Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Athanasia Dervisi' 'Simon Coles' 'Michael B. Hursthouse' 'Robert L. Jenkins' 'K. M. Abdul Malik' _publ_contact_author_name 'Dr Athanasia Dervisi' _publ_contact_author_address ; Dr Athanasia Dervisi Department of Chemistry Cardiff University PO Box 912 Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email DERVISIA@CF.AC.UK _publ_section_title ; The synthesis of new chiral phosphino-thiol and -thioether ligands and their late transition metal chemistry. ; data_1 _database_code_CSD 194251 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36.4 Cl2 Ni2 O0.20 P2 S2' _chemical_formula_weight 738.59 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.523(2) _cell_length_b 12.031(2) _cell_length_c 13.325(3) _cell_angle_alpha 76.37(3) _cell_angle_beta 79.93(3) _cell_angle_gamma 65.29(3) _cell_volume 1624.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17257 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 1.573 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.6852 _exptl_absorpt_correction_T_max 0.8337 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 26806 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7363 _reflns_number_gt 6188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, Pearce 1993)' _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^)+(0.0334P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7363 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.2153(7) 0.4931(7) 0.0387(6) 0.0392(18) Uiso 0.20 1 d P . . C1 C 0.61635(17) 0.28443(16) 0.16058(13) 0.0180(4) Uani 1 1 d . . . C2 C 0.72930(18) 0.25890(18) 0.09596(14) 0.0257(4) Uani 1 1 d . . . H2 H 0.8049 0.2528 0.1203 0.031 Uiso 1 1 calc R . . C3 C 0.7319(2) 0.2423(2) -0.00408(16) 0.0340(5) Uani 1 1 d . . . H3 H 0.8096 0.2238 -0.0477 0.041 Uiso 1 1 calc R . . C4 C 0.6223(2) 0.25251(19) -0.04056(15) 0.0286(5) Uani 1 1 d . . . H4 H 0.6248 0.2403 -0.1089 0.034 Uiso 1 1 calc R . . C5 C 0.5093(2) 0.28043(19) 0.02218(15) 0.0289(5) Uani 1 1 d . . . H5 H 0.4334 0.2891 -0.0034 0.035 Uiso 1 1 calc R . . C6 C 0.50571(19) 0.29597(19) 0.12261(15) 0.0262(4) Uani 1 1 d . . . H6 H 0.4276 0.3146 0.1658 0.031 Uiso 1 1 calc R . . C7 C 0.47036(16) 0.41672(16) 0.33143(14) 0.0175(4) Uani 1 1 d . . . C8 C 0.43506(18) 0.41700(18) 0.43658(14) 0.0249(4) Uani 1 1 d . . . H8 H 0.4852 0.3505 0.4858 0.030 Uiso 1 1 calc R . . C9 C 0.32753(18) 0.51304(18) 0.47085(15) 0.0260(4) Uani 1 1 d . . . H9 H 0.3043 0.5124 0.5429 0.031 Uiso 1 1 calc R . . C10 C 0.25470(17) 0.60959(17) 0.39888(15) 0.0230(4) Uani 1 1 d . . . H10 H 0.1805 0.6751 0.4216 0.028 Uiso 1 1 calc R . . C11 C 0.28947(17) 0.61105(17) 0.29427(15) 0.0230(4) Uani 1 1 d . . . H11 H 0.2392 0.6779 0.2453 0.028 Uiso 1 1 calc R . . C12 C 0.39758(17) 0.51540(17) 0.25986(14) 0.0206(4) Uani 1 1 d . . . H12 H 0.4216 0.5175 0.1877 0.025 Uiso 1 1 calc R . . C13 C 0.60320(17) 0.14755(16) 0.36790(14) 0.0198(4) Uani 1 1 d . . . H13A H 0.5581 0.1605 0.4372 0.024 Uiso 1 1 calc R . . H13B H 0.5535 0.1223 0.3308 0.024 Uiso 1 1 calc R . . C14 C 0.73813(16) 0.04664(16) 0.37880(14) 0.0177(4) Uani 1 1 d . . . H14 H 0.7776 0.0252 0.3092 0.021 Uiso 1 1 calc R . . C15 C 0.74283(18) -0.07128(17) 0.45464(14) 0.0227(4) Uani 1 1 d . . . H15A H 0.6972 -0.0489 0.5218 0.027 Uiso 1 1 calc R . . H15B H 0.8333 -0.1259 0.4666 0.027 Uiso 1 1 calc R . . C16 C 0.6825(2) -0.14271(19) 0.41577(17) 0.0323(5) Uani 1 1 d . . . H16A H 0.5917 -0.0906 0.4071 0.048 Uiso 1 1 calc R . . H16B H 0.6900 -0.2188 0.4662 0.048 Uiso 1 1 calc R . . H16C H 0.7269 -0.1647 0.3491 0.048 Uiso 1 1 calc R . . C17 C 1.33003(16) -0.00873(17) 0.21926(13) 0.0176(4) Uani 1 1 d . . . C18 C 1.35713(17) -0.12212(16) 0.28661(13) 0.0195(4) Uani 1 1 d . . . H18 H 1.2926 -0.1353 0.3369 0.023 Uiso 1 1 calc R . . C19 C 1.47923(17) -0.21666(17) 0.28033(14) 0.0222(4) Uani 1 1 d . . . H19 H 1.4969 -0.2951 0.3250 0.027 Uiso 1 1 calc R . . C20 C 1.57471(17) -0.19645(18) 0.20910(14) 0.0240(4) Uani 1 1 d . . . H20 H 1.6579 -0.2609 0.2053 0.029 Uiso 1 1 calc R . . C21 C 1.54923(18) -0.08281(18) 0.14367(15) 0.0264(4) Uani 1 1 d . . . H21 H 1.6154 -0.0685 0.0960 0.032 Uiso 1 1 calc R . . C22 C 1.42648(18) 0.01096(18) 0.14753(15) 0.0239(4) Uani 1 1 d . . . H22 H 1.4085 0.0883 0.1013 0.029 Uiso 1 1 calc R . . C23 C 1.13270(16) 0.16133(17) 0.08831(13) 0.0197(4) Uani 1 1 d . . . C24 C 1.12605(19) 0.07304(19) 0.04120(14) 0.0264(4) Uani 1 1 d . . . H24 H 1.1411 -0.0083 0.0797 0.032 Uiso 1 1 calc R . . C25 C 1.0978(2) 0.1017(2) -0.06108(15) 0.0304(5) Uani 1 1 d . . . H25 H 1.0936 0.0402 -0.0921 0.036 Uiso 1 1 calc R . . C26 C 1.07582(19) 0.2194(2) -0.11784(15) 0.0300(5) Uani 1 1 d . . . H26 H 1.0563 0.2393 -0.1879 0.036 Uiso 1 1 calc R . . C27 C 1.0824(2) 0.3083(2) -0.07222(15) 0.0339(5) Uani 1 1 d . . . H27 H 1.0673 0.3894 -0.1111 0.041 Uiso 1 1 calc R . . C28 C 1.11089(19) 0.27984(18) 0.03033(15) 0.0290(5) Uani 1 1 d . . . H28 H 1.1155 0.3414 0.0610 0.035 Uiso 1 1 calc R . . C29 C 1.19501(17) 0.24527(17) 0.25213(14) 0.0207(4) Uani 1 1 d . . . H29A H 1.2526 0.2142 0.3086 0.025 Uiso 1 1 calc R . . H29B H 1.2362 0.2829 0.1901 0.025 Uiso 1 1 calc R . . C30 C 1.06671(17) 0.34368(16) 0.28499(14) 0.0182(4) Uani 1 1 d . . . H30 H 1.0167 0.3880 0.2231 0.022 Uiso 1 1 calc R . . C31 C 1.08566(18) 0.43824(17) 0.33235(15) 0.0245(4) Uani 1 1 d . . . H31A H 1.1370 0.3932 0.3925 0.029 Uiso 1 1 calc R . . H31B H 1.1358 0.4783 0.2805 0.029 Uiso 1 1 calc R . . C32 C 0.96192(18) 0.53956(17) 0.36791(15) 0.0260(4) Uani 1 1 d . . . H32A H 0.9061 0.5792 0.3110 0.039 Uiso 1 1 calc R . . H32B H 0.9821 0.6021 0.3884 0.039 Uiso 1 1 calc R . . H32C H 0.9180 0.5025 0.4272 0.039 Uiso 1 1 calc R . . P1 P 0.61730(4) 0.29205(4) 0.29464(3) 0.01602(11) Uani 1 1 d . . . P8 P 1.17101(4) 0.11561(4) 0.22289(4) 0.01678(11) Uani 1 1 d . . . S1 S 0.83080(4) 0.11517(4) 0.42613(3) 0.01640(10) Uani 1 1 d . . . S2 S 0.97960(4) 0.25989(4) 0.37949(3) 0.01635(10) Uani 1 1 d . . . Ni1 Ni 0.78980(2) 0.29655(2) 0.329996(16) 0.01501(7) Uani 1 1 d . . . Ni2 Ni 1.01611(2) 0.08871(2) 0.328525(16) 0.01521(7) Uani 1 1 d . . . Cl1 Cl 0.75224(4) 0.47507(4) 0.22532(4) 0.02356(11) Uani 1 1 d . . . Cl2 Cl 1.04032(4) -0.08175(4) 0.28034(3) 0.02152(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0204(9) 0.0137(9) 0.0201(9) -0.0023(7) -0.0029(7) -0.0069(7) C2 0.0198(10) 0.0318(11) 0.0256(11) -0.0101(9) -0.0010(8) -0.0081(9) C3 0.0334(12) 0.0441(14) 0.0264(11) -0.0150(10) 0.0064(9) -0.0162(10) C4 0.0414(13) 0.0288(11) 0.0200(10) -0.0054(8) -0.0033(9) -0.0173(10) C5 0.0323(12) 0.0335(12) 0.0283(11) -0.0044(9) -0.0067(9) -0.0191(10) C6 0.0247(10) 0.0340(12) 0.0258(11) -0.0092(9) 0.0017(8) -0.0165(9) C7 0.0152(9) 0.0172(9) 0.0225(10) -0.0062(7) -0.0014(7) -0.0074(7) C8 0.0244(10) 0.0266(11) 0.0225(10) -0.0047(8) -0.0053(8) -0.0075(8) C9 0.0277(11) 0.0302(11) 0.0215(10) -0.0117(8) 0.0035(8) -0.0114(9) C10 0.0174(10) 0.0206(10) 0.0320(11) -0.0102(8) 0.0036(8) -0.0079(8) C11 0.0187(10) 0.0183(10) 0.0286(11) -0.0020(8) -0.0012(8) -0.0056(8) C12 0.0189(9) 0.0199(10) 0.0221(10) -0.0034(8) 0.0004(7) -0.0078(8) C13 0.0166(9) 0.0191(9) 0.0238(10) -0.0026(8) 0.0008(7) -0.0089(8) C14 0.0178(9) 0.0171(9) 0.0195(9) -0.0030(7) -0.0023(7) -0.0079(7) C15 0.0243(10) 0.0204(10) 0.0238(10) 0.0025(8) -0.0068(8) -0.0108(8) C16 0.0344(12) 0.0237(11) 0.0439(13) -0.0011(9) -0.0071(10) -0.0177(10) C17 0.0154(9) 0.0197(9) 0.0180(9) -0.0068(7) -0.0012(7) -0.0055(7) C18 0.0200(9) 0.0222(10) 0.0169(9) -0.0048(7) 0.0000(7) -0.0089(8) C19 0.0235(10) 0.0197(10) 0.0231(10) -0.0027(8) -0.0082(8) -0.0067(8) C20 0.0155(9) 0.0266(11) 0.0276(11) -0.0108(8) -0.0047(8) -0.0019(8) C21 0.0170(10) 0.0304(11) 0.0295(11) -0.0078(9) 0.0046(8) -0.0085(8) C22 0.0218(10) 0.0203(10) 0.0257(10) -0.0011(8) 0.0010(8) -0.0073(8) C23 0.0156(9) 0.0214(10) 0.0198(10) -0.0034(8) 0.0006(7) -0.0060(8) C24 0.0321(11) 0.0258(11) 0.0232(10) -0.0005(8) -0.0024(8) -0.0154(9) C25 0.0359(12) 0.0387(13) 0.0247(11) -0.0037(9) -0.0043(9) -0.0229(10) C26 0.0278(11) 0.0400(13) 0.0208(10) 0.0015(9) -0.0046(8) -0.0149(10) C27 0.0421(13) 0.0268(11) 0.0244(11) 0.0051(9) -0.0036(9) -0.0105(10) C28 0.0370(12) 0.0217(10) 0.0270(11) -0.0052(8) 0.0013(9) -0.0115(9) C29 0.0186(9) 0.0210(10) 0.0247(10) -0.0051(8) -0.0006(7) -0.0098(8) C30 0.0181(9) 0.0174(9) 0.0206(9) -0.0038(7) 0.0007(7) -0.0092(8) C31 0.0233(10) 0.0236(10) 0.0320(11) -0.0108(8) -0.0003(8) -0.0122(8) C32 0.0301(11) 0.0215(10) 0.0291(11) -0.0085(8) -0.0019(8) -0.0111(9) P1 0.0143(2) 0.0148(2) 0.0179(2) -0.00206(18) -0.00133(17) -0.00529(18) P8 0.0149(2) 0.0154(2) 0.0194(2) -0.00367(18) -0.00018(18) -0.00560(19) S1 0.0167(2) 0.0163(2) 0.0159(2) -0.00140(17) -0.00115(17) -0.00708(18) S2 0.0154(2) 0.0165(2) 0.0182(2) -0.00458(17) -0.00132(17) -0.00664(18) Ni1 0.01384(13) 0.01278(12) 0.01784(13) -0.00228(9) -0.00111(9) -0.00507(9) Ni2 0.01399(13) 0.01354(13) 0.01791(13) -0.00329(9) -0.00060(9) -0.00531(9) Cl1 0.0236(2) 0.0152(2) 0.0307(3) 0.00190(18) -0.00620(19) -0.00812(19) Cl2 0.0197(2) 0.0165(2) 0.0294(3) -0.00797(18) -0.00070(18) -0.00667(18) _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 C1 C2 1.389(3) . ? C1 C6 1.395(3) . ? C1 P1 1.8124(18) . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? C4 C5 1.376(3) . ? C4 H4 0.9500 . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.389(3) . ? C7 C12 1.391(3) . ? C7 P1 1.8140(19) . ? C8 C9 1.390(3) . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C12 1.392(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.527(2) . ? C13 P1 1.8391(19) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.522(3) . ? C14 S1 1.8532(18) . ? C14 H14 1.0000 . ? C15 C16 1.525(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.389(3) . ? C17 C22 1.395(3) . ? C17 P8 1.8193(19) . ? C18 C19 1.395(3) . ? C18 H18 0.9500 . ? C19 C20 1.386(3) . ? C19 H19 0.9500 . ? C20 C21 1.381(3) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.388(3) . ? C23 C28 1.394(3) . ? C23 P8 1.8228(19) . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.382(3) . ? C26 H26 0.9500 . ? C27 C28 1.391(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.528(2) . ? C29 P8 1.8294(18) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.528(2) . ? C30 S2 1.8479(19) . ? C30 H30 1.0000 . ? C31 C32 1.525(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? P1 Ni1 2.1460(7) . ? P8 Ni2 2.1591(9) . ? S1 Ni1 2.1583(9) . ? S1 Ni2 2.2378(9) . ? S2 Ni2 2.1713(7) . ? S2 Ni1 2.2303(7) . ? Ni1 Cl1 2.1835(9) . ? Ni1 Ni2 2.7583(12) . ? Ni2 Cl2 2.1853(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.10(17) . . ? C2 C1 P1 119.69(14) . . ? C6 C1 P1 121.08(14) . . ? C3 C2 C1 120.04(18) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.44(19) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.92(18) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.21(19) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.27(18) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C8 C7 C12 119.11(17) . . ? C8 C7 P1 117.64(14) . . ? C12 C7 P1 123.08(14) . . ? C9 C8 C7 121.02(18) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.32(18) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.23(17) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.51(18) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 119.80(18) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 P1 108.16(12) . . ? C14 C13 H13A 110.1 . . ? P1 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? P1 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? C15 C14 C13 113.92(15) . . ? C15 C14 S1 108.80(12) . . ? C13 C14 S1 106.24(12) . . ? C15 C14 H14 109.3 . . ? C13 C14 H14 109.3 . . ? S1 C14 H14 109.3 . . ? C14 C15 C16 112.59(16) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.59(16) . . ? C18 C17 P8 121.33(14) . . ? C22 C17 P8 119.08(14) . . ? C17 C18 C19 119.97(17) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.15(18) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.14(17) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.04(18) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 120.07(18) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C24 C23 C28 118.53(17) . . ? C24 C23 P8 118.15(14) . . ? C28 C23 P8 123.33(14) . . ? C25 C24 C23 121.04(19) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 120.07(19) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 119.64(18) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 120.4(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 120.30(19) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? C30 C29 P8 110.35(12) . . ? C30 C29 H29A 109.6 . . ? P8 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? P8 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 111.42(15) . . ? C29 C30 S2 106.74(13) . . ? C31 C30 S2 111.08(12) . . ? C29 C30 H30 109.2 . . ? C31 C30 H30 109.2 . . ? S2 C30 H30 109.2 . . ? C32 C31 C30 114.78(16) . . ? C32 C31 H31A 108.6 . . ? C30 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? C30 C31 H31B 108.6 . . ? H31A C31 H31B 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 P1 C7 108.64(9) . . ? C1 P1 C13 104.05(9) . . ? C7 P1 C13 105.37(9) . . ? C1 P1 Ni1 114.29(7) . . ? C7 P1 Ni1 114.95(6) . . ? C13 P1 Ni1 108.61(7) . . ? C17 P8 C23 103.83(9) . . ? C17 P8 C29 104.91(9) . . ? C23 P8 C29 105.89(9) . . ? C17 P8 Ni2 120.83(7) . . ? C23 P8 Ni2 112.32(6) . . ? C29 P8 Ni2 107.94(7) . . ? C14 S1 Ni1 105.69(6) . . ? C14 S1 Ni2 110.96(6) . . ? Ni1 S1 Ni2 77.70(4) . . ? C30 S2 Ni2 108.11(6) . . ? C30 S2 Ni1 112.52(7) . . ? Ni2 S2 Ni1 77.59(3) . . ? P1 Ni1 S1 88.52(4) . . ? P1 Ni1 Cl1 90.90(4) . . ? S1 Ni1 Cl1 176.855(19) . . ? P1 Ni1 S2 168.27(2) . . ? S1 Ni1 S2 80.06(4) . . ? Cl1 Ni1 S2 100.35(4) . . ? P1 Ni1 Ni2 119.90(3) . . ? S1 Ni1 Ni2 52.44(3) . . ? Cl1 Ni1 Ni2 125.54(3) . . ? S2 Ni1 Ni2 50.25(2) . . ? P8 Ni2 S2 88.49(4) . . ? P8 Ni2 Cl2 94.76(3) . . ? S2 Ni2 Cl2 176.412(19) . . ? P8 Ni2 S1 164.92(2) . . ? S2 Ni2 S1 79.61(4) . . ? Cl2 Ni2 S1 96.93(4) . . ? P8 Ni2 Ni1 115.25(3) . . ? S2 Ni2 Ni1 52.16(2) . . ? Cl2 Ni2 Ni1 124.75(3) . . ? S1 Ni2 Ni1 49.86(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.399 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.090 data_2 _database_code_CSD 194252 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Cl2 P2 Pd2 S2' _chemical_formula_weight 830.37 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.955(3) _cell_length_b 14.401(3) _cell_length_c 15.281(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.33(3) _cell_angle_gamma 90.00 _cell_volume 3288.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 51836 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.502 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.8403 _exptl_absorpt_correction_T_max 0.9706 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 30723 _diffrn_reflns_av_R_equivalents 0.1167 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7500 _reflns_number_gt 5123 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0405P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7500 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3243(3) 0.3265(3) 0.0138(3) 0.0233(9) Uani 1 1 d . . . H1 H 0.2591 0.3418 0.0138 0.028 Uiso 1 1 calc R . . C2 C 0.3367(3) 0.2322(3) -0.0304(3) 0.0299(10) Uani 1 1 d . . . H2A H 0.3222 0.2384 -0.0940 0.036 Uiso 1 1 calc R . . H2B H 0.4001 0.2132 -0.0231 0.036 Uiso 1 1 calc R . . C3 C 0.2781(3) 0.1575(3) 0.0068(3) 0.0386(12) Uani 1 1 d . . . H3A H 0.2928 0.1503 0.0696 0.058 Uiso 1 1 calc R . . H3B H 0.2887 0.0986 -0.0232 0.058 Uiso 1 1 calc R . . H3C H 0.2151 0.1751 -0.0018 0.058 Uiso 1 1 calc R . . C4 C 0.3641(3) 0.3325(3) 0.1064(3) 0.0225(9) Uani 1 1 d . . . H4A H 0.4272 0.3115 0.1076 0.027 Uiso 1 1 calc R . . H4B H 0.3306 0.2912 0.1453 0.027 Uiso 1 1 calc R . . C5 C 0.4432(3) 0.4624(3) 0.2342(2) 0.0202(9) Uani 1 1 d . . . C6 C 0.4636(3) 0.3878(3) 0.2908(3) 0.0265(10) Uani 1 1 d . . . H6 H 0.4303 0.3318 0.2858 0.032 Uiso 1 1 calc R . . C7 C 0.5324(3) 0.3960(3) 0.3538(3) 0.0315(10) Uani 1 1 d . . . H7 H 0.5457 0.3457 0.3924 0.038 Uiso 1 1 calc R . . C8 C 0.5824(3) 0.4777(3) 0.3608(3) 0.0328(11) Uani 1 1 d . . . H8 H 0.6302 0.4827 0.4034 0.039 Uiso 1 1 calc R . . C9 C 0.5620(3) 0.5508(3) 0.3059(3) 0.0291(10) Uani 1 1 d . . . H9 H 0.5953 0.6069 0.3113 0.035 Uiso 1 1 calc R . . C10 C 0.4930(3) 0.5435(3) 0.2424(3) 0.0229(9) Uani 1 1 d . . . H10 H 0.4799 0.5944 0.2044 0.027 Uiso 1 1 calc R . . C11 C 0.2497(3) 0.4621(3) 0.1949(3) 0.0261(10) Uani 1 1 d . . . C12 C 0.2266(3) 0.4019(4) 0.2616(3) 0.0392(12) Uani 1 1 d . . . H12 H 0.2677 0.3556 0.2820 0.047 Uiso 1 1 calc R . . C13 C 0.1435(3) 0.4095(5) 0.2985(3) 0.0532(15) Uani 1 1 d . . . H13 H 0.1277 0.3682 0.3438 0.064 Uiso 1 1 calc R . . C14 C 0.0841(3) 0.4766(4) 0.2695(4) 0.0509(16) Uani 1 1 d . . . H14 H 0.0277 0.4821 0.2954 0.061 Uiso 1 1 calc R . . C15 C 0.1055(3) 0.5352(4) 0.2038(4) 0.0463(14) Uani 1 1 d . . . H15 H 0.0638 0.5808 0.1836 0.056 Uiso 1 1 calc R . . C16 C 0.1885(3) 0.5284(3) 0.1662(3) 0.0350(11) Uani 1 1 d . . . H16 H 0.2032 0.5696 0.1204 0.042 Uiso 1 1 calc R . . C17 C 0.3163(3) 0.7220(3) -0.1146(3) 0.0191(8) Uani 1 1 d . . . H17 H 0.2748 0.7237 -0.0649 0.023 Uiso 1 1 calc R . . C18 C 0.3826(3) 0.8027(3) -0.1060(3) 0.0247(9) Uani 1 1 d . . . H18A H 0.4234 0.7919 -0.0544 0.030 Uiso 1 1 calc R . . H18B H 0.4192 0.8042 -0.1585 0.030 Uiso 1 1 calc R . . C19 C 0.3368(3) 0.8961(3) -0.0962(3) 0.0303(10) Uani 1 1 d . . . H19A H 0.2986 0.9087 -0.1484 0.045 Uiso 1 1 calc R . . H19B H 0.3822 0.9449 -0.0892 0.045 Uiso 1 1 calc R . . H19C H 0.3001 0.8949 -0.0445 0.045 Uiso 1 1 calc R . . C20 C 0.2619(3) 0.7210(3) -0.2018(3) 0.0232(9) Uani 1 1 d . . . H20A H 0.3026 0.7244 -0.2511 0.028 Uiso 1 1 calc R . . H20B H 0.2213 0.7753 -0.2052 0.028 Uiso 1 1 calc R . . C21 C 0.0952(3) 0.6411(3) -0.1515(3) 0.0230(9) Uani 1 1 d . . . C22 C 0.0776(3) 0.5967(3) -0.0730(3) 0.0298(10) Uani 1 1 d . . . H22 H 0.1169 0.5497 -0.0507 0.036 Uiso 1 1 calc R . . C23 C 0.0023(3) 0.6215(3) -0.0274(3) 0.0398(12) Uani 1 1 d . . . H23 H -0.0096 0.5915 0.0263 0.048 Uiso 1 1 calc R . . C24 C -0.0550(3) 0.6894(3) -0.0600(3) 0.0386(12) Uani 1 1 d . . . H24 H -0.1061 0.7060 -0.0286 0.046 Uiso 1 1 calc R . . C25 C -0.0384(3) 0.7331(3) -0.1377(3) 0.0393(12) Uani 1 1 d . . . H25 H -0.0782 0.7795 -0.1602 0.047 Uiso 1 1 calc R . . C26 C 0.0362(3) 0.7096(3) -0.1829(3) 0.0325(11) Uani 1 1 d . . . H26 H 0.0476 0.7404 -0.2363 0.039 Uiso 1 1 calc R . . C27 C 0.1622(3) 0.6008(3) -0.3237(3) 0.0229(9) Uani 1 1 d . . . C28 C 0.1423(3) 0.5135(3) -0.3574(3) 0.0245(9) Uani 1 1 d . . . H28 H 0.1487 0.4603 -0.3209 0.029 Uiso 1 1 calc R . . C29 C 0.1132(3) 0.5035(3) -0.4439(3) 0.0302(10) Uani 1 1 d . . . H29 H 0.0986 0.4437 -0.4665 0.036 Uiso 1 1 calc R . . C30 C 0.1054(3) 0.5810(3) -0.4979(3) 0.0331(11) Uani 1 1 d . . . H30 H 0.0858 0.5741 -0.5574 0.040 Uiso 1 1 calc R . . C31 C 0.1258(3) 0.6677(3) -0.4652(3) 0.0314(10) Uani 1 1 d . . . H31 H 0.1200 0.7206 -0.5022 0.038 Uiso 1 1 calc R . . C32 C 0.1547(3) 0.6783(3) -0.3788(3) 0.0278(10) Uani 1 1 d . . . H32 H 0.1695 0.7383 -0.3567 0.033 Uiso 1 1 calc R . . P1 P 0.35863(7) 0.45301(7) 0.14629(7) 0.0203(2) Uani 1 1 d . . . P2 P 0.19639(7) 0.61313(7) -0.20886(7) 0.0209(2) Uani 1 1 d . . . S1 S 0.38275(7) 0.41394(7) -0.05181(6) 0.0210(2) Uani 1 1 d . . . S2 S 0.38025(6) 0.61232(7) -0.11119(6) 0.0205(2) Uani 1 1 d . . . Cl1 Cl 0.35557(8) 0.68511(7) 0.10399(7) 0.0291(2) Uani 1 1 d . . . Cl2 Cl 0.17224(7) 0.37857(7) -0.16150(7) 0.0333(3) Uani 1 1 d . . . Pd1 Pd 0.37515(2) 0.54556(2) 0.029679(19) 0.01931(10) Uani 1 1 d . . . Pd2 Pd 0.27748(2) 0.49935(2) -0.14216(2) 0.01993(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(2) 0.016(2) 0.030(2) 0.0021(18) 0.0043(19) -0.0015(18) C2 0.040(3) 0.018(2) 0.031(2) -0.0043(19) -0.001(2) 0.003(2) C3 0.050(3) 0.018(2) 0.048(3) -0.001(2) -0.004(2) 0.001(2) C4 0.027(2) 0.0140(19) 0.027(2) 0.0030(18) 0.0039(18) 0.0019(17) C5 0.024(2) 0.018(2) 0.019(2) -0.0012(17) 0.0056(17) 0.0075(18) C6 0.029(2) 0.023(2) 0.028(2) 0.0019(19) 0.0045(19) 0.0050(19) C7 0.035(3) 0.029(2) 0.030(2) 0.006(2) 0.001(2) 0.009(2) C8 0.031(3) 0.041(3) 0.027(2) -0.001(2) -0.003(2) 0.005(2) C9 0.029(2) 0.027(2) 0.031(2) -0.004(2) -0.001(2) 0.000(2) C10 0.023(2) 0.024(2) 0.022(2) -0.0002(18) 0.0018(18) 0.0032(19) C11 0.024(2) 0.028(2) 0.027(2) -0.010(2) 0.0006(19) -0.003(2) C12 0.032(3) 0.065(3) 0.021(2) 0.002(2) 0.001(2) -0.002(3) C13 0.035(3) 0.092(5) 0.033(3) -0.002(3) 0.008(2) -0.020(3) C14 0.022(3) 0.083(4) 0.049(3) -0.035(3) 0.015(2) -0.010(3) C15 0.023(3) 0.040(3) 0.076(4) -0.027(3) 0.001(3) 0.000(2) C16 0.029(3) 0.028(2) 0.048(3) -0.012(2) 0.006(2) -0.002(2) C17 0.019(2) 0.0152(19) 0.023(2) 0.0003(17) -0.0027(17) 0.0032(17) C18 0.027(2) 0.020(2) 0.026(2) -0.0014(18) 0.0006(19) -0.0020(18) C19 0.036(3) 0.022(2) 0.034(2) 0.000(2) 0.002(2) -0.010(2) C20 0.025(2) 0.017(2) 0.027(2) 0.0011(18) 0.0043(19) -0.0035(18) C21 0.024(2) 0.022(2) 0.023(2) -0.0034(18) -0.0020(18) -0.0027(18) C22 0.035(3) 0.021(2) 0.034(2) 0.001(2) 0.008(2) -0.001(2) C23 0.044(3) 0.030(3) 0.047(3) -0.001(2) 0.019(2) -0.013(2) C24 0.027(2) 0.031(3) 0.059(3) -0.015(3) 0.014(2) -0.005(2) C25 0.030(3) 0.037(3) 0.051(3) -0.010(3) -0.003(2) 0.009(2) C26 0.035(3) 0.029(2) 0.033(3) -0.003(2) -0.001(2) 0.006(2) C27 0.018(2) 0.028(2) 0.024(2) 0.0001(19) 0.0011(17) -0.0006(18) C28 0.022(2) 0.022(2) 0.030(2) -0.0012(19) 0.0001(19) 0.0026(18) C29 0.028(2) 0.027(2) 0.036(3) -0.006(2) 0.001(2) 0.002(2) C30 0.027(2) 0.049(3) 0.022(2) -0.004(2) -0.0022(19) 0.005(2) C31 0.032(2) 0.033(2) 0.029(2) 0.007(2) -0.003(2) 0.003(2) C32 0.032(2) 0.025(2) 0.026(2) 0.0017(19) -0.0004(19) -0.004(2) P1 0.0229(6) 0.0174(5) 0.0208(5) -0.0007(4) 0.0025(4) 0.0009(4) P2 0.0227(5) 0.0177(5) 0.0221(5) 0.0013(4) -0.0010(4) -0.0017(5) S1 0.0235(5) 0.0167(5) 0.0229(5) -0.0008(4) 0.0033(4) 0.0014(4) S2 0.0207(5) 0.0178(5) 0.0230(5) 0.0006(4) 0.0019(4) -0.0015(4) Cl1 0.0445(6) 0.0166(5) 0.0259(5) -0.0038(4) 0.0001(5) 0.0033(5) Cl2 0.0386(6) 0.0237(5) 0.0370(6) 0.0030(5) -0.0079(5) -0.0109(5) Pd1 0.02313(18) 0.01443(16) 0.02034(17) -0.00060(13) 0.00033(13) 0.00042(13) Pd2 0.02287(18) 0.01541(16) 0.02146(17) -0.00011(13) 0.00011(13) -0.00180(13) _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 C1 C4 1.516(6) . ? C1 C2 1.531(5) . ? C1 S1 1.851(4) . ? C1 H1 1.0000 . ? C2 C3 1.513(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 P1 1.843(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.388(6) . ? C5 C6 1.404(5) . ? C5 P1 1.813(4) . ? C6 C7 1.385(6) . ? C6 H6 0.9500 . ? C7 C8 1.395(6) . ? C7 H7 0.9500 . ? C8 C9 1.373(6) . ? C8 H8 0.9500 . ? C9 C10 1.391(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.381(6) . ? C11 C12 1.393(6) . ? C11 P1 1.822(4) . ? C12 C13 1.390(6) . ? C12 H12 0.9500 . ? C13 C14 1.374(8) . ? C13 H13 0.9500 . ? C14 C15 1.359(8) . ? C14 H14 0.9500 . ? C15 C16 1.393(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.529(5) . ? C17 C20 1.532(5) . ? C17 S2 1.846(4) . ? C17 H17 1.0000 . ? C18 C19 1.520(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 P2 1.837(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.394(6) . ? C21 C26 1.395(6) . ? C21 P2 1.824(4) . ? C22 C23 1.396(6) . ? C22 H22 0.9500 . ? C23 C24 1.379(7) . ? C23 H23 0.9500 . ? C24 C25 1.377(7) . ? C24 H24 0.9500 . ? C25 C26 1.377(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.387(6) . ? C27 C32 1.400(6) . ? C27 P2 1.816(4) . ? C28 C29 1.382(6) . ? C28 H28 0.9500 . ? C29 C30 1.390(6) . ? C29 H29 0.9500 . ? C30 C31 1.374(6) . ? C30 H30 0.9500 . ? C31 C32 1.381(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? P1 Pd1 2.2469(11) . ? P2 Pd2 2.2570(12) . ? S1 Pd1 2.2732(10) . ? S1 Pd2 2.3918(12) . ? S2 Pd2 2.2746(11) . ? S2 Pd1 2.3616(11) . ? Cl1 Pd1 2.3326(11) . ? Cl2 Pd2 2.3562(11) . ? Pd1 Pd2 3.0266(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 C2 114.4(3) . . ? C4 C1 S1 106.9(3) . . ? C2 C1 S1 107.3(3) . . ? C4 C1 H1 109.4 . . ? C2 C1 H1 109.4 . . ? S1 C1 H1 109.4 . . ? C3 C2 C1 112.5(3) . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 P1 110.0(3) . . ? C1 C4 H4A 109.7 . . ? P1 C4 H4A 109.7 . . ? C1 C4 H4B 109.7 . . ? P1 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C10 C5 C6 119.1(4) . . ? C10 C5 P1 119.0(3) . . ? C6 C5 P1 121.8(3) . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.3(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.5(4) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C5 C10 C9 120.4(4) . . ? C5 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C16 C11 C12 118.9(4) . . ? C16 C11 P1 120.8(3) . . ? C12 C11 P1 120.3(3) . . ? C13 C12 C11 120.0(5) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.1(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.5(5) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C20 113.7(3) . . ? C18 C17 S2 108.3(3) . . ? C20 C17 S2 105.8(3) . . ? C18 C17 H17 109.7 . . ? C20 C17 H17 109.7 . . ? S2 C17 H17 109.7 . . ? C19 C18 C17 112.8(3) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 P2 108.8(3) . . ? C17 C20 H20A 109.9 . . ? P2 C20 H20A 109.9 . . ? C17 C20 H20B 109.9 . . ? P2 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C22 C21 C26 118.8(4) . . ? C22 C21 P2 120.1(3) . . ? C26 C21 P2 121.1(3) . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.2(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 119.9(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 121.0(4) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C28 C27 C32 119.2(4) . . ? C28 C27 P2 119.7(3) . . ? C32 C27 P2 121.1(3) . . ? C29 C28 C27 120.3(4) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.0(4) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.1(4) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 120.1(4) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C5 P1 C11 107.54(18) . . ? C5 P1 C4 106.04(18) . . ? C11 P1 C4 104.77(19) . . ? C5 P1 Pd1 116.59(13) . . ? C11 P1 Pd1 114.16(15) . . ? C4 P1 Pd1 106.79(13) . . ? C27 P2 C21 106.20(18) . . ? C27 P2 C20 105.54(19) . . ? C21 P2 C20 103.64(18) . . ? C27 P2 Pd2 119.38(14) . . ? C21 P2 Pd2 112.61(14) . . ? C20 P2 Pd2 108.16(14) . . ? C1 S1 Pd1 103.63(13) . . ? C1 S1 Pd2 110.40(14) . . ? Pd1 S1 Pd2 80.86(4) . . ? C17 S2 Pd2 105.13(13) . . ? C17 S2 Pd1 109.76(13) . . ? Pd2 S2 Pd1 81.48(4) . . ? P1 Pd1 S1 87.10(4) . . ? P1 Pd1 Cl1 96.02(4) . . ? S1 Pd1 Cl1 174.32(4) . . ? P1 Pd1 S2 166.67(4) . . ? S1 Pd1 S2 80.56(4) . . ? Cl1 Pd1 S2 95.87(4) . . ? P1 Pd1 Pd2 119.53(3) . . ? S1 Pd1 Pd2 51.28(3) . . ? Cl1 Pd1 Pd2 123.10(3) . . ? S2 Pd1 Pd2 48.01(3) . . ? P2 Pd2 S2 85.46(4) . . ? P2 Pd2 Cl2 97.78(4) . . ? S2 Pd2 Cl2 175.08(4) . . ? P2 Pd2 S1 164.36(4) . . ? S2 Pd2 S1 79.88(4) . . ? Cl2 Pd2 S1 96.51(4) . . ? P2 Pd2 Pd1 117.63(3) . . ? S2 Pd2 Pd1 50.51(3) . . ? Cl2 Pd2 Pd1 124.58(3) . . ? S1 Pd2 Pd1 47.86(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.266 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.153 data_4 _database_code_CSD 194253 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 P2 Pd S2' _chemical_formula_weight 653.07 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' 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.0549(18) _cell_length_b 10.873(2) _cell_length_c 15.972(3) _cell_angle_alpha 109.06(3) _cell_angle_beta 90.56(3) _cell_angle_gamma 101.02(3) _cell_volume 1454.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15195 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.8530 _exptl_absorpt_correction_T_max 0.9820 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 21282 _diffrn_reflns_av_R_equivalents 0.1253 _diffrn_reflns_av_sigmaI/netI 0.1331 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12285 _reflns_number_gt 9765 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0923P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(4) _refine_ls_number_reflns 12285 _refine_ls_number_parameters 672 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1779 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0555(10) 0.7382(9) 0.1003(5) 0.0191(18) Uani 1 1 d . . . C2 C -0.0067(10) 0.6133(10) 0.1059(6) 0.025(2) Uani 1 1 d . . . H2 H 0.0553 0.5506 0.1022 0.030 Uiso 1 1 calc R . . C3 C -0.1600(12) 0.5814(12) 0.1170(7) 0.038(3) Uani 1 1 d . . . H3 H -0.2035 0.4962 0.1198 0.045 Uiso 1 1 calc R . . C4 C -0.2473(11) 0.6723(14) 0.1239(6) 0.045(3) Uani 1 1 d . . . H4 H -0.3509 0.6505 0.1336 0.054 Uiso 1 1 calc R . . C5 C -0.1886(11) 0.7987(11) 0.1170(6) 0.036(2) Uani 1 1 d . . . H5 H -0.2512 0.8605 0.1198 0.043 Uiso 1 1 calc R . . C6 C -0.0354(10) 0.8281(10) 0.1060(5) 0.028(2) Uani 1 1 d . . . H6 H 0.0078 0.9127 0.1022 0.034 Uiso 1 1 calc R . . C7 C 0.2766(10) 0.6281(8) -0.0059(5) 0.0173(16) Uani 1 1 d . . . C8 C 0.1972(9) 0.5997(8) -0.0885(5) 0.0235(17) Uani 1 1 d . . . H8 H 0.1339 0.6569 -0.0950 0.028 Uiso 1 1 calc R . . C9 C 0.2096(11) 0.4916(9) -0.1595(5) 0.032(2) Uani 1 1 d . . . H9 H 0.1559 0.4754 -0.2147 0.039 Uiso 1 1 calc R . . C10 C 0.3001(13) 0.4043(10) -0.1523(7) 0.035(3) Uani 1 1 d . . . H10 H 0.3072 0.3282 -0.2015 0.042 Uiso 1 1 calc R . . C11 C 0.3796(12) 0.4317(10) -0.0710(6) 0.030(2) Uani 1 1 d . . . H11 H 0.4433 0.3743 -0.0653 0.036 Uiso 1 1 calc R . . C12 C 0.3678(12) 0.5414(12) 0.0021(8) 0.023(2) Uani 1 1 d . . . H12 H 0.4215 0.5574 0.0573 0.028 Uiso 1 1 calc R . . C13 C 0.2907(10) 0.9062(8) 0.0386(5) 0.0260(18) Uani 1 1 d . . . H13A H 0.3642 0.8866 -0.0069 0.031 Uiso 1 1 calc R . . H13B H 0.1954 0.9082 0.0086 0.031 Uiso 1 1 calc R . . C14 C 0.3507(10) 1.0411(8) 0.1068(5) 0.0249(17) Uani 1 1 d . . . H14 H 0.2676 1.0703 0.1442 0.030 Uiso 1 1 calc R . . C15 C 0.4074(12) 1.1427(9) 0.0601(6) 0.029(2) Uani 1 1 d . . . H15A H 0.4931 1.1161 0.0255 0.035 Uiso 1 1 calc R . . H15B H 0.3256 1.1404 0.0176 0.035 Uiso 1 1 calc R . . C16 C 0.4582(13) 1.2852(9) 0.1239(6) 0.047(3) Uani 1 1 d . . . H16A H 0.3756 1.3111 0.1603 0.071 Uiso 1 1 calc R . . H16B H 0.4860 1.3453 0.0898 0.071 Uiso 1 1 calc R . . H16C H 0.5457 1.2904 0.1624 0.071 Uiso 1 1 calc R . . C17 C 0.4281(9) 0.6646(8) 0.3501(5) 0.0204(16) Uani 1 1 d . . . H17 H 0.3746 0.7147 0.4005 0.024 Uiso 1 1 calc R . . C18 C 0.4295(10) 0.5274(8) 0.3566(5) 0.0220(18) Uani 1 1 d . . . H18A H 0.4791 0.4773 0.3053 0.026 Uiso 1 1 calc R . . H18B H 0.4915 0.5394 0.4111 0.026 Uiso 1 1 calc R . . C19 C 0.2760(10) 0.4446(8) 0.3585(6) 0.0308(19) Uani 1 1 d . . . H19A H 0.2338 0.4841 0.4150 0.046 Uiso 1 1 calc R . . H19B H 0.2858 0.3540 0.3525 0.046 Uiso 1 1 calc R . . H19C H 0.2087 0.4421 0.3092 0.046 Uiso 1 1 calc R . . C20 C 0.5900(9) 0.7419(7) 0.3558(5) 0.0203(16) Uani 1 1 d . . . H20A H 0.6487 0.6863 0.3128 0.024 Uiso 1 1 calc R . . H20B H 0.6385 0.7639 0.4162 0.024 Uiso 1 1 calc R . . C21 C 0.5421(9) 1.0124(8) 0.4314(5) 0.0158(16) Uani 1 1 d . . . C22 C 0.4703(14) 1.1117(11) 0.4245(8) 0.024(2) Uani 1 1 d . . . H22 H 0.4379 1.1095 0.3672 0.029 Uiso 1 1 calc R . . C23 C 0.4445(12) 1.2128(9) 0.4978(6) 0.031(2) Uani 1 1 d . . . H23 H 0.3939 1.2785 0.4915 0.037 Uiso 1 1 calc R . . C24 C 0.4948(12) 1.2165(9) 0.5822(7) 0.031(2) Uani 1 1 d . . . H24 H 0.4814 1.2870 0.6336 0.037 Uiso 1 1 calc R . . C25 C 0.5632(10) 1.1185(8) 0.5905(5) 0.0278(18) Uani 1 1 d . . . H25 H 0.5932 1.1195 0.6479 0.033 Uiso 1 1 calc R . . C26 C 0.5890(9) 1.0186(8) 0.5164(5) 0.0213(16) Uani 1 1 d . . . H26 H 0.6394 0.9531 0.5232 0.026 Uiso 1 1 calc R . . C27 C 0.7888(10) 0.9657(8) 0.3278(5) 0.0149(18) Uani 1 1 d . . . C28 C 0.9030(10) 0.8985(9) 0.3298(5) 0.024(2) Uani 1 1 d . . . H28 H 0.8784 0.8129 0.3356 0.029 Uiso 1 1 calc R . . C29 C 1.0517(10) 0.9521(9) 0.3237(6) 0.0230(19) Uani 1 1 d . . . H29 H 1.1285 0.9037 0.3243 0.028 Uiso 1 1 calc R . . C30 C 1.0878(10) 1.0805(10) 0.3165(6) 0.0244(19) Uani 1 1 d . . . H30 H 1.1897 1.1196 0.3129 0.029 Uiso 1 1 calc R . . C31 C 0.9756(10) 1.1484(9) 0.3148(6) 0.028(2) Uani 1 1 d . . . H31 H 1.0005 1.2343 0.3093 0.034 Uiso 1 1 calc R . . C32 C 0.8250(11) 1.0935(9) 0.3209(6) 0.025(2) Uani 1 1 d . . . H32 H 0.7482 1.1419 0.3205 0.031 Uiso 1 1 calc R . . C33 C 0.9582(10) 0.6561(8) 0.4962(5) 0.0202(17) Uani 1 1 d . . . C34 C 1.0019(9) 0.6522(8) 0.4126(5) 0.0213(17) Uani 1 1 d . . . H34 H 1.0823 0.7188 0.4072 0.026 Uiso 1 1 calc R . . C35 C 0.9300(11) 0.5524(9) 0.3367(5) 0.032(2) Uani 1 1 d . . . H35 H 0.9595 0.5524 0.2798 0.038 Uiso 1 1 calc R . . C36 C 0.8165(12) 0.4542(10) 0.3439(7) 0.035(3) Uani 1 1 d . . . H36 H 0.7682 0.3852 0.2921 0.042 Uiso 1 1 calc R . . C37 C 0.7721(12) 0.4557(10) 0.4275(6) 0.034(2) Uani 1 1 d . . . H37 H 0.6941 0.3869 0.4324 0.041 Uiso 1 1 calc R . . C38 C 0.8418(13) 0.5578(12) 0.5043(8) 0.029(3) Uani 1 1 d . . . H38 H 0.8099 0.5599 0.5612 0.035 Uiso 1 1 calc R . . C39 C 1.2247(10) 0.7044(9) 0.6036(5) 0.0185(19) Uani 1 1 d . . . C40 C 1.2026(10) 0.5835(8) 0.6165(6) 0.0231(19) Uani 1 1 d . . . H40 H 1.1034 0.5398 0.6215 0.028 Uiso 1 1 calc R . . C41 C 1.3251(11) 0.5240(10) 0.6223(6) 0.031(2) Uani 1 1 d . . . H41 H 1.3086 0.4394 0.6298 0.037 Uiso 1 1 calc R . . C42 C 1.4703(11) 0.5890(9) 0.6169(5) 0.025(2) Uani 1 1 d . . . H42 H 1.5539 0.5496 0.6209 0.031 Uiso 1 1 calc R . . C43 C 1.4924(11) 0.7143(10) 0.6054(6) 0.024(2) Uani 1 1 d . . . H43 H 1.5913 0.7609 0.6027 0.029 Uiso 1 1 calc R . . C44 C 1.3680(11) 0.7692(9) 0.5980(6) 0.028(2) Uani 1 1 d . . . H44 H 1.3825 0.8527 0.5890 0.033 Uiso 1 1 calc R . . C45 C 1.1297(9) 0.9293(7) 0.5750(5) 0.0227(17) Uani 1 1 d . . . H45A H 1.2148 0.9841 0.6188 0.027 Uiso 1 1 calc R . . H45B H 1.1677 0.9079 0.5151 0.027 Uiso 1 1 calc R . . C46 C 1.0068(9) 1.0076(7) 0.5798(5) 0.0199(16) Uani 1 1 d . . . H46 H 0.9304 0.9577 0.5284 0.024 Uiso 1 1 calc R . . C47 C 1.0704(11) 1.1450(8) 0.5733(6) 0.028(2) Uani 1 1 d . . . H47A H 1.1436 1.1957 0.6252 0.033 Uiso 1 1 calc R . . H47B H 1.1266 1.1332 0.5193 0.033 Uiso 1 1 calc R . . C48 C 0.9551(11) 1.2264(9) 0.5699(6) 0.035(2) Uani 1 1 d . . . H48A H 0.8791 1.1758 0.5205 0.053 Uiso 1 1 calc R . . H48B H 1.0049 1.3092 0.5612 0.053 Uiso 1 1 calc R . . H48C H 0.9061 1.2473 0.6259 0.053 Uiso 1 1 calc R . . C49 C 0.7565(9) 0.6300(8) 0.8244(5) 0.0209(16) Uani 1 1 d . . . H49 H 0.6578 0.6010 0.7879 0.025 Uiso 1 1 calc R . . C50 C 0.7683(11) 0.5308(8) 0.8694(5) 0.0233(19) Uani 1 1 d . . . H50A H 0.6896 0.5346 0.9122 0.028 Uiso 1 1 calc R . . H50B H 0.8674 0.5590 0.9041 0.028 Uiso 1 1 calc R . . C51 C 0.7530(13) 0.3874(9) 0.8105(7) 0.048(3) Uani 1 1 d . . . H51A H 0.6518 0.3547 0.7796 0.072 Uiso 1 1 calc R . . H51B H 0.7684 0.3332 0.8470 0.072 Uiso 1 1 calc R . . H51C H 0.8287 0.3815 0.7667 0.072 Uiso 1 1 calc R . . C52 C 0.7629(10) 0.7672(8) 0.8913(5) 0.0231(17) Uani 1 1 d . . . H52A H 0.8494 0.7886 0.9356 0.028 Uiso 1 1 calc R . . H52B H 0.6696 0.7664 0.9231 0.028 Uiso 1 1 calc R . . C53 C 0.8680(10) 1.0443(8) 0.9337(5) 0.0208(17) Uani 1 1 d . . . C54 C 0.9904(16) 1.1371(12) 0.9259(9) 0.036(3) Uani 1 1 d . . . H54 H 1.0330 1.1253 0.8704 0.043 Uiso 1 1 calc R . . C55 C 1.0511(13) 1.2477(10) 0.9996(7) 0.040(3) Uani 1 1 d . . . H55 H 1.1303 1.3141 0.9928 0.047 Uiso 1 1 calc R . . C56 C 0.9992(12) 1.2620(10) 1.0800(7) 0.032(2) Uani 1 1 d . . . H56 H 1.0463 1.3350 1.1302 0.039 Uiso 1 1 calc R . . C57 C 0.8768(11) 1.1703(8) 1.0900(5) 0.032(2) Uani 1 1 d . . . H57 H 0.8390 1.1808 1.1467 0.038 Uiso 1 1 calc R . . C58 C 0.8109(11) 1.0639(8) 1.0169(5) 0.029(2) Uani 1 1 d . . . H58 H 0.7252 1.0029 1.0232 0.035 Uiso 1 1 calc R . . C59 C 0.5949(10) 0.9259(8) 0.8247(5) 0.0182(18) Uani 1 1 d . . . C60 C 0.4606(9) 0.8353(8) 0.8256(5) 0.0206(17) Uani 1 1 d . . . H60 H 0.4663 0.7535 0.8336 0.025 Uiso 1 1 calc R . . C61 C 0.3223(9) 0.8644(9) 0.8148(5) 0.0256(18) Uani 1 1 d . . . H61 H 0.2325 0.8019 0.8136 0.031 Uiso 1 1 calc R . . C62 C 0.3143(11) 0.9854(10) 0.8058(6) 0.029(2) Uani 1 1 d . . . H62 H 0.2185 1.0069 0.8006 0.034 Uiso 1 1 calc R . . C63 C 0.4421(12) 1.0740(9) 0.8042(6) 0.032(2) Uani 1 1 d . . . H63 H 0.4344 1.1556 0.7965 0.038 Uiso 1 1 calc R . . C64 C 0.5839(10) 1.0461(9) 0.8137(6) 0.0229(19) Uani 1 1 d . . . H64 H 0.6726 1.1083 0.8126 0.028 Uiso 1 1 calc R . . P1 P 0.2557(3) 0.7739(2) 0.08671(14) 0.0175(5) Uani 1 1 d . . . P2 P 0.5901(3) 0.8938(2) 0.33165(14) 0.0161(4) Uani 1 1 d . . . P3 P 1.0592(3) 0.7765(2) 0.59784(14) 0.0175(5) Uani 1 1 d . . . P4 P 0.7821(3) 0.8967(2) 0.84048(14) 0.0168(5) Uani 1 1 d . . . S1 S 0.5056(3) 1.0314(2) 0.17860(15) 0.0227(5) Uani 1 1 d . . . S2 S 0.3279(3) 0.6458(2) 0.24407(15) 0.0243(5) Uani 1 1 d . . . S3 S 0.9122(3) 1.0243(2) 0.68288(15) 0.0263(5) Uani 1 1 d . . . S4 S 0.9107(3) 0.6391(2) 0.74972(15) 0.0235(5) Uani 1 1 d . . . Pd1 Pd 0.41977(7) 0.83753(6) 0.21102(4) 0.01575(15) Uani 1 1 d . . . Pd2 Pd 0.91515(8) 0.83286(6) 0.71688(4) 0.01608(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(4) 0.025(5) 0.013(4) 0.003(3) -0.001(3) 0.004(4) C2 0.017(4) 0.032(5) 0.026(4) 0.008(4) 0.003(3) 0.005(4) C3 0.026(6) 0.050(7) 0.029(5) 0.016(5) -0.002(4) -0.015(5) C4 0.013(5) 0.087(10) 0.025(5) 0.008(6) -0.003(4) 0.006(6) C5 0.035(6) 0.051(7) 0.024(5) 0.005(5) 0.001(4) 0.024(5) C6 0.026(5) 0.039(6) 0.017(4) 0.002(4) -0.006(3) 0.012(4) C7 0.018(4) 0.014(4) 0.016(3) -0.001(3) 0.002(3) 0.004(3) C8 0.027(4) 0.026(4) 0.023(4) 0.012(4) 0.003(3) 0.012(4) C9 0.044(6) 0.032(5) 0.018(4) 0.003(4) 0.000(4) 0.012(4) C10 0.047(6) 0.027(6) 0.020(4) -0.009(4) -0.006(4) 0.012(5) C11 0.029(5) 0.032(5) 0.025(4) 0.001(4) -0.002(4) 0.013(4) C12 0.016(5) 0.027(5) 0.021(5) -0.001(4) -0.004(4) 0.006(4) C13 0.037(5) 0.023(4) 0.016(4) 0.003(3) -0.002(3) 0.007(4) C14 0.034(5) 0.020(4) 0.022(4) 0.004(3) -0.004(3) 0.014(4) C15 0.047(6) 0.021(5) 0.016(4) 0.003(4) -0.010(4) 0.006(4) C16 0.073(7) 0.021(5) 0.041(5) 0.005(4) -0.032(5) 0.005(5) C17 0.023(4) 0.019(4) 0.023(4) 0.011(3) 0.005(3) 0.006(3) C18 0.025(5) 0.017(4) 0.022(4) 0.005(3) -0.003(4) 0.004(4) C19 0.034(5) 0.019(4) 0.040(5) 0.017(4) -0.002(4) -0.004(4) C20 0.021(4) 0.018(4) 0.019(4) 0.005(3) -0.006(3) 0.001(3) C21 0.011(4) 0.018(4) 0.016(3) 0.002(3) 0.001(3) 0.000(3) C22 0.029(6) 0.024(5) 0.022(5) 0.010(4) 0.010(4) 0.008(4) C23 0.035(6) 0.027(5) 0.032(5) 0.009(4) 0.004(4) 0.015(4) C24 0.039(6) 0.023(5) 0.021(4) -0.008(4) 0.004(4) 0.010(4) C25 0.031(5) 0.023(4) 0.026(4) 0.007(4) 0.002(4) 0.003(4) C26 0.025(4) 0.022(4) 0.020(4) 0.009(3) 0.006(3) 0.007(3) C27 0.020(4) 0.009(4) 0.010(3) -0.001(3) 0.000(3) 0.000(3) C28 0.028(5) 0.025(5) 0.015(4) 0.005(4) 0.002(3) 0.000(4) C29 0.024(5) 0.023(5) 0.024(4) 0.009(4) -0.005(3) 0.007(4) C30 0.015(4) 0.035(5) 0.022(4) 0.012(4) -0.002(3) -0.002(4) C31 0.029(5) 0.014(4) 0.034(5) 0.009(4) -0.012(4) -0.012(4) C32 0.025(5) 0.019(5) 0.030(4) 0.005(4) -0.005(4) 0.006(4) C33 0.023(4) 0.021(4) 0.020(4) 0.007(3) 0.005(3) 0.011(3) C34 0.022(4) 0.020(4) 0.021(4) 0.004(3) -0.003(3) 0.006(3) C35 0.044(5) 0.033(5) 0.019(4) 0.006(4) -0.002(4) 0.014(4) C36 0.039(6) 0.029(6) 0.027(5) -0.003(5) -0.011(4) 0.011(5) C37 0.030(5) 0.026(5) 0.036(5) -0.001(4) -0.004(4) 0.002(4) C38 0.023(5) 0.029(6) 0.024(5) -0.001(4) 0.002(4) -0.003(4) C39 0.019(4) 0.016(4) 0.017(4) -0.003(3) -0.001(3) 0.007(4) C40 0.021(5) 0.015(4) 0.028(4) 0.001(4) 0.002(4) 0.003(4) C41 0.039(5) 0.026(5) 0.028(4) 0.006(4) 0.005(4) 0.011(4) C42 0.030(5) 0.036(5) 0.015(4) 0.004(4) 0.005(3) 0.024(4) C43 0.023(5) 0.030(5) 0.022(4) 0.007(4) 0.004(3) 0.010(4) C44 0.032(5) 0.026(5) 0.025(4) 0.011(4) 0.002(4) 0.003(4) C45 0.026(4) 0.016(4) 0.023(4) 0.001(3) 0.003(3) 0.008(3) C46 0.027(4) 0.015(4) 0.018(4) 0.007(3) 0.002(3) 0.000(3) C47 0.028(5) 0.019(5) 0.031(5) 0.008(4) 0.010(4) -0.003(4) C48 0.048(6) 0.019(4) 0.038(5) 0.012(4) 0.004(4) 0.000(4) C49 0.023(4) 0.018(4) 0.019(4) 0.005(3) -0.002(3) 0.000(3) C50 0.032(5) 0.013(4) 0.023(4) 0.004(3) 0.010(4) 0.004(4) C51 0.071(8) 0.017(5) 0.053(6) 0.010(5) 0.006(6) 0.004(5) C52 0.030(5) 0.023(4) 0.017(4) 0.007(3) 0.008(3) 0.008(4) C53 0.018(4) 0.021(4) 0.017(4) 0.001(3) -0.004(3) 0.000(3) C54 0.039(7) 0.025(6) 0.031(6) -0.001(5) 0.010(5) -0.008(5) C55 0.033(6) 0.023(5) 0.043(5) -0.005(4) 0.004(5) -0.013(4) C56 0.033(5) 0.024(5) 0.029(5) -0.005(4) -0.004(4) 0.002(4) C57 0.052(6) 0.022(5) 0.018(4) 0.004(3) 0.002(4) 0.003(4) C58 0.042(5) 0.016(4) 0.023(4) -0.002(3) 0.000(4) 0.003(4) C59 0.021(4) 0.017(4) 0.013(4) 0.000(3) 0.003(3) 0.004(3) C60 0.020(4) 0.025(4) 0.014(4) 0.005(3) 0.000(3) 0.001(4) C61 0.018(4) 0.035(5) 0.017(4) 0.005(4) 0.005(3) -0.002(4) C62 0.026(5) 0.036(6) 0.022(4) -0.001(4) 0.005(4) 0.019(4) C63 0.038(6) 0.026(5) 0.031(5) 0.000(4) 0.000(4) 0.021(5) C64 0.020(4) 0.022(5) 0.021(4) 0.002(3) 0.000(3) -0.001(4) P1 0.0178(12) 0.0165(11) 0.0160(9) 0.0033(8) -0.0015(8) 0.0025(9) P2 0.0171(11) 0.0150(10) 0.0146(9) 0.0032(8) -0.0014(8) 0.0027(9) P3 0.0199(12) 0.0141(10) 0.0169(9) 0.0031(8) 0.0009(8) 0.0033(9) P4 0.0188(12) 0.0130(10) 0.0172(9) 0.0032(8) 0.0020(8) 0.0036(9) S1 0.0277(13) 0.0188(11) 0.0214(10) 0.0096(9) -0.0040(10) -0.0009(10) S2 0.0263(13) 0.0195(11) 0.0245(11) 0.0096(9) -0.0096(10) -0.0051(10) S3 0.0403(15) 0.0232(12) 0.0248(11) 0.0134(10) 0.0126(11) 0.0188(12) S4 0.0322(14) 0.0179(11) 0.0234(11) 0.0087(9) 0.0082(10) 0.0084(10) Pd1 0.0167(3) 0.0143(2) 0.0146(3) 0.00337(19) -0.00157(18) 0.00218(18) Pd2 0.0184(3) 0.0138(2) 0.0154(3) 0.00350(19) 0.00153(19) 0.00444(18) _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 C1 C6 1.376(12) . ? C1 C2 1.399(12) . ? C1 P1 1.810(9) . ? C2 C3 1.393(14) . ? C3 C4 1.358(17) . ? C4 C5 1.415(17) . ? C5 C6 1.389(14) . ? C7 C12 1.401(13) . ? C7 C8 1.409(11) . ? C7 P1 1.824(8) . ? C8 C9 1.365(11) . ? C9 C10 1.397(13) . ? C10 C11 1.393(13) . ? C11 C12 1.393(14) . ? C13 C14 1.507(11) . ? C13 P1 1.820(8) . ? C14 C15 1.540(11) . ? C14 S1 1.843(8) . ? C15 C16 1.529(12) . ? C17 C20 1.530(11) . ? C17 C18 1.531(10) . ? C17 S2 1.846(8) . ? C18 C19 1.511(12) . ? C20 P2 1.815(7) . ? C21 C22 1.394(14) . ? C21 C26 1.395(10) . ? C21 P2 1.810(8) . ? C22 C23 1.377(15) . ? C23 C24 1.403(13) . ? C24 C25 1.371(12) . ? C25 C26 1.378(11) . ? C27 C28 1.382(13) . ? C27 C32 1.406(11) . ? C27 P2 1.830(9) . ? C28 C29 1.379(12) . ? C29 C30 1.414(12) . ? C30 C31 1.371(13) . ? C31 C32 1.398(13) . ? C33 C34 1.386(11) . ? C33 C38 1.390(15) . ? C33 P3 1.819(9) . ? C34 C35 1.388(11) . ? C35 C36 1.368(14) . ? C36 C37 1.394(15) . ? C37 C38 1.401(15) . ? C39 C40 1.373(12) . ? C39 C44 1.372(13) . ? C39 P3 1.835(9) . ? C40 C41 1.404(13) . ? C41 C42 1.386(14) . ? C42 C43 1.411(13) . ? C43 C44 1.392(12) . ? C45 C46 1.513(11) . ? C45 P3 1.815(8) . ? C46 C47 1.533(10) . ? C46 S3 1.836(8) . ? C47 C48 1.503(13) . ? C49 C50 1.496(10) . ? C49 C52 1.515(11) . ? C49 S4 1.854(8) . ? C50 C51 1.514(12) . ? C52 P4 1.824(7) . ? C53 C54 1.386(15) . ? C53 C58 1.396(11) . ? C53 P4 1.827(8) . ? C54 C55 1.395(16) . ? C55 C56 1.343(14) . ? C56 C57 1.391(13) . ? C57 C58 1.377(12) . ? C59 C64 1.396(12) . ? C59 C60 1.414(11) . ? C59 P4 1.813(9) . ? C60 C61 1.372(12) . ? C61 C62 1.385(13) . ? C62 C63 1.364(14) . ? C63 C64 1.393(13) . ? P1 Pd1 2.298(3) . ? P2 Pd1 2.297(2) . ? P3 Pd2 2.299(3) . ? P4 Pd2 2.303(2) . ? S1 Pd1 2.326(2) . ? S2 Pd1 2.319(2) . ? S3 Pd2 2.321(2) . ? S4 Pd2 2.325(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 C6 C1 C2 119.6(9) . . ? C6 C1 P1 123.0(7) . . ? C2 C1 P1 117.4(7) . . ? C3 C2 C1 119.6(9) . . ? C4 C3 C2 119.9(10) . . ? C3 C4 C5 122.0(9) . . ? C6 C5 C4 117.0(9) . . ? C1 C6 C5 121.9(10) . . ? C12 C7 C8 118.3(8) . . ? C12 C7 P1 122.4(7) . . ? C8 C7 P1 119.3(6) . . ? C9 C8 C7 121.2(7) . . ? C8 C9 C10 121.1(8) . . ? C11 C10 C9 118.2(9) . . ? C10 C11 C12 121.4(9) . . ? C11 C12 C7 119.8(9) . . ? C14 C13 P1 112.8(5) . . ? C13 C14 C15 109.9(6) . . ? C13 C14 S1 109.8(5) . . ? C15 C14 S1 110.0(6) . . ? C16 C15 C14 113.7(7) . . ? C20 C17 C18 109.9(6) . . ? C20 C17 S2 109.8(5) . . ? C18 C17 S2 109.8(5) . . ? C19 C18 C17 115.1(7) . . ? C17 C20 P2 110.1(5) . . ? C22 C21 C26 117.5(8) . . ? C22 C21 P2 119.5(7) . . ? C26 C21 P2 122.5(6) . . ? C23 C22 C21 122.4(10) . . ? C22 C23 C24 118.5(9) . . ? C25 C24 C23 120.1(9) . . ? C24 C25 C26 120.7(8) . . ? C25 C26 C21 120.9(7) . . ? C28 C27 C32 119.2(8) . . ? C28 C27 P2 122.6(6) . . ? C32 C27 P2 118.2(7) . . ? C29 C28 C27 121.9(8) . . ? C28 C29 C30 118.7(9) . . ? C31 C30 C29 120.0(8) . . ? C30 C31 C32 121.0(8) . . ? C31 C32 C27 119.1(8) . . ? C34 C33 C38 119.6(9) . . ? C34 C33 P3 122.5(7) . . ? C38 C33 P3 117.7(7) . . ? C33 C34 C35 121.0(8) . . ? C36 C35 C34 120.0(8) . . ? C35 C36 C37 119.9(9) . . ? C36 C37 C38 120.5(10) . . ? C33 C38 C37 119.1(11) . . ? C40 C39 C44 120.0(8) . . ? C40 C39 P3 118.1(7) . . ? C44 C39 P3 122.0(7) . . ? C39 C40 C41 120.6(9) . . ? C42 C41 C40 119.8(9) . . ? C41 C42 C43 119.3(8) . . ? C44 C43 C42 119.5(9) . . ? C39 C44 C43 120.9(9) . . ? C46 C45 P3 110.9(5) . . ? C45 C46 C47 111.1(7) . . ? C45 C46 S3 110.4(5) . . ? C47 C46 S3 110.3(5) . . ? C48 C47 C46 115.2(8) . . ? C50 C49 C52 111.5(6) . . ? C50 C49 S4 110.7(6) . . ? C52 C49 S4 109.0(5) . . ? C49 C50 C51 117.1(7) . . ? C49 C52 P4 113.1(5) . . ? C54 C53 C58 118.2(9) . . ? C54 C53 P4 122.6(8) . . ? C58 C53 P4 119.2(6) . . ? C53 C54 C55 119.9(11) . . ? C56 C55 C54 121.1(10) . . ? C55 C56 C57 120.2(9) . . ? C58 C57 C56 119.3(8) . . ? C57 C58 C53 121.2(9) . . ? C64 C59 C60 118.7(8) . . ? C64 C59 P4 117.8(7) . . ? C60 C59 P4 123.5(6) . . ? C61 C60 C59 120.7(8) . . ? C60 C61 C62 119.6(8) . . ? C63 C62 C61 120.8(8) . . ? C62 C63 C64 120.7(9) . . ? C59 C64 C63 119.5(9) . . ? C1 P1 C13 107.5(4) . . ? C1 P1 C7 102.0(4) . . ? C13 P1 C7 102.8(4) . . ? C1 P1 Pd1 117.9(3) . . ? C13 P1 Pd1 107.6(3) . . ? C7 P1 Pd1 117.7(3) . . ? C21 P2 C20 106.9(4) . . ? C21 P2 C27 101.5(4) . . ? C20 P2 C27 105.5(4) . . ? C21 P2 Pd1 114.4(3) . . ? C20 P2 Pd1 106.4(3) . . ? C27 P2 Pd1 121.2(3) . . ? C45 P3 C33 107.3(4) . . ? C45 P3 C39 105.7(4) . . ? C33 P3 C39 100.5(4) . . ? C45 P3 Pd2 105.9(3) . . ? C33 P3 Pd2 115.2(3) . . ? C39 P3 Pd2 121.3(3) . . ? C59 P4 C52 107.4(4) . . ? C59 P4 C53 102.3(4) . . ? C52 P4 C53 101.6(4) . . ? C59 P4 Pd2 117.8(3) . . ? C52 P4 Pd2 107.6(3) . . ? C53 P4 Pd2 118.6(3) . . ? C14 S1 Pd1 104.7(3) . . ? C17 S2 Pd1 106.8(3) . . ? C46 S3 Pd2 107.0(3) . . ? C49 S4 Pd2 105.8(3) . . ? P2 Pd1 P1 177.31(11) . . ? P2 Pd1 S2 85.86(9) . . ? P1 Pd1 S2 93.36(9) . . ? P2 Pd1 S1 94.85(9) . . ? P1 Pd1 S1 85.99(9) . . ? S2 Pd1 S1 178.45(14) . . ? P3 Pd2 P4 176.98(11) . . ? P3 Pd2 S3 85.80(9) . . ? P4 Pd2 S3 93.62(9) . . ? P3 Pd2 S4 94.82(9) . . ? P4 Pd2 S4 85.84(9) . . ? S3 Pd2 S4 178.35(14) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.779 _refine_diff_density_min -2.629 _refine_diff_density_rms 0.168 data_5 _database_code_CSD 194254 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 P2 Pt S2' _chemical_formula_weight 741.76 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.104(4) _cell_length_b 9.885(2) _cell_length_c 15.240(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.69(3) _cell_angle_gamma 90.00 _cell_volume 2942.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14770 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 5.039 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.3776 _exptl_absorpt_correction_T_max 0.8239 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 20261 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3367 _reflns_number_gt 3090 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0745P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00069(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3367 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.4132(2) 0.7887(4) 0.3059(3) 0.0145(8) Uani 1 1 d . . . C2 C 0.4287(2) 0.6541(5) 0.2925(3) 0.0194(9) Uani 1 1 d . . . H2 H 0.4339 0.6259 0.2349 0.023 Uiso 1 1 calc R . . C3 C 0.4366(3) 0.5604(4) 0.3622(4) 0.0216(11) Uani 1 1 d . . . H3 H 0.4472 0.4688 0.3524 0.026 Uiso 1 1 calc R . . C4 C 0.4289(3) 0.6023(5) 0.4469(3) 0.0232(10) Uani 1 1 d . . . H4 H 0.4347 0.5391 0.4951 0.028 Uiso 1 1 calc R . . C5 C 0.4129(2) 0.7351(5) 0.4608(3) 0.0202(9) Uani 1 1 d . . . H5 H 0.4073 0.7627 0.5183 0.024 Uiso 1 1 calc R . . C6 C 0.4050(2) 0.8283(4) 0.3912(3) 0.0173(9) Uani 1 1 d . . . H6 H 0.3940 0.9195 0.4013 0.021 Uiso 1 1 calc R . . C7 C 0.3924(2) 0.8351(4) 0.1134(3) 0.0148(8) Uani 1 1 d . . . C8 C 0.3414(2) 0.7363(4) 0.0911(3) 0.0203(9) Uani 1 1 d . . . H8 H 0.3171 0.7094 0.1346 0.024 Uiso 1 1 calc R . . C9 C 0.3260(2) 0.6774(4) 0.0066(3) 0.0234(10) Uani 1 1 d . . . H9 H 0.2917 0.6096 -0.0077 0.028 Uiso 1 1 calc R . . C10 C 0.3609(2) 0.7176(4) -0.0574(3) 0.0232(10) Uani 1 1 d . . . H10 H 0.3499 0.6782 -0.1159 0.028 Uiso 1 1 calc R . . C11 C 0.4114(2) 0.8141(5) -0.0368(3) 0.0222(10) Uani 1 1 d . . . H11 H 0.4355 0.8403 -0.0807 0.027 Uiso 1 1 calc R . . C12 C 0.4273(2) 0.8735(4) 0.0483(3) 0.0178(9) Uani 1 1 d . . . H12 H 0.4621 0.9405 0.0622 0.021 Uiso 1 1 calc R . . C13 C 0.3335(2) 1.0180(5) 0.2193(3) 0.0181(9) Uani 1 1 d . . . H13A H 0.2925 0.9649 0.1899 0.022 Uiso 1 1 calc R . . H13B H 0.3304 1.0402 0.2815 0.022 Uiso 1 1 calc R . . C14 C 0.3371(2) 1.1482(4) 0.1660(3) 0.0169(8) Uani 1 1 d . . . H14 H 0.3366 1.1234 0.1022 0.020 Uiso 1 1 calc R . . C15 C 0.2763(2) 1.2411(5) 0.1655(3) 0.0205(9) Uani 1 1 d . . . H15A H 0.2764 1.2657 0.2285 0.025 Uiso 1 1 calc R . . H15B H 0.2333 1.1913 0.1400 0.025 Uiso 1 1 calc R . . C16 C 0.2773(2) 1.3708(5) 0.1108(4) 0.0262(10) Uani 1 1 d . . . H16A H 0.3165 1.4266 0.1404 0.039 Uiso 1 1 calc R . . H16B H 0.2348 1.4215 0.1073 0.039 Uiso 1 1 calc R . . H16C H 0.2811 1.3474 0.0497 0.039 Uiso 1 1 calc R . . P1 P 0.41154(6) 0.91964(10) 0.22195(9) 0.0121(3) Uani 1 1 d . . . S1 S 0.41812(5) 1.23700(10) 0.21560(8) 0.0150(2) Uani 1 1 d . . . Pt1 Pt 0.5000 1.066365(19) 0.2500 0.01189(12) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0119(18) 0.017(2) 0.016(2) 0.0027(16) 0.0055(15) -0.0034(15) C2 0.020(2) 0.017(2) 0.023(2) -0.0009(17) 0.0069(17) 0.0000(17) C3 0.026(3) 0.013(2) 0.027(3) 0.0000(16) 0.006(2) 0.0017(16) C4 0.023(2) 0.020(2) 0.026(3) 0.004(2) 0.0051(19) -0.004(2) C5 0.018(2) 0.028(2) 0.015(2) 0.0005(18) 0.0052(17) -0.0021(18) C6 0.015(2) 0.014(2) 0.023(2) -0.0030(16) 0.0058(17) -0.0009(16) C7 0.0132(19) 0.0118(19) 0.018(2) -0.0021(16) 0.0012(16) 0.0027(15) C8 0.020(2) 0.019(2) 0.021(2) 0.0004(17) 0.0026(17) 0.0009(17) C9 0.026(2) 0.014(2) 0.026(3) -0.0021(17) -0.0022(18) 0.0020(17) C10 0.028(2) 0.017(2) 0.022(2) -0.0034(18) -0.0008(18) 0.0076(18) C11 0.026(2) 0.021(2) 0.021(2) 0.0023(18) 0.0072(18) 0.0058(19) C12 0.020(2) 0.015(2) 0.019(2) 0.0009(17) 0.0061(17) 0.0016(16) C13 0.016(2) 0.017(2) 0.022(2) 0.0025(19) 0.0058(17) 0.0015(17) C14 0.016(2) 0.016(2) 0.018(2) 0.0021(17) 0.0034(16) 0.0016(16) C15 0.015(2) 0.018(2) 0.029(2) 0.0014(18) 0.0075(18) 0.0034(16) C16 0.018(2) 0.019(3) 0.041(3) 0.006(2) 0.008(2) 0.0056(18) P1 0.0107(5) 0.0091(5) 0.0170(6) 0.0003(4) 0.0042(5) -0.0009(4) S1 0.0141(5) 0.0091(5) 0.0210(6) 0.0000(4) 0.0028(4) 0.0014(4) Pt1 0.01250(16) 0.00940(16) 0.01433(18) 0.000 0.00429(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.393(6) . ? C1 C6 1.404(6) . ? C1 P1 1.815(4) . ? C2 C3 1.390(7) . ? C3 C4 1.399(8) . ? C4 C5 1.379(7) . ? C5 C6 1.385(6) . ? C7 C12 1.397(6) . ? C7 C8 1.398(6) . ? C7 P1 1.811(4) . ? C8 C9 1.380(7) . ? C9 C10 1.388(7) . ? C10 C11 1.374(7) . ? C11 C12 1.389(6) . ? C13 C14 1.532(6) . ? C13 P1 1.838(4) . ? C14 C15 1.528(6) . ? C14 S1 1.848(4) . ? C15 C16 1.532(6) . ? P1 Pt1 2.2560(12) . ? S1 Pt1 2.3284(11) . ? Pt1 P1 2.2560(12) 2_655 ? Pt1 S1 2.3284(11) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.8(4) . . ? C2 C1 P1 123.0(3) . . ? C6 C1 P1 117.9(3) . . ? C3 C2 C1 120.9(4) . . ? C2 C3 C4 119.4(4) . . ? C5 C4 C3 120.2(4) . . ? C4 C5 C6 120.3(4) . . ? C5 C6 C1 120.4(4) . . ? C12 C7 C8 118.6(4) . . ? C12 C7 P1 119.3(3) . . ? C8 C7 P1 122.0(3) . . ? C9 C8 C7 120.8(4) . . ? C8 C9 C10 119.7(4) . . ? C11 C10 C9 120.4(4) . . ? C10 C11 C12 120.1(4) . . ? C11 C12 C7 120.3(4) . . ? C14 C13 P1 108.0(3) . . ? C15 C14 C13 111.7(4) . . ? C15 C14 S1 110.1(3) . . ? C13 C14 S1 109.2(3) . . ? C14 C15 C16 113.1(4) . . ? C7 P1 C1 106.22(19) . . ? C7 P1 C13 103.2(2) . . ? C1 P1 C13 105.4(2) . . ? C7 P1 Pt1 117.20(14) . . ? C1 P1 Pt1 116.30(14) . . ? C13 P1 Pt1 107.12(16) . . ? C14 S1 Pt1 104.82(14) . . ? P1 Pt1 P1 99.98(6) . 2_655 ? P1 Pt1 S1 172.77(4) . 2_655 ? P1 Pt1 S1 86.53(4) 2_655 2_655 ? P1 Pt1 S1 86.53(4) . . ? P1 Pt1 S1 172.77(4) 2_655 . ? S1 Pt1 S1 87.16(5) 2_655 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.752 _refine_diff_density_min -4.076 _refine_diff_density_rms 0.249 data_6 _database_code_CSD 194255 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H33 Cl P2 Pd S' _chemical_formula_weight 677.45 _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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.509(2) _cell_length_b 10.5654(13) _cell_length_c 17.553(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.021(14) _cell_angle_gamma 90.00 _cell_volume 1558.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method ? _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.8560 _exptl_absorpt_correction_T_max 0.9225 _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 'Enraf Nonius CAD4 diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3175 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.18 _reflns_number_total 2966 _reflns_number_observed 2398 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Wocadlo & Harms, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0794P] 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 calculated _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 2966 _refine_ls_number_parameters 293 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_obs 0.0311 _refine_ls_wR_factor_all 0.0731 _refine_ls_wR_factor_obs 0.0650 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.062 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.22157(5) 0.38838(5) 0.29885(2) 0.03624(13) Uani 1 d . . Cl1 Cl 0.2338(3) 0.6015(2) 0.33670(11) 0.0624(5) Uani 1 d . . S1 S 0.1956(3) 0.1817(2) 0.26216(11) 0.0559(5) Uani 1 d . . P1 P 0.1452(2) 0.3222(2) 0.41134(9) 0.0359(4) Uani 1 d . . P2 P 0.2946(2) 0.4332(2) 0.17835(9) 0.0376(4) Uani 1 d . . C1 C 0.1478(8) 0.1503(6) 0.4109(3) 0.044(2) Uani 1 d . . H1A H 0.2559(8) 0.1198(6) 0.4253(3) 0.052 Uiso 1 calc R . H1B H 0.0840(8) 0.1178(6) 0.4478(3) 0.052 Uiso 1 calc R . C2 C 0.0809(8) 0.1061(6) 0.3308(4) 0.046(2) Uani 1 d . . H2 H -0.0298(8) 0.1347(6) 0.3188(4) 0.055 Uiso 1 calc R . C3 C 0.0837(9) -0.0355(6) 0.3217(4) 0.058(2) Uani 1 d . . H3A H 0.1936(9) -0.0634(6) 0.3315(4) 0.070 Uiso 1 calc R . H3B H 0.0299(9) -0.0731(6) 0.3610(4) 0.070 Uiso 1 calc R . C4 C 0.0087(10) -0.0855(8) 0.2449(5) 0.086(3) Uani 1 d . . H4A H -0.1024(20) -0.0644(53) 0.2360(17) 0.129 Uiso 1 calc R . H4B H 0.0207(66) -0.1758(10) 0.2440(13) 0.129 Uiso 1 calc R . H4C H 0.0597(53) -0.0484(46) 0.2052(5) 0.129 Uiso 1 calc R . C5 C 0.2543(5) 0.3716(4) 0.5039(2) 0.0378(14) Uani 1 d G . C6 C 0.3377(6) 0.2849(3) 0.5544(3) 0.050(2) Uani 1 d G . H6 H 0.3369(8) 0.1995(4) 0.5414(4) 0.061 Uiso 1 calc R . C7 C 0.4224(5) 0.3258(5) 0.6242(2) 0.067(2) Uani 1 d G . H7 H 0.4782(8) 0.2677(6) 0.6580(3) 0.080 Uiso 1 calc R . C8 C 0.4236(5) 0.4534(5) 0.6436(2) 0.059(2) Uani 1 d G . H8 H 0.4803(7) 0.4807(7) 0.6903(2) 0.070 Uiso 1 calc R . C9 C 0.3402(6) 0.5401(4) 0.5930(3) 0.061(2) Uani 1 d G . H9 H 0.3410(9) 0.6255(4) 0.6060(4) 0.073 Uiso 1 calc R . C10 C 0.2555(5) 0.4992(4) 0.5232(2) 0.052(2) Uani 1 d G . H10 H 0.1997(8) 0.5572(5) 0.4894(3) 0.063 Uiso 1 calc R . C11 C -0.0601(3) 0.3646(4) 0.4178(2) 0.0371(15) Uani 1 d G . C12 C -0.1272(4) 0.3223(4) 0.4805(2) 0.045(2) Uani 1 d G . H12 H -0.0674(6) 0.2733(5) 0.5185(3) 0.054 Uiso 1 calc R . C13 C -0.2836(5) 0.3531(4) 0.4864(2) 0.056(2) Uani 1 d G . H13 H -0.3285(6) 0.3248(6) 0.5283(3) 0.067 Uiso 1 calc R . C14 C -0.3730(4) 0.4263(5) 0.4296(3) 0.060(2) Uani 1 d G . H14 H -0.4777(4) 0.4469(6) 0.4335(4) 0.072 Uiso 1 calc R . C15 C -0.3060(5) 0.4686(4) 0.3669(2) 0.060(2) Uani 1 d G . H15 H -0.3658(6) 0.5175(6) 0.3289(3) 0.072 Uiso 1 calc R . C16 C -0.1495(5) 0.4377(4) 0.3610(2) 0.048(2) Uani 1 d G . H16 H -0.1047(7) 0.4660(6) 0.3191(2) 0.058 Uiso 1 calc R . C17 C 0.4129(5) 0.3066(4) 0.1453(2) 0.0391(15) Uani 1 d G . C18 C 0.5317(6) 0.2536(5) 0.1993(2) 0.053(2) Uani 1 d G . H18 H 0.5451(8) 0.2805(6) 0.2504(2) 0.064 Uiso 1 calc R . C19 C 0.6303(5) 0.1604(5) 0.1770(3) 0.064(2) Uani 1 d G . H19 H 0.7098(7) 0.1249(7) 0.2131(3) 0.077 Uiso 1 calc R . C20 C 0.6102(6) 0.1202(4) 0.1006(3) 0.073(2) Uani 1 d G . H20 H 0.6762(8) 0.0578(6) 0.0857(4) 0.088 Uiso 1 calc R . C21 C 0.4915(6) 0.1732(5) 0.0467(2) 0.066(2) Uani 1 d G . H21 H 0.4780(9) 0.1463(7) -0.0044(2) 0.079 Uiso 1 calc R . C22 C 0.3928(5) 0.2664(4) 0.0690(2) 0.054(2) Uani 1 d G . H22 H 0.3133(6) 0.3019(6) 0.0329(3) 0.064 Uiso 1 calc R . C23 C 0.4171(5) 0.5734(4) 0.1719(2) 0.042(2) Uani 1 d G . C24 C 0.5779(5) 0.5621(4) 0.1668(3) 0.058(2) Uani 1 d G . H24 H 0.6239(7) 0.4824(5) 0.1659(4) 0.069 Uiso 1 calc R . C25 C 0.6699(4) 0.6700(6) 0.1631(3) 0.075(2) Uani 1 d G . H25 H 0.7775(4) 0.6624(8) 0.1597(4) 0.090 Uiso 1 calc R . C26 C 0.6012(6) 0.7892(4) 0.1645(3) 0.082(3) Uani 1 d G . H26 H 0.6628(9) 0.8613(5) 0.1620(4) 0.099 Uiso 1 calc R . C27 C 0.4404(7) 0.8005(3) 0.1696(3) 0.071(2) Uani 1 d G . H27 H 0.3945(9) 0.8802(4) 0.1706(4) 0.086 Uiso 1 calc R . C28 C 0.3484(4) 0.6926(4) 0.1733(2) 0.052(2) Uani 1 d G . H28 H 0.2409(5) 0.7002(6) 0.1768(4) 0.062 Uiso 1 calc R . C29 C 0.1230(4) 0.4548(5) 0.1026(2) 0.0402(15) Uani 1 d G . C30 C -0.0141(5) 0.3854(5) 0.1070(2) 0.057(2) Uani 1 d G . H30 H -0.0183(7) 0.3321(7) 0.1488(3) 0.069 Uiso 1 calc R . C31 C -0.1448(4) 0.3956(5) 0.0490(3) 0.074(2) Uani 1 d G . H31 H -0.2365(5) 0.3491(8) 0.0519(4) 0.088 Uiso 1 calc R . C32 C -0.1385(5) 0.4751(6) -0.0135(2) 0.070(2) Uani 1 d G . H32 H -0.2260(6) 0.4820(8) -0.0524(3) 0.084 Uiso 1 calc R . C33 C -0.0015(6) 0.5445(5) -0.0180(2) 0.073(2) Uani 1 d G . H33 H 0.0027(9) 0.5978(7) -0.0598(3) 0.087 Uiso 1 calc R . C34 C 0.1292(5) 0.5343(5) 0.0400(3) 0.066(2) Uani 1 d G . H34 H 0.2209(7) 0.5808(7) 0.0371(4) 0.079 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 0.0420(2) 0.0345(2) 0.0338(2) 0.0013(2) 0.0110(2) -0.0015(3) Cl1 0.097(2) 0.0404(10) 0.0544(11) -0.0058(9) 0.0258(10) -0.0117(11) S1 0.0893(14) 0.0360(10) 0.0470(11) -0.0029(9) 0.0253(10) -0.0036(10) P1 0.0394(9) 0.0365(9) 0.0332(9) 0.0008(7) 0.0100(7) 0.0002(8) P2 0.0401(9) 0.0395(10) 0.0340(9) 0.0021(6) 0.0078(7) -0.0032(7) C1 0.054(4) 0.039(4) 0.040(4) 0.005(3) 0.010(3) -0.002(3) C2 0.052(4) 0.038(4) 0.047(4) 0.007(3) 0.009(3) 0.006(3) C3 0.066(5) 0.044(4) 0.065(5) 0.002(4) 0.011(4) -0.006(4) C4 0.090(6) 0.054(7) 0.105(6) -0.022(5) -0.014(5) -0.000(5) C5 0.036(3) 0.047(4) 0.032(3) -0.002(3) 0.011(2) 0.002(3) C6 0.065(5) 0.044(4) 0.042(4) 0.001(3) 0.005(4) 0.008(4) C7 0.080(6) 0.072(6) 0.043(4) 0.016(4) -0.005(4) 0.015(5) C8 0.059(5) 0.079(6) 0.035(4) -0.000(4) -0.003(3) 0.004(5) C9 0.079(6) 0.055(5) 0.045(4) -0.009(4) 0.002(4) -0.003(4) C10 0.063(5) 0.050(4) 0.041(4) -0.001(3) 0.000(4) 0.010(4) C11 0.035(3) 0.037(4) 0.040(3) -0.004(3) 0.009(2) -0.001(3) C12 0.036(3) 0.056(4) 0.043(4) -0.008(3) 0.009(3) -0.003(3) C13 0.046(4) 0.066(6) 0.061(4) -0.016(4) 0.021(3) -0.017(3) C14 0.038(4) 0.073(6) 0.070(5) -0.028(4) 0.016(4) -0.006(3) C15 0.052(4) 0.069(5) 0.055(5) -0.015(4) -0.004(4) 0.014(4) C16 0.047(4) 0.061(4) 0.038(3) -0.001(3) 0.010(3) 0.005(3) C17 0.038(3) 0.047(4) 0.035(3) -0.003(3) 0.013(3) -0.009(3) C18 0.066(5) 0.051(5) 0.044(4) 0.003(3) 0.010(4) 0.014(4) C19 0.064(5) 0.065(6) 0.067(5) 0.011(4) 0.020(4) 0.013(5) C20 0.088(6) 0.052(5) 0.091(6) 0.005(5) 0.050(5) 0.015(5) C21 0.077(5) 0.073(5) 0.051(4) -0.014(4) 0.023(4) 0.006(5) C22 0.055(4) 0.063(5) 0.042(4) -0.009(4) 0.008(3) 0.002(4) C23 0.054(4) 0.043(4) 0.028(3) 0.003(3) 0.006(3) -0.007(3) C24 0.049(5) 0.064(5) 0.060(5) 0.007(4) 0.007(4) -0.016(4) C25 0.063(5) 0.075(6) 0.084(6) 0.011(5) 0.004(4) -0.027(5) C26 0.097(7) 0.069(6) 0.074(6) 0.008(5) -0.005(5) -0.045(6) C27 0.096(7) 0.048(5) 0.062(5) 0.005(4) -0.013(5) -0.015(5) C28 0.057(4) 0.053(5) 0.042(4) 0.003(3) -0.004(3) -0.014(4) C29 0.040(3) 0.042(4) 0.039(3) -0.007(3) 0.009(3) -0.007(3) C30 0.046(3) 0.060(4) 0.064(4) 0.002(5) 0.005(3) -0.002(5) C31 0.047(4) 0.079(5) 0.091(5) 0.002(7) -0.000(4) -0.014(6) C32 0.045(4) 0.087(6) 0.072(6) -0.009(5) -0.014(4) 0.002(4) C33 0.078(5) 0.074(6) 0.060(5) 0.015(4) -0.008(4) -0.002(5) C34 0.071(5) 0.079(6) 0.047(4) 0.019(4) 0.008(4) -0.020(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 Pd1 S1 2.278(2) . ? Pd1 P1 2.283(2) . ? Pd1 P2 2.344(2) . ? Pd1 Cl1 2.345(2) . ? S1 C2 1.847(6) . ? P1 C5 1.816(3) . ? P1 C1 1.816(6) . ? P1 C11 1.825(3) . ? P2 C17 1.822(3) . ? P2 C23 1.825(4) . ? P2 C29 1.829(3) . ? C1 C2 1.507(8) . ? C2 C3 1.505(9) . ? C3 C4 1.496(9) . ? C5 C6 1.39 . ? C5 C10 1.39 . ? C6 C7 1.39 . ? C7 C8 1.39 . ? C8 C9 1.39 . ? C9 C10 1.39 . ? C11 C12 1.39 . ? C11 C16 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C17 C18 1.39 . ? C17 C22 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C23 C24 1.39 . ? C23 C28 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C29 C30 1.39 . ? C29 C34 1.39 . ? C30 C31 1.39 . ? C31 C32 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? 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 S1 Pd1 P1 85.57(6) . . ? S1 Pd1 P2 88.07(6) . . ? P1 Pd1 P2 173.61(6) . . ? S1 Pd1 Cl1 176.98(8) . . ? P1 Pd1 Cl1 93.15(6) . . ? P2 Pd1 Cl1 93.17(6) . . ? C2 S1 Pd1 105.5(2) . . ? C5 P1 C1 106.6(2) . . ? C5 P1 C11 103.5(2) . . ? C1 P1 C11 104.9(3) . . ? C5 P1 Pd1 120.7(2) . . ? C1 P1 Pd1 107.3(2) . . ? C11 P1 Pd1 112.59(14) . . ? C17 P2 C23 103.1(2) . . ? C17 P2 C29 106.1(2) . . ? C23 P2 C29 104.6(2) . . ? C17 P2 Pd1 112.1(2) . . ? C23 P2 Pd1 117.0(2) . . ? C29 P2 Pd1 112.77(15) . . ? C2 C1 P1 108.1(4) . . ? C3 C2 C1 113.4(5) . . ? C3 C2 S1 110.0(5) . . ? C1 C2 S1 108.3(4) . . ? C4 C3 C2 115.8(6) . . ? C6 C5 C10 120.0 . . ? C6 C5 P1 121.3(2) . . ? C10 C5 P1 118.7(2) . . ? C5 C6 C7 120.0 . . ? C8 C7 C6 120.0 . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C9 C10 C5 120.0 . . ? C12 C11 C16 120.0 . . ? C12 C11 P1 119.1(2) . . ? C16 C11 P1 120.9(2) . . ? C11 C12 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C18 C17 C22 120.0 . . ? C18 C17 P2 117.2(3) . . ? C22 C17 P2 122.7(3) . . ? C19 C18 C17 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? C24 C23 C28 120.0 . . ? C24 C23 P2 120.8(3) . . ? C28 C23 P2 119.2(3) . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C27 C28 C23 120.0 . . ? C30 C29 C34 120.0 . . ? C30 C29 P2 118.3(2) . . ? C34 C29 P2 121.6(2) . . ? C29 C30 C31 120.0 . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C29 120.0 . . ? 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 Pd1 S1 C2 15.2(2) . . . . ? P2 Pd1 S1 C2 -164.3(2) . . . . ? Cl1 Pd1 S1 C2 -50.0(15) . . . . ? S1 Pd1 P1 C5 132.7(2) . . . . ? P2 Pd1 P1 C5 137.7(6) . . . . ? Cl1 Pd1 P1 C5 -50.1(2) . . . . ? S1 Pd1 P1 C1 10.4(2) . . . . ? P2 Pd1 P1 C1 15.5(7) . . . . ? Cl1 Pd1 P1 C1 -172.3(2) . . . . ? S1 Pd1 P1 C11 -104.6(2) . . . . ? P2 Pd1 P1 C11 -99.5(6) . . . . ? Cl1 Pd1 P1 C11 72.7(2) . . . . ? S1 Pd1 P2 C17 -36.2(2) . . . . ? P1 Pd1 P2 C17 -41.3(6) . . . . ? Cl1 Pd1 P2 C17 146.5(2) . . . . ? S1 Pd1 P2 C23 -155.0(2) . . . . ? P1 Pd1 P2 C23 -160.1(5) . . . . ? Cl1 Pd1 P2 C23 27.7(2) . . . . ? S1 Pd1 P2 C29 83.5(2) . . . . ? P1 Pd1 P2 C29 78.5(6) . . . . ? Cl1 Pd1 P2 C29 -93.7(2) . . . . ? C5 P1 C1 C2 -171.3(4) . . . . ? C11 P1 C1 C2 79.3(5) . . . . ? Pd1 P1 C1 C2 -40.7(5) . . . . ? P1 C1 C2 C3 177.2(5) . . . . ? P1 C1 C2 S1 54.8(5) . . . . ? Pd1 S1 C2 C3 -169.0(4) . . . . ? Pd1 S1 C2 C1 -44.6(5) . . . . ? C1 C2 C3 C4 176.0(6) . . . . ? S1 C2 C3 C4 -62.5(8) . . . . ? C1 P1 C5 C6 8.3(3) . . . . ? C11 P1 C5 C6 118.7(3) . . . . ? Pd1 P1 C5 C6 -114.3(2) . . . . ? C1 P1 C5 C10 -172.8(3) . . . . ? C11 P1 C5 C10 -62.4(3) . . . . ? Pd1 P1 C5 C10 64.6(3) . . . . ? C10 C5 C6 C7 0.0 . . . . ? P1 C5 C6 C7 178.9(3) . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C5 0.0 . . . . ? C6 C5 C10 C9 0.0 . . . . ? P1 C5 C10 C9 -178.9(3) . . . . ? C5 P1 C11 C12 -52.8(3) . . . . ? C1 P1 C11 C12 58.8(3) . . . . ? Pd1 P1 C11 C12 175.2(2) . . . . ? C5 P1 C11 C16 127.4(3) . . . . ? C1 P1 C11 C16 -120.9(3) . . . . ? Pd1 P1 C11 C16 -4.5(3) . . . . ? C16 C11 C12 C13 0.0 . . . . ? P1 C11 C12 C13 -179.8(3) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C11 0.0 . . . . ? C12 C11 C16 C15 0.0 . . . . ? P1 C11 C16 C15 179.7(3) . . . . ? C23 P2 C17 C18 83.6(3) . . . . ? C29 P2 C17 C18 -166.6(2) . . . . ? Pd1 P2 C17 C18 -43.1(3) . . . . ? C23 P2 C17 C22 -93.6(3) . . . . ? C29 P2 C17 C22 16.1(3) . . . . ? Pd1 P2 C17 C22 139.7(2) . . . . ? C22 C17 C18 C19 0.0 . . . . ? P2 C17 C18 C19 -177.3(3) . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C17 0.0 . . . . ? C18 C17 C22 C21 0.0 . . . . ? P2 C17 C22 C21 177.2(4) . . . . ? C17 P2 C23 C24 -17.5(3) . . . . ? C29 P2 C23 C24 -128.4(3) . . . . ? Pd1 P2 C23 C24 106.0(2) . . . . ? C17 P2 C23 C28 163.4(3) . . . . ? C29 P2 C23 C28 52.6(3) . . . . ? Pd1 P2 C23 C28 -73.1(3) . . . . ? C28 C23 C24 C25 0.0 . . . . ? P2 C23 C24 C25 -179.1(3) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C23 0.0 . . . . ? C24 C23 C28 C27 0.0 . . . . ? P2 C23 C28 C27 179.1(3) . . . . ? C17 P2 C29 C30 90.6(3) . . . . ? C23 P2 C29 C30 -160.8(3) . . . . ? Pd1 P2 C29 C30 -32.5(3) . . . . ? C17 P2 C29 C34 -86.9(3) . . . . ? C23 P2 C29 C34 21.7(4) . . . . ? Pd1 P2 C29 C34 150.0(3) . . . . ? C34 C29 C30 C31 0.0 . . . . ? P2 C29 C30 C31 -177.5(4) . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C29 0.0 . . . . ? C30 C29 C34 C33 0.0 . . . . ? P2 C29 C34 C33 177.5(4) . . . . ? _refine_diff_density_max 0.392 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.074 data_9 _database_code_CSD 194256 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H21 Cl2 P Pd S' _chemical_formula_weight 465.67 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8678(18) _cell_length_b 15.492(3) _cell_length_c 13.085(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.49(3) _cell_angle_gamma 90.00 _cell_volume 1789.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19520 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.7488 _exptl_absorpt_correction_T_max 0.8870 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 24775 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4094 _reflns_number_gt 3669 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & Collect (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0627P)^2^+0.3583P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4094 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.093 _refine_ls_shift/su_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_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 C1 C -0.2062(3) -0.10088(16) 0.14213(19) 0.0237(5) Uani 1 1 d . . . H1 H -0.2103 -0.1097 0.2175 0.028 Uiso 1 1 calc R . . C2 C -0.3043(3) -0.17059(17) 0.0841(2) 0.0272(6) Uani 1 1 d . . . H2A H -0.2688 -0.2278 0.1100 0.033 Uiso 1 1 calc R . . H2B H -0.4100 -0.1635 0.1011 0.033 Uiso 1 1 calc R . . C3 C -0.3048(3) -0.1706(2) -0.0313(2) 0.0354(7) Uani 1 1 d . . . H3A H -0.3429 -0.1150 -0.0587 0.053 Uiso 1 1 calc R . . H3B H -0.3703 -0.2171 -0.0604 0.053 Uiso 1 1 calc R . . H3C H -0.2014 -0.1796 -0.0498 0.053 Uiso 1 1 calc R . . C4 C -0.2546(3) -0.00933(16) 0.1157(2) 0.0239(6) Uani 1 1 d . . . H4A H -0.3610 -0.0003 0.1302 0.029 Uiso 1 1 calc R . . H4B H -0.2471 0.0019 0.0419 0.029 Uiso 1 1 calc R . . C5 C -0.1988(3) 0.07020(14) 0.32038(18) 0.0180(5) Uani 1 1 d . . . C6 C -0.3548(3) 0.07367(16) 0.3288(2) 0.0236(5) Uani 1 1 d . . . H6 H -0.4243 0.0713 0.2689 0.028 Uiso 1 1 calc R . . C7 C -0.4075(3) 0.08058(17) 0.4249(2) 0.0275(6) Uani 1 1 d . . . H7 H -0.5134 0.0815 0.4306 0.033 Uiso 1 1 calc R . . C8 C -0.3072(3) 0.08619(18) 0.5126(2) 0.0290(6) Uani 1 1 d . . . H8 H -0.3440 0.0915 0.5781 0.035 Uiso 1 1 calc R . . C9 C -0.1528(3) 0.08393(18) 0.5040(2) 0.0285(6) Uani 1 1 d . . . H9 H -0.0836 0.0882 0.5639 0.034 Uiso 1 1 calc R . . C10 C -0.0980(3) 0.07546(16) 0.40843(19) 0.0228(5) Uani 1 1 d . . . H10 H 0.0080 0.0733 0.4033 0.027 Uiso 1 1 calc R . . C11 C -0.1653(3) 0.17037(15) 0.13958(17) 0.0176(5) Uani 1 1 d . . . C12 C -0.2750(3) 0.18287(17) 0.0565(2) 0.0264(6) Uani 1 1 d . . . H12 H -0.3287 0.1348 0.0261 0.032 Uiso 1 1 calc R . . C13 C -0.3051(3) 0.26501(18) 0.0187(2) 0.0314(6) Uani 1 1 d . . . H13 H -0.3797 0.2730 -0.0376 0.038 Uiso 1 1 calc R . . C14 C -0.2279(3) 0.33589(17) 0.0622(2) 0.0258(5) Uani 1 1 d . . . H14 H -0.2498 0.3922 0.0362 0.031 Uiso 1 1 calc R . . C15 C -0.1184(3) 0.32378(16) 0.14374(19) 0.0219(5) Uani 1 1 d . . . H15 H -0.0644 0.3720 0.1733 0.026 Uiso 1 1 calc R . . C16 C -0.0872(3) 0.24188(16) 0.18253(18) 0.0203(5) Uani 1 1 d . . . H16 H -0.0121 0.2343 0.2387 0.024 Uiso 1 1 calc R . . C17 C 0.0499(4) -0.2014(2) 0.1909(3) 0.0507(9) Uani 1 1 d . . . H17A H 0.0127 -0.1956 0.2587 0.076 Uiso 1 1 calc R . . H17B H 0.1607 -0.2056 0.1987 0.076 Uiso 1 1 calc R . . H17C H 0.0071 -0.2537 0.1573 0.076 Uiso 1 1 calc R . . P1 P -0.12888(6) 0.06436(4) 0.19436(5) 0.01624(15) Uani 1 1 d . . . S1 S -0.00685(7) -0.10807(4) 0.11345(5) 0.02293(16) Uani 1 1 d . . . Cl1 Cl 0.34235(6) -0.05812(4) 0.17990(5) 0.02500(15) Uani 1 1 d . . . Cl2 Cl 0.21998(6) 0.12283(4) 0.28283(5) 0.02428(15) Uani 1 1 d . . . Pd1 Pd 0.104423(18) 0.008175(11) 0.194753(12) 0.01454(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0250(13) 0.0219(13) 0.0245(13) -0.0006(10) 0.0038(10) 0.0003(10) C2 0.0237(13) 0.0220(13) 0.0360(15) -0.0057(11) 0.0027(10) -0.0055(10) C3 0.0389(16) 0.0356(16) 0.0312(15) 0.0003(12) 0.0006(12) -0.0128(12) C4 0.0191(14) 0.0212(13) 0.0310(15) -0.0055(10) 0.0000(11) -0.0007(9) C5 0.0199(11) 0.0108(11) 0.0241(12) 0.0026(9) 0.0057(9) 0.0014(8) C6 0.0209(12) 0.0206(12) 0.0296(13) 0.0015(10) 0.0048(10) 0.0021(9) C7 0.0243(13) 0.0270(14) 0.0326(14) 0.0066(11) 0.0100(10) 0.0021(10) C8 0.0323(14) 0.0279(14) 0.0289(14) 0.0034(11) 0.0129(11) 0.0046(11) C9 0.0337(14) 0.0284(14) 0.0233(13) 0.0011(11) 0.0024(10) 0.0026(11) C10 0.0213(12) 0.0198(12) 0.0285(13) 0.0012(10) 0.0075(10) -0.0002(9) C11 0.0175(11) 0.0188(12) 0.0173(11) -0.0022(9) 0.0058(8) 0.0011(9) C12 0.0301(14) 0.0219(13) 0.0255(13) -0.0022(10) -0.0054(10) -0.0031(10) C13 0.0364(15) 0.0308(15) 0.0253(13) 0.0072(11) -0.0049(11) 0.0007(11) C14 0.0285(13) 0.0224(13) 0.0273(13) 0.0094(10) 0.0061(10) 0.0021(10) C15 0.0210(12) 0.0173(12) 0.0281(13) -0.0008(10) 0.0071(9) -0.0022(9) C16 0.0191(12) 0.0202(12) 0.0214(12) -0.0023(9) 0.0006(9) 0.0007(9) C17 0.0446(19) 0.0184(15) 0.086(3) 0.0081(16) -0.0087(17) 0.0001(13) P1 0.0148(3) 0.0126(3) 0.0214(3) -0.0029(2) 0.0021(2) 0.0001(2) S1 0.0190(3) 0.0168(3) 0.0328(4) -0.0085(2) 0.0017(2) 0.0013(2) Cl1 0.0167(3) 0.0259(3) 0.0320(3) -0.0058(2) 0.0004(2) 0.0053(2) Cl2 0.0186(3) 0.0222(3) 0.0318(3) -0.0093(2) 0.0009(2) -0.0036(2) Pd1 0.01338(14) 0.01363(13) 0.01663(14) -0.00096(6) 0.00154(8) 0.00024(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.512(4) . ? C1 C2 1.541(4) . ? C1 S1 1.846(3) . ? C2 C3 1.510(4) . ? C4 P1 1.840(3) . ? C5 C10 1.391(3) . ? C5 C6 1.399(3) . ? C5 P1 1.819(2) . ? C6 C7 1.386(4) . ? C7 C8 1.386(4) . ? C8 C9 1.385(4) . ? C9 C10 1.390(4) . ? C11 C16 1.396(3) . ? C11 C12 1.401(3) . ? C11 P1 1.809(2) . ? C12 C13 1.382(4) . ? C13 C14 1.387(4) . ? C14 C15 1.385(4) . ? C15 C16 1.385(3) . ? C17 S1 1.810(3) . ? P1 Pd1 2.2441(7) . ? S1 Pd1 2.2688(7) . ? Cl1 Pd1 2.3713(7) . ? Cl2 Pd1 2.3037(7) . ? 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 C4 C1 C2 114.3(2) . . ? C4 C1 S1 105.44(17) . . ? C2 C1 S1 111.35(17) . . ? C3 C2 C1 116.1(2) . . ? C1 C4 P1 108.13(18) . . ? C10 C5 C6 119.6(2) . . ? C10 C5 P1 120.39(17) . . ? C6 C5 P1 119.93(19) . . ? C7 C6 C5 119.7(2) . . ? C8 C7 C6 120.7(2) . . ? C7 C8 C9 119.5(2) . . ? C8 C9 C10 120.6(3) . . ? C9 C10 C5 119.9(2) . . ? C16 C11 C12 118.9(2) . . ? C16 C11 P1 119.88(18) . . ? C12 C11 P1 121.16(18) . . ? C13 C12 C11 120.1(2) . . ? C12 C13 C14 120.8(2) . . ? C15 C14 C13 119.4(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 120.4(2) . . ? C11 P1 C5 104.51(10) . . ? C11 P1 C4 105.45(11) . . ? C5 P1 C4 107.27(12) . . ? C11 P1 Pd1 118.88(8) . . ? C5 P1 Pd1 114.30(8) . . ? C4 P1 Pd1 105.64(9) . . ? C17 S1 C1 98.90(15) . . ? C17 S1 Pd1 106.66(12) . . ? C1 S1 Pd1 103.82(8) . . ? P1 Pd1 S1 86.98(3) . . ? P1 Pd1 Cl2 93.89(3) . . ? S1 Pd1 Cl2 177.75(2) . . ? P1 Pd1 Cl1 174.37(2) . . ? S1 Pd1 Cl1 88.18(3) . . ? Cl2 Pd1 Cl1 91.05(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.944 _refine_diff_density_min -1.561 _refine_diff_density_rms 0.153 ##END