# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email 962403601@cc.ncu.edu.tw _publ_contact_author_name 'Nguyen Quang Bac' loop_ _publ_author_name 'Quang Bac Nguyen' 'Kwang-Hwa Lii' data_1 _database_code_depnum_ccdc_archive 'CCDC 835664' #TrackingRef 'AmNbGeO.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'F Ge6 H2 Nb O16, C8 H24 N4' _chemical_formula_sum 'C8 H26 F Ge6 N4 Nb O16' _chemical_formula_weight 981.87 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 9.8678(3) _cell_length_b 14.3940(5) _cell_length_c 16.6338(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2362.62(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9705 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.31 _exptl_crystal_description Paralellepiped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 8.087 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6447 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24557 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5672 _reflns_number_gt 5431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0245P)^2^+1.8629P] 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 SHELXL _refine_ls_extinction_coef 0.00022(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.030(7) _refine_ls_number_reflns 5672 _refine_ls_number_parameters 326 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0498 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 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 Nb1 Nb 0.47749(3) 0.260006(19) 0.35991(2) 0.01779(7) Uani 1 1 d . . . Ge1 Ge 0.37115(4) 0.06936(2) 0.44769(2) 0.01417(8) Uani 1 1 d . . . Ge2 Ge 0.67252(3) 0.10782(2) 0.44971(2) 0.01410(8) Uani 1 1 d . . . Ge3 Ge 0.28717(4) 0.38631(2) 0.47882(2) 0.01571(8) Uani 1 1 d . . . Ge4 Ge 0.59040(4) 0.42699(2) 0.47648(2) 0.01506(8) Uani 1 1 d . . . Ge5 Ge 0.34061(4) 0.21353(2) 0.58247(2) 0.01598(8) Uani 1 1 d . . . Ge6 Ge 0.62581(4) 0.25237(2) 0.58103(2) 0.01605(8) Uani 1 1 d . . . F1 F 0.4835(2) 0.24113(16) 0.50138(16) 0.0279(5) Uani 1 1 d . . . O1 O 0.5367(2) 0.03351(16) 0.47423(17) 0.0182(5) Uani 1 1 d . . . O2 O 0.3673(2) 0.14518(17) 0.36808(16) 0.0185(5) Uani 1 1 d . . . O3 O 0.3034(3) -0.03699(17) 0.41588(16) 0.0208(6) Uani 1 1 d . . . O4 O 0.2908(3) 0.10730(18) 0.53480(16) 0.0216(6) Uani 1 1 d . . . O5 O 0.7303(3) 0.16420(19) 0.53554(16) 0.0218(6) Uani 1 1 d . . . O6 O 0.6419(2) 0.17920(16) 0.36864(15) 0.0175(5) Uani 1 1 d . . . O7 O 0.2377(3) 0.31038(18) 0.55551(16) 0.0226(6) Uani 1 1 d . . . O8 O 0.3152(3) 0.33392(18) 0.38748(16) 0.0190(5) Uani 1 1 d . . . O9 O 0.1497(3) 0.45966(18) 0.4715(2) 0.0308(7) Uani 1 1 d . . . O10 O 0.4251(3) 0.45376(18) 0.50976(17) 0.0204(5) Uani 1 1 d . . . O11 O 0.5922(3) 0.37033(17) 0.38545(15) 0.0181(5) Uani 1 1 d . . . O12 O 0.6768(3) 0.36681(18) 0.55227(16) 0.0198(6) Uani 1 1 d . . . O13 O 0.4858(3) 0.22686(19) 0.64644(16) 0.0212(6) Uani 1 1 d . . . O14 O 0.2307(3) 0.18121(19) 0.66545(16) 0.0249(6) Uani 1 1 d . . . H14A H 0.1829 0.2256 0.6777 0.037 Uiso 1 1 calc R . . O15 O 0.7422(3) 0.25488(18) 0.66545(16) 0.0233(6) Uani 1 1 d . . . H15A H 0.8134 0.2295 0.6527 0.028 Uiso 1 1 calc R . . O16 O 0.4715(3) 0.27287(19) 0.25637(17) 0.0264(6) Uani 1 1 d . . . N1 N -0.0145(4) 0.1104(3) 0.6158(3) 0.0438(11) Uani 1 1 d . . . H1C H -0.0770 0.1489 0.5965 0.066 Uiso 1 1 calc R . . H1D H 0.0142 0.0730 0.5767 0.066 Uiso 1 1 calc R . . H1E H 0.0551 0.1431 0.6348 0.066 Uiso 1 1 calc R . . N2 N 0.0428(4) -0.1561(2) 0.7993(2) 0.0287(8) Uani 1 1 d . . . H2C H 0.1178 -0.1692 0.7756 0.034 Uiso 1 1 calc R . . N3 N 0.1034(5) -0.3531(4) 0.8103(3) 0.0572(13) Uani 1 1 d . . . H3C H 0.1823 -0.3509 0.7883 0.069 Uiso 1 1 calc R . . N4 N -0.0475(5) -0.6093(3) 0.6314(3) 0.0431(11) Uani 1 1 d . . . H4C H -0.1239 -0.6364 0.6153 0.065 Uiso 1 1 calc R . . H4D H 0.0064 -0.6514 0.6539 0.065 Uiso 1 1 calc R . . H4E H -0.0058 -0.5841 0.5892 0.065 Uiso 1 1 calc R . . C1 C -0.0741(4) 0.0538(3) 0.6818(3) 0.0315(10) Uani 1 1 d . . . H1A H -0.1507 0.0189 0.6611 0.038 Uiso 1 1 calc R . . H1B H -0.1071 0.0948 0.7237 0.038 Uiso 1 1 calc R . . C2 C 0.0272(4) -0.0122(3) 0.7168(3) 0.0293(10) Uani 1 1 d . . . H2A H 0.1008 0.0225 0.7411 0.035 Uiso 1 1 calc R . . H2B H 0.0647 -0.0507 0.6745 0.035 Uiso 1 1 calc R . . C3 C -0.0391(5) -0.0734(3) 0.7798(3) 0.0329(10) Uani 1 1 d . . . H3A H -0.0531 -0.0373 0.8284 0.039 Uiso 1 1 calc R . . H3B H -0.1271 -0.0932 0.7604 0.039 Uiso 1 1 calc R . . C4 C -0.0170(5) -0.2145(3) 0.8640(3) 0.0379(10) Uani 1 1 d . . . H4A H -0.1077 -0.2333 0.8484 0.045 Uiso 1 1 calc R . . H4B H -0.0241 -0.1781 0.9129 0.045 Uiso 1 1 calc R . . C5 C 0.0665(5) -0.2988(3) 0.8799(3) 0.0394(12) Uani 1 1 d . . . H5A H 0.1490 -0.2795 0.9069 0.047 Uiso 1 1 calc R . . H5B H 0.0170 -0.3385 0.9167 0.047 Uiso 1 1 calc R . . C6 C -0.0037(7) -0.4107(5) 0.7816(4) 0.066(2) Uani 1 1 d . . . H6A H -0.0711 -0.3713 0.7563 0.079 Uiso 1 1 calc R . . H6B H -0.0465 -0.4402 0.8275 0.079 Uiso 1 1 calc R . . C7 C 0.0367(7) -0.4860(4) 0.7222(3) 0.0544(16) Uani 1 1 d . . . H7A H 0.0856 -0.4581 0.6777 0.065 Uiso 1 1 calc R . . H7B H 0.0967 -0.5299 0.7484 0.065 Uiso 1 1 calc R . . C8 C -0.0798(6) -0.5345(4) 0.6917(4) 0.0546(15) Uani 1 1 d . . . H8A H -0.1403 -0.4898 0.6669 0.066 Uiso 1 1 calc R . . H8B H -0.1277 -0.5624 0.7365 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.01657(15) 0.01234(13) 0.02445(17) -0.00139(14) -0.00055(14) -0.00127(12) Ge1 0.01272(16) 0.01091(16) 0.01888(19) -0.00018(14) 0.00236(15) -0.00135(13) Ge2 0.01214(16) 0.01130(16) 0.01884(19) 0.00039(14) 0.00089(15) 0.00124(13) Ge3 0.01257(16) 0.01090(16) 0.0237(2) -0.00061(15) -0.00278(15) 0.00149(13) Ge4 0.01359(17) 0.01100(16) 0.02059(19) -0.00084(14) -0.00290(15) -0.00184(13) Ge5 0.01665(17) 0.01440(17) 0.01688(18) 0.00012(15) 0.00077(17) 0.00221(14) Ge6 0.01604(18) 0.01508(16) 0.01701(19) -0.00005(15) -0.00123(16) 0.00217(13) F1 0.0245(12) 0.0296(13) 0.0295(13) -0.0009(10) -0.0004(10) -0.0009(10) O1 0.0132(11) 0.0128(11) 0.0285(14) 0.0048(11) 0.0008(11) -0.0003(9) O2 0.0201(13) 0.0153(12) 0.0200(13) 0.0009(11) -0.0027(11) -0.0030(10) O3 0.0180(12) 0.0140(12) 0.0303(15) -0.0038(11) 0.0067(11) -0.0071(10) O4 0.0214(14) 0.0175(13) 0.0260(15) -0.0027(11) 0.0077(12) -0.0038(10) O5 0.0181(13) 0.0226(13) 0.0247(15) -0.0048(11) -0.0056(11) 0.0067(11) O6 0.0198(12) 0.0144(11) 0.0184(13) 0.0037(10) 0.0028(11) 0.0030(10) O7 0.0165(12) 0.0203(13) 0.0311(15) 0.0069(11) 0.0078(11) 0.0067(11) O8 0.0181(13) 0.0170(13) 0.0220(14) -0.0022(10) -0.0037(10) 0.0032(10) O9 0.0199(13) 0.0154(13) 0.057(2) -0.0044(14) -0.0124(14) 0.0080(10) O10 0.0150(12) 0.0165(12) 0.0297(15) -0.0077(11) -0.0024(11) -0.0018(10) O11 0.0208(13) 0.0159(12) 0.0176(13) -0.0014(10) -0.0015(10) -0.0041(10) O12 0.0191(13) 0.0177(13) 0.0225(14) -0.0005(11) -0.0070(11) -0.0025(10) O13 0.0228(14) 0.0269(14) 0.0139(13) 0.0046(11) -0.0011(11) -0.0029(12) O14 0.0258(15) 0.0272(15) 0.0217(14) 0.0041(11) 0.0095(12) 0.0070(12) O15 0.0221(14) 0.0278(14) 0.0201(14) 0.0013(11) -0.0094(11) 0.0054(12) O16 0.0344(17) 0.0231(14) 0.0216(16) -0.0024(11) -0.0005(12) -0.0067(12) N1 0.032(2) 0.051(3) 0.049(3) 0.018(2) -0.009(2) 0.0001(19) N2 0.0299(19) 0.0313(19) 0.0249(19) 0.0020(15) 0.0040(15) -0.0035(16) N3 0.063(3) 0.054(3) 0.055(3) -0.005(2) 0.003(3) -0.004(3) N4 0.058(3) 0.029(2) 0.042(3) 0.0091(18) -0.017(2) -0.0188(19) C1 0.027(2) 0.030(2) 0.037(3) -0.0048(19) -0.0007(19) -0.0042(19) C2 0.029(2) 0.028(2) 0.031(3) -0.0080(18) -0.0010(19) -0.0031(18) C3 0.036(2) 0.030(2) 0.033(3) -0.0068(18) -0.004(2) -0.0022(19) C4 0.035(2) 0.038(2) 0.041(3) 0.008(2) 0.007(2) -0.011(2) C5 0.055(3) 0.035(2) 0.028(3) 0.0072(19) -0.002(2) -0.014(2) C6 0.089(5) 0.069(4) 0.040(3) 0.005(3) 0.004(3) -0.048(4) C7 0.087(5) 0.042(3) 0.034(3) 0.005(2) 0.002(3) -0.017(3) C8 0.055(4) 0.060(4) 0.048(4) 0.014(3) 0.002(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O16 1.733(3) . ? Nb1 O8 1.977(3) . ? Nb1 O2 1.983(2) . ? Nb1 O11 1.996(2) . ? Nb1 O6 2.002(2) . ? Nb1 F1 2.370(3) . ? Ge1 O2 1.716(3) . ? Ge1 O4 1.739(3) . ? Ge1 O3 1.752(2) . ? Ge1 O1 1.769(2) . ? Ge2 O6 1.722(2) . ? Ge2 O5 1.738(3) . ? Ge2 O3 1.739(2) 3 ? Ge2 O1 1.763(2) . ? Ge3 O8 1.719(3) . ? Ge3 O9 1.724(3) . ? Ge3 O7 1.749(3) . ? Ge3 O10 1.750(3) . ? Ge4 O11 1.720(3) . ? Ge4 O9 1.735(3) 3_565 ? Ge4 O12 1.751(3) . ? Ge4 O10 1.765(3) . ? Ge5 O7 1.782(3) . ? Ge5 O4 1.791(3) . ? Ge5 O13 1.795(3) . ? Ge5 O14 1.816(3) . ? Ge5 F1 1.991(2) . ? Ge5 Ge6 2.8694(5) . ? Ge6 O12 1.788(3) . ? Ge6 O13 1.796(3) . ? Ge6 O5 1.802(3) . ? Ge6 O15 1.814(3) . ? Ge6 F1 1.937(2) . ? O3 Ge2 1.739(2) 3_455 ? O9 Ge4 1.735(3) 3_465 ? O14 H14A 0.8200 . ? O15 H15A 0.8200 . ? N1 C1 1.488(6) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N2 C3 1.474(6) . ? N2 C4 1.487(6) . ? N2 H2C 0.8600 . ? N3 C6 1.426(7) . ? N3 C5 1.444(7) . ? N3 H3C 0.8600 . ? N4 C8 1.506(7) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? C1 C2 1.497(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.517(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.491(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.520(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.438(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O16 Nb1 O8 98.36(13) . . ? O16 Nb1 O2 97.95(12) . . ? O8 Nb1 O2 89.35(10) . . ? O16 Nb1 O11 98.39(12) . . ? O8 Nb1 O11 88.97(11) . . ? O2 Nb1 O11 163.64(11) . . ? O16 Nb1 O6 99.31(12) . . ? O8 Nb1 O6 162.32(11) . . ? O2 Nb1 O6 87.42(10) . . ? O11 Nb1 O6 89.26(10) . . ? O16 Nb1 F1 179.31(11) . . ? O8 Nb1 F1 81.47(10) . . ? O2 Nb1 F1 81.38(9) . . ? O11 Nb1 F1 82.28(9) . . ? O6 Nb1 F1 80.85(9) . . ? O2 Ge1 O4 115.66(12) . . ? O2 Ge1 O3 108.31(12) . . ? O4 Ge1 O3 110.60(12) . . ? O2 Ge1 O1 113.47(12) . . ? O4 Ge1 O1 107.73(13) . . ? O3 Ge1 O1 99.95(12) . . ? O6 Ge2 O5 114.97(12) . . ? O6 Ge2 O3 103.09(12) . 3 ? O5 Ge2 O3 107.22(13) . 3 ? O6 Ge2 O1 114.20(12) . . ? O5 Ge2 O1 110.03(13) . . ? O3 Ge2 O1 106.49(12) 3 . ? O8 Ge3 O9 109.45(14) . . ? O8 Ge3 O7 114.54(13) . . ? O9 Ge3 O7 102.38(14) . . ? O8 Ge3 O10 112.24(13) . . ? O9 Ge3 O10 107.06(13) . . ? O7 Ge3 O10 110.45(14) . . ? O11 Ge4 O9 113.60(14) . 3_565 ? O11 Ge4 O12 113.20(13) . . ? O9 Ge4 O12 109.59(13) 3_565 . ? O11 Ge4 O10 112.93(12) . . ? O9 Ge4 O10 96.95(13) 3_565 . ? O12 Ge4 O10 109.40(13) . . ? O7 Ge5 O4 113.58(13) . . ? O7 Ge5 O13 121.36(13) . . ? O4 Ge5 O13 124.93(13) . . ? O7 Ge5 O14 92.95(12) . . ? O4 Ge5 O14 87.37(12) . . ? O13 Ge5 O14 93.07(13) . . ? O7 Ge5 F1 94.42(11) . . ? O4 Ge5 F1 93.71(11) . . ? O13 Ge5 F1 79.33(11) . . ? O14 Ge5 F1 171.41(12) . . ? O7 Ge5 Ge6 113.85(9) . . ? O4 Ge5 Ge6 115.57(8) . . ? O13 Ge5 Ge6 36.98(9) . . ? O14 Ge5 Ge6 129.93(9) . . ? F1 Ge5 Ge6 42.35(7) . . ? O12 Ge6 O13 124.54(13) . . ? O12 Ge6 O5 112.06(13) . . ? O13 Ge6 O5 123.39(13) . . ? O12 Ge6 O15 90.61(12) . . ? O13 Ge6 O15 91.26(13) . . ? O5 Ge6 O15 88.69(12) . . ? O12 Ge6 F1 95.63(11) . . ? O13 Ge6 F1 80.78(11) . . ? O5 Ge6 F1 93.93(11) . . ? O15 Ge6 F1 171.76(12) . . ? O12 Ge6 Ge5 117.26(9) . . ? O13 Ge6 Ge5 36.95(9) . . ? O5 Ge6 Ge5 115.30(9) . . ? O15 Ge6 Ge5 128.18(10) . . ? F1 Ge6 Ge5 43.83(7) . . ? Ge6 F1 Ge5 93.83(11) . . ? Ge6 F1 Nb1 133.45(12) . . ? Ge5 F1 Nb1 132.67(12) . . ? Ge2 O1 Ge1 117.87(13) . . ? Ge1 O2 Nb1 124.81(14) . . ? Ge2 O3 Ge1 134.26(16) 3_455 . ? Ge1 O4 Ge5 120.78(14) . . ? Ge2 O5 Ge6 119.10(14) . . ? Ge2 O6 Nb1 123.06(13) . . ? Ge3 O7 Ge5 120.88(14) . . ? Ge3 O8 Nb1 124.86(14) . . ? Ge3 O9 Ge4 146.92(17) . 3_465 ? Ge3 O10 Ge4 120.37(15) . . ? Ge4 O11 Nb1 123.96(14) . . ? Ge4 O12 Ge6 120.75(14) . . ? Ge5 O13 Ge6 106.07(14) . . ? Ge5 O14 H14A 109.5 . . ? Ge6 O15 H15A 109.5 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N2 C4 113.5(4) . . ? C3 N2 H2C 123.3 . . ? C4 N2 H2C 123.3 . . ? C6 N3 C5 113.3(5) . . ? C6 N3 H3C 123.3 . . ? C5 N3 H3C 123.3 . . ? C8 N4 H4C 109.5 . . ? C8 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C8 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? N1 C1 C2 111.8(4) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? C1 C2 C3 110.5(4) . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C2 112.6(4) . . ? N2 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N2 C4 C5 111.7(4) . . ? N2 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C4 116.0(4) . . ? N3 C5 H5A 108.3 . . ? C4 C5 H5A 108.3 . . ? N3 C5 H5B 108.3 . . ? C4 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? N3 C6 C7 116.0(6) . . ? N3 C6 H6A 108.3 . . ? C7 C6 H6A 108.3 . . ? N3 C6 H6B 108.3 . . ? C7 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C8 C7 C6 111.5(6) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 N4 114.4(5) . . ? C7 C8 H8A 108.7 . . ? N4 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? N4 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.008 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.100