# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Heinz Gornitzka' _publ_contact_author_email HEINZ.GORNITZKA@LCC-TOULOUSE.FR _publ_section_title ; Reactions of germenes with various naphthoquinones controlled by substituent effects ; loop_ _publ_author_name 'Heinz Gornitzka' 'Jean Escudie' 'Dumitru Ghereg' 'Henri Ranaivonjatovo' # Attachment 'DumitruDalton.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 751860' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H46 Ge' _chemical_formula_weight 587.35 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' 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 C2/c 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' '-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 15.315(2) _cell_length_b 20.473(3) _cell_length_c 11.6852(16) _cell_angle_alpha 90.00 _cell_angle_beta 113.839(2) _cell_angle_gamma 90.00 _cell_volume 3351.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2544 _cell_measurement_theta_min 2.755 _cell_measurement_theta_max 25.517 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.379405 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _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 'Bruker CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8738 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 5.19 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3053 _reflns_number_gt 2204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3053 _refine_ls_number_parameters 213 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 1.0000 0.43573(2) 0.2500 0.03327(17) Uani 1 2 d S . . C1 C 1.0000 0.52393(19) 0.2500 0.0357(10) Uani 1 2 d S . . C2 C 0.9179(2) 0.56745(13) 0.1920(2) 0.0347(6) Uani 1 1 d . . . C3 C 0.8209(2) 0.55427(14) 0.1251(3) 0.0411(8) Uani 1 1 d . . . H3 H 0.8002 0.5102 0.1092 0.049 Uiso 1 1 calc R . . C4 C 0.7540(2) 0.60430(15) 0.0812(3) 0.0435(8) Uani 1 1 d . A . C5 C 0.7871(3) 0.66870(15) 0.1090(3) 0.0507(9) Uani 1 1 d . . . H5 H 0.7424 0.7036 0.0819 0.061 Uiso 1 1 calc R . . C6 C 0.8818(3) 0.68282(15) 0.1739(3) 0.0496(9) Uani 1 1 d . . . H6 H 0.9019 0.7270 0.1909 0.060 Uiso 1 1 calc R . . C7 C 0.9484(2) 0.63304(13) 0.2147(3) 0.0380(7) Uani 1 1 d . . . C8 C 0.6481(3) 0.58841(16) 0.0095(3) 0.0539(9) Uani 1 1 d DU . . C9 C 0.5960(16) 0.5866(16) 0.0993(18) 0.103(7) Uani 0.44(3) 1 d PDU A 1 H9A H 0.6067 0.5441 0.1415 0.155 Uiso 0.44(3) 1 calc PR A 1 H9B H 0.5274 0.5932 0.0512 0.155 Uiso 0.44(3) 1 calc PR A 1 H9C H 0.6210 0.6213 0.1619 0.155 Uiso 0.44(3) 1 calc PR A 1 C10 C 0.6213(18) 0.5240(10) -0.062(3) 0.155(11) Uani 0.44(3) 1 d PDU A 1 H10A H 0.6595 0.5182 -0.1110 0.232 Uiso 0.44(3) 1 calc PR A 1 H10B H 0.5534 0.5246 -0.1177 0.232 Uiso 0.44(3) 1 calc PR A 1 H10C H 0.6338 0.4879 -0.0022 0.232 Uiso 0.44(3) 1 calc PR A 1 C11 C 0.5997(16) 0.6440(9) -0.0812(18) 0.096(6) Uani 0.44(3) 1 d PDU A 1 H11A H 0.6078 0.6849 -0.0344 0.144 Uiso 0.44(3) 1 calc PR A 1 H11B H 0.5315 0.6345 -0.1255 0.144 Uiso 0.44(3) 1 calc PR A 1 H11C H 0.6287 0.6483 -0.1417 0.144 Uiso 0.44(3) 1 calc PR A 1 C9' C 0.6154(17) 0.5593(14) 0.1042(16) 0.137(8) Uani 0.56(3) 1 d PDU A 2 H9'1 H 0.6522 0.5196 0.1398 0.205 Uiso 0.56(3) 1 calc PR A 2 H9'2 H 0.5474 0.5484 0.0631 0.205 Uiso 0.56(3) 1 calc PR A 2 H9'3 H 0.6253 0.5910 0.1711 0.205 Uiso 0.56(3) 1 calc PR A 2 C10' C 0.6424(11) 0.5387(9) -0.0903(14) 0.106(6) Uani 0.56(3) 1 d PDU A 2 H10D H 0.6825 0.5532 -0.1329 0.159 Uiso 0.56(3) 1 calc PR A 2 H10E H 0.5761 0.5348 -0.1513 0.159 Uiso 0.56(3) 1 calc PR A 2 H10F H 0.6649 0.4962 -0.0509 0.159 Uiso 0.56(3) 1 calc PR A 2 C11' C 0.5839(15) 0.6448(6) -0.0567(19) 0.109(6) Uani 0.56(3) 1 d PDU A 2 H11D H 0.5827 0.6767 0.0053 0.164 Uiso 0.56(3) 1 calc PR A 2 H11E H 0.5192 0.6286 -0.1049 0.164 Uiso 0.56(3) 1 calc PR A 2 H11F H 0.6083 0.6658 -0.1132 0.164 Uiso 0.56(3) 1 calc PR A 2 C12 C 1.1174(2) 0.38813(12) 0.3366(3) 0.0336(7) Uani 1 1 d . . . C13 C 1.1551(2) 0.35032(14) 0.2659(3) 0.0403(7) Uani 1 1 d . . . C14 C 1.2419(2) 0.31853(15) 0.3275(4) 0.0509(9) Uani 1 1 d . . . H14 H 1.2673 0.2936 0.2796 0.061 Uiso 1 1 calc R . . C15 C 1.2927(2) 0.32180(15) 0.4556(4) 0.0509(9) Uani 1 1 d . . . C16 C 1.2534(2) 0.35856(16) 0.5227(3) 0.0486(8) Uani 1 1 d . . . H16 H 1.2871 0.3614 0.6109 0.058 Uiso 1 1 calc R . . C17 C 1.1675(2) 0.39115(13) 0.4670(3) 0.0385(7) Uani 1 1 d . . . C18 C 1.1040(2) 0.34550(17) 0.1258(3) 0.0554(9) Uani 1 1 d . . . H18A H 1.1387 0.3156 0.0937 0.083 Uiso 1 1 calc R . . H18B H 1.1008 0.3888 0.0886 0.083 Uiso 1 1 calc R . . H18C H 1.0392 0.3290 0.1039 0.083 Uiso 1 1 calc R . . C19 C 1.3862(2) 0.28673(19) 0.5207(4) 0.0760(13) Uani 1 1 d . . . H19A H 1.4036 0.2648 0.4584 0.114 Uiso 1 1 calc R . . H19B H 1.3799 0.2543 0.5785 0.114 Uiso 1 1 calc R . . H19C H 1.4359 0.3183 0.5675 0.114 Uiso 1 1 calc R . . C20 C 1.1305(2) 0.43024(16) 0.5483(3) 0.0519(8) Uani 1 1 d . . . H20A H 1.0831 0.4044 0.5649 0.078 Uiso 1 1 calc R . . H20B H 1.1010 0.4706 0.5050 0.078 Uiso 1 1 calc R . . H20C H 1.1837 0.4410 0.6276 0.078 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 0.0523(3) 0.0232(2) 0.0300(3) 0.000 0.0225(2) 0.000 C1 0.056(3) 0.026(2) 0.034(2) 0.000 0.028(2) 0.000 C2 0.060(2) 0.0243(14) 0.0315(15) 0.0003(13) 0.0305(14) 0.0007(16) C3 0.066(2) 0.0301(17) 0.0360(17) 0.0028(13) 0.0302(16) 0.0048(15) C4 0.065(2) 0.0359(19) 0.0397(18) 0.0062(14) 0.0316(17) 0.0119(16) C5 0.078(3) 0.0348(19) 0.051(2) 0.0091(15) 0.037(2) 0.0169(18) C6 0.086(3) 0.0249(17) 0.053(2) 0.0001(14) 0.043(2) 0.0013(17) C7 0.067(2) 0.0245(16) 0.0384(18) 0.0043(12) 0.0376(17) 0.0047(13) C8 0.070(2) 0.044(2) 0.047(2) 0.0065(15) 0.0220(19) 0.0129(17) C9 0.060(8) 0.194(19) 0.059(8) 0.048(8) 0.027(6) 0.028(10) C10 0.081(11) 0.093(9) 0.29(3) -0.104(13) 0.078(15) -0.014(9) C11 0.062(10) 0.124(11) 0.071(9) 0.061(8) -0.003(8) 0.008(8) C9' 0.079(12) 0.22(2) 0.101(9) 0.040(9) 0.023(8) -0.067(12) C10' 0.043(7) 0.124(10) 0.097(8) -0.060(7) -0.028(6) 0.026(6) C11' 0.092(9) 0.054(6) 0.193(15) 0.019(7) 0.070(10) 0.021(5) C12 0.0499(18) 0.0231(15) 0.0339(17) 0.0015(11) 0.0234(15) -0.0039(13) C13 0.053(2) 0.0288(16) 0.0479(19) -0.0003(14) 0.0295(16) -0.0028(15) C14 0.056(2) 0.0347(18) 0.076(3) 0.0018(16) 0.041(2) 0.0016(16) C15 0.045(2) 0.0333(18) 0.075(3) 0.0154(17) 0.0238(19) -0.0048(15) C16 0.052(2) 0.0438(19) 0.043(2) 0.0107(15) 0.0115(17) -0.0111(17) C17 0.051(2) 0.0310(16) 0.0367(18) 0.0052(13) 0.0214(16) -0.0042(14) C18 0.069(2) 0.059(2) 0.050(2) -0.0140(17) 0.0369(19) 0.0024(18) C19 0.045(2) 0.060(3) 0.116(4) 0.029(2) 0.025(2) 0.0014(19) C20 0.073(2) 0.059(2) 0.0276(16) -0.0008(16) 0.0236(16) -0.0031(19) _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 C1 1.806(4) . ? Ge1 C12 1.932(3) . ? Ge1 C12 1.932(3) 2_755 ? C1 C2 1.465(4) 2_755 ? C1 C2 1.465(4) . ? C2 C3 1.397(4) . ? C2 C7 1.412(4) . ? C3 C4 1.392(4) . ? C4 C5 1.403(4) . ? C4 C8 1.529(5) . ? C5 C6 1.369(5) . ? C6 C7 1.383(4) . ? C7 C7 1.457(6) 2_755 ? C8 C9' 1.509(11) . ? C8 C11' 1.511(11) . ? C8 C10' 1.523(9) . ? C8 C10 1.524(13) . ? C8 C11 1.528(11) . ? C8 C9 1.555(12) . ? C12 C17 1.404(4) . ? C12 C13 1.415(4) . ? C13 C14 1.391(4) . ? C13 C18 1.506(4) . ? C14 C15 1.381(5) . ? C15 C16 1.387(5) . ? C15 C19 1.504(5) . ? C16 C17 1.381(4) . ? C17 C20 1.516(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ge1 C12 120.29(8) . . ? C1 Ge1 C12 120.29(8) . 2_755 ? C12 Ge1 C12 119.43(15) . 2_755 ? C2 C1 C2 105.1(3) 2_755 . ? C2 C1 Ge1 127.46(17) 2_755 . ? C2 C1 Ge1 127.46(17) . . ? C3 C2 C7 119.1(3) . . ? C3 C2 C1 131.4(3) . . ? C7 C2 C1 109.5(3) . . ? C4 C3 C2 121.5(3) . . ? C3 C4 C5 117.6(3) . . ? C3 C4 C8 120.3(3) . . ? C5 C4 C8 122.1(3) . . ? C6 C5 C4 122.0(3) . . ? C5 C6 C7 120.3(3) . . ? C6 C7 C2 119.6(3) . . ? C6 C7 C7 132.45(19) . 2_755 ? C2 C7 C7 107.92(17) . 2_755 ? C9' C8 C11' 109.7(10) . . ? C9' C8 C10' 111.4(10) . . ? C11' C8 C10' 107.1(8) . . ? C9' C8 C10 87.9(16) . . ? C11' C8 C10 113.9(14) . . ? C10' C8 C10 23.8(16) . . ? C9' C8 C11 126.2(14) . . ? C11' C8 C11 16.8(15) . . ? C10' C8 C11 96.0(11) . . ? C10 C8 C11 108.5(12) . . ? C9' C8 C4 106.0(9) . . ? C11' C8 C4 116.4(9) . . ? C10' C8 C4 106.4(7) . . ? C10 C8 C4 118.4(10) . . ? C11 C8 C4 109.4(9) . . ? C9' C8 C9 23.5(15) . . ? C11' C8 C9 87.6(12) . . ? C10' C8 C9 127.9(15) . . ? C10 C8 C9 104.5(13) . . ? C11 C8 C9 104.4(10) . . ? C4 C8 C9 110.8(10) . . ? C17 C12 C13 119.0(3) . . ? C17 C12 Ge1 122.1(2) . . ? C13 C12 Ge1 118.9(2) . . ? C14 C13 C12 119.0(3) . . ? C14 C13 C18 120.0(3) . . ? C12 C13 C18 121.0(3) . . ? C15 C14 C13 122.7(3) . . ? C14 C15 C16 117.1(3) . . ? C14 C15 C19 121.9(4) . . ? C16 C15 C19 121.0(4) . . ? C17 C16 C15 123.0(3) . . ? C16 C17 C12 119.3(3) . . ? C16 C17 C20 119.1(3) . . ? C12 C17 C20 121.6(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.401 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.055 _vrf_PLAT242_5 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C8 RESPONSE: C8 is a central carbon atom of a disordered t-butyl group. ; _vrf_PLAT761_5 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen atoms were refined using a riding model. ; _vrf_PLAT762_5 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen atoms were refined using a riding model. ; #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 751861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75.50 H74 Ge2 O5' _chemical_formula_weight 1206.53 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3584(3) _cell_length_b 14.2970(4) _cell_length_c 20.0687(5) _cell_angle_alpha 74.574(2) _cell_angle_beta 81.440(2) _cell_angle_gamma 72.261(2) _cell_volume 2984.03(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5615 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1262 _exptl_absorpt_coefficient_mu 1.061 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.6189 _exptl_absorpt_correction_T_max 0.9013 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26341 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10826 _reflns_number_gt 7030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10826 _refine_ls_number_parameters 779 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.971 _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 0.67583(3) -0.05922(3) 0.189391(19) 0.02524(11) Uani 1 1 d . . . Ge2 Ge 0.67490(3) 0.39996(3) 0.246884(19) 0.02563(11) Uani 1 1 d . . . O1 O 0.48196(19) 0.21321(16) 0.15994(12) 0.0304(6) Uani 1 1 d . . . O2 O 0.5009(2) 0.30321(16) 0.17606(12) 0.0283(6) Uani 1 1 d . . . O3 O 0.6519(2) 0.46359(19) 0.02265(13) 0.0387(6) Uani 1 1 d . . . O4 O 0.5784(2) 0.05839(17) 0.13955(12) 0.0315(6) Uani 1 1 d . . . O5 O 0.6293(2) 0.40021(16) 0.16343(12) 0.0285(6) Uani 1 1 d . . . C1 C 0.6043(3) 0.1436(2) 0.14517(18) 0.0251(8) Uani 1 1 d . . . C2 C 0.6521(3) 0.2007(3) 0.07801(18) 0.0262(8) Uani 1 1 d . . . C3 C 0.6757(3) 0.1698(3) 0.01643(19) 0.0345(9) Uani 1 1 d . . . H3 H 0.6728 0.1045 0.0153 0.041 Uiso 1 1 calc R . . C4 C 0.7032(3) 0.2358(3) -0.0430(2) 0.0412(10) Uani 1 1 d . . . H4 H 0.7252 0.2141 -0.0851 0.049 Uiso 1 1 calc R . . C5 C 0.6994(3) 0.3340(3) -0.0427(2) 0.0406(10) Uani 1 1 d . . . H5 H 0.7156 0.3793 -0.0848 0.049 Uiso 1 1 calc R . . C6 C 0.6721(3) 0.3663(3) 0.01922(19) 0.0324(9) Uani 1 1 d . . . C7 C 0.6576(3) 0.2952(3) 0.08132(18) 0.0266(8) Uani 1 1 d . . . C8 C 0.6307(3) 0.3087(2) 0.15459(18) 0.0252(8) Uani 1 1 d . . . C9 C 0.7162(3) 0.2191(2) 0.20561(17) 0.0223(8) Uani 1 1 d . . . H9 H 0.8034 0.2095 0.1846 0.027 Uiso 1 1 calc R . . C10 C 0.6787(3) 0.1223(2) 0.20850(17) 0.0218(8) Uani 1 1 d . . . H10 H 0.6181 0.1154 0.2498 0.026 Uiso 1 1 calc R . . C11 C 0.6517(4) 0.5380(3) -0.0413(2) 0.0510(11) Uani 1 1 d . . . H11A H 0.7351 0.5256 -0.0648 0.077 Uiso 1 1 calc R . . H11B H 0.6266 0.6054 -0.0318 0.077 Uiso 1 1 calc R . . H11C H 0.5932 0.5339 -0.0710 0.077 Uiso 1 1 calc R . . C12 C 0.7113(3) 0.2455(2) 0.27705(17) 0.0232(8) Uani 1 1 d . . . C13 C 0.6225(3) 0.2095(2) 0.33494(18) 0.0274(8) Uani 1 1 d . . . C14 C 0.4964(3) 0.2186(3) 0.3356(2) 0.0348(9) Uani 1 1 d . . . H14 H 0.4531 0.2519 0.2950 0.042 Uiso 1 1 calc R . . C15 C 0.4352(4) 0.1780(3) 0.3968(2) 0.0445(11) Uani 1 1 d . . . H15 H 0.3497 0.1828 0.3976 0.053 Uiso 1 1 calc R . . C16 C 0.4968(4) 0.1310(3) 0.4563(2) 0.0472(11) Uani 1 1 d . . . H16 H 0.4530 0.1046 0.4976 0.057 Uiso 1 1 calc R . . C17 C 0.6217(4) 0.1217(3) 0.4567(2) 0.0386(10) Uani 1 1 d . . . H17 H 0.6636 0.0897 0.4980 0.046 Uiso 1 1 calc R . . C18 C 0.6844(3) 0.1600(3) 0.39590(19) 0.0300(9) Uani 1 1 d . . . C19 C 0.8149(3) 0.1578(2) 0.38105(18) 0.0275(8) Uani 1 1 d . . . C20 C 0.9128(4) 0.1195(3) 0.4239(2) 0.0370(10) Uani 1 1 d . . . H20 H 0.8993 0.0898 0.4717 0.044 Uiso 1 1 calc R . . C21 C 1.0291(4) 0.1255(3) 0.3961(2) 0.0438(11) Uani 1 1 d . . . H21 H 1.0962 0.1008 0.4251 0.053 Uiso 1 1 calc R . . C22 C 1.0493(3) 0.1670(3) 0.3262(2) 0.0359(10) Uani 1 1 d . . . H22 H 1.1307 0.1693 0.3078 0.043 Uiso 1 1 calc R . . C23 C 0.9527(3) 0.2054(3) 0.2824(2) 0.0297(8) Uani 1 1 d . . . H23 H 0.9676 0.2330 0.2344 0.036 Uiso 1 1 calc R . . C24 C 0.8336(3) 0.2023(2) 0.31064(18) 0.0237(8) Uani 1 1 d . . . C25 C 0.8309(3) 0.4384(3) 0.2352(2) 0.0302(9) Uani 1 1 d . . . C26 C 0.9039(3) 0.4532(3) 0.1722(2) 0.0355(9) Uani 1 1 d . . . C27 C 1.0229(4) 0.4624(3) 0.1729(2) 0.0452(11) Uani 1 1 d . . . H27 H 1.0711 0.4739 0.1302 0.054 Uiso 1 1 calc R . . C28 C 1.0731(4) 0.4555(3) 0.2334(2) 0.0464(11) Uani 1 1 d . . . C29 C 0.9982(4) 0.4467(3) 0.2943(2) 0.0453(11) Uani 1 1 d . . . H29 H 1.0289 0.4467 0.3358 0.054 Uiso 1 1 calc R . . C30 C 0.8778(3) 0.4378(3) 0.2964(2) 0.0341(9) Uani 1 1 d . . . C31 C 0.8627(4) 0.4592(4) 0.1031(2) 0.0550(12) Uani 1 1 d . . . H31A H 0.9209 0.4831 0.0662 0.082 Uiso 1 1 calc R . . H31B H 0.7797 0.5063 0.0973 0.082 Uiso 1 1 calc R . . H31C H 0.8607 0.3921 0.1008 0.082 Uiso 1 1 calc R . . C32 C 1.2066(4) 0.4559(5) 0.2323(3) 0.0753(16) Uani 1 1 d . . . H32A H 1.2603 0.4063 0.2073 0.113 Uiso 1 1 calc R . . H32B H 1.2307 0.4382 0.2800 0.113 Uiso 1 1 calc R . . H32C H 1.2151 0.5233 0.2090 0.113 Uiso 1 1 calc R . . C33 C 0.8052(4) 0.4238(3) 0.3655(2) 0.0421(10) Uani 1 1 d . . . H33A H 0.7934 0.3560 0.3787 0.063 Uiso 1 1 calc R . . H33B H 0.7242 0.4744 0.3624 0.063 Uiso 1 1 calc R . . H33C H 0.8506 0.4320 0.4005 0.063 Uiso 1 1 calc R . . C34 C 0.5262(3) 0.4961(2) 0.27864(19) 0.0286(8) Uani 1 1 d . . . C35 C 0.4809(3) 0.5864(3) 0.2276(2) 0.0347(9) Uani 1 1 d . . . C36 C 0.3626(4) 0.6483(3) 0.2394(2) 0.0426(11) Uani 1 1 d . . . H36 H 0.3323 0.7086 0.2054 0.051 Uiso 1 1 calc R . . C37 C 0.2877(4) 0.6254(3) 0.2988(2) 0.0454(11) Uani 1 1 d . . . C38 C 0.3384(4) 0.5434(3) 0.3505(2) 0.0394(10) Uani 1 1 d . . . H38 H 0.2907 0.5298 0.3932 0.047 Uiso 1 1 calc R . . C39 C 0.4574(3) 0.4799(3) 0.34212(19) 0.0323(9) Uani 1 1 d . . . C40 C 0.5556(4) 0.6189(3) 0.1612(2) 0.0409(10) Uani 1 1 d . . . H40A H 0.5584 0.5765 0.1294 0.061 Uiso 1 1 calc R . . H40B H 0.6401 0.6113 0.1715 0.061 Uiso 1 1 calc R . . H40C H 0.5167 0.6897 0.1395 0.061 Uiso 1 1 calc R . . C41 C 0.1526(4) 0.6855(4) 0.3068(3) 0.0777(17) Uani 1 1 d . . . H41A H 0.0997 0.6522 0.2930 0.117 Uiso 1 1 calc R . . H41B H 0.1408 0.7540 0.2774 0.117 Uiso 1 1 calc R . . H41C H 0.1303 0.6892 0.3554 0.117 Uiso 1 1 calc R . . C42 C 0.5060(4) 0.4012(3) 0.40550(19) 0.0397(10) Uani 1 1 d . . . H42A H 0.5842 0.3547 0.3926 0.060 Uiso 1 1 calc R . . H42B H 0.4453 0.3633 0.4258 0.060 Uiso 1 1 calc R . . H42C H 0.5202 0.4341 0.4394 0.060 Uiso 1 1 calc R . . C43 C 0.7789(3) 0.0177(2) 0.21750(17) 0.0224(8) Uani 1 1 d . . . C44 C 0.8155(3) -0.0285(2) 0.29126(18) 0.0236(8) Uani 1 1 d . . . C45 C 0.7426(3) -0.0503(2) 0.35223(18) 0.0286(8) Uani 1 1 d . . . H45 H 0.6550 -0.0334 0.3520 0.034 Uiso 1 1 calc R . . C46 C 0.8003(3) -0.0974(3) 0.41350(19) 0.0346(9) Uani 1 1 d . . . H46 H 0.7516 -0.1141 0.4553 0.042 Uiso 1 1 calc R . . C47 C 0.9281(4) -0.1204(3) 0.4147(2) 0.0377(10) Uani 1 1 d . . . H47 H 0.9658 -0.1531 0.4572 0.045 Uiso 1 1 calc R . . C48 C 1.0003(3) -0.0965(3) 0.3553(2) 0.0357(10) Uani 1 1 d . . . H48 H 1.0874 -0.1106 0.3565 0.043 Uiso 1 1 calc R . . C49 C 0.9444(3) -0.0512(2) 0.29299(18) 0.0258(8) Uani 1 1 d . . . C50 C 0.9981(3) -0.0223(2) 0.22260(18) 0.0254(8) Uani 1 1 d . . . C51 C 1.1222(3) -0.0329(3) 0.1977(2) 0.0368(10) Uani 1 1 d . . . H51 H 1.1861 -0.0589 0.2288 0.044 Uiso 1 1 calc R . . C52 C 1.1504(3) -0.0051(3) 0.1272(2) 0.0417(10) Uani 1 1 d . . . H52 H 1.2343 -0.0114 0.1097 0.050 Uiso 1 1 calc R . . C53 C 1.0572(3) 0.0322(3) 0.0817(2) 0.0412(10) Uani 1 1 d . . . H53 H 1.0779 0.0503 0.0332 0.049 Uiso 1 1 calc R . . C54 C 0.9337(3) 0.0432(3) 0.10640(19) 0.0339(9) Uani 1 1 d . . . H54 H 0.8705 0.0692 0.0748 0.041 Uiso 1 1 calc R . . C55 C 0.9028(3) 0.0164(2) 0.17673(18) 0.0244(8) Uani 1 1 d . . . C56 C 0.7340(3) -0.1374(3) 0.11793(18) 0.0285(8) Uani 1 1 d . . . C57 C 0.8571(3) -0.1919(3) 0.1045(2) 0.0326(9) Uani 1 1 d . . . C58 C 0.8876(4) -0.2357(3) 0.0475(2) 0.0447(11) Uani 1 1 d . . . H58 H 0.9712 -0.2720 0.0385 0.054 Uiso 1 1 calc R . . C59 C 0.8001(4) -0.2278(3) 0.0037(2) 0.0445(10) Uani 1 1 d . . . C60 C 0.6779(4) -0.1795(3) 0.0201(2) 0.0380(10) Uani 1 1 d . . . H60 H 0.6160 -0.1766 -0.0081 0.046 Uiso 1 1 calc R . . C61 C 0.6425(3) -0.1352(3) 0.07628(19) 0.0289(8) Uani 1 1 d . . . C62 C 0.9613(3) -0.2091(3) 0.1499(2) 0.0459(11) Uani 1 1 d . . . H62A H 0.9285 -0.1769 0.1888 0.069 Uiso 1 1 calc R . . H62B H 1.0258 -0.1798 0.1225 0.069 Uiso 1 1 calc R . . H62C H 0.9968 -0.2818 0.1678 0.069 Uiso 1 1 calc R . . C63 C 0.8367(5) -0.2692(4) -0.0610(2) 0.0697(15) Uani 1 1 d . . . H63A H 0.7637 -0.2517 -0.0873 0.105 Uiso 1 1 calc R . . H63B H 0.8698 -0.3428 -0.0477 0.105 Uiso 1 1 calc R . . H63C H 0.9001 -0.2399 -0.0898 0.105 Uiso 1 1 calc R . . C64 C 0.5052(3) -0.0885(3) 0.0915(2) 0.0365(9) Uani 1 1 d . . . H64A H 0.4853 -0.0151 0.0741 0.055 Uiso 1 1 calc R . . H64B H 0.4845 -0.1048 0.1416 0.055 Uiso 1 1 calc R . . H64C H 0.4570 -0.1156 0.0685 0.055 Uiso 1 1 calc R . . C65 C 0.5739(3) -0.1217(3) 0.26620(18) 0.0291(8) Uani 1 1 d . . . C66 C 0.4498(3) -0.0724(3) 0.28633(19) 0.0308(9) Uani 1 1 d . . . C67 C 0.3845(3) -0.1246(3) 0.3404(2) 0.0379(10) Uani 1 1 d . . . H67 H 0.3021 -0.0906 0.3539 0.046 Uiso 1 1 calc R . . C68 C 0.4344(4) -0.2237(3) 0.3754(2) 0.0404(10) Uani 1 1 d . . . C69 C 0.5550(4) -0.2707(3) 0.3549(2) 0.0429(10) Uani 1 1 d . . . H69 H 0.5913 -0.3388 0.3777 0.052 Uiso 1 1 calc R . . C70 C 0.6253(3) -0.2219(3) 0.3021(2) 0.0347(9) Uani 1 1 d . . . C71 C 0.3810(3) 0.0350(3) 0.2533(2) 0.0468(11) Uani 1 1 d . . . H71A H 0.2950 0.0500 0.2731 0.070 Uiso 1 1 calc R . . H71B H 0.3822 0.0429 0.2032 0.070 Uiso 1 1 calc R . . H71C H 0.4213 0.0817 0.2621 0.070 Uiso 1 1 calc R . . C72 C 0.3595(4) -0.2765(4) 0.4330(2) 0.0540(12) Uani 1 1 d . . . H72A H 0.3931 -0.3498 0.4390 0.081 Uiso 1 1 calc R . . H72B H 0.2730 -0.2560 0.4214 0.081 Uiso 1 1 calc R . . H72C H 0.3635 -0.2582 0.4761 0.081 Uiso 1 1 calc R . . C73 C 0.7585(4) -0.2781(3) 0.2851(2) 0.0505(11) Uani 1 1 d . . . H73A H 0.7800 -0.3445 0.3175 0.076 Uiso 1 1 calc R . . H73B H 0.8137 -0.2393 0.2892 0.076 Uiso 1 1 calc R . . H73C H 0.7677 -0.2869 0.2376 0.076 Uiso 1 1 calc R . . C74 C 0.8356(14) 0.6482(11) 0.5193(10) 0.120(6) Uani 0.50 1 d PDU A -1 H74A H 0.8092 0.6016 0.5600 0.180 Uiso 0.50 1 calc PR A -1 H74B H 0.7651 0.6856 0.4911 0.180 Uiso 0.50 1 calc PR A -1 H74C H 0.8662 0.6958 0.5344 0.180 Uiso 0.50 1 calc PR A -1 C75 C 0.9281(19) 0.5947(14) 0.4809(11) 0.138(8) Uani 0.50 1 d PDU A -1 H75A H 0.8901 0.5775 0.4461 0.166 Uiso 0.50 1 calc PR A -1 H75B H 0.9805 0.6388 0.4554 0.166 Uiso 0.50 1 calc PR A -1 C76 C 1.0013(12) 0.5092(10) 0.5171(7) 0.074(4) Uani 0.50 1 d PDU A -1 H76A H 1.0372 0.5286 0.5517 0.088 Uiso 0.50 1 calc PR A -1 H76B H 0.9462 0.4679 0.5434 0.088 Uiso 0.50 1 calc PR A -1 C77 C 1.0871(17) 0.4531(16) 0.4895(10) 0.126(7) Uani 0.50 1 d PDU A -1 H77A H 1.1301 0.4980 0.4551 0.151 Uiso 0.50 1 calc PR A -1 H77B H 1.0480 0.4236 0.4624 0.151 Uiso 0.50 1 calc PR A -1 C78 C 1.1777(17) 0.3758(13) 0.5214(9) 0.108(5) Uani 0.50 1 d PDU A -1 H78A H 1.2242 0.4014 0.5465 0.161 Uiso 0.50 1 calc PR A -1 H78B H 1.2338 0.3436 0.4868 0.161 Uiso 0.50 1 calc PR A -1 H78C H 1.1409 0.3262 0.5542 0.161 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.02057(19) 0.0247(2) 0.0310(2) -0.00688(17) -0.00856(17) -0.00376(16) Ge2 0.0252(2) 0.0228(2) 0.0275(2) -0.00419(16) -0.00738(17) -0.00367(16) O1 0.0212(12) 0.0255(13) 0.0441(16) -0.0062(11) -0.0111(11) -0.0037(10) O2 0.0245(12) 0.0238(13) 0.0352(15) -0.0058(11) -0.0059(11) -0.0038(10) O3 0.0455(16) 0.0355(15) 0.0323(16) 0.0056(12) -0.0109(13) -0.0150(13) O4 0.0294(13) 0.0261(13) 0.0422(16) -0.0071(11) -0.0192(12) -0.0053(11) O5 0.0351(13) 0.0225(12) 0.0266(14) 0.0001(10) -0.0125(11) -0.0064(11) C1 0.0237(17) 0.0242(18) 0.029(2) -0.0054(16) -0.0090(16) -0.0054(15) C2 0.0232(17) 0.0279(19) 0.026(2) -0.0053(16) -0.0136(16) -0.0011(15) C3 0.031(2) 0.038(2) 0.031(2) -0.0082(19) -0.0168(18) 0.0020(17) C4 0.038(2) 0.056(3) 0.030(2) -0.017(2) -0.0128(19) -0.005(2) C5 0.039(2) 0.058(3) 0.022(2) -0.001(2) -0.0062(18) -0.016(2) C6 0.0286(19) 0.035(2) 0.032(2) -0.0004(18) -0.0100(17) -0.0102(17) C7 0.0224(17) 0.031(2) 0.024(2) -0.0023(16) -0.0088(16) -0.0049(15) C8 0.0240(17) 0.0220(18) 0.027(2) -0.0027(15) -0.0043(16) -0.0042(15) C9 0.0172(16) 0.0225(17) 0.0236(19) -0.0006(15) -0.0057(14) -0.0026(14) C10 0.0188(16) 0.0237(18) 0.0207(19) -0.0037(15) -0.0075(14) -0.0014(14) C11 0.054(3) 0.045(3) 0.040(3) 0.013(2) -0.005(2) -0.014(2) C12 0.0246(17) 0.0200(17) 0.023(2) -0.0046(15) -0.0040(15) -0.0032(15) C13 0.0309(19) 0.0234(18) 0.027(2) -0.0084(16) -0.0029(17) -0.0028(16) C14 0.031(2) 0.036(2) 0.036(2) -0.0107(18) 0.0012(18) -0.0063(17) C15 0.038(2) 0.046(3) 0.049(3) -0.012(2) 0.009(2) -0.015(2) C16 0.052(3) 0.041(2) 0.042(3) -0.005(2) 0.014(2) -0.015(2) C17 0.052(3) 0.032(2) 0.026(2) -0.0053(17) 0.002(2) -0.0068(19) C18 0.039(2) 0.0225(18) 0.027(2) -0.0065(16) 0.0020(18) -0.0062(16) C19 0.035(2) 0.0199(17) 0.025(2) -0.0070(15) -0.0061(17) 0.0006(16) C20 0.047(2) 0.035(2) 0.024(2) -0.0072(17) -0.0127(19) 0.0001(19) C21 0.039(2) 0.043(2) 0.047(3) -0.015(2) -0.025(2) 0.0052(19) C22 0.0222(18) 0.038(2) 0.050(3) -0.022(2) -0.0095(18) 0.0015(17) C23 0.0284(19) 0.0282(19) 0.034(2) -0.0102(17) -0.0063(17) -0.0055(16) C24 0.0251(18) 0.0188(17) 0.028(2) -0.0085(15) -0.0056(16) -0.0027(14) C25 0.0264(18) 0.0239(19) 0.040(2) -0.0070(17) -0.0083(18) -0.0046(16) C26 0.0273(19) 0.038(2) 0.041(3) -0.0045(19) -0.0075(19) -0.0109(17) C27 0.033(2) 0.057(3) 0.048(3) -0.015(2) 0.001(2) -0.015(2) C28 0.034(2) 0.057(3) 0.057(3) -0.020(2) -0.006(2) -0.019(2) C29 0.045(2) 0.046(3) 0.054(3) -0.021(2) -0.015(2) -0.011(2) C30 0.035(2) 0.0262(19) 0.045(3) -0.0110(18) -0.0115(19) -0.0077(17) C31 0.042(2) 0.088(4) 0.037(3) -0.004(2) -0.001(2) -0.031(2) C32 0.045(3) 0.120(5) 0.080(4) -0.039(3) -0.009(3) -0.035(3) C33 0.047(2) 0.043(2) 0.041(3) -0.016(2) -0.016(2) -0.009(2) C34 0.0306(19) 0.0216(18) 0.034(2) -0.0064(16) -0.0130(18) -0.0026(15) C35 0.041(2) 0.0245(19) 0.040(2) -0.0100(18) -0.0150(19) -0.0043(17) C36 0.053(3) 0.026(2) 0.043(3) -0.0089(19) -0.023(2) 0.0074(19) C37 0.045(2) 0.041(2) 0.044(3) -0.023(2) -0.013(2) 0.012(2) C38 0.041(2) 0.042(2) 0.034(2) -0.0176(19) -0.0063(19) 0.0012(19) C39 0.037(2) 0.0246(19) 0.034(2) -0.0101(17) -0.0123(18) 0.0006(16) C40 0.047(2) 0.026(2) 0.047(3) -0.0014(18) -0.010(2) -0.0089(19) C41 0.059(3) 0.084(4) 0.062(3) -0.027(3) -0.012(3) 0.033(3) C42 0.046(2) 0.031(2) 0.037(2) -0.0094(18) -0.0078(19) 0.0008(18) C43 0.0196(16) 0.0233(17) 0.0231(19) -0.0061(15) -0.0073(15) -0.0011(14) C44 0.0236(17) 0.0200(17) 0.026(2) -0.0041(15) -0.0078(16) -0.0033(14) C45 0.0274(18) 0.0264(19) 0.033(2) -0.0077(17) -0.0069(17) -0.0058(16) C46 0.039(2) 0.031(2) 0.028(2) -0.0036(17) -0.0045(18) -0.0030(18) C47 0.045(2) 0.037(2) 0.027(2) -0.0059(18) -0.016(2) -0.0013(19) C48 0.0286(19) 0.039(2) 0.037(2) -0.0120(19) -0.0134(19) 0.0027(17) C49 0.0252(18) 0.0226(18) 0.030(2) -0.0085(16) -0.0093(16) -0.0017(15) C50 0.0207(17) 0.0255(18) 0.030(2) -0.0084(16) -0.0060(16) -0.0029(15) C51 0.0225(19) 0.048(2) 0.042(3) -0.015(2) -0.0064(18) -0.0083(18) C52 0.0206(19) 0.054(3) 0.049(3) -0.014(2) 0.0040(19) -0.0095(18) C53 0.036(2) 0.052(3) 0.031(2) -0.0070(19) 0.0054(19) -0.012(2) C54 0.0272(19) 0.040(2) 0.031(2) -0.0079(18) -0.0060(17) -0.0031(17) C55 0.0244(17) 0.0274(19) 0.024(2) -0.0100(16) -0.0030(16) -0.0070(15) C56 0.0298(19) 0.0273(19) 0.030(2) -0.0074(16) -0.0039(17) -0.0097(16) C57 0.0288(19) 0.033(2) 0.039(2) -0.0115(18) -0.0016(18) -0.0108(17) C58 0.041(2) 0.040(2) 0.054(3) -0.020(2) 0.007(2) -0.0090(19) C59 0.054(3) 0.045(2) 0.043(3) -0.022(2) 0.005(2) -0.021(2) C60 0.048(2) 0.036(2) 0.036(2) -0.0064(19) -0.012(2) -0.0173(19) C61 0.0309(19) 0.0258(19) 0.033(2) -0.0049(17) -0.0083(17) -0.0105(16) C62 0.031(2) 0.044(2) 0.062(3) -0.020(2) -0.010(2) -0.0020(19) C63 0.083(4) 0.078(4) 0.063(3) -0.042(3) 0.004(3) -0.025(3) C64 0.032(2) 0.038(2) 0.047(3) -0.0126(19) -0.0162(19) -0.0127(18) C65 0.0300(19) 0.032(2) 0.028(2) -0.0085(17) -0.0062(17) -0.0103(16) C66 0.0254(18) 0.037(2) 0.034(2) -0.0114(18) -0.0048(17) -0.0113(17) C67 0.030(2) 0.049(2) 0.040(2) -0.016(2) -0.0034(19) -0.0134(19) C68 0.047(2) 0.055(3) 0.029(2) -0.013(2) -0.006(2) -0.026(2) C69 0.060(3) 0.034(2) 0.035(2) -0.0002(19) -0.016(2) -0.015(2) C70 0.038(2) 0.032(2) 0.032(2) -0.0058(18) -0.0096(19) -0.0055(18) C71 0.025(2) 0.037(2) 0.073(3) -0.009(2) 0.006(2) -0.0076(18) C72 0.067(3) 0.067(3) 0.033(3) -0.005(2) -0.004(2) -0.031(3) C73 0.052(3) 0.036(2) 0.053(3) -0.004(2) -0.009(2) 0.000(2) C74 0.110(11) 0.058(8) 0.163(18) 0.013(10) -0.007(11) -0.018(7) C75 0.142(16) 0.138(16) 0.110(18) 0.001(11) -0.022(12) -0.024(11) C76 0.079(8) 0.070(8) 0.085(12) -0.027(7) -0.049(8) -0.011(6) C77 0.135(16) 0.146(17) 0.084(15) -0.016(10) 0.016(11) -0.040(10) C78 0.142(13) 0.086(11) 0.102(13) -0.040(9) -0.016(10) -0.023(8) _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 O4 1.831(2) . ? Ge1 C56 1.966(3) . ? Ge1 C65 1.970(4) . ? Ge1 C43 2.052(3) . ? Ge2 O5 1.824(2) . ? Ge2 C34 1.970(3) . ? Ge2 C25 1.975(4) . ? Ge2 C12 2.055(3) . ? O1 C1 1.483(4) . ? O1 O2 1.489(3) . ? O2 C8 1.493(4) . ? O3 C6 1.358(4) . ? O3 C11 1.432(4) . ? O4 C1 1.373(4) . ? O5 C8 1.362(4) . ? C1 C2 1.498(5) . ? C1 C10 1.542(4) . ? C2 C3 1.383(5) . ? C2 C7 1.391(5) . ? C3 C4 1.371(5) . ? C4 C5 1.393(6) . ? C5 C6 1.399(5) . ? C6 C7 1.407(5) . ? C7 C8 1.508(5) . ? C8 C9 1.572(4) . ? C9 C10 1.552(5) . ? C9 C12 1.566(5) . ? C10 C43 1.563(4) . ? C12 C13 1.510(5) . ? C12 C24 1.517(4) . ? C13 C14 1.397(5) . ? C13 C18 1.409(5) . ? C14 C15 1.394(5) . ? C15 C16 1.380(6) . ? C16 C17 1.385(6) . ? C17 C18 1.386(5) . ? C18 C19 1.460(5) . ? C19 C20 1.393(5) . ? C19 C24 1.400(5) . ? C20 C21 1.374(6) . ? C21 C22 1.384(6) . ? C22 C23 1.394(5) . ? C23 C24 1.396(5) . ? C25 C30 1.406(5) . ? C25 C26 1.407(5) . ? C26 C27 1.400(5) . ? C26 C31 1.501(5) . ? C27 C28 1.384(5) . ? C28 C29 1.382(6) . ? C28 C32 1.514(6) . ? C29 C30 1.406(5) . ? C30 C33 1.502(5) . ? C34 C39 1.395(5) . ? C34 C35 1.424(5) . ? C35 C36 1.391(5) . ? C35 C40 1.513(5) . ? C36 C37 1.383(6) . ? C37 C38 1.380(5) . ? C37 C41 1.522(6) . ? C38 C39 1.395(5) . ? C39 C42 1.503(5) . ? C43 C44 1.515(4) . ? C43 C55 1.517(5) . ? C44 C45 1.390(5) . ? C44 C49 1.404(4) . ? C45 C46 1.387(5) . ? C46 C47 1.390(5) . ? C47 C48 1.369(5) . ? C48 C49 1.392(5) . ? C49 C50 1.458(5) . ? C50 C51 1.400(5) . ? C50 C55 1.409(4) . ? C51 C52 1.380(5) . ? C52 C53 1.387(5) . ? C53 C54 1.392(5) . ? C54 C55 1.382(5) . ? C56 C57 1.404(5) . ? C56 C61 1.416(5) . ? C57 C58 1.398(5) . ? C57 C62 1.522(5) . ? C58 C59 1.384(6) . ? C59 C60 1.383(5) . ? C59 C63 1.519(5) . ? C60 C61 1.387(5) . ? C61 C64 1.518(5) . ? C65 C70 1.406(5) . ? C65 C66 1.423(5) . ? C66 C67 1.397(5) . ? C66 C71 1.513(5) . ? C67 C68 1.386(5) . ? C68 C69 1.384(5) . ? C68 C72 1.505(6) . ? C69 C70 1.394(5) . ? C70 C73 1.517(5) . ? C74 C75 1.367(16) . ? C75 C76 1.342(15) . ? C76 C77 1.225(14) . ? C77 C78 1.348(14) . ? 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 O4 Ge1 C56 100.68(12) . . ? O4 Ge1 C65 109.59(13) . . ? C56 Ge1 C65 112.50(14) . . ? O4 Ge1 C43 91.36(11) . . ? C56 Ge1 C43 123.47(14) . . ? C65 Ge1 C43 114.65(14) . . ? O5 Ge2 C34 100.37(12) . . ? O5 Ge2 C25 110.74(13) . . ? C34 Ge2 C25 115.80(14) . . ? O5 Ge2 C12 90.80(11) . . ? C34 Ge2 C12 124.73(14) . . ? C25 Ge2 C12 109.80(13) . . ? C1 O1 O2 109.2(2) . . ? O1 O2 C8 110.5(2) . . ? C6 O3 C11 117.7(3) . . ? C1 O4 Ge1 113.79(18) . . ? C8 O5 Ge2 115.9(2) . . ? O4 C1 O1 105.0(2) . . ? O4 C1 C2 113.3(3) . . ? O1 C1 C2 103.3(2) . . ? O4 C1 C10 111.6(3) . . ? O1 C1 C10 106.0(2) . . ? C2 C1 C10 116.3(3) . . ? C3 C2 C7 122.0(3) . . ? C3 C2 C1 124.8(3) . . ? C7 C2 C1 112.8(3) . . ? C4 C3 C2 118.4(4) . . ? C3 C4 C5 121.2(4) . . ? C4 C5 C6 120.4(4) . . ? O3 C6 C5 123.9(3) . . ? O3 C6 C7 117.8(3) . . ? C5 C6 C7 118.2(4) . . ? C2 C7 C6 119.0(3) . . ? C2 C7 C8 111.2(3) . . ? C6 C7 C8 129.3(3) . . ? O5 C8 O2 103.8(2) . . ? O5 C8 C7 116.1(3) . . ? O2 C8 C7 106.5(3) . . ? O5 C8 C9 111.8(3) . . ? O2 C8 C9 106.6(2) . . ? C7 C8 C9 111.1(3) . . ? C10 C9 C12 115.7(3) . . ? C10 C9 C8 107.2(2) . . ? C12 C9 C8 110.9(3) . . ? C1 C10 C9 107.7(3) . . ? C1 C10 C43 111.3(3) . . ? C9 C10 C43 120.1(3) . . ? C13 C12 C24 101.9(3) . . ? C13 C12 C9 118.2(3) . . ? C24 C12 C9 113.6(3) . . ? C13 C12 Ge2 113.8(2) . . ? C24 C12 Ge2 108.8(2) . . ? C9 C12 Ge2 100.8(2) . . ? C14 C13 C18 119.4(3) . . ? C14 C13 C12 130.4(3) . . ? C18 C13 C12 110.2(3) . . ? C15 C14 C13 118.8(4) . . ? C16 C15 C14 121.0(4) . . ? C15 C16 C17 121.0(4) . . ? C16 C17 C18 118.7(4) . . ? C17 C18 C13 121.1(3) . . ? C17 C18 C19 130.3(3) . . ? C13 C18 C19 108.7(3) . . ? C20 C19 C24 120.9(3) . . ? C20 C19 C18 130.8(3) . . ? C24 C19 C18 108.3(3) . . ? C21 C20 C19 119.0(4) . . ? C20 C21 C22 120.6(3) . . ? C21 C22 C23 121.3(4) . . ? C22 C23 C24 118.5(3) . . ? C23 C24 C19 119.6(3) . . ? C23 C24 C12 129.7(3) . . ? C19 C24 C12 110.6(3) . . ? C30 C25 C26 118.9(3) . . ? C30 C25 Ge2 116.0(3) . . ? C26 C25 Ge2 124.5(3) . . ? C27 C26 C25 119.0(4) . . ? C27 C26 C31 116.9(4) . . ? C25 C26 C31 124.1(3) . . ? C28 C27 C26 122.6(4) . . ? C29 C28 C27 117.8(4) . . ? C29 C28 C32 121.5(4) . . ? C27 C28 C32 120.6(4) . . ? C28 C29 C30 121.6(4) . . ? C29 C30 C25 119.8(4) . . ? C29 C30 C33 117.9(4) . . ? C25 C30 C33 122.2(3) . . ? C39 C34 C35 118.6(3) . . ? C39 C34 Ge2 126.6(2) . . ? C35 C34 Ge2 114.5(3) . . ? C36 C35 C34 118.7(4) . . ? C36 C35 C40 118.2(3) . . ? C34 C35 C40 123.1(3) . . ? C37 C36 C35 122.4(4) . . ? C38 C37 C36 117.7(4) . . ? C38 C37 C41 120.3(4) . . ? C36 C37 C41 122.0(4) . . ? C37 C38 C39 122.1(4) . . ? C34 C39 C38 119.6(3) . . ? C34 C39 C42 124.2(3) . . ? C38 C39 C42 116.1(3) . . ? C44 C43 C55 102.7(2) . . ? C44 C43 C10 113.7(3) . . ? C55 C43 C10 116.5(3) . . ? C44 C43 Ge1 111.2(2) . . ? C55 C43 Ge1 116.0(2) . . ? C10 C43 Ge1 97.27(19) . . ? C45 C44 C49 119.9(3) . . ? C45 C44 C43 130.1(3) . . ? C49 C44 C43 110.0(3) . . ? C46 C45 C44 118.7(3) . . ? C45 C46 C47 121.1(4) . . ? C48 C47 C46 120.6(3) . . ? C47 C48 C49 119.2(3) . . ? C48 C49 C44 120.5(3) . . ? C48 C49 C50 130.8(3) . . ? C44 C49 C50 108.7(3) . . ? C51 C50 C55 120.8(3) . . ? C51 C50 C49 130.0(3) . . ? C55 C50 C49 109.1(3) . . ? C52 C51 C50 119.1(3) . . ? C51 C52 C53 120.4(3) . . ? C52 C53 C54 120.5(4) . . ? C55 C54 C53 120.2(3) . . ? C54 C55 C50 118.9(3) . . ? C54 C55 C43 131.5(3) . . ? C50 C55 C43 109.5(3) . . ? C57 C56 C61 118.7(3) . . ? C57 C56 Ge1 125.4(3) . . ? C61 C56 Ge1 115.9(2) . . ? C58 C57 C56 119.3(3) . . ? C58 C57 C62 116.9(3) . . ? C56 C57 C62 123.8(3) . . ? C59 C58 C57 122.2(4) . . ? C60 C59 C58 117.8(4) . . ? C60 C59 C63 120.9(4) . . ? C58 C59 C63 121.3(4) . . ? C59 C60 C61 122.3(4) . . ? C60 C61 C56 119.4(3) . . ? C60 C61 C64 117.8(3) . . ? C56 C61 C64 122.7(3) . . ? C70 C65 C66 117.9(3) . . ? C70 C65 Ge1 118.3(3) . . ? C66 C65 Ge1 123.8(3) . . ? C67 C66 C65 119.2(3) . . ? C67 C66 C71 116.3(3) . . ? C65 C66 C71 124.5(3) . . ? C68 C67 C66 123.1(4) . . ? C69 C68 C67 117.0(4) . . ? C69 C68 C72 122.2(4) . . ? C67 C68 C72 120.8(4) . . ? C68 C69 C70 122.5(4) . . ? C69 C70 C65 120.4(3) . . ? C69 C70 C73 118.8(3) . . ? C65 C70 C73 120.8(4) . . ? C76 C75 C74 115.3(18) . . ? C77 C76 C75 122.5(18) . . ? C76 C77 C78 127(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.630 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.070 _vrf_PLAT761_9 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen atoms have been refined by the use of a riding model. ; _vrf_PLAT762_9 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen atoms have been refined by the use of a riding model. ; # Attachment '10 new Dalton.cif' data_10 _database_code_depnum_ccdc_archive 'CCDC 751862' #TrackingRef '10 new Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H100 Cl2 Ge2 O2' _chemical_formula_weight 1417.77 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' 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' Cl Cl 0.1484 0.1585 '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 17.3042(17) _cell_length_b 25.114(2) _cell_length_c 19.401(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.691(2) _cell_angle_gamma 90.00 _cell_volume 7778.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2040 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 19.02 _exptl_crystal_description plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9165 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56978 _diffrn_reflns_av_R_equivalents 0.2136 _diffrn_reflns_av_sigmaI/netI 0.2010 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 14120 _reflns_number_gt 6935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14120 _refine_ls_number_parameters 965 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.1778 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.16552(4) 0.22300(2) 0.28732(3) 0.02492(18) Uani 1 1 d . . . Ge2 Ge 0.63124(4) 0.16361(2) 0.34594(3) 0.02455(17) Uani 1 1 d . . . O1 O 0.2219(2) 0.21886(15) 0.2266(2) 0.0289(9) Uani 1 1 d . . . O2 O 0.5645(2) 0.22156(14) 0.3086(2) 0.0305(10) Uani 1 1 d . . . C1 C 0.3074(4) 0.2195(2) 0.2500(3) 0.0246(13) Uani 1 1 d . . . C2 C 0.3415(4) 0.2440(2) 0.2042(3) 0.0287(15) Uani 1 1 d . . . H2 H 0.3060 0.2603 0.1589 0.034 Uiso 1 1 calc R . . C3 C 0.4283(4) 0.2445(2) 0.2249(3) 0.0304(15) Uani 1 1 d . . . H3 H 0.4522 0.2613 0.1940 0.036 Uiso 1 1 calc R . . C4 C 0.4790(4) 0.2204(2) 0.2907(3) 0.0244(13) Uani 1 1 d . . . C5 C 0.4468(4) 0.1961(2) 0.3382(3) 0.0215(13) Uani 1 1 d . . . C6 C 0.5063(3) 0.1682(2) 0.4072(3) 0.0215(13) Uani 1 1 d . . . H6 H 0.5481 0.1951 0.4377 0.026 Uiso 1 1 calc R . . C7 C 0.4635(4) 0.1466(2) 0.4549(3) 0.0219(13) Uani 1 1 d . . . H7 H 0.4975 0.1311 0.5014 0.026 Uiso 1 1 calc R . . C8 C 0.3816(4) 0.1476(2) 0.4370(3) 0.0273(14) Uani 1 1 d . . . H8 H 0.3609 0.1321 0.4712 0.033 Uiso 1 1 calc R . . C9 C 0.3198(3) 0.1711(2) 0.3677(3) 0.0222(13) Uani 1 1 d . . . H9 H 0.2829 0.1413 0.3389 0.027 Uiso 1 1 calc R . . C10 C 0.3590(4) 0.1953(2) 0.3179(3) 0.0228(13) Uani 1 1 d . . . C11 C 0.2615(3) 0.2123(2) 0.3870(3) 0.0248(14) Uani 1 1 d . . . C12 C 0.3085(4) 0.2614(2) 0.4286(3) 0.0248(14) Uani 1 1 d . . . C13 C 0.3551(3) 0.2987(2) 0.4078(3) 0.0249(14) Uani 1 1 d . . . H13 H 0.3604 0.2955 0.3611 0.030 Uiso 1 1 calc R . . C14 C 0.3943(4) 0.3410(2) 0.4561(3) 0.0275(14) Uani 1 1 d . . . C15 C 0.3831(4) 0.3451(2) 0.5235(3) 0.0293(15) Uani 1 1 d . . . H15 H 0.4078 0.3743 0.5557 0.035 Uiso 1 1 calc R . . C16 C 0.3377(4) 0.3084(2) 0.5451(3) 0.0311(15) Uani 1 1 d . . . H16 H 0.3318 0.3119 0.5915 0.037 Uiso 1 1 calc R . . C17 C 0.3010(4) 0.2665(2) 0.4976(3) 0.0278(14) Uani 1 1 d . . . C18 C 0.2511(4) 0.2213(2) 0.5061(3) 0.0288(14) Uani 1 1 d . . . C19 C 0.2287(4) 0.2070(2) 0.5650(3) 0.0344(16) Uani 1 1 d . . . H19 H 0.2424 0.2296 0.6073 0.041 Uiso 1 1 calc R . . C20 C 0.1865(4) 0.1598(2) 0.5620(3) 0.0360(16) Uani 1 1 d . . . H20 H 0.1701 0.1507 0.6020 0.043 Uiso 1 1 calc R . . C21 C 0.1671(4) 0.1247(2) 0.5002(3) 0.0301(15) Uani 1 1 d . A . C22 C 0.1887(4) 0.1399(2) 0.4418(3) 0.0273(14) Uani 1 1 d . . . H22 H 0.1762 0.1171 0.3998 0.033 Uiso 1 1 calc R . . C23 C 0.2290(4) 0.1885(2) 0.4435(3) 0.0270(14) Uani 1 1 d . . . C24 C 0.4487(4) 0.3820(2) 0.4371(3) 0.0291(15) Uani 1 1 d . . . C25 C 0.4622(4) 0.3685(2) 0.3657(3) 0.0358(16) Uani 1 1 d . . . H25A H 0.4915 0.3343 0.3720 0.054 Uiso 1 1 calc R . . H25B H 0.4959 0.3964 0.3555 0.054 Uiso 1 1 calc R . . H25C H 0.4078 0.3660 0.3237 0.054 Uiso 1 1 calc R . . C26 C 0.4049(5) 0.4366(2) 0.4270(4) 0.054(2) Uani 1 1 d . . . H26A H 0.3496 0.4345 0.3863 0.081 Uiso 1 1 calc R . . H26B H 0.4388 0.4635 0.4150 0.081 Uiso 1 1 calc R . . H26C H 0.3985 0.4465 0.4734 0.081 Uiso 1 1 calc R . . C27 C 0.5348(4) 0.3859(3) 0.5017(3) 0.0488(19) Uani 1 1 d . . . H27A H 0.5280 0.4002 0.5461 0.073 Uiso 1 1 calc R . . H27B H 0.5711 0.4096 0.4874 0.073 Uiso 1 1 calc R . . H27C H 0.5602 0.3504 0.5130 0.073 Uiso 1 1 calc R . . C28 C 0.1256(4) 0.0711(2) 0.5016(3) 0.0347(15) Uani 1 1 d DU . . C29 C 0.0392(6) 0.0820(4) 0.5018(8) 0.058(4) Uani 0.642(10) 1 d PDU A 1 H29A H 0.0450 0.1016 0.5473 0.086 Uiso 0.642(10) 1 calc PR A 1 H29B H 0.0106 0.0481 0.5006 0.086 Uiso 0.642(10) 1 calc PR A 1 H29C H 0.0065 0.1032 0.4579 0.086 Uiso 0.642(10) 1 calc PR A 1 C30 C 0.1208(8) 0.0355(4) 0.4367(6) 0.050(3) Uani 0.642(10) 1 d PDU A 1 H30A H 0.0883 0.0533 0.3894 0.075 Uiso 0.642(10) 1 calc PR A 1 H30B H 0.0935 0.0018 0.4396 0.075 Uiso 0.642(10) 1 calc PR A 1 H30C H 0.1775 0.0283 0.4392 0.075 Uiso 0.642(10) 1 calc PR A 1 C31 C 0.1782(7) 0.0410(4) 0.5760(6) 0.058(4) Uani 0.642(10) 1 d PDU A 1 H31A H 0.2349 0.0346 0.5780 0.086 Uiso 0.642(10) 1 calc PR A 1 H31B H 0.1513 0.0069 0.5773 0.086 Uiso 0.642(10) 1 calc PR A 1 H31C H 0.1811 0.0627 0.6189 0.086 Uiso 0.642(10) 1 calc PR A 1 C29' C 0.0482(10) 0.0644(7) 0.4248(8) 0.051(6) Uani 0.358(10) 1 d PDU A 2 H29D H 0.0073 0.0926 0.4198 0.077 Uiso 0.358(10) 1 calc PR A 2 H29E H 0.0221 0.0296 0.4236 0.077 Uiso 0.358(10) 1 calc PR A 2 H29F H 0.0674 0.0668 0.3835 0.077 Uiso 0.358(10) 1 calc PR A 2 C30' C 0.1875(10) 0.0276(6) 0.5034(12) 0.049(6) Uani 0.358(10) 1 d PDU A 2 H30D H 0.2172 0.0378 0.4713 0.074 Uiso 0.358(10) 1 calc PR A 2 H30E H 0.1573 -0.0059 0.4852 0.074 Uiso 0.358(10) 1 calc PR A 2 H30F H 0.2280 0.0227 0.5547 0.074 Uiso 0.358(10) 1 calc PR A 2 C31' C 0.0899(13) 0.0646(8) 0.5619(10) 0.051(6) Uani 0.358(10) 1 d PDU A 2 H31D H 0.1341 0.0521 0.6082 0.077 Uiso 0.358(10) 1 calc PR A 2 H31E H 0.0442 0.0386 0.5453 0.077 Uiso 0.358(10) 1 calc PR A 2 H31F H 0.0685 0.0990 0.5709 0.077 Uiso 0.358(10) 1 calc PR A 2 C32 C 0.5565(3) 0.1229(2) 0.3843(3) 0.0204(13) Uani 1 1 d . . . C33 C 0.4971(3) 0.0838(2) 0.3296(3) 0.0205(13) Uani 1 1 d . . . C34 C 0.4479(3) 0.0890(2) 0.2542(3) 0.0248(14) Uani 1 1 d . . . H34 H 0.4451 0.1225 0.2306 0.030 Uiso 1 1 calc R . . C35 C 0.4029(3) 0.0465(2) 0.2127(3) 0.0259(14) Uani 1 1 d . . . C36 C 0.4055(4) -0.0015(2) 0.2504(3) 0.0315(15) Uani 1 1 d . . . H36 H 0.3723 -0.0305 0.2234 0.038 Uiso 1 1 calc R . . C37 C 0.4543(3) -0.0083(2) 0.3252(3) 0.0260(14) Uani 1 1 d . . . H37 H 0.4551 -0.0415 0.3489 0.031 Uiso 1 1 calc R . . C38 C 0.5024(3) 0.0339(2) 0.3655(3) 0.0226(13) Uani 1 1 d . . . C39 C 0.5678(3) 0.0368(2) 0.4403(3) 0.0220(13) Uani 1 1 d . . . C40 C 0.5980(4) -0.0005(2) 0.4975(3) 0.0255(14) Uani 1 1 d . . . H40 H 0.5756 -0.0355 0.4906 0.031 Uiso 1 1 calc R . . C41 C 0.6610(3) 0.0138(2) 0.5645(3) 0.0260(14) Uani 1 1 d . . . H41 H 0.6816 -0.0119 0.6033 0.031 Uiso 1 1 calc R . . C42 C 0.6954(4) 0.0654(2) 0.5769(3) 0.0260(14) Uani 1 1 d . . . C43 C 0.6648(3) 0.1021(2) 0.5192(3) 0.0241(14) Uani 1 1 d . . . H43 H 0.6869 0.1372 0.5264 0.029 Uiso 1 1 calc R . . C44 C 0.6031(3) 0.0885(2) 0.4520(3) 0.0218(13) Uani 1 1 d . . . C45 C 0.3585(4) 0.0501(2) 0.1275(3) 0.0351(16) Uani 1 1 d . . . C46 C 0.3238(6) 0.1057(3) 0.1033(4) 0.082(3) Uani 1 1 d . . . H46A H 0.2831 0.1143 0.1254 0.124 Uiso 1 1 calc R . . H46B H 0.2962 0.1070 0.0487 0.124 Uiso 1 1 calc R . . H46C H 0.3697 0.1316 0.1202 0.124 Uiso 1 1 calc R . . C47 C 0.4221(5) 0.0364(4) 0.0936(4) 0.089(3) Uani 1 1 d . . . H47A H 0.4699 0.0608 0.1132 0.133 Uiso 1 1 calc R . . H47B H 0.3959 0.0399 0.0391 0.133 Uiso 1 1 calc R . . H47C H 0.4415 -0.0003 0.1067 0.133 Uiso 1 1 calc R . . C48 C 0.2847(4) 0.0116(3) 0.0967(4) 0.063(2) Uani 1 1 d . . . H48A H 0.3052 -0.0251 0.1071 0.094 Uiso 1 1 calc R . . H48B H 0.2565 0.0167 0.0427 0.094 Uiso 1 1 calc R . . H48C H 0.2452 0.0186 0.1207 0.094 Uiso 1 1 calc R . . C49 C 0.7635(4) 0.0822(2) 0.6517(3) 0.0308(15) Uani 1 1 d . . . C50 C 0.7967(4) 0.0345(3) 0.7059(3) 0.0486(19) Uani 1 1 d . . . H50A H 0.7526 0.0219 0.7218 0.073 Uiso 1 1 calc R . . H50B H 0.8454 0.0459 0.7497 0.073 Uiso 1 1 calc R . . H50C H 0.8132 0.0057 0.6804 0.073 Uiso 1 1 calc R . . C51 C 0.7251(4) 0.1229(2) 0.6884(3) 0.0402(17) Uani 1 1 d . . . H51A H 0.7039 0.1534 0.6550 0.060 Uiso 1 1 calc R . . H51B H 0.7680 0.1349 0.7358 0.060 Uiso 1 1 calc R . . H51C H 0.6789 0.1063 0.6979 0.060 Uiso 1 1 calc R . . C52 C 0.8379(4) 0.1076(2) 0.6391(3) 0.0405(17) Uani 1 1 d . . . H52A H 0.8620 0.0817 0.6153 0.061 Uiso 1 1 calc R . . H52B H 0.8806 0.1185 0.6872 0.061 Uiso 1 1 calc R . . H52C H 0.8185 0.1388 0.6067 0.061 Uiso 1 1 calc R . . C53 C 0.0946(3) 0.2861(2) 0.2485(3) 0.0261(14) Uani 1 1 d . . . C54 C 0.0421(4) 0.2844(2) 0.1720(3) 0.0286(14) Uani 1 1 d . . . C55 C -0.0223(4) 0.3221(2) 0.1443(3) 0.0326(15) Uani 1 1 d . . . H55 H -0.0582 0.3205 0.0929 0.039 Uiso 1 1 calc R . . C56 C -0.0360(4) 0.3613(2) 0.1879(4) 0.0329(15) Uani 1 1 d . . . C57 C 0.0200(4) 0.3642(2) 0.2614(4) 0.0415(17) Uani 1 1 d . . . H57 H 0.0149 0.3929 0.2913 0.050 Uiso 1 1 calc R . . C58 C 0.0833(4) 0.3272(2) 0.2934(3) 0.0333(15) Uani 1 1 d . . . C59 C 0.0513(4) 0.2456(2) 0.1169(3) 0.0331(15) Uani 1 1 d . . . H59A H 0.1032 0.2530 0.1096 0.050 Uiso 1 1 calc R . . H59B H 0.0034 0.2490 0.0691 0.050 Uiso 1 1 calc R . . H59C H 0.0532 0.2093 0.1360 0.050 Uiso 1 1 calc R . . C60 C -0.1087(4) 0.3998(2) 0.1569(4) 0.0456(18) Uani 1 1 d . . . H60A H -0.1207 0.4065 0.1040 0.068 Uiso 1 1 calc R . . H60B H -0.0942 0.4333 0.1847 0.068 Uiso 1 1 calc R . . H60C H -0.1583 0.3844 0.1620 0.068 Uiso 1 1 calc R . . C61 C 0.1382(4) 0.3326(3) 0.3754(3) 0.0477(19) Uani 1 1 d . . . H61A H 0.1958 0.3404 0.3809 0.071 Uiso 1 1 calc R . . H61B H 0.1371 0.2993 0.4012 0.071 Uiso 1 1 calc R . . H61C H 0.1172 0.3617 0.3971 0.071 Uiso 1 1 calc R . . C62 C 0.0877(4) 0.1618(2) 0.2646(3) 0.0318(15) Uani 1 1 d . . . C63 C 0.0947(4) 0.1158(2) 0.2256(3) 0.0396(17) Uani 1 1 d . . . C64 C 0.0327(5) 0.0772(3) 0.2076(4) 0.055(2) Uani 1 1 d . . . H64 H 0.0385 0.0463 0.1818 0.066 Uiso 1 1 calc R . . C65 C -0.0361(6) 0.0814(3) 0.2251(5) 0.073(3) Uani 1 1 d . . . C66 C -0.0439(5) 0.1261(3) 0.2634(5) 0.073(3) Uani 1 1 d . . . H66 H -0.0919 0.1297 0.2754 0.087 Uiso 1 1 calc R . . C67 C 0.0174(4) 0.1662(3) 0.2851(4) 0.0455(18) Uani 1 1 d . . . C68 C 0.1644(4) 0.1045(3) 0.2001(4) 0.051(2) Uani 1 1 d . . . H68A H 0.2167 0.0994 0.2438 0.076 Uiso 1 1 calc R . . H68B H 0.1707 0.1346 0.1705 0.076 Uiso 1 1 calc R . . H68C H 0.1516 0.0722 0.1695 0.076 Uiso 1 1 calc R . . C69 C -0.1049(6) 0.0377(4) 0.2058(7) 0.131(5) Uani 1 1 d . . . H69A H -0.1004 0.0141 0.1673 0.197 Uiso 1 1 calc R . . H69B H -0.1602 0.0546 0.1870 0.197 Uiso 1 1 calc R . . H69C H -0.0974 0.0171 0.2507 0.197 Uiso 1 1 calc R . . C70 C 0.0065(5) 0.2124(3) 0.3309(5) 0.065(2) Uani 1 1 d . . . H70A H -0.0184 0.2427 0.2979 0.098 Uiso 1 1 calc R . . H70B H 0.0612 0.2227 0.3683 0.098 Uiso 1 1 calc R . . H70C H -0.0305 0.2016 0.3560 0.098 Uiso 1 1 calc R . . C71 C 0.7353(4) 0.1944(2) 0.4207(3) 0.0263(14) Uani 1 1 d . . . C72 C 0.7416(4) 0.2457(3) 0.4526(4) 0.0408(17) Uani 1 1 d . . . C73 C 0.8197(5) 0.2669(3) 0.4925(4) 0.055(2) Uani 1 1 d . . . H73 H 0.8229 0.3016 0.5128 0.066 Uiso 1 1 calc R . . C74 C 0.8934(4) 0.2402(3) 0.5045(4) 0.051(2) Uani 1 1 d . . . C75 C 0.8867(4) 0.1881(3) 0.4778(4) 0.0484(19) Uani 1 1 d . . . H75 H 0.9361 0.1678 0.4876 0.058 Uiso 1 1 calc R . . C76 C 0.8089(4) 0.1653(3) 0.4371(3) 0.0373(16) Uani 1 1 d . . . C77 C 0.6677(5) 0.2799(3) 0.4464(6) 0.088(3) Uani 1 1 d . . . H77A H 0.6463 0.2688 0.4841 0.133 Uiso 1 1 calc R . . H77B H 0.6236 0.2757 0.3965 0.133 Uiso 1 1 calc R . . H77C H 0.6851 0.3172 0.4544 0.133 Uiso 1 1 calc R . . C78 C 0.9782(5) 0.2651(3) 0.5451(4) 0.075(3) Uani 1 1 d . . . H78A H 0.9720 0.2973 0.5710 0.112 Uiso 1 1 calc R . . H78B H 1.0030 0.2744 0.5090 0.112 Uiso 1 1 calc R . . H78C H 1.0147 0.2398 0.5815 0.112 Uiso 1 1 calc R . . C79 C 0.8092(4) 0.1075(2) 0.4131(4) 0.056(2) Uani 1 1 d . . . H79A H 0.7649 0.0879 0.4219 0.084 Uiso 1 1 calc R . . H79B H 0.8636 0.0914 0.4422 0.084 Uiso 1 1 calc R . . H79C H 0.7991 0.1062 0.3599 0.084 Uiso 1 1 calc R . . C80 C 0.6509(4) 0.1367(2) 0.2586(3) 0.0275(14) Uani 1 1 d . . . C81 C 0.6489(3) 0.0827(2) 0.2399(3) 0.0272(14) Uani 1 1 d . . . C82 C 0.6565(4) 0.0689(3) 0.1728(3) 0.0388(17) Uani 1 1 d . . . H82 H 0.6546 0.0323 0.1599 0.047 Uiso 1 1 calc R . . C83 C 0.6665(4) 0.1054(3) 0.1253(4) 0.0430(18) Uani 1 1 d . . . C84 C 0.6735(4) 0.1575(2) 0.1463(3) 0.0385(17) Uani 1 1 d . . . H84 H 0.6834 0.1832 0.1147 0.046 Uiso 1 1 calc R . . C85 C 0.6668(4) 0.1749(2) 0.2122(3) 0.0346(16) Uani 1 1 d . . . C86 C 0.6408(4) 0.0373(2) 0.2878(3) 0.0349(16) Uani 1 1 d . . . H86A H 0.6484 0.0508 0.3373 0.052 Uiso 1 1 calc R . . H86B H 0.6837 0.0104 0.2927 0.052 Uiso 1 1 calc R . . H86C H 0.5852 0.0212 0.2643 0.052 Uiso 1 1 calc R . . C87 C 0.6720(5) 0.0879(3) 0.0518(4) 0.063(2) Uani 1 1 d . . . H87A H 0.6684 0.0490 0.0479 0.095 Uiso 1 1 calc R . . H87B H 0.7254 0.0997 0.0506 0.095 Uiso 1 1 calc R . . H87C H 0.6257 0.1037 0.0098 0.095 Uiso 1 1 calc R . . C88 C 0.6815(4) 0.2334(2) 0.2314(4) 0.0463(19) Uani 1 1 d . . . H88A H 0.6972 0.2514 0.1939 0.069 Uiso 1 1 calc R . . H88B H 0.7267 0.2373 0.2808 0.069 Uiso 1 1 calc R . . H88C H 0.6301 0.2494 0.2321 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.4151(7) 0.0975(5) 0.9028(6) 0.214(5) Uani 0.454(3) 1 d PDU B 1 C89 C 0.3416(15) 0.1400(14) 0.8471(14) 0.216(11) Uani 0.454(3) 1 d PDU B 1 H89A H 0.3700 0.1600 0.8195 0.259 Uiso 0.454(3) 1 calc PR B 1 H89B H 0.3327 0.1659 0.8817 0.259 Uiso 0.454(3) 1 calc PR B 1 Cl2 Cl 0.2443(13) 0.1270(5) 0.7826(6) 0.279(9) Uani 0.454(3) 1 d PDU B 1 Cl1' Cl 0.0901(6) 0.1212(3) 0.7304(5) 0.112(4) Uani 0.336(6) 1 d PDU C 2 C89' C 0.170(2) 0.1315(15) 0.8086(12) 0.155(13) Uani 0.336(6) 1 d PDU C 2 H89C H 0.1617 0.1669 0.8270 0.186 Uiso 0.336(6) 1 calc PR C 2 H89D H 0.2200 0.1344 0.7959 0.186 Uiso 0.336(6) 1 calc PR C 2 Cl2' Cl 0.1952(9) 0.0896(4) 0.8814(5) 0.140(5) Uani 0.336(6) 1 d PDU C 2 Cl1" Cl 0.3492(11) 0.1685(7) 0.8134(13) 0.168(10) Uani 0.210(6) 1 d PDU D 3 C89" C 0.302(6) 0.111(2) 0.817(3) 0.199(16) Uani 0.210(6) 1 d PDU D 3 H89E H 0.2502 0.1117 0.7705 0.238 Uiso 0.210(6) 1 calc PR D 3 H89F H 0.3381 0.0838 0.8083 0.238 Uiso 0.210(6) 1 calc PR D 3 Cl2" Cl 0.271(2) 0.0838(11) 0.8794(18) 0.259(14) Uani 0.210(6) 1 d PDU D 3 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 0.0277(4) 0.0216(3) 0.0239(3) -0.0010(3) 0.0082(3) 0.0024(3) Ge2 0.0277(4) 0.0194(3) 0.0277(3) 0.0012(3) 0.0119(3) -0.0009(3) O1 0.023(2) 0.038(2) 0.026(2) -0.0014(19) 0.0102(18) 0.006(2) O2 0.032(2) 0.018(2) 0.047(3) 0.0127(19) 0.021(2) 0.003(2) C1 0.033(4) 0.019(3) 0.022(3) -0.004(3) 0.012(3) 0.000(3) C2 0.039(4) 0.026(3) 0.023(3) 0.007(3) 0.014(3) 0.006(3) C3 0.041(4) 0.023(3) 0.032(4) 0.002(3) 0.019(3) 0.000(3) C4 0.028(3) 0.014(3) 0.032(3) -0.002(3) 0.013(3) -0.001(3) C5 0.033(4) 0.013(3) 0.022(3) -0.002(2) 0.013(3) -0.004(3) C6 0.025(3) 0.012(3) 0.029(3) -0.003(3) 0.012(3) -0.003(3) C7 0.027(3) 0.022(3) 0.016(3) 0.005(2) 0.008(3) 0.012(3) C8 0.038(4) 0.023(3) 0.023(3) 0.004(3) 0.015(3) 0.002(3) C9 0.025(3) 0.021(3) 0.021(3) -0.002(3) 0.010(3) 0.005(3) C10 0.032(4) 0.016(3) 0.023(3) -0.001(2) 0.015(3) 0.000(3) C11 0.028(3) 0.023(3) 0.020(3) 0.002(2) 0.006(3) 0.000(3) C12 0.028(3) 0.022(3) 0.018(3) -0.003(2) 0.003(3) 0.001(3) C13 0.032(3) 0.019(3) 0.024(3) -0.001(3) 0.011(3) 0.004(3) C14 0.031(3) 0.021(3) 0.024(3) 0.004(3) 0.004(3) 0.008(3) C15 0.036(4) 0.020(3) 0.026(3) -0.010(3) 0.006(3) -0.004(3) C16 0.040(4) 0.032(4) 0.022(3) -0.001(3) 0.013(3) 0.009(3) C17 0.032(3) 0.025(3) 0.023(3) 0.001(3) 0.006(3) 0.008(3) C18 0.030(3) 0.029(3) 0.025(3) 0.003(3) 0.009(3) 0.002(3) C19 0.049(4) 0.033(4) 0.027(3) -0.003(3) 0.021(3) -0.001(3) C20 0.043(4) 0.037(4) 0.036(4) 0.006(3) 0.025(3) 0.000(3) C21 0.029(4) 0.029(4) 0.036(4) -0.001(3) 0.017(3) 0.005(3) C22 0.030(3) 0.025(3) 0.027(3) 0.000(3) 0.011(3) 0.004(3) C23 0.031(4) 0.030(3) 0.023(3) -0.003(3) 0.015(3) 0.003(3) C24 0.040(4) 0.015(3) 0.034(4) 0.000(3) 0.016(3) 0.000(3) C25 0.042(4) 0.030(4) 0.036(4) 0.002(3) 0.016(3) 0.000(3) C26 0.068(5) 0.037(4) 0.062(5) 0.008(4) 0.031(4) 0.005(4) C27 0.045(4) 0.058(5) 0.035(4) 0.001(3) 0.006(3) -0.009(4) C28 0.033(4) 0.028(4) 0.045(4) 0.011(3) 0.017(3) 0.002(3) C29 0.043(6) 0.035(7) 0.102(12) 0.012(7) 0.036(7) 0.013(5) C30 0.067(9) 0.032(6) 0.055(7) 0.001(5) 0.029(7) -0.010(6) C31 0.066(8) 0.036(7) 0.057(7) 0.018(5) 0.009(6) 0.005(6) C29' 0.050(11) 0.034(12) 0.061(9) 0.020(10) 0.011(8) -0.009(9) C30' 0.054(11) 0.013(9) 0.081(17) 0.010(10) 0.028(10) -0.005(7) C31' 0.064(15) 0.036(12) 0.059(11) 0.008(10) 0.030(11) -0.013(11) C32 0.021(3) 0.021(3) 0.023(3) -0.001(2) 0.013(3) -0.003(3) C33 0.023(3) 0.021(3) 0.023(3) 0.000(2) 0.014(3) 0.000(3) C34 0.030(3) 0.022(3) 0.021(3) 0.000(3) 0.009(3) -0.002(3) C35 0.025(3) 0.024(3) 0.030(3) 0.005(3) 0.012(3) 0.001(3) C36 0.037(4) 0.024(3) 0.029(4) -0.007(3) 0.007(3) -0.005(3) C37 0.031(3) 0.011(3) 0.037(4) 0.005(3) 0.014(3) 0.001(3) C38 0.026(3) 0.024(3) 0.021(3) 0.005(3) 0.012(3) 0.004(3) C39 0.022(3) 0.021(3) 0.023(3) 0.004(3) 0.009(3) 0.007(3) C40 0.039(4) 0.018(3) 0.025(3) 0.004(3) 0.019(3) -0.001(3) C41 0.032(4) 0.024(3) 0.025(3) 0.007(3) 0.013(3) 0.007(3) C42 0.028(3) 0.027(3) 0.025(3) 0.001(3) 0.013(3) 0.006(3) C43 0.028(3) 0.017(3) 0.032(3) 0.004(3) 0.017(3) 0.003(3) C44 0.028(3) 0.022(3) 0.020(3) 0.002(3) 0.015(3) -0.001(3) C45 0.044(4) 0.028(4) 0.027(3) -0.004(3) 0.009(3) -0.002(3) C46 0.132(8) 0.041(5) 0.036(4) 0.001(4) -0.010(5) 0.005(5) C47 0.076(6) 0.155(9) 0.029(4) -0.010(5) 0.013(5) 0.003(6) C48 0.061(5) 0.059(5) 0.048(5) -0.004(4) -0.002(4) -0.010(4) C49 0.029(4) 0.034(4) 0.024(3) 0.005(3) 0.004(3) 0.007(3) C50 0.063(5) 0.049(4) 0.029(4) -0.001(3) 0.011(4) 0.015(4) C51 0.046(4) 0.039(4) 0.034(4) -0.007(3) 0.013(3) -0.005(3) C52 0.036(4) 0.045(4) 0.033(4) -0.002(3) 0.006(3) -0.002(3) C53 0.021(3) 0.023(3) 0.036(4) 0.002(3) 0.013(3) 0.000(3) C54 0.025(3) 0.030(4) 0.027(3) -0.001(3) 0.006(3) -0.001(3) C55 0.035(4) 0.036(4) 0.026(3) 0.004(3) 0.010(3) -0.002(3) C56 0.028(4) 0.023(3) 0.044(4) 0.009(3) 0.009(3) 0.002(3) C57 0.045(4) 0.030(4) 0.045(4) -0.001(3) 0.013(4) 0.015(3) C58 0.040(4) 0.028(4) 0.030(3) -0.005(3) 0.012(3) 0.003(3) C59 0.031(4) 0.037(4) 0.024(3) -0.002(3) 0.004(3) 0.007(3) C60 0.043(4) 0.033(4) 0.057(5) 0.006(3) 0.015(4) 0.008(3) C61 0.054(4) 0.042(4) 0.034(4) -0.015(3) 0.002(3) 0.026(4) C62 0.030(4) 0.022(3) 0.036(4) 0.004(3) 0.004(3) -0.005(3) C63 0.041(4) 0.024(4) 0.035(4) 0.006(3) -0.006(3) 0.003(3) C64 0.063(5) 0.030(4) 0.050(5) -0.002(3) -0.003(4) 0.006(4) C65 0.060(6) 0.049(5) 0.090(7) 0.004(5) 0.005(5) -0.025(5) C66 0.040(5) 0.056(5) 0.125(8) 0.021(6) 0.036(5) -0.004(4) C67 0.036(4) 0.040(4) 0.058(5) 0.013(4) 0.015(4) 0.004(4) C68 0.059(5) 0.033(4) 0.048(4) -0.012(3) 0.007(4) 0.013(4) C69 0.096(8) 0.068(7) 0.208(13) -0.003(7) 0.034(8) -0.053(6) C70 0.064(5) 0.051(5) 0.109(7) 0.013(5) 0.065(5) 0.010(4) C71 0.025(3) 0.033(4) 0.020(3) -0.002(3) 0.008(3) -0.005(3) C72 0.038(4) 0.046(4) 0.042(4) -0.017(3) 0.020(4) -0.005(4) C73 0.050(5) 0.056(5) 0.061(5) -0.023(4) 0.025(4) -0.020(4) C74 0.036(4) 0.060(5) 0.053(5) -0.012(4) 0.013(4) -0.017(4) C75 0.039(4) 0.056(5) 0.047(4) -0.001(4) 0.013(4) -0.005(4) C76 0.035(4) 0.041(4) 0.035(4) 0.004(3) 0.012(3) -0.006(4) C77 0.054(5) 0.068(6) 0.146(9) -0.068(6) 0.042(6) -0.021(5) C78 0.049(5) 0.101(7) 0.064(6) -0.027(5) 0.011(4) -0.035(5) C79 0.039(4) 0.035(4) 0.083(6) -0.003(4) 0.011(4) 0.002(4) C80 0.034(4) 0.022(3) 0.028(3) 0.001(3) 0.013(3) -0.004(3) C81 0.023(3) 0.029(4) 0.029(3) 0.006(3) 0.009(3) 0.001(3) C82 0.047(4) 0.037(4) 0.037(4) -0.012(3) 0.021(4) -0.007(3) C83 0.061(5) 0.040(4) 0.034(4) -0.006(3) 0.026(4) -0.005(4) C84 0.055(4) 0.035(4) 0.033(4) 0.013(3) 0.026(3) -0.002(4) C85 0.038(4) 0.039(4) 0.034(4) 0.002(3) 0.022(3) 0.001(3) C86 0.045(4) 0.026(3) 0.040(4) 0.004(3) 0.024(3) 0.001(3) C87 0.101(7) 0.060(5) 0.042(5) -0.006(4) 0.042(5) -0.017(5) C88 0.068(5) 0.033(4) 0.051(4) 0.007(3) 0.036(4) -0.012(4) Cl1 0.218(10) 0.282(12) 0.175(9) 0.090(8) 0.115(8) 0.004(9) C89 0.36(2) 0.21(3) 0.14(2) -0.001(16) 0.162(15) 0.131(17) Cl2 0.46(2) 0.188(10) 0.128(9) 0.028(8) 0.052(10) 0.141(13) Cl1' 0.181(9) 0.075(5) 0.112(6) 0.009(5) 0.094(6) -0.003(5) C89' 0.24(3) 0.16(3) 0.099(17) 0.010(16) 0.104(13) -0.05(3) Cl2' 0.199(12) 0.123(8) 0.099(6) -0.014(5) 0.058(7) -0.072(8) Cl1" 0.146(13) 0.156(14) 0.29(2) 0.120(14) 0.175(15) 0.122(11) C89" 0.31(3) 0.13(3) 0.19(3) 0.06(3) 0.13(2) 0.07(2) Cl2" 0.33(3) 0.22(2) 0.29(3) 0.04(2) 0.19(3) -0.03(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 1.799(4) . ? Ge1 C53 1.967(5) . ? Ge1 C62 1.978(6) . ? Ge1 C11 2.023(5) . ? Ge2 O2 1.825(4) . ? Ge2 C80 1.973(6) . ? Ge2 C71 1.982(5) . ? Ge2 C32 2.003(5) . ? O1 C1 1.370(6) . ? O2 C4 1.384(6) . ? C1 C2 1.386(7) . ? C1 C10 1.413(7) . ? C2 C3 1.397(8) . ? C3 C4 1.378(7) . ? C4 C5 1.388(7) . ? C5 C10 1.415(7) . ? C5 C6 1.511(7) . ? C6 C7 1.491(7) . ? C6 C32 1.595(7) . ? C7 C8 1.323(7) . ? C8 C9 1.479(7) . ? C9 C10 1.507(7) . ? C9 C11 1.587(7) . ? C11 C12 1.526(7) . ? C11 C23 1.533(8) . ? C12 C13 1.392(7) . ? C12 C17 1.401(7) . ? C13 C14 1.405(7) . ? C14 C15 1.398(7) . ? C14 C24 1.533(8) . ? C15 C16 1.376(8) . ? C16 C17 1.382(7) . ? C17 C18 1.474(8) . ? C18 C19 1.388(8) . ? C18 C23 1.392(7) . ? C19 C20 1.381(8) . ? C20 C21 1.421(8) . ? C21 C22 1.376(8) . ? C21 C28 1.531(8) . ? C22 C23 1.400(7) . ? C24 C25 1.530(8) . ? C24 C27 1.536(8) . ? C24 C26 1.543(8) . ? C28 C29 1.520(9) . ? C28 C30 1.521(9) . ? C28 C30' 1.523(12) . ? C28 C31' 1.528(12) . ? C28 C31 1.572(9) . ? C28 C29' 1.581(12) . ? C32 C44 1.518(7) . ? C32 C33 1.518(7) . ? C33 C34 1.385(7) . ? C33 C38 1.420(7) . ? C34 C35 1.383(7) . ? C35 C36 1.404(7) . ? C35 C45 1.533(8) . ? C36 C37 1.380(8) . ? C37 C38 1.387(7) . ? C38 C39 1.457(7) . ? C39 C40 1.391(7) . ? C39 C44 1.415(7) . ? C40 C41 1.384(7) . ? C41 C42 1.406(7) . ? C42 C43 1.388(7) . ? C42 C49 1.534(8) . ? C43 C44 1.372(7) . ? C45 C46 1.520(9) . ? C45 C47 1.525(9) . ? C45 C48 1.527(9) . ? C49 C51 1.536(8) . ? C49 C52 1.539(8) . ? C49 C50 1.549(8) . ? C53 C54 1.410(8) . ? C53 C58 1.414(7) . ? C54 C55 1.401(8) . ? C54 C59 1.500(8) . ? C55 C56 1.376(8) . ? C56 C57 1.383(8) . ? C56 C60 1.515(8) . ? C57 C58 1.387(8) . ? C58 C61 1.511(8) . ? C62 C63 1.413(8) . ? C62 C67 1.422(8) . ? C63 C64 1.386(9) . ? C63 C68 1.497(9) . ? C64 C65 1.361(11) . ? C65 C66 1.381(11) . ? C65 C69 1.554(11) . ? C66 C67 1.405(9) . ? C67 C70 1.517(9) . ? C71 C76 1.394(8) . ? C71 C72 1.417(8) . ? C72 C73 1.379(9) . ? C72 C77 1.505(9) . ? C73 C74 1.378(9) . ? C74 C75 1.396(9) . ? C74 C78 1.507(9) . ? C75 C76 1.393(8) . ? C76 C79 1.524(8) . ? C80 C81 1.401(8) . ? C80 C85 1.412(8) . ? C81 C82 1.403(8) . ? C81 C86 1.511(7) . ? C82 C83 1.356(8) . ? C83 C84 1.361(8) . ? C83 C87 1.530(8) . ? C84 C85 1.398(8) . ? C85 C88 1.513(8) . ? Cl1 C89 1.693(18) . ? C89 Cl2 1.698(18) . ? Cl1' C89' 1.632(18) . ? C89' Cl2' 1.677(17) . ? Cl1" C89" 1.671(19) . ? C89" Cl2" 1.658(19) . ? 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 C53 102.2(2) . . ? O1 Ge1 C62 107.7(2) . . ? C53 Ge1 C62 105.7(2) . . ? O1 Ge1 C11 99.5(2) . . ? C53 Ge1 C11 129.4(2) . . ? C62 Ge1 C11 110.3(2) . . ? O2 Ge2 C80 103.0(2) . . ? O2 Ge2 C71 103.7(2) . . ? C80 Ge2 C71 110.6(2) . . ? O2 Ge2 C32 98.87(19) . . ? C80 Ge2 C32 119.7(2) . . ? C71 Ge2 C32 117.5(2) . . ? C1 O1 Ge1 124.9(3) . . ? C4 O2 Ge2 122.3(3) . . ? O1 C1 C2 117.7(5) . . ? O1 C1 C10 121.1(5) . . ? C2 C1 C10 121.1(5) . . ? C1 C2 C3 119.7(5) . . ? C4 C3 C2 119.5(5) . . ? C3 C4 O2 117.4(5) . . ? C3 C4 C5 122.2(5) . . ? O2 C4 C5 120.4(5) . . ? C4 C5 C10 119.0(5) . . ? C4 C5 C6 118.8(5) . . ? C10 C5 C6 122.1(5) . . ? C7 C6 C5 112.7(4) . . ? C7 C6 C32 111.6(4) . . ? C5 C6 C32 110.0(4) . . ? C8 C7 C6 124.7(5) . . ? C7 C8 C9 124.9(5) . . ? C8 C9 C10 113.3(5) . . ? C8 C9 C11 110.3(4) . . ? C10 C9 C11 111.9(4) . . ? C1 C10 C5 118.5(5) . . ? C1 C10 C9 119.5(5) . . ? C5 C10 C9 122.0(5) . . ? C12 C11 C23 101.8(4) . . ? C12 C11 C9 113.2(4) . . ? C23 C11 C9 110.9(4) . . ? C12 C11 Ge1 118.1(4) . . ? C23 C11 Ge1 110.1(4) . . ? C9 C11 Ge1 102.9(3) . . ? C13 C12 C17 119.5(5) . . ? C13 C12 C11 129.9(5) . . ? C17 C12 C11 110.6(5) . . ? C12 C13 C14 120.0(5) . . ? C15 C14 C13 118.4(5) . . ? C15 C14 C24 119.6(5) . . ? C13 C14 C24 122.0(5) . . ? C16 C15 C14 122.4(5) . . ? C15 C16 C17 118.5(5) . . ? C16 C17 C12 121.2(5) . . ? C16 C17 C18 130.7(5) . . ? C12 C17 C18 108.2(5) . . ? C19 C18 C23 119.7(6) . . ? C19 C18 C17 130.8(5) . . ? C23 C18 C17 109.4(5) . . ? C20 C19 C18 119.9(6) . . ? C19 C20 C21 121.1(6) . . ? C22 C21 C20 118.2(5) . . ? C22 C21 C28 122.5(5) . . ? C20 C21 C28 119.3(5) . . ? C21 C22 C23 120.9(5) . . ? C18 C23 C22 120.2(5) . . ? C18 C23 C11 110.0(5) . . ? C22 C23 C11 129.7(5) . . ? C25 C24 C14 113.0(5) . . ? C25 C24 C27 108.4(5) . . ? C14 C24 C27 109.8(5) . . ? C25 C24 C26 108.8(5) . . ? C14 C24 C26 108.1(5) . . ? C27 C24 C26 108.7(5) . . ? C29 C28 C30 111.6(7) . . ? C29 C28 C30' 144.3(9) . . ? C30 C28 C30' 53.8(8) . . ? C29 C28 C31' 47.8(8) . . ? C30 C28 C31' 131.4(9) . . ? C30' C28 C31' 113.2(10) . . ? C29 C28 C21 108.2(6) . . ? C30 C28 C21 112.2(6) . . ? C30' C28 C21 107.5(8) . . ? C31' C28 C21 116.1(8) . . ? C29 C28 C31 107.8(7) . . ? C30 C28 C31 107.6(7) . . ? C30' C28 C31 58.6(8) . . ? C31' C28 C31 60.5(9) . . ? C21 C28 C31 109.3(6) . . ? C29 C28 C29' 63.0(8) . . ? C30 C28 C29' 53.2(8) . . ? C30' C28 C29' 106.1(10) . . ? C31' C28 C29' 105.4(10) . . ? C21 C28 C29' 108.1(7) . . ? C31 C28 C29' 142.5(9) . . ? C44 C32 C33 103.2(4) . . ? C44 C32 C6 109.2(4) . . ? C33 C32 C6 111.2(4) . . ? C44 C32 Ge2 114.1(4) . . ? C33 C32 Ge2 115.5(3) . . ? C6 C32 Ge2 103.8(3) . . ? C34 C33 C38 119.9(5) . . ? C34 C33 C32 130.7(5) . . ? C38 C33 C32 109.2(5) . . ? C35 C34 C33 121.4(5) . . ? C34 C35 C36 117.5(5) . . ? C34 C35 C45 121.2(5) . . ? C36 C35 C45 121.0(5) . . ? C37 C36 C35 122.5(5) . . ? C36 C37 C38 119.3(5) . . ? C37 C38 C33 119.1(5) . . ? C37 C38 C39 131.7(5) . . ? C33 C38 C39 108.9(5) . . ? C40 C39 C44 118.9(5) . . ? C40 C39 C38 132.0(5) . . ? C44 C39 C38 109.1(5) . . ? C41 C40 C39 119.5(5) . . ? C40 C41 C42 121.9(5) . . ? C43 C42 C41 117.9(5) . . ? C43 C42 C49 119.7(5) . . ? C41 C42 C49 122.4(5) . . ? C44 C43 C42 121.1(5) . . ? C43 C44 C39 120.7(5) . . ? C43 C44 C32 129.7(5) . . ? C39 C44 C32 109.3(4) . . ? C46 C45 C47 109.8(7) . . ? C46 C45 C48 106.8(6) . . ? C47 C45 C48 108.8(6) . . ? C46 C45 C35 111.2(5) . . ? C47 C45 C35 107.8(5) . . ? C48 C45 C35 112.3(5) . . ? C42 C49 C51 108.0(5) . . ? C42 C49 C52 110.4(5) . . ? C51 C49 C52 109.6(5) . . ? C42 C49 C50 112.2(5) . . ? C51 C49 C50 108.3(5) . . ? C52 C49 C50 108.3(5) . . ? C54 C53 C58 118.9(5) . . ? C54 C53 Ge1 115.7(4) . . ? C58 C53 Ge1 124.5(4) . . ? C55 C54 C53 118.6(5) . . ? C55 C54 C59 116.9(5) . . ? C53 C54 C59 124.5(5) . . ? C56 C55 C54 123.1(6) . . ? C55 C56 C57 117.0(6) . . ? C55 C56 C60 121.7(6) . . ? C57 C56 C60 121.3(6) . . ? C56 C57 C58 123.0(6) . . ? C57 C58 C53 119.1(6) . . ? C57 C58 C61 118.6(5) . . ? C53 C58 C61 122.3(5) . . ? C63 C62 C67 118.2(6) . . ? C63 C62 Ge1 124.3(5) . . ? C67 C62 Ge1 117.4(5) . . ? C64 C63 C62 119.3(7) . . ? C64 C63 C68 115.4(6) . . ? C62 C63 C68 125.3(6) . . ? C65 C64 C63 123.3(7) . . ? C64 C65 C66 118.3(7) . . ? C64 C65 C69 123.2(9) . . ? C66 C65 C69 118.5(9) . . ? C65 C66 C67 121.6(8) . . ? C66 C67 C62 119.3(7) . . ? C66 C67 C70 118.3(7) . . ? C62 C67 C70 122.4(6) . . ? C76 C71 C72 117.9(5) . . ? C76 C71 Ge2 117.1(4) . . ? C72 C71 Ge2 124.7(5) . . ? C73 C72 C71 119.4(6) . . ? C73 C72 C77 116.3(6) . . ? C71 C72 C77 124.3(6) . . ? C74 C73 C72 123.3(7) . . ? C73 C74 C75 117.0(6) . . ? C73 C74 C78 122.5(7) . . ? C75 C74 C78 120.5(7) . . ? C76 C75 C74 121.3(7) . . ? C75 C76 C71 120.8(6) . . ? C75 C76 C79 116.7(6) . . ? C71 C76 C79 122.6(6) . . ? C81 C80 C85 119.0(5) . . ? C81 C80 Ge2 123.9(4) . . ? C85 C80 Ge2 117.1(4) . . ? C80 C81 C82 118.5(5) . . ? C80 C81 C86 124.9(5) . . ? C82 C81 C86 116.6(5) . . ? C83 C82 C81 123.1(6) . . ? C82 C83 C84 117.8(6) . . ? C82 C83 C87 120.5(6) . . ? C84 C83 C87 121.7(6) . . ? C83 C84 C85 123.0(6) . . ? C84 C85 C80 118.4(6) . . ? C84 C85 C88 117.7(5) . . ? C80 C85 C88 123.9(5) . . ? Cl1 C89 Cl2 130(2) . . ? Cl1' C89' Cl2' 122.4(19) . . ? Cl2" C89" Cl1" 134(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.576 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.086 _vrf_PLAT220_10 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.33 Ratio RESPONSE: Terminal methyls of the mesityl groups show strong vibrations. ; _vrf_PLAT222_10 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.65 Ratio RESPONSE: Terminal methyls of the mesityl groups show strong vibrations. ; _vrf_PLAT761_10 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen atoms have been refined by the use of a riding model. ; _vrf_PLAT762_10 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen atoms have been refined by the use of a riding model. ; #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 751863' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H112 Ge2 O3' _chemical_formula_weight 1435.02 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5470(6) _cell_length_b 17.4292(8) _cell_length_c 19.4232(11) _cell_angle_alpha 95.521(2) _cell_angle_beta 93.110(3) _cell_angle_gamma 108.741(3) _cell_volume 3987.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1412 _cell_measurement_theta_min 2.432 _cell_measurement_theta_max 26.735 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9240 _exptl_absorpt_correction_T_max 0.9610 _exptl_absorpt_process_details ? _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 'Bruker CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33775 _diffrn_reflns_av_R_equivalents 0.2098 _diffrn_reflns_av_sigmaI/netI 0.5404 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13802 _reflns_number_gt 4008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13802 _refine_ls_number_parameters 943 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.2580 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 0.703 _refine_ls_restrained_S_all 0.718 _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 0.00498(7) -0.15055(5) 0.26830(4) 0.0241(3) Uani 1 1 d . . . Ge2 Ge 0.06398(7) 0.31590(5) 0.34162(4) 0.0252(3) Uani 1 1 d . . . O1 O 0.0249(4) -0.0803(3) 0.3477(2) 0.0303(14) Uani 1 1 d . . . O2 O -0.0232(4) 0.2231(3) 0.3720(2) 0.0292(14) Uani 1 1 d . . . O3 O 0.1943(5) -0.0113(3) 0.2531(2) 0.0347(14) Uani 1 1 d . . . C1 C 0.0183(6) -0.0029(4) 0.3495(4) 0.024(2) Uani 1 1 d . . . C2 C -0.0290(6) 0.0214(4) 0.4075(4) 0.023(2) Uani 1 1 d U . . H2 H -0.0531 -0.0141 0.4420 0.027 Uiso 1 1 calc R . . C3 C -0.0402(6) 0.0988(4) 0.4140(4) 0.027(2) Uani 1 1 d . . . H3 H -0.0717 0.1168 0.4534 0.032 Uiso 1 1 calc R . . C4 C -0.0053(6) 0.1493(4) 0.3629(4) 0.025(2) Uani 1 1 d . . . C5 C 0.0409(6) 0.1241(4) 0.3037(4) 0.0192(19) Uani 1 1 d . . . C6 C 0.0540(6) 0.0473(5) 0.2979(4) 0.021(2) Uani 1 1 d . . . C7 C 0.0987(6) 0.0129(4) 0.2346(4) 0.0158(19) Uani 1 1 d . . . C8 C 0.1314(6) 0.0731(4) 0.1836(4) 0.026(2) Uani 1 1 d . . . H8 H 0.1611 0.0571 0.1427 0.031 Uiso 1 1 calc R . . C9 C 0.1225(6) 0.1464(4) 0.1905(4) 0.025(2) Uani 1 1 d . . . H9 H 0.1491 0.1799 0.1551 0.030 Uiso 1 1 calc R . . C10 C 0.0731(6) 0.1823(4) 0.2503(3) 0.021(2) Uani 1 1 d . . . H10 H 0.0030 0.1912 0.2312 0.025 Uiso 1 1 calc R . . C11 C 0.2919(7) 0.0545(5) 0.2876(4) 0.056(3) Uani 1 1 d . . . H11A H 0.3104 0.1004 0.2598 0.085 Uiso 1 1 calc R . . H11B H 0.3565 0.0349 0.2924 0.085 Uiso 1 1 calc R . . H11C H 0.2742 0.0726 0.3336 0.085 Uiso 1 1 calc R . . C12 C 0.0092(6) -0.0703(4) 0.1999(3) 0.0195(19) Uani 1 1 d . . . C13 C 0.0380(7) -0.0919(4) 0.1271(4) 0.0179(18) Uani 1 1 d . . . C14 C 0.1335(7) -0.1095(4) 0.1069(4) 0.029(2) Uani 1 1 d . . . H14 H 0.1886 -0.1119 0.1414 0.035 Uiso 1 1 calc R . . C15 C 0.1496(7) -0.1237(4) 0.0359(4) 0.027(2) Uani 1 1 d . . . C16 C 0.0655(7) -0.1199(4) -0.0131(4) 0.035(2) Uani 1 1 d . . . H16 H 0.0734 -0.1294 -0.0613 0.043 Uiso 1 1 calc R . . C17 C -0.0286(7) -0.1025(4) 0.0078(4) 0.033(2) Uani 1 1 d . . . H17 H -0.0846 -0.1010 -0.0265 0.039 Uiso 1 1 calc R . . C18 C -0.0439(7) -0.0873(4) 0.0772(4) 0.024(2) Uani 1 1 d . . . C19 C -0.1341(7) -0.0680(4) 0.1113(4) 0.025(2) Uani 1 1 d . . . C20 C -0.2341(7) -0.0624(4) 0.0858(4) 0.033(2) Uani 1 1 d . . . H20 H -0.2493 -0.0629 0.0373 0.039 Uiso 1 1 calc R . . C21 C -0.3130(7) -0.0561(4) 0.1301(4) 0.037(2) Uani 1 1 d . . . H21 H -0.3831 -0.0530 0.1118 0.045 Uiso 1 1 calc R . . C22 C -0.2917(7) -0.0542(4) 0.2022(5) 0.030(2) Uani 1 1 d . A . C23 C -0.1858(7) -0.0545(4) 0.2272(4) 0.028(2) Uani 1 1 d . . . H23 H -0.1677 -0.0502 0.2759 0.034 Uiso 1 1 calc R . . C24 C -0.1053(7) -0.0610(4) 0.1815(4) 0.024(2) Uani 1 1 d . . . C25 C 0.2537(7) -0.1429(5) 0.0148(4) 0.036(2) Uani 1 1 d . . . C26 C 0.2676(7) -0.2143(5) 0.0510(4) 0.055(3) Uani 1 1 d . . . H26A H 0.2716 -0.2007 0.1015 0.083 Uiso 1 1 calc R . . H26B H 0.3372 -0.2240 0.0386 0.083 Uiso 1 1 calc R . . H26C H 0.2027 -0.2635 0.0361 0.083 Uiso 1 1 calc R . . C27 C 0.2527(7) -0.1652(4) -0.0638(4) 0.053(3) Uani 1 1 d . . . H27A H 0.1859 -0.2126 -0.0800 0.080 Uiso 1 1 calc R . . H27B H 0.3210 -0.1785 -0.0734 0.080 Uiso 1 1 calc R . . H27C H 0.2505 -0.1189 -0.0880 0.080 Uiso 1 1 calc R . . C28 C 0.3604(6) -0.0662(4) 0.0374(4) 0.049(3) Uani 1 1 d . . . H28A H 0.3560 -0.0213 0.0119 0.074 Uiso 1 1 calc R . . H28B H 0.4286 -0.0793 0.0271 0.074 Uiso 1 1 calc R . . H28C H 0.3634 -0.0498 0.0874 0.074 Uiso 1 1 calc R . . C29 C -0.3836(7) -0.0566(5) 0.2525(4) 0.039(2) Uani 1 1 d DU . . C30 C -0.4990(10) -0.0719(9) 0.2212(7) 0.064(4) Uani 0.702(9) 1 d PDU A 1 H30A H -0.5531 -0.1096 0.2471 0.095 Uiso 0.702(9) 1 calc PR A 1 H30B H -0.5059 -0.0959 0.1728 0.095 Uiso 0.702(9) 1 calc PR A 1 H30C H -0.5149 -0.0202 0.2229 0.095 Uiso 0.702(9) 1 calc PR A 1 C31 C -0.3464(11) 0.0223(7) 0.3052(8) 0.071(4) Uani 0.702(9) 1 d PDU A 1 H31A H -0.4086 0.0228 0.3334 0.107 Uiso 0.702(9) 1 calc PR A 1 H31B H -0.3263 0.0702 0.2800 0.107 Uiso 0.702(9) 1 calc PR A 1 H31C H -0.2807 0.0234 0.3355 0.107 Uiso 0.702(9) 1 calc PR A 1 C32 C -0.3925(14) -0.1287(8) 0.2954(7) 0.068(4) Uani 0.702(9) 1 d PDU A 1 H32A H -0.3332 -0.1112 0.3340 0.102 Uiso 0.702(9) 1 calc PR A 1 H32B H -0.3832 -0.1743 0.2655 0.102 Uiso 0.702(9) 1 calc PR A 1 H32C H -0.4668 -0.1462 0.3136 0.102 Uiso 0.702(9) 1 calc PR A 1 C30' C -0.373(4) -0.078(2) 0.3208(12) 0.077(7) Uani 0.298(9) 1 d PDU A 2 H30D H -0.4463 -0.0895 0.3405 0.115 Uiso 0.298(9) 1 calc PR A 2 H30E H -0.3165 -0.0327 0.3500 0.115 Uiso 0.298(9) 1 calc PR A 2 H30F H -0.3500 -0.1267 0.3190 0.115 Uiso 0.298(9) 1 calc PR A 2 C31' C -0.487(2) -0.1297(16) 0.2114(15) 0.064(6) Uani 0.298(9) 1 d PDU A 2 H31D H -0.4683 -0.1802 0.2081 0.095 Uiso 0.298(9) 1 calc PR A 2 H31E H -0.5017 -0.1165 0.1647 0.095 Uiso 0.298(9) 1 calc PR A 2 H31F H -0.5548 -0.1370 0.2365 0.095 Uiso 0.298(9) 1 calc PR A 2 C32' C -0.411(3) 0.0222(14) 0.2456(17) 0.059(4) Uani 0.298(9) 1 d PDU A 2 H32D H -0.4646 0.0276 0.2793 0.089 Uiso 0.298(9) 1 calc PR A 2 H32E H -0.4450 0.0201 0.1985 0.089 Uiso 0.298(9) 1 calc PR A 2 H32F H -0.3416 0.0692 0.2548 0.089 Uiso 0.298(9) 1 calc PR A 2 C33 C 0.1599(6) 0.2684(4) 0.2827(4) 0.0182(18) Uani 1 1 d . . . C34 C 0.2060(8) 0.3204(4) 0.2257(4) 0.026(2) Uani 1 1 d . . . C35 C 0.1471(7) 0.3421(4) 0.1710(4) 0.025(2) Uani 1 1 d . . . H35 H 0.0669 0.3244 0.1666 0.030 Uiso 1 1 calc R . . C36 C 0.2075(8) 0.3895(4) 0.1238(4) 0.030(2) Uani 1 1 d . . . C37 C 0.3259(8) 0.4163(4) 0.1316(4) 0.039(2) Uani 1 1 d . . . H37 H 0.3669 0.4514 0.1007 0.047 Uiso 1 1 calc R . . C38 C 0.3845(7) 0.3927(5) 0.1838(4) 0.038(2) Uani 1 1 d . . . H38 H 0.4647 0.4104 0.1882 0.045 Uiso 1 1 calc R . . C39 C 0.3239(8) 0.3434(4) 0.2288(4) 0.027(2) Uani 1 1 d . . . C40 C 0.3613(7) 0.3064(4) 0.2869(4) 0.026(2) Uani 1 1 d . . . C41 C 0.4687(7) 0.3105(5) 0.3119(4) 0.036(2) Uani 1 1 d . . . H41 H 0.5334 0.3371 0.2893 0.043 Uiso 1 1 calc R . . C42 C 0.4779(8) 0.2737(5) 0.3724(5) 0.042(2) Uani 1 1 d . . . H42 H 0.5508 0.2757 0.3904 0.051 Uiso 1 1 calc R . . C43 C 0.3867(8) 0.2351(5) 0.4067(4) 0.031(2) Uani 1 1 d . . . C44 C 0.2797(7) 0.2313(4) 0.3786(4) 0.024(2) Uani 1 1 d . . . H44 H 0.2151 0.2047 0.4013 0.029 Uiso 1 1 calc R . . C45 C 0.2662(7) 0.2651(4) 0.3193(4) 0.025(2) Uani 1 1 d . . . C46 C 0.1484(8) 0.4150(5) 0.0631(4) 0.041(2) Uani 1 1 d . . . C47 C 0.0184(8) 0.3706(5) 0.0562(4) 0.053(3) Uani 1 1 d . . . H47A H -0.0160 0.3857 0.0154 0.079 Uiso 1 1 calc R . . H47B H -0.0135 0.3868 0.0979 0.079 Uiso 1 1 calc R . . H47C H 0.0029 0.3115 0.0509 0.079 Uiso 1 1 calc R . . C48 C 0.1670(8) 0.5069(5) 0.0749(4) 0.080(3) Uani 1 1 d . . . H48A H 0.2482 0.5370 0.0830 0.119 Uiso 1 1 calc R . . H48B H 0.1293 0.5188 0.1155 0.119 Uiso 1 1 calc R . . H48C H 0.1355 0.5235 0.0339 0.119 Uiso 1 1 calc R . . C49 C 0.1920(8) 0.3927(5) -0.0059(4) 0.061(3) Uani 1 1 d . . . H49A H 0.2724 0.4242 -0.0056 0.092 Uiso 1 1 calc R . . H49B H 0.1494 0.4055 -0.0445 0.092 Uiso 1 1 calc R . . H49C H 0.1820 0.3343 -0.0118 0.092 Uiso 1 1 calc R . . C50 C 0.4035(9) 0.1996(6) 0.4762(4) 0.050(3) Uani 1 1 d . . . C51 C 0.4660(8) 0.2716(5) 0.5312(4) 0.073(3) Uani 1 1 d . . . H51A H 0.4222 0.3089 0.5364 0.110 Uiso 1 1 calc R . . H51B H 0.5404 0.3006 0.5166 0.110 Uiso 1 1 calc R . . H51C H 0.4754 0.2512 0.5757 0.110 Uiso 1 1 calc R . . C52 C 0.4773(8) 0.1437(5) 0.4635(4) 0.075(3) Uani 1 1 d . . . H52A H 0.4896 0.1215 0.5066 0.113 Uiso 1 1 calc R . . H52B H 0.5502 0.1756 0.4489 0.113 Uiso 1 1 calc R . . H52C H 0.4383 0.0988 0.4272 0.113 Uiso 1 1 calc R . . C53 C 0.2907(8) 0.1501(5) 0.5019(4) 0.073(3) Uani 1 1 d . . . H53A H 0.3056 0.1282 0.5447 0.110 Uiso 1 1 calc R . . H53B H 0.2496 0.1049 0.4663 0.110 Uiso 1 1 calc R . . H53C H 0.2449 0.1855 0.5111 0.110 Uiso 1 1 calc R . . C54 C -0.1366(6) -0.2365(4) 0.2804(4) 0.025(2) Uani 1 1 d . . . C55 C -0.1477(7) -0.2675(4) 0.3456(4) 0.024(2) Uani 1 1 d . . . C56 C -0.2440(7) -0.3294(4) 0.3573(4) 0.032(2) Uani 1 1 d . . . H56 H -0.2492 -0.3483 0.4017 0.039 Uiso 1 1 calc R . . C57 C -0.3321(7) -0.3644(4) 0.3071(5) 0.032(2) Uani 1 1 d . . . C58 C -0.3219(7) -0.3355(4) 0.2427(4) 0.027(2) Uani 1 1 d . . . H58 H -0.3816 -0.3590 0.2069 0.033 Uiso 1 1 calc R . . C59 C -0.2275(7) -0.2734(4) 0.2294(4) 0.025(2) Uani 1 1 d . . . C60 C -0.0534(7) -0.2364(4) 0.4052(4) 0.043(2) Uani 1 1 d . . . H60A H -0.0753 -0.2681 0.4442 0.065 Uiso 1 1 calc R . . H60B H -0.0410 -0.1787 0.4202 0.065 Uiso 1 1 calc R . . H60C H 0.0164 -0.2427 0.3892 0.065 Uiso 1 1 calc R . . C61 C -0.4359(7) -0.4327(4) 0.3209(4) 0.046(2) Uani 1 1 d . . . H61A H -0.4234 -0.4852 0.3109 0.069 Uiso 1 1 calc R . . H61B H -0.5011 -0.4321 0.2910 0.069 Uiso 1 1 calc R . . H61C H -0.4505 -0.4250 0.3697 0.069 Uiso 1 1 calc R . . C62 C -0.2290(6) -0.2506(4) 0.1557(3) 0.032(2) Uani 1 1 d . . . H62A H -0.2594 -0.3004 0.1228 0.049 Uiso 1 1 calc R . . H62B H -0.1519 -0.2207 0.1459 0.049 Uiso 1 1 calc R . . H62C H -0.2767 -0.2162 0.1511 0.049 Uiso 1 1 calc R . . C63 C 0.1256(6) -0.1990(4) 0.2724(4) 0.0179(18) Uani 1 1 d . . . C64 C 0.2161(7) -0.1788(4) 0.3234(4) 0.029(2) Uani 1 1 d . . . C65 C 0.2931(7) -0.2214(5) 0.3229(4) 0.039(2) Uani 1 1 d . . . H65 H 0.3525 -0.2070 0.3591 0.047 Uiso 1 1 calc R . . C66 C 0.2858(7) -0.2843(5) 0.2712(5) 0.040(2) Uani 1 1 d . . . C67 C 0.1972(7) -0.3045(4) 0.2206(4) 0.038(2) Uani 1 1 d . . . H67 H 0.1910 -0.3469 0.1845 0.046 Uiso 1 1 calc R . . C68 C 0.1151(7) -0.2651(4) 0.2199(4) 0.029(2) Uani 1 1 d . . . C69 C 0.2374(7) -0.1118(4) 0.3846(4) 0.047(2) Uani 1 1 d . . . H69A H 0.2255 -0.0635 0.3681 0.070 Uiso 1 1 calc R . . H69B H 0.3154 -0.0974 0.4052 0.070 Uiso 1 1 calc R . . H69C H 0.1851 -0.1316 0.4196 0.070 Uiso 1 1 calc R . . C70 C 0.3712(7) -0.3290(5) 0.2712(5) 0.078(3) Uani 1 1 d . . . H70A H 0.3325 -0.3870 0.2744 0.116 Uiso 1 1 calc R . . H70B H 0.4275 -0.3058 0.3111 0.116 Uiso 1 1 calc R . . H70C H 0.4088 -0.3231 0.2282 0.116 Uiso 1 1 calc R . . C71 C 0.0205(6) -0.2961(4) 0.1643(4) 0.031(2) Uani 1 1 d . . . H71A H 0.0393 -0.3317 0.1282 0.046 Uiso 1 1 calc R . . H71B H 0.0081 -0.2500 0.1440 0.046 Uiso 1 1 calc R . . H71C H -0.0483 -0.3271 0.1841 0.046 Uiso 1 1 calc R . . C72 C 0.1226(7) 0.3876(4) 0.4295(4) 0.026(2) Uani 1 1 d . . . C73 C 0.2325(7) 0.4356(4) 0.4477(4) 0.026(2) Uani 1 1 d . . . C74 C 0.2649(7) 0.4857(4) 0.5120(4) 0.036(2) Uani 1 1 d . . . H74 H 0.3413 0.5196 0.5226 0.043 Uiso 1 1 calc R . . C75 C 0.1870(7) 0.4863(4) 0.5600(4) 0.030(2) Uani 1 1 d . . . C76 C 0.0749(7) 0.4390(4) 0.5414(4) 0.031(2) Uani 1 1 d . . . H76 H 0.0199 0.4408 0.5727 0.038 Uiso 1 1 calc R . . C77 C 0.0402(7) 0.3885(4) 0.4778(4) 0.030(2) Uani 1 1 d . . . C78 C 0.3246(6) 0.4431(4) 0.4008(4) 0.039(2) Uani 1 1 d . . . H78A H 0.3718 0.4114 0.4157 0.058 Uiso 1 1 calc R . . H78B H 0.3711 0.5006 0.4028 0.058 Uiso 1 1 calc R . . H78C H 0.2915 0.4221 0.3531 0.058 Uiso 1 1 calc R . . C79 C 0.2250(7) 0.5373(4) 0.6297(4) 0.046(3) Uani 1 1 d . . . H79A H 0.1667 0.5604 0.6436 0.069 Uiso 1 1 calc R . . H79B H 0.2955 0.5817 0.6263 0.069 Uiso 1 1 calc R . . H79C H 0.2377 0.5031 0.6643 0.069 Uiso 1 1 calc R . . C80 C -0.0841(6) 0.3413(4) 0.4646(4) 0.033(2) Uani 1 1 d . . . H80A H -0.0976 0.2850 0.4744 0.050 Uiso 1 1 calc R . . H80B H -0.1092 0.3412 0.4159 0.050 Uiso 1 1 calc R . . H80C H -0.1263 0.3669 0.4948 0.050 Uiso 1 1 calc R . . C81 C -0.0357(7) 0.3571(5) 0.2841(3) 0.024(2) Uani 1 1 d . . . C82 C 0.0092(7) 0.4392(5) 0.2690(4) 0.028(2) Uani 1 1 d . . . C83 C -0.0565(8) 0.4719(5) 0.2294(4) 0.035(2) Uani 1 1 d . . . H83 H -0.0264 0.5274 0.2214 0.042 Uiso 1 1 calc R . . C84 C -0.1626(8) 0.4274(6) 0.2013(4) 0.038(2) Uani 1 1 d . . . C85 C -0.2076(7) 0.3475(5) 0.2152(4) 0.041(2) Uani 1 1 d . . . H85 H -0.2820 0.3161 0.1963 0.049 Uiso 1 1 calc R . . C86 C -0.1461(7) 0.3120(5) 0.2562(4) 0.026(2) Uani 1 1 d . . . C87 C 0.1255(7) 0.4943(4) 0.2968(4) 0.038(2) Uani 1 1 d . . . H87A H 0.1820 0.4743 0.2753 0.057 Uiso 1 1 calc R . . H87B H 0.1346 0.4946 0.3472 0.057 Uiso 1 1 calc R . . H87C H 0.1358 0.5498 0.2858 0.057 Uiso 1 1 calc R . . C88 C -0.2347(8) 0.4631(5) 0.1565(4) 0.071(3) Uani 1 1 d . . . H88A H -0.3022 0.4192 0.1351 0.107 Uiso 1 1 calc R . . H88B H -0.1907 0.4897 0.1202 0.107 Uiso 1 1 calc R . . H88C H -0.2575 0.5032 0.1857 0.107 Uiso 1 1 calc R . . C89 C -0.2068(7) 0.2241(4) 0.2687(4) 0.051(3) Uani 1 1 d . . . H89A H -0.1667 0.1887 0.2485 0.077 Uiso 1 1 calc R . . H89B H -0.2844 0.2063 0.2468 0.077 Uiso 1 1 calc R . . H89C H -0.2081 0.2209 0.3187 0.077 Uiso 1 1 calc R . . C90 C 0.5072(10) 0.3519(7) -0.0113(6) 0.100(4) Uani 1 1 d DU . . H90A H 0.4693 0.3928 -0.0041 0.150 Uiso 1 1 calc R . . H90B H 0.5166 0.3422 -0.0608 0.150 Uiso 1 1 calc R . . H90C H 0.5815 0.3717 0.0152 0.150 Uiso 1 1 calc R . . C91 C 0.4499(13) 0.2881(7) 0.0085(6) 0.116(5) Uani 1 1 d DU . . H91A H 0.4336 0.2471 -0.0330 0.139 Uiso 1 1 calc R . . H91B H 0.3770 0.2963 0.0171 0.139 Uiso 1 1 calc R . . C92 C 0.4722(11) 0.2478(7) 0.0633(6) 0.118(4) Uani 1 1 d DU . . H92A H 0.5447 0.2391 0.0545 0.141 Uiso 1 1 calc R . . H92B H 0.4891 0.2889 0.1048 0.141 Uiso 1 1 calc R . . C93 C 0.4110(8) 0.1807(5) 0.0842(4) 0.039(3) Uani 1 1 d DU . . H93A H 0.3973 0.1360 0.0459 0.047 Uiso 1 1 calc R . . H93B H 0.3368 0.1859 0.0939 0.047 Uiso 1 1 calc R . . C94 C 0.4568(12) 0.1585(8) 0.1434(6) 0.158(5) Uani 1 1 d DU . . H94A H 0.5069 0.1278 0.1297 0.237 Uiso 1 1 calc R . . H94B H 0.3956 0.1244 0.1675 0.237 Uiso 1 1 calc R . . H94C H 0.4999 0.2077 0.1745 0.237 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 0.0355(7) 0.0192(5) 0.0199(5) 0.0043(4) 0.0023(5) 0.0115(5) Ge2 0.0338(6) 0.0190(5) 0.0228(5) 0.0038(4) 0.0076(5) 0.0078(5) O1 0.062(4) 0.017(3) 0.016(3) 0.004(3) 0.008(3) 0.017(3) O2 0.040(4) 0.021(3) 0.029(3) 0.004(3) 0.014(3) 0.011(3) O3 0.043(4) 0.026(3) 0.033(3) -0.002(3) -0.003(3) 0.010(3) C1 0.039(6) 0.017(4) 0.017(5) -0.004(4) -0.011(4) 0.015(4) C2 0.031(5) 0.022(4) 0.017(4) 0.019(4) 0.007(4) 0.007(4) C3 0.032(6) 0.030(5) 0.018(5) 0.001(4) 0.010(4) 0.008(4) C4 0.033(6) 0.019(5) 0.021(5) 0.004(4) 0.006(4) 0.006(4) C5 0.022(5) 0.016(4) 0.018(5) 0.008(4) 0.002(4) 0.002(4) C6 0.028(5) 0.027(5) 0.009(4) 0.005(4) -0.003(4) 0.009(4) C7 0.011(5) 0.016(4) 0.015(5) 0.011(4) -0.002(4) -0.004(4) C8 0.039(6) 0.018(4) 0.018(5) -0.002(4) 0.004(4) 0.007(4) C9 0.033(6) 0.024(5) 0.015(4) 0.000(4) 0.004(4) 0.006(4) C10 0.027(5) 0.021(4) 0.011(4) 0.003(4) 0.003(4) 0.004(4) C11 0.044(6) 0.052(6) 0.064(7) 0.002(5) -0.015(6) 0.009(5) C12 0.025(5) 0.023(4) 0.014(4) 0.007(4) 0.001(4) 0.011(4) C13 0.027(5) 0.014(4) 0.013(4) 0.008(4) 0.003(4) 0.005(4) C14 0.043(6) 0.014(4) 0.030(5) 0.010(4) -0.003(5) 0.008(4) C15 0.032(6) 0.025(5) 0.024(5) 0.003(4) 0.013(5) 0.008(4) C16 0.048(6) 0.036(5) 0.019(5) 0.001(4) 0.001(5) 0.011(5) C17 0.038(6) 0.036(5) 0.026(5) 0.001(4) 0.000(5) 0.014(5) C18 0.037(6) 0.026(5) 0.009(4) 0.006(4) 0.004(5) 0.010(4) C19 0.031(6) 0.023(5) 0.023(5) 0.011(4) -0.001(5) 0.010(4) C20 0.050(7) 0.036(5) 0.015(5) 0.010(4) -0.013(5) 0.018(5) C21 0.038(6) 0.047(6) 0.035(6) 0.017(5) -0.005(5) 0.024(5) C22 0.028(6) 0.017(4) 0.047(6) 0.004(5) 0.006(5) 0.008(4) C23 0.032(6) 0.024(5) 0.025(5) 0.003(4) -0.001(5) 0.004(4) C24 0.030(6) 0.016(4) 0.030(5) 0.013(4) 0.007(5) 0.009(4) C25 0.050(7) 0.037(5) 0.024(5) 0.012(5) 0.018(5) 0.017(5) C26 0.069(7) 0.060(6) 0.059(6) 0.023(5) 0.041(6) 0.042(6) C27 0.061(7) 0.057(6) 0.042(6) -0.004(5) 0.024(5) 0.019(5) C28 0.037(6) 0.045(6) 0.058(6) 0.016(5) 0.018(5) -0.002(5) C29 0.030(5) 0.041(5) 0.049(6) 0.011(4) 0.011(5) 0.012(5) C30 0.029(6) 0.081(9) 0.083(9) 0.011(8) 0.021(6) 0.019(7) C31 0.052(9) 0.061(7) 0.086(10) -0.012(7) 0.043(7) -0.002(7) C32 0.082(11) 0.080(9) 0.061(10) 0.041(8) 0.049(9) 0.037(11) C30' 0.088(13) 0.096(14) 0.054(10) 0.027(11) 0.036(10) 0.032(15) C31' 0.030(10) 0.070(10) 0.078(11) 0.019(12) 0.028(9) -0.007(10) C32' 0.035(9) 0.062(8) 0.089(10) 0.009(8) 0.037(8) 0.023(7) C33 0.021(5) 0.013(4) 0.020(5) 0.002(4) -0.001(4) 0.005(4) C34 0.044(7) 0.013(4) 0.018(5) -0.003(4) 0.005(5) 0.008(4) C35 0.038(6) 0.015(4) 0.026(5) 0.003(4) 0.013(5) 0.012(4) C36 0.047(7) 0.017(5) 0.024(5) 0.001(4) 0.012(5) 0.007(5) C37 0.061(8) 0.028(5) 0.015(5) 0.000(4) 0.015(5) -0.003(5) C38 0.042(6) 0.034(5) 0.027(5) -0.004(5) 0.008(5) 0.001(5) C39 0.043(7) 0.013(4) 0.021(5) -0.004(4) 0.009(5) 0.001(4) C40 0.023(6) 0.023(5) 0.030(5) 0.000(4) 0.011(5) 0.002(4) C41 0.026(6) 0.048(6) 0.034(6) 0.003(5) 0.016(5) 0.009(5) C42 0.030(6) 0.048(6) 0.051(7) 0.002(5) -0.005(6) 0.018(5) C43 0.034(6) 0.042(6) 0.019(5) 0.000(5) -0.004(5) 0.016(5) C44 0.027(6) 0.024(5) 0.018(5) -0.001(4) 0.001(5) 0.004(4) C45 0.043(6) 0.018(4) 0.013(5) -0.001(4) 0.000(5) 0.010(4) C46 0.066(8) 0.026(5) 0.035(6) 0.003(5) 0.016(6) 0.020(5) C47 0.088(9) 0.055(6) 0.027(6) 0.016(5) -0.007(6) 0.038(6) C48 0.125(10) 0.043(6) 0.076(8) 0.014(6) -0.009(7) 0.037(6) C49 0.071(8) 0.100(8) 0.020(5) -0.001(5) 0.006(5) 0.041(6) C50 0.063(8) 0.059(7) 0.031(6) -0.002(5) -0.016(6) 0.031(6) C51 0.080(8) 0.087(8) 0.041(6) -0.019(6) -0.030(6) 0.024(6) C52 0.080(8) 0.091(8) 0.074(8) 0.024(6) -0.008(6) 0.054(7) C53 0.062(8) 0.084(8) 0.067(7) 0.043(6) -0.016(6) 0.008(6) C54 0.038(6) 0.016(4) 0.022(5) -0.002(4) 0.006(5) 0.011(4) C55 0.032(6) 0.025(5) 0.024(5) 0.014(4) 0.009(5) 0.018(4) C56 0.031(6) 0.032(5) 0.036(6) 0.025(5) 0.010(5) 0.007(5) C57 0.029(6) 0.023(5) 0.051(6) 0.013(5) 0.024(5) 0.013(4) C58 0.028(6) 0.023(5) 0.033(5) 0.003(4) 0.010(5) 0.008(4) C59 0.040(6) 0.025(5) 0.019(5) 0.013(4) 0.012(5) 0.018(5) C60 0.046(6) 0.052(6) 0.032(5) 0.013(5) 0.003(5) 0.015(5) C61 0.043(6) 0.044(6) 0.057(6) 0.019(5) 0.024(5) 0.014(5) C62 0.041(6) 0.031(5) 0.025(5) 0.003(4) 0.002(5) 0.012(4) C63 0.023(5) 0.016(4) 0.016(4) 0.009(4) 0.000(4) 0.007(4) C64 0.024(5) 0.019(5) 0.043(6) 0.007(4) 0.005(5) 0.006(4) C65 0.036(6) 0.037(5) 0.046(6) 0.014(5) -0.005(5) 0.013(5) C66 0.034(6) 0.025(5) 0.070(7) 0.011(5) 0.012(6) 0.016(5) C67 0.045(6) 0.022(5) 0.049(6) 0.006(4) 0.006(5) 0.012(5) C68 0.026(6) 0.028(5) 0.037(5) 0.018(4) 0.011(5) 0.008(4) C69 0.055(7) 0.046(6) 0.033(5) -0.003(5) -0.010(5) 0.011(5) C70 0.047(7) 0.065(7) 0.138(10) 0.014(6) 0.001(7) 0.041(6) C71 0.043(6) 0.018(4) 0.037(5) -0.001(4) 0.003(5) 0.019(4) C72 0.035(6) 0.020(5) 0.022(5) -0.002(4) 0.000(5) 0.008(4) C73 0.030(6) 0.021(4) 0.028(5) 0.000(4) 0.013(5) 0.009(4) C74 0.045(6) 0.022(5) 0.037(5) 0.005(4) 0.011(5) 0.005(4) C75 0.036(6) 0.027(5) 0.032(5) 0.009(4) 0.009(5) 0.014(5) C76 0.047(7) 0.035(5) 0.020(5) 0.003(4) 0.007(5) 0.024(5) C77 0.027(6) 0.030(5) 0.035(5) 0.011(5) -0.002(5) 0.010(4) C78 0.044(6) 0.031(5) 0.028(5) -0.010(4) 0.008(5) -0.001(4) C79 0.054(7) 0.054(6) 0.035(6) -0.011(5) 0.003(5) 0.030(5) C80 0.041(6) 0.030(5) 0.034(5) -0.003(4) 0.011(5) 0.018(4) C81 0.031(6) 0.031(5) 0.014(5) 0.005(4) 0.008(4) 0.015(4) C82 0.043(6) 0.026(5) 0.017(5) -0.003(4) 0.009(5) 0.018(5) C83 0.052(7) 0.025(5) 0.032(6) 0.010(4) 0.003(5) 0.019(5) C84 0.052(7) 0.056(7) 0.023(5) 0.016(5) 0.000(5) 0.035(6) C85 0.049(7) 0.047(6) 0.029(6) 0.000(5) 0.002(5) 0.022(5) C86 0.038(6) 0.027(5) 0.017(5) 0.005(4) 0.009(5) 0.015(5) C87 0.052(7) 0.029(5) 0.040(6) 0.016(4) 0.012(5) 0.018(5) C88 0.073(8) 0.085(8) 0.061(7) 0.026(6) -0.004(6) 0.031(7) C89 0.041(6) 0.039(6) 0.063(7) -0.002(5) -0.010(5) 0.005(5) C90 0.091(11) 0.157(12) 0.087(10) -0.004(8) -0.007(8) 0.096(10) C91 0.228(17) 0.134(11) 0.060(8) 0.021(8) 0.015(10) 0.159(11) C92 0.174(13) 0.148(10) 0.081(9) 0.002(7) 0.041(9) 0.119(9) C93 0.072(8) 0.044(6) 0.016(5) 0.000(5) 0.004(5) 0.041(6) C94 0.193(16) 0.194(14) 0.111(10) 0.020(9) 0.033(10) 0.094(12) _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 1.828(4) . ? Ge1 C63 1.957(7) . ? Ge1 C54 1.964(7) . ? Ge1 C12 2.010(7) . ? Ge2 O2 1.810(5) . ? Ge2 C72 1.969(7) . ? Ge2 C81 1.976(7) . ? Ge2 C33 2.013(6) . ? O1 C1 1.375(7) . ? O2 C4 1.372(7) . ? O3 C7 1.432(7) . ? O3 C11 1.457(8) . ? C1 C6 1.392(9) . ? C1 C2 1.394(8) . ? C2 C3 1.395(8) . ? C3 C4 1.386(9) . ? C4 C5 1.411(9) . ? C5 C6 1.396(7) . ? C5 C10 1.500(9) . ? C6 C7 1.528(9) . ? C7 C8 1.489(9) . ? C7 C12 1.582(8) . ? C8 C9 1.313(8) . ? C9 C10 1.519(8) . ? C10 C33 1.590(8) . ? C12 C13 1.521(8) . ? C12 C24 1.524(9) . ? C13 C14 1.396(9) . ? C13 C18 1.400(9) . ? C14 C15 1.415(9) . ? C15 C16 1.404(9) . ? C15 C25 1.516(9) . ? C16 C17 1.383(9) . ? C17 C18 1.384(9) . ? C18 C19 1.454(9) . ? C19 C20 1.360(9) . ? C19 C24 1.377(9) . ? C20 C21 1.369(9) . ? C21 C22 1.407(9) . ? C22 C23 1.392(9) . ? C22 C29 1.544(10) . ? C23 C24 1.405(9) . ? C25 C27 1.536(9) . ? C25 C26 1.538(9) . ? C25 C28 1.564(9) . ? C29 C30' 1.424(19) . ? C29 C30 1.470(12) . ? C29 C32' 1.536(17) . ? C29 C32 1.551(12) . ? C29 C31 1.556(11) . ? C29 C31' 1.605(17) . ? C33 C45 1.497(9) . ? C33 C34 1.519(9) . ? C34 C39 1.399(9) . ? C34 C35 1.412(9) . ? C35 C36 1.383(9) . ? C36 C37 1.402(10) . ? C36 C46 1.535(10) . ? C37 C38 1.388(9) . ? C38 C39 1.369(9) . ? C39 C40 1.480(10) . ? C40 C41 1.384(9) . ? C40 C45 1.399(9) . ? C41 C42 1.409(10) . ? C42 C43 1.371(10) . ? C43 C44 1.400(9) . ? C43 C50 1.569(10) . ? C44 C45 1.370(9) . ? C46 C48 1.535(9) . ? C46 C49 1.537(9) . ? C46 C47 1.557(10) . ? C50 C51 1.532(10) . ? C50 C53 1.541(11) . ? C50 C52 1.557(10) . ? C54 C59 1.407(9) . ? C54 C55 1.419(9) . ? C55 C56 1.384(9) . ? C55 C60 1.534(9) . ? C56 C57 1.371(9) . ? C57 C58 1.390(9) . ? C57 C61 1.513(9) . ? C58 C59 1.380(9) . ? C59 C62 1.522(8) . ? C63 C64 1.396(9) . ? C63 C68 1.431(8) . ? C64 C65 1.396(9) . ? C64 C69 1.531(9) . ? C65 C66 1.390(9) . ? C66 C67 1.374(9) . ? C66 C70 1.513(9) . ? C67 C68 1.409(9) . ? C68 C71 1.483(9) . ? C72 C73 1.370(9) . ? C72 C77 1.436(9) . ? C73 C74 1.412(9) . ? C73 C78 1.490(9) . ? C74 C75 1.389(9) . ? C75 C76 1.390(9) . ? C75 C79 1.508(9) . ? C76 C77 1.406(9) . ? C77 C80 1.505(9) . ? C81 C86 1.403(9) . ? C81 C82 1.426(9) . ? C82 C83 1.383(9) . ? C82 C87 1.502(9) . ? C83 C84 1.359(10) . ? C84 C85 1.383(10) . ? C84 C88 1.531(10) . ? C85 C86 1.396(9) . ? C86 C89 1.525(9) . ? C90 C91 1.224(11) . ? C91 C92 1.394(11) . ? C92 C93 1.292(10) . ? C93 C94 1.400(10) . ? 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 C63 107.5(3) . . ? O1 Ge1 C54 102.2(3) . . ? C63 Ge1 C54 107.2(3) . . ? O1 Ge1 C12 97.7(2) . . ? C63 Ge1 C12 118.6(3) . . ? C54 Ge1 C12 120.9(3) . . ? O2 Ge2 C72 101.7(3) . . ? O2 Ge2 C81 107.7(3) . . ? C72 Ge2 C81 111.4(3) . . ? O2 Ge2 C33 98.8(2) . . ? C72 Ge2 C33 123.4(3) . . ? C81 Ge2 C33 111.3(3) . . ? C1 O1 Ge1 124.2(4) . . ? C4 O2 Ge2 124.9(4) . . ? C7 O3 C11 114.6(5) . . ? O1 C1 C6 123.6(7) . . ? O1 C1 C2 114.3(7) . . ? C6 C1 C2 122.1(7) . . ? C1 C2 C3 118.8(7) . . ? C4 C3 C2 119.7(7) . . ? O2 C4 C3 116.0(6) . . ? O2 C4 C5 122.5(7) . . ? C3 C4 C5 121.5(7) . . ? C6 C5 C4 118.7(7) . . ? C6 C5 C10 123.8(6) . . ? C4 C5 C10 117.5(6) . . ? C1 C6 C5 119.2(7) . . ? C1 C6 C7 117.9(7) . . ? C5 C6 C7 122.8(7) . . ? O3 C7 C8 108.4(6) . . ? O3 C7 C6 112.3(6) . . ? C8 C7 C6 111.5(6) . . ? O3 C7 C12 102.3(5) . . ? C8 C7 C12 111.4(6) . . ? C6 C7 C12 110.6(6) . . ? C9 C8 C7 125.3(7) . . ? C8 C9 C10 125.6(7) . . ? C5 C10 C9 110.9(6) . . ? C5 C10 C33 112.0(6) . . ? C9 C10 C33 109.9(6) . . ? C13 C12 C24 99.0(6) . . ? C13 C12 C7 110.2(6) . . ? C24 C12 C7 111.8(5) . . ? C13 C12 Ge1 117.0(4) . . ? C24 C12 Ge1 113.7(5) . . ? C7 C12 Ge1 105.2(4) . . ? C14 C13 C18 120.5(7) . . ? C14 C13 C12 128.7(7) . . ? C18 C13 C12 110.7(6) . . ? C13 C14 C15 121.1(7) . . ? C16 C15 C14 117.3(7) . . ? C16 C15 C25 122.3(7) . . ? C14 C15 C25 120.4(7) . . ? C17 C16 C15 120.9(7) . . ? C16 C17 C18 122.0(8) . . ? C17 C18 C13 118.2(7) . . ? C17 C18 C19 131.9(7) . . ? C13 C18 C19 109.9(6) . . ? C20 C19 C24 121.7(8) . . ? C20 C19 C18 132.0(7) . . ? C24 C19 C18 106.2(7) . . ? C19 C20 C21 120.1(7) . . ? C20 C21 C22 120.9(8) . . ? C23 C22 C21 117.8(8) . . ? C23 C22 C29 120.1(8) . . ? C21 C22 C29 122.0(8) . . ? C22 C23 C24 120.9(7) . . ? C19 C24 C23 118.4(7) . . ? C19 C24 C12 114.0(7) . . ? C23 C24 C12 127.3(7) . . ? C15 C25 C27 113.9(7) . . ? C15 C25 C26 110.7(6) . . ? C27 C25 C26 107.7(6) . . ? C15 C25 C28 108.9(6) . . ? C27 C25 C28 107.2(6) . . ? C26 C25 C28 108.3(7) . . ? C30' C29 C30 117(2) . . ? C30' C29 C32' 116.9(16) . . ? C30 C29 C32' 67.0(11) . . ? C30' C29 C22 121.3(19) . . ? C30 C29 C22 117.0(8) . . ? C32' C29 C22 104.6(11) . . ? C30' C29 C32 35.7(13) . . ? C30 C29 C32 105.1(9) . . ? C32' C29 C32 147.0(13) . . ? C22 C29 C32 107.2(8) . . ? C30' C29 C31 70.9(14) . . ? C30 C29 C31 110.0(8) . . ? C32' C29 C31 52.9(11) . . ? C22 C29 C31 110.3(7) . . ? C32 C29 C31 106.6(8) . . ? C30' C29 C31' 105.7(17) . . ? C30 C29 C31' 40.2(10) . . ? C32' C29 C31' 106.4(14) . . ? C22 C29 C31' 99.7(12) . . ? C32 C29 C31' 76.7(12) . . ? C31 C29 C31' 146.6(14) . . ? C45 C33 C34 101.5(6) . . ? C45 C33 C10 115.0(5) . . ? C34 C33 C10 110.6(6) . . ? C45 C33 Ge2 115.6(5) . . ? C34 C33 Ge2 111.8(4) . . ? C10 C33 Ge2 102.7(4) . . ? C39 C34 C35 119.1(8) . . ? C39 C34 C33 111.4(7) . . ? C35 C34 C33 129.3(8) . . ? C36 C35 C34 119.3(8) . . ? C35 C36 C37 119.7(8) . . ? C35 C36 C46 121.8(8) . . ? C37 C36 C46 118.5(8) . . ? C38 C37 C36 121.3(8) . . ? C39 C38 C37 118.5(8) . . ? C38 C39 C34 121.7(8) . . ? C38 C39 C40 131.0(8) . . ? C34 C39 C40 107.3(7) . . ? C41 C40 C45 121.1(8) . . ? C41 C40 C39 130.5(8) . . ? C45 C40 C39 108.3(7) . . ? C40 C41 C42 117.1(8) . . ? C43 C42 C41 123.2(8) . . ? C42 C43 C44 117.5(8) . . ? C42 C43 C50 120.6(8) . . ? C44 C43 C50 121.9(8) . . ? C45 C44 C43 121.5(8) . . ? C44 C45 C40 119.5(8) . . ? C44 C45 C33 129.1(8) . . ? C40 C45 C33 111.4(7) . . ? C48 C46 C36 110.1(7) . . ? C48 C46 C49 110.6(7) . . ? C36 C46 C49 110.5(7) . . ? C48 C46 C47 106.9(7) . . ? C36 C46 C47 111.6(7) . . ? C49 C46 C47 107.0(7) . . ? C51 C50 C53 109.4(7) . . ? C51 C50 C52 109.6(7) . . ? C53 C50 C52 109.4(7) . . ? C51 C50 C43 107.7(7) . . ? C53 C50 C43 112.5(7) . . ? C52 C50 C43 108.2(7) . . ? C59 C54 C55 116.1(7) . . ? C59 C54 Ge1 126.2(6) . . ? C55 C54 Ge1 117.7(6) . . ? C56 C55 C54 120.9(7) . . ? C56 C55 C60 116.9(7) . . ? C54 C55 C60 122.2(7) . . ? C57 C56 C55 122.3(7) . . ? C56 C57 C58 117.6(7) . . ? C56 C57 C61 121.3(8) . . ? C58 C57 C61 121.2(8) . . ? C59 C58 C57 121.7(8) . . ? C58 C59 C54 121.5(7) . . ? C58 C59 C62 114.8(7) . . ? C54 C59 C62 123.6(7) . . ? C64 C63 C68 117.3(7) . . ? C64 C63 Ge1 126.6(5) . . ? C68 C63 Ge1 116.0(5) . . ? C65 C64 C63 121.1(7) . . ? C65 C64 C69 114.8(7) . . ? C63 C64 C69 124.1(7) . . ? C66 C65 C64 122.3(8) . . ? C67 C66 C65 117.1(8) . . ? C67 C66 C70 121.7(8) . . ? C65 C66 C70 121.3(8) . . ? C66 C67 C68 123.0(8) . . ? C67 C68 C63 119.2(7) . . ? C67 C68 C71 117.3(7) . . ? C63 C68 C71 123.5(7) . . ? C73 C72 C77 118.4(7) . . ? C73 C72 Ge2 126.1(6) . . ? C77 C72 Ge2 115.4(6) . . ? C72 C73 C74 121.3(7) . . ? C72 C73 C78 123.5(7) . . ? C74 C73 C78 115.1(7) . . ? C75 C74 C73 121.2(8) . . ? C74 C75 C76 117.8(8) . . ? C74 C75 C79 120.1(8) . . ? C76 C75 C79 122.1(7) . . ? C75 C76 C77 122.2(8) . . ? C76 C77 C72 119.0(7) . . ? C76 C77 C80 116.2(7) . . ? C72 C77 C80 124.8(7) . . ? C86 C81 C82 117.4(7) . . ? C86 C81 Ge2 125.5(6) . . ? C82 C81 Ge2 117.1(6) . . ? C83 C82 C81 120.0(8) . . ? C83 C82 C87 117.5(7) . . ? C81 C82 C87 122.5(7) . . ? C84 C83 C82 122.3(8) . . ? C83 C84 C85 118.5(8) . . ? C83 C84 C88 122.4(8) . . ? C85 C84 C88 119.0(9) . . ? C84 C85 C86 121.6(8) . . ? C85 C86 C81 120.2(7) . . ? C85 C86 C89 116.2(8) . . ? C81 C86 C89 123.7(7) . . ? C90 C91 C92 130.3(17) . . ? C93 C92 C91 130.0(15) . . ? C92 C93 C94 115.5(11) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.521 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.078 _vrf_PLAT026_12 ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 29 Perc. RESPONSE: We obtained only small weak diffracting crystals. ; _vrf_PLAT213_12 ; PROBLEM: Atom C2 has ADP max/min Ratio ..... 9.80 oblat RESPONSE: This is due to the poor quality of the data. ; _vrf_PLAT360_12 ; PROBLEM: Short C(sp3)-C(sp3) Bond C90 - C91 ... 1.23 Ang. RESPONSE: These atoms take part of a a disordered non coordinating pentane molecule. ; _vrf_PLAT223_12 ; PROBLEM: Large Solvent/Anion H Ueq(max)/Ueq(min) ... 5.04 Ratio RESPONSE: These atoms take part of a a disordered non coordinating pentane molecule. ; _vrf_PLAT761_12 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen atoms have been refined by the use of a riding model. ; _vrf_PLAT762_12 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen atoms have been refined by the use of a riding model. ; #===END