data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C36 H31 N2 P2 Pt.C24 H20 N1 O1 P2 Se.(CH4O1)0.5 ' _chemical_formula_structural 'C60.50 H53 N3 O1.50 P4 Pt Se' _chemical_formula_analytical 'C60.50 H53 N3 O1.50 P4 Pt Se' _chemical_formula_sum 'C60.50 H53 N3 O1.50 P4 Pt Se' _chemical_formula_weight 1243.99 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3168(6) _cell_length_b 13.4648(6) _cell_length_c 18.2628(8) _cell_angle_alpha 109.01 _cell_angle_beta 96.1290(10) _cell_angle_gamma 113.8590(10) _cell_volume 2721.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .13 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .13 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method - _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 3.409 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.835703 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 12436 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 23.26 _reflns_number_total 7564 _reflns_number_observed 6323 _reflns_observed_criterion 2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+3.5466P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7514 _refine_ls_number_parameters 662 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_obs 0.0359 _refine_ls_wR_factor_all 0.1009 _refine_ls_wR_factor_obs 0.0824 _refine_ls_goodness_of_fit_all 0.937 _refine_ls_goodness_of_fit_obs 0.935 _refine_ls_restrained_S_all 1.046 _refine_ls_restrained_S_obs 0.934 _refine_ls_shift/esd_max -0.139 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.58672(2) 0.75376(2) 0.707238(14) 0.03254(11) Uani 1 d . . P1 P 0.64283(13) 0.64460(14) 0.75388(9) 0.0335(4) Uani 1 d . . C1 C 0.7935(5) 0.7147(5) 0.7656(4) 0.0377(15) Uani 1 d . . C2 C 0.8318(5) 0.8128(5) 0.7439(4) 0.0400(15) Uani 1 d . . N2 N 0.7537(4) 0.8445(5) 0.7180(3) 0.0440(13) Uani 1 d D . H2A H 0.7870(41) 0.9193(25) 0.7110(32) 0.034(15) Uiso 1 d D . C3 C 0.9485(5) 0.8690(6) 0.7466(4) 0.053(2) Uani 1 d . . H3A H 0.9760(5) 0.9326(6) 0.7315(4) 0.064 Uiso 1 calc R . C4 C 1.0208(6) 0.8309(7) 0.7710(5) 0.065(2) Uani 1 d . . H4A H 1.0975(6) 0.8697(7) 0.7731(5) 0.078 Uiso 1 calc R . C5 C 0.9828(6) 0.7355(7) 0.7929(5) 0.066(2) Uani 1 d . . H5A H 1.0333(6) 0.7104(7) 0.8095(5) 0.079 Uiso 1 calc R . C6 C 0.8700(6) 0.6787(6) 0.7898(4) 0.051(2) Uani 1 d . . H6A H 0.8442(6) 0.6145(6) 0.8043(4) 0.061 Uiso 1 calc R . C7 C 0.5870(5) 0.4878(5) 0.6895(4) 0.0362(14) Uani 1 d . . C8 C 0.5912(6) 0.4083(6) 0.7204(4) 0.053(2) Uani 1 d . . H8A H 0.6193(6) 0.4339(6) 0.7757(4) 0.064 Uiso 1 calc R . C9 C 0.5534(7) 0.2897(7) 0.6696(5) 0.066(2) Uani 1 d . . H9A H 0.5564(7) 0.2363(7) 0.6905(5) 0.079 Uiso 1 calc R . C10 C 0.5119(7) 0.2531(7) 0.5883(5) 0.064(2) Uani 1 d . . H10A H 0.4859(7) 0.1741(7) 0.5540(5) 0.077 Uiso 1 calc R . C11 C 0.5083(6) 0.3314(7) 0.5575(5) 0.062(2) Uani 1 d . . H11A H 0.4809(6) 0.3058(7) 0.5022(5) 0.074 Uiso 1 calc R . C12 C 0.5453(5) 0.4492(6) 0.6081(4) 0.045(2) Uani 1 d . . H12A H 0.5417(5) 0.5020(6) 0.5866(4) 0.055 Uiso 1 calc R . C13 C 0.6208(5) 0.6498(6) 0.8512(4) 0.0400(15) Uani 1 d . . C14 C 0.5211(6) 0.5704(7) 0.8582(4) 0.053(2) Uani 1 d . . H14A H 0.4658(6) 0.5077(7) 0.8122(4) 0.063 Uiso 1 calc R . C15 C 0.5025(7) 0.5832(8) 0.9329(5) 0.066(2) Uani 1 d . . H15A H 0.4351(7) 0.5285(8) 0.9367(5) 0.080 Uiso 1 calc R . C16 C 0.5823(9) 0.6753(9) 1.0014(5) 0.075(3) Uani 1 d . . H16A H 0.5689(9) 0.6837(9) 1.0514(5) 0.090 Uiso 1 calc R . C17 C 0.6814(9) 0.7547(8) 0.9959(5) 0.077(3) Uani 1 d . . H17A H 0.7359(9) 0.8174(8) 1.0424(5) 0.093 Uiso 1 calc R . C18 C 0.7013(7) 0.7425(6) 0.9212(4) 0.058(2) Uani 1 d . . H18A H 0.7694(7) 0.7970(6) 0.9180(4) 0.069 Uiso 1 calc R . P2 P 0.39729(13) 0.66374(14) 0.68865(9) 0.0334(4) Uani 1 d . . C19 C 0.3527(5) 0.7538(5) 0.6525(4) 0.0368(14) Uani 1 d . . C20 C 0.4378(5) 0.8446(5) 0.6399(3) 0.0363(14) Uani 1 d . . N20 N 0.5561(4) 0.8721(5) 0.6675(3) 0.0384(12) Uani 1 d D . H20A H 0.6083(39) 0.8903(54) 0.6343(29) 0.048(18) Uiso 1 d D . H20B H 0.5877(50) 0.9409(34) 0.7194(18) 0.052(19) Uiso 1 d D . C21 C 0.4112(6) 0.9121(6) 0.6060(4) 0.053(2) Uani 1 d . . H21A H 0.4680(6) 0.9714(6) 0.5968(4) 0.063 Uiso 1 calc R . C22 C 0.2997(7) 0.8902(7) 0.5863(5) 0.065(2) Uani 1 d . . H22A H 0.2811(7) 0.9339(7) 0.5622(5) 0.078 Uiso 1 calc R . C23 C 0.2149(7) 0.8050(7) 0.6015(5) 0.063(2) Uani 1 d . . H23A H 0.1406(7) 0.7945(7) 0.5904(5) 0.075 Uiso 1 calc R . C24 C 0.2408(6) 0.7349(6) 0.6334(4) 0.050(2) Uani 1 d . . H24A H 0.1833(6) 0.6753(6) 0.6419(4) 0.060 Uiso 1 calc R . C25 C 0.3414(5) 0.6616(5) 0.7745(4) 0.0378(15) Uani 1 d . . C26 C 0.2312(6) 0.5824(7) 0.7676(5) 0.059(2) Uani 1 d . . H26A H 0.1840(6) 0.5240(7) 0.7172(5) 0.071 Uiso 1 calc R . C27 C 0.1912(8) 0.5889(8) 0.8336(6) 0.078(3) Uani 1 d . . H27A H 0.1170(8) 0.5351(8) 0.8283(6) 0.094 Uiso 1 calc R . C28 C 0.2608(9) 0.6753(9) 0.9082(6) 0.082(3) Uani 1 d . . H28A H 0.2336(9) 0.6784(9) 0.9533(6) 0.099 Uiso 1 calc R . C29 C 0.3701(8) 0.7572(9) 0.9171(5) 0.079(3) Uani 1 d . . H29A H 0.4158(8) 0.8169(9) 0.9674(5) 0.094 Uiso 1 calc R . C30 C 0.4106(6) 0.7494(6) 0.8503(4) 0.050(2) Uani 1 d . . H30A H 0.4849(6) 0.8032(6) 0.8558(4) 0.060 Uiso 1 calc R . C31 C 0.3157(5) 0.5142(5) 0.6088(4) 0.0357(14) Uani 1 d . . C32 C 0.2919(5) 0.4129(6) 0.6233(4) 0.043(2) Uani 1 d . . H32A H 0.3114(5) 0.4199(6) 0.6759(4) 0.052 Uiso 1 calc R . C33 C 0.2400(6) 0.3030(6) 0.5608(4) 0.050(2) Uani 1 d . . H33A H 0.2247(6) 0.2359(6) 0.5712(4) 0.060 Uiso 1 calc R . C34 C 0.2105(6) 0.2914(6) 0.4837(5) 0.056(2) Uani 1 d . . H34A H 0.1746(6) 0.2163(6) 0.4416(5) 0.067 Uiso 1 calc R . C35 C 0.2336(6) 0.3900(6) 0.4677(4) 0.057(2) Uani 1 d . . H35A H 0.2136(6) 0.3815(6) 0.4149(4) 0.068 Uiso 1 calc R . C36 C 0.2866(5) 0.5020(5) 0.5301(4) 0.041(2) Uani 1 d . . H36A H 0.3026(5) 0.5688(5) 0.5191(4) 0.049 Uiso 1 calc R . Se3 Se 0.75118(7) 0.98976(6) 0.57198(4) 0.0586(2) Uani 1 d . . P3 P 0.87439(14) 1.15012(15) 0.67093(10) 0.0385(4) Uani 1 d . . N3 N 0.8522(5) 1.1813(5) 0.7564(3) 0.0525(15) Uani 1 d . . P4 P 0.76730(14) 1.17844(15) 0.80951(10) 0.0397(4) Uani 1 d . . O4 O 0.6390(4) 1.1058(4) 0.7712(3) 0.0519(12) Uani 1 d . . C37 C 1.0110(6) 1.1500(7) 0.6858(5) 0.054(2) Uani 1 d . . C38 C 1.0959(7) 1.2329(10) 0.7565(6) 0.085(3) Uani 1 d . . H38A H 1.0830(7) 1.2878(10) 0.7953(6) 0.102 Uiso 1 calc R . C39 C 1.2030(10) 1.2327(15) 0.7688(9) 0.132(5) Uani 1 d . . H39A H 1.2612(10) 1.2885(15) 0.8156(9) 0.158 Uiso 1 calc R . C40 C 1.2206(12) 1.1500(19) 0.7117(13) 0.150(8) Uani 1 d . . H40A H 1.2903(12) 1.1490(19) 0.7206(13) 0.180 Uiso 1 calc R . C41 C 1.1366(13) 1.0691(14) 0.6419(11) 0.134(6) Uani 1 d . . H41A H 1.1498(13) 1.0143(14) 0.6034(11) 0.161 Uiso 1 calc R . C42 C 1.0322(8) 1.0682(9) 0.6282(7) 0.086(3) Uani 1 d . . H42A H 0.9757(8) 1.0131(9) 0.5804(7) 0.103 Uiso 1 calc R . C43 C 0.8996(5) 1.2720(5) 0.6408(4) 0.0364(14) Uani 1 d . . C44 C 0.9775(5) 1.3046(6) 0.5991(4) 0.051(2) Uani 1 d . . H44A H 1.0198(5) 1.2639(6) 0.5861(4) 0.061 Uiso 1 calc R . C45 C 0.9948(6) 1.3974(7) 0.5757(5) 0.063(2) Uani 1 d . . H45A H 1.0497(6) 1.4201(7) 0.5487(5) 0.076 Uiso 1 calc R . C46 C 0.9305(7) 1.4554(7) 0.5925(5) 0.062(2) Uani 1 d . . H46A H 0.9410(7) 1.5171(7) 0.5765(5) 0.075 Uiso 1 calc R . C47 C 0.8508(8) 1.4219(8) 0.6328(5) 0.078(3) Uani 1 d . . H47A H 0.8071(8) 1.4612(8) 0.6441(5) 0.094 Uiso 1 calc R . C48 C 0.8341(7) 1.3305(7) 0.6571(5) 0.066(2) Uani 1 d . . H48A H 0.7792(7) 1.3084(7) 0.6842(5) 0.080 Uiso 1 calc R . C49 C 0.7975(5) 1.3293(6) 0.8670(4) 0.042(2) Uani 1 d . . C50 C 0.7151(6) 1.3564(6) 0.8949(4) 0.055(2) Uani 1 d . . H50A H 0.6420(6) 1.2954(6) 0.8836(4) 0.066 Uiso 1 calc R . C51 C 0.7399(8) 1.4733(8) 0.9396(5) 0.068(2) Uani 1 d . . H51A H 0.6832(8) 1.4897(8) 0.9574(5) 0.081 Uiso 1 calc R . C52 C 0.8457(9) 1.5628(8) 0.9571(5) 0.078(3) Uani 1 d . . H52A H 0.8611(9) 1.6406(8) 0.9867(5) 0.093 Uiso 1 calc R . C53 C 0.9288(8) 1.5413(8) 0.9326(7) 0.091(3) Uani 1 d . . H53A H 1.0018(8) 1.6035(8) 0.9456(7) 0.109 Uiso 1 calc R . C54 C 0.9045(7) 1.4221(7) 0.8863(5) 0.074(2) Uani 1 d . . H54A H 0.9620(7) 1.4071(7) 0.8689(5) 0.089 Uiso 1 calc R . C55 C 0.8062(7) 1.1299(6) 0.8839(4) 0.051(2) Uani 1 d . . C56 C 0.9109(8) 1.1318(8) 0.9000(6) 0.094(3) Uani 1 d . . H56A H 0.9613(8) 1.1557(8) 0.8703(6) 0.112 Uiso 1 calc R . C57 C 0.9423(12) 1.0990(10) 0.9591(9) 0.131(6) Uani 1 d . . H57A H 1.0138(12) 1.1025(10) 0.9697(9) 0.157 Uiso 1 calc R . C58 C 0.8701(19) 1.0623(12) 1.0010(7) 0.146(8) Uani 1 d . . H58A H 0.8923(19) 1.0417(12) 1.0415(7) 0.175 Uiso 1 calc R . C59 C 0.7630(20) 1.0546(13) 0.9852(9) 0.172(8) Uani 1 d . . H59A H 0.7126(20) 1.0278(13) 1.0142(9) 0.206 Uiso 1 calc R . C60 C 0.7312(11) 1.0874(10) 0.9253(7) 0.109(4) Uani 1 d . . H60A H 0.6583(11) 1.0804(10) 0.9133(7) 0.131 Uiso 1 calc R . C70 C 0.3790(10) 1.0274(10) 0.8279(7) 0.038(3) Uani 0.50 d P . O70 O 0.4530(8) 1.1221(9) 0.8198(9) 0.098(5) Uani 0.50 d P . 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 0.03321(15) 0.0280(2) 0.0386(2) 0.01691(11) 0.01005(10) 0.01361(11) P1 0.0360(9) 0.0310(9) 0.0376(9) 0.0172(7) 0.0109(7) 0.0166(7) C1 0.038(4) 0.033(4) 0.036(3) 0.012(3) 0.001(3) 0.014(3) C2 0.039(4) 0.035(4) 0.040(4) 0.011(3) 0.008(3) 0.016(3) N2 0.039(3) 0.034(3) 0.060(4) 0.027(3) 0.016(3) 0.011(3) C3 0.034(4) 0.047(4) 0.068(5) 0.024(4) 0.016(3) 0.009(3) C4 0.030(4) 0.075(6) 0.083(6) 0.033(5) 0.008(4) 0.018(4) C5 0.043(4) 0.073(6) 0.082(6) 0.030(5) 0.005(4) 0.031(4) C6 0.043(4) 0.056(5) 0.054(4) 0.025(4) 0.006(3) 0.025(4) C7 0.032(3) 0.030(3) 0.047(4) 0.016(3) 0.014(3) 0.015(3) C8 0.066(5) 0.036(4) 0.059(4) 0.020(4) 0.012(4) 0.026(4) C9 0.087(6) 0.040(5) 0.079(6) 0.030(4) 0.029(5) 0.033(4) C10 0.063(5) 0.040(5) 0.067(5) 0.002(4) 0.013(4) 0.020(4) C11 0.062(5) 0.059(5) 0.052(5) 0.005(4) 0.009(4) 0.031(4) C12 0.044(4) 0.044(4) 0.047(4) 0.017(3) 0.015(3) 0.020(3) C13 0.049(4) 0.037(4) 0.044(4) 0.019(3) 0.013(3) 0.028(3) C14 0.059(5) 0.056(5) 0.058(5) 0.034(4) 0.026(4) 0.029(4) C15 0.076(6) 0.076(6) 0.075(6) 0.049(5) 0.043(5) 0.042(5) C16 0.121(8) 0.089(7) 0.063(6) 0.049(6) 0.055(6) 0.070(7) C17 0.111(7) 0.071(6) 0.039(5) 0.009(4) 0.024(5) 0.043(6) C18 0.071(5) 0.048(5) 0.049(4) 0.017(4) 0.022(4) 0.023(4) P2 0.0341(8) 0.0288(9) 0.0379(9) 0.0157(7) 0.0092(7) 0.0139(7) C19 0.042(4) 0.031(4) 0.037(3) 0.012(3) 0.006(3) 0.019(3) C20 0.042(4) 0.035(4) 0.034(3) 0.011(3) 0.009(3) 0.024(3) N20 0.045(3) 0.034(3) 0.043(3) 0.021(3) 0.017(3) 0.019(3) C21 0.068(5) 0.048(4) 0.056(4) 0.027(4) 0.017(4) 0.033(4) C22 0.088(6) 0.065(6) 0.062(5) 0.031(4) 0.008(4) 0.053(5) C23 0.061(5) 0.066(6) 0.065(5) 0.019(4) 0.004(4) 0.042(5) C24 0.039(4) 0.042(4) 0.066(5) 0.021(4) 0.007(3) 0.020(3) C25 0.040(4) 0.039(4) 0.044(4) 0.020(3) 0.015(3) 0.023(3) C26 0.056(5) 0.055(5) 0.056(5) 0.018(4) 0.022(4) 0.019(4) C27 0.078(6) 0.075(6) 0.083(7) 0.035(6) 0.052(5) 0.027(5) C28 0.113(8) 0.100(8) 0.070(6) 0.049(6) 0.057(6) 0.063(7) C29 0.088(7) 0.097(7) 0.054(5) 0.022(5) 0.024(5) 0.051(6) C30 0.052(4) 0.051(5) 0.051(4) 0.016(4) 0.017(4) 0.030(4) C31 0.031(3) 0.030(3) 0.048(4) 0.017(3) 0.016(3) 0.014(3) C32 0.048(4) 0.036(4) 0.047(4) 0.020(3) 0.010(3) 0.020(3) C33 0.052(4) 0.026(4) 0.070(5) 0.020(4) 0.016(4) 0.015(3) C34 0.056(5) 0.031(4) 0.060(5) 0.006(4) 0.012(4) 0.013(3) C35 0.076(5) 0.041(4) 0.042(4) 0.007(4) 0.016(4) 0.024(4) C36 0.045(4) 0.031(4) 0.048(4) 0.019(3) 0.019(3) 0.015(3) Se3 0.0799(5) 0.0369(4) 0.0477(4) 0.0185(3) 0.0235(4) 0.0147(4) P3 0.0413(9) 0.0413(10) 0.0438(10) 0.0220(8) 0.0198(8) 0.0236(8) N3 0.046(3) 0.065(4) 0.041(3) 0.020(3) 0.016(3) 0.020(3) P4 0.0411(9) 0.0372(10) 0.0356(9) 0.0129(8) 0.0123(7) 0.0146(8) O4 0.037(2) 0.043(3) 0.054(3) 0.006(2) 0.011(2) 0.009(2) C37 0.057(5) 0.073(5) 0.081(6) 0.060(5) 0.044(4) 0.046(4) C38 0.055(5) 0.125(9) 0.109(8) 0.071(7) 0.031(5) 0.052(6) C39 0.076(8) 0.224(16) 0.166(13) 0.140(13) 0.050(8) 0.082(10) C40 0.095(10) 0.259(22) 0.262(22) 0.217(20) 0.109(12) 0.133(13) C41 0.154(12) 0.178(14) 0.246(18) 0.169(15) 0.153(13) 0.149(12) C42 0.098(7) 0.095(7) 0.148(9) 0.089(7) 0.087(7) 0.078(6) C43 0.036(3) 0.032(4) 0.039(4) 0.009(3) 0.009(3) 0.019(3) C44 0.038(4) 0.048(4) 0.081(5) 0.037(4) 0.021(4) 0.024(3) C45 0.038(4) 0.062(5) 0.093(6) 0.050(5) 0.015(4) 0.013(4) C46 0.069(5) 0.045(5) 0.066(5) 0.027(4) 0.001(4) 0.021(4) C47 0.115(7) 0.079(6) 0.089(6) 0.045(5) 0.035(6) 0.078(6) C48 0.081(6) 0.081(6) 0.081(6) 0.051(5) 0.040(5) 0.058(5) C49 0.049(4) 0.042(4) 0.041(4) 0.021(3) 0.012(3) 0.024(3) C50 0.056(5) 0.045(5) 0.061(5) 0.019(4) 0.020(4) 0.021(4) C51 0.086(6) 0.059(6) 0.073(6) 0.023(5) 0.031(5) 0.049(5) C52 0.102(8) 0.043(5) 0.080(6) 0.015(4) 0.002(5) 0.038(5) C53 0.070(6) 0.043(5) 0.131(9) 0.024(6) 0.005(6) 0.015(5) C54 0.052(5) 0.042(5) 0.105(7) 0.016(5) 0.019(5) 0.013(4) C55 0.083(5) 0.027(4) 0.032(4) 0.006(3) 0.013(4) 0.021(4) C56 0.077(6) 0.079(7) 0.101(7) 0.055(6) -0.015(5) 0.010(5) C57 0.133(11) 0.083(8) 0.129(11) 0.058(8) -0.041(9) 0.015(7) C58 0.287(23) 0.079(9) 0.067(7) 0.025(6) -0.003(11) 0.097(12) C59 0.379(27) 0.160(14) 0.137(12) 0.128(11) 0.183(16) 0.192(17) C60 0.199(12) 0.125(9) 0.124(8) 0.102(8) 0.116(9) 0.127(9) C70 0.033(7) 0.026(7) 0.044(7) 0.002(6) 0.025(6) 0.010(6) O70 0.034(6) 0.049(7) 0.157(12) -0.017(7) 0.043(7) 0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.008(5) . ? Pt1 N20 2.108(5) . ? Pt1 P1 2.2389(15) . ? Pt1 P2 2.241(2) . ? P1 C1 1.790(6) . ? P1 C13 1.816(6) . ? P1 C7 1.822(6) . ? C1 C6 1.383(9) . ? C1 C2 1.414(8) . ? C2 N2 1.369(8) . ? C2 C3 1.413(9) . ? C3 C4 1.360(10) . ? C4 C5 1.384(11) . ? C5 C6 1.367(10) . ? C7 C12 1.370(9) . ? C7 C8 1.380(8) . ? C8 C9 1.396(10) . ? C9 C10 1.370(11) . ? C10 C11 1.362(11) . ? C11 C12 1.388(10) . ? C13 C14 1.378(9) . ? C13 C18 1.388(9) . ? C14 C15 1.380(10) . ? C15 C16 1.368(12) . ? C16 C17 1.360(12) . ? C17 C18 1.388(10) . ? P2 C19 1.811(6) . ? P2 C25 1.809(6) . ? P2 C31 1.828(6) . ? C19 C24 1.390(8) . ? C19 C20 1.396(8) . ? C20 C21 1.383(8) . ? C20 N20 1.453(8) . ? C21 C22 1.372(10) . ? C22 C23 1.376(11) . ? C23 C24 1.389(10) . ? C25 C30 1.395(9) . ? C25 C26 1.383(9) . ? C26 C27 1.360(10) . ? C27 C28 1.377(12) . ? C28 C29 1.377(12) . ? C29 C30 1.376(10) . ? C31 C36 1.385(8) . ? C31 C32 1.391(8) . ? C32 C33 1.369(9) . ? C33 C34 1.361(10) . ? C34 C35 1.372(9) . ? C35 C36 1.385(9) . ? Se3 P3 2.140(2) . ? P3 N3 1.572(6) . ? P3 C43 1.814(6) . ? P3 C37 1.812(7) . ? N3 P4 1.563(6) . ? P4 O4 1.520(5) . ? P4 C55 1.801(7) . ? P4 C49 1.803(7) . ? C37 C42 1.399(11) . ? C37 C38 1.386(12) . ? C38 C39 1.421(14) . ? C39 C40 1.37(2) . ? C40 C41 1.37(2) . ? C41 C42 1.380(15) . ? C43 C44 1.367(9) . ? C43 C48 1.389(9) . ? C44 C45 1.391(9) . ? C45 C46 1.370(11) . ? C46 C47 1.367(11) . ? C47 C48 1.384(10) . ? C49 C54 1.372(10) . ? C49 C50 1.384(9) . ? C50 C51 1.392(10) . ? C51 C52 1.349(12) . ? C52 C53 1.338(13) . ? C53 C54 1.425(12) . ? C55 C60 1.370(11) . ? C55 C56 1.383(12) . ? C56 C57 1.377(14) . ? C57 C58 1.33(2) . ? C58 C59 1.38(2) . ? C59 C60 1.39(2) . ? C70 O70 1.32(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N20 89.5(2) . . ? N2 Pt1 P1 83.3(2) . . ? N20 Pt1 P1 172.70(15) . . ? N2 Pt1 P2 173.99(15) . . ? N20 Pt1 P2 84.56(15) . . ? P1 Pt1 P2 102.61(6) . . ? C1 P1 C13 108.2(3) . . ? C1 P1 C7 107.1(3) . . ? C13 P1 C7 105.7(3) . . ? C1 P1 Pt1 102.1(2) . . ? C13 P1 Pt1 114.9(2) . . ? C7 P1 Pt1 118.2(2) . . ? C6 C1 C2 119.8(6) . . ? C6 C1 P1 126.3(5) . . ? C2 C1 P1 113.8(4) . . ? N2 C2 C3 123.6(6) . . ? N2 C2 C1 118.7(5) . . ? C3 C2 C1 117.7(6) . . ? C2 N2 Pt1 122.0(4) . . ? C4 C3 C2 120.5(7) . . ? C3 C4 C5 121.5(7) . . ? C6 C5 C4 119.1(7) . . ? C5 C6 C1 121.5(7) . . ? C12 C7 C8 119.3(6) . . ? C12 C7 P1 119.2(5) . . ? C8 C7 P1 121.4(5) . . ? C7 C8 C9 120.6(7) . . ? C10 C9 C8 119.2(7) . . ? C11 C10 C9 120.5(7) . . ? C10 C11 C12 120.4(7) . . ? C7 C12 C11 120.1(7) . . ? C14 C13 C18 118.1(6) . . ? C14 C13 P1 122.0(5) . . ? C18 C13 P1 119.7(5) . . ? C13 C14 C15 120.6(7) . . ? C16 C15 C14 120.7(8) . . ? C15 C16 C17 119.7(8) . . ? C16 C17 C18 120.2(8) . . ? C17 C18 C13 120.7(7) . . ? C19 P2 C25 105.0(3) . . ? C19 P2 C31 104.2(3) . . ? C25 P2 C31 106.9(3) . . ? C19 P2 Pt1 102.4(2) . . ? C25 P2 Pt1 119.5(2) . . ? C31 P2 Pt1 117.0(2) . . ? C24 C19 C20 119.0(5) . . ? C24 C19 P2 124.7(5) . . ? C20 C19 P2 116.3(4) . . ? C21 C20 C19 120.9(6) . . ? C21 C20 N20 120.2(6) . . ? C19 C20 N20 118.8(5) . . ? C20 N20 Pt1 117.3(4) . . ? C20 C21 C22 119.0(7) . . ? C23 C22 C21 121.4(7) . . ? C22 C23 C24 119.7(7) . . ? C23 C24 C19 119.9(7) . . ? C30 C25 C26 118.8(6) . . ? C30 C25 P2 117.9(5) . . ? C26 C25 P2 123.1(5) . . ? C27 C26 C25 120.8(7) . . ? C26 C27 C28 119.8(8) . . ? C27 C28 C29 121.0(8) . . ? C28 C29 C30 118.9(8) . . ? C29 C30 C25 120.6(7) . . ? C36 C31 C32 118.9(6) . . ? C36 C31 P2 118.6(4) . . ? C32 C31 P2 122.1(5) . . ? C33 C32 C31 120.4(6) . . ? C34 C33 C32 120.4(6) . . ? C33 C34 C35 120.2(7) . . ? C34 C35 C36 120.2(7) . . ? C31 C36 C35 119.8(6) . . ? N3 P3 C43 109.7(3) . . ? N3 P3 C37 105.4(3) . . ? C43 P3 C37 104.0(3) . . ? N3 P3 Se3 119.6(2) . . ? C43 P3 Se3 107.5(2) . . ? C37 P3 Se3 109.5(3) . . ? P4 N3 P3 149.9(4) . . ? O4 P4 N3 120.5(3) . . ? O4 P4 C55 108.6(3) . . ? N3 P4 C55 106.5(3) . . ? O4 P4 C49 107.6(3) . . ? N3 P4 C49 108.1(3) . . ? C55 P4 C49 104.4(3) . . ? C42 C37 C38 119.7(8) . . ? C42 C37 P3 121.7(7) . . ? C38 C37 P3 118.6(6) . . ? C37 C38 C39 118.9(11) . . ? C40 C39 C38 120.1(14) . . ? C41 C40 C39 120.5(12) . . ? C40 C41 C42 120.5(14) . . ? C37 C42 C41 120.3(12) . . ? C44 C43 C48 118.7(6) . . ? C44 C43 P3 122.0(5) . . ? C48 C43 P3 119.2(5) . . ? C43 C44 C45 121.2(6) . . ? C46 C45 C44 119.8(7) . . ? C45 C46 C47 119.4(7) . . ? C46 C47 C48 121.1(8) . . ? C47 C48 C43 119.7(7) . . ? C54 C49 C50 117.3(7) . . ? C54 C49 P4 120.9(6) . . ? C50 C49 P4 121.8(5) . . ? C49 C50 C51 121.1(7) . . ? C52 C51 C50 120.2(8) . . ? C53 C52 C51 121.0(8) . . ? C52 C53 C54 119.4(8) . . ? C49 C54 C53 121.0(8) . . ? C60 C55 C56 117.8(8) . . ? C60 C55 P4 120.6(7) . . ? C56 C55 P4 121.5(6) . . ? C57 C56 C55 121.4(11) . . ? C58 C57 C56 120.0(14) . . ? C57 C58 C59 120.9(12) . . ? C58 C59 C60 119.2(13) . . ? C55 C60 C59 120.6(13) . . ? 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 Pt1 P1 C1 -0.8(3) . . . . ? N20 Pt1 P1 C1 -12.6(12) . . . . ? P2 Pt1 P1 C1 178.3(2) . . . . ? N2 Pt1 P1 C13 116.1(3) . . . . ? N20 Pt1 P1 C13 104.2(12) . . . . ? P2 Pt1 P1 C13 -64.8(2) . . . . ? N2 Pt1 P1 C7 -117.9(3) . . . . ? N20 Pt1 P1 C7 -129.8(12) . . . . ? P2 Pt1 P1 C7 61.2(2) . . . . ? C13 P1 C1 C6 61.4(7) . . . . ? C7 P1 C1 C6 -52.1(7) . . . . ? Pt1 P1 C1 C6 -177.0(6) . . . . ? C13 P1 C1 C2 -121.3(5) . . . . ? C7 P1 C1 C2 125.2(5) . . . . ? Pt1 P1 C1 C2 0.3(5) . . . . ? C6 C1 C2 N2 178.2(6) . . . . ? P1 C1 C2 N2 0.7(8) . . . . ? C6 C1 C2 C3 1.3(9) . . . . ? P1 C1 C2 C3 -176.2(5) . . . . ? C3 C2 N2 Pt1 175.2(5) . . . . ? C1 C2 N2 Pt1 -1.5(8) . . . . ? N20 Pt1 N2 C2 179.9(5) . . . . ? P1 Pt1 N2 C2 1.3(5) . . . . ? P2 Pt1 N2 C2 -170.1(13) . . . . ? N2 C2 C3 C4 -178.2(7) . . . . ? C1 C2 C3 C4 -1.5(10) . . . . ? C2 C3 C4 C5 0.9(12) . . . . ? C3 C4 C5 C6 -0.1(13) . . . . ? C4 C5 C6 C1 -0.2(12) . . . . ? C2 C1 C6 C5 -0.5(11) . . . . ? P1 C1 C6 C5 176.7(6) . . . . ? C1 P1 C7 C12 -93.1(5) . . . . ? C13 P1 C7 C12 151.7(5) . . . . ? Pt1 P1 C7 C12 21.3(6) . . . . ? C1 P1 C7 C8 83.6(6) . . . . ? C13 P1 C7 C8 -31.6(6) . . . . ? Pt1 P1 C7 C8 -162.0(5) . . . . ? C12 C7 C8 C9 0.0(10) . . . . ? P1 C7 C8 C9 -176.7(6) . . . . ? C7 C8 C9 C10 -0.1(12) . . . . ? C8 C9 C10 C11 0.5(12) . . . . ? C9 C10 C11 C12 -0.9(12) . . . . ? C8 C7 C12 C11 -0.4(10) . . . . ? P1 C7 C12 C11 176.4(5) . . . . ? C10 C11 C12 C7 0.8(11) . . . . ? C1 P1 C13 C14 -156.6(5) . . . . ? C7 P1 C13 C14 -42.1(6) . . . . ? Pt1 P1 C13 C14 90.1(5) . . . . ? C1 P1 C13 C18 29.5(6) . . . . ? C7 P1 C13 C18 144.0(5) . . . . ? Pt1 P1 C13 C18 -83.8(5) . . . . ? C18 C13 C14 C15 -0.1(10) . . . . ? P1 C13 C14 C15 -174.1(5) . . . . ? C13 C14 C15 C16 0.5(11) . . . . ? C14 C15 C16 C17 -0.5(13) . . . . ? C15 C16 C17 C18 0.1(13) . . . . ? C16 C17 C18 C13 0.3(13) . . . . ? C14 C13 C18 C17 -0.3(10) . . . . ? P1 C13 C18 C17 173.8(6) . . . . ? N2 Pt1 P2 C19 -9.6(16) . . . . ? N20 Pt1 P2 C19 0.5(3) . . . . ? P1 Pt1 P2 C19 179.1(2) . . . . ? N2 Pt1 P2 C25 -125.0(16) . . . . ? N20 Pt1 P2 C25 -114.9(3) . . . . ? P1 Pt1 P2 C25 63.7(2) . . . . ? N2 Pt1 P2 C31 103.6(16) . . . . ? N20 Pt1 P2 C31 113.6(3) . . . . ? P1 Pt1 P2 C31 -67.8(2) . . . . ? C25 P2 C19 C24 -53.3(6) . . . . ? C31 P2 C19 C24 58.9(6) . . . . ? Pt1 P2 C19 C24 -178.8(5) . . . . ? C25 P2 C19 C20 129.9(5) . . . . ? C31 P2 C19 C20 -117.9(5) . . . . ? Pt1 P2 C19 C20 4.4(5) . . . . ? C24 C19 C20 C21 -2.5(9) . . . . ? P2 C19 C20 C21 174.5(5) . . . . ? C24 C19 C20 N20 173.8(6) . . . . ? P2 C19 C20 N20 -9.2(8) . . . . ? C21 C20 N20 Pt1 -173.9(5) . . . . ? C19 C20 N20 Pt1 9.8(7) . . . . ? N2 Pt1 N20 C20 173.7(4) . . . . ? P1 Pt1 N20 C20 -174.5(9) . . . . ? P2 Pt1 N20 C20 -5.2(4) . . . . ? C19 C20 C21 C22 1.3(10) . . . . ? N20 C20 C21 C22 -174.9(6) . . . . ? C20 C21 C22 C23 1.7(12) . . . . ? C21 C22 C23 C24 -3.5(12) . . . . ? C22 C23 C24 C19 2.3(11) . . . . ? C20 C19 C24 C23 0.6(10) . . . . ? P2 C19 C24 C23 -176.1(5) . . . . ? C19 P2 C25 C30 -90.8(5) . . . . ? C31 P2 C25 C30 159.0(5) . . . . ? Pt1 P2 C25 C30 23.3(6) . . . . ? C19 P2 C25 C26 84.7(6) . . . . ? C31 P2 C25 C26 -25.6(6) . . . . ? Pt1 P2 C25 C26 -161.3(5) . . . . ? C30 C25 C26 C27 -0.7(11) . . . . ? P2 C25 C26 C27 -176.2(6) . . . . ? C25 C26 C27 C28 0.1(13) . . . . ? C26 C27 C28 C29 1.3(15) . . . . ? C27 C28 C29 C30 -2.0(14) . . . . ? C28 C29 C30 C25 1.4(12) . . . . ? C26 C25 C30 C29 -0.1(10) . . . . ? P2 C25 C30 C29 175.6(6) . . . . ? C19 P2 C31 C36 30.5(6) . . . . ? C25 P2 C31 C36 141.4(5) . . . . ? Pt1 P2 C31 C36 -81.6(5) . . . . ? C19 P2 C31 C32 -156.0(5) . . . . ? C25 P2 C31 C32 -45.1(6) . . . . ? Pt1 P2 C31 C32 91.9(5) . . . . ? C36 C31 C32 C33 -0.4(9) . . . . ? P2 C31 C32 C33 -173.9(5) . . . . ? C31 C32 C33 C34 -0.3(10) . . . . ? C32 C33 C34 C35 0.6(11) . . . . ? C33 C34 C35 C36 -0.3(11) . . . . ? C32 C31 C36 C35 0.7(9) . . . . ? P2 C31 C36 C35 174.4(5) . . . . ? C34 C35 C36 C31 -0.4(10) . . . . ? C43 P3 N3 P4 90.9(9) . . . . ? C37 P3 N3 P4 -157.7(8) . . . . ? Se3 P3 N3 P4 -34.0(10) . . . . ? P3 N3 P4 O4 9.1(10) . . . . ? P3 N3 P4 C55 133.2(8) . . . . ? P3 N3 P4 C49 -115.1(8) . . . . ? N3 P3 C37 C42 142.8(6) . . . . ? C43 P3 C37 C42 -101.8(6) . . . . ? Se3 P3 C37 C42 13.0(6) . . . . ? N3 P3 C37 C38 -36.8(7) . . . . ? C43 P3 C37 C38 78.7(6) . . . . ? Se3 P3 C37 C38 -166.6(5) . . . . ? C42 C37 C38 C39 -0.1(12) . . . . ? P3 C37 C38 C39 179.5(7) . . . . ? C37 C38 C39 C40 -1.0(16) . . . . ? C38 C39 C40 C41 1.5(20) . . . . ? C39 C40 C41 C42 -0.9(20) . . . . ? C38 C37 C42 C41 0.7(12) . . . . ? P3 C37 C42 C41 -178.9(7) . . . . ? C40 C41 C42 C37 -0.3(16) . . . . ? N3 P3 C43 C44 142.9(5) . . . . ? C37 P3 C43 C44 30.5(6) . . . . ? Se3 P3 C43 C44 -85.6(6) . . . . ? N3 P3 C43 C48 -40.3(6) . . . . ? C37 P3 C43 C48 -152.7(6) . . . . ? Se3 P3 C43 C48 91.2(6) . . . . ? C48 C43 C44 C45 2.4(11) . . . . ? P3 C43 C44 C45 179.2(6) . . . . ? C43 C44 C45 C46 -1.9(11) . . . . ? C44 C45 C46 C47 0.6(12) . . . . ? C45 C46 C47 C48 0.1(13) . . . . ? C46 C47 C48 C43 0.4(13) . . . . ? C44 C43 C48 C47 -1.7(11) . . . . ? P3 C43 C48 C47 -178.6(6) . . . . ? O4 P4 C49 C54 -158.3(6) . . . . ? N3 P4 C49 C54 -26.6(7) . . . . ? C55 P4 C49 C54 86.5(7) . . . . ? O4 P4 C49 C50 23.1(6) . . . . ? N3 P4 C49 C50 154.8(5) . . . . ? C55 P4 C49 C50 -92.1(6) . . . . ? C54 C49 C50 C51 1.0(11) . . . . ? P4 C49 C50 C51 179.7(6) . . . . ? C49 C50 C51 C52 -0.5(12) . . . . ? C50 C51 C52 C53 -0.4(14) . . . . ? C51 C52 C53 C54 0.9(15) . . . . ? C50 C49 C54 C53 -0.5(12) . . . . ? P4 C49 C54 C53 -179.2(7) . . . . ? C52 C53 C54 C49 -0.4(15) . . . . ? O4 P4 C55 C60 -30.9(8) . . . . ? N3 P4 C55 C60 -162.1(7) . . . . ? C49 P4 C55 C60 83.6(8) . . . . ? O4 P4 C55 C56 147.7(7) . . . . ? N3 P4 C55 C56 16.5(8) . . . . ? C49 P4 C55 C56 -97.8(7) . . . . ? C60 C55 C56 C57 -3.9(14) . . . . ? P4 C55 C56 C57 177.4(8) . . . . ? C55 C56 C57 C58 1.3(19) . . . . ? C56 C57 C58 C59 1.1(22) . . . . ? C57 C58 C59 C60 -1.0(23) . . . . ? C56 C55 C60 C59 4.0(15) . . . . ? P4 C55 C60 C59 -177.3(9) . . . . ? C58 C59 C60 C55 -1.7(20) . . . . ? _refine_diff_density_max 1.113 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.100 #end data_6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C42 H35 N2 O P3 Pd S' _chemical_formula_structural 'C42 H35 N2 O P3 Pd S' _chemical_formula_analytical 'C42 H35 N2 O P3 Pd S' _chemical_formula_sum 'C42 H35 N2 O P3 Pd S' _chemical_formula_weight 815.09 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8531(3) _cell_length_b 13.4561(4) _cell_length_c 15.5289(5) _cell_angle_alpha 102.9820(10) _cell_angle_beta 94.7740(10) _cell_angle_gamma 110.6100(10) _cell_volume 1847.89(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method - _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.678166 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 8374 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 23.28 _reflns_number_total 5236 _reflns_number_observed 3928 _reflns_observed_criterion 2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.5285P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5186 _refine_ls_number_parameters 456 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_obs 0.0490 _refine_ls_wR_factor_all 0.1452 _refine_ls_wR_factor_obs 0.1157 _refine_ls_goodness_of_fit_all 0.950 _refine_ls_goodness_of_fit_obs 0.993 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 0.994 _refine_ls_shift/esd_max -0.136 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 1.05075(5) 0.22019(3) 1.26840(3) 0.0354(2) Uani 1 d . . S1 S 1.3071(2) 0.27753(12) 1.30916(11) 0.0449(4) Uani 1 d . . P1 P 1.3927(2) 0.39554(12) 1.24556(10) 0.0383(4) Uani 1 d . . C1 C 1.5694(6) 0.4896(5) 1.3124(4) 0.0376(14) Uani 1 d . . N1 N 1.2953(5) 0.4618(4) 1.2211(3) 0.0457(12) Uani 1 d . . P2 P 1.1609(2) 0.47719(12) 1.26605(11) 0.0414(4) Uani 1 d . . O2 O 1.0444(4) 0.3764(3) 1.2786(3) 0.0523(11) Uani 1 d . . C2 C 1.6680(7) 0.5583(6) 1.2714(5) 0.059(2) Uani 1 d . . H2A H 1.6464(7) 0.5497(6) 1.2101(5) 0.071 Uiso 1 calc R . P3 P 1.0129(2) 0.04516(12) 1.25126(10) 0.0364(4) Uani 1 d . . C3 C 1.7983(7) 0.6394(6) 1.3221(6) 0.063(2) Uani 1 d . . H3A H 1.8645(7) 0.6850(6) 1.2947(6) 0.076 Uiso 1 calc R . C4 C 1.8297(8) 0.6529(6) 1.4120(5) 0.062(2) Uani 1 d . . H4A H 1.9163(8) 0.7087(6) 1.4458(5) 0.074 Uiso 1 calc R . C5 C 1.7361(8) 0.5857(6) 1.4527(5) 0.068(2) Uani 1 d . . H5A H 1.7594(8) 0.5948(6) 1.5140(5) 0.081 Uiso 1 calc R . C6 C 1.6055(7) 0.5032(5) 1.4032(4) 0.055(2) Uani 1 d . . H6A H 1.5420(7) 0.4568(5) 1.4313(4) 0.066 Uiso 1 calc R . C7 C 1.4398(6) 0.3364(5) 1.1419(4) 0.046(2) Uani 1 d . . C8 C 1.4034(7) 0.3585(6) 1.0642(5) 0.068(2) Uani 1 d . . H8A H 1.3514(7) 0.4041(6) 1.0628(5) 0.082 Uiso 1 calc R . C9 C 1.4461(10) 0.3107(9) 0.9844(5) 0.095(3) Uani 1 d . . H9A H 1.4236(10) 0.3265(9) 0.9310(5) 0.115 Uiso 1 calc R . C10 C 1.5196(10) 0.2424(9) 0.9865(7) 0.097(3) Uani 1 d . . H10A H 1.5430(10) 0.2091(9) 0.9338(7) 0.117 Uiso 1 calc R . C11 C 1.5591(10) 0.2221(7) 1.0645(7) 0.088(3) Uani 1 d . . H11A H 1.6135(10) 0.1781(7) 1.0660(7) 0.106 Uiso 1 calc R . C12 C 1.5175(8) 0.2677(6) 1.1419(5) 0.069(2) Uani 1 d . . H12A H 1.5419(8) 0.2521(6) 1.1951(5) 0.083 Uiso 1 calc R . C13 C 1.0776(6) 0.5332(5) 1.1919(4) 0.0413(14) Uani 1 d . . C14 C 1.1528(8) 0.6317(6) 1.1756(5) 0.065(2) Uani 1 d . . H14A H 1.2496(8) 0.6729(6) 1.2047(5) 0.078 Uiso 1 calc R . C15 C 1.0870(9) 0.6709(6) 1.1165(5) 0.076(2) Uani 1 d . . H15A H 1.1403(9) 0.7377(6) 1.1054(5) 0.092 Uiso 1 calc R . C16 C 0.9457(9) 0.6132(7) 1.0745(5) 0.072(2) Uani 1 d . . H16A H 0.9012(9) 0.6406(7) 1.0354(5) 0.087 Uiso 1 calc R . C17 C 0.8690(8) 0.5148(8) 1.0897(6) 0.079(2) Uani 1 d . . H17A H 0.7728(8) 0.4742(8) 1.0594(6) 0.095 Uiso 1 calc R . C18 C 0.9312(7) 0.4746(6) 1.1488(5) 0.064(2) Uani 1 d . . H18A H 0.8762(7) 0.4084(6) 1.1603(5) 0.077 Uiso 1 calc R . C19 C 1.2265(7) 0.5795(5) 1.3733(4) 0.0441(15) Uani 1 d . . C20 C 1.3704(8) 0.6545(5) 1.3986(5) 0.056(2) Uani 1 d . . H20A H 1.4356(8) 0.6546(5) 1.3586(5) 0.068 Uiso 1 calc R . C21 C 1.4196(8) 0.7303(6) 1.4836(5) 0.070(2) Uani 1 d . . H21A H 1.5178(8) 0.7783(6) 1.5014(5) 0.084 Uiso 1 calc R . C22 C 1.3204(10) 0.7327(7) 1.5401(5) 0.073(2) Uani 1 d . . H22A H 1.3513(10) 0.7849(7) 1.5957(5) 0.087 Uiso 1 calc R . C23 C 1.1767(10) 0.6597(7) 1.5164(5) 0.079(2) Uani 1 d . . H23A H 1.1113(10) 0.6614(7) 1.5560(5) 0.095 Uiso 1 calc R . C24 C 1.1303(8) 0.5843(6) 1.4340(5) 0.061(2) Uani 1 d . . H24A H 1.0326(8) 0.5351(6) 1.4179(5) 0.073 Uiso 1 calc R . C25 C 0.8169(6) -0.0145(5) 1.2484(4) 0.0407(14) Uani 1 d . . N26 N 0.8302(5) 0.1638(4) 1.2478(3) 0.0482(13) Uani 1 d D . H26A H 0.7720(51) 0.2065(38) 1.2491(37) 0.045(17) Uiso 1 d D . C26 C 0.7469(6) 0.0596(5) 1.2483(4) 0.0411(14) Uani 1 d . . C27 C 0.5956(7) 0.0211(5) 1.2493(4) 0.054(2) Uani 1 d . . H27A H 0.5456(7) 0.0677(5) 1.2465(4) 0.065 Uiso 1 calc R . C28 C 0.5194(8) -0.0845(7) 1.2543(5) 0.064(2) Uani 1 d . . H28A H 0.4195(8) -0.1072(7) 1.2572(5) 0.077 Uiso 1 calc R . C29 C 0.5898(7) -0.1571(6) 1.2550(4) 0.058(2) Uani 1 d . . H29A H 0.5376(7) -0.2285(6) 1.2578(4) 0.070 Uiso 1 calc R . C30 C 0.7392(7) -0.1224(5) 1.2514(4) 0.051(2) Uani 1 d . . H30A H 0.7873(7) -0.1708(5) 1.2511(4) 0.062 Uiso 1 calc R . C31 C 1.0550(6) -0.0227(4) 1.1477(4) 0.0368(13) Uani 1 d . . C32 C 0.9447(7) -0.0957(5) 1.0765(4) 0.046(2) Uani 1 d . . H32A H 0.8461(7) -0.1148(5) 1.0821(4) 0.055 Uiso 1 calc R . C33 C 0.9829(8) -0.1401(5) 0.9965(4) 0.052(2) Uani 1 d . . H33A H 0.9091(8) -0.1883(5) 0.9485(4) 0.063 Uiso 1 calc R . C34 C 1.1265(8) -0.1138(5) 0.9878(4) 0.056(2) Uani 1 d . . H34A H 1.1505(8) -0.1446(5) 0.9343(4) 0.067 Uiso 1 calc R . C35 C 1.2370(8) -0.0414(6) 1.0584(5) 0.059(2) Uani 1 d . . H35A H 1.3352(8) -0.0232(6) 1.0520(5) 0.070 Uiso 1 calc R . C36 C 1.2024(7) 0.0040(5) 1.1384(4) 0.050(2) Uani 1 d . . H36A H 1.2771(7) 0.0523(5) 1.1859(4) 0.060 Uiso 1 calc R . C37 C 1.1047(6) 0.0128(5) 1.3412(4) 0.0374(13) Uani 1 d . . C38 C 1.1389(7) 0.0819(5) 1.4266(4) 0.053(2) Uani 1 d . . H38A H 1.1213(7) 0.1468(5) 1.4364(4) 0.063 Uiso 1 calc R . C39 C 1.1986(9) 0.0565(7) 1.4976(5) 0.074(2) Uani 1 d . . H39A H 1.2206(9) 0.1039(7) 1.5551(5) 0.089 Uiso 1 calc R . C40 C 1.2256(8) -0.0378(7) 1.4842(5) 0.075(2) Uani 1 d . . H40A H 1.2666(8) -0.0546(7) 1.5324(5) 0.090 Uiso 1 calc R . C41 C 1.1924(8) -0.1075(7) 1.4000(6) 0.075(2) Uani 1 d . . H41A H 1.2101(8) -0.1722(7) 1.3913(6) 0.090 Uiso 1 calc R . C42 C 1.1327(7) -0.0835(5) 1.3273(5) 0.057(2) Uani 1 d . . H42A H 1.1115(7) -0.1310(5) 1.2699(5) 0.069 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0355(3) 0.0357(3) 0.0414(3) 0.0144(2) 0.0084(2) 0.0186(2) S1 0.0383(9) 0.0453(9) 0.0579(10) 0.0220(8) 0.0066(7) 0.0193(7) P1 0.0351(9) 0.0420(9) 0.0440(9) 0.0141(7) 0.0094(7) 0.0200(7) C1 0.036(3) 0.043(3) 0.043(3) 0.017(3) 0.010(3) 0.022(3) N1 0.041(3) 0.053(3) 0.058(3) 0.030(3) 0.017(2) 0.024(3) P2 0.0379(9) 0.0384(9) 0.0586(10) 0.0215(8) 0.0116(7) 0.0215(8) O2 0.050(3) 0.037(2) 0.087(3) 0.028(2) 0.026(2) 0.027(2) C2 0.047(4) 0.060(4) 0.061(4) 0.015(4) 0.006(3) 0.012(4) P3 0.0377(9) 0.0357(8) 0.0394(9) 0.0129(7) 0.0061(7) 0.0169(7) C3 0.048(4) 0.050(4) 0.088(6) 0.022(4) 0.014(4) 0.012(4) C4 0.050(4) 0.047(4) 0.078(6) -0.002(4) -0.004(4) 0.020(4) C5 0.061(5) 0.082(6) 0.053(4) 0.007(4) -0.002(4) 0.029(4) C6 0.059(4) 0.058(4) 0.049(4) 0.015(3) 0.011(3) 0.023(4) C7 0.033(3) 0.051(4) 0.048(4) 0.010(3) 0.007(3) 0.011(3) C8 0.047(4) 0.103(6) 0.050(4) 0.011(4) 0.000(3) 0.033(4) C9 0.080(6) 0.134(8) 0.047(5) 0.013(5) 0.001(4) 0.020(6) C10 0.075(6) 0.115(8) 0.074(7) -0.019(6) 0.014(5) 0.029(6) C11 0.088(6) 0.082(6) 0.092(7) -0.003(5) 0.034(5) 0.042(5) C12 0.076(5) 0.067(5) 0.078(5) 0.015(4) 0.026(4) 0.044(4) C13 0.039(4) 0.044(4) 0.045(4) 0.013(3) 0.008(3) 0.020(3) C14 0.051(4) 0.053(4) 0.088(5) 0.034(4) -0.012(4) 0.013(4) C15 0.082(6) 0.065(5) 0.086(6) 0.042(4) -0.006(5) 0.024(4) C16 0.075(6) 0.089(6) 0.070(5) 0.030(5) -0.001(4) 0.049(5) C17 0.049(5) 0.098(7) 0.092(6) 0.032(5) -0.007(4) 0.029(5) C18 0.044(4) 0.065(5) 0.092(6) 0.035(4) 0.003(4) 0.022(4) C19 0.044(4) 0.045(4) 0.060(4) 0.027(3) 0.013(3) 0.028(3) C20 0.059(5) 0.059(4) 0.059(4) 0.021(4) 0.010(3) 0.029(4) C21 0.059(5) 0.070(5) 0.075(5) 0.014(4) -0.002(4) 0.025(4) C22 0.092(6) 0.076(5) 0.053(5) 0.001(4) -0.005(4) 0.050(5) C23 0.094(7) 0.104(7) 0.062(5) 0.025(5) 0.025(5) 0.061(6) C24 0.054(4) 0.081(5) 0.063(5) 0.025(4) 0.017(4) 0.038(4) C25 0.036(3) 0.040(4) 0.041(3) 0.012(3) 0.008(3) 0.008(3) N26 0.039(3) 0.047(3) 0.058(3) 0.009(3) 0.004(2) 0.020(3) C26 0.028(3) 0.046(4) 0.048(4) 0.011(3) 0.003(3) 0.015(3) C27 0.041(4) 0.053(4) 0.069(5) 0.011(3) 0.013(3) 0.022(3) C28 0.039(4) 0.082(6) 0.064(5) 0.017(4) 0.008(3) 0.017(4) C29 0.045(4) 0.057(4) 0.057(4) 0.022(3) 0.005(3) -0.001(4) C30 0.054(4) 0.053(4) 0.051(4) 0.021(3) 0.005(3) 0.023(3) C31 0.046(4) 0.029(3) 0.046(3) 0.020(3) 0.014(3) 0.021(3) C32 0.042(4) 0.045(4) 0.050(4) 0.016(3) 0.001(3) 0.015(3) C33 0.072(5) 0.046(4) 0.038(4) 0.011(3) 0.001(3) 0.023(4) C34 0.076(5) 0.053(4) 0.050(4) 0.011(3) 0.017(4) 0.038(4) C35 0.059(4) 0.070(5) 0.062(5) 0.015(4) 0.023(4) 0.041(4) C36 0.044(4) 0.055(4) 0.053(4) 0.013(3) 0.005(3) 0.025(3) C37 0.040(3) 0.044(3) 0.037(3) 0.020(3) 0.008(3) 0.020(3) C38 0.067(5) 0.052(4) 0.044(4) 0.021(3) 0.005(3) 0.025(3) C39 0.085(6) 0.080(6) 0.045(4) 0.017(4) -0.002(4) 0.021(5) C40 0.075(6) 0.100(6) 0.066(5) 0.048(5) 0.007(4) 0.038(5) C41 0.078(6) 0.087(6) 0.091(6) 0.049(5) 0.021(5) 0.052(5) C42 0.073(5) 0.064(4) 0.054(4) 0.025(3) 0.012(3) 0.042(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N26 2.003(5) . ? Pd1 O2 2.096(4) . ? Pd1 P3 2.200(2) . ? Pd1 S1 2.350(2) . ? S1 P1 2.027(2) . ? P1 N1 1.598(5) . ? P1 C7 1.803(6) . ? P1 C1 1.808(6) . ? C1 C2 1.392(9) . ? C1 C6 1.380(8) . ? N1 P2 1.602(5) . ? P2 O2 1.502(4) . ? P2 C13 1.799(6) . ? P2 C19 1.803(6) . ? C2 C3 1.386(9) . ? P3 C25 1.804(6) . ? P3 C37 1.817(5) . ? P3 C31 1.820(6) . ? C3 C4 1.361(10) . ? C4 C5 1.354(10) . ? C5 C6 1.387(9) . ? C7 C8 1.355(9) . ? C7 C12 1.392(9) . ? C8 C9 1.430(11) . ? C9 C10 1.360(13) . ? C10 C11 1.355(13) . ? C11 C12 1.386(10) . ? C13 C14 1.364(9) . ? C13 C18 1.397(9) . ? C14 C15 1.379(9) . ? C15 C16 1.352(10) . ? C16 C17 1.358(11) . ? C17 C18 1.370(10) . ? C19 C20 1.380(9) . ? C19 C24 1.399(9) . ? C20 C21 1.399(9) . ? C21 C22 1.371(11) . ? C22 C23 1.370(11) . ? C23 C24 1.367(10) . ? C25 C26 1.398(8) . ? C25 C30 1.396(8) . ? N26 C26 1.356(7) . ? C26 C27 1.398(8) . ? C27 C28 1.377(10) . ? C28 C29 1.386(10) . ? C29 C30 1.388(9) . ? C31 C32 1.389(8) . ? C31 C36 1.397(8) . ? C32 C33 1.394(9) . ? C33 C34 1.359(9) . ? C34 C35 1.382(9) . ? C35 C36 1.382(8) . ? C37 C38 1.375(8) . ? C37 C42 1.391(8) . ? C38 C39 1.371(10) . ? C39 C40 1.362(11) . ? C40 C41 1.364(11) . ? C41 C42 1.383(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N26 Pd1 O2 86.1(2) . . ? N26 Pd1 P3 83.4(2) . . ? O2 Pd1 P3 169.42(12) . . ? N26 Pd1 S1 172.5(2) . . ? O2 Pd1 S1 97.52(12) . . ? P3 Pd1 S1 93.06(5) . . ? P1 S1 Pd1 104.56(7) . . ? N1 P1 C7 106.5(3) . . ? N1 P1 C1 110.6(3) . . ? C7 P1 C1 103.3(3) . . ? N1 P1 S1 118.3(2) . . ? C7 P1 S1 109.9(2) . . ? C1 P1 S1 107.2(2) . . ? C2 C1 C6 118.7(6) . . ? C2 C1 P1 117.8(4) . . ? C6 C1 P1 123.2(5) . . ? P2 N1 P1 127.8(3) . . ? O2 P2 N1 117.7(2) . . ? O2 P2 C13 108.9(3) . . ? N1 P2 C13 104.2(3) . . ? O2 P2 C19 107.7(3) . . ? N1 P2 C19 111.0(3) . . ? C13 P2 C19 106.7(3) . . ? P2 O2 Pd1 128.4(2) . . ? C1 C2 C3 119.9(7) . . ? C25 P3 C37 108.2(3) . . ? C25 P3 C31 108.8(3) . . ? C37 P3 C31 106.1(2) . . ? C25 P3 Pd1 101.7(2) . . ? C37 P3 Pd1 116.5(2) . . ? C31 P3 Pd1 115.2(2) . . ? C4 C3 C2 120.3(7) . . ? C3 C4 C5 120.6(7) . . ? C4 C5 C6 120.2(7) . . ? C5 C6 C1 120.3(7) . . ? C8 C7 C12 119.2(6) . . ? C8 C7 P1 121.6(5) . . ? C12 C7 P1 119.1(5) . . ? C7 C8 C9 119.1(7) . . ? C10 C9 C8 120.2(8) . . ? C11 C10 C9 120.9(8) . . ? C10 C11 C12 119.1(9) . . ? C11 C12 C7 121.4(8) . . ? C14 C13 C18 118.3(6) . . ? C14 C13 P2 122.2(5) . . ? C18 C13 P2 119.5(5) . . ? C13 C14 C15 120.8(6) . . ? C16 C15 C14 120.6(7) . . ? C15 C16 C17 119.5(7) . . ? C16 C17 C18 121.1(7) . . ? C13 C18 C17 119.7(7) . . ? C20 C19 C24 117.9(6) . . ? C20 C19 P2 122.2(5) . . ? C24 C19 P2 119.9(5) . . ? C21 C20 C19 120.9(7) . . ? C20 C21 C22 118.8(7) . . ? C23 C22 C21 121.3(7) . . ? C24 C23 C22 119.4(7) . . ? C23 C24 C19 121.5(7) . . ? C26 C25 C30 121.2(6) . . ? C26 C25 P3 113.9(4) . . ? C30 C25 P3 124.8(5) . . ? C26 N26 Pd1 121.9(4) . . ? N26 C26 C27 124.4(6) . . ? N26 C26 C25 117.9(5) . . ? C27 C26 C25 117.7(6) . . ? C28 C27 C26 121.2(6) . . ? C27 C28 C29 120.7(6) . . ? C30 C29 C28 119.4(7) . . ? C29 C30 C25 119.7(6) . . ? C32 C31 C36 119.5(5) . . ? C32 C31 P3 121.7(5) . . ? C36 C31 P3 118.7(4) . . ? C31 C32 C33 119.5(6) . . ? C34 C33 C32 120.8(6) . . ? C33 C34 C35 120.1(6) . . ? C34 C35 C36 120.3(6) . . ? C35 C36 C31 119.8(6) . . ? C38 C37 C42 119.1(5) . . ? C38 C37 P3 118.9(4) . . ? C42 C37 P3 121.9(5) . . ? C37 C38 C39 120.8(7) . . ? C40 C39 C38 120.2(7) . . ? C39 C40 C41 119.9(7) . . ? C40 C41 C42 121.0(7) . . ? C37 C42 C41 119.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N26 Pd1 S1 P1 -159.5(11) . . . . ? O2 Pd1 S1 P1 -41.07(14) . . . . ? P3 Pd1 S1 P1 139.23(8) . . . . ? Pd1 S1 P1 N1 25.6(2) . . . . ? Pd1 S1 P1 C7 -96.9(2) . . . . ? Pd1 S1 P1 C1 151.4(2) . . . . ? N1 P1 C1 C2 -67.8(5) . . . . ? C7 P1 C1 C2 45.8(5) . . . . ? S1 P1 C1 C2 161.8(4) . . . . ? N1 P1 C1 C6 106.2(5) . . . . ? C7 P1 C1 C6 -140.2(5) . . . . ? S1 P1 C1 C6 -24.1(5) . . . . ? C7 P1 N1 P2 145.8(4) . . . . ? C1 P1 N1 P2 -102.6(4) . . . . ? S1 P1 N1 P2 21.6(5) . . . . ? P1 N1 P2 O2 -47.3(5) . . . . ? P1 N1 P2 C13 -167.9(4) . . . . ? P1 N1 P2 C19 77.5(5) . . . . ? N1 P2 O2 Pd1 13.0(5) . . . . ? C13 P2 O2 Pd1 131.2(3) . . . . ? C19 P2 O2 Pd1 -113.4(3) . . . . ? N26 Pd1 O2 P2 -158.3(4) . . . . ? P3 Pd1 O2 P2 -153.3(5) . . . . ? S1 Pd1 O2 P2 28.3(3) . . . . ? C6 C1 C2 C3 -1.0(9) . . . . ? P1 C1 C2 C3 173.3(5) . . . . ? N26 Pd1 P3 C25 -8.1(2) . . . . ? O2 Pd1 P3 C25 -13.1(7) . . . . ? S1 Pd1 P3 C25 165.3(2) . . . . ? N26 Pd1 P3 C37 -125.5(3) . . . . ? O2 Pd1 P3 C37 -130.5(7) . . . . ? S1 Pd1 P3 C37 47.9(2) . . . . ? N26 Pd1 P3 C31 109.3(3) . . . . ? O2 Pd1 P3 C31 104.3(7) . . . . ? S1 Pd1 P3 C31 -77.3(2) . . . . ? C1 C2 C3 C4 -0.5(10) . . . . ? C2 C3 C4 C5 1.5(11) . . . . ? C3 C4 C5 C6 -1.0(11) . . . . ? C4 C5 C6 C1 -0.6(10) . . . . ? C2 C1 C6 C5 1.5(9) . . . . ? P1 C1 C6 C5 -172.4(5) . . . . ? N1 P1 C7 C8 5.0(6) . . . . ? C1 P1 C7 C8 -111.6(6) . . . . ? S1 P1 C7 C8 134.3(5) . . . . ? N1 P1 C7 C12 -176.0(5) . . . . ? C1 P1 C7 C12 67.4(6) . . . . ? S1 P1 C7 C12 -46.7(6) . . . . ? C12 C7 C8 C9 -0.1(10) . . . . ? P1 C7 C8 C9 178.9(6) . . . . ? C7 C8 C9 C10 1.3(12) . . . . ? C8 C9 C10 C11 -2.9(15) . . . . ? C9 C10 C11 C12 3.1(14) . . . . ? C10 C11 C12 C7 -1.9(13) . . . . ? C8 C7 C12 C11 0.4(11) . . . . ? P1 C7 C12 C11 -178.6(6) . . . . ? O2 P2 C13 C14 172.7(5) . . . . ? N1 P2 C13 C14 -60.9(6) . . . . ? C19 P2 C13 C14 56.7(6) . . . . ? O2 P2 C13 C18 -7.5(6) . . . . ? N1 P2 C13 C18 118.9(5) . . . . ? C19 P2 C13 C18 -123.5(5) . . . . ? C18 C13 C14 C15 -1.6(11) . . . . ? P2 C13 C14 C15 178.2(6) . . . . ? C13 C14 C15 C16 1.0(13) . . . . ? C14 C15 C16 C17 -1.1(13) . . . . ? C15 C16 C17 C18 1.8(13) . . . . ? C14 C13 C18 C17 2.2(11) . . . . ? P2 C13 C18 C17 -177.5(6) . . . . ? C16 C17 C18 C13 -2.4(13) . . . . ? O2 P2 C19 C20 147.5(5) . . . . ? N1 P2 C19 C20 17.3(6) . . . . ? C13 P2 C19 C20 -95.7(5) . . . . ? O2 P2 C19 C24 -32.4(5) . . . . ? N1 P2 C19 C24 -162.6(5) . . . . ? C13 P2 C19 C24 84.4(5) . . . . ? C24 C19 C20 C21 2.2(9) . . . . ? P2 C19 C20 C21 -177.6(5) . . . . ? C19 C20 C21 C22 -3.2(10) . . . . ? C20 C21 C22 C23 2.7(11) . . . . ? C21 C22 C23 C24 -1.4(12) . . . . ? C22 C23 C24 C19 0.4(11) . . . . ? C20 C19 C24 C23 -0.8(10) . . . . ? P2 C19 C24 C23 179.0(5) . . . . ? C37 P3 C25 C26 129.2(4) . . . . ? C31 P3 C25 C26 -115.9(4) . . . . ? Pd1 P3 C25 C26 6.0(5) . . . . ? C37 P3 C25 C30 -47.0(6) . . . . ? C31 P3 C25 C30 67.8(6) . . . . ? Pd1 P3 C25 C30 -170.3(5) . . . . ? O2 Pd1 N26 C26 -169.3(5) . . . . ? P3 Pd1 N26 C26 11.6(4) . . . . ? S1 Pd1 N26 C26 -50.2(14) . . . . ? Pd1 N26 C26 C27 168.9(5) . . . . ? Pd1 N26 C26 C25 -10.7(7) . . . . ? C30 C25 C26 N26 178.2(5) . . . . ? P3 C25 C26 N26 1.8(7) . . . . ? C30 C25 C26 C27 -1.4(9) . . . . ? P3 C25 C26 C27 -177.9(5) . . . . ? N26 C26 C27 C28 -176.7(6) . . . . ? C25 C26 C27 C28 2.9(9) . . . . ? C26 C27 C28 C29 -2.5(10) . . . . ? C27 C28 C29 C30 0.6(10) . . . . ? C28 C29 C30 C25 0.9(9) . . . . ? C26 C25 C30 C29 -0.4(9) . . . . ? P3 C25 C30 C29 175.6(5) . . . . ? C25 P3 C31 C32 8.6(5) . . . . ? C37 P3 C31 C32 124.8(5) . . . . ? Pd1 P3 C31 C32 -104.7(4) . . . . ? C25 P3 C31 C36 -174.7(4) . . . . ? C37 P3 C31 C36 -58.5(5) . . . . ? Pd1 P3 C31 C36 72.0(5) . . . . ? C36 C31 C32 C33 -0.7(8) . . . . ? P3 C31 C32 C33 175.9(4) . . . . ? C31 C32 C33 C34 0.8(9) . . . . ? C32 C33 C34 C35 -0.7(10) . . . . ? C33 C34 C35 C36 0.6(10) . . . . ? C34 C35 C36 C31 -0.5(10) . . . . ? C32 C31 C36 C35 0.6(9) . . . . ? P3 C31 C36 C35 -176.2(5) . . . . ? C25 P3 C37 C38 -87.0(5) . . . . ? C31 P3 C37 C38 156.5(5) . . . . ? Pd1 P3 C37 C38 26.8(6) . . . . ? C25 P3 C37 C42 88.7(6) . . . . ? C31 P3 C37 C42 -27.8(6) . . . . ? Pd1 P3 C37 C42 -157.6(5) . . . . ? C42 C37 C38 C39 -0.5(10) . . . . ? P3 C37 C38 C39 175.3(6) . . . . ? C37 C38 C39 C40 0.3(12) . . . . ? C38 C39 C40 C41 -0.4(13) . . . . ? C39 C40 C41 C42 0.7(12) . . . . ? C38 C37 C42 C41 0.8(10) . . . . ? P3 C37 C42 C41 -174.9(5) . . . . ? C40 C41 C42 C37 -0.8(11) . . . . ? _refine_diff_density_max 1.044 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.088 #end data_7 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C42 H36 Au N2 O P3 S' _chemical_formula_structural 'C42 H36 Au N2 O P3 S' _chemical_formula_analytical 'C42 H36 Au N2 O P3 S' _chemical_formula_sum 'C42 H36 Au N2 O P3 S' _chemical_formula_weight 906.66 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0446(3) _cell_length_b 11.5989(3) _cell_length_c 19.1145(6) _cell_angle_alpha 91.8030(10) _cell_angle_beta 95.2790(10) _cell_angle_gamma 104.4790(10) _cell_volume 1930.24(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max .17 _exptl_crystal_size_mid .17 _exptl_crystal_size_min .17 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method - _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 4.024 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.401105 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 6880 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.16 _reflns_number_total 5133 _reflns_number_observed 4439 _reflns_observed_criterion 2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5083 _refine_ls_number_parameters 460 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_obs 0.0413 _refine_ls_wR_factor_all 0.1229 _refine_ls_wR_factor_obs 0.1006 _refine_ls_goodness_of_fit_all 0.905 _refine_ls_goodness_of_fit_obs 0.930 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 0.930 _refine_ls_shift/esd_max -0.061 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au1 Au 0.66251(3) 0.64843(2) 0.701461(14) 0.0417(2) Uani 1 d . . P1 P 0.7643(2) 0.8018(2) 0.63385(9) 0.0373(4) Uani 1 d . . C1 C 0.6484(8) 0.7880(7) 0.5485(4) 0.042(2) Uani 1 d . . C2 C 0.5555(9) 0.6786(7) 0.5238(4) 0.052(2) Uani 1 d . . H2A H 0.5508(9) 0.6125(7) 0.5506(4) 0.063 Uiso 1 calc R . C3 C 0.4685(10) 0.6666(9) 0.4587(4) 0.065(2) Uani 1 d . . H3A H 0.4066(10) 0.5921(9) 0.4425(4) 0.078 Uiso 1 calc R . C4 C 0.4724(11) 0.7609(10) 0.4189(5) 0.068(3) Uani 1 d . . H4A H 0.4138(11) 0.7514(10) 0.3755(5) 0.082 Uiso 1 calc R . C5 C 0.5629(12) 0.8710(10) 0.4426(5) 0.076(3) Uani 1 d . . H5A H 0.5643(12) 0.9357(10) 0.4150(5) 0.091 Uiso 1 calc R . C6 C 0.6535(10) 0.8882(8) 0.5074(4) 0.059(2) Uani 1 d . . H6A H 0.7150(10) 0.9632(8) 0.5229(4) 0.070 Uiso 1 calc R . C7 C 0.7786(8) 0.9521(7) 0.6703(4) 0.042(2) Uani 1 d . . C8 C 0.6592(9) 0.9732(8) 0.7055(4) 0.055(2) Uani 1 d . . H8A H 0.5729(9) 0.9117(8) 0.7101(4) 0.066 Uiso 1 calc R . C9 C 0.6706(12) 1.0898(9) 0.7342(4) 0.066(2) Uani 1 d . . H9A H 0.5924(12) 1.1042(9) 0.7588(4) 0.080 Uiso 1 calc R . C10 C 0.7960(12) 1.1812(8) 0.7260(4) 0.066(2) Uani 1 d . . H10A H 0.8015(12) 1.2575(8) 0.7445(4) 0.079 Uiso 1 calc R . C11 C 0.9139(11) 1.1611(8) 0.6906(5) 0.067(2) Uani 1 d . . H11A H 0.9982(11) 1.2237(8) 0.6848(5) 0.081 Uiso 1 calc R . C12 C 0.9068(10) 1.0478(8) 0.6636(5) 0.059(2) Uani 1 d . . H12A H 0.9878(10) 1.0345(8) 0.6407(5) 0.071 Uiso 1 calc R . C13 C 0.9561(8) 0.7986(6) 0.6136(4) 0.039(2) Uani 1 d . . C14 C 1.0708(8) 0.7922(6) 0.6688(4) 0.042(2) Uani 1 d . . N14 N 1.0482(8) 0.7921(6) 0.7390(3) 0.056(2) Uani 1 d D . H14A H 1.1333(60) 0.7815(74) 0.7717(34) 0.069(25) Uiso 1 d D . H14B H 0.9486(52) 0.7840(92) 0.7573(46) 0.095(34) Uiso 1 d D . C15 C 1.2166(8) 0.7892(7) 0.6501(4) 0.053(2) Uani 1 d . . H15A H 1.2932(8) 0.7851(7) 0.6852(4) 0.064 Uiso 1 calc R . C16 C 1.2487(9) 0.7922(8) 0.5809(5) 0.062(2) Uani 1 d . . H16A H 1.3464(9) 0.7907(8) 0.5701(5) 0.074 Uiso 1 calc R . C17 C 1.1369(9) 0.7974(8) 0.5278(4) 0.058(2) Uani 1 d . . H17A H 1.1588(9) 0.7990(8) 0.4811(4) 0.070 Uiso 1 calc R . C18 C 0.9924(8) 0.8001(7) 0.5444(4) 0.049(2) Uani 1 d . . H18A H 0.9172(8) 0.8031(7) 0.5083(4) 0.059 Uiso 1 calc R . S2 S 0.5895(2) 0.4712(2) 0.75704(10) 0.0496(5) Uani 1 d . . P2 P 0.3749(2) 0.4587(2) 0.78967(9) 0.0395(4) Uani 1 d . . N2 N 0.3581(8) 0.5409(6) 0.8544(3) 0.050(2) Uani 1 d . . P3 P 0.4006(2) 0.6839(2) 0.86844(10) 0.0488(5) Uani 1 d . . O3 O 0.3450(7) 0.7598(5) 0.8145(3) 0.067(2) Uani 1 d . . C19 C 0.2395(8) 0.4673(6) 0.7143(4) 0.041(2) Uani 1 d . . C20 C 0.1005(9) 0.4908(7) 0.7277(4) 0.052(2) Uani 1 d . . H20A H 0.0803(9) 0.5060(7) 0.7734(4) 0.062 Uiso 1 calc R . C21 C -0.0085(10) 0.4909(8) 0.6701(5) 0.065(2) Uani 1 d . . H21A H -0.1008(10) 0.5075(8) 0.6787(5) 0.078 Uiso 1 calc R . C22 C 0.0159(11) 0.4676(8) 0.6026(5) 0.067(3) Uani 1 d . . H22A H -0.0592(11) 0.4663(8) 0.5658(5) 0.080 Uiso 1 calc R . C23 C 0.1577(11) 0.4455(9) 0.5897(5) 0.070(3) Uani 1 d . . H23A H 0.1774(11) 0.4311(9) 0.5438(5) 0.084 Uiso 1 calc R . C24 C 0.2675(9) 0.4452(7) 0.6451(4) 0.052(2) Uani 1 d . . H24A H 0.3605(9) 0.4302(7) 0.6361(4) 0.063 Uiso 1 calc R . C25 C 0.3220(8) 0.3043(7) 0.8147(4) 0.046(2) Uani 1 d . . C26 C 0.3007(13) 0.2771(9) 0.8824(5) 0.085(3) Uani 1 d . . H26A H 0.3090(13) 0.3377(9) 0.9168(5) 0.102 Uiso 1 calc R . C27 C 0.2661(18) 0.1574(12) 0.9004(7) 0.124(5) Uani 1 d . . H27A H 0.2511(18) 0.1387(12) 0.9466(7) 0.149 Uiso 1 calc R . C28 C 0.2545(13) 0.0681(9) 0.8498(7) 0.089(3) Uani 1 d . . H28A H 0.2323(13) -0.0108(9) 0.8623(7) 0.107 Uiso 1 calc R . C29 C 0.2748(11) 0.0926(8) 0.7822(6) 0.075(3) Uani 1 d . . H29A H 0.2653(11) 0.0313(8) 0.7481(6) 0.090 Uiso 1 calc R . C30 C 0.3105(10) 0.2120(7) 0.7642(5) 0.062(2) Uani 1 d . . H30A H 0.3266(10) 0.2300(7) 0.7180(5) 0.075 Uiso 1 calc R . C31 C 0.3292(10) 0.7072(8) 0.9518(4) 0.059(2) Uani 1 d . . C32 C 0.2516(14) 0.6132(11) 0.9877(5) 0.091(3) Uani 1 d . . H32A H 0.2354(14) 0.5350(11) 0.9699(5) 0.110 Uiso 1 calc R . C33 C 0.1968(18) 0.6384(15) 1.0526(6) 0.124(5) Uani 1 d . . H33A H 0.1473(18) 0.5758(15) 1.0781(6) 0.148 Uiso 1 calc R . C34 C 0.2159(20) 0.7521(20) 1.0775(7) 0.140(7) Uani 1 d . . H34A H 0.1751(20) 0.7674(20) 1.1187(7) 0.168 Uiso 1 calc R . C35 C 0.2962(17) 0.8457(15) 1.0418(8) 0.130(6) Uani 1 d . . H35A H 0.3133(17) 0.9237(15) 1.0601(8) 0.156 Uiso 1 calc R . C36 C 0.3500(15) 0.8235(11) 0.9799(6) 0.103(4) Uani 1 d . . H36A H 0.4018(15) 0.8871(11) 0.9558(6) 0.124 Uiso 1 calc R . C37 C 0.6098(9) 0.7370(7) 0.8860(4) 0.051(2) Uani 1 d . . C38 C 0.6957(10) 0.6656(10) 0.9199(5) 0.071(3) Uani 1 d . . H38A H 0.6471(10) 0.5906(10) 0.9338(5) 0.085 Uiso 1 calc R . C39 C 0.8542(13) 0.7082(12) 0.9323(6) 0.097(4) Uani 1 d . . H39A H 0.9118(13) 0.6610(12) 0.9543(6) 0.116 Uiso 1 calc R . C40 C 0.9271(13) 0.8202(13) 0.9123(6) 0.101(4) Uani 1 d . . H40A H 1.0331(13) 0.8485(13) 0.9215(6) 0.121 Uiso 1 calc R . C41 C 0.8431(13) 0.8892(12) 0.8790(6) 0.098(4) Uani 1 d . . H41A H 0.8920(13) 0.9639(12) 0.8649(6) 0.117 Uiso 1 calc R . C42 C 0.6825(11) 0.8469(8) 0.8662(4) 0.064(2) Uani 1 d . . H42A H 0.6255(11) 0.8943(8) 0.8440(4) 0.077 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0397(2) 0.0398(2) 0.0461(2) 0.00762(13) 0.01172(12) 0.00749(14) P1 0.0355(10) 0.0329(10) 0.0434(10) 0.0054(8) 0.0073(8) 0.0067(8) C1 0.042(4) 0.045(5) 0.042(4) -0.003(3) 0.003(3) 0.017(4) C2 0.057(5) 0.046(5) 0.058(5) 0.001(4) 0.008(4) 0.021(4) C3 0.063(5) 0.071(7) 0.062(5) -0.013(5) -0.005(4) 0.025(5) C4 0.071(6) 0.083(8) 0.054(5) -0.012(5) -0.007(4) 0.033(6) C5 0.094(7) 0.078(8) 0.064(6) 0.022(5) -0.002(5) 0.040(6) C6 0.068(5) 0.054(5) 0.054(5) 0.017(4) 0.000(4) 0.015(5) C7 0.042(4) 0.037(5) 0.046(4) 0.001(3) 0.001(3) 0.011(4) C8 0.050(5) 0.055(5) 0.057(5) -0.002(4) 0.009(4) 0.010(4) C9 0.085(7) 0.072(7) 0.055(5) 0.002(5) 0.010(5) 0.041(6) C10 0.097(7) 0.043(6) 0.062(5) -0.001(4) -0.006(5) 0.032(6) C11 0.068(6) 0.040(5) 0.092(7) 0.001(5) 0.005(5) 0.011(5) C12 0.052(5) 0.054(6) 0.073(6) 0.010(4) 0.019(4) 0.013(5) C13 0.036(4) 0.035(4) 0.045(4) 0.007(3) 0.004(3) 0.008(3) C14 0.039(4) 0.035(4) 0.053(4) 0.010(3) 0.006(3) 0.012(3) N14 0.059(4) 0.056(5) 0.052(4) 0.005(3) 0.001(3) 0.016(4) C15 0.035(4) 0.054(5) 0.073(6) 0.005(4) 0.004(4) 0.016(4) C16 0.038(4) 0.065(6) 0.084(6) -0.003(5) 0.016(4) 0.013(4) C17 0.056(5) 0.067(6) 0.051(5) 0.006(4) 0.023(4) 0.009(5) C18 0.043(4) 0.051(5) 0.054(5) 0.002(4) 0.006(4) 0.012(4) S2 0.0446(10) 0.0455(12) 0.0615(12) 0.0173(10) 0.0150(9) 0.0118(10) P2 0.0444(10) 0.0345(11) 0.0395(10) 0.0050(8) 0.0104(8) 0.0074(9) N2 0.061(4) 0.041(4) 0.044(3) -0.003(3) 0.010(3) 0.005(3) P3 0.0632(13) 0.0412(12) 0.0406(10) -0.0012(9) -0.0076(9) 0.0160(11) O3 0.085(4) 0.054(4) 0.055(3) 0.009(3) -0.018(3) 0.015(3) C19 0.046(4) 0.022(4) 0.050(4) -0.005(3) 0.002(3) 0.003(3) C20 0.052(5) 0.043(5) 0.065(5) -0.003(4) 0.010(4) 0.018(4) C21 0.059(5) 0.051(5) 0.091(7) 0.003(5) 0.004(5) 0.026(5) C22 0.070(6) 0.051(6) 0.072(6) 0.001(5) -0.019(5) 0.012(5) C23 0.085(7) 0.073(7) 0.050(5) 0.001(4) 0.000(5) 0.020(6) C24 0.056(5) 0.045(5) 0.054(5) 0.004(4) 0.004(4) 0.010(4) C25 0.045(4) 0.033(4) 0.056(5) 0.010(4) 0.007(3) 0.002(4) C26 0.125(9) 0.053(6) 0.072(6) 0.016(5) 0.028(6) 0.005(6) C27 0.199(15) 0.084(10) 0.082(8) 0.044(8) 0.032(9) 0.011(10) C28 0.091(8) 0.041(6) 0.127(10) 0.018(7) 0.008(7) 0.002(6) C29 0.083(7) 0.036(6) 0.104(8) 0.005(5) 0.020(6) 0.008(5) C30 0.068(6) 0.041(5) 0.072(6) -0.003(4) 0.013(4) 0.002(5) C31 0.061(5) 0.068(6) 0.052(5) -0.013(4) -0.014(4) 0.031(5) C32 0.132(10) 0.103(9) 0.053(6) 0.007(6) 0.016(6) 0.052(8) C33 0.189(15) 0.157(14) 0.058(7) 0.019(8) 0.050(8) 0.091(12) C34 0.156(15) 0.220(21) 0.063(8) -0.035(11) 0.021(8) 0.084(15) C35 0.127(12) 0.137(14) 0.121(12) -0.083(11) 0.012(9) 0.037(11) C36 0.118(9) 0.083(9) 0.105(9) -0.038(7) 0.006(7) 0.029(8) C37 0.068(5) 0.047(5) 0.037(4) 0.005(4) 0.006(4) 0.014(4) C38 0.062(6) 0.085(7) 0.065(6) 0.016(5) -0.004(5) 0.019(5) C39 0.076(7) 0.113(10) 0.098(8) 0.025(8) -0.014(6) 0.022(7) C40 0.061(6) 0.134(12) 0.102(9) 0.018(8) 0.020(6) 0.008(8) C41 0.076(7) 0.101(10) 0.107(9) 0.017(7) 0.032(7) -0.002(7) C42 0.081(6) 0.051(6) 0.061(5) 0.006(4) 0.010(5) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.286(2) . ? Au1 S2 2.319(2) . ? P1 C13 1.821(7) . ? P1 C7 1.827(7) . ? P1 C1 1.836(7) . ? C1 C2 1.377(11) . ? C1 C6 1.418(10) . ? C2 C3 1.392(11) . ? C3 C4 1.348(13) . ? C4 C5 1.370(13) . ? C5 C6 1.399(12) . ? C7 C8 1.390(10) . ? C7 C12 1.409(11) . ? C8 C9 1.419(12) . ? C9 C10 1.370(13) . ? C10 C11 1.378(13) . ? C11 C12 1.380(12) . ? C13 C18 1.392(10) . ? C13 C14 1.428(9) . ? C14 N14 1.374(10) . ? C14 C15 1.406(10) . ? C15 C16 1.379(11) . ? C16 C17 1.380(11) . ? C17 C18 1.381(10) . ? S2 P2 2.065(3) . ? P2 N2 1.579(6) . ? P2 C25 1.826(8) . ? P2 C19 1.826(7) . ? N2 P3 1.615(7) . ? P3 O3 1.507(5) . ? P3 C31 1.811(9) . ? P3 C37 1.833(8) . ? C19 C20 1.395(10) . ? C19 C24 1.398(10) . ? C20 C21 1.408(11) . ? C21 C22 1.359(13) . ? C22 C23 1.410(13) . ? C23 C24 1.383(11) . ? C25 C26 1.362(12) . ? C25 C30 1.395(11) . ? C26 C27 1.41(2) . ? C27 C28 1.37(2) . ? C28 C29 1.351(14) . ? C29 C30 1.403(12) . ? C31 C32 1.380(14) . ? C31 C36 1.398(14) . ? C32 C33 1.426(14) . ? C33 C34 1.35(2) . ? C34 C35 1.38(2) . ? C35 C36 1.36(2) . ? C37 C42 1.362(12) . ? C37 C38 1.404(11) . ? C38 C39 1.389(14) . ? C39 C40 1.39(2) . ? C40 C41 1.37(2) . ? C41 C42 1.408(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 S2 167.80(6) . . ? C13 P1 C7 106.6(3) . . ? C13 P1 C1 105.7(3) . . ? C7 P1 C1 105.7(3) . . ? C13 P1 Au1 111.5(2) . . ? C7 P1 Au1 116.3(2) . . ? C1 P1 Au1 110.4(3) . . ? C2 C1 C6 119.4(7) . . ? C2 C1 P1 119.6(6) . . ? C6 C1 P1 121.0(6) . . ? C1 C2 C3 120.2(8) . . ? C4 C3 C2 121.2(9) . . ? C3 C4 C5 119.7(8) . . ? C4 C5 C6 121.6(9) . . ? C5 C6 C1 117.9(9) . . ? C8 C7 C12 118.8(7) . . ? C8 C7 P1 119.2(6) . . ? C12 C7 P1 122.0(6) . . ? C7 C8 C9 119.2(8) . . ? C10 C9 C8 120.5(8) . . ? C9 C10 C11 120.5(8) . . ? C12 C11 C10 119.9(9) . . ? C11 C12 C7 121.0(8) . . ? C18 C13 C14 119.1(6) . . ? C18 C13 P1 120.8(5) . . ? C14 C13 P1 120.1(5) . . ? N14 C14 C15 118.4(7) . . ? N14 C14 C13 123.9(6) . . ? C15 C14 C13 117.6(7) . . ? C16 C15 C14 121.6(7) . . ? C17 C16 C15 120.4(7) . . ? C16 C17 C18 119.4(7) . . ? C17 C18 C13 121.8(7) . . ? P2 S2 Au1 108.18(9) . . ? N2 P2 C25 107.8(4) . . ? N2 P2 C19 111.3(3) . . ? C25 P2 C19 105.9(3) . . ? N2 P2 S2 119.4(3) . . ? C25 P2 S2 101.5(3) . . ? C19 P2 S2 109.7(2) . . ? P2 N2 P3 132.3(4) . . ? O3 P3 N2 119.7(3) . . ? O3 P3 C31 109.9(4) . . ? N2 P3 C31 104.7(4) . . ? O3 P3 C37 108.8(4) . . ? N2 P3 C37 108.0(4) . . ? C31 P3 C37 104.7(4) . . ? C20 C19 C24 119.9(7) . . ? C20 C19 P2 117.8(6) . . ? C24 C19 P2 122.3(6) . . ? C19 C20 C21 118.3(7) . . ? C22 C21 C20 122.6(8) . . ? C21 C22 C23 118.5(8) . . ? C24 C23 C22 120.3(8) . . ? C23 C24 C19 120.4(8) . . ? C26 C25 C30 119.0(8) . . ? C26 C25 P2 121.4(7) . . ? C30 C25 P2 119.5(6) . . ? C25 C26 C27 119.9(11) . . ? C28 C27 C26 120.0(11) . . ? C29 C28 C27 121.3(10) . . ? C28 C29 C30 118.8(10) . . ? C25 C30 C29 121.0(9) . . ? C32 C31 C36 119.0(10) . . ? C32 C31 P3 121.8(7) . . ? C36 C31 P3 119.2(9) . . ? C31 C32 C33 118.6(12) . . ? C34 C33 C32 120.9(14) . . ? C33 C34 C35 120.0(12) . . ? C36 C35 C34 120.0(14) . . ? C35 C36 C31 121.4(14) . . ? C42 C37 C38 119.8(8) . . ? C42 C37 P3 119.7(6) . . ? C38 C37 P3 120.6(7) . . ? C39 C38 C37 119.2(10) . . ? C38 C39 C40 120.7(10) . . ? C41 C40 C39 119.9(10) . . ? C40 C41 C42 119.9(11) . . ? C37 C42 C41 120.6(9) . . ? 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 S2 Au1 P1 C13 -32.2(4) . . . . ? S2 Au1 P1 C7 -154.6(4) . . . . ? S2 Au1 P1 C1 85.0(4) . . . . ? C13 P1 C1 C2 98.8(6) . . . . ? C7 P1 C1 C2 -148.4(6) . . . . ? Au1 P1 C1 C2 -21.9(6) . . . . ? C13 P1 C1 C6 -80.9(7) . . . . ? C7 P1 C1 C6 31.9(7) . . . . ? Au1 P1 C1 C6 158.4(6) . . . . ? C6 C1 C2 C3 0.6(11) . . . . ? P1 C1 C2 C3 -179.2(6) . . . . ? C1 C2 C3 C4 -0.4(12) . . . . ? C2 C3 C4 C5 -0.2(14) . . . . ? C3 C4 C5 C6 0.6(14) . . . . ? C4 C5 C6 C1 -0.4(13) . . . . ? C2 C1 C6 C5 -0.2(11) . . . . ? P1 C1 C6 C5 179.5(6) . . . . ? C13 P1 C7 C8 -165.2(6) . . . . ? C1 P1 C7 C8 82.7(6) . . . . ? Au1 P1 C7 C8 -40.2(6) . . . . ? C13 P1 C7 C12 15.2(7) . . . . ? C1 P1 C7 C12 -97.0(6) . . . . ? Au1 P1 C7 C12 140.2(6) . . . . ? C12 C7 C8 C9 -0.7(11) . . . . ? P1 C7 C8 C9 179.7(6) . . . . ? C7 C8 C9 C10 1.5(12) . . . . ? C8 C9 C10 C11 -0.9(13) . . . . ? C9 C10 C11 C12 -0.6(13) . . . . ? C10 C11 C12 C7 1.4(13) . . . . ? C8 C7 C12 C11 -0.7(12) . . . . ? P1 C7 C12 C11 178.9(6) . . . . ? C7 P1 C13 C18 -105.4(6) . . . . ? C1 P1 C13 C18 6.8(7) . . . . ? Au1 P1 C13 C18 126.8(6) . . . . ? C7 P1 C13 C14 75.8(6) . . . . ? C1 P1 C13 C14 -172.0(6) . . . . ? Au1 P1 C13 C14 -52.0(6) . . . . ? C18 C13 C14 N14 178.9(7) . . . . ? P1 C13 C14 N14 -2.3(10) . . . . ? C18 C13 C14 C15 0.8(11) . . . . ? P1 C13 C14 C15 179.6(6) . . . . ? N14 C14 C15 C16 -178.3(8) . . . . ? C13 C14 C15 C16 -0.1(12) . . . . ? C14 C15 C16 C17 -0.5(13) . . . . ? C15 C16 C17 C18 0.3(14) . . . . ? C16 C17 C18 C13 0.4(13) . . . . ? C14 C13 C18 C17 -0.9(12) . . . . ? P1 C13 C18 C17 -179.8(6) . . . . ? P1 Au1 S2 P2 -152.3(3) . . . . ? Au1 S2 P2 N2 -72.9(3) . . . . ? Au1 S2 P2 C25 168.9(3) . . . . ? Au1 S2 P2 C19 57.2(3) . . . . ? C25 P2 N2 P3 173.9(5) . . . . ? C19 P2 N2 P3 -70.5(6) . . . . ? S2 P2 N2 P3 59.0(6) . . . . ? P2 N2 P3 O3 51.1(7) . . . . ? P2 N2 P3 C31 174.8(5) . . . . ? P2 N2 P3 C37 -74.0(6) . . . . ? N2 P2 C19 C20 -29.7(7) . . . . ? C25 P2 C19 C20 87.2(6) . . . . ? S2 P2 C19 C20 -164.1(5) . . . . ? N2 P2 C19 C24 153.7(6) . . . . ? C25 P2 C19 C24 -89.4(7) . . . . ? S2 P2 C19 C24 19.3(7) . . . . ? C24 C19 C20 C21 0.3(11) . . . . ? P2 C19 C20 C21 -176.4(6) . . . . ? C19 C20 C21 C22 0.8(13) . . . . ? C20 C21 C22 C23 -1.6(14) . . . . ? C21 C22 C23 C24 1.3(14) . . . . ? C22 C23 C24 C19 -0.3(13) . . . . ? C20 C19 C24 C23 -0.5(12) . . . . ? P2 C19 C24 C23 176.0(7) . . . . ? N2 P2 C25 C26 -10.3(9) . . . . ? C19 P2 C25 C26 -129.4(8) . . . . ? S2 P2 C25 C26 116.0(8) . . . . ? N2 P2 C25 C30 172.9(6) . . . . ? C19 P2 C25 C30 53.8(7) . . . . ? S2 P2 C25 C30 -60.8(7) . . . . ? C30 C25 C26 C27 -0.6(16) . . . . ? P2 C25 C26 C27 -177.4(10) . . . . ? C25 C26 C27 C28 0.3(21) . . . . ? C26 C27 C28 C29 -0.5(21) . . . . ? C27 C28 C29 C30 0.9(18) . . . . ? C26 C25 C30 C29 1.1(13) . . . . ? P2 C25 C30 C29 178.0(7) . . . . ? C28 C29 C30 C25 -1.2(15) . . . . ? O3 P3 C31 C32 127.5(7) . . . . ? N2 P3 C31 C32 -2.3(8) . . . . ? C37 P3 C31 C32 -115.8(8) . . . . ? O3 P3 C31 C36 -51.0(8) . . . . ? N2 P3 C31 C36 179.1(8) . . . . ? C37 P3 C31 C36 65.6(8) . . . . ? C36 C31 C32 C33 -0.6(15) . . . . ? P3 C31 C32 C33 -179.1(9) . . . . ? C31 C32 C33 C34 2.1(21) . . . . ? C32 C33 C34 C35 -3.2(25) . . . . ? C33 C34 C35 C36 2.9(25) . . . . ? C34 C35 C36 C31 -1.4(22) . . . . ? C32 C31 C36 C35 0.3(17) . . . . ? P3 C31 C36 C35 178.9(10) . . . . ? O3 P3 C37 C42 16.5(8) . . . . ? N2 P3 C37 C42 147.9(6) . . . . ? C31 P3 C37 C42 -100.9(7) . . . . ? O3 P3 C37 C38 -163.8(7) . . . . ? N2 P3 C37 C38 -32.4(8) . . . . ? C31 P3 C37 C38 78.8(8) . . . . ? C42 C37 C38 C39 -0.4(14) . . . . ? P3 C37 C38 C39 179.9(8) . . . . ? C37 C38 C39 C40 0.7(18) . . . . ? C38 C39 C40 C41 -1.0(20) . . . . ? C39 C40 C41 C42 1.0(20) . . . . ? C38 C37 C42 C41 0.5(14) . . . . ? P3 C37 C42 C41 -179.9(8) . . . . ? C40 C41 C42 C37 -0.8(17) . . . . ? _refine_diff_density_max 1.180 _refine_diff_density_min -1.935 _refine_diff_density_rms 0.117 #end data_13 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C43 H39 N2 O P3 Pt S.(C H Cl3)0.25' _chemical_formula_structural 'C43.25 H39.25 Cl0.75 N2 O P3 Pt S' _chemical_formula_analytical 'C43.25 H39.25 Cl0.75 N2 O P3 Pt S' _chemical_formula_sum 'C43.25 H39.25 Cl0.75 N2 O P3 Pt S' _chemical_formula_weight 949.66 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7499(3) _cell_length_b 13.9705(4) _cell_length_c 16.7686(4) _cell_angle_alpha 112.0190(10) _cell_angle_beta 99.4310(10) _cell_angle_gamma 98.6350(10) _cell_volume 2240.61(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 79 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max .18 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .3 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method - _exptl_crystal_F_000 945 _exptl_absorpt_coefficient_mu 3.362 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.680984 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 11568 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 23.29 _reflns_number_total 6429 _reflns_number_observed 4890 _reflns_observed_criterion 2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6379 _refine_ls_number_parameters 498 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_obs 0.0438 _refine_ls_wR_factor_all 0.1344 _refine_ls_wR_factor_obs 0.0994 _refine_ls_goodness_of_fit_all 0.962 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_restrained_S_all 1.258 _refine_ls_restrained_S_obs 1.068 _refine_ls_shift/esd_max -0.722 _refine_ls_shift/esd_mean 0.013 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.19259(3) -1.69696(2) 0.10674(2) 0.04040(15) Uani 1 d . . C50 C 0.0142(8) -1.8026(7) 0.0521(7) 0.077(3) Uani 1 d . . H50A H -0.0330(26) -1.7889(34) 0.0053(29) 0.115 Uiso 1 calc R . H50B H -0.0336(26) -1.7943(36) 0.0970(12) 0.115 Uiso 1 calc R . H50C H 0.0261(8) -1.8738(7) 0.0287(39) 0.115 Uiso 1 calc R . P1 P 0.2982(2) -1.82425(15) 0.07491(12) 0.0398(5) Uani 1 d . . C1 C 0.2686(7) -1.9202(6) 0.1219(5) 0.044(2) Uani 1 d . . C2 C 0.3005(8) -2.0184(6) 0.0893(5) 0.052(2) Uani 1 d . . H2A H 0.3372(8) -2.0362(6) 0.0406(5) 0.063 Uiso 1 calc R . C3 C 0.2796(9) -2.0892(7) 0.1266(7) 0.069(3) Uani 1 d . . H3A H 0.2999(9) -2.1548(7) 0.1020(7) 0.083 Uiso 1 calc R . C4 C 0.2288(10) -2.0646(9) 0.2002(8) 0.081(3) Uani 1 d . . H4A H 0.2175(10) -2.1118(9) 0.2269(8) 0.097 Uiso 1 calc R . C5 C 0.1948(10) -1.9673(10) 0.2338(7) 0.085(3) Uani 1 d . . H5A H 0.1584(10) -1.9501(10) 0.2825(7) 0.102 Uiso 1 calc R . C6 C 0.2150(9) -1.8948(7) 0.1945(6) 0.064(2) Uani 1 d . . H6A H 0.1923(9) -1.8300(7) 0.2175(6) 0.077 Uiso 1 calc R . C7 C 0.2853(8) -1.9060(6) -0.0412(5) 0.041(2) Uani 1 d . . C8 C 0.3807(8) -1.8935(6) -0.0849(5) 0.050(2) Uani 1 d . . H8A H 0.4576(8) -1.8425(6) -0.0542(5) 0.060 Uiso 1 calc R . C9 C 0.3623(9) -1.9571(7) -0.1751(5) 0.058(2) Uani 1 d . . H9A H 0.4275(9) -1.9482(7) -0.2037(5) 0.070 Uiso 1 calc R . C10 C 0.2508(9) -2.0316(7) -0.2213(6) 0.059(2) Uani 1 d . . H10A H 0.2397(9) -2.0733(7) -0.2813(6) 0.070 Uiso 1 calc R . C11 C 0.1553(10) -2.0451(7) -0.1799(6) 0.064(2) Uani 1 d . . H11A H 0.0791(10) -2.0967(7) -0.2114(6) 0.077 Uiso 1 calc R . C12 C 0.1710(8) -1.9826(6) -0.0913(6) 0.059(2) Uani 1 d . . H12A H 0.1040(8) -1.9915(6) -0.0642(6) 0.070 Uiso 1 calc R . C13 C 0.4683(7) -1.7546(6) 0.1204(5) 0.039(2) Uani 1 d . . C14 C 0.4925(7) -1.6455(6) 0.1575(4) 0.038(2) Uani 1 d . . N14 N 0.3830(6) -1.5934(5) 0.1653(4) 0.041(2) Uani 1 d D . H14A H 0.4006(65) -1.5292(34) 0.1560(42) 0.044(21) Uiso 1 d D . H14B H 0.3901(76) -1.5595(55) 0.2283(22) 0.064(26) Uiso 1 d D . C15 C 0.6169(8) -1.5857(7) 0.1893(5) 0.055(2) Uani 1 d . . H15A H 0.6323(8) -1.5121(7) 0.2152(5) 0.066 Uiso 1 calc R . C16 C 0.7202(8) -1.6343(7) 0.1833(5) 0.059(2) Uani 1 d . . H16A H 0.8048(8) -1.5937(7) 0.2020(5) 0.071 Uiso 1 calc R . C17 C 0.6962(8) -1.7435(7) 0.1492(6) 0.062(2) Uani 1 d . . H17A H 0.7653(8) -1.7765(7) 0.1470(6) 0.075 Uiso 1 calc R . C18 C 0.5728(8) -1.8034(6) 0.1187(5) 0.051(2) Uani 1 d . . H18A H 0.5578(8) -1.8769(6) 0.0966(5) 0.061 Uiso 1 calc R . S2 S 0.0633(2) -1.5700(2) 0.13372(13) 0.0505(5) Uani 1 d . . P2 P 0.1676(2) -1.4207(2) 0.21455(13) 0.0443(5) Uani 1 d . . N2 N 0.2282(7) -1.3912(5) 0.3152(4) 0.058(2) Uani 1 d . . P3 P 0.2870(2) -1.4517(2) 0.37028(13) 0.0504(6) Uani 1 d . . O3 O 0.3905(5) -1.5077(4) 0.3425(3) 0.064(2) Uani 1 d . . C19 C 0.2939(8) -1.3871(6) 0.1643(6) 0.051(2) Uani 1 d . . C20 C 0.4160(10) -1.3281(7) 0.2169(7) 0.076(3) Uani 1 d . . H20A H 0.4315(10) -1.2994(7) 0.2784(7) 0.091 Uiso 1 calc R . C21 C 0.5166(12) -1.3129(10) 0.1742(14) 0.119(5) Uani 1 d . . H21A H 0.5988(12) -1.2742(10) 0.2090(14) 0.142 Uiso 1 calc R . C22 C 0.4974(18) -1.3524(12) 0.0849(14) 0.126(6) Uani 1 d . . H22A H 0.5657(18) -1.3433(12) 0.0588(14) 0.151 Uiso 1 calc R . C23 C 0.3798(16) -1.4040(11) 0.0358(9) 0.100(4) Uani 1 d . . H23A H 0.3647(16) -1.4287(11) -0.0255(9) 0.120 Uiso 1 calc R . C24 C 0.2773(11) -1.4224(8) 0.0736(7) 0.077(3) Uani 1 d . . H24A H 0.1957(11) -1.4595(8) 0.0368(7) 0.092 Uiso 1 calc R . C25 C 0.0574(8) -1.3371(6) 0.2117(5) 0.050(2) Uani 1 d . . C26 C 0.0359(11) -1.2690(8) 0.2892(6) 0.094(4) Uani 1 d . . H26A H 0.0800(11) -1.2653(8) 0.3433(6) 0.112 Uiso 1 calc R . C27 C -0.0536(13) -1.2042(9) 0.2870(8) 0.118(5) Uani 1 d . . H27A H -0.0705(13) -1.1588(9) 0.3389(8) 0.141 Uiso 1 calc R . C28 C -0.1144(11) -1.2109(9) 0.2055(9) 0.096(4) Uani 1 d . . H28A H -0.1732(11) -1.1689(9) 0.2032(9) 0.116 Uiso 1 calc R . C29 C -0.0928(10) -1.2740(8) 0.1309(7) 0.080(3) Uani 1 d . . H29A H -0.1346(10) -1.2758(8) 0.0771(7) 0.096 Uiso 1 calc R . C30 C -0.0087(9) -1.3364(7) 0.1337(6) 0.065(3) Uani 1 d . . H30A H 0.0055(9) -1.3811(7) 0.0805(6) 0.078 Uiso 1 calc R . C31 C 0.3494(7) -1.3507(6) 0.4812(5) 0.048(2) Uani 1 d . . C32 C 0.4114(9) -1.3747(7) 0.5485(6) 0.069(3) Uani 1 d . . H32A H 0.4190(9) -1.4440(7) 0.5359(6) 0.083 Uiso 1 calc R . C33 C 0.4610(9) -1.2991(9) 0.6320(6) 0.076(3) Uani 1 d . . H33A H 0.4983(9) -1.3184(9) 0.6761(6) 0.091 Uiso 1 calc R . C34 C 0.4578(10) -1.1968(8) 0.6528(6) 0.073(3) Uani 1 d . . H34A H 0.4947(10) -1.1455(8) 0.7100(6) 0.088 Uiso 1 calc R . C35 C 0.4002(11) -1.1703(8) 0.5894(7) 0.082(3) Uani 1 d . . H35A H 0.3970(11) -1.0999(8) 0.6030(7) 0.098 Uiso 1 calc R . C36 C 0.3448(10) -1.2468(7) 0.5029(6) 0.075(3) Uani 1 d . . H36A H 0.3047(10) -1.2268(7) 0.4600(6) 0.090 Uiso 1 calc R . C37 C 0.1571(10) -1.5428(8) 0.3784(6) 0.071(3) Uani 1 d G . C38 C 0.0335(11) -1.5247(13) 0.3785(8) 0.112(4) Uani 1 d G . H38A H 0.0168(39) -1.4649(55) 0.3707(86) 0.135 Uiso 1 calc R . C39 C -0.0624(21) -1.5874(22) 0.3890(12) 0.182(13) Uani 1 d G . H39A H -0.1412(21) -1.5678(22) 0.3911(12) 0.218 Uiso 1 calc R . C40 C -0.0504(35) -1.6745(26) 0.3964(17) 0.231(22) Uani 1 d G . H40A H -0.1189(35) -1.7174(26) 0.4035(17) 0.277 Uiso 1 calc R . C41 C 0.0722(31) -1.7030(14) 0.3934(11) 0.192(11) Uani 1 d G . H41A H 0.0838(31) -1.7662(14) 0.3965(11) 0.230 Uiso 1 calc R . C42 C 0.1775(16) -1.6321(11) 0.3853(8) 0.123(5) Uani 1 d G . H42A H 0.2583(16) -1.6482(11) 0.3850(8) 0.148 Uiso 1 calc R . C60 C 0.2917(44) -1.8556(38) 0.5233(32) 0.300(61) Uiso 0.25 d PD . Cl1 Cl 0.3388(22) -1.8984(17) 0.6102(14) 0.188(8) Uiso 0.25 d PD . Cl2 Cl 0.2640(42) -1.9881(34) 0.4479(27) 0.318(18) Uiso 0.25 d PD . Cl3 Cl 0.1215(25) -1.9122(18) 0.4724(15) 0.201(8) Uiso 0.25 d PD . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0340(2) 0.0426(2) 0.0457(2) 0.01507(14) 0.01522(13) 0.01381(13) C50 0.038(5) 0.060(6) 0.120(8) 0.025(6) 0.018(5) 0.007(4) P1 0.0362(11) 0.0403(11) 0.0434(12) 0.0146(9) 0.0148(9) 0.0115(9) C1 0.044(5) 0.047(5) 0.043(5) 0.020(4) 0.007(4) 0.009(4) C2 0.054(5) 0.051(5) 0.058(5) 0.024(4) 0.022(4) 0.017(4) C3 0.068(7) 0.059(6) 0.083(7) 0.032(6) 0.008(6) 0.022(5) C4 0.081(8) 0.074(7) 0.103(9) 0.057(7) 0.014(6) 0.016(6) C5 0.084(8) 0.116(9) 0.080(7) 0.065(7) 0.041(6) 0.009(7) C6 0.078(7) 0.069(6) 0.060(6) 0.033(5) 0.030(5) 0.026(5) C7 0.051(5) 0.034(4) 0.041(4) 0.015(4) 0.016(4) 0.015(4) C8 0.048(5) 0.064(5) 0.048(5) 0.025(4) 0.021(4) 0.024(4) C9 0.060(6) 0.067(6) 0.051(6) 0.019(5) 0.026(5) 0.028(5) C10 0.062(6) 0.056(5) 0.042(5) 0.003(4) 0.006(5) 0.022(5) C11 0.068(7) 0.052(5) 0.052(6) 0.001(5) 0.013(5) 0.011(5) C12 0.051(5) 0.057(5) 0.066(6) 0.020(5) 0.024(4) 0.005(5) C13 0.037(4) 0.046(5) 0.041(4) 0.019(4) 0.015(3) 0.015(4) C14 0.028(4) 0.048(5) 0.036(4) 0.013(4) 0.015(3) 0.008(4) N14 0.040(4) 0.032(4) 0.046(4) 0.010(3) 0.008(3) 0.008(3) C15 0.044(5) 0.054(5) 0.059(5) 0.013(4) 0.013(4) 0.015(4) C16 0.030(5) 0.075(6) 0.063(6) 0.024(5) 0.002(4) 0.008(4) C17 0.043(6) 0.076(7) 0.075(6) 0.030(5) 0.021(5) 0.029(5) C18 0.046(5) 0.048(5) 0.057(5) 0.015(4) 0.015(4) 0.019(4) S2 0.0404(12) 0.0529(12) 0.0581(13) 0.0190(10) 0.0126(10) 0.0201(10) P2 0.0464(13) 0.0520(13) 0.0380(12) 0.0171(10) 0.0104(9) 0.0243(10) N2 0.069(5) 0.063(4) 0.045(4) 0.018(3) 0.012(3) 0.032(4) P3 0.0538(14) 0.0634(14) 0.0391(12) 0.0201(11) 0.0140(10) 0.0278(12) O3 0.066(4) 0.083(4) 0.049(3) 0.020(3) 0.019(3) 0.047(3) C19 0.057(6) 0.043(5) 0.058(6) 0.022(4) 0.017(4) 0.021(4) C20 0.071(7) 0.054(6) 0.098(8) 0.026(6) 0.027(6) 0.010(5) C21 0.068(8) 0.075(9) 0.218(18) 0.061(11) 0.059(11) 0.002(7) C22 0.141(15) 0.090(11) 0.196(18) 0.074(12) 0.117(15) 0.040(10) C23 0.127(11) 0.113(10) 0.104(10) 0.060(8) 0.081(9) 0.051(9) C24 0.091(8) 0.086(7) 0.073(7) 0.041(6) 0.036(6) 0.036(6) C25 0.055(5) 0.054(5) 0.048(5) 0.022(4) 0.015(4) 0.027(4) C26 0.124(9) 0.112(8) 0.053(6) 0.020(6) 0.019(6) 0.087(8) C27 0.160(12) 0.119(10) 0.088(9) 0.022(7) 0.047(8) 0.109(10) C28 0.087(8) 0.109(9) 0.124(11) 0.066(8) 0.022(7) 0.068(7) C29 0.079(7) 0.100(8) 0.071(7) 0.032(6) 0.014(5) 0.062(7) C30 0.071(6) 0.074(6) 0.052(6) 0.023(5) 0.014(5) 0.032(5) C31 0.047(5) 0.064(6) 0.044(5) 0.024(4) 0.015(4) 0.027(4) C32 0.087(7) 0.074(6) 0.049(6) 0.023(5) 0.010(5) 0.040(6) C33 0.078(7) 0.108(8) 0.044(6) 0.033(6) 0.005(5) 0.033(6) C34 0.084(7) 0.081(7) 0.048(6) 0.014(5) 0.012(5) 0.038(6) C35 0.113(9) 0.059(6) 0.066(7) 0.010(5) 0.027(6) 0.031(6) C36 0.102(8) 0.072(7) 0.056(6) 0.027(5) 0.012(5) 0.040(6) C37 0.090(8) 0.070(7) 0.050(6) 0.021(5) 0.021(5) 0.012(6) C38 0.084(9) 0.179(15) 0.068(8) 0.042(9) 0.031(7) 0.021(10) C39 0.101(13) 0.285(32) 0.081(11) 0.031(17) 0.027(9) -0.072(19) C40 0.234(30) 0.243(36) 0.093(14) -0.016(18) 0.080(17) -0.120(30) C41 0.359(37) 0.076(10) 0.101(12) 0.006(8) 0.091(19) -0.023(18) C42 0.178(15) 0.074(8) 0.114(11) 0.026(8) 0.076(10) 0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C50 2.063(8) . ? Pt1 N14 2.153(6) . ? Pt1 P1 2.197(2) . ? Pt1 S2 2.372(2) . ? P1 C1 1.807(8) . ? P1 C7 1.820(7) . ? P1 C13 1.823(7) . ? C1 C6 1.382(11) . ? C1 C2 1.392(10) . ? C2 C3 1.365(12) . ? C3 C4 1.379(14) . ? C4 C5 1.393(14) . ? C5 C6 1.409(12) . ? C7 C8 1.381(11) . ? C7 C12 1.397(10) . ? C8 C9 1.399(10) . ? C9 C10 1.355(11) . ? C10 C11 1.359(12) . ? C11 C12 1.378(11) . ? C13 C14 1.377(9) . ? C13 C18 1.397(10) . ? C14 C15 1.366(10) . ? C14 N14 1.472(9) . ? C15 C16 1.383(11) . ? C16 C17 1.379(11) . ? C17 C18 1.359(11) . ? S2 P2 2.030(3) . ? P2 N2 1.574(6) . ? P2 C25 1.791(7) . ? P2 C19 1.804(9) . ? N2 P3 1.589(6) . ? P3 O3 1.492(5) . ? P3 C31 1.800(8) . ? P3 C37 1.801(10) . ? C19 C24 1.382(12) . ? C19 C20 1.389(12) . ? C20 C21 1.42(2) . ? C21 C22 1.35(2) . ? C22 C23 1.32(2) . ? C23 C24 1.40(2) . ? C25 C26 1.373(11) . ? C25 C30 1.388(10) . ? C26 C27 1.422(13) . ? C27 C28 1.378(14) . ? C28 C29 1.314(14) . ? C29 C30 1.353(11) . ? C31 C36 1.370(11) . ? C31 C32 1.390(10) . ? C32 C33 1.356(12) . ? C33 C34 1.345(12) . ? C34 C35 1.342(12) . ? C35 C36 1.401(12) . ? C37 C38 1.39 . ? C37 C42 1.342(15) . ? C38 C39 1.33(2) . ? C39 C40 1.29(4) . ? C40 C41 1.44(4) . ? C41 C42 1.45(2) . ? C60 Cl2 1.75(3) . ? C60 Cl3 1.80(3) . ? C60 Cl1 1.80(3) . ? Cl1 Cl2 2.46(5) . ? Cl2 Cl3 2.00(4) . ? 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 C50 Pt1 N14 176.8(3) . . ? C50 Pt1 P1 92.9(3) . . ? N14 Pt1 P1 84.3(2) . . ? C50 Pt1 S2 82.6(3) . . ? N14 Pt1 S2 100.2(2) . . ? P1 Pt1 S2 175.41(7) . . ? C1 P1 C7 103.5(3) . . ? C1 P1 C13 107.2(3) . . ? C7 P1 C13 105.4(3) . . ? C1 P1 Pt1 117.4(3) . . ? C7 P1 Pt1 118.3(2) . . ? C13 P1 Pt1 104.2(2) . . ? C6 C1 C2 118.2(7) . . ? C6 C1 P1 119.1(6) . . ? C2 C1 P1 122.7(6) . . ? C3 C2 C1 121.9(8) . . ? C2 C3 C4 120.9(9) . . ? C3 C4 C5 118.4(9) . . ? C4 C5 C6 120.6(10) . . ? C1 C6 C5 120.0(9) . . ? C8 C7 C12 117.1(7) . . ? C8 C7 P1 123.6(6) . . ? C12 C7 P1 119.3(6) . . ? C7 C8 C9 120.4(8) . . ? C10 C9 C8 120.9(8) . . ? C9 C10 C11 119.9(8) . . ? C10 C11 C12 120.1(8) . . ? C11 C12 C7 121.6(8) . . ? C14 C13 C18 119.0(7) . . ? C14 C13 P1 115.9(5) . . ? C18 C13 P1 125.1(6) . . ? C15 C14 C13 120.5(7) . . ? C15 C14 N14 120.1(6) . . ? C13 C14 N14 119.4(6) . . ? C14 N14 Pt1 116.0(4) . . ? C14 C15 C16 120.3(8) . . ? C17 C16 C15 119.2(8) . . ? C18 C17 C16 120.7(8) . . ? C17 C18 C13 120.1(7) . . ? P2 S2 Pt1 112.75(10) . . ? N2 P2 C25 106.7(4) . . ? N2 P2 C19 109.0(4) . . ? C25 P2 C19 107.1(4) . . ? N2 P2 S2 120.5(3) . . ? C25 P2 S2 104.9(3) . . ? C19 P2 S2 107.9(3) . . ? P2 N2 P3 135.5(4) . . ? O3 P3 N2 119.1(4) . . ? O3 P3 C31 109.1(3) . . ? N2 P3 C31 104.3(3) . . ? O3 P3 C37 109.3(4) . . ? N2 P3 C37 109.3(4) . . ? C31 P3 C37 104.8(4) . . ? C24 C19 C20 117.2(9) . . ? C24 C19 P2 122.7(7) . . ? C20 C19 P2 120.0(7) . . ? C19 C20 C21 118.2(11) . . ? C22 C21 C20 122.7(14) . . ? C23 C22 C21 118.5(14) . . ? C22 C23 C24 121.6(13) . . ? C19 C24 C23 121.7(11) . . ? C26 C25 C30 116.9(7) . . ? C26 C25 P2 120.0(6) . . ? C30 C25 P2 123.1(6) . . ? C25 C26 C27 120.2(9) . . ? C28 C27 C26 117.8(10) . . ? C29 C28 C27 122.7(9) . . ? C28 C29 C30 119.0(9) . . ? C29 C30 C25 123.4(9) . . ? C36 C31 C32 116.7(8) . . ? C36 C31 P3 122.6(6) . . ? C32 C31 P3 120.6(6) . . ? C33 C32 C31 121.3(9) . . ? C34 C33 C32 121.8(9) . . ? C35 C34 C33 118.6(9) . . ? C34 C35 C36 121.2(9) . . ? C31 C36 C35 120.3(8) . . ? C38 C37 C42 117.0(12) . . ? C38 C37 P3 122.7(10) . . ? C42 C37 P3 120.3(10) . . ? C39 C38 C37 124.2(17) . . ? C38 C39 C40 122.4(31) . . ? C41 C40 C39 117.9(28) . . ? C40 C41 C42 119.2(22) . . ? C41 C42 C37 119.2(17) . . ? Cl2 C60 Cl3 68.5(20) . . ? Cl2 C60 Cl1 87.6(25) . . ? Cl3 C60 Cl1 108.9(26) . . ? C60 Cl1 Cl2 45.4(14) . . ? C60 Cl2 Cl3 57.0(14) . . ? C60 Cl2 Cl1 47.0(15) . . ? Cl3 Cl2 Cl1 81.5(16) . . ? Cl2 Cl3 C60 54.5(14) . . ? 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 C50 Pt1 P1 C1 -59.6(4) . . . . ? N14 Pt1 P1 C1 118.9(3) . . . . ? S2 Pt1 P1 C1 -71.0(10) . . . . ? C50 Pt1 P1 C7 65.7(4) . . . . ? N14 Pt1 P1 C7 -115.9(3) . . . . ? S2 Pt1 P1 C7 54.2(10) . . . . ? C50 Pt1 P1 C13 -177.9(4) . . . . ? N14 Pt1 P1 C13 0.6(3) . . . . ? S2 Pt1 P1 C13 170.7(9) . . . . ? C7 P1 C1 C6 -151.6(7) . . . . ? C13 P1 C1 C6 97.4(7) . . . . ? Pt1 P1 C1 C6 -19.3(7) . . . . ? C7 P1 C1 C2 30.1(7) . . . . ? C13 P1 C1 C2 -81.0(7) . . . . ? Pt1 P1 C1 C2 162.4(5) . . . . ? C6 C1 C2 C3 0.5(12) . . . . ? P1 C1 C2 C3 178.8(6) . . . . ? C1 C2 C3 C4 -1.8(13) . . . . ? C2 C3 C4 C5 2.3(15) . . . . ? C3 C4 C5 C6 -1.6(15) . . . . ? C2 C1 C6 C5 0.3(12) . . . . ? P1 C1 C6 C5 -178.1(7) . . . . ? C4 C5 C6 C1 0.3(14) . . . . ? C1 P1 C7 C8 -126.1(6) . . . . ? C13 P1 C7 C8 -13.7(7) . . . . ? Pt1 P1 C7 C8 102.1(6) . . . . ? C1 P1 C7 C12 57.2(7) . . . . ? C13 P1 C7 C12 169.5(6) . . . . ? Pt1 P1 C7 C12 -74.6(6) . . . . ? C12 C7 C8 C9 -1.1(11) . . . . ? P1 C7 C8 C9 -177.9(5) . . . . ? C7 C8 C9 C10 0.3(12) . . . . ? C8 C9 C10 C11 -0.1(13) . . . . ? C9 C10 C11 C12 0.7(13) . . . . ? C10 C11 C12 C7 -1.6(13) . . . . ? C8 C7 C12 C11 1.8(12) . . . . ? P1 C7 C12 C11 178.7(6) . . . . ? C1 P1 C13 C14 -128.5(6) . . . . ? C7 P1 C13 C14 121.8(6) . . . . ? Pt1 P1 C13 C14 -3.4(6) . . . . ? C1 P1 C13 C18 52.7(7) . . . . ? C7 P1 C13 C18 -57.0(7) . . . . ? Pt1 P1 C13 C18 177.9(6) . . . . ? C18 C13 C14 C15 2.2(11) . . . . ? P1 C13 C14 C15 -176.7(6) . . . . ? C18 C13 C14 N14 -175.7(6) . . . . ? P1 C13 C14 N14 5.5(9) . . . . ? C15 C14 N14 Pt1 177.2(6) . . . . ? C13 C14 N14 Pt1 -4.9(9) . . . . ? C50 Pt1 N14 C14 30.9(64) . . . . ? P1 Pt1 N14 C14 2.0(5) . . . . ? S2 Pt1 N14 C14 -177.2(5) . . . . ? C13 C14 C15 C16 1.2(12) . . . . ? N14 C14 C15 C16 179.0(7) . . . . ? C14 C15 C16 C17 -3.5(13) . . . . ? C15 C16 C17 C18 2.4(13) . . . . ? C16 C17 C18 C13 1.0(13) . . . . ? C14 C13 C18 C17 -3.3(11) . . . . ? P1 C13 C18 C17 175.5(6) . . . . ? C50 Pt1 S2 P2 169.5(3) . . . . ? N14 Pt1 S2 P2 -9.0(2) . . . . ? P1 Pt1 S2 P2 -179.0(1000) . . . . ? Pt1 S2 P2 N2 -68.5(3) . . . . ? Pt1 S2 P2 C25 171.4(3) . . . . ? Pt1 S2 P2 C19 57.5(3) . . . . ? C25 P2 N2 P3 152.5(7) . . . . ? C19 P2 N2 P3 -92.2(7) . . . . ? S2 P2 N2 P3 33.3(8) . . . . ? P2 N2 P3 O3 52.1(8) . . . . ? P2 N2 P3 C31 174.0(7) . . . . ? P2 N2 P3 C37 -74.3(8) . . . . ? N2 P2 C19 C24 166.7(7) . . . . ? C25 P2 C19 C24 -78.3(7) . . . . ? S2 P2 C19 C24 34.2(7) . . . . ? N2 P2 C19 C20 -9.8(8) . . . . ? C25 P2 C19 C20 105.3(7) . . . . ? S2 P2 C19 C20 -142.3(6) . . . . ? C24 C19 C20 C21 -3.2(13) . . . . ? P2 C19 C20 C21 173.5(8) . . . . ? C19 C20 C21 C22 0.8(18) . . . . ? C20 C21 C22 C23 2.3(22) . . . . ? C21 C22 C23 C24 -2.8(21) . . . . ? C20 C19 C24 C23 2.8(13) . . . . ? P2 C19 C24 C23 -173.8(8) . . . . ? C22 C23 C24 C19 0.3(18) . . . . ? N2 P2 C25 C26 -3.4(9) . . . . ? C19 P2 C25 C26 -120.0(8) . . . . ? S2 P2 C25 C26 125.5(8) . . . . ? N2 P2 C25 C30 176.1(7) . . . . ? C19 P2 C25 C30 59.4(8) . . . . ? S2 P2 C25 C30 -55.1(8) . . . . ? C30 C25 C26 C27 1.9(16) . . . . ? P2 C25 C26 C27 -178.7(10) . . . . ? C25 C26 C27 C28 -1.4(19) . . . . ? C26 C27 C28 C29 0.0(20) . . . . ? C27 C28 C29 C30 0.9(19) . . . . ? C28 C29 C30 C25 -0.4(17) . . . . ? C26 C25 C30 C29 -1.0(15) . . . . ? P2 C25 C30 C29 179.5(8) . . . . ? O3 P3 C31 C36 126.1(8) . . . . ? N2 P3 C31 C36 -2.2(9) . . . . ? C37 P3 C31 C36 -117.0(9) . . . . ? O3 P3 C31 C32 -50.4(8) . . . . ? N2 P3 C31 C32 -178.7(7) . . . . ? C37 P3 C31 C32 66.5(8) . . . . ? C36 C31 C32 C33 2.1(14) . . . . ? P3 C31 C32 C33 178.8(8) . . . . ? C31 C32 C33 C34 -3.0(16) . . . . ? C32 C33 C34 C35 2.0(17) . . . . ? C33 C34 C35 C36 -0.3(17) . . . . ? C32 C31 C36 C35 -0.4(14) . . . . ? P3 C31 C36 C35 -177.0(8) . . . . ? C34 C35 C36 C31 -0.5(17) . . . . ? O3 P3 C37 C38 -161.6(8) . . . . ? N2 P3 C37 C38 -29.7(10) . . . . ? C31 P3 C37 C38 81.6(9) . . . . ? O3 P3 C37 C42 18.9(9) . . . . ? N2 P3 C37 C42 150.8(8) . . . . ? C31 P3 C37 C42 -97.9(9) . . . . ? C42 C37 C38 C39 3.2(19) . . . . ? P3 C37 C38 C39 -176.3(12) . . . . ? C37 C38 C39 C40 -3.1(32) . . . . ? C38 C39 C40 C41 0.3(41) . . . . ? C39 C40 C41 C42 2.1(38) . . . . ? C40 C41 C42 C37 -1.9(26) . . . . ? C38 C37 C42 C41 -0.6(17) . . . . ? P3 C37 C42 C41 178.9(10) . . . . ? Cl2 C60 Cl1 Cl2 0.00(3) . . . . ? Cl3 C60 Cl1 Cl2 66.3(24) . . . . ? Cl3 C60 Cl2 Cl3 0.000(10) . . . . ? Cl1 C60 Cl2 Cl3 111.4(26) . . . . ? Cl3 C60 Cl2 Cl1 -111.4(26) . . . . ? Cl1 C60 Cl2 Cl1 0.00(3) . . . . ? C60 Cl1 Cl2 C60 0.00(4) . . . . ? C60 Cl1 Cl2 Cl3 -52.1(22) . . . . ? C60 Cl2 Cl3 C60 0.000(9) . . . . ? Cl1 Cl2 Cl3 C60 43.5(18) . . . . ? Cl2 C60 Cl3 Cl2 0.000(10) . . . . ? Cl1 C60 Cl3 Cl2 -79.5(29) . . . . ? _refine_diff_density_max 1.366 _refine_diff_density_min -1.577 _refine_diff_density_rms 0.118 #end