# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Norihiro Tokitoh' _publ_contact_author_address ; Institute for Chemical Research Kyoto University Gokasho Uji Kyoto 611-0011 JAPAN ; _publ_contact_author_email TOKITOH@BOC.KUICR.KYOTO-U.AC.JP _publ_section_title ; Unusual Carbon-Sulfur Bond Cleavage in the Reaction of a New Type of Bulky Hexathioether with a Zerovalent Palladium Complex ; loop_ _publ_author_name 'Norihiro Tokitoh' 'Daisuke Shimizu' 'Nobuhiro Takeda' # Attachment 'compound4.CIF' data_pd3s4 _database_code_depnum_ccdc_archive 'CCDC 285411' _audit_creation_date 2005-09-06 _audit_update_record ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C114 H164 P2 Pd3 S6 Si12, 3.2(C6 H6), 0.8(C1 H1 Cl3)' _chemical_formula_sum 'C134 H184 Cl2.40 P2 Pd3 S6 Si12' _chemical_formula_weight 2790.47 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' Cl Cl 0.1484 0.1585 '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' Pd Pd -0.9988 1.0072 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 31.9316(5) _cell_length_b 24.7082(6) _cell_length_c 24.0157(5) _cell_angle_alpha 90.00 _cell_angle_beta 130.2043(8) _cell_angle_gamma 90.00 _cell_volume 14471.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 11285 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5843 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8252 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 47590 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12714 _reflns_number_gt 8144 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution SIR97 _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^)+(0.0320P)^2^+0.0010P] 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 12714 _refine_ls_number_parameters 769 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.069358(12) 0.661941(13) 0.402518(16) 0.01816(9) Uani 1 1 d . . . Pd2 Pd 0.0000 0.724036(18) 0.2500 0.01740(12) Uani 1 2 d S . . S1 S 0.09290(4) 0.71520(4) 0.33911(5) 0.0196(2) Uani 1 1 d . . . C1 C 0.10962(15) 0.68414(15) 0.2884(2) 0.0193(10) Uani 1 1 d . . . C2 C 0.16104(15) 0.65995(16) 0.3252(2) 0.0237(10) Uani 1 1 d . . . H1 H 0.1860 0.6585 0.3770 0.028 Uiso 1 1 calc R . . C3 C 0.17575(17) 0.63838(17) 0.2875(2) 0.0298(11) Uani 1 1 d . . . H2 H 0.2104 0.6212 0.3130 0.036 Uiso 1 1 calc R . . C4 C 0.14025(16) 0.64151(16) 0.2121(2) 0.0262(11) Uani 1 1 d . . . H3 H 0.1508 0.6269 0.1862 0.031 Uiso 1 1 calc R . . C5 C 0.08963(16) 0.66565(16) 0.1746(2) 0.0241(10) Uani 1 1 d . . . H4 H 0.0657 0.6683 0.1229 0.029 Uiso 1 1 calc R . . C6 C 0.07326(15) 0.68632(16) 0.2121(2) 0.0188(10) Uani 1 1 d . . . S2 S 0.00899(4) 0.72042(4) 0.16330(5) 0.0197(2) Uani 1 1 d . . . C7 C 0.04860(15) 0.63988(16) 0.4628(2) 0.0189(10) Uani 1 1 d . . . C8 C 0.02009(15) 0.59306(17) 0.4527(2) 0.0217(10) Uani 1 1 d . . . H5 H 0.0130 0.5663 0.4190 0.026 Uiso 1 1 calc R . . C9 C 0.00204(16) 0.58515(17) 0.4913(2) 0.0247(11) Uani 1 1 d . . . H6 H -0.0166 0.5527 0.4848 0.030 Uiso 1 1 calc R . . C10 C 0.01097(16) 0.62394(17) 0.5390(2) 0.0270(11) Uani 1 1 d . . . H7 H -0.0030 0.6190 0.5636 0.032 Uiso 1 1 calc R . . C11 C 0.04053(16) 0.67034(17) 0.5513(2) 0.0249(11) Uani 1 1 d . . . H8 H 0.0472 0.6969 0.5847 0.030 Uiso 1 1 calc R . . C12 C 0.06023(15) 0.67772(16) 0.5149(2) 0.0188(10) Uani 1 1 d . . . S3 S 0.10601(4) 0.73061(4) 0.53487(5) 0.0206(2) Uani 1 1 d . . . C13 C 0.10236(15) 0.78255(16) 0.5834(2) 0.0189(10) Uani 1 1 d . . . C14 C 0.07437(15) 0.83072(17) 0.5462(2) 0.0220(10) Uani 1 1 d . . . C15 C 0.08004(16) 0.87476(17) 0.5864(2) 0.0229(10) Uani 1 1 d . . . H9 H 0.0611 0.9072 0.5611 0.027 Uiso 1 1 calc R . . C16 C 0.11179(16) 0.87385(16) 0.6612(2) 0.0216(10) Uani 1 1 d . . . C17 C 0.13834(16) 0.82569(17) 0.6967(2) 0.0236(10) Uani 1 1 d . . . H10 H 0.1599 0.8240 0.7481 0.028 Uiso 1 1 calc R . . C18 C 0.13464(15) 0.77952(17) 0.6599(2) 0.0204(10) Uani 1 1 d . . . C19 C 0.03981(16) 0.83855(17) 0.4644(2) 0.0251(10) Uani 1 1 d . . . H11 H 0.0399 0.8021 0.4464 0.030 Uiso 1 1 calc R . . C20 C 0.11751(16) 0.92505(16) 0.7014(2) 0.0226(10) Uani 1 1 d . . . H12 H 0.0951 0.9522 0.6613 0.027 Uiso 1 1 calc R . . C21 C 0.16423(16) 0.72871(16) 0.7033(2) 0.0237(10) Uani 1 1 d . . . H13 H 0.1491 0.6998 0.6655 0.028 Uiso 1 1 calc R . . Si1 Si -0.03495(5) 0.85060(5) 0.41787(7) 0.0341(4) Uani 1 1 d . . . Si2 Si 0.07667(6) 0.88326(5) 0.44460(7) 0.0346(3) Uani 1 1 d . . . Si3 Si 0.08056(5) 0.91912(5) 0.73843(7) 0.0324(3) Uani 1 1 d . . . Si4 Si 0.18905(5) 0.95429(5) 0.75958(6) 0.0244(3) Uani 1 1 d . . . Si5 Si 0.14711(6) 0.70485(5) 0.76151(7) 0.0386(4) Uani 1 1 d . . . Si6 Si 0.24029(5) 0.73080(5) 0.75096(7) 0.0338(3) Uani 1 1 d . . . C22 C -0.05695(18) 0.7947(2) 0.4454(3) 0.0478(14) Uani 1 1 d . . . H14 H -0.0956 0.7996 0.4221 0.072 Uiso 1 1 calc R . . H15 H -0.0346 0.7950 0.4985 0.072 Uiso 1 1 calc R . . H16 H -0.0522 0.7601 0.4302 0.072 Uiso 1 1 calc R . . C23 C -0.04954(19) 0.91578(19) 0.4429(2) 0.0499(15) Uani 1 1 d . . . H17 H -0.0892 0.9198 0.4139 0.075 Uiso 1 1 calc R . . H18 H -0.0354 0.9462 0.4331 0.075 Uiso 1 1 calc R . . H19 H -0.0316 0.9152 0.4949 0.075 Uiso 1 1 calc R . . C24 C -0.07737(18) 0.85066(19) 0.3165(2) 0.0431(14) Uani 1 1 d . . . H20 H -0.0686 0.8186 0.3018 0.065 Uiso 1 1 calc R . . H21 H -0.0694 0.8833 0.3017 0.065 Uiso 1 1 calc R . . H22 H -0.1163 0.8501 0.2930 0.065 Uiso 1 1 calc R . . C25 C 0.0686(3) 0.9574(2) 0.4536(3) 0.074(2) Uani 1 1 d . . . H23 H 0.0887 0.9787 0.4432 0.110 Uiso 1 1 calc R . . H24 H 0.0833 0.9650 0.5034 0.110 Uiso 1 1 calc R . . H25 H 0.0297 0.9671 0.4190 0.110 Uiso 1 1 calc R . . C26 C 0.05023(18) 0.87208(19) 0.3501(2) 0.0388(13) Uani 1 1 d . . . H26 H 0.0722 0.8930 0.3425 0.058 Uiso 1 1 calc R . . H27 H 0.0119 0.8838 0.3152 0.058 Uiso 1 1 calc R . . H28 H 0.0526 0.8335 0.3430 0.058 Uiso 1 1 calc R . . C27 C 0.15119(17) 0.8661(2) 0.5099(2) 0.0529(16) Uani 1 1 d . . . H29 H 0.1562 0.8281 0.5037 0.079 Uiso 1 1 calc R . . H30 H 0.1656 0.8719 0.5600 0.079 Uiso 1 1 calc R . . H31 H 0.1709 0.8893 0.5005 0.079 Uiso 1 1 calc R . . C28 C 0.1108(2) 0.86763(19) 0.8117(3) 0.0481(14) Uani 1 1 d . . . H32 H 0.1500 0.8750 0.8502 0.072 Uiso 1 1 calc R . . H33 H 0.1059 0.8315 0.7913 0.072 Uiso 1 1 calc R . . H34 H 0.0924 0.8693 0.8321 0.072 Uiso 1 1 calc R . . C29 C 0.08170(19) 0.98574(19) 0.7761(3) 0.0453(14) Uani 1 1 d . . . H35 H 0.0696 1.0143 0.7402 0.068 Uiso 1 1 calc R . . H36 H 0.1191 0.9935 0.8209 0.068 Uiso 1 1 calc R . . H37 H 0.0570 0.9844 0.7871 0.068 Uiso 1 1 calc R . . C30 C 0.00816(19) 0.9000(2) 0.6614(3) 0.0544(15) Uani 1 1 d . . . H38 H -0.0125 0.8983 0.6787 0.082 Uiso 1 1 calc R . . H39 H 0.0073 0.8645 0.6425 0.082 Uiso 1 1 calc R . . H40 H -0.0084 0.9271 0.6226 0.082 Uiso 1 1 calc R . . C31 C 0.22118(17) 0.93424(18) 0.7198(2) 0.0343(12) Uani 1 1 d . . . H41 H 0.2245 0.8947 0.7211 0.052 Uiso 1 1 calc R . . H42 H 0.2577 0.9506 0.7483 0.052 Uiso 1 1 calc R . . H43 H 0.1983 0.9468 0.6692 0.052 Uiso 1 1 calc R . . C32 C 0.23314(17) 0.93180(18) 0.8567(2) 0.0364(12) Uani 1 1 d . . . H44 H 0.2172 0.9444 0.8782 0.055 Uiso 1 1 calc R . . H45 H 0.2700 0.9470 0.8841 0.055 Uiso 1 1 calc R . . H46 H 0.2354 0.8922 0.8589 0.055 Uiso 1 1 calc R . . C33 C 0.18306(17) 1.02940(16) 0.7540(2) 0.0334(12) Uani 1 1 d . . . H47 H 0.1669 1.0412 0.7048 0.050 Uiso 1 1 calc R . . H48 H 0.2195 1.0455 0.7895 0.050 Uiso 1 1 calc R . . H49 H 0.1596 1.0410 0.7647 0.050 Uiso 1 1 calc R . . C34 C 0.0761(2) 0.7236(2) 0.7205(3) 0.0501(14) Uani 1 1 d . . . H50 H 0.0680 0.7602 0.7000 0.075 Uiso 1 1 calc R . . H51 H 0.0726 0.7227 0.7581 0.075 Uiso 1 1 calc R . . H52 H 0.0503 0.6979 0.6817 0.075 Uiso 1 1 calc R . . C35 C 0.1502(2) 0.62908(18) 0.7649(3) 0.0565(16) Uani 1 1 d . . . H53 H 0.1251 0.6146 0.7152 0.085 Uiso 1 1 calc R . . H54 H 0.1394 0.6158 0.7925 0.085 Uiso 1 1 calc R . . H55 H 0.1876 0.6172 0.7888 0.085 Uiso 1 1 calc R . . C36 C 0.1939(2) 0.7313(2) 0.8576(2) 0.0607(17) Uani 1 1 d . . . H56 H 0.2313 0.7184 0.8829 0.091 Uiso 1 1 calc R . . H57 H 0.1813 0.7183 0.8832 0.091 Uiso 1 1 calc R . . H58 H 0.1934 0.7709 0.8568 0.091 Uiso 1 1 calc R . . C37 C 0.27218(19) 0.66371(19) 0.7949(3) 0.0598(17) Uani 1 1 d . . . H59 H 0.2520 0.6349 0.7584 0.090 Uiso 1 1 calc R . . H60 H 0.2708 0.6575 0.8340 0.090 Uiso 1 1 calc R . . H61 H 0.3105 0.6636 0.8154 0.090 Uiso 1 1 calc R . . C38 C 0.27845(18) 0.78365(19) 0.8232(2) 0.0427(13) Uani 1 1 d . . . H62 H 0.3174 0.7823 0.8465 0.064 Uiso 1 1 calc R . . H63 H 0.2744 0.7771 0.8598 0.064 Uiso 1 1 calc R . . H64 H 0.2636 0.8194 0.8013 0.064 Uiso 1 1 calc R . . C39 C 0.24939(18) 0.7437(2) 0.6835(2) 0.0497(15) Uani 1 1 d . . . H65 H 0.2292 0.7764 0.6557 0.075 Uiso 1 1 calc R . . H66 H 0.2353 0.7128 0.6502 0.075 Uiso 1 1 calc R . . H67 H 0.2884 0.7486 0.7089 0.075 Uiso 1 1 calc R . . P1 P 0.13825(4) 0.60059(4) 0.45873(6) 0.0201(3) Uani 1 1 d . . . C40 C 0.13000(17) 0.56087(16) 0.3876(2) 0.0254(11) Uani 1 1 d . . . C41 C 0.17300(18) 0.53316(17) 0.3991(2) 0.0319(12) Uani 1 1 d . . . H68 H 0.2083 0.5324 0.4461 0.038 Uiso 1 1 calc R . . C42 C 0.1639(2) 0.50687(19) 0.3415(3) 0.0443(14) Uani 1 1 d . . . H69 H 0.1933 0.4884 0.3493 0.053 Uiso 1 1 calc R . . C43 C 0.1132(2) 0.50679(19) 0.2731(3) 0.0482(15) Uani 1 1 d . . . H70 H 0.1077 0.4882 0.2342 0.058 Uiso 1 1 calc R . . C44 C 0.0704(2) 0.53396(19) 0.2614(3) 0.0495(15) Uani 1 1 d . . . H71 H 0.0352 0.5341 0.2143 0.059 Uiso 1 1 calc R . . C45 C 0.07882(18) 0.56110(18) 0.3186(2) 0.0361(12) Uani 1 1 d . . . H72 H 0.0493 0.5799 0.3103 0.043 Uiso 1 1 calc R . . C46 C 0.13945(15) 0.55149(17) 0.5166(2) 0.0229(10) Uani 1 1 d . . . C47 C 0.11911(15) 0.49959(17) 0.4932(2) 0.0264(11) Uani 1 1 d . . . H73 H 0.1076 0.4870 0.4478 0.032 Uiso 1 1 calc R . . C48 C 0.11546(17) 0.46569(19) 0.5363(3) 0.0348(12) Uani 1 1 d . . . H74 H 0.1017 0.4299 0.5205 0.042 Uiso 1 1 calc R . . C49 C 0.13183(17) 0.4842(2) 0.6020(3) 0.0373(13) Uani 1 1 d . . . H75 H 0.1286 0.4613 0.6308 0.045 Uiso 1 1 calc R . . C50 C 0.15289(17) 0.53583(19) 0.6262(2) 0.0334(12) Uani 1 1 d . . . H76 H 0.1647 0.5481 0.6719 0.040 Uiso 1 1 calc R . . C51 C 0.15658(15) 0.56940(18) 0.5834(2) 0.0257(11) Uani 1 1 d . . . H77 H 0.1709 0.6049 0.5998 0.031 Uiso 1 1 calc R . . C52 C 0.20839(15) 0.62643(17) 0.5189(2) 0.0207(10) Uani 1 1 d . . . C53 C 0.21835(16) 0.68133(17) 0.5214(2) 0.0234(10) Uani 1 1 d . . . H78 H 0.1884 0.7056 0.4914 0.028 Uiso 1 1 calc R . . C54 C 0.27159(16) 0.70127(18) 0.5671(2) 0.0267(11) Uani 1 1 d . . . H79 H 0.2779 0.7390 0.5684 0.032 Uiso 1 1 calc R . . C55 C 0.31522(17) 0.66633(19) 0.6106(2) 0.0297(11) Uani 1 1 d . . . H80 H 0.3517 0.6798 0.6416 0.036 Uiso 1 1 calc R . . C56 C 0.30580(17) 0.61169(19) 0.6091(2) 0.0364(13) Uani 1 1 d . . . H81 H 0.3360 0.5877 0.6390 0.044 Uiso 1 1 calc R . . C57 C 0.25273(16) 0.59141(18) 0.5644(2) 0.0291(11) Uani 1 1 d . . . H82 H 0.2466 0.5538 0.5647 0.035 Uiso 1 1 calc R . . C58 C 0.0942(4) 0.3839(3) 0.3707(4) 0.086(2) Uani 1 1 d . . . H83 H 0.0828 0.4122 0.3368 0.103 Uiso 1 1 calc R . . C59 C 0.1467(4) 0.3804(3) 0.4320(4) 0.100(3) Uani 1 1 d . . . H84 H 0.1726 0.4061 0.4409 0.121 Uiso 1 1 calc R . . C60 C 0.1633(4) 0.3411(3) 0.4809(4) 0.137(4) Uani 1 1 d . . . H85 H 0.2006 0.3389 0.5240 0.165 Uiso 1 1 calc R . . C61 C 0.1260(4) 0.3040(3) 0.4686(4) 0.107(3) Uani 1 1 d . . . H86 H 0.1377 0.2769 0.5041 0.129 Uiso 1 1 calc R . . C62 C 0.0733(3) 0.3054(3) 0.4069(4) 0.094(2) Uani 1 1 d . . . H87 H 0.0477 0.2789 0.3974 0.113 Uiso 1 1 calc R . . C63 C 0.0573(3) 0.3466(4) 0.3575(4) 0.103(3) Uani 1 1 d . . . H88 H 0.0202 0.3488 0.3139 0.124 Uiso 1 1 calc R . . C64 C 0.1404(3) 0.1440(4) 0.4909(5) 0.085(5) Uani 0.60 1 d PG A 1 H89 H 0.1118 0.1647 0.4828 0.102 Uiso 0.60 1 calc PR A 1 C65 C 0.1788(4) 0.1691(3) 0.4897(5) 0.160(9) Uani 0.60 1 d PG A 1 H90 H 0.1764 0.2069 0.4808 0.193 Uiso 0.60 1 calc PR A 1 C66 C 0.2206(3) 0.1389(4) 0.5015(4) 0.105(5) Uani 0.60 1 d PG A 1 H91 H 0.2468 0.1560 0.5007 0.126 Uiso 0.60 1 calc PR A 1 C67 C 0.2240(3) 0.0836(4) 0.5145(4) 0.092(4) Uani 0.60 1 d PG A 1 H92 H 0.2526 0.0629 0.5226 0.110 Uiso 0.60 1 calc PR A 1 C68 C 0.1856(5) 0.0585(3) 0.5157(5) 0.194(5) Uani 0.60 1 d PGU A 1 H93 H 0.1879 0.0207 0.5246 0.233 Uiso 0.60 1 calc PR A 1 C69 C 0.1438(4) 0.0888(4) 0.5039(5) 0.110(6) Uani 0.60 1 d PG A 1 H94 H 0.1176 0.0716 0.5048 0.132 Uiso 0.60 1 calc PR A 1 C70 C 0.1774(18) 0.0670(7) 0.5238(15) 0.221(6) Uani 0.40 1 d PDU B 2 H95 H 0.1377 0.0570 0.4898 0.265 Uiso 0.40 1 calc PR B 2 Cl1 Cl 0.1890(4) 0.0441(4) 0.5951(4) 0.203(3) Uani 0.40 1 d PDU B 2 Cl2 Cl 0.1912(4) 0.0337(4) 0.4804(4) 0.203(3) Uani 0.40 1 d PDU B 2 Cl3 Cl 0.1664(5) 0.1309(7) 0.5121(8) 0.278(5) Uani 0.40 1 d PDU B 2 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 0.01376(16) 0.02036(19) 0.01882(18) 0.00012(15) 0.00983(14) 0.00043(15) Pd2 0.0134(2) 0.0179(3) 0.0195(3) 0.000 0.0100(2) 0.000 S1 0.0149(5) 0.0217(6) 0.0203(6) -0.0010(5) 0.0105(5) -0.0012(5) C1 0.016(2) 0.016(2) 0.025(3) -0.0009(19) 0.013(2) -0.0038(18) C2 0.016(2) 0.026(3) 0.023(2) 0.000(2) 0.009(2) -0.002(2) C3 0.024(2) 0.027(3) 0.039(3) 0.000(2) 0.021(2) 0.005(2) C4 0.023(2) 0.027(3) 0.034(3) -0.006(2) 0.021(2) -0.002(2) C5 0.022(2) 0.023(3) 0.026(2) -0.005(2) 0.015(2) -0.007(2) C6 0.017(2) 0.018(2) 0.023(3) 0.0001(19) 0.013(2) -0.0040(19) S2 0.0163(5) 0.0211(6) 0.0206(6) 0.0011(5) 0.0114(5) -0.0008(5) C7 0.014(2) 0.021(2) 0.021(2) 0.008(2) 0.010(2) 0.0052(19) C8 0.015(2) 0.024(3) 0.022(2) 0.001(2) 0.010(2) 0.0012(19) C9 0.018(2) 0.020(3) 0.032(3) 0.002(2) 0.015(2) -0.0035(19) C10 0.024(2) 0.031(3) 0.030(3) 0.001(2) 0.020(2) -0.003(2) C11 0.023(2) 0.028(3) 0.024(3) -0.003(2) 0.015(2) 0.001(2) C12 0.011(2) 0.017(2) 0.023(2) 0.0022(19) 0.0090(19) -0.0012(18) S3 0.0207(6) 0.0200(6) 0.0228(6) -0.0037(5) 0.0147(5) -0.0042(5) C13 0.016(2) 0.020(2) 0.023(2) -0.003(2) 0.014(2) -0.0032(19) C14 0.016(2) 0.025(3) 0.024(2) -0.004(2) 0.013(2) -0.005(2) C15 0.023(2) 0.020(3) 0.023(3) -0.003(2) 0.014(2) -0.0024(19) C16 0.016(2) 0.026(3) 0.027(3) -0.003(2) 0.016(2) -0.003(2) C17 0.018(2) 0.030(3) 0.019(2) -0.002(2) 0.010(2) -0.005(2) C18 0.013(2) 0.026(3) 0.023(3) -0.007(2) 0.013(2) -0.005(2) C19 0.028(2) 0.024(3) 0.018(2) -0.001(2) 0.012(2) 0.003(2) C20 0.023(2) 0.023(3) 0.025(2) -0.003(2) 0.017(2) -0.001(2) C21 0.029(2) 0.017(2) 0.022(2) -0.003(2) 0.016(2) -0.002(2) Si1 0.0251(7) 0.0367(9) 0.0267(7) -0.0009(6) 0.0105(6) 0.0086(6) Si2 0.0447(8) 0.0282(8) 0.0296(8) -0.0033(6) 0.0234(7) -0.0053(7) Si3 0.0300(7) 0.0351(8) 0.0411(8) -0.0111(7) 0.0270(7) -0.0061(6) Si4 0.0201(6) 0.0250(7) 0.0254(7) -0.0052(6) 0.0135(6) -0.0015(6) Si5 0.0607(10) 0.0297(8) 0.0360(8) 0.0000(7) 0.0360(8) -0.0061(7) Si6 0.0258(7) 0.0332(8) 0.0302(8) -0.0032(6) 0.0125(6) 0.0017(6) C22 0.024(3) 0.061(4) 0.049(3) -0.001(3) 0.020(3) 0.002(3) C23 0.039(3) 0.054(4) 0.035(3) -0.007(3) 0.014(3) 0.017(3) C24 0.028(3) 0.041(3) 0.035(3) -0.006(2) 0.009(2) 0.010(2) C25 0.131(6) 0.038(4) 0.099(5) -0.012(3) 0.096(5) -0.020(4) C26 0.041(3) 0.044(3) 0.031(3) 0.006(2) 0.023(3) 0.005(2) C27 0.033(3) 0.094(5) 0.028(3) 0.001(3) 0.018(3) -0.018(3) C28 0.067(4) 0.042(3) 0.067(4) -0.008(3) 0.057(3) -0.008(3) C29 0.047(3) 0.046(3) 0.058(3) -0.014(3) 0.040(3) 0.000(3) C30 0.044(3) 0.064(4) 0.067(4) -0.023(3) 0.040(3) -0.021(3) C31 0.029(3) 0.037(3) 0.038(3) -0.007(2) 0.022(2) -0.002(2) C32 0.026(3) 0.044(3) 0.029(3) -0.001(2) 0.013(2) 0.000(2) C33 0.024(2) 0.033(3) 0.038(3) -0.004(2) 0.017(2) -0.003(2) C34 0.067(4) 0.053(4) 0.060(4) -0.010(3) 0.055(3) -0.019(3) C35 0.088(4) 0.040(3) 0.054(4) 0.005(3) 0.051(3) -0.010(3) C36 0.093(5) 0.056(4) 0.039(3) -0.002(3) 0.045(3) -0.013(3) C37 0.039(3) 0.040(3) 0.063(4) 0.004(3) 0.016(3) 0.011(3) C38 0.033(3) 0.049(3) 0.032(3) -0.005(2) 0.015(2) -0.006(3) C39 0.029(3) 0.076(4) 0.041(3) -0.023(3) 0.021(3) -0.016(3) P1 0.0144(6) 0.0215(6) 0.0220(6) 0.0016(5) 0.0106(5) 0.0007(5) C40 0.029(3) 0.017(3) 0.032(3) 0.003(2) 0.021(2) 0.001(2) C41 0.031(3) 0.029(3) 0.036(3) -0.002(2) 0.022(2) 0.004(2) C42 0.054(4) 0.035(3) 0.059(4) 0.003(3) 0.044(3) 0.014(3) C43 0.080(4) 0.033(3) 0.042(3) 0.004(3) 0.044(3) 0.017(3) C44 0.068(4) 0.034(3) 0.029(3) 0.000(2) 0.024(3) 0.015(3) C45 0.031(3) 0.038(3) 0.029(3) -0.002(2) 0.015(2) 0.008(2) C46 0.011(2) 0.025(3) 0.028(3) 0.004(2) 0.011(2) 0.0027(19) C47 0.016(2) 0.027(3) 0.030(3) 0.002(2) 0.013(2) 0.002(2) C48 0.023(3) 0.028(3) 0.052(3) 0.005(3) 0.023(3) -0.001(2) C49 0.018(2) 0.045(3) 0.046(3) 0.024(3) 0.019(2) 0.006(2) C50 0.022(3) 0.044(3) 0.029(3) 0.011(2) 0.015(2) 0.006(2) C51 0.016(2) 0.027(3) 0.031(3) 0.004(2) 0.014(2) -0.001(2) C52 0.019(2) 0.025(3) 0.020(2) 0.004(2) 0.013(2) 0.003(2) C53 0.024(2) 0.028(3) 0.018(2) 0.005(2) 0.013(2) 0.005(2) C54 0.023(2) 0.029(3) 0.023(3) 0.002(2) 0.013(2) -0.006(2) C55 0.017(2) 0.042(3) 0.022(3) 0.009(2) 0.009(2) -0.004(2) C56 0.018(2) 0.043(3) 0.038(3) 0.019(2) 0.013(2) 0.003(2) C57 0.022(2) 0.029(3) 0.034(3) 0.010(2) 0.017(2) 0.000(2) C58 0.128(7) 0.092(6) 0.096(6) 0.037(5) 0.098(6) 0.057(6) C59 0.140(8) 0.046(5) 0.080(6) -0.010(4) 0.055(6) -0.005(5) C60 0.154(8) 0.072(6) 0.049(5) -0.018(5) 0.004(5) -0.039(6) C61 0.137(8) 0.076(6) 0.044(5) 0.010(4) 0.029(5) -0.004(5) C62 0.086(6) 0.121(7) 0.073(5) 0.025(5) 0.050(5) 0.012(5) C63 0.085(6) 0.174(9) 0.069(5) 0.053(6) 0.058(5) 0.046(6) C64 0.044(7) 0.117(12) 0.066(9) -0.042(8) 0.023(7) 0.005(7) C65 0.127(13) 0.27(2) 0.149(14) -0.151(15) 0.117(12) -0.141(15) C66 0.039(7) 0.139(13) 0.094(9) -0.068(9) 0.024(7) 0.008(7) C67 0.094(10) 0.091(10) 0.076(8) 0.009(8) 0.048(8) 0.042(8) C68 0.213(7) 0.254(8) 0.137(6) 0.010(7) 0.122(6) 0.024(7) C69 0.103(11) 0.074(9) 0.114(11) -0.041(8) 0.052(9) -0.085(9) C70 0.226(7) 0.257(8) 0.147(7) 0.023(7) 0.105(6) 0.017(7) Cl1 0.210(6) 0.252(7) 0.151(5) 0.026(5) 0.119(5) 0.000(5) Cl2 0.201(6) 0.274(8) 0.150(5) 0.044(5) 0.120(5) 0.028(5) Cl3 0.257(7) 0.276(8) 0.173(6) 0.017(6) 0.081(6) 0.017(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 Pd1 C7 2.017(4) . ? Pd1 P1 2.2640(11) . ? Pd1 S2 2.3957(10) 2 ? Pd1 S1 2.4684(11) . ? Pd1 Pd2 3.1941(4) . ? Pd2 S2 2.2798(10) . ? Pd2 S2 2.2798(10) 2 ? Pd2 S1 2.2873(10) 2 ? Pd2 S1 2.2873(10) . ? Pd2 Pd1 3.1941(4) 2 ? S1 C1 1.789(4) . ? C1 C2 1.400(5) . ? C1 C6 1.400(5) . ? C2 C3 1.371(5) . ? C2 H1 0.9500 . ? C3 C4 1.384(5) . ? C3 H2 0.9500 . ? C4 C5 1.378(5) . ? C4 H3 0.9500 . ? C5 C6 1.399(5) . ? C5 H4 0.9500 . ? C6 S2 1.786(4) . ? S2 Pd1 2.3957(10) 2 ? C7 C8 1.393(5) . ? C7 C12 1.406(5) . ? C8 C9 1.387(5) . ? C8 H5 0.9500 . ? C9 C10 1.375(5) . ? C9 H6 0.9500 . ? C10 C11 1.390(5) . ? C10 H7 0.9500 . ? C11 C12 1.380(5) . ? C11 H8 0.9500 . ? C12 S3 1.780(4) . ? S3 C13 1.787(4) . ? C13 C14 1.408(5) . ? C13 C18 1.415(5) . ? C14 C15 1.386(5) . ? C14 C19 1.521(5) . ? C15 C16 1.381(5) . ? C15 H9 0.9500 . ? C16 C17 1.388(5) . ? C16 C20 1.528(5) . ? C17 C18 1.401(5) . ? C17 H10 0.9500 . ? C18 C21 1.511(5) . ? C19 Si2 1.886(4) . ? C19 Si1 1.895(4) . ? C19 H11 1.0000 . ? C20 Si3 1.887(4) . ? C20 Si4 1.890(4) . ? C20 H12 1.0000 . ? C21 Si5 1.894(4) . ? C21 Si6 1.903(4) . ? C21 H13 1.0000 . ? Si1 C22 1.854(5) . ? Si1 C24 1.871(4) . ? Si1 C23 1.880(5) . ? Si2 C26 1.861(4) . ? Si2 C27 1.866(5) . ? Si2 C25 1.881(5) . ? Si3 C28 1.858(5) . ? Si3 C30 1.862(5) . ? Si3 C29 1.868(4) . ? Si4 C33 1.862(4) . ? Si4 C31 1.864(4) . ? Si4 C32 1.869(4) . ? Si5 C34 1.855(5) . ? Si5 C35 1.874(5) . ? Si5 C36 1.879(5) . ? Si6 C39 1.848(5) . ? Si6 C38 1.863(4) . ? Si6 C37 1.874(5) . ? C22 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C23 H17 0.9800 . ? C23 H18 0.9800 . ? C23 H19 0.9800 . ? C24 H20 0.9800 . ? C24 H21 0.9800 . ? C24 H22 0.9800 . ? C25 H23 0.9800 . ? C25 H24 0.9800 . ? C25 H25 0.9800 . ? C26 H26 0.9800 . ? C26 H27 0.9800 . ? C26 H28 0.9800 . ? C27 H29 0.9800 . ? C27 H30 0.9800 . ? C27 H31 0.9800 . ? C28 H32 0.9800 . ? C28 H33 0.9800 . ? C28 H34 0.9800 . ? C29 H35 0.9800 . ? C29 H36 0.9800 . ? C29 H37 0.9800 . ? C30 H38 0.9800 . ? C30 H39 0.9800 . ? C30 H40 0.9800 . ? C31 H41 0.9800 . ? C31 H42 0.9800 . ? C31 H43 0.9800 . ? C32 H44 0.9800 . ? C32 H45 0.9800 . ? C32 H46 0.9800 . ? C33 H47 0.9800 . ? C33 H48 0.9800 . ? C33 H49 0.9800 . ? C34 H50 0.9800 . ? C34 H51 0.9800 . ? C34 H52 0.9800 . ? C35 H53 0.9800 . ? C35 H54 0.9800 . ? C35 H55 0.9800 . ? C36 H56 0.9800 . ? C36 H57 0.9800 . ? C36 H58 0.9800 . ? C37 H59 0.9800 . ? C37 H60 0.9800 . ? C37 H61 0.9800 . ? C38 H62 0.9800 . ? C38 H63 0.9800 . ? C38 H64 0.9800 . ? C39 H65 0.9800 . ? C39 H66 0.9800 . ? C39 H67 0.9800 . ? P1 C52 1.826(4) . ? P1 C46 1.826(4) . ? P1 C40 1.835(4) . ? C40 C45 1.386(5) . ? C40 C41 1.394(6) . ? C41 C42 1.377(6) . ? C41 H68 0.9500 . ? C42 C43 1.372(6) . ? C42 H69 0.9500 . ? C43 C44 1.378(7) . ? C43 H70 0.9500 . ? C44 C45 1.390(6) . ? C44 H71 0.9500 . ? C45 H72 0.9500 . ? C46 C47 1.382(5) . ? C46 C51 1.393(5) . ? C47 C48 1.394(6) . ? C47 H73 0.9500 . ? C48 C49 1.380(6) . ? C48 H74 0.9500 . ? C49 C50 1.383(6) . ? C49 H75 0.9500 . ? C50 C51 1.383(6) . ? C50 H76 0.9500 . ? C51 H77 0.9500 . ? C52 C53 1.386(5) . ? C52 C57 1.396(5) . ? C53 C54 1.389(5) . ? C53 H78 0.9500 . ? C54 C55 1.378(5) . ? C54 H79 0.9500 . ? C55 C56 1.378(6) . ? C55 H80 0.9500 . ? C56 C57 1.388(5) . ? C56 H81 0.9500 . ? C57 H82 0.9500 . ? C58 C59 1.341(9) . ? C58 C63 1.363(10) . ? C58 H83 0.9500 . ? C59 C60 1.342(9) . ? C59 H84 0.9500 . ? C60 C61 1.373(10) . ? C60 H85 0.9500 . ? C61 C62 1.347(8) . ? C61 H86 0.9500 . ? C62 C63 1.387(9) . ? C62 H87 0.9500 . ? C63 H88 0.9500 . ? C64 C65 1.3900 . ? C64 C69 1.3900 . ? C64 H89 0.9500 . ? C65 C66 1.3900 . ? C65 H90 0.9500 . ? C66 C67 1.3900 . ? C66 H91 0.9500 . ? C67 C68 1.3900 . ? C67 H92 0.9500 . ? C68 C69 1.3900 . ? C68 H93 0.9500 . ? C69 H94 0.9500 . ? C70 Cl3 1.602(9) . ? C70 Cl2 1.596(9) . ? C70 Cl1 1.604(9) . ? C70 H95 1.0000 . ? 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 C7 Pd1 P1 91.96(11) . . ? C7 Pd1 S2 87.11(11) . 2 ? P1 Pd1 S2 174.95(4) . 2 ? C7 Pd1 S1 163.44(12) . . ? P1 Pd1 S1 99.15(4) . . ? S2 Pd1 S1 82.86(4) 2 . ? C7 Pd1 Pd2 130.30(10) . . ? P1 Pd1 Pd2 133.86(3) . . ? S2 Pd1 Pd2 45.41(3) 2 . ? S1 Pd1 Pd2 45.44(2) . . ? S2 Pd2 S2 175.51(6) . 2 ? S2 Pd2 S1 89.63(4) . 2 ? S2 Pd2 S1 89.94(4) 2 2 ? S2 Pd2 S1 89.94(4) . . ? S2 Pd2 S1 89.63(4) 2 . ? S1 Pd2 S1 169.04(6) 2 . ? S2 Pd2 Pd1 48.45(3) . 2 ? S2 Pd2 Pd1 128.73(3) 2 2 ? S1 Pd2 Pd1 50.26(3) 2 2 ? S1 Pd2 Pd1 123.20(3) . 2 ? S2 Pd2 Pd1 128.73(3) . . ? S2 Pd2 Pd1 48.45(3) 2 . ? S1 Pd2 Pd1 123.20(3) 2 . ? S1 Pd2 Pd1 50.26(3) . . ? Pd1 Pd2 Pd1 122.585(18) 2 . ? C1 S1 Pd2 100.41(13) . . ? C1 S1 Pd1 122.37(13) . . ? Pd2 S1 Pd1 84.29(3) . . ? C2 C1 C6 119.2(4) . . ? C2 C1 S1 119.7(3) . . ? C6 C1 S1 121.0(3) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H1 119.7 . . ? C1 C2 H1 119.7 . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H2 119.9 . . ? C4 C3 H2 119.9 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 H3 119.8 . . ? C3 C4 H3 119.8 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H4 119.9 . . ? C6 C5 H4 119.9 . . ? C5 C6 C1 119.3(4) . . ? C5 C6 S2 119.9(3) . . ? C1 C6 S2 120.5(3) . . ? C6 S2 Pd2 100.82(14) . . ? C6 S2 Pd1 114.62(13) . 2 ? Pd2 S2 Pd1 86.15(4) . 2 ? C8 C7 C12 118.4(4) . . ? C8 C7 Pd1 125.4(3) . . ? C12 C7 Pd1 116.0(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H5 119.8 . . ? C7 C8 H5 119.8 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H6 119.8 . . ? C8 C9 H6 119.8 . . ? C9 C10 C11 119.9(4) . . ? C9 C10 H7 120.0 . . ? C11 C10 H7 120.0 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H8 120.0 . . ? C10 C11 H8 120.0 . . ? C11 C12 C7 120.6(4) . . ? C11 C12 S3 123.9(3) . . ? C7 C12 S3 115.3(3) . . ? C12 S3 C13 108.36(19) . . ? C14 C13 C18 120.0(4) . . ? C14 C13 S3 118.4(3) . . ? C18 C13 S3 120.7(3) . . ? C15 C14 C13 118.5(4) . . ? C15 C14 C19 117.3(4) . . ? C13 C14 C19 124.1(4) . . ? C16 C15 C14 123.3(4) . . ? C16 C15 H9 118.3 . . ? C14 C15 H9 118.3 . . ? C15 C16 C17 117.2(4) . . ? C15 C16 C20 119.7(4) . . ? C17 C16 C20 123.0(4) . . ? C16 C17 C18 122.8(4) . . ? C16 C17 H10 118.6 . . ? C18 C17 H10 118.6 . . ? C17 C18 C13 118.1(4) . . ? C17 C18 C21 118.8(3) . . ? C13 C18 C21 123.1(4) . . ? C14 C19 Si2 110.5(3) . . ? C14 C19 Si1 111.7(3) . . ? Si2 C19 Si1 120.8(2) . . ? C14 C19 H11 104.0 . . ? Si2 C19 H11 104.0 . . ? Si1 C19 H11 104.0 . . ? C16 C20 Si3 112.1(3) . . ? C16 C20 Si4 112.2(3) . . ? Si3 C20 Si4 120.4(2) . . ? C16 C20 H12 103.2 . . ? Si3 C20 H12 103.2 . . ? Si4 C20 H12 103.2 . . ? C18 C21 Si5 114.7(3) . . ? C18 C21 Si6 112.3(3) . . ? Si5 C21 Si6 115.4(2) . . ? C18 C21 H13 104.3 . . ? Si5 C21 H13 104.3 . . ? Si6 C21 H13 104.3 . . ? C22 Si1 C24 110.0(2) . . ? C22 Si1 C23 107.1(2) . . ? C24 Si1 C23 107.2(2) . . ? C22 Si1 C19 107.2(2) . . ? C24 Si1 C19 110.2(2) . . ? C23 Si1 C19 115.1(2) . . ? C26 Si2 C27 108.7(2) . . ? C26 Si2 C25 107.3(2) . . ? C27 Si2 C25 108.6(3) . . ? C26 Si2 C19 110.8(2) . . ? C27 Si2 C19 108.6(2) . . ? C25 Si2 C19 112.8(2) . . ? C28 Si3 C30 108.6(2) . . ? C28 Si3 C29 108.0(2) . . ? C30 Si3 C29 109.2(2) . . ? C28 Si3 C20 113.5(2) . . ? C30 Si3 C20 107.8(2) . . ? C29 Si3 C20 109.7(2) . . ? C33 Si4 C31 107.0(2) . . ? C33 Si4 C32 110.2(2) . . ? C31 Si4 C32 109.9(2) . . ? C33 Si4 C20 107.99(19) . . ? C31 Si4 C20 108.78(19) . . ? C32 Si4 C20 112.7(2) . . ? C34 Si5 C35 106.5(2) . . ? C34 Si5 C36 107.2(2) . . ? C35 Si5 C36 108.4(2) . . ? C34 Si5 C21 111.5(2) . . ? C35 Si5 C21 108.2(2) . . ? C36 Si5 C21 114.7(2) . . ? C39 Si6 C38 108.5(2) . . ? C39 Si6 C37 108.1(3) . . ? C38 Si6 C37 107.7(2) . . ? C39 Si6 C21 109.83(19) . . ? C38 Si6 C21 113.1(2) . . ? C37 Si6 C21 109.5(2) . . ? Si1 C22 H14 109.5 . . ? Si1 C22 H15 109.5 . . ? H14 C22 H15 109.5 . . ? Si1 C22 H16 109.5 . . ? H14 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? Si1 C23 H17 109.5 . . ? Si1 C23 H18 109.5 . . ? H17 C23 H18 109.5 . . ? Si1 C23 H19 109.5 . . ? H17 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? Si1 C24 H20 109.5 . . ? Si1 C24 H21 109.5 . . ? H20 C24 H21 109.5 . . ? Si1 C24 H22 109.5 . . ? H20 C24 H22 109.5 . . ? H21 C24 H22 109.5 . . ? Si2 C25 H23 109.5 . . ? Si2 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? Si2 C25 H25 109.5 . . ? H23 C25 H25 109.5 . . ? H24 C25 H25 109.5 . . ? Si2 C26 H26 109.5 . . ? Si2 C26 H27 109.5 . . ? H26 C26 H27 109.5 . . ? Si2 C26 H28 109.5 . . ? H26 C26 H28 109.5 . . ? H27 C26 H28 109.5 . . ? Si2 C27 H29 109.5 . . ? Si2 C27 H30 109.5 . . ? H29 C27 H30 109.5 . . ? Si2 C27 H31 109.5 . . ? H29 C27 H31 109.5 . . ? H30 C27 H31 109.5 . . ? Si3 C28 H32 109.5 . . ? Si3 C28 H33 109.5 . . ? H32 C28 H33 109.5 . . ? Si3 C28 H34 109.5 . . ? H32 C28 H34 109.5 . . ? H33 C28 H34 109.5 . . ? Si3 C29 H35 109.5 . . ? Si3 C29 H36 109.5 . . ? H35 C29 H36 109.5 . . ? Si3 C29 H37 109.5 . . ? H35 C29 H37 109.5 . . ? H36 C29 H37 109.5 . . ? Si3 C30 H38 109.5 . . ? Si3 C30 H39 109.5 . . ? H38 C30 H39 109.5 . . ? Si3 C30 H40 109.5 . . ? H38 C30 H40 109.5 . . ? H39 C30 H40 109.5 . . ? Si4 C31 H41 109.5 . . ? Si4 C31 H42 109.5 . . ? H41 C31 H42 109.5 . . ? Si4 C31 H43 109.5 . . ? H41 C31 H43 109.5 . . ? H42 C31 H43 109.5 . . ? Si4 C32 H44 109.5 . . ? Si4 C32 H45 109.5 . . ? H44 C32 H45 109.5 . . ? Si4 C32 H46 109.5 . . ? H44 C32 H46 109.5 . . ? H45 C32 H46 109.5 . . ? Si4 C33 H47 109.5 . . ? Si4 C33 H48 109.5 . . ? H47 C33 H48 109.5 . . ? Si4 C33 H49 109.5 . . ? H47 C33 H49 109.5 . . ? H48 C33 H49 109.5 . . ? Si5 C34 H50 109.5 . . ? Si5 C34 H51 109.5 . . ? H50 C34 H51 109.5 . . ? Si5 C34 H52 109.5 . . ? H50 C34 H52 109.5 . . ? H51 C34 H52 109.5 . . ? Si5 C35 H53 109.5 . . ? Si5 C35 H54 109.5 . . ? H53 C35 H54 109.5 . . ? Si5 C35 H55 109.5 . . ? H53 C35 H55 109.5 . . ? H54 C35 H55 109.5 . . ? Si5 C36 H56 109.5 . . ? Si5 C36 H57 109.5 . . ? H56 C36 H57 109.5 . . ? Si5 C36 H58 109.5 . . ? H56 C36 H58 109.5 . . ? H57 C36 H58 109.5 . . ? Si6 C37 H59 109.5 . . ? Si6 C37 H60 109.5 . . ? H59 C37 H60 109.5 . . ? Si6 C37 H61 109.5 . . ? H59 C37 H61 109.5 . . ? H60 C37 H61 109.5 . . ? Si6 C38 H62 109.5 . . ? Si6 C38 H63 109.5 . . ? H62 C38 H63 109.5 . . ? Si6 C38 H64 109.5 . . ? H62 C38 H64 109.5 . . ? H63 C38 H64 109.5 . . ? Si6 C39 H65 109.5 . . ? Si6 C39 H66 109.5 . . ? H65 C39 H66 109.5 . . ? Si6 C39 H67 109.5 . . ? H65 C39 H67 109.5 . . ? H66 C39 H67 109.5 . . ? C52 P1 C46 102.58(18) . . ? C52 P1 C40 106.83(19) . . ? C46 P1 C40 105.8(2) . . ? C52 P1 Pd1 117.46(14) . . ? C46 P1 Pd1 115.70(13) . . ? C40 P1 Pd1 107.62(14) . . ? C45 C40 C41 119.2(4) . . ? C45 C40 P1 117.5(3) . . ? C41 C40 P1 123.2(3) . . ? C42 C41 C40 119.4(4) . . ? C42 C41 H68 120.3 . . ? C40 C41 H68 120.3 . . ? C43 C42 C41 121.6(5) . . ? C43 C42 H69 119.2 . . ? C41 C42 H69 119.2 . . ? C42 C43 C44 119.4(5) . . ? C42 C43 H70 120.3 . . ? C44 C43 H70 120.3 . . ? C43 C44 C45 120.0(5) . . ? C43 C44 H71 120.0 . . ? C45 C44 H71 120.0 . . ? C40 C45 C44 120.4(4) . . ? C40 C45 H72 119.8 . . ? C44 C45 H72 119.8 . . ? C47 C46 C51 119.6(4) . . ? C47 C46 P1 122.3(3) . . ? C51 C46 P1 117.8(3) . . ? C46 C47 C48 119.9(4) . . ? C46 C47 H73 120.0 . . ? C48 C47 H73 120.0 . . ? C49 C48 C47 119.9(4) . . ? C49 C48 H74 120.1 . . ? C47 C48 H74 120.1 . . ? C48 C49 C50 120.6(4) . . ? C48 C49 H75 119.7 . . ? C50 C49 H75 119.7 . . ? C49 C50 C51 119.5(5) . . ? C49 C50 H76 120.2 . . ? C51 C50 H76 120.2 . . ? C50 C51 C46 120.5(4) . . ? C50 C51 H77 119.8 . . ? C46 C51 H77 119.8 . . ? C53 C52 C57 119.0(4) . . ? C53 C52 P1 120.4(3) . . ? C57 C52 P1 120.6(3) . . ? C52 C53 C54 120.7(4) . . ? C52 C53 H78 119.6 . . ? C54 C53 H78 119.6 . . ? C55 C54 C53 120.0(4) . . ? C55 C54 H79 120.0 . . ? C53 C54 H79 120.0 . . ? C54 C55 C56 119.8(4) . . ? C54 C55 H80 120.1 . . ? C56 C55 H80 120.1 . . ? C55 C56 C57 120.7(4) . . ? C55 C56 H81 119.6 . . ? C57 C56 H81 119.6 . . ? C56 C57 C52 119.8(4) . . ? C56 C57 H82 120.1 . . ? C52 C57 H82 120.1 . . ? C59 C58 C63 119.4(7) . . ? C59 C58 H83 120.3 . . ? C63 C58 H83 120.3 . . ? C58 C59 C60 121.1(8) . . ? C58 C59 H84 119.5 . . ? C60 C59 H84 119.5 . . ? C59 C60 C61 119.8(8) . . ? C59 C60 H85 120.1 . . ? C61 C60 H85 120.1 . . ? C62 C61 C60 121.0(7) . . ? C62 C61 H86 119.5 . . ? C60 C61 H86 119.5 . . ? C61 C62 C63 117.8(8) . . ? C61 C62 H87 121.1 . . ? C63 C62 H87 121.1 . . ? C58 C63 C62 120.9(7) . . ? C58 C63 H88 119.5 . . ? C62 C63 H88 119.5 . . ? C65 C64 C69 120.0 . . ? C65 C64 H89 120.0 . . ? C69 C64 H89 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H90 120.0 . . ? C66 C65 H90 120.0 . . ? C65 C66 C67 120.0 . . ? C65 C66 H91 120.0 . . ? C67 C66 H91 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H92 120.0 . . ? C66 C67 H92 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H93 120.0 . . ? C69 C68 H93 120.0 . . ? C68 C69 C64 120.0 . . ? C68 C69 H94 120.0 . . ? C64 C69 H94 120.0 . . ? Cl3 C70 Cl2 121.1(11) . . ? Cl3 C70 Cl1 114.0(10) . . ? Cl2 C70 Cl1 123.0(11) . . ? Cl3 C70 H95 94.6 . . ? Cl2 C70 H95 94.6 . . ? Cl1 C70 H95 94.6 . . ? 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 C7 Pd1 Pd2 S2 -153.70(16) . . . . ? P1 Pd1 Pd2 S2 -2.40(6) . . . . ? S2 Pd1 Pd2 S2 -175.42(6) 2 . . . ? S1 Pd1 Pd2 S2 48.05(5) . . . . ? C7 Pd1 Pd2 S2 21.72(16) . . . 2 ? P1 Pd1 Pd2 S2 173.03(5) . . . 2 ? S1 Pd1 Pd2 S2 -136.52(5) . . . 2 ? C7 Pd1 Pd2 S1 -32.71(16) . . . 2 ? P1 Pd1 Pd2 S1 118.59(5) . . . 2 ? S2 Pd1 Pd2 S1 -54.43(5) 2 . . 2 ? S1 Pd1 Pd2 S1 169.04(5) . . . 2 ? C7 Pd1 Pd2 S1 158.25(16) . . . . ? P1 Pd1 Pd2 S1 -50.45(5) . . . . ? S2 Pd1 Pd2 S1 136.52(5) 2 . . . ? C7 Pd1 Pd2 Pd1 -93.47(15) . . . 2 ? P1 Pd1 Pd2 Pd1 57.83(4) . . . 2 ? S2 Pd1 Pd2 Pd1 -115.19(3) 2 . . 2 ? S1 Pd1 Pd2 Pd1 108.28(3) . . . 2 ? S2 Pd2 S1 C1 -22.62(13) . . . . ? S2 Pd2 S1 C1 152.91(13) 2 . . . ? S1 Pd2 S1 C1 65.13(13) 2 . . . ? Pd1 Pd2 S1 C1 14.88(14) 2 . . . ? Pd1 Pd2 S1 C1 121.92(14) . . . . ? S2 Pd2 S1 Pd1 -144.53(4) . . . . ? S2 Pd2 S1 Pd1 30.99(4) 2 . . . ? S1 Pd2 S1 Pd1 -56.79(2) 2 . . . ? Pd1 Pd2 S1 Pd1 -107.04(3) 2 . . . ? C7 Pd1 S1 C1 178.6(4) . . . . ? P1 Pd1 S1 C1 47.01(15) . . . . ? S2 Pd1 S1 C1 -128.31(15) 2 . . . ? Pd2 Pd1 S1 C1 -98.72(15) . . . . ? C7 Pd1 S1 Pd2 -82.7(4) . . . . ? P1 Pd1 S1 Pd2 145.73(4) . . . . ? S2 Pd1 S1 Pd2 -29.59(3) 2 . . . ? Pd2 S1 C1 C2 -165.3(3) . . . . ? Pd1 S1 C1 C2 -75.5(3) . . . . ? Pd2 S1 C1 C6 18.4(3) . . . . ? Pd1 S1 C1 C6 108.2(3) . . . . ? C6 C1 C2 C3 -0.3(6) . . . . ? S1 C1 C2 C3 -176.6(3) . . . . ? C1 C2 C3 C4 1.6(6) . . . . ? C2 C3 C4 C5 -0.9(6) . . . . ? C3 C4 C5 C6 -1.2(6) . . . . ? C4 C5 C6 C1 2.5(6) . . . . ? C4 C5 C6 S2 177.0(3) . . . . ? C2 C1 C6 C5 -1.7(6) . . . . ? S1 C1 C6 C5 174.6(3) . . . . ? C2 C1 C6 S2 -176.2(3) . . . . ? S1 C1 C6 S2 0.1(5) . . . . ? C5 C6 S2 Pd2 166.9(3) . . . . ? C1 C6 S2 Pd2 -18.6(3) . . . . ? C5 C6 S2 Pd1 76.2(3) . . . 2 ? C1 C6 S2 Pd1 -109.3(3) . . . 2 ? S1 Pd2 S2 C6 -146.30(13) 2 . . . ? S1 Pd2 S2 C6 22.75(13) . . . . ? Pd1 Pd2 S2 C6 -114.35(13) 2 . . . ? Pd1 Pd2 S2 C6 -12.13(14) . . . . ? S1 Pd2 S2 Pd1 -31.95(4) 2 . . 2 ? S1 Pd2 S2 Pd1 137.10(4) . . . 2 ? Pd1 Pd2 S2 Pd1 102.22(3) . . . 2 ? P1 Pd1 C7 C8 -75.9(3) . . . . ? S2 Pd1 C7 C8 99.1(3) 2 . . . ? S1 Pd1 C7 C8 151.7(3) . . . . ? Pd2 Pd1 C7 C8 83.8(4) . . . . ? P1 Pd1 C7 C12 109.7(3) . . . . ? S2 Pd1 C7 C12 -75.3(3) 2 . . . ? S1 Pd1 C7 C12 -22.6(6) . . . . ? Pd2 Pd1 C7 C12 -90.6(3) . . . . ? C12 C7 C8 C9 2.3(6) . . . . ? Pd1 C7 C8 C9 -172.0(3) . . . . ? C7 C8 C9 C10 1.4(6) . . . . ? C8 C9 C10 C11 -3.0(6) . . . . ? C9 C10 C11 C12 0.8(6) . . . . ? C10 C11 C12 C7 2.9(6) . . . . ? C10 C11 C12 S3 -171.3(3) . . . . ? C8 C7 C12 C11 -4.4(6) . . . . ? Pd1 C7 C12 C11 170.3(3) . . . . ? C8 C7 C12 S3 170.2(3) . . . . ? Pd1 C7 C12 S3 -15.0(4) . . . . ? C11 C12 S3 C13 -19.7(4) . . . . ? C7 C12 S3 C13 165.8(3) . . . . ? C12 S3 C13 C14 -105.6(3) . . . . ? C12 S3 C13 C18 85.3(3) . . . . ? C18 C13 C14 C15 1.1(6) . . . . ? S3 C13 C14 C15 -168.0(3) . . . . ? C18 C13 C14 C19 178.5(4) . . . . ? S3 C13 C14 C19 9.4(5) . . . . ? C13 C14 C15 C16 -0.1(6) . . . . ? C19 C14 C15 C16 -177.6(4) . . . . ? C14 C15 C16 C17 -0.9(6) . . . . ? C14 C15 C16 C20 177.5(4) . . . . ? C15 C16 C17 C18 1.0(6) . . . . ? C20 C16 C17 C18 -177.4(4) . . . . ? C16 C17 C18 C13 0.0(6) . . . . ? C16 C17 C18 C21 -178.9(4) . . . . ? C14 C13 C18 C17 -1.0(6) . . . . ? S3 C13 C18 C17 167.8(3) . . . . ? C14 C13 C18 C21 177.8(4) . . . . ? S3 C13 C18 C21 -13.4(5) . . . . ? C15 C14 C19 Si2 71.3(4) . . . . ? C13 C14 C19 Si2 -106.1(4) . . . . ? C15 C14 C19 Si1 -66.2(4) . . . . ? C13 C14 C19 Si1 116.4(4) . . . . ? C15 C16 C20 Si3 109.7(4) . . . . ? C17 C16 C20 Si3 -71.9(4) . . . . ? C15 C16 C20 Si4 -111.1(4) . . . . ? C17 C16 C20 Si4 67.3(5) . . . . ? C17 C18 C21 Si5 54.2(4) . . . . ? C13 C18 C21 Si5 -124.6(4) . . . . ? C17 C18 C21 Si6 -80.1(4) . . . . ? C13 C18 C21 Si6 101.1(4) . . . . ? C14 C19 Si1 C22 -52.7(3) . . . . ? Si2 C19 Si1 C22 174.8(2) . . . . ? C14 C19 Si1 C24 -172.4(3) . . . . ? Si2 C19 Si1 C24 55.1(3) . . . . ? C14 C19 Si1 C23 66.3(4) . . . . ? Si2 C19 Si1 C23 -66.2(3) . . . . ? C14 C19 Si2 C26 157.8(3) . . . . ? Si1 C19 Si2 C26 -69.2(3) . . . . ? C14 C19 Si2 C27 38.5(4) . . . . ? Si1 C19 Si2 C27 171.5(3) . . . . ? C14 C19 Si2 C25 -82.0(4) . . . . ? Si1 C19 Si2 C25 51.1(3) . . . . ? C16 C20 Si3 C28 66.2(3) . . . . ? Si4 C20 Si3 C28 -69.1(3) . . . . ? C16 C20 Si3 C30 -54.1(3) . . . . ? Si4 C20 Si3 C30 170.5(3) . . . . ? C16 C20 Si3 C29 -172.9(3) . . . . ? Si4 C20 Si3 C29 51.8(3) . . . . ? C16 C20 Si4 C33 142.4(3) . . . . ? Si3 C20 Si4 C33 -82.2(3) . . . . ? C16 C20 Si4 C31 26.6(4) . . . . ? Si3 C20 Si4 C31 162.0(2) . . . . ? C16 C20 Si4 C32 -95.5(3) . . . . ? Si3 C20 Si4 C32 39.8(3) . . . . ? C18 C21 Si5 C34 30.0(4) . . . . ? Si6 C21 Si5 C34 162.8(2) . . . . ? C18 C21 Si5 C35 146.7(3) . . . . ? Si6 C21 Si5 C35 -80.4(3) . . . . ? C18 C21 Si5 C36 -92.1(3) . . . . ? Si6 C21 Si5 C36 40.7(3) . . . . ? C18 C21 Si6 C39 -55.5(3) . . . . ? Si5 C21 Si6 C39 170.6(2) . . . . ? C18 C21 Si6 C38 65.9(3) . . . . ? Si5 C21 Si6 C38 -68.0(3) . . . . ? C18 C21 Si6 C37 -174.0(3) . . . . ? Si5 C21 Si6 C37 52.1(3) . . . . ? C7 Pd1 P1 C52 -110.76(19) . . . . ? S1 Pd1 P1 C52 56.92(15) . . . . ? Pd2 Pd1 P1 C52 90.74(15) . . . . ? C7 Pd1 P1 C46 10.74(19) . . . . ? S1 Pd1 P1 C46 178.42(16) . . . . ? Pd2 Pd1 P1 C46 -147.76(15) . . . . ? C7 Pd1 P1 C40 128.75(18) . . . . ? S1 Pd1 P1 C40 -63.57(15) . . . . ? Pd2 Pd1 P1 C40 -29.75(15) . . . . ? C52 P1 C40 C45 -146.5(3) . . . . ? C46 P1 C40 C45 104.7(4) . . . . ? Pd1 P1 C40 C45 -19.5(4) . . . . ? C52 P1 C40 C41 30.2(4) . . . . ? C46 P1 C40 C41 -78.6(4) . . . . ? Pd1 P1 C40 C41 157.2(3) . . . . ? C45 C40 C41 C42 0.4(7) . . . . ? P1 C40 C41 C42 -176.3(4) . . . . ? C40 C41 C42 C43 -0.7(7) . . . . ? C41 C42 C43 C44 0.5(8) . . . . ? C42 C43 C44 C45 0.0(8) . . . . ? C41 C40 C45 C44 0.1(7) . . . . ? P1 C40 C45 C44 177.0(4) . . . . ? C43 C44 C45 C40 -0.3(8) . . . . ? C52 P1 C46 C47 -131.3(3) . . . . ? C40 P1 C46 C47 -19.5(4) . . . . ? Pd1 P1 C46 C47 99.5(3) . . . . ? C52 P1 C46 C51 55.2(3) . . . . ? C40 P1 C46 C51 167.0(3) . . . . ? Pd1 P1 C46 C51 -74.0(3) . . . . ? C51 C46 C47 C48 0.5(6) . . . . ? P1 C46 C47 C48 -172.9(3) . . . . ? C46 C47 C48 C49 0.4(6) . . . . ? C47 C48 C49 C50 -1.3(6) . . . . ? C48 C49 C50 C51 1.2(6) . . . . ? C49 C50 C51 C46 -0.2(6) . . . . ? C47 C46 C51 C50 -0.6(6) . . . . ? P1 C46 C51 C50 173.1(3) . . . . ? C46 P1 C52 C53 -137.1(3) . . . . ? C40 P1 C52 C53 111.9(4) . . . . ? Pd1 P1 C52 C53 -9.0(4) . . . . ? C46 P1 C52 C57 41.4(4) . . . . ? C40 P1 C52 C57 -69.6(4) . . . . ? Pd1 P1 C52 C57 169.5(3) . . . . ? C57 C52 C53 C54 1.4(6) . . . . ? P1 C52 C53 C54 179.9(3) . . . . ? C52 C53 C54 C55 0.1(6) . . . . ? C53 C54 C55 C56 -0.6(7) . . . . ? C54 C55 C56 C57 -0.3(7) . . . . ? C55 C56 C57 C52 1.8(7) . . . . ? C53 C52 C57 C56 -2.3(6) . . . . ? P1 C52 C57 C56 179.2(3) . . . . ? C63 C58 C59 C60 -0.9(12) . . . . ? C58 C59 C60 C61 -0.3(14) . . . . ? C59 C60 C61 C62 2.0(14) . . . . ? C60 C61 C62 C63 -2.3(13) . . . . ? C59 C58 C63 C62 0.6(12) . . . . ? C61 C62 C63 C58 1.0(12) . . . . ? C69 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C64 0.0 . . . . ? C65 C64 C69 C68 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.400 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.091 # Attachment 'compound1.CIF' data_s6 _database_code_depnum_ccdc_archive 'CCDC 285412' _audit_creation_date 2005-09-06 _audit_update_record ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H134 S6 Si12, 0.5(C1 H2 Cl2), 0.5(C6 H14)' _chemical_formula_sum 'C81.50 H142 Cl S6 Si12' _chemical_formula_weight 1686.84 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.920(2) _cell_length_b 20.424(5) _cell_length_c 23.068(5) _cell_angle_alpha 71.290(7) _cell_angle_beta 83.335(10) _cell_angle_gamma 83.675(11) _cell_volume 4825.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 8892 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.00 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9004 _exptl_absorpt_correction_T_max 0.9964 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 31210 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0810 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16506 _reflns_number_gt 12446 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _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^)+(0.0636P)^2^+7.9460P] 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 16506 _refine_ls_number_parameters 941 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 S1 S 0.52324(9) 0.46657(5) 0.76004(5) 0.0167(2) Uani 1 1 d . . . C1 C 0.6180(4) 0.5317(2) 0.71127(17) 0.0161(8) Uani 1 1 d . . . C2 C 0.7470(4) 0.52358(19) 0.71703(17) 0.0146(8) Uani 1 1 d . . . C3 C 0.8227(4) 0.56514(19) 0.66991(18) 0.0153(8) Uani 1 1 d . . . H1 H 0.9094 0.5595 0.6732 0.018 Uiso 1 1 calc R . . C4 C 0.7773(4) 0.61473(19) 0.61814(18) 0.0145(8) Uani 1 1 d . . . C5 C 0.6495(3) 0.6240(2) 0.61546(18) 0.0151(8) Uani 1 1 d . . . H2 H 0.6168 0.6587 0.5813 0.018 Uiso 1 1 calc R . . C6 C 0.5670(4) 0.58414(19) 0.66111(17) 0.0144(8) Uani 1 1 d . . . C7 C 0.8055(4) 0.4722(2) 0.77230(18) 0.0169(8) Uani 1 1 d . . . H3 H 0.7336 0.4522 0.8011 0.020 Uiso 1 1 calc R . . C8 C 0.8656(4) 0.6563(2) 0.56804(18) 0.0163(8) Uani 1 1 d . . . H4 H 0.9488 0.6359 0.5818 0.020 Uiso 1 1 calc R . . C9 C 0.4304(4) 0.5998(2) 0.65555(18) 0.0167(8) Uani 1 1 d . . . H5 H 0.3915 0.5730 0.6966 0.020 Uiso 1 1 calc R . . Si1 Si 0.89174(10) 0.39530(6) 0.75200(5) 0.0184(3) Uani 1 1 d . . . Si2 Si 0.88520(11) 0.51762(6) 0.81591(5) 0.0203(3) Uani 1 1 d . . . Si3 Si 0.86286(10) 0.74936(6) 0.56788(5) 0.0175(2) Uani 1 1 d . . . Si4 Si 0.86317(10) 0.63704(6) 0.49255(5) 0.0179(2) Uani 1 1 d . . . Si5 Si 0.37778(10) 0.69402(6) 0.64755(5) 0.0172(2) Uani 1 1 d . . . Si6 Si 0.37410(10) 0.56100(6) 0.59938(5) 0.0165(2) Uani 1 1 d . . . C10 C 0.7806(4) 0.3583(2) 0.7175(2) 0.0307(11) Uani 1 1 d . . . H6 H 0.7508 0.3940 0.6810 0.046 Uiso 1 1 calc R . . H7 H 0.7105 0.3427 0.7476 0.046 Uiso 1 1 calc R . . H8 H 0.8224 0.3189 0.7056 0.046 Uiso 1 1 calc R . . C11 C 0.9419(4) 0.3273(2) 0.8229(2) 0.0312(11) Uani 1 1 d . . . H9 H 0.9667 0.2838 0.8139 0.047 Uiso 1 1 calc R . . H10 H 0.8732 0.3202 0.8551 0.047 Uiso 1 1 calc R . . H11 H 1.0121 0.3423 0.8370 0.047 Uiso 1 1 calc R . . C12 C 1.0311(4) 0.4175(2) 0.6959(2) 0.0280(10) Uani 1 1 d . . . H12 H 1.0887 0.4390 0.7126 0.042 Uiso 1 1 calc R . . H13 H 1.0055 0.4500 0.6570 0.042 Uiso 1 1 calc R . . H14 H 1.0719 0.3752 0.6889 0.042 Uiso 1 1 calc R . . C13 C 0.9100(5) 0.4576(2) 0.8948(2) 0.0317(11) Uani 1 1 d . . . H15 H 0.9766 0.4221 0.8923 0.048 Uiso 1 1 calc R . . H16 H 0.8337 0.4353 0.9133 0.048 Uiso 1 1 calc R . . H17 H 0.9327 0.4840 0.9202 0.048 Uiso 1 1 calc R . . C14 C 1.0379(4) 0.5496(2) 0.7780(2) 0.0297(11) Uani 1 1 d . . . H18 H 1.0755 0.5696 0.8044 0.045 Uiso 1 1 calc R . . H19 H 1.0254 0.5852 0.7384 0.045 Uiso 1 1 calc R . . H20 H 1.0927 0.5109 0.7713 0.045 Uiso 1 1 calc R . . C15 C 0.7825(5) 0.5941(2) 0.8245(2) 0.0360(12) Uani 1 1 d . . . H21 H 0.7085 0.5780 0.8516 0.054 Uiso 1 1 calc R . . H22 H 0.7581 0.6232 0.7841 0.054 Uiso 1 1 calc R . . H23 H 0.8271 0.6211 0.8423 0.054 Uiso 1 1 calc R . . C16 C 0.8601(4) 0.7481(2) 0.6498(2) 0.0237(10) Uani 1 1 d . . . H24 H 0.8722 0.7945 0.6507 0.036 Uiso 1 1 calc R . . H25 H 0.9266 0.7152 0.6697 0.036 Uiso 1 1 calc R . . H26 H 0.7802 0.7338 0.6716 0.036 Uiso 1 1 calc R . . C17 C 1.0092(4) 0.7866(2) 0.5256(2) 0.0281(10) Uani 1 1 d . . . H27 H 1.0147 0.8321 0.5304 0.042 Uiso 1 1 calc R . . H28 H 1.0091 0.7916 0.4819 0.042 Uiso 1 1 calc R . . H29 H 1.0804 0.7555 0.5423 0.042 Uiso 1 1 calc R . . C18 C 0.7290(4) 0.8072(2) 0.5317(2) 0.0236(10) Uani 1 1 d . . . H30 H 0.6516 0.7901 0.5548 0.035 Uiso 1 1 calc R . . H31 H 0.7292 0.8072 0.4891 0.035 Uiso 1 1 calc R . . H32 H 0.7359 0.8545 0.5321 0.035 Uiso 1 1 calc R . . C19 C 1.0197(4) 0.6509(2) 0.4491(2) 0.0253(10) Uani 1 1 d . . . H33 H 1.0209 0.6394 0.4110 0.038 Uiso 1 1 calc R . . H34 H 1.0829 0.6210 0.4744 0.038 Uiso 1 1 calc R . . H35 H 1.0369 0.6995 0.4394 0.038 Uiso 1 1 calc R . . C20 C 0.7443(4) 0.6910(2) 0.4413(2) 0.0267(10) Uani 1 1 d . . . H36 H 0.7669 0.7391 0.4251 0.040 Uiso 1 1 calc R . . H37 H 0.6634 0.6895 0.4648 0.040 Uiso 1 1 calc R . . H38 H 0.7403 0.6728 0.4072 0.040 Uiso 1 1 calc R . . C21 C 0.8354(4) 0.5427(2) 0.5125(2) 0.0280(10) Uani 1 1 d . . . H39 H 0.8373 0.5304 0.4747 0.042 Uiso 1 1 calc R . . H40 H 0.7543 0.5344 0.5355 0.042 Uiso 1 1 calc R . . H41 H 0.8999 0.5143 0.5377 0.042 Uiso 1 1 calc R . . C22 C 0.4826(4) 0.7319(2) 0.6848(2) 0.0238(10) Uani 1 1 d . . . H42 H 0.4547 0.7805 0.6795 0.036 Uiso 1 1 calc R . . H43 H 0.5672 0.7289 0.6657 0.036 Uiso 1 1 calc R . . H44 H 0.4810 0.7060 0.7287 0.036 Uiso 1 1 calc R . . C23 C 0.3726(4) 0.7511(2) 0.5661(2) 0.0261(10) Uani 1 1 d . . . H45 H 0.3497 0.7991 0.5653 0.039 Uiso 1 1 calc R . . H46 H 0.3112 0.7359 0.5464 0.039 Uiso 1 1 calc R . . H47 H 0.4541 0.7483 0.5439 0.039 Uiso 1 1 calc R . . C24 C 0.2196(4) 0.6989(2) 0.6876(2) 0.0307(11) Uani 1 1 d . . . H48 H 0.2202 0.6692 0.7305 0.046 Uiso 1 1 calc R . . H49 H 0.1606 0.6830 0.6670 0.046 Uiso 1 1 calc R . . H50 H 0.1950 0.7469 0.6863 0.046 Uiso 1 1 calc R . . C25 C 0.4477(4) 0.5949(2) 0.51978(19) 0.0248(10) Uani 1 1 d . . . H51 H 0.5370 0.5825 0.5196 0.037 Uiso 1 1 calc R . . H52 H 0.4323 0.6454 0.5049 0.037 Uiso 1 1 calc R . . H53 H 0.4125 0.5745 0.4929 0.037 Uiso 1 1 calc R . . C26 C 0.2025(4) 0.5816(2) 0.5988(2) 0.0250(10) Uani 1 1 d . . . H54 H 0.1845 0.6317 0.5814 0.037 Uiso 1 1 calc R . . H55 H 0.1638 0.5658 0.6410 0.037 Uiso 1 1 calc R . . H56 H 0.1695 0.5579 0.5738 0.037 Uiso 1 1 calc R . . C27 C 0.4080(4) 0.4647(2) 0.6247(2) 0.0253(10) Uani 1 1 d . . . H57 H 0.3787 0.4455 0.5954 0.038 Uiso 1 1 calc R . . H58 H 0.3657 0.4445 0.6655 0.038 Uiso 1 1 calc R . . H59 H 0.4974 0.4535 0.6265 0.038 Uiso 1 1 calc R . . C28 C 0.4327(4) 0.5044(2) 0.81167(17) 0.0151(8) Uani 1 1 d . . . C29 C 0.4567(4) 0.5666(2) 0.81845(19) 0.0244(10) Uani 1 1 d . . . H60 H 0.5258 0.5900 0.7956 0.029 Uiso 1 1 calc R . . C30 C 0.3814(5) 0.5952(2) 0.8581(2) 0.0307(11) Uani 1 1 d . . . H61 H 0.3971 0.6390 0.8607 0.037 Uiso 1 1 calc R . . C31 C 0.2834(5) 0.5604(2) 0.8940(2) 0.0314(11) Uani 1 1 d . . . H62 H 0.2327 0.5797 0.9218 0.038 Uiso 1 1 calc R . . C32 C 0.2602(4) 0.4971(2) 0.8889(2) 0.0254(10) Uani 1 1 d . . . H63 H 0.1942 0.4725 0.9139 0.030 Uiso 1 1 calc R . . C33 C 0.3331(4) 0.4693(2) 0.84734(19) 0.0192(9) Uani 1 1 d . . . S2 S 0.28028(9) 0.39494(5) 0.83589(5) 0.0216(2) Uani 1 1 d . . . C34 C 0.4088(4) 0.3320(2) 0.85123(18) 0.0187(9) Uani 1 1 d . . . C35 C 0.4892(4) 0.3291(2) 0.89404(19) 0.0234(10) Uani 1 1 d . . . H64 H 0.4769 0.3618 0.9160 0.028 Uiso 1 1 calc R . . C36 C 0.5881(4) 0.2788(2) 0.90539(19) 0.0272(10) Uani 1 1 d . . . H65 H 0.6451 0.2780 0.9338 0.033 Uiso 1 1 calc R . . C37 C 0.6023(4) 0.2298(2) 0.87460(19) 0.0263(10) Uani 1 1 d . . . H66 H 0.6678 0.1943 0.8832 0.032 Uiso 1 1 calc R . . C38 C 0.5224(4) 0.2317(2) 0.83144(19) 0.0211(9) Uani 1 1 d . . . H67 H 0.5331 0.1978 0.8107 0.025 Uiso 1 1 calc R . . C39 C 0.4264(4) 0.2837(2) 0.81873(18) 0.0179(9) Uani 1 1 d . . . S3 S 0.32250(10) 0.29383(5) 0.76112(5) 0.0219(2) Uani 1 1 d . . . S4 S 0.35258(10) 0.20627(5) 0.73574(5) 0.0221(2) Uani 1 1 d . . . C40 C 0.4810(4) 0.2213(2) 0.67845(18) 0.0185(9) Uani 1 1 d . . . C41 C 0.5579(4) 0.2746(2) 0.66697(19) 0.0216(9) Uani 1 1 d . . . H68 H 0.5407 0.3077 0.6885 0.026 Uiso 1 1 calc R . . C42 C 0.6594(4) 0.2798(2) 0.62450(19) 0.0248(10) Uani 1 1 d . . . H69 H 0.7115 0.3165 0.6168 0.030 Uiso 1 1 calc R . . C43 C 0.6858(4) 0.2316(2) 0.59285(19) 0.0239(10) Uani 1 1 d . . . H70 H 0.7569 0.2346 0.5644 0.029 Uiso 1 1 calc R . . C44 C 0.6083(4) 0.1792(2) 0.60290(18) 0.0213(9) Uani 1 1 d . . . H71 H 0.6249 0.1471 0.5804 0.026 Uiso 1 1 calc R . . C45 C 0.5059(4) 0.1732(2) 0.64574(19) 0.0175(9) Uani 1 1 d . . . S5 S 0.40106(10) 0.10838(5) 0.65813(5) 0.0225(2) Uani 1 1 d . . . C46 C 0.4960(4) 0.0366(2) 0.64676(19) 0.0211(9) Uani 1 1 d . . . C47 C 0.4659(4) 0.0087(2) 0.6026(2) 0.0302(11) Uani 1 1 d . . . H72 H 0.4033 0.0322 0.5763 0.036 Uiso 1 1 calc R . . C48 C 0.5250(4) -0.0521(2) 0.5964(2) 0.0325(11) Uani 1 1 d . . . H73 H 0.5037 -0.0702 0.5661 0.039 Uiso 1 1 calc R . . C49 C 0.6157(5) -0.0868(2) 0.6348(2) 0.0334(11) Uani 1 1 d . . . H74 H 0.6553 -0.1294 0.6314 0.040 Uiso 1 1 calc R . . C50 C 0.6493(4) -0.0599(2) 0.6783(2) 0.0253(10) Uani 1 1 d . . . H75 H 0.7132 -0.0835 0.7037 0.030 Uiso 1 1 calc R . . C51 C 0.5903(4) 0.0014(2) 0.68501(19) 0.0195(9) Uani 1 1 d . . . S6 S 0.62805(10) 0.03804(5) 0.74018(5) 0.0192(2) Uani 1 1 d . . . C52 C 0.7264(4) -0.0274(2) 0.78833(18) 0.0180(9) Uani 1 1 d . . . C53 C 0.8551(4) -0.0198(2) 0.78261(19) 0.0219(9) Uani 1 1 d . . . C54 C 0.9251(4) -0.0637(2) 0.82829(19) 0.0211(9) Uani 1 1 d . . . H76 H 1.0112 -0.0584 0.8249 0.025 Uiso 1 1 calc R . . C55 C 0.8761(4) -0.1153(2) 0.87888(18) 0.0176(9) Uani 1 1 d . . . C56 C 0.7497(4) -0.1234(2) 0.88198(18) 0.0177(9) Uani 1 1 d . . . H77 H 0.7145 -0.1591 0.9152 0.021 Uiso 1 1 calc R . . C57 C 0.6732(4) -0.0806(2) 0.83768(18) 0.0153(8) Uani 1 1 d . . . C58 C 0.9192(4) 0.0336(2) 0.7290(2) 0.0241(10) Uani 1 1 d . . . H78 H 0.8537 0.0540 0.7000 0.029 Uiso 1 1 calc R . . C59 C 0.9571(4) -0.1592(2) 0.92812(18) 0.0172(9) Uani 1 1 d . . . H79 H 1.0394 -0.1399 0.9138 0.021 Uiso 1 1 calc R . . C60 C 0.5384(4) -0.0944(2) 0.84383(18) 0.0156(8) Uani 1 1 d . . . H80 H 0.5084 -0.0662 0.8032 0.019 Uiso 1 1 calc R . . Si7 Si 0.95892(11) 0.10902(6) 0.75287(6) 0.0289(3) Uani 1 1 d . . . Si8 Si 1.04303(13) -0.00742(7) 0.68381(6) 0.0342(3) Uani 1 1 d . . . Si9 Si 0.98859(11) -0.25237(6) 0.92772(6) 0.0216(3) Uani 1 1 d . . . Si10 Si 0.91652(11) -0.14049(6) 1.00404(5) 0.0203(3) Uani 1 1 d . . . Si11 Si 0.51470(10) -0.18751(6) 0.84975(5) 0.0187(3) Uani 1 1 d . . . Si12 Si 0.44227(10) -0.05636(6) 0.90097(5) 0.0184(3) Uani 1 1 d . . . C61 C 0.8142(4) 0.1433(3) 0.7885(3) 0.0423(14) Uani 1 1 d . . . H81 H 0.8321 0.1822 0.8015 0.064 Uiso 1 1 calc R . . H82 H 0.7822 0.1065 0.8242 0.064 Uiso 1 1 calc R . . H83 H 0.7522 0.1591 0.7584 0.064 Uiso 1 1 calc R . . C62 C 1.0153(5) 0.1802(3) 0.6840(3) 0.0525(16) Uani 1 1 d . . . H84 H 1.0159 0.2226 0.6951 0.079 Uiso 1 1 calc R . . H85 H 0.9602 0.1886 0.6513 0.079 Uiso 1 1 calc R . . H86 H 1.0992 0.1667 0.6695 0.079 Uiso 1 1 calc R . . C63 C 1.0783(5) 0.0860(2) 0.8093(2) 0.0374(12) Uani 1 1 d . . . H87 H 1.1555 0.0684 0.7914 0.056 Uiso 1 1 calc R . . H88 H 1.0492 0.0503 0.8467 0.056 Uiso 1 1 calc R . . H89 H 1.0928 0.1274 0.8196 0.056 Uiso 1 1 calc R . . C64 C 1.0762(6) 0.0553(3) 0.6062(3) 0.072(2) Uani 1 1 d . . . H90 H 1.1334 0.0325 0.5813 0.108 Uiso 1 1 calc R . . H91 H 1.1138 0.0949 0.6101 0.108 Uiso 1 1 calc R . . H92 H 0.9990 0.0714 0.5864 0.108 Uiso 1 1 calc R . . C65 C 1.1917(5) -0.0348(3) 0.7199(3) 0.0469(15) Uani 1 1 d . . . H93 H 1.2524 -0.0522 0.6925 0.070 Uiso 1 1 calc R . . H94 H 1.1785 -0.0716 0.7591 0.070 Uiso 1 1 calc R . . H95 H 1.2225 0.0050 0.7271 0.070 Uiso 1 1 calc R . . C66 C 0.9874(5) -0.0867(3) 0.6747(3) 0.0504(15) Uani 1 1 d . . . H96 H 0.9165 -0.0733 0.6498 0.076 Uiso 1 1 calc R . . H97 H 0.9624 -0.1184 0.7152 0.076 Uiso 1 1 calc R . . H98 H 1.0541 -0.1097 0.6543 0.076 Uiso 1 1 calc R . . C67 C 1.0298(4) -0.2518(2) 0.8466(2) 0.0310(11) Uani 1 1 d . . . H99 H 1.0549 -0.2992 0.8460 0.047 Uiso 1 1 calc R . . H100 H 1.0982 -0.2224 0.8284 0.047 Uiso 1 1 calc R . . H101 H 0.9579 -0.2336 0.8228 0.047 Uiso 1 1 calc R . . C68 C 0.8569(4) -0.3078(2) 0.9607(2) 0.0320(11) Uani 1 1 d . . . H102 H 0.7851 -0.2881 0.9372 0.048 Uiso 1 1 calc R . . H103 H 0.8359 -0.3098 1.0036 0.048 Uiso 1 1 calc R . . H104 H 0.8807 -0.3547 0.9585 0.048 Uiso 1 1 calc R . . C69 C 1.1248(5) -0.2914(2) 0.9735(2) 0.0339(11) Uani 1 1 d . . . H105 H 1.1473 -0.3385 0.9716 0.051 Uiso 1 1 calc R . . H106 H 1.1033 -0.2930 1.0163 0.051 Uiso 1 1 calc R . . H107 H 1.1950 -0.2630 0.9564 0.051 Uiso 1 1 calc R . . C70 C 0.8608(4) -0.0466(2) 0.9860(2) 0.0297(11) Uani 1 1 d . . . H108 H 0.7847 -0.0379 0.9651 0.045 Uiso 1 1 calc R . . H109 H 0.9243 -0.0180 0.9593 0.045 Uiso 1 1 calc R . . H110 H 0.8441 -0.0347 1.0242 0.045 Uiso 1 1 calc R . . C71 C 1.0588(4) -0.1548(2) 1.0458(2) 0.0297(11) Uani 1 1 d . . . H111 H 1.0377 -0.1455 1.0851 0.044 Uiso 1 1 calc R . . H112 H 1.1202 -0.1233 1.0209 0.044 Uiso 1 1 calc R . . H113 H 1.0931 -0.2029 1.0534 0.044 Uiso 1 1 calc R . . C72 C 0.7970(4) -0.1950(2) 1.0563(2) 0.0283(10) Uani 1 1 d . . . H114 H 0.7695 -0.1766 1.0904 0.042 Uiso 1 1 calc R . . H115 H 0.8325 -0.2428 1.0724 0.042 Uiso 1 1 calc R . . H116 H 0.7263 -0.1940 1.0334 0.042 Uiso 1 1 calc R . . C73 C 0.6465(4) -0.2253(2) 0.8082(2) 0.0247(10) Uani 1 1 d . . . H117 H 0.6366 -0.2745 0.8157 0.037 Uiso 1 1 calc R . . H118 H 0.7244 -0.2204 0.8231 0.037 Uiso 1 1 calc R . . H119 H 0.6475 -0.2007 0.7640 0.037 Uiso 1 1 calc R . . C74 C 0.4963(4) -0.2463(2) 0.9307(2) 0.0282(10) Uani 1 1 d . . . H120 H 0.4232 -0.2296 0.9524 0.042 Uiso 1 1 calc R . . H121 H 0.5699 -0.2467 0.9515 0.042 Uiso 1 1 calc R . . H122 H 0.4861 -0.2933 0.9307 0.042 Uiso 1 1 calc R . . C75 C 0.3722(4) -0.1876(2) 0.8127(2) 0.0281(10) Uani 1 1 d . . . H123 H 0.3611 -0.2350 0.8139 0.042 Uiso 1 1 calc R . . H124 H 0.3801 -0.1577 0.7699 0.042 Uiso 1 1 calc R . . H125 H 0.3006 -0.1703 0.8348 0.042 Uiso 1 1 calc R . . C76 C 0.2773(4) -0.0744(2) 0.9024(2) 0.0261(10) Uani 1 1 d . . . H126 H 0.2251 -0.0521 0.9294 0.039 Uiso 1 1 calc R . . H127 H 0.2700 -0.1246 0.9179 0.039 Uiso 1 1 calc R . . H128 H 0.2505 -0.0560 0.8608 0.039 Uiso 1 1 calc R . . C77 C 0.4506(4) 0.0396(2) 0.8764(2) 0.0268(10) Uani 1 1 d . . . H129 H 0.4023 0.0584 0.9069 0.040 Uiso 1 1 calc R . . H130 H 0.4168 0.0606 0.8365 0.040 Uiso 1 1 calc R . . H131 H 0.5370 0.0503 0.8731 0.040 Uiso 1 1 calc R . . C78 C 0.4936(4) -0.0929(2) 0.9804(2) 0.0267(10) Uani 1 1 d . . . H132 H 0.5794 -0.0828 0.9799 0.040 Uiso 1 1 calc R . . H133 H 0.4878 -0.1432 0.9949 0.040 Uiso 1 1 calc R . . H134 H 0.4404 -0.0719 1.0079 0.040 Uiso 1 1 calc R . . C81 C 0.7344(8) 0.0626(4) 0.4703(4) 0.093(3) Uani 1 1 d . . . H139 H 0.6602 0.0932 0.4737 0.139 Uiso 1 1 calc R . . H140 H 0.7105 0.0197 0.4659 0.139 Uiso 1 1 calc R . . H141 H 0.7884 0.0858 0.4342 0.139 Uiso 1 1 calc R . . C82 C 0.814(4) 0.0427(19) 0.5373(11) 0.64(4) Uani 1 1 d . . . H146 H 0.8468 0.0845 0.5408 0.763 Uiso 1 1 calc R . . H147 H 0.7606 0.0215 0.5748 0.763 Uiso 1 1 calc R . . C83 C 0.9335(13) -0.0161(9) 0.5245(6) 0.230(15) Uani 1 1 d . . . H144 H 0.8983 -0.0478 0.5073 0.276 Uiso 1 1 calc R . . H145 H 0.9617 -0.0444 0.5649 0.276 Uiso 1 1 calc R . . C80 C 0.4327(11) 0.4526(6) 0.0203(6) 0.055(3) Uiso 0.50 1 d P . . H137 H 0.4377 0.4161 0.0606 0.066 Uiso 0.50 1 calc PR . . H138 H 0.3606 0.4467 0.0006 0.066 Uiso 0.50 1 calc PR . . Cl3 Cl 0.4268(2) 0.54719(12) 0.02818(10) 0.0927(7) 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 S1 0.0189(5) 0.0125(5) 0.0170(5) -0.0031(4) 0.0023(4) -0.0025(4) C1 0.019(2) 0.0118(19) 0.014(2) -0.0012(16) 0.0020(16) 0.0005(16) C2 0.018(2) 0.0110(19) 0.015(2) -0.0052(16) -0.0033(16) 0.0022(16) C3 0.014(2) 0.0113(19) 0.019(2) -0.0038(16) -0.0025(16) 0.0015(15) C4 0.018(2) 0.0111(19) 0.017(2) -0.0080(16) -0.0005(16) -0.0031(16) C5 0.016(2) 0.014(2) 0.015(2) -0.0036(16) -0.0042(16) -0.0023(16) C6 0.017(2) 0.0117(19) 0.016(2) -0.0054(16) -0.0051(16) 0.0001(16) C7 0.017(2) 0.013(2) 0.018(2) -0.0004(16) -0.0023(16) -0.0001(16) C8 0.015(2) 0.0116(19) 0.020(2) -0.0019(16) -0.0036(17) 0.0001(16) C9 0.019(2) 0.013(2) 0.018(2) -0.0046(16) -0.0012(17) -0.0009(16) Si1 0.0192(6) 0.0129(5) 0.0221(6) -0.0031(5) -0.0059(5) 0.0000(4) Si2 0.0259(6) 0.0160(6) 0.0188(6) -0.0039(5) -0.0072(5) 0.0001(5) Si3 0.0154(6) 0.0138(6) 0.0208(6) -0.0028(5) 0.0006(5) -0.0014(4) Si4 0.0181(6) 0.0176(6) 0.0165(6) -0.0042(5) 0.0005(5) -0.0003(5) Si5 0.0146(6) 0.0154(6) 0.0216(6) -0.0059(5) -0.0029(5) -0.0002(4) Si6 0.0150(6) 0.0169(6) 0.0183(6) -0.0059(5) -0.0033(4) -0.0013(4) C10 0.031(3) 0.018(2) 0.048(3) -0.016(2) -0.012(2) 0.0027(19) C11 0.035(3) 0.020(2) 0.032(3) -0.001(2) -0.003(2) 0.007(2) C12 0.027(2) 0.021(2) 0.034(3) -0.009(2) 0.001(2) 0.0022(19) C13 0.040(3) 0.035(3) 0.021(2) -0.006(2) -0.010(2) -0.008(2) C14 0.030(3) 0.031(3) 0.034(3) -0.012(2) -0.010(2) -0.013(2) C15 0.044(3) 0.030(3) 0.041(3) -0.020(2) -0.018(2) 0.010(2) C16 0.023(2) 0.020(2) 0.031(3) -0.0108(19) -0.0061(19) -0.0018(18) C17 0.022(2) 0.021(2) 0.034(3) -0.002(2) 0.003(2) -0.0021(19) C18 0.022(2) 0.021(2) 0.026(2) -0.0048(18) -0.0055(19) 0.0026(18) C19 0.025(2) 0.028(2) 0.020(2) -0.0074(19) 0.0044(18) -0.0019(19) C20 0.025(2) 0.029(2) 0.024(2) -0.0053(19) -0.0047(19) -0.0016(19) C21 0.030(3) 0.027(2) 0.027(2) -0.011(2) 0.006(2) -0.003(2) C22 0.026(2) 0.021(2) 0.028(2) -0.0116(19) -0.0025(19) -0.0003(18) C23 0.026(2) 0.021(2) 0.029(3) -0.0027(19) -0.010(2) -0.0002(19) C24 0.021(2) 0.027(3) 0.044(3) -0.012(2) -0.001(2) -0.0010(19) C25 0.024(2) 0.026(2) 0.024(2) -0.0074(19) -0.0032(19) -0.0010(19) C26 0.018(2) 0.028(2) 0.031(3) -0.010(2) -0.0069(19) -0.0018(18) C27 0.034(3) 0.020(2) 0.025(2) -0.0084(19) -0.007(2) -0.0047(19) C28 0.021(2) 0.0122(19) 0.0109(19) -0.0019(15) -0.0045(16) 0.0002(16) C29 0.031(3) 0.019(2) 0.021(2) -0.0027(18) -0.0031(19) -0.0026(19) C30 0.044(3) 0.022(2) 0.030(3) -0.012(2) -0.005(2) -0.002(2) C31 0.042(3) 0.028(3) 0.028(3) -0.018(2) -0.006(2) 0.010(2) C32 0.023(2) 0.029(2) 0.024(2) -0.0103(19) 0.0041(19) -0.0007(19) C33 0.019(2) 0.017(2) 0.022(2) -0.0072(17) -0.0026(17) 0.0032(17) S2 0.0173(5) 0.0188(5) 0.0287(6) -0.0088(4) 0.0032(4) -0.0023(4) C34 0.021(2) 0.013(2) 0.019(2) -0.0008(16) 0.0036(17) -0.0036(16) C35 0.030(2) 0.022(2) 0.016(2) -0.0044(18) 0.0031(18) -0.0047(19) C36 0.034(3) 0.027(2) 0.016(2) 0.0010(18) -0.0041(19) -0.004(2) C37 0.032(3) 0.022(2) 0.020(2) -0.0002(18) -0.0040(19) 0.0013(19) C38 0.023(2) 0.016(2) 0.022(2) -0.0057(17) 0.0041(18) -0.0017(17) C39 0.017(2) 0.016(2) 0.015(2) -0.0004(16) 0.0061(16) -0.0017(16) S3 0.0221(6) 0.0184(5) 0.0263(6) -0.0090(4) -0.0033(4) 0.0014(4) S4 0.0219(6) 0.0181(5) 0.0269(6) -0.0083(4) 0.0020(4) -0.0047(4) C40 0.018(2) 0.018(2) 0.017(2) -0.0016(17) -0.0060(17) 0.0007(17) C41 0.026(2) 0.019(2) 0.020(2) -0.0053(18) -0.0064(18) -0.0008(18) C42 0.024(2) 0.025(2) 0.022(2) -0.0020(19) 0.0011(18) -0.0097(19) C43 0.023(2) 0.026(2) 0.018(2) -0.0010(18) 0.0012(18) -0.0001(19) C44 0.027(2) 0.019(2) 0.016(2) -0.0028(17) -0.0048(18) 0.0027(18) C45 0.017(2) 0.014(2) 0.024(2) -0.0055(17) -0.0118(17) -0.0003(16) S5 0.0171(5) 0.0196(5) 0.0338(6) -0.0120(5) -0.0045(5) -0.0007(4) C46 0.019(2) 0.017(2) 0.026(2) -0.0076(18) 0.0006(18) 0.0014(17) C47 0.033(3) 0.028(3) 0.032(3) -0.014(2) -0.004(2) 0.002(2) C48 0.035(3) 0.034(3) 0.037(3) -0.023(2) -0.002(2) -0.005(2) C49 0.038(3) 0.026(3) 0.042(3) -0.022(2) 0.005(2) -0.001(2) C50 0.026(2) 0.020(2) 0.026(2) -0.0041(19) 0.0010(19) 0.0018(18) C51 0.020(2) 0.017(2) 0.020(2) -0.0068(17) 0.0053(17) -0.0034(17) S6 0.0227(5) 0.0136(5) 0.0194(5) -0.0035(4) -0.0019(4) 0.0016(4) C52 0.022(2) 0.012(2) 0.018(2) -0.0025(16) -0.0012(17) -0.0004(16) C53 0.026(2) 0.0093(19) 0.026(2) -0.0024(17) 0.0049(19) 0.0030(17) C54 0.017(2) 0.017(2) 0.026(2) -0.0042(18) 0.0027(18) 0.0012(17) C55 0.019(2) 0.013(2) 0.021(2) -0.0051(16) -0.0001(17) -0.0009(16) C56 0.017(2) 0.014(2) 0.019(2) -0.0032(17) 0.0024(17) -0.0020(16) C57 0.014(2) 0.014(2) 0.019(2) -0.0082(16) 0.0004(16) 0.0002(16) C58 0.017(2) 0.019(2) 0.030(2) 0.0015(18) 0.0007(18) 0.0000(17) C59 0.013(2) 0.016(2) 0.021(2) -0.0033(17) -0.0006(16) -0.0034(16) C60 0.017(2) 0.015(2) 0.013(2) -0.0031(16) 0.0002(16) -0.0013(16) Si7 0.0191(6) 0.0149(6) 0.0433(8) 0.0023(5) 0.0032(6) -0.0023(5) Si8 0.0311(7) 0.0244(7) 0.0325(8) 0.0038(6) 0.0149(6) 0.0026(6) Si9 0.0220(6) 0.0139(6) 0.0269(7) -0.0049(5) -0.0012(5) 0.0017(5) Si10 0.0207(6) 0.0162(6) 0.0228(6) -0.0042(5) -0.0011(5) -0.0024(5) Si11 0.0193(6) 0.0147(6) 0.0225(6) -0.0066(5) 0.0003(5) -0.0026(5) Si12 0.0176(6) 0.0164(6) 0.0213(6) -0.0072(5) 0.0022(5) -0.0020(5) C61 0.028(3) 0.026(3) 0.076(4) -0.024(3) 0.007(3) -0.005(2) C62 0.040(3) 0.032(3) 0.067(4) 0.013(3) -0.004(3) -0.010(2) C63 0.038(3) 0.020(2) 0.048(3) -0.003(2) -0.005(2) 0.001(2) C64 0.070(5) 0.052(4) 0.055(4) 0.018(3) 0.034(3) 0.015(3) C65 0.031(3) 0.047(3) 0.055(4) -0.014(3) 0.017(3) 0.003(2) C66 0.050(4) 0.049(4) 0.051(4) -0.023(3) 0.019(3) -0.004(3) C67 0.035(3) 0.026(2) 0.036(3) -0.014(2) -0.009(2) 0.006(2) C68 0.036(3) 0.019(2) 0.041(3) -0.010(2) 0.001(2) -0.004(2) C69 0.041(3) 0.021(2) 0.036(3) -0.006(2) -0.009(2) 0.009(2) C70 0.035(3) 0.022(2) 0.033(3) -0.010(2) -0.001(2) 0.001(2) C71 0.033(3) 0.029(3) 0.026(3) -0.009(2) -0.003(2) 0.000(2) C72 0.029(3) 0.029(3) 0.027(2) -0.007(2) 0.000(2) -0.005(2) C73 0.027(2) 0.015(2) 0.033(3) -0.0112(19) 0.000(2) 0.0003(18) C74 0.033(3) 0.018(2) 0.031(3) -0.0053(19) 0.004(2) -0.0081(19) C75 0.026(2) 0.025(2) 0.041(3) -0.021(2) -0.002(2) -0.0013(19) C76 0.017(2) 0.028(2) 0.038(3) -0.021(2) 0.0026(19) -0.0003(18) C77 0.031(3) 0.018(2) 0.029(3) -0.0075(19) 0.003(2) -0.0003(19) C78 0.031(3) 0.026(2) 0.024(2) -0.0100(19) 0.0001(19) -0.001(2) C81 0.105(7) 0.049(4) 0.118(7) -0.032(5) 0.014(5) 0.015(4) C82 0.94(9) 0.68(7) 0.23(3) -0.20(4) -0.20(4) 0.51(7) C83 0.32(3) 0.236(19) 0.23(2) -0.212(19) -0.24(2) 0.22(2) Cl3 0.1165(18) 0.0934(16) 0.0802(14) -0.0385(12) -0.0347(13) 0.0034(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 S1 C28 1.772(4) . ? S1 C1 1.782(4) . ? C1 C2 1.417(6) . ? C1 C6 1.421(5) . ? C2 C3 1.393(5) . ? C2 C7 1.522(5) . ? C3 C4 1.396(5) . ? C4 C5 1.393(5) . ? C4 C8 1.509(5) . ? C5 C6 1.405(5) . ? C6 C9 1.502(5) . ? C7 Si2 1.900(4) . ? C7 Si1 1.903(4) . ? C8 Si3 1.896(4) . ? C8 Si4 1.908(4) . ? C9 Si5 1.903(4) . ? C9 Si6 1.906(4) . ? Si1 C11 1.867(4) . ? Si1 C10 1.868(5) . ? Si1 C12 1.874(5) . ? Si2 C15 1.869(5) . ? Si2 C13 1.871(4) . ? Si2 C14 1.873(5) . ? Si3 C18 1.871(4) . ? Si3 C17 1.875(4) . ? Si3 C16 1.878(4) . ? Si4 C20 1.872(4) . ? Si4 C19 1.879(4) . ? Si4 C21 1.882(5) . ? Si5 C22 1.870(4) . ? Si5 C23 1.870(4) . ? Si5 C24 1.870(5) . ? Si6 C25 1.860(4) . ? Si6 C27 1.871(4) . ? Si6 C26 1.875(4) . ? C28 C29 1.386(6) . ? C28 C33 1.400(6) . ? C29 C30 1.383(6) . ? C30 C31 1.386(7) . ? C31 C32 1.388(6) . ? C32 C33 1.396(6) . ? C33 S2 1.787(4) . ? S2 C34 1.781(4) . ? C34 C35 1.379(6) . ? C34 C39 1.404(6) . ? C35 C36 1.394(6) . ? C36 C37 1.388(6) . ? C37 C38 1.386(6) . ? C38 C39 1.393(6) . ? C39 S3 1.794(4) . ? S3 S4 2.0364(15) . ? S4 C40 1.792(4) . ? C40 C41 1.389(6) . ? C40 C45 1.405(6) . ? C41 C42 1.381(6) . ? C42 C43 1.391(6) . ? C43 C44 1.382(6) . ? C44 C45 1.392(6) . ? C45 S5 1.779(4) . ? S5 C46 1.773(4) . ? C46 C47 1.401(6) . ? C46 C51 1.412(6) . ? C47 C48 1.377(6) . ? C48 C49 1.383(7) . ? C49 C50 1.388(6) . ? C50 C51 1.390(6) . ? C51 S6 1.774(4) . ? S6 C52 1.784(4) . ? C52 C57 1.416(5) . ? C52 C53 1.418(6) . ? C53 C54 1.389(6) . ? C53 C58 1.520(6) . ? C54 C55 1.396(6) . ? C55 C56 1.399(6) . ? C55 C59 1.510(5) . ? C56 C57 1.404(6) . ? C57 C60 1.511(5) . ? C58 Si8 1.897(4) . ? C58 Si7 1.901(5) . ? C59 Si9 1.899(4) . ? C59 Si10 1.903(4) . ? C60 Si12 1.897(4) . ? C60 Si11 1.907(4) . ? Si7 C63 1.866(5) . ? Si7 C61 1.867(5) . ? Si7 C62 1.873(5) . ? Si8 C65 1.859(6) . ? Si8 C64 1.859(5) . ? Si8 C66 1.870(6) . ? Si9 C68 1.866(5) . ? Si9 C67 1.870(5) . ? Si9 C69 1.878(5) . ? Si10 C72 1.867(5) . ? Si10 C71 1.870(5) . ? Si10 C70 1.875(4) . ? Si11 C75 1.861(5) . ? Si11 C73 1.869(4) . ? Si11 C74 1.870(4) . ? Si12 C77 1.868(4) . ? Si12 C78 1.869(4) . ? Si12 C76 1.873(4) . ? C81 C82 1.77(3) . ? C82 C83 1.74(3) . ? C83 C83 1.78(4) 2_756 ? C80 Cl3 1.790(12) 2_665 ? C80 Cl3 1.992(12) . ? Cl3 C80 1.790(12) 2_665 ? 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 C28 S1 C1 106.39(18) . . ? C2 C1 C6 120.7(3) . . ? C2 C1 S1 119.0(3) . . ? C6 C1 S1 119.4(3) . . ? C3 C2 C1 118.0(3) . . ? C3 C2 C7 119.0(3) . . ? C1 C2 C7 123.0(3) . . ? C2 C3 C4 123.2(4) . . ? C5 C4 C3 117.4(4) . . ? C5 C4 C8 122.5(3) . . ? C3 C4 C8 120.1(3) . . ? C4 C5 C6 122.8(4) . . ? C5 C6 C1 117.7(4) . . ? C5 C6 C9 119.0(3) . . ? C1 C6 C9 123.3(4) . . ? C2 C7 Si2 111.9(3) . . ? C2 C7 Si1 111.3(3) . . ? Si2 C7 Si1 118.9(2) . . ? C4 C8 Si3 112.3(3) . . ? C4 C8 Si4 112.2(3) . . ? Si3 C8 Si4 119.9(2) . . ? C6 C9 Si5 112.6(3) . . ? C6 C9 Si6 112.0(3) . . ? Si5 C9 Si6 117.3(2) . . ? C11 Si1 C10 108.4(2) . . ? C11 Si1 C12 108.3(2) . . ? C10 Si1 C12 108.4(2) . . ? C11 Si1 C7 110.2(2) . . ? C10 Si1 C7 107.06(19) . . ? C12 Si1 C7 114.35(19) . . ? C15 Si2 C13 107.6(2) . . ? C15 Si2 C14 107.6(2) . . ? C13 Si2 C14 108.3(2) . . ? C15 Si2 C7 109.0(2) . . ? C13 Si2 C7 109.8(2) . . ? C14 Si2 C7 114.37(19) . . ? C18 Si3 C17 108.3(2) . . ? C18 Si3 C16 109.3(2) . . ? C17 Si3 C16 108.1(2) . . ? C18 Si3 C8 114.54(19) . . ? C17 Si3 C8 108.70(19) . . ? C16 Si3 C8 107.71(18) . . ? C20 Si4 C19 108.2(2) . . ? C20 Si4 C21 109.4(2) . . ? C19 Si4 C21 108.3(2) . . ? C20 Si4 C8 115.03(19) . . ? C19 Si4 C8 108.53(19) . . ? C21 Si4 C8 107.21(19) . . ? C22 Si5 C23 107.2(2) . . ? C22 Si5 C24 107.2(2) . . ? C23 Si5 C24 108.1(2) . . ? C22 Si5 C9 110.88(19) . . ? C23 Si5 C9 113.78(19) . . ? C24 Si5 C9 109.3(2) . . ? C25 Si6 C27 107.0(2) . . ? C25 Si6 C26 109.3(2) . . ? C27 Si6 C26 109.0(2) . . ? C25 Si6 C9 113.42(19) . . ? C27 Si6 C9 110.43(18) . . ? C26 Si6 C9 107.61(19) . . ? C29 C28 C33 118.9(4) . . ? C29 C28 S1 122.9(3) . . ? C33 C28 S1 118.2(3) . . ? C30 C29 C28 121.0(4) . . ? C29 C30 C31 120.5(4) . . ? C30 C31 C32 119.2(4) . . ? C31 C32 C33 120.6(4) . . ? C32 C33 C28 119.9(4) . . ? C32 C33 S2 116.6(3) . . ? C28 C33 S2 123.1(3) . . ? C34 S2 C33 103.88(19) . . ? C35 C34 C39 119.8(4) . . ? C35 C34 S2 122.2(3) . . ? C39 C34 S2 118.0(3) . . ? C34 C35 C36 120.7(4) . . ? C37 C36 C35 119.0(4) . . ? C38 C37 C36 121.1(4) . . ? C37 C38 C39 119.4(4) . . ? C38 C39 C34 119.8(4) . . ? C38 C39 S3 123.2(3) . . ? C34 C39 S3 117.0(3) . . ? C39 S3 S4 106.17(14) . . ? C40 S4 S3 105.52(15) . . ? C41 C40 C45 119.5(4) . . ? C41 C40 S4 124.2(3) . . ? C45 C40 S4 116.3(3) . . ? C42 C41 C40 120.3(4) . . ? C41 C42 C43 120.4(4) . . ? C44 C43 C42 119.8(4) . . ? C43 C44 C45 120.4(4) . . ? C44 C45 C40 119.6(4) . . ? C44 C45 S5 121.8(3) . . ? C40 C45 S5 118.6(3) . . ? C46 S5 C45 103.9(2) . . ? C47 C46 C51 118.7(4) . . ? C47 C46 S5 117.9(3) . . ? C51 C46 S5 122.9(3) . . ? C48 C47 C46 121.4(4) . . ? C47 C48 C49 119.5(4) . . ? C48 C49 C50 120.5(4) . . ? C49 C50 C51 120.6(4) . . ? C50 C51 C46 119.3(4) . . ? C50 C51 S6 122.7(3) . . ? C46 C51 S6 118.0(3) . . ? C51 S6 C52 104.95(19) . . ? C57 C52 C53 120.4(4) . . ? C57 C52 S6 119.4(3) . . ? C53 C52 S6 119.4(3) . . ? C54 C53 C52 117.9(4) . . ? C54 C53 C58 119.0(4) . . ? C52 C53 C58 123.1(4) . . ? C53 C54 C55 123.8(4) . . ? C54 C55 C56 117.0(4) . . ? C54 C55 C59 120.7(4) . . ? C56 C55 C59 122.2(4) . . ? C55 C56 C57 122.3(4) . . ? C56 C57 C52 118.5(4) . . ? C56 C57 C60 118.6(3) . . ? C52 C57 C60 122.8(4) . . ? C53 C58 Si8 112.6(3) . . ? C53 C58 Si7 111.0(3) . . ? Si8 C58 Si7 118.5(2) . . ? C55 C59 Si9 113.3(3) . . ? C55 C59 Si10 112.3(3) . . ? Si9 C59 Si10 119.7(2) . . ? C57 C60 Si12 112.4(3) . . ? C57 C60 Si11 113.0(3) . . ? Si12 C60 Si11 117.2(2) . . ? C63 Si7 C61 108.1(3) . . ? C63 Si7 C62 107.9(2) . . ? C61 Si7 C62 108.2(3) . . ? C63 Si7 C58 114.4(2) . . ? C61 Si7 C58 107.7(2) . . ? C62 Si7 C58 110.3(3) . . ? C65 Si8 C64 107.7(3) . . ? C65 Si8 C66 106.7(3) . . ? C64 Si8 C66 108.5(3) . . ? C65 Si8 C58 114.5(2) . . ? C64 Si8 C58 109.4(2) . . ? C66 Si8 C58 109.9(2) . . ? C68 Si9 C67 108.5(2) . . ? C68 Si9 C69 108.6(2) . . ? C67 Si9 C69 108.9(2) . . ? C68 Si9 C59 114.76(19) . . ? C67 Si9 C59 108.4(2) . . ? C69 Si9 C59 107.5(2) . . ? C72 Si10 C71 108.0(2) . . ? C72 Si10 C70 109.6(2) . . ? C71 Si10 C70 107.8(2) . . ? C72 Si10 C59 114.2(2) . . ? C71 Si10 C59 109.53(19) . . ? C70 Si10 C59 107.62(19) . . ? C75 Si11 C73 107.4(2) . . ? C75 Si11 C74 107.8(2) . . ? C73 Si11 C74 108.1(2) . . ? C75 Si11 C60 108.74(19) . . ? C73 Si11 C60 111.15(18) . . ? C74 Si11 C60 113.37(19) . . ? C77 Si12 C78 107.8(2) . . ? C77 Si12 C76 108.2(2) . . ? C78 Si12 C76 109.2(2) . . ? C77 Si12 C60 110.39(19) . . ? C78 Si12 C60 112.97(19) . . ? C76 Si12 C60 108.21(19) . . ? C83 C82 C81 102.0(13) . . ? C82 C83 C83 119(2) . 2_756 ? Cl3 C80 Cl3 100.0(6) 2_665 . ? C80 Cl3 C80 80.0(6) 2_665 . ? 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 C28 S1 C1 C2 110.3(3) . . . . ? C28 S1 C1 C6 -80.1(3) . . . . ? C6 C1 C2 C3 -4.5(6) . . . . ? S1 C1 C2 C3 164.9(3) . . . . ? C6 C1 C2 C7 175.0(4) . . . . ? S1 C1 C2 C7 -15.6(5) . . . . ? C1 C2 C3 C4 1.0(6) . . . . ? C7 C2 C3 C4 -178.5(3) . . . . ? C2 C3 C4 C5 2.4(6) . . . . ? C2 C3 C4 C8 -178.2(4) . . . . ? C3 C4 C5 C6 -2.3(6) . . . . ? C8 C4 C5 C6 178.2(4) . . . . ? C4 C5 C6 C1 -1.1(6) . . . . ? C4 C5 C6 C9 177.6(3) . . . . ? C2 C1 C6 C5 4.5(5) . . . . ? S1 C1 C6 C5 -164.9(3) . . . . ? C2 C1 C6 C9 -174.0(4) . . . . ? S1 C1 C6 C9 16.6(5) . . . . ? C3 C2 C7 Si2 62.4(4) . . . . ? C1 C2 C7 Si2 -117.1(4) . . . . ? C3 C2 C7 Si1 -73.2(4) . . . . ? C1 C2 C7 Si1 107.3(4) . . . . ? C5 C4 C8 Si3 72.8(4) . . . . ? C3 C4 C8 Si3 -106.7(4) . . . . ? C5 C4 C8 Si4 -65.7(4) . . . . ? C3 C4 C8 Si4 114.8(3) . . . . ? C5 C6 C9 Si5 -55.1(4) . . . . ? C1 C6 C9 Si5 123.4(3) . . . . ? C5 C6 C9 Si6 79.7(4) . . . . ? C1 C6 C9 Si6 -101.7(4) . . . . ? C2 C7 Si1 C11 -171.5(3) . . . . ? Si2 C7 Si1 C11 56.3(3) . . . . ? C2 C7 Si1 C10 -53.8(3) . . . . ? Si2 C7 Si1 C10 174.0(2) . . . . ? C2 C7 Si1 C12 66.3(3) . . . . ? Si2 C7 Si1 C12 -65.9(3) . . . . ? C2 C7 Si2 C15 44.3(3) . . . . ? Si1 C7 Si2 C15 176.3(2) . . . . ? C2 C7 Si2 C13 162.0(3) . . . . ? Si1 C7 Si2 C13 -66.1(3) . . . . ? C2 C7 Si2 C14 -76.2(3) . . . . ? Si1 C7 Si2 C14 55.8(3) . . . . ? C4 C8 Si3 C18 -78.8(3) . . . . ? Si4 C8 Si3 C18 56.1(3) . . . . ? C4 C8 Si3 C17 159.9(3) . . . . ? Si4 C8 Si3 C17 -65.1(3) . . . . ? C4 C8 Si3 C16 43.0(3) . . . . ? Si4 C8 Si3 C16 177.9(2) . . . . ? C4 C8 Si4 C20 87.8(3) . . . . ? Si3 C8 Si4 C20 -47.3(3) . . . . ? C4 C8 Si4 C19 -150.9(3) . . . . ? Si3 C8 Si4 C19 74.1(3) . . . . ? C4 C8 Si4 C21 -34.1(3) . . . . ? Si3 C8 Si4 C21 -169.1(2) . . . . ? C6 C9 Si5 C22 -27.3(3) . . . . ? Si6 C9 Si5 C22 -159.5(2) . . . . ? C6 C9 Si5 C23 93.7(3) . . . . ? Si6 C9 Si5 C23 -38.5(3) . . . . ? C6 C9 Si5 C24 -145.3(3) . . . . ? Si6 C9 Si5 C24 82.5(3) . . . . ? C6 C9 Si6 C25 -61.0(3) . . . . ? Si5 C9 Si6 C25 71.6(3) . . . . ? C6 C9 Si6 C27 59.2(3) . . . . ? Si5 C9 Si6 C27 -168.3(2) . . . . ? C6 C9 Si6 C26 178.1(3) . . . . ? Si5 C9 Si6 C26 -49.4(3) . . . . ? C1 S1 C28 C29 -12.6(4) . . . . ? C1 S1 C28 C33 167.8(3) . . . . ? C33 C28 C29 C30 -2.3(6) . . . . ? S1 C28 C29 C30 178.2(3) . . . . ? C28 C29 C30 C31 2.9(7) . . . . ? C29 C30 C31 C32 -1.2(7) . . . . ? C30 C31 C32 C33 -1.2(7) . . . . ? C31 C32 C33 C28 1.8(6) . . . . ? C31 C32 C33 S2 -170.4(3) . . . . ? C29 C28 C33 C32 -0.1(6) . . . . ? S1 C28 C33 C32 179.5(3) . . . . ? C29 C28 C33 S2 171.6(3) . . . . ? S1 C28 C33 S2 -8.9(5) . . . . ? C32 C33 S2 C34 -125.3(3) . . . . ? C28 C33 S2 C34 62.8(4) . . . . ? C33 S2 C34 C35 32.7(4) . . . . ? C33 S2 C34 C39 -148.1(3) . . . . ? C39 C34 C35 C36 0.1(6) . . . . ? S2 C34 C35 C36 179.3(3) . . . . ? C34 C35 C36 C37 -2.4(6) . . . . ? C35 C36 C37 C38 2.3(6) . . . . ? C36 C37 C38 C39 0.0(6) . . . . ? C37 C38 C39 C34 -2.3(6) . . . . ? C37 C38 C39 S3 176.8(3) . . . . ? C35 C34 C39 C38 2.2(6) . . . . ? S2 C34 C39 C38 -177.0(3) . . . . ? C35 C34 C39 S3 -176.9(3) . . . . ? S2 C34 C39 S3 3.9(4) . . . . ? C38 C39 S3 S4 11.6(4) . . . . ? C34 C39 S3 S4 -169.4(3) . . . . ? C39 S3 S4 C40 -84.65(19) . . . . ? S3 S4 C40 C41 13.8(4) . . . . ? S3 S4 C40 C45 -169.1(3) . . . . ? C45 C40 C41 C42 -1.1(6) . . . . ? S4 C40 C41 C42 176.0(3) . . . . ? C40 C41 C42 C43 -0.1(6) . . . . ? C41 C42 C43 C44 1.6(6) . . . . ? C42 C43 C44 C45 -1.8(6) . . . . ? C43 C44 C45 C40 0.6(6) . . . . ? C43 C44 C45 S5 177.8(3) . . . . ? C41 C40 C45 C44 0.8(6) . . . . ? S4 C40 C45 C44 -176.4(3) . . . . ? C41 C40 C45 S5 -176.5(3) . . . . ? S4 C40 C45 S5 6.2(4) . . . . ? C44 C45 S5 C46 34.0(4) . . . . ? C40 C45 S5 C46 -148.7(3) . . . . ? C45 S5 C46 C47 -123.7(4) . . . . ? C45 S5 C46 C51 64.3(4) . . . . ? C51 C46 C47 C48 0.8(7) . . . . ? S5 C46 C47 C48 -171.6(4) . . . . ? C46 C47 C48 C49 0.3(7) . . . . ? C47 C48 C49 C50 -1.5(7) . . . . ? C48 C49 C50 C51 1.6(7) . . . . ? C49 C50 C51 C46 -0.5(6) . . . . ? C49 C50 C51 S6 179.4(3) . . . . ? C47 C46 C51 C50 -0.7(6) . . . . ? S5 C46 C51 C50 171.3(3) . . . . ? C47 C46 C51 S6 179.4(3) . . . . ? S5 C46 C51 S6 -8.6(5) . . . . ? C50 C51 S6 C52 -10.7(4) . . . . ? C46 C51 S6 C52 169.2(3) . . . . ? C51 S6 C52 C57 -84.0(4) . . . . ? C51 S6 C52 C53 105.5(3) . . . . ? C57 C52 C53 C54 -3.0(6) . . . . ? S6 C52 C53 C54 167.3(3) . . . . ? C57 C52 C53 C58 176.6(4) . . . . ? S6 C52 C53 C58 -13.0(6) . . . . ? C52 C53 C54 C55 0.8(6) . . . . ? C58 C53 C54 C55 -178.8(4) . . . . ? C53 C54 C55 C56 1.6(6) . . . . ? C53 C54 C55 C59 -177.5(4) . . . . ? C54 C55 C56 C57 -2.0(6) . . . . ? C59 C55 C56 C57 177.1(4) . . . . ? C55 C56 C57 C52 -0.1(6) . . . . ? C55 C56 C57 C60 178.4(4) . . . . ? C53 C52 C57 C56 2.7(6) . . . . ? S6 C52 C57 C56 -167.6(3) . . . . ? C53 C52 C57 C60 -175.7(4) . . . . ? S6 C52 C57 C60 13.9(5) . . . . ? C54 C53 C58 Si8 60.0(5) . . . . ? C52 C53 C58 Si8 -119.6(4) . . . . ? C54 C53 C58 Si7 -75.5(4) . . . . ? C52 C53 C58 Si7 104.9(4) . . . . ? C54 C55 C59 Si9 -109.1(4) . . . . ? C56 C55 C59 Si9 71.9(4) . . . . ? C54 C55 C59 Si10 111.5(4) . . . . ? C56 C55 C59 Si10 -67.6(4) . . . . ? C56 C57 C60 Si12 81.0(4) . . . . ? C52 C57 C60 Si12 -100.6(4) . . . . ? C56 C57 C60 Si11 -54.5(4) . . . . ? C52 C57 C60 Si11 123.9(4) . . . . ? C53 C58 Si7 C63 66.8(4) . . . . ? Si8 C58 Si7 C63 -65.8(3) . . . . ? C53 C58 Si7 C61 -53.5(4) . . . . ? Si8 C58 Si7 C61 173.9(3) . . . . ? C53 C58 Si7 C62 -171.3(3) . . . . ? Si8 C58 Si7 C62 56.1(3) . . . . ? C53 C58 Si8 C65 -79.0(4) . . . . ? Si7 C58 Si8 C65 52.9(3) . . . . ? C53 C58 Si8 C64 160.1(4) . . . . ? Si7 C58 Si8 C64 -68.0(4) . . . . ? C53 C58 Si8 C66 41.1(4) . . . . ? Si7 C58 Si8 C66 173.0(3) . . . . ? C55 C59 Si9 C68 -76.0(3) . . . . ? Si10 C59 Si9 C68 60.2(3) . . . . ? C55 C59 Si9 C67 45.5(3) . . . . ? Si10 C59 Si9 C67 -178.3(2) . . . . ? C55 C59 Si9 C69 163.1(3) . . . . ? Si10 C59 Si9 C69 -60.7(3) . . . . ? C55 C59 Si10 C72 89.8(3) . . . . ? Si9 C59 Si10 C72 -46.8(3) . . . . ? C55 C59 Si10 C71 -149.0(3) . . . . ? Si9 C59 Si10 C71 74.4(3) . . . . ? C55 C59 Si10 C70 -32.1(3) . . . . ? Si9 C59 Si10 C70 -168.7(2) . . . . ? C57 C60 Si11 C75 -147.3(3) . . . . ? Si12 C60 Si11 C75 79.5(3) . . . . ? C57 C60 Si11 C73 -29.2(3) . . . . ? Si12 C60 Si11 C73 -162.4(2) . . . . ? C57 C60 Si11 C74 92.8(3) . . . . ? Si12 C60 Si11 C74 -40.4(3) . . . . ? C57 C60 Si12 C77 60.0(3) . . . . ? Si11 C60 Si12 C77 -166.6(2) . . . . ? C57 C60 Si12 C78 -60.8(3) . . . . ? Si11 C60 Si12 C78 72.7(3) . . . . ? C57 C60 Si12 C76 178.2(3) . . . . ? Si11 C60 Si12 C76 -48.4(3) . . . . ? C81 C82 C83 C83 81(3) . . . 2_756 ? Cl3 C80 Cl3 C80 0.000(1) 2_665 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.554 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.087