# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_3 _database_code_depnum_ccdc_archive 'CCDC 791555' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H21 N2 P S2' _chemical_formula_sum 'C25 H21 N2 P S2' _chemical_formula_weight 444.53 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6678(14) _cell_length_b 9.4087(15) _cell_length_c 13.727(2) _cell_angle_alpha 77.734(3) _cell_angle_beta 87.897(4) _cell_angle_gamma 87.815(4) _cell_volume 1092.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2551 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13017 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 29.00 _reflns_number_total 5781 _reflns_number_gt 4762 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0435P)^2^+0.3975P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5781 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 P1 P 0.39800(4) 1.06158(4) -0.20603(3) 0.01275(9) Uani 1 1 d . . . S1 S 0.28208(4) 1.16201(4) -0.11433(3) 0.01468(9) Uani 1 1 d . . . S2 S 0.27744(4) 0.34331(4) 0.18862(3) 0.01717(9) Uani 1 1 d . . . N1 N 0.49221(14) 0.54437(14) 0.16597(9) 0.0147(2) Uani 1 1 d . . . H1N H 0.5269 0.6312 0.1339 0.018 Uiso 1 1 d R . . N2 N 0.40930(15) 0.88159(14) -0.16824(9) 0.0158(3) Uani 1 1 d . . . H2N H 0.5081 0.8306 -0.1817 0.019 Uiso 1 1 d R . . C1 C 0.28741(17) 0.60536(16) 0.05292(11) 0.0139(3) Uani 1 1 d . . . C2 C 0.37859(17) 0.69722(16) -0.01789(10) 0.0132(3) Uani 1 1 d . . . H2A H 0.4878 0.6916 -0.0128 0.016 Uiso 1 1 calc R . . C3 C 0.31161(17) 0.79637(16) -0.09548(11) 0.0137(3) Uani 1 1 d . . . C4 C 0.15176(17) 0.80661(17) -0.10271(11) 0.0161(3) Uani 1 1 d . . . H4A H 0.1054 0.8746 -0.1556 0.019 Uiso 1 1 calc R . . C5 C 0.06037(17) 0.71659(17) -0.03188(11) 0.0165(3) Uani 1 1 d . . . H5A H -0.0489 0.7246 -0.0358 0.020 Uiso 1 1 calc R . . C6 C 0.12739(17) 0.61536(16) 0.04442(11) 0.0155(3) Uani 1 1 d . . . H6A H 0.0640 0.5524 0.0912 0.019 Uiso 1 1 calc R . . C7 C 0.32120(17) 1.10320(17) -0.33022(11) 0.0152(3) Uani 1 1 d . . . C8 C 0.26081(17) 1.24227(17) -0.36972(11) 0.0166(3) Uani 1 1 d . . . H8A H 0.2548 1.3141 -0.3303 0.020 Uiso 1 1 calc R . . C9 C 0.20948(19) 1.27521(19) -0.46678(12) 0.0218(3) Uani 1 1 d . . . H9A H 0.1682 1.3698 -0.4937 0.026 Uiso 1 1 calc R . . C10 C 0.2181(2) 1.1714(2) -0.52442(12) 0.0271(4) Uani 1 1 d . . . H10A H 0.1828 1.1946 -0.5908 0.033 Uiso 1 1 calc R . . C11 C 0.2782(2) 1.0332(2) -0.48538(13) 0.0330(4) Uani 1 1 d . . . H11A H 0.2842 0.9618 -0.5251 0.040 Uiso 1 1 calc R . . C12 C 0.3299(2) 0.9987(2) -0.38815(12) 0.0257(4) Uani 1 1 d . . . H12A H 0.3710 0.9040 -0.3615 0.031 Uiso 1 1 calc R . . C13 C 0.59827(17) 1.10841(17) -0.22178(11) 0.0148(3) Uani 1 1 d . . . C14 C 0.65103(19) 1.2100(2) -0.30340(12) 0.0231(4) Uani 1 1 d . . . H14A H 0.5831 1.2499 -0.3557 0.028 Uiso 1 1 calc R . . C15 C 0.8031(2) 1.2537(2) -0.30904(13) 0.0303(4) Uani 1 1 d . . . H15A H 0.8390 1.3238 -0.3649 0.036 Uiso 1 1 calc R . . C16 C 0.90206(19) 1.1949(2) -0.23312(13) 0.0261(4) Uani 1 1 d . . . H16A H 1.0063 1.2240 -0.2372 0.031 Uiso 1 1 calc R . . C17 C 0.84977(19) 1.09382(19) -0.15130(13) 0.0221(3) Uani 1 1 d . . . H17A H 0.9182 1.0539 -0.0993 0.026 Uiso 1 1 calc R . . C18 C 0.69829(18) 1.05051(17) -0.14472(12) 0.0185(3) Uani 1 1 d . . . H18A H 0.6625 0.9818 -0.0881 0.022 Uiso 1 1 calc R . . C19 C 0.35894(16) 0.50153(16) 0.13762(11) 0.0137(3) Uani 1 1 d . . . C20 C 0.58769(17) 0.47153(16) 0.24472(11) 0.0154(3) Uani 1 1 d . . . C21 C 0.52888(19) 0.42756(18) 0.34135(11) 0.0200(3) Uani 1 1 d . . . H21A H 0.4214 0.4371 0.3556 0.024 Uiso 1 1 calc R . . C22 C 0.6293(2) 0.36954(19) 0.41673(12) 0.0258(4) Uani 1 1 d . . . H22A H 0.5901 0.3394 0.4832 0.031 Uiso 1 1 calc R . . C23 C 0.7860(2) 0.35473(19) 0.39669(13) 0.0262(4) Uani 1 1 d . . . H23A H 0.8536 0.3147 0.4491 0.031 Uiso 1 1 calc R . . C24 C 0.8441(2) 0.39830(18) 0.30016(13) 0.0228(3) Uani 1 1 d . . . H24A H 0.9516 0.3880 0.2861 0.027 Uiso 1 1 calc R . . C25 C 0.74445(18) 0.45722(17) 0.22375(12) 0.0175(3) Uani 1 1 d . . . H25A H 0.7838 0.4876 0.1574 0.021 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 P1 0.01321(18) 0.01338(18) 0.01101(17) -0.00098(14) -0.00102(13) -0.00043(13) S1 0.01462(17) 0.01583(18) 0.01353(17) -0.00304(13) 0.00020(13) -0.00051(13) S2 0.01510(18) 0.01522(18) 0.01929(19) 0.00108(14) -0.00044(14) -0.00307(14) N1 0.0159(6) 0.0148(6) 0.0121(6) 0.0003(5) -0.0014(5) -0.0026(5) N2 0.0160(6) 0.0142(6) 0.0157(6) -0.0004(5) 0.0015(5) 0.0014(5) C1 0.0151(7) 0.0138(7) 0.0135(7) -0.0044(5) -0.0013(5) -0.0004(5) C2 0.0131(6) 0.0138(7) 0.0132(6) -0.0039(5) -0.0009(5) -0.0009(5) C3 0.0171(7) 0.0115(7) 0.0130(6) -0.0039(5) -0.0007(5) -0.0007(5) C4 0.0175(7) 0.0146(7) 0.0168(7) -0.0043(6) -0.0047(6) 0.0029(6) C5 0.0129(7) 0.0168(7) 0.0207(7) -0.0058(6) -0.0016(6) 0.0006(5) C6 0.0142(7) 0.0158(7) 0.0169(7) -0.0039(6) -0.0004(5) -0.0023(5) C7 0.0139(7) 0.0189(7) 0.0123(7) -0.0019(6) -0.0013(5) -0.0014(5) C8 0.0162(7) 0.0175(7) 0.0157(7) -0.0019(6) -0.0016(6) -0.0021(6) C9 0.0216(8) 0.0230(8) 0.0177(7) 0.0035(6) -0.0053(6) -0.0015(6) C10 0.0322(9) 0.0344(10) 0.0138(7) -0.0012(7) -0.0074(7) -0.0036(8) C11 0.0516(12) 0.0305(10) 0.0197(8) -0.0107(7) -0.0112(8) 0.0029(9) C12 0.0368(10) 0.0221(8) 0.0188(8) -0.0055(7) -0.0078(7) 0.0052(7) C13 0.0130(7) 0.0175(7) 0.0139(7) -0.0038(6) -0.0002(5) 0.0011(5) C14 0.0174(8) 0.0350(10) 0.0144(7) 0.0009(7) -0.0014(6) -0.0045(7) C15 0.0208(8) 0.0471(12) 0.0206(8) -0.0002(8) 0.0042(7) -0.0127(8) C16 0.0137(7) 0.0411(11) 0.0268(9) -0.0145(8) 0.0014(6) -0.0021(7) C17 0.0185(8) 0.0256(9) 0.0249(8) -0.0115(7) -0.0075(6) 0.0053(6) C18 0.0205(8) 0.0172(7) 0.0175(7) -0.0024(6) -0.0040(6) 0.0013(6) C19 0.0130(7) 0.0149(7) 0.0134(7) -0.0036(5) 0.0019(5) -0.0013(5) C20 0.0174(7) 0.0135(7) 0.0158(7) -0.0031(6) -0.0044(6) -0.0018(5) C21 0.0215(8) 0.0221(8) 0.0159(7) -0.0025(6) 0.0004(6) -0.0017(6) C22 0.0356(10) 0.0268(9) 0.0132(7) 0.0003(6) -0.0037(7) -0.0026(7) C23 0.0323(9) 0.0235(9) 0.0220(8) -0.0019(7) -0.0137(7) 0.0033(7) C24 0.0209(8) 0.0208(8) 0.0276(8) -0.0066(7) -0.0076(7) 0.0027(6) C25 0.0194(7) 0.0168(7) 0.0171(7) -0.0053(6) -0.0015(6) -0.0009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N2 1.6626(13) . ? P1 C13 1.8013(15) . ? P1 C7 1.8117(15) . ? P1 S1 1.9563(6) . ? S2 C19 1.6752(15) . ? N1 C19 1.3354(19) . ? N1 C20 1.4251(19) . ? N1 H1N 0.8987 . ? N2 C3 1.4166(19) . ? N2 H2N 0.9961 . ? C1 C6 1.394(2) . ? C1 C2 1.398(2) . ? C1 C19 1.488(2) . ? C2 C3 1.387(2) . ? C2 H2A 0.9500 . ? C3 C4 1.391(2) . ? C4 C5 1.391(2) . ? C4 H4A 0.9500 . ? C5 C6 1.386(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.388(2) . ? C7 C8 1.395(2) . ? C8 C9 1.388(2) . ? C8 H8A 0.9500 . ? C9 C10 1.380(2) . ? C9 H9A 0.9500 . ? C10 C11 1.387(3) . ? C10 H10A 0.9500 . ? C11 C12 1.391(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.385(2) . ? C13 C18 1.398(2) . ? C14 C15 1.391(2) . ? C14 H14A 0.9500 . ? C15 C16 1.383(2) . ? C15 H15A 0.9500 . ? C16 C17 1.383(2) . ? C16 H16A 0.9500 . ? C17 C18 1.384(2) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C20 C25 1.386(2) . ? C20 C21 1.387(2) . ? C21 C22 1.384(2) . ? C21 H21A 0.9500 . ? C22 C23 1.383(3) . ? C22 H22A 0.9500 . ? C23 C24 1.383(3) . ? C23 H23A 0.9500 . ? C24 C25 1.391(2) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? 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 N2 P1 C13 102.34(7) . . ? N2 P1 C7 107.99(7) . . ? C13 P1 C7 105.66(7) . . ? N2 P1 S1 114.34(5) . . ? C13 P1 S1 113.26(5) . . ? C7 P1 S1 112.41(5) . . ? C19 N1 C20 128.19(13) . . ? C19 N1 H1N 117.9 . . ? C20 N1 H1N 113.9 . . ? C3 N2 P1 126.00(11) . . ? C3 N2 H2N 113.8 . . ? P1 N2 H2N 117.8 . . ? C6 C1 C2 118.80(13) . . ? C6 C1 C19 120.34(13) . . ? C2 C1 C19 120.84(13) . . ? C3 C2 C1 120.81(14) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C2 C3 C4 119.96(14) . . ? C2 C3 N2 118.62(13) . . ? C4 C3 N2 121.37(13) . . ? C3 C4 C5 119.49(14) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 120.55(14) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C1 120.36(14) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? C12 C7 C8 119.88(14) . . ? C12 C7 P1 119.84(12) . . ? C8 C7 P1 120.18(12) . . ? C9 C8 C7 119.74(15) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C10 C9 C8 120.40(16) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 C11 119.97(15) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 C12 120.18(17) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C7 C12 C11 119.83(16) . . ? C7 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C18 119.75(14) . . ? C14 C13 P1 121.52(11) . . ? C18 C13 P1 118.45(12) . . ? C13 C14 C15 120.19(15) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C16 C15 C14 119.82(16) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C17 120.21(16) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C16 C17 C18 120.37(15) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C13 119.66(15) . . ? C17 C18 H18A 120.2 . . ? C13 C18 H18A 120.2 . . ? N1 C19 C1 114.31(13) . . ? N1 C19 S2 124.39(11) . . ? C1 C19 S2 121.27(11) . . ? C25 C20 C21 120.60(14) . . ? C25 C20 N1 117.83(13) . . ? C21 C20 N1 121.33(14) . . ? C22 C21 C20 118.96(15) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? C23 C22 C21 120.95(16) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C24 C23 C22 119.89(15) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C25 119.74(16) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C20 C25 C24 119.86(15) . . ? C20 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? 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 C13 P1 N2 C3 141.82(12) . . . . ? C7 P1 N2 C3 -106.99(13) . . . . ? S1 P1 N2 C3 18.95(14) . . . . ? C6 C1 C2 C3 -0.2(2) . . . . ? C19 C1 C2 C3 -178.46(13) . . . . ? C1 C2 C3 C4 0.9(2) . . . . ? C1 C2 C3 N2 -176.71(13) . . . . ? P1 N2 C3 C2 -128.88(13) . . . . ? P1 N2 C3 C4 53.57(19) . . . . ? C2 C3 C4 C5 -0.2(2) . . . . ? N2 C3 C4 C5 177.34(13) . . . . ? C3 C4 C5 C6 -1.2(2) . . . . ? C4 C5 C6 C1 1.9(2) . . . . ? C2 C1 C6 C5 -1.2(2) . . . . ? C19 C1 C6 C5 177.08(14) . . . . ? N2 P1 C7 C12 -20.60(15) . . . . ? C13 P1 C7 C12 88.32(14) . . . . ? S1 P1 C7 C12 -147.67(12) . . . . ? N2 P1 C7 C8 162.79(12) . . . . ? C13 P1 C7 C8 -88.29(13) . . . . ? S1 P1 C7 C8 35.72(14) . . . . ? C12 C7 C8 C9 0.1(2) . . . . ? P1 C7 C8 C9 176.72(12) . . . . ? C7 C8 C9 C10 -0.1(2) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? C9 C10 C11 C12 0.1(3) . . . . ? C8 C7 C12 C11 0.0(3) . . . . ? P1 C7 C12 C11 -176.66(15) . . . . ? C10 C11 C12 C7 0.0(3) . . . . ? N2 P1 C13 C14 137.35(14) . . . . ? C7 P1 C13 C14 24.41(15) . . . . ? S1 P1 C13 C14 -99.06(14) . . . . ? N2 P1 C13 C18 -48.81(13) . . . . ? C7 P1 C13 C18 -161.75(12) . . . . ? S1 P1 C13 C18 74.78(13) . . . . ? C18 C13 C14 C15 0.4(3) . . . . ? P1 C13 C14 C15 174.13(14) . . . . ? C13 C14 C15 C16 0.3(3) . . . . ? C14 C15 C16 C17 -0.6(3) . . . . ? C15 C16 C17 C18 0.1(3) . . . . ? C16 C17 C18 C13 0.6(2) . . . . ? C14 C13 C18 C17 -0.8(2) . . . . ? P1 C13 C18 C17 -174.79(12) . . . . ? C20 N1 C19 C1 179.10(13) . . . . ? C20 N1 C19 S2 -2.6(2) . . . . ? C6 C1 C19 N1 -149.88(14) . . . . ? C2 C1 C19 N1 28.4(2) . . . . ? C6 C1 C19 S2 31.74(19) . . . . ? C2 C1 C19 S2 -150.01(12) . . . . ? C19 N1 C20 C25 131.67(16) . . . . ? C19 N1 C20 C21 -53.9(2) . . . . ? C25 C20 C21 C22 0.2(2) . . . . ? N1 C20 C21 C22 -174.04(15) . . . . ? C20 C21 C22 C23 -0.2(3) . . . . ? C21 C22 C23 C24 0.0(3) . . . . ? C22 C23 C24 C25 0.2(3) . . . . ? C21 C20 C25 C24 0.0(2) . . . . ? N1 C20 C25 C24 174.43(14) . . . . ? C23 C24 C25 C20 -0.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.465 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.061 data_8a _database_code_depnum_ccdc_archive 'CCDC 791556' #TrackingRef '- 8a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H20 Cl N2 P Pd S2, C2 H6 O S' _chemical_formula_sum 'C27 H26 Cl N2 O P Pd S3' _chemical_formula_weight 663.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5061(6) _cell_length_b 9.2117(7) _cell_length_c 17.5787(13) _cell_angle_alpha 101.584(2) _cell_angle_beta 94.219(1) _cell_angle_gamma 90.813(1) _cell_volume 1345.09(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2554 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.856 _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16148 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7137 _reflns_number_gt 6011 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0181P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7137 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 -0.116771(17) 0.794575(16) 0.235183(9) 0.01186(4) Uani 1 1 d . . . Cl1 Cl -0.36834(6) 0.85643(6) 0.18104(3) 0.02000(11) Uani 1 1 d . . . P1 P 0.16349(6) 0.81042(6) 0.12207(3) 0.01350(11) Uani 1 1 d . . . S1 S -0.04973(6) 0.71682(6) 0.10684(3) 0.01820(11) Uani 1 1 d . . . S2 S -0.21744(6) 0.83947(6) 0.35361(3) 0.01524(10) Uani 1 1 d . . . N1 N -0.0940(2) 0.73990(18) 0.47528(9) 0.0156(4) Uani 1 1 d . . . H1N H -0.0236 0.6842 0.4967 0.019 Uiso 1 1 d R . . N2 N 0.27343(19) 0.75036(18) 0.18914(9) 0.0147(3) Uani 1 1 d . . . H2N H 0.3731 0.7486 0.1807 0.018 Uiso 1 1 d R . . C1 C 0.0783(2) 0.7388(2) 0.37165(11) 0.0134(4) Uani 1 1 d . . . C2 C 0.0859(2) 0.7520(2) 0.29260(11) 0.0131(4) Uani 1 1 d . . . C3 C 0.2363(2) 0.7338(2) 0.26419(11) 0.0135(4) Uani 1 1 d . . . C4 C 0.3658(2) 0.6984(2) 0.31027(12) 0.0161(4) Uani 1 1 d . . . H4A H 0.4645 0.6821 0.2885 0.019 Uiso 1 1 calc R . . C5 C 0.3530(2) 0.6866(2) 0.38665(12) 0.0175(4) Uani 1 1 d . . . H5A H 0.4424 0.6639 0.4173 0.021 Uiso 1 1 calc R . . C6 C 0.2093(2) 0.7079(2) 0.41806(12) 0.0162(4) Uani 1 1 d . . . H6A H 0.1994 0.7018 0.4708 0.019 Uiso 1 1 calc R . . C7 C 0.1610(2) 1.0107(2) 0.14375(11) 0.0144(4) Uani 1 1 d . . . C8 C 0.0479(3) 1.0837(2) 0.10544(12) 0.0196(4) Uani 1 1 d . . . H8A H -0.0317 1.0280 0.0704 0.024 Uiso 1 1 calc R . . C9 C 0.0508(3) 1.2373(2) 0.11826(12) 0.0225(5) Uani 1 1 d . . . H9A H -0.0245 1.2869 0.0909 0.027 Uiso 1 1 calc R . . C10 C 0.1645(3) 1.3181(2) 0.17133(12) 0.0223(5) Uani 1 1 d . . . H10A H 0.1669 1.4233 0.1803 0.027 Uiso 1 1 calc R . . C11 C 0.2741(3) 1.2461(2) 0.21109(12) 0.0209(5) Uani 1 1 d . . . H11A H 0.3495 1.3023 0.2485 0.025 Uiso 1 1 calc R . . C12 C 0.2750(2) 1.0923(2) 0.19690(12) 0.0176(4) Uani 1 1 d . . . H12A H 0.3526 1.0432 0.2232 0.021 Uiso 1 1 calc R . . C13 C 0.2677(2) 0.7557(2) 0.03609(11) 0.0146(4) Uani 1 1 d . . . C14 C 0.3274(2) 0.8577(2) -0.00381(12) 0.0188(4) Uani 1 1 d . . . H14A H 0.3165 0.9609 0.0150 0.023 Uiso 1 1 calc R . . C15 C 0.4031(2) 0.8081(2) -0.07117(12) 0.0224(5) Uani 1 1 d . . . H15A H 0.4439 0.8773 -0.0987 0.027 Uiso 1 1 calc R . . C16 C 0.4189(2) 0.6574(2) -0.09805(12) 0.0223(5) Uani 1 1 d . . . H16A H 0.4720 0.6238 -0.1437 0.027 Uiso 1 1 calc R . . C17 C 0.3581(2) 0.5551(2) -0.05913(12) 0.0198(4) Uani 1 1 d . . . H17A H 0.3689 0.4520 -0.0783 0.024 Uiso 1 1 calc R . . C18 C 0.2820(2) 0.6037(2) 0.00743(12) 0.0180(4) Uani 1 1 d . . . H18A H 0.2390 0.5339 0.0339 0.022 Uiso 1 1 calc R . . C19 C -0.0731(2) 0.7690(2) 0.40572(11) 0.0129(4) Uani 1 1 d . . . C20 C -0.2347(2) 0.7665(2) 0.51558(11) 0.0154(4) Uani 1 1 d . . . C21 C -0.2909(2) 0.9082(2) 0.53530(11) 0.0189(4) Uani 1 1 d . . . H21A H -0.2390 0.9890 0.5205 0.023 Uiso 1 1 calc R . . C22 C -0.4235(3) 0.9310(2) 0.57684(12) 0.0210(5) Uani 1 1 d . . . H22A H -0.4633 1.0279 0.5905 0.025 Uiso 1 1 calc R . . C23 C -0.4981(3) 0.8135(2) 0.59850(12) 0.0215(5) Uani 1 1 d . . . H23A H -0.5895 0.8296 0.6267 0.026 Uiso 1 1 calc R . . C24 C -0.4407(3) 0.6729(2) 0.57936(12) 0.0216(5) Uani 1 1 d . . . H24A H -0.4926 0.5925 0.5946 0.026 Uiso 1 1 calc R . . C25 C -0.3072(2) 0.6480(2) 0.53786(12) 0.0180(4) Uani 1 1 d . . . H25A H -0.2666 0.5514 0.5251 0.022 Uiso 1 1 calc R . . O1S O 0.90475(18) 0.39528(16) 0.42350(8) 0.0237(3) Uani 1 1 d . . . S1S S 0.95629(6) 0.36644(6) 0.34141(3) 0.01740(11) Uani 1 1 d . . . C1S C 0.7898(3) 0.4044(2) 0.28187(12) 0.0248(5) Uani 1 1 d . . . H1SA H 0.7672 0.5101 0.2955 0.037 Uiso 1 1 calc R . . H1SB H 0.6982 0.3456 0.2904 0.037 Uiso 1 1 calc R . . H1SC H 0.8123 0.3785 0.2270 0.037 Uiso 1 1 calc R . . C2S C 0.9489(3) 0.1699(2) 0.31009(12) 0.0225(5) Uani 1 1 d . . . H2SA H 1.0363 0.1273 0.3370 0.034 Uiso 1 1 calc R . . H2SB H 0.9578 0.1442 0.2537 0.034 Uiso 1 1 calc R . . H2SC H 0.8485 0.1300 0.3224 0.034 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 0.00980(7) 0.01450(8) 0.01155(7) 0.00303(6) 0.00149(5) -0.00019(5) Cl1 0.0117(2) 0.0306(3) 0.0197(3) 0.0096(2) 0.0015(2) 0.0024(2) P1 0.0110(2) 0.0179(3) 0.0111(2) 0.0015(2) 0.0013(2) 0.0002(2) S1 0.0118(2) 0.0275(3) 0.0134(2) -0.0002(2) 0.0017(2) -0.0031(2) S2 0.0140(2) 0.0191(3) 0.0139(2) 0.0054(2) 0.0034(2) 0.00300(19) N1 0.0182(9) 0.0157(9) 0.0142(8) 0.0045(7) 0.0042(7) 0.0040(7) N2 0.0085(8) 0.0216(9) 0.0151(8) 0.0053(7) 0.0030(7) 0.0016(7) C1 0.0147(10) 0.0108(9) 0.0149(10) 0.0024(8) 0.0044(8) -0.0014(7) C2 0.0151(10) 0.0101(9) 0.0140(9) 0.0026(7) -0.0005(8) -0.0012(7) C3 0.0153(10) 0.0112(9) 0.0135(9) 0.0015(8) 0.0007(8) -0.0022(7) C4 0.0113(9) 0.0164(10) 0.0208(11) 0.0040(8) 0.0015(8) 0.0004(8) C5 0.0157(10) 0.0173(10) 0.0204(11) 0.0069(8) -0.0019(9) 0.0015(8) C6 0.0192(10) 0.0150(10) 0.0153(10) 0.0056(8) 0.0013(8) -0.0011(8) C7 0.0150(10) 0.0176(10) 0.0102(9) 0.0009(8) 0.0048(8) 0.0011(8) C8 0.0217(11) 0.0241(11) 0.0116(10) 0.0010(8) -0.0007(8) 0.0027(9) C9 0.0279(12) 0.0256(12) 0.0155(10) 0.0066(9) 0.0022(9) 0.0087(9) C10 0.0299(12) 0.0177(11) 0.0207(11) 0.0040(9) 0.0101(10) 0.0007(9) C11 0.0189(11) 0.0229(11) 0.0194(11) 0.0001(9) 0.0046(9) -0.0039(9) C12 0.0141(10) 0.0234(11) 0.0154(10) 0.0035(9) 0.0035(8) 0.0018(8) C13 0.0100(9) 0.0205(10) 0.0123(9) 0.0014(8) -0.0006(8) 0.0007(8) C14 0.0177(10) 0.0200(11) 0.0173(10) -0.0003(8) 0.0029(9) -0.0033(8) C15 0.0189(11) 0.0312(13) 0.0179(11) 0.0058(9) 0.0052(9) -0.0057(9) C16 0.0147(10) 0.0356(13) 0.0139(10) -0.0026(9) 0.0031(8) 0.0002(9) C17 0.0158(10) 0.0225(11) 0.0186(11) -0.0015(9) 0.0002(9) 0.0017(8) C18 0.0146(10) 0.0223(11) 0.0171(10) 0.0037(9) 0.0011(8) 0.0001(8) C19 0.0159(10) 0.0093(9) 0.0131(9) 0.0015(7) 0.0008(8) -0.0021(7) C20 0.0164(10) 0.0205(11) 0.0095(9) 0.0029(8) 0.0025(8) 0.0018(8) C21 0.0237(11) 0.0170(10) 0.0159(10) 0.0023(8) 0.0034(9) -0.0007(9) C22 0.0269(12) 0.0181(11) 0.0175(11) 0.0004(9) 0.0059(9) 0.0083(9) C23 0.0187(11) 0.0289(12) 0.0179(11) 0.0048(9) 0.0072(9) 0.0049(9) C24 0.0236(11) 0.0222(11) 0.0213(11) 0.0081(9) 0.0061(9) -0.0013(9) C25 0.0223(11) 0.0154(10) 0.0168(10) 0.0034(8) 0.0029(9) 0.0028(8) O1S 0.0354(9) 0.0252(8) 0.0111(7) 0.0030(6) 0.0042(7) 0.0130(7) S1S 0.0245(3) 0.0148(2) 0.0125(2) 0.0019(2) 0.0017(2) -0.0001(2) C1S 0.0313(13) 0.0262(12) 0.0168(11) 0.0057(9) -0.0025(10) 0.0026(10) C2S 0.0297(12) 0.0153(11) 0.0224(11) 0.0009(9) 0.0099(10) 0.0013(9) _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 C2 2.0167(19) . ? Pd1 S2 2.2725(5) . ? Pd1 S1 2.3409(5) . ? Pd1 Cl1 2.4004(5) . ? P1 N2 1.6386(17) . ? P1 C13 1.797(2) . ? P1 C7 1.808(2) . ? P1 S1 1.9738(7) . ? S2 C19 1.692(2) . ? N1 C19 1.327(2) . ? N1 C20 1.435(2) . ? N1 H1N 0.9038 . ? N2 C3 1.416(2) . ? N2 H2N 0.8710 . ? C1 C6 1.399(3) . ? C1 C2 1.425(3) . ? C1 C19 1.467(3) . ? C2 C3 1.407(3) . ? C3 C4 1.400(3) . ? C4 C5 1.381(3) . ? C4 H4A 0.9500 . ? C5 C6 1.378(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.392(3) . ? C7 C12 1.394(3) . ? C8 C9 1.387(3) . ? C8 H8A 0.9500 . ? C9 C10 1.388(3) . ? C9 H9A 0.9500 . ? C10 C11 1.380(3) . ? C10 H10A 0.9500 . ? C11 C12 1.389(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.392(3) . ? C13 C18 1.399(3) . ? C14 C15 1.389(3) . ? C14 H14A 0.9500 . ? C15 C16 1.386(3) . ? C15 H15A 0.9500 . ? C16 C17 1.386(3) . ? C16 H16A 0.9500 . ? C17 C18 1.378(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C20 C25 1.383(3) . ? C20 C21 1.383(3) . ? C21 C22 1.384(3) . ? C21 H21A 0.9500 . ? C22 C23 1.378(3) . ? C22 H22A 0.9500 . ? C23 C24 1.377(3) . ? C23 H23A 0.9500 . ? C24 C25 1.392(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? O1S S1S 1.5124(14) . ? S1S C1S 1.779(2) . ? S1S C2S 1.783(2) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 S2 85.90(6) . . ? C2 Pd1 S1 99.52(6) . . ? S2 Pd1 S1 169.798(19) . . ? C2 Pd1 Cl1 173.51(6) . . ? S2 Pd1 Cl1 87.741(18) . . ? S1 Pd1 Cl1 86.958(18) . . ? N2 P1 C13 103.39(9) . . ? N2 P1 C7 110.43(9) . . ? C13 P1 C7 107.51(9) . . ? N2 P1 S1 111.54(6) . . ? C13 P1 S1 110.52(7) . . ? C7 P1 S1 112.96(7) . . ? P1 S1 Pd1 96.75(2) . . ? C19 S2 Pd1 99.54(7) . . ? C19 N1 C20 125.44(17) . . ? C19 N1 H1N 119.5 . . ? C20 N1 H1N 114.1 . . ? C3 N2 P1 129.10(14) . . ? C3 N2 H2N 116.2 . . ? P1 N2 H2N 113.0 . . ? C6 C1 C2 123.04(18) . . ? C6 C1 C19 119.77(18) . . ? C2 C1 C19 117.07(18) . . ? C3 C2 C1 115.17(18) . . ? C3 C2 Pd1 127.85(15) . . ? C1 C2 Pd1 116.98(14) . . ? C4 C3 C2 121.39(18) . . ? C4 C3 N2 113.62(17) . . ? C2 C3 N2 124.98(18) . . ? C5 C4 C3 121.41(19) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C6 C5 C4 119.44(19) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C1 119.47(19) . . ? C5 C6 H6A 120.3 . . ? C1 C6 H6A 120.3 . . ? C8 C7 C12 119.85(19) . . ? C8 C7 P1 119.87(15) . . ? C12 C7 P1 120.25(16) . . ? C9 C8 C7 120.26(19) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 120.5(2) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C11 C12 C7 119.5(2) . . ? C11 C12 H12A 120.3 . . ? C7 C12 H12A 120.3 . . ? C14 C13 C18 119.83(18) . . ? C14 C13 P1 122.53(16) . . ? C18 C13 P1 117.58(15) . . ? C15 C14 C13 119.8(2) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 119.7(2) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C17 120.83(19) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 119.7(2) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C13 120.15(19) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? N1 C19 C1 119.88(18) . . ? N1 C19 S2 121.99(15) . . ? C1 C19 S2 118.13(14) . . ? C25 C20 C21 121.07(19) . . ? C25 C20 N1 118.09(18) . . ? C21 C20 N1 120.74(18) . . ? C20 C21 C22 119.31(19) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 120.18(19) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C20 C25 C24 118.83(19) . . ? C20 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? O1S S1S C1S 105.48(10) . . ? O1S S1S C2S 105.40(9) . . ? C1S S1S C2S 97.39(11) . . ? S1S C1S H1SA 109.5 . . ? S1S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? S1S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? S1S C2S H2SA 109.5 . . ? S1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? S1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 P1 S1 Pd1 58.39(7) . . . . ? C13 P1 S1 Pd1 172.82(7) . . . . ? C7 P1 S1 Pd1 -66.69(7) . . . . ? C2 Pd1 S1 P1 -44.03(6) . . . . ? S2 Pd1 S1 P1 -165.57(10) . . . . ? Cl1 Pd1 S1 P1 135.64(3) . . . . ? C2 Pd1 S2 C19 -12.73(8) . . . . ? S1 Pd1 S2 C19 109.84(12) . . . . ? Cl1 Pd1 S2 C19 168.57(7) . . . . ? C13 P1 N2 C3 -165.57(16) . . . . ? C7 P1 N2 C3 79.68(18) . . . . ? S1 P1 N2 C3 -46.80(18) . . . . ? C6 C1 C2 C3 -0.8(3) . . . . ? C19 C1 C2 C3 175.10(16) . . . . ? C6 C1 C2 Pd1 179.33(14) . . . . ? C19 C1 C2 Pd1 -4.7(2) . . . . ? S2 Pd1 C2 C3 -168.69(17) . . . . ? S1 Pd1 C2 C3 20.02(17) . . . . ? S2 Pd1 C2 C1 11.11(13) . . . . ? S1 Pd1 C2 C1 -160.18(13) . . . . ? C1 C2 C3 C4 2.9(3) . . . . ? Pd1 C2 C3 C4 -177.34(14) . . . . ? C1 C2 C3 N2 -176.29(17) . . . . ? Pd1 C2 C3 N2 3.5(3) . . . . ? P1 N2 C3 C4 -171.76(14) . . . . ? P1 N2 C3 C2 7.4(3) . . . . ? C2 C3 C4 C5 -3.0(3) . . . . ? N2 C3 C4 C5 176.21(17) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? C4 C5 C6 C1 1.1(3) . . . . ? C2 C1 C6 C5 -1.1(3) . . . . ? C19 C1 C6 C5 -176.95(17) . . . . ? N2 P1 C7 C8 -165.04(15) . . . . ? C13 P1 C7 C8 82.84(17) . . . . ? S1 P1 C7 C8 -39.36(18) . . . . ? N2 P1 C7 C12 16.96(19) . . . . ? C13 P1 C7 C12 -95.17(17) . . . . ? S1 P1 C7 C12 142.64(14) . . . . ? C12 C7 C8 C9 1.9(3) . . . . ? P1 C7 C8 C9 -176.16(16) . . . . ? C7 C8 C9 C10 -1.9(3) . . . . ? C8 C9 C10 C11 0.1(3) . . . . ? C9 C10 C11 C12 1.9(3) . . . . ? C10 C11 C12 C7 -1.9(3) . . . . ? C8 C7 C12 C11 0.1(3) . . . . ? P1 C7 C12 C11 178.08(15) . . . . ? N2 P1 C13 C14 -118.49(17) . . . . ? C7 P1 C13 C14 -1.7(2) . . . . ? S1 P1 C13 C14 122.04(16) . . . . ? N2 P1 C13 C18 64.25(17) . . . . ? C7 P1 C13 C18 -178.92(15) . . . . ? S1 P1 C13 C18 -55.22(16) . . . . ? C18 C13 C14 C15 -1.0(3) . . . . ? P1 C13 C14 C15 -178.22(16) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C17 0.9(3) . . . . ? C15 C16 C17 C18 -0.5(3) . . . . ? C16 C17 C18 C13 -0.7(3) . . . . ? C14 C13 C18 C17 1.5(3) . . . . ? P1 C13 C18 C17 178.81(15) . . . . ? C20 N1 C19 C1 178.88(17) . . . . ? C20 N1 C19 S2 -1.6(3) . . . . ? C6 C1 C19 N1 -12.7(3) . . . . ? C2 C1 C19 N1 171.17(17) . . . . ? C6 C1 C19 S2 167.76(14) . . . . ? C2 C1 C19 S2 -8.3(2) . . . . ? Pd1 S2 C19 N1 -164.85(15) . . . . ? Pd1 S2 C19 C1 14.64(15) . . . . ? C19 N1 C20 C25 123.3(2) . . . . ? C19 N1 C20 C21 -60.2(3) . . . . ? C25 C20 C21 C22 -1.1(3) . . . . ? N1 C20 C21 C22 -177.49(19) . . . . ? C20 C21 C22 C23 0.3(3) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C22 C23 C24 C25 -0.1(3) . . . . ? C21 C20 C25 C24 1.4(3) . . . . ? N1 C20 C25 C24 177.81(19) . . . . ? C23 C24 C25 C20 -0.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1N O1S 2_666 0.90 1.94 2.799(2) 159 ? N2 H2N Cl1 1_655 0.87 2.40 3.2086(17) 155 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.788 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.082 data_9a _database_code_depnum_ccdc_archive 'CCDC 791557' #TrackingRef '- 9a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H19 Cl N O P Pd S2, C2 H6 O S' _chemical_formula_sum 'C27 H25 Cl N O2 P Pd S3' _chemical_formula_weight 664.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.7874(10) _cell_length_b 9.6210(7) _cell_length_c 21.4447(15) _cell_angle_alpha 90.00 _cell_angle_beta 107.1200(10) _cell_angle_gamma 90.00 _cell_volume 2718.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2245 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.766 _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28131 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 29.00 _reflns_number_total 14280 _reflns_number_gt 12724 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0057P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.268(14) _refine_ls_number_reflns 14280 _refine_ls_number_parameters 654 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.731566(16) 0.937699(19) 0.125669(10) 0.01162(5) Uani 1 1 d . . . Cl1 Cl 0.87639(6) 1.03605(9) 0.20231(4) 0.01744(17) Uani 1 1 d . . . P1 P 0.77613(6) 0.76586(9) 0.00615(4) 0.01269(17) Uani 1 1 d . . . S1 S 0.82821(6) 0.94050(10) 0.05176(4) 0.01544(16) Uani 1 1 d . . . S2 S 0.64688(6) 0.97414(9) 0.19973(4) 0.01639(19) Uani 1 1 d . . . O1 O 0.65653(15) 0.7668(2) -0.02345(9) 0.0138(5) Uani 1 1 d . . . N1 N 0.45212(19) 0.9154(3) 0.18230(12) 0.0168(6) Uani 1 1 d . . . H1N H 0.3886 0.8991 0.1542 0.020 Uiso 1 1 d R . . C1 C 0.5240(2) 0.8214(3) 0.10161(14) 0.0128(6) Uani 1 1 d . . . C2 C 0.6058(2) 0.8358(3) 0.07364(14) 0.0117(6) Uani 1 1 d . . . C3 C 0.5901(2) 0.7602(3) 0.01592(15) 0.0129(6) Uani 1 1 d . . . C4 C 0.5086(2) 0.6721(3) -0.01019(14) 0.0155(7) Uani 1 1 d . . . H4A H 0.5040 0.6222 -0.0492 0.019 Uiso 1 1 calc R . . C5 C 0.4341(2) 0.6570(3) 0.02042(14) 0.0175(6) Uani 1 1 d . . . H5A H 0.3787 0.5954 0.0036 0.021 Uiso 1 1 calc R . . C6 C 0.4420(2) 0.7338(3) 0.07617(14) 0.0176(6) Uani 1 1 d . . . H6A H 0.3906 0.7264 0.0973 0.021 Uiso 1 1 calc R . . C7 C 0.8085(2) 0.6148(4) 0.05686(14) 0.0142(7) Uani 1 1 d . . . C8 C 0.8708(2) 0.6235(3) 0.12064(14) 0.0154(7) Uani 1 1 d . . . H8A H 0.8967 0.7109 0.1386 0.018 Uiso 1 1 calc R . . C9 C 0.8947(2) 0.5045(4) 0.15780(16) 0.0208(8) Uani 1 1 d . . . H9A H 0.9382 0.5097 0.2013 0.025 Uiso 1 1 calc R . . C10 C 0.8555(3) 0.3771(4) 0.13194(17) 0.0232(8) Uani 1 1 d . . . H10A H 0.8718 0.2956 0.1579 0.028 Uiso 1 1 calc R . . C11 C 0.7929(2) 0.3682(3) 0.06865(16) 0.0238(8) Uani 1 1 d . . . H11A H 0.7660 0.2808 0.0512 0.029 Uiso 1 1 calc R . . C12 C 0.7695(2) 0.4862(3) 0.03070(15) 0.0201(7) Uani 1 1 d . . . H12A H 0.7271 0.4802 -0.0131 0.024 Uiso 1 1 calc R . . C13 C 0.8171(2) 0.7478(3) -0.06505(15) 0.0139(7) Uani 1 1 d . . . C14 C 0.8928(2) 0.6533(3) -0.06730(15) 0.0156(7) Uani 1 1 d . . . H14A H 0.9179 0.5888 -0.0328 0.019 Uiso 1 1 calc R . . C15 C 0.9310(2) 0.6542(4) -0.12023(15) 0.0176(7) Uani 1 1 d . . . H15A H 0.9827 0.5904 -0.1220 0.021 Uiso 1 1 calc R . . C16 C 0.8939(2) 0.7480(3) -0.17043(15) 0.0208(7) Uani 1 1 d . . . H16A H 0.9210 0.7492 -0.2063 0.025 Uiso 1 1 calc R . . C17 C 0.8176(2) 0.8403(3) -0.16885(13) 0.0225(7) Uani 1 1 d . . . H17A H 0.7917 0.9032 -0.2040 0.027 Uiso 1 1 calc R . . C18 C 0.7790(2) 0.8412(3) -0.11621(14) 0.0198(6) Uani 1 1 d . . . H18A H 0.7270 0.9048 -0.1149 0.024 Uiso 1 1 calc R . . C19 C 0.5331(2) 0.9012(3) 0.16154(14) 0.0142(7) Uani 1 1 d . . . C20 C 0.4441(2) 0.9850(3) 0.24007(15) 0.0168(7) Uani 1 1 d . . . C21 C 0.5181(2) 0.9719(3) 0.29986(13) 0.0206(6) Uani 1 1 d . . . H21A H 0.5786 0.9209 0.3035 0.025 Uiso 1 1 calc R . . C22 C 0.5018(2) 1.0350(3) 0.35444(14) 0.0252(7) Uani 1 1 d . . . H22A H 0.5524 1.0297 0.3955 0.030 Uiso 1 1 calc R . . C23 C 0.4119(3) 1.1055(4) 0.34900(16) 0.0269(8) Uani 1 1 d . . . H23A H 0.4004 1.1459 0.3866 0.032 Uiso 1 1 calc R . . C24 C 0.3393(2) 1.1173(3) 0.28942(15) 0.0263(7) Uani 1 1 d . . . H24A H 0.2784 1.1671 0.2858 0.032 Uiso 1 1 calc R . . C25 C 0.3554(2) 1.0562(3) 0.23465(14) 0.0208(7) Uani 1 1 d . . . H25A H 0.3053 1.0636 0.1935 0.025 Uiso 1 1 calc R . . S1S S 0.20534(5) 0.72414(8) 0.14215(4) 0.02034(16) Uani 1 1 d . . . O1S O 0.25135(17) 0.8490(3) 0.11895(10) 0.0215(5) Uani 1 1 d . . . C1S C 0.0948(2) 0.6838(3) 0.07692(15) 0.0286(8) Uani 1 1 d . . . H1SA H 0.1148 0.6527 0.0390 0.043 Uiso 1 1 calc R . . H1SB H 0.0520 0.7668 0.0653 0.043 Uiso 1 1 calc R . . H1SC H 0.0567 0.6097 0.0906 0.043 Uiso 1 1 calc R . . C2S C 0.1443(2) 0.7865(3) 0.19909(15) 0.0244(8) Uani 1 1 d . . . H2SA H 0.1954 0.8230 0.2377 0.037 Uiso 1 1 calc R . . H2SB H 0.1073 0.7102 0.2121 0.037 Uiso 1 1 calc R . . H2SC H 0.0967 0.8606 0.1789 0.037 Uiso 1 1 calc R . . Pd1A Pd 0.273688(16) 0.596571(19) 0.380484(10) 0.01166(5) Uani 1 1 d . . . Cl1A Cl 0.12609(6) 0.49689(9) 0.30530(4) 0.01685(17) Uani 1 1 d . . . P1A P 0.22708(6) 0.77388(9) 0.49675(4) 0.01264(17) Uani 1 1 d . . . S1A S 0.18122(6) 0.59176(10) 0.45743(4) 0.01728(17) Uani 1 1 d . . . S2A S 0.35723(6) 0.55948(9) 0.30607(4) 0.0183(2) Uani 1 1 d . . . O1A O 0.34680(15) 0.7838(2) 0.52500(10) 0.0161(5) Uani 1 1 d . . . N1A N 0.55524(17) 0.5917(3) 0.32455(11) 0.0140(5) Uani 1 1 d . . . H1NA H 0.6156 0.6267 0.3481 0.017 Uiso 1 1 d R . . C1A C 0.4892(2) 0.6835(3) 0.41001(14) 0.0133(6) Uani 1 1 d . . . C2A C 0.4027(2) 0.6906(3) 0.43342(14) 0.0129(7) Uani 1 1 d . . . C3A C 0.4197(2) 0.7672(3) 0.49071(14) 0.0130(7) Uani 1 1 d . . . C4A C 0.5087(2) 0.8337(3) 0.52220(13) 0.0157(7) Uani 1 1 d . . . H4AA H 0.5135 0.8870 0.5603 0.019 Uiso 1 1 calc R . . C5A C 0.5909(2) 0.8231(3) 0.49866(14) 0.0204(7) Uani 1 1 d . . . H5AA H 0.6532 0.8675 0.5205 0.024 Uiso 1 1 calc R . . C6A C 0.5810(2) 0.7462(3) 0.44235(14) 0.0180(7) Uani 1 1 d . . . H6AA H 0.6374 0.7363 0.4258 0.022 Uiso 1 1 calc R . . C7A C 0.1846(2) 0.9170(4) 0.44250(14) 0.0136(7) Uani 1 1 d . . . C8A C 0.1408(2) 0.8971(4) 0.37597(15) 0.0198(8) Uani 1 1 d . . . H8AA H 0.1321 0.8057 0.3584 0.024 Uiso 1 1 calc R . . C9A C 0.1097(3) 1.0120(4) 0.33478(17) 0.0250(8) Uani 1 1 d . . . H9AA H 0.0801 0.9989 0.2892 0.030 Uiso 1 1 calc R . . C10A C 0.1220(3) 1.1434(4) 0.36052(17) 0.0259(8) Uani 1 1 d . . . H10B H 0.1011 1.2214 0.3326 0.031 Uiso 1 1 calc R . . C11A C 0.1648(2) 1.1632(4) 0.42665(17) 0.0284(8) Uani 1 1 d . . . H11B H 0.1726 1.2547 0.4441 0.034 Uiso 1 1 calc R . . C12A C 0.1963(2) 1.0502(3) 0.46783(16) 0.0221(8) Uani 1 1 d . . . H12B H 0.2260 1.0643 0.5133 0.026 Uiso 1 1 calc R . . C13A C 0.1916(2) 0.8043(3) 0.56903(14) 0.0139(7) Uani 1 1 d . . . C14A C 0.0946(2) 0.8541(4) 0.56391(15) 0.0197(7) Uani 1 1 d . . . H14B H 0.0498 0.8777 0.5224 0.024 Uiso 1 1 calc R . . C15A C 0.0637(3) 0.8691(4) 0.61952(16) 0.0225(8) Uani 1 1 d . . . H15B H -0.0015 0.9059 0.6163 0.027 Uiso 1 1 calc R . . C16A C 0.1274(2) 0.8307(3) 0.67903(15) 0.0196(7) Uani 1 1 d . . . H16B H 0.1048 0.8376 0.7167 0.024 Uiso 1 1 calc R . . C17A C 0.2241(2) 0.7820(3) 0.68510(14) 0.0214(6) Uani 1 1 d . . . H17B H 0.2685 0.7590 0.7268 0.026 Uiso 1 1 calc R . . C18A C 0.2558(2) 0.7671(3) 0.62997(13) 0.0177(6) Uani 1 1 d . . . H18B H 0.3215 0.7315 0.6337 0.021 Uiso 1 1 calc R . . C19A C 0.4761(2) 0.6116(3) 0.34761(14) 0.0131(6) Uani 1 1 d . . . C20A C 0.5563(2) 0.5237(4) 0.26527(14) 0.0148(7) Uani 1 1 d . . . C21A C 0.5063(2) 0.3992(3) 0.24438(14) 0.0184(6) Uani 1 1 d . . . H21B H 0.4666 0.3567 0.2685 0.022 Uiso 1 1 calc R . . C22A C 0.5153(2) 0.3376(3) 0.18774(14) 0.0221(7) Uani 1 1 d . . . H22B H 0.4796 0.2541 0.1723 0.026 Uiso 1 1 calc R . . C23A C 0.5757(2) 0.3968(4) 0.15367(16) 0.0212(8) Uani 1 1 d . . . H23B H 0.5821 0.3534 0.1153 0.025 Uiso 1 1 calc R . . C24A C 0.6269(2) 0.5195(3) 0.17555(14) 0.0197(6) Uani 1 1 d . . . H24B H 0.6683 0.5602 0.1521 0.024 Uiso 1 1 calc R . . C25A C 0.61788(19) 0.5834(3) 0.23180(12) 0.0158(6) Uani 1 1 d . . . H25B H 0.6536 0.6670 0.2471 0.019 Uiso 1 1 calc R . . S1SA S 0.13989(5) 0.24931(8) 0.61917(4) 0.02126(16) Uani 1 1 d . . . O1SA O 0.24906(18) 0.2162(3) 0.62850(12) 0.0394(8) Uani 1 1 d . . . C1SA C 0.1317(2) 0.4337(3) 0.61986(15) 0.0336(8) Uani 1 1 d . . . H1SD H 0.1462 0.4714 0.5811 0.050 Uiso 1 1 calc R . . H1SE H 0.1813 0.4700 0.6592 0.050 Uiso 1 1 calc R . . H1SF H 0.0632 0.4612 0.6197 0.050 Uiso 1 1 calc R . . C2SA C 0.1182(2) 0.2152(3) 0.69548(16) 0.0241(8) Uani 1 1 d . . . H2SD H 0.1353 0.1182 0.7079 0.036 Uiso 1 1 calc R . . H2SE H 0.0466 0.2319 0.6918 0.036 Uiso 1 1 calc R . . H2SF H 0.1608 0.2768 0.7288 0.036 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 0.01262(11) 0.01126(12) 0.01090(11) 0.00005(10) 0.00333(9) -0.00087(10) Cl1 0.0175(4) 0.0191(4) 0.0147(4) -0.0015(3) 0.0031(3) -0.0055(3) P1 0.0144(4) 0.0134(4) 0.0106(4) 0.0010(3) 0.0042(3) 0.0005(4) S1 0.0182(4) 0.0145(4) 0.0151(4) -0.0020(4) 0.0074(3) -0.0039(4) S2 0.0159(4) 0.0193(5) 0.0144(4) -0.0042(3) 0.0051(3) -0.0032(3) O1 0.0157(11) 0.0171(11) 0.0090(10) 0.0009(9) 0.0043(9) 0.0008(10) N1 0.0156(12) 0.0225(16) 0.0121(13) -0.0022(11) 0.0039(10) -0.0005(11) C1 0.0144(14) 0.0118(15) 0.0117(15) 0.0015(11) 0.0031(12) 0.0027(12) C2 0.0109(14) 0.0111(15) 0.0120(15) 0.0017(12) 0.0017(12) 0.0009(12) C3 0.0097(14) 0.0132(16) 0.0152(16) 0.0018(13) 0.0029(12) 0.0027(13) C4 0.0172(15) 0.0154(16) 0.0128(16) -0.0027(12) 0.0030(12) 0.0022(12) C5 0.0147(14) 0.0181(15) 0.0181(16) -0.0038(12) 0.0021(12) -0.0042(12) C6 0.0124(14) 0.0205(16) 0.0199(17) -0.0026(13) 0.0047(12) 0.0004(12) C7 0.0160(15) 0.0151(18) 0.0141(16) 0.0043(14) 0.0087(13) 0.0025(14) C8 0.0135(14) 0.0197(18) 0.0141(15) 0.0000(13) 0.0056(12) -0.0016(13) C9 0.0186(17) 0.031(2) 0.0137(17) 0.0092(15) 0.0057(13) 0.0061(15) C10 0.0273(19) 0.0216(18) 0.0240(19) 0.0089(14) 0.0126(15) 0.0055(15) C11 0.0284(19) 0.0155(16) 0.0287(19) 0.0015(13) 0.0102(15) 0.0000(14) C12 0.0217(17) 0.0201(16) 0.0174(17) -0.0004(13) 0.0043(13) -0.0007(14) C13 0.0157(15) 0.0140(16) 0.0126(15) -0.0001(12) 0.0053(12) -0.0026(13) C14 0.0171(16) 0.0181(16) 0.0105(16) 0.0015(12) 0.0022(12) 0.0012(13) C15 0.0149(16) 0.0215(18) 0.0180(17) -0.0041(14) 0.0072(13) 0.0015(14) C16 0.0210(16) 0.0283(19) 0.0163(16) -0.0027(14) 0.0105(13) -0.0055(14) C17 0.0291(17) 0.0268(17) 0.0123(15) 0.0073(13) 0.0072(13) 0.0019(14) C18 0.0211(16) 0.0194(15) 0.0212(17) 0.0033(13) 0.0097(13) 0.0052(13) C19 0.0178(15) 0.0123(16) 0.0135(15) 0.0019(11) 0.0064(12) -0.0007(12) C20 0.0180(16) 0.0166(16) 0.0188(17) -0.0038(13) 0.0098(13) -0.0067(13) C21 0.0264(16) 0.0204(16) 0.0168(16) 0.0010(12) 0.0091(13) -0.0016(12) C22 0.0353(18) 0.0262(16) 0.0135(16) -0.0027(13) 0.0063(14) -0.0079(15) C23 0.0367(19) 0.0277(19) 0.0227(18) -0.0077(16) 0.0186(15) -0.0087(17) C24 0.0262(16) 0.0298(18) 0.0286(19) -0.0084(15) 0.0170(14) -0.0036(14) C25 0.0200(15) 0.0261(17) 0.0166(16) -0.0032(12) 0.0060(12) -0.0043(12) S1S 0.0172(4) 0.0218(4) 0.0219(4) -0.0025(3) 0.0055(3) 0.0005(3) O1S 0.0183(11) 0.0301(13) 0.0181(12) -0.0007(10) 0.0083(9) -0.0063(10) C1S 0.0189(16) 0.041(2) 0.0259(19) -0.0098(15) 0.0070(14) -0.0066(14) C2S 0.0325(19) 0.0238(18) 0.0224(18) 0.0038(14) 0.0164(15) -0.0017(15) Pd1A 0.01167(11) 0.01362(12) 0.01025(11) -0.00100(10) 0.00408(9) 0.00051(10) Cl1A 0.0148(4) 0.0224(4) 0.0140(4) -0.0026(3) 0.0051(3) -0.0039(3) P1A 0.0136(4) 0.0149(4) 0.0101(4) -0.0013(3) 0.0046(3) 0.0010(4) S1A 0.0231(4) 0.0154(4) 0.0169(4) -0.0024(4) 0.0112(3) -0.0023(4) S2A 0.0125(4) 0.0293(6) 0.0136(4) -0.0059(3) 0.0043(3) -0.0007(4) O1A 0.0136(11) 0.0250(13) 0.0102(11) -0.0034(10) 0.0044(9) 0.0041(10) N1A 0.0108(11) 0.0168(13) 0.0150(12) -0.0048(11) 0.0046(10) -0.0033(11) C1A 0.0182(15) 0.0095(14) 0.0127(15) -0.0002(11) 0.0052(12) 0.0007(12) C2A 0.0152(15) 0.0118(16) 0.0114(15) 0.0039(12) 0.0033(12) 0.0023(13) C3A 0.0152(15) 0.0142(17) 0.0112(15) 0.0026(13) 0.0063(12) 0.0034(13) C4A 0.0196(15) 0.0153(15) 0.0115(15) -0.0035(12) 0.0037(13) -0.0002(13) C5A 0.0183(15) 0.0239(17) 0.0189(17) -0.0055(13) 0.0053(13) -0.0085(13) C6A 0.0143(14) 0.0235(17) 0.0175(16) -0.0004(13) 0.0068(12) -0.0010(13) C7A 0.0120(15) 0.0157(19) 0.0143(16) 0.0022(14) 0.0055(12) 0.0020(14) C8A 0.0226(17) 0.0210(18) 0.0172(17) -0.0011(13) 0.0082(14) 0.0066(14) C9A 0.0296(19) 0.030(2) 0.0168(18) 0.0043(15) 0.0096(15) 0.0100(17) C10A 0.0274(18) 0.026(2) 0.027(2) 0.0145(15) 0.0125(16) 0.0090(15) C11A 0.034(2) 0.0158(16) 0.035(2) 0.0014(15) 0.0104(17) 0.0027(15) C12A 0.0265(18) 0.0227(17) 0.0153(17) -0.0022(13) 0.0035(14) -0.0001(14) C13A 0.0185(16) 0.0140(16) 0.0106(15) -0.0031(12) 0.0062(12) -0.0008(13) C14A 0.0208(16) 0.0236(17) 0.0149(16) 0.0014(13) 0.0055(13) 0.0010(14) C15A 0.0210(18) 0.026(2) 0.0238(19) -0.0010(16) 0.0123(15) 0.0013(16) C16A 0.0272(17) 0.0221(17) 0.0135(16) -0.0031(13) 0.0122(14) -0.0033(14) C17A 0.0306(17) 0.0216(16) 0.0111(15) 0.0035(12) 0.0048(13) 0.0001(14) C18A 0.0183(14) 0.0186(15) 0.0173(16) 0.0000(12) 0.0069(12) 0.0029(12) C19A 0.0129(14) 0.0117(15) 0.0137(15) 0.0038(12) 0.0025(11) 0.0007(12) C20A 0.0144(15) 0.0188(16) 0.0119(15) -0.0007(12) 0.0049(12) 0.0028(13) C21A 0.0179(14) 0.0171(14) 0.0230(17) -0.0017(12) 0.0101(13) 0.0002(11) C22A 0.0202(15) 0.0197(15) 0.0278(18) -0.0076(13) 0.0094(13) -0.0017(12) C23A 0.0215(16) 0.0259(19) 0.0175(17) -0.0063(13) 0.0076(14) 0.0053(14) C24A 0.0216(15) 0.0246(16) 0.0169(16) 0.0062(13) 0.0121(13) 0.0040(13) C25A 0.0154(13) 0.0154(14) 0.0157(14) -0.0003(12) 0.0033(11) 0.0002(12) S1SA 0.0197(4) 0.0263(4) 0.0189(4) -0.0008(3) 0.0074(3) 0.0043(3) O1SA 0.0265(13) 0.066(2) 0.0326(15) 0.0220(14) 0.0199(12) 0.0254(14) C1SA 0.047(2) 0.0255(16) 0.0338(19) 0.0081(17) 0.0213(17) 0.0026(18) C2SA 0.0260(17) 0.0225(18) 0.0304(19) 0.0039(14) 0.0186(15) 0.0007(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 Pd1 C2 2.018(3) . ? Pd1 S2 2.2584(8) . ? Pd1 S1 2.3519(8) . ? Pd1 Cl1 2.3773(8) . ? P1 O1 1.583(2) . ? P1 C13 1.786(3) . ? P1 C7 1.791(3) . ? P1 S1 1.9703(13) . ? S2 C19 1.693(3) . ? O1 C3 1.419(3) . ? N1 C19 1.326(4) . ? N1 C20 1.441(4) . ? N1 H1N 0.9194 . ? C1 C6 1.387(4) . ? C1 C2 1.431(4) . ? C1 C19 1.470(4) . ? C2 C3 1.396(4) . ? C3 C4 1.387(4) . ? C4 C5 1.379(4) . ? C4 H4A 0.9500 . ? C5 C6 1.382(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.387(4) . ? C7 C12 1.399(4) . ? C8 C9 1.379(4) . ? C8 H8A 0.9500 . ? C9 C10 1.388(5) . ? C9 H9A 0.9500 . ? C10 C11 1.380(4) . ? C10 H10A 0.9500 . ? C11 C12 1.379(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.395(4) . ? C13 C14 1.396(4) . ? C14 C15 1.385(4) . ? C14 H14A 0.9500 . ? C15 C16 1.382(4) . ? C15 H15A 0.9500 . ? C16 C17 1.385(4) . ? C16 H16A 0.9500 . ? C17 C18 1.382(4) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C20 C25 1.376(4) . ? C20 C21 1.390(4) . ? C21 C22 1.394(4) . ? C21 H21A 0.9500 . ? C22 C23 1.387(4) . ? C22 H22A 0.9500 . ? C23 C24 1.376(4) . ? C23 H23A 0.9500 . ? C24 C25 1.388(4) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? S1S O1S 1.509(2) . ? S1S C2S 1.779(3) . ? S1S C1S 1.782(3) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? Pd1A C2A 2.020(3) . ? Pd1A S2A 2.2545(8) . ? Pd1A S1A 2.3641(8) . ? Pd1A Cl1A 2.3934(8) . ? P1A O1A 1.585(2) . ? P1A C13A 1.781(3) . ? P1A C7A 1.787(3) . ? P1A S1A 1.9664(13) . ? S2A C19A 1.695(3) . ? O1A C3A 1.418(3) . ? N1A C19A 1.338(3) . ? N1A C20A 1.434(4) . ? N1A H1NA 0.9014 . ? C1A C6A 1.390(4) . ? C1A C2A 1.425(4) . ? C1A C19A 1.470(4) . ? C2A C3A 1.392(4) . ? C3A C4A 1.373(4) . ? C4A C5A 1.374(4) . ? C4A H4AA 0.9500 . ? C5A C6A 1.388(4) . ? C5A H5AA 0.9500 . ? C6A H6AA 0.9500 . ? C7A C12A 1.382(4) . ? C7A C8A 1.389(4) . ? C8A C9A 1.401(5) . ? C8A H8AA 0.9500 . ? C9A C10A 1.370(5) . ? C9A H9AA 0.9500 . ? C10A C11A 1.379(5) . ? C10A H10B 0.9500 . ? C11A C12A 1.387(4) . ? C11A H11B 0.9500 . ? C12A H12B 0.9500 . ? C13A C18A 1.392(4) . ? C13A C14A 1.394(4) . ? C14A C15A 1.387(4) . ? C14A H14B 0.9500 . ? C15A C16A 1.370(4) . ? C15A H15B 0.9500 . ? C16A C17A 1.383(4) . ? C16A H16B 0.9500 . ? C17A C18A 1.383(4) . ? C17A H17B 0.9500 . ? C18A H18B 0.9500 . ? C20A C25A 1.387(4) . ? C20A C21A 1.389(4) . ? C21A C22A 1.389(4) . ? C21A H21B 0.9500 . ? C22A C23A 1.382(4) . ? C22A H22B 0.9500 . ? C23A C24A 1.384(4) . ? C23A H23B 0.9500 . ? C24A C25A 1.391(4) . ? C24A H24B 0.9500 . ? C25A H25B 0.9500 . ? S1SA O1SA 1.493(2) . ? S1SA C1SA 1.778(3) . ? S1SA C2SA 1.778(3) . ? C1SA H1SD 0.9800 . ? C1SA H1SE 0.9800 . ? C1SA H1SF 0.9800 . ? C2SA H2SD 0.9800 . ? C2SA H2SE 0.9800 . ? C2SA H2SF 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 S2 85.78(9) . . ? C2 Pd1 S1 101.42(8) . . ? S2 Pd1 S1 170.02(3) . . ? C2 Pd1 Cl1 170.26(9) . . ? S2 Pd1 Cl1 87.42(3) . . ? S1 Pd1 Cl1 86.22(3) . . ? O1 P1 C13 102.26(13) . . ? O1 P1 C7 106.99(13) . . ? C13 P1 C7 110.81(15) . . ? O1 P1 S1 112.24(10) . . ? C13 P1 S1 110.28(11) . . ? C7 P1 S1 113.65(11) . . ? P1 S1 Pd1 97.40(4) . . ? C19 S2 Pd1 101.10(11) . . ? C3 O1 P1 122.70(18) . . ? C19 N1 C20 128.5(3) . . ? C19 N1 H1N 119.8 . . ? C20 N1 H1N 110.1 . . ? C6 C1 C2 123.1(3) . . ? C6 C1 C19 120.7(3) . . ? C2 C1 C19 116.2(3) . . ? C3 C2 C1 112.6(3) . . ? C3 C2 Pd1 128.8(2) . . ? C1 C2 Pd1 118.0(2) . . ? C4 C3 C2 124.9(3) . . ? C4 C3 O1 112.1(3) . . ? C2 C3 O1 123.0(3) . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 118.4(3) . . ? C4 C5 H5A 120.8 . . ? C6 C5 H5A 120.8 . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? C8 C7 C12 120.1(3) . . ? C8 C7 P1 121.4(3) . . ? C12 C7 P1 118.5(2) . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 119.8(3) . . ? C11 C12 H12A 120.1 . . ? C7 C12 H12A 120.1 . . ? C18 C13 C14 120.3(3) . . ? C18 C13 P1 118.0(2) . . ? C14 C13 P1 121.4(2) . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C18 C17 C16 120.1(3) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C13 119.5(3) . . ? C17 C18 H18A 120.2 . . ? C13 C18 H18A 120.2 . . ? N1 C19 C1 118.9(3) . . ? N1 C19 S2 123.2(2) . . ? C1 C19 S2 117.9(2) . . ? C25 C20 C21 121.1(3) . . ? C25 C20 N1 116.7(3) . . ? C21 C20 N1 122.0(3) . . ? C20 C21 C22 118.6(3) . . ? C20 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C20 C25 C24 119.9(3) . . ? C20 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? O1S S1S C2S 106.72(15) . . ? O1S S1S C1S 105.07(14) . . ? C2S S1S C1S 98.28(15) . . ? S1S C1S H1SA 109.5 . . ? S1S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? S1S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? S1S C2S H2SA 109.5 . . ? S1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? S1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C2A Pd1A S2A 85.41(9) . . ? C2A Pd1A S1A 100.54(9) . . ? S2A Pd1A S1A 169.68(4) . . ? C2A Pd1A Cl1A 172.40(9) . . ? S2A Pd1A Cl1A 88.28(3) . . ? S1A Pd1A Cl1A 86.33(3) . . ? O1A P1A C13A 100.33(13) . . ? O1A P1A C7A 107.92(14) . . ? C13A P1A C7A 108.58(15) . . ? O1A P1A S1A 112.63(10) . . ? C13A P1A S1A 112.54(11) . . ? C7A P1A S1A 113.91(11) . . ? P1A S1A Pd1A 96.34(4) . . ? C19A S2A Pd1A 101.40(11) . . ? C3A O1A P1A 127.74(19) . . ? C19A N1A C20A 128.0(3) . . ? C19A N1A H1NA 117.3 . . ? C20A N1A H1NA 114.7 . . ? C6A C1A C2A 122.5(3) . . ? C6A C1A C19A 120.5(3) . . ? C2A C1A C19A 116.9(3) . . ? C3A C2A C1A 113.3(3) . . ? C3A C2A Pd1A 128.6(2) . . ? C1A C2A Pd1A 118.0(2) . . ? C4A C3A C2A 125.1(3) . . ? C4A C3A O1A 111.1(3) . . ? C2A C3A O1A 123.8(3) . . ? C3A C4A C5A 120.0(3) . . ? C3A C4A H4AA 120.0 . . ? C5A C4A H4AA 120.0 . . ? C4A C5A C6A 118.6(3) . . ? C4A C5A H5AA 120.7 . . ? C6A C5A H5AA 120.7 . . ? C5A C6A C1A 120.5(3) . . ? C5A C6A H6AA 119.8 . . ? C1A C6A H6AA 119.8 . . ? C12A C7A C8A 119.8(3) . . ? C12A C7A P1A 118.7(2) . . ? C8A C7A P1A 121.5(3) . . ? C7A C8A C9A 119.9(3) . . ? C7A C8A H8AA 120.1 . . ? C9A C8A H8AA 120.1 . . ? C10A C9A C8A 119.7(3) . . ? C10A C9A H9AA 120.2 . . ? C8A C9A H9AA 120.2 . . ? C9A C10A C11A 120.4(3) . . ? C9A C10A H10B 119.8 . . ? C11A C10A H10B 119.8 . . ? C10A C11A C12A 120.4(3) . . ? C10A C11A H11B 119.8 . . ? C12A C11A H11B 119.8 . . ? C7A C12A C11A 119.8(3) . . ? C7A C12A H12B 120.1 . . ? C11A C12A H12B 120.1 . . ? C18A C13A C14A 119.5(3) . . ? C18A C13A P1A 120.9(2) . . ? C14A C13A P1A 119.4(2) . . ? C15A C14A C13A 119.9(3) . . ? C15A C14A H14B 120.0 . . ? C13A C14A H14B 120.0 . . ? C16A C15A C14A 119.9(3) . . ? C16A C15A H15B 120.1 . . ? C14A C15A H15B 120.1 . . ? C15A C16A C17A 121.0(3) . . ? C15A C16A H16B 119.5 . . ? C17A C16A H16B 119.5 . . ? C16A C17A C18A 119.5(3) . . ? C16A C17A H17B 120.2 . . ? C18A C17A H17B 120.2 . . ? C17A C18A C13A 120.1(3) . . ? C17A C18A H18B 119.9 . . ? C13A C18A H18B 119.9 . . ? N1A C19A C1A 120.6(3) . . ? N1A C19A S2A 122.1(2) . . ? C1A C19A S2A 117.3(2) . . ? C25A C20A C21A 120.8(3) . . ? C25A C20A N1A 115.9(3) . . ? C21A C20A N1A 123.1(3) . . ? C22A C21A C20A 119.1(3) . . ? C22A C21A H21B 120.5 . . ? C20A C21A H21B 120.5 . . ? C23A C22A C21A 120.6(3) . . ? C23A C22A H22B 119.7 . . ? C21A C22A H22B 119.7 . . ? C22A C23A C24A 119.9(3) . . ? C22A C23A H23B 120.1 . . ? C24A C23A H23B 120.1 . . ? C23A C24A C25A 120.3(3) . . ? C23A C24A H24B 119.9 . . ? C25A C24A H24B 119.9 . . ? C20A C25A C24A 119.3(3) . . ? C20A C25A H25B 120.3 . . ? C24A C25A H25B 120.3 . . ? O1SA S1SA C1SA 105.97(17) . . ? O1SA S1SA C2SA 105.86(14) . . ? C1SA S1SA C2SA 98.52(15) . . ? S1SA C1SA H1SD 109.5 . . ? S1SA C1SA H1SE 109.5 . . ? H1SD C1SA H1SE 109.5 . . ? S1SA C1SA H1SF 109.5 . . ? H1SD C1SA H1SF 109.5 . . ? H1SE C1SA H1SF 109.5 . . ? S1SA C2SA H2SD 109.5 . . ? S1SA C2SA H2SE 109.5 . . ? H2SD C2SA H2SE 109.5 . . ? S1SA C2SA H2SF 109.5 . . ? H2SD C2SA H2SF 109.5 . . ? H2SE C2SA H2SF 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 S1 Pd1 56.36(9) . . . . ? C13 P1 S1 Pd1 169.67(11) . . . . ? C7 P1 S1 Pd1 -65.22(11) . . . . ? C2 Pd1 S1 P1 -29.92(10) . . . . ? Cl1 Pd1 S1 P1 143.98(4) . . . . ? C2 Pd1 S2 C19 -3.03(14) . . . . ? Cl1 Pd1 S2 C19 -176.06(11) . . . . ? C13 P1 O1 C3 171.1(2) . . . . ? C7 P1 O1 C3 54.6(3) . . . . ? S1 P1 O1 C3 -70.8(2) . . . . ? C6 C1 C2 C3 4.3(4) . . . . ? C19 C1 C2 C3 -178.2(3) . . . . ? C6 C1 C2 Pd1 -168.4(2) . . . . ? C19 C1 C2 Pd1 9.1(4) . . . . ? S2 Pd1 C2 C3 -174.1(3) . . . . ? S1 Pd1 C2 C3 12.8(3) . . . . ? S2 Pd1 C2 C1 -2.8(2) . . . . ? S1 Pd1 C2 C1 -175.9(2) . . . . ? C1 C2 C3 C4 -4.4(5) . . . . ? Pd1 C2 C3 C4 167.3(2) . . . . ? C1 C2 C3 O1 174.8(3) . . . . ? Pd1 C2 C3 O1 -13.5(5) . . . . ? P1 O1 C3 C4 -138.0(2) . . . . ? P1 O1 C3 C2 42.7(4) . . . . ? C2 C3 C4 C5 1.7(5) . . . . ? O1 C3 C4 C5 -177.6(3) . . . . ? C3 C4 C5 C6 1.5(4) . . . . ? C4 C5 C6 C1 -1.5(4) . . . . ? C2 C1 C6 C5 -1.6(5) . . . . ? C19 C1 C6 C5 -179.0(3) . . . . ? O1 P1 C7 C8 -128.8(3) . . . . ? C13 P1 C7 C8 120.4(3) . . . . ? S1 P1 C7 C8 -4.4(3) . . . . ? O1 P1 C7 C12 51.2(3) . . . . ? C13 P1 C7 C12 -59.5(3) . . . . ? S1 P1 C7 C12 175.7(2) . . . . ? C12 C7 C8 C9 0.6(5) . . . . ? P1 C7 C8 C9 -179.3(2) . . . . ? C7 C8 C9 C10 -1.0(5) . . . . ? C8 C9 C10 C11 0.6(5) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C10 C11 C12 C7 -0.7(5) . . . . ? C8 C7 C12 C11 0.3(5) . . . . ? P1 C7 C12 C11 -179.8(2) . . . . ? O1 P1 C13 C18 52.5(3) . . . . ? C7 P1 C13 C18 166.3(2) . . . . ? S1 P1 C13 C18 -67.0(3) . . . . ? O1 P1 C13 C14 -134.1(3) . . . . ? C7 P1 C13 C14 -20.4(3) . . . . ? S1 P1 C13 C14 106.3(3) . . . . ? C18 C13 C14 C15 1.0(5) . . . . ? P1 C13 C14 C15 -172.2(2) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? C14 C15 C16 C17 -0.9(5) . . . . ? C15 C16 C17 C18 1.2(5) . . . . ? C16 C17 C18 C13 -0.4(5) . . . . ? C14 C13 C18 C17 -0.7(5) . . . . ? P1 C13 C18 C17 172.8(2) . . . . ? C20 N1 C19 C1 178.1(3) . . . . ? C20 N1 C19 S2 -3.5(5) . . . . ? C6 C1 C19 N1 -16.2(4) . . . . ? C2 C1 C19 N1 166.3(3) . . . . ? C6 C1 C19 S2 165.3(2) . . . . ? C2 C1 C19 S2 -12.2(4) . . . . ? Pd1 S2 C19 N1 -169.6(3) . . . . ? Pd1 S2 C19 C1 8.8(2) . . . . ? C19 N1 C20 C25 143.0(3) . . . . ? C19 N1 C20 C21 -42.2(5) . . . . ? C25 C20 C21 C22 -1.3(4) . . . . ? N1 C20 C21 C22 -175.8(3) . . . . ? C20 C21 C22 C23 2.0(4) . . . . ? C21 C22 C23 C24 -1.9(5) . . . . ? C22 C23 C24 C25 1.1(5) . . . . ? C21 C20 C25 C24 0.6(5) . . . . ? N1 C20 C25 C24 175.4(3) . . . . ? C23 C24 C25 C20 -0.4(5) . . . . ? O1A P1A S1A Pd1A -57.58(10) . . . . ? C13A P1A S1A Pd1A -170.12(11) . . . . ? C7A P1A S1A Pd1A 65.74(11) . . . . ? C2A Pd1A S1A P1A 37.14(10) . . . . ? S2A Pd1A S1A P1A 161.71(16) . . . . ? Cl1A Pd1A S1A P1A -139.59(4) . . . . ? C2A Pd1A S2A C19A 8.13(15) . . . . ? S1A Pd1A S2A C19A -117.6(2) . . . . ? Cl1A Pd1A S2A C19A -176.11(12) . . . . ? C13A P1A O1A C3A 179.3(3) . . . . ? C7A P1A O1A C3A -67.1(3) . . . . ? S1A P1A O1A C3A 59.5(3) . . . . ? C6A C1A C2A C3A 0.8(4) . . . . ? C19A C1A C2A C3A -176.5(3) . . . . ? C6A C1A C2A Pd1A 179.2(2) . . . . ? C19A C1A C2A Pd1A 1.9(4) . . . . ? S2A Pd1A C2A C3A 171.6(3) . . . . ? S1A Pd1A C2A C3A -16.9(3) . . . . ? S2A Pd1A C2A C1A -6.5(2) . . . . ? S1A Pd1A C2A C1A 165.0(2) . . . . ? C1A C2A C3A C4A 1.5(5) . . . . ? Pd1A C2A C3A C4A -176.7(2) . . . . ? C1A C2A C3A O1A -177.0(3) . . . . ? Pd1A C2A C3A O1A 4.8(5) . . . . ? P1A O1A C3A C4A 156.3(2) . . . . ? P1A O1A C3A C2A -25.0(4) . . . . ? C2A C3A C4A C5A -2.5(5) . . . . ? O1A C3A C4A C5A 176.2(3) . . . . ? C3A C4A C5A C6A 1.0(5) . . . . ? C4A C5A C6A C1A 1.1(5) . . . . ? C2A C1A C6A C5A -2.1(5) . . . . ? C19A C1A C6A C5A 175.1(3) . . . . ? O1A P1A C7A C12A -65.8(3) . . . . ? C13A P1A C7A C12A 42.1(3) . . . . ? S1A P1A C7A C12A 168.4(2) . . . . ? O1A P1A C7A C8A 113.9(3) . . . . ? C13A P1A C7A C8A -138.2(3) . . . . ? S1A P1A C7A C8A -12.0(3) . . . . ? C12A C7A C8A C9A 0.5(5) . . . . ? P1A C7A C8A C9A -179.1(2) . . . . ? C7A C8A C9A C10A -0.3(5) . . . . ? C8A C9A C10A C11A -0.1(5) . . . . ? C9A C10A C11A C12A 0.4(5) . . . . ? C8A C7A C12A C11A -0.2(5) . . . . ? P1A C7A C12A C11A 179.4(2) . . . . ? C10A C11A C12A C7A -0.3(5) . . . . ? O1A P1A C13A C18A -29.0(3) . . . . ? C7A P1A C13A C18A -142.1(3) . . . . ? S1A P1A C13A C18A 90.9(3) . . . . ? O1A P1A C13A C14A 156.9(3) . . . . ? C7A P1A C13A C14A 43.8(3) . . . . ? S1A P1A C13A C14A -83.2(3) . . . . ? C18A C13A C14A C15A 1.4(5) . . . . ? P1A C13A C14A C15A 175.6(3) . . . . ? C13A C14A C15A C16A -2.1(5) . . . . ? C14A C15A C16A C17A 2.6(5) . . . . ? C15A C16A C17A C18A -2.3(5) . . . . ? C16A C17A C18A C13A 1.6(4) . . . . ? C14A C13A C18A C17A -1.2(5) . . . . ? P1A C13A C18A C17A -175.3(2) . . . . ? C20A N1A C19A C1A 179.7(3) . . . . ? C20A N1A C19A S2A -1.9(5) . . . . ? C6A C1A C19A N1A 7.5(5) . . . . ? C2A C1A C19A N1A -175.2(3) . . . . ? C6A C1A C19A S2A -171.0(2) . . . . ? C2A C1A C19A S2A 6.3(4) . . . . ? Pd1A S2A C19A N1A 171.6(3) . . . . ? Pd1A S2A C19A C1A -9.9(3) . . . . ? C19A N1A C20A C25A 141.3(3) . . . . ? C19A N1A C20A C21A -44.0(5) . . . . ? C25A C20A C21A C22A -2.7(4) . . . . ? N1A C20A C21A C22A -177.2(3) . . . . ? C20A C21A C22A C23A 2.1(4) . . . . ? C21A C22A C23A C24A -0.8(5) . . . . ? C22A C23A C24A C25A 0.1(4) . . . . ? C21A C20A C25A C24A 2.0(4) . . . . ? N1A C20A C25A C24A 176.9(3) . . . . ? C23A C24A C25A C20A -0.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1N O1S 1_555 0.92 1.88 2.775(4) 163 ? N1A H1NA O1SA 2_656 0.90 1.98 2.851(4) 162 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.618 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.072 data_9b _database_code_depnum_ccdc_archive 'CCDC 791558' #TrackingRef '- 9b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H19 Cl N O P Pt S2, C2 H6 O S' _chemical_formula_sum 'C27 H25 Cl N O2 P Pt S3' _chemical_formula_weight 753.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.7922(9) _cell_length_b 9.6927(6) _cell_length_c 21.3471(13) _cell_angle_alpha 90.00 _cell_angle_beta 107.3340(10) _cell_angle_gamma 90.00 _cell_volume 2724.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2015 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 5.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.206 _exptl_absorpt_correction_T_max 0.236 _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30297 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 28.00 _reflns_number_total 13054 _reflns_number_gt 12337 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0176P)^2^+0.4972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.426(4) _refine_ls_number_reflns 13054 _refine_ls_number_parameters 654 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.269634(12) 0.552753(13) 0.374116(7) 0.01236(5) Uani 1 1 d . . . Cl1 Cl 0.12444(9) 0.65384(14) 0.29794(5) 0.0190(3) Uani 1 1 d . . . P1 P 0.22446(9) 0.37953(15) 0.49317(6) 0.0140(3) Uani 1 1 d . . . S1 S 0.17180(9) 0.5529(2) 0.44668(5) 0.0169(2) Uani 1 1 d . . . S2 S 0.35452(10) 0.59072(14) 0.30028(6) 0.0174(3) Uani 1 1 d . . . N1 N 0.5485(3) 0.5301(5) 0.31748(18) 0.0175(10) Uani 1 1 d . . . H1N H 0.6166 0.5183 0.3471 0.021 Uiso 1 1 d R . . O1 O 0.3449(2) 0.3827(4) 0.52358(15) 0.0161(7) Uani 1 1 d . . . C1 C 0.4769(3) 0.4383(5) 0.3979(2) 0.0141(10) Uani 1 1 d . . . C2 C 0.3944(4) 0.4518(6) 0.4257(2) 0.0161(10) Uani 1 1 d . . . C3 C 0.4110(3) 0.3746(6) 0.4843(2) 0.0155(10) Uani 1 1 d . . . C4 C 0.4927(4) 0.2884(5) 0.5106(2) 0.0170(10) Uani 1 1 d . . . H4A H 0.4979 0.2389 0.5499 0.020 Uiso 1 1 calc R . . C5 C 0.5669(4) 0.2744(5) 0.4796(2) 0.0214(10) Uani 1 1 d . . . H5A H 0.6221 0.2128 0.4964 0.026 Uiso 1 1 calc R . . C6 C 0.5601(3) 0.3504(5) 0.4240(2) 0.0211(10) Uani 1 1 d . . . H6A H 0.6119 0.3434 0.4031 0.025 Uiso 1 1 calc R . . C7 C 0.1928(3) 0.2291(6) 0.4427(2) 0.0134(10) Uani 1 1 d . . . C8 C 0.1285(3) 0.2373(6) 0.3792(2) 0.0162(10) Uani 1 1 d . . . H8A H 0.1008 0.3234 0.3613 0.019 Uiso 1 1 calc R . . C9 C 0.1050(4) 0.1161(6) 0.3418(2) 0.0202(11) Uani 1 1 d . . . H9A H 0.0604 0.1202 0.2983 0.024 Uiso 1 1 calc R . . C10 C 0.1459(4) -0.0091(6) 0.3675(3) 0.0248(12) Uani 1 1 d . . . H10A H 0.1300 -0.0903 0.3415 0.030 Uiso 1 1 calc R . . C11 C 0.2103(4) -0.0161(6) 0.4315(3) 0.0271(12) Uani 1 1 d . . . H11A H 0.2384 -0.1023 0.4491 0.033 Uiso 1 1 calc R . . C12 C 0.2336(4) 0.1010(5) 0.4693(2) 0.0204(11) Uani 1 1 d . . . H12A H 0.2769 0.0957 0.5131 0.024 Uiso 1 1 calc R . . C13 C 0.1830(3) 0.3638(5) 0.5645(2) 0.0140(10) Uani 1 1 d . . . C14 C 0.1084(4) 0.2681(6) 0.5671(3) 0.0196(11) Uani 1 1 d . . . H14A H 0.0844 0.2031 0.5327 0.023 Uiso 1 1 calc R . . C15 C 0.0693(4) 0.2682(6) 0.6202(2) 0.0201(11) Uani 1 1 d . . . H15A H 0.0184 0.2037 0.6220 0.024 Uiso 1 1 calc R . . C16 C 0.1056(4) 0.3633(5) 0.6704(2) 0.0226(11) Uani 1 1 d . . . H16A H 0.0788 0.3647 0.7066 0.027 Uiso 1 1 calc R . . C17 C 0.1815(4) 0.4573(5) 0.6678(2) 0.0258(11) Uani 1 1 d . . . H17A H 0.2067 0.5214 0.7026 0.031 Uiso 1 1 calc R . . C18 C 0.2195(4) 0.4571(6) 0.6156(2) 0.0233(11) Uani 1 1 d . . . H18A H 0.2710 0.5210 0.6141 0.028 Uiso 1 1 calc R . . C19 C 0.4679(4) 0.5169(5) 0.3383(2) 0.0154(11) Uani 1 1 d . . . C20 C 0.5569(4) 0.6000(6) 0.2598(2) 0.0178(11) Uani 1 1 d . . . C21 C 0.4823(4) 0.5891(5) 0.1995(2) 0.0249(10) Uani 1 1 d . . . H21A H 0.4214 0.5393 0.1957 0.030 Uiso 1 1 calc R . . C22 C 0.4983(4) 0.6525(5) 0.1448(2) 0.0283(11) Uani 1 1 d . . . H22A H 0.4480 0.6463 0.1034 0.034 Uiso 1 1 calc R . . C23 C 0.5874(4) 0.7245(7) 0.1507(2) 0.0303(13) Uani 1 1 d . . . H23A H 0.5982 0.7657 0.1129 0.036 Uiso 1 1 calc R . . C24 C 0.6603(4) 0.7371(5) 0.2106(2) 0.0281(11) Uani 1 1 d . . . H24A H 0.7204 0.7884 0.2143 0.034 Uiso 1 1 calc R . . C25 C 0.6456(4) 0.6742(5) 0.2657(2) 0.0229(10) Uani 1 1 d . . . H25A H 0.6958 0.6820 0.3072 0.027 Uiso 1 1 calc R . . Pt1A Pt 0.725712(12) 0.212576(13) 0.119846(7) 0.01212(5) Uani 1 1 d . . . Cl1A Cl 0.87336(9) 0.11160(14) 0.19431(5) 0.0176(3) Uani 1 1 d . . . P1A P 0.77233(9) 0.39305(15) 0.00410(6) 0.0137(3) Uani 1 1 d . . . S1A S 0.81984(9) 0.2126(2) 0.04482(5) 0.0179(2) Uani 1 1 d . . . S2A S 0.64213(10) 0.17282(15) 0.19396(6) 0.0189(4) Uani 1 1 d . . . N1A N 0.4447(3) 0.2087(6) 0.17637(17) 0.0150(8) Uani 1 1 d . . . H1NA H 0.3822 0.2414 0.1521 0.018 Uiso 1 1 d R . . O1A O 0.6530(2) 0.3997(4) -0.02451(15) 0.0179(8) Uani 1 1 d . . . C1A C 0.5106(4) 0.2991(5) 0.0905(2) 0.0161(10) Uani 1 1 d . . . C2A C 0.5972(4) 0.3074(5) 0.0670(2) 0.0133(10) Uani 1 1 d . . . C3A C 0.5807(4) 0.3831(6) 0.0098(2) 0.0153(10) Uani 1 1 d . . . C4A C 0.4912(4) 0.4516(6) -0.0212(2) 0.0190(11) Uani 1 1 d . . . H4AA H 0.4863 0.5057 -0.0591 0.023 Uiso 1 1 calc R . . C5A C 0.4102(4) 0.4416(5) 0.0025(2) 0.0223(11) Uani 1 1 d . . . H5AA H 0.3482 0.4870 -0.0190 0.027 Uiso 1 1 calc R . . C6A C 0.4195(3) 0.3643(5) 0.0584(2) 0.0205(10) Uani 1 1 d . . . H6AA H 0.3631 0.3557 0.0751 0.025 Uiso 1 1 calc R . . C7A C 0.8148(4) 0.5361(7) 0.0580(2) 0.0178(11) Uani 1 1 d . . . C8A C 0.8578(4) 0.5187(6) 0.1251(2) 0.0224(12) Uani 1 1 d . . . H8AA H 0.8653 0.4286 0.1434 0.027 Uiso 1 1 calc R . . C9A C 0.8897(4) 0.6314(7) 0.1653(3) 0.0296(14) Uani 1 1 d . . . H9AA H 0.9205 0.6191 0.2110 0.036 Uiso 1 1 calc R . . C10A C 0.8765(5) 0.7623(7) 0.1385(3) 0.0302(14) Uani 1 1 d . . . H10B H 0.8979 0.8401 0.1663 0.036 Uiso 1 1 calc R . . C11A C 0.8328(4) 0.7818(6) 0.0720(3) 0.0320(13) Uani 1 1 d . . . H11B H 0.8238 0.8724 0.0542 0.038 Uiso 1 1 calc R . . C12A C 0.8020(4) 0.6680(6) 0.0312(3) 0.0273(13) Uani 1 1 d . . . H12B H 0.7724 0.6804 -0.0147 0.033 Uiso 1 1 calc R . . C13A C 0.8096(4) 0.4225(6) -0.0682(2) 0.0176(11) Uani 1 1 d . . . C14A C 0.9060(4) 0.4718(6) -0.0631(2) 0.0218(12) Uani 1 1 d . . . H14B H 0.9508 0.4971 -0.0216 0.026 Uiso 1 1 calc R . . C15A C 0.9364(4) 0.4837(6) -0.1187(3) 0.0247(12) Uani 1 1 d . . . H15B H 1.0024 0.5179 -0.1150 0.030 Uiso 1 1 calc R . . C16A C 0.8740(4) 0.4477(5) -0.1786(2) 0.0221(11) Uani 1 1 d . . . H16B H 0.8969 0.4561 -0.2162 0.026 Uiso 1 1 calc R . . C17A C 0.7770(4) 0.3985(5) -0.1852(2) 0.0245(10) Uani 1 1 d . . . H17B H 0.7335 0.3742 -0.2273 0.029 Uiso 1 1 calc R . . C18A C 0.7431(3) 0.3848(5) -0.1299(2) 0.0193(9) Uani 1 1 d . . . H18B H 0.6769 0.3509 -0.1339 0.023 Uiso 1 1 calc R . . C19A C 0.5225(3) 0.2273(6) 0.1527(2) 0.0150(9) Uani 1 1 d . . . C20A C 0.4431(4) 0.1392(6) 0.2350(2) 0.0155(10) Uani 1 1 d . . . C21A C 0.4936(3) 0.0161(5) 0.2558(2) 0.0225(10) Uani 1 1 d . . . H21B H 0.5343 -0.0253 0.2321 0.027 Uiso 1 1 calc R . . C22A C 0.4832(4) -0.0449(5) 0.3121(2) 0.0238(10) Uani 1 1 d . . . H22B H 0.5176 -0.1292 0.3268 0.029 Uiso 1 1 calc R . . C23A C 0.4245(4) 0.0126(6) 0.3474(2) 0.0226(12) Uani 1 1 d . . . H23B H 0.4195 -0.0307 0.3862 0.027 Uiso 1 1 calc R . . C24A C 0.3726(4) 0.1347(5) 0.3254(2) 0.0226(10) Uani 1 1 d . . . H24B H 0.3302 0.1737 0.3485 0.027 Uiso 1 1 calc R . . C25A C 0.3827(3) 0.1997(5) 0.2697(2) 0.0181(9) Uani 1 1 d . . . H25B H 0.3489 0.2846 0.2553 0.022 Uiso 1 1 calc R . . S1S S 0.20483(9) 0.84030(13) 0.64244(6) 0.0232(2) Uani 1 1 d . . . O1S O 0.2499(3) 0.9640(5) 0.61908(17) 0.0241(8) Uani 1 1 d . . . C1S C 0.0949(4) 0.8004(6) 0.5761(3) 0.0315(12) Uani 1 1 d . . . H1SA H 0.1154 0.7748 0.5375 0.047 Uiso 1 1 calc R . . H1SB H 0.0503 0.8813 0.5658 0.047 Uiso 1 1 calc R . . H1SC H 0.0585 0.7233 0.5885 0.047 Uiso 1 1 calc R . . C2S C 0.1442(4) 0.9019(6) 0.6995(2) 0.0270(12) Uani 1 1 d . . . H2SA H 0.1948 0.9442 0.7369 0.041 Uiso 1 1 calc R . . H2SB H 0.1114 0.8247 0.7149 0.041 Uiso 1 1 calc R . . H2SC H 0.0929 0.9707 0.6782 0.041 Uiso 1 1 calc R . . S1SA S 0.86048(9) 0.86639(13) 0.88071(6) 0.0224(2) Uani 1 1 d . . . O1SA O 0.7510(3) 0.8316(6) 0.8710(2) 0.0473(15) Uani 1 1 d . . . C1SA C 0.8675(4) 1.0499(6) 0.8794(3) 0.0366(12) Uani 1 1 d . . . H1SD H 0.8526 1.0877 0.9181 0.055 Uiso 1 1 calc R . . H1SE H 0.8179 1.0851 0.8396 0.055 Uiso 1 1 calc R . . H1SF H 0.9360 1.0779 0.8798 0.055 Uiso 1 1 calc R . . C2SA C 0.8820(4) 0.8330(6) 0.8037(3) 0.0264(12) Uani 1 1 d . . . H2SD H 0.8645 0.7370 0.7909 0.040 Uiso 1 1 calc R . . H2SE H 0.9537 0.8491 0.8076 0.040 Uiso 1 1 calc R . . H2SF H 0.8395 0.8947 0.7702 0.040 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 Pt1 0.01200(9) 0.01381(10) 0.01092(8) -0.00037(7) 0.00286(6) 0.00079(7) Cl1 0.0181(6) 0.0235(7) 0.0141(5) 0.0013(4) 0.0029(4) 0.0055(5) P1 0.0126(6) 0.0182(7) 0.0113(5) -0.0019(5) 0.0036(4) -0.0006(5) S1 0.0183(6) 0.0180(6) 0.0161(5) 0.0006(6) 0.0076(4) 0.0021(7) S2 0.0162(6) 0.0201(9) 0.0157(6) 0.0043(4) 0.0045(4) 0.0042(5) N1 0.018(2) 0.022(3) 0.0126(17) 0.0018(16) 0.0041(14) 0.0008(17) O1 0.0150(17) 0.0215(19) 0.0105(15) -0.0024(13) 0.0020(12) -0.0001(15) C1 0.010(2) 0.017(2) 0.014(2) -0.0003(17) 0.0021(16) -0.0021(17) C2 0.021(3) 0.015(3) 0.011(2) 0.0002(18) 0.0032(18) 0.000(2) C3 0.009(2) 0.025(3) 0.014(2) -0.002(2) 0.0048(16) -0.005(2) C4 0.019(2) 0.018(3) 0.013(2) 0.0057(18) 0.0033(17) -0.0030(18) C5 0.018(2) 0.024(3) 0.022(2) 0.008(2) 0.0051(19) 0.0080(19) C6 0.014(2) 0.026(3) 0.024(3) 0.001(2) 0.0071(18) 0.0013(19) C7 0.013(2) 0.018(3) 0.0122(19) -0.006(2) 0.0073(15) -0.004(2) C8 0.011(2) 0.024(3) 0.013(2) -0.0012(18) 0.0024(15) -0.0003(19) C9 0.020(3) 0.027(3) 0.014(2) -0.011(2) 0.0049(18) -0.007(2) C10 0.025(3) 0.023(3) 0.028(3) -0.011(2) 0.011(2) -0.004(2) C11 0.026(3) 0.020(3) 0.034(3) -0.004(2) 0.007(2) 0.002(2) C12 0.021(3) 0.021(3) 0.016(2) -0.0011(18) 0.0013(18) 0.0013(19) C13 0.015(2) 0.015(2) 0.013(2) 0.0003(17) 0.0059(16) 0.0003(18) C14 0.017(2) 0.024(3) 0.017(2) -0.0003(19) 0.0054(19) 0.003(2) C15 0.019(3) 0.024(3) 0.019(2) 0.001(2) 0.0080(19) -0.002(2) C16 0.026(3) 0.023(3) 0.024(3) 0.001(2) 0.014(2) 0.003(2) C17 0.028(3) 0.031(3) 0.019(2) -0.009(2) 0.007(2) -0.003(2) C18 0.021(3) 0.026(3) 0.025(3) -0.008(2) 0.009(2) -0.0049(19) C19 0.013(2) 0.015(3) 0.016(2) -0.0021(16) 0.0008(17) -0.0001(17) C20 0.023(3) 0.017(3) 0.019(2) 0.0041(18) 0.0135(19) 0.0095(19) C21 0.032(3) 0.024(3) 0.022(2) 0.0006(19) 0.012(2) 0.0021(19) C22 0.034(3) 0.029(3) 0.022(3) 0.002(2) 0.009(2) 0.009(2) C23 0.040(3) 0.032(3) 0.025(3) 0.009(2) 0.019(2) 0.012(3) C24 0.030(3) 0.031(3) 0.027(3) 0.011(2) 0.013(2) 0.000(2) C25 0.022(2) 0.027(3) 0.020(2) 0.0042(18) 0.0072(18) 0.0040(19) Pt1A 0.01101(9) 0.01552(10) 0.01007(8) 0.00091(7) 0.00353(6) -0.00056(7) Cl1A 0.0140(6) 0.0242(7) 0.0146(5) 0.0027(4) 0.0043(4) 0.0058(5) P1A 0.0140(6) 0.0172(7) 0.0103(5) 0.0018(5) 0.0041(4) -0.0013(5) S1A 0.0208(6) 0.0194(6) 0.0164(5) 0.0030(6) 0.0102(4) 0.0043(7) S2A 0.0121(6) 0.0326(10) 0.0124(5) 0.0063(5) 0.0046(4) 0.0008(5) N1A 0.0129(18) 0.018(2) 0.0150(17) 0.0006(18) 0.0056(13) 0.0012(17) O1A 0.0123(17) 0.029(2) 0.0131(15) 0.0040(14) 0.0052(12) -0.0045(15) C1A 0.019(2) 0.014(2) 0.014(2) -0.0026(17) 0.0029(17) 0.0001(18) C2A 0.013(2) 0.016(3) 0.009(2) -0.0032(17) 0.0011(16) 0.0019(19) C3A 0.018(2) 0.012(3) 0.015(2) -0.0036(18) 0.0054(17) -0.0059(19) C4A 0.022(3) 0.020(3) 0.014(2) 0.0011(19) 0.0034(19) -0.001(2) C5A 0.020(2) 0.027(3) 0.019(2) 0.0033(19) 0.0051(18) 0.006(2) C6A 0.015(2) 0.029(3) 0.020(2) 0.003(2) 0.0100(18) 0.005(2) C7A 0.017(2) 0.022(3) 0.015(2) -0.001(2) 0.0054(17) -0.001(2) C8A 0.025(3) 0.025(3) 0.018(2) 0.0012(19) 0.0065(19) -0.005(2) C9A 0.031(3) 0.042(4) 0.018(3) -0.004(2) 0.010(2) -0.015(3) C10A 0.028(3) 0.030(3) 0.036(3) -0.014(2) 0.014(2) -0.008(2) C11A 0.036(3) 0.018(3) 0.040(3) -0.003(2) 0.006(3) 0.001(2) C12A 0.033(3) 0.027(3) 0.019(3) 0.004(2) 0.003(2) 0.006(2) C13A 0.022(3) 0.018(3) 0.012(2) 0.0028(18) 0.0056(18) 0.0034(19) C14A 0.020(3) 0.033(3) 0.011(2) -0.003(2) 0.0033(18) -0.006(2) C15A 0.019(3) 0.032(3) 0.027(3) 0.001(2) 0.012(2) -0.006(2) C16A 0.032(3) 0.022(3) 0.018(2) 0.0016(19) 0.016(2) 0.001(2) C17A 0.033(3) 0.025(3) 0.015(2) -0.0013(19) 0.0070(19) 0.001(2) C18A 0.016(2) 0.024(2) 0.019(2) 0.0011(19) 0.0065(16) -0.003(2) C19A 0.017(2) 0.015(2) 0.0129(19) -0.0023(18) 0.0054(15) -0.0026(19) C20A 0.015(2) 0.018(2) 0.015(2) -0.0006(17) 0.0060(17) -0.0003(18) C21A 0.021(2) 0.021(2) 0.028(3) 0.0058(18) 0.0110(19) 0.0017(18) C22A 0.019(2) 0.023(2) 0.030(3) 0.007(2) 0.0075(19) 0.0037(18) C23A 0.025(3) 0.029(3) 0.015(2) 0.0071(18) 0.0078(19) -0.001(2) C24A 0.023(3) 0.032(3) 0.017(2) -0.004(2) 0.0107(19) -0.003(2) C25A 0.016(2) 0.020(2) 0.017(2) 0.0035(18) 0.0049(16) -0.0011(17) S1S 0.0181(6) 0.0266(6) 0.0244(6) -0.0021(5) 0.0053(4) 0.0008(5) O1S 0.0162(17) 0.035(2) 0.0213(19) 0.0012(15) 0.0051(13) -0.0006(16) C1S 0.026(3) 0.041(3) 0.028(3) -0.008(2) 0.008(2) -0.010(2) C2S 0.034(3) 0.026(3) 0.026(3) 0.002(2) 0.016(2) -0.002(2) S1SA 0.0179(5) 0.0301(6) 0.0207(6) 0.0008(5) 0.0077(4) -0.0046(5) O1SA 0.026(2) 0.083(4) 0.043(3) -0.027(2) 0.0256(18) -0.029(2) C1SA 0.052(4) 0.030(3) 0.034(3) -0.006(3) 0.023(2) 0.000(3) C2SA 0.027(3) 0.026(3) 0.032(3) -0.002(2) 0.018(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C2 2.000(5) . ? Pt1 S2 2.2561(13) . ? Pt1 S1 2.3380(12) . ? Pt1 Cl1 2.3821(12) . ? P1 O1 1.593(3) . ? P1 C13 1.784(5) . ? P1 C7 1.787(6) . ? P1 S1 1.976(2) . ? S2 C19 1.691(5) . ? N1 C19 1.321(6) . ? N1 C20 1.440(6) . ? N1 H1N 0.9697 . ? O1 C3 1.412(6) . ? C1 C6 1.405(6) . ? C1 C2 1.436(7) . ? C1 C19 1.457(7) . ? C2 C3 1.418(7) . ? C3 C4 1.381(7) . ? C4 C5 1.382(7) . ? C4 H4A 0.9500 . ? C5 C6 1.376(7) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.384(6) . ? C7 C12 1.410(8) . ? C8 C9 1.403(7) . ? C8 H8A 0.9500 . ? C9 C10 1.381(8) . ? C9 H9A 0.9500 . ? C10 C11 1.391(7) . ? C10 H10A 0.9500 . ? C11 C12 1.374(7) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.391(7) . ? C13 C14 1.399(7) . ? C14 C15 1.392(7) . ? C14 H14A 0.9500 . ? C15 C16 1.390(7) . ? C15 H15A 0.9500 . ? C16 C17 1.402(7) . ? C16 H16A 0.9500 . ? C17 C18 1.366(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C20 C25 1.391(7) . ? C20 C21 1.393(7) . ? C21 C22 1.394(7) . ? C21 H21A 0.9500 . ? C22 C23 1.385(8) . ? C22 H22A 0.9500 . ? C23 C24 1.377(7) . ? C23 H23A 0.9500 . ? C24 C25 1.394(6) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? Pt1A C2A 2.016(5) . ? Pt1A S2A 2.2510(13) . ? Pt1A S1A 2.3429(12) . ? Pt1A Cl1A 2.3880(11) . ? P1A O1A 1.577(3) . ? P1A C7A 1.785(6) . ? P1A C13A 1.789(5) . ? P1A S1A 1.976(2) . ? S2A C19A 1.706(5) . ? N1A C19A 1.328(6) . ? N1A C20A 1.428(6) . ? N1A H1NA 0.9201 . ? O1A C3A 1.412(6) . ? C1A C6A 1.392(6) . ? C1A C2A 1.428(7) . ? C1A C19A 1.464(7) . ? C2A C3A 1.385(7) . ? C3A C4A 1.384(7) . ? C4A C5A 1.360(7) . ? C4A H4AA 0.9500 . ? C5A C6A 1.383(7) . ? C5A H5AA 0.9500 . ? C6A H6AA 0.9500 . ? C7A C8A 1.387(6) . ? C7A C12A 1.390(8) . ? C8A C9A 1.377(8) . ? C8A H8AA 0.9500 . ? C9A C10A 1.382(9) . ? C9A H9AA 0.9500 . ? C10A C11A 1.379(8) . ? C10A H10B 0.9500 . ? C11A C12A 1.391(8) . ? C11A H11B 0.9500 . ? C12A H12B 0.9500 . ? C13A C14A 1.386(7) . ? C13A C18A 1.411(6) . ? C14A C15A 1.375(7) . ? C14A H14B 0.9500 . ? C15A C16A 1.358(7) . ? C15A H15B 0.9500 . ? C16A C17A 1.387(7) . ? C16A H16B 0.9500 . ? C17A C18A 1.398(6) . ? C17A H17B 0.9500 . ? C18A H18B 0.9500 . ? C20A C21A 1.387(7) . ? C20A C25A 1.397(6) . ? C21A C22A 1.385(6) . ? C21A H21B 0.9500 . ? C22A C23A 1.378(7) . ? C22A H22B 0.9500 . ? C23A C24A 1.390(7) . ? C23A H23B 0.9500 . ? C24A C25A 1.389(6) . ? C24A H24B 0.9500 . ? C25A H25B 0.9500 . ? S1S O1S 1.502(5) . ? S1S C2S 1.774(5) . ? S1S C1S 1.782(5) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? S1SA O1SA 1.500(4) . ? S1SA C1SA 1.782(6) . ? S1SA C2SA 1.785(5) . ? C1SA H1SD 0.9800 . ? C1SA H1SE 0.9800 . ? C1SA H1SF 0.9800 . ? C2SA H2SD 0.9800 . ? C2SA H2SE 0.9800 . ? C2SA H2SF 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt1 S2 85.62(15) . . ? C2 Pt1 S1 101.97(15) . . ? S2 Pt1 S1 170.03(6) . . ? C2 Pt1 Cl1 170.84(14) . . ? S2 Pt1 Cl1 87.80(4) . . ? S1 Pt1 Cl1 85.31(4) . . ? O1 P1 C13 102.36(19) . . ? O1 P1 C7 107.4(2) . . ? C13 P1 C7 111.2(2) . . ? O1 P1 S1 111.76(16) . . ? C13 P1 S1 109.74(18) . . ? C7 P1 S1 113.82(18) . . ? P1 S1 Pt1 97.69(7) . . ? C19 S2 Pt1 101.20(18) . . ? C19 N1 C20 128.6(4) . . ? C19 N1 H1N 121.2 . . ? C20 N1 H1N 107.7 . . ? C3 O1 P1 122.4(3) . . ? C6 C1 C2 123.1(4) . . ? C6 C1 C19 120.6(4) . . ? C2 C1 C19 116.2(4) . . ? C3 C2 C1 112.2(4) . . ? C3 C2 Pt1 129.0(4) . . ? C1 C2 Pt1 118.4(3) . . ? C4 C3 O1 112.7(4) . . ? C4 C3 C2 125.1(4) . . ? O1 C3 C2 122.2(5) . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 119.4(4) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C1 120.2(4) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? C8 C7 C12 120.4(5) . . ? C8 C7 P1 120.9(4) . . ? C12 C7 P1 118.7(3) . . ? C7 C8 C9 118.8(5) . . ? C7 C8 H8A 120.6 . . ? C9 C8 H8A 120.6 . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 119.9(5) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 120.4(5) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C7 119.7(4) . . ? C11 C12 H12A 120.1 . . ? C7 C12 H12A 120.1 . . ? C18 C13 C14 119.9(4) . . ? C18 C13 P1 118.7(4) . . ? C14 C13 P1 121.2(4) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 119.4(5) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 C17 120.2(5) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C13 120.3(5) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? N1 C19 C1 119.0(4) . . ? N1 C19 S2 123.3(4) . . ? C1 C19 S2 117.7(4) . . ? C25 C20 C21 120.8(4) . . ? C25 C20 N1 117.2(4) . . ? C21 C20 N1 121.9(5) . . ? C20 C21 C22 118.8(5) . . ? C20 C21 H21A 120.6 . . ? C22 C21 H21A 120.6 . . ? C23 C22 C21 120.3(5) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 120.7(5) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 119.7(5) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C20 C25 C24 119.6(4) . . ? C20 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C2A Pt1A S2A 85.53(14) . . ? C2A Pt1A S1A 101.04(14) . . ? S2A Pt1A S1A 169.92(6) . . ? C2A Pt1A Cl1A 172.79(13) . . ? S2A Pt1A Cl1A 88.61(4) . . ? S1A Pt1A Cl1A 85.35(4) . . ? O1A P1A C7A 108.8(2) . . ? O1A P1A C13A 101.2(2) . . ? C7A P1A C13A 108.0(2) . . ? O1A P1A S1A 112.20(17) . . ? C7A P1A S1A 113.68(18) . . ? C13A P1A S1A 112.21(19) . . ? P1A S1A Pt1A 97.03(7) . . ? C19A S2A Pt1A 101.69(16) . . ? C19A N1A C20A 128.6(4) . . ? C19A N1A H1NA 117.9 . . ? C20A N1A H1NA 113.4 . . ? C3A O1A P1A 127.7(3) . . ? C6A C1A C2A 122.0(4) . . ? C6A C1A C19A 120.1(4) . . ? C2A C1A C19A 117.7(4) . . ? C3A C2A C1A 113.8(4) . . ? C3A C2A Pt1A 128.4(4) . . ? C1A C2A Pt1A 117.8(3) . . ? C4A C3A C2A 124.4(5) . . ? C4A C3A O1A 111.4(4) . . ? C2A C3A O1A 124.2(4) . . ? C5A C4A C3A 120.2(5) . . ? C5A C4A H4AA 119.9 . . ? C3A C4A H4AA 119.9 . . ? C4A C5A C6A 119.0(5) . . ? C4A C5A H5AA 120.5 . . ? C6A C5A H5AA 120.5 . . ? C5A C6A C1A 120.5(4) . . ? C5A C6A H6AA 119.7 . . ? C1A C6A H6AA 119.7 . . ? C8A C7A C12A 119.9(5) . . ? C8A C7A P1A 121.9(5) . . ? C12A C7A P1A 118.2(4) . . ? C9A C8A C7A 120.4(5) . . ? C9A C8A H8AA 119.8 . . ? C7A C8A H8AA 119.8 . . ? C8A C9A C10A 119.5(5) . . ? C8A C9A H9AA 120.3 . . ? C10A C9A H9AA 120.3 . . ? C11A C10A C9A 121.0(5) . . ? C11A C10A H10B 119.5 . . ? C9A C10A H10B 119.5 . . ? C10A C11A C12A 119.6(5) . . ? C10A C11A H11B 120.2 . . ? C12A C11A H11B 120.2 . . ? C7A C12A C11A 119.6(5) . . ? C7A C12A H12B 120.2 . . ? C11A C12A H12B 120.2 . . ? C14A C13A C18A 120.3(4) . . ? C14A C13A P1A 120.2(4) . . ? C18A C13A P1A 119.4(4) . . ? C15A C14A C13A 119.6(5) . . ? C15A C14A H14B 120.2 . . ? C13A C14A H14B 120.2 . . ? C16A C15A C14A 121.3(5) . . ? C16A C15A H15B 119.3 . . ? C14A C15A H15B 119.3 . . ? C15A C16A C17A 120.4(5) . . ? C15A C16A H16B 119.8 . . ? C17A C16A H16B 119.8 . . ? C16A C17A C18A 120.1(4) . . ? C16A C17A H17B 119.9 . . ? C18A C17A H17B 119.9 . . ? C17A C18A C13A 118.3(4) . . ? C17A C18A H18B 120.8 . . ? C13A C18A H18B 120.8 . . ? N1A C19A C1A 121.7(4) . . ? N1A C19A S2A 121.8(4) . . ? C1A C19A S2A 116.4(3) . . ? C21A C20A C25A 120.9(4) . . ? C21A C20A N1A 123.3(5) . . ? C25A C20A N1A 115.7(5) . . ? C22A C21A C20A 118.2(5) . . ? C22A C21A H21B 120.9 . . ? C20A C21A H21B 120.9 . . ? C23A C22A C21A 122.1(5) . . ? C23A C22A H22B 118.9 . . ? C21A C22A H22B 118.9 . . ? C22A C23A C24A 119.1(5) . . ? C22A C23A H23B 120.5 . . ? C24A C23A H23B 120.5 . . ? C25A C24A C23A 120.2(5) . . ? C25A C24A H24B 119.9 . . ? C23A C24A H24B 119.9 . . ? C24A C25A C20A 119.3(4) . . ? C24A C25A H25B 120.3 . . ? C20A C25A H25B 120.3 . . ? O1S S1S C2S 106.6(3) . . ? O1S S1S C1S 104.3(2) . . ? C2S S1S C1S 98.9(3) . . ? S1S C1S H1SA 109.5 . . ? S1S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? S1S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? S1S C2S H2SA 109.5 . . ? S1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? S1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O1SA S1SA C1SA 106.3(3) . . ? O1SA S1SA C2SA 105.6(3) . . ? C1SA S1SA C2SA 98.1(3) . . ? S1SA C1SA H1SD 109.5 . . ? S1SA C1SA H1SE 109.5 . . ? H1SD C1SA H1SE 109.5 . . ? S1SA C1SA H1SF 109.5 . . ? H1SD C1SA H1SF 109.5 . . ? H1SE C1SA H1SF 109.5 . . ? S1SA C2SA H2SD 109.5 . . ? S1SA C2SA H2SE 109.5 . . ? H2SD C2SA H2SE 109.5 . . ? S1SA C2SA H2SF 109.5 . . ? H2SD C2SA H2SF 109.5 . . ? H2SE C2SA H2SF 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 S1 Pt1 55.83(15) . . . . ? C13 P1 S1 Pt1 168.66(17) . . . . ? C7 P1 S1 Pt1 -66.04(17) . . . . ? C2 Pt1 S1 P1 -29.11(16) . . . . ? Cl1 Pt1 S1 P1 145.28(7) . . . . ? C2 Pt1 S2 C19 -2.6(2) . . . . ? Cl1 Pt1 S2 C19 -176.23(17) . . . . ? C13 P1 O1 C3 170.7(4) . . . . ? C7 P1 O1 C3 53.6(5) . . . . ? S1 P1 O1 C3 -71.9(4) . . . . ? C6 C1 C2 C3 4.3(7) . . . . ? C19 C1 C2 C3 -178.5(4) . . . . ? C6 C1 C2 Pt1 -168.7(4) . . . . ? C19 C1 C2 Pt1 8.5(6) . . . . ? S2 Pt1 C2 C3 -174.4(5) . . . . ? S1 Pt1 C2 C3 12.1(5) . . . . ? S2 Pt1 C2 C1 -2.8(4) . . . . ? S1 Pt1 C2 C1 -176.2(4) . . . . ? P1 O1 C3 C4 -137.3(4) . . . . ? P1 O1 C3 C2 44.6(7) . . . . ? C1 C2 C3 C4 -4.1(7) . . . . ? Pt1 C2 C3 C4 168.0(4) . . . . ? C1 C2 C3 O1 173.8(4) . . . . ? Pt1 C2 C3 O1 -14.2(7) . . . . ? O1 C3 C4 C5 -177.0(5) . . . . ? C2 C3 C4 C5 1.0(8) . . . . ? C3 C4 C5 C6 2.2(8) . . . . ? C4 C5 C6 C1 -1.9(8) . . . . ? C2 C1 C6 C5 -1.6(7) . . . . ? C19 C1 C6 C5 -178.7(4) . . . . ? O1 P1 C7 C8 -130.4(4) . . . . ? C13 P1 C7 C8 118.4(4) . . . . ? S1 P1 C7 C8 -6.2(5) . . . . ? O1 P1 C7 C12 50.5(4) . . . . ? C13 P1 C7 C12 -60.7(4) . . . . ? S1 P1 C7 C12 174.8(3) . . . . ? C12 C7 C8 C9 -0.2(7) . . . . ? P1 C7 C8 C9 -179.2(4) . . . . ? C7 C8 C9 C10 -0.6(8) . . . . ? C8 C9 C10 C11 0.8(9) . . . . ? C9 C10 C11 C12 0.0(9) . . . . ? C10 C11 C12 C7 -0.8(8) . . . . ? C8 C7 C12 C11 0.9(8) . . . . ? P1 C7 C12 C11 180.0(4) . . . . ? O1 P1 C13 C18 52.3(5) . . . . ? C7 P1 C13 C18 166.6(4) . . . . ? S1 P1 C13 C18 -66.5(4) . . . . ? O1 P1 C13 C14 -133.6(4) . . . . ? C7 P1 C13 C14 -19.2(5) . . . . ? S1 P1 C13 C14 107.6(4) . . . . ? C18 C13 C14 C15 1.2(8) . . . . ? P1 C13 C14 C15 -172.9(4) . . . . ? C13 C14 C15 C16 -0.4(8) . . . . ? C14 C15 C16 C17 -0.7(8) . . . . ? C15 C16 C17 C18 0.8(8) . . . . ? C16 C17 C18 C13 0.1(8) . . . . ? C14 C13 C18 C17 -1.1(8) . . . . ? P1 C13 C18 C17 173.2(4) . . . . ? C20 N1 C19 C1 178.7(5) . . . . ? C20 N1 C19 S2 -3.2(8) . . . . ? C6 C1 C19 N1 -15.6(7) . . . . ? C2 C1 C19 N1 167.2(5) . . . . ? C6 C1 C19 S2 166.1(4) . . . . ? C2 C1 C19 S2 -11.1(6) . . . . ? Pt1 S2 C19 N1 -170.2(4) . . . . ? Pt1 S2 C19 C1 7.9(4) . . . . ? C19 N1 C20 C25 140.9(5) . . . . ? C19 N1 C20 C21 -42.2(8) . . . . ? C25 C20 C21 C22 0.8(7) . . . . ? N1 C20 C21 C22 -176.0(5) . . . . ? C20 C21 C22 C23 0.2(7) . . . . ? C21 C22 C23 C24 -1.3(9) . . . . ? C22 C23 C24 C25 1.4(9) . . . . ? C21 C20 C25 C24 -0.7(7) . . . . ? N1 C20 C25 C24 176.2(4) . . . . ? C23 C24 C25 C20 -0.4(8) . . . . ? O1A P1A S1A Pt1A -56.42(16) . . . . ? C7A P1A S1A Pt1A 67.55(19) . . . . ? C13A P1A S1A Pt1A -169.55(18) . . . . ? C2A Pt1A S1A P1A 35.42(16) . . . . ? S2A Pt1A S1A P1A 165.5(2) . . . . ? Cl1A Pt1A S1A P1A -141.19(7) . . . . ? C2A Pt1A S2A C19A 7.6(2) . . . . ? S1A Pt1A S2A C19A -123.5(3) . . . . ? Cl1A Pt1A S2A C19A -176.6(2) . . . . ? C7A P1A O1A C3A -66.7(5) . . . . ? C13A P1A O1A C3A 179.7(4) . . . . ? S1A P1A O1A C3A 59.9(5) . . . . ? C6A C1A C2A C3A -1.1(7) . . . . ? C19A C1A C2A C3A -176.8(5) . . . . ? C6A C1A C2A Pt1A 178.2(4) . . . . ? C19A C1A C2A Pt1A 2.5(6) . . . . ? S2A Pt1A C2A C3A 172.7(5) . . . . ? S1A Pt1A C2A C3A -15.0(5) . . . . ? S2A Pt1A C2A C1A -6.5(4) . . . . ? S1A Pt1A C2A C1A 165.8(3) . . . . ? C1A C2A C3A C4A 3.2(7) . . . . ? Pt1A C2A C3A C4A -176.0(4) . . . . ? C1A C2A C3A O1A -176.5(4) . . . . ? Pt1A C2A C3A O1A 4.3(8) . . . . ? P1A O1A C3A C4A 153.8(4) . . . . ? P1A O1A C3A C2A -26.5(7) . . . . ? C2A C3A C4A C5A -3.3(8) . . . . ? O1A C3A C4A C5A 176.4(4) . . . . ? C3A C4A C5A C6A 1.2(8) . . . . ? C4A C5A C6A C1A 0.8(8) . . . . ? C2A C1A C6A C5A -0.8(8) . . . . ? C19A C1A C6A C5A 174.8(5) . . . . ? O1A P1A C7A C8A 112.7(5) . . . . ? C13A P1A C7A C8A -138.3(4) . . . . ? S1A P1A C7A C8A -13.1(5) . . . . ? O1A P1A C7A C12A -66.0(5) . . . . ? C13A P1A C7A C12A 43.0(5) . . . . ? S1A P1A C7A C12A 168.2(4) . . . . ? C12A C7A C8A C9A -1.2(8) . . . . ? P1A C7A C8A C9A -179.9(4) . . . . ? C7A C8A C9A C10A 1.4(9) . . . . ? C8A C9A C10A C11A -0.6(9) . . . . ? C9A C10A C11A C12A -0.4(9) . . . . ? C8A C7A C12A C11A 0.2(8) . . . . ? P1A C7A C12A C11A 179.0(4) . . . . ? C10A C11A C12A C7A 0.6(8) . . . . ? O1A P1A C13A C14A 157.7(5) . . . . ? C7A P1A C13A C14A 43.6(5) . . . . ? S1A P1A C13A C14A -82.5(5) . . . . ? O1A P1A C13A C18A -27.3(5) . . . . ? C7A P1A C13A C18A -141.5(4) . . . . ? S1A P1A C13A C18A 92.4(4) . . . . ? C18A C13A C14A C15A 0.0(9) . . . . ? P1A C13A C14A C15A 174.9(5) . . . . ? C13A C14A C15A C16A -0.3(9) . . . . ? C14A C15A C16A C17A 0.5(9) . . . . ? C15A C16A C17A C18A -0.5(8) . . . . ? C16A C17A C18A C13A 0.3(7) . . . . ? C14A C13A C18A C17A 0.0(8) . . . . ? P1A C13A C18A C17A -175.0(4) . . . . ? C20A N1A C19A C1A 178.6(5) . . . . ? C20A N1A C19A S2A -3.0(8) . . . . ? C6A C1A C19A N1A 7.8(8) . . . . ? C2A C1A C19A N1A -176.5(5) . . . . ? C6A C1A C19A S2A -170.7(4) . . . . ? C2A C1A C19A S2A 5.0(6) . . . . ? Pt1A S2A C19A N1A 172.8(4) . . . . ? Pt1A S2A C19A C1A -8.8(4) . . . . ? C19A N1A C20A C21A -41.4(8) . . . . ? C19A N1A C20A C25A 141.4(5) . . . . ? C25A C20A C21A C22A -0.4(7) . . . . ? N1A C20A C21A C22A -177.4(5) . . . . ? C20A C21A C22A C23A 0.1(7) . . . . ? C21A C22A C23A C24A 1.0(8) . . . . ? C22A C23A C24A C25A -2.0(7) . . . . ? C23A C24A C25A C20A 1.8(7) . . . . ? C21A C20A C25A C24A -0.6(7) . . . . ? N1A C20A C25A C24A 176.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1A H1NA O1SA 2_646 0.92 1.96 2.846(6) 161 ? N1 H1N O1S 2_646 0.97 1.84 2.781(6) 162 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.339 _refine_diff_density_min -1.740 _refine_diff_density_rms 0.107