Electronic Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yong-Joo Kim' _publ_contact_author_address ; Department of Chemistry Kangnung National University Kangnung 210-702 SOUTH KOREA ; _publ_contact_author_email YJKIM@KANGNUNG.AC.KR _publ_section_title ; Bis(isothiocyanato)bis(phosphine) complexes of group 10 metals: reactivity toward organic isocyanides ; loop_ _publ_author_name 'Yong-Joo Kim.' 'Xiaohong Chang.' 'Kyung-Eun Lee.' 'H.-K. Lee' 'Soon W. Lee' data_nincs2 _database_code_depnum_ccdc_archive 'CCDC 275741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H31 N3 Ni P2 S2' _chemical_formula_weight 582.32 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pnma ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.503(3) _cell_length_b 12.9769(15) _cell_length_c 15.918(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2995.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.07 _cell_measurement_theta_max 15.88 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'RED ' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5501 _exptl_absorpt_correction_T_max 0.5935 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2731 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2731 _reflns_number_gt 1188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+2.6601P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2731 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1722 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.68690(9) 0.2500 0.42136(7) 0.0567(4) Uani 1 2 d S . . S1 S 0.8641(3) 0.2500 0.6631(2) 0.166(2) Uani 1 2 d S . . S2 S 0.4413(2) 0.2500 0.62069(18) 0.0873(10) Uani 1 2 d S . . P1 P 0.68224(14) 0.07995(14) 0.41784(12) 0.0680(6) Uani 1 1 d . . . N1 N 0.6659(5) 0.2500 0.2380(5) 0.062(2) Uani 1 2 d S . . N2 N 0.7679(6) 0.2500 0.5152(5) 0.082(3) Uani 1 2 d S . . N3 N 0.5619(7) 0.2500 0.4876(6) 0.101(3) Uani 1 2 d S . . C1 C 0.6751(7) 0.2500 0.3105(6) 0.062(3) Uani 1 2 d S . . C2 C 0.6526(8) 0.2500 0.1505(5) 0.061(3) Uani 1 2 d S . . C3 C 0.5621(9) 0.2500 0.1237(7) 0.072(3) Uani 1 2 d S . . C4 C 0.5483(10) 0.2500 0.0374(8) 0.097(4) Uani 1 2 d S . . H4 H 0.4889 0.2500 0.0156 0.117 Uiso 1 2 calc SR . . C5 C 0.6205(12) 0.2500 -0.0138(8) 0.094(4) Uani 1 2 d S . . H5 H 0.6091 0.2500 -0.0713 0.113 Uiso 1 2 calc SR . . C6 C 0.7107(9) 0.2500 0.0121(7) 0.084(4) Uani 1 2 d S . . H6 H 0.7585 0.2500 -0.0269 0.101 Uiso 1 2 calc SR . . C7 C 0.7297(8) 0.2500 0.0990(6) 0.072(3) Uani 1 2 d S . . C8 C 0.4804(8) 0.2500 0.1825(7) 0.102(4) Uani 1 2 d S . . H8A H 0.4244 0.2500 0.1503 0.153 Uiso 1 2 calc SR . . H8B H 0.4825 0.3104 0.2173 0.153 Uiso 0.50 1 calc PR . . H8C H 0.4825 0.1896 0.2173 0.153 Uiso 0.50 1 calc PR . . C9 C 0.8247(7) 0.2500 0.1352(7) 0.099(4) Uani 1 2 d S . . H9A H 0.8691 0.2500 0.0905 0.148 Uiso 1 2 calc SR . . H9B H 0.8330 0.1896 0.1692 0.148 Uiso 0.50 1 calc PR . . H9C H 0.8330 0.3104 0.1692 0.148 Uiso 0.50 1 calc PR . . C10 C 0.6746(5) 0.0249(6) 0.5221(4) 0.102(3) Uani 1 1 d . . . H10A H 0.7282 0.0439 0.5540 0.154 Uiso 1 1 calc R . . H10B H 0.6712 -0.0488 0.5180 0.154 Uiso 1 1 calc R . . H10C H 0.6203 0.0504 0.5497 0.154 Uiso 1 1 calc R . . C11 C 0.5780(5) 0.0350(6) 0.3642(6) 0.120(3) Uani 1 1 d . . . H11A H 0.5249 0.0680 0.3883 0.179 Uiso 1 1 calc R . . H11B H 0.5725 -0.0383 0.3707 0.179 Uiso 1 1 calc R . . H11C H 0.5818 0.0518 0.3056 0.179 Uiso 1 1 calc R . . C12 C 0.7788(6) 0.0162(6) 0.3712(5) 0.073(2) Uani 1 1 d . . . C13 C 0.7714(8) -0.0448(6) 0.3001(5) 0.113(3) Uani 1 1 d . . . H13 H 0.7142 -0.0534 0.2747 0.135 Uiso 1 1 calc R . . C14 C 0.8483(12) -0.0933(11) 0.2663(8) 0.165(7) Uani 1 1 d . . . H14 H 0.8417 -0.1354 0.2194 0.198 Uiso 1 1 calc R . . C15 C 0.9311(11) -0.0799(11) 0.3004(10) 0.154(7) Uani 1 1 d . . . H15 H 0.9822 -0.1127 0.2773 0.184 Uiso 1 1 calc R . . C16 C 0.9413(8) -0.0180(9) 0.3697(8) 0.140(4) Uani 1 1 d . . . H16 H 0.9996 -0.0074 0.3923 0.168 Uiso 1 1 calc R . . C17 C 0.8652(7) 0.0289(7) 0.4060(6) 0.103(3) Uani 1 1 d . . . H17 H 0.8724 0.0690 0.4540 0.123 Uiso 1 1 calc R . . C18 C 0.8080(7) 0.2500 0.5760(7) 0.076(3) Uani 1 2 d S . . C19 C 0.5126(7) 0.2500 0.5436(6) 0.062(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0675(9) 0.0565(8) 0.0461(7) 0.000 -0.0004(7) 0.000 S1 0.106(3) 0.314(7) 0.078(2) 0.000 -0.034(2) 0.000 S2 0.111(3) 0.0712(19) 0.0798(18) 0.000 0.0283(19) 0.000 P1 0.0751(14) 0.0561(12) 0.0727(12) 0.0123(10) 0.0011(12) -0.0043(11) N1 0.081(6) 0.052(5) 0.052(5) 0.000 -0.005(5) 0.000 N2 0.094(7) 0.091(7) 0.062(6) 0.000 -0.019(5) 0.000 N3 0.103(8) 0.105(8) 0.095(7) 0.000 0.046(6) 0.000 C1 0.076(7) 0.055(6) 0.053(6) 0.000 -0.006(6) 0.000 C2 0.092(9) 0.051(6) 0.039(5) 0.000 -0.015(6) 0.000 C3 0.092(9) 0.060(7) 0.065(7) 0.000 -0.017(7) 0.000 C4 0.122(13) 0.092(10) 0.077(9) 0.000 -0.045(9) 0.000 C5 0.151(14) 0.069(8) 0.063(8) 0.000 -0.013(9) 0.000 C6 0.109(11) 0.073(8) 0.071(8) 0.000 0.025(7) 0.000 C7 0.087(8) 0.066(7) 0.061(7) 0.000 0.011(6) 0.000 C8 0.078(9) 0.124(11) 0.105(9) 0.000 -0.005(8) 0.000 C9 0.075(9) 0.130(11) 0.090(8) 0.000 0.012(7) 0.000 C10 0.138(7) 0.081(6) 0.088(5) 0.038(5) 0.031(5) 0.008(6) C11 0.110(7) 0.069(5) 0.179(9) 0.021(6) -0.044(7) -0.034(6) C12 0.110(7) 0.049(4) 0.062(4) 0.008(4) 0.016(5) 0.003(5) C13 0.182(10) 0.074(6) 0.082(6) -0.008(5) -0.004(6) 0.017(7) C14 0.29(2) 0.098(9) 0.105(9) 0.002(7) 0.083(13) 0.065(14) C15 0.198(15) 0.085(9) 0.178(16) 0.048(10) 0.113(14) 0.033(13) C16 0.136(10) 0.094(8) 0.191(12) 0.010(8) 0.059(10) 0.013(8) C17 0.089(7) 0.081(6) 0.138(8) -0.011(6) 0.027(7) 0.000(6) C18 0.057(6) 0.107(9) 0.065(6) 0.000 0.014(7) 0.000 C19 0.064(7) 0.047(6) 0.074(7) 0.000 0.002(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.773(9) . ? Ni1 N2 1.899(9) . ? Ni1 N3 2.097(9) . ? Ni1 P1 2.2084(18) 7_565 ? Ni1 P1 2.2084(18) . ? S1 C18 1.608(12) . ? S2 C19 1.605(11) . ? P1 C12 1.788(8) . ? P1 C10 1.811(6) . ? P1 C11 1.832(7) . ? N1 C1 1.163(9) . ? N1 C2 1.405(10) . ? N2 C18 1.130(11) . ? N3 C19 1.142(11) . ? C2 C3 1.380(13) . ? C2 C7 1.387(13) . ? C3 C4 1.388(13) . ? C3 C8 1.509(13) . ? C4 C5 1.327(15) . ? C5 C6 1.372(15) . ? C6 C7 1.410(14) . ? C7 C9 1.494(13) . ? C12 C17 1.380(10) . ? C12 C13 1.385(10) . ? C13 C14 1.388(14) . ? C14 C15 1.330(17) . ? C15 C16 1.372(16) . ? C16 C17 1.387(12) . ? 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 C1 Ni1 N2 147.3(4) . . ? C1 Ni1 N3 114.6(4) . . ? N2 Ni1 N3 98.0(4) . . ? C1 Ni1 P1 88.38(6) . 7_565 ? N2 Ni1 P1 92.23(7) . 7_565 ? N3 Ni1 P1 89.21(7) . 7_565 ? C1 Ni1 P1 88.38(6) . . ? N2 Ni1 P1 92.23(7) . . ? N3 Ni1 P1 89.21(7) . . ? P1 Ni1 P1 175.44(14) 7_565 . ? C12 P1 C10 104.2(3) . . ? C12 P1 C11 107.8(4) . . ? C10 P1 C11 104.5(4) . . ? C12 P1 Ni1 116.7(3) . . ? C10 P1 Ni1 111.9(3) . . ? C11 P1 Ni1 110.8(3) . . ? C1 N1 C2 178.8(10) . . ? C18 N2 Ni1 172.8(9) . . ? C19 N3 Ni1 158.8(10) . . ? N1 C1 Ni1 178.9(9) . . ? C3 C2 C7 125.7(9) . . ? C3 C2 N1 115.9(10) . . ? C7 C2 N1 118.4(9) . . ? C2 C3 C4 116.3(12) . . ? C2 C3 C8 123.7(9) . . ? C4 C3 C8 120.1(12) . . ? C5 C4 C3 119.7(13) . . ? C4 C5 C6 124.6(12) . . ? C5 C6 C7 118.7(11) . . ? C2 C7 C6 115.0(10) . . ? C2 C7 C9 121.0(9) . . ? C6 C7 C9 123.9(10) . . ? C17 C12 C13 117.8(9) . . ? C17 C12 P1 119.3(7) . . ? C13 C12 P1 122.9(8) . . ? C12 C13 C14 120.9(11) . . ? C15 C14 C13 120.5(16) . . ? C14 C15 C16 120.1(18) . . ? C15 C16 C17 120.4(14) . . ? C12 C17 C16 120.2(10) . . ? N2 C18 S1 179.4(10) . . ? N3 C19 S2 178.5(11) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.535 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.064 #=========================================================END data_dimer _database_code_depnum_ccdc_archive 'CCDC 275742' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H71 Cl2 N7 Ni2 P2 S4' _chemical_formula_weight 1004.52 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.104(4) _cell_length_b 13.141(4) _cell_length_c 17.539(3) _cell_angle_alpha 81.160(19) _cell_angle_beta 82.24(2) _cell_angle_gamma 67.39(2) _cell_volume 2745.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 12.49 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'ORANGE ' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3056 _exptl_absorpt_correction_T_max 0.7435 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10037 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.1001 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9585 _reflns_number_gt 4834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1432P)^2^+3.9486P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9585 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1797 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2974 _refine_ls_wR_factor_gt 0.2354 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.31665(8) 0.67821(8) 0.24885(6) 0.0494(3) Uani 1 1 d . . . Ni2 Ni 0.64114(11) 0.96823(11) 0.35920(7) 0.0760(4) Uani 1 1 d . . . S1 S 0.6680(4) 1.0481(5) 0.4663(2) 0.194(3) Uani 1 1 d . . . S2 S 0.9333(3) 1.0749(3) 0.2272(3) 0.1385(16) Uani 1 1 d . . . S3 S 0.4086(3) 1.1552(3) 0.1563(3) 0.1332(14) Uani 1 1 d . . . S4 S 0.8399(3) 0.5864(3) 0.3377(3) 0.1489(17) Uani 1 1 d . . . P1 P 0.2246(2) 0.5789(2) 0.21944(14) 0.0649(6) Uani 1 1 d . . . P2 P 0.40858(19) 0.77635(18) 0.27863(12) 0.0566(6) Uani 1 1 d . . . N1 N 0.5280(6) 0.4754(6) 0.2497(4) 0.0656(19) Uani 1 1 d . . . N2 N 0.2654(6) 0.8299(6) 0.0995(4) 0.0676(19) Uani 1 1 d . . . N3 N 0.1592(6) 0.7314(6) 0.3932(4) 0.0683(19) Uani 1 1 d . . . N4 N 0.5095(10) 0.9468(12) 0.4242(6) 0.155(6) Uani 1 1 d . . . N5 N 0.7682(7) 1.0083(7) 0.3077(5) 0.084(2) Uani 1 1 d . . . N6 N 0.5525(9) 1.0331(8) 0.2684(6) 0.101(3) Uani 1 1 d . . . N7 N 0.7179(8) 0.8086(8) 0.3467(6) 0.096(3) Uani 1 1 d . . . C1 C 0.4476(8) 0.5527(7) 0.2504(5) 0.058(2) Uani 1 1 d . . . C2 C 0.6278(8) 0.3737(8) 0.2506(6) 0.076(3) Uani 1 1 d . . . C3 C 0.7044(16) 0.3974(17) 0.1879(17) 0.32(2) Uani 1 1 d . . . H3A H 0.6713 0.4142 0.1396 0.480 Uiso 1 1 calc R . . H3B H 0.7723 0.3339 0.1852 0.480 Uiso 1 1 calc R . . H3C H 0.7197 0.4598 0.1978 0.480 Uiso 1 1 calc R . . C4 C 0.6729(18) 0.3435(17) 0.3192(10) 0.304(19) Uani 1 1 d . . . H4A H 0.6752 0.4074 0.3379 0.457 Uiso 1 1 calc R . . H4B H 0.7468 0.2895 0.3127 0.457 Uiso 1 1 calc R . . H4C H 0.6287 0.3121 0.3559 0.457 Uiso 1 1 calc R . . C5 C 0.6054(15) 0.2898(12) 0.2217(19) 0.32(2) Uani 1 1 d . . . H5A H 0.5604 0.3220 0.1789 0.486 Uiso 1 1 calc R . . H5B H 0.5667 0.2568 0.2619 0.486 Uiso 1 1 calc R . . H5C H 0.6740 0.2340 0.2048 0.486 Uiso 1 1 calc R . . C6 C 0.2834(7) 0.7728(7) 0.1562(5) 0.056(2) Uani 1 1 d . . . C7 C 0.2396(10) 0.9042(9) 0.0280(6) 0.086(3) Uani 1 1 d . . . C8 C 0.163(2) 0.8748(19) -0.0089(11) 0.276(16) Uani 1 1 d . . . H8A H 0.0975 0.8822 0.0257 0.414 Uiso 1 1 calc R . . H8B H 0.1978 0.7996 -0.0208 0.414 Uiso 1 1 calc R . . H8C H 0.1423 0.9234 -0.0557 0.414 Uiso 1 1 calc R . . C9 C 0.183(2) 1.0179(13) 0.0472(9) 0.250(14) Uani 1 1 d . . . H9A H 0.1168 1.0233 0.0804 0.375 Uiso 1 1 calc R . . H9B H 0.1635 1.0672 0.0006 0.375 Uiso 1 1 calc R . . H9C H 0.2311 1.0378 0.0734 0.375 Uiso 1 1 calc R . . C10 C 0.3380(16) 0.893(2) -0.0190(12) 0.35(2) Uani 1 1 d . . . H10A H 0.3732 0.8182 -0.0318 0.520 Uiso 1 1 calc R . . H10B H 0.3870 0.9103 0.0082 0.520 Uiso 1 1 calc R . . H10C H 0.3211 0.9430 -0.0657 0.520 Uiso 1 1 calc R . . C11 C 0.2205(7) 0.7116(7) 0.3384(5) 0.056(2) Uani 1 1 d . . . C12 C 0.0794(8) 0.7609(10) 0.4605(5) 0.077(3) Uani 1 1 d . . . C13 C 0.078(3) 0.650(2) 0.4995(15) 0.36(2) Uani 1 1 d . . . H13A H 0.1506 0.6029 0.5138 0.542 Uiso 1 1 calc R . . H13B H 0.0544 0.6154 0.4645 0.542 Uiso 1 1 calc R . . H13C H 0.0268 0.6616 0.5451 0.542 Uiso 1 1 calc R . . C14 C -0.0187(14) 0.834(2) 0.4389(9) 0.33(2) Uani 1 1 d . . . H14A H -0.0427 0.8059 0.4001 0.495 Uiso 1 1 calc R . . H14B H -0.0115 0.9031 0.4181 0.495 Uiso 1 1 calc R . . H14C H -0.0723 0.8454 0.4830 0.495 Uiso 1 1 calc R . . C15 C 0.1280(17) 0.790(3) 0.5150(11) 0.31(2) Uani 1 1 d . . . H15A H 0.1999 0.7334 0.5231 0.470 Uiso 1 1 calc R . . H15B H 0.0822 0.7962 0.5630 0.470 Uiso 1 1 calc R . . H15C H 0.1357 0.8593 0.4968 0.470 Uiso 1 1 calc R . . C16 C 0.0932(10) 0.6618(10) 0.1761(9) 0.121(5) Uani 1 1 d . . . H16A H 0.1124 0.6853 0.1228 0.145 Uiso 1 1 calc R . . H16B H 0.0555 0.6116 0.1744 0.145 Uiso 1 1 calc R . . C17 C 0.0166(11) 0.7536(11) 0.2063(8) 0.116(4) Uani 1 1 d . . . H17A H 0.0494 0.8091 0.2023 0.139 Uiso 1 1 calc R . . H17B H 0.0007 0.7336 0.2609 0.139 Uiso 1 1 calc R . . C18 C -0.0925(10) 0.8058(11) 0.1686(7) 0.115(4) Uani 1 1 d . . . H18A H -0.1407 0.8690 0.1940 0.173 Uiso 1 1 calc R . . H18B H -0.1272 0.7525 0.1732 0.173 Uiso 1 1 calc R . . H18C H -0.0786 0.8288 0.1149 0.173 Uiso 1 1 calc R . . C19 C 0.2946(11) 0.4872(11) 0.1471(7) 0.109(4) Uani 1 1 d . . . H19A H 0.3538 0.4254 0.1713 0.131 Uiso 1 1 calc R . . H19B H 0.2423 0.4575 0.1347 0.131 Uiso 1 1 calc R . . C20 C 0.3411(14) 0.5232(12) 0.0766(7) 0.136(5) Uani 1 1 d . . . H20A H 0.3990 0.5466 0.0872 0.163 Uiso 1 1 calc R . . H20B H 0.2843 0.5875 0.0524 0.163 Uiso 1 1 calc R . . C21 C 0.3900(17) 0.4367(13) 0.0196(8) 0.186(8) Uani 1 1 d . . . H21A H 0.4191 0.4682 -0.0272 0.279 Uiso 1 1 calc R . . H21B H 0.3332 0.4136 0.0079 0.279 Uiso 1 1 calc R . . H21C H 0.4485 0.3738 0.0421 0.279 Uiso 1 1 calc R . . C22 C 0.1887(12) 0.4897(12) 0.2966(8) 0.125(5) Uani 1 1 d . . . H22A H 0.1306 0.5367 0.3304 0.150 Uiso 1 1 calc R . . H22B H 0.1563 0.4473 0.2741 0.150 Uiso 1 1 calc R . . C23 C 0.2713(12) 0.4129(12) 0.3444(8) 0.128(5) Uani 1 1 d . . . H23A H 0.2989 0.4546 0.3717 0.154 Uiso 1 1 calc R . . H23B H 0.3328 0.3691 0.3111 0.154 Uiso 1 1 calc R . . C24 C 0.2347(14) 0.3350(12) 0.4029(8) 0.146(6) Uani 1 1 d . . . H24A H 0.2965 0.2853 0.4306 0.218 Uiso 1 1 calc R . . H24B H 0.2069 0.2930 0.3768 0.218 Uiso 1 1 calc R . . H24C H 0.1771 0.3767 0.4386 0.218 Uiso 1 1 calc R . . C25 C 0.5017(11) 0.7088(10) 0.3518(7) 0.109(4) Uani 1 1 d . . . H25A H 0.5651 0.6526 0.3279 0.131 Uiso 1 1 calc R . . H25B H 0.5283 0.7635 0.3640 0.131 Uiso 1 1 calc R . . C26 C 0.4727(12) 0.6578(11) 0.4225(7) 0.118(4) Uani 1 1 d . . . H26A H 0.4547 0.5965 0.4119 0.141 Uiso 1 1 calc R . . H26B H 0.4053 0.7107 0.4453 0.141 Uiso 1 1 calc R . . C27 C 0.5550(10) 0.6141(11) 0.4819(6) 0.111(4) Uani 1 1 d . . . H27A H 0.5245 0.5813 0.5273 0.167 Uiso 1 1 calc R . . H27B H 0.5718 0.6739 0.4951 0.167 Uiso 1 1 calc R . . H27C H 0.6215 0.5592 0.4615 0.167 Uiso 1 1 calc R . . C28 C 0.4988(11) 0.8132(12) 0.1999(7) 0.123(5) Uani 1 1 d . . . H28A H 0.4508 0.8749 0.1674 0.147 Uiso 1 1 calc R . . H28B H 0.5436 0.8420 0.2233 0.147 Uiso 1 1 calc R . . C29 C 0.5706(10) 0.7398(11) 0.1505(7) 0.111(4) Uani 1 1 d . . . H29A H 0.5271 0.7156 0.1221 0.133 Uiso 1 1 calc R . . H29B H 0.6170 0.6750 0.1816 0.133 Uiso 1 1 calc R . . C30 C 0.6448(11) 0.7821(13) 0.0933(7) 0.129(5) Uani 1 1 d . . . H30A H 0.6926 0.7238 0.0633 0.194 Uiso 1 1 calc R . . H30B H 0.6888 0.8063 0.1203 0.194 Uiso 1 1 calc R . . H30C H 0.6004 0.8432 0.0595 0.194 Uiso 1 1 calc R . . C31 C 0.3249(10) 0.9078(10) 0.3128(10) 0.133(6) Uani 1 1 d . . . H31A H 0.3049 0.8919 0.3674 0.160 Uiso 1 1 calc R . . H31B H 0.3738 0.9483 0.3102 0.160 Uiso 1 1 calc R . . C32 C 0.2264(10) 0.9837(9) 0.2812(8) 0.109(4) Uani 1 1 d . . . H32A H 0.1733 0.9475 0.2870 0.131 Uiso 1 1 calc R . . H32B H 0.2433 0.9996 0.2261 0.131 Uiso 1 1 calc R . . C33 C 0.1725(11) 1.0905(9) 0.3147(8) 0.123(5) Uani 1 1 d . . . H33A H 0.1081 1.1361 0.2880 0.185 Uiso 1 1 calc R . . H33B H 0.2236 1.1279 0.3092 0.185 Uiso 1 1 calc R . . H33C H 0.1507 1.0768 0.3686 0.185 Uiso 1 1 calc R . . C34 C 0.5630(14) 1.0502(16) 0.5303(8) 0.166(8) Uani 1 1 d . . . C35 C 0.8373(9) 1.0353(9) 0.2755(6) 0.085(3) Uani 1 1 d . . . C36 C 0.4937(10) 1.0840(10) 0.2224(8) 0.092(3) Uani 1 1 d . . . C37 C 0.7684(10) 0.7149(12) 0.3439(7) 0.098(3) Uani 1 1 d . . . Cl1 Cl 0.0000(12) 0.3927(11) 0.1804(8) 0.424(7) Uiso 1 1 d . . . Cl2 Cl -0.0009(14) 0.3366(13) 0.0451(10) 0.507(9) Uiso 1 1 d . . . C38 C 0.107(2) 0.300(2) 0.1114(15) 0.255(12) Uiso 1 1 d . . . H38A H 0.1666 0.3253 0.0913 0.306 Uiso 1 1 calc R . . H38B H 0.1349 0.2224 0.1315 0.306 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0493(6) 0.0543(6) 0.0485(6) -0.0091(4) -0.0053(4) -0.0217(5) Ni2 0.0802(9) 0.0923(9) 0.0735(8) -0.0275(7) 0.0094(7) -0.0502(8) S1 0.201(4) 0.376(8) 0.135(3) -0.158(4) 0.090(3) -0.235(5) S2 0.071(2) 0.128(3) 0.205(4) 0.018(3) 0.015(2) -0.047(2) S3 0.127(3) 0.119(3) 0.155(3) 0.028(2) -0.044(3) -0.054(2) S4 0.106(3) 0.090(2) 0.241(5) -0.011(3) -0.007(3) -0.031(2) P1 0.0661(15) 0.0687(15) 0.0704(15) -0.0125(12) -0.0097(12) -0.0337(13) P2 0.0576(14) 0.0618(13) 0.0578(13) -0.0139(10) -0.0042(11) -0.0277(11) N1 0.060(5) 0.060(5) 0.076(5) -0.016(4) -0.009(4) -0.018(4) N2 0.061(5) 0.077(5) 0.064(5) 0.000(4) -0.011(4) -0.025(4) N3 0.055(5) 0.085(5) 0.063(5) -0.006(4) -0.001(4) -0.025(4) N4 0.167(11) 0.280(15) 0.114(8) -0.121(9) 0.069(8) -0.178(12) N5 0.089(6) 0.086(6) 0.086(6) -0.015(5) 0.008(5) -0.044(5) N6 0.105(8) 0.098(7) 0.116(8) 0.007(6) -0.029(6) -0.057(6) N7 0.101(7) 0.080(6) 0.115(7) -0.006(6) 0.006(6) -0.049(6) C1 0.066(6) 0.058(5) 0.060(5) -0.010(4) -0.009(4) -0.031(5) C2 0.065(6) 0.072(6) 0.075(6) -0.020(5) -0.015(5) -0.001(5) C3 0.151(18) 0.17(2) 0.45(4) 0.05(2) 0.13(2) 0.069(15) C4 0.30(3) 0.26(2) 0.143(15) -0.103(15) -0.131(17) 0.20(2) C5 0.168(17) 0.082(10) 0.72(6) -0.18(2) -0.22(3) 0.065(11) C6 0.046(5) 0.072(6) 0.050(5) -0.015(4) 0.001(4) -0.022(4) C7 0.092(8) 0.097(8) 0.054(6) 0.016(5) -0.010(6) -0.024(6) C8 0.46(4) 0.32(3) 0.166(17) 0.158(19) -0.22(2) -0.28(3) C9 0.44(4) 0.094(11) 0.118(13) 0.022(10) -0.081(18) 0.014(17) C10 0.148(17) 0.46(4) 0.20(2) 0.23(3) 0.044(16) 0.02(2) C11 0.043(5) 0.067(5) 0.059(5) -0.009(4) -0.008(4) -0.021(4) C12 0.055(6) 0.114(8) 0.051(5) -0.008(5) 0.013(5) -0.024(6) C13 0.43(5) 0.32(4) 0.21(3) -0.01(2) 0.24(3) -0.11(3) C14 0.110(13) 0.55(5) 0.085(11) -0.014(18) 0.024(10) 0.12(2) C15 0.19(2) 0.70(6) 0.144(16) -0.25(3) 0.087(15) -0.22(3) C16 0.097(9) 0.100(9) 0.186(14) -0.048(9) -0.029(9) -0.040(8) C17 0.103(10) 0.100(9) 0.150(12) -0.016(8) -0.043(9) -0.032(8) C18 0.088(9) 0.149(12) 0.110(9) -0.021(8) -0.028(7) -0.036(8) C19 0.116(10) 0.138(11) 0.108(9) -0.053(8) -0.011(8) -0.071(9) C20 0.195(16) 0.131(11) 0.087(9) -0.030(8) 0.018(10) -0.071(11) C21 0.30(2) 0.148(14) 0.089(10) -0.052(9) 0.021(13) -0.061(16) C22 0.151(13) 0.146(12) 0.118(10) 0.018(9) -0.043(9) -0.103(11) C23 0.143(12) 0.135(11) 0.128(11) 0.034(9) -0.054(10) -0.080(10) C24 0.194(16) 0.137(12) 0.134(12) 0.043(10) -0.033(11) -0.109(12) C25 0.145(11) 0.113(9) 0.103(9) 0.031(7) -0.079(8) -0.079(9) C26 0.150(12) 0.131(11) 0.097(9) 0.018(8) -0.060(9) -0.075(10) C27 0.118(10) 0.155(12) 0.082(7) 0.016(7) -0.037(7) -0.074(9) C28 0.135(11) 0.183(14) 0.103(9) -0.053(9) 0.038(8) -0.118(11) C29 0.107(9) 0.142(11) 0.104(9) -0.049(8) 0.038(8) -0.071(9) C30 0.102(10) 0.193(15) 0.105(9) -0.029(9) 0.030(8) -0.075(10) C31 0.095(9) 0.084(8) 0.242(17) -0.079(10) -0.030(10) -0.030(7) C32 0.096(9) 0.087(8) 0.141(11) -0.037(8) -0.009(8) -0.021(7) C33 0.128(11) 0.070(7) 0.164(12) -0.044(8) -0.013(10) -0.017(7) C34 0.191(15) 0.32(2) 0.104(10) -0.134(13) 0.072(10) -0.204(17) C35 0.076(7) 0.081(7) 0.091(8) 0.008(6) -0.006(6) -0.028(6) C36 0.094(9) 0.088(8) 0.115(10) -0.021(7) 0.001(7) -0.058(7) C37 0.080(8) 0.112(10) 0.114(9) -0.002(8) -0.009(7) -0.053(8) _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 Ni1 C1 1.868(10) . ? Ni1 C11 1.870(9) . ? Ni1 C6 1.879(9) . ? Ni1 P2 2.227(2) . ? Ni1 P1 2.239(2) . ? Ni2 N7 1.980(10) . ? Ni2 N6 1.984(11) . ? Ni2 N5 1.997(9) . ? Ni2 N4 2.025(10) . ? Ni2 S1 2.414(3) . ? S1 C34 1.648(13) . ? S2 C35 1.629(12) . ? S3 C36 1.636(14) . ? S4 C37 1.599(15) . ? P1 C22 1.786(12) . ? P1 C19 1.791(11) . ? P1 C16 1.840(13) . ? P2 C25 1.779(10) . ? P2 C31 1.798(11) . ? P2 C28 1.825(11) . ? N1 C1 1.148(10) . ? N1 C2 1.467(11) . ? N2 C6 1.142(10) . ? N2 C7 1.457(11) . ? N3 C11 1.160(10) . ? N3 C12 1.460(11) . ? N4 C34 1.147(13) 2_676 ? N5 C35 1.145(12) . ? N6 C36 1.139(13) . ? N7 C37 1.157(14) . ? C2 C4 1.349(16) . ? C2 C5 1.420(17) . ? C2 C3 1.47(2) . ? C7 C10 1.403(19) . ? C7 C9 1.460(18) . ? C7 C8 1.460(19) . ? C12 C14 1.337(17) . ? C12 C15 1.388(19) . ? C12 C13 1.52(3) . ? C16 C17 1.365(16) . ? C17 C18 1.521(15) . ? C19 C20 1.400(16) . ? C20 C21 1.523(17) . ? C22 C23 1.428(16) . ? C23 C24 1.501(15) . ? C25 C26 1.395(15) . ? C26 C27 1.490(14) . ? C28 C29 1.380(15) . ? C29 C30 1.496(14) . ? C31 C32 1.415(15) . ? C32 C33 1.481(14) . ? C34 N4 1.147(13) 2_676 ? Cl1 C38 1.89(3) . ? Cl2 C38 1.82(2) . ? 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 C1 Ni1 C11 120.9(4) . . ? C1 Ni1 C6 119.1(4) . . ? C11 Ni1 C6 120.0(3) . . ? C1 Ni1 P2 89.4(2) . . ? C11 Ni1 P2 90.5(2) . . ? C6 Ni1 P2 89.0(3) . . ? C1 Ni1 P1 90.4(2) . . ? C11 Ni1 P1 89.4(2) . . ? C6 Ni1 P1 91.3(3) . . ? P2 Ni1 P1 179.69(11) . . ? N7 Ni2 N6 105.3(4) . . ? N7 Ni2 N5 93.9(4) . . ? N6 Ni2 N5 92.9(4) . . ? N7 Ni2 N4 93.8(5) . . ? N6 Ni2 N4 91.2(5) . . ? N5 Ni2 N4 170.0(4) . . ? N7 Ni2 S1 122.1(3) . . ? N6 Ni2 S1 132.6(3) . . ? N5 Ni2 S1 83.2(3) . . ? N4 Ni2 S1 87.3(3) . . ? C34 S1 Ni2 104.5(4) . . ? C22 P1 C19 102.8(7) . . ? C22 P1 C16 104.4(6) . . ? C19 P1 C16 100.8(6) . . ? C22 P1 Ni1 116.9(4) . . ? C19 P1 Ni1 115.3(4) . . ? C16 P1 Ni1 114.6(4) . . ? C25 P2 C31 103.5(7) . . ? C25 P2 C28 102.0(6) . . ? C31 P2 C28 102.8(7) . . ? C25 P2 Ni1 114.9(4) . . ? C31 P2 Ni1 116.0(4) . . ? C28 P2 Ni1 115.7(4) . . ? C1 N1 C2 177.5(9) . . ? C6 N2 C7 178.5(10) . . ? C11 N3 C12 177.5(9) . . ? C34 N4 Ni2 166.1(9) 2_676 . ? C35 N5 Ni2 176.3(9) . . ? C36 N6 Ni2 169.6(11) . . ? C37 N7 Ni2 174.3(11) . . ? N1 C1 Ni1 178.5(8) . . ? C4 C2 C5 115.1(17) . . ? C4 C2 C3 111.9(18) . . ? C5 C2 C3 101.2(17) . . ? C4 C2 N1 113.3(9) . . ? C5 C2 N1 109.3(9) . . ? C3 C2 N1 104.9(10) . . ? N2 C6 Ni1 178.6(8) . . ? C10 C7 N2 109.5(10) . . ? C10 C7 C9 110.8(17) . . ? N2 C7 C9 108.8(9) . . ? C10 C7 C8 112.4(17) . . ? N2 C7 C8 107.1(10) . . ? C9 C7 C8 108.1(16) . . ? N3 C11 Ni1 178.4(7) . . ? C14 C12 C15 117.2(19) . . ? C14 C12 N3 110.8(9) . . ? C15 C12 N3 108.5(10) . . ? C14 C12 C13 115(2) . . ? C15 C12 C13 100.6(17) . . ? N3 C12 C13 103.7(11) . . ? C17 C16 P1 122.5(10) . . ? C16 C17 C18 115.8(12) . . ? C20 C19 P1 121.8(10) . . ? C19 C20 C21 114.8(12) . . ? C23 C22 P1 120.3(10) . . ? C22 C23 C24 116.0(12) . . ? C26 C25 P2 123.6(10) . . ? C25 C26 C27 118.2(11) . . ? C29 C28 P2 123.9(10) . . ? C28 C29 C30 116.6(11) . . ? C32 C31 P2 124.7(10) . . ? C31 C32 C33 116.6(11) . . ? N4 C34 S1 178.5(10) 2_676 . ? N5 C35 S2 178.2(11) . . ? N6 C36 S3 179.0(11) . . ? N7 C37 S4 178.4(13) . . ? Cl2 C38 Cl1 88.6(13) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.915 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.091 #=========================================================END data_cnrncs _database_code_depnum_ccdc_archive 'CCDC 275743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H30 N3 P Pd S2' _chemical_formula_weight 465.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pca2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 13.5684(12) _cell_length_b 9.0189(5) _cell_length_c 18.6982(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2288.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 3.91 _cell_measurement_theta_max 12.45 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2285 _exptl_absorpt_correction_T_max 0.2961 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2079 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2079 _reflns_number_gt 1956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.1989P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(4) _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 0.01(4) _refine_ls_number_reflns 2079 _refine_ls_number_parameters 209 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.41751(2) 0.29445(3) -0.00055(3) 0.05267(14) Uani 1 1 d . . . S1 S 0.4367(2) 0.3838(4) -0.24852(12) 0.1235(9) Uani 1 1 d . . . S2 S 0.26817(10) 0.16722(16) -0.02746(9) 0.0698(4) Uani 1 1 d . . . P1 P 0.55911(8) 0.42707(13) 0.01667(7) 0.0542(3) Uani 1 1 d . . . N1 N 0.4154(4) 0.3546(8) -0.1032(3) 0.0798(15) Uani 1 1 d . . . N2 N 0.2039(5) 0.0126(8) 0.0939(4) 0.110(2) Uani 1 1 d . . . N3 N 0.4231(3) 0.1925(5) 0.1555(3) 0.0712(14) Uani 1 1 d . . . C1 C 0.6335(4) 0.3718(6) 0.0922(3) 0.0581(11) Uani 1 1 d . . . H1A H 0.5954 0.3870 0.1355 0.070 Uiso 1 1 calc R . . H1B H 0.6469 0.2665 0.0883 0.070 Uiso 1 1 calc R . . C2 C 0.7316(4) 0.4537(8) 0.0999(3) 0.0766(15) Uani 1 1 d . . . H2A H 0.7712 0.4383 0.0574 0.092 Uiso 1 1 calc R . . H2B H 0.7196 0.5592 0.1048 0.092 Uiso 1 1 calc R . . C3 C 0.7861(5) 0.3979(10) 0.1643(4) 0.097(2) Uani 1 1 d . . . H3A H 0.8476 0.4499 0.1687 0.145 Uiso 1 1 calc R . . H3B H 0.7987 0.2937 0.1590 0.145 Uiso 1 1 calc R . . H3C H 0.7471 0.4144 0.2063 0.145 Uiso 1 1 calc R . . C4 C 0.5302(4) 0.6216(6) 0.0334(4) 0.0731(15) Uani 1 1 d . . . H4A H 0.4908 0.6276 0.0766 0.088 Uiso 1 1 calc R . . H4B H 0.5914 0.6740 0.0424 0.088 Uiso 1 1 calc R . . C5 C 0.4767(6) 0.6999(6) -0.0250(4) 0.091(2) Uani 1 1 d . . . H5A H 0.4133 0.6526 -0.0328 0.109 Uiso 1 1 calc R . . H5B H 0.5143 0.6930 -0.0690 0.109 Uiso 1 1 calc R . . C6 C 0.4611(5) 0.8621(7) -0.0059(8) 0.125(3) Uani 1 1 d . . . H6A H 0.4265 0.9108 -0.0440 0.187 Uiso 1 1 calc R . . H6B H 0.5238 0.9091 0.0012 0.187 Uiso 1 1 calc R . . H6C H 0.4231 0.8688 0.0373 0.187 Uiso 1 1 calc R . . C7 C 0.6386(4) 0.4179(7) -0.0607(3) 0.0649(13) Uani 1 1 d . . . H7A H 0.6026 0.4533 -0.1021 0.078 Uiso 1 1 calc R . . H7B H 0.6943 0.4836 -0.0533 0.078 Uiso 1 1 calc R . . C8 C 0.6767(5) 0.2622(8) -0.0760(3) 0.0809(16) Uani 1 1 d . . . H8A H 0.7138 0.2273 -0.0349 0.097 Uiso 1 1 calc R . . H8B H 0.6211 0.1960 -0.0826 0.097 Uiso 1 1 calc R . . C9 C 0.7421(7) 0.2559(13) -0.1419(4) 0.111(2) Uani 1 1 d . . . H9A H 0.7641 0.1559 -0.1492 0.167 Uiso 1 1 calc R . . H9B H 0.7980 0.3195 -0.1352 0.167 Uiso 1 1 calc R . . H9C H 0.7053 0.2882 -0.1829 0.167 Uiso 1 1 calc R . . C10 C 0.4236(4) 0.3663(7) -0.1635(3) 0.0664(14) Uani 1 1 d . . . C11 C 0.2333(4) 0.0776(7) 0.0456(4) 0.0762(16) Uani 1 1 d . . . C12 C 0.4213(3) 0.2332(7) 0.0976(3) 0.0587(12) Uani 1 1 d . . . C13 C 0.4264(6) 0.1343(9) 0.2289(4) 0.090(2) Uani 1 1 d . . . C14 C 0.4074(14) -0.0273(14) 0.2227(7) 0.233(10) Uani 1 1 d . . . H14A H 0.4582 -0.0723 0.1943 0.349 Uiso 1 1 calc R . . H14B H 0.3446 -0.0431 0.2003 0.349 Uiso 1 1 calc R . . H14C H 0.4071 -0.0711 0.2695 0.349 Uiso 1 1 calc R . . C15 C 0.3549(13) 0.215(2) 0.2705(7) 0.246(12) Uani 1 1 d . . . H15A H 0.3727 0.3182 0.2718 0.369 Uiso 1 1 calc R . . H15B H 0.3534 0.1767 0.3183 0.369 Uiso 1 1 calc R . . H15C H 0.2910 0.2048 0.2491 0.369 Uiso 1 1 calc R . . C16 C 0.5312(9) 0.1533(18) 0.2551(6) 0.166(6) Uani 1 1 d . . . H16A H 0.5749 0.0971 0.2252 0.249 Uiso 1 1 calc R . . H16B H 0.5362 0.1187 0.3035 0.249 Uiso 1 1 calc R . . H16C H 0.5490 0.2563 0.2531 0.249 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.05349(19) 0.05073(19) 0.0538(2) 0.00125(18) -0.00282(18) 0.00069(12) S1 0.1468(18) 0.162(2) 0.0619(10) 0.0212(14) 0.0080(11) 0.0203(17) S2 0.0621(7) 0.0665(7) 0.0807(9) -0.0067(7) -0.0125(6) -0.0037(6) P1 0.0510(5) 0.0516(6) 0.0600(8) 0.0061(5) 0.0003(5) 0.0006(4) N1 0.079(3) 0.097(4) 0.063(3) 0.007(3) -0.012(2) -0.014(3) N2 0.104(4) 0.103(4) 0.124(5) 0.014(4) -0.001(4) -0.032(4) N3 0.079(3) 0.068(3) 0.067(3) 0.009(2) -0.003(2) -0.018(2) C1 0.059(3) 0.057(3) 0.058(3) 0.005(2) -0.001(2) -0.001(2) C2 0.060(3) 0.094(4) 0.076(3) 0.004(3) -0.005(3) -0.005(3) C3 0.075(4) 0.114(5) 0.102(5) 0.004(4) -0.027(4) 0.001(4) C4 0.060(3) 0.060(3) 0.100(4) 0.005(3) -0.005(3) -0.003(2) C5 0.088(4) 0.076(4) 0.107(6) 0.008(3) -0.006(4) 0.020(3) C6 0.096(4) 0.065(3) 0.213(11) 0.001(7) -0.035(7) 0.030(3) C7 0.062(3) 0.073(3) 0.060(3) 0.012(3) 0.001(2) -0.002(3) C8 0.077(4) 0.101(4) 0.065(4) -0.001(4) 0.011(3) 0.007(4) C9 0.097(5) 0.159(6) 0.078(5) -0.029(5) 0.016(4) -0.017(6) C10 0.065(3) 0.073(4) 0.061(4) 0.006(3) -0.006(2) -0.002(2) C11 0.068(3) 0.061(3) 0.100(5) -0.004(3) -0.007(3) -0.012(3) C12 0.064(3) 0.051(3) 0.061(3) 0.004(3) -0.003(2) -0.009(2) C13 0.121(6) 0.092(5) 0.058(3) 0.024(4) -0.014(3) -0.035(4) C14 0.41(3) 0.143(10) 0.148(11) 0.087(10) -0.102(13) -0.119(13) C15 0.25(2) 0.39(3) 0.106(9) 0.097(14) 0.080(11) 0.13(2) C16 0.161(10) 0.232(14) 0.105(7) 0.060(9) -0.042(8) -0.073(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C12 1.917(6) . ? Pd1 N1 1.995(6) . ? Pd1 P1 2.2860(12) . ? Pd1 S2 2.3824(14) . ? S1 C10 1.607(6) . ? S2 C11 1.656(8) . ? P1 C7 1.805(5) . ? P1 C1 1.806(5) . ? P1 C4 1.824(6) . ? N1 C10 1.138(9) . ? N2 C11 1.148(9) . ? N3 C12 1.143(9) . ? N3 C13 1.471(9) . ? C1 C2 1.529(8) . ? C2 C3 1.500(9) . ? C4 C5 1.489(9) . ? C5 C6 1.521(9) . ? C7 C8 1.524(9) . ? C8 C9 1.519(10) . ? C13 C15 1.441(16) . ? C13 C14 1.485(16) . ? C13 C16 1.513(12) . ? 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 C12 Pd1 N1 178.8(3) . . ? C12 Pd1 P1 89.63(15) . . ? N1 Pd1 P1 90.30(15) . . ? C12 Pd1 S2 94.94(15) . . ? N1 Pd1 S2 85.15(15) . . ? P1 Pd1 S2 175.28(6) . . ? C11 S2 Pd1 107.7(2) . . ? C7 P1 C1 106.3(2) . . ? C7 P1 C4 108.0(3) . . ? C1 P1 C4 104.6(3) . . ? C7 P1 Pd1 111.4(2) . . ? C1 P1 Pd1 115.80(17) . . ? C4 P1 Pd1 110.29(17) . . ? C10 N1 Pd1 167.7(6) . . ? C12 N3 C13 177.8(7) . . ? C2 C1 P1 115.3(4) . . ? C3 C2 C1 110.1(5) . . ? C5 C4 P1 115.8(5) . . ? C4 C5 C6 110.6(8) . . ? C8 C7 P1 113.3(4) . . ? C9 C8 C7 112.7(7) . . ? N1 C10 S1 179.2(6) . . ? N2 C11 S2 175.7(6) . . ? N3 C12 Pd1 178.0(5) . . ? C15 C13 N3 107.6(8) . . ? C15 C13 C14 115.0(12) . . ? N3 C13 C14 105.8(8) . . ? C15 C13 C16 113.6(12) . . ? N3 C13 C16 106.8(6) . . ? C14 C13 C16 107.4(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.335 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.055 #=========================================================END data_isomers _database_code_depnum_ccdc_archive 'CCDC 275744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H42 N2 P2 Pd S2' _chemical_formula_weight 543.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7268(9) _cell_length_b 9.3401(12) _cell_length_c 17.114(2) _cell_angle_alpha 89.676(9) _cell_angle_beta 86.225(9) _cell_angle_gamma 87.750(10) _cell_volume 1390.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.94 _cell_measurement_theta_max 12.48 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6359 _exptl_absorpt_correction_T_max 0.8930 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5192 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4843 _reflns_number_gt 3783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.6258P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4843 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.0000 0.05224(12) Uani 1 2 d S . . S1 S 0.19903(17) 0.18558(14) -0.13450(9) 0.1028(4) Uani 1 1 d . . . P1 P 0.33589(11) 0.69915(10) -0.01450(5) 0.0553(2) Uani 1 1 d . . . N1 N 0.3700(4) 0.3741(4) -0.0583(2) 0.0719(9) Uani 1 1 d . . . C1 C 0.2994(4) 0.2966(4) -0.0897(2) 0.0624(9) Uani 1 1 d . . . C2 C 0.2868(5) 0.7880(4) 0.0783(2) 0.0667(10) Uani 1 1 d . . . H2A H 0.3772 0.8333 0.0951 0.080 Uiso 1 1 calc R . . H2B H 0.2091 0.8629 0.0707 0.080 Uiso 1 1 calc R . . C3 C 0.2267(6) 0.6866(5) 0.1436(2) 0.0856(13) Uani 1 1 d . . . H3A H 0.1321 0.6466 0.1285 0.103 Uiso 1 1 calc R . . H3B H 0.3013 0.6080 0.1489 0.103 Uiso 1 1 calc R . . C4 C 0.1971(7) 0.7589(6) 0.2208(3) 0.1157(18) Uani 1 1 d . . . H4A H 0.1594 0.6909 0.2590 0.174 Uiso 1 1 calc R . . H4B H 0.1219 0.8358 0.2163 0.174 Uiso 1 1 calc R . . H4C H 0.2909 0.7964 0.2369 0.174 Uiso 1 1 calc R . . C5 C 0.4272(4) 0.8326(4) -0.0770(2) 0.0610(9) Uani 1 1 d . . . H5A H 0.3594 0.9174 -0.0780 0.073 Uiso 1 1 calc R . . H5B H 0.5210 0.8596 -0.0545 0.073 Uiso 1 1 calc R . . C6 C 0.4661(5) 0.7829(5) -0.1607(2) 0.0800(12) Uani 1 1 d . . . H6A H 0.5350 0.6989 -0.1599 0.096 Uiso 1 1 calc R . . H6B H 0.3727 0.7552 -0.1833 0.096 Uiso 1 1 calc R . . C7 C 0.5404(6) 0.8959(5) -0.2117(3) 0.0944(14) Uani 1 1 d . . . H7A H 0.5625 0.8588 -0.2636 0.142 Uiso 1 1 calc R . . H7B H 0.6342 0.9224 -0.1903 0.142 Uiso 1 1 calc R . . H7C H 0.4719 0.9786 -0.2138 0.142 Uiso 1 1 calc R . . C8 C 0.1546(4) 0.6615(4) -0.0556(2) 0.0648(9) Uani 1 1 d . . . H8A H 0.1775 0.6106 -0.1045 0.078 Uiso 1 1 calc R . . H8B H 0.0996 0.5972 -0.0201 0.078 Uiso 1 1 calc R . . C9 C 0.0480(5) 0.7884(5) -0.0714(3) 0.0825(12) Uani 1 1 d . . . H9A H 0.0206 0.8384 -0.0226 0.099 Uiso 1 1 calc R . . H9B H 0.1014 0.8542 -0.1066 0.099 Uiso 1 1 calc R . . C10 C -0.0964(5) 0.7450(6) -0.1069(3) 0.1049(17) Uani 1 1 d . . . H10A H -0.1600 0.8288 -0.1161 0.157 Uiso 1 1 calc R . . H10B H -0.1512 0.6818 -0.0716 0.157 Uiso 1 1 calc R . . H10C H -0.0700 0.6967 -0.1556 0.157 Uiso 1 1 calc R . . Pd2 Pd 0.5000 0.0000 -0.5000 0.04984(12) Uani 1 2 d S . . S2 S 0.67242(12) 0.08724(13) -0.41462(6) 0.0758(3) Uani 1 1 d . . . P2 P 0.30263(11) 0.16428(10) -0.45602(5) 0.0557(2) Uani 1 1 d . . . N2 N 0.7850(7) 0.3214(6) -0.4995(4) 0.148(2) Uani 1 1 d . . . C11 C 0.7359(6) 0.2246(6) -0.4662(3) 0.0916(15) Uani 1 1 d . . . C12 C 0.1425(4) 0.0688(4) -0.4101(2) 0.0633(9) Uani 1 1 d . . . H12A H 0.0608 0.1375 -0.3933 0.076 Uiso 1 1 calc R . . H12B H 0.1029 0.0061 -0.4483 0.076 Uiso 1 1 calc R . . C13 C 0.1883(5) -0.0201(5) -0.3396(2) 0.0796(12) Uani 1 1 d . . . H13A H 0.2767 -0.0819 -0.3554 0.095 Uiso 1 1 calc R . . H13B H 0.2188 0.0438 -0.2995 0.095 Uiso 1 1 calc R . . C14 C 0.0637(6) -0.1095(6) -0.3058(3) 0.1062(16) Uani 1 1 d . . . H14A H 0.0994 -0.1626 -0.2619 0.159 Uiso 1 1 calc R . . H14B H 0.0345 -0.1749 -0.3448 0.159 Uiso 1 1 calc R . . H14C H -0.0234 -0.0490 -0.2888 0.159 Uiso 1 1 calc R . . C15 C 0.3488(4) 0.2985(4) -0.3847(2) 0.0668(10) Uani 1 1 d . . . H15A H 0.3955 0.2494 -0.3417 0.080 Uiso 1 1 calc R . . H15B H 0.4252 0.3597 -0.4094 0.080 Uiso 1 1 calc R . . C16 C 0.2154(6) 0.3929(5) -0.3513(3) 0.0915(14) Uani 1 1 d . . . H16A H 0.1394 0.3329 -0.3251 0.110 Uiso 1 1 calc R . . H16B H 0.1674 0.4423 -0.3938 0.110 Uiso 1 1 calc R . . C17 C 0.2639(7) 0.5028(5) -0.2935(3) 0.1129(18) Uani 1 1 d . . . H17A H 0.1756 0.5599 -0.2744 0.169 Uiso 1 1 calc R . . H17B H 0.3379 0.5636 -0.3193 0.169 Uiso 1 1 calc R . . H17C H 0.3089 0.4545 -0.2504 0.169 Uiso 1 1 calc R . . C18 C 0.2218(5) 0.2663(4) -0.5356(2) 0.0692(10) Uani 1 1 d . . . H18A H 0.1707 0.2012 -0.5684 0.083 Uiso 1 1 calc R . . H18B H 0.1445 0.3347 -0.5135 0.083 Uiso 1 1 calc R . . C19 C 0.3375(6) 0.3459(5) -0.5861(3) 0.0897(13) Uani 1 1 d . . . H19A H 0.4189 0.2790 -0.6055 0.108 Uiso 1 1 calc R . . H19B H 0.3830 0.4167 -0.5545 0.108 Uiso 1 1 calc R . . C20 C 0.2684(7) 0.4199(6) -0.6547(3) 0.120(2) Uani 1 1 d . . . H20A H 0.3470 0.4686 -0.6851 0.180 Uiso 1 1 calc R . . H20B H 0.1895 0.4881 -0.6360 0.180 Uiso 1 1 calc R . . H20C H 0.2248 0.3502 -0.6868 0.180 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0531(2) 0.0506(2) 0.0538(2) -0.00629(16) -0.00920(17) -0.00271(16) S1 0.1019(9) 0.0911(9) 0.1207(11) -0.0261(7) -0.0381(8) -0.0161(7) P1 0.0571(5) 0.0534(5) 0.0557(5) -0.0038(4) -0.0068(4) -0.0002(4) N1 0.070(2) 0.0636(19) 0.083(2) -0.0107(17) -0.0104(18) -0.0007(17) C1 0.058(2) 0.055(2) 0.075(2) -0.0068(18) -0.0168(19) 0.0063(17) C2 0.074(2) 0.064(2) 0.061(2) -0.0103(18) -0.0044(19) 0.0057(19) C3 0.095(3) 0.091(3) 0.069(3) -0.002(2) 0.010(2) 0.003(3) C4 0.143(5) 0.128(5) 0.073(3) 0.001(3) 0.011(3) -0.001(4) C5 0.060(2) 0.057(2) 0.067(2) -0.0018(17) -0.0068(18) -0.0046(17) C6 0.087(3) 0.085(3) 0.068(3) -0.003(2) 0.001(2) -0.014(2) C7 0.092(3) 0.121(4) 0.069(3) 0.013(3) 0.002(2) -0.008(3) C8 0.058(2) 0.069(2) 0.068(2) 0.0005(18) -0.0098(18) -0.0032(18) C9 0.070(3) 0.092(3) 0.086(3) 0.006(2) -0.014(2) 0.008(2) C10 0.060(3) 0.141(5) 0.115(4) 0.029(3) -0.017(3) -0.005(3) Pd2 0.0460(2) 0.0556(2) 0.0486(2) -0.00604(16) -0.00711(16) -0.00406(16) S2 0.0675(6) 0.0904(8) 0.0721(6) -0.0195(5) -0.0220(5) -0.0052(5) P2 0.0525(5) 0.0598(5) 0.0547(5) -0.0050(4) -0.0039(4) 0.0004(4) N2 0.149(5) 0.107(4) 0.188(6) -0.009(4) 0.009(4) -0.044(4) C11 0.074(3) 0.087(3) 0.114(4) -0.034(3) -0.011(3) -0.006(3) C12 0.055(2) 0.070(2) 0.065(2) -0.0032(18) -0.0029(17) -0.0025(17) C13 0.086(3) 0.094(3) 0.060(2) 0.001(2) -0.008(2) -0.019(2) C14 0.112(4) 0.109(4) 0.096(4) 0.018(3) 0.009(3) -0.011(3) C15 0.070(2) 0.065(2) 0.066(2) -0.0110(18) -0.0027(19) -0.0049(19) C16 0.102(3) 0.077(3) 0.093(3) -0.019(2) 0.012(3) 0.003(3) C17 0.147(5) 0.080(3) 0.109(4) -0.032(3) 0.018(4) -0.001(3) C18 0.069(2) 0.073(2) 0.065(2) 0.0010(19) -0.0096(19) 0.013(2) C19 0.102(4) 0.088(3) 0.077(3) 0.021(2) -0.003(3) 0.002(3) C20 0.152(5) 0.109(4) 0.096(4) 0.036(3) -0.002(4) 0.012(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 Pd1 N1 1.983(3) . ? Pd1 N1 1.983(3) 2_665 ? Pd1 P1 2.3248(10) 2_665 ? Pd1 P1 2.3248(10) . ? S1 C1 1.612(4) . ? P1 C5 1.812(4) . ? P1 C2 1.815(4) . ? P1 C8 1.821(4) . ? N1 C1 1.130(5) . ? C2 C3 1.540(6) . ? C3 C4 1.490(6) . ? C5 C6 1.520(5) . ? C6 C7 1.506(6) . ? C8 C9 1.512(5) . ? C9 C10 1.504(6) . ? Pd2 S2 2.3371(10) 2_654 ? Pd2 S2 2.3371(10) . ? Pd2 P2 2.3500(10) 2_654 ? Pd2 P2 2.3500(10) . ? S2 C11 1.646(6) . ? P2 C12 1.820(4) . ? P2 C18 1.823(4) . ? P2 C15 1.829(4) . ? N2 C11 1.148(6) . ? C12 C13 1.526(5) . ? C13 C14 1.482(6) . ? C15 C16 1.516(5) . ? C16 C17 1.521(6) . ? C18 C19 1.502(6) . ? C19 C20 1.507(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 Pd1 N1 180.00(17) . 2_665 ? N1 Pd1 P1 87.16(10) . 2_665 ? N1 Pd1 P1 92.84(10) 2_665 2_665 ? N1 Pd1 P1 92.84(10) . . ? N1 Pd1 P1 87.16(10) 2_665 . ? P1 Pd1 P1 180.00(5) 2_665 . ? C5 P1 C2 105.55(17) . . ? C5 P1 C8 106.96(18) . . ? C2 P1 C8 106.34(19) . . ? C5 P1 Pd1 110.94(13) . . ? C2 P1 Pd1 111.67(13) . . ? C8 P1 Pd1 114.81(13) . . ? C1 N1 Pd1 176.5(3) . . ? N1 C1 S1 179.8(4) . . ? C3 C2 P1 113.7(3) . . ? C4 C3 C2 113.2(4) . . ? C6 C5 P1 114.0(3) . . ? C7 C6 C5 113.0(4) . . ? C9 C8 P1 117.1(3) . . ? C10 C9 C8 112.4(4) . . ? S2 Pd2 S2 180.0 2_654 . ? S2 Pd2 P2 92.93(4) 2_654 2_654 ? S2 Pd2 P2 87.07(4) . 2_654 ? S2 Pd2 P2 87.07(4) 2_654 . ? S2 Pd2 P2 92.93(4) . . ? P2 Pd2 P2 180.00(4) 2_654 . ? C11 S2 Pd2 99.80(18) . . ? C12 P2 C18 105.08(18) . . ? C12 P2 C15 105.62(18) . . ? C18 P2 C15 105.08(19) . . ? C12 P2 Pd2 109.84(13) . . ? C18 P2 Pd2 112.77(13) . . ? C15 P2 Pd2 117.51(13) . . ? N2 C11 S2 176.7(6) . . ? C13 C12 P2 112.5(3) . . ? C14 C13 C12 113.5(4) . . ? C16 C15 P2 116.2(3) . . ? C15 C16 C17 112.8(4) . . ? C19 C18 P2 114.4(3) . . ? C18 C19 C20 112.8(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.413 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.056 #=========================================================END data_lee192 _database_code_depnum_ccdc_archive 'CCDC 275745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 N4 P2 Pd S2' _chemical_formula_weight 789.23 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.029(4) _cell_length_b 11.899(3) _cell_length_c 17.761(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.217(16) _cell_angle_gamma 90.00 _cell_volume 2063.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.98 _cell_measurement_theta_max 12.57 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.658 #_exptl_absorpt_correction_type ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6940 _exptl_absorpt_correction_T_max 0.8993 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4019 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0330 _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 -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3795 _reflns_number_gt 3569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.4851P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 3795 _refine_ls_number_parameters 424 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -1.29101(3) -0.54640(3) -0.250297(17) 0.04289(10) Uani 1 1 d . . . S1 S -0.9528(4) -0.2862(4) -0.2968(2) 0.1610(14) Uani 1 1 d . . . S2 S -1.4666(2) -0.74578(16) -0.23499(16) 0.0983(7) Uani 1 1 d . . . P1 P -1.47614(13) -0.43607(11) -0.31696(7) 0.0501(3) Uani 1 1 d . . . P2 P -1.08306(13) -0.62414(11) -0.18031(7) 0.0478(3) Uani 1 1 d . . . N1 N -1.3520(4) -0.4427(4) -0.1001(2) 0.0567(10) Uani 1 1 d . . . N2 N -1.1862(5) -0.6049(5) -0.3982(3) 0.0650(12) Uani 1 1 d . . . N3 N -1.1275(14) -0.1912(12) -0.4001(8) 0.172(6) Uani 1 1 d . . . N4 N -1.5841(7) -0.6487(8) -0.1212(4) 0.106(2) Uani 1 1 d . . . C1 C -1.4968(6) -0.4297(5) -0.4219(3) 0.0604(13) Uani 1 1 d . . . C2 C -1.4323(9) -0.3472(7) -0.4551(4) 0.090(2) Uani 1 1 d . . . H2 H -1.3789 -0.2937 -0.4239 0.108 Uiso 1 1 calc R . . C3 C -1.4465(11) -0.3432(8) -0.5356(4) 0.111(3) Uani 1 1 d . . . H3 H -1.4035 -0.2869 -0.5576 0.133 Uiso 1 1 calc R . . C4 C -1.5227(12) -0.4213(9) -0.5806(4) 0.118(4) Uani 1 1 d . . . H4 H -1.5315 -0.4188 -0.6338 0.142 Uiso 1 1 calc R . . C5 C -1.5874(12) -0.5040(8) -0.5497(5) 0.119(4) Uani 1 1 d . . . H5 H -1.6401 -0.5574 -0.5815 0.143 Uiso 1 1 calc R . . C6 C -1.5738(9) -0.5078(6) -0.4703(4) 0.093(2) Uani 1 1 d . . . H6 H -1.6177 -0.5644 -0.4493 0.112 Uiso 1 1 calc R . . C7 C -1.4546(6) -0.2913(4) -0.2821(3) 0.0565(13) Uani 1 1 d . . . C8 C -1.3267(8) -0.2471(6) -0.2557(3) 0.0717(16) Uani 1 1 d . . . H8 H -1.2501 -0.2904 -0.2571 0.086 Uiso 1 1 calc R . . C9 C -1.3097(11) -0.1373(7) -0.2266(4) 0.104(3) Uani 1 1 d . . . H9 H -1.2222 -0.1084 -0.2078 0.125 Uiso 1 1 calc R . . C10 C -1.4220(16) -0.0727(6) -0.2261(5) 0.124(4) Uani 1 1 d . . . H10 H -1.4113 0.0007 -0.2077 0.149 Uiso 1 1 calc R . . C11 C -1.5511(14) -0.1165(8) -0.2527(6) 0.120(4) Uani 1 1 d . . . H11 H -1.6276 -0.0733 -0.2510 0.144 Uiso 1 1 calc R . . C12 C -1.5672(9) -0.2232(7) -0.2816(5) 0.090(2) Uani 1 1 d . . . H12 H -1.6550 -0.2509 -0.3014 0.108 Uiso 1 1 calc R . . C13 C -1.6397(6) -0.4858(7) -0.3005(4) 0.0812(19) Uani 1 1 d . . . H13A H -1.6548 -0.5619 -0.3182 0.122 Uiso 1 1 calc R . . H13B H -1.7124 -0.4390 -0.3284 0.122 Uiso 1 1 calc R . . H13C H -1.6376 -0.4824 -0.2462 0.122 Uiso 1 1 calc R . . C14 C -1.0795(6) -0.6521(6) -0.0786(3) 0.0704(17) Uani 1 1 d . . . C15 C -1.0200(10) -0.5774(9) -0.0212(4) 0.112(3) Uani 1 1 d . . . H15 H -0.9770 -0.5129 -0.0334 0.135 Uiso 1 1 calc R . . C16 C -1.0252(15) -0.5998(15) 0.0567(5) 0.168(7) Uani 1 1 d . . . H16 H -0.9863 -0.5492 0.0954 0.202 Uiso 1 1 calc R . . C17 C -1.0860(19) -0.6939(19) 0.0750(7) 0.195(10) Uani 1 1 d . . . H17 H -1.0872 -0.7086 0.1262 0.234 Uiso 1 1 calc R . . C18 C -1.1449(12) -0.7667(13) 0.0191(7) 0.141(5) Uani 1 1 d . . . H18 H -1.1863 -0.8314 0.0324 0.170 Uiso 1 1 calc R . . C19 C -1.1449(8) -0.7463(9) -0.0590(5) 0.102(3) Uani 1 1 d . . . H19 H -1.1887 -0.7959 -0.0972 0.123 Uiso 1 1 calc R . . C20 C -1.0288(5) -0.7535(5) -0.2187(3) 0.0531(11) Uani 1 1 d . . . C21 C -1.1235(6) -0.8303(5) -0.2583(4) 0.0665(15) Uani 1 1 d . . . H21 H -1.2167 -0.8153 -0.2664 0.080 Uiso 1 1 calc R . . C22 C -1.0795(7) -0.9294(6) -0.2858(4) 0.0834(19) Uani 1 1 d . . . H22 H -1.1433 -0.9814 -0.3113 0.100 Uiso 1 1 calc R . . C23 C -0.9408(8) -0.9512(7) -0.2755(5) 0.093(2) Uani 1 1 d . . . H23 H -0.9114 -1.0181 -0.2935 0.112 Uiso 1 1 calc R . . C24 C -0.8473(7) -0.8737(7) -0.2388(4) 0.088(2) Uani 1 1 d . . . H24 H -0.7542 -0.8869 -0.2335 0.106 Uiso 1 1 calc R . . C25 C -0.8902(6) -0.7766(6) -0.2097(4) 0.0777(19) Uani 1 1 d . . . H25 H -0.8256 -0.7256 -0.1837 0.093 Uiso 1 1 calc R . . C26 C -0.9466(7) -0.5228(5) -0.1793(4) 0.081(2) Uani 1 1 d . . . H26A H -0.9703 -0.4523 -0.1595 0.121 Uiso 1 1 calc R . . H26B H -0.9347 -0.5123 -0.2310 0.121 Uiso 1 1 calc R . . H26C H -0.8629 -0.5502 -0.1470 0.121 Uiso 1 1 calc R . . C27 C -1.3291(5) -0.4842(4) -0.1535(3) 0.0491(11) Uani 1 1 d . . . C28 C -1.3835(7) -0.3785(6) -0.0342(3) 0.0709(16) Uani 1 1 d . . . C29 C -1.2676(10) -0.2947(9) -0.0106(6) 0.125(4) Uani 1 1 d . . . H29A H -1.2657 -0.2457 -0.0532 0.188 Uiso 1 1 calc R . . H29B H -1.1821 -0.3342 0.0040 0.188 Uiso 1 1 calc R . . H29C H -1.2815 -0.2511 0.0325 0.188 Uiso 1 1 calc R . . C30 C -1.3955(10) -0.4584(9) 0.0283(4) 0.112(3) Uani 1 1 d . . . H30A H -1.3092 -0.4952 0.0473 0.168 Uiso 1 1 calc R . . H30B H -1.4644 -0.5135 0.0082 0.168 Uiso 1 1 calc R . . H30C H -1.4207 -0.4181 0.0698 0.168 Uiso 1 1 calc R . . C31 C -1.5155(9) -0.3177(10) -0.0659(5) 0.118(3) Uani 1 1 d . . . H31A H -1.5038 -0.2672 -0.1061 0.178 Uiso 1 1 calc R . . H31B H -1.5412 -0.2757 -0.0253 0.178 Uiso 1 1 calc R . . H31C H -1.5860 -0.3712 -0.0867 0.178 Uiso 1 1 calc R . . C32 C -1.2303(5) -0.5853(5) -0.3460(3) 0.0550(13) Uani 1 1 d . . . C33 C -1.1173(7) -0.6333(7) -0.4613(3) 0.0787(19) Uani 1 1 d . . . C34 C -1.1881(16) -0.7271(18) -0.5035(8) 0.246(12) Uani 1 1 d . . . H34A H -1.2818 -0.7068 -0.5249 0.369 Uiso 1 1 calc R . . H34B H -1.1849 -0.7899 -0.4693 0.369 Uiso 1 1 calc R . . H34C H -1.1449 -0.7470 -0.5446 0.369 Uiso 1 1 calc R . . C35 C -0.9752(10) -0.653(2) -0.4268(6) 0.222(10) Uani 1 1 d . . . H35A H -0.9356 -0.5872 -0.3998 0.333 Uiso 1 1 calc R . . H35B H -0.9279 -0.6715 -0.4665 0.333 Uiso 1 1 calc R . . H35C H -0.9672 -0.7149 -0.3911 0.333 Uiso 1 1 calc R . . C36 C -1.134(2) -0.537(2) -0.5141(10) 0.313(16) Uani 1 1 d . . . H36A H -1.0873 -0.4727 -0.4872 0.469 Uiso 1 1 calc R . . H36B H -1.2291 -0.5198 -0.5322 0.469 Uiso 1 1 calc R . . H36C H -1.0948 -0.5543 -0.5573 0.469 Uiso 1 1 calc R . . C37 C -1.0718(13) -0.2564(17) -0.3658(7) 0.158(8) Uani 1 1 d . . . C38 C -1.5351(7) -0.6910(6) -0.1667(4) 0.0742(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04691(17) 0.04263(16) 0.03924(15) 0.00038(18) 0.01006(11) 0.00601(19) S1 0.168(3) 0.166(3) 0.169(3) 0.048(3) 0.079(3) 0.049(3) S2 0.0818(12) 0.0536(9) 0.168(2) -0.0100(12) 0.0453(13) -0.0093(9) P1 0.0473(6) 0.0460(7) 0.0532(7) 0.0055(5) 0.0033(5) 0.0034(5) P2 0.0458(6) 0.0473(7) 0.0491(6) -0.0009(5) 0.0083(5) 0.0041(5) N1 0.063(3) 0.061(3) 0.048(2) -0.010(2) 0.018(2) 0.008(2) N2 0.064(3) 0.084(3) 0.047(2) -0.002(2) 0.016(2) 0.006(2) N3 0.187(12) 0.186(12) 0.182(11) -0.074(10) 0.123(10) -0.082(10) N4 0.099(5) 0.145(7) 0.080(4) 0.019(4) 0.031(4) -0.038(5) C1 0.072(3) 0.048(3) 0.053(3) 0.001(2) -0.003(3) 0.007(3) C2 0.128(6) 0.085(5) 0.056(3) -0.003(3) 0.018(4) -0.017(5) C3 0.175(9) 0.095(6) 0.065(4) 0.007(4) 0.031(5) 0.002(6) C4 0.194(10) 0.092(6) 0.049(4) -0.006(4) -0.014(5) 0.048(7) C5 0.175(10) 0.079(5) 0.073(5) -0.023(4) -0.034(5) 0.018(6) C6 0.123(6) 0.067(4) 0.071(4) -0.006(3) -0.018(4) 0.001(4) C7 0.076(4) 0.039(3) 0.053(3) 0.006(2) 0.012(3) 0.012(3) C8 0.093(4) 0.054(3) 0.068(4) 0.003(3) 0.016(3) -0.010(3) C9 0.164(8) 0.063(4) 0.076(4) 0.002(4) 0.006(5) -0.026(6) C10 0.251(14) 0.048(5) 0.069(4) 0.001(3) 0.026(6) 0.018(6) C11 0.186(11) 0.069(6) 0.113(7) 0.008(5) 0.051(7) 0.061(6) C12 0.097(5) 0.078(5) 0.100(5) 0.006(4) 0.031(4) 0.037(4) C13 0.051(3) 0.081(4) 0.106(5) 0.029(4) 0.007(3) 0.002(3) C14 0.068(3) 0.093(5) 0.048(3) 0.012(3) 0.009(3) 0.034(4) C15 0.126(6) 0.136(10) 0.062(4) -0.011(4) -0.005(4) 0.042(6) C16 0.198(12) 0.246(19) 0.044(4) -0.010(6) -0.008(5) 0.117(13) C17 0.215(16) 0.30(2) 0.085(7) 0.087(11) 0.064(9) 0.171(17) C18 0.130(8) 0.192(13) 0.119(8) 0.085(9) 0.064(7) 0.069(9) C19 0.088(5) 0.134(7) 0.091(5) 0.053(5) 0.032(4) 0.035(5) C20 0.054(3) 0.051(3) 0.053(3) 0.002(2) 0.010(2) 0.007(2) C21 0.049(3) 0.049(3) 0.103(5) -0.007(3) 0.019(3) -0.001(2) C22 0.085(4) 0.057(4) 0.109(5) -0.022(4) 0.024(4) -0.006(3) C23 0.102(5) 0.070(4) 0.106(5) -0.021(4) 0.022(4) 0.029(4) C24 0.056(3) 0.096(5) 0.106(5) -0.031(4) 0.005(3) 0.025(4) C25 0.055(3) 0.079(4) 0.091(4) -0.021(4) -0.001(3) 0.017(3) C26 0.075(4) 0.061(5) 0.103(5) -0.012(3) 0.015(3) -0.019(3) C27 0.050(3) 0.047(3) 0.049(3) 0.006(2) 0.009(2) 0.006(2) C28 0.079(4) 0.079(4) 0.061(3) -0.020(3) 0.028(3) 0.010(3) C29 0.133(7) 0.139(8) 0.120(7) -0.081(7) 0.061(6) -0.046(7) C30 0.164(8) 0.116(7) 0.072(4) 0.002(5) 0.060(5) 0.012(7) C31 0.109(6) 0.154(9) 0.092(5) -0.028(5) 0.022(5) 0.066(6) C32 0.051(3) 0.065(3) 0.050(3) 0.001(2) 0.013(2) 0.003(2) C33 0.077(4) 0.116(6) 0.051(3) 0.001(4) 0.030(3) 0.014(4) C34 0.224(15) 0.37(3) 0.189(13) -0.193(18) 0.146(13) -0.136(17) C35 0.087(6) 0.49(3) 0.103(7) -0.054(13) 0.044(5) 0.033(12) C36 0.53(4) 0.27(2) 0.250(17) 0.154(19) 0.31(2) 0.20(3) C37 0.119(8) 0.28(2) 0.096(7) 0.088(10) 0.063(6) 0.058(11) C38 0.064(4) 0.073(4) 0.082(4) 0.023(3) 0.008(3) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C32 1.987(5) . ? Pd1 C27 1.987(5) . ? Pd1 P2 2.3590(14) . ? Pd1 P1 2.3596(14) . ? S1 C37 1.544(12) . ? S2 C38 1.657(9) . ? P1 C7 1.827(5) . ? P1 C13 1.829(6) . ? P1 C1 1.830(6) . ? P2 C20 1.816(5) . ? P2 C26 1.821(6) . ? P2 C14 1.829(6) . ? N1 C27 1.139(6) . ? N1 C28 1.491(7) . ? N2 C32 1.140(7) . ? N2 C33 1.482(7) . ? N3 C37 1.063(18) . ? N4 C38 1.154(10) . ? C1 C6 1.376(9) . ? C1 C2 1.379(10) . ? C2 C3 1.405(10) . ? C3 C4 1.344(14) . ? C4 C5 1.361(15) . ? C5 C6 1.386(12) . ? C7 C8 1.366(9) . ? C7 C12 1.391(9) . ? C8 C9 1.401(11) . ? C9 C10 1.366(15) . ? C10 C11 1.375(15) . ? C11 C12 1.366(13) . ? C14 C15 1.382(11) . ? C14 C19 1.383(12) . ? C15 C16 1.421(14) . ? C16 C17 1.35(3) . ? C17 C18 1.35(2) . ? C18 C19 1.408(12) . ? C20 C21 1.388(8) . ? C20 C25 1.390(8) . ? C21 C22 1.386(9) . ? C22 C23 1.385(10) . ? C23 C24 1.369(11) . ? C24 C25 1.374(9) . ? C28 C30 1.487(11) . ? C28 C31 1.501(10) . ? C28 C29 1.516(11) . ? C33 C35 1.437(12) . ? C33 C34 1.438(16) . ? C33 C36 1.469(18) . ? 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 C32 Pd1 C27 169.7(2) . . ? C32 Pd1 P2 87.27(15) . . ? C27 Pd1 P2 90.69(14) . . ? C32 Pd1 P1 93.46(15) . . ? C27 Pd1 P1 86.67(14) . . ? P2 Pd1 P1 169.12(5) . . ? C7 P1 C13 107.0(3) . . ? C7 P1 C1 106.5(2) . . ? C13 P1 C1 106.3(3) . . ? C7 P1 Pd1 109.63(18) . . ? C13 P1 Pd1 111.8(2) . . ? C1 P1 Pd1 115.3(2) . . ? C20 P2 C26 106.0(3) . . ? C20 P2 C14 106.0(3) . . ? C26 P2 C14 105.4(3) . . ? C20 P2 Pd1 116.06(17) . . ? C26 P2 Pd1 108.5(2) . . ? C14 P2 Pd1 114.03(18) . . ? C27 N1 C28 174.8(6) . . ? C32 N2 C33 174.9(6) . . ? C6 C1 C2 117.6(6) . . ? C6 C1 P1 121.7(5) . . ? C2 C1 P1 120.6(5) . . ? C1 C2 C3 120.7(7) . . ? C4 C3 C2 119.5(9) . . ? C3 C4 C5 121.2(7) . . ? C4 C5 C6 119.2(8) . . ? C1 C6 C5 121.6(8) . . ? C8 C7 C12 118.3(6) . . ? C8 C7 P1 120.5(5) . . ? C12 C7 P1 121.2(5) . . ? C7 C8 C9 120.7(8) . . ? C10 C9 C8 119.8(9) . . ? C9 C10 C11 119.9(7) . . ? C12 C11 C10 120.2(9) . . ? C11 C12 C7 121.1(9) . . ? C15 C14 C19 119.0(7) . . ? C15 C14 P2 121.3(7) . . ? C19 C14 P2 119.6(6) . . ? C14 C15 C16 119.5(12) . . ? C17 C16 C15 120.6(14) . . ? C18 C17 C16 120.1(11) . . ? C17 C18 C19 121.1(14) . . ? C14 C19 C18 119.7(11) . . ? C21 C20 C25 118.6(5) . . ? C21 C20 P2 121.3(4) . . ? C25 C20 P2 120.2(4) . . ? C22 C21 C20 120.2(5) . . ? C23 C22 C21 120.3(6) . . ? C24 C23 C22 119.6(6) . . ? C23 C24 C25 120.4(6) . . ? C24 C25 C20 120.9(6) . . ? N1 C27 Pd1 176.1(5) . . ? C30 C28 N1 109.0(6) . . ? C30 C28 C31 112.0(7) . . ? N1 C28 C31 106.2(5) . . ? C30 C28 C29 113.7(7) . . ? N1 C28 C29 105.5(5) . . ? C31 C28 C29 110.0(8) . . ? N2 C32 Pd1 175.0(5) . . ? C35 C33 C34 114.6(14) . . ? C35 C33 C36 110.9(13) . . ? C34 C33 C36 107.8(13) . . ? C35 C33 N2 107.7(6) . . ? C34 C33 N2 108.1(7) . . ? C36 C33 N2 107.5(8) . . ? N3 C37 S1 146(2) . . ? N4 C38 S2 176.9(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 C32 Pd1 P1 C7 -118.9(3) . . . . ? C27 Pd1 P1 C7 50.8(2) . . . . ? P2 Pd1 P1 C7 -25.3(4) . . . . ? C32 Pd1 P1 C13 122.7(3) . . . . ? C27 Pd1 P1 C13 -67.6(3) . . . . ? P2 Pd1 P1 C13 -143.8(4) . . . . ? C32 Pd1 P1 C1 1.2(3) . . . . ? C27 Pd1 P1 C1 170.9(3) . . . . ? P2 Pd1 P1 C1 94.8(3) . . . . ? C32 Pd1 P2 C20 -41.3(3) . . . . ? C27 Pd1 P2 C20 148.8(2) . . . . ? P1 Pd1 P2 C20 -135.4(3) . . . . ? C32 Pd1 P2 C26 77.9(3) . . . . ? C27 Pd1 P2 C26 -92.0(3) . . . . ? P1 Pd1 P2 C26 -16.2(4) . . . . ? C32 Pd1 P2 C14 -165.0(3) . . . . ? C27 Pd1 P2 C14 25.1(3) . . . . ? P1 Pd1 P2 C14 100.9(4) . . . . ? C7 P1 C1 C6 -149.8(6) . . . . ? C13 P1 C1 C6 -36.0(7) . . . . ? Pd1 P1 C1 C6 88.4(6) . . . . ? C7 P1 C1 C2 31.7(7) . . . . ? C13 P1 C1 C2 145.5(6) . . . . ? Pd1 P1 C1 C2 -90.1(6) . . . . ? C6 C1 C2 C3 0.6(12) . . . . ? P1 C1 C2 C3 179.1(7) . . . . ? C1 C2 C3 C4 -0.6(15) . . . . ? C2 C3 C4 C5 0.5(16) . . . . ? C3 C4 C5 C6 -0.2(16) . . . . ? C2 C1 C6 C5 -0.3(12) . . . . ? P1 C1 C6 C5 -178.9(7) . . . . ? C4 C5 C6 C1 0.2(15) . . . . ? C13 P1 C7 C8 152.0(5) . . . . ? C1 P1 C7 C8 -94.7(5) . . . . ? Pd1 P1 C7 C8 30.6(5) . . . . ? C13 P1 C7 C12 -28.0(6) . . . . ? C1 P1 C7 C12 85.3(6) . . . . ? Pd1 P1 C7 C12 -149.4(5) . . . . ? C12 C7 C8 C9 2.1(9) . . . . ? P1 C7 C8 C9 -178.0(5) . . . . ? C7 C8 C9 C10 -1.4(11) . . . . ? C8 C9 C10 C11 1.1(13) . . . . ? C9 C10 C11 C12 -1.8(14) . . . . ? C10 C11 C12 C7 2.6(14) . . . . ? C8 C7 C12 C11 -2.7(11) . . . . ? P1 C7 C12 C11 177.4(6) . . . . ? C20 P2 C14 C15 133.3(6) . . . . ? C26 P2 C14 C15 21.2(6) . . . . ? Pd1 P2 C14 C15 -97.7(6) . . . . ? C20 P2 C14 C19 -50.8(5) . . . . ? C26 P2 C14 C19 -163.0(5) . . . . ? Pd1 P2 C14 C19 78.1(5) . . . . ? C19 C14 C15 C16 1.2(12) . . . . ? P2 C14 C15 C16 177.0(7) . . . . ? C14 C15 C16 C17 0.8(17) . . . . ? C15 C16 C17 C18 -1(2) . . . . ? C16 C17 C18 C19 0(2) . . . . ? C15 C14 C19 C18 -2.6(10) . . . . ? P2 C14 C19 C18 -178.6(6) . . . . ? C17 C18 C19 C14 2.2(15) . . . . ? C26 P2 C20 C21 -151.7(5) . . . . ? C14 P2 C20 C21 96.6(5) . . . . ? Pd1 P2 C20 C21 -31.2(5) . . . . ? C26 P2 C20 C25 27.4(6) . . . . ? C14 P2 C20 C25 -84.4(6) . . . . ? Pd1 P2 C20 C25 147.9(5) . . . . ? C25 C20 C21 C22 2.1(10) . . . . ? P2 C20 C21 C22 -178.8(5) . . . . ? C20 C21 C22 C23 -1.5(11) . . . . ? C21 C22 C23 C24 -0.8(13) . . . . ? C22 C23 C24 C25 2.4(13) . . . . ? C23 C24 C25 C20 -1.7(12) . . . . ? C21 C20 C25 C24 -0.5(11) . . . . ? P2 C20 C25 C24 -179.6(6) . . . . ? C28 N1 C27 Pd1 0(12) . . . . ? C32 Pd1 C27 N1 49(7) . . . . ? P2 Pd1 C27 N1 127(7) . . . . ? P1 Pd1 C27 N1 -42(7) . . . . ? C27 N1 C28 C30 173(6) . . . . ? C27 N1 C28 C31 52(6) . . . . ? C27 N1 C28 C29 -64(6) . . . . ? C33 N2 C32 Pd1 36(12) . . . . ? C27 Pd1 C32 N2 36(7) . . . . ? P2 Pd1 C32 N2 -42(6) . . . . ? P1 Pd1 C32 N2 127(6) . . . . ? C32 N2 C33 C35 -9(8) . . . . ? C32 N2 C33 C34 115(7) . . . . ? C32 N2 C33 C36 -129(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.531 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.051 #=========================================================END data_lee178 _database_code_depnum_ccdc_archive 'CCDC 275746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 N4 P2 Pt S2' _chemical_formula_weight 725.74 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' S S 0.1246 0.1234 '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 'Pn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.1931(9) _cell_length_b 12.2373(18) _cell_length_c 15.4579(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.128(9) _cell_angle_gamma 90.00 _cell_volume 1537.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.29 _cell_measurement_theta_max 12.47 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'ORANGE ' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 4.823 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3811 _exptl_absorpt_correction_T_max 0.7857 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2900 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2900 _reflns_number_gt 2646 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+1.4893P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.079(12) _refine_ls_number_reflns 2900 _refine_ls_number_parameters 320 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.24773(6) -0.22591(3) -0.25446(5) 0.05114(12) Uani 1 1 d . . . S1 S -0.7175(7) -0.4677(4) -0.1441(3) 0.1052(13) Uani 1 1 d . . . S2 S -0.5532(8) -0.1684(7) -0.4150(5) 0.138(2) Uani 1 1 d . . . P1 P -0.1219(4) -0.2728(3) -0.37753(19) 0.0592(7) Uani 1 1 d . . . P2 P -0.3551(4) -0.1803(3) -0.12751(17) 0.0565(6) Uani 1 1 d . . . N1 N -0.3352(12) -0.4700(9) -0.2295(5) 0.056(2) Uani 1 1 d . . . N2 N -0.1517(12) 0.0170(8) -0.2834(6) 0.058(2) Uani 1 1 d . . . N3 N -0.9402(19) -0.3241(19) -0.0972(13) 0.134(7) Uani 1 1 d . . . N4 N -0.7290(13) -0.0055(8) -0.3461(6) 0.053(2) Uani 1 1 d . . . C1 C -0.2959(12) -0.3756(12) -0.2375(5) 0.057(3) Uani 1 1 d . . . C2 C -0.3803(14) -0.5795(9) -0.2216(7) 0.053(2) Uani 1 1 d . . . C3 C -0.4971(14) -0.6215(11) -0.2845(7) 0.063(3) Uani 1 1 d . . . C4 C -0.542(4) -0.7295(18) -0.2759(19) 0.080(7) Uani 1 1 d . . . H4 H -0.6207 -0.7616 -0.3165 0.096 Uiso 1 1 calc R . . C5 C -0.466(2) -0.7898(12) -0.2051(13) 0.089(5) Uani 1 1 d . . . H5 H -0.4936 -0.8632 -0.2013 0.107 Uiso 1 1 calc R . . C6 C -0.354(4) -0.7465(18) -0.1411(18) 0.084(6) Uani 1 1 d . . . H6 H -0.3090 -0.7882 -0.0937 0.101 Uiso 1 1 calc R . . C7 C -0.3090(14) -0.6370(11) -0.1498(8) 0.062(3) Uani 1 1 d . . . C8 C -0.5759(18) -0.5563(14) -0.3591(9) 0.088(4) Uani 1 1 d . . . H8A H -0.5842 -0.4814 -0.3416 0.132 Uiso 1 1 calc R . . H8B H -0.6839 -0.5846 -0.3776 0.132 Uiso 1 1 calc R . . H8C H -0.5106 -0.5607 -0.4065 0.132 Uiso 1 1 calc R . . C9 C -0.1821(19) -0.5847(12) -0.0822(9) 0.085(4) Uani 1 1 d . . . H9A H -0.1376 -0.6391 -0.0412 0.127 Uiso 1 1 calc R . . H9B H -0.2334 -0.5280 -0.0522 0.127 Uiso 1 1 calc R . . H9C H -0.0951 -0.5539 -0.1107 0.127 Uiso 1 1 calc R . . C10 C -0.1854(16) -0.0707(10) -0.2731(7) 0.059(3) Uani 1 1 d . . . C11 C -0.1109(15) 0.1247(11) -0.3005(8) 0.065(3) Uani 1 1 d . . . C12 C -0.1914(16) 0.1737(13) -0.3728(9) 0.070(3) Uani 1 1 d . . . C13 C -0.145(4) 0.2823(14) -0.381(2) 0.099(10) Uani 1 1 d . . . H13 H -0.1978 0.3216 -0.4283 0.119 Uiso 1 1 calc R . . C14 C -0.030(2) 0.3348(14) -0.3264(16) 0.109(7) Uani 1 1 d . . . H14 H -0.0040 0.4072 -0.3369 0.130 Uiso 1 1 calc R . . C15 C 0.048(3) 0.2815(16) -0.256(2) 0.092(10) Uani 1 1 d . . . H15 H 0.1272 0.3182 -0.2180 0.110 Uiso 1 1 calc R . . C16 C 0.0115(16) 0.1722(15) -0.2387(11) 0.079(4) Uani 1 1 d . . . C17 C -0.3203(19) 0.1220(13) -0.4330(9) 0.087(4) Uani 1 1 d . . . H17A H -0.3543 0.1709 -0.4804 0.130 Uiso 1 1 calc R . . H17B H -0.4126 0.1051 -0.4028 0.130 Uiso 1 1 calc R . . H17C H -0.2785 0.0558 -0.4555 0.130 Uiso 1 1 calc R . . C18 C 0.092(2) 0.1152(17) -0.1622(11) 0.106(6) Uani 1 1 d . . . H18A H 0.1213 0.0428 -0.1783 0.159 Uiso 1 1 calc R . . H18B H 0.0179 0.1109 -0.1187 0.159 Uiso 1 1 calc R . . H18C H 0.1890 0.1544 -0.1391 0.159 Uiso 1 1 calc R . . C19 C 0.086(2) -0.3238(18) -0.3477(11) 0.106(5) Uani 1 1 d . . . H19A H 0.1497 -0.2700 -0.3131 0.159 Uiso 1 1 calc R . . H19B H 0.1358 -0.3382 -0.3996 0.159 Uiso 1 1 calc R . . H19C H 0.0822 -0.3900 -0.3147 0.159 Uiso 1 1 calc R . . C20 C -0.097(2) -0.1618(15) -0.4513(8) 0.094(5) Uani 1 1 d . . . H20A H -0.0370 -0.1037 -0.4202 0.142 Uiso 1 1 calc R . . H20B H -0.2035 -0.1356 -0.4756 0.142 Uiso 1 1 calc R . . H20C H -0.0382 -0.1871 -0.4973 0.142 Uiso 1 1 calc R . . C21 C -0.230(2) -0.3781(16) -0.4435(10) 0.113(6) Uani 1 1 d . . . H21A H -0.2460 -0.4402 -0.4077 0.169 Uiso 1 1 calc R . . H21B H -0.1658 -0.3994 -0.4888 0.169 Uiso 1 1 calc R . . H21C H -0.3343 -0.3507 -0.4692 0.169 Uiso 1 1 calc R . . C22 C -0.327(2) -0.2846(13) -0.0448(8) 0.085(4) Uani 1 1 d . . . H22A H -0.3731 -0.3520 -0.0681 0.127 Uiso 1 1 calc R . . H22B H -0.3805 -0.2629 0.0042 0.127 Uiso 1 1 calc R . . H22C H -0.2113 -0.2943 -0.0265 0.127 Uiso 1 1 calc R . . C23 C -0.5718(19) -0.1551(19) -0.1485(11) 0.115(7) Uani 1 1 d . . . H23A H -0.6259 -0.2182 -0.1755 0.172 Uiso 1 1 calc R . . H23B H -0.5914 -0.0933 -0.1866 0.172 Uiso 1 1 calc R . . H23C H -0.6143 -0.1402 -0.0945 0.172 Uiso 1 1 calc R . . C24 C -0.263(3) -0.0604(17) -0.0758(10) 0.119(7) Uani 1 1 d . . . H24A H -0.1461 -0.0704 -0.0644 0.178 Uiso 1 1 calc R . . H24B H -0.3069 -0.0482 -0.0219 0.178 Uiso 1 1 calc R . . H24C H -0.2868 0.0015 -0.1134 0.178 Uiso 1 1 calc R . . C25 C -0.848(2) -0.3874(18) -0.1151(10) 0.100(5) Uani 1 1 d . . . C26 C -0.650(3) -0.064(2) -0.3691(14) 0.131(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.05933(19) 0.04777(18) 0.04671(17) -0.0011(4) 0.00817(12) -0.0055(5) S1 0.119(3) 0.097(3) 0.103(3) 0.010(2) 0.027(3) -0.006(3) S2 0.114(4) 0.144(5) 0.158(5) -0.031(4) 0.020(3) -0.011(4) P1 0.0646(17) 0.066(2) 0.0477(14) -0.0020(18) 0.0098(13) 0.003(2) P2 0.0683(17) 0.0533(18) 0.0488(15) 0.0016(14) 0.0109(12) 0.0005(17) N1 0.064(5) 0.056(6) 0.048(5) -0.003(4) 0.004(4) -0.002(5) N2 0.067(6) 0.043(5) 0.065(5) 0.005(4) 0.011(5) -0.018(5) N3 0.082(10) 0.160(17) 0.160(16) -0.064(14) 0.017(10) -0.022(11) N4 0.059(6) 0.051(5) 0.053(5) -0.010(4) 0.019(4) -0.001(4) C1 0.046(6) 0.094(10) 0.024(5) -0.004(5) -0.023(4) 0.003(5) C2 0.057(6) 0.044(6) 0.062(6) 0.001(5) 0.014(5) -0.005(5) C3 0.059(6) 0.064(8) 0.066(6) -0.015(6) 0.012(5) -0.004(6) C4 0.064(12) 0.078(14) 0.096(12) -0.029(9) -0.002(9) -0.013(9) C5 0.077(9) 0.060(10) 0.136(15) -0.015(9) 0.041(11) -0.012(8) C6 0.093(15) 0.061(10) 0.099(13) 0.013(9) 0.018(11) -0.014(11) C7 0.061(7) 0.060(8) 0.068(7) -0.006(6) 0.013(6) -0.002(6) C8 0.080(9) 0.093(11) 0.085(9) -0.017(8) -0.009(8) -0.007(8) C9 0.095(10) 0.072(9) 0.082(8) -0.001(7) -0.009(8) -0.002(8) C10 0.080(8) 0.046(6) 0.055(7) -0.003(5) 0.019(6) -0.002(6) C11 0.065(7) 0.054(7) 0.083(8) -0.018(6) 0.034(6) -0.009(6) C12 0.071(7) 0.050(8) 0.095(9) 0.014(7) 0.034(7) 0.001(7) C13 0.074(13) 0.051(11) 0.19(3) 0.001(11) 0.068(15) 0.000(9) C14 0.079(11) 0.052(9) 0.21(2) -0.010(12) 0.065(13) -0.007(9) C15 0.061(13) 0.068(15) 0.15(3) -0.047(13) 0.041(15) -0.020(10) C16 0.063(8) 0.071(10) 0.108(11) -0.028(9) 0.031(8) -0.010(7) C17 0.096(10) 0.085(10) 0.079(8) 0.007(7) 0.005(8) -0.006(8) C18 0.079(10) 0.133(16) 0.103(11) -0.040(11) -0.001(9) -0.021(10) C19 0.080(9) 0.138(15) 0.100(11) 0.011(11) 0.010(8) 0.032(11) C20 0.123(12) 0.103(13) 0.064(8) 0.024(8) 0.037(8) 0.031(10) C21 0.140(15) 0.112(13) 0.091(10) -0.046(10) 0.036(11) -0.044(13) C22 0.106(11) 0.095(12) 0.055(7) 0.020(6) 0.019(7) 0.008(9) C23 0.084(10) 0.160(19) 0.107(11) 0.045(12) 0.042(9) 0.055(11) C24 0.172(19) 0.110(14) 0.079(10) -0.032(9) 0.035(12) -0.035(14) C25 0.100(12) 0.120(15) 0.083(10) -0.017(9) 0.022(9) -0.039(11) C26 0.102(14) 0.17(2) 0.111(15) 0.088(16) -0.025(12) -0.053(15) _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 C1 1.899(15) . ? Pt1 C10 1.997(12) . ? Pt1 P2 2.316(3) . ? Pt1 P1 2.345(3) . ? S1 C25 1.56(2) . ? S2 C26 1.70(3) . ? P1 C20 1.800(15) . ? P1 C21 1.805(16) . ? P1 C19 1.819(15) . ? P2 C23 1.792(15) . ? P2 C24 1.792(17) . ? P2 C22 1.800(13) . ? N1 C1 1.210(15) . ? N1 C2 1.399(15) . ? N2 C10 1.125(14) . ? N2 C11 1.393(15) . ? N3 C25 1.14(3) . ? N4 C26 1.06(3) . ? C2 C3 1.377(15) . ? C2 C7 1.381(16) . ? C3 C4 1.38(2) . ? C3 C8 1.48(2) . ? C4 C5 1.40(3) . ? C5 C6 1.37(3) . ? C6 C7 1.40(2) . ? C7 C9 1.521(17) . ? C11 C12 1.364(19) . ? C11 C16 1.421(19) . ? C12 C13 1.39(2) . ? C12 C17 1.46(2) . ? C13 C14 1.35(4) . ? C14 C15 1.36(3) . ? C15 C16 1.40(3) . ? C16 C18 1.46(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 C1 Pt1 C10 177.1(5) . . ? C1 Pt1 P2 90.5(3) . . ? C10 Pt1 P2 91.4(3) . . ? C1 Pt1 P1 89.8(3) . . ? C10 Pt1 P1 88.2(3) . . ? P2 Pt1 P1 176.21(11) . . ? C20 P1 C21 105.4(9) . . ? C20 P1 C19 104.2(8) . . ? C21 P1 C19 106.0(10) . . ? C20 P1 Pt1 115.1(5) . . ? C21 P1 Pt1 113.5(6) . . ? C19 P1 Pt1 111.7(6) . . ? C23 P2 C24 107.0(11) . . ? C23 P2 C22 106.8(8) . . ? C24 P2 C22 104.7(8) . . ? C23 P2 Pt1 111.1(6) . . ? C24 P2 Pt1 113.1(6) . . ? C22 P2 Pt1 113.7(5) . . ? C1 N1 C2 179.2(10) . . ? C10 N2 C11 177.2(11) . . ? N1 C1 Pt1 176.2(8) . . ? C3 C2 C7 124.4(11) . . ? C3 C2 N1 117.6(10) . . ? C7 C2 N1 118.0(10) . . ? C2 C3 C4 117.3(16) . . ? C2 C3 C8 123.1(12) . . ? C4 C3 C8 119.6(16) . . ? C3 C4 C5 119(2) . . ? C6 C5 C4 123.6(17) . . ? C5 C6 C7 117(2) . . ? C2 C7 C6 118.4(16) . . ? C2 C7 C9 121.5(12) . . ? C6 C7 C9 120.1(16) . . ? N2 C10 Pt1 179.3(12) . . ? C12 C11 N2 117.9(12) . . ? C12 C11 C16 126.9(14) . . ? N2 C11 C16 115.1(14) . . ? C11 C12 C13 112.9(19) . . ? C11 C12 C17 124.7(13) . . ? C13 C12 C17 122.4(19) . . ? C14 C13 C12 125(3) . . ? C13 C14 C15 120.0(18) . . ? C14 C15 C16 121.0(19) . . ? C15 C16 C11 114.5(18) . . ? C15 C16 C18 121.4(17) . . ? C11 C16 C18 124.1(15) . . ? N3 C25 S1 176(2) . . ? N4 C26 S2 170.3(19) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.658 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.091 #=========================================================END data_lke4 _database_code_depnum_ccdc_archive 'CCDC 275747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 N4 P2 Pt S2' _chemical_formula_weight 809.89 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' S S 0.1246 0.1234 '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 9.9813(15) _cell_length_b 12.1211(14) _cell_length_c 16.122(3) _cell_angle_alpha 90.367(12) _cell_angle_beta 104.795(12) _cell_angle_gamma 104.703(11) _cell_volume 1818.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.98 _cell_measurement_theta_max 12.50 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 4.086 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4418 _exptl_absorpt_correction_T_max 0.8153 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6740 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6345 _reflns_number_gt 5452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+2.4723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6345 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.68456(3) 0.782052(19) 0.734492(16) 0.04316(10) Uani 1 1 d . . . P1 P 0.57197(18) 0.93154(14) 0.72095(12) 0.0494(4) Uani 1 1 d . . . P2 P 0.7988(2) 0.63621(16) 0.77872(14) 0.0582(5) Uani 1 1 d . . . N1 N 0.3966(6) 0.6033(5) 0.7229(4) 0.0567(14) Uani 1 1 d . . . N2 N 0.9757(6) 0.9671(5) 0.7670(4) 0.0533(13) Uani 1 1 d . . . C1 C 0.5028(7) 0.6723(5) 0.7250(4) 0.0498(15) Uani 1 1 d . . . C2 C 0.2719(7) 0.5154(6) 0.7184(5) 0.0580(18) Uani 1 1 d . . . C3 C 0.2479(9) 0.4779(7) 0.7955(6) 0.069(2) Uani 1 1 d . . . C4 C 0.1212(9) 0.3911(7) 0.7892(7) 0.078(2) Uani 1 1 d . . . H4 H 0.0985 0.3642 0.8392 0.094 Uiso 1 1 calc R . . C5 C 0.0334(9) 0.3470(7) 0.7133(7) 0.076(3) Uani 1 1 d . . . H5 H -0.0491 0.2891 0.7113 0.092 Uiso 1 1 calc R . . C6 C 0.0605(9) 0.3841(7) 0.6371(7) 0.078(2) Uani 1 1 d . . . H6 H -0.0018 0.3503 0.5848 0.094 Uiso 1 1 calc R . . C7 C 0.1811(8) 0.4720(6) 0.6391(6) 0.064(2) Uani 1 1 d . . . C8 C 0.3490(13) 0.5274(9) 0.8812(7) 0.105(3) Uani 1 1 d . . . H8A H 0.2992 0.5114 0.9253 0.157 Uiso 1 1 calc R . . H8B H 0.3838 0.6086 0.8799 0.157 Uiso 1 1 calc R . . H8C H 0.4285 0.4937 0.8933 0.157 Uiso 1 1 calc R . . C9 C 0.2131(12) 0.5187(9) 0.5569(6) 0.100(3) Uani 1 1 d . . . H9A H 0.1505 0.4690 0.5082 0.151 Uiso 1 1 calc R . . H9B H 0.3112 0.5229 0.5587 0.151 Uiso 1 1 calc R . . H9C H 0.1979 0.5938 0.5518 0.151 Uiso 1 1 calc R . . C10 C 0.8692(7) 0.8972(5) 0.7568(4) 0.0479(15) Uani 1 1 d . . . C11 C 1.1063(7) 1.0516(5) 0.7788(5) 0.0501(16) Uani 1 1 d . . . C12 C 1.1424(7) 1.0967(6) 0.7051(5) 0.0555(17) Uani 1 1 d . . . C13 C 1.2729(8) 1.1796(6) 0.7199(6) 0.066(2) Uani 1 1 d . . . H13 H 1.3016 1.2133 0.6733 0.079 Uiso 1 1 calc R . . C14 C 1.3584(8) 1.2121(6) 0.7999(7) 0.072(2) Uani 1 1 d . . . H14 H 1.4456 1.2669 0.8075 0.086 Uiso 1 1 calc R . . C15 C 1.3196(8) 1.1659(7) 0.8708(6) 0.074(2) Uani 1 1 d . . . H15 H 1.3806 1.1904 0.9254 0.089 Uiso 1 1 calc R . . C16 C 1.1919(8) 1.0840(7) 0.8621(5) 0.0612(18) Uani 1 1 d . . . C17 C 1.0454(10) 1.0591(8) 0.6170(5) 0.079(2) Uani 1 1 d . . . H17A H 1.1003 1.0750 0.5754 0.118 Uiso 1 1 calc R . . H17B H 0.9724 1.0996 0.6053 0.118 Uiso 1 1 calc R . . H17C H 1.0013 0.9784 0.6135 0.118 Uiso 1 1 calc R . . C18 C 1.1476(11) 1.0286(10) 0.9381(6) 0.097(3) Uani 1 1 d . . . H18A H 1.2121 1.0685 0.9905 0.146 Uiso 1 1 calc R . . H18B H 1.1511 0.9502 0.9365 0.146 Uiso 1 1 calc R . . H18C H 1.0516 1.0318 0.9356 0.146 Uiso 1 1 calc R . . C19 C 0.3856(8) 0.8952(8) 0.6597(6) 0.077(2) Uani 1 1 d . . . H19A H 0.3328 0.8314 0.6846 0.092 Uiso 1 1 calc R . . H19B H 0.3471 0.9597 0.6656 0.092 Uiso 1 1 calc R . . C20 C 0.3590(10) 0.8631(9) 0.5638(6) 0.093(3) Uani 1 1 d . . . H20A H 0.2578 0.8452 0.5364 0.139 Uiso 1 1 calc R . . H20B H 0.3939 0.7976 0.5569 0.139 Uiso 1 1 calc R . . H20C H 0.4085 0.9262 0.5379 0.139 Uiso 1 1 calc R . . C21 C 0.5723(10) 0.9856(7) 0.8273(5) 0.071(2) Uani 1 1 d . . . H21A H 0.6710 1.0113 0.8620 0.085 Uiso 1 1 calc R . . H21B H 0.5333 1.0517 0.8207 0.085 Uiso 1 1 calc R . . C22 C 0.4888(11) 0.9010(9) 0.8744(6) 0.093(3) Uani 1 1 d . . . H22A H 0.4931 0.9363 0.9288 0.139 Uiso 1 1 calc R . . H22B H 0.5291 0.8367 0.8837 0.139 Uiso 1 1 calc R . . H22C H 0.3906 0.8757 0.8410 0.139 Uiso 1 1 calc R . . C23 C 0.6686(8) 1.0531(6) 0.6761(5) 0.0619(18) Uani 1 1 d . . . H23A H 0.7637 1.0814 0.7151 0.074 Uiso 1 1 calc R . . H23B H 0.6805 1.0266 0.6223 0.074 Uiso 1 1 calc R . . C24 C 0.6014(10) 1.1532(7) 0.6592(7) 0.081(2) Uani 1 1 d . . . H24A H 0.6610 1.2119 0.6349 0.121 Uiso 1 1 calc R . . H24B H 0.5929 1.1833 0.7123 0.121 Uiso 1 1 calc R . . H24C H 0.5078 1.1275 0.6196 0.121 Uiso 1 1 calc R . . C25 C 0.6892(17) 0.4936(12) 0.7461(10) 0.142(5) Uiso 1 1 d . . . H25A H 0.7466 0.4409 0.7673 0.171 Uiso 1 1 calc R . . H25B H 0.6113 0.4796 0.7737 0.171 Uiso 1 1 calc R . . C26 C 0.6244(12) 0.4656(9) 0.6494(7) 0.099(3) Uiso 1 1 d . . . H26A H 0.5723 0.3864 0.6385 0.149 Uiso 1 1 calc R . . H26B H 0.6999 0.4806 0.6209 0.149 Uiso 1 1 calc R . . H26C H 0.5603 0.5123 0.6281 0.149 Uiso 1 1 calc R . . C27 C 0.9594(18) 0.6293(15) 0.7442(12) 0.167(6) Uiso 1 1 d . . . H27A H 0.9831 0.5589 0.7624 0.200 Uiso 1 1 calc R . . H27B H 0.9339 0.6242 0.6819 0.200 Uiso 1 1 calc R . . C28 C 1.0896(13) 0.7240(10) 0.7755(8) 0.115(4) Uiso 1 1 d . . . H28A H 1.1662 0.7090 0.7552 0.172 Uiso 1 1 calc R . . H28B H 1.1168 0.7310 0.8372 0.172 Uiso 1 1 calc R . . H28C H 1.0709 0.7940 0.7543 0.172 Uiso 1 1 calc R . . C29 C 0.863(2) 0.6399(16) 0.8945(11) 0.173(6) Uiso 1 1 d . . . H29A H 0.8986 0.5735 0.9095 0.207 Uiso 1 1 calc R . . H29B H 0.9419 0.7075 0.9147 0.207 Uiso 1 1 calc R . . C30 C 0.7536(19) 0.6412(15) 0.9380(11) 0.169(6) Uiso 1 1 d . . . H30A H 0.7894 0.6319 0.9980 0.253 Uiso 1 1 calc R . . H30B H 0.6698 0.5798 0.9134 0.253 Uiso 1 1 calc R . . H30C H 0.7290 0.7129 0.9316 0.253 Uiso 1 1 calc R . . S1 S 0.3167(3) 0.2273(2) 0.44950(15) 0.0881(7) Uani 1 1 d . . . N3 N 0.0411(13) 0.2444(9) 0.4398(7) 0.119(3) Uani 1 1 d . . . C31 C 0.1536(13) 0.2383(7) 0.4436(6) 0.081(3) Uani 1 1 d . . . S2 S 0.2688(6) 0.7194(5) 0.0389(4) 0.209(3) Uani 1 1 d . . . N4 N 0.1129(15) 0.7902(15) 0.1188(11) 0.159(7) Uani 1 1 d . . . C32 C 0.1640(19) 0.7589(15) 0.0935(10) 0.120(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03605(14) 0.03968(14) 0.05159(16) 0.00638(9) 0.01317(10) 0.00455(9) P1 0.0430(9) 0.0468(9) 0.0595(10) 0.0088(7) 0.0159(8) 0.0115(7) P2 0.0515(10) 0.0498(10) 0.0747(12) 0.0185(9) 0.0168(9) 0.0155(8) N1 0.045(3) 0.044(3) 0.078(4) 0.005(3) 0.020(3) 0.001(3) N2 0.040(3) 0.048(3) 0.068(4) 0.010(3) 0.013(3) 0.005(3) C1 0.052(4) 0.046(3) 0.050(4) 0.008(3) 0.011(3) 0.012(3) C2 0.045(4) 0.043(3) 0.087(5) 0.006(3) 0.022(4) 0.008(3) C3 0.063(5) 0.058(4) 0.093(6) 0.014(4) 0.033(5) 0.015(4) C4 0.061(5) 0.065(5) 0.117(8) 0.021(5) 0.043(5) 0.013(4) C5 0.049(4) 0.046(4) 0.131(8) 0.009(5) 0.027(5) 0.004(3) C6 0.050(4) 0.062(5) 0.114(7) 0.001(5) 0.014(5) 0.008(4) C7 0.051(4) 0.047(4) 0.091(6) 0.004(4) 0.013(4) 0.010(3) C8 0.114(9) 0.104(8) 0.083(7) 0.009(6) 0.036(6) -0.003(6) C9 0.097(7) 0.093(7) 0.081(6) 0.008(5) -0.007(5) 0.001(6) C10 0.052(4) 0.046(3) 0.048(4) 0.005(3) 0.019(3) 0.011(3) C11 0.038(3) 0.042(3) 0.072(5) 0.005(3) 0.022(3) 0.007(3) C12 0.051(4) 0.046(3) 0.074(5) 0.005(3) 0.025(4) 0.013(3) C13 0.057(4) 0.050(4) 0.096(6) 0.010(4) 0.036(5) 0.006(3) C14 0.042(4) 0.055(4) 0.115(7) 0.001(4) 0.026(4) -0.001(3) C15 0.046(4) 0.074(5) 0.085(6) -0.009(4) 0.001(4) 0.001(4) C16 0.050(4) 0.067(4) 0.063(4) 0.008(4) 0.014(4) 0.011(3) C17 0.085(6) 0.075(5) 0.070(5) 0.003(4) 0.021(5) 0.010(5) C18 0.075(6) 0.123(8) 0.070(6) 0.007(5) 0.015(5) -0.009(6) C19 0.046(4) 0.085(6) 0.097(7) 0.010(5) 0.015(4) 0.019(4) C20 0.081(6) 0.108(7) 0.071(6) 0.006(5) 0.002(5) 0.011(5) C21 0.084(6) 0.065(5) 0.069(5) 0.001(4) 0.029(4) 0.022(4) C22 0.098(7) 0.112(8) 0.076(6) 0.005(5) 0.041(5) 0.022(6) C23 0.057(4) 0.057(4) 0.077(5) 0.013(4) 0.024(4) 0.016(3) C24 0.085(6) 0.063(5) 0.104(7) 0.028(5) 0.031(5) 0.030(4) S1 0.0980(18) 0.0968(17) 0.0674(13) 0.0024(12) 0.0189(12) 0.0252(14) N3 0.128(9) 0.114(7) 0.139(9) 0.020(6) 0.071(8) 0.040(7) C31 0.105(8) 0.059(5) 0.085(6) 0.007(4) 0.043(6) 0.016(5) S2 0.155(4) 0.232(6) 0.202(5) -0.085(5) -0.020(4) 0.058(4) N4 0.100(9) 0.177(15) 0.163(14) -0.032(10) 0.073(8) -0.063(9) C32 0.127(14) 0.113(10) 0.081(8) -0.029(7) 0.013(8) -0.022(10) _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 C1 1.927(7) . ? Pt1 C10 1.955(7) . ? Pt1 P1 2.3468(17) . ? Pt1 P2 2.3575(18) . ? P1 C19 1.808(8) . ? P1 C23 1.809(7) . ? P1 C21 1.830(8) . ? P2 C25 1.788(15) . ? P2 C29 1.808(18) . ? P2 C27 1.846(17) . ? N1 C1 1.164(8) . ? N1 C2 1.404(8) . ? N2 C10 1.152(8) . ? N2 C11 1.406(8) . ? C2 C7 1.376(11) . ? C2 C3 1.382(11) . ? C3 C4 1.405(11) . ? C3 C8 1.503(13) . ? C4 C5 1.327(13) . ? C5 C6 1.377(14) . ? C6 C7 1.384(11) . ? C7 C9 1.521(13) . ? C11 C16 1.386(10) . ? C11 C12 1.402(10) . ? C12 C13 1.391(10) . ? C12 C17 1.494(11) . ? C13 C14 1.345(13) . ? C14 C15 1.376(13) . ? C15 C16 1.377(11) . ? C16 C18 1.512(12) . ? C19 C20 1.532(13) . ? C21 C22 1.491(12) . ? C23 C24 1.523(10) . ? C25 C26 1.526(17) . ? C27 C28 1.470(18) . ? C29 C30 1.44(2) . ? S1 C31 1.646(12) . ? N3 C31 1.130(13) . ? S2 C32 1.677(18) . ? N4 C32 0.880(19) . ? 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 C1 Pt1 C10 173.9(3) . . ? C1 Pt1 P1 90.4(2) . . ? C10 Pt1 P1 88.4(2) . . ? C1 Pt1 P2 88.4(2) . . ? C10 Pt1 P2 91.59(19) . . ? P1 Pt1 P2 167.99(7) . . ? C19 P1 C23 108.2(4) . . ? C19 P1 C21 104.9(4) . . ? C23 P1 C21 105.1(4) . . ? C19 P1 Pt1 116.0(3) . . ? C23 P1 Pt1 111.8(2) . . ? C21 P1 Pt1 110.0(3) . . ? C25 P2 C29 105.0(8) . . ? C25 P2 C27 100.2(7) . . ? C29 P2 C27 102.1(8) . . ? C25 P2 Pt1 115.2(5) . . ? C29 P2 Pt1 112.2(6) . . ? C27 P2 Pt1 120.2(6) . . ? C1 N1 C2 176.6(7) . . ? C10 N2 C11 179.2(7) . . ? N1 C1 Pt1 176.4(6) . . ? C7 C2 C3 123.9(7) . . ? C7 C2 N1 119.0(7) . . ? C3 C2 N1 117.1(7) . . ? C2 C3 C4 116.0(8) . . ? C2 C3 C8 122.6(7) . . ? C4 C3 C8 121.4(8) . . ? C5 C4 C3 121.0(9) . . ? C4 C5 C6 122.1(8) . . ? C5 C6 C7 119.6(9) . . ? C2 C7 C6 117.4(8) . . ? C2 C7 C9 121.1(7) . . ? C6 C7 C9 121.6(8) . . ? N2 C10 Pt1 177.3(6) . . ? C16 C11 C12 124.2(6) . . ? C16 C11 N2 118.2(6) . . ? C12 C11 N2 117.6(6) . . ? C13 C12 C11 115.6(7) . . ? C13 C12 C17 122.5(7) . . ? C11 C12 C17 121.8(7) . . ? C14 C13 C12 121.4(8) . . ? C13 C14 C15 121.4(7) . . ? C14 C15 C16 121.0(8) . . ? C15 C16 C11 116.4(7) . . ? C15 C16 C18 122.5(8) . . ? C11 C16 C18 121.1(7) . . ? C20 C19 P1 115.0(6) . . ? C22 C21 P1 114.7(6) . . ? C24 C23 P1 116.9(6) . . ? C26 C25 P2 115.9(10) . . ? C28 C27 P2 117.5(12) . . ? C30 C29 P2 113.4(14) . . ? N3 C31 S1 179.0(10) . . ? N4 C32 S2 171(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.421 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.115 #=========================================================END data_398 _database_code_depnum_ccdc_archive 'CCDC 275748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H48 N2 P4 Pt S2' _chemical_formula_weight 723.71 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' S S 0.1246 0.1234 '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 11.103(3) _cell_length_b 11.378(4) _cell_length_c 12.928(3) _cell_angle_alpha 101.485(17) _cell_angle_beta 90.380(17) _cell_angle_gamma 91.10(2) _cell_volume 1600.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.13 _cell_measurement_theta_max 12.58 _exptl_crystal_description 'block ' _exptl_crystal_colour 'colorless ' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 4.728 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2221 _exptl_absorpt_correction_T_max 0.6865 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5833 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5525 _reflns_number_gt 4528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+4.2504P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5525 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.5000 0.5000 0.04002(12) Uani 1 2 d S . . Pt2 Pt 0.5000 0.0000 0.0000 0.04312(12) Uani 1 2 d S . . P1 P 0.04429(15) 0.32996(14) 0.56896(14) 0.0507(4) Uani 1 1 d . . . P2 P 0.19850(15) 0.57324(14) 0.50495(15) 0.0506(4) Uani 1 1 d . . . P3 P 0.35836(17) -0.11657(18) 0.06937(15) 0.0610(5) Uani 1 1 d . . . P4 P 0.33065(17) 0.10216(16) -0.04239(14) 0.0557(4) Uani 1 1 d . . . C1 C 0.1614(8) 0.2308(7) 0.5045(6) 0.0657(19) Uani 1 1 d . . . H1A H 0.1519 0.2224 0.4287 0.079 Uiso 1 1 calc R . . H1B H 0.2392 0.2692 0.5241 0.079 Uiso 1 1 calc R . . C2 C 0.1620(8) 0.1058(7) 0.5303(8) 0.083(2) Uani 1 1 d . . . H2A H 0.2252 0.0604 0.4919 0.124 Uiso 1 1 calc R . . H2B H 0.0859 0.0661 0.5105 0.124 Uiso 1 1 calc R . . H2C H 0.1755 0.1123 0.6046 0.124 Uiso 1 1 calc R . . C3 C 0.0864(8) 0.3568(7) 0.7079(6) 0.071(2) Uani 1 1 d . . . H3A H 0.0755 0.2824 0.7330 0.085 Uiso 1 1 calc R . . H3B H 0.1714 0.3786 0.7146 0.085 Uiso 1 1 calc R . . C4 C 0.0145(11) 0.4560(9) 0.7804(8) 0.105(3) Uani 1 1 d . . . H4A H 0.0414 0.4632 0.8521 0.158 Uiso 1 1 calc R . . H4B H -0.0698 0.4351 0.7752 0.158 Uiso 1 1 calc R . . H4C H 0.0275 0.5311 0.7586 0.158 Uiso 1 1 calc R . . C5 C -0.0918(7) 0.2329(8) 0.5530(10) 0.087(3) Uani 1 1 d . . . H5A H -0.0890 0.1784 0.4851 0.105 Uiso 1 1 calc R . . H5B H -0.0913 0.1849 0.6072 0.105 Uiso 1 1 calc R . . C6 C -0.2031(7) 0.2976(7) 0.5594(9) 0.088(3) Uani 1 1 d . . . H6A H -0.2226 0.3250 0.6332 0.106 Uiso 1 1 calc R . . H6B H -0.2672 0.2430 0.5274 0.106 Uiso 1 1 calc R . . C7 C 0.3143(6) 0.4779(7) 0.4343(6) 0.0666(19) Uani 1 1 d . . . H7A H 0.3864 0.5266 0.4314 0.080 Uiso 1 1 calc R . . H7B H 0.3341 0.4172 0.4745 0.080 Uiso 1 1 calc R . . C8 C 0.2798(9) 0.4150(9) 0.3218(7) 0.091(3) Uani 1 1 d . . . H8A H 0.3454 0.3671 0.2908 0.137 Uiso 1 1 calc R . . H8B H 0.2623 0.4741 0.2804 0.137 Uiso 1 1 calc R . . H8C H 0.2098 0.3645 0.3236 0.137 Uiso 1 1 calc R . . C9 C 0.2584(6) 0.6236(7) 0.6382(6) 0.0666(19) Uani 1 1 d . . . H9A H 0.2064 0.6850 0.6757 0.080 Uiso 1 1 calc R . . H9B H 0.2551 0.5566 0.6742 0.080 Uiso 1 1 calc R . . C10 C 0.3892(7) 0.6745(8) 0.6452(7) 0.078(2) Uani 1 1 d . . . H10A H 0.4127 0.6997 0.7180 0.118 Uiso 1 1 calc R . . H10B H 0.3937 0.7419 0.6109 0.118 Uiso 1 1 calc R . . H10C H 0.4424 0.6136 0.6111 0.118 Uiso 1 1 calc R . . C11 C 0.3815(12) -0.2792(10) 0.0446(12) 0.114(4) Uani 1 1 d . . . H11A H 0.3985 -0.3078 -0.0296 0.137 Uiso 1 1 calc R . . H11B H 0.4505 -0.2961 0.0854 0.137 Uiso 1 1 calc R . . C12 C 0.268(2) -0.3465(17) 0.075(2) 0.258(13) Uani 1 1 d . . . H12A H 0.2808 -0.4313 0.0597 0.386 Uiso 1 1 calc R . . H12B H 0.1994 -0.3286 0.0360 0.386 Uiso 1 1 calc R . . H12C H 0.2534 -0.3210 0.1496 0.386 Uiso 1 1 calc R . . C13 C 0.3434(8) -0.0720(10) 0.2140(7) 0.088(3) Uani 1 1 d . . . H13A H 0.2701 -0.1086 0.2344 0.106 Uiso 1 1 calc R . . H13B H 0.4103 -0.1048 0.2469 0.106 Uiso 1 1 calc R . . C14 C 0.3403(9) 0.0629(11) 0.2586(7) 0.100(3) Uani 1 1 d . . . H14A H 0.3349 0.0765 0.3341 0.150 Uiso 1 1 calc R . . H14B H 0.2716 0.0961 0.2303 0.150 Uiso 1 1 calc R . . H14C H 0.4125 0.1007 0.2394 0.150 Uiso 1 1 calc R . . C15 C 0.2137(7) -0.0992(10) 0.0089(8) 0.093(3) Uani 1 1 d . . . H15A H 0.2088 -0.1524 -0.0597 0.112 Uiso 1 1 calc R . . H15B H 0.1502 -0.1229 0.0523 0.112 Uiso 1 1 calc R . . C16 C 0.1939(7) 0.0246(9) -0.0039(8) 0.084(3) Uani 1 1 d . . . H16A H 0.1643 0.0706 0.0620 0.101 Uiso 1 1 calc R . . H16B H 0.1318 0.0235 -0.0573 0.101 Uiso 1 1 calc R . . C17 C 0.3124(10) 0.2558(8) 0.0290(8) 0.092(3) Uani 1 1 d . . . H17A H 0.3202 0.2571 0.1040 0.110 Uiso 1 1 calc R . . H17B H 0.3774 0.3051 0.0097 0.110 Uiso 1 1 calc R . . C18 C 0.1940(12) 0.3114(10) 0.0092(10) 0.120(4) Uani 1 1 d . . . H18A H 0.1919 0.3918 0.0498 0.181 Uiso 1 1 calc R . . H18B H 0.1288 0.2647 0.0297 0.181 Uiso 1 1 calc R . . H18C H 0.1862 0.3131 -0.0645 0.181 Uiso 1 1 calc R . . C19 C 0.3150(7) 0.1071(7) -0.1809(6) 0.0668(19) Uani 1 1 d . . . H19A H 0.2380 0.1413 -0.1927 0.080 Uiso 1 1 calc R . . H19B H 0.3778 0.1589 -0.2000 0.080 Uiso 1 1 calc R . . C20 C 0.3228(8) -0.0183(8) -0.2526(6) 0.082(2) Uani 1 1 d . . . H20A H 0.3128 -0.0116 -0.3250 0.123 Uiso 1 1 calc R . . H20B H 0.2606 -0.0699 -0.2342 0.123 Uiso 1 1 calc R . . H20C H 0.4001 -0.0514 -0.2432 0.123 Uiso 1 1 calc R . . S1 S 0.0006(2) 0.1809(2) 0.23538(19) 0.0861(6) Uani 1 1 d . . . C21 C 0.0076(7) 0.0377(11) 0.2380(7) 0.080(2) Uani 1 1 d . . . N1 N 0.0154(7) -0.0601(9) 0.2386(8) 0.109(3) Uani 1 1 d . . . S2 S 0.4225(8) 0.4576(7) 0.8300(6) 0.249(3) Uiso 1 1 d . . . C22 C 0.4482(6) 0.3729(6) 0.7194(5) 0.0518(15) Uiso 1 1 d . . . N2 N 0.4584(9) 0.3170(9) 0.6604(8) 0.108(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03464(18) 0.03892(18) 0.0492(2) 0.01511(13) 0.00108(12) 0.00177(12) Pt2 0.0440(2) 0.0470(2) 0.03993(19) 0.01224(13) 0.00169(13) 0.00195(13) P1 0.0461(9) 0.0444(8) 0.0673(10) 0.0245(7) -0.0034(7) 0.0033(7) P2 0.0389(8) 0.0460(8) 0.0710(11) 0.0215(8) -0.0005(7) -0.0006(6) P3 0.0554(10) 0.0694(11) 0.0644(11) 0.0288(9) 0.0015(8) -0.0064(8) P4 0.0580(10) 0.0579(10) 0.0527(9) 0.0139(8) -0.0008(8) 0.0130(8) C1 0.071(5) 0.063(4) 0.068(5) 0.022(4) 0.002(4) 0.017(4) C2 0.082(6) 0.061(4) 0.114(7) 0.037(5) 0.019(5) 0.021(4) C3 0.092(6) 0.062(4) 0.063(4) 0.024(4) -0.009(4) 0.004(4) C4 0.143(10) 0.096(7) 0.079(6) 0.022(5) 0.017(6) 0.035(7) C5 0.055(4) 0.067(5) 0.158(9) 0.066(6) -0.009(5) -0.009(4) C6 0.046(4) 0.076(5) 0.163(9) 0.074(6) -0.019(5) -0.018(4) C7 0.046(4) 0.072(5) 0.082(5) 0.013(4) 0.006(3) 0.000(3) C8 0.081(6) 0.108(7) 0.079(6) 0.007(5) 0.010(5) -0.003(5) C9 0.054(4) 0.067(4) 0.074(5) 0.003(4) -0.003(3) 0.005(3) C10 0.056(4) 0.074(5) 0.098(6) 0.001(4) -0.017(4) -0.004(4) C11 0.119(9) 0.084(7) 0.148(11) 0.045(7) -0.010(8) -0.021(6) C12 0.30(3) 0.147(15) 0.34(3) 0.074(17) 0.13(2) -0.069(16) C13 0.067(5) 0.134(8) 0.077(5) 0.053(6) 0.003(4) -0.001(5) C14 0.071(6) 0.147(10) 0.075(6) 0.003(6) 0.000(4) 0.022(6) C15 0.052(5) 0.139(9) 0.103(7) 0.064(6) -0.009(4) -0.026(5) C16 0.049(4) 0.118(7) 0.095(6) 0.042(6) 0.008(4) 0.012(4) C17 0.109(7) 0.073(5) 0.086(6) -0.004(5) 0.003(5) 0.029(5) C18 0.142(10) 0.092(7) 0.126(9) 0.011(6) 0.014(7) 0.061(7) C19 0.065(4) 0.079(5) 0.062(4) 0.027(4) -0.004(3) 0.014(4) C20 0.077(5) 0.097(6) 0.064(5) -0.003(4) -0.009(4) 0.019(5) S1 0.0711(13) 0.0983(16) 0.0847(15) 0.0077(12) 0.0022(11) 0.0036(11) C21 0.051(4) 0.123(8) 0.070(5) 0.035(5) 0.004(4) -0.007(5) N1 0.074(5) 0.119(7) 0.156(9) 0.080(7) 0.000(5) -0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.3370(18) 2_566 ? Pt1 P2 2.3370(18) . ? Pt1 P1 2.3446(17) 2_566 ? Pt1 P1 2.3446(17) . ? Pt2 P3 2.3342(19) 2_655 ? Pt2 P3 2.3342(19) . ? Pt2 P4 2.3475(18) . ? Pt2 P4 2.3475(18) 2_655 ? P1 C3 1.817(7) . ? P1 C1 1.831(8) . ? P1 C5 1.840(8) . ? P2 C9 1.820(8) . ? P2 C6 1.828(7) 2_566 ? P2 C7 1.827(7) . ? P3 C15 1.812(9) . ? P3 C11 1.837(12) . ? P3 C13 1.846(9) . ? P4 C19 1.810(7) . ? P4 C17 1.822(9) . ? P4 C16 1.861(9) . ? C1 C2 1.523(10) . ? C3 C4 1.554(12) . ? C5 C6 1.445(12) . ? C6 P2 1.828(7) 2_566 ? C7 C8 1.530(11) . ? C9 C10 1.548(10) . ? C11 C12 1.56(2) . ? C13 C14 1.530(14) . ? C15 C16 1.472(13) . ? C17 C18 1.511(14) . ? C19 C20 1.543(11) . ? S1 C21 1.641(12) . ? C21 N1 1.119(12) . ? S2 C22 1.589(10) . ? C22 N2 0.900(9) . ? 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 P2 Pt1 P2 180.0 2_566 . ? P2 Pt1 P1 95.59(6) 2_566 2_566 ? P2 Pt1 P1 84.41(6) . 2_566 ? P2 Pt1 P1 84.41(6) 2_566 . ? P2 Pt1 P1 95.59(6) . . ? P1 Pt1 P1 180.0 2_566 . ? P3 Pt2 P3 180.00(12) 2_655 . ? P3 Pt2 P4 95.91(7) 2_655 . ? P3 Pt2 P4 84.09(7) . . ? P3 Pt2 P4 84.09(7) 2_655 2_655 ? P3 Pt2 P4 95.91(7) . 2_655 ? P4 Pt2 P4 180.00(8) . 2_655 ? C3 P1 C1 103.7(4) . . ? C3 P1 C5 106.8(5) . . ? C1 P1 C5 103.5(5) . . ? C3 P1 Pt1 116.3(2) . . ? C1 P1 Pt1 118.0(3) . . ? C5 P1 Pt1 107.4(3) . . ? C9 P2 C6 107.2(4) . 2_566 ? C9 P2 C7 105.2(3) . . ? C6 P2 C7 102.3(4) 2_566 . ? C9 P2 Pt1 113.6(3) . . ? C6 P2 Pt1 108.5(2) 2_566 . ? C7 P2 Pt1 119.1(3) . . ? C15 P3 C11 105.0(6) . . ? C15 P3 C13 108.3(5) . . ? C11 P3 C13 104.9(6) . . ? C15 P3 Pt2 107.7(3) . . ? C11 P3 Pt2 117.1(4) . . ? C13 P3 Pt2 113.2(3) . . ? C19 P4 C17 105.9(4) . . ? C19 P4 C16 107.5(4) . . ? C17 P4 C16 102.4(5) . . ? C19 P4 Pt2 114.7(2) . . ? C17 P4 Pt2 117.3(3) . . ? C16 P4 Pt2 108.0(3) . . ? C2 C1 P1 115.7(6) . . ? C4 C3 P1 115.0(6) . . ? C6 C5 P1 113.9(6) . . ? C5 C6 P2 114.0(6) . 2_566 ? C8 C7 P2 115.1(6) . . ? C10 C9 P2 115.3(6) . . ? C12 C11 P3 110.8(12) . . ? C14 C13 P3 116.0(6) . . ? C16 C15 P3 112.7(6) . . ? C15 C16 P4 114.2(6) . . ? C18 C17 P4 115.0(8) . . ? C20 C19 P4 112.3(5) . . ? N1 C21 S1 178.1(9) . . ? N2 C22 S2 172.3(10) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.741 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.124