Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2011 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_fh72tet _database_code_depnum_ccdc_archive 'CCDC 807921' #TrackingRef '- FH72tet(CCDC-807921).pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.50 H119 Ge9 Li Mo N4 O3 Si12' _chemical_formula_weight 1851.71 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 25.696(4) _cell_length_b 25.696(4) _cell_length_c 26.818(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17708(5) _cell_formula_units_Z 8 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 12614 _cell_measurement_theta_min 1.10 _cell_measurement_theta_max 23.08 _exptl_crystal_description diamond _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7512 _exptl_absorpt_coefficient_mu 3.339 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4868 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 149(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33783 _diffrn_reflns_av_R_equivalents 0.1641 _diffrn_reflns_av_sigmaI/netI 0.2518 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 22.78 _reflns_number_total 11755 _reflns_number_gt 4983 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 11755 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1695 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.801 _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 Mo1 Mo 0.60543(5) 0.31323(6) 0.84943(8) 0.0507(5) Uani 1 1 d . . . Ge1 Ge 0.64313(7) 0.21102(7) 0.84283(10) 0.0515(6) Uani 1 1 d . . . Ge2 Ge 0.76899(7) 0.28866(8) 0.84272(11) 0.0717(8) Uani 1 1 d . . . Ge3 Ge 0.65466(6) 0.30912(7) 0.75466(9) 0.0532(6) Uani 1 1 d . . . Ge4 Ge 0.69119(8) 0.27677(8) 0.89902(10) 0.0570(7) Uani 1 1 d . . . Ge5 Ge 0.69961(7) 0.35675(7) 0.82723(9) 0.0589(7) Uani 1 1 d . . . Ge6 Ge 0.58311(7) 0.24324(7) 0.77387(9) 0.0552(7) Uani 1 1 d . . . Ge7 Ge 0.67834(7) 0.20681(7) 0.74676(10) 0.0598(7) Uani 1 1 d . . . Ge8 Ge 0.75032(7) 0.27746(8) 0.75086(11) 0.0634(7) Uani 1 1 d . . . Ge9 Ge 0.74082(7) 0.19780(8) 0.82208(9) 0.0609(7) Uani 1 1 d . . . Si1 Si 0.6143(2) 0.12947(19) 0.8777(3) 0.0588(19) Uani 1 1 d . . . Si2 Si 0.8541(2) 0.3080(2) 0.8708(3) 0.0642(18) Uani 1 1 d . . . Si3 Si 0.6391(2) 0.3525(2) 0.6769(3) 0.0664(18) Uani 1 1 d . . . Si10 Si 0.6117(2) 0.06534(19) 0.8145(3) 0.071(2) Uani 1 1 d . . . Si11 Si 0.5300(2) 0.1399(2) 0.9098(3) 0.077(2) Uani 1 1 d . . . Si12 Si 0.6695(3) 0.1032(3) 0.9417(3) 0.098(3) Uani 1 1 d . . . Si20 Si 0.8798(2) 0.2369(3) 0.9206(3) 0.107(3) Uani 1 1 d . . . Si21 Si 0.8481(2) 0.3839(3) 0.9193(4) 0.117(4) Uani 1 1 d . . . Si22 Si 0.9068(2) 0.3233(2) 0.8020(3) 0.067(2) Uani 1 1 d . . . Si30 Si 0.7039(3) 0.4117(3) 0.6575(3) 0.104(3) Uani 1 1 d . . . Si31 Si 0.6332(2) 0.2902(2) 0.6125(3) 0.075(2) Uani 1 1 d . . . Si32 Si 0.5578(3) 0.3954(3) 0.6825(3) 0.094(2) Uani 1 1 d . . . O1 O 0.4872(5) 0.3180(5) 0.8262(6) 0.080(4) Uiso 1 1 d . . . O2 O 0.5677(5) 0.3029(5) 0.9584(7) 0.083(5) Uiso 1 1 d . . . O3 O 0.5924(6) 0.4317(6) 0.8625(6) 0.095(5) Uiso 1 1 d . . . C1 C 0.5331(7) 0.3152(7) 0.8335(8) 0.056(5) Uiso 1 1 d . . . C2 C 0.5832(7) 0.3072(7) 0.9142(8) 0.056(5) Uiso 1 1 d . . . C3 C 0.5998(6) 0.3836(7) 0.8596(8) 0.053(5) Uiso 1 1 d . . . C10B C 0.6041(8) 0.0013(8) 0.8448(11) 0.099(8) Uiso 1 1 d . . . H10A H 0.6029 -0.0260 0.8192 0.148 Uiso 1 1 calc R . . H10B H 0.5717 0.0008 0.8640 0.148 Uiso 1 1 calc R . . H10C H 0.6336 -0.0050 0.8671 0.148 Uiso 1 1 calc R . . C10A C 0.5569(9) 0.0777(10) 0.7696(12) 0.133(10) Uiso 1 1 d . . . H10D H 0.5569 0.0506 0.7438 0.200 Uiso 1 1 calc R . . H10E H 0.5616 0.1118 0.7539 0.200 Uiso 1 1 calc R . . H10F H 0.5237 0.0770 0.7875 0.200 Uiso 1 1 calc R . . C10C C 0.6697(8) 0.0632(9) 0.7751(11) 0.112(9) Uiso 1 1 d . . . H10G H 0.6657 0.0359 0.7500 0.168 Uiso 1 1 calc R . . H10H H 0.7003 0.0557 0.7958 0.168 Uiso 1 1 calc R . . H10I H 0.6743 0.0969 0.7586 0.168 Uiso 1 1 calc R . . C11B C 0.5036(8) 0.0746(7) 0.9247(9) 0.077(7) Uiso 1 1 d . . . H11A H 0.4683 0.0782 0.9383 0.115 Uiso 1 1 calc R . . H11B H 0.5260 0.0577 0.9494 0.115 Uiso 1 1 calc R . . H11C H 0.5024 0.0535 0.8943 0.115 Uiso 1 1 calc R . . C11A C 0.4874(8) 0.1748(8) 0.8697(10) 0.098(8) Uiso 1 1 d . . . H11D H 0.4531 0.1778 0.8854 0.147 Uiso 1 1 calc R . . H11E H 0.4841 0.1562 0.8379 0.147 Uiso 1 1 calc R . . H11F H 0.5016 0.2097 0.8636 0.147 Uiso 1 1 calc R . . C11C C 0.5330(10) 0.1735(10) 0.9726(12) 0.125(10) Uiso 1 1 d . . . H11G H 0.4977 0.1776 0.9858 0.188 Uiso 1 1 calc R . . H11H H 0.5493 0.2077 0.9688 0.188 Uiso 1 1 calc R . . H11I H 0.5537 0.1523 0.9958 0.188 Uiso 1 1 calc R . . C12A C 0.7355(9) 0.0846(10) 0.9161(11) 0.116(9) Uiso 1 1 d . . . H12A H 0.7582 0.0735 0.9435 0.173 Uiso 1 1 calc R . . H12B H 0.7511 0.1147 0.8993 0.173 Uiso 1 1 calc R . . H12C H 0.7316 0.0561 0.8922 0.173 Uiso 1 1 calc R . . C12C C 0.6441(11) 0.0459(10) 0.9764(12) 0.131(10) Uiso 1 1 d . . . H12D H 0.6687 0.0363 1.0028 0.197 Uiso 1 1 calc R . . H12E H 0.6399 0.0165 0.9533 0.197 Uiso 1 1 calc R . . H12F H 0.6103 0.0545 0.9912 0.197 Uiso 1 1 calc R . . C12B C 0.6776(10) 0.1543(10) 0.9927(12) 0.136(11) Uiso 1 1 d . . . H12G H 0.7010 0.1410 1.0185 0.205 Uiso 1 1 calc R . . H12H H 0.6436 0.1621 1.0075 0.205 Uiso 1 1 calc R . . H12I H 0.6923 0.1861 0.9783 0.205 Uiso 1 1 calc R . . C20C C 0.8767(9) 0.1769(9) 0.8906(11) 0.113(9) Uiso 1 1 d . . . H20A H 0.8879 0.1494 0.9136 0.170 Uiso 1 1 calc R . . H20B H 0.8995 0.1773 0.8613 0.170 Uiso 1 1 calc R . . H20C H 0.8408 0.1701 0.8800 0.170 Uiso 1 1 calc R . . C20B C 0.9471(9) 0.2456(10) 0.9422(11) 0.123(10) Uiso 1 1 d . . . H20D H 0.9573 0.2157 0.9628 0.184 Uiso 1 1 calc R . . H20E H 0.9496 0.2775 0.9619 0.184 Uiso 1 1 calc R . . H20F H 0.9704 0.2480 0.9133 0.184 Uiso 1 1 calc R . . C20A C 0.8351(11) 0.2411(12) 0.9776(12) 0.157(13) Uiso 1 1 d . . . H20G H 0.8433 0.2126 1.0006 0.236 Uiso 1 1 calc R . . H20H H 0.7988 0.2383 0.9669 0.236 Uiso 1 1 calc R . . H20I H 0.8405 0.2745 0.9945 0.236 Uiso 1 1 calc R . . C21A C 0.8451(9) 0.4409(9) 0.8752(10) 0.106(9) Uiso 1 1 d . . . H21A H 0.8428 0.4733 0.8944 0.158 Uiso 1 1 calc R . . H21B H 0.8145 0.4376 0.8537 0.158 Uiso 1 1 calc R . . H21C H 0.8766 0.4415 0.8546 0.158 Uiso 1 1 calc R . . C21C C 0.7900(9) 0.3859(10) 0.9584(11) 0.119(10) Uiso 1 1 d . . . H21D H 0.7899 0.4182 0.9779 0.179 Uiso 1 1 calc R . . H21E H 0.7901 0.3561 0.9812 0.179 Uiso 1 1 calc R . . H21F H 0.7589 0.3846 0.9373 0.179 Uiso 1 1 calc R . . C21B C 0.9043(9) 0.3895(9) 0.9618(11) 0.119(10) Uiso 1 1 d . . . H21G H 0.9010 0.4214 0.9816 0.179 Uiso 1 1 calc R . . H21H H 0.9365 0.3909 0.9423 0.179 Uiso 1 1 calc R . . H21I H 0.9052 0.3593 0.9841 0.179 Uiso 1 1 calc R . . C22B C 0.9117(10) 0.2660(9) 0.7672(11) 0.125(10) Uiso 1 1 d . . . H22A H 0.9340 0.2720 0.7381 0.188 Uiso 1 1 calc R . . H22B H 0.8770 0.2553 0.7561 0.188 Uiso 1 1 calc R . . H22C H 0.9270 0.2385 0.7880 0.188 Uiso 1 1 calc R . . C22A C 0.9706(7) 0.3453(8) 0.8233(10) 0.086(7) Uiso 1 1 d . . . H22D H 0.9930 0.3518 0.7943 0.129 Uiso 1 1 calc R . . H22E H 0.9864 0.3184 0.8443 0.129 Uiso 1 1 calc R . . H22F H 0.9667 0.3775 0.8425 0.129 Uiso 1 1 calc R . . C22C C 0.8796(9) 0.3731(9) 0.7603(12) 0.121(10) Uiso 1 1 d . . . H22G H 0.9031 0.3783 0.7319 0.182 Uiso 1 1 calc R . . H22H H 0.8757 0.4059 0.7785 0.182 Uiso 1 1 calc R . . H22I H 0.8455 0.3616 0.7481 0.182 Uiso 1 1 calc R . . C30B C 0.7675(13) 0.3820(13) 0.6444(16) 0.199(15) Uiso 1 1 d . . . H30A H 0.7928 0.4094 0.6365 0.299 Uiso 1 1 calc R . . H30B H 0.7643 0.3582 0.6161 0.299 Uiso 1 1 calc R . . H30C H 0.7794 0.3627 0.6738 0.299 Uiso 1 1 calc R . . C30A C 0.7202(18) 0.4560(17) 0.704(2) 0.27(2) Uiso 1 1 d . . . H30D H 0.7479 0.4790 0.6919 0.409 Uiso 1 1 calc R . . H30E H 0.7323 0.4372 0.7336 0.409 Uiso 1 1 calc R . . H30F H 0.6895 0.4768 0.7127 0.409 Uiso 1 1 calc R . . C30C C 0.6954(13) 0.4390(12) 0.5959(15) 0.180(14) Uiso 1 1 d . . . H30G H 0.7235 0.4638 0.5890 0.269 Uiso 1 1 calc R . . H30H H 0.6618 0.4569 0.5941 0.269 Uiso 1 1 calc R . . H30I H 0.6963 0.4110 0.5711 0.269 Uiso 1 1 calc R . . C31C C 0.6985(8) 0.2636(8) 0.6015(10) 0.096(8) Uiso 1 1 d . . . H31A H 0.6969 0.2375 0.5748 0.144 Uiso 1 1 calc R . . H31B H 0.7114 0.2473 0.6321 0.144 Uiso 1 1 calc R . . H31C H 0.7221 0.2917 0.5916 0.144 Uiso 1 1 calc R . . C31B C 0.5897(8) 0.2377(9) 0.6277(10) 0.102(8) Uiso 1 1 d . . . H31D H 0.5886 0.2129 0.6000 0.154 Uiso 1 1 calc R . . H31E H 0.5548 0.2516 0.6336 0.154 Uiso 1 1 calc R . . H31F H 0.6021 0.2200 0.6578 0.154 Uiso 1 1 calc R . . C31A C 0.6083(9) 0.3188(9) 0.5575(10) 0.109(9) Uiso 1 1 d . . . H31G H 0.6061 0.2924 0.5312 0.163 Uiso 1 1 calc R . . H31H H 0.6314 0.3469 0.5467 0.163 Uiso 1 1 calc R . . H31I H 0.5735 0.3328 0.5641 0.163 Uiso 1 1 calc R . . C32A C 0.5043(9) 0.3475(9) 0.6931(11) 0.110(9) Uiso 1 1 d . . . H32A H 0.4710 0.3659 0.6954 0.165 Uiso 1 1 calc R . . H32B H 0.5108 0.3285 0.7242 0.165 Uiso 1 1 calc R . . H32C H 0.5031 0.3229 0.6652 0.165 Uiso 1 1 calc R . . C32B C 0.5562(9) 0.4345(9) 0.7424(13) 0.131(10) Uiso 1 1 d . . . H32D H 0.5227 0.4525 0.7451 0.196 Uiso 1 1 calc R . . H32E H 0.5844 0.4602 0.7420 0.196 Uiso 1 1 calc R . . H32F H 0.5607 0.4111 0.7709 0.196 Uiso 1 1 calc R . . C32C C 0.5480(14) 0.4337(13) 0.6260(16) 0.198(16) Uiso 1 1 d . . . H32G H 0.5144 0.4517 0.6279 0.296 Uiso 1 1 calc R . . H32H H 0.5482 0.4106 0.5969 0.296 Uiso 1 1 calc R . . H32I H 0.5760 0.4593 0.6228 0.296 Uiso 1 1 calc R . . C100 C 0.8038(13) 0.0770(13) 0.7061(15) 0.170(13) Uiso 1 1 d . . . H10J H 0.8076 0.0577 0.7378 0.204 Uiso 1 1 calc R . . H10K H 0.7775 0.1046 0.7112 0.204 Uiso 1 1 calc R . . C101 C 0.7873(12) 0.0442(12) 0.6702(16) 0.150(13) Uiso 1 1 d . . . H10L H 0.7514 0.0340 0.6791 0.180 Uiso 1 1 calc R . . H10M H 0.8089 0.0124 0.6731 0.180 Uiso 1 1 calc R . . C110 C 0.7877(10) 0.0132(10) 0.5884(13) 0.124(10) Uiso 1 1 d . . . H11J H 0.7546 -0.0054 0.5916 0.186 Uiso 1 1 calc R . . H11K H 0.8161 -0.0093 0.5997 0.186 Uiso 1 1 calc R . . H11L H 0.7934 0.0226 0.5534 0.186 Uiso 1 1 calc R . . C103 C 0.7409(11) 0.0823(11) 0.6068(12) 0.138(11) Uiso 1 1 d . . . H10P H 0.7125 0.0568 0.6069 0.206 Uiso 1 1 calc R . . H10Q H 0.7431 0.0987 0.5738 0.206 Uiso 1 1 calc R . . H10R H 0.7341 0.1089 0.6321 0.206 Uiso 1 1 calc R . . C104 C 0.8553(9) 0.1463(9) 0.7231(11) 0.111(9) Uiso 1 1 d . . . H10S H 0.8556 0.1367 0.7584 0.167 Uiso 1 1 calc R . . H10T H 0.8251 0.1685 0.7163 0.167 Uiso 1 1 calc R . . H10U H 0.8873 0.1653 0.7150 0.167 Uiso 1 1 calc R . . C105 C 0.8970(11) 0.0700(11) 0.7193(13) 0.149(12) Uiso 1 1 d . . . H10V H 0.8920 0.0715 0.7555 0.224 Uiso 1 1 calc R . . H10W H 0.9304 0.0861 0.7106 0.224 Uiso 1 1 calc R . . H10X H 0.8970 0.0337 0.7083 0.224 Uiso 1 1 calc R . . C200 C 0.917(2) 0.1307(17) 0.532(2) 0.067(14) Uiso 0.50 1 d P A 1 H20J H 0.9497 0.1333 0.5132 0.080 Uiso 0.50 1 calc PR A 1 H20K H 0.8877 0.1251 0.5085 0.080 Uiso 0.50 1 calc PR A 1 C201 C 0.9369(16) 0.1326(16) 0.556(2) 0.057(13) Uiso 0.50 1 d P A 2 H20L H 0.9497 0.1537 0.5843 0.068 Uiso 0.50 1 calc PR A 2 H20M H 0.9661 0.1277 0.5322 0.068 Uiso 0.50 1 calc PR A 2 C202 C 0.9649(10) 0.0715(9) 0.6034(11) 0.112(9) Uiso 1 1 d . A . H20N H 0.9938 0.0618 0.5814 0.167 Uiso 1 1 calc R . . H20O H 0.9573 0.0427 0.6262 0.167 Uiso 1 1 calc R . . H20P H 0.9744 0.1025 0.6227 0.167 Uiso 1 1 calc R . . C203 C 0.9116(8) 0.0390(7) 0.5420(8) 0.070(6) Uiso 1 1 d . A . H20Q H 0.9436 0.0319 0.5232 0.105 Uiso 1 1 calc R . . H20R H 0.8833 0.0467 0.5187 0.105 Uiso 1 1 calc R . . H20S H 0.9025 0.0085 0.5621 0.105 Uiso 1 1 calc R . . C204 C 0.868(2) 0.213(2) 0.608(2) 0.09(2) Uiso 0.50 1 d P A 2 H20T H 0.8712 0.2453 0.5884 0.128 Uiso 0.50 1 calc PR A 2 H20U H 0.9018 0.2050 0.6232 0.128 Uiso 0.50 1 calc PR A 2 H20V H 0.8417 0.2173 0.6336 0.128 Uiso 0.50 1 calc PR A 2 C214 C 0.8537(18) 0.2268(16) 0.6153(18) 0.051(14) Uiso 0.50 1 d P A 1 H21N H 0.8557 0.2585 0.5952 0.076 Uiso 0.50 1 calc PR A 1 H21O H 0.8832 0.2256 0.6385 0.076 Uiso 0.50 1 calc PR A 1 H21P H 0.8211 0.2267 0.6343 0.076 Uiso 0.50 1 calc PR A 1 C205 C 0.8102(8) 0.1844(8) 0.5463(9) 0.090(7) Uiso 1 1 d . A . H20W H 0.8133 0.2179 0.5290 0.135 Uiso 1 1 calc R . . H20X H 0.7781 0.1841 0.5661 0.135 Uiso 1 1 calc R . . H20Y H 0.8091 0.1562 0.5217 0.135 Uiso 1 1 calc R . . C210 C 0.9072(17) 0.1823(17) 0.565(2) 0.077(14) Uiso 0.50 1 d P A 1 H21J H 0.9307 0.1833 0.5942 0.092 Uiso 0.50 1 calc PR A 1 H21K H 0.9124 0.2141 0.5447 0.092 Uiso 0.50 1 calc PR A 1 C211 C 0.8951(17) 0.160(2) 0.531(2) 0.077(15) Uiso 0.50 1 d P A 2 H21L H 0.8767 0.1366 0.5076 0.092 Uiso 0.50 1 calc PR A 2 H21M H 0.9081 0.1906 0.5134 0.092 Uiso 0.50 1 calc PR A 2 C300 C 0.9211(12) 0.5665(11) 0.8787(13) 0.158(12) Uiso 1 1 d . . . H30J H 0.8984 0.5822 0.9039 0.236 Uiso 1 1 calc R . . H30K H 0.9000 0.5468 0.8549 0.236 Uiso 1 1 calc R . . H30L H 0.9401 0.5940 0.8611 0.236 Uiso 1 1 calc R . . C301 C 0.9603(14) 0.5296(13) 0.9044(18) 0.187(15) Uiso 1 1 d . . . H30M H 0.9770 0.5514 0.9303 0.224 Uiso 1 1 calc R . . H30N H 0.9382 0.5045 0.9228 0.224 Uiso 1 1 calc R . . C302 C 1.0000 0.5000 0.8859(19) 0.138(16) Uiso 1 2 d S . . H30O H 0.9817 0.4755 0.8634 0.166 Uiso 0.50 1 calc PR . . H30P H 1.0183 0.5245 0.8634 0.166 Uiso 0.50 1 calc PR . . N1 N 0.7864(6) 0.0579(7) 0.6172(8) 0.079(6) Uani 1 1 d . . . N2 N 0.8522(7) 0.0999(6) 0.6930(7) 0.079(6) Uani 1 1 d . . . N3 N 0.9197(7) 0.0826(6) 0.5738(8) 0.086(7) Uani 1 1 d . . . N4 N 0.8555(7) 0.1770(7) 0.5796(9) 0.090(7) Uani 1 1 d . . . Li1 Li 0.8517(11) 0.1054(10) 0.6178(13) 0.049(9) Uani 1 1 d . A . 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 Mo1 0.0382(9) 0.0485(9) 0.0654(15) -0.0084(10) 0.0065(10) -0.0020(8) Ge1 0.0426(11) 0.0430(11) 0.0689(19) -0.0071(12) 0.0049(12) -0.0003(9) Ge2 0.0457(12) 0.0757(15) 0.094(2) -0.0123(16) 0.0004(14) -0.0011(11) Ge3 0.0442(11) 0.0518(12) 0.0637(18) -0.0077(13) 0.0064(12) -0.0005(9) Ge4 0.0437(12) 0.0625(13) 0.065(2) -0.0139(12) 0.0057(12) -0.0040(11) Ge5 0.0484(13) 0.0509(12) 0.077(2) -0.0140(12) 0.0041(12) -0.0079(10) Ge6 0.0419(11) 0.0505(13) 0.073(2) -0.0108(13) 0.0031(12) -0.0015(10) Ge7 0.0494(12) 0.0549(12) 0.075(2) -0.0151(14) 0.0032(13) 0.0045(10) Ge8 0.0445(11) 0.0718(14) 0.0738(19) -0.0116(14) 0.0129(14) -0.0005(11) Ge9 0.0413(11) 0.0591(13) 0.082(2) -0.0101(13) 0.0047(12) 0.0062(10) Si1 0.053(3) 0.037(3) 0.086(6) -0.007(3) -0.012(3) -0.004(3) Si2 0.040(3) 0.088(4) 0.065(5) -0.006(4) 0.004(3) -0.001(3) Si3 0.069(4) 0.064(4) 0.066(5) -0.007(4) 0.006(4) -0.015(3) Si10 0.068(4) 0.039(3) 0.106(7) -0.021(4) 0.012(4) -0.006(3) Si11 0.073(4) 0.055(4) 0.102(7) -0.002(4) 0.025(4) -0.010(3) Si12 0.106(6) 0.068(4) 0.118(8) 0.018(5) -0.031(5) -0.004(4) Si20 0.046(4) 0.150(7) 0.124(9) 0.046(6) -0.008(4) -0.002(4) Si21 0.046(4) 0.151(7) 0.153(10) -0.073(7) 0.027(5) -0.027(4) Si22 0.049(3) 0.070(4) 0.082(6) -0.003(4) 0.010(3) -0.007(3) Si30 0.133(6) 0.104(5) 0.074(7) 0.017(5) 0.015(6) -0.053(5) Si31 0.062(4) 0.079(4) 0.084(6) -0.013(4) -0.004(4) -0.002(3) Si32 0.107(5) 0.078(4) 0.096(7) 0.000(5) -0.005(5) 0.019(4) N1 0.053(11) 0.117(15) 0.067(18) -0.012(13) -0.035(10) 0.004(10) N2 0.098(13) 0.062(11) 0.076(17) -0.013(10) 0.010(12) -0.056(10) N3 0.078(12) 0.056(11) 0.12(2) -0.056(12) 0.026(12) -0.006(10) N4 0.079(14) 0.066(12) 0.13(2) 0.019(13) -0.001(14) -0.014(11) Li1 0.051(18) 0.038(17) 0.06(3) -0.017(16) -0.006(18) 0.012(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C3 1.834(18) . ? Mo1 C2 1.84(2) . ? Mo1 C1 1.907(18) . ? Mo1 Ge5 2.732(2) . ? Mo1 Ge4 2.739(3) . ? Mo1 Ge6 2.769(3) . ? Mo1 Ge1 2.805(2) . ? Mo1 Ge3 2.841(3) . ? Ge1 Si1 2.412(6) . ? Ge1 Ge6 2.546(3) . ? Ge1 Ge4 2.579(3) . ? Ge1 Ge9 2.594(3) . ? Ge1 Ge7 2.733(4) . ? Ge2 Si2 2.366(6) . ? Ge2 Ge9 2.506(3) . ? Ge2 Ge4 2.524(3) . ? Ge2 Ge8 2.526(4) . ? Ge2 Ge5 2.532(3) . ? Ge3 Si3 2.399(7) . ? Ge3 Ge6 2.552(3) . ? Ge3 Ge5 2.573(3) . ? Ge3 Ge8 2.591(3) . ? Ge3 Ge7 2.707(3) . ? Ge4 Ge5 2.824(3) . ? Ge6 Ge7 2.719(3) . ? Ge7 Ge9 2.591(3) . ? Ge7 Ge8 2.594(3) . ? Ge8 Ge9 2.810(3) . ? Si1 Si12 2.327(10) . ? Si1 Si11 2.345(9) . ? Si1 Si10 2.365(9) . ? Si2 Si22 2.322(9) . ? Si2 Si21 2.349(10) . ? Si2 Si20 2.357(10) . ? Si3 Si30 2.314(9) . ? Si3 Si31 2.361(9) . ? Si3 Si32 2.366(9) . ? Si10 C10C 1.83(2) . ? Si10 C10B 1.85(2) . ? Si10 C10A 1.88(3) . ? Si11 C11A 1.78(2) . ? Si11 C11B 1.854(19) . ? Si11 C11C 1.89(3) . ? Si12 C12C 1.86(3) . ? Si12 C12A 1.89(2) . ? Si12 C12B 1.91(3) . ? Si20 C20C 1.74(2) . ? Si20 C20B 1.84(2) . ? Si20 C20A 1.91(3) . ? Si21 C21C 1.83(3) . ? Si21 C21B 1.85(3) . ? Si21 C21A 1.88(2) . ? Si22 C22B 1.75(2) . ? Si22 C22A 1.82(2) . ? Si22 C22C 1.84(3) . ? Si30 C30A 1.74(5) . ? Si30 C30C 1.81(4) . ? Si30 C30B 1.84(3) . ? Si31 C31A 1.77(3) . ? Si31 C31B 1.80(2) . ? Si31 C31C 1.84(2) . ? Si32 C32C 1.82(4) . ? Si32 C32A 1.87(2) . ? Si32 C32B 1.89(3) . ? O1 C1 1.197(18) . ? O2 C2 1.25(2) . ? O3 C3 1.253(18) . ? C100 C101 1.35(4) . ? C100 N2 1.42(3) . ? C100 Li1 2.77(5) . ? C101 N1 1.46(4) . ? C101 Li1 2.68(5) . ? C110 N1 1.38(3) . ? C103 N1 1.36(3) . ? C104 N2 1.44(3) . ? C105 N2 1.55(3) . ? C200 C210 1.61(6) . ? C200 N3 1.67(5) . ? C201 C211 1.44(6) . ? C201 N3 1.44(4) . ? C202 N3 1.43(3) . ? C203 N3 1.42(2) . ? C204 N4 1.24(6) . ? C214 N4 1.60(5) . ? C205 N4 1.48(3) . ? C210 N4 1.39(4) . ? C211 N4 1.70(6) . ? C300 C301 1.55(4) . ? C301 C302 1.37(4) . ? C302 C301 1.37(4) 2_765 ? N1 Li1 2.08(3) . ? N2 Li1 2.02(4) . ? N3 Li1 2.19(3) . ? N4 Li1 2.11(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo1 C2 85.3(9) . . ? C3 Mo1 C1 86.1(8) . . ? C2 Mo1 C1 84.8(9) . . ? C3 Mo1 Ge5 72.4(5) . . ? C2 Mo1 Ge5 121.1(6) . . ? C1 Mo1 Ge5 143.5(6) . . ? C3 Mo1 Ge4 109.2(6) . . ? C2 Mo1 Ge4 76.3(5) . . ? C1 Mo1 Ge4 154.3(6) . . ? Ge5 Mo1 Ge4 62.16(7) . . ? C3 Mo1 Ge6 137.1(6) . . ? C2 Mo1 Ge6 125.0(6) . . ? C1 Mo1 Ge6 69.6(6) . . ? Ge5 Mo1 Ge6 106.85(9) . . ? Ge4 Mo1 Ge6 107.44(8) . . ? C3 Mo1 Ge1 163.6(5) . . ? C2 Mo1 Ge1 95.1(6) . . ? C1 Mo1 Ge1 110.3(5) . . ? Ge5 Mo1 Ge1 93.64(7) . . ? Ge4 Mo1 Ge1 55.42(7) . . ? Ge6 Mo1 Ge1 54.36(7) . . ? C3 Mo1 Ge3 101.8(6) . . ? C2 Mo1 Ge3 169.2(6) . . ? C1 Mo1 Ge3 103.6(6) . . ? Ge5 Mo1 Ge3 54.95(7) . . ? Ge4 Mo1 Ge3 93.63(8) . . ? Ge6 Mo1 Ge3 54.09(7) . . ? Ge1 Mo1 Ge3 75.82(7) . . ? Si1 Ge1 Ge6 112.21(16) . . ? Si1 Ge1 Ge4 119.33(19) . . ? Ge6 Ge1 Ge4 120.09(9) . . ? Si1 Ge1 Ge9 105.49(15) . . ? Ge6 Ge1 Ge9 118.23(12) . . ? Ge4 Ge1 Ge9 75.39(8) . . ? Si1 Ge1 Ge7 115.67(17) . . ? Ge6 Ge1 Ge7 61.88(9) . . ? Ge4 Ge1 Ge7 114.73(9) . . ? Ge9 Ge1 Ge7 58.14(8) . . ? Si1 Ge1 Mo1 133.06(16) . . ? Ge6 Ge1 Mo1 62.11(7) . . ? Ge4 Ge1 Mo1 60.99(7) . . ? Ge9 Ge1 Mo1 118.07(8) . . ? Ge7 Ge1 Mo1 102.18(9) . . ? Si2 Ge2 Ge9 122.17(18) . . ? Si2 Ge2 Ge4 124.6(2) . . ? Ge9 Ge2 Ge4 77.91(9) . . ? Si2 Ge2 Ge8 120.65(19) . . ? Ge9 Ge2 Ge8 67.89(10) . . ? Ge4 Ge2 Ge8 114.78(11) . . ? Si2 Ge2 Ge5 123.94(18) . . ? Ge9 Ge2 Ge5 113.84(10) . . ? Ge4 Ge2 Ge5 67.92(9) . . ? Ge8 Ge2 Ge5 77.59(10) . . ? Si3 Ge3 Ge6 111.33(16) . . ? Si3 Ge3 Ge5 120.75(16) . . ? Ge6 Ge3 Ge5 119.10(12) . . ? Si3 Ge3 Ge8 105.68(17) . . ? Ge6 Ge3 Ge8 118.89(9) . . ? Ge5 Ge3 Ge8 75.71(9) . . ? Si3 Ge3 Ge7 114.91(17) . . ? Ge6 Ge3 Ge7 62.19(7) . . ? Ge5 Ge3 Ge7 114.85(10) . . ? Ge8 Ge3 Ge7 58.58(7) . . ? Si3 Ge3 Mo1 133.32(16) . . ? Ge6 Ge3 Mo1 61.52(8) . . ? Ge5 Ge3 Mo1 60.37(8) . . ? Ge8 Ge3 Mo1 117.99(11) . . ? Ge7 Ge3 Mo1 101.90(10) . . ? Ge2 Ge4 Ge1 96.26(11) . . ? Ge2 Ge4 Mo1 107.78(11) . . ? Ge1 Ge4 Mo1 63.58(7) . . ? Ge2 Ge4 Ge5 56.18(8) . . ? Ge1 Ge4 Ge5 96.61(11) . . ? Mo1 Ge4 Ge5 58.79(7) . . ? Ge2 Ge5 Ge3 96.41(10) . . ? Ge2 Ge5 Mo1 107.77(9) . . ? Ge3 Ge5 Mo1 64.68(8) . . ? Ge2 Ge5 Ge4 55.90(9) . . ? Ge3 Ge5 Ge4 97.76(9) . . ? Mo1 Ge5 Ge4 59.05(7) . . ? Ge1 Ge6 Ge3 85.75(9) . . ? Ge1 Ge6 Ge7 62.43(9) . . ? Ge3 Ge6 Ge7 61.71(7) . . ? Ge1 Ge6 Mo1 63.53(8) . . ? Ge3 Ge6 Mo1 64.39(8) . . ? Ge7 Ge6 Mo1 103.47(9) . . ? Ge9 Ge7 Ge8 65.64(9) . . ? Ge9 Ge7 Ge3 99.50(10) . . ? Ge8 Ge7 Ge3 58.48(7) . . ? Ge9 Ge7 Ge6 112.33(12) . . ? Ge8 Ge7 Ge6 112.92(9) . . ? Ge3 Ge7 Ge6 56.11(7) . . ? Ge9 Ge7 Ge1 58.24(9) . . ? Ge8 Ge7 Ge1 99.69(11) . . ? Ge3 Ge7 Ge1 79.24(9) . . ? Ge6 Ge7 Ge1 55.69(8) . . ? Ge2 Ge8 Ge3 96.09(11) . . ? Ge2 Ge8 Ge7 104.86(12) . . ? Ge3 Ge8 Ge7 62.93(7) . . ? Ge2 Ge8 Ge9 55.72(9) . . ? Ge3 Ge8 Ge9 96.87(9) . . ? Ge7 Ge8 Ge9 57.12(9) . . ? Ge2 Ge9 Ge7 105.54(11) . . ? Ge2 Ge9 Ge1 96.32(9) . . ? Ge7 Ge9 Ge1 63.62(9) . . ? Ge2 Ge9 Ge8 56.38(9) . . ? Ge7 Ge9 Ge8 57.24(8) . . ? Ge1 Ge9 Ge8 97.73(9) . . ? Si12 Si1 Si11 109.0(4) . . ? Si12 Si1 Si10 110.1(3) . . ? Si11 Si1 Si10 108.5(3) . . ? Si12 Si1 Ge1 110.5(3) . . ? Si11 Si1 Ge1 109.1(2) . . ? Si10 Si1 Ge1 109.6(3) . . ? Si22 Si2 Si21 109.7(3) . . ? Si22 Si2 Si20 114.7(3) . . ? Si21 Si2 Si20 110.3(4) . . ? Si22 Si2 Ge2 108.8(3) . . ? Si21 Si2 Ge2 106.8(3) . . ? Si20 Si2 Ge2 106.1(3) . . ? Si30 Si3 Si31 109.1(4) . . ? Si30 Si3 Si32 110.1(3) . . ? Si31 Si3 Si32 107.8(3) . . ? Si30 Si3 Ge3 112.4(3) . . ? Si31 Si3 Ge3 109.3(3) . . ? Si32 Si3 Ge3 108.0(3) . . ? C10C Si10 C10B 108.3(11) . . ? C10C Si10 C10A 104.2(13) . . ? C10B Si10 C10A 110.6(11) . . ? C10C Si10 Si1 114.4(9) . . ? C10B Si10 Si1 108.0(9) . . ? C10A Si10 Si1 111.3(9) . . ? C11A Si11 C11B 111.2(10) . . ? C11A Si11 C11C 109.5(11) . . ? C11B Si11 C11C 103.6(12) . . ? C11A Si11 Si1 113.9(9) . . ? C11B Si11 Si1 108.3(7) . . ? C11C Si11 Si1 109.9(8) . . ? C12C Si12 C12A 107.2(12) . . ? C12C Si12 C12B 103.1(14) . . ? C12A Si12 C12B 109.6(12) . . ? C12C Si12 Si1 112.6(10) . . ? C12A Si12 Si1 110.6(10) . . ? C12B Si12 Si1 113.3(9) . . ? C20C Si20 C20B 107.2(12) . . ? C20C Si20 C20A 113.0(13) . . ? C20B Si20 C20A 107.9(14) . . ? C20C Si20 Si2 114.3(10) . . ? C20B Si20 Si2 110.4(9) . . ? C20A Si20 Si2 104.0(10) . . ? C21C Si21 C21B 106.3(14) . . ? C21C Si21 C21A 107.7(13) . . ? C21B Si21 C21A 111.0(11) . . ? C21C Si21 Si2 113.3(9) . . ? C21B Si21 Si2 110.9(9) . . ? C21A Si21 Si2 107.6(10) . . ? C22B Si22 C22A 111.3(11) . . ? C22B Si22 C22C 106.8(14) . . ? C22A Si22 C22C 108.4(11) . . ? C22B Si22 Si2 108.8(10) . . ? C22A Si22 Si2 109.2(9) . . ? C22C Si22 Si2 112.3(9) . . ? C30A Si30 C30C 116(2) . . ? C30A Si30 C30B 101(2) . . ? C30C Si30 C30B 95.4(18) . . ? C30A Si30 Si3 116.3(18) . . ? C30C Si30 Si3 111.9(11) . . ? C30B Si30 Si3 114.2(11) . . ? C31A Si31 C31B 106.0(11) . . ? C31A Si31 C31C 110.6(12) . . ? C31B Si31 C31C 109.0(10) . . ? C31A Si31 Si3 110.6(9) . . ? C31B Si31 Si3 112.5(9) . . ? C31C Si31 Si3 108.2(8) . . ? C32C Si32 C32A 112.4(14) . . ? C32C Si32 C32B 114.5(15) . . ? C32A Si32 C32B 101.9(12) . . ? C32C Si32 Si3 108.7(12) . . ? C32A Si32 Si3 110.6(8) . . ? C32B Si32 Si3 108.6(9) . . ? O1 C1 Mo1 176.0(18) . . ? O2 C2 Mo1 179.6(19) . . ? O3 C3 Mo1 173.4(17) . . ? C101 C100 N2 111(3) . . ? C101 C100 Li1 72(3) . . ? N2 C100 Li1 44.7(16) . . ? C100 C101 N1 123(3) . . ? C100 C101 Li1 79(2) . . ? N1 C101 Li1 50.2(14) . . ? C210 C200 N3 105(4) . . ? C211 C201 N3 111(4) . . ? N4 C210 C200 103(4) . . ? C201 C211 N4 103(4) . . ? C302 C301 C300 132(4) . . ? C301 C302 C301 137(6) 2_765 . ? C103 N1 C110 107(2) . . ? C103 N1 C101 109(2) . . ? C110 N1 C101 110(2) . . ? C103 N1 Li1 115.3(19) . . ? C110 N1 Li1 118.3(18) . . ? C101 N1 Li1 96.9(18) . . ? C100 N2 C104 105(2) . . ? C100 N2 C105 109(2) . . ? C104 N2 C105 96.5(19) . . ? C100 N2 Li1 106(2) . . ? C104 N2 Li1 120.1(17) . . ? C105 N2 Li1 119.4(19) . . ? C203 N3 C202 107.0(17) . . ? C203 N3 C201 123(3) . . ? C202 N3 C201 96(2) . . ? C203 N3 C200 100(2) . . ? C202 N3 C200 124(3) . . ? C201 N3 C200 30(2) . . ? C203 N3 Li1 114.7(15) . . ? C202 N3 Li1 114(2) . . ? C201 N3 Li1 101(2) . . ? C200 N3 Li1 97(2) . . ? C204 N4 C210 81(3) . . ? C204 N4 C205 119(3) . . ? C210 N4 C205 125(3) . . ? C204 N4 C214 17(4) . . ? C210 N4 C214 97(3) . . ? C205 N4 C214 104(2) . . ? C204 N4 C211 120(3) . . ? C210 N4 C211 41(2) . . ? C205 N4 C211 93(2) . . ? C214 N4 C211 133(3) . . ? C204 N4 Li1 112(4) . . ? C210 N4 Li1 105(2) . . ? C205 N4 Li1 111.7(15) . . ? C214 N4 Li1 114(2) . . ? C211 N4 Li1 100(2) . . ? N2 Li1 N1 88.3(15) . . ? N2 Li1 N4 123.1(16) . . ? N1 Li1 N4 123.2(16) . . ? N2 Li1 N3 120.9(16) . . ? N1 Li1 N3 118.9(14) . . ? N4 Li1 N3 86.3(14) . . ? N2 Li1 C101 55.9(13) . . ? N1 Li1 C101 32.8(10) . . ? N4 Li1 C101 142.7(15) . . ? N3 Li1 C101 128.2(14) . . ? N2 Li1 C100 29.6(9) . . ? N1 Li1 C100 59.4(12) . . ? N4 Li1 C100 131.8(15) . . ? N3 Li1 C100 138.2(16) . . ? C101 Li1 C100 28.6(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 22.78 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.496 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.091 data_fh72mon _database_code_depnum_ccdc_archive 'CCDC 807922' #TrackingRef '- FH72mon(CCDC-807922).pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H117 Ge9 Li Mo O6 Si12' _chemical_formula_weight 1871.68 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' Li Li -0.0003 0.0001 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7684(8) _cell_length_b 16.7824(10) _cell_length_c 32.886(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.823(8) _cell_angle_gamma 90.00 _cell_volume 8701.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 199(2) _cell_measurement_reflns_used 64784 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.00 _exptl_crystal_description diamond _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 3.399 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4628 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 199(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63795 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.01 _reflns_number_total 16097 _reflns_number_gt 9759 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some Si(SiMe3)3 groups as well as thf and the solvent(pentane) molecule are disordered and refined applying a split model. During refinement SADI restrains are used to obtain a similar arrangement of both split positions. ; _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^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16097 _refine_ls_number_parameters 719 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.875 _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 Mo1 Mo 0.68735(3) 0.21232(2) 0.171131(13) 0.03804(11) Uani 1 1 d . . . Ge1 Ge 0.92734(4) 0.26730(3) 0.120221(16) 0.04711(14) Uani 1 1 d . A . Ge2 Ge 0.81874(3) 0.26194(3) 0.222943(14) 0.03563(12) Uani 1 1 d . . . Ge3 Ge 0.72027(3) 0.37002(3) 0.146190(15) 0.03803(12) Uani 1 1 d . B . Ge4 Ge 0.85325(4) 0.16655(3) 0.164444(16) 0.04048(13) Uani 1 1 d . . . Ge6 Ge 0.68439(4) 0.34478(3) 0.219877(16) 0.04287(14) Uani 1 1 d . . . Ge9 Ge 0.83364(4) 0.41876(3) 0.204040(15) 0.04200(13) Uani 1 1 d . . . Ge7 Ge 0.95512(3) 0.31831(3) 0.190907(15) 0.04064(13) Uani 1 1 d . . . Ge5 Ge 0.77154(4) 0.25342(3) 0.102293(15) 0.04241(13) Uani 1 1 d . . . Ge8 Ge 0.87502(4) 0.40650(3) 0.128729(15) 0.04052(13) Uani 1 1 d . . . Si1 Si 1.04048(10) 0.24864(8) 0.07495(4) 0.0443(3) Uani 1 1 d D . . Si2 Si 0.85381(9) 0.22529(7) 0.29156(4) 0.0381(3) Uani 1 1 d . . . Si3 Si 0.63522(10) 0.47253(8) 0.11546(4) 0.0442(3) Uani 1 1 d . . . Si10 Si 1.12934(14) 0.36272(11) 0.07941(6) 0.0576(6) Uani 0.832(3) 1 d PD A 1 Si11 Si 0.98682(15) 0.23409(13) 0.00960(6) 0.0655(6) Uani 0.832(3) 1 d PD A 1 Si12 Si 1.11393(14) 0.13530(11) 0.09733(7) 0.0625(6) Uani 0.832(3) 1 d PD A 1 Si13 Si 1.1690(6) 0.2673(8) 0.1041(4) 0.089(4) Uani 0.168(3) 1 d PD A 2 Si14 Si 1.0248(9) 0.1124(5) 0.0509(3) 0.072(4) Uani 0.168(3) 1 d PD A 2 Si15 Si 1.0121(8) 0.3289(6) 0.0160(3) 0.069(4) Uani 0.168(3) 1 d PD A 2 Si20 Si 0.95457(12) 0.12270(9) 0.29152(5) 0.0575(4) Uani 1 1 d . '' . Si21 Si 0.73249(12) 0.18207(10) 0.32568(5) 0.0628(5) Uani 1 1 d . . . Si22 Si 0.90594(11) 0.33749(8) 0.32611(4) 0.0515(4) Uani 1 1 d . . . Si30 Si 0.6844(6) 0.5115(5) 0.0515(3) 0.076(3) Uani 0.50 1 d PD B 1 Si31 Si 0.6388(8) 0.5873(8) 0.1554(3) 0.0571(18) Uani 0.50 1 d PD B 1 Si32 Si 0.4981(10) 0.4242(7) 0.1094(3) 0.055(2) Uani 0.50 1 d PD B 1 Si33 Si 0.6675(6) 0.4816(4) 0.0463(3) 0.067(2) Uani 0.50 1 d PD B 2 Si34 Si 0.6578(8) 0.5930(9) 0.1505(4) 0.091(4) Uani 0.50 1 d PD B 2 Si35 Si 0.4926(11) 0.4334(8) 0.1222(3) 0.072(3) Uani 0.50 1 d PD B 2 C1 C 0.6929(3) 0.1026(3) 0.18781(16) 0.0456(13) Uani 1 1 d . . . C2 C 0.5810(4) 0.2151(3) 0.2011(2) 0.0607(16) Uani 1 1 d . . . C3 C 0.6149(4) 0.1763(4) 0.1256(2) 0.0715(19) Uani 1 1 d . . . O1 O 0.6942(3) 0.0357(2) 0.19764(12) 0.0640(11) Uani 1 1 d . . . O2 O 0.5176(3) 0.2104(3) 0.21823(18) 0.1012(18) Uani 1 1 d . . . O3 O 0.5718(4) 0.1526(3) 0.10006(16) 0.1067(19) Uani 1 1 d . . . C10C C 1.1580(5) 0.3868(4) 0.1319(2) 0.099(3) Uani 1 1 d . A 1 H10A H 1.1946 0.4340 0.1324 0.149 Uiso 1 1 calc R A 1 H10B H 1.1884 0.3417 0.1442 0.149 Uiso 1 1 calc R A 1 H10C H 1.1065 0.3977 0.1473 0.149 Uiso 1 1 calc R A 1 C10B C 1.2314(5) 0.3366(5) 0.0541(3) 0.114(3) Uani 1 1 d . A 1 H10D H 1.2699 0.3824 0.0554 0.171 Uiso 1 1 calc R A 1 H10E H 1.2200 0.3226 0.0256 0.171 Uiso 1 1 calc R A 1 H10F H 1.2577 0.2911 0.0681 0.171 Uiso 1 1 calc R A 1 C10A C 1.0736(6) 0.4488(4) 0.0519(3) 0.120(4) Uani 1 1 d . A 1 H10G H 1.1093 0.4965 0.0535 0.180 Uiso 1 1 calc R A 1 H10H H 1.0192 0.4596 0.0649 0.180 Uiso 1 1 calc R A 1 H10I H 1.0636 0.4344 0.0234 0.180 Uiso 1 1 calc R A 1 C11B C 0.9053(5) 0.3124(5) -0.0030(2) 0.105(3) Uani 1 1 d . A 1 H11A H 0.8841 0.3044 -0.0308 0.157 Uiso 1 1 calc R A 1 H11B H 0.9312 0.3653 -0.0006 0.157 Uiso 1 1 calc R A 1 H11C H 0.8582 0.3083 0.0160 0.157 Uiso 1 1 calc R A 1 C11A C 1.0758(6) 0.2512(8) -0.0271(2) 0.166(5) Uani 1 1 d . A 1 H11D H 1.0542 0.2454 -0.0550 0.249 Uiso 1 1 calc R A 1 H11E H 1.1208 0.2120 -0.0220 0.249 Uiso 1 1 calc R A 1 H11F H 1.0986 0.3050 -0.0232 0.249 Uiso 1 1 calc R A 1 C11C C 0.9359(7) 0.1301(5) 0.0045(3) 0.151(4) Uani 1 1 d . A 1 H11G H 0.9129 0.1233 -0.0231 0.227 Uiso 1 1 calc R A 1 H11H H 0.8900 0.1249 0.0242 0.227 Uiso 1 1 calc R A 1 H11I H 0.9789 0.0891 0.0100 0.227 Uiso 1 1 calc R A 1 C12B C 1.1694(6) 0.1594(5) 0.1467(3) 0.122(3) Uani 1 1 d . A 1 H12A H 1.2004 0.1124 0.1565 0.183 Uiso 1 1 calc R A 1 H12B H 1.1274 0.1750 0.1669 0.183 Uiso 1 1 calc R A 1 H12C H 1.2092 0.2034 0.1426 0.183 Uiso 1 1 calc R A 1 C12A C 1.0339(5) 0.0509(3) 0.1016(3) 0.104(3) Uani 1 1 d . A 1 H12D H 1.0629 0.0025 0.1110 0.156 Uiso 1 1 calc R A 1 H12E H 1.0073 0.0412 0.0750 0.156 Uiso 1 1 calc R A 1 H12F H 0.9903 0.0657 0.1212 0.156 Uiso 1 1 calc R A 1 C12C C 1.1908(7) 0.1029(6) 0.0576(4) 0.175(6) Uani 1 1 d . A 1 H12G H 1.2214 0.0554 0.0670 0.263 Uiso 1 1 calc R A 1 H12H H 1.2314 0.1459 0.0525 0.263 Uiso 1 1 calc R A 1 H12I H 1.1598 0.0904 0.0323 0.263 Uiso 1 1 calc R A 1 C20C C 0.9942(5) 0.1052(4) 0.3442(2) 0.095(2) Uani 1 1 d . . . H20A H 1.0363 0.0623 0.3441 0.142 Uiso 1 1 calc R . . H20B H 0.9467 0.0900 0.3615 0.142 Uiso 1 1 calc R . . H20C H 1.0204 0.1541 0.3547 0.142 Uiso 1 1 calc R . . C20B C 1.0450(5) 0.1466(4) 0.2589(3) 0.111(3) Uani 1 1 d . . . H20D H 1.0857 0.1024 0.2596 0.167 Uiso 1 1 calc R . . H20E H 1.0728 0.1952 0.2687 0.167 Uiso 1 1 calc R . . H20F H 1.0247 0.1547 0.2309 0.167 Uiso 1 1 calc R . . C20A C 0.9035(5) 0.0293(3) 0.2720(3) 0.106(3) Uani 1 1 d . . . H20G H 0.9453 -0.0139 0.2719 0.159 Uiso 1 1 calc R . . H20H H 0.8820 0.0382 0.2442 0.159 Uiso 1 1 calc R . . H20I H 0.8563 0.0147 0.2896 0.159 Uiso 1 1 calc R . . C21C C 0.7634(5) 0.1446(5) 0.3772(2) 0.096(2) Uani 1 1 d . . . H21A H 0.7127 0.1266 0.3914 0.144 Uiso 1 1 calc R . . H21B H 0.7908 0.1876 0.3927 0.144 Uiso 1 1 calc R . . H21C H 0.8030 0.1000 0.3745 0.144 Uiso 1 1 calc R . . C21B C 0.6763(6) 0.1022(6) 0.2975(2) 0.142(4) Uani 1 1 d . . . H21D H 0.6262 0.0858 0.3127 0.212 Uiso 1 1 calc R . . H21E H 0.7142 0.0565 0.2943 0.212 Uiso 1 1 calc R . . H21F H 0.6586 0.1220 0.2707 0.212 Uiso 1 1 calc R . . C21A C 0.6573(5) 0.2666(5) 0.3336(3) 0.128(4) Uani 1 1 d . . . H21G H 0.6073 0.2473 0.3479 0.193 Uiso 1 1 calc R . . H21H H 0.6400 0.2887 0.3072 0.193 Uiso 1 1 calc R . . H21I H 0.6854 0.3080 0.3499 0.193 Uiso 1 1 calc R . . C22C C 0.9190(5) 0.3150(4) 0.38133(18) 0.092(3) Uani 1 1 d . . . H22A H 0.9407 0.3622 0.3955 0.139 Uiso 1 1 calc R . . H22B H 0.9591 0.2708 0.3849 0.139 Uiso 1 1 calc R . . H22C H 0.8640 0.3000 0.3925 0.139 Uiso 1 1 calc R . . C22B C 0.8325(6) 0.4231(4) 0.3200(2) 0.107(3) Uani 1 1 d . . . H22D H 0.8555 0.4693 0.3347 0.161 Uiso 1 1 calc R . . H22E H 0.7770 0.4091 0.3310 0.161 Uiso 1 1 calc R . . H22F H 0.8261 0.4362 0.2911 0.161 Uiso 1 1 calc R . . C22A C 1.0114(5) 0.3674(5) 0.3076(2) 0.115(3) Uani 1 1 d . . . H22G H 1.0312 0.4144 0.3226 0.173 Uiso 1 1 calc R . . H22H H 1.0073 0.3801 0.2785 0.173 Uiso 1 1 calc R . . H22I H 1.0516 0.3235 0.3117 0.173 Uiso 1 1 calc R . . C30A C 0.6113(9) 0.5855(8) 0.0295(4) 0.067(4) Uiso 0.50 1 d PD B 1 H30A H 0.6317 0.6021 0.0028 0.101 Uiso 0.50 1 calc PR B 1 H30B H 0.6086 0.6319 0.0475 0.101 Uiso 0.50 1 calc PR B 1 H30C H 0.5547 0.5620 0.0265 0.101 Uiso 0.50 1 calc PR B 1 C30B C 0.7867(10) 0.5651(10) 0.0540(6) 0.128(6) Uiso 0.50 1 d PD B 1 H30D H 0.8039 0.5796 0.0265 0.191 Uiso 0.50 1 calc PR B 1 H30E H 0.8299 0.5306 0.0665 0.191 Uiso 0.50 1 calc PR B 1 H30F H 0.7804 0.6135 0.0704 0.191 Uiso 0.50 1 calc PR B 1 C30C C 0.7046(13) 0.4249(9) 0.0195(5) 0.123(6) Uiso 0.50 1 d PD B 1 H30G H 0.7254 0.4426 -0.0070 0.184 Uiso 0.50 1 calc PR B 1 H30H H 0.6519 0.3947 0.0156 0.184 Uiso 0.50 1 calc PR B 1 H30I H 0.7474 0.3909 0.0327 0.184 Uiso 0.50 1 calc PR B 1 C31A C 0.5668(12) 0.6650(10) 0.1359(6) 0.076(6) Uiso 0.50 1 d PD B 1 H31A H 0.5711 0.7123 0.1533 0.114 Uiso 0.50 1 calc PR B 1 H31B H 0.5084 0.6451 0.1359 0.114 Uiso 0.50 1 calc PR B 1 H31C H 0.5826 0.6791 0.1081 0.114 Uiso 0.50 1 calc PR B 1 C31B C 0.7473(9) 0.6265(8) 0.1656(5) 0.085(4) Uiso 0.50 1 d PD B 1 H31D H 0.7437 0.6750 0.1821 0.127 Uiso 0.50 1 calc PR B 1 H31E H 0.7746 0.6388 0.1398 0.127 Uiso 0.50 1 calc PR B 1 H31F H 0.7808 0.5863 0.1803 0.127 Uiso 0.50 1 calc PR B 1 C31C C 0.5870(10) 0.5671(7) 0.2055(4) 0.075(4) Uiso 0.50 1 d PD B 1 H31G H 0.5886 0.6154 0.2222 0.112 Uiso 0.50 1 calc PR B 1 H31H H 0.6175 0.5242 0.2197 0.112 Uiso 0.50 1 calc PR B 1 H31I H 0.5280 0.5511 0.2007 0.112 Uiso 0.50 1 calc PR B 1 C32A C 0.4171(11) 0.4965(9) 0.0909(5) 0.063(5) Uiso 0.50 1 d PD B 1 H32A H 0.3615 0.4704 0.0896 0.095 Uiso 0.50 1 calc PR B 1 H32B H 0.4323 0.5154 0.0638 0.095 Uiso 0.50 1 calc PR B 1 H32C H 0.4148 0.5418 0.1097 0.095 Uiso 0.50 1 calc PR B 1 C32B C 0.4579(10) 0.3846(8) 0.1583(4) 0.082(4) Uiso 0.50 1 d PD B 1 H32D H 0.3997 0.3654 0.1543 0.124 Uiso 0.50 1 calc PR B 1 H32E H 0.4587 0.4271 0.1787 0.124 Uiso 0.50 1 calc PR B 1 H32F H 0.4941 0.3406 0.1675 0.124 Uiso 0.50 1 calc PR B 1 C32C C 0.4952(10) 0.3434(7) 0.0705(4) 0.090(4) Uiso 0.50 1 d PD B 1 H32G H 0.4372 0.3230 0.0676 0.135 Uiso 0.50 1 calc PR B 1 H32H H 0.5331 0.3000 0.0791 0.135 Uiso 0.50 1 calc PR B 1 H32I H 0.5138 0.3646 0.0443 0.135 Uiso 0.50 1 calc PR B 1 C33A C 0.6017(9) 0.5589(7) 0.0209(4) 0.062(4) Uiso 0.50 1 d PD B 2 H33A H 0.6164 0.5620 -0.0079 0.092 Uiso 0.50 1 calc PR B 2 H33B H 0.6123 0.6106 0.0339 0.092 Uiso 0.50 1 calc PR B 2 H33C H 0.5416 0.5451 0.0233 0.092 Uiso 0.50 1 calc PR B 2 C33B C 0.7812(8) 0.4989(9) 0.0374(5) 0.096(5) Uiso 0.50 1 d PD B 2 H33D H 0.7910 0.5025 0.0081 0.144 Uiso 0.50 1 calc PR B 2 H33E H 0.8143 0.4546 0.0488 0.144 Uiso 0.50 1 calc PR B 2 H33F H 0.7987 0.5488 0.0505 0.144 Uiso 0.50 1 calc PR B 2 C33C C 0.6414(10) 0.3919(7) 0.0170(4) 0.080(4) Uiso 0.50 1 d PD B 2 H33G H 0.6565 0.4000 -0.0115 0.120 Uiso 0.50 1 calc PR B 2 H33H H 0.5805 0.3812 0.0188 0.120 Uiso 0.50 1 calc PR B 2 H33I H 0.6733 0.3465 0.0282 0.120 Uiso 0.50 1 calc PR B 2 C34A C 0.5885(12) 0.6733(10) 0.1286(6) 0.083(6) Uiso 0.50 1 d PD B 2 H34A H 0.5986 0.7232 0.1435 0.124 Uiso 0.50 1 calc PR B 2 H34B H 0.5288 0.6579 0.1311 0.124 Uiso 0.50 1 calc PR B 2 H34C H 0.6017 0.6810 0.0999 0.124 Uiso 0.50 1 calc PR B 2 C34B C 0.7651(9) 0.6319(9) 0.1381(5) 0.095(5) Uiso 0.50 1 d PD B 2 H34D H 0.7750 0.6821 0.1526 0.143 Uiso 0.50 1 calc PR B 2 H34E H 0.7685 0.6411 0.1087 0.143 Uiso 0.50 1 calc PR B 2 H34F H 0.8082 0.5929 0.1464 0.143 Uiso 0.50 1 calc PR B 2 C34C C 0.6514(12) 0.5773(9) 0.2061(4) 0.106(5) Uiso 0.50 1 d PD B 2 H34G H 0.6611 0.6280 0.2202 0.159 Uiso 0.50 1 calc PR B 2 H34H H 0.6945 0.5387 0.2147 0.159 Uiso 0.50 1 calc PR B 2 H34I H 0.5950 0.5570 0.2127 0.159 Uiso 0.50 1 calc PR B 2 C35A C 0.4255(12) 0.5127(10) 0.0978(6) 0.070(6) Uiso 0.50 1 d PD B 2 H35A H 0.3655 0.4985 0.1001 0.105 Uiso 0.50 1 calc PR B 2 H35B H 0.4399 0.5174 0.0690 0.105 Uiso 0.50 1 calc PR B 2 H35C H 0.4360 0.5638 0.1114 0.105 Uiso 0.50 1 calc PR B 2 C35B C 0.4645(11) 0.4297(9) 0.1773(4) 0.093(5) Uiso 0.50 1 d PD B 2 H35D H 0.4052 0.4131 0.1799 0.140 Uiso 0.50 1 calc PR B 2 H35E H 0.4720 0.4827 0.1894 0.140 Uiso 0.50 1 calc PR B 2 H35F H 0.5015 0.3915 0.1915 0.140 Uiso 0.50 1 calc PR B 2 C35C C 0.4710(12) 0.3318(8) 0.1013(5) 0.109(5) Uiso 0.50 1 d PD B 2 H35G H 0.4112 0.3182 0.1053 0.163 Uiso 0.50 1 calc PR B 2 H35H H 0.5070 0.2928 0.1155 0.163 Uiso 0.50 1 calc PR B 2 H35I H 0.4833 0.3310 0.0722 0.163 Uiso 0.50 1 calc PR B 2 O100 O 0.6959(4) -0.0742(3) 0.12248(17) 0.1046(18) Uani 1 1 d D . . O200 O 0.5262(3) -0.0404(3) 0.16793(15) 0.0841(13) Uani 1 1 d D . . O300 O 0.6776(3) -0.1429(2) 0.21031(15) 0.0814(14) Uani 1 1 d D . . C100 C 0.6948(10) -0.0153(8) 0.0900(5) 0.120(6) Uiso 0.605(12) 1 d PD C 1 H10J H 0.6777 0.0375 0.1005 0.144 Uiso 0.605(12) 1 calc PR C 1 H10K H 0.6547 -0.0312 0.0680 0.144 Uiso 0.605(12) 1 calc PR C 1 C103 C 0.7636(12) -0.1307(9) 0.1122(6) 0.157(8) Uiso 0.605(12) 1 d PD C 1 H10L H 0.7846 -0.1600 0.1364 0.188 Uiso 0.605(12) 1 calc PR C 1 H10M H 0.7447 -0.1692 0.0911 0.188 Uiso 0.605(12) 1 calc PR C 1 C101 C 0.7815(12) -0.0127(13) 0.0751(7) 0.184(10) Uiso 0.605(12) 1 d PD C 1 H10N H 0.7823 -0.0224 0.0454 0.221 Uiso 0.605(12) 1 calc PR C 1 H10O H 0.8077 0.0398 0.0808 0.221 Uiso 0.605(12) 1 calc PR C 1 C102 C 0.8266(10) -0.0758(11) 0.0969(7) 0.174(9) Uiso 0.605(12) 1 d PD C 1 H10P H 0.8656 -0.1038 0.0784 0.209 Uiso 0.605(12) 1 calc PR C 1 H10Q H 0.8604 -0.0530 0.1197 0.209 Uiso 0.605(12) 1 calc PR C 1 C110 C 0.7629(15) -0.0238(13) 0.1101(7) 0.128(9) Uiso 0.395(12) 1 d PD C 2 H11J H 0.8127 -0.0279 0.1287 0.154 Uiso 0.395(12) 1 calc PR C 2 H11K H 0.7446 0.0326 0.1083 0.154 Uiso 0.395(12) 1 calc PR C 2 C112 C 0.7532(19) -0.1383(13) 0.0720(9) 0.160(12) Uiso 0.395(12) 1 d PD C 2 H11L H 0.8011 -0.1731 0.0804 0.192 Uiso 0.395(12) 1 calc PR C 2 H11M H 0.7321 -0.1562 0.0450 0.192 Uiso 0.395(12) 1 calc PR C 2 C113 C 0.6868(18) -0.1427(11) 0.1012(7) 0.135(10) Uiso 0.395(12) 1 d PD C 2 H11N H 0.6304 -0.1454 0.0876 0.162 Uiso 0.395(12) 1 calc PR C 2 H11O H 0.6940 -0.1897 0.1191 0.162 Uiso 0.395(12) 1 calc PR C 2 C111 C 0.781(3) -0.0571(18) 0.0699(9) 0.21(2) Uiso 0.395(12) 1 d PD C 2 H11P H 0.7489 -0.0279 0.0484 0.255 Uiso 0.395(12) 1 calc PR C 2 H11Q H 0.8420 -0.0541 0.0641 0.255 Uiso 0.395(12) 1 calc PR C 2 C200 C 0.4762(6) -0.0395(6) 0.1313(3) 0.127(3) Uani 1 1 d D C . H20J H 0.4567 -0.0941 0.1245 0.153 Uiso 1 1 calc R . . H20K H 0.5103 -0.0194 0.1084 0.153 Uiso 1 1 calc R . . C201 C 0.4039(7) 0.0121(8) 0.1377(3) 0.152(4) Uani 1 1 d D . . H20L H 0.4081 0.0604 0.1205 0.182 Uiso 1 1 calc R C . H20M H 0.3506 -0.0160 0.1305 0.182 Uiso 1 1 calc R . . C202 C 0.4047(7) 0.0336(7) 0.1800(4) 0.156(5) Uani 1 1 d D C . H20N H 0.3509 0.0173 0.1928 0.187 Uiso 1 1 calc R . . H20O H 0.4109 0.0920 0.1830 0.187 Uiso 1 1 calc R . . C203 C 0.4757(6) -0.0069(5) 0.1994(2) 0.109(3) Uani 1 1 d D C . H20P H 0.5097 0.0313 0.2158 0.131 Uiso 1 1 calc R . . H20Q H 0.4550 -0.0494 0.2176 0.131 Uiso 1 1 calc R . . C300 C 0.7627(6) -0.1446(5) 0.2239(4) 0.137(4) Uani 1 1 d D C . H30J H 0.7982 -0.1731 0.2041 0.164 Uiso 1 1 calc R . . H30K H 0.7848 -0.0896 0.2270 0.164 Uiso 1 1 calc R . . C301 C 0.7655(6) -0.1841(7) 0.2616(3) 0.151(4) Uani 1 1 d D . . H30L H 0.7762 -0.1451 0.2838 0.181 Uiso 1 1 calc R C . H30M H 0.8122 -0.2235 0.2620 0.181 Uiso 1 1 calc R . . C302 C 0.6862(6) -0.2235(5) 0.2678(2) 0.110(3) Uani 1 1 d D C . H30N H 0.6655 -0.2139 0.2956 0.132 Uiso 1 1 calc R . . H30O H 0.6917 -0.2816 0.2634 0.132 Uiso 1 1 calc R . . C303 C 0.6277(4) -0.1875(4) 0.2370(2) 0.084(2) Uani 1 1 d D C . H30P H 0.5968 -0.2298 0.2219 0.101 Uiso 1 1 calc R . . H30Q H 0.5858 -0.1527 0.2503 0.101 Uiso 1 1 calc R . . Li1 Li 0.6442(8) -0.0617(6) 0.1729(3) 0.070(3) Uiso 1 1 d . C . C500 C 0.688(3) 0.109(2) -0.0307(15) 0.29(2) Uiso 0.50(2) 1 d PD D 1 H50A H 0.7423 0.1114 -0.0445 0.431 Uiso 0.50(2) 1 calc PR D 1 H50B H 0.6539 0.0649 -0.0419 0.431 Uiso 0.50(2) 1 calc PR D 1 H50C H 0.6974 0.1005 -0.0015 0.431 Uiso 0.50(2) 1 calc PR D 1 C501 C 0.640(2) 0.187(2) -0.0373(12) 0.228(18) Uiso 0.50(2) 1 d PD D 1 H50D H 0.6262 0.1997 -0.0660 0.274 Uiso 0.50(2) 1 calc PR D 1 H50E H 0.6651 0.2337 -0.0229 0.274 Uiso 0.50(2) 1 calc PR D 1 C502 C 0.569(2) 0.145(2) -0.0141(10) 0.164(11) Uiso 0.50(2) 1 d PD D 1 H50F H 0.5864 0.1409 0.0149 0.196 Uiso 0.50(2) 1 calc PR D 1 H50G H 0.5639 0.0897 -0.0247 0.196 Uiso 0.50(2) 1 calc PR D 1 C503 C 0.475(2) 0.1861(19) -0.0164(10) 0.212(16) Uiso 0.50(2) 1 d PD D 1 H50H H 0.4494 0.1827 -0.0441 0.254 Uiso 0.50(2) 1 calc PR D 1 H50I H 0.4763 0.2424 -0.0075 0.254 Uiso 0.50(2) 1 calc PR D 1 C504 C 0.424(3) 0.128(2) 0.0168(11) 0.26(2) Uiso 0.50(2) 1 d PD D 1 H50J H 0.3655 0.1463 0.0196 0.385 Uiso 0.50(2) 1 calc PR D 1 H50K H 0.4531 0.1300 0.0433 0.385 Uiso 0.50(2) 1 calc PR D 1 H50L H 0.4238 0.0726 0.0068 0.385 Uiso 0.50(2) 1 calc PR D 1 C510 C 0.699(3) 0.160(3) -0.0389(13) 0.240(18) Uiso 0.50(2) 1 d PD D 2 H51A H 0.7475 0.1236 -0.0367 0.360 Uiso 0.50(2) 1 calc PR D 2 H51B H 0.7163 0.2128 -0.0283 0.360 Uiso 0.50(2) 1 calc PR D 2 H51C H 0.6817 0.1657 -0.0674 0.360 Uiso 0.50(2) 1 calc PR D 2 C511 C 0.626(3) 0.128(4) -0.014(3) 0.52(8) Uiso 0.50(2) 1 d PD D 2 H51D H 0.6403 0.1257 0.0152 0.627 Uiso 0.50(2) 1 calc PR D 2 H51E H 0.6078 0.0749 -0.0237 0.627 Uiso 0.50(2) 1 calc PR D 2 C512 C 0.557(3) 0.192(2) -0.0230(13) 0.25(2) Uiso 0.50(2) 1 d PD D 2 H51F H 0.5467 0.2034 -0.0521 0.304 Uiso 0.50(2) 1 calc PR D 2 H51G H 0.5612 0.2405 -0.0063 0.304 Uiso 0.50(2) 1 calc PR D 2 C513 C 0.498(2) 0.120(2) -0.0040(14) 0.27(2) Uiso 0.50(2) 1 d PD D 2 H51H H 0.5196 0.1009 0.0227 0.326 Uiso 0.50(2) 1 calc PR D 2 H51I H 0.4905 0.0746 -0.0229 0.326 Uiso 0.50(2) 1 calc PR D 2 C514 C 0.411(2) 0.176(2) -0.0002(14) 0.254(19) Uiso 0.50(2) 1 d PD D 2 H51J H 0.3643 0.1438 0.0103 0.381 Uiso 0.50(2) 1 calc PR D 2 H51K H 0.3949 0.1972 -0.0270 0.381 Uiso 0.50(2) 1 calc PR D 2 H51L H 0.4220 0.2207 0.0185 0.381 Uiso 0.50(2) 1 calc PR D 2 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 Mo1 0.0337(3) 0.0382(2) 0.0422(2) 0.00338(17) -0.00277(18) -0.00365(17) Ge1 0.0459(4) 0.0492(3) 0.0463(3) 0.0013(2) 0.0065(3) 0.0002(2) Ge2 0.0373(3) 0.0363(2) 0.0333(3) 0.00530(19) -0.0023(2) -0.0024(2) Ge3 0.0367(4) 0.0387(2) 0.0386(3) 0.0057(2) -0.0029(2) 0.0035(2) Ge4 0.0414(4) 0.0350(2) 0.0451(3) 0.0019(2) 0.0028(2) 0.0012(2) Ge6 0.0434(4) 0.0434(3) 0.0419(3) 0.0025(2) 0.0046(2) 0.0053(2) Ge9 0.0494(4) 0.0358(3) 0.0407(3) -0.0011(2) 0.0003(2) -0.0032(2) Ge7 0.0343(4) 0.0479(3) 0.0396(3) 0.0058(2) -0.0041(2) -0.0038(2) Ge5 0.0443(4) 0.0472(3) 0.0356(3) -0.0008(2) -0.0035(2) -0.0015(2) Ge8 0.0422(4) 0.0381(3) 0.0413(3) 0.0084(2) 0.0016(2) -0.0021(2) Si1 0.0435(10) 0.0489(8) 0.0406(8) 0.0005(6) 0.0072(6) 0.0022(6) Si2 0.0424(9) 0.0375(7) 0.0342(7) 0.0063(5) -0.0027(6) -0.0005(6) Si3 0.0386(10) 0.0493(8) 0.0448(8) 0.0119(6) 0.0015(6) 0.0098(6) Si10 0.0562(15) 0.0640(12) 0.0529(12) 0.0013(9) 0.0130(9) -0.0156(9) Si11 0.0680(17) 0.0898(15) 0.0385(11) -0.0039(9) -0.0026(9) -0.0035(11) Si12 0.0597(16) 0.0563(11) 0.0713(14) -0.0024(9) -0.0013(11) 0.0157(9) Si13 0.040(8) 0.121(10) 0.107(10) -0.040(8) 0.011(6) -0.007(6) Si14 0.112(11) 0.044(5) 0.059(7) -0.012(4) 0.025(6) 0.000(5) Si15 0.086(9) 0.072(6) 0.049(6) 0.013(5) 0.034(6) 0.009(6) Si20 0.0657(13) 0.0477(8) 0.0589(10) 0.0113(7) -0.0084(8) 0.0165(7) Si21 0.0609(13) 0.0797(11) 0.0479(10) 0.0140(8) 0.0074(8) -0.0198(9) Si22 0.0648(12) 0.0494(8) 0.0399(8) -0.0002(6) -0.0089(7) -0.0067(7) Si30 0.067(5) 0.102(6) 0.059(5) 0.042(4) 0.022(3) 0.026(4) Si31 0.065(4) 0.038(3) 0.068(3) 0.000(2) -0.015(3) 0.004(2) Si32 0.036(5) 0.058(3) 0.071(4) 0.006(3) -0.010(4) 0.006(2) Si33 0.075(5) 0.084(5) 0.041(3) 0.022(3) -0.001(3) 0.031(4) Si34 0.099(8) 0.043(4) 0.129(8) 0.012(4) -0.016(5) 0.010(4) Si35 0.041(3) 0.068(4) 0.108(8) 0.017(5) 0.008(6) 0.015(3) C1 0.039(4) 0.046(3) 0.052(3) 0.000(2) 0.000(2) -0.008(2) C2 0.042(4) 0.048(3) 0.092(5) 0.000(3) 0.012(3) -0.007(3) C3 0.075(5) 0.072(4) 0.067(4) 0.013(3) -0.026(4) -0.026(3) O1 0.070(3) 0.038(2) 0.084(3) 0.0117(18) 0.001(2) -0.0103(18) O2 0.058(4) 0.079(3) 0.168(5) -0.008(3) 0.051(3) -0.012(2) O3 0.110(5) 0.122(4) 0.086(4) 0.011(3) -0.052(3) -0.053(3) C10C 0.116(7) 0.105(5) 0.077(5) -0.015(4) 0.007(5) -0.051(5) C10B 0.070(7) 0.163(8) 0.109(7) -0.005(5) 0.025(5) -0.037(5) C10A 0.138(9) 0.069(5) 0.156(8) 0.039(5) 0.069(7) 0.012(5) C11B 0.106(7) 0.142(7) 0.065(5) 0.025(4) -0.013(4) 0.014(5) C11A 0.100(8) 0.360(16) 0.037(4) -0.023(7) 0.012(4) 0.002(9) C11C 0.190(12) 0.147(8) 0.114(8) -0.027(6) -0.064(7) -0.048(7) C12B 0.136(9) 0.113(6) 0.114(7) 0.009(5) -0.058(6) 0.039(6) C12A 0.131(8) 0.046(4) 0.135(7) 0.016(4) 0.008(6) 0.011(4) C12C 0.167(12) 0.156(9) 0.206(12) 0.025(8) 0.097(10) 0.093(8) C20C 0.101(7) 0.100(5) 0.083(5) 0.018(4) -0.022(4) 0.046(4) C20B 0.088(7) 0.111(6) 0.136(7) 0.043(5) 0.033(5) 0.054(5) C20A 0.131(8) 0.044(3) 0.143(8) -0.007(4) -0.027(6) 0.018(4) C21C 0.100(7) 0.134(6) 0.055(4) 0.029(4) 0.001(4) -0.027(5) C21B 0.149(10) 0.193(9) 0.084(6) -0.009(6) 0.015(6) -0.119(8) C21A 0.077(7) 0.168(8) 0.142(8) 0.047(6) 0.055(6) 0.030(6) C22C 0.153(8) 0.070(4) 0.053(4) 0.006(3) -0.020(4) -0.028(4) C22B 0.161(9) 0.069(4) 0.091(6) -0.029(4) -0.041(5) 0.033(5) C22A 0.116(8) 0.141(7) 0.090(6) -0.037(5) 0.017(5) -0.081(6) O100 0.117(5) 0.083(3) 0.115(4) -0.010(3) 0.046(4) -0.001(3) O200 0.063(4) 0.105(3) 0.084(4) -0.009(3) 0.002(3) -0.004(3) O300 0.060(4) 0.060(2) 0.124(4) 0.030(2) -0.006(3) -0.017(2) C200 0.080(8) 0.203(10) 0.099(7) -0.015(6) -0.007(6) -0.024(7) C201 0.081(9) 0.231(13) 0.144(11) 0.042(9) -0.014(7) 0.007(8) C202 0.096(10) 0.184(11) 0.185(13) -0.054(9) -0.047(8) 0.027(7) C203 0.078(7) 0.144(7) 0.105(7) -0.012(6) 0.007(5) -0.005(5) C300 0.077(8) 0.100(6) 0.232(13) 0.059(7) -0.016(7) -0.018(5) C301 0.108(10) 0.217(12) 0.127(9) 0.058(8) -0.043(7) -0.036(8) C302 0.113(8) 0.132(7) 0.084(6) 0.023(5) 0.005(5) 0.005(6) C303 0.078(6) 0.097(5) 0.079(5) 0.019(4) 0.008(4) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.923(5) . ? Mo1 C2 1.958(6) . ? Mo1 C3 1.965(6) . ? Mo1 Ge5 2.7293(7) . ? Mo1 Ge4 2.7383(7) . ? Mo1 Ge6 2.7415(6) . ? Mo1 Ge2 2.7907(7) . ? Mo1 Ge3 2.8210(6) . ? Ge1 Si1 2.3609(15) . ? Ge1 Ge8 2.4946(7) . ? Ge1 Ge7 2.5098(8) . ? Ge1 Ge4 2.5275(7) . ? Ge1 Ge5 2.5289(8) . ? Ge2 Si2 2.3958(13) . ? Ge2 Ge6 2.5349(7) . ? Ge2 Ge4 2.5671(7) . ? Ge2 Ge7 2.5874(8) . ? Ge2 Ge9 2.7152(7) . ? Ge3 Si3 2.3961(14) . ? Ge3 Ge6 2.5320(7) . ? Ge3 Ge5 2.5691(7) . ? Ge3 Ge8 2.5884(8) . ? Ge3 Ge9 2.7179(8) . ? Ge4 Ge5 2.8085(7) . ? Ge6 Ge9 2.7179(8) . ? Ge9 Ge8 2.5784(8) . ? Ge9 Ge7 2.5926(8) . ? Ge7 Ge8 2.8095(7) . ? Si1 Si13 2.252(10) . ? Si1 Si11 2.311(2) . ? Si1 Si12 2.340(2) . ? Si1 Si10 2.376(2) . ? Si1 Si15 2.399(9) . ? Si1 Si14 2.431(8) . ? Si2 Si22 2.3422(19) . ? Si2 Si20 2.343(2) . ? Si2 Si21 2.347(2) . ? Si3 Si32 2.315(16) . ? Si3 Si31 2.332(13) . ? Si3 Si33 2.344(11) . ? Si3 Si30 2.346(11) . ? Si3 Si34 2.351(16) . ? Si3 Si35 2.356(17) . ? Si10 C10C 1.824(7) . ? Si10 C10B 1.874(8) . ? Si10 C10A 1.911(8) . ? Si11 C11B 1.880(8) . ? Si11 C11A 1.884(8) . ? Si11 C11C 1.928(8) . ? Si12 C12C 1.877(9) . ? Si12 C12B 1.878(8) . ? Si12 C12A 1.903(7) . ? Si20 C20B 1.842(8) . ? Si20 C20C 1.855(7) . ? Si20 C20A 1.872(7) . ? Si21 C21B 1.848(7) . ? Si21 C21C 1.865(7) . ? Si21 C21A 1.869(8) . ? Si22 C22A 1.849(8) . ? Si22 C22B 1.855(7) . ? Si22 C22C 1.863(6) . ? Si30 C30C 1.826(12) . ? Si30 C30A 1.835(11) . ? Si30 C30B 1.847(13) . ? Si31 C31A 1.838(11) . ? Si31 C31B 1.859(12) . ? Si31 C31C 1.880(12) . ? Si32 C32A 1.857(11) . ? Si32 C32B 1.859(12) . ? Si32 C32C 1.865(12) . ? Si33 C33C 1.829(11) . ? Si33 C33B 1.845(12) . ? Si33 C33A 1.852(10) . ? Si34 C34C 1.852(12) . ? Si34 C34B 1.864(13) . ? Si34 C34A 1.872(12) . ? Si35 C35C 1.869(12) . ? Si35 C35B 1.874(12) . ? Si35 C35A 1.874(12) . ? C1 O1 1.168(5) . ? C2 O2 1.157(7) . ? C3 O3 1.145(7) . ? O1 Li1 1.985(11) . ? O100 C113 1.353(15) . ? O100 C110 1.417(15) . ? O100 C100 1.454(12) . ? O100 C103 1.471(13) . ? O100 Li1 1.868(12) . ? O200 C203 1.431(8) . ? O200 C200 1.431(8) . ? O200 Li1 1.899(13) . ? O300 C303 1.402(7) . ? O300 C300 1.410(9) . ? O300 Li1 1.906(11) . ? C100 C101 1.460(14) . ? C103 C102 1.452(14) . ? C101 C102 1.457(14) . ? C110 C111 1.466(16) . ? C112 C111 1.432(15) . ? C112 C113 1.433(15) . ? C200 C201 1.451(10) . ? C201 C202 1.437(10) . ? C202 C203 1.449(10) . ? C300 C301 1.406(10) . ? C301 C302 1.432(9) . ? C302 C303 1.488(9) . ? C500 C501 1.53(3) . ? C501 C502 1.54(3) . ? C502 C503 1.64(2) . ? C503 C504 1.68(2) . ? C510 C511 1.53(3) . ? C511 C512 1.54(3) . ? C512 C513 1.65(2) . ? C513 C514 1.68(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo1 C2 85.1(2) . . ? C1 Mo1 C3 86.9(2) . . ? C2 Mo1 C3 84.2(3) . . ? C1 Mo1 Ge5 117.26(16) . . ? C2 Mo1 Ge5 147.35(19) . . ? C3 Mo1 Ge5 74.3(2) . . ? C1 Mo1 Ge4 73.43(16) . . ? C2 Mo1 Ge4 150.82(19) . . ? C3 Mo1 Ge4 113.4(2) . . ? Ge5 Mo1 Ge4 61.816(19) . . ? C1 Mo1 Ge6 127.64(15) . . ? C2 Mo1 Ge6 70.35(16) . . ? C3 Mo1 Ge6 132.9(2) . . ? Ge5 Mo1 Ge6 107.02(2) . . ? Ge4 Mo1 Ge6 107.39(2) . . ? C1 Mo1 Ge2 94.66(15) . . ? C2 Mo1 Ge2 108.58(19) . . ? C3 Mo1 Ge2 167.2(2) . . ? Ge5 Mo1 Ge2 93.75(2) . . ? Ge4 Mo1 Ge2 55.320(18) . . ? Ge6 Mo1 Ge2 54.534(17) . . ? C1 Mo1 Ge3 166.78(16) . . ? C2 Mo1 Ge3 106.63(15) . . ? C3 Mo1 Ge3 100.03(17) . . ? Ge5 Mo1 Ge3 55.114(16) . . ? Ge4 Mo1 Ge3 93.43(2) . . ? Ge6 Mo1 Ge3 54.131(17) . . ? Ge2 Mo1 Ge3 76.086(17) . . ? Si1 Ge1 Ge8 116.69(4) . . ? Si1 Ge1 Ge7 120.39(4) . . ? Ge8 Ge1 Ge7 68.31(2) . . ? Si1 Ge1 Ge4 129.33(4) . . ? Ge8 Ge1 Ge4 113.93(3) . . ? Ge7 Ge1 Ge4 76.77(2) . . ? Si1 Ge1 Ge5 125.53(4) . . ? Ge8 Ge1 Ge5 77.92(2) . . ? Ge7 Ge1 Ge5 113.79(3) . . ? Ge4 Ge1 Ge5 67.48(2) . . ? Si2 Ge2 Ge6 111.08(4) . . ? Si2 Ge2 Ge4 119.81(4) . . ? Ge6 Ge2 Ge4 119.88(3) . . ? Si2 Ge2 Ge7 107.18(4) . . ? Ge6 Ge2 Ge7 118.84(2) . . ? Ge4 Ge2 Ge7 74.72(2) . . ? Si2 Ge2 Ge9 116.42(4) . . ? Ge6 Ge2 Ge9 62.24(2) . . ? Ge4 Ge2 Ge9 114.39(2) . . ? Ge7 Ge2 Ge9 58.480(19) . . ? Si2 Ge2 Mo1 131.13(4) . . ? Ge6 Ge2 Mo1 61.745(19) . . ? Ge4 Ge2 Mo1 61.305(19) . . ? Ge7 Ge2 Mo1 118.33(2) . . ? Ge9 Ge2 Mo1 102.44(2) . . ? Si3 Ge3 Ge6 113.10(4) . . ? Si3 Ge3 Ge5 119.25(4) . . ? Ge6 Ge3 Ge5 119.13(2) . . ? Si3 Ge3 Ge8 105.09(4) . . ? Ge6 Ge3 Ge8 118.44(3) . . ? Ge5 Ge3 Ge8 75.54(2) . . ? Si3 Ge3 Ge9 115.96(4) . . ? Ge6 Ge3 Ge9 62.24(2) . . ? Ge5 Ge3 Ge9 114.42(3) . . ? Ge8 Ge3 Ge9 58.08(2) . . ? Si3 Ge3 Mo1 133.79(4) . . ? Ge6 Ge3 Mo1 61.332(17) . . ? Ge5 Ge3 Mo1 60.629(18) . . ? Ge8 Ge3 Mo1 117.67(2) . . ? Ge9 Ge3 Mo1 101.58(2) . . ? Ge1 Ge4 Ge2 96.82(2) . . ? Ge1 Ge4 Mo1 107.97(2) . . ? Ge2 Ge4 Mo1 63.37(2) . . ? Ge1 Ge4 Ge5 56.28(2) . . ? Ge2 Ge4 Ge5 96.99(2) . . ? Mo1 Ge4 Ge5 58.935(19) . . ? Ge3 Ge6 Ge2 86.08(2) . . ? Ge3 Ge6 Ge9 62.24(2) . . ? Ge2 Ge6 Ge9 62.13(2) . . ? Ge3 Ge6 Mo1 64.537(18) . . ? Ge2 Ge6 Mo1 63.720(19) . . ? Ge9 Ge6 Mo1 103.66(2) . . ? Ge8 Ge9 Ge7 65.82(2) . . ? Ge8 Ge9 Ge2 99.59(2) . . ? Ge7 Ge9 Ge2 58.294(19) . . ? Ge8 Ge9 Ge3 58.44(2) . . ? Ge7 Ge9 Ge3 99.66(2) . . ? Ge2 Ge9 Ge3 79.066(19) . . ? Ge8 Ge9 Ge6 112.30(3) . . ? Ge7 Ge9 Ge6 112.26(2) . . ? Ge2 Ge9 Ge6 55.623(18) . . ? Ge3 Ge9 Ge6 55.525(19) . . ? Ge1 Ge7 Ge2 96.74(2) . . ? Ge1 Ge7 Ge9 104.86(3) . . ? Ge2 Ge7 Ge9 63.23(2) . . ? Ge1 Ge7 Ge8 55.590(19) . . ? Ge2 Ge7 Ge8 96.97(2) . . ? Ge9 Ge7 Ge8 56.848(19) . . ? Ge1 Ge5 Ge3 96.39(2) . . ? Ge1 Ge5 Mo1 108.20(2) . . ? Ge3 Ge5 Mo1 64.256(19) . . ? Ge1 Ge5 Ge4 56.23(2) . . ? Ge3 Ge5 Ge4 97.54(2) . . ? Mo1 Ge5 Ge4 59.249(18) . . ? Ge1 Ge8 Ge9 105.73(2) . . ? Ge1 Ge8 Ge3 96.76(2) . . ? Ge9 Ge8 Ge3 63.47(2) . . ? Ge1 Ge8 Ge7 56.104(19) . . ? Ge9 Ge8 Ge7 57.333(19) . . ? Ge3 Ge8 Ge7 97.43(2) . . ? Si13 Si1 Si11 136.5(3) . . ? Si13 Si1 Si12 62.7(4) . . ? Si11 Si1 Si12 112.30(9) . . ? Si13 Si1 Ge1 113.4(3) . . ? Si11 Si1 Ge1 109.30(9) . . ? Si12 Si1 Ge1 106.53(8) . . ? Si13 Si1 Si10 48.3(4) . . ? Si11 Si1 Si10 110.51(9) . . ? Si12 Si1 Si10 110.29(10) . . ? Ge1 Si1 Si10 107.73(7) . . ? Si13 Si1 Si15 115.0(5) . . ? Si11 Si1 Si15 41.0(3) . . ? Si12 Si1 Si15 142.8(2) . . ? Ge1 Si1 Si15 107.5(3) . . ? Si10 Si1 Si15 72.6(3) . . ? Si13 Si1 Si14 110.9(5) . . ? Si11 Si1 Si14 64.1(3) . . ? Si12 Si1 Si14 52.1(3) . . ? Ge1 Si1 Si14 104.8(3) . . ? Si10 Si1 Si14 146.6(3) . . ? Si15 Si1 Si14 104.3(4) . . ? Si22 Si2 Si20 110.96(8) . . ? Si22 Si2 Si21 107.42(8) . . ? Si20 Si2 Si21 109.31(8) . . ? Si22 Si2 Ge2 108.98(6) . . ? Si20 Si2 Ge2 109.61(7) . . ? Si21 Si2 Ge2 110.55(7) . . ? Si32 Si3 Si31 110.7(4) . . ? Si32 Si3 Si33 98.9(3) . . ? Si31 Si3 Si33 119.3(3) . . ? Si32 Si3 Si30 109.9(3) . . ? Si31 Si3 Si30 105.6(4) . . ? Si33 Si3 Si30 14.5(3) . . ? Si32 Si3 Si34 118.6(4) . . ? Si31 Si3 Si34 8.7(6) . . ? Si33 Si3 Si34 112.7(4) . . ? Si30 Si3 Si34 98.6(4) . . ? Si32 Si3 Si35 11.2(4) . . ? Si31 Si3 Si35 101.1(4) . . ? Si33 Si3 Si35 109.3(3) . . ? Si30 Si3 Si35 119.4(4) . . ? Si34 Si3 Si35 109.4(4) . . ? Si32 Si3 Ge3 107.5(3) . . ? Si31 Si3 Ge3 110.3(3) . . ? Si33 Si3 Ge3 109.2(2) . . ? Si30 Si3 Ge3 112.8(2) . . ? Si34 Si3 Ge3 109.3(3) . . ? Si35 Si3 Ge3 106.8(3) . . ? C10C Si10 C10B 105.6(4) . . ? C10C Si10 C10A 112.7(4) . . ? C10B Si10 C10A 111.1(4) . . ? C10C Si10 Si1 112.0(2) . . ? C10B Si10 Si1 107.1(3) . . ? C10A Si10 Si1 108.2(3) . . ? C11B Si11 C11A 105.4(4) . . ? C11B Si11 C11C 109.4(5) . . ? C11A Si11 C11C 113.3(5) . . ? C11B Si11 Si1 111.8(3) . . ? C11A Si11 Si1 108.2(3) . . ? C11C Si11 Si1 108.8(3) . . ? C12C Si12 C12B 111.6(5) . . ? C12C Si12 C12A 105.8(5) . . ? C12B Si12 C12A 113.4(4) . . ? C12C Si12 Si1 109.8(3) . . ? C12B Si12 Si1 108.6(2) . . ? C12A Si12 Si1 107.6(3) . . ? C20B Si20 C20C 109.0(4) . . ? C20B Si20 C20A 108.3(4) . . ? C20C Si20 C20A 109.0(4) . . ? C20B Si20 Si2 111.8(2) . . ? C20C Si20 Si2 109.6(2) . . ? C20A Si20 Si2 109.1(3) . . ? C21B Si21 C21C 109.1(4) . . ? C21B Si21 C21A 108.6(5) . . ? C21C Si21 C21A 106.7(4) . . ? C21B Si21 Si2 111.9(3) . . ? C21C Si21 Si2 109.5(3) . . ? C21A Si21 Si2 110.8(3) . . ? C22A Si22 C22B 108.5(4) . . ? C22A Si22 C22C 106.8(4) . . ? C22B Si22 C22C 108.8(3) . . ? C22A Si22 Si2 111.7(2) . . ? C22B Si22 Si2 110.9(2) . . ? C22C Si22 Si2 110.0(2) . . ? C30C Si30 C30A 115.2(10) . . ? C30C Si30 C30B 104.7(10) . . ? C30A Si30 C30B 103.4(9) . . ? C30C Si30 Si3 110.9(7) . . ? C30A Si30 Si3 109.1(7) . . ? C30B Si30 Si3 113.3(8) . . ? C31A Si31 C31B 112.0(11) . . ? C31A Si31 C31C 99.3(10) . . ? C31B Si31 C31C 108.4(8) . . ? C31A Si31 Si3 112.3(8) . . ? C31B Si31 Si3 114.1(8) . . ? C31C Si31 Si3 109.7(7) . . ? C32A Si32 C32B 105.9(10) . . ? C32A Si32 C32C 103.9(9) . . ? C32B Si32 C32C 109.2(9) . . ? C32A Si32 Si3 115.9(8) . . ? C32B Si32 Si3 112.4(8) . . ? C32C Si32 Si3 109.1(8) . . ? C33C Si33 C33B 104.9(8) . . ? C33C Si33 C33A 102.7(8) . . ? C33B Si33 C33A 111.0(8) . . ? C33C Si33 Si3 114.0(6) . . ? C33B Si33 Si3 112.9(7) . . ? C33A Si33 Si3 110.8(7) . . ? C34C Si34 C34B 109.1(10) . . ? C34C Si34 C34A 116.2(12) . . ? C34B Si34 C34A 101.0(10) . . ? C34C Si34 Si3 110.6(8) . . ? C34B Si34 Si3 109.0(8) . . ? C34A Si34 Si3 110.4(9) . . ? C35C Si35 C35B 106.3(10) . . ? C35C Si35 C35A 113.1(11) . . ? C35B Si35 C35A 107.3(10) . . ? C35C Si35 Si3 112.9(8) . . ? C35B Si35 Si3 109.9(8) . . ? C35A Si35 Si3 107.2(9) . . ? O1 C1 Mo1 178.3(5) . . ? O2 C2 Mo1 174.6(5) . . ? O3 C3 Mo1 177.1(5) . . ? C1 O1 Li1 132.3(5) . . ? C113 O100 C110 115.7(14) . . ? C113 O100 C100 101.4(14) . . ? C110 O100 C100 52.1(12) . . ? C113 O100 C103 53.5(13) . . ? C110 O100 C103 76.9(13) . . ? C100 O100 C103 105.7(10) . . ? C113 O100 Li1 120.6(11) . . ? C110 O100 Li1 121.6(10) . . ? C100 O100 Li1 125.0(7) . . ? C103 O100 Li1 127.1(9) . . ? C203 O200 C200 107.4(7) . . ? C203 O200 Li1 124.6(6) . . ? C200 O200 Li1 126.9(6) . . ? C303 O300 C300 109.3(6) . . ? C303 O300 Li1 129.3(6) . . ? C300 O300 Li1 118.2(5) . . ? O100 C100 C101 105.4(10) . . ? C102 C103 O100 100.0(11) . . ? C102 C101 C100 105.4(10) . . ? C103 C102 C101 107.4(10) . . ? O100 C110 C111 100.6(14) . . ? C111 C112 C113 107.8(13) . . ? O100 C113 C112 103.2(13) . . ? C112 C111 C110 104.9(13) . . ? O200 C200 C201 107.9(7) . . ? C202 C201 C200 107.2(7) . . ? C201 C202 C203 107.7(7) . . ? O200 C203 C202 107.5(7) . . ? C301 C300 O300 107.9(6) . . ? C300 C301 C302 109.0(6) . . ? C301 C302 C303 104.5(6) . . ? O300 C303 C302 107.2(6) . . ? O100 Li1 O200 112.6(6) . . ? O100 Li1 O300 111.9(6) . . ? O200 Li1 O300 116.8(6) . . ? O100 Li1 O1 106.3(6) . . ? O200 Li1 O1 105.2(5) . . ? O300 Li1 O1 102.7(5) . . ? C500 C501 C502 84(3) . . ? C501 C502 C503 116(3) . . ? C502 C503 C504 99(3) . . ? C510 C511 C512 101(5) . . ? C511 C512 C513 80(3) . . ? C512 C513 C514 95(3) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.615 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.082 data_fh81tet _database_code_depnum_ccdc_archive 'CCDC 807923' #TrackingRef '- FH81tet(CCDC-807923).pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.50 H119 Ge9 Li N4 O3 Si12 W' _chemical_formula_weight 1939.62 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' N N 0.0061 0.0033 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 25.736(4) _cell_length_b 25.736(4) _cell_length_c 26.755(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17721(5) _cell_formula_units_Z 8 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 46994 _cell_measurement_theta_min 1.12 _cell_measurement_theta_max 25.14 _exptl_crystal_description diamond _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7768 _exptl_absorpt_coefficient_mu 4.492 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1598 _exptl_absorpt_correction_T_max 0.3209 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 149(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 106832 _diffrn_reflns_av_R_equivalents 0.1474 _diffrn_reflns_av_sigmaI/netI 0.1006 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.72 _reflns_number_total 14978 _reflns_number_gt 10377 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A Si(SiMe3)3 group is disordered over two positions and refined applying a split model. During refinement SADI restrains are used to obtain a similar arrangement of both split positions. ; _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^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(8) _refine_ls_number_reflns 14978 _refine_ls_number_parameters 664 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _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 W1 W 0.313239(14) 0.393640(13) 0.150057(17) 0.04178(9) Uani 1 1 d . . . Ge2 Ge 0.21108(3) 0.35624(3) 0.15656(4) 0.0430(3) Uani 1 1 d . . . Ge1 Ge 0.28862(4) 0.23050(4) 0.15739(5) 0.0573(3) Uani 1 1 d . . . Ge3 Ge 0.30901(4) 0.34496(3) 0.24457(4) 0.0438(2) Uani 1 1 d . . . Ge4 Ge 0.27695(4) 0.30813(4) 0.10050(4) 0.0461(3) Uani 1 1 d . . . Ge6 Ge 0.24364(4) 0.41684(4) 0.22482(4) 0.0434(3) Uani 1 1 d . . . Ge5 Ge 0.35682(4) 0.29984(4) 0.17214(4) 0.0474(3) Uani 1 1 d . . . Ge7 Ge 0.19767(4) 0.25873(4) 0.17762(4) 0.0512(3) Uani 1 1 d . . . Ge9 Ge 0.20699(4) 0.32153(4) 0.25286(4) 0.0487(3) Uani 1 1 d . . . Ge8 Ge 0.27702(4) 0.24949(4) 0.24865(5) 0.0518(3) Uani 1 1 d . . . Si2 Si 0.13006(10) 0.38597(10) 0.12209(11) 0.0457(7) Uani 1 1 d . . . Si1 Si 0.30762(13) 0.14505(10) 0.12878(12) 0.0549(8) Uani 1 1 d . . . Si3 Si 0.35291(11) 0.36145(11) 0.32188(12) 0.0527(7) Uani 1 1 d . A . Si10 Si 0.13988(12) 0.47053(13) 0.08996(15) 0.0687(10) Uani 1 1 d . . . Si11 Si 0.06541(11) 0.38794(13) 0.18481(14) 0.0623(9) Uani 1 1 d . . . Si12 Si 0.10341(14) 0.33118(15) 0.05671(15) 0.0820(11) Uani 1 1 d . . . Si20 Si 0.38317(17) 0.15121(13) 0.08019(17) 0.0933(14) Uani 1 1 d . . . Si21 Si 0.23728(18) 0.12026(13) 0.07932(17) 0.0943(14) Uani 1 1 d . . . Si22 Si 0.32350(12) 0.09271(11) 0.19839(13) 0.0610(9) Uani 1 1 d . . . Si30 Si 0.41296(16) 0.29638(16) 0.34124(15) 0.0974(13) Uani 1 1 d D . . Si31 Si 0.39546(14) 0.44177(14) 0.31526(15) 0.0794(10) Uani 1 1 d D . . Si32 Si 0.29053(13) 0.36647(12) 0.38607(12) 0.0641(9) Uani 1 1 d . . . O1 O 0.3188(3) 0.5121(3) 0.1754(3) 0.082(3) Uani 1 1 d . . . O2 O 0.4329(3) 0.4058(3) 0.1366(4) 0.100(3) Uani 1 1 d . . . O3 O 0.3025(3) 0.4303(3) 0.0396(3) 0.080(3) Uani 1 1 d . . . C1 C 0.3146(4) 0.4663(4) 0.1666(4) 0.063(3) Uani 1 1 d . . . C2 C 0.3866(5) 0.4001(4) 0.1414(4) 0.070(3) Uani 1 1 d . . . C3 C 0.3063(4) 0.4144(4) 0.0832(5) 0.064(3) Uani 1 1 d . . . C10C C 0.1765(6) 0.5123(4) 0.1320(7) 0.134(7) Uani 1 1 d . . . H10A H 0.1798 0.5470 0.1171 0.200 Uiso 1 1 calc R . . H10B H 0.2111 0.4976 0.1373 0.200 Uiso 1 1 calc R . . H10C H 0.1583 0.5150 0.1640 0.200 Uiso 1 1 calc R . . C10B C 0.0760(5) 0.4990(5) 0.0768(6) 0.090(4) Uani 1 1 d . . . H10D H 0.0805 0.5341 0.0634 0.134 Uiso 1 1 calc R . . H10E H 0.0557 0.5006 0.1077 0.134 Uiso 1 1 calc R . . H10F H 0.0577 0.4775 0.0523 0.134 Uiso 1 1 calc R . . C10A C 0.1741(6) 0.4693(7) 0.0283(7) 0.139(7) Uani 1 1 d . . . H10G H 0.1778 0.5048 0.0157 0.208 Uiso 1 1 calc R . . H10H H 0.1539 0.4486 0.0045 0.208 Uiso 1 1 calc R . . H10I H 0.2086 0.4537 0.0325 0.208 Uiso 1 1 calc R . . C11C C 0.0777(6) 0.4422(6) 0.2282(7) 0.141(7) Uani 1 1 d . . . H11A H 0.0508 0.4427 0.2540 0.211 Uiso 1 1 calc R . . H11B H 0.0771 0.4751 0.2097 0.211 Uiso 1 1 calc R . . H11C H 0.1118 0.4377 0.2438 0.211 Uiso 1 1 calc R . . C11B C 0.0624(4) 0.3295(5) 0.2229(6) 0.108(5) Uani 1 1 d . . . H11D H 0.0350 0.3332 0.2481 0.162 Uiso 1 1 calc R . . H11E H 0.0959 0.3242 0.2397 0.162 Uiso 1 1 calc R . . H11F H 0.0548 0.2995 0.2016 0.162 Uiso 1 1 calc R . . C11A C -0.0002(4) 0.3969(6) 0.1551(6) 0.111(5) Uani 1 1 d . . . H11G H -0.0270 0.3978 0.1812 0.167 Uiso 1 1 calc R . . H11H H -0.0072 0.3679 0.1323 0.167 Uiso 1 1 calc R . . H11I H -0.0007 0.4296 0.1364 0.167 Uiso 1 1 calc R . . C12B C 0.0474(5) 0.3585(6) 0.0231(5) 0.116(6) Uani 1 1 d . . . H12A H 0.0372 0.3348 -0.0039 0.174 Uiso 1 1 calc R . . H12B H 0.0570 0.3922 0.0088 0.174 Uiso 1 1 calc R . . H12C H 0.0183 0.3630 0.0463 0.174 Uiso 1 1 calc R . . C12A C 0.0841(6) 0.2668(5) 0.0839(6) 0.121(6) Uani 1 1 d . . . H12D H 0.0728 0.2436 0.0569 0.182 Uiso 1 1 calc R . . H12E H 0.0555 0.2719 0.1075 0.182 Uiso 1 1 calc R . . H12F H 0.1138 0.2515 0.1013 0.182 Uiso 1 1 calc R . . C12C C 0.1570(5) 0.3227(7) 0.0086(6) 0.130(7) Uani 1 1 d . . . H12G H 0.1449 0.2997 -0.0181 0.195 Uiso 1 1 calc R . . H12H H 0.1876 0.3074 0.0247 0.195 Uiso 1 1 calc R . . H12I H 0.1662 0.3567 -0.0055 0.195 Uiso 1 1 calc R . . C20C C 0.3850(6) 0.2098(5) 0.0413(6) 0.130(7) Uani 1 1 d . . . H20A H 0.4172 0.2103 0.0218 0.195 Uiso 1 1 calc R . . H20B H 0.3835 0.2407 0.0627 0.195 Uiso 1 1 calc R . . H20C H 0.3551 0.2098 0.0185 0.195 Uiso 1 1 calc R . . C20B C 0.3897(6) 0.0937(5) 0.0391(6) 0.116(6) Uani 1 1 d . . . H20D H 0.4214 0.0968 0.0190 0.174 Uiso 1 1 calc R . . H20E H 0.3595 0.0915 0.0168 0.174 Uiso 1 1 calc R . . H20F H 0.3916 0.0622 0.0596 0.174 Uiso 1 1 calc R . . C20A C 0.4423(5) 0.1543(5) 0.1208(6) 0.110(6) Uani 1 1 d . . . H20G H 0.4734 0.1568 0.0998 0.166 Uiso 1 1 calc R . . H20H H 0.4442 0.1228 0.1414 0.166 Uiso 1 1 calc R . . H20I H 0.4401 0.1848 0.1426 0.166 Uiso 1 1 calc R . . C21A C 0.1764(5) 0.1240(5) 0.1109(7) 0.138(8) Uani 1 1 d . . . H21A H 0.1485 0.1131 0.0882 0.206 Uiso 1 1 calc R . . H21B H 0.1701 0.1599 0.1216 0.206 Uiso 1 1 calc R . . H21C H 0.1769 0.1011 0.1402 0.206 Uiso 1 1 calc R . . C21C C 0.2446(6) 0.0531(5) 0.0559(6) 0.112(5) Uani 1 1 d . . . H21D H 0.2144 0.0440 0.0354 0.169 Uiso 1 1 calc R . . H21E H 0.2470 0.0291 0.0843 0.169 Uiso 1 1 calc R . . H21F H 0.2762 0.0506 0.0357 0.169 Uiso 1 1 calc R . . C21B C 0.2384(10) 0.1654(5) 0.0231(7) 0.205(12) Uani 1 1 d . . . H21G H 0.2094 0.1568 0.0008 0.307 Uiso 1 1 calc R . . H21H H 0.2713 0.1611 0.0051 0.307 Uiso 1 1 calc R . . H21I H 0.2351 0.2015 0.0344 0.307 Uiso 1 1 calc R . . C22A C 0.2662(5) 0.0867(5) 0.2365(5) 0.099(5) Uani 1 1 d . . . H22A H 0.2738 0.0647 0.2654 0.148 Uiso 1 1 calc R . . H22B H 0.2382 0.0710 0.2168 0.148 Uiso 1 1 calc R . . H22C H 0.2553 0.1212 0.2479 0.148 Uiso 1 1 calc R . . C22C C 0.3745(5) 0.1193(5) 0.2393(6) 0.097(5) Uani 1 1 d . . . H22D H 0.3797 0.0960 0.2678 0.146 Uiso 1 1 calc R . . H22E H 0.3640 0.1537 0.2513 0.146 Uiso 1 1 calc R . . H22F H 0.4071 0.1223 0.2204 0.146 Uiso 1 1 calc R . . C22B C 0.3440(5) 0.0276(4) 0.1757(6) 0.100(5) Uani 1 1 d . . . H22G H 0.3510 0.0049 0.2043 0.151 Uiso 1 1 calc R . . H22H H 0.3756 0.0311 0.1555 0.151 Uiso 1 1 calc R . . H22I H 0.3163 0.0125 0.1553 0.151 Uiso 1 1 calc R . . C30B C 0.4737(8) 0.3067(12) 0.3044(11) 0.109(10) Uiso 0.50 1 d PD A 1 H30A H 0.4989 0.2794 0.3126 0.164 Uiso 0.50 1 calc PR A 1 H30B H 0.4885 0.3407 0.3127 0.164 Uiso 0.50 1 calc PR A 1 H30C H 0.4657 0.3054 0.2686 0.164 Uiso 0.50 1 calc PR A 1 C30A C 0.3925(16) 0.2286(8) 0.3297(17) 0.164(17) Uiso 0.50 1 d PD A 1 H30D H 0.4207 0.2049 0.3389 0.246 Uiso 0.50 1 calc PR A 1 H30E H 0.3842 0.2242 0.2942 0.246 Uiso 0.50 1 calc PR A 1 H30F H 0.3617 0.2207 0.3499 0.246 Uiso 0.50 1 calc PR A 1 C30C C 0.4307(12) 0.2942(12) 0.4082(6) 0.103(11) Uiso 0.50 1 d PD A 1 H30G H 0.4557 0.2660 0.4138 0.154 Uiso 0.50 1 calc PR A 1 H30H H 0.3995 0.2879 0.4283 0.154 Uiso 0.50 1 calc PR A 1 H30I H 0.4463 0.3274 0.4180 0.154 Uiso 0.50 1 calc PR A 1 C31C C 0.3480(15) 0.4927(14) 0.2965(17) 0.14(2) Uiso 0.50 1 d PD A 1 H31A H 0.3658 0.5262 0.2937 0.207 Uiso 0.50 1 calc PR A 1 H31B H 0.3205 0.4952 0.3218 0.207 Uiso 0.50 1 calc PR A 1 H31C H 0.3326 0.4835 0.2642 0.207 Uiso 0.50 1 calc PR A 1 C31B C 0.4477(15) 0.4346(18) 0.2684(15) 0.19(2) Uiso 0.50 1 d PD A 1 H31D H 0.4660 0.4677 0.2646 0.290 Uiso 0.50 1 calc PR A 1 H31E H 0.4325 0.4245 0.2362 0.290 Uiso 0.50 1 calc PR A 1 H31F H 0.4722 0.4078 0.2794 0.290 Uiso 0.50 1 calc PR A 1 C31A C 0.4194(10) 0.4647(10) 0.3765(7) 0.089(8) Uiso 0.50 1 d PD A 1 H31G H 0.4370 0.4982 0.3723 0.133 Uiso 0.50 1 calc PR A 1 H31H H 0.4439 0.4393 0.3902 0.133 Uiso 0.50 1 calc PR A 1 H31I H 0.3901 0.4688 0.3995 0.133 Uiso 0.50 1 calc PR A 1 C30D C 0.3780(13) 0.2357(10) 0.3611(14) 0.126(12) Uiso 0.50 1 d PD A 2 H30J H 0.4034 0.2086 0.3691 0.188 Uiso 0.50 1 calc PR A 2 H30K H 0.3555 0.2238 0.3338 0.188 Uiso 0.50 1 calc PR A 2 H30L H 0.3568 0.2431 0.3907 0.188 Uiso 0.50 1 calc PR A 2 C30E C 0.4460(10) 0.2697(10) 0.2850(8) 0.100(9) Uiso 0.50 1 d PD A 2 H30M H 0.4706 0.2426 0.2952 0.150 Uiso 0.50 1 calc PR A 2 H30N H 0.4647 0.2976 0.2678 0.150 Uiso 0.50 1 calc PR A 2 H30O H 0.4201 0.2548 0.2623 0.150 Uiso 0.50 1 calc PR A 2 C30F C 0.4498(11) 0.3124(13) 0.3988(9) 0.104(11) Uiso 0.50 1 d PD A 2 H30P H 0.4746 0.2845 0.4060 0.157 Uiso 0.50 1 calc PR A 2 H30Q H 0.4256 0.3160 0.4269 0.157 Uiso 0.50 1 calc PR A 2 H30R H 0.4686 0.3451 0.3939 0.157 Uiso 0.50 1 calc PR A 2 C31D C 0.4474(9) 0.4436(11) 0.3637(9) 0.097(9) Uiso 0.50 1 d PD A 2 H31J H 0.4659 0.4768 0.3618 0.145 Uiso 0.50 1 calc PR A 2 H31K H 0.4718 0.4150 0.3580 0.145 Uiso 0.50 1 calc PR A 2 H31L H 0.4317 0.4399 0.3969 0.145 Uiso 0.50 1 calc PR A 2 C31E C 0.4338(8) 0.4500(9) 0.2565(7) 0.054(6) Uiso 0.50 1 d PD A 2 H31M H 0.4504 0.4843 0.2565 0.081 Uiso 0.50 1 calc PR A 2 H31N H 0.4106 0.4471 0.2276 0.081 Uiso 0.50 1 calc PR A 2 H31O H 0.4606 0.4230 0.2547 0.081 Uiso 0.50 1 calc PR A 2 C31F C 0.3475(10) 0.4965(9) 0.3137(13) 0.063(9) Uiso 0.50 1 d PD A 2 H31P H 0.3661 0.5296 0.3108 0.094 Uiso 0.50 1 calc PR A 2 H31Q H 0.3269 0.4964 0.3445 0.094 Uiso 0.50 1 calc PR A 2 H31R H 0.3244 0.4923 0.2848 0.094 Uiso 0.50 1 calc PR A 2 C32C C 0.2635(5) 0.3021(5) 0.3982(4) 0.086(4) Uani 1 1 d . A . H32A H 0.2375 0.3044 0.4249 0.129 Uiso 1 1 calc R . . H32B H 0.2914 0.2785 0.4085 0.129 Uiso 1 1 calc R . . H32C H 0.2471 0.2888 0.3677 0.129 Uiso 1 1 calc R . . C32B C 0.3202(6) 0.3924(6) 0.4430(4) 0.105(4) Uani 1 1 d . A . H32D H 0.2940 0.3944 0.4695 0.157 Uiso 1 1 calc R . . H32E H 0.3339 0.4273 0.4363 0.157 Uiso 1 1 calc R . . H32F H 0.3486 0.3696 0.4536 0.157 Uiso 1 1 calc R . . C32A C 0.2360(5) 0.4112(4) 0.3709(5) 0.085(4) Uani 1 1 d . A . H32G H 0.2112 0.4117 0.3987 0.127 Uiso 1 1 calc R . . H32H H 0.2184 0.3990 0.3405 0.127 Uiso 1 1 calc R . . H32I H 0.2496 0.4463 0.3653 0.127 Uiso 1 1 calc R . . C100 C 0.3032(6) 0.4256(7) -0.2034(5) 0.113(6) Uani 1 1 d . . . H10J H 0.3061 0.4451 -0.2352 0.136 Uiso 1 1 calc R . . H10K H 0.2771 0.3979 -0.2088 0.136 Uiso 1 1 calc R . . C101 C 0.2838(6) 0.4581(7) -0.1692(6) 0.125(7) Uani 1 1 d . . . H10L H 0.2468 0.4640 -0.1774 0.150 Uiso 1 1 calc R . . H10M H 0.3019 0.4918 -0.1730 0.150 Uiso 1 1 calc R . . C102 C 0.2416(5) 0.4165(6) -0.1017(8) 0.145(8) Uani 1 1 d . . . H10N H 0.2447 0.4066 -0.0664 0.218 Uiso 1 1 calc R . . H10O H 0.2375 0.3852 -0.1222 0.218 Uiso 1 1 calc R . . H10P H 0.2113 0.4391 -0.1060 0.218 Uiso 1 1 calc R . . C103 C 0.2898(5) 0.4893(6) -0.0861(6) 0.109(5) Uani 1 1 d . . . H10Q H 0.2915 0.4794 -0.0508 0.164 Uiso 1 1 calc R . . H10R H 0.2589 0.5108 -0.0918 0.164 Uiso 1 1 calc R . . H10S H 0.3209 0.5091 -0.0950 0.164 Uiso 1 1 calc R . . C104 C 0.3970(5) 0.4311(5) -0.2150(5) 0.094(4) Uani 1 1 d . . . H10T H 0.3982 0.4652 -0.1987 0.141 Uiso 1 1 calc R . . H10U H 0.3923 0.4356 -0.2511 0.141 Uiso 1 1 calc R . . H10V H 0.4295 0.4124 -0.2086 0.141 Uiso 1 1 calc R . . C105 C 0.3544(6) 0.3521(5) -0.2203(5) 0.107(5) Uani 1 1 d . . . H10W H 0.3880 0.3353 -0.2141 0.161 Uiso 1 1 calc R . . H10$ H 0.3501 0.3581 -0.2562 0.161 Uiso 1 1 calc R . . H10 H 0.3263 0.3296 -0.2082 0.161 Uiso 1 1 calc R . . C200 C 0.3925(9) 0.3379(9) -0.0355(9) 0.065(6) Uiso 0.50 1 d P B 1 H20J H 0.3733 0.3595 -0.0110 0.078 Uiso 0.50 1 calc PR B 1 H20K H 0.4046 0.3061 -0.0183 0.078 Uiso 0.50 1 calc PR B 1 C201 C 0.4386(8) 0.3679(7) -0.0556(9) 0.048(5) Uiso 0.50 1 d P B 1 H20L H 0.4644 0.3734 -0.0287 0.058 Uiso 0.50 1 calc PR B 1 H20M H 0.4555 0.3479 -0.0828 0.058 Uiso 0.50 1 calc PR B 1 C210 C 0.4112(8) 0.3182(9) -0.0632(9) 0.059(6) Uiso 0.50 1 d P B 2 H21J H 0.4351 0.3171 -0.0921 0.071 Uiso 0.50 1 calc PR B 2 H21K H 0.4166 0.2870 -0.0422 0.071 Uiso 0.50 1 calc PR B 2 C211 C 0.4178(11) 0.3672(9) -0.0336(9) 0.060(6) Uiso 0.50 1 d P B 2 H21L H 0.4500 0.3656 -0.0135 0.072 Uiso 0.50 1 calc PR B 2 H21M H 0.3880 0.3720 -0.0106 0.072 Uiso 0.50 1 calc PR B 2 C203 C 0.3624(6) 0.2790(5) -0.1104(6) 0.115(6) Uani 1 1 d . B . H20N H 0.3924 0.2844 -0.1324 0.173 Uiso 1 1 calc R . . H20O H 0.3311 0.2739 -0.1307 0.173 Uiso 1 1 calc R . . H20P H 0.3683 0.2483 -0.0896 0.173 Uiso 1 1 calc R . . C204 C 0.3130(5) 0.3157(5) -0.0460(5) 0.092(4) Uani 1 1 d . B . H20Q H 0.3101 0.3460 -0.0239 0.138 Uiso 1 1 calc R . . H20R H 0.3189 0.2844 -0.0258 0.138 Uiso 1 1 calc R . . H20S H 0.2809 0.3117 -0.0652 0.138 Uiso 1 1 calc R . . C205 C 0.4660(4) 0.4296(5) -0.1040(5) 0.096(5) Uani 1 1 d . B . H20T H 0.4724 0.4015 -0.1280 0.144 Uiso 1 1 calc R . . H20U H 0.4962 0.4335 -0.0821 0.144 Uiso 1 1 calc R . . H20V H 0.4600 0.4621 -0.1221 0.144 Uiso 1 1 calc R . . C206 C 0.4122(4) 0.4598(4) -0.0399(4) 0.064(3) Uani 1 1 d . B . H20W H 0.3814 0.4525 -0.0196 0.096 Uiso 1 1 calc R . . H20$ H 0.4070 0.4920 -0.0587 0.096 Uiso 1 1 calc R . . H20 H 0.4425 0.4635 -0.0180 0.096 Uiso 1 1 calc R . . C300 C 0.5000 0.0000 0.1160(10) 0.125(9) Uani 1 2 d S . . H30S H 0.4763 0.0197 0.1382 0.150 Uiso 0.50 1 calc PR . . H30T H 0.5237 -0.0197 0.1382 0.150 Uiso 0.50 1 calc PR . . C301 C 0.5323(10) 0.0388(8) 0.0904(10) 0.191(13) Uani 1 1 d . . . H30U H 0.5089 0.0592 0.0687 0.230 Uiso 1 1 calc R . . H30V H 0.5560 0.0194 0.0680 0.230 Uiso 1 1 calc R . . C302 C 0.5663(9) 0.0785(9) 0.1194(12) 0.213(14) Uani 1 1 d . . . H30W H 0.5849 0.1007 0.0956 0.320 Uiso 1 1 calc R . . H30$ H 0.5914 0.0598 0.1403 0.320 Uiso 1 1 calc R . . H30 H 0.5439 0.1000 0.1407 0.320 Uiso 1 1 calc R . . N1 N 0.2868(4) 0.4433(5) -0.1166(5) 0.081(3) Uani 1 1 d . . . N2 N 0.3526(3) 0.4006(3) -0.1945(3) 0.055(2) Uani 1 1 d . . . N3 N 0.3558(4) 0.3230(4) -0.0795(4) 0.073(3) Uani 1 1 d . . . N4 N 0.4208(3) 0.4173(3) -0.0744(4) 0.064(3) Uani 1 1 d . . . Li1 Li 0.3543(6) 0.3948(7) -0.1159(6) 0.049(4) Uani 1 1 d . B . 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 W1 0.0416(2) 0.0339(2) 0.0499(2) 0.0061(2) 0.0113(2) 0.00105(16) Ge2 0.0417(5) 0.0385(5) 0.0487(7) 0.0033(5) 0.0069(5) 0.0001(4) Ge1 0.0680(7) 0.0380(5) 0.0657(8) 0.0025(6) 0.0132(7) 0.0004(5) Ge3 0.0463(6) 0.0381(5) 0.0470(7) 0.0058(5) 0.0069(6) 0.0016(4) Ge4 0.0544(6) 0.0380(5) 0.0460(7) 0.0021(5) 0.0114(5) 0.0020(5) Ge6 0.0444(6) 0.0371(5) 0.0488(7) 0.0008(5) 0.0099(5) 0.0021(4) Ge5 0.0458(6) 0.0383(6) 0.0582(7) 0.0032(5) 0.0111(5) 0.0077(4) Ge7 0.0528(7) 0.0404(6) 0.0605(7) 0.0016(5) 0.0110(6) -0.0098(5) Ge9 0.0504(6) 0.0439(6) 0.0519(7) 0.0033(6) 0.0163(6) -0.0035(5) Ge8 0.0654(7) 0.0371(5) 0.0528(7) 0.0095(6) 0.0102(6) -0.0013(5) Si2 0.0377(14) 0.0494(16) 0.0501(19) -0.0010(14) 0.0035(13) 0.0018(12) Si1 0.080(2) 0.0302(14) 0.055(2) 0.0037(14) 0.0132(17) 0.0040(15) Si3 0.0562(17) 0.0557(17) 0.0464(18) 0.0034(15) 0.0003(15) 0.0101(14) Si10 0.0475(18) 0.066(2) 0.092(3) 0.028(2) 0.0012(19) 0.0058(16) Si11 0.0490(17) 0.068(2) 0.070(2) 0.0034(19) 0.0154(16) 0.0050(15) Si12 0.069(2) 0.096(3) 0.082(3) -0.030(2) -0.013(2) 0.000(2) Si20 0.123(3) 0.050(2) 0.107(3) 0.018(2) 0.056(3) 0.020(2) Si21 0.128(3) 0.055(2) 0.100(3) -0.009(2) -0.051(3) 0.005(2) Si22 0.067(2) 0.0457(18) 0.070(2) 0.0114(16) 0.0038(18) 0.0069(14) Si30 0.111(3) 0.114(3) 0.067(3) 0.004(3) -0.015(2) 0.064(2) Si31 0.076(2) 0.087(2) 0.075(3) 0.000(2) -0.006(2) -0.027(2) Si32 0.081(2) 0.0593(19) 0.052(2) -0.0008(16) 0.0105(18) -0.0004(16) O1 0.102(6) 0.039(4) 0.105(7) -0.011(4) 0.052(5) -0.014(4) O2 0.052(5) 0.075(5) 0.173(11) 0.031(6) 0.034(6) -0.009(4) O3 0.104(7) 0.070(5) 0.066(6) 0.010(5) 0.025(5) -0.008(5) C1 0.055(6) 0.071(7) 0.062(8) 0.019(6) 0.021(6) 0.010(6) C2 0.099(9) 0.048(6) 0.064(9) 0.019(6) 0.029(7) 0.004(6) C3 0.049(6) 0.050(6) 0.092(10) -0.006(7) 0.014(7) 0.000(5) C10C 0.139(13) 0.045(7) 0.22(2) 0.041(10) -0.067(13) -0.033(8) C10B 0.077(9) 0.084(9) 0.107(12) 0.015(8) 0.013(8) 0.026(7) C10A 0.097(12) 0.165(16) 0.154(17) 0.064(14) 0.047(11) 0.030(10) C11C 0.106(11) 0.175(16) 0.142(16) -0.095(13) 0.056(11) -0.020(11) C11B 0.065(8) 0.128(12) 0.130(14) 0.058(10) 0.052(8) 0.029(8) C11A 0.057(7) 0.173(14) 0.103(12) 0.065(12) 0.006(8) 0.019(8) C12B 0.104(11) 0.161(14) 0.083(11) -0.028(11) -0.038(9) 0.028(10) C12A 0.130(13) 0.080(10) 0.154(16) -0.012(10) -0.041(12) -0.022(9) C12C 0.085(10) 0.212(19) 0.092(12) -0.073(13) -0.002(9) -0.014(11) C20C 0.149(14) 0.081(10) 0.160(16) 0.043(10) 0.097(13) 0.033(9) C20B 0.159(14) 0.082(10) 0.108(13) 0.006(9) 0.062(12) 0.018(9) C20A 0.069(9) 0.075(9) 0.187(18) 0.034(10) 0.048(10) 0.003(7) C21A 0.076(10) 0.074(9) 0.26(2) -0.063(11) -0.074(12) 0.002(7) C21C 0.152(14) 0.084(10) 0.101(12) -0.037(9) -0.038(11) 0.010(9) C21B 0.42(3) 0.072(10) 0.127(16) -0.004(10) -0.17(2) 0.005(15) C22A 0.123(11) 0.077(8) 0.097(11) 0.054(8) 0.017(9) 0.002(8) C22C 0.099(10) 0.080(9) 0.112(13) 0.015(9) -0.026(9) 0.002(7) C22B 0.134(11) 0.037(6) 0.130(13) 0.011(7) 0.021(10) 0.021(7) C32C 0.108(10) 0.091(9) 0.060(8) 0.005(7) 0.029(8) -0.013(8) C32B 0.119(12) 0.125(12) 0.070(9) -0.010(9) 0.012(9) -0.017(10) C32A 0.095(9) 0.083(9) 0.076(9) -0.023(7) 0.018(8) 0.021(7) C100 0.105(12) 0.167(15) 0.067(10) 0.015(10) -0.012(9) 0.056(11) C101 0.125(13) 0.173(16) 0.077(12) -0.012(11) -0.024(10) 0.096(12) C102 0.061(10) 0.141(14) 0.23(2) 0.045(15) -0.018(12) 0.031(10) C103 0.092(11) 0.122(12) 0.114(14) 0.029(11) -0.002(10) 0.047(9) C104 0.094(10) 0.123(11) 0.064(9) 0.013(8) 0.023(8) 0.000(9) C105 0.138(13) 0.099(11) 0.084(11) -0.003(9) -0.036(10) -0.007(9) C203 0.124(12) 0.072(9) 0.149(15) 0.038(10) 0.053(11) 0.028(9) C204 0.111(10) 0.074(8) 0.090(10) 0.012(8) 0.027(9) 0.002(8) C205 0.041(7) 0.147(12) 0.100(11) -0.075(10) -0.002(7) 0.006(7) C206 0.054(7) 0.076(8) 0.062(8) -0.027(7) -0.004(6) 0.002(6) C300 0.13(2) 0.13(2) 0.11(2) 0.000 0.000 0.074(17) C301 0.27(4) 0.14(2) 0.16(3) 0.076(18) 0.05(2) 0.11(2) C302 0.17(2) 0.19(3) 0.28(4) 0.07(2) 0.02(2) 0.085(19) N1 0.047(6) 0.120(9) 0.076(9) 0.006(7) 0.014(6) 0.026(6) N2 0.064(6) 0.056(6) 0.047(6) -0.007(5) -0.009(5) 0.004(5) N3 0.053(6) 0.068(7) 0.098(9) 0.037(6) -0.010(6) -0.013(5) N4 0.045(5) 0.057(6) 0.091(8) -0.022(5) -0.022(5) 0.010(4) Li1 0.031(8) 0.064(11) 0.052(11) -0.008(9) 0.006(8) -0.010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C3 1.876(14) . ? W1 C2 1.910(13) . ? W1 C1 1.922(12) . ? W1 Ge5 2.7267(11) . ? W1 Ge4 2.7337(11) . ? W1 Ge6 2.7506(11) . ? W1 Ge2 2.8053(10) . ? W1 Ge3 2.8243(12) . ? Ge2 Si2 2.405(3) . ? Ge2 Ge6 2.5435(15) . ? Ge2 Ge4 2.5799(14) . ? Ge2 Ge7 2.5948(13) . ? Ge2 Ge9 2.7291(17) . ? Ge1 Si1 2.379(3) . ? Ge1 Ge8 2.5081(18) . ? Ge1 Ge7 2.5097(15) . ? Ge1 Ge4 2.5293(15) . ? Ge1 Ge5 2.5339(14) . ? Ge3 Si3 2.395(3) . ? Ge3 Ge6 2.5558(14) . ? Ge3 Ge5 2.5727(15) . ? Ge3 Ge8 2.5934(14) . ? Ge3 Ge9 2.7029(14) . ? Ge4 Ge5 2.8186(16) . ? Ge6 Ge9 2.7331(14) . ? Ge7 Ge9 2.5927(16) . ? Ge7 Ge8 2.7999(17) . ? Ge9 Ge8 2.5882(14) . ? Si2 Si12 2.349(5) . ? Si2 Si10 2.354(4) . ? Si2 Si11 2.364(4) . ? Si1 Si21 2.331(5) . ? Si1 Si22 2.335(4) . ? Si1 Si20 2.344(5) . ? Si3 Si30 2.337(4) . ? Si3 Si31 2.346(4) . ? Si3 Si32 2.355(4) . ? Si10 C10C 1.819(14) . ? Si10 C10B 1.833(11) . ? Si10 C10A 1.870(16) . ? Si11 C11B 1.820(12) . ? Si11 C11C 1.842(14) . ? Si11 C11A 1.881(11) . ? Si12 C12B 1.838(13) . ? Si12 C12A 1.875(14) . ? Si12 C12C 1.899(14) . ? Si20 C20C 1.834(13) . ? Si20 C20B 1.853(13) . ? Si20 C20A 1.871(15) . ? Si21 C21A 1.783(16) . ? Si21 C21C 1.848(12) . ? Si21 C21B 1.901(17) . ? Si22 C22A 1.799(12) . ? Si22 C22C 1.841(13) . ? Si22 C22B 1.859(11) . ? Si30 C30A 1.849(16) . ? Si30 C30C 1.849(15) . ? Si30 C30F 1.855(15) . ? Si30 C30E 1.860(15) . ? Si30 C30B 1.867(15) . ? Si30 C30D 1.879(15) . ? Si31 C31A 1.847(15) . ? Si31 C31B 1.848(16) . ? Si31 C31C 1.861(16) . ? Si31 C31D 1.862(15) . ? Si31 C31E 1.868(14) . ? Si31 C31F 1.874(13) . ? Si32 C32C 1.827(11) . ? Si32 C32B 1.831(13) . ? Si32 C32A 1.859(11) . ? O1 C1 1.208(11) . ? O2 C2 1.209(12) . ? O3 C3 1.239(13) . ? C100 C101 1.337(17) . ? C100 N2 1.445(14) . ? C101 N1 1.460(17) . ? C102 N1 1.410(17) . ? C103 N1 1.441(17) . ? C104 N2 1.490(14) . ? C105 N2 1.426(15) . ? C200 C201 1.52(3) . ? C200 N3 1.56(3) . ? C200 Li1 2.78(3) . ? C201 N4 1.44(2) . ? C210 N3 1.50(2) . ? C210 C211 1.50(3) . ? C211 N4 1.69(3) . ? C203 N3 1.411(16) . ? C204 N3 1.434(14) . ? C205 N4 1.441(14) . ? C206 N4 1.450(12) . ? C300 C301 1.47(2) . ? C300 C301 1.47(2) 2_655 ? C301 C302 1.55(3) . ? N1 Li1 2.139(18) . ? N2 Li1 2.107(18) . ? N3 Li1 2.088(19) . ? N4 Li1 2.122(17) . ? 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 C3 W1 C2 87.3(5) . . ? C3 W1 C1 86.8(4) . . ? C2 W1 C1 85.7(4) . . ? C3 W1 Ge5 119.9(3) . . ? C2 W1 Ge5 72.3(3) . . ? C1 W1 Ge5 143.5(3) . . ? C3 W1 Ge4 74.6(3) . . ? C2 W1 Ge4 110.4(3) . . ? C1 W1 Ge4 154.3(3) . . ? Ge5 W1 Ge4 62.15(3) . . ? C3 W1 Ge6 124.7(3) . . ? C2 W1 Ge6 135.5(4) . . ? C1 W1 Ge6 68.5(3) . . ? Ge5 W1 Ge6 107.61(3) . . ? Ge4 W1 Ge6 107.75(3) . . ? C3 W1 Ge2 93.9(3) . . ? C2 W1 Ge2 164.6(3) . . ? C1 W1 Ge2 109.7(3) . . ? Ge5 W1 Ge2 93.92(3) . . ? Ge4 W1 Ge2 55.50(3) . . ? Ge6 W1 Ge2 54.48(3) . . ? C3 W1 Ge3 167.6(3) . . ? C2 W1 Ge3 100.7(3) . . ? C1 W1 Ge3 103.1(3) . . ? Ge5 W1 Ge3 55.19(3) . . ? Ge4 W1 Ge3 93.67(3) . . ? Ge6 W1 Ge3 54.56(3) . . ? Ge2 W1 Ge3 75.88(3) . . ? Si2 Ge2 Ge6 111.46(8) . . ? Si2 Ge2 Ge4 119.96(9) . . ? Ge6 Ge2 Ge4 119.68(5) . . ? Si2 Ge2 Ge7 106.00(8) . . ? Ge6 Ge2 Ge7 118.75(6) . . ? Ge4 Ge2 Ge7 75.49(4) . . ? Si2 Ge2 Ge9 115.64(8) . . ? Ge6 Ge2 Ge9 62.33(4) . . ? Ge4 Ge2 Ge9 114.65(5) . . ? Ge7 Ge2 Ge9 58.22(4) . . ? Si2 Ge2 W1 132.82(8) . . ? Ge6 Ge2 W1 61.67(3) . . ? Ge4 Ge2 W1 60.84(3) . . ? Ge7 Ge2 W1 118.03(4) . . ? Ge9 Ge2 W1 101.95(4) . . ? Si1 Ge1 Ge8 121.18(9) . . ? Si1 Ge1 Ge7 121.91(9) . . ? Ge8 Ge1 Ge7 67.83(5) . . ? Si1 Ge1 Ge4 124.11(9) . . ? Ge8 Ge1 Ge4 114.70(5) . . ? Ge7 Ge1 Ge4 77.90(4) . . ? Si1 Ge1 Ge5 123.96(9) . . ? Ge8 Ge1 Ge5 78.09(5) . . ? Ge7 Ge1 Ge5 114.12(5) . . ? Ge4 Ge1 Ge5 67.65(4) . . ? Si3 Ge3 Ge6 111.16(8) . . ? Si3 Ge3 Ge5 120.33(8) . . ? Ge6 Ge3 Ge5 119.06(5) . . ? Si3 Ge3 Ge8 106.34(8) . . ? Ge6 Ge3 Ge8 119.05(5) . . ? Ge5 Ge3 Ge8 75.87(4) . . ? Si3 Ge3 Ge9 115.27(8) . . ? Ge6 Ge3 Ge9 62.55(4) . . ? Ge5 Ge3 Ge9 115.20(5) . . ? Ge8 Ge3 Ge9 58.46(4) . . ? Si3 Ge3 W1 132.57(8) . . ? Ge6 Ge3 W1 61.25(3) . . ? Ge5 Ge3 W1 60.48(3) . . ? Ge8 Ge3 W1 118.05(5) . . ? Ge9 Ge3 W1 102.12(4) . . ? Ge1 Ge4 Ge2 96.16(5) . . ? Ge1 Ge4 W1 107.66(5) . . ? Ge2 Ge4 W1 63.65(3) . . ? Ge1 Ge4 Ge5 56.25(4) . . ? Ge2 Ge4 Ge5 96.91(5) . . ? W1 Ge4 Ge5 58.80(3) . . ? Ge2 Ge6 Ge3 85.50(4) . . ? Ge2 Ge6 Ge9 62.17(4) . . ? Ge3 Ge6 Ge9 61.36(4) . . ? Ge2 Ge6 W1 63.85(3) . . ? Ge3 Ge6 W1 64.19(3) . . ? Ge9 Ge6 W1 103.27(4) . . ? Ge1 Ge5 Ge3 95.96(5) . . ? Ge1 Ge5 W1 107.74(4) . . ? Ge3 Ge5 W1 64.33(3) . . ? Ge1 Ge5 Ge4 56.10(4) . . ? Ge3 Ge5 Ge4 97.42(5) . . ? W1 Ge5 Ge4 59.05(3) . . ? Ge1 Ge7 Ge9 105.17(5) . . ? Ge1 Ge7 Ge2 96.26(4) . . ? Ge9 Ge7 Ge2 63.48(4) . . ? Ge1 Ge7 Ge8 56.05(4) . . ? Ge9 Ge7 Ge8 57.21(4) . . ? Ge2 Ge7 Ge8 97.62(4) . . ? Ge8 Ge9 Ge7 65.43(4) . . ? Ge8 Ge9 Ge3 58.65(4) . . ? Ge7 Ge9 Ge3 99.51(5) . . ? Ge8 Ge9 Ge2 99.59(5) . . ? Ge7 Ge9 Ge2 58.30(4) . . ? Ge3 Ge9 Ge2 79.17(4) . . ? Ge8 Ge9 Ge6 113.00(5) . . ? Ge7 Ge9 Ge6 112.22(5) . . ? Ge3 Ge9 Ge6 56.09(3) . . ? Ge2 Ge9 Ge6 55.51(4) . . ? Ge1 Ge8 Ge9 105.35(6) . . ? Ge1 Ge8 Ge3 96.07(5) . . ? Ge9 Ge8 Ge3 62.88(4) . . ? Ge1 Ge8 Ge7 56.11(4) . . ? Ge9 Ge8 Ge7 57.37(4) . . ? Ge3 Ge8 Ge7 97.03(5) . . ? Si12 Si2 Si10 108.32(18) . . ? Si12 Si2 Si11 109.64(17) . . ? Si10 Si2 Si11 108.37(16) . . ? Si12 Si2 Ge2 110.35(14) . . ? Si10 Si2 Ge2 109.95(13) . . ? Si11 Si2 Ge2 110.17(15) . . ? Si21 Si1 Si22 115.51(17) . . ? Si21 Si1 Si20 110.4(2) . . ? Si22 Si1 Si20 109.65(18) . . ? Si21 Si1 Ge1 106.02(15) . . ? Si22 Si1 Ge1 108.22(15) . . ? Si20 Si1 Ge1 106.64(14) . . ? Si30 Si3 Si31 109.85(18) . . ? Si30 Si3 Si32 109.18(18) . . ? Si31 Si3 Si32 108.96(17) . . ? Si30 Si3 Ge3 112.11(16) . . ? Si31 Si3 Ge3 108.13(15) . . ? Si32 Si3 Ge3 108.54(14) . . ? C10C Si10 C10B 110.3(6) . . ? C10C Si10 C10A 108.1(8) . . ? C10B Si10 C10A 105.1(7) . . ? C10C Si10 Si2 112.1(5) . . ? C10B Si10 Si2 110.1(4) . . ? C10A Si10 Si2 110.9(5) . . ? C11B Si11 C11C 106.3(8) . . ? C11B Si11 C11A 107.5(6) . . ? C11C Si11 C11A 109.1(7) . . ? C11B Si11 Si2 114.2(4) . . ? C11C Si11 Si2 110.0(5) . . ? C11A Si11 Si2 109.6(5) . . ? C12B Si12 C12A 108.6(7) . . ? C12B Si12 C12C 106.3(7) . . ? C12A Si12 C12C 110.7(8) . . ? C12B Si12 Si2 111.4(5) . . ? C12A Si12 Si2 108.6(5) . . ? C12C Si12 Si2 111.2(5) . . ? C20C Si20 C20B 108.5(7) . . ? C20C Si20 C20A 106.0(7) . . ? C20B Si20 C20A 107.8(7) . . ? C20C Si20 Si1 113.0(5) . . ? C20B Si20 Si1 110.5(5) . . ? C20A Si20 Si1 110.8(5) . . ? C21A Si21 C21C 107.5(7) . . ? C21A Si21 C21B 110.8(9) . . ? C21C Si21 C21B 107.6(7) . . ? C21A Si21 Si1 113.5(5) . . ? C21C Si21 Si1 111.7(5) . . ? C21B Si21 Si1 105.7(6) . . ? C22A Si22 C22C 106.3(7) . . ? C22A Si22 C22B 109.9(6) . . ? C22C Si22 C22B 109.1(6) . . ? C22A Si22 Si1 111.0(4) . . ? C22C Si22 Si1 112.6(4) . . ? C22B Si22 Si1 108.0(5) . . ? C30A Si30 C30C 101.7(18) . . ? C30A Si30 C30F 119.6(18) . . ? C30C Si30 C30F 22.6(13) . . ? C30A Si30 C30E 69.3(16) . . ? C30C Si30 C30E 131.2(13) . . ? C30F Si30 C30E 121.3(13) . . ? C30A Si30 C30B 106.5(17) . . ? C30C Si30 C30B 108.0(14) . . ? C30F Si30 C30B 88.8(14) . . ? C30E Si30 C30B 40.8(11) . . ? C30A Si30 C30D 29.1(15) . . ? C30C Si30 C30D 79.6(16) . . ? C30F Si30 C30D 101.2(16) . . ? C30E Si30 C30D 98.1(15) . . ? C30B Si30 C30D 131.9(16) . . ? C30A Si30 Si3 116.8(14) . . ? C30C Si30 Si3 113.6(10) . . ? C30F Si30 Si3 111.3(10) . . ? C30E Si30 Si3 112.8(9) . . ? C30B Si30 Si3 109.6(9) . . ? C30D Si30 Si3 110.0(11) . . ? C31A Si31 C31B 113.0(19) . . ? C31A Si31 C31C 103.5(17) . . ? C31B Si31 C31C 111(2) . . ? C31A Si31 C31D 30.1(10) . . ? C31B Si31 C31D 87.3(18) . . ? C31C Si31 C31D 129.9(17) . . ? C31A Si31 C31E 122.2(11) . . ? C31B Si31 C31E 19.2(17) . . ? C31C Si31 C31E 92.3(17) . . ? C31D Si31 C31E 101.8(12) . . ? C31A Si31 C31F 90.0(14) . . ? C31B Si31 C31F 122.6(19) . . ? C31C Si31 C31F 14(2) . . ? C31D Si31 C31F 118.0(13) . . ? C31E Si31 C31F 104.1(13) . . ? C31A Si31 Si3 111.8(8) . . ? C31B Si31 Si3 107.6(15) . . ? C31C Si31 Si3 109.5(15) . . ? C31D Si31 Si3 107.7(8) . . ? C31E Si31 Si3 114.2(7) . . ? C31F Si31 Si3 110.9(10) . . ? C32C Si32 C32B 110.0(6) . . ? C32C Si32 C32A 108.2(6) . . ? C32B Si32 C32A 105.8(6) . . ? C32C Si32 Si3 109.8(4) . . ? C32B Si32 Si3 110.0(5) . . ? C32A Si32 Si3 112.9(4) . . ? O1 C1 W1 175.6(9) . . ? O2 C2 W1 177.7(10) . . ? O3 C3 W1 177.1(9) . . ? C101 C100 N2 119.5(13) . . ? C100 C101 N1 118.5(14) . . ? C201 C200 N3 109.3(17) . . ? C201 C200 Li1 74.6(12) . . ? N3 C200 Li1 48.0(8) . . ? N4 C201 C200 108.9(16) . . ? N3 C210 C211 101.1(18) . . ? C210 C211 N4 107.7(17) . . ? C301 C300 C301 125(3) . 2_655 ? C300 C301 C302 122(3) . . ? C102 N1 C103 106.6(12) . . ? C102 N1 C101 110.9(14) . . ? C103 N1 C101 109.5(13) . . ? C102 N1 Li1 112.5(10) . . ? C103 N1 Li1 115.7(9) . . ? C101 N1 Li1 101.7(9) . . ? C105 N2 C100 109.7(11) . . ? C105 N2 C104 104.9(10) . . ? C100 N2 C104 112.3(10) . . ? C105 N2 Li1 114.8(9) . . ? C100 N2 Li1 102.4(9) . . ? C104 N2 Li1 112.9(8) . . ? C203 N3 C204 110.8(9) . . ? C203 N3 C210 89.5(13) . . ? C204 N3 C210 122.5(13) . . ? C203 N3 C200 124.6(13) . . ? C204 N3 C200 91.3(13) . . ? C210 N3 C200 38.9(10) . . ? C203 N3 Li1 116.0(10) . . ? C204 N3 Li1 113.2(9) . . ? C210 N3 Li1 103.1(10) . . ? C200 N3 Li1 98.4(11) . . ? C205 N4 C201 97.5(12) . . ? C205 N4 C206 107.9(9) . . ? C201 N4 C206 119.4(13) . . ? C205 N4 C211 124.1(12) . . ? C201 N4 C211 28.1(10) . . ? C206 N4 C211 98.9(11) . . ? C205 N4 Li1 115.0(9) . . ? C201 N4 Li1 101.4(10) . . ? C206 N4 Li1 114.6(8) . . ? C211 N4 Li1 95.3(10) . . ? N3 Li1 N2 121.9(9) . . ? N3 Li1 N4 89.0(7) . . ? N2 Li1 N4 121.3(8) . . ? N3 Li1 N1 122.4(8) . . ? N2 Li1 N1 86.2(8) . . ? N4 Li1 N1 120.0(9) . . ? N3 Li1 C200 33.6(6) . . ? N2 Li1 C200 144.7(10) . . ? N4 Li1 C200 56.9(7) . . ? N1 Li1 C200 126.9(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.735 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.090 data_fh92tet _database_code_depnum_ccdc_archive 'CCDC 807924' #TrackingRef '- FH92tet(CCDC-807924).pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.50 H119 Cr Ge9 Li N4 O3 Si12' _chemical_formula_weight 1807.77 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 25.726(4) _cell_length_b 25.726(4) _cell_length_c 26.657(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17643(5) _cell_formula_units_Z 8 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 6409 _cell_measurement_theta_min 1.10 _cell_measurement_theta_max 20.07 _exptl_crystal_description diamond _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7368 _exptl_absorpt_coefficient_mu 3.332 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5825 _exptl_absorpt_correction_T_max 0.9027 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 149(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25868 _diffrn_reflns_av_R_equivalents 0.1674 _diffrn_reflns_av_sigmaI/netI 0.3511 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 22.78 _reflns_number_total 10149 _reflns_number_gt 3089 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 10149 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2243 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1274 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 0.759 _refine_ls_restrained_S_all 0.759 _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 Cr1 Cr 0.39148(15) 0.69075(17) 0.15159(14) 0.0643(12) Uani 1 1 d . . . Ge1 Ge 0.35707(11) 0.78884(10) 0.15598(10) 0.0684(8) Uani 1 1 d . . . Ge2 Ge 0.23146(11) 0.71226(15) 0.15615(11) 0.0980(12) Uani 1 1 d . . . Ge3 Ge 0.34553(10) 0.69137(11) 0.24285(9) 0.0691(8) Uani 1 1 d . . . Ge4 Ge 0.31068(11) 0.72375(11) 0.10061(9) 0.0689(9) Uani 1 1 d . . . Ge5 Ge 0.30151(11) 0.64443(11) 0.17057(9) 0.0739(9) Uani 1 1 d . . . Ge6 Ge 0.41751(11) 0.75630(12) 0.22417(9) 0.0656(8) Uani 1 1 d . . . Ge7 Ge 0.32195(10) 0.79306(11) 0.25237(10) 0.0755(9) Uani 1 1 d . . . Ge8 Ge 0.25004(11) 0.72313(12) 0.24794(11) 0.0837(10) Uani 1 1 d . . . Ge9 Ge 0.25921(11) 0.80291(13) 0.17707(10) 0.0801(10) Uani 1 1 d . . . Si1 Si 0.3865(3) 0.8696(3) 0.1221(3) 0.080(3) Uani 1 1 d . . . Si2 Si 0.1464(3) 0.6934(5) 0.1282(3) 0.107(3) Uani 1 1 d . . . Si3 Si 0.3605(3) 0.6463(4) 0.3197(3) 0.088(3) Uani 1 1 d . . . Si10 Si 0.3886(4) 0.9349(3) 0.1860(3) 0.101(3) Uani 1 1 d . . . Si11 Si 0.4714(4) 0.8597(3) 0.0905(3) 0.094(3) Uani 1 1 d . . . Si12 Si 0.3319(5) 0.8970(4) 0.0576(4) 0.129(4) Uani 1 1 d . . . Si20 Si 0.1206(4) 0.7637(7) 0.0789(4) 0.162(6) Uani 1 1 d . . . Si21 Si 0.1527(4) 0.6146(7) 0.0807(5) 0.202(8) Uani 1 1 d . . . Si22 Si 0.0927(3) 0.6769(4) 0.1955(3) 0.096(3) Uani 1 1 d . . . Si30 Si 0.2959(5) 0.5873(5) 0.3398(4) 0.144(4) Uani 1 1 d . . . Si31 Si 0.3665(3) 0.7081(4) 0.3852(3) 0.091(3) Uani 1 1 d . . . Si32 Si 0.4381(4) 0.6017(4) 0.3135(3) 0.121(4) Uani 1 1 d . . . O1 O 0.5031(8) 0.6822(8) 0.1726(7) 0.114(7) Uiso 1 1 d . . . O2 O 0.4295(8) 0.6963(9) 0.0485(8) 0.122(8) Uiso 1 1 d . . . O3 O 0.4027(13) 0.5837(14) 0.1314(9) 0.197(12) Uiso 1 1 d . . . C1 C 0.4538(12) 0.6901(11) 0.1687(9) 0.088(9) Uiso 1 1 d . . . C2 C 0.4112(11) 0.6938(11) 0.0917(10) 0.084(9) Uiso 1 1 d . . . C3 C 0.3980(15) 0.630(2) 0.1460(12) 0.152(14) Uiso 1 1 d . . . C10B C 0.3982(12) 0.9989(12) 0.1523(11) 0.130(12) Uiso 1 1 d . . . H10A H 0.3993 1.0272 0.1769 0.195 Uiso 1 1 calc R . . H10B H 0.3692 1.0047 0.1291 0.195 Uiso 1 1 calc R . . H10C H 0.4309 0.9980 0.1335 0.195 Uiso 1 1 calc R . . C10A C 0.4415(13) 0.9182(14) 0.2294(12) 0.155(14) Uiso 1 1 d . . . H10D H 0.4434 0.9443 0.2561 0.233 Uiso 1 1 calc R . . H10E H 0.4745 0.9175 0.2111 0.233 Uiso 1 1 calc R . . H10F H 0.4349 0.8839 0.2442 0.233 Uiso 1 1 calc R . . C10C C 0.3279(10) 0.9367(11) 0.2210(9) 0.102(10) Uiso 1 1 d . . . H10G H 0.3299 0.9637 0.2469 0.154 Uiso 1 1 calc R . . H10H H 0.3219 0.9029 0.2369 0.154 Uiso 1 1 calc R . . H10I H 0.2992 0.9445 0.1981 0.154 Uiso 1 1 calc R . . C11B C 0.4966(13) 0.9247(12) 0.0744(10) 0.130(12) Uiso 1 1 d . . . H11A H 0.5319 0.9214 0.0610 0.195 Uiso 1 1 calc R . . H11B H 0.4973 0.9464 0.1046 0.195 Uiso 1 1 calc R . . H11C H 0.4740 0.9407 0.0492 0.195 Uiso 1 1 calc R . . C11A C 0.5164(12) 0.8303(12) 0.1327(10) 0.118(11) Uiso 1 1 d . . . H11D H 0.5504 0.8272 0.1164 0.178 Uiso 1 1 calc R . . H11E H 0.5039 0.7956 0.1420 0.178 Uiso 1 1 calc R . . H11F H 0.5196 0.8518 0.1629 0.178 Uiso 1 1 calc R . . C11C C 0.4627(18) 0.8280(18) 0.0263(16) 0.24(2) Uiso 1 1 d . . . H11G H 0.4968 0.8224 0.0108 0.359 Uiso 1 1 calc R . . H11H H 0.4418 0.8509 0.0048 0.359 Uiso 1 1 calc R . . H11I H 0.4449 0.7946 0.0302 0.359 Uiso 1 1 calc R . . C12A C 0.2663(14) 0.9150(14) 0.0815(10) 0.145(12) Uiso 1 1 d . . . H12A H 0.2444 0.9262 0.0534 0.218 Uiso 1 1 calc R . . H12B H 0.2695 0.9433 0.1058 0.218 Uiso 1 1 calc R . . H12C H 0.2503 0.8847 0.0978 0.218 Uiso 1 1 calc R . . C12C C 0.3611(15) 0.9557(14) 0.0225(12) 0.165(14) Uiso 1 1 d . . . H12D H 0.3376 0.9662 -0.0046 0.248 Uiso 1 1 calc R . . H12E H 0.3949 0.9460 0.0083 0.248 Uiso 1 1 calc R . . H12F H 0.3657 0.9847 0.0459 0.248 Uiso 1 1 calc R . . C12B C 0.3259(14) 0.8514(15) 0.0084(12) 0.177(16) Uiso 1 1 d . . . H12G H 0.3026 0.8653 -0.0174 0.265 Uiso 1 1 calc R . . H12H H 0.3116 0.8188 0.0216 0.265 Uiso 1 1 calc R . . H12I H 0.3602 0.8448 -0.0063 0.265 Uiso 1 1 calc R . . C20C C 0.1215(18) 0.8214(16) 0.1082(15) 0.200(19) Uiso 1 1 d . . . H20A H 0.1102 0.8486 0.0849 0.300 Uiso 1 1 calc R . . H20B H 0.1569 0.8289 0.1197 0.300 Uiso 1 1 calc R . . H20C H 0.0979 0.8203 0.1371 0.300 Uiso 1 1 calc R . . C20B C 0.0523(15) 0.7530(17) 0.0570(12) 0.195(17) Uiso 1 1 d . . . H20D H 0.0412 0.7826 0.0364 0.293 Uiso 1 1 calc R . . H20E H 0.0292 0.7498 0.0861 0.293 Uiso 1 1 calc R . . H20F H 0.0506 0.7211 0.0370 0.293 Uiso 1 1 calc R . . C20A C 0.1637(16) 0.7569(18) 0.0209(13) 0.216(19) Uiso 1 1 d . . . H20G H 0.1562 0.7853 -0.0024 0.325 Uiso 1 1 calc R . . H20H H 0.1566 0.7235 0.0045 0.325 Uiso 1 1 calc R . . H20I H 0.2003 0.7583 0.0310 0.325 Uiso 1 1 calc R . . C21A C 0.1566(18) 0.5561(17) 0.1310(14) 0.20(2) Uiso 1 1 d . . . H21A H 0.1591 0.5228 0.1132 0.306 Uiso 1 1 calc R . . H21B H 0.1253 0.5562 0.1520 0.306 Uiso 1 1 calc R . . H21C H 0.1874 0.5607 0.1522 0.306 Uiso 1 1 calc R . . C21C C 0.2134(13) 0.6067(13) 0.0513(11) 0.143(13) Uiso 1 1 d . . . H21D H 0.2137 0.5739 0.0326 0.215 Uiso 1 1 calc R . . H21E H 0.2408 0.6060 0.0768 0.215 Uiso 1 1 calc R . . H21F H 0.2195 0.6356 0.0282 0.215 Uiso 1 1 calc R . . C21B C 0.0925(16) 0.6128(15) 0.0382(13) 0.178(16) Uiso 1 1 d . . . H21G H 0.0932 0.5811 0.0178 0.267 Uiso 1 1 calc R . . H21H H 0.0925 0.6433 0.0162 0.267 Uiso 1 1 calc R . . H21I H 0.0610 0.6130 0.0590 0.267 Uiso 1 1 calc R . . C22B C 0.0939(13) 0.7345(14) 0.2356(11) 0.158(14) Uiso 1 1 d . . . H22A H 0.0711 0.7290 0.2646 0.237 Uiso 1 1 calc R . . H22B H 0.0817 0.7647 0.2165 0.237 Uiso 1 1 calc R . . H22C H 0.1295 0.7408 0.2472 0.237 Uiso 1 1 calc R . . C22A C 0.0285(11) 0.6581(12) 0.1749(10) 0.118(11) Uiso 1 1 d . . . H22D H 0.0065 0.6512 0.2041 0.177 Uiso 1 1 calc R . . H22E H 0.0310 0.6265 0.1543 0.177 Uiso 1 1 calc R . . H22F H 0.0133 0.6862 0.1549 0.177 Uiso 1 1 calc R . . C22C C 0.1213(15) 0.6286(15) 0.2390(13) 0.181(16) Uiso 1 1 d . . . H22G H 0.0972 0.6223 0.2669 0.272 Uiso 1 1 calc R . . H22H H 0.1543 0.6418 0.2521 0.272 Uiso 1 1 calc R . . H22I H 0.1274 0.5959 0.2210 0.272 Uiso 1 1 calc R . . C30B C 0.2303(19) 0.6170(18) 0.3471(15) 0.23(2) Uiso 1 1 d . . . H30A H 0.2051 0.5899 0.3558 0.345 Uiso 1 1 calc R . . H30B H 0.2200 0.6336 0.3155 0.345 Uiso 1 1 calc R . . H30C H 0.2314 0.6432 0.3738 0.345 Uiso 1 1 calc R . . C30A C 0.2763(16) 0.5446(16) 0.2862(13) 0.191(17) Uiso 1 1 d . . . H30D H 0.2490 0.5206 0.2972 0.287 Uiso 1 1 calc R . . H30E H 0.3065 0.5246 0.2746 0.287 Uiso 1 1 calc R . . H30F H 0.2632 0.5661 0.2586 0.287 Uiso 1 1 calc R . . C30C C 0.3074(17) 0.5590(15) 0.3989(15) 0.203(18) Uiso 1 1 d . . . H30G H 0.2795 0.5343 0.4066 0.305 Uiso 1 1 calc R . . H30H H 0.3082 0.5862 0.4246 0.305 Uiso 1 1 calc R . . H30I H 0.3408 0.5407 0.3984 0.305 Uiso 1 1 calc R . . C31C C 0.3034(11) 0.7330(11) 0.3953(9) 0.102(9) Uiso 1 1 d . . . H31A H 0.3043 0.7585 0.4226 0.153 Uiso 1 1 calc R . . H31B H 0.2798 0.7046 0.4043 0.153 Uiso 1 1 calc R . . H31C H 0.2909 0.7499 0.3646 0.153 Uiso 1 1 calc R . . C31B C 0.4142(11) 0.7590(11) 0.3719(8) 0.105(9) Uiso 1 1 d . . . H31D H 0.4153 0.7835 0.4000 0.158 Uiso 1 1 calc R . . H31E H 0.4043 0.7774 0.3412 0.158 Uiso 1 1 calc R . . H31F H 0.4486 0.7432 0.3675 0.158 Uiso 1 1 calc R . . C31A C 0.3920(14) 0.6712(14) 0.4436(11) 0.170(15) Uiso 1 1 d . . . H31G H 0.3945 0.6952 0.4720 0.254 Uiso 1 1 calc R . . H31H H 0.4263 0.6566 0.4363 0.254 Uiso 1 1 calc R . . H31I H 0.3679 0.6430 0.4520 0.254 Uiso 1 1 calc R . . C32A C 0.4969(15) 0.6558(16) 0.3035(14) 0.172(16) Uiso 1 1 d . . . H32A H 0.5304 0.6378 0.3012 0.258 Uiso 1 1 calc R . . H32B H 0.4974 0.6797 0.3321 0.258 Uiso 1 1 calc R . . H32C H 0.4907 0.6753 0.2726 0.258 Uiso 1 1 calc R . . C32B C 0.4429(16) 0.5654(16) 0.2550(15) 0.21(2) Uiso 1 1 d . . . H32D H 0.4762 0.5470 0.2538 0.310 Uiso 1 1 calc R . . H32E H 0.4406 0.5895 0.2266 0.310 Uiso 1 1 calc R . . H32F H 0.4144 0.5402 0.2531 0.310 Uiso 1 1 calc R . . C32C C 0.450(2) 0.572(2) 0.3749(19) 0.30(3) Uiso 1 1 d . . . H32G H 0.4827 0.5536 0.3744 0.455 Uiso 1 1 calc R . . H32H H 0.4213 0.5483 0.3827 0.455 Uiso 1 1 calc R . . H32I H 0.4510 0.5998 0.4004 0.455 Uiso 1 1 calc R . . C100 C 0.4185(14) 0.6932(15) -0.2053(11) 0.146(13) Uiso 1 1 d . . . H10J H 0.3896 0.7183 -0.2088 0.175 Uiso 1 1 calc R . . H10K H 0.4349 0.6901 -0.2388 0.175 Uiso 1 1 calc R . . C101 C 0.4584(15) 0.7181(15) -0.1711(13) 0.153(14) Uiso 1 1 d . . . H10L H 0.4612 0.7556 -0.1788 0.183 Uiso 1 1 calc R . . H10M H 0.4928 0.7019 -0.1766 0.183 Uiso 1 1 calc R . . C102 C 0.4858(17) 0.7172(17) -0.0890(14) 0.195(18) Uiso 1 1 d . . . H10N H 0.5076 0.6861 -0.0919 0.293 Uiso 1 1 calc R . . H10O H 0.4765 0.7228 -0.0538 0.293 Uiso 1 1 calc R . . H10P H 0.5051 0.7475 -0.1015 0.293 Uiso 1 1 calc R . . C103 C 0.413(2) 0.762(2) -0.1099(17) 0.29(3) Uiso 1 1 d . . . H10Q H 0.3809 0.7615 -0.1290 0.436 Uiso 1 1 calc R . . H10R H 0.4355 0.7905 -0.1221 0.436 Uiso 1 1 calc R . . H10S H 0.4058 0.7674 -0.0742 0.436 Uiso 1 1 calc R . . C104 C 0.3492(15) 0.6414(15) -0.2201(12) 0.160(14) Uiso 1 1 d . . . H10T H 0.3340 0.6074 -0.2127 0.240 Uiso 1 1 calc R . . H10U H 0.3550 0.6446 -0.2563 0.240 Uiso 1 1 calc R . . H10V H 0.3255 0.6689 -0.2090 0.240 Uiso 1 1 calc R . . C110 C 0.4231(14) 0.6094(14) -0.2174(11) 0.146(13) Uiso 1 1 d . . . H11J H 0.4189 0.6127 -0.2538 0.219 Uiso 1 1 calc R . . H11K H 0.4101 0.5755 -0.2064 0.219 Uiso 1 1 calc R . . H11L H 0.4600 0.6125 -0.2088 0.219 Uiso 1 1 calc R . . C200 C 0.322(2) 0.588(2) -0.0573(19) 0.26(2) Uiso 1 1 d . . . H20J H 0.2925 0.5837 -0.0338 0.315 Uiso 1 1 calc R . . H20K H 0.3190 0.5606 -0.0836 0.315 Uiso 1 1 calc R . . C201 C 0.3644(16) 0.5825(16) -0.0341(13) 0.158(14) Uiso 1 1 d . . . H20L H 0.3622 0.5523 -0.0112 0.190 Uiso 1 1 calc R . . H20M H 0.3711 0.6139 -0.0136 0.190 Uiso 1 1 calc R . . C202 C 0.4301(15) 0.5318(16) -0.1083(14) 0.183(16) Uiso 1 1 d . . . H20N H 0.4003 0.5220 -0.1292 0.275 Uiso 1 1 calc R . . H20O H 0.4407 0.5020 -0.0878 0.275 Uiso 1 1 calc R . . H20P H 0.4591 0.5423 -0.1299 0.275 Uiso 1 1 calc R . . C203 C 0.4614(12) 0.5886(12) -0.0419(10) 0.121(10) Uiso 1 1 d . . . H20Q H 0.4498 0.6161 -0.0190 0.181 Uiso 1 1 calc R . . H20R H 0.4907 0.6013 -0.0620 0.181 Uiso 1 1 calc R . . H20S H 0.4724 0.5582 -0.0225 0.181 Uiso 1 1 calc R . . C204 C 0.2753(13) 0.6377(13) -0.1136(11) 0.137(12) Uiso 1 1 d . . . H20T H 0.2810 0.6100 -0.1382 0.205 Uiso 1 1 calc R . . H20U H 0.2692 0.6707 -0.1311 0.205 Uiso 1 1 calc R . . H20V H 0.2449 0.6293 -0.0930 0.205 Uiso 1 1 calc R . . C210 C 0.3156(11) 0.6820(11) -0.0433(9) 0.112(11) Uiso 1 1 d . . . H21J H 0.2808 0.6801 -0.0284 0.168 Uiso 1 1 calc R . . H21K H 0.3208 0.7165 -0.0582 0.168 Uiso 1 1 calc R . . H21L H 0.3418 0.6762 -0.0172 0.168 Uiso 1 1 calc R . . C300 C 0.080(2) 0.4405(19) 0.1231(15) 0.22(2) Uiso 1 1 d . . . H30J H 0.1043 0.4245 0.0997 0.337 Uiso 1 1 calc R . . H30K H 0.0619 0.4132 0.1423 0.337 Uiso 1 1 calc R . . H30L H 0.0985 0.4634 0.1462 0.337 Uiso 1 1 calc R . . C301 C 0.038(2) 0.473(2) 0.0925(17) 0.216(19) Uiso 1 1 d . . . H30M H 0.0584 0.4980 0.0720 0.260 Uiso 1 1 calc R . . H30N H 0.0220 0.4486 0.0687 0.260 Uiso 1 1 calc R . . C302 C 0.0000 0.5000 0.110(3) 0.22(3) Uiso 1 2 d S . . H30O H -0.0176 0.4750 0.1331 0.260 Uiso 0.50 1 calc PR . . H30P H 0.0176 0.5250 0.1331 0.260 Uiso 0.50 1 calc PR . . N1 N 0.4418(11) 0.7108(11) -0.1167(10) 0.123(9) Uiso 1 1 d . . . N2 N 0.3968(10) 0.6464(11) -0.1948(8) 0.103(8) Uiso 1 1 d . . . N3 N 0.4162(11) 0.5733(10) -0.0770(9) 0.119(9) Uiso 1 1 d . . . N4 N 0.3207(10) 0.6425(11) -0.0817(9) 0.125(9) Uiso 1 1 d . . . Li1 Li 0.3979(17) 0.6471(19) -0.1167(14) 0.073(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.057(3) 0.058(3) 0.077(3) -0.007(2) 0.013(2) 0.000(3) Ge1 0.067(2) 0.060(2) 0.079(2) -0.0077(15) 0.0057(16) 0.0087(19) Ge2 0.057(2) 0.136(3) 0.102(2) -0.027(2) 0.0041(17) 0.000(2) Ge3 0.056(2) 0.080(2) 0.0718(19) -0.0129(17) 0.0085(15) -0.0007(18) Ge4 0.057(2) 0.083(2) 0.0661(19) -0.0212(15) 0.0073(14) -0.0010(19) Ge5 0.059(2) 0.072(2) 0.091(2) -0.0206(16) 0.0088(16) -0.0109(19) Ge6 0.054(2) 0.062(2) 0.081(2) -0.0086(16) -0.0012(14) 0.0045(19) Ge7 0.067(2) 0.080(2) 0.079(2) -0.0235(18) 0.0001(16) 0.0153(19) Ge8 0.056(2) 0.114(3) 0.081(2) -0.0223(18) 0.0164(17) 0.011(2) Ge9 0.059(2) 0.089(3) 0.092(2) -0.0281(17) -0.0097(15) 0.027(2) Si1 0.093(7) 0.067(6) 0.079(6) -0.020(4) -0.006(4) -0.001(6) Si2 0.066(6) 0.189(11) 0.064(6) -0.043(6) 0.015(4) -0.011(8) Si3 0.083(7) 0.109(7) 0.070(6) -0.009(5) 0.014(4) -0.010(7) Si10 0.101(8) 0.066(7) 0.136(9) -0.015(5) -0.005(6) -0.009(6) Si11 0.107(8) 0.064(6) 0.112(7) -0.020(5) 0.037(5) -0.022(6) Si12 0.192(13) 0.094(8) 0.102(8) -0.001(6) -0.050(7) 0.007(8) Si20 0.052(7) 0.307(19) 0.125(9) 0.104(10) 0.000(6) -0.009(9) Si21 0.068(8) 0.34(2) 0.199(13) -0.172(13) 0.011(8) -0.035(11) Si22 0.063(7) 0.093(8) 0.131(8) -0.004(6) -0.010(5) -0.009(6) Si30 0.162(12) 0.167(11) 0.103(8) -0.003(7) 0.023(7) -0.066(10) Si31 0.081(7) 0.103(8) 0.090(6) -0.014(5) 0.000(4) 0.006(7) Si32 0.146(11) 0.104(9) 0.112(8) 0.001(6) 0.020(6) 0.018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C3 1.57(5) . ? Cr1 C1 1.67(3) . ? Cr1 C2 1.68(3) . ? Cr1 Ge4 2.625(5) . ? Cr1 Ge5 2.652(5) . ? Cr1 Ge6 2.652(5) . ? Cr1 Ge1 2.677(5) . ? Cr1 Ge3 2.705(5) . ? Ge1 Si1 2.389(9) . ? Ge1 Ge4 2.531(4) . ? Ge1 Ge6 2.534(4) . ? Ge1 Ge9 2.605(4) . ? Ge1 Ge7 2.726(4) . ? Ge2 Si2 2.362(9) . ? Ge2 Ge9 2.502(5) . ? Ge2 Ge8 2.509(4) . ? Ge2 Ge4 2.536(4) . ? Ge2 Ge5 2.538(4) . ? Ge3 Si3 2.385(9) . ? Ge3 Ge5 2.540(4) . ? Ge3 Ge6 2.543(4) . ? Ge3 Ge8 2.592(4) . ? Ge3 Ge7 2.697(4) . ? Ge4 Ge5 2.774(4) . ? Ge6 C1 2.44(3) . ? Ge6 Ge7 2.739(4) . ? Ge7 Ge8 2.583(4) . ? Ge7 Ge9 2.588(4) . ? Ge8 Ge9 2.800(5) . ? Si1 Si12 2.329(13) . ? Si1 Si11 2.354(13) . ? Si1 Si10 2.392(12) . ? Si2 Si22 2.304(13) . ? Si2 Si20 2.331(16) . ? Si2 Si21 2.396(16) . ? Si3 Si32 2.309(14) . ? Si3 Si30 2.313(13) . ? Si3 Si31 2.366(11) . ? Si10 C10C 1.82(3) . ? Si10 C10A 1.84(3) . ? Si10 C10B 1.89(3) . ? Si11 C11A 1.78(3) . ? Si11 C11B 1.84(3) . ? Si11 C11C 1.91(4) . ? Si12 C12B 1.77(3) . ? Si12 C12A 1.86(3) . ? Si12 C12C 1.93(4) . ? Si20 C20C 1.68(4) . ? Si20 C20B 1.87(4) . ? Si20 C20A 1.91(4) . ? Si21 C21C 1.76(3) . ? Si21 C21B 1.92(4) . ? Si21 C21A 2.02(4) . ? Si22 C22A 1.81(3) . ? Si22 C22B 1.83(3) . ? Si22 C22C 1.85(4) . ? Si30 C30C 1.76(4) . ? Si30 C30B 1.86(5) . ? Si30 C30A 1.87(4) . ? Si31 C31C 1.77(3) . ? Si31 C31B 1.83(3) . ? Si31 C31A 1.94(3) . ? Si32 C32B 1.82(4) . ? Si32 C32C 1.82(5) . ? Si32 C32A 2.07(4) . ? O1 C1 1.29(3) . ? O2 C2 1.24(3) . ? O3 C3 1.27(4) . ? C100 N2 1.36(4) . ? C100 C101 1.51(4) . ? C100 Li1 2.70(5) . ? C101 N1 1.53(3) . ? C102 N1 1.36(4) . ? C103 N1 1.52(6) . ? C104 N2 1.40(4) . ? C110 N2 1.31(4) . ? C200 C201 1.26(6) . ? C200 N4 1.55(5) . ? C201 N3 1.77(4) . ? C202 N3 1.40(4) . ? C203 N3 1.54(3) . ? C204 N4 1.45(3) . ? C210 N4 1.45(3) . ? C300 C301 1.59(6) . ? C301 C302 1.28(5) . ? C302 C301 1.28(5) 2_565 ? N1 Li1 1.99(5) . ? N2 Li1 2.08(4) . ? N3 Li1 2.22(5) . ? N4 Li1 2.20(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 C3 Cr1 C1 85.0(18) . . ? C3 Cr1 C2 85.6(15) . . ? C1 Cr1 C2 88.4(12) . . ? C3 Cr1 Ge4 110.8(14) . . ? C1 Cr1 Ge4 155.1(9) . . ? C2 Cr1 Ge4 74.4(9) . . ? C3 Cr1 Ge5 70.5(15) . . ? C1 Cr1 Ge5 141.5(9) . . ? C2 Cr1 Ge5 117.8(9) . . ? Ge4 Cr1 Ge5 63.44(13) . . ? C3 Cr1 Ge6 132.2(13) . . ? C1 Cr1 Ge6 64.1(10) . . ? C2 Cr1 Ge6 126.1(10) . . ? Ge4 Cr1 Ge6 111.84(18) . . ? Ge5 Cr1 Ge6 111.52(16) . . ? C3 Cr1 Ge1 166.5(15) . . ? C1 Cr1 Ge1 108.4(10) . . ? C2 Cr1 Ge1 95.6(10) . . ? Ge4 Cr1 Ge1 57.03(12) . . ? Ge5 Cr1 Ge1 97.27(15) . . ? Ge6 Cr1 Ge1 56.79(13) . . ? C3 Cr1 Ge3 97.9(13) . . ? C1 Cr1 Ge3 100.0(8) . . ? C2 Cr1 Ge3 171.1(9) . . ? Ge4 Cr1 Ge3 96.76(15) . . ? Ge5 Cr1 Ge3 56.61(12) . . ? Ge6 Cr1 Ge3 56.67(11) . . ? Ge1 Cr1 Ge3 79.08(14) . . ? Si1 Ge1 Ge4 120.3(2) . . ? Si1 Ge1 Ge6 111.3(2) . . ? Ge4 Ge1 Ge6 119.27(14) . . ? Si1 Ge1 Ge9 105.5(2) . . ? Ge4 Ge1 Ge9 76.25(12) . . ? Ge6 Ge1 Ge9 118.95(13) . . ? Si1 Ge1 Cr1 134.3(2) . . ? Ge4 Ge1 Cr1 60.45(12) . . ? Ge6 Ge1 Cr1 61.12(13) . . ? Ge9 Ge1 Cr1 117.40(15) . . ? Si1 Ge1 Ge7 115.2(2) . . ? Ge4 Ge1 Ge7 114.82(14) . . ? Ge6 Ge1 Ge7 62.64(10) . . ? Ge9 Ge1 Ge7 58.04(10) . . ? Cr1 Ge1 Ge7 100.85(14) . . ? Si2 Ge2 Ge9 121.7(3) . . ? Si2 Ge2 Ge8 120.5(2) . . ? Ge9 Ge2 Ge8 67.93(13) . . ? Si2 Ge2 Ge4 125.7(2) . . ? Ge9 Ge2 Ge4 78.01(13) . . ? Ge8 Ge2 Ge4 113.78(15) . . ? Si2 Ge2 Ge5 124.4(3) . . ? Ge9 Ge2 Ge5 113.86(15) . . ? Ge8 Ge2 Ge5 78.08(12) . . ? Ge4 Ge2 Ge5 66.29(12) . . ? Si3 Ge3 Ge5 119.5(2) . . ? Si3 Ge3 Ge6 111.7(2) . . ? Ge5 Ge3 Ge6 119.23(13) . . ? Si3 Ge3 Ge8 105.1(2) . . ? Ge5 Ge3 Ge8 76.53(12) . . ? Ge6 Ge3 Ge8 119.55(15) . . ? Si3 Ge3 Ge7 115.3(2) . . ? Ge5 Ge3 Ge7 115.60(13) . . ? Ge6 Ge3 Ge7 62.94(11) . . ? Ge8 Ge3 Ge7 58.42(10) . . ? Si3 Ge3 Cr1 134.4(2) . . ? Ge5 Ge3 Cr1 60.65(12) . . ? Ge6 Ge3 Cr1 60.63(12) . . ? Ge8 Ge3 Cr1 117.58(15) . . ? Ge7 Ge3 Cr1 100.87(15) . . ? Ge1 Ge4 Ge2 96.63(12) . . ? Ge1 Ge4 Cr1 62.53(13) . . ? Ge2 Ge4 Cr1 107.24(14) . . ? Ge1 Ge4 Ge5 97.74(12) . . ? Ge2 Ge4 Ge5 56.88(12) . . ? Cr1 Ge4 Ge5 58.76(13) . . ? Ge2 Ge5 Ge3 96.01(13) . . ? Ge2 Ge5 Cr1 106.37(16) . . ? Ge3 Ge5 Cr1 62.75(13) . . ? Ge2 Ge5 Ge4 56.83(11) . . ? Ge3 Ge5 Ge4 97.03(13) . . ? Cr1 Ge5 Ge4 57.80(12) . . ? C1 Ge6 Ge1 91.8(7) . . ? C1 Ge6 Ge3 86.5(7) . . ? Ge1 Ge6 Ge3 84.87(12) . . ? C1 Ge6 Cr1 38.0(7) . . ? Ge1 Ge6 Cr1 62.09(13) . . ? Ge3 Ge6 Cr1 62.70(12) . . ? C1 Ge6 Ge7 138.7(7) . . ? Ge1 Ge6 Ge7 62.10(11) . . ? Ge3 Ge6 Ge7 61.28(11) . . ? Cr1 Ge6 Ge7 101.13(14) . . ? Ge8 Ge7 Ge9 65.56(13) . . ? Ge8 Ge7 Ge3 58.76(11) . . ? Ge9 Ge7 Ge3 99.35(13) . . ? Ge8 Ge7 Ge1 99.59(13) . . ? Ge9 Ge7 Ge1 58.63(11) . . ? Ge3 Ge7 Ge1 78.36(10) . . ? Ge8 Ge7 Ge6 112.94(13) . . ? Ge9 Ge7 Ge6 112.38(12) . . ? Ge3 Ge7 Ge6 55.77(10) . . ? Ge1 Ge7 Ge6 55.26(10) . . ? Ge2 Ge8 Ge7 104.99(15) . . ? Ge2 Ge8 Ge3 95.42(12) . . ? Ge7 Ge8 Ge3 62.82(11) . . ? Ge2 Ge8 Ge9 55.92(12) . . ? Ge7 Ge8 Ge9 57.30(12) . . ? Ge3 Ge8 Ge9 96.66(13) . . ? Ge2 Ge9 Ge7 105.04(15) . . ? Ge2 Ge9 Ge1 95.63(14) . . ? Ge7 Ge9 Ge1 63.33(11) . . ? Ge2 Ge9 Ge8 56.15(12) . . ? Ge7 Ge9 Ge8 57.14(11) . . ? Ge1 Ge9 Ge8 97.19(13) . . ? Si12 Si1 Si11 109.2(5) . . ? Si12 Si1 Ge1 110.5(4) . . ? Si11 Si1 Ge1 109.5(4) . . ? Si12 Si1 Si10 109.1(5) . . ? Si11 Si1 Si10 108.1(5) . . ? Ge1 Si1 Si10 110.4(4) . . ? Si22 Si2 Si20 114.3(5) . . ? Si22 Si2 Ge2 110.3(4) . . ? Si20 Si2 Ge2 106.4(5) . . ? Si22 Si2 Si21 107.3(6) . . ? Si20 Si2 Si21 112.2(6) . . ? Ge2 Si2 Si21 106.1(5) . . ? Si32 Si3 Si30 108.2(6) . . ? Si32 Si3 Si31 109.3(5) . . ? Si30 Si3 Si31 108.5(4) . . ? Si32 Si3 Ge3 108.6(4) . . ? Si30 Si3 Ge3 113.7(4) . . ? Si31 Si3 Ge3 108.5(4) . . ? C10C Si10 C10A 108.6(15) . . ? C10C Si10 C10B 109.4(14) . . ? C10A Si10 C10B 114.0(16) . . ? C10C Si10 Si1 111.3(10) . . ? C10A Si10 Si1 107.5(13) . . ? C10B Si10 Si1 106.0(10) . . ? C11A Si11 C11B 107.7(15) . . ? C11A Si11 C11C 117.5(17) . . ? C11B Si11 C11C 102.7(17) . . ? C11A Si11 Si1 115.0(11) . . ? C11B Si11 Si1 108.1(11) . . ? C11C Si11 Si1 105.0(14) . . ? C12B Si12 C12A 109.9(16) . . ? C12B Si12 C12C 101.1(17) . . ? C12A Si12 C12C 108.9(17) . . ? C12B Si12 Si1 113.6(14) . . ? C12A Si12 Si1 111.7(11) . . ? C12C Si12 Si1 111.1(12) . . ? C20C Si20 C20B 107(2) . . ? C20C Si20 C20A 117(2) . . ? C20B Si20 C20A 106.2(17) . . ? C20C Si20 Si2 114.8(15) . . ? C20B Si20 Si2 109.3(15) . . ? C20A Si20 Si2 102.7(16) . . ? C21C Si21 C21B 116.8(17) . . ? C21C Si21 C21A 99.4(19) . . ? C21B Si21 C21A 114.5(19) . . ? C21C Si21 Si2 113.2(13) . . ? C21B Si21 Si2 106.1(14) . . ? C21A Si21 Si2 106.5(13) . . ? C22A Si22 C22B 114.3(15) . . ? C22A Si22 C22C 111.9(16) . . ? C22B Si22 C22C 99.9(17) . . ? C22A Si22 Si2 111.1(10) . . ? C22B Si22 Si2 107.2(12) . . ? C22C Si22 Si2 111.9(13) . . ? C30C Si30 C30B 103(2) . . ? C30C Si30 C30A 119(2) . . ? C30B Si30 C30A 94.4(19) . . ? C30C Si30 Si3 111.0(15) . . ? C30B Si30 Si3 114.0(16) . . ? C30A Si30 Si3 113.7(14) . . ? C31C Si31 C31B 112.8(14) . . ? C31C Si31 C31A 111.5(13) . . ? C31B Si31 C31A 106.2(14) . . ? C31C Si31 Si3 107.2(9) . . ? C31B Si31 Si3 112.5(8) . . ? C31A Si31 Si3 106.6(12) . . ? C32B Si32 C32C 123(3) . . ? C32B Si32 C32A 100.7(15) . . ? C32C Si32 C32A 106(2) . . ? C32B Si32 Si3 112.0(15) . . ? C32C Si32 Si3 106.3(19) . . ? C32A Si32 Si3 107.9(12) . . ? O1 C1 Cr1 166(2) . . ? O1 C1 Ge6 116.1(19) . . ? Cr1 C1 Ge6 77.9(11) . . ? O2 C2 Cr1 175(2) . . ? O3 C3 Cr1 168(3) . . ? N2 C100 C101 122(3) . . ? N2 C100 Li1 49.3(18) . . ? C101 C100 Li1 78(2) . . ? C100 C101 N1 109(3) . . ? C201 C200 N4 109(5) . . ? C200 C201 N3 110(4) . . ? C302 C301 C300 127(5) . . ? C301 C302 C301 136(9) 2_565 . ? C102 N1 C103 103(4) . . ? C102 N1 C101 105(3) . . ? C103 N1 C101 98(3) . . ? C102 N1 Li1 125(3) . . ? C103 N1 Li1 116(3) . . ? C101 N1 Li1 105(2) . . ? C110 N2 C100 110(3) . . ? C110 N2 C104 99(3) . . ? C100 N2 C104 110(3) . . ? C110 N2 Li1 117(3) . . ? C100 N2 Li1 101(2) . . ? C104 N2 Li1 119(2) . . ? C202 N3 C203 111(3) . . ? C202 N3 C201 133(3) . . ? C203 N3 C201 98(2) . . ? C202 N3 Li1 115(3) . . ? C203 N3 Li1 103(2) . . ? C201 N3 Li1 92(2) . . ? C210 N4 C204 114(3) . . ? C210 N4 C200 110(3) . . ? C204 N4 C200 101(3) . . ? C210 N4 Li1 110(2) . . ? C204 N4 Li1 119(2) . . ? C200 N4 Li1 102(3) . . ? N1 Li1 N2 91(2) . . ? N1 Li1 N4 124(2) . . ? N2 Li1 N4 114(2) . . ? N1 Li1 N3 126(2) . . ? N2 Li1 N3 118(2) . . ? N4 Li1 N3 86.8(19) . . ? N1 Li1 C100 61.7(15) . . ? N2 Li1 C100 29.6(11) . . ? N4 Li1 C100 125(2) . . ? N3 Li1 C100 139(2) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 22.78 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.410 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.079