# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(TPFC)Ge(TEMPO) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H26 F15 Ge N5 O' _chemical_formula_sum 'C46 H26 F15 Ge N5 O' _chemical_formula_weight 1022.31 _chemical_absolute_configuration ad 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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.9476(18) _cell_length_b 15.748(3) _cell_length_c 32.247(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4543.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15497 _cell_measurement_theta_min 1.4390 _cell_measurement_theta_max 27.4812 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6112 _exptl_absorpt_correction_T_max 1.0000 _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 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32966 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10402 _reflns_number_gt 9471 _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 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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^)+(0.0434P)^2^+3.3081P] 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 0.035(9) _refine_ls_number_reflns 10402 _refine_ls_number_parameters 617 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _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 0.40327(4) 0.37130(2) 0.696345(11) 0.02373(9) Uani 1 1 d . . . F1 F 0.5431(3) 0.43357(16) 0.85720(7) 0.0382(6) Uani 1 1 d . . . F2 F 0.5012(3) 0.48824(19) 0.93538(8) 0.0518(7) Uani 1 1 d . . . F3 F 0.2281(4) 0.5434(2) 0.95996(9) 0.0676(9) Uani 1 1 d . . . F4 F -0.0018(3) 0.5475(2) 0.90477(10) 0.0642(9) Uani 1 1 d . . . F5 F 0.0381(3) 0.49111(18) 0.82705(8) 0.0475(7) Uani 1 1 d . . . F6 F 0.0201(3) 0.64916(17) 0.66909(9) 0.0516(7) Uani 1 1 d . . . F7 F -0.0221(3) 0.80802(19) 0.64067(11) 0.0634(8) Uani 1 1 d . . . F8 F 0.1930(4) 0.88581(18) 0.59556(9) 0.0577(8) Uani 1 1 d . . . F9 F 0.4568(3) 0.80417(18) 0.58029(9) 0.0567(8) Uani 1 1 d . . . F10 F 0.5026(3) 0.64790(17) 0.61062(8) 0.0466(6) Uani 1 1 d . . . F11 F 0.0274(3) 0.24925(18) 0.57019(8) 0.0444(6) Uani 1 1 d . . . F12 F -0.0266(3) 0.16279(19) 0.50033(8) 0.0537(7) Uani 1 1 d . . . F13 F 0.1987(4) 0.0847(2) 0.45918(8) 0.0612(8) Uani 1 1 d . . . F14 F 0.4834(4) 0.0964(2) 0.48831(9) 0.0604(8) Uani 1 1 d . . . F15 F 0.5385(3) 0.18295(19) 0.55828(8) 0.0494(7) Uani 1 1 d . . . O1 O 0.5926(3) 0.40527(16) 0.69055(8) 0.0306(5) Uani 1 1 d . . . N1 N 0.3771(3) 0.3160(2) 0.74915(9) 0.0269(7) Uani 1 1 d . . . N2 N 0.3798(3) 0.25595(19) 0.67869(9) 0.0256(6) Uani 1 1 d . . . N3 N 0.3241(3) 0.4049(2) 0.64277(10) 0.0265(7) Uani 1 1 d . . . N4 N 0.3227(4) 0.4722(2) 0.72147(10) 0.0278(7) Uani 1 1 d . . . N5 N 0.7147(3) 0.3460(2) 0.70109(10) 0.0305(7) Uani 1 1 d . . . C1 C 0.3858(4) 0.2288(2) 0.74924(11) 0.0278(8) Uani 1 1 d . . . C2 C 0.3683(5) 0.2003(3) 0.79106(12) 0.0345(9) Uani 1 1 d . . . H2 H 0.3715 0.1433 0.8006 0.041 Uiso 1 1 calc R . . C3 C 0.3460(4) 0.2716(3) 0.81474(12) 0.0312(8) Uani 1 1 d . . . H3 H 0.3322 0.2720 0.8439 0.037 Uiso 1 1 calc R . . C4 C 0.3470(4) 0.3442(2) 0.78897(11) 0.0271(8) Uani 1 1 d . . . C5 C 0.3180(4) 0.4297(2) 0.79645(11) 0.0269(8) Uani 1 1 d . . . C6 C 0.3094(4) 0.4894(2) 0.76455(11) 0.0277(8) Uani 1 1 d . . . C7 C 0.2858(5) 0.5778(3) 0.76898(13) 0.0352(9) Uani 1 1 d . . . H7 H 0.2744 0.6069 0.7946 0.042 Uiso 1 1 calc R . . C8 C 0.2820(5) 0.6145(2) 0.73086(12) 0.0334(9) Uani 1 1 d . . . H8 H 0.2691 0.6732 0.7251 0.040 Uiso 1 1 calc R . . C9 C 0.3011(4) 0.5484(2) 0.70120(12) 0.0276(8) Uani 1 1 d . . . C10 C 0.2909(4) 0.5563(2) 0.65784(12) 0.0289(8) Uani 1 1 d . . . C11 C 0.2962(4) 0.4875(2) 0.63063(12) 0.0288(8) Uani 1 1 d . . . C12 C 0.2651(5) 0.4891(3) 0.58766(12) 0.0348(9) Uani 1 1 d . . . H12 H 0.2437 0.5381 0.5716 0.042 Uiso 1 1 calc R . . C13 C 0.2711(4) 0.4083(2) 0.57360(12) 0.0299(8) Uani 1 1 d . . . H13 H 0.2552 0.3909 0.5457 0.036 Uiso 1 1 calc R . . C14 C 0.3053(4) 0.3535(2) 0.60746(11) 0.0260(8) Uani 1 1 d . . . C15 C 0.3176(4) 0.2646(2) 0.60645(11) 0.0257(7) Uani 1 1 d . . . C16 C 0.3497(4) 0.2179(2) 0.64159(11) 0.0266(8) Uani 1 1 d . . . C17 C 0.3429(4) 0.1290(3) 0.64884(12) 0.0325(8) Uani 1 1 d . . . H17 H 0.3257 0.0867 0.6284 0.039 Uiso 1 1 calc R . . C18 C 0.3658(4) 0.1141(2) 0.69086(12) 0.0341(9) Uani 1 1 d . . . H18 H 0.3676 0.0605 0.7044 0.041 Uiso 1 1 calc R . . C19 C 0.3856(4) 0.1945(2) 0.70945(11) 0.0247(7) Uani 1 1 d . . . C20 C 0.8002(5) 0.3302(3) 0.66153(12) 0.0371(10) Uani 1 1 d . . . C21 C 0.9303(4) 0.2721(3) 0.67367(14) 0.0403(10) Uani 1 1 d . . . H21B H 0.8897 0.2170 0.6832 0.048 Uiso 1 1 calc R . . H21A H 0.9925 0.2611 0.6488 0.048 Uiso 1 1 calc R . . C22 C 1.0276(5) 0.3088(3) 0.70730(14) 0.0438(11) Uani 1 1 d . . . H22B H 1.1070 0.2678 0.7147 0.053 Uiso 1 1 calc R . . H22A H 1.0760 0.3615 0.6972 0.053 Uiso 1 1 calc R . . C23 C 0.9345(4) 0.3282(3) 0.74465(13) 0.0369(10) Uani 1 1 d . . . H23B H 0.9985 0.3555 0.7659 0.044 Uiso 1 1 calc R . . H23A H 0.8970 0.2742 0.7564 0.044 Uiso 1 1 calc R . . C24 C 0.8013(4) 0.3863(2) 0.73569(11) 0.0290(8) Uani 1 1 d . . . C25 C 0.8529(6) 0.4094(4) 0.63835(15) 0.0542(14) Uani 1 1 d . . . H25A H 0.8667 0.3957 0.6090 0.081 Uiso 1 1 calc R . . H25C H 0.9479 0.4288 0.6501 0.081 Uiso 1 1 calc R . . H25B H 0.7778 0.4543 0.6411 0.081 Uiso 1 1 calc R . . C26 C 0.6971(5) 0.2794(3) 0.63245(14) 0.0462(11) Uani 1 1 d . . . H26B H 0.6159 0.3161 0.6227 0.069 Uiso 1 1 calc R . . H26C H 0.6550 0.2310 0.6475 0.069 Uiso 1 1 calc R . . H26A H 0.7547 0.2589 0.6086 0.069 Uiso 1 1 calc R . . C27 C 0.8532(5) 0.4788(3) 0.72822(14) 0.0398(10) Uani 1 1 d . . . H27B H 0.9413 0.4788 0.7102 0.060 Uiso 1 1 calc R . . H27C H 0.8786 0.5053 0.7548 0.060 Uiso 1 1 calc R . . H27A H 0.7725 0.5110 0.7150 0.060 Uiso 1 1 calc R . . C28 C 0.7009(5) 0.3858(3) 0.77368(12) 0.0376(10) Uani 1 1 d . . . H28A H 0.6175 0.4252 0.7694 0.056 Uiso 1 1 calc R . . H28C H 0.7586 0.4035 0.7980 0.056 Uiso 1 1 calc R . . H28B H 0.6619 0.3284 0.7781 0.056 Uiso 1 1 calc R . . C29 C 0.2927(5) 0.4589(3) 0.83946(12) 0.0322(9) Uani 1 1 d . . . C30 C 0.4043(5) 0.4592(2) 0.86882(11) 0.0319(8) Uani 1 1 d . . . C31 C 0.3855(5) 0.4883(3) 0.90886(12) 0.0361(9) Uani 1 1 d . . . C32 C 0.2487(6) 0.5171(3) 0.92091(14) 0.0460(11) Uani 1 1 d . . . C33 C 0.1312(5) 0.5185(3) 0.89298(14) 0.0452(11) Uani 1 1 d . . . C34 C 0.1548(5) 0.4893(3) 0.85316(13) 0.0375(9) Uani 1 1 d . . . C35 C 0.2637(4) 0.6425(2) 0.64108(12) 0.0305(8) Uani 1 1 d . . . C36 C 0.1316(5) 0.6863(3) 0.64780(13) 0.0375(9) Uani 1 1 d . . . C37 C 0.1078(5) 0.7677(3) 0.63251(15) 0.0432(10) Uani 1 1 d . . . C38 C 0.2159(6) 0.8072(3) 0.61003(13) 0.0405(10) Uani 1 1 d . . . C39 C 0.3489(6) 0.7654(3) 0.60225(13) 0.0426(11) Uani 1 1 d . . . C40 C 0.3711(5) 0.6857(3) 0.61814(12) 0.0349(9) Uani 1 1 d . . . C41 C 0.2854(4) 0.2189(3) 0.56728(11) 0.0291(8) Uani 1 1 d . . . C42 C 0.1438(4) 0.2128(3) 0.55077(12) 0.0336(9) Uani 1 1 d . . . C43 C 0.1136(5) 0.1677(3) 0.51455(12) 0.0379(9) Uani 1 1 d . . . C44 C 0.2262(5) 0.1274(3) 0.49417(12) 0.0409(10) Uani 1 1 d . . . C45 C 0.3706(5) 0.1339(3) 0.50880(12) 0.0397(10) Uani 1 1 d . . . C46 C 0.3964(5) 0.1787(3) 0.54473(12) 0.0357(9) 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 0.02071(17) 0.02286(16) 0.02762(17) -0.00087(15) -0.00057(15) 0.00029(16) F1 0.0360(13) 0.0416(14) 0.0370(13) -0.0042(11) -0.0010(10) 0.0029(11) F2 0.0599(18) 0.0564(18) 0.0391(14) -0.0121(12) -0.0077(13) 0.0011(15) F3 0.068(2) 0.087(2) 0.0481(17) -0.0325(16) 0.0111(15) -0.0006(19) F4 0.0467(17) 0.082(2) 0.0639(19) -0.0255(17) 0.0111(15) 0.0058(17) F5 0.0351(14) 0.0567(17) 0.0508(15) -0.0130(13) -0.0021(12) 0.0040(13) F6 0.0401(15) 0.0429(16) 0.0720(19) 0.0099(13) 0.0078(13) 0.0029(12) F7 0.0482(17) 0.0431(17) 0.099(2) 0.0082(16) -0.0019(17) 0.0146(14) F8 0.072(2) 0.0330(15) 0.0682(18) 0.0120(13) -0.0107(16) 0.0014(14) F9 0.071(2) 0.0436(16) 0.0558(17) 0.0080(13) 0.0132(14) -0.0065(15) F10 0.0425(15) 0.0397(15) 0.0575(16) 0.0009(12) 0.0110(12) 0.0014(12) F11 0.0324(13) 0.0530(16) 0.0477(14) -0.0112(12) -0.0013(11) 0.0022(12) F12 0.0512(17) 0.0605(19) 0.0492(16) -0.0069(13) -0.0166(13) -0.0068(14) F13 0.081(2) 0.0635(19) 0.0392(15) -0.0191(14) -0.0050(15) -0.0031(17) F14 0.0634(19) 0.069(2) 0.0488(16) -0.0136(14) 0.0144(14) 0.0122(16) F15 0.0355(14) 0.0618(18) 0.0508(15) -0.0113(13) 0.0019(11) 0.0039(13) O1 0.0221(12) 0.0315(13) 0.0381(14) 0.0057(11) -0.0006(12) -0.0002(12) N1 0.0249(17) 0.0254(15) 0.0304(16) -0.0038(12) -0.0026(12) 0.0011(13) N2 0.0238(16) 0.0256(15) 0.0274(14) -0.0014(12) -0.0020(12) 0.0019(13) N3 0.0241(16) 0.0232(15) 0.0322(17) -0.0005(13) 0.0024(13) -0.0004(13) N4 0.0269(17) 0.0243(16) 0.0321(17) 0.0005(13) 0.0000(13) -0.0018(13) N5 0.0187(14) 0.0373(17) 0.0355(17) -0.0021(14) -0.0026(13) 0.0015(13) C1 0.027(2) 0.0250(18) 0.0315(18) 0.0006(14) 0.0000(16) 0.0021(16) C2 0.036(2) 0.029(2) 0.038(2) 0.0026(16) -0.0031(16) -0.0023(17) C3 0.032(2) 0.033(2) 0.0277(19) 0.0015(15) 0.0011(15) 0.0017(17) C4 0.0270(19) 0.0305(19) 0.0238(17) -0.0012(14) 0.0038(14) 0.0008(15) C5 0.0253(19) 0.0279(18) 0.028(2) -0.0020(14) -0.0007(15) -0.0034(15) C6 0.0261(19) 0.0286(19) 0.0284(19) -0.0005(15) -0.0011(15) -0.0025(16) C7 0.038(2) 0.029(2) 0.039(2) -0.0060(16) 0.0045(18) 0.0009(18) C8 0.039(2) 0.0242(19) 0.037(2) -0.0046(16) -0.0052(17) 0.0014(17) C9 0.0253(18) 0.0214(16) 0.036(2) -0.0027(15) 0.0008(16) -0.0008(14) C10 0.0258(19) 0.0273(19) 0.033(2) 0.0019(15) -0.0032(15) -0.0024(16) C11 0.029(2) 0.0249(18) 0.033(2) 0.0052(15) -0.0011(16) 0.0008(16) C12 0.039(2) 0.030(2) 0.035(2) 0.0025(16) 0.0010(18) 0.0028(18) C13 0.031(2) 0.0309(19) 0.0278(19) -0.0009(15) -0.0019(16) 0.0012(17) C14 0.0238(18) 0.0269(19) 0.0273(17) -0.0015(14) 0.0004(14) 0.0018(14) C15 0.0197(18) 0.0264(19) 0.0311(19) -0.0026(14) 0.0005(14) 0.0022(14) C16 0.0237(18) 0.0289(19) 0.0273(18) -0.0016(15) -0.0014(14) -0.0007(15) C17 0.038(2) 0.0256(18) 0.0336(19) -0.0043(17) -0.0011(15) 0.0008(18) C18 0.036(2) 0.0241(18) 0.042(2) -0.0014(16) -0.0022(16) 0.0039(15) C19 0.0217(18) 0.0210(16) 0.0314(17) 0.0001(13) -0.0037(14) 0.0027(15) C20 0.026(2) 0.052(3) 0.034(2) -0.0081(18) 0.0030(16) 0.0003(19) C21 0.023(2) 0.049(3) 0.049(2) -0.011(2) 0.0056(18) 0.0013(18) C22 0.024(2) 0.052(3) 0.055(3) 0.002(2) -0.0026(18) 0.003(2) C23 0.027(2) 0.046(2) 0.038(2) 0.0016(18) -0.0030(16) 0.0001(18) C24 0.0221(18) 0.032(2) 0.0325(19) 0.0051(15) -0.0019(14) -0.0019(16) C25 0.047(3) 0.078(4) 0.038(3) 0.011(2) 0.002(2) -0.006(3) C26 0.032(2) 0.065(3) 0.042(2) -0.012(2) 0.0079(19) 0.002(2) C27 0.039(2) 0.037(2) 0.043(2) -0.0056(19) -0.0041(19) -0.0100(19) C28 0.032(2) 0.045(3) 0.035(2) -0.0062(18) -0.0011(17) -0.0049(19) C29 0.033(2) 0.0260(19) 0.038(2) -0.0048(16) 0.0024(17) -0.0018(17) C30 0.033(2) 0.0316(19) 0.0314(18) -0.0020(15) 0.0022(18) -0.0011(19) C31 0.041(2) 0.039(2) 0.0291(19) -0.0034(16) -0.0005(18) -0.002(2) C32 0.051(3) 0.049(3) 0.038(2) -0.012(2) 0.010(2) -0.002(2) C33 0.038(3) 0.051(3) 0.046(2) -0.017(2) 0.0081(19) 0.000(2) C34 0.031(2) 0.040(2) 0.041(2) -0.0028(19) 0.0019(18) -0.0020(18) C35 0.033(2) 0.0253(19) 0.0332(19) -0.0007(15) -0.0016(15) -0.0025(16) C36 0.033(2) 0.034(2) 0.045(2) 0.0011(18) 0.0006(18) 0.0005(18) C37 0.040(2) 0.031(2) 0.059(3) 0.0004(19) -0.009(2) 0.006(2) C38 0.054(3) 0.027(2) 0.040(2) 0.0097(17) -0.007(2) 0.000(2) C39 0.056(3) 0.033(2) 0.039(2) 0.0047(18) 0.005(2) -0.006(2) C40 0.037(2) 0.030(2) 0.037(2) -0.0041(16) 0.0012(17) 0.0022(18) C41 0.031(2) 0.0293(19) 0.0274(19) -0.0018(15) 0.0011(15) -0.0012(17) C42 0.031(2) 0.038(2) 0.032(2) 0.0008(17) 0.0017(16) 0.0005(17) C43 0.041(2) 0.040(2) 0.032(2) -0.0020(16) -0.0102(18) -0.005(2) C44 0.052(3) 0.043(2) 0.0272(19) -0.0034(19) -0.0046(17) -0.004(2) C45 0.049(3) 0.038(2) 0.0315(19) -0.0048(18) 0.0076(17) 0.004(2) C46 0.035(2) 0.040(2) 0.0323(19) -0.0020(16) 0.0005(18) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O1 1.786(3) . ? Ge1 N2 1.915(3) . ? Ge1 N4 1.923(3) . ? Ge1 N1 1.927(3) . ? Ge1 N3 1.941(3) . ? F1 C30 1.359(5) . ? F2 C31 1.343(5) . ? F3 C32 1.339(5) . ? F4 C33 1.331(5) . ? F5 C34 1.342(5) . ? F6 C36 1.344(5) . ? F7 C37 1.350(5) . ? F8 C38 1.339(5) . ? F9 C39 1.344(5) . ? F10 C40 1.340(5) . ? F11 C42 1.344(4) . ? F12 C43 1.338(5) . ? F13 C44 1.336(5) . ? F14 C45 1.344(5) . ? F15 C46 1.346(5) . ? O1 N5 1.477(4) . ? N1 C1 1.375(5) . ? N1 C4 1.385(5) . ? N2 C16 1.365(5) . ? N2 C19 1.387(4) . ? N3 C11 1.382(5) . ? N3 C14 1.407(5) . ? N4 C9 1.380(5) . ? N4 C6 1.421(5) . ? N5 C24 1.500(5) . ? N5 C20 1.508(5) . ? C1 C19 1.392(5) . ? C1 C2 1.430(5) . ? C2 C3 1.372(5) . ? C2 H2 0.9500 . ? C3 C4 1.414(5) . ? C3 H3 0.9500 . ? C4 C5 1.392(5) . ? C5 C6 1.395(5) . ? C5 C29 1.479(5) . ? C6 C7 1.416(5) . ? C7 C8 1.359(6) . ? C7 H7 0.9500 . ? C8 C9 1.424(5) . ? C8 H8 0.9500 . ? C9 C10 1.407(5) . ? C10 C11 1.395(5) . ? C10 C35 1.482(5) . ? C11 C12 1.413(5) . ? C12 C13 1.352(5) . ? C12 H12 0.9500 . ? C13 C14 1.425(5) . ? C13 H13 0.9500 . ? C14 C15 1.404(5) . ? C15 C16 1.382(5) . ? C15 C41 1.483(5) . ? C16 C17 1.421(6) . ? C17 C18 1.390(5) . ? C17 H17 0.9500 . ? C18 C19 1.412(5) . ? C18 H18 0.9500 . ? C20 C25 1.528(7) . ? C20 C21 1.532(6) . ? C20 C26 1.540(6) . ? C21 C22 1.506(6) . ? C21 H21B 0.9900 . ? C21 H21A 0.9900 . ? C22 C23 1.496(6) . ? C22 H22B 0.9900 . ? C22 H22A 0.9900 . ? C23 C24 1.530(5) . ? C23 H23B 0.9900 . ? C23 H23A 0.9900 . ? C24 C28 1.519(5) . ? C24 C27 1.548(6) . ? C25 H25A 0.9800 . ? C25 H25C 0.9800 . ? C25 H25B 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27A 0.9800 . ? C28 H28A 0.9800 . ? C28 H28C 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.376(6) . ? C29 C34 1.395(6) . ? C30 C31 1.380(5) . ? C31 C32 1.362(6) . ? C32 C33 1.384(7) . ? C33 C34 1.380(6) . ? C35 C36 1.386(6) . ? C35 C40 1.390(6) . ? C36 C37 1.391(6) . ? C37 C38 1.359(7) . ? C38 C39 1.382(7) . ? C39 C40 1.371(6) . ? C41 C42 1.378(5) . ? C41 C46 1.384(6) . ? C42 C43 1.393(6) . ? C43 C44 1.360(6) . ? C44 C45 1.379(6) . ? C45 C46 1.377(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 N2 110.92(12) . . ? O1 Ge1 N4 98.75(13) . . ? N2 Ge1 N4 150.16(13) . . ? O1 Ge1 N1 110.06(12) . . ? N2 Ge1 N1 79.65(13) . . ? N4 Ge1 N1 87.46(13) . . ? O1 Ge1 N3 99.87(12) . . ? N2 Ge1 N3 87.35(13) . . ? N4 Ge1 N3 90.75(13) . . ? N1 Ge1 N3 149.94(13) . . ? N5 O1 Ge1 119.2(2) . . ? C1 N1 C4 109.2(3) . . ? C1 N1 Ge1 116.5(2) . . ? C4 N1 Ge1 134.2(3) . . ? C16 N2 C19 109.1(3) . . ? C16 N2 Ge1 134.3(3) . . ? C19 N2 Ge1 116.4(2) . . ? C11 N3 C14 106.9(3) . . ? C11 N3 Ge1 125.1(3) . . ? C14 N3 Ge1 127.4(3) . . ? C9 N4 C6 106.6(3) . . ? C9 N4 Ge1 124.8(3) . . ? C6 N4 Ge1 126.9(3) . . ? O1 N5 C24 106.6(3) . . ? O1 N5 C20 106.6(3) . . ? C24 N5 C20 115.9(3) . . ? N1 C1 C19 112.6(3) . . ? N1 C1 C2 108.0(3) . . ? C19 C1 C2 138.4(4) . . ? C3 C2 C1 106.5(3) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 C4 109.5(3) . . ? C2 C3 H3 125.2 . . ? C4 C3 H3 125.2 . . ? N1 C4 C5 120.5(3) . . ? N1 C4 C3 106.6(3) . . ? C5 C4 C3 132.8(3) . . ? C4 C5 C6 122.3(3) . . ? C4 C5 C29 119.5(3) . . ? C6 C5 C29 118.2(3) . . ? C5 C6 C7 126.6(4) . . ? C5 C6 N4 126.0(4) . . ? C7 C6 N4 107.4(3) . . ? C8 C7 C6 109.3(4) . . ? C8 C7 H7 125.3 . . ? C6 C7 H7 125.3 . . ? C7 C8 C9 107.0(4) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? N4 C9 C10 123.8(3) . . ? N4 C9 C8 109.6(3) . . ? C10 C9 C8 126.5(4) . . ? C11 C10 C9 123.7(4) . . ? C11 C10 C35 119.2(3) . . ? C9 C10 C35 117.0(3) . . ? N3 C11 C10 124.0(3) . . ? N3 C11 C12 109.2(3) . . ? C10 C11 C12 126.7(4) . . ? C13 C12 C11 107.8(4) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 108.7(3) . . ? C12 C13 H13 125.6 . . ? C14 C13 H13 125.6 . . ? C15 C14 N3 125.6(3) . . ? C15 C14 C13 127.1(3) . . ? N3 C14 C13 107.3(3) . . ? C16 C15 C14 121.9(3) . . ? C16 C15 C41 118.7(3) . . ? C14 C15 C41 119.3(3) . . ? N2 C16 C15 121.7(3) . . ? N2 C16 C17 107.3(3) . . ? C15 C16 C17 130.7(4) . . ? C18 C17 C16 108.6(3) . . ? C18 C17 H17 125.7 . . ? C16 C17 H17 125.7 . . ? C17 C18 C19 106.4(3) . . ? C17 C18 H18 126.8 . . ? C19 C18 H18 126.8 . . ? N2 C19 C1 112.9(3) . . ? N2 C19 C18 108.5(3) . . ? C1 C19 C18 137.7(4) . . ? N5 C20 C25 115.8(4) . . ? N5 C20 C21 105.5(3) . . ? C25 C20 C21 112.2(4) . . ? N5 C20 C26 107.2(3) . . ? C25 C20 C26 108.1(4) . . ? C21 C20 C26 107.5(4) . . ? C22 C21 C20 113.1(4) . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? H21B C21 H21A 107.8 . . ? C23 C22 C21 109.6(4) . . ? C23 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? C23 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? H22B C22 H22A 108.2 . . ? C22 C23 C24 113.8(3) . . ? C22 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? H23B C23 H23A 107.7 . . ? N5 C24 C28 107.0(3) . . ? N5 C24 C23 106.8(3) . . ? C28 C24 C23 107.8(3) . . ? N5 C24 C27 116.0(3) . . ? C28 C24 C27 107.9(3) . . ? C23 C24 C27 111.0(3) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C20 C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? C24 C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? H28C C28 H28B 109.5 . . ? C30 C29 C34 115.0(4) . . ? C30 C29 C5 122.4(4) . . ? C34 C29 C5 122.6(4) . . ? F1 C30 C29 118.2(3) . . ? F1 C30 C31 117.9(4) . . ? C29 C30 C31 123.8(4) . . ? F2 C31 C32 120.8(4) . . ? F2 C31 C30 120.1(4) . . ? C32 C31 C30 119.1(4) . . ? F3 C32 C31 119.7(4) . . ? F3 C32 C33 120.2(4) . . ? C31 C32 C33 120.1(4) . . ? F4 C33 C34 121.1(4) . . ? F4 C33 C32 119.9(4) . . ? C34 C33 C32 118.9(4) . . ? F5 C34 C33 117.2(4) . . ? F5 C34 C29 119.8(4) . . ? C33 C34 C29 123.0(4) . . ? C36 C35 C40 115.5(4) . . ? C36 C35 C10 122.6(4) . . ? C40 C35 C10 121.9(4) . . ? F6 C36 C35 119.8(4) . . ? F6 C36 C37 117.9(4) . . ? C35 C36 C37 122.2(4) . . ? F7 C37 C38 120.1(4) . . ? F7 C37 C36 119.7(4) . . ? C38 C37 C36 120.1(4) . . ? F8 C38 C37 120.0(4) . . ? F8 C38 C39 120.6(4) . . ? C37 C38 C39 119.5(4) . . ? F9 C39 C40 120.6(4) . . ? F9 C39 C38 119.9(4) . . ? C40 C39 C38 119.5(4) . . ? F10 C40 C39 117.8(4) . . ? F10 C40 C35 119.1(4) . . ? C39 C40 C35 123.1(4) . . ? C42 C41 C46 115.2(4) . . ? C42 C41 C15 122.8(4) . . ? C46 C41 C15 122.0(4) . . ? F11 C42 C41 120.2(4) . . ? F11 C42 C43 117.3(4) . . ? C41 C42 C43 122.5(4) . . ? F12 C43 C44 120.1(4) . . ? F12 C43 C42 119.9(4) . . ? C44 C43 C42 120.0(4) . . ? F13 C44 C43 120.4(4) . . ? F13 C44 C45 119.9(4) . . ? C43 C44 C45 119.6(4) . . ? F14 C45 C46 120.9(4) . . ? F14 C45 C44 120.2(4) . . ? C46 C45 C44 118.9(4) . . ? F15 C46 C45 117.2(4) . . ? F15 C46 C41 119.0(3) . . ? C45 C46 C41 123.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ge1 O1 N5 -40.0(3) . . . . ? N4 Ge1 O1 N5 136.7(2) . . . . ? N1 Ge1 O1 N5 46.3(3) . . . . ? N3 Ge1 O1 N5 -131.0(2) . . . . ? O1 Ge1 N1 C1 -96.3(3) . . . . ? N2 Ge1 N1 C1 12.3(3) . . . . ? N4 Ge1 N1 C1 165.3(3) . . . . ? N3 Ge1 N1 C1 78.2(4) . . . . ? O1 Ge1 N1 C4 85.4(4) . . . . ? N2 Ge1 N1 C4 -165.9(4) . . . . ? N4 Ge1 N1 C4 -13.0(4) . . . . ? N3 Ge1 N1 C4 -100.1(4) . . . . ? O1 Ge1 N2 C16 -88.1(4) . . . . ? N4 Ge1 N2 C16 98.4(4) . . . . ? N1 Ge1 N2 C16 164.3(4) . . . . ? N3 Ge1 N2 C16 11.5(4) . . . . ? O1 Ge1 N2 C19 96.1(3) . . . . ? N4 Ge1 N2 C19 -77.5(4) . . . . ? N1 Ge1 N2 C19 -11.6(3) . . . . ? N3 Ge1 N2 C19 -164.3(3) . . . . ? O1 Ge1 N3 C11 -72.8(3) . . . . ? N2 Ge1 N3 C11 176.5(3) . . . . ? N4 Ge1 N3 C11 26.3(3) . . . . ? N1 Ge1 N3 C11 112.5(4) . . . . ? O1 Ge1 N3 C14 97.1(3) . . . . ? N2 Ge1 N3 C14 -13.7(3) . . . . ? N4 Ge1 N3 C14 -163.9(3) . . . . ? N1 Ge1 N3 C14 -77.6(4) . . . . ? O1 Ge1 N4 C9 71.0(3) . . . . ? N2 Ge1 N4 C9 -115.1(3) . . . . ? N1 Ge1 N4 C9 -179.1(3) . . . . ? N3 Ge1 N4 C9 -29.1(3) . . . . ? O1 Ge1 N4 C6 -92.4(3) . . . . ? N2 Ge1 N4 C6 81.5(4) . . . . ? N1 Ge1 N4 C6 17.5(3) . . . . ? N3 Ge1 N4 C6 167.5(3) . . . . ? Ge1 O1 N5 C24 -118.5(3) . . . . ? Ge1 O1 N5 C20 117.1(3) . . . . ? C4 N1 C1 C19 167.8(3) . . . . ? Ge1 N1 C1 C19 -10.9(4) . . . . ? C4 N1 C1 C2 -3.1(4) . . . . ? Ge1 N1 C1 C2 178.2(2) . . . . ? N1 C1 C2 C3 1.4(4) . . . . ? C19 C1 C2 C3 -165.9(5) . . . . ? C1 C2 C3 C4 0.8(5) . . . . ? C1 N1 C4 C5 -173.6(4) . . . . ? Ge1 N1 C4 C5 4.8(6) . . . . ? C1 N1 C4 C3 3.5(4) . . . . ? Ge1 N1 C4 C3 -178.1(3) . . . . ? C2 C3 C4 N1 -2.6(5) . . . . ? C2 C3 C4 C5 173.9(4) . . . . ? N1 C4 C5 C6 3.7(6) . . . . ? C3 C4 C5 C6 -172.5(4) . . . . ? N1 C4 C5 C29 -177.3(3) . . . . ? C3 C4 C5 C29 6.5(7) . . . . ? C4 C5 C6 C7 -177.6(4) . . . . ? C29 C5 C6 C7 3.4(6) . . . . ? C4 C5 C6 N4 2.4(6) . . . . ? C29 C5 C6 N4 -176.5(4) . . . . ? C9 N4 C6 C5 177.5(4) . . . . ? Ge1 N4 C6 C5 -16.6(6) . . . . ? C9 N4 C6 C7 -2.4(4) . . . . ? Ge1 N4 C6 C7 163.5(3) . . . . ? C5 C6 C7 C8 -179.0(4) . . . . ? N4 C6 C7 C8 0.9(5) . . . . ? C6 C7 C8 C9 0.9(5) . . . . ? C6 N4 C9 C10 -173.4(4) . . . . ? Ge1 N4 C9 C10 20.3(5) . . . . ? C6 N4 C9 C8 3.0(4) . . . . ? Ge1 N4 C9 C8 -163.2(3) . . . . ? C7 C8 C9 N4 -2.5(5) . . . . ? C7 C8 C9 C10 173.8(4) . . . . ? N4 C9 C10 C11 2.4(6) . . . . ? C8 C9 C10 C11 -173.4(4) . . . . ? N4 C9 C10 C35 178.5(3) . . . . ? C8 C9 C10 C35 2.6(6) . . . . ? C14 N3 C11 C10 174.2(4) . . . . ? Ge1 N3 C11 C10 -14.2(6) . . . . ? C14 N3 C11 C12 -2.0(4) . . . . ? Ge1 N3 C11 C12 169.6(3) . . . . ? C9 C10 C11 N3 -5.5(7) . . . . ? C35 C10 C11 N3 178.5(4) . . . . ? C9 C10 C11 C12 170.0(4) . . . . ? C35 C10 C11 C12 -6.0(6) . . . . ? N3 C11 C12 C13 1.0(5) . . . . ? C10 C11 C12 C13 -175.1(4) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C11 N3 C14 C15 -177.5(4) . . . . ? Ge1 N3 C14 C15 11.2(5) . . . . ? C11 N3 C14 C13 2.2(4) . . . . ? Ge1 N3 C14 C13 -169.1(3) . . . . ? C12 C13 C14 C15 178.1(4) . . . . ? C12 C13 C14 N3 -1.6(4) . . . . ? N3 C14 C15 C16 0.5(6) . . . . ? C13 C14 C15 C16 -179.2(4) . . . . ? N3 C14 C15 C41 176.2(3) . . . . ? C13 C14 C15 C41 -3.4(6) . . . . ? C19 N2 C16 C15 171.2(3) . . . . ? Ge1 N2 C16 C15 -4.9(6) . . . . ? C19 N2 C16 C17 -2.6(4) . . . . ? Ge1 N2 C16 C17 -178.7(3) . . . . ? C14 C15 C16 N2 -3.9(6) . . . . ? C41 C15 C16 N2 -179.7(3) . . . . ? C14 C15 C16 C17 168.3(4) . . . . ? C41 C15 C16 C17 -7.5(6) . . . . ? N2 C16 C17 C18 1.4(4) . . . . ? C15 C16 C17 C18 -171.7(4) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C16 N2 C19 C1 -167.8(3) . . . . ? Ge1 N2 C19 C1 9.0(4) . . . . ? C16 N2 C19 C18 2.9(4) . . . . ? Ge1 N2 C19 C18 179.8(2) . . . . ? N1 C1 C19 N2 1.2(5) . . . . ? C2 C1 C19 N2 168.1(5) . . . . ? N1 C1 C19 C18 -165.7(4) . . . . ? C2 C1 C19 C18 1.2(9) . . . . ? C17 C18 C19 N2 -2.0(4) . . . . ? C17 C18 C19 C1 165.3(5) . . . . ? O1 N5 C20 C25 52.6(4) . . . . ? C24 N5 C20 C25 -65.9(5) . . . . ? O1 N5 C20 C21 177.4(3) . . . . ? C24 N5 C20 C21 59.0(4) . . . . ? O1 N5 C20 C26 -68.2(4) . . . . ? C24 N5 C20 C26 173.4(3) . . . . ? N5 C20 C21 C22 -56.9(5) . . . . ? C25 C20 C21 C22 70.2(5) . . . . ? C26 C20 C21 C22 -171.1(4) . . . . ? C20 C21 C22 C23 57.0(5) . . . . ? C21 C22 C23 C24 -55.2(5) . . . . ? O1 N5 C24 C28 68.8(4) . . . . ? C20 N5 C24 C28 -172.9(3) . . . . ? O1 N5 C24 C23 -176.1(3) . . . . ? C20 N5 C24 C23 -57.7(4) . . . . ? O1 N5 C24 C27 -51.7(4) . . . . ? C20 N5 C24 C27 66.7(5) . . . . ? C22 C23 C24 N5 54.0(5) . . . . ? C22 C23 C24 C28 168.7(4) . . . . ? C22 C23 C24 C27 -73.3(5) . . . . ? C4 C5 C29 C30 67.9(5) . . . . ? C6 C5 C29 C30 -113.1(4) . . . . ? C4 C5 C29 C34 -113.0(5) . . . . ? C6 C5 C29 C34 66.1(6) . . . . ? C34 C29 C30 F1 -177.5(4) . . . . ? C5 C29 C30 F1 1.7(6) . . . . ? C34 C29 C30 C31 -1.1(6) . . . . ? C5 C29 C30 C31 178.1(4) . . . . ? F1 C30 C31 F2 -2.0(6) . . . . ? C29 C30 C31 F2 -178.4(4) . . . . ? F1 C30 C31 C32 177.8(4) . . . . ? C29 C30 C31 C32 1.4(7) . . . . ? F2 C31 C32 F3 -1.9(7) . . . . ? C30 C31 C32 F3 178.3(4) . . . . ? F2 C31 C32 C33 178.6(4) . . . . ? C30 C31 C32 C33 -1.2(7) . . . . ? F3 C32 C33 F4 1.3(8) . . . . ? C31 C32 C33 F4 -179.2(4) . . . . ? F3 C32 C33 C34 -178.7(5) . . . . ? C31 C32 C33 C34 0.8(8) . . . . ? F4 C33 C34 F5 -0.3(7) . . . . ? C32 C33 C34 F5 179.6(4) . . . . ? F4 C33 C34 C29 179.5(4) . . . . ? C32 C33 C34 C29 -0.6(8) . . . . ? C30 C29 C34 F5 -179.5(4) . . . . ? C5 C29 C34 F5 1.3(6) . . . . ? C30 C29 C34 C33 0.7(7) . . . . ? C5 C29 C34 C33 -178.5(4) . . . . ? C11 C10 C35 C36 109.9(5) . . . . ? C9 C10 C35 C36 -66.3(5) . . . . ? C11 C10 C35 C40 -71.4(5) . . . . ? C9 C10 C35 C40 112.3(4) . . . . ? C40 C35 C36 F6 178.9(4) . . . . ? C10 C35 C36 F6 -2.3(6) . . . . ? C40 C35 C36 C37 0.2(6) . . . . ? C10 C35 C36 C37 179.0(4) . . . . ? F6 C36 C37 F7 2.5(6) . . . . ? C35 C36 C37 F7 -178.8(4) . . . . ? F6 C36 C37 C38 -178.6(4) . . . . ? C35 C36 C37 C38 0.2(7) . . . . ? F7 C37 C38 F8 -0.7(7) . . . . ? C36 C37 C38 F8 -179.6(4) . . . . ? F7 C37 C38 C39 179.4(4) . . . . ? C36 C37 C38 C39 0.5(7) . . . . ? F8 C38 C39 F9 0.6(7) . . . . ? C37 C38 C39 F9 -179.6(4) . . . . ? F8 C38 C39 C40 178.6(4) . . . . ? C37 C38 C39 C40 -1.5(7) . . . . ? F9 C39 C40 F10 -0.7(6) . . . . ? C38 C39 C40 F10 -178.7(4) . . . . ? F9 C39 C40 C35 180.0(4) . . . . ? C38 C39 C40 C35 2.0(7) . . . . ? C36 C35 C40 F10 179.4(4) . . . . ? C10 C35 C40 F10 0.6(6) . . . . ? C36 C35 C40 C39 -1.3(6) . . . . ? C10 C35 C40 C39 180.0(4) . . . . ? C16 C15 C41 C42 106.6(5) . . . . ? C14 C15 C41 C42 -69.3(5) . . . . ? C16 C15 C41 C46 -73.1(5) . . . . ? C14 C15 C41 C46 111.0(4) . . . . ? C46 C41 C42 F11 179.8(4) . . . . ? C15 C41 C42 F11 0.1(6) . . . . ? C46 C41 C42 C43 1.6(6) . . . . ? C15 C41 C42 C43 -178.2(4) . . . . ? F11 C42 C43 F12 0.6(6) . . . . ? C41 C42 C43 F12 178.9(4) . . . . ? F11 C42 C43 C44 -178.2(4) . . . . ? C41 C42 C43 C44 0.1(7) . . . . ? F12 C43 C44 F13 1.9(7) . . . . ? C42 C43 C44 F13 -179.3(4) . . . . ? F12 C43 C44 C45 179.1(4) . . . . ? C42 C43 C44 C45 -2.1(7) . . . . ? F13 C44 C45 F14 -1.0(7) . . . . ? C43 C44 C45 F14 -178.2(4) . . . . ? F13 C44 C45 C46 179.5(4) . . . . ? C43 C44 C45 C46 2.3(7) . . . . ? F14 C45 C46 F15 -0.2(6) . . . . ? C44 C45 C46 F15 179.4(4) . . . . ? F14 C45 C46 C41 180.0(4) . . . . ? C44 C45 C46 C41 -0.5(7) . . . . ? C42 C41 C46 F15 178.8(4) . . . . ? C15 C41 C46 F15 -1.5(6) . . . . ? C42 C41 C46 C45 -1.4(6) . . . . ? C15 C41 C46 C45 178.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.451 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.072 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.009 0.750 0.000 371 131 ' ' 2 -0.026 0.250 0.500 371 131 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 945438' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(TPFC)Ge-OH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C37 H9 F15 Ge N4 O), C6 H14' _chemical_formula_sum 'C80 H32 F30 Ge2 N8 O2' _chemical_formula_weight 1852.32 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.016(4) _cell_length_b 15.843(5) _cell_length_c 18.314(6) _cell_angle_alpha 102.173(4) _cell_angle_beta 103.316(5) _cell_angle_gamma 99.283(3) _cell_volume 3503.9(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11898 _cell_measurement_theta_min 1.1827 _cell_measurement_theta_max 27.4615 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6114 _exptl_absorpt_correction_T_max 1.0000 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38156 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12355 _reflns_number_gt 10569 _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 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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^)+(0.0456P)^2^+6.8585P] 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 12355 _refine_ls_number_parameters 1101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _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 0.65696(5) 0.67065(4) 0.20327(3) 0.03587(16) Uani 1 1 d . . . Ge2 Ge 0.23573(4) 0.66915(3) 0.07962(3) 0.03335(16) Uani 1 1 d . . . F1 F 0.7116(3) 0.7754(2) -0.07538(18) 0.0493(8) Uani 1 1 d . . . F2 F 0.6227(3) 0.8429(2) -0.19025(19) 0.0609(10) Uani 1 1 d . . . F3 F 0.4506(3) 0.9200(2) -0.1829(2) 0.0658(10) Uani 1 1 d . . . F4 F 0.3738(3) 0.9314(2) -0.0571(2) 0.0547(9) Uani 1 1 d . . . F5 F 0.4600(3) 0.8639(2) 0.05838(18) 0.0459(8) Uani 1 1 d . . . F6 F 0.9473(3) 0.9875(3) 0.4017(2) 0.0690(11) Uani 1 1 d . . . F7 F 0.9713(4) 1.1413(3) 0.5082(3) 0.0905(14) Uani 1 1 d . . . F8 F 0.8054(4) 1.1745(2) 0.5686(2) 0.0803(13) Uani 1 1 d . . . F9 F 0.6152(3) 1.0537(3) 0.5218(2) 0.0731(11) Uani 1 1 d . . . F10 F 0.5910(3) 0.9011(2) 0.4163(2) 0.0610(10) Uani 1 1 d . . . F11 F 0.9009(4) 0.4545(4) 0.3503(3) 0.0998(16) Uani 1 1 d . . . F12 F 0.9249(5) 0.3503(4) 0.4479(4) 0.148(3) Uani 1 1 d . . . F13 F 0.7775(6) 0.3241(4) 0.5301(3) 0.139(2) Uani 1 1 d . . . F14 F 0.6076(4) 0.4024(3) 0.5123(3) 0.1012(16) Uani 1 1 d . . . F15 F 0.5843(3) 0.5083(3) 0.4160(2) 0.0673(10) Uani 1 1 d . . . F16 F -0.0686(3) 0.8127(3) -0.1022(2) 0.0668(11) Uani 1 1 d . . . F17 F -0.1419(4) 0.8679(3) -0.2287(3) 0.0950(15) Uani 1 1 d . . . F18 F -0.0225(4) 0.8762(3) -0.3323(2) 0.1001(16) Uani 1 1 d . . . F19 F 0.1727(4) 0.8309(3) -0.3052(2) 0.0767(12) Uani 1 1 d . . . F20 F 0.2472(3) 0.7771(2) -0.1777(2) 0.0553(9) Uani 1 1 d . . . F21 F 0.1780(3) 0.9617(2) 0.3074(2) 0.0598(9) Uani 1 1 d . . . F22 F 0.2727(3) 1.1201(2) 0.4059(2) 0.0729(11) Uani 1 1 d . . . F23 F 0.4861(3) 1.1897(2) 0.4291(2) 0.0741(12) Uani 1 1 d . . . F24 F 0.6020(3) 1.0981(2) 0.3494(2) 0.0690(11) Uani 1 1 d . . . F25 F 0.5072(3) 0.9378(2) 0.2510(2) 0.0609(10) Uani 1 1 d . . . F26 F 0.4275(3) 0.4545(3) 0.2229(2) 0.0642(10) Uani 1 1 d . . . F27 F 0.4538(4) 0.3376(3) 0.3097(2) 0.0837(13) Uani 1 1 d . . . F28 F 0.3165(4) 0.3081(3) 0.3987(3) 0.1014(16) Uani 1 1 d . . . F29 F 0.1534(4) 0.3953(3) 0.3979(2) 0.0860(14) Uani 1 1 d . . . F30 F 0.1276(3) 0.5118(2) 0.31202(19) 0.0567(9) Uani 1 1 d . . . O1 O 0.5156(3) 0.6554(2) 0.1954(2) 0.0428(9) Uani 1 1 d . . . H1 H 0.5137 0.6781 0.2407 0.051 Uiso 1 1 d R . . O2 O 0.3646(3) 0.6760(2) 0.0646(2) 0.0367(8) Uani 1 1 d . . . H2A H 0.4087 0.6745 0.1055 0.044 Uiso 1 1 d R . . N1 N 0.7261(4) 0.6956(3) 0.3123(2) 0.0370(10) Uani 1 1 d . . . N2 N 0.6848(3) 0.5539(3) 0.1928(2) 0.0360(10) Uani 1 1 d . . . N3 N 0.6526(4) 0.6395(3) 0.0962(2) 0.0376(10) Uani 1 1 d . . . N4 N 0.6939(3) 0.7914(3) 0.2016(2) 0.0339(10) Uani 1 1 d . . . N5 N 0.2607(4) 0.6950(3) 0.1906(2) 0.0360(10) Uani 1 1 d . . . N6 N 0.2061(3) 0.7831(3) 0.0767(2) 0.0348(10) Uani 1 1 d . . . N7 N 0.1444(3) 0.6254(3) -0.0248(2) 0.0342(10) Uani 1 1 d . . . N8 N 0.1846(3) 0.5475(3) 0.0767(2) 0.0368(10) Uani 1 1 d . . . C1 C 0.6429(4) 0.5510(3) 0.0629(3) 0.0363(12) Uani 1 1 d . . . C2 C 0.6128(4) 0.5368(4) -0.0189(3) 0.0393(13) Uani 1 1 d . . . H2 H 0.6030 0.4825 -0.0564 0.047 Uiso 1 1 calc R . . C3 C 0.6006(4) 0.6166(4) -0.0334(3) 0.0382(12) Uani 1 1 d . . . H3 H 0.5785 0.6269 -0.0834 0.046 Uiso 1 1 calc R . . C4 C 0.6265(4) 0.6816(3) 0.0388(3) 0.0354(12) Uani 1 1 d . . . C5 C 0.6307(4) 0.7729(3) 0.0586(3) 0.0358(12) Uani 1 1 d . . . C6 C 0.5884(4) 0.8155(3) -0.0041(3) 0.0369(12) Uani 1 1 d . . . C7 C 0.6274(4) 0.8130(4) -0.0695(3) 0.0392(13) Uani 1 1 d . . . C8 C 0.5823(5) 0.8477(4) -0.1281(3) 0.0469(15) Uani 1 1 d . . . C9 C 0.4966(5) 0.8868(4) -0.1253(3) 0.0471(15) Uani 1 1 d . . . C10 C 0.4571(5) 0.8915(3) -0.0612(3) 0.0425(13) Uani 1 1 d . . . C11 C 0.5028(5) 0.8571(4) -0.0022(3) 0.0402(13) Uani 1 1 d . . . C12 C 0.6692(4) 0.8243(3) 0.1356(3) 0.0363(12) Uani 1 1 d . . . C13 C 0.6893(4) 0.9177(3) 0.1612(3) 0.0355(12) Uani 1 1 d . . . H13 H 0.6801 0.9570 0.1288 0.043 Uiso 1 1 calc R . . C14 C 0.7240(4) 0.9417(4) 0.2402(3) 0.0399(13) Uani 1 1 d . . . H14 H 0.7437 1.0005 0.2723 0.048 Uiso 1 1 calc R . . C15 C 0.7259(4) 0.8637(3) 0.2665(3) 0.0389(13) Uani 1 1 d . . . C16 C 0.7496(4) 0.8568(3) 0.3427(3) 0.0391(13) Uani 1 1 d . . . C17 C 0.7677(5) 0.9398(4) 0.4053(3) 0.0425(14) Uani 1 1 d . . . C18 C 0.8631(5) 1.0024(4) 0.4305(4) 0.0530(16) Uani 1 1 d . . . C19 C 0.8760(6) 1.0815(4) 0.4853(4) 0.0606(18) Uani 1 1 d . . . C20 C 0.7925(6) 1.0978(4) 0.5164(3) 0.0565(18) Uani 1 1 d . . . C21 C 0.6978(5) 1.0366(4) 0.4922(3) 0.0509(15) Uani 1 1 d . . . C22 C 0.6859(5) 0.9593(4) 0.4390(3) 0.0436(14) Uani 1 1 d . . . C23 C 0.7515(4) 0.7782(4) 0.3651(3) 0.0392(13) Uani 1 1 d . . . C24 C 0.7830(5) 0.7666(4) 0.4410(3) 0.0454(14) Uani 1 1 d . . . H24 H 0.8049 0.8124 0.4879 0.055 Uiso 1 1 calc R . . C25 C 0.7766(5) 0.6792(4) 0.4358(3) 0.0445(14) Uani 1 1 d . . . H25 H 0.7924 0.6532 0.4782 0.053 Uiso 1 1 calc R . . C26 C 0.7421(4) 0.6328(4) 0.3552(3) 0.0410(13) Uani 1 1 d . . . C27 C 0.7267(5) 0.5419(4) 0.3245(3) 0.0428(14) Uani 1 1 d . . . C28 C 0.7412(5) 0.4842(4) 0.3798(3) 0.0489(15) Uani 1 1 d . . . C29 C 0.8264(7) 0.4421(5) 0.3896(4) 0.071(2) Uani 1 1 d . . . C30 C 0.8404(8) 0.3885(6) 0.4402(5) 0.094(3) Uani 1 1 d . . . C31 C 0.7653(9) 0.3753(5) 0.4806(5) 0.091(3) Uani 1 1 d . . . C32 C 0.6812(7) 0.4158(5) 0.4720(4) 0.075(2) Uani 1 1 d . . . C33 C 0.6682(6) 0.4701(4) 0.4229(4) 0.0552(16) Uani 1 1 d . . . C34 C 0.7001(4) 0.5028(4) 0.2449(3) 0.0403(13) Uani 1 1 d . . . C35 C 0.6861(5) 0.4146(4) 0.1994(3) 0.0447(14) Uani 1 1 d . . . H35 H 0.6915 0.3642 0.2192 0.054 Uiso 1 1 calc R . . C36 C 0.6634(5) 0.4143(4) 0.1225(3) 0.0433(14) Uani 1 1 d . . . H36 H 0.6507 0.3642 0.0799 0.052 Uiso 1 1 calc R . . C37 C 0.6624(4) 0.5021(3) 0.1183(3) 0.0358(12) Uani 1 1 d . . . C38 C 0.1090(4) 0.5346(3) -0.0529(3) 0.0371(12) Uani 1 1 d . . . C39 C 0.0576(4) 0.5161(4) -0.1331(3) 0.0413(13) Uani 1 1 d . . . H39 H 0.0266 0.4591 -0.1677 0.050 Uiso 1 1 calc R . . C40 C 0.0607(5) 0.5964(4) -0.1520(3) 0.0435(14) Uani 1 1 d . . . H40 H 0.0324 0.6043 -0.2021 0.052 Uiso 1 1 calc R . . C41 C 0.1139(4) 0.6653(4) -0.0828(3) 0.0391(13) Uani 1 1 d . . . C42 C 0.1311(4) 0.7572(3) -0.0666(3) 0.0380(12) Uani 1 1 d . . . C43 C 0.0936(5) 0.7951(3) -0.1339(3) 0.0396(13) Uani 1 1 d . . . C44 C 0.1507(5) 0.8005(4) -0.1880(3) 0.0447(14) Uani 1 1 d . . . C45 C 0.1133(6) 0.8275(4) -0.2544(3) 0.0550(17) Uani 1 1 d . . . C46 C 0.0141(6) 0.8504(5) -0.2678(4) 0.0652(19) Uani 1 1 d . . . C47 C -0.0458(6) 0.8461(5) -0.2160(4) 0.0653(19) Uani 1 1 d . . . C48 C -0.0055(5) 0.8188(4) -0.1500(3) 0.0491(15) Uani 1 1 d . . . C49 C 0.1728(4) 0.8121(3) 0.0084(3) 0.0351(12) Uani 1 1 d . . . C50 C 0.1883(4) 0.9057(3) 0.0319(3) 0.0402(13) Uani 1 1 d . . . H50 H 0.1711 0.9426 -0.0017 0.048 Uiso 1 1 calc R . . C51 C 0.2312(4) 0.9339(3) 0.1096(3) 0.0386(13) Uani 1 1 d . . . H51 H 0.2491 0.9936 0.1398 0.046 Uiso 1 1 calc R . . C52 C 0.2451(4) 0.8583(4) 0.1384(3) 0.0393(13) Uani 1 1 d . . . C53 C 0.2892(4) 0.8571(3) 0.2155(3) 0.0371(12) Uani 1 1 d . . . C54 C 0.3386(4) 0.9443(3) 0.2742(3) 0.0357(12) Uani 1 1 d . . . C55 C 0.2831(5) 0.9934(4) 0.3151(3) 0.0427(13) Uani 1 1 d . . . C56 C 0.3312(5) 1.0761(4) 0.3674(3) 0.0474(15) Uani 1 1 d . . . C57 C 0.4385(6) 1.1100(4) 0.3782(4) 0.0540(16) Uani 1 1 d . . . C58 C 0.4962(5) 1.0645(4) 0.3397(4) 0.0477(14) Uani 1 1 d . . . C59 C 0.4471(5) 0.9822(4) 0.2880(3) 0.0431(13) Uani 1 1 d . . . C60 C 0.2976(4) 0.7792(3) 0.2401(3) 0.0360(12) Uani 1 1 d . . . C61 C 0.3407(5) 0.7727(4) 0.3165(3) 0.0427(13) Uani 1 1 d . . . H61 H 0.3716 0.8207 0.3614 0.051 Uiso 1 1 calc R . . C62 C 0.3302(5) 0.6859(4) 0.3142(3) 0.0438(14) Uani 1 1 d . . . H62 H 0.3525 0.6625 0.3575 0.053 Uiso 1 1 calc R . . C63 C 0.2804(4) 0.6354(3) 0.2367(3) 0.0361(12) Uani 1 1 d . . . C64 C 0.2553(4) 0.5431(4) 0.2089(3) 0.0374(12) Uani 1 1 d . . . C65 C 0.2761(4) 0.4867(4) 0.2635(3) 0.0398(13) Uani 1 1 d . . . C66 C 0.3588(5) 0.4408(4) 0.2660(3) 0.0476(15) Uani 1 1 d . . . C67 C 0.3726(6) 0.3809(4) 0.3106(4) 0.0607(18) Uani 1 1 d . . . C68 C 0.3033(6) 0.3662(4) 0.3551(4) 0.0627(19) Uani 1 1 d . . . C69 C 0.2220(6) 0.4104(5) 0.3551(4) 0.0597(18) Uani 1 1 d . . . C70 C 0.2095(5) 0.4704(4) 0.3104(3) 0.0452(14) Uani 1 1 d . . . C71 C 0.2050(4) 0.4998(3) 0.1307(3) 0.0371(12) Uani 1 1 d . . . C72 C 0.1631(4) 0.4084(4) 0.0907(3) 0.0415(13) Uani 1 1 d . . . H72 H 0.1661 0.3599 0.1134 0.050 Uiso 1 1 calc R . . C73 C 0.1180(4) 0.4028(4) 0.0141(3) 0.0391(13) Uani 1 1 d . . . H73 H 0.0835 0.3501 -0.0257 0.047 Uiso 1 1 calc R . . C74 C 0.1325(4) 0.4907(3) 0.0054(3) 0.0373(12) Uani 1 1 d . . . C75 C -0.0025(6) 0.6834(4) 0.3032(4) 0.0611(18) Uani 1 1 d . . . H75B H -0.0679 0.6377 0.2743 0.092 Uiso 1 1 calc R . . H75C H 0.0049 0.6935 0.3590 0.092 Uiso 1 1 calc R . . H75A H 0.0610 0.6638 0.2916 0.092 Uiso 1 1 calc R . . C76 C -0.0110(5) 0.7691(4) 0.2794(4) 0.0574(17) Uani 1 1 d . . . H76B H -0.0700 0.7920 0.2972 0.069 Uiso 1 1 calc R . . H76A H 0.0573 0.8135 0.3065 0.069 Uiso 1 1 calc R . . C77 C -0.0327(5) 0.7597(4) 0.1934(3) 0.0485(15) Uani 1 1 d . . . H77B H -0.1014 0.7158 0.1662 0.058 Uiso 1 1 calc R . . H77A H 0.0260 0.7366 0.1754 0.058 Uiso 1 1 calc R . . C78 C -0.0402(5) 0.8467(4) 0.1709(4) 0.0526(16) Uani 1 1 d . . . H78B H -0.0942 0.8722 0.1933 0.063 Uiso 1 1 calc R . . H78A H 0.0307 0.8888 0.1950 0.063 Uiso 1 1 calc R . . C79 C -0.0708(5) 0.8397(4) 0.0852(4) 0.0511(15) Uani 1 1 d . . . H79B H -0.1413 0.7974 0.0604 0.061 Uiso 1 1 calc R . . H79A H -0.0159 0.8161 0.0624 0.061 Uiso 1 1 calc R . . C80 C -0.0789(6) 0.9285(4) 0.0674(4) 0.0630(18) Uani 1 1 d . . . H80A H -0.1000 0.9204 0.0111 0.095 Uiso 1 1 calc R . . H80B H -0.0086 0.9701 0.0903 0.095 Uiso 1 1 calc R . . H80C H -0.1335 0.9520 0.0896 0.095 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 0.0463(4) 0.0332(3) 0.0342(3) 0.0147(2) 0.0116(3) 0.0172(3) Ge2 0.0424(3) 0.0284(3) 0.0329(3) 0.0118(2) 0.0100(2) 0.0134(2) F1 0.060(2) 0.052(2) 0.0477(19) 0.0231(16) 0.0223(16) 0.0203(17) F2 0.086(3) 0.062(2) 0.046(2) 0.0246(18) 0.0257(19) 0.022(2) F3 0.094(3) 0.066(2) 0.050(2) 0.0356(19) 0.012(2) 0.036(2) F4 0.063(2) 0.048(2) 0.062(2) 0.0251(17) 0.0128(17) 0.0307(17) F5 0.058(2) 0.0449(19) 0.0497(19) 0.0219(15) 0.0241(16) 0.0261(16) F6 0.061(2) 0.069(3) 0.075(3) 0.021(2) 0.019(2) 0.005(2) F7 0.091(3) 0.062(3) 0.093(3) 0.009(2) 0.006(3) -0.013(2) F8 0.122(4) 0.044(2) 0.058(2) -0.0051(18) 0.003(2) 0.026(2) F9 0.095(3) 0.076(3) 0.057(2) 0.005(2) 0.028(2) 0.049(2) F10 0.058(2) 0.062(2) 0.055(2) -0.0008(18) 0.0155(18) 0.0140(19) F11 0.102(4) 0.137(4) 0.110(4) 0.073(3) 0.050(3) 0.083(3) F12 0.190(6) 0.165(6) 0.153(5) 0.105(5) 0.051(5) 0.133(5) F13 0.244(7) 0.114(4) 0.106(4) 0.091(4) 0.053(4) 0.077(5) F14 0.147(5) 0.088(3) 0.087(3) 0.049(3) 0.056(3) 0.010(3) F15 0.075(3) 0.071(3) 0.072(3) 0.031(2) 0.035(2) 0.024(2) F16 0.061(2) 0.088(3) 0.076(3) 0.045(2) 0.029(2) 0.039(2) F17 0.082(3) 0.132(4) 0.100(3) 0.069(3) 0.019(3) 0.063(3) F18 0.128(4) 0.123(4) 0.070(3) 0.069(3) 0.015(3) 0.042(3) F19 0.113(3) 0.074(3) 0.055(2) 0.031(2) 0.036(2) 0.018(2) F20 0.061(2) 0.055(2) 0.062(2) 0.0210(18) 0.0272(18) 0.0214(18) F21 0.057(2) 0.053(2) 0.071(2) 0.0038(18) 0.0286(19) 0.0170(18) F22 0.098(3) 0.049(2) 0.073(3) -0.0018(19) 0.034(2) 0.028(2) F23 0.095(3) 0.040(2) 0.066(3) -0.0009(18) 0.000(2) 0.006(2) F24 0.058(2) 0.061(2) 0.075(3) 0.019(2) 0.0006(19) 0.0011(19) F25 0.052(2) 0.060(2) 0.074(2) 0.0106(19) 0.0253(19) 0.0185(18) F26 0.071(2) 0.075(3) 0.065(2) 0.031(2) 0.027(2) 0.041(2) F27 0.106(3) 0.071(3) 0.084(3) 0.033(2) 0.010(2) 0.054(3) F28 0.147(4) 0.081(3) 0.096(3) 0.068(3) 0.023(3) 0.039(3) F29 0.096(3) 0.109(4) 0.077(3) 0.064(3) 0.037(2) 0.018(3) F30 0.059(2) 0.072(2) 0.055(2) 0.0293(19) 0.0253(17) 0.0267(19) O1 0.042(2) 0.051(2) 0.044(2) 0.0212(19) 0.0133(18) 0.0176(18) O2 0.042(2) 0.035(2) 0.036(2) 0.0114(16) 0.0106(16) 0.0149(17) N1 0.055(3) 0.033(2) 0.029(2) 0.0136(19) 0.010(2) 0.022(2) N2 0.047(3) 0.034(2) 0.030(2) 0.0114(19) 0.008(2) 0.016(2) N3 0.049(3) 0.031(2) 0.037(2) 0.015(2) 0.012(2) 0.014(2) N4 0.047(3) 0.033(2) 0.027(2) 0.0145(19) 0.0109(19) 0.017(2) N5 0.053(3) 0.027(2) 0.034(2) 0.0116(19) 0.014(2) 0.014(2) N6 0.045(3) 0.030(2) 0.032(2) 0.0119(19) 0.009(2) 0.012(2) N7 0.043(3) 0.030(2) 0.029(2) 0.0087(18) 0.0073(19) 0.011(2) N8 0.045(3) 0.032(2) 0.036(2) 0.014(2) 0.008(2) 0.011(2) C1 0.039(3) 0.032(3) 0.046(3) 0.015(2) 0.017(2) 0.013(2) C2 0.055(3) 0.034(3) 0.038(3) 0.013(2) 0.019(3) 0.020(3) C3 0.048(3) 0.043(3) 0.030(3) 0.015(2) 0.015(2) 0.017(3) C4 0.040(3) 0.037(3) 0.037(3) 0.019(2) 0.012(2) 0.016(2) C5 0.039(3) 0.038(3) 0.040(3) 0.018(2) 0.016(2) 0.018(2) C6 0.044(3) 0.033(3) 0.040(3) 0.016(2) 0.013(2) 0.014(2) C7 0.044(3) 0.035(3) 0.045(3) 0.012(3) 0.018(3) 0.016(3) C8 0.070(4) 0.041(3) 0.038(3) 0.020(3) 0.019(3) 0.014(3) C9 0.064(4) 0.037(3) 0.042(3) 0.022(3) 0.005(3) 0.016(3) C10 0.053(4) 0.030(3) 0.047(3) 0.014(3) 0.005(3) 0.020(3) C11 0.049(3) 0.038(3) 0.034(3) 0.014(2) 0.006(3) 0.013(3) C12 0.045(3) 0.034(3) 0.041(3) 0.018(2) 0.017(3) 0.020(2) C13 0.046(3) 0.030(3) 0.038(3) 0.017(2) 0.013(2) 0.018(2) C14 0.046(3) 0.034(3) 0.042(3) 0.012(2) 0.011(3) 0.016(3) C15 0.048(3) 0.030(3) 0.046(3) 0.015(2) 0.018(3) 0.016(2) C16 0.054(3) 0.030(3) 0.035(3) 0.010(2) 0.009(3) 0.015(3) C17 0.060(4) 0.038(3) 0.029(3) 0.014(2) 0.003(3) 0.012(3) C18 0.062(4) 0.055(4) 0.046(4) 0.016(3) 0.015(3) 0.020(3) C19 0.067(5) 0.045(4) 0.057(4) 0.016(3) -0.002(3) -0.001(3) C20 0.089(5) 0.040(4) 0.036(3) 0.004(3) 0.004(3) 0.030(4) C21 0.068(4) 0.044(4) 0.041(3) 0.012(3) 0.007(3) 0.021(3) C22 0.063(4) 0.035(3) 0.034(3) 0.006(2) 0.013(3) 0.018(3) C23 0.048(3) 0.036(3) 0.036(3) 0.010(2) 0.012(3) 0.016(3) C24 0.063(4) 0.045(3) 0.031(3) 0.011(3) 0.013(3) 0.018(3) C25 0.062(4) 0.044(3) 0.037(3) 0.023(3) 0.015(3) 0.019(3) C26 0.049(3) 0.046(3) 0.038(3) 0.024(3) 0.014(3) 0.020(3) C27 0.057(4) 0.040(3) 0.040(3) 0.022(3) 0.010(3) 0.023(3) C28 0.076(4) 0.035(3) 0.041(3) 0.018(3) 0.011(3) 0.025(3) C29 0.092(6) 0.077(5) 0.073(5) 0.047(4) 0.034(4) 0.045(4) C30 0.140(8) 0.106(7) 0.073(6) 0.052(5) 0.031(5) 0.085(6) C31 0.158(9) 0.070(5) 0.073(6) 0.052(5) 0.034(6) 0.052(6) C32 0.122(7) 0.057(5) 0.052(4) 0.025(4) 0.031(4) 0.012(5) C33 0.081(5) 0.046(4) 0.045(4) 0.020(3) 0.020(3) 0.017(3) C34 0.048(3) 0.041(3) 0.043(3) 0.021(3) 0.015(3) 0.022(3) C35 0.057(4) 0.033(3) 0.056(4) 0.021(3) 0.021(3) 0.025(3) C36 0.055(4) 0.035(3) 0.049(3) 0.015(3) 0.019(3) 0.023(3) C37 0.042(3) 0.034(3) 0.037(3) 0.012(2) 0.011(2) 0.020(2) C38 0.041(3) 0.025(3) 0.043(3) 0.008(2) 0.008(2) 0.008(2) C39 0.048(3) 0.031(3) 0.043(3) 0.006(2) 0.011(3) 0.010(3) C40 0.050(3) 0.046(3) 0.033(3) 0.009(3) 0.005(3) 0.014(3) C41 0.043(3) 0.045(3) 0.031(3) 0.014(2) 0.006(2) 0.015(3) C42 0.046(3) 0.035(3) 0.041(3) 0.019(2) 0.009(3) 0.020(3) C43 0.049(3) 0.032(3) 0.040(3) 0.015(2) 0.009(3) 0.014(3) C44 0.055(4) 0.036(3) 0.047(3) 0.016(3) 0.012(3) 0.016(3) C45 0.083(5) 0.043(4) 0.044(4) 0.019(3) 0.027(3) 0.003(3) C46 0.081(5) 0.072(5) 0.051(4) 0.040(4) 0.008(4) 0.025(4) C47 0.065(4) 0.076(5) 0.062(4) 0.037(4) 0.004(4) 0.030(4) C48 0.059(4) 0.052(4) 0.045(3) 0.023(3) 0.015(3) 0.020(3) C49 0.044(3) 0.033(3) 0.037(3) 0.016(2) 0.015(2) 0.018(2) C50 0.052(3) 0.033(3) 0.044(3) 0.016(2) 0.016(3) 0.019(3) C51 0.048(3) 0.030(3) 0.044(3) 0.013(2) 0.017(3) 0.016(2) C52 0.046(3) 0.035(3) 0.044(3) 0.015(3) 0.016(3) 0.018(3) C53 0.048(3) 0.032(3) 0.037(3) 0.008(2) 0.017(3) 0.015(2) C54 0.047(3) 0.031(3) 0.035(3) 0.018(2) 0.009(2) 0.016(2) C55 0.045(3) 0.040(3) 0.047(3) 0.015(3) 0.012(3) 0.016(3) C56 0.072(4) 0.036(3) 0.040(3) 0.005(3) 0.020(3) 0.026(3) C57 0.066(4) 0.031(3) 0.053(4) 0.012(3) -0.004(3) 0.009(3) C58 0.048(4) 0.039(3) 0.052(4) 0.015(3) 0.003(3) 0.006(3) C59 0.053(4) 0.042(3) 0.040(3) 0.015(3) 0.015(3) 0.017(3) C60 0.043(3) 0.035(3) 0.036(3) 0.010(2) 0.016(2) 0.015(2) C61 0.054(4) 0.039(3) 0.036(3) 0.009(2) 0.012(3) 0.013(3) C62 0.060(4) 0.041(3) 0.037(3) 0.018(3) 0.015(3) 0.017(3) C63 0.042(3) 0.036(3) 0.035(3) 0.017(2) 0.011(2) 0.013(2) C64 0.044(3) 0.036(3) 0.039(3) 0.020(2) 0.013(2) 0.013(2) C65 0.045(3) 0.035(3) 0.041(3) 0.013(2) 0.010(3) 0.014(3) C66 0.059(4) 0.054(4) 0.036(3) 0.016(3) 0.018(3) 0.017(3) C67 0.076(5) 0.043(4) 0.066(4) 0.024(3) 0.000(4) 0.033(3) C68 0.086(5) 0.050(4) 0.057(4) 0.035(3) 0.012(4) 0.013(4) C69 0.069(5) 0.062(4) 0.054(4) 0.035(3) 0.015(3) 0.009(4) C70 0.055(4) 0.041(3) 0.039(3) 0.019(3) 0.007(3) 0.008(3) C71 0.045(3) 0.037(3) 0.040(3) 0.019(2) 0.020(3) 0.014(3) C72 0.053(3) 0.031(3) 0.044(3) 0.015(2) 0.015(3) 0.013(3) C73 0.042(3) 0.032(3) 0.046(3) 0.012(2) 0.013(3) 0.013(2) C74 0.045(3) 0.038(3) 0.036(3) 0.013(2) 0.015(2) 0.019(3) C75 0.071(5) 0.055(4) 0.059(4) 0.018(3) 0.014(3) 0.020(3) C76 0.062(4) 0.056(4) 0.054(4) 0.017(3) 0.012(3) 0.014(3) C77 0.048(4) 0.048(4) 0.051(4) 0.012(3) 0.015(3) 0.012(3) C78 0.048(4) 0.053(4) 0.059(4) 0.019(3) 0.013(3) 0.018(3) C79 0.052(4) 0.040(3) 0.065(4) 0.019(3) 0.014(3) 0.016(3) C80 0.081(5) 0.053(4) 0.073(5) 0.027(4) 0.034(4) 0.032(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O1 1.785(4) . ? Ge1 N3 1.903(4) . ? Ge1 N4 1.905(4) . ? Ge1 N1 1.918(4) . ? Ge1 N2 1.920(4) . ? Ge2 O2 1.751(3) . ? Ge2 N6 1.915(4) . ? Ge2 N7 1.918(4) . ? Ge2 N8 1.921(4) . ? Ge2 N5 1.925(4) . ? F1 C7 1.344(6) . ? F2 C8 1.353(6) . ? F3 C9 1.338(6) . ? F4 C10 1.348(6) . ? F5 C11 1.344(6) . ? F6 C18 1.353(7) . ? F7 C19 1.351(7) . ? F8 C20 1.338(7) . ? F9 C21 1.350(7) . ? F10 C22 1.336(7) . ? F11 C29 1.347(8) . ? F12 C30 1.332(9) . ? F13 C31 1.338(8) . ? F14 C32 1.353(8) . ? F15 C33 1.326(7) . ? F16 C48 1.339(6) . ? F17 C47 1.333(7) . ? F18 C46 1.341(7) . ? F19 C45 1.344(7) . ? F20 C44 1.350(6) . ? F21 C55 1.343(6) . ? F22 C56 1.333(6) . ? F23 C57 1.354(7) . ? F24 C58 1.350(7) . ? F25 C59 1.337(6) . ? F26 C66 1.343(6) . ? F27 C67 1.351(7) . ? F28 C68 1.346(7) . ? F29 C69 1.343(7) . ? F30 C70 1.342(7) . ? O1 H1 0.8401 . ? O2 H2A 0.8400 . ? N1 C23 1.391(7) . ? N1 C26 1.404(6) . ? N2 C37 1.373(6) . ? N2 C34 1.376(6) . ? N3 C4 1.368(6) . ? N3 C1 1.378(6) . ? N4 C15 1.394(7) . ? N4 C12 1.405(6) . ? N5 C60 1.384(6) . ? N5 C63 1.409(6) . ? N6 C52 1.387(7) . ? N6 C49 1.422(6) . ? N7 C41 1.362(6) . ? N7 C38 1.383(6) . ? N8 C74 1.369(6) . ? N8 C71 1.369(6) . ? C1 C37 1.403(7) . ? C1 C2 1.417(7) . ? C2 C3 1.373(7) . ? C2 H2 0.9500 . ? C3 C4 1.425(7) . ? C3 H3 0.9500 . ? C4 C5 1.403(7) . ? C5 C12 1.401(7) . ? C5 C6 1.494(7) . ? C6 C11 1.386(7) . ? C6 C7 1.400(7) . ? C7 C8 1.365(7) . ? C8 C9 1.366(8) . ? C9 C10 1.379(8) . ? C10 C11 1.370(7) . ? C12 C13 1.416(7) . ? C13 C14 1.362(7) . ? C13 H13 0.9500 . ? C14 C15 1.418(7) . ? C14 H14 0.9500 . ? C15 C16 1.390(7) . ? C16 C23 1.393(7) . ? C16 C17 1.496(7) . ? C17 C18 1.373(8) . ? C17 C22 1.393(8) . ? C18 C19 1.390(9) . ? C19 C20 1.373(9) . ? C20 C21 1.356(9) . ? C21 C22 1.356(8) . ? C23 C24 1.416(7) . ? C24 C25 1.355(8) . ? C24 H24 0.9500 . ? C25 C26 1.431(8) . ? C25 H25 0.9500 . ? C26 C27 1.394(8) . ? C27 C34 1.396(8) . ? C27 C28 1.502(7) . ? C28 C29 1.379(9) . ? C28 C33 1.390(8) . ? C29 C30 1.385(10) . ? C30 C31 1.371(12) . ? C31 C32 1.351(11) . ? C32 C33 1.371(9) . ? C34 C35 1.427(7) . ? C35 C36 1.368(8) . ? C35 H35 0.9500 . ? C36 C37 1.412(7) . ? C36 H36 0.9500 . ? C38 C74 1.396(7) . ? C38 C39 1.412(7) . ? C39 C40 1.384(7) . ? C39 H39 0.9500 . ? C40 C41 1.430(7) . ? C40 H40 0.9500 . ? C41 C42 1.393(7) . ? C42 C49 1.393(7) . ? C42 C43 1.498(7) . ? C43 C44 1.377(8) . ? C43 C48 1.385(8) . ? C44 C45 1.383(8) . ? C45 C46 1.379(9) . ? C46 C47 1.363(10) . ? C47 C48 1.389(8) . ? C49 C50 1.421(7) . ? C50 C51 1.348(7) . ? C50 H50 0.9500 . ? C51 C52 1.428(7) . ? C51 H51 0.9500 . ? C52 C53 1.402(7) . ? C53 C60 1.412(7) . ? C53 C54 1.500(7) . ? C54 C55 1.368(7) . ? C54 C59 1.384(8) . ? C55 C56 1.399(8) . ? C56 C57 1.365(9) . ? C57 C58 1.337(9) . ? C58 C59 1.391(8) . ? C60 C61 1.414(7) . ? C61 C62 1.350(7) . ? C61 H61 0.9500 . ? C62 C63 1.416(7) . ? C62 H62 0.9500 . ? C63 C64 1.399(7) . ? C64 C71 1.401(7) . ? C64 C65 1.484(7) . ? C65 C70 1.387(8) . ? C65 C66 1.390(8) . ? C66 C67 1.384(8) . ? C67 C68 1.372(10) . ? C68 C69 1.360(9) . ? C69 C70 1.383(8) . ? C71 C72 1.430(7) . ? C72 C73 1.367(7) . ? C72 H72 0.9500 . ? C73 C74 1.422(7) . ? C73 H73 0.9500 . ? C75 C76 1.523(8) . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C75 H75A 0.9800 . ? C76 C77 1.506(8) . ? C76 H76B 0.9900 . ? C76 H76A 0.9900 . ? C77 C78 1.531(8) . ? C77 H77B 0.9900 . ? C77 H77A 0.9900 . ? C78 C79 1.503(8) . ? C78 H78B 0.9900 . ? C78 H78A 0.9900 . ? C79 C80 1.523(8) . ? C79 H79B 0.9900 . ? C79 H79A 0.9900 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 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 N3 99.99(18) . . ? O1 Ge1 N4 101.83(17) . . ? N3 Ge1 N4 87.64(17) . . ? O1 Ge1 N1 105.24(18) . . ? N3 Ge1 N1 154.03(19) . . ? N4 Ge1 N1 93.11(17) . . ? O1 Ge1 N2 104.58(18) . . ? N3 Ge1 N2 79.64(17) . . ? N4 Ge1 N2 152.27(18) . . ? N1 Ge1 N2 88.05(17) . . ? O2 Ge2 N6 104.07(17) . . ? O2 Ge2 N7 101.47(17) . . ? N6 Ge2 N7 87.69(17) . . ? O2 Ge2 N8 105.71(17) . . ? N6 Ge2 N8 149.27(19) . . ? N7 Ge2 N8 79.17(18) . . ? O2 Ge2 N5 105.02(17) . . ? N6 Ge2 N5 92.30(17) . . ? N7 Ge2 N5 152.67(18) . . ? N8 Ge2 N5 87.24(18) . . ? Ge1 O1 H1 103.4 . . ? Ge2 O2 H2A 109.0 . . ? C23 N1 C26 107.4(4) . . ? C23 N1 Ge1 125.5(3) . . ? C26 N1 Ge1 126.1(4) . . ? C37 N2 C34 110.0(4) . . ? C37 N2 Ge1 116.3(3) . . ? C34 N2 Ge1 131.8(4) . . ? C4 N3 C1 109.1(4) . . ? C4 N3 Ge1 131.6(4) . . ? C1 N3 Ge1 116.3(3) . . ? C15 N4 C12 107.3(4) . . ? C15 N4 Ge1 125.4(3) . . ? C12 N4 Ge1 125.7(3) . . ? C60 N5 C63 106.6(4) . . ? C60 N5 Ge2 124.3(3) . . ? C63 N5 Ge2 126.0(3) . . ? C52 N6 C49 107.0(4) . . ? C52 N6 Ge2 124.7(3) . . ? C49 N6 Ge2 125.6(3) . . ? C41 N7 C38 109.9(4) . . ? C41 N7 Ge2 132.8(4) . . ? C38 N7 Ge2 116.9(3) . . ? C74 N8 C71 109.3(4) . . ? C74 N8 Ge2 117.1(3) . . ? C71 N8 Ge2 132.5(4) . . ? N3 C1 C37 112.6(5) . . ? N3 C1 C2 108.4(4) . . ? C37 C1 C2 139.0(5) . . ? C3 C2 C1 106.7(5) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 C4 108.7(5) . . ? C2 C3 H3 125.6 . . ? C4 C3 H3 125.6 . . ? N3 C4 C5 119.7(5) . . ? N3 C4 C3 107.0(4) . . ? C5 C4 C3 133.3(5) . . ? C12 C5 C4 122.0(5) . . ? C12 C5 C6 119.1(5) . . ? C4 C5 C6 118.9(5) . . ? C11 C6 C7 115.6(5) . . ? C11 C6 C5 120.9(5) . . ? C7 C6 C5 123.4(5) . . ? F1 C7 C8 118.4(5) . . ? F1 C7 C6 119.6(5) . . ? C8 C7 C6 121.9(5) . . ? F2 C8 C7 119.5(5) . . ? F2 C8 C9 119.4(5) . . ? C7 C8 C9 121.1(5) . . ? F3 C9 C8 121.8(5) . . ? F3 C9 C10 119.7(5) . . ? C8 C9 C10 118.5(5) . . ? F4 C10 C11 120.6(5) . . ? F4 C10 C9 119.1(5) . . ? C11 C10 C9 120.4(5) . . ? F5 C11 C10 117.1(5) . . ? F5 C11 C6 120.4(5) . . ? C10 C11 C6 122.5(5) . . ? C5 C12 N4 125.5(5) . . ? C5 C12 C13 126.7(5) . . ? N4 C12 C13 107.8(4) . . ? C14 C13 C12 108.4(5) . . ? C14 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? C13 C14 C15 108.3(5) . . ? C13 C14 H14 125.8 . . ? C15 C14 H14 125.8 . . ? C16 C15 N4 124.0(5) . . ? C16 C15 C14 127.8(5) . . ? N4 C15 C14 108.1(5) . . ? C15 C16 C23 125.3(5) . . ? C15 C16 C17 117.2(5) . . ? C23 C16 C17 117.4(5) . . ? C18 C17 C22 116.2(5) . . ? C18 C17 C16 122.5(6) . . ? C22 C17 C16 121.2(5) . . ? F6 C18 C17 119.8(6) . . ? F6 C18 C19 118.6(6) . . ? C17 C18 C19 121.6(6) . . ? F7 C19 C20 120.6(6) . . ? F7 C19 C18 119.5(7) . . ? C20 C19 C18 119.9(6) . . ? F8 C20 C21 121.3(7) . . ? F8 C20 C19 119.4(7) . . ? C21 C20 C19 119.3(6) . . ? F9 C21 C20 119.1(6) . . ? F9 C21 C22 120.3(6) . . ? C20 C21 C22 120.6(6) . . ? F10 C22 C21 118.7(6) . . ? F10 C22 C17 118.8(5) . . ? C21 C22 C17 122.4(6) . . ? N1 C23 C16 123.1(5) . . ? N1 C23 C24 108.3(5) . . ? C16 C23 C24 128.5(5) . . ? C25 C24 C23 108.7(5) . . ? C25 C24 H24 125.7 . . ? C23 C24 H24 125.7 . . ? C24 C25 C26 108.1(5) . . ? C24 C25 H25 126.0 . . ? C26 C25 H25 126.0 . . ? C27 C26 N1 125.9(5) . . ? C27 C26 C25 126.6(5) . . ? N1 C26 C25 107.5(5) . . ? C26 C27 C34 122.8(5) . . ? C26 C27 C28 118.4(5) . . ? C34 C27 C28 118.8(5) . . ? C29 C28 C33 116.9(6) . . ? C29 C28 C27 122.0(6) . . ? C33 C28 C27 121.1(5) . . ? F11 C29 C28 119.6(6) . . ? F11 C29 C30 117.9(7) . . ? C28 C29 C30 122.5(7) . . ? F12 C30 C31 121.6(8) . . ? F12 C30 C29 119.8(8) . . ? C31 C30 C29 118.6(7) . . ? F13 C31 C32 120.3(9) . . ? F13 C31 C30 119.7(9) . . ? C32 C31 C30 120.0(7) . . ? C31 C32 F14 119.6(7) . . ? C31 C32 C33 121.4(8) . . ? F14 C32 C33 119.0(8) . . ? F15 C33 C32 119.5(7) . . ? F15 C33 C28 120.0(5) . . ? C32 C33 C28 120.5(7) . . ? N2 C34 C27 120.1(5) . . ? N2 C34 C35 106.0(5) . . ? C27 C34 C35 133.9(5) . . ? C36 C35 C34 109.0(5) . . ? C36 C35 H35 125.5 . . ? C34 C35 H35 125.5 . . ? C35 C36 C37 107.3(5) . . ? C35 C36 H36 126.3 . . ? C37 C36 H36 126.3 . . ? N2 C37 C1 112.1(4) . . ? N2 C37 C36 107.8(5) . . ? C1 C37 C36 140.1(5) . . ? N7 C38 C74 112.2(5) . . ? N7 C38 C39 107.8(4) . . ? C74 C38 C39 140.0(5) . . ? C40 C39 C38 107.3(5) . . ? C40 C39 H39 126.4 . . ? C38 C39 H39 126.4 . . ? C39 C40 C41 108.1(5) . . ? C39 C40 H40 126.0 . . ? C41 C40 H40 126.0 . . ? N7 C41 C42 120.3(5) . . ? N7 C41 C40 107.0(5) . . ? C42 C41 C40 132.6(5) . . ? C41 C42 C49 122.8(5) . . ? C41 C42 C43 116.5(5) . . ? C49 C42 C43 120.5(5) . . ? C44 C43 C48 115.5(5) . . ? C44 C43 C42 121.9(5) . . ? C48 C43 C42 122.3(5) . . ? F20 C44 C43 119.5(5) . . ? F20 C44 C45 117.2(5) . . ? C43 C44 C45 123.2(6) . . ? F19 C45 C46 120.7(6) . . ? F19 C45 C44 120.3(6) . . ? C46 C45 C44 119.0(6) . . ? F18 C46 C47 120.8(7) . . ? F18 C46 C45 119.1(7) . . ? C47 C46 C45 120.1(6) . . ? F17 C47 C46 120.5(6) . . ? F17 C47 C48 120.3(7) . . ? C46 C47 C48 119.2(6) . . ? F16 C48 C43 119.9(5) . . ? F16 C48 C47 117.1(6) . . ? C43 C48 C47 122.9(6) . . ? C42 C49 C50 127.6(5) . . ? C42 C49 N6 125.3(5) . . ? C50 C49 N6 107.1(4) . . ? C51 C50 C49 109.3(5) . . ? C51 C50 H50 125.4 . . ? C49 C50 H50 125.4 . . ? C50 C51 C52 107.9(5) . . ? C50 C51 H51 126.0 . . ? C52 C51 H51 126.0 . . ? N6 C52 C53 124.1(5) . . ? N6 C52 C51 108.6(5) . . ? C53 C52 C51 127.3(5) . . ? C52 C53 C60 124.2(5) . . ? C52 C53 C54 117.7(5) . . ? C60 C53 C54 117.9(5) . . ? C55 C54 C59 115.3(5) . . ? C55 C54 C53 124.7(5) . . ? C59 C54 C53 119.9(5) . . ? F21 C55 C54 120.1(5) . . ? F21 C55 C56 116.8(5) . . ? C54 C55 C56 123.1(5) . . ? F22 C56 C57 121.2(6) . . ? F22 C56 C55 120.0(6) . . ? C57 C56 C55 118.8(5) . . ? C58 C57 F23 120.4(6) . . ? C58 C57 C56 120.3(6) . . ? F23 C57 C56 119.3(6) . . ? C57 C58 F24 120.7(6) . . ? C57 C58 C59 120.2(6) . . ? F24 C58 C59 119.2(6) . . ? F25 C59 C54 118.9(5) . . ? F25 C59 C58 118.8(5) . . ? C54 C59 C58 122.4(5) . . ? N5 C60 C53 123.3(5) . . ? N5 C60 C61 109.2(5) . . ? C53 C60 C61 127.5(5) . . ? C62 C61 C60 107.8(5) . . ? C62 C61 H61 126.1 . . ? C60 C61 H61 126.1 . . ? C61 C62 C63 108.8(5) . . ? C61 C62 H62 125.6 . . ? C63 C62 H62 125.6 . . ? C64 C63 N5 125.0(5) . . ? C64 C63 C62 127.3(5) . . ? N5 C63 C62 107.7(4) . . ? C63 C64 C71 122.6(5) . . ? C63 C64 C65 120.2(5) . . ? C71 C64 C65 117.1(5) . . ? C70 C65 C66 115.6(5) . . ? C70 C65 C64 122.5(5) . . ? C66 C65 C64 121.7(5) . . ? F26 C66 C67 118.6(6) . . ? F26 C66 C65 118.8(5) . . ? C67 C66 C65 122.6(6) . . ? F27 C67 C68 120.9(6) . . ? F27 C67 C66 119.7(7) . . ? C68 C67 C66 119.4(6) . . ? F28 C68 C69 120.4(7) . . ? F28 C68 C67 119.7(7) . . ? C69 C68 C67 119.9(6) . . ? F29 C69 C68 119.9(6) . . ? F29 C69 C70 120.1(6) . . ? C68 C69 C70 120.0(6) . . ? F30 C70 C69 117.7(5) . . ? F30 C70 C65 119.8(5) . . ? C69 C70 C65 122.5(6) . . ? N8 C71 C64 120.4(5) . . ? N8 C71 C72 107.1(5) . . ? C64 C71 C72 132.5(5) . . ? C73 C72 C71 108.3(5) . . ? C73 C72 H72 125.9 . . ? C71 C72 H72 125.9 . . ? C72 C73 C74 107.1(5) . . ? C72 C73 H73 126.4 . . ? C74 C73 H73 126.4 . . ? N8 C74 C38 112.7(5) . . ? N8 C74 C73 108.2(4) . . ? C38 C74 C73 139.1(5) . . ? C76 C75 H75B 109.5 . . ? C76 C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C76 C75 H75A 109.5 . . ? H75B C75 H75A 109.5 . . ? H75C C75 H75A 109.5 . . ? C77 C76 C75 114.3(5) . . ? C77 C76 H76B 108.7 . . ? C75 C76 H76B 108.7 . . ? C77 C76 H76A 108.7 . . ? C75 C76 H76A 108.7 . . ? H76B C76 H76A 107.6 . . ? C76 C77 C78 113.4(5) . . ? C76 C77 H77B 108.9 . . ? C78 C77 H77B 108.9 . . ? C76 C77 H77A 108.9 . . ? C78 C77 H77A 108.9 . . ? H77B C77 H77A 107.7 . . ? C79 C78 C77 115.6(5) . . ? C79 C78 H78B 108.4 . . ? C77 C78 H78B 108.4 . . ? C79 C78 H78A 108.4 . . ? C77 C78 H78A 108.4 . . ? H78B C78 H78A 107.4 . . ? C78 C79 C80 112.5(5) . . ? C78 C79 H79B 109.1 . . ? C80 C79 H79B 109.1 . . ? C78 C79 H79A 109.1 . . ? C80 C79 H79A 109.1 . . ? H79B C79 H79A 107.8 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 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 O1 Ge1 N1 C23 -83.4(5) . . . . ? N3 Ge1 N1 C23 110.8(5) . . . . ? N4 Ge1 N1 C23 19.8(5) . . . . ? N2 Ge1 N1 C23 172.1(5) . . . . ? O1 Ge1 N1 C26 84.3(4) . . . . ? N3 Ge1 N1 C26 -81.6(6) . . . . ? N4 Ge1 N1 C26 -172.6(4) . . . . ? N2 Ge1 N1 C26 -20.3(4) . . . . ? O1 Ge1 N2 C37 82.7(4) . . . . ? N3 Ge1 N2 C37 -15.0(4) . . . . ? N4 Ge1 N2 C37 -79.1(5) . . . . ? N1 Ge1 N2 C37 -172.0(4) . . . . ? O1 Ge1 N2 C34 -80.1(5) . . . . ? N3 Ge1 N2 C34 -177.8(5) . . . . ? N4 Ge1 N2 C34 118.2(5) . . . . ? N1 Ge1 N2 C34 25.2(5) . . . . ? O1 Ge1 N3 C4 70.7(5) . . . . ? N4 Ge1 N3 C4 -30.9(5) . . . . ? N1 Ge1 N3 C4 -123.1(5) . . . . ? N2 Ge1 N3 C4 173.9(5) . . . . ? O1 Ge1 N3 C1 -87.6(4) . . . . ? N4 Ge1 N3 C1 170.8(4) . . . . ? N1 Ge1 N3 C1 78.6(6) . . . . ? N2 Ge1 N3 C1 15.6(4) . . . . ? O1 Ge1 N4 C15 88.6(4) . . . . ? N3 Ge1 N4 C15 -171.7(4) . . . . ? N1 Ge1 N4 C15 -17.7(4) . . . . ? N2 Ge1 N4 C15 -109.4(5) . . . . ? O1 Ge1 N4 C12 -75.0(4) . . . . ? N3 Ge1 N4 C12 24.7(4) . . . . ? N1 Ge1 N4 C12 178.7(4) . . . . ? N2 Ge1 N4 C12 87.0(5) . . . . ? O2 Ge2 N5 C60 77.4(4) . . . . ? N6 Ge2 N5 C60 -27.8(4) . . . . ? N7 Ge2 N5 C60 -117.2(5) . . . . ? N8 Ge2 N5 C60 -177.1(4) . . . . ? O2 Ge2 N5 C63 -79.9(4) . . . . ? N6 Ge2 N5 C63 174.9(4) . . . . ? N7 Ge2 N5 C63 85.5(6) . . . . ? N8 Ge2 N5 C63 25.6(4) . . . . ? O2 Ge2 N6 C52 -80.7(4) . . . . ? N7 Ge2 N6 C52 178.1(4) . . . . ? N8 Ge2 N6 C52 113.9(5) . . . . ? N5 Ge2 N6 C52 25.4(4) . . . . ? O2 Ge2 N6 C49 77.9(4) . . . . ? N7 Ge2 N6 C49 -23.4(4) . . . . ? N8 Ge2 N6 C49 -87.6(5) . . . . ? N5 Ge2 N6 C49 -176.0(4) . . . . ? O2 Ge2 N7 C41 -79.9(5) . . . . ? N6 Ge2 N7 C41 24.0(5) . . . . ? N8 Ge2 N7 C41 176.0(5) . . . . ? N5 Ge2 N7 C41 114.5(5) . . . . ? O2 Ge2 N7 C38 92.0(4) . . . . ? N6 Ge2 N7 C38 -164.1(4) . . . . ? N8 Ge2 N7 C38 -12.0(4) . . . . ? N5 Ge2 N7 C38 -73.6(5) . . . . ? O2 Ge2 N8 C74 -86.8(4) . . . . ? N6 Ge2 N8 C74 78.5(5) . . . . ? N7 Ge2 N8 C74 12.2(4) . . . . ? N5 Ge2 N8 C74 168.4(4) . . . . ? O2 Ge2 N8 C71 79.9(5) . . . . ? N6 Ge2 N8 C71 -114.8(5) . . . . ? N7 Ge2 N8 C71 178.9(5) . . . . ? N5 Ge2 N8 C71 -24.9(5) . . . . ? C4 N3 C1 C37 -176.6(4) . . . . ? Ge1 N3 C1 C37 -13.6(6) . . . . ? C4 N3 C1 C2 2.0(6) . . . . ? Ge1 N3 C1 C2 164.9(3) . . . . ? N3 C1 C2 C3 -2.5(6) . . . . ? C37 C1 C2 C3 175.5(6) . . . . ? C1 C2 C3 C4 2.0(6) . . . . ? C1 N3 C4 C5 -179.9(5) . . . . ? Ge1 N3 C4 C5 20.7(7) . . . . ? C1 N3 C4 C3 -0.7(6) . . . . ? Ge1 N3 C4 C3 -160.2(4) . . . . ? C2 C3 C4 N3 -0.9(6) . . . . ? C2 C3 C4 C5 178.1(6) . . . . ? N3 C4 C5 C12 5.1(8) . . . . ? C3 C4 C5 C12 -173.7(5) . . . . ? N3 C4 C5 C6 -172.2(5) . . . . ? C3 C4 C5 C6 8.9(9) . . . . ? C12 C5 C6 C11 -58.4(7) . . . . ? C4 C5 C6 C11 119.0(6) . . . . ? C12 C5 C6 C7 124.7(6) . . . . ? C4 C5 C6 C7 -57.9(7) . . . . ? C11 C6 C7 F1 178.8(5) . . . . ? C5 C6 C7 F1 -4.2(8) . . . . ? C11 C6 C7 C8 -1.3(8) . . . . ? C5 C6 C7 C8 175.7(5) . . . . ? F1 C7 C8 F2 0.4(8) . . . . ? C6 C7 C8 F2 -179.6(5) . . . . ? F1 C7 C8 C9 -179.9(5) . . . . ? C6 C7 C8 C9 0.2(9) . . . . ? F2 C8 C9 F3 0.6(9) . . . . ? C7 C8 C9 F3 -179.1(5) . . . . ? F2 C8 C9 C10 -179.5(5) . . . . ? C7 C8 C9 C10 0.7(9) . . . . ? F3 C9 C10 F4 -1.3(8) . . . . ? C8 C9 C10 F4 178.9(5) . . . . ? F3 C9 C10 C11 179.4(5) . . . . ? C8 C9 C10 C11 -0.4(9) . . . . ? F4 C10 C11 F5 0.9(8) . . . . ? C9 C10 C11 F5 -179.8(5) . . . . ? F4 C10 C11 C6 179.9(5) . . . . ? C9 C10 C11 C6 -0.8(9) . . . . ? C7 C6 C11 F5 -179.4(5) . . . . ? C5 C6 C11 F5 3.6(8) . . . . ? C7 C6 C11 C10 1.7(8) . . . . ? C5 C6 C11 C10 -175.4(5) . . . . ? C4 C5 C12 N4 -8.8(8) . . . . ? C6 C5 C12 N4 168.5(5) . . . . ? C4 C5 C12 C13 171.7(5) . . . . ? C6 C5 C12 C13 -10.9(8) . . . . ? C15 N4 C12 C5 -178.0(5) . . . . ? Ge1 N4 C12 C5 -12.0(7) . . . . ? C15 N4 C12 C13 1.5(6) . . . . ? Ge1 N4 C12 C13 167.6(3) . . . . ? C5 C12 C13 C14 178.9(5) . . . . ? N4 C12 C13 C14 -0.7(6) . . . . ? C12 C13 C14 C15 -0.4(6) . . . . ? C12 N4 C15 C16 175.4(5) . . . . ? Ge1 N4 C15 C16 9.3(8) . . . . ? C12 N4 C15 C14 -1.8(6) . . . . ? Ge1 N4 C15 C14 -167.9(3) . . . . ? C13 C14 C15 C16 -175.6(5) . . . . ? C13 C14 C15 N4 1.4(6) . . . . ? N4 C15 C16 C23 4.3(9) . . . . ? C14 C15 C16 C23 -179.1(6) . . . . ? N4 C15 C16 C17 -171.7(5) . . . . ? C14 C15 C16 C17 4.8(9) . . . . ? C15 C16 C17 C18 -78.3(7) . . . . ? C23 C16 C17 C18 105.3(7) . . . . ? C15 C16 C17 C22 99.0(6) . . . . ? C23 C16 C17 C22 -77.4(7) . . . . ? C22 C17 C18 F6 178.7(5) . . . . ? C16 C17 C18 F6 -3.9(8) . . . . ? C22 C17 C18 C19 -1.5(9) . . . . ? C16 C17 C18 C19 175.9(5) . . . . ? F6 C18 C19 F7 0.1(9) . . . . ? C17 C18 C19 F7 -179.7(5) . . . . ? F6 C18 C19 C20 -179.1(5) . . . . ? C17 C18 C19 C20 1.1(10) . . . . ? F7 C19 C20 F8 1.3(9) . . . . ? C18 C19 C20 F8 -179.5(5) . . . . ? F7 C19 C20 C21 179.9(6) . . . . ? C18 C19 C20 C21 -0.9(10) . . . . ? F8 C20 C21 F9 -0.1(9) . . . . ? C19 C20 C21 F9 -178.7(5) . . . . ? F8 C20 C21 C22 179.8(5) . . . . ? C19 C20 C21 C22 1.2(9) . . . . ? F9 C21 C22 F10 0.4(8) . . . . ? C20 C21 C22 F10 -179.4(5) . . . . ? F9 C21 C22 C17 178.1(5) . . . . ? C20 C21 C22 C17 -1.7(9) . . . . ? C18 C17 C22 F10 179.5(5) . . . . ? C16 C17 C22 F10 2.1(8) . . . . ? C18 C17 C22 C21 1.8(8) . . . . ? C16 C17 C22 C21 -175.6(5) . . . . ? C26 N1 C23 C16 177.0(5) . . . . ? Ge1 N1 C23 C16 -13.4(8) . . . . ? C26 N1 C23 C24 -0.2(6) . . . . ? Ge1 N1 C23 C24 169.3(4) . . . . ? C15 C16 C23 N1 -2.1(9) . . . . ? C17 C16 C23 N1 173.9(5) . . . . ? C15 C16 C23 C24 174.5(6) . . . . ? C17 C16 C23 C24 -9.5(9) . . . . ? N1 C23 C24 C25 -0.4(7) . . . . ? C16 C23 C24 C25 -177.5(6) . . . . ? C23 C24 C25 C26 0.9(7) . . . . ? C23 N1 C26 C27 -179.4(5) . . . . ? Ge1 N1 C26 C27 11.1(8) . . . . ? C23 N1 C26 C25 0.7(6) . . . . ? Ge1 N1 C26 C25 -168.7(4) . . . . ? C24 C25 C26 C27 179.2(6) . . . . ? C24 C25 C26 N1 -1.0(7) . . . . ? N1 C26 C27 C34 4.8(9) . . . . ? C25 C26 C27 C34 -175.3(6) . . . . ? N1 C26 C27 C28 -176.3(5) . . . . ? C25 C26 C27 C28 3.5(9) . . . . ? C26 C27 C28 C29 -111.0(7) . . . . ? C34 C27 C28 C29 67.9(9) . . . . ? C26 C27 C28 C33 69.6(8) . . . . ? C34 C27 C28 C33 -111.5(7) . . . . ? C33 C28 C29 F11 -178.9(6) . . . . ? C27 C28 C29 F11 1.8(11) . . . . ? C33 C28 C29 C30 -0.5(12) . . . . ? C27 C28 C29 C30 -179.8(7) . . . . ? F11 C29 C30 F12 -0.9(13) . . . . ? C28 C29 C30 F12 -179.3(8) . . . . ? F11 C29 C30 C31 180.0(8) . . . . ? C28 C29 C30 C31 1.6(14) . . . . ? F12 C30 C31 F13 1.2(15) . . . . ? C29 C30 C31 F13 -179.7(8) . . . . ? F12 C30 C31 C32 179.4(9) . . . . ? C29 C30 C31 C32 -1.5(15) . . . . ? F13 C31 C32 F14 -1.7(13) . . . . ? C30 C31 C32 F14 -179.8(8) . . . . ? F13 C31 C32 C33 178.6(7) . . . . ? C30 C31 C32 C33 0.4(14) . . . . ? C31 C32 C33 F15 179.8(7) . . . . ? F14 C32 C33 F15 0.1(10) . . . . ? C31 C32 C33 C28 0.7(12) . . . . ? F14 C32 C33 C28 -179.0(6) . . . . ? C29 C28 C33 F15 -179.8(6) . . . . ? C27 C28 C33 F15 -0.4(9) . . . . ? C29 C28 C33 C32 -0.7(10) . . . . ? C27 C28 C33 C32 178.7(6) . . . . ? C37 N2 C34 C27 178.4(5) . . . . ? Ge1 N2 C34 C27 -18.0(8) . . . . ? C37 N2 C34 C35 -0.1(6) . . . . ? Ge1 N2 C34 C35 163.5(4) . . . . ? C26 C27 C34 N2 -2.0(9) . . . . ? C28 C27 C34 N2 179.1(5) . . . . ? C26 C27 C34 C35 175.9(6) . . . . ? C28 C27 C34 C35 -2.9(10) . . . . ? N2 C34 C35 C36 0.2(6) . . . . ? C27 C34 C35 C36 -178.0(6) . . . . ? C34 C35 C36 C37 -0.2(6) . . . . ? C34 N2 C37 C1 178.2(4) . . . . ? Ge1 N2 C37 C1 11.8(6) . . . . ? C34 N2 C37 C36 -0.1(6) . . . . ? Ge1 N2 C37 C36 -166.5(4) . . . . ? N3 C1 C37 N2 1.1(6) . . . . ? C2 C1 C37 N2 -176.8(6) . . . . ? N3 C1 C37 C36 178.5(6) . . . . ? C2 C1 C37 C36 0.6(12) . . . . ? C35 C36 C37 N2 0.2(6) . . . . ? C35 C36 C37 C1 -177.3(7) . . . . ? C41 N7 C38 C74 -176.4(4) . . . . ? Ge2 N7 C38 C74 9.9(6) . . . . ? C41 N7 C38 C39 2.5(6) . . . . ? Ge2 N7 C38 C39 -171.3(3) . . . . ? N7 C38 C39 C40 -1.3(6) . . . . ? C74 C38 C39 C40 177.1(7) . . . . ? C38 C39 C40 C41 -0.3(6) . . . . ? C38 N7 C41 C42 173.6(5) . . . . ? Ge2 N7 C41 C42 -14.0(8) . . . . ? C38 N7 C41 C40 -2.6(6) . . . . ? Ge2 N7 C41 C40 169.7(4) . . . . ? C39 C40 C41 N7 1.8(6) . . . . ? C39 C40 C41 C42 -173.8(6) . . . . ? N7 C41 C42 C49 -4.2(8) . . . . ? C40 C41 C42 C49 170.9(6) . . . . ? N7 C41 C42 C43 -179.2(5) . . . . ? C40 C41 C42 C43 -4.1(9) . . . . ? C41 C42 C43 C44 -76.8(7) . . . . ? C49 C42 C43 C44 108.0(6) . . . . ? C41 C42 C43 C48 96.7(7) . . . . ? C49 C42 C43 C48 -78.4(7) . . . . ? C48 C43 C44 F20 -178.7(5) . . . . ? C42 C43 C44 F20 -4.8(8) . . . . ? C48 C43 C44 C45 -0.1(9) . . . . ? C42 C43 C44 C45 173.8(5) . . . . ? F20 C44 C45 F19 -0.9(8) . . . . ? C43 C44 C45 F19 -179.6(5) . . . . ? F20 C44 C45 C46 178.8(6) . . . . ? C43 C44 C45 C46 0.1(10) . . . . ? F19 C45 C46 F18 -0.1(10) . . . . ? C44 C45 C46 F18 -179.8(6) . . . . ? F19 C45 C46 C47 179.6(6) . . . . ? C44 C45 C46 C47 -0.1(11) . . . . ? F18 C46 C47 F17 -0.1(12) . . . . ? C45 C46 C47 F17 -179.8(7) . . . . ? F18 C46 C47 C48 179.8(7) . . . . ? C45 C46 C47 C48 0.1(11) . . . . ? C44 C43 C48 F16 177.7(5) . . . . ? C42 C43 C48 F16 3.8(9) . . . . ? C44 C43 C48 C47 0.1(9) . . . . ? C42 C43 C48 C47 -173.8(6) . . . . ? F17 C47 C48 F16 2.2(10) . . . . ? C46 C47 C48 F16 -177.8(6) . . . . ? F17 C47 C48 C43 179.8(6) . . . . ? C46 C47 C48 C43 -0.1(11) . . . . ? C41 C42 C49 C50 -176.4(5) . . . . ? C43 C42 C49 C50 -1.6(9) . . . . ? C41 C42 C49 N6 2.2(9) . . . . ? C43 C42 C49 N6 177.0(5) . . . . ? C52 N6 C49 C42 178.4(5) . . . . ? Ge2 N6 C49 C42 16.7(7) . . . . ? C52 N6 C49 C50 -2.8(6) . . . . ? Ge2 N6 C49 C50 -164.5(4) . . . . ? C42 C49 C50 C51 -179.6(5) . . . . ? N6 C49 C50 C51 1.6(6) . . . . ? C49 C50 C51 C52 0.2(6) . . . . ? C49 N6 C52 C53 -177.6(5) . . . . ? Ge2 N6 C52 C53 -15.8(7) . . . . ? C49 N6 C52 C51 2.9(6) . . . . ? Ge2 N6 C52 C51 164.8(3) . . . . ? C50 C51 C52 N6 -2.0(6) . . . . ? C50 C51 C52 C53 178.6(5) . . . . ? N6 C52 C53 C60 -1.2(9) . . . . ? C51 C52 C53 C60 178.1(5) . . . . ? N6 C52 C53 C54 173.6(5) . . . . ? C51 C52 C53 C54 -7.1(8) . . . . ? C52 C53 C54 C55 88.1(7) . . . . ? C60 C53 C54 C55 -96.7(6) . . . . ? C52 C53 C54 C59 -89.5(6) . . . . ? C60 C53 C54 C59 85.7(6) . . . . ? C59 C54 C55 F21 -178.3(5) . . . . ? C53 C54 C55 F21 4.0(8) . . . . ? C59 C54 C55 C56 0.0(8) . . . . ? C53 C54 C55 C56 -177.6(5) . . . . ? F21 C55 C56 F22 -0.9(8) . . . . ? C54 C55 C56 F22 -179.4(5) . . . . ? F21 C55 C56 C57 178.7(5) . . . . ? C54 C55 C56 C57 0.2(9) . . . . ? F22 C56 C57 C58 179.3(5) . . . . ? C55 C56 C57 C58 -0.3(9) . . . . ? F22 C56 C57 F23 0.1(9) . . . . ? C55 C56 C57 F23 -179.5(5) . . . . ? F23 C57 C58 F24 -1.6(9) . . . . ? C56 C57 C58 F24 179.2(5) . . . . ? F23 C57 C58 C59 179.3(5) . . . . ? C56 C57 C58 C59 0.1(9) . . . . ? C55 C54 C59 F25 179.2(5) . . . . ? C53 C54 C59 F25 -3.1(7) . . . . ? C55 C54 C59 C58 -0.3(8) . . . . ? C53 C54 C59 C58 177.5(5) . . . . ? C57 C58 C59 F25 -179.2(5) . . . . ? F24 C58 C59 F25 1.6(8) . . . . ? C57 C58 C59 C54 0.2(9) . . . . ? F24 C58 C59 C54 -178.9(5) . . . . ? C63 N5 C60 C53 -178.3(5) . . . . ? Ge2 N5 C60 C53 20.7(7) . . . . ? C63 N5 C60 C61 0.4(6) . . . . ? Ge2 N5 C60 C61 -160.6(4) . . . . ? C52 C53 C60 N5 -1.4(8) . . . . ? C54 C53 C60 N5 -176.3(5) . . . . ? C52 C53 C60 C61 -179.9(5) . . . . ? C54 C53 C60 C61 5.3(8) . . . . ? N5 C60 C61 C62 -0.3(6) . . . . ? C53 C60 C61 C62 178.4(5) . . . . ? C60 C61 C62 C63 0.1(7) . . . . ? C60 N5 C63 C64 -179.8(5) . . . . ? Ge2 N5 C63 C64 -19.2(7) . . . . ? C60 N5 C63 C62 -0.3(6) . . . . ? Ge2 N5 C63 C62 160.2(4) . . . . ? C61 C62 C63 C64 179.6(5) . . . . ? C61 C62 C63 N5 0.2(6) . . . . ? N5 C63 C64 C71 -1.2(9) . . . . ? C62 C63 C64 C71 179.4(5) . . . . ? N5 C63 C64 C65 -177.7(5) . . . . ? C62 C63 C64 C65 3.0(9) . . . . ? C63 C64 C65 C70 77.0(7) . . . . ? C71 C64 C65 C70 -99.6(7) . . . . ? C63 C64 C65 C66 -108.5(7) . . . . ? C71 C64 C65 C66 74.8(7) . . . . ? C70 C65 C66 F26 -179.0(5) . . . . ? C64 C65 C66 F26 6.3(9) . . . . ? C70 C65 C66 C67 1.6(9) . . . . ? C64 C65 C66 C67 -173.2(6) . . . . ? F26 C66 C67 F27 -0.2(9) . . . . ? C65 C66 C67 F27 179.2(6) . . . . ? F26 C66 C67 C68 179.8(6) . . . . ? C65 C66 C67 C68 -0.8(10) . . . . ? F27 C67 C68 F28 0.2(10) . . . . ? C66 C67 C68 F28 -179.9(6) . . . . ? F27 C67 C68 C69 -179.9(6) . . . . ? C66 C67 C68 C69 0.1(11) . . . . ? F28 C68 C69 F29 -0.9(11) . . . . ? C67 C68 C69 F29 179.2(6) . . . . ? F28 C68 C69 C70 179.6(6) . . . . ? C67 C68 C69 C70 -0.3(11) . . . . ? F29 C69 C70 F30 0.0(9) . . . . ? C68 C69 C70 F30 179.6(6) . . . . ? F29 C69 C70 C65 -178.2(6) . . . . ? C68 C69 C70 C65 1.3(10) . . . . ? C66 C65 C70 F30 179.9(5) . . . . ? C64 C65 C70 F30 -5.4(8) . . . . ? C66 C65 C70 C69 -1.9(9) . . . . ? C64 C65 C70 C69 172.8(6) . . . . ? C74 N8 C71 C64 -178.3(5) . . . . ? Ge2 N8 C71 C64 14.3(8) . . . . ? C74 N8 C71 C72 -0.1(6) . . . . ? Ge2 N8 C71 C72 -167.6(4) . . . . ? C63 C64 C71 N8 4.3(8) . . . . ? C65 C64 C71 N8 -179.1(5) . . . . ? C63 C64 C71 C72 -173.3(6) . . . . ? C65 C64 C71 C72 3.3(9) . . . . ? N8 C71 C72 C73 -0.4(6) . . . . ? C64 C71 C72 C73 177.5(6) . . . . ? C71 C72 C73 C74 0.7(6) . . . . ? C71 N8 C74 C38 -179.9(4) . . . . ? Ge2 N8 C74 C38 -10.3(6) . . . . ? C71 N8 C74 C73 0.5(6) . . . . ? Ge2 N8 C74 C73 170.2(3) . . . . ? N7 C38 C74 N8 0.2(7) . . . . ? C39 C38 C74 N8 -178.1(6) . . . . ? N7 C38 C74 C73 179.6(6) . . . . ? C39 C38 C74 C73 1.3(13) . . . . ? C72 C73 C74 N8 -0.7(6) . . . . ? C72 C73 C74 C38 179.8(6) . . . . ? C75 C76 C77 C78 -179.6(5) . . . . ? C76 C77 C78 C79 -175.2(5) . . . . ? C77 C78 C79 C80 178.8(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O1 0.84 2.01 2.841(5) 172.4 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.804 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 945439'