number_total 4595 _reflns_number_gt 3600 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.02416 _diffrn_reflns_av_sigmaI/netI - _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 60.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00669 _diffrn_orient_matrix_UB_12 -0.04045 _diffrn_orient_matrix_UB_13 0.03824 _diffrn_orient_matrix_UB_21 0.04984 _diffrn_orient_matrix_UB_22 0.05602 _diffrn_orient_matrix_UB_23 0.02463 _diffrn_orient_matrix_UB_31 -0.08169 _diffrn_orient_matrix_UB_32 0.03749 _diffrn_orient_matrix_UB_33 0.00445 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 136 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 112 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 4 -5.233 6.925 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.23486(2) 0.17269(2) 0.13299(1) 0.02895(7) 1.000 . Uani d ? P(1) 0.3678(1) 0.1465(1) 0.06339(6) 0.0329(4) 1.000 . Uani d ? P(2) 0.2903(2) 0.3281(1) 0.17579(7) 0.0340(4) 1.000 . Uani d ? N(1) 0.1584(5) 0.0329(3) 0.0910(2) 0.034(1) 1.000 . Uani d ? N(2) 0.3499(5) 0.0220(4) 0.0451(2) 0.040(1) 1.000 . Uani d ? N(21) 0.1285(5) 0.1733(3) 0.2073(2) 0.034(1) 1.000 . Uani d ? N(22) 0.1826(5) 0.3532(3) 0.2210(2) 0.038(1) 1.000 . Uani d ? C(2) 0.2380(6) -0.0183(4) 0.0553(3) 0.036(2) 1.000 . Uani d ? C(3) 0.1914(7) -0.1155(5) 0.0274(3) 0.047(2) 1.000 . Uani d ? C(4) 0.0729(7) -0.1517(5) 0.0328(3) 0.052(2) 1.000 . Uani d ? C(5) -0.0083(6) -0.0924(5) 0.0650(3) 0.047(2) 1.000 . Uani d ? C(6) 0.0384(6) -0.0026(5) 0.0928(3) 0.039(2) 1.000 . Uani d ? C(7) 0.5361(6) 0.1639(5) 0.0918(2) 0.037(2) 1.000 . Uani d ? C(8) 0.6051(6) 0.0821(5) 0.1224(3) 0.049(2) 1.000 . Uani d ? C(9) 0.7293(7) 0.0983(6) 0.1500(3) 0.062(3) 1.000 . Uani d ? C(10) 0.7856(7) 0.1949(7) 0.1462(3) 0.062(3) 1.000 . Uani d ? C(11) 0.7209(7) 0.2755(6) 0.1154(3) 0.057(2) 1.000 . Uani d ? C(12) 0.5962(6) 0.2606(5) 0.0878(3) 0.045(2) 1.000 . Uani d ? C(13) 0.3454(6) 0.2201(4) -0.0076(3) 0.037(2) 1.000 . Uani d ? C(14) 0.2626(6) 0.3034(5) -0.0176(3) 0.047(2) 1.000 . Uani d ? C(15) 0.2459(7) 0.3536(5) -0.0744(3) 0.058(2) 1.000 . Uani d ? C(16) 0.3102(7) 0.3188(6) -0.1205(3) 0.061(2) 1.000 . Uani d ? C(17) 0.3919(7) 0.2351(6) -0.1103(3) 0.059(2) 1.000 . Uani d ? C(18) 0.4091(7) 0.1858(5) -0.0545(3) 0.049(2) 1.000 . Uani d ? C(22) 0.1200(5) 0.2685(5) 0.2365(2) 0.035(2) 1.000 . Uani d ? C(23) 0.0406(6) 0.2740(5) 0.2837(3) 0.045(2) 1.000 . Uani d ? C(24) -0.0147(6) 0.1854(5) 0.3033(3) 0.044(2) 1.000 . Uani d ? C(25) 0.0054(7) 0.0876(5) 0.2770(3) 0.054(2) 1.000 . Uani d ? C(26) 0.0756(6) 0.0854(5) 0.2292(3) 0.040(2) 1.000 . Uani d ? C(27) 0.4466(6) 0.3357(4) 0.2217(3) 0.039(2) 1.000 . Uani d ? C(28) 0.5172(6) 0.2455(5) 0.2378(3) 0.042(2) 1.000 . Uani d ? C(29) 0.6309(6) 0.2488(5) 0.2764(3) 0.051(2) 1.000 . Uani d ? C(30) 0.6783(7) 0.3443(6) 0.2996(3) 0.059(2) 1.000 . Uani d ? C(31) 0.6097(7) 0.4348(5) 0.2850(3) 0.062(2) 1.000 . Uani d ? C(32) 0.4943(7) 0.4314(5) 0.2468(3) 0.052(2) 1.000 . Uani d ? C(33) 0.2814(6) 0.4389(4) 0.1233(3) 0.039(2) 1.000 . Uani d ? C(34) 0.1576(7) 0.4738(5) 0.1004(3) 0.050(2) 1.000 . Uani d ? C(35) 0.1452(8) 0.5533(6) 0.0569(3) 0.064(3) 1.000 . Uani d ? C(36) 0.250(1) 0.5973(6) 0.0378(3) 0.074(3) 1.000 . Uani d ? C(37) 0.3713(8) 0.5627(5) 0.0596(3) 0.064(3) 1.000 . Uani d ? C(38) 0.3860(7) 0.4842(5) 0.1034(3) 0.051(2) 1.000 . Uani d ? H(3) 0.2447 -0.1557 0.0046 0.055 1.000 . Uiso c ? H(4) 0.0442 -0.2174 0.0152 0.062 1.000 . Uiso c ? H(5) -0.0941 -0.1147 0.0671 0.056 1.000 . Uiso c ? H(6) -0.0159 0.0369 0.1155 0.046 1.000 . Uiso c ? H(8) 0.5679 0.0156 0.1252 0.057 1.000 . Uiso c ? H(9) 0.7767 0.0429 0.1703 0.072 1.000 . Uiso c ? H(10) 0.8720 0.2054 0.1649 0.076 1.000 . Uiso c ? H(11) 0.7611 0.3419 0.1135 0.066 1.000 . Uiso c ? H(12) 0.5521 0.3170 0.0664 0.054 1.000 . Uiso c ? H(14) 0.2167 0.3268 0.0138 0.057 1.000 . Uiso c ? H(15) 0.1894 0.4116 -0.0814 0.067 1.000 . Uiso c ? H(16) 0.2980 0.3526 -0.1591 0.072 1.000 . Uiso c ? H(17) 0.4363 0.2108 -0.1424 0.073 1.000 . Uiso c ? H(18) 0.4662 0.1280 -0.0478 0.059 1.000 . Uiso c ? H(23) 0.0266 0.3396 0.3014 0.053 1.000 . Uiso c ? H(24) -0.0675 0.1902 0.3349 0.053 1.000 . Uiso c ? H(25) -0.0294 0.0253 0.2913 0.063 1.000 . Uiso c ? H(26) 0.0891 0.0197 0.2107 0.048 1.000 . Uiso c ? H(28) 0.4867 0.1794 0.2218 0.050 1.000 . Uiso c ? H(29) 0.6770 0.1857 0.2869 0.062 1.000 . Uiso c ? H(30) 0.7578 0.3471 0.3262 0.071 1.000 . Uiso c ? H(31) 0.6429 0.5001 0.3008 0.075 1.000 . Uiso c ? H(32) 0.4467 0.4945 0.2382 0.065 1.000 . Uiso c ? H(34) 0.0840 0.4439 0.1150 0.059 1.000 . Uiso c ? H(35) 0.0625 0.5780 0.0399 0.075 1.000 . Uiso c ? H(36) 0.2423 0.6537 0.0091 0.089 1.000 . Uiso c ? H(37) 0.4452 0.5912 0.0451 0.077 1.000 . Uiso c ? H(38) 0.4702 0.4611 0.1198 0.058 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0424(2) 0.0193(1) 0.0255(1) -0.0009(1) 0.0060(1) -0.0014(1) P(1) 0.0474(9) 0.0240(8) 0.0282(8) -0.0003(7) 0.0084(7) -0.0040(6) P(2) 0.0524(9) 0.0204(7) 0.0298(8) -0.0026(7) 0.0080(7) -0.0034(6) N(1) 0.049(3) 0.020(3) 0.031(3) -0.005(2) 0.001(2) -0.002(2) N(2) 0.050(3) 0.024(3) 0.047(3) -0.001(2) 0.008(2) -0.005(2) N(21) 0.051(3) 0.028(3) 0.024(2) 0.000(2) 0.011(2) -0.001(2) N(22) 0.053(3) 0.023(3) 0.041(3) 0.001(2) 0.014(2) -0.002(2) C(2) 0.052(4) 0.023(3) 0.032(3) 0.006(3) 0.000(3) 0.002(3) C(3) 0.076(5) 0.020(3) 0.046(4) 0.001(3) 0.007(4) -0.007(3) C(4) 0.080(5) 0.026(4) 0.048(4) -0.011(3) 0.000(4) -0.003(3) C(5) 0.056(4) 0.039(4) 0.044(4) -0.016(3) 0.002(3) -0.001(3) C(6) 0.046(4) 0.034(4) 0.036(3) -0.006(3) 0.006(3) 0.001(3) C(7) 0.046(4) 0.040(4) 0.027(3) 0.003(3) 0.011(3) -0.009(3) C(8) 0.051(4) 0.043(4) 0.054(4) 0.006(3) 0.010(3) -0.007(3) C(9) 0.062(5) 0.075(6) 0.048(5) 0.017(4) 0.005(4) -0.002(4) C(10) 0.045(4) 0.081(6) 0.058(5) 0.000(4) -0.001(4) -0.010(4) C(11) 0.059(5) 0.066(5) 0.045(4) -0.015(4) 0.010(4) -0.008(4) C(12) 0.059(4) 0.044(4) 0.033(4) -0.005(3) 0.009(3) -0.003(3) C(13) 0.052(4) 0.024(3) 0.035(3) -0.006(3) 0.007(3) -0.005(3) C(14) 0.065(4) 0.039(4) 0.038(4) 0.006(3) 0.003(3) -0.005(3) C(15) 0.073(5) 0.048(4) 0.048(4) 0.010(4) -0.005(4) 0.000(3) C(16) 0.078(5) 0.068(5) 0.037(4) -0.006(4) 0.006(4) 0.007(4) C(17) 0.086(6) 0.066(5) 0.029(4) 0.002(4) 0.022(4) -0.001(3) C(18) 0.071(5) 0.040(4) 0.039(4) 0.006(3) 0.012(3) -0.004(3) C(22) 0.039(3) 0.037(4) 0.029(3) 0.004(3) 0.001(3) -0.003(3) C(23) 0.055(4) 0.043(4) 0.039(4) 0.012(3) 0.014(3) -0.005(3) C(24) 0.051(4) 0.055(4) 0.028(3) 0.003(3) 0.011(3) 0.008(3) C(25) 0.069(5) 0.053(5) 0.042(4) -0.013(4) 0.015(4) 0.009(3) C(26) 0.054(4) 0.033(4) 0.034(3) -0.005(3) 0.009(3) 0.003(3) C(27) 0.056(4) 0.032(3) 0.031(3) -0.004(3) 0.011(3) -0.007(3) C(28) 0.061(4) 0.030(3) 0.035(4) -0.003(3) 0.008(3) -0.006(3) C(29) 0.059(4) 0.048(4) 0.043(4) 0.012(3) 0.000(4) -0.011(3) C(30) 0.063(5) 0.061(5) 0.050(4) 0.003(4) -0.005(4) -0.019(4) C(31) 0.079(6) 0.039(4) 0.063(5) -0.010(4) -0.003(4) -0.028(4) C(32) 0.069(5) 0.035(4) 0.051(4) -0.004(3) 0.001(4) -0.011(3) C(33) 0.065(4) 0.017(3) 0.038(3) 0.000(3) 0.019(3) -0.003(3) C(34) 0.069(5) 0.039(4) 0.041(4) 0.010(4) 0.010(3) -0.001(3) C(35) 0.094(6) 0.048(4) 0.052(5) 0.029(4) 0.016(4) 0.009(4) C(36) 0.133(8) 0.036(4) 0.058(5) 0.011(5) 0.028(5) 0.019(4) C(37) 0.102(7) 0.036(4) 0.058(5) -0.016(4) 0.023(5) 0.010(4) C(38) 0.075(5) 0.031(4) 0.048(4) -0.013(3) 0.011(4) 0.001(3) #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000001149 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 3600 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all - _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_all - _refine_ls_wR_factor_ref 0.0274 _refine_ls_goodness_of_fit_all - _refine_ls_goodness_of_fit_ref 1.840 _refine_ls_shift/esd_max 0.3230 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.64 _refine_diff_density_max 0.50 #----------------------------------------------------------------------- _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) P(1) 2.243(2) . . yes Pt(1) P(2) 2.234(1) . . yes Pt(1) N(1) 2.112(4) . . yes Pt(1) N(21) 2.112(4) . . yes P(1) N(2) 1.640(5) . . yes P(1) C(7) 1.809(6) . . yes P(1) C(13) 1.814(6) . . yes P(2) N(22) 1.644(5) . . yes P(2) C(27) 1.811(6) . . yes P(2) C(33) 1.819(6) . . yes N(1) C(2) 1.390(7) . . yes N(1) C(6) 1.348(7) . . yes N(2) C(2) 1.332(7) . . yes N(21) C(22) 1.380(7) . . yes N(21) C(26) 1.367(7) . . yes N(22) C(22) 1.333(7) . . yes C(2) C(3) 1.436(8) . . yes C(3) C(4) 1.351(9) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.405(9) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.356(8) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.96 . . no C(7) C(8) 1.390(8) . . yes C(7) C(12) 1.391(8) . . yes C(8) C(9) 1.379(9) . . yes C(8) H(8) 0.94 . . no C(9) C(10) 1.37(1) . . yes C(9) H(9) 0.94 . . no C(10) C(11) 1.36(1) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.382(9) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.94 . . no C(13) C(14) 1.370(8) . . yes C(13) C(18) 1.381(8) . . yes C(14) C(15) 1.397(9) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.373(9) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.37(1) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.373(8) . . yes C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(22) C(23) 1.426(8) . . yes C(23) C(24) 1.367(8) . . yes C(23) H(23) 0.94 . . no C(24) C(25) 1.401(9) . . yes C(24) H(24) 0.95 . . no C(25) C(26) 1.371(8) . . yes C(25) H(25) 0.95 . . no C(26) H(26) 0.95 . . no C(27) C(28) 1.386(8) . . yes C(27) C(32) 1.401(8) . . yes C(28) C(29) 1.370(8) . . yes C(28) H(28) 0.95 . . no C(29) C(30) 1.384(9) . . yes C(29) H(29) 0.95 . . no C(30) C(31) 1.374(9) . . yes C(30) H(30) 0.95 . . no C(31) C(32) 1.380(9) . . yes C(31) H(31) 0.95 . . no C(32) H(32) 0.95 . . no C(33) C(34) 1.403(8) . . yes C(33) C(38) 1.368(8) . . yes C(34) C(35) 1.389(9) . . yes C(34) H(34) 0.96 . . no C(35) C(36) 1.36(1) . . yes C(35) H(35) 0.95 . . no C(36) C(37) 1.37(1) . . yes C(36) H(36) 0.95 . . no C(37) C(38) 1.383(9) . . yes C(37) H(37) 0.95 . . no C(38) H(38) 0.96 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Pt(1) P(2) 105.68(5) . . . yes P(1) Pt(1) N(1) 79.0(1) . . . yes P(1) Pt(1) N(21) 169.1(1) . . . yes P(2) Pt(1) N(1) 172.8(1) . . . yes P(2) Pt(1) N(21) 78.7(1) . . . yes N(1) Pt(1) N(21) 97.7(2) . . . yes Pt(1) P(1) N(2) 104.5(2) . . . yes Pt(1) P(1) C(7) 114.7(2) . . . yes Pt(1) P(1) C(13) 119.8(2) . . . yes N(2) P(1) C(7) 106.1(3) . . . yes N(2) P(1) C(13) 106.8(3) . . . yes C(7) P(1) C(13) 103.9(3) . . . yes Pt(1) P(2) N(22) 105.5(2) . . . yes Pt(1) P(2) C(27) 116.6(2) . . . yes Pt(1) P(2) C(33) 115.4(2) . . . yes N(22) P(2) C(27) 107.4(3) . . . yes N(22) P(2) C(33) 105.0(3) . . . yes C(27) P(2) C(33) 106.1(3) . . . yes Pt(1) N(1) C(2) 114.9(4) . . . yes Pt(1) N(1) C(6) 124.8(4) . . . yes C(2) N(1) C(6) 120.0(5) . . . yes P(1) N(2) C(2) 113.8(4) . . . yes Pt(1) N(21) C(22) 116.2(4) . . . yes Pt(1) N(21) C(26) 123.9(4) . . . yes C(22) N(21) C(26) 119.8(5) . . . yes P(2) N(22) C(22) 114.0(4) . . . yes N(1) C(2) N(2) 122.2(5) . . . yes N(1) C(2) C(3) 116.7(5) . . . yes N(2) C(2) C(3) 121.1(6) . . . yes C(2) C(3) C(4) 121.4(6) . . . yes C(2) C(3) H(3) 119.8 . . . no C(4) C(3) H(3) 118.8 . . . no C(3) C(4) C(5) 119.7(6) . . . yes C(3) C(4) H(4) 120.5 . . . no C(5) C(4) H(4) 119.8 . . . no C(4) C(5) C(6) 118.3(6) . . . yes C(4) C(5) H(5) 120.7 . . . no C(6) C(5) H(5) 121.0 . . . no N(1) C(6) C(5) 123.5(6) . . . yes N(1) C(6) H(6) 118.1 . . . no C(5) C(6) H(6) 118.4 . . . no P(1) C(7) C(8) 119.9(5) . . . yes P(1) C(7) C(12) 121.2(5) . . . yes C(8) C(7) C(12) 118.7(6) . . . yes C(7) C(8) C(9) 120.2(6) . . . yes C(7) C(8) H(8) 120.8 . . . no C(9) C(8) H(8) 118.9 . . . no C(8) C(9) C(10) 119.9(7) . . . yes C(8) C(9) H(9) 120.4 . . . no C(10) C(9) H(9) 119.7 . . . no C(9) C(10) C(11) 121.0(7) . . . yes C(9) C(10) H(10) 119.6 . . . no C(11) C(10) H(10) 119.4 . . . no C(10) C(11) C(12) 119.8(7) . . . yes C(10) C(11) H(11) 119.9 . . . no C(12) C(11) H(11) 120.3 . . . no C(7) C(12) C(11) 120.4(6) . . . yes C(7) C(12) H(12) 120.5 . . . no C(11) C(12) H(12) 119.2 . . . no P(1) C(13) C(14) 122.8(5) . . . yes P(1) C(13) C(18) 117.8(5) . . . yes C(14) C(13) C(18) 119.2(6) . . . yes C(13) C(14) C(15) 119.7(6) . . . yes C(13) C(14) H(14) 120.2 . . . no C(15) C(14) H(14) 120.1 . . . no C(14) C(15) C(16) 120.4(7) . . . yes C(14) C(15) H(15) 120.0 . . . no C(16) C(15) H(15) 119.5 . . . no C(15) C(16) C(17) 119.4(6) . . . yes C(15) C(16) H(16) 120.2 . . . no C(17) C(16) H(16) 120.4 . . . no C(16) C(17) C(18) 120.4(6) . . . yes C(16) C(17) H(17) 119.5 . . . no C(18) C(17) H(17) 120.2 . . . no C(13) C(18) C(17) 120.8(6) . . . yes C(13) C(18) H(18) 119.4 . . . no C(17) C(18) H(18) 119.8 . . . no N(21) C(22) N(22) 121.6(5) . . . yes N(21) C(22) C(23) 117.9(5) . . . yes N(22) C(22) C(23) 120.5(5) . . . yes C(22) C(23) C(24) 120.6(6) . . . yes C(22) C(23) H(23) 119.3 . . . no C(24) C(23) H(23) 120.1 . . . no C(23) C(24) C(25) 120.4(6) . . . yes C(23) C(24) H(24) 119.8 . . . no C(25) C(24) H(24) 119.8 . . . no C(24) C(25) C(26) 117.8(6) . . . yes C(24) C(25) H(25) 121.2 . . . no C(26) C(25) H(25) 121.0 . . . no N(21) C(26) C(25) 123.0(6) . . . yes N(21) C(26) H(26) 118.3 . . . no C(25) C(26) H(26) 118.6 . . . no P(2) C(27) C(28) 120.8(5) . . . yes P(2) C(27) C(32) 121.0(5) . . . yes C(28) C(27) C(32) 117.9(6) . . . yes C(27) C(28) C(29) 121.7(6) . . . yes C(27) C(28) H(28) 119.7 . . . no C(29) C(28) H(28) 118.6 . . . no C(28) C(29) C(30) 119.8(6) . . . yes C(28) C(29) H(29) 119.8 . . . no C(30) C(29) H(29) 120.4 . . . no C(29) C(30) C(31) 119.8(6) . . . yes C(29) C(30) H(30) 120.1 . . . no C(31) C(30) H(30) 120.1 . . . no C(30) C(31) C(32) 120.5(6) . . . yes C(30) C(31) H(31) 119.4 . . . no C(32) C(31) H(31) 120.1 . . . no C(27) C(32) C(31) 120.4(6) . . . yes C(27) C(32) H(32) 120.3 . . . no C(31) C(32) H(32) 119.3 . . . no P(2) C(33) C(34) 116.0(5) . . . yes P(2) C(33) C(38) 124.0(5) . . . yes C(34) C(33) C(38) 119.9(6) . . . yes C(33) C(34) C(35) 118.3(7) . . . yes C(33) C(34) H(34) 120.4 . . . no C(35) C(34) H(34) 121.3 . . . no C(34) C(35) C(36) 120.8(8) . . . yes C(34) C(35) H(35) 120.4 . . . no C(36) C(35) H(35) 118.8 . . . no C(35) C(36) C(37) 121.1(7) . . . yes C(35) C(36) H(36) 121.0 . . . no C(37) C(36) H(36) 117.9 . . . no C(36) C(37) C(38) 119.1(7) . . . yes C(36) C(37) H(37) 121.4 . . . no C(38) C(37) H(37) 119.5 . . . no C(33) C(38) C(37) 120.8(7) . . . yes C(33) C(38) H(38) 119.6 . . . no C(37) C(38) H(38) 119.7 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(22) C(25) 3.582(8) . 2 no C(4) C(6) 3.468(9) . 3 no C(16) C(23) 3.50(1) . 4_554 no C(16) C(24) 3.60(1) . 4_554 no #---end data_12 #----------------------------------------------------------------------- _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 10.530(2) _cell_length_b 12.715(1) _cell_length_c 22.115(1) _cell_angle_alpha 90 _cell_angle_beta 98.097(8) _cell_angle_gamma 90 _cell_volume 2931.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 37.1 _cell_measurement_theta_max 37.5 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 660.97 _chemical_formula_analytical 'C34 H28 N4 P2 Pd ' _chemical_formula_sum 'C34 H28 N4 P2 Pd ' _chemical_formula_moiety 'C34 H28 N4 P2 Pd ' _chemical_formula_structural 'C34 H28 N4 P2 Pd ' _chemical_compound_source - _exptl_crystal_F_000 1344.00 _exptl_absorpt_coefficient_mu 6.371 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.963 _exptl_special_details ; The scan width was (0.94+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.92 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 0 -4 -3 -4 -1 -3 -1 -6 _diffrn_reflns_number 4882 _reflns_number_total 4600 _reflns_number_gt 3811 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.13093 _diffrn_reflns_av_sigmaI/netI - _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 60.07 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00779 _diffrn_orient_matrix_UB_12 -0.05292 _diffrn_orient_matrix_UB_13 -0.03377 _diffrn_orient_matrix_UB_21 0.00938 _diffrn_orient_matrix_UB_22 -0.05816 _diffrn_orient_matrix_UB_23 0.03075 _diffrn_orient_matrix_UB_31 -0.09515 _diffrn_orient_matrix_UB_32 -0.00140 _diffrn_orient_matrix_UB_33 -0.00069 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 136 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 112 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 4 -0.059 3.934 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.23545(3) 0.17144(2) 0.13369(1) 0.03412(9) 1.000 . Uani d ? P(1) 0.3701(1) 0.14654(8) 0.06469(4) 0.0379(3) 1.000 . Uani d ? P(2) 0.2915(1) 0.32827(8) 0.17575(4) 0.0381(3) 1.000 . Uani d ? N(1) 0.1605(3) 0.0313(3) 0.0907(1) 0.0385(9) 1.000 . Uani d ? N(2) 0.3531(3) 0.0215(3) 0.0476(1) 0.046(1) 1.000 . Uani d ? N(21) 0.1302(3) 0.1726(3) 0.2085(1) 0.0399(9) 1.000 . Uani d ? N(22) 0.1823(3) 0.3532(3) 0.2202(1) 0.044(1) 1.000 . Uani d ? C(2) 0.2397(4) -0.0189(3) 0.0551(2) 0.040(1) 1.000 . Uani d ? C(3) 0.1962(4) -0.1143(3) 0.0263(2) 0.052(1) 1.000 . Uani d ? C(4) 0.0763(5) -0.1513(3) 0.0301(2) 0.057(1) 1.000 . Uani d ? C(5) -0.0051(4) -0.0960(4) 0.0632(2) 0.053(1) 1.000 . Uani d ? C(6) 0.0403(4) -0.0063(3) 0.0920(2) 0.045(1) 1.000 . Uani d ? C(7) 0.5384(4) 0.1646(3) 0.0924(2) 0.041(1) 1.000 . Uani d ? C(8) 0.6067(4) 0.0842(4) 0.1234(2) 0.053(1) 1.000 . Uani d ? C(9) 0.7331(4) 0.0999(4) 0.1504(2) 0.064(2) 1.000 . Uani d ? C(10) 0.7884(4) 0.1962(5) 0.1466(2) 0.067(2) 1.000 . Uani d ? C(11) 0.7227(4) 0.2773(4) 0.1158(2) 0.064(2) 1.000 . Uani d ? C(12) 0.5963(4) 0.2613(4) 0.0882(2) 0.050(1) 1.000 . Uani d ? C(13) 0.3466(4) 0.2194(3) -0.0064(2) 0.039(1) 1.000 . Uani d ? C(14) 0.2632(4) 0.3035(4) -0.0167(2) 0.053(1) 1.000 . Uani d ? C(15) 0.2448(5) 0.3542(4) -0.0728(2) 0.062(2) 1.000 . Uani d ? C(16) 0.3079(5) 0.3180(4) -0.1196(2) 0.066(2) 1.000 . Uani d ? C(17) 0.3891(5) 0.2346(4) -0.1097(2) 0.064(2) 1.000 . Uani d ? C(18) 0.4089(4) 0.1849(4) -0.0541(2) 0.052(1) 1.000 . Uani d ? C(22) 0.1203(4) 0.2680(3) 0.2366(2) 0.042(1) 1.000 . Uani d ? C(23) 0.0423(4) 0.2744(4) 0.2846(2) 0.049(1) 1.000 . Uani d ? C(24) -0.0131(4) 0.1880(4) 0.3039(2) 0.056(1) 1.000 . Uani d ? C(25) 0.0052(4) 0.0903(4) 0.2782(2) 0.055(1) 1.000 . Uani d ? C(26) 0.0770(4) 0.0863(3) 0.2313(2) 0.046(1) 1.000 . Uani d ? C(27) 0.4480(4) 0.3354(3) 0.2224(2) 0.042(1) 1.000 . Uani d ? C(28) 0.5154(4) 0.2441(3) 0.2386(2) 0.048(1) 1.000 . Uani d ? C(29) 0.6304(4) 0.2474(4) 0.2780(2) 0.059(2) 1.000 . Uani d ? C(30) 0.6760(4) 0.3414(4) 0.3018(2) 0.064(2) 1.000 . Uani d ? C(31) 0.6095(5) 0.4319(4) 0.2868(2) 0.068(2) 1.000 . Uani d ? C(32) 0.4952(5) 0.4302(4) 0.2472(2) 0.059(1) 1.000 . Uani d ? C(33) 0.2831(4) 0.4390(3) 0.1243(2) 0.043(1) 1.000 . Uani d ? C(34) 0.1612(4) 0.4751(4) 0.1002(2) 0.052(1) 1.000 . Uani d ? C(35) 0.1467(5) 0.5553(4) 0.0577(2) 0.071(2) 1.000 . Uani d ? C(36) 0.2538(6) 0.5985(4) 0.0379(2) 0.078(2) 1.000 . Uani d ? C(37) 0.3729(5) 0.5641(4) 0.0609(2) 0.070(2) 1.000 . Uani d ? C(38) 0.3888(4) 0.4847(4) 0.1043(2) 0.055(1) 1.000 . Uani d ? H(3) 0.2518 -0.1525 0.0039 0.062 1.000 . Uiso c ? H(4) 0.0486 -0.2150 0.0102 0.068 1.000 . Uiso c ? H(5) -0.0898 -0.1201 0.0654 0.063 1.000 . Uiso c ? H(6) -0.0150 0.0318 0.1144 0.054 1.000 . Uiso c ? H(8) 0.5672 0.0175 0.1265 0.063 1.000 . Uiso c ? H(9) 0.7802 0.0436 0.1713 0.077 1.000 . Uiso c ? H(10) 0.8740 0.2077 0.1652 0.082 1.000 . Uiso c ? H(11) 0.7625 0.3438 0.1130 0.077 1.000 . Uiso c ? H(12) 0.5501 0.3172 0.0668 0.059 1.000 . Uiso c ? H(14) 0.2177 0.3269 0.0153 0.063 1.000 . Uiso c ? H(15) 0.1889 0.4132 -0.0794 0.074 1.000 . Uiso c ? H(16) 0.2960 0.3516 -0.1585 0.080 1.000 . Uiso c ? H(17) 0.4328 0.2100 -0.1419 0.077 1.000 . Uiso c ? H(18) 0.4663 0.1266 -0.0483 0.063 1.000 . Uiso c ? H(23) 0.0302 0.3405 0.3033 0.059 1.000 . Uiso c ? H(24) -0.0660 0.1936 0.3355 0.067 1.000 . Uiso c ? H(25) -0.0312 0.0287 0.2930 0.066 1.000 . Uiso c ? H(26) 0.0910 0.0196 0.2136 0.055 1.000 . Uiso c ? H(28) 0.4833 0.1788 0.2227 0.058 1.000 . Uiso c ? H(29) 0.6776 0.1845 0.2882 0.069 1.000 . Uiso c ? H(30) 0.7547 0.3440 0.3286 0.076 1.000 . Uiso c ? H(31) 0.6424 0.4968 0.3033 0.080 1.000 . Uiso c ? H(32) 0.4494 0.4935 0.2373 0.070 1.000 . Uiso c ? H(34) 0.0875 0.4444 0.1135 0.062 1.000 . Uiso c ? H(35) 0.0644 0.5812 0.0417 0.085 1.000 . Uiso c ? H(36) 0.2455 0.6523 0.0078 0.093 1.000 . Uiso c ? H(37) 0.4462 0.5950 0.0472 0.083 1.000 . Uiso c ? H(38) 0.4730 0.4614 0.1201 0.066 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0402(2) 0.0356(2) 0.0297(2) -0.0012(1) 0.0157(1) -0.0016(1) P(1) 0.0430(6) 0.0407(6) 0.0335(5) -0.0009(5) 0.0170(4) -0.0026(4) P(2) 0.0476(6) 0.0366(6) 0.0332(5) -0.0014(5) 0.0166(4) -0.0035(4) N(1) 0.046(2) 0.041(2) 0.029(2) -0.002(2) 0.008(1) -0.001(1) N(2) 0.053(2) 0.040(2) 0.048(2) -0.001(2) 0.023(2) -0.007(2) N(21) 0.046(2) 0.043(2) 0.034(2) -0.003(2) 0.016(1) -0.001(1) N(22) 0.055(2) 0.040(2) 0.043(2) 0.003(2) 0.027(2) -0.006(2) C(2) 0.053(2) 0.034(2) 0.036(2) 0.005(2) 0.011(2) 0.000(2) C(3) 0.068(3) 0.040(3) 0.051(3) 0.002(2) 0.015(2) -0.008(2) C(4) 0.076(3) 0.038(3) 0.056(3) -0.010(2) 0.005(2) -0.004(2) C(5) 0.058(3) 0.054(3) 0.047(3) -0.014(2) 0.010(2) -0.001(2) C(6) 0.050(2) 0.047(3) 0.040(2) -0.002(2) 0.015(2) 0.001(2) C(7) 0.044(2) 0.053(3) 0.029(2) 0.002(2) 0.018(2) -0.004(2) C(8) 0.051(3) 0.063(3) 0.046(3) 0.004(2) 0.016(2) -0.006(2) C(9) 0.052(3) 0.086(4) 0.057(3) 0.017(3) 0.013(2) -0.002(3) C(10) 0.042(3) 0.104(5) 0.057(3) -0.002(3) 0.010(2) -0.010(3) C(11) 0.058(3) 0.084(4) 0.054(3) -0.018(3) 0.019(2) -0.005(3) C(12) 0.049(3) 0.062(3) 0.041(2) -0.003(2) 0.016(2) -0.003(2) C(13) 0.043(2) 0.039(2) 0.037(2) -0.005(2) 0.013(2) -0.004(2) C(14) 0.062(3) 0.058(3) 0.039(2) 0.005(2) 0.010(2) -0.009(2) C(15) 0.080(3) 0.058(3) 0.047(3) 0.012(3) 0.004(2) 0.001(2) C(16) 0.080(4) 0.077(4) 0.041(3) -0.004(3) 0.007(2) 0.008(3) C(17) 0.078(3) 0.081(4) 0.039(3) 0.001(3) 0.025(2) 0.000(2) C(18) 0.060(3) 0.060(3) 0.042(2) 0.005(2) 0.021(2) -0.004(2) C(22) 0.040(2) 0.053(3) 0.034(2) 0.002(2) 0.013(2) 0.003(2) C(23) 0.053(3) 0.060(3) 0.038(2) 0.010(2) 0.021(2) -0.001(2) C(24) 0.055(3) 0.080(4) 0.039(2) 0.003(3) 0.025(2) 0.009(2) C(25) 0.060(3) 0.066(3) 0.041(2) -0.011(3) 0.019(2) 0.014(2) C(26) 0.055(3) 0.047(3) 0.038(2) -0.006(2) 0.017(2) 0.005(2) C(27) 0.046(2) 0.045(3) 0.037(2) -0.006(2) 0.016(2) -0.006(2) C(28) 0.060(3) 0.048(3) 0.040(2) -0.001(2) 0.017(2) -0.008(2) C(29) 0.060(3) 0.065(3) 0.051(3) 0.008(3) 0.006(2) -0.005(2) C(30) 0.054(3) 0.079(4) 0.058(3) -0.003(3) 0.007(2) -0.019(3) C(31) 0.065(3) 0.064(3) 0.072(3) -0.008(3) 0.004(3) -0.023(3) C(32) 0.068(3) 0.049(3) 0.059(3) 0.003(2) 0.007(2) -0.012(2) C(33) 0.060(3) 0.039(2) 0.035(2) 0.001(2) 0.021(2) -0.006(2) C(34) 0.062(3) 0.055(3) 0.043(2) 0.011(2) 0.021(2) 0.001(2) C(35) 0.093(4) 0.064(3) 0.061(3) 0.026(3) 0.028(3) 0.011(3) C(36) 0.127(5) 0.052(3) 0.062(3) 0.014(3) 0.038(3) 0.020(3) C(37) 0.097(4) 0.056(3) 0.065(3) -0.016(3) 0.037(3) 0.008(3) C(38) 0.068(3) 0.049(3) 0.053(3) -0.011(2) 0.022(2) 0.001(2) #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000003003 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 3811 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all - _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_all - _refine_ls_wR_factor_ref 0.0302 _refine_ls_goodness_of_fit_all - _refine_ls_goodness_of_fit_ref 2.600 _refine_ls_shift/esd_max 0.0290 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.51 _refine_diff_density_max 0.49 #----------------------------------------------------------------------- _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) P(1) 2.247(1) . . yes Pd(1) P(2) 2.244(1) . . yes Pd(1) N(1) 2.119(3) . . yes Pd(1) N(21) 2.118(3) . . yes P(1) N(2) 1.638(3) . . yes P(1) C(7) 1.806(4) . . yes P(1) C(13) 1.811(4) . . yes P(2) N(22) 1.645(3) . . yes P(2) C(27) 1.819(4) . . yes P(2) C(33) 1.805(4) . . yes N(1) C(2) 1.381(4) . . yes N(1) C(6) 1.357(5) . . yes N(2) C(2) 1.331(5) . . yes N(21) C(22) 1.374(5) . . yes N(21) C(26) 1.361(5) . . yes N(22) C(22) 1.341(5) . . yes C(2) C(3) 1.415(5) . . yes C(3) C(4) 1.361(6) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.393(6) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.361(6) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.377(6) . . yes C(7) C(12) 1.381(6) . . yes C(8) C(9) 1.395(6) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.363(7) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.368(7) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.399(6) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) C(14) 1.382(5) . . yes C(13) C(18) 1.391(5) . . yes C(14) C(15) 1.387(6) . . yes C(14) H(14) 0.96 . . no C(15) C(16) 1.385(6) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.361(7) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.372(6) . . yes C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(22) C(23) 1.433(5) . . yes C(23) C(24) 1.342(6) . . yes C(23) H(23) 0.95 . . no C(24) C(25) 1.390(6) . . yes C(24) H(24) 0.96 . . no C(25) C(26) 1.367(5) . . yes C(25) H(25) 0.95 . . no C(26) H(26) 0.95 . . no C(27) C(28) 1.381(6) . . yes C(27) C(32) 1.387(6) . . yes C(28) C(29) 1.389(6) . . yes C(28) H(28) 0.95 . . no C(29) C(30) 1.366(6) . . yes C(29) H(29) 0.95 . . no C(30) C(31) 1.363(7) . . yes C(30) H(30) 0.95 . . no C(31) C(32) 1.385(6) . . yes C(31) H(31) 0.95 . . no C(32) H(32) 0.95 . . no C(33) C(34) 1.395(5) . . yes C(33) C(38) 1.382(5) . . yes C(34) C(35) 1.382(6) . . yes C(34) H(34) 0.95 . . no C(35) C(36) 1.381(7) . . yes C(35) H(35) 0.95 . . no C(36) C(37) 1.357(7) . . yes C(36) H(36) 0.95 . . no C(37) C(38) 1.387(6) . . yes C(37) H(37) 0.95 . . no C(38) H(38) 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Pd(1) P(2) 104.62(4) . . . yes P(1) Pd(1) N(1) 78.89(8) . . . yes P(1) Pd(1) N(21) 168.99(9) . . . yes P(2) Pd(1) N(1) 173.13(9) . . . yes P(2) Pd(1) N(21) 78.80(9) . . . yes N(1) Pd(1) N(21) 98.9(1) . . . yes Pd(1) P(1) N(2) 103.5(1) . . . yes Pd(1) P(1) C(7) 115.7(1) . . . yes Pd(1) P(1) C(13) 119.7(1) . . . yes N(2) P(1) C(7) 105.8(2) . . . yes N(2) P(1) C(13) 107.4(2) . . . yes C(7) P(1) C(13) 103.7(2) . . . yes Pd(1) P(2) N(22) 104.7(1) . . . yes Pd(1) P(2) C(27) 116.3(1) . . . yes Pd(1) P(2) C(33) 116.4(1) . . . yes N(22) P(2) C(27) 107.7(2) . . . yes N(22) P(2) C(33) 104.5(2) . . . yes C(27) P(2) C(33) 106.2(2) . . . yes Pd(1) N(1) C(2) 115.3(2) . . . yes Pd(1) N(1) C(6) 125.1(3) . . . yes C(2) N(1) C(6) 119.3(3) . . . yes P(1) N(2) C(2) 114.7(3) . . . yes Pd(1) N(21) C(22) 116.2(2) . . . yes Pd(1) N(21) C(26) 124.9(3) . . . yes C(22) N(21) C(26) 118.9(3) . . . yes P(2) N(22) C(22) 114.5(3) . . . yes N(1) C(2) N(2) 121.1(4) . . . yes N(1) C(2) C(3) 118.0(4) . . . yes N(2) C(2) C(3) 121.0(4) . . . yes C(2) C(3) C(4) 120.9(4) . . . yes C(2) C(3) H(3) 119.2 . . . no C(4) C(3) H(3) 119.9 . . . no C(3) C(4) C(5) 120.2(4) . . . yes C(3) C(4) H(4) 119.6 . . . no C(5) C(4) H(4) 120.2 . . . no C(4) C(5) C(6) 117.9(4) . . . yes C(4) C(5) H(5) 121.0 . . . no C(6) C(5) H(5) 121.2 . . . no N(1) C(6) C(5) 123.5(4) . . . yes N(1) C(6) H(6) 118.4 . . . no C(5) C(6) H(6) 118.1 . . . no P(1) C(7) C(8) 119.5(3) . . . yes P(1) C(7) C(12) 120.8(3) . . . yes C(8) C(7) C(12) 119.4(4) . . . yes C(7) C(8) C(9) 120.5(5) . . . yes C(7) C(8) H(8) 119.7 . . . no C(9) C(8) H(8) 119.8 . . . no C(8) C(9) C(10) 119.4(5) . . . yes C(8) C(9) H(9) 120.1 . . . no C(10) C(9) H(9) 120.5 . . . no C(9) C(10) C(11) 121.2(4) . . . yes C(9) C(10) H(10) 119.9 . . . no C(11) C(10) H(10) 118.9 . . . no C(10) C(11) C(12) 119.4(5) . . . yes C(10) C(11) H(11) 120.4 . . . no C(12) C(11) H(11) 120.2 . . . no C(7) C(12) C(11) 120.1(4) . . . yes C(7) C(12) H(12) 120.0 . . . no C(11) C(12) H(12) 119.9 . . . no P(1) C(13) C(14) 123.1(3) . . . yes P(1) C(13) C(18) 118.4(3) . . . yes C(14) C(13) C(18) 118.4(4) . . . yes C(13) C(14) C(15) 120.9(4) . . . yes C(13) C(14) H(14) 119.4 . . . no C(15) C(14) H(14) 119.8 . . . no C(14) C(15) C(16) 119.5(5) . . . yes C(14) C(15) H(15) 120.5 . . . no C(16) C(15) H(15) 120.0 . . . no C(15) C(16) C(17) 119.7(4) . . . yes C(15) C(16) H(16) 120.7 . . . no C(17) C(16) H(16) 119.6 . . . no C(16) C(17) C(18) 121.1(4) . . . yes C(16) C(17) H(17) 119.6 . . . no C(18) C(17) H(17) 119.3 . . . no C(13) C(18) C(17) 120.5(4) . . . yes C(13) C(18) H(18) 120.0 . . . no C(17) C(18) H(18) 119.6 . . . no N(21) C(22) N(22) 121.3(3) . . . yes N(21) C(22) C(23) 118.3(4) . . . yes N(22) C(22) C(23) 120.4(4) . . . yes C(22) C(23) C(24) 120.5(4) . . . yes C(22) C(23) H(23) 119.8 . . . no C(24) C(23) H(23) 119.6 . . . no C(23) C(24) C(25) 120.7(4) . . . yes C(23) C(24) H(24) 119.7 . . . no C(25) C(24) H(24) 119.6 . . . no C(24) C(25) C(26) 117.8(4) . . . yes C(24) C(25) H(25) 120.7 . . . no C(26) C(25) H(25) 121.5 . . . no N(21) C(26) C(25) 123.4(4) . . . yes N(21) C(26) H(26) 118.0 . . . no C(25) C(26) H(26) 118.6 . . . no P(2) C(27) C(28) 119.8(3) . . . yes P(2) C(27) C(32) 120.9(3) . . . yes C(28) C(27) C(32) 119.1(4) . . . yes C(27) C(28) C(29) 120.5(4) . . . yes C(27) C(28) H(28) 119.9 . . . no C(29) C(28) H(28) 119.6 . . . no C(28) C(29) C(30) 119.7(5) . . . yes C(28) C(29) H(29) 120.2 . . . no C(30) C(29) H(29) 120.1 . . . no C(29) C(30) C(31) 120.3(4) . . . yes C(29) C(30) H(30) 120.0 . . . no C(31) C(30) H(30) 119.8 . . . no C(30) C(31) C(32) 120.8(5) . . . yes C(30) C(31) H(31) 119.6 . . . no C(32) C(31) H(31) 119.6 . . . no C(27) C(32) C(31) 119.6(5) . . . yes C(27) C(32) H(32) 120.3 . . . no C(31) C(32) H(32) 120.1 . . . no P(2) C(33) C(34) 117.2(3) . . . yes P(2) C(33) C(38) 124.0(3) . . . yes C(34) C(33) C(38) 118.6(4) . . . yes C(33) C(34) C(35) 120.6(4) . . . yes C(33) C(34) H(34) 119.7 . . . no C(35) C(34) H(34) 119.7 . . . no C(34) C(35) C(36) 119.6(5) . . . yes C(34) C(35) H(35) 121.2 . . . no C(36) C(35) H(35) 119.2 . . . no C(35) C(36) C(37) 120.4(5) . . . yes C(35) C(36) H(36) 120.7 . . . no C(37) C(36) H(36) 119.0 . . . no C(36) C(37) C(38) 120.6(5) . . . yes C(36) C(37) H(37) 119.7 . . . no C(38) C(37) H(37) 119.7 . . . no C(33) C(38) C(37) 120.2(5) . . . yes C(33) C(38) H(38) 120.2 . . . no C(37) C(38) H(38) 119.6 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(1) C(31) 3.599(5) . 2_645 no C(4) C(6) 3.447(6) . 3 no C(16) C(23) 3.467(6) . 4_554 no C(16) C(24) 3.561(7) . 4_554 no #---END data_14 #----------------------------------------------------------------------- _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 24.662(4) _cell_length_b 26.730(3) _cell_length_c 10.728(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7072(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 31.6 _cell_measurement_theta_max 37.4 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2 ' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' +x, +y, +z' ' +x, +y, +z' ' -x, -y, +z' ' -x, -y, +z' ' -x, -y, +z' ' -x, -y, +z' '1/4-x,1/4+y,1/4+z' ' -x, +y, +z' ' -x, +y, +z' ' -x, +y, +z' '1/4+x,1/4-y,1/4+z' ' +x, -y, +z' ' +x, -y, +z' ' +x, -y, +z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ; _exptl_crystal_description 'block' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 836.59 _chemical_formula_analytical 'C34 H30 B2 F8 N4 P2 Pd ' _chemical_formula_sum 'C34 H30 B2 F8 N4 P2 Pd ' _chemical_formula_moiety 'C34 H30 N4 P2 Pd.[B F4]2' _chemical_formula_structural 'C34 H30 B2 F8 N4 P2 Pd ' _chemical_compound_source - _exptl_crystal_F_000 3360.00 _exptl_absorpt_coefficient_mu 5.742 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_correction_T_min 0.658 _exptl_special_details ; The scan width was (1.15+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -8.52 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -9 3 -1 9 3 1 -9 3 _diffrn_reflns_number 1479 _reflns_number_total 1479 _reflns_number_gt 1259 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI - _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 60.08 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01140 _diffrn_orient_matrix_UB_12 0.00348 _diffrn_orient_matrix_UB_13 0.08904 _diffrn_orient_matrix_UB_21 -0.00251 _diffrn_orient_matrix_UB_22 0.03722 _diffrn_orient_matrix_UB_23 -0.00733 _diffrn_orient_matrix_UB_31 -0.03883 _diffrn_orient_matrix_UB_32 -0.00139 _diffrn_orient_matrix_UB_33 0.02660 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 272 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 240 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; B 0 16 0.008 0.004 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 64 0.069 0.053 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 32 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 16 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 8 -0.059 3.934 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.2500 0.2500 0.0066 0.0462(2) 0.500 ST Uani d ? P(1) 0.2736(1) 0.18881(9) 0.1377(3) 0.0499(7) 1.000 . Uani d ? F(1) 0.3820(3) -0.0135(3) 0.145(1) 0.135(4) 1.000 . Uani d ? F(2) 0.3404(7) 0.0220(5) -0.007(1) 0.228(7) 1.000 . Uani d ? F(3) 0.3521(4) 0.0625(3) 0.155(1) 0.154(4) 1.000 . Uani d ? F(4) 0.2969(3) -0.0007(3) 0.152(2) 0.222(7) 1.000 . Uani d ? N(1) 0.2539(3) 0.1911(3) -0.1205(9) 0.051(2) 1.000 . Uani d ? N(2) 0.2977(3) 0.1478(3) 0.0332(7) 0.061(2) 1.000 . Uani d ? C(2) 0.2765(4) 0.1478(3) -0.0868(9) 0.054(3) 1.000 . Uani d ? C(3) 0.2784(4) 0.1065(4) -0.163(1) 0.066(3) 1.000 . Uani d ? C(4) 0.2533(5) 0.1095(5) -0.278(2) 0.079(5) 1.000 . Uani d ? C(5) 0.2274(5) 0.1532(4) -0.311(1) 0.076(4) 1.000 . Uani d ? C(6) 0.2283(4) 0.1925(4) -0.235(1) 0.065(3) 1.000 . Uani d ? C(7) 0.2232(4) 0.1581(3) 0.2304(8) 0.052(3) 1.000 . Uani d ? C(8) 0.1686(4) 0.1684(3) 0.213(1) 0.065(3) 1.000 . Uani d ? C(9) 0.1301(4) 0.1448(4) 0.286(1) 0.085(4) 1.000 . Uani d ? C(10) 0.1457(6) 0.1094(5) 0.372(1) 0.094(5) 1.000 . Uani d ? C(11) 0.1999(6) 0.0972(4) 0.387(1) 0.083(4) 1.000 . Uani d ? C(12) 0.2387(5) 0.1217(5) 0.316(1) 0.067(4) 1.000 . Uani d ? C(13) 0.3291(4) 0.2019(3) 0.2392(9) 0.052(3) 1.000 . Uani d ? C(14) 0.3198(4) 0.2175(4) 0.3617(9) 0.062(3) 1.000 . Uani d ? C(15) 0.3616(5) 0.2329(4) 0.437(1) 0.070(3) 1.000 . Uani d ? C(16) 0.4136(5) 0.2320(4) 0.390(1) 0.083(4) 1.000 . Uani d ? C(17) 0.4241(5) 0.2165(5) 0.272(2) 0.094(5) 1.000 . Uani d ? C(18) 0.3823(4) 0.2021(4) 0.196(1) 0.072(4) 1.000 . Uani d ? B(1) 0.3424(6) 0.0165(5) 0.114(2) 0.076(4) 1.000 . Uani d ? H(2) 0.3091 0.1236 0.0510 0.044 1.000 . Uiso c ? H(3) 0.2958 0.0767 -0.1386 0.078 1.000 . Uiso c ? H(4) 0.2531 0.0822 -0.3345 0.092 1.000 . Uiso c ? H(5) 0.2094 0.1553 -0.3902 0.091 1.000 . Uiso c ? H(6) 0.2103 0.2226 -0.2589 0.077 1.000 . Uiso c ? H(8) 0.1577 0.1915 0.1509 0.078 1.000 . Uiso c ? H(9) 0.0925 0.1526 0.2758 0.102 1.000 . Uiso c ? H(10) 0.1192 0.0935 0.4217 0.111 1.000 . Uiso c ? H(11) 0.2103 0.0724 0.4463 0.099 1.000 . Uiso c ? H(12) 0.2758 0.1133 0.3240 0.082 1.000 . Uiso c ? H(14) 0.2837 0.2179 0.3931 0.072 1.000 . Uiso c ? H(15) 0.3549 0.2437 0.5194 0.081 1.000 . Uiso c ? H(16) 0.4425 0.2419 0.4423 0.099 1.000 . Uiso c ? H(17) 0.4605 0.2161 0.2433 0.114 1.000 . Uiso c ? H(18) 0.3898 0.1917 0.1126 0.084 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0505(5) 0.0510(4) 0.0371(4) 0.0023(5) 0.0000 0.0000 P(1) 0.054(2) 0.056(1) 0.040(1) 0.003(1) 0.000(1) 0.004(1) F(1) 0.092(6) 0.133(6) 0.180(9) 0.034(5) -0.008(7) 0.058(7) F(2) 0.36(2) 0.20(1) 0.12(1) 0.00(1) -0.09(1) 0.02(1) F(3) 0.158(8) 0.094(6) 0.21(1) -0.010(5) -0.029(9) -0.019(7) F(4) 0.077(6) 0.174(9) 0.41(2) -0.016(5) 0.05(1) 0.04(1) N(1) 0.046(5) 0.056(5) 0.050(5) -0.001(3) 0.002(5) 0.004(4) N(2) 0.074(5) 0.053(4) 0.054(5) 0.014(4) 0.004(4) 0.006(4) C(2) 0.061(6) 0.055(5) 0.046(5) -0.004(4) 0.009(5) -0.005(5) C(3) 0.078(7) 0.053(5) 0.066(7) 0.005(5) 0.008(6) -0.002(5) C(4) 0.10(1) 0.062(7) 0.07(1) -0.002(6) 0.012(7) -0.023(7) C(5) 0.082(7) 0.088(8) 0.058(7) 0.005(6) -0.007(6) -0.022(6) C(6) 0.068(6) 0.070(6) 0.057(6) 0.001(5) -0.006(6) -0.001(6) C(7) 0.056(5) 0.059(5) 0.039(5) -0.006(4) -0.002(4) 0.000(4) C(8) 0.063(6) 0.061(6) 0.073(7) 0.001(5) 0.003(5) -0.009(5) C(9) 0.067(7) 0.080(7) 0.11(1) -0.013(6) 0.026(7) -0.017(8) C(10) 0.10(1) 0.086(8) 0.09(1) -0.035(7) 0.033(9) -0.022(8) C(11) 0.12(1) 0.079(7) 0.048(6) -0.033(7) 0.001(8) 0.006(6) C(12) 0.074(8) 0.075(8) 0.051(7) -0.015(6) -0.003(6) 0.011(6) C(13) 0.056(5) 0.052(5) 0.048(6) 0.003(4) -0.006(5) 0.011(4) C(14) 0.066(6) 0.068(6) 0.052(6) -0.001(5) -0.009(5) 0.010(5) C(15) 0.086(8) 0.059(6) 0.064(7) -0.002(5) -0.023(6) 0.009(5) C(16) 0.081(9) 0.083(7) 0.085(9) -0.008(6) -0.032(8) 0.015(8) C(17) 0.056(7) 0.098(9) 0.13(1) -0.002(6) -0.028(9) 0.02(1) C(18) 0.061(6) 0.088(8) 0.067(7) 0.005(6) 0.000(6) 0.002(6) B(1) 0.071(9) 0.054(7) 0.10(1) 0.002(6) -0.012(8) 0.011(8) #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000029(2) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1259 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_all 0.0448 _refine_ls_wR_factor_ref 0.0448 _refine_ls_goodness_of_fit_all 2.346 _refine_ls_goodness_of_fit_ref 2.346 _refine_ls_shift/esd_max 0.2720 _refine_ls_shift/esd_mean 0.5400 _refine_diff_density_min -0.54 _refine_diff_density_max 1.34 #----------------------------------------------------------------------- _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) P(1) 2.234(2) . . yes Pd(1) P(1) 2.234(2) . 14 yes Pd(1) N(1) 2.084(9) . . yes Pd(1) N(1) 2.084(9) . 14 yes P(1) N(2) 1.677(7) . . yes P(1) C(7) 1.791(9) . . yes P(1) C(13) 1.784(9) . . yes F(1) B(1) 1.31(1) . . yes F(2) B(1) 1.31(2) . . yes F(3) B(1) 1.33(1) . . yes F(4) B(1) 1.28(2) . . yes N(1) C(2) 1.33(1) . . yes N(1) C(6) 1.38(1) . . yes N(2) C(2) 1.39(1) . . yes N(2) H(2) 0.73 . . no C(2) C(3) 1.38(1) . . yes C(3) C(4) 1.38(2) . . yes C(3) H(3) 0.94 . . no C(4) C(5) 1.38(2) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.33(1) . . yes C(5) H(5) 0.96 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.38(1) . . yes C(7) C(12) 1.39(2) . . yes C(8) C(9) 1.38(1) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.37(2) . . yes C(9) H(9) 0.96 . . no C(10) C(11) 1.38(2) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.39(2) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) C(14) 1.40(1) . . yes C(13) C(18) 1.39(1) . . yes C(14) C(15) 1.37(1) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.38(2) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.35(2) . . yes C(16) H(16) 0.94 . . no C(17) C(18) 1.38(2) . . yes C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Pd(1) P(1) 101.9(1) . . 14 yes P(1) Pd(1) N(1) 81.2(2) . . . yes P(1) Pd(1) N(1) 167.6(2) . . 14 yes P(1) Pd(1) N(1) 167.6(2) 14 . . yes P(1) Pd(1) N(1) 81.2(2) 14 . 14 yes N(1) Pd(1) N(1) 98.3(5) . . 14 yes Pd(1) P(1) N(2) 98.6(3) . . . yes Pd(1) P(1) C(7) 120.3(3) . . . yes Pd(1) P(1) C(13) 116.1(3) . . . yes N(2) P(1) C(7) 108.5(4) . . . yes N(2) P(1) C(13) 105.3(4) . . . yes C(7) P(1) C(13) 106.5(4) . . . yes Pd(1) N(1) C(2) 119.8(7) . . . yes Pd(1) N(1) C(6) 122.6(7) . . . yes C(2) N(1) C(6) 117.1(9) . . . yes P(1) N(2) C(2) 119.1(6) . . . yes P(1) N(2) H(2) 122.7 . . . no C(2) N(2) H(2) 112.8 . . . no N(1) C(2) N(2) 114.2(8) . . . yes N(1) C(2) C(3) 123(1) . . . yes N(2) C(2) C(3) 122.7(9) . . . yes C(2) C(3) C(4) 118(1) . . . yes C(2) C(3) H(3) 121.7 . . . no C(4) C(3) H(3) 120.2 . . . no C(3) C(4) C(5) 119(1) . . . yes C(3) C(4) H(4) 122.0 . . . no C(5) C(4) H(4) 118.9 . . . no C(4) C(5) C(6) 120(1) . . . yes C(4) C(5) H(5) 119.5 . . . no C(6) C(5) H(5) 120.3 . . . no N(1) C(6) C(5) 122(1) . . . yes N(1) C(6) H(6) 118.6 . . . no C(5) C(6) H(6) 119.3 . . . no P(1) C(7) C(8) 120.5(7) . . . yes P(1) C(7) C(12) 119.7(8) . . . yes C(8) C(7) C(12) 119.7(9) . . . yes C(7) C(8) C(9) 120(1) . . . yes C(7) C(8) H(8) 120.0 . . . no C(9) C(8) H(8) 119.9 . . . no C(8) C(9) C(10) 120(1) . . . yes C(8) C(9) H(9) 120.1 . . . no C(10) C(9) H(9) 120.1 . . . no C(9) C(10) C(11) 121(1) . . . yes C(9) C(10) H(10) 119.6 . . . no C(11) C(10) H(10) 119.4 . . . no C(10) C(11) C(12) 119(1) . . . yes C(10) C(11) H(11) 120.4 . . . no C(12) C(11) H(11) 120.6 . . . no C(7) C(12) C(11) 120(1) . . . yes C(7) C(12) H(12) 119.8 . . . no C(11) C(12) H(12) 120.0 . . . no P(1) C(13) C(14) 120.4(7) . . . yes P(1) C(13) C(18) 121.3(8) . . . yes C(14) C(13) C(18) 117.9(9) . . . yes C(13) C(14) C(15) 121(1) . . . yes C(13) C(14) H(14) 119.3 . . . no C(15) C(14) H(14) 119.4 . . . no C(14) C(15) C(16) 119(1) . . . yes C(14) C(15) H(15) 120.7 . . . no C(16) C(15) H(15) 120.7 . . . no C(15) C(16) C(17) 122(1) . . . yes C(15) C(16) H(16) 118.6 . . . no C(17) C(16) H(16) 119.8 . . . no C(16) C(17) C(18) 120(1) . . . yes C(16) C(17) H(17) 119.4 . . . no C(18) C(17) H(17) 120.6 . . . no C(13) C(18) C(17) 121(1) . . . yes C(13) C(18) H(18) 119.8 . . . no C(17) C(18) H(18) 119.7 . . . no F(1) B(1) F(2) 110(2) . . . yes F(1) B(1) F(3) 111(1) . . . yes F(1) B(1) F(4) 111(1) . . . yes F(2) B(1) F(3) 103(1) . . . yes F(2) B(1) F(4) 109(2) . . . yes F(3) B(1) F(4) 113(1) . . . yes #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd(1) F(1) 3.168(9) . 11_554 no Pd(1) F(1) 3.168(9) . 12_454 no F(1) N(1) 3.07(1) . 15_545 no F(1) C(2) 3.28(1) . 15_545 no F(1) N(2) 3.29(1) . 15_545 no F(1) C(6) 3.34(1) . 4 no F(1) C(18) 3.37(2) . 15_545 no F(1) N(1) 3.58(1) . 4 no F(2) C(3) 3.20(2) . . no F(2) C(11) 3.52(2) . 10_554 no F(2) C(6) 3.54(2) . 4 no F(2) N(2) 3.55(1) . . no F(3) N(2) 2.95(1) . . no F(3) C(6) 3.45(1) . 4 no F(4) C(4) 3.25(2) . 10 no F(4) C(16) 3.33(2) . 12_454 no F(4) C(17) 3.45(2) . 12_454 no C(10) C(15) 3.28(2) . 12_454 no C(10) C(16) 3.51(2) . 12_454 no C(11) C(16) 3.51(2) . 12_454 no #----------------------------------------------------------------------- loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(2)' 'H(2)' 'F(3)' '0.73' '2.24' '2.95(1)' '163.0' '.' #---end data_17 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C17 H15 Au Cl N2 P' _chemical_formula_structural 'C17 H15 Au Cl N2 P' _chemical_formula_analytical 'C17 H15 Au Cl N2 P' _chemical_formula_sum 'C17 H15 Au Cl N2 P' _chemical_formula_weight 510.70 _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' '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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.42620(10) _cell_length_b 18.80220(10) _cell_length_c 10.16510(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.7120(10) _cell_angle_gamma 90.00 _cell_volume 1685.16(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.013 _exptl_crystal_density_method - _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 8.980 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.585192 _exptl_absorpt_correction_T_max 1.0000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 7247 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 23.29 _reflns_number_total 2431 _reflns_number_observed 2097 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 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^)+(0.0411P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2381 _refine_ls_number_parameters 216 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_obs 0.0212 _refine_ls_wR_factor_all 0.0633 _refine_ls_wR_factor_obs 0.0516 _refine_ls_goodness_of_fit_all 0.893 _refine_ls_goodness_of_fit_obs 0.928 _refine_ls_restrained_S_all 1.062 _refine_ls_restrained_S_obs 0.928 _refine_ls_shift/esd_max -1.855 _refine_ls_shift/esd_mean 0.123 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 Au1 Au 0.49386(2) -0.094953(9) -0.34460(2) 0.04403(11) Uani 1 d . . Cl1 Cl 0.2845(2) -0.03669(8) -0.48926(15) 0.0725(4) Uani 1 d . . N1 N 0.5048(5) -0.2659(2) -0.3719(4) 0.0577(11) Uani 1 d . . C2 C 0.5426(6) -0.2801(3) -0.2350(5) 0.0542(12) Uani 1 d . . C3 C 0.4887(7) -0.3384(3) -0.1835(6) 0.070(2) Uani 1 d . . H3A H 0.5199(7) -0.3470(3) -0.0874(6) 0.085 Uiso 1 calc R . C4 C 0.3906(9) -0.3821(4) -0.2756(9) 0.089(2) Uani 1 d . . H4A H 0.3543(9) -0.4220(4) -0.2437(9) 0.106 Uiso 1 calc R . C5 C 0.3441(7) -0.3681(3) -0.4156(8) 0.082(2) Uani 1 d . . H5A H 0.2741(7) -0.3976(3) -0.4797(8) 0.099 Uiso 1 calc R . C6 C 0.4016(6) -0.3097(3) -0.4620(6) 0.0632(14) Uani 1 d . . H6A H 0.3685(6) -0.3002(3) -0.5579(6) 0.076 Uiso 1 calc R . N2 N 0.6437(5) -0.2325(2) -0.1427(4) 0.0589(11) Uani 1 d D . H2N H 0.6563(90) -0.2450(43) -0.0457(29) 0.140(29) Uiso 1 d D . P1 P 0.68988(14) -0.15441(6) -0.19883(12) 0.0462(3) Uani 1 d . . C7 C 0.8407(6) -0.1750(3) -0.2626(5) 0.0565(13) Uani 1 d . . C8 C 0.8718(6) -0.1295(3) -0.3550(6) 0.0663(14) Uani 1 d . . H8A H 0.8103(6) -0.0901(3) -0.3898(6) 0.080 Uiso 1 calc R . C9 C 0.9949(8) -0.1424(5) -0.3965(8) 0.094(2) Uani 1 d . . H9A H 1.0160(8) -0.1120(5) -0.4594(8) 0.113 Uiso 1 calc R . C10 C 1.0852(9) -0.2007(7) -0.3435(10) 0.125(4) Uani 1 d . . H10A H 1.1693(9) -0.2090(7) -0.3690(10) 0.149 Uiso 1 calc R . C11 C 1.0533(11) -0.2455(6) -0.2556(9) 0.141(4) Uani 1 d . . H11A H 1.1156(11) -0.2847(6) -0.2211(9) 0.169 Uiso 1 calc R . C12 C 0.9301(8) -0.2347(4) -0.2153(7) 0.099(2) Uani 1 d . . H12A H 0.9071(8) -0.2673(4) -0.1569(7) 0.119 Uiso 1 calc R . C13 C 0.7782(5) -0.1085(2) -0.0345(5) 0.0516(12) Uani 1 d G . C14 C 0.6847(6) -0.0762(3) 0.0273(7) 0.080(2) Uani 1 d G . H14A H 0.5801(10) -0.0779(31) -0.0181(29) 0.096 Uiso 1 calc R . C15 C 0.7444(8) -0.0417(4) 0.1543(7) 0.086(2) Uani 1 d G . H15A H 0.6797(8) -0.0209(4) 0.1941(7) 0.103 Uiso 1 calc R . C16 C 0.8939(8) -0.0376(4) 0.2210(6) 0.091(2) Uani 1 d G . H16A H 0.9347(8) -0.0141(4) 0.3066(6) 0.109 Uiso 1 calc R . C17 C 0.9815(9) -0.0678(9) 0.1622(12) 0.228(9) Uani 1 d G . H17A H 1.0861(9) -0.0653(9) 0.2072(12) 0.273 Uiso 1 calc R . C18 C 0.9231(9) -0.1038(7) 0.0343(10) 0.177(6) Uani 1 d G . H18A H 0.9898(9) -0.1250(7) -0.0029(10) 0.212 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 Au1 0.04510(15) 0.04462(15) 0.03740(14) -0.00061(7) 0.00843(9) 0.00506(7) Cl1 0.0583(8) 0.0927(10) 0.0576(8) 0.0073(7) 0.0095(6) 0.0295(7) N1 0.082(3) 0.049(2) 0.040(2) -0.001(2) 0.018(2) -0.009(2) C2 0.076(3) 0.046(3) 0.045(3) 0.002(2) 0.027(3) 0.003(3) C3 0.092(4) 0.065(4) 0.067(3) 0.009(3) 0.044(3) -0.004(3) C4 0.107(5) 0.078(4) 0.108(6) 0.003(4) 0.071(5) -0.026(4) C5 0.071(4) 0.077(4) 0.113(6) -0.030(4) 0.050(4) -0.025(3) C6 0.073(4) 0.067(3) 0.053(3) -0.015(3) 0.026(3) -0.014(3) N2 0.093(3) 0.044(2) 0.035(2) 0.005(2) 0.016(2) 0.006(2) P1 0.0539(7) 0.0448(6) 0.0336(6) -0.0006(5) 0.0078(5) 0.0078(5) C7 0.057(3) 0.068(3) 0.036(2) -0.011(2) 0.005(2) 0.016(3) C8 0.067(3) 0.068(3) 0.066(4) -0.011(3) 0.027(3) -0.002(3) C9 0.082(5) 0.134(7) 0.078(4) -0.036(5) 0.041(4) -0.023(5) C10 0.069(5) 0.217(11) 0.083(6) -0.062(6) 0.021(4) 0.041(6) C11 0.131(7) 0.212(11) 0.077(5) 0.003(6) 0.035(5) 0.111(8) C12 0.116(5) 0.117(6) 0.062(4) 0.014(4) 0.028(4) 0.071(5) C13 0.057(3) 0.050(3) 0.038(3) -0.006(2) 0.005(2) 0.007(2) C14 0.059(4) 0.100(4) 0.086(5) -0.040(4) 0.030(3) -0.020(3) C15 0.086(5) 0.104(5) 0.074(4) -0.042(4) 0.037(4) -0.010(4) C16 0.087(5) 0.117(5) 0.048(3) -0.034(3) -0.001(3) 0.018(4) C17 0.061(5) 0.426(20) 0.136(10) -0.179(13) -0.039(6) 0.059(8) C18 0.057(4) 0.321(15) 0.114(7) -0.143(9) -0.015(5) 0.054(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2187(11) . ? Au1 Cl1 2.2813(12) . ? N1 C2 1.336(6) . ? N1 C6 1.354(6) . ? C2 N2 1.399(7) . ? C2 C3 1.387(7) . ? C3 C4 1.338(9) . ? C4 C5 1.359(10) . ? C5 C6 1.378(8) . ? N2 P1 1.687(4) . ? P1 C7 1.801(5) . ? P1 C13 1.801(5) . ? C7 C8 1.377(8) . ? C7 C12 1.385(8) . ? C8 C9 1.389(8) . ? C9 C10 1.375(12) . ? C10 C11 1.338(14) . ? C11 C12 1.376(12) . ? C13 C14 1.39 . ? C13 C18 1.298(9) . ? C14 C15 1.375(8) . ? C15 C16 1.332(9) . ? C16 C17 1.308(10) . ? C17 C18 1.395(11) . ? 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 P1 Au1 Cl1 177.04(5) . . ? C2 N1 C6 116.4(4) . . ? N1 C2 N2 116.0(4) . . ? N1 C2 C3 123.6(5) . . ? N2 C2 C3 120.4(5) . . ? C4 C3 C2 118.4(6) . . ? C3 C4 C5 120.0(6) . . ? C4 C5 C6 119.5(6) . . ? N1 C6 C5 121.9(5) . . ? C2 N2 P1 121.7(3) . . ? N2 P1 C7 105.4(2) . . ? N2 P1 C13 101.1(2) . . ? C7 P1 C13 105.8(2) . . ? N2 P1 Au1 114.3(2) . . ? C7 P1 Au1 116.4(2) . . ? C13 P1 Au1 112.38(15) . . ? C8 C7 C12 119.4(6) . . ? C8 C7 P1 119.9(4) . . ? C12 C7 P1 120.7(5) . . ? C7 C8 C9 120.1(6) . . ? C10 C9 C8 119.2(8) . . ? C11 C10 C9 120.7(7) . . ? C10 C11 C12 121.2(8) . . ? C11 C12 C7 119.4(8) . . ? C14 C13 C18 116.2(5) . . ? C14 C13 P1 118.0(4) . . ? C18 C13 P1 125.8(4) . . ? C15 C14 C13 121.1(5) . . ? C14 C15 C16 120.8(6) . . ? C17 C16 C15 117.9(6) . . ? C16 C17 C18 122.1(7) . . ? C17 C18 C13 121.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 N2 -177.0(4) . . . . ? C6 N1 C2 C3 3.7(8) . . . . ? N1 C2 C3 C4 -1.6(9) . . . . ? N2 C2 C3 C4 179.1(6) . . . . ? C2 C3 C4 C5 -1.2(10) . . . . ? C3 C4 C5 C6 1.6(10) . . . . ? C2 N1 C6 C5 -3.2(8) . . . . ? C4 C5 C6 N1 0.6(9) . . . . ? N1 C2 N2 P1 10.7(7) . . . . ? C3 C2 N2 P1 -170.0(4) . . . . ? C2 N2 P1 C7 -84.3(4) . . . . ? C2 N2 P1 C13 165.7(4) . . . . ? C2 N2 P1 Au1 44.8(4) . . . . ? Cl1 Au1 P1 N2 26.4(10) . . . . ? Cl1 Au1 P1 C7 149.7(9) . . . . ? Cl1 Au1 P1 C13 -88.1(9) . . . . ? N2 P1 C7 C8 159.2(4) . . . . ? C13 P1 C7 C8 -94.1(4) . . . . ? Au1 P1 C7 C8 31.4(5) . . . . ? N2 P1 C7 C12 -23.3(5) . . . . ? C13 P1 C7 C12 83.3(5) . . . . ? Au1 P1 C7 C12 -151.1(4) . . . . ? C12 C7 C8 C9 -2.2(8) . . . . ? P1 C7 C8 C9 175.3(4) . . . . ? C7 C8 C9 C10 -0.4(9) . . . . ? C8 C9 C10 C11 1.6(12) . . . . ? C9 C10 C11 C12 -0.2(14) . . . . ? C10 C11 C12 C7 -2.4(13) . . . . ? C8 C7 C12 C11 3.5(10) . . . . ? P1 C7 C12 C11 -173.9(6) . . . . ? N2 P1 C13 C14 -80.5(5) . . . . ? C7 P1 C13 C14 169.8(5) . . . . ? Au1 P1 C13 C14 41.8(5) . . . . ? N2 P1 C13 C18 98.1(9) . . . . ? C7 P1 C13 C18 -11.6(9) . . . . ? Au1 P1 C13 C18 -139.6(8) . . . . ? C18 C13 C14 C15 -0.3(12) . . . . ? P1 C13 C14 C15 178.5(5) . . . . ? C13 C14 C15 C16 0.7(12) . . . . ? C14 C15 C16 C17 -0.4(15) . . . . ? C15 C16 C17 C18 -0.4(22) . . . . ? C16 C17 C18 C13 0.8(25) . . . . ? C14 C13 C18 C17 -0.5(18) . . . . ? P1 C13 C18 C17 -179.1(11) . . . . ? _refine_diff_density_max 0.839 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.081 #---end data_19 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C26 H29 N2 O P Pt.H2 O ' _chemical_formula_structural 'C26 H31 N2 O2 P Pt' _chemical_formula_analytical 'C26 H31 N2 O2 P Pt' _chemical_formula_sum 'C26 H31 N2 O2 P Pt' _chemical_formula_weight 629.59 _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' 'Pt' 'Pt' -1.7033 8.3905 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6006(7) _cell_length_b 9.9187(7) _cell_length_c 13.3323(9) _cell_angle_alpha 100.1220(10) _cell_angle_beta 100.3670(10) _cell_angle_gamma 98.1210(10) _cell_volume 1209.66(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 78 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max .1 _exptl_crystal_size_mid .06 _exptl_crystal_size_min .05 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method - _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 5.891 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.704006 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 5390 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3396 _reflns_number_observed 3011 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 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^)+(0.0231P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3346 _refine_ls_number_parameters 298 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_obs 0.0204 _refine_ls_wR_factor_all 0.0497 _refine_ls_wR_factor_obs 0.0444 _refine_ls_goodness_of_fit_all 0.986 _refine_ls_goodness_of_fit_obs 1.019 _refine_ls_restrained_S_all 1.075 _refine_ls_restrained_S_obs 1.019 _refine_ls_shift/esd_max -0.005 _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 0.05656(2) 0.78052(2) 0.175651(13) 0.03153(8) Uani 1 d . . P1 P 0.28810(11) 0.83727(11) 0.17286(8) 0.0305(2) Uani 1 d . . N1 N 0.0394(4) 0.8193(3) 0.0220(3) 0.0347(8) Uani 1 d . . C2 C 0.1669(5) 0.8529(4) -0.0094(3) 0.0340(10) Uani 1 d . . N2 N 0.2958(4) 0.8667(4) 0.0560(3) 0.0356(8) Uani 1 d . . C3 C 0.1621(5) 0.8745(4) -0.1119(3) 0.0415(11) Uani 1 d . . H3A H 0.2469(5) 0.8966(4) -0.1346(3) 0.050 Uiso 1 calc R . C4 C 0.0298(6) 0.8625(5) -0.1783(4) 0.0505(13) Uani 1 d . . H4A H 0.0262(6) 0.8761(5) -0.2460(4) 0.061 Uiso 1 calc R . C5 C -0.0965(5) 0.8305(5) -0.1448(4) 0.0495(12) Uani 1 d . . H5A H -0.1854(5) 0.8227(5) -0.1888(4) 0.059 Uiso 1 calc R . C6 C -0.0872(5) 0.8106(5) -0.0455(4) 0.0436(11) Uani 1 d . . H6A H -0.1723(5) 0.7899(5) -0.0227(4) 0.052 Uiso 1 calc R . C7 C 0.3974(4) 0.9837(4) 0.2696(3) 0.0337(10) Uani 1 d . . C8 C 0.5421(5) 1.0240(5) 0.2691(4) 0.0484(12) Uani 1 d . . H8A H 0.5827(5) 0.9760(5) 0.2186(4) 0.058 Uiso 1 calc R . C9 C 0.6258(6) 1.1348(5) 0.3428(4) 0.0610(15) Uani 1 d . . H9A H 0.7218(6) 1.1625(5) 0.3409(4) 0.073 Uiso 1 calc R . C10 C 0.5678(6) 1.2040(5) 0.4187(4) 0.0597(15) Uani 1 d . . H10A H 0.6254(6) 1.2764(5) 0.4697(4) 0.072 Uiso 1 calc R . C11 C 0.4238(6) 1.1666(5) 0.4198(4) 0.0566(14) Uani 1 d . . H11A H 0.3844(6) 1.2155(5) 0.4706(4) 0.068 Uiso 1 calc R . C12 C 0.3381(5) 1.0568(5) 0.3458(4) 0.0440(11) Uani 1 d . . H12A H 0.2414(5) 1.0318(5) 0.3469(4) 0.053 Uiso 1 calc R . C13 C 0.3815(4) 0.6942(4) 0.1931(3) 0.0324(10) Uani 1 d . . C14 C 0.3826(5) 0.5906(5) 0.1084(4) 0.0448(12) Uani 1 d . . H14A H 0.3490(5) 0.6023(5) 0.0411(4) 0.054 Uiso 1 calc R . C15 C 0.4331(6) 0.4704(5) 0.1233(4) 0.0541(13) Uani 1 d . . H15A H 0.4328(6) 0.4014(5) 0.0661(4) 0.065 Uiso 1 calc R . C16 C 0.4834(5) 0.4525(5) 0.2216(4) 0.0526(13) Uani 1 d . . H16A H 0.5164(5) 0.3709(5) 0.2313(4) 0.063 Uiso 1 calc R . C17 C 0.4854(5) 0.5549(5) 0.3065(4) 0.0532(13) Uani 1 d . . H17A H 0.5203(5) 0.5432(5) 0.3736(4) 0.064 Uiso 1 calc R . C18 C 0.4355(5) 0.6751(5) 0.2913(4) 0.0434(11) Uani 1 d . . H18A H 0.4383(5) 0.7446(5) 0.3488(4) 0.052 Uiso 1 calc R . C19 C -0.1596(5) 0.6383(5) 0.1420(4) 0.0464(12) Uani 1 d . . H19A H -0.1628(5) 0.6386(5) 0.0719(4) 0.056 Uiso 1 calc R . C20 C -0.1750(5) 0.7619(6) 0.2000(4) 0.0533(13) Uani 1 d . . H20A H -0.1921(5) 0.8328(6) 0.1646(4) 0.064 Uiso 1 calc R . C21 C -0.1665(6) 0.7933(6) 0.3175(4) 0.064(2) Uani 1 d . . H21A H -0.2259(6) 0.7172(6) 0.3352(4) 0.077 Uiso 1 calc R . H21B H -0.2063(6) 0.8767(6) 0.3355(4) 0.077 Uiso 1 calc R . C22 C -0.0139(5) 0.8142(5) 0.3833(4) 0.0494(12) Uani 1 d . . H22A H 0.0241(5) 0.9132(5) 0.4051(4) 0.059 Uiso 1 calc R . H22B H -0.0182(5) 0.7771(5) 0.4456(4) 0.059 Uiso 1 calc R . C23 C 0.0879(5) 0.7440(5) 0.3251(3) 0.0407(11) Uani 1 d . . H23A H 0.1862(5) 0.7894(5) 0.3605(3) 0.049 Uiso 1 calc R . C24 C 0.0780(5) 0.5890(4) 0.3231(3) 0.0387(11) Uani 1 d . . H24A H 0.1394(5) 0.5521(4) 0.2775(3) 0.046 Uiso 1 calc R . O24 O 0.1360(4) 0.5760(3) 0.4283(2) 0.0526(9) Uani 1 d . . C25 C -0.0727(5) 0.5031(5) 0.2857(4) 0.0477(12) Uani 1 d . . H25A H -0.1345(5) 0.5398(5) 0.3298(4) 0.057 Uiso 1 calc R . H25B H -0.0693(5) 0.4080(5) 0.2931(4) 0.057 Uiso 1 calc R . C26 C -0.1384(5) 0.5028(5) 0.1722(4) 0.0500(12) Uani 1 d . . H26A H -0.0780(5) 0.4610(5) 0.1292(4) 0.060 Uiso 1 calc R . H26B H -0.2315(5) 0.4419(5) 0.1539(4) 0.060 Uiso 1 calc R . C27 C 0.1713(7) 0.4440(6) 0.4358(5) 0.070(2) Uani 1 d . . H27A H 0.2089(7) 0.4430(6) 0.5074(5) 0.105 Uiso 1 calc R . H27B H 0.2424(7) 0.4255(6) 0.3954(5) 0.105 Uiso 1 calc R . H27C H 0.0865(7) 0.3738(6) 0.4096(5) 0.105 Uiso 1 calc R . O30 O 0.5698(4) 0.8511(4) -0.0128(4) 0.0686(11) Uani 1 d D . H30A H 0.6041(63) 0.9347(36) -0.0372(44) 0.092(20) Uiso 1 d D . H30B H 0.4712(23) 0.8568(61) -0.0050(48) 0.095(21) Uiso 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02599(11) 0.03403(11) 0.03340(11) 0.00886(7) 0.00272(7) 0.00363(7) P1 0.0277(6) 0.0338(6) 0.0281(6) 0.0064(5) 0.0022(5) 0.0034(5) N1 0.030(2) 0.036(2) 0.035(2) 0.010(2) -0.001(2) 0.004(2) C2 0.042(3) 0.027(2) 0.029(2) 0.002(2) 0.002(2) 0.004(2) N2 0.030(2) 0.043(2) 0.032(2) 0.012(2) 0.000(2) 0.004(2) C3 0.053(3) 0.038(2) 0.032(2) 0.012(2) 0.003(2) 0.007(2) C4 0.074(4) 0.046(3) 0.029(2) 0.013(2) -0.001(2) 0.012(3) C5 0.047(3) 0.053(3) 0.044(3) 0.016(2) -0.012(2) 0.012(2) C6 0.034(3) 0.046(3) 0.047(3) 0.015(2) -0.006(2) 0.008(2) C7 0.030(2) 0.033(2) 0.034(2) 0.009(2) -0.003(2) -0.001(2) C8 0.041(3) 0.049(3) 0.050(3) 0.002(2) 0.006(2) 0.003(2) C9 0.044(3) 0.055(3) 0.069(4) 0.007(3) -0.006(3) -0.010(3) C10 0.069(4) 0.051(3) 0.044(3) 0.004(3) -0.012(3) -0.005(3) C11 0.067(4) 0.051(3) 0.043(3) -0.005(2) 0.003(3) 0.011(3) C12 0.042(3) 0.044(3) 0.044(3) 0.007(2) 0.005(2) 0.008(2) C13 0.023(2) 0.037(2) 0.036(2) 0.011(2) 0.003(2) 0.000(2) C14 0.048(3) 0.045(3) 0.038(3) 0.007(2) 0.001(2) 0.011(2) C15 0.059(3) 0.038(3) 0.062(3) 0.004(3) 0.007(3) 0.016(3) C16 0.041(3) 0.045(3) 0.077(4) 0.024(3) 0.011(3) 0.014(2) C17 0.049(3) 0.066(3) 0.050(3) 0.030(3) 0.003(2) 0.016(3) C18 0.036(3) 0.055(3) 0.035(3) 0.010(2) -0.002(2) 0.007(2) C19 0.032(3) 0.052(3) 0.049(3) 0.018(2) -0.004(2) -0.008(2) C20 0.035(3) 0.060(3) 0.071(4) 0.026(3) 0.010(2) 0.011(2) C21 0.062(4) 0.062(3) 0.084(4) 0.020(3) 0.040(3) 0.023(3) C22 0.051(3) 0.048(3) 0.048(3) 0.006(2) 0.017(2) 0.001(2) C23 0.035(3) 0.047(3) 0.038(3) 0.008(2) 0.010(2) -0.001(2) C24 0.041(3) 0.043(3) 0.036(2) 0.017(2) 0.009(2) 0.007(2) O24 0.060(2) 0.057(2) 0.041(2) 0.023(2) -0.002(2) 0.007(2) C25 0.050(3) 0.041(3) 0.052(3) 0.017(2) 0.005(2) 0.006(2) C26 0.045(3) 0.049(3) 0.051(3) 0.013(2) 0.002(2) -0.003(2) C27 0.070(4) 0.066(4) 0.075(4) 0.036(3) -0.001(3) 0.011(3) O30 0.062(3) 0.046(2) 0.110(3) 0.022(2) 0.038(2) 0.017(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 Pt1 C23 2.064(4) . ? Pt1 N1 2.132(3) . ? Pt1 P1 2.2233(11) . ? Pt1 C19 2.261(4) . ? Pt1 C20 2.290(5) . ? P1 N2 1.647(3) . ? P1 C7 1.816(4) . ? P1 C13 1.816(4) . ? N1 C6 1.358(5) . ? N1 C2 1.380(5) . ? C2 N2 1.354(5) . ? C2 C3 1.413(6) . ? C3 C4 1.388(7) . ? C4 C5 1.381(7) . ? C5 C6 1.361(6) . ? C7 C8 1.392(6) . ? C7 C12 1.396(6) . ? C8 C9 1.381(7) . ? C9 C10 1.367(8) . ? C10 C11 1.384(7) . ? C11 C12 1.383(6) . ? C13 C18 1.375(6) . ? C13 C14 1.390(6) . ? C14 C15 1.382(6) . ? C15 C16 1.364(7) . ? C16 C17 1.377(7) . ? C17 C18 1.379(7) . ? C19 C20 1.372(7) . ? C19 C26 1.499(7) . ? C20 C21 1.527(7) . ? C21 C22 1.532(7) . ? C22 C23 1.523(6) . ? C23 C24 1.523(6) . ? C24 O24 1.448(5) . ? C24 C25 1.520(6) . ? O24 C27 1.414(6) . ? C25 C26 1.531(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 C23 Pt1 N1 176.2(2) . . ? C23 Pt1 P1 96.43(13) . . ? N1 Pt1 P1 79.77(9) . . ? C23 Pt1 C19 87.8(2) . . ? N1 Pt1 C19 95.4(2) . . ? P1 Pt1 C19 155.68(14) . . ? C23 Pt1 C20 80.2(2) . . ? N1 Pt1 C20 103.6(2) . . ? P1 Pt1 C20 169.13(14) . . ? C19 Pt1 C20 35.1(2) . . ? N2 P1 C7 108.7(2) . . ? N2 P1 C13 108.4(2) . . ? C7 P1 C13 103.2(2) . . ? N2 P1 Pt1 106.97(13) . . ? C7 P1 Pt1 118.64(14) . . ? C13 P1 Pt1 110.60(13) . . ? C6 N1 C2 119.2(4) . . ? C6 N1 Pt1 124.3(3) . . ? C2 N1 Pt1 116.5(3) . . ? N2 C2 N1 121.4(4) . . ? N2 C2 C3 119.6(4) . . ? N1 C2 C3 119.0(4) . . ? C2 N2 P1 115.3(3) . . ? C4 C3 C2 119.5(4) . . ? C5 C4 C3 120.5(4) . . ? C6 C5 C4 118.2(4) . . ? N1 C6 C5 123.6(4) . . ? C8 C7 C12 119.0(4) . . ? C8 C7 P1 120.3(3) . . ? C12 C7 P1 120.7(3) . . ? C9 C8 C7 120.5(5) . . ? C10 C9 C8 120.1(5) . . ? C9 C10 C11 120.2(5) . . ? C12 C11 C10 120.3(5) . . ? C11 C12 C7 119.8(4) . . ? C18 C13 C14 118.2(4) . . ? C18 C13 P1 121.8(3) . . ? C14 C13 P1 119.5(3) . . ? C15 C14 C13 120.5(4) . . ? C16 C15 C14 120.3(5) . . ? C15 C16 C17 120.1(5) . . ? C16 C17 C18 119.5(5) . . ? C13 C18 C17 121.4(5) . . ? C20 C19 C26 131.0(5) . . ? C20 C19 Pt1 73.6(3) . . ? C26 C19 Pt1 108.9(3) . . ? C19 C20 C21 125.7(5) . . ? C19 C20 Pt1 71.3(3) . . ? C21 C20 Pt1 107.0(3) . . ? C20 C21 C22 114.3(4) . . ? C23 C22 C21 112.9(4) . . ? C24 C23 C22 115.0(4) . . ? C24 C23 Pt1 110.6(3) . . ? C22 C23 Pt1 109.2(3) . . ? O24 C24 C25 109.7(3) . . ? O24 C24 C23 106.7(3) . . ? C25 C24 C23 115.1(4) . . ? C27 O24 C24 114.1(4) . . ? C24 C25 C26 113.1(4) . . ? C19 C26 C25 118.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 Pt1 P1 N2 177.7(2) . . . . ? N1 Pt1 P1 N2 -1.7(2) . . . . ? C19 Pt1 P1 N2 78.7(3) . . . . ? C20 Pt1 P1 N2 -110.9(7) . . . . ? C23 Pt1 P1 C7 -59.1(2) . . . . ? N1 Pt1 P1 C7 121.5(2) . . . . ? C19 Pt1 P1 C7 -158.0(3) . . . . ? C20 Pt1 P1 C7 12.3(7) . . . . ? C23 Pt1 P1 C13 59.8(2) . . . . ? N1 Pt1 P1 C13 -119.6(2) . . . . ? C19 Pt1 P1 C13 -39.2(3) . . . . ? C20 Pt1 P1 C13 131.2(7) . . . . ? C23 Pt1 N1 C6 172.4(21) . . . . ? P1 Pt1 N1 C6 -178.6(3) . . . . ? C19 Pt1 N1 C6 25.5(4) . . . . ? C20 Pt1 N1 C6 -9.1(4) . . . . ? C23 Pt1 N1 C2 -6.4(23) . . . . ? P1 Pt1 N1 C2 2.6(3) . . . . ? C19 Pt1 N1 C2 -153.3(3) . . . . ? C20 Pt1 N1 C2 172.0(3) . . . . ? C6 N1 C2 N2 178.1(4) . . . . ? Pt1 N1 C2 N2 -3.0(5) . . . . ? C6 N1 C2 C3 -1.3(6) . . . . ? Pt1 N1 C2 C3 177.6(3) . . . . ? N1 C2 N2 P1 1.3(5) . . . . ? C3 C2 N2 P1 -179.3(3) . . . . ? C7 P1 N2 C2 -128.4(3) . . . . ? C13 P1 N2 C2 120.1(3) . . . . ? Pt1 P1 N2 C2 0.8(3) . . . . ? N2 C2 C3 C4 -178.9(4) . . . . ? N1 C2 C3 C4 0.4(6) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C3 C4 C5 C6 -0.3(7) . . . . ? C2 N1 C6 C5 1.4(7) . . . . ? Pt1 N1 C6 C5 -177.4(3) . . . . ? C4 C5 C6 N1 -0.6(7) . . . . ? N2 P1 C7 C8 -56.4(4) . . . . ? C13 P1 C7 C8 58.6(4) . . . . ? Pt1 P1 C7 C8 -178.8(3) . . . . ? N2 P1 C7 C12 124.1(4) . . . . ? C13 P1 C7 C12 -121.0(4) . . . . ? Pt1 P1 C7 C12 1.7(4) . . . . ? C12 C7 C8 C9 -0.1(7) . . . . ? P1 C7 C8 C9 -179.6(4) . . . . ? C7 C8 C9 C10 1.5(8) . . . . ? C8 C9 C10 C11 -2.3(8) . . . . ? C9 C10 C11 C12 1.6(8) . . . . ? C10 C11 C12 C7 -0.1(7) . . . . ? C8 C7 C12 C11 -0.6(7) . . . . ? P1 C7 C12 C11 178.9(4) . . . . ? N2 P1 C13 C18 157.8(3) . . . . ? C7 P1 C13 C18 42.7(4) . . . . ? Pt1 P1 C13 C18 -85.2(4) . . . . ? N2 P1 C13 C14 -30.9(4) . . . . ? C7 P1 C13 C14 -146.0(3) . . . . ? Pt1 P1 C13 C14 86.1(3) . . . . ? C18 C13 C14 C15 1.7(7) . . . . ? P1 C13 C14 C15 -169.9(4) . . . . ? C13 C14 C15 C16 -0.4(8) . . . . ? C14 C15 C16 C17 -0.7(8) . . . . ? C15 C16 C17 C18 0.4(7) . . . . ? C14 C13 C18 C17 -2.0(7) . . . . ? P1 C13 C18 C17 169.5(4) . . . . ? C16 C17 C18 C13 0.9(7) . . . . ? C23 Pt1 C19 C20 76.1(3) . . . . ? N1 Pt1 C19 C20 -106.0(3) . . . . ? P1 Pt1 C19 C20 176.8(3) . . . . ? C20 Pt1 C19 C20 0.0 . . . . ? C23 Pt1 C19 C26 -52.5(3) . . . . ? N1 Pt1 C19 C26 125.4(3) . . . . ? P1 Pt1 C19 C26 48.3(5) . . . . ? C20 Pt1 C19 C26 -128.5(5) . . . . ? C26 C19 C20 C21 3.3(8) . . . . ? Pt1 C19 C20 C21 -97.9(5) . . . . ? C26 C19 C20 Pt1 101.1(5) . . . . ? Pt1 C19 C20 Pt1 0.0 . . . . ? C23 Pt1 C20 C19 -100.2(3) . . . . ? N1 Pt1 C20 C19 79.9(3) . . . . ? P1 Pt1 C20 C19 -173.1(6) . . . . ? C19 Pt1 C20 C19 0.0 . . . . ? C23 Pt1 C20 C21 22.5(3) . . . . ? N1 Pt1 C20 C21 -157.4(3) . . . . ? P1 Pt1 C20 C21 -50.3(9) . . . . ? C19 Pt1 C20 C21 122.8(5) . . . . ? C19 C20 C21 C22 73.8(7) . . . . ? Pt1 C20 C21 C22 -5.1(5) . . . . ? C20 C21 C22 C23 -23.6(6) . . . . ? C21 C22 C23 C24 -81.6(5) . . . . ? C21 C22 C23 Pt1 43.5(5) . . . . ? N1 Pt1 C23 C24 -89.3(22) . . . . ? P1 Pt1 C23 C24 -98.2(3) . . . . ? C19 Pt1 C23 C24 57.8(3) . . . . ? C20 Pt1 C23 C24 92.3(3) . . . . ? N1 Pt1 C23 C22 143.1(21) . . . . ? P1 Pt1 C23 C22 134.2(3) . . . . ? C19 Pt1 C23 C22 -69.8(3) . . . . ? C20 Pt1 C23 C22 -35.3(3) . . . . ? C22 C23 C24 O24 -69.7(5) . . . . ? Pt1 C23 C24 O24 166.0(3) . . . . ? C22 C23 C24 C25 52.1(5) . . . . ? Pt1 C23 C24 C25 -72.2(4) . . . . ? C25 C24 O24 C27 71.0(5) . . . . ? C23 C24 O24 C27 -163.8(4) . . . . ? O24 C24 C25 C26 -176.1(4) . . . . ? C23 C24 C25 C26 63.8(5) . . . . ? C20 C19 C26 C25 -24.1(8) . . . . ? Pt1 C19 C26 C25 60.3(5) . . . . ? C24 C25 C26 C19 -60.6(6) . . . . ? _refine_diff_density_max 0.500 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.076 #---END data_20 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C20 H24 Cl5 N2 P2 Pt.Cl.C H Cl3' _chemical_formula_structural 'C21 H25 Cl5 N2 P2 Pt' _chemical_formula_analytical 'C21 H25 Cl5 N2 P2 Pt' _chemical_formula_sum 'C21 H25 Cl5 N2 P2 Pt' _chemical_formula_weight 739.71 _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' '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' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3444(3) _cell_length_b 15.4169(5) _cell_length_c 19.5595(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.0410(10) _cell_angle_gamma 90.00 _cell_volume 2755.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 121 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour clear _exptl_crystal_size_max .05 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method - _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 5.705 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.740343 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 22430 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3934 _reflns_number_observed 2899 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 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^)+(0.0590P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0074(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3884 _refine_ls_number_parameters 301 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_obs 0.0434 _refine_ls_wR_factor_all 0.1095 _refine_ls_wR_factor_obs 0.0883 _refine_ls_goodness_of_fit_all 0.942 _refine_ls_goodness_of_fit_obs 0.991 _refine_ls_restrained_S_all 1.053 _refine_ls_restrained_S_obs 1.004 _refine_ls_shift/esd_max 0.908 _refine_ls_shift/esd_mean 0.066 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 1.47917(3) 0.31730(2) 0.337560(15) 0.0406(2) Uani 1 d . . P1 P 1.5720(2) 0.30855(12) 0.24239(11) 0.0380(5) Uani 1 d . . Cl1 Cl 1.3978(3) 0.3369(2) 0.44283(12) 0.0729(7) Uani 1 d . . N1 N 1.6570(7) 0.4045(4) 0.3700(3) 0.046(2) Uani 1 d . . N2 N 1.7290(7) 0.3641(5) 0.2674(3) 0.047(2) Uani 1 d D . H2N H 1.8007(91) 0.3729(73) 0.2379(48) 0.118(41) Uiso 1 d D . C2 C 1.7528(8) 0.4117(5) 0.3282(4) 0.041(2) Uani 1 d . . C3 C 1.8744(9) 0.4666(5) 0.3457(5) 0.054(2) Uani 1 d . . H3A H 1.9407(9) 0.4714(5) 0.3164(5) 0.064 Uiso 1 calc R . C4 C 1.8940(10) 0.5134(6) 0.4068(5) 0.063(3) Uani 1 d . . H4A H 1.9749(10) 0.5495(6) 0.4193(5) 0.076 Uiso 1 calc R . C5 C 1.7970(11) 0.5072(6) 0.4486(5) 0.064(2) Uani 1 d . . H5A H 1.8095(11) 0.5395(6) 0.4896(5) 0.076 Uiso 1 calc R . C6 C 1.6784(10) 0.4520(6) 0.4300(4) 0.058(2) Uani 1 d . . H6A H 1.6117(10) 0.4473(6) 0.4590(4) 0.069 Uiso 1 calc R . C7 C 1.6334(8) 0.2039(5) 0.2172(4) 0.040(2) Uani 1 d . . C8 C 1.5738(11) 0.1650(6) 0.1534(5) 0.056(2) Uani 1 d . . H8A H 1.5002(11) 0.1925(6) 0.1215(5) 0.067 Uiso 1 calc R . C9 C 1.6264(12) 0.0835(6) 0.1381(6) 0.070(3) Uani 1 d . . H9A H 1.5889(12) 0.0571(6) 0.0953(6) 0.083 Uiso 1 calc R . C10 C 1.7325(12) 0.0433(6) 0.1859(6) 0.075(3) Uani 1 d . . H10A H 1.7666(12) -0.0106(6) 0.1752(6) 0.089 Uiso 1 calc R . C11 C 1.7913(11) 0.0810(6) 0.2506(6) 0.067(3) Uani 1 d . . H11A H 1.8630(11) 0.0527(6) 0.2831(6) 0.081 Uiso 1 calc R . C12 C 1.7403(10) 0.1607(6) 0.2647(5) 0.057(2) Uani 1 d . . H12A H 1.7785(10) 0.1867(6) 0.3076(5) 0.069 Uiso 1 calc R . C13 C 1.4742(9) 0.3597(5) 0.1644(4) 0.044(2) Uani 1 d . . C14 C 1.3366(9) 0.3977(5) 0.1609(4) 0.052(2) Uani 1 d . . H14A H 1.2930(9) 0.3953(5) 0.1995(4) 0.062 Uiso 1 calc R . C15 C 1.2657(10) 0.4384(6) 0.1011(5) 0.062(2) Uani 1 d . . H15A H 1.1742(10) 0.4630(6) 0.0994(5) 0.074 Uiso 1 calc R . C16 C 1.3281(10) 0.4432(6) 0.0434(5) 0.064(3) Uani 1 d . . H16A H 1.2783(10) 0.4702(6) 0.0029(5) 0.077 Uiso 1 calc R . C17 C 1.4670(11) 0.4073(6) 0.0461(5) 0.067(3) Uani 1 d . . H17A H 1.5104(11) 0.4116(6) 0.0075(5) 0.080 Uiso 1 calc R . C18 C 1.5397(9) 0.3656(6) 0.1058(4) 0.051(2) Uani 1 d . . H18A H 1.6315(9) 0.3414(6) 0.1073(4) 0.062 Uiso 1 calc R . P2 P 1.2986(3) 0.2189(2) 0.30549(13) 0.0617(7) Uani 1 d . . C19 C 1.2410(15) 0.1912(8) 0.2160(6) 0.109(5) Uani 1 d . . H19A H 1.1641(15) 0.1489(8) 0.2108(6) 0.164 Uiso 1 calc R . H19B H 1.3221(15) 0.1676(8) 0.1990(6) 0.164 Uiso 1 calc R . H19C H 1.2056(15) 0.2422(8) 0.1896(6) 0.164 Uiso 1 calc R . C20 C 1.3875(30) 0.1026(17) 0.3249(14) 0.109(8) Uiso 0.50 d P 1 H20A H 1.4711(30) 0.0979(17) 0.3038(14) 0.164 Uiso 0.50 calc PR 1 H20B H 1.3170(30) 0.0591(17) 0.3058(14) 0.164 Uiso 0.50 calc PR 1 H20C H 1.4174(30) 0.0946(17) 0.3745(14) 0.164 Uiso 0.50 calc PR 1 C21 C 1.1577(35) 0.2166(22) 0.3460(17) 0.130(10) Uiso 0.50 d P 1 H21A H 1.1913(35) 0.2316(22) 0.3943(17) 0.195 Uiso 0.50 calc PR 1 H21B H 1.1163(35) 0.1594(22) 0.3427(17) 0.195 Uiso 0.50 calc PR 1 H21C H 1.0847(35) 0.2575(22) 0.3243(17) 0.195 Uiso 0.50 calc PR 1 C20' C 1.3158(20) 0.1330(12) 0.3654(9) 0.060(5) Uiso 0.50 d P 2 H20D H 1.3475(20) 0.1552(12) 0.4120(9) 0.090 Uiso 0.50 calc PR 2 H20E H 1.3863(20) 0.0922(12) 0.3557(9) 0.090 Uiso 0.50 calc PR 2 H20F H 1.2228(20) 0.1048(12) 0.3614(9) 0.090 Uiso 0.50 calc PR 2 C21' C 1.1175(18) 0.2734(12) 0.3134(9) 0.049(4) Uiso 0.50 d P 2 H21D H 1.0990(18) 0.3219(12) 0.2820(9) 0.074 Uiso 0.50 calc PR 2 H21E H 1.1242(18) 0.2932(12) 0.3605(9) 0.074 Uiso 0.50 calc PR 2 H21F H 1.0390(18) 0.2324(12) 0.3016(9) 0.074 Uiso 0.50 calc PR 2 Cl2 Cl 1.9356(3) 0.4208(2) 0.17053(15) 0.0943(10) Uani 1 d . . C50 C 0.9432(7) 0.2961(4) 0.0316(4) 0.102(4) Uani 1 d D . Cl3 Cl 1.0939(4) 0.2342(2) 0.0178(2) 0.1073(11) Uani 1 d D . Cl4 Cl 0.9518(16) 0.3784(6) -0.0328(5) 0.184(6) Uani 0.50 d PD . Cl5 Cl 0.8409(9) 0.2117(4) 0.0644(6) 0.140(4) Uani 0.50 d PD . Cl6 Cl 0.7669(9) 0.2655(9) -0.0134(7) 0.162(5) Uani 0.50 d PD . Cl7 Cl 0.8684(33) 0.3528(15) -0.0465(6) 0.453(28) Uani 0.50 d PD . 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 0.0404(2) 0.0481(2) 0.0357(2) -0.0005(2) 0.01363(14) -0.0027(2) P1 0.0375(11) 0.0390(11) 0.0399(11) -0.0040(9) 0.0139(9) -0.0045(9) Cl1 0.078(2) 0.100(2) 0.0500(13) -0.0097(13) 0.0355(13) -0.0174(15) N1 0.055(4) 0.044(4) 0.041(4) -0.003(3) 0.019(3) 0.000(3) N2 0.040(4) 0.055(4) 0.052(4) -0.022(4) 0.021(3) -0.007(3) C2 0.033(4) 0.035(4) 0.051(5) 0.000(4) 0.002(4) 0.003(4) C3 0.047(5) 0.044(5) 0.070(6) -0.003(5) 0.012(4) -0.009(4) C4 0.050(6) 0.056(6) 0.073(7) -0.005(5) -0.012(5) -0.007(5) C5 0.080(7) 0.051(6) 0.053(5) -0.010(5) 0.000(5) -0.013(5) C6 0.069(6) 0.061(6) 0.044(5) 0.000(5) 0.014(4) 0.017(5) C7 0.038(5) 0.039(5) 0.047(5) -0.002(4) 0.016(4) -0.003(4) C8 0.063(6) 0.060(6) 0.045(5) -0.010(5) 0.011(4) 0.004(5) C9 0.084(7) 0.049(6) 0.079(7) -0.022(6) 0.022(6) -0.001(6) C10 0.083(8) 0.035(5) 0.117(9) 0.004(6) 0.047(7) 0.011(5) C11 0.067(7) 0.049(6) 0.083(7) 0.010(6) 0.010(6) 0.009(5) C12 0.061(6) 0.054(6) 0.056(6) 0.004(5) 0.011(5) 0.005(5) C13 0.044(5) 0.038(4) 0.055(5) -0.002(4) 0.023(4) 0.002(4) C14 0.057(6) 0.051(5) 0.052(5) 0.008(4) 0.024(4) 0.003(4) C15 0.057(6) 0.058(6) 0.076(6) 0.018(5) 0.027(5) 0.008(5) C16 0.068(6) 0.068(6) 0.057(6) 0.023(5) 0.015(5) 0.008(5) C17 0.079(7) 0.070(6) 0.061(6) 0.015(5) 0.039(5) 0.007(6) C18 0.056(5) 0.057(5) 0.047(5) 0.003(5) 0.022(4) 0.009(5) P2 0.059(2) 0.078(2) 0.0510(14) 0.0060(14) 0.0173(12) -0.0212(14) C19 0.112(10) 0.137(12) 0.080(8) -0.030(8) 0.024(7) -0.087(9) Cl2 0.085(2) 0.118(2) 0.097(2) -0.053(2) 0.060(2) -0.057(2) C50 0.119(11) 0.092(9) 0.099(9) -0.030(8) 0.034(8) 0.009(8) Cl3 0.143(3) 0.080(2) 0.109(2) 0.012(2) 0.047(2) 0.037(2) Cl4 0.255(12) 0.122(7) 0.112(10) -0.032(6) -0.108(8) 0.095(8) Cl5 0.097(5) 0.078(4) 0.273(13) -0.051(6) 0.105(7) -0.019(4) Cl6 0.108(6) 0.196(11) 0.180(10) -0.102(9) 0.025(7) -0.020(7) Cl7 0.694(56) 0.473(40) 0.079(7) -0.086(15) -0.178(20) 0.489(40) _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 N1 2.129(7) . ? Pt1 P1 2.216(2) . ? Pt1 P2 2.258(3) . ? Pt1 Cl1 2.358(2) . ? P1 N2 1.681(7) . ? P1 C13 1.790(8) . ? P1 C7 1.814(8) . ? N1 C2 1.337(9) . ? N1 C6 1.361(10) . ? N2 C2 1.376(10) . ? C2 C3 1.401(11) . ? C3 C4 1.374(12) . ? C4 C5 1.346(12) . ? C5 C6 1.385(12) . ? C7 C8 1.391(11) . ? C7 C12 1.386(12) . ? C8 C9 1.403(12) . ? C9 C10 1.362(14) . ? C10 C11 1.397(14) . ? C11 C12 1.367(12) . ? C13 C14 1.402(11) . ? C13 C18 1.411(10) . ? C14 C15 1.371(12) . ? C15 C16 1.375(12) . ? C16 C17 1.402(13) . ? C17 C18 1.381(12) . ? P2 C21 1.67(3) . ? P2 C20' 1.75(2) . ? P2 C19 1.774(11) . ? P2 C21' 1.92(2) . ? P2 C20 1.98(3) . ? C50 Cl7 1.772(5) . ? C50 Cl6 1.763(5) . ? C50 Cl3 1.768(5) . ? C50 Cl4 1.802(5) . ? C50 Cl5 1.809(5) . ? Cl4 Cl7 0.86(3) . ? Cl5 Cl6 1.74(2) . ? Cl6 Cl7 1.84(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 N1 Pt1 P1 82.6(2) . . ? N1 Pt1 P2 176.9(2) . . ? P1 Pt1 P2 97.27(8) . . ? N1 Pt1 Cl1 91.9(2) . . ? P1 Pt1 Cl1 174.44(8) . . ? P2 Pt1 Cl1 88.29(9) . . ? N2 P1 C13 106.4(4) . . ? N2 P1 C7 103.0(3) . . ? C13 P1 C7 107.1(4) . . ? N2 P1 Pt1 101.3(2) . . ? C13 P1 Pt1 118.0(3) . . ? C7 P1 Pt1 119.0(3) . . ? C2 N1 C6 119.0(7) . . ? C2 N1 Pt1 116.8(5) . . ? C6 N1 Pt1 124.2(6) . . ? C2 N2 P1 119.8(5) . . ? N1 C2 N2 118.5(7) . . ? N1 C2 C3 120.9(8) . . ? N2 C2 C3 120.6(7) . . ? C4 C3 C2 118.9(8) . . ? C5 C4 C3 120.5(9) . . ? C4 C5 C6 119.1(9) . . ? N1 C6 C5 121.6(8) . . ? C8 C7 C12 119.5(8) . . ? C8 C7 P1 122.5(7) . . ? C12 C7 P1 118.0(6) . . ? C7 C8 C9 119.1(9) . . ? C10 C9 C8 119.8(10) . . ? C9 C10 C11 121.7(9) . . ? C12 C11 C10 118.0(10) . . ? C11 C12 C7 122.0(9) . . ? C14 C13 C18 118.9(8) . . ? C14 C13 P1 121.7(6) . . ? C18 C13 P1 119.3(6) . . ? C15 C14 C13 120.5(8) . . ? C14 C15 C16 120.9(8) . . ? C15 C16 C17 119.8(9) . . ? C18 C17 C16 120.2(8) . . ? C17 C18 C13 119.8(8) . . ? C21 P2 C19 110.9(12) . . ? C20' P2 C19 116.4(7) . . ? C20' P2 C21' 103.6(8) . . ? C19 P2 C21' 95.4(7) . . ? C21 P2 C20 103.3(14) . . ? C19 P2 C20 90.0(9) . . ? C21 P2 Pt1 119.9(11) . . ? C20' P2 Pt1 111.3(6) . . ? C19 P2 Pt1 119.4(4) . . ? C21' P2 Pt1 107.6(5) . . ? C20 P2 Pt1 107.2(8) . . ? Cl7 C50 Cl6 62.7(11) . . ? Cl7 C50 Cl3 108.5(9) . . ? Cl6 C50 Cl3 118.1(6) . . ? Cl7 C50 Cl4 28.0(11) . . ? Cl6 C50 Cl4 90.7(7) . . ? Cl3 C50 Cl4 96.9(5) . . ? Cl7 C50 Cl5 121.2(13) . . ? Cl6 C50 Cl5 58.5(6) . . ? Cl3 C50 Cl5 99.4(4) . . ? Cl4 C50 Cl5 149.1(8) . . ? Cl7 Cl4 C50 74.1(8) . . ? Cl6 Cl5 C50 59.4(3) . . ? Cl7 Cl6 Cl5 121.0(7) . . ? Cl7 Cl6 C50 58.9(6) . . ? Cl5 Cl6 C50 62.1(4) . . ? Cl4 Cl7 Cl6 136.3(7) . . ? Cl4 Cl7 C50 78.0(6) . . ? Cl6 Cl7 C50 58.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 P1 N2 8.0(3) . . . . ? P2 Pt1 P1 N2 -168.9(3) . . . . ? Cl1 Pt1 P1 N2 11.8(10) . . . . ? N1 Pt1 P1 C13 -107.6(4) . . . . ? P2 Pt1 P1 C13 75.5(3) . . . . ? Cl1 Pt1 P1 C13 -103.8(9) . . . . ? N1 Pt1 P1 C7 120.0(4) . . . . ? P2 Pt1 P1 C7 -56.9(3) . . . . ? Cl1 Pt1 P1 C7 123.8(9) . . . . ? P1 Pt1 N1 C2 -6.2(5) . . . . ? P2 Pt1 N1 C2 81.3(32) . . . . ? Cl1 Pt1 N1 C2 174.1(5) . . . . ? P1 Pt1 N1 C6 174.1(6) . . . . ? P2 Pt1 N1 C6 -98.4(31) . . . . ? Cl1 Pt1 N1 C6 -5.5(6) . . . . ? C13 P1 N2 C2 112.8(7) . . . . ? C7 P1 N2 C2 -134.6(6) . . . . ? Pt1 P1 N2 C2 -11.1(7) . . . . ? C6 N1 C2 N2 -179.3(7) . . . . ? Pt1 N1 C2 N2 1.0(9) . . . . ? C6 N1 C2 C3 0.5(11) . . . . ? Pt1 N1 C2 C3 -179.1(6) . . . . ? P1 N2 C2 N1 7.5(10) . . . . ? P1 N2 C2 C3 -172.3(6) . . . . ? N1 C2 C3 C4 -0.1(12) . . . . ? N2 C2 C3 C4 179.8(8) . . . . ? C2 C3 C4 C5 -0.8(13) . . . . ? C3 C4 C5 C6 1.0(14) . . . . ? C2 N1 C6 C5 -0.2(12) . . . . ? Pt1 N1 C6 C5 179.4(6) . . . . ? C4 C5 C6 N1 -0.6(14) . . . . ? N2 P1 C7 C8 -129.4(7) . . . . ? C13 P1 C7 C8 -17.4(8) . . . . ? Pt1 P1 C7 C8 119.7(6) . . . . ? N2 P1 C7 C12 52.9(7) . . . . ? C13 P1 C7 C12 164.9(6) . . . . ? Pt1 P1 C7 C12 -58.1(7) . . . . ? C12 C7 C8 C9 -1.7(12) . . . . ? P1 C7 C8 C9 -179.4(7) . . . . ? C7 C8 C9 C10 1.2(14) . . . . ? C8 C9 C10 C11 0.0(15) . . . . ? C9 C10 C11 C12 -0.7(15) . . . . ? C10 C11 C12 C7 0.1(14) . . . . ? C8 C7 C12 C11 1.1(13) . . . . ? P1 C7 C12 C11 178.9(7) . . . . ? N2 P1 C13 C14 -118.5(7) . . . . ? C7 P1 C13 C14 131.8(7) . . . . ? Pt1 P1 C13 C14 -5.7(8) . . . . ? N2 P1 C13 C18 58.7(7) . . . . ? C7 P1 C13 C18 -51.0(8) . . . . ? Pt1 P1 C13 C18 171.5(6) . . . . ? C18 C13 C14 C15 1.2(13) . . . . ? P1 C13 C14 C15 178.4(7) . . . . ? C13 C14 C15 C16 -0.3(14) . . . . ? C14 C15 C16 C17 -1.0(15) . . . . ? C15 C16 C17 C18 1.4(15) . . . . ? C16 C17 C18 C13 -0.5(14) . . . . ? C14 C13 C18 C17 -0.8(13) . . . . ? P1 C13 C18 C17 -178.0(7) . . . . ? N1 Pt1 P2 C21 110.7(34) . . . . ? P1 Pt1 P2 C21 -162.2(14) . . . . ? Cl1 Pt1 P2 C21 17.7(14) . . . . ? N1 Pt1 P2 C20' 33.6(32) . . . . ? P1 Pt1 P2 C20' 120.7(7) . . . . ? Cl1 Pt1 P2 C20' -59.3(7) . . . . ? N1 Pt1 P2 C19 -106.6(32) . . . . ? P1 Pt1 P2 C19 -19.4(6) . . . . ? Cl1 Pt1 P2 C19 160.5(6) . . . . ? N1 Pt1 P2 C21' 146.5(31) . . . . ? P1 Pt1 P2 C21' -126.4(6) . . . . ? Cl1 Pt1 P2 C21' 53.6(6) . . . . ? N1 Pt1 P2 C20 -6.5(33) . . . . ? P1 Pt1 P2 C20 80.7(8) . . . . ? Cl1 Pt1 P2 C20 -99.4(8) . . . . ? Cl7 C50 Cl4 Cl7 0.000(4) . . . . ? Cl6 C50 Cl4 Cl7 -1.4(23) . . . . ? Cl3 C50 Cl4 Cl7 117.0(23) . . . . ? Cl5 C50 Cl4 Cl7 -4.5(31) . . . . ? Cl7 C50 Cl5 Cl6 1.2(10) . . . . ? Cl6 C50 Cl5 Cl6 0.0 . . . . ? Cl3 C50 Cl5 Cl6 -117.3(6) . . . . ? Cl4 C50 Cl5 Cl6 3.6(13) . . . . ? C50 Cl5 Cl6 Cl7 -1.1(9) . . . . ? C50 Cl5 Cl6 C50 0.0 . . . . ? Cl7 C50 Cl6 Cl7 0.000(2) . . . . ? Cl3 C50 Cl6 Cl7 -97.5(10) . . . . ? Cl4 C50 Cl6 Cl7 0.7(12) . . . . ? Cl5 C50 Cl6 Cl7 178.9(9) . . . . ? Cl7 C50 Cl6 Cl5 -178.9(9) . . . . ? Cl3 C50 Cl6 Cl5 83.6(5) . . . . ? Cl4 C50 Cl6 Cl5 -178.1(7) . . . . ? Cl5 C50 Cl6 Cl5 0.0 . . . . ? C50 Cl4 Cl7 Cl6 1.9(32) . . . . ? C50 Cl4 Cl7 C50 0.000(1) . . . . ? Cl5 Cl6 Cl7 Cl4 -1.0(45) . . . . ? C50 Cl6 Cl7 Cl4 -2.2(36) . . . . ? Cl5 Cl6 Cl7 C50 1.2(9) . . . . ? C50 Cl6 Cl7 C50 0.000(1) . . . . ? Cl6 C50 Cl7 Cl4 178.5(26) . . . . ? Cl3 C50 Cl7 Cl4 -68.8(23) . . . . ? Cl4 C50 Cl7 Cl4 0.000(4) . . . . ? Cl5 C50 Cl7 Cl4 177.3(19) . . . . ? Cl6 C50 Cl7 Cl6 0.000(1) . . . . ? Cl3 C50 Cl7 Cl6 112.7(8) . . . . ? Cl4 C50 Cl7 Cl6 -178.5(26) . . . . ? Cl5 C50 Cl7 Cl6 -1.1(9) . . . . ? _refine_diff_density_max 1.399 _refine_diff_density_min -2.402 _refine_diff_density_rms 0.191 #---END data_21 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C20 H23 Cl N2 P2 Pt' _chemical_formula_structural 'C20 H23 Cl N2 P2 Pt' _chemical_formula_analytical 'C20 H23 Cl N2 P2 Pt' _chemical_formula_sum 'C20 H23 Cl N2 P2 Pt' _chemical_formula_weight 583.88 _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' '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 11.3818(2) _cell_length_b 13.2084(2) _cell_length_c 14.19120(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2133.44(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 156 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .15 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method - _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 6.859 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.618686 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 9437 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3054 _reflns_number_observed 2942 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0163P)^2^+0.0465P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00449(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(6) _refine_ls_number_reflns 3054 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_obs 0.0174 _refine_ls_wR_factor_all 0.0387 _refine_ls_wR_factor_obs 0.0380 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.052 _refine_ls_restrained_S_all 1.049 _refine_ls_restrained_S_obs 1.052 _refine_ls_shift/esd_max -0.002 _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 0.148922(15) 0.528124(14) 0.682537(12) 0.03153(8) Uani 1 d . . Cl1 Cl 0.33164(12) 0.59682(13) 0.73342(12) 0.0666(4) Uani 1 d . . P1 P -0.02271(10) 0.48102(11) 0.62371(8) 0.0313(3) Uani 1 d . . N1 N 0.1160(3) 0.6487(3) 0.5907(3) 0.0356(10) Uani 1 d . . C2 C 0.0214(4) 0.6384(4) 0.5310(3) 0.0342(12) Uani 1 d . . N2 N -0.0485(4) 0.5579(3) 0.5356(3) 0.0386(10) Uani 1 d . . C3 C 0.0003(5) 0.7154(4) 0.4635(4) 0.0450(15) Uani 1 d . . H3A H -0.0619(5) 0.7085(4) 0.4215(4) 0.054 Uiso 1 calc R . C4 C 0.0698(6) 0.7992(5) 0.4593(4) 0.055(2) Uani 1 d . . H4A H 0.0548(6) 0.8496(5) 0.4152(4) 0.066 Uiso 1 calc R . C5 C 0.1629(6) 0.8086(4) 0.5213(4) 0.053(2) Uani 1 d . . H5A H 0.2114(6) 0.8652(4) 0.5191(4) 0.064 Uiso 1 calc R . C6 C 0.1825(5) 0.7341(4) 0.5854(4) 0.0438(14) Uani 1 d . . H6A H 0.2444(5) 0.7419(4) 0.6276(4) 0.053 Uiso 1 calc R . C7 C -0.1467(4) 0.4932(3) 0.7033(3) 0.0358(11) Uani 1 d . . C8 C -0.2601(4) 0.4825(4) 0.6684(4) 0.0483(13) Uani 1 d . . H8A H -0.2716(4) 0.4651(4) 0.6056(4) 0.058 Uiso 1 calc R . C9 C -0.3566(5) 0.4980(5) 0.7271(5) 0.065(2) Uani 1 d . . H9A H -0.4323(5) 0.4888(5) 0.7040(5) 0.078 Uiso 1 calc R . C10 C -0.3403(5) 0.5262(5) 0.8173(4) 0.069(2) Uani 1 d . . H10A H -0.4052(5) 0.5357(5) 0.8562(4) 0.083 Uiso 1 calc R . C11 C -0.2294(6) 0.5412(5) 0.8531(4) 0.067(2) Uani 1 d . . H11A H -0.2192(6) 0.5632(5) 0.9148(4) 0.081 Uiso 1 calc R . C12 C -0.1327(5) 0.5232(4) 0.7956(3) 0.0491(13) Uani 1 d . . H12A H -0.0574(5) 0.5315(4) 0.8198(3) 0.059 Uiso 1 calc R . C13 C -0.0328(4) 0.3548(4) 0.5740(3) 0.0349(12) Uani 1 d . . C14 C -0.1077(5) 0.2800(4) 0.6054(4) 0.051(2) Uani 1 d . . H14A H -0.1590(5) 0.2938(4) 0.6547(4) 0.061 Uiso 1 calc R . C15 C -0.1080(6) 0.1856(4) 0.5650(5) 0.063(2) Uani 1 d . . H15A H -0.1591(6) 0.1363(4) 0.5876(5) 0.076 Uiso 1 calc R . C16 C -0.0349(7) 0.1634(5) 0.4932(5) 0.071(2) Uani 1 d . . H16A H -0.0356(7) 0.0990(5) 0.4666(5) 0.085 Uiso 1 calc R . C17 C 0.0410(7) 0.2363(5) 0.4593(5) 0.070(2) Uani 1 d . . H17A H 0.0918(7) 0.2216(5) 0.4097(5) 0.083 Uiso 1 calc R . C18 C 0.0405(5) 0.3314(5) 0.4999(4) 0.053(2) Uani 1 d . . H18A H 0.0910(5) 0.3808(5) 0.4767(4) 0.064 Uiso 1 calc R . P2 P 0.18939(11) 0.39300(11) 0.77391(10) 0.0384(3) Uani 1 d . . C19 C 0.0854(5) 0.2922(5) 0.7858(4) 0.063(2) Uani 1 d . . H19A H 0.0118(5) 0.3190(5) 0.8074(4) 0.095 Uiso 1 calc R . H19B H 0.1143(5) 0.2436(5) 0.8305(4) 0.095 Uiso 1 calc R . H19C H 0.0745(5) 0.2599(5) 0.7258(4) 0.095 Uiso 1 calc R . C20 C 0.2193(6) 0.4239(5) 0.8953(4) 0.069(2) Uani 1 d . . H20A H 0.2752(6) 0.4782(5) 0.8980(4) 0.104 Uiso 1 calc R . H20B H 0.2508(6) 0.3655(5) 0.9267(4) 0.104 Uiso 1 calc R . H20C H 0.1478(6) 0.4443(5) 0.9257(4) 0.104 Uiso 1 calc R . C21 C 0.3178(6) 0.3265(5) 0.7336(5) 0.079(2) Uani 1 d . . H21A H 0.3809(6) 0.3738(5) 0.7245(5) 0.118 Uiso 1 calc R . H21B H 0.3006(6) 0.2933(5) 0.6750(5) 0.118 Uiso 1 calc R . H21C H 0.3404(6) 0.2771(5) 0.7797(5) 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 Pt1 0.02581(10) 0.03683(11) 0.03196(10) 0.00332(9) -0.00014(8) - 0.00258(9) Cl1 0.0373(8) 0.0742(11) 0.0883(11) 0.0178(9) -0.0190(8) -0.0182(8) P1 0.0286(6) 0.0352(7) 0.0299(6) 0.0030(6) 0.0004(5) -0.0036(6) N1 0.032(2) 0.039(2) 0.036(2) 0.002(2) 0.009(2) 0.001(2) C2 0.028(3) 0.041(3) 0.033(3) 0.001(2) 0.006(2) 0.005(2) N2 0.037(2) 0.042(3) 0.036(2) 0.006(2) -0.002(2) -0.005(2) C3 0.042(3) 0.050(4) 0.043(3) 0.014(3) 0.003(3) 0.009(3) C4 0.062(4) 0.045(4) 0.058(4) 0.016(3) 0.011(3) 0.017(3) C5 0.064(4) 0.031(3) 0.065(4) 0.006(3) 0.016(3) -0.004(3) C6 0.042(3) 0.042(3) 0.048(3) -0.001(3) 0.008(2) -0.007(3) C7 0.038(3) 0.035(3) 0.034(3) 0.005(2) 0.005(2) 0.000(2) C8 0.034(3) 0.060(3) 0.050(3) 0.005(3) -0.001(2) -0.005(3) C9 0.030(3) 0.090(5) 0.074(4) 0.020(3) 0.011(3) 0.007(3) C10 0.058(4) 0.077(4) 0.072(4) 0.023(5) 0.034(4) 0.016(4) C11 0.076(5) 0.080(5) 0.046(3) 0.001(3) 0.014(3) 0.014(4) C12 0.046(3) 0.057(3) 0.045(3) 0.003(3) 0.006(2) 0.006(3) C13 0.030(3) 0.041(3) 0.034(3) 0.004(2) -0.004(2) 0.001(2) C14 0.051(4) 0.041(3) 0.060(4) 0.005(3) 0.003(3) -0.008(3) C15 0.067(4) 0.040(4) 0.082(5) -0.003(3) -0.005(4) -0.018(3) C16 0.094(5) 0.045(4) 0.073(5) -0.014(4) -0.011(4) 0.006(4) C17 0.082(5) 0.064(5) 0.062(4) -0.015(4) 0.013(4) 0.015(4) C18 0.058(4) 0.052(4) 0.050(4) -0.004(3) 0.005(3) -0.001(3) P2 0.0369(7) 0.0418(8) 0.0366(8) 0.0043(6) -0.0026(6) 0.0044(6) C19 0.066(4) 0.060(4) 0.063(4) 0.033(3) -0.011(3) -0.014(3) C20 0.106(5) 0.059(4) 0.043(4) 0.009(3) -0.025(3) 0.012(4) C21 0.082(6) 0.071(5) 0.083(5) 0.014(4) 0.018(4) 0.033(4) _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 N1 2.091(4) . ? Pt1 P1 2.2136(11) . ? Pt1 P2 2.2537(14) . ? Pt1 Cl1 2.3811(14) . ? P1 N2 1.638(4) . ? P1 C13 1.814(5) . ? P1 C7 1.814(5) . ? N1 C6 1.361(7) . ? N1 C2 1.377(6) . ? C2 N2 1.329(6) . ? C2 C3 1.417(7) . ? C3 C4 1.363(8) . ? C4 C5 1.382(8) . ? C5 C6 1.359(8) . ? C7 C12 1.378(6) . ? C7 C8 1.389(7) . ? C8 C9 1.394(8) . ? C9 C10 1.346(8) . ? C10 C11 1.375(8) . ? C11 C12 1.390(8) . ? C13 C18 1.378(7) . ? C13 C14 1.378(7) . ? C14 C15 1.373(8) . ? C15 C16 1.348(9) . ? C16 C17 1.381(10) . ? C17 C18 1.382(8) . ? P2 C19 1.789(6) . ? P2 C21 1.798(6) . ? P2 C20 1.802(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 N1 Pt1 P1 79.69(11) . . ? N1 Pt1 P2 176.44(11) . . ? P1 Pt1 P2 100.06(5) . . ? N1 Pt1 Cl1 93.17(12) . . ? P1 Pt1 Cl1 172.85(5) . . ? P2 Pt1 Cl1 87.06(5) . . ? N2 P1 C13 105.2(2) . . ? N2 P1 C7 106.3(2) . . ? C13 P1 C7 105.9(2) . . ? N2 P1 Pt1 105.8(2) . . ? C13 P1 Pt1 117.4(2) . . ? C7 P1 Pt1 115.3(2) . . ? C6 N1 C2 118.9(4) . . ? C6 N1 Pt1 124.5(3) . . ? C2 N1 Pt1 116.7(3) . . ? N2 C2 N1 121.1(4) . . ? N2 C2 C3 120.3(5) . . ? N1 C2 C3 118.6(5) . . ? C2 N2 P1 115.2(3) . . ? C4 C3 C2 120.9(6) . . ? C3 C4 C5 119.4(5) . . ? C6 C5 C4 119.2(5) . . ? C5 C6 N1 123.1(5) . . ? C12 C7 C8 118.3(4) . . ? C12 C7 P1 121.8(4) . . ? C8 C7 P1 119.5(3) . . ? C7 C8 C9 120.3(5) . . ? C10 C9 C8 120.0(5) . . ? C9 C10 C11 121.2(5) . . ? C10 C11 C12 119.0(6) . . ? C7 C12 C11 121.1(5) . . ? C18 C13 C14 117.4(5) . . ? C18 C13 P1 117.7(4) . . ? C14 C13 P1 124.9(4) . . ? C15 C14 C13 121.2(6) . . ? C16 C15 C14 120.8(6) . . ? C15 C16 C17 119.9(6) . . ? C16 C17 C18 119.1(6) . . ? C13 C18 C17 121.7(6) . . ? C19 P2 C21 101.8(3) . . ? C19 P2 C20 101.7(3) . . ? C21 P2 C20 105.1(3) . . ? C19 P2 Pt1 120.5(2) . . ? C21 P2 Pt1 111.7(2) . . ? C20 P2 Pt1 114.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 P1 N2 10.3(2) . . . . ? P2 Pt1 P1 N2 -166.1(2) . . . . ? Cl1 Pt1 P1 N2 9.9(5) . . . . ? N1 Pt1 P1 C13 127.3(2) . . . . ? P2 Pt1 P1 C13 -49.1(2) . . . . ? Cl1 Pt1 P1 C13 126.9(5) . . . . ? N1 Pt1 P1 C7 -106.8(2) . . . . ? P2 Pt1 P1 C7 76.8(2) . . . . ? Cl1 Pt1 P1 C7 -107.3(5) . . . . ? P1 Pt1 N1 C6 172.7(4) . . . . ? P2 Pt1 N1 C6 -101.0(19) . . . . ? Cl1 Pt1 N1 C6 -7.3(4) . . . . ? P1 Pt1 N1 C2 -8.5(3) . . . . ? P2 Pt1 N1 C2 77.8(19) . . . . ? Cl1 Pt1 N1 C2 171.5(3) . . . . ? C6 N1 C2 N2 -177.8(4) . . . . ? Pt1 N1 C2 N2 3.3(6) . . . . ? C6 N1 C2 C3 2.8(7) . . . . ? Pt1 N1 C2 C3 -176.0(4) . . . . ? N1 C2 N2 P1 6.9(6) . . . . ? C3 C2 N2 P1 -173.8(4) . . . . ? C13 P1 N2 C2 -137.4(4) . . . . ? C7 P1 N2 C2 110.6(4) . . . . ? Pt1 P1 N2 C2 -12.5(4) . . . . ? N2 C2 C3 C4 178.7(5) . . . . ? N1 C2 C3 C4 -1.9(8) . . . . ? C2 C3 C4 C5 0.6(9) . . . . ? C3 C4 C5 C6 -0.3(9) . . . . ? C4 C5 C6 N1 1.3(8) . . . . ? C2 N1 C6 C5 -2.6(7) . . . . ? Pt1 N1 C6 C5 176.1(4) . . . . ? N2 P1 C7 C12 -121.0(4) . . . . ? C13 P1 C7 C12 127.5(4) . . . . ? Pt1 P1 C7 C12 -4.2(5) . . . . ? N2 P1 C7 C8 52.0(4) . . . . ? C13 P1 C7 C8 -59.5(4) . . . . ? Pt1 P1 C7 C8 168.9(4) . . . . ? C12 C7 C8 C9 -2.6(8) . . . . ? P1 C7 C8 C9 -175.9(4) . . . . ? C7 C8 C9 C10 2.0(9) . . . . ? C8 C9 C10 C11 0.6(9) . . . . ? C9 C10 C11 C12 -2.4(10) . . . . ? C8 C7 C12 C11 0.8(8) . . . . ? P1 C7 C12 C11 173.9(5) . . . . ? C10 C11 C12 C7 1.7(9) . . . . ? N2 P1 C13 C18 57.7(5) . . . . ? C7 P1 C13 C18 170.0(4) . . . . ? Pt1 P1 C13 C18 -59.6(4) . . . . ? N2 P1 C13 C14 -122.9(5) . . . . ? C7 P1 C13 C14 -10.6(5) . . . . ? Pt1 P1 C13 C14 119.8(4) . . . . ? C18 C13 C14 C15 0.8(8) . . . . ? P1 C13 C14 C15 -178.5(5) . . . . ? C13 C14 C15 C16 -0.2(9) . . . . ? C14 C15 C16 C17 -0.2(10) . . . . ? C15 C16 C17 C18 0.0(11) . . . . ? C14 C13 C18 C17 -1.1(9) . . . . ? P1 C13 C18 C17 178.3(5) . . . . ? C16 C17 C18 C13 0.7(10) . . . . ? N1 Pt1 P2 C19 -89.4(18) . . . . ? P1 Pt1 P2 C19 -3.7(3) . . . . ? Cl1 Pt1 P2 C19 176.8(3) . . . . ? N1 Pt1 P2 C21 29.9(19) . . . . ? P1 Pt1 P2 C21 115.6(3) . . . . ? Cl1 Pt1 P2 C21 -63.9(3) . . . . ? N1 Pt1 P2 C20 149.0(19) . . . . ? P1 Pt1 P2 C20 -125.3(2) . . . . ? Cl1 Pt1 P2 C20 55.2(3) . . . . ? _refine_diff_density_max 0.576 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.059 #---end data_39 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C35 H30 CL N2 O3 P2 Pt.Cl.C H2 Cl2' _chemical_formula_structural 'C36 H32 Cl4 N2 O3 P2 Pt' _chemical_formula_analytical 'C36 H32 Cl4 N2 O3 P2 Pt' _chemical_formula_sum 'C36 H32 Cl4 N2 O3 P2 Pt' _chemical_formula_weight 939.47 _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' 'Pt' 'Pt' -1.7033 8.3905 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.19290(10) _cell_length_b 11.43150(10) _cell_length_c 16.5134(3) _cell_angle_alpha 71.7460(10) _cell_angle_beta 82.0510(10) _cell_angle_gamma 73.6220(10) _cell_volume 1922.27(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 71 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max .44 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method - _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 4.048 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.879463 _exptl_absorpt_correction_T_max 1.00000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 8317 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.22 _reflns_number_total 5405 _reflns_number_observed 4654 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 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^)+(0.0360P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5355 _refine_ls_number_parameters 438 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_obs 0.0262 _refine_ls_wR_factor_all 0.0772 _refine_ls_wR_factor_obs 0.0616 _refine_ls_goodness_of_fit_all 1.000 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 1.216 _refine_ls_restrained_S_obs 1.043 _refine_ls_shift/esd_max 0.002 _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 0.24064(2) 0.07086(2) 0.182178(12) 0.03354(9) Uani 1 d . . Cl1 Cl 0.17576(15) 0.18525(14) 0.04391(9) 0.0626(4) Uani 1 d . . P1 P 0.29510(11) -0.05035(11) 0.31331(8) 0.0339(3) Uani 1 d . . N1 N 0.1638(4) -0.0805(4) 0.1867(3) 0.0399(10) Uani 1 d . . C2 C 0.1611(4) -0.1701(4) 0.2629(3) 0.0382(12) Uani 1 d . . C3 C 0.1034(5) -0.2698(5) 0.2745(4) 0.0506(14) Uani 1 d . . H3A H 0.1007(5) -0.3301(5) 0.3273(4) 0.061 Uiso 1 calc R . C4 C 0.0518(6) -0.2747(6) 0.2057(4) 0.063(2) Uani 1 d . . H4A H 0.0122(6) -0.3386(6) 0.2118(4) 0.075 Uiso 1 calc R . C5 C 0.0580(6) -0.1853(6) 0.1272(4) 0.067(2) Uani 1 d . . H5A H 0.0239(6) -0.1893(6) 0.0802(4) 0.080 Uiso 1 calc R . C6 C 0.1146(5) -0.0918(5) 0.1201(4) 0.058(2) Uani 1 d . . H6A H 0.1199(5) -0.0329(5) 0.0669(4) 0.070 Uiso 1 calc R . N2 N 0.2141(4) -0.1601(4) 0.3299(3) 0.0427(10) Uani 1 d D . H2N H 0.2254(45) -0.2213(35) 0.3868(13) 0.051(15) Uiso 1 d D . C8 C 0.4579(4) -0.1349(4) 0.3233(3) 0.0388(12) Uani 1 d . . C9 C 0.5493(5) -0.0985(5) 0.2622(4) 0.0525(14) Uani 1 d . . H9A H 0.5283(5) -0.0270(5) 0.2155(4) 0.063 Uiso 1 calc R . C10 C 0.6727(5) -0.1700(7) 0.2716(5) 0.069(2) Uani 1 d . . H10A H 0.7339(5) -0.1449(7) 0.2310(5) 0.082 Uiso 1 calc R . C11 C 0.7055(6) -0.2755(6) 0.3388(5) 0.065(2) Uani 1 d . . H11A H 0.7880(6) -0.3232(6) 0.3434(5) 0.079 Uiso 1 calc R . C12 C 0.6162(6) -0.3109(5) 0.3995(4) 0.062(2) Uani 1 d . . H12A H 0.6388(6) -0.3824(5) 0.4459(4) 0.075 Uiso 1 calc R . C13 C 0.4916(5) -0.2418(5) 0.3930(4) 0.0521(14) Uani 1 d . . H13A H 0.4317(5) -0.2668(5) 0.4348(4) 0.063 Uiso 1 calc R . C14 C 0.2453(4) 0.0141(4) 0.4030(3) 0.0381(11) Uani 1 d . . C15 C 0.3285(5) 0.0218(5) 0.4546(4) 0.0529(14) Uani 1 d . . H15A H 0.4134(5) -0.0131(5) 0.4466(4) 0.064 Uiso 1 calc R . C16 C 0.2859(6) 0.0814(6) 0.5180(4) 0.070(2) Uani 1 d . . H16A H 0.3418(6) 0.0851(6) 0.5533(4) 0.084 Uiso 1 calc R . C17 C 0.1609(7) 0.1349(6) 0.5285(4) 0.070(2) Uani 1 d . . H17A H 0.1329(7) 0.1761(6) 0.5705(4) 0.084 Uiso 1 calc R . C18 C 0.0775(6) 0.1289(6) 0.4792(4) 0.061(2) Uani 1 d . . H18A H -0.0069(6) 0.1654(6) 0.4876(4) 0.073 Uiso 1 calc R . C19 C 0.1187(5) 0.0674(5) 0.4152(3) 0.0485(13) Uani 1 d . . H19A H 0.0617(5) 0.0624(5) 0.3813(3) 0.058 Uiso 1 calc R . P2 P 0.31900(12) 0.22828(12) 0.18183(9) 0.0387(3) Uani 1 d . . O1 O 0.3627(3) 0.2058(3) 0.2739(2) 0.0455(8) Uani 1 d . . C20 C 0.4270(5) 0.2791(5) 0.3000(3) 0.0418(12) Uani 1 d . . C21 C 0.5499(5) 0.2304(6) 0.3121(4) 0.059(2) Uani 1 d . . H21A H 0.5930(5) 0.1564(6) 0.2980(4) 0.071 Uiso 1 calc R . C22 C 0.6104(6) 0.2934(7) 0.3462(5) 0.074(2) Uani 1 d . . H22A H 0.6947(6) 0.2603(7) 0.3565(5) 0.089 Uiso 1 calc R . C23 C 0.5476(7) 0.4021(7) 0.3646(4) 0.071(2) Uani 1 d . . H23A H 0.5891(7) 0.4437(7) 0.3871(4) 0.085 Uiso 1 calc R . C24 C 0.4243(7) 0.4517(7) 0.3505(5) 0.079(2) Uani 1 d . . H24A H 0.3822(7) 0.5276(7) 0.3624(5) 0.095 Uiso 1 calc R . C25 C 0.3615(6) 0.3888(6) 0.3184(4) 0.064(2) Uani 1 d . . H25A H 0.2767(6) 0.4206(6) 0.3096(4) 0.077 Uiso 1 calc R . O2 O 0.4424(3) 0.2446(3) 0.1255(2) 0.0488(9) Uani 1 d . . C26 C 0.4575(5) 0.2704(5) 0.0352(3) 0.0480(13) Uani 1 d . . C27 C 0.5136(6) 0.1697(7) 0.0022(4) 0.069(2) Uani 1 d . . H27A H 0.5356(6) 0.0869(7) 0.0381(4) 0.083 Uiso 1 calc R . C28 C 0.5361(7) 0.1935(9) -0.0833(6) 0.090(2) Uani 1 d . . H28A H 0.5739(7) 0.1261(9) -0.1059(6) 0.107 Uiso 1 calc R . C29 C 0.5051(8) 0.3114(11) -0.1358(5) 0.099(3) Uani 1 d . . H29A H 0.5202(8) 0.3252(11) -0.1945(5) 0.118 Uiso 1 calc R . C30 C 0.4508(7) 0.4127(8) -0.1036(5) 0.090(2) Uani 1 d . . H30A H 0.4315(7) 0.4950(8) -0.1405(5) 0.107 Uiso 1 calc R . C31 C 0.4243(6) 0.3928(6) -0.0155(4) 0.065(2) Uani 1 d . . H31A H 0.3859(6) 0.4600(6) 0.0072(4) 0.078 Uiso 1 calc R . O3 O 0.2328(3) 0.3674(3) 0.1526(2) 0.0450(8) Uani 1 d . . C32 C 0.1024(5) 0.4036(4) 0.1753(3) 0.0394(12) Uani 1 d . . C33 C 0.0279(5) 0.4858(5) 0.1114(3) 0.0462(13) Uani 1 d . . H33A H 0.0605(5) 0.5127(5) 0.0557(3) 0.055 Uiso 1 calc R . C34 C -0.0979(5) 0.5275(5) 0.1325(4) 0.0571(15) Uani 1 d . . H34A H -0.1506(5) 0.5827(5) 0.0900(4) 0.069 Uiso 1 calc R . C35 C -0.1464(5) 0.4893(5) 0.2147(4) 0.0545(15) Uani 1 d . . H35A H -0.2311(5) 0.5180(5) 0.2278(4) 0.065 Uiso 1 calc R . C36 C -0.0686(5) 0.4084(6) 0.2771(4) 0.0575(15) Uani 1 d . . H36A H -0.1002(5) 0.3833(6) 0.3331(4) 0.069 Uiso 1 calc R . C37 C 0.0569(5) 0.3638(5) 0.2573(3) 0.0487(13) Uani 1 d . . H37A H 0.1095(5) 0.3073(5) 0.2994(3) 0.058 Uiso 1 calc R . Cl2 Cl 0.20268(13) -0.37094(13) 0.49696(9) 0.0586(4) Uani 1 d . . C40 C -0.1383(8) 0.2002(9) 0.1647(6) 0.110(3) Uani 1 d . . H40A H -0.1721(8) 0.2776(9) 0.1815(6) 0.132 Uiso 1 calc R . H40B H -0.0549(8) 0.2015(9) 0.1394(6) 0.132 Uiso 1 calc R . Cl3 Cl -0.1264(2) 0.0712(2) 0.2562(2) 0.1127(7) Uani 1 d . . Cl4 Cl -0.2267(3) 0.2025(5) 0.0894(2) 0.198(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03860(13) 0.03325(12) 0.03076(12) -0.00832(8) -0.00632(8) - 0.01116(8) Cl1 0.0879(11) 0.0617(9) 0.0407(8) 0.0026(7) -0.0236(7) -0.0327(8) P1 0.0371(7) 0.0331(6) 0.0334(7) -0.0101(6) -0.0053(6) -0.0097(5) N1 0.048(2) 0.038(2) 0.039(3) -0.013(2) -0.008(2) -0.014(2) C2 0.039(3) 0.035(3) 0.043(3) -0.015(3) -0.002(2) -0.008(2) C3 0.057(3) 0.039(3) 0.060(4) -0.013(3) -0.008(3) -0.019(3) C4 0.080(4) 0.050(3) 0.075(5) -0.026(3) -0.008(4) -0.032(3) C5 0.098(5) 0.064(4) 0.060(4) -0.021(4) -0.024(4) -0.041(4) C6 0.080(4) 0.059(4) 0.045(3) -0.015(3) -0.021(3) -0.026(3) N2 0.051(3) 0.041(2) 0.040(3) -0.006(2) -0.010(2) -0.021(2) C8 0.040(3) 0.036(3) 0.044(3) -0.019(2) -0.009(2) -0.003(2) C9 0.052(3) 0.052(3) 0.051(4) -0.017(3) -0.001(3) -0.007(3) C10 0.042(4) 0.086(5) 0.081(5) -0.042(4) 0.004(3) -0.005(3) C11 0.056(4) 0.053(4) 0.088(5) -0.040(4) -0.017(4) 0.013(3) C12 0.063(4) 0.044(3) 0.073(5) -0.013(3) -0.025(4) 0.003(3) C13 0.050(3) 0.043(3) 0.060(4) -0.013(3) -0.009(3) -0.006(3) C14 0.041(3) 0.035(3) 0.035(3) -0.006(2) -0.005(2) -0.008(2) C15 0.053(3) 0.064(4) 0.049(3) -0.032(3) -0.009(3) -0.007(3) C16 0.071(4) 0.089(5) 0.065(4) -0.045(4) -0.012(3) -0.011(4) C17 0.092(5) 0.067(4) 0.055(4) -0.033(3) 0.006(4) -0.013(4) C18 0.055(4) 0.062(4) 0.056(4) -0.023(3) 0.015(3) -0.003(3) C19 0.044(3) 0.052(3) 0.047(3) -0.012(3) -0.001(3) -0.010(3) P2 0.0420(7) 0.0386(7) 0.0379(8) -0.0108(6) -0.0022(6) -0.0142(6) O1 0.054(2) 0.047(2) 0.041(2) -0.011(2) -0.009(2) -0.021(2) C20 0.053(3) 0.044(3) 0.035(3) -0.011(2) -0.002(2) -0.024(3) C21 0.047(3) 0.063(4) 0.076(4) -0.035(3) -0.013(3) -0.007(3) C22 0.059(4) 0.081(5) 0.094(5) -0.031(4) -0.016(4) -0.024(4) C23 0.090(5) 0.077(5) 0.066(4) -0.029(4) -0.013(4) -0.040(4) C24 0.086(5) 0.071(4) 0.099(6) -0.049(4) -0.012(4) -0.016(4) C25 0.059(4) 0.059(4) 0.081(5) -0.033(4) -0.009(3) -0.011(3) O2 0.044(2) 0.059(2) 0.045(2) -0.015(2) 0.000(2) -0.018(2) C26 0.046(3) 0.060(4) 0.039(3) -0.012(3) 0.005(2) -0.022(3) C27 0.078(4) 0.070(4) 0.067(5) -0.031(4) 0.005(4) -0.022(4) C28 0.089(6) 0.111(7) 0.073(6) -0.046(5) 0.023(4) -0.025(5) C29 0.089(6) 0.151(9) 0.059(5) -0.035(6) 0.020(4) -0.039(6) C30 0.089(5) 0.100(6) 0.070(5) -0.003(5) 0.000(4) -0.035(5) C31 0.067(4) 0.065(4) 0.059(4) -0.008(3) -0.003(3) -0.024(3) O3 0.046(2) 0.042(2) 0.045(2) -0.010(2) 0.002(2) -0.015(2) C32 0.045(3) 0.035(3) 0.043(3) -0.015(2) 0.000(2) -0.014(2) C33 0.058(4) 0.044(3) 0.036(3) -0.008(3) -0.008(3) -0.013(3) C34 0.059(4) 0.047(3) 0.062(4) -0.006(3) -0.021(3) -0.010(3) C35 0.046(3) 0.050(3) 0.068(4) -0.020(3) -0.003(3) -0.008(3) C36 0.057(4) 0.069(4) 0.046(4) -0.016(3) 0.008(3) -0.023(3) C37 0.051(3) 0.048(3) 0.037(3) 0.002(3) -0.003(3) -0.013(3) Cl2 0.0572(9) 0.0519(8) 0.0502(9) -0.0013(7) 0.0009(7) -0.0048(7) C40 0.088(6) 0.126(7) 0.139(9) -0.056(7) 0.005(5) -0.046(5) Cl3 0.0809(13) 0.102(2) 0.133(2) -0.0252(15) 0.0031(13) -0.0035(11) Cl4 0.132(2) 0.356(6) 0.131(3) -0.093(3) -0.036(2) -0.060(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 Pt1 N1 2.117(4) . ? Pt1 P2 2.2113(12) . ? Pt1 P1 2.2338(13) . ? Pt1 Cl1 2.3459(14) . ? P1 N2 1.681(4) . ? P1 C8 1.809(5) . ? P1 C14 1.809(5) . ? N1 C6 1.352(6) . ? N1 C2 1.353(6) . ? C2 N2 1.374(6) . ? C2 C3 1.412(7) . ? C3 C4 1.366(8) . ? C4 C5 1.384(8) . ? C5 C6 1.356(8) . ? C8 C9 1.388(7) . ? C8 C13 1.392(7) . ? C9 C10 1.394(8) . ? C10 C11 1.358(9) . ? C11 C12 1.366(9) . ? C12 C13 1.395(8) . ? C14 C15 1.383(7) . ? C14 C19 1.390(7) . ? C15 C16 1.382(8) . ? C16 C17 1.371(9) . ? C17 C18 1.348(8) . ? C18 C19 1.404(8) . ? P2 O3 1.574(3) . ? P2 O2 1.578(4) . ? P2 O1 1.583(4) . ? O1 C20 1.434(5) . ? C20 C21 1.348(7) . ? C20 C25 1.364(7) . ? C21 C22 1.389(8) . ? C22 C23 1.347(9) . ? C23 C24 1.358(9) . ? C24 C25 1.385(8) . ? O2 C26 1.422(6) . ? C26 C31 1.362(8) . ? C26 C27 1.382(8) . ? C27 C28 1.353(10) . ? C28 C29 1.333(11) . ? C29 C30 1.377(11) . ? C30 C31 1.402(10) . ? O3 C32 1.431(6) . ? C32 C37 1.361(7) . ? C32 C33 1.369(7) . ? C33 C34 1.386(8) . ? C34 C35 1.374(8) . ? C35 C36 1.368(8) . ? C36 C37 1.383(7) . ? C40 Cl4 1.683(9) . ? C40 Cl3 1.739(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 N1 Pt1 P2 178.14(12) . . ? N1 Pt1 P1 82.50(11) . . ? P2 Pt1 P1 96.03(5) . . ? N1 Pt1 Cl1 92.77(11) . . ? P2 Pt1 Cl1 88.69(5) . . ? P1 Pt1 Cl1 175.27(5) . . ? N2 P1 C8 107.0(2) . . ? N2 P1 C14 103.9(2) . . ? C8 P1 C14 107.8(2) . . ? N2 P1 Pt1 100.7(2) . . ? C8 P1 Pt1 115.9(2) . . ? C14 P1 Pt1 119.8(2) . . ? C6 N1 C2 118.2(4) . . ? C6 N1 Pt1 124.8(4) . . ? C2 N1 Pt1 117.0(3) . . ? N1 C2 N2 118.0(4) . . ? N1 C2 C3 121.5(4) . . ? N2 C2 C3 120.5(5) . . ? C4 C3 C2 117.9(5) . . ? C3 C4 C5 120.5(5) . . ? C6 C5 C4 118.9(5) . . ? N1 C6 C5 122.9(6) . . ? C2 N2 P1 120.1(3) . . ? C9 C8 C13 119.3(5) . . ? C9 C8 P1 121.8(4) . . ? C13 C8 P1 118.8(4) . . ? C8 C9 C10 119.4(6) . . ? C11 C10 C9 121.5(6) . . ? C10 C11 C12 119.3(6) . . ? C11 C12 C13 121.2(6) . . ? C8 C13 C12 119.3(6) . . ? C15 C14 C19 119.3(5) . . ? C15 C14 P1 122.7(4) . . ? C19 C14 P1 117.8(4) . . ? C16 C15 C14 120.3(5) . . ? C17 C16 C15 119.7(6) . . ? C18 C17 C16 121.5(6) . . ? C17 C18 C19 119.8(6) . . ? C14 C19 C18 119.5(5) . . ? O3 P2 O2 101.1(2) . . ? O3 P2 O1 107.9(2) . . ? O2 P2 O1 100.8(2) . . ? O3 P2 Pt1 117.17(13) . . ? O2 P2 Pt1 118.40(14) . . ? O1 P2 Pt1 109.79(14) . . ? C20 O1 P2 128.1(3) . . ? C21 C20 C25 122.2(5) . . ? C21 C20 O1 117.7(5) . . ? C25 C20 O1 119.8(5) . . ? C20 C21 C22 118.4(6) . . ? C23 C22 C21 120.3(6) . . ? C22 C23 C24 120.8(6) . . ? C23 C24 C25 119.8(6) . . ? C20 C25 C24 118.5(6) . . ? C26 O2 P2 126.0(3) . . ? C31 C26 C27 122.2(6) . . ? C31 C26 O2 119.8(5) . . ? C27 C26 O2 117.9(5) . . ? C28 C27 C26 118.9(7) . . ? C29 C28 C27 121.4(8) . . ? C28 C29 C30 120.2(7) . . ? C29 C30 C31 120.5(7) . . ? C26 C31 C30 116.8(6) . . ? C32 O3 P2 124.9(3) . . ? C37 C32 C33 122.2(5) . . ? C37 C32 O3 121.4(5) . . ? C33 C32 O3 116.3(4) . . ? C32 C33 C34 117.6(5) . . ? C35 C34 C33 121.5(5) . . ? C36 C35 C34 119.1(5) . . ? C35 C36 C37 120.4(5) . . ? C32 C37 C36 119.1(5) . . ? Cl4 C40 Cl3 115.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 P1 N2 -10.3(2) . . . . ? P2 Pt1 P1 N2 168.6(2) . . . . ? Cl1 Pt1 P1 N2 -9.6(7) . . . . ? N1 Pt1 P1 C8 104.7(2) . . . . ? P2 Pt1 P1 C8 -76.4(2) . . . . ? Cl1 Pt1 P1 C8 105.4(7) . . . . ? N1 Pt1 P1 C14 -123.2(2) . . . . ? P2 Pt1 P1 C14 55.6(2) . . . . ? Cl1 Pt1 P1 C14 -122.6(7) . . . . ? P2 Pt1 N1 C6 149.1(32) . . . . ? P1 Pt1 N1 C6 -172.8(4) . . . . ? Cl1 Pt1 N1 C6 7.3(4) . . . . ? P2 Pt1 N1 C2 -29.0(37) . . . . ? P1 Pt1 N1 C2 9.1(3) . . . . ? Cl1 Pt1 N1 C2 -170.9(3) . . . . ? C6 N1 C2 N2 178.3(4) . . . . ? Pt1 N1 C2 N2 -3.5(6) . . . . ? C6 N1 C2 C3 -3.1(7) . . . . ? Pt1 N1 C2 C3 175.2(4) . . . . ? N1 C2 C3 C4 1.1(8) . . . . ? N2 C2 C3 C4 179.7(5) . . . . ? C2 C3 C4 C5 0.9(9) . . . . ? C3 C4 C5 C6 -0.9(10) . . . . ? C2 N1 C6 C5 3.1(8) . . . . ? Pt1 N1 C6 C5 -175.0(5) . . . . ? C4 C5 C6 N1 -1.2(10) . . . . ? N1 C2 N2 P1 -7.5(6) . . . . ? C3 C2 N2 P1 173.8(4) . . . . ? C8 P1 N2 C2 -108.4(4) . . . . ? C14 P1 N2 C2 137.6(4) . . . . ? Pt1 P1 N2 C2 13.1(4) . . . . ? N2 P1 C8 C9 130.7(4) . . . . ? C14 P1 C8 C9 -118.1(4) . . . . ? Pt1 P1 C8 C9 19.3(5) . . . . ? N2 P1 C8 C13 -47.4(4) . . . . ? C14 P1 C8 C13 63.9(4) . . . . ? Pt1 P1 C8 C13 -158.8(3) . . . . ? C13 C8 C9 C10 0.4(7) . . . . ? P1 C8 C9 C10 -177.6(4) . . . . ? C8 C9 C10 C11 0.7(9) . . . . ? C9 C10 C11 C12 -1.4(9) . . . . ? C10 C11 C12 C13 1.0(9) . . . . ? C9 C8 C13 C12 -0.8(8) . . . . ? P1 C8 C13 C12 177.3(4) . . . . ? C11 C12 C13 C8 0.1(8) . . . . ? N2 P1 C14 C15 128.0(4) . . . . ? C8 P1 C14 C15 14.7(5) . . . . ? Pt1 P1 C14 C15 -120.7(4) . . . . ? N2 P1 C14 C19 -57.6(4) . . . . ? C8 P1 C14 C19 -171.0(4) . . . . ? Pt1 P1 C14 C19 53.6(4) . . . . ? C19 C14 C15 C16 0.4(9) . . . . ? P1 C14 C15 C16 174.7(5) . . . . ? C14 C15 C16 C17 -1.2(10) . . . . ? C15 C16 C17 C18 1.2(11) . . . . ? C16 C17 C18 C19 -0.3(10) . . . . ? C15 C14 C19 C18 0.4(8) . . . . ? P1 C14 C19 C18 -174.1(4) . . . . ? C17 C18 C19 C14 -0.5(9) . . . . ? N1 Pt1 P2 O3 -93.5(35) . . . . ? P1 Pt1 P2 O3 -131.5(2) . . . . ? Cl1 Pt1 P2 O3 48.4(2) . . . . ? N1 Pt1 P2 O2 144.9(34) . . . . ? P1 Pt1 P2 O2 106.9(2) . . . . ? Cl1 Pt1 P2 O2 -73.2(2) . . . . ? N1 Pt1 P2 O1 30.0(35) . . . . ? P1 Pt1 P2 O1 -8.02(15) . . . . ? Cl1 Pt1 P2 O1 171.83(15) . . . . ? O3 P2 O1 C20 -56.4(4) . . . . ? O2 P2 O1 C20 49.1(4) . . . . ? Pt1 P2 O1 C20 174.8(4) . . . . ? P2 O1 C20 C21 -103.8(5) . . . . ? P2 O1 C20 C25 81.7(6) . . . . ? C25 C20 C21 C22 1.3(9) . . . . ? O1 C20 C21 C22 -173.1(5) . . . . ? C20 C21 C22 C23 -1.6(10) . . . . ? C21 C22 C23 C24 0.3(11) . . . . ? C22 C23 C24 C25 1.2(11) . . . . ? C21 C20 C25 C24 0.2(9) . . . . ? O1 C20 C25 C24 174.5(6) . . . . ? C23 C24 C25 C20 -1.4(10) . . . . ? O3 P2 O2 C26 -67.6(4) . . . . ? O1 P2 O2 C26 -178.4(4) . . . . ? Pt1 P2 O2 C26 61.9(4) . . . . ? P2 O2 C26 C31 84.5(6) . . . . ? P2 O2 C26 C27 -99.7(5) . . . . ? C31 C26 C27 C28 -0.1(9) . . . . ? O2 C26 C27 C28 -175.8(6) . . . . ? C26 C27 C28 C29 -0.1(12) . . . . ? C27 C28 C29 C30 1.0(13) . . . . ? C28 C29 C30 C31 -1.8(12) . . . . ? C27 C26 C31 C30 -0.6(9) . . . . ? O2 C26 C31 C30 175.0(5) . . . . ? C29 C30 C31 C26 1.5(10) . . . . ? O2 P2 O3 C32 171.1(3) . . . . ? O1 P2 O3 C32 -83.6(4) . . . . ? Pt1 P2 O3 C32 40.8(4) . . . . ? P2 O3 C32 C37 46.5(6) . . . . ? P2 O3 C32 C33 -137.2(4) . . . . ? C37 C32 C33 C34 -0.5(7) . . . . ? O3 C32 C33 C34 -176.8(4) . . . . ? C32 C33 C34 C35 0.7(8) . . . . ? C33 C34 C35 C36 0.2(8) . . . . ? C34 C35 C36 C37 -1.3(8) . . . . ? C33 C32 C37 C36 -0.5(8) . . . . ? O3 C32 C37 C36 175.6(5) . . . . ? C35 C36 C37 C32 1.5(8) . . . . ? _refine_diff_density_max 1.683 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.084 #---END