# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Norihiro Tokitoh' 'Takayo Sasaki' 'Takahiro Sasamori' 'Tomoyuki Tajima' _publ_contact_author_name 'Prof Norihiro Tokitoh' _publ_contact_author_address ; Institute for Chemical Research Kyoto University Gokasho Uji, Kyoto 611-0011 JAPAN ; _publ_contact_author_email TOKITOH@BOC.KUICR.KYOTO-U.AC.JP _publ_requested_journal 'Chemical Communications' _publ_section_title ; Thermal reactions of an overcrowded germacyclopropabenzene with group 6 metal hexacarbonyl complexes [M(CO)6] (M = Cr, Mo, and W): a novel mode of CO insertion leading to the formation of cyclic germoxycarbene metal complexes ; data_Cr(CO)6 _database_code_depnum_ccdc_archive 'CCDC 224028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cr complex' _chemical_melting_point ? _chemical_formula_moiety 'C51 H80 Ge O6 Si6 Cr' _chemical_formula_sum 'C51 H80 Cr Ge O6 Si6' _chemical_formula_weight 1082.28 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.8841(16) _cell_length_b 13.7144(8) _cell_length_c 19.8020(9) _cell_angle_alpha 77.335(4) _cell_angle_beta 71.540(3) _cell_angle_gamma 84.6841(17) _cell_volume 2985.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisum _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7851 _exptl_absorpt_correction_T_max 0.8488 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU/MSC Meacury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28396 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10452 _reflns_number_gt 7940 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _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^)+(0.0671P)^2^+1.1906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10452 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Ge1 Ge 0.23454(3) 0.35706(2) 0.333372(16) 0.01975(10) Uani 1 1 d . . . C1 C 0.3578(3) 0.5282(3) 0.30950(17) 0.0297(7) Uani 1 1 d . . . O1 O 0.37243(19) 0.43379(16) 0.30930(11) 0.0285(5) Uani 1 1 d . . . C2 C 0.1467(3) 0.4827(2) 0.34423(17) 0.0280(7) Uani 1 1 d . . . C3 C 0.2277(3) 0.5579(2) 0.33132(17) 0.0295(7) Uani 1 1 d . . . C4 C 0.1841(3) 0.6541(3) 0.33943(19) 0.0365(8) Uani 1 1 d . . . H1 H 0.2380 0.7058 0.3303 0.044 Uiso 1 1 calc R . . C5 C 0.0630(3) 0.6751(3) 0.3606(2) 0.0419(9) Uani 1 1 d . . . H2 H 0.0343 0.7409 0.3657 0.050 Uiso 1 1 calc R . . C6 C -0.0156(3) 0.5998(3) 0.3742(2) 0.0442(9) Uani 1 1 d . . . H3 H -0.0985 0.6144 0.3892 0.053 Uiso 1 1 calc R . . C7 C 0.0242(3) 0.5031(3) 0.36647(17) 0.0312(7) Uani 1 1 d . . . H4 H -0.0306 0.4518 0.3761 0.037 Uiso 1 1 calc R . . Cr1 Cr 0.50069(5) 0.61568(4) 0.28836(3) 0.03296(15) Uani 1 1 d . . . C8 C 0.4314(3) 0.7199(3) 0.2322(2) 0.0419(9) Uani 1 1 d . . . C9 C 0.5859(3) 0.5726(2) 0.2001(2) 0.0337(8) Uani 1 1 d . . . C10 C 0.5799(3) 0.5112(3) 0.3364(2) 0.0393(9) Uani 1 1 d . . . C11 C 0.4196(3) 0.6560(3) 0.3772(2) 0.0393(9) Uani 1 1 d . . . O2 O 0.3945(3) 0.7849(2) 0.19577(15) 0.0518(7) Uani 1 1 d . . . O3 O 0.6425(2) 0.55093(18) 0.14688(14) 0.0397(6) Uani 1 1 d . . . O4 O 0.6329(2) 0.4509(2) 0.36353(15) 0.0532(7) Uani 1 1 d . . . O5 O 0.3699(2) 0.6784(2) 0.43177(16) 0.0559(8) Uani 1 1 d . . . C12 C 0.6261(3) 0.6989(3) 0.2760(2) 0.0449(10) Uani 1 1 d . . . O6 O 0.7016(2) 0.7496(2) 0.2701(2) 0.0663(9) Uani 1 1 d . . . C13 C 0.2559(2) 0.2890(2) 0.25236(15) 0.0185(6) Uani 1 1 d . . . C14 C 0.1974(2) 0.3250(2) 0.19897(15) 0.0185(6) Uani 1 1 d . . . C15 C 0.1976(2) 0.2638(2) 0.15072(16) 0.0218(6) Uani 1 1 d . . . H5 H 0.1563 0.2868 0.1160 0.026 Uiso 1 1 calc R . . C16 C 0.2558(3) 0.1707(2) 0.15168(16) 0.0212(6) Uani 1 1 d . . . C17 C 0.3192(3) 0.1410(2) 0.20096(16) 0.0215(6) Uani 1 1 d . . . H6 H 0.3626 0.0792 0.2006 0.026 Uiso 1 1 calc R . . C18 C 0.3227(2) 0.1973(2) 0.25122(15) 0.0185(6) Uani 1 1 d . . . C19 C 0.1423(3) 0.4293(2) 0.18706(16) 0.0224(6) Uani 1 1 d . . . H7 H 0.1368 0.4536 0.2321 0.027 Uiso 1 1 calc R . . C20 C 0.2545(3) 0.1035(2) 0.09988(16) 0.0253(7) Uani 1 1 d . . . H8 H 0.3154 0.0501 0.1069 0.030 Uiso 1 1 calc R . . C21 C 0.4052(3) 0.1579(2) 0.29701(16) 0.0211(6) Uani 1 1 d . . . H9 H 0.3854 0.1982 0.3358 0.025 Uiso 1 1 calc R . . Si1 Si 0.24980(8) 0.51857(6) 0.11164(5) 0.0262(2) Uani 1 1 d . . . Si2 Si -0.01723(8) 0.43920(7) 0.18411(5) 0.0297(2) Uani 1 1 d . . . Si3 Si 0.31495(9) 0.16561(7) 0.00024(5) 0.0326(2) Uani 1 1 d . . . Si4 Si 0.11211(9) 0.03227(7) 0.12867(5) 0.0360(2) Uani 1 1 d . . . Si5 Si 0.56779(7) 0.18312(7) 0.24217(5) 0.0270(2) Uani 1 1 d . . . Si6 Si 0.38480(8) 0.02122(7) 0.34647(5) 0.0301(2) Uani 1 1 d . . . C22 C 0.4038(3) 0.4790(3) 0.11182(19) 0.0344(8) Uani 1 1 d . . . H10 H 0.4197 0.4106 0.1034 0.052 Uiso 1 1 calc R . . H11 H 0.4127 0.4815 0.1589 0.052 Uiso 1 1 calc R . . H12 H 0.4602 0.5241 0.0732 0.052 Uiso 1 1 calc R . . C23 C 0.2207(4) 0.6479(3) 0.1309(2) 0.0473(10) Uani 1 1 d . . . H13 H 0.2154 0.6457 0.1816 0.071 Uiso 1 1 calc R . . H14 H 0.1458 0.6746 0.1225 0.071 Uiso 1 1 calc R . . H15 H 0.2856 0.6911 0.0986 0.071 Uiso 1 1 calc R . . C24 C 0.2409(3) 0.5224(3) 0.01876(18) 0.0421(9) Uani 1 1 d . . . H16 H 0.3068 0.5608 -0.0175 0.063 Uiso 1 1 calc R . . H17 H 0.1654 0.5543 0.0146 0.063 Uiso 1 1 calc R . . H18 H 0.2457 0.4541 0.0103 0.063 Uiso 1 1 calc R . . C25 C -0.0758(4) 0.5681(3) 0.1921(3) 0.0593(12) Uani 1 1 d . . . H19 H -0.1626 0.5691 0.2056 0.089 Uiso 1 1 calc R . . H20 H -0.0439 0.6139 0.1454 0.089 Uiso 1 1 calc R . . H21 H -0.0517 0.5892 0.2296 0.089 Uiso 1 1 calc R . . C26 C -0.0397(3) 0.4120(3) 0.1009(2) 0.0464(10) Uani 1 1 d . . . H22 H -0.1196 0.4345 0.0991 0.070 Uiso 1 1 calc R . . H23 H -0.0306 0.3399 0.1023 0.070 Uiso 1 1 calc R . . H24 H 0.0192 0.4473 0.0576 0.070 Uiso 1 1 calc R . . C27 C -0.1100(3) 0.3492(3) 0.2621(2) 0.0417(9) Uani 1 1 d . . . H25 H -0.1128 0.3676 0.3077 0.063 Uiso 1 1 calc R . . H26 H -0.0755 0.2816 0.2611 0.063 Uiso 1 1 calc R . . H27 H -0.1906 0.3510 0.2586 0.063 Uiso 1 1 calc R . . C28 C 0.4355(3) 0.2502(3) -0.00993(19) 0.0417(9) Uani 1 1 d . . . H28 H 0.4749 0.2756 -0.0617 0.063 Uiso 1 1 calc R . . H29 H 0.4934 0.2131 0.0125 0.063 Uiso 1 1 calc R . . H30 H 0.4017 0.3063 0.0140 0.063 Uiso 1 1 calc R . . C29 C 0.1991(4) 0.2366(3) -0.0378(2) 0.0473(10) Uani 1 1 d . . . H31 H 0.1642 0.2898 -0.0110 0.071 Uiso 1 1 calc R . . H32 H 0.1369 0.1910 -0.0331 0.071 Uiso 1 1 calc R . . H33 H 0.2354 0.2661 -0.0893 0.071 Uiso 1 1 calc R . . C30 C 0.3810(4) 0.0679(3) -0.0548(2) 0.0574(12) Uani 1 1 d . . . H34 H 0.4230 0.1002 -0.1048 0.086 Uiso 1 1 calc R . . H35 H 0.3177 0.0270 -0.0551 0.086 Uiso 1 1 calc R . . H36 H 0.4369 0.0251 -0.0334 0.086 Uiso 1 1 calc R . . C31 C -0.0209(3) 0.1155(3) 0.1334(3) 0.0566(11) Uani 1 1 d . . . H37 H -0.0916 0.0749 0.1477 0.085 Uiso 1 1 calc R . . H38 H -0.0125 0.1586 0.0856 0.085 Uiso 1 1 calc R . . H39 H -0.0291 0.1569 0.1693 0.085 Uiso 1 1 calc R . . C32 C 0.1189(4) -0.0523(3) 0.0652(2) 0.0516(11) Uani 1 1 d . . . H40 H 0.0500 -0.0955 0.0851 0.077 Uiso 1 1 calc R . . H41 H 0.1919 -0.0936 0.0594 0.077 Uiso 1 1 calc R . . H42 H 0.1183 -0.0121 0.0178 0.077 Uiso 1 1 calc R . . C33 C 0.0943(5) -0.0474(4) 0.2207(2) 0.0673(14) Uani 1 1 d . . . H43 H 0.0805 -0.0047 0.2564 0.101 Uiso 1 1 calc R . . H44 H 0.1666 -0.0884 0.2201 0.101 Uiso 1 1 calc R . . H45 H 0.0266 -0.0910 0.2340 0.101 Uiso 1 1 calc R . . C34 C 0.5942(3) 0.3192(3) 0.2163(2) 0.0359(8) Uani 1 1 d . . . H46 H 0.6761 0.3310 0.1849 0.054 Uiso 1 1 calc R . . H47 H 0.5814 0.3461 0.2602 0.054 Uiso 1 1 calc R . . H48 H 0.5392 0.3526 0.1901 0.054 Uiso 1 1 calc R . . C35 C 0.6141(3) 0.1353(3) 0.1558(2) 0.0441(9) Uani 1 1 d . . . H49 H 0.5652 0.1678 0.1252 0.066 Uiso 1 1 calc R . . H50 H 0.6039 0.0629 0.1669 0.066 Uiso 1 1 calc R . . H51 H 0.6977 0.1502 0.1299 0.066 Uiso 1 1 calc R . . C36 C 0.6680(3) 0.1272(3) 0.2979(2) 0.0433(9) Uani 1 1 d . . . H52 H 0.7495 0.1481 0.2713 0.065 Uiso 1 1 calc R . . H53 H 0.6650 0.0541 0.3075 0.065 Uiso 1 1 calc R . . H54 H 0.6418 0.1502 0.3441 0.065 Uiso 1 1 calc R . . C37 C 0.2299(3) -0.0194(3) 0.3709(2) 0.0443(9) Uani 1 1 d . . . H55 H 0.2263 -0.0916 0.3901 0.066 Uiso 1 1 calc R . . H56 H 0.2033 -0.0036 0.3276 0.066 Uiso 1 1 calc R . . H57 H 0.1783 0.0157 0.4079 0.066 Uiso 1 1 calc R . . C38 C 0.4790(4) -0.0688(3) 0.2924(2) 0.0470(10) Uani 1 1 d . . . H58 H 0.4691 -0.1366 0.3222 0.070 Uiso 1 1 calc R . . H59 H 0.5624 -0.0507 0.2777 0.070 Uiso 1 1 calc R . . H60 H 0.4549 -0.0664 0.2491 0.070 Uiso 1 1 calc R . . C39 C 0.4203(4) 0.0024(3) 0.4337(2) 0.0516(11) Uani 1 1 d . . . H61 H 0.3727 0.0496 0.4628 0.077 Uiso 1 1 calc R . . H62 H 0.5048 0.0138 0.4235 0.077 Uiso 1 1 calc R . . H63 H 0.4020 -0.0662 0.4607 0.077 Uiso 1 1 calc R . . C40 C 0.2024(3) 0.2662(2) 0.43006(17) 0.0289(7) Uani 1 1 d . . . C41 C 0.0948(3) 0.2141(3) 0.45316(18) 0.0318(8) Uani 1 1 d . . . C42 C 0.0661(3) 0.1439(3) 0.51840(18) 0.0389(8) Uani 1 1 d . . . H64 H -0.0041 0.1068 0.5329 0.047 Uiso 1 1 calc R . . C43 C 0.1395(3) 0.1282(3) 0.56219(19) 0.0402(9) Uani 1 1 d . . . H65 H 0.1207 0.0790 0.6058 0.048 Uiso 1 1 calc R . . C44 C 0.2402(3) 0.1841(3) 0.54231(19) 0.0400(9) Uani 1 1 d . . . H66 H 0.2870 0.1767 0.5742 0.048 Uiso 1 1 calc R . . C45 C 0.2737(3) 0.2517(2) 0.47545(17) 0.0302(7) Uani 1 1 d . . . C46 C 0.0020(3) 0.2342(3) 0.41236(18) 0.0342(8) Uani 1 1 d . . . H67 H 0.0321 0.2893 0.3693 0.041 Uiso 1 1 calc R . . C47 C 0.3860(3) 0.3102(3) 0.4583(2) 0.0388(8) Uani 1 1 d . . . H68 H 0.4137 0.3363 0.4046 0.047 Uiso 1 1 calc R . . C48 C -0.0196(4) 0.1453(3) 0.3841(2) 0.0526(11) Uani 1 1 d . . . H69 H 0.0516 0.1309 0.3457 0.079 Uiso 1 1 calc R . . H70 H -0.0866 0.1609 0.3645 0.079 Uiso 1 1 calc R . . H71 H -0.0377 0.0868 0.4240 0.079 Uiso 1 1 calc R . . C49 C -0.1146(3) 0.2731(3) 0.4620(2) 0.0517(11) Uani 1 1 d . . . H72 H -0.1542 0.2175 0.5000 0.077 Uiso 1 1 calc R . . H73 H -0.1670 0.3023 0.4328 0.077 Uiso 1 1 calc R . . H74 H -0.0964 0.3242 0.4844 0.077 Uiso 1 1 calc R . . C50 C 0.4877(4) 0.2460(3) 0.4787(2) 0.0540(11) Uani 1 1 d . . . H75 H 0.5611 0.2837 0.4582 0.081 Uiso 1 1 calc R . . H76 H 0.4984 0.1848 0.4592 0.081 Uiso 1 1 calc R . . H77 H 0.4685 0.2285 0.5317 0.081 Uiso 1 1 calc R . . C51 C 0.3590(4) 0.3990(3) 0.4947(2) 0.0507(10) Uani 1 1 d . . . H78 H 0.3339 0.3757 0.5476 0.076 Uiso 1 1 calc R . . H79 H 0.2952 0.4402 0.4804 0.076 Uiso 1 1 calc R . . H80 H 0.4303 0.4389 0.4799 0.076 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 Ge1 0.01970(17) 0.01972(18) 0.02005(17) -0.00591(12) -0.00563(13) 0.00141(12) C1 0.0346(18) 0.0291(19) 0.0252(17) -0.0056(14) -0.0085(14) -0.0021(15) O1 0.0282(12) 0.0276(13) 0.0304(12) -0.0115(10) -0.0060(10) -0.0012(10) C2 0.0302(17) 0.0318(19) 0.0234(16) -0.0086(14) -0.0094(14) 0.0037(14) C3 0.0330(18) 0.0306(18) 0.0258(17) -0.0091(14) -0.0088(14) 0.0018(15) C4 0.040(2) 0.0297(19) 0.044(2) -0.0143(16) -0.0139(17) 0.0017(16) C5 0.040(2) 0.037(2) 0.053(2) -0.0228(18) -0.0144(18) 0.0105(17) C6 0.038(2) 0.046(2) 0.051(2) -0.0199(19) -0.0135(18) 0.0120(18) C7 0.0265(17) 0.0351(19) 0.0318(18) -0.0118(15) -0.0064(14) 0.0044(15) Cr1 0.0278(3) 0.0316(3) 0.0425(3) -0.0182(3) -0.0068(2) -0.0037(2) C8 0.044(2) 0.038(2) 0.046(2) -0.0183(19) -0.0098(18) -0.0045(18) C9 0.0286(18) 0.0270(19) 0.048(2) -0.0100(16) -0.0111(17) -0.0080(15) C10 0.035(2) 0.041(2) 0.044(2) -0.0189(18) -0.0076(17) -0.0011(18) C11 0.0322(19) 0.040(2) 0.055(2) -0.0230(19) -0.0178(18) -0.0002(16) O2 0.0584(18) 0.0462(17) 0.0532(17) -0.0078(14) -0.0225(15) 0.0014(14) O3 0.0390(14) 0.0375(15) 0.0415(15) -0.0157(12) -0.0045(12) -0.0050(11) O4 0.0477(17) 0.0584(19) 0.0523(17) -0.0137(15) -0.0146(14) 0.0087(15) O5 0.0475(16) 0.076(2) 0.0586(18) -0.0443(17) -0.0181(14) 0.0079(15) C12 0.035(2) 0.034(2) 0.070(3) -0.026(2) -0.0123(19) 0.0013(18) O6 0.0378(16) 0.0466(18) 0.121(3) -0.0396(18) -0.0159(16) -0.0091(14) C13 0.0158(14) 0.0193(15) 0.0204(15) -0.0060(12) -0.0043(12) -0.0009(12) C14 0.0157(14) 0.0177(15) 0.0202(15) -0.0016(12) -0.0038(12) -0.0017(12) C15 0.0190(15) 0.0264(17) 0.0218(16) -0.0042(13) -0.0086(12) -0.0029(13) C16 0.0208(15) 0.0216(16) 0.0221(16) -0.0067(12) -0.0056(12) -0.0033(13) C17 0.0201(15) 0.0180(15) 0.0265(16) -0.0068(13) -0.0060(13) 0.0004(12) C18 0.0167(14) 0.0186(15) 0.0192(15) -0.0025(12) -0.0051(12) -0.0009(12) C19 0.0232(15) 0.0243(16) 0.0232(16) -0.0056(13) -0.0120(13) 0.0016(13) C20 0.0289(17) 0.0234(17) 0.0291(17) -0.0111(13) -0.0119(14) -0.0026(13) C21 0.0235(16) 0.0187(15) 0.0246(16) -0.0093(12) -0.0114(13) 0.0081(12) Si1 0.0294(5) 0.0226(5) 0.0283(5) 0.0000(4) -0.0141(4) -0.0025(4) Si2 0.0230(5) 0.0293(5) 0.0403(5) -0.0053(4) -0.0173(4) 0.0045(4) Si3 0.0405(6) 0.0356(5) 0.0243(5) -0.0121(4) -0.0077(4) -0.0070(4) Si4 0.0423(6) 0.0342(6) 0.0365(5) -0.0076(4) -0.0149(4) -0.0143(5) Si5 0.0215(4) 0.0256(5) 0.0383(5) -0.0124(4) -0.0129(4) 0.0048(4) Si6 0.0372(5) 0.0221(5) 0.0329(5) -0.0028(4) -0.0169(4) 0.0054(4) C22 0.0288(18) 0.039(2) 0.0342(19) 0.0014(16) -0.0122(15) -0.0063(16) C23 0.057(3) 0.029(2) 0.055(2) -0.0030(18) -0.018(2) -0.0057(18) C24 0.043(2) 0.056(2) 0.0280(19) 0.0036(17) -0.0171(16) -0.0140(19) C25 0.041(2) 0.047(3) 0.103(4) -0.027(2) -0.039(2) 0.020(2) C26 0.034(2) 0.065(3) 0.045(2) 0.002(2) -0.0244(18) -0.0087(19) C27 0.0241(18) 0.061(3) 0.042(2) -0.0116(19) -0.0112(16) -0.0039(17) C28 0.041(2) 0.053(2) 0.0299(19) -0.0129(17) -0.0022(16) -0.0155(18) C29 0.065(3) 0.049(2) 0.033(2) -0.0007(17) -0.0243(19) -0.015(2) C30 0.076(3) 0.057(3) 0.040(2) -0.029(2) -0.004(2) -0.006(2) C31 0.036(2) 0.055(3) 0.082(3) -0.027(2) -0.011(2) -0.011(2) C32 0.062(3) 0.042(2) 0.062(3) -0.021(2) -0.024(2) -0.016(2) C33 0.084(3) 0.070(3) 0.048(3) 0.009(2) -0.021(2) -0.049(3) C34 0.0242(17) 0.034(2) 0.051(2) -0.0117(17) -0.0114(16) -0.0013(15) C35 0.0306(19) 0.055(3) 0.049(2) -0.029(2) -0.0030(17) -0.0039(18) C36 0.0308(19) 0.041(2) 0.064(3) -0.0087(19) -0.0255(18) 0.0040(17) C37 0.048(2) 0.036(2) 0.042(2) 0.0062(17) -0.0106(18) -0.0067(18) C38 0.052(2) 0.0233(19) 0.063(3) -0.0093(18) -0.016(2) 0.0055(17) C39 0.074(3) 0.042(2) 0.046(2) 0.0001(19) -0.036(2) 0.007(2) C40 0.0334(18) 0.0265(18) 0.0239(17) -0.0054(13) -0.0054(14) 0.0026(14) C41 0.0354(19) 0.0304(19) 0.0289(18) -0.0082(15) -0.0075(15) 0.0002(15) C42 0.042(2) 0.038(2) 0.0314(19) -0.0064(16) -0.0039(16) -0.0033(17) C43 0.053(2) 0.035(2) 0.0287(19) -0.0012(15) -0.0102(17) -0.0002(18) C44 0.050(2) 0.043(2) 0.032(2) -0.0073(17) -0.0219(17) 0.0060(18) C45 0.0363(19) 0.0280(18) 0.0261(17) -0.0062(14) -0.0097(14) 0.0020(15) C46 0.0273(18) 0.040(2) 0.0317(18) 0.0026(15) -0.0081(14) -0.0103(15) C47 0.042(2) 0.044(2) 0.034(2) -0.0059(16) -0.0189(16) 0.0035(17) C48 0.060(3) 0.041(2) 0.068(3) -0.005(2) -0.035(2) -0.010(2) C49 0.036(2) 0.064(3) 0.042(2) 0.002(2) -0.0022(18) -0.002(2) C50 0.052(3) 0.055(3) 0.063(3) -0.003(2) -0.035(2) 0.001(2) C51 0.048(2) 0.053(3) 0.056(3) -0.015(2) -0.016(2) -0.013(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 Ge1 O1 1.904(2) . ? Ge1 C2 1.947(3) . ? Ge1 C13 1.966(3) . ? Ge1 C40 1.986(3) . ? C1 O1 1.292(4) . ? C1 C3 1.510(5) . ? C1 Cr1 2.050(3) . ? C2 C7 1.402(4) . ? C2 C3 1.403(5) . ? C3 C4 1.396(5) . ? C4 C5 1.387(5) . ? C5 C6 1.382(5) . ? C6 C7 1.392(5) . ? Cr1 C12 1.883(4) . ? Cr1 C10 1.888(4) . ? Cr1 C11 1.893(4) . ? Cr1 C8 1.903(4) . ? Cr1 C9 1.911(4) . ? C8 O2 1.163(5) . ? C9 O3 1.141(4) . ? C10 O4 1.137(4) . ? C11 O5 1.148(4) . ? C12 O6 1.147(4) . ? C13 C14 1.420(4) . ? C13 C18 1.424(4) . ? C14 C15 1.402(4) . ? C14 C19 1.520(4) . ? C15 C16 1.394(4) . ? C16 C17 1.387(4) . ? C16 C20 1.526(4) . ? C17 C18 1.399(4) . ? C18 C21 1.524(4) . ? C19 Si2 1.907(3) . ? C19 Si1 1.908(3) . ? C20 Si4 1.896(3) . ? C20 Si3 1.901(3) . ? C21 Si6 1.913(3) . ? C21 Si5 1.914(3) . ? Si1 C22 1.861(3) . ? Si1 C24 1.865(3) . ? Si1 C23 1.874(4) . ? Si2 C27 1.861(4) . ? Si2 C25 1.860(4) . ? Si2 C26 1.869(4) . ? Si3 C28 1.860(3) . ? Si3 C29 1.870(4) . ? Si3 C30 1.872(4) . ? Si4 C31 1.852(4) . ? Si4 C32 1.868(4) . ? Si4 C33 1.868(4) . ? Si5 C34 1.853(3) . ? Si5 C35 1.867(4) . ? Si5 C36 1.875(3) . ? Si6 C37 1.855(4) . ? Si6 C39 1.864(4) . ? Si6 C38 1.868(4) . ? C40 C45 1.392(4) . ? C40 C41 1.418(5) . ? C41 C42 1.396(5) . ? C41 C46 1.534(5) . ? C42 C43 1.386(5) . ? C43 C44 1.384(5) . ? C44 C45 1.403(5) . ? C45 C47 1.526(5) . ? C46 C48 1.521(5) . ? C46 C49 1.550(5) . ? C47 C51 1.509(5) . ? C47 C50 1.535(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 C2 85.39(12) . . ? O1 Ge1 C13 106.47(10) . . ? C2 Ge1 C13 124.90(12) . . ? O1 Ge1 C40 112.60(11) . . ? C2 Ge1 C40 109.19(13) . . ? C13 Ge1 C40 114.32(12) . . ? O1 C1 C3 111.1(3) . . ? O1 C1 Cr1 120.6(2) . . ? C3 C1 Cr1 128.2(2) . . ? C1 O1 Ge1 117.9(2) . . ? C7 C2 C3 120.7(3) . . ? C7 C2 Ge1 130.5(3) . . ? C3 C2 Ge1 108.6(2) . . ? C4 C3 C2 118.7(3) . . ? C4 C3 C1 124.4(3) . . ? C2 C3 C1 116.9(3) . . ? C5 C4 C3 120.9(3) . . ? C6 C5 C4 119.7(3) . . ? C5 C6 C7 121.3(3) . . ? C6 C7 C2 118.7(3) . . ? C12 Cr1 C10 87.97(16) . . ? C12 Cr1 C11 89.15(16) . . ? C10 Cr1 C11 90.83(16) . . ? C12 Cr1 C8 90.44(17) . . ? C10 Cr1 C8 174.98(16) . . ? C11 Cr1 C8 93.90(16) . . ? C12 Cr1 C9 90.31(15) . . ? C10 Cr1 C9 87.44(15) . . ? C11 Cr1 C9 178.21(16) . . ? C8 Cr1 C9 87.81(15) . . ? C12 Cr1 C1 175.54(15) . . ? C10 Cr1 C1 91.90(14) . . ? C11 Cr1 C1 86.39(14) . . ? C8 Cr1 C1 90.05(14) . . ? C9 Cr1 C1 94.13(13) . . ? O2 C8 Cr1 176.8(3) . . ? O3 C9 Cr1 175.5(3) . . ? O4 C10 Cr1 176.4(3) . . ? O5 C11 Cr1 178.6(4) . . ? O6 C12 Cr1 178.4(4) . . ? C14 C13 C18 119.7(2) . . ? C14 C13 Ge1 121.1(2) . . ? C18 C13 Ge1 118.9(2) . . ? C15 C14 C13 118.5(3) . . ? C15 C14 C19 117.5(2) . . ? C13 C14 C19 123.9(2) . . ? C16 C15 C14 122.6(3) . . ? C17 C16 C15 117.4(3) . . ? C17 C16 C20 119.9(3) . . ? C15 C16 C20 122.7(3) . . ? C16 C17 C18 123.4(3) . . ? C17 C18 C13 118.0(2) . . ? C17 C18 C21 116.4(2) . . ? C13 C18 C21 125.4(2) . . ? C14 C19 Si2 117.1(2) . . ? C14 C19 Si1 111.1(2) . . ? Si2 C19 Si1 115.31(15) . . ? C16 C20 Si4 113.2(2) . . ? C16 C20 Si3 113.3(2) . . ? Si4 C20 Si3 117.34(15) . . ? C18 C21 Si6 115.4(2) . . ? C18 C21 Si5 111.5(2) . . ? Si6 C21 Si5 111.15(14) . . ? C22 Si1 C24 107.83(17) . . ? C22 Si1 C23 108.39(17) . . ? C24 Si1 C23 108.55(18) . . ? C22 Si1 C19 108.50(14) . . ? C24 Si1 C19 114.32(15) . . ? C23 Si1 C19 109.11(16) . . ? C27 Si2 C25 108.7(2) . . ? C27 Si2 C26 105.96(17) . . ? C25 Si2 C26 107.7(2) . . ? C27 Si2 C19 109.63(15) . . ? C25 Si2 C19 108.57(16) . . ? C26 Si2 C19 116.05(15) . . ? C28 Si3 C29 110.17(18) . . ? C28 Si3 C30 107.84(19) . . ? C29 Si3 C30 107.36(19) . . ? C28 Si3 C20 108.55(14) . . ? C29 Si3 C20 113.37(16) . . ? C30 Si3 C20 109.41(17) . . ? C31 Si4 C32 108.46(19) . . ? C31 Si4 C33 108.4(2) . . ? C32 Si4 C33 107.7(2) . . ? C31 Si4 C20 112.90(17) . . ? C32 Si4 C20 110.96(17) . . ? C33 Si4 C20 108.32(17) . . ? C34 Si5 C35 106.53(18) . . ? C34 Si5 C36 106.46(16) . . ? C35 Si5 C36 109.43(18) . . ? C34 Si5 C21 110.64(14) . . ? C35 Si5 C21 112.81(14) . . ? C36 Si5 C21 110.71(16) . . ? C37 Si6 C39 106.04(19) . . ? C37 Si6 C38 105.79(18) . . ? C39 Si6 C38 107.90(19) . . ? C37 Si6 C21 112.69(15) . . ? C39 Si6 C21 110.34(16) . . ? C38 Si6 C21 113.64(16) . . ? C45 C40 C41 119.3(3) . . ? C45 C40 Ge1 126.1(2) . . ? C41 C40 Ge1 114.6(2) . . ? C42 C41 C40 119.7(3) . . ? C42 C41 C46 116.6(3) . . ? C40 C41 C46 123.6(3) . . ? C43 C42 C41 120.4(3) . . ? C42 C43 C44 120.0(3) . . ? C43 C44 C45 120.5(3) . . ? C40 C45 C44 119.9(3) . . ? C40 C45 C47 123.2(3) . . ? C44 C45 C47 116.8(3) . . ? C48 C46 C41 114.3(3) . . ? C48 C46 C49 111.4(3) . . ? C41 C46 C49 108.9(3) . . ? C51 C47 C45 110.5(3) . . ? C51 C47 C50 110.3(3) . . ? C45 C47 C50 113.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 O1 Ge1 1.1(3) . . . . ? Cr1 C1 O1 Ge1 177.48(13) . . . . ? C2 Ge1 O1 C1 0.3(2) . . . . ? C13 Ge1 O1 C1 125.4(2) . . . . ? C40 Ge1 O1 C1 -108.6(2) . . . . ? O1 Ge1 C2 C7 -176.7(3) . . . . ? C13 Ge1 C2 C7 76.4(3) . . . . ? C40 Ge1 C2 C7 -64.4(3) . . . . ? O1 Ge1 C2 C3 -1.7(2) . . . . ? C13 Ge1 C2 C3 -108.6(2) . . . . ? C40 Ge1 C2 C3 110.7(2) . . . . ? C7 C2 C3 C4 -1.4(5) . . . . ? Ge1 C2 C3 C4 -177.1(2) . . . . ? C7 C2 C3 C1 178.4(3) . . . . ? Ge1 C2 C3 C1 2.8(3) . . . . ? O1 C1 C3 C4 177.2(3) . . . . ? Cr1 C1 C3 C4 1.2(5) . . . . ? O1 C1 C3 C2 -2.7(4) . . . . ? Cr1 C1 C3 C2 -178.7(2) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C1 C3 C4 C5 -179.1(3) . . . . ? C3 C4 C5 C6 0.3(6) . . . . ? C4 C5 C6 C7 -0.6(6) . . . . ? C5 C6 C7 C2 -0.1(5) . . . . ? C3 C2 C7 C6 1.2(5) . . . . ? Ge1 C2 C7 C6 175.7(3) . . . . ? O1 C1 Cr1 C12 -124(2) . . . . ? C3 C1 Cr1 C12 52(2) . . . . ? O1 C1 Cr1 C10 -35.7(3) . . . . ? C3 C1 Cr1 C10 140.0(3) . . . . ? O1 C1 Cr1 C11 -126.4(3) . . . . ? C3 C1 Cr1 C11 49.3(3) . . . . ? O1 C1 Cr1 C8 139.7(3) . . . . ? C3 C1 Cr1 C8 -44.6(3) . . . . ? O1 C1 Cr1 C9 51.9(3) . . . . ? C3 C1 Cr1 C9 -132.5(3) . . . . ? C12 Cr1 C8 O2 38(6) . . . . ? C10 Cr1 C8 O2 -33(7) . . . . ? C11 Cr1 C8 O2 127(6) . . . . ? C9 Cr1 C8 O2 -52(6) . . . . ? C1 Cr1 C8 O2 -146(6) . . . . ? C12 Cr1 C9 O3 -1(4) . . . . ? C10 Cr1 C9 O3 -89(4) . . . . ? C11 Cr1 C9 O3 -74(7) . . . . ? C8 Cr1 C9 O3 89(4) . . . . ? C1 Cr1 C9 O3 179(100) . . . . ? C12 Cr1 C10 O4 -22(5) . . . . ? C11 Cr1 C10 O4 -111(5) . . . . ? C8 Cr1 C10 O4 49(6) . . . . ? C9 Cr1 C10 O4 68(5) . . . . ? C1 Cr1 C10 O4 162(5) . . . . ? C12 Cr1 C11 O5 -134(13) . . . . ? C10 Cr1 C11 O5 -46(13) . . . . ? C8 Cr1 C11 O5 136(13) . . . . ? C9 Cr1 C11 O5 -61(15) . . . . ? C1 Cr1 C11 O5 46(13) . . . . ? C10 Cr1 C12 O6 -70(13) . . . . ? C11 Cr1 C12 O6 21(13) . . . . ? C8 Cr1 C12 O6 114(13) . . . . ? C9 Cr1 C12 O6 -158(13) . . . . ? C1 Cr1 C12 O6 18(14) . . . . ? O1 Ge1 C13 C14 -101.8(2) . . . . ? C2 Ge1 C13 C14 -5.8(3) . . . . ? C40 Ge1 C13 C14 133.3(2) . . . . ? O1 Ge1 C13 C18 83.9(2) . . . . ? C2 Ge1 C13 C18 179.9(2) . . . . ? C40 Ge1 C13 C18 -41.1(3) . . . . ? C18 C13 C14 C15 6.2(4) . . . . ? Ge1 C13 C14 C15 -168.1(2) . . . . ? C18 C13 C14 C19 -168.9(3) . . . . ? Ge1 C13 C14 C19 16.8(4) . . . . ? C13 C14 C15 C16 -2.0(4) . . . . ? C19 C14 C15 C16 173.5(3) . . . . ? C14 C15 C16 C17 -2.6(4) . . . . ? C14 C15 C16 C20 179.1(3) . . . . ? C15 C16 C17 C18 3.1(4) . . . . ? C20 C16 C17 C18 -178.6(3) . . . . ? C16 C17 C18 C13 1.1(4) . . . . ? C16 C17 C18 C21 -175.0(3) . . . . ? C14 C13 C18 C17 -5.8(4) . . . . ? Ge1 C13 C18 C17 168.7(2) . . . . ? C14 C13 C18 C21 169.9(3) . . . . ? Ge1 C13 C18 C21 -15.6(4) . . . . ? C15 C14 C19 Si2 55.3(3) . . . . ? C13 C14 C19 Si2 -129.5(3) . . . . ? C15 C14 C19 Si1 -80.1(3) . . . . ? C13 C14 C19 Si1 95.1(3) . . . . ? C17 C16 C20 Si4 102.6(3) . . . . ? C15 C16 C20 Si4 -79.1(3) . . . . ? C17 C16 C20 Si3 -120.6(3) . . . . ? C15 C16 C20 Si3 57.6(3) . . . . ? C17 C18 C21 Si6 -52.2(3) . . . . ? C13 C18 C21 Si6 132.0(3) . . . . ? C17 C18 C21 Si5 75.9(3) . . . . ? C13 C18 C21 Si5 -99.9(3) . . . . ? C14 C19 Si1 C22 -31.5(2) . . . . ? Si2 C19 Si1 C22 -167.76(17) . . . . ? C14 C19 Si1 C24 88.8(2) . . . . ? Si2 C19 Si1 C24 -47.4(2) . . . . ? C14 C19 Si1 C23 -149.4(2) . . . . ? Si2 C19 Si1 C23 74.3(2) . . . . ? C14 C19 Si2 C27 47.5(3) . . . . ? Si1 C19 Si2 C27 -178.90(17) . . . . ? C14 C19 Si2 C25 166.2(3) . . . . ? Si1 C19 Si2 C25 -60.3(2) . . . . ? C14 C19 Si2 C26 -72.4(3) . . . . ? Si1 C19 Si2 C26 61.2(2) . . . . ? C16 C20 Si3 C28 34.0(3) . . . . ? Si4 C20 Si3 C28 168.81(19) . . . . ? C16 C20 Si3 C29 -88.8(2) . . . . ? Si4 C20 Si3 C29 46.0(2) . . . . ? C16 C20 Si3 C30 151.4(2) . . . . ? Si4 C20 Si3 C30 -73.8(2) . . . . ? C16 C20 Si4 C31 60.3(3) . . . . ? Si3 C20 Si4 C31 -74.6(2) . . . . ? C16 C20 Si4 C32 -177.7(2) . . . . ? Si3 C20 Si4 C32 47.4(2) . . . . ? C16 C20 Si4 C33 -59.7(3) . . . . ? Si3 C20 Si4 C33 165.4(2) . . . . ? C18 C21 Si5 C34 65.6(2) . . . . ? Si6 C21 Si5 C34 -164.02(15) . . . . ? C18 C21 Si5 C35 -53.6(3) . . . . ? Si6 C21 Si5 C35 76.8(2) . . . . ? C18 C21 Si5 C36 -176.6(2) . . . . ? Si6 C21 Si5 C36 -46.2(2) . . . . ? C18 C21 Si6 C37 -30.2(3) . . . . ? Si5 C21 Si6 C37 -158.46(17) . . . . ? C18 C21 Si6 C39 -148.5(2) . . . . ? Si5 C21 Si6 C39 83.2(2) . . . . ? C18 C21 Si6 C38 90.2(2) . . . . ? Si5 C21 Si6 C38 -38.1(2) . . . . ? O1 Ge1 C40 C45 -4.3(3) . . . . ? C2 Ge1 C40 C45 -97.3(3) . . . . ? C13 Ge1 C40 C45 117.4(3) . . . . ? O1 Ge1 C40 C41 174.6(2) . . . . ? C2 Ge1 C40 C41 81.6(3) . . . . ? C13 Ge1 C40 C41 -63.7(3) . . . . ? C45 C40 C41 C42 -4.6(5) . . . . ? Ge1 C40 C41 C42 176.4(2) . . . . ? C45 C40 C41 C46 171.8(3) . . . . ? Ge1 C40 C41 C46 -7.2(4) . . . . ? C40 C41 C42 C43 2.8(5) . . . . ? C46 C41 C42 C43 -173.8(3) . . . . ? C41 C42 C43 C44 1.8(5) . . . . ? C42 C43 C44 C45 -4.7(6) . . . . ? C41 C40 C45 C44 1.7(5) . . . . ? Ge1 C40 C45 C44 -179.4(3) . . . . ? C41 C40 C45 C47 -175.1(3) . . . . ? Ge1 C40 C45 C47 3.8(5) . . . . ? C43 C44 C45 C40 2.9(5) . . . . ? C43 C44 C45 C47 180.0(3) . . . . ? C42 C41 C46 C48 -65.5(4) . . . . ? C40 C41 C46 C48 118.0(4) . . . . ? C42 C41 C46 C49 59.9(4) . . . . ? C40 C41 C46 C49 -116.7(4) . . . . ? C40 C45 C47 C51 95.1(4) . . . . ? C44 C45 C47 C51 -81.9(4) . . . . ? C40 C45 C47 C50 -140.6(3) . . . . ? C44 C45 C47 C50 42.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.048 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.071 #--------------------------------------------------------- data_mo _database_code_depnum_ccdc_archive 'CCDC 224029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common 'Mo complex' _chemical_melting_point ? _chemical_formula_moiety 'C51 H80 O6 Ge1 Mo1 Si6' _chemical_formula_sum 'C51 H80 Ge Mo O6 Si6' _chemical_formula_weight 1126.22 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' O O 0.0106 0.0060 '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' Mo Mo -1.6832 0.6857 '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 11.911(5) _cell_length_b 13.826(6) _cell_length_c 19.818(8) _cell_angle_alpha 77.247(12) _cell_angle_beta 71.363(11) _cell_angle_gamma 84.446(14) _cell_volume 3015(2) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisum _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7512 _exptl_absorpt_correction_T_max 0.8457 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU/MSC Meacury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20001 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10414 _reflns_number_gt 8307 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10414 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Ge1 Ge 0.73198(5) 0.35315(4) 0.83432(3) 0.01085(16) Uani 1 1 d . . . C1 C 0.6439(5) 0.4763(4) 0.8458(3) 0.0162(12) Uani 1 1 d . . . C2 C 0.5215(5) 0.4975(4) 0.8681(3) 0.0196(13) Uani 1 1 d . . . H1 H 0.4671 0.4465 0.8777 0.024 Uiso 1 1 calc R . . C3 C 0.4792(5) 0.5937(4) 0.8763(3) 0.0257(14) Uani 1 1 d . . . H2 H 0.3964 0.6083 0.8908 0.031 Uiso 1 1 calc R . . C4 C 0.5593(5) 0.6682(4) 0.8631(4) 0.0262(14) Uani 1 1 d . . . H3 H 0.5308 0.7335 0.8684 0.031 Uiso 1 1 calc R . . C5 C 0.6800(5) 0.6474(4) 0.8423(3) 0.0251(14) Uani 1 1 d . . . H4 H 0.7337 0.6984 0.8341 0.030 Uiso 1 1 calc R . . C6 C 0.7237(5) 0.5516(4) 0.8334(3) 0.0172(12) Uani 1 1 d . . . C7 C 0.8527(5) 0.5235(4) 0.8114(3) 0.0150(12) Uani 1 1 d . . . O1 O 0.8684(3) 0.4297(3) 0.8101(2) 0.0157(8) Uani 1 1 d . . . Mo1 Mo 1.00432(4) 0.61762(4) 0.78744(3) 0.01845(16) Uani 1 1 d . . . C8 C 1.1400(5) 0.7065(5) 0.7735(4) 0.0321(16) Uani 1 1 d . . . O2 O 1.2147(4) 0.7566(4) 0.7676(4) 0.0558(17) Uani 1 1 d . . . C9 C 1.0898(5) 0.5076(5) 0.8398(3) 0.0238(14) Uani 1 1 d . . . O3 O 1.1448(4) 0.4489(4) 0.8680(3) 0.0407(12) Uani 1 1 d . . . C10 C 0.9151(5) 0.6603(5) 0.8832(4) 0.0264(15) Uani 1 1 d . . . O4 O 0.8640(4) 0.6809(4) 0.9377(3) 0.0473(14) Uani 1 1 d . . . C11 C 0.9263(5) 0.7293(5) 0.7296(4) 0.0286(15) Uani 1 1 d . . . O5 O 0.8868(4) 0.7924(3) 0.6946(3) 0.0368(12) Uani 1 1 d . . . C12 C 1.0973(5) 0.5712(4) 0.6924(4) 0.0226(13) Uani 1 1 d . . . O6 O 1.1528(4) 0.5492(3) 0.6395(2) 0.0287(10) Uani 1 1 d . . . C13 C 0.7551(4) 0.2872(4) 0.7526(3) 0.0118(11) Uani 1 1 d . . . C14 C 0.6972(4) 0.3231(4) 0.6989(3) 0.0109(11) Uani 1 1 d . . . C15 C 0.6985(5) 0.2625(4) 0.6506(3) 0.0159(12) Uani 1 1 d . . . H5 H 0.6579 0.2858 0.6156 0.019 Uiso 1 1 calc R . . C16 C 0.7559(4) 0.1704(4) 0.6510(3) 0.0113(11) Uani 1 1 d . . . C17 C 0.8202(4) 0.1411(4) 0.7004(3) 0.0126(11) Uani 1 1 d . . . H6 H 0.8646 0.0802 0.6997 0.015 Uiso 1 1 calc R . . C18 C 0.8223(4) 0.1968(4) 0.7505(3) 0.0118(11) Uani 1 1 d . . . C19 C 0.6412(5) 0.4270(4) 0.6877(3) 0.0152(12) Uani 1 1 d . . . H7 H 0.6343 0.4501 0.7333 0.018 Uiso 1 1 calc R . . Si1 Si 0.74906(13) 0.51693(11) 0.61325(9) 0.0162(3) Uani 1 1 d . . . Si2 Si 0.48330(13) 0.43662(12) 0.68381(9) 0.0191(4) Uani 1 1 d . . . C20 C 0.9030(5) 0.4761(5) 0.6126(3) 0.0241(14) Uani 1 1 d . . . H8 H 0.9197 0.4097 0.6012 0.036 Uiso 1 1 calc R . . H9 H 0.9112 0.4743 0.6605 0.036 Uiso 1 1 calc R . . H10 H 0.9592 0.5227 0.5757 0.036 Uiso 1 1 calc R . . C21 C 0.7209(6) 0.6430(4) 0.6346(4) 0.0327(16) Uani 1 1 d . . . H11 H 0.7262 0.6404 0.6833 0.049 Uiso 1 1 calc R . . H12 H 0.6415 0.6671 0.6329 0.049 Uiso 1 1 calc R . . H13 H 0.7801 0.6882 0.5987 0.049 Uiso 1 1 calc R . . C22 C 0.7391(6) 0.5243(5) 0.5204(3) 0.0308(15) Uani 1 1 d . . . H14 H 0.7537 0.4582 0.5084 0.046 Uiso 1 1 calc R . . H15 H 0.7985 0.5697 0.4851 0.046 Uiso 1 1 calc R . . H16 H 0.6598 0.5489 0.5189 0.046 Uiso 1 1 calc R . . C23 C 0.3904(5) 0.3463(5) 0.7620(3) 0.0251(14) Uani 1 1 d . . . H17 H 0.3989 0.3565 0.8075 0.038 Uiso 1 1 calc R . . H18 H 0.4165 0.2785 0.7559 0.038 Uiso 1 1 calc R . . H19 H 0.3071 0.3566 0.7636 0.038 Uiso 1 1 calc R . . C24 C 0.4247(6) 0.5654(5) 0.6921(4) 0.0407(19) Uani 1 1 d . . . H20 H 0.4346 0.5810 0.7357 0.061 Uiso 1 1 calc R . . H21 H 0.3404 0.5700 0.6958 0.061 Uiso 1 1 calc R . . H22 H 0.4685 0.6126 0.6491 0.061 Uiso 1 1 calc R . . C25 C 0.4613(5) 0.4108(5) 0.5998(3) 0.0285(15) Uani 1 1 d . . . H23 H 0.4916 0.3438 0.5938 0.043 Uiso 1 1 calc R . . H24 H 0.5043 0.4592 0.5573 0.043 Uiso 1 1 calc R . . H25 H 0.3767 0.4160 0.6044 0.043 Uiso 1 1 calc R . . C26 C 0.7548(5) 0.1044(4) 0.5989(3) 0.0163(12) Uani 1 1 d . . . H26 H 0.8158 0.0513 0.6057 0.020 Uiso 1 1 calc R . . Si3 Si 0.81467(15) 0.16571(13) 0.49942(9) 0.0222(4) Uani 1 1 d . . . Si4 Si 0.61288(15) 0.03392(12) 0.62849(10) 0.0240(4) Uani 1 1 d . . . C27 C 0.9341(5) 0.2516(5) 0.4885(3) 0.0303(15) Uani 1 1 d . . . H27 H 0.9008 0.3033 0.5168 0.045 Uiso 1 1 calc R . . H28 H 0.9671 0.2824 0.4371 0.045 Uiso 1 1 calc R . . H29 H 0.9969 0.2142 0.5060 0.045 Uiso 1 1 calc R . . C28 C 0.6978(6) 0.2360(5) 0.4617(4) 0.0347(16) Uani 1 1 d . . . H30 H 0.6614 0.2878 0.4892 0.052 Uiso 1 1 calc R . . H31 H 0.6369 0.1903 0.4657 0.052 Uiso 1 1 calc R . . H32 H 0.7340 0.2665 0.4105 0.052 Uiso 1 1 calc R . . C29 C 0.8806(7) 0.0683(5) 0.4453(4) 0.0431(19) Uani 1 1 d . . . H33 H 0.9112 0.0995 0.3937 0.065 Uiso 1 1 calc R . . H34 H 0.8198 0.0212 0.4519 0.065 Uiso 1 1 calc R . . H35 H 0.9456 0.0331 0.4618 0.065 Uiso 1 1 calc R . . C30 C 0.5932(6) -0.0443(6) 0.7210(4) 0.0420(18) Uani 1 1 d . . . H36 H 0.6628 -0.0886 0.7203 0.063 Uiso 1 1 calc R . . H37 H 0.5223 -0.0839 0.7355 0.063 Uiso 1 1 calc R . . H38 H 0.5841 -0.0015 0.7559 0.063 Uiso 1 1 calc R . . C31 C 0.4781(5) 0.1175(5) 0.6327(4) 0.0385(18) Uani 1 1 d . . . H39 H 0.4863 0.1595 0.5847 0.058 Uiso 1 1 calc R . . H40 H 0.4699 0.1595 0.6680 0.058 Uiso 1 1 calc R . . H41 H 0.4076 0.0773 0.6477 0.058 Uiso 1 1 calc R . . C32 C 0.6191(6) -0.0504(5) 0.5653(4) 0.0400(18) Uani 1 1 d . . . H42 H 0.6888 -0.0951 0.5623 0.060 Uiso 1 1 calc R . . H43 H 0.6244 -0.0108 0.5169 0.060 Uiso 1 1 calc R . . H44 H 0.5472 -0.0895 0.5837 0.060 Uiso 1 1 calc R . . C33 C 0.9051(4) 0.1572(4) 0.7976(3) 0.0106(11) Uani 1 1 d . . . H45 H 0.8844 0.1966 0.8367 0.013 Uiso 1 1 calc R . . Si5 Si 1.06731(13) 0.18446(11) 0.74173(9) 0.0161(3) Uani 1 1 d . . . Si6 Si 0.88658(13) 0.02161(11) 0.84542(9) 0.0175(4) Uani 1 1 d . . . C34 C 1.0921(5) 0.3189(4) 0.7179(4) 0.0234(14) Uani 1 1 d . . . H46 H 1.0689 0.3458 0.7624 0.035 Uiso 1 1 calc R . . H47 H 1.0443 0.3516 0.6867 0.035 Uiso 1 1 calc R . . H48 H 1.1762 0.3309 0.6919 0.035 Uiso 1 1 calc R . . C35 C 1.1137(5) 0.1396(5) 0.6547(3) 0.0291(15) Uani 1 1 d . . . H49 H 1.1025 0.0679 0.6648 0.044 Uiso 1 1 calc R . . H50 H 1.1975 0.1536 0.6292 0.044 Uiso 1 1 calc R . . H51 H 1.0656 0.1736 0.6241 0.044 Uiso 1 1 calc R . . C36 C 1.1675(5) 0.1276(5) 0.7974(4) 0.0275(15) Uani 1 1 d . . . H52 H 1.1577 0.0556 0.8112 0.041 Uiso 1 1 calc R . . H53 H 1.1469 0.1556 0.8413 0.041 Uiso 1 1 calc R . . H54 H 1.2500 0.1419 0.7687 0.041 Uiso 1 1 calc R . . C37 C 0.9209(6) 0.0034(5) 0.9330(4) 0.0332(16) Uani 1 1 d . . . H55 H 1.0016 0.0247 0.9235 0.050 Uiso 1 1 calc R . . H56 H 0.9147 -0.0669 0.9566 0.050 Uiso 1 1 calc R . . H57 H 0.8645 0.0428 0.9650 0.050 Uiso 1 1 calc R . . C38 C 0.7331(5) -0.0204(4) 0.8701(4) 0.0299(15) Uani 1 1 d . . . H58 H 0.7097 -0.0124 0.8261 0.045 Uiso 1 1 calc R . . H59 H 0.6793 0.0194 0.9030 0.045 Uiso 1 1 calc R . . H60 H 0.7291 -0.0904 0.8945 0.045 Uiso 1 1 calc R . . C39 C 0.9832(6) -0.0653(4) 0.7903(4) 0.0320(16) Uani 1 1 d . . . H61 H 0.9662 -0.0565 0.7441 0.048 Uiso 1 1 calc R . . H62 H 0.9676 -0.1337 0.8171 0.048 Uiso 1 1 calc R . . H63 H 1.0665 -0.0513 0.7809 0.048 Uiso 1 1 calc R . . C40 C 0.7001(5) 0.2631(4) 0.9306(3) 0.0151(12) Uani 1 1 d . . . C41 C 0.5927(5) 0.2106(4) 0.9539(3) 0.0181(12) Uani 1 1 d . . . C42 C 0.5659(5) 0.1423(4) 1.0187(3) 0.0229(13) Uani 1 1 d . . . H64 H 0.4968 0.1044 1.0327 0.028 Uiso 1 1 calc R . . C43 C 0.6363(5) 0.1272(4) 1.0638(3) 0.0270(14) Uani 1 1 d . . . H65 H 0.6161 0.0800 1.1083 0.032 Uiso 1 1 calc R . . C44 C 0.7380(5) 0.1831(4) 1.0423(3) 0.0262(14) Uani 1 1 d . . . H66 H 0.7850 0.1756 1.0739 0.031 Uiso 1 1 calc R . . C45 C 0.7722(5) 0.2488(4) 0.9763(3) 0.0188(12) Uani 1 1 d . . . C46 C 0.5019(5) 0.2315(4) 0.9122(3) 0.0185(12) Uani 1 1 d . . . H67 H 0.5318 0.2868 0.8696 0.022 Uiso 1 1 calc R . . C47 C 0.4829(6) 0.1429(5) 0.8832(4) 0.0355(17) Uani 1 1 d . . . H68 H 0.4240 0.1611 0.8573 0.053 Uiso 1 1 calc R . . H69 H 0.4546 0.0871 0.9239 0.053 Uiso 1 1 calc R . . H70 H 0.5580 0.1237 0.8499 0.053 Uiso 1 1 calc R . . C48 C 0.3830(5) 0.2671(5) 0.9613(4) 0.0357(17) Uani 1 1 d . . . H71 H 0.3965 0.3238 0.9796 0.054 Uiso 1 1 calc R . . H72 H 0.3496 0.2130 1.0023 0.054 Uiso 1 1 calc R . . H73 H 0.3275 0.2871 0.9330 0.054 Uiso 1 1 calc R . . C49 C 0.8843(5) 0.3071(4) 0.9581(3) 0.0224(13) Uani 1 1 d . . . H74 H 0.9113 0.3331 0.9044 0.027 Uiso 1 1 calc R . . C50 C 0.9862(5) 0.2435(5) 0.9782(4) 0.0319(16) Uani 1 1 d . . . H75 H 1.0042 0.1873 0.9534 0.048 Uiso 1 1 calc R . . H76 H 0.9630 0.2187 1.0309 0.048 Uiso 1 1 calc R . . H77 H 1.0567 0.2838 0.9631 0.048 Uiso 1 1 calc R . . C51 C 0.8559(6) 0.3960(5) 0.9955(4) 0.0323(16) Uani 1 1 d . . . H78 H 0.9280 0.4334 0.9832 0.048 Uiso 1 1 calc R . . H79 H 0.8260 0.3726 1.0482 0.048 Uiso 1 1 calc R . . H80 H 0.7956 0.4390 0.9788 0.048 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 Ge1 0.0109(3) 0.0109(3) 0.0110(3) -0.0030(2) -0.0034(2) 0.0004(2) C1 0.021(3) 0.018(3) 0.012(3) -0.006(2) -0.005(2) -0.001(2) C2 0.015(3) 0.022(3) 0.022(3) -0.011(3) -0.004(2) 0.002(2) C3 0.018(3) 0.026(3) 0.033(4) -0.008(3) -0.008(3) 0.009(3) C4 0.026(3) 0.019(3) 0.036(4) -0.017(3) -0.008(3) 0.012(3) C5 0.028(3) 0.021(3) 0.028(4) -0.008(3) -0.010(3) -0.001(3) C6 0.020(3) 0.017(3) 0.014(3) -0.003(2) -0.005(2) 0.002(2) C7 0.020(3) 0.015(3) 0.010(3) -0.003(2) -0.006(2) 0.001(2) O1 0.0163(19) 0.0132(19) 0.018(2) -0.0070(16) -0.0023(16) -0.0028(15) Mo1 0.0153(3) 0.0167(3) 0.0248(3) -0.0108(2) -0.0031(2) -0.0029(2) C8 0.024(3) 0.026(4) 0.053(5) -0.018(3) -0.015(3) 0.003(3) O2 0.023(3) 0.037(3) 0.112(5) -0.034(3) -0.012(3) -0.009(2) C9 0.019(3) 0.026(3) 0.026(4) -0.012(3) -0.001(3) -0.001(3) O3 0.037(3) 0.043(3) 0.038(3) -0.007(2) -0.011(2) 0.011(2) C10 0.020(3) 0.029(3) 0.039(4) -0.017(3) -0.015(3) -0.001(3) O4 0.030(3) 0.081(4) 0.047(3) -0.048(3) -0.012(2) 0.004(3) C11 0.029(4) 0.021(3) 0.037(4) -0.004(3) -0.012(3) -0.002(3) O5 0.035(3) 0.029(3) 0.045(3) -0.005(2) -0.014(2) 0.002(2) C12 0.024(3) 0.015(3) 0.032(4) -0.001(3) -0.014(3) -0.004(2) O6 0.031(2) 0.032(3) 0.021(2) -0.009(2) -0.003(2) -0.005(2) C13 0.009(3) 0.012(3) 0.017(3) -0.004(2) -0.007(2) 0.000(2) C14 0.010(3) 0.014(3) 0.010(3) 0.000(2) -0.005(2) -0.005(2) C15 0.017(3) 0.019(3) 0.014(3) -0.001(2) -0.008(2) -0.004(2) C16 0.009(3) 0.011(3) 0.013(3) -0.006(2) 0.001(2) -0.003(2) C17 0.008(3) 0.013(3) 0.017(3) -0.005(2) -0.003(2) 0.000(2) C18 0.010(3) 0.014(3) 0.010(3) 0.000(2) -0.002(2) -0.004(2) C19 0.017(3) 0.013(3) 0.016(3) -0.004(2) -0.006(2) -0.002(2) Si1 0.0178(8) 0.0169(8) 0.0150(8) -0.0005(6) -0.0078(7) -0.0019(6) Si2 0.0153(8) 0.0208(8) 0.0240(9) -0.0042(7) -0.0112(7) 0.0026(7) C20 0.018(3) 0.034(4) 0.019(3) 0.001(3) -0.005(3) -0.012(3) C21 0.039(4) 0.019(3) 0.042(4) -0.006(3) -0.013(3) -0.006(3) C22 0.033(4) 0.042(4) 0.018(3) 0.000(3) -0.011(3) -0.008(3) C23 0.019(3) 0.037(4) 0.020(3) -0.007(3) -0.005(3) -0.003(3) C24 0.034(4) 0.032(4) 0.067(6) -0.016(4) -0.032(4) 0.012(3) C25 0.026(3) 0.042(4) 0.022(3) 0.001(3) -0.017(3) -0.007(3) C26 0.022(3) 0.018(3) 0.013(3) -0.008(2) -0.007(2) 0.000(2) Si3 0.0285(9) 0.0255(9) 0.0159(9) -0.0094(7) -0.0065(7) -0.0053(7) Si4 0.0274(9) 0.0224(9) 0.0263(10) -0.0064(7) -0.0100(8) -0.0105(7) C27 0.028(3) 0.042(4) 0.019(3) -0.007(3) -0.003(3) -0.008(3) C28 0.044(4) 0.038(4) 0.026(4) -0.002(3) -0.015(3) -0.011(3) C29 0.054(5) 0.044(4) 0.029(4) -0.018(3) 0.000(3) -0.006(4) C30 0.048(4) 0.050(5) 0.028(4) 0.001(3) -0.008(3) -0.029(4) C31 0.022(3) 0.042(4) 0.057(5) -0.020(4) -0.013(3) -0.001(3) C32 0.045(4) 0.043(4) 0.040(4) -0.021(4) -0.012(4) -0.018(3) C33 0.010(3) 0.010(3) 0.014(3) -0.005(2) -0.007(2) 0.003(2) Si5 0.0134(8) 0.0157(8) 0.0222(9) -0.0077(7) -0.0074(7) 0.0016(6) Si6 0.0207(8) 0.0125(8) 0.0207(9) -0.0017(7) -0.0099(7) 0.0013(6) C34 0.012(3) 0.018(3) 0.037(4) 0.002(3) -0.006(3) -0.003(2) C35 0.020(3) 0.042(4) 0.025(4) -0.013(3) 0.000(3) -0.005(3) C36 0.022(3) 0.027(3) 0.036(4) -0.006(3) -0.014(3) 0.005(3) C37 0.051(4) 0.022(3) 0.030(4) 0.003(3) -0.024(3) 0.004(3) C38 0.033(4) 0.019(3) 0.034(4) 0.003(3) -0.010(3) -0.006(3) C39 0.036(4) 0.010(3) 0.049(4) -0.006(3) -0.013(3) 0.002(3) C40 0.022(3) 0.012(3) 0.010(3) -0.001(2) -0.004(2) -0.001(2) C41 0.020(3) 0.015(3) 0.017(3) -0.003(2) -0.004(2) 0.001(2) C42 0.023(3) 0.020(3) 0.021(3) -0.003(3) -0.001(3) -0.004(2) C43 0.040(4) 0.020(3) 0.020(3) 0.000(3) -0.010(3) -0.003(3) C44 0.033(4) 0.024(3) 0.021(3) -0.002(3) -0.009(3) 0.003(3) C45 0.021(3) 0.019(3) 0.015(3) -0.004(2) -0.002(2) -0.001(2) C46 0.013(3) 0.024(3) 0.015(3) 0.001(2) 0.000(2) -0.009(2) C47 0.039(4) 0.026(4) 0.049(5) 0.002(3) -0.027(4) -0.012(3) C48 0.021(3) 0.048(4) 0.025(4) 0.006(3) 0.001(3) 0.003(3) C49 0.025(3) 0.021(3) 0.023(3) -0.001(3) -0.012(3) -0.001(3) C50 0.032(4) 0.028(4) 0.043(4) -0.004(3) -0.024(3) 0.002(3) C51 0.034(4) 0.025(3) 0.040(4) -0.008(3) -0.011(3) -0.006(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 Ge1 O1 1.898(4) . ? Ge1 C1 1.930(5) . ? Ge1 C13 1.963(5) . ? Ge1 C40 1.979(5) . ? C1 C2 1.403(7) . ? C1 C6 1.407(8) . ? C2 C3 1.402(8) . ? C3 C4 1.396(8) . ? C4 C5 1.382(8) . ? C5 C6 1.402(8) . ? C6 C7 1.494(7) . ? C7 O1 1.298(6) . ? C7 Mo1 2.194(5) . ? Mo1 C9 2.026(7) . ? Mo1 C8 2.036(6) . ? Mo1 C10 2.041(7) . ? Mo1 C11 2.045(7) . ? Mo1 C12 2.061(7) . ? C8 O2 1.141(7) . ? C9 O3 1.155(7) . ? C10 O4 1.140(7) . ? C11 O5 1.151(7) . ? C12 O6 1.134(7) . ? C13 C18 1.418(7) . ? C13 C14 1.423(7) . ? C14 C15 1.400(7) . ? C14 C19 1.526(7) . ? C15 C16 1.386(7) . ? C16 C17 1.397(7) . ? C16 C26 1.526(7) . ? C17 C18 1.391(7) . ? C18 C33 1.550(7) . ? C19 Si2 1.897(5) . ? C19 Si1 1.913(5) . ? Si1 C21 1.858(6) . ? Si1 C22 1.861(6) . ? Si1 C20 1.863(6) . ? Si2 C23 1.871(6) . ? Si2 C24 1.870(7) . ? Si2 C25 1.878(6) . ? C26 Si4 1.893(6) . ? C26 Si3 1.896(6) . ? Si3 C29 1.864(7) . ? Si3 C27 1.870(6) . ? Si3 C28 1.878(7) . ? Si4 C30 1.867(7) . ? Si4 C32 1.870(6) . ? Si4 C31 1.876(6) . ? C33 Si6 1.903(5) . ? C33 Si5 1.921(5) . ? Si5 C34 1.843(6) . ? Si5 C35 1.861(6) . ? Si5 C36 1.880(6) . ? Si6 C38 1.851(6) . ? Si6 C39 1.862(6) . ? Si6 C37 1.867(6) . ? C40 C45 1.407(8) . ? C40 C41 1.425(8) . ? C41 C42 1.380(8) . ? C41 C46 1.530(8) . ? C42 C43 1.381(8) . ? C43 C44 1.397(9) . ? C44 C45 1.381(8) . ? C45 C49 1.529(8) . ? C46 C47 1.525(8) . ? C46 C48 1.546(8) . ? C49 C51 1.528(8) . ? C49 C50 1.534(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 C1 85.33(19) . . ? O1 Ge1 C13 105.89(18) . . ? C1 Ge1 C13 124.8(2) . . ? O1 Ge1 C40 112.8(2) . . ? C1 Ge1 C40 108.9(2) . . ? C13 Ge1 C40 114.9(2) . . ? C2 C1 C6 119.6(5) . . ? C2 C1 Ge1 131.2(4) . . ? C6 C1 Ge1 108.9(4) . . ? C3 C2 C1 120.1(5) . . ? C4 C3 C2 119.8(5) . . ? C5 C4 C3 120.4(5) . . ? C4 C5 C6 120.5(5) . . ? C5 C6 C1 119.6(5) . . ? C5 C6 C7 123.5(5) . . ? C1 C6 C7 116.9(5) . . ? O1 C7 C6 110.9(5) . . ? O1 C7 Mo1 120.7(4) . . ? C6 C7 Mo1 128.3(4) . . ? C7 O1 Ge1 117.9(3) . . ? C9 Mo1 C8 87.3(3) . . ? C9 Mo1 C10 90.4(2) . . ? C8 Mo1 C10 90.0(3) . . ? C9 Mo1 C11 176.8(2) . . ? C8 Mo1 C11 91.0(3) . . ? C10 Mo1 C11 92.3(3) . . ? C9 Mo1 C12 87.8(2) . . ? C8 Mo1 C12 89.8(2) . . ? C10 Mo1 C12 178.2(2) . . ? C11 Mo1 C12 89.5(2) . . ? C9 Mo1 C7 91.7(2) . . ? C8 Mo1 C7 175.5(2) . . ? C10 Mo1 C7 85.6(2) . . ? C11 Mo1 C7 90.2(2) . . ? C12 Mo1 C7 94.6(2) . . ? O2 C8 Mo1 178.1(7) . . ? O3 C9 Mo1 175.6(5) . . ? O4 C10 Mo1 177.7(6) . . ? O5 C11 Mo1 177.1(6) . . ? O6 C12 Mo1 176.4(5) . . ? C18 C13 C14 119.1(5) . . ? C18 C13 Ge1 119.3(4) . . ? C14 C13 Ge1 121.4(4) . . ? C15 C14 C13 118.4(5) . . ? C15 C14 C19 118.1(5) . . ? C13 C14 C19 123.4(5) . . ? C16 C15 C14 123.4(5) . . ? C15 C16 C17 116.6(5) . . ? C15 C16 C26 122.9(5) . . ? C17 C16 C26 120.4(5) . . ? C18 C17 C16 123.1(5) . . ? C17 C18 C13 118.9(5) . . ? C17 C18 C33 116.4(4) . . ? C13 C18 C33 124.6(5) . . ? C14 C19 Si2 116.9(3) . . ? C14 C19 Si1 111.1(3) . . ? Si2 C19 Si1 115.4(3) . . ? C21 Si1 C22 108.5(3) . . ? C21 Si1 C20 108.3(3) . . ? C22 Si1 C20 108.1(3) . . ? C21 Si1 C19 109.2(3) . . ? C22 Si1 C19 114.0(3) . . ? C20 Si1 C19 108.6(3) . . ? C23 Si2 C24 109.1(3) . . ? C23 Si2 C25 106.2(3) . . ? C24 Si2 C25 107.5(3) . . ? C23 Si2 C19 109.3(3) . . ? C24 Si2 C19 108.0(3) . . ? C25 Si2 C19 116.6(3) . . ? C16 C26 Si4 112.7(4) . . ? C16 C26 Si3 113.8(4) . . ? Si4 C26 Si3 117.5(3) . . ? C29 Si3 C27 108.5(3) . . ? C29 Si3 C28 107.7(3) . . ? C27 Si3 C28 109.6(3) . . ? C29 Si3 C26 109.0(3) . . ? C27 Si3 C26 108.8(3) . . ? C28 Si3 C26 113.2(3) . . ? C30 Si4 C32 107.8(3) . . ? C30 Si4 C31 107.9(4) . . ? C32 Si4 C31 107.9(3) . . ? C30 Si4 C26 109.1(3) . . ? C32 Si4 C26 111.0(3) . . ? C31 Si4 C26 113.0(3) . . ? C18 C33 Si6 115.3(3) . . ? C18 C33 Si5 110.4(3) . . ? Si6 C33 Si5 111.5(2) . . ? C34 Si5 C35 106.7(3) . . ? C34 Si5 C36 106.4(3) . . ? C35 Si5 C36 109.8(3) . . ? C34 Si5 C33 110.9(2) . . ? C35 Si5 C33 113.0(3) . . ? C36 Si5 C33 109.9(3) . . ? C38 Si6 C39 106.2(3) . . ? C38 Si6 C37 105.6(3) . . ? C39 Si6 C37 108.5(3) . . ? C38 Si6 C33 113.2(2) . . ? C39 Si6 C33 113.4(3) . . ? C37 Si6 C33 109.6(3) . . ? C45 C40 C41 119.3(5) . . ? C45 C40 Ge1 125.9(4) . . ? C41 C40 Ge1 114.7(4) . . ? C42 C41 C40 118.9(5) . . ? C42 C41 C46 118.4(5) . . ? C40 C41 C46 122.6(5) . . ? C41 C42 C43 122.2(6) . . ? C42 C43 C44 118.3(6) . . ? C45 C44 C43 121.9(6) . . ? C44 C45 C40 119.2(5) . . ? C44 C45 C49 117.9(5) . . ? C40 C45 C49 122.8(5) . . ? C47 C46 C41 113.5(5) . . ? C47 C46 C48 110.3(5) . . ? C41 C46 C48 109.5(5) . . ? C45 C49 C51 109.8(5) . . ? C45 C49 C50 113.1(5) . . ? C51 C49 C50 110.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ge1 C1 C2 -177.1(6) . . . . ? C13 Ge1 C1 C2 76.8(6) . . . . ? C40 Ge1 C1 C2 -64.5(6) . . . . ? O1 Ge1 C1 C6 -2.1(4) . . . . ? C13 Ge1 C1 C6 -108.3(4) . . . . ? C40 Ge1 C1 C6 110.4(4) . . . . ? C6 C1 C2 C3 1.5(9) . . . . ? Ge1 C1 C2 C3 176.0(5) . . . . ? C1 C2 C3 C4 -0.9(9) . . . . ? C2 C3 C4 C5 -0.3(10) . . . . ? C3 C4 C5 C6 0.7(10) . . . . ? C4 C5 C6 C1 -0.1(9) . . . . ? C4 C5 C6 C7 -179.7(6) . . . . ? C2 C1 C6 C5 -1.1(8) . . . . ? Ge1 C1 C6 C5 -176.7(4) . . . . ? C2 C1 C6 C7 178.6(5) . . . . ? Ge1 C1 C6 C7 3.0(6) . . . . ? C5 C6 C7 O1 177.4(5) . . . . ? C1 C6 C7 O1 -2.3(7) . . . . ? C5 C6 C7 Mo1 -0.2(8) . . . . ? C1 C6 C7 Mo1 -179.9(4) . . . . ? C6 C7 O1 Ge1 0.4(6) . . . . ? Mo1 C7 O1 Ge1 178.2(2) . . . . ? C1 Ge1 O1 C7 1.0(4) . . . . ? C13 Ge1 O1 C7 125.9(4) . . . . ? C40 Ge1 O1 C7 -107.6(4) . . . . ? O1 C7 Mo1 C9 -37.8(4) . . . . ? C6 C7 Mo1 C9 139.6(5) . . . . ? O1 C7 Mo1 C8 -115(3) . . . . ? C6 C7 Mo1 C8 62(3) . . . . ? O1 C7 Mo1 C10 -128.1(5) . . . . ? C6 C7 Mo1 C10 49.3(5) . . . . ? O1 C7 Mo1 C11 139.7(4) . . . . ? C6 C7 Mo1 C11 -42.9(5) . . . . ? O1 C7 Mo1 C12 50.2(4) . . . . ? C6 C7 Mo1 C12 -132.5(5) . . . . ? C9 Mo1 C8 O2 -81(19) . . . . ? C10 Mo1 C8 O2 10(19) . . . . ? C11 Mo1 C8 O2 102(19) . . . . ? C12 Mo1 C8 O2 -168(19) . . . . ? C7 Mo1 C8 O2 -3(21) . . . . ? C8 Mo1 C9 O3 -11(7) . . . . ? C10 Mo1 C9 O3 -101(7) . . . . ? C11 Mo1 C9 O3 47(10) . . . . ? C12 Mo1 C9 O3 79(7) . . . . ? C7 Mo1 C9 O3 173(7) . . . . ? C9 Mo1 C10 O4 -53(14) . . . . ? C8 Mo1 C10 O4 -140(14) . . . . ? C11 Mo1 C10 O4 129(14) . . . . ? C12 Mo1 C10 O4 -56(17) . . . . ? C7 Mo1 C10 O4 39(14) . . . . ? C9 Mo1 C11 O5 -1(14) . . . . ? C8 Mo1 C11 O5 56(11) . . . . ? C10 Mo1 C11 O5 146(11) . . . . ? C12 Mo1 C11 O5 -34(11) . . . . ? C7 Mo1 C11 O5 -128(11) . . . . ? C9 Mo1 C12 O6 -92(9) . . . . ? C8 Mo1 C12 O6 -5(9) . . . . ? C10 Mo1 C12 O6 -89(11) . . . . ? C11 Mo1 C12 O6 86(9) . . . . ? C7 Mo1 C12 O6 177(9) . . . . ? O1 Ge1 C13 C18 84.3(4) . . . . ? C1 Ge1 C13 C18 179.8(4) . . . . ? C40 Ge1 C13 C18 -40.9(5) . . . . ? O1 Ge1 C13 C14 -101.5(4) . . . . ? C1 Ge1 C13 C14 -6.0(5) . . . . ? C40 Ge1 C13 C14 133.3(4) . . . . ? C18 C13 C14 C15 6.6(7) . . . . ? Ge1 C13 C14 C15 -167.6(4) . . . . ? C18 C13 C14 C19 -168.9(4) . . . . ? Ge1 C13 C14 C19 16.9(7) . . . . ? C13 C14 C15 C16 -1.7(8) . . . . ? C19 C14 C15 C16 174.0(5) . . . . ? C14 C15 C16 C17 -3.5(8) . . . . ? C14 C15 C16 C26 178.9(5) . . . . ? C15 C16 C17 C18 4.0(8) . . . . ? C26 C16 C17 C18 -178.4(5) . . . . ? C16 C17 C18 C13 0.8(8) . . . . ? C16 C17 C18 C33 -175.8(5) . . . . ? C14 C13 C18 C17 -6.2(7) . . . . ? Ge1 C13 C18 C17 168.1(4) . . . . ? C14 C13 C18 C33 170.2(5) . . . . ? Ge1 C13 C18 C33 -15.5(7) . . . . ? C15 C14 C19 Si2 54.5(6) . . . . ? C13 C14 C19 Si2 -129.9(5) . . . . ? C15 C14 C19 Si1 -80.8(5) . . . . ? C13 C14 C19 Si1 94.7(5) . . . . ? C14 C19 Si1 C21 -148.2(4) . . . . ? Si2 C19 Si1 C21 75.7(4) . . . . ? C14 C19 Si1 C22 90.2(4) . . . . ? Si2 C19 Si1 C22 -45.9(4) . . . . ? C14 C19 Si1 C20 -30.3(5) . . . . ? Si2 C19 Si1 C20 -166.4(3) . . . . ? C14 C19 Si2 C23 48.3(5) . . . . ? Si1 C19 Si2 C23 -178.3(3) . . . . ? C14 C19 Si2 C24 166.8(4) . . . . ? Si1 C19 Si2 C24 -59.8(4) . . . . ? C14 C19 Si2 C25 -72.1(5) . . . . ? Si1 C19 Si2 C25 61.3(4) . . . . ? C15 C16 C26 Si4 -79.8(6) . . . . ? C17 C16 C26 Si4 102.8(5) . . . . ? C15 C16 C26 Si3 57.3(6) . . . . ? C17 C16 C26 Si3 -120.2(5) . . . . ? C16 C26 Si3 C29 151.1(4) . . . . ? Si4 C26 Si3 C29 -74.0(4) . . . . ? C16 C26 Si3 C27 33.0(5) . . . . ? Si4 C26 Si3 C27 167.9(3) . . . . ? C16 C26 Si3 C28 -89.1(4) . . . . ? Si4 C26 Si3 C28 45.8(4) . . . . ? C16 C26 Si4 C30 -58.6(5) . . . . ? Si3 C26 Si4 C30 166.1(3) . . . . ? C16 C26 Si4 C32 -177.3(4) . . . . ? Si3 C26 Si4 C32 47.4(4) . . . . ? C16 C26 Si4 C31 61.4(5) . . . . ? Si3 C26 Si4 C31 -73.9(4) . . . . ? C17 C18 C33 Si6 -51.2(6) . . . . ? C13 C18 C33 Si6 132.4(5) . . . . ? C17 C18 C33 Si5 76.3(5) . . . . ? C13 C18 C33 Si5 -100.1(5) . . . . ? C18 C33 Si5 C34 66.9(4) . . . . ? Si6 C33 Si5 C34 -163.6(3) . . . . ? C18 C33 Si5 C35 -52.8(4) . . . . ? Si6 C33 Si5 C35 76.7(4) . . . . ? C18 C33 Si5 C36 -175.8(4) . . . . ? Si6 C33 Si5 C36 -46.2(4) . . . . ? C18 C33 Si6 C38 -31.3(5) . . . . ? Si5 C33 Si6 C38 -158.2(3) . . . . ? C18 C33 Si6 C39 89.9(4) . . . . ? Si5 C33 Si6 C39 -37.1(4) . . . . ? C18 C33 Si6 C37 -148.8(4) . . . . ? Si5 C33 Si6 C37 84.2(3) . . . . ? O1 Ge1 C40 C45 -4.4(5) . . . . ? C1 Ge1 C40 C45 -97.3(5) . . . . ? C13 Ge1 C40 C45 117.1(5) . . . . ? O1 Ge1 C40 C41 174.7(4) . . . . ? C1 Ge1 C40 C41 81.8(4) . . . . ? C13 Ge1 C40 C41 -63.7(4) . . . . ? C45 C40 C41 C42 -4.0(8) . . . . ? Ge1 C40 C41 C42 176.8(4) . . . . ? C45 C40 C41 C46 172.0(5) . . . . ? Ge1 C40 C41 C46 -7.2(7) . . . . ? C40 C41 C42 C43 3.7(9) . . . . ? C46 C41 C42 C43 -172.5(5) . . . . ? C41 C42 C43 C44 -0.3(9) . . . . ? C42 C43 C44 C45 -3.0(9) . . . . ? C43 C44 C45 C40 2.6(9) . . . . ? C43 C44 C45 C49 179.5(5) . . . . ? C41 C40 C45 C44 0.9(8) . . . . ? Ge1 C40 C45 C44 -180.0(4) . . . . ? C41 C40 C45 C49 -175.8(5) . . . . ? Ge1 C40 C45 C49 3.3(8) . . . . ? C42 C41 C46 C47 -66.1(7) . . . . ? C40 C41 C46 C47 117.8(6) . . . . ? C42 C41 C46 C48 57.7(7) . . . . ? C40 C41 C46 C48 -118.4(6) . . . . ? C44 C45 C49 C51 -81.1(7) . . . . ? C40 C45 C49 C51 95.7(7) . . . . ? C44 C45 C49 C50 42.7(7) . . . . ? C40 C45 C49 C50 -140.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.724 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.091 #--------------------------------------------------------- data_w(co)6 _database_code_depnum_ccdc_archive 'CCDC 224030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'W complex' _chemical_melting_point ? _chemical_formula_moiety 'C51 H80 Ge O6 Si6 W' _chemical_formula_sum 'C51 H80 Ge O6 Si6 W' _chemical_formula_weight 1214.13 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' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 '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 11.907(3) _cell_length_b 13.800(4) _cell_length_c 19.771(5) _cell_angle_alpha 77.242(8) _cell_angle_beta 71.489(7) _cell_angle_gamma 84.456(9) _cell_volume 3003.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisum _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 2.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5121 _exptl_absorpt_correction_T_max 0.6269 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 Meacury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19763 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10352 _reflns_number_gt 9542 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.0991P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10352 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Ge1 Ge 0.26802(4) 1.14663(3) 0.16599(2) 0.01059(10) Uani 1 1 d . . . C1 C 0.3573(4) 1.0230(3) 0.1537(2) 0.0184(9) Uani 1 1 d . . . C2 C 0.4788(4) 1.0021(3) 0.1318(2) 0.0196(9) Uani 1 1 d . . . H1 H 0.5333 1.0529 0.1225 0.024 Uiso 1 1 calc R . . C3 C 0.5195(4) 0.9067(4) 0.1235(3) 0.0309(12) Uani 1 1 d . . . H2 H 0.6023 0.8922 0.1088 0.037 Uiso 1 1 calc R . . C4 C 0.4407(5) 0.8322(4) 0.1367(3) 0.0327(12) Uani 1 1 d . . . H3 H 0.4697 0.7669 0.1310 0.039 Uiso 1 1 calc R . . C5 C 0.3202(4) 0.8524(4) 0.1579(3) 0.0262(11) Uani 1 1 d . . . H4 H 0.2666 0.8011 0.1665 0.031 Uiso 1 1 calc R . . C6 C 0.2769(4) 0.9475(3) 0.1668(2) 0.0197(9) Uani 1 1 d . . . C7 C 0.1475(4) 0.9770(3) 0.1887(2) 0.0194(9) Uani 1 1 d . . . O1 O 0.1314(3) 1.0707(2) 0.18973(16) 0.0183(6) Uani 1 1 d . . . W1 W -0.004179(17) 0.883172(14) 0.211993(11) 0.02354(7) Uani 1 1 d . . . C8 C -0.1388(4) 0.7940(4) 0.2260(3) 0.0324(12) Uani 1 1 d . . . O2 O -0.2135(3) 0.7437(3) 0.2316(3) 0.0561(13) Uani 1 1 d . . . C9 C 0.0844(4) 0.8398(4) 0.1166(3) 0.0312(12) Uani 1 1 d . . . O3 O 0.1349(3) 0.8174(4) 0.0629(2) 0.0509(12) Uani 1 1 d . . . C10 C 0.0738(5) 0.7710(4) 0.2706(3) 0.0295(11) Uani 1 1 d . . . O4 O 0.1132(4) 0.7081(3) 0.3043(2) 0.0411(9) Uani 1 1 d . . . C11 C -0.0957(4) 0.9290(3) 0.3069(3) 0.0231(10) Uani 1 1 d . . . O5 O -0.1521(3) 0.9520(2) 0.35953(18) 0.0271(7) Uani 1 1 d . . . C12 C -0.0896(4) 0.9932(4) 0.1602(3) 0.0280(11) Uani 1 1 d . . . O6 O -0.1427(4) 1.0530(3) 0.1321(2) 0.0470(10) Uani 1 1 d . . . C13 C 0.2452(3) 1.2132(3) 0.2472(2) 0.0101(8) Uani 1 1 d . . . C14 C 0.3026(3) 1.1769(3) 0.3014(2) 0.0112(8) Uani 1 1 d . . . C15 C 0.3016(4) 1.2371(3) 0.3498(2) 0.0138(8) Uani 1 1 d . . . H5 H 0.3424 1.2138 0.3848 0.017 Uiso 1 1 calc R . . C16 C 0.2437(4) 1.3292(3) 0.3493(2) 0.0143(9) Uani 1 1 d . . . C17 C 0.1798(3) 1.3593(3) 0.2997(2) 0.0121(8) Uani 1 1 d . . . H6 H 0.1362 1.4206 0.3001 0.015 Uiso 1 1 calc R . . C18 C 0.1770(3) 1.3035(3) 0.2493(2) 0.0121(8) Uani 1 1 d . . . C19 C 0.3578(4) 1.0726(3) 0.3126(2) 0.0138(8) Uani 1 1 d . . . H7 H 0.3643 1.0495 0.2669 0.017 Uiso 1 1 calc R . . Si1 Si 0.25064(11) 0.98322(9) 0.38687(7) 0.0168(3) Uani 1 1 d . . . Si2 Si 0.51643(11) 1.06280(9) 0.31646(7) 0.0202(3) Uani 1 1 d . . . C20 C 0.0965(4) 1.0230(4) 0.3873(3) 0.0240(10) Uani 1 1 d . . . H8 H 0.0794 1.0898 0.3983 0.036 Uiso 1 1 calc R . . H9 H 0.0407 0.9763 0.4245 0.036 Uiso 1 1 calc R . . H10 H 0.0882 1.0239 0.3394 0.036 Uiso 1 1 calc R . . C21 C 0.2798(5) 0.8555(4) 0.3661(3) 0.0341(12) Uani 1 1 d . . . H11 H 0.3607 0.8332 0.3656 0.051 Uiso 1 1 calc R . . H12 H 0.2708 0.8570 0.3183 0.051 Uiso 1 1 calc R . . H13 H 0.2233 0.8096 0.4034 0.051 Uiso 1 1 calc R . . C22 C 0.2601(5) 0.9759(4) 0.4802(3) 0.0305(12) Uani 1 1 d . . . H14 H 0.3406 0.9549 0.4813 0.046 Uiso 1 1 calc R . . H15 H 0.2037 0.9277 0.5151 0.046 Uiso 1 1 calc R . . H16 H 0.2410 1.0414 0.4932 0.046 Uiso 1 1 calc R . . C23 C 0.6084(4) 1.1536(4) 0.2390(3) 0.0299(12) Uani 1 1 d . . . H17 H 0.6001 1.1438 0.1933 0.045 Uiso 1 1 calc R . . H18 H 0.6917 1.1435 0.2376 0.045 Uiso 1 1 calc R . . H19 H 0.5820 1.2214 0.2455 0.045 Uiso 1 1 calc R . . C24 C 0.5758(5) 0.9348(4) 0.3076(4) 0.0409(14) Uani 1 1 d . . . H20 H 0.5656 0.9193 0.2639 0.061 Uiso 1 1 calc R . . H21 H 0.5328 0.8871 0.3506 0.061 Uiso 1 1 calc R . . H22 H 0.6602 0.9307 0.3036 0.061 Uiso 1 1 calc R . . C25 C 0.5382(4) 1.0884(4) 0.4004(3) 0.0307(12) Uani 1 1 d . . . H23 H 0.4915 1.0423 0.4431 0.046 Uiso 1 1 calc R . . H24 H 0.5121 1.1568 0.4049 0.046 Uiso 1 1 calc R . . H25 H 0.6222 1.0793 0.3971 0.046 Uiso 1 1 calc R . . C26 C 0.2438(4) 1.3955(3) 0.4012(2) 0.0171(9) Uani 1 1 d . . . H26 H 0.1829 1.4487 0.3941 0.021 Uiso 1 1 calc R . . Si3 Si 0.38652(12) 1.46580(10) 0.37225(7) 0.0246(3) Uani 1 1 d . . . Si4 Si 0.18460(12) 1.33385(10) 0.50097(7) 0.0229(3) Uani 1 1 d . . . C27 C 0.4064(6) 1.5442(5) 0.2795(3) 0.0477(16) Uani 1 1 d . . . H27 H 0.3374 1.5894 0.2803 0.072 Uiso 1 1 calc R . . H28 H 0.4142 1.5014 0.2446 0.072 Uiso 1 1 calc R . . H29 H 0.4780 1.5831 0.2648 0.072 Uiso 1 1 calc R . . C28 C 0.5199(5) 1.3825(4) 0.3676(3) 0.0410(14) Uani 1 1 d . . . H30 H 0.5119 1.3400 0.4156 0.062 Uiso 1 1 calc R . . H31 H 0.5905 1.4226 0.3527 0.062 Uiso 1 1 calc R . . H32 H 0.5277 1.3408 0.3320 0.062 Uiso 1 1 calc R . . C29 C 0.3789(5) 1.5511(4) 0.4353(3) 0.0415(14) Uani 1 1 d . . . H33 H 0.3089 1.5956 0.4379 0.062 Uiso 1 1 calc R . . H34 H 0.4504 1.5907 0.4170 0.062 Uiso 1 1 calc R . . H35 H 0.3734 1.5119 0.4840 0.062 Uiso 1 1 calc R . . C30 C 0.0649(5) 1.2491(4) 0.5116(3) 0.0308(12) Uani 1 1 d . . . H36 H 0.0043 1.2865 0.4917 0.046 Uiso 1 1 calc R . . H37 H 0.0290 1.2209 0.5634 0.046 Uiso 1 1 calc R . . H38 H 0.0984 1.1954 0.4854 0.046 Uiso 1 1 calc R . . C31 C 0.3007(5) 1.2638(4) 0.5389(3) 0.0368(13) Uani 1 1 d . . . H39 H 0.3632 1.3090 0.5332 0.055 Uiso 1 1 calc R . . H40 H 0.3348 1.2101 0.5127 0.055 Uiso 1 1 calc R . . H41 H 0.2651 1.2356 0.5907 0.055 Uiso 1 1 calc R . . C32 C 0.1179(6) 1.4310(4) 0.5556(3) 0.0455(15) Uani 1 1 d . . . H42 H 0.1791 1.4769 0.5508 0.068 Uiso 1 1 calc R . . H43 H 0.0844 1.3993 0.6069 0.068 Uiso 1 1 calc R . . H44 H 0.0550 1.4680 0.5376 0.068 Uiso 1 1 calc R . . C33 C 0.0950(3) 1.3430(3) 0.2031(2) 0.0118(8) Uani 1 1 d . . . H45 H 0.1157 1.3035 0.1639 0.014 Uiso 1 1 calc R . . Si5 Si -0.06703(10) 1.31603(9) 0.25791(7) 0.0169(3) Uani 1 1 d . . . Si6 Si 0.11360(11) 1.47869(9) 0.15470(7) 0.0189(3) Uani 1 1 d . . . C34 C -0.0920(4) 1.1807(3) 0.2824(3) 0.0251(11) Uani 1 1 d . . . H46 H -0.0684 1.1533 0.2380 0.038 Uiso 1 1 calc R . . H47 H -0.1762 1.1689 0.3081 0.038 Uiso 1 1 calc R . . H48 H -0.0447 1.1482 0.3140 0.038 Uiso 1 1 calc R . . C35 C -0.1138(4) 1.3613(4) 0.3452(3) 0.0324(12) Uani 1 1 d . . . H49 H -0.1021 1.4330 0.3351 0.049 Uiso 1 1 calc R . . H50 H -0.0662 1.3269 0.3762 0.049 Uiso 1 1 calc R . . H51 H -0.1978 1.3477 0.3704 0.049 Uiso 1 1 calc R . . C36 C -0.1672(4) 1.3721(4) 0.2022(3) 0.0320(12) Uani 1 1 d . . . H52 H -0.1570 1.4442 0.1877 0.048 Uiso 1 1 calc R . . H53 H -0.2497 1.3583 0.2312 0.048 Uiso 1 1 calc R . . H54 H -0.1471 1.3433 0.1586 0.048 Uiso 1 1 calc R . . C37 C 0.0797(5) 1.4982(4) 0.0669(3) 0.0368(13) Uani 1 1 d . . . H55 H -0.0012 1.4776 0.0761 0.055 Uiso 1 1 calc R . . H56 H 0.1357 1.4586 0.0348 0.055 Uiso 1 1 calc R . . H57 H 0.0866 1.5688 0.0435 0.055 Uiso 1 1 calc R . . C38 C 0.2679(5) 1.5203(4) 0.1302(3) 0.0321(12) Uani 1 1 d . . . H58 H 0.2913 1.5118 0.1745 0.048 Uiso 1 1 calc R . . H59 H 0.2723 1.5905 0.1060 0.048 Uiso 1 1 calc R . . H60 H 0.3215 1.4805 0.0972 0.048 Uiso 1 1 calc R . . C39 C 0.0162(5) 1.5667(4) 0.2092(3) 0.0340(12) Uani 1 1 d . . . H61 H -0.0665 1.5474 0.2235 0.051 Uiso 1 1 calc R . . H62 H 0.0247 1.6343 0.1797 0.051 Uiso 1 1 calc R . . H63 H 0.0393 1.5645 0.2528 0.051 Uiso 1 1 calc R . . C40 C 0.2996(4) 1.2371(3) 0.0696(2) 0.0185(9) Uani 1 1 d . . . C41 C 0.4067(4) 1.2895(3) 0.0466(2) 0.0204(10) Uani 1 1 d . . . C42 C 0.4349(4) 1.3584(4) -0.0191(3) 0.0262(11) Uani 1 1 d . . . H64 H 0.5047 1.3956 -0.0339 0.031 Uiso 1 1 calc R . . C43 C 0.3624(5) 1.3730(4) -0.0629(3) 0.0293(11) Uani 1 1 d . . . H65 H 0.3816 1.4210 -0.1071 0.035 Uiso 1 1 calc R . . C44 C 0.2619(5) 1.3179(4) -0.0426(3) 0.0299(11) Uani 1 1 d . . . H66 H 0.2147 1.3257 -0.0744 0.036 Uiso 1 1 calc R . . C45 C 0.2289(4) 1.2511(3) 0.0238(2) 0.0190(9) Uani 1 1 d . . . C46 C 0.4975(4) 1.2692(3) 0.0880(2) 0.0219(10) Uani 1 1 d . . . H67 H 0.4678 1.2135 0.1305 0.026 Uiso 1 1 calc R . . C47 C 0.5160(5) 1.3571(4) 0.1177(3) 0.0403(14) Uani 1 1 d . . . H68 H 0.5756 1.3388 0.1434 0.060 Uiso 1 1 calc R . . H69 H 0.4411 1.3755 0.1515 0.060 Uiso 1 1 calc R . . H70 H 0.5434 1.4137 0.0774 0.060 Uiso 1 1 calc R . . C48 C 0.6159(5) 1.2333(5) 0.0389(3) 0.0398(14) Uani 1 1 d . . . H71 H 0.6744 1.2201 0.0655 0.060 Uiso 1 1 calc R . . H72 H 0.6448 1.2847 -0.0050 0.060 Uiso 1 1 calc R . . H73 H 0.6036 1.1721 0.0249 0.060 Uiso 1 1 calc R . . C49 C 0.1158(4) 1.1927(4) 0.0420(3) 0.0255(11) Uani 1 1 d . . . H74 H 0.0888 1.1669 0.0958 0.031 Uiso 1 1 calc R . . C50 C 0.1429(5) 1.1043(4) 0.0056(3) 0.0382(13) Uani 1 1 d . . . H75 H 0.0703 1.0679 0.0173 0.057 Uiso 1 1 calc R . . H76 H 0.2021 1.0605 0.0230 0.057 Uiso 1 1 calc R . . H77 H 0.1740 1.1272 -0.0473 0.057 Uiso 1 1 calc R . . C51 C 0.0142(5) 1.2572(4) 0.0219(3) 0.0399(14) Uani 1 1 d . . . H78 H -0.0552 1.2163 0.0346 0.060 Uiso 1 1 calc R . . H79 H 0.0389 1.2850 -0.0305 0.060 Uiso 1 1 calc R . . H80 H -0.0059 1.3113 0.0489 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0099(2) 0.0113(2) 0.0110(2) -0.00410(17) -0.00271(16) 0.00047(16) C1 0.020(2) 0.024(2) 0.015(2) -0.0078(18) -0.0081(18) 0.0032(18) C2 0.016(2) 0.025(2) 0.020(2) -0.0088(19) -0.0054(18) 0.0036(18) C3 0.020(2) 0.036(3) 0.036(3) -0.015(2) -0.005(2) 0.008(2) C4 0.031(3) 0.030(3) 0.041(3) -0.020(2) -0.012(2) 0.014(2) C5 0.024(3) 0.023(2) 0.035(3) -0.014(2) -0.010(2) 0.003(2) C6 0.020(2) 0.023(2) 0.018(2) -0.0067(19) -0.0072(19) 0.0024(18) C7 0.021(2) 0.023(2) 0.014(2) -0.0067(18) -0.0030(18) -0.0024(18) O1 0.0166(15) 0.0178(16) 0.0208(16) -0.0089(13) -0.0021(13) -0.0024(12) W1 0.01835(10) 0.02275(11) 0.03150(12) -0.01497(8) -0.00295(8) -0.00389(7) C8 0.021(3) 0.022(3) 0.056(4) -0.021(2) -0.006(2) 0.001(2) O2 0.027(2) 0.037(2) 0.112(4) -0.036(3) -0.016(2) -0.0072(18) C9 0.021(3) 0.035(3) 0.047(3) -0.023(3) -0.015(2) 0.000(2) O3 0.029(2) 0.087(3) 0.053(3) -0.055(3) -0.0110(19) 0.011(2) C10 0.029(3) 0.030(3) 0.033(3) -0.013(2) -0.008(2) -0.002(2) O4 0.045(2) 0.036(2) 0.045(2) -0.0064(19) -0.020(2) 0.0051(19) C11 0.020(2) 0.017(2) 0.034(3) -0.007(2) -0.009(2) -0.0061(19) O5 0.0259(18) 0.0259(18) 0.0277(19) -0.0106(15) -0.0016(15) -0.0030(14) C12 0.027(3) 0.028(3) 0.026(3) -0.008(2) -0.004(2) 0.009(2) O6 0.039(2) 0.054(3) 0.040(2) -0.007(2) -0.0059(19) 0.012(2) C13 0.0092(19) 0.0127(19) 0.0102(19) -0.0034(16) -0.0042(16) -0.0015(15) C14 0.0059(18) 0.013(2) 0.013(2) -0.0016(16) -0.0003(16) -0.0011(15) C15 0.015(2) 0.017(2) 0.012(2) -0.0025(17) -0.0095(17) -0.0013(17) C16 0.012(2) 0.017(2) 0.015(2) -0.0061(17) -0.0016(17) -0.0046(16) C17 0.0105(19) 0.0094(19) 0.016(2) -0.0036(16) -0.0028(16) 0.0005(15) C18 0.0078(19) 0.013(2) 0.015(2) -0.0016(16) -0.0028(16) -0.0030(15) C19 0.014(2) 0.015(2) 0.017(2) -0.0051(17) -0.0092(17) 0.0020(16) Si1 0.0180(6) 0.0167(6) 0.0175(6) -0.0007(5) -0.0094(5) -0.0017(5) Si2 0.0141(6) 0.0225(6) 0.0275(7) -0.0054(5) -0.0126(5) 0.0047(5) C20 0.017(2) 0.031(3) 0.023(2) 0.002(2) -0.0074(19) -0.0086(19) C21 0.045(3) 0.021(3) 0.037(3) -0.001(2) -0.015(3) -0.007(2) C22 0.029(3) 0.044(3) 0.018(2) 0.000(2) -0.009(2) -0.009(2) C23 0.014(2) 0.048(3) 0.029(3) -0.010(2) -0.005(2) -0.005(2) C24 0.028(3) 0.033(3) 0.070(4) -0.015(3) -0.028(3) 0.015(2) C25 0.024(3) 0.046(3) 0.026(3) -0.001(2) -0.015(2) -0.005(2) C26 0.021(2) 0.017(2) 0.017(2) -0.0079(18) -0.0080(18) -0.0017(18) Si3 0.0281(7) 0.0243(7) 0.0263(7) -0.0076(6) -0.0106(6) -0.0104(6) Si4 0.0295(7) 0.0256(7) 0.0160(6) -0.0098(5) -0.0051(5) -0.0065(5) C27 0.055(4) 0.052(4) 0.038(3) 0.004(3) -0.018(3) -0.031(3) C28 0.023(3) 0.043(3) 0.058(4) -0.017(3) -0.008(3) -0.007(2) C29 0.052(4) 0.037(3) 0.044(3) -0.018(3) -0.015(3) -0.017(3) C30 0.032(3) 0.037(3) 0.020(2) -0.007(2) 0.002(2) -0.015(2) C31 0.046(3) 0.044(3) 0.025(3) 0.002(2) -0.019(3) -0.012(3) C32 0.065(4) 0.043(3) 0.028(3) -0.022(3) -0.002(3) -0.009(3) C33 0.012(2) 0.012(2) 0.014(2) -0.0054(16) -0.0078(17) 0.0048(16) Si5 0.0125(6) 0.0156(6) 0.0258(7) -0.0087(5) -0.0084(5) 0.0028(5) Si6 0.0239(6) 0.0126(6) 0.0216(6) -0.0006(5) -0.0118(5) 0.0028(5) C34 0.014(2) 0.020(2) 0.041(3) -0.006(2) -0.007(2) -0.0010(18) C35 0.023(3) 0.043(3) 0.031(3) -0.022(2) 0.001(2) -0.004(2) C36 0.021(3) 0.028(3) 0.052(3) -0.006(2) -0.021(2) 0.002(2) C37 0.057(4) 0.023(3) 0.036(3) 0.001(2) -0.028(3) 0.007(2) C38 0.035(3) 0.022(3) 0.034(3) 0.008(2) -0.011(2) -0.009(2) C39 0.038(3) 0.015(2) 0.052(3) -0.011(2) -0.015(3) 0.003(2) C40 0.020(2) 0.016(2) 0.016(2) -0.0032(18) -0.0025(18) 0.0010(18) C41 0.023(2) 0.019(2) 0.017(2) -0.0053(18) -0.0019(19) 0.0002(18) C42 0.028(3) 0.024(2) 0.023(3) -0.005(2) -0.002(2) -0.001(2) C43 0.041(3) 0.025(3) 0.016(2) 0.000(2) -0.005(2) -0.002(2) C44 0.039(3) 0.030(3) 0.026(3) -0.006(2) -0.017(2) 0.006(2) C45 0.026(2) 0.018(2) 0.014(2) -0.0046(18) -0.0073(19) 0.0025(18) C46 0.017(2) 0.024(2) 0.020(2) 0.0027(19) -0.0023(19) -0.0086(19) C47 0.046(3) 0.025(3) 0.061(4) -0.004(3) -0.031(3) -0.008(2) C48 0.023(3) 0.053(4) 0.032(3) 0.003(3) 0.000(2) -0.005(2) C49 0.025(3) 0.033(3) 0.021(2) -0.004(2) -0.012(2) 0.002(2) C50 0.039(3) 0.035(3) 0.044(3) -0.013(3) -0.011(3) -0.009(2) C51 0.039(3) 0.040(3) 0.051(4) -0.007(3) -0.029(3) 0.002(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 Ge1 O1 1.895(3) . ? Ge1 C1 1.941(4) . ? Ge1 C13 1.954(4) . ? Ge1 C40 1.979(4) . ? C1 C2 1.393(6) . ? C1 C6 1.409(6) . ? C2 C3 1.384(7) . ? C3 C4 1.386(7) . ? C4 C5 1.380(7) . ? C5 C6 1.390(6) . ? C6 C7 1.503(6) . ? C7 O1 1.292(5) . ? C7 W1 2.194(4) . ? W1 C12 2.015(5) . ? W1 C8 2.027(5) . ? W1 C9 2.035(5) . ? W1 C11 2.049(5) . ? W1 C10 2.052(6) . ? C8 O2 1.143(6) . ? C9 O3 1.135(6) . ? C10 O4 1.133(6) . ? C11 O5 1.138(6) . ? C12 O6 1.145(6) . ? C13 C18 1.421(6) . ? C13 C14 1.425(6) . ? C14 C15 1.395(6) . ? C14 C19 1.525(5) . ? C15 C16 1.386(6) . ? C16 C17 1.395(6) . ? C16 C26 1.519(6) . ? C17 C18 1.397(6) . ? C18 C33 1.526(5) . ? C19 Si1 1.903(4) . ? C19 Si2 1.905(4) . ? Si1 C20 1.862(5) . ? Si1 C22 1.864(5) . ? Si1 C21 1.872(5) . ? Si2 C24 1.862(5) . ? Si2 C23 1.862(5) . ? Si2 C25 1.869(5) . ? C26 Si4 1.899(4) . ? C26 Si3 1.900(4) . ? Si3 C28 1.859(6) . ? Si3 C27 1.868(6) . ? Si3 C29 1.872(5) . ? Si4 C30 1.862(5) . ? Si4 C32 1.866(5) . ? Si4 C31 1.867(6) . ? C33 Si6 1.905(4) . ? C33 Si5 1.915(4) . ? Si5 C34 1.852(5) . ? Si5 C35 1.865(5) . ? Si5 C36 1.874(5) . ? Si6 C38 1.859(5) . ? Si6 C37 1.863(5) . ? Si6 C39 1.869(5) . ? C40 C45 1.394(6) . ? C40 C41 1.421(6) . ? C41 C42 1.394(6) . ? C41 C46 1.523(6) . ? C42 C43 1.376(7) . ? C43 C44 1.382(7) . ? C44 C45 1.391(7) . ? C45 C49 1.539(6) . ? C46 C47 1.522(7) . ? C46 C48 1.545(7) . ? C49 C50 1.508(7) . ? C49 C51 1.533(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 C1 85.81(16) . . ? O1 Ge1 C13 106.13(14) . . ? C1 Ge1 C13 125.38(17) . . ? O1 Ge1 C40 112.55(16) . . ? C1 Ge1 C40 108.60(18) . . ? C13 Ge1 C40 114.44(17) . . ? C2 C1 C6 120.0(4) . . ? C2 C1 Ge1 131.4(4) . . ? C6 C1 Ge1 108.5(3) . . ? C3 C2 C1 119.5(4) . . ? C2 C3 C4 120.7(4) . . ? C5 C4 C3 120.2(5) . . ? C4 C5 C6 120.3(5) . . ? C5 C6 C1 119.3(4) . . ? C5 C6 C7 124.2(4) . . ? C1 C6 C7 116.5(4) . . ? O1 C7 C6 111.8(4) . . ? O1 C7 W1 120.4(3) . . ? C6 C7 W1 127.7(3) . . ? C7 O1 Ge1 117.4(3) . . ? C12 W1 C8 87.7(2) . . ? C12 W1 C9 91.0(2) . . ? C8 W1 C9 89.7(2) . . ? C12 W1 C11 87.74(19) . . ? C8 W1 C11 90.01(19) . . ? C9 W1 C11 178.7(2) . . ? C12 W1 C10 176.4(2) . . ? C8 W1 C10 90.7(2) . . ? C9 W1 C10 92.3(2) . . ? C11 W1 C10 89.00(19) . . ? C12 W1 C7 91.89(19) . . ? C8 W1 C7 175.71(19) . . ? C9 W1 C7 85.99(18) . . ? C11 W1 C7 94.24(16) . . ? C10 W1 C7 89.97(19) . . ? O2 C8 W1 177.8(5) . . ? O3 C9 W1 178.6(5) . . ? O4 C10 W1 177.7(5) . . ? O5 C11 W1 176.1(4) . . ? O6 C12 W1 176.7(5) . . ? C18 C13 C14 119.2(4) . . ? C18 C13 Ge1 119.3(3) . . ? C14 C13 Ge1 121.3(3) . . ? C15 C14 C13 118.7(4) . . ? C15 C14 C19 118.1(4) . . ? C13 C14 C19 123.1(4) . . ? C16 C15 C14 123.0(4) . . ? C15 C16 C17 117.1(4) . . ? C15 C16 C26 123.2(4) . . ? C17 C16 C26 119.7(4) . . ? C16 C17 C18 123.1(4) . . ? C17 C18 C13 118.4(4) . . ? C17 C18 C33 116.4(3) . . ? C13 C18 C33 125.2(4) . . ? C14 C19 Si1 111.2(3) . . ? C14 C19 Si2 116.6(3) . . ? Si1 C19 Si2 115.4(2) . . ? C20 Si1 C22 108.0(2) . . ? C20 Si1 C21 108.2(2) . . ? C22 Si1 C21 108.1(2) . . ? C20 Si1 C19 108.9(2) . . ? C22 Si1 C19 114.3(2) . . ? C21 Si1 C19 109.2(2) . . ? C24 Si2 C23 109.0(3) . . ? C24 Si2 C25 107.7(3) . . ? C23 Si2 C25 105.9(2) . . ? C24 Si2 C19 108.3(2) . . ? C23 Si2 C19 109.3(2) . . ? C25 Si2 C19 116.5(2) . . ? C16 C26 Si4 113.7(3) . . ? C16 C26 Si3 112.6(3) . . ? Si4 C26 Si3 117.0(2) . . ? C28 Si3 C27 107.6(3) . . ? C28 Si3 C29 109.0(3) . . ? C27 Si3 C29 107.4(3) . . ? C28 Si3 C26 113.1(2) . . ? C27 Si3 C26 108.7(2) . . ? C29 Si3 C26 110.9(2) . . ? C30 Si4 C32 107.8(3) . . ? C30 Si4 C31 110.0(3) . . ? C32 Si4 C31 107.7(3) . . ? C30 Si4 C26 108.5(2) . . ? C32 Si4 C26 109.2(2) . . ? C31 Si4 C26 113.5(2) . . ? C18 C33 Si6 115.6(3) . . ? C18 C33 Si5 111.2(3) . . ? Si6 C33 Si5 111.37(19) . . ? C34 Si5 C35 106.4(2) . . ? C34 Si5 C36 106.3(2) . . ? C35 Si5 C36 109.8(3) . . ? C34 Si5 C33 110.92(19) . . ? C35 Si5 C33 112.6(2) . . ? C36 Si5 C33 110.5(2) . . ? C38 Si6 C37 105.4(3) . . ? C38 Si6 C39 106.6(2) . . ? C37 Si6 C39 107.6(3) . . ? C38 Si6 C33 112.9(2) . . ? C37 Si6 C33 110.4(2) . . ? C39 Si6 C33 113.5(2) . . ? C45 C40 C41 119.1(4) . . ? C45 C40 Ge1 126.2(3) . . ? C41 C40 Ge1 114.7(3) . . ? C42 C41 C40 119.3(4) . . ? C42 C41 C46 117.6(4) . . ? C40 C41 C46 122.9(4) . . ? C43 C42 C41 120.6(5) . . ? C42 C43 C44 120.2(4) . . ? C43 C44 C45 120.6(5) . . ? C44 C45 C40 120.0(4) . . ? C44 C45 C49 117.3(4) . . ? C40 C45 C49 122.7(4) . . ? C47 C46 C41 114.0(4) . . ? C47 C46 C48 110.8(4) . . ? C41 C46 C48 109.4(4) . . ? C50 C49 C51 110.7(4) . . ? C50 C49 C45 110.2(4) . . ? C51 C49 C45 113.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ge1 C1 C2 177.3(4) . . . . ? C13 Ge1 C1 C2 -75.8(5) . . . . ? C40 Ge1 C1 C2 64.9(5) . . . . ? O1 Ge1 C1 C6 1.2(3) . . . . ? C13 Ge1 C1 C6 108.1(3) . . . . ? C40 Ge1 C1 C6 -111.2(3) . . . . ? C6 C1 C2 C3 -0.5(7) . . . . ? Ge1 C1 C2 C3 -176.3(4) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C2 C3 C4 C5 0.2(8) . . . . ? C3 C4 C5 C6 -0.4(8) . . . . ? C4 C5 C6 C1 0.2(7) . . . . ? C4 C5 C6 C7 179.0(5) . . . . ? C2 C1 C6 C5 0.3(7) . . . . ? Ge1 C1 C6 C5 176.9(4) . . . . ? C2 C1 C6 C7 -178.6(4) . . . . ? Ge1 C1 C6 C7 -2.0(5) . . . . ? C5 C6 C7 O1 -176.9(4) . . . . ? C1 C6 C7 O1 2.0(6) . . . . ? C5 C6 C7 W1 0.0(7) . . . . ? C1 C6 C7 W1 178.9(3) . . . . ? C6 C7 O1 Ge1 -0.9(5) . . . . ? W1 C7 O1 Ge1 -178.11(17) . . . . ? C1 Ge1 O1 C7 -0.2(3) . . . . ? C13 Ge1 O1 C7 -125.8(3) . . . . ? C40 Ge1 O1 C7 108.3(3) . . . . ? O1 C7 W1 C12 36.9(4) . . . . ? C6 C7 W1 C12 -139.8(4) . . . . ? O1 C7 W1 C8 121(3) . . . . ? C6 C7 W1 C8 -56(3) . . . . ? O1 C7 W1 C9 127.7(4) . . . . ? C6 C7 W1 C9 -49.0(4) . . . . ? O1 C7 W1 C11 -51.0(4) . . . . ? C6 C7 W1 C11 132.3(4) . . . . ? O1 C7 W1 C10 -140.0(4) . . . . ? C6 C7 W1 C10 43.3(4) . . . . ? C12 W1 C8 O2 70(12) . . . . ? C9 W1 C8 O2 -21(12) . . . . ? C11 W1 C8 O2 158(12) . . . . ? C10 W1 C8 O2 -113(12) . . . . ? C7 W1 C8 O2 -14(14) . . . . ? C12 W1 C9 O3 66(20) . . . . ? C8 W1 C9 O3 153(20) . . . . ? C11 W1 C9 O3 74(22) . . . . ? C10 W1 C9 O3 -116(20) . . . . ? C7 W1 C9 O3 -26(20) . . . . ? C12 W1 C10 O4 30(13) . . . . ? C8 W1 C10 O4 -33(11) . . . . ? C9 W1 C10 O4 -123(11) . . . . ? C11 W1 C10 O4 57(11) . . . . ? C7 W1 C10 O4 151(11) . . . . ? C12 W1 C11 O5 76(6) . . . . ? C8 W1 C11 O5 -11(6) . . . . ? C9 W1 C11 O5 68(12) . . . . ? C10 W1 C11 O5 -102(6) . . . . ? C7 W1 C11 O5 168(6) . . . . ? C8 W1 C12 O6 13(8) . . . . ? C9 W1 C12 O6 102(8) . . . . ? C11 W1 C12 O6 -77(8) . . . . ? C10 W1 C12 O6 -51(9) . . . . ? C7 W1 C12 O6 -171(8) . . . . ? O1 Ge1 C13 C18 -83.3(3) . . . . ? C1 Ge1 C13 C18 -179.7(3) . . . . ? C40 Ge1 C13 C18 41.5(4) . . . . ? O1 Ge1 C13 C14 101.4(3) . . . . ? C1 Ge1 C13 C14 4.9(4) . . . . ? C40 Ge1 C13 C14 -133.9(3) . . . . ? C18 C13 C14 C15 -7.4(6) . . . . ? Ge1 C13 C14 C15 167.9(3) . . . . ? C18 C13 C14 C19 168.2(4) . . . . ? Ge1 C13 C14 C19 -16.5(5) . . . . ? C13 C14 C15 C16 2.3(6) . . . . ? C19 C14 C15 C16 -173.5(4) . . . . ? C14 C15 C16 C17 3.0(6) . . . . ? C14 C15 C16 C26 -179.1(4) . . . . ? C15 C16 C17 C18 -3.2(6) . . . . ? C26 C16 C17 C18 178.8(4) . . . . ? C16 C17 C18 C13 -1.9(6) . . . . ? C16 C17 C18 C33 175.3(4) . . . . ? C14 C13 C18 C17 7.2(6) . . . . ? Ge1 C13 C18 C17 -168.2(3) . . . . ? C14 C13 C18 C33 -169.7(4) . . . . ? Ge1 C13 C18 C33 14.9(5) . . . . ? C15 C14 C19 Si1 80.4(4) . . . . ? C13 C14 C19 Si1 -95.2(4) . . . . ? C15 C14 C19 Si2 -54.8(5) . . . . ? C13 C14 C19 Si2 129.6(3) . . . . ? C14 C19 Si1 C20 31.2(3) . . . . ? Si2 C19 Si1 C20 166.9(2) . . . . ? C14 C19 Si1 C22 -89.6(3) . . . . ? Si2 C19 Si1 C22 46.1(3) . . . . ? C14 C19 Si1 C21 149.2(3) . . . . ? Si2 C19 Si1 C21 -75.1(3) . . . . ? C14 C19 Si2 C24 -166.4(3) . . . . ? Si1 C19 Si2 C24 60.3(3) . . . . ? C14 C19 Si2 C23 -47.8(4) . . . . ? Si1 C19 Si2 C23 178.9(2) . . . . ? C14 C19 Si2 C25 72.2(4) . . . . ? Si1 C19 Si2 C25 -61.1(3) . . . . ? C15 C16 C26 Si4 -56.9(5) . . . . ? C17 C16 C26 Si4 120.9(4) . . . . ? C15 C16 C26 Si3 79.1(5) . . . . ? C17 C16 C26 Si3 -103.1(4) . . . . ? C16 C26 Si3 C28 -60.2(4) . . . . ? Si4 C26 Si3 C28 74.3(3) . . . . ? C16 C26 Si3 C27 59.2(4) . . . . ? Si4 C26 Si3 C27 -166.3(3) . . . . ? C16 C26 Si3 C29 177.1(3) . . . . ? Si4 C26 Si3 C29 -48.4(3) . . . . ? C16 C26 Si4 C30 -34.2(4) . . . . ? Si3 C26 Si4 C30 -168.2(3) . . . . ? C16 C26 Si4 C32 -151.4(3) . . . . ? Si3 C26 Si4 C32 74.6(3) . . . . ? C16 C26 Si4 C31 88.5(4) . . . . ? Si3 C26 Si4 C31 -45.5(3) . . . . ? C17 C18 C33 Si6 51.5(4) . . . . ? C13 C18 C33 Si6 -131.6(4) . . . . ? C17 C18 C33 Si5 -76.7(4) . . . . ? C13 C18 C33 Si5 100.2(4) . . . . ? C18 C33 Si5 C34 -66.0(3) . . . . ? Si6 C33 Si5 C34 163.6(2) . . . . ? C18 C33 Si5 C35 53.2(4) . . . . ? Si6 C33 Si5 C35 -77.2(3) . . . . ? C18 C33 Si5 C36 176.4(3) . . . . ? Si6 C33 Si5 C36 46.0(3) . . . . ? C18 C33 Si6 C38 30.6(4) . . . . ? Si5 C33 Si6 C38 158.7(2) . . . . ? C18 C33 Si6 C37 148.3(3) . . . . ? Si5 C33 Si6 C37 -83.6(3) . . . . ? C18 C33 Si6 C39 -90.8(3) . . . . ? Si5 C33 Si6 C39 37.3(3) . . . . ? O1 Ge1 C40 C45 3.6(4) . . . . ? C1 Ge1 C40 C45 96.8(4) . . . . ? C13 Ge1 C40 C45 -117.7(4) . . . . ? O1 Ge1 C40 C41 -174.8(3) . . . . ? C1 Ge1 C40 C41 -81.6(3) . . . . ? C13 Ge1 C40 C41 63.9(4) . . . . ? C45 C40 C41 C42 4.2(6) . . . . ? Ge1 C40 C41 C42 -177.3(3) . . . . ? C45 C40 C41 C46 -171.7(4) . . . . ? Ge1 C40 C41 C46 6.9(6) . . . . ? C40 C41 C42 C43 -2.6(7) . . . . ? C46 C41 C42 C43 173.5(4) . . . . ? C41 C42 C43 C44 -1.2(7) . . . . ? C42 C43 C44 C45 3.5(7) . . . . ? C43 C44 C45 C40 -1.9(7) . . . . ? C43 C44 C45 C49 -179.9(4) . . . . ? C41 C40 C45 C44 -1.9(6) . . . . ? Ge1 C40 C45 C44 179.7(3) . . . . ? C41 C40 C45 C49 175.9(4) . . . . ? Ge1 C40 C45 C49 -2.4(6) . . . . ? C42 C41 C46 C47 67.0(6) . . . . ? C40 C41 C46 C47 -117.1(5) . . . . ? C42 C41 C46 C48 -57.7(5) . . . . ? C40 C41 C46 C48 118.2(5) . . . . ? C44 C45 C49 C50 82.0(5) . . . . ? C40 C45 C49 C50 -96.0(5) . . . . ? C44 C45 C49 C51 -42.4(6) . . . . ? C40 C45 C49 C51 139.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 3.244 _refine_diff_density_min -1.737 _refine_diff_density_rms 0.105