# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Carsten von Hanisch' _publ_contact_author_address ;Fachbereich Chemie, Universit\"at Marburg Hans-Meerwein-Str. 35032 Marburg, Germany ; _publ_contact_author_email haenisch@chemie.uni-marburg.de _publ_author_name 'Carsten von Hanisch' data_d:\struk\c-com2\v2-neu\verb-2 _database_code_depnum_ccdc_archive 'CCDC 876450' #TrackingRef '- Comp-2-CvH.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H92 Si4 Sn2 Te4' _chemical_formula_sum 'C56 H92 Si4 Sn2 Te4' _chemical_formula_weight 1625.44 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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 29.684(3) _cell_length_b 8.3463(5) _cell_length_c 30.084(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.768(6) _cell_angle_gamma 90.00 _cell_volume 6533.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 388 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 20.97 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.449 _exptl_crystal_size_mid 0.029 _exptl_crystal_size_min 0.024 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 2.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5677 _exptl_absorpt_correction_T_max 0.6244 _exptl_special_details ; ? ; _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 IPDS2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24640 _diffrn_reflns_av_R_equivalents 0.1726 _diffrn_reflns_av_sigmaI/netI 0.2593 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 22.73 _reflns_number_total 8634 _reflns_number_gt 3644 _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^)+(0.0000P)^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 8634 _refine_ls_number_parameters 595 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1948 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 0.815 _refine_ls_restrained_S_all 0.812 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.3755(2) 0.7328(7) 0.5188(2) 0.0446(16) Uani 1 1 d . . . Si2 Si 0.1404(2) 0.6786(8) 0.2574(2) 0.0440(16) Uani 1 1 d . . . Si3 Si 0.3563(2) 1.0540(8) 0.2655(2) 0.0453(17) Uani 1 1 d . . . Si4 Si 0.1334(2) 1.1338(7) 0.47040(19) 0.0428(16) Uani 1 1 d . . . Sn1 Sn 0.20919(6) 0.8299(2) 0.41514(5) 0.0491(5) Uani 1 1 d . . . Sn2 Sn 0.31175(6) 0.79785(19) 0.35676(5) 0.0477(5) Uani 1 1 d . . . Te1 Te 0.31790(6) 0.93033(17) 0.45064(5) 0.0447(4) Uani 1 1 d . . . Te2 Te 0.20208(6) 0.89051(18) 0.31572(5) 0.0436(4) Uani 1 1 d . . . Te3 Te 0.33543(6) 1.10810(18) 0.33576(5) 0.0495(4) Uani 1 1 d . . . Te4 Te 0.17538(7) 1.14575(19) 0.41472(6) 0.0576(5) Uani 1 1 d . . . C1 C 0.3432(9) 0.531(3) 0.5081(8) 0.057(7) Uani 1 1 d U . . C2 C 0.3254(10) 0.482(3) 0.4551(7) 0.071(8) Uani 1 1 d U . . H2A H 0.3550 0.4725 0.4492 0.086 Uiso 1 1 calc R . . H2B H 0.3017 0.5634 0.4322 0.086 Uiso 1 1 calc R . . H2C H 0.3077 0.3791 0.4487 0.086 Uiso 1 1 calc R . . C3 C 0.3827(8) 0.398(3) 0.5445(7) 0.063(7) Uani 1 1 d U . . H3A H 0.3960 0.4298 0.5800 0.076 Uiso 1 1 calc R . . H3B H 0.4113 0.3880 0.5370 0.076 Uiso 1 1 calc R . . H3C H 0.3650 0.2947 0.5387 0.076 Uiso 1 1 calc R . . C4 C 0.2977(9) 0.531(3) 0.5196(8) 0.062(7) Uani 1 1 d U . . H4C H 0.2821 0.4243 0.5132 0.075 Uiso 1 1 calc R . . H4B H 0.2719 0.6095 0.4978 0.075 Uiso 1 1 calc R . . H4A H 0.3102 0.5598 0.5553 0.075 Uiso 1 1 calc R . . C5 C 0.3916(8) 0.843(2) 0.5807(6) 0.038(5) Uani 1 1 d U . . C6 C 0.4147(9) 0.729(3) 0.6269(7) 0.062(7) Uani 1 1 d U . . H6A H 0.4462 0.6808 0.6302 0.075 Uiso 1 1 calc R . . H6B H 0.3898 0.6451 0.6223 0.075 Uiso 1 1 calc R . . H6C H 0.4228 0.7905 0.6577 0.075 Uiso 1 1 calc R . . C7 C 0.3448(9) 0.915(3) 0.5804(7) 0.057(6) Uani 1 1 d U . . H7A H 0.3200 0.8306 0.5754 0.069 Uiso 1 1 calc R . . H7B H 0.3291 0.9934 0.5527 0.069 Uiso 1 1 calc R . . H7C H 0.3551 0.9691 0.6128 0.069 Uiso 1 1 calc R . . C8 C 0.4290(9) 0.982(2) 0.5894(7) 0.050(6) Uani 1 1 d U . . H8C H 0.4369 1.0374 0.6211 0.060 Uiso 1 1 calc R . . H8B H 0.4132 1.0581 0.5611 0.060 Uiso 1 1 calc R . . H8A H 0.4609 0.9404 0.5916 0.060 Uiso 1 1 calc R . . C9 C 0.4374(8) 0.720(2) 0.5159(6) 0.040(6) Uani 1 1 d U . . C10 C 0.4803(9) 0.643(3) 0.5540(8) 0.064(7) Uani 1 1 d U . . H10A H 0.4767 0.5873 0.5797 0.077 Uiso 1 1 calc R . . C11 C 0.5274(9) 0.644(3) 0.5560(9) 0.063(7) Uani 1 1 d U . . H11A H 0.5550 0.5843 0.5815 0.076 Uiso 1 1 calc R . . C12 C 0.5353(9) 0.729(3) 0.5219(8) 0.059(7) Uani 1 1 d U . . H12A H 0.5685 0.7332 0.5246 0.070 Uiso 1 1 calc R . . C13 C 0.4945(9) 0.811(3) 0.4827(7) 0.055(6) Uani 1 1 d U . . H13A H 0.4996 0.8717 0.4588 0.066 Uiso 1 1 calc R . . C14 C 0.4444(8) 0.803(3) 0.4794(7) 0.050(6) Uani 1 1 d U . . H14A H 0.4160 0.8549 0.4522 0.060 Uiso 1 1 calc R . . C15 C 0.1731(9) 0.474(3) 0.2707(8) 0.046(6) Uani 1 1 d U . . C16 C 0.1356(9) 0.336(3) 0.2466(7) 0.070(7) Uani 1 1 d U . . H16A H 0.1157 0.3530 0.2099 0.085 Uiso 1 1 calc R . . H16B H 0.1123 0.3307 0.2611 0.085 Uiso 1 1 calc R . . H16C H 0.1548 0.2352 0.2534 0.085 Uiso 1 1 calc R . . C17 C 0.2095(9) 0.478(3) 0.2471(8) 0.061(7) Uani 1 1 d U . . H17A H 0.2358 0.5606 0.2640 0.073 Uiso 1 1 calc R . . H17B H 0.1895 0.5030 0.2108 0.073 Uiso 1 1 calc R . . H17C H 0.2260 0.3734 0.2514 0.073 Uiso 1 1 calc R . . C18 C 0.2055(9) 0.441(3) 0.3267(7) 0.057(6) Uani 1 1 d U . . H18C H 0.2214 0.3349 0.3315 0.069 Uiso 1 1 calc R . . H18B H 0.1837 0.4433 0.3429 0.069 Uiso 1 1 calc R . . H18A H 0.2323 0.5226 0.3420 0.069 Uiso 1 1 calc R . . C19 C 0.0811(9) 0.693(3) 0.2643(7) 0.052(6) Uani 1 1 d U . . C20 C 0.0343(8) 0.613(3) 0.2190(8) 0.064(7) Uani 1 1 d U . . H20A H 0.0413 0.4985 0.2179 0.077 Uiso 1 1 calc R . . H20B H 0.0283 0.6641 0.1874 0.077 Uiso 1 1 calc R . . H20C H 0.0037 0.6253 0.2233 0.077 Uiso 1 1 calc R . . C21 C 0.0872(9) 0.610(3) 0.3121(7) 0.073(8) Uani 1 1 d U . . H21A H 0.1165 0.6572 0.3418 0.087 Uiso 1 1 calc R . . H21B H 0.0933 0.4956 0.3104 0.087 Uiso 1 1 calc R . . H21C H 0.0559 0.6251 0.3148 0.087 Uiso 1 1 calc R . . C22 C 0.0667(9) 0.864(3) 0.2641(8) 0.064(7) Uani 1 1 d U . . H22C H 0.0355 0.8708 0.2674 0.077 Uiso 1 1 calc R . . H22B H 0.0604 0.9143 0.2321 0.077 Uiso 1 1 calc R . . H22A H 0.0948 0.9205 0.2925 0.077 Uiso 1 1 calc R . . C23 C 0.1220(8) 0.753(2) 0.1917(7) 0.038(5) Uani 1 1 d U . . C24 C 0.0939(8) 0.652(3) 0.1499(7) 0.046(6) Uani 1 1 d U . . H24A H 0.0868 0.5453 0.1561 0.056 Uiso 1 1 calc R . . C25 C 0.0760(10) 0.700(3) 0.1003(8) 0.063(7) Uani 1 1 d U . . H25A H 0.0562 0.6281 0.0732 0.076 Uiso 1 1 calc R . . C26 C 0.0869(9) 0.848(4) 0.0903(8) 0.068(8) Uani 1 1 d U . . H26A H 0.0753 0.8821 0.0563 0.081 Uiso 1 1 calc R . . C27 C 0.1146(8) 0.948(3) 0.1297(9) 0.062(7) Uani 1 1 d U . . H27A H 0.1221 1.0547 0.1241 0.075 Uiso 1 1 calc R . . C28 C 0.1319(8) 0.890(3) 0.1789(8) 0.053(6) Uani 1 1 d U . . H28A H 0.1533 0.9598 0.2059 0.064 Uiso 1 1 calc R . . C29 C 0.2963(9) 0.969(3) 0.2070(7) 0.056(6) Uani 1 1 d U . . C30 C 0.2757(9) 0.825(3) 0.2211(7) 0.051(6) Uani 1 1 d U . . H30A H 0.2646 0.8569 0.2456 0.061 Uiso 1 1 calc R . . H30B H 0.3026 0.7438 0.2361 0.061 Uiso 1 1 calc R . . H30C H 0.2464 0.7818 0.1907 0.061 Uiso 1 1 calc R . . C31 C 0.2555(9) 1.103(3) 0.1851(7) 0.062(6) Uani 1 1 d U . . H31A H 0.2697 1.1950 0.1756 0.075 Uiso 1 1 calc R . . H31B H 0.2462 1.1368 0.2109 0.075 Uiso 1 1 calc R . . H31C H 0.2249 1.0635 0.1552 0.075 Uiso 1 1 calc R . . C32 C 0.3094(10) 0.913(3) 0.1644(7) 0.078(8) Uani 1 1 d U . . H32C H 0.2784 0.8700 0.1356 0.094 Uiso 1 1 calc R . . H32B H 0.3359 0.8299 0.1780 0.094 Uiso 1 1 calc R . . H32A H 0.3220 1.0048 0.1532 0.094 Uiso 1 1 calc R . . C33 C 0.3820(9) 1.258(3) 0.2563(8) 0.055(6) Uani 1 1 d U . . C34 C 0.4369(9) 1.274(3) 0.3001(7) 0.062(7) Uani 1 1 d U . . H34A H 0.4579 1.1846 0.2993 0.074 Uiso 1 1 calc R . . H34B H 0.4364 1.2737 0.3324 0.074 Uiso 1 1 calc R . . H34C H 0.4518 1.3754 0.2967 0.074 Uiso 1 1 calc R . . C35 C 0.3857(10) 1.266(3) 0.2066(7) 0.069(7) Uani 1 1 d U . . H35A H 0.3513 1.2536 0.1774 0.083 Uiso 1 1 calc R . . H35B H 0.4081 1.1800 0.2065 0.083 Uiso 1 1 calc R . . H35C H 0.4000 1.3699 0.2046 0.083 Uiso 1 1 calc R . . C36 C 0.3509(12) 1.398(3) 0.2580(9) 0.084(9) Uani 1 1 d U . . H36C H 0.3655 1.4979 0.2531 0.101 Uiso 1 1 calc R . . H36B H 0.3518 1.4012 0.2910 0.101 Uiso 1 1 calc R . . H36A H 0.3153 1.3875 0.2310 0.101 Uiso 1 1 calc R . . C37 C 0.4117(8) 0.908(3) 0.2884(7) 0.044(5) Uani 1 1 d U . . C38 C 0.4314(8) 0.827(3) 0.3337(7) 0.044(5) Uani 1 1 d U . . H38A H 0.4161 0.8429 0.3548 0.053 Uiso 1 1 calc R . . C39 C 0.4714(9) 0.725(3) 0.3494(8) 0.058(7) Uani 1 1 d U . . H39A H 0.4843 0.6764 0.3818 0.070 Uiso 1 1 calc R . . C40 C 0.4937(9) 0.690(3) 0.3213(8) 0.060(6) Uani 1 1 d U . . H40A H 0.5229 0.6222 0.3338 0.071 Uiso 1 1 calc R . . C41 C 0.4738(8) 0.754(3) 0.2753(9) 0.052(6) Uani 1 1 d U . . H41A H 0.4878 0.7249 0.2539 0.063 Uiso 1 1 calc R . . C42 C 0.4335(9) 0.859(3) 0.2576(7) 0.055(6) Uani 1 1 d U . . H42A H 0.4198 0.9003 0.2242 0.066 Uiso 1 1 calc R . . C43 C 0.1854(9) 1.082(3) 0.5393(7) 0.052(6) Uani 1 1 d U . . C44 C 0.1964(10) 0.904(3) 0.5423(8) 0.079(8) Uani 1 1 d U . . H44A H 0.2093 0.8770 0.5188 0.095 Uiso 1 1 calc R . . H44B H 0.1647 0.8444 0.5330 0.095 Uiso 1 1 calc R . . H44C H 0.2222 0.8762 0.5769 0.095 Uiso 1 1 calc R . . C45 C 0.1673(8) 1.118(3) 0.5795(7) 0.064(7) Uani 1 1 d U . . H45A H 0.1367 1.0539 0.5718 0.077 Uiso 1 1 calc R . . H45B H 0.1590 1.2320 0.5784 0.077 Uiso 1 1 calc R . . H45C H 0.1949 1.0904 0.6134 0.077 Uiso 1 1 calc R . . C46 C 0.2347(8) 1.173(3) 0.5561(8) 0.077(8) Uani 1 1 d U . . H46C H 0.2594 1.1433 0.5909 0.092 Uiso 1 1 calc R . . H46B H 0.2276 1.2886 0.5546 0.092 Uiso 1 1 calc R . . H46A H 0.2490 1.1483 0.5336 0.092 Uiso 1 1 calc R . . C47 C 0.0990(8) 1.336(3) 0.4592(8) 0.048(6) Uani 1 1 d U . . C48 C 0.0654(10) 1.362(3) 0.4061(7) 0.078(8) Uani 1 1 d U . . H48A H 0.0393 1.2773 0.3928 0.094 Uiso 1 1 calc R . . H48B H 0.0854 1.3601 0.3880 0.094 Uiso 1 1 calc R . . H48C H 0.0485 1.4663 0.4011 0.094 Uiso 1 1 calc R . . C49 C 0.0666(9) 1.344(3) 0.4862(8) 0.065(7) Uani 1 1 d U . . H49A H 0.0884 1.3227 0.5225 0.078 Uiso 1 1 calc R . . H49B H 0.0391 1.2641 0.4717 0.078 Uiso 1 1 calc R . . H49C H 0.0515 1.4514 0.4818 0.078 Uiso 1 1 calc R . . C50 C 0.1385(11) 1.468(3) 0.4808(12) 0.104(10) Uani 1 1 d U . . H50A H 0.1593 1.4685 0.4635 0.125 Uiso 1 1 calc R . . H50B H 0.1608 1.4494 0.5171 0.125 Uiso 1 1 calc R . . H50C H 0.1211 1.5714 0.4758 0.125 Uiso 1 1 calc R . . C51 C 0.0587(10) 0.914(3) 0.3976(9) 0.065(7) Uani 1 1 d U . . H51A H 0.0749 0.9391 0.3778 0.078 Uiso 1 1 calc R . . C52 C 0.0169(9) 0.809(3) 0.3756(8) 0.058(6) Uani 1 1 d U . . H52A H 0.0031 0.7723 0.3417 0.069 Uiso 1 1 calc R . . C53 C -0.0029(10) 0.764(2) 0.4065(8) 0.054(6) Uani 1 1 d U . . H53A H -0.0298 0.6871 0.3944 0.064 Uiso 1 1 calc R . . C54 C 0.0141(10) 0.824(3) 0.4526(9) 0.067(7) Uani 1 1 d U . . H54A H -0.0016 0.7939 0.4724 0.080 Uiso 1 1 calc R . . C55 C 0.0560(9) 0.932(3) 0.4720(8) 0.067(7) Uani 1 1 d U . . H55A H 0.0688 0.9704 0.5057 0.080 Uiso 1 1 calc R . . C56 C 0.0790(9) 0.985(3) 0.4446(7) 0.046(6) Uani 1 1 d U . . 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 0.037(4) 0.046(4) 0.046(3) 0.003(3) 0.015(3) 0.004(3) Si2 0.037(4) 0.052(4) 0.040(3) 0.010(3) 0.016(3) 0.002(4) Si3 0.036(4) 0.056(5) 0.043(3) 0.005(3) 0.018(3) -0.004(4) Si4 0.037(4) 0.049(4) 0.043(3) -0.004(3) 0.019(3) -0.004(4) Sn1 0.0497(11) 0.0546(11) 0.0444(8) 0.0013(8) 0.0238(9) -0.0018(10) Sn2 0.0468(11) 0.0542(11) 0.0445(9) 0.0020(8) 0.0238(9) 0.0041(9) Te1 0.0470(11) 0.0457(10) 0.0386(8) 0.0031(7) 0.0184(8) 0.0035(9) Te2 0.0439(10) 0.0451(10) 0.0391(8) -0.0016(8) 0.0178(8) -0.0007(9) Te3 0.0549(11) 0.0492(10) 0.0510(8) -0.0025(8) 0.0309(8) -0.0021(9) Te4 0.0705(13) 0.0519(11) 0.0687(10) 0.0075(9) 0.0482(10) 0.0061(10) C1 0.035(15) 0.085(19) 0.050(13) 0.004(12) 0.018(12) 0.006(14) C2 0.08(2) 0.09(2) 0.045(12) -0.011(13) 0.026(14) -0.031(17) C3 0.048(16) 0.071(18) 0.048(12) -0.005(12) 0.005(12) 0.010(14) C4 0.048(16) 0.068(17) 0.085(16) 0.049(14) 0.044(15) 0.014(14) C5 0.040(14) 0.033(13) 0.031(10) 0.007(10) 0.009(11) 0.006(11) C6 0.052(17) 0.082(19) 0.035(12) -0.014(11) 0.006(12) -0.013(14) C7 0.081(18) 0.039(15) 0.058(13) -0.010(12) 0.039(14) 0.011(14) C8 0.061(17) 0.049(15) 0.047(13) -0.013(11) 0.032(13) 0.001(13) C9 0.055(15) 0.052(15) 0.021(10) 0.009(10) 0.025(11) 0.005(12) C10 0.046(16) 0.09(2) 0.058(13) 0.008(14) 0.022(13) -0.011(15) C11 0.051(15) 0.08(2) 0.067(14) 0.007(14) 0.036(13) 0.016(15) C12 0.036(14) 0.08(2) 0.045(13) -0.024(12) 0.010(12) -0.001(14) C13 0.047(15) 0.088(19) 0.030(11) -0.033(12) 0.017(11) -0.020(15) C14 0.044(14) 0.062(16) 0.040(12) -0.006(11) 0.018(11) 0.021(14) C15 0.046(16) 0.045(14) 0.059(13) 0.003(11) 0.034(13) 0.017(12) C16 0.065(18) 0.062(18) 0.057(13) 0.013(13) 0.007(13) 0.005(15) C17 0.066(19) 0.043(15) 0.072(15) 0.015(12) 0.031(15) 0.033(14) C18 0.038(15) 0.049(16) 0.064(13) 0.006(12) 0.008(12) 0.007(14) C19 0.077(18) 0.057(15) 0.021(10) -0.018(11) 0.021(12) -0.013(14) C20 0.049(16) 0.080(19) 0.081(14) -0.012(15) 0.046(13) -0.023(15) C21 0.062(18) 0.09(2) 0.056(12) -0.022(14) 0.023(13) -0.038(17) C22 0.036(15) 0.077(17) 0.064(14) -0.036(13) 0.012(12) -0.005(15) C23 0.023(13) 0.044(14) 0.041(11) 0.013(10) 0.011(11) 0.013(11) C24 0.043(15) 0.046(15) 0.054(13) -0.003(11) 0.027(12) -0.007(13) C25 0.08(2) 0.062(16) 0.056(13) -0.012(13) 0.045(15) -0.002(16) C26 0.037(15) 0.11(2) 0.033(11) 0.022(13) -0.002(11) -0.025(16) C27 0.030(16) 0.061(17) 0.090(17) 0.030(13) 0.023(14) -0.004(13) C28 0.043(15) 0.077(17) 0.050(12) 0.002(13) 0.030(12) -0.016(14) C29 0.051(17) 0.067(17) 0.044(13) 0.005(12) 0.017(13) 0.000(14) C30 0.056(16) 0.044(14) 0.055(13) 0.002(11) 0.028(12) 0.005(13) C31 0.065(18) 0.069(17) 0.054(13) 0.004(13) 0.029(13) -0.009(15) C32 0.10(2) 0.09(2) 0.037(12) -0.026(14) 0.028(13) -0.008(18) C33 0.065(17) 0.044(15) 0.058(13) -0.015(12) 0.033(13) -0.040(13) C34 0.053(15) 0.081(19) 0.059(13) -0.025(13) 0.033(12) -0.038(15) C35 0.08(2) 0.061(18) 0.059(13) 0.025(13) 0.028(14) 0.000(16) C36 0.15(3) 0.046(16) 0.095(18) 0.017(15) 0.09(2) 0.018(18) C37 0.049(15) 0.048(14) 0.037(11) 0.000(11) 0.021(11) -0.010(12) C38 0.028(13) 0.058(16) 0.038(11) -0.006(11) 0.008(11) -0.005(12) C39 0.057(17) 0.079(18) 0.060(14) -0.016(13) 0.045(14) -0.009(14) C40 0.036(15) 0.066(18) 0.055(14) -0.009(13) 0.005(12) 0.002(14) C41 0.026(14) 0.039(15) 0.060(14) -0.011(12) -0.004(12) 0.015(12) C42 0.060(16) 0.054(16) 0.045(12) 0.006(12) 0.020(12) 0.008(14) C43 0.065(17) 0.044(14) 0.044(12) -0.009(12) 0.023(12) -0.020(14) C44 0.09(2) 0.057(16) 0.076(16) 0.015(15) 0.024(16) 0.017(17) C45 0.033(14) 0.088(19) 0.064(14) -0.005(15) 0.016(12) -0.012(15) C46 0.023(14) 0.11(2) 0.079(16) -0.030(17) 0.012(13) -0.008(15) C47 0.037(14) 0.050(15) 0.066(13) 0.001(12) 0.033(12) 0.001(12) C48 0.09(2) 0.069(19) 0.059(13) 0.028(14) 0.026(14) 0.054(17) C49 0.053(17) 0.067(18) 0.069(14) -0.023(14) 0.025(14) -0.003(15) C50 0.07(2) 0.07(2) 0.18(3) -0.05(2) 0.07(2) -0.032(18) C51 0.045(16) 0.08(2) 0.079(16) 0.021(15) 0.036(14) 0.015(15) C52 0.039(15) 0.074(18) 0.057(14) 0.001(13) 0.021(12) 0.018(14) C53 0.065(18) 0.033(14) 0.052(13) 0.000(11) 0.021(13) 0.005(12) C54 0.052(16) 0.077(19) 0.072(15) -0.005(15) 0.031(14) -0.010(16) C55 0.046(17) 0.08(2) 0.053(13) -0.004(14) 0.007(12) -0.009(15) C56 0.054(16) 0.076(17) 0.018(10) -0.001(10) 0.025(11) 0.005(12) _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 1.88(2) . ? Si1 C1 1.89(2) . ? Si1 C5 1.917(18) . ? Si1 Te1 2.545(6) . ? Si2 C19 1.88(2) . ? Si2 C23 1.882(19) . ? Si2 C15 1.91(2) . ? Si2 Te2 2.543(7) . ? Si3 C37 1.89(2) . ? Si3 C33 1.94(2) . ? Si3 C29 1.94(2) . ? Si3 Te3 2.513(5) . ? Si4 C56 1.89(2) . ? Si4 C47 1.92(2) . ? Si4 C43 1.95(2) . ? Si4 Te4 2.525(5) . ? Sn1 Te4 2.818(2) . ? Sn1 Te2 2.9394(18) . ? Sn1 Te1 2.990(2) . ? Sn2 Te3 2.833(2) . ? Sn2 Te1 2.9555(19) . ? Sn2 Te2 2.975(2) . ? C1 C2 1.48(3) . ? C1 C4 1.55(3) . ? C1 C3 1.60(3) . ? C5 C7 1.51(3) . ? C5 C6 1.54(3) . ? C5 C8 1.54(3) . ? C9 C10 1.39(3) . ? C9 C14 1.40(2) . ? C10 C11 1.37(3) . ? C11 C12 1.36(3) . ? C12 C13 1.40(3) . ? C13 C14 1.44(3) . ? C15 C18 1.51(3) . ? C15 C16 1.52(3) . ? C15 C17 1.55(3) . ? C19 C22 1.49(3) . ? C19 C21 1.52(3) . ? C19 C20 1.55(3) . ? C23 C28 1.29(3) . ? C23 C24 1.41(3) . ? C24 C25 1.38(3) . ? C25 C26 1.35(3) . ? C26 C27 1.36(3) . ? C27 C28 1.40(3) . ? C29 C30 1.50(3) . ? C29 C31 1.55(3) . ? C29 C32 1.58(3) . ? C33 C36 1.51(3) . ? C33 C34 1.53(3) . ? C33 C35 1.55(2) . ? C37 C38 1.37(2) . ? C37 C42 1.42(2) . ? C38 C39 1.35(3) . ? C39 C40 1.33(3) . ? C40 C41 1.33(3) . ? C41 C42 1.37(3) . ? C43 C46 1.51(3) . ? C43 C44 1.51(3) . ? C43 C45 1.57(2) . ? C47 C48 1.44(3) . ? C47 C50 1.51(3) . ? C47 C49 1.53(2) . ? C51 C56 1.38(3) . ? C51 C52 1.40(3) . ? C52 C53 1.37(3) . ? C53 C54 1.32(3) . ? C54 C55 1.42(3) . ? C55 C56 1.37(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 111.6(10) . . ? C9 Si1 C5 106.3(9) . . ? C1 Si1 C5 117.4(9) . . ? C9 Si1 Te1 107.0(6) . . ? C1 Si1 Te1 110.5(7) . . ? C5 Si1 Te1 103.2(6) . . ? C19 Si2 C23 106.4(9) . . ? C19 Si2 C15 116.2(10) . . ? C23 Si2 C15 112.1(9) . . ? C19 Si2 Te2 106.4(7) . . ? C23 Si2 Te2 104.2(7) . . ? C15 Si2 Te2 110.6(8) . . ? C37 Si3 C33 106.6(10) . . ? C37 Si3 C29 110.6(10) . . ? C33 Si3 C29 116.4(10) . . ? C37 Si3 Te3 109.4(6) . . ? C33 Si3 Te3 103.7(7) . . ? C29 Si3 Te3 109.8(7) . . ? C56 Si4 C47 103.3(10) . . ? C56 Si4 C43 111.9(9) . . ? C47 Si4 C43 117.8(9) . . ? C56 Si4 Te4 110.6(5) . . ? C47 Si4 Te4 103.9(6) . . ? C43 Si4 Te4 108.9(7) . . ? Te4 Sn1 Te2 89.06(6) . . ? Te4 Sn1 Te1 93.46(7) . . ? Te2 Sn1 Te1 81.48(5) . . ? Te3 Sn2 Te1 87.90(6) . . ? Te3 Sn2 Te2 90.53(6) . . ? Te1 Sn2 Te2 81.46(6) . . ? Si1 Te1 Sn2 103.67(14) . . ? Si1 Te1 Sn1 107.32(15) . . ? Sn2 Te1 Sn1 89.67(6) . . ? Si2 Te2 Sn1 104.97(13) . . ? Si2 Te2 Sn2 112.71(15) . . ? Sn1 Te2 Sn2 90.26(6) . . ? Si3 Te3 Sn2 102.21(16) . . ? Si4 Te4 Sn1 104.38(15) . . ? C2 C1 C4 110(2) . . ? C2 C1 C3 108.0(18) . . ? C4 C1 C3 106.2(16) . . ? C2 C1 Si1 108.5(15) . . ? C4 C1 Si1 112.9(15) . . ? C3 C1 Si1 110.8(15) . . ? C7 C5 C6 105.1(16) . . ? C7 C5 C8 106.4(17) . . ? C6 C5 C8 109.7(17) . . ? C7 C5 Si1 112.9(14) . . ? C6 C5 Si1 112.2(14) . . ? C8 C5 Si1 110.4(12) . . ? C10 C9 C14 117.0(19) . . ? C10 C9 Si1 120.9(13) . . ? C14 C9 Si1 121.6(16) . . ? C11 C10 C9 123(2) . . ? C12 C11 C10 121(2) . . ? C11 C12 C13 120(2) . . ? C12 C13 C14 119(2) . . ? C9 C14 C13 120(2) . . ? C18 C15 C16 108.6(17) . . ? C18 C15 C17 107.8(19) . . ? C16 C15 C17 107.9(17) . . ? C18 C15 Si2 112.7(14) . . ? C16 C15 Si2 113.3(16) . . ? C17 C15 Si2 106.2(13) . . ? C22 C19 C21 110.0(17) . . ? C22 C19 C20 106(2) . . ? C21 C19 C20 106.6(18) . . ? C22 C19 Si2 109.9(16) . . ? C21 C19 Si2 112.6(17) . . ? C20 C19 Si2 111.5(12) . . ? C28 C23 C24 113.0(19) . . ? C28 C23 Si2 127.8(18) . . ? C24 C23 Si2 119.3(16) . . ? C25 C24 C23 123(2) . . ? C26 C25 C24 120(2) . . ? C25 C26 C27 119(2) . . ? C26 C27 C28 118(2) . . ? C23 C28 C27 127(2) . . ? C30 C29 C31 110.9(19) . . ? C30 C29 C32 106.8(19) . . ? C31 C29 C32 108.5(16) . . ? C30 C29 Si3 111.0(14) . . ? C31 C29 Si3 107.9(15) . . ? C32 C29 Si3 111.6(16) . . ? C36 C33 C34 108.3(19) . . ? C36 C33 C35 108.9(18) . . ? C34 C33 C35 106.6(17) . . ? C36 C33 Si3 112.9(16) . . ? C34 C33 Si3 106.7(16) . . ? C35 C33 Si3 113.1(14) . . ? C38 C37 C42 113(2) . . ? C38 C37 Si3 124.0(15) . . ? C42 C37 Si3 122.4(15) . . ? C39 C38 C37 123(2) . . ? C40 C39 C38 122(2) . . ? C41 C40 C39 118(2) . . ? C40 C41 C42 122(2) . . ? C41 C42 C37 121.2(19) . . ? C46 C43 C44 110(2) . . ? C46 C43 C45 106.3(16) . . ? C44 C43 C45 106.7(17) . . ? C46 C43 Si4 112.8(15) . . ? C44 C43 Si4 108.7(15) . . ? C45 C43 Si4 112.7(15) . . ? C48 C47 C50 110(2) . . ? C48 C47 C49 107.9(19) . . ? C50 C47 C49 107.2(18) . . ? C48 C47 Si4 110.7(15) . . ? C50 C47 Si4 109.1(16) . . ? C49 C47 Si4 111.4(15) . . ? C56 C51 C52 127(2) . . ? C53 C52 C51 115(2) . . ? C54 C53 C52 122(2) . . ? C53 C54 C55 119(2) . . ? C56 C55 C54 123(2) . . ? C55 C56 C51 113(2) . . ? C55 C56 Si4 122.7(15) . . ? C51 C56 Si4 124.8(16) . . ? 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 Te1 Sn2 55.8(7) . . . . ? C1 Si1 Te1 Sn2 -65.9(7) . . . . ? C5 Si1 Te1 Sn2 167.8(7) . . . . ? C9 Si1 Te1 Sn1 149.8(6) . . . . ? C1 Si1 Te1 Sn1 28.1(7) . . . . ? C5 Si1 Te1 Sn1 -98.2(7) . . . . ? Te3 Sn2 Te1 Si1 -131.07(16) . . . . ? Te2 Sn2 Te1 Si1 138.08(16) . . . . ? Te3 Sn2 Te1 Sn1 121.18(6) . . . . ? Te2 Sn2 Te1 Sn1 30.33(5) . . . . ? Te4 Sn1 Te1 Si1 136.52(14) . . . . ? Te2 Sn1 Te1 Si1 -134.96(14) . . . . ? Te4 Sn1 Te1 Sn2 -119.26(6) . . . . ? Te2 Sn1 Te1 Sn2 -30.73(5) . . . . ? C19 Si2 Te2 Sn1 52.4(7) . . . . ? C23 Si2 Te2 Sn1 164.7(6) . . . . ? C15 Si2 Te2 Sn1 -74.6(6) . . . . ? C19 Si2 Te2 Sn2 149.2(7) . . . . ? C23 Si2 Te2 Sn2 -98.6(6) . . . . ? C15 Si2 Te2 Sn2 22.1(7) . . . . ? Te4 Sn1 Te2 Si2 -122.22(16) . . . . ? Te1 Sn1 Te2 Si2 144.14(16) . . . . ? Te4 Sn1 Te2 Sn2 124.15(7) . . . . ? Te1 Sn1 Te2 Sn2 30.51(5) . . . . ? Te3 Sn2 Te2 Si2 134.93(14) . . . . ? Te1 Sn2 Te2 Si2 -137.27(14) . . . . ? Te3 Sn2 Te2 Sn1 -118.70(6) . . . . ? Te1 Sn2 Te2 Sn1 -30.90(5) . . . . ? C37 Si3 Te3 Sn2 -58.9(7) . . . . ? C33 Si3 Te3 Sn2 -172.3(8) . . . . ? C29 Si3 Te3 Sn2 62.6(8) . . . . ? Te1 Sn2 Te3 Si3 167.01(16) . . . . ? Te2 Sn2 Te3 Si3 -111.56(16) . . . . ? C56 Si4 Te4 Sn1 -58.7(7) . . . . ? C47 Si4 Te4 Sn1 -169.0(7) . . . . ? C43 Si4 Te4 Sn1 64.6(7) . . . . ? Te2 Sn1 Te4 Si4 153.83(15) . . . . ? Te1 Sn1 Te4 Si4 -124.77(15) . . . . ? C9 Si1 C1 C2 -67.7(18) . . . . ? C5 Si1 C1 C2 169.2(16) . . . . ? Te1 Si1 C1 C2 51.2(17) . . . . ? C9 Si1 C1 C4 169.8(14) . . . . ? C5 Si1 C1 C4 46.7(19) . . . . ? Te1 Si1 C1 C4 -71.3(16) . . . . ? C9 Si1 C1 C3 50.7(15) . . . . ? C5 Si1 C1 C3 -72.3(16) . . . . ? Te1 Si1 C1 C3 169.7(11) . . . . ? C9 Si1 C5 C7 159.4(15) . . . . ? C1 Si1 C5 C7 -75.0(17) . . . . ? Te1 Si1 C5 C7 46.9(15) . . . . ? C9 Si1 C5 C6 -82.2(17) . . . . ? C1 Si1 C5 C6 43.5(19) . . . . ? Te1 Si1 C5 C6 165.3(14) . . . . ? C9 Si1 C5 C8 40.5(16) . . . . ? C1 Si1 C5 C8 166.2(14) . . . . ? Te1 Si1 C5 C8 -72.0(14) . . . . ? C1 Si1 C9 C10 -70(2) . . . . ? C5 Si1 C9 C10 59(2) . . . . ? Te1 Si1 C9 C10 168.8(17) . . . . ? C1 Si1 C9 C14 118.2(17) . . . . ? C5 Si1 C9 C14 -112.6(17) . . . . ? Te1 Si1 C9 C14 -2.8(18) . . . . ? C14 C9 C10 C11 -1(3) . . . . ? Si1 C9 C10 C11 -173(2) . . . . ? C9 C10 C11 C12 4(4) . . . . ? C10 C11 C12 C13 -3(4) . . . . ? C11 C12 C13 C14 0(3) . . . . ? C10 C9 C14 C13 -2(3) . . . . ? Si1 C9 C14 C13 170.2(16) . . . . ? C12 C13 C14 C9 3(3) . . . . ? C19 Si2 C15 C18 -79.1(19) . . . . ? C23 Si2 C15 C18 158.2(16) . . . . ? Te2 Si2 C15 C18 42.4(17) . . . . ? C19 Si2 C15 C16 44.7(17) . . . . ? C23 Si2 C15 C16 -78.0(16) . . . . ? Te2 Si2 C15 C16 166.2(12) . . . . ? C19 Si2 C15 C17 163.0(14) . . . . ? C23 Si2 C15 C17 40.3(18) . . . . ? Te2 Si2 C15 C17 -75.5(15) . . . . ? C23 Si2 C19 C22 -66.9(15) . . . . ? C15 Si2 C19 C22 167.5(13) . . . . ? Te2 Si2 C19 C22 43.8(14) . . . . ? C23 Si2 C19 C21 170.1(15) . . . . ? C15 Si2 C19 C21 44.5(18) . . . . ? Te2 Si2 C19 C21 -79.2(16) . . . . ? C23 Si2 C19 C20 50.3(18) . . . . ? C15 Si2 C19 C20 -75.3(18) . . . . ? Te2 Si2 C19 C20 161.0(14) . . . . ? C19 Si2 C23 C28 103(2) . . . . ? C15 Si2 C23 C28 -129(2) . . . . ? Te2 Si2 C23 C28 -9(2) . . . . ? C19 Si2 C23 C24 -77.2(17) . . . . ? C15 Si2 C23 C24 50.9(19) . . . . ? Te2 Si2 C23 C24 170.6(14) . . . . ? C28 C23 C24 C25 -4(3) . . . . ? Si2 C23 C24 C25 175.9(17) . . . . ? C23 C24 C25 C26 2(4) . . . . ? C24 C25 C26 C27 -1(4) . . . . ? C25 C26 C27 C28 2(4) . . . . ? C24 C23 C28 C27 5(3) . . . . ? Si2 C23 C28 C27 -174.7(17) . . . . ? C26 C27 C28 C23 -4(4) . . . . ? C37 Si3 C29 C30 66.9(17) . . . . ? C33 Si3 C29 C30 -171.3(15) . . . . ? Te3 Si3 C29 C30 -53.9(17) . . . . ? C37 Si3 C29 C31 -171.3(13) . . . . ? C33 Si3 C29 C31 -49.5(17) . . . . ? Te3 Si3 C29 C31 67.8(14) . . . . ? C37 Si3 C29 C32 -52.1(18) . . . . ? C33 Si3 C29 C32 69.7(19) . . . . ? Te3 Si3 C29 C32 -173.0(14) . . . . ? C37 Si3 C33 C36 -157.7(16) . . . . ? C29 Si3 C33 C36 78.4(19) . . . . ? Te3 Si3 C33 C36 -42.3(18) . . . . ? C37 Si3 C33 C34 -38.9(16) . . . . ? C29 Si3 C33 C34 -162.7(13) . . . . ? Te3 Si3 C33 C34 76.5(14) . . . . ? C37 Si3 C33 C35 78.0(18) . . . . ? C29 Si3 C33 C35 -46(2) . . . . ? Te3 Si3 C33 C35 -166.6(15) . . . . ? C33 Si3 C37 C38 120.7(18) . . . . ? C29 Si3 C37 C38 -111.9(18) . . . . ? Te3 Si3 C37 C38 9(2) . . . . ? C33 Si3 C37 C42 -66.0(19) . . . . ? C29 Si3 C37 C42 61.4(19) . . . . ? Te3 Si3 C37 C42 -177.5(16) . . . . ? C42 C37 C38 C39 7(3) . . . . ? Si3 C37 C38 C39 -178.9(17) . . . . ? C37 C38 C39 C40 -3(3) . . . . ? C38 C39 C40 C41 -3(3) . . . . ? C39 C40 C41 C42 4(3) . . . . ? C40 C41 C42 C37 1(3) . . . . ? C38 C37 C42 C41 -6(3) . . . . ? Si3 C37 C42 C41 179.6(17) . . . . ? C56 Si4 C43 C46 166.2(15) . . . . ? C47 Si4 C43 C46 -74.3(18) . . . . ? Te4 Si4 C43 C46 43.6(17) . . . . ? C56 Si4 C43 C44 44.6(18) . . . . ? C47 Si4 C43 C44 164.1(15) . . . . ? Te4 Si4 C43 C44 -78.0(16) . . . . ? C56 Si4 C43 C45 -73.5(17) . . . . ? C47 Si4 C43 C45 46.0(18) . . . . ? Te4 Si4 C43 C45 163.9(13) . . . . ? C56 Si4 C47 C48 -61.2(17) . . . . ? C43 Si4 C47 C48 174.8(16) . . . . ? Te4 Si4 C47 C48 54.3(17) . . . . ? C56 Si4 C47 C50 177.1(15) . . . . ? C43 Si4 C47 C50 53.1(18) . . . . ? Te4 Si4 C47 C50 -67.4(16) . . . . ? C56 Si4 C47 C49 58.9(16) . . . . ? C43 Si4 C47 C49 -65.1(18) . . . . ? Te4 Si4 C47 C49 174.4(13) . . . . ? C56 C51 C52 C53 -6(3) . . . . ? C51 C52 C53 C54 4(3) . . . . ? C52 C53 C54 C55 -3(3) . . . . ? C53 C54 C55 C56 3(4) . . . . ? C54 C55 C56 C51 -3(3) . . . . ? C54 C55 C56 Si4 178.1(19) . . . . ? C52 C51 C56 C55 5(3) . . . . ? C52 C51 C56 Si4 -176.5(19) . . . . ? C47 Si4 C56 C55 -82(2) . . . . ? C43 Si4 C56 C55 46(2) . . . . ? Te4 Si4 C56 C55 167.4(17) . . . . ? C47 Si4 C56 C51 100(2) . . . . ? C43 Si4 C56 C51 -132.7(19) . . . . ? Te4 Si4 C56 C51 -11(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 22.73 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.665 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.125 # Attachment '- Comp-3-CvH.CIF' data_d:\struk\c-com2\verb-3\verb-3 _database_code_depnum_ccdc_archive 'CCDC 876451' #TrackingRef '- Comp-3-CvH.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H92 Pb2 Si4 Te4' _chemical_formula_sum 'C56 H92 Pb2 Si4 Te4' _chemical_formula_weight 1802.44 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' Pb Pb -3.3944 10.1111 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.621(7) _cell_length_b 8.1720(16) _cell_length_c 31.760(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.06(3) _cell_angle_gamma 90.00 _cell_volume 6650(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 727 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 26.02 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.4520 _exptl_crystal_size_mid 0.1180 _exptl_crystal_size_min 0.0420 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 6.880 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1960 _exptl_absorpt_correction_T_max 0.7080 _exptl_absorpt_process_details ; (a) W. R. Busing and H. A. Levy, Acta Crystallogr. 1957, 10, 180-182. (b) P. Coppens, L. Leiserowitz and D. Rabinovich, Acta Crystallogr. 1965, 18, 1035-1038. ; _exptl_special_details ; ? ; _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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14149 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.63 _reflns_number_total 5785 _reflns_number_gt 4998 _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^)+(0.0425P)^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 5785 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 Pb1 Pb 0.050155(6) 0.02739(2) -0.195839(6) 0.03903(7) Uani 1 1 d . . . Te1 Te -0.062129(10) 0.12726(4) -0.212793(10) 0.03462(8) Uani 1 1 d . . . Te2 Te 0.077494(12) 0.35850(4) -0.172373(11) 0.04389(9) Uani 1 1 d . . . Si1 Si -0.12522(4) -0.08156(16) -0.18197(4) 0.0328(3) Uani 1 1 d . . . Si2 Si 0.10602(5) 0.32515(18) -0.09705(4) 0.0387(3) Uani 1 1 d . . . C1 C -0.0953(2) -0.2964(7) -0.18333(19) 0.0481(12) Uani 1 1 d . . . C2 C -0.1347(3) -0.4308(8) -0.1756(3) 0.087(3) Uani 1 1 d . . . H2A H -0.1537 -0.4082 -0.1495 0.131 Uiso 1 1 calc R . . H2B H -0.1166 -0.5360 -0.1732 0.131 Uiso 1 1 calc R . . H2C H -0.1594 -0.4352 -0.1992 0.131 Uiso 1 1 calc R . . C3 C -0.0536(3) -0.3038(10) -0.1480(3) 0.076(2) Uani 1 1 d . . . H3A H -0.0354 -0.4092 -0.1492 0.115 Uiso 1 1 calc R . . H3B H -0.0706 -0.2921 -0.1205 0.115 Uiso 1 1 calc R . . H3C H -0.0284 -0.2148 -0.1518 0.115 Uiso 1 1 calc R . . C4 C -0.0668(3) -0.3306(9) -0.2249(3) 0.079(2) Uani 1 1 d . . . H4A H -0.0515 -0.4405 -0.2241 0.118 Uiso 1 1 calc R . . H4B H -0.0390 -0.2495 -0.2289 0.118 Uiso 1 1 calc R . . H4C H -0.0916 -0.3237 -0.2483 0.118 Uiso 1 1 calc R . . C5 C -0.18931(19) -0.0449(7) -0.21187(17) 0.0452(12) Uani 1 1 d . . . C6 C -0.23304(19) -0.1575(8) -0.1950(2) 0.0532(14) Uani 1 1 d . . . H6A H -0.2660 -0.1308 -0.2091 0.080 Uiso 1 1 calc R . . H6B H -0.2369 -0.1411 -0.1646 0.080 Uiso 1 1 calc R . . H6C H -0.2240 -0.2720 -0.2006 0.080 Uiso 1 1 calc R . . C7 C -0.2065(3) 0.1311(9) -0.2037(3) 0.084(3) Uani 1 1 d . . . H7A H -0.2094 0.1494 -0.1733 0.126 Uiso 1 1 calc R . . H7B H -0.2405 0.1503 -0.2170 0.126 Uiso 1 1 calc R . . H7C H -0.1807 0.2067 -0.2155 0.126 Uiso 1 1 calc R . . C8 C -0.1842(3) -0.0746(13) -0.2590(2) 0.083(2) Uani 1 1 d . . . H8A H -0.1703 -0.1847 -0.2639 0.124 Uiso 1 1 calc R . . H8B H -0.1605 0.0066 -0.2712 0.124 Uiso 1 1 calc R . . H8C H -0.2186 -0.0650 -0.2723 0.124 Uiso 1 1 calc R . . C9 C -0.13715(16) -0.0158(6) -0.12584(15) 0.0350(10) Uani 1 1 d . . . C10 C -0.11966(17) 0.1331(6) -0.10940(17) 0.0421(11) Uani 1 1 d . . . H10A H -0.0987 0.2028 -0.1263 0.050 Uiso 1 1 calc R . . C11 C -0.13234(19) 0.1806(8) -0.06881(18) 0.0491(13) Uani 1 1 d . . . H11A H -0.1199 0.2822 -0.0583 0.059 Uiso 1 1 calc R . . C12 C -0.1628(2) 0.0828(8) -0.04340(18) 0.0527(13) Uani 1 1 d . . . H12A H -0.1714 0.1164 -0.0156 0.063 Uiso 1 1 calc R . . C13 C -0.1805(2) -0.0648(8) -0.05896(18) 0.0540(14) Uani 1 1 d . . . H13A H -0.2018 -0.1330 -0.0419 0.065 Uiso 1 1 calc R . . C14 C -0.16754(19) -0.1137(7) -0.09911(17) 0.0444(12) Uani 1 1 d . . . H14A H -0.1795 -0.2168 -0.1090 0.053 Uiso 1 1 calc R . . C15 C 0.04898(19) 0.2498(9) -0.06270(18) 0.0546(15) Uani 1 1 d . . . C16 C 0.0059(2) 0.3787(9) -0.0598(2) 0.0687(19) Uani 1 1 d . . . H16A H -0.0233 0.3351 -0.0433 0.103 Uiso 1 1 calc R . . H16B H -0.0062 0.4068 -0.0881 0.103 Uiso 1 1 calc R . . H16C H 0.0196 0.4770 -0.0459 0.103 Uiso 1 1 calc R . . C17 C 0.0239(2) 0.0984(9) -0.0841(2) 0.0666(17) Uani 1 1 d . . . H17A H 0.0101 0.1296 -0.1117 0.100 Uiso 1 1 calc R . . H17B H -0.0045 0.0569 -0.0665 0.100 Uiso 1 1 calc R . . H17C H 0.0504 0.0128 -0.0876 0.100 Uiso 1 1 calc R . . C18 C 0.0658(3) 0.2005(16) -0.0186(2) 0.107(4) Uani 1 1 d . . . H18A H 0.0843 0.2918 -0.0053 0.161 Uiso 1 1 calc R . . H18B H 0.0890 0.1054 -0.0203 0.161 Uiso 1 1 calc R . . H18C H 0.0349 0.1725 -0.0019 0.161 Uiso 1 1 calc R . . C19 C 0.1339(2) 0.5357(8) -0.0825(2) 0.0598(16) Uani 1 1 d . . . C20 C 0.0975(3) 0.6778(9) -0.0943(3) 0.086(3) Uani 1 1 d . . . H20A H 0.0907 0.6753 -0.1247 0.129 Uiso 1 1 calc R . . H20B H 0.1141 0.7818 -0.0868 0.129 Uiso 1 1 calc R . . H20C H 0.0645 0.6668 -0.0791 0.129 Uiso 1 1 calc R . . C21 C 0.1846(2) 0.5569(9) -0.1077(3) 0.079(2) Uani 1 1 d . . . H21A H 0.1989 0.6664 -0.1026 0.119 Uiso 1 1 calc R . . H21B H 0.1773 0.5435 -0.1378 0.119 Uiso 1 1 calc R . . H21C H 0.2101 0.4743 -0.0987 0.119 Uiso 1 1 calc R . . C22 C 0.1458(4) 0.5479(12) -0.0352(3) 0.112(4) Uani 1 1 d . . . H22A H 0.1618 0.6543 -0.0291 0.168 Uiso 1 1 calc R . . H22B H 0.1700 0.4604 -0.0271 0.168 Uiso 1 1 calc R . . H22C H 0.1134 0.5367 -0.0191 0.168 Uiso 1 1 calc R . . C23 C 0.16235(15) 0.1741(6) -0.09420(15) 0.0355(10) Uani 1 1 d . . . C24 C 0.18309(16) 0.0984(7) -0.12971(17) 0.0413(11) Uani 1 1 d . . . H24A H 0.1668 0.1162 -0.1562 0.050 Uiso 1 1 calc R . . C25 C 0.22632(19) -0.0013(7) -0.12776(19) 0.0470(12) Uani 1 1 d . . . H25A H 0.2395 -0.0500 -0.1527 0.056 Uiso 1 1 calc R . . C26 C 0.25069(18) -0.0310(7) -0.0897(2) 0.0502(14) Uani 1 1 d . . . H26A H 0.2804 -0.1001 -0.0884 0.060 Uiso 1 1 calc R . . C27 C 0.23129(19) 0.0410(8) -0.05375(19) 0.0540(15) Uani 1 1 d . . . H27A H 0.2479 0.0222 -0.0274 0.065 Uiso 1 1 calc R . . C28 C 0.18756(19) 0.1406(8) -0.05578(18) 0.0502(14) Uani 1 1 d . . . H28A H 0.1743 0.1875 -0.0306 0.060 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 Pb1 0.04036(10) 0.04020(11) 0.03654(11) 0.00146(8) -0.00172(7) 0.00331(7) Te1 0.03582(14) 0.03262(17) 0.03541(17) 0.00084(12) 0.00159(12) -0.00200(11) Te2 0.04818(17) 0.04134(19) 0.0421(2) 0.00441(14) -0.01173(14) -0.00123(13) Si1 0.0348(5) 0.0293(6) 0.0341(7) 0.0005(5) -0.0009(5) -0.0009(5) Si2 0.0351(6) 0.0439(8) 0.0371(7) -0.0059(6) -0.0035(5) 0.0051(5) C1 0.059(3) 0.033(3) 0.053(3) 0.001(2) 0.014(2) 0.008(2) C2 0.082(4) 0.036(4) 0.145(8) 0.011(4) 0.040(5) 0.004(3) C3 0.076(4) 0.069(5) 0.085(5) 0.025(4) 0.000(4) 0.031(3) C4 0.116(5) 0.042(4) 0.078(5) -0.008(4) 0.031(4) 0.012(3) C5 0.045(2) 0.053(3) 0.038(3) 0.008(2) -0.009(2) -0.013(2) C6 0.040(2) 0.068(4) 0.052(3) 0.009(3) -0.004(2) -0.013(2) C7 0.057(3) 0.062(4) 0.132(8) 0.014(4) -0.046(4) 0.004(3) C8 0.063(4) 0.146(8) 0.039(3) 0.019(4) -0.009(3) -0.037(4) C9 0.0331(19) 0.039(3) 0.033(2) 0.002(2) -0.0034(18) 0.0049(17) C10 0.039(2) 0.043(3) 0.044(3) -0.001(2) 0.004(2) -0.0011(19) C11 0.048(3) 0.054(3) 0.045(3) -0.012(3) -0.001(2) -0.002(2) C12 0.052(3) 0.068(4) 0.038(3) -0.006(3) 0.003(2) -0.002(3) C13 0.054(3) 0.073(4) 0.035(3) 0.002(3) 0.002(2) -0.012(3) C14 0.051(3) 0.044(3) 0.038(3) 0.001(2) -0.001(2) -0.013(2) C15 0.039(2) 0.084(5) 0.040(3) 0.002(3) 0.006(2) 0.010(3) C16 0.047(3) 0.084(5) 0.075(5) -0.013(4) 0.013(3) 0.009(3) C17 0.055(3) 0.065(4) 0.081(5) 0.011(4) 0.023(3) -0.002(3) C18 0.058(4) 0.204(12) 0.059(5) 0.046(6) 0.005(3) -0.001(5) C19 0.056(3) 0.051(4) 0.072(4) -0.023(3) -0.008(3) 0.006(2) C20 0.074(4) 0.043(4) 0.141(8) -0.012(4) -0.006(4) 0.009(3) C21 0.058(3) 0.051(4) 0.129(7) -0.022(4) -0.006(4) -0.010(3) C22 0.155(8) 0.088(7) 0.091(7) -0.049(5) -0.049(6) 0.000(6) C23 0.0311(19) 0.043(3) 0.032(2) 0.003(2) 0.0013(18) -0.0016(18) C24 0.035(2) 0.049(3) 0.041(3) -0.002(2) -0.004(2) 0.001(2) C25 0.043(2) 0.047(3) 0.051(3) 0.004(3) 0.005(2) 0.006(2) C26 0.035(2) 0.045(3) 0.071(4) 0.013(3) 0.003(2) 0.003(2) C27 0.041(2) 0.076(4) 0.045(3) 0.012(3) -0.010(2) 0.006(3) C28 0.046(3) 0.069(4) 0.036(3) -0.001(3) -0.002(2) 0.008(2) _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 Pb1 Te2 2.8924(6) . ? Pb1 Te1 3.0303(7) 2_554 ? Pb1 Te1 3.0379(8) . ? Te1 Si1 2.5470(14) . ? Te1 Pb1 3.0303(7) 2_554 ? Te2 Si2 2.5155(15) . ? Si1 C9 1.887(5) . ? Si1 C1 1.917(5) . ? Si1 C5 1.919(5) . ? Si2 C23 1.901(5) . ? Si2 C19 1.920(6) . ? Si2 C15 1.925(6) . ? C1 C2 1.512(9) . ? C1 C4 1.536(9) . ? C1 C3 1.551(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.523(9) . ? C5 C7 1.527(9) . ? C5 C6 1.546(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.397(7) . ? C9 C14 1.403(7) . ? C10 C11 1.385(8) . ? C10 H10A 0.9500 . ? C11 C12 1.379(8) . ? C11 H11A 0.9500 . ? C12 C13 1.380(9) . ? C12 H12A 0.9500 . ? C13 C14 1.378(8) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C18 1.518(9) . ? C15 C16 1.528(8) . ? C15 C17 1.551(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C22 1.535(11) . ? C19 C20 1.536(9) . ? C19 C21 1.538(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.392(7) . ? C23 C28 1.407(7) . ? C24 C25 1.377(7) . ? C24 H24A 0.9500 . ? C25 C26 1.381(8) . ? C25 H25A 0.9500 . ? C26 C27 1.378(9) . ? C26 H26A 0.9500 . ? C27 C28 1.387(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te2 Pb1 Te1 88.285(14) . 2_554 ? Te2 Pb1 Te1 91.340(16) . . ? Te1 Pb1 Te1 81.65(3) 2_554 . ? Si1 Te1 Pb1 104.63(4) . 2_554 ? Si1 Te1 Pb1 110.68(3) . . ? Pb1 Te1 Pb1 90.03(3) 2_554 . ? Si2 Te2 Pb1 102.34(4) . . ? C9 Si1 C1 110.3(2) . . ? C9 Si1 C5 106.5(2) . . ? C1 Si1 C5 118.3(2) . . ? C9 Si1 Te1 106.01(15) . . ? C1 Si1 Te1 110.54(17) . . ? C5 Si1 Te1 104.37(17) . . ? C23 Si2 C19 106.8(2) . . ? C23 Si2 C15 110.0(2) . . ? C19 Si2 C15 115.6(3) . . ? C23 Si2 Te2 109.59(16) . . ? C19 Si2 Te2 103.9(2) . . ? C15 Si2 Te2 110.70(16) . . ? C2 C1 C4 109.0(6) . . ? C2 C1 C3 108.3(6) . . ? C4 C1 C3 106.8(5) . . ? C2 C1 Si1 113.2(4) . . ? C4 C1 Si1 112.1(4) . . ? C3 C1 Si1 107.1(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 110.1(6) . . ? C8 C5 C6 108.0(5) . . ? C7 C5 C6 107.0(5) . . ? C8 C5 Si1 112.8(4) . . ? C7 C5 Si1 108.0(3) . . ? C6 C5 Si1 110.8(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 116.6(5) . . ? C10 C9 Si1 123.3(4) . . ? C14 C9 Si1 120.0(4) . . ? C11 C10 C9 121.1(5) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 121.0(5) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 118.9(6) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 120.3(6) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C9 122.0(5) . . ? C13 C14 H14A 119.0 . . ? C9 C14 H14A 119.0 . . ? C18 C15 C16 109.3(6) . . ? C18 C15 C17 108.0(7) . . ? C16 C15 C17 106.1(5) . . ? C18 C15 Si2 113.1(4) . . ? C16 C15 Si2 111.3(5) . . ? C17 C15 Si2 108.7(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C20 108.2(7) . . ? C22 C19 C21 109.5(6) . . ? C20 C19 C21 107.5(7) . . ? C22 C19 Si2 111.6(6) . . ? C20 C19 Si2 113.1(4) . . ? C21 C19 Si2 106.8(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 116.2(4) . . ? C24 C23 Si2 122.7(4) . . ? C28 C23 Si2 121.0(4) . . ? C25 C24 C23 122.3(5) . . ? C25 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? C24 C25 C26 120.4(6) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C27 C26 C25 119.2(5) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C26 C27 C28 120.3(5) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C23 121.7(5) . . ? C27 C28 H28A 119.2 . . ? C23 C28 H28A 119.2 . . ? 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 Te2 Pb1 Te1 Si1 -136.03(4) . . . . ? Te1 Pb1 Te1 Si1 135.90(3) 2_554 . . . ? Te2 Pb1 Te1 Pb1 118.299(13) . . . 2_554 ? Te1 Pb1 Te1 Pb1 30.230(15) 2_554 . . 2_554 ? Te1 Pb1 Te2 Si2 -159.85(3) 2_554 . . . ? Te1 Pb1 Te2 Si2 118.55(4) . . . . ? Pb1 Te1 Si1 C9 -176.48(13) 2_554 . . . ? Pb1 Te1 Si1 C9 87.83(14) . . . . ? Pb1 Te1 Si1 C1 63.9(2) 2_554 . . . ? Pb1 Te1 Si1 C1 -31.7(2) . . . . ? Pb1 Te1 Si1 C5 -64.27(19) 2_554 . . . ? Pb1 Te1 Si1 C5 -159.96(19) . . . . ? Pb1 Te2 Si2 C23 58.32(16) . . . . ? Pb1 Te2 Si2 C19 172.13(19) . . . . ? Pb1 Te2 Si2 C15 -63.2(2) . . . . ? C9 Si1 C1 C2 77.1(6) . . . . ? C5 Si1 C1 C2 -45.8(6) . . . . ? Te1 Si1 C1 C2 -165.9(5) . . . . ? C9 Si1 C1 C4 -159.1(4) . . . . ? C5 Si1 C1 C4 78.1(5) . . . . ? Te1 Si1 C1 C4 -42.1(5) . . . . ? C9 Si1 C1 C3 -42.2(5) . . . . ? C5 Si1 C1 C3 -165.1(4) . . . . ? Te1 Si1 C1 C3 74.7(4) . . . . ? C9 Si1 C5 C8 173.7(5) . . . . ? C1 Si1 C5 C8 -61.5(6) . . . . ? Te1 Si1 C5 C8 61.8(5) . . . . ? C9 Si1 C5 C7 51.8(5) . . . . ? C1 Si1 C5 C7 176.6(5) . . . . ? Te1 Si1 C5 C7 -60.1(5) . . . . ? C9 Si1 C5 C6 -65.1(5) . . . . ? C1 Si1 C5 C6 59.7(5) . . . . ? Te1 Si1 C5 C6 -177.0(4) . . . . ? C1 Si1 C9 C10 128.4(4) . . . . ? C5 Si1 C9 C10 -102.0(4) . . . . ? Te1 Si1 C9 C10 8.7(4) . . . . ? C1 Si1 C9 C14 -55.5(4) . . . . ? C5 Si1 C9 C14 74.0(4) . . . . ? Te1 Si1 C9 C14 -175.2(3) . . . . ? C14 C9 C10 C11 -0.5(7) . . . . ? Si1 C9 C10 C11 175.7(4) . . . . ? C9 C10 C11 C12 -0.3(8) . . . . ? C10 C11 C12 C13 0.2(8) . . . . ? C11 C12 C13 C14 0.6(9) . . . . ? C12 C13 C14 C9 -1.4(8) . . . . ? C10 C9 C14 C13 1.3(7) . . . . ? Si1 C9 C14 C13 -175.0(4) . . . . ? C23 Si2 C15 C18 49.2(7) . . . . ? C19 Si2 C15 C18 -71.8(7) . . . . ? Te2 Si2 C15 C18 170.5(6) . . . . ? C23 Si2 C15 C16 172.7(4) . . . . ? C19 Si2 C15 C16 51.7(5) . . . . ? Te2 Si2 C15 C16 -66.0(5) . . . . ? C23 Si2 C15 C17 -70.8(4) . . . . ? C19 Si2 C15 C17 168.3(4) . . . . ? Te2 Si2 C15 C17 50.5(4) . . . . ? C23 Si2 C19 C22 -72.9(6) . . . . ? C15 Si2 C19 C22 49.8(6) . . . . ? Te2 Si2 C19 C22 171.3(5) . . . . ? C23 Si2 C19 C20 164.8(6) . . . . ? C15 Si2 C19 C20 -72.5(7) . . . . ? Te2 Si2 C19 C20 49.0(6) . . . . ? C23 Si2 C19 C21 46.7(5) . . . . ? C15 Si2 C19 C21 169.4(4) . . . . ? Te2 Si2 C19 C21 -69.1(5) . . . . ? C19 Si2 C23 C24 -111.5(5) . . . . ? C15 Si2 C23 C24 122.3(4) . . . . ? Te2 Si2 C23 C24 0.4(5) . . . . ? C19 Si2 C23 C28 64.4(5) . . . . ? C15 Si2 C23 C28 -61.7(5) . . . . ? Te2 Si2 C23 C28 176.4(4) . . . . ? C28 C23 C24 C25 -1.1(8) . . . . ? Si2 C23 C24 C25 175.0(4) . . . . ? C23 C24 C25 C26 0.5(8) . . . . ? C24 C25 C26 C27 -0.2(8) . . . . ? C25 C26 C27 C28 0.6(9) . . . . ? C26 C27 C28 C23 -1.3(9) . . . . ? C24 C23 C28 C27 1.5(8) . . . . ? Si2 C23 C28 C27 -174.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.610 _refine_diff_density_min -1.652 _refine_diff_density_rms 0.111 # Attachment '- Comp-4-CvH.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 876452' #TrackingRef '- Comp-4-CvH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H100 Pb2 Si8 Te2' _chemical_formula_sum 'C48 H100 Pb2 Si8 Te2' _chemical_formula_weight 1571.58 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' Pb Pb -3.3944 10.1111 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.153 0.604 0.017 7 2 ' ' 2 0.161 0.952 0.375 8 1 ' ' 3 0.205 0.255 0.108 14 3 ' ' 4 0.295 0.755 0.392 14 3 ' ' 5 0.338 0.452 0.125 8 1 ' ' 6 0.347 0.104 0.483 7 2 ' ' 7 0.661 0.548 0.875 8 1 ' ' 8 0.653 0.896 0.517 7 2 ' ' 9 0.705 0.245 0.608 14 3 ' ' 10 0.795 0.745 0.892 14 3 ' ' 11 0.838 0.048 0.625 8 1 ' ' 12 0.847 0.396 0.983 7 2 ' ' _platon_squeeze_details ; ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.762(6) _cell_length_b 19.778(7) _cell_length_c 25.104(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.36(4) _cell_angle_gamma 90.00 _cell_volume 6648(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 20820 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 26.62 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.1430 _exptl_crystal_size_mid 0.1230 _exptl_crystal_size_min 0.0350 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 6.090 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4408 _exptl_absorpt_correction_T_max 0.8502 _exptl_absorpt_process_details ; (a) W. R. Busing and H. A. Levy, Acta Crystallogr. 1957, 10, 180-182. (b) P. Coppens, L. Leiserowitz and D. Rabinovich, Acta Crystallogr. 1965, 18, 1035-1038. ; _exptl_special_details ; ? ; _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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41516 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.1173 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.79 _reflns_number_total 14056 _reflns_number_gt 7953 _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^)+(0.0814P)^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 14056 _refine_ls_number_parameters 573 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1312 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0357(10) 0.1156(6) 0.3751(7) 0.049(4) Uani 1 1 d . . . C2 C 0.0511(12) 0.0763(8) 0.3255(8) 0.065(5) Uani 1 1 d . . . H2A H 0.1223 0.0757 0.3255 0.098 Uiso 1 1 calc R . . H2B H 0.0136 0.0981 0.2919 0.098 Uiso 1 1 calc R . . H2C H 0.0272 0.0298 0.3271 0.098 Uiso 1 1 calc R . . C3 C 0.0691(11) 0.1899(7) 0.3678(7) 0.059(4) Uani 1 1 d . . . H3A H 0.0619 0.2171 0.3993 0.089 Uiso 1 1 calc R . . H3B H 0.0272 0.2091 0.3342 0.089 Uiso 1 1 calc R . . H3C H 0.1391 0.1902 0.3653 0.089 Uiso 1 1 calc R . . C4 C 0.1028(12) 0.0888(8) 0.4284(7) 0.065(5) Uani 1 1 d . . . H4A H 0.0809 0.0434 0.4359 0.098 Uiso 1 1 calc R . . H4B H 0.0982 0.1190 0.4587 0.098 Uiso 1 1 calc R . . H4C H 0.1721 0.0870 0.4247 0.098 Uiso 1 1 calc R . . C5 C -0.1609(11) 0.0252(6) 0.3771(6) 0.049(4) Uani 1 1 d . . . C6 C -0.1921(12) 0.0009(6) 0.3175(7) 0.060(4) Uani 1 1 d . . . H6A H -0.2283 -0.0420 0.3160 0.090 Uiso 1 1 calc R . . H6B H -0.1324 -0.0057 0.3030 0.090 Uiso 1 1 calc R . . H6C H -0.2354 0.0348 0.2954 0.090 Uiso 1 1 calc R . . C7 C -0.0861(11) -0.0270(6) 0.4105(7) 0.053(4) Uani 1 1 d . . . H7A H -0.1200 -0.0704 0.4114 0.080 Uiso 1 1 calc R . . H7B H -0.0615 -0.0104 0.4480 0.080 Uiso 1 1 calc R . . H7C H -0.0297 -0.0330 0.3932 0.080 Uiso 1 1 calc R . . C8 C -0.2530(11) 0.0266(7) 0.4016(8) 0.066(5) Uani 1 1 d . . . H8A H -0.3015 0.0592 0.3815 0.099 Uiso 1 1 calc R . . H8B H -0.2330 0.0400 0.4402 0.099 Uiso 1 1 calc R . . H8C H -0.2833 -0.0184 0.3988 0.099 Uiso 1 1 calc R . . C9 C -0.1089(10) 0.1626(7) 0.4427(6) 0.044(3) Uani 1 1 d . . . C10 C -0.1128(9) 0.2323(6) 0.4421(6) 0.045(3) Uani 1 1 d . . . H10 H -0.1163 0.2559 0.4087 0.054 Uiso 1 1 calc R . . C11 C -0.1117(11) 0.2686(7) 0.4900(7) 0.056(4) Uani 1 1 d . . . H11 H -0.1116 0.3166 0.4892 0.068 Uiso 1 1 calc R . . C12 C -0.1107(14) 0.2355(9) 0.5380(8) 0.070(5) Uani 1 1 d . . . H12 H -0.1156 0.2601 0.5697 0.084 Uiso 1 1 calc R . . C13 C -0.1024(14) 0.1658(8) 0.5397(8) 0.071(5) Uani 1 1 d . . . H13 H -0.0963 0.1427 0.5735 0.085 Uiso 1 1 calc R . . C14 C -0.1029(11) 0.1289(8) 0.4917(7) 0.058(4) Uani 1 1 d . . . H14 H -0.0991 0.0810 0.4929 0.070 Uiso 1 1 calc R . . C15 C -0.4658(10) -0.0590(6) 0.1504(6) 0.044(3) Uani 1 1 d . . . C16 C -0.3670(11) -0.0625(7) 0.1951(6) 0.051(4) Uani 1 1 d . . . H16A H -0.3315 -0.1043 0.1906 0.076 Uiso 1 1 calc R . . H16B H -0.3820 -0.0620 0.2314 0.076 Uiso 1 1 calc R . . H16C H -0.3251 -0.0235 0.1914 0.076 Uiso 1 1 calc R . . C17 C -0.4385(13) -0.0553(9) 0.0960(7) 0.066(5) Uani 1 1 d . . . H17A H -0.3970 -0.0943 0.0919 0.099 Uiso 1 1 calc R . . H17B H -0.4012 -0.0135 0.0940 0.099 Uiso 1 1 calc R . . H17C H -0.4994 -0.0556 0.0667 0.099 Uiso 1 1 calc R . . C18 C -0.5242(12) -0.1243(7) 0.1558(8) 0.066(5) Uani 1 1 d . . . H18A H -0.5816 -0.1282 0.1246 0.099 Uiso 1 1 calc R . . H18B H -0.5476 -0.1228 0.1898 0.099 Uiso 1 1 calc R . . H18C H -0.4803 -0.1635 0.1565 0.099 Uiso 1 1 calc R . . C19 C -0.6561(10) 0.0387(6) 0.1053(7) 0.049(4) Uani 1 1 d . . . C20 C -0.7160(11) 0.0967(8) 0.1239(7) 0.061(4) Uani 1 1 d . . . H20A H -0.6748 0.1376 0.1304 0.092 Uiso 1 1 calc R . . H20B H -0.7348 0.0837 0.1579 0.092 Uiso 1 1 calc R . . H20C H -0.7764 0.1057 0.0954 0.092 Uiso 1 1 calc R . . C21 C -0.7256(11) -0.0235(7) 0.0888(7) 0.056(4) Uani 1 1 d . . . H21A H -0.7861 -0.0096 0.0621 0.084 Uiso 1 1 calc R . . H21B H -0.7439 -0.0419 0.1214 0.084 Uiso 1 1 calc R . . H21C H -0.6906 -0.0581 0.0725 0.084 Uiso 1 1 calc R . . C22 C -0.6209(11) 0.0626(8) 0.0548(7) 0.058(4) Uani 1 1 d . . . H22A H -0.6790 0.0730 0.0252 0.086 Uiso 1 1 calc R . . H22B H -0.5813 0.0268 0.0429 0.086 Uiso 1 1 calc R . . H22C H -0.5797 0.1032 0.0641 0.086 Uiso 1 1 calc R . . C23 C -0.5806(10) -0.0011(6) 0.2309(6) 0.042(3) Uani 1 1 d . . . C24 C -0.5113(12) -0.0034(6) 0.2801(6) 0.050(4) Uani 1 1 d . . . H24 H -0.4433 0.0036 0.2794 0.060 Uiso 1 1 calc R . . C25 C -0.5325(12) -0.0152(6) 0.3303(7) 0.053(4) Uani 1 1 d . . . H25 H -0.4807 -0.0149 0.3628 0.064 Uiso 1 1 calc R . . C26 C -0.6324(14) -0.0275(8) 0.3330(8) 0.068(5) Uani 1 1 d . . . H26 H -0.6491 -0.0369 0.3669 0.082 Uiso 1 1 calc R . . C27 C -0.7068(14) -0.0255(8) 0.2837(8) 0.072(5) Uani 1 1 d . . . H27 H -0.7748 -0.0326 0.2844 0.086 Uiso 1 1 calc R . . C28 C -0.6813(11) -0.0132(7) 0.2343(7) 0.057(4) Uani 1 1 d . . . H28 H -0.7325 -0.0129 0.2017 0.068 Uiso 1 1 calc R . . C29 C -0.1615(10) 0.1767(6) 0.1232(5) 0.039(3) Uani 1 1 d . . . C30 C -0.2235(14) 0.2059(9) -0.0049(8) 0.077(5) Uani 1 1 d . . . H30A H -0.1795 0.2453 -0.0020 0.115 Uiso 1 1 calc R . . H30B H -0.2822 0.2127 -0.0350 0.115 Uiso 1 1 calc R . . H30C H -0.1875 0.1654 -0.0120 0.115 Uiso 1 1 calc R . . C31 C -0.3542(14) 0.1237(10) 0.0426(8) 0.082(6) Uani 1 1 d . . . H31A H -0.3170 0.0824 0.0386 0.123 Uiso 1 1 calc R . . H31B H -0.4005 0.1342 0.0076 0.123 Uiso 1 1 calc R . . H31C H -0.3919 0.1167 0.0708 0.123 Uiso 1 1 calc R . . C32 C -0.3455(14) 0.2691(8) 0.0704(11) 0.096(7) Uani 1 1 d . . . H32A H -0.3646 0.2662 0.1056 0.143 Uiso 1 1 calc R . . H32B H -0.4057 0.2690 0.0405 0.143 Uiso 1 1 calc R . . H32C H -0.3080 0.3109 0.0690 0.143 Uiso 1 1 calc R . . C33 C -0.1282(18) 0.0378(9) 0.0686(10) 0.107(8) Uani 1 1 d . . . H33A H -0.1733 0.0166 0.0887 0.161 Uiso 1 1 calc R . . H33B H -0.0760 0.0056 0.0650 0.161 Uiso 1 1 calc R . . H33C H -0.1661 0.0511 0.0320 0.161 Uiso 1 1 calc R . . C34 C 0.0151(15) 0.1545(11) 0.0648(9) 0.090(6) Uani 1 1 d . . . H34A H 0.0617 0.1204 0.0570 0.135 Uiso 1 1 calc R . . H34B H 0.0527 0.1917 0.0857 0.135 Uiso 1 1 calc R . . H34C H -0.0257 0.1720 0.0303 0.135 Uiso 1 1 calc R . . C35 C 0.0190(11) 0.0799(9) 0.1679(9) 0.075(6) Uani 1 1 d . . . H35A H -0.0159 0.0476 0.1866 0.112 Uiso 1 1 calc R . . H35B H 0.0456 0.1170 0.1929 0.112 Uiso 1 1 calc R . . H35C H 0.0741 0.0569 0.1566 0.112 Uiso 1 1 calc R . . C36 C -0.0697(17) 0.3152(9) 0.0897(9) 0.093(7) Uani 1 1 d . . . H36A H -0.0418 0.3588 0.1043 0.139 Uiso 1 1 calc R . . H36B H -0.1324 0.3227 0.0625 0.139 Uiso 1 1 calc R . . H36C H -0.0222 0.2920 0.0723 0.139 Uiso 1 1 calc R . . C37 C 0.0246(15) 0.2480(11) 0.2017(11) 0.105(8) Uani 1 1 d . . . H37A H 0.0140 0.2178 0.2308 0.157 Uiso 1 1 calc R . . H37B H 0.0481 0.2921 0.2175 0.157 Uiso 1 1 calc R . . H37C H 0.0747 0.2284 0.1842 0.157 Uiso 1 1 calc R . . C38 C -0.1697(17) 0.3165(8) 0.1847(9) 0.089(7) Uani 1 1 d . . . H38A H -0.1534 0.3070 0.2241 0.134 Uiso 1 1 calc R . . H38B H -0.2411 0.3088 0.1697 0.134 Uiso 1 1 calc R . . H38C H -0.1534 0.3637 0.1786 0.134 Uiso 1 1 calc R . . C39 C -0.5044(9) 0.2600(5) 0.3120(6) 0.037(3) Uani 1 1 d . . . C40 C -0.3777(11) 0.2274(8) 0.4302(6) 0.053(4) Uani 1 1 d . . . H40A H -0.4318 0.1970 0.4344 0.080 Uiso 1 1 calc R . . H40B H -0.3479 0.2484 0.4656 0.080 Uiso 1 1 calc R . . H40C H -0.3266 0.2015 0.4176 0.080 Uiso 1 1 calc R . . C41 C -0.3180(11) 0.3466(7) 0.3717(7) 0.056(4) Uani 1 1 d . . . H41A H -0.2728 0.3184 0.3563 0.084 Uiso 1 1 calc R . . H41B H -0.2830 0.3631 0.4078 0.084 Uiso 1 1 calc R . . H41C H -0.3402 0.3852 0.3474 0.084 Uiso 1 1 calc R . . C42 C -0.5055(12) 0.3531(7) 0.4126(7) 0.059(4) Uani 1 1 d . . . H42A H -0.5356 0.3887 0.3870 0.088 Uiso 1 1 calc R . . H42B H -0.4621 0.3735 0.4451 0.088 Uiso 1 1 calc R . . H42C H -0.5583 0.3270 0.4235 0.088 Uiso 1 1 calc R . . C43 C -0.6170(13) 0.3008(8) 0.1926(7) 0.065(4) Uani 1 1 d . . . H43A H -0.6192 0.3356 0.1646 0.098 Uiso 1 1 calc R . . H43B H -0.6805 0.3003 0.2039 0.098 Uiso 1 1 calc R . . H43C H -0.6057 0.2565 0.1775 0.098 Uiso 1 1 calc R . . C44 C -0.3963(13) 0.3230(7) 0.2272(7) 0.061(4) Uani 1 1 d . . . H44A H -0.3425 0.3435 0.2549 0.092 Uiso 1 1 calc R . . H44B H -0.4082 0.3502 0.1936 0.092 Uiso 1 1 calc R . . H44C H -0.3772 0.2771 0.2192 0.092 Uiso 1 1 calc R . . C45 C -0.5364(12) 0.4090(7) 0.2726(6) 0.054(4) Uani 1 1 d . . . H45A H -0.4829 0.4234 0.3035 0.081 Uiso 1 1 calc R . . H45B H -0.6006 0.4112 0.2831 0.081 Uiso 1 1 calc R . . H45C H -0.5381 0.4389 0.2413 0.081 Uiso 1 1 calc R . . C46 C -0.6228(11) 0.1776(7) 0.3814(8) 0.059(4) Uani 1 1 d . . . H46A H -0.5732 0.1415 0.3834 0.089 Uiso 1 1 calc R . . H46B H -0.6883 0.1576 0.3804 0.089 Uiso 1 1 calc R . . H46C H -0.6034 0.2069 0.4136 0.089 Uiso 1 1 calc R . . C47 C -0.7240(11) 0.2974(7) 0.3172(7) 0.057(4) Uani 1 1 d . . . H47A H -0.7002 0.3280 0.3482 0.085 Uiso 1 1 calc R . . H47B H -0.7877 0.2773 0.3201 0.085 Uiso 1 1 calc R . . H47C H -0.7335 0.3229 0.2829 0.085 Uiso 1 1 calc R . . C48 C -0.6875(10) 0.1667(7) 0.2632(7) 0.055(4) Uani 1 1 d . . . H48A H -0.7032 0.1897 0.2276 0.083 Uiso 1 1 calc R . . H48B H -0.7489 0.1485 0.2710 0.083 Uiso 1 1 calc R . . H48C H -0.6406 0.1296 0.2622 0.083 Uiso 1 1 calc R . . Pb1 Pb -0.21636(4) 0.10840(2) 0.19205(3) 0.04552(15) Uani 1 1 d . . . Pb2 Pb -0.42101(4) 0.15458(2) 0.30316(2) 0.04082(14) Uani 1 1 d . . . Si1 Si -0.1017(3) 0.11394(17) 0.37906(18) 0.0447(9) Uani 1 1 d . . . Si2 Si -0.5442(3) 0.01647(16) 0.16481(17) 0.0413(9) Uani 1 1 d . . . Si3 Si -0.2657(3) 0.1948(2) 0.0627(2) 0.0568(11) Uani 1 1 d . . . Si4 Si -0.0698(4) 0.1142(2) 0.1065(2) 0.0678(13) Uani 1 1 d . . . Si5 Si -0.0954(4) 0.2592(2) 0.1497(2) 0.0686(14) Uani 1 1 d . . . Si6 Si -0.5126(3) 0.31983(17) 0.25327(18) 0.0482(10) Uani 1 1 d . . . Si7 Si -0.6293(3) 0.22855(17) 0.31813(19) 0.0460(9) Uani 1 1 d . . . Si8 Si -0.4295(3) 0.29528(19) 0.37846(18) 0.0469(9) Uani 1 1 d . . . Te1 Te -0.19937(7) 0.18792(4) 0.30043(4) 0.0438(2) Uani 1 1 d . . . Te2 Te -0.44605(7) 0.12861(4) 0.18021(4) 0.0424(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(7) 0.039(7) 0.069(10) -0.011(7) 0.007(7) 0.007(6) C2 0.053(9) 0.061(9) 0.086(13) -0.023(9) 0.026(9) 0.006(8) C3 0.051(9) 0.044(8) 0.078(12) -0.005(7) 0.008(8) -0.008(7) C4 0.049(9) 0.061(9) 0.081(13) 0.003(9) 0.004(9) 0.010(7) C5 0.056(9) 0.032(6) 0.058(10) -0.002(6) 0.012(7) 0.008(6) C6 0.068(10) 0.026(6) 0.078(12) 0.003(7) 0.000(9) -0.009(6) C7 0.062(9) 0.034(6) 0.061(10) 0.006(6) 0.009(8) 0.010(6) C8 0.046(9) 0.046(8) 0.102(15) 0.009(8) 0.010(9) -0.007(7) C9 0.038(7) 0.048(7) 0.042(8) 0.002(6) 0.002(6) -0.003(6) C10 0.035(7) 0.041(7) 0.054(9) -0.010(6) 0.002(6) 0.002(6) C11 0.059(9) 0.045(8) 0.067(11) -0.001(8) 0.017(8) 0.009(7) C12 0.082(13) 0.065(10) 0.059(12) -0.010(9) 0.007(10) 0.021(9) C13 0.085(13) 0.063(10) 0.059(11) 0.002(8) 0.008(9) 0.027(9) C14 0.053(9) 0.052(8) 0.073(12) -0.007(8) 0.019(8) 0.013(7) C15 0.047(8) 0.025(5) 0.065(10) -0.006(6) 0.024(7) -0.005(5) C16 0.063(9) 0.036(6) 0.054(10) -0.003(6) 0.013(8) 0.002(6) C17 0.072(11) 0.072(10) 0.057(11) -0.006(8) 0.021(9) 0.025(9) C18 0.065(10) 0.032(7) 0.100(14) -0.004(8) 0.017(10) -0.004(7) C19 0.045(8) 0.035(6) 0.066(10) -0.007(6) 0.013(7) 0.001(6) C20 0.046(8) 0.068(10) 0.069(11) -0.005(8) 0.011(8) -0.003(7) C21 0.049(9) 0.052(8) 0.062(11) -0.006(7) 0.002(8) -0.011(7) C22 0.053(9) 0.057(8) 0.059(11) 0.006(8) 0.004(8) -0.003(7) C23 0.056(8) 0.025(5) 0.045(9) 0.003(5) 0.013(7) 0.009(5) C24 0.077(11) 0.026(6) 0.059(10) 0.011(6) 0.038(9) 0.002(6) C25 0.061(9) 0.037(7) 0.068(11) 0.003(7) 0.028(8) -0.009(6) C26 0.084(12) 0.071(10) 0.063(12) -0.022(9) 0.042(10) -0.030(9) C27 0.070(11) 0.071(10) 0.088(14) -0.025(10) 0.047(11) -0.031(9) C28 0.050(9) 0.053(8) 0.073(12) -0.021(8) 0.026(8) -0.022(7) C29 0.044(7) 0.040(6) 0.036(7) 0.003(5) 0.013(6) 0.000(6) C30 0.070(12) 0.072(11) 0.088(14) 0.000(10) 0.016(10) -0.020(9) C31 0.068(11) 0.111(15) 0.071(13) -0.034(11) 0.023(10) 0.007(11) C32 0.064(12) 0.046(9) 0.17(2) 0.008(11) 0.018(13) 0.004(8) C33 0.14(2) 0.062(11) 0.103(18) -0.022(11) -0.007(15) 0.046(12) C34 0.076(13) 0.117(16) 0.094(16) 0.002(13) 0.055(12) 0.018(12) C35 0.044(9) 0.064(10) 0.118(17) 0.039(10) 0.023(10) 0.003(8) C36 0.123(18) 0.059(10) 0.107(17) -0.010(11) 0.049(14) -0.040(11) C37 0.071(13) 0.101(16) 0.14(2) -0.044(15) 0.016(14) -0.017(12) C38 0.125(17) 0.038(8) 0.097(16) -0.006(9) 0.007(13) 0.000(10) C39 0.040(7) 0.026(5) 0.046(8) -0.007(5) 0.014(6) 0.002(5) C40 0.056(9) 0.071(9) 0.037(8) 0.006(7) 0.018(7) -0.003(7) C41 0.052(9) 0.034(6) 0.081(12) -0.010(7) 0.014(8) -0.014(6) C42 0.057(9) 0.051(8) 0.077(12) 0.002(8) 0.032(9) -0.019(7) C43 0.086(12) 0.057(9) 0.048(10) 0.005(7) 0.008(9) 0.018(9) C44 0.089(12) 0.037(7) 0.068(11) 0.006(7) 0.037(10) 0.006(7) C45 0.074(10) 0.043(7) 0.051(10) 0.012(7) 0.026(8) 0.007(7) C46 0.049(9) 0.042(7) 0.096(13) 0.009(8) 0.034(9) -0.001(6) C47 0.056(9) 0.041(7) 0.070(11) -0.001(7) 0.009(8) 0.008(7) C48 0.027(6) 0.053(8) 0.087(12) -0.017(8) 0.015(7) -0.006(6) Pb1 0.0474(3) 0.0309(2) 0.0639(4) 0.0002(2) 0.0243(3) -0.0026(2) Pb2 0.0435(3) 0.0288(2) 0.0538(3) 0.0026(2) 0.0187(2) 0.0013(2) Si1 0.041(2) 0.0349(17) 0.058(3) 0.0004(17) 0.0100(18) 0.0035(15) Si2 0.046(2) 0.0299(16) 0.053(2) -0.0033(16) 0.0206(18) -0.0053(15) Si3 0.053(2) 0.057(2) 0.065(3) 0.018(2) 0.022(2) 0.005(2) Si4 0.078(3) 0.069(3) 0.065(3) 0.011(2) 0.035(3) 0.029(3) Si5 0.080(3) 0.063(3) 0.075(3) -0.013(2) 0.043(3) -0.029(2) Si6 0.062(3) 0.0292(16) 0.058(3) 0.0033(17) 0.025(2) 0.0034(16) Si7 0.045(2) 0.0338(17) 0.065(3) -0.0024(17) 0.024(2) 0.0004(15) Si8 0.049(2) 0.0413(19) 0.054(3) -0.0020(17) 0.021(2) -0.0069(17) Te1 0.0431(5) 0.0296(4) 0.0597(6) 0.0009(4) 0.0141(4) -0.0002(3) Te2 0.0460(5) 0.0306(4) 0.0542(6) -0.0020(4) 0.0190(4) -0.0057(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.52(2) . ? C1 C4 1.53(2) . ? C1 C3 1.564(19) . ? C1 Si1 1.916(14) . ? C5 C8 1.53(2) . ? C5 C6 1.54(2) . ? C5 C7 1.559(18) . ? C5 Si1 1.930(14) . ? C9 C10 1.379(18) . ? C9 C14 1.38(2) . ? C9 Si1 1.887(15) . ? C10 C11 1.40(2) . ? C11 C12 1.37(2) . ? C12 C13 1.38(2) . ? C13 C14 1.41(2) . ? C15 C17 1.50(2) . ? C15 C18 1.545(18) . ? C15 C16 1.55(2) . ? C15 Si2 1.923(13) . ? C19 C22 1.53(2) . ? C19 C20 1.55(2) . ? C19 C21 1.553(18) . ? C19 Si2 1.933(15) . ? C23 C24 1.38(2) . ? C23 C28 1.429(19) . ? C23 Si2 1.873(15) . ? C24 C25 1.38(2) . ? C25 C26 1.41(2) . ? C26 C27 1.41(3) . ? C27 C28 1.39(2) . ? C29 Si3 1.866(14) . ? C29 Si4 1.881(13) . ? C29 Si5 1.912(13) . ? C29 Pb1 2.447(13) . ? C30 Si3 1.93(2) . ? C31 Si3 1.85(2) . ? C32 Si3 1.871(18) . ? C33 Si4 1.87(2) . ? C34 Si4 1.913(19) . ? C35 Si4 1.861(18) . ? C36 Si5 1.97(2) . ? C37 Si5 1.87(2) . ? C38 Si5 1.88(2) . ? C39 Si7 1.867(13) . ? C39 Si6 1.874(14) . ? C39 Si8 1.881(13) . ? C39 Pb2 2.414(11) . ? C40 Si8 1.890(15) . ? C41 Si8 1.880(14) . ? C42 Si8 1.884(16) . ? C43 Si6 1.875(17) . ? C44 Si6 1.865(16) . ? C45 Si6 1.878(14) . ? C46 Si7 1.866(17) . ? C47 Si7 1.882(14) . ? C48 Si7 1.880(15) . ? Pb1 Te1 3.1045(11) . ? Pb1 Te2 3.1315(11) . ? Pb2 Te2 3.0689(11) . ? Pb2 Te1 3.1368(10) . ? Si1 Te1 2.573(4) . ? Si2 Te2 2.579(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 C2 C1 C4 111.6(12) . . ? C2 C1 C3 106.5(14) . . ? C4 C1 C3 107.0(12) . . ? C2 C1 Si1 111.0(10) . . ? C4 C1 Si1 110.6(11) . . ? C3 C1 Si1 110.0(9) . . ? C8 C5 C6 109.0(13) . . ? C8 C5 C7 107.5(13) . . ? C6 C5 C7 108.5(11) . . ? C8 C5 Si1 110.9(9) . . ? C6 C5 Si1 109.3(10) . . ? C7 C5 Si1 111.5(10) . . ? C10 C9 C14 119.0(14) . . ? C10 C9 Si1 120.7(11) . . ? C14 C9 Si1 120.1(11) . . ? C9 C10 C11 120.8(15) . . ? C12 C11 C10 120.5(14) . . ? C11 C12 C13 119.2(17) . . ? C12 C13 C14 120.4(17) . . ? C9 C14 C13 119.9(15) . . ? C17 C15 C18 111.5(13) . . ? C17 C15 C16 107.3(12) . . ? C18 C15 C16 106.5(12) . . ? C17 C15 Si2 113.8(10) . . ? C18 C15 Si2 107.9(9) . . ? C16 C15 Si2 109.6(9) . . ? C22 C19 C20 108.3(12) . . ? C22 C19 C21 108.5(13) . . ? C20 C19 C21 109.3(12) . . ? C22 C19 Si2 111.2(10) . . ? C20 C19 Si2 108.6(11) . . ? C21 C19 Si2 110.9(10) . . ? C24 C23 C28 114.9(14) . . ? C24 C23 Si2 122.0(11) . . ? C28 C23 Si2 123.1(12) . . ? C23 C24 C25 125.3(15) . . ? C24 C25 C26 119.1(16) . . ? C27 C26 C25 118.1(16) . . ? C28 C27 C26 120.4(16) . . ? C27 C28 C23 122.2(16) . . ? Si3 C29 Si4 111.9(7) . . ? Si3 C29 Si5 109.5(6) . . ? Si4 C29 Si5 110.5(7) . . ? Si3 C29 Pb1 112.0(6) . . ? Si4 C29 Pb1 97.3(5) . . ? Si5 C29 Pb1 115.1(6) . . ? Si7 C39 Si6 112.7(7) . . ? Si7 C39 Si8 112.1(7) . . ? Si6 C39 Si8 112.6(6) . . ? Si7 C39 Pb2 100.8(5) . . ? Si6 C39 Pb2 114.6(6) . . ? Si8 C39 Pb2 103.2(5) . . ? C29 Pb1 Te1 111.5(3) . . ? C29 Pb1 Te2 109.4(3) . . ? Te1 Pb1 Te2 83.60(3) . . ? C39 Pb2 Te2 107.0(3) . . ? C39 Pb2 Te1 107.8(3) . . ? Te2 Pb2 Te1 84.09(3) . . ? C9 Si1 C1 106.3(6) . . ? C9 Si1 C5 112.4(7) . . ? C1 Si1 C5 115.4(6) . . ? C9 Si1 Te1 103.8(4) . . ? C1 Si1 Te1 107.3(5) . . ? C5 Si1 Te1 110.8(5) . . ? C23 Si2 C15 107.4(6) . . ? C23 Si2 C19 113.5(7) . . ? C15 Si2 C19 114.4(6) . . ? C23 Si2 Te2 105.3(4) . . ? C15 Si2 Te2 113.5(4) . . ? C19 Si2 Te2 102.5(4) . . ? C31 Si3 C29 114.2(8) . . ? C31 Si3 C32 105.1(8) . . ? C29 Si3 C32 115.2(9) . . ? C31 Si3 C30 99.1(8) . . ? C29 Si3 C30 114.0(7) . . ? C32 Si3 C30 107.6(10) . . ? C35 Si4 C33 104.5(9) . . ? C35 Si4 C29 113.6(8) . . ? C33 Si4 C29 114.4(9) . . ? C35 Si4 C34 103.8(9) . . ? C33 Si4 C34 107.7(11) . . ? C29 Si4 C34 112.0(8) . . ? C37 Si5 C38 103.5(10) . . ? C37 Si5 C29 114.5(8) . . ? C38 Si5 C29 114.4(8) . . ? C37 Si5 C36 108.4(11) . . ? C38 Si5 C36 103.5(9) . . ? C29 Si5 C36 111.7(7) . . ? C44 Si6 C39 113.4(6) . . ? C44 Si6 C43 106.2(8) . . ? C39 Si6 C43 114.1(7) . . ? C44 Si6 C45 105.9(7) . . ? C39 Si6 C45 111.9(6) . . ? C43 Si6 C45 104.6(7) . . ? C46 Si7 C39 112.7(7) . . ? C46 Si7 C48 101.7(7) . . ? C39 Si7 C48 113.6(6) . . ? C46 Si7 C47 107.3(7) . . ? C39 Si7 C47 114.0(6) . . ? C48 Si7 C47 106.6(7) . . ? C41 Si8 C39 114.3(7) . . ? C41 Si8 C42 105.3(6) . . ? C39 Si8 C42 112.4(7) . . ? C41 Si8 C40 105.1(7) . . ? C39 Si8 C40 112.9(6) . . ? C42 Si8 C40 106.2(7) . . ? Si1 Te1 Pb1 107.73(9) . . ? Si1 Te1 Pb2 101.65(9) . . ? Pb1 Te1 Pb2 92.06(3) . . ? Si2 Te2 Pb2 103.17(10) . . ? Si2 Te2 Pb1 112.75(9) . . ? Pb2 Te2 Pb1 92.84(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.79 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.439 _refine_diff_density_min -2.438 _refine_diff_density_rms 0.214 # Attachment '- Comp-5-CvH.CIF' data_e:\traut\crystal\ah9\ah9abs\p21n _database_code_depnum_ccdc_archive 'CCDC 876453' #TrackingRef '- Comp-5-CvH.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H108 Si16 Sn4 Te6' _chemical_formula_weight 2231.02 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5474(19) _cell_length_b 26.049(5) _cell_length_c 17.285(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.70(3) _cell_angle_gamma 90.00 _cell_volume 4297.0(15) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2068 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.11 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.281 _exptl_crystal_size_mid 0.092 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 3.390 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6503 _exptl_absorpt_correction_T_max 0.9040 _exptl_absorpt_process_details ; (a) W. R. Busing and H. A. Levy, Acta Crystallogr. 1957, 10, 180-182. (b) P. Coppens, L. Leiserowitz and D. Rabinovich, Acta Crystallogr. 1965, 18, 1035-1038. ; _exptl_special_details ; ? ; _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 IPDS2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19869 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.62 _reflns_number_total 7752 _reflns_number_gt 6339 _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^)+(0.0549P)^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 7752 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1296(8) 0.2142(3) 0.9930(6) 0.075(3) Uani 1 1 d . . . H1A H 0.1411 0.1768 0.9939 0.090 Uiso 1 1 calc R . . H1B H 0.1845 0.2294 1.0360 0.090 Uiso 1 1 calc R . . H1C H 0.1626 0.2277 0.9439 0.090 Uiso 1 1 calc R . . C2 C -0.1158(12) 0.2042(4) 1.0975(5) 0.091(3) Uani 1 1 d . . . H2A H -0.0589 0.2195 1.1397 0.109 Uiso 1 1 calc R . . H2B H -0.1036 0.1669 1.0980 0.109 Uiso 1 1 calc R . . H2C H -0.2147 0.2126 1.1045 0.109 Uiso 1 1 calc R . . C3 C -0.0721(10) 0.3019(3) 1.0047(7) 0.083(3) Uani 1 1 d . . . H3A H -0.0373 0.3160 0.9563 0.100 Uiso 1 1 calc R . . H3B H -0.0158 0.3154 1.0485 0.100 Uiso 1 1 calc R . . H3C H -0.1702 0.3120 1.0103 0.100 Uiso 1 1 calc R . . C4 C -0.4913(8) 0.1558(3) 0.9909(5) 0.063(2) Uani 1 1 d . . . H4A H -0.5906 0.1595 1.0026 0.076 Uiso 1 1 calc R . . H4B H -0.4349 0.1565 1.0392 0.076 Uiso 1 1 calc R . . H4C H -0.4768 0.1231 0.9642 0.076 Uiso 1 1 calc R . . C5 C -0.4661(8) 0.2720(3) 0.9793(5) 0.061(2) Uani 1 1 d . . . H5A H -0.4099 0.2725 1.0277 0.073 Uiso 1 1 calc R . . H5B H -0.5655 0.2755 0.9909 0.073 Uiso 1 1 calc R . . H5C H -0.4379 0.3006 0.9464 0.073 Uiso 1 1 calc R . . C6 C -0.5464(8) 0.2086(3) 0.8357(5) 0.0613(19) Uani 1 1 d . . . H6A H -0.6455 0.2125 0.8478 0.074 Uiso 1 1 calc R . . H6B H -0.5326 0.1758 0.8090 0.074 Uiso 1 1 calc R . . H6C H -0.5182 0.2369 0.8021 0.074 Uiso 1 1 calc R . . C7 C -0.2294(10) 0.3094(3) 0.7819(7) 0.094(4) Uani 1 1 d . . . H7A H -0.3309 0.3072 0.7879 0.113 Uiso 1 1 calc R . . H7B H -0.2096 0.3267 0.7330 0.113 Uiso 1 1 calc R . . H7C H -0.1873 0.3289 0.8251 0.113 Uiso 1 1 calc R . . C8 C -0.2318(12) 0.2061(4) 0.6978(5) 0.091(3) Uani 1 1 d . . . H8A H -0.2116 0.2237 0.6493 0.109 Uiso 1 1 calc R . . H8B H -0.3335 0.2038 0.7033 0.109 Uiso 1 1 calc R . . H8C H -0.1918 0.1714 0.6970 0.109 Uiso 1 1 calc R . . C9 C 0.0403(9) 0.2469(4) 0.7679(6) 0.082(3) Uani 1 1 d . . . H9A H 0.0836 0.2665 0.8106 0.098 Uiso 1 1 calc R . . H9B H 0.0585 0.2641 0.7188 0.098 Uiso 1 1 calc R . . H9C H 0.0801 0.2122 0.7673 0.098 Uiso 1 1 calc R . . C10 C 0.3793(13) 0.1107(3) 0.6824(5) 0.093(4) Uani 1 1 d . . . H10A H 0.3450 0.1185 0.7340 0.112 Uiso 1 1 calc R . . H10B H 0.3812 0.1422 0.6516 0.112 Uiso 1 1 calc R . . H10C H 0.4740 0.0964 0.6873 0.112 Uiso 1 1 calc R . . C11 C 0.0829(11) 0.0915(3) 0.6245(5) 0.078(3) Uani 1 1 d . . . H11A H 0.0870 0.1231 0.5939 0.093 Uiso 1 1 calc R . . H11B H 0.0490 0.0995 0.6761 0.093 Uiso 1 1 calc R . . H11C H 0.0188 0.0671 0.5987 0.093 Uiso 1 1 calc R . . C12 C 0.3277(10) 0.0486(3) 0.5355(4) 0.064(2) Uani 1 1 d . . . H12A H 0.4218 0.0337 0.5409 0.077 Uiso 1 1 calc R . . H12B H 0.3317 0.0804 0.5054 0.077 Uiso 1 1 calc R . . H12C H 0.2650 0.0241 0.5088 0.077 Uiso 1 1 calc R . . C13 C 0.0009(11) -0.0671(3) 0.5888(5) 0.075(2) Uani 1 1 d . . . H13A H -0.0639 -0.0575 0.6292 0.089 Uiso 1 1 calc R . . H13B H -0.0366 -0.0967 0.5601 0.089 Uiso 1 1 calc R . . H13C H 0.0119 -0.0381 0.5532 0.089 Uiso 1 1 calc R . . C14 C 0.1435(11) -0.1394(3) 0.6995(6) 0.079(3) Uani 1 1 d . . . H14A H 0.1038 -0.1682 0.6696 0.095 Uiso 1 1 calc R . . H14B H 0.0784 -0.1294 0.7396 0.095 Uiso 1 1 calc R . . H14C H 0.2331 -0.1498 0.7238 0.095 Uiso 1 1 calc R . . C15 C 0.2961(14) -0.1013(4) 0.5554(8) 0.125(6) Uani 1 1 d . . . H15A H 0.3071 -0.0720 0.5205 0.150 Uiso 1 1 calc R . . H15B H 0.2583 -0.1307 0.5261 0.150 Uiso 1 1 calc R . . H15C H 0.3874 -0.1105 0.5789 0.150 Uiso 1 1 calc R . . C16 C 0.4818(8) 0.0165(3) 0.8589(5) 0.064(2) Uani 1 1 d . . . H16A H 0.5703 0.0102 0.8875 0.076 Uiso 1 1 calc R . . H16B H 0.4033 0.0109 0.8931 0.076 Uiso 1 1 calc R . . H16C H 0.4799 0.0520 0.8401 0.076 Uiso 1 1 calc R . . C17 C 0.4709(10) -0.0962(3) 0.8113(6) 0.074(2) Uani 1 1 d . . . H17A H 0.3927 -0.1017 0.8458 0.088 Uiso 1 1 calc R . . H17B H 0.5596 -0.1024 0.8398 0.088 Uiso 1 1 calc R . . H17C H 0.4628 -0.1200 0.7675 0.088 Uiso 1 1 calc R . . C18 C 0.6169(10) -0.0187(5) 0.7095(6) 0.093(3) Uani 1 1 d . . . H18C H 0.6082 -0.0423 0.6655 0.112 Uiso 1 1 calc R . . H18B H 0.7051 -0.0254 0.7382 0.112 Uiso 1 1 calc R . . H18A H 0.6163 0.0168 0.6906 0.112 Uiso 1 1 calc R . . Si1 Si -0.19920(16) 0.20102(5) 0.89815(10) 0.0352(3) Uani 1 1 d . . . Si2 Si -0.0589(2) 0.23052(6) 1.00290(12) 0.0474(4) Uani 1 1 d . . . Si3 Si -0.43729(17) 0.20976(6) 0.92752(11) 0.0400(4) Uani 1 1 d . . . Si4 Si -0.1529(2) 0.24281(7) 0.78118(14) 0.0574(5) Uani 1 1 d . . . Si5 Si 0.25436(17) -0.01336(5) 0.70623(10) 0.0352(3) Uani 1 1 d . . . Si6 Si 0.46661(19) -0.02853(8) 0.77476(12) 0.0499(4) Uani 1 1 d . . . Si7 Si 0.1724(2) -0.08370(6) 0.63341(12) 0.0476(4) Uani 1 1 d . . . Si8 Si 0.2599(2) 0.06287(6) 0.63354(11) 0.0507(5) Uani 1 1 d . . . Sn1 Sn 0.12446(4) 0.092647(13) 0.86652(2) 0.03652(11) Uani 1 1 d . . . Sn2 Sn -0.14325(5) 0.051091(14) 1.04071(3) 0.04224(12) Uani 1 1 d . . . Te1 Te -0.17284(4) 0.106205(12) 0.86887(2) 0.03711(10) Uani 1 1 d . . . Te2 Te 0.05245(4) -0.005166(13) 0.79777(2) 0.03581(10) Uani 1 1 d . . . Te3 Te 0.15885(4) 0.052053(14) 1.02596(2) 0.03983(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(4) 0.084(5) 0.098(7) -0.046(5) -0.014(5) 0.006(4) C2 0.096(8) 0.120(8) 0.056(5) -0.013(5) -0.005(5) -0.037(6) C3 0.074(6) 0.042(4) 0.134(9) -0.034(4) 0.003(6) -0.005(4) C4 0.046(4) 0.059(4) 0.086(6) 0.021(4) 0.016(4) 0.000(3) C5 0.047(4) 0.051(4) 0.084(6) -0.013(3) 0.000(4) 0.014(3) C6 0.040(4) 0.062(4) 0.082(6) -0.014(4) -0.003(4) 0.005(3) C7 0.069(6) 0.064(5) 0.151(10) 0.056(6) 0.031(6) 0.019(4) C8 0.095(8) 0.121(8) 0.057(5) 0.034(5) 0.002(5) 0.022(6) C9 0.056(5) 0.092(6) 0.099(7) 0.035(5) 0.029(5) -0.004(4) C10 0.156(11) 0.060(4) 0.064(5) -0.002(4) 0.009(6) -0.064(6) C11 0.114(8) 0.061(4) 0.059(5) 0.020(4) 0.018(5) 0.031(5) C12 0.081(6) 0.064(4) 0.048(4) 0.000(3) 0.017(4) -0.013(4) C13 0.092(7) 0.069(5) 0.062(5) -0.014(4) -0.021(5) -0.003(4) C14 0.086(7) 0.048(4) 0.101(7) 0.001(4) -0.020(6) -0.015(4) C15 0.116(10) 0.103(7) 0.161(12) -0.089(8) 0.074(9) -0.028(7) C16 0.037(4) 0.079(5) 0.075(5) -0.020(4) -0.001(4) -0.007(3) C17 0.064(5) 0.082(5) 0.074(6) -0.001(4) -0.007(5) 0.032(4) C18 0.043(5) 0.159(10) 0.079(7) -0.008(6) 0.011(5) 0.001(5) Si1 0.0288(8) 0.0270(6) 0.0499(9) 0.0016(6) 0.0032(7) 0.0002(5) Si2 0.0382(9) 0.0417(8) 0.0622(12) -0.0160(8) 0.0028(9) -0.0051(7) Si3 0.0298(8) 0.0334(7) 0.0571(11) 0.0001(7) 0.0031(8) 0.0040(6) Si4 0.0476(11) 0.0541(10) 0.0712(14) 0.0284(9) 0.0128(10) 0.0061(8) Si5 0.0341(8) 0.0338(7) 0.0380(8) -0.0021(6) 0.0038(7) -0.0018(6) Si6 0.0303(9) 0.0675(11) 0.0520(11) -0.0061(8) 0.0005(8) 0.0039(8) Si7 0.0497(11) 0.0391(8) 0.0542(11) -0.0124(7) 0.0060(9) -0.0021(7) Si8 0.0752(14) 0.0398(8) 0.0377(9) -0.0003(7) 0.0122(9) -0.0075(8) Sn1 0.0374(2) 0.03422(18) 0.0381(2) 0.00250(15) 0.00417(18) -0.00212(15) Sn2 0.0384(2) 0.0386(2) 0.0501(3) 0.00390(17) 0.0090(2) 0.00711(16) Te1 0.0354(2) 0.02858(16) 0.0471(2) -0.00017(14) -0.00403(18) 0.00287(13) Te2 0.0333(2) 0.03777(18) 0.0365(2) -0.00328(14) 0.00361(16) -0.00069(14) Te3 0.0360(2) 0.0454(2) 0.0379(2) 0.00250(15) -0.00145(17) -0.00460(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si2 1.862(8) . ? C2 Si2 1.869(10) . ? C3 Si2 1.865(7) . ? C4 Si3 1.864(7) . ? C5 Si3 1.876(7) . ? C6 Si3 1.873(9) . ? C7 Si4 1.882(8) . ? C8 Si4 1.870(11) . ? C9 Si4 1.869(9) . ? C10 Si8 1.873(8) . ? C11 Si8 1.850(10) . ? C12 Si8 1.869(7) . ? C13 Si7 1.842(10) . ? C14 Si7 1.873(9) . ? C15 Si7 1.875(9) . ? C16 Si6 1.870(8) . ? C17 Si6 1.874(8) . ? C18 Si6 1.869(9) . ? Si1 Si2 2.349(3) . ? Si1 Si4 2.350(3) . ? Si1 Si3 2.355(2) . ? Si1 Te1 2.5353(15) . ? Si5 Si7 2.344(2) . ? Si5 Si6 2.350(3) . ? Si5 Si8 2.351(2) . ? Si5 Te2 2.5389(18) . ? Sn1 Te1 2.8618(8) . ? Sn1 Te2 2.8859(7) . ? Sn1 Te3 2.9610(8) . ? Sn2 Te3 2.9032(8) . ? Sn2 Te3 2.9256(8) 3_557 ? Sn2 Te2 3.1360(9) 3_557 ? Te2 Sn2 3.1360(9) 3_557 ? Te3 Sn2 2.9256(8) 3_557 ? 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 Si2 Si1 Si4 113.21(10) . . ? Si2 Si1 Si3 109.54(9) . . ? Si4 Si1 Si3 110.37(10) . . ? Si2 Si1 Te1 114.51(8) . . ? Si4 Si1 Te1 104.90(8) . . ? Si3 Si1 Te1 103.85(6) . . ? C1 Si2 C3 107.2(4) . . ? C1 Si2 C2 107.7(5) . . ? C3 Si2 C2 109.2(5) . . ? C1 Si2 Si1 112.6(3) . . ? C3 Si2 Si1 107.6(4) . . ? C2 Si2 Si1 112.4(3) . . ? C4 Si3 C6 109.2(4) . . ? C4 Si3 C5 108.9(4) . . ? C6 Si3 C5 109.4(4) . . ? C4 Si3 Si1 109.9(2) . . ? C6 Si3 Si1 109.4(3) . . ? C5 Si3 Si1 110.0(3) . . ? C9 Si4 C8 108.1(5) . . ? C9 Si4 C7 109.5(4) . . ? C8 Si4 C7 109.2(5) . . ? C9 Si4 Si1 110.1(3) . . ? C8 Si4 Si1 110.2(3) . . ? C7 Si4 Si1 109.8(3) . . ? Si7 Si5 Si6 114.09(9) . . ? Si7 Si5 Si8 112.68(10) . . ? Si6 Si5 Si8 112.25(10) . . ? Si7 Si5 Te2 98.79(7) . . ? Si6 Si5 Te2 111.06(8) . . ? Si8 Si5 Te2 106.95(8) . . ? C18 Si6 C16 109.9(4) . . ? C18 Si6 C17 108.8(5) . . ? C16 Si6 C17 109.1(4) . . ? C18 Si6 Si5 109.8(4) . . ? C16 Si6 Si5 109.4(3) . . ? C17 Si6 Si5 109.8(3) . . ? C13 Si7 C14 107.0(4) . . ? C13 Si7 C15 109.1(6) . . ? C14 Si7 C15 110.9(5) . . ? C13 Si7 Si5 108.6(3) . . ? C14 Si7 Si5 109.3(3) . . ? C15 Si7 Si5 111.7(3) . . ? C11 Si8 C12 110.1(4) . . ? C11 Si8 C10 108.2(5) . . ? C12 Si8 C10 108.6(4) . . ? C11 Si8 Si5 110.5(3) . . ? C12 Si8 Si5 109.3(3) . . ? C10 Si8 Si5 110.1(3) . . ? Te1 Sn1 Te2 83.72(2) . . ? Te1 Sn1 Te3 96.52(3) . . ? Te2 Sn1 Te3 94.96(2) . . ? Te3 Sn2 Te3 90.713(19) . 3_557 ? Te3 Sn2 Te2 80.35(3) . 3_557 ? Te3 Sn2 Te2 90.563(19) 3_557 3_557 ? Si1 Te1 Sn1 103.15(4) . . ? Si5 Te2 Sn1 98.91(4) . . ? Si5 Te2 Sn2 109.13(4) . 3_557 ? Sn1 Te2 Sn2 85.07(2) . 3_557 ? Sn2 Te3 Sn2 89.287(19) . 3_557 ? Sn2 Te3 Sn1 90.10(3) . . ? Sn2 Te3 Sn1 87.617(19) 3_557 . ? 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 Si4 Si1 Si2 C1 -67.0(4) . . . . ? Si3 Si1 Si2 C1 169.4(4) . . . . ? Te1 Si1 Si2 C1 53.2(4) . . . . ? Si4 Si1 Si2 C3 51.0(4) . . . . ? Si3 Si1 Si2 C3 -72.7(3) . . . . ? Te1 Si1 Si2 C3 171.2(3) . . . . ? Si4 Si1 Si2 C2 171.2(4) . . . . ? Si3 Si1 Si2 C2 47.6(4) . . . . ? Te1 Si1 Si2 C2 -68.6(4) . . . . ? Si2 Si1 Si3 C4 -79.7(3) . . . . ? Si4 Si1 Si3 C4 155.0(3) . . . . ? Te1 Si1 Si3 C4 43.0(3) . . . . ? Si2 Si1 Si3 C6 160.4(3) . . . . ? Si4 Si1 Si3 C6 35.1(3) . . . . ? Te1 Si1 Si3 C6 -76.8(3) . . . . ? Si2 Si1 Si3 C5 40.2(3) . . . . ? Si4 Si1 Si3 C5 -85.1(3) . . . . ? Te1 Si1 Si3 C5 162.9(3) . . . . ? Si2 Si1 Si4 C9 45.8(4) . . . . ? Si3 Si1 Si4 C9 169.0(4) . . . . ? Te1 Si1 Si4 C9 -79.7(4) . . . . ? Si2 Si1 Si4 C8 164.9(4) . . . . ? Si3 Si1 Si4 C8 -71.9(4) . . . . ? Te1 Si1 Si4 C8 39.4(4) . . . . ? Si2 Si1 Si4 C7 -74.8(4) . . . . ? Si3 Si1 Si4 C7 48.4(4) . . . . ? Te1 Si1 Si4 C7 159.7(4) . . . . ? Si7 Si5 Si6 C18 83.0(4) . . . . ? Si8 Si5 Si6 C18 -46.8(4) . . . . ? Te2 Si5 Si6 C18 -166.5(4) . . . . ? Si7 Si5 Si6 C16 -156.4(3) . . . . ? Si8 Si5 Si6 C16 73.9(3) . . . . ? Te2 Si5 Si6 C16 -45.8(3) . . . . ? Si7 Si5 Si6 C17 -36.7(3) . . . . ? Si8 Si5 Si6 C17 -166.4(3) . . . . ? Te2 Si5 Si6 C17 73.9(3) . . . . ? Si6 Si5 Si7 C13 176.3(3) . . . . ? Si8 Si5 Si7 C13 -54.1(4) . . . . ? Te2 Si5 Si7 C13 58.5(4) . . . . ? Si6 Si5 Si7 C14 59.9(4) . . . . ? Si8 Si5 Si7 C14 -170.6(4) . . . . ? Te2 Si5 Si7 C14 -58.0(4) . . . . ? Si6 Si5 Si7 C15 -63.2(6) . . . . ? Si8 Si5 Si7 C15 66.3(6) . . . . ? Te2 Si5 Si7 C15 178.9(6) . . . . ? Si7 Si5 Si8 C11 79.7(3) . . . . ? Si6 Si5 Si8 C11 -149.9(3) . . . . ? Te2 Si5 Si8 C11 -27.8(3) . . . . ? Si7 Si5 Si8 C12 -41.7(3) . . . . ? Si6 Si5 Si8 C12 88.8(3) . . . . ? Te2 Si5 Si8 C12 -149.2(3) . . . . ? Si7 Si5 Si8 C10 -160.9(4) . . . . ? Si6 Si5 Si8 C10 -30.4(4) . . . . ? Te2 Si5 Si8 C10 91.7(4) . . . . ? Si2 Si1 Te1 Sn1 -48.58(9) . . . . ? Si4 Si1 Te1 Sn1 76.13(8) . . . . ? Si3 Si1 Te1 Sn1 -167.98(7) . . . . ? Te2 Sn1 Te1 Si1 -167.07(4) . . . . ? Te3 Sn1 Te1 Si1 98.63(4) . . . . ? Si7 Si5 Te2 Sn1 -169.24(7) . . . . ? Si6 Si5 Te2 Sn1 70.61(7) . . . . ? Si8 Si5 Te2 Sn1 -52.18(8) . . . . ? Si7 Si5 Te2 Sn2 102.92(7) . . . 3_557 ? Si6 Si5 Te2 Sn2 -17.22(8) . . . 3_557 ? Si8 Si5 Te2 Sn2 -140.01(7) . . . 3_557 ? Te1 Sn1 Te2 Si5 145.36(4) . . . . ? Te3 Sn1 Te2 Si5 -118.61(5) . . . . ? Te1 Sn1 Te2 Sn2 -106.01(3) . . . 3_557 ? Te3 Sn1 Te2 Sn2 -9.979(15) . . . 3_557 ? Te3 Sn2 Te3 Sn2 0.0 3_557 . . 3_557 ? Te2 Sn2 Te3 Sn2 90.450(19) 3_557 . . 3_557 ? Te3 Sn2 Te3 Sn1 87.616(19) 3_557 . . . ? Te2 Sn2 Te3 Sn1 178.066(14) 3_557 . . . ? Te1 Sn1 Te3 Sn2 5.614(15) . . . . ? Te2 Sn1 Te3 Sn2 -78.609(19) . . . . ? Te1 Sn1 Te3 Sn2 94.896(19) . . . 3_557 ? Te2 Sn1 Te3 Sn2 10.674(17) . . . 3_557 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.780 _refine_diff_density_min -1.328 _refine_diff_density_rms 0.138