# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Heinz Gornitzka' _publ_contact_author_email HEINZ.GORNITZKA@LCC-TOULOUSE.FR _publ_section_title ; An Isolable o-Quinodimethane and its Fixation of Molecular Oxygen to give an Endoperoxide ; loop_ _publ_author_name 'Heinz Gornitzka' 'Sakina Ech-Cherif El Kettani' 'Jean Escudie' 'Dumitru Ghereg' 'Mohamed Lazraq' ; H.Ranaivonjatovo ; 'Wolfgang Schoeller' #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 713321' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H98 Ge2 O6' _chemical_formula_weight 1396.84 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 14.7436(10) _cell_length_b 17.0689(11) _cell_length_c 17.6474(11) _cell_angle_alpha 67.0840(10) _cell_angle_beta 66.9350(10) _cell_angle_gamma 67.8440(10) _cell_volume 3629.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7465 _cell_measurement_theta_min 2.304 _cell_measurement_theta_max 26.300 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.574095 _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' _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 21106 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0767 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14464 _reflns_number_gt 9177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.2391P] 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 14464 _refine_ls_number_parameters 1061 _refine_ls_number_restraints 1216 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.040 _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 0.76945(3) 0.00424(2) 0.27863(2) 0.02972(11) Uani 1 1 d . . . Ge2 Ge 0.77099(3) 0.35374(2) -0.17174(2) 0.02893(11) Uani 1 1 d . . . O1 O 0.86432(18) 0.01139(15) 0.17495(14) 0.0334(6) Uani 1 1 d . . . O2 O 0.7983(2) 0.23521(15) -0.13230(14) 0.0354(6) Uani 1 1 d . . . C1 C 0.8416(3) 0.0686(2) 0.10079(19) 0.0269(7) Uani 1 1 d . . . C2 C 0.8720(3) 0.0371(2) 0.0313(2) 0.0319(8) Uani 1 1 d . . . H2 H 0.9035 -0.0238 0.0363 0.038 Uiso 1 1 calc R . . C3 C 0.8562(3) 0.0950(2) -0.0458(2) 0.0312(8) Uani 1 1 d . . . H3 H 0.8787 0.0739 -0.0943 0.037 Uiso 1 1 calc R . . C4 C 0.8080(3) 0.1835(2) -0.0530(2) 0.0285(8) Uani 1 1 d . . . C5 C 0.7728(3) 0.2161(2) 0.0183(2) 0.0267(7) Uani 1 1 d . . . C6 C 0.7166(3) 0.3125(2) 0.0091(2) 0.0310(8) Uani 1 1 d . . . H6 H 0.6511 0.3218 -0.0019 0.037 Uiso 1 1 calc R . . C7 C 0.6877(3) 0.3368(2) 0.0903(2) 0.0349(9) Uani 1 1 d . . . H7 H 0.6536 0.3967 0.0893 0.042 Uiso 1 1 calc R . . C8 C 0.7059(3) 0.2817(2) 0.1625(2) 0.0344(9) Uani 1 1 d . . . H8 H 0.6852 0.3049 0.2094 0.041 Uiso 1 1 calc R . . C9 C 0.7569(3) 0.1848(2) 0.1765(2) 0.0296(8) Uani 1 1 d . . . H9 H 0.8191 0.1718 0.1939 0.036 Uiso 1 1 calc R . . C10 C 0.7911(3) 0.1578(2) 0.0955(2) 0.0278(8) Uani 1 1 d . . . C11 C 0.6823(3) 0.1301(2) 0.2537(2) 0.0286(8) Uani 1 1 d . . . C12 C 0.5864(3) 0.1453(2) 0.2320(2) 0.0327(8) Uani 1 1 d . . . C13 C 0.5739(3) 0.1248(2) 0.1684(2) 0.0364(9) Uani 1 1 d . . . H13 H 0.6313 0.0969 0.1299 0.044 Uiso 1 1 calc R . . C14 C 0.4765(3) 0.1457(3) 0.1623(3) 0.0486(11) Uani 1 1 d . . . H14 H 0.4672 0.1315 0.1193 0.058 Uiso 1 1 calc R . . C15 C 0.3916(3) 0.1872(3) 0.2178(3) 0.0545(12) Uani 1 1 d . . . H15 H 0.3254 0.2011 0.2122 0.065 Uiso 1 1 calc R . . C16 C 0.4032(3) 0.2079(3) 0.2804(3) 0.0513(12) Uani 1 1 d . . . H16 H 0.3452 0.2363 0.3182 0.062 Uiso 1 1 calc R . . C17 C 0.5003(3) 0.1870(2) 0.2885(2) 0.0378(9) Uani 1 1 d . . . C18 C 0.5342(3) 0.2000(2) 0.3486(2) 0.0392(10) Uani 1 1 d . . . C19 C 0.4798(4) 0.2415(2) 0.4137(3) 0.0567(13) Uani 1 1 d . . . H19 H 0.4074 0.2632 0.4274 0.068 Uiso 1 1 calc R . . C20 C 0.5329(5) 0.2503(3) 0.4576(3) 0.0665(16) Uani 1 1 d . . . H20 H 0.4970 0.2801 0.5008 0.080 Uiso 1 1 calc R . . C21 C 0.6376(5) 0.2167(3) 0.4398(3) 0.0608(14) Uani 1 1 d . . . H21 H 0.6724 0.2229 0.4716 0.073 Uiso 1 1 calc R . . C22 C 0.6935(4) 0.1733(2) 0.3758(2) 0.0452(10) Uani 1 1 d . . . H22 H 0.7655 0.1499 0.3639 0.054 Uiso 1 1 calc R . . C23 C 0.6404(3) 0.1657(2) 0.3305(2) 0.0354(9) Uani 1 1 d . . . C24 C 0.8479(3) -0.0280(2) 0.3599(2) 0.0337(8) Uani 1 1 d . . . C25 C 0.9496(3) -0.0236(3) 0.3344(2) 0.0410(9) Uani 1 1 d . . . C26 C 1.0024(4) -0.0598(3) 0.3953(3) 0.0496(11) Uani 1 1 d . . . H26 H 1.0711 -0.0570 0.3772 0.060 Uiso 1 1 calc R . . C27 C 0.9609(4) -0.0995(3) 0.4803(3) 0.0499(11) Uani 1 1 d . . . C28 C 0.8607(4) -0.1007(3) 0.5051(2) 0.0476(11) Uani 1 1 d . . . H28 H 0.8294 -0.1260 0.5639 0.057 Uiso 1 1 calc R . . C29 C 0.8028(3) -0.0662(2) 0.4472(2) 0.0392(9) Uani 1 1 d . . . C30 C 1.0075(3) 0.0179(4) 0.2441(3) 0.0613(13) Uani 1 1 d . . . H30A H 1.0708 0.0238 0.2448 0.092 Uiso 1 1 calc R . . H30B H 0.9652 0.0764 0.2214 0.092 Uiso 1 1 calc R . . H30C H 1.0242 -0.0194 0.2076 0.092 Uiso 1 1 calc R . . C31 C 1.0231(5) -0.1393(4) 0.5439(3) 0.0769(16) Uani 1 1 d . . . H31A H 0.9768 -0.1459 0.6025 0.115 Uiso 1 1 calc R . . H31B H 1.0646 -0.1005 0.5324 0.115 Uiso 1 1 calc R . . H31C H 1.0679 -0.1973 0.5380 0.115 Uiso 1 1 calc R . . C32 C 0.6929(3) -0.0694(3) 0.4811(2) 0.0505(11) Uani 1 1 d . . . H32A H 0.6495 -0.0112 0.4593 0.076 Uiso 1 1 calc R . . H32B H 0.6721 -0.0861 0.5440 0.076 Uiso 1 1 calc R . . H32C H 0.6856 -0.1130 0.4621 0.076 Uiso 1 1 calc R . . C33 C 0.7204(3) -0.0950(2) 0.2947(2) 0.0324(8) Uani 1 1 d . . . C34 C 0.7970(3) -0.1699(2) 0.2709(2) 0.0380(9) Uani 1 1 d . . . C35 C 0.7672(4) -0.2396(3) 0.2757(3) 0.0495(11) Uani 1 1 d . . . H35 H 0.8185 -0.2894 0.2602 0.059 Uiso 1 1 calc R . . C36 C 0.6657(4) -0.2400(3) 0.3021(3) 0.0541(12) Uani 1 1 d . . . C37 C 0.5923(3) -0.1681(3) 0.3281(3) 0.0477(10) Uani 1 1 d . . . H37 H 0.5222 -0.1675 0.3474 0.057 Uiso 1 1 calc R . . C38 C 0.6179(3) -0.0974(2) 0.3268(2) 0.0355(9) Uani 1 1 d . . . C39 C 0.9103(3) -0.1785(3) 0.2430(3) 0.0455(10) Uani 1 1 d . . . H39A H 0.9480 -0.2408 0.2506 0.068 Uiso 1 1 calc R . . H39B H 0.9251 -0.1547 0.2780 0.068 Uiso 1 1 calc R . . H39C H 0.9314 -0.1455 0.1824 0.068 Uiso 1 1 calc R . . C40 C 0.6340(5) -0.3155(4) 0.3036(4) 0.0851(18) Uani 1 1 d . . . H40A H 0.6133 -0.2996 0.2519 0.128 Uiso 1 1 calc R . . H40B H 0.5765 -0.3272 0.3547 0.128 Uiso 1 1 calc R . . H40C H 0.6917 -0.3684 0.3051 0.128 Uiso 1 1 calc R . . C41 C 0.5319(3) -0.0286(2) 0.3657(2) 0.0428(10) Uani 1 1 d . . . H41A H 0.4852 0.0031 0.3298 0.064 Uiso 1 1 calc R . . H41B H 0.5601 0.0131 0.3691 0.064 Uiso 1 1 calc R . . H41C H 0.4944 -0.0575 0.4235 0.064 Uiso 1 1 calc R . . C42 C 0.7759(3) 0.3773(2) -0.0705(2) 0.0296(8) Uani 1 1 d . . . C43 C 0.8825(3) 0.3636(2) -0.0682(2) 0.0345(9) Uani 1 1 d . . . C44 C 0.9678(3) 0.2922(3) -0.0754(2) 0.0410(9) Uani 1 1 d . . . H44 H 0.9637 0.2398 -0.0794 0.049 Uiso 1 1 calc R . . C45 C 1.0590(3) 0.2989(3) -0.0766(3) 0.0536(11) Uani 1 1 d . . . H45 H 1.1178 0.2502 -0.0810 0.064 Uiso 1 1 calc R . . C46 C 1.0664(4) 0.3751(4) -0.0715(3) 0.0641(14) Uani 1 1 d . . . H46 H 1.1301 0.3785 -0.0734 0.077 Uiso 1 1 calc R . . C47 C 0.9814(4) 0.4467(3) -0.0638(3) 0.0522(11) Uani 1 1 d . . . H47 H 0.9861 0.4988 -0.0597 0.063 Uiso 1 1 calc R . . C48 C 0.8902(3) 0.4407(3) -0.0621(2) 0.0406(10) Uani 1 1 d . . . C49 C 0.7921(3) 0.5065(2) -0.0596(2) 0.0384(9) Uani 1 1 d . . . C50 C 0.7592(4) 0.5918(3) -0.0507(2) 0.0503(12) Uani 1 1 d . . . H50 H 0.8044 0.6152 -0.0449 0.060 Uiso 1 1 calc R . . C51 C 0.6610(4) 0.6410(3) -0.0506(3) 0.0539(12) Uani 1 1 d . . . H51 H 0.6385 0.6990 -0.0452 0.065 Uiso 1 1 calc R . . C52 C 0.5947(4) 0.6068(3) -0.0583(2) 0.0488(11) Uani 1 1 d . . . H52 H 0.5272 0.6420 -0.0585 0.059 Uiso 1 1 calc R . . C53 C 0.6251(3) 0.5221(2) -0.0656(2) 0.0378(9) Uani 1 1 d . . . H53 H 0.5785 0.4985 -0.0694 0.045 Uiso 1 1 calc R . . C54 C 0.7246(3) 0.4724(2) -0.0674(2) 0.0335(9) Uani 1 1 d . . . C55 C 0.6321(3) 0.3976(2) -0.1838(2) 0.0318(8) Uani 1 1 d . . . C56 C 0.5614(3) 0.3458(2) -0.1480(2) 0.0357(9) Uani 1 1 d . . . C57 C 0.4656(3) 0.3835(3) -0.1626(3) 0.0451(10) Uani 1 1 d . . . H57 H 0.4193 0.3480 -0.1397 0.054 Uiso 1 1 calc R . . C58 C 0.4351(3) 0.4709(3) -0.2092(3) 0.0469(10) Uani 1 1 d . . . C59 C 0.5043(3) 0.5207(3) -0.2435(3) 0.0436(10) Uani 1 1 d . . . H59 H 0.4852 0.5804 -0.2760 0.052 Uiso 1 1 calc R . . C60 C 0.6016(3) 0.4860(2) -0.2321(2) 0.0344(9) Uani 1 1 d . . . C61 C 0.5826(3) 0.2508(2) -0.0955(2) 0.0426(10) Uani 1 1 d . . . H61A H 0.6416 0.2155 -0.1297 0.064 Uiso 1 1 calc R . . H61B H 0.5226 0.2291 -0.0786 0.064 Uiso 1 1 calc R . . H61C H 0.5972 0.2457 -0.0439 0.064 Uiso 1 1 calc R . . C62 C 0.3290(4) 0.5096(4) -0.2203(4) 0.0731(15) Uani 1 1 d . . . H62A H 0.2822 0.5340 -0.1725 0.110 Uiso 1 1 calc R . . H62B H 0.3055 0.4633 -0.2209 0.110 Uiso 1 1 calc R . . H62C H 0.3304 0.5565 -0.2746 0.110 Uiso 1 1 calc R . . C63 C 0.6729(3) 0.5457(2) -0.2749(2) 0.0440(10) Uani 1 1 d . . . H63A H 0.7010 0.5449 -0.2326 0.066 Uiso 1 1 calc R . . H63B H 0.6348 0.6061 -0.2983 0.066 Uiso 1 1 calc R . . H63C H 0.7287 0.5248 -0.3216 0.066 Uiso 1 1 calc R . . C64 C 0.8761(3) 0.3657(2) -0.2838(2) 0.0296(8) Uani 1 1 d . . . C65 C 0.8866(3) 0.3137(2) -0.3338(2) 0.0348(9) Uani 1 1 d . . . C66 C 0.9679(3) 0.3111(3) -0.4089(2) 0.0425(10) Uani 1 1 d . . . H66 H 0.9750 0.2752 -0.4418 0.051 Uiso 1 1 calc R . . C67 C 1.0381(3) 0.3588(3) -0.4367(2) 0.0484(11) Uani 1 1 d . . . C68 C 1.0239(3) 0.4132(3) -0.3899(2) 0.0444(10) Uani 1 1 d . . . H68 H 1.0697 0.4487 -0.4098 0.053 Uiso 1 1 calc R . . C69 C 0.9445(3) 0.4176(2) -0.3142(2) 0.0356(9) Uani 1 1 d . . . C70 C 0.8155(3) 0.2585(3) -0.3099(2) 0.0449(10) Uani 1 1 d . . . H70A H 0.8361 0.2022 -0.2683 0.067 Uiso 1 1 calc R . . H70B H 0.8184 0.2474 -0.3615 0.067 Uiso 1 1 calc R . . H70C H 0.7455 0.2898 -0.2844 0.067 Uiso 1 1 calc R . . C71 C 1.1286(4) 0.3502(3) -0.5156(3) 0.0685(15) Uani 1 1 d . . . H71A H 1.1915 0.3190 -0.4982 0.103 Uiso 1 1 calc R . . H71B H 1.1334 0.4091 -0.5541 0.103 Uiso 1 1 calc R . . H71C H 1.1196 0.3171 -0.5455 0.103 Uiso 1 1 calc R . . C72 C 0.9383(3) 0.4789(3) -0.2689(2) 0.0480(11) Uani 1 1 d . . . H72A H 0.8696 0.4923 -0.2295 0.072 Uiso 1 1 calc R . . H72B H 0.9528 0.5337 -0.3113 0.072 Uiso 1 1 calc R . . H72C H 0.9886 0.4507 -0.2363 0.072 Uiso 1 1 calc R . . O3 O -0.0528(11) 0.3550(10) 0.2547(9) 0.139(5) Uani 0.600(11) 1 d PDU A 1 C73 C 0.0618(11) 0.3207(9) 0.2446(12) 0.098(5) Uani 0.600(11) 1 d PDU A 1 H73A H 0.0973 0.3649 0.1995 0.118 Uiso 0.600(11) 1 calc PR A 1 H73B H 0.0747 0.3102 0.2992 0.118 Uiso 0.600(11) 1 calc PR A 1 C74 C 0.0995(7) 0.2400(6) 0.2214(7) 0.071(3) Uani 0.600(11) 1 d PDU A 1 H74A H 0.1716 0.2320 0.1856 0.085 Uiso 0.600(11) 1 calc PR A 1 H74B H 0.0942 0.1886 0.2731 0.085 Uiso 0.600(11) 1 calc PR A 1 C75 C 0.0360(12) 0.2508(12) 0.1753(12) 0.130(5) Uani 0.600(11) 1 d PDU A 1 H75A H 0.0283 0.1926 0.1837 0.156 Uiso 0.600(11) 1 calc PR A 1 H75B H 0.0678 0.2754 0.1134 0.156 Uiso 0.600(11) 1 calc PR A 1 C76 C -0.0628(13) 0.3085(13) 0.2015(15) 0.138(6) Uani 0.600(11) 1 d PDU A 1 H76A H -0.1142 0.2744 0.2362 0.166 Uiso 0.600(11) 1 calc PR A 1 H76B H -0.0842 0.3520 0.1508 0.166 Uiso 0.600(11) 1 calc PR A 1 O3' O -0.052(2) 0.333(2) 0.2776(17) 0.219(13) Uani 0.400(11) 1 d PDU A 2 C73' C 0.0611(17) 0.2986(19) 0.2305(13) 0.110(7) Uani 0.400(11) 1 d PDU A 2 H73C H 0.1028 0.3357 0.2247 0.132 Uiso 0.400(11) 1 calc PR A 2 H73D H 0.0897 0.2368 0.2609 0.132 Uiso 0.400(11) 1 calc PR A 2 C74' C 0.0568(10) 0.3053(11) 0.1476(8) 0.068(4) Uani 0.400(11) 1 d PDU A 2 H74C H 0.0624 0.3643 0.1076 0.082 Uiso 0.400(11) 1 calc PR A 2 H74D H 0.1145 0.2602 0.1231 0.082 Uiso 0.400(11) 1 calc PR A 2 C75' C -0.0391(13) 0.2921(15) 0.1580(10) 0.089(6) Uani 0.400(11) 1 d PDU A 2 H75C H -0.0277 0.2374 0.1446 0.106 Uiso 0.400(11) 1 calc PR A 2 H75D H -0.0770 0.3426 0.1202 0.106 Uiso 0.400(11) 1 calc PR A 2 C76' C -0.0951(13) 0.2854(15) 0.2488(10) 0.094(6) Uani 0.400(11) 1 d PDU A 2 H76C H -0.0854 0.2228 0.2833 0.113 Uiso 0.400(11) 1 calc PR A 2 H76D H -0.1691 0.3129 0.2557 0.113 Uiso 0.400(11) 1 calc PR A 2 O4 O 0.6420(9) 0.3810(8) 0.5220(8) 0.153(5) Uani 0.629(16) 1 d PDU B 1 C77 C 0.7502(11) 0.3696(10) 0.4737(10) 0.113(5) Uani 0.629(16) 1 d PDU B 1 H77A H 0.7942 0.3240 0.5094 0.136 Uiso 0.629(16) 1 calc PR B 1 H77B H 0.7652 0.3529 0.4214 0.136 Uiso 0.629(16) 1 calc PR B 1 C78 C 0.7649(16) 0.4559(13) 0.4520(15) 0.146(8) Uani 0.629(16) 1 d PDU B 1 H78A H 0.8378 0.4520 0.4397 0.175 Uiso 0.629(16) 1 calc PR B 1 H78B H 0.7412 0.4967 0.4015 0.175 Uiso 0.629(16) 1 calc PR B 1 C79 C 0.7032(15) 0.4848(11) 0.5281(11) 0.121(6) Uani 0.629(16) 1 d PDU B 1 H79A H 0.7444 0.4663 0.5679 0.146 Uiso 0.629(16) 1 calc PR B 1 H79B H 0.6774 0.5499 0.5124 0.146 Uiso 0.629(16) 1 calc PR B 1 C80 C 0.6189(12) 0.4451(11) 0.5687(9) 0.118(5) Uani 0.629(16) 1 d PDU B 1 H80A H 0.5537 0.4903 0.5638 0.142 Uiso 0.629(16) 1 calc PR B 1 H80B H 0.6137 0.4148 0.6303 0.142 Uiso 0.629(16) 1 calc PR B 1 O4' O 0.699(2) 0.4073(18) 0.4494(17) 0.179(8) Uani 0.371(16) 1 d PDU B 2 C77' C 0.613(2) 0.431(3) 0.525(3) 0.212(16) Uani 0.371(16) 1 d PDU B 2 H77C H 0.5465 0.4385 0.5189 0.254 Uiso 0.371(16) 1 calc PR B 2 H77D H 0.6213 0.3839 0.5793 0.254 Uiso 0.371(16) 1 calc PR B 2 C78' C 0.6212(15) 0.5124(17) 0.5258(17) 0.115(8) Uani 0.371(16) 1 d PDU B 2 H78C H 0.5946 0.5181 0.5848 0.138 Uiso 0.371(16) 1 calc PR B 2 H78D H 0.5824 0.5636 0.4892 0.138 Uiso 0.371(16) 1 calc PR B 2 C79' C 0.7298(18) 0.5064(19) 0.491(2) 0.124(9) Uani 0.371(16) 1 d PDU B 2 H79C H 0.7412 0.5619 0.4468 0.149 Uiso 0.371(16) 1 calc PR B 2 H79D H 0.7578 0.4973 0.5377 0.149 Uiso 0.371(16) 1 calc PR B 2 C80' C 0.7808(16) 0.433(2) 0.455(2) 0.109(7) Uani 0.371(16) 1 d PDU B 2 H80C H 0.8206 0.3838 0.4915 0.131 Uiso 0.371(16) 1 calc PR B 2 H80D H 0.8279 0.4515 0.3969 0.131 Uiso 0.371(16) 1 calc PR B 2 O5 O 0.7030(9) 0.1405(8) 0.6362(7) 0.092(3) Uani 0.659(12) 1 d PDU C 1 C81 C 0.7252(14) 0.0613(8) 0.6135(7) 0.063(3) Uani 0.659(12) 1 d PDU C 1 H81A H 0.7922 0.0518 0.5696 0.076 Uiso 0.659(12) 1 calc PR C 1 H81B H 0.6718 0.0648 0.5907 0.076 Uiso 0.659(12) 1 calc PR C 1 C82 C 0.7267(9) -0.0114(6) 0.6951(6) 0.069(3) Uani 0.659(12) 1 d PDU C 1 H82A H 0.7945 -0.0327 0.7054 0.083 Uiso 0.659(12) 1 calc PR C 1 H82B H 0.7085 -0.0615 0.6949 0.083 Uiso 0.659(12) 1 calc PR C 1 C83 C 0.6466(9) 0.0332(7) 0.7605(6) 0.089(4) Uani 0.659(12) 1 d PDU C 1 H83A H 0.5776 0.0323 0.7657 0.107 Uiso 0.659(12) 1 calc PR C 1 H83B H 0.6594 0.0041 0.8174 0.107 Uiso 0.659(12) 1 calc PR C 1 C84 C 0.6559(15) 0.1217(8) 0.7281(9) 0.103(5) Uani 0.659(12) 1 d PDU C 1 H84A H 0.6985 0.1281 0.7558 0.123 Uiso 0.659(12) 1 calc PR C 1 H84B H 0.5876 0.1635 0.7408 0.123 Uiso 0.659(12) 1 calc PR C 1 O5' O 0.6547(16) 0.1550(15) 0.6405(12) 0.092(6) Uani 0.341(12) 1 d PDU C 2 C81' C 0.6277(19) 0.1565(13) 0.7290(14) 0.075(6) Uani 0.341(12) 1 d PDU C 2 H81C H 0.5536 0.1623 0.7566 0.090 Uiso 0.341(12) 1 calc PR C 2 H81D H 0.6436 0.2074 0.7298 0.090 Uiso 0.341(12) 1 calc PR C 2 C82' C 0.6862(14) 0.0743(12) 0.7757(11) 0.082(6) Uani 0.341(12) 1 d PDU C 2 H82C H 0.6431 0.0524 0.8345 0.098 Uiso 0.341(12) 1 calc PR C 2 H82D H 0.7460 0.0839 0.7800 0.098 Uiso 0.341(12) 1 calc PR C 2 C83' C 0.720(2) 0.0108(13) 0.7273(15) 0.109(8) Uani 0.341(12) 1 d PDU C 2 H83C H 0.6716 -0.0262 0.7504 0.131 Uiso 0.341(12) 1 calc PR C 2 H83D H 0.7888 -0.0279 0.7296 0.131 Uiso 0.341(12) 1 calc PR C 2 C84' C 0.720(3) 0.0654(18) 0.6391(14) 0.081(7) Uani 0.341(12) 1 d PDU C 2 H84C H 0.6950 0.0391 0.6129 0.097 Uiso 0.341(12) 1 calc PR C 2 H84D H 0.7911 0.0681 0.6041 0.097 Uiso 0.341(12) 1 calc PR C 2 O6 O 0.6695(14) 0.8130(10) 0.0442(13) 0.142(7) Uani 0.398(13) 1 d PDU D 1 C85 C 0.714(2) 0.8549(18) -0.0481(13) 0.096(7) Uani 0.398(13) 1 d PDU D 1 H85A H 0.7690 0.8116 -0.0767 0.115 Uiso 0.398(13) 1 calc PR D 1 H85B H 0.6607 0.8845 -0.0789 0.115 Uiso 0.398(13) 1 calc PR D 1 C86 C 0.753(2) 0.919(2) -0.042(2) 0.109(9) Uani 0.398(13) 1 d PDU D 1 H86A H 0.7684 0.9640 -0.0978 0.131 Uiso 0.398(13) 1 calc PR D 1 H86B H 0.8157 0.8892 -0.0229 0.131 Uiso 0.398(13) 1 calc PR D 1 C87 C 0.669(2) 0.9593(15) 0.0229(17) 0.121(8) Uani 0.398(13) 1 d PDU D 1 H87A H 0.6936 0.9588 0.0677 0.145 Uiso 0.398(13) 1 calc PR D 1 H87B H 0.6347 1.0208 -0.0040 0.145 Uiso 0.398(13) 1 calc PR D 1 C88 C 0.600(2) 0.9039(16) 0.059(2) 0.188(14) Uani 0.398(13) 1 d PDU D 1 H88A H 0.5465 0.9281 0.0286 0.226 Uiso 0.398(13) 1 calc PR D 1 H88B H 0.5664 0.8984 0.1206 0.226 Uiso 0.398(13) 1 calc PR D 1 O6' O 0.6209(6) 0.8628(7) -0.0065(5) 0.089(3) Uani 0.602(13) 1 d PDU D 2 C85' C 0.7326(11) 0.8372(13) -0.0325(12) 0.104(6) Uani 0.602(13) 1 d PDU D 2 H85C H 0.7605 0.8346 -0.0927 0.125 Uiso 0.602(13) 1 calc PR D 2 H85D H 0.7592 0.7789 0.0052 0.125 Uiso 0.602(13) 1 calc PR D 2 C86' C 0.7593(14) 0.9073(14) -0.0231(13) 0.096(5) Uani 0.602(13) 1 d PDU D 2 H86C H 0.7505 0.9619 -0.0709 0.116 Uiso 0.602(13) 1 calc PR D 2 H86D H 0.8304 0.8881 -0.0202 0.116 Uiso 0.602(13) 1 calc PR D 2 C87' C 0.6847(14) 0.9203(12) 0.0596(11) 0.104(5) Uani 0.602(13) 1 d PDU D 2 H87C H 0.7193 0.8982 0.1048 0.125 Uiso 0.602(13) 1 calc PR D 2 H87D H 0.6487 0.9835 0.0535 0.125 Uiso 0.602(13) 1 calc PR D 2 C88' C 0.6136(15) 0.8697(16) 0.0802(10) 0.164(7) Uani 0.602(13) 1 d PDU D 2 H88C H 0.5432 0.9002 0.1078 0.197 Uiso 0.602(13) 1 calc PR D 2 H88D H 0.6333 0.8104 0.1195 0.197 Uiso 0.602(13) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0302(2) 0.0278(2) 0.02330(19) -0.00652(15) -0.00348(15) -0.00458(16) Ge2 0.0351(2) 0.0264(2) 0.02178(18) -0.00736(15) -0.00474(15) -0.00755(16) O1 0.0299(14) 0.0332(14) 0.0232(12) -0.0060(10) -0.0031(10) -0.0007(11) O2 0.0555(17) 0.0239(12) 0.0233(12) -0.0059(10) -0.0098(11) -0.0091(11) C1 0.0241(18) 0.0304(18) 0.0171(15) -0.0033(13) -0.0002(13) -0.0072(14) C2 0.030(2) 0.0252(18) 0.0330(19) -0.0115(15) -0.0029(15) -0.0025(15) C3 0.034(2) 0.033(2) 0.0240(17) -0.0132(15) -0.0025(15) -0.0073(16) C4 0.031(2) 0.0275(18) 0.0226(16) -0.0067(14) -0.0033(14) -0.0082(15) C5 0.0281(19) 0.0241(17) 0.0253(16) -0.0074(14) -0.0023(14) -0.0095(14) C6 0.037(2) 0.0266(18) 0.0275(17) -0.0122(14) -0.0030(15) -0.0078(15) C7 0.048(2) 0.0256(18) 0.0256(18) -0.0112(15) 0.0018(16) -0.0129(16) C8 0.048(2) 0.0311(19) 0.0224(17) -0.0106(15) 0.0009(16) -0.0164(17) C9 0.033(2) 0.0282(18) 0.0238(17) -0.0051(14) -0.0023(15) -0.0126(15) C10 0.0269(19) 0.0298(18) 0.0234(16) -0.0081(14) 0.0000(14) -0.0110(15) C11 0.035(2) 0.0211(17) 0.0213(16) -0.0054(13) -0.0013(14) -0.0067(15) C12 0.031(2) 0.0207(17) 0.0331(19) -0.0011(14) -0.0033(16) -0.0064(15) C13 0.036(2) 0.033(2) 0.036(2) -0.0050(16) -0.0074(17) -0.0138(17) C14 0.046(3) 0.043(2) 0.053(3) -0.002(2) -0.017(2) -0.018(2) C15 0.035(3) 0.044(3) 0.066(3) 0.001(2) -0.013(2) -0.010(2) C16 0.031(2) 0.034(2) 0.056(3) -0.0007(19) 0.002(2) -0.0008(17) C17 0.036(2) 0.0223(19) 0.034(2) -0.0016(15) 0.0027(17) -0.0066(16) C18 0.050(3) 0.0193(17) 0.0285(18) -0.0035(14) 0.0049(17) -0.0081(16) C19 0.073(3) 0.028(2) 0.035(2) -0.0073(17) 0.011(2) -0.006(2) C20 0.107(5) 0.036(2) 0.028(2) -0.0143(19) 0.002(3) -0.007(3) C21 0.110(5) 0.040(2) 0.033(2) -0.0092(19) -0.022(3) -0.021(3) C22 0.070(3) 0.032(2) 0.0297(19) -0.0073(16) -0.0124(19) -0.012(2) C23 0.050(2) 0.0216(18) 0.0235(17) -0.0036(14) -0.0023(16) -0.0094(16) C24 0.038(2) 0.0305(19) 0.0276(18) -0.0098(15) -0.0102(16) -0.0014(16) C25 0.042(2) 0.046(2) 0.035(2) -0.0160(18) -0.0102(18) -0.0084(19) C26 0.049(3) 0.050(3) 0.055(3) -0.018(2) -0.020(2) -0.010(2) C27 0.067(3) 0.041(2) 0.047(2) -0.0110(19) -0.029(2) -0.008(2) C28 0.067(3) 0.041(2) 0.030(2) -0.0067(17) -0.015(2) -0.011(2) C29 0.049(3) 0.032(2) 0.0304(19) -0.0110(16) -0.0081(17) -0.0053(17) C30 0.042(3) 0.098(4) 0.044(2) -0.015(2) -0.009(2) -0.029(3) C31 0.096(4) 0.082(4) 0.062(3) -0.004(3) -0.048(3) -0.024(3) C32 0.044(3) 0.065(3) 0.027(2) -0.0106(19) 0.0002(18) -0.013(2) C33 0.041(2) 0.0231(18) 0.0284(18) -0.0087(14) -0.0098(16) -0.0023(15) C34 0.046(2) 0.029(2) 0.0274(18) -0.0073(15) -0.0107(17) 0.0009(17) C35 0.066(3) 0.030(2) 0.043(2) -0.0152(18) -0.011(2) -0.002(2) C36 0.079(4) 0.040(2) 0.047(2) -0.013(2) -0.016(2) -0.022(2) C37 0.051(3) 0.043(2) 0.048(2) -0.0073(19) -0.016(2) -0.015(2) C38 0.040(2) 0.0278(19) 0.0325(19) -0.0028(15) -0.0117(17) -0.0074(16) C39 0.043(2) 0.036(2) 0.045(2) -0.0145(18) -0.0118(19) 0.0050(18) C40 0.116(5) 0.061(3) 0.095(4) -0.035(3) -0.025(4) -0.033(3) C41 0.035(2) 0.034(2) 0.043(2) -0.0030(17) -0.0027(18) -0.0088(17) C42 0.038(2) 0.0294(18) 0.0214(16) -0.0108(14) -0.0035(15) -0.0110(16) C43 0.041(2) 0.042(2) 0.0199(16) -0.0068(15) -0.0039(15) -0.0178(18) C44 0.040(2) 0.047(2) 0.032(2) -0.0106(17) -0.0072(17) -0.0119(19) C45 0.043(3) 0.071(3) 0.043(2) -0.016(2) -0.011(2) -0.014(2) C46 0.055(3) 0.104(4) 0.050(3) -0.020(3) -0.017(2) -0.037(3) C47 0.061(3) 0.071(3) 0.038(2) -0.017(2) -0.013(2) -0.032(3) C48 0.060(3) 0.047(2) 0.0215(17) -0.0083(16) -0.0074(17) -0.027(2) C49 0.056(3) 0.038(2) 0.0226(17) -0.0077(15) -0.0042(17) -0.0221(19) C50 0.085(4) 0.042(2) 0.030(2) -0.0097(18) -0.007(2) -0.035(2) C51 0.082(4) 0.030(2) 0.042(2) -0.0150(18) -0.001(2) -0.018(2) C52 0.059(3) 0.032(2) 0.040(2) -0.0125(18) -0.001(2) -0.008(2) C53 0.043(2) 0.031(2) 0.0313(19) -0.0099(16) 0.0005(17) -0.0125(17) C54 0.051(2) 0.0267(18) 0.0170(16) -0.0050(14) -0.0004(15) -0.0160(17) C55 0.036(2) 0.034(2) 0.0271(17) -0.0145(15) -0.0041(15) -0.0094(16) C56 0.042(2) 0.039(2) 0.0302(19) -0.0175(16) -0.0048(16) -0.0129(18) C57 0.046(3) 0.055(3) 0.046(2) -0.029(2) -0.0075(19) -0.017(2) C58 0.046(3) 0.050(3) 0.055(3) -0.032(2) -0.016(2) -0.004(2) C59 0.046(3) 0.038(2) 0.044(2) -0.0190(18) -0.0141(19) 0.0007(19) C60 0.037(2) 0.035(2) 0.0296(18) -0.0158(16) -0.0050(16) -0.0055(17) C61 0.051(3) 0.041(2) 0.041(2) -0.0124(18) -0.0095(19) -0.0214(19) C62 0.056(3) 0.075(4) 0.107(4) -0.050(3) -0.034(3) -0.001(3) C63 0.048(3) 0.030(2) 0.040(2) -0.0052(17) -0.0097(19) -0.0048(18) C64 0.032(2) 0.0270(18) 0.0212(16) -0.0052(14) -0.0072(14) -0.0016(15) C65 0.038(2) 0.0318(19) 0.0259(18) -0.0062(15) -0.0089(16) -0.0024(16) C66 0.050(3) 0.041(2) 0.0281(19) -0.0138(17) -0.0067(18) -0.0038(19) C67 0.051(3) 0.040(2) 0.031(2) -0.0068(17) -0.0003(19) -0.004(2) C68 0.040(2) 0.045(2) 0.036(2) -0.0059(18) -0.0024(18) -0.0140(19) C69 0.043(2) 0.033(2) 0.0231(17) -0.0019(15) -0.0090(16) -0.0083(17) C70 0.052(3) 0.050(2) 0.036(2) -0.0220(19) -0.0101(19) -0.011(2) C71 0.061(3) 0.075(3) 0.045(3) -0.028(2) 0.016(2) -0.015(3) C72 0.058(3) 0.048(2) 0.036(2) -0.0087(19) -0.004(2) -0.025(2) O3 0.195(10) 0.119(10) 0.112(7) -0.033(7) -0.044(7) -0.051(8) C73 0.106(9) 0.094(9) 0.124(9) -0.059(7) 0.005(7) -0.067(7) C74 0.057(6) 0.047(5) 0.095(7) -0.027(5) -0.008(5) -0.006(4) C75 0.131(12) 0.121(11) 0.156(11) -0.104(9) -0.019(10) -0.008(9) C76 0.160(13) 0.141(12) 0.158(14) -0.054(12) -0.073(11) -0.046(10) O3' 0.209(16) 0.122(14) 0.220(18) -0.010(14) -0.017(15) -0.020(13) C73' 0.096(12) 0.114(14) 0.147(14) -0.025(12) -0.015(11) -0.091(10) C74' 0.072(8) 0.087(9) 0.066(8) -0.053(7) 0.028(6) -0.061(7) C75' 0.089(12) 0.091(11) 0.097(12) -0.033(10) -0.017(10) -0.038(9) C76' 0.106(12) 0.098(12) 0.103(12) 0.010(10) -0.070(10) -0.051(9) O4 0.183(11) 0.146(9) 0.149(8) -0.096(7) -0.008(8) -0.052(8) C77 0.118(11) 0.129(11) 0.114(10) -0.071(9) -0.035(8) -0.014(9) C78 0.138(12) 0.137(13) 0.166(13) -0.044(11) -0.021(11) -0.063(10) C79 0.170(14) 0.125(11) 0.119(12) -0.053(9) -0.081(10) -0.032(10) C80 0.130(10) 0.137(11) 0.095(9) -0.087(8) -0.033(8) 0.012(9) O4' 0.178(16) 0.194(16) 0.168(14) -0.098(12) -0.024(13) -0.029(13) C77' 0.154(18) 0.18(2) 0.20(2) -0.05(2) 0.008(18) -0.010(19) C78' 0.094(13) 0.111(15) 0.123(15) -0.046(12) -0.025(12) -0.004(12) C79' 0.124(15) 0.140(16) 0.119(17) -0.060(14) 0.005(13) -0.062(13) C80' 0.134(15) 0.134(15) 0.115(12) -0.066(11) -0.059(11) -0.036(13) O5 0.127(9) 0.098(6) 0.074(5) -0.016(4) -0.038(6) -0.054(6) C81 0.077(6) 0.082(6) 0.059(6) -0.021(5) -0.033(5) -0.034(5) C82 0.068(6) 0.072(6) 0.078(7) -0.011(5) -0.030(5) -0.028(5) C83 0.109(8) 0.102(8) 0.075(6) 0.003(5) -0.039(6) -0.063(7) C84 0.135(12) 0.117(10) 0.080(8) -0.046(8) -0.018(8) -0.052(10) O5' 0.111(13) 0.127(12) 0.062(8) -0.008(8) -0.022(9) -0.078(11) C81' 0.094(13) 0.111(14) 0.060(10) -0.020(10) -0.037(9) -0.058(11) C82' 0.084(11) 0.110(13) 0.084(11) -0.029(10) -0.041(9) -0.040(10) C83' 0.086(13) 0.096(14) 0.143(18) -0.033(13) 0.001(15) -0.060(12) C84' 0.095(12) 0.116(14) 0.082(14) -0.039(12) -0.028(13) -0.066(11) O6 0.124(12) 0.117(10) 0.172(14) -0.031(10) -0.004(10) -0.069(9) C85 0.101(13) 0.109(14) 0.108(12) -0.020(10) -0.061(10) -0.040(11) C86 0.143(15) 0.097(14) 0.077(11) -0.007(11) -0.051(11) -0.021(12) C87 0.161(16) 0.096(14) 0.116(16) -0.052(12) -0.011(14) -0.050(13) C88 0.149(16) 0.175(17) 0.148(17) -0.037(15) 0.060(14) -0.063(15) O6' 0.074(5) 0.137(8) 0.091(5) -0.054(5) -0.019(4) -0.048(5) C85' 0.110(10) 0.106(10) 0.140(12) -0.058(9) -0.071(8) -0.014(8) C86' 0.111(9) 0.083(9) 0.123(13) -0.004(9) -0.073(8) -0.039(7) C87' 0.138(10) 0.114(11) 0.112(11) -0.043(8) -0.044(9) -0.069(10) C88' 0.180(14) 0.221(15) 0.133(12) -0.120(11) 0.042(10) -0.114(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 1.808(2) . ? Ge1 C33 1.966(4) . ? Ge1 C24 1.975(4) . ? Ge1 C11 2.021(3) . ? Ge2 O2 1.802(2) . ? Ge2 C55 1.964(4) . ? Ge2 C64 1.969(3) . ? Ge2 C42 2.011(3) . ? O1 C1 1.371(4) . ? O2 C4 1.363(4) . ? C1 C2 1.375(5) . ? C1 C10 1.404(4) . ? C2 C3 1.382(5) . ? C3 C4 1.383(5) . ? C4 C5 1.407(4) . ? C5 C10 1.396(5) . ? C5 C6 1.513(4) . ? C6 C7 1.503(4) . ? C6 C42 1.587(5) . ? C7 C8 1.314(5) . ? C8 C9 1.500(5) . ? C9 C10 1.511(4) . ? C9 C11 1.596(4) . ? C11 C12 1.510(5) . ? C11 C23 1.514(4) . ? C12 C13 1.391(5) . ? C12 C17 1.411(5) . ? C13 C14 1.380(6) . ? C14 C15 1.392(6) . ? C15 C16 1.368(7) . ? C16 C17 1.390(6) . ? C17 C18 1.452(6) . ? C18 C19 1.395(5) . ? C18 C23 1.399(5) . ? C19 C20 1.377(7) . ? C20 C21 1.379(7) . ? C21 C22 1.401(5) . ? C22 C23 1.385(6) . ? C24 C29 1.408(5) . ? C24 C25 1.409(5) . ? C25 C26 1.385(6) . ? C25 C30 1.510(6) . ? C26 C27 1.373(6) . ? C27 C28 1.373(6) . ? C27 C31 1.519(6) . ? C28 C29 1.399(6) . ? C29 C32 1.506(6) . ? C33 C38 1.401(5) . ? C33 C34 1.430(5) . ? C34 C35 1.379(6) . ? C34 C39 1.511(6) . ? C35 C36 1.383(6) . ? C36 C37 1.391(6) . ? C36 C40 1.517(6) . ? C37 C38 1.383(5) . ? C38 C41 1.511(5) . ? C42 C43 1.513(5) . ? C42 C54 1.524(5) . ? C43 C44 1.387(5) . ? C43 C48 1.410(5) . ? C44 C45 1.383(6) . ? C45 C46 1.386(7) . ? C46 C47 1.386(7) . ? C47 C48 1.374(6) . ? C48 C49 1.456(6) . ? C49 C54 1.397(5) . ? C49 C50 1.401(5) . ? C50 C51 1.372(6) . ? C51 C52 1.382(6) . ? C52 C53 1.385(5) . ? C53 C54 1.386(5) . ? C55 C60 1.411(5) . ? C55 C56 1.418(5) . ? C56 C57 1.395(5) . ? C56 C61 1.504(5) . ? C57 C58 1.391(6) . ? C58 C59 1.378(6) . ? C58 C62 1.510(6) . ? C59 C60 1.394(5) . ? C60 C63 1.516(5) . ? C64 C69 1.403(5) . ? C64 C65 1.412(5) . ? C65 C66 1.398(5) . ? C65 C70 1.501(6) . ? C66 C67 1.379(6) . ? C67 C68 1.380(6) . ? C67 C71 1.516(5) . ? C68 C69 1.395(5) . ? C69 C72 1.506(5) . ? O3 C76 1.519(12) . ? O3 C73 1.525(12) . ? C73 C74 1.434(11) . ? C74 C75 1.386(12) . ? C75 C76 1.432(12) . ? O3' C76' 1.511(14) . ? O3' C73' 1.545(14) . ? C73' C74' 1.448(14) . ? C74' C75' 1.446(13) . ? C75' C76' 1.467(13) . ? O4 C77 1.462(12) . ? O4 C80 1.481(11) . ? C77 C78 1.450(13) . ? C78 C79 1.447(13) . ? C79 C80 1.441(12) . ? O4' C80' 1.473(15) . ? O4' C77' 1.506(15) . ? C77' C78' 1.446(15) . ? C78' C79' 1.452(14) . ? C79' C80' 1.441(14) . ? O5 C81 1.443(11) . ? O5 C84 1.448(10) . ? C81 C82 1.491(10) . ? C82 C83 1.498(11) . ? C83 C84 1.431(12) . ? O5' C81' 1.461(14) . ? O5' C84' 1.473(14) . ? C81' C82' 1.461(14) . ? C82' C83' 1.462(14) . ? C83' C84' 1.469(14) . ? O6 C85 1.483(15) . ? O6 C88 1.558(15) . ? C85 C86 1.475(14) . ? C86 C87 1.477(14) . ? C87 C88 1.441(14) . ? O6' C85' 1.462(13) . ? O6' C88' 1.539(13) . ? C85' C86' 1.476(11) . ? C86' C87' 1.482(12) . ? C87' C88' 1.455(12) . ? 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 C33 102.53(13) . . ? O1 Ge1 C24 104.50(13) . . ? C33 Ge1 C24 110.65(15) . . ? O1 Ge1 C11 98.28(11) . . ? C33 Ge1 C11 121.76(15) . . ? C24 Ge1 C11 115.59(14) . . ? O2 Ge2 C55 106.94(14) . . ? O2 Ge2 C64 99.63(12) . . ? C55 Ge2 C64 112.14(14) . . ? O2 Ge2 C42 98.44(12) . . ? C55 Ge2 C42 111.83(14) . . ? C64 Ge2 C42 124.38(15) . . ? C1 O1 Ge1 121.9(2) . . ? C4 O2 Ge2 127.4(2) . . ? O1 C1 C2 118.5(3) . . ? O1 C1 C10 120.4(3) . . ? C2 C1 C10 121.0(3) . . ? C1 C2 C3 119.4(3) . . ? C2 C3 C4 120.7(3) . . ? O2 C4 C3 116.0(3) . . ? O2 C4 C5 123.4(3) . . ? C3 C4 C5 120.7(3) . . ? C10 C5 C4 118.4(3) . . ? C10 C5 C6 122.3(3) . . ? C4 C5 C6 119.3(3) . . ? C7 C6 C5 112.3(3) . . ? C7 C6 C42 110.9(3) . . ? C5 C6 C42 113.3(3) . . ? C8 C7 C6 125.0(3) . . ? C7 C8 C9 124.9(3) . . ? C8 C9 C10 112.0(3) . . ? C8 C9 C11 109.6(3) . . ? C10 C9 C11 111.8(3) . . ? C5 C10 C1 119.8(3) . . ? C5 C10 C9 123.4(3) . . ? C1 C10 C9 116.8(3) . . ? C12 C11 C23 102.2(3) . . ? C12 C11 C9 111.1(3) . . ? C23 C11 C9 110.4(3) . . ? C12 C11 Ge1 116.1(2) . . ? C23 C11 Ge1 112.3(2) . . ? C9 C11 Ge1 104.9(2) . . ? C13 C12 C17 119.8(4) . . ? C13 C12 C11 130.2(3) . . ? C17 C12 C11 110.0(3) . . ? C14 C13 C12 118.8(4) . . ? C13 C14 C15 121.3(4) . . ? C16 C15 C14 120.3(4) . . ? C15 C16 C17 119.6(4) . . ? C16 C17 C12 120.2(4) . . ? C16 C17 C18 131.2(4) . . ? C12 C17 C18 108.7(3) . . ? C19 C18 C23 120.4(4) . . ? C19 C18 C17 130.8(4) . . ? C23 C18 C17 108.8(3) . . ? C20 C19 C18 118.7(5) . . ? C19 C20 C21 121.0(4) . . ? C20 C21 C22 121.2(5) . . ? C23 C22 C21 117.9(4) . . ? C22 C23 C18 120.8(3) . . ? C22 C23 C11 128.6(4) . . ? C18 C23 C11 110.3(3) . . ? C29 C24 C25 118.4(3) . . ? C29 C24 Ge1 117.5(3) . . ? C25 C24 Ge1 123.7(3) . . ? C26 C25 C24 118.9(4) . . ? C26 C25 C30 116.1(4) . . ? C24 C25 C30 125.0(3) . . ? C27 C26 C25 123.7(4) . . ? C28 C27 C26 117.0(4) . . ? C28 C27 C31 121.7(4) . . ? C26 C27 C31 121.3(5) . . ? C27 C28 C29 122.6(4) . . ? C28 C29 C24 119.4(4) . . ? C28 C29 C32 118.4(3) . . ? C24 C29 C32 122.2(3) . . ? C38 C33 C34 118.5(3) . . ? C38 C33 Ge1 125.3(3) . . ? C34 C33 Ge1 116.1(3) . . ? C35 C34 C33 119.0(4) . . ? C35 C34 C39 117.5(3) . . ? C33 C34 C39 123.4(4) . . ? C34 C35 C36 122.7(4) . . ? C35 C36 C37 117.6(4) . . ? C35 C36 C40 122.1(4) . . ? C37 C36 C40 120.3(5) . . ? C38 C37 C36 122.1(4) . . ? C37 C38 C33 119.8(3) . . ? C37 C38 C41 116.6(4) . . ? C33 C38 C41 123.5(3) . . ? C43 C42 C54 102.4(3) . . ? C43 C42 C6 112.9(3) . . ? C54 C42 C6 110.5(3) . . ? C43 C42 Ge2 114.7(2) . . ? C54 C42 Ge2 113.8(2) . . ? C6 C42 Ge2 103.0(2) . . ? C44 C43 C48 119.8(4) . . ? C44 C43 C42 130.3(4) . . ? C48 C43 C42 109.9(3) . . ? C45 C44 C43 118.6(4) . . ? C44 C45 C46 121.3(4) . . ? C45 C46 C47 120.5(4) . . ? C48 C47 C46 118.7(4) . . ? C47 C48 C43 121.1(4) . . ? C47 C48 C49 130.1(4) . . ? C43 C48 C49 108.7(4) . . ? C54 C49 C50 119.8(4) . . ? C54 C49 C48 109.1(3) . . ? C50 C49 C48 131.1(4) . . ? C51 C50 C49 119.2(4) . . ? C50 C51 C52 120.6(4) . . ? C51 C52 C53 121.1(4) . . ? C52 C53 C54 118.7(4) . . ? C53 C54 C49 120.4(3) . . ? C53 C54 C42 129.5(3) . . ? C49 C54 C42 109.9(3) . . ? C60 C55 C56 118.2(4) . . ? C60 C55 Ge2 117.7(3) . . ? C56 C55 Ge2 124.2(3) . . ? C57 C56 C55 119.1(4) . . ? C57 C56 C61 116.4(4) . . ? C55 C56 C61 124.5(4) . . ? C58 C57 C56 122.7(4) . . ? C59 C58 C57 117.7(4) . . ? C59 C58 C62 121.7(4) . . ? C57 C58 C62 120.7(4) . . ? C58 C59 C60 122.0(4) . . ? C59 C60 C55 120.3(4) . . ? C59 C60 C63 117.6(3) . . ? C55 C60 C63 122.0(3) . . ? C69 C64 C65 118.4(3) . . ? C69 C64 Ge2 124.6(3) . . ? C65 C64 Ge2 116.8(3) . . ? C66 C65 C64 119.4(4) . . ? C66 C65 C70 117.2(3) . . ? C64 C65 C70 123.4(3) . . ? C67 C66 C65 122.2(4) . . ? C66 C67 C68 118.0(4) . . ? C66 C67 C71 120.6(4) . . ? C68 C67 C71 121.4(4) . . ? C67 C68 C69 122.0(4) . . ? C68 C69 C64 119.9(3) . . ? C68 C69 C72 116.7(4) . . ? C64 C69 C72 123.4(3) . . ? C76 O3 C73 100.8(9) . . ? C74 C73 O3 108.6(10) . . ? C75 C74 C73 103.5(9) . . ? C74 C75 C76 111.8(10) . . ? C75 C76 O3 106.4(10) . . ? C76' O3' C73' 96.7(12) . . ? C74' C73' O3' 102.6(13) . . ? C75' C74' C73' 109.0(10) . . ? C74' C75' C76' 104.3(10) . . ? C75' C76' O3' 106.7(12) . . ? C77 O4 C80 105.3(10) . . ? C78 C77 O4 103.2(11) . . ? C79 C78 C77 103.7(12) . . ? C80 C79 C78 107.7(10) . . ? C79 C80 O4 105.3(9) . . ? C80' O4' C77' 101.0(15) . . ? C78' C77' O4' 104.7(14) . . ? C77' C78' C79' 104.4(13) . . ? C80' C79' C78' 108.9(13) . . ? C79' C80' O4' 106.0(14) . . ? C81 O5 C84 107.1(9) . . ? O5 C81 C82 105.1(8) . . ? C81 C82 C83 102.0(8) . . ? C84 C83 C82 104.3(8) . . ? C83 C84 O5 108.4(9) . . ? C81' O5' C84' 105.0(12) . . ? O5' C81' C82' 108.6(12) . . ? C81' C82' C83' 106.8(12) . . ? C82' C83' C84' 104.5(12) . . ? C83' C84' O5' 109.3(13) . . ? C85 O6 C88 91.5(14) . . ? C86 C85 O6 100.6(15) . . ? C85 C86 C87 103.6(13) . . ? C88 C87 C86 103.6(12) . . ? C87 C88 O6 104.5(14) . . ? C85' O6' C88' 92.9(11) . . ? O6' C85' C86' 104.0(11) . . ? C85' C86' C87' 102.1(9) . . ? C88' C87' C86' 104.7(9) . . ? C87' C88' O6' 105.2(10) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.786 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.071 # Attachment 'B910001F.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 713322' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H71 Ge2 O2.50' _chemical_formula_weight 1145.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5043(9) _cell_length_b 21.2079(19) _cell_length_c 26.522(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.893(2) _cell_angle_gamma 90.00 _cell_volume 5877.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3077 _cell_measurement_theta_min 2.173 _cell_measurement_theta_max 20.748 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2396 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.572649 _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' _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 8361 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1873 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 23.26 _reflns_number_total 8361 _reflns_number_gt 4646 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+5.6393P] 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 8361 _refine_ls_number_parameters 742 _refine_ls_number_restraints 142 _refine_ls_R_factor_all 0.1720 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.014 _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 1.03600(9) 0.64872(4) 0.28986(3) 0.0163(3) Uani 1 1 d . . . Ge2 Ge 0.78163(9) 0.71273(4) 0.51672(3) 0.0186(3) Uani 1 1 d . . . O1 O 1.1240(5) 0.6128(3) 0.3444(2) 0.0215(15) Uani 1 1 d . . . O2 O 0.8865(6) 0.6458(3) 0.51918(19) 0.0227(15) Uani 1 1 d . . . C1 C 1.0672(8) 0.6208(4) 0.3880(3) 0.016(2) Uani 1 1 d U . . C2 C 1.1121(8) 0.5901(4) 0.4305(3) 0.0148(19) Uani 1 1 d U . . C3 C 1.2212(9) 0.5475(4) 0.4328(4) 0.030(2) Uani 1 1 d U . . H3 H 1.2658 0.5417 0.4038 0.035 Uiso 1 1 calc R . . C4 C 1.2596(9) 0.5160(4) 0.4763(4) 0.039(3) Uani 1 1 d U . . H4 H 1.3316 0.4887 0.4775 0.046 Uiso 1 1 calc R . . C5 C 1.1932(10) 0.5233(4) 0.5202(4) 0.036(3) Uani 1 1 d U . . H5 H 1.2224 0.5008 0.5501 0.043 Uiso 1 1 calc R . . C6 C 1.0924(9) 0.5603(4) 0.5205(3) 0.028(2) Uani 1 1 d U . . H6 H 1.0485 0.5624 0.5501 0.034 Uiso 1 1 calc R . . C7 C 1.0477(9) 0.5976(4) 0.4770(3) 0.017(2) Uani 1 1 d U . . C8 C 0.9488(8) 0.6396(4) 0.4766(3) 0.016(2) Uani 1 1 d U . . C9 C 0.9439(8) 0.6594(4) 0.3822(3) 0.012(2) Uani 1 1 d . . . H9 H 0.8725 0.6295 0.3715 0.015 Uiso 1 1 calc R . . C10 C 0.9173(8) 0.6874(4) 0.4349(3) 0.0085(19) Uani 1 1 d . . . H10 H 0.9789 0.7230 0.4419 0.010 Uiso 1 1 calc R . . C11 C 0.9517(8) 0.7061(4) 0.3386(3) 0.0115(19) Uani 1 1 d . . . C12 C 1.0304(9) 0.7656(4) 0.3502(3) 0.016(2) Uani 1 1 d . . . C13 C 1.1522(9) 0.7707(4) 0.3775(3) 0.022(2) Uani 1 1 d U . . H13 H 1.1967 0.7348 0.3916 0.027 Uiso 1 1 calc R . . C14 C 1.2040(10) 0.8309(5) 0.3829(4) 0.033(3) Uani 1 1 d . . . H14 H 1.2859 0.8362 0.4012 0.040 Uiso 1 1 calc R . . C15 C 1.1407(12) 0.8827(5) 0.3626(4) 0.040(3) Uani 1 1 d . . . H15 H 1.1790 0.9231 0.3675 0.048 Uiso 1 1 calc R . . C16 C 1.0230(12) 0.8776(4) 0.3352(4) 0.035(3) Uani 1 1 d . . . H16 H 0.9803 0.9139 0.3209 0.042 Uiso 1 1 calc R . . C17 C 0.9677(9) 0.8182(4) 0.3288(3) 0.024(2) Uani 1 1 d U . . C18 C 0.8450(9) 0.7980(4) 0.3034(3) 0.017(2) Uani 1 1 d U . . C19 C 0.7500(11) 0.8317(5) 0.2747(3) 0.036(3) Uani 1 1 d . . . H19 H 0.7609 0.8753 0.2682 0.043 Uiso 1 1 calc R . . C20 C 0.6390(10) 0.8007(6) 0.2556(4) 0.041(3) Uani 1 1 d . . . H20 H 0.5730 0.8237 0.2365 0.050 Uiso 1 1 calc R . . C21 C 0.6230(9) 0.7376(6) 0.2638(3) 0.037(3) Uani 1 1 d . . . H21 H 0.5470 0.7173 0.2496 0.045 Uiso 1 1 calc R . . C22 C 0.7170(9) 0.7025(5) 0.2927(3) 0.025(2) Uani 1 1 d . . . H22 H 0.7047 0.6591 0.2997 0.031 Uiso 1 1 calc R . . C23 C 0.8286(8) 0.7334(4) 0.3109(3) 0.016(2) Uani 1 1 d U . . C24 C 0.7814(8) 0.7152(4) 0.4387(3) 0.0105(19) Uani 1 1 d U . . C25 C 0.7583(8) 0.7817(4) 0.4219(3) 0.013(2) Uani 1 1 d U . . C26 C 0.8287(9) 0.8351(4) 0.4313(3) 0.024(2) Uani 1 1 d . . . H26 H 0.9117 0.8324 0.4491 0.029 Uiso 1 1 calc R . . C27 C 0.7803(10) 0.8937(4) 0.4153(3) 0.029(3) Uani 1 1 d . . . H27 H 0.8299 0.9309 0.4217 0.035 Uiso 1 1 calc R . . C28 C 0.6586(11) 0.8969(5) 0.3897(4) 0.040(3) Uani 1 1 d . . . H28 H 0.6240 0.9369 0.3794 0.048 Uiso 1 1 calc R . . C29 C 0.5877(10) 0.8441(5) 0.3789(4) 0.034(3) Uani 1 1 d . . . H29 H 0.5055 0.8470 0.3603 0.040 Uiso 1 1 calc R . . C30 C 0.6362(8) 0.7862(4) 0.3951(3) 0.016(2) Uani 1 1 d U . . C31 C 0.5825(8) 0.7233(4) 0.3886(3) 0.017(2) Uani 1 1 d U . . C32 C 0.4694(9) 0.7017(5) 0.3622(3) 0.028(2) Uani 1 1 d U . . H32 H 0.4114 0.7303 0.3444 0.034 Uiso 1 1 calc R . . C33 C 0.4438(9) 0.6384(5) 0.3624(4) 0.037(3) Uani 1 1 d . . . H33 H 0.3674 0.6233 0.3441 0.045 Uiso 1 1 calc R . . C34 C 0.5263(10) 0.5955(5) 0.3886(4) 0.044(3) Uani 1 1 d . . . H34 H 0.5055 0.5520 0.3889 0.053 Uiso 1 1 calc R . . C35 C 0.6404(9) 0.6177(5) 0.4144(4) 0.030(3) Uani 1 1 d . . . H35 H 0.6983 0.5891 0.4324 0.036 Uiso 1 1 calc R . . C36 C 0.6682(8) 0.6814(4) 0.4137(3) 0.017(2) Uani 1 1 d . . . C37 C 1.1686(8) 0.6664(4) 0.2451(3) 0.017(2) Uani 1 1 d . . . C38 C 1.1910(8) 0.7253(4) 0.2233(3) 0.022(2) Uani 1 1 d . . . C39 C 1.2843(9) 0.7309(5) 0.1890(3) 0.026(2) Uani 1 1 d . . . H39 H 1.2994 0.7711 0.1750 0.032 Uiso 1 1 calc R . . C40 C 1.3540(9) 0.6804(5) 0.1752(3) 0.028(2) Uani 1 1 d . . . C41 C 1.3328(9) 0.6230(5) 0.1964(3) 0.030(3) Uani 1 1 d . . . H41 H 1.3806 0.5876 0.1873 0.036 Uiso 1 1 calc R . . C42 C 1.2416(9) 0.6152(4) 0.2316(3) 0.024(2) Uani 1 1 d . . . C43 C 1.1190(10) 0.7841(4) 0.2347(4) 0.040(3) Uani 1 1 d . . . H43A H 1.1615 0.8044 0.2651 0.060 Uiso 1 1 calc R . . H43B H 1.0311 0.7730 0.2405 0.060 Uiso 1 1 calc R . . H43C H 1.1175 0.8132 0.2060 0.060 Uiso 1 1 calc R . . C44 C 1.4526(10) 0.6886(5) 0.1383(4) 0.043(3) Uani 1 1 d . . . H44A H 1.4347 0.6592 0.1099 0.065 Uiso 1 1 calc R . . H44B H 1.5379 0.6801 0.1555 0.065 Uiso 1 1 calc R . . H44C H 1.4494 0.7319 0.1254 0.065 Uiso 1 1 calc R . . C45 C 1.2254(10) 0.5488(4) 0.2505(4) 0.036(3) Uani 1 1 d . . . H45A H 1.2893 0.5212 0.2374 0.055 Uiso 1 1 calc R . . H45B H 1.1394 0.5335 0.2387 0.055 Uiso 1 1 calc R . . H45C H 1.2371 0.5484 0.2876 0.055 Uiso 1 1 calc R . . C46 C 0.9064(8) 0.5904(4) 0.2577(3) 0.019(2) Uani 1 1 d . . . C47 C 0.8365(9) 0.6128(4) 0.2128(3) 0.026(2) Uani 1 1 d . . . C48 C 0.7400(10) 0.5751(5) 0.1889(3) 0.033(3) Uani 1 1 d . . . H48 H 0.6933 0.5902 0.1587 0.040 Uiso 1 1 calc R . . C49 C 0.7097(10) 0.5172(5) 0.2071(4) 0.035(3) Uani 1 1 d . . . C50 C 0.7826(10) 0.4956(5) 0.2505(4) 0.034(3) Uani 1 1 d . . . H50 H 0.7646 0.4550 0.2631 0.041 Uiso 1 1 calc R . . C51 C 0.8796(10) 0.5304(4) 0.2759(3) 0.026(2) Uani 1 1 d . . . C52 C 0.8624(9) 0.6757(4) 0.1893(3) 0.025(2) Uani 1 1 d . . . H52A H 0.7893 0.6877 0.1653 0.038 Uiso 1 1 calc R . . H52B H 0.9394 0.6727 0.1715 0.038 Uiso 1 1 calc R . . H52C H 0.8755 0.7077 0.2160 0.038 Uiso 1 1 calc R . . C53 C 0.5997(10) 0.4785(5) 0.1831(4) 0.053(3) Uani 1 1 d . . . H53A H 0.5234 0.4868 0.2004 0.080 Uiso 1 1 calc R . . H53B H 0.6216 0.4337 0.1859 0.080 Uiso 1 1 calc R . . H53C H 0.5826 0.4900 0.1472 0.080 Uiso 1 1 calc R . . C54 C 0.9501(10) 0.5007(5) 0.3237(4) 0.043(3) Uani 1 1 d . . . H54A H 1.0427 0.5040 0.3222 0.065 Uiso 1 1 calc R . . H54B H 0.9260 0.4562 0.3257 0.065 Uiso 1 1 calc R . . H54C H 0.9266 0.5230 0.3538 0.065 Uiso 1 1 calc R . . C55 C 0.6450(9) 0.6791(4) 0.5562(3) 0.023(2) Uani 1 1 d U . . C56 C 0.6923(9) 0.6512(5) 0.6025(3) 0.029(2) Uani 1 1 d . . . C57 C 0.6024(11) 0.6202(4) 0.6307(3) 0.032(3) Uani 1 1 d . . . H57 H 0.6329 0.6000 0.6615 0.039 Uiso 1 1 calc R . . C58 C 0.4755(11) 0.6182(5) 0.6155(4) 0.033(3) Uani 1 1 d . . . C59 C 0.4323(9) 0.6480(5) 0.5698(4) 0.035(3) Uani 1 1 d . . . H59 H 0.3436 0.6468 0.5583 0.042 Uiso 1 1 calc R . . C60 C 0.5145(9) 0.6791(4) 0.5408(3) 0.023(2) Uani 1 1 d U . . C61 C 0.8314(10) 0.6509(5) 0.6250(3) 0.042(3) Uani 1 1 d . . . H61A H 0.8753 0.6145 0.6120 0.062 Uiso 1 1 calc R . . H61B H 0.8354 0.6483 0.6620 0.062 Uiso 1 1 calc R . . H61C H 0.8732 0.6899 0.6154 0.062 Uiso 1 1 calc R . . C62 C 0.3820(12) 0.5857(5) 0.6465(4) 0.057(4) Uani 1 1 d . . . H62A H 0.4061 0.5939 0.6826 0.085 Uiso 1 1 calc R . . H62B H 0.3836 0.5402 0.6402 0.085 Uiso 1 1 calc R . . H62C H 0.2956 0.6020 0.6368 0.085 Uiso 1 1 calc R . . C63 C 0.4565(9) 0.7106(5) 0.4930(4) 0.041(3) Uani 1 1 d . . . H63A H 0.4290 0.6784 0.4677 0.061 Uiso 1 1 calc R . . H63B H 0.5203 0.7381 0.4797 0.061 Uiso 1 1 calc R . . H63C H 0.3825 0.7358 0.5004 0.061 Uiso 1 1 calc R . . C64 C 0.8704(9) 0.7877(4) 0.5466(3) 0.021(2) Uani 1 1 d . . . C65 C 0.7973(9) 0.8422(4) 0.5505(3) 0.020(2) Uani 1 1 d U . . C66 C 0.8546(10) 0.8965(5) 0.5696(3) 0.030(3) Uani 1 1 d . . . H66 H 0.8032 0.9331 0.5716 0.036 Uiso 1 1 calc R . . C67 C 0.9830(11) 0.9005(4) 0.5859(4) 0.035(3) Uani 1 1 d . . . C68 C 1.0559(10) 0.8467(5) 0.5817(3) 0.030(3) Uani 1 1 d . . . H68 H 1.1449 0.8485 0.5924 0.036 Uiso 1 1 calc R . . C69 C 1.0040(9) 0.7899(5) 0.5624(3) 0.026(2) Uani 1 1 d . . . C70 C 0.6555(9) 0.8427(4) 0.5343(3) 0.030(3) Uani 1 1 d . . . H70A H 0.6208 0.8846 0.5404 0.045 Uiso 1 1 calc R . . H70B H 0.6131 0.8113 0.5539 0.045 Uiso 1 1 calc R . . H70C H 0.6404 0.8326 0.4981 0.045 Uiso 1 1 calc R . . C71 C 1.0407(12) 0.9592(5) 0.6092(5) 0.065(4) Uani 1 1 d . . . H71A H 1.0095 0.9957 0.5889 0.097 Uiso 1 1 calc R . . H71B H 1.1341 0.9569 0.6103 0.097 Uiso 1 1 calc R . . H71C H 1.0163 0.9636 0.6437 0.097 Uiso 1 1 calc R . . C72 C 1.0947(9) 0.7352(5) 0.5587(4) 0.033(3) Uani 1 1 d . . . H72A H 1.1809 0.7475 0.5729 0.050 Uiso 1 1 calc R . . H72B H 1.0962 0.7232 0.5231 0.050 Uiso 1 1 calc R . . H72C H 1.0657 0.6993 0.5778 0.050 Uiso 1 1 calc R . . C73 C 0.662(4) 1.066(2) 0.511(2) 0.12(2) Uani 0.50 1 d PDU A -1 H73A H 0.6136 1.0820 0.5382 0.185 Uiso 0.50 1 calc PR A -1 H73B H 0.6831 1.1001 0.4892 0.185 Uiso 0.50 1 calc PR A -1 H73C H 0.7414 1.0460 0.5268 0.185 Uiso 0.50 1 calc PR A -1 C74 C 0.585(2) 1.0181(15) 0.4816(10) 0.068(7) Uani 0.50 1 d PDU A -1 H74A H 0.5463 1.0377 0.4497 0.081 Uiso 0.50 1 calc PR A -1 H74B H 0.6409 0.9833 0.4725 0.081 Uiso 0.50 1 calc PR A -1 O100 O 0.486(3) 0.9931(17) 0.5078(12) 0.075(7) Uani 0.50 1 d PDU A -1 C75 C 0.395(3) 0.9559(15) 0.4781(8) 0.053(6) Uani 0.50 1 d PDU A -1 H75A H 0.4368 0.9172 0.4669 0.063 Uiso 0.50 1 calc PR A -1 H75B H 0.3614 0.9799 0.4476 0.063 Uiso 0.50 1 calc PR A -1 C76 C 0.288(3) 0.9386(18) 0.5080(16) 0.096(12) Uani 0.50 1 d PDU A -1 H76A H 0.3180 0.9069 0.5334 0.144 Uiso 0.50 1 calc PR A -1 H76B H 0.2174 0.9213 0.4853 0.144 Uiso 0.50 1 calc PR A -1 H76C H 0.2592 0.9762 0.5250 0.144 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 0.0130(6) 0.0211(6) 0.0160(5) -0.0007(4) 0.0076(4) -0.0003(5) Ge2 0.0160(6) 0.0298(6) 0.0112(5) 0.0047(4) 0.0067(4) 0.0029(5) O1 0.013(4) 0.033(4) 0.020(3) 0.003(3) 0.009(3) 0.008(3) O2 0.026(4) 0.034(4) 0.010(3) 0.007(3) 0.007(3) 0.001(3) C1 0.015(5) 0.013(5) 0.021(5) 0.004(4) 0.010(4) -0.002(4) C2 0.007(5) 0.012(5) 0.025(4) 0.000(4) 0.000(4) 0.004(4) C3 0.016(6) 0.032(6) 0.042(5) 0.001(5) 0.006(5) 0.008(4) C4 0.020(6) 0.023(6) 0.072(7) 0.013(5) 0.001(5) 0.015(5) C5 0.037(7) 0.024(6) 0.042(6) 0.012(5) -0.011(5) 0.014(5) C6 0.024(6) 0.025(6) 0.034(5) 0.012(4) -0.001(5) 0.011(4) C7 0.022(5) 0.014(5) 0.015(4) 0.003(4) 0.001(4) -0.002(4) C8 0.011(5) 0.023(5) 0.013(5) 0.000(4) 0.000(4) -0.002(4) C9 0.014(5) 0.015(5) 0.009(4) 0.003(4) 0.004(4) 0.001(4) C10 0.008(5) 0.014(5) 0.004(4) 0.000(4) 0.002(4) 0.002(4) C11 0.010(5) 0.014(5) 0.011(4) 0.003(4) 0.000(4) 0.002(4) C12 0.022(6) 0.013(5) 0.015(5) -0.003(4) 0.015(4) 0.000(4) C13 0.021(5) 0.035(5) 0.012(4) -0.005(4) 0.011(4) -0.002(4) C14 0.023(6) 0.037(7) 0.042(7) -0.018(5) 0.022(5) -0.020(6) C15 0.046(8) 0.021(7) 0.061(8) -0.012(6) 0.042(7) -0.013(6) C16 0.054(9) 0.016(6) 0.041(7) -0.001(5) 0.030(6) -0.003(6) C17 0.028(4) 0.026(4) 0.022(4) -0.001(3) 0.015(3) 0.005(3) C18 0.023(4) 0.022(4) 0.008(3) 0.002(3) 0.009(3) 0.008(3) C19 0.042(8) 0.042(7) 0.027(6) 0.020(5) 0.019(6) 0.027(6) C20 0.018(7) 0.067(9) 0.039(7) 0.021(6) 0.006(5) 0.029(6) C21 0.017(6) 0.077(9) 0.017(5) -0.003(6) -0.003(5) 0.014(6) C22 0.017(6) 0.048(7) 0.011(5) -0.005(5) 0.002(4) 0.006(5) C23 0.013(4) 0.022(4) 0.016(3) -0.003(3) 0.006(3) 0.006(3) C24 0.010(4) 0.018(4) 0.003(3) 0.001(3) 0.000(3) 0.002(3) C25 0.016(5) 0.013(5) 0.013(4) -0.001(4) 0.010(4) 0.001(4) C26 0.019(6) 0.029(6) 0.026(5) 0.006(4) 0.017(5) 0.005(5) C27 0.041(7) 0.016(6) 0.035(6) 0.004(5) 0.022(5) 0.006(5) C28 0.040(8) 0.033(7) 0.050(7) 0.013(5) 0.022(6) 0.023(6) C29 0.031(7) 0.039(7) 0.035(6) 0.012(5) 0.023(5) 0.015(6) C30 0.019(4) 0.021(4) 0.010(3) 0.004(3) 0.009(3) 0.008(3) C31 0.013(4) 0.025(4) 0.013(3) 0.003(3) 0.005(3) 0.008(3) C32 0.008(5) 0.048(6) 0.028(5) 0.006(5) 0.001(4) 0.009(5) C33 0.008(6) 0.068(9) 0.035(6) -0.010(6) -0.001(5) -0.002(6) C34 0.029(7) 0.032(7) 0.073(8) -0.007(6) 0.013(6) -0.011(6) C35 0.012(6) 0.025(6) 0.052(7) -0.001(5) 0.007(5) 0.004(5) C36 0.017(6) 0.028(6) 0.008(5) 0.003(4) 0.006(4) 0.002(5) C37 0.011(5) 0.027(6) 0.013(5) -0.003(4) 0.005(4) 0.004(4) C38 0.011(5) 0.029(6) 0.025(5) -0.010(5) 0.002(4) -0.001(5) C39 0.028(6) 0.041(7) 0.012(5) 0.002(4) 0.013(5) -0.015(5) C40 0.017(6) 0.048(7) 0.022(5) 0.002(5) 0.009(5) 0.003(5) C41 0.011(6) 0.045(7) 0.034(6) -0.008(5) 0.010(5) 0.008(5) C42 0.025(6) 0.031(6) 0.015(5) 0.001(4) 0.000(5) 0.001(5) C43 0.054(8) 0.026(6) 0.044(6) 0.005(5) 0.031(6) -0.012(6) C44 0.030(7) 0.076(8) 0.026(6) 0.010(6) 0.014(5) -0.002(6) C45 0.026(7) 0.042(7) 0.042(7) -0.008(5) 0.007(5) 0.009(5) C46 0.010(5) 0.023(6) 0.025(5) -0.006(4) 0.010(4) 0.000(4) C47 0.019(6) 0.031(6) 0.028(6) -0.013(5) 0.009(5) 0.003(5) C48 0.028(7) 0.049(7) 0.022(5) -0.016(5) 0.000(5) 0.002(6) C49 0.025(7) 0.040(7) 0.044(7) -0.026(6) 0.020(6) -0.004(6) C50 0.033(7) 0.035(6) 0.040(7) -0.002(5) 0.029(6) -0.013(6) C51 0.035(7) 0.011(5) 0.036(6) -0.002(5) 0.020(5) 0.000(5) C52 0.014(6) 0.042(6) 0.018(5) -0.001(5) -0.006(4) 0.006(5) C53 0.029(7) 0.057(8) 0.077(8) -0.034(7) 0.019(6) -0.021(6) C54 0.047(8) 0.025(6) 0.060(8) 0.000(5) 0.012(6) -0.010(6) C55 0.025(5) 0.029(5) 0.016(5) 0.006(4) 0.015(4) 0.000(4) C56 0.025(6) 0.041(6) 0.023(5) -0.004(5) 0.004(5) 0.000(5) C57 0.059(8) 0.030(6) 0.010(5) 0.004(4) 0.016(5) -0.001(6) C58 0.042(8) 0.037(6) 0.023(6) -0.005(5) 0.013(5) -0.004(6) C59 0.018(6) 0.051(7) 0.037(6) -0.011(6) 0.014(5) -0.004(6) C60 0.021(5) 0.033(5) 0.016(4) -0.003(4) 0.014(4) 0.000(4) C61 0.046(8) 0.058(7) 0.022(5) 0.013(5) 0.006(5) 0.002(6) C62 0.073(9) 0.066(8) 0.039(7) -0.007(6) 0.041(7) -0.033(7) C63 0.015(6) 0.067(8) 0.043(6) 0.005(6) 0.012(5) 0.009(6) C64 0.020(6) 0.026(6) 0.018(5) 0.004(4) 0.004(4) 0.000(5) C65 0.029(5) 0.022(5) 0.010(4) 0.009(4) 0.011(4) 0.000(5) C66 0.030(7) 0.027(6) 0.034(6) 0.006(5) 0.010(5) 0.007(5) C67 0.048(8) 0.017(6) 0.041(6) 0.005(5) 0.011(6) 0.004(6) C68 0.028(6) 0.033(7) 0.031(6) 0.004(5) 0.009(5) -0.020(6) C69 0.032(7) 0.032(6) 0.015(5) 0.012(5) 0.013(5) 0.005(5) C70 0.026(6) 0.030(6) 0.036(6) 0.000(5) 0.009(5) 0.012(5) C71 0.064(10) 0.040(8) 0.088(10) -0.003(7) -0.002(8) -0.013(7) C72 0.018(6) 0.051(7) 0.029(6) -0.001(5) -0.012(5) -0.008(5) C73 0.05(3) 0.13(4) 0.19(5) -0.08(3) 0.02(3) 0.003(19) C74 0.051(17) 0.079(18) 0.073(18) -0.026(14) 0.006(13) 0.038(12) O100 0.079(10) 0.074(9) 0.072(11) -0.010(8) 0.007(8) 0.010(8) C75 0.049(17) 0.08(2) 0.028(13) -0.011(12) -0.001(10) 0.041(11) C76 0.09(3) 0.09(2) 0.11(3) -0.01(2) 0.048(19) 0.01(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 1.805(5) . ? Ge1 C37 1.958(8) . ? Ge1 C46 1.967(8) . ? Ge1 C11 2.043(8) . ? Ge2 O2 1.793(6) . ? Ge2 C64 1.967(9) . ? Ge2 C55 1.993(9) . ? Ge2 C24 2.070(7) . ? O1 C1 1.364(10) . ? O2 C8 1.369(9) . ? C1 C2 1.344(11) . ? C1 C9 1.527(11) . ? C2 C3 1.456(12) . ? C2 C7 1.475(11) . ? C3 C4 1.358(12) . ? C4 C5 1.424(14) . ? C5 C6 1.319(12) . ? C6 C7 1.439(11) . ? C7 C8 1.367(11) . ? C8 C10 1.511(11) . ? C9 C11 1.530(10) . ? C9 C10 1.570(10) . ? C10 C24 1.557(11) . ? C11 C12 1.522(11) . ? C11 C23 1.534(11) . ? C12 C17 1.387(12) . ? C12 C13 1.408(12) . ? C13 C14 1.390(12) . ? C14 C15 1.365(14) . ? C15 C16 1.372(14) . ? C16 C17 1.391(12) . ? C17 C18 1.456(12) . ? C18 C19 1.389(12) . ? C18 C23 1.397(11) . ? C19 C20 1.388(14) . ? C20 C21 1.369(14) . ? C21 C22 1.402(12) . ? C22 C23 1.386(12) . ? C24 C36 1.486(11) . ? C24 C25 1.492(11) . ? C25 C26 1.362(11) . ? C25 C30 1.404(11) . ? C26 C27 1.393(12) . ? C27 C28 1.387(13) . ? C28 C29 1.360(13) . ? C29 C30 1.382(12) . ? C30 C31 1.452(12) . ? C31 C36 1.385(11) . ? C31 C32 1.393(12) . ? C32 C33 1.369(13) . ? C33 C34 1.392(13) . ? C34 C35 1.399(13) . ? C35 C36 1.383(12) . ? C37 C42 1.398(12) . ? C37 C38 1.406(11) . ? C38 C39 1.409(12) . ? C38 C43 1.505(12) . ? C39 C40 1.367(12) . ? C40 C41 1.369(13) . ? C40 C44 1.507(13) . ? C41 C42 1.413(12) . ? C42 C45 1.511(12) . ? C46 C51 1.400(12) . ? C46 C47 1.416(12) . ? C47 C48 1.390(12) . ? C47 C52 1.509(12) . ? C48 C49 1.370(13) . ? C49 C50 1.393(14) . ? C49 C53 1.504(13) . ? C50 C51 1.377(13) . ? C51 C54 1.536(13) . ? C55 C60 1.390(12) . ? C55 C56 1.408(12) . ? C56 C57 1.423(13) . ? C56 C61 1.520(13) . ? C57 C58 1.352(14) . ? C58 C59 1.402(13) . ? C58 C62 1.510(13) . ? C59 C60 1.380(12) . ? C60 C63 1.507(12) . ? C64 C65 1.398(12) . ? C64 C69 1.424(12) . ? C65 C66 1.373(12) . ? C65 C70 1.507(12) . ? C66 C67 1.375(13) . ? C67 C68 1.384(13) . ? C67 C71 1.491(13) . ? C68 C69 1.398(12) . ? C69 C72 1.510(12) . ? C73 C74 1.47(3) . ? C74 O100 1.41(3) . ? O100 C75 1.41(3) . ? C75 C76 1.48(3) . ? 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 C37 103.3(3) . . ? O1 Ge1 C46 110.9(3) . . ? C37 Ge1 C46 111.2(3) . . ? O1 Ge1 C11 87.9(3) . . ? C37 Ge1 C11 130.7(3) . . ? C46 Ge1 C11 108.9(3) . . ? O2 Ge2 C64 111.1(3) . . ? O2 Ge2 C55 99.8(3) . . ? C64 Ge2 C55 114.5(4) . . ? O2 Ge2 C24 89.6(3) . . ? C64 Ge2 C24 109.5(3) . . ? C55 Ge2 C24 127.4(3) . . ? C1 O1 Ge1 113.2(5) . . ? C8 O2 Ge2 113.0(5) . . ? C2 C1 O1 120.2(8) . . ? C2 C1 C9 124.4(8) . . ? O1 C1 C9 115.0(7) . . ? C1 C2 C3 122.9(8) . . ? C1 C2 C7 119.8(8) . . ? C3 C2 C7 117.3(7) . . ? C4 C3 C2 120.4(9) . . ? C3 C4 C5 120.8(9) . . ? C6 C5 C4 122.1(9) . . ? C5 C6 C7 121.2(9) . . ? C8 C7 C6 123.3(8) . . ? C8 C7 C2 118.5(7) . . ? C6 C7 C2 118.2(8) . . ? C7 C8 O2 119.0(7) . . ? C7 C8 C10 123.4(7) . . ? O2 C8 C10 116.9(7) . . ? C1 C9 C11 108.2(7) . . ? C1 C9 C10 109.9(6) . . ? C11 C9 C10 117.1(6) . . ? C8 C10 C24 109.9(6) . . ? C8 C10 C9 110.6(6) . . ? C24 C10 C9 116.6(6) . . ? C12 C11 C9 117.0(6) . . ? C12 C11 C23 101.4(6) . . ? C9 C11 C23 119.9(7) . . ? C12 C11 Ge1 111.1(5) . . ? C9 C11 Ge1 98.8(5) . . ? C23 C11 Ge1 108.7(5) . . ? C17 C12 C13 121.1(8) . . ? C17 C12 C11 111.1(8) . . ? C13 C12 C11 127.9(8) . . ? C14 C13 C12 116.7(9) . . ? C15 C14 C13 121.9(10) . . ? C14 C15 C16 121.4(10) . . ? C15 C16 C17 118.6(9) . . ? C12 C17 C16 120.3(9) . . ? C12 C17 C18 108.3(8) . . ? C16 C17 C18 131.4(9) . . ? C19 C18 C23 119.3(9) . . ? C19 C18 C17 130.9(9) . . ? C23 C18 C17 109.8(7) . . ? C20 C19 C18 119.1(9) . . ? C21 C20 C19 121.1(9) . . ? C20 C21 C22 121.0(10) . . ? C23 C22 C21 117.5(9) . . ? C22 C23 C18 121.8(8) . . ? C22 C23 C11 129.0(8) . . ? C18 C23 C11 109.2(7) . . ? C36 C24 C25 103.0(6) . . ? C36 C24 C10 119.0(7) . . ? C25 C24 C10 117.5(7) . . ? C36 C24 Ge2 110.6(5) . . ? C25 C24 Ge2 107.8(5) . . ? C10 C24 Ge2 98.5(4) . . ? C26 C25 C30 119.2(8) . . ? C26 C25 C24 131.6(8) . . ? C30 C25 C24 109.1(7) . . ? C25 C26 C27 120.8(9) . . ? C28 C27 C26 118.8(9) . . ? C29 C28 C27 121.4(9) . . ? C28 C29 C30 119.4(10) . . ? C29 C30 C25 120.4(9) . . ? C29 C30 C31 130.8(9) . . ? C25 C30 C31 108.7(7) . . ? C36 C31 C32 120.6(8) . . ? C36 C31 C30 107.9(8) . . ? C32 C31 C30 131.5(8) . . ? C33 C32 C31 118.6(9) . . ? C32 C33 C34 121.9(9) . . ? C33 C34 C35 118.9(10) . . ? C36 C35 C34 119.5(9) . . ? C35 C36 C31 120.4(8) . . ? C35 C36 C24 128.8(8) . . ? C31 C36 C24 110.8(8) . . ? C42 C37 C38 117.8(8) . . ? C42 C37 Ge1 116.7(6) . . ? C38 C37 Ge1 125.4(6) . . ? C37 C38 C39 119.8(8) . . ? C37 C38 C43 123.0(8) . . ? C39 C38 C43 117.2(8) . . ? C40 C39 C38 122.3(9) . . ? C39 C40 C41 118.1(9) . . ? C39 C40 C44 120.4(9) . . ? C41 C40 C44 121.4(9) . . ? C40 C41 C42 121.7(9) . . ? C37 C42 C41 120.3(9) . . ? C37 C42 C45 123.8(8) . . ? C41 C42 C45 115.8(9) . . ? C51 C46 C47 119.2(8) . . ? C51 C46 Ge1 125.2(7) . . ? C47 C46 Ge1 115.5(7) . . ? C48 C47 C46 118.8(9) . . ? C48 C47 C52 118.3(8) . . ? C46 C47 C52 122.8(8) . . ? C49 C48 C47 122.6(9) . . ? C48 C49 C50 117.4(9) . . ? C48 C49 C53 122.4(10) . . ? C50 C49 C53 120.2(10) . . ? C51 C50 C49 122.9(9) . . ? C50 C51 C46 119.0(9) . . ? C50 C51 C54 117.0(8) . . ? C46 C51 C54 124.0(9) . . ? C60 C55 C56 120.3(8) . . ? C60 C55 Ge2 126.0(6) . . ? C56 C55 Ge2 113.6(7) . . ? C55 C56 C57 117.3(9) . . ? C55 C56 C61 125.6(9) . . ? C57 C56 C61 117.1(8) . . ? C58 C57 C56 123.1(9) . . ? C57 C58 C59 117.6(9) . . ? C57 C58 C62 122.0(10) . . ? C59 C58 C62 120.4(10) . . ? C60 C59 C58 122.1(9) . . ? C59 C60 C55 119.4(8) . . ? C59 C60 C63 117.3(9) . . ? C55 C60 C63 123.2(8) . . ? C65 C64 C69 118.9(8) . . ? C65 C64 Ge2 117.2(7) . . ? C69 C64 Ge2 123.9(7) . . ? C66 C65 C64 119.9(9) . . ? C66 C65 C70 118.8(8) . . ? C64 C65 C70 121.3(8) . . ? C65 C66 C67 123.1(9) . . ? C66 C67 C68 117.2(9) . . ? C66 C67 C71 121.7(10) . . ? C68 C67 C71 121.1(10) . . ? C67 C68 C69 122.8(10) . . ? C68 C69 C64 118.1(9) . . ? C68 C69 C72 117.5(9) . . ? C64 C69 C72 124.4(9) . . ? O100 C74 C73 113(2) . . ? C74 O100 C75 115(2) . . ? O100 C75 C76 110(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.678 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.112 _vrf_PLAT220_2 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.22 Ratio RESPONSE: A disordered ether molecule shows very large ellipsoids. ; _vrf_PLAT222_2 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.70 Ratio RESPONSE: A disordered ether molecule shows very large ellipsoids. ; _vrf_PLAT761_2 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen atoms have been placed by using a riding model and the distances are fixed by SHELXL. ; _vrf_PLAT762_2 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen atoms have been placed by using a riding model and the distances are fixed by SHELXL. ; _vrf_THTM01_2 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5556 RESPONSE: For the refinement of this structure we merged the data of the best two data sets that we could obtain, but nevertheless we were forced to cut the data at a higher resolution than 0.9 Angstrom. The data between 0.9 and 0.8 Angstrom show an R value of 0.5, so it is only background and it would not be reasonable to take this into account for the refinement. The problem is the high sensibility of this compound, which reacts spontaneously with oxygen, and crystals can only be obtained in a sealed tube and handling the crystals is a little bit difficult. So this is the best data set that we can obtain. ; _vrf_PLAT023_2 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.26 Deg. RESPONSE: For the refinement of this structure we merged the data of the best two data sets that we could obtain, but nevertheless we were forced to cut the data at a higher resolution than 0.9 Angstrom. The data between 0.9 and 0.8 Angstrom show an R value of 0.5, so it is only background and it would not be reasonable to take this into account for the refinement. The problem is the high sensibility of this compound, which reacts spontaneously with oxygen, and crystals can only be obtained in a sealed tube and handling the crystals is a little bit difficult. So this is the best data set that we can obtain. ; #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 713323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80.50 H79 Cl Ge2 O6' _chemical_formula_weight 1323.07 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 13.9981(7) _cell_length_b 24.1749(11) _cell_length_c 19.9318(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.962(3) _cell_angle_gamma 90.00 _cell_volume 6643.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9957 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.34 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2764 _exptl_absorpt_coefficient_mu 1.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6347 _exptl_absorpt_correction_T_max 0.8251 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 65912 _diffrn_reflns_av_R_equivalents 0.1046 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12500 _reflns_number_gt 8133 _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^)+(0.0552P)^2^+13.4950P] 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 12500 _refine_ls_number_parameters 862 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.094 _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 0.60076(4) 0.062670(19) 0.28163(2) 0.02491(14) Uani 1 1 d . . . Ge2 Ge 0.39496(4) 0.31081(2) 0.36874(2) 0.02676(14) Uani 1 1 d . . . O1 O 0.6810(2) 0.11450(13) 0.32710(16) 0.0284(7) Uani 1 1 d . . . O2 O 0.4917(2) 0.28063(12) 0.43059(15) 0.0280(7) Uani 1 1 d . . . O3 O 0.8546(3) 0.19103(17) 0.3710(2) 0.0552(11) Uani 1 1 d . . . O4 O 0.7940(3) 0.25502(14) 0.43315(17) 0.0378(9) Uani 1 1 d . . . O5 O 0.7027(3) 0.31901(16) 0.47208(19) 0.0482(10) Uani 1 1 d . . . C1 C 0.6324(3) 0.15826(19) 0.3530(2) 0.0271(11) Uani 1 1 d . . . C2 C 0.5279(3) 0.16376(18) 0.3121(2) 0.0234(10) Uani 1 1 d . . . H2 H 0.5348 0.1809 0.2675 0.028 Uiso 1 1 calc R . . C3 C 0.4700(3) 0.20605(18) 0.3481(2) 0.0241(10) Uani 1 1 d . . . H3 H 0.4280 0.1835 0.3734 0.029 Uiso 1 1 calc R . . C4 C 0.5423(3) 0.23796(18) 0.4041(2) 0.0234(10) Uani 1 1 d . . . C5 C 0.6340(3) 0.15320(18) 0.4292(2) 0.0242(10) Uani 1 1 d . . . C6 C 0.5848(3) 0.19591(18) 0.4567(2) 0.0238(10) Uani 1 1 d . . . C7 C 0.5848(4) 0.19782(19) 0.5259(2) 0.0285(11) Uani 1 1 d . . . H7 H 0.5520 0.2268 0.5447 0.034 Uiso 1 1 calc R . . C8 C 0.6329(4) 0.1572(2) 0.5679(2) 0.0336(12) Uani 1 1 d . . . H8 H 0.6317 0.1580 0.6154 0.040 Uiso 1 1 calc R . . C9 C 0.6825(4) 0.1156(2) 0.5410(3) 0.0363(12) Uani 1 1 d . . . H9 H 0.7163 0.0883 0.5703 0.044 Uiso 1 1 calc R . . C10 C 0.6832(4) 0.1133(2) 0.4714(2) 0.0316(11) Uani 1 1 d . . . H10 H 0.7172 0.0847 0.4530 0.038 Uiso 1 1 calc R . . C11 C 0.6823(3) 0.21472(19) 0.3432(2) 0.0256(10) Uani 1 1 d . . . H11 H 0.6802 0.2223 0.2936 0.031 Uiso 1 1 calc R . . C12 C 0.6311(3) 0.26093(18) 0.3754(2) 0.0257(10) Uani 1 1 d . . . H12 H 0.6097 0.2906 0.3411 0.031 Uiso 1 1 calc R . . C13 C 0.7860(4) 0.2165(2) 0.3807(3) 0.0358(12) Uani 1 1 d . . . C14 C 0.7070(4) 0.2833(2) 0.4322(3) 0.0331(12) Uani 1 1 d . . . C15 C 0.4804(3) 0.10596(18) 0.2945(2) 0.0226(10) Uani 1 1 d . . . C16 C 0.4209(3) 0.08125(19) 0.3443(2) 0.0274(11) Uani 1 1 d . . . C17 C 0.4459(4) 0.0699(2) 0.4136(2) 0.0340(12) Uani 1 1 d . . . H17 H 0.5088 0.0786 0.4375 0.041 Uiso 1 1 calc R . . C18 C 0.3773(4) 0.0456(2) 0.4472(3) 0.0422(14) Uani 1 1 d . . . H18 H 0.3942 0.0377 0.4945 0.051 Uiso 1 1 calc R . . C19 C 0.2856(4) 0.0327(2) 0.4135(3) 0.0433(14) Uani 1 1 d . . . H19 H 0.2397 0.0166 0.4377 0.052 Uiso 1 1 calc R . . C20 C 0.2600(4) 0.0432(2) 0.3443(3) 0.0404(13) Uani 1 1 d . . . H20 H 0.1970 0.0343 0.3207 0.048 Uiso 1 1 calc R . . C21 C 0.3282(3) 0.06689(19) 0.3101(3) 0.0306(11) Uani 1 1 d . . . C22 C 0.3206(3) 0.08107(19) 0.2376(3) 0.0298(11) Uani 1 1 d . . . C23 C 0.2452(4) 0.0737(2) 0.1833(3) 0.0395(13) Uani 1 1 d . . . H23 H 0.1867 0.0562 0.1897 0.047 Uiso 1 1 calc R . . C24 C 0.2566(4) 0.0924(2) 0.1200(3) 0.0420(14) Uani 1 1 d . . . H24 H 0.2055 0.0878 0.0824 0.050 Uiso 1 1 calc R . . C25 C 0.3420(4) 0.1180(2) 0.1104(3) 0.0338(12) Uani 1 1 d . . . H25 H 0.3482 0.1310 0.0664 0.041 Uiso 1 1 calc R . . C26 C 0.4185(4) 0.12482(19) 0.1644(2) 0.0295(11) Uani 1 1 d . . . H26 H 0.4770 0.1422 0.1577 0.035 Uiso 1 1 calc R . . C27 C 0.4076(3) 0.10578(18) 0.2282(2) 0.0242(10) Uani 1 1 d . . . C28 C 0.4001(3) 0.24608(18) 0.3018(2) 0.0253(10) Uani 1 1 d . . . C29 C 0.4248(4) 0.26108(19) 0.2327(2) 0.0295(11) Uani 1 1 d . . . C30 C 0.5084(4) 0.2815(2) 0.2137(3) 0.0353(12) Uani 1 1 d . . . H30 H 0.5638 0.2886 0.2474 0.042 Uiso 1 1 calc R . . C31 C 0.5118(4) 0.2919(2) 0.1457(3) 0.0433(14) Uani 1 1 d . . . H31 H 0.5696 0.3059 0.1331 0.052 Uiso 1 1 calc R . . C32 C 0.4311(5) 0.2819(2) 0.0960(3) 0.0465(15) Uani 1 1 d . . . H32 H 0.4344 0.2891 0.0496 0.056 Uiso 1 1 calc R . . C33 C 0.3467(5) 0.2618(2) 0.1127(2) 0.0423(14) Uani 1 1 d . . . H33 H 0.2915 0.2555 0.0786 0.051 Uiso 1 1 calc R . . C34 C 0.3438(4) 0.25050(19) 0.1815(2) 0.0325(12) Uani 1 1 d . . . C35 C 0.2654(4) 0.2278(2) 0.2123(3) 0.0340(12) Uani 1 1 d . . . C36 C 0.1722(4) 0.2118(2) 0.1843(3) 0.0437(14) Uani 1 1 d . . . H36 H 0.1501 0.2152 0.1367 0.052 Uiso 1 1 calc R . . C37 C 0.1121(4) 0.1913(2) 0.2254(4) 0.0516(16) Uani 1 1 d . . . H37 H 0.0478 0.1809 0.2063 0.062 Uiso 1 1 calc R . . C38 C 0.1444(4) 0.1856(2) 0.2955(3) 0.0488(15) Uani 1 1 d . . . H38 H 0.1021 0.1710 0.3236 0.059 Uiso 1 1 calc R . . C39 C 0.2377(4) 0.2012(2) 0.3243(3) 0.0378(13) Uani 1 1 d . . . H39 H 0.2600 0.1969 0.3718 0.045 Uiso 1 1 calc R . . C40 C 0.2982(4) 0.22305(19) 0.2826(3) 0.0303(11) Uani 1 1 d . . . C41 C 0.6472(4) -0.00598(19) 0.3308(2) 0.0292(11) Uani 1 1 d . . . C42 C 0.7486(4) -0.0129(2) 0.3443(3) 0.0349(12) Uani 1 1 d . . . C43 C 0.7887(4) -0.0569(2) 0.3850(3) 0.0434(14) Uani 1 1 d . . . H43 H 0.8572 -0.0609 0.3948 0.052 Uiso 1 1 calc R . . C44 C 0.7308(5) -0.0954(2) 0.4115(3) 0.0466(15) Uani 1 1 d . . . C45 C 0.6322(5) -0.0904(2) 0.3937(3) 0.0418(14) Uani 1 1 d . . . H45 H 0.5921 -0.1176 0.4091 0.050 Uiso 1 1 calc R . . C46 C 0.5881(4) -0.0466(2) 0.3534(2) 0.0346(12) Uani 1 1 d . . . C47 C 0.8182(4) 0.0236(2) 0.3143(3) 0.0460(14) Uani 1 1 d . . . H47A H 0.7968 0.0265 0.2649 0.069 Uiso 1 1 calc R . . H47B H 0.8833 0.0074 0.3237 0.069 Uiso 1 1 calc R . . H47C H 0.8196 0.0605 0.3348 0.069 Uiso 1 1 calc R . . C48 C 0.7769(6) -0.1413(3) 0.4582(4) 0.069(2) Uani 1 1 d . . . H48A H 0.7487 -0.1416 0.4999 0.104 Uiso 1 1 calc R . . H48B H 0.8470 -0.1350 0.4698 0.104 Uiso 1 1 calc R . . H48C H 0.7649 -0.1770 0.4349 0.104 Uiso 1 1 calc R . . C49 C 0.4792(4) -0.0479(2) 0.3371(3) 0.0400(13) Uani 1 1 d . . . H49A H 0.4558 -0.0161 0.3084 0.060 Uiso 1 1 calc R . . H49B H 0.4528 -0.0462 0.3795 0.060 Uiso 1 1 calc R . . H49C H 0.4580 -0.0822 0.3128 0.060 Uiso 1 1 calc R . . C50 C 0.6227(3) 0.0576(2) 0.1869(2) 0.0291(11) Uani 1 1 d . . . C51 C 0.5757(4) 0.0142(2) 0.1471(3) 0.0346(12) Uani 1 1 d . . . C52 C 0.5974(4) 0.0031(2) 0.0828(3) 0.0424(14) Uani 1 1 d . . . H52 H 0.5643 -0.0260 0.0564 0.051 Uiso 1 1 calc R . . C53 C 0.6663(4) 0.0335(2) 0.0565(3) 0.0445(14) Uani 1 1 d . . . C54 C 0.7092(4) 0.0778(2) 0.0947(3) 0.0379(13) Uani 1 1 d . . . H54 H 0.7548 0.0999 0.0765 0.045 Uiso 1 1 calc R . . C55 C 0.6881(4) 0.0911(2) 0.1582(2) 0.0322(12) Uani 1 1 d . . . C56 C 0.5009(4) -0.0212(2) 0.1720(3) 0.0414(14) Uani 1 1 d . . . H56A H 0.5322 -0.0438 0.2104 0.062 Uiso 1 1 calc R . . H56B H 0.4701 -0.0454 0.1351 0.062 Uiso 1 1 calc R . . H56C H 0.4516 0.0025 0.1868 0.062 Uiso 1 1 calc R . . C57 C 0.6953(6) 0.0191(3) -0.0117(3) 0.068(2) Uani 1 1 d . . . H57A H 0.7621 0.0052 -0.0041 0.102 Uiso 1 1 calc R . . H57B H 0.6909 0.0523 -0.0404 0.102 Uiso 1 1 calc R . . H57C H 0.6515 -0.0094 -0.0346 0.102 Uiso 1 1 calc R . . C58 C 0.7362(4) 0.1425(2) 0.1921(3) 0.0388(13) Uani 1 1 d . . . H58A H 0.7883 0.1543 0.1683 0.058 Uiso 1 1 calc R . . H58B H 0.7634 0.1342 0.2398 0.058 Uiso 1 1 calc R . . H58C H 0.6880 0.1721 0.1904 0.058 Uiso 1 1 calc R . . C59 C 0.2782(4) 0.31266(19) 0.4117(3) 0.0326(12) Uani 1 1 d . . . C60 C 0.1930(4) 0.3345(2) 0.3734(3) 0.0335(12) Uani 1 1 d . . . C61 C 0.1088(4) 0.3388(2) 0.4012(3) 0.0408(13) Uani 1 1 d . . . H61 H 0.0518 0.3532 0.3739 0.049 Uiso 1 1 calc R . . C62 C 0.1053(4) 0.3227(2) 0.4676(3) 0.0417(14) Uani 1 1 d . . . C63 C 0.1882(4) 0.3001(2) 0.5043(3) 0.0414(13) Uani 1 1 d . . . H63 H 0.1864 0.2875 0.5493 0.050 Uiso 1 1 calc R . . C64 C 0.2748(4) 0.2946(2) 0.4794(3) 0.0347(12) Uani 1 1 d . . . C65 C 0.1883(4) 0.3533(2) 0.3012(3) 0.0435(14) Uani 1 1 d . . . H65A H 0.2201 0.3894 0.3008 0.065 Uiso 1 1 calc R . . H65B H 0.1203 0.3565 0.2791 0.065 Uiso 1 1 calc R . . H65C H 0.2213 0.3263 0.2765 0.065 Uiso 1 1 calc R . . C66 C 0.0147(4) 0.3313(3) 0.4981(4) 0.0596(17) Uani 1 1 d . . . H66A H 0.0180 0.3084 0.5389 0.089 Uiso 1 1 calc R . . H66B H -0.0423 0.3209 0.4647 0.089 Uiso 1 1 calc R . . H66C H 0.0098 0.3704 0.5104 0.089 Uiso 1 1 calc R . . C67 C 0.3592(4) 0.2695(3) 0.5263(3) 0.0492(15) Uani 1 1 d . . . H67A H 0.3413 0.2631 0.5711 0.074 Uiso 1 1 calc R . . H67B H 0.4148 0.2947 0.5311 0.074 Uiso 1 1 calc R . . H67C H 0.3765 0.2342 0.5074 0.074 Uiso 1 1 calc R . . C68 C 0.4360(4) 0.38712(19) 0.3502(2) 0.0300(11) Uani 1 1 d . . . C69 C 0.4226(3) 0.4133(2) 0.2860(3) 0.0308(11) Uani 1 1 d . . . C70 C 0.4579(4) 0.4671(2) 0.2812(3) 0.0346(12) Uani 1 1 d . . . H70 H 0.4503 0.4838 0.2374 0.042 Uiso 1 1 calc R . . C71 C 0.5027(4) 0.4970(2) 0.3359(3) 0.0378(13) Uani 1 1 d . . . C72 C 0.5129(4) 0.4714(2) 0.3991(3) 0.0385(13) Uani 1 1 d . . . H72 H 0.5431 0.4913 0.4382 0.046 Uiso 1 1 calc R . . C73 C 0.4808(4) 0.4182(2) 0.4076(3) 0.0338(12) Uani 1 1 d . . . C74 C 0.3682(4) 0.3896(2) 0.2203(3) 0.0402(13) Uani 1 1 d . . . H74A H 0.3131 0.4137 0.2027 0.060 Uiso 1 1 calc R . . H74B H 0.3443 0.3526 0.2287 0.060 Uiso 1 1 calc R . . H74C H 0.4117 0.3873 0.1868 0.060 Uiso 1 1 calc R . . C75 C 0.5385(4) 0.5551(2) 0.3285(3) 0.0498(15) Uani 1 1 d . . . H75A H 0.5117 0.5692 0.2830 0.075 Uiso 1 1 calc R . . H75B H 0.6095 0.5550 0.3346 0.075 Uiso 1 1 calc R . . H75C H 0.5177 0.5789 0.3631 0.075 Uiso 1 1 calc R . . C76 C 0.4922(4) 0.3958(2) 0.4795(3) 0.0441(14) Uani 1 1 d . . . H76A H 0.5152 0.4253 0.5120 0.066 Uiso 1 1 calc R . . H76B H 0.5392 0.3654 0.4850 0.066 Uiso 1 1 calc R . . H76C H 0.4294 0.3821 0.4879 0.066 Uiso 1 1 calc R . . C77 C 0.9089(7) 0.2954(4) 0.2423(5) 0.102(3) Uani 1 1 d . . . H77A H 0.9366 0.3325 0.2414 0.152 Uiso 1 1 calc R . . H77B H 0.9285 0.2729 0.2061 0.152 Uiso 1 1 calc R . . H77C H 0.9325 0.2781 0.2865 0.152 Uiso 1 1 calc R . . C78 C 0.8070(7) 0.2990(4) 0.2320(4) 0.085(3) Uani 1 1 d . . . H78A H 0.7802 0.2614 0.2227 0.102 Uiso 1 1 calc R . . H78B H 0.7854 0.3215 0.1906 0.102 Uiso 1 1 calc R . . O6 O 0.7658(3) 0.32213(17) 0.2862(2) 0.0636(12) Uani 1 1 d . . . C79 C 0.7847(6) 0.3791(3) 0.2984(5) 0.091(3) Uani 1 1 d . . . H79A H 0.7943 0.3971 0.2555 0.109 Uiso 1 1 calc R . . H79B H 0.8456 0.3832 0.3317 0.109 Uiso 1 1 calc R . . C80 C 0.7083(6) 0.4064(3) 0.3239(5) 0.085(3) Uani 1 1 d . . . H80A H 0.6473 0.4011 0.2920 0.127 Uiso 1 1 calc R . . H80B H 0.7227 0.4460 0.3287 0.127 Uiso 1 1 calc R . . H80C H 0.7022 0.3909 0.3683 0.127 Uiso 1 1 calc R . . C81 C 0.019(3) 1.0098(11) 0.474(2) 0.128(6) Uani 0.178(8) 1 d PDU A -1 H81A H -0.0506 1.0037 0.4550 0.154 Uiso 0.178(8) 1 calc PR A -1 H81B H 0.0199 1.0202 0.5224 0.154 Uiso 0.178(8) 1 calc PR A -1 Cl1 Cl 0.0642(12) 0.9488(11) 0.4788(11) 0.123(4) Uani 0.178(8) 1 d PDU A -1 Cl2 Cl 0.044(2) 1.0663(14) 0.4394(14) 0.148(7) Uani 0.178(8) 1 d PDU A -1 C81' C 0.0483(16) 0.9216(15) 0.5359(8) 0.102(4) Uani 0.322(8) 1 d PDU A -2 H81C H 0.0931 0.9517 0.5546 0.123 Uiso 0.322(8) 1 calc PR A -2 H81D H 0.0830 0.8871 0.5516 0.123 Uiso 0.322(8) 1 calc PR A -2 Cl1' Cl 0.0567(6) 0.9228(5) 0.4558(5) 0.107(3) Uani 0.322(8) 1 d PDU A -2 Cl2' Cl -0.0341(8) 0.9246(6) 0.5843(6) 0.102(3) Uani 0.322(8) 1 d PDU A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0285(3) 0.0199(3) 0.0269(3) -0.0026(2) 0.0067(2) 0.0001(2) Ge2 0.0342(3) 0.0211(3) 0.0249(3) -0.0019(2) 0.0052(2) 0.0036(2) O1 0.0296(19) 0.0251(18) 0.0312(18) -0.0053(14) 0.0073(15) 0.0035(14) O2 0.040(2) 0.0224(17) 0.0216(16) -0.0046(13) 0.0037(14) 0.0067(15) O3 0.028(2) 0.050(3) 0.085(3) -0.011(2) 0.003(2) 0.0016(19) O4 0.036(2) 0.037(2) 0.037(2) -0.0031(17) -0.0030(16) -0.0089(17) O5 0.058(3) 0.042(2) 0.042(2) -0.0180(19) 0.0013(19) -0.0097(19) C1 0.030(3) 0.022(3) 0.031(3) 0.001(2) 0.008(2) 0.001(2) C2 0.029(3) 0.022(2) 0.020(2) -0.0009(19) 0.005(2) -0.003(2) C3 0.028(3) 0.018(2) 0.026(2) -0.0016(19) 0.002(2) 0.0000(19) C4 0.032(3) 0.017(2) 0.020(2) -0.0039(18) 0.002(2) 0.002(2) C5 0.024(3) 0.018(2) 0.029(3) 0.0010(19) 0.001(2) -0.0039(19) C6 0.026(3) 0.020(2) 0.025(2) 0.0028(19) 0.0010(19) -0.0049(19) C7 0.035(3) 0.023(3) 0.027(3) -0.001(2) 0.005(2) -0.004(2) C8 0.043(3) 0.034(3) 0.023(3) 0.004(2) 0.003(2) -0.006(2) C9 0.044(3) 0.028(3) 0.035(3) 0.009(2) 0.001(2) -0.001(2) C10 0.035(3) 0.025(3) 0.034(3) 0.000(2) 0.006(2) -0.002(2) C11 0.028(3) 0.025(2) 0.024(2) -0.003(2) 0.004(2) -0.003(2) C12 0.032(3) 0.020(2) 0.023(2) -0.0006(19) 0.000(2) -0.004(2) C13 0.033(3) 0.030(3) 0.043(3) 0.004(2) 0.002(2) -0.009(2) C14 0.042(3) 0.026(3) 0.030(3) 0.003(2) 0.002(2) -0.009(2) C15 0.020(2) 0.021(2) 0.027(2) -0.0013(19) 0.005(2) 0.0012(19) C16 0.027(3) 0.023(2) 0.035(3) -0.005(2) 0.012(2) -0.002(2) C17 0.044(3) 0.030(3) 0.030(3) -0.004(2) 0.010(2) -0.010(2) C18 0.060(4) 0.035(3) 0.038(3) -0.001(2) 0.027(3) -0.007(3) C19 0.048(4) 0.033(3) 0.058(4) -0.001(3) 0.032(3) -0.006(3) C20 0.032(3) 0.031(3) 0.061(4) -0.003(3) 0.017(3) -0.003(2) C21 0.031(3) 0.020(2) 0.043(3) -0.003(2) 0.011(2) 0.001(2) C22 0.026(3) 0.021(2) 0.041(3) -0.005(2) 0.003(2) 0.001(2) C23 0.027(3) 0.036(3) 0.055(4) -0.010(3) 0.005(3) -0.002(2) C24 0.040(3) 0.044(3) 0.037(3) -0.016(3) -0.006(3) 0.006(3) C25 0.037(3) 0.034(3) 0.028(3) -0.004(2) 0.000(2) 0.006(2) C26 0.030(3) 0.026(3) 0.032(3) -0.007(2) 0.005(2) 0.000(2) C27 0.025(3) 0.020(2) 0.027(3) -0.0058(19) 0.003(2) 0.003(2) C28 0.031(3) 0.021(2) 0.024(2) -0.0010(19) 0.005(2) 0.005(2) C29 0.039(3) 0.022(3) 0.028(3) -0.002(2) 0.005(2) 0.008(2) C30 0.038(3) 0.038(3) 0.029(3) 0.002(2) 0.004(2) 0.004(2) C31 0.055(4) 0.047(3) 0.030(3) 0.009(3) 0.012(3) 0.009(3) C32 0.073(5) 0.042(3) 0.026(3) 0.007(2) 0.011(3) 0.014(3) C33 0.064(4) 0.037(3) 0.020(3) -0.004(2) -0.008(3) 0.014(3) C34 0.042(3) 0.021(3) 0.032(3) -0.008(2) -0.002(2) 0.008(2) C35 0.033(3) 0.026(3) 0.039(3) -0.004(2) -0.004(2) 0.010(2) C36 0.040(3) 0.032(3) 0.053(4) -0.006(3) -0.009(3) 0.008(3) C37 0.026(3) 0.035(3) 0.088(5) -0.013(3) -0.006(3) 0.004(3) C38 0.038(3) 0.034(3) 0.077(5) -0.006(3) 0.017(3) -0.001(3) C39 0.034(3) 0.026(3) 0.053(3) -0.009(2) 0.007(3) 0.001(2) C40 0.032(3) 0.018(2) 0.041(3) -0.006(2) 0.006(2) 0.004(2) C41 0.039(3) 0.025(3) 0.024(2) -0.002(2) 0.008(2) 0.005(2) C42 0.047(3) 0.024(3) 0.035(3) -0.003(2) 0.009(2) 0.004(2) C43 0.048(3) 0.035(3) 0.047(3) 0.002(3) 0.010(3) 0.014(3) C44 0.070(5) 0.031(3) 0.041(3) 0.005(3) 0.015(3) 0.009(3) C45 0.062(4) 0.024(3) 0.043(3) 0.001(2) 0.021(3) 0.000(3) C46 0.052(3) 0.024(3) 0.031(3) -0.005(2) 0.015(2) 0.000(2) C47 0.034(3) 0.041(3) 0.064(4) 0.007(3) 0.011(3) 0.006(3) C48 0.090(5) 0.048(4) 0.072(5) 0.026(4) 0.018(4) 0.017(4) C49 0.048(3) 0.025(3) 0.049(3) -0.003(2) 0.014(3) -0.006(2) C50 0.031(3) 0.029(3) 0.027(3) -0.005(2) 0.006(2) 0.004(2) C51 0.040(3) 0.027(3) 0.036(3) -0.003(2) 0.004(2) 0.005(2) C52 0.054(4) 0.037(3) 0.033(3) -0.011(2) -0.001(3) 0.010(3) C53 0.052(4) 0.051(4) 0.029(3) -0.006(3) 0.004(3) 0.020(3) C54 0.043(3) 0.043(3) 0.030(3) 0.006(2) 0.012(2) 0.012(3) C55 0.037(3) 0.030(3) 0.030(3) -0.002(2) 0.008(2) 0.009(2) C56 0.048(4) 0.028(3) 0.045(3) -0.009(2) 0.000(3) -0.004(2) C57 0.091(5) 0.079(5) 0.034(3) -0.009(3) 0.013(3) 0.027(4) C58 0.046(3) 0.036(3) 0.038(3) 0.001(2) 0.018(3) -0.005(3) C59 0.040(3) 0.020(2) 0.038(3) -0.006(2) 0.008(2) 0.003(2) C60 0.030(3) 0.025(3) 0.046(3) -0.005(2) 0.010(2) 0.002(2) C61 0.041(3) 0.025(3) 0.055(4) -0.001(3) 0.006(3) 0.002(2) C62 0.041(3) 0.032(3) 0.056(4) -0.007(3) 0.019(3) -0.005(2) C63 0.051(4) 0.034(3) 0.042(3) -0.002(2) 0.017(3) -0.004(3) C64 0.044(3) 0.029(3) 0.033(3) -0.001(2) 0.010(2) 0.001(2) C65 0.037(3) 0.048(3) 0.045(3) 0.009(3) 0.007(3) 0.014(3) C66 0.043(4) 0.068(4) 0.072(4) 0.003(4) 0.022(3) -0.002(3) C67 0.056(4) 0.061(4) 0.033(3) 0.013(3) 0.015(3) 0.007(3) C68 0.030(3) 0.024(3) 0.035(3) -0.004(2) 0.005(2) 0.005(2) C69 0.027(3) 0.027(3) 0.040(3) 0.001(2) 0.007(2) 0.007(2) C70 0.032(3) 0.029(3) 0.047(3) 0.005(2) 0.015(2) 0.006(2) C71 0.029(3) 0.026(3) 0.060(4) -0.003(3) 0.012(3) 0.004(2) C72 0.039(3) 0.028(3) 0.048(3) -0.012(3) 0.006(3) 0.004(2) C73 0.038(3) 0.026(3) 0.038(3) -0.007(2) 0.008(2) 0.008(2) C74 0.055(4) 0.031(3) 0.034(3) 0.003(2) 0.007(3) 0.003(3) C75 0.041(3) 0.032(3) 0.077(4) -0.002(3) 0.014(3) -0.007(3) C76 0.060(4) 0.035(3) 0.035(3) -0.013(2) 0.000(3) 0.002(3) C77 0.088(7) 0.106(7) 0.116(8) 0.010(6) 0.032(6) 0.028(5) C78 0.100(7) 0.083(6) 0.079(6) 0.021(5) 0.032(5) -0.025(5) O6 0.084(3) 0.039(3) 0.075(3) 0.003(2) 0.036(3) -0.007(2) C79 0.090(6) 0.050(5) 0.141(8) 0.012(5) 0.046(6) -0.008(4) C80 0.075(5) 0.048(4) 0.146(8) 0.011(5) 0.059(5) 0.002(4) C81 0.062(9) 0.208(11) 0.094(11) -0.058(10) -0.045(9) 0.020(9) Cl1 0.060(5) 0.204(9) 0.096(8) -0.054(7) -0.014(6) 0.016(6) Cl2 0.095(10) 0.221(12) 0.103(13) -0.051(10) -0.047(9) 0.024(10) C81' 0.052(6) 0.182(9) 0.072(7) -0.045(7) 0.008(6) 0.015(6) Cl1' 0.057(4) 0.186(8) 0.071(5) -0.052(5) -0.010(3) 0.025(5) Cl2' 0.046(4) 0.175(8) 0.085(7) -0.035(6) 0.009(5) -0.006(5) _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 1.817(3) . ? Ge1 C50 1.969(5) . ? Ge1 C41 1.979(5) . ? Ge1 C15 2.037(4) . ? Ge2 O2 1.819(3) . ? Ge2 C59 1.973(5) . ? Ge2 C68 1.985(5) . ? Ge2 C28 2.066(4) . ? O1 C1 1.403(5) . ? O2 C4 1.405(5) . ? O3 C13 1.184(6) . ? O4 C13 1.390(6) . ? O4 C14 1.393(6) . ? O5 C14 1.183(6) . ? C1 C5 1.519(6) . ? C1 C2 1.553(6) . ? C1 C11 1.561(6) . ? C2 C3 1.556(6) . ? C2 C15 1.561(6) . ? C3 C28 1.560(6) . ? C3 C4 1.573(6) . ? C4 C6 1.506(6) . ? C4 C12 1.557(6) . ? C5 C10 1.382(6) . ? C5 C6 1.404(6) . ? C6 C7 1.381(6) . ? C7 C8 1.387(7) . ? C8 C9 1.382(7) . ? C9 C10 1.391(7) . ? C11 C13 1.513(7) . ? C11 C12 1.528(6) . ? C12 C14 1.512(7) . ? C15 C27 1.521(6) . ? C15 C16 1.524(6) . ? C16 C17 1.391(7) . ? C16 C21 1.401(7) . ? C17 C18 1.393(7) . ? C18 C19 1.378(8) . ? C19 C20 1.388(8) . ? C20 C21 1.389(7) . ? C21 C22 1.470(7) . ? C22 C23 1.386(7) . ? C22 C27 1.398(6) . ? C23 C24 1.376(8) . ? C24 C25 1.387(8) . ? C25 C26 1.391(7) . ? C26 C27 1.386(6) . ? C28 C40 1.517(7) . ? C28 C29 1.520(6) . ? C29 C30 1.382(7) . ? C29 C34 1.411(7) . ? C30 C31 1.386(7) . ? C31 C32 1.389(8) . ? C32 C33 1.370(8) . ? C33 C34 1.406(7) . ? C34 C35 1.455(7) . ? C35 C36 1.381(7) . ? C35 C40 1.403(7) . ? C36 C37 1.365(8) . ? C37 C38 1.399(9) . ? C38 C39 1.384(8) . ? C39 C40 1.389(7) . ? C41 C46 1.406(7) . ? C41 C42 1.409(7) . ? C42 C43 1.395(7) . ? C42 C47 1.513(7) . ? C43 C44 1.396(8) . ? C44 C45 1.369(8) . ? C44 C48 1.519(8) . ? C45 C46 1.407(7) . ? C46 C49 1.504(8) . ? C50 C51 1.407(7) . ? C50 C55 1.415(7) . ? C51 C52 1.393(7) . ? C51 C56 1.503(7) . ? C52 C53 1.386(8) . ? C53 C54 1.388(8) . ? C53 C57 1.525(7) . ? C54 C55 1.388(7) . ? C55 C58 1.515(7) . ? C59 C60 1.404(7) . ? C59 C64 1.427(7) . ? C60 C61 1.391(7) . ? C60 C65 1.499(7) . ? C61 C62 1.388(8) . ? C62 C63 1.374(8) . ? C62 C66 1.513(8) . ? C63 C64 1.393(7) . ? C64 C67 1.503(7) . ? C68 C69 1.412(7) . ? C68 C73 1.421(7) . ? C69 C70 1.400(7) . ? C69 C74 1.508(7) . ? C70 C71 1.367(7) . ? C71 C72 1.388(7) . ? C71 C75 1.508(7) . ? C72 C73 1.382(7) . ? C73 C76 1.514(7) . ? C77 C78 1.408(11) . ? C78 O6 1.425(9) . ? O6 C79 1.415(8) . ? C79 C80 1.422(10) . ? C81 Cl2 1.602(19) . ? C81 Cl1 1.603(19) . ? C81' Cl1' 1.621(15) . ? C81' Cl2' 1.628(15) . ? 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 C50 109.65(17) . . ? O1 Ge1 C41 102.13(18) . . ? C50 Ge1 C41 109.24(19) . . ? O1 Ge1 C15 92.09(16) . . ? C50 Ge1 C15 115.00(19) . . ? C41 Ge1 C15 125.21(19) . . ? O2 Ge2 C59 106.90(18) . . ? O2 Ge2 C68 107.05(17) . . ? C59 Ge2 C68 110.35(19) . . ? O2 Ge2 C28 91.65(16) . . ? C59 Ge2 C28 114.94(19) . . ? C68 Ge2 C28 122.69(19) . . ? C1 O1 Ge1 114.0(3) . . ? C4 O2 Ge2 113.9(3) . . ? C13 O4 C14 111.2(4) . . ? O1 C1 C5 112.5(4) . . ? O1 C1 C2 110.1(4) . . ? C5 C1 C2 112.5(4) . . ? O1 C1 C11 110.9(4) . . ? C5 C1 C11 105.4(4) . . ? C2 C1 C11 105.1(4) . . ? C1 C2 C3 109.4(3) . . ? C1 C2 C15 111.6(4) . . ? C3 C2 C15 117.1(4) . . ? C2 C3 C28 117.2(4) . . ? C2 C3 C4 109.1(4) . . ? C28 C3 C4 112.1(3) . . ? O2 C4 C6 113.5(4) . . ? O2 C4 C12 111.2(4) . . ? C6 C4 C12 104.6(4) . . ? O2 C4 C3 108.8(4) . . ? C6 C4 C3 106.9(3) . . ? C12 C4 C3 111.7(3) . . ? C10 C5 C6 120.1(4) . . ? C10 C5 C1 125.8(4) . . ? C6 C5 C1 114.0(4) . . ? C7 C6 C5 120.0(4) . . ? C7 C6 C4 127.2(4) . . ? C5 C6 C4 112.7(4) . . ? C6 C7 C8 119.7(5) . . ? C9 C8 C7 120.4(5) . . ? C8 C9 C10 120.4(5) . . ? C5 C10 C9 119.5(5) . . ? C13 C11 C12 104.6(4) . . ? C13 C11 C1 112.0(4) . . ? C12 C11 C1 109.5(4) . . ? C14 C12 C11 104.8(4) . . ? C14 C12 C4 110.7(4) . . ? C11 C12 C4 110.9(4) . . ? O3 C13 O4 120.6(5) . . ? O3 C13 C11 129.8(5) . . ? O4 C13 C11 109.6(4) . . ? O5 C14 O4 119.7(5) . . ? O5 C14 C12 130.8(5) . . ? O4 C14 C12 109.5(4) . . ? C27 C15 C16 101.9(4) . . ? C27 C15 C2 113.1(4) . . ? C16 C15 C2 117.7(4) . . ? C27 C15 Ge1 109.5(3) . . ? C16 C15 Ge1 115.9(3) . . ? C2 C15 Ge1 99.1(3) . . ? C17 C16 C21 119.1(4) . . ? C17 C16 C15 130.7(4) . . ? C21 C16 C15 110.1(4) . . ? C16 C17 C18 119.1(5) . . ? C19 C18 C17 121.5(5) . . ? C18 C19 C20 120.1(5) . . ? C19 C20 C21 118.9(5) . . ? C20 C21 C16 121.4(5) . . ? C20 C21 C22 129.7(5) . . ? C16 C21 C22 108.9(4) . . ? C23 C22 C27 120.9(5) . . ? C23 C22 C21 130.8(5) . . ? C27 C22 C21 108.3(4) . . ? C24 C23 C22 118.7(5) . . ? C23 C24 C25 120.8(5) . . ? C24 C25 C26 120.9(5) . . ? C27 C26 C25 118.6(5) . . ? C26 C27 C22 120.1(4) . . ? C26 C27 C15 129.2(4) . . ? C22 C27 C15 110.7(4) . . ? C40 C28 C29 102.2(4) . . ? C40 C28 C3 112.8(4) . . ? C29 C28 C3 117.8(4) . . ? C40 C28 Ge2 107.7(3) . . ? C29 C28 Ge2 116.3(3) . . ? C3 C28 Ge2 100.1(3) . . ? C30 C29 C34 118.6(5) . . ? C30 C29 C28 132.0(5) . . ? C34 C29 C28 109.4(4) . . ? C29 C30 C31 120.4(5) . . ? C30 C31 C32 120.3(6) . . ? C33 C32 C31 121.1(5) . . ? C32 C33 C34 118.6(5) . . ? C33 C34 C29 121.0(5) . . ? C33 C34 C35 129.5(5) . . ? C29 C34 C35 109.5(4) . . ? C36 C35 C40 120.3(5) . . ? C36 C35 C34 131.6(5) . . ? C40 C35 C34 108.1(4) . . ? C37 C36 C35 119.7(6) . . ? C36 C37 C38 120.6(5) . . ? C39 C38 C37 120.3(6) . . ? C38 C39 C40 119.0(5) . . ? C39 C40 C35 120.0(5) . . ? C39 C40 C28 129.3(5) . . ? C35 C40 C28 110.7(4) . . ? C46 C41 C42 118.9(4) . . ? C46 C41 Ge1 125.7(4) . . ? C42 C41 Ge1 115.4(4) . . ? C43 C42 C41 119.6(5) . . ? C43 C42 C47 116.9(5) . . ? C41 C42 C47 123.5(5) . . ? C42 C43 C44 121.7(5) . . ? C45 C44 C43 118.0(5) . . ? C45 C44 C48 121.7(6) . . ? C43 C44 C48 120.3(6) . . ? C44 C45 C46 122.4(5) . . ? C41 C46 C45 119.0(5) . . ? C41 C46 C49 125.1(5) . . ? C45 C46 C49 115.8(5) . . ? C51 C50 C55 118.1(4) . . ? C51 C50 Ge1 116.9(4) . . ? C55 C50 Ge1 124.8(4) . . ? C52 C51 C50 120.5(5) . . ? C52 C51 C56 118.0(5) . . ? C50 C51 C56 121.5(4) . . ? C53 C52 C51 121.5(5) . . ? C52 C53 C54 117.7(5) . . ? C52 C53 C57 121.7(6) . . ? C54 C53 C57 120.5(6) . . ? C55 C54 C53 122.6(5) . . ? C54 C55 C50 119.4(5) . . ? C54 C55 C58 116.7(5) . . ? C50 C55 C58 123.9(4) . . ? C60 C59 C64 117.8(5) . . ? C60 C59 Ge2 117.5(4) . . ? C64 C59 Ge2 124.7(4) . . ? C61 C60 C59 120.6(5) . . ? C61 C60 C65 117.4(5) . . ? C59 C60 C65 121.9(5) . . ? C62 C61 C60 122.1(5) . . ? C63 C62 C61 117.0(5) . . ? C63 C62 C66 122.1(5) . . ? C61 C62 C66 120.9(5) . . ? C62 C63 C64 123.6(5) . . ? C63 C64 C59 118.8(5) . . ? C63 C64 C67 117.0(5) . . ? C59 C64 C67 124.1(5) . . ? C69 C68 C73 117.7(4) . . ? C69 C68 Ge2 126.0(4) . . ? C73 C68 Ge2 116.3(4) . . ? C70 C69 C68 119.0(5) . . ? C70 C69 C74 115.1(4) . . ? C68 C69 C74 125.8(4) . . ? C71 C70 C69 123.7(5) . . ? C70 C71 C72 116.8(5) . . ? C70 C71 C75 121.9(5) . . ? C72 C71 C75 121.3(5) . . ? C73 C72 C71 122.7(5) . . ? C72 C73 C68 120.1(5) . . ? C72 C73 C76 117.8(5) . . ? C68 C73 C76 122.1(5) . . ? C77 C78 O6 116.5(8) . . ? C79 O6 C78 115.1(6) . . ? O6 C79 C80 112.5(6) . . ? Cl2 C81 Cl1 134(3) . . ? Cl1' C81' Cl2' 139.7(17) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.321 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.085 #===END #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 713324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H81 Ge2 O5.50' _chemical_formula_weight 1251.61 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 9.8547(6) _cell_length_b 14.9574(9) _cell_length_c 23.1368(15) _cell_angle_alpha 71.1490(10) _cell_angle_beta 83.0260(10) _cell_angle_gamma 81.4140(10) _cell_volume 3181.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 3511 _cell_measurement_theta_min 2.361 _cell_measurement_theta_max 25.001 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1314 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.467544 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 18888 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.1337 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12781 _reflns_number_gt 7253 _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^)+(0.0548P)^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 12781 _refine_ls_number_parameters 807 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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 0.87429(5) 0.37371(3) 0.20334(2) 0.02359(13) Uani 1 1 d . . . Ge2 Ge 0.81412(5) 0.75584(3) 0.31630(2) 0.02619(14) Uani 1 1 d . . . O1 O 0.6311(3) 0.5118(2) 0.25556(13) 0.0260(7) Uani 1 1 d . . . O2 O 0.5968(3) 0.6010(2) 0.27315(13) 0.0262(7) Uani 1 1 d . . . O3 O 0.7588(3) 0.3703(2) 0.27194(13) 0.0251(7) Uani 1 1 d . . . O4 O 0.6659(3) 0.6925(2) 0.32207(14) 0.0293(7) Uani 1 1 d . . . C1 C 0.9376(4) 0.4990(3) 0.2012(2) 0.0231(10) Uani 1 1 d . . . C2 C 0.8780(4) 0.5046(3) 0.26603(18) 0.0206(9) Uani 1 1 d . . . H2 H 0.9500 0.4717 0.2953 0.025 Uiso 1 1 calc R . . C3 C 0.7488(4) 0.4508(3) 0.28847(19) 0.0222(10) Uani 1 1 d . . . C4 C 0.9484(4) 0.6527(3) 0.29162(19) 0.0218(10) Uani 1 1 d . . . C5 C 0.8382(4) 0.6054(3) 0.27132(19) 0.0207(10) Uani 1 1 d . . . H5 H 0.8168 0.6473 0.2293 0.025 Uiso 1 1 calc R . . C6 C 0.7011(5) 0.6060(3) 0.3117(2) 0.0254(10) Uani 1 1 d . . . C7 C 0.7111(4) 0.4366(3) 0.3555(2) 0.0252(10) Uani 1 1 d . . . C8 C 0.6959(5) 0.3511(3) 0.4008(2) 0.0311(11) Uani 1 1 d . . . H8 H 0.7076 0.2929 0.3916 0.037 Uiso 1 1 calc R . . C9 C 0.6626(5) 0.3538(3) 0.4607(2) 0.0324(12) Uani 1 1 d . . . H9 H 0.6528 0.2960 0.4929 0.039 Uiso 1 1 calc R . . C10 C 0.6435(5) 0.4382(3) 0.4743(2) 0.0297(11) Uani 1 1 d . . . H10 H 0.6224 0.4380 0.5155 0.036 Uiso 1 1 calc R . . C11 C 0.6551(4) 0.5239(3) 0.4275(2) 0.0276(11) Uani 1 1 d . . . H11 H 0.6392 0.5827 0.4362 0.033 Uiso 1 1 calc R . . C12 C 0.6900(4) 0.5216(3) 0.36842(19) 0.0228(10) Uani 1 1 d . . . C13 C 1.0934(4) 0.4902(3) 0.19276(19) 0.0237(10) Uani 1 1 d . . . C14 C 1.1911(5) 0.4317(3) 0.2313(2) 0.0286(11) Uani 1 1 d . . . H14 H 1.1632 0.3875 0.2692 0.034 Uiso 1 1 calc R . . C15 C 1.3303(5) 0.4388(4) 0.2136(2) 0.0390(13) Uani 1 1 d . . . H15 H 1.3976 0.3997 0.2398 0.047 Uiso 1 1 calc R . . C16 C 1.3716(5) 0.5021(4) 0.1583(3) 0.0419(14) Uani 1 1 d . . . H16 H 1.4671 0.5048 0.1465 0.050 Uiso 1 1 calc R . . C17 C 1.2773(5) 0.5609(4) 0.1205(2) 0.0353(12) Uani 1 1 d . . . H17 H 1.3066 0.6051 0.0829 0.042 Uiso 1 1 calc R . . C18 C 1.1371(5) 0.5555(3) 0.1375(2) 0.0268(10) Uani 1 1 d . . . C19 C 1.0157(5) 0.6135(3) 0.1089(2) 0.0290(11) Uani 1 1 d . . . C20 C 1.0047(6) 0.6893(4) 0.0554(2) 0.0381(13) Uani 1 1 d . . . H20 H 1.0843 0.7084 0.0293 0.046 Uiso 1 1 calc R . . C21 C 0.8765(6) 0.7363(4) 0.0407(2) 0.0433(14) Uani 1 1 d . . . H21 H 0.8682 0.7893 0.0046 0.052 Uiso 1 1 calc R . . C22 C 0.7594(6) 0.7078(4) 0.0775(2) 0.0397(13) Uani 1 1 d . . . H22 H 0.6722 0.7419 0.0665 0.048 Uiso 1 1 calc R . . C23 C 0.7675(5) 0.6297(3) 0.1305(2) 0.0309(11) Uani 1 1 d . . . H23 H 0.6868 0.6091 0.1552 0.037 Uiso 1 1 calc R . . C24 C 0.8959(5) 0.5831(3) 0.14620(19) 0.0261(10) Uani 1 1 d . . . C25 C 1.0213(5) 0.2661(3) 0.2240(2) 0.0279(11) Uani 1 1 d . . . C26 C 1.0480(5) 0.2102(3) 0.2843(2) 0.0377(12) Uani 1 1 d . . . C27 C 1.1567(5) 0.1357(3) 0.2940(3) 0.0428(14) Uani 1 1 d . . . H27 H 1.1732 0.0978 0.3348 0.051 Uiso 1 1 calc R . . C28 C 1.2400(5) 0.1158(4) 0.2462(3) 0.0448(14) Uani 1 1 d . . . C29 C 1.2133(5) 0.1710(4) 0.1876(3) 0.0436(14) Uani 1 1 d . . . H29 H 1.2690 0.1576 0.1542 0.052 Uiso 1 1 calc R . . C30 C 1.1061(5) 0.2468(3) 0.1754(2) 0.0341(12) Uani 1 1 d . . . C31 C 0.9656(6) 0.2252(4) 0.3406(2) 0.0467(15) Uani 1 1 d . . . H31A H 1.0017 0.1779 0.3773 0.070 Uiso 1 1 calc R . . H31B H 0.8689 0.2183 0.3391 0.070 Uiso 1 1 calc R . . H31C H 0.9729 0.2892 0.3418 0.070 Uiso 1 1 calc R . . C32 C 1.3559(6) 0.0336(4) 0.2582(3) 0.0647(19) Uani 1 1 d . . . H32A H 1.3165 -0.0269 0.2737 0.097 Uiso 1 1 calc R . . H32B H 1.4129 0.0386 0.2887 0.097 Uiso 1 1 calc R . . H32C H 1.4127 0.0364 0.2200 0.097 Uiso 1 1 calc R . . C33 C 1.0912(6) 0.3064(4) 0.1104(2) 0.0454(14) Uani 1 1 d . . . H33A H 0.9974 0.3075 0.0999 0.068 Uiso 1 1 calc R . . H33B H 1.1572 0.2794 0.0834 0.068 Uiso 1 1 calc R . . H33C H 1.1092 0.3713 0.1051 0.068 Uiso 1 1 calc R . . C34 C 0.7502(4) 0.3612(3) 0.1466(2) 0.0251(10) Uani 1 1 d . . . C35 C 0.6567(5) 0.2919(3) 0.1714(2) 0.0305(11) Uani 1 1 d . . . C36 C 0.5615(5) 0.2820(4) 0.1355(2) 0.0379(13) Uani 1 1 d . . . H36 H 0.4994 0.2357 0.1529 0.045 Uiso 1 1 calc R . . C37 C 0.5538(5) 0.3373(4) 0.0749(2) 0.0367(12) Uani 1 1 d . . . C38 C 0.6465(5) 0.4023(3) 0.0507(2) 0.0311(11) Uani 1 1 d . . . H38 H 0.6431 0.4405 0.0090 0.037 Uiso 1 1 calc R . . C39 C 0.7450(5) 0.4142(3) 0.0847(2) 0.0282(11) Uani 1 1 d . . . C40 C 0.6594(6) 0.2235(3) 0.2365(2) 0.0389(13) Uani 1 1 d . . . H40A H 0.6122 0.2559 0.2653 0.058 Uiso 1 1 calc R . . H40B H 0.7551 0.2019 0.2465 0.058 Uiso 1 1 calc R . . H40C H 0.6127 0.1685 0.2396 0.058 Uiso 1 1 calc R . . C41 C 0.4500(6) 0.3251(5) 0.0359(3) 0.0602(18) Uani 1 1 d . . . H41A H 0.3596 0.3566 0.0457 0.090 Uiso 1 1 calc R . . H41B H 0.4442 0.2572 0.0442 0.090 Uiso 1 1 calc R . . H41C H 0.4788 0.3537 -0.0075 0.090 Uiso 1 1 calc R . . C42 C 0.8494(5) 0.4814(3) 0.0496(2) 0.0332(12) Uani 1 1 d . . . H42A H 0.8896 0.4638 0.0134 0.050 Uiso 1 1 calc R . . H42B H 0.9223 0.4771 0.0760 0.050 Uiso 1 1 calc R . . H42C H 0.8036 0.5468 0.0368 0.050 Uiso 1 1 calc R . . C43 C 1.0480(5) 0.6994(3) 0.2390(2) 0.0239(10) Uani 1 1 d . . . C44 C 1.0224(5) 0.7641(3) 0.18138(19) 0.0259(10) Uani 1 1 d . . . H44 H 0.9311 0.7838 0.1695 0.031 Uiso 1 1 calc R . . C45 C 1.1339(5) 0.7987(3) 0.1420(2) 0.0326(12) Uani 1 1 d . . . H45 H 1.1184 0.8425 0.1025 0.039 Uiso 1 1 calc R . . C46 C 1.2675(5) 0.7704(4) 0.1592(2) 0.0355(12) Uani 1 1 d . . . H46 H 1.3416 0.7973 0.1321 0.043 Uiso 1 1 calc R . . C47 C 1.2949(5) 0.7038(3) 0.2151(2) 0.0318(11) Uani 1 1 d . . . H47 H 1.3868 0.6830 0.2262 0.038 Uiso 1 1 calc R . . C48 C 1.1839(4) 0.6681(3) 0.2547(2) 0.0240(10) Uani 1 1 d . . . C49 C 1.1799(4) 0.5982(3) 0.3162(2) 0.0236(10) Uani 1 1 d . . . C50 C 1.2884(5) 0.5445(3) 0.3497(2) 0.0292(11) Uani 1 1 d . . . H50 H 1.3812 0.5490 0.3332 0.035 Uiso 1 1 calc R . . C51 C 1.2572(5) 0.4847(3) 0.4076(2) 0.0323(11) Uani 1 1 d . . . H51 H 1.3296 0.4484 0.4318 0.039 Uiso 1 1 calc R . . C52 C 1.1207(5) 0.4765(4) 0.4313(2) 0.0349(12) Uani 1 1 d . . . H52 H 1.1015 0.4351 0.4714 0.042 Uiso 1 1 calc R . . C53 C 1.0135(5) 0.5281(3) 0.3969(2) 0.0298(11) Uani 1 1 d . . . H53 H 0.9209 0.5220 0.4131 0.036 Uiso 1 1 calc R . . C54 C 1.0427(4) 0.5890(3) 0.33835(19) 0.0226(10) Uani 1 1 d . . . C55 C 0.7966(5) 0.8764(3) 0.2482(2) 0.0295(11) Uani 1 1 d . . . C56 C 0.8987(5) 0.9369(4) 0.2405(2) 0.0371(12) Uani 1 1 d . . . C57 C 0.9031(6) 1.0175(4) 0.1905(3) 0.0455(14) Uani 1 1 d . . . H57 H 0.9714 1.0581 0.1865 0.055 Uiso 1 1 calc R . . C58 C 0.8112(6) 1.0409(4) 0.1459(3) 0.0434(14) Uani 1 1 d . . . C59 C 0.7088(6) 0.9834(3) 0.1544(2) 0.0392(13) Uani 1 1 d . . . H59 H 0.6421 1.0001 0.1251 0.047 Uiso 1 1 calc R . . C60 C 0.6997(5) 0.9014(3) 0.2048(2) 0.0309(11) Uani 1 1 d . . . C61 C 1.0098(6) 0.9133(4) 0.2847(3) 0.0527(16) Uani 1 1 d . . . H61A H 1.0737 0.8592 0.2795 0.079 Uiso 1 1 calc R . . H61B H 0.9675 0.8971 0.3268 0.079 Uiso 1 1 calc R . . H61C H 1.0600 0.9685 0.2764 0.079 Uiso 1 1 calc R . . C62 C 0.8238(7) 1.1265(4) 0.0889(3) 0.0610(18) Uani 1 1 d . . . H62A H 0.8354 1.1820 0.1007 0.092 Uiso 1 1 calc R . . H62B H 0.7404 1.1397 0.0670 0.092 Uiso 1 1 calc R . . H62C H 0.9039 1.1129 0.0622 0.092 Uiso 1 1 calc R . . C63 C 0.5835(5) 0.8432(3) 0.2070(2) 0.0345(12) Uani 1 1 d . . . H63A H 0.6223 0.7830 0.2000 0.052 Uiso 1 1 calc R . . H63B H 0.5214 0.8790 0.1752 0.052 Uiso 1 1 calc R . . H63C H 0.5322 0.8301 0.2473 0.052 Uiso 1 1 calc R . . C64 C 0.7961(5) 0.7691(3) 0.3986(2) 0.0318(11) Uani 1 1 d . . . C65 C 0.9045(6) 0.7520(3) 0.4371(2) 0.0388(13) Uani 1 1 d . . . C66 C 0.8742(6) 0.7538(4) 0.4974(2) 0.0448(14) Uani 1 1 d . . . H66 H 0.9476 0.7424 0.5230 0.054 Uiso 1 1 calc R . . C67 C 0.7399(7) 0.7718(4) 0.5213(2) 0.0460(14) Uani 1 1 d . . . C68 C 0.6368(6) 0.7940(4) 0.4824(2) 0.0440(14) Uani 1 1 d . . . H68 H 0.5454 0.8096 0.4975 0.053 Uiso 1 1 calc R . . C69 C 0.6601(5) 0.7945(3) 0.4215(2) 0.0354(12) Uani 1 1 d . . . C70 C 1.0554(5) 0.7314(4) 0.4169(3) 0.0478(15) Uani 1 1 d . . . H70A H 1.1060 0.7820 0.4186 0.072 Uiso 1 1 calc R . . H70B H 1.0635 0.7288 0.3748 0.072 Uiso 1 1 calc R . . H70C H 1.0938 0.6703 0.4442 0.072 Uiso 1 1 calc R . . C71 C 0.7106(8) 0.7664(5) 0.5882(3) 0.0676(19) Uani 1 1 d . . . H71A H 0.6146 0.7915 0.5954 0.101 Uiso 1 1 calc R . . H71B H 0.7717 0.8042 0.5984 0.101 Uiso 1 1 calc R . . H71C H 0.7267 0.7000 0.6140 0.101 Uiso 1 1 calc R . . C72 C 0.5388(5) 0.8254(4) 0.3833(2) 0.0426(13) Uani 1 1 d . . . H72A H 0.4989 0.7693 0.3832 0.064 Uiso 1 1 calc R . . H72B H 0.5688 0.8611 0.3413 0.064 Uiso 1 1 calc R . . H72C H 0.4695 0.8660 0.4005 0.064 Uiso 1 1 calc R . . C73 C 0.8262(10) 0.0744(6) 0.5355(5) 0.110(3) Uani 1 1 d . . . H73A H 0.9033 0.1077 0.5120 0.165 Uiso 1 1 calc R . . H73B H 0.8595 0.0239 0.5716 0.165 Uiso 1 1 calc R . . H73C H 0.7567 0.1195 0.5486 0.165 Uiso 1 1 calc R . . C74 C 0.7659(16) 0.0334(7) 0.4978(5) 0.152(5) Uani 1 1 d . . . H74A H 0.8373 -0.0107 0.4838 0.182 Uiso 1 1 calc R . . H74B H 0.6926 -0.0041 0.5227 0.182 Uiso 1 1 calc R . . O5 O 0.7144(9) 0.0964(6) 0.4507(4) 0.135(3) Uani 1 1 d . . . C75 C 0.6340(12) 0.0687(8) 0.4007(6) 0.140(5) Uani 1 1 d . . . H75A H 0.5639 0.0250 0.4208 0.168 Uiso 1 1 calc R . . H75B H 0.5922 0.1255 0.3697 0.168 Uiso 1 1 calc R . . C76 C 0.7474(14) 0.0252(6) 0.3776(7) 0.174(6) Uani 1 1 d . . . H76A H 0.8084 0.0726 0.3540 0.260 Uiso 1 1 calc R . . H76B H 0.7204 -0.0071 0.3508 0.260 Uiso 1 1 calc R . . H76C H 0.7957 -0.0216 0.4112 0.260 Uiso 1 1 calc R . . C77 C 0.2814(16) 0.0294(9) 0.0760(7) 0.078(4) Uani 0.50 1 d PDU A -1 H77A H 0.3126 -0.0171 0.1140 0.116 Uiso 0.50 1 calc PR A -1 H77B H 0.1817 0.0311 0.0756 0.116 Uiso 0.50 1 calc PR A -1 H77C H 0.3032 0.0925 0.0733 0.116 Uiso 0.50 1 calc PR A -1 C78 C 0.352(2) 0.002(3) 0.0230(14) 0.103(8) Uani 0.50 1 d PDU A -1 H78A H 0.3342 -0.0632 0.0263 0.123 Uiso 0.50 1 calc PR A -1 H78B H 0.3171 0.0463 -0.0156 0.123 Uiso 0.50 1 calc PR A -1 O6 O 0.4953(16) 0.0048(18) 0.0229(9) 0.111(6) Uani 0.50 1 d PDU A -1 C79 C 0.574(3) -0.021(3) -0.0256(15) 0.120(10) Uani 0.50 1 d PDU A -1 H79A H 0.5398 0.0199 -0.0653 0.144 Uiso 0.50 1 calc PR A -1 H79B H 0.5667 -0.0880 -0.0214 0.144 Uiso 0.50 1 calc PR A -1 C80 C 0.718(3) -0.007(2) -0.0221(15) 0.131(12) Uani 0.50 1 d PDU A -1 H80A H 0.7205 0.0553 -0.0176 0.196 Uiso 0.50 1 calc PR A -1 H80B H 0.7724 -0.0113 -0.0598 0.196 Uiso 0.50 1 calc PR A -1 H80C H 0.7561 -0.0569 0.0132 0.196 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 0.0203(3) 0.0284(3) 0.0227(3) -0.0087(2) 0.0000(2) -0.0043(2) Ge2 0.0216(3) 0.0292(3) 0.0304(3) -0.0132(2) -0.0050(2) 0.0000(2) O1 0.0222(17) 0.0291(17) 0.0293(17) -0.0116(14) -0.0053(14) -0.0029(13) O2 0.0193(17) 0.0306(17) 0.0283(17) -0.0085(14) -0.0042(14) -0.0014(13) O3 0.0252(18) 0.0261(17) 0.0237(16) -0.0083(13) 0.0069(14) -0.0082(14) O4 0.0204(17) 0.0325(18) 0.0358(18) -0.0138(15) 0.0009(15) -0.0007(14) C1 0.015(2) 0.030(2) 0.028(2) -0.015(2) 0.0003(19) -0.0053(19) C2 0.016(2) 0.026(2) 0.019(2) -0.0060(19) -0.0019(18) -0.0024(18) C3 0.020(2) 0.024(2) 0.023(2) -0.0066(19) -0.0056(19) -0.0008(19) C4 0.013(2) 0.032(3) 0.021(2) -0.0094(19) -0.0004(18) -0.0032(19) C5 0.017(2) 0.026(2) 0.021(2) -0.0102(19) -0.0011(19) -0.0009(18) C6 0.020(3) 0.030(3) 0.025(2) -0.007(2) -0.003(2) -0.004(2) C7 0.015(2) 0.033(3) 0.026(2) -0.007(2) -0.0033(19) -0.0030(19) C8 0.028(3) 0.034(3) 0.029(3) -0.007(2) 0.005(2) -0.010(2) C9 0.025(3) 0.037(3) 0.029(3) -0.001(2) -0.002(2) -0.008(2) C10 0.020(3) 0.048(3) 0.022(2) -0.013(2) 0.003(2) -0.006(2) C11 0.019(3) 0.035(3) 0.030(3) -0.011(2) 0.002(2) -0.003(2) C12 0.010(2) 0.033(3) 0.025(2) -0.008(2) 0.0014(19) -0.0055(19) C13 0.019(2) 0.033(3) 0.025(2) -0.017(2) 0.004(2) -0.008(2) C14 0.024(3) 0.031(3) 0.031(3) -0.011(2) -0.001(2) -0.003(2) C15 0.018(3) 0.052(3) 0.055(3) -0.030(3) -0.001(2) -0.001(2) C16 0.022(3) 0.053(3) 0.058(4) -0.030(3) 0.014(3) -0.010(3) C17 0.033(3) 0.048(3) 0.031(3) -0.019(2) 0.014(2) -0.020(3) C18 0.025(3) 0.034(3) 0.027(2) -0.016(2) 0.002(2) -0.008(2) C19 0.041(3) 0.033(3) 0.020(2) -0.012(2) 0.003(2) -0.018(2) C20 0.052(4) 0.042(3) 0.025(3) -0.010(2) -0.001(3) -0.023(3) C21 0.074(4) 0.035(3) 0.021(3) -0.001(2) -0.011(3) -0.016(3) C22 0.052(4) 0.039(3) 0.026(3) -0.006(2) -0.017(3) 0.003(3) C23 0.033(3) 0.035(3) 0.027(3) -0.011(2) -0.007(2) 0.000(2) C24 0.034(3) 0.026(2) 0.021(2) -0.010(2) -0.007(2) -0.001(2) C25 0.026(3) 0.027(3) 0.033(3) -0.009(2) -0.003(2) -0.007(2) C26 0.035(3) 0.030(3) 0.046(3) -0.009(2) -0.001(3) -0.005(2) C27 0.034(3) 0.029(3) 0.057(4) -0.003(3) -0.003(3) -0.002(2) C28 0.027(3) 0.034(3) 0.071(4) -0.015(3) 0.000(3) -0.005(2) C29 0.028(3) 0.044(3) 0.067(4) -0.031(3) 0.005(3) -0.007(2) C30 0.027(3) 0.036(3) 0.044(3) -0.018(2) 0.000(2) -0.010(2) C31 0.050(4) 0.045(3) 0.032(3) 0.001(2) -0.008(3) 0.011(3) C32 0.032(3) 0.044(4) 0.106(5) -0.013(4) -0.004(4) 0.010(3) C33 0.037(3) 0.064(4) 0.038(3) -0.026(3) 0.003(3) 0.003(3) C34 0.017(2) 0.034(3) 0.027(2) -0.015(2) 0.005(2) -0.005(2) C35 0.028(3) 0.033(3) 0.032(3) -0.012(2) -0.002(2) -0.004(2) C36 0.031(3) 0.040(3) 0.043(3) -0.011(2) 0.003(2) -0.018(2) C37 0.025(3) 0.051(3) 0.040(3) -0.020(3) -0.003(2) -0.009(2) C38 0.029(3) 0.041(3) 0.024(2) -0.011(2) -0.004(2) -0.004(2) C39 0.026(3) 0.034(3) 0.028(2) -0.015(2) 0.004(2) -0.008(2) C40 0.043(3) 0.038(3) 0.037(3) -0.009(2) 0.002(3) -0.019(2) C41 0.049(4) 0.082(5) 0.050(4) -0.007(3) -0.019(3) -0.029(3) C42 0.037(3) 0.044(3) 0.024(2) -0.016(2) 0.003(2) -0.014(2) C43 0.022(3) 0.027(2) 0.028(2) -0.014(2) -0.001(2) -0.006(2) C44 0.026(3) 0.029(3) 0.022(2) -0.007(2) -0.004(2) -0.005(2) C45 0.038(3) 0.031(3) 0.027(3) -0.002(2) -0.006(2) -0.010(2) C46 0.027(3) 0.046(3) 0.033(3) -0.008(2) 0.005(2) -0.019(2) C47 0.020(3) 0.039(3) 0.038(3) -0.013(2) -0.005(2) -0.003(2) C48 0.019(2) 0.029(2) 0.024(2) -0.009(2) -0.001(2) -0.0051(19) C49 0.016(2) 0.029(2) 0.028(2) -0.011(2) -0.005(2) -0.0008(19) C50 0.018(3) 0.042(3) 0.030(3) -0.015(2) -0.005(2) -0.001(2) C51 0.022(3) 0.046(3) 0.026(3) -0.006(2) -0.009(2) 0.001(2) C52 0.034(3) 0.042(3) 0.024(3) -0.002(2) -0.003(2) -0.005(2) C53 0.019(3) 0.040(3) 0.028(3) -0.009(2) 0.000(2) -0.004(2) C54 0.015(2) 0.031(3) 0.024(2) -0.011(2) -0.0013(19) -0.0015(19) C55 0.029(3) 0.027(3) 0.034(3) -0.012(2) -0.005(2) 0.002(2) C56 0.031(3) 0.037(3) 0.048(3) -0.019(3) -0.002(3) -0.006(2) C57 0.046(4) 0.035(3) 0.060(4) -0.019(3) 0.008(3) -0.017(3) C58 0.046(4) 0.031(3) 0.047(3) -0.011(3) 0.012(3) 0.000(3) C59 0.042(3) 0.029(3) 0.043(3) -0.009(2) 0.000(3) 0.002(2) C60 0.031(3) 0.026(3) 0.034(3) -0.010(2) -0.003(2) 0.005(2) C61 0.040(4) 0.051(4) 0.074(4) -0.022(3) -0.010(3) -0.015(3) C62 0.072(5) 0.035(3) 0.060(4) -0.002(3) 0.016(4) -0.003(3) C63 0.032(3) 0.035(3) 0.034(3) -0.006(2) -0.012(2) 0.001(2) C64 0.031(3) 0.033(3) 0.034(3) -0.015(2) -0.005(2) 0.003(2) C65 0.044(3) 0.035(3) 0.043(3) -0.019(2) -0.010(3) 0.001(2) C66 0.054(4) 0.040(3) 0.046(3) -0.020(3) -0.022(3) 0.009(3) C67 0.061(4) 0.042(3) 0.038(3) -0.020(3) -0.005(3) 0.001(3) C68 0.051(4) 0.040(3) 0.042(3) -0.018(3) 0.006(3) -0.005(3) C69 0.042(3) 0.031(3) 0.033(3) -0.013(2) 0.001(2) -0.002(2) C70 0.034(3) 0.065(4) 0.055(4) -0.033(3) -0.020(3) 0.005(3) C71 0.091(5) 0.071(4) 0.050(4) -0.036(3) -0.004(4) -0.001(4) C72 0.030(3) 0.052(3) 0.049(3) -0.028(3) -0.001(3) 0.009(3) C73 0.110(7) 0.101(7) 0.130(8) -0.054(6) 0.000(6) -0.014(6) C74 0.288(18) 0.068(6) 0.092(8) -0.016(6) 0.002(10) -0.028(8) O5 0.163(7) 0.161(7) 0.098(5) -0.054(5) 0.023(5) -0.068(6) C75 0.133(10) 0.089(7) 0.162(11) -0.006(7) 0.024(9) -0.005(7) C76 0.171(12) 0.041(5) 0.281(16) -0.024(7) 0.022(12) -0.017(6) C77 0.113(11) 0.048(8) 0.076(9) -0.021(7) -0.038(8) 0.006(8) C78 0.147(17) 0.11(2) 0.050(11) -0.007(12) -0.012(16) -0.04(2) O6 0.135(13) 0.136(11) 0.071(9) -0.051(9) -0.025(9) 0.015(11) C79 0.19(2) 0.088(17) 0.058(13) 0.002(11) 0.03(2) -0.03(2) C80 0.17(2) 0.055(13) 0.13(2) -0.003(13) 0.049(19) -0.019(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O3 1.828(3) . ? Ge1 C34 1.967(4) . ? Ge1 C25 1.973(5) . ? Ge1 C1 2.046(4) . ? Ge2 O4 1.826(3) . ? Ge2 C64 1.961(5) . ? Ge2 C55 1.975(5) . ? Ge2 C4 2.057(4) . ? O1 C3 1.486(5) . ? O1 O2 1.496(4) . ? O2 C6 1.466(5) . ? O3 C3 1.363(5) . ? O4 C6 1.377(5) . ? C1 C13 1.515(6) . ? C1 C24 1.519(6) . ? C1 C2 1.567(6) . ? C2 C5 1.540(6) . ? C2 C3 1.554(6) . ? C3 C7 1.504(6) . ? C4 C54 1.502(6) . ? C4 C43 1.516(6) . ? C4 C5 1.572(6) . ? C5 C6 1.547(6) . ? C6 C12 1.505(6) . ? C7 C12 1.378(6) . ? C7 C8 1.381(6) . ? C8 C9 1.397(6) . ? C9 C10 1.377(6) . ? C10 C11 1.395(6) . ? C11 C12 1.379(6) . ? C13 C14 1.393(6) . ? C13 C18 1.399(6) . ? C14 C15 1.393(6) . ? C15 C16 1.380(7) . ? C16 C17 1.364(7) . ? C17 C18 1.397(6) . ? C18 C19 1.461(7) . ? C19 C20 1.386(6) . ? C19 C24 1.415(6) . ? C20 C21 1.375(8) . ? C21 C22 1.382(7) . ? C22 C23 1.395(6) . ? C23 C24 1.379(6) . ? C25 C30 1.399(6) . ? C25 C26 1.408(6) . ? C26 C27 1.407(7) . ? C26 C31 1.511(7) . ? C27 C28 1.379(7) . ? C28 C29 1.375(7) . ? C28 C32 1.526(7) . ? C29 C30 1.411(7) . ? C30 C33 1.492(7) . ? C34 C39 1.398(6) . ? C34 C35 1.422(6) . ? C35 C36 1.380(7) . ? C35 C40 1.524(6) . ? C36 C37 1.383(7) . ? C37 C38 1.372(6) . ? C37 C41 1.510(7) . ? C38 C39 1.387(6) . ? C39 C42 1.520(6) . ? C43 C44 1.396(6) . ? C43 C48 1.402(6) . ? C44 C45 1.388(6) . ? C45 C46 1.387(7) . ? C46 C47 1.382(6) . ? C47 C48 1.391(6) . ? C48 C49 1.469(6) . ? C49 C50 1.390(6) . ? C49 C54 1.397(6) . ? C50 C51 1.378(6) . ? C51 C52 1.396(6) . ? C52 C53 1.381(6) . ? C53 C54 1.390(6) . ? C55 C60 1.394(6) . ? C55 C56 1.409(6) . ? C56 C57 1.378(7) . ? C56 C61 1.514(7) . ? C57 C58 1.379(8) . ? C58 C59 1.378(7) . ? C58 C62 1.520(7) . ? C59 C60 1.398(6) . ? C60 C63 1.525(7) . ? C64 C65 1.415(7) . ? C64 C69 1.425(7) . ? C65 C66 1.401(7) . ? C65 C70 1.520(7) . ? C66 C67 1.393(7) . ? C67 C68 1.372(8) . ? C67 C71 1.518(7) . ? C68 C69 1.396(7) . ? C69 C72 1.500(7) . ? C73 C74 1.438(14) . ? C74 O5 1.289(12) . ? O5 C75 1.664(14) . ? C75 C76 1.349(12) . ? C77 C78 1.48(2) . ? C78 O6 1.42(2) . ? O6 C79 1.41(2) . ? C79 C80 1.48(2) . ? 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 O3 Ge1 C34 102.34(15) . . ? O3 Ge1 C25 108.84(16) . . ? C34 Ge1 C25 112.64(18) . . ? O3 Ge1 C1 91.84(15) . . ? C34 Ge1 C1 124.70(18) . . ? C25 Ge1 C1 112.39(18) . . ? O4 Ge2 C64 99.78(17) . . ? O4 Ge2 C55 109.43(17) . . ? C64 Ge2 C55 115.37(19) . . ? O4 Ge2 C4 92.57(15) . . ? C64 Ge2 C4 123.30(18) . . ? C55 Ge2 C4 111.71(17) . . ? C3 O1 O2 110.8(3) . . ? C6 O2 O1 109.3(3) . . ? C3 O3 Ge1 113.5(2) . . ? C6 O4 Ge2 113.1(3) . . ? C13 C1 C24 102.7(3) . . ? C13 C1 C2 113.6(4) . . ? C24 C1 C2 117.1(4) . . ? C13 C1 Ge1 108.8(3) . . ? C24 C1 Ge1 114.4(3) . . ? C2 C1 Ge1 100.5(3) . . ? C5 C2 C3 107.3(3) . . ? C5 C2 C1 116.0(3) . . ? C3 C2 C1 110.9(3) . . ? O3 C3 O1 103.5(3) . . ? O3 C3 C7 114.6(3) . . ? O1 C3 C7 106.4(3) . . ? O3 C3 C2 112.9(3) . . ? O1 C3 C2 107.8(3) . . ? C7 C3 C2 110.8(4) . . ? C54 C4 C43 102.8(3) . . ? C54 C4 C5 117.3(4) . . ? C43 C4 C5 112.9(3) . . ? C54 C4 Ge2 117.5(3) . . ? C43 C4 Ge2 109.6(3) . . ? C5 C4 Ge2 97.1(3) . . ? C2 C5 C6 108.2(3) . . ? C2 C5 C4 118.4(4) . . ? C6 C5 C4 111.8(3) . . ? O4 C6 O2 104.9(3) . . ? O4 C6 C12 114.0(4) . . ? O2 C6 C12 105.4(3) . . ? O4 C6 C5 110.8(3) . . ? O2 C6 C5 104.6(3) . . ? C12 C6 C5 115.8(4) . . ? C12 C7 C8 121.6(4) . . ? C12 C7 C3 111.9(4) . . ? C8 C7 C3 126.6(4) . . ? C7 C8 C9 117.3(4) . . ? C10 C9 C8 121.7(4) . . ? C9 C10 C11 120.0(4) . . ? C12 C11 C10 118.6(4) . . ? C7 C12 C11 120.9(4) . . ? C7 C12 C6 112.5(4) . . ? C11 C12 C6 126.6(4) . . ? C14 C13 C18 119.3(4) . . ? C14 C13 C1 130.2(4) . . ? C18 C13 C1 110.5(4) . . ? C15 C14 C13 119.2(4) . . ? C16 C15 C14 120.7(5) . . ? C17 C16 C15 120.9(5) . . ? C16 C17 C18 119.4(5) . . ? C17 C18 C13 120.5(4) . . ? C17 C18 C19 131.0(4) . . ? C13 C18 C19 108.3(4) . . ? C20 C19 C24 120.1(5) . . ? C20 C19 C18 130.6(4) . . ? C24 C19 C18 109.3(4) . . ? C21 C20 C19 118.8(5) . . ? C20 C21 C22 121.2(5) . . ? C21 C22 C23 121.0(5) . . ? C24 C23 C22 118.2(5) . . ? C23 C24 C19 120.6(4) . . ? C23 C24 C1 130.4(4) . . ? C19 C24 C1 109.0(4) . . ? C30 C25 C26 118.6(4) . . ? C30 C25 Ge1 117.3(3) . . ? C26 C25 Ge1 124.1(4) . . ? C27 C26 C25 119.5(5) . . ? C27 C26 C31 116.9(5) . . ? C25 C26 C31 123.6(4) . . ? C28 C27 C26 122.2(5) . . ? C29 C28 C27 117.9(5) . . ? C29 C28 C32 121.2(5) . . ? C27 C28 C32 120.9(6) . . ? C28 C29 C30 122.2(5) . . ? C25 C30 C29 119.6(5) . . ? C25 C30 C33 122.3(4) . . ? C29 C30 C33 118.1(5) . . ? C39 C34 C35 117.4(4) . . ? C39 C34 Ge1 126.1(3) . . ? C35 C34 Ge1 116.5(3) . . ? C36 C35 C34 120.1(4) . . ? C36 C35 C40 116.9(4) . . ? C34 C35 C40 122.9(4) . . ? C35 C36 C37 122.0(4) . . ? C38 C37 C36 117.8(5) . . ? C38 C37 C41 120.7(5) . . ? C36 C37 C41 121.5(5) . . ? C37 C38 C39 122.3(4) . . ? C38 C39 C34 120.3(4) . . ? C38 C39 C42 115.9(4) . . ? C34 C39 C42 123.6(4) . . ? C44 C43 C48 119.9(4) . . ? C44 C43 C4 130.1(4) . . ? C48 C43 C4 110.0(4) . . ? C45 C44 C43 118.4(4) . . ? C46 C45 C44 121.1(4) . . ? C47 C46 C45 121.3(4) . . ? C46 C47 C48 118.0(4) . . ? C47 C48 C43 121.3(4) . . ? C47 C48 C49 130.6(4) . . ? C43 C48 C49 108.1(4) . . ? C50 C49 C54 121.9(4) . . ? C50 C49 C48 129.1(4) . . ? C54 C49 C48 108.9(4) . . ? C51 C50 C49 117.8(4) . . ? C50 C51 C52 121.1(4) . . ? C53 C52 C51 120.6(4) . . ? C52 C53 C54 119.3(4) . . ? C53 C54 C49 119.1(4) . . ? C53 C54 C4 130.7(4) . . ? C49 C54 C4 110.2(4) . . ? C60 C55 C56 118.4(4) . . ? C60 C55 Ge2 125.0(4) . . ? C56 C55 Ge2 116.3(4) . . ? C57 C56 C55 120.2(5) . . ? C57 C56 C61 118.2(5) . . ? C55 C56 C61 121.6(5) . . ? C56 C57 C58 122.0(5) . . ? C59 C58 C57 117.8(5) . . ? C59 C58 C62 121.1(6) . . ? C57 C58 C62 121.1(5) . . ? C58 C59 C60 122.1(5) . . ? C55 C60 C59 119.5(5) . . ? C55 C60 C63 124.3(4) . . ? C59 C60 C63 116.2(4) . . ? C65 C64 C69 118.3(4) . . ? C65 C64 Ge2 125.8(4) . . ? C69 C64 Ge2 115.9(4) . . ? C66 C65 C64 119.5(5) . . ? C66 C65 C70 116.8(5) . . ? C64 C65 C70 123.7(4) . . ? C67 C66 C65 122.2(5) . . ? C68 C67 C66 117.7(5) . . ? C68 C67 C71 121.9(6) . . ? C66 C67 C71 120.4(6) . . ? C67 C68 C69 123.0(5) . . ? C68 C69 C64 119.1(5) . . ? C68 C69 C72 117.2(5) . . ? C64 C69 C72 123.7(4) . . ? O5 C74 C73 112.8(9) . . ? C74 O5 C75 122.8(9) . . ? C76 C75 O5 95.6(10) . . ? O6 C78 C77 108.1(17) . . ? C79 O6 C78 113.3(19) . . ? O6 C79 C80 107(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.803 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.084