# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xuefeng Fu' _publ_contact_author_email fuxf@pku.edu.cn loop_ _publ_author_name 'Huayi Fang' 'Zhen Ling' P.Brothers 'Xuefeng Fu' data_(TPFC)Ge-CH3 _database_code_depnum_ccdc_archive 'CCDC 839547' #TrackingRef '- Crystal structure data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C38 H11 F15 Ge N4, C3 H6 O' _chemical_formula_sum 'C41 H17 F15 Ge N4 O' _chemical_formula_weight 939.18 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' 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 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 18.678(4) _cell_length_b 7.4805(15) _cell_length_c 26.052(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.76(3) _cell_angle_gamma 90.00 _cell_volume 3635.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 496 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description strip _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8090 _exptl_absorpt_correction_T_max 0.9625 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24143 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6375 _reflns_number_gt 5804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0343P)^2^+6.6169P] 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 6375 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 0.39722(2) 0.62256(6) 0.234107(15) 0.02328(13) Uani 1 1 d . . . F1 F 0.28325(14) 0.3850(3) 0.05438(9) 0.0399(6) Uani 1 1 d . . . F2 F 0.23127(15) 0.3924(4) -0.04291(10) 0.0500(7) Uani 1 1 d . . . F3 F 0.22420(17) 0.7050(4) -0.09562(10) 0.0604(9) Uani 1 1 d . . . F4 F 0.27304(17) 1.0109(4) -0.04998(10) 0.0566(8) Uani 1 1 d . . . F5 F 0.32640(13) 1.0070(3) 0.04692(9) 0.0364(6) Uani 1 1 d . . . F6 F 0.42949(13) 1.0024(3) 0.42612(9) 0.0367(6) Uani 1 1 d . . . F7 F 0.42631(14) 1.0002(4) 0.52822(11) 0.0554(8) Uani 1 1 d . . . F8 F 0.41524(16) 0.6857(5) 0.57988(10) 0.0723(11) Uani 1 1 d . . . F9 F 0.40488(16) 0.3733(4) 0.52681(11) 0.0619(9) Uani 1 1 d . . . F10 F 0.40586(15) 0.3744(3) 0.42435(11) 0.0471(7) Uani 1 1 d . . . F11 F 0.64949(14) 0.5793(4) 0.18326(12) 0.0494(7) Uani 1 1 d . . . F12 F 0.78471(14) 0.6578(4) 0.16105(12) 0.0540(8) Uani 1 1 d . . . F13 F 0.83382(13) 0.9986(4) 0.17091(11) 0.0518(8) Uani 1 1 d . . . F14 F 0.74564(13) 1.2600(4) 0.20343(10) 0.0430(7) Uani 1 1 d . . . F15 F 0.61106(13) 1.1820(3) 0.22698(10) 0.0405(6) Uani 1 1 d . . . O1 O 0.4350(2) 0.8314(7) -0.03648(14) 0.0736(13) Uani 1 1 d . . . N1 N 0.43275(16) 0.7462(5) 0.17509(12) 0.0262(8) Uani 1 1 d . . . N2 N 0.30511(16) 0.6235(4) 0.19692(12) 0.0251(7) Uani 1 1 d . . . N3 N 0.33290(16) 0.6262(4) 0.28984(12) 0.0254(7) Uani 1 1 d . . . N4 N 0.46384(16) 0.7505(4) 0.28021(12) 0.0246(7) Uani 1 1 d . . . C1 C 0.5031(2) 0.8066(5) 0.17236(15) 0.0248(9) Uani 1 1 d . . . C2 C 0.5167(2) 0.8404(5) 0.12057(15) 0.0281(9) Uani 1 1 d . . . H2A H 0.5607 0.8821 0.1082 0.034 Uiso 1 1 calc R . . C3 C 0.4565(2) 0.8034(6) 0.09115(16) 0.0298(9) Uani 1 1 d . . . H3A H 0.4511 0.8156 0.0549 0.036 Uiso 1 1 calc R . . C4 C 0.4027(2) 0.7431(6) 0.12417(15) 0.0271(9) Uani 1 1 d . . . C5 C 0.3332(2) 0.6909(6) 0.10998(15) 0.0259(9) Uani 1 1 d . . . C6 C 0.2843(2) 0.6382(5) 0.14611(15) 0.0264(9) Uani 1 1 d . . . C7 C 0.2090(2) 0.6083(6) 0.14172(16) 0.0296(9) Uani 1 1 d . . . H7A H 0.1801 0.6080 0.1107 0.036 Uiso 1 1 calc R . . C8 C 0.1854(2) 0.5801(5) 0.18989(16) 0.0276(9) Uani 1 1 d . . . H8A H 0.1374 0.5575 0.1985 0.033 Uiso 1 1 calc R . . C9 C 0.2460(2) 0.5911(5) 0.22469(15) 0.0258(9) Uani 1 1 d . . . C10 C 0.2615(2) 0.5922(5) 0.27766(15) 0.0257(9) Uani 1 1 d . . . C11 C 0.2257(2) 0.5783(5) 0.32428(15) 0.0268(9) Uani 1 1 d . . . H11A H 0.1762 0.5543 0.3276 0.032 Uiso 1 1 calc R . . C12 C 0.2759(2) 0.6059(5) 0.36354(16) 0.0283(9) Uani 1 1 d . . . H12A H 0.2672 0.6047 0.3992 0.034 Uiso 1 1 calc R . . C13 C 0.3430(2) 0.6365(5) 0.34185(15) 0.0252(9) Uani 1 1 d . . . C14 C 0.4097(2) 0.6881(5) 0.36376(15) 0.0243(9) Uani 1 1 d . . . C15 C 0.4661(2) 0.7438(5) 0.33424(15) 0.0252(9) Uani 1 1 d . . . C16 C 0.5347(2) 0.8043(6) 0.35268(16) 0.0300(9) Uani 1 1 d . . . H16A H 0.5506 0.8142 0.3878 0.036 Uiso 1 1 calc R . . C17 C 0.5737(2) 0.8457(6) 0.31161(15) 0.0292(9) Uani 1 1 d . . . H17A H 0.6214 0.8900 0.3130 0.035 Uiso 1 1 calc R . . C18 C 0.5309(2) 0.8112(5) 0.26639(15) 0.0260(9) Uani 1 1 d . . . C19 C 0.5496(2) 0.8311(5) 0.21539(15) 0.0259(9) Uani 1 1 d . . . C20 C 0.3070(2) 0.6962(6) 0.05473(14) 0.0255(9) Uani 1 1 d . . . C21 C 0.2816(2) 0.5436(6) 0.02971(16) 0.0288(9) Uani 1 1 d . . . C22 C 0.2545(2) 0.5449(6) -0.02049(16) 0.0349(10) Uani 1 1 d . . . C23 C 0.2509(2) 0.7020(7) -0.04694(16) 0.0383(11) Uani 1 1 d . . . C24 C 0.2753(2) 0.8564(6) -0.02390(16) 0.0357(10) Uani 1 1 d . . . C25 C 0.3028(2) 0.8513(6) 0.02624(16) 0.0281(9) Uani 1 1 d . . . C26 C 0.4170(2) 0.6885(6) 0.42098(15) 0.0264(9) Uani 1 1 d . . . C27 C 0.4233(2) 0.8440(6) 0.44988(16) 0.0299(10) Uani 1 1 d . . . C28 C 0.4226(2) 0.8441(7) 0.50282(17) 0.0369(11) Uani 1 1 d . . . C29 C 0.4161(2) 0.6871(8) 0.52868(17) 0.0443(13) Uani 1 1 d . . . C30 C 0.4105(2) 0.5297(7) 0.50187(17) 0.0406(12) Uani 1 1 d . . . C31 C 0.4111(2) 0.5317(6) 0.44889(17) 0.0322(10) Uani 1 1 d . . . C32 C 0.6254(2) 0.8787(6) 0.20526(15) 0.0270(9) Uani 1 1 d . . . C33 C 0.6717(2) 0.7496(6) 0.18820(16) 0.0304(9) Uani 1 1 d . . . C34 C 0.7411(2) 0.7878(6) 0.17653(17) 0.0345(10) Uani 1 1 d . . . C35 C 0.7664(2) 0.9586(6) 0.18194(16) 0.0328(10) Uani 1 1 d . . . C36 C 0.7216(2) 1.0918(6) 0.19862(15) 0.0306(10) Uani 1 1 d . . . C37 C 0.6525(2) 1.0500(6) 0.21056(15) 0.0269(9) Uani 1 1 d . . . C38 C 0.4349(2) 0.3837(6) 0.23137(17) 0.0372(10) Uani 1 1 d . . . H38A H 0.4062 0.3134 0.2062 0.056 Uiso 1 1 calc R . . H38B H 0.4330 0.3278 0.2653 0.056 Uiso 1 1 calc R . . H38C H 0.4848 0.3880 0.2212 0.056 Uiso 1 1 calc R . . C39 C 0.4503(5) 0.6693(11) -0.1112(3) 0.119(3) Uani 1 1 d . . . H39A H 0.4034 0.7202 -0.1213 0.179 Uiso 1 1 calc R . . H39B H 0.4467 0.5387 -0.1100 0.179 Uiso 1 1 calc R . . H39C H 0.4852 0.7036 -0.1364 0.179 Uiso 1 1 calc R . . C40 C 0.4742(3) 0.7379(7) -0.0597(2) 0.0504(13) Uani 1 1 d . . . C41 C 0.5472(3) 0.6945(9) -0.0394(3) 0.089(2) Uani 1 1 d . . . H41A H 0.5588 0.7675 -0.0089 0.133 Uiso 1 1 calc R . . H41B H 0.5817 0.7195 -0.0657 0.133 Uiso 1 1 calc R . . H41C H 0.5497 0.5676 -0.0301 0.133 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 0.0187(2) 0.0288(2) 0.0226(2) 0.00004(18) 0.00401(16) -0.00187(17) F1 0.0469(15) 0.0357(15) 0.0368(14) 0.0009(12) -0.0010(12) -0.0052(12) F2 0.0550(18) 0.0567(18) 0.0381(15) -0.0163(14) -0.0004(13) -0.0113(14) F3 0.072(2) 0.083(2) 0.0257(15) 0.0014(15) -0.0091(13) 0.0047(17) F4 0.080(2) 0.0525(19) 0.0375(16) 0.0172(14) 0.0012(14) 0.0115(16) F5 0.0409(14) 0.0336(14) 0.0354(14) -0.0023(11) 0.0084(11) -0.0015(11) F6 0.0356(14) 0.0316(14) 0.0424(15) -0.0033(12) -0.0046(11) 0.0013(11) F7 0.0454(17) 0.076(2) 0.0442(17) -0.0307(16) -0.0022(13) 0.0038(15) F8 0.059(2) 0.135(3) 0.0230(15) 0.0035(18) 0.0051(13) -0.008(2) F9 0.0577(19) 0.077(2) 0.0500(18) 0.0360(17) -0.0035(14) -0.0122(16) F10 0.0571(18) 0.0330(15) 0.0507(17) 0.0038(13) -0.0024(13) -0.0056(13) F11 0.0355(15) 0.0357(15) 0.078(2) -0.0070(14) 0.0118(14) -0.0041(12) F12 0.0340(15) 0.0530(18) 0.077(2) -0.0064(16) 0.0209(14) 0.0099(13) F13 0.0244(14) 0.071(2) 0.0618(18) 0.0011(16) 0.0171(12) -0.0091(13) F14 0.0357(14) 0.0479(16) 0.0460(16) -0.0022(13) 0.0098(12) -0.0151(12) F15 0.0334(14) 0.0385(15) 0.0505(16) -0.0067(13) 0.0119(12) 0.0023(11) O1 0.056(2) 0.128(4) 0.038(2) 0.001(2) 0.0160(18) 0.007(2) N1 0.0182(16) 0.036(2) 0.0247(18) -0.0013(15) 0.0019(13) -0.0037(14) N2 0.0189(16) 0.0318(19) 0.0250(18) 0.0008(15) 0.0042(13) -0.0022(14) N3 0.0202(17) 0.0314(19) 0.0244(18) 0.0001(15) 0.0006(13) -0.0027(14) N4 0.0209(17) 0.0310(19) 0.0222(17) 0.0025(15) 0.0048(13) 0.0002(14) C1 0.019(2) 0.029(2) 0.027(2) 0.0005(17) 0.0032(16) -0.0007(16) C2 0.025(2) 0.034(2) 0.026(2) 0.0028(18) 0.0079(17) -0.0020(17) C3 0.027(2) 0.040(3) 0.023(2) 0.0015(19) 0.0066(17) 0.0010(19) C4 0.031(2) 0.028(2) 0.022(2) 0.0019(18) 0.0052(17) -0.0024(17) C5 0.023(2) 0.033(2) 0.021(2) -0.0002(18) -0.0019(16) -0.0013(17) C6 0.023(2) 0.030(2) 0.026(2) 0.0011(18) 0.0040(16) -0.0025(17) C7 0.022(2) 0.036(2) 0.030(2) -0.0038(19) -0.0022(17) -0.0003(18) C8 0.017(2) 0.032(2) 0.034(2) -0.0026(19) 0.0033(17) -0.0034(17) C9 0.022(2) 0.026(2) 0.030(2) -0.0003(18) 0.0087(16) -0.0033(16) C10 0.022(2) 0.026(2) 0.029(2) -0.0009(18) 0.0042(16) -0.0049(16) C11 0.020(2) 0.031(2) 0.030(2) 0.0004(18) 0.0076(17) -0.0026(17) C12 0.029(2) 0.032(2) 0.025(2) 0.0036(18) 0.0106(17) 0.0012(18) C13 0.026(2) 0.027(2) 0.023(2) 0.0040(17) 0.0019(16) 0.0020(17) C14 0.023(2) 0.026(2) 0.024(2) 0.0002(17) 0.0016(16) 0.0008(16) C15 0.023(2) 0.028(2) 0.025(2) 0.0000(17) 0.0046(16) 0.0001(16) C16 0.028(2) 0.038(2) 0.024(2) -0.0004(19) 0.0000(17) -0.0011(19) C17 0.020(2) 0.039(3) 0.029(2) -0.0008(19) 0.0008(17) -0.0012(17) C18 0.018(2) 0.031(2) 0.029(2) 0.0027(18) 0.0044(16) 0.0024(16) C19 0.019(2) 0.033(2) 0.027(2) 0.0042(18) 0.0052(16) -0.0037(16) C20 0.022(2) 0.036(2) 0.019(2) -0.0027(18) 0.0030(15) 0.0046(17) C21 0.027(2) 0.033(2) 0.027(2) 0.0004(19) 0.0057(17) 0.0015(18) C22 0.031(2) 0.044(3) 0.030(2) -0.011(2) 0.0009(18) -0.005(2) C23 0.036(3) 0.059(3) 0.020(2) 0.002(2) -0.0008(18) 0.006(2) C24 0.038(3) 0.042(3) 0.027(2) 0.008(2) 0.0055(19) 0.008(2) C25 0.023(2) 0.032(2) 0.030(2) -0.0044(19) 0.0084(17) 0.0013(17) C26 0.021(2) 0.036(2) 0.023(2) 0.0042(18) 0.0055(16) 0.0020(17) C27 0.020(2) 0.034(3) 0.036(2) 0.002(2) 0.0034(17) 0.0035(17) C28 0.027(2) 0.053(3) 0.030(2) -0.011(2) 0.0014(18) 0.004(2) C29 0.029(2) 0.082(4) 0.021(2) 0.003(3) 0.0042(18) 0.000(2) C30 0.028(2) 0.060(3) 0.033(3) 0.020(2) 0.0018(19) -0.006(2) C31 0.025(2) 0.035(3) 0.036(2) 0.000(2) 0.0020(18) -0.0021(18) C32 0.022(2) 0.039(2) 0.020(2) 0.0024(18) 0.0023(16) -0.0014(18) C33 0.025(2) 0.033(2) 0.034(2) -0.0006(19) 0.0045(18) -0.0015(18) C34 0.019(2) 0.047(3) 0.038(3) -0.002(2) 0.0065(18) 0.0036(19) C35 0.015(2) 0.053(3) 0.031(2) 0.005(2) 0.0077(17) -0.0037(19) C36 0.030(2) 0.037(3) 0.025(2) 0.0007(19) 0.0002(17) -0.0108(19) C37 0.020(2) 0.035(2) 0.025(2) -0.0025(18) 0.0034(16) 0.0004(17) C38 0.039(3) 0.037(3) 0.036(3) 0.001(2) 0.005(2) 0.002(2) C39 0.196(10) 0.093(6) 0.066(5) -0.026(4) -0.013(6) 0.034(6) C40 0.057(3) 0.054(3) 0.042(3) 0.003(3) 0.021(3) -0.007(3) C41 0.049(4) 0.072(5) 0.146(7) -0.017(5) 0.020(4) -0.006(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 C38 1.923(4) . ? Ge1 N3 1.929(3) . ? Ge1 N2 1.933(3) . ? Ge1 N1 1.939(3) . ? Ge1 N4 1.940(3) . ? F1 C21 1.349(5) . ? F2 C22 1.344(5) . ? F3 C23 1.340(5) . ? F4 C24 1.340(5) . ? F5 C25 1.349(5) . ? F6 C27 1.345(5) . ? F7 C28 1.342(5) . ? F8 C29 1.335(5) . ? F9 C30 1.345(5) . ? F10 C31 1.340(5) . ? F11 C33 1.345(5) . ? F12 C34 1.343(5) . ? F13 C35 1.338(4) . ? F14 C36 1.339(5) . ? F15 C37 1.338(5) . ? O1 C40 1.198(6) . ? N1 C1 1.395(5) . ? N1 C4 1.415(5) . ? N2 C6 1.366(5) . ? N2 C9 1.371(5) . ? N3 C13 1.361(5) . ? N3 C10 1.379(5) . ? N4 C18 1.395(5) . ? N4 C15 1.407(5) . ? C1 C19 1.397(5) . ? C1 C2 1.407(5) . ? C2 C3 1.358(6) . ? C2 H2A 0.9500 . ? C3 C4 1.427(5) . ? C3 H3A 0.9500 . ? C4 C5 1.389(5) . ? C5 C6 1.399(5) . ? C5 C20 1.499(5) . ? C6 C7 1.424(5) . ? C7 C8 1.366(6) . ? C7 H7A 0.9500 . ? C8 C9 1.418(6) . ? C8 H8A 0.9500 . ? C9 C10 1.396(5) . ? C10 C11 1.419(5) . ? C11 C12 1.369(6) . ? C11 H11A 0.9500 . ? C12 C13 1.419(5) . ? C12 H12A 0.9500 . ? C13 C14 1.399(5) . ? C14 C15 1.397(5) . ? C14 C26 1.490(5) . ? C15 C16 1.421(5) . ? C16 C17 1.359(6) . ? C16 H16A 0.9500 . ? C17 C18 1.415(5) . ? C17 H17A 0.9500 . ? C18 C19 1.398(5) . ? C19 C32 1.496(5) . ? C20 C25 1.377(6) . ? C20 C21 1.387(6) . ? C21 C22 1.380(6) . ? C22 C23 1.362(6) . ? C23 C24 1.370(6) . ? C24 C25 1.381(6) . ? C26 C27 1.387(6) . ? C26 C31 1.387(6) . ? C27 C28 1.380(6) . ? C28 C29 1.362(7) . ? C29 C30 1.370(7) . ? C30 C31 1.381(6) . ? C32 C37 1.382(6) . ? C32 C33 1.383(6) . ? C33 C34 1.375(6) . ? C34 C35 1.367(6) . ? C35 C36 1.385(6) . ? C36 C37 1.378(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.484(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.476(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 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 C38 Ge1 N3 106.47(17) . . ? C38 Ge1 N2 107.67(17) . . ? N3 Ge1 N2 78.80(13) . . ? C38 Ge1 N1 105.90(17) . . ? N3 Ge1 N1 147.11(14) . . ? N2 Ge1 N1 86.06(13) . . ? C38 Ge1 N4 104.84(17) . . ? N3 Ge1 N4 86.05(13) . . ? N2 Ge1 N4 146.85(14) . . ? N1 Ge1 N4 91.24(13) . . ? C1 N1 C4 106.8(3) . . ? C1 N1 Ge1 123.7(3) . . ? C4 N1 Ge1 126.9(3) . . ? C6 N2 C9 109.1(3) . . ? C6 N2 Ge1 133.7(3) . . ? C9 N2 Ge1 117.1(3) . . ? C13 N3 C10 109.0(3) . . ? C13 N3 Ge1 133.5(3) . . ? C10 N3 Ge1 117.0(3) . . ? C18 N4 C15 106.6(3) . . ? C18 N4 Ge1 123.9(3) . . ? C15 N4 Ge1 126.1(3) . . ? N1 C1 C19 123.5(3) . . ? N1 C1 C2 108.7(3) . . ? C19 C1 C2 127.8(4) . . ? C3 C2 C1 108.8(4) . . ? C3 C2 H2A 125.6 . . ? C1 C2 H2A 125.6 . . ? C2 C3 C4 108.2(4) . . ? C2 C3 H3A 125.9 . . ? C4 C3 H3A 125.9 . . ? C5 C4 N1 125.2(3) . . ? C5 C4 C3 127.2(4) . . ? N1 C4 C3 107.5(3) . . ? C4 C5 C6 122.1(4) . . ? C4 C5 C20 120.4(4) . . ? C6 C5 C20 117.4(3) . . ? N2 C6 C5 120.7(3) . . ? N2 C6 C7 107.4(3) . . ? C5 C6 C7 131.6(4) . . ? C8 C7 C6 108.2(4) . . ? C8 C7 H7A 125.9 . . ? C6 C7 H7A 125.9 . . ? C7 C8 C9 107.2(3) . . ? C7 C8 H8A 126.4 . . ? C9 C8 H8A 126.4 . . ? N2 C9 C10 112.7(3) . . ? N2 C9 C8 108.1(3) . . ? C10 C9 C8 138.9(4) . . ? N3 C10 C9 112.4(3) . . ? N3 C10 C11 107.9(3) . . ? C9 C10 C11 139.6(4) . . ? C12 C11 C10 107.1(3) . . ? C12 C11 H11A 126.4 . . ? C10 C11 H11A 126.4 . . ? C11 C12 C13 108.3(3) . . ? C11 C12 H12A 125.9 . . ? C13 C12 H12A 125.9 . . ? N3 C13 C14 120.0(3) . . ? N3 C13 C12 107.7(3) . . ? C14 C13 C12 132.0(4) . . ? C15 C14 C13 122.5(4) . . ? C15 C14 C26 121.0(4) . . ? C13 C14 C26 116.5(3) . . ? C14 C15 N4 125.1(4) . . ? C14 C15 C16 126.9(4) . . ? N4 C15 C16 108.0(3) . . ? C17 C16 C15 108.4(4) . . ? C17 C16 H16A 125.8 . . ? C15 C16 H16A 125.8 . . ? C16 C17 C18 108.2(4) . . ? C16 C17 H17A 125.9 . . ? C18 C17 H17A 125.9 . . ? N4 C18 C19 123.3(3) . . ? N4 C18 C17 108.8(3) . . ? C19 C18 C17 127.9(4) . . ? C1 C19 C18 125.0(3) . . ? C1 C19 C32 116.5(3) . . ? C18 C19 C32 118.4(3) . . ? C25 C20 C21 115.5(4) . . ? C25 C20 C5 123.2(4) . . ? C21 C20 C5 121.2(4) . . ? F1 C21 C22 117.2(4) . . ? F1 C21 C20 120.0(4) . . ? C22 C21 C20 122.8(4) . . ? F2 C22 C23 120.4(4) . . ? F2 C22 C21 120.1(4) . . ? C23 C22 C21 119.5(4) . . ? F3 C23 C22 120.0(4) . . ? F3 C23 C24 120.1(4) . . ? C22 C23 C24 119.9(4) . . ? F4 C24 C23 120.2(4) . . ? F4 C24 C25 120.3(4) . . ? C23 C24 C25 119.4(4) . . ? F5 C25 C20 120.2(4) . . ? F5 C25 C24 116.9(4) . . ? C20 C25 C24 122.8(4) . . ? C27 C26 C31 115.5(4) . . ? C27 C26 C14 123.1(4) . . ? C31 C26 C14 121.1(4) . . ? F6 C27 C28 117.7(4) . . ? F6 C27 C26 119.7(4) . . ? C28 C27 C26 122.6(4) . . ? F7 C28 C29 120.7(4) . . ? F7 C28 C27 119.4(4) . . ? C29 C28 C27 120.0(4) . . ? F8 C29 C28 120.4(5) . . ? F8 C29 C30 119.9(5) . . ? C28 C29 C30 119.7(4) . . ? F9 C30 C29 120.5(4) . . ? F9 C30 C31 119.8(5) . . ? C29 C30 C31 119.7(4) . . ? F10 C31 C30 117.6(4) . . ? F10 C31 C26 119.9(4) . . ? C30 C31 C26 122.5(4) . . ? C37 C32 C33 116.6(4) . . ? C37 C32 C19 123.2(4) . . ? C33 C32 C19 120.1(4) . . ? F11 C33 C34 117.8(4) . . ? F11 C33 C32 119.8(4) . . ? C34 C33 C32 122.4(4) . . ? F12 C34 C35 119.7(4) . . ? F12 C34 C33 120.5(4) . . ? C35 C34 C33 119.8(4) . . ? F13 C35 C34 120.7(4) . . ? F13 C35 C36 119.7(4) . . ? C34 C35 C36 119.5(4) . . ? F14 C36 C37 120.4(4) . . ? F14 C36 C35 120.0(4) . . ? C37 C36 C35 119.6(4) . . ? F15 C37 C36 117.8(4) . . ? F15 C37 C32 120.1(3) . . ? C36 C37 C32 122.0(4) . . ? Ge1 C38 H38A 109.5 . . ? Ge1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Ge1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O1 C40 C41 121.6(6) . . ? O1 C40 C39 119.7(6) . . ? C41 C40 C39 118.7(6) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? 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 C38 Ge1 N1 C1 -75.5(3) . . . . ? N3 Ge1 N1 C1 115.0(3) . . . . ? N2 Ge1 N1 C1 177.3(3) . . . . ? N4 Ge1 N1 C1 30.3(3) . . . . ? C38 Ge1 N1 C4 83.6(4) . . . . ? N3 Ge1 N1 C4 -85.9(4) . . . . ? N2 Ge1 N1 C4 -23.6(3) . . . . ? N4 Ge1 N1 C4 -170.5(3) . . . . ? C38 Ge1 N2 C6 -83.1(4) . . . . ? N3 Ge1 N2 C6 173.0(4) . . . . ? N1 Ge1 N2 C6 22.4(4) . . . . ? N4 Ge1 N2 C6 108.6(4) . . . . ? C38 Ge1 N2 C9 91.6(3) . . . . ? N3 Ge1 N2 C9 -12.3(3) . . . . ? N1 Ge1 N2 C9 -163.0(3) . . . . ? N4 Ge1 N2 C9 -76.8(4) . . . . ? C38 Ge1 N3 C13 78.4(4) . . . . ? N2 Ge1 N3 C13 -176.2(4) . . . . ? N1 Ge1 N3 C13 -112.1(4) . . . . ? N4 Ge1 N3 C13 -25.9(4) . . . . ? C38 Ge1 N3 C10 -92.9(3) . . . . ? N2 Ge1 N3 C10 12.4(3) . . . . ? N1 Ge1 N3 C10 76.6(4) . . . . ? N4 Ge1 N3 C10 162.8(3) . . . . ? C38 Ge1 N4 C18 76.7(3) . . . . ? N3 Ge1 N4 C18 -177.3(3) . . . . ? N2 Ge1 N4 C18 -114.8(3) . . . . ? N1 Ge1 N4 C18 -30.1(3) . . . . ? C38 Ge1 N4 C15 -79.7(3) . . . . ? N3 Ge1 N4 C15 26.3(3) . . . . ? N2 Ge1 N4 C15 88.8(4) . . . . ? N1 Ge1 N4 C15 173.5(3) . . . . ? C4 N1 C1 C19 178.6(4) . . . . ? Ge1 N1 C1 C19 -18.7(6) . . . . ? C4 N1 C1 C2 -0.1(4) . . . . ? Ge1 N1 C1 C2 162.6(3) . . . . ? N1 C1 C2 C3 0.3(5) . . . . ? C19 C1 C2 C3 -178.3(4) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C1 N1 C4 C5 -180.0(4) . . . . ? Ge1 N1 C4 C5 18.1(6) . . . . ? C1 N1 C4 C3 -0.2(4) . . . . ? Ge1 N1 C4 C3 -162.2(3) . . . . ? C2 C3 C4 C5 -179.8(4) . . . . ? C2 C3 C4 N1 0.4(5) . . . . ? N1 C4 C5 C6 1.4(7) . . . . ? C3 C4 C5 C6 -178.3(4) . . . . ? N1 C4 C5 C20 178.9(4) . . . . ? C3 C4 C5 C20 -0.8(7) . . . . ? C9 N2 C6 C5 172.9(4) . . . . ? Ge1 N2 C6 C5 -12.2(6) . . . . ? C9 N2 C6 C7 -1.8(5) . . . . ? Ge1 N2 C6 C7 173.2(3) . . . . ? C4 C5 C6 N2 -4.9(6) . . . . ? C20 C5 C6 N2 177.5(4) . . . . ? C4 C5 C6 C7 168.3(4) . . . . ? C20 C5 C6 C7 -9.3(7) . . . . ? N2 C6 C7 C8 1.3(5) . . . . ? C5 C6 C7 C8 -172.5(4) . . . . ? C6 C7 C8 C9 -0.4(5) . . . . ? C6 N2 C9 C10 -173.9(3) . . . . ? Ge1 N2 C9 C10 10.2(5) . . . . ? C6 N2 C9 C8 1.6(5) . . . . ? Ge1 N2 C9 C8 -174.3(3) . . . . ? C7 C8 C9 N2 -0.7(5) . . . . ? C7 C8 C9 C10 173.0(5) . . . . ? C13 N3 C10 C9 176.1(3) . . . . ? Ge1 N3 C10 C9 -10.5(4) . . . . ? C13 N3 C10 C11 -0.8(5) . . . . ? Ge1 N3 C10 C11 172.6(3) . . . . ? N2 C9 C10 N3 0.2(5) . . . . ? C8 C9 C10 N3 -173.3(5) . . . . ? N2 C9 C10 C11 175.7(5) . . . . ? C8 C9 C10 C11 2.2(10) . . . . ? N3 C10 C11 C12 0.6(5) . . . . ? C9 C10 C11 C12 -175.0(5) . . . . ? C10 C11 C12 C13 -0.2(5) . . . . ? C10 N3 C13 C14 -173.5(4) . . . . ? Ge1 N3 C13 C14 14.7(6) . . . . ? C10 N3 C13 C12 0.7(5) . . . . ? Ge1 N3 C13 C12 -171.1(3) . . . . ? C11 C12 C13 N3 -0.3(5) . . . . ? C11 C12 C13 C14 172.9(4) . . . . ? N3 C13 C14 C15 5.1(6) . . . . ? C12 C13 C14 C15 -167.5(4) . . . . ? N3 C13 C14 C26 -177.5(4) . . . . ? C12 C13 C14 C26 9.9(7) . . . . ? C13 C14 C15 N4 -1.8(6) . . . . ? C26 C14 C15 N4 -179.0(4) . . . . ? C13 C14 C15 C16 177.7(4) . . . . ? C26 C14 C15 C16 0.4(7) . . . . ? C18 N4 C15 C14 -179.4(4) . . . . ? Ge1 N4 C15 C14 -19.7(6) . . . . ? C18 N4 C15 C16 1.1(4) . . . . ? Ge1 N4 C15 C16 160.7(3) . . . . ? C14 C15 C16 C17 -180.0(4) . . . . ? N4 C15 C16 C17 -0.4(5) . . . . ? C15 C16 C17 C18 -0.4(5) . . . . ? C15 N4 C18 C19 178.4(4) . . . . ? Ge1 N4 C18 C19 18.1(6) . . . . ? C15 N4 C18 C17 -1.3(4) . . . . ? Ge1 N4 C18 C17 -161.5(3) . . . . ? C16 C17 C18 N4 1.1(5) . . . . ? C16 C17 C18 C19 -178.6(4) . . . . ? N1 C1 C19 C18 -4.8(7) . . . . ? C2 C1 C19 C18 173.6(4) . . . . ? N1 C1 C19 C32 174.0(4) . . . . ? C2 C1 C19 C32 -7.6(6) . . . . ? N4 C18 C19 C1 5.1(7) . . . . ? C17 C18 C19 C1 -175.3(4) . . . . ? N4 C18 C19 C32 -173.6(4) . . . . ? C17 C18 C19 C32 6.0(7) . . . . ? C4 C5 C20 C25 -61.7(6) . . . . ? C6 C5 C20 C25 116.0(4) . . . . ? C4 C5 C20 C21 121.8(4) . . . . ? C6 C5 C20 C21 -60.6(5) . . . . ? C25 C20 C21 F1 -179.9(3) . . . . ? C5 C20 C21 F1 -3.0(6) . . . . ? C25 C20 C21 C22 0.6(6) . . . . ? C5 C20 C21 C22 177.4(4) . . . . ? F1 C21 C22 F2 -0.2(6) . . . . ? C20 C21 C22 F2 179.4(4) . . . . ? F1 C21 C22 C23 179.3(4) . . . . ? C20 C21 C22 C23 -1.1(6) . . . . ? F2 C22 C23 F3 -0.1(7) . . . . ? C21 C22 C23 F3 -179.5(4) . . . . ? F2 C22 C23 C24 -179.4(4) . . . . ? C21 C22 C23 C24 1.1(7) . . . . ? F3 C23 C24 F4 -0.4(7) . . . . ? C22 C23 C24 F4 178.9(4) . . . . ? F3 C23 C24 C25 -179.9(4) . . . . ? C22 C23 C24 C25 -0.6(7) . . . . ? C21 C20 C25 F5 -179.6(3) . . . . ? C5 C20 C25 F5 3.6(6) . . . . ? C21 C20 C25 C24 0.0(6) . . . . ? C5 C20 C25 C24 -176.8(4) . . . . ? F4 C24 C25 F5 0.1(6) . . . . ? C23 C24 C25 F5 179.6(4) . . . . ? F4 C24 C25 C20 -179.5(4) . . . . ? C23 C24 C25 C20 0.0(6) . . . . ? C15 C14 C26 C27 67.2(5) . . . . ? C13 C14 C26 C27 -110.3(4) . . . . ? C15 C14 C26 C31 -119.0(4) . . . . ? C13 C14 C26 C31 63.5(5) . . . . ? C31 C26 C27 F6 179.9(3) . . . . ? C14 C26 C27 F6 -6.0(6) . . . . ? C31 C26 C27 C28 -1.0(6) . . . . ? C14 C26 C27 C28 173.1(4) . . . . ? F6 C27 C28 F7 1.5(6) . . . . ? C26 C27 C28 F7 -177.6(4) . . . . ? F6 C27 C28 C29 179.7(4) . . . . ? C26 C27 C28 C29 0.5(6) . . . . ? F7 C28 C29 F8 -1.8(6) . . . . ? C27 C28 C29 F8 -180.0(4) . . . . ? F7 C28 C29 C30 178.4(4) . . . . ? C27 C28 C29 C30 0.2(7) . . . . ? F8 C29 C30 F9 -0.6(7) . . . . ? C28 C29 C30 F9 179.2(4) . . . . ? F8 C29 C30 C31 179.7(4) . . . . ? C28 C29 C30 C31 -0.4(7) . . . . ? F9 C30 C31 F10 0.0(6) . . . . ? C29 C30 C31 F10 179.7(4) . . . . ? F9 C30 C31 C26 -179.8(4) . . . . ? C29 C30 C31 C26 -0.1(7) . . . . ? C27 C26 C31 F10 -179.0(3) . . . . ? C14 C26 C31 F10 6.8(6) . . . . ? C27 C26 C31 C30 0.8(6) . . . . ? C14 C26 C31 C30 -173.4(4) . . . . ? C1 C19 C32 C37 102.9(5) . . . . ? C18 C19 C32 C37 -78.2(5) . . . . ? C1 C19 C32 C33 -75.1(5) . . . . ? C18 C19 C32 C33 103.8(5) . . . . ? C37 C32 C33 F11 178.5(4) . . . . ? C19 C32 C33 F11 -3.4(6) . . . . ? C37 C32 C33 C34 -0.5(6) . . . . ? C19 C32 C33 C34 177.6(4) . . . . ? F11 C33 C34 F12 -0.4(6) . . . . ? C32 C33 C34 F12 178.7(4) . . . . ? F11 C33 C34 C35 -178.7(4) . . . . ? C32 C33 C34 C35 0.3(7) . . . . ? F12 C34 C35 F13 1.5(7) . . . . ? C33 C34 C35 F13 179.9(4) . . . . ? F12 C34 C35 C36 -179.1(4) . . . . ? C33 C34 C35 C36 -0.7(7) . . . . ? F13 C35 C36 F14 0.3(6) . . . . ? C34 C35 C36 F14 -179.2(4) . . . . ? F13 C35 C36 C37 -179.2(4) . . . . ? C34 C35 C36 C37 1.3(6) . . . . ? F14 C36 C37 F15 -0.1(6) . . . . ? C35 C36 C37 F15 179.4(4) . . . . ? F14 C36 C37 C32 178.9(4) . . . . ? C35 C36 C37 C32 -1.6(6) . . . . ? C33 C32 C37 F15 -179.9(4) . . . . ? C19 C32 C37 F15 2.1(6) . . . . ? C33 C32 C37 C36 1.2(6) . . . . ? C19 C32 C37 C36 -176.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.460 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.073 #===END data_(TPFC)Ge-OCH2CH3 _database_code_depnum_ccdc_archive 'CCDC 839548' #TrackingRef '- Crystal structure data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H13 F15 Ge N4 O' _chemical_formula_sum 'C39 H13 F15 Ge N4 O' _chemical_formula_weight 911.12 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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 31.403(18) _cell_length_b 15.539(9) _cell_length_c 7.241(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3534(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 624 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7834 _exptl_absorpt_correction_T_max 0.9523 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18842 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.17 _reflns_number_total 5856 _reflns_number_gt 5309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 200)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0961P)^2^+8.1887P] 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 0.55(2) _refine_ls_number_reflns 5856 _refine_ls_number_parameters 543 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2040 _refine_ls_wR_factor_gt 0.1987 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 0.56346(2) -0.36816(5) 0.29248(17) 0.0355(2) Uani 1 1 d . . . F1 F 0.66864(17) -0.5815(4) -0.1425(8) 0.0552(15) Uani 1 1 d . . . F2 F 0.71800(18) -0.7192(4) -0.1979(11) 0.0700(16) Uani 1 1 d . . . F3 F 0.7344(2) -0.8325(4) 0.0897(12) 0.082(2) Uani 1 1 d . . . F4 F 0.7000(2) -0.8033(4) 0.4291(12) 0.080(2) Uani 1 1 d . . . F5 F 0.6506(2) -0.6638(4) 0.4895(8) 0.0620(16) Uani 1 1 d . . . F6 F 0.4258(2) -0.1818(4) 0.5252(9) 0.0661(18) Uani 1 1 d . . . F7 F 0.3533(2) -0.0885(4) 0.4859(9) 0.0709(19) Uani 1 1 d . . . F8 F 0.3307(2) -0.0280(4) 0.1541(11) 0.078(2) Uani 1 1 d . . . F9 F 0.3810(3) -0.0574(5) -0.1492(10) 0.089(2) Uani 1 1 d . . . F10 F 0.4529(2) -0.1507(4) -0.1144(9) 0.0668(17) Uani 1 1 d . . . F11 F 0.66893(19) -0.1185(4) 0.4192(9) 0.0586(16) Uani 1 1 d . . . F12 F 0.7345(2) -0.0065(4) 0.3670(9) 0.0701(19) Uani 1 1 d . . . F13 F 0.77169(17) 0.0081(3) 0.0280(10) 0.0586(15) Uani 1 1 d . . . F14 F 0.74038(17) -0.0867(4) -0.2636(8) 0.0549(15) Uani 1 1 d . . . F15 F 0.67597(17) -0.1981(4) -0.2115(10) 0.0674(16) Uani 1 1 d . . . O1 O 0.57031(17) -0.3566(4) 0.5365(11) 0.0458(17) Uani 1 1 d . . . N1 N 0.55701(19) -0.4903(4) 0.2692(13) 0.0374(16) Uani 1 1 d . . . N2 N 0.5024(2) -0.3784(4) 0.2686(13) 0.0363(16) Uani 1 1 d . . . N3 N 0.5581(2) -0.2525(4) 0.1972(10) 0.0362(16) Uani 1 1 d . . . N4 N 0.6201(2) -0.3809(5) 0.1875(12) 0.0432(18) Uani 1 1 d . . . C1 C 0.6277(2) -0.5417(6) 0.2060(13) 0.038(2) Uani 1 1 d . . . C2 C 0.5849(2) -0.5584(5) 0.2484(13) 0.038(2) Uani 1 1 d . . . C3 C 0.5614(3) -0.6366(5) 0.2554(15) 0.044(3) Uani 1 1 d . . . H3A H 0.5729 -0.6931 0.2469 0.053 Uiso 1 1 calc R . . C4 C 0.5185(2) -0.6156(5) 0.2772(17) 0.0425(19) Uani 1 1 d . . . H4A H 0.4955 -0.6546 0.2907 0.051 Uiso 1 1 calc R . . C5 C 0.5160(2) -0.5238(5) 0.2751(14) 0.0336(16) Uani 1 1 d . . . C6 C 0.4849(2) -0.4590(5) 0.2774(15) 0.0395(18) Uani 1 1 d . . . C7 C 0.4403(2) -0.4524(5) 0.2722(15) 0.039(2) Uani 1 1 d . . . H7A H 0.4206 -0.4988 0.2743 0.047 Uiso 1 1 calc R . . C8 C 0.4303(2) -0.3642(6) 0.2634(18) 0.047(3) Uani 1 1 d . . . H8A H 0.4025 -0.3401 0.2635 0.056 Uiso 1 1 calc R . . C9 C 0.4699(2) -0.3169(5) 0.2541(11) 0.0340(19) Uani 1 1 d . . . C10 C 0.4796(2) -0.2305(5) 0.2224(12) 0.039(2) Uani 1 1 d . . . C11 C 0.5207(3) -0.2001(6) 0.1953(14) 0.042(2) Uani 1 1 d . . . C12 C 0.5344(3) -0.1133(6) 0.1558(17) 0.050(3) Uani 1 1 d . . . H12A H 0.5161 -0.0649 0.1442 0.060 Uiso 1 1 calc R . . C13 C 0.5775(3) -0.1112(6) 0.1376(15) 0.045(2) Uani 1 1 d . . . H13A H 0.5942 -0.0614 0.1142 0.054 Uiso 1 1 calc R . . C14 C 0.5933(3) -0.1960(6) 0.1595(14) 0.042(2) Uani 1 1 d . . . C15 C 0.6355(2) -0.2270(5) 0.1403(13) 0.038(2) Uani 1 1 d . . . C16 C 0.6477(2) -0.3124(5) 0.1470(13) 0.0364(19) Uani 1 1 d . . . C17 C 0.6891(3) -0.3471(5) 0.1204(13) 0.038(2) Uani 1 1 d . . . H17A H 0.7141 -0.3145 0.0960 0.046 Uiso 1 1 calc R . . C18 C 0.6873(2) -0.4334(6) 0.1352(13) 0.041(2) Uani 1 1 d . . . H18A H 0.7106 -0.4719 0.1206 0.049 Uiso 1 1 calc R . . C19 C 0.6444(3) -0.4572(6) 0.1769(13) 0.041(2) Uani 1 1 d . . . C20 C 0.6573(3) -0.6174(6) 0.1756(13) 0.038(2) Uani 1 1 d . . . C21 C 0.6755(3) -0.6354(6) 0.0026(14) 0.046(2) Uani 1 1 d . . . C22 C 0.7006(3) -0.7062(6) -0.0295(14) 0.047(2) Uani 1 1 d . . . C23 C 0.7096(3) -0.7622(6) 0.1164(17) 0.053(3) Uani 1 1 d . . . C24 C 0.6924(3) -0.7481(6) 0.282(2) 0.057(2) Uani 1 1 d . . . C25 C 0.6666(3) -0.6761(6) 0.3097(19) 0.056(3) Uani 1 1 d . . . C26 C 0.4420(3) -0.1693(6) 0.2102(14) 0.042(2) Uani 1 1 d . . . C27 C 0.4149(3) -0.1523(6) 0.3591(14) 0.047(2) Uani 1 1 d . . . C28 C 0.3788(3) -0.1021(7) 0.3412(14) 0.051(3) Uani 1 1 d . . . C29 C 0.3667(3) -0.0726(6) 0.1703(16) 0.049(2) Uani 1 1 d . . . C30 C 0.3920(4) -0.0889(6) 0.0182(16) 0.055(3) Uani 1 1 d . . . C31 C 0.4292(3) -0.1361(6) 0.0411(18) 0.052(3) Uani 1 1 d . . . C32 C 0.6698(3) -0.1610(6) 0.1098(14) 0.037(2) Uani 1 1 d . . . C33 C 0.6854(3) -0.1107(5) 0.2486(12) 0.038(2) Uani 1 1 d . . . C34 C 0.7198(3) -0.0514(6) 0.2245(15) 0.051(3) Uani 1 1 d . . . C35 C 0.7385(3) -0.0465(5) 0.0539(16) 0.047(2) Uani 1 1 d . . . C36 C 0.7229(3) -0.0934(6) -0.0964(14) 0.045(2) Uani 1 1 d . . . C37 C 0.6894(3) -0.1501(6) -0.0661(16) 0.048(2) Uani 1 1 d . . . C38 C 0.6005(4) -0.2961(8) 0.6136(16) 0.065(3) Uani 1 1 d . . . H38A H 0.6237 -0.2846 0.5243 0.078 Uiso 1 1 calc R . . H38B H 0.6132 -0.3196 0.7281 0.078 Uiso 1 1 calc R . . C39 C 0.5744(4) -0.2079(9) 0.658(2) 0.088(4) Uani 1 1 d . . . H39A H 0.5943 -0.1637 0.7016 0.132 Uiso 1 1 calc R . . H39B H 0.5531 -0.2192 0.7538 0.132 Uiso 1 1 calc R . . H39C H 0.5602 -0.1878 0.5456 0.132 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 0.0243(3) 0.0387(4) 0.0436(5) -0.0006(5) -0.0018(4) -0.0042(3) F1 0.043(3) 0.063(3) 0.059(4) -0.001(3) 0.002(2) 0.004(3) F2 0.063(3) 0.075(4) 0.072(4) -0.013(4) 0.013(4) 0.013(3) F3 0.059(4) 0.049(3) 0.139(7) -0.014(4) 0.006(4) 0.019(3) F4 0.075(4) 0.065(4) 0.100(5) 0.023(4) -0.002(4) 0.021(3) F5 0.065(4) 0.074(4) 0.047(4) 0.015(3) 0.005(3) 0.019(3) F6 0.064(4) 0.082(5) 0.052(4) 0.013(3) 0.009(3) 0.030(3) F7 0.066(4) 0.078(4) 0.069(5) 0.015(3) 0.021(3) 0.027(3) F8 0.061(4) 0.077(4) 0.095(5) 0.005(4) 0.001(4) 0.035(4) F9 0.102(5) 0.088(5) 0.075(6) 0.022(4) -0.015(4) 0.030(4) F10 0.072(4) 0.076(4) 0.052(4) 0.002(3) 0.015(3) 0.018(3) F11 0.056(3) 0.068(4) 0.052(4) -0.008(3) 0.007(3) -0.021(3) F12 0.073(4) 0.077(4) 0.061(4) -0.006(3) -0.005(3) -0.037(3) F13 0.040(3) 0.049(3) 0.087(4) 0.003(3) 0.008(3) -0.017(2) F14 0.047(3) 0.065(3) 0.052(4) 0.003(3) 0.013(3) -0.008(3) F15 0.065(3) 0.084(4) 0.053(3) -0.006(4) 0.009(4) -0.030(3) O1 0.023(3) 0.039(3) 0.075(5) -0.005(3) -0.007(3) -0.006(2) N1 0.035(3) 0.034(3) 0.043(5) 0.002(4) -0.005(4) -0.002(2) N2 0.035(3) 0.032(3) 0.042(5) 0.001(3) 0.000(3) -0.003(2) N3 0.023(3) 0.036(4) 0.049(4) -0.002(3) 0.003(3) -0.010(3) N4 0.037(4) 0.039(4) 0.054(5) 0.006(4) -0.006(4) -0.001(3) C1 0.027(4) 0.040(4) 0.048(5) -0.001(4) -0.006(4) 0.007(3) C2 0.029(4) 0.030(4) 0.054(7) -0.002(4) 0.003(4) 0.009(3) C3 0.038(4) 0.035(4) 0.059(9) 0.006(4) -0.003(4) -0.002(3) C4 0.038(4) 0.042(4) 0.048(5) -0.004(5) 0.005(5) -0.007(3) C5 0.027(3) 0.044(4) 0.030(4) 0.002(4) -0.003(4) -0.003(3) C6 0.031(4) 0.046(4) 0.042(5) 0.001(5) -0.002(4) -0.002(3) C7 0.027(3) 0.048(4) 0.042(6) -0.001(5) 0.004(4) 0.000(3) C8 0.022(3) 0.058(5) 0.060(8) 0.007(5) -0.001(4) -0.001(3) C9 0.021(3) 0.051(4) 0.030(5) -0.005(4) 0.000(3) -0.001(3) C10 0.022(3) 0.043(4) 0.051(6) 0.003(4) 0.007(3) 0.002(3) C11 0.028(4) 0.038(5) 0.059(6) 0.004(4) 0.001(4) 0.003(3) C12 0.033(4) 0.030(4) 0.088(8) 0.002(5) 0.003(5) 0.008(3) C13 0.032(4) 0.037(4) 0.067(7) 0.001(4) 0.001(4) -0.008(4) C14 0.025(4) 0.040(5) 0.063(6) 0.000(4) 0.002(4) -0.002(3) C15 0.020(4) 0.042(5) 0.052(6) 0.002(4) -0.003(3) -0.007(3) C16 0.018(4) 0.046(5) 0.045(5) 0.009(4) -0.001(3) -0.008(3) C17 0.028(4) 0.031(4) 0.056(6) 0.012(4) 0.006(4) 0.002(3) C18 0.018(4) 0.052(5) 0.051(6) 0.007(4) 0.006(3) 0.004(3) C19 0.030(4) 0.046(5) 0.046(6) 0.005(4) -0.006(4) -0.007(4) C20 0.026(4) 0.044(5) 0.045(6) 0.000(4) 0.001(4) 0.001(3) C21 0.034(5) 0.051(5) 0.052(6) 0.010(5) -0.011(4) 0.008(4) C22 0.034(4) 0.059(6) 0.049(6) -0.001(5) 0.005(4) -0.002(4) C23 0.028(4) 0.039(5) 0.092(9) -0.012(5) -0.004(5) 0.010(4) C24 0.044(5) 0.047(5) 0.078(7) 0.019(6) 0.003(6) 0.003(4) C25 0.031(4) 0.055(5) 0.081(8) 0.007(6) 0.007(6) 0.004(4) C26 0.036(4) 0.036(5) 0.053(6) 0.008(4) 0.000(4) -0.005(4) C27 0.039(5) 0.045(5) 0.056(7) 0.006(4) 0.007(4) 0.014(4) C28 0.046(5) 0.059(6) 0.046(7) -0.002(5) 0.016(4) 0.016(4) C29 0.034(5) 0.045(5) 0.067(8) -0.010(5) -0.005(5) 0.010(4) C30 0.068(7) 0.038(5) 0.059(7) 0.010(5) -0.009(6) 0.002(5) C31 0.040(5) 0.040(5) 0.077(8) -0.002(5) 0.017(5) 0.001(4) C32 0.029(4) 0.031(4) 0.052(6) 0.000(4) 0.004(4) -0.012(3) C33 0.032(4) 0.046(5) 0.036(6) 0.003(4) 0.003(3) -0.007(3) C34 0.048(5) 0.042(5) 0.063(7) -0.015(4) -0.007(5) 0.001(4) C35 0.028(4) 0.033(4) 0.081(8) 0.001(5) 0.004(5) -0.004(3) C36 0.029(4) 0.057(5) 0.049(6) 0.016(5) 0.017(4) 0.000(4) C37 0.041(5) 0.039(5) 0.064(7) 0.002(5) -0.005(5) -0.017(4) C38 0.063(7) 0.083(8) 0.048(6) -0.009(6) 0.001(5) -0.034(6) C39 0.078(9) 0.081(9) 0.104(12) -0.017(8) -0.016(8) -0.016(7) _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 O1 1.789(8) . ? Ge1 N1 1.917(7) . ? Ge1 N2 1.932(6) . ? Ge1 N3 1.933(7) . ? Ge1 N4 1.945(8) . ? F1 C21 1.360(11) . ? F2 C22 1.351(11) . ? F3 C23 1.355(10) . ? F4 C24 1.388(14) . ? F5 C25 1.410(14) . ? F6 C27 1.332(11) . ? F7 C28 1.336(10) . ? F8 C29 1.332(11) . ? F9 C30 1.352(13) . ? F10 C31 1.370(13) . ? F11 C33 1.344(11) . ? F12 C34 1.329(11) . ? F13 C35 1.355(9) . ? F14 C36 1.334(11) . ? F15 C37 1.358(12) . ? O1 C38 1.446(11) . ? N1 C2 1.381(9) . ? N1 C5 1.388(9) . ? N2 C6 1.368(10) . ? N2 C9 1.402(10) . ? N3 C11 1.430(11) . ? N3 C14 1.438(10) . ? N4 C16 1.404(11) . ? N4 C19 1.412(11) . ? C1 C2 1.402(11) . ? C1 C19 1.429(12) . ? C1 C20 1.517(11) . ? C2 C3 1.422(11) . ? C3 C4 1.394(11) . ? C3 H3A 0.9500 . ? C4 C5 1.429(11) . ? C4 H4A 0.9500 . ? C5 C6 1.402(10) . ? C6 C7 1.406(10) . ? C7 C8 1.407(12) . ? C7 H7A 0.9500 . ? C8 C9 1.446(11) . ? C8 H8A 0.9500 . ? C9 C10 1.395(12) . ? C10 C11 1.388(11) . ? C10 C26 1.517(12) . ? C11 C12 1.445(12) . ? C12 C13 1.361(13) . ? C12 H12A 0.9500 . ? C13 C14 1.417(12) . ? C13 H13A 0.9500 . ? C14 C15 1.417(11) . ? C15 C16 1.382(12) . ? C15 C32 1.503(11) . ? C16 C17 1.420(11) . ? C17 C18 1.348(12) . ? C17 H17A 0.9500 . ? C18 C19 1.431(11) . ? C18 H18A 0.9500 . ? C20 C25 1.363(14) . ? C20 C21 1.404(14) . ? C21 C22 1.375(13) . ? C22 C23 1.398(15) . ? C23 C24 1.334(18) . ? C24 C25 1.395(13) . ? C26 C31 1.389(15) . ? C26 C27 1.399(13) . ? C27 C28 1.382(13) . ? C28 C29 1.373(15) . ? C29 C30 1.380(15) . ? C30 C31 1.390(14) . ? C32 C33 1.363(13) . ? C32 C37 1.425(14) . ? C33 C34 1.432(13) . ? C34 C35 1.370(14) . ? C35 C36 1.399(15) . ? C36 C37 1.388(12) . ? C38 C39 1.628(19) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 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 O1 Ge1 N1 101.5(3) . . ? O1 Ge1 N2 102.5(3) . . ? N1 Ge1 N2 78.8(3) . . ? O1 Ge1 N3 105.6(3) . . ? N1 Ge1 N3 151.7(3) . . ? N2 Ge1 N3 87.6(3) . . ? O1 Ge1 N4 106.6(3) . . ? N1 Ge1 N4 87.8(3) . . ? N2 Ge1 N4 149.9(3) . . ? N3 Ge1 N4 92.0(3) . . ? C38 O1 Ge1 121.7(6) . . ? C2 N1 C5 107.7(6) . . ? C2 N1 Ge1 134.5(5) . . ? C5 N1 Ge1 117.8(5) . . ? C6 N2 C9 109.6(6) . . ? C6 N2 Ge1 117.9(5) . . ? C9 N2 Ge1 132.3(5) . . ? C11 N3 C14 106.5(7) . . ? C11 N3 Ge1 127.2(5) . . ? C14 N3 Ge1 124.6(5) . . ? C16 N4 C19 107.0(7) . . ? C16 N4 Ge1 124.8(6) . . ? C19 N4 Ge1 126.9(6) . . ? C2 C1 C19 123.7(8) . . ? C2 C1 C20 118.4(7) . . ? C19 C1 C20 117.7(7) . . ? N1 C2 C1 119.3(7) . . ? N1 C2 C3 108.8(7) . . ? C1 C2 C3 131.5(7) . . ? C4 C3 C2 107.7(7) . . ? C4 C3 H3A 126.2 . . ? C2 C3 H3A 126.2 . . ? C3 C4 C5 106.6(7) . . ? C3 C4 H4A 126.7 . . ? C5 C4 H4A 126.7 . . ? N1 C5 C6 112.1(6) . . ? N1 C5 C4 108.8(6) . . ? C6 C5 C4 139.0(7) . . ? N2 C6 C5 112.2(6) . . ? N2 C6 C7 109.4(7) . . ? C5 C6 C7 138.2(7) . . ? C6 C7 C8 107.1(7) . . ? C6 C7 H7A 126.4 . . ? C8 C7 H7A 126.4 . . ? C7 C8 C9 107.8(7) . . ? C7 C8 H8A 126.1 . . ? C9 C8 H8A 126.1 . . ? C10 C9 N2 120.6(7) . . ? C10 C9 C8 133.2(7) . . ? N2 C9 C8 106.0(7) . . ? C11 C10 C9 123.6(7) . . ? C11 C10 C26 120.1(8) . . ? C9 C10 C26 116.3(7) . . ? C10 C11 N3 124.7(8) . . ? C10 C11 C12 128.5(8) . . ? N3 C11 C12 106.7(7) . . ? C13 C12 C11 109.7(7) . . ? C13 C12 H12A 125.1 . . ? C11 C12 H12A 125.1 . . ? C12 C13 C14 108.4(8) . . ? C12 C13 H13A 125.8 . . ? C14 C13 H13A 125.8 . . ? C13 C14 C15 129.3(8) . . ? C13 C14 N3 108.6(7) . . ? C15 C14 N3 122.0(7) . . ? C16 C15 C14 125.6(7) . . ? C16 C15 C32 117.5(7) . . ? C14 C15 C32 116.9(8) . . ? C15 C16 N4 124.3(7) . . ? C15 C16 C17 127.8(7) . . ? N4 C16 C17 107.9(7) . . ? C18 C17 C16 109.2(7) . . ? C18 C17 H17A 125.4 . . ? C16 C17 H17A 125.4 . . ? C17 C18 C19 108.3(7) . . ? C17 C18 H18A 125.9 . . ? C19 C18 H18A 125.9 . . ? N4 C19 C1 124.4(7) . . ? N4 C19 C18 107.7(7) . . ? C1 C19 C18 127.9(8) . . ? C25 C20 C21 114.6(8) . . ? C25 C20 C1 123.2(9) . . ? C21 C20 C1 122.2(8) . . ? F1 C21 C22 116.9(9) . . ? F1 C21 C20 120.2(8) . . ? C22 C21 C20 122.9(9) . . ? F2 C22 C21 120.3(9) . . ? F2 C22 C23 120.5(9) . . ? C21 C22 C23 119.1(9) . . ? C24 C23 F3 119.6(10) . . ? C24 C23 C22 119.7(8) . . ? F3 C23 C22 120.6(10) . . ? C23 C24 F4 121.2(9) . . ? C23 C24 C25 119.7(11) . . ? F4 C24 C25 119.0(13) . . ? C20 C25 C24 123.9(12) . . ? C20 C25 F5 119.4(8) . . ? C24 C25 F5 116.7(11) . . ? C31 C26 C27 115.6(8) . . ? C31 C26 C10 120.6(9) . . ? C27 C26 C10 123.1(8) . . ? F6 C27 C28 119.3(8) . . ? F6 C27 C26 118.4(8) . . ? C28 C27 C26 122.2(9) . . ? F7 C28 C29 119.2(8) . . ? F7 C28 C27 120.5(9) . . ? C29 C28 C27 120.0(8) . . ? F8 C29 C28 119.2(9) . . ? F8 C29 C30 120.8(10) . . ? C28 C29 C30 120.0(8) . . ? F9 C30 C29 120.2(9) . . ? F9 C30 C31 120.8(10) . . ? C29 C30 C31 119.0(10) . . ? F10 C31 C26 120.3(9) . . ? F10 C31 C30 116.6(11) . . ? C26 C31 C30 123.1(10) . . ? C33 C32 C37 115.8(7) . . ? C33 C32 C15 122.6(8) . . ? C37 C32 C15 121.5(8) . . ? F11 C33 C32 119.2(7) . . ? F11 C33 C34 117.4(8) . . ? C32 C33 C34 123.3(8) . . ? F12 C34 C35 121.4(9) . . ? F12 C34 C33 120.4(9) . . ? C35 C34 C33 118.1(8) . . ? F13 C35 C34 119.3(9) . . ? F13 C35 C36 119.2(9) . . ? C34 C35 C36 121.4(8) . . ? F14 C36 C37 120.3(10) . . ? F14 C36 C35 121.3(8) . . ? C37 C36 C35 118.3(9) . . ? F15 C37 C36 117.5(10) . . ? F15 C37 C32 119.5(7) . . ? C36 C37 C32 122.9(9) . . ? O1 C38 C39 107.1(9) . . ? O1 C38 H38A 110.3 . . ? C39 C38 H38A 110.3 . . ? O1 C38 H38B 110.3 . . ? C39 C38 H38B 110.3 . . ? H38A C38 H38B 108.6 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? 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 N1 Ge1 O1 C38 140.3(8) . . . . ? N2 Ge1 O1 C38 -138.7(8) . . . . ? N3 Ge1 O1 C38 -47.7(8) . . . . ? N4 Ge1 O1 C38 49.2(8) . . . . ? O1 Ge1 N1 C2 -87.5(10) . . . . ? N2 Ge1 N1 C2 171.9(10) . . . . ? N3 Ge1 N1 C2 109.1(9) . . . . ? N4 Ge1 N1 C2 19.0(10) . . . . ? O1 Ge1 N1 C5 91.7(7) . . . . ? N2 Ge1 N1 C5 -8.9(7) . . . . ? N3 Ge1 N1 C5 -71.7(10) . . . . ? N4 Ge1 N1 C5 -161.8(8) . . . . ? O1 Ge1 N2 C6 -89.5(8) . . . . ? N1 Ge1 N2 C6 9.9(8) . . . . ? N3 Ge1 N2 C6 165.0(8) . . . . ? N4 Ge1 N2 C6 75.1(10) . . . . ? O1 Ge1 N2 C9 85.8(9) . . . . ? N1 Ge1 N2 C9 -174.7(9) . . . . ? N3 Ge1 N2 C9 -19.6(9) . . . . ? N4 Ge1 N2 C9 -109.5(9) . . . . ? O1 Ge1 N3 C11 -81.6(8) . . . . ? N1 Ge1 N3 C11 81.4(10) . . . . ? N2 Ge1 N3 C11 20.7(8) . . . . ? N4 Ge1 N3 C11 170.5(8) . . . . ? O1 Ge1 N3 C14 81.3(8) . . . . ? N1 Ge1 N3 C14 -115.6(8) . . . . ? N2 Ge1 N3 C14 -176.4(8) . . . . ? N4 Ge1 N3 C14 -26.6(8) . . . . ? O1 Ge1 N4 C16 -82.2(8) . . . . ? N1 Ge1 N4 C16 176.5(8) . . . . ? N2 Ge1 N4 C16 113.5(8) . . . . ? N3 Ge1 N4 C16 24.8(8) . . . . ? O1 Ge1 N4 C19 82.6(8) . . . . ? N1 Ge1 N4 C19 -18.7(8) . . . . ? N2 Ge1 N4 C19 -81.7(10) . . . . ? N3 Ge1 N4 C19 -170.4(8) . . . . ? C5 N1 C2 C1 168.9(9) . . . . ? Ge1 N1 C2 C1 -11.9(15) . . . . ? C5 N1 C2 C3 -4.5(11) . . . . ? Ge1 N1 C2 C3 174.8(8) . . . . ? C19 C1 C2 N1 -2.0(14) . . . . ? C20 C1 C2 N1 -177.5(8) . . . . ? C19 C1 C2 C3 169.6(10) . . . . ? C20 C1 C2 C3 -5.9(16) . . . . ? N1 C2 C3 C4 1.2(12) . . . . ? C1 C2 C3 C4 -171.1(10) . . . . ? C2 C3 C4 C5 2.5(12) . . . . ? C2 N1 C5 C6 -174.0(9) . . . . ? Ge1 N1 C5 C6 6.6(12) . . . . ? C2 N1 C5 C4 6.1(11) . . . . ? Ge1 N1 C5 C4 -173.3(7) . . . . ? C3 C4 C5 N1 -5.3(12) . . . . ? C3 C4 C5 C6 174.8(13) . . . . ? C9 N2 C6 C5 174.6(8) . . . . ? Ge1 N2 C6 C5 -9.1(12) . . . . ? C9 N2 C6 C7 -1.1(12) . . . . ? Ge1 N2 C6 C7 175.3(7) . . . . ? N1 C5 C6 N2 1.5(13) . . . . ? C4 C5 C6 N2 -178.5(13) . . . . ? N1 C5 C6 C7 175.3(12) . . . . ? C4 C5 C6 C7 -5(2) . . . . ? N2 C6 C7 C8 -1.1(12) . . . . ? C5 C6 C7 C8 -175.0(13) . . . . ? C6 C7 C8 C9 2.8(13) . . . . ? C6 N2 C9 C10 -172.8(9) . . . . ? Ge1 N2 C9 C10 11.5(13) . . . . ? C6 N2 C9 C8 2.7(11) . . . . ? Ge1 N2 C9 C8 -173.0(8) . . . . ? C7 C8 C9 C10 171.4(10) . . . . ? C7 C8 C9 N2 -3.4(12) . . . . ? N2 C9 C10 C11 2.9(14) . . . . ? C8 C9 C10 C11 -171.2(11) . . . . ? N2 C9 C10 C26 -179.6(8) . . . . ? C8 C9 C10 C26 6.3(16) . . . . ? C9 C10 C11 N3 -0.3(15) . . . . ? C26 C10 C11 N3 -177.7(9) . . . . ? C9 C10 C11 C12 177.9(10) . . . . ? C26 C10 C11 C12 0.5(16) . . . . ? C14 N3 C11 C10 178.7(9) . . . . ? Ge1 N3 C11 C10 -15.9(14) . . . . ? C14 N3 C11 C12 0.2(11) . . . . ? Ge1 N3 C11 C12 165.6(7) . . . . ? C10 C11 C12 C13 -179.5(10) . . . . ? N3 C11 C12 C13 -1.1(12) . . . . ? C11 C12 C13 C14 1.5(13) . . . . ? C12 C13 C14 C15 175.3(10) . . . . ? C12 C13 C14 N3 -1.3(12) . . . . ? C11 N3 C14 C13 0.7(11) . . . . ? Ge1 N3 C14 C13 -165.2(7) . . . . ? C11 N3 C14 C15 -176.3(9) . . . . ? Ge1 N3 C14 C15 17.8(13) . . . . ? C13 C14 C15 C16 -173.5(10) . . . . ? N3 C14 C15 C16 2.8(16) . . . . ? C13 C14 C15 C32 6.5(16) . . . . ? N3 C14 C15 C32 -177.3(8) . . . . ? C14 C15 C16 N4 -4.8(16) . . . . ? C32 C15 C16 N4 175.2(9) . . . . ? C14 C15 C16 C17 176.9(10) . . . . ? C32 C15 C16 C17 -3.1(15) . . . . ? C19 N4 C16 C15 178.7(9) . . . . ? Ge1 N4 C16 C15 -13.9(13) . . . . ? C19 N4 C16 C17 -2.7(10) . . . . ? Ge1 N4 C16 C17 164.7(7) . . . . ? C15 C16 C17 C18 -178.9(10) . . . . ? N4 C16 C17 C18 2.6(11) . . . . ? C16 C17 C18 C19 -1.4(11) . . . . ? C16 N4 C19 C1 -178.9(9) . . . . ? Ge1 N4 C19 C1 14.1(13) . . . . ? C16 N4 C19 C18 1.8(10) . . . . ? Ge1 N4 C19 C18 -165.1(7) . . . . ? C2 C1 C19 N4 0.2(15) . . . . ? C20 C1 C19 N4 175.6(9) . . . . ? C2 C1 C19 C18 179.3(9) . . . . ? C20 C1 C19 C18 -5.3(14) . . . . ? C17 C18 C19 N4 -0.3(11) . . . . ? C17 C18 C19 C1 -179.5(10) . . . . ? C2 C1 C20 C25 -62.9(13) . . . . ? C19 C1 C20 C25 121.4(10) . . . . ? C2 C1 C20 C21 113.2(10) . . . . ? C19 C1 C20 C21 -62.5(12) . . . . ? C25 C20 C21 F1 -179.9(8) . . . . ? C1 C20 C21 F1 3.8(13) . . . . ? C25 C20 C21 C22 -0.1(13) . . . . ? C1 C20 C21 C22 -176.5(8) . . . . ? F1 C21 C22 F2 1.2(13) . . . . ? C20 C21 C22 F2 -178.5(8) . . . . ? F1 C21 C22 C23 178.1(8) . . . . ? C20 C21 C22 C23 -1.6(14) . . . . ? F2 C22 C23 C24 179.6(9) . . . . ? C21 C22 C23 C24 2.7(15) . . . . ? F2 C22 C23 F3 -3.0(14) . . . . ? C21 C22 C23 F3 -179.9(9) . . . . ? F3 C23 C24 F4 1.3(15) . . . . ? C22 C23 C24 F4 178.8(8) . . . . ? F3 C23 C24 C25 -179.5(9) . . . . ? C22 C23 C24 C25 -2.0(15) . . . . ? C21 C20 C25 C24 0.9(14) . . . . ? C1 C20 C25 C24 177.2(9) . . . . ? C21 C20 C25 F5 179.1(8) . . . . ? C1 C20 C25 F5 -4.6(14) . . . . ? C23 C24 C25 C20 0.2(15) . . . . ? F4 C24 C25 C20 179.4(9) . . . . ? C23 C24 C25 F5 -178.1(9) . . . . ? F4 C24 C25 F5 1.2(13) . . . . ? C11 C10 C26 C31 71.5(12) . . . . ? C9 C10 C26 C31 -106.0(10) . . . . ? C11 C10 C26 C27 -117.7(11) . . . . ? C9 C10 C26 C27 64.8(12) . . . . ? C31 C26 C27 F6 -179.4(9) . . . . ? C10 C26 C27 F6 9.4(14) . . . . ? C31 C26 C27 C28 -3.1(15) . . . . ? C10 C26 C27 C28 -174.3(9) . . . . ? F6 C27 C28 F7 -5.0(16) . . . . ? C26 C27 C28 F7 178.8(9) . . . . ? F6 C27 C28 C29 -178.7(9) . . . . ? C26 C27 C28 C29 5.1(16) . . . . ? F7 C28 C29 F8 2.8(15) . . . . ? C27 C28 C29 F8 176.7(9) . . . . ? F7 C28 C29 C30 -177.6(9) . . . . ? C27 C28 C29 C30 -3.8(16) . . . . ? F8 C29 C30 F9 1.9(15) . . . . ? C28 C29 C30 F9 -177.7(10) . . . . ? F8 C29 C30 C31 -179.7(9) . . . . ? C28 C29 C30 C31 0.8(16) . . . . ? C27 C26 C31 F10 -178.5(9) . . . . ? C10 C26 C31 F10 -7.0(14) . . . . ? C27 C26 C31 C30 0.0(14) . . . . ? C10 C26 C31 C30 171.5(9) . . . . ? F9 C30 C31 F10 -1.9(15) . . . . ? C29 C30 C31 F10 179.7(9) . . . . ? F9 C30 C31 C26 179.5(9) . . . . ? C29 C30 C31 C26 1.1(15) . . . . ? C16 C15 C32 C33 -103.6(11) . . . . ? C14 C15 C32 C33 76.4(12) . . . . ? C16 C15 C32 C37 73.5(12) . . . . ? C14 C15 C32 C37 -106.4(11) . . . . ? C37 C32 C33 F11 -178.9(8) . . . . ? C15 C32 C33 F11 -1.6(13) . . . . ? C37 C32 C33 C34 -1.3(14) . . . . ? C15 C32 C33 C34 176.0(8) . . . . ? F11 C33 C34 F12 0.1(13) . . . . ? C32 C33 C34 F12 -177.6(9) . . . . ? F11 C33 C34 C35 176.3(8) . . . . ? C32 C33 C34 C35 -1.4(14) . . . . ? F12 C34 C35 F13 -2.7(14) . . . . ? C33 C34 C35 F13 -178.9(8) . . . . ? F12 C34 C35 C36 -179.5(9) . . . . ? C33 C34 C35 C36 4.3(14) . . . . ? F13 C35 C36 F14 1.3(13) . . . . ? C34 C35 C36 F14 178.1(9) . . . . ? F13 C35 C36 C37 178.8(8) . . . . ? C34 C35 C36 C37 -4.4(14) . . . . ? F14 C36 C37 F15 0.6(14) . . . . ? C35 C36 C37 F15 -176.9(8) . . . . ? F14 C36 C37 C32 179.0(8) . . . . ? C35 C36 C37 C32 1.5(15) . . . . ? C33 C32 C37 F15 179.7(8) . . . . ? C15 C32 C37 F15 2.3(14) . . . . ? C33 C32 C37 C36 1.2(14) . . . . ? C15 C32 C37 C36 -176.1(9) . . . . ? Ge1 O1 C38 C39 94.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.809 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.111 #===END data_(TPFC)Ge-CH2CH2COOCH3 _database_code_depnum_ccdc_archive 'CCDC 839549' #TrackingRef '- Crystal structure data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H15 F15 Ge N4 O2' _chemical_formula_sum 'C41 H15 F15 Ge N4 O2' _chemical_formula_weight 953.16 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' 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' 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' _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 8.5832(15) _cell_length_b 19.679(4) _cell_length_c 25.475(5) _cell_angle_alpha 105.640(5) _cell_angle_beta 96.460(7) _cell_angle_gamma 100.770(7) _cell_volume 4009.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 489 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8654 _exptl_absorpt_correction_T_max 0.9022 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39408 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.33 _reflns_number_total 14587 _reflns_number_gt 12925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 200)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.1406P)^2^+9.9634P] 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 14587 _refine_ls_number_parameters 1200 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.2669 _refine_ls_wR_factor_gt 0.2585 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.002 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 1.01224(7) 0.90384(3) 0.10254(3) 0.0422(2) Uani 1 1 d . B . Ge2 Ge 0.53071(7) 0.61340(3) 0.41108(2) 0.04001(19) Uani 1 1 d . D . O1 O 1.3642(7) 0.9342(4) 0.2696(2) 0.0805(16) Uani 1 1 d . B . O3 O 0.8967(7) 0.8227(3) 0.4004(3) 0.0896(19) Uani 1 1 d D . . N1 N 0.8075(6) 0.8799(3) 0.1265(2) 0.0454(11) Uani 1 1 d . . . N2 N 0.9811(6) 0.8062(3) 0.0543(2) 0.0477(12) Uani 1 1 d . . . N3 N 1.1273(6) 0.9347(3) 0.0494(2) 0.0432(11) Uani 1 1 d . . . N4 N 0.9733(6) 1.0000(3) 0.1126(2) 0.0446(11) Uani 1 1 d . . . N5 N 0.5032(6) 0.5385(3) 0.3416(2) 0.0444(11) Uani 1 1 d . . . N6 N 0.3309(6) 0.6374(3) 0.3887(2) 0.0469(11) Uani 1 1 d . . . N7 N 0.4862(6) 0.6408(3) 0.4856(2) 0.0451(11) Uani 1 1 d . . . N8 N 0.6404(6) 0.5537(3) 0.4438(2) 0.0429(11) Uani 1 1 d . . . C1 C 0.7740(7) 1.0041(4) 0.1710(3) 0.0491(14) Uani 1 1 d . . . C2 C 0.7369(7) 0.9292(3) 0.1606(3) 0.0483(14) Uani 1 1 d . . . C3 C 0.6126(8) 0.8885(4) 0.1803(3) 0.0571(16) Uani 1 1 d . . . H3A H 0.5436 0.9077 0.2041 0.069 Uiso 1 1 calc R . . C4 C 0.6116(8) 0.8173(4) 0.1586(3) 0.0599(17) Uani 1 1 d . . . H4A H 0.5415 0.7780 0.1651 0.072 Uiso 1 1 calc R . . C5 C 0.7312(8) 0.8109(4) 0.1251(3) 0.0545(15) Uani 1 1 d . . . C6 C 0.7708(8) 0.7485(4) 0.0953(3) 0.0598(17) Uani 1 1 d . . . C7 C 0.8840(8) 0.7462(3) 0.0620(3) 0.0534(15) Uani 1 1 d . . . C8 C 0.9271(9) 0.6822(4) 0.0277(3) 0.0643(19) Uani 1 1 d . . . H8A H 0.8798 0.6332 0.0241 0.077 Uiso 1 1 calc R . . C9 C 1.0457(9) 0.7055(4) 0.0023(3) 0.0575(16) Uani 1 1 d . . . H9A H 1.0976 0.6751 -0.0221 0.069 Uiso 1 1 calc R . . C10 C 1.0816(8) 0.7819(3) 0.0171(3) 0.0499(14) Uani 1 1 d . . . C11 C 1.1936(7) 0.8263(3) -0.0027(2) 0.0457(13) Uani 1 1 d . . . C12 C 1.2125(7) 0.9012(3) 0.0113(2) 0.0417(12) Uani 1 1 d . . . C13 C 1.2953(7) 0.9544(3) -0.0093(2) 0.0443(13) Uani 1 1 d . . . H13A H 1.3654 0.9469 -0.0355 0.053 Uiso 1 1 calc R . . C14 C 1.2567(7) 1.0197(3) 0.0154(2) 0.0459(13) Uani 1 1 d . . . H14A H 1.2932 1.0647 0.0086 0.055 Uiso 1 1 calc R . . C15 C 1.1536(7) 1.0063(3) 0.0522(2) 0.0419(12) Uani 1 1 d . . . C16 C 1.0659(7) 1.0438(3) 0.0891(2) 0.0437(13) Uani 1 1 d . . . C17 C 1.0390(7) 1.1146(3) 0.1082(3) 0.0475(14) Uani 1 1 d . . . H17A H 1.0868 1.1560 0.0984 0.057 Uiso 1 1 calc R . . C18 C 0.9291(7) 1.1119(3) 0.1441(3) 0.0494(14) Uani 1 1 d . . . H18A H 0.8887 1.1514 0.1637 0.059 Uiso 1 1 calc R . . C19 C 0.8879(7) 1.0390(3) 0.1462(3) 0.0462(13) Uani 1 1 d . . . C20 C 0.6823(7) 1.0464(3) 0.2080(2) 0.0465(13) Uani 1 1 d . . . C21 C 0.7157(9) 1.0606(4) 0.2654(3) 0.0649(18) Uani 1 1 d . . . C22 C 0.6240(12) 1.0947(5) 0.2998(3) 0.077(2) Uani 1 1 d . . . C23 C 0.4920(11) 1.1140(5) 0.2791(4) 0.083(3) Uani 1 1 d . . . C24 C 0.4586(9) 1.1032(5) 0.2225(4) 0.086(3) Uani 1 1 d . . . C25 C 0.5522(8) 1.0686(5) 0.1888(3) 0.067(2) Uani 1 1 d . . . C26 C 0.6762(11) 0.6786(4) 0.0987(4) 0.078(3) Uani 1 1 d . . . C27 C 0.7266(15) 0.6513(6) 0.1420(6) 0.102(4) Uani 1 1 d . . . C28 C 0.635(2) 0.5852(8) 0.1437(8) 0.139(6) Uani 1 1 d . . . C29 C 0.508(2) 0.5461(6) 0.1073(7) 0.135(6) Uani 1 1 d . . . C30 C 0.462(2) 0.5750(8) 0.0655(7) 0.166(8) Uani 1 1 d . . . C31 C 0.5409(15) 0.6397(6) 0.0601(6) 0.110(4) Uani 1 1 d . . . C32 C 1.2896(7) 0.7911(3) -0.0431(2) 0.0456(13) Uani 1 1 d . . . C33 C 1.2226(9) 0.7478(4) -0.0959(3) 0.0561(16) Uani 1 1 d . . . C34 C 1.3147(12) 0.7174(4) -0.1325(3) 0.068(2) Uani 1 1 d . . . C35 C 1.4776(12) 0.7272(4) -0.1185(4) 0.074(2) Uani 1 1 d . . . C36 C 1.5456(9) 0.7694(4) -0.0661(4) 0.071(2) Uani 1 1 d . . . C37 C 1.4531(8) 0.8018(4) -0.0288(3) 0.0525(15) Uani 1 1 d . . . C38 C 1.1735(7) 0.9125(4) 0.1646(3) 0.0514(15) Uani 1 1 d D . . H38A H 1.2699 0.8998 0.1501 0.062 Uiso 1 1 calc R A 1 H38B H 1.2049 0.9641 0.1872 0.062 Uiso 1 1 calc R A 1 C40 C 1.2382(9) 0.8961(5) 0.2588(4) 0.073(2) Uani 1 1 d D . . O2 O 1.1724(16) 0.8761(12) 0.2998(6) 0.090(4) Uani 0.54(2) 1 d PDU B 1 C39 C 1.129(2) 0.8676(10) 0.2020(6) 0.064(4) Uani 0.54(2) 1 d PDU B 1 H39A H 1.1347 0.8171 0.1842 0.077 Uiso 0.54(2) 1 calc PR B 1 H39B H 1.0158 0.8673 0.2071 0.077 Uiso 0.54(2) 1 calc PR B 1 C41 C 1.279(2) 0.8794(12) 0.3491(7) 0.075(5) Uani 0.54(2) 1 d PDU B 1 H41A H 1.2152 0.8712 0.3774 0.113 Uiso 0.54(2) 1 calc PR B 1 H41B H 1.3528 0.9272 0.3633 0.113 Uiso 0.54(2) 1 calc PR B 1 H41C H 1.3409 0.8420 0.3402 0.113 Uiso 0.54(2) 1 calc PR B 1 O2' O 1.201(2) 0.8421(11) 0.2823(9) 0.094(4) Uani 0.46(2) 1 d PDU B 2 C39' C 1.1076(18) 0.8966(14) 0.2137(7) 0.063(5) Uani 0.46(2) 1 d PDU B 2 H39C H 1.0307 0.8488 0.2010 0.076 Uiso 0.46(2) 1 calc PR B 2 H39D H 1.0478 0.9335 0.2292 0.076 Uiso 0.46(2) 1 calc PR B 2 C41' C 1.315(4) 0.8515(18) 0.3318(12) 0.116(9) Uani 0.46(2) 1 d PDU B 2 H41D H 1.2766 0.8148 0.3497 0.174 Uiso 0.46(2) 1 calc PR B 2 H41E H 1.3270 0.8999 0.3575 0.174 Uiso 0.46(2) 1 calc PR B 2 H41F H 1.4201 0.8460 0.3216 0.174 Uiso 0.46(2) 1 calc PR B 2 C42 C 0.7067(7) 0.4726(3) 0.3659(2) 0.0421(12) Uani 1 1 d . . . C43 C 0.6035(7) 0.4900(3) 0.3282(3) 0.0478(14) Uani 1 1 d . . . C44 C 0.5715(8) 0.4586(4) 0.2695(3) 0.0525(15) Uani 1 1 d . . . H44A H 0.6232 0.4242 0.2489 0.063 Uiso 1 1 calc R . . C45 C 0.4550(8) 0.4862(4) 0.2483(3) 0.0551(16) Uani 1 1 d . . . H45A H 0.4097 0.4738 0.2102 0.066 Uiso 1 1 calc R . . C46 C 0.4109(8) 0.5372(3) 0.2926(3) 0.0495(14) Uani 1 1 d . . . C47 C 0.2958(8) 0.5768(4) 0.2893(3) 0.0494(14) Uani 1 1 d . . . C48 C 0.2561(7) 0.6227(4) 0.3338(3) 0.0489(14) Uani 1 1 d . . . C49 C 0.1345(8) 0.6638(4) 0.3341(3) 0.0538(15) Uani 1 1 d . . . H49A H 0.0643 0.6641 0.3025 0.065 Uiso 1 1 calc R . . C50 C 0.1374(8) 0.7024(4) 0.3875(3) 0.0550(16) Uani 1 1 d . . . H50A H 0.0694 0.7343 0.3994 0.066 Uiso 1 1 calc R . . C51 C 0.2587(7) 0.6869(3) 0.4223(3) 0.0468(13) Uani 1 1 d . . . C52 C 0.2935(7) 0.7128(3) 0.4801(3) 0.0458(13) Uani 1 1 d . . . C53 C 0.4021(7) 0.6889(3) 0.5117(3) 0.0452(13) Uani 1 1 d . . . C54 C 0.4412(8) 0.6993(3) 0.5695(3) 0.0491(14) Uani 1 1 d . . . H54A H 0.4020 0.7305 0.5978 0.059 Uiso 1 1 calc R . . C55 C 0.5452(8) 0.6566(3) 0.5772(3) 0.0511(14) Uani 1 1 d . . . H55A H 0.5899 0.6522 0.6117 0.061 Uiso 1 1 calc R . . C56 C 0.5738(7) 0.6201(3) 0.5244(3) 0.0455(13) Uani 1 1 d . . . C57 C 0.6592(7) 0.5691(3) 0.5006(2) 0.0440(13) Uani 1 1 d . . . C58 C 0.7559(7) 0.5250(3) 0.5162(3) 0.0475(14) Uani 1 1 d . . . H58A H 0.7886 0.5238 0.5528 0.057 Uiso 1 1 calc R . . C59 C 0.7941(7) 0.4840(3) 0.4685(2) 0.0447(13) Uani 1 1 d . . . H59A H 0.8597 0.4498 0.4667 0.054 Uiso 1 1 calc R . . C60 C 0.7199(7) 0.5009(3) 0.4228(2) 0.0417(12) Uani 1 1 d . . . C61 C 0.8067(7) 0.4201(3) 0.3442(2) 0.0411(12) Uani 1 1 d . . . C62 C 0.9712(7) 0.4414(3) 0.3513(3) 0.0443(13) Uani 1 1 d . . . C63 C 1.0675(8) 0.3947(4) 0.3310(3) 0.0545(16) Uani 1 1 d . . . C64 C 1.0004(9) 0.3239(4) 0.3009(3) 0.0603(18) Uani 1 1 d . . . C65 C 0.8355(9) 0.3013(3) 0.2938(3) 0.0593(17) Uani 1 1 d . . . C66 C 0.7421(8) 0.3471(3) 0.3154(3) 0.0494(14) Uani 1 1 d . . . C67 C 0.2071(8) 0.5686(4) 0.2332(3) 0.0541(15) Uani 1 1 d . . . C68 C 0.0854(10) 0.5088(4) 0.2057(3) 0.072(2) Uani 1 1 d . . . C69 C 0.0026(12) 0.5001(5) 0.1546(4) 0.084(3) Uani 1 1 d . . . C70 C 0.0361(11) 0.5512(5) 0.1280(3) 0.077(2) Uani 1 1 d . . . C71 C 0.1608(11) 0.6110(5) 0.1538(4) 0.077(2) Uani 1 1 d . . . C72 C 0.2419(9) 0.6186(4) 0.2052(3) 0.0618(17) Uani 1 1 d . . . C73 C 0.2039(8) 0.7667(4) 0.5079(3) 0.0531(15) Uani 1 1 d . . . C74 C 0.2369(11) 0.8361(4) 0.5060(4) 0.075(2) Uani 1 1 d . . . C75 C 0.1468(13) 0.8846(5) 0.5272(4) 0.090(3) Uani 1 1 d . . . C76 C 0.0212(12) 0.8658(5) 0.5526(4) 0.088(3) Uani 1 1 d . . . C77 C -0.0141(9) 0.7966(5) 0.5551(4) 0.092(3) Uani 1 1 d . . . C78 C 0.0762(9) 0.7470(4) 0.5323(4) 0.073(2) Uani 1 1 d . . . C79 C 0.6975(7) 0.6922(3) 0.4070(3) 0.0480(14) Uani 1 1 d D . . H79A H 0.7321 0.7279 0.4442 0.058 Uiso 1 1 calc R C 1 H79B H 0.7916 0.6729 0.3964 0.058 Uiso 1 1 calc R C 1 O4 O 0.7037(19) 0.8280(9) 0.3327(7) 0.094(5) Uani 0.56(2) 1 d PDU D 1 C80 C 0.646(2) 0.7300(9) 0.3670(8) 0.073(5) Uani 0.56(2) 1 d PDU D 1 H80A H 0.5324 0.7326 0.3673 0.088 Uiso 0.56(2) 1 calc PR D 1 H80B H 0.6561 0.7027 0.3291 0.088 Uiso 0.56(2) 1 calc PR D 1 C81 C 0.7570(15) 0.8093(9) 0.3836(7) 0.059(5) Uani 0.56(2) 1 d PDU D 1 C82 C 0.800(3) 0.8958(11) 0.3301(10) 0.098(6) Uani 0.56(2) 1 d PDU D 1 H82A H 0.7608 0.9051 0.2956 0.147 Uiso 0.56(2) 1 calc PR D 1 H82B H 0.9131 0.8924 0.3310 0.147 Uiso 0.56(2) 1 calc PR D 1 H82C H 0.7925 0.9356 0.3618 0.147 Uiso 0.56(2) 1 calc PR D 1 O4' O 0.697(2) 0.8532(9) 0.3591(10) 0.082(5) Uani 0.44(2) 1 d PDU D 2 C80' C 0.634(2) 0.7490(11) 0.3880(10) 0.058(5) Uani 0.44(2) 1 d PDU D 2 H80C H 0.5959 0.7808 0.4187 0.070 Uiso 0.44(2) 1 calc PR D 2 H80D H 0.5420 0.7259 0.3571 0.070 Uiso 0.44(2) 1 calc PR D 2 C81' C 0.7738(19) 0.7949(10) 0.3681(9) 0.060(6) Uani 0.44(2) 1 d PDU D 2 C82' C 0.815(3) 0.9182(13) 0.3596(14) 0.099(8) Uani 0.44(2) 1 d PDU D 2 H82D H 0.7589 0.9551 0.3536 0.148 Uiso 0.44(2) 1 calc PR D 2 H82E H 0.8783 0.9054 0.3301 0.148 Uiso 0.44(2) 1 calc PR D 2 H82F H 0.8875 0.9373 0.3955 0.148 Uiso 0.44(2) 1 calc PR D 2 F1 F 0.8434(7) 1.0406(3) 0.28741(19) 0.0940(16) Uani 1 1 d . . . F2 F 0.6608(10) 1.1065(4) 0.3542(2) 0.132(3) Uani 1 1 d . . . F3 F 0.4001(8) 1.1494(4) 0.3133(3) 0.136(3) Uani 1 1 d . . . F4 F 0.3313(7) 1.1212(4) 0.2012(3) 0.150(3) Uani 1 1 d . . . F5 F 0.5117(7) 1.0565(4) 0.13411(19) 0.112(2) Uani 1 1 d . . . F6 F 0.8544(9) 0.6881(5) 0.1807(4) 0.137(3) Uani 1 1 d . . . F7 F 0.6886(14) 0.5610(6) 0.1859(6) 0.225(6) Uani 1 1 d . . . F8 F 0.4226(17) 0.4748(8) 0.1078(6) 0.280(7) Uani 1 1 d . . . F9 F 0.3236(16) 0.5396(6) 0.0265(5) 0.247(7) Uani 1 1 d . . . F10 F 0.4896(11) 0.6658(5) 0.0203(4) 0.173(4) Uani 1 1 d . . . F11 F 1.0628(5) 0.7346(2) -0.11355(17) 0.0704(11) Uani 1 1 d . . . F12 F 1.2409(9) 0.6746(3) -0.18357(19) 0.1046(19) Uani 1 1 d . . . F13 F 1.5625(11) 0.6933(4) -0.1539(3) 0.156(3) Uani 1 1 d . . . F14 F 1.7056(6) 0.7821(3) -0.0479(3) 0.1022(18) Uani 1 1 d . . . F15 F 1.5281(5) 0.8417(2) 0.02212(18) 0.0665(10) Uani 1 1 d . . . F16 F 1.0437(4) 0.5108(2) 0.37789(16) 0.0572(9) Uani 1 1 d . . . F17 F 1.2268(5) 0.4201(3) 0.33980(19) 0.0711(11) Uani 1 1 d . . . F18 F 1.0926(8) 0.2786(3) 0.2793(3) 0.118(2) Uani 1 1 d . . . F19 F 0.7640(7) 0.2328(2) 0.2633(2) 0.0881(15) Uani 1 1 d . . . F20 F 0.5800(5) 0.3213(2) 0.30595(17) 0.0638(10) Uani 1 1 d . . . F21 F 0.0470(7) 0.4562(3) 0.2294(2) 0.106(2) Uani 1 1 d . . . F22 F -0.1129(9) 0.4407(3) 0.1291(3) 0.138(3) Uani 1 1 d . . . F23 F -0.0467(8) 0.5440(4) 0.0773(2) 0.118(2) Uani 1 1 d . . . F24 F 0.1979(8) 0.6630(4) 0.1290(3) 0.119(2) Uani 1 1 d . . . F25 F 0.3623(6) 0.6782(3) 0.2288(2) 0.0972(17) Uani 1 1 d . . . F26 F 0.3586(8) 0.8587(3) 0.4822(3) 0.117(2) Uani 1 1 d . . . F27 F 0.1844(12) 0.9531(4) 0.5253(4) 0.158(3) Uani 1 1 d . . . F28 F -0.0658(10) 0.9136(4) 0.5747(4) 0.158(3) Uani 1 1 d . . . F29 F -0.1350(8) 0.7732(4) 0.5791(4) 0.174(4) Uani 1 1 d . . . F30 F 0.0367(8) 0.6794(3) 0.5358(3) 0.130(3) 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 0.0405(3) 0.0466(4) 0.0462(4) 0.0194(3) 0.0147(3) 0.0135(3) Ge2 0.0395(3) 0.0397(3) 0.0444(4) 0.0141(3) 0.0123(3) 0.0123(2) O1 0.071(4) 0.104(4) 0.067(3) 0.037(3) 0.009(3) 0.004(3) O3 0.066(4) 0.073(4) 0.133(6) 0.049(4) 0.008(4) 0.003(3) N1 0.043(3) 0.047(3) 0.053(3) 0.022(2) 0.018(2) 0.009(2) N2 0.048(3) 0.048(3) 0.053(3) 0.020(2) 0.020(2) 0.011(2) N3 0.043(3) 0.043(3) 0.046(3) 0.014(2) 0.014(2) 0.014(2) N4 0.044(3) 0.048(3) 0.047(3) 0.019(2) 0.014(2) 0.014(2) N5 0.044(3) 0.048(3) 0.046(3) 0.016(2) 0.010(2) 0.018(2) N6 0.040(3) 0.048(3) 0.054(3) 0.016(2) 0.011(2) 0.011(2) N7 0.048(3) 0.045(3) 0.047(3) 0.015(2) 0.012(2) 0.019(2) N8 0.045(3) 0.044(3) 0.042(3) 0.012(2) 0.014(2) 0.013(2) C1 0.043(3) 0.058(4) 0.045(3) 0.011(3) 0.008(3) 0.016(3) C2 0.044(3) 0.053(4) 0.052(3) 0.019(3) 0.014(3) 0.013(3) C3 0.042(3) 0.069(4) 0.068(4) 0.026(4) 0.022(3) 0.014(3) C4 0.054(4) 0.055(4) 0.079(5) 0.027(4) 0.032(4) 0.010(3) C5 0.046(3) 0.058(4) 0.065(4) 0.026(3) 0.017(3) 0.012(3) C6 0.057(4) 0.050(4) 0.079(5) 0.024(3) 0.025(4) 0.011(3) C7 0.054(4) 0.047(3) 0.066(4) 0.025(3) 0.020(3) 0.011(3) C8 0.081(5) 0.045(4) 0.081(5) 0.031(4) 0.036(4) 0.017(3) C9 0.070(4) 0.049(4) 0.063(4) 0.018(3) 0.028(3) 0.025(3) C10 0.054(4) 0.045(3) 0.057(4) 0.021(3) 0.019(3) 0.013(3) C11 0.048(3) 0.049(3) 0.044(3) 0.014(3) 0.013(3) 0.014(3) C12 0.043(3) 0.045(3) 0.041(3) 0.014(2) 0.011(2) 0.014(2) C13 0.042(3) 0.053(3) 0.041(3) 0.017(3) 0.013(2) 0.011(3) C14 0.043(3) 0.046(3) 0.047(3) 0.014(3) 0.011(3) 0.005(2) C15 0.038(3) 0.040(3) 0.047(3) 0.011(2) 0.006(2) 0.009(2) C16 0.039(3) 0.049(3) 0.046(3) 0.017(3) 0.011(2) 0.012(2) C17 0.051(3) 0.041(3) 0.048(3) 0.010(3) 0.004(3) 0.011(3) C18 0.049(3) 0.048(3) 0.052(3) 0.015(3) 0.009(3) 0.016(3) C19 0.043(3) 0.051(3) 0.047(3) 0.017(3) 0.011(3) 0.012(3) C20 0.041(3) 0.053(4) 0.045(3) 0.011(3) 0.010(3) 0.013(3) C21 0.067(4) 0.070(5) 0.050(4) 0.015(3) 0.012(3) 0.002(4) C22 0.096(6) 0.077(5) 0.048(4) 0.006(4) 0.032(4) 0.005(5) C23 0.080(6) 0.066(5) 0.082(6) -0.013(4) 0.045(5) 0.000(4) C24 0.043(4) 0.101(7) 0.084(6) -0.024(5) 0.005(4) 0.025(4) C25 0.050(4) 0.089(5) 0.048(4) -0.006(4) 0.004(3) 0.027(4) C26 0.079(5) 0.058(4) 0.115(7) 0.037(5) 0.063(5) 0.013(4) C27 0.102(8) 0.081(6) 0.158(11) 0.068(7) 0.080(8) 0.028(6) C28 0.169(13) 0.104(9) 0.206(16) 0.100(11) 0.131(13) 0.046(9) C29 0.172(14) 0.062(6) 0.170(14) 0.031(8) 0.100(12) -0.015(7) C30 0.195(16) 0.099(9) 0.150(13) -0.001(9) 0.078(12) -0.072(10) C31 0.117(9) 0.070(6) 0.146(11) 0.044(7) 0.055(8) -0.009(6) C32 0.056(4) 0.042(3) 0.047(3) 0.019(3) 0.017(3) 0.017(3) C33 0.076(5) 0.048(4) 0.049(4) 0.017(3) 0.010(3) 0.023(3) C34 0.110(7) 0.055(4) 0.049(4) 0.016(3) 0.034(4) 0.031(4) C35 0.113(7) 0.057(4) 0.078(5) 0.030(4) 0.062(5) 0.036(4) C36 0.066(5) 0.072(5) 0.108(7) 0.055(5) 0.050(5) 0.035(4) C37 0.051(4) 0.053(4) 0.061(4) 0.026(3) 0.018(3) 0.012(3) C38 0.046(3) 0.065(4) 0.054(4) 0.025(3) 0.022(3) 0.020(3) C40 0.053(4) 0.106(6) 0.079(5) 0.058(5) 0.019(4) 0.012(4) O2 0.087(6) 0.115(8) 0.075(6) 0.050(6) 0.013(5) 0.010(5) C39 0.062(7) 0.064(8) 0.068(7) 0.030(6) 0.002(5) 0.010(6) C41 0.082(8) 0.087(9) 0.064(7) 0.039(7) 0.010(6) 0.013(6) O2' 0.098(7) 0.101(8) 0.086(7) 0.054(6) -0.003(5) 0.004(6) C39' 0.057(7) 0.070(9) 0.067(8) 0.028(7) 0.009(6) 0.014(6) C41' 0.124(12) 0.115(12) 0.113(12) 0.045(9) 0.006(9) 0.027(9) C42 0.043(3) 0.039(3) 0.047(3) 0.011(2) 0.016(3) 0.012(2) C43 0.050(3) 0.046(3) 0.050(3) 0.012(3) 0.015(3) 0.015(3) C44 0.057(4) 0.058(4) 0.044(3) 0.011(3) 0.014(3) 0.020(3) C45 0.065(4) 0.062(4) 0.040(3) 0.015(3) 0.006(3) 0.018(3) C46 0.053(4) 0.052(4) 0.046(3) 0.018(3) 0.010(3) 0.014(3) C47 0.049(3) 0.055(4) 0.048(3) 0.018(3) 0.007(3) 0.016(3) C48 0.039(3) 0.054(4) 0.058(4) 0.026(3) 0.007(3) 0.009(3) C49 0.046(3) 0.062(4) 0.060(4) 0.024(3) 0.009(3) 0.019(3) C50 0.044(3) 0.058(4) 0.072(4) 0.026(3) 0.015(3) 0.022(3) C51 0.039(3) 0.044(3) 0.058(4) 0.014(3) 0.013(3) 0.012(2) C52 0.039(3) 0.046(3) 0.058(4) 0.015(3) 0.020(3) 0.016(2) C53 0.043(3) 0.041(3) 0.053(3) 0.010(3) 0.016(3) 0.012(2) C54 0.052(3) 0.052(4) 0.044(3) 0.009(3) 0.017(3) 0.017(3) C55 0.057(4) 0.054(4) 0.049(3) 0.017(3) 0.019(3) 0.020(3) C56 0.044(3) 0.042(3) 0.050(3) 0.012(3) 0.010(3) 0.010(2) C57 0.045(3) 0.046(3) 0.045(3) 0.015(3) 0.014(3) 0.015(3) C58 0.048(3) 0.048(3) 0.048(3) 0.018(3) 0.002(3) 0.013(3) C59 0.042(3) 0.042(3) 0.050(3) 0.010(3) 0.011(3) 0.014(2) C60 0.041(3) 0.038(3) 0.050(3) 0.013(3) 0.015(3) 0.013(2) C61 0.050(3) 0.036(3) 0.040(3) 0.012(2) 0.011(2) 0.014(2) C62 0.046(3) 0.045(3) 0.051(3) 0.020(3) 0.017(3) 0.017(3) C63 0.048(4) 0.066(4) 0.064(4) 0.034(3) 0.022(3) 0.020(3) C64 0.073(5) 0.057(4) 0.071(4) 0.028(4) 0.040(4) 0.036(4) C65 0.082(5) 0.036(3) 0.060(4) 0.009(3) 0.025(4) 0.015(3) C66 0.054(4) 0.044(3) 0.050(3) 0.012(3) 0.017(3) 0.007(3) C67 0.054(4) 0.054(4) 0.060(4) 0.026(3) 0.003(3) 0.016(3) C68 0.078(5) 0.069(5) 0.066(5) 0.030(4) -0.004(4) 0.004(4) C69 0.093(6) 0.074(5) 0.077(5) 0.027(5) -0.018(5) 0.009(5) C70 0.098(6) 0.084(6) 0.052(4) 0.024(4) -0.007(4) 0.035(5) C71 0.087(6) 0.089(6) 0.071(5) 0.048(5) 0.013(4) 0.020(5) C72 0.058(4) 0.066(4) 0.065(4) 0.028(4) 0.004(3) 0.014(3) C73 0.053(4) 0.050(4) 0.059(4) 0.012(3) 0.014(3) 0.022(3) C74 0.088(6) 0.060(5) 0.089(6) 0.026(4) 0.035(5) 0.033(4) C75 0.112(7) 0.073(6) 0.115(8) 0.041(5) 0.050(6) 0.054(5) C76 0.083(6) 0.069(6) 0.103(7) -0.006(5) 0.006(5) 0.046(5) C77 0.050(4) 0.095(7) 0.111(7) -0.012(5) 0.037(5) 0.020(4) C78 0.061(4) 0.052(4) 0.101(6) 0.006(4) 0.035(4) 0.010(3) C79 0.044(3) 0.053(4) 0.056(4) 0.021(3) 0.017(3) 0.021(3) O4 0.103(7) 0.085(8) 0.099(8) 0.054(6) 0.007(6) 0.002(6) C80 0.075(7) 0.076(8) 0.071(8) 0.035(7) 0.017(6) 0.002(6) C81 0.054(6) 0.057(7) 0.077(8) 0.025(6) 0.022(6) 0.025(5) C82 0.118(10) 0.085(9) 0.095(10) 0.057(8) 0.010(8) -0.002(7) O4' 0.086(7) 0.071(8) 0.098(9) 0.044(7) 0.013(7) 0.014(6) C80' 0.060(7) 0.053(8) 0.066(9) 0.024(7) 0.014(6) 0.012(6) C81' 0.062(8) 0.059(9) 0.065(9) 0.028(7) 0.019(6) 0.013(6) C82' 0.114(11) 0.090(10) 0.104(11) 0.051(9) 0.021(8) 0.018(8) F1 0.121(4) 0.111(4) 0.060(3) 0.031(3) -0.001(3) 0.051(3) F2 0.223(8) 0.125(5) 0.054(3) 0.018(3) 0.053(4) 0.050(5) F3 0.121(5) 0.117(5) 0.137(5) -0.027(4) 0.072(4) 0.015(4) F4 0.091(4) 0.197(7) 0.123(5) -0.049(5) -0.017(4) 0.100(5) F5 0.101(4) 0.182(6) 0.053(3) -0.004(3) -0.007(2) 0.097(4) F6 0.111(5) 0.160(7) 0.192(8) 0.135(6) 0.040(5) 0.027(5) F7 0.245(11) 0.198(9) 0.348(15) 0.224(11) 0.146(11) 0.065(8) F8 0.269(14) 0.302(15) 0.298(15) 0.173(13) 0.140(12) -0.043(11) F9 0.267(12) 0.163(9) 0.218(11) 0.016(8) 0.056(9) -0.124(9) F10 0.176(8) 0.148(7) 0.142(7) 0.049(6) -0.020(6) -0.072(6) F11 0.076(3) 0.063(3) 0.063(2) 0.009(2) -0.011(2) 0.020(2) F12 0.187(6) 0.072(3) 0.053(3) 0.005(2) 0.031(3) 0.038(3) F13 0.223(9) 0.133(6) 0.176(7) 0.068(5) 0.148(7) 0.096(6) F14 0.059(3) 0.124(4) 0.157(5) 0.073(4) 0.052(3) 0.038(3) F15 0.051(2) 0.078(3) 0.069(3) 0.026(2) 0.0043(19) 0.0089(19) F16 0.053(2) 0.049(2) 0.064(2) 0.0124(17) 0.0107(18) 0.0047(16) F17 0.050(2) 0.091(3) 0.090(3) 0.042(3) 0.027(2) 0.025(2) F18 0.134(5) 0.106(4) 0.150(5) 0.045(4) 0.083(4) 0.072(4) F19 0.118(4) 0.043(2) 0.099(3) 0.005(2) 0.045(3) 0.015(2) F20 0.056(2) 0.054(2) 0.072(3) 0.0084(19) 0.0171(19) 0.0013(17) F21 0.117(4) 0.087(4) 0.102(4) 0.059(3) -0.031(3) -0.025(3) F22 0.150(6) 0.104(4) 0.117(5) 0.046(4) -0.069(4) -0.042(4) F23 0.148(5) 0.129(5) 0.081(4) 0.047(3) -0.016(3) 0.044(4) F24 0.130(5) 0.138(5) 0.111(4) 0.091(4) 0.002(4) 0.012(4) F25 0.090(3) 0.093(4) 0.103(4) 0.055(3) -0.012(3) -0.014(3) F26 0.162(6) 0.070(3) 0.161(6) 0.060(4) 0.108(5) 0.045(3) F27 0.250(9) 0.092(4) 0.197(8) 0.073(5) 0.112(7) 0.106(6) F28 0.151(6) 0.142(6) 0.185(8) 0.005(5) 0.057(6) 0.089(5) F29 0.116(5) 0.104(5) 0.275(10) -0.019(5) 0.142(6) 0.008(4) F30 0.123(5) 0.057(3) 0.218(7) 0.018(4) 0.126(5) 0.013(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 N3 1.922(5) . ? Ge1 C38 1.928(7) . ? Ge1 N2 1.933(5) . ? Ge1 N4 1.937(5) . ? Ge1 N1 1.941(5) . ? Ge2 N6 1.929(5) . ? Ge2 N8 1.931(5) . ? Ge2 N7 1.931(5) . ? Ge2 N5 1.932(5) . ? Ge2 C79 1.938(6) . ? O1 C40 1.151(9) . ? O3 C81 1.182(13) . ? O3 C81' 1.198(15) . ? N1 C5 1.383(8) . ? N1 C2 1.395(8) . ? N2 C7 1.386(8) . ? N2 C10 1.402(8) . ? N3 C15 1.366(7) . ? N3 C12 1.381(7) . ? N4 C19 1.363(7) . ? N4 C16 1.364(7) . ? N5 C46 1.392(8) . ? N5 C43 1.402(7) . ? N6 C48 1.400(8) . ? N6 C51 1.400(8) . ? N7 C56 1.368(8) . ? N7 C53 1.373(7) . ? N8 C60 1.370(7) . ? N8 C57 1.379(7) . ? C1 C2 1.393(9) . ? C1 C19 1.396(9) . ? C1 C20 1.479(8) . ? C2 C3 1.432(9) . ? C3 C4 1.359(10) . ? C3 H3A 0.9500 . ? C4 C5 1.410(9) . ? C4 H4A 0.9500 . ? C5 C6 1.381(10) . ? C6 C7 1.360(9) . ? C6 C26 1.490(10) . ? C7 C8 1.462(10) . ? C8 C9 1.341(9) . ? C8 H8A 0.9500 . ? C9 C10 1.412(9) . ? C9 H9A 0.9500 . ? C10 C11 1.405(8) . ? C11 C12 1.394(8) . ? C11 C32 1.495(8) . ? C12 C13 1.406(8) . ? C13 C14 1.387(8) . ? C13 H13A 0.9500 . ? C14 C15 1.402(8) . ? C14 H14A 0.9500 . ? C15 C16 1.409(8) . ? C16 C17 1.420(8) . ? C17 C18 1.389(9) . ? C17 H17A 0.9500 . ? C18 C19 1.429(9) . ? C18 H18A 0.9500 . ? C20 C25 1.362(9) . ? C20 C21 1.398(9) . ? C21 F1 1.346(9) . ? C21 C22 1.370(11) . ? C22 F2 1.332(10) . ? C22 C23 1.356(13) . ? C23 F3 1.378(9) . ? C23 C24 1.386(13) . ? C24 F4 1.316(10) . ? C24 C25 1.375(10) . ? C25 F5 1.341(8) . ? C26 C31 1.380(16) . ? C26 C27 1.413(15) . ? C27 F6 1.332(15) . ? C27 C28 1.403(15) . ? C28 C29 1.31(2) . ? C28 F7 1.355(19) . ? C29 C30 1.39(2) . ? C29 F8 1.460(15) . ? C30 C31 1.377(15) . ? C30 F9 1.39(2) . ? C31 F10 1.324(15) . ? C32 C37 1.371(9) . ? C32 C33 1.376(9) . ? C33 F11 1.347(8) . ? C33 C34 1.376(10) . ? C34 F12 1.352(9) . ? C34 C35 1.367(13) . ? C35 F13 1.339(9) . ? C35 C36 1.363(13) . ? C36 F14 1.353(10) . ? C36 C37 1.404(10) . ? C37 F15 1.338(8) . ? C38 C39 1.500(13) . ? C38 C39' 1.513(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C40 O2 1.354(12) . ? C40 O2' 1.360(13) . ? C40 C39' 1.516(15) . ? C40 C39 1.534(14) . ? O2 C41 1.447(15) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? O2' C41' 1.457(18) . ? C39' H39C 0.9900 . ? C39' H39D 0.9900 . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42 C43 1.387(9) . ? C42 C60 1.389(8) . ? C42 C61 1.496(7) . ? C43 C44 1.429(9) . ? C44 C45 1.352(9) . ? C44 H44A 0.9500 . ? C45 C46 1.432(9) . ? C45 H45A 0.9500 . ? C46 C47 1.376(9) . ? C47 C48 1.367(9) . ? C47 C67 1.493(9) . ? C48 C49 1.435(8) . ? C49 C50 1.362(10) . ? C49 H49A 0.9500 . ? C50 C51 1.422(9) . ? C50 H50A 0.9500 . ? C51 C52 1.399(9) . ? C52 C53 1.390(9) . ? C52 C73 1.498(8) . ? C53 C54 1.423(9) . ? C54 C55 1.369(9) . ? C54 H54A 0.9500 . ? C55 C56 1.416(9) . ? C55 H55A 0.9500 . ? C56 C57 1.401(8) . ? C57 C58 1.407(8) . ? C58 C59 1.376(8) . ? C58 H58A 0.9500 . ? C59 C60 1.413(8) . ? C59 H59A 0.9500 . ? C61 C62 1.372(8) . ? C61 C66 1.397(8) . ? C62 F16 1.342(7) . ? C62 C63 1.384(9) . ? C63 F17 1.336(8) . ? C63 C64 1.374(10) . ? C64 F18 1.348(8) . ? C64 C65 1.378(10) . ? C65 F19 1.348(8) . ? C65 C66 1.363(9) . ? C66 F20 1.359(7) . ? C67 C72 1.372(10) . ? C67 C68 1.379(10) . ? C68 F21 1.342(9) . ? C68 C69 1.362(11) . ? C69 F22 1.336(10) . ? C69 C70 1.362(12) . ? C70 F23 1.360(9) . ? C70 C71 1.383(13) . ? C71 F24 1.349(9) . ? C71 C72 1.368(11) . ? C72 F25 1.354(9) . ? C73 C74 1.358(10) . ? C73 C78 1.364(10) . ? C74 F26 1.331(9) . ? C74 C75 1.375(11) . ? C75 F27 1.342(11) . ? C75 C76 1.362(14) . ? C76 F28 1.352(9) . ? C76 C77 1.360(14) . ? C77 F29 1.334(11) . ? C77 C78 1.404(10) . ? C78 F30 1.338(9) . ? C79 C80 1.489(14) . ? C79 C80' 1.497(14) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? O4 C82 1.457(15) . ? O4 C81 1.487(15) . ? C80 C81 1.586(16) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? O4' C82' 1.474(18) . ? O4' C81' 1.481(17) . ? C80' C81' 1.579(17) . ? C80' H80C 0.9900 . ? C80' H80D 0.9900 . ? C82' H82D 0.9800 . ? C82' H82E 0.9800 . ? C82' H82F 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 N3 Ge1 C38 105.9(2) . . ? N3 Ge1 N2 86.7(2) . . ? C38 Ge1 N2 105.9(3) . . ? N3 Ge1 N4 78.7(2) . . ? C38 Ge1 N4 105.7(3) . . ? N2 Ge1 N4 147.8(2) . . ? N3 Ge1 N1 148.1(2) . . ? C38 Ge1 N1 105.2(2) . . ? N2 Ge1 N1 91.4(2) . . ? N4 Ge1 N1 86.4(2) . . ? N6 Ge2 N8 148.4(2) . . ? N6 Ge2 N7 86.7(2) . . ? N8 Ge2 N7 78.75(19) . . ? N6 Ge2 N5 91.4(2) . . ? N8 Ge2 N5 86.6(2) . . ? N7 Ge2 N5 147.9(2) . . ? N6 Ge2 C79 105.0(2) . . ? N8 Ge2 C79 105.9(2) . . ? N7 Ge2 C79 106.0(2) . . ? N5 Ge2 C79 105.4(2) . . ? C81 O3 C81' 23.0(15) . . ? C5 N1 C2 108.0(5) . . ? C5 N1 Ge1 124.5(4) . . ? C2 N1 Ge1 125.4(4) . . ? C7 N2 C10 108.3(5) . . ? C7 N2 Ge1 123.9(4) . . ? C10 N2 Ge1 125.6(4) . . ? C15 N3 C12 108.4(5) . . ? C15 N3 Ge1 117.8(4) . . ? C12 N3 Ge1 133.1(4) . . ? C19 N4 C16 109.8(5) . . ? C19 N4 Ge1 132.6(4) . . ? C16 N4 Ge1 116.7(4) . . ? C46 N5 C43 108.0(5) . . ? C46 N5 Ge2 124.3(4) . . ? C43 N5 Ge2 125.5(4) . . ? C48 N6 C51 107.8(5) . . ? C48 N6 Ge2 125.0(4) . . ? C51 N6 Ge2 125.5(4) . . ? C56 N7 C53 109.1(5) . . ? C56 N7 Ge2 117.3(4) . . ? C53 N7 Ge2 132.5(4) . . ? C60 N8 C57 109.7(5) . . ? C60 N8 Ge2 133.0(4) . . ? C57 N8 Ge2 117.0(4) . . ? C2 C1 C19 122.4(6) . . ? C2 C1 C20 117.4(6) . . ? C19 C1 C20 120.1(6) . . ? C1 C2 N1 126.2(5) . . ? C1 C2 C3 126.0(6) . . ? N1 C2 C3 107.6(5) . . ? C4 C3 C2 107.3(6) . . ? C4 C3 H3A 126.3 . . ? C2 C3 H3A 126.3 . . ? C3 C4 C5 109.1(6) . . ? C3 C4 H4A 125.4 . . ? C5 C4 H4A 125.4 . . ? C6 C5 N1 123.9(6) . . ? C6 C5 C4 128.2(6) . . ? N1 C5 C4 107.9(6) . . ? C7 C6 C5 125.1(6) . . ? C7 C6 C26 118.1(6) . . ? C5 C6 C26 116.7(6) . . ? C6 C7 N2 125.1(6) . . ? C6 C7 C8 128.0(6) . . ? N2 C7 C8 106.9(5) . . ? C9 C8 C7 107.5(6) . . ? C9 C8 H8A 126.3 . . ? C7 C8 H8A 126.3 . . ? C8 C9 C10 109.8(6) . . ? C8 C9 H9A 125.1 . . ? C10 C9 H9A 125.1 . . ? N2 C10 C11 125.6(6) . . ? N2 C10 C9 107.5(5) . . ? C11 C10 C9 126.9(6) . . ? C12 C11 C10 122.7(5) . . ? C12 C11 C32 118.7(5) . . ? C10 C11 C32 118.5(5) . . ? N3 C12 C11 119.4(5) . . ? N3 C12 C13 107.6(5) . . ? C11 C12 C13 132.8(5) . . ? C14 C13 C12 108.2(5) . . ? C14 C13 H13A 125.9 . . ? C12 C13 H13A 125.9 . . ? C13 C14 C15 106.7(5) . . ? C13 C14 H14A 126.7 . . ? C15 C14 H14A 126.7 . . ? N3 C15 C14 109.2(5) . . ? N3 C15 C16 111.8(5) . . ? C14 C15 C16 139.0(6) . . ? N4 C16 C15 112.9(5) . . ? N4 C16 C17 108.3(5) . . ? C15 C16 C17 138.8(6) . . ? C18 C17 C16 106.9(5) . . ? C18 C17 H17A 126.6 . . ? C16 C17 H17A 126.6 . . ? C17 C18 C19 107.6(5) . . ? C17 C18 H18A 126.2 . . ? C19 C18 H18A 126.2 . . ? N4 C19 C1 120.0(6) . . ? N4 C19 C18 107.4(5) . . ? C1 C19 C18 132.3(6) . . ? C25 C20 C21 115.3(6) . . ? C25 C20 C1 122.9(6) . . ? C21 C20 C1 121.6(6) . . ? F1 C21 C22 119.1(7) . . ? F1 C21 C20 118.7(6) . . ? C22 C21 C20 122.2(8) . . ? F2 C22 C23 119.5(8) . . ? F2 C22 C21 119.6(9) . . ? C23 C22 C21 120.8(8) . . ? C22 C23 F3 121.4(9) . . ? C22 C23 C24 118.5(7) . . ? F3 C23 C24 119.8(10) . . ? F4 C24 C25 120.4(8) . . ? F4 C24 C23 119.9(8) . . ? C25 C24 C23 119.5(8) . . ? F5 C25 C20 118.8(6) . . ? F5 C25 C24 117.6(7) . . ? C20 C25 C24 123.6(7) . . ? C31 C26 C27 119.3(9) . . ? C31 C26 C6 121.5(9) . . ? C27 C26 C6 119.3(9) . . ? F6 C27 C28 121.2(13) . . ? F6 C27 C26 120.9(8) . . ? C28 C27 C26 117.8(14) . . ? C29 C28 F7 119.7(13) . . ? C29 C28 C27 124.7(15) . . ? F7 C28 C27 115.7(17) . . ? C28 C29 C30 115.8(11) . . ? C28 C29 F8 123.4(17) . . ? C30 C29 F8 120.8(16) . . ? C31 C30 F9 115.1(18) . . ? C31 C30 C29 124.5(15) . . ? F9 C30 C29 120.3(12) . . ? F10 C31 C30 122.2(14) . . ? F10 C31 C26 119.8(8) . . ? C30 C31 C26 117.9(14) . . ? C37 C32 C33 116.2(6) . . ? C37 C32 C11 120.5(6) . . ? C33 C32 C11 123.2(6) . . ? F11 C33 C32 120.3(6) . . ? F11 C33 C34 117.9(7) . . ? C32 C33 C34 121.9(7) . . ? F12 C34 C35 118.8(7) . . ? F12 C34 C33 118.8(8) . . ? C35 C34 C33 122.3(7) . . ? F13 C35 C36 122.5(10) . . ? F13 C35 C34 120.9(9) . . ? C36 C35 C34 116.5(7) . . ? F14 C36 C35 121.3(7) . . ? F14 C36 C37 117.1(8) . . ? C35 C36 C37 121.6(8) . . ? F15 C37 C32 120.4(6) . . ? F15 C37 C36 118.1(6) . . ? C32 C37 C36 121.4(7) . . ? C39 C38 C39' 24.3(9) . . ? C39 C38 Ge1 117.1(6) . . ? C39' C38 Ge1 114.8(6) . . ? C39 C38 H38A 108.1 . . ? C39' C38 H38A 127.7 . . ? Ge1 C38 H38A 108.0 . . ? C39 C38 H38B 108.0 . . ? C39' C38 H38B 87.0 . . ? Ge1 C38 H38B 108.0 . . ? H38A C38 H38B 107.3 . . ? O1 C40 O2 118.8(10) . . ? O1 C40 O2' 121.9(10) . . ? O2 C40 O2' 33.9(9) . . ? O1 C40 C39' 123.3(10) . . ? O2 C40 C39' 110.5(10) . . ? O2' C40 C39' 114.5(12) . . ? O1 C40 C39 126.5(8) . . ? O2 C40 C39 114.6(10) . . ? O2' C40 C39 103.9(10) . . ? C39' C40 C39 24.0(9) . . ? C40 O2 C41 118.4(12) . . ? C38 C39 C40 112.5(9) . . ? C38 C39 H39A 109.1 . . ? C40 C39 H39A 109.1 . . ? C38 C39 H39B 109.1 . . ? C40 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.4 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 O2' C41' 112.5(17) . . ? C38 C39' C40 112.8(10) . . ? C38 C39' H39C 109.0 . . ? C40 C39' H39C 109.0 . . ? C38 C39' H39D 109.1 . . ? C40 C39' H39D 109.1 . . ? H39C C39' H39D 107.8 . . ? O2' C41' H41D 109.5 . . ? O2' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? O2' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C43 C42 C60 123.0(5) . . ? C43 C42 C61 118.4(5) . . ? C60 C42 C61 118.6(5) . . ? C42 C43 N5 125.6(5) . . ? C42 C43 C44 126.6(6) . . ? N5 C43 C44 107.7(5) . . ? C45 C44 C43 108.1(6) . . ? C45 C44 H44A 125.9 . . ? C43 C44 H44A 125.9 . . ? C44 C45 C46 108.9(6) . . ? C44 C45 H45A 125.5 . . ? C46 C45 H45A 125.5 . . ? C47 C46 N5 124.8(6) . . ? C47 C46 C45 127.9(6) . . ? N5 C46 C45 107.3(5) . . ? C48 C47 C46 124.6(6) . . ? C48 C47 C67 117.7(6) . . ? C46 C47 C67 117.8(6) . . ? C47 C48 N6 124.4(6) . . ? C47 C48 C49 128.0(6) . . ? N6 C48 C49 107.7(6) . . ? C50 C49 C48 108.0(6) . . ? C50 C49 H49A 126.0 . . ? C48 C49 H49A 126.0 . . ? C49 C50 C51 108.8(6) . . ? C49 C50 H50A 125.6 . . ? C51 C50 H50A 125.6 . . ? C52 C51 N6 125.8(5) . . ? C52 C51 C50 126.3(6) . . ? N6 C51 C50 107.8(6) . . ? C53 C52 C51 122.9(5) . . ? C53 C52 C73 120.0(6) . . ? C51 C52 C73 117.0(5) . . ? N7 C53 C52 119.4(5) . . ? N7 C53 C54 107.3(5) . . ? C52 C53 C54 133.1(5) . . ? C55 C54 C53 108.0(5) . . ? C55 C54 H54A 126.0 . . ? C53 C54 H54A 126.0 . . ? C54 C55 C56 107.4(6) . . ? C54 C55 H55A 126.3 . . ? C56 C55 H55A 126.3 . . ? N7 C56 C57 112.3(5) . . ? N7 C56 C55 108.2(5) . . ? C57 C56 C55 139.5(6) . . ? N8 C57 C56 112.6(5) . . ? N8 C57 C58 107.7(5) . . ? C56 C57 C58 139.7(6) . . ? C59 C58 C57 107.1(5) . . ? C59 C58 H58A 126.5 . . ? C57 C58 H58A 126.5 . . ? C58 C59 C60 108.9(5) . . ? C58 C59 H59A 125.5 . . ? C60 C59 H59A 125.5 . . ? N8 C60 C42 119.7(5) . . ? N8 C60 C59 106.6(5) . . ? C42 C60 C59 133.5(5) . . ? C62 C61 C66 115.1(5) . . ? C62 C61 C42 121.4(5) . . ? C66 C61 C42 123.5(5) . . ? F16 C62 C61 119.2(5) . . ? F16 C62 C63 117.7(5) . . ? C61 C62 C63 123.0(6) . . ? F17 C63 C64 120.2(6) . . ? F17 C63 C62 119.0(6) . . ? C64 C63 C62 120.7(6) . . ? F18 C64 C63 121.2(7) . . ? F18 C64 C65 121.8(7) . . ? C63 C64 C65 117.1(6) . . ? F19 C65 C66 119.1(7) . . ? F19 C65 C64 119.1(6) . . ? C66 C65 C64 121.7(6) . . ? F20 C66 C65 118.4(6) . . ? F20 C66 C61 119.3(5) . . ? C65 C66 C61 122.3(6) . . ? C72 C67 C68 115.4(7) . . ? C72 C67 C47 123.1(6) . . ? C68 C67 C47 121.5(6) . . ? F21 C68 C69 118.1(7) . . ? F21 C68 C67 119.3(7) . . ? C69 C68 C67 122.6(7) . . ? F22 C69 C68 120.6(8) . . ? F22 C69 C70 118.3(8) . . ? C68 C69 C70 121.1(8) . . ? F23 C70 C69 122.0(9) . . ? F23 C70 C71 120.3(8) . . ? C69 C70 C71 117.7(7) . . ? F24 C71 C72 120.1(8) . . ? F24 C71 C70 119.8(7) . . ? C72 C71 C70 120.1(7) . . ? F25 C72 C71 117.8(7) . . ? F25 C72 C67 119.2(6) . . ? C71 C72 C67 123.0(7) . . ? C74 C73 C78 116.6(6) . . ? C74 C73 C52 121.6(6) . . ? C78 C73 C52 121.6(6) . . ? F26 C74 C73 119.7(7) . . ? F26 C74 C75 118.0(8) . . ? C73 C74 C75 122.3(8) . . ? F27 C75 C76 117.7(8) . . ? F27 C75 C74 120.7(9) . . ? C76 C75 C74 121.5(8) . . ? F28 C76 C77 120.7(10) . . ? F28 C76 C75 122.0(10) . . ? C77 C76 C75 117.3(7) . . ? F29 C77 C76 121.7(8) . . ? F29 C77 C78 117.5(9) . . ? C76 C77 C78 120.8(8) . . ? F30 C78 C73 120.0(6) . . ? F30 C78 C77 118.6(7) . . ? C73 C78 C77 121.4(8) . . ? C80 C79 C80' 23.1(9) . . ? C80 C79 Ge2 113.8(7) . . ? C80' C79 Ge2 113.7(8) . . ? C80 C79 H79A 108.8 . . ? C80' C79 H79A 87.9 . . ? Ge2 C79 H79A 108.8 . . ? C80 C79 H79B 108.8 . . ? C80' C79 H79B 126.6 . . ? Ge2 C79 H79B 108.8 . . ? H79A C79 H79B 107.7 . . ? C82 O4 C81 113.0(14) . . ? C79 C80 C81 109.3(12) . . ? C79 C80 H80A 109.8 . . ? C81 C80 H80A 109.8 . . ? C79 C80 H80B 109.8 . . ? C81 C80 H80B 109.8 . . ? H80A C80 H80B 108.3 . . ? O3 C81 O4 117.8(14) . . ? O3 C81 C80 123.0(15) . . ? O4 C81 C80 97.8(12) . . ? O4 C82 H82A 109.5 . . ? O4 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O4 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C82' O4' C81' 112.5(18) . . ? C79 C80' C81' 108.4(13) . . ? C79 C80' H80C 110.0 . . ? C81' C80' H80C 110.0 . . ? C79 C80' H80D 110.0 . . ? C81' C80' H80D 110.0 . . ? H80C C80' H80D 108.4 . . ? O3 C81' O4' 108.0(17) . . ? O3 C81' C80' 117.3(18) . . ? O4' C81' C80' 100.4(14) . . ? O4' C82' H82D 109.5 . . ? O4' C82' H82E 109.5 . . ? H82D C82' H82E 109.5 . . ? O4' C82' H82F 109.5 . . ? H82D C82' H82F 109.5 . . ? H82E C82' H82F 109.5 . . ? 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 N1 C5 110.5(6) . . . . ? C38 Ge1 N1 C5 -82.5(6) . . . . ? N2 Ge1 N1 C5 24.4(5) . . . . ? N4 Ge1 N1 C5 172.2(5) . . . . ? N3 Ge1 N1 C2 -87.8(6) . . . . ? C38 Ge1 N1 C2 79.2(5) . . . . ? N2 Ge1 N1 C2 -173.9(5) . . . . ? N4 Ge1 N1 C2 -26.1(5) . . . . ? N3 Ge1 N2 C7 -172.6(5) . . . . ? C38 Ge1 N2 C7 81.8(5) . . . . ? N4 Ge1 N2 C7 -109.9(6) . . . . ? N1 Ge1 N2 C7 -24.5(5) . . . . ? N3 Ge1 N2 C10 26.0(5) . . . . ? C38 Ge1 N2 C10 -79.6(5) . . . . ? N4 Ge1 N2 C10 88.7(6) . . . . ? N1 Ge1 N2 C10 174.1(5) . . . . ? C38 Ge1 N3 C15 -90.6(5) . . . . ? N2 Ge1 N3 C15 163.8(4) . . . . ? N4 Ge1 N3 C15 12.7(4) . . . . ? N1 Ge1 N3 C15 76.3(6) . . . . ? C38 Ge1 N3 C12 79.0(6) . . . . ? N2 Ge1 N3 C12 -26.6(6) . . . . ? N4 Ge1 N3 C12 -177.7(6) . . . . ? N1 Ge1 N3 C12 -114.0(6) . . . . ? N3 Ge1 N4 C19 179.1(6) . . . . ? C38 Ge1 N4 C19 -77.4(6) . . . . ? N2 Ge1 N4 C19 114.3(6) . . . . ? N1 Ge1 N4 C19 27.4(6) . . . . ? N3 Ge1 N4 C16 -13.2(4) . . . . ? C38 Ge1 N4 C16 90.4(5) . . . . ? N2 Ge1 N4 C16 -77.9(6) . . . . ? N1 Ge1 N4 C16 -164.9(5) . . . . ? N6 Ge2 N5 C46 24.3(5) . . . . ? N8 Ge2 N5 C46 172.7(5) . . . . ? N7 Ge2 N5 C46 110.2(5) . . . . ? C79 Ge2 N5 C46 -81.7(5) . . . . ? N6 Ge2 N5 C43 -174.6(5) . . . . ? N8 Ge2 N5 C43 -26.2(5) . . . . ? N7 Ge2 N5 C43 -88.7(6) . . . . ? C79 Ge2 N5 C43 79.4(5) . . . . ? N8 Ge2 N6 C48 -108.5(6) . . . . ? N7 Ge2 N6 C48 -170.6(5) . . . . ? N5 Ge2 N6 C48 -22.7(5) . . . . ? C79 Ge2 N6 C48 83.7(5) . . . . ? N8 Ge2 N6 C51 88.2(6) . . . . ? N7 Ge2 N6 C51 26.0(5) . . . . ? N5 Ge2 N6 C51 174.0(5) . . . . ? C79 Ge2 N6 C51 -79.6(5) . . . . ? N6 Ge2 N7 C56 165.2(5) . . . . ? N8 Ge2 N7 C56 13.4(4) . . . . ? N5 Ge2 N7 C56 77.9(6) . . . . ? C79 Ge2 N7 C56 -90.1(5) . . . . ? N6 Ge2 N7 C53 -28.5(6) . . . . ? N8 Ge2 N7 C53 179.7(6) . . . . ? N5 Ge2 N7 C53 -115.8(6) . . . . ? C79 Ge2 N7 C53 76.2(6) . . . . ? N6 Ge2 N8 C60 111.1(6) . . . . ? N7 Ge2 N8 C60 175.2(6) . . . . ? N5 Ge2 N8 C60 23.9(5) . . . . ? C79 Ge2 N8 C60 -81.2(6) . . . . ? N6 Ge2 N8 C57 -75.9(6) . . . . ? N7 Ge2 N8 C57 -11.8(4) . . . . ? N5 Ge2 N8 C57 -163.1(4) . . . . ? C79 Ge2 N8 C57 91.8(5) . . . . ? C19 C1 C2 N1 1.7(10) . . . . ? C20 C1 C2 N1 179.0(6) . . . . ? C19 C1 C2 C3 -174.2(6) . . . . ? C20 C1 C2 C3 3.2(10) . . . . ? C5 N1 C2 C1 -176.9(6) . . . . ? Ge1 N1 C2 C1 18.9(9) . . . . ? C5 N1 C2 C3 -0.4(7) . . . . ? Ge1 N1 C2 C3 -164.6(4) . . . . ? C1 C2 C3 C4 177.1(7) . . . . ? N1 C2 C3 C4 0.5(8) . . . . ? C2 C3 C4 C5 -0.5(8) . . . . ? C2 N1 C5 C6 -179.7(7) . . . . ? Ge1 N1 C5 C6 -15.3(10) . . . . ? C2 N1 C5 C4 0.1(7) . . . . ? Ge1 N1 C5 C4 164.5(5) . . . . ? C3 C4 C5 C6 -179.9(7) . . . . ? C3 C4 C5 N1 0.3(9) . . . . ? N1 C5 C6 C7 -2.9(12) . . . . ? C4 C5 C6 C7 177.4(8) . . . . ? N1 C5 C6 C26 179.8(7) . . . . ? C4 C5 C6 C26 0.1(12) . . . . ? C5 C6 C7 N2 2.5(13) . . . . ? C26 C6 C7 N2 179.7(7) . . . . ? C5 C6 C7 C8 -177.2(8) . . . . ? C26 C6 C7 C8 0.1(13) . . . . ? C10 N2 C7 C6 -179.8(7) . . . . ? Ge1 N2 C7 C6 16.0(10) . . . . ? C10 N2 C7 C8 -0.1(7) . . . . ? Ge1 N2 C7 C8 -164.3(5) . . . . ? C6 C7 C8 C9 -179.5(8) . . . . ? N2 C7 C8 C9 0.8(8) . . . . ? C7 C8 C9 C10 -1.2(9) . . . . ? C7 N2 C10 C11 177.7(6) . . . . ? Ge1 N2 C10 C11 -18.5(9) . . . . ? C7 N2 C10 C9 -0.6(7) . . . . ? Ge1 N2 C10 C9 163.2(5) . . . . ? C8 C9 C10 N2 1.1(9) . . . . ? C8 C9 C10 C11 -177.1(7) . . . . ? N2 C10 C11 C12 -2.8(10) . . . . ? C9 C10 C11 C12 175.1(7) . . . . ? N2 C10 C11 C32 -179.1(6) . . . . ? C9 C10 C11 C32 -1.2(10) . . . . ? C15 N3 C12 C11 -174.2(5) . . . . ? Ge1 N3 C12 C11 15.4(9) . . . . ? C15 N3 C12 C13 0.9(6) . . . . ? Ge1 N3 C12 C13 -169.5(4) . . . . ? C10 C11 C12 N3 5.1(9) . . . . ? C32 C11 C12 N3 -178.6(5) . . . . ? C10 C11 C12 C13 -168.5(6) . . . . ? C32 C11 C12 C13 7.8(10) . . . . ? N3 C12 C13 C14 -1.5(7) . . . . ? C11 C12 C13 C14 172.6(6) . . . . ? C12 C13 C14 C15 1.6(7) . . . . ? C12 N3 C15 C14 0.1(7) . . . . ? Ge1 N3 C15 C14 172.2(4) . . . . ? C12 N3 C15 C16 178.0(5) . . . . ? Ge1 N3 C15 C16 -10.0(6) . . . . ? C13 C14 C15 N3 -1.1(7) . . . . ? C13 C14 C15 C16 -178.1(7) . . . . ? C19 N4 C16 C15 -177.9(5) . . . . ? Ge1 N4 C16 C15 11.6(7) . . . . ? C19 N4 C16 C17 -0.2(7) . . . . ? Ge1 N4 C16 C17 -170.6(4) . . . . ? N3 C15 C16 N4 -1.2(7) . . . . ? C14 C15 C16 N4 175.8(7) . . . . ? N3 C15 C16 C17 -177.9(7) . . . . ? C14 C15 C16 C17 -1.0(14) . . . . ? N4 C16 C17 C18 0.6(7) . . . . ? C15 C16 C17 C18 177.4(7) . . . . ? C16 C17 C18 C19 -0.7(7) . . . . ? C16 N4 C19 C1 174.4(5) . . . . ? Ge1 N4 C19 C1 -17.2(9) . . . . ? C16 N4 C19 C18 -0.2(7) . . . . ? Ge1 N4 C19 C18 168.1(4) . . . . ? C2 C1 C19 N4 -3.4(9) . . . . ? C20 C1 C19 N4 179.3(5) . . . . ? C2 C1 C19 C18 169.8(7) . . . . ? C20 C1 C19 C18 -7.6(11) . . . . ? C17 C18 C19 N4 0.6(7) . . . . ? C17 C18 C19 C1 -173.2(7) . . . . ? C2 C1 C20 C25 -97.4(8) . . . . ? C19 C1 C20 C25 80.1(9) . . . . ? C2 C1 C20 C21 76.8(8) . . . . ? C19 C1 C20 C21 -105.7(8) . . . . ? C25 C20 C21 F1 -179.5(7) . . . . ? C1 C20 C21 F1 5.8(10) . . . . ? C25 C20 C21 C22 -0.2(11) . . . . ? C1 C20 C21 C22 -174.8(7) . . . . ? F1 C21 C22 F2 -1.1(12) . . . . ? C20 C21 C22 F2 179.5(7) . . . . ? F1 C21 C22 C23 -178.2(8) . . . . ? C20 C21 C22 C23 2.4(13) . . . . ? F2 C22 C23 F3 3.9(13) . . . . ? C21 C22 C23 F3 -178.9(8) . . . . ? F2 C22 C23 C24 178.2(8) . . . . ? C21 C22 C23 C24 -4.7(13) . . . . ? C22 C23 C24 F4 179.9(9) . . . . ? F3 C23 C24 F4 -5.8(14) . . . . ? C22 C23 C24 C25 4.9(14) . . . . ? F3 C23 C24 C25 179.2(8) . . . . ? C21 C20 C25 F5 -179.6(7) . . . . ? C1 C20 C25 F5 -5.0(12) . . . . ? C21 C20 C25 C24 0.4(12) . . . . ? C1 C20 C25 C24 175.0(8) . . . . ? F4 C24 C25 F5 2.1(14) . . . . ? C23 C24 C25 F5 177.2(8) . . . . ? F4 C24 C25 C20 -177.8(9) . . . . ? C23 C24 C25 C20 -2.8(14) . . . . ? C7 C6 C26 C31 -84.2(11) . . . . ? C5 C6 C26 C31 93.3(11) . . . . ? C7 C6 C26 C27 95.3(10) . . . . ? C5 C6 C26 C27 -87.2(10) . . . . ? C31 C26 C27 F6 -178.5(10) . . . . ? C6 C26 C27 F6 2.0(14) . . . . ? C31 C26 C27 C28 -0.2(14) . . . . ? C6 C26 C27 C28 -179.8(9) . . . . ? F6 C27 C28 C29 179.7(13) . . . . ? C26 C27 C28 C29 1.5(19) . . . . ? F6 C27 C28 F7 -2.0(17) . . . . ? C26 C27 C28 F7 179.8(10) . . . . ? F7 C28 C29 C30 -179.9(13) . . . . ? C27 C28 C29 C30 -2(2) . . . . ? F7 C28 C29 F8 -3(2) . . . . ? C27 C28 C29 F8 174.9(12) . . . . ? C28 C29 C30 C31 1(2) . . . . ? F8 C29 C30 C31 -175.9(14) . . . . ? C28 C29 C30 F9 -176.7(14) . . . . ? F8 C29 C30 F9 7(2) . . . . ? F9 C30 C31 F10 -1(2) . . . . ? C29 C30 C31 F10 -178.1(14) . . . . ? F9 C30 C31 C26 177.9(12) . . . . ? C29 C30 C31 C26 0(2) . . . . ? C27 C26 C31 F10 177.9(10) . . . . ? C6 C26 C31 F10 -2.6(16) . . . . ? C27 C26 C31 C30 -0.6(17) . . . . ? C6 C26 C31 C30 178.9(11) . . . . ? C12 C11 C32 C37 69.2(8) . . . . ? C10 C11 C32 C37 -114.3(7) . . . . ? C12 C11 C32 C33 -109.8(7) . . . . ? C10 C11 C32 C33 66.7(8) . . . . ? C37 C32 C33 F11 -179.7(6) . . . . ? C11 C32 C33 F11 -0.6(9) . . . . ? C37 C32 C33 C34 -0.5(9) . . . . ? C11 C32 C33 C34 178.6(6) . . . . ? F11 C33 C34 F12 -1.7(10) . . . . ? C32 C33 C34 F12 179.1(6) . . . . ? F11 C33 C34 C35 -179.6(6) . . . . ? C32 C33 C34 C35 1.1(11) . . . . ? F12 C34 C35 F13 -2.2(11) . . . . ? C33 C34 C35 F13 175.8(7) . . . . ? F12 C34 C35 C36 -178.5(7) . . . . ? C33 C34 C35 C36 -0.5(11) . . . . ? F13 C35 C36 F14 3.1(11) . . . . ? C34 C35 C36 F14 179.3(7) . . . . ? F13 C35 C36 C37 -176.9(7) . . . . ? C34 C35 C36 C37 -0.7(11) . . . . ? C33 C32 C37 F15 -178.5(6) . . . . ? C11 C32 C37 F15 2.4(9) . . . . ? C33 C32 C37 C36 -0.7(9) . . . . ? C11 C32 C37 C36 -179.8(6) . . . . ? F14 C36 C37 F15 -0.9(9) . . . . ? C35 C36 C37 F15 179.2(6) . . . . ? F14 C36 C37 C32 -178.7(6) . . . . ? C35 C36 C37 C32 1.3(11) . . . . ? N3 Ge1 C38 C39 -157.7(11) . . . . ? N2 Ge1 C38 C39 -66.6(11) . . . . ? N4 Ge1 C38 C39 119.8(11) . . . . ? N1 Ge1 C38 C39 29.4(11) . . . . ? N3 Ge1 C38 C39' 175.3(12) . . . . ? N2 Ge1 C38 C39' -93.6(12) . . . . ? N4 Ge1 C38 C39' 92.8(12) . . . . ? N1 Ge1 C38 C39' 2.4(12) . . . . ? O1 C40 O2 C41 -23(2) . . . . ? O2' C40 O2 C41 82(2) . . . . ? C39' C40 O2 C41 -174.0(19) . . . . ? C39 C40 O2 C41 160.3(18) . . . . ? C39' C38 C39 C40 -70.1(17) . . . . ? Ge1 C38 C39 C40 -160.8(10) . . . . ? O1 C40 C39 C38 -19(2) . . . . ? O2 C40 C39 C38 157.1(18) . . . . ? O2' C40 C39 C38 -169(2) . . . . ? C39' C40 C39 C38 71.8(18) . . . . ? O1 C40 O2' C41' 16(3) . . . . ? O2 C40 O2' C41' -79(2) . . . . ? C39' C40 O2' C41' -169.4(19) . . . . ? C39 C40 O2' C41' 168(2) . . . . ? C39 C38 C39' C40 72.5(18) . . . . ? Ge1 C38 C39' C40 173.7(11) . . . . ? O1 C40 C39' C38 35(2) . . . . ? O2 C40 C39' C38 -175.3(19) . . . . ? O2' C40 C39' C38 -139(2) . . . . ? C39 C40 C39' C38 -70.6(18) . . . . ? C60 C42 C43 N5 1.5(10) . . . . ? C61 C42 C43 N5 -179.3(5) . . . . ? C60 C42 C43 C44 -173.8(6) . . . . ? C61 C42 C43 C44 5.3(10) . . . . ? C46 N5 C43 C42 -175.9(6) . . . . ? Ge2 N5 C43 C42 20.4(9) . . . . ? C46 N5 C43 C44 0.2(7) . . . . ? Ge2 N5 C43 C44 -163.5(4) . . . . ? C42 C43 C44 C45 175.2(6) . . . . ? N5 C43 C44 C45 -0.8(8) . . . . ? C43 C44 C45 C46 1.1(8) . . . . ? C43 N5 C46 C47 178.6(6) . . . . ? Ge2 N5 C46 C47 -17.5(9) . . . . ? C43 N5 C46 C45 0.5(7) . . . . ? Ge2 N5 C46 C45 164.4(4) . . . . ? C44 C45 C46 C47 -179.0(7) . . . . ? C44 C45 C46 N5 -1.0(8) . . . . ? N5 C46 C47 C48 -0.2(11) . . . . ? C45 C46 C47 C48 177.4(7) . . . . ? N5 C46 C47 C67 -179.7(6) . . . . ? C45 C46 C47 C67 -2.0(10) . . . . ? C46 C47 C48 N6 2.2(10) . . . . ? C67 C47 C48 N6 -178.3(6) . . . . ? C46 C47 C48 C49 -177.7(6) . . . . ? C67 C47 C48 C49 1.8(10) . . . . ? C51 N6 C48 C47 179.6(6) . . . . ? Ge2 N6 C48 C47 13.9(9) . . . . ? C51 N6 C48 C49 -0.4(6) . . . . ? Ge2 N6 C48 C49 -166.2(4) . . . . ? C47 C48 C49 C50 -179.6(6) . . . . ? N6 C48 C49 C50 0.4(7) . . . . ? C48 C49 C50 C51 -0.2(8) . . . . ? C48 N6 C51 C52 176.6(6) . . . . ? Ge2 N6 C51 C52 -17.6(9) . . . . ? C48 N6 C51 C50 0.3(7) . . . . ? Ge2 N6 C51 C50 166.0(4) . . . . ? C49 C50 C51 C52 -176.4(6) . . . . ? C49 C50 C51 N6 0.0(7) . . . . ? N6 C51 C52 C53 -3.1(10) . . . . ? C50 C51 C52 C53 172.6(6) . . . . ? N6 C51 C52 C73 178.9(6) . . . . ? C50 C51 C52 C73 -5.4(9) . . . . ? C56 N7 C53 C52 -174.6(5) . . . . ? Ge2 N7 C53 C52 18.3(9) . . . . ? C56 N7 C53 C54 0.8(7) . . . . ? Ge2 N7 C53 C54 -166.3(5) . . . . ? C51 C52 C53 N7 3.6(9) . . . . ? C73 C52 C53 N7 -178.5(5) . . . . ? C51 C52 C53 C54 -170.4(7) . . . . ? C73 C52 C53 C54 7.6(11) . . . . ? N7 C53 C54 C55 -1.1(7) . . . . ? C52 C53 C54 C55 173.4(7) . . . . ? C53 C54 C55 C56 1.0(7) . . . . ? C53 N7 C56 C57 178.1(5) . . . . ? Ge2 N7 C56 C57 -12.6(7) . . . . ? C53 N7 C56 C55 -0.2(7) . . . . ? Ge2 N7 C56 C55 169.1(4) . . . . ? C54 C55 C56 N7 -0.5(7) . . . . ? C54 C55 C56 C57 -178.1(8) . . . . ? C60 N8 C57 C56 -177.0(5) . . . . ? Ge2 N8 C57 C56 8.4(7) . . . . ? C60 N8 C57 C58 0.7(7) . . . . ? Ge2 N8 C57 C58 -173.9(4) . . . . ? N7 C56 C57 N8 2.5(7) . . . . ? C55 C56 C57 N8 -179.9(7) . . . . ? N7 C56 C57 C58 -174.1(7) . . . . ? C55 C56 C57 C58 3.4(15) . . . . ? N8 C57 C58 C59 0.2(7) . . . . ? C56 C57 C58 C59 176.9(8) . . . . ? C57 C58 C59 C60 -1.0(7) . . . . ? C57 N8 C60 C42 174.8(5) . . . . ? Ge2 N8 C60 C42 -11.8(8) . . . . ? C57 N8 C60 C59 -1.3(6) . . . . ? Ge2 N8 C60 C59 172.1(4) . . . . ? C43 C42 C60 N8 -6.4(9) . . . . ? C61 C42 C60 N8 174.4(5) . . . . ? C43 C42 C60 C59 168.4(6) . . . . ? C61 C42 C60 C59 -10.8(10) . . . . ? C58 C59 C60 N8 1.4(7) . . . . ? C58 C59 C60 C42 -173.9(6) . . . . ? C43 C42 C61 C62 113.6(7) . . . . ? C60 C42 C61 C62 -67.2(8) . . . . ? C43 C42 C61 C66 -66.2(8) . . . . ? C60 C42 C61 C66 113.0(7) . . . . ? C66 C61 C62 F16 179.1(5) . . . . ? C42 C61 C62 F16 -0.8(8) . . . . ? C66 C61 C62 C63 1.0(9) . . . . ? C42 C61 C62 C63 -178.8(6) . . . . ? F16 C62 C63 F17 1.8(9) . . . . ? C61 C62 C63 F17 179.9(6) . . . . ? F16 C62 C63 C64 -176.6(6) . . . . ? C61 C62 C63 C64 1.5(10) . . . . ? F17 C63 C64 F18 -0.6(10) . . . . ? C62 C63 C64 F18 177.8(6) . . . . ? F17 C63 C64 C65 179.5(6) . . . . ? C62 C63 C64 C65 -2.2(10) . . . . ? F18 C64 C65 F19 -1.7(11) . . . . ? C63 C64 C65 F19 178.2(6) . . . . ? F18 C64 C65 C66 -179.6(7) . . . . ? C63 C64 C65 C66 0.3(11) . . . . ? F19 C65 C66 F20 1.1(10) . . . . ? C64 C65 C66 F20 179.0(6) . . . . ? F19 C65 C66 C61 -175.6(6) . . . . ? C64 C65 C66 C61 2.4(11) . . . . ? C62 C61 C66 F20 -179.6(5) . . . . ? C42 C61 C66 F20 0.2(9) . . . . ? C62 C61 C66 C65 -2.9(9) . . . . ? C42 C61 C66 C65 176.9(6) . . . . ? C48 C47 C67 C72 78.8(9) . . . . ? C46 C47 C67 C72 -101.7(8) . . . . ? C48 C47 C67 C68 -102.4(8) . . . . ? C46 C47 C67 C68 77.1(9) . . . . ? C72 C67 C68 F21 178.0(8) . . . . ? C47 C67 C68 F21 -0.9(12) . . . . ? C72 C67 C68 C69 -1.2(13) . . . . ? C47 C67 C68 C69 179.9(8) . . . . ? F21 C68 C69 F22 -0.2(15) . . . . ? C67 C68 C69 F22 179.0(9) . . . . ? F21 C68 C69 C70 -179.6(9) . . . . ? C67 C68 C69 C70 -0.4(16) . . . . ? F22 C69 C70 F23 1.5(15) . . . . ? C68 C69 C70 F23 -179.1(9) . . . . ? F22 C69 C70 C71 -177.2(9) . . . . ? C68 C69 C70 C71 2.3(15) . . . . ? F23 C70 C71 F24 1.5(14) . . . . ? C69 C70 C71 F24 -179.8(9) . . . . ? F23 C70 C71 C72 178.9(8) . . . . ? C69 C70 C71 C72 -2.4(14) . . . . ? F24 C71 C72 F25 -2.3(13) . . . . ? C70 C71 C72 F25 -179.6(8) . . . . ? F24 C71 C72 C67 178.2(8) . . . . ? C70 C71 C72 C67 0.8(14) . . . . ? C68 C67 C72 F25 -178.6(7) . . . . ? C47 C67 C72 F25 0.3(11) . . . . ? C68 C67 C72 C71 1.0(12) . . . . ? C47 C67 C72 C71 179.8(7) . . . . ? C53 C52 C73 C74 109.2(8) . . . . ? C51 C52 C73 C74 -72.7(9) . . . . ? C53 C52 C73 C78 -76.5(9) . . . . ? C51 C52 C73 C78 101.6(8) . . . . ? C78 C73 C74 F26 -179.2(8) . . . . ? C52 C73 C74 F26 -4.6(13) . . . . ? C78 C73 C74 C75 -0.3(14) . . . . ? C52 C73 C74 C75 174.3(9) . . . . ? F26 C74 C75 F27 -2.1(16) . . . . ? C73 C74 C75 F27 179.0(10) . . . . ? F26 C74 C75 C76 -179.4(10) . . . . ? C73 C74 C75 C76 1.7(17) . . . . ? F27 C75 C76 F28 0.9(16) . . . . ? C74 C75 C76 F28 178.4(10) . . . . ? F27 C75 C76 C77 -178.9(10) . . . . ? C74 C75 C76 C77 -1.5(16) . . . . ? F28 C76 C77 F29 0.2(16) . . . . ? C75 C76 C77 F29 -179.9(10) . . . . ? F28 C76 C77 C78 -179.9(9) . . . . ? C75 C76 C77 C78 0.0(16) . . . . ? C74 C73 C78 F30 -179.8(9) . . . . ? C52 C73 C78 F30 5.6(13) . . . . ? C74 C73 C78 C77 -1.2(13) . . . . ? C52 C73 C78 C77 -175.8(8) . . . . ? F29 C77 C78 F30 -0.1(15) . . . . ? C76 C77 C78 F30 180.0(9) . . . . ? F29 C77 C78 C73 -178.7(9) . . . . ? C76 C77 C78 C73 1.4(15) . . . . ? N6 Ge2 C79 C80 -25.9(11) . . . . ? N8 Ge2 C79 C80 160.7(11) . . . . ? N7 Ge2 C79 C80 -116.7(11) . . . . ? N5 Ge2 C79 C80 69.9(11) . . . . ? N6 Ge2 C79 C80' -0.5(11) . . . . ? N8 Ge2 C79 C80' -174.0(11) . . . . ? N7 Ge2 C79 C80' -91.4(11) . . . . ? N5 Ge2 C79 C80' 95.2(11) . . . . ? C80' C79 C80 C81 62(3) . . . . ? Ge2 C79 C80 C81 156.9(12) . . . . ? C81' O3 C81 O4 -61(3) . . . . ? C81' O3 C81 C80 61(3) . . . . ? C82 O4 C81 O3 -38(3) . . . . ? C82 O4 C81 C80 -171.5(17) . . . . ? C79 C80 C81 O3 39(3) . . . . ? C79 C80 C81 O4 169.5(13) . . . . ? C80 C79 C80' C81' -66(3) . . . . ? Ge2 C79 C80' C81' -161.9(13) . . . . ? C81 O3 C81' O4' 56(3) . . . . ? C81 O3 C81' C80' -57(3) . . . . ? C82' O4' C81' O3 36(3) . . . . ? C82' O4' C81' C80' 159.4(19) . . . . ? C79 C80' C81' O3 -55(3) . . . . ? C79 C80' C81' O4' -172.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.625 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.112