Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_m054 _database_code_CSD 186635 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Chen Yan-Min' ; Faculty of Chemistry, Quanzhou Normal College, Quanzhou 362000, P. R. China ; 'Wang En-Bo' ;Faculty of Chemistry, Institute of Polyoxometalate Chemistry, Northeast Normal University, Changchun 130024, P. R. China ; 'Lin Bi-Zhou' ; Institute of Materials Physical Chemistry, Huaqiao University, Quanzhou 362011, P. R. China ; 'Wang Shu-Tao' ; Faculty of Chemistry, Institute of Polyoxometalate Chemistry, Northeast Normal University, Changchun 130024, P. R. China ; _publ_contact_author_name 'Dr En-Bo Wang' _publ_contact_author_address ; Faculty of Chemistry Instirute of Poluoxometalate Chemistry Northeast Normal Universety Changchun 130024 P. R. China ; _publ_contact_author_phone '86-4315685085' _publ_contact_author_fax '86-4315647295' _publ_contact_author_email wangenbo@public.cc.jl.cn _publ_requested_journal 'Chemical Communications' #================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; First polyoxoalkoxovanadium germanate anion with a novel cage-like structure: solvothermal synthesis and structur characterization of [H2(V3O10)2(VO)3(Ge2O)3(L)6]2- (L=OCH2CH2O) ; #======================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H33 Ge6 N O39 V9' _chemical_formula_weight 1709.39 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' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 18.5773(6) _cell_length_b 22.7989(9) _cell_length_c 14.5097(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6145.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 63155 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 27.98 _exptl_crystal_description 'block' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.412 _exptl_crystal_size_mid 0.367 _exptl_crystal_size_min 0.313 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3292 _exptl_absorpt_coefficient_mu 4.265 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.158 _exptl_absorpt_correction_T_max 0.263 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '18 kW rotate anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_reflns_number 12985 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7129 _reflns_number_gt 3883 _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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00130(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7129 _refine_ls_number_parameters 334 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1665 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.04277(5) 0.29037(6) 0.0000 0.0468(3) Uani 1 2 d S . . Ge2 Ge 0.13602(7) 0.18540(6) 0.0000 0.0511(3) Uani 1 2 d S . . Ge3 Ge 0.25682(4) 0.41660(4) 0.19577(5) 0.0517(2) Uani 1 1 d . . . Ge4 Ge 0.35177(4) 0.31273(4) 0.19533(6) 0.0551(3) Uani 1 1 d . . . V1 V 0.09826(6) 0.39929(6) 0.11653(8) 0.0440(3) Uani 1 1 d . . . V2 V 0.36122(9) 0.39994(10) 0.0000 0.0541(5) Uani 1 2 d S . . V3 V 0.28392(7) 0.19544(6) 0.11519(9) 0.0493(3) Uani 1 1 d . . . V4 V 0.22358(10) 0.47503(9) 0.0000 0.0499(5) Uani 1 2 d S . . V5 V 0.16880(6) 0.28355(6) 0.17599(7) 0.0405(3) Uani 1 1 d . . . V6 V 0.41015(9) 0.27158(10) 0.0000 0.0574(6) Uani 1 2 d S . . O1 O 0.4301(4) 0.4416(4) 0.0000 0.080(3) Uani 1 2 d S . . O2 O 0.3897(3) 0.2171(3) 0.1074(4) 0.0643(16) Uani 1 1 d . . . O3 O 0.1529(3) 0.4753(2) 0.1074(3) 0.0553(14) Uani 1 1 d . . . O4 O 0.2878(3) 0.1452(3) 0.1909(4) 0.0730(17) Uani 1 1 d . . . O5 O 0.4169(3) 0.2822(3) 0.2658(5) 0.084(2) Uani 1 1 d . . . O6 O 0.2913(3) 0.4347(2) 0.0860(3) 0.0536(13) Uani 1 1 d . . . O7 O 0.2454(5) 0.5422(4) 0.0000 0.076(3) Uani 1 2 d S . . O8 O 0.4941(4) 0.2705(5) 0.0000 0.082(3) Uani 1 2 d S . . O9 O -0.0479(4) 0.3058(4) 0.0000 0.069(3) Uani 1 2 d S . . O10 O 0.2414(3) 0.4773(3) 0.2664(4) 0.0710(17) Uani 1 1 d . . . O11 O 0.2785(4) 0.1470(4) 0.0000 0.057(2) Uani 1 2 d SD . . O12 O 0.3256(3) 0.3772(2) 0.2513(4) 0.0579(14) Uani 1 1 d . . . O13 O 0.0887(2) 0.3129(2) 0.1000(3) 0.0412(11) Uani 1 1 d . . . O14 O 0.3827(2) 0.3344(2) 0.0868(4) 0.0549(14) Uani 1 1 d . . . O15 O 0.2740(2) 0.2703(2) 0.1854(3) 0.0463(12) Uani 1 1 d . . . O16 O 0.1340(3) 0.2627(3) 0.2700(3) 0.0561(14) Uani 1 1 d . . . O17 O 0.1239(6) 0.1092(4) 0.0000 0.084(3) Uani 1 2 d SD . . O18 O 0.0397(3) 0.4162(3) 0.1905(3) 0.0629(15) Uani 1 1 d . . . O19 O 0.1797(2) 0.2124(2) 0.0985(3) 0.0450(12) Uani 1 1 d . . . O20 O 0.0493(4) 0.2148(4) 0.0000 0.059(2) Uani 1 2 d S . . O21 O 0.0398(3) 0.4066(3) 0.0000 0.0493(19) Uani 1 2 d S . . O22 O 0.1827(2) 0.3695(2) 0.1869(3) 0.0445(12) Uani 1 1 d . . . O23 O 0.2952(3) 0.2554(3) 0.0000 0.0255(12) Uani 1 2 d S . . O24 O 0.1713(3) 0.3907(2) 0.0000 0.0220(11) Uani 1 2 d S . . C1 C -0.0700(8) 0.3627(10) 0.0423(12) 0.076(6) Uani 0.50 1 d P . . C2 C -0.0374(6) 0.4115(7) 0.0000 0.071(4) Uani 1 2 d S . . C3 C 0.1457(5) 0.5227(4) 0.1755(6) 0.070(3) Uani 1 1 d . . . C4 C 0.1667(6) 0.4999(5) 0.2710(6) 0.082(3) Uani 1 1 d . . . C5 C 0.4388(9) 0.2259(8) 0.2525(12) 0.197(10) Uani 1 1 d . . . C6 C 0.4442(5) 0.1963(6) 0.1699(7) 0.093(4) Uani 1 1 d . . . C7 C 0.2674(16) 0.0800(8) 0.0000 0.183(11) Uani 1 2 d SD . . C8 C 0.1856(14) 0.0723(16) 0.018(4) 0.36(2) Uiso 0.50 1 d PD . . OW1 O 0.2418(13) 0.2497(11) 0.5000 0.122(8) Uiso 0.50 2 d SP . . OW2 O 0.6590(13) 0.2507(12) 0.0000 0.130(9) Uiso 0.50 2 d SP . . N3 N 0.5798(10) 0.4114(9) 0.2056(14) 0.116(7) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0340(5) 0.0680(9) 0.0382(5) 0.000 0.000 -0.0083(5) Ge2 0.0662(7) 0.0425(7) 0.0447(6) 0.000 0.000 -0.0131(6) Ge3 0.0603(5) 0.0487(5) 0.0462(4) -0.0077(4) -0.0130(3) -0.0033(4) Ge4 0.0442(4) 0.0651(6) 0.0560(5) 0.0020(5) -0.0183(3) 0.0013(4) V1 0.0430(6) 0.0532(9) 0.0358(6) -0.0042(6) 0.0017(5) 0.0086(6) V2 0.0388(9) 0.0568(13) 0.0666(12) 0.000 0.000 -0.0113(9) V3 0.0583(7) 0.0436(8) 0.0461(7) 0.0054(6) -0.0049(6) 0.0083(6) V4 0.0602(11) 0.0392(11) 0.0502(10) 0.000 0.000 -0.0017(9) V5 0.0442(6) 0.0466(8) 0.0307(5) 0.0029(6) -0.0012(4) -0.0007(6) V6 0.0324(8) 0.0736(16) 0.0661(12) 0.000 0.000 0.0096(9) O1 0.056(5) 0.094(7) 0.088(6) 0.000 0.000 -0.033(5) O2 0.050(3) 0.077(4) 0.066(4) 0.006(3) -0.013(2) 0.021(3) O3 0.072(3) 0.046(3) 0.048(3) -0.009(3) 0.000(2) 0.011(3) O4 0.098(4) 0.055(4) 0.066(4) 0.016(3) -0.009(3) 0.013(3) O5 0.070(4) 0.093(5) 0.090(5) -0.005(4) -0.045(3) 0.013(4) O6 0.052(3) 0.052(4) 0.056(3) -0.004(3) -0.007(2) -0.010(3) O7 0.108(7) 0.041(5) 0.077(6) 0.000 0.000 -0.020(5) O8 0.036(4) 0.126(9) 0.086(6) 0.000 0.000 0.006(5) O9 0.035(4) 0.110(8) 0.060(5) 0.000 0.000 -0.009(4) O10 0.096(4) 0.060(4) 0.057(3) -0.020(3) -0.018(3) -0.001(4) O11 0.074(5) 0.039(5) 0.060(5) 0.000 0.000 0.008(4) O12 0.057(3) 0.061(4) 0.055(3) -0.008(3) -0.020(2) 0.000(3) O13 0.036(2) 0.050(3) 0.037(2) 0.003(2) -0.0006(18) -0.002(2) O14 0.039(3) 0.060(4) 0.065(3) 0.001(3) -0.012(2) -0.003(2) O15 0.044(2) 0.053(3) 0.042(3) 0.001(2) -0.0048(19) 0.004(2) O16 0.061(3) 0.070(4) 0.036(3) 0.008(3) 0.007(2) -0.005(3) O17 0.132(8) 0.050(6) 0.071(6) 0.000 0.000 -0.021(6) O18 0.065(3) 0.071(4) 0.052(3) -0.006(3) 0.009(2) 0.016(3) O19 0.054(3) 0.043(3) 0.038(2) 0.003(2) 0.000(2) -0.004(2) O20 0.052(4) 0.076(6) 0.049(4) 0.000 0.000 -0.021(4) O21 0.038(3) 0.066(5) 0.044(4) 0.000 0.000 0.024(3) O22 0.056(3) 0.043(3) 0.035(2) -0.001(2) -0.0083(19) 0.005(2) O23 0.024(3) 0.026(3) 0.027(3) 0.000 0.000 0.003(2) O24 0.023(2) 0.024(3) 0.019(2) 0.000 0.000 -0.001(2) C1 0.039(8) 0.109(17) 0.078(11) 0.002(12) 0.013(7) 0.003(9) C2 0.039(6) 0.103(12) 0.070(8) 0.000 0.000 0.018(7) C3 0.099(7) 0.060(6) 0.052(5) -0.016(5) -0.013(4) 0.019(5) C4 0.103(7) 0.082(8) 0.062(5) -0.027(6) -0.019(5) 0.027(6) C5 0.217(16) 0.205(18) 0.168(14) -0.092(14) -0.142(13) 0.160(15) C6 0.075(6) 0.132(11) 0.072(6) 0.007(7) -0.031(5) 0.040(6) C7 0.30(3) 0.18(3) 0.064(11) 0.000 0.000 0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O9 1.720(7) . ? Ge1 O20 1.726(9) . ? Ge1 O13 1.759(4) . ? Ge1 O13 1.759(4) 6 ? Ge2 O20 1.746(8) . ? Ge2 O19 1.754(5) . ? Ge2 O19 1.754(5) 6 ? Ge2 O17 1.751(9) . ? Ge3 O10 1.746(6) . ? Ge3 O22 1.751(5) . ? Ge3 O12 1.758(5) . ? Ge3 O6 1.765(5) . ? Ge4 O5 1.731(6) . ? Ge4 O12 1.747(6) . ? Ge4 O14 1.747(5) . ? Ge4 O15 1.745(5) . ? V1 O18 1.576(5) . ? V1 O22 1.991(4) . ? V1 O13 1.992(5) . ? V1 O3 2.012(6) . ? V1 O21 2.016(3) . ? V1 O24 2.177(3) . ? V1 V5 3.0699(18) . ? V2 O1 1.594(8) . ? V2 O6 1.968(5) . ? V2 O6 1.968(5) 6 ? V2 O14 1.995(6) 6 ? V2 O14 1.995(6) . ? V2 V6 3.064(3) . ? V2 V4 3.077(3) . ? V3 O4 1.588(6) . ? V3 O15 1.997(5) . ? V3 O19 1.990(5) . ? V3 O11 2.005(5) . ? V3 O2 2.028(5) . ? V3 O23 2.169(4) . ? V3 V5 3.0639(18) . ? V4 O7 1.584(8) . ? V4 O6 1.996(5) 6 ? V4 O6 1.996(5) . ? V4 O3 2.038(5) 6 ? V4 O3 2.038(5) . ? V4 O24 2.153(6) . ? V5 O16 1.582(5) . ? V5 O13 1.970(4) . ? V5 O15 1.982(4) . ? V5 O19 1.984(5) . ? V5 O22 1.983(5) . ? V6 O8 1.559(7) . ? V6 O14 1.974(6) . ? V6 O14 1.974(6) 6 ? V6 O2 2.029(6) 6 ? V6 O2 2.029(6) . ? V6 O23 2.168(5) . ? O2 C6 1.440(9) . ? O3 C3 1.472(10) . ? O5 C5 1.359(15) . ? O9 C1 1.49(2) . ? O9 C1 1.49(2) 6 ? O10 C4 1.482(11) . ? O11 C7 1.543(17) . ? O11 V3 2.005(5) 6 ? O17 C8 1.446(19) 6 ? O17 C8 1.446(19) . ? O21 C2 1.439(11) . ? O21 V1 2.016(3) 6 ? O23 V3 2.169(4) 6 ? O24 V1 2.177(3) 6 ? C1 C1 1.23(4) 6 ? C1 C2 1.41(2) . ? C2 C1 1.41(2) 6 ? C3 C4 1.531(12) . ? C5 C6 1.380(17) . ? C7 C8 1.549(19) . ? C7 C8 1.549(19) 6 ? C8 C8 0.51(11) 6 ? OW1 OW2 1.54(3) 7_566 ? OW2 OW1 1.54(3) 7_665 ? 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 O9 Ge1 O20 105.8(4) . . ? O9 Ge1 O13 114.5(2) . . ? O20 Ge1 O13 104.9(2) . . ? O9 Ge1 O13 114.5(2) . 6 ? O20 Ge1 O13 104.9(2) . 6 ? O13 Ge1 O13 111.1(3) . 6 ? O20 Ge2 O19 107.0(2) . . ? O20 Ge2 O19 107.0(2) . 6 ? O19 Ge2 O19 109.0(3) . 6 ? O20 Ge2 O17 105.2(4) . . ? O19 Ge2 O17 114.1(2) . . ? O19 Ge2 O17 114.1(2) 6 . ? O10 Ge3 O22 113.6(3) . . ? O10 Ge3 O12 104.8(3) . . ? O22 Ge3 O12 107.0(2) . . ? O10 Ge3 O6 113.8(3) . . ? O22 Ge3 O6 111.2(2) . . ? O12 Ge3 O6 105.6(2) . . ? O5 Ge4 O12 105.0(3) . . ? O5 Ge4 O14 114.6(3) . . ? O12 Ge4 O14 105.8(3) . . ? O5 Ge4 O15 113.9(3) . . ? O12 Ge4 O15 105.9(2) . . ? O14 Ge4 O15 110.8(2) . . ? O18 V1 O22 106.1(2) . . ? O18 V1 O13 105.2(3) . . ? O22 V1 O13 78.19(19) . . ? O18 V1 O3 100.5(3) . . ? O22 V1 O3 86.0(2) . . ? O13 V1 O3 152.7(2) . . ? O18 V1 O21 100.4(2) . . ? O22 V1 O21 151.9(2) . . ? O13 V1 O21 86.1(3) . . ? O3 V1 O21 98.4(3) . . ? O18 V1 O24 168.9(3) . . ? O22 V1 O24 82.92(17) . . ? O13 V1 O24 82.74(19) . . ? O3 V1 O24 73.2(2) . . ? O21 V1 O24 72.05(17) . . ? O18 V1 V5 108.2(2) . . ? O22 V1 V5 39.33(15) . . ? O13 V1 V5 38.96(12) . . ? O3 V1 V5 122.90(15) . . ? O21 V1 V5 122.4(2) . . ? O24 V1 V5 82.83(14) . . ? O1 V2 O6 106.9(3) . . ? O1 V2 O6 106.9(3) . 6 ? O6 V2 O6 78.7(3) . 6 ? O1 V2 O14 106.6(3) . 6 ? O6 V2 O14 146.5(2) . 6 ? O6 V2 O14 91.9(2) 6 6 ? O1 V2 O14 106.6(3) . . ? O6 V2 O14 91.9(2) . . ? O6 V2 O14 146.5(2) 6 . ? O14 V2 O14 78.3(3) 6 . ? O1 V2 V6 109.3(4) . . ? O6 V2 V6 125.45(17) . . ? O6 V2 V6 125.45(17) 6 . ? O14 V2 V6 39.22(16) 6 . ? O14 V2 V6 39.22(16) . . ? O1 V2 V4 109.6(4) . . ? O6 V2 V4 39.41(15) . . ? O6 V2 V4 39.41(15) 6 . ? O14 V2 V4 125.65(15) 6 . ? O14 V2 V4 125.65(15) . . ? V6 V2 V4 141.06(8) . . ? O4 V3 O15 105.5(3) . . ? O4 V3 O19 105.6(3) . . ? O15 V3 O19 78.81(19) . . ? O4 V3 O11 100.5(3) . . ? O15 V3 O11 153.1(2) . . ? O19 V3 O11 87.5(3) . . ? O4 V3 O2 99.8(3) . . ? O15 V3 O2 84.9(2) . . ? O19 V3 O2 152.7(2) . . ? O11 V3 O2 97.8(3) . . ? O4 V3 O23 169.4(3) . . ? O15 V3 O23 82.17(18) . . ? O19 V3 O23 82.94(19) . . ? O11 V3 O23 73.1(2) . . ? O2 V3 O23 73.2(2) . . ? O4 V3 V5 107.8(2) . . ? O15 V3 V5 39.46(13) . . ? O19 V3 V5 39.49(14) . . ? O11 V3 V5 124.5(2) . . ? O2 V3 V5 122.19(18) . . ? O23 V3 V5 82.87(13) . . ? O7 V4 O6 106.6(3) . 6 ? O7 V4 O6 106.6(3) . . ? O6 V4 O6 77.4(3) 6 . ? O7 V4 O3 99.3(3) . 6 ? O6 V4 O3 85.9(2) 6 6 ? O6 V4 O3 152.3(2) . 6 ? O7 V4 O3 99.3(3) . . ? O6 V4 O3 152.3(2) 6 . ? O6 V4 O3 85.9(2) . . ? O3 V4 O3 99.8(3) 6 . ? O7 V4 O24 168.0(4) . . ? O6 V4 O24 82.67(19) 6 . ? O6 V4 O24 82.67(19) . . ? O3 V4 O24 73.25(18) 6 . ? O3 V4 O24 73.25(18) . . ? O7 V4 V2 109.0(4) . . ? O6 V4 V2 38.74(15) 6 . ? O6 V4 V2 38.74(15) . . ? O3 V4 V2 122.48(16) 6 . ? O3 V4 V2 122.48(16) . . ? O24 V4 V2 83.00(15) . . ? O16 V5 O13 106.0(2) . . ? O16 V5 O15 107.3(2) . . ? O13 V5 O15 146.68(19) . . ? O16 V5 O19 106.6(3) . . ? O13 V5 O19 92.1(2) . . ? O15 V5 O19 79.3(2) . . ? O16 V5 O22 106.3(3) . . ? O13 V5 O22 78.88(19) . . ? O15 V5 O22 91.0(2) . . ? O19 V5 O22 147.13(19) . . ? O16 V5 V3 109.7(2) . . ? O13 V5 V3 126.09(14) . . ? O15 V5 V3 39.81(15) . . ? O19 V5 V3 39.62(14) . . ? O22 V5 V3 125.47(14) . . ? O16 V5 V1 109.0(2) . . ? O13 V5 V1 39.47(14) . . ? O15 V5 V1 124.84(16) . . ? O19 V5 V1 125.93(14) . . ? O22 V5 V1 39.50(13) . . ? V3 V5 V1 141.31(5) . . ? O8 V6 O14 105.7(3) . . ? O8 V6 O14 105.7(3) . 6 ? O14 V6 O14 79.3(3) . 6 ? O8 V6 O2 100.3(3) . 6 ? O14 V6 O2 152.3(2) . 6 ? O14 V6 O2 84.6(2) 6 6 ? O8 V6 O2 100.3(3) . . ? O14 V6 O2 84.6(2) . . ? O14 V6 O2 152.3(2) 6 . ? O2 V6 O2 100.3(4) 6 . ? O8 V6 O23 169.3(4) . . ? O14 V6 O23 82.46(18) . . ? O14 V6 O23 82.46(18) 6 . ? O2 V6 O23 73.19(17) 6 . ? O2 V6 O23 73.19(17) . . ? O8 V6 V2 108.2(4) . . ? O14 V6 V2 39.70(16) . . ? O14 V6 V2 39.70(16) 6 . ? O2 V6 V2 121.96(17) 6 . ? O2 V6 V2 121.96(17) . . ? O23 V6 V2 82.55(16) . . ? C6 O2 V3 124.5(6) . . ? C6 O2 V6 123.6(6) . . ? V3 O2 V6 111.9(2) . . ? C3 O3 V1 122.9(5) . . ? C3 O3 V4 125.0(5) . . ? V1 O3 V4 111.9(2) . . ? C5 O5 Ge4 120.4(6) . . ? Ge3 O6 V2 135.9(3) . . ? Ge3 O6 V4 116.3(3) . . ? V2 O6 V4 101.8(2) . . ? C1 O9 C1 48.5(15) . 6 ? C1 O9 Ge1 116.6(8) . . ? C1 O9 Ge1 116.6(8) 6 . ? C4 O10 Ge3 117.1(5) . . ? C7 O11 V3 123.5(2) . . ? C7 O11 V3 123.5(2) . 6 ? V3 O11 V3 112.9(4) . 6 ? Ge4 O12 Ge3 114.8(3) . . ? Ge1 O13 V5 136.8(3) . . ? Ge1 O13 V1 115.6(2) . . ? V5 O13 V1 101.6(2) . . ? Ge4 O14 V6 117.1(3) . . ? Ge4 O14 V2 135.7(3) . . ? V6 O14 V2 101.1(2) . . ? Ge4 O15 V5 137.5(3) . . ? Ge4 O15 V3 116.1(2) . . ? V5 O15 V3 100.7(2) . . ? C8 O17 C8 20(5) 6 . ? C8 O17 Ge2 118.4(18) 6 . ? C8 O17 Ge2 118.4(18) . . ? Ge2 O19 V5 134.6(3) . . ? Ge2 O19 V3 118.7(3) . . ? V5 O19 V3 100.9(2) . . ? Ge1 O20 Ge2 116.6(4) . . ? C2 O21 V1 122.91(15) . 6 ? C2 O21 V1 122.91(15) . . ? V1 O21 V1 114.0(3) 6 . ? Ge3 O22 V1 116.6(3) . . ? Ge3 O22 V5 135.6(3) . . ? V1 O22 V5 101.2(2) . . ? V3 O23 V3 100.8(2) 6 . ? V3 O23 V6 101.66(17) 6 . ? V3 O23 V6 101.66(17) . . ? V4 O24 V1 101.60(19) . . ? V4 O24 V1 101.60(19) . 6 ? V1 O24 V1 101.9(2) . 6 ? C1 C1 C2 64.2(8) 6 . ? C1 C1 O9 65.8(7) 6 . ? C2 C1 O9 112.9(12) . . ? C1 C2 C1 51.7(16) 6 . ? C1 C2 O21 111.6(11) 6 . ? C1 C2 O21 111.6(11) . . ? O3 C3 C4 109.5(7) . . ? O10 C4 C3 108.4(8) . . ? C6 C5 O5 127.3(14) . . ? C5 C6 O2 109.6(9) . . ? O11 C7 C8 104(2) . . ? O11 C7 C8 104(2) . 6 ? C8 C7 C8 19(4) . 6 ? C8 C8 O17 80(2) 6 . ? C8 C8 C7 81(2) 6 . ? O17 C8 C7 133(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.995 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.196