# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'Naokazu Kano' ; Department of Chemistry, Graduate School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo, 113-0033, Japan ; 'Takayuki Kawashima' ; Department of Chemistry, Graduate School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo, 113-0033, Japan ; 'Shinpei Kusaka' ; Department of Chemistry, Graduate School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo, 113-0033, Japan ; _publ_contact_author_name 'Naokazu Kano' _publ_contact_author_email KANO@CHEM.S.U-TOKYO.AC.JP _publ_section_title ; Insertion of Platinum and Palladium into Both a Sulfur(IV)-Sulfur(II) and a Sulfur(IV)-Oxygen Bond of a Sulfur-substituted Sulfurane ; _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo, 113-0033, Japan ; _publ_contact_author_fax +81-5800-6899 _publ_contact_author_phone +81-5841-4341 _publ_requested_category FA # Attachment 'pt1220.cif' data_pt1220 _database_code_depnum_ccdc_archive 'CCDC 735607' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H35 F6 O P Pt S2, 1.5(C6 H6)' _chemical_formula_sum 'C56 H44 F6 O P Pt S2' _chemical_formula_weight 1137.09 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.677(6) _cell_length_b 24.536(9) _cell_length_c 14.131(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.8966(18) _cell_angle_gamma 90.00 _cell_volume 4708(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13551 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 3.168 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5047 _exptl_absorpt_correction_T_max 0.7424 _exptl_absorpt_process_details ; Jacobson, R. (1998), Rigaku, Private communication ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_source_power 2.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 40.0000 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.5666 _diffrn_measurement_method dtprofit.ref _diffrn_reflns_number 28581 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8250 _reflns_number_gt 6306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 600 Slice: -70.0000 - 110.0000 Image width: 0.3000 Exp time: 25.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 45.0282 2theta: 19.7982 scan: Number of images: 600 Slice: -70.0000 - 110.0000 Image width: 0.3000 Exp time: 25.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 45.0282 2theta: 19.7982 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_orient_matrix_UB_11 -0.0099 _diffrn_orient_matrix_UB_12 -0.0724 _diffrn_orient_matrix_UB_13 -0.0094 _diffrn_orient_matrix_UB_21 0.0270 _diffrn_orient_matrix_UB_22 0.0002 _diffrn_orient_matrix_UB_23 -0.0305 _diffrn_orient_matrix_UB_31 0.0510 _diffrn_orient_matrix_UB_32 -0.0215 _diffrn_orient_matrix_UB_33 0.0449 _diffrn_orient_matrix_type d*Trek _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+12.2708P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8250 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.11919(2) 0.641246(11) 0.21866(2) 0.02130(15) Uani 1 1 d . . . O1 O -0.0075(4) 0.6851(2) 0.1768(4) 0.0269(13) Uani 1 1 d . . . P1 P 0.06687(16) 0.59284(8) 0.33840(14) 0.0244(5) Uani 1 1 d . . . S1 S 0.18362(15) 0.70074(8) 0.11914(13) 0.0236(4) Uani 1 1 d . . . S2 S 0.26270(15) 0.59392(8) 0.23657(14) 0.0242(4) Uani 1 1 d . . . C1 C 0.1029(7) 0.7058(3) 0.0100(5) 0.0271(18) Uani 1 1 d . . . C2 C 0.1503(7) 0.7219(3) -0.0674(6) 0.0271(19) Uani 1 1 d . . . H1 H 0.2182 0.7311 -0.0587 0.033 Uiso 1 1 calc R . . C3 C 0.0967(8) 0.7245(3) -0.1579(6) 0.033(2) Uani 1 1 d . . . H2 H 0.1278 0.7364 -0.2108 0.040 Uiso 1 1 calc R . . C4 C -0.0015(7) 0.7097(3) -0.1707(6) 0.035(2) Uani 1 1 d . . . H3 H -0.0374 0.7088 -0.2325 0.043 Uiso 1 1 calc R . . C5 C -0.0461(7) 0.6962(3) -0.0915(6) 0.0315(19) Uani 1 1 d . . . H4 H -0.1142 0.6874 -0.1007 0.038 Uiso 1 1 calc R . . C6 C 0.0010(6) 0.6944(3) -0.0002(5) 0.0241(17) Uani 1 1 d . . . C7 C -0.0560(6) 0.6809(3) 0.0858(6) 0.0246(17) Uani 1 1 d . . . C8 C -0.1038(7) 0.6244(4) 0.0710(6) 0.033(2) Uani 1 1 d . . . F1 F -0.0379(4) 0.58649(19) 0.0584(4) 0.0359(12) Uani 1 1 d . . . F2 F -0.1737(4) 0.6216(2) -0.0056(3) 0.0345(11) Uani 1 1 d . . . F3 F -0.1490(4) 0.6102(2) 0.1450(3) 0.0386(12) Uani 1 1 d . . . C9 C -0.1360(7) 0.7264(4) 0.0877(6) 0.033(2) Uani 1 1 d . . . F4 F -0.0935(4) 0.7754(2) 0.0947(4) 0.0383(13) Uani 1 1 d . . . F5 F -0.2037(4) 0.7278(2) 0.0101(4) 0.0422(14) Uani 1 1 d . . . F6 F -0.1862(4) 0.7198(2) 0.1613(4) 0.0490(15) Uani 1 1 d . . . C10 C 0.2906(6) 0.6637(3) 0.0875(6) 0.0268(17) Uani 1 1 d . . . H5 H 0.3352 0.6913 0.0631 0.032 Uiso 1 1 calc R . . C11 C 0.2679(6) 0.6213(4) 0.0083(5) 0.0275(18) Uani 1 1 d . . . C12 C 0.3293(6) 0.6183(4) -0.0627(6) 0.0307(19) Uani 1 1 d . . . H6 H 0.3859 0.6409 -0.0603 0.037 Uiso 1 1 calc R . . C13 C 0.3075(7) 0.5817(4) -0.1377(6) 0.035(2) Uani 1 1 d . . . H7 H 0.3493 0.5802 -0.1866 0.042 Uiso 1 1 calc R . . C14 C 0.2288(8) 0.5487(4) -0.1427(6) 0.040(2) Uani 1 1 d . . . H8 H 0.2164 0.5235 -0.1937 0.048 Uiso 1 1 calc R . . C15 C 0.1655(7) 0.5515(4) -0.0723(6) 0.035(2) Uani 1 1 d . . . H9 H 0.1079 0.5296 -0.0773 0.042 Uiso 1 1 calc R . . C16 C 0.1860(6) 0.5858(3) 0.0034(6) 0.0305(19) Uani 1 1 d . . . H10 H 0.1451 0.5858 0.0532 0.037 Uiso 1 1 calc R . . C17 C 0.3457(7) 0.6406(3) 0.1811(6) 0.0238(18) Uani 1 1 d . . . C18 C 0.4362(6) 0.6085(4) 0.1551(6) 0.0298(19) Uani 1 1 d . . . C19 C 0.5184(6) 0.6387(3) 0.1384(7) 0.030(2) Uani 1 1 d . . . H11 H 0.5188 0.6770 0.1484 0.036 Uiso 1 1 calc R . . C20 C 0.6009(7) 0.6135(4) 0.1069(7) 0.041(2) Uani 1 1 d . . . H12 H 0.6565 0.6345 0.0949 0.049 Uiso 1 1 calc R . . C21 C 0.6000(7) 0.5580(4) 0.0937(7) 0.042(2) Uani 1 1 d . . . H13 H 0.6546 0.5403 0.0716 0.051 Uiso 1 1 calc R . . C22 C 0.5206(7) 0.5286(4) 0.1126(6) 0.037(2) Uani 1 1 d . . . H14 H 0.5217 0.4901 0.1056 0.044 Uiso 1 1 calc R . . C23 C 0.4366(7) 0.5534(4) 0.1421(6) 0.033(2) Uani 1 1 d . . . H15 H 0.3810 0.5321 0.1529 0.040 Uiso 1 1 calc R . . C24 C 0.3836(6) 0.6858(4) 0.2542(6) 0.0306(19) Uani 1 1 d . . . C25 C 0.4246(7) 0.6683(4) 0.3451(7) 0.037(2) Uani 1 1 d . . . H16 H 0.4249 0.6306 0.3604 0.045 Uiso 1 1 calc R . . C26 C 0.4645(7) 0.7055(4) 0.4125(6) 0.038(2) Uani 1 1 d . . . H17 H 0.4908 0.6933 0.4741 0.045 Uiso 1 1 calc R . . C27 C 0.4663(7) 0.7593(4) 0.3907(7) 0.043(2) Uani 1 1 d . . . H18 H 0.4945 0.7846 0.4370 0.051 Uiso 1 1 calc R . . C28 C 0.4269(7) 0.7775(4) 0.3008(7) 0.037(2) Uani 1 1 d . . . H19 H 0.4278 0.8152 0.2856 0.045 Uiso 1 1 calc R . . C29 C 0.3863(7) 0.7399(3) 0.2337(6) 0.033(2) Uani 1 1 d . . . H20 H 0.3598 0.7523 0.1722 0.039 Uiso 1 1 calc R . . C30 C 0.1233(6) 0.6142(3) 0.4552(6) 0.0279(18) Uani 1 1 d . . . C31 C 0.0728(8) 0.6057(4) 0.5352(6) 0.039(2) Uani 1 1 d . . . H21 H 0.0091 0.5897 0.5281 0.047 Uiso 1 1 calc R . . C32 C 0.1169(7) 0.6209(4) 0.6236(6) 0.040(2) Uani 1 1 d . . . H22 H 0.0823 0.6164 0.6775 0.047 Uiso 1 1 calc R . . C33 C 0.2106(8) 0.6426(3) 0.6356(7) 0.038(2) Uani 1 1 d . . . H23 H 0.2399 0.6527 0.6975 0.045 Uiso 1 1 calc R . . C34 C 0.2624(8) 0.6499(4) 0.5580(7) 0.041(2) Uani 1 1 d . . . H24 H 0.3274 0.6643 0.5664 0.050 Uiso 1 1 calc R . . C35 C 0.2176(8) 0.6359(3) 0.4673(7) 0.032(2) Uani 1 1 d . . . H25 H 0.2520 0.6412 0.4135 0.038 Uiso 1 1 calc R . . C36 C -0.0645(6) 0.5980(3) 0.3467(5) 0.0221(17) Uani 1 1 d . . . C37 C -0.1257(6) 0.5522(4) 0.3396(6) 0.0289(18) Uani 1 1 d . . . H26 H -0.0989 0.5168 0.3344 0.035 Uiso 1 1 calc R . . C38 C -0.2272(7) 0.5595(4) 0.3400(6) 0.036(2) Uani 1 1 d . . . H27 H -0.2702 0.5291 0.3315 0.043 Uiso 1 1 calc R . . C39 C -0.2655(7) 0.6114(5) 0.3531(6) 0.041(2) Uani 1 1 d . . . H28 H -0.3340 0.6164 0.3554 0.049 Uiso 1 1 calc R . . C40 C -0.2014(8) 0.6552(4) 0.3625(7) 0.038(2) Uani 1 1 d . . . H29 H -0.2266 0.6907 0.3714 0.046 Uiso 1 1 calc R . . C41 C -0.1044(7) 0.6488(4) 0.3592(6) 0.032(2) Uani 1 1 d . . . H30 H -0.0624 0.6798 0.3657 0.038 Uiso 1 1 calc R . . C42 C 0.0948(6) 0.5205(3) 0.3290(6) 0.0251(18) Uani 1 1 d . . . C43 C 0.0736(7) 0.4963(3) 0.2373(6) 0.033(2) Uani 1 1 d . . . H31 H 0.0443 0.5169 0.1844 0.039 Uiso 1 1 calc R . . C44 C 0.0971(8) 0.4416(4) 0.2277(7) 0.045(2) Uani 1 1 d . . . H32 H 0.0820 0.4242 0.1676 0.054 Uiso 1 1 calc R . . C45 C 0.1420(7) 0.4122(4) 0.3039(7) 0.038(2) Uani 1 1 d . . . H33 H 0.1612 0.3755 0.2951 0.046 Uiso 1 1 calc R . . C46 C 0.1588(9) 0.4355(4) 0.3920(7) 0.046(3) Uani 1 1 d . . . H34 H 0.1858 0.4142 0.4450 0.055 Uiso 1 1 calc R . . C47 C 0.1371(6) 0.4897(4) 0.4051(6) 0.0300(19) Uani 1 1 d . . . H35 H 0.1512 0.5058 0.4663 0.036 Uiso 1 1 calc R . . C48 C 0.4160(11) 0.4082(5) 0.2651(9) 0.063(3) Uani 1 1 d . . . H36 H 0.4398 0.4446 0.2698 0.076 Uiso 1 1 calc R . . C49 C 0.4145(9) 0.3771(5) 0.3471(8) 0.055(3) Uani 1 1 d . . . H37 H 0.4436 0.3904 0.4071 0.066 Uiso 1 1 calc R . . C50 C 0.3703(9) 0.3266(5) 0.3399(8) 0.056(3) Uani 1 1 d . . . H38 H 0.3628 0.3063 0.3958 0.067 Uiso 1 1 calc R . . C51 C 0.3375(8) 0.3057(5) 0.2524(8) 0.052(3) Uani 1 1 d . . . H39 H 0.3123 0.2696 0.2471 0.063 Uiso 1 1 calc R . . C52 C 0.3407(8) 0.3369(5) 0.1717(8) 0.050(3) Uani 1 1 d . . . H40 H 0.3130 0.3235 0.1113 0.061 Uiso 1 1 calc R . . C53 C 0.3838(9) 0.3871(5) 0.1791(8) 0.056(3) Uani 1 1 d . . . H41 H 0.3912 0.4073 0.1231 0.067 Uiso 1 1 calc R . . C54 C 0.5245(9) 0.5171(5) 0.4129(7) 0.052(3) Uani 1 1 d . . . H42 H 0.5420 0.5289 0.3532 0.062 Uiso 1 1 calc R . . C55 C 0.4280(8) 0.5218(4) 0.4330(7) 0.047(3) Uani 1 1 d . . . H43 H 0.3786 0.5367 0.3872 0.056 Uiso 1 1 calc R . . C56 C 0.4053(8) 0.5047(5) 0.5195(8) 0.053(3) Uani 1 1 d . . . H44 H 0.3393 0.5080 0.5336 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0228(2) 0.0264(2) 0.0150(2) 0.00140(10) 0.00331(14) 0.00014(11) O1 0.029(3) 0.039(3) 0.012(3) -0.005(2) -0.002(2) 0.006(2) P1 0.0262(11) 0.0307(11) 0.0169(10) -0.0001(8) 0.0051(9) -0.0024(8) S1 0.0252(11) 0.0285(10) 0.0176(9) 0.0017(7) 0.0047(8) 0.0021(8) S2 0.0229(10) 0.0288(10) 0.0217(10) 0.0047(8) 0.0054(8) 0.0005(8) C1 0.038(5) 0.024(4) 0.018(4) 0.005(3) 0.000(4) 0.008(3) C2 0.033(5) 0.026(4) 0.022(4) 0.008(3) 0.003(4) 0.011(3) C3 0.054(6) 0.027(5) 0.019(4) 0.005(3) 0.006(4) 0.000(4) C4 0.045(6) 0.033(5) 0.027(4) -0.002(4) 0.000(4) -0.001(4) C5 0.029(5) 0.042(5) 0.024(4) -0.003(4) 0.005(4) -0.004(4) C6 0.029(5) 0.024(4) 0.019(4) 0.000(3) 0.004(3) 0.005(3) C7 0.019(4) 0.030(4) 0.026(4) -0.005(3) 0.006(3) 0.002(3) C8 0.024(5) 0.048(5) 0.029(5) 0.000(4) 0.004(4) 0.005(4) F1 0.026(3) 0.029(3) 0.052(3) -0.006(2) 0.000(2) -0.003(2) F2 0.028(3) 0.044(3) 0.028(3) 0.002(2) -0.008(2) -0.010(2) F3 0.037(3) 0.058(3) 0.021(2) 0.003(2) 0.002(2) -0.014(3) C9 0.031(5) 0.046(5) 0.020(4) -0.006(4) -0.004(4) -0.002(4) F4 0.043(3) 0.035(3) 0.035(3) -0.006(2) 0.000(2) 0.009(2) F5 0.036(3) 0.053(3) 0.034(3) -0.007(2) -0.013(2) 0.015(2) F6 0.044(4) 0.069(4) 0.037(3) 0.007(3) 0.017(3) 0.023(3) C10 0.030(5) 0.027(4) 0.025(4) 0.001(3) 0.012(4) -0.003(3) C11 0.021(4) 0.041(5) 0.020(4) 0.005(4) 0.002(3) -0.003(4) C12 0.025(4) 0.037(5) 0.031(5) -0.004(4) 0.011(4) 0.004(4) C13 0.033(5) 0.046(5) 0.025(4) -0.006(4) 0.001(4) 0.015(4) C14 0.049(6) 0.051(6) 0.018(4) -0.015(4) -0.005(4) 0.010(5) C15 0.032(5) 0.042(5) 0.030(5) -0.008(4) -0.003(4) -0.004(4) C16 0.026(5) 0.039(5) 0.028(4) -0.007(4) 0.008(4) 0.000(4) C17 0.027(5) 0.025(5) 0.019(4) -0.003(3) 0.001(4) 0.003(3) C18 0.029(5) 0.041(5) 0.021(4) 0.008(3) 0.010(4) 0.007(4) C19 0.015(4) 0.040(5) 0.033(5) -0.001(3) -0.002(4) 0.000(3) C20 0.024(5) 0.050(6) 0.050(6) 0.028(5) 0.012(4) 0.016(4) C21 0.023(5) 0.069(7) 0.036(5) 0.006(5) 0.011(4) 0.015(4) C22 0.038(6) 0.040(5) 0.032(5) -0.007(4) 0.005(4) 0.013(4) C23 0.037(5) 0.034(5) 0.030(5) -0.003(4) 0.009(4) 0.010(4) C24 0.020(4) 0.050(6) 0.022(4) 0.000(4) 0.005(3) -0.001(4) C25 0.040(5) 0.037(5) 0.037(5) 0.014(4) 0.011(4) 0.007(4) C26 0.032(5) 0.061(7) 0.019(4) 0.001(4) 0.002(4) -0.012(4) C27 0.033(5) 0.054(6) 0.040(5) -0.024(5) -0.001(4) -0.012(4) C28 0.035(5) 0.029(5) 0.048(6) -0.012(4) 0.004(4) -0.010(4) C29 0.029(5) 0.033(5) 0.033(5) -0.004(4) -0.010(4) -0.006(4) C30 0.033(5) 0.032(5) 0.019(4) -0.001(3) 0.001(3) 0.005(4) C31 0.039(6) 0.059(6) 0.023(4) 0.003(4) 0.011(4) 0.002(5) C32 0.041(6) 0.052(6) 0.027(5) -0.009(4) 0.008(4) -0.006(5) C33 0.041(6) 0.044(6) 0.027(5) -0.007(3) 0.002(4) 0.000(4) C34 0.034(6) 0.071(7) 0.019(5) -0.003(4) 0.002(4) -0.010(5) C35 0.039(6) 0.032(5) 0.026(5) -0.007(3) 0.012(4) -0.009(4) C36 0.018(4) 0.031(4) 0.019(4) -0.008(3) 0.010(3) -0.008(3) C37 0.026(5) 0.040(5) 0.022(4) 0.002(4) 0.007(3) -0.009(4) C38 0.023(5) 0.053(6) 0.031(5) -0.004(4) -0.001(4) -0.017(4) C39 0.019(5) 0.089(8) 0.015(4) 0.001(4) 0.001(3) 0.000(5) C40 0.039(6) 0.038(5) 0.039(5) 0.002(4) 0.004(4) 0.009(4) C41 0.034(5) 0.043(5) 0.018(4) -0.007(3) 0.000(4) -0.001(4) C42 0.027(4) 0.024(4) 0.026(4) -0.004(3) 0.009(3) -0.016(3) C43 0.039(5) 0.035(5) 0.023(4) -0.002(3) -0.003(4) 0.006(4) C44 0.056(7) 0.043(6) 0.038(6) -0.011(4) 0.010(5) -0.001(5) C45 0.026(5) 0.040(5) 0.051(6) 0.003(4) 0.012(4) 0.006(4) C46 0.061(7) 0.047(6) 0.030(5) 0.016(4) 0.011(5) 0.005(5) C47 0.027(5) 0.043(5) 0.019(4) 0.001(4) -0.003(4) -0.004(4) C48 0.081(9) 0.056(7) 0.051(7) 0.001(5) -0.001(7) -0.005(6) C49 0.048(7) 0.063(7) 0.050(7) -0.010(6) -0.011(5) -0.006(6) C50 0.047(7) 0.080(8) 0.041(6) 0.007(6) 0.004(5) -0.005(6) C51 0.038(6) 0.061(7) 0.060(7) 0.002(5) 0.008(5) -0.012(5) C52 0.038(6) 0.069(8) 0.042(6) -0.004(5) -0.004(5) -0.002(5) C53 0.065(8) 0.065(8) 0.036(6) 0.004(5) 0.002(5) 0.003(6) C54 0.058(8) 0.071(7) 0.028(5) 0.008(5) 0.007(5) -0.011(6) C55 0.049(7) 0.045(6) 0.041(6) 0.015(4) -0.011(5) -0.008(5) C56 0.033(6) 0.067(7) 0.060(7) 0.011(6) 0.007(5) -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 O1 2.066(6) . ? Pt1 P1 2.253(2) . ? Pt1 S2 2.268(2) . ? Pt1 S1 2.277(2) . ? O1 C7 1.378(9) . ? P1 C30 1.813(8) . ? P1 C36 1.819(8) . ? P1 C42 1.824(8) . ? S1 C1 1.789(8) . ? S1 C10 1.824(9) . ? S2 C17 1.852(9) . ? C1 C2 1.394(11) . ? C1 C6 1.412(12) . ? C2 C3 1.398(12) . ? C2 H1 0.9500 . ? C3 C4 1.382(14) . ? C3 H2 0.9500 . ? C4 C5 1.377(12) . ? C4 H3 0.9500 . ? C5 C6 1.372(11) . ? C5 H4 0.9500 . ? C6 C7 1.557(11) . ? C7 C8 1.537(12) . ? C7 C9 1.564(12) . ? C8 F1 1.321(10) . ? C8 F3 1.324(10) . ? C8 F2 1.357(10) . ? C9 F6 1.325(10) . ? C9 F4 1.334(10) . ? C9 F5 1.348(10) . ? C10 C11 1.532(11) . ? C10 C17 1.548(11) . ? C10 H5 1.0000 . ? C11 C12 1.386(11) . ? C11 C16 1.414(12) . ? C12 C13 1.392(12) . ? C12 H6 0.9500 . ? C13 C14 1.342(14) . ? C13 H7 0.9500 . ? C14 C15 1.396(13) . ? C14 H8 0.9500 . ? C15 C16 1.364(12) . ? C15 H9 0.9500 . ? C16 H10 0.9500 . ? C17 C18 1.549(11) . ? C17 C24 1.561(11) . ? C18 C23 1.365(12) . ? C18 C19 1.391(12) . ? C19 C20 1.405(13) . ? C19 H11 0.9500 . ? C20 C21 1.375(14) . ? C20 H12 0.9500 . ? C21 C22 1.355(14) . ? C21 H13 0.9500 . ? C22 C23 1.406(12) . ? C22 H14 0.9500 . ? C23 H15 0.9500 . ? C24 C29 1.360(12) . ? C24 C25 1.406(12) . ? C25 C26 1.382(13) . ? C25 H16 0.9500 . ? C26 C27 1.356(14) . ? C26 H17 0.9500 . ? C27 C28 1.393(14) . ? C27 H18 0.9500 . ? C28 C29 1.391(12) . ? C28 H19 0.9500 . ? C29 H20 0.9500 . ? C30 C35 1.387(13) . ? C30 C31 1.410(12) . ? C31 C32 1.372(12) . ? C31 H21 0.9500 . ? C32 C33 1.379(14) . ? C32 H22 0.9500 . ? C33 C34 1.387(14) . ? C33 H23 0.9500 . ? C34 C35 1.395(13) . ? C34 H24 0.9500 . ? C35 H25 0.9500 . ? C36 C41 1.381(11) . ? C36 C37 1.396(11) . ? C37 C38 1.401(12) . ? C37 H26 0.9500 . ? C38 C39 1.395(14) . ? C38 H27 0.9500 . ? C39 C40 1.385(14) . ? C39 H28 0.9500 . ? C40 C41 1.342(14) . ? C40 H29 0.9500 . ? C41 H30 0.9500 . ? C42 C47 1.383(12) . ? C42 C43 1.424(11) . ? C43 C44 1.391(13) . ? C43 H31 0.9500 . ? C44 C45 1.378(14) . ? C44 H32 0.9500 . ? C45 C46 1.365(14) . ? C45 H33 0.9500 . ? C46 C47 1.380(13) . ? C46 H34 0.9500 . ? C47 H35 0.9500 . ? C48 C53 1.345(16) . ? C48 C49 1.389(17) . ? C48 H36 0.9500 . ? C49 C50 1.377(16) . ? C49 H37 0.9500 . ? C50 C51 1.363(15) . ? C50 H38 0.9500 . ? C51 C52 1.379(15) . ? C51 H39 0.9500 . ? C52 C53 1.364(17) . ? C52 H40 0.9500 . ? C53 H41 0.9500 . ? C54 C56 1.379(15) 3_666 ? C54 C55 1.388(16) . ? C54 H42 0.9500 . ? C55 C56 1.363(14) . ? C55 H43 0.9500 . ? C56 C54 1.379(15) 3_666 ? C56 H44 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 P1 99.13(17) . . ? O1 Pt1 S2 169.66(15) . . ? P1 Pt1 S2 89.71(8) . . ? O1 Pt1 S1 82.09(17) . . ? P1 Pt1 S1 169.52(7) . . ? S2 Pt1 S1 90.18(7) . . ? C7 O1 Pt1 121.4(5) . . ? C30 P1 C36 103.7(4) . . ? C30 P1 C42 106.1(4) . . ? C36 P1 C42 106.8(4) . . ? C30 P1 Pt1 113.1(3) . . ? C36 P1 Pt1 114.7(3) . . ? C42 P1 Pt1 111.7(3) . . ? C1 S1 C10 104.7(4) . . ? C1 S1 Pt1 109.4(3) . . ? C10 S1 Pt1 102.3(3) . . ? C17 S2 Pt1 101.7(3) . . ? C2 C1 C6 121.4(7) . . ? C2 C1 S1 113.6(7) . . ? C6 C1 S1 125.0(6) . . ? C1 C2 C3 119.3(9) . . ? C1 C2 H1 120.3 . . ? C3 C2 H1 120.3 . . ? C4 C3 C2 120.1(8) . . ? C4 C3 H2 119.9 . . ? C2 C3 H2 119.9 . . ? C5 C4 C3 118.4(8) . . ? C5 C4 H3 120.8 . . ? C3 C4 H3 120.8 . . ? C6 C5 C4 124.6(9) . . ? C6 C5 H4 117.7 . . ? C4 C5 H4 117.7 . . ? C5 C6 C1 115.9(7) . . ? C5 C6 C7 121.2(8) . . ? C1 C6 C7 122.9(7) . . ? O1 C7 C8 110.1(7) . . ? O1 C7 C6 118.8(7) . . ? C8 C7 C6 109.3(6) . . ? O1 C7 C9 100.9(6) . . ? C8 C7 C9 111.1(7) . . ? C6 C7 C9 106.1(6) . . ? F1 C8 F3 108.2(8) . . ? F1 C8 F2 106.5(7) . . ? F3 C8 F2 105.4(7) . . ? F1 C8 C7 111.6(7) . . ? F3 C8 C7 111.1(7) . . ? F2 C8 C7 113.7(7) . . ? F6 C9 F4 108.2(7) . . ? F6 C9 F5 105.7(8) . . ? F4 C9 F5 106.7(7) . . ? F6 C9 C7 110.9(7) . . ? F4 C9 C7 110.2(7) . . ? F5 C9 C7 114.7(7) . . ? C11 C10 C17 114.3(7) . . ? C11 C10 S1 114.8(6) . . ? C17 C10 S1 107.1(5) . . ? C11 C10 H5 106.7 . . ? C17 C10 H5 106.7 . . ? S1 C10 H5 106.7 . . ? C12 C11 C16 118.5(8) . . ? C12 C11 C10 118.6(8) . . ? C16 C11 C10 122.9(7) . . ? C11 C12 C13 119.5(9) . . ? C11 C12 H6 120.3 . . ? C13 C12 H6 120.3 . . ? C14 C13 C12 121.8(9) . . ? C14 C13 H7 119.1 . . ? C12 C13 H7 119.1 . . ? C13 C14 C15 119.6(8) . . ? C13 C14 H8 120.2 . . ? C15 C14 H8 120.2 . . ? C16 C15 C14 120.2(9) . . ? C16 C15 H9 119.9 . . ? C14 C15 H9 119.9 . . ? C15 C16 C11 120.3(8) . . ? C15 C16 H10 119.9 . . ? C11 C16 H10 119.9 . . ? C10 C17 C18 107.7(7) . . ? C10 C17 C24 113.3(6) . . ? C18 C17 C24 107.9(7) . . ? C10 C17 S2 109.1(6) . . ? C18 C17 S2 109.5(5) . . ? C24 C17 S2 109.3(6) . . ? C23 C18 C19 119.3(8) . . ? C23 C18 C17 123.5(8) . . ? C19 C18 C17 117.0(7) . . ? C18 C19 C20 121.0(8) . . ? C18 C19 H11 119.5 . . ? C20 C19 H11 119.5 . . ? C21 C20 C19 118.9(9) . . ? C21 C20 H12 120.5 . . ? C19 C20 H12 120.5 . . ? C22 C21 C20 119.7(9) . . ? C22 C21 H13 120.2 . . ? C20 C21 H13 120.2 . . ? C21 C22 C23 122.0(9) . . ? C21 C22 H14 119.0 . . ? C23 C22 H14 119.0 . . ? C18 C23 C22 119.0(9) . . ? C18 C23 H15 120.5 . . ? C22 C23 H15 120.5 . . ? C29 C24 C25 118.3(8) . . ? C29 C24 C17 124.6(7) . . ? C25 C24 C17 116.9(8) . . ? C26 C25 C24 120.7(9) . . ? C26 C25 H16 119.7 . . ? C24 C25 H16 119.7 . . ? C27 C26 C25 120.1(8) . . ? C27 C26 H17 119.9 . . ? C25 C26 H17 119.9 . . ? C26 C27 C28 120.3(8) . . ? C26 C27 H18 119.8 . . ? C28 C27 H18 119.8 . . ? C29 C28 C27 119.2(9) . . ? C29 C28 H19 120.4 . . ? C27 C28 H19 120.4 . . ? C24 C29 C28 121.5(9) . . ? C24 C29 H20 119.3 . . ? C28 C29 H20 119.3 . . ? C35 C30 C31 119.7(8) . . ? C35 C30 P1 120.7(7) . . ? C31 C30 P1 119.5(7) . . ? C32 C31 C30 119.1(9) . . ? C32 C31 H21 120.5 . . ? C30 C31 H21 120.5 . . ? C31 C32 C33 121.2(9) . . ? C31 C32 H22 119.4 . . ? C33 C32 H22 119.4 . . ? C32 C33 C34 120.5(9) . . ? C32 C33 H23 119.8 . . ? C34 C33 H23 119.8 . . ? C33 C34 C35 119.0(10) . . ? C33 C34 H24 120.5 . . ? C35 C34 H24 120.5 . . ? C30 C35 C34 120.5(9) . . ? C30 C35 H25 119.8 . . ? C34 C35 H25 119.8 . . ? C41 C36 C37 119.5(8) . . ? C41 C36 P1 118.6(6) . . ? C37 C36 P1 121.9(6) . . ? C36 C37 C38 118.9(8) . . ? C36 C37 H26 120.6 . . ? C38 C37 H26 120.6 . . ? C39 C38 C37 120.3(8) . . ? C39 C38 H27 119.8 . . ? C37 C38 H27 119.8 . . ? C40 C39 C38 118.5(9) . . ? C40 C39 H28 120.7 . . ? C38 C39 H28 120.7 . . ? C41 C40 C39 121.5(9) . . ? C41 C40 H29 119.3 . . ? C39 C40 H29 119.3 . . ? C40 C41 C36 121.2(9) . . ? C40 C41 H30 119.4 . . ? C36 C41 H30 119.4 . . ? C47 C42 C43 120.1(8) . . ? C47 C42 P1 123.2(6) . . ? C43 C42 P1 116.7(6) . . ? C44 C43 C42 117.8(8) . . ? C44 C43 H31 121.1 . . ? C42 C43 H31 121.1 . . ? C45 C44 C43 121.1(9) . . ? C45 C44 H32 119.5 . . ? C43 C44 H32 119.5 . . ? C46 C45 C44 120.3(9) . . ? C46 C45 H33 119.9 . . ? C44 C45 H33 119.9 . . ? C45 C46 C47 120.7(9) . . ? C45 C46 H34 119.6 . . ? C47 C46 H34 119.6 . . ? C46 C47 C42 120.0(8) . . ? C46 C47 H35 120.0 . . ? C42 C47 H35 120.0 . . ? C53 C48 C49 120.3(12) . . ? C53 C48 H36 119.8 . . ? C49 C48 H36 119.8 . . ? C50 C49 C48 118.9(10) . . ? C50 C49 H37 120.6 . . ? C48 C49 H37 120.6 . . ? C51 C50 C49 120.0(11) . . ? C51 C50 H38 120.0 . . ? C49 C50 H38 120.0 . . ? C50 C51 C52 120.1(11) . . ? C50 C51 H39 119.9 . . ? C52 C51 H39 119.9 . . ? C53 C52 C51 119.6(10) . . ? C53 C52 H40 120.2 . . ? C51 C52 H40 120.2 . . ? C48 C53 C52 120.6(11) . . ? C48 C53 H41 119.7 . . ? C52 C53 H41 119.7 . . ? C56 C54 C55 119.4(10) 3_666 . ? C56 C54 H42 120.3 3_666 . ? C55 C54 H42 120.3 . . ? C56 C55 C54 118.8(10) . . ? C56 C55 H43 120.6 . . ? C54 C55 H43 120.6 . . ? C55 C56 C54 121.7(11) . 3_666 ? C55 C56 H44 119.1 . . ? C54 C56 H44 119.1 3_666 . ? 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 P1 Pt1 O1 C7 -119.7(5) . . . . ? S2 Pt1 O1 C7 28.8(13) . . . . ? S1 Pt1 O1 C7 70.8(6) . . . . ? O1 Pt1 P1 C30 -109.2(3) . . . . ? S2 Pt1 P1 C30 76.2(3) . . . . ? S1 Pt1 P1 C30 -13.3(6) . . . . ? O1 Pt1 P1 C36 9.5(3) . . . . ? S2 Pt1 P1 C36 -165.2(3) . . . . ? S1 Pt1 P1 C36 105.4(5) . . . . ? O1 Pt1 P1 C42 131.2(3) . . . . ? S2 Pt1 P1 C42 -43.5(3) . . . . ? S1 Pt1 P1 C42 -132.9(5) . . . . ? O1 Pt1 S1 C1 -46.2(3) . . . . ? P1 Pt1 S1 C1 -143.7(5) . . . . ? S2 Pt1 S1 C1 126.9(3) . . . . ? O1 Pt1 S1 C10 -156.8(3) . . . . ? P1 Pt1 S1 C10 105.7(5) . . . . ? S2 Pt1 S1 C10 16.3(3) . . . . ? O1 Pt1 S2 C17 52.5(10) . . . . ? P1 Pt1 S2 C17 -158.5(3) . . . . ? S1 Pt1 S2 C17 11.0(3) . . . . ? C10 S1 C1 C2 -46.2(7) . . . . ? Pt1 S1 C1 C2 -155.2(5) . . . . ? C10 S1 C1 C6 133.3(7) . . . . ? Pt1 S1 C1 C6 24.2(8) . . . . ? C6 C1 C2 C3 -3.1(12) . . . . ? S1 C1 C2 C3 176.4(6) . . . . ? C1 C2 C3 C4 -1.8(12) . . . . ? C2 C3 C4 C5 4.4(13) . . . . ? C3 C4 C5 C6 -2.4(14) . . . . ? C4 C5 C6 C1 -2.2(13) . . . . ? C4 C5 C6 C7 177.6(8) . . . . ? C2 C1 C6 C5 4.9(12) . . . . ? S1 C1 C6 C5 -174.5(6) . . . . ? C2 C1 C6 C7 -174.9(7) . . . . ? S1 C1 C6 C7 5.7(11) . . . . ? Pt1 O1 C7 C8 69.3(8) . . . . ? Pt1 O1 C7 C6 -57.8(8) . . . . ? Pt1 O1 C7 C9 -173.2(5) . . . . ? C5 C6 C7 O1 -173.5(7) . . . . ? C1 C6 C7 O1 6.3(11) . . . . ? C5 C6 C7 C8 59.0(10) . . . . ? C1 C6 C7 C8 -121.2(8) . . . . ? C5 C6 C7 C9 -60.9(9) . . . . ? C1 C6 C7 C9 118.9(8) . . . . ? O1 C7 C8 F1 -76.2(9) . . . . ? C6 C7 C8 F1 56.1(9) . . . . ? C9 C7 C8 F1 172.8(7) . . . . ? O1 C7 C8 F3 44.6(9) . . . . ? C6 C7 C8 F3 176.9(7) . . . . ? C9 C7 C8 F3 -66.3(9) . . . . ? O1 C7 C8 F2 163.3(7) . . . . ? C6 C7 C8 F2 -64.4(9) . . . . ? C9 C7 C8 F2 52.3(9) . . . . ? O1 C7 C9 F6 -52.8(9) . . . . ? C8 C7 C9 F6 64.0(9) . . . . ? C6 C7 C9 F6 -177.3(7) . . . . ? O1 C7 C9 F4 67.1(8) . . . . ? C8 C7 C9 F4 -176.2(7) . . . . ? C6 C7 C9 F4 -57.5(8) . . . . ? O1 C7 C9 F5 -172.5(7) . . . . ? C8 C7 C9 F5 -55.7(10) . . . . ? C6 C7 C9 F5 63.0(9) . . . . ? C1 S1 C10 C11 -32.7(7) . . . . ? Pt1 S1 C10 C11 81.4(6) . . . . ? C1 S1 C10 C17 -160.8(5) . . . . ? Pt1 S1 C10 C17 -46.7(5) . . . . ? C17 C10 C11 C12 -99.1(9) . . . . ? S1 C10 C11 C12 136.5(7) . . . . ? C17 C10 C11 C16 81.9(10) . . . . ? S1 C10 C11 C16 -42.4(10) . . . . ? C16 C11 C12 C13 1.8(13) . . . . ? C10 C11 C12 C13 -177.2(8) . . . . ? C11 C12 C13 C14 -0.9(14) . . . . ? C12 C13 C14 C15 1.5(14) . . . . ? C13 C14 C15 C16 -3.2(14) . . . . ? C14 C15 C16 C11 4.2(14) . . . . ? C12 C11 C16 C15 -3.5(13) . . . . ? C10 C11 C16 C15 175.4(8) . . . . ? C11 C10 C17 C18 51.1(9) . . . . ? S1 C10 C17 C18 179.4(5) . . . . ? C11 C10 C17 C24 170.3(7) . . . . ? S1 C10 C17 C24 -61.4(8) . . . . ? C11 C10 C17 S2 -67.7(8) . . . . ? S1 C10 C17 S2 60.7(6) . . . . ? Pt1 S2 C17 C10 -43.3(5) . . . . ? Pt1 S2 C17 C18 -160.9(5) . . . . ? Pt1 S2 C17 C24 81.1(6) . . . . ? C10 C17 C18 C23 -96.4(9) . . . . ? C24 C17 C18 C23 141.0(8) . . . . ? S2 C17 C18 C23 22.1(10) . . . . ? C10 C17 C18 C19 79.3(9) . . . . ? C24 C17 C18 C19 -43.3(10) . . . . ? S2 C17 C18 C19 -162.2(7) . . . . ? C23 C18 C19 C20 1.1(13) . . . . ? C17 C18 C19 C20 -174.8(8) . . . . ? C18 C19 C20 C21 -0.8(14) . . . . ? C19 C20 C21 C22 -0.9(14) . . . . ? C20 C21 C22 C23 2.4(14) . . . . ? C19 C18 C23 C22 0.3(12) . . . . ? C17 C18 C23 C22 175.9(8) . . . . ? C21 C22 C23 C18 -2.1(14) . . . . ? C10 C17 C24 C29 -12.0(12) . . . . ? C18 C17 C24 C29 107.0(9) . . . . ? S2 C17 C24 C29 -134.0(8) . . . . ? C10 C17 C24 C25 173.1(8) . . . . ? C18 C17 C24 C25 -67.8(9) . . . . ? S2 C17 C24 C25 51.1(9) . . . . ? C29 C24 C25 C26 1.5(14) . . . . ? C17 C24 C25 C26 176.7(9) . . . . ? C24 C25 C26 C27 -1.3(15) . . . . ? C25 C26 C27 C28 0.8(15) . . . . ? C26 C27 C28 C29 -0.3(15) . . . . ? C25 C24 C29 C28 -1.0(14) . . . . ? C17 C24 C29 C28 -175.8(9) . . . . ? C27 C28 C29 C24 0.4(15) . . . . ? C36 P1 C30 C35 -154.8(7) . . . . ? C42 P1 C30 C35 92.9(8) . . . . ? Pt1 P1 C30 C35 -29.9(8) . . . . ? C36 P1 C30 C31 28.8(8) . . . . ? C42 P1 C30 C31 -83.6(8) . . . . ? Pt1 P1 C30 C31 153.6(6) . . . . ? C35 C30 C31 C32 2.2(14) . . . . ? P1 C30 C31 C32 178.7(7) . . . . ? C30 C31 C32 C33 -2.0(15) . . . . ? C31 C32 C33 C34 0.4(15) . . . . ? C32 C33 C34 C35 1.1(15) . . . . ? C31 C30 C35 C34 -0.7(13) . . . . ? P1 C30 C35 C34 -177.1(7) . . . . ? C33 C34 C35 C30 -1.0(14) . . . . ? C30 P1 C36 C41 65.1(7) . . . . ? C42 P1 C36 C41 176.9(6) . . . . ? Pt1 P1 C36 C41 -58.8(7) . . . . ? C30 P1 C36 C37 -115.8(7) . . . . ? C42 P1 C36 C37 -4.0(8) . . . . ? Pt1 P1 C36 C37 120.4(6) . . . . ? C41 C36 C37 C38 3.5(12) . . . . ? P1 C36 C37 C38 -175.7(6) . . . . ? C36 C37 C38 C39 -3.7(13) . . . . ? C37 C38 C39 C40 2.0(13) . . . . ? C38 C39 C40 C41 0.0(14) . . . . ? C39 C40 C41 C36 -0.3(14) . . . . ? C37 C36 C41 C40 -1.5(13) . . . . ? P1 C36 C41 C40 177.6(7) . . . . ? C30 P1 C42 C47 9.1(8) . . . . ? C36 P1 C42 C47 -101.0(8) . . . . ? Pt1 P1 C42 C47 132.8(7) . . . . ? C30 P1 C42 C43 -169.1(7) . . . . ? C36 P1 C42 C43 80.7(7) . . . . ? Pt1 P1 C42 C43 -45.4(7) . . . . ? C47 C42 C43 C44 -0.2(13) . . . . ? P1 C42 C43 C44 178.0(7) . . . . ? C42 C43 C44 C45 -1.8(15) . . . . ? C43 C44 C45 C46 4.0(16) . . . . ? C44 C45 C46 C47 -4.1(16) . . . . ? C45 C46 C47 C42 2.1(15) . . . . ? C43 C42 C47 C46 0.1(13) . . . . ? P1 C42 C47 C46 -178.1(7) . . . . ? C53 C48 C49 C50 -7(2) . . . . ? C48 C49 C50 C51 6.3(19) . . . . ? C49 C50 C51 C52 -5.6(18) . . . . ? C50 C51 C52 C53 5.0(18) . . . . ? C49 C48 C53 C52 6(2) . . . . ? C51 C52 C53 C48 -5(2) . . . . ? C56 C54 C55 C56 0.1(18) 3_666 . . . ? C54 C55 C56 C54 -0.1(19) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 5.843 _refine_diff_density_min -1.785 _refine_diff_density_rms 0.210 # Attachment 'pdpph3q1.cif' data_pdpph3q1 _database_code_depnum_ccdc_archive 'CCDC 735608' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H28 F6 O P2 Pd S, C6 H6' _chemical_formula_sum 'C41 H34 F6 O P2 Pd S' _chemical_formula_weight 857.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.054(4) _cell_length_b 11.308(4) _cell_length_c 17.161(7) _cell_angle_alpha 98.614(14) _cell_angle_beta 94.818(13) _cell_angle_gamma 105.675(15) _cell_volume 1841.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4952 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8827 _exptl_absorpt_correction_T_max 0.9653 _exptl_absorpt_process_details ; Jacobson, R. (2001) Private communication ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.5666 _diffrn_measurement_method dtprofit.ref _diffrn_reflns_number 11967 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6315 _reflns_number_gt 4273 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 600 Slice: -70.0000 - 110.0000 Image width: 0.3000 Exp time: 24.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 45.2267 2theta: 19.2053 scan: Number of images: 600 Slice: -70.0000 - 110.0000 Image width: 0.3000 Exp time: 24.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 45.2267 2theta: 19.2053 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_orient_matrix_UB_11 0.0221 _diffrn_orient_matrix_UB_12 -0.0021 _diffrn_orient_matrix_UB_13 -0.1018 _diffrn_orient_matrix_UB_21 0.0025 _diffrn_orient_matrix_UB_22 0.0888 _diffrn_orient_matrix_UB_23 -0.0288 _diffrn_orient_matrix_UB_31 0.0582 _diffrn_orient_matrix_UB_32 0.0110 _diffrn_orient_matrix_UB_33 0.0045 _diffrn_orient_matrix_type d*Trek _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^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 none _refine_ls_extinction_coef 0.711 _refine_ls_number_reflns 6315 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.46240(3) 0.44452(3) 0.743825(19) 0.02344(12) Uani 1 1 d . . . S1 S 0.32198(11) 0.56506(10) 0.78615(6) 0.0276(3) Uani 1 1 d . . . C1 C 0.1857(4) 0.5392(4) 0.7078(2) 0.0263(10) Uani 1 1 d . . . C2 C 0.1320(4) 0.6412(4) 0.7082(3) 0.0307(11) Uani 1 1 d . . . H1 H 0.1719 0.7134 0.7480 0.037 Uiso 1 1 calc R . . C3 C 0.0233(5) 0.6415(4) 0.6533(3) 0.0362(12) Uani 1 1 d . . . H2 H -0.0106 0.7125 0.6548 0.043 Uiso 1 1 calc R . . C4 C -0.0346(5) 0.5354(5) 0.5962(3) 0.0383(12) Uani 1 1 d . . . H3 H -0.1088 0.5334 0.5574 0.046 Uiso 1 1 calc R . . C5 C 0.0141(4) 0.4328(4) 0.5950(3) 0.0308(11) Uani 1 1 d . . . H4 H -0.0289 0.3606 0.5558 0.037 Uiso 1 1 calc R . . C6 C 0.1252(4) 0.4308(4) 0.6496(2) 0.0258(10) Uani 1 1 d . . . C7 C 0.1747(5) 0.3118(4) 0.6445(3) 0.0306(11) Uani 1 1 d . . . C8 C 0.1394(6) 0.2310(5) 0.5600(3) 0.0460(14) Uani 1 1 d . . . F1 F 0.1884(3) 0.3010(3) 0.50587(16) 0.0569(9) Uani 1 1 d . . . F2 F 0.0025(3) 0.1752(3) 0.53355(19) 0.0674(10) Uani 1 1 d . . . F3 F 0.1999(3) 0.1381(3) 0.55402(17) 0.0611(9) Uani 1 1 d . . . C9 C 0.0938(5) 0.2334(5) 0.7022(3) 0.0431(13) Uani 1 1 d . . . F4 F 0.1211(3) 0.2926(3) 0.77806(18) 0.0634(9) Uani 1 1 d . . . F5 F -0.0473(3) 0.2042(2) 0.68485(19) 0.0530(8) Uani 1 1 d . . . F6 F 0.1205(3) 0.1231(3) 0.7004(2) 0.0637(10) Uani 1 1 d . . . O1 O 0.3098(3) 0.3253(2) 0.66173(17) 0.0267(7) Uani 1 1 d . . . P1 P 0.60743(11) 0.32770(10) 0.70662(6) 0.0213(3) Uani 1 1 d . . . C10 C 0.6152(4) 0.2963(4) 0.5998(2) 0.0285(11) Uani 1 1 d . . . C11 C 0.6055(5) 0.3882(4) 0.5555(3) 0.0336(12) Uani 1 1 d . . . H5 H 0.5899 0.4634 0.5803 0.040 Uiso 1 1 calc R . . C12 C 0.6188(5) 0.3694(5) 0.4751(3) 0.0375(12) Uani 1 1 d . . . H6 H 0.6131 0.4323 0.4451 0.045 Uiso 1 1 calc R . . C13 C 0.6401(5) 0.2605(5) 0.4386(3) 0.0445(13) Uani 1 1 d . . . H7 H 0.6484 0.2481 0.3834 0.053 Uiso 1 1 calc R . . C14 C 0.6495(5) 0.1686(5) 0.4822(3) 0.0530(15) Uani 1 1 d . . . H8 H 0.6638 0.0931 0.4570 0.064 Uiso 1 1 calc R . . C15 C 0.6379(5) 0.1874(4) 0.5636(3) 0.0385(12) Uani 1 1 d . . . H9 H 0.6457 0.1252 0.5938 0.046 Uiso 1 1 calc R . . C16 C 0.5602(4) 0.1777(4) 0.7381(2) 0.0240(10) Uani 1 1 d . . . C17 C 0.4255(5) 0.1011(4) 0.7098(2) 0.0275(11) Uani 1 1 d . . . H10 H 0.3660 0.1278 0.6748 0.033 Uiso 1 1 calc R . . C18 C 0.3787(5) -0.0134(4) 0.7326(2) 0.0282(11) Uani 1 1 d . . . H11 H 0.2870 -0.0650 0.7129 0.034 Uiso 1 1 calc R . . C19 C 0.4636(5) -0.0538(4) 0.7836(3) 0.0354(12) Uani 1 1 d . . . H12 H 0.4308 -0.1331 0.7987 0.043 Uiso 1 1 calc R . . C20 C 0.5963(5) 0.0218(4) 0.8124(3) 0.0367(12) Uani 1 1 d . . . H13 H 0.6551 -0.0049 0.8479 0.044 Uiso 1 1 calc R . . C21 C 0.6439(5) 0.1366(4) 0.7897(3) 0.0331(11) Uani 1 1 d . . . H14 H 0.7356 0.1880 0.8097 0.040 Uiso 1 1 calc R . . C22 C 0.7851(4) 0.4149(4) 0.7558(2) 0.0274(11) Uani 1 1 d . . . H15 H 0.8408 0.3561 0.7623 0.033 Uiso 1 1 calc R . . H16 H 0.8318 0.4739 0.7226 0.033 Uiso 1 1 calc R . . C23 C 0.7763(4) 0.4860(4) 0.8363(2) 0.0275(11) Uani 1 1 d . . . H17 H 0.8682 0.5453 0.8587 0.033 Uiso 1 1 calc R . . H18 H 0.7485 0.4273 0.8734 0.033 Uiso 1 1 calc R . . P2 P 0.64625(12) 0.57129(10) 0.82378(6) 0.0230(3) Uani 1 1 d . . . C24 C 0.6296(4) 0.6427(4) 0.9230(2) 0.0244(10) Uani 1 1 d . . . C25 C 0.6602(5) 0.5956(4) 0.9908(2) 0.0319(11) Uani 1 1 d . . . H19 H 0.6915 0.5230 0.9862 0.038 Uiso 1 1 calc R . . C26 C 0.6451(5) 0.6546(5) 1.0648(3) 0.0393(13) Uani 1 1 d . . . H20 H 0.6685 0.6229 1.1106 0.047 Uiso 1 1 calc R . . C27 C 0.5975(5) 0.7571(5) 1.0735(3) 0.0400(13) Uani 1 1 d . . . H21 H 0.5873 0.7962 1.1247 0.048 Uiso 1 1 calc R . . C28 C 0.5640(5) 0.8032(5) 1.0065(3) 0.0440(13) Uani 1 1 d . . . H22 H 0.5287 0.8735 1.0118 0.053 Uiso 1 1 calc R . . C29 C 0.5816(5) 0.7481(4) 0.9317(3) 0.0342(12) Uani 1 1 d . . . H23 H 0.5608 0.7821 0.8864 0.041 Uiso 1 1 calc R . . C30 C 0.7301(4) 0.7005(4) 0.7770(2) 0.0254(10) Uani 1 1 d . . . C31 C 0.8560(5) 0.7858(4) 0.8108(3) 0.0317(11) Uani 1 1 d . . . H24 H 0.9002 0.7775 0.8600 0.038 Uiso 1 1 calc R . . C32 C 0.9177(5) 0.8826(4) 0.7735(3) 0.0395(12) Uani 1 1 d . . . H25 H 1.0048 0.9398 0.7968 0.047 Uiso 1 1 calc R . . C33 C 0.8532(5) 0.8972(4) 0.7020(3) 0.0424(13) Uani 1 1 d . . . H26 H 0.8962 0.9643 0.6767 0.051 Uiso 1 1 calc R . . C34 C 0.7273(5) 0.8144(4) 0.6679(3) 0.0371(12) Uani 1 1 d . . . H27 H 0.6832 0.8239 0.6190 0.045 Uiso 1 1 calc R . . C35 C 0.6655(5) 0.7175(4) 0.7052(3) 0.0285(11) Uani 1 1 d . . . H28 H 0.5778 0.6612 0.6819 0.034 Uiso 1 1 calc R . . C36 C 0.8107(6) 0.2510(7) 1.0533(3) 0.0659(19) Uani 1 1 d . . . H29 H 0.7605 0.2835 1.0914 0.079 Uiso 1 1 calc R . . C37 C 0.8013(6) 0.1262(6) 1.0421(3) 0.0570(16) Uani 1 1 d . . . H30 H 0.7466 0.0712 1.0716 0.068 Uiso 1 1 calc R . . C38 C 0.8774(6) 0.0847(6) 0.9845(4) 0.0667(18) Uani 1 1 d . . . H31 H 0.8731 -0.0013 0.9737 0.080 Uiso 1 1 calc R . . C39 C 0.9586(6) 0.1664(7) 0.9430(4) 0.0700(19) Uani 1 1 d . . . H32 H 1.0114 0.1375 0.9050 0.084 Uiso 1 1 calc R . . C40 C 0.9617(6) 0.2897(6) 0.9575(4) 0.0613(17) Uani 1 1 d . . . H33 H 1.0159 0.3460 0.9285 0.074 Uiso 1 1 calc R . . C41 C 0.8913(6) 0.3308(6) 1.0105(4) 0.0605(18) Uani 1 1 d . . . H34 H 0.8954 0.4168 1.0199 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0274(2) 0.01980(19) 0.0233(2) 0.00393(15) 0.00409(15) 0.00671(15) S1 0.0307(7) 0.0242(6) 0.0284(6) -0.0015(5) 0.0036(5) 0.0120(5) C1 0.026(3) 0.025(2) 0.029(3) 0.010(2) 0.006(2) 0.006(2) C2 0.029(3) 0.031(3) 0.037(3) 0.011(2) 0.010(2) 0.012(2) C3 0.039(3) 0.032(3) 0.049(3) 0.018(2) 0.019(3) 0.018(2) C4 0.032(3) 0.048(3) 0.041(3) 0.011(3) 0.013(2) 0.019(3) C5 0.027(3) 0.037(3) 0.030(3) 0.009(2) 0.002(2) 0.011(2) C6 0.024(3) 0.030(3) 0.026(2) 0.011(2) 0.007(2) 0.009(2) C7 0.035(3) 0.019(2) 0.034(3) 0.003(2) -0.007(2) 0.006(2) C8 0.048(4) 0.036(3) 0.050(4) -0.003(3) -0.011(3) 0.016(3) F1 0.080(2) 0.072(2) 0.0315(17) 0.0005(16) 0.0047(16) 0.0469(19) F2 0.050(2) 0.054(2) 0.080(2) -0.0264(18) -0.0278(19) 0.0162(17) F3 0.072(2) 0.0433(18) 0.061(2) -0.0227(15) -0.0250(17) 0.0323(17) C9 0.029(3) 0.033(3) 0.068(4) 0.013(3) 0.009(3) 0.007(2) F4 0.081(2) 0.062(2) 0.0448(19) 0.0257(17) 0.0164(18) 0.0038(18) F5 0.0293(17) 0.0338(17) 0.098(2) 0.0162(16) 0.0158(16) 0.0074(13) F6 0.0445(19) 0.0380(18) 0.123(3) 0.040(2) 0.0249(19) 0.0181(15) O1 0.0221(17) 0.0204(16) 0.0349(18) -0.0037(14) 0.0014(14) 0.0071(13) P1 0.0242(6) 0.0188(6) 0.0212(6) 0.0025(5) 0.0050(5) 0.0066(5) C10 0.028(3) 0.027(3) 0.024(2) -0.001(2) 0.006(2) -0.001(2) C11 0.041(3) 0.033(3) 0.025(3) 0.002(2) 0.000(2) 0.010(2) C12 0.039(3) 0.047(3) 0.027(3) 0.010(2) 0.003(2) 0.010(2) C13 0.046(3) 0.056(4) 0.026(3) 0.003(3) 0.009(2) 0.006(3) C14 0.072(4) 0.046(3) 0.040(3) -0.007(3) 0.024(3) 0.018(3) C15 0.052(3) 0.037(3) 0.030(3) 0.008(2) 0.016(2) 0.015(3) C16 0.032(3) 0.023(2) 0.021(2) 0.001(2) 0.011(2) 0.012(2) C17 0.040(3) 0.026(3) 0.019(2) 0.005(2) 0.005(2) 0.013(2) C18 0.031(3) 0.023(2) 0.029(3) 0.004(2) 0.004(2) 0.004(2) C19 0.050(3) 0.025(3) 0.037(3) 0.015(2) 0.012(3) 0.014(2) C20 0.046(3) 0.029(3) 0.038(3) 0.013(2) -0.004(3) 0.016(2) C21 0.033(3) 0.030(3) 0.037(3) 0.006(2) 0.001(2) 0.011(2) C22 0.024(3) 0.029(3) 0.032(3) 0.013(2) 0.002(2) 0.008(2) C23 0.023(2) 0.029(3) 0.028(3) 0.004(2) -0.001(2) 0.005(2) P2 0.0285(7) 0.0221(6) 0.0187(6) 0.0029(5) 0.0020(5) 0.0087(5) C24 0.027(3) 0.022(2) 0.022(2) 0.003(2) 0.001(2) 0.005(2) C25 0.040(3) 0.032(3) 0.025(3) 0.006(2) 0.001(2) 0.011(2) C26 0.042(3) 0.048(3) 0.023(3) 0.013(2) 0.002(2) 0.003(3) C27 0.040(3) 0.047(3) 0.025(3) -0.004(2) 0.014(2) 0.002(3) C28 0.045(3) 0.043(3) 0.044(3) -0.008(3) 0.006(3) 0.022(3) C29 0.049(3) 0.035(3) 0.020(2) 0.004(2) 0.001(2) 0.017(2) C30 0.030(3) 0.020(2) 0.025(2) -0.0007(19) 0.011(2) 0.006(2) C31 0.039(3) 0.030(3) 0.027(3) 0.002(2) 0.009(2) 0.012(2) C32 0.034(3) 0.028(3) 0.047(3) -0.004(2) 0.006(3) -0.001(2) C33 0.054(4) 0.029(3) 0.051(3) 0.016(3) 0.026(3) 0.013(3) C34 0.048(3) 0.030(3) 0.039(3) 0.012(2) 0.011(3) 0.016(3) C35 0.033(3) 0.022(2) 0.030(3) 0.005(2) 0.007(2) 0.006(2) C36 0.037(4) 0.106(6) 0.048(4) -0.022(4) 0.002(3) 0.030(4) C37 0.042(4) 0.062(4) 0.056(4) 0.003(3) -0.009(3) 0.005(3) C38 0.048(4) 0.052(4) 0.087(5) -0.014(4) -0.012(4) 0.012(3) C39 0.048(4) 0.090(5) 0.063(4) -0.017(4) 0.010(3) 0.020(4) C40 0.052(4) 0.056(4) 0.061(4) 0.006(3) -0.014(3) 0.001(3) C41 0.051(4) 0.051(4) 0.065(4) -0.017(3) -0.026(3) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O1 2.026(3) . ? Pd1 P2 2.2152(13) . ? Pd1 P1 2.2855(13) . ? Pd1 S1 2.3009(13) . ? S1 C1 1.768(4) . ? C1 C2 1.399(5) . ? C1 C6 1.414(6) . ? C2 C3 1.383(6) . ? C2 H1 0.9500 . ? C3 C4 1.384(6) . ? C3 H2 0.9500 . ? C4 C5 1.374(6) . ? C4 H3 0.9500 . ? C5 C6 1.404(5) . ? C5 H4 0.9500 . ? C6 C7 1.549(6) . ? C7 O1 1.328(5) . ? C7 C8 1.552(6) . ? C7 C9 1.561(6) . ? C8 F3 1.344(5) . ? C8 F1 1.348(6) . ? C8 F2 1.356(5) . ? C9 F4 1.340(6) . ? C9 F6 1.341(5) . ? C9 F5 1.363(5) . ? P1 C16 1.810(4) . ? P1 C10 1.827(4) . ? P1 C22 1.850(4) . ? C10 C15 1.379(6) . ? C10 C11 1.394(6) . ? C11 C12 1.388(6) . ? C11 H5 0.9500 . ? C12 C13 1.375(6) . ? C12 H6 0.9500 . ? C13 C14 1.387(7) . ? C13 H7 0.9500 . ? C14 C15 1.400(6) . ? C14 H8 0.9500 . ? C15 H9 0.9500 . ? C16 C21 1.385(5) . ? C16 C17 1.396(6) . ? C17 C18 1.379(6) . ? C17 H10 0.9500 . ? C18 C19 1.382(5) . ? C18 H11 0.9500 . ? C19 C20 1.379(6) . ? C19 H12 0.9500 . ? C20 C21 1.383(6) . ? C20 H13 0.9500 . ? C21 H14 0.9500 . ? C22 C23 1.514(6) . ? C22 H15 0.9900 . ? C22 H16 0.9900 . ? C23 P2 1.839(4) . ? C23 H17 0.9900 . ? C23 H18 0.9900 . ? P2 C24 1.813(4) . ? P2 C30 1.814(4) . ? C24 C29 1.394(6) . ? C24 C25 1.396(5) . ? C25 C26 1.383(6) . ? C25 H19 0.9500 . ? C26 C27 1.362(6) . ? C26 H20 0.9500 . ? C27 C28 1.384(6) . ? C27 H21 0.9500 . ? C28 C29 1.388(6) . ? C28 H22 0.9500 . ? C29 H23 0.9500 . ? C30 C31 1.385(6) . ? C30 C35 1.408(5) . ? C31 C32 1.379(6) . ? C31 H24 0.9500 . ? C32 C33 1.393(6) . ? C32 H25 0.9500 . ? C33 C34 1.376(6) . ? C33 H26 0.9500 . ? C34 C35 1.381(6) . ? C34 H27 0.9500 . ? C35 H28 0.9500 . ? C36 C37 1.372(8) . ? C36 C41 1.383(8) . ? C36 H29 0.9500 . ? C37 C38 1.402(8) . ? C37 H30 0.9500 . ? C38 C39 1.385(8) . ? C38 H31 0.9500 . ? C39 C40 1.370(8) . ? C39 H32 0.9500 . ? C40 C41 1.306(8) . ? C40 H33 0.9500 . ? C41 H34 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pd1 P2 173.36(9) . . ? O1 Pd1 P1 88.64(9) . . ? P2 Pd1 P1 85.92(5) . . ? O1 Pd1 S1 93.48(9) . . ? P2 Pd1 S1 92.01(5) . . ? P1 Pd1 S1 177.69(4) . . ? C1 S1 Pd1 106.91(15) . . ? C2 C1 C6 118.8(4) . . ? C2 C1 S1 112.6(3) . . ? C6 C1 S1 128.5(3) . . ? C3 C2 C1 122.9(4) . . ? C3 C2 H1 118.6 . . ? C1 C2 H1 118.6 . . ? C2 C3 C4 117.9(4) . . ? C2 C3 H2 121.0 . . ? C4 C3 H2 121.0 . . ? C5 C4 C3 120.6(5) . . ? C5 C4 H3 119.7 . . ? C3 C4 H3 119.7 . . ? C4 C5 C6 122.4(4) . . ? C4 C5 H4 118.8 . . ? C6 C5 H4 118.8 . . ? C5 C6 C1 117.3(4) . . ? C5 C6 C7 119.5(4) . . ? C1 C6 C7 123.2(4) . . ? O1 C7 C6 118.3(4) . . ? O1 C7 C8 102.7(4) . . ? C6 C7 C8 112.7(3) . . ? O1 C7 C9 108.7(3) . . ? C6 C7 C9 106.0(4) . . ? C8 C7 C9 108.1(4) . . ? F3 C8 F1 106.3(5) . . ? F3 C8 F2 105.4(4) . . ? F1 C8 F2 105.9(4) . . ? F3 C8 C7 111.7(4) . . ? F1 C8 C7 110.3(4) . . ? F2 C8 C7 116.6(5) . . ? F4 C9 F6 107.5(4) . . ? F4 C9 F5 104.6(4) . . ? F6 C9 F5 104.8(4) . . ? F4 C9 C7 113.2(4) . . ? F6 C9 C7 112.5(4) . . ? F5 C9 C7 113.4(4) . . ? C7 O1 Pd1 133.7(3) . . ? C16 P1 C10 106.67(19) . . ? C16 P1 C22 107.96(19) . . ? C10 P1 C22 107.6(2) . . ? C16 P1 Pd1 112.09(14) . . ? C10 P1 Pd1 114.82(15) . . ? C22 P1 Pd1 107.44(15) . . ? C15 C10 C11 120.0(4) . . ? C15 C10 P1 121.3(3) . . ? C11 C10 P1 118.6(3) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H5 120.2 . . ? C10 C11 H5 120.2 . . ? C13 C12 C11 120.6(5) . . ? C13 C12 H6 119.7 . . ? C11 C12 H6 119.7 . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H7 120.0 . . ? C14 C13 H7 120.0 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H8 120.1 . . ? C15 C14 H8 120.1 . . ? C10 C15 C14 119.9(5) . . ? C10 C15 H9 120.1 . . ? C14 C15 H9 120.1 . . ? C21 C16 C17 118.5(4) . . ? C21 C16 P1 125.4(3) . . ? C17 C16 P1 116.0(3) . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H10 119.9 . . ? C16 C17 H10 119.9 . . ? C17 C18 C19 120.8(4) . . ? C17 C18 H11 119.6 . . ? C19 C18 H11 119.6 . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H12 120.3 . . ? C18 C19 H12 120.3 . . ? C19 C20 C21 120.0(4) . . ? C19 C20 H13 120.0 . . ? C21 C20 H13 120.0 . . ? C20 C21 C16 121.1(4) . . ? C20 C21 H14 119.5 . . ? C16 C21 H14 119.5 . . ? C23 C22 P1 109.4(3) . . ? C23 C22 H15 109.8 . . ? P1 C22 H15 109.8 . . ? C23 C22 H16 109.8 . . ? P1 C22 H16 109.8 . . ? H15 C22 H16 108.3 . . ? C22 C23 P2 108.4(3) . . ? C22 C23 H17 110.0 . . ? P2 C23 H17 110.0 . . ? C22 C23 H18 110.0 . . ? P2 C23 H18 110.0 . . ? H17 C23 H18 108.4 . . ? C24 P2 C30 105.02(19) . . ? C24 P2 C23 106.09(19) . . ? C30 P2 C23 105.1(2) . . ? C24 P2 Pd1 121.02(15) . . ? C30 P2 Pd1 110.31(14) . . ? C23 P2 Pd1 108.20(14) . . ? C29 C24 C25 118.5(4) . . ? C29 C24 P2 118.5(3) . . ? C25 C24 P2 122.9(3) . . ? C26 C25 C24 120.0(4) . . ? C26 C25 H19 120.0 . . ? C24 C25 H19 120.0 . . ? C27 C26 C25 121.6(4) . . ? C27 C26 H20 119.2 . . ? C25 C26 H20 119.2 . . ? C26 C27 C28 119.0(4) . . ? C26 C27 H21 120.5 . . ? C28 C27 H21 120.5 . . ? C27 C28 C29 120.7(5) . . ? C27 C28 H22 119.6 . . ? C29 C28 H22 119.6 . . ? C28 C29 C24 120.1(4) . . ? C28 C29 H23 119.9 . . ? C24 C29 H23 119.9 . . ? C31 C30 C35 118.3(4) . . ? C31 C30 P2 121.8(3) . . ? C35 C30 P2 119.9(3) . . ? C32 C31 C30 120.5(4) . . ? C32 C31 H24 119.7 . . ? C30 C31 H24 119.7 . . ? C31 C32 C33 120.5(4) . . ? C31 C32 H25 119.8 . . ? C33 C32 H25 119.8 . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H26 120.0 . . ? C32 C33 H26 120.0 . . ? C33 C34 C35 119.6(4) . . ? C33 C34 H27 120.2 . . ? C35 C34 H27 120.2 . . ? C34 C35 C30 121.2(4) . . ? C34 C35 H28 119.4 . . ? C30 C35 H28 119.4 . . ? C37 C36 C41 121.8(6) . . ? C37 C36 H29 119.1 . . ? C41 C36 H29 119.1 . . ? C36 C37 C38 116.0(6) . . ? C36 C37 H30 122.0 . . ? C38 C37 H30 122.0 . . ? C39 C38 C37 121.3(6) . . ? C39 C38 H31 119.4 . . ? C37 C38 H31 119.4 . . ? C40 C39 C38 119.0(6) . . ? C40 C39 H32 120.5 . . ? C38 C39 H32 120.5 . . ? C41 C40 C39 121.0(6) . . ? C41 C40 H33 119.5 . . ? C39 C40 H33 119.5 . . ? C40 C41 C36 120.9(6) . . ? C40 C41 H34 119.5 . . ? C36 C41 H34 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pd1 S1 C1 -22.32(17) . . . . ? P2 Pd1 S1 C1 153.95(15) . . . . ? Pd1 S1 C1 C2 -152.6(3) . . . . ? Pd1 S1 C1 C6 29.6(4) . . . . ? C6 C1 C2 C3 -1.0(7) . . . . ? S1 C1 C2 C3 -179.0(3) . . . . ? C1 C2 C3 C4 0.5(7) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C3 C4 C5 C6 -1.3(7) . . . . ? C4 C5 C6 C1 0.8(6) . . . . ? C4 C5 C6 C7 -179.9(4) . . . . ? C2 C1 C6 C5 0.3(6) . . . . ? S1 C1 C6 C5 177.9(3) . . . . ? C2 C1 C6 C7 -179.0(4) . . . . ? S1 C1 C6 C7 -1.3(6) . . . . ? C5 C6 C7 O1 144.5(4) . . . . ? C1 C6 C7 O1 -36.3(6) . . . . ? C5 C6 C7 C8 24.7(6) . . . . ? C1 C6 C7 C8 -156.0(4) . . . . ? C5 C6 C7 C9 -93.3(5) . . . . ? C1 C6 C7 C9 86.0(5) . . . . ? O1 C7 C8 F3 42.9(5) . . . . ? C6 C7 C8 F3 171.3(4) . . . . ? C9 C7 C8 F3 -71.9(5) . . . . ? O1 C7 C8 F1 -75.0(4) . . . . ? C6 C7 C8 F1 53.4(5) . . . . ? C9 C7 C8 F1 170.1(4) . . . . ? O1 C7 C8 F2 164.1(4) . . . . ? C6 C7 C8 F2 -67.5(5) . . . . ? C9 C7 C8 F2 49.3(5) . . . . ? O1 C7 C9 F4 66.7(5) . . . . ? C6 C7 C9 F4 -61.5(5) . . . . ? C8 C7 C9 F4 177.5(4) . . . . ? O1 C7 C9 F6 -55.5(5) . . . . ? C6 C7 C9 F6 176.3(4) . . . . ? C8 C7 C9 F6 55.3(5) . . . . ? O1 C7 C9 F5 -174.3(4) . . . . ? C6 C7 C9 F5 57.5(5) . . . . ? C8 C7 C9 F5 -63.5(5) . . . . ? C6 C7 O1 Pd1 38.1(6) . . . . ? C8 C7 O1 Pd1 162.9(3) . . . . ? C9 C7 O1 Pd1 -82.7(4) . . . . ? P1 Pd1 O1 C7 172.1(4) . . . . ? S1 Pd1 O1 C7 -7.0(4) . . . . ? O1 Pd1 P1 C16 -70.94(17) . . . . ? P2 Pd1 P1 C16 112.88(15) . . . . ? O1 Pd1 P1 C10 50.99(17) . . . . ? P2 Pd1 P1 C10 -125.20(16) . . . . ? O1 Pd1 P1 C22 170.62(16) . . . . ? P2 Pd1 P1 C22 -5.57(14) . . . . ? C16 P1 C10 C15 -23.7(4) . . . . ? C22 P1 C10 C15 92.0(4) . . . . ? Pd1 P1 C10 C15 -148.5(3) . . . . ? C16 P1 C10 C11 159.9(3) . . . . ? C22 P1 C10 C11 -84.4(4) . . . . ? Pd1 P1 C10 C11 35.1(4) . . . . ? C15 C10 C11 C12 0.0(7) . . . . ? P1 C10 C11 C12 176.5(3) . . . . ? C10 C11 C12 C13 0.6(7) . . . . ? C11 C12 C13 C14 -0.5(8) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C11 C10 C15 C14 -0.8(7) . . . . ? P1 C10 C15 C14 -177.2(4) . . . . ? C13 C14 C15 C10 0.9(8) . . . . ? C10 P1 C16 C21 115.1(4) . . . . ? C22 P1 C16 C21 -0.3(4) . . . . ? Pd1 P1 C16 C21 -118.4(4) . . . . ? C10 P1 C16 C17 -67.7(4) . . . . ? C22 P1 C16 C17 176.9(3) . . . . ? Pd1 P1 C16 C17 58.7(3) . . . . ? C21 C16 C17 C18 -0.6(6) . . . . ? P1 C16 C17 C18 -178.0(3) . . . . ? C16 C17 C18 C19 0.1(7) . . . . ? C17 C18 C19 C20 0.5(7) . . . . ? C18 C19 C20 C21 -0.6(7) . . . . ? C19 C20 C21 C16 0.1(7) . . . . ? C17 C16 C21 C20 0.5(7) . . . . ? P1 C16 C21 C20 177.6(4) . . . . ? C16 P1 C22 C23 -87.4(3) . . . . ? C10 P1 C22 C23 157.8(3) . . . . ? Pd1 P1 C22 C23 33.7(3) . . . . ? P1 C22 C23 P2 -48.8(3) . . . . ? C22 C23 P2 C24 175.1(3) . . . . ? C22 C23 P2 C30 -74.0(3) . . . . ? C22 C23 P2 Pd1 43.8(3) . . . . ? P1 Pd1 P2 C24 -140.43(16) . . . . ? S1 Pd1 P2 C24 38.53(16) . . . . ? P1 Pd1 P2 C30 96.55(15) . . . . ? S1 Pd1 P2 C30 -84.49(15) . . . . ? P1 Pd1 P2 C23 -17.88(15) . . . . ? S1 Pd1 P2 C23 161.08(15) . . . . ? C30 P2 C24 C29 45.2(4) . . . . ? C23 P2 C24 C29 156.1(4) . . . . ? Pd1 P2 C24 C29 -80.3(4) . . . . ? C30 P2 C24 C25 -136.1(4) . . . . ? C23 P2 C24 C25 -25.1(4) . . . . ? Pd1 P2 C24 C25 98.4(4) . . . . ? C29 C24 C25 C26 -1.2(7) . . . . ? P2 C24 C25 C26 -179.9(3) . . . . ? C24 C25 C26 C27 1.6(7) . . . . ? C25 C26 C27 C28 -0.3(7) . . . . ? C26 C27 C28 C29 -1.4(7) . . . . ? C27 C28 C29 C24 1.8(8) . . . . ? C25 C24 C29 C28 -0.5(7) . . . . ? P2 C24 C29 C28 178.3(4) . . . . ? C24 P2 C30 C31 55.2(4) . . . . ? C23 P2 C30 C31 -56.5(4) . . . . ? Pd1 P2 C30 C31 -172.9(3) . . . . ? C24 P2 C30 C35 -123.5(3) . . . . ? C23 P2 C30 C35 124.8(3) . . . . ? Pd1 P2 C30 C35 8.4(4) . . . . ? C35 C30 C31 C32 -1.7(6) . . . . ? P2 C30 C31 C32 179.5(3) . . . . ? C30 C31 C32 C33 1.0(7) . . . . ? C31 C32 C33 C34 -0.2(7) . . . . ? C32 C33 C34 C35 0.2(7) . . . . ? C33 C34 C35 C30 -1.0(7) . . . . ? C31 C30 C35 C34 1.7(6) . . . . ? P2 C30 C35 C34 -179.5(3) . . . . ? C41 C36 C37 C38 -0.4(8) . . . . ? C36 C37 C38 C39 1.2(8) . . . . ? C37 C38 C39 C40 -1.5(9) . . . . ? C38 C39 C40 C41 1.1(9) . . . . ? C39 C40 C41 C36 -0.4(9) . . . . ? C37 C36 C41 C40 0.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.232 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.092