# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Mitsuo Kira' 'Takashi Abe' 'Takeaki Iwamoto' 'Chizuko Kabuto' _publ_contact_author_name 'Mitsuo Kira' _publ_contact_author_address ; Department of Chemistry Tohoku University Graduate School of Science Aoba-ku Sendai 980-8578 JAPAN ; _publ_contact_author_email MKIRA@SI.CHEM.TOHOKU.AC.JP _publ_contact_author_fax +81-22-795-6589 _publ_contact_author_phone +81-22-795-6585 _publ_requested_journal 'Chemical Communications' _publ_section_title ; A Missing Group-14 Element Trimetallaallene. 2-Germadisilaallene ; data_2-germadisilaallene_crystalA_223K _database_code_depnum_ccdc_archive 'CCDC 279203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C32 H80 Ge Si10 ' _chemical_formula_moiety 'C32 H80 Ge Si10 ' _chemical_formula_weight 818.45 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.783(3) _cell_length_b 12.317(2) _cell_length_c 18.638(4) _cell_angle_alpha 73.548(8) _cell_angle_beta 87.246(10) _cell_angle_gamma 72.204(8) _cell_volume 2467.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5210 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 55.0 _exptl_crystal_description prism _exptl_crystal_colour dark_green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.7775 _exptl_absorpt_correction_T_max 0.9169 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20066 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1106 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10288 _reflns_number_gt 6830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+1.6489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10288 _refine_ls_number_parameters 443 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1362 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.1921 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1A Ge 0.85216(8) 0.79657(10) 0.75344(5) 0.0490(3) Uani 0.6123(18) 1 d PU . . Ge1B Ge 0.7710(3) 0.8463(3) 0.71158(18) 0.0501(9) Uani 0.1703(16) 1 d PU . . Ge1C Ge 0.7280(10) 0.7659(11) 0.7331(6) 0.0477(14) Uani 0.0492(13) 1 d PU . . Ge1D Ge 0.8177(3) 0.7178(3) 0.77685(18) 0.0529(10) Uani 0.1682(16) 1 d PU . . Si1 Si 0.88185(12) 0.68954(12) 0.67192(7) 0.0423(3) Uani 1 1 d U . . Si2 Si 0.69487(12) 0.87297(13) 0.81478(7) 0.0450(3) Uani 1 1 d U . . Si3 Si 1.05664(14) 0.42892(13) 0.74036(9) 0.0539(4) Uani 1 1 d . . . Si4 Si 1.15598(14) 0.64652(14) 0.69906(9) 0.0573(4) Uani 1 1 d . . . Si5 Si 0.67958(12) 0.67794(14) 0.57592(8) 0.0514(4) Uani 1 1 d . . . Si6 Si 0.82691(12) 0.85250(13) 0.50058(8) 0.0480(4) Uani 1 1 d . . . Si7 Si 0.83050(17) 1.01503(18) 0.88429(11) 0.0761(5) Uani 1 1 d . . . Si8 Si 0.65083(14) 1.14312(14) 0.74598(9) 0.0565(4) Uani 1 1 d . . . Si9 Si 0.66688(15) 0.66200(14) 0.94977(9) 0.0603(4) Uani 1 1 d . . . Si10 Si 0.44058(14) 0.83281(15) 0.85020(9) 0.0608(4) Uani 1 1 d . . . C1 C 1.0380(4) 0.5838(4) 0.6752(2) 0.0401(10) Uani 1 1 d . . . C2 C 1.0504(4) 0.5791(4) 0.5913(3) 0.0470(12) Uani 1 1 d . . . H1 H 1.0860 0.6398 0.5629 0.056 Uiso 1 1 calc R . . H2 H 1.1037 0.5012 0.5898 0.056 Uiso 1 1 calc R . . C3 C 0.9290(4) 0.6005(4) 0.5550(3) 0.0430(11) Uani 1 1 d . . . H3 H 0.9053 0.5280 0.5728 0.052 Uiso 1 1 calc R . . H4 H 0.9359 0.6176 0.5006 0.052 Uiso 1 1 calc R . . C4 C 0.8298(4) 0.7064(4) 0.5733(2) 0.0392(10) Uani 1 1 d . . . C5 C 0.6931(4) 1.0150(4) 0.8355(3) 0.0458(12) Uani 1 1 d . . . C6 C 0.5843(5) 1.0301(5) 0.8883(3) 0.0631(16) Uani 1 1 d . . . H5 H 0.5931 1.0773 0.9209 0.076 Uiso 1 1 calc R . . H6 H 0.5102 1.0730 0.8578 0.076 Uiso 1 1 calc R . . C7 C 0.5767(6) 0.9099(5) 0.9363(3) 0.0645(16) Uani 1 1 d . . . H7 H 0.4990 0.9207 0.9594 0.077 Uiso 1 1 calc R . . H8 H 0.6386 0.8773 0.9766 0.077 Uiso 1 1 calc R . . C8 C 0.5928(4) 0.8193(4) 0.8891(2) 0.0444(11) Uani 1 1 d . . . C9 C 1.2164(6) 0.3377(6) 0.7585(5) 0.102(3) Uani 1 1 d . . . H9 H 1.2216 0.2576 0.7883 0.153 Uiso 1 1 calc R . . H10 H 1.2570 0.3729 0.7854 0.153 Uiso 1 1 calc R . . H11 H 1.2539 0.3351 0.7113 0.153 Uiso 1 1 calc R . . C10 C 0.9866(7) 0.4303(6) 0.8317(3) 0.091(2) Uani 1 1 d . . . H12 H 0.9006 0.4621 0.8239 0.137 Uiso 1 1 calc R . . H13 H 1.0152 0.4797 0.8542 0.137 Uiso 1 1 calc R . . H14 H 1.0076 0.3499 0.8648 0.137 Uiso 1 1 calc R . . C11 C 0.9907(5) 0.3397(5) 0.6985(3) 0.0713(17) Uani 1 1 d . . . H15 H 1.0086 0.2595 0.7316 0.107 Uiso 1 1 calc R . . H16 H 1.0244 0.3374 0.6503 0.107 Uiso 1 1 calc R . . H17 H 0.9049 0.3760 0.6921 0.107 Uiso 1 1 calc R . . C12 C 1.3031(5) 0.5781(6) 0.6612(5) 0.097(2) Uani 1 1 d . . . H18 H 1.2972 0.6038 0.6069 0.146 Uiso 1 1 calc R . . H19 H 1.3234 0.4922 0.6785 0.146 Uiso 1 1 calc R . . H20 H 1.3647 0.6031 0.6786 0.146 Uiso 1 1 calc R . . C13 C 1.1239(5) 0.8090(5) 0.6563(3) 0.0663(16) Uani 1 1 d . . . H21 H 1.1257 0.8260 0.6023 0.100 Uiso 1 1 calc R . . H22 H 1.1838 0.8356 0.6742 0.100 Uiso 1 1 calc R . . H23 H 1.0457 0.8503 0.6702 0.100 Uiso 1 1 calc R . . C14 C 1.1731(7) 0.6202(6) 0.8024(3) 0.094(2) Uani 1 1 d . . . H24 H 1.2281 0.6594 0.8123 0.141 Uiso 1 1 calc R . . H25 H 1.2040 0.5356 0.8265 0.141 Uiso 1 1 calc R . . H26 H 1.0961 0.6521 0.8219 0.141 Uiso 1 1 calc R . . C15 C 0.6605(6) 0.6187(7) 0.4963(4) 0.086(2) Uani 1 1 d . . . H27 H 0.5812 0.6104 0.4964 0.129 Uiso 1 1 calc R . . H28 H 0.7196 0.5418 0.5022 0.129 Uiso 1 1 calc R . . H29 H 0.6707 0.6734 0.4493 0.129 Uiso 1 1 calc R . . C16 C 0.6678(5) 0.5598(5) 0.6619(3) 0.0683(16) Uani 1 1 d . . . H30 H 0.6861 0.5798 0.7058 0.103 Uiso 1 1 calc R . . H31 H 0.7238 0.4842 0.6604 0.103 Uiso 1 1 calc R . . H32 H 0.5873 0.5541 0.6641 0.103 Uiso 1 1 calc R . . C17 C 0.5538(5) 0.8139(6) 0.5730(4) 0.0767(19) Uani 1 1 d . . . H33 H 0.4799 0.7936 0.5813 0.115 Uiso 1 1 calc R . . H34 H 0.5485 0.8714 0.5244 0.115 Uiso 1 1 calc R . . H35 H 0.5671 0.8477 0.6117 0.115 Uiso 1 1 calc R . . C18 C 0.7617(6) 0.9844(5) 0.5360(3) 0.0701(17) Uani 1 1 d . . . H36 H 0.8145 0.9825 0.5750 0.105 Uiso 1 1 calc R . . H37 H 0.6846 0.9831 0.5562 0.105 Uiso 1 1 calc R . . H38 H 0.7521 1.0563 0.4952 0.105 Uiso 1 1 calc R . . C19 C 0.9793(5) 0.8539(5) 0.4664(3) 0.0650(15) Uani 1 1 d . . . H39 H 0.9725 0.9263 0.4265 0.097 Uiso 1 1 calc R . . H40 H 1.0149 0.7857 0.4477 0.097 Uiso 1 1 calc R . . H41 H 1.0292 0.8506 0.5074 0.097 Uiso 1 1 calc R . . C20 C 0.7406(6) 0.8750(6) 0.4126(3) 0.0776(19) Uani 1 1 d . . . H42 H 0.6581 0.8809 0.4240 0.116 Uiso 1 1 calc R . . H43 H 0.7749 0.8081 0.3924 0.116 Uiso 1 1 calc R . . H44 H 0.7442 0.9475 0.3761 0.116 Uiso 1 1 calc R . . C21 C 0.9731(6) 0.9536(9) 0.8420(6) 0.144(4) Uani 1 1 d . . . H45 H 0.9676 0.9927 0.7887 0.216 Uiso 1 1 calc R . . H46 H 0.9883 0.8689 0.8502 0.216 Uiso 1 1 calc R . . H47 H 1.0377 0.9669 0.8652 0.216 Uiso 1 1 calc R . . C22 C 0.8250(7) 1.1671(6) 0.8847(4) 0.093(2) Uani 1 1 d . . . H48 H 0.8929 1.1628 0.9141 0.140 Uiso 1 1 calc R . . H49 H 0.7518 1.2031 0.9065 0.140 Uiso 1 1 calc R . . H50 H 0.8276 1.2150 0.8338 0.140 Uiso 1 1 calc R . . C23 C 0.8406(10) 0.9336(9) 0.9863(4) 0.156(5) Uani 1 1 d . . . H51 H 0.8886 0.9621 1.0131 0.234 Uiso 1 1 calc R . . H52 H 0.8773 0.8491 0.9930 0.234 Uiso 1 1 calc R . . H53 H 0.7612 0.9472 1.0058 0.234 Uiso 1 1 calc R . . C24 C 0.7819(6) 1.1564(7) 0.6877(3) 0.084(2) Uani 1 1 d . . . H54 H 0.7557 1.2212 0.6422 0.126 Uiso 1 1 calc R . . H55 H 0.8188 1.0828 0.6749 0.126 Uiso 1 1 calc R . . H56 H 0.8393 1.1723 0.7157 0.126 Uiso 1 1 calc R . . C25 C 0.5404(5) 1.1269(6) 0.6839(3) 0.0753(18) Uani 1 1 d . . . H57 H 0.4647 1.1345 0.7080 0.113 Uiso 1 1 calc R . . H58 H 0.5697 1.0495 0.6749 0.113 Uiso 1 1 calc R . . H59 H 0.5296 1.1884 0.6366 0.113 Uiso 1 1 calc R . . C26 C 0.5758(6) 1.2870(6) 0.7679(4) 0.090(2) Uani 1 1 d . . . H60 H 0.6344 1.3118 0.7886 0.136 Uiso 1 1 calc R . . H61 H 0.5152 1.2765 0.8040 0.136 Uiso 1 1 calc R . . H62 H 0.5389 1.3472 0.7224 0.136 Uiso 1 1 calc R . . C27 C 0.6560(6) 0.5485(5) 0.9035(4) 0.088(2) Uani 1 1 d . . . H63 H 0.7041 0.4702 0.9323 0.132 Uiso 1 1 calc R . . H64 H 0.6848 0.5667 0.8532 0.132 Uiso 1 1 calc R . . H65 H 0.5735 0.5499 0.9012 0.132 Uiso 1 1 calc R . . C28 C 0.8293(5) 0.6308(6) 0.9723(3) 0.084(2) Uani 1 1 d . . . H66 H 0.8379 0.6806 1.0025 0.125 Uiso 1 1 calc R . . H67 H 0.8707 0.6479 0.9262 0.125 Uiso 1 1 calc R . . H68 H 0.8633 0.5479 0.9999 0.125 Uiso 1 1 calc R . . C29 C 0.5963(7) 0.6379(6) 1.0432(3) 0.092(2) Uani 1 1 d . . . H69 H 0.6316 0.5564 1.0730 0.139 Uiso 1 1 calc R . . H70 H 0.5113 0.6535 1.0358 0.139 Uiso 1 1 calc R . . H71 H 0.6097 0.6915 1.0689 0.139 Uiso 1 1 calc R . . C30 C 0.3538(5) 0.7546(6) 0.9216(3) 0.0735(17) Uani 1 1 d . . . H72 H 0.3496 0.7813 0.9662 0.110 Uiso 1 1 calc R . . H73 H 0.3930 0.6695 0.9344 0.110 Uiso 1 1 calc R . . H74 H 0.2738 0.7722 0.9014 0.110 Uiso 1 1 calc R . . C31 C 0.3395(6) 0.9891(6) 0.8208(5) 0.128(4) Uani 1 1 d . . . H75 H 0.2624 0.9899 0.8042 0.192 Uiso 1 1 calc R . . H76 H 0.3740 1.0361 0.7800 0.192 Uiso 1 1 calc R . . H77 H 0.3297 1.0225 0.8628 0.192 Uiso 1 1 calc R . . C32 C 0.4532(6) 0.7747(9) 0.7676(4) 0.119(3) Uani 1 1 d . . . H78 H 0.4987 0.6910 0.7819 0.178 Uiso 1 1 calc R . . H79 H 0.4935 0.8182 0.7286 0.178 Uiso 1 1 calc R . . H80 H 0.3742 0.7845 0.7490 0.178 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1A 0.0401(5) 0.0620(7) 0.0553(6) -0.0338(5) 0.0058(4) -0.0149(5) Ge1B 0.0585(18) 0.0445(16) 0.0454(16) -0.0193(13) 0.0071(13) -0.0076(13) Ge1C 0.049(3) 0.055(3) 0.044(3) -0.023(2) 0.006(2) -0.015(2) Ge1D 0.0564(18) 0.0514(17) 0.0443(16) -0.0152(13) 0.0067(13) -0.0063(14) Si1 0.0410(7) 0.0429(8) 0.0431(7) -0.0171(6) -0.0011(6) -0.0080(6) Si2 0.0426(8) 0.0498(8) 0.0458(8) -0.0204(6) 0.0062(6) -0.0130(6) Si3 0.0544(9) 0.0380(8) 0.0652(9) -0.0096(7) -0.0141(7) -0.0102(7) Si4 0.0481(9) 0.0510(9) 0.0751(10) -0.0161(8) -0.0176(7) -0.0171(7) Si5 0.0363(7) 0.0577(9) 0.0627(9) -0.0193(7) -0.0048(6) -0.0146(7) Si6 0.0443(8) 0.0500(8) 0.0457(8) -0.0087(6) -0.0044(6) -0.0121(7) Si7 0.0709(12) 0.0808(13) 0.0874(13) -0.0327(10) -0.0198(10) -0.0268(10) Si8 0.0497(9) 0.0531(9) 0.0667(10) -0.0118(7) 0.0069(7) -0.0209(7) Si9 0.0642(10) 0.0526(9) 0.0564(9) -0.0047(7) -0.0050(7) -0.0157(8) Si10 0.0435(8) 0.0706(11) 0.0626(10) -0.0078(8) 0.0050(7) -0.0200(8) C1 0.038(2) 0.038(3) 0.047(3) -0.019(2) -0.004(2) -0.008(2) C2 0.037(3) 0.047(3) 0.056(3) -0.020(2) -0.001(2) -0.006(2) C3 0.046(3) 0.045(3) 0.044(3) -0.023(2) 0.001(2) -0.013(2) C4 0.035(2) 0.041(3) 0.044(3) -0.019(2) -0.0002(19) -0.008(2) C5 0.044(3) 0.051(3) 0.050(3) -0.021(2) 0.006(2) -0.020(2) C6 0.077(4) 0.059(4) 0.064(3) -0.031(3) 0.031(3) -0.028(3) C7 0.088(4) 0.062(4) 0.058(3) -0.032(3) 0.028(3) -0.034(3) C8 0.055(3) 0.046(3) 0.036(2) -0.014(2) 0.006(2) -0.020(2) C9 0.075(5) 0.050(4) 0.162(7) -0.012(4) -0.045(5) -0.001(3) C10 0.146(7) 0.064(4) 0.053(4) 0.005(3) -0.009(4) -0.034(4) C11 0.075(4) 0.047(3) 0.096(5) -0.016(3) -0.012(3) -0.025(3) C12 0.042(3) 0.091(5) 0.168(7) -0.051(5) -0.008(4) -0.018(3) C13 0.071(4) 0.065(4) 0.074(4) -0.015(3) -0.008(3) -0.040(3) C14 0.124(6) 0.076(5) 0.087(5) -0.007(4) -0.057(4) -0.043(4) C15 0.067(4) 0.115(6) 0.097(5) -0.045(4) -0.011(4) -0.042(4) C16 0.054(3) 0.055(4) 0.098(5) -0.013(3) 0.000(3) -0.027(3) C17 0.039(3) 0.079(4) 0.092(4) -0.009(4) 0.004(3) -0.003(3) C18 0.075(4) 0.048(3) 0.076(4) -0.008(3) 0.006(3) -0.012(3) C19 0.061(4) 0.066(4) 0.066(4) -0.008(3) 0.005(3) -0.027(3) C20 0.076(4) 0.100(5) 0.051(3) -0.006(3) -0.016(3) -0.031(4) C21 0.044(4) 0.166(9) 0.250(11) -0.126(9) -0.032(5) -0.003(5) C22 0.100(6) 0.101(6) 0.110(5) -0.047(5) 0.000(4) -0.059(5) C23 0.230(12) 0.147(8) 0.108(6) 0.017(6) -0.097(7) -0.112(8) C24 0.085(5) 0.115(6) 0.073(4) -0.029(4) 0.027(4) -0.062(4) C25 0.057(4) 0.082(5) 0.073(4) 0.004(3) -0.016(3) -0.022(3) C26 0.093(5) 0.059(4) 0.114(6) -0.021(4) 0.007(4) -0.021(4) C27 0.093(5) 0.051(4) 0.121(6) -0.024(4) -0.005(4) -0.022(4) C28 0.073(4) 0.084(5) 0.073(4) -0.003(4) -0.023(3) -0.008(4) C29 0.104(6) 0.094(5) 0.063(4) 0.009(4) -0.001(4) -0.034(5) C30 0.061(4) 0.084(5) 0.084(4) -0.022(4) 0.010(3) -0.035(3) C31 0.049(4) 0.078(5) 0.208(9) 0.035(6) 0.001(5) -0.019(4) C32 0.077(5) 0.235(11) 0.082(5) -0.072(6) 0.010(4) -0.076(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1A Si2 2.2287(15) . ? Ge1A Si1 2.2294(15) . ? Ge1B Si2 2.150(3) . ? Ge1B Si1 2.271(3) . ? Ge1C Si1 2.199(10) . ? Ge1C Si2 2.231(10) . ? Ge1D Si1 2.145(3) . ? Ge1D Si2 2.285(4) . ? Si1 C1 1.894(5) . ? Si1 C4 1.899(4) . ? Si2 C5 1.889(5) . ? Si2 C8 1.900(5) . ? Si3 C10 1.858(6) . ? Si3 C9 1.864(6) . ? Si3 C11 1.866(6) . ? Si3 C1 1.902(5) . ? Si4 C13 1.856(6) . ? Si4 C14 1.871(6) . ? Si4 C12 1.882(6) . ? Si4 C1 1.907(5) . ? Si5 C17 1.856(6) . ? Si5 C16 1.867(6) . ? Si5 C15 1.878(6) . ? Si5 C4 1.903(5) . ? Si6 C18 1.860(6) . ? Si6 C20 1.879(5) . ? Si6 C19 1.880(5) . ? Si6 C4 1.914(5) . ? Si7 C21 1.857(8) . ? Si7 C22 1.857(7) . ? Si7 C23 1.872(8) . ? Si7 C5 1.895(5) . ? Si8 C24 1.867(6) . ? Si8 C26 1.872(6) . ? Si8 C25 1.872(6) . ? Si8 C5 1.905(5) . ? Si9 C27 1.875(6) . ? Si9 C28 1.877(6) . ? Si9 C29 1.878(6) . ? Si9 C8 1.901(5) . ? Si10 C32 1.856(7) . ? Si10 C31 1.868(7) . ? Si10 C30 1.869(6) . ? Si10 C8 1.909(5) . ? C1 C2 1.579(6) . ? C2 C3 1.528(6) . ? C2 H1 0.9800 . ? C2 H2 0.9800 . ? C3 C4 1.571(6) . ? C3 H3 0.9800 . ? C3 H4 0.9800 . ? C5 C6 1.576(6) . ? C6 C7 1.525(7) . ? C6 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.570(6) . ? C7 H7 0.9800 . ? C7 H8 0.9800 . ? C9 H9 0.9700 . ? C9 H10 0.9700 . ? C9 H11 0.9700 . ? C10 H12 0.9700 . ? C10 H13 0.9700 . ? C10 H14 0.9700 . ? C11 H15 0.9700 . ? C11 H16 0.9700 . ? C11 H17 0.9700 . ? C12 H18 0.9700 . ? C12 H19 0.9700 . ? C12 H20 0.9700 . ? C13 H21 0.9700 . ? C13 H22 0.9700 . ? C13 H23 0.9700 . ? C14 H24 0.9700 . ? C14 H25 0.9700 . ? C14 H26 0.9700 . ? C15 H27 0.9700 . ? C15 H28 0.9700 . ? C15 H29 0.9700 . ? C16 H30 0.9700 . ? C16 H31 0.9700 . ? C16 H32 0.9700 . ? C17 H33 0.9700 . ? C17 H34 0.9700 . ? C17 H35 0.9700 . ? C18 H36 0.9700 . ? C18 H37 0.9700 . ? C18 H38 0.9700 . ? C19 H39 0.9700 . ? C19 H40 0.9700 . ? C19 H41 0.9700 . ? C20 H42 0.9700 . ? C20 H43 0.9700 . ? C20 H44 0.9700 . ? C21 H45 0.9700 . ? C21 H46 0.9700 . ? C21 H47 0.9700 . ? C22 H48 0.9700 . ? C22 H49 0.9700 . ? C22 H50 0.9700 . ? C23 H51 0.9700 . ? C23 H52 0.9700 . ? C23 H53 0.9700 . ? C24 H54 0.9700 . ? C24 H55 0.9700 . ? C24 H56 0.9700 . ? C25 H57 0.9700 . ? C25 H58 0.9700 . ? C25 H59 0.9700 . ? C26 H60 0.9700 . ? C26 H61 0.9700 . ? C26 H62 0.9700 . ? C27 H63 0.9700 . ? C27 H64 0.9700 . ? C27 H65 0.9700 . ? C28 H66 0.9700 . ? C28 H67 0.9700 . ? C28 H68 0.9700 . ? C29 H69 0.9700 . ? C29 H70 0.9700 . ? C29 H71 0.9700 . ? C30 H72 0.9700 . ? C30 H73 0.9700 . ? C30 H74 0.9700 . ? C31 H75 0.9700 . ? C31 H76 0.9700 . ? C31 H77 0.9700 . ? C32 H78 0.9700 . ? C32 H79 0.9700 . ? C32 H80 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 Ge1A Si1 134.07(7) . . ? Si2 Ge1B Si1 136.39(17) . . ? Si1 Ge1C Si2 135.8(6) . . ? Si1 Ge1D Si2 135.78(18) . . ? C1 Si1 C4 100.16(19) . . ? C1 Si1 Ge1D 115.86(17) . . ? C4 Si1 Ge1D 142.37(18) . . ? C1 Si1 Ge1C 148.4(3) . . ? C4 Si1 Ge1C 109.2(3) . . ? C1 Si1 Ge1A 115.09(15) . . ? C4 Si1 Ge1A 138.71(15) . . ? C1 Si1 Ge1B 143.24(18) . . ? C4 Si1 Ge1B 109.89(17) . . ? C5 Si2 C8 100.4(2) . . ? C5 Si2 Ge1B 116.68(18) . . ? C8 Si2 Ge1B 141.21(19) . . ? C5 Si2 Ge1A 114.75(16) . . ? C8 Si2 Ge1A 138.77(16) . . ? C5 Si2 Ge1C 148.0(4) . . ? C8 Si2 Ge1C 109.6(3) . . ? C5 Si2 Ge1D 141.8(2) . . ? C8 Si2 Ge1D 110.57(19) . . ? C10 Si3 C9 108.6(4) . . ? C10 Si3 C11 106.7(3) . . ? C9 Si3 C11 103.3(3) . . ? C10 Si3 C1 113.2(2) . . ? C9 Si3 C1 112.2(3) . . ? C11 Si3 C1 112.3(2) . . ? C13 Si4 C14 106.3(3) . . ? C13 Si4 C12 104.7(3) . . ? C14 Si4 C12 110.0(4) . . ? C13 Si4 C1 114.1(2) . . ? C14 Si4 C1 111.5(3) . . ? C12 Si4 C1 110.0(3) . . ? C17 Si5 C16 107.8(3) . . ? C17 Si5 C15 109.7(3) . . ? C16 Si5 C15 104.5(3) . . ? C17 Si5 C4 111.9(3) . . ? C16 Si5 C4 111.8(2) . . ? C15 Si5 C4 110.7(2) . . ? C18 Si6 C20 108.2(3) . . ? C18 Si6 C19 108.2(3) . . ? C20 Si6 C19 103.1(3) . . ? C18 Si6 C4 112.7(2) . . ? C20 Si6 C4 111.6(3) . . ? C19 Si6 C4 112.5(2) . . ? C21 Si7 C22 106.4(4) . . ? C21 Si7 C23 108.7(5) . . ? C22 Si7 C23 103.0(4) . . ? C21 Si7 C5 114.3(3) . . ? C22 Si7 C5 111.9(3) . . ? C23 Si7 C5 111.9(3) . . ? C24 Si8 C26 109.7(3) . . ? C24 Si8 C25 105.9(3) . . ? C26 Si8 C25 105.0(3) . . ? C24 Si8 C5 112.5(3) . . ? C26 Si8 C5 110.8(3) . . ? C25 Si8 C5 112.7(2) . . ? C27 Si9 C28 107.0(3) . . ? C27 Si9 C29 110.0(3) . . ? C28 Si9 C29 104.8(3) . . ? C27 Si9 C8 111.5(3) . . ? C28 Si9 C8 113.5(3) . . ? C29 Si9 C8 109.8(3) . . ? C32 Si10 C31 106.9(4) . . ? C32 Si10 C30 108.5(3) . . ? C31 Si10 C30 103.1(3) . . ? C32 Si10 C8 112.1(3) . . ? C31 Si10 C8 113.2(3) . . ? C30 Si10 C8 112.5(2) . . ? C2 C1 Si1 101.5(3) . . ? C2 C1 Si3 110.0(3) . . ? Si1 C1 Si3 113.4(2) . . ? C2 C1 Si4 108.9(3) . . ? Si1 C1 Si4 112.0(2) . . ? Si3 C1 Si4 110.6(2) . . ? C3 C2 C1 111.1(4) . . ? C3 C2 H1 109.4 . . ? C1 C2 H1 109.4 . . ? C3 C2 H2 109.4 . . ? C1 C2 H2 109.4 . . ? H1 C2 H2 108.0 . . ? C2 C3 C4 112.3(4) . . ? C2 C3 H3 109.1 . . ? C4 C3 H3 109.1 . . ? C2 C3 H4 109.1 . . ? C4 C3 H4 109.1 . . ? H3 C3 H4 107.9 . . ? C3 C4 Si1 100.1(3) . . ? C3 C4 Si5 109.5(3) . . ? Si1 C4 Si5 109.7(2) . . ? C3 C4 Si6 109.8(3) . . ? Si1 C4 Si6 115.7(2) . . ? Si5 C4 Si6 111.4(2) . . ? C6 C5 Si2 100.2(3) . . ? C6 C5 Si7 110.0(3) . . ? Si2 C5 Si7 117.7(3) . . ? C6 C5 Si8 108.0(3) . . ? Si2 C5 Si8 109.3(2) . . ? Si7 C5 Si8 110.9(3) . . ? C7 C6 C5 111.3(4) . . ? C7 C6 H5 109.4 . . ? C5 C6 H5 109.4 . . ? C7 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? H5 C6 H6 108.0 . . ? C6 C7 C8 111.8(4) . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C6 C7 H8 109.3 . . ? C8 C7 H8 109.3 . . ? H7 C7 H8 107.9 . . ? C7 C8 Si2 100.6(3) . . ? C7 C8 Si9 110.0(3) . . ? Si2 C8 Si9 112.0(2) . . ? C7 C8 Si10 109.3(4) . . ? Si2 C8 Si10 113.9(2) . . ? Si9 C8 Si10 110.6(3) . . ? Si3 C9 H9 109.5 . . ? Si3 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? Si3 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? Si3 C10 H12 109.5 . . ? Si3 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? Si3 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? Si3 C11 H15 109.5 . . ? Si3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? Si3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? Si4 C12 H18 109.5 . . ? Si4 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? Si4 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? Si4 C13 H21 109.5 . . ? Si4 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? Si4 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? Si4 C14 H24 109.5 . . ? Si4 C14 H25 109.5 . . ? H24 C14 H25 109.5 . . ? Si4 C14 H26 109.5 . . ? H24 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? Si5 C15 H27 109.5 . . ? Si5 C15 H28 109.5 . . ? H27 C15 H28 109.5 . . ? Si5 C15 H29 109.5 . . ? H27 C15 H29 109.5 . . ? H28 C15 H29 109.5 . . ? Si5 C16 H30 109.5 . . ? Si5 C16 H31 109.5 . . ? H30 C16 H31 109.5 . . ? Si5 C16 H32 109.5 . . ? H30 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? Si5 C17 H33 109.5 . . ? Si5 C17 H34 109.5 . . ? H33 C17 H34 109.5 . . ? Si5 C17 H35 109.5 . . ? H33 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? Si6 C18 H36 109.5 . . ? Si6 C18 H37 109.5 . . ? H36 C18 H37 109.5 . . ? Si6 C18 H38 109.5 . . ? H36 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? Si6 C19 H39 109.5 . . ? Si6 C19 H40 109.5 . . ? H39 C19 H40 109.5 . . ? Si6 C19 H41 109.5 . . ? H39 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si6 C20 H42 109.5 . . ? Si6 C20 H43 109.5 . . ? H42 C20 H43 109.5 . . ? Si6 C20 H44 109.5 . . ? H42 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si7 C21 H45 109.5 . . ? Si7 C21 H46 109.5 . . ? H45 C21 H46 109.5 . . ? Si7 C21 H47 109.5 . . ? H45 C21 H47 109.5 . . ? H46 C21 H47 109.5 . . ? Si7 C22 H48 109.5 . . ? Si7 C22 H49 109.5 . . ? H48 C22 H49 109.5 . . ? Si7 C22 H50 109.5 . . ? H48 C22 H50 109.5 . . ? H49 C22 H50 109.5 . . ? Si7 C23 H51 109.5 . . ? Si7 C23 H52 109.5 . . ? H51 C23 H52 109.5 . . ? Si7 C23 H53 109.5 . . ? H51 C23 H53 109.5 . . ? H52 C23 H53 109.5 . . ? Si8 C24 H54 109.5 . . ? Si8 C24 H55 109.5 . . ? H54 C24 H55 109.5 . . ? Si8 C24 H56 109.5 . . ? H54 C24 H56 109.5 . . ? H55 C24 H56 109.5 . . ? Si8 C25 H57 109.5 . . ? Si8 C25 H58 109.5 . . ? H57 C25 H58 109.5 . . ? Si8 C25 H59 109.5 . . ? H57 C25 H59 109.5 . . ? H58 C25 H59 109.5 . . ? Si8 C26 H60 109.5 . . ? Si8 C26 H61 109.5 . . ? H60 C26 H61 109.5 . . ? Si8 C26 H62 109.5 . . ? H60 C26 H62 109.5 . . ? H61 C26 H62 109.5 . . ? Si9 C27 H63 109.5 . . ? Si9 C27 H64 109.5 . . ? H63 C27 H64 109.5 . . ? Si9 C27 H65 109.5 . . ? H63 C27 H65 109.5 . . ? H64 C27 H65 109.5 . . ? Si9 C28 H66 109.5 . . ? Si9 C28 H67 109.5 . . ? H66 C28 H67 109.5 . . ? Si9 C28 H68 109.5 . . ? H66 C28 H68 109.5 . . ? H67 C28 H68 109.5 . . ? Si9 C29 H69 109.5 . . ? Si9 C29 H70 109.5 . . ? H69 C29 H70 109.5 . . ? Si9 C29 H71 109.5 . . ? H69 C29 H71 109.5 . . ? H70 C29 H71 109.5 . . ? Si10 C30 H72 109.5 . . ? Si10 C30 H73 109.5 . . ? H72 C30 H73 109.5 . . ? Si10 C30 H74 109.5 . . ? H72 C30 H74 109.5 . . ? H73 C30 H74 109.5 . . ? Si10 C31 H75 109.5 . . ? Si10 C31 H76 109.5 . . ? H75 C31 H76 109.5 . . ? Si10 C31 H77 109.5 . . ? H75 C31 H77 109.5 . . ? H76 C31 H77 109.5 . . ? Si10 C32 H78 109.5 . . ? Si10 C32 H79 109.5 . . ? H78 C32 H79 109.5 . . ? Si10 C32 H80 109.5 . . ? H78 C32 H80 109.5 . . ? H79 C32 H80 109.5 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.361 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.064 data_2-germadisilaallene_crystalB_123K _database_code_depnum_ccdc_archive 'CCDC 279204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C32 H80 Ge Si10 ' _chemical_formula_moiety 'C32 H80 Ge Si10 ' _chemical_formula_weight 818.45 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.709(3) _cell_length_b 12.239(2) _cell_length_c 18.548(4) _cell_angle_alpha 73.464(7) _cell_angle_beta 87.139(8) _cell_angle_gamma 71.999(7) _cell_volume 2421.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7461 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 56.6 _exptl_crystal_description prism _exptl_crystal_colour dark_green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.7740 _exptl_absorpt_correction_T_max 0.9154 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38183 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11049 _reflns_number_gt 10357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+2.0351P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11049 _refine_ls_number_parameters 433 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1A Ge 0.35366(2) 0.79411(3) 0.254908(15) 0.02476(9) Uani 0.8776(10) 1 d PU . . Ge1B Ge 0.3209(3) 0.7137(3) 0.27886(18) 0.0294(9) Uani 0.0760(9) 1 d PU . . Ge1D Ge 0.2716(5) 0.8464(5) 0.2119(3) 0.0286(12) Uani 0.0464(8) 1 d PU . . Si1 Si 0.19117(5) 0.87427(5) 0.31323(3) 0.02074(12) Uani 1 1 d U . . Si2 Si 0.38356(5) 0.68496(5) 0.17364(3) 0.01911(12) Uani 1 1 d U . . Si3 Si 0.15424(6) 1.14387(6) 0.24626(4) 0.02807(14) Uani 1 1 d . . . Si4 Si 0.32178(6) 1.01346(7) 0.39241(4) 0.03726(17) Uani 1 1 d . . . Si5 Si -0.06076(6) 0.82363(6) 0.34580(4) 0.02831(14) Uani 1 1 d . . . Si6 Si 0.16731(6) 0.66041(6) 0.44964(4) 0.02906(15) Uani 1 1 d . . . Si7 Si 0.66151(5) 0.64370(6) 0.19723(4) 0.02593(14) Uani 1 1 d . . . Si8 Si 0.56274(6) 0.42460(5) 0.23946(4) 0.02547(14) Uani 1 1 d . . . Si9 Si 0.32587(5) 0.85459(5) 0.00218(3) 0.02241(13) Uani 1 1 d . . . Si10 Si 0.17742(5) 0.67920(5) 0.07683(3) 0.02334(13) Uani 1 1 d . . . C1 C 0.18779(19) 1.01576(19) 0.33729(12) 0.0227(4) Uani 1 1 d . . . C2 C 0.0725(2) 1.0326(2) 0.38572(13) 0.0285(5) Uani 1 1 d . . . H1 H 0.0764 1.0819 0.4191 0.034 Uiso 1 1 calc R . . H2 H 0.0000 1.0755 0.3519 0.034 Uiso 1 1 calc R . . C3 C 0.0631(2) 0.9107(2) 0.43369(13) 0.0288(5) Uani 1 1 d . . . H3 H -0.0184 0.9215 0.4536 0.035 Uiso 1 1 calc R . . H4 H 0.1216 0.8789 0.4771 0.035 Uiso 1 1 calc R . . C4 C 0.08842(19) 0.81789(19) 0.38679(12) 0.0221(4) Uani 1 1 d . . . C5 C 0.54190(18) 0.58139(18) 0.17341(12) 0.0197(4) Uani 1 1 d . . . C6 C 0.55188(18) 0.57783(19) 0.08958(12) 0.0224(4) Uani 1 1 d . . . H5 H 0.5875 0.6398 0.0604 0.027 Uiso 1 1 calc R . . H6 H 0.6059 0.4987 0.0874 0.027 Uiso 1 1 calc R . . C7 C 0.42787(18) 0.59999(19) 0.05392(12) 0.0223(4) Uani 1 1 d . . . H7 H 0.4039 0.5263 0.0720 0.027 Uiso 1 1 calc R . . H8 H 0.4332 0.6185 -0.0015 0.027 Uiso 1 1 calc R . . C8 C 0.32950(17) 0.70629(18) 0.07412(11) 0.0185(4) Uani 1 1 d . . . C9 C 0.0802(3) 1.2910(2) 0.26576(18) 0.0471(7) Uani 1 1 d . . . H9 H 0.1396 1.3142 0.2884 0.071 Uiso 1 1 calc R . . H10 H 0.0154 1.2836 0.3006 0.071 Uiso 1 1 calc R . . H11 H 0.0468 1.3521 0.2185 0.071 Uiso 1 1 calc R . . C10 C 0.0436(2) 1.1313(2) 0.18155(15) 0.0371(6) Uani 1 1 d . . . H12 H -0.0363 1.1486 0.2026 0.056 Uiso 1 1 calc R . . H13 H 0.0684 1.0500 0.1762 0.056 Uiso 1 1 calc R . . H14 H 0.0409 1.1890 0.1321 0.056 Uiso 1 1 calc R . . C11 C 0.2929(3) 1.1481(3) 0.19228(16) 0.0442(7) Uani 1 1 d . . . H15 H 0.2713 1.2108 0.1443 0.066 Uiso 1 1 calc R . . H16 H 0.3308 1.0703 0.1827 0.066 Uiso 1 1 calc R . . H17 H 0.3492 1.1652 0.2216 0.066 Uiso 1 1 calc R . . C12 C 0.3166(3) 0.9407(3) 0.49641(17) 0.0540(8) Uani 1 1 d . . . H18 H 0.3202 0.8570 0.5047 0.081 Uiso 1 1 calc R . . H19 H 0.2416 0.9834 0.5155 0.081 Uiso 1 1 calc R . . H20 H 0.3851 0.9441 0.5230 0.081 Uiso 1 1 calc R . . C13 C 0.3195(3) 1.1687(3) 0.38887(18) 0.0475(7) Uani 1 1 d . . . H21 H 0.3829 1.1642 0.4232 0.071 Uiso 1 1 calc R . . H22 H 0.2412 1.2118 0.4041 0.071 Uiso 1 1 calc R . . H23 H 0.3333 1.2112 0.3374 0.071 Uiso 1 1 calc R . . C14 C 0.4710(3) 0.9393(4) 0.3603(2) 0.0693(11) Uani 1 1 d . . . H24 H 0.4749 0.9742 0.3061 0.104 Uiso 1 1 calc R . . H25 H 0.4825 0.8534 0.3710 0.104 Uiso 1 1 calc R . . H26 H 0.5343 0.9513 0.3870 0.104 Uiso 1 1 calc R . . C15 C -0.1625(2) 0.9793(3) 0.30633(17) 0.0452(7) Uani 1 1 d . . . H27 H -0.2399 0.9766 0.2904 0.068 Uiso 1 1 calc R . . H28 H -0.1260 1.0212 0.2629 0.068 Uiso 1 1 calc R . . H29 H -0.1752 1.0219 0.3449 0.068 Uiso 1 1 calc R . . C16 C -0.1509(2) 0.7511(2) 0.41955(14) 0.0339(5) Uani 1 1 d . . . H30 H -0.1604 0.7863 0.4616 0.051 Uiso 1 1 calc R . . H31 H -0.1093 0.6649 0.4377 0.051 Uiso 1 1 calc R . . H32 H -0.2303 0.7641 0.3978 0.051 Uiso 1 1 calc R . . C17 C -0.0366(3) 0.7498(3) 0.26817(16) 0.0521(8) Uani 1 1 d . . . H33 H -0.1061 0.7868 0.2325 0.078 Uiso 1 1 calc R . . H34 H -0.0269 0.6642 0.2894 0.078 Uiso 1 1 calc R . . H35 H 0.0359 0.7596 0.2419 0.078 Uiso 1 1 calc R . . C18 C 0.0951(3) 0.6395(3) 0.54335(15) 0.0458(7) Uani 1 1 d . . . H36 H 0.0082 0.6582 0.5356 0.069 Uiso 1 1 calc R . . H37 H 0.1108 0.6931 0.5693 0.069 Uiso 1 1 calc R . . H38 H 0.1287 0.5562 0.5739 0.069 Uiso 1 1 calc R . . C19 C 0.1604(3) 0.5425(2) 0.40641(18) 0.0433(7) Uani 1 1 d . . . H39 H 0.1911 0.5586 0.3556 0.065 Uiso 1 1 calc R . . H40 H 0.0769 0.5429 0.4037 0.065 Uiso 1 1 calc R . . H41 H 0.2096 0.4639 0.4372 0.065 Uiso 1 1 calc R . . C20 C 0.3304(2) 0.6314(2) 0.47165(16) 0.0422(6) Uani 1 1 d . . . H42 H 0.3643 0.5495 0.5041 0.063 Uiso 1 1 calc R . . H43 H 0.3386 0.6883 0.4975 0.063 Uiso 1 1 calc R . . H44 H 0.3736 0.6414 0.4248 0.063 Uiso 1 1 calc R . . C21 C 0.6837(3) 0.6143(2) 0.30088(15) 0.0406(6) Uani 1 1 d . . . H45 H 0.7480 0.6446 0.3105 0.061 Uiso 1 1 calc R . . H46 H 0.7058 0.5279 0.3253 0.061 Uiso 1 1 calc R . . H47 H 0.6089 0.6549 0.3212 0.061 Uiso 1 1 calc R . . C22 C 0.6296(2) 0.8090(2) 0.15580(14) 0.0331(5) Uani 1 1 d . . . H48 H 0.5505 0.8509 0.1708 0.050 Uiso 1 1 calc R . . H49 H 0.6303 0.8280 0.1008 0.050 Uiso 1 1 calc R . . H50 H 0.6913 0.8346 0.1741 0.050 Uiso 1 1 calc R . . C23 C 0.8072(2) 0.5769(3) 0.1558(2) 0.0499(8) Uani 1 1 d . . . H51 H 0.7974 0.6022 0.1008 0.075 Uiso 1 1 calc R . . H52 H 0.8301 0.4893 0.1741 0.075 Uiso 1 1 calc R . . H53 H 0.8701 0.6043 0.1709 0.075 Uiso 1 1 calc R . . C24 C 0.4952(2) 0.3353(2) 0.19757(16) 0.0362(6) Uani 1 1 d . . . H54 H 0.5162 0.2526 0.2300 0.054 Uiso 1 1 calc R . . H55 H 0.5265 0.3357 0.1475 0.054 Uiso 1 1 calc R . . H56 H 0.4076 0.3707 0.1932 0.054 Uiso 1 1 calc R . . C25 C 0.4941(3) 0.4254(2) 0.33215(15) 0.0440(7) Uani 1 1 d . . . H57 H 0.4063 0.4535 0.3253 0.066 Uiso 1 1 calc R . . H58 H 0.5200 0.4792 0.3533 0.066 Uiso 1 1 calc R . . H59 H 0.5198 0.3442 0.3666 0.066 Uiso 1 1 calc R . . C26 C 0.7251(2) 0.3324(2) 0.2560(2) 0.0502(8) Uani 1 1 d . . . H60 H 0.7683 0.3710 0.2797 0.075 Uiso 1 1 calc R . . H61 H 0.7604 0.3256 0.2078 0.075 Uiso 1 1 calc R . . H62 H 0.7316 0.2523 0.2891 0.075 Uiso 1 1 calc R . . C27 C 0.2613(2) 0.9856(2) 0.03980(14) 0.0333(5) Uani 1 1 d . . . H63 H 0.3158 0.9821 0.0794 0.050 Uiso 1 1 calc R . . H64 H 0.1832 0.9840 0.0608 0.050 Uiso 1 1 calc R . . H65 H 0.2509 1.0598 -0.0009 0.050 Uiso 1 1 calc R . . C28 C 0.2375(2) 0.8805(2) -0.08614(14) 0.0367(6) Uani 1 1 d . . . H66 H 0.1537 0.8864 -0.0743 0.055 Uiso 1 1 calc R . . H67 H 0.2718 0.8136 -0.1077 0.055 Uiso 1 1 calc R . . H68 H 0.2408 0.9552 -0.1226 0.055 Uiso 1 1 calc R . . C29 C 0.4783(2) 0.8560(2) -0.03325(14) 0.0342(5) Uani 1 1 d . . . H69 H 0.4708 0.9304 -0.0733 0.051 Uiso 1 1 calc R . . H70 H 0.5136 0.7873 -0.0531 0.051 Uiso 1 1 calc R . . H71 H 0.5302 0.8511 0.0082 0.051 Uiso 1 1 calc R . . C30 C 0.1550(2) 0.6229(3) -0.00394(16) 0.0403(6) Uani 1 1 d . . . H72 H 0.2157 0.5453 0.0002 0.061 Uiso 1 1 calc R . . H73 H 0.1629 0.6804 -0.0515 0.061 Uiso 1 1 calc R . . H74 H 0.0746 0.6137 -0.0027 0.061 Uiso 1 1 calc R . . C31 C 0.0510(2) 0.8175(2) 0.07539(15) 0.0352(6) Uani 1 1 d . . . H75 H -0.0242 0.7974 0.0849 0.053 Uiso 1 1 calc R . . H76 H 0.0444 0.8764 0.0260 0.053 Uiso 1 1 calc R . . H77 H 0.0665 0.8513 0.1145 0.053 Uiso 1 1 calc R . . C32 C 0.1677(2) 0.5577(2) 0.16254(15) 0.0325(5) Uani 1 1 d . . . H78 H 0.1899 0.5749 0.2074 0.049 Uiso 1 1 calc R . . H79 H 0.2227 0.4809 0.1590 0.049 Uiso 1 1 calc R . . H80 H 0.0853 0.5535 0.1662 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1A 0.02081(14) 0.03235(17) 0.02739(16) -0.01877(12) 0.00396(11) -0.00803(11) Ge1B 0.0332(17) 0.0278(15) 0.0225(15) -0.0079(12) 0.0045(12) -0.0027(12) Ge1D 0.033(2) 0.025(2) 0.024(2) -0.0101(16) 0.0048(16) -0.0023(17) Si1 0.0203(3) 0.0228(3) 0.0203(3) -0.0090(2) 0.0026(2) -0.0060(2) Si2 0.0183(3) 0.0199(3) 0.0196(3) -0.0083(2) -0.0001(2) -0.0039(2) Si3 0.0270(3) 0.0255(3) 0.0324(3) -0.0060(3) 0.0064(3) -0.0120(3) Si4 0.0317(4) 0.0437(4) 0.0454(4) -0.0251(3) -0.0056(3) -0.0115(3) Si5 0.0229(3) 0.0354(3) 0.0256(3) -0.0042(3) 0.0029(2) -0.0118(3) Si6 0.0322(3) 0.0248(3) 0.0262(3) -0.0021(3) -0.0022(3) -0.0072(3) Si7 0.0206(3) 0.0242(3) 0.0355(3) -0.0104(3) -0.0046(2) -0.0077(2) Si8 0.0246(3) 0.0175(3) 0.0331(3) -0.0065(2) -0.0053(3) -0.0043(2) Si9 0.0236(3) 0.0234(3) 0.0203(3) -0.0052(2) -0.0004(2) -0.0079(2) Si10 0.0177(3) 0.0262(3) 0.0275(3) -0.0083(3) -0.0008(2) -0.0078(2) C1 0.0218(10) 0.0241(10) 0.0247(11) -0.0108(9) 0.0026(8) -0.0075(8) C2 0.0322(12) 0.0285(12) 0.0273(12) -0.0134(10) 0.0104(9) -0.0094(10) C3 0.0336(12) 0.0308(12) 0.0240(11) -0.0115(10) 0.0077(9) -0.0102(10) C4 0.0249(10) 0.0237(10) 0.0189(10) -0.0060(8) 0.0029(8) -0.0091(8) C5 0.0180(9) 0.0186(9) 0.0238(10) -0.0077(8) -0.0023(8) -0.0053(8) C6 0.0188(10) 0.0237(10) 0.0270(11) -0.0120(9) 0.0035(8) -0.0056(8) C7 0.0218(10) 0.0236(10) 0.0239(11) -0.0118(9) 0.0017(8) -0.0060(8) C8 0.0164(9) 0.0202(10) 0.0204(10) -0.0084(8) -0.0001(8) -0.0052(8) C9 0.0491(17) 0.0262(13) 0.0607(19) -0.0068(13) 0.0111(14) -0.0106(12) C10 0.0334(13) 0.0370(14) 0.0334(13) 0.0031(11) -0.0042(11) -0.0116(11) C11 0.0458(16) 0.0588(18) 0.0427(15) -0.0204(14) 0.0177(13) -0.0337(14) C12 0.062(2) 0.0574(19) 0.0475(17) -0.0182(15) -0.0214(15) -0.0185(16) C13 0.0547(18) 0.0550(18) 0.0519(17) -0.0293(15) 0.0068(14) -0.0316(15) C14 0.0261(14) 0.096(3) 0.107(3) -0.072(3) -0.0081(16) -0.0085(16) C15 0.0288(13) 0.0458(16) 0.0503(17) 0.0059(13) -0.0052(12) -0.0133(12) C16 0.0329(13) 0.0378(13) 0.0345(13) -0.0094(11) 0.0083(10) -0.0178(11) C17 0.0425(16) 0.095(3) 0.0379(15) -0.0314(16) 0.0090(13) -0.0385(17) C18 0.0526(17) 0.0454(16) 0.0286(13) 0.0035(12) 0.0001(12) -0.0123(13) C19 0.0453(16) 0.0277(13) 0.0581(18) -0.0139(12) 0.0023(13) -0.0115(11) C20 0.0399(15) 0.0372(14) 0.0399(15) -0.0011(12) -0.0122(12) -0.0053(12) C21 0.0488(16) 0.0343(13) 0.0403(15) -0.0048(11) -0.0192(12) -0.0170(12) C22 0.0370(13) 0.0313(12) 0.0357(13) -0.0060(10) -0.0017(10) -0.0198(11) C23 0.0224(12) 0.0537(18) 0.083(2) -0.0342(17) 0.0058(13) -0.0126(12) C24 0.0375(13) 0.0229(11) 0.0504(16) -0.0095(11) -0.0059(12) -0.0121(10) C25 0.0649(19) 0.0300(13) 0.0313(14) -0.0010(11) 0.0006(13) -0.0134(13) C26 0.0335(14) 0.0238(13) 0.086(2) -0.0102(14) -0.0173(14) -0.0003(11) C27 0.0420(14) 0.0240(11) 0.0309(13) -0.0057(10) 0.0012(11) -0.0079(10) C28 0.0395(14) 0.0446(15) 0.0247(12) -0.0032(11) -0.0057(10) -0.0164(12) C29 0.0322(13) 0.0352(13) 0.0331(13) -0.0019(11) 0.0045(10) -0.0147(10) C30 0.0356(14) 0.0542(17) 0.0427(15) -0.0218(13) -0.0026(11) -0.0219(13) C31 0.0237(11) 0.0333(13) 0.0395(14) -0.0019(11) 0.0024(10) -0.0040(10) C32 0.0245(11) 0.0276(12) 0.0447(14) -0.0058(11) 0.0047(10) -0.0116(9) _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 Ge1A Si2 2.2323(7) . ? Ge1A Si1 2.2355(7) . ? Ge1B Si2 2.135(3) . ? Ge1B Si1 2.312(3) . ? Ge1D Si1 2.127(5) . ? Ge1D Si2 2.287(5) . ? Si1 C1 1.896(2) . ? Si1 C4 1.897(2) . ? Si2 C5 1.896(2) . ? Si2 C8 1.902(2) . ? Si3 C9 1.870(3) . ? Si3 C11 1.871(3) . ? Si3 C10 1.878(3) . ? Si3 C1 1.908(2) . ? Si4 C14 1.858(3) . ? Si4 C13 1.874(3) . ? Si4 C12 1.887(3) . ? Si4 C1 1.904(2) . ? Si5 C15 1.864(3) . ? Si5 C17 1.874(3) . ? Si5 C16 1.876(2) . ? Si5 C4 1.913(2) . ? Si6 C19 1.863(3) . ? Si6 C20 1.875(3) . ? Si6 C18 1.880(3) . ? Si6 C4 1.912(2) . ? Si7 C21 1.868(3) . ? Si7 C22 1.870(2) . ? Si7 C23 1.880(3) . ? Si7 C5 1.911(2) . ? Si8 C25 1.863(3) . ? Si8 C24 1.872(2) . ? Si8 C26 1.876(3) . ? Si8 C5 1.909(2) . ? Si9 C27 1.862(2) . ? Si9 C29 1.874(2) . ? Si9 C28 1.878(2) . ? Si9 C8 1.912(2) . ? Si10 C31 1.867(2) . ? Si10 C32 1.869(2) . ? Si10 C30 1.878(3) . ? Si10 C8 1.905(2) . ? C1 C2 1.576(3) . ? C2 C3 1.539(3) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.569(3) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C5 C6 1.565(3) . ? C6 C7 1.539(3) . ? C6 H5 0.9900 . ? C6 H6 0.9900 . ? C7 C8 1.571(3) . ? C7 H7 0.9900 . ? C7 H8 0.9900 . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C9 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C11 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C12 H20 0.9800 . ? C13 H21 0.9800 . ? C13 H22 0.9800 . ? C13 H23 0.9800 . ? C14 H24 0.9800 . ? C14 H25 0.9800 . ? C14 H26 0.9800 . ? C15 H27 0.9800 . ? C15 H28 0.9800 . ? C15 H29 0.9800 . ? C16 H30 0.9800 . ? C16 H31 0.9800 . ? C16 H32 0.9800 . ? C17 H33 0.9800 . ? C17 H34 0.9800 . ? C17 H35 0.9800 . ? C18 H36 0.9800 . ? C18 H37 0.9800 . ? C18 H38 0.9800 . ? C19 H39 0.9800 . ? C19 H40 0.9800 . ? C19 H41 0.9800 . ? C20 H42 0.9800 . ? C20 H43 0.9800 . ? C20 H44 0.9800 . ? C21 H45 0.9800 . ? C21 H46 0.9800 . ? C21 H47 0.9800 . ? C22 H48 0.9800 . ? C22 H49 0.9800 . ? C22 H50 0.9800 . ? C23 H51 0.9800 . ? C23 H52 0.9800 . ? C23 H53 0.9800 . ? C24 H54 0.9800 . ? C24 H55 0.9800 . ? C24 H56 0.9800 . ? C25 H57 0.9800 . ? C25 H58 0.9800 . ? C25 H59 0.9800 . ? C26 H60 0.9800 . ? C26 H61 0.9800 . ? C26 H62 0.9800 . ? C27 H63 0.9800 . ? C27 H64 0.9800 . ? C27 H65 0.9800 . ? C28 H66 0.9800 . ? C28 H67 0.9800 . ? C28 H68 0.9800 . ? C29 H69 0.9800 . ? C29 H70 0.9800 . ? C29 H71 0.9800 . ? C30 H72 0.9800 . ? C30 H73 0.9800 . ? C30 H74 0.9800 . ? C31 H75 0.9800 . ? C31 H76 0.9800 . ? C31 H77 0.9800 . ? C32 H78 0.9800 . ? C32 H79 0.9800 . ? C32 H80 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 Ge1A Si1 132.72(3) . . ? Si2 Ge1B Si1 133.91(16) . . ? Si1 Ge1D Si2 136.0(3) . . ? C1 Si1 C4 99.90(9) . . ? C1 Si1 Ge1D 118.18(17) . . ? C4 Si1 Ge1D 140.67(17) . . ? C1 Si1 Ge1A 115.73(7) . . ? C4 Si1 Ge1A 137.03(7) . . ? C1 Si1 Ge1B 141.67(12) . . ? C4 Si1 Ge1B 109.04(11) . . ? C5 Si2 C8 99.64(9) . . ? C5 Si2 Ge1B 117.20(11) . . ? C8 Si2 Ge1B 142.18(11) . . ? C5 Si2 Ge1A 115.96(7) . . ? C8 Si2 Ge1A 137.04(7) . . ? C5 Si2 Ge1D 143.52(16) . . ? C8 Si2 Ge1D 107.98(15) . . ? C9 Si3 C11 110.45(13) . . ? C9 Si3 C10 104.34(14) . . ? C11 Si3 C10 106.76(13) . . ? C9 Si3 C1 110.95(12) . . ? C11 Si3 C1 111.78(12) . . ? C10 Si3 C1 112.25(11) . . ? C14 Si4 C13 106.81(16) . . ? C14 Si4 C12 108.07(18) . . ? C13 Si4 C12 102.86(14) . . ? C14 Si4 C1 114.85(12) . . ? C13 Si4 C1 111.48(12) . . ? C12 Si4 C1 111.96(12) . . ? C15 Si5 C17 107.03(15) . . ? C15 Si5 C16 104.00(12) . . ? C17 Si5 C16 108.94(13) . . ? C15 Si5 C4 113.10(11) . . ? C17 Si5 C4 111.47(11) . . ? C16 Si5 C4 111.90(11) . . ? C19 Si6 C20 106.26(13) . . ? C19 Si6 C18 110.04(14) . . ? C20 Si6 C18 105.29(13) . . ? C19 Si6 C4 111.89(12) . . ? C20 Si6 C4 114.26(11) . . ? C18 Si6 C4 108.86(12) . . ? C21 Si7 C22 105.93(12) . . ? C21 Si7 C23 110.15(15) . . ? C22 Si7 C23 104.09(13) . . ? C21 Si7 C5 112.32(11) . . ? C22 Si7 C5 114.69(10) . . ? C23 Si7 C5 109.30(11) . . ? C25 Si8 C24 106.94(13) . . ? C25 Si8 C26 108.82(15) . . ? C24 Si8 C26 103.26(12) . . ? C25 Si8 C5 113.26(11) . . ? C24 Si8 C5 111.76(11) . . ? C26 Si8 C5 112.19(12) . . ? C27 Si9 C29 108.53(12) . . ? C27 Si9 C28 108.29(12) . . ? C29 Si9 C28 102.73(12) . . ? C27 Si9 C8 112.59(10) . . ? C29 Si9 C8 112.48(10) . . ? C28 Si9 C8 111.69(11) . . ? C31 Si10 C32 108.55(11) . . ? C31 Si10 C30 109.41(13) . . ? C32 Si10 C30 104.39(13) . . ? C31 Si10 C8 111.76(11) . . ? C32 Si10 C8 111.29(10) . . ? C30 Si10 C8 111.15(11) . . ? C2 C1 Si1 100.10(14) . . ? C2 C1 Si4 110.27(15) . . ? Si1 C1 Si4 118.43(11) . . ? C2 C1 Si3 108.29(15) . . ? Si1 C1 Si3 107.85(11) . . ? Si4 C1 Si3 111.06(11) . . ? C3 C2 C1 110.80(18) . . ? C3 C2 H1 109.5 . . ? C1 C2 H1 109.5 . . ? C3 C2 H2 109.5 . . ? C1 C2 H2 109.5 . . ? H1 C2 H2 108.1 . . ? C2 C3 C4 111.64(18) . . ? C2 C3 H3 109.3 . . ? C4 C3 H3 109.3 . . ? C2 C3 H4 109.3 . . ? C4 C3 H4 109.3 . . ? H3 C3 H4 108.0 . . ? C3 C4 Si1 101.60(14) . . ? C3 C4 Si6 109.98(15) . . ? Si1 C4 Si6 111.76(11) . . ? C3 C4 Si5 108.98(15) . . ? Si1 C4 Si5 113.81(11) . . ? Si6 C4 Si5 110.34(11) . . ? C6 C5 Si2 102.16(13) . . ? C6 C5 Si8 110.43(14) . . ? Si2 C5 Si8 112.04(11) . . ? C6 C5 Si7 109.47(14) . . ? Si2 C5 Si7 112.67(10) . . ? Si8 C5 Si7 109.83(10) . . ? C7 C6 C5 111.24(16) . . ? C7 C6 H5 109.4 . . ? C5 C6 H5 109.4 . . ? C7 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? H5 C6 H6 108.0 . . ? C6 C7 C8 111.65(16) . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C6 C7 H8 109.3 . . ? C8 C7 H8 109.3 . . ? H7 C7 H8 108.0 . . ? C7 C8 Si2 100.25(13) . . ? C7 C8 Si10 109.27(13) . . ? Si2 C8 Si10 109.50(10) . . ? C7 C8 Si9 109.90(14) . . ? Si2 C8 Si9 116.08(10) . . ? Si10 C8 Si9 111.20(10) . . ? Si3 C9 H9 109.5 . . ? Si3 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? Si3 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? Si3 C10 H12 109.5 . . ? Si3 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? Si3 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? Si3 C11 H15 109.5 . . ? Si3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? Si3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? Si4 C12 H18 109.5 . . ? Si4 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? Si4 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? Si4 C13 H21 109.5 . . ? Si4 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? Si4 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? Si4 C14 H24 109.5 . . ? Si4 C14 H25 109.5 . . ? H24 C14 H25 109.5 . . ? Si4 C14 H26 109.5 . . ? H24 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? Si5 C15 H27 109.5 . . ? Si5 C15 H28 109.5 . . ? H27 C15 H28 109.5 . . ? Si5 C15 H29 109.5 . . ? H27 C15 H29 109.5 . . ? H28 C15 H29 109.5 . . ? Si5 C16 H30 109.5 . . ? Si5 C16 H31 109.5 . . ? H30 C16 H31 109.5 . . ? Si5 C16 H32 109.5 . . ? H30 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? Si5 C17 H33 109.5 . . ? Si5 C17 H34 109.5 . . ? H33 C17 H34 109.5 . . ? Si5 C17 H35 109.5 . . ? H33 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? Si6 C18 H36 109.5 . . ? Si6 C18 H37 109.5 . . ? H36 C18 H37 109.5 . . ? Si6 C18 H38 109.5 . . ? H36 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? Si6 C19 H39 109.5 . . ? Si6 C19 H40 109.5 . . ? H39 C19 H40 109.5 . . ? Si6 C19 H41 109.5 . . ? H39 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si6 C20 H42 109.5 . . ? Si6 C20 H43 109.5 . . ? H42 C20 H43 109.5 . . ? Si6 C20 H44 109.5 . . ? H42 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si7 C21 H45 109.5 . . ? Si7 C21 H46 109.5 . . ? H45 C21 H46 109.5 . . ? Si7 C21 H47 109.5 . . ? H45 C21 H47 109.5 . . ? H46 C21 H47 109.5 . . ? Si7 C22 H48 109.5 . . ? Si7 C22 H49 109.5 . . ? H48 C22 H49 109.5 . . ? Si7 C22 H50 109.5 . . ? H48 C22 H50 109.5 . . ? H49 C22 H50 109.5 . . ? Si7 C23 H51 109.5 . . ? Si7 C23 H52 109.5 . . ? H51 C23 H52 109.5 . . ? Si7 C23 H53 109.5 . . ? H51 C23 H53 109.5 . . ? H52 C23 H53 109.5 . . ? Si8 C24 H54 109.5 . . ? Si8 C24 H55 109.5 . . ? H54 C24 H55 109.5 . . ? Si8 C24 H56 109.5 . . ? H54 C24 H56 109.5 . . ? H55 C24 H56 109.5 . . ? Si8 C25 H57 109.5 . . ? Si8 C25 H58 109.5 . . ? H57 C25 H58 109.5 . . ? Si8 C25 H59 109.5 . . ? H57 C25 H59 109.5 . . ? H58 C25 H59 109.5 . . ? Si8 C26 H60 109.5 . . ? Si8 C26 H61 109.5 . . ? H60 C26 H61 109.5 . . ? Si8 C26 H62 109.5 . . ? H60 C26 H62 109.5 . . ? H61 C26 H62 109.5 . . ? Si9 C27 H63 109.5 . . ? Si9 C27 H64 109.5 . . ? H63 C27 H64 109.5 . . ? Si9 C27 H65 109.5 . . ? H63 C27 H65 109.5 . . ? H64 C27 H65 109.5 . . ? Si9 C28 H66 109.5 . . ? Si9 C28 H67 109.5 . . ? H66 C28 H67 109.5 . . ? Si9 C28 H68 109.5 . . ? H66 C28 H68 109.5 . . ? H67 C28 H68 109.5 . . ? Si9 C29 H69 109.5 . . ? Si9 C29 H70 109.5 . . ? H69 C29 H70 109.5 . . ? Si9 C29 H71 109.5 . . ? H69 C29 H71 109.5 . . ? H70 C29 H71 109.5 . . ? Si10 C30 H72 109.5 . . ? Si10 C30 H73 109.5 . . ? H72 C30 H73 109.5 . . ? Si10 C30 H74 109.5 . . ? H72 C30 H74 109.5 . . ? H73 C30 H74 109.5 . . ? Si10 C31 H75 109.5 . . ? Si10 C31 H76 109.5 . . ? H75 C31 H76 109.5 . . ? Si10 C31 H77 109.5 . . ? H75 C31 H77 109.5 . . ? H76 C31 H77 109.5 . . ? Si10 C32 H78 109.5 . . ? Si10 C32 H79 109.5 . . ? H78 C32 H79 109.5 . . ? Si10 C32 H80 109.5 . . ? H78 C32 H80 109.5 . . ? H79 C32 H80 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.788 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.061 data_2-germadisilaallene_crystalB_173K _database_code_depnum_ccdc_archive 'CCDC 279205' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C32 H80 Ge Si10 ' _chemical_formula_moiety 'C32 H80 Ge Si10 ' _chemical_formula_weight 818.45 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7571(2) _cell_length_b 12.2792(1) _cell_length_c 18.5740(5) _cell_angle_alpha 73.558(5) _cell_angle_beta 87.309(7) _cell_angle_gamma 72.299(5) _cell_volume 2447.83(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6370 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 55.0 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.7760 _exptl_absorpt_correction_T_max 0.9162 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19094 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10527 _reflns_number_gt 8879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+2.9583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10527 _refine_ls_number_parameters 443 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1A Ge 0.35270(4) 0.29637(5) 0.25394(3) 0.03489(17) Uani 0.7260(14) 1 d PU . . Ge1B Ge 0.3193(2) 0.2166(2) 0.27773(14) 0.0384(8) Uani 0.1364(12) 1 d PU . . Ge1C Ge 0.2295(15) 0.2630(15) 0.2336(9) 0.0349(14) Uani 0.0204(9) 1 d PU . . Ge1D Ge 0.2713(3) 0.3469(3) 0.21145(16) 0.0380(8) Uani 0.1171(11) 1 d PU . . Si1 Si 0.19292(7) 0.37437(8) 0.31374(5) 0.03203(19) Uani 1 1 d U . . Si2 Si 0.38283(7) 0.18760(7) 0.17287(5) 0.02949(18) Uani 1 1 d U . . Si3 Si 0.15117(8) 0.64466(8) 0.24544(6) 0.0406(2) Uani 1 1 d . . . Si4 Si 0.32651(11) 0.51657(11) 0.38681(7) 0.0565(3) Uani 1 1 d . . . Si5 Si -0.06008(8) 0.32983(9) 0.34828(6) 0.0443(2) Uani 1 1 d . . . Si6 Si 0.16699(9) 0.16198(9) 0.44950(6) 0.0433(2) Uani 1 1 d . . . Si7 Si 0.65846(8) 0.14564(8) 0.19849(6) 0.0399(2) Uani 1 1 d . . . Si8 Si 0.55919(8) -0.07263(8) 0.24014(6) 0.0383(2) Uani 1 1 d . . . Si9 Si 0.32677(8) 0.35325(8) 0.00112(5) 0.0334(2) Uani 1 1 d . . . Si10 Si 0.17900(7) 0.17849(8) 0.07624(5) 0.0354(2) Uani 1 1 d . . . C1 C 0.1901(3) 0.5166(3) 0.33587(18) 0.0345(7) Uani 1 1 d . . . C2 C 0.0794(3) 0.5324(3) 0.3873(2) 0.0473(9) Uani 1 1 d . . . H1 H 0.0872 0.5801 0.4207 0.057 Uiso 1 1 calc R . . H2 H 0.0053 0.5760 0.3556 0.057 Uiso 1 1 calc R . . C3 C 0.0708(4) 0.4109(3) 0.43511(19) 0.0471(9) Uani 1 1 d . . . H3 H -0.0090 0.4217 0.4568 0.057 Uiso 1 1 calc R . . H4 H 0.1314 0.3786 0.4772 0.057 Uiso 1 1 calc R . . C4 C 0.0909(3) 0.3195(3) 0.38815(17) 0.0329(6) Uani 1 1 d . . . C5 C 0.5394(2) 0.0834(3) 0.17425(16) 0.0289(6) Uani 1 1 d . . . C6 C 0.5508(3) 0.0786(3) 0.09075(17) 0.0329(7) Uani 1 1 d . . . H5 H 0.5868 0.1401 0.0618 0.039 Uiso 1 1 calc R . . H6 H 0.6046 -0.0002 0.0892 0.039 Uiso 1 1 calc R . . C7 C 0.4282(3) 0.1000(3) 0.05422(17) 0.0310(6) Uani 1 1 d . . . H7 H 0.4040 0.0267 0.0721 0.037 Uiso 1 1 calc R . . H8 H 0.4345 0.1179 -0.0010 0.037 Uiso 1 1 calc R . . C8 C 0.3304(2) 0.2061(3) 0.07363(16) 0.0274(6) Uani 1 1 d . . . C9 C 0.0409(3) 0.6289(4) 0.1823(2) 0.0544(10) Uani 1 1 d . . . H9 H -0.0379 0.6440 0.2042 0.082 Uiso 1 1 calc R . . H10 H 0.0669 0.5480 0.1769 0.082 Uiso 1 1 calc R . . H11 H 0.0361 0.6866 0.1329 0.082 Uiso 1 1 calc R . . C10 C 0.0765(4) 0.7899(4) 0.2661(3) 0.0692(13) Uani 1 1 d . . . H12 H 0.1353 0.8137 0.2887 0.104 Uiso 1 1 calc R . . H13 H 0.0127 0.7809 0.3012 0.104 Uiso 1 1 calc R . . H14 H 0.0422 0.8510 0.2194 0.104 Uiso 1 1 calc R . . C11 C 0.2843(4) 0.6550(4) 0.1886(2) 0.0616(11) Uani 1 1 d . . . H15 H 0.2590 0.7176 0.1411 0.092 Uiso 1 1 calc R . . H16 H 0.3233 0.5785 0.1783 0.092 Uiso 1 1 calc R . . H17 H 0.3405 0.6743 0.2166 0.092 Uiso 1 1 calc R . . C12 C 0.3209(4) 0.6711(4) 0.3856(3) 0.0689(12) Uani 1 1 d . . . H18 H 0.3879 0.6674 0.4166 0.103 Uiso 1 1 calc R . . H19 H 0.2455 0.7090 0.4058 0.103 Uiso 1 1 calc R . . H20 H 0.3263 0.7177 0.3339 0.103 Uiso 1 1 calc R . . C13 C 0.3304(6) 0.4390(5) 0.4899(3) 0.105(2) Uani 1 1 d . . . H21 H 0.3441 0.3537 0.4971 0.158 Uiso 1 1 calc R . . H22 H 0.2540 0.4726 0.5107 0.158 Uiso 1 1 calc R . . H23 H 0.3951 0.4502 0.5155 0.158 Uiso 1 1 calc R . . C14 C 0.4716(4) 0.4510(6) 0.3487(4) 0.112(2) Uani 1 1 d . . . H24 H 0.4675 0.4839 0.2939 0.168 Uiso 1 1 calc R . . H25 H 0.4891 0.3643 0.3616 0.168 Uiso 1 1 calc R . . H26 H 0.5350 0.4702 0.3703 0.168 Uiso 1 1 calc R . . C15 C -0.1620(4) 0.4860(4) 0.3150(3) 0.097(2) Uani 1 1 d . . . H27 H -0.1290 0.5307 0.2713 0.145 Uiso 1 1 calc R . . H28 H -0.1697 0.5245 0.3554 0.145 Uiso 1 1 calc R . . H29 H -0.2409 0.4848 0.3011 0.145 Uiso 1 1 calc R . . C16 C -0.0432(4) 0.2662(6) 0.2674(3) 0.0923(19) Uani 1 1 d . . . H30 H -0.0152 0.1790 0.2858 0.138 Uiso 1 1 calc R . . H31 H 0.0151 0.2941 0.2337 0.138 Uiso 1 1 calc R . . H32 H -0.1204 0.2918 0.2402 0.138 Uiso 1 1 calc R . . C17 C -0.1481(3) 0.2531(4) 0.4208(2) 0.0524(9) Uani 1 1 d . . . H33 H -0.2281 0.2684 0.3996 0.079 Uiso 1 1 calc R . . H34 H -0.1548 0.2836 0.4647 0.079 Uiso 1 1 calc R . . H35 H -0.1073 0.1671 0.4360 0.079 Uiso 1 1 calc R . . C18 C 0.0955(4) 0.1389(4) 0.5427(2) 0.0688(12) Uani 1 1 d . . . H36 H 0.1289 0.0558 0.5726 0.103 Uiso 1 1 calc R . . H37 H 0.0091 0.1574 0.5349 0.103 Uiso 1 1 calc R . . H38 H 0.1111 0.1916 0.5694 0.103 Uiso 1 1 calc R . . C19 C 0.1580(4) 0.0471(3) 0.4039(3) 0.0647(12) Uani 1 1 d . . . H39 H 0.1900 0.0636 0.3536 0.097 Uiso 1 1 calc R . . H40 H 0.0744 0.0495 0.3997 0.097 Uiso 1 1 calc R . . H41 H 0.2048 -0.0321 0.4343 0.097 Uiso 1 1 calc R . . C20 C 0.3294(4) 0.1317(4) 0.4721(2) 0.0612(11) Uani 1 1 d . . . H42 H 0.3381 0.1859 0.4999 0.092 Uiso 1 1 calc R . . H43 H 0.3722 0.1442 0.4254 0.092 Uiso 1 1 calc R . . H44 H 0.3628 0.0491 0.5029 0.092 Uiso 1 1 calc R . . C21 C 0.6781(4) 0.1187(4) 0.3017(2) 0.0631(12) Uani 1 1 d . . . H45 H 0.7389 0.1530 0.3114 0.095 Uiso 1 1 calc R . . H46 H 0.7037 0.0327 0.3263 0.095 Uiso 1 1 calc R . . H47 H 0.6022 0.1561 0.3215 0.095 Uiso 1 1 calc R . . C22 C 0.6267(3) 0.3102(3) 0.1563(2) 0.0485(9) Uani 1 1 d . . . H48 H 0.5461 0.3516 0.1684 0.073 Uiso 1 1 calc R . . H49 H 0.6324 0.3279 0.1016 0.073 Uiso 1 1 calc R . . H50 H 0.6852 0.3372 0.1768 0.073 Uiso 1 1 calc R . . C23 C 0.8046(3) 0.0778(4) 0.1589(3) 0.0717(13) Uani 1 1 d . . . H51 H 0.8660 0.1083 0.1724 0.108 Uiso 1 1 calc R . . H52 H 0.7952 0.0988 0.1041 0.108 Uiso 1 1 calc R . . H53 H 0.8286 -0.0091 0.1796 0.108 Uiso 1 1 calc R . . C24 C 0.7202(4) -0.1645(3) 0.2573(3) 0.0718(14) Uani 1 1 d . . . H54 H 0.7260 -0.2441 0.2904 0.108 Uiso 1 1 calc R . . H55 H 0.7632 -0.1260 0.2812 0.108 Uiso 1 1 calc R . . H56 H 0.7557 -0.1714 0.2094 0.108 Uiso 1 1 calc R . . C25 C 0.4925(3) -0.1616(3) 0.1979(2) 0.0512(9) Uani 1 1 d . . . H57 H 0.5118 -0.2434 0.2308 0.077 Uiso 1 1 calc R . . H58 H 0.5253 -0.1625 0.1485 0.077 Uiso 1 1 calc R . . H59 H 0.4056 -0.1256 0.1923 0.077 Uiso 1 1 calc R . . C26 C 0.4895(5) -0.0712(4) 0.3324(2) 0.0661(12) Uani 1 1 d . . . H60 H 0.4023 -0.0418 0.3249 0.099 Uiso 1 1 calc R . . H61 H 0.5163 -0.0187 0.3542 0.099 Uiso 1 1 calc R . . H62 H 0.5132 -0.1521 0.3666 0.099 Uiso 1 1 calc R . . C27 C 0.2612(4) 0.4850(3) 0.0377(2) 0.0505(9) Uani 1 1 d . . . H63 H 0.3159 0.4838 0.0764 0.076 Uiso 1 1 calc R . . H64 H 0.1844 0.4819 0.0596 0.076 Uiso 1 1 calc R . . H65 H 0.2491 0.5583 -0.0035 0.076 Uiso 1 1 calc R . . C28 C 0.2402(4) 0.3769(4) -0.0872(2) 0.0548(10) Uani 1 1 d . . . H66 H 0.2450 0.4501 -0.1242 0.082 Uiso 1 1 calc R . . H67 H 0.1564 0.3839 -0.0760 0.082 Uiso 1 1 calc R . . H68 H 0.2740 0.3090 -0.1077 0.082 Uiso 1 1 calc R . . C29 C 0.4784(3) 0.3554(3) -0.0335(2) 0.0473(9) Uani 1 1 d . . . H69 H 0.4711 0.4289 -0.0739 0.071 Uiso 1 1 calc R . . H70 H 0.5142 0.2864 -0.0527 0.071 Uiso 1 1 calc R . . H71 H 0.5292 0.3519 0.0079 0.071 Uiso 1 1 calc R . . C30 C 0.1673(3) 0.0593(3) 0.1627(2) 0.0477(9) Uani 1 1 d . . . H72 H 0.1871 0.0788 0.2073 0.071 Uiso 1 1 calc R . . H73 H 0.2232 -0.0174 0.1607 0.071 Uiso 1 1 calc R . . H74 H 0.0856 0.0541 0.1653 0.071 Uiso 1 1 calc R . . C31 C 0.0531(3) 0.3161(3) 0.0737(2) 0.0521(9) Uani 1 1 d . . . H75 H -0.0217 0.2959 0.0832 0.078 Uiso 1 1 calc R . . H76 H 0.0468 0.3740 0.0242 0.078 Uiso 1 1 calc R . . H77 H 0.0682 0.3508 0.1124 0.078 Uiso 1 1 calc R . . C32 C 0.1585(4) 0.1201(4) -0.0039(2) 0.0587(11) Uani 1 1 d . . . H78 H 0.0778 0.1127 -0.0039 0.088 Uiso 1 1 calc R . . H79 H 0.2175 0.0417 0.0020 0.088 Uiso 1 1 calc R . . H80 H 0.1695 0.1753 -0.0514 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1A 0.0287(3) 0.0447(3) 0.0394(3) -0.0259(2) 0.00526(19) -0.0104(2) Ge1B 0.0414(14) 0.0382(13) 0.0297(12) -0.0127(10) 0.0053(10) -0.0013(11) Ge1C 0.037(3) 0.039(3) 0.032(3) -0.018(3) 0.004(2) -0.010(2) Ge1D 0.0457(16) 0.0345(14) 0.0318(14) -0.0137(11) 0.0074(11) -0.0060(11) Si1 0.0315(4) 0.0343(4) 0.0321(4) -0.0146(4) 0.0050(3) -0.0082(4) Si2 0.0293(4) 0.0301(4) 0.0298(4) -0.0137(3) 0.0004(3) -0.0052(3) Si3 0.0358(5) 0.0385(5) 0.0470(5) -0.0078(4) 0.0066(4) -0.0154(4) Si4 0.0555(7) 0.0600(7) 0.0644(7) -0.0289(6) -0.0141(5) -0.0194(5) Si5 0.0322(5) 0.0531(6) 0.0423(5) -0.0041(4) 0.0050(4) -0.0146(4) Si6 0.0472(5) 0.0370(5) 0.0400(5) -0.0041(4) -0.0042(4) -0.0102(4) Si7 0.0340(5) 0.0351(5) 0.0527(6) -0.0128(4) -0.0114(4) -0.0111(4) Si8 0.0383(5) 0.0255(4) 0.0483(5) -0.0083(4) -0.0091(4) -0.0061(4) Si9 0.0327(4) 0.0346(4) 0.0311(4) -0.0069(4) -0.0018(3) -0.0092(4) Si10 0.0252(4) 0.0393(5) 0.0427(5) -0.0127(4) -0.0018(4) -0.0098(4) C1 0.0328(16) 0.0374(17) 0.0372(17) -0.0161(14) 0.0043(13) -0.0115(13) C2 0.062(2) 0.0413(19) 0.048(2) -0.0236(16) 0.0246(17) -0.0212(17) C3 0.066(2) 0.045(2) 0.0379(19) -0.0198(16) 0.0192(17) -0.0224(18) C4 0.0374(16) 0.0332(16) 0.0299(15) -0.0107(13) 0.0045(12) -0.0123(13) C5 0.0260(14) 0.0279(14) 0.0332(15) -0.0116(12) -0.0035(11) -0.0051(12) C6 0.0264(14) 0.0326(16) 0.0406(17) -0.0151(13) 0.0041(12) -0.0063(12) C7 0.0293(15) 0.0337(16) 0.0324(15) -0.0163(13) 0.0011(12) -0.0065(12) C8 0.0226(13) 0.0314(15) 0.0297(15) -0.0124(12) -0.0003(11) -0.0069(11) C9 0.041(2) 0.058(2) 0.053(2) 0.0034(19) -0.0105(17) -0.0143(18) C10 0.065(3) 0.041(2) 0.097(4) -0.014(2) 0.013(2) -0.016(2) C11 0.065(3) 0.087(3) 0.051(2) -0.023(2) 0.020(2) -0.049(2) C12 0.083(3) 0.074(3) 0.074(3) -0.035(2) 0.005(2) -0.045(3) C13 0.151(6) 0.101(4) 0.078(4) -0.008(3) -0.058(4) -0.067(4) C14 0.038(2) 0.139(5) 0.188(7) -0.110(5) -0.021(3) -0.004(3) C15 0.037(2) 0.070(3) 0.143(5) 0.033(3) -0.005(3) -0.016(2) C16 0.061(3) 0.188(6) 0.057(3) -0.050(3) 0.009(2) -0.066(4) C17 0.049(2) 0.060(2) 0.055(2) -0.0168(19) 0.0136(18) -0.0274(19) C18 0.079(3) 0.068(3) 0.045(2) 0.005(2) -0.001(2) -0.021(2) C19 0.065(3) 0.038(2) 0.092(3) -0.022(2) 0.000(2) -0.0138(19) C20 0.053(2) 0.059(2) 0.058(3) -0.005(2) -0.0189(19) -0.0061(19) C21 0.083(3) 0.051(2) 0.058(2) -0.0024(19) -0.033(2) -0.029(2) C22 0.054(2) 0.044(2) 0.054(2) -0.0094(17) -0.0036(17) -0.0277(18) C23 0.032(2) 0.071(3) 0.122(4) -0.042(3) 0.001(2) -0.017(2) C24 0.047(2) 0.034(2) 0.121(4) -0.010(2) -0.026(2) -0.0014(17) C25 0.053(2) 0.0310(17) 0.069(3) -0.0096(17) -0.0087(19) -0.0153(16) C26 0.104(4) 0.042(2) 0.044(2) 0.0010(18) -0.004(2) -0.021(2) C27 0.059(2) 0.0326(17) 0.054(2) -0.0103(16) 0.0033(18) -0.0080(16) C28 0.062(2) 0.066(3) 0.0334(18) -0.0010(17) -0.0126(17) -0.024(2) C29 0.045(2) 0.048(2) 0.047(2) -0.0038(17) 0.0050(16) -0.0203(17) C30 0.0360(18) 0.0421(19) 0.064(2) -0.0079(17) 0.0038(16) -0.0167(15) C31 0.0300(17) 0.050(2) 0.065(2) -0.0060(19) 0.0046(16) -0.0058(16) C32 0.052(2) 0.078(3) 0.063(3) -0.032(2) -0.0033(19) -0.033(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1A Si2 2.2311(9) . ? Ge1A Si1 2.2343(9) . ? Ge1B Si2 2.139(3) . ? Ge1B Si1 2.301(3) . ? Ge1C Si2 2.183(16) . ? Ge1C Si1 2.238(15) . ? Ge1D Si1 2.141(3) . ? Ge1D Si2 2.281(3) . ? Si1 C1 1.894(3) . ? Si1 C4 1.900(3) . ? Si2 C5 1.892(3) . ? Si2 C8 1.901(3) . ? Si3 C11 1.862(4) . ? Si3 C10 1.872(4) . ? Si3 C9 1.875(4) . ? Si3 C1 1.909(3) . ? Si4 C14 1.853(5) . ? Si4 C12 1.872(4) . ? Si4 C13 1.877(5) . ? Si4 C1 1.900(3) . ? Si5 C16 1.856(5) . ? Si5 C15 1.870(5) . ? Si5 C17 1.875(4) . ? Si5 C4 1.910(3) . ? Si6 C19 1.870(4) . ? Si6 C20 1.875(4) . ? Si6 C18 1.875(4) . ? Si6 C4 1.907(3) . ? Si7 C21 1.863(4) . ? Si7 C22 1.873(4) . ? Si7 C23 1.882(4) . ? Si7 C5 1.912(3) . ? Si8 C25 1.867(4) . ? Si8 C26 1.868(4) . ? Si8 C24 1.874(4) . ? Si8 C5 1.910(3) . ? Si9 C27 1.868(4) . ? Si9 C29 1.872(3) . ? Si9 C28 1.877(3) . ? Si9 C8 1.913(3) . ? Si10 C31 1.868(4) . ? Si10 C30 1.874(4) . ? Si10 C32 1.879(4) . ? Si10 C8 1.907(3) . ? C1 C2 1.575(4) . ? C2 C3 1.535(5) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.565(4) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C5 C6 1.566(4) . ? C6 C7 1.538(4) . ? C6 H5 0.9900 . ? C6 H6 0.9900 . ? C7 C8 1.571(4) . ? C7 H7 0.9900 . ? C7 H8 0.9900 . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C9 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C11 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C12 H20 0.9800 . ? C13 H21 0.9800 . ? C13 H22 0.9800 . ? C13 H23 0.9800 . ? C14 H24 0.9800 . ? C14 H25 0.9800 . ? C14 H26 0.9800 . ? C15 H27 0.9800 . ? C15 H28 0.9800 . ? C15 H29 0.9800 . ? C16 H30 0.9800 . ? C16 H31 0.9800 . ? C16 H32 0.9800 . ? C17 H33 0.9800 . ? C17 H34 0.9800 . ? C17 H35 0.9800 . ? C18 H36 0.9800 . ? C18 H37 0.9800 . ? C18 H38 0.9800 . ? C19 H39 0.9800 . ? C19 H40 0.9800 . ? C19 H41 0.9800 . ? C20 H42 0.9800 . ? C20 H43 0.9800 . ? C20 H44 0.9800 . ? C21 H45 0.9800 . ? C21 H46 0.9800 . ? C21 H47 0.9800 . ? C22 H48 0.9800 . ? C22 H49 0.9800 . ? C22 H50 0.9800 . ? C23 H51 0.9800 . ? C23 H52 0.9800 . ? C23 H53 0.9800 . ? C24 H54 0.9800 . ? C24 H55 0.9800 . ? C24 H56 0.9800 . ? C25 H57 0.9800 . ? C25 H58 0.9800 . ? C25 H59 0.9800 . ? C26 H60 0.9800 . ? C26 H61 0.9800 . ? C26 H62 0.9800 . ? C27 H63 0.9800 . ? C27 H64 0.9800 . ? C27 H65 0.9800 . ? C28 H66 0.9800 . ? C28 H67 0.9800 . ? C28 H68 0.9800 . ? C29 H69 0.9800 . ? C29 H70 0.9800 . ? C29 H71 0.9800 . ? C30 H72 0.9800 . ? C30 H73 0.9800 . ? C30 H74 0.9800 . ? C31 H75 0.9800 . ? C31 H76 0.9800 . ? C31 H77 0.9800 . ? C32 H78 0.9800 . ? C32 H79 0.9800 . ? C32 H80 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 Ge1A Si1 133.45(4) . . ? Si2 Ge1B Si1 134.97(13) . . ? Si2 Ge1C Si1 136.2(8) . . ? Si1 Ge1D Si2 136.11(15) . . ? C1 Si1 C4 99.91(14) . . ? C1 Si1 Ge1D 117.38(13) . . ? C4 Si1 Ge1D 141.25(13) . . ? C1 Si1 Ge1A 115.26(10) . . ? C4 Si1 Ge1A 138.04(10) . . ? C1 Si1 Ge1C 149.6(5) . . ? C4 Si1 Ge1C 108.9(5) . . ? C1 Si1 Ge1B 141.75(13) . . ? C4 Si1 Ge1B 110.00(12) . . ? C5 Si2 C8 99.54(12) . . ? C5 Si2 Ge1B 116.84(12) . . ? C8 Si2 Ge1B 142.37(12) . . ? C5 Si2 Ge1C 149.6(5) . . ? C8 Si2 Ge1C 108.9(4) . . ? C5 Si2 Ge1A 115.90(9) . . ? C8 Si2 Ge1A 137.79(10) . . ? C5 Si2 Ge1D 143.70(12) . . ? C8 Si2 Ge1D 108.93(12) . . ? C11 Si3 C10 109.9(2) . . ? C11 Si3 C9 106.02(19) . . ? C10 Si3 C9 104.8(2) . . ? C11 Si3 C1 112.41(18) . . ? C10 Si3 C1 110.95(18) . . ? C9 Si3 C1 112.39(15) . . ? C14 Si4 C12 106.7(3) . . ? C14 Si4 C13 108.6(3) . . ? C12 Si4 C13 102.8(2) . . ? C14 Si4 C1 114.86(19) . . ? C12 Si4 C1 111.47(19) . . ? C13 Si4 C1 111.6(2) . . ? C16 Si5 C15 106.9(3) . . ? C16 Si5 C17 108.7(2) . . ? C15 Si5 C17 103.3(2) . . ? C16 Si5 C4 111.81(17) . . ? C15 Si5 C4 113.35(19) . . ? C17 Si5 C4 112.28(16) . . ? C19 Si6 C20 106.5(2) . . ? C19 Si6 C18 110.2(2) . . ? C20 Si6 C18 105.1(2) . . ? C19 Si6 C4 111.63(17) . . ? C20 Si6 C4 113.97(17) . . ? C18 Si6 C4 109.17(18) . . ? C21 Si7 C22 105.79(18) . . ? C21 Si7 C23 110.1(2) . . ? C22 Si7 C23 104.5(2) . . ? C21 Si7 C5 112.27(16) . . ? C22 Si7 C5 114.28(15) . . ? C23 Si7 C5 109.55(16) . . ? C25 Si8 C26 107.0(2) . . ? C25 Si8 C24 103.08(19) . . ? C26 Si8 C24 109.0(2) . . ? C25 Si8 C5 111.76(15) . . ? C26 Si8 C5 113.10(16) . . ? C24 Si8 C5 112.29(17) . . ? C27 Si9 C29 108.46(18) . . ? C27 Si9 C28 108.30(19) . . ? C29 Si9 C28 102.72(18) . . ? C27 Si9 C8 112.60(15) . . ? C29 Si9 C8 112.42(14) . . ? C28 Si9 C8 111.79(15) . . ? C31 Si10 C30 108.00(17) . . ? C31 Si10 C32 109.74(19) . . ? C30 Si10 C32 104.59(19) . . ? C31 Si10 C8 111.84(15) . . ? C30 Si10 C8 111.62(14) . . ? C32 Si10 C8 110.76(16) . . ? C2 C1 Si1 100.6(2) . . ? C2 C1 Si4 110.0(2) . . ? Si1 C1 Si4 117.91(17) . . ? C2 C1 Si3 108.2(2) . . ? Si1 C1 Si3 108.70(16) . . ? Si4 C1 Si3 110.70(16) . . ? C3 C2 C1 110.9(3) . . ? C3 C2 H1 109.5 . . ? C1 C2 H1 109.5 . . ? C3 C2 H2 109.5 . . ? C1 C2 H2 109.5 . . ? H1 C2 H2 108.1 . . ? C2 C3 C4 112.1(3) . . ? C2 C3 H3 109.2 . . ? C4 C3 H3 109.2 . . ? C2 C3 H4 109.2 . . ? C4 C3 H4 109.2 . . ? H3 C3 H4 107.9 . . ? C3 C4 Si1 101.2(2) . . ? C3 C4 Si6 110.3(2) . . ? Si1 C4 Si6 111.82(16) . . ? C3 C4 Si5 108.9(2) . . ? Si1 C4 Si5 113.63(16) . . ? Si6 C4 Si5 110.55(15) . . ? C6 C5 Si2 102.17(18) . . ? C6 C5 Si8 110.07(19) . . ? Si2 C5 Si8 112.76(15) . . ? C6 C5 Si7 109.3(2) . . ? Si2 C5 Si7 112.35(14) . . ? Si8 C5 Si7 109.89(14) . . ? C7 C6 C5 111.3(2) . . ? C7 C6 H5 109.4 . . ? C5 C6 H5 109.4 . . ? C7 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? H5 C6 H6 108.0 . . ? C6 C7 C8 111.4(2) . . ? C6 C7 H7 109.4 . . ? C8 C7 H7 109.4 . . ? C6 C7 H8 109.4 . . ? C8 C7 H8 109.4 . . ? H7 C7 H8 108.0 . . ? C7 C8 Si2 100.63(18) . . ? C7 C8 Si10 109.24(19) . . ? Si2 C8 Si10 109.40(14) . . ? C7 C8 Si9 110.02(19) . . ? Si2 C8 Si9 115.95(15) . . ? Si10 C8 Si9 111.02(14) . . ? Si3 C9 H9 109.5 . . ? Si3 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? Si3 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? Si3 C10 H12 109.5 . . ? Si3 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? Si3 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? Si3 C11 H15 109.5 . . ? Si3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? Si3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? Si4 C12 H18 109.5 . . ? Si4 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? Si4 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? Si4 C13 H21 109.5 . . ? Si4 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? Si4 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? Si4 C14 H24 109.5 . . ? Si4 C14 H25 109.5 . . ? H24 C14 H25 109.5 . . ? Si4 C14 H26 109.5 . . ? H24 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? Si5 C15 H27 109.5 . . ? Si5 C15 H28 109.5 . . ? H27 C15 H28 109.5 . . ? Si5 C15 H29 109.5 . . ? H27 C15 H29 109.5 . . ? H28 C15 H29 109.5 . . ? Si5 C16 H30 109.5 . . ? Si5 C16 H31 109.5 . . ? H30 C16 H31 109.5 . . ? Si5 C16 H32 109.5 . . ? H30 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? Si5 C17 H33 109.5 . . ? Si5 C17 H34 109.5 . . ? H33 C17 H34 109.5 . . ? Si5 C17 H35 109.5 . . ? H33 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? Si6 C18 H36 109.5 . . ? Si6 C18 H37 109.5 . . ? H36 C18 H37 109.5 . . ? Si6 C18 H38 109.5 . . ? H36 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? Si6 C19 H39 109.5 . . ? Si6 C19 H40 109.5 . . ? H39 C19 H40 109.5 . . ? Si6 C19 H41 109.5 . . ? H39 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si6 C20 H42 109.5 . . ? Si6 C20 H43 109.5 . . ? H42 C20 H43 109.5 . . ? Si6 C20 H44 109.5 . . ? H42 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si7 C21 H45 109.5 . . ? Si7 C21 H46 109.5 . . ? H45 C21 H46 109.5 . . ? Si7 C21 H47 109.5 . . ? H45 C21 H47 109.5 . . ? H46 C21 H47 109.5 . . ? Si7 C22 H48 109.5 . . ? Si7 C22 H49 109.5 . . ? H48 C22 H49 109.5 . . ? Si7 C22 H50 109.5 . . ? H48 C22 H50 109.5 . . ? H49 C22 H50 109.5 . . ? Si7 C23 H51 109.5 . . ? Si7 C23 H52 109.5 . . ? H51 C23 H52 109.5 . . ? Si7 C23 H53 109.5 . . ? H51 C23 H53 109.5 . . ? H52 C23 H53 109.5 . . ? Si8 C24 H54 109.5 . . ? Si8 C24 H55 109.5 . . ? H54 C24 H55 109.5 . . ? Si8 C24 H56 109.5 . . ? H54 C24 H56 109.5 . . ? H55 C24 H56 109.5 . . ? Si8 C25 H57 109.5 . . ? Si8 C25 H58 109.5 . . ? H57 C25 H58 109.5 . . ? Si8 C25 H59 109.5 . . ? H57 C25 H59 109.5 . . ? H58 C25 H59 109.5 . . ? Si8 C26 H60 109.5 . . ? Si8 C26 H61 109.5 . . ? H60 C26 H61 109.5 . . ? Si8 C26 H62 109.5 . . ? H60 C26 H62 109.5 . . ? H61 C26 H62 109.5 . . ? Si9 C27 H63 109.5 . . ? Si9 C27 H64 109.5 . . ? H63 C27 H64 109.5 . . ? Si9 C27 H65 109.5 . . ? H63 C27 H65 109.5 . . ? H64 C27 H65 109.5 . . ? Si9 C28 H66 109.5 . . ? Si9 C28 H67 109.5 . . ? H66 C28 H67 109.5 . . ? Si9 C28 H68 109.5 . . ? H66 C28 H68 109.5 . . ? H67 C28 H68 109.5 . . ? Si9 C29 H69 109.5 . . ? Si9 C29 H70 109.5 . . ? H69 C29 H70 109.5 . . ? Si9 C29 H71 109.5 . . ? H69 C29 H71 109.5 . . ? H70 C29 H71 109.5 . . ? Si10 C30 H72 109.5 . . ? Si10 C30 H73 109.5 . . ? H72 C30 H73 109.5 . . ? Si10 C30 H74 109.5 . . ? H72 C30 H74 109.5 . . ? H73 C30 H74 109.5 . . ? Si10 C31 H75 109.5 . . ? Si10 C31 H76 109.5 . . ? H75 C31 H76 109.5 . . ? Si10 C31 H77 109.5 . . ? H75 C31 H77 109.5 . . ? H76 C31 H77 109.5 . . ? Si10 C32 H78 109.5 . . ? Si10 C32 H79 109.5 . . ? H78 C32 H79 109.5 . . ? Si10 C32 H80 109.5 . . ? H78 C32 H80 109.5 . . ? H79 C32 H80 109.5 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.604 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.064 data_2-germadisilaallene_crystalB_223K _database_code_depnum_ccdc_archive 'CCDC 279206' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C32 H80 Ge Si10 ' _chemical_formula_moiety 'C32 H80 Ge Si10 ' _chemical_formula_weight 818.45 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.777(3) _cell_length_b 12.315(3) _cell_length_c 18.633(5) _cell_angle_alpha 73.588(8) _cell_angle_beta 87.260(9) _cell_angle_gamma 72.249(8) _cell_volume 2466.8(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6118 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 55.0 _cell_measurement_temperature 223.2 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.7775 _exptl_absorpt_correction_T_max 0.9168 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19021 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10558 _reflns_number_gt 8679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+2.2220P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10558 _refine_ls_number_parameters 443 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1550 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1A Ge 0.35219(5) 0.29669(6) 0.25346(4) 0.0449(2) Uani 0.6136(15) 1 d PU . . Ge1B Ge 0.3186(2) 0.2178(2) 0.27706(12) 0.0497(7) Uani 0.1688(13) 1 d PU . . Ge1C Ge 0.2281(7) 0.2657(7) 0.2343(4) 0.0453(11) Uani 0.0483(10) 1 d PU . . Ge1D Ge 0.2715(2) 0.3461(2) 0.21184(13) 0.0483(7) Uani 0.1693(13) 1 d PU . . Si1 Si 0.19470(8) 0.37306(9) 0.31467(5) 0.0417(2) Uani 1 1 d U . . Si2 Si 0.38197(8) 0.18934(8) 0.17205(5) 0.0386(2) Uani 1 1 d U . . Si3 Si 0.15068(9) 0.64340(9) 0.24591(6) 0.0519(3) Uani 1 1 d . . . Si4 Si 0.33040(12) 0.51519(12) 0.38436(8) 0.0723(4) Uani 1 1 d . . . Si5 Si -0.05943(9) 0.33260(11) 0.35012(6) 0.0568(3) Uani 1 1 d . . . Si6 Si 0.16704(10) 0.16213(10) 0.44970(6) 0.0563(3) Uani 1 1 d . . . Si7 Si 0.65622(9) 0.14636(9) 0.19909(7) 0.0529(3) Uani 1 1 d . . . Si8 Si 0.55666(9) -0.07086(8) 0.24026(6) 0.0499(3) Uani 1 1 d . . . Si9 Si 0.32695(9) 0.35234(9) 0.00073(5) 0.0444(2) Uani 1 1 d . . . Si10 Si 0.17949(8) 0.17808(9) 0.07599(6) 0.0476(2) Uani 1 1 d . . . C1 C 0.1922(3) 0.5157(3) 0.33561(19) 0.0430(8) Uani 1 1 d . . . C2 C 0.0845(4) 0.5305(3) 0.3887(2) 0.0592(10) Uani 1 1 d . . . H1 H 0.0943 0.5769 0.4216 0.071 Uiso 1 1 calc R . . H2 H 0.0102 0.5743 0.3585 0.071 Uiso 1 1 calc R . . C3 C 0.0762(4) 0.4091(3) 0.4366(2) 0.0607(10) Uani 1 1 d . . . H3 H -0.0018 0.4199 0.4593 0.073 Uiso 1 1 calc R . . H4 H 0.1378 0.3761 0.4771 0.073 Uiso 1 1 calc R . . C4 C 0.0926(3) 0.3198(3) 0.38909(18) 0.0419(7) Uani 1 1 d . . . C5 C 0.5382(3) 0.0840(3) 0.17478(18) 0.0379(7) Uani 1 1 d . . . C6 C 0.5505(3) 0.0794(3) 0.09140(19) 0.0420(7) Uani 1 1 d . . . H5 H 0.5860 0.1403 0.0630 0.050 Uiso 1 1 calc R . . H6 H 0.6040 0.0017 0.0898 0.050 Uiso 1 1 calc R . . C7 C 0.4283(3) 0.1006(3) 0.05474(19) 0.0410(7) Uani 1 1 d . . . H7 H 0.4045 0.0282 0.0724 0.049 Uiso 1 1 calc R . . H8 H 0.4351 0.1179 0.0003 0.049 Uiso 1 1 calc R . . C8 C 0.3302(3) 0.2063(3) 0.07354(17) 0.0361(7) Uani 1 1 d . . . C9 C 0.0400(4) 0.6267(4) 0.1842(2) 0.0708(12) Uani 1 1 d . . . H9 H -0.0363 0.6366 0.2077 0.106 Uiso 1 1 calc R . . H10 H 0.0682 0.5483 0.1765 0.106 Uiso 1 1 calc R . . H11 H 0.0308 0.6866 0.1362 0.106 Uiso 1 1 calc R . . C10 C 0.0758(5) 0.7878(4) 0.2678(3) 0.0895(16) Uani 1 1 d . . . H12 H 0.1339 0.8106 0.2907 0.134 Uiso 1 1 calc R . . H13 H 0.0127 0.7785 0.3021 0.134 Uiso 1 1 calc R . . H14 H 0.0422 0.8489 0.2219 0.134 Uiso 1 1 calc R . . C11 C 0.2816(4) 0.6560(5) 0.1878(3) 0.0792(14) Uani 1 1 d . . . H15 H 0.2554 0.7195 0.1418 0.119 Uiso 1 1 calc R . . H16 H 0.3193 0.5817 0.1760 0.119 Uiso 1 1 calc R . . H17 H 0.3384 0.6735 0.2154 0.119 Uiso 1 1 calc R . . C12 C 0.3246(5) 0.6681(5) 0.3845(3) 0.0896(16) Uani 1 1 d . . . H18 H 0.3932 0.6642 0.4130 0.134 Uiso 1 1 calc R . . H19 H 0.2520 0.7034 0.4072 0.134 Uiso 1 1 calc R . . H20 H 0.3255 0.7162 0.3335 0.134 Uiso 1 1 calc R . . C13 C 0.4729(4) 0.4533(7) 0.3427(5) 0.139(3) Uani 1 1 d . . . H21 H 0.4662 0.4886 0.2889 0.209 Uiso 1 1 calc R . . H22 H 0.4905 0.3679 0.3537 0.209 Uiso 1 1 calc R . . H23 H 0.5367 0.4711 0.3637 0.209 Uiso 1 1 calc R . . C14 C 0.3401(7) 0.4333(6) 0.4864(3) 0.148(3) Uani 1 1 d . . . H24 H 0.3604 0.3487 0.4923 0.222 Uiso 1 1 calc R . . H25 H 0.2638 0.4600 0.5082 0.222 Uiso 1 1 calc R . . H26 H 0.4012 0.4487 0.5117 0.222 Uiso 1 1 calc R . . C15 C -0.0461(5) 0.2751(7) 0.2674(3) 0.118(2) Uani 1 1 d . . . H27 H 0.0030 0.1927 0.2809 0.177 Uiso 1 1 calc R . . H28 H -0.0096 0.3217 0.2276 0.177 Uiso 1 1 calc R . . H29 H -0.1248 0.2810 0.2502 0.177 Uiso 1 1 calc R . . C16 C -0.1606(4) 0.4897(5) 0.3207(4) 0.127(3) Uani 1 1 d . . . H30 H -0.2391 0.4903 0.3068 0.190 Uiso 1 1 calc R . . H31 H -0.1282 0.5355 0.2782 0.190 Uiso 1 1 calc R . . H32 H -0.1667 0.5244 0.3620 0.190 Uiso 1 1 calc R . . C17 C -0.1461(4) 0.2547(4) 0.4217(3) 0.0696(12) Uani 1 1 d . . . H33 H -0.2255 0.2704 0.4011 0.104 Uiso 1 1 calc R . . H34 H -0.1522 0.2834 0.4656 0.104 Uiso 1 1 calc R . . H35 H -0.1057 0.1699 0.4357 0.104 Uiso 1 1 calc R . . C18 C 0.0961(5) 0.1388(5) 0.5432(3) 0.0874(15) Uani 1 1 d . . . H36 H 0.1290 0.0566 0.5725 0.131 Uiso 1 1 calc R . . H37 H 0.0106 0.1575 0.5358 0.131 Uiso 1 1 calc R . . H38 H 0.1123 0.1904 0.5697 0.131 Uiso 1 1 calc R . . C19 C 0.1563(5) 0.0492(4) 0.4032(3) 0.0845(15) Uani 1 1 d . . . H39 H 0.1878 0.0661 0.3536 0.127 Uiso 1 1 calc R . . H40 H 0.0735 0.0525 0.3992 0.127 Uiso 1 1 calc R . . H41 H 0.2022 -0.0294 0.4327 0.127 Uiso 1 1 calc R . . C20 C 0.3294(4) 0.1305(4) 0.4721(3) 0.0790(14) Uani 1 1 d . . . H42 H 0.3385 0.1819 0.5009 0.118 Uiso 1 1 calc R . . H43 H 0.3712 0.1452 0.4259 0.118 Uiso 1 1 calc R . . H44 H 0.3626 0.0482 0.5009 0.118 Uiso 1 1 calc R . . C21 C 0.6249(4) 0.3093(4) 0.1565(2) 0.0633(11) Uani 1 1 d . . . H45 H 0.6268 0.3264 0.1025 0.095 Uiso 1 1 calc R . . H46 H 0.6849 0.3355 0.1746 0.095 Uiso 1 1 calc R . . H47 H 0.5466 0.3508 0.1704 0.095 Uiso 1 1 calc R . . C22 C 0.6737(5) 0.1207(4) 0.3021(3) 0.0884(17) Uani 1 1 d . . . H48 H 0.7311 0.1575 0.3119 0.133 Uiso 1 1 calc R . . H49 H 0.7018 0.0360 0.3265 0.133 Uiso 1 1 calc R . . H50 H 0.5974 0.1552 0.3214 0.133 Uiso 1 1 calc R . . C23 C 0.8030(4) 0.0782(5) 0.1611(4) 0.0959(18) Uani 1 1 d . . . H51 H 0.7960 0.1014 0.1068 0.144 Uiso 1 1 calc R . . H52 H 0.8248 -0.0076 0.1800 0.144 Uiso 1 1 calc R . . H53 H 0.8640 0.1058 0.1767 0.144 Uiso 1 1 calc R . . C24 C 0.4910(4) -0.1605(3) 0.1985(3) 0.0666(11) Uani 1 1 d . . . H54 H 0.5083 -0.2405 0.2318 0.100 Uiso 1 1 calc R . . H55 H 0.5252 -0.1635 0.1505 0.100 Uiso 1 1 calc R . . H56 H 0.4052 -0.1241 0.1916 0.100 Uiso 1 1 calc R . . C25 C 0.4868(5) -0.0694(4) 0.3318(2) 0.0860(15) Uani 1 1 d . . . H57 H 0.4007 -0.0418 0.3244 0.129 Uiso 1 1 calc R . . H58 H 0.5120 -0.0165 0.3529 0.129 Uiso 1 1 calc R . . H59 H 0.5113 -0.1490 0.3657 0.129 Uiso 1 1 calc R . . C26 C 0.7171(4) -0.1621(4) 0.2578(4) 0.0981(19) Uani 1 1 d . . . H60 H 0.7228 -0.2402 0.2911 0.147 Uiso 1 1 calc R . . H61 H 0.7595 -0.1233 0.2807 0.147 Uiso 1 1 calc R . . H62 H 0.7522 -0.1703 0.2107 0.147 Uiso 1 1 calc R . . C27 C 0.2622(4) 0.4843(3) 0.0360(2) 0.0652(11) Uani 1 1 d . . . H63 H 0.3179 0.4856 0.0723 0.098 Uiso 1 1 calc R . . H64 H 0.1879 0.4801 0.0596 0.098 Uiso 1 1 calc R . . H65 H 0.2472 0.5560 -0.0055 0.098 Uiso 1 1 calc R . . C28 C 0.2412(4) 0.3754(4) -0.0873(2) 0.0743(13) Uani 1 1 d . . . H66 H 0.2492 0.4454 -0.1247 0.111 Uiso 1 1 calc R . . H67 H 0.1576 0.3863 -0.0768 0.111 Uiso 1 1 calc R . . H68 H 0.2723 0.3065 -0.1060 0.111 Uiso 1 1 calc R . . C29 C 0.4784(4) 0.3546(4) -0.0336(2) 0.0624(10) Uani 1 1 d . . . H69 H 0.4714 0.4278 -0.0728 0.094 Uiso 1 1 calc R . . H70 H 0.5135 0.2873 -0.0533 0.094 Uiso 1 1 calc R . . H71 H 0.5289 0.3498 0.0076 0.094 Uiso 1 1 calc R . . C30 C 0.1602(4) 0.1192(5) -0.0037(3) 0.0809(14) Uani 1 1 d . . . H72 H 0.2153 0.0397 0.0040 0.121 Uiso 1 1 calc R . . H73 H 0.1764 0.1708 -0.0503 0.121 Uiso 1 1 calc R . . H74 H 0.0790 0.1166 -0.0059 0.121 Uiso 1 1 calc R . . C31 C 0.0538(3) 0.3146(4) 0.0733(3) 0.0713(12) Uani 1 1 d . . . H75 H -0.0203 0.2948 0.0813 0.107 Uiso 1 1 calc R . . H76 H 0.0489 0.3724 0.0248 0.107 Uiso 1 1 calc R . . H77 H 0.0674 0.3479 0.1123 0.107 Uiso 1 1 calc R . . C32 C 0.1670(3) 0.0598(4) 0.1620(3) 0.0645(11) Uani 1 1 d . . . H78 H 0.1874 0.0785 0.2060 0.097 Uiso 1 1 calc R . . H79 H 0.2212 -0.0162 0.1599 0.097 Uiso 1 1 calc R . . H80 H 0.0858 0.0559 0.1648 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1A 0.0380(4) 0.0564(4) 0.0500(4) -0.0315(3) 0.0063(3) -0.0139(3) Ge1B 0.0559(14) 0.0471(13) 0.0379(11) -0.0144(9) 0.0081(9) -0.0027(10) Ge1C 0.045(2) 0.052(2) 0.044(2) -0.0255(19) 0.0081(18) -0.0134(18) Ge1D 0.0597(14) 0.0407(11) 0.0411(12) -0.0178(9) 0.0117(10) -0.0061(9) Si1 0.0414(5) 0.0453(5) 0.0416(5) -0.0191(4) 0.0072(4) -0.0124(4) Si2 0.0382(5) 0.0396(5) 0.0386(5) -0.0170(4) 0.0003(4) -0.0068(4) Si3 0.0476(6) 0.0495(6) 0.0587(6) -0.0098(5) 0.0076(5) -0.0207(5) Si4 0.0710(8) 0.0780(9) 0.0809(9) -0.0335(7) -0.0182(7) -0.0277(7) Si5 0.0422(6) 0.0659(7) 0.0566(6) -0.0063(5) 0.0066(5) -0.0190(5) Si6 0.0613(7) 0.0483(6) 0.0517(6) -0.0039(5) -0.0037(5) -0.0144(5) Si7 0.0457(6) 0.0463(6) 0.0687(7) -0.0141(5) -0.0164(5) -0.0161(5) Si8 0.0521(6) 0.0333(5) 0.0604(6) -0.0093(4) -0.0117(5) -0.0091(4) Si9 0.0442(5) 0.0454(5) 0.0399(5) -0.0082(4) -0.0032(4) -0.0112(4) Si10 0.0343(5) 0.0530(6) 0.0573(6) -0.0172(5) -0.0028(4) -0.0136(4) C1 0.0420(18) 0.0465(19) 0.0451(19) -0.0183(15) 0.0058(14) -0.0158(15) C2 0.073(3) 0.053(2) 0.063(2) -0.0319(19) 0.031(2) -0.026(2) C3 0.083(3) 0.056(2) 0.056(2) -0.0277(19) 0.027(2) -0.032(2) C4 0.049(2) 0.0417(18) 0.0371(17) -0.0133(14) 0.0070(14) -0.0153(15) C5 0.0339(16) 0.0365(16) 0.0438(18) -0.0135(14) -0.0053(13) -0.0085(13) C6 0.0338(17) 0.0415(18) 0.0509(19) -0.0188(15) 0.0050(14) -0.0068(14) C7 0.0415(18) 0.0449(18) 0.0416(18) -0.0224(15) 0.0016(14) -0.0107(15) C8 0.0335(16) 0.0389(16) 0.0380(16) -0.0154(13) 0.0000(13) -0.0094(13) C9 0.058(3) 0.076(3) 0.067(3) 0.003(2) -0.017(2) -0.022(2) C10 0.087(4) 0.054(3) 0.121(4) -0.018(3) 0.012(3) -0.020(2) C11 0.084(3) 0.106(4) 0.069(3) -0.027(3) 0.027(2) -0.062(3) C12 0.103(4) 0.100(4) 0.098(4) -0.045(3) 0.003(3) -0.061(3) C13 0.047(3) 0.168(7) 0.236(9) -0.129(6) -0.025(4) -0.010(3) C14 0.228(8) 0.139(6) 0.098(5) 0.010(4) -0.091(5) -0.109(6) C15 0.074(3) 0.237(8) 0.075(3) -0.064(4) 0.008(3) -0.074(4) C16 0.045(3) 0.079(4) 0.204(7) 0.039(4) 0.000(3) -0.015(2) C17 0.063(3) 0.078(3) 0.073(3) -0.015(2) 0.012(2) -0.036(2) C18 0.100(4) 0.089(4) 0.058(3) 0.010(2) 0.000(3) -0.034(3) C19 0.087(3) 0.047(2) 0.120(4) -0.023(3) -0.001(3) -0.020(2) C20 0.074(3) 0.077(3) 0.070(3) -0.006(2) -0.022(2) -0.012(2) C21 0.072(3) 0.060(2) 0.068(3) -0.012(2) -0.003(2) -0.039(2) C22 0.125(4) 0.070(3) 0.076(3) -0.004(2) -0.048(3) -0.047(3) C23 0.045(3) 0.092(4) 0.163(6) -0.052(4) -0.001(3) -0.022(2) C24 0.071(3) 0.041(2) 0.090(3) -0.017(2) -0.006(2) -0.0211(19) C25 0.138(5) 0.055(3) 0.055(3) 0.005(2) -0.002(3) -0.032(3) C26 0.070(3) 0.045(2) 0.164(6) -0.014(3) -0.042(3) -0.003(2) C27 0.078(3) 0.041(2) 0.069(3) -0.0119(19) 0.005(2) -0.0109(19) C28 0.078(3) 0.092(3) 0.048(2) -0.001(2) -0.016(2) -0.032(3) C29 0.060(2) 0.063(3) 0.062(2) -0.005(2) 0.0046(19) -0.026(2) C30 0.069(3) 0.108(4) 0.086(3) -0.043(3) -0.008(2) -0.041(3) C31 0.040(2) 0.070(3) 0.086(3) -0.004(2) 0.004(2) -0.0079(19) C32 0.048(2) 0.054(2) 0.090(3) -0.011(2) 0.005(2) -0.0233(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1A Si1 2.2284(11) . ? Ge1A Si2 2.2297(11) . ? Ge1B Si2 2.144(2) . ? Ge1B Si1 2.288(2) . ? Ge1C Si2 2.210(7) . ? Ge1C Si1 2.212(7) . ? Ge1D Si1 2.147(2) . ? Ge1D Si2 2.271(2) . ? Si1 C1 1.896(3) . ? Si1 C4 1.899(3) . ? Si2 C5 1.894(3) . ? Si2 C8 1.897(3) . ? Si3 C11 1.862(4) . ? Si3 C9 1.872(4) . ? Si3 C10 1.877(5) . ? Si3 C1 1.905(4) . ? Si4 C13 1.852(6) . ? Si4 C12 1.864(5) . ? Si4 C14 1.875(6) . ? Si4 C1 1.899(4) . ? Si5 C15 1.852(5) . ? Si5 C17 1.867(4) . ? Si5 C16 1.876(5) . ? Si5 C4 1.909(4) . ? Si6 C19 1.870(5) . ? Si6 C20 1.875(5) . ? Si6 C18 1.882(5) . ? Si6 C4 1.906(4) . ? Si7 C21 1.862(4) . ? Si7 C22 1.866(5) . ? Si7 C23 1.879(5) . ? Si7 C5 1.906(3) . ? Si8 C25 1.860(5) . ? Si8 C24 1.867(4) . ? Si8 C26 1.870(5) . ? Si8 C5 1.905(3) . ? Si9 C27 1.859(4) . ? Si9 C29 1.872(4) . ? Si9 C28 1.874(4) . ? Si9 C8 1.913(3) . ? Si10 C31 1.861(4) . ? Si10 C32 1.871(4) . ? Si10 C30 1.877(4) . ? Si10 C8 1.906(3) . ? C1 C2 1.569(5) . ? C2 C3 1.539(5) . ? C2 H1 0.9800 . ? C2 H2 0.9800 . ? C3 C4 1.560(5) . ? C3 H3 0.9800 . ? C3 H4 0.9800 . ? C5 C6 1.569(4) . ? C6 C7 1.540(4) . ? C6 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.568(4) . ? C7 H7 0.9800 . ? C7 H8 0.9800 . ? C9 H9 0.9700 . ? C9 H10 0.9700 . ? C9 H11 0.9700 . ? C10 H12 0.9700 . ? C10 H13 0.9700 . ? C10 H14 0.9700 . ? C11 H15 0.9700 . ? C11 H16 0.9700 . ? C11 H17 0.9700 . ? C12 H18 0.9700 . ? C12 H19 0.9700 . ? C12 H20 0.9700 . ? C13 H21 0.9700 . ? C13 H22 0.9700 . ? C13 H23 0.9700 . ? C14 H24 0.9700 . ? C14 H25 0.9700 . ? C14 H26 0.9700 . ? C15 H27 0.9700 . ? C15 H28 0.9700 . ? C15 H29 0.9700 . ? C16 H30 0.9700 . ? C16 H31 0.9700 . ? C16 H32 0.9700 . ? C17 H33 0.9700 . ? C17 H34 0.9700 . ? C17 H35 0.9700 . ? C18 H36 0.9700 . ? C18 H37 0.9700 . ? C18 H38 0.9700 . ? C19 H39 0.9700 . ? C19 H40 0.9700 . ? C19 H41 0.9700 . ? C20 H42 0.9700 . ? C20 H43 0.9700 . ? C20 H44 0.9700 . ? C21 H45 0.9700 . ? C21 H46 0.9700 . ? C21 H47 0.9700 . ? C22 H48 0.9700 . ? C22 H49 0.9700 . ? C22 H50 0.9700 . ? C23 H51 0.9700 . ? C23 H52 0.9700 . ? C23 H53 0.9700 . ? C24 H54 0.9700 . ? C24 H55 0.9700 . ? C24 H56 0.9700 . ? C25 H57 0.9700 . ? C25 H58 0.9700 . ? C25 H59 0.9700 . ? C26 H60 0.9700 . ? C26 H61 0.9700 . ? C26 H62 0.9700 . ? C27 H63 0.9700 . ? C27 H64 0.9700 . ? C27 H65 0.9700 . ? C28 H66 0.9700 . ? C28 H67 0.9700 . ? C28 H68 0.9700 . ? C29 H69 0.9700 . ? C29 H70 0.9700 . ? C29 H71 0.9700 . ? C30 H72 0.9700 . ? C30 H73 0.9700 . ? C30 H74 0.9700 . ? C31 H75 0.9700 . ? C31 H76 0.9700 . ? C31 H77 0.9700 . ? C32 H78 0.9700 . ? C32 H79 0.9700 . ? C32 H80 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 Ge1A Si2 133.99(5) . . ? Si2 Ge1B Si1 135.59(12) . . ? Si2 Ge1C Si1 136.2(4) . . ? Si1 Ge1D Si2 136.51(12) . . ? C1 Si1 C4 99.94(15) . . ? C1 Si1 Ge1D 116.83(13) . . ? C4 Si1 Ge1D 141.53(13) . . ? C1 Si1 Ge1C 148.5(2) . . ? C4 Si1 Ge1C 109.6(2) . . ? C1 Si1 Ge1A 114.97(11) . . ? C4 Si1 Ge1A 138.93(11) . . ? C1 Si1 Ge1B 141.77(13) . . ? C4 Si1 Ge1B 110.85(13) . . ? C5 Si2 C8 99.87(14) . . ? C5 Si2 Ge1B 115.98(12) . . ? C8 Si2 Ge1B 142.66(12) . . ? C5 Si2 Ge1C 148.4(2) . . ? C8 Si2 Ge1C 109.6(2) . . ? C5 Si2 Ge1A 115.34(10) . . ? C8 Si2 Ge1A 138.58(10) . . ? C5 Si2 Ge1D 143.23(12) . . ? C8 Si2 Ge1D 109.96(12) . . ? C11 Si3 C9 106.0(2) . . ? C11 Si3 C10 109.8(2) . . ? C9 Si3 C10 105.1(2) . . ? C11 Si3 C1 112.6(2) . . ? C9 Si3 C1 112.42(18) . . ? C10 Si3 C1 110.6(2) . . ? C13 Si4 C12 106.6(3) . . ? C13 Si4 C14 108.4(4) . . ? C12 Si4 C14 103.4(3) . . ? C13 Si4 C1 114.7(2) . . ? C12 Si4 C1 111.5(2) . . ? C14 Si4 C1 111.6(2) . . ? C15 Si5 C17 109.0(3) . . ? C15 Si5 C16 106.9(3) . . ? C17 Si5 C16 103.1(2) . . ? C15 Si5 C4 112.01(19) . . ? C17 Si5 C4 112.43(18) . . ? C16 Si5 C4 112.8(2) . . ? C19 Si6 C20 106.7(2) . . ? C19 Si6 C18 110.5(3) . . ? C20 Si6 C18 105.0(2) . . ? C19 Si6 C4 111.44(19) . . ? C20 Si6 C4 113.68(19) . . ? C18 Si6 C4 109.4(2) . . ? C21 Si7 C22 105.9(2) . . ? C21 Si7 C23 104.5(2) . . ? C22 Si7 C23 110.0(3) . . ? C21 Si7 C5 114.22(16) . . ? C22 Si7 C5 112.05(19) . . ? C23 Si7 C5 109.84(19) . . ? C25 Si8 C24 106.8(2) . . ? C25 Si8 C26 108.9(3) . . ? C24 Si8 C26 103.0(2) . . ? C25 Si8 C5 113.33(18) . . ? C24 Si8 C5 112.31(17) . . ? C26 Si8 C5 111.9(2) . . ? C27 Si9 C29 107.9(2) . . ? C27 Si9 C28 108.2(2) . . ? C29 Si9 C28 102.7(2) . . ? C27 Si9 C8 112.86(17) . . ? C29 Si9 C8 112.62(16) . . ? C28 Si9 C8 112.03(18) . . ? C31 Si10 C32 107.7(2) . . ? C31 Si10 C30 109.9(2) . . ? C32 Si10 C30 104.5(2) . . ? C31 Si10 C8 111.73(18) . . ? C32 Si10 C8 111.94(16) . . ? C30 Si10 C8 110.74(18) . . ? C2 C1 Si1 100.6(2) . . ? C2 C1 Si4 109.8(2) . . ? Si1 C1 Si4 117.23(18) . . ? C2 C1 Si3 108.5(2) . . ? Si1 C1 Si3 109.17(17) . . ? Si4 C1 Si3 110.84(17) . . ? C3 C2 C1 111.3(3) . . ? C3 C2 H1 109.4 . . ? C1 C2 H1 109.4 . . ? C3 C2 H2 109.4 . . ? C1 C2 H2 109.4 . . ? H1 C2 H2 108.0 . . ? C2 C3 C4 111.7(3) . . ? C2 C3 H3 109.3 . . ? C4 C3 H3 109.3 . . ? C2 C3 H4 109.3 . . ? C4 C3 H4 109.3 . . ? H3 C3 H4 107.9 . . ? C3 C4 Si1 101.2(2) . . ? C3 C4 Si6 109.8(2) . . ? Si1 C4 Si6 111.79(17) . . ? C3 C4 Si5 109.4(3) . . ? Si1 C4 Si5 113.79(17) . . ? Si6 C4 Si5 110.45(17) . . ? C6 C5 Si2 101.73(19) . . ? C6 C5 Si8 110.3(2) . . ? Si2 C5 Si8 113.06(17) . . ? C6 C5 Si7 109.1(2) . . ? Si2 C5 Si7 112.00(16) . . ? Si8 C5 Si7 110.31(15) . . ? C7 C6 C5 111.2(3) . . ? C7 C6 H5 109.4 . . ? C5 C6 H5 109.4 . . ? C7 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? H5 C6 H6 108.0 . . ? C6 C7 C8 111.6(2) . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C6 C7 H8 109.3 . . ? C8 C7 H8 109.3 . . ? H7 C7 H8 108.0 . . ? C7 C8 Si2 100.5(2) . . ? C7 C8 Si10 109.2(2) . . ? Si2 C8 Si10 109.65(16) . . ? C7 C8 Si9 109.8(2) . . ? Si2 C8 Si9 115.87(16) . . ? Si10 C8 Si9 111.19(16) . . ? Si3 C9 H9 109.5 . . ? Si3 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? Si3 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? Si3 C10 H12 109.5 . . ? Si3 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? Si3 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? Si3 C11 H15 109.5 . . ? Si3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? Si3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? Si4 C12 H18 109.5 . . ? Si4 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? Si4 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? Si4 C13 H21 109.5 . . ? Si4 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? Si4 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? Si4 C14 H24 109.5 . . ? Si4 C14 H25 109.5 . . ? H24 C14 H25 109.5 . . ? Si4 C14 H26 109.5 . . ? H24 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? Si5 C15 H27 109.5 . . ? Si5 C15 H28 109.5 . . ? H27 C15 H28 109.5 . . ? Si5 C15 H29 109.5 . . ? H27 C15 H29 109.5 . . ? H28 C15 H29 109.5 . . ? Si5 C16 H30 109.5 . . ? Si5 C16 H31 109.5 . . ? H30 C16 H31 109.5 . . ? Si5 C16 H32 109.5 . . ? H30 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? Si5 C17 H33 109.5 . . ? Si5 C17 H34 109.5 . . ? H33 C17 H34 109.5 . . ? Si5 C17 H35 109.5 . . ? H33 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? Si6 C18 H36 109.5 . . ? Si6 C18 H37 109.5 . . ? H36 C18 H37 109.5 . . ? Si6 C18 H38 109.5 . . ? H36 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? Si6 C19 H39 109.5 . . ? Si6 C19 H40 109.5 . . ? H39 C19 H40 109.5 . . ? Si6 C19 H41 109.5 . . ? H39 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si6 C20 H42 109.5 . . ? Si6 C20 H43 109.5 . . ? H42 C20 H43 109.5 . . ? Si6 C20 H44 109.5 . . ? H42 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si7 C21 H45 109.5 . . ? Si7 C21 H46 109.5 . . ? H45 C21 H46 109.5 . . ? Si7 C21 H47 109.5 . . ? H45 C21 H47 109.5 . . ? H46 C21 H47 109.5 . . ? Si7 C22 H48 109.5 . . ? Si7 C22 H49 109.5 . . ? H48 C22 H49 109.5 . . ? Si7 C22 H50 109.5 . . ? H48 C22 H50 109.5 . . ? H49 C22 H50 109.5 . . ? Si7 C23 H51 109.5 . . ? Si7 C23 H52 109.5 . . ? H51 C23 H52 109.5 . . ? Si7 C23 H53 109.5 . . ? H51 C23 H53 109.5 . . ? H52 C23 H53 109.5 . . ? Si8 C24 H54 109.5 . . ? Si8 C24 H55 109.5 . . ? H54 C24 H55 109.5 . . ? Si8 C24 H56 109.5 . . ? H54 C24 H56 109.5 . . ? H55 C24 H56 109.5 . . ? Si8 C25 H57 109.5 . . ? Si8 C25 H58 109.5 . . ? H57 C25 H58 109.5 . . ? Si8 C25 H59 109.5 . . ? H57 C25 H59 109.5 . . ? H58 C25 H59 109.5 . . ? Si8 C26 H60 109.5 . . ? Si8 C26 H61 109.5 . . ? H60 C26 H61 109.5 . . ? Si8 C26 H62 109.5 . . ? H60 C26 H62 109.5 . . ? H61 C26 H62 109.5 . . ? Si9 C27 H63 109.5 . . ? Si9 C27 H64 109.5 . . ? H63 C27 H64 109.5 . . ? Si9 C27 H65 109.5 . . ? H63 C27 H65 109.5 . . ? H64 C27 H65 109.5 . . ? Si9 C28 H66 109.5 . . ? Si9 C28 H67 109.5 . . ? H66 C28 H67 109.5 . . ? Si9 C28 H68 109.5 . . ? H66 C28 H68 109.5 . . ? H67 C28 H68 109.5 . . ? Si9 C29 H69 109.5 . . ? Si9 C29 H70 109.5 . . ? H69 C29 H70 109.5 . . ? Si9 C29 H71 109.5 . . ? H69 C29 H71 109.5 . . ? H70 C29 H71 109.5 . . ? Si10 C30 H72 109.5 . . ? Si10 C30 H73 109.5 . . ? H72 C30 H73 109.5 . . ? Si10 C30 H74 109.5 . . ? H72 C30 H74 109.5 . . ? H73 C30 H74 109.5 . . ? Si10 C31 H75 109.5 . . ? Si10 C31 H76 109.5 . . ? H75 C31 H76 109.5 . . ? Si10 C31 H77 109.5 . . ? H75 C31 H77 109.5 . . ? H76 C31 H77 109.5 . . ? Si10 C32 H78 109.5 . . ? Si10 C32 H79 109.5 . . ? H78 C32 H79 109.5 . . ? Si10 C32 H80 109.5 . . ? H78 C32 H80 109.5 . . ? H79 C32 H80 109.5 . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.449 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.058 data_2-germadisilaallene_crystalB_273K _database_code_depnum_ccdc_archive 'CCDC 279207' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C32 H80 Ge Si10 ' _chemical_formula_moiety 'C32 H80 Ge Si10 ' _chemical_formula_weight 818.45 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.792(2) _cell_length_b 12.365(2) _cell_length_c 18.719(4) _cell_angle_alpha 73.572(6) _cell_angle_beta 87.166(8) _cell_angle_gamma 72.153(6) _cell_volume 2489.9(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5007 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 28.3 _cell_measurement_temperature 273.2 _exptl_crystal_description platelet _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.7792 _exptl_absorpt_correction_T_max 0.9176 _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23225 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10992 _reflns_number_gt 8472 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+1.6288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10992 _refine_ls_number_parameters 443 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1A Ge 0.35173(7) 0.79629(9) 0.25306(5) 0.0562(3) Uani 0.5328(15) 1 d PU . . Ge1B Ge 0.2711(2) 0.84539(19) 0.21223(12) 0.0574(6) Uani 0.2020(13) 1 d PU . . Ge1C Ge 0.2299(5) 0.7652(5) 0.2347(3) 0.0561(9) Uani 0.0781(10) 1 d PU . . Ge1D Ge 0.3180(2) 0.7186(2) 0.27626(13) 0.0602(7) Uani 0.1871(13) 1 d PU . . Si1 Si 0.38126(9) 0.69057(9) 0.17135(6) 0.0476(2) Uani 1 1 d U . . Si2 Si 0.19614(9) 0.87103(10) 0.31572(6) 0.0515(3) Uani 1 1 d U . . Si3 Si 0.55489(11) 0.43000(10) 0.24017(7) 0.0625(3) Uani 1 1 d . . . Si4 Si 0.65466(11) 0.64627(11) 0.19938(8) 0.0666(3) Uani 1 1 d . . . Si5 Si 0.17968(10) 0.67793(11) 0.07596(7) 0.0610(3) Uani 1 1 d . . . Si6 Si 0.32668(10) 0.85180(10) 0.00076(6) 0.0564(3) Uani 1 1 d . . . Si7 Si 0.33367(14) 1.01215(14) 0.38300(9) 0.0883(5) Uani 1 1 d . . . Si8 Si 0.15112(11) 1.14142(11) 0.24697(7) 0.0640(3) Uani 1 1 d . . . Si9 Si 0.16707(12) 0.66210(11) 0.45005(7) 0.0705(4) Uani 1 1 d . . . Si10 Si -0.05907(11) 0.83402(12) 0.35150(7) 0.0696(4) Uani 1 1 d . . . C1 C 0.5366(3) 0.5846(3) 0.1749(2) 0.0464(8) Uani 1 1 d . . . C2 C 0.5494(3) 0.5799(3) 0.0921(2) 0.0530(9) Uani 1 1 d . . . H1 H 0.5846 0.6399 0.0642 0.064 Uiso 1 1 calc R . . H2 H 0.6024 0.5032 0.0907 0.064 Uiso 1 1 calc R . . C3 C 0.4284(3) 0.6009(3) 0.0555(2) 0.0506(9) Uani 1 1 d . . . H3 H 0.4048 0.5295 0.0731 0.061 Uiso 1 1 calc R . . H4 H 0.4357 0.6173 0.0020 0.061 Uiso 1 1 calc R . . C4 C 0.3298(3) 0.7064(3) 0.07343(19) 0.0452(8) Uani 1 1 d . . . C5 C 0.1943(3) 1.0132(3) 0.3359(2) 0.0533(9) Uani 1 1 d . . . C6 C 0.0878(4) 1.0288(4) 0.3893(3) 0.0721(12) Uani 1 1 d . . . H5 H 0.0988 1.0740 0.4217 0.087 Uiso 1 1 calc R . . H6 H 0.0140 1.0728 0.3600 0.087 Uiso 1 1 calc R . . C7 C 0.0791(5) 0.9084(4) 0.4368(2) 0.0734(13) Uani 1 1 d . . . H7 H 0.0022 0.9196 0.4596 0.088 Uiso 1 1 calc R . . H8 H 0.1404 0.8753 0.4764 0.088 Uiso 1 1 calc R . . C8 C 0.0939(3) 0.8195(3) 0.3898(2) 0.0507(9) Uani 1 1 d . . . C9 C 0.4903(5) 0.3413(4) 0.1982(3) 0.0844(15) Uani 1 1 d . . . H9 H 0.4053 0.3764 0.1921 0.127 Uiso 1 1 calc R . . H10 H 0.5086 0.2619 0.2304 0.127 Uiso 1 1 calc R . . H11 H 0.5235 0.3398 0.1505 0.127 Uiso 1 1 calc R . . C10 C 0.7149(5) 0.3387(4) 0.2582(4) 0.118(2) Uani 1 1 d . . . H12 H 0.7201 0.2605 0.2888 0.177 Uiso 1 1 calc R . . H13 H 0.7556 0.3747 0.2833 0.177 Uiso 1 1 calc R . . H14 H 0.7513 0.3341 0.2117 0.177 Uiso 1 1 calc R . . C11 C 0.4840(6) 0.4318(5) 0.3311(3) 0.107(2) Uani 1 1 d . . . H15 H 0.3989 0.4618 0.3233 0.161 Uiso 1 1 calc R . . H16 H 0.5109 0.4816 0.3529 0.161 Uiso 1 1 calc R . . H17 H 0.5056 0.3527 0.3640 0.161 Uiso 1 1 calc R . . C12 C 0.8020(4) 0.5778(6) 0.1621(4) 0.117(2) Uani 1 1 d . . . H18 H 0.7950 0.5983 0.1087 0.176 Uiso 1 1 calc R . . H19 H 0.8246 0.4932 0.1821 0.176 Uiso 1 1 calc R . . H20 H 0.8616 0.6068 0.1765 0.176 Uiso 1 1 calc R . . C13 C 0.6704(6) 0.6217(5) 0.3023(3) 0.112(2) Uani 1 1 d . . . H21 H 0.7221 0.6632 0.3119 0.168 Uiso 1 1 calc R . . H22 H 0.7036 0.5386 0.3263 0.168 Uiso 1 1 calc R . . H23 H 0.5934 0.6508 0.3214 0.168 Uiso 1 1 calc R . . C14 C 0.6236(5) 0.8078(4) 0.1562(3) 0.0789(14) Uani 1 1 d . . . H24 H 0.6849 0.8333 0.1719 0.118 Uiso 1 1 calc R . . H25 H 0.5478 0.8494 0.1714 0.118 Uiso 1 1 calc R . . H26 H 0.6220 0.8242 0.1029 0.118 Uiso 1 1 calc R . . C15 C 0.1604(5) 0.6193(6) -0.0034(3) 0.1029(19) Uani 1 1 d . . . H27 H 0.2148 0.5409 0.0042 0.154 Uiso 1 1 calc R . . H28 H 0.1765 0.6701 -0.0493 0.154 Uiso 1 1 calc R . . H29 H 0.0801 0.6169 -0.0056 0.154 Uiso 1 1 calc R . . C16 C 0.1675(4) 0.5604(4) 0.1614(3) 0.0831(15) Uani 1 1 d . . . H30 H 0.0891 0.5521 0.1622 0.125 Uiso 1 1 calc R . . H31 H 0.1814 0.5821 0.2048 0.125 Uiso 1 1 calc R . . H32 H 0.2258 0.4867 0.1611 0.125 Uiso 1 1 calc R . . C17 C 0.0529(4) 0.8139(5) 0.0728(3) 0.0908(16) Uani 1 1 d . . . H33 H 0.0468 0.8700 0.0247 0.136 Uiso 1 1 calc R . . H34 H 0.0664 0.8483 0.1104 0.136 Uiso 1 1 calc R . . H35 H -0.0199 0.7935 0.0819 0.136 Uiso 1 1 calc R . . C18 C 0.4781(4) 0.8538(4) -0.0334(3) 0.0787(14) Uani 1 1 d . . . H36 H 0.4708 0.9241 -0.0737 0.118 Uiso 1 1 calc R . . H37 H 0.5145 0.7853 -0.0505 0.118 Uiso 1 1 calc R . . H38 H 0.5267 0.8531 0.0065 0.118 Uiso 1 1 calc R . . C19 C 0.2409(5) 0.8746(5) -0.0869(3) 0.0953(17) Uani 1 1 d . . . H39 H 0.2463 0.9452 -0.1232 0.143 Uiso 1 1 calc R . . H40 H 0.1588 0.8825 -0.0761 0.143 Uiso 1 1 calc R . . H41 H 0.2737 0.8079 -0.1063 0.143 Uiso 1 1 calc R . . C20 C 0.2609(5) 0.9835(4) 0.0358(3) 0.0856(15) Uani 1 1 d . . . H42 H 0.3171 0.9873 0.0697 0.128 Uiso 1 1 calc R . . H43 H 0.1894 0.9773 0.0611 0.128 Uiso 1 1 calc R . . H44 H 0.2423 1.0540 -0.0054 0.128 Uiso 1 1 calc R . . C21 C 0.4742(5) 0.9514(8) 0.3393(5) 0.169(4) Uani 1 1 d . . . H45 H 0.5393 0.9628 0.3620 0.253 Uiso 1 1 calc R . . H46 H 0.4680 0.9915 0.2870 0.253 Uiso 1 1 calc R . . H47 H 0.4882 0.8683 0.3463 0.253 Uiso 1 1 calc R . . C22 C 0.3470(9) 0.9293(7) 0.4840(4) 0.187(5) Uani 1 1 d . . . H48 H 0.3699 0.8458 0.4893 0.281 Uiso 1 1 calc R . . H49 H 0.2717 0.9529 0.5063 0.281 Uiso 1 1 calc R . . H50 H 0.4064 0.9464 0.5085 0.281 Uiso 1 1 calc R . . C23 C 0.3285(6) 1.1632(5) 0.3848(4) 0.113(2) Uani 1 1 d . . . H51 H 0.2596 1.1956 0.4105 0.169 Uiso 1 1 calc R . . H52 H 0.3240 1.2131 0.3347 0.169 Uiso 1 1 calc R . . H53 H 0.3992 1.1590 0.4102 0.169 Uiso 1 1 calc R . . C24 C 0.2808(5) 1.1552(5) 0.1876(3) 0.0981(18) Uani 1 1 d . . . H54 H 0.2530 1.2144 0.1411 0.147 Uiso 1 1 calc R . . H55 H 0.3210 1.0806 0.1782 0.147 Uiso 1 1 calc R . . H56 H 0.3350 1.1776 0.2128 0.147 Uiso 1 1 calc R . . C25 C 0.0402(4) 1.1255(5) 0.1859(3) 0.0886(16) Uani 1 1 d . . . H57 H -0.0327 1.1273 0.2114 0.133 Uiso 1 1 calc R . . H58 H 0.0715 1.0515 0.1740 0.133 Uiso 1 1 calc R . . H59 H 0.0248 1.1894 0.1407 0.133 Uiso 1 1 calc R . . C26 C 0.0783(6) 1.2846(4) 0.2692(4) 0.109(2) Uani 1 1 d . . . H60 H 0.1365 1.3065 0.2914 0.163 Uiso 1 1 calc R . . H61 H 0.0162 1.2757 0.3035 0.163 Uiso 1 1 calc R . . H62 H 0.0446 1.3452 0.2243 0.163 Uiso 1 1 calc R . . C27 C 0.3293(5) 0.6297(5) 0.4719(3) 0.0982(18) Uani 1 1 d . . . H63 H 0.3386 0.6778 0.5021 0.147 Uiso 1 1 calc R . . H64 H 0.3699 0.6472 0.4263 0.147 Uiso 1 1 calc R . . H65 H 0.3626 0.5476 0.4984 0.147 Uiso 1 1 calc R . . C28 C 0.1540(5) 0.5505(4) 0.4039(4) 0.1051(19) Uani 1 1 d . . . H66 H 0.1871 0.5652 0.3555 0.158 Uiso 1 1 calc R . . H67 H 0.0715 0.5565 0.3988 0.158 Uiso 1 1 calc R . . H68 H 0.1967 0.4724 0.4337 0.158 Uiso 1 1 calc R . . C29 C 0.0968(6) 0.6380(5) 0.5435(3) 0.109(2) Uani 1 1 d . . . H69 H 0.1264 0.5559 0.5710 0.163 Uiso 1 1 calc R . . H70 H 0.0118 0.6603 0.5363 0.163 Uiso 1 1 calc R . . H71 H 0.1164 0.6854 0.5708 0.163 Uiso 1 1 calc R . . C30 C -0.1458(5) 0.7557(5) 0.4227(3) 0.0896(16) Uani 1 1 d . . . H72 H -0.2252 0.7739 0.4031 0.134 Uiso 1 1 calc R . . H73 H -0.1491 0.7812 0.4669 0.134 Uiso 1 1 calc R . . H74 H -0.1074 0.6718 0.4348 0.134 Uiso 1 1 calc R . . C31 C -0.0486(5) 0.7799(8) 0.2684(3) 0.141(3) Uani 1 1 d . . . H75 H -0.1266 0.7832 0.2534 0.212 Uiso 1 1 calc R . . H76 H 0.0027 0.6996 0.2800 0.212 Uiso 1 1 calc R . . H77 H -0.0165 0.8287 0.2285 0.212 Uiso 1 1 calc R . . C32 C -0.1597(5) 0.9905(5) 0.3241(5) 0.151(4) Uani 1 1 d . . . H78 H -0.1253 1.0377 0.2848 0.227 Uiso 1 1 calc R . . H79 H -0.1694 1.0215 0.3664 0.227 Uiso 1 1 calc R . . H80 H -0.2360 0.9924 0.3072 0.227 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1A 0.0477(5) 0.0702(6) 0.0628(6) -0.0389(5) 0.0076(4) -0.0174(4) Ge1B 0.0704(13) 0.0484(11) 0.0490(11) -0.0202(9) 0.0101(9) -0.0070(9) Ge1C 0.0529(17) 0.068(2) 0.056(2) -0.0313(15) 0.0098(14) -0.0194(15) Ge1D 0.0667(14) 0.0571(12) 0.0471(11) -0.0159(9) 0.0081(9) -0.0049(10) Si1 0.0470(6) 0.0476(6) 0.0481(6) -0.0201(4) -0.0003(4) -0.0081(4) Si2 0.0493(6) 0.0573(6) 0.0521(6) -0.0241(5) 0.0085(5) -0.0154(5) Si3 0.0642(7) 0.0421(6) 0.0757(8) -0.0110(5) -0.0143(6) -0.0110(5) Si4 0.0570(7) 0.0578(7) 0.0866(9) -0.0158(6) -0.0201(6) -0.0206(6) Si5 0.0426(6) 0.0689(7) 0.0734(8) -0.0221(6) -0.0047(5) -0.0170(5) Si6 0.0552(6) 0.0583(7) 0.0507(6) -0.0111(5) -0.0043(5) -0.0133(5) Si7 0.0825(10) 0.0970(11) 0.1008(11) -0.0397(9) -0.0220(8) -0.0344(8) Si8 0.0595(7) 0.0615(7) 0.0719(8) -0.0140(6) 0.0083(6) -0.0250(6) Si9 0.0759(9) 0.0615(7) 0.0638(8) -0.0046(6) -0.0032(6) -0.0173(6) Si10 0.0513(7) 0.0811(9) 0.0702(8) -0.0083(7) 0.0065(6) -0.0242(6) C1 0.047(2) 0.0445(19) 0.050(2) -0.0171(16) -0.0050(16) -0.0136(16) C2 0.043(2) 0.050(2) 0.065(2) -0.0228(19) 0.0020(18) -0.0071(16) C3 0.051(2) 0.054(2) 0.052(2) -0.0284(18) -0.0003(17) -0.0105(17) C4 0.0373(18) 0.050(2) 0.050(2) -0.0194(16) -0.0017(15) -0.0093(15) C5 0.050(2) 0.059(2) 0.057(2) -0.0225(19) 0.0074(18) -0.0198(18) C6 0.093(3) 0.063(3) 0.074(3) -0.037(2) 0.032(3) -0.032(2) C7 0.098(4) 0.074(3) 0.064(3) -0.035(2) 0.030(2) -0.038(3) C8 0.059(2) 0.050(2) 0.045(2) -0.0155(17) 0.0049(17) -0.0185(18) C9 0.093(4) 0.051(3) 0.110(4) -0.016(3) -0.011(3) -0.027(3) C10 0.081(4) 0.055(3) 0.195(7) -0.012(4) -0.048(4) 0.001(3) C11 0.167(6) 0.071(3) 0.072(3) 0.001(3) -0.002(4) -0.037(4) C12 0.054(3) 0.116(5) 0.191(7) -0.052(5) -0.003(4) -0.030(3) C13 0.155(6) 0.087(4) 0.099(4) -0.003(3) -0.066(4) -0.056(4) C14 0.091(3) 0.071(3) 0.086(3) -0.012(2) -0.009(3) -0.048(3) C15 0.085(4) 0.141(5) 0.113(4) -0.063(4) -0.015(3) -0.049(4) C16 0.060(3) 0.072(3) 0.118(4) -0.015(3) 0.007(3) -0.033(2) C17 0.048(3) 0.094(4) 0.109(4) -0.009(3) 0.005(3) -0.008(2) C18 0.076(3) 0.080(3) 0.073(3) -0.003(2) 0.006(2) -0.033(3) C19 0.099(4) 0.118(4) 0.061(3) -0.004(3) -0.022(3) -0.037(3) C20 0.100(4) 0.056(3) 0.089(4) -0.012(2) 0.009(3) -0.016(3) C21 0.051(3) 0.213(8) 0.278(10) -0.149(8) -0.027(5) -0.013(4) C22 0.281(11) 0.175(7) 0.127(6) 0.018(5) -0.121(7) -0.135(8) C23 0.126(5) 0.125(5) 0.127(5) -0.058(4) 0.001(4) -0.074(4) C24 0.102(4) 0.134(5) 0.084(3) -0.031(3) 0.033(3) -0.074(4) C25 0.071(3) 0.091(4) 0.087(3) 0.003(3) -0.018(3) -0.023(3) C26 0.119(5) 0.061(3) 0.140(5) -0.022(3) 0.012(4) -0.026(3) C27 0.090(4) 0.097(4) 0.082(3) -0.004(3) -0.027(3) -0.006(3) C28 0.110(5) 0.057(3) 0.151(6) -0.033(3) 0.000(4) -0.024(3) C29 0.117(5) 0.115(5) 0.070(3) 0.013(3) 0.003(3) -0.036(4) C30 0.075(3) 0.105(4) 0.098(4) -0.022(3) 0.016(3) -0.050(3) C31 0.094(4) 0.285(10) 0.088(4) -0.080(5) 0.008(3) -0.094(6) C32 0.050(3) 0.099(5) 0.243(9) 0.037(5) 0.003(4) -0.013(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 Ge1A Ge1D 1.119(3) . ? Ge1A Ge1B 1.145(2) . ? Ge1A Ge1C 1.671(6) . ? Ge1A Si2 2.2263(14) . ? Ge1A Si1 2.2290(13) . ? Ge1B Ge1C 1.199(6) . ? Ge1B Ge1D 1.634(3) . ? Ge1B Si2 2.154(2) . ? Ge1B Si1 2.268(2) . ? Ge1C Ge1D 1.215(6) . ? Ge1C Si1 2.201(5) . ? Ge1C Si2 2.217(5) . ? Ge1D Si1 2.148(3) . ? Ge1D Si2 2.277(3) . ? Si1 C1 1.889(4) . ? Si1 C4 1.898(4) . ? Si2 C5 1.893(4) . ? Si2 C8 1.895(4) . ? Si3 C9 1.860(5) . ? Si3 C11 1.862(6) . ? Si3 C10 1.868(5) . ? Si3 C1 1.909(4) . ? Si4 C14 1.856(4) . ? Si4 C13 1.872(5) . ? Si4 C12 1.880(6) . ? Si4 C1 1.908(3) . ? Si5 C16 1.865(5) . ? Si5 C17 1.865(5) . ? Si5 C15 1.877(5) . ? Si5 C4 1.904(4) . ? Si6 C20 1.861(5) . ? Si6 C18 1.872(5) . ? Si6 C19 1.878(5) . ? Si6 C4 1.915(4) . ? Si7 C21 1.852(7) . ? Si7 C23 1.860(6) . ? Si7 C22 1.867(7) . ? Si7 C5 1.898(4) . ? Si8 C24 1.868(5) . ? Si8 C25 1.869(5) . ? Si8 C26 1.870(6) . ? Si8 C5 1.908(4) . ? Si9 C28 1.869(5) . ? Si9 C27 1.871(5) . ? Si9 C29 1.883(5) . ? Si9 C8 1.905(4) . ? Si10 C31 1.845(6) . ? Si10 C30 1.872(5) . ? Si10 C32 1.872(6) . ? Si10 C8 1.912(4) . ? C1 C2 1.565(5) . ? C2 C3 1.530(5) . ? C2 H1 0.9700 . ? C2 H2 0.9700 . ? C3 C4 1.564(5) . ? C3 H3 0.9700 . ? C3 H4 0.9700 . ? C5 C6 1.565(5) . ? C6 C7 1.535(6) . ? C6 H5 0.9700 . ? C6 H6 0.9700 . ? C7 C8 1.558(5) . ? C7 H7 0.9700 . ? C7 H8 0.9700 . ? C9 H9 0.9600 . ? C9 H10 0.9600 . ? C9 H11 0.9600 . ? C10 H12 0.9600 . ? C10 H13 0.9600 . ? C10 H14 0.9600 . ? C11 H15 0.9600 . ? C11 H16 0.9600 . ? C11 H17 0.9600 . ? C12 H18 0.9600 . ? C12 H19 0.9600 . ? C12 H20 0.9600 . ? C13 H21 0.9600 . ? C13 H22 0.9600 . ? C13 H23 0.9600 . ? C14 H24 0.9600 . ? C14 H25 0.9600 . ? C14 H26 0.9600 . ? C15 H27 0.9600 . ? C15 H28 0.9600 . ? C15 H29 0.9600 . ? C16 H30 0.9600 . ? C16 H31 0.9600 . ? C16 H32 0.9600 . ? C17 H33 0.9600 . ? C17 H34 0.9600 . ? C17 H35 0.9600 . ? C18 H36 0.9600 . ? C18 H37 0.9600 . ? C18 H38 0.9600 . ? C19 H39 0.9600 . ? C19 H40 0.9600 . ? C19 H41 0.9600 . ? C20 H42 0.9600 . ? C20 H43 0.9600 . ? C20 H44 0.9600 . ? C21 H45 0.9600 . ? C21 H46 0.9600 . ? C21 H47 0.9600 . ? C22 H48 0.9600 . ? C22 H49 0.9600 . ? C22 H50 0.9600 . ? C23 H51 0.9600 . ? C23 H52 0.9600 . ? C23 H53 0.9600 . ? C24 H54 0.9600 . ? C24 H55 0.9600 . ? C24 H56 0.9600 . ? C25 H57 0.9600 . ? C25 H58 0.9600 . ? C25 H59 0.9600 . ? C26 H60 0.9600 . ? C26 H61 0.9600 . ? C26 H62 0.9600 . ? C27 H63 0.9600 . ? C27 H64 0.9600 . ? C27 H65 0.9600 . ? C28 H66 0.9600 . ? C28 H67 0.9600 . ? C28 H68 0.9600 . ? C29 H69 0.9600 . ? C29 H70 0.9600 . ? C29 H71 0.9600 . ? C30 H72 0.9600 . ? C30 H73 0.9600 . ? C30 H74 0.9600 . ? C31 H75 0.9600 . ? C31 H76 0.9600 . ? C31 H77 0.9600 . ? C32 H78 0.9600 . ? C32 H79 0.9600 . ? C32 H80 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 Ge1A Si1 134.55(6) . . ? Si2 Ge1B Si1 136.64(11) . . ? Si1 Ge1C Si2 136.9(3) . . ? Si1 Ge1D Si2 136.44(12) . . ? C1 Si1 C4 99.96(15) . . ? C1 Si1 Ge1D 115.43(13) . . ? C4 Si1 Ge1D 142.89(14) . . ? C1 Si1 Ge1C 147.0(2) . . ? C4 Si1 Ge1C 110.69(19) . . ? C1 Si1 Ge1A 115.02(12) . . ? C4 Si1 Ge1A 139.34(12) . . ? C1 Si1 Ge1B 143.04(13) . . ? C4 Si1 Ge1B 110.83(13) . . ? C5 Si2 C8 99.93(17) . . ? C5 Si2 Ge1B 116.32(14) . . ? C8 Si2 Ge1B 141.75(14) . . ? C5 Si2 Ge1C 147.6(2) . . ? C8 Si2 Ge1C 110.40(19) . . ? C5 Si2 Ge1A 114.67(13) . . ? C8 Si2 Ge1A 139.80(13) . . ? Ge1B Si2 Ge1A 30.26(7) . . ? Ge1C Si2 Ge1A 44.19(15) . . ? C5 Si2 Ge1D 141.59(15) . . ? C8 Si2 Ge1D 111.80(14) . . ? Ge1B Si2 Ge1D 43.18(9) . . ? Ge1C Si2 Ge1D 31.33(16) . . ? Ge1A Si2 Ge1D 28.74(7) . . ? C9 Si3 C11 107.0(3) . . ? C9 Si3 C10 102.9(3) . . ? C11 Si3 C10 108.8(3) . . ? C9 Si3 C1 112.13(19) . . ? C11 Si3 C1 113.3(2) . . ? C10 Si3 C1 112.1(2) . . ? C14 Si4 C13 106.2(2) . . ? C14 Si4 C12 104.3(3) . . ? C13 Si4 C12 110.2(3) . . ? C14 Si4 C1 113.81(18) . . ? C13 Si4 C1 111.9(2) . . ? C12 Si4 C1 110.0(2) . . ? C16 Si5 C17 107.8(2) . . ? C16 Si5 C15 104.6(3) . . ? C17 Si5 C15 109.4(3) . . ? C16 Si5 C4 111.92(18) . . ? C17 Si5 C4 112.0(2) . . ? C15 Si5 C4 110.8(2) . . ? C20 Si6 C18 108.1(2) . . ? C20 Si6 C19 108.0(3) . . ? C18 Si6 C19 102.8(2) . . ? C20 Si6 C4 112.75(19) . . ? C18 Si6 C4 112.62(18) . . ? C19 Si6 C4 112.0(2) . . ? C21 Si7 C23 106.9(3) . . ? C21 Si7 C22 108.4(4) . . ? C23 Si7 C22 102.8(3) . . ? C21 Si7 C5 114.3(3) . . ? C23 Si7 C5 111.8(2) . . ? C22 Si7 C5 111.9(3) . . ? C24 Si8 C25 105.4(3) . . ? C24 Si8 C26 109.2(3) . . ? C25 Si8 C26 105.5(3) . . ? C24 Si8 C5 112.8(2) . . ? C25 Si8 C5 112.6(2) . . ? C26 Si8 C5 110.9(2) . . ? C28 Si9 C27 107.2(3) . . ? C28 Si9 C29 109.8(3) . . ? C27 Si9 C29 104.9(3) . . ? C28 Si9 C8 111.3(2) . . ? C27 Si9 C8 113.4(2) . . ? C29 Si9 C8 109.9(2) . . ? C31 Si10 C30 108.9(3) . . ? C31 Si10 C32 106.7(4) . . ? C30 Si10 C32 102.9(3) . . ? C31 Si10 C8 112.3(2) . . ? C30 Si10 C8 112.6(2) . . ? C32 Si10 C8 112.9(3) . . ? C2 C1 Si1 101.5(2) . . ? C2 C1 Si4 109.1(2) . . ? Si1 C1 Si4 111.83(18) . . ? C2 C1 Si3 110.2(2) . . ? Si1 C1 Si3 113.61(19) . . ? Si4 C1 Si3 110.19(17) . . ? C3 C2 C1 111.3(3) . . ? C3 C2 H1 109.4 . . ? C1 C2 H1 109.4 . . ? C3 C2 H2 109.4 . . ? C1 C2 H2 109.4 . . ? H1 C2 H2 108.0 . . ? C2 C3 C4 111.9(3) . . ? C2 C3 H3 109.2 . . ? C4 C3 H3 109.2 . . ? C2 C3 H4 109.2 . . ? C4 C3 H4 109.2 . . ? H3 C3 H4 107.9 . . ? C3 C4 Si1 100.3(2) . . ? C3 C4 Si5 109.3(2) . . ? Si1 C4 Si5 109.77(18) . . ? C3 C4 Si6 110.0(2) . . ? Si1 C4 Si6 115.55(18) . . ? Si5 C4 Si6 111.31(17) . . ? C6 C5 Si2 100.9(2) . . ? C6 C5 Si7 109.9(3) . . ? Si2 C5 Si7 116.9(2) . . ? C6 C5 Si8 108.0(3) . . ? Si2 C5 Si8 109.7(2) . . ? Si7 C5 Si8 110.69(19) . . ? C7 C6 C5 111.1(3) . . ? C7 C6 H5 109.4 . . ? C5 C6 H5 109.4 . . ? C7 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? H5 C6 H6 108.0 . . ? C6 C7 C8 112.1(3) . . ? C6 C7 H7 109.2 . . ? C8 C7 H7 109.2 . . ? C6 C7 H8 109.2 . . ? C8 C7 H8 109.2 . . ? H7 C7 H8 107.9 . . ? C7 C8 Si2 101.0(2) . . ? C7 C8 Si9 109.9(3) . . ? Si2 C8 Si9 111.8(2) . . ? C7 C8 Si10 109.3(3) . . ? Si2 C8 Si10 113.95(19) . . ? Si9 C8 Si10 110.43(19) . . ? Si3 C9 H9 109.5 . . ? Si3 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? Si3 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? Si3 C10 H12 109.5 . . ? Si3 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? Si3 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? Si3 C11 H15 109.5 . . ? Si3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? Si3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? Si4 C12 H18 109.5 . . ? Si4 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? Si4 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? Si4 C13 H21 109.5 . . ? Si4 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? Si4 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? Si4 C14 H24 109.5 . . ? Si4 C14 H25 109.5 . . ? H24 C14 H25 109.5 . . ? Si4 C14 H26 109.5 . . ? H24 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? Si5 C15 H27 109.5 . . ? Si5 C15 H28 109.5 . . ? H27 C15 H28 109.5 . . ? Si5 C15 H29 109.5 . . ? H27 C15 H29 109.5 . . ? H28 C15 H29 109.5 . . ? Si5 C16 H30 109.5 . . ? Si5 C16 H31 109.5 . . ? H30 C16 H31 109.5 . . ? Si5 C16 H32 109.5 . . ? H30 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? Si5 C17 H33 109.5 . . ? Si5 C17 H34 109.5 . . ? H33 C17 H34 109.5 . . ? Si5 C17 H35 109.5 . . ? H33 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? Si6 C18 H36 109.5 . . ? Si6 C18 H37 109.5 . . ? H36 C18 H37 109.5 . . ? Si6 C18 H38 109.5 . . ? H36 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? Si6 C19 H39 109.5 . . ? Si6 C19 H40 109.5 . . ? H39 C19 H40 109.5 . . ? Si6 C19 H41 109.5 . . ? H39 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si6 C20 H42 109.5 . . ? Si6 C20 H43 109.5 . . ? H42 C20 H43 109.5 . . ? Si6 C20 H44 109.5 . . ? H42 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si7 C21 H45 109.5 . . ? Si7 C21 H46 109.5 . . ? H45 C21 H46 109.5 . . ? Si7 C21 H47 109.5 . . ? H45 C21 H47 109.5 . . ? H46 C21 H47 109.5 . . ? Si7 C22 H48 109.5 . . ? Si7 C22 H49 109.5 . . ? H48 C22 H49 109.5 . . ? Si7 C22 H50 109.5 . . ? H48 C22 H50 109.5 . . ? H49 C22 H50 109.5 . . ? Si7 C23 H51 109.5 . . ? Si7 C23 H52 109.5 . . ? H51 C23 H52 109.5 . . ? Si7 C23 H53 109.5 . . ? H51 C23 H53 109.5 . . ? H52 C23 H53 109.5 . . ? Si8 C24 H54 109.5 . . ? Si8 C24 H55 109.5 . . ? H54 C24 H55 109.5 . . ? Si8 C24 H56 109.5 . . ? H54 C24 H56 109.5 . . ? H55 C24 H56 109.5 . . ? Si8 C25 H57 109.5 . . ? Si8 C25 H58 109.5 . . ? H57 C25 H58 109.5 . . ? Si8 C25 H59 109.5 . . ? H57 C25 H59 109.5 . . ? H58 C25 H59 109.5 . . ? Si8 C26 H60 109.5 . . ? Si8 C26 H61 109.5 . . ? H60 C26 H61 109.5 . . ? Si8 C26 H62 109.5 . . ? H60 C26 H62 109.5 . . ? H61 C26 H62 109.5 . . ? Si9 C27 H63 109.5 . . ? Si9 C27 H64 109.5 . . ? H63 C27 H64 109.5 . . ? Si9 C27 H65 109.5 . . ? H63 C27 H65 109.5 . . ? H64 C27 H65 109.5 . . ? Si9 C28 H66 109.5 . . ? Si9 C28 H67 109.5 . . ? H66 C28 H67 109.5 . . ? Si9 C28 H68 109.5 . . ? H66 C28 H68 109.5 . . ? H67 C28 H68 109.5 . . ? Si9 C29 H69 109.5 . . ? Si9 C29 H70 109.5 . . ? H69 C29 H70 109.5 . . ? Si9 C29 H71 109.5 . . ? H69 C29 H71 109.5 . . ? H70 C29 H71 109.5 . . ? Si10 C30 H72 109.5 . . ? Si10 C30 H73 109.5 . . ? H72 C30 H73 109.5 . . ? Si10 C30 H74 109.5 . . ? H72 C30 H74 109.5 . . ? H73 C30 H74 109.5 . . ? Si10 C31 H75 109.5 . . ? Si10 C31 H76 109.5 . . ? H75 C31 H76 109.5 . . ? Si10 C31 H77 109.5 . . ? H75 C31 H77 109.5 . . ? H76 C31 H77 109.5 . . ? Si10 C32 H78 109.5 . . ? Si10 C32 H79 109.5 . . ? H78 C32 H79 109.5 . . ? Si10 C32 H80 109.5 . . ? H78 C32 H80 109.5 . . ? H79 C32 H80 109.5 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.324 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.051 data_2-germadisilaallene_crystal_C_093K _database_code_depnum_ccdc_archive 'CCDC 279208' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C32 H80 Ge Si10 ' _chemical_formula_moiety 'C32 H80 Ge Si10 ' _chemical_melting_point ? _chemical_formula_weight 818.45 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.683(3) _cell_length_b 12.214(3) _cell_length_c 18.607(4) _cell_angle_alpha 73.588(7) _cell_angle_beta 87.156(8) _cell_angle_gamma 71.628(7) _cell_volume 2414.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 93.0(2) _cell_measurement_reflns_used 7294 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 55.0 _exptl_crystal_description prism _exptl_crystal_colour dark_green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.7735 _exptl_absorpt_correction_T_max 0.9152 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37880 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10992 _reflns_number_gt 10291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+1.8542P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10992 _refine_ls_number_parameters 433 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1A Ge 0.85486(2) 0.29192(2) 0.255748(13) 0.01816(7) Uani 0.9499(8) 1 d PU . . Ge1B Ge 0.8223(5) 0.2110(5) 0.2791(3) 0.0224(14) Uani 0.0384(8) 1 d PU . . Ge1C Ge 0.7707(17) 0.3473(18) 0.2117(11) 0.022(2) Uani 0.0116(6) 1 d PU . . Si1 Si 0.69112(5) 0.37281(5) 0.31373(3) 0.01417(11) Uani 1 1 d U . . Si2 Si 0.88427(5) 0.18358(5) 0.17370(3) 0.01345(11) Uani 1 1 d U . . Si3 Si 0.65753(5) 0.64256(5) 0.24898(3) 0.02029(12) Uani 1 1 d . . . Si4 Si 0.82033(5) 0.50874(6) 0.39735(4) 0.02395(13) Uani 1 1 d . . . Si5 Si 0.44050(5) 0.31864(5) 0.34458(3) 0.01769(12) Uani 1 1 d . . . Si6 Si 0.66932(5) 0.15793(5) 0.44959(3) 0.02013(12) Uani 1 1 d . . . Si7 Si 1.16359(5) 0.14268(5) 0.19592(3) 0.01793(12) Uani 1 1 d . . . Si8 Si 1.06610(5) -0.07725(5) 0.23810(3) 0.01831(12) Uani 1 1 d . . . Si9 Si 0.82469(5) 0.35579(5) 0.00326(3) 0.01611(11) Uani 1 1 d . . . Si10 Si 0.67641(5) 0.18010(5) 0.07708(3) 0.01648(11) Uani 1 1 d . . . C1 C 0.68695(17) 0.51381(17) 0.33956(11) 0.0160(4) Uani 1 1 d . . . C2 C 0.56970(18) 0.53139(18) 0.38590(11) 0.0175(4) Uani 1 1 d . . . H1 H 0.5716 0.5812 0.4193 0.021 Uiso 1 1 calc R . . H2 H 0.4979 0.5742 0.3512 0.021 Uiso 1 1 calc R . . C3 C 0.56003(18) 0.40909(18) 0.43322(11) 0.0178(4) Uani 1 1 d . . . H3 H 0.4775 0.4203 0.4520 0.021 Uiso 1 1 calc R . . H4 H 0.6175 0.3773 0.4771 0.021 Uiso 1 1 calc R . . C4 C 0.58819(17) 0.31533(17) 0.38628(10) 0.0155(4) Uani 1 1 d . . . C5 C 1.04364(17) 0.08011(16) 0.17245(11) 0.0144(4) Uani 1 1 d . . . C6 C 1.05270(17) 0.07700(18) 0.08862(11) 0.0168(4) Uani 1 1 d . . . H5 H 1.0878 0.1392 0.0595 0.020 Uiso 1 1 calc R . . H6 H 1.1071 -0.0023 0.0861 0.020 Uiso 1 1 calc R . . C7 C 0.92761(17) 0.09958(17) 0.05364(11) 0.0164(4) Uani 1 1 d . . . H7 H 0.9040 0.0257 0.0716 0.020 Uiso 1 1 calc R . . H8 H 0.9321 0.1184 -0.0016 0.020 Uiso 1 1 calc R . . C8 C 0.82892(16) 0.20658(17) 0.07460(10) 0.0140(4) Uani 1 1 d . . . C9 C 0.5850(2) 0.7914(2) 0.26837(14) 0.0328(5) Uani 1 1 d . . . H9 H 0.6464 0.8156 0.2883 0.049 Uiso 1 1 calc R . . H10 H 0.5229 0.7843 0.3052 0.049 Uiso 1 1 calc R . . H11 H 0.5480 0.8520 0.2218 0.049 Uiso 1 1 calc R . . C10 C 0.5464(2) 0.6334(2) 0.18305(12) 0.0270(5) Uani 1 1 d . . . H12 H 0.5437 0.6925 0.1344 0.041 Uiso 1 1 calc R . . H13 H 0.4661 0.6503 0.2040 0.041 Uiso 1 1 calc R . . H14 H 0.5715 0.5525 0.1764 0.041 Uiso 1 1 calc R . . C11 C 0.7988(2) 0.6426(2) 0.19723(13) 0.0304(5) Uani 1 1 d . . . H15 H 0.7798 0.7078 0.1503 0.046 Uiso 1 1 calc R . . H16 H 0.8341 0.5654 0.1860 0.046 Uiso 1 1 calc R . . H17 H 0.8566 0.6546 0.2283 0.046 Uiso 1 1 calc R . . C12 C 0.8213(2) 0.6643(2) 0.39312(15) 0.0344(6) Uani 1 1 d . . . H18 H 0.8843 0.6587 0.4281 0.052 Uiso 1 1 calc R . . H19 H 0.7426 0.7102 0.4070 0.052 Uiso 1 1 calc R . . H20 H 0.8375 0.7050 0.3421 0.052 Uiso 1 1 calc R . . C13 C 0.9721(2) 0.4277(3) 0.36925(16) 0.0409(7) Uani 1 1 d . . . H21 H 1.0349 0.4403 0.3960 0.061 Uiso 1 1 calc R . . H22 H 0.9786 0.4589 0.3151 0.061 Uiso 1 1 calc R . . H23 H 0.9822 0.3416 0.3819 0.061 Uiso 1 1 calc R . . C14 C 0.8112(2) 0.4390(2) 0.50055(13) 0.0323(5) Uani 1 1 d . . . H24 H 0.8169 0.3544 0.5095 0.048 Uiso 1 1 calc R . . H25 H 0.7341 0.4819 0.5180 0.048 Uiso 1 1 calc R . . H26 H 0.8778 0.4443 0.5280 0.048 Uiso 1 1 calc R . . C15 C 0.3489(2) 0.2490(2) 0.41840(12) 0.0241(4) Uani 1 1 d . . . H27 H 0.2702 0.2604 0.3963 0.036 Uiso 1 1 calc R . . H28 H 0.3374 0.2875 0.4590 0.036 Uiso 1 1 calc R . . H29 H 0.3915 0.1629 0.4384 0.036 Uiso 1 1 calc R . . C16 C 0.3386(2) 0.4756(2) 0.30300(13) 0.0273(5) Uani 1 1 d . . . H30 H 0.3765 0.5160 0.2599 0.041 Uiso 1 1 calc R . . H31 H 0.3247 0.5198 0.3408 0.041 Uiso 1 1 calc R . . H32 H 0.2614 0.4730 0.2865 0.041 Uiso 1 1 calc R . . C17 C 0.4685(2) 0.2400(2) 0.26946(13) 0.0297(5) Uani 1 1 d . . . H33 H 0.3995 0.2753 0.2332 0.044 Uiso 1 1 calc R . . H34 H 0.4788 0.1544 0.2920 0.044 Uiso 1 1 calc R . . H35 H 0.5417 0.2489 0.2439 0.044 Uiso 1 1 calc R . . C18 C 0.8334(2) 0.1289(2) 0.47048(13) 0.0293(5) Uani 1 1 d . . . H36 H 0.8424 0.1915 0.4910 0.044 Uiso 1 1 calc R . . H37 H 0.8774 0.1300 0.4242 0.044 Uiso 1 1 calc R . . H38 H 0.8661 0.0502 0.5071 0.044 Uiso 1 1 calc R . . C19 C 0.5976(2) 0.1396(2) 0.54300(12) 0.0314(5) Uani 1 1 d . . . H39 H 0.6274 0.0551 0.5727 0.047 Uiso 1 1 calc R . . H40 H 0.5098 0.1641 0.5354 0.047 Uiso 1 1 calc R . . H41 H 0.6184 0.1898 0.5697 0.047 Uiso 1 1 calc R . . C20 C 0.6634(2) 0.0369(2) 0.40829(14) 0.0292(5) Uani 1 1 d . . . H42 H 0.7154 -0.0410 0.4387 0.044 Uiso 1 1 calc R . . H43 H 0.6914 0.0529 0.3570 0.044 Uiso 1 1 calc R . . H44 H 0.5801 0.0352 0.4075 0.044 Uiso 1 1 calc R . . C21 C 1.1879(2) 0.1117(2) 0.29937(13) 0.0282(5) Uani 1 1 d . . . H45 H 1.2542 0.1396 0.3088 0.042 Uiso 1 1 calc R . . H46 H 1.2082 0.0251 0.3234 0.042 Uiso 1 1 calc R . . H47 H 1.1140 0.1543 0.3200 0.042 Uiso 1 1 calc R . . C22 C 1.3092(2) 0.0763(2) 0.15332(16) 0.0347(6) Uani 1 1 d . . . H48 H 1.2986 0.1036 0.0985 0.052 Uiso 1 1 calc R . . H49 H 1.3321 -0.0116 0.1703 0.052 Uiso 1 1 calc R . . H50 H 1.3728 0.1023 0.1689 0.052 Uiso 1 1 calc R . . C23 C 1.1307(2) 0.30885(19) 0.15543(12) 0.0242(5) Uani 1 1 d . . . H51 H 1.0493 0.3507 0.1682 0.036 Uiso 1 1 calc R . . H52 H 1.1355 0.3280 0.1008 0.036 Uiso 1 1 calc R . . H53 H 1.1898 0.3348 0.1761 0.036 Uiso 1 1 calc R . . C24 C 1.2296(2) -0.1702(2) 0.25345(16) 0.0358(6) Uani 1 1 d . . . H54 H 1.2730 -0.1325 0.2778 0.054 Uiso 1 1 calc R . . H55 H 1.2645 -0.1754 0.2051 0.054 Uiso 1 1 calc R . . H56 H 1.2367 -0.2511 0.2856 0.054 Uiso 1 1 calc R . . C25 C 0.9991(2) -0.0769(2) 0.33117(13) 0.0332(5) Uani 1 1 d . . . H57 H 0.9109 -0.0454 0.3247 0.050 Uiso 1 1 calc R . . H58 H 1.0281 -0.0259 0.3531 0.050 Uiso 1 1 calc R . . H59 H 1.0230 -0.1591 0.3645 0.050 Uiso 1 1 calc R . . C26 C 0.9978(2) -0.16692(19) 0.19673(14) 0.0277(5) Uani 1 1 d . . . H60 H 1.0202 -0.2501 0.2287 0.042 Uiso 1 1 calc R . . H61 H 1.0278 -0.1659 0.1465 0.042 Uiso 1 1 calc R . . H62 H 0.9097 -0.1317 0.1933 0.042 Uiso 1 1 calc R . . C27 C 0.7611(2) 0.48691(18) 0.04174(12) 0.0243(5) Uani 1 1 d . . . H63 H 0.8153 0.4810 0.0821 0.036 Uiso 1 1 calc R . . H64 H 0.6817 0.4871 0.0615 0.036 Uiso 1 1 calc R . . H65 H 0.7527 0.5615 0.0018 0.036 Uiso 1 1 calc R . . C28 C 0.7342(2) 0.3838(2) -0.08473(12) 0.0258(5) Uani 1 1 d . . . H66 H 0.6501 0.3903 -0.0725 0.039 Uiso 1 1 calc R . . H67 H 0.7680 0.3170 -0.1067 0.039 Uiso 1 1 calc R . . H68 H 0.7372 0.4588 -0.1207 0.039 Uiso 1 1 calc R . . C29 C 0.9773(2) 0.3566(2) -0.03275(13) 0.0263(5) Uani 1 1 d . . . H69 H 0.9695 0.4321 -0.0718 0.040 Uiso 1 1 calc R . . H70 H 1.0117 0.2887 -0.0538 0.040 Uiso 1 1 calc R . . H71 H 1.0306 0.3495 0.0085 0.040 Uiso 1 1 calc R . . C30 C 0.66908(19) 0.05559(19) 0.16143(12) 0.0233(4) Uani 1 1 d . . . H72 H 0.6946 0.0699 0.2064 0.035 Uiso 1 1 calc R . . H73 H 0.7227 -0.0211 0.1558 0.035 Uiso 1 1 calc R . . H74 H 0.5861 0.0528 0.1662 0.035 Uiso 1 1 calc R . . C31 C 0.54958(19) 0.3189(2) 0.07754(13) 0.0254(5) Uani 1 1 d . . . H75 H 0.4744 0.2988 0.0881 0.038 Uiso 1 1 calc R . . H76 H 0.5410 0.3784 0.0285 0.038 Uiso 1 1 calc R . . H77 H 0.5668 0.3523 0.1164 0.038 Uiso 1 1 calc R . . C32 C 0.6521(2) 0.1265(2) -0.00436(13) 0.0284(5) Uani 1 1 d . . . H78 H 0.5720 0.1164 -0.0024 0.043 Uiso 1 1 calc R . . H79 H 0.7139 0.0494 -0.0018 0.043 Uiso 1 1 calc R . . H80 H 0.6578 0.1858 -0.0514 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1A 0.01471(12) 0.02440(13) 0.01977(12) -0.01370(10) 0.00317(8) -0.00589(9) Ge1B 0.025(3) 0.022(2) 0.017(2) -0.0065(18) 0.005(2) -0.0044(19) Ge1C 0.019(4) 0.024(4) 0.020(3) -0.009(3) 0.004(3) 0.002(4) Si1 0.0133(3) 0.0162(3) 0.0137(2) -0.0059(2) 0.00083(19) -0.0042(2) Si2 0.0126(2) 0.0139(2) 0.0138(2) -0.0055(2) 0.00001(19) -0.0026(2) Si3 0.0199(3) 0.0186(3) 0.0231(3) -0.0046(2) 0.0054(2) -0.0087(2) Si4 0.0170(3) 0.0310(3) 0.0304(3) -0.0188(3) -0.0005(2) -0.0074(2) Si5 0.0156(3) 0.0228(3) 0.0158(3) -0.0044(2) 0.0016(2) -0.0087(2) Si6 0.0214(3) 0.0173(3) 0.0181(3) -0.0016(2) -0.0015(2) -0.0039(2) Si7 0.0137(3) 0.0180(3) 0.0240(3) -0.0081(2) -0.0017(2) -0.0052(2) Si8 0.0172(3) 0.0132(3) 0.0233(3) -0.0044(2) -0.0031(2) -0.0031(2) Si9 0.0173(3) 0.0170(3) 0.0140(3) -0.0038(2) 0.0000(2) -0.0057(2) Si10 0.0128(3) 0.0186(3) 0.0188(3) -0.0059(2) -0.0004(2) -0.0053(2) C1 0.0141(9) 0.0193(10) 0.0173(9) -0.0082(8) 0.0028(7) -0.0064(8) C2 0.0177(10) 0.0187(10) 0.0176(10) -0.0087(8) 0.0041(7) -0.0051(8) C3 0.0178(10) 0.0210(10) 0.0150(9) -0.0064(8) 0.0032(7) -0.0060(8) C4 0.0146(9) 0.0174(9) 0.0132(9) -0.0039(7) 0.0004(7) -0.0038(7) C5 0.0133(9) 0.0133(9) 0.0171(9) -0.0065(7) 0.0004(7) -0.0028(7) C6 0.0141(9) 0.0185(9) 0.0187(10) -0.0076(8) 0.0021(7) -0.0043(8) C7 0.0164(9) 0.0163(9) 0.0176(10) -0.0081(8) 0.0010(7) -0.0037(8) C8 0.0123(9) 0.0153(9) 0.0155(9) -0.0068(7) 0.0012(7) -0.0035(7) C9 0.0361(13) 0.0210(11) 0.0403(14) -0.0066(10) 0.0109(11) -0.0105(10) C10 0.0245(11) 0.0274(12) 0.0237(11) 0.0007(9) -0.0009(9) -0.0073(9) C11 0.0305(12) 0.0376(13) 0.0306(12) -0.0126(10) 0.0110(10) -0.0196(11) C12 0.0361(14) 0.0416(14) 0.0385(14) -0.0226(12) 0.0039(11) -0.0204(12) C13 0.0176(11) 0.0598(18) 0.0576(17) -0.0408(15) -0.0024(11) -0.0070(11) C14 0.0315(13) 0.0369(13) 0.0307(13) -0.0138(11) -0.0109(10) -0.0079(11) C15 0.0247(11) 0.0274(11) 0.0238(11) -0.0077(9) 0.0054(9) -0.0133(9) C16 0.0208(11) 0.0298(12) 0.0267(12) 0.0027(9) -0.0050(9) -0.0098(9) C17 0.0248(12) 0.0498(15) 0.0249(11) -0.0178(11) 0.0052(9) -0.0204(11) C18 0.0256(12) 0.0251(11) 0.0298(12) -0.0034(10) -0.0077(9) -0.0002(9) C19 0.0352(13) 0.0322(13) 0.0187(11) 0.0031(9) 0.0008(9) -0.0085(11) C20 0.0301(12) 0.0204(11) 0.0355(13) -0.0075(10) 0.0022(10) -0.0060(9) C21 0.0303(12) 0.0276(12) 0.0294(12) -0.0066(10) -0.0113(9) -0.0124(10) C22 0.0166(11) 0.0384(14) 0.0581(17) -0.0262(13) 0.0057(10) -0.0106(10) C23 0.0261(11) 0.0230(11) 0.0273(11) -0.0057(9) -0.0008(9) -0.0139(9) C24 0.0222(12) 0.0181(11) 0.0604(17) -0.0070(11) -0.0103(11) 0.0010(9) C25 0.0468(15) 0.0230(11) 0.0245(12) -0.0013(9) 0.0012(10) -0.0083(11) C26 0.0286(12) 0.0168(10) 0.0379(13) -0.0051(9) -0.0061(10) -0.0088(9) C27 0.0313(12) 0.0156(10) 0.0231(11) -0.0042(8) -0.0006(9) -0.0042(9) C28 0.0281(12) 0.0306(12) 0.0172(10) -0.0027(9) -0.0028(9) -0.0101(10) C29 0.0242(11) 0.0268(11) 0.0268(11) -0.0019(9) 0.0032(9) -0.0116(9) C30 0.0170(10) 0.0205(10) 0.0316(12) -0.0043(9) 0.0029(8) -0.0079(8) C31 0.0167(10) 0.0260(11) 0.0282(12) -0.0038(9) 0.0028(8) -0.0029(9) C32 0.0271(12) 0.0363(13) 0.0286(12) -0.0134(10) -0.0026(9) -0.0150(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1A Si2 2.2366(7) . ? Ge1A Si1 2.2373(7) . ? Ge1B Si2 2.136(6) . ? Ge1B Si1 2.319(6) . ? Ge1C Si1 2.130(18) . ? Ge1C Si2 2.301(18) . ? Si1 C4 1.896(2) . ? Si1 C1 1.900(2) . ? Si2 C5 1.8956(19) . ? Si2 C8 1.900(2) . ? Si3 C11 1.869(2) . ? Si3 C9 1.877(2) . ? Si3 C10 1.879(2) . ? Si3 C1 1.911(2) . ? Si4 C13 1.868(2) . ? Si4 C14 1.881(3) . ? Si4 C12 1.883(2) . ? Si4 C1 1.912(2) . ? Si5 C17 1.871(2) . ? Si5 C16 1.872(2) . ? Si5 C15 1.877(2) . ? Si5 C4 1.911(2) . ? Si6 C20 1.869(2) . ? Si6 C18 1.876(2) . ? Si6 C19 1.878(2) . ? Si6 C4 1.914(2) . ? Si7 C21 1.872(2) . ? Si7 C23 1.873(2) . ? Si7 C22 1.882(2) . ? Si7 C5 1.914(2) . ? Si8 C25 1.865(2) . ? Si8 C26 1.875(2) . ? Si8 C24 1.877(2) . ? Si8 C5 1.908(2) . ? Si9 C27 1.864(2) . ? Si9 C29 1.876(2) . ? Si9 C28 1.882(2) . ? Si9 C8 1.915(2) . ? Si10 C31 1.869(2) . ? Si10 C30 1.872(2) . ? Si10 C32 1.878(2) . ? Si10 C8 1.905(2) . ? C1 C2 1.571(3) . ? C2 C3 1.540(3) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.575(3) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C5 C6 1.568(3) . ? C6 C7 1.541(3) . ? C6 H5 0.9900 . ? C6 H6 0.9900 . ? C7 C8 1.576(3) . ? C7 H7 0.9900 . ? C7 H8 0.9900 . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C9 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C11 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C12 H20 0.9800 . ? C13 H21 0.9800 . ? C13 H22 0.9800 . ? C13 H23 0.9800 . ? C14 H24 0.9800 . ? C14 H25 0.9800 . ? C14 H26 0.9800 . ? C15 H27 0.9800 . ? C15 H28 0.9800 . ? C15 H29 0.9800 . ? C16 H30 0.9800 . ? C16 H31 0.9800 . ? C16 H32 0.9800 . ? C17 H33 0.9800 . ? C17 H34 0.9800 . ? C17 H35 0.9800 . ? C18 H36 0.9800 . ? C18 H37 0.9800 . ? C18 H38 0.9800 . ? C19 H39 0.9800 . ? C19 H40 0.9800 . ? C19 H41 0.9800 . ? C20 H42 0.9800 . ? C20 H43 0.9800 . ? C20 H44 0.9800 . ? C21 H45 0.9800 . ? C21 H46 0.9800 . ? C21 H47 0.9800 . ? C22 H48 0.9800 . ? C22 H49 0.9800 . ? C22 H50 0.9800 . ? C23 H51 0.9800 . ? C23 H52 0.9800 . ? C23 H53 0.9800 . ? C24 H54 0.9800 . ? C24 H55 0.9800 . ? C24 H56 0.9800 . ? C25 H57 0.9800 . ? C25 H58 0.9800 . ? C25 H59 0.9800 . ? C26 H60 0.9800 . ? C26 H61 0.9800 . ? C26 H62 0.9800 . ? C27 H63 0.9800 . ? C27 H64 0.9800 . ? C27 H65 0.9800 . ? C28 H66 0.9800 . ? C28 H67 0.9800 . ? C28 H68 0.9800 . ? C29 H69 0.9800 . ? C29 H70 0.9800 . ? C29 H71 0.9800 . ? C30 H72 0.9800 . ? C30 H73 0.9800 . ? C30 H74 0.9800 . ? C31 H75 0.9800 . ? C31 H76 0.9800 . ? C31 H77 0.9800 . ? C32 H78 0.9800 . ? C32 H79 0.9800 . ? C32 H80 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 Ge1A Si1 132.38(2) . . ? Si2 Ge1B Si1 133.4(3) . . ? Si1 Ge1C Si2 134.9(9) . . ? C4 Si1 C1 99.81(8) . . ? C4 Si1 Ge1C 140.4(6) . . ? C1 Si1 Ge1C 118.4(6) . . ? C4 Si1 Ge1A 136.59(6) . . ? C1 Si1 Ge1A 116.10(6) . . ? C4 Si1 Ge1B 108.56(16) . . ? C1 Si1 Ge1B 141.89(17) . . ? C5 Si2 C8 99.70(8) . . ? C5 Si2 Ge1B 117.23(17) . . ? C8 Si2 Ge1B 142.14(18) . . ? C5 Si2 Ge1A 115.82(6) . . ? C8 Si2 Ge1A 136.99(6) . . ? C5 Si2 Ge1C 143.6(5) . . ? C8 Si2 Ge1C 107.3(5) . . ? C11 Si3 C9 110.43(11) . . ? C11 Si3 C10 107.02(11) . . ? C9 Si3 C10 104.35(11) . . ? C11 Si3 C1 111.77(10) . . ? C9 Si3 C1 110.98(10) . . ? C10 Si3 C1 111.98(9) . . ? C13 Si4 C14 107.08(13) . . ? C13 Si4 C12 106.96(12) . . ? C14 Si4 C12 102.84(11) . . ? C13 Si4 C1 114.90(10) . . ? C14 Si4 C1 112.66(10) . . ? C12 Si4 C1 111.53(10) . . ? C17 Si5 C16 107.76(11) . . ? C17 Si5 C15 109.24(10) . . ? C16 Si5 C15 104.12(10) . . ? C17 Si5 C4 111.51(9) . . ? C16 Si5 C4 112.29(9) . . ? C15 Si5 C4 111.60(9) . . ? C20 Si6 C18 105.78(11) . . ? C20 Si6 C19 110.03(11) . . ? C18 Si6 C19 105.51(11) . . ? C20 Si6 C4 112.29(10) . . ? C18 Si6 C4 114.50(10) . . ? C19 Si6 C4 108.49(10) . . ? C21 Si7 C23 105.93(10) . . ? C21 Si7 C22 110.19(12) . . ? C23 Si7 C22 103.90(11) . . ? C21 Si7 C5 112.31(9) . . ? C23 Si7 C5 114.98(9) . . ? C22 Si7 C5 109.15(10) . . ? C25 Si8 C26 106.95(11) . . ? C25 Si8 C24 108.75(12) . . ? C26 Si8 C24 103.15(11) . . ? C25 Si8 C5 113.37(10) . . ? C26 Si8 C5 111.81(9) . . ? C24 Si8 C5 112.19(10) . . ? C27 Si9 C29 108.41(10) . . ? C27 Si9 C28 108.27(10) . . ? C29 Si9 C28 102.69(10) . . ? C27 Si9 C8 112.53(9) . . ? C29 Si9 C8 112.58(9) . . ? C28 Si9 C8 111.81(9) . . ? C31 Si10 C30 109.03(10) . . ? C31 Si10 C32 109.38(11) . . ? C30 Si10 C32 104.16(11) . . ? C31 Si10 C8 111.56(9) . . ? C30 Si10 C8 111.00(9) . . ? C32 Si10 C8 111.44(9) . . ? C2 C1 Si1 99.99(12) . . ? C2 C1 Si3 108.78(13) . . ? Si1 C1 Si3 107.53(10) . . ? C2 C1 Si4 110.36(13) . . ? Si1 C1 Si4 118.43(10) . . ? Si3 C1 Si4 110.97(10) . . ? C3 C2 C1 110.70(16) . . ? C3 C2 H1 109.5 . . ? C1 C2 H1 109.5 . . ? C3 C2 H2 109.5 . . ? C1 C2 H2 109.5 . . ? H1 C2 H2 108.1 . . ? C2 C3 C4 111.60(15) . . ? C2 C3 H3 109.3 . . ? C4 C3 H3 109.3 . . ? C2 C3 H4 109.3 . . ? C4 C3 H4 109.3 . . ? H3 C3 H4 108.0 . . ? C3 C4 Si1 101.57(12) . . ? C3 C4 Si5 109.28(13) . . ? Si1 C4 Si5 113.85(10) . . ? C3 C4 Si6 109.66(13) . . ? Si1 C4 Si6 111.75(10) . . ? Si5 C4 Si6 110.34(10) . . ? C6 C5 Si2 102.23(12) . . ? C6 C5 Si8 110.58(12) . . ? Si2 C5 Si8 111.84(10) . . ? C6 C5 Si7 109.47(12) . . ? Si2 C5 Si7 112.72(10) . . ? Si8 C5 Si7 109.78(10) . . ? C7 C6 C5 111.14(15) . . ? C7 C6 H5 109.4 . . ? C5 C6 H5 109.4 . . ? C7 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? H5 C6 H6 108.0 . . ? C6 C7 C8 111.46(15) . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C6 C7 H8 109.3 . . ? C8 C7 H8 109.3 . . ? H7 C7 H8 108.0 . . ? C7 C8 Si2 100.24(12) . . ? C7 C8 Si10 109.01(12) . . ? Si2 C8 Si10 109.67(9) . . ? C7 C8 Si9 109.84(12) . . ? Si2 C8 Si9 116.24(10) . . ? Si10 C8 Si9 111.19(10) . . ? Si3 C9 H9 109.5 . . ? Si3 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? Si3 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? Si3 C10 H12 109.5 . . ? Si3 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? Si3 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? Si3 C11 H15 109.5 . . ? Si3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? Si3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? Si4 C12 H18 109.5 . . ? Si4 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? Si4 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? Si4 C13 H21 109.5 . . ? Si4 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? Si4 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? Si4 C14 H24 109.5 . . ? Si4 C14 H25 109.5 . . ? H24 C14 H25 109.5 . . ? Si4 C14 H26 109.5 . . ? H24 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? Si5 C15 H27 109.5 . . ? Si5 C15 H28 109.5 . . ? H27 C15 H28 109.5 . . ? Si5 C15 H29 109.5 . . ? H27 C15 H29 109.5 . . ? H28 C15 H29 109.5 . . ? Si5 C16 H30 109.5 . . ? Si5 C16 H31 109.5 . . ? H30 C16 H31 109.5 . . ? Si5 C16 H32 109.5 . . ? H30 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? Si5 C17 H33 109.5 . . ? Si5 C17 H34 109.5 . . ? H33 C17 H34 109.5 . . ? Si5 C17 H35 109.5 . . ? H33 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? Si6 C18 H36 109.5 . . ? Si6 C18 H37 109.5 . . ? H36 C18 H37 109.5 . . ? Si6 C18 H38 109.5 . . ? H36 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? Si6 C19 H39 109.5 . . ? Si6 C19 H40 109.5 . . ? H39 C19 H40 109.5 . . ? Si6 C19 H41 109.5 . . ? H39 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si6 C20 H42 109.5 . . ? Si6 C20 H43 109.5 . . ? H42 C20 H43 109.5 . . ? Si6 C20 H44 109.5 . . ? H42 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si7 C21 H45 109.5 . . ? Si7 C21 H46 109.5 . . ? H45 C21 H46 109.5 . . ? Si7 C21 H47 109.5 . . ? H45 C21 H47 109.5 . . ? H46 C21 H47 109.5 . . ? Si7 C22 H48 109.5 . . ? Si7 C22 H49 109.5 . . ? H48 C22 H49 109.5 . . ? Si7 C22 H50 109.5 . . ? H48 C22 H50 109.5 . . ? H49 C22 H50 109.5 . . ? Si7 C23 H51 109.5 . . ? Si7 C23 H52 109.5 . . ? H51 C23 H52 109.5 . . ? Si7 C23 H53 109.5 . . ? H51 C23 H53 109.5 . . ? H52 C23 H53 109.5 . . ? Si8 C24 H54 109.5 . . ? Si8 C24 H55 109.5 . . ? H54 C24 H55 109.5 . . ? Si8 C24 H56 109.5 . . ? H54 C24 H56 109.5 . . ? H55 C24 H56 109.5 . . ? Si8 C25 H57 109.5 . . ? Si8 C25 H58 109.5 . . ? H57 C25 H58 109.5 . . ? Si8 C25 H59 109.5 . . ? H57 C25 H59 109.5 . . ? H58 C25 H59 109.5 . . ? Si8 C26 H60 109.5 . . ? Si8 C26 H61 109.5 . . ? H60 C26 H61 109.5 . . ? Si8 C26 H62 109.5 . . ? H60 C26 H62 109.5 . . ? H61 C26 H62 109.5 . . ? Si9 C27 H63 109.5 . . ? Si9 C27 H64 109.5 . . ? H63 C27 H64 109.5 . . ? Si9 C27 H65 109.5 . . ? H63 C27 H65 109.5 . . ? H64 C27 H65 109.5 . . ? Si9 C28 H66 109.5 . . ? Si9 C28 H67 109.5 . . ? H66 C28 H67 109.5 . . ? Si9 C28 H68 109.5 . . ? H66 C28 H68 109.5 . . ? H67 C28 H68 109.5 . . ? Si9 C29 H69 109.5 . . ? Si9 C29 H70 109.5 . . ? H69 C29 H70 109.5 . . ? Si9 C29 H71 109.5 . . ? H69 C29 H71 109.5 . . ? H70 C29 H71 109.5 . . ? Si10 C30 H72 109.5 . . ? Si10 C30 H73 109.5 . . ? H72 C30 H73 109.5 . . ? Si10 C30 H74 109.5 . . ? H72 C30 H74 109.5 . . ? H73 C30 H74 109.5 . . ? Si10 C31 H75 109.5 . . ? Si10 C31 H76 109.5 . . ? H75 C31 H76 109.5 . . ? Si10 C31 H77 109.5 . . ? H75 C31 H77 109.5 . . ? H76 C31 H77 109.5 . . ? Si10 C32 H78 109.5 . . ? Si10 C32 H79 109.5 . . ? H78 C32 H79 109.5 . . ? Si10 C32 H80 109.5 . . ? H78 C32 H80 109.5 . . ? H79 C32 H80 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.419 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.062 data_2-germadisilaallene_crystal_C_223K _database_code_depnum_ccdc_archive 'CCDC 279209' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C32 H80 Ge Si10 ' _chemical_formula_moiety 'C32 H80 Ge Si10 ' _chemical_melting_point ? _chemical_formula_weight 818.45 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.787(3) _cell_length_b 12.318(2) _cell_length_c 18.634(4) _cell_angle_alpha 73.594(6) _cell_angle_beta 87.201(7) _cell_angle_gamma 72.174(6) _cell_volume 2468.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5595 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 55.0 _exptl_crystal_description prism _exptl_crystal_colour dark_green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.7776 _exptl_absorpt_correction_T_max 0.9169 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28393 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11079 _reflns_number_gt 9099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+1.7672P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11079 _refine_ls_number_parameters 443 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1A Ge 0.35212(5) 0.29671(6) 0.75345(4) 0.0451(2) Uani 0.6211(15) 1 d PU . . Ge1B Ge 0.3184(2) 0.2180(2) 0.77695(12) 0.0488(7) Uani 0.1680(13) 1 d PU . . Ge1C Ge 0.2292(7) 0.2645(7) 0.7346(4) 0.0447(11) Uani 0.0467(9) 1 d PU . . Ge1D Ge 0.2713(2) 0.3463(2) 0.71196(13) 0.0465(7) Uani 0.1641(12) 1 d PU . . Si1 Si 0.19477(8) 0.37296(8) 0.81465(5) 0.0410(2) Uani 1 1 d U . . Si2 Si 0.38205(8) 0.18941(8) 0.67203(5) 0.0382(2) Uani 1 1 d U . . Si3 Si 0.15066(9) 0.64324(9) 0.74593(6) 0.0515(3) Uani 1 1 d . . . Si4 Si 0.33035(12) 0.51517(12) 0.88436(8) 0.0715(4) Uani 1 1 d . . . Si5 Si -0.05939(9) 0.33249(10) 0.85013(6) 0.0565(3) Uani 1 1 d . . . Si6 Si 0.16713(10) 0.16203(9) 0.94975(6) 0.0555(3) Uani 1 1 d . . . Si7 Si 0.65635(9) 0.14643(9) 0.69908(6) 0.0523(3) Uani 1 1 d . . . Si8 Si 0.55675(9) -0.07099(8) 0.74018(6) 0.0495(3) Uani 1 1 d . . . Si9 Si 0.32701(8) 0.35234(9) 0.50068(5) 0.0442(2) Uani 1 1 d . . . Si10 Si 0.17963(8) 0.17806(9) 0.57602(6) 0.0469(2) Uani 1 1 d . . . C1 C 0.1921(3) 0.5156(3) 0.83563(19) 0.0426(7) Uani 1 1 d . . . C2 C 0.0842(4) 0.5307(3) 0.8885(2) 0.0593(10) Uani 1 1 d . . . H1 H 0.0935 0.5774 0.9212 0.071 Uiso 1 1 calc R . . H2 H 0.0100 0.5741 0.8582 0.071 Uiso 1 1 calc R . . C3 C 0.0761(4) 0.4095(3) 0.9366(2) 0.0594(10) Uani 1 1 d . . . H3 H -0.0019 0.4203 0.9593 0.071 Uiso 1 1 calc R . . H4 H 0.1376 0.3767 0.9770 0.071 Uiso 1 1 calc R . . C4 C 0.0927(3) 0.3198(3) 0.88908(18) 0.0417(7) Uani 1 1 d . . . C5 C 0.5383(3) 0.0841(3) 0.67464(18) 0.0377(7) Uani 1 1 d . . . C6 C 0.5505(3) 0.0794(3) 0.59124(18) 0.0408(7) Uani 1 1 d . . . H5 H 0.5858 0.1402 0.5628 0.049 Uiso 1 1 calc R . . H6 H 0.6040 0.0016 0.5897 0.049 Uiso 1 1 calc R . . C7 C 0.4285(3) 0.1003(3) 0.55473(18) 0.0402(7) Uani 1 1 d . . . H7 H 0.4048 0.0279 0.5725 0.048 Uiso 1 1 calc R . . H8 H 0.4351 0.1174 0.5003 0.048 Uiso 1 1 calc R . . C8 C 0.3304(3) 0.2061(3) 0.57360(17) 0.0357(7) Uani 1 1 d . . . C9 C 0.0405(4) 0.6267(4) 0.6838(2) 0.0697(12) Uani 1 1 d . . . H9 H 0.0299 0.6879 0.6364 0.105 Uiso 1 1 calc R . . H10 H -0.0353 0.6345 0.7078 0.105 Uiso 1 1 calc R . . H11 H 0.0699 0.5491 0.6751 0.105 Uiso 1 1 calc R . . C10 C 0.0758(5) 0.7872(4) 0.7678(3) 0.0864(15) Uani 1 1 d . . . H12 H 0.1339 0.8105 0.7901 0.130 Uiso 1 1 calc R . . H13 H 0.0132 0.7776 0.8025 0.130 Uiso 1 1 calc R . . H14 H 0.0414 0.8481 0.7220 0.130 Uiso 1 1 calc R . . C11 C 0.2816(4) 0.6560(5) 0.6879(3) 0.0776(13) Uani 1 1 d . . . H15 H 0.2555 0.7199 0.6421 0.116 Uiso 1 1 calc R . . H16 H 0.3191 0.5818 0.6758 0.116 Uiso 1 1 calc R . . H17 H 0.3385 0.6729 0.7157 0.116 Uiso 1 1 calc R . . C12 C 0.3244(5) 0.6681(5) 0.8850(3) 0.0901(16) Uani 1 1 d . . . H18 H 0.3924 0.6640 0.9140 0.135 Uiso 1 1 calc R . . H19 H 0.2513 0.7037 0.9072 0.135 Uiso 1 1 calc R . . H20 H 0.3263 0.7162 0.8340 0.135 Uiso 1 1 calc R . . C13 C 0.4723(4) 0.4535(6) 0.8426(5) 0.140(3) Uani 1 1 d . . . H21 H 0.5358 0.4727 0.8626 0.210 Uiso 1 1 calc R . . H22 H 0.4649 0.4874 0.7887 0.210 Uiso 1 1 calc R . . H23 H 0.4909 0.3678 0.8545 0.210 Uiso 1 1 calc R . . C14 C 0.3405(7) 0.4336(6) 0.9861(3) 0.152(3) Uani 1 1 d . . . H24 H 0.3645 0.3488 0.9921 0.229 Uiso 1 1 calc R . . H25 H 0.2634 0.4577 1.0076 0.229 Uiso 1 1 calc R . . H26 H 0.3991 0.4521 1.0116 0.229 Uiso 1 1 calc R . . C15 C -0.1605(4) 0.4886(5) 0.8208(4) 0.124(3) Uani 1 1 d . . . H27 H -0.1289 0.5342 0.7778 0.187 Uiso 1 1 calc R . . H28 H -0.1660 0.5239 0.8617 0.187 Uiso 1 1 calc R . . H29 H -0.2392 0.4889 0.8076 0.187 Uiso 1 1 calc R . . C16 C -0.0460(5) 0.2749(7) 0.7676(3) 0.115(2) Uani 1 1 d . . . H30 H 0.0044 0.1929 0.7809 0.173 Uiso 1 1 calc R . . H31 H -0.0108 0.3223 0.7275 0.173 Uiso 1 1 calc R . . H32 H -0.1244 0.2794 0.7510 0.173 Uiso 1 1 calc R . . C17 C -0.1461(4) 0.2546(4) 0.9217(2) 0.0691(12) Uani 1 1 d . . . H33 H -0.2254 0.2706 0.9011 0.104 Uiso 1 1 calc R . . H34 H -0.1520 0.2830 0.9657 0.104 Uiso 1 1 calc R . . H35 H -0.1058 0.1697 0.9355 0.104 Uiso 1 1 calc R . . C18 C 0.0966(5) 0.1383(5) 1.0433(2) 0.0871(15) Uani 1 1 d . . . H36 H 0.1321 0.0570 1.0732 0.131 Uiso 1 1 calc R . . H37 H 0.0116 0.1535 1.0360 0.131 Uiso 1 1 calc R . . H38 H 0.1096 0.1922 1.0689 0.131 Uiso 1 1 calc R . . C19 C 0.1564(5) 0.0489(4) 0.9033(3) 0.0828(14) Uani 1 1 d . . . H39 H 0.1895 0.0645 0.8541 0.124 Uiso 1 1 calc R . . H40 H 0.0734 0.0536 0.8983 0.124 Uiso 1 1 calc R . . H41 H 0.2007 -0.0299 0.9335 0.124 Uiso 1 1 calc R . . C20 C 0.3296(4) 0.1306(4) 0.9723(3) 0.0770(13) Uani 1 1 d . . . H42 H 0.3385 0.1834 1.0002 0.115 Uiso 1 1 calc R . . H43 H 0.3718 0.1434 0.9262 0.115 Uiso 1 1 calc R . . H44 H 0.3624 0.0488 1.0023 0.115 Uiso 1 1 calc R . . C21 C 0.8033(4) 0.0781(5) 0.6609(3) 0.0927(17) Uani 1 1 d . . . H45 H 0.7960 0.1004 0.6067 0.139 Uiso 1 1 calc R . . H46 H 0.8257 -0.0077 0.6804 0.139 Uiso 1 1 calc R . . H47 H 0.8640 0.1065 0.6760 0.139 Uiso 1 1 calc R . . C22 C 0.6738(5) 0.1203(4) 0.8021(3) 0.0887(17) Uani 1 1 d . . . H48 H 0.7305 0.1577 0.8120 0.133 Uiso 1 1 calc R . . H49 H 0.7027 0.0355 0.8264 0.133 Uiso 1 1 calc R . . H50 H 0.5973 0.1541 0.8216 0.133 Uiso 1 1 calc R . . C23 C 0.6243(4) 0.3097(3) 0.6564(2) 0.0621(11) Uani 1 1 d . . . H51 H 0.5447 0.3508 0.6685 0.093 Uiso 1 1 calc R . . H52 H 0.6295 0.3264 0.6024 0.093 Uiso 1 1 calc R . . H53 H 0.6821 0.3368 0.6760 0.093 Uiso 1 1 calc R . . C24 C 0.4864(5) -0.0692(4) 0.8316(2) 0.0855(15) Uani 1 1 d . . . H54 H 0.4003 -0.0423 0.8241 0.128 Uiso 1 1 calc R . . H55 H 0.5109 -0.0157 0.8525 0.128 Uiso 1 1 calc R . . H56 H 0.5114 -0.1487 0.8658 0.128 Uiso 1 1 calc R . . C25 C 0.4910(4) -0.1602(3) 0.6982(3) 0.0661(11) Uani 1 1 d . . . H57 H 0.5092 -0.2406 0.7310 0.099 Uiso 1 1 calc R . . H58 H 0.5245 -0.1621 0.6498 0.099 Uiso 1 1 calc R . . H59 H 0.4052 -0.1242 0.6919 0.099 Uiso 1 1 calc R . . C26 C 0.7172(4) -0.1622(4) 0.7580(3) 0.0932(18) Uani 1 1 d . . . H60 H 0.7229 -0.2407 0.7907 0.140 Uiso 1 1 calc R . . H61 H 0.7590 -0.1240 0.7817 0.140 Uiso 1 1 calc R . . H62 H 0.7530 -0.1693 0.7109 0.140 Uiso 1 1 calc R . . C27 C 0.4784(3) 0.3546(4) 0.4660(2) 0.0611(10) Uani 1 1 d . . . H63 H 0.4710 0.4272 0.4263 0.092 Uiso 1 1 calc R . . H64 H 0.5139 0.2866 0.4470 0.092 Uiso 1 1 calc R . . H65 H 0.5285 0.3511 0.5069 0.092 Uiso 1 1 calc R . . C28 C 0.2619(4) 0.4844(3) 0.5360(2) 0.0673(11) Uani 1 1 d . . . H66 H 0.3152 0.4832 0.5744 0.101 Uiso 1 1 calc R . . H67 H 0.1853 0.4827 0.5568 0.101 Uiso 1 1 calc R . . H68 H 0.2513 0.5562 0.4950 0.101 Uiso 1 1 calc R . . C29 C 0.2413(4) 0.3748(4) 0.4127(2) 0.0736(13) Uani 1 1 d . . . H69 H 0.1582 0.3833 0.4236 0.110 Uiso 1 1 calc R . . H70 H 0.2741 0.3068 0.3934 0.110 Uiso 1 1 calc R . . H71 H 0.2472 0.4460 0.3757 0.110 Uiso 1 1 calc R . . C30 C 0.1602(4) 0.1191(5) 0.4964(3) 0.0801(14) Uani 1 1 d . . . H72 H 0.0791 0.1164 0.4943 0.120 Uiso 1 1 calc R . . H73 H 0.2154 0.0398 0.5039 0.120 Uiso 1 1 calc R . . H74 H 0.1760 0.1708 0.4497 0.120 Uiso 1 1 calc R . . C31 C 0.0535(3) 0.3149(4) 0.5731(3) 0.0710(12) Uani 1 1 d . . . H75 H -0.0203 0.2947 0.5823 0.107 Uiso 1 1 calc R . . H76 H 0.0475 0.3719 0.5243 0.107 Uiso 1 1 calc R . . H77 H 0.0676 0.3494 0.6113 0.107 Uiso 1 1 calc R . . C32 C 0.1672(3) 0.0598(4) 0.6622(2) 0.0641(11) Uani 1 1 d . . . H78 H 0.1857 0.0796 0.7062 0.096 Uiso 1 1 calc R . . H79 H 0.2229 -0.0159 0.6606 0.096 Uiso 1 1 calc R . . H80 H 0.0867 0.0545 0.6645 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1A 0.0379(4) 0.0574(4) 0.0504(4) -0.0327(3) 0.0068(3) -0.0140(3) Ge1B 0.0550(13) 0.0469(13) 0.0374(11) -0.0143(9) 0.0073(9) -0.0037(10) Ge1C 0.045(2) 0.052(2) 0.043(2) -0.0246(19) 0.0084(18) -0.0151(18) Ge1D 0.0572(14) 0.0399(12) 0.0394(12) -0.0169(9) 0.0096(10) -0.0066(10) Si1 0.0400(5) 0.0455(5) 0.0404(5) -0.0192(4) 0.0067(4) -0.0114(4) Si2 0.0382(5) 0.0394(5) 0.0380(5) -0.0176(4) 0.0003(4) -0.0070(4) Si3 0.0471(6) 0.0500(6) 0.0576(6) -0.0109(5) 0.0076(5) -0.0199(5) Si4 0.0701(8) 0.0769(8) 0.0805(9) -0.0334(7) -0.0181(6) -0.0274(7) Si5 0.0415(6) 0.0670(7) 0.0559(7) -0.0070(5) 0.0059(5) -0.0190(5) Si6 0.0606(7) 0.0475(6) 0.0510(6) -0.0042(5) -0.0039(5) -0.0138(5) Si7 0.0453(6) 0.0465(6) 0.0680(7) -0.0151(5) -0.0148(5) -0.0165(5) Si8 0.0513(6) 0.0333(5) 0.0603(6) -0.0100(4) -0.0119(5) -0.0089(4) Si9 0.0430(5) 0.0470(5) 0.0394(5) -0.0086(4) -0.0029(4) -0.0118(4) Si10 0.0336(5) 0.0532(6) 0.0562(6) -0.0179(5) -0.0021(4) -0.0137(4) C1 0.0405(18) 0.0464(19) 0.0454(19) -0.0172(15) 0.0052(14) -0.0163(15) C2 0.074(3) 0.051(2) 0.064(2) -0.0321(19) 0.030(2) -0.024(2) C3 0.082(3) 0.056(2) 0.052(2) -0.0269(19) 0.025(2) -0.030(2) C4 0.0489(19) 0.0419(18) 0.0385(18) -0.0159(14) 0.0084(14) -0.0166(15) C5 0.0369(17) 0.0355(16) 0.0428(18) -0.0139(14) -0.0055(13) -0.0104(13) C6 0.0333(17) 0.0416(18) 0.0493(19) -0.0203(15) 0.0024(14) -0.0072(14) C7 0.0410(18) 0.0455(18) 0.0384(17) -0.0225(15) 0.0011(13) -0.0097(15) C8 0.0319(16) 0.0412(17) 0.0368(17) -0.0162(14) 0.0000(12) -0.0101(13) C9 0.059(3) 0.073(3) 0.066(3) 0.002(2) -0.013(2) -0.021(2) C10 0.087(3) 0.050(3) 0.115(4) -0.016(3) 0.010(3) -0.017(2) C11 0.077(3) 0.109(4) 0.068(3) -0.027(3) 0.024(2) -0.060(3) C12 0.106(4) 0.101(4) 0.097(4) -0.045(3) 0.006(3) -0.065(3) C13 0.048(3) 0.167(6) 0.235(8) -0.126(6) -0.029(4) -0.008(3) C14 0.232(8) 0.144(6) 0.104(5) 0.013(4) -0.097(5) -0.116(6) C15 0.046(3) 0.082(4) 0.196(7) 0.035(4) -0.001(3) -0.016(3) C16 0.077(3) 0.229(8) 0.073(3) -0.061(4) 0.008(3) -0.078(4) C17 0.063(3) 0.078(3) 0.075(3) -0.019(2) 0.014(2) -0.037(2) C18 0.097(4) 0.091(4) 0.056(3) 0.008(3) 0.004(2) -0.030(3) C19 0.088(3) 0.047(2) 0.115(4) -0.026(3) 0.001(3) -0.020(2) C20 0.071(3) 0.075(3) 0.068(3) -0.006(2) -0.021(2) -0.007(2) C21 0.043(2) 0.088(4) 0.157(5) -0.048(4) -0.004(3) -0.022(2) C22 0.125(4) 0.075(3) 0.073(3) -0.006(2) -0.047(3) -0.045(3) C23 0.069(3) 0.056(2) 0.069(3) -0.011(2) -0.006(2) -0.035(2) C24 0.133(5) 0.060(3) 0.054(3) 0.001(2) 0.000(3) -0.031(3) C25 0.069(3) 0.043(2) 0.090(3) -0.020(2) -0.007(2) -0.020(2) C26 0.068(3) 0.045(2) 0.150(5) -0.011(3) -0.039(3) -0.001(2) C27 0.058(2) 0.059(2) 0.061(2) -0.0047(19) 0.0055(19) -0.022(2) C28 0.077(3) 0.043(2) 0.073(3) -0.011(2) 0.008(2) -0.011(2) C29 0.075(3) 0.092(3) 0.047(2) 0.000(2) -0.016(2) -0.031(3) C30 0.071(3) 0.105(4) 0.086(3) -0.043(3) -0.009(2) -0.042(3) C31 0.038(2) 0.070(3) 0.087(3) -0.007(2) 0.004(2) -0.0045(19) C32 0.049(2) 0.058(2) 0.090(3) -0.016(2) 0.011(2) -0.0271(19) _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 Ge1A Si1 2.2259(11) . ? Ge1A Si2 2.2290(11) . ? Ge1B Si2 2.143(2) . ? Ge1B Si1 2.284(2) . ? Ge1C Si2 2.201(7) . ? Ge1C Si1 2.216(7) . ? Ge1D Si1 2.142(2) . ? Ge1D Si2 2.273(2) . ? Si1 C1 1.896(3) . ? Si1 C4 1.899(3) . ? Si2 C5 1.894(3) . ? Si2 C8 1.896(3) . ? Si3 C11 1.862(4) . ? Si3 C10 1.872(5) . ? Si3 C9 1.873(4) . ? Si3 C1 1.905(4) . ? Si4 C13 1.847(6) . ? Si4 C12 1.867(5) . ? Si4 C14 1.869(6) . ? Si4 C1 1.902(3) . ? Si5 C16 1.849(5) . ? Si5 C15 1.867(5) . ? Si5 C17 1.867(4) . ? Si5 C4 1.912(4) . ? Si6 C19 1.872(5) . ? Si6 C20 1.878(4) . ? Si6 C18 1.880(5) . ? Si6 C4 1.907(4) . ? Si7 C23 1.866(4) . ? Si7 C22 1.866(5) . ? Si7 C21 1.881(5) . ? Si7 C5 1.909(3) . ? Si8 C24 1.860(5) . ? Si8 C25 1.868(4) . ? Si8 C26 1.871(4) . ? Si8 C5 1.909(3) . ? Si9 C28 1.860(4) . ? Si9 C27 1.873(4) . ? Si9 C29 1.876(4) . ? Si9 C8 1.916(3) . ? Si10 C31 1.865(4) . ? Si10 C32 1.873(4) . ? Si10 C30 1.878(4) . ? Si10 C8 1.908(3) . ? C1 C2 1.568(5) . ? C2 C3 1.537(5) . ? C2 H1 0.9800 . ? C2 H2 0.9800 . ? C3 C4 1.564(5) . ? C3 H3 0.9800 . ? C3 H4 0.9800 . ? C5 C6 1.570(4) . ? C6 C7 1.538(4) . ? C6 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.568(4) . ? C7 H7 0.9800 . ? C7 H8 0.9800 . ? C9 H9 0.9700 . ? C9 H10 0.9700 . ? C9 H11 0.9700 . ? C10 H12 0.9700 . ? C10 H13 0.9700 . ? C10 H14 0.9700 . ? C11 H15 0.9700 . ? C11 H16 0.9700 . ? C11 H17 0.9700 . ? C12 H18 0.9700 . ? C12 H19 0.9700 . ? C12 H20 0.9700 . ? C13 H21 0.9700 . ? C13 H22 0.9700 . ? C13 H23 0.9700 . ? C14 H24 0.9700 . ? C14 H25 0.9700 . ? C14 H26 0.9700 . ? C15 H27 0.9700 . ? C15 H28 0.9700 . ? C15 H29 0.9700 . ? C16 H30 0.9700 . ? C16 H31 0.9700 . ? C16 H32 0.9700 . ? C17 H33 0.9700 . ? C17 H34 0.9700 . ? C17 H35 0.9700 . ? C18 H36 0.9700 . ? C18 H37 0.9700 . ? C18 H38 0.9700 . ? C19 H39 0.9700 . ? C19 H40 0.9700 . ? C19 H41 0.9700 . ? C20 H42 0.9700 . ? C20 H43 0.9700 . ? C20 H44 0.9700 . ? C21 H45 0.9700 . ? C21 H46 0.9700 . ? C21 H47 0.9700 . ? C22 H48 0.9700 . ? C22 H49 0.9700 . ? C22 H50 0.9700 . ? C23 H51 0.9700 . ? C23 H52 0.9700 . ? C23 H53 0.9700 . ? C24 H54 0.9700 . ? C24 H55 0.9700 . ? C24 H56 0.9700 . ? C25 H57 0.9700 . ? C25 H58 0.9700 . ? C25 H59 0.9700 . ? C26 H60 0.9700 . ? C26 H61 0.9700 . ? C26 H62 0.9700 . ? C27 H63 0.9700 . ? C27 H64 0.9700 . ? C27 H65 0.9700 . ? C28 H66 0.9700 . ? C28 H67 0.9700 . ? C28 H68 0.9700 . ? C29 H69 0.9700 . ? C29 H70 0.9700 . ? C29 H71 0.9700 . ? C30 H72 0.9700 . ? C30 H73 0.9700 . ? C30 H74 0.9700 . ? C31 H75 0.9700 . ? C31 H76 0.9700 . ? C31 H77 0.9700 . ? C32 H78 0.9700 . ? C32 H79 0.9700 . ? C32 H80 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 Ge1A Si2 133.98(4) . . ? Si2 Ge1B Si1 135.69(12) . . ? Si2 Ge1C Si1 136.4(4) . . ? Si1 Ge1D Si2 136.46(12) . . ? C1 Si1 C4 99.94(14) . . ? C1 Si1 Ge1D 116.79(13) . . ? C4 Si1 Ge1D 141.54(13) . . ? C1 Si1 Ge1C 148.7(2) . . ? C4 Si1 Ge1C 109.5(2) . . ? C1 Si1 Ge1A 114.95(11) . . ? C4 Si1 Ge1A 138.95(11) . . ? C1 Si1 Ge1B 141.80(13) . . ? C4 Si1 Ge1B 110.86(13) . . ? C5 Si2 C8 99.81(13) . . ? C5 Si2 Ge1B 116.07(12) . . ? C8 Si2 Ge1B 142.62(12) . . ? C5 Si2 Ge1C 148.1(2) . . ? C8 Si2 Ge1C 109.9(2) . . ? C5 Si2 Ge1A 115.34(10) . . ? C8 Si2 Ge1A 138.67(10) . . ? C5 Si2 Ge1D 143.24(12) . . ? C8 Si2 Ge1D 110.04(12) . . ? C11 Si3 C10 109.7(2) . . ? C11 Si3 C9 105.8(2) . . ? C10 Si3 C9 105.1(2) . . ? C11 Si3 C1 112.6(2) . . ? C10 Si3 C1 110.6(2) . . ? C9 Si3 C1 112.57(17) . . ? C13 Si4 C12 106.7(3) . . ? C13 Si4 C14 108.4(4) . . ? C12 Si4 C14 103.1(3) . . ? C13 Si4 C1 114.6(2) . . ? C12 Si4 C1 111.6(2) . . ? C14 Si4 C1 111.8(2) . . ? C16 Si5 C15 106.8(3) . . ? C16 Si5 C17 108.9(2) . . ? C15 Si5 C17 103.0(2) . . ? C16 Si5 C4 112.00(19) . . ? C15 Si5 C4 113.0(2) . . ? C17 Si5 C4 112.49(18) . . ? C19 Si6 C20 106.9(2) . . ? C19 Si6 C18 110.3(2) . . ? C20 Si6 C18 104.7(2) . . ? C19 Si6 C4 111.43(19) . . ? C20 Si6 C4 113.61(19) . . ? C18 Si6 C4 109.62(19) . . ? C23 Si7 C22 106.2(2) . . ? C23 Si7 C21 104.6(2) . . ? C22 Si7 C21 110.0(3) . . ? C23 Si7 C5 113.97(16) . . ? C22 Si7 C5 112.01(19) . . ? C21 Si7 C5 109.80(18) . . ? C24 Si8 C25 106.9(2) . . ? C24 Si8 C26 108.8(3) . . ? C25 Si8 C26 103.2(2) . . ? C24 Si8 C5 113.24(18) . . ? C25 Si8 C5 112.15(17) . . ? C26 Si8 C5 111.91(19) . . ? C28 Si9 C27 108.0(2) . . ? C28 Si9 C29 108.3(2) . . ? C27 Si9 C29 102.6(2) . . ? C28 Si9 C8 112.86(16) . . ? C27 Si9 C8 112.67(16) . . ? C29 Si9 C8 111.82(18) . . ? C31 Si10 C32 107.8(2) . . ? C31 Si10 C30 109.7(2) . . ? C32 Si10 C30 104.6(2) . . ? C31 Si10 C8 111.87(18) . . ? C32 Si10 C8 111.82(16) . . ? C30 Si10 C8 110.84(18) . . ? C2 C1 Si1 100.6(2) . . ? C2 C1 Si4 110.0(2) . . ? Si1 C1 Si4 117.26(18) . . ? C2 C1 Si3 108.4(2) . . ? Si1 C1 Si3 109.14(17) . . ? Si4 C1 Si3 110.79(17) . . ? C3 C2 C1 111.3(3) . . ? C3 C2 H1 109.4 . . ? C1 C2 H1 109.4 . . ? C3 C2 H2 109.4 . . ? C1 C2 H2 109.4 . . ? H1 C2 H2 108.0 . . ? C2 C3 C4 111.6(3) . . ? C2 C3 H3 109.3 . . ? C4 C3 H3 109.3 . . ? C2 C3 H4 109.3 . . ? C4 C3 H4 109.3 . . ? H3 C3 H4 108.0 . . ? C3 C4 Si1 101.2(2) . . ? C3 C4 Si6 109.8(2) . . ? Si1 C4 Si6 111.85(17) . . ? C3 C4 Si5 109.4(3) . . ? Si1 C4 Si5 113.82(17) . . ? Si6 C4 Si5 110.42(17) . . ? C6 C5 Si2 101.71(19) . . ? C6 C5 Si8 110.1(2) . . ? Si2 C5 Si8 112.97(17) . . ? C6 C5 Si7 109.3(2) . . ? Si2 C5 Si7 112.05(16) . . ? Si8 C5 Si7 110.29(15) . . ? C7 C6 C5 111.3(2) . . ? C7 C6 H5 109.4 . . ? C5 C6 H5 109.4 . . ? C7 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? H5 C6 H6 108.0 . . ? C6 C7 C8 111.5(2) . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C6 C7 H8 109.3 . . ? C8 C7 H8 109.3 . . ? H7 C7 H8 108.0 . . ? C7 C8 Si2 100.66(19) . . ? C7 C8 Si10 109.2(2) . . ? Si2 C8 Si10 109.71(16) . . ? C7 C8 Si9 109.8(2) . . ? Si2 C8 Si9 115.81(16) . . ? Si10 C8 Si9 111.09(15) . . ? Si3 C9 H9 109.5 . . ? Si3 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? Si3 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? Si3 C10 H12 109.5 . . ? Si3 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? Si3 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? Si3 C11 H15 109.5 . . ? Si3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? Si3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? Si4 C12 H18 109.5 . . ? Si4 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? Si4 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? Si4 C13 H21 109.5 . . ? Si4 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? Si4 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? Si4 C14 H24 109.5 . . ? Si4 C14 H25 109.5 . . ? H24 C14 H25 109.5 . . ? Si4 C14 H26 109.5 . . ? H24 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? Si5 C15 H27 109.5 . . ? Si5 C15 H28 109.5 . . ? H27 C15 H28 109.5 . . ? Si5 C15 H29 109.5 . . ? H27 C15 H29 109.5 . . ? H28 C15 H29 109.5 . . ? Si5 C16 H30 109.5 . . ? Si5 C16 H31 109.5 . . ? H30 C16 H31 109.5 . . ? Si5 C16 H32 109.5 . . ? H30 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? Si5 C17 H33 109.5 . . ? Si5 C17 H34 109.5 . . ? H33 C17 H34 109.5 . . ? Si5 C17 H35 109.5 . . ? H33 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? Si6 C18 H36 109.5 . . ? Si6 C18 H37 109.5 . . ? H36 C18 H37 109.5 . . ? Si6 C18 H38 109.5 . . ? H36 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? Si6 C19 H39 109.5 . . ? Si6 C19 H40 109.5 . . ? H39 C19 H40 109.5 . . ? Si6 C19 H41 109.5 . . ? H39 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si6 C20 H42 109.5 . . ? Si6 C20 H43 109.5 . . ? H42 C20 H43 109.5 . . ? Si6 C20 H44 109.5 . . ? H42 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si7 C21 H45 109.5 . . ? Si7 C21 H46 109.5 . . ? H45 C21 H46 109.5 . . ? Si7 C21 H47 109.5 . . ? H45 C21 H47 109.5 . . ? H46 C21 H47 109.5 . . ? Si7 C22 H48 109.5 . . ? Si7 C22 H49 109.5 . . ? H48 C22 H49 109.5 . . ? Si7 C22 H50 109.5 . . ? H48 C22 H50 109.5 . . ? H49 C22 H50 109.5 . . ? Si7 C23 H51 109.5 . . ? Si7 C23 H52 109.5 . . ? H51 C23 H52 109.5 . . ? Si7 C23 H53 109.5 . . ? H51 C23 H53 109.5 . . ? H52 C23 H53 109.5 . . ? Si8 C24 H54 109.5 . . ? Si8 C24 H55 109.5 . . ? H54 C24 H55 109.5 . . ? Si8 C24 H56 109.5 . . ? H54 C24 H56 109.5 . . ? H55 C24 H56 109.5 . . ? Si8 C25 H57 109.5 . . ? Si8 C25 H58 109.5 . . ? H57 C25 H58 109.5 . . ? Si8 C25 H59 109.5 . . ? H57 C25 H59 109.5 . . ? H58 C25 H59 109.5 . . ? Si8 C26 H60 109.5 . . ? Si8 C26 H61 109.5 . . ? H60 C26 H61 109.5 . . ? Si8 C26 H62 109.5 . . ? H60 C26 H62 109.5 . . ? H61 C26 H62 109.5 . . ? Si9 C27 H63 109.5 . . ? Si9 C27 H64 109.5 . . ? H63 C27 H64 109.5 . . ? Si9 C27 H65 109.5 . . ? H63 C27 H65 109.5 . . ? H64 C27 H65 109.5 . . ? Si9 C28 H66 109.5 . . ? Si9 C28 H67 109.5 . . ? H66 C28 H67 109.5 . . ? Si9 C28 H68 109.5 . . ? H66 C28 H68 109.5 . . ? H67 C28 H68 109.5 . . ? Si9 C29 H69 109.5 . . ? Si9 C29 H70 109.5 . . ? H69 C29 H70 109.5 . . ? Si9 C29 H71 109.5 . . ? H69 C29 H71 109.5 . . ? H70 C29 H71 109.5 . . ? Si10 C30 H72 109.5 . . ? Si10 C30 H73 109.5 . . ? H72 C30 H73 109.5 . . ? Si10 C30 H74 109.5 . . ? H72 C30 H74 109.5 . . ? H73 C30 H74 109.5 . . ? Si10 C31 H75 109.5 . . ? Si10 C31 H76 109.5 . . ? H75 C31 H76 109.5 . . ? Si10 C31 H77 109.5 . . ? H75 C31 H77 109.5 . . ? H76 C31 H77 109.5 . . ? Si10 C32 H78 109.5 . . ? Si10 C32 H79 109.5 . . ? H78 C32 H79 109.5 . . ? Si10 C32 H80 109.5 . . ? H78 C32 H80 109.5 . . ? H79 C32 H80 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.408 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.056