#Electronic Supplementary Material for Dalton Transactions #This Journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Frank Breher' _publ_contact_author_email BREHER@AOC1.UNI-KARLSRUHE.DE _publ_section_title ; Neutral and Cationic Main Group Element Cages of Germanium(II) with Pyrazolyl Ligands - Solid State Structures, DFT Calculations and Advanced Solution NMR Investigations ; loop_ _publ_author_name 'Frank Breher' 'Ignacio Fernandez' 'Ivo Krummenacher' 'Heinz Ruegger' 'Florian Weigend' # Attachment 'revised_germanium_cages.cif' data_Ge2CF3CF3neutral _database_code_depnum_ccdc_archive 'CCDC 718005' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H4 F24 Ge2 N8' _chemical_formula_sum 'C20 H4 F24 Ge2 N8' _chemical_formula_weight 957.49 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' F F 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 9.1677(6) _cell_length_b 37.262(2) _cell_length_c 9.3337(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.560(1) _cell_angle_gamma 90.00 _cell_volume 2985.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 28474 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.28 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 2.195 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2600 _exptl_absorpt_correction_T_max 0.4664 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28474 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7406 _reflns_number_gt 6291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0387P)^2^+4.3565P] 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 7406 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.58198(3) 0.122309(8) 0.47908(3) 0.02364(8) Uani 1 1 d . . . N1 N 0.6789(3) 0.10536(6) 0.3182(3) 0.0237(5) Uani 1 1 d . . . Ge2 Ge 0.94991(3) 0.157204(8) 0.39914(4) 0.02628(8) Uani 1 1 d . . . N2 N 0.8257(3) 0.11206(6) 0.3219(3) 0.0234(5) Uani 1 1 d . . . N3 N 0.7830(3) 0.14881(6) 0.6262(3) 0.0248(5) Uani 1 1 d . . . N4 N 0.9194(3) 0.15285(6) 0.6021(3) 0.0242(5) Uani 1 1 d . . . N5 N 0.6218(3) 0.17949(7) 0.3327(3) 0.0292(5) Uani 1 1 d . . . N6 N 0.7596(3) 0.18778(6) 0.3184(3) 0.0274(5) Uani 1 1 d . . . N7 N 0.6892(3) 0.07745(7) 0.5980(3) 0.0278(5) Uani 1 1 d . . . N8 N 0.8431(3) 0.07341(7) 0.6204(3) 0.0301(5) Uani 1 1 d . . . F10 F 0.4225(2) 0.05757(7) 0.3051(2) 0.0582(6) Uani 1 1 d . . . C10 C 0.4604(3) 0.06476(8) 0.1828(4) 0.0330(6) Uani 1 1 d . . . C11 C 0.6246(3) 0.07758(7) 0.2237(3) 0.0255(5) Uani 1 1 d . . . F11 F 0.3597(2) 0.08919(7) 0.1033(3) 0.0747(8) Uani 1 1 d . . . F12 F 0.4360(2) 0.03541(6) 0.1004(2) 0.0491(5) Uani 1 1 d . . . C12 C 0.7348(3) 0.06533(8) 0.1669(3) 0.0308(6) Uani 1 1 d . . . H12A H 0.7265 0.0459 0.0988 0.037 Uiso 1 1 calc R . . C13 C 0.8597(3) 0.08770(8) 0.2312(3) 0.0269(6) Uani 1 1 d . . . F13 F 1.1296(3) 0.08624(10) 0.3442(3) 0.0865(10) Uani 1 1 d . . . F14 F 1.0267(3) 0.05837(8) 0.1349(5) 0.1000(12) Uani 1 1 d . . . C14 C 1.0154(4) 0.08626(9) 0.2131(4) 0.0382(7) Uani 1 1 d . . . F15 F 1.0410(3) 0.11481(8) 0.1417(4) 0.0763(8) Uani 1 1 d . . . C20 C 0.6863(4) 0.15430(10) 0.8428(4) 0.0374(7) Uani 1 1 d . . . F20 F 0.5831(11) 0.1299(4) 0.7917(15) 0.086(5) Uani 0.57(3) 1 d P A 1 F20' F 0.5664(13) 0.1726(7) 0.757(2) 0.092(5) Uani 0.43(3) 1 d P A 2 C21 C 0.8130(3) 0.15442(8) 0.7756(3) 0.0286(6) Uani 1 1 d . A . F21 F 0.614(2) 0.1855(3) 0.825(2) 0.092(4) Uani 0.57(3) 1 d P A 1 F21' F 0.7293(19) 0.1657(8) 0.976(2) 0.095(7) Uani 0.43(3) 1 d P A 2 F22 F 0.7445(14) 0.1507(3) 0.9935(11) 0.064(3) Uani 0.57(3) 1 d P A 1 F22' F 0.631(3) 0.1223(4) 0.844(3) 0.095(6) Uani 0.43(3) 1 d P A 2 C22 C 0.9683(4) 0.16197(9) 0.8508(4) 0.0334(6) Uani 1 1 d . . . H22A H 1.0199 0.1670 0.9564 0.040 Uiso 1 1 calc R A . C23 C 1.0308(3) 0.16060(8) 0.7378(3) 0.0293(6) Uani 1 1 d . A . F23 F 1.2863(3) 0.16838(11) 0.8963(3) 0.0916(11) Uani 1 1 d . A . F24 F 1.2490(2) 0.14030(7) 0.6875(3) 0.0668(7) Uani 1 1 d . A . C24 C 1.1971(4) 0.16645(11) 0.7525(4) 0.0423(8) Uani 1 1 d . . . F25 F 1.2150(3) 0.19614(7) 0.6834(3) 0.0701(7) Uani 1 1 d . A . F30 F 0.2922(2) 0.17398(7) 0.2226(3) 0.0607(6) Uani 1 1 d . . . C30 C 0.3605(4) 0.20543(10) 0.2600(5) 0.0458(8) Uani 1 1 d . . . C31 C 0.5239(4) 0.20560(8) 0.2632(4) 0.0333(6) Uani 1 1 d . . . F31 F 0.3510(3) 0.21354(12) 0.3927(4) 0.1083(13) Uani 1 1 d . . . C32 C 0.5954(4) 0.23148(9) 0.2021(4) 0.0393(7) Uani 1 1 d . . . H32A H 0.5510 0.2526 0.1472 0.047 Uiso 1 1 calc R . . F32 F 0.2726(3) 0.22788(8) 0.1562(4) 0.0968(11) Uani 1 1 d . . . F33 F 0.8300(3) 0.26503(6) 0.1223(3) 0.0656(7) Uani 1 1 d . . . C33 C 0.7440(4) 0.21916(8) 0.2398(3) 0.0308(6) Uani 1 1 d . . . F34 F 0.9436(3) 0.21445(7) 0.1367(3) 0.0643(7) Uani 1 1 d . . . C34 C 0.8770(4) 0.23616(9) 0.2090(4) 0.0405(8) Uani 1 1 d . . . F35 F 0.9905(3) 0.24633(7) 0.3356(3) 0.0595(6) Uani 1 1 d . . . C40 C 0.4826(3) 0.04751(9) 0.6721(4) 0.0324(6) Uani 1 1 d . . . F40 F 0.4800(2) 0.04418(8) 0.8121(2) 0.0653(7) Uani 1 1 d . . . C41 C 0.6442(3) 0.05099(8) 0.6726(3) 0.0260(5) Uani 1 1 d . . . F41 F 0.4104(3) 0.01872(7) 0.5966(3) 0.0682(7) Uani 1 1 d . . . F42 F 0.3942(2) 0.07527(6) 0.6073(3) 0.0486(5) Uani 1 1 d . . . C42 C 0.7689(3) 0.02934(8) 0.7457(4) 0.0337(7) Uani 1 1 d . . . H42A H 0.7726 0.0087 0.8067 0.040 Uiso 1 1 calc R . . C43 C 0.8891(3) 0.04493(8) 0.7086(4) 0.0309(6) Uani 1 1 d . . . F43 F 1.1499(3) 0.06066(9) 0.7742(5) 0.1189(16) Uani 1 1 d . . . F44 F 1.1027(3) 0.01688(7) 0.8894(3) 0.0651(7) Uani 1 1 d . . . C44 C 1.0541(4) 0.03328(10) 0.7547(4) 0.0449(8) Uani 1 1 d . . . F45 F 1.0807(4) 0.01108(13) 0.6617(4) 0.1305(18) Uani 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 Ge1 0.01585(13) 0.02842(15) 0.02693(15) -0.00022(11) 0.00786(11) 0.00091(10) N1 0.0200(10) 0.0247(12) 0.0279(12) 0.0013(9) 0.0103(9) 0.0000(8) Ge2 0.02118(14) 0.02769(16) 0.03292(16) -0.00134(12) 0.01319(12) -0.00359(11) N2 0.0195(10) 0.0261(12) 0.0262(11) 0.0014(9) 0.0102(9) 0.0000(8) N3 0.0207(11) 0.0264(12) 0.0279(12) -0.0008(9) 0.0090(9) -0.0004(9) N4 0.0198(10) 0.0249(11) 0.0297(12) -0.0014(9) 0.0111(9) -0.0014(8) N5 0.0273(12) 0.0283(12) 0.0336(13) 0.0013(10) 0.0125(10) -0.0003(10) N6 0.0284(12) 0.0257(12) 0.0305(12) 0.0010(10) 0.0133(10) -0.0007(9) N7 0.0189(11) 0.0312(13) 0.0350(13) 0.0061(10) 0.0115(10) 0.0029(9) N8 0.0185(11) 0.0323(13) 0.0400(14) 0.0060(11) 0.0109(10) 0.0013(9) F10 0.0425(11) 0.0930(18) 0.0463(12) -0.0224(12) 0.0247(10) -0.0324(12) C10 0.0265(14) 0.0342(16) 0.0364(16) -0.0051(13) 0.0086(12) -0.0051(12) C11 0.0223(12) 0.0248(13) 0.0260(13) 0.0014(11) 0.0045(10) -0.0002(10) F11 0.0269(10) 0.0589(15) 0.114(2) 0.0218(15) -0.0056(12) 0.0012(10) F12 0.0432(11) 0.0536(13) 0.0514(12) -0.0234(10) 0.0178(9) -0.0219(9) C12 0.0292(14) 0.0309(15) 0.0325(15) -0.0057(12) 0.0112(12) 0.0014(12) C13 0.0267(13) 0.0281(14) 0.0271(14) -0.0001(11) 0.0107(11) 0.0032(11) F13 0.0281(11) 0.161(3) 0.0670(17) 0.0104(18) 0.0122(11) 0.0227(15) F14 0.0775(19) 0.082(2) 0.179(3) -0.076(2) 0.094(2) -0.0282(15) C14 0.0314(16) 0.0394(17) 0.0494(19) -0.0077(15) 0.0212(14) -0.0001(13) F15 0.0601(16) 0.0786(18) 0.113(2) 0.0310(16) 0.0592(16) 0.0053(13) C20 0.0345(16) 0.0461(19) 0.0333(16) -0.0074(14) 0.0139(13) -0.0030(14) F20 0.047(4) 0.146(12) 0.084(6) -0.079(7) 0.047(4) -0.056(5) F20' 0.040(5) 0.160(15) 0.093(8) 0.041(8) 0.043(5) 0.042(6) C21 0.0268(14) 0.0296(15) 0.0299(14) -0.0030(11) 0.0105(11) -0.0010(11) F21 0.120(9) 0.071(5) 0.130(10) 0.049(5) 0.102(8) 0.060(5) F21' 0.055(7) 0.171(16) 0.069(9) -0.092(10) 0.036(7) -0.047(9) F22 0.049(3) 0.118(7) 0.031(3) 0.016(5) 0.021(2) 0.009(4) F22' 0.150(14) 0.053(5) 0.141(13) -0.027(7) 0.126(12) -0.045(8) C22 0.0291(15) 0.0393(17) 0.0290(15) -0.0046(13) 0.0068(12) -0.0042(12) C23 0.0223(13) 0.0300(15) 0.0323(15) -0.0016(12) 0.0056(11) -0.0029(11) F23 0.0313(12) 0.187(3) 0.0451(14) -0.0156(17) -0.0006(10) -0.0261(16) F24 0.0315(11) 0.0733(17) 0.098(2) -0.0159(14) 0.0260(12) 0.0060(11) C24 0.0242(15) 0.058(2) 0.0423(19) -0.0068(16) 0.0083(14) -0.0093(14) F25 0.0503(14) 0.0630(16) 0.103(2) 0.0009(14) 0.0341(14) -0.0245(12) F30 0.0357(11) 0.0561(14) 0.0857(18) 0.0005(12) 0.0155(11) -0.0067(10) C30 0.0316(17) 0.042(2) 0.060(2) 0.0010(17) 0.0114(16) 0.0093(14) C31 0.0329(15) 0.0274(15) 0.0389(17) 0.0000(12) 0.0117(13) 0.0041(12) F31 0.0487(15) 0.191(4) 0.098(2) -0.074(2) 0.0423(16) -0.0219(19) C32 0.0425(18) 0.0281(16) 0.0443(18) 0.0069(14) 0.0115(15) 0.0039(13) F32 0.0451(14) 0.0756(19) 0.164(3) 0.057(2) 0.0292(17) 0.0286(13) F33 0.0743(16) 0.0487(14) 0.0762(17) 0.0302(12) 0.0294(14) -0.0079(12) C33 0.0389(16) 0.0241(14) 0.0310(15) -0.0002(11) 0.0141(13) -0.0023(12) F34 0.0756(16) 0.0563(14) 0.0861(18) -0.0152(13) 0.0598(15) -0.0183(12) C34 0.053(2) 0.0292(16) 0.0433(19) 0.0034(14) 0.0211(16) -0.0083(14) F35 0.0523(13) 0.0662(15) 0.0569(14) -0.0033(12) 0.0153(11) -0.0270(11) C40 0.0235(14) 0.0398(17) 0.0349(16) 0.0061(13) 0.0116(12) -0.0027(12) F40 0.0357(11) 0.125(2) 0.0414(12) 0.0221(13) 0.0206(10) 0.0022(12) C41 0.0217(12) 0.0294(14) 0.0272(13) 0.0007(11) 0.0088(11) -0.0024(10) F41 0.0380(12) 0.0638(15) 0.107(2) -0.0278(14) 0.0310(13) -0.0235(11) F42 0.0257(9) 0.0548(13) 0.0690(14) 0.0217(11) 0.0209(9) 0.0087(8) C42 0.0268(14) 0.0319(16) 0.0408(17) 0.0120(13) 0.0098(13) 0.0011(12) C43 0.0229(13) 0.0336(16) 0.0355(16) 0.0048(12) 0.0095(12) 0.0021(11) F43 0.0267(12) 0.089(2) 0.226(4) 0.070(3) 0.0254(18) 0.0045(13) F44 0.0401(12) 0.0840(18) 0.0607(15) 0.0220(13) 0.0046(10) 0.0232(12) C44 0.0285(16) 0.051(2) 0.056(2) 0.0153(17) 0.0153(15) 0.0093(14) F45 0.0694(19) 0.239(5) 0.0704(19) -0.041(2) 0.0092(15) 0.087(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 N7 2.056(2) . ? Ge1 N1 2.093(2) . ? Ge1 N3 2.117(2) . ? N1 C11 1.337(4) . ? N1 N2 1.357(3) . ? Ge2 N6 1.996(2) . ? Ge2 N4 2.016(2) . ? Ge2 N2 2.017(2) . ? N2 C13 1.350(4) . ? N3 C21 1.340(4) . ? N3 N4 1.354(3) . ? N4 C23 1.349(4) . ? N5 C31 1.328(4) . ? N5 N6 1.352(3) . ? N6 C33 1.361(4) . ? N7 C41 1.353(4) . ? N7 N8 1.360(3) . ? N8 C43 1.318(4) . ? F10 C10 1.332(4) . ? C10 F12 1.310(4) . ? C10 F11 1.323(4) . ? C10 C11 1.495(4) . ? C11 C12 1.374(4) . ? C12 C13 1.372(4) . ? C12 H12A 0.9500 . ? C13 C14 1.496(4) . ? F13 C14 1.301(4) . ? F14 C14 1.294(4) . ? C14 F15 1.319(4) . ? C20 F21' 1.240(12) . ? C20 F20 1.278(10) . ? C20 F22' 1.296(13) . ? C20 F20' 1.303(12) . ? C20 F21 1.318(8) . ? C20 F22 1.324(9) . ? C20 C21 1.501(4) . ? C21 C22 1.378(4) . ? C22 C23 1.367(4) . ? C22 H22A 0.9500 . ? C23 C24 1.498(4) . ? F23 C24 1.305(4) . ? F24 C24 1.322(4) . ? C24 F25 1.319(4) . ? F30 C30 1.317(4) . ? C30 F31 1.307(5) . ? C30 F32 1.319(4) . ? C30 C31 1.488(5) . ? C31 C32 1.396(5) . ? C32 C33 1.362(5) . ? C32 H32A 0.9500 . ? F33 C34 1.324(4) . ? C33 C34 1.488(4) . ? F34 C34 1.332(4) . ? C34 F35 1.326(4) . ? C40 F40 1.321(4) . ? C40 F42 1.322(4) . ? C40 F41 1.326(4) . ? C40 C41 1.485(4) . ? C41 C42 1.369(4) . ? C42 C43 1.392(4) . ? C42 H42A 0.9500 . ? C43 C44 1.484(4) . ? F43 C44 1.317(5) . ? F44 C44 1.326(4) . ? C44 F45 1.283(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 N7 Ge1 N1 84.20(9) . . ? N7 Ge1 N3 83.50(9) . . ? N1 Ge1 N3 96.53(9) . . ? C11 N1 N2 107.2(2) . . ? C11 N1 Ge1 123.56(18) . . ? N2 N1 Ge1 126.39(17) . . ? N6 Ge2 N4 90.54(9) . . ? N6 Ge2 N2 91.84(9) . . ? N4 Ge2 N2 91.23(9) . . ? C13 N2 N1 107.8(2) . . ? C13 N2 Ge2 123.98(18) . . ? N1 N2 Ge2 126.37(17) . . ? C21 N3 N4 107.0(2) . . ? C21 N3 Ge1 124.14(19) . . ? N4 N3 Ge1 126.07(18) . . ? C23 N4 N3 107.9(2) . . ? C23 N4 Ge2 123.73(19) . . ? N3 N4 Ge2 127.27(18) . . ? C31 N5 N6 106.2(2) . . ? N5 N6 C33 108.9(2) . . ? N5 N6 Ge2 123.73(18) . . ? C33 N6 Ge2 127.3(2) . . ? C41 N7 N8 109.1(2) . . ? C41 N7 Ge1 134.12(18) . . ? N8 N7 Ge1 116.53(18) . . ? C43 N8 N7 105.8(2) . . ? F12 C10 F11 107.7(3) . . ? F12 C10 F10 107.0(3) . . ? F11 C10 F10 106.2(3) . . ? F12 C10 C11 111.5(3) . . ? F11 C10 C11 111.4(3) . . ? F10 C10 C11 112.8(3) . . ? N1 C11 C12 110.9(2) . . ? N1 C11 C10 121.6(3) . . ? C12 C11 C10 127.3(3) . . ? C13 C12 C11 104.1(3) . . ? C13 C12 H12A 128.0 . . ? C11 C12 H12A 128.0 . . ? N2 C13 C12 110.0(2) . . ? N2 C13 C14 122.3(3) . . ? C12 C13 C14 127.7(3) . . ? F14 C14 F13 109.4(3) . . ? F14 C14 F15 107.4(3) . . ? F13 C14 F15 104.4(3) . . ? F14 C14 C13 111.1(3) . . ? F13 C14 C13 112.2(3) . . ? F15 C14 C13 112.0(3) . . ? F21' C20 F20 123.5(10) . . ? F21' C20 F22' 107.1(11) . . ? F21' C20 F20' 110.0(9) . . ? F20 C20 F20' 77.8(9) . . ? F22' C20 F20' 103.8(10) . . ? F21' C20 F21 78.0(9) . . ? F20 C20 F21 108.0(8) . . ? F22' C20 F21 129.2(9) . . ? F20 C20 F22 107.1(8) . . ? F22' C20 F22 84.9(11) . . ? F20' C20 F22 130.2(9) . . ? F21 C20 F22 102.7(7) . . ? F21' C20 C21 113.4(7) . . ? F20 C20 C21 115.2(6) . . ? F22' C20 C21 111.6(8) . . ? F20' C20 C21 110.5(6) . . ? F21 C20 C21 111.8(5) . . ? F22 C20 C21 111.2(6) . . ? N3 C21 C22 111.0(3) . . ? N3 C21 C20 121.9(3) . . ? C22 C21 C20 126.9(3) . . ? C23 C22 C21 103.8(3) . . ? C23 C22 H22A 128.1 . . ? C21 C22 H22A 128.1 . . ? N4 C23 C22 110.4(3) . . ? N4 C23 C24 121.9(3) . . ? C22 C23 C24 127.8(3) . . ? F23 C24 F25 108.4(3) . . ? F23 C24 F24 108.4(3) . . ? F25 C24 F24 105.5(3) . . ? F23 C24 C23 110.6(3) . . ? F25 C24 C23 112.0(3) . . ? F24 C24 C23 111.7(3) . . ? F31 C30 F30 105.9(4) . . ? F31 C30 F32 108.8(4) . . ? F30 C30 F32 105.0(3) . . ? F31 C30 C31 112.5(3) . . ? F30 C30 C31 113.0(3) . . ? F32 C30 C31 111.3(3) . . ? N5 C31 C32 111.8(3) . . ? N5 C31 C30 120.6(3) . . ? C32 C31 C30 127.5(3) . . ? C33 C32 C31 103.4(3) . . ? C33 C32 H32A 128.3 . . ? C31 C32 H32A 128.3 . . ? N6 C33 C32 109.6(3) . . ? N6 C33 C34 122.1(3) . . ? C32 C33 C34 128.3(3) . . ? F33 C34 F35 107.3(3) . . ? F33 C34 F34 107.0(3) . . ? F35 C34 F34 105.6(3) . . ? F33 C34 C33 110.6(3) . . ? F35 C34 C33 112.9(3) . . ? F34 C34 C33 113.1(3) . . ? F40 C40 F42 107.7(3) . . ? F40 C40 F41 105.7(3) . . ? F42 C40 F41 106.2(3) . . ? F40 C40 C41 111.7(2) . . ? F42 C40 C41 112.6(2) . . ? F41 C40 C41 112.6(3) . . ? N7 C41 C42 109.5(2) . . ? N7 C41 C40 123.1(3) . . ? C42 C41 C40 127.4(3) . . ? C41 C42 C43 103.1(3) . . ? C41 C42 H42A 128.5 . . ? C43 C42 H42A 128.5 . . ? N8 C43 C42 112.6(3) . . ? N8 C43 C44 119.1(3) . . ? C42 C43 C44 128.4(3) . . ? F45 C44 F43 108.5(4) . . ? F45 C44 F44 105.3(3) . . ? F43 C44 F44 103.9(3) . . ? F45 C44 C43 114.1(3) . . ? F43 C44 C43 112.1(3) . . ? F44 C44 C43 112.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Ge1 N1 C11 74.6(2) . . . . ? N3 Ge1 N1 C11 157.3(2) . . . . ? N7 Ge1 N1 N2 -83.8(2) . . . . ? N3 Ge1 N1 N2 -1.1(2) . . . . ? C11 N1 N2 C13 -1.1(3) . . . . ? Ge1 N1 N2 C13 160.18(19) . . . . ? C11 N1 N2 Ge2 163.73(19) . . . . ? Ge1 N1 N2 Ge2 -35.0(3) . . . . ? N6 Ge2 N2 C13 126.5(2) . . . . ? N4 Ge2 N2 C13 -143.0(2) . . . . ? N6 Ge2 N2 N1 -36.0(2) . . . . ? N4 Ge2 N2 N1 54.5(2) . . . . ? N7 Ge1 N3 C21 -71.9(2) . . . . ? N1 Ge1 N3 C21 -155.2(2) . . . . ? N7 Ge1 N3 N4 86.6(2) . . . . ? N1 Ge1 N3 N4 3.2(2) . . . . ? C21 N3 N4 C23 0.5(3) . . . . ? Ge1 N3 N4 C23 -161.00(19) . . . . ? C21 N3 N4 Ge2 -167.63(19) . . . . ? Ge1 N3 N4 Ge2 30.9(3) . . . . ? N6 Ge2 N4 C23 -127.0(2) . . . . ? N2 Ge2 N4 C23 141.2(2) . . . . ? N6 Ge2 N4 N3 39.4(2) . . . . ? N2 Ge2 N4 N3 -52.4(2) . . . . ? C31 N5 N6 C33 0.1(3) . . . . ? C31 N5 N6 Ge2 -178.9(2) . . . . ? N4 Ge2 N6 N5 -47.7(2) . . . . ? N2 Ge2 N6 N5 43.5(2) . . . . ? N4 Ge2 N6 C33 133.4(2) . . . . ? N2 Ge2 N6 C33 -135.3(2) . . . . ? N1 Ge1 N7 C41 -134.8(3) . . . . ? N3 Ge1 N7 C41 127.9(3) . . . . ? N1 Ge1 N7 N8 51.3(2) . . . . ? N3 Ge1 N7 N8 -46.0(2) . . . . ? C41 N7 N8 C43 -0.4(3) . . . . ? Ge1 N7 N8 C43 175.0(2) . . . . ? N2 N1 C11 C12 1.2(3) . . . . ? Ge1 N1 C11 C12 -160.8(2) . . . . ? N2 N1 C11 C10 -175.0(2) . . . . ? Ge1 N1 C11 C10 23.0(4) . . . . ? F12 C10 C11 N1 -174.2(3) . . . . ? F11 C10 C11 N1 65.4(4) . . . . ? F10 C10 C11 N1 -53.8(4) . . . . ? F12 C10 C11 C12 10.2(4) . . . . ? F11 C10 C11 C12 -110.1(4) . . . . ? F10 C10 C11 C12 130.7(3) . . . . ? N1 C11 C12 C13 -0.7(3) . . . . ? C10 C11 C12 C13 175.2(3) . . . . ? N1 N2 C13 C12 0.7(3) . . . . ? Ge2 N2 C13 C12 -164.6(2) . . . . ? N1 N2 C13 C14 -177.6(3) . . . . ? Ge2 N2 C13 C14 17.1(4) . . . . ? C11 C12 C13 N2 0.0(3) . . . . ? C11 C12 C13 C14 178.2(3) . . . . ? N2 C13 C14 F14 172.7(3) . . . . ? C12 C13 C14 F14 -5.2(5) . . . . ? N2 C13 C14 F13 49.8(4) . . . . ? C12 C13 C14 F13 -128.1(4) . . . . ? N2 C13 C14 F15 -67.1(4) . . . . ? C12 C13 C14 F15 114.9(4) . . . . ? N4 N3 C21 C22 -0.3(3) . . . . ? Ge1 N3 C21 C22 161.6(2) . . . . ? N4 N3 C21 C20 176.3(3) . . . . ? Ge1 N3 C21 C20 -21.8(4) . . . . ? F21' C20 C21 N3 -168.7(16) . . . . ? F20 C20 C21 N3 41.1(10) . . . . ? F22' C20 C21 N3 70.2(14) . . . . ? F20' C20 C21 N3 -44.7(14) . . . . ? F21 C20 C21 N3 -82.7(11) . . . . ? F22 C20 C21 N3 163.1(7) . . . . ? F21' C20 C21 C22 7.3(16) . . . . ? F20 C20 C21 C22 -142.9(9) . . . . ? F22' C20 C21 C22 -113.8(14) . . . . ? F20' C20 C21 C22 131.3(14) . . . . ? F21 C20 C21 C22 93.3(11) . . . . ? F22 C20 C21 C22 -20.8(8) . . . . ? N3 C21 C22 C23 0.0(4) . . . . ? C20 C21 C22 C23 -176.4(3) . . . . ? N3 N4 C23 C22 -0.5(3) . . . . ? Ge2 N4 C23 C22 168.1(2) . . . . ? N3 N4 C23 C24 179.4(3) . . . . ? Ge2 N4 C23 C24 -11.9(4) . . . . ? C21 C22 C23 N4 0.3(4) . . . . ? C21 C22 C23 C24 -179.6(3) . . . . ? N4 C23 C24 F23 -170.9(3) . . . . ? C22 C23 C24 F23 9.1(5) . . . . ? N4 C23 C24 F25 68.1(4) . . . . ? C22 C23 C24 F25 -112.0(4) . . . . ? N4 C23 C24 F24 -50.0(4) . . . . ? C22 C23 C24 F24 129.9(4) . . . . ? N6 N5 C31 C32 0.0(4) . . . . ? N6 N5 C31 C30 -178.7(3) . . . . ? F31 C30 C31 N5 73.2(4) . . . . ? F30 C30 C31 N5 -46.6(5) . . . . ? F32 C30 C31 N5 -164.4(3) . . . . ? F31 C30 C31 C32 -105.2(5) . . . . ? F30 C30 C31 C32 135.0(4) . . . . ? F32 C30 C31 C32 17.2(5) . . . . ? N5 C31 C32 C33 -0.1(4) . . . . ? C30 C31 C32 C33 178.4(3) . . . . ? N5 N6 C33 C32 -0.2(3) . . . . ? Ge2 N6 C33 C32 178.8(2) . . . . ? N5 N6 C33 C34 178.1(3) . . . . ? Ge2 N6 C33 C34 -2.9(4) . . . . ? C31 C32 C33 N6 0.1(4) . . . . ? C31 C32 C33 C34 -178.0(3) . . . . ? N6 C33 C34 F33 175.8(3) . . . . ? C32 C33 C34 F33 -6.2(5) . . . . ? N6 C33 C34 F35 -64.0(4) . . . . ? C32 C33 C34 F35 114.0(4) . . . . ? N6 C33 C34 F34 55.9(4) . . . . ? C32 C33 C34 F34 -126.2(4) . . . . ? N8 N7 C41 C42 0.3(3) . . . . ? Ge1 N7 C41 C42 -174.0(2) . . . . ? N8 N7 C41 C40 179.9(3) . . . . ? Ge1 N7 C41 C40 5.6(5) . . . . ? F40 C40 C41 N7 -129.1(3) . . . . ? F42 C40 C41 N7 -7.7(4) . . . . ? F41 C40 C41 N7 112.2(3) . . . . ? F40 C40 C41 C42 50.4(4) . . . . ? F42 C40 C41 C42 171.8(3) . . . . ? F41 C40 C41 C42 -68.3(4) . . . . ? N7 C41 C42 C43 0.0(4) . . . . ? C40 C41 C42 C43 -179.6(3) . . . . ? N7 N8 C43 C42 0.4(4) . . . . ? N7 N8 C43 C44 -180.0(3) . . . . ? C41 C42 C43 N8 -0.3(4) . . . . ? C41 C42 C43 C44 -179.8(3) . . . . ? N8 C43 C44 F45 -89.5(5) . . . . ? C42 C43 C44 F45 90.0(5) . . . . ? N8 C43 C44 F43 34.3(5) . . . . ? C42 C43 C44 F43 -146.1(4) . . . . ? N8 C43 C44 F44 150.8(3) . . . . ? C42 C43 C44 F44 -29.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.925 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.083 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Ge2MeCF3neutral _database_code_depnum_ccdc_archive 'CCDC 718006' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C20 H16 F12 Ge2 N8), 3(C7 H8)' _chemical_formula_sum 'C61 H56 F24 Ge4 N16' _chemical_formula_weight 1759.58 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0216(8) _cell_length_b 10.9980(10) _cell_length_c 18.9911(17) _cell_angle_alpha 73.454(2) _cell_angle_beta 89.557(2) _cell_angle_gamma 83.108(2) _cell_volume 1792.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 15787 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 878 _exptl_absorpt_coefficient_mu 1.774 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5520 _exptl_absorpt_correction_T_max 0.7407 _exptl_absorpt_process_details 'Blessing 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15787 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7031 _reflns_number_gt 4471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0530P)^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 7031 _refine_ls_number_parameters 576 _refine_ls_number_restraints 239 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.936 _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 Ge1 Ge 0.53030(5) 0.54578(5) 0.23134(3) 0.02837(15) Uani 1 1 d . . . N1 N 0.8110(4) 0.6102(4) 0.1382(2) 0.0281(9) Uani 1 1 d . . . Ge2 Ge 0.94934(5) 0.60791(5) 0.22105(3) 0.03115(16) Uani 1 1 d . . . N2 N 0.6626(4) 0.5984(3) 0.1410(2) 0.0269(9) Uani 1 1 d . . . N3 N 0.8569(4) 0.4656(3) 0.2887(2) 0.0262(9) Uani 1 1 d . . . N4 N 0.7108(4) 0.4423(3) 0.2962(2) 0.0262(9) Uani 1 1 d . . . N5 N 0.8122(4) 0.7388(4) 0.2482(2) 0.0316(9) Uani 1 1 d . . . N6 N 0.6695(4) 0.7220(4) 0.2675(2) 0.0354(10) Uani 1 1 d . . . N7 N 0.5013(4) 0.3879(4) 0.2023(2) 0.0291(9) Uani 1 1 d . . . N8 N 0.3545(4) 0.3705(4) 0.2090(2) 0.0277(9) Uani 1 1 d . . . F10 F 1.0992(4) 0.5635(4) 0.0700(2) 0.0757(11) Uani 1 1 d . . . C10 C 0.9992(6) 0.6654(6) 0.0425(3) 0.0500(15) Uani 1 1 d . . . F11 F 1.0479(4) 0.7590(4) 0.0633(2) 0.0766(11) Uani 1 1 d . . . C11 C 0.8456(5) 0.6430(5) 0.0665(3) 0.0330(12) Uani 1 1 d . . . F12 F 1.0066(4) 0.6955(5) -0.0290(2) 0.1135(19) Uani 1 1 d . . . C12 C 0.7208(5) 0.6523(5) 0.0238(3) 0.0382(13) Uani 1 1 d . . . H12 H 0.7143 0.6733 -0.0283 0.046 Uiso 1 1 calc R . . C13 C 0.6067(5) 0.6247(5) 0.0722(3) 0.0325(11) Uani 1 1 d . . . C14 C 0.4469(5) 0.6227(5) 0.0555(3) 0.0409(13) Uani 1 1 d . . . H14A H 0.4277 0.5342 0.0627 0.061 Uiso 1 1 calc R . . H14B H 0.4227 0.6724 0.0045 0.061 Uiso 1 1 calc R . . H14C H 0.3848 0.6600 0.0885 0.061 Uiso 1 1 calc R . . F20 F 0.5810(4) 0.2360(4) 0.45580(17) 0.0733(11) Uani 1 1 d . . . C20 C 0.5702(6) 0.2853(6) 0.3827(3) 0.0473(14) Uani 1 1 d . . . F21 F 0.4514(3) 0.3740(3) 0.36967(19) 0.0656(10) Uani 1 1 d . . . C21 C 0.7091(5) 0.3408(5) 0.3539(3) 0.0338(12) Uani 1 1 d . . . F22 F 0.5386(4) 0.1917(4) 0.3557(2) 0.0741(11) Uani 1 1 d . . . C22 C 0.8488(5) 0.2957(5) 0.3835(3) 0.0377(12) Uani 1 1 d . . . H22 H 0.8761 0.2242 0.4249 0.045 Uiso 1 1 calc R . . C23 C 0.9413(5) 0.3745(5) 0.3412(3) 0.0308(11) Uani 1 1 d . . . C24 C 1.1065(5) 0.3728(5) 0.3501(3) 0.0430(14) Uani 1 1 d . . . H24A H 1.1571 0.3481 0.3095 0.065 Uiso 1 1 calc R . . H24B H 1.1419 0.3110 0.3968 0.065 Uiso 1 1 calc R . . H24C H 1.1285 0.4580 0.3498 0.065 Uiso 1 1 calc R . . C30 C 0.4635(7) 0.8390(6) 0.3117(4) 0.0594(17) Uani 1 1 d . . . C31 C 0.6164(5) 0.8243(5) 0.2873(3) 0.0364(12) Uani 1 1 d . . . C32 C 0.7218(6) 0.9080(5) 0.2811(3) 0.0455(14) Uani 1 1 d . . . H32 H 0.7099 0.9882 0.2913 0.055 Uiso 1 1 calc R . . C33 C 0.8463(6) 0.8507(5) 0.2570(3) 0.0392(13) Uani 1 1 d . . . C34 C 0.9960(6) 0.8947(6) 0.2393(4) 0.069(2) Uani 1 1 d . . . H34A H 1.0732 0.8315 0.2696 0.103 Uiso 1 1 calc R . . H34B H 0.9981 0.9770 0.2495 0.103 Uiso 1 1 calc R . . H34C H 1.0151 0.9046 0.1872 0.103 Uiso 1 1 calc R . . F40 F 0.0821(3) 0.3065(3) 0.1771(2) 0.0628(10) Uani 1 1 d . . . C40 C 0.1968(6) 0.2146(5) 0.1951(3) 0.0380(13) Uani 1 1 d . . . F41 F 0.1885(3) 0.1403(3) 0.15153(18) 0.0600(9) Uani 1 1 d . . . C41 C 0.3432(5) 0.2657(4) 0.1896(3) 0.0302(11) Uani 1 1 d . . . F42 F 0.1712(3) 0.1436(3) 0.26306(18) 0.0603(9) Uani 1 1 d . . . C42 C 0.4793(5) 0.2127(5) 0.1710(3) 0.0362(12) Uani 1 1 d . . . H42 H 0.4993 0.1373 0.1558 0.043 Uiso 1 1 calc R . . C43 C 0.5795(5) 0.2928(5) 0.1793(3) 0.0341(12) Uani 1 1 d . . . C44 C 0.7440(5) 0.2837(5) 0.1673(3) 0.0489(15) Uani 1 1 d . . . H44A H 0.7662 0.3585 0.1281 0.073 Uiso 1 1 calc R . . H44B H 0.7767 0.2059 0.1532 0.073 Uiso 1 1 calc R . . H44C H 0.7968 0.2808 0.2128 0.073 Uiso 1 1 calc R . . F30 F 0.4367(4) 0.9293(5) 0.3437(3) 0.1170(18) Uani 1 1 d . . . F31 F 0.4222(5) 0.7345(4) 0.3562(3) 0.1128(17) Uani 1 1 d . . . F32 F 0.3628(4) 0.8696(5) 0.2572(3) 0.1157(18) Uani 1 1 d . . . C70 C 0.880(2) 1.003(3) 0.5516(13) 0.059(4) Uani 0.50 1 d PDU A -1 H70 H 0.8100 1.0129 0.5878 0.071 Uiso 0.50 1 calc PR A -1 C75 C 1.019(2) 1.040(3) 0.5522(13) 0.053(4) Uani 0.50 1 d PDU A -1 H75 H 1.0442 1.0739 0.5906 0.063 Uiso 0.50 1 calc PR A -1 C74 C 1.124(2) 1.031(3) 0.5010(14) 0.050(4) Uani 0.50 1 d PDU A -1 H74 H 1.2210 1.0555 0.5032 0.060 Uiso 0.50 1 calc PR A -1 C71 C 0.845(3) 0.952(4) 0.4972(16) 0.064(4) Uani 0.50 1 d PDU A -1 C72 C 0.944(2) 0.941(3) 0.4439(15) 0.061(4) Uani 0.50 1 d PDU A -1 H72 H 0.9190 0.9059 0.4060 0.073 Uiso 0.50 1 calc PR A -1 C73 C 1.080(2) 0.983(3) 0.4465(13) 0.049(4) Uani 0.50 1 d PDU A -1 H73 H 1.1470 0.9789 0.4084 0.059 Uiso 0.50 1 calc PR A -1 C76 C 0.7182(15) 0.9205(13) 0.4944(9) 0.099(5) Uani 0.50 1 d PDU A -1 H76A H 0.6746 0.9595 0.4448 0.148 Uiso 0.50 1 calc PR A -1 H76B H 0.6551 0.9500 0.5299 0.148 Uiso 0.50 1 calc PR A -1 H76C H 0.7246 0.8272 0.5061 0.148 Uiso 0.50 1 calc PR A -1 C6 C 1.1404(16) 0.5987(16) 0.4559(9) 0.106(5) Uani 0.50 1 d PDU B -1 H6 H 1.1941 0.6639 0.4272 0.127 Uiso 0.50 1 calc PR B -1 C9 C 0.9828(15) 0.4134(15) 0.5363(9) 0.089(5) Uani 0.50 1 d PDU B -1 H9 H 0.9286 0.3483 0.5647 0.107 Uiso 0.50 1 calc PR B -1 C7 C 1.214(3) 0.4936(17) 0.5059(10) 0.115(6) Uani 0.50 1 d PDU B -1 H7 H 1.3198 0.4855 0.5120 0.138 Uiso 0.50 1 calc PR B -1 C8 C 1.1351(15) 0.4000(17) 0.5471(9) 0.096(4) Uani 0.50 1 d PDU B -1 H8 H 1.1848 0.3273 0.5824 0.115 Uiso 0.50 1 calc PR B -1 C99 C 0.906(2) 0.5164(12) 0.4864(8) 0.087(4) Uani 0.50 1 d PDU B -1 C96 C 0.742(2) 0.5307(17) 0.4770(10) 0.123(7) Uani 0.50 1 d PDU B -1 H96A H 0.6993 0.6140 0.4820 0.184 Uiso 0.50 1 calc PR B -1 H96B H 0.7015 0.4626 0.5145 0.184 Uiso 0.50 1 calc PR B -1 H96C H 0.7160 0.5251 0.4281 0.184 Uiso 0.50 1 calc PR B -1 C97 C 0.9885(16) 0.6085(17) 0.4478(12) 0.102(5) Uani 0.50 1 d PDU B -1 H97 H 0.9382 0.6827 0.4139 0.123 Uiso 0.50 1 calc PR B -1 C4 C 0.4695(14) 0.9565(16) 0.0555(7) 0.086(5) Uani 0.50 1 d PDU C -1 H4 H 0.4013 0.9255 0.0928 0.103 Uiso 0.50 1 calc PR C -1 C3 C 0.6168(15) 0.9530(14) 0.0735(7) 0.089(4) Uani 0.50 1 d PDU C -1 H3 H 0.6508 0.9214 0.1233 0.106 Uiso 0.50 1 calc PR C -1 C5 C 0.4208(16) 1.0047(12) -0.0160(6) 0.073(3) Uani 0.50 1 d PDU C -1 C1 C 0.6662(14) 1.0466(14) -0.0517(8) 0.094(4) Uani 0.50 1 d PDU C -1 H1 H 0.7341 1.0786 -0.0889 0.112 Uiso 0.50 1 calc PR C -1 C2 C 0.715(2) 0.995(3) 0.0194(9) 0.108(6) Uani 0.50 1 d PDU C -1 H2 H 0.8180 0.9887 0.0315 0.129 Uiso 0.50 1 calc PR C -1 C88 C 0.5190(15) 1.0516(19) -0.0686(8) 0.085(4) Uani 0.50 1 d PDU C -1 H88 H 0.4842 1.0885 -0.1181 0.102 Uiso 0.50 1 calc PR C -1 C89 C 0.265(2) 1.007(3) -0.0358(10) 0.131(8) Uani 0.50 1 d PDU C -1 H89A H 0.2483 0.9229 -0.0402 0.197 Uiso 0.50 1 calc PR C -1 H89B H 0.2401 1.0719 -0.0828 0.197 Uiso 0.50 1 calc PR C -1 H89C H 0.2014 1.0274 0.0024 0.197 Uiso 0.50 1 calc PR C -1 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 0.0168(3) 0.0296(3) 0.0400(3) -0.0109(2) 0.0032(2) -0.0060(2) N1 0.021(2) 0.034(2) 0.030(2) -0.0080(18) 0.0024(17) -0.0090(17) Ge2 0.0179(3) 0.0368(3) 0.0396(3) -0.0095(3) 0.0012(2) -0.0099(2) N2 0.022(2) 0.028(2) 0.031(2) -0.0078(18) 0.0040(17) -0.0070(17) N3 0.0179(19) 0.025(2) 0.034(2) -0.0040(18) -0.0005(17) -0.0064(16) N4 0.0187(19) 0.027(2) 0.032(2) -0.0056(18) -0.0010(17) -0.0049(16) N5 0.023(2) 0.032(2) 0.045(3) -0.017(2) 0.0009(18) -0.0086(18) N6 0.021(2) 0.039(3) 0.049(3) -0.017(2) 0.0044(19) -0.0089(19) N7 0.0149(19) 0.029(2) 0.047(3) -0.0147(19) 0.0051(18) -0.0089(17) N8 0.021(2) 0.029(2) 0.034(2) -0.0070(18) 0.0011(17) -0.0106(17) F10 0.0323(19) 0.086(3) 0.107(3) -0.027(2) 0.011(2) -0.0034(19) C10 0.035(3) 0.072(4) 0.040(4) -0.005(3) 0.005(3) -0.024(3) F11 0.048(2) 0.075(3) 0.106(3) -0.015(2) 0.015(2) -0.035(2) C11 0.027(3) 0.036(3) 0.036(3) -0.010(2) 0.004(2) -0.007(2) F12 0.052(2) 0.234(6) 0.045(2) -0.016(3) 0.0176(19) -0.043(3) C12 0.034(3) 0.049(3) 0.032(3) -0.012(3) 0.000(2) -0.006(3) C13 0.028(3) 0.032(3) 0.038(3) -0.010(2) -0.002(2) -0.006(2) C14 0.028(3) 0.055(4) 0.038(3) -0.008(3) -0.003(2) -0.009(3) F20 0.059(2) 0.101(3) 0.045(2) 0.009(2) 0.0050(18) -0.028(2) C20 0.041(3) 0.049(4) 0.047(4) -0.005(3) 0.000(3) -0.012(3) F21 0.0355(19) 0.081(3) 0.071(2) -0.003(2) 0.0122(17) -0.0165(18) C21 0.026(3) 0.037(3) 0.038(3) -0.008(3) 0.008(2) -0.011(2) F22 0.072(2) 0.073(3) 0.080(3) -0.013(2) 0.010(2) -0.044(2) C22 0.039(3) 0.032(3) 0.037(3) -0.003(2) 0.000(2) -0.001(2) C23 0.025(2) 0.037(3) 0.031(3) -0.012(2) 0.004(2) -0.001(2) C24 0.029(3) 0.051(4) 0.045(3) -0.009(3) -0.009(2) 0.001(3) C30 0.050(4) 0.045(4) 0.093(5) -0.035(4) 0.016(4) -0.005(3) C31 0.034(3) 0.038(3) 0.040(3) -0.016(3) -0.001(2) -0.006(2) C32 0.050(4) 0.032(3) 0.059(4) -0.018(3) -0.006(3) -0.009(3) C33 0.039(3) 0.033(3) 0.049(3) -0.014(3) -0.003(3) -0.013(3) C34 0.050(4) 0.059(4) 0.113(6) -0.038(4) 0.016(4) -0.038(3) F40 0.0250(16) 0.059(2) 0.107(3) -0.025(2) -0.0072(18) -0.0097(16) C40 0.034(3) 0.038(3) 0.045(3) -0.013(3) -0.001(3) -0.013(3) F41 0.055(2) 0.068(2) 0.075(2) -0.039(2) 0.0089(18) -0.0333(18) C41 0.025(3) 0.029(3) 0.036(3) -0.005(2) 0.000(2) -0.009(2) F42 0.060(2) 0.063(2) 0.060(2) -0.0075(18) 0.0099(17) -0.0382(18) C42 0.034(3) 0.032(3) 0.047(3) -0.018(3) 0.003(2) -0.008(2) C43 0.026(3) 0.030(3) 0.046(3) -0.009(2) 0.004(2) -0.004(2) C44 0.027(3) 0.052(4) 0.076(4) -0.030(3) 0.008(3) -0.006(3) F30 0.069(3) 0.126(4) 0.202(5) -0.120(4) 0.044(3) -0.015(3) F31 0.075(3) 0.087(3) 0.159(4) -0.012(3) 0.071(3) -0.005(3) F32 0.031(2) 0.178(5) 0.141(4) -0.057(4) -0.007(3) 0.008(3) C70 0.056(9) 0.044(10) 0.062(9) 0.005(7) 0.011(8) 0.001(8) C75 0.066(10) 0.032(10) 0.058(8) -0.012(6) -0.013(8) 0.002(9) C74 0.037(9) 0.039(10) 0.064(8) 0.003(6) -0.015(6) -0.014(7) C71 0.044(8) 0.044(11) 0.093(9) 0.001(7) -0.013(7) -0.010(8) C72 0.076(10) 0.048(11) 0.061(8) -0.014(7) -0.024(7) -0.015(8) C73 0.052(9) 0.040(10) 0.044(7) 0.003(6) -0.008(7) 0.002(8) C76 0.055(8) 0.057(9) 0.160(14) 0.014(9) -0.030(8) -0.018(7) C6 0.168(12) 0.078(8) 0.093(10) -0.045(6) 0.034(11) -0.050(10) C9 0.155(11) 0.071(9) 0.049(9) -0.033(6) 0.017(10) -0.004(9) C7 0.160(13) 0.112(12) 0.098(13) -0.061(9) -0.009(12) -0.036(11) C8 0.160(11) 0.075(9) 0.060(9) -0.037(6) -0.013(10) 0.002(10) C99 0.127(10) 0.075(9) 0.069(9) -0.036(6) 0.012(9) -0.008(8) C96 0.122(10) 0.159(18) 0.116(15) -0.097(13) 0.016(11) 0.003(9) C97 0.167(12) 0.063(8) 0.085(11) -0.034(7) 0.025(12) -0.016(10) C4 0.120(9) 0.049(10) 0.084(7) -0.015(9) 0.005(7) 0.001(10) C3 0.132(10) 0.057(9) 0.082(7) -0.038(7) -0.024(7) 0.014(9) C5 0.090(7) 0.042(7) 0.095(7) -0.033(7) -0.008(6) -0.002(7) C1 0.120(9) 0.059(9) 0.116(8) -0.042(8) 0.034(9) -0.030(9) C2 0.113(10) 0.067(13) 0.148(10) -0.037(11) -0.011(9) -0.014(12) C88 0.131(9) 0.058(11) 0.078(7) -0.041(8) 0.009(7) -0.011(10) C89 0.092(9) 0.068(15) 0.241(19) -0.061(17) -0.045(10) 0.011(11) _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 N7 2.011(4) . ? Ge1 N4 2.062(4) . ? Ge1 N2 2.066(4) . ? N1 C11 1.350(6) . ? N1 N2 1.360(5) . ? N1 Ge2 2.008(4) . ? Ge2 N5 1.964(4) . ? Ge2 N3 1.987(3) . ? N2 C13 1.344(6) . ? N3 C23 1.356(6) . ? N3 N4 1.372(5) . ? N4 C21 1.325(6) . ? N5 N6 1.355(5) . ? N5 C33 1.359(6) . ? N6 C31 1.322(6) . ? N7 N8 1.360(5) . ? N7 C43 1.363(6) . ? N8 C41 1.320(6) . ? F10 C10 1.332(7) . ? C10 F12 1.307(6) . ? C10 F11 1.324(7) . ? C10 C11 1.482(7) . ? C11 C12 1.370(6) . ? C12 C13 1.378(6) . ? C12 H12 0.9500 . ? C13 C14 1.483(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? F20 C20 1.338(6) . ? C20 F22 1.333(6) . ? C20 F21 1.334(6) . ? C20 C21 1.492(7) . ? C21 C22 1.361(6) . ? C22 C23 1.364(6) . ? C22 H22 0.9500 . ? C23 C24 1.498(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 F30 1.302(6) . ? C30 F31 1.312(7) . ? C30 F32 1.325(7) . ? C30 C31 1.457(7) . ? C31 C32 1.383(7) . ? C32 C33 1.361(7) . ? C32 H32 0.9500 . ? C33 C34 1.493(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? F40 C40 1.329(6) . ? C40 F41 1.327(6) . ? C40 F42 1.340(6) . ? C40 C41 1.488(6) . ? C41 C42 1.383(6) . ? C42 C43 1.375(6) . ? C42 H42 0.9500 . ? C43 C44 1.495(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C70 C75 1.362(7) . ? C70 C71 1.367(7) . ? C70 H70 0.9500 . ? C75 C74 1.371(7) . ? C75 H75 0.9500 . ? C74 C73 1.368(7) . ? C74 H74 0.9500 . ? C71 C76 1.24(2) . ? C71 C72 1.365(7) . ? C72 C73 1.364(7) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C6 C97 1.368(9) . ? C6 C7 1.372(9) . ? C6 H6 0.9500 . ? C9 C99 1.369(9) . ? C9 C8 1.375(9) . ? C9 H9 0.9500 . ? C7 C8 1.375(10) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C99 C97 1.367(9) . ? C99 C96 1.48(3) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97 0.9500 . ? C4 C5 1.365(8) . ? C4 C3 1.368(9) . ? C4 H4 0.9500 . ? C3 C2 1.366(9) . ? C3 H3 0.9500 . ? C5 C88 1.361(9) . ? C5 C89 1.45(3) . ? C1 C2 1.359(9) . ? C1 C88 1.360(9) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C88 H88 0.9500 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ge1 N4 88.21(15) . . ? N7 Ge1 N2 88.40(14) . . ? N4 Ge1 N2 91.73(14) . . ? C11 N1 N2 106.8(4) . . ? C11 N1 Ge2 124.8(3) . . ? N2 N1 Ge2 127.8(3) . . ? N5 Ge2 N3 92.76(15) . . ? N5 Ge2 N1 91.19(15) . . ? N3 Ge2 N1 91.16(14) . . ? C13 N2 N1 109.0(4) . . ? C13 N2 Ge1 121.5(3) . . ? N1 N2 Ge1 129.4(3) . . ? C23 N3 N4 108.6(4) . . ? C23 N3 Ge2 120.4(3) . . ? N4 N3 Ge2 130.9(3) . . ? C21 N4 N3 106.1(4) . . ? C21 N4 Ge1 127.1(3) . . ? N3 N4 Ge1 126.9(3) . . ? N6 N5 C33 110.4(4) . . ? N6 N5 Ge2 122.6(3) . . ? C33 N5 Ge2 126.7(3) . . ? C31 N6 N5 105.4(4) . . ? N8 N7 C43 110.4(4) . . ? N8 N7 Ge1 108.4(3) . . ? C43 N7 Ge1 141.1(3) . . ? C41 N8 N7 105.4(4) . . ? F12 C10 F11 107.0(5) . . ? F12 C10 F10 107.4(5) . . ? F11 C10 F10 105.4(5) . . ? F12 C10 C11 111.1(5) . . ? F11 C10 C11 112.9(5) . . ? F10 C10 C11 112.7(5) . . ? N1 C11 C12 110.0(4) . . ? N1 C11 C10 121.7(4) . . ? C12 C11 C10 128.2(5) . . ? C11 C12 C13 105.5(4) . . ? C11 C12 H12 127.3 . . ? C13 C12 H12 127.3 . . ? N2 C13 C12 108.7(4) . . ? N2 C13 C14 122.9(4) . . ? C12 C13 C14 128.4(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? F22 C20 F21 107.6(5) . . ? F22 C20 F20 106.5(5) . . ? F21 C20 F20 105.7(5) . . ? F22 C20 C21 114.1(5) . . ? F21 C20 C21 111.7(5) . . ? F20 C20 C21 110.6(4) . . ? N4 C21 C22 111.4(4) . . ? N4 C21 C20 123.6(4) . . ? C22 C21 C20 124.9(5) . . ? C21 C22 C23 105.7(4) . . ? C21 C22 H22 127.2 . . ? C23 C22 H22 127.2 . . ? N3 C23 C22 108.2(4) . . ? N3 C23 C24 122.8(4) . . ? C22 C23 C24 128.9(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F30 C30 F31 107.5(6) . . ? F30 C30 F32 104.4(6) . . ? F31 C30 F32 103.1(5) . . ? F30 C30 C31 113.6(5) . . ? F31 C30 C31 114.1(5) . . ? F32 C30 C31 113.1(6) . . ? N6 C31 C32 111.7(5) . . ? N6 C31 C30 120.7(5) . . ? C32 C31 C30 127.7(5) . . ? C33 C32 C31 105.1(5) . . ? C33 C32 H32 127.4 . . ? C31 C32 H32 127.4 . . ? N5 C33 C32 107.4(4) . . ? N5 C33 C34 122.1(5) . . ? C32 C33 C34 130.4(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? F41 C40 F40 107.3(4) . . ? F41 C40 F42 106.3(4) . . ? F40 C40 F42 105.8(4) . . ? F41 C40 C41 111.5(4) . . ? F40 C40 C41 112.7(4) . . ? F42 C40 C41 112.9(4) . . ? N8 C41 C42 112.1(4) . . ? N8 C41 C40 119.3(4) . . ? C42 C41 C40 128.4(4) . . ? C43 C42 C41 104.9(4) . . ? C43 C42 H42 127.5 . . ? C41 C42 H42 127.5 . . ? N7 C43 C42 107.1(4) . . ? N7 C43 C44 123.7(4) . . ? C42 C43 C44 129.2(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C75 C70 C71 117.8(13) . . ? C75 C70 H70 121.1 . . ? C71 C70 H70 121.1 . . ? C70 C75 C74 124.2(11) . . ? C70 C75 H75 117.9 . . ? C74 C75 H75 117.9 . . ? C73 C74 C75 115.0(11) . . ? C73 C74 H74 122.5 . . ? C75 C74 H74 122.5 . . ? C76 C71 C72 119.7(9) . . ? C76 C71 C70 119.1(9) . . ? C72 C71 C70 121.1(15) . . ? C73 C72 C71 118.1(13) . . ? C73 C72 H72 120.9 . . ? C71 C72 H72 120.9 . . ? C72 C73 C74 123.8(11) . . ? C72 C73 H73 118.1 . . ? C74 C73 H73 118.1 . . ? C97 C6 C7 119.2(16) . . ? C97 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C99 C9 C8 122.9(14) . . ? C99 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C6 C7 C8 120(2) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 118.8(16) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C97 C99 C9 116.4(16) . . ? C97 C99 C96 121.5(10) . . ? C9 C99 C96 122.1(10) . . ? C99 C97 C6 122.9(14) . . ? C99 C97 H97 118.5 . . ? C6 C97 H97 118.5 . . ? C5 C4 C3 119.8(8) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C2 C3 C4 119.7(8) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C88 C5 C4 119.5(11) . . ? C88 C5 C89 120.2(8) . . ? C4 C5 C89 120.2(8) . . ? C2 C1 C88 119.0(10) . . ? C2 C1 H1 120.5 . . ? C88 C1 H1 120.5 . . ? C1 C2 C3 120.7(12) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C1 C88 C5 121.1(11) . . ? C1 C88 H88 119.4 . . ? C5 C88 H88 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 N1 Ge2 N5 118.2(4) . . . . ? N2 N1 Ge2 N5 -51.4(4) . . . . ? C11 N1 Ge2 N3 -149.0(4) . . . . ? N2 N1 Ge2 N3 41.4(4) . . . . ? C11 N1 N2 C13 -0.6(5) . . . . ? Ge2 N1 N2 C13 170.5(3) . . . . ? C11 N1 N2 Ge1 178.1(3) . . . . ? Ge2 N1 N2 Ge1 -10.8(6) . . . . ? N7 Ge1 N2 C13 64.0(4) . . . . ? N4 Ge1 N2 C13 152.1(4) . . . . ? N7 Ge1 N2 N1 -114.6(4) . . . . ? N4 Ge1 N2 N1 -26.4(4) . . . . ? N5 Ge2 N3 C23 -123.6(4) . . . . ? N1 Ge2 N3 C23 145.1(4) . . . . ? N5 Ge2 N3 N4 52.3(4) . . . . ? N1 Ge2 N3 N4 -39.0(4) . . . . ? C23 N3 N4 C21 1.9(5) . . . . ? Ge2 N3 N4 C21 -174.4(3) . . . . ? C23 N3 N4 Ge1 -178.8(3) . . . . ? Ge2 N3 N4 Ge1 4.9(5) . . . . ? N7 Ge1 N4 C21 -63.2(4) . . . . ? N2 Ge1 N4 C21 -151.5(4) . . . . ? N7 Ge1 N4 N3 117.6(3) . . . . ? N2 Ge1 N4 N3 29.3(3) . . . . ? N3 Ge2 N5 N6 -32.2(4) . . . . ? N1 Ge2 N5 N6 59.0(4) . . . . ? N3 Ge2 N5 C33 141.6(4) . . . . ? N1 Ge2 N5 C33 -127.2(4) . . . . ? C33 N5 N6 C31 0.6(5) . . . . ? Ge2 N5 N6 C31 175.3(3) . . . . ? N4 Ge1 N7 N8 132.2(3) . . . . ? N2 Ge1 N7 N8 -136.0(3) . . . . ? N4 Ge1 N7 C43 -46.8(5) . . . . ? N2 Ge1 N7 C43 45.0(5) . . . . ? C43 N7 N8 C41 -0.4(5) . . . . ? Ge1 N7 N8 C41 -179.7(3) . . . . ? N2 N1 C11 C12 0.1(5) . . . . ? Ge2 N1 C11 C12 -171.3(3) . . . . ? N2 N1 C11 C10 179.4(5) . . . . ? Ge2 N1 C11 C10 7.9(7) . . . . ? F12 C10 C11 N1 179.8(5) . . . . ? F11 C10 C11 N1 -60.0(7) . . . . ? F10 C10 C11 N1 59.3(7) . . . . ? F12 C10 C11 C12 -1.1(9) . . . . ? F11 C10 C11 C12 119.1(6) . . . . ? F10 C10 C11 C12 -121.6(6) . . . . ? N1 C11 C12 C13 0.4(6) . . . . ? C10 C11 C12 C13 -178.8(5) . . . . ? N1 N2 C13 C12 0.9(5) . . . . ? Ge1 N2 C13 C12 -177.9(3) . . . . ? N1 N2 C13 C14 -179.0(4) . . . . ? Ge1 N2 C13 C14 2.2(6) . . . . ? C11 C12 C13 N2 -0.8(6) . . . . ? C11 C12 C13 C14 179.1(5) . . . . ? N3 N4 C21 C22 -1.2(5) . . . . ? Ge1 N4 C21 C22 179.5(3) . . . . ? N3 N4 C21 C20 178.1(5) . . . . ? Ge1 N4 C21 C20 -1.2(7) . . . . ? F22 C20 C21 N4 93.0(6) . . . . ? F21 C20 C21 N4 -29.4(7) . . . . ? F20 C20 C21 N4 -146.9(5) . . . . ? F22 C20 C21 C22 -87.8(7) . . . . ? F21 C20 C21 C22 149.7(5) . . . . ? F20 C20 C21 C22 32.3(8) . . . . ? N4 C21 C22 C23 0.0(6) . . . . ? C20 C21 C22 C23 -179.2(5) . . . . ? N4 N3 C23 C22 -1.9(5) . . . . ? Ge2 N3 C23 C22 174.8(3) . . . . ? N4 N3 C23 C24 -178.6(4) . . . . ? Ge2 N3 C23 C24 -1.8(6) . . . . ? C21 C22 C23 N3 1.1(6) . . . . ? C21 C22 C23 C24 177.6(5) . . . . ? N5 N6 C31 C32 0.2(6) . . . . ? N5 N6 C31 C30 180.0(5) . . . . ? F30 C30 C31 N6 166.4(5) . . . . ? F31 C30 C31 N6 42.7(8) . . . . ? F32 C30 C31 N6 -74.7(7) . . . . ? F30 C30 C31 C32 -13.9(10) . . . . ? F31 C30 C31 C32 -137.5(6) . . . . ? F32 C30 C31 C32 105.0(7) . . . . ? N6 C31 C32 C33 -0.9(6) . . . . ? C30 C31 C32 C33 179.3(6) . . . . ? N6 N5 C33 C32 -1.2(6) . . . . ? Ge2 N5 C33 C32 -175.6(3) . . . . ? N6 N5 C33 C34 -179.4(5) . . . . ? Ge2 N5 C33 C34 6.2(7) . . . . ? C31 C32 C33 N5 1.3(6) . . . . ? C31 C32 C33 C34 179.3(6) . . . . ? N7 N8 C41 C42 0.6(5) . . . . ? N7 N8 C41 C40 176.3(4) . . . . ? F41 C40 C41 N8 158.1(4) . . . . ? F40 C40 C41 N8 37.3(6) . . . . ? F42 C40 C41 N8 -82.4(6) . . . . ? F41 C40 C41 C42 -27.0(7) . . . . ? F40 C40 C41 C42 -147.8(5) . . . . ? F42 C40 C41 C42 92.6(6) . . . . ? N8 C41 C42 C43 -0.5(6) . . . . ? C40 C41 C42 C43 -175.8(5) . . . . ? N8 N7 C43 C42 0.1(5) . . . . ? Ge1 N7 C43 C42 179.0(4) . . . . ? N8 N7 C43 C44 -179.5(5) . . . . ? Ge1 N7 C43 C44 -0.5(9) . . . . ? C41 C42 C43 N7 0.3(5) . . . . ? C41 C42 C43 C44 179.8(5) . . . . ? C71 C70 C75 C74 1.3(18) . . . . ? C70 C75 C74 C73 1.2(19) . . . . ? C75 C70 C71 C76 -178(2) . . . . ? C75 C70 C71 C72 -2(3) . . . . ? C76 C71 C72 C73 177(3) . . . . ? C70 C71 C72 C73 0(3) . . . . ? C71 C72 C73 C74 2(3) . . . . ? C75 C74 C73 C72 -3(3) . . . . ? C97 C6 C7 C8 -0.1(19) . . . . ? C99 C9 C8 C7 0(3) . . . . ? C6 C7 C8 C9 1(2) . . . . ? C8 C9 C99 C97 -1(3) . . . . ? C8 C9 C99 C96 -178.4(14) . . . . ? C9 C99 C97 C6 2(3) . . . . ? C96 C99 C97 C6 179.4(17) . . . . ? C7 C6 C97 C99 -1(3) . . . . ? C5 C4 C3 C2 -1(2) . . . . ? C3 C4 C5 C88 -2(2) . . . . ? C3 C4 C5 C89 179(2) . . . . ? C88 C1 C2 C3 -2(4) . . . . ? C4 C3 C2 C1 3(4) . . . . ? C2 C1 C88 C5 -1(3) . . . . ? C4 C5 C88 C1 3(3) . . . . ? C89 C5 C88 C1 -178(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.617 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.094 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Ge2CF3CF3cat _database_code_depnum_ccdc_archive 'CCDC 718007' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H3 F18 Ge2 N6, C F3 O3 S' _chemical_formula_sum 'C16 H3 F21 Ge2 N6 O3 S' _chemical_formula_weight 903.48 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 19.664(1) _cell_length_b 11.6115(6) _cell_length_c 15.4412(8) _cell_angle_alpha 90.00 _cell_angle_beta 127.789(1) _cell_angle_gamma 90.00 _cell_volume 2786.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11541 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.408 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3079 _exptl_absorpt_correction_T_max 0.4948 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11541 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5899 _reflns_number_gt 5758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0535P)^2^+0.2682P] 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 0.004(6) _refine_ls_number_reflns 5899 _refine_ls_number_parameters 526 _refine_ls_number_restraints 164 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.109 _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 Ge1 Ge 0.443278(17) 0.47728(2) 0.68872(2) 0.02479(8) Uani 1 1 d . . . N1 N 0.58390(15) 0.4047(2) 0.93068(18) 0.0238(5) Uani 1 1 d . . . Ge2 Ge 0.52836(2) 0.24591(2) 0.90483(2) 0.02557(8) Uani 1 1 d . . . N2 N 0.55330(15) 0.4884(2) 0.85346(19) 0.0243(5) Uani 1 1 d . . . S3 S 0.23325(4) 0.32254(6) 0.42831(6) 0.02713(15) Uani 1 1 d . . . N3 N 0.41353(15) 0.3422(2) 0.8301(2) 0.0253(5) Uani 1 1 d . . . N4 N 0.38246(15) 0.4220(2) 0.7497(2) 0.0271(5) Uani 1 1 d . . . N5 N 0.49227(15) 0.2300(2) 0.7503(2) 0.0240(5) Uani 1 1 d . . . N6 N 0.48979(14) 0.3203(2) 0.69250(18) 0.0222(4) Uani 1 1 d . . . O10 O 0.17424(15) 0.2926(2) 0.4515(2) 0.0372(5) Uani 1 1 d . . . F10 F 0.64566(18) 0.7682(2) 0.9043(2) 0.0614(7) Uani 1 1 d . . . C10 C 0.5918(2) 0.6856(3) 0.8377(3) 0.0337(6) Uani 1 1 d . . . F11 F 0.51203(15) 0.72448(18) 0.7879(2) 0.0484(5) Uani 1 1 d . . . O11 O 0.31796(15) 0.3530(2) 0.5243(2) 0.0458(6) Uani 1 1 d . . . C11 C 0.60801(18) 0.5778(2) 0.9000(2) 0.0252(5) Uani 1 1 d . . . F12 F 0.6006(2) 0.6708(2) 0.7602(2) 0.0587(6) Uani 1 1 d . . . O12 O 0.19753(18) 0.3940(3) 0.3351(2) 0.0498(6) Uani 1 1 d . . . C12 C 0.67420(19) 0.5542(3) 1.0081(2) 0.0305(6) Uani 1 1 d . . . H12 H 0.7212 0.6025 1.0601 0.037 Uiso 1 1 calc R . . C13 C 0.65677(18) 0.4456(3) 1.0235(2) 0.0271(6) Uani 1 1 d . . . F13 F 0.72813(19) 0.4537(2) 1.21115(17) 0.0644(8) Uani 1 1 d . . . F14 F 0.78102(14) 0.3409(2) 1.15785(18) 0.0490(5) Uani 1 1 d . . . C14 C 0.7081(2) 0.3827(3) 1.1315(2) 0.0339(7) Uani 1 1 d . . . F15 F 0.66499(15) 0.2945(2) 1.13230(17) 0.0510(5) Uani 1 1 d . . . C20 C 0.2596(2) 0.5621(3) 0.6487(3) 0.0456(9) Uani 1 1 d D . . C21 C 0.31018(19) 0.4666(3) 0.7288(3) 0.0322(7) Uani 1 1 d . B . C22 C 0.2935(2) 0.4162(3) 0.7944(3) 0.0353(7) Uani 1 1 d . . . H22 H 0.2472 0.4315 0.7967 0.042 Uiso 1 1 calc R B . C23 C 0.35984(19) 0.3377(3) 0.8563(2) 0.0297(6) Uani 1 1 d . B . F23 F 0.45234(18) 0.2787(3) 1.03871(19) 0.0603(7) Uani 1 1 d . B . F24 F 0.3773(2) 0.1492(2) 0.9211(2) 0.0679(8) Uani 1 1 d . B . C24 C 0.3759(3) 0.2594(3) 0.9429(3) 0.0407(8) Uani 1 1 d . . . F25 F 0.3190(3) 0.2742(4) 0.9600(4) 0.1009(14) Uani 1 1 d . B . C30 C 0.4981(2) 0.3535(3) 0.5396(3) 0.0373(7) Uani 1 1 d D . . C31 C 0.49362(17) 0.2782(3) 0.6149(2) 0.0253(5) Uani 1 1 d . A . C32 C 0.4985(2) 0.1599(3) 0.6198(3) 0.0309(6) Uani 1 1 d . . . H32 H 0.5019 0.1087 0.5746 0.037 Uiso 1 1 calc R A . C33 C 0.49711(19) 0.1334(2) 0.7055(2) 0.0278(6) Uani 1 1 d . A . C34 C 0.4965(3) 0.0149(3) 0.7441(3) 0.0403(8) Uani 1 1 d D . . C90 C 0.2522(2) 0.1844(3) 0.3898(3) 0.0373(7) Uani 1 1 d . . . F90 F 0.29029(17) 0.1099(2) 0.4718(2) 0.0559(6) Uani 1 1 d . . . F91 F 0.17800(16) 0.1370(3) 0.3075(2) 0.0701(9) Uani 1 1 d . . . F92 F 0.30239(18) 0.1949(2) 0.3607(2) 0.0597(6) Uani 1 1 d . . . F30 F 0.5201(6) 0.2982(8) 0.4865(6) 0.078(3) Uani 0.50 1 d PDU A 1 F31 F 0.5508(5) 0.4427(7) 0.5915(9) 0.056(3) Uani 0.50 1 d PDU A 1 F32 F 0.4221(4) 0.4044(7) 0.4635(5) 0.059(2) Uani 0.50 1 d PDU A 1 F30' F 0.5590(5) 0.3077(7) 0.5362(7) 0.071(2) Uani 0.50 1 d PDU A 2 F31' F 0.5254(5) 0.4587(6) 0.5797(9) 0.054(2) Uani 0.50 1 d PDU A 2 F32' F 0.4280(4) 0.3615(8) 0.4403(5) 0.073(3) Uani 0.50 1 d PDU A 2 F20 F 0.1766(7) 0.5304(12) 0.5926(13) 0.056(4) Uani 0.20 1 d PDU B 1 F21 F 0.2698(13) 0.5782(16) 0.5727(14) 0.049(5) Uani 0.20 1 d PDU B 1 F22 F 0.2681(9) 0.6561(10) 0.6945(11) 0.050(4) Uani 0.20 1 d PDU B 1 F20' F 0.2500(4) 0.5481(5) 0.5570(4) 0.0566(13) Uani 0.80 1 d PDU B 2 F21' F 0.3029(4) 0.6618(4) 0.6899(4) 0.098(2) Uani 0.80 1 d PDU B 2 F22' F 0.1857(3) 0.5769(6) 0.6247(5) 0.101(2) Uani 0.80 1 d PDU B 2 F33 F 0.5380(4) -0.0557(6) 0.7189(6) 0.0539(16) Uani 0.50 1 d PDU A 1 F34 F 0.5370(5) 0.0033(10) 0.8470(4) 0.061(3) Uani 0.50 1 d PDU A 1 F35 F 0.4196(4) -0.0262(9) 0.6881(7) 0.081(3) Uani 0.50 1 d PDU A 1 F33' F 0.4979(7) -0.0641(7) 0.6848(7) 0.098(4) Uani 0.50 1 d PDU A 2 F34' F 0.5600(5) -0.0020(11) 0.8467(5) 0.061(3) Uani 0.50 1 d PDU A 2 F35' F 0.4260(4) -0.0014(9) 0.7350(9) 0.104(4) Uani 0.50 1 d PDU A 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 Ge1 0.02501(14) 0.02028(14) 0.02245(13) 0.00590(11) 0.01116(11) 0.00356(11) N1 0.0211(10) 0.0246(11) 0.0183(10) 0.0044(9) 0.0082(9) 0.0062(9) Ge2 0.02968(15) 0.02349(14) 0.02228(13) 0.00644(10) 0.01528(11) 0.00360(11) N2 0.0231(11) 0.0210(11) 0.0221(11) 0.0023(9) 0.0104(9) 0.0033(8) S3 0.0192(3) 0.0301(4) 0.0270(3) -0.0019(3) 0.0115(3) -0.0065(3) N3 0.0243(11) 0.0268(12) 0.0230(11) 0.0020(9) 0.0135(9) 0.0013(9) N4 0.0218(11) 0.0271(12) 0.0258(11) 0.0029(9) 0.0111(9) 0.0055(9) N5 0.0258(11) 0.0199(10) 0.0238(11) 0.0052(9) 0.0139(10) 0.0015(9) N6 0.0209(10) 0.0207(11) 0.0195(10) 0.0052(8) 0.0096(8) 0.0013(8) O10 0.0318(11) 0.0386(13) 0.0465(13) 0.0009(11) 0.0267(11) -0.0047(10) F10 0.0582(15) 0.0347(12) 0.0544(14) -0.0059(10) 0.0157(12) -0.0216(11) C10 0.0344(15) 0.0259(14) 0.0334(16) -0.0016(12) 0.0169(13) -0.0056(12) F11 0.0399(11) 0.0320(9) 0.0576(14) 0.0145(10) 0.0219(10) 0.0093(9) O11 0.0232(10) 0.0502(15) 0.0444(14) -0.0188(12) 0.0107(10) -0.0070(10) C11 0.0247(12) 0.0226(13) 0.0246(13) -0.0012(10) 0.0133(11) 0.0018(10) F12 0.0829(18) 0.0569(15) 0.0544(14) 0.0125(12) 0.0512(14) 0.0048(13) O12 0.0460(14) 0.0531(16) 0.0500(15) 0.0190(13) 0.0292(13) 0.0036(12) C12 0.0234(13) 0.0328(15) 0.0250(14) -0.0043(12) 0.0096(11) 0.0012(11) C13 0.0229(13) 0.0337(15) 0.0193(12) 0.0019(11) 0.0103(10) 0.0080(11) F13 0.0776(18) 0.0653(16) 0.0208(10) -0.0023(10) 0.0152(11) 0.0247(13) F14 0.0327(10) 0.0636(14) 0.0350(10) 0.0148(11) 0.0127(8) 0.0221(10) C14 0.0308(15) 0.0423(18) 0.0197(13) 0.0038(12) 0.0109(12) 0.0095(13) F15 0.0446(12) 0.0667(15) 0.0307(10) 0.0179(10) 0.0175(9) 0.0038(11) C20 0.043(2) 0.050(2) 0.0314(16) 0.0057(16) 0.0164(15) 0.0246(17) C21 0.0225(14) 0.0356(16) 0.0261(14) -0.0058(12) 0.0085(11) 0.0067(11) C22 0.0256(14) 0.0449(18) 0.0329(15) -0.0090(14) 0.0166(12) 0.0030(13) C23 0.0261(13) 0.0353(16) 0.0268(14) -0.0063(12) 0.0158(12) -0.0034(12) F23 0.0641(16) 0.0706(15) 0.0278(10) -0.0016(11) 0.0188(11) -0.0108(13) F24 0.105(2) 0.0406(13) 0.0508(14) -0.0019(11) 0.0436(15) -0.0204(14) C24 0.0390(18) 0.053(2) 0.0351(18) 0.0009(15) 0.0252(16) -0.0040(15) F25 0.082(2) 0.156(4) 0.113(3) 0.062(3) 0.085(2) 0.041(2) C30 0.0370(16) 0.0481(19) 0.0326(15) 0.0018(14) 0.0242(13) -0.0059(14) C31 0.0181(12) 0.0316(14) 0.0212(13) 0.0018(11) 0.0095(10) -0.0020(10) C32 0.0319(15) 0.0301(15) 0.0288(14) -0.0034(12) 0.0176(12) 0.0004(12) C33 0.0276(13) 0.0197(13) 0.0298(14) 0.0011(11) 0.0144(12) 0.0024(10) C34 0.047(2) 0.0222(15) 0.0389(18) 0.0045(12) 0.0198(16) 0.0008(13) C90 0.0255(14) 0.0428(18) 0.0394(17) -0.0086(14) 0.0178(13) -0.0073(12) F90 0.0594(14) 0.0399(12) 0.0711(15) 0.0093(11) 0.0413(13) 0.0091(10) F91 0.0360(11) 0.0756(19) 0.0682(16) -0.0441(15) 0.0163(11) -0.0116(12) F92 0.0639(15) 0.0688(17) 0.0729(17) -0.0079(13) 0.0555(15) -0.0023(13) F30 0.133(7) 0.079(4) 0.070(5) 0.008(4) 0.087(5) 0.014(5) F31 0.045(4) 0.060(5) 0.049(3) 0.006(3) 0.023(3) -0.024(3) F32 0.046(3) 0.080(5) 0.036(3) 0.025(3) 0.019(2) -0.003(3) F30' 0.089(5) 0.080(4) 0.097(6) 0.024(4) 0.084(5) 0.016(4) F31' 0.081(6) 0.036(3) 0.068(5) 0.006(3) 0.058(5) -0.006(3) F32' 0.064(4) 0.111(7) 0.026(3) 0.017(3) 0.018(3) -0.025(4) F20 0.024(5) 0.052(7) 0.057(7) 0.005(5) 0.007(4) 0.014(5) F21 0.060(8) 0.043(9) 0.056(8) 0.020(6) 0.042(7) 0.029(6) F22 0.078(9) 0.028(6) 0.036(5) 0.004(4) 0.032(6) 0.028(6) F20' 0.071(3) 0.047(3) 0.0408(19) 0.0099(16) 0.0284(19) 0.025(2) F21' 0.112(4) 0.037(2) 0.068(3) 0.0001(18) 0.017(3) 0.011(2) F22' 0.080(3) 0.142(5) 0.101(4) 0.060(4) 0.065(3) 0.084(3) F33 0.075(4) 0.023(3) 0.070(4) -0.001(3) 0.048(4) 0.007(3) F34 0.106(7) 0.033(3) 0.047(4) 0.002(3) 0.049(4) -0.008(4) F35 0.059(4) 0.053(4) 0.092(5) 0.019(4) 0.027(3) -0.024(3) F33' 0.186(9) 0.027(3) 0.061(4) -0.015(3) 0.066(6) -0.015(5) F34' 0.049(3) 0.049(4) 0.057(4) 0.032(3) 0.019(3) 0.004(3) F35' 0.068(4) 0.061(5) 0.174(9) 0.059(6) 0.070(5) 0.001(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 Ge1 N6 2.024(2) . ? Ge1 N4 2.027(3) . ? Ge1 N2 2.103(2) . ? N1 C13 1.347(4) . ? N1 N2 1.359(3) . ? N1 Ge2 2.054(2) . ? Ge2 N5 2.039(3) . ? Ge2 N3 2.118(2) . ? N2 C11 1.343(4) . ? S3 O12 1.420(3) . ? S3 O11 1.439(2) . ? S3 O10 1.451(2) . ? S3 C90 1.827(4) . ? N3 C23 1.343(4) . ? N3 N4 1.358(3) . ? N4 C21 1.353(4) . ? N5 C33 1.351(4) . ? N5 N6 1.359(3) . ? N6 C31 1.338(4) . ? F10 C10 1.329(4) . ? C10 F12 1.321(4) . ? C10 F11 1.333(4) . ? C10 C11 1.489(4) . ? C11 C12 1.376(4) . ? C12 C13 1.366(5) . ? C12 H12 0.9500 . ? C13 C14 1.506(4) . ? F13 C14 1.325(4) . ? F14 C14 1.319(4) . ? C14 F15 1.334(4) . ? C20 F22 1.255(9) . ? C20 F22' 1.272(6) . ? C20 F20' 1.319(6) . ? C20 F21 1.319(10) . ? C20 F21' 1.344(6) . ? C20 F20 1.348(9) . ? C20 C21 1.496(5) . ? C21 C22 1.372(5) . ? C22 C23 1.385(5) . ? C22 H22 0.9500 . ? C23 C24 1.482(5) . ? F23 C24 1.332(5) . ? F24 C24 1.328(5) . ? C24 F25 1.308(5) . ? C30 F32' 1.292(6) . ? C30 F30 1.307(6) . ? C30 F31' 1.325(7) . ? C30 F31 1.332(7) . ? C30 F30' 1.341(6) . ? C30 F32 1.346(6) . ? C30 C31 1.499(4) . ? C31 C32 1.376(4) . ? C32 C33 1.375(4) . ? C32 H32 0.9500 . ? C33 C34 1.502(4) . ? C34 F34 1.276(7) . ? C34 F35 1.289(7) . ? C34 F34' 1.298(7) . ? C34 F33' 1.308(7) . ? C34 F35' 1.319(7) . ? C34 F33 1.371(6) . ? C90 F92 1.316(4) . ? C90 F90 1.323(4) . ? C90 F91 1.332(4) . ? 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 N6 Ge1 N4 94.96(9) . . ? N6 Ge1 N2 84.74(9) . . ? N4 Ge1 N2 85.41(10) . . ? C13 N1 N2 107.0(2) . . ? C13 N1 Ge2 128.0(2) . . ? N2 N1 Ge2 125.04(18) . . ? N5 Ge2 N1 94.09(9) . . ? N5 Ge2 N3 85.41(10) . . ? N1 Ge2 N3 83.95(9) . . ? C11 N2 N1 107.7(2) . . ? C11 N2 Ge1 125.96(19) . . ? N1 N2 Ge1 126.27(18) . . ? O12 S3 O11 116.23(18) . . ? O12 S3 O10 114.62(16) . . ? O11 S3 O10 113.65(16) . . ? O12 S3 C90 104.84(18) . . ? O11 S3 C90 102.25(15) . . ? O10 S3 C90 102.94(16) . . ? C23 N3 N4 107.8(2) . . ? C23 N3 Ge2 126.0(2) . . ? N4 N3 Ge2 126.19(18) . . ? C21 N4 N3 107.3(3) . . ? C21 N4 Ge1 126.9(2) . . ? N3 N4 Ge1 125.30(18) . . ? C33 N5 N6 106.9(2) . . ? C33 N5 Ge2 126.25(19) . . ? N6 N5 Ge2 123.04(19) . . ? C31 N6 N5 107.9(2) . . ? C31 N6 Ge1 125.15(19) . . ? N5 N6 Ge1 123.23(18) . . ? F12 C10 F10 108.1(3) . . ? F12 C10 F11 106.5(3) . . ? F10 C10 F11 107.5(3) . . ? F12 C10 C11 112.4(3) . . ? F10 C10 C11 110.6(3) . . ? F11 C10 C11 111.6(3) . . ? N2 C11 C12 110.3(3) . . ? N2 C11 C10 121.3(3) . . ? C12 C11 C10 128.3(3) . . ? C13 C12 C11 104.1(3) . . ? C13 C12 H12 128.0 . . ? C11 C12 H12 128.0 . . ? N1 C13 C12 110.9(3) . . ? N1 C13 C14 124.1(3) . . ? C12 C13 C14 124.8(3) . . ? F14 C14 F13 107.1(3) . . ? F14 C14 F15 107.0(3) . . ? F13 C14 F15 107.3(3) . . ? F14 C14 C13 112.6(3) . . ? F13 C14 C13 110.0(3) . . ? F15 C14 C13 112.6(3) . . ? F22 C20 F22' 77.3(6) . . ? F22 C20 F20' 126.4(8) . . ? F22' C20 F20' 108.4(4) . . ? F22 C20 F21 109.7(8) . . ? F22' C20 F21 119.3(10) . . ? F22' C20 F21' 107.5(4) . . ? F20' C20 F21' 104.2(5) . . ? F21 C20 F21' 84.3(8) . . ? F22 C20 F20 106.9(7) . . ? F20' C20 F20 87.4(8) . . ? F21 C20 F20 104.5(8) . . ? F21' C20 F20 134.9(7) . . ? F22 C20 C21 112.8(8) . . ? F22' C20 C21 113.8(4) . . ? F20' C20 C21 112.4(4) . . ? F21 C20 C21 117.0(9) . . ? F21' C20 C21 109.9(3) . . ? F20 C20 C21 105.0(8) . . ? N4 C21 C22 110.6(3) . . ? N4 C21 C20 123.3(3) . . ? C22 C21 C20 126.0(3) . . ? C21 C22 C23 103.9(3) . . ? C21 C22 H22 128.1 . . ? C23 C22 H22 128.1 . . ? N3 C23 C22 110.4(3) . . ? N3 C23 C24 121.5(3) . . ? C22 C23 C24 128.0(3) . . ? F25 C24 F24 109.3(4) . . ? F25 C24 F23 106.0(4) . . ? F24 C24 F23 105.0(3) . . ? F25 C24 C23 111.5(3) . . ? F24 C24 C23 112.9(3) . . ? F23 C24 C23 111.8(3) . . ? F32' C30 F30 79.2(5) . . ? F32' C30 F31' 108.7(6) . . ? F30 C30 F31' 123.4(8) . . ? F32' C30 F31 122.0(8) . . ? F30 C30 F31 108.9(6) . . ? F32' C30 F30' 108.1(5) . . ? F31' C30 F30' 105.6(5) . . ? F31 C30 F30' 86.9(6) . . ? F30 C30 F32 106.6(5) . . ? F31' C30 F32 85.3(6) . . ? F31 C30 F32 102.9(5) . . ? F30' C30 F32 132.9(5) . . ? F32' C30 C31 115.8(5) . . ? F30 C30 C31 113.6(5) . . ? F31' C30 C31 112.0(6) . . ? F31 C30 C31 112.4(6) . . ? F30' C30 C31 106.1(4) . . ? F32 C30 C31 111.8(4) . . ? N6 C31 C32 110.9(3) . . ? N6 C31 C30 122.9(3) . . ? C32 C31 C30 126.1(3) . . ? C33 C32 C31 103.6(3) . . ? C33 C32 H32 128.2 . . ? C31 C32 H32 128.2 . . ? N5 C33 C32 110.8(3) . . ? N5 C33 C34 122.5(3) . . ? C32 C33 C34 126.6(3) . . ? F34 C34 F35 112.1(6) . . ? F35 C34 F34' 128.2(8) . . ? F34 C34 F33' 122.2(8) . . ? F35 C34 F33' 77.9(7) . . ? F34' C34 F33' 109.4(6) . . ? F34 C34 F35' 86.0(7) . . ? F34' C34 F35' 105.6(6) . . ? F33' C34 F35' 107.3(6) . . ? F34 C34 F33 105.4(5) . . ? F35 C34 F33 104.3(5) . . ? F34' C34 F33 87.8(6) . . ? F35' C34 F33 130.8(6) . . ? F34 C34 C33 116.1(6) . . ? F35 C34 C33 111.3(6) . . ? F34' C34 C33 112.8(6) . . ? F33' C34 C33 110.8(5) . . ? F35' C34 C33 110.6(5) . . ? F33 C34 C33 106.6(5) . . ? F92 C90 F90 106.5(3) . . ? F92 C90 F91 108.9(3) . . ? F90 C90 F91 106.8(3) . . ? F92 C90 S3 112.0(3) . . ? F90 C90 S3 111.8(2) . . ? F91 C90 S3 110.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 N1 Ge2 N5 -141.3(2) . . . . ? N2 N1 Ge2 N5 37.0(2) . . . . ? C13 N1 Ge2 N3 133.8(2) . . . . ? N2 N1 Ge2 N3 -47.9(2) . . . . ? C13 N1 N2 C11 0.5(3) . . . . ? Ge2 N1 N2 C11 -178.12(19) . . . . ? C13 N1 N2 Ge1 177.87(19) . . . . ? Ge2 N1 N2 Ge1 -0.7(3) . . . . ? N6 Ge1 N2 C11 131.5(2) . . . . ? N4 Ge1 N2 C11 -133.0(2) . . . . ? N6 Ge1 N2 N1 -45.4(2) . . . . ? N4 Ge1 N2 N1 50.0(2) . . . . ? N5 Ge2 N3 C23 140.5(3) . . . . ? N1 Ge2 N3 C23 -124.9(3) . . . . ? N5 Ge2 N3 N4 -41.8(2) . . . . ? N1 Ge2 N3 N4 52.8(2) . . . . ? C23 N3 N4 C21 0.8(3) . . . . ? Ge2 N3 N4 C21 -177.3(2) . . . . ? C23 N3 N4 Ge1 173.4(2) . . . . ? Ge2 N3 N4 Ge1 -4.7(3) . . . . ? N6 Ge1 N4 C21 -150.0(3) . . . . ? N2 Ge1 N4 C21 125.7(3) . . . . ? N6 Ge1 N4 N3 38.9(2) . . . . ? N2 Ge1 N4 N3 -45.4(2) . . . . ? N1 Ge2 N5 C33 138.9(2) . . . . ? N3 Ge2 N5 C33 -137.5(3) . . . . ? N1 Ge2 N5 N6 -16.0(2) . . . . ? N3 Ge2 N5 N6 67.6(2) . . . . ? C33 N5 N6 C31 -0.4(3) . . . . ? Ge2 N5 N6 C31 158.75(18) . . . . ? C33 N5 N6 Ge1 158.72(19) . . . . ? Ge2 N5 N6 Ge1 -42.2(3) . . . . ? N4 Ge1 N6 C31 139.9(2) . . . . ? N2 Ge1 N6 C31 -135.2(2) . . . . ? N4 Ge1 N6 N5 -15.5(2) . . . . ? N2 Ge1 N6 N5 69.4(2) . . . . ? N1 N2 C11 C12 -0.7(3) . . . . ? Ge1 N2 C11 C12 -178.2(2) . . . . ? N1 N2 C11 C10 -178.4(3) . . . . ? Ge1 N2 C11 C10 4.2(4) . . . . ? F12 C10 C11 N2 -69.6(4) . . . . ? F10 C10 C11 N2 169.5(3) . . . . ? F11 C10 C11 N2 49.9(4) . . . . ? F12 C10 C11 C12 113.2(4) . . . . ? F10 C10 C11 C12 -7.7(5) . . . . ? F11 C10 C11 C12 -127.3(3) . . . . ? N2 C11 C12 C13 0.7(3) . . . . ? C10 C11 C12 C13 178.1(3) . . . . ? N2 N1 C13 C12 0.0(3) . . . . ? Ge2 N1 C13 C12 178.5(2) . . . . ? N2 N1 C13 C14 175.8(3) . . . . ? Ge2 N1 C13 C14 -5.6(4) . . . . ? C11 C12 C13 N1 -0.4(3) . . . . ? C11 C12 C13 C14 -176.2(3) . . . . ? N1 C13 C14 F14 107.5(3) . . . . ? C12 C13 C14 F14 -77.2(4) . . . . ? N1 C13 C14 F13 -133.2(3) . . . . ? C12 C13 C14 F13 42.2(4) . . . . ? N1 C13 C14 F15 -13.6(4) . . . . ? C12 C13 C14 F15 161.7(3) . . . . ? N3 N4 C21 C22 -0.3(3) . . . . ? Ge1 N4 C21 C22 -172.8(2) . . . . ? N3 N4 C21 C20 176.7(3) . . . . ? Ge1 N4 C21 C20 4.3(4) . . . . ? F22 C20 C21 N4 -107.2(8) . . . . ? F22' C20 C21 N4 167.1(4) . . . . ? F20' C20 C21 N4 43.3(5) . . . . ? F21 C20 C21 N4 21.5(9) . . . . ? F21' C20 C21 N4 -72.3(5) . . . . ? F20 C20 C21 N4 136.8(7) . . . . ? F22 C20 C21 C22 69.4(8) . . . . ? F22' C20 C21 C22 -16.3(6) . . . . ? F20' C20 C21 C22 -140.1(4) . . . . ? F21 C20 C21 C22 -161.9(9) . . . . ? F21' C20 C21 C22 104.3(5) . . . . ? F20 C20 C21 C22 -46.6(8) . . . . ? N4 C21 C22 C23 -0.2(4) . . . . ? C20 C21 C22 C23 -177.2(3) . . . . ? N4 N3 C23 C22 -0.9(3) . . . . ? Ge2 N3 C23 C22 177.1(2) . . . . ? N4 N3 C23 C24 -179.3(3) . . . . ? Ge2 N3 C23 C24 -1.3(4) . . . . ? C21 C22 C23 N3 0.7(4) . . . . ? C21 C22 C23 C24 179.0(3) . . . . ? N3 C23 C24 F25 175.9(4) . . . . ? C22 C23 C24 F25 -2.2(6) . . . . ? N3 C23 C24 F24 -60.6(4) . . . . ? C22 C23 C24 F24 121.3(4) . . . . ? N3 C23 C24 F23 57.4(4) . . . . ? C22 C23 C24 F23 -120.7(4) . . . . ? N5 N6 C31 C32 0.2(3) . . . . ? Ge1 N6 C31 C32 -158.4(2) . . . . ? N5 N6 C31 C30 -176.0(3) . . . . ? Ge1 N6 C31 C30 25.4(4) . . . . ? F32' C30 C31 N6 -105.0(6) . . . . ? F30 C30 C31 N6 165.9(5) . . . . ? F31' C30 C31 N6 20.4(6) . . . . ? F31 C30 C31 N6 41.7(6) . . . . ? F30' C30 C31 N6 135.1(5) . . . . ? F32 C30 C31 N6 -73.4(5) . . . . ? F32' C30 C31 C32 79.5(6) . . . . ? F30 C30 C31 C32 -9.6(6) . . . . ? F31' C30 C31 C32 -155.1(5) . . . . ? F31 C30 C31 C32 -133.8(5) . . . . ? F30' C30 C31 C32 -40.4(6) . . . . ? F32 C30 C31 C32 111.0(5) . . . . ? N6 C31 C32 C33 0.1(3) . . . . ? C30 C31 C32 C33 176.1(3) . . . . ? N6 N5 C33 C32 0.4(3) . . . . ? Ge2 N5 C33 C32 -157.8(2) . . . . ? N6 N5 C33 C34 -176.8(3) . . . . ? Ge2 N5 C33 C34 24.9(4) . . . . ? C31 C32 C33 N5 -0.3(3) . . . . ? C31 C32 C33 C34 176.8(3) . . . . ? N5 C33 C34 F34 -37.5(7) . . . . ? C32 C33 C34 F34 145.7(6) . . . . ? N5 C33 C34 F35 92.4(6) . . . . ? C32 C33 C34 F35 -84.4(6) . . . . ? N5 C33 C34 F34' -59.8(6) . . . . ? C32 C33 C34 F34' 123.4(6) . . . . ? N5 C33 C34 F33' 177.2(6) . . . . ? C32 C33 C34 F33' 0.4(7) . . . . ? N5 C33 C34 F35' 58.3(7) . . . . ? C32 C33 C34 F35' -118.5(6) . . . . ? N5 C33 C34 F33 -154.5(4) . . . . ? C32 C33 C34 F33 28.7(5) . . . . ? O12 S3 C90 F92 57.0(3) . . . . ? O11 S3 C90 F92 -64.7(3) . . . . ? O10 S3 C90 F92 177.2(3) . . . . ? O12 S3 C90 F90 176.5(2) . . . . ? O11 S3 C90 F90 54.8(3) . . . . ? O10 S3 C90 F90 -63.3(3) . . . . ? O12 S3 C90 F91 -64.7(3) . . . . ? O11 S3 C90 F91 173.6(3) . . . . ? O10 S3 C90 F91 55.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.449 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.054 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Ge2MeCF3cat _database_code_depnum_ccdc_archive 'CCDC 718008' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 F9 Ge2 N6, C F3 O3 S' _chemical_formula_sum 'C16 H12 F12 Ge2 N6 O3 S' _chemical_formula_weight 741.56 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7923(5) _cell_length_b 14.6965(8) _cell_length_c 40.138(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.056(1) _cell_angle_gamma 90.00 _cell_volume 5157.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 32897 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 24.75 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 2.531 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4712 _exptl_absorpt_correction_T_max 0.4712 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32897 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.75 _reflns_number_total 8798 _reflns_number_gt 7906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0248P)^2^+16.5127P] 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 8798 _refine_ls_number_parameters 799 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.75541(5) 0.13731(3) 0.057047(11) 0.02884(12) Uani 1 1 d . . . Ge2 Ge 1.15984(5) 0.21055(3) 0.068978(12) 0.03088(12) Uani 1 1 d . . . Ge3 Ge 0.31604(6) 0.70459(4) 0.125052(13) 0.04048(14) Uani 1 1 d . . . Ge4 Ge 0.32327(7) 0.62940(4) 0.213475(15) 0.05238(17) Uani 1 1 d . . . S2 S 0.13778(14) 0.97074(8) 0.13734(3) 0.0376(3) Uani 1 1 d . . . N5 N 0.8648(4) 0.1841(2) 0.09908(9) 0.0282(8) Uani 1 1 d . . . F11 F 0.7149(3) -0.0923(2) 0.06446(7) 0.0501(7) Uani 1 1 d . . . N2 N 1.0833(4) 0.0825(2) 0.05529(8) 0.0272(8) Uani 1 1 d . . . N6 N 1.0149(4) 0.2102(2) 0.10365(9) 0.0290(8) Uani 1 1 d . . . N11 N 0.4319(5) 0.7387(3) 0.19768(10) 0.0412(10) Uani 1 1 d . . . N4 N 0.9983(4) 0.2588(2) 0.03377(9) 0.0291(8) Uani 1 1 d . . . N1 N 0.9330(4) 0.0574(2) 0.04974(8) 0.0268(7) Uani 1 1 d . . . N8 N 0.3968(5) 0.5832(3) 0.14389(10) 0.0392(9) Uani 1 1 d . . . F12 F 0.6822(3) -0.0408(2) 0.01503(7) 0.0576(8) Uani 1 1 d . . . N7 N 0.3991(4) 0.5567(3) 0.17681(10) 0.0388(9) Uani 1 1 d . . . F22 F 0.5301(4) 0.2837(3) 0.02064(10) 0.0841(12) Uani 1 1 d . . . C21 C 0.7786(5) 0.2823(3) 0.00478(12) 0.0369(10) Uani 1 1 d . . . N3 N 0.8471(4) 0.2351(2) 0.03092(9) 0.0321(8) Uani 1 1 d . . . O5 O 0.2072(4) 0.8855(2) 0.12926(9) 0.0483(9) Uani 1 1 d . . . N12 N 0.4424(5) 0.7607(3) 0.16502(9) 0.0374(9) Uani 1 1 d . . . C33 C 1.0529(5) 0.2286(3) 0.13624(11) 0.0348(10) Uani 1 1 d . . . C11 C 0.9305(5) -0.0320(3) 0.04296(10) 0.0297(9) Uani 1 1 d . . . F31 F 0.5528(4) 0.2198(3) 0.11486(11) 0.0754(11) Uani 1 1 d . . . O6 O 0.2320(4) 1.0487(2) 0.13346(9) 0.0511(9) Uani 1 1 d . . . F32 F 0.6116(4) 0.0822(2) 0.12435(10) 0.0708(10) Uani 1 1 d . . . F41 F 0.5707(4) 0.4652(2) 0.23491(9) 0.0702(10) Uani 1 1 d . . . F10 F 0.8065(4) -0.1642(2) 0.02485(12) 0.0894(14) Uani 1 1 d . . . C10 C 0.7840(5) -0.0827(3) 0.03698(12) 0.0387(11) Uani 1 1 d . . . C13 C 1.1709(5) 0.0096(3) 0.05218(10) 0.0296(9) Uani 1 1 d . . . C31 C 0.8117(5) 0.1875(3) 0.12920(12) 0.0369(11) Uani 1 1 d . . . C12 C 1.0775(5) -0.0647(3) 0.04390(11) 0.0329(10) Uani 1 1 d . . . H12 H 1.1083 -0.1252 0.0398 0.039 Uiso 1 1 calc R . . F5 F 0.0723(5) 1.0363(3) 0.19497(8) 0.0848(13) Uani 1 1 d . . . F30 F 0.6220(5) 0.1779(4) 0.16464(10) 0.1064(17) Uani 1 1 d . . . C32 C 0.9252(6) 0.2156(3) 0.15281(12) 0.0438(12) Uani 1 1 d . . . H32 H 0.9176 0.2244 0.1760 0.053 Uiso 1 1 calc R . . F42 F 0.3481(4) 0.4099(3) 0.22387(10) 0.0828(12) Uani 1 1 d . . . C20 C 0.6109(6) 0.2738(4) -0.00549(15) 0.0536(14) Uani 1 1 d . . . C14 C 1.3427(5) 0.0138(4) 0.05895(12) 0.0396(11) Uani 1 1 d . . . H14A H 1.3806 0.0676 0.0480 0.059 Uiso 1 1 calc R . . H14B H 1.3874 -0.0411 0.0502 0.059 Uiso 1 1 calc R . . H14C H 1.3718 0.0178 0.0832 0.059 Uiso 1 1 calc R . . C34 C 1.2092(6) 0.2588(3) 0.14993(13) 0.0444(12) Uani 1 1 d . . . H34A H 1.2680 0.2062 0.1592 0.067 Uiso 1 1 calc R . . H34B H 1.2011 0.3038 0.1677 0.067 Uiso 1 1 calc R . . H34C H 1.2612 0.2861 0.1320 0.067 Uiso 1 1 calc R . . F6 F 0.2670(6) 0.9508(3) 0.19866(9) 0.1008(16) Uani 1 1 d . . . C30 C 0.6499(6) 0.1656(4) 0.13352(14) 0.0508(14) Uani 1 1 d . . . F40 F 0.5387(5) 0.3406(2) 0.20704(10) 0.0857(12) Uani 1 1 d . . . N9 N 0.1382(5) 0.6629(3) 0.18304(13) 0.0542(12) Uani 1 1 d . . . C61 C 0.5272(6) 0.7954(4) 0.21606(13) 0.0490(13) Uani 1 1 d . . . C41 C 0.4619(5) 0.4726(3) 0.17902(13) 0.0402(11) Uani 1 1 d . . . N10 N 0.1363(5) 0.6942(3) 0.15075(12) 0.0471(11) Uani 1 1 d . . . C24 C 1.1722(5) 0.3619(3) 0.00618(14) 0.0443(12) Uani 1 1 d . . . H24A H 1.2485 0.3379 0.0235 0.066 Uiso 1 1 calc R . . H24B H 1.1647 0.4281 0.0086 0.066 Uiso 1 1 calc R . . H24C H 1.2030 0.3475 -0.0160 0.066 Uiso 1 1 calc R . . F20 F 0.5625(4) 0.3361(3) -0.02718(12) 0.1027(16) Uani 1 1 d . . . C62 C 0.5983(7) 0.8533(4) 0.19625(14) 0.0523(14) Uani 1 1 d . . . H62 H 0.6707 0.8994 0.2031 0.063 Uiso 1 1 calc R . . C23 C 1.0212(5) 0.3198(3) 0.00978(11) 0.0347(10) Uani 1 1 d . . . F4 F 0.0451(6) 0.8914(3) 0.18995(10) 0.1052(16) Uani 1 1 d . . . C63 C 0.5412(6) 0.8299(3) 0.16364(13) 0.0424(12) Uani 1 1 d . . . C999 C 0.1309(8) 0.9624(4) 0.18253(14) 0.0646(17) Uani 1 1 d . . . F21 F 0.5713(4) 0.1934(3) -0.01784(12) 0.0912(13) Uani 1 1 d . . . C53 C -0.0089(6) 0.7114(4) 0.13834(19) 0.0645(18) Uani 1 1 d . . . C42 C 0.5004(6) 0.4464(3) 0.14860(14) 0.0447(12) Uani 1 1 d . . . H42 H 0.5471 0.3907 0.1434 0.054 Uiso 1 1 calc R . . C50 C -0.0460(11) 0.6303(6) 0.2240(3) 0.117(4) Uani 1 1 d . . . C22 C 0.8824(6) 0.3360(3) -0.00927(12) 0.0404(11) Uani 1 1 d . . . H22 H 0.8636 0.3756 -0.0280 0.048 Uiso 1 1 calc R . . O4 O -0.0192(4) 0.9810(2) 0.12460(9) 0.0501(9) Uani 1 1 d . . . C43 C 0.4584(6) 0.5169(3) 0.12670(13) 0.0441(12) Uani 1 1 d . . . C54 C -0.0518(7) 0.7459(4) 0.1037(2) 0.078(2) Uani 1 1 d . . . H54A H -0.0396 0.8122 0.1034 0.117 Uiso 1 1 calc R . . H54B H -0.1586 0.7302 0.0966 0.117 Uiso 1 1 calc R . . H54C H 0.0145 0.7181 0.0884 0.117 Uiso 1 1 calc R . . C51 C -0.0098(8) 0.6607(4) 0.1898(2) 0.081(2) Uani 1 1 d . . . C40 C 0.4795(7) 0.4223(4) 0.21101(15) 0.0536(14) Uani 1 1 d . . . C44 C 0.4730(8) 0.5240(4) 0.08990(14) 0.0658(17) Uani 1 1 d . . . H44A H 0.3712 0.5311 0.0776 0.099 Uiso 1 1 calc R . . H44B H 0.5211 0.4687 0.0823 0.099 Uiso 1 1 calc R . . H44C H 0.5362 0.5769 0.0857 0.099 Uiso 1 1 calc R . . F60 F 0.4118(5) 0.7955(3) 0.26615(9) 0.0896(13) Uani 1 1 d . . . F62 F 0.6070(6) 0.7136(3) 0.26486(8) 0.1041(17) Uani 1 1 d . . . F61 F 0.6292(6) 0.8580(4) 0.26661(10) 0.1138(17) Uani 1 1 d . . . F52 F 0.0050(6) 0.5478(3) 0.23119(14) 0.1180(19) Uani 1 1 d . . . C64 C 0.5775(7) 0.8712(4) 0.13147(15) 0.0586(15) Uani 1 1 d . . . H64A H 0.5688 0.8247 0.1139 0.088 Uiso 1 1 calc R . . H64B H 0.6820 0.8953 0.1342 0.088 Uiso 1 1 calc R . . H64C H 0.5054 0.9207 0.1252 0.088 Uiso 1 1 calc R . . F50 F -0.2046(6) 0.6210(5) 0.2209(2) 0.171(3) Uani 1 1 d . . . F51 F -0.0032(10) 0.6827(4) 0.24748(17) 0.165(3) Uani 1 1 d . . . C60 C 0.5419(9) 0.7908(5) 0.25320(15) 0.0693(18) Uani 1 1 d . . . C52 C -0.1026(7) 0.6911(4) 0.1629(2) 0.092(3) Uani 1 1 d . . . H52 H -0.2107 0.6973 0.1613 0.110 Uiso 1 1 calc R . . O1 O 1.1311(9) 0.3995(5) 0.0862(2) 0.037(4) Uani 0.581(6) 1 d PD A 1 O1' O 1.1434(14) 0.3922(8) 0.0843(3) 0.062(7) Uani 0.419(6) 1 d PD A 2 O2 O 1.1034(11) 0.5642(5) 0.0874(2) 0.059(4) Uani 0.581(6) 1 d PD A 1 O2' O 1.1258(13) 0.5582(7) 0.0833(3) 0.057(5) Uani 0.419(6) 1 d PD A 2 S1 S 1.0262(4) 0.47553(19) 0.08365(9) 0.0544(9) Uani 0.581(6) 1 d PD A 1 S1' S 1.0831(5) 0.4735(2) 0.09850(11) 0.0376(10) Uani 0.419(6) 1 d PD A 2 F1 F 1.0227(9) 0.4689(6) 0.14834(16) 0.113(4) Uani 0.581(6) 1 d PD A 1 F1' F 0.8465(13) 0.4646(10) 0.0528(2) 0.099(5) Uani 0.419(6) 1 d PD A 2 C888 C 0.9250(9) 0.4685(5) 0.1212(2) 0.073(4) Uani 0.581(6) 1 d PD A 1 C88' C 0.8773(10) 0.4657(6) 0.0857(3) 0.058(4) Uani 0.419(6) 1 d PD A 2 O3 O 0.9069(11) 0.4733(8) 0.05598(19) 0.117(6) Uani 0.581(6) 1 d PD A 1 O3' O 1.0927(9) 0.4748(6) 0.13477(15) 0.049(2) Uani 0.419(6) 1 d PD A 2 F3 F 0.8468(10) 0.3921(5) 0.1203(3) 0.163(8) Uani 0.581(6) 1 d PD A 1 F3' F 0.8178(11) 0.3920(6) 0.0977(3) 0.087(5) Uani 0.419(6) 1 d PD A 2 F2 F 0.8301(7) 0.5380(4) 0.1230(2) 0.077(2) Uani 0.581(6) 1 d PD A 1 F2' F 0.8039(8) 0.5374(5) 0.0970(3) 0.076(3) Uani 0.419(6) 1 d PD A 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 Ge1 0.0207(2) 0.0316(2) 0.0337(2) -0.00137(19) 0.00066(18) -0.00113(18) Ge2 0.0211(2) 0.0339(3) 0.0368(3) -0.0007(2) -0.00096(18) -0.00161(19) Ge3 0.0440(3) 0.0385(3) 0.0381(3) 0.0093(2) 0.0007(2) 0.0076(2) Ge4 0.0700(4) 0.0435(3) 0.0478(3) 0.0181(3) 0.0260(3) 0.0146(3) S2 0.0496(7) 0.0320(6) 0.0315(6) 0.0036(5) 0.0049(5) 0.0116(5) N5 0.0235(18) 0.0261(18) 0.035(2) -0.0029(15) 0.0018(15) -0.0003(14) F11 0.0414(16) 0.066(2) 0.0439(16) 0.0129(14) 0.0101(13) -0.0129(14) N2 0.0224(18) 0.0302(19) 0.0282(18) -0.0003(15) -0.0003(14) -0.0009(15) N6 0.0238(18) 0.0277(18) 0.035(2) -0.0027(15) 0.0010(15) 0.0007(15) N11 0.054(3) 0.037(2) 0.034(2) 0.0085(18) 0.0090(19) 0.0105(19) N4 0.0211(18) 0.0301(19) 0.036(2) 0.0033(16) 0.0011(15) -0.0002(15) N1 0.0235(18) 0.0305(19) 0.0260(18) -0.0007(15) 0.0005(14) -0.0004(15) N8 0.042(2) 0.035(2) 0.040(2) 0.0060(18) 0.0023(18) 0.0081(18) F12 0.0467(17) 0.083(2) 0.0403(16) 0.0092(16) -0.0097(14) -0.0213(16) N7 0.039(2) 0.033(2) 0.045(2) 0.0092(18) 0.0044(18) 0.0064(17) F22 0.0348(17) 0.129(4) 0.089(3) 0.023(3) 0.0109(18) 0.022(2) C21 0.036(3) 0.035(2) 0.039(3) 0.005(2) -0.001(2) 0.005(2) N3 0.0237(18) 0.035(2) 0.037(2) 0.0026(16) -0.0013(15) 0.0003(15) O5 0.060(2) 0.0344(18) 0.050(2) 0.0026(15) 0.0069(17) 0.0173(16) N12 0.047(2) 0.033(2) 0.032(2) 0.0093(17) 0.0036(17) 0.0066(18) C33 0.042(3) 0.027(2) 0.035(2) -0.0036(19) -0.003(2) 0.0031(19) C11 0.033(2) 0.030(2) 0.026(2) -0.0031(18) 0.0048(18) -0.0014(18) F31 0.0382(18) 0.075(2) 0.115(3) -0.003(2) 0.0156(19) 0.0108(17) O6 0.063(2) 0.040(2) 0.050(2) -0.0039(16) 0.0058(18) 0.0024(17) F32 0.055(2) 0.060(2) 0.100(3) -0.012(2) 0.0219(19) -0.0234(17) F41 0.081(2) 0.062(2) 0.064(2) 0.0172(18) -0.0099(19) -0.0016(19) F10 0.060(2) 0.050(2) 0.164(4) -0.058(2) 0.037(2) -0.0192(17) C10 0.038(3) 0.040(3) 0.040(3) -0.006(2) 0.012(2) -0.005(2) C13 0.029(2) 0.037(2) 0.023(2) 0.0042(18) 0.0028(17) 0.0049(19) C31 0.040(3) 0.034(2) 0.038(3) -0.008(2) 0.008(2) -0.002(2) C12 0.037(2) 0.031(2) 0.032(2) -0.0007(19) 0.0095(19) 0.0046(19) F5 0.130(3) 0.082(3) 0.0443(19) -0.0016(18) 0.019(2) 0.048(2) F30 0.071(3) 0.194(5) 0.061(2) -0.041(3) 0.039(2) -0.040(3) C32 0.049(3) 0.048(3) 0.035(3) -0.011(2) 0.006(2) -0.003(2) F42 0.079(3) 0.078(3) 0.094(3) 0.041(2) 0.021(2) -0.010(2) C20 0.037(3) 0.065(4) 0.056(3) 0.017(3) -0.007(3) 0.007(3) C14 0.028(2) 0.055(3) 0.036(3) 0.004(2) 0.0039(19) 0.009(2) C34 0.046(3) 0.041(3) 0.043(3) -0.006(2) -0.011(2) -0.005(2) F6 0.125(4) 0.131(4) 0.0404(19) 0.001(2) -0.021(2) 0.061(3) C30 0.042(3) 0.063(4) 0.050(3) -0.016(3) 0.019(3) -0.008(3) F40 0.122(3) 0.043(2) 0.090(3) 0.0199(19) -0.002(2) 0.021(2) N9 0.049(3) 0.039(2) 0.079(3) 0.015(2) 0.028(2) 0.008(2) C61 0.057(3) 0.048(3) 0.041(3) 0.002(2) 0.002(2) 0.021(3) C41 0.032(2) 0.032(3) 0.055(3) 0.009(2) -0.001(2) 0.000(2) N10 0.040(2) 0.033(2) 0.068(3) 0.013(2) 0.008(2) 0.0072(18) C24 0.038(3) 0.037(3) 0.059(3) 0.008(2) 0.014(2) -0.002(2) F20 0.051(2) 0.132(4) 0.118(3) 0.078(3) -0.026(2) 0.005(2) C62 0.056(3) 0.042(3) 0.057(3) 0.003(3) -0.005(3) 0.004(3) C23 0.035(2) 0.030(2) 0.039(3) 0.001(2) 0.004(2) 0.0035(19) F4 0.167(5) 0.089(3) 0.068(3) 0.023(2) 0.050(3) -0.001(3) C63 0.045(3) 0.035(3) 0.046(3) 0.010(2) -0.001(2) 0.007(2) C999 0.097(5) 0.057(4) 0.041(3) 0.007(3) 0.012(3) 0.028(4) F21 0.050(2) 0.097(3) 0.120(3) -0.015(3) -0.023(2) -0.015(2) C53 0.040(3) 0.037(3) 0.116(5) 0.017(3) 0.004(3) 0.006(2) C42 0.042(3) 0.030(3) 0.060(3) -0.003(2) -0.002(2) 0.006(2) C50 0.095(6) 0.075(6) 0.199(12) 0.046(7) 0.107(7) 0.025(5) C22 0.044(3) 0.036(3) 0.040(3) 0.009(2) 0.001(2) 0.006(2) O4 0.048(2) 0.053(2) 0.050(2) 0.0007(17) 0.0025(17) 0.0153(17) C43 0.040(3) 0.036(3) 0.055(3) -0.002(2) -0.001(2) 0.003(2) C54 0.056(4) 0.037(3) 0.132(6) 0.016(4) -0.030(4) 0.007(3) C51 0.066(4) 0.052(4) 0.135(7) 0.025(4) 0.054(5) 0.014(3) C40 0.058(4) 0.034(3) 0.067(4) 0.016(3) 0.001(3) 0.002(3) C44 0.084(5) 0.063(4) 0.049(3) -0.007(3) 0.003(3) 0.017(3) F60 0.103(3) 0.123(4) 0.046(2) -0.003(2) 0.020(2) 0.046(3) F62 0.154(4) 0.122(4) 0.0364(18) 0.014(2) 0.013(2) 0.082(3) F61 0.138(4) 0.139(4) 0.058(2) -0.025(3) -0.019(3) -0.010(4) F52 0.129(4) 0.084(3) 0.156(5) 0.051(3) 0.082(4) 0.014(3) C64 0.057(3) 0.055(3) 0.064(4) 0.023(3) 0.003(3) -0.008(3) F50 0.103(4) 0.165(6) 0.269(8) 0.063(6) 0.122(5) 0.018(4) F51 0.282(10) 0.095(4) 0.143(5) 0.000(4) 0.142(6) 0.005(5) C60 0.090(5) 0.076(5) 0.040(3) -0.005(3) -0.001(3) 0.026(4) C52 0.040(3) 0.053(4) 0.184(9) 0.037(5) 0.022(5) 0.018(3) O1 0.038(6) 0.020(6) 0.054(8) -0.009(5) 0.006(6) 0.001(4) O1' 0.075(14) 0.041(11) 0.064(14) 0.012(9) -0.022(10) 0.010(9) O2 0.079(7) 0.033(7) 0.071(7) 0.015(5) 0.025(6) 0.001(5) O2' 0.064(9) 0.031(9) 0.070(10) -0.012(7) -0.015(7) -0.001(7) S1 0.065(2) 0.0379(14) 0.056(2) -0.0053(14) -0.0110(16) 0.0129(14) S1' 0.037(2) 0.0265(16) 0.047(2) 0.0021(16) -0.0033(16) -0.0039(14) F1 0.123(8) 0.147(8) 0.072(5) 0.022(5) 0.030(5) 0.068(7) F1' 0.078(9) 0.098(10) 0.112(11) -0.021(8) -0.027(7) 0.003(7) C888 0.056(7) 0.031(5) 0.139(13) 0.013(6) 0.038(8) 0.007(5) C88' 0.071(11) 0.044(8) 0.053(9) 0.002(7) -0.023(7) -0.028(7) O3 0.147(14) 0.080(9) 0.108(10) -0.036(7) -0.067(8) 0.064(9) O3' 0.049(6) 0.047(5) 0.050(6) -0.003(4) 0.007(4) 0.002(4) F3 0.095(9) 0.046(5) 0.37(2) 0.024(9) 0.125(12) 0.003(5) F3' 0.028(4) 0.032(5) 0.197(14) 0.003(6) -0.012(7) -0.009(4) F2 0.051(4) 0.042(4) 0.143(8) -0.009(5) 0.026(5) 0.001(3) F2' 0.040(5) 0.036(5) 0.147(10) -0.029(6) -0.005(6) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 N5 1.975(3) . ? Ge1 N3 1.998(4) . ? Ge1 N1 1.999(3) . ? Ge2 N6 1.984(3) . ? Ge2 N4 2.023(3) . ? Ge2 N2 2.054(3) . ? Ge3 N10 1.982(4) . ? Ge3 N12 2.028(4) . ? Ge3 N8 2.036(4) . ? Ge4 N7 1.989(4) . ? Ge4 N9 1.991(5) . ? Ge4 N11 2.005(4) . ? S2 O4 1.428(4) . ? S2 O6 1.432(4) . ? S2 O5 1.446(3) . ? S2 C999 1.825(6) . ? N5 C31 1.342(6) . ? N5 N6 1.368(5) . ? F11 C10 1.322(5) . ? N2 C13 1.334(5) . ? N2 N1 1.367(5) . ? N6 C33 1.343(6) . ? N11 C61 1.345(7) . ? N11 N12 1.363(5) . ? N4 C23 1.347(6) . ? N4 N3 1.368(5) . ? N1 C11 1.341(5) . ? N8 C43 1.341(6) . ? N8 N7 1.375(5) . ? F12 C10 1.339(6) . ? N7 C41 1.354(6) . ? F22 C20 1.335(7) . ? C21 N3 1.346(6) . ? C21 C22 1.372(7) . ? C21 C20 1.494(7) . ? N12 C63 1.342(6) . ? C33 C32 1.378(7) . ? C33 C34 1.492(6) . ? C11 C12 1.376(6) . ? C11 C10 1.486(6) . ? F31 C30 1.339(7) . ? F32 C30 1.313(6) . ? F41 C40 1.341(7) . ? F10 C10 1.315(6) . ? C13 C12 1.386(6) . ? C13 C14 1.507(6) . ? C31 C32 1.366(7) . ? C31 C30 1.486(7) . ? C12 H12 0.9500 . ? F5 C999 1.323(7) . ? F30 C30 1.311(6) . ? C32 H32 0.9500 . ? F42 C40 1.327(7) . ? C20 F20 1.304(6) . ? C20 F21 1.314(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? F6 C999 1.311(8) . ? F40 C40 1.325(6) . ? N9 C51 1.357(7) . ? N9 N10 1.374(6) . ? C61 C62 1.361(8) . ? C61 C60 1.484(8) . ? C41 C42 1.356(7) . ? C41 C40 1.476(7) . ? N10 C53 1.344(7) . ? C24 C23 1.485(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C62 C63 1.394(7) . ? C62 H62 0.9500 . ? C23 C22 1.390(7) . ? F4 C999 1.339(8) . ? C63 C64 1.492(7) . ? C53 C52 1.383(10) . ? C53 C54 1.490(10) . ? C42 C43 1.383(7) . ? C42 H42 0.9500 . ? C50 F51 1.245(14) . ? C50 F52 1.314(9) . ? C50 F50 1.394(11) . ? C50 C51 1.507(12) . ? C22 H22 0.9500 . ? C43 C44 1.500(8) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C51 C52 1.358(11) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? F60 C60 1.307(8) . ? F62 C60 1.334(7) . ? F61 C60 1.330(8) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C52 H52 0.9500 . ? O1 S1 1.445(7) . ? O1' S1' 1.448(7) . ? O2 S1 1.469(7) . ? O2' S1' 1.453(7) . ? S1 O3 1.445(7) . ? S1 C888 1.834(8) . ? S1' O3' 1.449(7) . ? S1' C88' 1.832(8) . ? F1 C888 1.313(8) . ? F1' C88' 1.317(8) . ? C888 F3 1.316(8) . ? C888 F2 1.325(7) . ? C88' F3' 1.316(8) . ? C88' F2' 1.341(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ge1 N3 90.62(15) . . ? N5 Ge1 N1 90.72(14) . . ? N3 Ge1 N1 88.92(14) . . ? N6 Ge2 N4 92.03(14) . . ? N6 Ge2 N2 88.21(14) . . ? N4 Ge2 N2 87.03(14) . . ? N10 Ge3 N12 91.14(18) . . ? N10 Ge3 N8 90.30(16) . . ? N12 Ge3 N8 85.55(15) . . ? N7 Ge4 N9 89.69(18) . . ? N7 Ge4 N11 89.33(16) . . ? N9 Ge4 N11 89.64(17) . . ? O4 S2 O6 115.2(2) . . ? O4 S2 O5 115.2(2) . . ? O6 S2 O5 114.0(2) . . ? O4 S2 C999 103.3(3) . . ? O6 S2 C999 104.0(3) . . ? O5 S2 C999 102.9(2) . . ? C31 N5 N6 106.9(3) . . ? C31 N5 Ge1 126.7(3) . . ? N6 N5 Ge1 126.0(3) . . ? C13 N2 N1 109.1(3) . . ? C13 N2 Ge2 125.8(3) . . ? N1 N2 Ge2 125.1(3) . . ? C33 N6 N5 109.0(3) . . ? C33 N6 Ge2 124.8(3) . . ? N5 N6 Ge2 126.1(3) . . ? C61 N11 N12 106.2(4) . . ? C61 N11 Ge4 127.8(3) . . ? N12 N11 Ge4 125.3(3) . . ? C23 N4 N3 109.1(3) . . ? C23 N4 Ge2 125.9(3) . . ? N3 N4 Ge2 125.0(3) . . ? C11 N1 N2 107.0(3) . . ? C11 N1 Ge1 127.5(3) . . ? N2 N1 Ge1 125.0(3) . . ? C43 N8 N7 108.9(4) . . ? C43 N8 Ge3 126.1(3) . . ? N7 N8 Ge3 125.0(3) . . ? C41 N7 N8 106.6(4) . . ? C41 N7 Ge4 127.5(3) . . ? N8 N7 Ge4 126.0(3) . . ? N3 C21 C22 110.8(4) . . ? N3 C21 C20 121.2(4) . . ? C22 C21 C20 128.0(4) . . ? C21 N3 N4 106.6(4) . . ? C21 N3 Ge1 127.4(3) . . ? N4 N3 Ge1 125.5(3) . . ? C63 N12 N11 109.2(4) . . ? C63 N12 Ge3 125.3(3) . . ? N11 N12 Ge3 125.3(3) . . ? N6 C33 C32 108.1(4) . . ? N6 C33 C34 122.9(4) . . ? C32 C33 C34 129.0(4) . . ? N1 C11 C12 110.0(4) . . ? N1 C11 C10 121.3(4) . . ? C12 C11 C10 128.7(4) . . ? F10 C10 F11 108.2(4) . . ? F10 C10 F12 107.0(4) . . ? F11 C10 F12 105.3(4) . . ? F10 C10 C11 110.8(4) . . ? F11 C10 C11 112.7(4) . . ? F12 C10 C11 112.6(4) . . ? N2 C13 C12 108.8(4) . . ? N2 C13 C14 121.9(4) . . ? C12 C13 C14 129.3(4) . . ? N5 C31 C32 109.8(4) . . ? N5 C31 C30 121.7(4) . . ? C32 C31 C30 128.5(4) . . ? C11 C12 C13 105.2(4) . . ? C11 C12 H12 127.4 . . ? C13 C12 H12 127.4 . . ? C31 C32 C33 106.3(4) . . ? C31 C32 H32 126.9 . . ? C33 C32 H32 126.9 . . ? F20 C20 F21 109.0(5) . . ? F20 C20 F22 106.5(5) . . ? F21 C20 F22 104.7(5) . . ? F20 C20 C21 111.6(5) . . ? F21 C20 C21 113.2(5) . . ? F22 C20 C21 111.4(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? F30 C30 F32 109.1(5) . . ? F30 C30 F31 106.2(5) . . ? F32 C30 F31 105.6(5) . . ? F30 C30 C31 111.0(5) . . ? F32 C30 C31 113.0(4) . . ? F31 C30 C31 111.5(5) . . ? C51 N9 N10 106.3(5) . . ? C51 N9 Ge4 127.6(5) . . ? N10 N9 Ge4 126.1(3) . . ? N11 C61 C62 111.4(5) . . ? N11 C61 C60 120.4(6) . . ? C62 C61 C60 128.2(6) . . ? N7 C41 C42 109.8(4) . . ? N7 C41 C40 121.3(5) . . ? C42 C41 C40 128.9(5) . . ? C53 N10 N9 109.2(5) . . ? C53 N10 Ge3 124.8(4) . . ? N9 N10 Ge3 125.8(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C61 C62 C63 104.6(5) . . ? C61 C62 H62 127.7 . . ? C63 C62 H62 127.7 . . ? N4 C23 C22 108.5(4) . . ? N4 C23 C24 123.3(4) . . ? C22 C23 C24 128.1(4) . . ? N12 C63 C62 108.6(4) . . ? N12 C63 C64 122.9(5) . . ? C62 C63 C64 128.6(5) . . ? F6 C999 F5 107.0(6) . . ? F6 C999 F4 107.2(5) . . ? F5 C999 F4 107.8(6) . . ? F6 C999 S2 112.0(5) . . ? F5 C999 S2 112.0(4) . . ? F4 C999 S2 110.6(5) . . ? N10 C53 C52 108.0(6) . . ? N10 C53 C54 123.2(6) . . ? C52 C53 C54 128.9(6) . . ? C41 C42 C43 106.5(4) . . ? C41 C42 H42 126.7 . . ? C43 C42 H42 126.7 . . ? F51 C50 F52 109.5(11) . . ? F51 C50 F50 110.3(8) . . ? F52 C50 F50 104.2(7) . . ? F51 C50 C51 115.5(7) . . ? F52 C50 C51 111.9(7) . . ? F50 C50 C51 104.7(9) . . ? C21 C22 C23 105.0(4) . . ? C21 C22 H22 127.5 . . ? C23 C22 H22 127.5 . . ? N8 C43 C42 108.2(5) . . ? N8 C43 C44 122.5(5) . . ? C42 C43 C44 129.3(5) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N9 C51 C52 109.9(6) . . ? N9 C51 C50 119.2(7) . . ? C52 C51 C50 130.8(7) . . ? F40 C40 F42 107.0(5) . . ? F40 C40 F41 107.5(5) . . ? F42 C40 F41 105.4(5) . . ? F40 C40 C41 110.8(5) . . ? F42 C40 C41 113.0(5) . . ? F41 C40 C41 112.8(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? F60 C60 F61 107.0(5) . . ? F60 C60 F62 105.5(6) . . ? F61 C60 F62 106.4(6) . . ? F60 C60 C61 114.2(6) . . ? F61 C60 C61 111.0(6) . . ? F62 C60 C61 112.3(5) . . ? C51 C52 C53 106.6(6) . . ? C51 C52 H52 126.7 . . ? C53 C52 H52 126.7 . . ? O1 S1 O3 116.3(5) . . ? O1 S1 O2 113.2(5) . . ? O3 S1 O2 112.9(6) . . ? O1 S1 C888 105.1(5) . . ? O3 S1 C888 104.8(5) . . ? O2 S1 C888 103.0(5) . . ? O1' S1' O3' 115.0(6) . . ? O1' S1' O2' 114.8(6) . . ? O3' S1' O2' 114.9(6) . . ? O1' S1' C88' 103.2(6) . . ? O3' S1' C88' 103.6(5) . . ? O2' S1' C88' 103.1(6) . . ? F1 C888 F3 108.8(7) . . ? F1 C888 F2 108.3(7) . . ? F3 C888 F2 109.3(7) . . ? F1 C888 S1 110.5(6) . . ? F3 C888 S1 108.8(7) . . ? F2 C888 S1 111.2(6) . . ? F3' C88' F1' 108.0(8) . . ? F3' C88' F2' 107.3(8) . . ? F1' C88' F2' 107.2(8) . . ? F3' C88' S1' 111.5(7) . . ? F1' C88' S1' 112.0(7) . . ? F2' C88' S1' 110.6(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ge1 N5 C31 142.7(4) . . . . ? N1 Ge1 N5 C31 -128.4(4) . . . . ? N3 Ge1 N5 N6 -44.8(3) . . . . ? N1 Ge1 N5 N6 44.2(3) . . . . ? N6 Ge2 N2 C13 -128.3(3) . . . . ? N4 Ge2 N2 C13 139.6(3) . . . . ? N6 Ge2 N2 N1 47.8(3) . . . . ? N4 Ge2 N2 N1 -44.3(3) . . . . ? C31 N5 N6 C33 0.5(5) . . . . ? Ge1 N5 N6 C33 -173.3(3) . . . . ? C31 N5 N6 Ge2 175.3(3) . . . . ? Ge1 N5 N6 Ge2 1.6(5) . . . . ? N4 Ge2 N6 C33 -145.2(3) . . . . ? N2 Ge2 N6 C33 127.9(3) . . . . ? N4 Ge2 N6 N5 40.7(3) . . . . ? N2 Ge2 N6 N5 -46.2(3) . . . . ? N7 Ge4 N11 C61 -129.9(4) . . . . ? N9 Ge4 N11 C61 140.4(4) . . . . ? N7 Ge4 N11 N12 38.5(4) . . . . ? N9 Ge4 N11 N12 -51.2(4) . . . . ? N6 Ge2 N4 C23 142.0(4) . . . . ? N2 Ge2 N4 C23 -129.9(4) . . . . ? N6 Ge2 N4 N3 -37.0(3) . . . . ? N2 Ge2 N4 N3 51.0(3) . . . . ? C13 N2 N1 C11 -0.4(4) . . . . ? Ge2 N2 N1 C11 -177.1(3) . . . . ? C13 N2 N1 Ge1 171.8(3) . . . . ? Ge2 N2 N1 Ge1 -4.8(4) . . . . ? N5 Ge1 N1 C11 129.3(4) . . . . ? N3 Ge1 N1 C11 -140.1(4) . . . . ? N5 Ge1 N1 N2 -41.3(3) . . . . ? N3 Ge1 N1 N2 49.3(3) . . . . ? N10 Ge3 N8 C43 137.6(4) . . . . ? N12 Ge3 N8 C43 -131.3(4) . . . . ? N10 Ge3 N8 N7 -43.7(4) . . . . ? N12 Ge3 N8 N7 47.5(4) . . . . ? C43 N8 N7 C41 -0.7(5) . . . . ? Ge3 N8 N7 C41 -179.6(3) . . . . ? C43 N8 N7 Ge4 179.5(3) . . . . ? Ge3 N8 N7 Ge4 0.6(5) . . . . ? N9 Ge4 N7 C41 -136.0(4) . . . . ? N11 Ge4 N7 C41 134.4(4) . . . . ? N9 Ge4 N7 N8 43.8(4) . . . . ? N11 Ge4 N7 N8 -45.9(4) . . . . ? C22 C21 N3 N4 0.0(5) . . . . ? C20 C21 N3 N4 -179.5(4) . . . . ? C22 C21 N3 Ge1 -172.7(3) . . . . ? C20 C21 N3 Ge1 7.9(7) . . . . ? C23 N4 N3 C21 0.2(5) . . . . ? Ge2 N4 N3 C21 179.4(3) . . . . ? C23 N4 N3 Ge1 173.1(3) . . . . ? Ge2 N4 N3 Ge1 -7.7(5) . . . . ? N5 Ge1 N3 C21 -141.0(4) . . . . ? N1 Ge1 N3 C21 128.3(4) . . . . ? N5 Ge1 N3 N4 47.7(3) . . . . ? N1 Ge1 N3 N4 -43.0(3) . . . . ? C61 N11 N12 C63 -0.5(5) . . . . ? Ge4 N11 N12 C63 -171.0(3) . . . . ? C61 N11 N12 Ge3 -176.0(3) . . . . ? Ge4 N11 N12 Ge3 13.5(5) . . . . ? N10 Ge3 N12 C63 -139.8(4) . . . . ? N8 Ge3 N12 C63 129.9(4) . . . . ? N10 Ge3 N12 N11 35.0(4) . . . . ? N8 Ge3 N12 N11 -55.2(4) . . . . ? N5 N6 C33 C32 -0.9(5) . . . . ? Ge2 N6 C33 C32 -175.9(3) . . . . ? N5 N6 C33 C34 179.8(4) . . . . ? Ge2 N6 C33 C34 4.8(6) . . . . ? N2 N1 C11 C12 -0.3(5) . . . . ? Ge1 N1 C11 C12 -172.3(3) . . . . ? N2 N1 C11 C10 177.5(4) . . . . ? Ge1 N1 C11 C10 5.5(6) . . . . ? N1 C11 C10 F10 168.4(4) . . . . ? C12 C11 C10 F10 -14.2(7) . . . . ? N1 C11 C10 F11 -70.2(6) . . . . ? C12 C11 C10 F11 107.2(5) . . . . ? N1 C11 C10 F12 48.6(6) . . . . ? C12 C11 C10 F12 -134.0(5) . . . . ? N1 N2 C13 C12 1.0(5) . . . . ? Ge2 N2 C13 C12 177.6(3) . . . . ? N1 N2 C13 C14 -176.1(4) . . . . ? Ge2 N2 C13 C14 0.5(6) . . . . ? N6 N5 C31 C32 0.2(5) . . . . ? Ge1 N5 C31 C32 173.9(3) . . . . ? N6 N5 C31 C30 178.4(4) . . . . ? Ge1 N5 C31 C30 -7.9(6) . . . . ? N1 C11 C12 C13 0.9(5) . . . . ? C10 C11 C12 C13 -176.7(4) . . . . ? N2 C13 C12 C11 -1.1(5) . . . . ? C14 C13 C12 C11 175.7(4) . . . . ? N5 C31 C32 C33 -0.8(6) . . . . ? C30 C31 C32 C33 -178.8(5) . . . . ? N6 C33 C32 C31 1.0(5) . . . . ? C34 C33 C32 C31 -179.7(5) . . . . ? N3 C21 C20 F20 168.7(5) . . . . ? C22 C21 C20 F20 -10.6(9) . . . . ? N3 C21 C20 F21 -67.9(7) . . . . ? C22 C21 C20 F21 112.8(6) . . . . ? N3 C21 C20 F22 49.7(7) . . . . ? C22 C21 C20 F22 -129.6(6) . . . . ? N5 C31 C30 F30 -176.8(5) . . . . ? C32 C31 C30 F30 1.1(8) . . . . ? N5 C31 C30 F32 60.2(7) . . . . ? C32 C31 C30 F32 -121.9(6) . . . . ? N5 C31 C30 F31 -58.6(6) . . . . ? C32 C31 C30 F31 119.3(6) . . . . ? N7 Ge4 N9 C51 133.1(5) . . . . ? N11 Ge4 N9 C51 -137.5(5) . . . . ? N7 Ge4 N9 N10 -47.8(4) . . . . ? N11 Ge4 N9 N10 41.5(4) . . . . ? N12 N11 C61 C62 0.2(6) . . . . ? Ge4 N11 C61 C62 170.3(4) . . . . ? N12 N11 C61 C60 179.0(5) . . . . ? Ge4 N11 C61 C60 -10.9(7) . . . . ? N8 N7 C41 C42 0.8(5) . . . . ? Ge4 N7 C41 C42 -179.5(3) . . . . ? N8 N7 C41 C40 -178.8(4) . . . . ? Ge4 N7 C41 C40 1.0(7) . . . . ? C51 N9 N10 C53 0.5(6) . . . . ? Ge4 N9 N10 C53 -178.7(4) . . . . ? C51 N9 N10 Ge3 -175.4(4) . . . . ? Ge4 N9 N10 Ge3 5.3(6) . . . . ? N12 Ge3 N10 C53 139.6(4) . . . . ? N8 Ge3 N10 C53 -134.9(5) . . . . ? N12 Ge3 N10 N9 -45.1(4) . . . . ? N8 Ge3 N10 N9 40.5(4) . . . . ? N11 C61 C62 C63 0.2(6) . . . . ? C60 C61 C62 C63 -178.5(5) . . . . ? N3 N4 C23 C22 -0.4(5) . . . . ? Ge2 N4 C23 C22 -179.5(3) . . . . ? N3 N4 C23 C24 178.3(4) . . . . ? Ge2 N4 C23 C24 -0.8(6) . . . . ? N11 N12 C63 C62 0.6(5) . . . . ? Ge3 N12 C63 C62 176.2(3) . . . . ? N11 N12 C63 C64 -179.3(5) . . . . ? Ge3 N12 C63 C64 -3.8(7) . . . . ? C61 C62 C63 N12 -0.5(6) . . . . ? C61 C62 C63 C64 179.4(5) . . . . ? O4 S2 C999 F6 178.8(5) . . . . ? O6 S2 C999 F6 -60.6(5) . . . . ? O5 S2 C999 F6 58.6(5) . . . . ? O4 S2 C999 F5 -61.0(6) . . . . ? O6 S2 C999 F5 59.7(6) . . . . ? O5 S2 C999 F5 178.8(5) . . . . ? O4 S2 C999 F4 59.3(5) . . . . ? O6 S2 C999 F4 179.9(4) . . . . ? O5 S2 C999 F4 -61.0(5) . . . . ? N9 N10 C53 C52 0.1(7) . . . . ? Ge3 N10 C53 C52 176.2(4) . . . . ? N9 N10 C53 C54 -179.7(5) . . . . ? Ge3 N10 C53 C54 -3.6(8) . . . . ? N7 C41 C42 C43 -0.6(6) . . . . ? C40 C41 C42 C43 179.0(5) . . . . ? N3 C21 C22 C23 -0.2(6) . . . . ? C20 C21 C22 C23 179.2(5) . . . . ? N4 C23 C22 C21 0.3(5) . . . . ? C24 C23 C22 C21 -178.3(5) . . . . ? N7 N8 C43 C42 0.4(5) . . . . ? Ge3 N8 C43 C42 179.2(3) . . . . ? N7 N8 C43 C44 179.9(5) . . . . ? Ge3 N8 C43 C44 -1.2(7) . . . . ? C41 C42 C43 N8 0.1(6) . . . . ? C41 C42 C43 C44 -179.4(6) . . . . ? N10 N9 C51 C52 -1.0(8) . . . . ? Ge4 N9 C51 C52 178.2(5) . . . . ? N10 N9 C51 C50 -179.0(7) . . . . ? Ge4 N9 C51 C50 0.3(10) . . . . ? F51 C50 C51 N9 68.2(10) . . . . ? F52 C50 C51 N9 -58.0(12) . . . . ? F50 C50 C51 N9 -170.3(7) . . . . ? F51 C50 C51 C52 -109.3(12) . . . . ? F52 C50 C51 C52 124.5(9) . . . . ? F50 C50 C51 C52 12.3(13) . . . . ? N7 C41 C40 F40 177.9(5) . . . . ? C42 C41 C40 F40 -1.6(8) . . . . ? N7 C41 C40 F42 57.8(7) . . . . ? C42 C41 C40 F42 -121.6(6) . . . . ? N7 C41 C40 F41 -61.6(7) . . . . ? C42 C41 C40 F41 118.9(6) . . . . ? N11 C61 C60 F60 -52.7(8) . . . . ? C62 C61 C60 F60 126.0(7) . . . . ? N11 C61 C60 F61 -173.7(5) . . . . ? C62 C61 C60 F61 4.9(9) . . . . ? N11 C61 C60 F62 67.4(8) . . . . ? C62 C61 C60 F62 -114.0(7) . . . . ? N9 C51 C52 C53 1.1(9) . . . . ? C50 C51 C52 C53 178.7(9) . . . . ? N10 C53 C52 C51 -0.7(8) . . . . ? C54 C53 C52 C51 179.0(7) . . . . ? O1 S1 C888 F1 56.3(7) . . . . ? O3 S1 C888 F1 179.3(6) . . . . ? O2 S1 C888 F1 -62.5(7) . . . . ? O1 S1 C888 F3 -63.0(7) . . . . ? O3 S1 C888 F3 60.0(7) . . . . ? O2 S1 C888 F3 178.2(7) . . . . ? O1 S1 C888 F2 176.5(6) . . . . ? O3 S1 C888 F2 -60.4(8) . . . . ? O2 S1 C888 F2 57.8(8) . . . . ? O1' S1' C88' F3' 60.8(9) . . . . ? O3' S1' C88' F3' -59.4(8) . . . . ? O2' S1' C88' F3' -179.5(8) . . . . ? O1' S1' C88' F1' -60.4(9) . . . . ? O3' S1' C88' F1' 179.4(7) . . . . ? O2' S1' C88' F1' 59.4(9) . . . . ? O1' S1' C88' F2' -179.8(8) . . . . ? O3' S1' C88' F2' 59.9(8) . . . . ? O2' S1' C88' F2' -60.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.75 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.669 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.078