# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1848 data_los21 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,1-Bis(N,N-dimethylaminoxy)-2,3,4,5-tetraphenyl-1-sila-cyclopentene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H35 N2 O2 Si' _chemical_formula_weight 543.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 12.547(2) _cell_length_b 9.905(2) _cell_length_c 24.461(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.91(1) _cell_angle_gamma 90.00 _cell_volume 3017.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 11 _cell_measurement_theta_max 18 _exptl_crystal_description Cylinder _exptl_crystal_colour Colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 'CAD 4 - four circle diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% None _diffrn_reflns_number 8841 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.08 _reflns_number_total 6592 _reflns_number_gt 3847 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+1.0675P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6592 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Si1 Si 0.98175(5) 0.29252(7) 0.12201(2) 0.02381(15) Uani 1 1 d . . . O1 O 0.88574(12) 0.37072(17) 0.08213(6) 0.0315(4) Uani 1 1 d . . . N1 N 0.86462(15) 0.2827(2) 0.03329(8) 0.0322(5) Uani 1 1 d . . . C1 C 0.7523(2) 0.2443(3) 0.03102(12) 0.0479(8) Uani 1 1 d . . . H1A H 0.7320(5) 0.1886(16) -0.0018(6) 0.047(8) Uiso 1 1 calc R . . H1B H 0.7075(8) 0.3259(13) 0.0291(7) 0.055(9) Uiso 1 1 calc R . . H1C H 0.7416(4) 0.1926(16) 0.0642(6) 0.045(8) Uiso 1 1 calc R . . C2 C 0.8819(3) 0.3672(3) -0.01312(10) 0.0491(7) Uani 1 1 d . . . H2A H 0.8628(13) 0.3162(10) -0.0478(6) 0.061(9) Uiso 1 1 calc R . . H2B H 0.9585(12) 0.3942(15) -0.0101(4) 0.054(9) Uiso 1 1 calc R . . H2C H 0.8363(12) 0.4489(16) -0.0132(4) 0.054(9) Uiso 1 1 calc R . . O2 O 1.08582(12) 0.28352(17) 0.08660(6) 0.0282(4) Uani 1 1 d . . . N2 N 1.17920(15) 0.2488(2) 0.12707(8) 0.0321(5) Uani 1 1 d . . . C3 C 1.2552(2) 0.3576(3) 0.12303(12) 0.0452(7) Uani 1 1 d . . . H3A H 1.2244(7) 0.4414(14) 0.1335(7) 0.047(8) Uiso 1 1 calc R . . H3B H 1.2717(11) 0.3642(11) 0.0857(6) 0.044(8) Uiso 1 1 calc R . . H3C H 1.3200(11) 0.3396(9) 0.1472(6) 0.066(10) Uiso 1 1 calc R . . C4 C 1.2201(2) 0.1217(3) 0.10849(12) 0.0469(7) Uani 1 1 d . . . H4A H 1.2858(13) 0.0973(10) 0.1321(6) 0.069(10) Uiso 1 1 calc R . . H4B H 1.2359(13) 0.1313(6) 0.0704(7) 0.048(8) Uiso 1 1 calc R . . H4C H 1.1662(11) 0.0510(13) 0.1103(7) 0.072(11) Uiso 1 1 calc R . . C10 C 0.93610(17) 0.1353(2) 0.15366(9) 0.0266(5) Uani 1 1 d . . . C11 C 0.89279(18) 0.0142(2) 0.12303(9) 0.0271(5) Uani 1 1 d . . . C12 C 0.9334(2) -0.0216(3) 0.07428(9) 0.0307(5) Uani 1 1 d . . . H12A H 0.9877(14) 0.0321(14) 0.0616(3) 0.026(6) Uiso 1 1 calc R . . C13 C 0.8962(2) -0.1339(3) 0.04408(10) 0.0349(6) Uani 1 1 d . . . H13A H 0.9267(9) -0.1575(7) 0.0111(9) 0.035(7) Uiso 1 1 calc R . . C14 C 0.8155(2) -0.2120(3) 0.06113(10) 0.0366(6) Uani 1 1 d . . . H14A H 0.7897(8) -0.292(2) 0.0403(7) 0.048(8) Uiso 1 1 calc R . . C15 C 0.7717(2) -0.1761(3) 0.10808(11) 0.0391(6) Uani 1 1 d . . . H15A H 0.7155(18) -0.2275(16) 0.1194(4) 0.043(8) Uiso 1 1 calc R . . C16 C 0.8096(2) -0.0651(3) 0.13868(10) 0.0341(6) Uani 1 1 d . . . H16A H 0.7796(8) -0.0431(7) 0.1699(9) 0.027(6) Uiso 1 1 calc R . . C20 C 0.93926(17) 0.1603(2) 0.20861(9) 0.0256(5) Uani 1 1 d . . . C21 C 0.90221(18) 0.0647(2) 0.24916(9) 0.0269(5) Uani 1 1 d . . . C22 C 0.9517(2) -0.0604(3) 0.25798(10) 0.0349(6) Uani 1 1 d . . . H22A H 1.0108(18) -0.0817(7) 0.2401(5) 0.040(7) Uiso 1 1 calc R . . C23 C 0.9136(3) -0.1530(3) 0.29304(11) 0.0452(7) Uani 1 1 d . . . H23A H 0.9483(12) -0.240(3) 0.2986(2) 0.055(9) Uiso 1 1 calc R . . C24 C 0.8268(2) -0.1226(3) 0.32008(11) 0.0467(7) Uani 1 1 d . . . H24A H 0.8006(9) -0.186(2) 0.3433(8) 0.055(9) Uiso 1 1 calc R . . C25 C 0.7784(2) 0.0021(3) 0.31288(10) 0.0410(7) Uani 1 1 d . . . H25A H 0.717(2) 0.0246(8) 0.3327(6) 0.052(8) Uiso 1 1 calc R . . C26 C 0.81601(19) 0.0961(3) 0.27781(9) 0.0319(6) Uani 1 1 d . . . H26A H 0.7823(10) 0.184(2) 0.27323(16) 0.033(7) Uiso 1 1 calc R . . C30 C 0.98129(17) 0.2976(2) 0.22825(9) 0.0248(5) Uani 1 1 d . . . C31 C 0.99658(17) 0.3297(2) 0.28805(9) 0.0262(5) Uani 1 1 d . . . C32 C 1.06177(19) 0.2502(3) 0.32523(10) 0.0328(6) Uani 1 1 d . . . H32A H 1.0930(9) 0.167(2) 0.3126(4) 0.035(7) Uiso 1 1 calc R . . C33 C 1.0827(2) 0.2881(3) 0.38018(10) 0.0422(7) Uani 1 1 d . . . H33A H 1.1316(15) 0.2299(18) 0.4070(8) 0.055(8) Uiso 1 1 calc R . . C34 C 1.0378(2) 0.4038(3) 0.39859(11) 0.0443(7) Uani 1 1 d . . . H34A H 1.0533(5) 0.4310(8) 0.4378(11) 0.043(7) Uiso 1 1 calc R . . C35 C 0.9712(2) 0.4817(3) 0.36237(10) 0.0400(6) Uani 1 1 d . . . H35A H 0.9393(10) 0.560(2) 0.3751(4) 0.045(8) Uiso 1 1 calc R . . C36 C 0.9510(2) 0.4458(3) 0.30737(10) 0.0316(5) Uani 1 1 d . . . H36A H 0.9047(14) 0.5021(17) 0.2821(7) 0.044(8) Uiso 1 1 calc R . . C40 C 1.00701(17) 0.3832(2) 0.18856(9) 0.0237(5) Uani 1 1 d . . . C41 C 1.05897(17) 0.5166(2) 0.19542(9) 0.0242(5) Uani 1 1 d . . . C42 C 1.14064(18) 0.5464(3) 0.23798(10) 0.0315(5) Uani 1 1 d . . . H42A H 1.1585(5) 0.4837(18) 0.2656(8) 0.030(7) Uiso 1 1 calc R . . C43 C 1.1950(2) 0.6680(3) 0.23940(11) 0.0371(6) Uani 1 1 d . . . H43A H 1.2523(18) 0.6862(6) 0.2687(9) 0.050(8) Uiso 1 1 calc R . . C44 C 1.1675(2) 0.7635(3) 0.19893(11) 0.0382(6) Uani 1 1 d . . . H44A H 1.2047(12) 0.848(3) 0.19999(11) 0.047(8) Uiso 1 1 calc R . . C45 C 1.0864(2) 0.7369(3) 0.15706(11) 0.0356(6) Uani 1 1 d . . . H45A H 1.0665(6) 0.804(2) 0.1289(9) 0.048(8) Uiso 1 1 calc R . . C46 C 1.03347(16) 0.6142(2) 0.15508(9) 0.0291(5) Uani 1 1 d . . . H46A H 0.97803(15) 0.5961(2) 0.12528(10) 0.045(8) Uiso 1 1 calc R . . C1A C 0.95691(16) 0.0474(3) 0.45006(12) 0.0744(12) Uani 1 1 d R . . H1AA H 0.92721(16) 0.0808(3) 0.41511(11) 0.105(14) Uiso 1 1 calc R . . C2A C 1.0047(3) -0.0764(5) 0.45388(17) 0.0713(11) Uani 1 1 d . . . H2AA H 1.0077(3) -0.131(2) 0.4210(13) 0.076(12) Uiso 1 1 calc R . . C3A C 0.9515(3) 0.1229(5) 0.49566(19) 0.0771(12) Uani 1 1 d . . . H3AA H 0.9167(16) 0.210(4) 0.4927(2) 0.092(13) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0233(3) 0.0280(3) 0.0198(3) -0.0007(3) 0.0013(2) 0.0007(3) O1 0.0293(9) 0.0405(10) 0.0232(8) -0.0047(7) -0.0036(7) 0.0060(8) N1 0.0323(10) 0.0385(12) 0.0245(10) -0.0046(9) -0.0014(8) 0.0006(10) C1 0.0333(14) 0.067(2) 0.0406(16) -0.0046(15) -0.0069(12) -0.0050(14) C2 0.0603(19) 0.0590(19) 0.0274(14) 0.0034(14) 0.0023(13) 0.0008(17) O2 0.0242(8) 0.0387(9) 0.0211(7) 0.0028(7) 0.0001(6) 0.0029(7) N2 0.0241(10) 0.0440(13) 0.0266(10) 0.0022(9) -0.0035(8) 0.0051(9) C3 0.0257(13) 0.063(2) 0.0468(16) -0.0007(15) 0.0041(12) -0.0057(14) C4 0.0417(16) 0.0565(19) 0.0415(16) -0.0004(14) 0.0000(13) 0.0194(15) C10 0.0240(11) 0.0307(13) 0.0255(11) -0.0009(10) 0.0051(9) -0.0009(10) C11 0.0291(12) 0.0262(12) 0.0253(11) -0.0004(10) 0.0006(9) -0.0010(10) C12 0.0331(13) 0.0331(13) 0.0263(12) 0.0008(11) 0.0046(10) -0.0005(11) C13 0.0428(15) 0.0364(14) 0.0250(12) -0.0054(11) 0.0016(11) 0.0038(12) C14 0.0437(14) 0.0319(13) 0.0320(13) -0.0060(12) -0.0043(11) -0.0032(13) C15 0.0383(14) 0.0392(15) 0.0389(14) -0.0018(12) 0.0014(12) -0.0114(12) C16 0.0355(13) 0.0383(14) 0.0289(12) -0.0048(11) 0.0056(11) -0.0035(12) C20 0.0219(11) 0.0293(12) 0.0261(11) -0.0004(10) 0.0045(9) 0.0004(9) C21 0.0298(12) 0.0298(12) 0.0205(11) -0.0029(10) 0.0011(9) -0.0055(10) C22 0.0386(14) 0.0344(14) 0.0317(13) 0.0001(11) 0.0041(11) 0.0015(11) C23 0.0636(19) 0.0330(15) 0.0368(15) 0.0043(12) -0.0031(14) -0.0084(14) C24 0.0598(19) 0.0487(18) 0.0313(14) 0.0085(13) 0.0045(13) -0.0234(15) C25 0.0399(15) 0.0546(18) 0.0293(13) -0.0047(13) 0.0070(12) -0.0150(14) C26 0.0311(13) 0.0376(15) 0.0270(12) -0.0047(11) 0.0041(10) -0.0055(11) C30 0.0223(10) 0.0282(11) 0.0233(10) -0.0022(10) -0.0001(8) 0.0029(10) C31 0.0246(11) 0.0314(13) 0.0232(11) -0.0013(10) 0.0051(9) -0.0059(10) C32 0.0313(12) 0.0373(14) 0.0290(12) 0.0032(11) 0.0004(10) -0.0052(11) C33 0.0433(15) 0.0529(17) 0.0279(13) 0.0054(14) -0.0061(11) -0.0101(14) C34 0.0536(17) 0.0584(19) 0.0204(12) -0.0056(13) 0.0026(12) -0.0170(15) C35 0.0433(15) 0.0444(16) 0.0341(14) -0.0112(13) 0.0114(12) -0.0091(13) C36 0.0316(12) 0.0368(14) 0.0267(12) -0.0035(11) 0.0043(10) -0.0037(11) C40 0.0209(10) 0.0280(12) 0.0219(11) -0.0004(9) 0.0013(8) 0.0024(9) C41 0.0237(11) 0.0280(12) 0.0211(11) -0.0013(9) 0.0040(9) 0.0012(9) C42 0.0283(12) 0.0381(14) 0.0268(12) 0.0040(12) -0.0024(10) -0.0029(11) C43 0.0295(13) 0.0484(16) 0.0331(13) -0.0058(12) 0.0018(11) -0.0092(12) C44 0.0378(14) 0.0357(15) 0.0423(15) -0.0045(12) 0.0098(12) -0.0109(12) C45 0.0410(14) 0.0301(14) 0.0354(13) 0.0038(12) 0.0028(11) -0.0002(11) C46 0.0286(12) 0.0307(13) 0.0272(12) 0.0019(10) -0.0005(10) 0.0002(10) C1A 0.055(2) 0.102(3) 0.062(2) 0.040(2) -0.0107(18) -0.019(2) C2A 0.0385(18) 0.109(3) 0.067(2) -0.005(2) 0.0079(16) -0.013(2) C3A 0.0357(17) 0.076(3) 0.114(3) 0.016(3) -0.014(2) -0.0028(18) _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 Si1 O1 1.6493(16) . ? Si1 O2 1.6538(16) . ? Si1 C40 1.853(2) . ? Si1 C10 1.860(2) . ? O1 N1 1.477(2) . ? N1 C2 1.447(3) . ? N1 C1 1.454(3) . ? C1 H1A 0.9822 . ? C1 H1B 0.9822 . ? C1 H1C 0.9822 . ? C2 H2A 0.9918 . ? C2 H2B 0.9918 . ? C2 H2C 0.9918 . ? O2 N2 1.480(2) . ? N2 C3 1.451(3) . ? N2 C4 1.452(3) . ? C3 H3A 0.9628 . ? C3 H3B 0.9628 . ? C3 H3C 0.9628 . ? C4 H4A 0.9790 . ? C4 H4B 0.9790 . ? C4 H4C 0.9790 . ? C10 C20 1.363(3) . ? C10 C11 1.482(3) . ? C11 C16 1.396(3) . ? C11 C12 1.398(3) . ? C12 C13 1.385(3) . ? C12 H12A 0.9445 . ? C13 C14 1.378(4) . ? C13 H13A 0.9624 . ? C14 C15 1.378(4) . ? C14 H14A 0.9722 . ? C15 C16 1.382(3) . ? C15 H15A 0.9381 . ? C16 H16A 0.9188 . ? C20 C21 1.486(3) . ? C20 C30 1.516(3) . ? C21 C22 1.391(4) . ? C21 C26 1.393(3) . ? C22 C23 1.380(4) . ? C22 H22A 0.9286 . ? C23 C24 1.374(4) . ? C23 H23A 0.9656 . ? C24 C25 1.379(4) . ? C24 H24A 0.9359 . ? C25 C26 1.387(4) . ? C25 H25A 0.9865 . ? C26 H26A 0.9672 . ? C30 C40 1.357(3) . ? C30 C31 1.487(3) . ? C31 C36 1.392(3) . ? C31 C32 1.392(3) . ? C32 C33 1.390(3) . ? C32 H32A 0.9764 . ? C33 C34 1.376(4) . ? C33 H33A 1.0216 . ? C34 C35 1.379(4) . ? C34 H34A 0.9922 . ? C35 C36 1.385(3) . ? C35 H35A 0.9391 . ? C36 H36A 0.9720 . ? C40 C41 1.473(3) . ? C41 C46 1.391(3) . ? C41 C42 1.402(3) . ? C42 C43 1.382(4) . ? C42 H42A 0.9247 . ? C43 C44 1.383(4) . ? C43 H43A 0.9692 . ? C44 C45 1.379(4) . ? C44 H44A 0.9608 . ? C45 C46 1.383(3) . ? C45 H45A 0.9702 . ? C46 H46A 0.9619 . ? C1A C3A 1.352(5) . ? C1A C2A 1.363(5) . ? C1A H1AA 0.9500 . ? C2A C3A 1.369(5) 3_756 ? C2A H2AA 0.9763 . ? C3A C2A 1.369(5) 3_756 ? C3A H3AA 0.9621 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si1 O2 106.39(8) . . ? O1 Si1 C40 109.11(9) . . ? O2 Si1 C40 115.08(9) . . ? O1 Si1 C10 113.57(10) . . ? O2 Si1 C10 118.36(10) . . ? C40 Si1 C10 93.95(10) . . ? N1 O1 Si1 104.38(13) . . ? C2 N1 C1 110.9(2) . . ? C2 N1 O1 105.31(19) . . ? C1 N1 O1 105.30(18) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 O2 Si1 105.88(12) . . ? C3 N2 C4 111.3(2) . . ? C3 N2 O2 104.81(18) . . ? C4 N2 O2 105.85(18) . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C20 C10 C11 127.7(2) . . ? C20 C10 Si1 106.55(17) . . ? C11 C10 Si1 125.41(16) . . ? C16 C11 C12 116.9(2) . . ? C16 C11 C10 123.9(2) . . ? C12 C11 C10 119.2(2) . . ? C13 C12 C11 121.6(2) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C14 C13 C12 120.2(2) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C15 C14 C13 119.2(2) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C15 C16 C11 121.3(2) . . ? C15 C16 H16A 119.3 . . ? C11 C16 H16A 119.3 . . ? C10 C20 C21 124.6(2) . . ? C10 C20 C30 116.3(2) . . ? C21 C20 C30 119.03(19) . . ? C22 C21 C26 118.7(2) . . ? C22 C21 C20 120.1(2) . . ? C26 C21 C20 121.2(2) . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 120.2(3) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C40 C30 C31 123.8(2) . . ? C40 C30 C20 115.96(19) . . ? C31 C30 C20 120.17(19) . . ? C36 C31 C32 118.6(2) . . ? C36 C31 C30 120.1(2) . . ? C32 C31 C30 121.2(2) . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C34 C33 C32 120.3(3) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 119.7(2) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C34 C35 C36 120.4(3) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 C31 120.5(2) . . ? C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? C30 C40 C41 128.2(2) . . ? C30 C40 Si1 107.18(16) . . ? C41 C40 Si1 124.15(16) . . ? C46 C41 C42 117.7(2) . . ? C46 C41 C40 118.79(19) . . ? C42 C41 C40 123.2(2) . . ? C43 C42 C41 121.1(2) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 119.9(2) . . ? C42 C43 H43A 120.1 . . ? C44 C43 H43A 120.1 . . ? C45 C44 C43 119.9(3) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 C45 C46 120.2(2) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 121.2(2) . . ? C45 C46 H46A 119.4 . . ? C41 C46 H46A 119.4 . . ? C3A C1A C2A 120.4(3) . . ? C3A C1A H1AA 119.8 . . ? C2A C1A H1AA 119.8 . . ? C1A C2A C3A 119.4(4) . 3_756 ? C1A C2A H2AA 120.3 . . ? C3A C2A H2AA 120.3 3_756 . ? C1A C3A C2A 120.2(4) . 3_756 ? C1A C3A H3AA 119.9 . . ? C2A C3A H3AA 119.9 3_756 . ? 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 O2 Si1 O1 N1 61.08(14) . . . . ? C40 Si1 O1 N1 -174.21(13) . . . . ? C10 Si1 O1 N1 -70.87(15) . . . . ? Si1 O1 N1 C2 -122.49(18) . . . . ? Si1 O1 N1 C1 120.18(18) . . . . ? O1 Si1 O2 N2 164.78(12) . . . . ? C40 Si1 O2 N2 43.82(16) . . . . ? C10 Si1 O2 N2 -65.99(16) . . . . ? Si1 O2 N2 C3 -121.99(17) . . . . ? Si1 O2 N2 C4 120.31(18) . . . . ? O1 Si1 C10 C20 -111.13(16) . . . . ? O2 Si1 C10 C20 123.04(15) . . . . ? C40 Si1 C10 C20 1.71(17) . . . . ? O1 Si1 C10 C11 62.2(2) . . . . ? O2 Si1 C10 C11 -63.6(2) . . . . ? C40 Si1 C10 C11 175.1(2) . . . . ? C20 C10 C11 C16 29.0(4) . . . . ? Si1 C10 C11 C16 -143.0(2) . . . . ? C20 C10 C11 C12 -153.6(2) . . . . ? Si1 C10 C11 C12 34.4(3) . . . . ? C16 C11 C12 C13 -2.6(3) . . . . ? C10 C11 C12 C13 179.8(2) . . . . ? C11 C12 C13 C14 1.4(4) . . . . ? C12 C13 C14 C15 0.7(4) . . . . ? C13 C14 C15 C16 -1.6(4) . . . . ? C14 C15 C16 C11 0.3(4) . . . . ? C12 C11 C16 C15 1.8(4) . . . . ? C10 C11 C16 C15 179.2(2) . . . . ? C11 C10 C20 C21 2.5(4) . . . . ? Si1 C10 C20 C21 175.69(18) . . . . ? C11 C10 C20 C30 -175.8(2) . . . . ? Si1 C10 C20 C30 -2.7(2) . . . . ? C10 C20 C21 C22 62.0(3) . . . . ? C30 C20 C21 C22 -119.7(2) . . . . ? C10 C20 C21 C26 -116.2(3) . . . . ? C30 C20 C21 C26 62.1(3) . . . . ? C26 C21 C22 C23 2.2(3) . . . . ? C20 C21 C22 C23 -176.0(2) . . . . ? C21 C22 C23 C24 -0.5(4) . . . . ? C22 C23 C24 C25 -1.1(4) . . . . ? C23 C24 C25 C26 1.0(4) . . . . ? C24 C25 C26 C21 0.7(4) . . . . ? C22 C21 C26 C25 -2.3(3) . . . . ? C20 C21 C26 C25 175.9(2) . . . . ? C10 C20 C30 C40 2.7(3) . . . . ? C21 C20 C30 C40 -175.7(2) . . . . ? C10 C20 C30 C31 -174.7(2) . . . . ? C21 C20 C30 C31 6.8(3) . . . . ? C40 C30 C31 C36 55.3(3) . . . . ? C20 C30 C31 C36 -127.5(2) . . . . ? C40 C30 C31 C32 -120.6(3) . . . . ? C20 C30 C31 C32 56.6(3) . . . . ? C36 C31 C32 C33 -1.5(3) . . . . ? C30 C31 C32 C33 174.4(2) . . . . ? C31 C32 C33 C34 1.0(4) . . . . ? C32 C33 C34 C35 0.5(4) . . . . ? C33 C34 C35 C36 -1.4(4) . . . . ? C34 C35 C36 C31 0.8(4) . . . . ? C32 C31 C36 C35 0.6(3) . . . . ? C30 C31 C36 C35 -175.3(2) . . . . ? C31 C30 C40 C41 3.8(4) . . . . ? C20 C30 C40 C41 -173.5(2) . . . . ? C31 C30 C40 Si1 176.19(17) . . . . ? C20 C30 C40 Si1 -1.1(2) . . . . ? O1 Si1 C40 C30 116.32(16) . . . . ? O2 Si1 C40 C30 -124.21(15) . . . . ? C10 Si1 C40 C30 -0.30(17) . . . . ? O1 Si1 C40 C41 -70.92(19) . . . . ? O2 Si1 C40 C41 48.5(2) . . . . ? C10 Si1 C40 C41 172.46(18) . . . . ? C30 C40 C41 C46 -148.9(2) . . . . ? Si1 C40 C41 C46 39.9(3) . . . . ? C30 C40 C41 C42 37.3(4) . . . . ? Si1 C40 C41 C42 -133.9(2) . . . . ? C46 C41 C42 C43 -0.9(3) . . . . ? C40 C41 C42 C43 172.9(2) . . . . ? C41 C42 C43 C44 1.3(4) . . . . ? C42 C43 C44 C45 -0.5(4) . . . . ? C43 C44 C45 C46 -0.8(4) . . . . ? C44 C45 C46 C41 1.2(4) . . . . ? C42 C41 C46 C45 -0.4(3) . . . . ? C40 C41 C46 C45 -174.5(2) . . . . ? C3A C1A C2A C3A -0.8(5) . . . 3_756 ? C2A C1A C3A C2A 0.8(5) . . . 3_756 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.346 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.053 #===END data_los25 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,1-Bis(N,N-dimethylaminoxy)-2,3,4,5-tetraphenyl-1-germacyclopentadien ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Ge N2 O2' _chemical_formula_weight 549.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.399(4) _cell_length_b 12.453(3) _cell_length_c 19.955(3) _cell_angle_alpha 81.16(2) _cell_angle_beta 84.37(2) _cell_angle_gamma 66.05(2) _cell_volume 2780.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description 'Thin plate' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% None _diffrn_reflns_number 10945 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2326 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.11 _reflns_number_total 10945 _reflns_number_gt 5152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Software' _computing_cell_refinement 'CAD4-Software' _computing_data_reduction 'CADSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10945 _refine_ls_number_parameters 761 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2201 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.003 _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 0.26771(6) 0.20692(7) 0.12953(4) 0.0280(2) Uani 1 1 d . . . O1 O 0.3487(4) 0.1103(4) 0.2007(3) 0.0394(13) Uani 1 1 d . . . N1 N 0.4609(6) 0.1241(6) 0.1931(4) 0.057(2) Uani 1 1 d . . . C1 C 0.5516(8) 0.0098(10) 0.1813(6) 0.089(4) Uani 1 1 d . . . H1A H 0.525(3) -0.025(3) 0.140(3) 0.133 Uiso 1 1 calc R . . H1B H 0.563(4) -0.054(4) 0.229(3) 0.133 Uiso 1 1 calc R . . H1C H 0.637(5) 0.0192(15) 0.166(4) 0.133 Uiso 1 1 calc R . . Ge2 Ge 0.22052(6) 0.69573(7) 0.38426(4) 0.0262(2) Uani 1 1 d . . . O2 O 0.3216(4) 0.1321(4) 0.0566(3) 0.0362(12) Uani 1 1 d . . . N2 N 0.2781(6) 0.0367(5) 0.0651(3) 0.0452(17) Uani 1 1 d . . . C2 C 0.4732(10) 0.1593(11) 0.2568(7) 0.099(5) Uani 1 1 d . . . H2A H 0.552(6) 0.170(7) 0.2555(16) 0.148 Uiso 1 1 calc R . . H2B H 0.473(7) 0.095(5) 0.296(2) 0.148 Uiso 1 1 calc R . . H2C H 0.404(6) 0.238(6) 0.264(2) 0.148 Uiso 1 1 calc R . . O3 O 0.0846(4) 0.8056(4) 0.3524(2) 0.0327(12) Uani 1 1 d . . . N3 N 0.0063(5) 0.8189(6) 0.4143(3) 0.0363(15) Uani 1 1 d . . . C3 C 0.3795(9) -0.0673(7) 0.0506(5) 0.068(3) Uani 1 1 d . . . H3A H 0.436(4) -0.084(3) 0.081(3) 0.102 Uiso 1 1 calc R . . H3B H 0.409(4) -0.054(2) 0.007(3) 0.102 Uiso 1 1 calc R . . H3C H 0.3578(18) -0.130(4) 0.054(3) 0.102 Uiso 1 1 calc R . . O4 O 0.3125(4) 0.6626(4) 0.3084(2) 0.0359(12) Uani 1 1 d . . . N4 N 0.3151(5) 0.7759(6) 0.2764(3) 0.0420(16) Uani 1 1 d . . . C4 C 0.1923(8) 0.0722(9) 0.0114(5) 0.064(3) Uani 1 1 d . . . H4A H 0.156(4) 0.011(4) 0.0141(19) 0.096 Uiso 1 1 calc R . . H4B H 0.234(2) 0.077(5) -0.035(2) 0.096 Uiso 1 1 calc R . . H4C H 0.127(4) 0.153(4) 0.0177(18) 0.096 Uiso 1 1 calc R . . C5 C -0.0373(6) 0.9435(7) 0.4235(5) 0.049(2) Uani 1 1 d . . . H5A H 0.028(3) 0.9627(16) 0.431(3) 0.074 Uiso 1 1 calc R . . H5B H -0.092(4) 0.9587(14) 0.462(2) 0.074 Uiso 1 1 calc R . . H5C H -0.077(4) 0.992(2) 0.383(2) 0.074 Uiso 1 1 calc R . . C6 C -0.0892(6) 0.7912(8) 0.3958(4) 0.045(2) Uani 1 1 d . . . H6A H -0.0556(16) 0.703(4) 0.386(2) 0.067 Uiso 1 1 calc R . . H6B H -0.128(3) 0.847(4) 0.353(2) 0.067 Uiso 1 1 calc R . . H6C H -0.152(3) 0.803(4) 0.4358(19) 0.067 Uiso 1 1 calc R . . C7 C 0.2800(8) 0.7889(7) 0.2077(4) 0.054(2) Uani 1 1 d . . . H7A H 0.201(4) 0.787(5) 0.2086(4) 0.080 Uiso 1 1 calc R . . H7B H 0.337(4) 0.723(4) 0.1844(14) 0.080 Uiso 1 1 calc R . . H7C H 0.278(4) 0.865(4) 0.1834(14) 0.080 Uiso 1 1 calc R . . C8 C 0.4385(8) 0.7578(10) 0.2785(6) 0.076(3) Uani 1 1 d . . . H8A H 0.464(2) 0.748(5) 0.336(3) 0.115 Uiso 1 1 calc R . . H8B H 0.4533(15) 0.841(5) 0.247(3) 0.115 Uiso 1 1 calc R . . H8C H 0.500(3) 0.670(5) 0.254(3) 0.115 Uiso 1 1 calc R . . C10 C 0.0981(6) 0.2702(6) 0.1441(3) 0.0263(16) Uani 1 1 d . . . C11 C 0.0237(5) 0.2008(6) 0.1610(3) 0.0227(15) Uani 1 1 d . . . C12 C 0.0659(6) 0.0987(6) 0.2070(4) 0.0290(16) Uani 1 1 d . . . H12A H 0.140(5) 0.0755(18) 0.2261(14) 0.035 Uiso 1 1 calc R . . C13 C -0.0002(6) 0.0299(6) 0.2254(4) 0.0342(18) Uani 1 1 d . . . H13A H 0.0270 -0.0370 0.2574 0.041 Uiso 1 1 calc R . . C14 C -0.1067(7) 0.0629(7) 0.1954(4) 0.0361(18) Uani 1 1 d . . . H14A H -0.150(3) 0.019(4) 0.2070(10) 0.043 Uiso 1 1 calc R . . C15 C -0.1488(7) 0.1622(6) 0.1476(4) 0.0327(17) Uani 1 1 d . . . H15A H -0.229(5) 0.1859(17) 0.1241(16) 0.039 Uiso 1 1 calc R . . C16 C -0.0821(6) 0.2294(7) 0.1318(4) 0.0313(17) Uani 1 1 d . . . H16A H -0.114(2) 0.305(5) 0.096(2) 0.038 Uiso 1 1 calc R . . C20 C 0.0597(5) 0.3901(6) 0.1331(3) 0.0227(15) Uani 1 1 d . . . C21 C -0.0655(6) 0.4745(6) 0.1350(3) 0.0238(15) Uani 1 1 d . . . C22 C -0.1142(6) 0.5572(6) 0.0785(4) 0.0271(16) Uani 1 1 d . . . H22A H -0.060(3) 0.5588(6) 0.032(3) 0.033 Uiso 1 1 calc R . . C23 C -0.2311(6) 0.6368(7) 0.0816(4) 0.0353(18) Uani 1 1 d . . . H23A H -0.262(3) 0.690(5) 0.045(3) 0.042 Uiso 1 1 calc R . . C24 C -0.3002(6) 0.6354(7) 0.1402(4) 0.038(2) Uani 1 1 d . . . H24A H -0.380(6) 0.691(4) 0.1422(4) 0.045 Uiso 1 1 calc R . . C25 C -0.2540(6) 0.5546(6) 0.1951(4) 0.0324(18) Uani 1 1 d . . . H25A H -0.301(4) 0.5532(7) 0.234(3) 0.039 Uiso 1 1 calc R . . C26 C -0.1370(6) 0.4741(6) 0.1932(4) 0.0302(17) Uani 1 1 d . . . H26A H -0.110(2) 0.426(4) 0.226(3) 0.036 Uiso 1 1 calc R . . C30 C 0.1562(5) 0.4399(6) 0.1187(3) 0.0258(16) Uani 1 1 d . . . C31 C 0.1176(5) 0.5710(6) 0.1122(3) 0.0238(15) Uani 1 1 d . . . C32 C 0.1473(6) 0.6322(6) 0.0546(4) 0.0290(17) Uani 1 1 d . . . H32A H 0.187(3) 0.595(3) 0.022(3) 0.035 Uiso 1 1 calc R . . C33 C 0.1133(6) 0.7520(7) 0.0494(4) 0.0347(18) Uani 1 1 d . . . H33A H 0.1315(17) 0.789(3) 0.013(3) 0.042 Uiso 1 1 calc R . . C34 C 0.0507(7) 0.8149(7) 0.1012(4) 0.041(2) Uani 1 1 d . . . H34A H 0.030(2) 0.893(7) 0.0976(5) 0.049 Uiso 1 1 calc R . . C35 C 0.0206(6) 0.7541(7) 0.1597(4) 0.0373(19) Uani 1 1 d . . . H35A H -0.028(3) 0.802(3) 0.201(3) 0.045 Uiso 1 1 calc R . . C36 C 0.0529(6) 0.6343(6) 0.1651(4) 0.0321(17) Uani 1 1 d . . . H36A H 0.0316(17) 0.595(3) 0.204(3) 0.039 Uiso 1 1 calc R . . C40 C 0.2679(6) 0.3635(6) 0.1127(4) 0.0295(17) Uani 1 1 d . . . C41 C 0.3751(6) 0.3904(6) 0.1027(3) 0.0255(15) Uani 1 1 d . . . C42 C 0.3923(6) 0.4691(6) 0.1387(4) 0.0298(16) Uani 1 1 d . . . H42A H 0.330(4) 0.512(3) 0.172(2) 0.036 Uiso 1 1 calc R . . C43 C 0.4957(6) 0.4885(6) 0.1296(4) 0.0353(18) Uani 1 1 d . . . H43A H 0.5072(10) 0.544(4) 0.1559(19) 0.042 Uiso 1 1 calc R . . C44 C 0.5806(6) 0.4316(7) 0.0844(4) 0.039(2) Uani 1 1 d . . . H44A H 0.643(5) 0.4452(13) 0.0782(7) 0.046 Uiso 1 1 calc R . . C45 C 0.5682(6) 0.3525(7) 0.0483(4) 0.041(2) Uani 1 1 d . . . H45A H 0.625(5) 0.314(3) 0.020(2) 0.049 Uiso 1 1 calc R . . C46 C 0.4645(6) 0.3329(7) 0.0572(4) 0.0367(19) Uani 1 1 d . . . H46A H 0.4553(9) 0.282(4) 0.033(2) 0.044 Uiso 1 1 calc R . . C50 C 0.2765(6) 0.7321(6) 0.4610(4) 0.0275(16) Uani 1 1 d . . . C51 C 0.2975(6) 0.8431(6) 0.4628(4) 0.0291(16) Uani 1 1 d . . . C52 C 0.2715(6) 0.9260(6) 0.4049(4) 0.0350(18) Uani 1 1 d . . . H52A H 0.239(2) 0.9097(13) 0.364(3) 0.042 Uiso 1 1 calc R . . C53 C 0.2886(7) 1.0306(7) 0.4013(5) 0.041(2) Uani 1 1 d . . . H53A H 0.2700(15) 1.092(5) 0.357(3) 0.049 Uiso 1 1 calc R . . C54 C 0.3303(6) 1.0519(7) 0.4575(5) 0.045(2) Uani 1 1 d . . . H54A H 0.3388(11) 1.113(6) 0.4565(5) 0.054 Uiso 1 1 calc R . . C55 C 0.3576(6) 0.9710(7) 0.5150(4) 0.0386(19) Uani 1 1 d . . . H55A H 0.391(2) 0.9884(14) 0.557(3) 0.046 Uiso 1 1 calc R . . C56 C 0.3415(6) 0.8673(7) 0.5182(4) 0.0348(19) Uani 1 1 d . . . H56A H 0.3564(16) 0.823(4) 0.550(3) 0.042 Uiso 1 1 calc R . . C60 C 0.2846(5) 0.6437(6) 0.5116(4) 0.0266(16) Uani 1 1 d . . . C61 C 0.3082(5) 0.6437(6) 0.5832(3) 0.0238(15) Uani 1 1 d . . . C62 C 0.2170(6) 0.7170(6) 0.6221(4) 0.0290(17) Uani 1 1 d . . . H62A H 0.143(6) 0.760(3) 0.6038(14) 0.035 Uiso 1 1 calc R . . C63 C 0.2352(7) 0.7260(7) 0.6882(4) 0.0348(18) Uani 1 1 d . . . H63A H 0.168(5) 0.780(4) 0.717(2) 0.042 Uiso 1 1 calc R . . C64 C 0.3468(7) 0.6605(7) 0.7154(4) 0.040(2) Uani 1 1 d . . . H64A H 0.3594(13) 0.6654(8) 0.758(4) 0.048 Uiso 1 1 calc R . . C65 C 0.4379(6) 0.5877(6) 0.6758(4) 0.0345(18) Uani 1 1 d . . . H65A H 0.531(6) 0.535(3) 0.6974(14) 0.041 Uiso 1 1 calc R . . C66 C 0.4175(6) 0.5783(6) 0.6108(4) 0.0326(18) Uani 1 1 d . . . H66A H 0.471(5) 0.533(4) 0.588(2) 0.039 Uiso 1 1 calc R . . C70 C 0.2572(5) 0.5423(6) 0.4955(3) 0.0244(15) Uani 1 1 d . . . C71 C 0.2820(6) 0.4369(6) 0.5473(3) 0.0250(15) Uani 1 1 d . . . C72 C 0.2176(6) 0.4419(7) 0.6091(4) 0.0325(17) Uani 1 1 d . . . H72A H 0.153(5) 0.520(5) 0.6198(8) 0.039 Uiso 1 1 calc R . . C73 C 0.2409(7) 0.3422(7) 0.6556(4) 0.0369(19) Uani 1 1 d . . . H73A H 0.200(4) 0.3466(8) 0.694(3) 0.044 Uiso 1 1 calc R . . C74 C 0.3290(7) 0.2351(7) 0.6419(4) 0.042(2) Uani 1 1 d . . . H74A H 0.3434(15) 0.173(6) 0.671(3) 0.051 Uiso 1 1 calc R . . C75 C 0.3924(6) 0.2294(7) 0.5821(4) 0.0365(19) Uani 1 1 d . . . H75A H 0.446(5) 0.165(6) 0.5738(8) 0.044 Uiso 1 1 calc R . . C76 C 0.3705(6) 0.3281(6) 0.5348(4) 0.0260(16) Uani 1 1 d . . . H76A H 0.414(3) 0.3223(7) 0.495(3) 0.031 Uiso 1 1 calc R . . C80 C 0.2182(6) 0.5510(6) 0.4330(3) 0.0281(16) Uani 1 1 d . . . C81 C 0.1782(6) 0.4695(6) 0.4067(4) 0.0280(16) Uani 1 1 d . . . C82 C 0.1192(6) 0.4073(6) 0.4484(4) 0.0306(17) Uani 1 1 d . . . H82A H 0.1062(10) 0.4145(8) 0.501(3) 0.037 Uiso 1 1 calc R . . C83 C 0.0782(6) 0.3364(7) 0.4205(4) 0.0379(19) Uani 1 1 d . . . H83A H 0.042(3) 0.299(3) 0.446(2) 0.046 Uiso 1 1 calc R . . C84 C 0.0948(6) 0.3254(7) 0.3519(4) 0.0390(19) Uani 1 1 d . . . H84A H 0.064(2) 0.273(4) 0.3318(15) 0.047 Uiso 1 1 calc R . . C85 C 0.1531(7) 0.3849(7) 0.3111(4) 0.042(2) Uani 1 1 d . . . H85A H 0.1662(13) 0.3765(9) 0.265(4) 0.050 Uiso 1 1 calc R . . C86 C 0.1927(7) 0.4577(7) 0.3382(4) 0.0397(19) Uani 1 1 d . . . H86A H 0.230(3) 0.499(3) 0.310(2) 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0280(4) 0.0272(5) 0.0284(5) -0.0038(4) -0.0008(3) -0.0104(4) O1 0.040(3) 0.046(3) 0.037(3) 0.009(3) -0.008(2) -0.025(3) N1 0.040(4) 0.045(5) 0.078(6) 0.025(4) -0.018(4) -0.016(4) C1 0.043(6) 0.079(8) 0.127(11) 0.002(7) -0.031(6) -0.006(6) Ge2 0.0263(4) 0.0269(5) 0.0244(5) -0.0032(4) -0.0009(3) -0.0096(3) O2 0.035(3) 0.031(3) 0.046(3) -0.011(3) 0.003(2) -0.017(2) N2 0.060(4) 0.030(4) 0.049(5) -0.009(3) 0.011(4) -0.023(3) C2 0.076(8) 0.107(10) 0.125(12) -0.033(9) -0.045(8) -0.032(7) O3 0.032(3) 0.033(3) 0.027(3) 0.003(2) -0.001(2) -0.011(2) N3 0.028(3) 0.045(4) 0.038(4) -0.010(3) 0.004(3) -0.016(3) C3 0.096(8) 0.029(5) 0.067(7) -0.010(5) 0.024(6) -0.018(5) O4 0.037(3) 0.036(3) 0.028(3) -0.008(2) 0.001(2) -0.006(2) N4 0.041(4) 0.051(4) 0.041(4) -0.006(3) 0.004(3) -0.028(3) C4 0.070(6) 0.086(8) 0.056(7) -0.019(6) -0.006(5) -0.047(6) C5 0.033(4) 0.052(6) 0.070(6) -0.021(5) 0.008(4) -0.020(4) C6 0.028(4) 0.058(6) 0.054(6) -0.010(5) 0.000(4) -0.022(4) C7 0.067(6) 0.045(5) 0.041(6) -0.002(4) -0.002(4) -0.015(5) C8 0.044(5) 0.122(10) 0.086(8) -0.032(7) 0.014(5) -0.054(6) C10 0.035(4) 0.035(4) 0.016(4) -0.005(3) 0.003(3) -0.020(3) C11 0.027(3) 0.021(4) 0.019(4) -0.001(3) 0.003(3) -0.010(3) C12 0.026(4) 0.025(4) 0.031(4) -0.005(3) 0.000(3) -0.004(3) C13 0.039(4) 0.020(4) 0.037(5) 0.002(3) 0.002(4) -0.008(3) C14 0.043(4) 0.036(5) 0.035(5) -0.007(4) 0.005(4) -0.022(4) C15 0.039(4) 0.032(4) 0.031(4) -0.003(4) 0.000(3) -0.018(4) C16 0.040(4) 0.031(4) 0.027(4) -0.002(3) -0.005(3) -0.017(3) C20 0.029(3) 0.028(4) 0.013(4) -0.007(3) 0.000(3) -0.012(3) C21 0.033(4) 0.025(4) 0.019(4) -0.005(3) 0.002(3) -0.018(3) C22 0.026(3) 0.026(4) 0.031(4) -0.006(3) 0.005(3) -0.013(3) C23 0.040(4) 0.033(4) 0.037(5) 0.002(4) -0.008(4) -0.020(4) C24 0.025(4) 0.042(5) 0.047(5) -0.016(4) 0.006(4) -0.012(4) C25 0.029(4) 0.042(5) 0.034(5) -0.014(4) 0.006(3) -0.020(4) C26 0.031(4) 0.036(4) 0.025(4) -0.005(3) 0.000(3) -0.015(3) C30 0.028(4) 0.034(4) 0.023(4) -0.007(3) 0.010(3) -0.021(3) C31 0.022(3) 0.027(4) 0.024(4) -0.003(3) 0.001(3) -0.011(3) C32 0.033(4) 0.027(4) 0.029(4) -0.010(3) -0.002(3) -0.011(3) C33 0.040(4) 0.042(5) 0.022(4) 0.001(4) -0.002(3) -0.018(4) C34 0.054(5) 0.025(4) 0.042(5) -0.005(4) -0.001(4) -0.014(4) C35 0.038(4) 0.034(4) 0.043(5) -0.018(4) 0.002(4) -0.013(4) C36 0.037(4) 0.036(4) 0.027(4) -0.007(4) 0.000(3) -0.018(3) C40 0.025(4) 0.039(4) 0.028(4) -0.013(4) 0.006(3) -0.014(3) C41 0.028(4) 0.024(4) 0.024(4) -0.001(3) -0.006(3) -0.009(3) C42 0.027(4) 0.033(4) 0.031(4) -0.010(3) 0.003(3) -0.012(3) C43 0.030(4) 0.032(4) 0.048(5) -0.012(4) -0.008(4) -0.013(3) C44 0.030(4) 0.045(5) 0.046(5) -0.012(4) 0.001(4) -0.020(4) C45 0.032(4) 0.046(5) 0.042(5) -0.011(4) 0.008(4) -0.013(4) C46 0.037(4) 0.042(5) 0.037(5) -0.015(4) 0.004(4) -0.018(4) C50 0.029(4) 0.020(4) 0.030(4) -0.008(3) 0.006(3) -0.006(3) C51 0.024(3) 0.025(4) 0.036(5) -0.007(4) 0.002(3) -0.007(3) C52 0.033(4) 0.022(4) 0.051(5) -0.006(4) -0.003(4) -0.010(3) C53 0.046(5) 0.026(4) 0.054(6) -0.002(4) -0.005(4) -0.019(4) C54 0.034(4) 0.030(5) 0.073(7) -0.017(5) 0.007(4) -0.015(4) C55 0.036(4) 0.032(4) 0.055(6) -0.014(4) -0.007(4) -0.017(4) C56 0.030(4) 0.036(4) 0.037(5) -0.008(4) -0.005(3) -0.009(3) C60 0.019(3) 0.033(4) 0.028(4) -0.011(3) 0.003(3) -0.009(3) C61 0.025(3) 0.026(4) 0.023(4) -0.005(3) -0.002(3) -0.012(3) C62 0.029(4) 0.028(4) 0.029(4) 0.000(3) -0.002(3) -0.011(3) C63 0.042(4) 0.037(4) 0.028(4) -0.013(4) 0.005(3) -0.015(4) C64 0.055(5) 0.041(5) 0.028(5) -0.004(4) -0.007(4) -0.021(4) C65 0.031(4) 0.035(4) 0.036(5) 0.002(4) -0.009(3) -0.011(3) C66 0.024(4) 0.031(4) 0.039(5) -0.010(4) -0.002(3) -0.006(3) C70 0.026(3) 0.029(4) 0.019(4) -0.010(3) 0.004(3) -0.011(3) C71 0.033(4) 0.029(4) 0.023(4) -0.007(3) -0.003(3) -0.021(3) C72 0.041(4) 0.031(4) 0.031(5) -0.008(4) 0.003(3) -0.020(4) C73 0.045(5) 0.050(5) 0.025(4) -0.006(4) -0.001(3) -0.028(4) C74 0.053(5) 0.043(5) 0.042(5) 0.015(4) -0.025(4) -0.032(4) C75 0.029(4) 0.032(4) 0.047(5) 0.003(4) -0.014(4) -0.011(3) C76 0.025(3) 0.028(4) 0.027(4) -0.008(3) -0.003(3) -0.011(3) C80 0.031(4) 0.028(4) 0.021(4) -0.003(3) 0.005(3) -0.009(3) C81 0.032(4) 0.022(4) 0.027(4) -0.005(3) -0.004(3) -0.007(3) C82 0.038(4) 0.031(4) 0.022(4) -0.004(3) -0.008(3) -0.012(3) C83 0.041(4) 0.038(5) 0.038(5) 0.001(4) -0.011(4) -0.020(4) C84 0.041(4) 0.037(5) 0.044(5) -0.010(4) -0.010(4) -0.017(4) C85 0.061(5) 0.038(5) 0.030(5) -0.009(4) -0.010(4) -0.019(4) C86 0.049(5) 0.048(5) 0.029(5) -0.004(4) -0.002(4) -0.027(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 O2 1.776(5) . ? Ge1 O1 1.802(5) . ? Ge1 C40 1.928(7) . ? Ge1 C10 1.932(7) . ? O1 N1 1.460(8) . ? N1 C1 1.448(11) . ? N1 C2 1.449(12) . ? C1 H1A 1.1214 . ? C1 H1B 1.1214 . ? C1 H1C 1.1214 . ? Ge2 O3 1.785(5) . ? Ge2 O4 1.798(5) . ? Ge2 C80 1.921(7) . ? Ge2 C50 1.926(7) . ? O2 N2 1.472(7) . ? N2 C3 1.437(10) . ? N2 C4 1.475(10) . ? C2 H2A 1.0326 . ? C2 H2B 1.0326 . ? C2 H2C 1.0326 . ? O3 N3 1.480(7) . ? N3 C6 1.455(8) . ? N3 C5 1.457(9) . ? C3 H3A 0.9206 . ? C3 H3B 0.9206 . ? C3 H3C 0.9206 . ? O4 N4 1.468(8) . ? N4 C7 1.444(10) . ? N4 C8 1.457(9) . ? C4 H4A 1.0239 . ? C4 H4B 1.0239 . ? C4 H4C 1.0239 . ? C5 H5A 0.9655 . ? C5 H5B 0.9655 . ? C5 H5C 0.9655 . ? C6 H6A 1.0455 . ? C6 H6B 1.0455 . ? C6 H6C 1.0455 . ? C7 H7A 0.9847 . ? C7 H7B 0.9847 . ? C7 H7C 0.9847 . ? C8 H8A 1.1925 . ? C8 H8B 1.1925 . ? C8 H8C 1.1925 . ? C10 C20 1.360(9) . ? C10 C11 1.486(8) . ? C11 C16 1.376(9) . ? C11 C12 1.389(9) . ? C12 C13 1.398(9) . ? C12 H12A 0.9445 . ? C13 C14 1.383(10) . ? C13 H13A 0.9300 . ? C14 C15 1.386(10) . ? C14 H14A 0.8996 . ? C15 C16 1.382(9) . ? C15 H15A 1.0553 . ? C16 H16A 1.0519 . ? C20 C21 1.480(9) . ? C20 C30 1.543(8) . ? C21 C26 1.392(9) . ? C21 C22 1.402(9) . ? C22 C23 1.387(9) . ? C22 H22A 1.0960 . ? C23 C24 1.381(10) . ? C23 H23A 0.8978 . ? C24 C25 1.364(10) . ? C24 H24A 0.9533 . ? C25 C26 1.390(9) . ? C25 H25A 0.9347 . ? C26 H26A 0.8162 . ? C30 C40 1.330(9) . ? C30 C31 1.492(9) . ? C31 C32 1.382(9) . ? C31 C36 1.398(9) . ? C32 C33 1.366(9) . ? C32 H32A 0.8479 . ? C33 C34 1.373(10) . ? C33 H33A 0.8611 . ? C34 C35 1.395(10) . ? C34 H34A 0.8916 . ? C35 C36 1.369(10) . ? C35 H35A 1.0721 . ? C36 H36A 0.9302 . ? C40 C41 1.486(9) . ? C41 C46 1.388(9) . ? C41 C42 1.392(9) . ? C42 C43 1.389(9) . ? C42 H42A 0.9949 . ? C43 C44 1.352(10) . ? C43 H43A 0.9856 . ? C44 C45 1.368(10) . ? C44 H44A 0.8525 . ? C45 C46 1.394(9) . ? C45 H45A 0.8860 . ? C46 H46A 0.9071 . ? C50 C60 1.353(10) . ? C50 C51 1.513(9) . ? C51 C52 1.394(10) . ? C51 C56 1.401(9) . ? C52 C53 1.392(9) . ? C52 H52A 1.0244 . ? C53 C54 1.382(11) . ? C53 H53A 1.0630 . ? C54 C55 1.375(11) . ? C54 H54A 0.8025 . ? C55 C56 1.377(10) . ? C55 H55A 1.0488 . ? C56 H56A 0.7539 . ? C60 C61 1.485(9) . ? C60 C70 1.518(9) . ? C61 C66 1.384(9) . ? C61 C62 1.386(9) . ? C62 C63 1.389(9) . ? C62 H62A 0.9337 . ? C63 C64 1.403(10) . ? C63 H63A 1.0246 . ? C64 C65 1.391(10) . ? C64 H64A 0.8955 . ? C65 C66 1.376(10) . ? C65 H65A 1.1574 . ? C66 H66A 0.8196 . ? C70 C80 1.355(9) . ? C70 C71 1.484(9) . ? C71 C76 1.395(9) . ? C71 C72 1.397(9) . ? C72 C73 1.376(10) . ? C72 H72A 1.0133 . ? C73 C74 1.385(10) . ? C73 H73A 0.8799 . ? C74 C75 1.359(10) . ? C74 H74A 0.8554 . ? C75 C76 1.378(10) . ? C75 H75A 0.8347 . ? C76 H76A 0.9055 . ? C80 C81 1.474(9) . ? C81 C86 1.385(10) . ? C81 C82 1.404(9) . ? C82 C83 1.385(9) . ? C82 H82A 1.0558 . ? C83 C84 1.384(10) . ? C83 H83A 0.8525 . ? C84 C85 1.367(10) . ? C84 H84A 1.0276 . ? C85 C86 1.386(10) . ? C85 H85A 0.9312 . ? C86 H86A 0.9259 . ? 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 O2 Ge1 O1 107.6(2) . . ? O2 Ge1 C40 110.7(3) . . ? O1 Ge1 C40 116.9(3) . . ? O2 Ge1 C10 115.0(2) . . ? O1 Ge1 C10 114.5(3) . . ? C40 Ge1 C10 91.8(3) . . ? N1 O1 Ge1 103.4(4) . . ? C1 N1 C2 112.3(8) . . ? C1 N1 O1 106.7(7) . . ? C2 N1 O1 105.0(7) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 Ge2 O4 102.7(2) . . ? O3 Ge2 C80 117.8(2) . . ? O4 Ge2 C80 108.9(2) . . ? O3 Ge2 C50 115.2(2) . . ? O4 Ge2 C50 120.4(2) . . ? C80 Ge2 C50 92.4(3) . . ? N2 O2 Ge1 105.8(4) . . ? C3 N2 O2 104.9(6) . . ? C3 N2 C4 109.9(7) . . ? O2 N2 C4 104.1(6) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 O3 Ge2 101.5(4) . . ? C6 N3 C5 110.2(6) . . ? C6 N3 O3 103.7(5) . . ? C5 N3 O3 105.5(5) . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 O4 Ge2 105.5(4) . . ? C7 N4 C8 111.8(7) . . ? C7 N4 O4 105.1(6) . . ? C8 N4 O4 103.9(7) . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C20 C10 C11 126.7(6) . . ? C20 C10 Ge1 106.8(4) . . ? C11 C10 Ge1 126.5(5) . . ? C16 C11 C12 118.2(6) . . ? C16 C11 C10 123.8(6) . . ? C12 C11 C10 117.9(6) . . ? C11 C12 C13 120.7(7) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C14 C13 C12 118.9(7) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 121.4(7) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C16 C15 C14 118.0(7) . . ? C16 C15 H15A 121.0 . . ? C14 C15 H15A 121.0 . . ? C11 C16 C15 122.7(7) . . ? C11 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? C10 C20 C21 125.3(6) . . ? C10 C20 C30 116.2(6) . . ? C21 C20 C30 118.5(6) . . ? C26 C21 C22 118.6(6) . . ? C26 C21 C20 120.5(6) . . ? C22 C21 C20 120.9(6) . . ? C23 C22 C21 120.0(6) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.4(8) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 120.1(7) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.5(7) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C21 120.4(7) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C40 C30 C31 124.4(6) . . ? C40 C30 C20 118.1(6) . . ? C31 C30 C20 117.5(5) . . ? C32 C31 C36 118.6(6) . . ? C32 C31 C30 120.9(6) . . ? C36 C31 C30 120.5(6) . . ? C33 C32 C31 120.6(7) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 121.3(7) . . ? C32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? C33 C34 C35 118.6(7) . . ? C33 C34 H34A 120.7 . . ? C35 C34 H34A 120.7 . . ? C36 C35 C34 120.6(7) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C31 120.3(7) . . ? C35 C36 H36A 119.9 . . ? C31 C36 H36A 119.9 . . ? C30 C40 C41 127.4(6) . . ? C30 C40 Ge1 107.0(5) . . ? C41 C40 Ge1 125.3(5) . . ? C46 C41 C42 117.7(6) . . ? C46 C41 C40 119.4(6) . . ? C42 C41 C40 122.9(6) . . ? C43 C42 C41 121.0(6) . . ? C43 C42 H42A 119.5 . . ? C41 C42 H42A 119.5 . . ? C44 C43 C42 119.7(7) . . ? C44 C43 H43A 120.2 . . ? C42 C43 H43A 120.2 . . ? C43 C44 C45 121.4(7) . . ? C43 C44 H44A 119.3 . . ? C45 C44 H44A 119.3 . . ? C44 C45 C46 119.2(7) . . ? C44 C45 H45A 120.4 . . ? C46 C45 H45A 120.4 . . ? C41 C46 C45 121.0(7) . . ? C41 C46 H46A 119.5 . . ? C45 C46 H46A 119.5 . . ? C60 C50 C51 128.9(7) . . ? C60 C50 Ge2 106.1(5) . . ? C51 C50 Ge2 124.9(5) . . ? C52 C51 C56 118.4(7) . . ? C52 C51 C50 117.1(6) . . ? C56 C51 C50 124.5(7) . . ? C53 C52 C51 121.4(8) . . ? C53 C52 H52A 119.3 . . ? C51 C52 H52A 119.3 . . ? C54 C53 C52 118.3(8) . . ? C54 C53 H53A 120.8 . . ? C52 C53 H53A 120.8 . . ? C55 C54 C53 121.3(7) . . ? C55 C54 H54A 119.3 . . ? C53 C54 H54A 119.3 . . ? C54 C55 C56 120.3(8) . . ? C54 C55 H55A 119.9 . . ? C56 C55 H55A 119.9 . . ? C55 C56 C51 120.3(8) . . ? C55 C56 H56A 119.9 . . ? C51 C56 H56A 119.9 . . ? C50 C60 C61 124.6(6) . . ? C50 C60 C70 117.6(6) . . ? C61 C60 C70 117.6(6) . . ? C66 C61 C62 119.7(6) . . ? C66 C61 C60 122.8(6) . . ? C62 C61 C60 117.5(6) . . ? C61 C62 C63 120.4(7) . . ? C61 C62 H62A 119.8 . . ? C63 C62 H62A 119.8 . . ? C62 C63 C64 119.5(7) . . ? C62 C63 H63A 120.3 . . ? C64 C63 H63A 120.3 . . ? C65 C64 C63 119.7(7) . . ? C65 C64 H64A 120.2 . . ? C63 C64 H64A 120.2 . . ? C66 C65 C64 120.0(7) . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C65 C66 C61 120.8(7) . . ? C65 C66 H66A 119.6 . . ? C61 C66 H66A 119.6 . . ? C80 C70 C71 124.0(6) . . ? C80 C70 C60 117.7(6) . . ? C71 C70 C60 118.2(6) . . ? C76 C71 C72 117.8(7) . . ? C76 C71 C70 120.2(6) . . ? C72 C71 C70 122.0(6) . . ? C73 C72 C71 120.7(7) . . ? C73 C72 H72A 119.6 . . ? C71 C72 H72A 119.6 . . ? C72 C73 C74 120.4(7) . . ? C72 C73 H73A 119.8 . . ? C74 C73 H73A 119.8 . . ? C75 C74 C73 119.3(8) . . ? C75 C74 H74A 120.3 . . ? C73 C74 H74A 120.3 . . ? C74 C75 C76 121.2(8) . . ? C74 C75 H75A 119.4 . . ? C76 C75 H75A 119.4 . . ? C75 C76 C71 120.6(7) . . ? C75 C76 H76A 119.7 . . ? C71 C76 H76A 119.7 . . ? C70 C80 C81 128.1(6) . . ? C70 C80 Ge2 106.1(5) . . ? C81 C80 Ge2 125.7(5) . . ? C86 C81 C82 117.9(6) . . ? C86 C81 C80 119.9(6) . . ? C82 C81 C80 122.1(6) . . ? C83 C82 C81 119.9(7) . . ? C83 C82 H82A 120.1 . . ? C81 C82 H82A 120.1 . . ? C84 C83 C82 120.9(7) . . ? C84 C83 H83A 119.5 . . ? C82 C83 H83A 119.5 . . ? C85 C84 C83 119.6(7) . . ? C85 C84 H84A 120.2 . . ? C83 C84 H84A 120.2 . . ? C84 C85 C86 120.0(8) . . ? C84 C85 H85A 120.0 . . ? C86 C85 H85A 120.0 . . ? C81 C86 C85 121.7(7) . . ? C81 C86 H86A 119.2 . . ? C85 C86 H86A 119.2 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.619 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.118