# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Alan Cowley' _publ_contact_author_address ; Chemistry & Biochemistry The University of Texas at Austin Austin Texas 78712-0165 UNITED STATES OF AMERICA ; _publ_contact_author_email COWLEY@MAIL.UTEXAS.EDU _publ_section_title ; pi-Indenyl tin(II) and lead(II) compounds ; loop_ _publ_author_name 'Alan Cowley' 'Jamie N. Jones' data_p21212 _database_code_depnum_ccdc_archive 'CCDC 244711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H76 Si4 Sn2' _chemical_formula_weight 1026.85 _chemical_absolute_configuration unk 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 21.232(5) _cell_length_b 24.238(5) _cell_length_c 10.398(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 5351(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) __cell_measurement_reflns_used all _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.23 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite __diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23473 _diffrn_reflns_av_R_equivalents 0.1077 _diffrn_reflns_av_sigmaI/netI 0.1457 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.23 _reflns_number_total 11903 _reflns_number_gt 7413 _reflns_threshold_expression >2sigma(I) __computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0207P)^2^+10.2428P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00174(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 11903 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0703(3) 0.7877(4) 0.9633(8) 0.050(2) Uani 1 1 d . . . C2 C 0.1083(4) 0.8001(3) 0.8544(8) 0.049(2) Uani 1 1 d . . . C3 C 0.1549(4) 0.7631(4) 0.8480(9) 0.057(2) Uani 1 1 d . . . C4 C 0.1503(4) 0.7259(3) 0.9465(9) 0.048(2) Uani 1 1 d . . . C5 C 0.0974(4) 0.7396(4) 1.0219(8) 0.051(2) Uani 1 1 d . . . C6 C 0.0210(5) 0.8238(5) 1.0227(14) 0.131(6) Uani 1 1 d . . . H6A H 0.0413 0.8517 1.0770 0.196 Uiso 1 1 calc R . . H6B H -0.0074 0.8013 1.0752 0.196 Uiso 1 1 calc R . . H6C H -0.0032 0.8422 0.9547 0.196 Uiso 1 1 calc R . . C7 C 0.1035(7) 0.8533(4) 0.7758(12) 0.137(6) Uani 1 1 d . . . H7A H 0.1353 0.8796 0.8057 0.205 Uiso 1 1 calc R . . H7B H 0.0614 0.8693 0.7867 0.205 Uiso 1 1 calc R . . H7C H 0.1106 0.8450 0.6847 0.205 Uiso 1 1 calc R . . C8 C 0.2086(5) 0.7636(6) 0.7454(11) 0.130(6) Uani 1 1 d . . . H8A H 0.2416 0.7893 0.7722 0.195 Uiso 1 1 calc R . . H8B H 0.1914 0.7753 0.6623 0.195 Uiso 1 1 calc R . . H8C H 0.2264 0.7265 0.7372 0.195 Uiso 1 1 calc R . . C9 C 0.1962(5) 0.6793(4) 0.9722(14) 0.118(5) Uani 1 1 d . . . H9A H 0.1735 0.6477 1.0086 0.177 Uiso 1 1 calc R . . H9B H 0.2284 0.6917 1.0332 0.177 Uiso 1 1 calc R . . H9C H 0.2164 0.6683 0.8915 0.177 Uiso 1 1 calc R . . C10 C 0.0780(6) 0.7135(5) 1.1471(8) 0.127(6) Uani 1 1 d . . . H10A H 0.1048 0.7274 1.2166 0.191 Uiso 1 1 calc R . . H10B H 0.0826 0.6733 1.1409 0.191 Uiso 1 1 calc R . . H10C H 0.0340 0.7226 1.1653 0.191 Uiso 1 1 calc R . . C11 C -0.0805(3) 0.7377(3) 0.7815(7) 0.0290(17) Uani 1 1 d . . . C12 C -0.0589(3) 0.7392(3) 0.6507(6) 0.0295(16) Uani 1 1 d . . . C13 C -0.0533(3) 0.6819(2) 0.6162(6) 0.0245(15) Uani 1 1 d . . . C14 C -0.0377(4) 0.6555(3) 0.4999(7) 0.0328(18) Uani 1 1 d . . . C15 C -0.0390(4) 0.5996(3) 0.4917(7) 0.0362(18) Uani 1 1 d . . . C16 C -0.0549(3) 0.5669(3) 0.5984(7) 0.0371(19) Uani 1 1 d . . . H16 H -0.0554 0.5279 0.5899 0.045 Uiso 1 1 calc R . . C17 C -0.0697(3) 0.5903(3) 0.7143(7) 0.0295(17) Uani 1 1 d . . . H17 H -0.0803 0.5679 0.7861 0.035 Uiso 1 1 calc R . . C18 C -0.0687(3) 0.6483(3) 0.7250(6) 0.0250(16) Uani 1 1 d . . . C19 C -0.0845(3) 0.6838(3) 0.8314(6) 0.0275(16) Uani 1 1 d . . . C20 C 0.0183(6) 0.8032(5) 0.4571(12) 0.065(3) Uani 1 1 d . . . C21 C -0.0708(4) 0.8641(3) 0.6305(8) 0.046(2) Uani 1 1 d . . . H21A H -0.0353 0.8710 0.6885 0.069 Uiso 1 1 calc R . . H21B H -0.1097 0.8611 0.6808 0.069 Uiso 1 1 calc R . . H21C H -0.0746 0.8947 0.5695 0.069 Uiso 1 1 calc R . . C22 C -0.1200(4) 0.7910(4) 0.4190(7) 0.062(3) Uani 1 1 d . . . H22A H -0.1142 0.7562 0.3728 0.093 Uiso 1 1 calc R . . H22B H -0.1179 0.8218 0.3579 0.093 Uiso 1 1 calc R . . H22C H -0.1612 0.7911 0.4615 0.093 Uiso 1 1 calc R . . C23 C -0.1300(5) 0.7256(4) 1.0872(8) 0.073(3) Uani 1 1 d . . . H23A H -0.0890 0.7427 1.1044 0.110 Uiso 1 1 calc R . . H23B H -0.1501 0.7156 1.1688 0.110 Uiso 1 1 calc R . . H23C H -0.1568 0.7517 1.0406 0.110 Uiso 1 1 calc R . . C24 C -0.1959(4) 0.6296(4) 0.9626(7) 0.049(2) Uani 1 1 d . . . H24A H -0.1908 0.5979 0.9052 0.074 Uiso 1 1 calc R . . H24B H -0.2250 0.6562 0.9235 0.074 Uiso 1 1 calc R . . H24C H -0.2131 0.6172 1.0452 0.074 Uiso 1 1 calc R . . C25 C -0.0668(4) 0.6133(3) 1.0763(7) 0.055(2) Uani 1 1 d . . . H25A H -0.0269 0.6314 1.0980 0.082 Uiso 1 1 calc R . . H25B H -0.0586 0.5812 1.0214 0.082 Uiso 1 1 calc R . . H25C H -0.0878 0.6012 1.1554 0.082 Uiso 1 1 calc R . . C26 C 0.2515(4) 0.3986(3) 0.4432(7) 0.046(2) Uani 1 1 d . . . C27 C 0.2631(4) 0.3633(3) 0.5473(8) 0.043(2) Uani 1 1 d . . . C28 C 0.3186(3) 0.3791(3) 0.6103(7) 0.0377(19) Uani 1 1 d . . . C29 C 0.3432(3) 0.4262(3) 0.5424(8) 0.0375(19) Uani 1 1 d . . . C30 C 0.3008(4) 0.4371(3) 0.4376(8) 0.048(2) Uani 1 1 d . . . C31 C 0.1987(4) 0.3929(5) 0.3480(10) 0.086(4) Uani 1 1 d . . . H31A H 0.1854 0.4296 0.3191 0.129 Uiso 1 1 calc R . . H31B H 0.1631 0.3741 0.3888 0.129 Uiso 1 1 calc R . . H31C H 0.2132 0.3713 0.2739 0.129 Uiso 1 1 calc R . . C32 C 0.2237(4) 0.3142(4) 0.5882(10) 0.075(3) Uani 1 1 d . . . H32A H 0.1831 0.3152 0.5434 0.112 Uiso 1 1 calc R . . H32B H 0.2166 0.3157 0.6813 0.112 Uiso 1 1 calc R . . H32C H 0.2459 0.2801 0.5664 0.112 Uiso 1 1 calc R . . C33 C 0.3482(4) 0.3509(4) 0.7229(8) 0.058(2) Uani 1 1 d . . . H33A H 0.3557 0.3121 0.7020 0.087 Uiso 1 1 calc R . . H33B H 0.3200 0.3534 0.7973 0.087 Uiso 1 1 calc R . . H33C H 0.3884 0.3688 0.7434 0.087 Uiso 1 1 calc R . . C34 C 0.4062(4) 0.4523(4) 0.5610(9) 0.064(3) Uani 1 1 d . . . H34A H 0.4378 0.4321 0.5110 0.096 Uiso 1 1 calc R . . H34B H 0.4175 0.4512 0.6524 0.096 Uiso 1 1 calc R . . H34C H 0.4047 0.4907 0.5319 0.096 Uiso 1 1 calc R . . C35 C 0.3129(5) 0.4792(4) 0.3322(9) 0.084(3) Uani 1 1 d . . . H35A H 0.3425 0.4638 0.2694 0.126 Uiso 1 1 calc R . . H35B H 0.3309 0.5127 0.3701 0.126 Uiso 1 1 calc R . . H35C H 0.2732 0.4883 0.2892 0.126 Uiso 1 1 calc R . . C36 C 0.2770(3) 0.5726(3) 0.6610(7) 0.0301(18) Uani 1 1 d . . . C37 C 0.2831(3) 0.5537(3) 0.7891(6) 0.0282(16) Uani 1 1 d . . . C38 C 0.2181(3) 0.5488(2) 0.8335(6) 0.0268(16) Uani 1 1 d . . . C39 C 0.1926(4) 0.5334(3) 0.9535(6) 0.0336(17) Uani 1 1 d . . . H39 H 0.2195 0.5226 1.0221 0.040 Uiso 1 1 calc R . . C40 C 0.1286(4) 0.5341(4) 0.9695(8) 0.040(2) Uani 1 1 d . . . C41 C 0.0881(4) 0.5496(3) 0.8717(8) 0.0407(19) Uani 1 1 d . . . H41 H 0.0440 0.5503 0.8871 0.049 Uiso 1 1 calc R . . C42 C 0.1108(3) 0.5641(3) 0.7533(7) 0.0317(17) Uani 1 1 d . . . H42 H 0.0826 0.5738 0.6861 0.038 Uiso 1 1 calc R . . C43 C 0.1765(3) 0.5644(3) 0.7316(6) 0.0262(16) Uani 1 1 d . . . C44 C 0.2130(3) 0.5782(3) 0.6187(6) 0.0300(17) Uani 1 1 d . . . C45 C 0.2491(4) 0.6271(3) 0.3582(8) 0.058(2) Uani 1 1 d . . . H45A H 0.2335 0.6326 0.2705 0.088 Uiso 1 1 calc R . . H45B H 0.2812 0.5980 0.3582 0.088 Uiso 1 1 calc R . . H45C H 0.2677 0.6616 0.3897 0.088 Uiso 1 1 calc R . . C46 C 0.1324(4) 0.5555(3) 0.3781(8) 0.053(2) Uani 1 1 d . . . H46A H 0.1161 0.5723 0.2991 0.079 Uiso 1 1 calc R . . H46B H 0.0972 0.5445 0.4333 0.079 Uiso 1 1 calc R . . H46C H 0.1576 0.5230 0.3564 0.079 Uiso 1 1 calc R . . C47 C 0.1350(4) 0.6689(3) 0.4959(8) 0.050(2) Uani 1 1 d . . . H47A H 0.1178 0.6827 0.4145 0.074 Uiso 1 1 calc R . . H47B H 0.1615 0.6974 0.5351 0.074 Uiso 1 1 calc R . . H47C H 0.1003 0.6597 0.5543 0.074 Uiso 1 1 calc R . . C48 C 0.4252(3) 0.5703(3) 0.7955(8) 0.052(2) Uani 1 1 d . . . H48A H 0.4216 0.6090 0.7694 0.078 Uiso 1 1 calc R . . H48B H 0.4285 0.5470 0.7188 0.078 Uiso 1 1 calc R . . H48C H 0.4629 0.5655 0.8487 0.078 Uiso 1 1 calc R . . C49 C 0.3662(4) 0.4797(3) 0.9557(8) 0.059(2) Uani 1 1 d . . . H49A H 0.3771 0.4543 0.8858 0.088 Uiso 1 1 calc R . . H49B H 0.3274 0.4673 0.9976 0.088 Uiso 1 1 calc R . . H49C H 0.4005 0.4804 1.0188 0.088 Uiso 1 1 calc R . . C50 C 0.3479(4) 0.5982(4) 1.0264(8) 0.057(2) Uani 1 1 d . . . H50A H 0.3860 0.5958 1.0791 0.085 Uiso 1 1 calc R . . H50B H 0.3111 0.5883 1.0786 0.085 Uiso 1 1 calc R . . H50C H 0.3430 0.6359 0.9941 0.085 Uiso 1 1 calc R . . Si1 Si -0.05727(10) 0.79883(8) 0.54107(19) 0.0344(5) Uani 1 1 d . . . Si2 Si -0.11859(10) 0.66291(9) 0.98903(19) 0.0361(5) Uani 1 1 d . . . Si3 Si 0.18272(10) 0.60658(9) 0.46491(19) 0.0343(5) Uani 1 1 d . . . Si4 Si 0.35435(10) 0.55011(8) 0.88938(19) 0.0355(5) Uani 1 1 d . . . Sn1 Sn 0.04255(2) 0.713376(19) 0.81024(4) 0.03015(14) Uani 1 1 d . . . Sn2 Sn 0.24394(2) 0.465810(19) 0.63945(4) 0.03168(14) Uani 1 1 d . . . H11 H -0.090(2) 0.768(2) 0.833(5) 0.006(14) Uiso 1 1 d . . . H14 H -0.025(2) 0.676(2) 0.431(5) 0.007(15) Uiso 1 1 d . . . H15 H -0.029(3) 0.581(2) 0.407(6) 0.034(18) Uiso 1 1 d . . . H20A H 0.051(4) 0.804(3) 0.526(8) 0.06(3) Uiso 1 1 d . . . H20B H 0.030(5) 0.774(4) 0.443(10) 0.08(4) Uiso 1 1 d . . . H20C H 0.022(3) 0.833(3) 0.403(6) 0.03(2) Uiso 1 1 d . . . H36 H 0.305(3) 0.580(3) 0.601(7) 0.04(2) Uiso 1 1 d . . . H40 H 0.111(3) 0.528(2) 1.038(5) 0.008(16) Uiso 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 0.031(4) 0.046(5) 0.073(6) -0.044(5) -0.014(4) 0.011(4) C2 0.055(5) 0.039(5) 0.053(5) 0.004(4) -0.017(5) -0.008(4) C3 0.050(5) 0.066(6) 0.055(6) -0.014(5) -0.006(5) -0.010(5) C4 0.048(5) 0.037(5) 0.060(6) -0.019(4) -0.020(5) 0.004(4) C5 0.064(6) 0.053(5) 0.037(5) 0.002(4) -0.009(5) -0.035(5) C6 0.062(8) 0.145(12) 0.185(14) -0.112(11) -0.031(8) 0.029(8) C7 0.200(14) 0.074(8) 0.136(12) 0.057(8) -0.112(11) -0.059(9) C8 0.078(8) 0.223(16) 0.087(8) -0.057(9) 0.019(7) -0.084(9) C9 0.082(8) 0.060(7) 0.212(15) -0.049(8) -0.089(9) 0.038(6) C10 0.192(13) 0.156(11) 0.034(5) 0.013(7) -0.030(7) -0.126(11) C11 0.030(4) 0.026(4) 0.031(4) -0.010(3) 0.005(3) 0.002(3) C12 0.031(4) 0.035(4) 0.022(4) -0.005(3) 0.007(3) -0.001(3) C13 0.026(4) 0.024(3) 0.024(4) 0.002(3) -0.001(3) -0.003(3) C14 0.036(5) 0.035(4) 0.028(4) -0.007(3) -0.002(4) -0.010(4) C15 0.034(4) 0.043(5) 0.032(4) -0.018(4) 0.000(4) 0.001(4) C16 0.040(5) 0.026(4) 0.046(5) -0.012(3) -0.001(4) -0.006(3) C17 0.030(4) 0.029(4) 0.030(4) 0.002(3) -0.012(3) -0.003(3) C18 0.024(4) 0.027(4) 0.025(4) 0.003(3) -0.002(3) -0.003(3) C19 0.036(4) 0.028(4) 0.019(4) -0.001(3) 0.001(3) -0.002(3) C20 0.092(9) 0.040(6) 0.062(7) 0.016(5) 0.025(7) 0.000(6) C21 0.051(5) 0.031(4) 0.057(5) -0.002(4) -0.004(4) 0.003(4) C22 0.098(7) 0.043(5) 0.044(5) 0.020(4) -0.016(5) -0.001(5) C23 0.094(7) 0.076(7) 0.050(5) -0.020(5) 0.043(5) -0.030(6) C24 0.043(5) 0.070(6) 0.035(5) 0.007(4) 0.002(4) -0.015(4) C25 0.050(5) 0.072(6) 0.042(5) 0.019(4) 0.000(4) -0.012(5) C26 0.039(5) 0.062(5) 0.037(5) -0.029(4) 0.005(4) 0.013(5) C27 0.030(5) 0.044(5) 0.053(5) -0.015(4) 0.010(4) 0.007(4) C28 0.028(4) 0.041(4) 0.044(5) -0.014(4) 0.005(4) 0.006(4) C29 0.029(4) 0.033(4) 0.051(5) -0.020(4) 0.014(4) 0.003(4) C30 0.050(5) 0.050(5) 0.043(5) -0.004(4) 0.008(4) 0.015(5) C31 0.064(6) 0.124(9) 0.070(7) -0.063(7) -0.021(6) 0.033(6) C32 0.051(6) 0.065(6) 0.108(8) -0.039(6) 0.037(6) -0.016(5) C33 0.042(5) 0.071(6) 0.060(6) 0.010(5) 0.002(4) 0.030(5) C34 0.044(5) 0.056(6) 0.092(7) -0.019(5) 0.015(5) -0.011(5) C35 0.105(8) 0.092(8) 0.054(6) 0.015(6) 0.036(6) 0.047(6) C36 0.032(4) 0.027(4) 0.032(5) 0.001(3) 0.006(3) -0.001(3) C37 0.039(4) 0.022(3) 0.024(4) 0.004(3) -0.003(3) 0.001(3) C38 0.040(4) 0.020(3) 0.020(4) -0.005(3) -0.002(3) -0.003(3) C39 0.051(5) 0.028(4) 0.022(4) -0.007(3) 0.000(3) -0.002(4) C40 0.046(5) 0.044(5) 0.031(4) 0.002(4) 0.021(4) -0.010(4) C41 0.040(4) 0.039(5) 0.043(5) -0.007(4) 0.004(4) 0.003(4) C42 0.036(4) 0.027(4) 0.032(4) -0.010(3) 0.008(4) 0.005(3) C43 0.027(4) 0.020(3) 0.031(4) -0.010(3) 0.010(3) 0.008(3) C44 0.031(4) 0.039(4) 0.020(4) -0.003(3) 0.002(3) -0.001(3) C45 0.050(5) 0.073(5) 0.052(5) 0.023(5) 0.005(5) -0.003(5) C46 0.058(5) 0.062(6) 0.038(5) -0.003(4) -0.010(4) 0.009(4) C47 0.058(6) 0.055(5) 0.037(5) 0.001(4) -0.004(4) 0.014(5) C48 0.048(5) 0.055(5) 0.054(5) -0.006(5) -0.009(5) -0.006(4) C49 0.062(6) 0.064(6) 0.051(5) 0.014(5) -0.007(5) 0.004(5) C50 0.052(6) 0.067(6) 0.052(5) -0.022(5) -0.013(5) 0.008(5) Si1 0.0421(13) 0.0300(11) 0.0310(11) 0.0030(9) 0.0062(10) -0.0011(10) Si2 0.0398(13) 0.0448(13) 0.0237(11) 0.0022(10) 0.0073(10) -0.0114(11) Si3 0.0336(12) 0.0459(12) 0.0234(11) 0.0032(10) -0.0016(9) 0.0054(10) Si4 0.0402(12) 0.0346(12) 0.0317(12) -0.0020(9) -0.0088(10) -0.0009(9) Sn1 0.0342(3) 0.0286(2) 0.0276(3) -0.0053(2) -0.0020(2) -0.0019(2) Sn2 0.0313(3) 0.0349(3) 0.0288(3) -0.0083(2) 0.0033(2) 0.0045(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 1.423(11) . ? C1 C5 1.435(11) . ? C1 C6 1.499(12) . ? C1 Sn1 2.474(7) . ? C2 C3 1.337(11) . ? C2 C7 1.529(12) . ? C2 Sn1 2.565(7) . ? C3 C4 1.367(11) . ? C3 C8 1.561(13) . ? C4 C5 1.410(12) . ? C4 C9 1.516(11) . ? C5 C10 1.505(12) . ? C5 Sn1 2.570(8) . ? C11 C19 1.409(9) . ? C11 C12 1.436(9) . ? C12 C13 1.438(8) . ? C12 Si1 1.841(7) . ? C13 C14 1.408(9) . ? C13 C18 1.432(8) . ? C14 C15 1.358(9) . ? C15 C16 1.404(10) . ? C16 C17 1.368(9) . ? C17 C18 1.410(9) . ? C18 C19 1.441(9) . ? C19 Si2 1.862(7) . ? C20 Si1 1.830(11) . ? C21 Si1 1.858(7) . ? C22 Si1 1.850(8) . ? C23 Si2 1.846(8) . ? C24 Si2 1.850(8) . ? C25 Si2 1.865(8) . ? C26 C27 1.401(10) . ? C26 C30 1.404(11) . ? C26 C31 1.501(11) . ? C26 Sn2 2.617(6) . ? C27 C28 1.403(10) . ? C27 C32 1.516(11) . ? C28 C29 1.440(10) . ? C28 C33 1.495(10) . ? C28 Sn2 2.649(7) . ? C29 C30 1.438(11) . ? C29 C34 1.492(10) . ? C29 Sn2 2.527(7) . ? C30 C35 1.520(11) . ? C30 Sn2 2.520(8) . ? C36 C37 1.415(10) . ? C36 C44 1.434(9) . ? C37 C38 1.460(9) . ? C37 Si4 1.839(7) . ? C38 C39 1.411(9) . ? C38 C43 1.430(9) . ? C39 C40 1.369(10) . ? C40 C41 1.384(10) . ? C41 C42 1.368(10) . ? C42 C43 1.413(9) . ? C43 C44 1.447(9) . ? C44 Si3 1.856(7) . ? C45 Si3 1.862(8) . ? C46 Si3 1.867(8) . ? C47 Si3 1.847(8) . ? C48 Si4 1.860(8) . ? C49 Si4 1.857(8) . ? C50 Si4 1.845(8) . ? 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 C5 106.4(7) . . ? C2 C1 C6 126.9(10) . . ? C5 C1 C6 125.4(10) . . ? C2 C1 Sn1 77.2(4) . . ? C5 C1 Sn1 77.2(4) . . ? C6 C1 Sn1 121.6(6) . . ? C3 C2 C1 108.5(7) . . ? C3 C2 C7 126.1(10) . . ? C1 C2 C7 124.4(10) . . ? C3 C2 Sn1 81.0(5) . . ? C1 C2 Sn1 70.1(4) . . ? C7 C2 Sn1 123.9(6) . . ? C2 C3 C4 110.7(8) . . ? C2 C3 C8 124.6(10) . . ? C4 C3 C8 124.7(10) . . ? C3 C4 C5 108.6(7) . . ? C3 C4 C9 125.3(10) . . ? C5 C4 C9 126.1(10) . . ? C4 C5 C1 105.9(7) . . ? C4 C5 C10 126.9(10) . . ? C1 C5 C10 126.8(10) . . ? C4 C5 Sn1 80.0(5) . . ? C1 C5 Sn1 69.8(4) . . ? C10 C5 Sn1 120.8(5) . . ? C19 C11 C12 113.0(6) . . ? C11 C12 C13 103.8(6) . . ? C11 C12 Si1 127.7(5) . . ? C13 C12 Si1 127.0(5) . . ? C14 C13 C18 118.2(6) . . ? C14 C13 C12 132.3(6) . . ? C18 C13 C12 109.5(6) . . ? C15 C14 C13 120.2(7) . . ? C14 C15 C16 121.2(7) . . ? C17 C16 C15 121.2(6) . . ? C16 C17 C18 118.6(6) . . ? C17 C18 C13 120.6(6) . . ? C17 C18 C19 130.7(6) . . ? C13 C18 C19 108.6(5) . . ? C11 C19 C18 104.9(5) . . ? C11 C19 Si2 126.8(5) . . ? C18 C19 Si2 127.1(5) . . ? C27 C26 C30 107.8(7) . . ? C27 C26 C31 125.8(9) . . ? C30 C26 C31 126.2(8) . . ? C27 C26 Sn2 77.7(4) . . ? C30 C26 Sn2 70.4(4) . . ? C31 C26 Sn2 121.7(5) . . ? C26 C27 C28 110.0(7) . . ? C26 C27 C32 126.8(8) . . ? C28 C27 C32 123.2(8) . . ? C27 C28 C29 107.0(7) . . ? C27 C28 C33 126.5(7) . . ? C29 C28 C33 126.4(7) . . ? C27 C28 Sn2 76.5(4) . . ? C29 C28 Sn2 69.2(4) . . ? C33 C28 Sn2 121.6(5) . . ? C30 C29 C28 106.8(6) . . ? C30 C29 C34 125.6(8) . . ? C28 C29 C34 126.7(8) . . ? C30 C29 Sn2 73.2(4) . . ? C28 C29 Sn2 78.6(4) . . ? C34 C29 Sn2 122.4(5) . . ? C26 C30 C29 108.3(7) . . ? C26 C30 C35 127.1(8) . . ? C29 C30 C35 124.3(8) . . ? C26 C30 Sn2 78.0(4) . . ? C29 C30 Sn2 73.7(4) . . ? C35 C30 Sn2 119.7(5) . . ? C37 C36 C44 114.0(6) . . ? C36 C37 C38 103.7(6) . . ? C36 C37 Si4 128.7(5) . . ? C38 C37 Si4 126.5(5) . . ? C39 C38 C43 119.2(6) . . ? C39 C38 C37 131.6(6) . . ? C43 C38 C37 109.2(6) . . ? C40 C39 C38 119.0(7) . . ? C39 C40 C41 122.1(7) . . ? C42 C41 C40 120.8(7) . . ? C41 C42 C43 119.5(7) . . ? C42 C43 C38 119.4(6) . . ? C42 C43 C44 131.3(6) . . ? C38 C43 C44 109.3(6) . . ? C36 C44 C43 103.8(6) . . ? C36 C44 Si3 128.8(5) . . ? C43 C44 Si3 126.8(5) . . ? C20 Si1 C12 110.9(4) . . ? C20 Si1 C22 108.0(5) . . ? C12 Si1 C22 109.3(3) . . ? C20 Si1 C21 109.0(5) . . ? C12 Si1 C21 110.8(3) . . ? C22 Si1 C21 108.6(4) . . ? C23 Si2 C24 108.9(4) . . ? C23 Si2 C19 108.3(3) . . ? C24 Si2 C19 109.4(3) . . ? C23 Si2 C25 109.8(4) . . ? C24 Si2 C25 108.3(4) . . ? C19 Si2 C25 112.0(3) . . ? C47 Si3 C44 110.1(3) . . ? C47 Si3 C45 107.5(4) . . ? C44 Si3 C45 110.5(3) . . ? C47 Si3 C46 108.2(4) . . ? C44 Si3 C46 111.7(3) . . ? C45 Si3 C46 108.8(4) . . ? C37 Si4 C50 110.3(4) . . ? C37 Si4 C49 111.5(3) . . ? C50 Si4 C49 107.7(4) . . ? C37 Si4 C48 110.8(3) . . ? C50 Si4 C48 107.4(4) . . ? C49 Si4 C48 109.1(4) . . ? C1 Sn1 C2 32.7(3) . . ? C1 Sn1 C5 33.0(3) . . ? C2 Sn1 C5 52.9(3) . . ? C30 Sn2 C29 33.1(2) . . ? C30 Sn2 C26 31.7(2) . . ? C29 Sn2 C26 53.2(3) . . ? C30 Sn2 C28 53.0(2) . . ? C29 Sn2 C28 32.2(2) . . ? C26 Sn2 C28 51.7(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.23 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.941 _refine_diff_density_min -1.588 _refine_diff_density_rms 0.139 data_p1bar _database_code_depnum_ccdc_archive 'CCDC 244712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H92 Si8 Sn2' _chemical_formula_weight 1275.44 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.440(5) _cell_length_b 17.300(5) _cell_length_c 18.587(5) _cell_angle_alpha 103.452(5) _cell_angle_beta 105.369(5) _cell_angle_gamma 91.091(5) _cell_volume 3437(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.43 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24136 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.43 _reflns_number_total 15537 _reflns_number_gt 11841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0243P)^2^+4.5461P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00152(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15537 _refine_ls_number_parameters 934 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.290 _refine_ls_shift/su_mean 0.006 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 0.0560(3) 0.4588(2) 0.6688(2) 0.0336(8) Uani 1 1 d . . . C2 C 0.1396(3) 0.5234(2) 0.6722(2) 0.0325(8) Uani 1 1 d . . . C3 C 0.1729(3) 0.57971(19) 0.74412(19) 0.0282(7) Uani 1 1 d . . . C4 C 0.1017(3) 0.55216(19) 0.78886(19) 0.0282(7) Uani 1 1 d . . . C5 C 0.0964(3) 0.5821(2) 0.8651(2) 0.0365(8) Uani 1 1 d . . . C6 C 0.0218(4) 0.5420(2) 0.8937(3) 0.0429(9) Uani 1 1 d . . . C7 C -0.0491(4) 0.4720(2) 0.8484(3) 0.0427(10) Uani 1 1 d . . . C8 C -0.0473(3) 0.4407(2) 0.7745(2) 0.0361(8) Uani 1 1 d . . . C9 C 0.0291(3) 0.47949(19) 0.7426(2) 0.0300(7) Uani 1 1 d . . . C10 C -0.1899(4) 0.4185(4) 0.5529(3) 0.0598(13) Uani 1 1 d . . . C11 C 0.0366(5) 0.3849(3) 0.5000(3) 0.0545(11) Uani 1 1 d . . . C12 C -0.0420(6) 0.2821(3) 0.5939(3) 0.0618(14) Uani 1 1 d . . . C13 C 0.3621(4) 0.6629(3) 0.6947(3) 0.0475(10) Uani 1 1 d . . . C14 C 0.4042(4) 0.6613(3) 0.8640(2) 0.0531(11) Uani 1 1 d . . . H14A H 0.4606 0.7096 0.8825 0.080 Uiso 1 1 calc R . . H14B H 0.4496 0.6144 0.8536 0.080 Uiso 1 1 calc R . . H14C H 0.3634 0.6571 0.9032 0.080 Uiso 1 1 calc R . . C15 C 0.2154(4) 0.7618(3) 0.7903(3) 0.0523(11) Uani 1 1 d . . . C16 C 0.3429(3) 0.30898(18) 0.81819(19) 0.0277(7) Uani 1 1 d . . . C17 C 0.3334(3) 0.2942(2) 0.7382(2) 0.0304(7) Uani 1 1 d . . . C18 C 0.4216(3) 0.34317(19) 0.7229(2) 0.0304(7) Uani 1 1 d . . . C19 C 0.4952(3) 0.38677(18) 0.79798(19) 0.0260(7) Uani 1 1 d . . . C20 C 0.5996(3) 0.4415(2) 0.8212(2) 0.0345(8) Uani 1 1 d . . . C21 C 0.6554(3) 0.4715(2) 0.8975(2) 0.0389(9) Uani 1 1 d . . . C22 C 0.6113(3) 0.4497(2) 0.9538(2) 0.0393(9) Uani 1 1 d . . . C23 C 0.5085(3) 0.3978(2) 0.9339(2) 0.0329(8) Uani 1 1 d . . . C24 C 0.4478(3) 0.36550(18) 0.85553(19) 0.0272(7) Uani 1 1 d . . . C25 C 0.2409(6) 0.3098(5) 0.9562(3) 0.079(2) Uani 1 1 d . . . C26 C 0.0899(4) 0.2352(3) 0.7937(3) 0.0447(10) Uani 1 1 d . . . C27 C 0.3107(4) 0.1570(3) 0.8660(4) 0.0862(19) Uani 1 1 d . . . H27A H 0.3921 0.1668 0.9024 0.129 Uiso 1 1 calc R . . H27B H 0.3163 0.1282 0.8151 0.129 Uiso 1 1 calc R . . H27C H 0.2579 0.1249 0.8837 0.129 Uiso 1 1 calc R . . C28 C 0.3332(4) 0.2633(3) 0.5539(3) 0.0520(11) Uani 1 1 d . . . C29 C 0.6057(4) 0.2948(4) 0.6340(3) 0.0547(12) Uani 1 1 d . . . C30 C 0.4545(7) 0.4321(4) 0.6031(4) 0.0698(16) Uani 1 1 d . . . C31 C 0.6751(3) -0.20363(18) 0.76226(19) 0.0266(7) Uani 1 1 d . . . C32 C 0.6276(3) -0.17797(19) 0.69446(19) 0.0264(7) Uani 1 1 d . . . C33 C 0.5455(3) -0.11716(19) 0.70457(19) 0.0287(7) Uani 1 1 d . . . C34 C 0.5371(3) -0.10821(19) 0.78244(18) 0.0260(7) Uani 1 1 d . . . C35 C 0.4689(3) -0.0591(2) 0.8254(2) 0.0341(8) Uani 1 1 d . . . C36 C 0.4805(3) -0.0617(2) 0.8993(2) 0.0385(9) Uani 1 1 d . . . C37 C 0.5577(3) -0.1123(2) 0.9341(2) 0.0388(9) Uani 1 1 d . . . C38 C 0.6254(3) -0.1613(2) 0.8944(2) 0.0325(8) Uani 1 1 d . . . C39 C 0.6166(3) -0.16051(17) 0.81744(18) 0.0250(7) Uani 1 1 d . . . C40 C 0.7183(5) -0.3684(3) 0.7925(4) 0.0582(13) Uani 1 1 d . . . C41 C 0.8433(4) -0.3083(3) 0.6886(3) 0.0590(12) Uani 1 1 d . . . H41A H 0.9057 -0.3459 0.6966 0.089 Uiso 1 1 calc R . . H41B H 0.8782 -0.2608 0.6790 0.089 Uiso 1 1 calc R . . H41C H 0.7751 -0.3338 0.6443 0.089 Uiso 1 1 calc R . . C42 C 0.9186(4) -0.2336(3) 0.8623(3) 0.0476(10) Uani 1 1 d . . . C43 C 0.2848(4) -0.1301(3) 0.6127(4) 0.0576(13) Uani 1 1 d . . . C44 C 0.4873(5) -0.1168(3) 0.5368(2) 0.0660(14) Uani 1 1 d . . . H44A H 0.5722 -0.0969 0.5464 0.099 Uiso 1 1 calc R . . H44B H 0.4356 -0.0962 0.4955 0.099 Uiso 1 1 calc R . . H44C H 0.4799 -0.1752 0.5215 0.099 Uiso 1 1 calc R . . C45 C 0.4365(4) 0.0277(3) 0.6487(3) 0.0474(10) Uani 1 1 d . . . C46 C 0.9066(3) 0.02768(18) 0.73059(18) 0.0253(7) Uani 1 1 d . . . C47 C 0.8277(3) 0.08519(18) 0.75398(19) 0.0257(7) Uani 1 1 d . . . C48 C 0.8504(3) 0.10961(17) 0.83478(18) 0.0237(6) Uani 1 1 d . . . C49 C 0.9556(3) 0.07007(17) 0.86491(17) 0.0217(6) Uani 1 1 d . . . C50 C 1.0232(3) 0.0723(2) 0.9410(2) 0.0293(7) Uani 1 1 d . . . C51 C 1.1193(3) 0.0268(2) 0.9534(2) 0.0338(8) Uani 1 1 d . . . C52 C 1.1519(3) -0.0231(2) 0.8918(2) 0.0321(8) Uani 1 1 d . . . C53 C 1.0893(3) -0.0274(2) 0.8174(2) 0.0285(7) Uani 1 1 d . . . C54 C 0.9896(3) 0.02019(18) 0.80197(17) 0.0233(6) Uani 1 1 d . . . C55 C 1.0676(5) 0.0389(3) 0.6267(3) 0.0557(12) Uani 1 1 d . . . C56 C 0.9222(4) -0.1176(3) 0.6023(2) 0.0557(11) Uani 1 1 d . . . H56A H 0.9893 -0.1352 0.6383 0.084 Uiso 1 1 calc R . . H56B H 0.9322 -0.1336 0.5502 0.084 Uiso 1 1 calc R . . H56C H 0.8448 -0.1423 0.6028 0.084 Uiso 1 1 calc R . . C57 C 0.7935(4) 0.0281(4) 0.5657(2) 0.0727(16) Uani 1 1 d . . . H57A H 0.7164 0.0071 0.5704 0.109 Uiso 1 1 calc R . . H57B H 0.7973 0.0091 0.5125 0.109 Uiso 1 1 calc R . . H57C H 0.7988 0.0865 0.5796 0.109 Uiso 1 1 calc R . . C58 C 0.8630(5) 0.2800(3) 0.9301(3) 0.0576(13) Uani 1 1 d . . . C59 C 0.7268(6) 0.1495(3) 0.9656(3) 0.0588(13) Uani 1 1 d . . . C60 C 0.6257(6) 0.1982(4) 0.8167(3) 0.0746(18) Uani 1 1 d . . . Si1 Si -0.03383(10) 0.38579(6) 0.57973(6) 0.0407(2) Uani 1 1 d . . . Si2 Si 0.28828(8) 0.66667(5) 0.77365(6) 0.0320(2) Uani 1 1 d . . . Si3 Si 0.24585(9) 0.25419(6) 0.85968(6) 0.0355(2) Uani 1 1 d . . . Si4 Si 0.45358(10) 0.33420(6) 0.62839(6) 0.0387(2) Uani 1 1 d . . . Si5 Si 0.78855(8) -0.27884(5) 0.77591(6) 0.0309(2) Uani 1 1 d . . . Si6 Si 0.43856(9) -0.08264(6) 0.62611(6) 0.0347(2) Uani 1 1 d . . . Si7 Si 0.92293(9) -0.00721(6) 0.63163(5) 0.0358(2) Uani 1 1 d . . . Si8 Si 0.76644(9) 0.18443(5) 0.88686(5) 0.0299(2) Uani 1 1 d . . . Sn1 Sn 0.26205(2) 0.436111(13) 0.763359(13) 0.02814(7) Uani 1 1 d . . . Sn2 Sn 0.759984(19) -0.046641(12) 0.783568(13) 0.02424(7) Uani 1 1 d . . . H2 H 0.172(3) 0.522(2) 0.633(2) 0.041(11) Uiso 1 1 d . . . H5 H 0.138(4) 0.627(2) 0.895(2) 0.044(11) Uiso 1 1 d . . . H6 H 0.026(3) 0.561(2) 0.944(2) 0.036(10) Uiso 1 1 d . . . H7 H -0.093(3) 0.446(2) 0.868(2) 0.038(10) Uiso 1 1 d . . . H8 H -0.093(3) 0.398(2) 0.745(2) 0.033(10) Uiso 1 1 d . . . H10A H -0.239(5) 0.381(3) 0.513(3) 0.081(17) Uiso 1 1 d . . . H10B H -0.234(4) 0.419(3) 0.587(3) 0.064(15) Uiso 1 1 d . . . H11A H 0.002(5) 0.349(3) 0.459(3) 0.073(16) Uiso 1 1 d . . . H12A H 0.043(5) 0.259(3) 0.608(3) 0.091(19) Uiso 1 1 d . . . H12B H -0.089(5) 0.250(3) 0.549(3) 0.083(17) Uiso 1 1 d . . . H13A H 0.296(4) 0.664(2) 0.651(3) 0.053(12) Uiso 1 1 d . . . H13B H 0.418(5) 0.707(3) 0.706(3) 0.079(16) Uiso 1 1 d . . . H13C H 0.391(4) 0.615(3) 0.683(3) 0.072(16) Uiso 1 1 d . . . H15A H 0.156(4) 0.765(2) 0.742(2) 0.048(12) Uiso 1 1 d . . . H15B H 0.181(4) 0.770(3) 0.830(3) 0.069(15) Uiso 1 1 d . . . H15C H 0.277(4) 0.805(3) 0.800(3) 0.069(14) Uiso 1 1 d . . . H17 H 0.275(3) 0.254(2) 0.697(2) 0.035(9) Uiso 1 1 d . . . H20 H 0.627(3) 0.457(2) 0.784(2) 0.040(10) Uiso 1 1 d . . . H21 H 0.727(3) 0.508(2) 0.9129(19) 0.033(9) Uiso 1 1 d . . . H22 H 0.649(3) 0.466(2) 1.002(2) 0.040(11) Uiso 1 1 d . . . H23 H 0.478(3) 0.385(2) 0.971(2) 0.037(10) Uiso 1 1 d . . . H24B H 0.886(5) -0.217(3) 0.910(3) 0.079(16) Uiso 1 1 d . . . H25A H 0.187(6) 0.287(4) 0.975(3) 0.10(2) Uiso 1 1 d . . . H25B H 0.213(3) 0.357(2) 0.952(2) 0.017(10) Uiso 1 1 d . . . H26A H 0.048(4) 0.284(3) 0.791(3) 0.076(15) Uiso 1 1 d . . . H26B H 0.088(5) 0.212(3) 0.745(3) 0.080(18) Uiso 1 1 d . . . H28A H 0.249(4) 0.274(2) 0.552(2) 0.057(12) Uiso 1 1 d . . . H28B H 0.339(4) 0.261(3) 0.500(3) 0.079(16) Uiso 1 1 d . . . H29A H 0.606(4) 0.248(3) 0.647(3) 0.058(15) Uiso 1 1 d . . . H29B H 0.628(5) 0.294(3) 0.588(3) 0.081(16) Uiso 1 1 d . . . H30A H 0.472(4) 0.426(3) 0.556(3) 0.078(16) Uiso 1 1 d . . . H32 H 0.651(3) -0.1967(19) 0.6476(19) 0.026(8) Uiso 1 1 d . . . H35 H 0.423(3) -0.028(2) 0.804(2) 0.032(10) Uiso 1 1 d . . . H36 H 0.437(4) -0.028(2) 0.924(2) 0.048(11) Uiso 1 1 d . . . H37 H 0.567(3) -0.114(2) 0.986(2) 0.042(10) Uiso 1 1 d . . . H38 H 0.682(3) -0.193(2) 0.921(2) 0.035(10) Uiso 1 1 d . . . H40A H 0.646(5) -0.394(3) 0.747(3) 0.066(14) Uiso 1 1 d . . . H40B H 0.771(5) -0.406(3) 0.793(3) 0.070(15) Uiso 1 1 d . . . H42A H 0.963(5) -0.189(3) 0.856(3) 0.080(16) Uiso 1 1 d . . . H43A H 0.229(5) -0.115(3) 0.575(3) 0.070(14) Uiso 1 1 d . . . H43B H 0.289(4) -0.186(3) 0.598(3) 0.062(14) Uiso 1 1 d . . . H45A H 0.413(4) 0.047(3) 0.694(3) 0.064(14) Uiso 1 1 d . . . H47 H 0.765(3) 0.1049(19) 0.7223(19) 0.024(8) Uiso 1 1 d . . . H50 H 1.003(3) 0.1027(19) 0.981(2) 0.024(9) Uiso 1 1 d . . . H51 H 1.159(3) 0.029(2) 0.999(2) 0.034(10) Uiso 1 1 d . . . H52 H 1.218(3) -0.055(2) 0.9012(19) 0.030(9) Uiso 1 1 d . . . H53 H 1.105(3) -0.0620(19) 0.7766(18) 0.018(8) Uiso 1 1 d . . . H55A H 1.141(4) 0.028(3) 0.666(3) 0.058(13) Uiso 1 1 d . . . H58A H 0.885(4) 0.296(3) 0.893(3) 0.065(15) Uiso 1 1 d . . . H58B H 0.937(5) 0.270(3) 0.968(3) 0.081(18) Uiso 1 1 d . . . H59A H 0.677(4) 0.186(3) 0.989(2) 0.057(12) Uiso 1 1 d . . . H59B H 0.680(5) 0.107(3) 0.946(3) 0.071(18) Uiso 1 1 d . . . H59C H 0.799(6) 0.145(4) 1.008(4) 0.12(2) Uiso 1 1 d . . . H60A H 0.651(5) 0.224(3) 0.777(3) 0.081(17) Uiso 1 1 d . . . H60B H 0.582(4) 0.231(3) 0.836(3) 0.056(13) Uiso 1 1 d . . . H55C H 1.063(5) 0.097(3) 0.634(3) 0.086(17) Uiso 1 1 d . . . H26C H 0.034(4) 0.205(3) 0.813(3) 0.066(13) Uiso 1 1 d . . . H25C H 0.328(6) 0.317(4) 1.001(4) 0.11(2) Uiso 1 1 d . . . H30B H 0.376(5) 0.453(3) 0.599(3) 0.086(19) Uiso 1 1 d . . . H10C H -0.189(5) 0.470(3) 0.542(3) 0.081(17) Uiso 1 1 d . . . H55B H 1.083(4) 0.021(3) 0.585(3) 0.059(13) Uiso 1 1 d . . . H29C H 0.660(5) 0.333(3) 0.676(3) 0.084(17) Uiso 1 1 d . . . H28C H 0.332(4) 0.211(3) 0.566(3) 0.078(17) Uiso 1 1 d . . . H45B H 0.519(5) 0.053(3) 0.658(3) 0.073(15) Uiso 1 1 d . . . H42C H 0.976(5) -0.268(3) 0.872(3) 0.076(15) Uiso 1 1 d . . . H58C H 0.810(5) 0.317(4) 0.952(3) 0.100(19) Uiso 1 1 d . . . H12C H -0.081(5) 0.280(3) 0.631(3) 0.078(17) Uiso 1 1 d . . . H11C H 0.117(5) 0.376(3) 0.514(3) 0.071(16) Uiso 1 1 d . . . H11B H 0.032(5) 0.435(3) 0.484(3) 0.087(17) Uiso 1 1 d . . . H45C H 0.384(5) 0.043(3) 0.615(3) 0.083(18) Uiso 1 1 d . . . H40C H 0.693(5) -0.352(3) 0.834(3) 0.076(18) Uiso 1 1 d . . . H43C H 0.255(5) -0.118(3) 0.657(3) 0.080(18) Uiso 1 1 d . . . H60C H 0.579(6) 0.156(4) 0.787(4) 0.12(3) Uiso 1 1 d . . . H31C H 0.514(6) 0.467(4) 0.638(4) 0.11(3) Uiso 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 0.0329(18) 0.0287(18) 0.038(2) 0.0114(15) 0.0056(16) -0.0018(14) C2 0.0303(18) 0.0317(19) 0.037(2) 0.0156(16) 0.0054(16) 0.0002(14) C3 0.0242(16) 0.0263(17) 0.0354(19) 0.0137(15) 0.0052(14) 0.0025(12) C4 0.0230(16) 0.0247(17) 0.0361(19) 0.0080(14) 0.0062(14) 0.0071(12) C5 0.0349(19) 0.028(2) 0.048(2) 0.0073(17) 0.0146(17) 0.0050(15) C6 0.049(2) 0.039(2) 0.049(3) 0.0096(19) 0.028(2) 0.0102(17) C7 0.040(2) 0.035(2) 0.068(3) 0.020(2) 0.032(2) 0.0093(16) C8 0.0271(18) 0.0265(19) 0.056(3) 0.0120(18) 0.0130(17) 0.0038(14) C9 0.0231(16) 0.0239(17) 0.042(2) 0.0087(15) 0.0073(15) 0.0039(12) C10 0.043(3) 0.075(4) 0.054(3) 0.021(3) 0.000(2) -0.015(2) C11 0.066(3) 0.054(3) 0.037(3) 0.008(2) 0.008(2) 0.002(2) C12 0.089(4) 0.038(3) 0.044(3) 0.005(2) -0.002(3) -0.020(2) C13 0.047(3) 0.040(3) 0.054(3) 0.006(2) 0.017(2) -0.013(2) C14 0.047(2) 0.052(3) 0.050(3) 0.010(2) 0.000(2) -0.0156(19) C15 0.047(3) 0.033(2) 0.077(4) 0.010(2) 0.021(3) 0.0012(18) C16 0.0261(16) 0.0239(17) 0.0348(19) 0.0108(14) 0.0083(14) 0.0036(12) C17 0.0301(18) 0.0255(18) 0.035(2) 0.0049(15) 0.0111(15) 0.0019(13) C18 0.0313(17) 0.0267(17) 0.0353(19) 0.0051(14) 0.0151(15) 0.0027(13) C19 0.0258(16) 0.0217(16) 0.0320(18) 0.0041(13) 0.0123(14) 0.0048(12) C20 0.0306(18) 0.0301(19) 0.046(2) 0.0065(17) 0.0178(17) -0.0004(14) C21 0.0271(18) 0.033(2) 0.051(2) -0.0033(17) 0.0137(17) -0.0036(14) C22 0.0311(19) 0.040(2) 0.037(2) -0.0027(18) 0.0044(17) 0.0023(15) C23 0.0302(18) 0.037(2) 0.0325(19) 0.0082(16) 0.0112(16) 0.0054(14) C24 0.0261(16) 0.0223(16) 0.0362(19) 0.0093(14) 0.0114(14) 0.0073(12) C25 0.084(4) 0.105(5) 0.049(3) 0.009(3) 0.030(3) -0.039(4) C26 0.036(2) 0.048(3) 0.053(3) 0.019(2) 0.013(2) -0.0054(18) C27 0.056(3) 0.079(4) 0.156(6) 0.090(4) 0.029(3) 0.014(3) C28 0.043(2) 0.068(3) 0.040(3) 0.000(2) 0.013(2) 0.009(2) C29 0.044(3) 0.069(4) 0.049(3) -0.002(3) 0.024(2) -0.003(2) C30 0.103(5) 0.066(4) 0.060(3) 0.027(3) 0.047(4) 0.009(3) C31 0.0225(15) 0.0234(16) 0.0313(18) 0.0052(14) 0.0046(14) -0.0021(12) C32 0.0235(16) 0.0256(17) 0.0264(18) 0.0022(14) 0.0043(14) 0.0021(12) C33 0.0249(16) 0.0276(17) 0.0289(18) 0.0044(14) 0.0017(14) 0.0047(12) C34 0.0158(14) 0.0301(17) 0.0292(17) 0.0044(14) 0.0039(13) 0.0016(12) C35 0.0226(17) 0.036(2) 0.037(2) 0.0019(16) 0.0029(15) 0.0029(14) C36 0.0253(18) 0.046(2) 0.037(2) -0.0051(17) 0.0099(16) -0.0019(15) C37 0.036(2) 0.050(2) 0.030(2) 0.0045(17) 0.0122(16) -0.0068(16) C38 0.0326(18) 0.0341(19) 0.0319(19) 0.0111(16) 0.0087(15) -0.0029(14) C39 0.0220(15) 0.0196(16) 0.0323(18) 0.0057(13) 0.0069(13) -0.0031(11) C40 0.045(3) 0.035(2) 0.094(4) 0.025(3) 0.011(3) 0.008(2) C41 0.065(3) 0.063(3) 0.056(3) 0.015(2) 0.025(2) 0.033(2) C42 0.032(2) 0.044(2) 0.060(3) 0.012(2) 0.002(2) 0.0073(18) C43 0.035(2) 0.055(3) 0.072(4) 0.024(3) -0.012(2) 0.0023(19) C44 0.073(3) 0.085(4) 0.033(2) 0.009(2) 0.006(2) 0.039(3) C45 0.048(3) 0.041(2) 0.047(3) 0.012(2) 0.002(2) 0.0104(19) C46 0.0262(16) 0.0259(17) 0.0241(16) 0.0056(13) 0.0078(13) 0.0034(12) C47 0.0256(16) 0.0246(17) 0.0311(18) 0.0137(14) 0.0090(14) 0.0052(12) C48 0.0270(16) 0.0200(16) 0.0272(17) 0.0082(13) 0.0109(13) 0.0036(12) C49 0.0242(15) 0.0176(15) 0.0249(16) 0.0059(12) 0.0092(13) -0.0006(11) C50 0.0299(17) 0.0316(19) 0.0245(18) 0.0050(15) 0.0065(14) -0.0015(13) C51 0.0242(17) 0.047(2) 0.029(2) 0.0174(17) -0.0021(15) -0.0042(14) C52 0.0203(16) 0.039(2) 0.042(2) 0.0209(17) 0.0062(15) 0.0063(14) C53 0.0226(16) 0.0248(17) 0.041(2) 0.0068(15) 0.0139(15) 0.0055(12) C54 0.0220(15) 0.0236(16) 0.0263(17) 0.0082(13) 0.0086(13) 0.0005(12) C55 0.066(3) 0.059(3) 0.053(3) 0.007(2) 0.042(3) 0.003(2) C56 0.060(3) 0.056(3) 0.045(2) -0.010(2) 0.024(2) -0.004(2) C57 0.065(3) 0.131(5) 0.031(2) 0.032(3) 0.015(2) 0.034(3) C58 0.073(3) 0.031(2) 0.071(3) -0.003(2) 0.038(3) 0.002(2) C59 0.078(4) 0.054(3) 0.069(3) 0.023(3) 0.054(3) 0.022(3) C60 0.068(4) 0.084(4) 0.060(3) 0.002(3) 0.008(3) 0.057(3) Si1 0.0426(6) 0.0374(6) 0.0352(6) 0.0106(5) -0.0013(5) -0.0100(4) Si2 0.0288(5) 0.0252(5) 0.0406(6) 0.0081(4) 0.0076(4) -0.0029(4) Si3 0.0328(5) 0.0384(6) 0.0395(6) 0.0186(5) 0.0099(4) -0.0050(4) Si4 0.0452(6) 0.0392(6) 0.0343(6) 0.0037(4) 0.0202(5) 0.0004(4) Si5 0.0303(5) 0.0241(5) 0.0370(5) 0.0072(4) 0.0074(4) 0.0061(4) Si6 0.0308(5) 0.0372(6) 0.0288(5) 0.0049(4) -0.0015(4) 0.0101(4) Si7 0.0344(5) 0.0502(6) 0.0242(5) 0.0066(4) 0.0126(4) 0.0062(4) Si8 0.0355(5) 0.0239(5) 0.0340(5) 0.0071(4) 0.0151(4) 0.0107(4) Sn1 0.02765(12) 0.02564(13) 0.03276(14) 0.00900(10) 0.00936(10) 0.00499(9) Sn2 0.02229(11) 0.02333(12) 0.02694(13) 0.00650(9) 0.00632(9) 0.00121(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.436(5) . ? C1 C9 1.451(5) . ? C1 Si1 1.862(4) . ? C1 Sn1 2.639(4) . ? C2 C3 1.411(5) . ? C3 C4 1.453(4) . ? C3 Si2 1.861(3) . ? C4 C5 1.410(5) . ? C4 C9 1.446(5) . ? C5 C6 1.372(5) . ? C6 C7 1.400(6) . ? C7 C8 1.359(6) . ? C8 C9 1.416(5) . ? C10 Si1 1.859(5) . ? C11 Si1 1.863(5) . ? C12 Si1 1.877(5) . ? C13 Si2 1.867(4) . ? C14 Si2 1.866(4) . ? C15 Si2 1.857(4) . ? C16 C17 1.422(5) . ? C16 C24 1.441(4) . ? C16 Si3 1.865(3) . ? C17 C18 1.431(4) . ? C17 Sn1 2.580(3) . ? C18 C19 1.445(5) . ? C18 Si4 1.861(3) . ? C18 Sn1 2.600(3) . ? C19 C20 1.415(4) . ? C19 C24 1.434(4) . ? C20 C21 1.361(5) . ? C21 C22 1.396(5) . ? C22 C23 1.379(5) . ? C23 C24 1.410(5) . ? C25 Si3 1.844(6) . ? C26 Si3 1.851(4) . ? C27 Si3 1.867(5) . ? C28 Si4 1.858(5) . ? C29 Si4 1.868(5) . ? C30 Si4 1.860(5) . ? C31 C32 1.410(4) . ? C31 C39 1.443(4) . ? C31 Si5 1.867(3) . ? C32 C33 1.437(4) . ? C32 Sn2 2.643(3) . ? C33 C34 1.448(5) . ? C33 Si6 1.862(3) . ? C33 Sn2 2.610(3) . ? C34 C35 1.416(5) . ? C34 C39 1.435(4) . ? C35 C36 1.356(5) . ? C36 C37 1.399(5) . ? C37 C38 1.379(5) . ? C38 C39 1.409(5) . ? C40 Si5 1.857(5) . ? C41 Si5 1.858(4) . ? C42 Si5 1.873(4) . ? C43 Si6 1.857(5) . ? C44 Si6 1.861(4) . ? C45 Si6 1.859(4) . ? C46 C47 1.426(4) . ? C46 C54 1.447(4) . ? C46 Si7 1.858(3) . ? C46 Sn2 2.612(3) . ? C47 C48 1.413(4) . ? C47 Sn2 2.617(3) . ? C48 C49 1.443(4) . ? C48 Si8 1.869(3) . ? C49 C50 1.411(4) . ? C49 C54 1.431(4) . ? C50 C51 1.366(5) . ? C51 C52 1.404(5) . ? C52 C53 1.362(5) . ? C53 C54 1.426(4) . ? C55 Si7 1.856(5) . ? C56 Si7 1.860(4) . ? C57 Si7 1.868(4) . ? C58 Si8 1.855(5) . ? C59 Si8 1.862(5) . ? C60 Si8 1.843(5) . ? 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 C9 104.3(3) . . ? C2 C1 Si1 125.9(3) . . ? C9 C1 Si1 127.0(2) . . ? C2 C1 Sn1 75.5(2) . . ? C9 C1 Sn1 78.04(19) . . ? Si1 C1 Sn1 126.28(17) . . ? C3 C2 C1 113.4(3) . . ? C2 C3 C4 104.7(3) . . ? C2 C3 Si2 126.2(2) . . ? C4 C3 Si2 129.0(3) . . ? C5 C4 C9 119.3(3) . . ? C5 C4 C3 131.8(3) . . ? C9 C4 C3 108.9(3) . . ? C6 C5 C4 119.4(4) . . ? C5 C6 C7 121.0(4) . . ? C8 C7 C6 122.0(4) . . ? C7 C8 C9 119.2(4) . . ? C8 C9 C4 119.2(3) . . ? C8 C9 C1 132.1(3) . . ? C4 C9 C1 108.6(3) . . ? C17 C16 C24 105.0(3) . . ? C17 C16 Si3 124.1(2) . . ? C24 C16 Si3 130.5(3) . . ? C16 C17 C18 112.2(3) . . ? C16 C17 Sn1 79.60(19) . . ? C18 C17 Sn1 74.73(19) . . ? C17 C18 C19 104.8(3) . . ? C17 C18 Si4 126.1(3) . . ? C19 C18 Si4 127.8(2) . . ? C17 C18 Sn1 73.18(18) . . ? C19 C18 Sn1 81.14(18) . . ? Si4 C18 Sn1 121.03(16) . . ? C20 C19 C24 119.3(3) . . ? C20 C19 C18 132.0(3) . . ? C24 C19 C18 108.7(3) . . ? C21 C20 C19 119.8(3) . . ? C20 C21 C22 121.3(3) . . ? C23 C22 C21 121.0(4) . . ? C22 C23 C24 119.5(3) . . ? C23 C24 C19 119.2(3) . . ? C23 C24 C16 131.7(3) . . ? C19 C24 C16 109.0(3) . . ? C32 C31 C39 105.6(3) . . ? C32 C31 Si5 126.5(2) . . ? C39 C31 Si5 127.9(2) . . ? C31 C32 C33 112.1(3) . . ? C31 C32 Sn2 79.93(18) . . ? C33 C32 Sn2 72.83(18) . . ? C32 C33 C34 104.9(3) . . ? C32 C33 Si6 125.9(2) . . ? C34 C33 Si6 126.7(2) . . ? C32 C33 Sn2 75.43(18) . . ? C34 C33 Sn2 79.23(18) . . ? Si6 C33 Sn2 124.89(16) . . ? C35 C34 C39 119.6(3) . . ? C35 C34 C33 131.9(3) . . ? C39 C34 C33 108.5(3) . . ? C36 C35 C34 119.5(4) . . ? C35 C36 C37 121.5(4) . . ? C38 C37 C36 120.9(3) . . ? C37 C38 C39 119.6(3) . . ? C38 C39 C34 118.9(3) . . ? C38 C39 C31 132.3(3) . . ? C34 C39 C31 108.9(3) . . ? C47 C46 C54 104.4(3) . . ? C47 C46 Si7 126.0(2) . . ? C54 C46 Si7 127.7(2) . . ? C47 C46 Sn2 74.36(17) . . ? C54 C46 Sn2 79.80(17) . . ? Si7 C46 Sn2 122.98(15) . . ? C48 C47 C46 112.8(3) . . ? C48 C47 Sn2 79.21(17) . . ? C46 C47 Sn2 73.97(17) . . ? C47 C48 C49 104.9(3) . . ? C47 C48 Si8 125.2(2) . . ? C49 C48 Si8 129.7(2) . . ? C50 C49 C54 119.3(3) . . ? C50 C49 C48 131.8(3) . . ? C54 C49 C48 108.9(3) . . ? C51 C50 C49 119.6(3) . . ? C50 C51 C52 121.3(3) . . ? C53 C52 C51 121.2(3) . . ? C52 C53 C54 119.3(3) . . ? C53 C54 C49 119.3(3) . . ? C53 C54 C46 131.9(3) . . ? C49 C54 C46 108.8(3) . . ? C10 Si1 C1 107.9(2) . . ? C10 Si1 C11 108.8(3) . . ? C1 Si1 C11 109.7(2) . . ? C10 Si1 C12 109.6(3) . . ? C1 Si1 C12 112.0(2) . . ? C11 Si1 C12 108.7(3) . . ? C15 Si2 C3 110.70(18) . . ? C15 Si2 C14 109.5(2) . . ? C3 Si2 C14 109.18(16) . . ? C15 Si2 C13 108.9(2) . . ? C3 Si2 C13 108.47(18) . . ? C14 Si2 C13 110.2(2) . . ? C25 Si3 C26 109.5(3) . . ? C25 Si3 C16 112.5(2) . . ? C26 Si3 C16 108.58(17) . . ? C25 Si3 C27 109.4(3) . . ? C26 Si3 C27 109.3(2) . . ? C16 Si3 C27 107.52(19) . . ? C28 Si4 C18 107.97(19) . . ? C28 Si4 C30 109.5(3) . . ? C18 Si4 C30 111.7(2) . . ? C28 Si4 C29 110.1(2) . . ? C18 Si4 C29 108.4(2) . . ? C30 Si4 C29 109.2(3) . . ? C41 Si5 C40 109.4(3) . . ? C41 Si5 C31 109.34(17) . . ? C40 Si5 C31 110.29(19) . . ? C41 Si5 C42 110.3(2) . . ? C40 Si5 C42 108.7(2) . . ? C31 Si5 C42 108.79(18) . . ? C43 Si6 C44 110.0(3) . . ? C43 Si6 C45 110.1(2) . . ? C44 Si6 C45 109.1(2) . . ? C43 Si6 C33 107.2(2) . . ? C44 Si6 C33 108.04(17) . . ? C45 Si6 C33 112.39(19) . . ? C55 Si7 C46 109.5(2) . . ? C55 Si7 C56 109.1(2) . . ? C46 Si7 C56 111.93(17) . . ? C55 Si7 C57 108.6(3) . . ? C46 Si7 C57 107.07(17) . . ? C56 Si7 C57 110.6(2) . . ? C60 Si8 C58 110.7(3) . . ? C60 Si8 C59 109.3(3) . . ? C58 Si8 C59 108.2(3) . . ? C60 Si8 C48 107.9(2) . . ? C58 Si8 C48 109.66(19) . . ? C59 Si8 C48 111.13(19) . . ? C17 Sn1 C18 32.09(10) . . ? C17 Sn1 C1 116.68(11) . . ? C18 Sn1 C1 124.72(11) . . ? C33 Sn2 C46 125.62(10) . . ? C33 Sn2 C47 117.81(10) . . ? C46 Sn2 C47 31.66(9) . . ? C33 Sn2 C32 31.74(10) . . ? C46 Sn2 C32 119.56(10) . . ? C47 Sn2 C32 132.11(10) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.765 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.088 data_pna21b _database_code_depnum_ccdc_archive 'CCDC 244713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H152 Pb4 Si8' _chemical_formula_weight 2407.70 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 35.144(5) _cell_length_b 10.548(5) _cell_length_c 31.090(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 11525(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 5.946 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4691 _exptl_absorpt_correction_T_max 0.5356 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24183 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1636 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 24183 _reflns_number_gt 14556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0789P)^2^+186.2521P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.492(11) _refine_ls_number_reflns 24183 _refine_ls_number_parameters 929 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.1998 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2319(7) -0.017(2) 0.3656(8) 0.055(3) Uani 1 1 d DU . . C2 C 0.2137(7) 0.092(2) 0.3836(7) 0.055(3) Uani 1 1 d DU . . C3 C 0.2379(7) 0.160(2) 0.4066(7) 0.055(3) Uani 1 1 d DU . . C4 C 0.2731(7) 0.100(2) 0.4057(8) 0.055(3) Uani 1 1 d DU . . C5 C 0.2695(7) -0.007(2) 0.3801(7) 0.055(3) Uani 1 1 d DU . . C6 C 0.2140(11) -0.125(3) 0.3450(10) 0.105(5) Uani 1 1 d U . . H6A H 0.2337 -0.1824 0.3343 0.157 Uiso 1 1 calc R . . H6B H 0.1983 -0.0953 0.3210 0.157 Uiso 1 1 calc R . . H6C H 0.1980 -0.1692 0.3659 0.157 Uiso 1 1 calc R . . C7 C 0.1700(10) 0.128(3) 0.3850(10) 0.105(5) Uani 1 1 d U . . H7A H 0.1597 0.1085 0.4135 0.157 Uiso 1 1 calc R . . H7B H 0.1562 0.0780 0.3633 0.157 Uiso 1 1 calc R . . H7C H 0.1669 0.2181 0.3789 0.157 Uiso 1 1 calc R . . C8 C 0.2307(11) 0.278(3) 0.4347(11) 0.105(5) Uani 1 1 d U . . H8A H 0.2505 0.3411 0.4292 0.157 Uiso 1 1 calc R . . H8B H 0.2313 0.2533 0.4651 0.157 Uiso 1 1 calc R . . H8C H 0.2057 0.3134 0.4278 0.157 Uiso 1 1 calc R . . C9 C 0.3104(11) 0.137(3) 0.4290(11) 0.105(5) Uani 1 1 d U . . H9A H 0.3170 0.2248 0.4216 0.157 Uiso 1 1 calc R . . H9B H 0.3309 0.0805 0.4200 0.157 Uiso 1 1 calc R . . H9C H 0.3068 0.1304 0.4602 0.157 Uiso 1 1 calc R . . C10 C 0.3018(10) -0.106(3) 0.3761(11) 0.105(5) Uani 1 1 d U . . H10A H 0.3264 -0.0644 0.3815 0.157 Uiso 1 1 calc R . . H10B H 0.3017 -0.1423 0.3472 0.157 Uiso 1 1 calc R . . H10C H 0.2979 -0.1733 0.3974 0.157 Uiso 1 1 calc R . . C11 C 0.2131(5) 0.3326(15) 0.2672(6) 0.023(4) Uani 1 1 d . . . C12 C 0.2507(5) 0.3733(17) 0.2530(6) 0.026(4) Uani 1 1 d . . . C13 C 0.2715(6) 0.4863(18) 0.2529(6) 0.034(5) Uani 1 1 d . . . H13 H 0.2611 0.5596 0.2662 0.040 Uiso 1 1 calc R . . C14 C 0.3061(6) 0.4929(16) 0.2343(7) 0.034(5) Uani 1 1 d . . . H14 H 0.3199 0.5701 0.2356 0.041 Uiso 1 1 calc R . . C15 C 0.3214(6) 0.393(2) 0.2140(7) 0.037(5) Uani 1 1 d . . . H15 H 0.3453 0.4029 0.2001 0.045 Uiso 1 1 calc R . . C16 C 0.3035(6) 0.2740(19) 0.2124(6) 0.034(5) Uani 1 1 d . . . H16 H 0.3156 0.2035 0.1993 0.041 Uiso 1 1 calc R . . C17 C 0.2667(5) 0.2619(17) 0.2309(7) 0.026(4) Uiso 1 1 d . . . C18 C 0.2405(5) 0.1562(17) 0.2331(6) 0.029(4) Uani 1 1 d . . . C19 C 0.2078(5) 0.2081(18) 0.2558(6) 0.031(5) Uani 1 1 d . . . H19 H 0.1854 0.1612 0.2620 0.037 Uiso 1 1 calc R . . C20 C 0.1629(6) 0.574(2) 0.2514(8) 0.054(7) Uani 1 1 d . . . H20A H 0.1862 0.6113 0.2396 0.082 Uiso 1 1 calc R . . H20B H 0.1485 0.6397 0.2668 0.082 Uiso 1 1 calc R . . H20C H 0.1473 0.5404 0.2280 0.082 Uiso 1 1 calc R . . C21 C 0.1930(8) 0.507(2) 0.3422(8) 0.068(8) Uani 1 1 d . . . H21A H 0.2025 0.4385 0.3606 0.102 Uiso 1 1 calc R . . H21B H 0.1721 0.5509 0.3568 0.102 Uiso 1 1 calc R . . H21C H 0.2137 0.5675 0.3366 0.102 Uiso 1 1 calc R . . C22 C 0.1314(6) 0.347(2) 0.2997(8) 0.051(6) Uani 1 1 d . . . H22A H 0.1246 0.3011 0.2734 0.076 Uiso 1 1 calc R . . H22B H 0.1107 0.4043 0.3076 0.076 Uiso 1 1 calc R . . H22C H 0.1357 0.2859 0.3230 0.076 Uiso 1 1 calc R . . C23 C 0.2880(7) -0.0911(19) 0.2292(7) 0.046(6) Uani 1 1 d . . . H23A H 0.3113 -0.0443 0.2222 0.069 Uiso 1 1 calc R . . H23B H 0.2889 -0.1751 0.2157 0.069 Uiso 1 1 calc R . . H23C H 0.2859 -0.1006 0.2604 0.069 Uiso 1 1 calc R . . C24 C 0.2522(7) 0.019(2) 0.1500(8) 0.052(6) Uani 1 1 d . . . H24A H 0.2299 0.0623 0.1379 0.078 Uiso 1 1 calc R . . H24B H 0.2550 -0.0643 0.1363 0.078 Uiso 1 1 calc R . . H24C H 0.2750 0.0697 0.1446 0.078 Uiso 1 1 calc R . . C25 C 0.2009(7) -0.0954(19) 0.2183(8) 0.050(6) Uani 1 1 d . . . H25A H 0.1992 -0.1167 0.2489 0.075 Uiso 1 1 calc R . . H25B H 0.2016 -0.1736 0.2012 0.075 Uiso 1 1 calc R . . H25C H 0.1788 -0.0448 0.2098 0.075 Uiso 1 1 calc R . . C26 C 0.2624(7) 0.536(3) 0.0640(10) 0.071(10) Uani 1 1 d . . . C27 C 0.2442(7) 0.427(3) 0.0432(7) 0.054(7) Uani 1 1 d . . . C28 C 0.2217(6) 0.370(2) 0.0715(7) 0.040(5) Uani 1 1 d . . . C29 C 0.2223(6) 0.431(2) 0.1114(7) 0.044(6) Uani 1 1 d . . . C30 C 0.2487(6) 0.5358(17) 0.1085(7) 0.040(5) Uani 1 1 d . . . C31 C 0.2584(9) 0.638(3) 0.1434(14) 0.110(14) Uani 1 1 d . . . H31A H 0.2408 0.7100 0.1407 0.165 Uiso 1 1 calc R . . H31B H 0.2846 0.6683 0.1392 0.165 Uiso 1 1 calc R . . H31C H 0.2560 0.6010 0.1721 0.165 Uiso 1 1 calc R . . C32 C 0.2890(10) 0.628(3) 0.0417(16) 0.15(2) Uani 1 1 d . . . H32A H 0.2763 0.6645 0.0165 0.220 Uiso 1 1 calc R . . H32B H 0.3121 0.5835 0.0326 0.220 Uiso 1 1 calc R . . H32C H 0.2959 0.6963 0.0618 0.220 Uiso 1 1 calc R . . C33 C 0.2472(11) 0.406(4) -0.0024(12) 0.136(18) Uani 1 1 d . . . H33A H 0.2487 0.3151 -0.0083 0.204 Uiso 1 1 calc R . . H33B H 0.2702 0.4480 -0.0133 0.204 Uiso 1 1 calc R . . H33C H 0.2248 0.4418 -0.0168 0.204 Uiso 1 1 calc R . . C34 C 0.1937(7) 0.266(3) 0.0585(10) 0.070(8) Uani 1 1 d . . . H34A H 0.1729 0.3030 0.0416 0.105 Uiso 1 1 calc R . . H34B H 0.1833 0.2257 0.0843 0.105 Uiso 1 1 calc R . . H34C H 0.2070 0.2023 0.0411 0.105 Uiso 1 1 calc R . . C35 C 0.2000(6) 0.398(2) 0.1525(7) 0.054(6) Uani 1 1 d . . . H35A H 0.1754 0.4416 0.1521 0.081 Uiso 1 1 calc R . . H35B H 0.2146 0.4245 0.1777 0.081 Uiso 1 1 calc R . . H35C H 0.1958 0.3060 0.1537 0.081 Uiso 1 1 calc R . . C36 C 0.3747(6) 0.3573(17) 0.0742(7) 0.036(5) Uani 1 1 d . . . C37 C 0.3782(5) 0.2528(14) 0.1053(7) 0.020(4) Uani 1 1 d . . . C38 C 0.3954(5) 0.2470(16) 0.1473(8) 0.029(5) Uani 1 1 d . . . H38 H 0.4072 0.3191 0.1598 0.034 Uiso 1 1 calc R . . C39 C 0.3938(6) 0.133(2) 0.1688(7) 0.044(6) Uani 1 1 d . . . H39 H 0.4069 0.1241 0.1954 0.053 Uiso 1 1 calc R . . C40 C 0.3739(5) 0.0300(17) 0.1527(7) 0.035(5) Uani 1 1 d . . . H40 H 0.3722 -0.0447 0.1697 0.042 Uiso 1 1 calc R . . C41 C 0.3564(6) 0.0322(16) 0.1129(6) 0.031(5) Uani 1 1 d . . . H41 H 0.3435 -0.0402 0.1021 0.038 Uiso 1 1 calc R . . C42 C 0.3584(5) 0.1443(15) 0.0891(7) 0.027(5) Uani 1 1 d . . . C43 C 0.3434(5) 0.1740(17) 0.0476(7) 0.030(5) Uani 1 1 d . . . C44 C 0.3542(6) 0.3037(19) 0.0411(6) 0.035(5) Uani 1 1 d . . . H44 H 0.3478 0.3493 0.0157 0.042 Uiso 1 1 calc R . . C45 C 0.3799(6) 0.619(2) 0.1206(8) 0.049(6) Uani 1 1 d . . . H45A H 0.3522 0.6101 0.1227 0.074 Uiso 1 1 calc R . . H45B H 0.3862 0.7076 0.1139 0.074 Uiso 1 1 calc R . . H45C H 0.3916 0.5955 0.1480 0.074 Uiso 1 1 calc R . . C46 C 0.4513(6) 0.491(2) 0.0860(8) 0.045(6) Uani 1 1 d . . . H46A H 0.4553 0.4573 0.1151 0.067 Uiso 1 1 calc R . . H46B H 0.4641 0.5734 0.0834 0.067 Uiso 1 1 calc R . . H46C H 0.4620 0.4321 0.0649 0.067 Uiso 1 1 calc R . . C47 C 0.3944(7) 0.588(2) 0.0217(7) 0.053(6) Uani 1 1 d . . . H47A H 0.4062 0.5332 -0.0001 0.080 Uiso 1 1 calc R . . H47B H 0.4073 0.6702 0.0220 0.080 Uiso 1 1 calc R . . H47C H 0.3674 0.6000 0.0148 0.080 Uiso 1 1 calc R . . C48 C 0.3544(7) -0.075(2) 0.0006(9) 0.063(7) Uani 1 1 d . . . H48A H 0.3396 -0.1533 -0.0004 0.094 Uiso 1 1 calc R . . H48B H 0.3723 -0.0781 0.0247 0.094 Uiso 1 1 calc R . . H48C H 0.3686 -0.0646 -0.0264 0.094 Uiso 1 1 calc R . . C49 C 0.2747(7) 0.011(2) 0.0281(8) 0.061(7) Uani 1 1 d . . . H49A H 0.2607 0.0847 0.0392 0.091 Uiso 1 1 calc R . . H49B H 0.2782 -0.0509 0.0511 0.091 Uiso 1 1 calc R . . H49C H 0.2602 -0.0273 0.0045 0.091 Uiso 1 1 calc R . . C50 C 0.3134(7) 0.145(2) -0.0429(8) 0.056(6) Uani 1 1 d . . . H50A H 0.2955 0.0960 -0.0605 0.084 Uiso 1 1 calc R . . H50B H 0.3375 0.1542 -0.0583 0.084 Uiso 1 1 calc R . . H50C H 0.3026 0.2292 -0.0372 0.084 Uiso 1 1 calc R . . C51 C 0.4871(6) -0.023(2) 0.0867(8) 0.045(6) Uani 1 1 d . . . C52 C 0.5232(7) -0.0215(17) 0.1056(7) 0.045(6) Uani 1 1 d . . . C53 C 0.5442(5) 0.0751(18) 0.0889(6) 0.034(5) Uani 1 1 d . . . C54 C 0.5211(7) 0.1442(17) 0.0592(6) 0.035(5) Uani 1 1 d . . . C55 C 0.4855(6) 0.082(2) 0.0600(8) 0.047(6) Uani 1 1 d . . . C56 C 0.4546(8) -0.117(2) 0.0951(10) 0.074(4) Uani 1 1 d U . . H56A H 0.4312 -0.0846 0.0820 0.111 Uiso 1 1 calc R . . H56B H 0.4509 -0.1261 0.1262 0.111 Uiso 1 1 calc R . . H56C H 0.4611 -0.1990 0.0825 0.111 Uiso 1 1 calc R . . C57 C 0.5406(8) -0.128(2) 0.1348(9) 0.074(4) Uani 1 1 d U . . H57A H 0.5684 -0.1224 0.1342 0.111 Uiso 1 1 calc R . . H57B H 0.5326 -0.2113 0.1241 0.111 Uiso 1 1 calc R . . H57C H 0.5316 -0.1170 0.1644 0.111 Uiso 1 1 calc R . . C58 C 0.5869(7) 0.091(2) 0.0985(9) 0.074(4) Uani 1 1 d U . . H58A H 0.5922 0.0642 0.1281 0.111 Uiso 1 1 calc R . . H58B H 0.5940 0.1806 0.0951 0.111 Uiso 1 1 calc R . . H58C H 0.6017 0.0394 0.0784 0.111 Uiso 1 1 calc R . . C59 C 0.5328(8) 0.251(3) 0.0350(9) 0.074(4) Uani 1 1 d U . . H59A H 0.5242 0.2414 0.0052 0.111 Uiso 1 1 calc R . . H59B H 0.5607 0.2566 0.0356 0.111 Uiso 1 1 calc R . . H59C H 0.5219 0.3278 0.0474 0.111 Uiso 1 1 calc R . . C60 C 0.4523(9) 0.120(3) 0.0327(11) 0.093(10) Uiso 1 1 d . . . H60A H 0.4535 0.0753 0.0052 0.140 Uiso 1 1 calc R . . H60B H 0.4532 0.2119 0.0276 0.074(4) Uani 1 1 calc RU . . H60C H 0.4286 0.0987 0.0476 0.111 Uiso 1 1 calc R . . C61 C 0.5141(5) 0.1711(18) 0.2312(6) 0.028(3) Uani 1 1 d U . . C62 C 0.4863(6) 0.2798(18) 0.2310(7) 0.031(3) Uani 1 1 d U . . C63 C 0.4496(5) 0.2918(19) 0.2504(6) 0.029(5) Uani 1 1 d . . . H63 H 0.4391 0.2221 0.2657 0.035 Uiso 1 1 calc R . . C64 C 0.4294(6) 0.4008(18) 0.2472(6) 0.033(5) Uani 1 1 d . . . H64 H 0.4048 0.4078 0.2595 0.040 Uiso 1 1 calc R . . C65 C 0.4466(6) 0.5082(18) 0.2241(6) 0.033(5) Uani 1 1 d . . . H65 H 0.4333 0.5864 0.2224 0.039 Uiso 1 1 calc R . . C66 C 0.4814(6) 0.4972(17) 0.2050(7) 0.033(5) Uani 1 1 d . . . H66 H 0.4913 0.5656 0.1886 0.039 Uiso 1 1 calc R . . C67 C 0.5030(6) 0.3824(18) 0.2096(6) 0.031(3) Uani 1 1 d U . . C68 C 0.5398(6) 0.3499(17) 0.1950(6) 0.028(3) Uani 1 1 d U . . C69 C 0.5456(6) 0.2239(17) 0.2098(7) 0.031(5) Uani 1 1 d . . . H69 H 0.5688 0.1792 0.2056 0.037 Uiso 1 1 calc R . . C70 C 0.5812(6) 0.598(2) 0.2042(7) 0.043(5) Uani 1 1 d . . . H70A H 0.5890 0.6698 0.1862 0.065 Uiso 1 1 calc R . . H70B H 0.6004 0.5832 0.2265 0.065 Uiso 1 1 calc R . . H70C H 0.5567 0.6172 0.2178 0.065 Uiso 1 1 calc R . . C71 C 0.6223(6) 0.369(2) 0.1650(8) 0.049(6) Uani 1 1 d . . . H71A H 0.6405 0.4223 0.1494 0.074 Uiso 1 1 calc R . . H71B H 0.6180 0.2903 0.1490 0.074 Uiso 1 1 calc R . . H71C H 0.6323 0.3491 0.1936 0.074 Uiso 1 1 calc R . . C72 C 0.5610(7) 0.511(2) 0.1170(7) 0.051(6) Uani 1 1 d . . . H72A H 0.5351 0.5444 0.1189 0.077 Uiso 1 1 calc R . . H72B H 0.5616 0.4397 0.0968 0.077 Uiso 1 1 calc R . . H72C H 0.5782 0.5776 0.1070 0.077 Uiso 1 1 calc R . . C73 C 0.5020(7) 0.044(2) 0.3178(6) 0.044(6) Uani 1 1 d . . . H73A H 0.5245 0.0848 0.3303 0.066 Uiso 1 1 calc R . . H73B H 0.4977 -0.0378 0.3318 0.066 Uiso 1 1 calc R . . H73C H 0.4797 0.0986 0.3222 0.066 Uiso 1 1 calc R . . C74 C 0.4689(6) -0.0745(19) 0.2377(8) 0.045(6) Uani 1 1 d . . . H74A H 0.4468 -0.0190 0.2339 0.067 Uiso 1 1 calc R . . H74B H 0.4626 -0.1423 0.2580 0.067 Uiso 1 1 calc R . . H74C H 0.4759 -0.1116 0.2099 0.067 Uiso 1 1 calc R . . C75 C 0.5554(6) -0.071(2) 0.2498(7) 0.040(5) Uani 1 1 d . . . H75A H 0.5634 -0.0612 0.2198 0.060 Uiso 1 1 calc R . . H75B H 0.5512 -0.1613 0.2559 0.060 Uiso 1 1 calc R . . H75C H 0.5753 -0.0382 0.2688 0.060 Uiso 1 1 calc R . . C76 C 0.5322(5) 0.3978(17) 0.3907(6) 0.034(2) Uani 1 1 d DU . . C77 C 0.5077(5) 0.4655(17) 0.4180(6) 0.034(2) Uani 1 1 d DU . . C78 C 0.4920(5) 0.5649(17) 0.3926(6) 0.034(2) Uani 1 1 d DU . . C79 C 0.5067(6) 0.5581(18) 0.3497(6) 0.034(2) Uani 1 1 d DU . . C80 C 0.5323(5) 0.4500(18) 0.3485(6) 0.034(2) Uani 1 1 d DU . . C81 C 0.5592(6) 0.290(2) 0.4025(8) 0.053(7) Uani 1 1 d . . . H81A H 0.5585 0.2768 0.4337 0.080 Uiso 1 1 calc R . . H81B H 0.5851 0.3129 0.3937 0.080 Uiso 1 1 calc R . . H81C H 0.5513 0.2127 0.3877 0.080 Uiso 1 1 calc R . . C82 C 0.5036(7) 0.454(3) 0.4667(7) 0.058(7) Uani 1 1 d . . . H82A H 0.5230 0.5057 0.4809 0.087 Uiso 1 1 calc R . . H82B H 0.5068 0.3649 0.4752 0.087 Uiso 1 1 calc R . . H82C H 0.4782 0.4830 0.4754 0.087 Uiso 1 1 calc R . . C83 C 0.4687(7) 0.6771(19) 0.4094(8) 0.052(6) Uani 1 1 d . . . H83A H 0.4476 0.6455 0.4271 0.078 Uiso 1 1 calc R . . H83B H 0.4585 0.7252 0.3850 0.078 Uiso 1 1 calc R . . H83C H 0.4850 0.7323 0.4268 0.078 Uiso 1 1 calc R . . C84 C 0.4981(7) 0.646(2) 0.3137(9) 0.062(7) Uani 1 1 d . . . H84A H 0.4705 0.6571 0.3115 0.092 Uiso 1 1 calc R . . H84B H 0.5079 0.6098 0.2868 0.092 Uiso 1 1 calc R . . H84C H 0.5103 0.7277 0.3191 0.092 Uiso 1 1 calc R . . C85 C 0.5551(7) 0.407(2) 0.3110(7) 0.053(6) Uani 1 1 d . . . H85A H 0.5504 0.3162 0.3061 0.079 Uiso 1 1 calc R . . H85B H 0.5822 0.4203 0.3168 0.079 Uiso 1 1 calc R . . H85C H 0.5476 0.4549 0.2854 0.079 Uiso 1 1 calc R . . C86 C 0.3802(5) 0.3747(19) 0.3872(6) 0.029(5) Uani 1 1 d . . . C87 C 0.3996(6) 0.3310(19) 0.4245(7) 0.038(5) Uani 1 1 d . . . H87 H 0.4033 0.3800 0.4498 0.046 Uiso 1 1 calc R . . C88 C 0.4131(6) 0.201(2) 0.4189(7) 0.045(6) Uani 1 1 d . . . C89 C 0.3990(5) 0.1693(17) 0.3763(7) 0.033(5) Uani 1 1 d . . . C90 C 0.4002(5) 0.0496(17) 0.3528(7) 0.035(5) Uani 1 1 d . . . H90 H 0.4129 -0.0210 0.3653 0.042 Uiso 1 1 calc R . . C91 C 0.3841(6) 0.0369(17) 0.3147(6) 0.036(5) Uani 1 1 d . . . H91 H 0.3861 -0.0411 0.2996 0.043 Uiso 1 1 calc R . . C92 C 0.3635(6) 0.1402(18) 0.2960(7) 0.035(5) Uani 1 1 d . . . H92 H 0.3512 0.1300 0.2691 0.042 Uiso 1 1 calc R . . C93 C 0.3616(6) 0.258(2) 0.3180(7) 0.038(5) Uani 1 1 d . . . H93 H 0.3488 0.3274 0.3050 0.045 Uiso 1 1 calc R . . C94 C 0.3778(5) 0.2732(17) 0.3574(7) 0.026(5) Uani 1 1 d . . . C95 C 0.3032(6) 0.505(2) 0.3732(8) 0.050(6) Uani 1 1 d . . . H95A H 0.2905 0.5871 0.3694 0.075 Uiso 1 1 calc R . . H95B H 0.2919 0.4603 0.3976 0.075 Uiso 1 1 calc R . . H95C H 0.3003 0.4543 0.3471 0.075 Uiso 1 1 calc R . . C96 C 0.3725(6) 0.6294(18) 0.3385(8) 0.046(6) Uani 1 1 d . . . H96A H 0.3706 0.5811 0.3116 0.069 Uiso 1 1 calc R . . H96B H 0.3992 0.6517 0.3437 0.069 Uiso 1 1 calc R . . H96C H 0.3574 0.7070 0.3361 0.069 Uiso 1 1 calc R . . C97 C 0.3586(6) 0.617(2) 0.4371(7) 0.047(6) Uani 1 1 d . . . H97A H 0.3855 0.6283 0.4444 0.071 Uiso 1 1 calc R . . H97B H 0.3461 0.5665 0.4595 0.071 Uiso 1 1 calc R . . H97C H 0.3462 0.6999 0.4351 0.071 Uiso 1 1 calc R . . C98 C 0.4014(7) -0.040(2) 0.4690(8) 0.053(4) Uani 1 1 d U . . H98A H 0.3806 -0.0158 0.4883 0.079 Uiso 1 1 calc R . . H98B H 0.4160 -0.1093 0.4818 0.079 Uiso 1 1 calc R . . H98C H 0.3909 -0.0672 0.4413 0.079 Uiso 1 1 calc R . . C99 C 0.4805(7) 0.034(2) 0.4421(8) 0.053(4) Uani 1 1 d U . . H99A H 0.4777 -0.0030 0.4134 0.079 Uiso 1 1 calc R . . H99B H 0.4889 -0.0313 0.4624 0.079 Uiso 1 1 calc R . . H99C H 0.4994 0.1025 0.4411 0.079 Uiso 1 1 calc R . . C100 C 0.4390(7) 0.187(2) 0.5114(8) 0.053(4) Uani 1 1 d U . . H10D H 0.4633 0.2325 0.5113 0.079 Uiso 1 1 calc R . . H10E H 0.4385 0.1271 0.5355 0.079 Uiso 1 1 calc R . . H10F H 0.4181 0.2480 0.5146 0.079 Uiso 1 1 calc R . . Si1 Si 0.17578(16) 0.4401(5) 0.29028(19) 0.0337(13) Uani 1 1 d . . . Si2 Si 0.24567(17) -0.0015(5) 0.20831(18) 0.0332(13) Uani 1 1 d . . . Si3 Si 0.39884(16) 0.5113(5) 0.07594(19) 0.0355(14) Uani 1 1 d . . . Si4 Si 0.32154(17) 0.0632(5) 0.00786(19) 0.0364(14) Uani 1 1 d . . . Si5 Si 0.57641(17) 0.4556(5) 0.17062(19) 0.0354(14) Uani 1 1 d . . . Si6 Si 0.50957(16) 0.0197(5) 0.25903(18) 0.0314(13) Uani 1 1 d . . . Si7 Si 0.35455(16) 0.5319(5) 0.38373(19) 0.0344(13) Uani 1 1 d . . . Si8 Si 0.43341(17) 0.1002(5) 0.46036(19) 0.0369(14) Uani 1 1 d . . . Pb1 Pb 0.25815(2) 0.17872(7) 0.32290(2) 0.02919(18) Uani 1 1 d . . . Pb2 Pb 0.29513(2) 0.33552(6) 0.09719(2) 0.03172(19) Uani 1 1 d . . . Pb3 Pb 0.49607(2) 0.17933(6) 0.14249(2) 0.02782(18) Uani 1 1 d . . . Pb4 Pb 0.45957(2) 0.36007(6) 0.36534(3) 0.03000(18) 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 0.062(7) 0.058(7) 0.043(7) 0.023(5) 0.009(6) 0.009(5) C2 0.062(7) 0.058(7) 0.043(7) 0.023(5) 0.009(6) 0.009(5) C3 0.062(7) 0.058(7) 0.043(7) 0.023(5) 0.009(6) 0.009(5) C4 0.062(7) 0.058(7) 0.043(7) 0.023(5) 0.009(6) 0.009(5) C5 0.062(7) 0.058(7) 0.043(7) 0.023(5) 0.009(6) 0.009(5) C6 0.132(13) 0.112(11) 0.070(10) 0.042(9) 0.016(9) -0.010(10) C7 0.132(13) 0.112(11) 0.070(10) 0.042(9) 0.016(9) -0.010(10) C8 0.132(13) 0.112(11) 0.070(10) 0.042(9) 0.016(9) -0.010(10) C9 0.132(13) 0.112(11) 0.070(10) 0.042(9) 0.016(9) -0.010(10) C10 0.132(13) 0.112(11) 0.070(10) 0.042(9) 0.016(9) -0.010(10) C11 0.024(10) 0.014(8) 0.031(11) 0.006(8) 0.003(8) 0.001(7) C12 0.028(11) 0.026(9) 0.023(10) 0.004(8) 0.012(8) 0.009(8) C13 0.040(13) 0.031(11) 0.030(11) -0.011(9) -0.016(9) 0.009(9) C14 0.037(12) 0.008(8) 0.059(14) 0.008(9) 0.009(11) -0.002(8) C15 0.020(11) 0.053(13) 0.038(13) 0.008(11) -0.003(9) -0.007(9) C16 0.062(15) 0.026(10) 0.016(11) 0.009(9) -0.008(10) 0.004(10) C18 0.022(10) 0.034(11) 0.031(11) 0.004(9) -0.016(9) 0.008(8) C19 0.024(11) 0.038(11) 0.031(12) 0.005(9) -0.001(9) -0.011(9) C20 0.022(12) 0.050(13) 0.09(2) 0.041(13) 0.011(12) 0.013(10) C21 0.08(2) 0.071(18) 0.056(17) -0.021(14) 0.007(14) 0.012(15) C22 0.039(14) 0.043(13) 0.070(18) -0.003(12) 0.011(12) -0.001(10) C23 0.063(16) 0.030(11) 0.046(14) -0.003(10) -0.003(12) 0.025(10) C24 0.059(16) 0.036(12) 0.060(17) 0.012(12) -0.003(13) 0.001(10) C25 0.066(16) 0.029(11) 0.055(15) -0.023(11) 0.008(12) -0.008(10) C26 0.043(15) 0.073(19) 0.10(2) 0.062(18) 0.037(15) 0.024(13) C27 0.066(17) 0.080(19) 0.016(12) 0.006(12) -0.004(11) 0.042(15) C28 0.048(14) 0.039(12) 0.034(13) -0.005(10) -0.025(11) -0.003(10) C29 0.040(13) 0.062(14) 0.031(12) 0.019(11) -0.018(10) 0.010(11) C30 0.056(14) 0.018(9) 0.045(14) 0.012(9) -0.017(11) 0.007(9) C31 0.11(3) 0.047(16) 0.17(4) -0.04(2) -0.02(3) 0.049(16) C32 0.07(2) 0.11(3) 0.26(6) 0.11(3) 0.05(3) 0.02(2) C33 0.11(3) 0.21(5) 0.09(3) 0.03(3) 0.01(2) 0.11(3) C34 0.047(16) 0.079(19) 0.09(2) 0.007(16) -0.003(15) 0.031(14) C35 0.028(13) 0.088(18) 0.046(15) 0.009(13) -0.001(10) -0.003(12) C36 0.047(13) 0.022(10) 0.039(13) 0.004(9) 0.007(10) 0.006(9) C37 0.015(9) 0.015(8) 0.032(13) 0.006(7) 0.000(8) -0.001(6) C38 0.017(10) 0.021(10) 0.047(15) -0.001(9) 0.006(10) -0.003(7) C39 0.028(12) 0.076(16) 0.028(12) 0.015(12) 0.002(10) 0.021(11) C40 0.023(11) 0.022(10) 0.061(16) 0.007(10) -0.020(10) 0.003(8) C41 0.036(12) 0.018(9) 0.040(13) -0.005(9) 0.003(9) 0.006(8) C42 0.022(10) 0.020(9) 0.039(13) -0.001(9) -0.003(9) 0.009(7) C43 0.023(10) 0.032(10) 0.034(12) 0.003(9) 0.000(9) -0.018(8) C44 0.046(13) 0.049(13) 0.009(10) -0.002(9) -0.003(9) -0.015(10) C45 0.035(13) 0.038(12) 0.076(18) -0.004(12) 0.008(11) -0.002(10) C46 0.050(14) 0.039(12) 0.045(15) 0.004(10) 0.000(11) 0.009(10) C47 0.069(17) 0.043(13) 0.048(15) 0.008(11) 0.004(12) -0.008(12) C48 0.057(17) 0.069(17) 0.063(17) -0.020(14) -0.020(13) -0.005(13) C49 0.056(16) 0.066(16) 0.061(17) -0.023(14) 0.024(13) -0.012(13) C50 0.040(14) 0.072(17) 0.055(16) 0.002(13) -0.002(11) -0.013(12) C51 0.044(14) 0.033(12) 0.058(16) -0.018(11) 0.013(11) -0.004(10) C52 0.080(18) 0.019(10) 0.036(13) 0.001(9) 0.007(12) 0.015(10) C53 0.018(10) 0.043(11) 0.040(12) -0.027(10) -0.004(9) 0.013(8) C54 0.063(15) 0.022(10) 0.020(10) -0.005(8) 0.012(10) -0.002(9) C55 0.031(13) 0.053(14) 0.058(16) -0.045(13) -0.018(11) 0.018(10) C56 0.085(10) 0.066(8) 0.071(10) -0.016(8) 0.011(8) 0.020(7) C57 0.085(10) 0.066(8) 0.071(10) -0.016(8) 0.011(8) 0.020(7) C58 0.085(10) 0.066(8) 0.071(10) -0.016(8) 0.011(8) 0.020(7) C59 0.085(10) 0.066(8) 0.071(10) -0.016(8) 0.011(8) 0.020(7) H60B 0.085(10) 0.066(8) 0.071(10) -0.016(8) 0.011(8) 0.020(7) C61 0.035(8) 0.038(8) 0.012(7) -0.002(6) -0.003(6) 0.001(6) C62 0.044(9) 0.028(7) 0.020(8) -0.002(6) -0.003(6) 0.004(6) C63 0.021(10) 0.042(12) 0.025(12) -0.004(9) 0.012(8) 0.004(8) C64 0.048(13) 0.032(11) 0.020(11) -0.017(9) 0.015(9) 0.003(9) C65 0.051(13) 0.032(11) 0.015(10) -0.016(9) -0.012(9) 0.021(9) C66 0.036(12) 0.025(10) 0.037(12) 0.002(9) 0.016(10) 0.008(8) C67 0.044(9) 0.028(7) 0.020(8) -0.002(6) -0.003(6) 0.004(6) C68 0.035(8) 0.038(8) 0.012(7) -0.002(6) -0.003(6) 0.001(6) C69 0.034(12) 0.019(9) 0.039(13) 0.008(9) 0.006(9) -0.004(8) C70 0.048(14) 0.053(13) 0.029(12) -0.007(10) 0.007(10) -0.018(10) C71 0.025(12) 0.055(14) 0.067(17) 0.004(12) 0.005(11) -0.008(10) C72 0.069(17) 0.045(13) 0.040(14) 0.004(11) -0.003(12) -0.026(12) C73 0.072(16) 0.043(12) 0.016(11) 0.010(9) -0.008(11) 0.010(11) C74 0.052(15) 0.027(11) 0.056(15) 0.001(11) 0.012(11) -0.001(9) C75 0.035(13) 0.044(12) 0.042(13) 0.005(10) -0.010(10) 0.003(9) C76 0.038(6) 0.032(5) 0.031(5) -0.011(4) -0.007(4) -0.005(4) C77 0.038(6) 0.032(5) 0.031(5) -0.011(4) -0.007(4) -0.005(4) C78 0.038(6) 0.032(5) 0.031(5) -0.011(4) -0.007(4) -0.005(4) C79 0.038(6) 0.032(5) 0.031(5) -0.011(4) -0.007(4) -0.005(4) C80 0.038(6) 0.032(5) 0.031(5) -0.011(4) -0.007(4) -0.005(4) C81 0.040(14) 0.064(15) 0.056(17) 0.033(13) -0.006(12) 0.004(11) C82 0.041(14) 0.094(19) 0.039(14) -0.016(13) -0.010(11) -0.026(13) C83 0.055(15) 0.037(12) 0.064(17) -0.011(11) -0.002(12) 0.022(11) C84 0.071(18) 0.052(15) 0.062(18) -0.017(13) -0.023(14) 0.002(12) C85 0.068(17) 0.049(14) 0.042(15) -0.015(11) -0.016(12) -0.006(12) C86 0.019(10) 0.041(11) 0.028(11) 0.000(9) -0.003(8) 0.005(8) C87 0.049(14) 0.044(12) 0.022(12) -0.002(10) 0.001(10) 0.017(10) C88 0.033(12) 0.060(15) 0.042(14) 0.015(12) -0.023(10) -0.019(10) C89 0.020(10) 0.039(11) 0.040(13) 0.006(9) 0.013(9) 0.002(8) C90 0.035(12) 0.020(9) 0.050(16) -0.010(9) 0.015(10) -0.008(8) C91 0.066(15) 0.020(10) 0.023(12) -0.007(9) 0.007(10) 0.004(9) C92 0.041(13) 0.030(11) 0.035(13) -0.007(9) -0.014(10) -0.007(9) C93 0.032(12) 0.057(14) 0.025(14) 0.015(11) -0.004(10) -0.003(9) C94 0.022(10) 0.029(9) 0.027(13) 0.017(9) -0.007(9) -0.001(7) C95 0.042(13) 0.049(13) 0.058(16) 0.011(12) -0.011(12) 0.012(10) C96 0.051(14) 0.020(10) 0.066(17) 0.009(10) -0.005(12) -0.003(9) C97 0.031(13) 0.053(14) 0.057(16) -0.005(12) -0.006(11) 0.015(10) C98 0.055(9) 0.055(8) 0.048(9) 0.016(7) -0.011(7) 0.002(7) C99 0.055(9) 0.055(8) 0.048(9) 0.016(7) -0.011(7) 0.002(7) C100 0.055(9) 0.055(8) 0.048(9) 0.016(7) -0.011(7) 0.002(7) Si1 0.033(3) 0.032(3) 0.037(3) -0.002(3) 0.007(3) 0.005(2) Si2 0.041(3) 0.027(3) 0.032(3) 0.000(2) 0.004(3) 0.001(2) Si3 0.034(3) 0.033(3) 0.040(3) 0.001(3) 0.002(3) -0.002(2) Si4 0.037(3) 0.036(3) 0.036(3) -0.008(3) 0.001(3) -0.008(2) Si5 0.040(4) 0.030(3) 0.036(3) -0.006(3) 0.003(3) -0.007(2) Si6 0.037(3) 0.026(3) 0.032(3) 0.004(2) -0.003(3) 0.003(2) Si7 0.034(3) 0.028(3) 0.042(4) 0.004(2) -0.003(3) 0.003(2) Si8 0.043(4) 0.036(3) 0.032(3) 0.011(3) -0.001(3) 0.005(3) Pb1 0.0326(4) 0.0288(4) 0.0262(4) 0.0060(4) 0.0028(3) -0.0005(3) Pb2 0.0323(4) 0.0312(4) 0.0317(4) 0.0072(4) 0.0008(3) 0.0063(3) Pb3 0.0335(4) 0.0268(3) 0.0232(4) -0.0038(4) 0.0025(3) 0.0043(3) Pb4 0.0308(4) 0.0281(3) 0.0311(4) -0.0040(4) -0.0042(4) -0.0026(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 C5 1.40(3) . ? C1 C2 1.43(3) . ? C1 C6 1.45(4) . ? C1 Pb1 2.62(2) . ? C2 C3 1.32(3) . ? C2 C7 1.58(4) . ? C2 Pb1 2.62(2) . ? C3 C4 1.39(3) . ? C3 C8 1.54(4) . ? C3 Pb1 2.70(2) . ? C4 C5 1.38(3) . ? C4 C9 1.55(4) . ? C4 Pb1 2.76(2) . ? C5 C10 1.55(4) . ? C5 Pb1 2.68(2) . ? C11 C19 1.37(2) . ? C11 C12 1.46(2) . ? C11 Si1 1.876(18) . ? C11 Pb1 2.854(17) . ? C12 C13 1.40(3) . ? C12 C17 1.47(3) . ? C13 C14 1.35(3) . ? C14 C15 1.34(3) . ? C15 C16 1.40(3) . ? C16 C17 1.42(3) . ? C17 C18 1.45(3) . ? C18 C19 1.45(3) . ? C18 Si2 1.84(2) . ? C19 Pb1 2.754(19) . ? C20 Si1 1.92(2) . ? C21 Si1 1.86(2) . ? C22 Si1 1.87(2) . ? C23 Si2 1.88(2) . ? C24 Si2 1.84(3) . ? C25 Si2 1.88(2) . ? C26 C27 1.46(4) . ? C26 C30 1.46(3) . ? C26 C32 1.52(4) . ? C26 Pb2 2.62(2) . ? C27 C28 1.32(3) . ? C27 C33 1.44(4) . ? C27 Pb2 2.63(2) . ? C28 C29 1.40(3) . ? C28 C34 1.53(3) . ? C28 Pb2 2.73(2) . ? C29 C30 1.45(3) . ? C29 C35 1.54(3) . ? C29 Pb2 2.78(2) . ? C30 C31 1.57(4) . ? C30 Pb2 2.692(19) . ? C36 C44 1.38(3) . ? C36 C37 1.47(3) . ? C36 Si3 1.83(2) . ? C37 C42 1.43(2) . ? C37 C38 1.44(3) . ? C38 C39 1.38(3) . ? C39 C40 1.38(3) . ? C40 C41 1.38(3) . ? C41 C42 1.40(3) . ? C42 C43 1.43(3) . ? C43 C44 1.43(3) . ? C43 Si4 1.87(2) . ? C43 Pb2 2.86(2) . ? C44 Pb2 2.73(2) . ? C45 Si3 1.91(2) . ? C46 Si3 1.88(2) . ? C47 Si3 1.88(2) . ? C48 Si4 1.87(3) . ? C49 Si4 1.84(2) . ? C50 Si4 1.82(2) . ? C51 C55 1.38(3) . ? C51 C52 1.40(3) . ? C51 C56 1.53(3) . ? C51 Pb3 2.76(2) . ? C52 C53 1.36(3) . ? C52 C57 1.57(3) . ? C52 Pb3 2.592(19) . ? C53 C54 1.43(3) . ? C53 C58 1.54(3) . ? C53 Pb3 2.615(17) . ? C54 C55 1.41(3) . ? C54 C59 1.41(3) . ? C54 Pb3 2.759(19) . ? C55 C60 1.50(4) . ? C55 Pb3 2.79(2) . ? C61 C69 1.41(3) . ? C61 C62 1.51(3) . ? C61 Si6 1.823(19) . ? C61 Pb3 2.832(18) . ? C62 C67 1.40(3) . ? C62 C63 1.43(3) . ? C63 C64 1.35(3) . ? C64 C65 1.47(3) . ? C65 C66 1.36(3) . ? C66 C67 1.44(3) . ? C67 C68 1.41(3) . ? C68 C69 1.42(2) . ? C68 Si5 1.86(2) . ? C69 Pb3 2.76(2) . ? C70 Si5 1.84(2) . ? C71 Si5 1.86(2) . ? C72 Si5 1.85(2) . ? C73 Si6 1.86(2) . ? C74 Si6 1.86(2) . ? C75 Si6 1.90(2) . ? C76 C77 1.40(3) . ? C76 C80 1.42(3) . ? C76 C81 1.52(3) . ? C76 Pb4 2.701(18) . ? C77 C78 1.42(3) . ? C77 C82 1.53(3) . ? C77 Pb4 2.603(17) . ? C78 C79 1.43(3) . ? C78 C83 1.53(3) . ? C78 Pb4 2.586(17) . ? C79 C80 1.45(3) . ? C79 C84 1.48(3) . ? C79 Pb4 2.710(19) . ? C80 C85 1.49(3) . ? C80 Pb4 2.777(19) . ? C86 C94 1.42(3) . ? C86 C87 1.42(3) . ? C86 Si7 1.89(2) . ? C87 C88 1.46(3) . ? C87 Pb4 2.81(2) . ? C88 C89 1.45(3) . ? C88 Si8 1.82(2) . ? C88 Pb4 2.87(2) . ? C89 C94 1.45(2) . ? C89 C90 1.46(3) . ? C90 C91 1.32(3) . ? C91 C92 1.43(3) . ? C92 C93 1.42(3) . ? C93 C94 1.36(3) . ? C95 Si7 1.85(2) . ? C96 Si7 1.85(2) . ? C97 Si7 1.89(2) . ? C98 Si8 1.88(2) . ? C99 Si8 1.88(2) . ? C100 Si8 1.84(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 104(2) . . ? C5 C1 C6 128(3) . . ? C2 C1 C6 128(3) . . ? C5 C1 Pb1 76.8(12) . . ? C2 C1 Pb1 73.9(11) . . ? C6 C1 Pb1 123.2(18) . . ? C3 C2 C1 111(2) . . ? C3 C2 C7 119(2) . . ? C1 C2 C7 129(3) . . ? C3 C2 Pb1 79.3(12) . . ? C1 C2 Pb1 74.4(11) . . ? C7 C2 Pb1 121.1(15) . . ? C2 C3 C4 108(2) . . ? C2 C3 C8 130(3) . . ? C4 C3 C8 122(3) . . ? C2 C3 Pb1 71.9(12) . . ? C4 C3 Pb1 77.4(13) . . ? C8 C3 Pb1 122.1(16) . . ? C5 C4 C3 108(2) . . ? C5 C4 C9 124(2) . . ? C3 C4 C9 129(3) . . ? C5 C4 Pb1 72.0(13) . . ? C3 C4 Pb1 73.2(12) . . ? C9 C4 Pb1 121.3(16) . . ? C4 C5 C1 109(2) . . ? C4 C5 C10 122(3) . . ? C1 C5 C10 128(3) . . ? C4 C5 Pb1 78.5(13) . . ? C1 C5 Pb1 72.6(11) . . ? C10 C5 Pb1 123.4(16) . . ? C19 C11 C12 109.0(16) . . ? C19 C11 Si1 125.6(14) . . ? C12 C11 Si1 124.9(12) . . ? C19 C11 Pb1 71.8(11) . . ? C12 C11 Pb1 81.2(10) . . ? Si1 C11 Pb1 120.0(8) . . ? C13 C12 C11 136.5(17) . . ? C13 C12 C17 118.7(17) . . ? C11 C12 C17 104.6(16) . . ? C14 C13 C12 121.1(18) . . ? C15 C14 C13 121.6(18) . . ? C14 C15 C16 122.5(19) . . ? C15 C16 C17 118.4(19) . . ? C16 C17 C18 131.9(18) . . ? C16 C17 C12 117.6(17) . . ? C18 C17 C12 110.5(17) . . ? C17 C18 C19 103.7(16) . . ? C17 C18 Si2 127.7(15) . . ? C19 C18 Si2 128.4(14) . . ? C11 C19 C18 112.2(16) . . ? C11 C19 Pb1 79.9(11) . . ? C18 C19 Pb1 79.5(11) . . ? C27 C26 C30 105.8(19) . . ? C27 C26 C32 125(3) . . ? C30 C26 C32 129(3) . . ? C27 C26 Pb2 74.4(12) . . ? C30 C26 Pb2 76.8(12) . . ? C32 C26 Pb2 115.2(17) . . ? C28 C27 C33 129(3) . . ? C28 C27 C26 108.8(19) . . ? C33 C27 C26 121(3) . . ? C28 C27 Pb2 79.7(13) . . ? C33 C27 Pb2 121.6(17) . . ? C26 C27 Pb2 73.2(13) . . ? C27 C28 C29 112(2) . . ? C27 C28 C34 122(2) . . ? C29 C28 C34 125(2) . . ? C27 C28 Pb2 71.8(13) . . ? C29 C28 Pb2 77.6(12) . . ? C34 C28 Pb2 126.0(15) . . ? C28 C29 C30 108(2) . . ? C28 C29 C35 129(2) . . ? C30 C29 C35 124(2) . . ? C28 C29 Pb2 73.1(13) . . ? C30 C29 Pb2 71.2(12) . . ? C35 C29 Pb2 121.2(13) . . ? C29 C30 C26 106(2) . . ? C29 C30 C31 129(2) . . ? C26 C30 C31 126(3) . . ? C29 C30 Pb2 78.3(11) . . ? C26 C30 Pb2 71.2(12) . . ? C31 C30 Pb2 119.9(15) . . ? C44 C36 C37 103.2(17) . . ? C44 C36 Si3 128.9(16) . . ? C37 C36 Si3 127.2(16) . . ? C42 C37 C38 119.2(15) . . ? C42 C37 C36 109.1(18) . . ? C38 C37 C36 131.5(16) . . ? C39 C38 C37 117.3(17) . . ? C40 C39 C38 122(2) . . ? C39 C40 C41 122.4(18) . . ? C40 C41 C42 117.7(18) . . ? C41 C42 C37 121.1(18) . . ? C41 C42 C43 130.2(17) . . ? C37 C42 C43 108.7(16) . . ? C42 C43 C44 103.8(15) . . ? C42 C43 Si4 127.8(13) . . ? C44 C43 Si4 127.8(15) . . ? C42 C43 Pb2 82.1(11) . . ? C44 C43 Pb2 70.5(11) . . ? Si4 C43 Pb2 119.1(8) . . ? C36 C44 C43 115.1(18) . . ? C36 C44 Pb2 82.5(12) . . ? C43 C44 Pb2 79.9(11) . . ? C55 C51 C52 106.5(18) . . ? C55 C51 C56 126(2) . . ? C52 C51 C56 128(2) . . ? C55 C51 Pb3 76.5(11) . . ? C52 C51 Pb3 68.1(11) . . ? C56 C51 Pb3 118.4(15) . . ? C53 C52 C51 109.7(18) . . ? C53 C52 C57 123(2) . . ? C51 C52 C57 126(2) . . ? C53 C52 Pb3 75.8(10) . . ? C51 C52 Pb3 81.8(12) . . ? C57 C52 Pb3 118.2(15) . . ? C52 C53 C54 108.8(18) . . ? C52 C53 C58 122(2) . . ? C54 C53 C58 128(2) . . ? C52 C53 Pb3 73.9(11) . . ? C54 C53 Pb3 80.2(10) . . ? C58 C53 Pb3 117.4(14) . . ? C55 C54 C59 130(2) . . ? C55 C54 C53 104.8(18) . . ? C59 C54 C53 126(2) . . ? C55 C54 Pb3 76.3(12) . . ? C59 C54 Pb3 119.1(15) . . ? C53 C54 Pb3 69.1(10) . . ? C51 C55 C54 110.0(19) . . ? C51 C55 C60 126(2) . . ? C54 C55 C60 124(3) . . ? C51 C55 Pb3 74.6(13) . . ? C54 C55 Pb3 74.1(11) . . ? C60 C55 Pb3 121.8(16) . . ? C69 C61 C62 102.0(16) . . ? C69 C61 Si6 129.8(15) . . ? C62 C61 Si6 127.7(14) . . ? C69 C61 Pb3 72.8(11) . . ? C62 C61 Pb3 80.0(11) . . ? Si6 C61 Pb3 118.0(8) . . ? C67 C62 C63 120.7(18) . . ? C67 C62 C61 108.6(17) . . ? C63 C62 C61 130.6(18) . . ? C64 C63 C62 121.1(19) . . ? C63 C64 C65 118.3(18) . . ? C66 C65 C64 121.0(17) . . ? C65 C66 C67 120.2(18) . . ? C62 C67 C68 110.4(17) . . ? C62 C67 C66 118.5(18) . . ? C68 C67 C66 131.1(18) . . ? C67 C68 C69 104.8(17) . . ? C67 C68 Si5 128.1(14) . . ? C69 C68 Si5 126.3(15) . . ? C61 C69 C68 114.2(18) . . ? C61 C69 Pb3 78.2(12) . . ? C68 C69 Pb3 79.8(12) . . ? C77 C76 C80 111.2(18) . . ? C77 C76 C81 127.9(19) . . ? C80 C76 C81 120.6(19) . . ? C77 C76 Pb4 70.9(9) . . ? C80 C76 Pb4 78.0(11) . . ? C81 C76 Pb4 123.4(13) . . ? C76 C77 C78 106.1(18) . . ? C76 C77 C82 128(2) . . ? C78 C77 C82 124.9(19) . . ? C76 C77 Pb4 78.5(9) . . ? C78 C77 Pb4 73.4(9) . . ? C82 C77 Pb4 121.8(13) . . ? C77 C78 C79 109.8(18) . . ? C77 C78 C83 126.1(19) . . ? C79 C78 C83 123.3(19) . . ? C77 C78 Pb4 74.8(9) . . ? C79 C78 Pb4 79.1(10) . . ? C83 C78 Pb4 121.4(13) . . ? C78 C79 C80 106.5(17) . . ? C78 C79 C84 126.8(19) . . ? C80 C79 C84 126.7(19) . . ? C78 C79 Pb4 69.6(10) . . ? C80 C79 Pb4 77.2(11) . . ? C84 C79 Pb4 119.5(14) . . ? C76 C80 C79 106.3(17) . . ? C76 C80 C85 127.3(19) . . ? C79 C80 C85 126.4(19) . . ? C76 C80 Pb4 72.0(10) . . ? C79 C80 Pb4 72.1(11) . . ? C85 C80 Pb4 122.5(13) . . ? C94 C86 C87 108.5(17) . . ? C94 C86 Si7 126.7(14) . . ? C87 C86 Si7 124.0(15) . . ? C86 C87 C88 111.2(18) . . ? C86 C87 Pb4 77.9(12) . . ? C88 C87 Pb4 77.3(12) . . ? C89 C88 C87 102.6(17) . . ? C89 C88 Si8 129.9(17) . . ? C87 C88 Si8 126.3(17) . . ? C89 C88 Pb4 78.5(12) . . ? C87 C88 Pb4 73.0(12) . . ? Si8 C88 Pb4 122.0(9) . . ? C94 C89 C88 111.6(18) . . ? C94 C89 C90 117.7(19) . . ? C88 C89 C90 130.4(19) . . ? C91 C90 C89 121.7(19) . . ? C90 C91 C92 120.3(17) . . ? C93 C92 C91 119.7(18) . . ? C94 C93 C92 121.1(19) . . ? C93 C94 C86 134.6(17) . . ? C93 C94 C89 119.4(19) . . ? C86 C94 C89 105.9(17) . . ? C21 Si1 C22 109.7(12) . . ? C21 Si1 C11 109.5(10) . . ? C22 Si1 C11 108.9(9) . . ? C21 Si1 C20 110.1(12) . . ? C22 Si1 C20 106.9(10) . . ? C11 Si1 C20 111.8(9) . . ? C18 Si2 C24 108.6(10) . . ? C18 Si2 C23 112.9(9) . . ? C24 Si2 C23 107.5(11) . . ? C18 Si2 C25 108.9(9) . . ? C24 Si2 C25 109.1(11) . . ? C23 Si2 C25 109.9(11) . . ? C36 Si3 C47 108.4(10) . . ? C36 Si3 C46 111.0(9) . . ? C47 Si3 C46 106.3(11) . . ? C36 Si3 C45 112.8(10) . . ? C47 Si3 C45 111.5(11) . . ? C46 Si3 C45 106.7(10) . . ? C50 Si4 C49 107.1(12) . . ? C50 Si4 C43 110.0(10) . . ? C49 Si4 C43 109.1(10) . . ? C50 Si4 C48 111.2(12) . . ? C49 Si4 C48 111.3(12) . . ? C43 Si4 C48 108.2(10) . . ? C70 Si5 C72 106.4(10) . . ? C70 Si5 C71 112.1(11) . . ? C72 Si5 C71 108.9(12) . . ? C70 Si5 C68 108.7(9) . . ? C72 Si5 C68 110.7(9) . . ? C71 Si5 C68 110.1(9) . . ? C61 Si6 C74 111.4(9) . . ? C61 Si6 C73 110.8(9) . . ? C74 Si6 C73 108.3(11) . . ? C61 Si6 C75 107.2(9) . . ? C74 Si6 C75 109.2(10) . . ? C73 Si6 C75 109.9(10) . . ? C96 Si7 C95 106.4(10) . . ? C96 Si7 C86 111.5(10) . . ? C95 Si7 C86 109.9(9) . . ? C96 Si7 C97 112.2(11) . . ? C95 Si7 C97 107.4(11) . . ? C86 Si7 C97 109.3(9) . . ? C88 Si8 C100 111.1(11) . . ? C88 Si8 C98 109.1(10) . . ? C100 Si8 C98 109.4(11) . . ? C88 Si8 C99 110.4(11) . . ? C100 Si8 C99 110.5(11) . . ? C98 Si8 C99 106.2(11) . . ? C2 Pb1 C1 31.7(7) . . ? C2 Pb1 C5 49.7(7) . . ? C1 Pb1 C5 30.6(7) . . ? C2 Pb1 C3 28.7(7) . . ? C1 Pb1 C3 50.4(8) . . ? C5 Pb1 C3 49.2(7) . . ? C2 Pb1 C19 101.7(7) . . ? C1 Pb1 C19 104.2(7) . . ? C5 Pb1 C19 133.0(7) . . ? C3 Pb1 C19 124.6(7) . . ? C2 Pb1 C4 48.2(8) . . ? C1 Pb1 C4 49.9(8) . . ? C5 Pb1 C4 29.5(7) . . ? C3 Pb1 C4 29.4(7) . . ? C19 Pb1 C4 149.8(7) . . ? C2 Pb1 C11 107.8(6) . . ? C1 Pb1 C11 124.0(6) . . ? C5 Pb1 C11 154.5(6) . . ? C3 Pb1 C11 118.7(6) . . ? C19 Pb1 C11 28.3(5) . . ? C4 Pb1 C11 147.6(6) . . ? C26 Pb2 C27 32.4(9) . . ? C26 Pb2 C30 32.0(7) . . ? C27 Pb2 C30 52.0(7) . . ? C26 Pb2 C28 50.1(7) . . ? C27 Pb2 C28 28.5(7) . . ? C30 Pb2 C28 50.1(6) . . ? C26 Pb2 C44 100.4(7) . . ? C27 Pb2 C44 98.9(7) . . ? C30 Pb2 C44 129.8(6) . . ? C28 Pb2 C44 123.3(6) . . ? C26 Pb2 C29 50.7(6) . . ? C27 Pb2 C29 49.1(6) . . ? C30 Pb2 C29 30.6(6) . . ? C28 Pb2 C29 29.3(6) . . ? C44 Pb2 C29 147.6(6) . . ? C26 Pb2 C43 122.0(8) . . ? C27 Pb2 C43 106.1(6) . . ? C30 Pb2 C43 153.9(6) . . ? C28 Pb2 C43 119.0(6) . . ? C44 Pb2 C43 29.6(5) . . ? C29 Pb2 C43 147.9(6) . . ? C52 Pb3 C53 30.3(6) . . ? C52 Pb3 C54 50.0(6) . . ? C53 Pb3 C54 30.7(6) . . ? C52 Pb3 C69 104.0(7) . . ? C53 Pb3 C69 98.4(6) . . ? C54 Pb3 C69 122.2(6) . . ? C52 Pb3 C51 30.0(7) . . ? C53 Pb3 C51 49.5(6) . . ? C54 Pb3 C51 49.0(6) . . ? C69 Pb3 C51 132.7(7) . . ? C52 Pb3 C55 48.8(7) . . ? C53 Pb3 C55 49.1(6) . . ? C54 Pb3 C55 29.5(6) . . ? C69 Pb3 C55 147.6(6) . . ? C51 Pb3 C55 28.9(7) . . ? C52 Pb3 C61 108.9(6) . . ? C53 Pb3 C61 117.6(6) . . ? C54 Pb3 C61 147.0(6) . . ? C69 Pb3 C61 29.1(5) . . ? C51 Pb3 C61 127.8(7) . . ? C55 Pb3 C61 156.2(6) . . ? C78 Pb4 C77 31.8(6) . . ? C78 Pb4 C76 50.5(6) . . ? C77 Pb4 C76 30.6(6) . . ? C78 Pb4 C79 31.3(6) . . ? C77 Pb4 C79 52.2(6) . . ? C76 Pb4 C79 50.3(6) . . ? C78 Pb4 C80 51.0(6) . . ? C77 Pb4 C80 51.2(6) . . ? C76 Pb4 C80 30.0(6) . . ? C79 Pb4 C80 30.7(6) . . ? C78 Pb4 C87 101.9(6) . . ? C77 Pb4 C87 97.0(6) . . ? C76 Pb4 C87 122.2(6) . . ? C79 Pb4 C87 131.2(6) . . ? C80 Pb4 C87 148.2(6) . . ? C78 Pb4 C88 123.2(7) . . ? C77 Pb4 C88 104.8(6) . . ? C76 Pb4 C88 117.1(6) . . ? C79 Pb4 C88 154.4(6) . . ? C80 Pb4 C88 146.3(6) . . ? C87 Pb4 C88 29.7(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.883 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.245 data_pna21 _database_code_depnum_ccdc_archive 'CCDC 244714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H38 Ge0 Li O2 Si2' _chemical_formula_weight 409.65 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 15.226(5) _cell_length_b 10.237(5) _cell_length_c 16.111(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 2511.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 30.19 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16418 _diffrn_reflns_av_R_equivalents 0.1423 _diffrn_reflns_av_sigmaI/netI 0.1410 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.37 _reflns_number_total 5206 _reflns_number_gt 3058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(16) _refine_ls_number_reflns 5206 _refine_ls_number_parameters 318 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.091 _refine_ls_shift/su_mean 0.012 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 C01 C 0.3744(2) 0.0689(4) 0.6443(3) 0.0264(10) Uani 1 1 d . . . C02 C 0.3749(2) 0.2121(4) 0.5308(2) 0.0256(9) Uani 1 1 d . . . C7 C 0.3865(2) 0.2814(4) 0.6057(3) 0.0258(9) Uani 1 1 d . . . C8 C 0.3701(3) -0.0539(4) 0.6839(3) 0.0363(11) Uani 1 1 d . . . H8 H 0.3734 -0.0596 0.7427 0.044 Uiso 1 1 calc R . . C9 C 0.1307(3) 0.0150(5) 0.5198(3) 0.0429(12) Uani 1 1 d . . . C10 C 0.1015(4) 0.5305(5) 0.5713(3) 0.0538(14) Uani 1 1 d . . . C11 C 0.1040(3) 0.3828(5) 0.5758(4) 0.0449(13) Uani 1 1 d . . . C12 C 0.3694(3) 0.0774(4) 0.5554(2) 0.0264(10) Uani 1 1 d . . . C13 C 0.3611(3) -0.1654(4) 0.6368(3) 0.0407(11) Uani 1 1 d . . . H13 H 0.3581 -0.2482 0.6633 0.049 Uiso 1 1 calc R . . C14 C 0.3562(3) -0.1572(5) 0.5490(3) 0.0402(12) Uani 1 1 d . . . C15 C 0.0559(4) -0.0887(5) 0.6287(3) 0.0470(13) Uani 1 1 d . . . C16 C 0.1296(4) 0.5653(5) 0.6584(3) 0.0599(16) Uani 1 1 d . . . H16A H 0.1538 0.6550 0.6606 0.072 Uiso 1 1 calc R . . H16B H 0.0796 0.5588 0.6975 0.072 Uiso 1 1 calc R . . C17 C 0.0972(4) -0.1175(5) 0.5447(3) 0.0428(12) Uani 1 1 d . . . C18 C 0.3598(3) -0.0396(4) 0.5099(3) 0.0331(10) Uani 1 1 d . . . H18 H 0.3558 -0.0361 0.4511 0.040 Uiso 1 1 calc R . . C19 C 0.1187(4) 0.0065(7) 0.6658(4) 0.0597(16) Uani 1 1 d . . . C20 C 0.4079(3) 0.4302(4) 0.7956(3) 0.0356(10) Uani 1 1 d . . . H20A H 0.4534 0.4623 0.7577 0.053 Uiso 1 1 calc R . . H20B H 0.4235 0.4533 0.8528 0.053 Uiso 1 1 calc R . . H20C H 0.3514 0.4701 0.7813 0.053 Uiso 1 1 calc R . . C21 C 0.1977(3) 0.4675(4) 0.6781(3) 0.0554(14) Uani 1 1 d . . . H21A H 0.2566 0.5008 0.6627 0.067 Uiso 1 1 calc R . . H21B H 0.1975 0.4472 0.7381 0.067 Uiso 1 1 calc R . . C22 C 0.3850(2) 0.2006(4) 0.6772(2) 0.0283(10) Uani 1 1 d . . . C23 C 0.3049(4) 0.1915(6) 0.8501(3) 0.0619(16) Uani 1 1 d . . . H23A H 0.2510 0.2343 0.8310 0.093 Uiso 1 1 calc R . . H23B H 0.3153 0.2135 0.9084 0.093 Uiso 1 1 calc R . . H23C H 0.2987 0.0966 0.8444 0.093 Uiso 1 1 calc R . . C24 C 0.3739(3) 0.4661(4) 0.4354(3) 0.0422(12) Uani 1 1 d . . . H24A H 0.3210 0.4934 0.4654 0.063 Uiso 1 1 calc R . . H24B H 0.3738 0.5053 0.3799 0.063 Uiso 1 1 calc R . . H24C H 0.4261 0.4952 0.4658 0.063 Uiso 1 1 calc R . . C25 C 0.2766(3) 0.2327(4) 0.3638(3) 0.0489(13) Uani 1 1 d . . . H25A H 0.2779 0.1382 0.3545 0.073 Uiso 1 1 calc R . . H25B H 0.2773 0.2781 0.3102 0.073 Uiso 1 1 calc R . . H25C H 0.2232 0.2561 0.3942 0.073 Uiso 1 1 calc R . . C26 C 0.4751(4) 0.2319(6) 0.3676(3) 0.0432(13) Uani 1 1 d . . . C27 C 0.5030(3) 0.1777(5) 0.8290(3) 0.0566(14) Uani 1 1 d . . . H27A H 0.5000 0.0822 0.8266 0.085 Uiso 1 1 calc R . . H27B H 0.5103 0.2056 0.8868 0.085 Uiso 1 1 calc R . . H27C H 0.5530 0.2084 0.7961 0.085 Uiso 1 1 calc R . . Si Si 0.39923(7) 0.24854(11) 0.78622(7) 0.0294(3) Uani 1 1 d . . . Si2 Si 0.37533(7) 0.28233(12) 0.42581(6) 0.0314(3) Uani 1 1 d . . . O1 O 0.15868(17) 0.0759(2) 0.5967(2) 0.0388(7) Uani 1 1 d . . . O2 O 0.17653(19) 0.3530(3) 0.63043(19) 0.0479(9) Uani 1 1 d . . . Li1 Li 0.2492(4) 0.2022(7) 0.6117(4) 0.0352(16) Uiso 1 1 d . . . H11 H 0.116(3) 0.351(5) 0.516(4) 0.067(16) Uiso 1 1 d . . . H26 H 0.179(3) 0.011(5) 0.475(3) 0.063(15) Uiso 1 1 d . . . H60 H 0.177(4) -0.007(5) 0.691(3) 0.073(17) Uiso 1 1 d . . . H61 H 0.100(3) 0.061(4) 0.703(3) 0.042(14) Uiso 1 1 d . . . H62 H 0.050(3) 0.335(4) 0.596(3) 0.069(15) Uiso 1 1 d . . . H63 H 0.348(3) -0.237(5) 0.520(3) 0.059(14) Uiso 1 1 d . . . H64 H -0.004(4) -0.042(5) 0.610(3) 0.080(16) Uiso 1 1 d . . . H65 H 0.048(4) -0.147(5) 0.512(4) 0.10(2) Uiso 1 1 d . . . H68 H 0.391(2) 0.385(3) 0.614(2) 0.024(9) Uiso 1 1 d . . . H70 H 0.050(3) -0.162(4) 0.659(3) 0.043(13) Uiso 1 1 d . . . H72 H 0.044(3) 0.555(4) 0.563(3) 0.047(14) Uiso 1 1 d . . . H90 H 0.143(4) -0.199(7) 0.542(4) 0.11(2) Uiso 1 1 d . . . H91 H 0.076(3) 0.081(4) 0.501(3) 0.057(14) Uiso 1 1 d . . . H94 H 0.527(3) 0.257(4) 0.396(3) 0.038(12) Uiso 1 1 d . . . H95 H 0.481(4) 0.136(6) 0.364(3) 0.08(2) Uiso 1 1 d . . . H96 H 0.476(3) 0.253(4) 0.321(3) 0.037(14) Uiso 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 C01 0.024(2) 0.024(2) 0.031(2) 0.0032(19) -0.0031(17) 0.0038(17) C02 0.025(2) 0.030(2) 0.022(2) 0.0006(18) -0.0005(16) 0.0020(17) C7 0.021(2) 0.031(2) 0.0249(18) -0.002(2) -0.0024(16) 0.0006(17) C8 0.034(3) 0.037(3) 0.038(3) 0.005(2) -0.003(2) 0.001(2) C9 0.042(3) 0.046(3) 0.040(3) 0.001(3) -0.010(3) -0.013(2) C10 0.043(3) 0.051(3) 0.067(4) 0.002(3) -0.019(3) 0.000(3) C11 0.033(3) 0.040(3) 0.062(4) -0.003(3) -0.013(2) 0.004(2) C12 0.026(2) 0.028(2) 0.026(2) -0.0042(19) 0.0009(16) 0.0005(18) C13 0.037(3) 0.026(2) 0.059(3) 0.003(2) 0.002(2) 0.0052(19) C14 0.041(3) 0.027(3) 0.052(3) -0.010(2) 0.001(2) 0.001(2) C15 0.061(4) 0.022(3) 0.059(3) 0.004(2) 0.011(3) 0.001(2) C16 0.078(4) 0.035(3) 0.067(4) -0.010(3) -0.010(3) 0.016(3) C17 0.053(3) 0.033(3) 0.043(3) 0.000(2) 0.002(2) -0.009(3) C18 0.030(3) 0.035(3) 0.035(2) -0.006(2) 0.0019(19) 0.0019(19) C19 0.049(4) 0.092(5) 0.038(3) -0.013(3) 0.010(3) -0.023(3) C20 0.037(3) 0.039(3) 0.031(2) -0.003(2) 0.000(2) -0.0021(19) C21 0.056(3) 0.037(3) 0.073(4) -0.021(2) -0.021(3) 0.011(2) C22 0.024(2) 0.036(3) 0.024(2) 0.002(2) -0.0022(16) 0.0006(18) C23 0.071(4) 0.083(4) 0.031(3) -0.005(3) 0.011(3) -0.032(3) C24 0.044(3) 0.038(3) 0.045(3) 0.009(2) -0.005(2) 0.005(2) C25 0.053(3) 0.068(4) 0.026(2) 0.000(2) -0.011(2) -0.017(3) C26 0.051(4) 0.053(4) 0.026(3) -0.003(3) 0.007(2) 0.004(3) C27 0.067(4) 0.051(3) 0.052(3) -0.009(3) -0.028(3) 0.010(3) Si 0.0356(6) 0.0329(6) 0.0197(5) 0.0013(5) -0.0022(5) -0.0038(5) Si2 0.0327(6) 0.0410(7) 0.0205(5) 0.0006(6) -0.0020(5) -0.0028(5) O1 0.0380(17) 0.0367(16) 0.0416(17) -0.0043(15) -0.0014(16) -0.0079(13) O2 0.0373(19) 0.0370(18) 0.069(2) -0.0171(16) -0.0213(16) 0.0097(14) _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 C01 C8 1.411(5) . ? C01 C12 1.437(5) . ? C01 C22 1.457(6) . ? C01 Li1 2.402(7) . ? C02 C7 1.411(6) . ? C02 C12 1.438(6) . ? C02 Si2 1.838(4) . ? C02 Li1 2.318(7) . ? C7 C22 1.417(6) . ? C7 Li1 2.243(7) . ? C8 C13 1.377(6) . ? C9 O1 1.451(6) . ? C9 C17 1.503(7) . ? C10 C16 1.509(7) . ? C10 C11 1.514(7) . ? C11 O2 1.444(5) . ? C12 C18 1.411(6) . ? C12 Li1 2.408(8) . ? C13 C14 1.419(6) . ? C14 C18 1.360(6) . ? C15 C19 1.489(8) . ? C15 C17 1.522(7) . ? C16 C21 1.476(6) . ? C19 O1 1.454(6) . ? C20 Si 1.871(4) . ? C21 O2 1.438(5) . ? C22 Si 1.837(4) . ? C22 Li1 2.321(7) . ? C23 Si 1.861(5) . ? C24 Si2 1.888(4) . ? C25 Si2 1.875(4) . ? C26 Si2 1.858(5) . ? C27 Si 1.870(5) . ? O1 Li1 1.906(7) . ? O2 Li1 1.924(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 C01 C12 120.1(4) . . ? C8 C01 C22 131.6(4) . . ? C12 C01 C22 108.2(3) . . ? C8 C01 Li1 124.6(3) . . ? C12 C01 Li1 72.9(3) . . ? C22 C01 Li1 69.0(3) . . ? C7 C02 C12 104.7(3) . . ? C7 C02 Si2 126.2(3) . . ? C12 C02 Si2 129.0(3) . . ? C7 C02 Li1 69.1(3) . . ? C12 C02 Li1 75.8(3) . . ? Si2 C02 Li1 122.5(3) . . ? C02 C7 C22 113.5(3) . . ? C02 C7 Li1 74.9(3) . . ? C22 C7 Li1 74.9(3) . . ? C13 C8 C01 119.6(4) . . ? O1 C9 C17 105.0(4) . . ? C16 C10 C11 100.6(4) . . ? O2 C11 C10 105.1(4) . . ? C18 C12 C01 118.1(4) . . ? C18 C12 C02 132.6(4) . . ? C01 C12 C02 109.2(3) . . ? C18 C12 Li1 124.6(3) . . ? C01 C12 Li1 72.4(3) . . ? C02 C12 Li1 68.9(3) . . ? C8 C13 C14 120.3(4) . . ? C18 C14 C13 120.8(4) . . ? C19 C15 C17 102.6(4) . . ? C21 C16 C10 103.8(4) . . ? C9 C17 C15 101.7(4) . . ? C14 C18 C12 121.0(4) . . ? O1 C19 C15 106.3(4) . . ? O2 C21 C16 106.2(4) . . ? C7 C22 C01 104.3(3) . . ? C7 C22 Si 128.2(3) . . ? C01 C22 Si 127.5(3) . . ? C7 C22 Li1 69.0(3) . . ? C01 C22 Li1 75.1(3) . . ? Si C22 Li1 122.5(3) . . ? C22 Si C23 110.7(2) . . ? C22 Si C27 110.4(2) . . ? C23 Si C27 109.1(3) . . ? C22 Si C20 110.6(2) . . ? C23 Si C20 108.8(2) . . ? C27 Si C20 107.2(2) . . ? C02 Si2 C26 111.0(2) . . ? C02 Si2 C25 112.5(2) . . ? C26 Si2 C25 108.1(3) . . ? C02 Si2 C24 108.3(2) . . ? C26 Si2 C24 109.1(2) . . ? C25 Si2 C24 107.7(2) . . ? C9 O1 C19 108.7(3) . . ? C9 O1 Li1 127.8(3) . . ? C19 O1 Li1 122.5(4) . . ? C21 O2 C11 109.0(3) . . ? C21 O2 Li1 127.5(3) . . ? C11 O2 Li1 120.9(3) . . ? O1 Li1 O2 98.5(3) . . ? O1 Li1 C7 156.0(4) . . ? O2 Li1 C7 104.6(3) . . ? O1 Li1 C02 123.8(4) . . ? O2 Li1 C02 121.9(4) . . ? C7 Li1 C02 36.01(18) . . ? O1 Li1 C22 134.2(4) . . ? O2 Li1 C22 116.5(3) . . ? C7 Li1 C22 36.14(18) . . ? C02 Li1 C22 61.3(2) . . ? O1 Li1 C01 102.5(3) . . ? O2 Li1 C01 151.4(4) . . ? C7 Li1 C01 58.4(2) . . ? C02 Li1 C01 59.5(2) . . ? C22 Li1 C01 35.90(17) . . ? O1 Li1 C12 98.2(3) . . ? O2 Li1 C12 157.2(4) . . ? C7 Li1 C12 57.9(2) . . ? C02 Li1 C12 35.35(17) . . ? C22 Li1 C12 59.4(2) . . ? C01 Li1 C12 34.76(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.332 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.062