# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Carsten von Hanisch' _publ_contact_author_email CARSTEN.VONHAENISCH@INT.FZK.DE _publ_section_title ; Synthesis and structure of [Pb4(SbSiiPr3)6]: the first structurally characterised compound with chemical bonds between lead and antimony ; loop_ _publ_author_name 'Carsten von Hanisch' 'Stephan Traut' # Attachment 'Pb4As4.CIF' data_e:\traut\crystal\st128\p-1 _database_code_depnum_ccdc_archive 'CCDC 751816' #TrackingRef 'Pb4As4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H108 As4 O2 Pb4 Si4' _chemical_formula_weight 2150.30 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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 14.324(3) _cell_length_b 16.404(3) _cell_length_c 18.630(4) _cell_angle_alpha 66.81(3) _cell_angle_beta 71.53(3) _cell_angle_gamma 81.69(3) _cell_volume 3815.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 758 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 26.08 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.283 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 10.619 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0810 _exptl_absorpt_correction_T_max 0.6000 _exptl_absorpt_process_details ? _exptl_special_details ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0350 -1 0 0 0.0140 0 0 -1 0.1330 0 -1 -1 0.1400 0 -2 -1 0.1490 0 -1 0 0.1500 0 1 2 0.1300 -1 8 9 0.1670 ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22737 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.64 _reflns_number_total 13420 _reflns_number_gt 11090 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13420 _refine_ls_number_parameters 653 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.010 _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 Si1 Si -0.22387(16) -0.32875(14) 0.00843(11) 0.0324(4) Uani 1 1 d . . . Si2 Si -0.12849(16) -0.62000(14) 0.40921(11) 0.0309(4) Uani 1 1 d . . . Si3 Si -0.36491(16) -0.16933(14) 0.35578(12) 0.0329(4) Uani 1 1 d . . . Si4 Si 0.16322(16) -0.21324(15) 0.12333(13) 0.0355(5) Uani 1 1 d . . . As1 As -0.18982(6) -0.34232(5) 0.12854(4) 0.03282(17) Uani 1 1 d . . . As2 As -0.13996(6) -0.47073(5) 0.32393(4) 0.03282(17) Uani 1 1 d . . . As3 As -0.24763(6) -0.25225(5) 0.28992(4) 0.03325(17) Uani 1 1 d . . . As4 As 0.00685(6) -0.27693(5) 0.17898(4) 0.03445(18) Uani 1 1 d . . . Pb1 Pb -0.31869(2) -0.40267(2) 0.289249(17) 0.03642(9) Uani 1 1 d . . . Pb2 Pb -0.01995(2) -0.43529(2) 0.163886(16) 0.03532(9) Uani 1 1 d . . . Pb3 Pb -0.08405(2) -0.32856(2) 0.347687(17) 0.03790(9) Uani 1 1 d . . . Pb4 Pb -0.14867(2) -0.176960(19) 0.122158(16) 0.03677(9) Uani 1 1 d . . . O1 O 0.1034(8) -0.0511(8) 0.4456(6) 0.100(3) Uiso 1 1 d . . . O2 O 0.4880(16) 0.1741(14) 0.2485(13) 0.192(7) Uiso 1 1 d . . . C1 C -0.2782(7) -0.4360(6) 0.0250(5) 0.045(2) Uani 1 1 d . . . C2 C -0.3677(11) -0.4579(10) 0.1008(9) 0.098(5) Uani 1 1 d . . . H2A H -0.4166 -0.4092 0.0927 0.118 Uiso 1 1 calc R . . H2B H -0.3469 -0.4656 0.1484 0.118 Uiso 1 1 calc R . . H2C H -0.3968 -0.5128 0.1096 0.118 Uiso 1 1 calc R . . C3 C -0.2056(10) -0.5142(7) 0.0419(9) 0.076(3) Uani 1 1 d . . . H3C H -0.2360 -0.5682 0.0501 0.092 Uiso 1 1 calc R . . H3B H -0.1879 -0.5221 0.0910 0.092 Uiso 1 1 calc R . . H3A H -0.1462 -0.5025 -0.0046 0.092 Uiso 1 1 calc R . . C4 C -0.3120(13) -0.4329(9) -0.0463(8) 0.093(5) Uani 1 1 d . . . H4A H -0.2560 -0.4191 -0.0956 0.111 Uiso 1 1 calc R . . H4B H -0.3636 -0.3869 -0.0554 0.111 Uiso 1 1 calc R . . H4C H -0.3379 -0.4906 -0.0336 0.111 Uiso 1 1 calc R . . C5 C -0.1044(7) -0.2937(6) -0.0788(5) 0.044(2) Uani 1 1 d . . . C6 C -0.0170(9) -0.3532(11) -0.0581(6) 0.095(5) Uani 1 1 d . . . H6A H -0.0299 -0.4146 -0.0475 0.114 Uiso 1 1 calc R . . H6B H -0.0073 -0.3500 -0.0095 0.114 Uiso 1 1 calc R . . H6C H 0.0424 -0.3333 -0.1040 0.114 Uiso 1 1 calc R . . C7 C -0.0820(11) -0.1999(10) -0.0942(7) 0.088(4) Uani 1 1 d . . . H7A H -0.0746 -0.1975 -0.0445 0.106 Uiso 1 1 calc R . . H7B H -0.1361 -0.1598 -0.1097 0.106 Uiso 1 1 calc R . . H7C H -0.0207 -0.1815 -0.1383 0.106 Uiso 1 1 calc R . . C8 C -0.1095(9) -0.2959(10) -0.1584(6) 0.074(4) Uani 1 1 d . . . H8A H -0.1628 -0.2561 -0.1758 0.088 Uiso 1 1 calc R . . H8B H -0.1221 -0.3565 -0.1503 0.088 Uiso 1 1 calc R . . H8C H -0.0468 -0.2766 -0.2004 0.088 Uiso 1 1 calc R . . C9 C -0.3199(6) -0.2359(5) -0.0097(5) 0.0380(18) Uani 1 1 d . . . C10 C -0.3683(6) -0.2002(6) 0.0491(5) 0.0390(18) Uani 1 1 d . . . H10A H -0.3534 -0.2236 0.0997 0.047 Uiso 1 1 calc R . . C11 C -0.4370(7) -0.1322(6) 0.0365(5) 0.047(2) Uani 1 1 d . . . H11A H -0.4680 -0.1089 0.0778 0.056 Uiso 1 1 calc R . . C12 C -0.4610(7) -0.0978(6) -0.0364(6) 0.046(2) Uani 1 1 d . . . H12A H -0.5078 -0.0504 -0.0455 0.055 Uiso 1 1 calc R . . C13 C -0.4168(8) -0.1327(7) -0.0954(6) 0.055(3) Uani 1 1 d . . . H13A H -0.4342 -0.1107 -0.1449 0.066 Uiso 1 1 calc R . . C14 C -0.3460(7) -0.2005(7) -0.0819(6) 0.051(2) Uani 1 1 d . . . H14A H -0.3146 -0.2233 -0.1236 0.062 Uiso 1 1 calc R . . C15 C -0.2221(7) -0.6389(6) 0.5140(5) 0.042(2) Uani 1 1 d . . . C16 C -0.2379(8) -0.7386(6) 0.5668(5) 0.059(3) Uani 1 1 d . . . H16A H -0.1752 -0.7671 0.5753 0.071 Uiso 1 1 calc R . . H16B H -0.2628 -0.7667 0.5391 0.071 Uiso 1 1 calc R . . H16C H -0.2857 -0.7451 0.6197 0.071 Uiso 1 1 calc R . . C17 C -0.1883(8) -0.5958(8) 0.5602(5) 0.059(3) Uani 1 1 d . . . H17C H -0.2369 -0.6058 0.6134 0.070 Uiso 1 1 calc R . . H17B H -0.1817 -0.5319 0.5289 0.070 Uiso 1 1 calc R . . H17A H -0.1246 -0.6218 0.5682 0.070 Uiso 1 1 calc R . . C18 C -0.3210(7) -0.5971(7) 0.5024(5) 0.057(3) Uani 1 1 d . . . H18C H -0.3689 -0.6064 0.5558 0.069 Uiso 1 1 calc R . . H18B H -0.3444 -0.6246 0.4733 0.069 Uiso 1 1 calc R . . H18A H -0.3135 -0.5333 0.4707 0.069 Uiso 1 1 calc R . . C19 C 0.0063(6) -0.6456(6) 0.4106(4) 0.0372(18) Uani 1 1 d . . . C20 C 0.0197(7) -0.7346(6) 0.4795(5) 0.046(2) Uani 1 1 d . . . H20A H -0.0035 -0.7834 0.4721 0.055 Uiso 1 1 calc R . . H20B H -0.0185 -0.7320 0.5325 0.055 Uiso 1 1 calc R . . H20C H 0.0895 -0.7446 0.4773 0.055 Uiso 1 1 calc R . . C21 C 0.0686(7) -0.6524(7) 0.3282(5) 0.050(2) Uani 1 1 d . . . H21A H 0.0638 -0.5961 0.2837 0.060 Uiso 1 1 calc R . . H21B H 0.0438 -0.7002 0.3206 0.060 Uiso 1 1 calc R . . H21C H 0.1375 -0.6653 0.3283 0.060 Uiso 1 1 calc R . . C22 C 0.0500(7) -0.5714(6) 0.4196(5) 0.046(2) Uani 1 1 d . . . H22A H 0.0117 -0.5641 0.4707 0.055 Uiso 1 1 calc R . . H22B H 0.0477 -0.5158 0.3736 0.055 Uiso 1 1 calc R . . H22C H 0.1185 -0.5869 0.4203 0.055 Uiso 1 1 calc R . . C23 C -0.1613(6) -0.6880(5) 0.3580(5) 0.0353(17) Uani 1 1 d . . . C24 C -0.1543(7) -0.7828(6) 0.3918(6) 0.049(2) Uani 1 1 d . . . H24A H -0.1357 -0.8117 0.4406 0.059 Uiso 1 1 calc R . . C25 C -0.1748(8) -0.8327(6) 0.3532(7) 0.056(2) Uani 1 1 d . . . H25A H -0.1701 -0.8956 0.3763 0.068 Uiso 1 1 calc R . . C26 C -0.2022(7) -0.7918(7) 0.2814(6) 0.054(2) Uani 1 1 d . . . H26A H -0.2147 -0.8262 0.2547 0.065 Uiso 1 1 calc R . . C27 C -0.2108(6) -0.7013(6) 0.2501(5) 0.043(2) Uani 1 1 d . . . H27A H -0.2315 -0.6727 0.2021 0.051 Uiso 1 1 calc R . . C28 C -0.1895(6) -0.6502(5) 0.2875(4) 0.0356(17) Uani 1 1 d . . . H28A H -0.1946 -0.5874 0.2636 0.043 Uiso 1 1 calc R . . C29 C -0.2963(6) -0.0863(6) 0.3688(5) 0.0411(19) Uani 1 1 d . . . C30 C -0.2460(8) -0.1384(7) 0.4357(7) 0.059(3) Uani 1 1 d . . . H30A H -0.1994 -0.1823 0.4194 0.071 Uiso 1 1 calc R . . H30B H -0.2958 -0.1687 0.4867 0.071 Uiso 1 1 calc R . . H30C H -0.2105 -0.0973 0.4438 0.071 Uiso 1 1 calc R . . C31 C -0.2157(9) -0.0411(7) 0.2911(6) 0.066(3) Uani 1 1 d . . . H31A H -0.2451 -0.0086 0.2465 0.079 Uiso 1 1 calc R . . H31B H -0.1686 -0.0859 0.2772 0.079 Uiso 1 1 calc R . . H31C H -0.1815 0.0004 0.2998 0.079 Uiso 1 1 calc R . . C32 C -0.3655(8) -0.0150(7) 0.3944(7) 0.063(3) Uani 1 1 d . . . H32A H -0.4150 -0.0438 0.4462 0.076 Uiso 1 1 calc R . . H32B H -0.3985 0.0190 0.3524 0.076 Uiso 1 1 calc R . . H32C H -0.3270 0.0250 0.4010 0.076 Uiso 1 1 calc R . . C33 C -0.4563(6) -0.1180(6) 0.2922(5) 0.0419(19) Uani 1 1 d . . . C34 C -0.4080(7) -0.0471(7) 0.2109(5) 0.055(3) Uani 1 1 d . . . H34A H -0.3522 -0.0735 0.1801 0.066 Uiso 1 1 calc R . . H34B H -0.3845 0.0000 0.2204 0.066 Uiso 1 1 calc R . . H34C H -0.4560 -0.0221 0.1799 0.066 Uiso 1 1 calc R . . C35 C -0.4903(7) -0.1914(7) 0.2746(6) 0.049(2) Uani 1 1 d . . . H35A H -0.5223 -0.2380 0.3261 0.059 Uiso 1 1 calc R . . H35B H -0.4332 -0.2169 0.2441 0.059 Uiso 1 1 calc R . . H35C H -0.5371 -0.1660 0.2423 0.059 Uiso 1 1 calc R . . C36 C -0.5500(7) -0.0783(7) 0.3362(6) 0.057(3) Uani 1 1 d . . . H36C H -0.5932 -0.0533 0.3007 0.068 Uiso 1 1 calc R . . H36B H -0.5320 -0.0315 0.3493 0.068 Uiso 1 1 calc R . . H36A H -0.5845 -0.1250 0.3866 0.068 Uiso 1 1 calc R . . C37 C -0.4323(6) -0.2500(6) 0.4612(4) 0.0389(18) Uani 1 1 d . . . C38 C -0.4031(7) -0.3382(6) 0.4914(5) 0.046(2) Uani 1 1 d . . . H38A H -0.3492 -0.3599 0.4579 0.055 Uiso 1 1 calc R . . C39 C -0.4489(9) -0.3949(6) 0.5675(5) 0.056(3) Uani 1 1 d . . . H39A H -0.4269 -0.4550 0.5862 0.068 Uiso 1 1 calc R . . C40 C -0.5286(8) -0.3645(8) 0.6183(5) 0.057(3) Uani 1 1 d . . . H40A H -0.5622 -0.4038 0.6710 0.068 Uiso 1 1 calc R . . C41 C -0.5565(7) -0.2773(7) 0.5902(5) 0.051(2) Uani 1 1 d . . . H41A H -0.6094 -0.2554 0.6243 0.061 Uiso 1 1 calc R . . C42 C -0.5100(7) -0.2209(7) 0.5142(5) 0.048(2) Uani 1 1 d . . . H42A H -0.5307 -0.1604 0.4967 0.058 Uiso 1 1 calc R . . C43 C 0.1542(7) -0.1126(6) 0.1543(6) 0.047(2) Uani 1 1 d . . . C44 C 0.1523(10) -0.1480(8) 0.2440(7) 0.068(3) Uani 1 1 d . . . H44A H 0.2130 -0.1824 0.2507 0.082 Uiso 1 1 calc R . . H44B H 0.0954 -0.1862 0.2772 0.082 Uiso 1 1 calc R . . H44C H 0.1473 -0.0982 0.2617 0.082 Uiso 1 1 calc R . . C45 C 0.0605(9) -0.0577(8) 0.1452(8) 0.070(3) Uani 1 1 d . . . H45A H 0.0031 -0.0947 0.1796 0.083 Uiso 1 1 calc R . . H45B H 0.0601 -0.0353 0.0881 0.083 Uiso 1 1 calc R . . H45C H 0.0579 -0.0075 0.1619 0.083 Uiso 1 1 calc R . . C46 C 0.2432(8) -0.0480(7) 0.1031(8) 0.066(3) Uani 1 1 d . . . H46A H 0.2461 -0.0252 0.0453 0.080 Uiso 1 1 calc R . . H46B H 0.3048 -0.0803 0.1105 0.080 Uiso 1 1 calc R . . H46C H 0.2343 0.0016 0.1215 0.080 Uiso 1 1 calc R . . C47 C 0.2031(7) -0.1873(6) 0.0073(5) 0.048(2) Uani 1 1 d . . . C48 C 0.1957(10) -0.2713(8) -0.0060(6) 0.070(3) Uani 1 1 d . . . H48A H 0.1277 -0.2915 0.0183 0.084 Uiso 1 1 calc R . . H48B H 0.2394 -0.3175 0.0197 0.084 Uiso 1 1 calc R . . H48C H 0.2153 -0.2592 -0.0646 0.084 Uiso 1 1 calc R . . C49 C 0.3106(9) -0.1569(9) -0.0317(7) 0.073(3) Uani 1 1 d . . . H49C H 0.3291 -0.1441 -0.0903 0.088 Uiso 1 1 calc R . . H49B H 0.3540 -0.2039 -0.0068 0.088 Uiso 1 1 calc R . . H49A H 0.3170 -0.1032 -0.0227 0.088 Uiso 1 1 calc R . . C50 C 0.1378(9) -0.1166(7) -0.0362(6) 0.064(3) Uani 1 1 d . . . H50A H 0.1403 -0.0618 -0.0277 0.077 Uiso 1 1 calc R . . H50B H 0.0699 -0.1370 -0.0143 0.077 Uiso 1 1 calc R . . H50C H 0.1611 -0.1054 -0.0946 0.077 Uiso 1 1 calc R . . C51 C 0.2510(6) -0.3000(6) 0.1694(5) 0.0397(18) Uani 1 1 d . . . C52 C 0.2279(7) -0.3900(6) 0.2076(6) 0.052(2) Uani 1 1 d . . . H52A H 0.1653 -0.4072 0.2119 0.063 Uiso 1 1 calc R . . C53 C 0.2930(8) -0.4549(7) 0.2395(6) 0.057(3) Uani 1 1 d . . . H53A H 0.2754 -0.5155 0.2646 0.069 Uiso 1 1 calc R . . C54 C 0.3838(7) -0.4304(8) 0.2342(6) 0.061(3) Uani 1 1 d . . . H54A H 0.4291 -0.4743 0.2558 0.073 Uiso 1 1 calc R . . C55 C 0.4086(8) -0.3432(8) 0.1982(7) 0.067(3) Uani 1 1 d . . . H55A H 0.4710 -0.3265 0.1951 0.080 Uiso 1 1 calc R . . C56 C 0.3438(7) -0.2798(7) 0.1665(7) 0.060(3) Uani 1 1 d . . . H56A H 0.3629 -0.2195 0.1415 0.072 Uiso 1 1 calc R . . C57 C 0.1884(15) -0.0012(14) 0.4132(11) 0.121(6) Uiso 1 1 d . . . H57A H 0.2482 -0.0398 0.4094 0.146 Uiso 1 1 calc R . . H57B H 0.1892 0.0322 0.4471 0.146 Uiso 1 1 calc R . . C58 C 0.1824(15) 0.0621(14) 0.3281(12) 0.127(6) Uiso 1 1 d . . . H58B H 0.2048 0.1218 0.3155 0.152 Uiso 1 1 calc R . . H58A H 0.2237 0.0394 0.2859 0.152 Uiso 1 1 calc R . . C59 C 0.0805(11) 0.0655(11) 0.3313(9) 0.091(4) Uiso 1 1 d . . . H59A H 0.0738 0.0677 0.2793 0.109 Uiso 1 1 calc R . . H59B H 0.0468 0.1184 0.3420 0.109 Uiso 1 1 calc R . . C60 C 0.0387(12) -0.0161(11) 0.3985(9) 0.093(4) Uiso 1 1 d . . . H60A H -0.0261 -0.0028 0.4321 0.112 Uiso 1 1 calc R . . H60B H 0.0291 -0.0594 0.3766 0.112 Uiso 1 1 calc R . . C61 C 0.373(2) 0.2642(17) 0.2973(15) 0.161(9) Uiso 1 1 d . . . H61A H 0.3578 0.2869 0.3418 0.193 Uiso 1 1 calc R . . H61B H 0.3109 0.2612 0.2857 0.193 Uiso 1 1 calc R . . C62 C 0.4233(16) 0.1756(14) 0.3193(12) 0.129(6) Uiso 1 1 d . . . H62A H 0.4584 0.1680 0.3597 0.155 Uiso 1 1 calc R . . H62B H 0.3752 0.1276 0.3426 0.155 Uiso 1 1 calc R . . C63 C 0.4459(17) 0.3216(15) 0.2224(13) 0.134(7) Uiso 1 1 d . . . H63A H 0.4137 0.3557 0.1792 0.160 Uiso 1 1 calc R . . H63B H 0.4750 0.3637 0.2350 0.160 Uiso 1 1 calc R . . C64 C 0.519(2) 0.2629(18) 0.1971(16) 0.167(9) Uiso 1 1 d . . . H64A H 0.5829 0.2730 0.2021 0.201 Uiso 1 1 calc R . . H64B H 0.5274 0.2730 0.1395 0.201 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0391(11) 0.0301(11) 0.0309(9) -0.0137(8) -0.0123(8) 0.0034(8) Si2 0.0379(11) 0.0265(10) 0.0284(9) -0.0094(8) -0.0099(8) -0.0025(8) Si3 0.0347(11) 0.0294(11) 0.0326(9) -0.0126(8) -0.0063(8) 0.0006(8) Si4 0.0312(10) 0.0316(11) 0.0387(10) -0.0086(9) -0.0065(8) -0.0067(8) As1 0.0379(4) 0.0328(4) 0.0283(3) -0.0108(3) -0.0115(3) 0.0003(3) As2 0.0393(4) 0.0251(4) 0.0317(3) -0.0065(3) -0.0115(3) -0.0022(3) As3 0.0347(4) 0.0312(4) 0.0323(3) -0.0130(3) -0.0072(3) 0.0019(3) As4 0.0315(4) 0.0303(4) 0.0382(4) -0.0103(3) -0.0069(3) -0.0046(3) Pb1 0.03525(16) 0.03394(17) 0.03721(15) -0.01030(12) -0.00880(11) -0.00418(12) Pb2 0.03865(16) 0.03122(16) 0.03472(14) -0.01233(12) -0.00986(11) 0.00230(12) Pb3 0.04500(18) 0.03599(17) 0.03765(15) -0.01516(12) -0.01657(12) -0.00057(13) Pb4 0.04154(17) 0.02870(16) 0.03481(15) -0.00764(12) -0.00956(12) -0.00020(12) C1 0.052(5) 0.039(5) 0.047(4) -0.016(4) -0.016(4) -0.005(4) C2 0.089(10) 0.100(11) 0.113(10) -0.062(9) 0.017(8) -0.062(9) C3 0.096(9) 0.038(6) 0.108(9) -0.032(6) -0.044(8) 0.009(6) C4 0.156(15) 0.062(8) 0.094(9) -0.030(7) -0.074(10) -0.014(8) C5 0.054(5) 0.044(5) 0.033(4) -0.011(3) -0.018(4) 0.003(4) C6 0.056(7) 0.135(12) 0.040(5) 0.006(6) -0.002(5) 0.024(7) C7 0.094(10) 0.089(10) 0.070(7) -0.045(7) 0.030(6) -0.041(8) C8 0.066(7) 0.114(11) 0.043(5) -0.036(6) -0.011(5) -0.001(7) C9 0.039(4) 0.032(4) 0.044(4) -0.013(3) -0.015(3) 0.000(3) C10 0.042(4) 0.037(4) 0.045(4) -0.019(4) -0.019(3) 0.005(3) C11 0.050(5) 0.039(5) 0.052(5) -0.021(4) -0.010(4) 0.004(4) C12 0.045(5) 0.036(5) 0.062(5) -0.019(4) -0.025(4) 0.010(4) C13 0.060(6) 0.051(6) 0.055(5) -0.010(4) -0.033(5) 0.006(5) C14 0.057(6) 0.056(6) 0.056(5) -0.033(4) -0.029(4) 0.021(4) C15 0.050(5) 0.040(5) 0.032(4) -0.009(3) -0.010(3) -0.006(4) C16 0.060(6) 0.045(5) 0.042(4) 0.004(4) 0.001(4) -0.007(4) C17 0.061(6) 0.077(7) 0.042(4) -0.030(5) -0.006(4) -0.008(5) C18 0.042(5) 0.066(6) 0.042(4) -0.004(4) -0.005(4) 0.002(4) C19 0.042(4) 0.039(4) 0.032(3) -0.009(3) -0.015(3) -0.005(3) C20 0.048(5) 0.045(5) 0.048(4) -0.014(4) -0.026(4) 0.009(4) C21 0.044(5) 0.058(6) 0.044(4) -0.022(4) -0.010(4) 0.013(4) C22 0.047(5) 0.041(5) 0.053(5) -0.017(4) -0.018(4) -0.003(4) C23 0.041(4) 0.029(4) 0.040(4) -0.011(3) -0.018(3) -0.002(3) C24 0.066(6) 0.031(4) 0.063(5) -0.019(4) -0.032(5) 0.000(4) C25 0.068(6) 0.033(5) 0.084(7) -0.030(5) -0.032(5) 0.000(4) C26 0.055(6) 0.057(6) 0.063(5) -0.029(5) -0.020(4) -0.010(5) C27 0.047(5) 0.045(5) 0.039(4) -0.017(4) -0.008(3) -0.015(4) C28 0.046(4) 0.033(4) 0.030(3) -0.013(3) -0.006(3) -0.014(3) C29 0.040(4) 0.035(4) 0.052(4) -0.019(4) -0.012(4) -0.005(3) C30 0.067(7) 0.049(6) 0.078(6) -0.036(5) -0.025(5) -0.009(5) C31 0.086(8) 0.043(6) 0.068(6) -0.031(5) -0.001(5) -0.019(5) C32 0.061(6) 0.048(6) 0.092(7) -0.052(6) -0.002(5) -0.006(5) C33 0.040(4) 0.034(4) 0.047(4) -0.012(4) -0.014(3) 0.008(3) C34 0.051(5) 0.060(6) 0.038(4) -0.004(4) -0.014(4) 0.006(4) C35 0.044(5) 0.054(6) 0.059(5) -0.025(4) -0.024(4) 0.002(4) C36 0.045(5) 0.064(6) 0.056(5) -0.021(5) -0.014(4) 0.014(5) C37 0.040(4) 0.042(5) 0.030(3) -0.010(3) -0.006(3) -0.004(3) C38 0.062(6) 0.036(5) 0.035(4) -0.009(4) -0.009(4) -0.009(4) C39 0.089(8) 0.034(5) 0.043(4) -0.012(4) -0.020(5) 0.006(5) C40 0.059(6) 0.069(7) 0.036(4) -0.015(4) -0.002(4) -0.021(5) C41 0.051(5) 0.061(6) 0.032(4) -0.015(4) 0.000(4) -0.014(4) C42 0.050(5) 0.053(6) 0.040(4) -0.017(4) -0.013(4) 0.004(4) C43 0.042(5) 0.036(5) 0.062(5) -0.018(4) -0.011(4) -0.005(4) C44 0.089(8) 0.057(7) 0.080(7) -0.046(6) -0.027(6) 0.001(6) C45 0.061(7) 0.052(6) 0.111(9) -0.043(6) -0.031(6) 0.006(5) C46 0.053(6) 0.045(6) 0.101(8) -0.029(6) -0.013(6) -0.017(5) C47 0.047(5) 0.044(5) 0.039(4) -0.006(4) -0.001(4) -0.018(4) C48 0.100(9) 0.065(7) 0.042(5) -0.019(5) -0.004(5) -0.031(6) C49 0.062(7) 0.083(8) 0.060(6) -0.014(6) -0.002(5) -0.031(6) C50 0.075(7) 0.056(6) 0.052(5) -0.007(5) -0.025(5) 0.002(5) C51 0.037(4) 0.040(5) 0.043(4) -0.016(4) -0.007(3) -0.012(3) C52 0.040(5) 0.041(5) 0.066(5) -0.011(4) -0.012(4) -0.007(4) C53 0.054(6) 0.038(5) 0.066(6) -0.006(4) -0.019(5) 0.004(4) C54 0.047(5) 0.065(7) 0.057(5) -0.008(5) -0.019(4) 0.011(5) C55 0.040(5) 0.073(7) 0.089(7) -0.027(6) -0.024(5) -0.001(5) C56 0.032(4) 0.055(6) 0.087(7) -0.016(5) -0.023(5) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C9 1.900(8) . ? Si1 C1 1.900(10) . ? Si1 C5 1.921(9) . ? Si1 As1 2.358(2) . ? Si2 C23 1.911(9) . ? Si2 C15 1.921(8) . ? Si2 C19 1.922(8) . ? Si2 As2 2.352(2) . ? Si3 C37 1.914(7) . ? Si3 C29 1.917(9) . ? Si3 C33 1.924(8) . ? Si3 As3 2.351(2) . ? Si4 C51 1.883(9) . ? Si4 C43 1.929(10) . ? Si4 C47 1.934(9) . ? Si4 As4 2.353(2) . ? As1 Pb2 2.7984(12) . ? As1 Pb4 2.8077(11) . ? As1 Pb1 2.8363(14) . ? As2 Pb3 2.8026(11) . ? As2 Pb2 2.8035(13) . ? As2 Pb1 2.8055(11) . ? As3 Pb1 2.8077(11) . ? As3 Pb3 2.8113(12) . ? As3 Pb4 2.8217(14) . ? As4 Pb4 2.8005(12) . ? As4 Pb2 2.8120(11) . ? As4 Pb3 2.8144(13) . ? O1 C60 1.386(17) . ? O1 C57 1.40(2) . ? O2 C62 1.36(3) . ? O2 C64 1.43(3) . ? C1 C3 1.527(15) . ? C1 C2 1.533(15) . ? C1 C4 1.533(14) . ? C5 C7 1.514(16) . ? C5 C8 1.522(12) . ? C5 C6 1.524(14) . ? C9 C10 1.388(12) . ? C9 C14 1.389(11) . ? C10 C11 1.375(12) . ? C11 C12 1.385(12) . ? C12 C13 1.373(15) . ? C13 C14 1.394(13) . ? C15 C17 1.523(13) . ? C15 C18 1.524(13) . ? C15 C16 1.546(12) . ? C19 C22 1.532(12) . ? C19 C21 1.550(12) . ? C19 C20 1.554(10) . ? C23 C28 1.376(10) . ? C23 C24 1.430(12) . ? C24 C25 1.393(14) . ? C25 C26 1.395(14) . ? C26 C27 1.368(14) . ? C27 C28 1.397(12) . ? C29 C31 1.523(13) . ? C29 C30 1.536(13) . ? C29 C32 1.544(13) . ? C33 C34 1.519(11) . ? C33 C36 1.538(12) . ? C33 C35 1.542(13) . ? C37 C38 1.385(12) . ? C37 C42 1.400(12) . ? C38 C39 1.361(12) . ? C39 C40 1.404(15) . ? C40 C41 1.363(15) . ? C41 C42 1.361(12) . ? C43 C45 1.522(14) . ? C43 C44 1.530(14) . ? C43 C46 1.575(12) . ? C47 C48 1.517(15) . ? C47 C50 1.517(14) . ? C47 C49 1.542(13) . ? C51 C56 1.397(12) . ? C51 C52 1.399(12) . ? C52 C53 1.387(13) . ? C53 C54 1.378(15) . ? C54 C55 1.364(16) . ? C55 C56 1.370(14) . ? C57 C58 1.54(2) . ? C58 C59 1.43(2) . ? C59 C60 1.47(2) . ? C61 C62 1.49(3) . ? C61 C63 1.50(3) . ? C63 C64 1.41(3) . ? 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 C9 Si1 C1 108.8(4) . . ? C9 Si1 C5 109.1(4) . . ? C1 Si1 C5 115.7(4) . . ? C9 Si1 As1 106.4(3) . . ? C1 Si1 As1 109.2(3) . . ? C5 Si1 As1 107.1(3) . . ? C23 Si2 C15 110.3(4) . . ? C23 Si2 C19 108.8(4) . . ? C15 Si2 C19 114.9(4) . . ? C23 Si2 As2 105.7(2) . . ? C15 Si2 As2 108.8(3) . . ? C19 Si2 As2 107.8(3) . . ? C37 Si3 C29 108.9(4) . . ? C37 Si3 C33 109.5(4) . . ? C29 Si3 C33 115.5(4) . . ? C37 Si3 As3 107.6(3) . . ? C29 Si3 As3 108.1(3) . . ? C33 Si3 As3 107.0(3) . . ? C51 Si4 C43 110.3(4) . . ? C51 Si4 C47 108.1(4) . . ? C43 Si4 C47 115.5(4) . . ? C51 Si4 As4 107.0(3) . . ? C43 Si4 As4 107.5(3) . . ? C47 Si4 As4 108.0(3) . . ? Si1 As1 Pb2 119.39(7) . . ? Si1 As1 Pb4 111.16(7) . . ? Pb2 As1 Pb4 98.42(4) . . ? Si1 As1 Pb1 127.03(6) . . ? Pb2 As1 Pb1 97.85(4) . . ? Pb4 As1 Pb1 97.68(4) . . ? Si2 As2 Pb3 123.58(6) . . ? Si2 As2 Pb2 112.51(7) . . ? Pb3 As2 Pb2 97.99(4) . . ? Si2 As2 Pb1 119.49(7) . . ? Pb3 As2 Pb1 100.16(4) . . ? Pb2 As2 Pb1 98.45(4) . . ? Si3 As3 Pb1 115.59(7) . . ? Si3 As3 Pb3 119.40(6) . . ? Pb1 As3 Pb3 99.90(3) . . ? Si3 As3 Pb4 121.04(6) . . ? Pb1 As3 Pb4 98.02(4) . . ? Pb3 As3 Pb4 98.69(4) . . ? Si4 As4 Pb4 118.15(6) . . ? Si4 As4 Pb2 120.02(7) . . ? Pb4 As4 Pb2 98.27(3) . . ? Si4 As4 Pb3 119.24(7) . . ? Pb4 As4 Pb3 99.12(4) . . ? Pb2 As4 Pb3 97.52(4) . . ? As2 Pb1 As3 79.40(3) . . ? As2 Pb1 As1 80.80(4) . . ? As3 Pb1 As1 81.14(4) . . ? As1 Pb2 As2 81.49(4) . . ? As1 Pb2 As4 81.14(3) . . ? As2 Pb2 As4 81.35(4) . . ? As2 Pb3 As3 79.40(3) . . ? As2 Pb3 As4 81.32(4) . . ? As3 Pb3 As4 80.39(4) . . ? As4 Pb4 As1 81.18(3) . . ? As4 Pb4 As3 80.45(4) . . ? As1 Pb4 As3 81.40(4) . . ? C60 O1 C57 111.8(12) . . ? C62 O2 C64 108(2) . . ? C3 C1 C2 106.5(10) . . ? C3 C1 C4 107.3(10) . . ? C2 C1 C4 107.8(11) . . ? C3 C1 Si1 111.7(7) . . ? C2 C1 Si1 108.8(7) . . ? C4 C1 Si1 114.3(7) . . ? C7 C5 C8 108.0(9) . . ? C7 C5 C6 107.9(11) . . ? C8 C5 C6 106.4(10) . . ? C7 C5 Si1 108.8(7) . . ? C8 C5 Si1 113.6(7) . . ? C6 C5 Si1 111.9(6) . . ? C10 C9 C14 116.4(8) . . ? C10 C9 Si1 121.6(6) . . ? C14 C9 Si1 122.0(7) . . ? C11 C10 C9 122.4(8) . . ? C10 C11 C12 119.9(9) . . ? C13 C12 C11 119.7(8) . . ? C12 C13 C14 119.4(8) . . ? C9 C14 C13 122.2(9) . . ? C17 C15 C18 108.3(9) . . ? C17 C15 C16 108.5(8) . . ? C18 C15 C16 107.9(8) . . ? C17 C15 Si2 110.5(6) . . ? C18 C15 Si2 109.3(5) . . ? C16 C15 Si2 112.2(7) . . ? C22 C19 C21 106.8(7) . . ? C22 C19 C20 108.5(7) . . ? C21 C19 C20 107.7(7) . . ? C22 C19 Si2 111.8(6) . . ? C21 C19 Si2 108.9(5) . . ? C20 C19 Si2 112.8(6) . . ? C28 C23 C24 117.1(8) . . ? C28 C23 Si2 123.1(6) . . ? C24 C23 Si2 119.8(6) . . ? C25 C24 C23 120.2(8) . . ? C24 C25 C26 121.0(9) . . ? C27 C26 C25 118.7(9) . . ? C26 C27 C28 121.0(8) . . ? C23 C28 C27 122.0(8) . . ? C31 C29 C30 107.2(8) . . ? C31 C29 C32 109.3(8) . . ? C30 C29 C32 108.2(8) . . ? C31 C29 Si3 111.3(7) . . ? C30 C29 Si3 107.8(6) . . ? C32 C29 Si3 112.8(6) . . ? C34 C33 C36 109.0(7) . . ? C34 C33 C35 107.7(8) . . ? C36 C33 C35 106.4(8) . . ? C34 C33 Si3 111.1(6) . . ? C36 C33 Si3 113.5(6) . . ? C35 C33 Si3 108.8(5) . . ? C38 C37 C42 116.4(7) . . ? C38 C37 Si3 122.2(7) . . ? C42 C37 Si3 121.3(7) . . ? C39 C38 C37 122.2(9) . . ? C38 C39 C40 120.0(9) . . ? C41 C40 C39 118.3(8) . . ? C42 C41 C40 121.3(9) . . ? C41 C42 C37 121.7(9) . . ? C45 C43 C44 108.5(9) . . ? C45 C43 C46 107.2(8) . . ? C44 C43 C46 108.4(9) . . ? C45 C43 Si4 111.6(7) . . ? C44 C43 Si4 107.6(6) . . ? C46 C43 Si4 113.4(7) . . ? C48 C47 C50 107.8(9) . . ? C48 C47 C49 108.4(9) . . ? C50 C47 C49 108.8(8) . . ? C48 C47 Si4 108.4(6) . . ? C50 C47 Si4 112.5(7) . . ? C49 C47 Si4 111.0(7) . . ? C56 C51 C52 115.3(8) . . ? C56 C51 Si4 122.7(7) . . ? C52 C51 Si4 121.9(6) . . ? C53 C52 C51 122.6(9) . . ? C54 C53 C52 119.1(9) . . ? C55 C54 C53 120.1(9) . . ? C54 C55 C56 120.2(10) . . ? C55 C56 C51 122.7(10) . . ? O1 C57 C58 104.0(15) . . ? C59 C58 C57 105.5(16) . . ? C58 C59 C60 105.4(14) . . ? O1 C60 C59 108.2(14) . . ? C62 C61 C63 104(2) . . ? O2 C62 C61 105.4(19) . . ? C64 C63 C61 106(2) . . ? C63 C64 O2 108(2) . . ? 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 C9 Si1 As1 Pb2 -163.7(3) . . . . ? C1 Si1 As1 Pb2 79.0(3) . . . . ? C5 Si1 As1 Pb2 -47.1(3) . . . . ? C9 Si1 As1 Pb4 -50.2(3) . . . . ? C1 Si1 As1 Pb4 -167.6(3) . . . . ? C5 Si1 As1 Pb4 66.4(3) . . . . ? C9 Si1 As1 Pb1 67.9(3) . . . . ? C1 Si1 As1 Pb1 -49.4(3) . . . . ? C5 Si1 As1 Pb1 -175.4(3) . . . . ? C23 Si2 As2 Pb3 -173.4(3) . . . . ? C15 Si2 As2 Pb3 68.1(3) . . . . ? C19 Si2 As2 Pb3 -57.2(3) . . . . ? C23 Si2 As2 Pb2 -56.3(3) . . . . ? C15 Si2 As2 Pb2 -174.8(3) . . . . ? C19 Si2 As2 Pb2 59.9(3) . . . . ? C23 Si2 As2 Pb1 58.3(3) . . . . ? C15 Si2 As2 Pb1 -60.2(3) . . . . ? C19 Si2 As2 Pb1 174.6(3) . . . . ? C37 Si3 As3 Pb1 50.7(3) . . . . ? C29 Si3 As3 Pb1 168.1(3) . . . . ? C33 Si3 As3 Pb1 -66.9(3) . . . . ? C37 Si3 As3 Pb3 -68.6(3) . . . . ? C29 Si3 As3 Pb3 48.9(3) . . . . ? C33 Si3 As3 Pb3 173.9(3) . . . . ? C37 Si3 As3 Pb4 168.6(3) . . . . ? C29 Si3 As3 Pb4 -73.9(3) . . . . ? C33 Si3 As3 Pb4 51.1(3) . . . . ? C51 Si4 As4 Pb4 -176.3(3) . . . . ? C43 Si4 As4 Pb4 65.1(3) . . . . ? C47 Si4 As4 Pb4 -60.1(3) . . . . ? C51 Si4 As4 Pb2 -56.5(3) . . . . ? C43 Si4 As4 Pb2 -175.0(3) . . . . ? C47 Si4 As4 Pb2 59.7(3) . . . . ? C51 Si4 As4 Pb3 63.3(3) . . . . ? C43 Si4 As4 Pb3 -55.3(3) . . . . ? C47 Si4 As4 Pb3 179.5(3) . . . . ? Si2 As2 Pb1 As3 146.46(7) . . . . ? Pb3 As2 Pb1 As3 8.14(2) . . . . ? Pb2 As2 Pb1 As3 -91.61(4) . . . . ? Si2 As2 Pb1 As1 -130.91(8) . . . . ? Pb3 As2 Pb1 As1 90.77(4) . . . . ? Pb2 As2 Pb1 As1 -8.99(3) . . . . ? Si3 As3 Pb1 As2 -137.61(6) . . . . ? Pb3 As3 Pb1 As2 -8.11(2) . . . . ? Pb4 As3 Pb1 As2 92.23(4) . . . . ? Si3 As3 Pb1 As1 140.18(7) . . . . ? Pb3 As3 Pb1 As1 -90.32(4) . . . . ? Pb4 As3 Pb1 As1 10.02(2) . . . . ? Si1 As1 Pb1 As2 145.42(8) . . . . ? Pb2 As1 Pb1 As2 8.99(3) . . . . ? Pb4 As1 Pb1 As2 -90.67(4) . . . . ? Si1 As1 Pb1 As3 -133.98(8) . . . . ? Pb2 As1 Pb1 As3 89.60(3) . . . . ? Pb4 As1 Pb1 As3 -10.06(2) . . . . ? Si1 As1 Pb2 As2 -149.82(7) . . . . ? Pb4 As1 Pb2 As2 90.04(4) . . . . ? Pb1 As1 Pb2 As2 -8.98(3) . . . . ? Si1 As1 Pb2 As4 127.69(8) . . . . ? Pb4 As1 Pb2 As4 7.54(2) . . . . ? Pb1 As1 Pb2 As4 -91.48(4) . . . . ? Si2 As2 Pb2 As1 135.99(7) . . . . ? Pb3 As2 Pb2 As1 -92.50(3) . . . . ? Pb1 As2 Pb2 As1 9.10(3) . . . . ? Si2 As2 Pb2 As4 -141.76(7) . . . . ? Pb3 As2 Pb2 As4 -10.25(2) . . . . ? Pb1 As2 Pb2 As4 91.35(4) . . . . ? Si4 As4 Pb2 As1 -136.96(7) . . . . ? Pb4 As4 Pb2 As1 -7.56(2) . . . . ? Pb3 As4 Pb2 As1 92.86(4) . . . . ? Si4 As4 Pb2 As2 140.38(7) . . . . ? Pb4 As4 Pb2 As2 -90.22(4) . . . . ? Pb3 As4 Pb2 As2 10.19(2) . . . . ? Si2 As2 Pb3 As3 -144.13(8) . . . . ? Pb2 As2 Pb3 As3 92.00(4) . . . . ? Pb1 As2 Pb3 As3 -8.13(2) . . . . ? Si2 As2 Pb3 As4 134.11(8) . . . . ? Pb2 As2 Pb3 As4 10.24(2) . . . . ? Pb1 As2 Pb3 As4 -89.90(4) . . . . ? Si3 As3 Pb3 As2 135.10(7) . . . . ? Pb1 As3 Pb3 As2 8.12(2) . . . . ? Pb4 As3 Pb3 As2 -91.67(4) . . . . ? Si3 As3 Pb3 As4 -142.02(7) . . . . ? Pb1 As3 Pb3 As4 91.00(4) . . . . ? Pb4 As3 Pb3 As4 -8.79(3) . . . . ? Si4 As4 Pb3 As2 -140.91(8) . . . . ? Pb4 As4 Pb3 As2 89.49(3) . . . . ? Pb2 As4 Pb3 As2 -10.20(2) . . . . ? Si4 As4 Pb3 As3 138.47(8) . . . . ? Pb4 As4 Pb3 As3 8.87(3) . . . . ? Pb2 As4 Pb3 As3 -90.82(4) . . . . ? Si4 As4 Pb4 As1 138.17(8) . . . . ? Pb2 As4 Pb4 As1 7.53(2) . . . . ? Pb3 As4 Pb4 As1 -91.51(4) . . . . ? Si4 As4 Pb4 As3 -139.15(8) . . . . ? Pb2 As4 Pb4 As3 90.22(4) . . . . ? Pb3 As4 Pb4 As3 -8.83(3) . . . . ? Si1 As1 Pb4 As4 -133.67(7) . . . . ? Pb2 As1 Pb4 As4 -7.57(2) . . . . ? Pb1 As1 Pb4 As4 91.59(4) . . . . ? Si1 As1 Pb4 As3 144.74(7) . . . . ? Pb2 As1 Pb4 As3 -89.16(4) . . . . ? Pb1 As1 Pb4 As3 10.01(2) . . . . ? Si3 As3 Pb4 As4 141.02(8) . . . . ? Pb1 As3 Pb4 As4 -92.54(3) . . . . ? Pb3 As3 Pb4 As4 8.83(3) . . . . ? Si3 As3 Pb4 As1 -136.56(8) . . . . ? Pb1 As3 Pb4 As1 -10.12(2) . . . . ? Pb3 As3 Pb4 As1 91.25(4) . . . . ? C9 Si1 C1 C3 -178.8(8) . . . . ? C5 Si1 C1 C3 58.0(8) . . . . ? As1 Si1 C1 C3 -62.9(8) . . . . ? C9 Si1 C1 C2 -61.4(9) . . . . ? C5 Si1 C1 C2 175.3(9) . . . . ? As1 Si1 C1 C2 54.4(9) . . . . ? C9 Si1 C1 C4 59.1(10) . . . . ? C5 Si1 C1 C4 -64.1(10) . . . . ? As1 Si1 C1 C4 175.0(9) . . . . ? C9 Si1 C5 C7 46.2(9) . . . . ? C1 Si1 C5 C7 169.3(8) . . . . ? As1 Si1 C5 C7 -68.7(8) . . . . ? C9 Si1 C5 C8 -74.1(9) . . . . ? C1 Si1 C5 C8 49.0(9) . . . . ? As1 Si1 C5 C8 171.0(7) . . . . ? C9 Si1 C5 C6 165.3(9) . . . . ? C1 Si1 C5 C6 -71.6(10) . . . . ? As1 Si1 C5 C6 50.5(10) . . . . ? C1 Si1 C9 C10 106.9(7) . . . . ? C5 Si1 C9 C10 -126.0(7) . . . . ? As1 Si1 C9 C10 -10.7(7) . . . . ? C1 Si1 C9 C14 -72.7(8) . . . . ? C5 Si1 C9 C14 54.4(9) . . . . ? As1 Si1 C9 C14 169.7(7) . . . . ? C14 C9 C10 C11 -1.3(13) . . . . ? Si1 C9 C10 C11 179.1(7) . . . . ? C9 C10 C11 C12 0.9(14) . . . . ? C10 C11 C12 C13 0.8(14) . . . . ? C11 C12 C13 C14 -1.9(15) . . . . ? C10 C9 C14 C13 0.1(14) . . . . ? Si1 C9 C14 C13 179.7(8) . . . . ? C12 C13 C14 C9 1.5(16) . . . . ? C23 Si2 C15 C17 171.8(6) . . . . ? C19 Si2 C15 C17 48.3(8) . . . . ? As2 Si2 C15 C17 -72.7(7) . . . . ? C23 Si2 C15 C18 -69.1(8) . . . . ? C19 Si2 C15 C18 167.3(7) . . . . ? As2 Si2 C15 C18 46.4(8) . . . . ? C23 Si2 C15 C16 50.5(8) . . . . ? C19 Si2 C15 C16 -73.0(8) . . . . ? As2 Si2 C15 C16 166.0(6) . . . . ? C23 Si2 C19 C22 158.2(5) . . . . ? C15 Si2 C19 C22 -77.4(6) . . . . ? As2 Si2 C19 C22 44.1(6) . . . . ? C23 Si2 C19 C21 40.4(7) . . . . ? C15 Si2 C19 C21 164.7(6) . . . . ? As2 Si2 C19 C21 -73.8(6) . . . . ? C23 Si2 C19 C20 -79.1(7) . . . . ? C15 Si2 C19 C20 45.2(8) . . . . ? As2 Si2 C19 C20 166.7(6) . . . . ? C15 Si2 C23 C28 114.7(7) . . . . ? C19 Si2 C23 C28 -118.3(7) . . . . ? As2 Si2 C23 C28 -2.8(8) . . . . ? C15 Si2 C23 C24 -67.0(8) . . . . ? C19 Si2 C23 C24 60.0(8) . . . . ? As2 Si2 C23 C24 175.5(7) . . . . ? C28 C23 C24 C25 0.6(14) . . . . ? Si2 C23 C24 C25 -177.8(8) . . . . ? C23 C24 C25 C26 0.1(16) . . . . ? C24 C25 C26 C27 -1.4(16) . . . . ? C25 C26 C27 C28 2.1(14) . . . . ? C24 C23 C28 C27 0.1(12) . . . . ? Si2 C23 C28 C27 178.4(6) . . . . ? C26 C27 C28 C23 -1.5(13) . . . . ? C37 Si3 C29 C31 161.1(7) . . . . ? C33 Si3 C29 C31 -75.3(8) . . . . ? As3 Si3 C29 C31 44.5(7) . . . . ? C37 Si3 C29 C30 43.7(7) . . . . ? C33 Si3 C29 C30 167.4(6) . . . . ? As3 Si3 C29 C30 -72.8(7) . . . . ? C37 Si3 C29 C32 -75.7(7) . . . . ? C33 Si3 C29 C32 48.0(8) . . . . ? As3 Si3 C29 C32 167.8(6) . . . . ? C37 Si3 C33 C34 174.6(7) . . . . ? C29 Si3 C33 C34 51.3(8) . . . . ? As3 Si3 C33 C34 -69.1(7) . . . . ? C37 Si3 C33 C36 51.3(8) . . . . ? C29 Si3 C33 C36 -72.0(8) . . . . ? As3 Si3 C33 C36 167.6(6) . . . . ? C37 Si3 C33 C35 -67.0(7) . . . . ? C29 Si3 C33 C35 169.8(6) . . . . ? As3 Si3 C33 C35 49.3(6) . . . . ? C29 Si3 C37 C38 -109.7(8) . . . . ? C33 Si3 C37 C38 123.1(8) . . . . ? As3 Si3 C37 C38 7.2(8) . . . . ? C29 Si3 C37 C42 65.8(8) . . . . ? C33 Si3 C37 C42 -61.3(8) . . . . ? As3 Si3 C37 C42 -177.2(7) . . . . ? C42 C37 C38 C39 2.0(14) . . . . ? Si3 C37 C38 C39 177.8(8) . . . . ? C37 C38 C39 C40 -0.1(16) . . . . ? C38 C39 C40 C41 -1.6(16) . . . . ? C39 C40 C41 C42 1.3(15) . . . . ? C40 C41 C42 C37 0.7(15) . . . . ? C38 C37 C42 C41 -2.3(14) . . . . ? Si3 C37 C42 C41 -178.1(7) . . . . ? C51 Si4 C43 C45 -159.6(7) . . . . ? C47 Si4 C43 C45 77.5(8) . . . . ? As4 Si4 C43 C45 -43.2(8) . . . . ? C51 Si4 C43 C44 -40.6(8) . . . . ? C47 Si4 C43 C44 -163.6(7) . . . . ? As4 Si4 C43 C44 75.8(7) . . . . ? C51 Si4 C43 C46 79.3(8) . . . . ? C47 Si4 C43 C46 -43.7(8) . . . . ? As4 Si4 C43 C46 -164.3(6) . . . . ? C51 Si4 C47 C48 61.9(8) . . . . ? C43 Si4 C47 C48 -174.0(7) . . . . ? As4 Si4 C47 C48 -53.6(8) . . . . ? C51 Si4 C47 C50 -179.1(7) . . . . ? C43 Si4 C47 C50 -55.0(8) . . . . ? As4 Si4 C47 C50 65.4(7) . . . . ? C51 Si4 C47 C49 -57.0(9) . . . . ? C43 Si4 C47 C49 67.1(9) . . . . ? As4 Si4 C47 C49 -172.5(7) . . . . ? C43 Si4 C51 C56 -47.0(9) . . . . ? C47 Si4 C51 C56 80.2(9) . . . . ? As4 Si4 C51 C56 -163.7(8) . . . . ? C43 Si4 C51 C52 134.3(8) . . . . ? C47 Si4 C51 C52 -98.5(8) . . . . ? As4 Si4 C51 C52 17.5(9) . . . . ? C56 C51 C52 C53 -0.9(16) . . . . ? Si4 C51 C52 C53 177.9(9) . . . . ? C51 C52 C53 C54 0.7(18) . . . . ? C52 C53 C54 C55 0.1(18) . . . . ? C53 C54 C55 C56 -0.5(19) . . . . ? C54 C55 C56 C51 0(2) . . . . ? C52 C51 C56 C55 0.5(17) . . . . ? Si4 C51 C56 C55 -178.3(10) . . . . ? C60 O1 C57 C58 -11(2) . . . . ? O1 C57 C58 C59 21(2) . . . . ? C57 C58 C59 C60 -22(2) . . . . ? C57 O1 C60 C59 -3(2) . . . . ? C58 C59 C60 O1 16(2) . . . . ? C64 O2 C62 C61 30(3) . . . . ? C63 C61 C62 O2 -26(3) . . . . ? C62 C61 C63 C64 12(3) . . . . ? C61 C63 C64 O2 5(3) . . . . ? C62 O2 C64 C63 -23(3) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.386 _refine_diff_density_min -2.817 _refine_diff_density_rms 0.204 # Attachment 'Pb4P4.CIF' data_e:\traut\crystal\st107\neu\p-1 _database_code_depnum_ccdc_archive 'CCDC 751817' #TrackingRef 'Pb4P4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H92 P4 Pb4 Si4' _chemical_formula_weight 1830.30 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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 14.187(3) _cell_length_b 15.491(3) _cell_length_c 15.998(3) _cell_angle_alpha 73.32(3) _cell_angle_beta 84.69(3) _cell_angle_gamma 80.68(3) _cell_volume 3319.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.3548 _exptl_crystal_size_mid 0.3144 _exptl_crystal_size_min 0.1177 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 10.313 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0545 _exptl_absorpt_correction_T_max 0.4026 _exptl_absorpt_process_details ? _exptl_special_details ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 19 0 1 0.1688 21 20 7 0.1810 19 18 24 0.1470 7 0 8 0.2667 23 -30 22 0.3167 3 -4 -1 0.2248 16 -21 -26 0.0528 24 0 -25 0.1562 21 20 -13 0.2206 4 27 8 0.1668 1 7 9 0.0609 0 0 1 0.2531 -3 -20 14 0.3124 -19 0 -1 0.1512 -21 -20 -7 0.1448 -19 -18 -24 0.1301 -7 0 -8 0.2134 -23 30 -22 0.2583 -3 4 1 0.1657 -16 21 26 0.0603 -24 0 25 0.1238 -21 -20 13 0.2092 -4 -27 -8 0.1962 -1 -7 -9 0.0533 0 0 -1 0.2296 3 20 -14 0.2762 ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15043 _diffrn_reflns_av_R_equivalents 0.1194 _diffrn_reflns_av_sigmaI/netI 0.1019 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8256 _reflns_number_gt 7323 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1492P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8256 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2033 _refine_ls_wR_factor_gt 0.1987 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.8294(3) 0.7836(2) 0.0475(2) 0.0379(8) Uani 1 1 d . . . P2 P 0.7569(3) 0.5950(2) 0.2091(2) 0.0391(8) Uani 1 1 d . . . P3 P 0.9729(3) 0.6736(2) 0.2287(2) 0.0391(8) Uani 1 1 d . . . P4 P 0.7469(3) 0.8095(2) 0.2582(2) 0.0413(9) Uani 1 1 d . . . Pb1 Pb 0.91798(4) 0.60785(3) 0.10184(3) 0.0418(2) Uani 1 1 d . . . Pb2 Pb 0.82251(4) 0.63576(4) 0.34555(3) 0.0436(2) Uani 1 1 d . . . Pb3 Pb 0.65846(4) 0.76314(3) 0.13612(3) 0.0409(2) Uani 1 1 d . . . Pb4 Pb 0.90888(4) 0.85402(3) 0.15748(3) 0.0405(2) Uani 1 1 d . . . Si1 Si 0.8322(3) 0.8585(2) -0.0942(2) 0.0376(8) Uani 1 1 d . . . Si2 Si 0.6850(3) 0.4694(2) 0.2385(2) 0.0379(8) Uani 1 1 d . . . Si3 Si 1.1204(3) 0.6388(3) 0.2793(2) 0.0402(9) Uani 1 1 d . . . Si4 Si 0.6624(3) 0.9040(3) 0.3306(3) 0.0425(9) Uani 1 1 d . . . C1 C 0.7636(10) 0.9782(8) -0.1081(8) 0.039(3) Uani 1 1 d . . . C2 C 0.8235(12) 1.0410(10) -0.0845(11) 0.052(4) Uani 1 1 d . . . H2C H 0.7862 1.1016 -0.0925 0.062 Uiso 1 1 calc R . . H2B H 0.8817 1.0455 -0.1226 0.062 Uiso 1 1 calc R . . H2A H 0.8407 1.0159 -0.0235 0.062 Uiso 1 1 calc R . . C3 C 0.6730(13) 0.9721(12) -0.0514(13) 0.069(5) Uani 1 1 d . . . H3C H 0.6375 1.0333 -0.0581 0.082 Uiso 1 1 calc R . . H3B H 0.6887 0.9446 0.0098 0.082 Uiso 1 1 calc R . . H3A H 0.6336 0.9344 -0.0690 0.082 Uiso 1 1 calc R . . C4 C 0.7342(12) 1.0225(11) -0.2037(11) 0.058(4) Uani 1 1 d . . . H4C H 0.6995 1.0838 -0.2089 0.070 Uiso 1 1 calc R . . H4B H 0.6930 0.9853 -0.2196 0.070 Uiso 1 1 calc R . . H4A H 0.7917 1.0265 -0.2428 0.070 Uiso 1 1 calc R . . C5 C 0.9620(10) 0.8524(10) -0.1356(9) 0.048(4) Uani 1 1 d . . . C6 C 1.0249(10) 0.8745(10) -0.0720(10) 0.049(4) Uani 1 1 d . . . H6C H 1.0916 0.8705 -0.0945 0.059 Uiso 1 1 calc R . . H6B H 1.0201 0.8307 -0.0143 0.059 Uiso 1 1 calc R . . H6A H 1.0026 0.9362 -0.0671 0.059 Uiso 1 1 calc R . . C7 C 0.9804(13) 0.9195(11) -0.2249(10) 0.057(4) Uani 1 1 d . . . H7C H 1.0488 0.9114 -0.2417 0.069 Uiso 1 1 calc R . . H7B H 0.9604 0.9820 -0.2212 0.069 Uiso 1 1 calc R . . H7A H 0.9439 0.9081 -0.2687 0.069 Uiso 1 1 calc R . . C8 C 0.9997(14) 0.7561(11) -0.1440(10) 0.064(5) Uani 1 1 d . . . H8C H 1.0668 0.7535 -0.1657 0.077 Uiso 1 1 calc R . . H8B H 0.9615 0.7418 -0.1850 0.077 Uiso 1 1 calc R . . H8A H 0.9950 0.7117 -0.0867 0.077 Uiso 1 1 calc R . . C9 C 0.7626(11) 0.8013(9) -0.1514(9) 0.042(3) Uani 1 1 d . . . C10 C 0.7043(14) 0.7376(14) -0.1060(13) 0.074(5) Uani 1 1 d . . . H10A H 0.7045 0.7180 -0.0440 0.089 Uiso 1 1 calc R . . C11 C 0.6447(16) 0.7009(14) -0.1488(14) 0.081(6) Uani 1 1 d . . . H11A H 0.6005 0.6623 -0.1164 0.097 Uiso 1 1 calc R . . C12 C 0.6524(14) 0.7227(13) -0.2398(11) 0.067(5) Uani 1 1 d . . . H12A H 0.6157 0.6959 -0.2697 0.080 Uiso 1 1 calc R . . C13 C 0.7130(15) 0.7830(13) -0.2870(11) 0.072(6) Uani 1 1 d . . . H13A H 0.7153 0.7997 -0.3490 0.087 Uiso 1 1 calc R . . C14 C 0.7693(15) 0.8184(12) -0.2447(12) 0.070(5) Uani 1 1 d . . . H14A H 0.8144 0.8555 -0.2779 0.083 Uiso 1 1 calc R . . C15 C 0.6453(11) 0.4586(10) 0.1312(10) 0.048(4) Uani 1 1 d . . . C16 C 0.6100(14) 0.3709(12) 0.1402(11) 0.064(5) Uani 1 1 d . . . H16C H 0.5910 0.3695 0.0833 0.077 Uiso 1 1 calc R . . H16B H 0.5549 0.3649 0.1821 0.077 Uiso 1 1 calc R . . H16A H 0.6611 0.3203 0.1612 0.077 Uiso 1 1 calc R . . C17 C 0.7281(16) 0.4668(16) 0.0645(12) 0.081(6) Uani 1 1 d . . . H17C H 0.7079 0.4611 0.0096 0.097 Uiso 1 1 calc R . . H17B H 0.7809 0.4185 0.0863 0.097 Uiso 1 1 calc R . . H17A H 0.7494 0.5263 0.0543 0.097 Uiso 1 1 calc R . . C18 C 0.5641(16) 0.5362(13) 0.0940(14) 0.086(7) Uani 1 1 d . . . H18C H 0.5446 0.5295 0.0392 0.104 Uiso 1 1 calc R . . H18B H 0.5870 0.5951 0.0828 0.104 Uiso 1 1 calc R . . H18A H 0.5093 0.5332 0.1362 0.104 Uiso 1 1 calc R . . C19 C 0.5822(11) 0.4795(11) 0.3244(11) 0.052(4) Uani 1 1 d . . . C20 C 0.5258(16) 0.5738(14) 0.3069(13) 0.080(6) Uani 1 1 d . . . H20C H 0.4749 0.5749 0.3526 0.096 Uiso 1 1 calc R . . H20B H 0.4975 0.5902 0.2499 0.096 Uiso 1 1 calc R . . H20A H 0.5684 0.6177 0.3070 0.096 Uiso 1 1 calc R . . C21 C 0.6261(13) 0.4570(15) 0.4146(12) 0.073(5) Uani 1 1 d . . . H21C H 0.5749 0.4616 0.4593 0.087 Uiso 1 1 calc R . . H21B H 0.6701 0.5003 0.4126 0.087 Uiso 1 1 calc R . . H21A H 0.6610 0.3951 0.4288 0.087 Uiso 1 1 calc R . . C22 C 0.5131(13) 0.4107(11) 0.3369(14) 0.069(5) Uani 1 1 d . . . H22C H 0.4634 0.4196 0.3816 0.083 Uiso 1 1 calc R . . H22B H 0.5480 0.3489 0.3554 0.083 Uiso 1 1 calc R . . H22A H 0.4834 0.4192 0.2816 0.083 Uiso 1 1 calc R . . C23 C 0.7724(12) 0.3667(10) 0.2887(10) 0.052(4) Uani 1 1 d . . . C24 C 0.7508(13) 0.2785(10) 0.3189(11) 0.058(4) Uani 1 1 d . . . H24A H 0.6885 0.2681 0.3107 0.070 Uiso 1 1 calc R . . C25 C 0.8142(13) 0.2061(10) 0.3598(11) 0.061(4) Uani 1 1 d . . . H25A H 0.7952 0.1472 0.3801 0.073 Uiso 1 1 calc R . . C26 C 0.9061(13) 0.2179(12) 0.3717(11) 0.062(5) Uani 1 1 d . . . H26A H 0.9512 0.1674 0.3989 0.075 Uiso 1 1 calc R . . C27 C 0.9302(11) 0.3020(10) 0.3442(10) 0.049(4) Uani 1 1 d . . . H27A H 0.9922 0.3115 0.3543 0.059 Uiso 1 1 calc R . . C28 C 0.8674(10) 0.3743(10) 0.3019(10) 0.048(4) Uani 1 1 d . . . H28A H 0.8885 0.4322 0.2804 0.057 Uiso 1 1 calc R . . C29 C 1.1521(12) 0.5099(10) 0.3129(12) 0.058(4) Uani 1 1 d . . . C30 C 1.1369(14) 0.4717(11) 0.2382(12) 0.071(5) Uani 1 1 d . . . H30C H 1.1539 0.4053 0.2561 0.086 Uiso 1 1 calc R . . H30B H 1.1773 0.4978 0.1870 0.086 Uiso 1 1 calc R . . H30A H 1.0696 0.4874 0.2233 0.086 Uiso 1 1 calc R . . C31 C 1.0948(13) 0.4667(11) 0.3911(12) 0.066(5) Uani 1 1 d . . . H31C H 1.1134 0.4006 0.4066 0.079 Uiso 1 1 calc R . . H31B H 1.0268 0.4815 0.3788 0.079 Uiso 1 1 calc R . . H31A H 1.1061 0.4896 0.4399 0.079 Uiso 1 1 calc R . . C32 C 1.2606(12) 0.4797(12) 0.3347(13) 0.070(5) Uani 1 1 d . . . H32C H 1.2745 0.4131 0.3518 0.083 Uiso 1 1 calc R . . H32B H 1.2738 0.5026 0.3830 0.083 Uiso 1 1 calc R . . H32A H 1.3009 0.5046 0.2831 0.083 Uiso 1 1 calc R . . C33 C 1.1216(11) 0.6962(12) 0.3717(10) 0.055(4) Uani 1 1 d . . . C34 C 1.0276(15) 0.6883(17) 0.4282(12) 0.086(6) Uani 1 1 d . . . H34C H 1.0282 0.7183 0.4743 0.103 Uiso 1 1 calc R . . H34B H 1.0214 0.6239 0.4546 0.103 Uiso 1 1 calc R . . H34A H 0.9733 0.7177 0.3915 0.103 Uiso 1 1 calc R . . C35 C 1.1248(14) 0.7996(12) 0.3298(12) 0.069(5) Uani 1 1 d . . . H35C H 1.1254 0.8295 0.3760 0.082 Uiso 1 1 calc R . . H35B H 1.0683 0.8265 0.2954 0.082 Uiso 1 1 calc R . . H35A H 1.1827 0.8079 0.2917 0.082 Uiso 1 1 calc R . . C36 C 1.2048(16) 0.6554(14) 0.4318(12) 0.080(6) Uani 1 1 d . . . H36C H 1.2017 0.6881 0.4763 0.097 Uiso 1 1 calc R . . H36B H 1.2655 0.6611 0.3973 0.097 Uiso 1 1 calc R . . H36A H 1.2007 0.5910 0.4602 0.097 Uiso 1 1 calc R . . C37 C 1.2076(11) 0.6866(10) 0.1844(10) 0.048(4) Uani 1 1 d . . . C38 C 1.1864(11) 0.7031(10) 0.0977(9) 0.046(3) Uani 1 1 d . . . H38A H 1.1253 0.6935 0.0853 0.055 Uiso 1 1 calc R . . C39 C 1.2487(12) 0.7319(11) 0.0306(11) 0.056(4) Uani 1 1 d . . . H39A H 1.2304 0.7425 -0.0276 0.067 Uiso 1 1 calc R . . C40 C 1.3379(12) 0.7460(10) 0.0445(11) 0.054(4) Uani 1 1 d . . . H40A H 1.3820 0.7658 -0.0029 0.065 Uiso 1 1 calc R . . C41 C 1.3617(10) 0.7306(9) 0.1304(12) 0.052(4) Uani 1 1 d . . . H41A H 1.4225 0.7415 0.1419 0.063 Uiso 1 1 calc R . . C42 C 1.2984(11) 0.6995(10) 0.1996(10) 0.049(4) Uani 1 1 d . . . H42A H 1.3171 0.6869 0.2579 0.059 Uiso 1 1 calc R . . C43 C 0.6229(10) 1.0223(10) 0.2474(10) 0.048(4) Uani 1 1 d . . . C44 C 0.5550(15) 1.0171(15) 0.1826(15) 0.086(7) Uani 1 1 d . . . H44C H 0.5384 1.0777 0.1424 0.103 Uiso 1 1 calc R . . H44B H 0.4969 0.9953 0.2138 0.103 Uiso 1 1 calc R . . H44A H 0.5856 0.9749 0.1495 0.103 Uiso 1 1 calc R . . C45 C 0.5784(17) 1.0905(11) 0.2968(13) 0.084(7) Uani 1 1 d . . . H45C H 0.5595 1.1497 0.2551 0.101 Uiso 1 1 calc R . . H45B H 0.6250 1.0967 0.3355 0.101 Uiso 1 1 calc R . . H45A H 0.5219 1.0691 0.3317 0.101 Uiso 1 1 calc R . . C46 C 0.7121(15) 1.0580(14) 0.1959(14) 0.079(6) Uani 1 1 d . . . H46C H 0.6932 1.1172 0.1542 0.095 Uiso 1 1 calc R . . H46B H 0.7437 1.0148 0.1642 0.095 Uiso 1 1 calc R . . H46A H 0.7564 1.0648 0.2364 0.095 Uiso 1 1 calc R . . C47 C 0.4863(17) 0.9034(17) 0.439(2) 0.109(9) Uani 1 1 d . . . H47C H 0.4359 0.8691 0.4716 0.131 Uiso 1 1 calc R . . H47B H 0.4580 0.9552 0.3929 0.131 Uiso 1 1 calc R . . H47A H 0.5184 0.9256 0.4788 0.131 Uiso 1 1 calc R . . C48 C 0.5594(12) 0.8412(10) 0.3979(11) 0.053(4) Uani 1 1 d . . . C49 C 0.6013(19) 0.7641(18) 0.4683(18) 0.110(8) Uani 1 1 d . . . H49C H 0.5502 0.7320 0.5027 0.132 Uiso 1 1 calc R . . H49B H 0.6356 0.7867 0.5062 0.132 Uiso 1 1 calc R . . H49A H 0.6458 0.7221 0.4427 0.132 Uiso 1 1 calc R . . C50 C 0.5065(17) 0.8069(16) 0.3381(13) 0.085(6) Uani 1 1 d . . . H50C H 0.4544 0.7759 0.3717 0.102 Uiso 1 1 calc R . . H50B H 0.5510 0.7642 0.3134 0.102 Uiso 1 1 calc R . . H50A H 0.4802 0.8585 0.2908 0.102 Uiso 1 1 calc R . . C51 C 0.7471(11) 0.9246(9) 0.4076(9) 0.043(3) Uani 1 1 d . . . C52 C 0.7099(14) 0.9634(12) 0.4753(11) 0.065(5) Uani 1 1 d . . . H52A H 0.6427 0.9776 0.4847 0.078 Uiso 1 1 calc R . . C53 C 0.7728(15) 0.9809(12) 0.5285(11) 0.067(5) Uani 1 1 d . . . H53A H 0.7472 1.0068 0.5743 0.081 Uiso 1 1 calc R . . C54 C 0.8677(14) 0.9625(12) 0.5176(11) 0.064(5) Uani 1 1 d . . . H54A H 0.9097 0.9752 0.5540 0.076 Uiso 1 1 calc R . . C55 C 0.9019(15) 0.9240(14) 0.4505(15) 0.080(6) Uani 1 1 d . . . H55A H 0.9690 0.9116 0.4397 0.096 Uiso 1 1 calc R . . C56 C 0.8431(13) 0.9037(14) 0.4006(14) 0.077(6) Uani 1 1 d . . . H56A H 0.8700 0.8733 0.3584 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.040(2) 0.0415(19) 0.0365(18) -0.0162(14) -0.0086(16) -0.0057(15) P2 0.041(2) 0.0387(18) 0.0455(19) -0.0198(14) -0.0088(17) -0.0086(15) P3 0.0362(19) 0.0415(19) 0.0455(19) -0.0214(14) -0.0125(16) 0.0005(15) P4 0.042(2) 0.0440(19) 0.046(2) -0.0255(15) -0.0050(17) -0.0038(16) Pb1 0.0413(4) 0.0427(3) 0.0477(4) -0.0236(2) -0.0048(3) -0.0030(2) Pb2 0.0430(4) 0.0496(4) 0.0424(4) -0.0181(2) -0.0061(3) -0.0072(3) Pb3 0.0351(4) 0.0446(4) 0.0482(4) -0.0199(2) -0.0069(3) -0.0049(2) Pb4 0.0393(4) 0.0430(3) 0.0465(4) -0.0218(2) -0.0059(3) -0.0072(2) Si1 0.041(2) 0.0383(19) 0.0391(19) -0.0183(15) -0.0052(17) -0.0062(15) Si2 0.036(2) 0.0356(19) 0.047(2) -0.0172(15) -0.0054(17) -0.0059(15) Si3 0.0307(19) 0.048(2) 0.045(2) -0.0162(16) -0.0075(17) -0.0029(15) Si4 0.039(2) 0.045(2) 0.052(2) -0.0304(16) -0.0003(18) -0.0017(16) C1 0.043(8) 0.032(7) 0.038(7) -0.012(5) -0.001(7) 0.008(6) C2 0.054(9) 0.040(8) 0.071(10) -0.028(7) -0.005(8) -0.011(7) C3 0.060(11) 0.051(10) 0.096(13) -0.030(9) -0.009(10) 0.010(8) C4 0.053(10) 0.058(10) 0.063(10) -0.015(7) -0.020(8) 0.001(7) C5 0.034(8) 0.060(9) 0.045(8) -0.012(6) -0.002(7) 0.003(6) C6 0.038(8) 0.044(8) 0.065(9) -0.019(6) -0.008(7) 0.004(6) C7 0.062(10) 0.068(10) 0.044(8) -0.020(7) 0.018(8) -0.020(8) C8 0.077(12) 0.063(10) 0.041(8) -0.017(7) 0.033(9) 0.005(8) C9 0.052(9) 0.036(7) 0.046(8) -0.018(6) -0.016(7) -0.006(6) C10 0.080(13) 0.091(14) 0.070(11) -0.043(10) -0.027(11) -0.018(11) C11 0.090(15) 0.094(14) 0.084(13) -0.043(11) -0.003(12) -0.052(12) C12 0.072(12) 0.085(12) 0.062(10) -0.044(9) -0.016(10) -0.016(10) C13 0.110(16) 0.082(12) 0.039(8) -0.022(8) -0.030(10) -0.030(11) C14 0.096(14) 0.052(9) 0.070(11) -0.019(8) -0.031(11) -0.021(9) C15 0.048(9) 0.049(8) 0.058(9) -0.024(7) -0.028(8) -0.002(7) C16 0.076(12) 0.075(11) 0.058(10) -0.039(8) -0.006(9) -0.022(9) C17 0.093(15) 0.118(16) 0.059(10) -0.056(10) 0.033(11) -0.058(13) C18 0.106(16) 0.079(12) 0.092(14) -0.049(10) -0.065(13) 0.016(11) C19 0.035(8) 0.063(10) 0.068(10) -0.035(8) 0.005(8) -0.009(7) C20 0.078(14) 0.085(13) 0.067(11) -0.019(9) 0.035(11) -0.012(10) C21 0.046(10) 0.115(16) 0.059(10) -0.031(10) 0.003(9) -0.009(10) C22 0.057(11) 0.051(9) 0.097(14) -0.028(9) 0.009(10) 0.004(8) C23 0.060(10) 0.043(8) 0.056(9) -0.016(6) -0.004(8) -0.012(7) C24 0.064(11) 0.037(8) 0.081(11) -0.025(7) -0.016(9) -0.004(7) C25 0.076(12) 0.037(8) 0.067(10) -0.013(7) -0.009(9) -0.001(8) C26 0.062(11) 0.072(12) 0.053(9) -0.030(8) -0.016(9) 0.023(9) C27 0.044(9) 0.054(9) 0.058(9) -0.034(7) -0.009(8) 0.004(7) C28 0.039(8) 0.055(9) 0.055(9) -0.022(7) 0.007(7) -0.018(7) C29 0.057(10) 0.041(8) 0.078(11) -0.013(7) -0.020(9) -0.007(7) C30 0.086(13) 0.047(9) 0.076(11) -0.020(8) -0.034(11) 0.028(9) C31 0.073(12) 0.051(9) 0.077(11) -0.015(8) -0.015(10) -0.018(8) C32 0.042(9) 0.068(11) 0.088(13) -0.012(9) -0.007(9) 0.006(8) C33 0.039(8) 0.075(11) 0.056(9) -0.018(8) 0.001(8) -0.029(8) C34 0.076(14) 0.15(2) 0.053(10) -0.059(12) 0.015(10) -0.032(13) C35 0.073(12) 0.066(11) 0.081(12) -0.031(9) -0.023(10) -0.021(9) C36 0.099(16) 0.094(14) 0.056(10) -0.027(9) -0.027(11) -0.012(12) C37 0.041(8) 0.053(9) 0.051(9) -0.017(6) -0.001(7) -0.006(7) C38 0.044(8) 0.063(9) 0.038(8) -0.018(6) 0.003(7) -0.023(7) C39 0.058(10) 0.063(10) 0.054(9) -0.033(7) -0.006(9) 0.000(8) C40 0.048(9) 0.050(9) 0.064(10) -0.022(7) 0.008(8) -0.001(7) C41 0.026(7) 0.037(8) 0.094(13) -0.020(7) 0.007(8) -0.005(6) C42 0.047(9) 0.049(8) 0.050(8) -0.017(6) 0.007(7) -0.005(7) C43 0.034(8) 0.058(9) 0.054(9) -0.024(7) -0.006(7) 0.006(6) C44 0.070(13) 0.097(15) 0.102(15) -0.043(12) -0.044(12) 0.004(11) C45 0.116(17) 0.040(9) 0.086(13) -0.024(8) -0.022(12) 0.042(10) C46 0.082(14) 0.074(12) 0.085(13) -0.026(10) -0.017(12) -0.011(10) C47 0.092(16) 0.115(18) 0.16(2) -0.094(17) 0.074(17) -0.059(14) C48 0.049(9) 0.050(9) 0.068(10) -0.031(7) 0.014(8) -0.008(7) C49 0.094(18) 0.11(2) 0.13(2) -0.040(16) 0.017(16) -0.029(15) C50 0.089(15) 0.120(17) 0.067(11) -0.048(11) 0.028(11) -0.053(13) C51 0.047(9) 0.041(7) 0.046(8) -0.030(6) 0.014(7) -0.002(6) C52 0.071(12) 0.086(12) 0.056(9) -0.052(9) -0.002(9) -0.001(9) C53 0.089(15) 0.074(11) 0.047(9) -0.033(8) -0.004(10) -0.005(10) C54 0.078(13) 0.077(11) 0.047(9) -0.029(8) -0.012(9) -0.014(9) C55 0.060(12) 0.089(14) 0.099(15) -0.041(11) -0.009(12) 0.000(10) C56 0.053(11) 0.100(14) 0.107(15) -0.079(12) -0.031(11) 0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 Si1 2.231(5) . ? P1 Pb3 2.711(4) . ? P1 Pb4 2.724(3) . ? P1 Pb1 2.736(3) . ? P2 Si2 2.253(5) . ? P2 Pb2 2.718(3) . ? P2 Pb1 2.726(4) . ? P2 Pb3 2.734(3) . ? P3 Si3 2.241(5) . ? P3 Pb2 2.726(4) . ? P3 Pb4 2.734(3) . ? P3 Pb1 2.738(3) . ? P4 Si4 2.251(5) . ? P4 Pb3 2.730(3) . ? P4 Pb2 2.745(4) . ? P4 Pb4 2.746(4) . ? Si1 C9 1.875(13) . ? Si1 C5 1.896(15) . ? Si1 C1 1.911(12) . ? Si2 C23 1.878(15) . ? Si2 C15 1.915(13) . ? Si2 C19 1.929(16) . ? Si3 C29 1.902(15) . ? Si3 C37 1.921(16) . ? Si3 C33 1.933(17) . ? Si4 C51 1.920(15) . ? Si4 C48 1.951(17) . ? Si4 C43 1.962(15) . ? C1 C3 1.50(2) . ? C1 C2 1.53(2) . ? C1 C4 1.55(2) . ? C5 C7 1.53(2) . ? C5 C8 1.54(2) . ? C5 C6 1.55(2) . ? C9 C10 1.39(3) . ? C9 C14 1.44(2) . ? C10 C11 1.41(2) . ? C11 C12 1.39(3) . ? C12 C13 1.38(3) . ? C13 C14 1.36(2) . ? C15 C16 1.49(2) . ? C15 C17 1.51(3) . ? C15 C18 1.55(2) . ? C19 C20 1.51(2) . ? C19 C22 1.52(3) . ? C19 C21 1.55(2) . ? C23 C24 1.39(2) . ? C23 C28 1.41(2) . ? C24 C25 1.36(2) . ? C25 C26 1.38(3) . ? C26 C27 1.34(3) . ? C27 C28 1.36(2) . ? C29 C31 1.48(2) . ? C29 C30 1.52(2) . ? C29 C32 1.57(2) . ? C33 C36 1.53(2) . ? C33 C34 1.54(3) . ? C33 C35 1.56(2) . ? C37 C42 1.39(2) . ? C37 C38 1.39(2) . ? C38 C39 1.35(2) . ? C39 C40 1.37(2) . ? C40 C41 1.39(2) . ? C41 C42 1.38(2) . ? C43 C44 1.51(2) . ? C43 C45 1.52(2) . ? C43 C46 1.54(3) . ? C47 C48 1.53(2) . ? C48 C49 1.47(3) . ? C48 C50 1.52(3) . ? C51 C56 1.35(2) . ? C51 C52 1.41(2) . ? C52 C53 1.39(3) . ? C53 C54 1.34(3) . ? C54 C55 1.39(3) . ? C55 C56 1.34(3) . ? 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 Si1 P1 Pb3 119.10(17) . . ? Si1 P1 Pb4 117.60(17) . . ? Pb3 P1 Pb4 98.08(12) . . ? Si1 P1 Pb1 120.11(17) . . ? Pb3 P1 Pb1 99.02(12) . . ? Pb4 P1 Pb1 98.55(10) . . ? Si2 P2 Pb2 117.70(17) . . ? Si2 P2 Pb1 119.58(18) . . ? Pb2 P2 Pb1 98.54(12) . . ? Si2 P2 Pb3 120.55(17) . . ? Pb2 P2 Pb3 97.08(11) . . ? Pb1 P2 Pb3 98.69(12) . . ? Si3 P3 Pb2 118.01(17) . . ? Si3 P3 Pb4 116.84(18) . . ? Pb2 P3 Pb4 97.34(11) . . ? Si3 P3 Pb1 123.35(18) . . ? Pb2 P3 Pb1 98.08(12) . . ? Pb4 P3 Pb1 98.25(11) . . ? Si4 P4 Pb3 118.64(17) . . ? Si4 P4 Pb2 120.91(18) . . ? Pb3 P4 Pb2 96.55(11) . . ? Si4 P4 Pb4 121.44(18) . . ? Pb3 P4 Pb4 97.07(12) . . ? Pb2 P4 Pb4 96.58(12) . . ? P2 Pb1 P1 80.39(12) . . ? P2 Pb1 P3 80.93(11) . . ? P1 Pb1 P3 80.76(10) . . ? P2 Pb2 P3 81.29(11) . . ? P2 Pb2 P4 82.61(11) . . ? P3 Pb2 P4 82.61(11) . . ? P1 Pb3 P4 82.16(11) . . ? P1 Pb3 P2 80.69(12) . . ? P4 Pb3 P2 82.61(11) . . ? P1 Pb4 P3 81.05(10) . . ? P1 Pb4 P4 81.62(11) . . ? P3 Pb4 P4 82.44(12) . . ? C9 Si1 C5 111.0(7) . . ? C9 Si1 C1 105.6(6) . . ? C5 Si1 C1 115.8(7) . . ? C9 Si1 P1 108.0(5) . . ? C5 Si1 P1 107.4(5) . . ? C1 Si1 P1 108.7(4) . . ? C23 Si2 C15 109.4(7) . . ? C23 Si2 C19 107.5(7) . . ? C15 Si2 C19 114.3(7) . . ? C23 Si2 P2 109.3(5) . . ? C15 Si2 P2 108.5(5) . . ? C19 Si2 P2 107.7(5) . . ? C29 Si3 C37 107.5(8) . . ? C29 Si3 C33 115.1(7) . . ? C37 Si3 C33 110.3(7) . . ? C29 Si3 P3 108.2(5) . . ? C37 Si3 P3 107.7(5) . . ? C33 Si3 P3 107.7(5) . . ? C51 Si4 C48 110.3(7) . . ? C51 Si4 C43 106.7(6) . . ? C48 Si4 C43 116.0(7) . . ? C51 Si4 P4 107.4(4) . . ? C48 Si4 P4 106.8(5) . . ? C43 Si4 P4 109.3(5) . . ? C3 C1 C2 110.1(13) . . ? C3 C1 C4 107.1(13) . . ? C2 C1 C4 107.6(12) . . ? C3 C1 Si1 109.0(10) . . ? C2 C1 Si1 111.7(9) . . ? C4 C1 Si1 111.2(10) . . ? C7 C5 C8 107.1(13) . . ? C7 C5 C6 105.3(13) . . ? C8 C5 C6 108.6(12) . . ? C7 C5 Si1 114.8(10) . . ? C8 C5 Si1 109.9(12) . . ? C6 C5 Si1 110.9(10) . . ? C10 C9 C14 116.1(14) . . ? C10 C9 Si1 122.1(11) . . ? C14 C9 Si1 121.8(12) . . ? C9 C10 C11 122.2(18) . . ? C12 C11 C10 118.3(19) . . ? C13 C12 C11 120.7(15) . . ? C14 C13 C12 120.2(16) . . ? C13 C14 C9 121.9(18) . . ? C16 C15 C17 108.1(14) . . ? C16 C15 C18 107.6(14) . . ? C17 C15 C18 107.5(16) . . ? C16 C15 Si2 113.4(11) . . ? C17 C15 Si2 109.4(11) . . ? C18 C15 Si2 110.6(11) . . ? C20 C19 C22 108.9(14) . . ? C20 C19 C21 107.6(16) . . ? C22 C19 C21 104.4(15) . . ? C20 C19 Si2 113.2(12) . . ? C22 C19 Si2 114.1(12) . . ? C21 C19 Si2 108.1(11) . . ? C24 C23 C28 113.8(14) . . ? C24 C23 Si2 124.7(13) . . ? C28 C23 Si2 121.5(12) . . ? C25 C24 C23 123.3(16) . . ? C24 C25 C26 120.3(16) . . ? C27 C26 C25 118.6(14) . . ? C26 C27 C28 121.2(15) . . ? C27 C28 C23 122.8(15) . . ? C31 C29 C30 109.2(15) . . ? C31 C29 C32 107.2(14) . . ? C30 C29 C32 106.5(15) . . ? C31 C29 Si3 111.8(12) . . ? C30 C29 Si3 110.2(10) . . ? C32 C29 Si3 111.6(12) . . ? C36 C33 C34 108.1(15) . . ? C36 C33 C35 109.8(14) . . ? C34 C33 C35 106.5(16) . . ? C36 C33 Si3 113.8(13) . . ? C34 C33 Si3 109.8(11) . . ? C35 C33 Si3 108.6(11) . . ? C42 C37 C38 116.7(15) . . ? C42 C37 Si3 121.1(11) . . ? C38 C37 Si3 122.0(12) . . ? C39 C38 C37 122.8(14) . . ? C38 C39 C40 121.2(15) . . ? C39 C40 C41 117.7(16) . . ? C42 C41 C40 121.2(15) . . ? C41 C42 C37 120.4(15) . . ? C44 C43 C45 110.3(14) . . ? C44 C43 C46 107.8(15) . . ? C45 C43 C46 107.2(16) . . ? C44 C43 Si4 112.9(13) . . ? C45 C43 Si4 109.6(11) . . ? C46 C43 Si4 108.8(10) . . ? C49 C48 C50 110.0(18) . . ? C49 C48 C47 108.6(19) . . ? C50 C48 C47 107.8(17) . . ? C49 C48 Si4 108.6(14) . . ? C50 C48 Si4 109.4(12) . . ? C47 C48 Si4 112.5(12) . . ? C56 C51 C52 116.6(15) . . ? C56 C51 Si4 123.3(11) . . ? C52 C51 Si4 120.1(12) . . ? C53 C52 C51 119.1(17) . . ? C54 C53 C52 122.6(16) . . ? C53 C54 C55 116.8(17) . . ? C56 C55 C54 122(2) . . ? C55 C56 C51 122.9(17) . . ? 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 Si2 P2 Pb1 P1 141.03(18) . . . . ? Pb2 P2 Pb1 P1 -90.23(11) . . . . ? Pb3 P2 Pb1 P1 8.34(10) . . . . ? Si2 P2 Pb1 P3 -136.90(19) . . . . ? Pb2 P2 Pb1 P3 -8.16(10) . . . . ? Pb3 P2 Pb1 P3 90.41(11) . . . . ? Si1 P1 Pb1 P2 -139.8(2) . . . . ? Pb3 P1 Pb1 P2 -8.42(10) . . . . ? Pb4 P1 Pb1 P2 91.23(12) . . . . ? Si1 P1 Pb1 P3 137.9(2) . . . . ? Pb3 P1 Pb1 P3 -90.70(12) . . . . ? Pb4 P1 Pb1 P3 8.96(12) . . . . ? Si3 P3 Pb1 P2 139.5(2) . . . . ? Pb2 P3 Pb1 P2 8.13(10) . . . . ? Pb4 P3 Pb1 P2 -90.56(12) . . . . ? Si3 P3 Pb1 P1 -138.8(2) . . . . ? Pb2 P3 Pb1 P1 89.77(12) . . . . ? Pb4 P3 Pb1 P1 -8.92(12) . . . . ? Si2 P2 Pb2 P3 138.2(2) . . . . ? Pb1 P2 Pb2 P3 8.19(10) . . . . ? Pb3 P2 Pb2 P3 -91.75(12) . . . . ? Si2 P2 Pb2 P4 -138.2(2) . . . . ? Pb1 P2 Pb2 P4 91.79(12) . . . . ? Pb3 P2 Pb2 P4 -8.14(12) . . . . ? Si3 P3 Pb2 P2 -142.9(2) . . . . ? Pb4 P3 Pb2 P2 91.32(11) . . . . ? Pb1 P3 Pb2 P2 -8.14(10) . . . . ? Si3 P3 Pb2 P4 133.5(2) . . . . ? Pb4 P3 Pb2 P4 7.72(10) . . . . ? Pb1 P3 Pb2 P4 -91.75(11) . . . . ? Si4 P4 Pb2 P2 137.3(2) . . . . ? Pb3 P4 Pb2 P2 8.14(12) . . . . ? Pb4 P4 Pb2 P2 -89.79(12) . . . . ? Si4 P4 Pb2 P3 -140.6(2) . . . . ? Pb3 P4 Pb2 P3 90.26(12) . . . . ? Pb4 P4 Pb2 P3 -7.67(10) . . . . ? Si1 P1 Pb3 P4 -135.84(19) . . . . ? Pb4 P1 Pb3 P4 -7.93(10) . . . . ? Pb1 P1 Pb3 P4 92.13(11) . . . . ? Si1 P1 Pb3 P2 140.42(19) . . . . ? Pb4 P1 Pb3 P2 -91.67(11) . . . . ? Pb1 P1 Pb3 P2 8.39(10) . . . . ? Si4 P4 Pb3 P1 139.7(2) . . . . ? Pb2 P4 Pb3 P1 -89.66(12) . . . . ? Pb4 P4 Pb3 P1 7.84(10) . . . . ? Si4 P4 Pb3 P2 -138.8(2) . . . . ? Pb2 P4 Pb3 P2 -8.10(12) . . . . ? Pb4 P4 Pb3 P2 89.40(12) . . . . ? Si2 P2 Pb3 P1 -140.5(2) . . . . ? Pb2 P2 Pb3 P1 91.40(12) . . . . ? Pb1 P2 Pb3 P1 -8.41(10) . . . . ? Si2 P2 Pb3 P4 136.3(2) . . . . ? Pb2 P2 Pb3 P4 8.19(12) . . . . ? Pb1 P2 Pb3 P4 -91.63(12) . . . . ? Si1 P1 Pb4 P3 -139.6(2) . . . . ? Pb3 P1 Pb4 P3 91.49(12) . . . . ? Pb1 P1 Pb4 P3 -8.96(12) . . . . ? Si1 P1 Pb4 P4 136.8(2) . . . . ? Pb3 P1 Pb4 P4 7.89(10) . . . . ? Pb1 P1 Pb4 P4 -92.56(12) . . . . ? Si3 P3 Pb4 P1 143.1(2) . . . . ? Pb2 P3 Pb4 P1 -90.37(12) . . . . ? Pb1 P3 Pb4 P1 8.95(12) . . . . ? Si3 P3 Pb4 P4 -134.3(2) . . . . ? Pb2 P3 Pb4 P4 -7.71(10) . . . . ? Pb1 P3 Pb4 P4 91.60(12) . . . . ? Si4 P4 Pb4 P1 -137.8(2) . . . . ? Pb3 P4 Pb4 P1 -7.81(10) . . . . ? Pb2 P4 Pb4 P1 89.65(11) . . . . ? Si4 P4 Pb4 P3 140.2(2) . . . . ? Pb3 P4 Pb4 P3 -89.82(11) . . . . ? Pb2 P4 Pb4 P3 7.65(10) . . . . ? Pb3 P1 Si1 C9 -56.4(5) . . . . ? Pb4 P1 Si1 C9 -174.5(5) . . . . ? Pb1 P1 Si1 C9 65.6(5) . . . . ? Pb3 P1 Si1 C5 -176.2(5) . . . . ? Pb4 P1 Si1 C5 65.6(6) . . . . ? Pb1 P1 Si1 C5 -54.2(6) . . . . ? Pb3 P1 Si1 C1 57.8(5) . . . . ? Pb4 P1 Si1 C1 -60.4(5) . . . . ? Pb1 P1 Si1 C1 179.8(5) . . . . ? Pb2 P2 Si2 C23 -61.4(6) . . . . ? Pb1 P2 Si2 C23 58.0(6) . . . . ? Pb3 P2 Si2 C23 -179.5(6) . . . . ? Pb2 P2 Si2 C15 179.4(5) . . . . ? Pb1 P2 Si2 C15 -61.2(5) . . . . ? Pb3 P2 Si2 C15 61.2(5) . . . . ? Pb2 P2 Si2 C19 55.1(5) . . . . ? Pb1 P2 Si2 C19 174.5(5) . . . . ? Pb3 P2 Si2 C19 -63.0(5) . . . . ? Pb2 P3 Si3 C29 70.8(6) . . . . ? Pb4 P3 Si3 C29 -173.7(6) . . . . ? Pb1 P3 Si3 C29 -52.0(7) . . . . ? Pb2 P3 Si3 C37 -173.2(5) . . . . ? Pb4 P3 Si3 C37 -57.7(5) . . . . ? Pb1 P3 Si3 C37 64.0(5) . . . . ? Pb2 P3 Si3 C33 -54.2(5) . . . . ? Pb4 P3 Si3 C33 61.3(6) . . . . ? Pb1 P3 Si3 C33 -177.0(5) . . . . ? Pb3 P4 Si4 C51 -178.2(5) . . . . ? Pb2 P4 Si4 C51 63.2(5) . . . . ? Pb4 P4 Si4 C51 -58.3(5) . . . . ? Pb3 P4 Si4 C48 63.5(6) . . . . ? Pb2 P4 Si4 C48 -55.1(6) . . . . ? Pb4 P4 Si4 C48 -176.6(5) . . . . ? Pb3 P4 Si4 C43 -62.8(5) . . . . ? Pb2 P4 Si4 C43 178.6(5) . . . . ? Pb4 P4 Si4 C43 57.1(5) . . . . ? C9 Si1 C1 C3 72.1(12) . . . . ? C5 Si1 C1 C3 -164.6(11) . . . . ? P1 Si1 C1 C3 -43.6(12) . . . . ? C9 Si1 C1 C2 -166.1(10) . . . . ? C5 Si1 C1 C2 -42.8(12) . . . . ? P1 Si1 C1 C2 78.2(10) . . . . ? C9 Si1 C1 C4 -45.8(13) . . . . ? C5 Si1 C1 C4 77.5(12) . . . . ? P1 Si1 C1 C4 -161.6(10) . . . . ? C9 Si1 C5 C7 76.9(13) . . . . ? C1 Si1 C5 C7 -43.6(14) . . . . ? P1 Si1 C5 C7 -165.3(11) . . . . ? C9 Si1 C5 C8 -43.9(12) . . . . ? C1 Si1 C5 C8 -164.4(10) . . . . ? P1 Si1 C5 C8 74.0(11) . . . . ? C9 Si1 C5 C6 -164.0(9) . . . . ? C1 Si1 C5 C6 75.6(11) . . . . ? P1 Si1 C5 C6 -46.1(11) . . . . ? C5 Si1 C9 C10 130.4(14) . . . . ? C1 Si1 C9 C10 -103.3(14) . . . . ? P1 Si1 C9 C10 12.9(15) . . . . ? C5 Si1 C9 C14 -47.3(14) . . . . ? C1 Si1 C9 C14 79.0(14) . . . . ? P1 Si1 C9 C14 -164.8(12) . . . . ? C14 C9 C10 C11 -8(3) . . . . ? Si1 C9 C10 C11 173.7(16) . . . . ? C9 C10 C11 C12 7(3) . . . . ? C10 C11 C12 C13 -4(3) . . . . ? C11 C12 C13 C14 3(3) . . . . ? C12 C13 C14 C9 -5(3) . . . . ? C10 C9 C14 C13 8(3) . . . . ? Si1 C9 C14 C13 -174.3(15) . . . . ? C23 Si2 C15 C16 52.1(14) . . . . ? C19 Si2 C15 C16 -68.5(14) . . . . ? P2 Si2 C15 C16 171.3(11) . . . . ? C23 Si2 C15 C17 -68.7(14) . . . . ? C19 Si2 C15 C17 170.7(12) . . . . ? P2 Si2 C15 C17 50.5(13) . . . . ? C23 Si2 C15 C18 173.1(14) . . . . ? C19 Si2 C15 C18 52.5(16) . . . . ? P2 Si2 C15 C18 -67.8(14) . . . . ? C23 Si2 C19 C20 159.7(13) . . . . ? C15 Si2 C19 C20 -78.6(15) . . . . ? P2 Si2 C19 C20 42.1(14) . . . . ? C23 Si2 C19 C22 -75.0(13) . . . . ? C15 Si2 C19 C22 46.7(14) . . . . ? P2 Si2 C19 C22 167.4(11) . . . . ? C23 Si2 C19 C21 40.7(14) . . . . ? C15 Si2 C19 C21 162.3(12) . . . . ? P2 Si2 C19 C21 -77.0(12) . . . . ? C15 Si2 C23 C24 -64.7(16) . . . . ? C19 Si2 C23 C24 59.9(16) . . . . ? P2 Si2 C23 C24 176.6(13) . . . . ? C15 Si2 C23 C28 117.8(14) . . . . ? C19 Si2 C23 C28 -117.6(14) . . . . ? P2 Si2 C23 C28 -0.9(15) . . . . ? C28 C23 C24 C25 2(3) . . . . ? Si2 C23 C24 C25 -176.0(14) . . . . ? C23 C24 C25 C26 -1(3) . . . . ? C24 C25 C26 C27 2(3) . . . . ? C25 C26 C27 C28 -3(2) . . . . ? C26 C27 C28 C23 4(2) . . . . ? C24 C23 C28 C27 -3(2) . . . . ? Si2 C23 C28 C27 174.8(12) . . . . ? C37 Si3 C29 C31 174.7(11) . . . . ? C33 Si3 C29 C31 51.3(14) . . . . ? P3 Si3 C29 C31 -69.2(12) . . . . ? C37 Si3 C29 C30 -63.6(14) . . . . ? C33 Si3 C29 C30 173.0(13) . . . . ? P3 Si3 C29 C30 52.5(14) . . . . ? C37 Si3 C29 C32 54.6(14) . . . . ? C33 Si3 C29 C32 -68.8(15) . . . . ? P3 Si3 C29 C32 170.7(12) . . . . ? C29 Si3 C33 C36 40.7(15) . . . . ? C37 Si3 C33 C36 -81.2(14) . . . . ? P3 Si3 C33 C36 161.4(12) . . . . ? C29 Si3 C33 C34 -80.6(15) . . . . ? C37 Si3 C33 C34 157.4(13) . . . . ? P3 Si3 C33 C34 40.1(14) . . . . ? C29 Si3 C33 C35 163.2(11) . . . . ? C37 Si3 C33 C35 41.3(13) . . . . ? P3 Si3 C33 C35 -76.0(11) . . . . ? C29 Si3 C37 C42 -82.3(14) . . . . ? C33 Si3 C37 C42 44.0(14) . . . . ? P3 Si3 C37 C42 161.3(11) . . . . ? C29 Si3 C37 C38 92.4(14) . . . . ? C33 Si3 C37 C38 -141.3(13) . . . . ? P3 Si3 C37 C38 -24.0(14) . . . . ? C42 C37 C38 C39 -1(2) . . . . ? Si3 C37 C38 C39 -176.3(12) . . . . ? C37 C38 C39 C40 1(2) . . . . ? C38 C39 C40 C41 -1(2) . . . . ? C39 C40 C41 C42 2(2) . . . . ? C40 C41 C42 C37 -3(2) . . . . ? C38 C37 C42 C41 2(2) . . . . ? Si3 C37 C42 C41 177.4(11) . . . . ? C51 Si4 C43 C44 -179.5(13) . . . . ? C48 Si4 C43 C44 -56.2(15) . . . . ? P4 Si4 C43 C44 64.6(14) . . . . ? C51 Si4 C43 C45 -56.1(15) . . . . ? C48 Si4 C43 C45 67.2(15) . . . . ? P4 Si4 C43 C45 -171.9(12) . . . . ? C51 Si4 C43 C46 60.8(13) . . . . ? C48 Si4 C43 C46 -175.8(11) . . . . ? P4 Si4 C43 C46 -55.0(12) . . . . ? C51 Si4 C48 C49 -47.4(16) . . . . ? C43 Si4 C48 C49 -168.8(14) . . . . ? P4 Si4 C48 C49 69.1(15) . . . . ? C51 Si4 C48 C50 -167.5(13) . . . . ? C43 Si4 C48 C50 71.1(14) . . . . ? P4 Si4 C48 C50 -51.1(14) . . . . ? C51 Si4 C48 C47 72.9(17) . . . . ? C43 Si4 C48 C47 -48.6(18) . . . . ? P4 Si4 C48 C47 -170.7(15) . . . . ? C48 Si4 C51 C56 130.8(16) . . . . ? C43 Si4 C51 C56 -102.3(16) . . . . ? P4 Si4 C51 C56 14.8(17) . . . . ? C48 Si4 C51 C52 -49.2(14) . . . . ? C43 Si4 C51 C52 77.6(14) . . . . ? P4 Si4 C51 C52 -165.3(12) . . . . ? C56 C51 C52 C53 2(3) . . . . ? Si4 C51 C52 C53 -177.7(14) . . . . ? C51 C52 C53 C54 0(3) . . . . ? C52 C53 C54 C55 -1(3) . . . . ? C53 C54 C55 C56 -2(3) . . . . ? C54 C55 C56 C51 5(4) . . . . ? C52 C51 C56 C55 -5(3) . . . . ? Si4 C51 C56 C55 175.3(18) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 2.508 _refine_diff_density_min -3.988 _refine_diff_density_rms 0.377 # Attachment 'Pb4Sb6.CIF' data_e:\traut\crystal\st155\p21c _database_code_depnum_ccdc_archive 'CCDC 751818' #TrackingRef 'Pb4Sb6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H122 Pb4 Sb6 Si6' _chemical_formula_weight 2499.32 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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 23.786(5) _cell_length_b 13.266(3) _cell_length_c 26.391(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.03(3) _cell_angle_gamma 90.00 _cell_volume 8043(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1422 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 26.09 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4656 _exptl_absorpt_coefficient_mu 10.438 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1355 _exptl_absorpt_correction_T_max 0.3878 _exptl_absorpt_process_details ? _exptl_special_details ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0460 0 0 1 0.0520 -1 0 0 0.0800 1 0 0 0.0720 -13 9 1 0.1560 -1 -5 -4 0.1300 0 -13 7 0.1430 ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33876 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.66 _reflns_number_total 14477 _reflns_number_gt 12169 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+58.1389P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14477 _refine_ls_number_parameters 630 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Si1 Si 0.27001(12) 0.7270(2) 0.11646(11) 0.0333(6) Uani 1 1 d . . . Si2 Si 0.21404(12) 0.6097(2) -0.15178(11) 0.0352(6) Uani 1 1 d . . . Si3 Si 0.10109(14) 0.1881(2) -0.14828(11) 0.0421(7) Uani 1 1 d . . . Si4 Si 0.08880(11) 0.2454(2) 0.06565(10) 0.0301(5) Uani 1 1 d . . . Si5 Si 0.43307(12) 0.2171(2) 0.00761(11) 0.0321(6) Uani 1 1 d . . . Si6 Si 0.38742(14) 0.3946(3) 0.21636(11) 0.0417(7) Uani 1 1 d . . . Sb1 Sb 0.27286(3) 0.54577(5) 0.07983(2) 0.02957(14) Uani 1 1 d . . . Sb2 Sb 0.23572(3) 0.48975(5) -0.07220(2) 0.03517(15) Uani 1 1 d . . . Sb3 Sb 0.17999(3) 0.16326(5) -0.06037(3) 0.03563(15) Uani 1 1 d . . . Sb4 Sb 0.17087(3) 0.29484(5) 0.02131(2) 0.02977(14) Uani 1 1 d . . . Sb5 Sb 0.34159(3) 0.30862(5) 0.01750(2) 0.02981(14) Uani 1 1 d . . . Sb6 Sb 0.28014(3) 0.40067(5) 0.15916(2) 0.03358(15) Uani 1 1 d . . . Pb1 Pb 0.350266(17) 0.52868(3) 0.006737(15) 0.03501(10) Uani 1 1 d . . . Pb2 Pb 0.159282(16) 0.51574(3) -0.001368(14) 0.03360(10) Uani 1 1 d . . . Pb3 Pb 0.270642(17) 0.28136(3) -0.092163(14) 0.03707(10) Uani 1 1 d . . . Pb4 Pb 0.281749(16) 0.22234(3) 0.092894(14) 0.03323(10) Uani 1 1 d . . . C1 C 0.2084(5) 0.7382(9) 0.1497(5) 0.046(3) Uani 1 1 d . . . H1A H 0.2108 0.8080 0.1644 0.055 Uiso 1 1 calc R . . C2 C 0.1487(5) 0.7283(11) 0.1130(6) 0.057(3) Uani 1 1 d . . . H2A H 0.1449 0.6622 0.0959 0.068 Uiso 1 1 calc R . . H2B H 0.1429 0.7814 0.0864 0.068 Uiso 1 1 calc R . . H2C H 0.1193 0.7349 0.1329 0.068 Uiso 1 1 calc R . . C3 C 0.2159(6) 0.6670(11) 0.1962(5) 0.060(3) Uani 1 1 d . . . H3A H 0.2526 0.6821 0.2222 0.072 Uiso 1 1 calc R . . H3B H 0.2165 0.5972 0.1842 0.072 Uiso 1 1 calc R . . H3C H 0.1833 0.6759 0.2123 0.072 Uiso 1 1 calc R . . C4 C 0.3413(5) 0.7520(9) 0.1665(4) 0.044(3) Uani 1 1 d . . . H4A H 0.3484 0.6936 0.1914 0.052 Uiso 1 1 calc R . . C5 C 0.3942(5) 0.7590(11) 0.1438(5) 0.058(3) Uani 1 1 d . . . H5A H 0.3887 0.8147 0.1186 0.070 Uiso 1 1 calc R . . H5B H 0.3985 0.6957 0.1260 0.070 Uiso 1 1 calc R . . H5C H 0.4293 0.7711 0.1722 0.070 Uiso 1 1 calc R . . C6 C 0.3397(7) 0.8485(15) 0.1999(7) 0.087(6) Uani 1 1 d . . . H6A H 0.3092 0.8413 0.2185 0.104 Uiso 1 1 calc R . . H6B H 0.3313 0.9074 0.1768 0.104 Uiso 1 1 calc R . . H6C H 0.3774 0.8574 0.2254 0.104 Uiso 1 1 calc R . . C7 C 0.2560(6) 0.8142(9) 0.0574(5) 0.049(3) Uani 1 1 d . . . H7A H 0.2160 0.7987 0.0353 0.059 Uiso 1 1 calc R . . C8 C 0.2969(7) 0.8049(11) 0.0222(5) 0.064(4) Uani 1 1 d . . . H8A H 0.2950 0.7362 0.0082 0.077 Uiso 1 1 calc R . . H8B H 0.3367 0.8196 0.0425 0.077 Uiso 1 1 calc R . . H8C H 0.2854 0.8529 -0.0068 0.077 Uiso 1 1 calc R . . C9 C 0.2558(9) 0.9276(10) 0.0747(8) 0.088(5) Uani 1 1 d . . . H9A H 0.2936 0.9444 0.0986 0.105 Uiso 1 1 calc R . . H9B H 0.2250 0.9380 0.0926 0.105 Uiso 1 1 calc R . . H9C H 0.2488 0.9710 0.0436 0.105 Uiso 1 1 calc R . . C10 C 0.1397(5) 0.5786(10) -0.1973(4) 0.045(3) Uani 1 1 d . . . H10A H 0.1399 0.5047 -0.2045 0.053 Uiso 1 1 calc R . . C11 C 0.0895(6) 0.5969(11) -0.1734(6) 0.061(3) Uani 1 1 d . . . H11A H 0.0887 0.6682 -0.1640 0.073 Uiso 1 1 calc R . . H11B H 0.0943 0.5553 -0.1419 0.073 Uiso 1 1 calc R . . H11C H 0.0530 0.5792 -0.1989 0.073 Uiso 1 1 calc R . . C12 C 0.1279(6) 0.6310(14) -0.2501(5) 0.072(5) Uani 1 1 d . . . H12A H 0.1576 0.6114 -0.2679 0.086 Uiso 1 1 calc R . . H12B H 0.1290 0.7042 -0.2449 0.086 Uiso 1 1 calc R . . H12C H 0.0894 0.6113 -0.2717 0.086 Uiso 1 1 calc R . . C13 C 0.2703(5) 0.5836(9) -0.1893(4) 0.045(3) Uani 1 1 d . . . H13A H 0.2655 0.6379 -0.2163 0.054 Uiso 1 1 calc R . . C14 C 0.2611(7) 0.4847(11) -0.2193(6) 0.065(4) Uani 1 1 d . . . H14A H 0.2230 0.4856 -0.2450 0.077 Uiso 1 1 calc R . . H14B H 0.2625 0.4288 -0.1948 0.077 Uiso 1 1 calc R . . H14C H 0.2917 0.4760 -0.2376 0.077 Uiso 1 1 calc R . . C15 C 0.3330(6) 0.5914(16) -0.1559(6) 0.082(6) Uani 1 1 d . . . H15A H 0.3395 0.5423 -0.1273 0.099 Uiso 1 1 calc R . . H15B H 0.3402 0.6595 -0.1413 0.099 Uiso 1 1 calc R . . H15C H 0.3597 0.5775 -0.1778 0.099 Uiso 1 1 calc R . . C16 C 0.2194(10) 0.7437(12) -0.1279(8) 0.091(6) Uani 1 1 d . . . C19 C 0.0677(5) 0.3186(9) -0.1601(4) 0.048(3) Uani 1 1 d . . . H19A H 0.0990 0.3647 -0.1652 0.058 Uiso 1 1 calc R . . C20 C 0.0455(6) 0.3627(10) -0.1167(5) 0.052(3) Uani 1 1 d . . . H20C H 0.0294 0.4298 -0.1270 0.063 Uiso 1 1 calc R . . H20B H 0.0776 0.3680 -0.0848 0.063 Uiso 1 1 calc R . . H20A H 0.0151 0.3190 -0.1098 0.063 Uiso 1 1 calc R . . C21 C 0.0185(7) 0.3215(13) -0.2115(5) 0.073(4) Uani 1 1 d . . . H21A H -0.0118 0.2729 -0.2094 0.087 Uiso 1 1 calc R . . H21B H 0.0344 0.3041 -0.2411 0.087 Uiso 1 1 calc R . . H21C H 0.0017 0.3893 -0.2167 0.087 Uiso 1 1 calc R . . C22 C 0.1379(7) 0.1581(12) -0.2043(5) 0.066(4) Uani 1 1 d . . . H22A H 0.1062 0.1306 -0.2337 0.079 Uiso 1 1 calc R . . C23 C 0.1833(8) 0.0770(14) -0.1917(6) 0.082(5) Uani 1 1 d . . . H23A H 0.1656 0.0142 -0.1838 0.098 Uiso 1 1 calc R . . H23B H 0.2145 0.0972 -0.1612 0.098 Uiso 1 1 calc R . . H23C H 0.1994 0.0665 -0.2219 0.098 Uiso 1 1 calc R . . C24 C 0.1602(7) 0.2518(14) -0.2266(6) 0.073(4) Uani 1 1 d . . . H24A H 0.1892 0.2861 -0.1987 0.088 Uiso 1 1 calc R . . H24B H 0.1276 0.2976 -0.2409 0.088 Uiso 1 1 calc R . . H24C H 0.1782 0.2320 -0.2546 0.088 Uiso 1 1 calc R . . C25 C 0.0410(5) 0.0901(10) -0.1545(5) 0.052(3) Uani 1 1 d . . . H25A H 0.0134 0.1019 -0.1897 0.062 Uiso 1 1 calc R . . C26 C 0.0600(8) -0.0176(12) -0.1549(8) 0.084(5) Uani 1 1 d . . . H26A H 0.0889 -0.0328 -0.1219 0.101 Uiso 1 1 calc R . . H26B H 0.0773 -0.0282 -0.1844 0.101 Uiso 1 1 calc R . . H26C H 0.0263 -0.0620 -0.1587 0.101 Uiso 1 1 calc R . . C27 C 0.0049(7) 0.1041(13) -0.1147(7) 0.076(4) Uani 1 1 d . . . H27A H -0.0132 0.1710 -0.1193 0.092 Uiso 1 1 calc R . . H27B H 0.0303 0.0981 -0.0791 0.092 Uiso 1 1 calc R . . H27C H -0.0254 0.0523 -0.1203 0.092 Uiso 1 1 calc R . . C28 C 0.0973(5) 0.3291(8) 0.1249(4) 0.036(2) Uani 1 1 d . . . H28A H 0.1336 0.3064 0.1508 0.043 Uiso 1 1 calc R . . C29 C 0.0474(6) 0.3114(11) 0.1510(5) 0.059(3) Uani 1 1 d . . . H29A H 0.0473 0.2407 0.1617 0.071 Uiso 1 1 calc R . . H29B H 0.0101 0.3274 0.1261 0.071 Uiso 1 1 calc R . . H29C H 0.0528 0.3549 0.1820 0.071 Uiso 1 1 calc R . . C30 C 0.1043(6) 0.4438(9) 0.1178(5) 0.049(3) Uani 1 1 d . . . H30A H 0.0701 0.4698 0.0920 0.059 Uiso 1 1 calc R . . H30B H 0.1392 0.4563 0.1055 0.059 Uiso 1 1 calc R . . H30C H 0.1082 0.4780 0.1515 0.059 Uiso 1 1 calc R . . C31 C 0.0968(5) 0.1107(8) 0.0896(4) 0.040(2) Uani 1 1 d . . . H31A H 0.0622 0.0966 0.1034 0.048 Uiso 1 1 calc R . . C32 C 0.1499(6) 0.0900(10) 0.1347(5) 0.051(3) Uani 1 1 d . . . H32A H 0.1487 0.1330 0.1646 0.061 Uiso 1 1 calc R . . H32B H 0.1852 0.1047 0.1235 0.061 Uiso 1 1 calc R . . H32C H 0.1500 0.0191 0.1450 0.061 Uiso 1 1 calc R . . C33 C 0.0938(6) 0.0354(9) 0.0453(5) 0.053(3) Uani 1 1 d . . . H33A H 0.1255 0.0490 0.0287 0.063 Uiso 1 1 calc R . . H33B H 0.0564 0.0421 0.0191 0.063 Uiso 1 1 calc R . . H33C H 0.0978 -0.0332 0.0595 0.063 Uiso 1 1 calc R . . C34 C 0.0150(4) 0.2555(8) 0.0154(4) 0.033(2) Uani 1 1 d . . . H34A H 0.0190 0.2223 -0.0175 0.040 Uiso 1 1 calc R . . C35 C -0.0350(5) 0.2030(10) 0.0311(5) 0.053(3) Uani 1 1 d . . . H35A H -0.0394 0.2318 0.0640 0.063 Uiso 1 1 calc R . . H35B H -0.0266 0.1308 0.0358 0.063 Uiso 1 1 calc R . . H35C H -0.0711 0.2127 0.0035 0.063 Uiso 1 1 calc R . . C36 C -0.0014(5) 0.3672(9) 0.0017(5) 0.047(3) Uani 1 1 d . . . H36A H 0.0283 0.3985 -0.0129 0.056 Uiso 1 1 calc R . . H36B H -0.0035 0.4033 0.0335 0.056 Uiso 1 1 calc R . . H36C H -0.0392 0.3704 -0.0242 0.056 Uiso 1 1 calc R . . C37 C 0.4000(7) 0.5101(13) 0.2606(5) 0.071(4) Uani 1 1 d . . . H37A H 0.4002 0.5679 0.2364 0.085 Uiso 1 1 calc R . . C38 C 0.3540(9) 0.5362(17) 0.2874(7) 0.107(8) Uani 1 1 d . . . H38A H 0.3495 0.4806 0.3105 0.128 Uiso 1 1 calc R . . H38B H 0.3171 0.5475 0.2611 0.128 Uiso 1 1 calc R . . H38C H 0.3652 0.5975 0.3082 0.128 Uiso 1 1 calc R . . C39 C 0.4609(8) 0.5134(16) 0.3003(7) 0.095(6) Uani 1 1 d . . . H39A H 0.4911 0.5120 0.2812 0.115 Uiso 1 1 calc R . . H39B H 0.4654 0.4549 0.3237 0.115 Uiso 1 1 calc R . . H39C H 0.4645 0.5754 0.3211 0.115 Uiso 1 1 calc R . . C40 C 0.4433(5) 0.3923(12) 0.1777(5) 0.057(3) Uani 1 1 d . . . H40A H 0.4271 0.3460 0.1476 0.069 Uiso 1 1 calc R . . C41 C 0.5034(6) 0.3482(15) 0.2054(6) 0.074(4) Uani 1 1 d . . . H41A H 0.4988 0.2780 0.2151 0.089 Uiso 1 1 calc R . . H41B H 0.5206 0.3876 0.2370 0.089 Uiso 1 1 calc R . . H41C H 0.5289 0.3511 0.1816 0.089 Uiso 1 1 calc R . . C42 C 0.4498(7) 0.4948(14) 0.1526(6) 0.075(5) Uani 1 1 d . . . H42A H 0.4624 0.5456 0.1802 0.090 Uiso 1 1 calc R . . H42B H 0.4122 0.5148 0.1293 0.090 Uiso 1 1 calc R . . H42C H 0.4788 0.4893 0.1323 0.090 Uiso 1 1 calc R . . C43 C 0.3950(6) 0.2741(11) 0.2573(5) 0.059(3) Uani 1 1 d . . . H43A H 0.4345 0.2763 0.2825 0.070 Uiso 1 1 calc R . . C44 C 0.3924(9) 0.1795(14) 0.2269(7) 0.089(5) Uani 1 1 d . . . H44A H 0.4237 0.1794 0.2089 0.106 Uiso 1 1 calc R . . H44B H 0.3547 0.1750 0.2008 0.106 Uiso 1 1 calc R . . H44C H 0.3972 0.1216 0.2507 0.106 Uiso 1 1 calc R . . C45 C 0.3507(11) 0.2663(17) 0.2907(8) 0.111(7) Uani 1 1 d . . . H45A H 0.3111 0.2656 0.2676 0.133 Uiso 1 1 calc R . . H45B H 0.3552 0.3244 0.3144 0.133 Uiso 1 1 calc R . . H45C H 0.3576 0.2041 0.3114 0.133 Uiso 1 1 calc R . . C46 C 0.4410(5) 0.2460(9) -0.0608(4) 0.044(2) Uani 1 1 d . . . H46A H 0.4052 0.2172 -0.0852 0.052 Uiso 1 1 calc R . . C47 C 0.4412(7) 0.3567(10) -0.0759(5) 0.062(4) Uani 1 1 d . . . H47A H 0.4740 0.3909 -0.0519 0.074 Uiso 1 1 calc R . . H47B H 0.4047 0.3883 -0.0738 0.074 Uiso 1 1 calc R . . H47C H 0.4452 0.3621 -0.1119 0.074 Uiso 1 1 calc R . . C48 C 0.4918(7) 0.1893(12) -0.0733(6) 0.068(4) Uani 1 1 d . . . H48A H 0.4856 0.1166 -0.0713 0.081 Uiso 1 1 calc R . . H48B H 0.5282 0.2082 -0.0479 0.081 Uiso 1 1 calc R . . H48C H 0.4942 0.2070 -0.1088 0.081 Uiso 1 1 calc R . . C49 C 0.4982(4) 0.2557(9) 0.0620(4) 0.043(2) Uani 1 1 d . . . H49A H 0.4861 0.2526 0.0955 0.052 Uiso 1 1 calc R . . C50 C 0.5171(5) 0.3651(10) 0.0558(6) 0.060(4) Uani 1 1 d . . . H50A H 0.4849 0.4110 0.0562 0.072 Uiso 1 1 calc R . . H50B H 0.5277 0.3720 0.0225 0.072 Uiso 1 1 calc R . . H50C H 0.5508 0.3820 0.0849 0.072 Uiso 1 1 calc R . . C51 C 0.5514(5) 0.1857(11) 0.0685(6) 0.060(3) Uani 1 1 d . . . H51C H 0.5832 0.2100 0.0975 0.072 Uiso 1 1 calc R . . H51B H 0.5640 0.1854 0.0360 0.072 Uiso 1 1 calc R . . H51A H 0.5407 0.1171 0.0762 0.072 Uiso 1 1 calc R . . C52 C 0.4204(5) 0.0761(8) 0.0119(5) 0.044(3) Uani 1 1 d . . . H52A H 0.4557 0.0415 0.0065 0.053 Uiso 1 1 calc R . . C53 C 0.3693(6) 0.0379(9) -0.0299(6) 0.057(3) Uani 1 1 d . . . H53A H 0.3753 0.0521 -0.0645 0.069 Uiso 1 1 calc R . . H53B H 0.3337 0.0716 -0.0266 0.069 Uiso 1 1 calc R . . H53C H 0.3654 -0.0350 -0.0258 0.069 Uiso 1 1 calc R . . C54 C 0.4150(6) 0.0458(9) 0.0659(6) 0.056(3) Uani 1 1 d . . . H54C H 0.4087 -0.0271 0.0668 0.067 Uiso 1 1 calc R . . H54B H 0.3820 0.0812 0.0735 0.067 Uiso 1 1 calc R . . H54A H 0.4508 0.0638 0.0923 0.067 Uiso 1 1 calc R . . C55 C 0.1794(8) 0.7720(11) -0.0930(6) 0.075(4) Uani 1 1 d . . . H55A H 0.1886 0.7298 -0.0615 0.090 Uiso 1 1 calc R . . H55B H 0.1388 0.7613 -0.1124 0.090 Uiso 1 1 calc R . . H55C H 0.1853 0.8431 -0.0828 0.090 Uiso 1 1 calc R . . C56 C 0.2697(16) 0.806(3) -0.1296(14) 0.077(9) Uiso 0.50 1 d P . . C57 C 0.2394(16) 0.824(3) -0.1589(14) 0.078(9) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0334(13) 0.0322(14) 0.0351(13) -0.0069(11) 0.0105(11) 0.0005(11) Si2 0.0356(14) 0.0363(15) 0.0351(13) 0.0091(11) 0.0118(11) 0.0030(12) Si3 0.0440(16) 0.0469(17) 0.0328(14) -0.0009(12) 0.0052(12) -0.0129(14) Si4 0.0309(13) 0.0297(13) 0.0306(12) 0.0042(10) 0.0095(10) 0.0006(11) Si5 0.0289(13) 0.0283(13) 0.0409(14) -0.0004(11) 0.0124(11) 0.0030(10) Si6 0.0432(16) 0.0513(18) 0.0280(13) 0.0032(12) 0.0045(12) -0.0003(14) Sb1 0.0353(3) 0.0258(3) 0.0289(3) -0.0033(2) 0.0108(2) -0.0002(2) Sb2 0.0387(4) 0.0398(4) 0.0282(3) 0.0072(3) 0.0108(3) 0.0067(3) Sb3 0.0382(3) 0.0357(4) 0.0320(3) -0.0039(3) 0.0073(3) -0.0022(3) Sb4 0.0276(3) 0.0304(3) 0.0319(3) 0.0022(2) 0.0086(2) -0.0013(2) Sb5 0.0262(3) 0.0290(3) 0.0347(3) -0.0014(2) 0.0086(2) 0.0036(2) Sb6 0.0350(3) 0.0383(4) 0.0287(3) -0.0001(3) 0.0105(3) 0.0016(3) Pb1 0.0374(2) 0.0320(2) 0.0385(2) 0.00067(15) 0.01497(16) 0.00006(15) Pb2 0.03361(19) 0.0321(2) 0.03596(19) 0.00295(14) 0.01058(15) 0.00291(15) Pb3 0.0364(2) 0.0458(2) 0.03088(18) -0.00516(16) 0.01199(15) -0.00057(17) Pb4 0.03477(19) 0.02964(19) 0.03583(19) 0.00273(14) 0.01013(15) 0.00250(15) C1 0.044(6) 0.033(6) 0.067(7) -0.012(5) 0.025(5) -0.001(5) C2 0.037(6) 0.059(8) 0.074(9) -0.011(7) 0.015(6) 0.001(6) C3 0.060(8) 0.069(9) 0.062(8) -0.001(7) 0.036(7) 0.013(7) C4 0.036(5) 0.048(6) 0.044(6) -0.014(5) 0.006(5) -0.002(5) C5 0.042(6) 0.067(9) 0.062(8) -0.015(7) 0.006(6) -0.006(6) C6 0.055(8) 0.123(15) 0.082(10) -0.071(11) 0.017(8) -0.020(9) C7 0.055(7) 0.038(6) 0.052(7) 0.002(5) 0.010(5) 0.006(5) C8 0.093(11) 0.055(8) 0.047(7) 0.015(6) 0.025(7) 0.011(7) C9 0.126(15) 0.036(7) 0.108(13) 0.011(8) 0.041(12) 0.028(9) C10 0.032(5) 0.054(7) 0.049(6) 0.023(5) 0.013(5) 0.001(5) C11 0.047(7) 0.061(8) 0.080(9) 0.015(7) 0.023(7) 0.001(6) C12 0.045(7) 0.109(13) 0.052(7) 0.035(8) -0.005(6) -0.011(8) C13 0.042(6) 0.053(7) 0.040(6) 0.015(5) 0.011(5) -0.001(5) C14 0.081(10) 0.057(8) 0.070(9) 0.001(7) 0.046(8) -0.002(7) C15 0.035(7) 0.145(17) 0.067(9) 0.037(10) 0.014(6) -0.002(8) C16 0.137(17) 0.042(8) 0.113(14) 0.001(8) 0.069(13) -0.012(9) C19 0.049(7) 0.046(7) 0.041(6) 0.007(5) -0.004(5) -0.008(5) C20 0.057(7) 0.049(7) 0.047(6) 0.007(5) 0.006(6) 0.001(6) C21 0.077(10) 0.076(10) 0.050(7) 0.010(7) -0.011(7) -0.002(8) C22 0.073(9) 0.079(10) 0.045(7) -0.019(7) 0.016(6) -0.026(8) C23 0.093(12) 0.092(12) 0.065(9) -0.031(9) 0.031(9) -0.014(10) C24 0.066(9) 0.103(12) 0.051(8) 0.007(8) 0.017(7) -0.018(9) C25 0.048(7) 0.059(8) 0.040(6) -0.001(5) -0.001(5) -0.020(6) C26 0.090(12) 0.061(10) 0.107(13) -0.031(9) 0.034(10) -0.030(9) C27 0.071(10) 0.069(10) 0.089(11) -0.007(8) 0.021(8) -0.026(8) C28 0.040(5) 0.031(5) 0.039(5) -0.005(4) 0.016(4) -0.001(4) C29 0.062(8) 0.069(9) 0.055(7) -0.005(6) 0.032(6) -0.008(7) C30 0.064(8) 0.038(6) 0.046(6) -0.010(5) 0.013(6) 0.005(5) C31 0.040(5) 0.032(5) 0.050(6) 0.008(5) 0.016(5) 0.002(4) C32 0.059(7) 0.048(7) 0.047(6) 0.010(5) 0.017(6) 0.014(6) C33 0.067(8) 0.030(6) 0.064(7) 0.004(5) 0.022(6) 0.003(5) C34 0.027(5) 0.035(5) 0.038(5) 0.001(4) 0.009(4) -0.002(4) C35 0.031(5) 0.061(8) 0.063(7) 0.004(6) 0.007(5) -0.015(5) C36 0.039(6) 0.041(6) 0.058(7) 0.011(5) 0.007(5) 0.004(5) C37 0.071(9) 0.086(11) 0.042(7) -0.008(7) -0.010(7) 0.001(8) C38 0.097(14) 0.127(17) 0.081(12) -0.054(12) -0.003(10) 0.033(13) C39 0.085(12) 0.116(16) 0.071(10) -0.035(10) -0.008(9) 0.000(11) C40 0.032(6) 0.097(11) 0.042(6) 0.007(6) 0.007(5) 0.007(6) C41 0.045(7) 0.112(14) 0.064(8) 0.001(8) 0.013(7) 0.016(8) C42 0.054(8) 0.111(13) 0.059(8) 0.023(8) 0.010(7) -0.013(8) C43 0.054(7) 0.061(8) 0.050(7) 0.014(6) -0.007(6) 0.001(6) C44 0.100(13) 0.076(12) 0.079(11) 0.012(9) 0.006(10) -0.003(10) C45 0.144(19) 0.113(16) 0.081(12) 0.038(12) 0.039(13) -0.019(15) C46 0.044(6) 0.043(6) 0.046(6) 0.003(5) 0.016(5) 0.005(5) C47 0.083(10) 0.056(8) 0.056(7) 0.008(6) 0.034(7) -0.015(7) C48 0.068(9) 0.080(10) 0.067(9) 0.011(7) 0.040(7) 0.022(8) C49 0.030(5) 0.054(7) 0.042(6) 0.003(5) 0.005(4) 0.000(5) C50 0.041(6) 0.050(7) 0.076(9) -0.007(6) -0.006(6) -0.004(6) C51 0.040(6) 0.067(9) 0.065(8) 0.001(7) 0.001(6) 0.012(6) C52 0.042(6) 0.027(5) 0.068(7) 0.001(5) 0.023(5) 0.005(4) C53 0.053(7) 0.032(6) 0.092(10) -0.015(6) 0.029(7) -0.005(5) C54 0.052(7) 0.037(6) 0.086(9) 0.017(6) 0.032(7) 0.012(5) C55 0.102(12) 0.048(8) 0.075(10) -0.007(7) 0.024(9) 0.013(8) _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 Si1 C4 1.890(11) . ? Si1 C1 1.899(12) . ? Si1 C7 1.900(12) . ? Si1 Sb1 2.599(3) . ? Si2 C16 1.880(17) . ? Si2 C13 1.891(12) . ? Si2 C10 1.907(11) . ? Si2 Sb2 2.578(3) . ? Si3 C19 1.896(13) . ? Si3 C25 1.908(12) . ? Si3 C22 1.945(15) . ? Si3 Sb3 2.599(3) . ? Si4 C28 1.886(10) . ? Si4 C31 1.889(11) . ? Si4 C34 1.911(10) . ? Si4 Sb4 2.607(3) . ? Si5 C49 1.890(11) . ? Si5 C46 1.901(12) . ? Si5 C52 1.903(11) . ? Si5 Sb5 2.563(3) . ? Si6 C40 1.874(13) . ? Si6 C37 1.902(15) . ? Si6 C43 1.912(13) . ? Si6 Sb6 2.607(3) . ? Sb1 Sb6 2.8162(10) . ? Sb1 Pb1 3.0006(10) . ? Sb1 Pb2 3.0077(13) . ? Sb2 Pb2 2.9466(11) . ? Sb2 Pb3 2.9728(10) . ? Sb2 Pb1 3.0143(13) . ? Sb3 Sb4 2.8255(10) . ? Sb3 Pb3 2.9574(10) . ? Sb4 Pb4 2.9774(12) . ? Sb4 Pb2 2.9894(9) . ? Sb5 Pb1 2.9456(10) . ? Sb5 Pb4 2.9605(10) . ? Sb5 Pb3 2.9700(12) . ? Sb6 Pb4 2.9482(9) . ? C1 C2 1.504(16) . ? C1 C3 1.522(18) . ? C4 C5 1.531(18) . ? C4 C6 1.561(17) . ? C7 C8 1.513(19) . ? C7 C9 1.572(18) . ? C10 C11 1.507(17) . ? C10 C12 1.518(16) . ? C13 C14 1.519(18) . ? C13 C15 1.527(17) . ? C16 C56 1.47(4) . ? C16 C57 1.49(4) . ? C16 C55 1.53(3) . ? C19 C20 1.499(18) . ? C19 C21 1.546(16) . ? C22 C23 1.50(2) . ? C22 C24 1.53(2) . ? C25 C26 1.50(2) . ? C25 C27 1.53(2) . ? C28 C29 1.539(16) . ? C28 C30 1.548(15) . ? C31 C32 1.518(15) . ? C31 C33 1.526(17) . ? C34 C35 1.525(15) . ? C34 C36 1.551(15) . ? C37 C38 1.49(3) . ? C37 C39 1.55(2) . ? C40 C42 1.54(2) . ? C40 C41 1.542(17) . ? C43 C44 1.48(2) . ? C43 C45 1.54(3) . ? C46 C47 1.523(17) . ? C46 C48 1.532(17) . ? C49 C50 1.540(17) . ? C49 C51 1.541(16) . ? C52 C53 1.501(17) . ? C52 C54 1.519(18) . ? C56 C57 0.94(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Si1 C1 108.9(5) . . ? C4 Si1 C7 113.7(6) . . ? C1 Si1 C7 109.8(6) . . ? C4 Si1 Sb1 108.5(4) . . ? C1 Si1 Sb1 110.0(4) . . ? C7 Si1 Sb1 105.9(4) . . ? C16 Si2 C13 110.6(7) . . ? C16 Si2 C10 112.8(8) . . ? C13 Si2 C10 107.3(5) . . ? C16 Si2 Sb2 109.2(6) . . ? C13 Si2 Sb2 107.1(4) . . ? C10 Si2 Sb2 109.7(3) . . ? C19 Si3 C25 109.6(6) . . ? C19 Si3 C22 108.3(7) . . ? C25 Si3 C22 105.7(6) . . ? C19 Si3 Sb3 115.9(3) . . ? C25 Si3 Sb3 110.0(4) . . ? C22 Si3 Sb3 106.8(5) . . ? C28 Si4 C31 107.4(5) . . ? C28 Si4 C34 114.6(5) . . ? C31 Si4 C34 107.0(5) . . ? C28 Si4 Sb4 107.0(3) . . ? C31 Si4 Sb4 111.5(4) . . ? C34 Si4 Sb4 109.3(3) . . ? C49 Si5 C46 113.8(5) . . ? C49 Si5 C52 109.5(5) . . ? C46 Si5 C52 108.1(5) . . ? C49 Si5 Sb5 110.2(4) . . ? C46 Si5 Sb5 107.3(4) . . ? C52 Si5 Sb5 107.9(4) . . ? C40 Si6 C37 109.1(7) . . ? C40 Si6 C43 108.5(7) . . ? C37 Si6 C43 110.5(7) . . ? C40 Si6 Sb6 114.3(4) . . ? C37 Si6 Sb6 107.8(5) . . ? C43 Si6 Sb6 106.7(4) . . ? Si1 Sb1 Sb6 110.99(7) . . ? Si1 Sb1 Pb1 112.87(7) . . ? Sb6 Sb1 Pb1 119.78(3) . . ? Si1 Sb1 Pb2 106.40(6) . . ? Sb6 Sb1 Pb2 108.04(3) . . ? Pb1 Sb1 Pb2 96.87(3) . . ? Si2 Sb2 Pb2 114.75(7) . . ? Si2 Sb2 Pb3 115.82(7) . . ? Pb2 Sb2 Pb3 117.90(3) . . ? Si2 Sb2 Pb1 114.29(7) . . ? Pb2 Sb2 Pb1 97.89(3) . . ? Pb3 Sb2 Pb1 92.16(2) . . ? Si3 Sb3 Sb4 114.97(8) . . ? Si3 Sb3 Pb3 95.19(7) . . ? Sb4 Sb3 Pb3 95.45(3) . . ? Si4 Sb4 Sb3 113.67(7) . . ? Si4 Sb4 Pb4 106.08(6) . . ? Sb3 Sb4 Pb4 93.09(3) . . ? Si4 Sb4 Pb2 107.20(6) . . ? Sb3 Sb4 Pb2 118.31(3) . . ? Pb4 Sb4 Pb2 117.66(2) . . ? Si5 Sb5 Pb1 112.14(7) . . ? Si5 Sb5 Pb4 117.01(7) . . ? Pb1 Sb5 Pb4 120.39(2) . . ? Si5 Sb5 Pb3 97.24(7) . . ? Pb1 Sb5 Pb3 93.61(2) . . ? Pb4 Sb5 Pb3 110.92(3) . . ? Si6 Sb6 Sb1 108.27(8) . . ? Si6 Sb6 Pb4 99.06(8) . . ? Sb1 Sb6 Pb4 96.61(3) . . ? Sb5 Pb1 Sb1 86.73(2) . . ? Sb5 Pb1 Sb2 79.83(2) . . ? Sb1 Pb1 Sb2 82.06(3) . . ? Sb2 Pb2 Sb4 88.41(2) . . ? Sb2 Pb2 Sb1 83.08(3) . . ? Sb4 Pb2 Sb1 88.17(2) . . ? Sb3 Pb3 Sb5 93.43(3) . . ? Sb3 Pb3 Sb2 100.64(3) . . ? Sb5 Pb3 Sb2 80.12(2) . . ? Sb6 Pb4 Sb5 99.84(3) . . ? Sb6 Pb4 Sb4 88.37(3) . . ? Sb5 Pb4 Sb4 87.12(3) . . ? C2 C1 C3 111.0(11) . . ? C2 C1 Si1 114.1(9) . . ? C3 C1 Si1 112.5(8) . . ? C5 C4 C6 108.4(11) . . ? C5 C4 Si1 114.6(8) . . ? C6 C4 Si1 112.9(9) . . ? C8 C7 C9 107.8(12) . . ? C8 C7 Si1 116.7(9) . . ? C9 C7 Si1 111.0(10) . . ? C11 C10 C12 109.4(11) . . ? C11 C10 Si2 114.1(9) . . ? C12 C10 Si2 113.6(8) . . ? C14 C13 C15 110.3(13) . . ? C14 C13 Si2 113.9(9) . . ? C15 C13 Si2 113.9(9) . . ? C56 C16 C57 37.1(17) . . ? C56 C16 C55 121(2) . . ? C57 C16 C55 119.3(19) . . ? C56 C16 Si2 120.7(19) . . ? C57 C16 Si2 119.7(18) . . ? C55 C16 Si2 115.7(12) . . ? C20 C19 C21 109.0(11) . . ? C20 C19 Si3 116.5(8) . . ? C21 C19 Si3 110.9(9) . . ? C23 C22 C24 111.6(14) . . ? C23 C22 Si3 114.8(11) . . ? C24 C22 Si3 113.3(11) . . ? C26 C25 C27 110.2(13) . . ? C26 C25 Si3 115.4(10) . . ? C27 C25 Si3 113.5(9) . . ? C29 C28 C30 108.9(10) . . ? C29 C28 Si4 110.7(8) . . ? C30 C28 Si4 118.1(7) . . ? C32 C31 C33 110.2(10) . . ? C32 C31 Si4 115.1(8) . . ? C33 C31 Si4 112.4(8) . . ? C35 C34 C36 109.5(9) . . ? C35 C34 Si4 114.9(7) . . ? C36 C34 Si4 111.0(7) . . ? C38 C37 C39 110.2(13) . . ? C38 C37 Si6 117.4(13) . . ? C39 C37 Si6 114.1(12) . . ? C42 C40 C41 110.8(12) . . ? C42 C40 Si6 112.6(11) . . ? C41 C40 Si6 116.7(9) . . ? C44 C43 C45 108.4(15) . . ? C44 C43 Si6 114.6(11) . . ? C45 C43 Si6 113.6(12) . . ? C47 C46 C48 111.0(11) . . ? C47 C46 Si5 116.9(9) . . ? C48 C46 Si5 112.6(8) . . ? C50 C49 C51 109.1(10) . . ? C50 C49 Si5 112.3(8) . . ? C51 C49 Si5 114.1(9) . . ? C53 C52 C54 110.5(11) . . ? C53 C52 Si5 113.6(8) . . ? C54 C52 Si5 111.6(8) . . ? C57 C56 C16 73(3) . . ? C56 C57 C16 70(3) . . ? 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 C4 Si1 Sb1 Sb6 64.3(4) . . . . ? C1 Si1 Sb1 Sb6 -54.7(4) . . . . ? C7 Si1 Sb1 Sb6 -173.4(4) . . . . ? C4 Si1 Sb1 Pb1 -73.4(4) . . . . ? C1 Si1 Sb1 Pb1 167.6(4) . . . . ? C7 Si1 Sb1 Pb1 49.0(4) . . . . ? C4 Si1 Sb1 Pb2 -178.4(4) . . . . ? C1 Si1 Sb1 Pb2 62.6(4) . . . . ? C7 Si1 Sb1 Pb2 -56.1(4) . . . . ? C16 Si2 Sb2 Pb2 57.5(7) . . . . ? C13 Si2 Sb2 Pb2 177.3(4) . . . . ? C10 Si2 Sb2 Pb2 -66.6(4) . . . . ? C16 Si2 Sb2 Pb3 -159.8(7) . . . . ? C13 Si2 Sb2 Pb3 -40.0(4) . . . . ? C10 Si2 Sb2 Pb3 76.1(4) . . . . ? C16 Si2 Sb2 Pb1 -54.5(7) . . . . ? C13 Si2 Sb2 Pb1 65.3(4) . . . . ? C10 Si2 Sb2 Pb1 -178.5(4) . . . . ? C19 Si3 Sb3 Sb4 25.6(5) . . . . ? C25 Si3 Sb3 Sb4 -99.3(5) . . . . ? C22 Si3 Sb3 Sb4 146.4(5) . . . . ? C19 Si3 Sb3 Pb3 -72.8(5) . . . . ? C25 Si3 Sb3 Pb3 162.2(5) . . . . ? C22 Si3 Sb3 Pb3 48.0(5) . . . . ? C28 Si4 Sb4 Sb3 171.5(3) . . . . ? C31 Si4 Sb4 Sb3 54.3(4) . . . . ? C34 Si4 Sb4 Sb3 -63.9(4) . . . . ? C28 Si4 Sb4 Pb4 70.7(4) . . . . ? C31 Si4 Sb4 Pb4 -46.5(4) . . . . ? C34 Si4 Sb4 Pb4 -164.7(3) . . . . ? C28 Si4 Sb4 Pb2 -55.8(4) . . . . ? C31 Si4 Sb4 Pb2 -173.0(4) . . . . ? C34 Si4 Sb4 Pb2 68.8(4) . . . . ? Si3 Sb3 Sb4 Si4 76.89(10) . . . . ? Pb3 Sb3 Sb4 Si4 175.21(6) . . . . ? Si3 Sb3 Sb4 Pb4 -174.05(8) . . . . ? Pb3 Sb3 Sb4 Pb4 -75.73(3) . . . . ? Si3 Sb3 Sb4 Pb2 -50.19(9) . . . . ? Pb3 Sb3 Sb4 Pb2 48.13(4) . . . . ? C49 Si5 Sb5 Pb1 63.4(4) . . . . ? C46 Si5 Sb5 Pb1 -61.0(4) . . . . ? C52 Si5 Sb5 Pb1 -177.2(4) . . . . ? C49 Si5 Sb5 Pb4 -81.7(4) . . . . ? C46 Si5 Sb5 Pb4 153.9(4) . . . . ? C52 Si5 Sb5 Pb4 37.7(4) . . . . ? C49 Si5 Sb5 Pb3 160.3(4) . . . . ? C46 Si5 Sb5 Pb3 36.0(4) . . . . ? C52 Si5 Sb5 Pb3 -80.2(4) . . . . ? C40 Si6 Sb6 Sb1 -45.5(6) . . . . ? C37 Si6 Sb6 Sb1 75.9(6) . . . . ? C43 Si6 Sb6 Sb1 -165.4(5) . . . . ? C40 Si6 Sb6 Pb4 54.6(6) . . . . ? C37 Si6 Sb6 Pb4 176.0(6) . . . . ? C43 Si6 Sb6 Pb4 -65.3(5) . . . . ? Si1 Sb1 Sb6 Si6 -78.07(11) . . . . ? Pb1 Sb1 Sb6 Si6 56.29(8) . . . . ? Pb2 Sb1 Sb6 Si6 165.64(8) . . . . ? Si1 Sb1 Sb6 Pb4 -179.91(7) . . . . ? Pb1 Sb1 Sb6 Pb4 -45.55(4) . . . . ? Pb2 Sb1 Sb6 Pb4 63.79(3) . . . . ? Si5 Sb5 Pb1 Sb1 -150.06(7) . . . . ? Pb4 Sb5 Pb1 Sb1 -6.24(3) . . . . ? Pb3 Sb5 Pb1 Sb1 110.62(3) . . . . ? Si5 Sb5 Pb1 Sb2 127.42(7) . . . . ? Pb4 Sb5 Pb1 Sb2 -88.76(3) . . . . ? Pb3 Sb5 Pb1 Sb2 28.10(2) . . . . ? Si1 Sb1 Pb1 Sb5 166.37(7) . . . . ? Sb6 Sb1 Pb1 Sb5 32.80(3) . . . . ? Pb2 Sb1 Pb1 Sb5 -82.57(2) . . . . ? Si1 Sb1 Pb1 Sb2 -113.45(7) . . . . ? Sb6 Sb1 Pb1 Sb2 112.98(3) . . . . ? Pb2 Sb1 Pb1 Sb2 -2.39(2) . . . . ? Si2 Sb2 Pb1 Sb5 -147.73(8) . . . . ? Pb2 Sb2 Pb1 Sb5 90.52(2) . . . . ? Pb3 Sb2 Pb1 Sb5 -28.04(2) . . . . ? Si2 Sb2 Pb1 Sb1 124.20(8) . . . . ? Pb2 Sb2 Pb1 Sb1 2.44(2) . . . . ? Pb3 Sb2 Pb1 Sb1 -116.11(2) . . . . ? Si2 Sb2 Pb2 Sb4 147.81(8) . . . . ? Pb3 Sb2 Pb2 Sb4 5.91(3) . . . . ? Pb1 Sb2 Pb2 Sb4 -90.78(2) . . . . ? Si2 Sb2 Pb2 Sb1 -123.84(8) . . . . ? Pb3 Sb2 Pb2 Sb1 94.26(3) . . . . ? Pb1 Sb2 Pb2 Sb1 -2.43(2) . . . . ? Si4 Sb4 Pb2 Sb2 -164.61(6) . . . . ? Sb3 Sb4 Pb2 Sb2 -34.50(3) . . . . ? Pb4 Sb4 Pb2 Sb2 76.07(3) . . . . ? Si4 Sb4 Pb2 Sb1 112.27(6) . . . . ? Sb3 Sb4 Pb2 Sb1 -117.63(4) . . . . ? Pb4 Sb4 Pb2 Sb1 -7.05(3) . . . . ? Si1 Sb1 Pb2 Sb2 118.76(7) . . . . ? Sb6 Sb1 Pb2 Sb2 -121.99(3) . . . . ? Pb1 Sb1 Pb2 Sb2 2.44(2) . . . . ? Si1 Sb1 Pb2 Sb4 -152.62(7) . . . . ? Sb6 Sb1 Pb2 Sb4 -33.37(3) . . . . ? Pb1 Sb1 Pb2 Sb4 91.06(2) . . . . ? Si3 Sb3 Pb3 Sb5 161.96(8) . . . . ? Sb4 Sb3 Pb3 Sb5 46.21(3) . . . . ? Si3 Sb3 Pb3 Sb2 81.38(8) . . . . ? Sb4 Sb3 Pb3 Sb2 -34.37(3) . . . . ? Si5 Sb5 Pb3 Sb3 118.41(7) . . . . ? Pb1 Sb5 Pb3 Sb3 -128.72(2) . . . . ? Pb4 Sb5 Pb3 Sb3 -4.19(3) . . . . ? Si5 Sb5 Pb3 Sb2 -141.38(7) . . . . ? Pb1 Sb5 Pb3 Sb2 -28.50(2) . . . . ? Pb4 Sb5 Pb3 Sb2 96.03(3) . . . . ? Si2 Sb2 Pb3 Sb3 -122.18(8) . . . . ? Pb2 Sb2 Pb3 Sb3 19.32(3) . . . . ? Pb1 Sb2 Pb3 Sb3 119.43(3) . . . . ? Si2 Sb2 Pb3 Sb5 146.15(8) . . . . ? Pb2 Sb2 Pb3 Sb5 -72.35(3) . . . . ? Pb1 Sb2 Pb3 Sb5 27.76(2) . . . . ? Si6 Sb6 Pb4 Sb5 -78.44(8) . . . . ? Sb1 Sb6 Pb4 Sb5 31.32(3) . . . . ? Si6 Sb6 Pb4 Sb4 -165.24(7) . . . . ? Sb1 Sb6 Pb4 Sb4 -55.47(3) . . . . ? Si5 Sb5 Pb4 Sb6 125.09(8) . . . . ? Pb1 Sb5 Pb4 Sb6 -17.04(3) . . . . ? Pb3 Sb5 Pb4 Sb6 -124.64(2) . . . . ? Si5 Sb5 Pb4 Sb4 -147.06(7) . . . . ? Pb1 Sb5 Pb4 Sb4 70.80(3) . . . . ? Pb3 Sb5 Pb4 Sb4 -36.80(3) . . . . ? Si4 Sb4 Pb4 Sb6 -79.03(7) . . . . ? Sb3 Sb4 Pb4 Sb6 165.25(2) . . . . ? Pb2 Sb4 Pb4 Sb6 40.88(3) . . . . ? Si4 Sb4 Pb4 Sb5 -178.97(7) . . . . ? Sb3 Sb4 Pb4 Sb5 65.31(3) . . . . ? Pb2 Sb4 Pb4 Sb5 -59.06(3) . . . . ? C4 Si1 C1 C2 175.2(9) . . . . ? C7 Si1 C1 C2 50.2(10) . . . . ? Sb1 Si1 C1 C2 -66.0(9) . . . . ? C4 Si1 C1 C3 -57.2(10) . . . . ? C7 Si1 C1 C3 177.8(9) . . . . ? Sb1 Si1 C1 C3 61.6(9) . . . . ? C1 Si1 C4 C5 -172.4(9) . . . . ? C7 Si1 C4 C5 -49.6(11) . . . . ? Sb1 Si1 C4 C5 67.9(10) . . . . ? C1 Si1 C4 C6 -47.7(13) . . . . ? C7 Si1 C4 C6 75.1(12) . . . . ? Sb1 Si1 C4 C6 -167.4(10) . . . . ? C4 Si1 C7 C8 65.4(11) . . . . ? C1 Si1 C7 C8 -172.4(10) . . . . ? Sb1 Si1 C7 C8 -53.6(10) . . . . ? C4 Si1 C7 C9 -58.7(12) . . . . ? C1 Si1 C7 C9 63.6(12) . . . . ? Sb1 Si1 C7 C9 -177.7(10) . . . . ? C16 Si2 C10 C11 -57.1(11) . . . . ? C13 Si2 C10 C11 -179.1(9) . . . . ? Sb2 Si2 C10 C11 64.9(9) . . . . ? C16 Si2 C10 C12 69.2(13) . . . . ? C13 Si2 C10 C12 -52.9(12) . . . . ? Sb2 Si2 C10 C12 -168.9(10) . . . . ? C16 Si2 C13 C14 -168.1(11) . . . . ? C10 Si2 C13 C14 -44.7(10) . . . . ? Sb2 Si2 C13 C14 73.0(9) . . . . ? C16 Si2 C13 C15 64.3(13) . . . . ? C10 Si2 C13 C15 -172.4(11) . . . . ? Sb2 Si2 C13 C15 -54.7(11) . . . . ? C13 Si2 C16 C56 -12(2) . . . . ? C10 Si2 C16 C56 -133(2) . . . . ? Sb2 Si2 C16 C56 105(2) . . . . ? C13 Si2 C16 C57 31(2) . . . . ? C10 Si2 C16 C57 -89(2) . . . . ? Sb2 Si2 C16 C57 148(2) . . . . ? C13 Si2 C16 C55 -175.1(13) . . . . ? C10 Si2 C16 C55 64.7(16) . . . . ? Sb2 Si2 C16 C55 -57.5(16) . . . . ? C25 Si3 C19 C20 74.7(10) . . . . ? C22 Si3 C19 C20 -170.4(9) . . . . ? Sb3 Si3 C19 C20 -50.5(10) . . . . ? C25 Si3 C19 C21 -50.7(11) . . . . ? C22 Si3 C19 C21 64.1(11) . . . . ? Sb3 Si3 C19 C21 -175.9(8) . . . . ? C19 Si3 C22 C23 159.4(10) . . . . ? C25 Si3 C22 C23 -83.2(11) . . . . ? Sb3 Si3 C22 C23 33.9(11) . . . . ? C19 Si3 C22 C24 29.6(12) . . . . ? C25 Si3 C22 C24 147.0(10) . . . . ? Sb3 Si3 C22 C24 -95.9(11) . . . . ? C19 Si3 C25 C26 170.4(11) . . . . ? C22 Si3 C25 C26 53.8(12) . . . . ? Sb3 Si3 C25 C26 -61.1(11) . . . . ? C19 Si3 C25 C27 -61.1(11) . . . . ? C22 Si3 C25 C27 -177.6(11) . . . . ? Sb3 Si3 C25 C27 67.5(11) . . . . ? C31 Si4 C28 C29 -64.9(9) . . . . ? C34 Si4 C28 C29 53.8(9) . . . . ? Sb4 Si4 C28 C29 175.2(7) . . . . ? C31 Si4 C28 C30 168.6(8) . . . . ? C34 Si4 C28 C30 -72.6(9) . . . . ? Sb4 Si4 C28 C30 48.7(9) . . . . ? C28 Si4 C31 C32 -49.7(10) . . . . ? C34 Si4 C31 C32 -173.2(8) . . . . ? Sb4 Si4 C31 C32 67.2(9) . . . . ? C28 Si4 C31 C33 -177.0(8) . . . . ? C34 Si4 C31 C33 59.5(10) . . . . ? Sb4 Si4 C31 C33 -60.1(9) . . . . ? C28 Si4 C34 C35 -75.4(10) . . . . ? C31 Si4 C34 C35 43.6(10) . . . . ? Sb4 Si4 C34 C35 164.5(8) . . . . ? C28 Si4 C34 C36 49.5(9) . . . . ? C31 Si4 C34 C36 168.4(8) . . . . ? Sb4 Si4 C34 C36 -70.6(8) . . . . ? C40 Si6 C37 C38 169.1(13) . . . . ? C43 Si6 C37 C38 -71.7(14) . . . . ? Sb6 Si6 C37 C38 44.5(14) . . . . ? C40 Si6 C37 C39 -59.8(15) . . . . ? C43 Si6 C37 C39 59.4(15) . . . . ? Sb6 Si6 C37 C39 175.6(12) . . . . ? C37 Si6 C40 C42 -47.4(11) . . . . ? C43 Si6 C40 C42 -167.8(9) . . . . ? Sb6 Si6 C40 C42 73.3(10) . . . . ? C37 Si6 C40 C41 82.4(13) . . . . ? C43 Si6 C40 C41 -38.0(14) . . . . ? Sb6 Si6 C40 C41 -156.9(11) . . . . ? C40 Si6 C43 C44 -54.0(13) . . . . ? C37 Si6 C43 C44 -173.5(12) . . . . ? Sb6 Si6 C43 C44 69.6(13) . . . . ? C40 Si6 C43 C45 -179.4(12) . . . . ? C37 Si6 C43 C45 61.1(13) . . . . ? Sb6 Si6 C43 C45 -55.8(12) . . . . ? C49 Si5 C46 C47 -68.3(11) . . . . ? C52 Si5 C46 C47 170.0(9) . . . . ? Sb5 Si5 C46 C47 53.9(10) . . . . ? C49 Si5 C46 C48 62.0(11) . . . . ? C52 Si5 C46 C48 -59.7(11) . . . . ? Sb5 Si5 C46 C48 -175.8(9) . . . . ? C46 Si5 C49 C50 49.8(11) . . . . ? C52 Si5 C49 C50 170.8(9) . . . . ? Sb5 Si5 C49 C50 -70.7(10) . . . . ? C46 Si5 C49 C51 -74.9(11) . . . . ? C52 Si5 C49 C51 46.1(11) . . . . ? Sb5 Si5 C49 C51 164.6(9) . . . . ? C49 Si5 C52 C53 180.0(9) . . . . ? C46 Si5 C52 C53 -55.6(10) . . . . ? Sb5 Si5 C52 C53 60.1(9) . . . . ? C49 Si5 C52 C54 54.2(10) . . . . ? C46 Si5 C52 C54 178.6(8) . . . . ? Sb5 Si5 C52 C54 -65.7(9) . . . . ? C55 C16 C56 C57 -98(4) . . . . ? Si2 C16 C56 C57 100(3) . . . . ? C55 C16 C57 C56 104(4) . . . . ? Si2 C16 C57 C56 -103(3) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 6.737 _refine_diff_density_min -1.243 _refine_diff_density_rms 0.210