#------------------------------------------------------------------------------ #$Date: 2019-11-17 15:43:18 +0200 (Sun, 17 Nov 2019) $ #$Revision: 230955 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/81/1548139.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1548139 loop_ _publ_author_name 'Eibel, Anna' 'Radebner, Judith' 'Haas, Michael' 'Fast, David E.' 'Frei\&smuth, Hilde' 'Stadler, Eduard' 'Faschauner, Paul' 'Torvisco, Ana' 'Lamparth, Iris' 'Moszner, Norbert' 'Stueger, Harald' 'Gescheidt, Georg' _publ_section_title ; From mono- to tetraacylgermanes: extending the scope of visible light photoinitiators ; _journal_issue 1 _journal_name_full 'Polymer Chemistry' _journal_page_first 38 _journal_paper_doi 10.1039/C7PY01590A _journal_volume 9 _journal_year 2018 _chemical_formula_moiety 'C32 H38 Ge O3' _chemical_formula_sum 'C32 H38 Ge O3' _chemical_formula_weight 543.21 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-07-12 deposited with the CCDC. 2017-11-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 14.4530(6) _cell_length_b 24.1484(10) _cell_length_c 24.5040(10) _cell_measurement_reflns_used 9135 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.02 _cell_measurement_theta_min 2.20 _cell_volume 8552.3(6) _computing_cell_refinement 'Bruker SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXT-2014/5 _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer monochromator' _diffrn_radiation_source 'Incoatec microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 424078 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.184 _diffrn_reflns_theta_min 1.636 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_T_max 0.741 _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.266 _exptl_crystal_description block _exptl_crystal_F_000 3432 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.090 _refine_diff_density_max 1.946 _refine_diff_density_min -1.793 _refine_diff_density_rms 0.083 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.068(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1003 _refine_ls_number_reflns 32647 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0443 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+6.1022P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.1051 _reflns_Friedel_coverage 0.866 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 27060 _reflns_number_total 32647 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7py01590a2.cif _cod_data_source_block AT667 _cod_depositor_comments 'Adding full bibliography for 1548139.cif.' _cod_database_code 1548139 _publcif_datablock.id {85c898e5-ee29-4528-b679-46ea93ebb3f7} _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.852 _shelx_estimated_absorpt_t_max 0.907 _shelx_res_file ; AT667.res created by SHELXL-2014/7 TITL AT667_a.res in P2(1)2(1)2(1) REM Old TITL AT667 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.100, Rweak 0.019, Alpha 0.007, Orientation as input REM Flack x = 0.092 ( 0.003 ) from Parsons' quotients REM Formula found by SHELXT: C96 Ge3 O9 CELL 0.71073 14.453 24.1484 24.504 90 90 90 ZERR 12 0.0006 0.001 0.001 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Ge O UNIT 384 456 12 36 L.S. 10 PLAN 20 SIZE 0.09 0.1 0.15 TEMP -173.14 BOND $H LIST 4 HTAB fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 1 1 OMIT 0 2 0 OMIT 8 0 0 OMIT 5 7 1 OMIT 1 0 9 OMIT -5 7 1 OMIT 0 8 16 OMIT 0 0 8 OMIT 0 4 12 OMIT 0 15 18 OMIT 7 3 0 OMIT 1 1 0 OMIT 0 9 18 OMIT 0 3 26 OMIT 5 1 6 OMIT 0 4 7 OMIT 0 7 26 OMIT 0 5 23 OMIT 3 1 0 OMIT 0 14 17 OMIT 1 3 0 WGHT 0.040500 6.104700 BASF 0.06882 FVAR 0.14580 GE1 3 0.535659 0.604177 0.942088 11.00000 0.01459 0.01457 = 0.02828 -0.00136 0.00123 -0.00238 C1 1 0.423418 0.651861 0.925165 11.00000 0.01770 0.02333 = 0.01765 0.00176 0.00001 -0.00088 O1 4 0.355962 0.625615 0.910651 11.00000 0.02201 0.02895 = 0.04618 0.00384 -0.00942 -0.00709 GE2 3 0.493655 0.607301 0.619260 11.00000 0.02398 0.01382 = 0.02808 -0.00430 0.00513 -0.00114 C2 1 0.532953 0.577540 1.020662 11.00000 0.01893 0.02108 = 0.03797 0.00964 -0.00184 -0.00608 O2 4 0.550794 0.610575 1.056409 11.00000 0.06077 0.03185 = 0.03893 0.01170 -0.01427 -0.01945 GE3 3 0.478442 0.607280 0.283951 11.00000 0.01575 0.01219 = 0.02079 -0.00110 0.00024 0.00070 C3 1 0.662928 0.639129 0.935083 11.00000 0.01793 0.02008 = 0.01482 -0.00215 0.00183 -0.00297 O3 4 0.728251 0.608603 0.943147 11.00000 0.01796 0.02704 = 0.03897 0.00491 -0.00021 0.00214 O4 4 0.673718 0.637101 0.592660 11.00000 0.02417 0.03025 = 0.05160 0.00658 0.01324 0.00834 C4 1 0.421014 0.713682 0.927983 11.00000 0.01190 0.02373 = 0.01804 -0.00151 -0.00235 0.00077 O5 4 0.308322 0.593486 0.599994 11.00000 0.04678 0.05921 = 0.11533 0.05274 -0.04995 -0.03639 C5 1 0.438478 0.744538 0.880722 11.00000 0.01536 0.02331 = 0.01906 -0.00086 -0.00321 0.00111 O6 4 0.502197 0.625392 0.735434 11.00000 0.08042 0.02572 = 0.03213 0.00157 0.00871 0.01593 C6 1 0.433756 0.802383 0.883959 11.00000 0.02263 0.02230 = 0.02605 0.00192 -0.00563 0.00038 AFIX 43 H6 2 0.446008 0.823725 0.852202 11.00000 -1.20000 AFIX 0 O7 4 0.300117 0.647214 0.271899 11.00000 0.01544 0.02434 = 0.04467 0.00403 -0.00340 -0.00205 C7 1 0.411699 0.829417 0.932214 11.00000 0.02227 0.02056 = 0.03678 -0.00490 -0.00870 0.00372 O8 4 0.464886 0.623696 0.399328 11.00000 0.04186 0.01705 = 0.02661 -0.00044 0.00734 -0.00313 C8 1 0.393284 0.797401 0.978507 11.00000 0.02017 0.03131 = 0.02639 -0.01029 -0.00185 0.00655 AFIX 43 H8 2 0.377119 0.815382 1.011646 11.00000 -1.20000 AFIX 0 O9 4 0.656144 0.582500 0.252686 11.00000 0.02738 0.02822 = 0.05784 0.00651 0.01322 0.01115 C9 1 0.398038 0.739956 0.977250 11.00000 0.01515 0.02965 = 0.01951 -0.00162 -0.00165 0.00284 C10 1 0.460385 0.716721 0.827309 11.00000 0.02593 0.03215 = 0.01661 -0.00171 0.00067 -0.00121 AFIX 137 H10A 2 0.497804 0.741624 0.804725 11.00000 -1.50000 H10B 2 0.402665 0.707904 0.808205 11.00000 -1.50000 H10C 2 0.494952 0.682518 0.834213 11.00000 -1.50000 AFIX 0 C12 1 0.378942 0.706386 1.027682 11.00000 0.02815 0.04105 = 0.01926 -0.00227 0.00533 0.00448 AFIX 137 H12A 2 0.358687 0.731003 1.057147 11.00000 -1.50000 H12B 2 0.435451 0.687013 1.038821 11.00000 -1.50000 H12C 2 0.330242 0.679260 1.019950 11.00000 -1.50000 AFIX 0 C11 1 0.407822 0.891965 0.934877 11.00000 0.04583 0.02232 = 0.05493 -0.00729 -0.01076 0.00590 AFIX 137 H11A 2 0.354506 0.903366 0.956885 11.00000 -1.50000 H11B 2 0.401674 0.906998 0.897906 11.00000 -1.50000 H11C 2 0.464774 0.906048 0.951565 11.00000 -1.50000 AFIX 0 C13 1 0.511236 0.518406 1.034837 11.00000 0.02131 0.02302 = 0.02750 0.00737 -0.00059 -0.00500 C14 1 0.583853 0.482929 1.050147 11.00000 0.02082 0.02519 = 0.02741 0.00647 -0.00169 -0.00365 C15 1 0.561361 0.429435 1.067686 11.00000 0.02704 0.02600 = 0.02575 0.00599 -0.00071 0.00026 AFIX 43 H15 2 0.609816 0.404490 1.076735 11.00000 -1.20000 AFIX 0 C16 1 0.470388 0.411809 1.072231 11.00000 0.03152 0.02402 = 0.01815 0.00250 -0.00147 -0.00714 C17 1 0.399964 0.448257 1.057052 11.00000 0.02370 0.02451 = 0.02530 0.00183 0.00361 -0.00811 AFIX 43 H17 2 0.337376 0.436631 1.060059 11.00000 -1.20000 AFIX 0 C18 1 0.419145 0.501291 1.037592 11.00000 0.02127 0.02348 = 0.02938 0.00344 -0.00028 -0.00514 C19 1 0.683746 0.501532 1.048522 11.00000 0.01936 0.03826 = 0.04939 0.01071 -0.00180 -0.00481 AFIX 137 H19A 2 0.724379 0.469221 1.051864 11.00000 -1.50000 H19B 2 0.695563 0.527072 1.078810 11.00000 -1.50000 H19C 2 0.696017 0.520356 1.013838 11.00000 -1.50000 AFIX 0 C20 1 0.446340 0.355586 1.094637 11.00000 0.04461 0.02523 = 0.02615 0.00687 -0.00482 -0.01045 AFIX 137 H20A 2 0.391941 0.341079 1.075517 11.00000 -1.50000 H20B 2 0.432732 0.358702 1.133696 11.00000 -1.50000 H20C 2 0.498691 0.330372 1.089285 11.00000 -1.50000 AFIX 0 C22 1 0.672575 0.697766 0.916287 11.00000 0.01271 0.01904 = 0.01800 -0.00129 0.00022 -0.00365 C21 1 0.341053 0.539818 1.022583 11.00000 0.01920 0.03061 = 0.07215 0.01282 -0.00189 -0.00418 AFIX 137 H21A 2 0.282013 0.520101 1.025625 11.00000 -1.50000 H21B 2 0.349404 0.552731 0.984989 11.00000 -1.50000 H21C 2 0.341001 0.571657 1.047381 11.00000 -1.50000 AFIX 0 C23 1 0.652575 0.741010 0.952634 11.00000 0.01543 0.02086 = 0.01943 0.00095 0.00072 -0.00272 C24 1 0.655436 0.795349 0.933329 11.00000 0.02199 0.01891 = 0.02324 -0.00033 -0.00075 -0.00103 AFIX 43 H24 2 0.640894 0.824894 0.957448 11.00000 -1.20000 AFIX 0 C25 1 0.679086 0.807219 0.879603 11.00000 0.02098 0.02361 = 0.02580 0.00538 -0.00225 -0.00393 C26 1 0.700903 0.763728 0.844916 11.00000 0.02131 0.02956 = 0.01719 0.00424 -0.00085 -0.00707 AFIX 43 H26 2 0.718665 0.771678 0.808421 11.00000 -1.20000 AFIX 0 C27 1 0.697529 0.708623 0.862052 11.00000 0.01536 0.02663 = 0.01695 -0.00167 -0.00029 -0.00423 C28 1 0.634844 0.729967 1.012102 11.00000 0.02663 0.02249 = 0.01936 -0.00127 0.00366 -0.00199 AFIX 137 H28A 2 0.586451 0.755012 1.025353 11.00000 -1.50000 H28B 2 0.691838 0.736172 1.032886 11.00000 -1.50000 H28C 2 0.614684 0.691518 1.016830 11.00000 -1.50000 AFIX 0 C29 1 0.680665 0.866844 0.859865 11.00000 0.04427 0.02592 = 0.03739 0.01193 -0.00296 -0.00555 AFIX 137 H29A 2 0.712077 0.868754 0.824472 11.00000 -1.50000 H29B 2 0.713844 0.889838 0.886379 11.00000 -1.50000 H29C 2 0.617091 0.880405 0.856011 11.00000 -1.50000 AFIX 0 C31 1 0.525702 0.543738 0.888250 11.00000 0.02781 0.03020 = 0.06654 -0.02088 -0.00301 -0.00399 AFIX 23 H31A 2 0.475628 0.518485 0.900112 11.00000 -1.20000 H31B 2 0.506725 0.559972 0.852880 11.00000 -1.20000 AFIX 0 C30 1 0.717370 0.662260 0.822393 11.00000 0.02929 0.03404 = 0.02025 -0.00311 0.00532 -0.00412 AFIX 137 H30A 2 0.739619 0.677832 0.787871 11.00000 -1.50000 H30B 2 0.660600 0.641090 0.815834 11.00000 -1.50000 H30C 2 0.764767 0.637768 0.837734 11.00000 -1.50000 AFIX 0 C32 1 0.611813 0.509797 0.879020 11.00000 0.04690 0.04076 = 0.05987 -0.01646 0.00471 -0.00060 AFIX 137 H32A 2 0.600037 0.482193 0.850538 11.00000 -1.50000 H32B 2 0.628947 0.490982 0.912984 11.00000 -1.50000 H32C 2 0.662442 0.534147 0.867537 11.00000 -1.50000 AFIX 0 C33 1 0.599148 0.659132 0.599709 11.00000 0.02170 0.01982 = 0.02111 -0.00044 0.00441 0.00163 C34 1 0.362608 0.631766 0.601197 11.00000 0.02566 0.03689 = 0.02386 0.00786 -0.00668 -0.01216 C35 1 0.504811 0.589576 0.700557 11.00000 0.02994 0.02019 = 0.03481 0.00605 0.00896 0.00601 C36 1 0.586605 0.720651 0.595898 11.00000 0.01225 0.01679 = 0.01919 0.00000 0.00269 -0.00075 C37 1 0.551898 0.743796 0.547402 11.00000 0.01270 0.02320 = 0.01632 -0.00158 0.00191 -0.00220 C38 1 0.538995 0.800968 0.545427 11.00000 0.01724 0.02424 = 0.01890 0.00308 0.00024 -0.00015 AFIX 43 H38 2 0.514516 0.817108 0.513153 11.00000 -1.20000 AFIX 0 C39 1 0.560934 0.835157 0.589383 11.00000 0.01816 0.01943 = 0.02450 0.00123 0.00303 -0.00204 C40 1 0.596753 0.811017 0.636208 11.00000 0.01730 0.02440 = 0.02110 -0.00440 0.00143 -0.00425 AFIX 43 H40 2 0.613402 0.834010 0.666094 11.00000 -1.20000 AFIX 0 C41 1 0.608949 0.754056 0.640583 11.00000 0.01383 0.02465 = 0.01593 0.00058 0.00121 -0.00207 C42 1 0.531640 0.708612 0.497983 11.00000 0.02182 0.02962 = 0.01797 -0.00294 0.00075 -0.00242 AFIX 137 H42A 2 0.485992 0.727385 0.474912 11.00000 -1.50000 H42B 2 0.506983 0.672730 0.509710 11.00000 -1.50000 H42C 2 0.588781 0.702857 0.477213 11.00000 -1.50000 AFIX 0 C44 1 0.643811 0.729407 0.693658 11.00000 0.02202 0.03805 = 0.01797 0.00352 -0.00135 -0.00323 AFIX 137 H44A 2 0.676820 0.757861 0.714494 11.00000 -1.50000 H44B 2 0.685890 0.698625 0.685703 11.00000 -1.50000 H44C 2 0.591253 0.715805 0.715078 11.00000 -1.50000 AFIX 0 C43 1 0.545193 0.896866 0.586042 11.00000 0.03655 0.02103 = 0.03935 -0.00065 0.00184 -0.00031 AFIX 137 H43A 2 0.547549 0.912834 0.622783 11.00000 -1.50000 H43B 2 0.484403 0.904111 0.569828 11.00000 -1.50000 H43C 2 0.593409 0.913710 0.563345 11.00000 -1.50000 AFIX 0 C45 1 0.336674 0.689847 0.586143 11.00000 0.01328 0.03811 = 0.01840 0.00430 -0.00037 -0.00621 C46 1 0.300834 0.700836 0.533432 11.00000 0.01355 0.03596 = 0.01871 -0.00038 0.00037 -0.00253 C47 1 0.282077 0.755795 0.519504 11.00000 0.01496 0.03765 = 0.01843 0.00201 0.00083 0.00049 AFIX 43 H47 2 0.259512 0.763845 0.483966 11.00000 -1.20000 AFIX 0 C48 1 0.295442 0.799084 0.556102 11.00000 0.01488 0.03325 = 0.02877 0.00022 0.00122 0.00181 C49 1 0.327224 0.786355 0.608195 11.00000 0.01398 0.03901 = 0.02479 -0.00637 -0.00094 0.00217 AFIX 43 H49 2 0.334501 0.815433 0.633953 11.00000 -1.20000 AFIX 0 C50 1 0.348566 0.732877 0.623754 11.00000 0.01208 0.04296 = 0.01676 0.00048 0.00046 -0.00223 C51 1 0.285172 0.655868 0.491861 11.00000 0.02300 0.03465 = 0.02305 -0.00169 -0.00303 -0.00480 AFIX 137 H51A 2 0.264068 0.672418 0.457531 11.00000 -1.50000 H51B 2 0.238086 0.630098 0.505396 11.00000 -1.50000 H51C 2 0.343170 0.635827 0.485605 11.00000 -1.50000 AFIX 0 C54 1 0.519753 0.529719 0.715423 11.00000 0.02132 0.01875 = 0.03042 0.00567 0.00385 0.00639 C53 1 0.382505 0.721180 0.680988 11.00000 0.01827 0.05513 = 0.01717 0.00004 -0.00109 -0.00333 AFIX 137 H53A 2 0.368312 0.752834 0.704574 11.00000 -1.50000 H53B 2 0.449538 0.715108 0.680330 11.00000 -1.50000 H53C 2 0.351655 0.688020 0.695146 11.00000 -1.50000 AFIX 0 C52 1 0.276139 0.858109 0.539714 11.00000 0.03338 0.03644 = 0.04127 0.00154 -0.00252 0.00392 AFIX 137 H52A 2 0.246727 0.877669 0.570160 11.00000 -1.50000 H52B 2 0.234740 0.858506 0.508042 11.00000 -1.50000 H52C 2 0.334394 0.876539 0.530281 11.00000 -1.50000 AFIX 0 C55 1 0.443115 0.496088 0.728157 11.00000 0.02191 0.02613 = 0.03635 0.00750 0.00222 0.00342 C56 1 0.459340 0.441205 0.742445 11.00000 0.02930 0.02193 = 0.02969 0.00676 0.00037 -0.00103 AFIX 43 H56 2 0.408368 0.418011 0.751201 11.00000 -1.20000 AFIX 0 C57 1 0.548494 0.419435 0.744224 11.00000 0.03645 0.01882 = 0.01962 0.00282 -0.00066 0.00636 C58 1 0.622588 0.453352 0.730904 11.00000 0.02588 0.02682 = 0.02548 -0.00234 -0.00194 0.01105 AFIX 43 H58 2 0.683450 0.438511 0.731616 11.00000 -1.20000 AFIX 0 C59 1 0.609928 0.508679 0.716498 11.00000 0.01922 0.02426 = 0.03435 -0.00108 0.00066 0.00390 C60 1 0.345974 0.518248 0.726988 11.00000 0.02327 0.04416 = 0.07271 0.02090 0.00794 0.00890 AFIX 137 H60A 2 0.302108 0.487573 0.731009 11.00000 -1.50000 H60B 2 0.334977 0.537077 0.692159 11.00000 -1.50000 H60C 2 0.337491 0.544546 0.757035 11.00000 -1.50000 AFIX 0 C61 1 0.564840 0.360197 0.762020 11.00000 0.06121 0.02526 = 0.02562 0.00657 0.00474 0.01659 AFIX 137 H61A 2 0.625134 0.347664 0.748521 11.00000 -1.50000 H61B 2 0.516033 0.336440 0.747099 11.00000 -1.50000 H61C 2 0.563933 0.358144 0.801959 11.00000 -1.50000 AFIX 0 C63 1 0.515858 0.537160 0.581410 11.00000 0.06333 0.02303 = 0.03854 -0.00869 0.00590 0.00318 AFIX 23 H63A 2 0.576805 0.522474 0.592837 11.00000 -1.20000 H63B 2 0.468152 0.510137 0.592868 11.00000 -1.20000 AFIX 0 C62 1 0.692441 0.544993 0.703541 11.00000 0.02419 0.03865 = 0.06509 -0.00499 0.00860 -0.00312 AFIX 137 H62A 2 0.749325 0.523097 0.706399 11.00000 -1.50000 H62B 2 0.694919 0.575856 0.729468 11.00000 -1.50000 H62C 2 0.686492 0.559532 0.666367 11.00000 -1.50000 AFIX 0 C64 1 0.514366 0.541716 0.521486 11.00000 0.20844 0.03803 = 0.03244 -0.00815 -0.01061 0.02865 AFIX 137 H64A 2 0.523436 0.504993 0.505326 11.00000 -1.50000 H64B 2 0.564089 0.566489 0.509514 11.00000 -1.50000 H64C 2 0.454578 0.556697 0.509740 11.00000 -1.50000 AFIX 0 C65 1 0.378821 0.665229 0.272347 11.00000 0.01891 0.01809 = 0.01527 0.00093 -0.00093 0.00058 C66 1 0.466975 0.588163 0.364532 11.00000 0.01744 0.01540 = 0.02401 0.00148 0.00005 -0.00167 C67 1 0.610507 0.624051 0.261575 11.00000 0.01640 0.02648 = 0.02595 0.00396 0.00365 0.00333 C68 1 0.398468 0.725943 0.266032 11.00000 0.01285 0.01648 = 0.01732 0.00303 -0.00124 0.00064 C69 1 0.380590 0.762041 0.309655 11.00000 0.01415 0.02013 = 0.01713 0.00085 -0.00168 0.00217 C70 1 0.397621 0.818433 0.301874 11.00000 0.01906 0.01749 = 0.02268 -0.00128 -0.00312 0.00135 AFIX 43 H70 2 0.384737 0.843512 0.330761 11.00000 -1.20000 AFIX 0 C71 1 0.432941 0.838979 0.253006 11.00000 0.01997 0.01723 = 0.03062 0.00485 -0.00332 -0.00010 C72 1 0.450472 0.802158 0.210808 11.00000 0.01954 0.02477 = 0.02327 0.00841 -0.00088 0.00111 AFIX 43 H72 2 0.474419 0.815885 0.177334 11.00000 -1.20000 AFIX 0 C73 1 0.433933 0.745672 0.216186 11.00000 0.01335 0.02292 = 0.01704 0.00238 -0.00160 0.00225 C74 1 0.346556 0.741815 0.364219 11.00000 0.02076 0.02725 = 0.01599 0.00127 0.00072 0.00356 AFIX 137 H74A 2 0.322431 0.773148 0.385280 11.00000 -1.50000 H74B 2 0.397824 0.724625 0.384171 11.00000 -1.50000 H74C 2 0.297268 0.714512 0.358711 11.00000 -1.50000 AFIX 0 C76 1 0.448983 0.707039 0.168761 11.00000 0.02045 0.02969 = 0.01892 0.00039 0.00094 0.00354 AFIX 137 H76A 2 0.485199 0.725931 0.140537 11.00000 -1.50000 H76B 2 0.389009 0.695926 0.153655 11.00000 -1.50000 H76C 2 0.482536 0.674122 0.181231 11.00000 -1.50000 AFIX 0 C75 1 0.451282 0.900242 0.246636 11.00000 0.04010 0.01972 = 0.04721 0.00749 0.00271 -0.00388 AFIX 137 H75A 2 0.495714 0.906119 0.216986 11.00000 -1.50000 H75B 2 0.476757 0.914977 0.280736 11.00000 -1.50000 H75C 2 0.393269 0.919361 0.238054 11.00000 -1.50000 AFIX 0 C77 1 0.454151 0.527938 0.378821 11.00000 0.02135 0.01581 = 0.02177 0.00272 -0.00031 -0.00369 C78 1 0.363946 0.507258 0.383893 11.00000 0.02194 0.01797 = 0.02276 -0.00124 0.00169 -0.00413 C79 1 0.352462 0.451802 0.398438 11.00000 0.03150 0.02255 = 0.02347 0.00034 0.00416 -0.00940 AFIX 43 H79 2 0.291716 0.437234 0.402072 11.00000 -1.20000 AFIX 0 C82 1 0.531480 0.493980 0.386734 11.00000 0.02369 0.01919 = 0.03235 0.00251 -0.00333 -0.00161 C81 1 0.516456 0.438719 0.401778 11.00000 0.03541 0.01878 = 0.03047 0.00398 -0.00513 0.00261 AFIX 43 H81 2 0.568067 0.415210 0.408074 11.00000 -1.20000 AFIX 0 C80 1 0.427546 0.417622 0.407669 11.00000 0.04556 0.01548 = 0.02062 0.00151 0.00088 -0.00472 C83 1 0.280451 0.543811 0.374881 11.00000 0.02098 0.02631 = 0.04351 -0.00265 0.00259 -0.00261 AFIX 137 H83A 2 0.224592 0.520863 0.373286 11.00000 -1.50000 H83B 2 0.287530 0.564025 0.340454 11.00000 -1.50000 H83C 2 0.275091 0.570247 0.405059 11.00000 -1.50000 AFIX 0 C86 1 0.645127 0.681287 0.250027 11.00000 0.01121 0.02416 = 0.02464 0.00411 0.00039 0.00185 C85 1 0.628602 0.516343 0.380547 11.00000 0.02218 0.02872 = 0.06774 0.00796 -0.00561 0.00228 AFIX 137 H85A 2 0.673124 0.488540 0.393164 11.00000 -1.50000 H85B 2 0.635241 0.550104 0.402391 11.00000 -1.50000 H85C 2 0.640407 0.524882 0.342074 11.00000 -1.50000 AFIX 0 C84 1 0.412251 0.357901 0.424004 11.00000 0.05716 0.01896 = 0.03361 0.00784 0.00421 -0.00387 AFIX 137 H84A 2 0.459784 0.346763 0.450329 11.00000 -1.50000 H84B 2 0.416112 0.334229 0.391599 11.00000 -1.50000 H84C 2 0.350950 0.354026 0.440665 11.00000 -1.50000 AFIX 0 C87 1 0.682467 0.693397 0.197897 11.00000 0.01293 0.03386 = 0.02236 0.00490 -0.00011 0.00312 C88 1 0.705062 0.748344 0.186441 11.00000 0.01543 0.03616 = 0.02408 0.01040 -0.00042 -0.00118 AFIX 43 H88 2 0.728440 0.757318 0.151302 11.00000 -1.20000 AFIX 0 C89 1 0.694582 0.790326 0.224567 11.00000 0.01693 0.02678 = 0.03124 0.00882 -0.00256 -0.00153 C90 1 0.661904 0.776887 0.276207 11.00000 0.01518 0.02582 = 0.02767 0.00259 -0.00265 -0.00134 AFIX 43 H90 2 0.656905 0.805081 0.303084 11.00000 -1.20000 AFIX 0 C91 1 0.636238 0.722730 0.289417 11.00000 0.01185 0.02573 = 0.02142 0.00494 -0.00208 -0.00012 C92 1 0.695937 0.649744 0.154266 11.00000 0.02424 0.04015 = 0.02596 -0.00123 0.00361 0.00244 AFIX 137 H92A 2 0.706862 0.667789 0.119028 11.00000 -1.50000 H92B 2 0.640371 0.626611 0.151898 11.00000 -1.50000 H92C 2 0.749296 0.626577 0.163630 11.00000 -1.50000 AFIX 0 C93 1 0.718005 0.849709 0.210803 11.00000 0.03350 0.02812 = 0.04346 0.01434 0.00050 -0.00249 AFIX 137 H93A 2 0.754529 0.865891 0.240486 11.00000 -1.50000 H93B 2 0.660765 0.870935 0.206106 11.00000 -1.50000 H93C 2 0.753909 0.850802 0.176893 11.00000 -1.50000 AFIX 0 C94 1 0.603402 0.709989 0.346398 11.00000 0.01725 0.02749 = 0.02151 0.00278 0.00043 -0.00013 AFIX 137 H94A 2 0.616143 0.741684 0.370218 11.00000 -1.50000 H94B 2 0.636001 0.677283 0.360214 11.00000 -1.50000 H94C 2 0.536702 0.702712 0.345830 11.00000 -1.50000 AFIX 0 C95 1 0.443432 0.540633 0.243594 11.00000 0.03643 0.01966 = 0.03408 -0.00630 0.00084 -0.00182 AFIX 23 H95A 2 0.486656 0.510535 0.253718 11.00000 -1.20000 H95B 2 0.380826 0.529287 0.255581 11.00000 -1.20000 AFIX 0 C96 1 0.442903 0.545904 0.181644 11.00000 0.08818 0.03388 = 0.02864 -0.01352 -0.00584 -0.01089 AFIX 137 H96A 2 0.428953 0.509807 0.165324 11.00000 -1.50000 H96B 2 0.503758 0.558515 0.169127 11.00000 -1.50000 H96C 2 0.395658 0.572781 0.170627 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 REM AT667_a.res in P2(1)2(1)2(1) REM R1 = 0.0440 for 27060 Fo > 4sig(Fo) and 0.0626 for all 32647 data REM 1004 parameters refined using 0 restraints END WGHT 0.0405 6.0841 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 1.946, deepest hole -1.793, 1-sigma level 0.083 Q1 1 0.4772 0.6130 0.5966 11.00000 0.05 1.95 Q2 1 0.5377 0.6015 0.9677 11.00000 0.05 1.49 Q3 1 0.4975 0.5495 0.5513 11.00000 0.05 1.31 Q4 1 0.4777 0.6076 0.3089 11.00000 0.05 1.02 Q5 1 0.5352 0.5388 0.8465 11.00000 0.05 0.98 Q6 1 0.5269 0.6103 0.2823 11.00000 0.05 0.94 Q7 1 0.4150 0.5112 0.5518 11.00000 0.05 0.92 Q8 1 0.5617 0.6295 0.9395 11.00000 0.05 0.86 Q9 1 0.4969 0.6014 0.6619 11.00000 0.05 0.84 Q10 1 0.4989 0.6240 0.9402 11.00000 0.05 0.82 Q11 1 0.5067 0.5834 0.9392 11.00000 0.05 0.82 Q12 1 0.4598 0.5927 0.6255 11.00000 0.05 0.80 Q13 1 0.5290 0.5347 0.9164 11.00000 0.05 0.79 Q14 1 0.5667 0.5798 0.9408 11.00000 0.05 0.74 Q15 1 0.4482 0.6298 0.2822 11.00000 0.05 0.70 Q16 1 0.4575 0.5818 0.2845 11.00000 0.05 0.67 Q17 1 0.4880 0.6149 0.9571 11.00000 0.05 0.66 Q18 1 0.4659 0.6119 0.7181 11.00000 0.05 0.64 Q19 1 0.5319 0.6134 0.2483 11.00000 0.05 0.63 Q20 1 0.5364 0.6017 0.9005 11.00000 0.05 0.55 ; _shelx_res_checksum 42699 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Ge1 Ge 0.53566(2) 0.60418(2) 0.94209(2) 0.01915(6) Uani 1 1 d . . C1 C 0.4234(2) 0.65186(13) 0.92517(11) 0.0196(5) Uani 1 1 d . . O1 O 0.35596(17) 0.62562(10) 0.91065(11) 0.0324(5) Uani 1 1 d . . Ge2 Ge 0.49366(2) 0.60730(2) 0.61926(2) 0.02196(7) Uani 1 1 d . . C2 C 0.5330(2) 0.57754(13) 1.02066(14) 0.0260(6) Uani 1 1 d . . O2 O 0.5508(2) 0.61058(11) 1.05641(11) 0.0438(7) Uani 1 1 d . . Ge3 Ge 0.47844(2) 0.60728(2) 0.28395(2) 0.01625(6) Uani 1 1 d . . C3 C 0.66293(19) 0.63913(12) 0.93508(11) 0.0176(5) Uani 1 1 d . . O3 O 0.72825(14) 0.60860(10) 0.94315(9) 0.0280(4) Uani 1 1 d . . O4 O 0.67372(17) 0.63710(11) 0.59266(12) 0.0353(6) Uani 1 1 d . . C4 C 0.42101(18) 0.71368(12) 0.92798(11) 0.0179(5) Uani 1 1 d . . O5 O 0.3083(2) 0.59349(15) 0.59999(18) 0.0738(13) Uani 1 1 d . . C5 C 0.43848(19) 0.74454(12) 0.88072(12) 0.0192(5) Uani 1 1 d . . O6 O 0.5022(2) 0.62539(11) 0.73543(11) 0.0461(8) Uani 1 1 d . . C6 C 0.4338(2) 0.80238(13) 0.88396(13) 0.0237(6) Uani 1 1 d . . H6 H 0.4460 0.8237 0.8522 0.028 Uiso 1 1 calc R U O7 O 0.30012(15) 0.64721(10) 0.27190(11) 0.0281(5) Uani 1 1 d . . C7 C 0.4117(2) 0.82942(13) 0.93221(14) 0.0265(6) Uani 1 1 d . . O8 O 0.46489(19) 0.62370(9) 0.39933(9) 0.0285(5) Uani 1 1 d . . C8 C 0.3933(2) 0.79740(14) 0.97851(13) 0.0260(6) Uani 1 1 d . . H8 H 0.3771 0.8154 1.0116 0.031 Uiso 1 1 calc R U O9 O 0.65614(18) 0.58250(11) 0.25269(12) 0.0378(6) Uani 1 1 d . . C9 C 0.3980(2) 0.73996(14) 0.97725(12) 0.0214(6) Uani 1 1 d . . C10 C 0.4604(2) 0.71672(14) 0.82731(12) 0.0249(6) Uani 1 1 d . . H10A H 0.4978 0.7416 0.8047 0.037 Uiso 1 1 calc R U H10B H 0.4027 0.7079 0.8082 0.037 Uiso 1 1 calc R U H10C H 0.4950 0.6825 0.8342 0.037 Uiso 1 1 calc R U C12 C 0.3789(2) 0.70639(16) 1.02768(13) 0.0295(7) Uani 1 1 d . . H12A H 0.3587 0.7310 1.0571 0.044 Uiso 1 1 calc R U H12B H 0.4355 0.6870 1.0388 0.044 Uiso 1 1 calc R U H12C H 0.3302 0.6793 1.0200 0.044 Uiso 1 1 calc R U C11 C 0.4078(3) 0.89197(15) 0.93488(17) 0.0410(8) Uani 1 1 d . . H11A H 0.3545 0.9034 0.9569 0.062 Uiso 1 1 calc R U H11B H 0.4017 0.9070 0.8979 0.062 Uiso 1 1 calc R U H11C H 0.4648 0.9060 0.9516 0.062 Uiso 1 1 calc R U C13 C 0.5112(2) 0.51841(13) 1.03484(13) 0.0239(6) Uani 1 1 d . . C14 C 0.5839(2) 0.48293(13) 1.05015(13) 0.0245(6) Uani 1 1 d . . C15 C 0.5614(2) 0.42943(14) 1.06769(13) 0.0263(6) Uani 1 1 d . . H15 H 0.6098 0.4045 1.0767 0.032 Uiso 1 1 calc R U C16 C 0.4704(2) 0.41181(13) 1.07223(12) 0.0246(6) Uani 1 1 d . . C17 C 0.4000(2) 0.44826(13) 1.05705(13) 0.0245(6) Uani 1 1 d . . H17 H 0.3374 0.4366 1.0601 0.029 Uiso 1 1 calc R U C18 C 0.4191(2) 0.50129(13) 1.03759(13) 0.0247(6) Uani 1 1 d . . C19 C 0.6837(2) 0.50153(16) 1.04852(18) 0.0357(8) Uani 1 1 d . . H19A H 0.7244 0.4692 1.0519 0.054 Uiso 1 1 calc R U H19B H 0.6956 0.5271 1.0788 0.054 Uiso 1 1 calc R U H19C H 0.6960 0.5204 1.0138 0.054 Uiso 1 1 calc R U C20 C 0.4463(3) 0.35559(14) 1.09464(14) 0.0320(7) Uani 1 1 d . . H20A H 0.3919 0.3411 1.0755 0.048 Uiso 1 1 calc R U H20B H 0.4327 0.3587 1.1337 0.048 Uiso 1 1 calc R U H20C H 0.4987 0.3304 1.0893 0.048 Uiso 1 1 calc R U C22 C 0.67258(18) 0.69777(12) 0.91629(11) 0.0166(5) Uani 1 1 d . . C21 C 0.3411(2) 0.53982(16) 1.0226(2) 0.0407(9) Uani 1 1 d . . H21A H 0.2820 0.5201 1.0256 0.061 Uiso 1 1 calc R U H21B H 0.3494 0.5527 0.9850 0.061 Uiso 1 1 calc R U H21C H 0.3410 0.5717 1.0474 0.061 Uiso 1 1 calc R U C23 C 0.65257(18) 0.74101(12) 0.95263(12) 0.0186(5) Uani 1 1 d . . C24 C 0.6554(2) 0.79535(12) 0.93333(12) 0.0214(5) Uani 1 1 d . . H24 H 0.6409 0.8249 0.9574 0.026 Uiso 1 1 calc R U C25 C 0.6791(2) 0.80722(13) 0.87960(13) 0.0235(6) Uani 1 1 d . . C26 C 0.7009(2) 0.76373(13) 0.84492(12) 0.0227(6) Uani 1 1 d . . H26 H 0.7187 0.7717 0.8084 0.027 Uiso 1 1 calc R U C27 C 0.69753(19) 0.70862(13) 0.86205(11) 0.0196(5) Uani 1 1 d . . C28 C 0.6348(2) 0.72997(13) 1.01210(12) 0.0228(6) Uani 1 1 d . . H28A H 0.5865 0.7550 1.0254 0.034 Uiso 1 1 calc R U H28B H 0.6918 0.7362 1.0329 0.034 Uiso 1 1 calc R U H28C H 0.6147 0.6915 1.0168 0.034 Uiso 1 1 calc R U C29 C 0.6807(3) 0.86684(15) 0.85987(16) 0.0359(8) Uani 1 1 d . . H29A H 0.7121 0.8688 0.8245 0.054 Uiso 1 1 calc R U H29B H 0.7138 0.8898 0.8864 0.054 Uiso 1 1 calc R U H29C H 0.6171 0.8804 0.8560 0.054 Uiso 1 1 calc R U C31 C 0.5257(3) 0.54374(16) 0.88825(19) 0.0415(9) Uani 1 1 d . . H31A H 0.4756 0.5185 0.9001 0.050 Uiso 1 1 calc R U H31B H 0.5067 0.5600 0.8529 0.050 Uiso 1 1 calc R U C30 C 0.7174(2) 0.66226(15) 0.82239(13) 0.0279(7) Uani 1 1 d . . H30A H 0.7396 0.6778 0.7879 0.042 Uiso 1 1 calc R U H30B H 0.6606 0.6411 0.8158 0.042 Uiso 1 1 calc R U H30C H 0.7648 0.6378 0.8377 0.042 Uiso 1 1 calc R U C32 C 0.6118(3) 0.50980(19) 0.8790(2) 0.0492(11) Uani 1 1 d . . H32A H 0.6000 0.4822 0.8505 0.074 Uiso 1 1 calc R U H32B H 0.6289 0.4910 0.9130 0.074 Uiso 1 1 calc R U H32C H 0.6624 0.5341 0.8675 0.074 Uiso 1 1 calc R U C33 C 0.5991(2) 0.65913(13) 0.59971(12) 0.0209(5) Uani 1 1 d . . C34 C 0.3626(2) 0.63177(15) 0.60120(14) 0.0288(7) Uani 1 1 d . . C35 C 0.5048(2) 0.58958(13) 0.70056(14) 0.0283(7) Uani 1 1 d . . C36 C 0.58661(18) 0.72065(11) 0.59590(11) 0.0161(5) Uani 1 1 d . . C37 C 0.55190(18) 0.74380(12) 0.54740(11) 0.0174(5) Uani 1 1 d . . C38 C 0.53900(19) 0.80097(12) 0.54543(12) 0.0201(5) Uani 1 1 d . . H38 H 0.5145 0.8171 0.5132 0.024 Uiso 1 1 calc R U C39 C 0.5609(2) 0.83516(12) 0.58938(12) 0.0207(5) Uani 1 1 d . . C40 C 0.5968(2) 0.81102(13) 0.63621(12) 0.0209(5) Uani 1 1 d . . H40 H 0.6134 0.8340 0.6661 0.025 Uiso 1 1 calc R U C41 C 0.60895(19) 0.75406(13) 0.64058(11) 0.0181(5) Uani 1 1 d . . C42 C 0.5316(2) 0.70861(13) 0.49798(11) 0.0231(6) Uani 1 1 d . . H42A H 0.4860 0.7274 0.4749 0.035 Uiso 1 1 calc R U H42B H 0.5070 0.6727 0.5097 0.035 Uiso 1 1 calc R U H42C H 0.5888 0.7029 0.4772 0.035 Uiso 1 1 calc R U C44 C 0.6438(2) 0.72941(15) 0.69366(12) 0.0260(6) Uani 1 1 d . . H44A H 0.6768 0.7579 0.7145 0.039 Uiso 1 1 calc R U H44B H 0.6859 0.6986 0.6857 0.039 Uiso 1 1 calc R U H44C H 0.5913 0.7158 0.7151 0.039 Uiso 1 1 calc R U C43 C 0.5452(2) 0.89687(14) 0.58604(14) 0.0323(7) Uani 1 1 d . . H43A H 0.5475 0.9128 0.6228 0.048 Uiso 1 1 calc R U H43B H 0.4844 0.9041 0.5698 0.048 Uiso 1 1 calc R U H43C H 0.5934 0.9137 0.5633 0.048 Uiso 1 1 calc R U C45 C 0.3367(2) 0.68985(14) 0.58614(12) 0.0233(6) Uani 1 1 d . . C46 C 0.3008(2) 0.70084(14) 0.53343(12) 0.0227(6) Uani 1 1 d . . C47 C 0.2821(2) 0.75580(14) 0.51950(12) 0.0237(6) Uani 1 1 d . . H47 H 0.2595 0.7638 0.4840 0.028 Uiso 1 1 calc R U C48 C 0.2954(2) 0.79908(14) 0.55610(13) 0.0256(6) Uani 1 1 d . . C49 C 0.3272(2) 0.78636(15) 0.60820(13) 0.0259(6) Uani 1 1 d . . H49 H 0.3345 0.8154 0.6340 0.031 Uiso 1 1 calc R U C50 C 0.34857(19) 0.73288(15) 0.62375(12) 0.0239(6) Uani 1 1 d . . C51 C 0.2852(2) 0.65587(15) 0.49186(13) 0.0269(6) Uani 1 1 d . . H51A H 0.2641 0.6724 0.4575 0.040 Uiso 1 1 calc R U H51B H 0.2381 0.6301 0.5054 0.040 Uiso 1 1 calc R U H51C H 0.3432 0.6358 0.4856 0.040 Uiso 1 1 calc R U C54 C 0.5198(2) 0.52972(13) 0.71542(13) 0.0235(6) Uani 1 1 d . . C53 C 0.3825(2) 0.72118(17) 0.68099(12) 0.0302(7) Uani 1 1 d . . H53A H 0.3683 0.7528 0.7046 0.045 Uiso 1 1 calc R U H53B H 0.4495 0.7151 0.6803 0.045 Uiso 1 1 calc R U H53C H 0.3517 0.6880 0.6951 0.045 Uiso 1 1 calc R U C52 C 0.2761(3) 0.85811(16) 0.53971(17) 0.0370(8) Uani 1 1 d . . H52A H 0.2467 0.8777 0.5702 0.056 Uiso 1 1 calc R U H52B H 0.2347 0.8585 0.5080 0.056 Uiso 1 1 calc R U H52C H 0.3344 0.8765 0.5303 0.056 Uiso 1 1 calc R U C55 C 0.4431(2) 0.49609(14) 0.72816(15) 0.0281(7) Uani 1 1 d . . C56 C 0.4593(2) 0.44121(13) 0.74244(13) 0.0270(6) Uani 1 1 d . . H56 H 0.4084 0.4180 0.7512 0.032 Uiso 1 1 calc R U C57 C 0.5485(2) 0.41943(13) 0.74422(12) 0.0250(6) Uani 1 1 d . . C58 C 0.6226(2) 0.45335(14) 0.73090(13) 0.0261(6) Uani 1 1 d . . H58 H 0.6834 0.4385 0.7316 0.031 Uiso 1 1 calc R U C59 C 0.6099(2) 0.50868(14) 0.71650(14) 0.0259(6) Uani 1 1 d . . C60 C 0.3460(3) 0.51825(19) 0.7270(2) 0.0467(11) Uani 1 1 d . . H60A H 0.3021 0.4876 0.7310 0.070 Uiso 1 1 calc R U H60B H 0.3350 0.5371 0.6922 0.070 Uiso 1 1 calc R U H60C H 0.3375 0.5445 0.7570 0.070 Uiso 1 1 calc R U C61 C 0.5648(3) 0.36020(15) 0.76202(15) 0.0374(9) Uani 1 1 d . . H61A H 0.6251 0.3477 0.7485 0.056 Uiso 1 1 calc R U H61B H 0.5160 0.3364 0.7471 0.056 Uiso 1 1 calc R U H61C H 0.5639 0.3581 0.8020 0.056 Uiso 1 1 calc R U C63 C 0.5159(3) 0.53716(15) 0.58141(16) 0.0416(9) Uani 1 1 d . . H63A H 0.5768 0.5225 0.5928 0.050 Uiso 1 1 calc R U H63B H 0.4682 0.5101 0.5929 0.050 Uiso 1 1 calc R U C62 C 0.6924(3) 0.54499(18) 0.7035(2) 0.0426(10) Uani 1 1 d . . H62A H 0.7493 0.5231 0.7064 0.064 Uiso 1 1 calc R U H62B H 0.6949 0.5759 0.7295 0.064 Uiso 1 1 calc R U H62C H 0.6865 0.5595 0.6664 0.064 Uiso 1 1 calc R U C64 C 0.5144(7) 0.5417(2) 0.52149(19) 0.093(3) Uani 1 1 d . . H64A H 0.5234 0.5050 0.5053 0.139 Uiso 1 1 calc R U H64B H 0.5641 0.5665 0.5095 0.139 Uiso 1 1 calc R U H64C H 0.4546 0.5567 0.5097 0.139 Uiso 1 1 calc R U C65 C 0.37882(19) 0.66523(12) 0.27235(11) 0.0174(5) Uani 1 1 d . . C66 C 0.4670(2) 0.58816(11) 0.36453(12) 0.0190(5) Uani 1 1 d . . C67 C 0.6105(2) 0.62405(13) 0.26157(13) 0.0229(6) Uani 1 1 d . . C68 C 0.39847(18) 0.72594(11) 0.26603(11) 0.0155(5) Uani 1 1 d . . C69 C 0.38059(19) 0.76204(12) 0.30966(11) 0.0171(5) Uani 1 1 d . . C70 C 0.3976(2) 0.81843(12) 0.30187(12) 0.0197(5) Uani 1 1 d . . H70 H 0.3847 0.8435 0.3308 0.024 Uiso 1 1 calc R U C71 C 0.4329(2) 0.83898(12) 0.25301(13) 0.0226(6) Uani 1 1 d . . C72 C 0.4505(2) 0.80216(13) 0.21081(12) 0.0225(6) Uani 1 1 d . . H72 H 0.4744 0.8159 0.1773 0.027 Uiso 1 1 calc R U C73 C 0.43393(19) 0.74567(12) 0.21619(11) 0.0178(5) Uani 1 1 d . . C74 C 0.3466(2) 0.74182(13) 0.36422(11) 0.0213(6) Uani 1 1 d . . H74A H 0.3224 0.7731 0.3853 0.032 Uiso 1 1 calc R U H74B H 0.3978 0.7246 0.3842 0.032 Uiso 1 1 calc R U H74C H 0.2973 0.7145 0.3587 0.032 Uiso 1 1 calc R U C76 C 0.4490(2) 0.70704(13) 0.16876(12) 0.0230(6) Uani 1 1 d . . H76A H 0.4852 0.7259 0.1405 0.035 Uiso 1 1 calc R U H76B H 0.3890 0.6959 0.1537 0.035 Uiso 1 1 calc R U H76C H 0.4825 0.6741 0.1812 0.035 Uiso 1 1 calc R U C75 C 0.4513(3) 0.90024(14) 0.24664(16) 0.0357(8) Uani 1 1 d . . H75A H 0.4957 0.9061 0.2170 0.054 Uiso 1 1 calc R U H75B H 0.4768 0.9150 0.2807 0.054 Uiso 1 1 calc R U H75C H 0.3933 0.9194 0.2381 0.054 Uiso 1 1 calc R U C77 C 0.4542(2) 0.52794(12) 0.37882(12) 0.0196(5) Uani 1 1 d . . C78 C 0.3639(2) 0.50726(13) 0.38389(12) 0.0209(5) Uani 1 1 d . . C79 C 0.3525(2) 0.45180(13) 0.39844(13) 0.0258(6) Uani 1 1 d . . H79 H 0.2917 0.4372 0.4021 0.031 Uiso 1 1 calc R U C82 C 0.5315(2) 0.49398(13) 0.38673(13) 0.0251(6) Uani 1 1 d . . C81 C 0.5165(3) 0.43872(13) 0.40178(14) 0.0282(6) Uani 1 1 d . . H81 H 0.5681 0.4152 0.4081 0.034 Uiso 1 1 calc R U C80 C 0.4275(3) 0.41762(13) 0.40767(13) 0.0272(7) Uani 1 1 d . . C83 C 0.2805(2) 0.54381(14) 0.37488(16) 0.0303(7) Uani 1 1 d . . H83A H 0.2246 0.5209 0.3733 0.045 Uiso 1 1 calc R U H83B H 0.2875 0.5640 0.3405 0.045 Uiso 1 1 calc R U H83C H 0.2751 0.5702 0.4051 0.045 Uiso 1 1 calc R U C86 C 0.64513(19) 0.68129(13) 0.25003(12) 0.0200(5) Uani 1 1 d . . C85 C 0.6286(2) 0.51634(16) 0.3805(2) 0.0395(9) Uani 1 1 d . . H85A H 0.6731 0.4885 0.3932 0.059 Uiso 1 1 calc R U H85B H 0.6352 0.5501 0.4024 0.059 Uiso 1 1 calc R U H85C H 0.6404 0.5249 0.3421 0.059 Uiso 1 1 calc R U C84 C 0.4123(3) 0.35790(14) 0.42400(16) 0.0366(9) Uani 1 1 d . . H84A H 0.4598 0.3468 0.4503 0.055 Uiso 1 1 calc R U H84B H 0.4161 0.3342 0.3916 0.055 Uiso 1 1 calc R U H84C H 0.3510 0.3540 0.4407 0.055 Uiso 1 1 calc R U C87 C 0.6825(2) 0.69340(14) 0.19790(12) 0.0231(6) Uani 1 1 d . . C88 C 0.7051(2) 0.74834(14) 0.18644(13) 0.0252(6) Uani 1 1 d . . H88 H 0.7284 0.7573 0.1513 0.030 Uiso 1 1 calc R U C89 C 0.6946(2) 0.79033(14) 0.22457(13) 0.0250(6) Uani 1 1 d . . C90 C 0.6619(2) 0.77689(13) 0.27621(13) 0.0229(6) Uani 1 1 d . . H90 H 0.6569 0.8051 0.3031 0.027 Uiso 1 1 calc R U C91 C 0.63624(19) 0.72273(13) 0.28942(12) 0.0197(5) Uani 1 1 d . . C92 C 0.6959(2) 0.64974(16) 0.15427(14) 0.0301(7) Uani 1 1 d . . H92A H 0.7069 0.6678 0.1190 0.045 Uiso 1 1 calc R U H92B H 0.6404 0.6266 0.1519 0.045 Uiso 1 1 calc R U H92C H 0.7493 0.6266 0.1636 0.045 Uiso 1 1 calc R U C93 C 0.7180(3) 0.84971(15) 0.21080(16) 0.0350(8) Uani 1 1 d . . H93A H 0.7545 0.8659 0.2405 0.053 Uiso 1 1 calc R U H93B H 0.6608 0.8709 0.2061 0.053 Uiso 1 1 calc R U H93C H 0.7539 0.8508 0.1769 0.053 Uiso 1 1 calc R U C94 C 0.6034(2) 0.70999(13) 0.34640(12) 0.0221(6) Uani 1 1 d . . H94A H 0.6161 0.7417 0.3702 0.033 Uiso 1 1 calc R U H94B H 0.6360 0.6773 0.3602 0.033 Uiso 1 1 calc R U H94C H 0.5367 0.7027 0.3458 0.033 Uiso 1 1 calc R U C95 C 0.4434(3) 0.54063(14) 0.24359(14) 0.0301(7) Uani 1 1 d . . H95A H 0.4867 0.5105 0.2537 0.036 Uiso 1 1 calc R U H95B H 0.3808 0.5293 0.2556 0.036 Uiso 1 1 calc R U C96 C 0.4429(4) 0.54590(18) 0.18164(16) 0.0502(12) Uani 1 1 d . . H96A H 0.4290 0.5098 0.1653 0.075 Uiso 1 1 calc R U H96B H 0.5038 0.5585 0.1691 0.075 Uiso 1 1 calc R U H96C H 0.3957 0.5728 0.1706 0.075 Uiso 1 1 calc R U 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 0.01459(12) 0.01457(12) 0.02828(14) -0.00136(12) 0.00123(10) -0.00238(11) C1 0.0177(12) 0.0233(14) 0.0176(12) 0.0018(10) 0.0000(9) -0.0009(10) O1 0.0220(11) 0.0290(12) 0.0462(15) 0.0038(11) -0.0094(10) -0.0071(9) Ge2 0.02398(14) 0.01382(13) 0.02808(14) -0.00430(12) 0.00513(11) -0.00114(13) C2 0.0189(13) 0.0211(14) 0.0380(16) 0.0096(12) -0.0018(12) -0.0061(11) O2 0.0608(17) 0.0318(13) 0.0389(14) 0.0117(12) -0.0143(12) -0.0194(13) Ge3 0.01575(12) 0.01219(12) 0.02079(12) -0.00110(11) 0.00024(9) 0.00070(12) C3 0.0179(12) 0.0201(13) 0.0148(11) -0.0022(9) 0.0018(9) -0.0030(10) O3 0.0180(9) 0.0270(11) 0.0390(12) 0.0049(11) -0.0002(8) 0.0021(9) O4 0.0242(12) 0.0302(13) 0.0516(16) 0.0066(12) 0.0132(11) 0.0083(10) C4 0.0119(11) 0.0237(14) 0.0180(12) -0.0015(10) -0.0023(9) 0.0008(10) O5 0.0468(18) 0.059(2) 0.115(3) 0.053(2) -0.050(2) -0.0364(16) C5 0.0154(11) 0.0233(14) 0.0191(12) -0.0009(10) -0.0032(10) 0.0011(10) O6 0.080(2) 0.0257(13) 0.0321(13) 0.0016(10) 0.0087(14) 0.0159(14) C6 0.0226(13) 0.0223(14) 0.0260(14) 0.0019(11) -0.0056(11) 0.0004(11) O7 0.0154(10) 0.0243(11) 0.0447(14) 0.0040(10) -0.0034(9) -0.0020(8) C7 0.0223(14) 0.0206(14) 0.0368(17) -0.0049(12) -0.0087(12) 0.0037(11) O8 0.0419(13) 0.0171(10) 0.0266(10) -0.0004(8) 0.0073(10) -0.0031(9) C8 0.0202(13) 0.0313(16) 0.0264(14) -0.0103(12) -0.0018(11) 0.0065(12) O9 0.0274(12) 0.0282(13) 0.0578(17) 0.0065(12) 0.0132(12) 0.0112(10) C9 0.0152(12) 0.0297(15) 0.0195(13) -0.0016(11) -0.0017(10) 0.0028(11) C10 0.0259(15) 0.0322(16) 0.0166(12) -0.0017(11) 0.0007(11) -0.0012(12) C12 0.0282(16) 0.041(2) 0.0193(13) -0.0023(13) 0.0053(12) 0.0045(14) C11 0.046(2) 0.0223(16) 0.055(2) -0.0073(17) -0.0108(17) 0.0059(17) C13 0.0213(14) 0.0230(14) 0.0275(14) 0.0074(11) -0.0006(11) -0.0050(11) C14 0.0208(13) 0.0252(14) 0.0274(14) 0.0065(12) -0.0017(12) -0.0036(11) C15 0.0270(15) 0.0260(15) 0.0257(15) 0.0060(12) -0.0007(12) 0.0003(12) C16 0.0315(15) 0.0240(14) 0.0181(12) 0.0025(10) -0.0015(11) -0.0071(12) C17 0.0237(14) 0.0245(14) 0.0253(14) 0.0018(12) 0.0036(11) -0.0081(11) C18 0.0213(14) 0.0235(15) 0.0294(16) 0.0034(12) -0.0003(11) -0.0051(11) C19 0.0194(14) 0.0383(19) 0.049(2) 0.0107(17) -0.0018(15) -0.0048(13) C20 0.045(2) 0.0252(16) 0.0262(15) 0.0069(12) -0.0048(14) -0.0104(14) C22 0.0127(11) 0.0190(13) 0.0180(12) -0.0013(10) 0.0002(9) -0.0037(9) C21 0.0192(15) 0.0306(18) 0.072(3) 0.0128(18) -0.0019(16) -0.0042(13) C23 0.0154(11) 0.0209(13) 0.0194(12) 0.0010(10) 0.0007(10) -0.0027(9) C24 0.0220(13) 0.0189(13) 0.0232(13) -0.0003(10) -0.0007(10) -0.0010(10) C25 0.0210(13) 0.0236(15) 0.0258(14) 0.0054(12) -0.0022(11) -0.0039(11) C26 0.0213(13) 0.0296(16) 0.0172(12) 0.0042(11) -0.0009(10) -0.0071(12) C27 0.0154(12) 0.0266(15) 0.0170(12) -0.0017(10) -0.0003(9) -0.0042(10) C28 0.0266(14) 0.0225(14) 0.0194(13) -0.0013(11) 0.0037(11) -0.0020(11) C29 0.044(2) 0.0259(17) 0.0374(19) 0.0119(14) -0.0030(16) -0.0055(15) C31 0.0278(16) 0.0302(19) 0.067(3) -0.0209(17) -0.0030(17) -0.0040(15) C30 0.0293(16) 0.0340(18) 0.0203(13) -0.0031(12) 0.0053(12) -0.0041(13) C32 0.047(2) 0.041(2) 0.060(3) -0.016(2) 0.005(2) -0.0006(19) C33 0.0217(13) 0.0198(14) 0.0211(13) -0.0004(11) 0.0044(11) 0.0016(10) C34 0.0257(15) 0.0369(19) 0.0239(14) 0.0079(13) -0.0067(12) -0.0122(13) C35 0.0299(16) 0.0202(14) 0.0348(16) 0.0061(12) 0.0090(13) 0.0060(12) C36 0.0123(11) 0.0168(12) 0.0192(12) 0.0000(10) 0.0027(9) -0.0007(9) C37 0.0127(11) 0.0232(13) 0.0163(11) -0.0016(10) 0.0019(9) -0.0022(9) C38 0.0172(12) 0.0242(13) 0.0189(11) 0.0031(10) 0.0002(10) -0.0002(10) C39 0.0182(12) 0.0194(13) 0.0245(14) 0.0012(11) 0.0030(10) -0.0020(10) C40 0.0173(12) 0.0244(15) 0.0211(13) -0.0044(11) 0.0014(10) -0.0042(10) C41 0.0138(11) 0.0247(14) 0.0159(11) 0.0006(10) 0.0012(9) -0.0021(10) C42 0.0218(13) 0.0296(15) 0.0180(12) -0.0029(11) 0.0007(11) -0.0024(12) C44 0.0220(14) 0.0381(18) 0.0180(13) 0.0035(12) -0.0014(11) -0.0032(13) C43 0.0365(17) 0.0210(15) 0.0394(17) -0.0007(14) 0.0018(13) -0.0003(15) C45 0.0133(12) 0.0381(18) 0.0184(13) 0.0043(12) -0.0004(10) -0.0062(11) C46 0.0135(12) 0.0360(17) 0.0187(12) -0.0004(11) 0.0004(9) -0.0025(11) C47 0.0150(12) 0.0377(18) 0.0184(12) 0.0020(12) 0.0008(10) 0.0005(11) C48 0.0149(12) 0.0333(16) 0.0288(15) 0.0002(13) 0.0012(11) 0.0018(11) C49 0.0140(12) 0.0390(19) 0.0248(14) -0.0064(12) -0.0009(10) 0.0022(12) C50 0.0121(11) 0.0430(19) 0.0168(12) 0.0005(12) 0.0005(10) -0.0022(11) C51 0.0230(14) 0.0347(18) 0.0231(14) -0.0017(12) -0.0030(11) -0.0048(12) C54 0.0213(14) 0.0188(13) 0.0304(14) 0.0057(11) 0.0039(11) 0.0064(11) C53 0.0183(14) 0.055(2) 0.0172(13) 0.0000(14) -0.0011(10) -0.0033(14) C52 0.0334(18) 0.036(2) 0.041(2) 0.0015(16) -0.0025(15) 0.0039(15) C55 0.0219(14) 0.0261(16) 0.0363(17) 0.0075(13) 0.0022(12) 0.0034(12) C56 0.0293(16) 0.0219(14) 0.0297(15) 0.0068(12) 0.0004(12) -0.0010(12) C57 0.0364(17) 0.0188(14) 0.0196(13) 0.0028(10) -0.0007(12) 0.0064(12) C58 0.0259(15) 0.0268(16) 0.0255(15) -0.0023(12) -0.0019(12) 0.0110(12) C59 0.0192(13) 0.0243(15) 0.0343(16) -0.0011(13) 0.0007(12) 0.0039(11) C60 0.0233(17) 0.044(2) 0.073(3) 0.021(2) 0.0079(18) 0.0089(16) C61 0.061(3) 0.0253(17) 0.0256(16) 0.0066(13) 0.0047(16) 0.0166(17) C63 0.063(3) 0.0230(16) 0.0385(19) -0.0087(14) 0.0059(19) 0.0032(17) C62 0.0242(17) 0.039(2) 0.065(3) -0.0050(19) 0.0086(17) -0.0031(15) C64 0.208(9) 0.038(3) 0.032(2) -0.0082(18) -0.011(4) 0.029(4) C65 0.0189(12) 0.0181(13) 0.0153(11) 0.0009(9) -0.0009(9) 0.0006(10) C66 0.0174(12) 0.0154(11) 0.0240(12) 0.0015(9) 0.0000(10) -0.0017(10) C67 0.0164(12) 0.0265(15) 0.0259(14) 0.0040(11) 0.0037(10) 0.0033(10) C68 0.0128(11) 0.0165(12) 0.0173(11) 0.0030(9) -0.0012(9) 0.0006(9) C69 0.0141(11) 0.0201(13) 0.0171(12) 0.0008(10) -0.0017(9) 0.0022(9) C70 0.0191(12) 0.0175(13) 0.0227(13) -0.0013(10) -0.0031(10) 0.0013(10) C71 0.0200(13) 0.0172(13) 0.0306(15) 0.0049(11) -0.0033(11) -0.0001(10) C72 0.0195(13) 0.0248(14) 0.0233(13) 0.0084(11) -0.0009(10) 0.0011(11) C73 0.0134(11) 0.0229(13) 0.0170(11) 0.0024(10) -0.0016(9) 0.0023(10) C74 0.0208(13) 0.0272(15) 0.0160(12) 0.0013(10) 0.0007(10) 0.0036(11) C76 0.0205(13) 0.0297(16) 0.0189(12) 0.0004(11) 0.0009(10) 0.0035(11) C75 0.0401(19) 0.0197(15) 0.0472(19) 0.0075(14) 0.0027(15) -0.0039(14) C77 0.0213(13) 0.0158(12) 0.0218(12) 0.0027(10) -0.0003(10) -0.0037(10) C78 0.0219(13) 0.0180(13) 0.0228(13) -0.0012(10) 0.0017(11) -0.0041(10) C79 0.0315(16) 0.0225(15) 0.0235(14) 0.0003(11) 0.0042(12) -0.0094(12) C82 0.0237(13) 0.0192(14) 0.0324(15) 0.0025(11) -0.0033(12) -0.0016(12) C81 0.0354(18) 0.0188(14) 0.0305(15) 0.0040(12) -0.0051(13) 0.0026(12) C80 0.0456(19) 0.0155(13) 0.0206(14) 0.0015(11) 0.0009(13) -0.0047(13) C83 0.0210(14) 0.0263(16) 0.0435(19) -0.0026(14) 0.0026(14) -0.0026(12) C86 0.0112(11) 0.0242(14) 0.0246(13) 0.0041(11) 0.0004(10) 0.0018(10) C85 0.0222(16) 0.0287(19) 0.068(3) 0.0080(18) -0.0056(17) 0.0023(13) C84 0.057(2) 0.0190(15) 0.0336(18) 0.0078(13) 0.0042(17) -0.0039(15) C87 0.0129(12) 0.0339(17) 0.0224(13) 0.0049(12) -0.0001(10) 0.0031(11) C88 0.0154(12) 0.0362(18) 0.0241(14) 0.0104(12) -0.0004(10) -0.0012(12) C89 0.0169(12) 0.0268(16) 0.0312(16) 0.0088(12) -0.0026(11) -0.0015(11) C90 0.0152(12) 0.0258(15) 0.0277(14) 0.0026(12) -0.0026(10) -0.0013(11) C91 0.0118(11) 0.0257(14) 0.0214(13) 0.0049(11) -0.0021(10) -0.0001(10) C92 0.0242(15) 0.0401(19) 0.0260(15) -0.0012(14) 0.0036(12) 0.0024(14) C93 0.0335(18) 0.0281(17) 0.043(2) 0.0143(15) 0.0005(15) -0.0025(14) C94 0.0172(12) 0.0275(15) 0.0215(13) 0.0028(11) 0.0004(10) -0.0001(11) C95 0.0364(18) 0.0197(15) 0.0341(17) -0.0063(12) 0.0008(14) -0.0018(13) C96 0.088(4) 0.034(2) 0.0286(18) -0.0135(15) -0.006(2) -0.011(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C31 Ge1 C2 113.48(17) C31 Ge1 C3 108.48(14) C2 Ge1 C3 103.25(12) C31 Ge1 C1 102.98(15) C2 Ge1 C1 110.96(12) C3 Ge1 C1 118.05(12) O1 C1 C4 121.0(3) O1 C1 Ge1 113.9(2) C4 C1 Ge1 125.1(2) C63 Ge2 C33 107.37(16) C63 Ge2 C34 107.52(18) C33 Ge2 C34 117.98(13) C63 Ge2 C35 105.52(15) C33 Ge2 C35 107.45(13) C34 Ge2 C35 110.28(14) O2 C2 C13 120.2(3) O2 C2 Ge1 118.2(2) C13 C2 Ge1 121.6(2) C95 Ge3 C67 105.74(15) C95 Ge3 C65 108.26(14) C67 Ge3 C65 119.53(12) C95 Ge3 C66 106.44(13) C67 Ge3 C66 112.62(12) C65 Ge3 C66 103.58(11) O3 C3 C22 123.5(3) O3 C3 Ge1 116.0(2) C22 C3 Ge1 120.3(2) C5 C4 C9 120.9(3) C5 C4 C1 119.3(2) C9 C4 C1 119.8(3) C4 C5 C6 118.4(3) C4 C5 C10 121.3(3) C6 C5 C10 120.3(3) C7 C6 C5 121.9(3) C7 C6 H6 119.0 C5 C6 H6 119.0 C6 C7 C8 118.3(3) C6 C7 C11 121.0(3) C8 C7 C11 120.7(3) C9 C8 C7 121.6(3) C9 C8 H8 119.2 C7 C8 H8 119.2 C8 C9 C4 118.8(3) C8 C9 C12 120.7(3) C4 C9 C12 120.4(3) C5 C10 H10A 109.5 C5 C10 H10B 109.5 H10A C10 H10B 109.5 C5 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C9 C12 H12A 109.5 C9 C12 H12B 109.5 H12A C12 H12B 109.5 C9 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C7 C11 H11A 109.5 C7 C11 H11B 109.5 H11A C11 H11B 109.5 C7 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C18 C13 C14 121.2(3) C18 C13 C2 119.5(3) C14 C13 C2 119.0(3) C15 C14 C13 118.1(3) C15 C14 C19 120.3(3) C13 C14 C19 121.6(3) C16 C15 C14 121.9(3) C16 C15 H15 119.1 C14 C15 H15 119.1 C15 C16 C17 118.5(3) C15 C16 C20 121.7(3) C17 C16 C20 119.8(3) C18 C17 C16 121.7(3) C18 C17 H17 119.2 C16 C17 H17 119.2 C17 C18 C13 118.6(3) C17 C18 C21 120.1(3) C13 C18 C21 121.3(3) C14 C19 H19A 109.5 C14 C19 H19B 109.5 H19A C19 H19B 109.5 C14 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C16 C20 H20A 109.5 C16 C20 H20B 109.5 H20A C20 H20B 109.5 C16 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C27 C22 C23 121.0(3) C27 C22 C3 119.5(3) C23 C22 C3 119.4(2) C18 C21 H21A 109.5 C18 C21 H21B 109.5 H21A C21 H21B 109.5 C18 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C24 C23 C22 118.6(3) C24 C23 C28 120.0(3) C22 C23 C28 121.2(3) C25 C24 C23 121.5(3) C25 C24 H24 119.3 C23 C24 H24 119.3 C26 C25 C24 118.7(3) C26 C25 C29 121.3(3) C24 C25 C29 120.0(3) C25 C26 C27 122.0(3) C25 C26 H26 119.0 C27 C26 H26 119.0 C26 C27 C22 118.2(3) C26 C27 C30 120.4(3) C22 C27 C30 121.4(3) C23 C28 H28A 109.5 C23 C28 H28B 109.5 H28A C28 H28B 109.5 C23 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C25 C29 H29A 109.5 C25 C29 H29B 109.5 H29A C29 H29B 109.5 C25 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C32 C31 Ge1 116.3(3) C32 C31 H31A 108.2 Ge1 C31 H31A 108.2 C32 C31 H31B 108.2 Ge1 C31 H31B 108.2 H31A C31 H31B 107.4 C27 C30 H30A 109.5 C27 C30 H30B 109.5 H30A C30 H30B 109.5 C27 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C31 C32 H32A 109.5 C31 C32 H32B 109.5 H32A C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 O4 C33 C36 122.2(3) O4 C33 Ge2 115.5(2) C36 C33 Ge2 122.3(2) O5 C34 C45 123.1(3) O5 C34 Ge2 112.7(3) C45 C34 Ge2 124.0(2) O6 C35 C54 121.1(3) O6 C35 Ge2 122.2(2) C54 C35 Ge2 116.6(2) C41 C36 C37 121.0(3) C41 C36 C33 119.7(3) C37 C36 C33 119.3(3) C38 C37 C36 118.1(3) C38 C37 C42 120.3(3) C36 C37 C42 121.6(3) C39 C38 C37 122.0(3) C39 C38 H38 119.0 C37 C38 H38 119.0 C40 C39 C38 118.4(3) C40 C39 C43 121.1(3) C38 C39 C43 120.6(3) C39 C40 C41 121.8(3) C39 C40 H40 119.1 C41 C40 H40 119.1 C40 C41 C36 118.8(3) C40 C41 C44 119.8(3) C36 C41 C44 121.5(3) C37 C42 H42A 109.5 C37 C42 H42B 109.5 H42A C42 H42B 109.5 C37 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C41 C44 H44A 109.5 C41 C44 H44B 109.5 H44A C44 H44B 109.5 C41 C44 H44C 109.5 H44A C44 H44C 109.5 H44B C44 H44C 109.5 C39 C43 H43A 109.5 C39 C43 H43B 109.5 H43A C43 H43B 109.5 C39 C43 H43C 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 C50 C45 C46 120.4(3) C50 C45 C34 120.2(3) C46 C45 C34 119.4(3) C47 C46 C45 118.1(3) C47 C46 C51 119.4(3) C45 C46 C51 122.4(3) C48 C47 C46 122.0(3) C48 C47 H47 119.0 C46 C47 H47 119.0 C47 C48 C49 118.1(3) C47 C48 C52 120.9(3) C49 C48 C52 121.0(3) C50 C49 C48 122.2(3) C50 C49 H49 118.9 C48 C49 H49 118.9 C49 C50 C45 119.0(3) C49 C50 C53 120.2(3) C45 C50 C53 120.8(3) C46 C51 H51A 109.5 C46 C51 H51B 109.5 H51A C51 H51B 109.5 C46 C51 H51C 109.5 H51A C51 H51C 109.5 H51B C51 H51C 109.5 C59 C54 C55 121.3(3) C59 C54 C35 119.1(3) C55 C54 C35 119.6(3) C50 C53 H53A 109.5 C50 C53 H53B 109.5 H53A C53 H53B 109.5 C50 C53 H53C 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 C48 C52 H52A 109.5 C48 C52 H52B 109.5 H52A C52 H52B 109.5 C48 C52 H52C 109.5 H52A C52 H52C 109.5 H52B C52 H52C 109.5 C56 C55 C54 118.2(3) C56 C55 C60 120.1(3) C54 C55 C60 121.7(3) C55 C56 C57 121.6(3) C55 C56 H56 119.2 C57 C56 H56 119.2 C58 C57 C56 119.0(3) C58 C57 C61 120.3(3) C56 C57 C61 120.7(3) C57 C58 C59 121.6(3) C57 C58 H58 119.2 C59 C58 H58 119.2 C58 C59 C54 118.4(3) C58 C59 C62 120.3(3) C54 C59 C62 121.3(3) C55 C60 H60A 109.5 C55 C60 H60B 109.5 H60A C60 H60B 109.5 C55 C60 H60C 109.5 H60A C60 H60C 109.5 H60B C60 H60C 109.5 C57 C61 H61A 109.5 C57 C61 H61B 109.5 H61A C61 H61B 109.5 C57 C61 H61C 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 C64 C63 Ge2 113.9(3) C64 C63 H63A 108.8 Ge2 C63 H63A 108.8 C64 C63 H63B 108.8 Ge2 C63 H63B 108.8 H63A C63 H63B 107.7 C59 C62 H62A 109.5 C59 C62 H62B 109.5 H62A C62 H62B 109.5 C59 C62 H62C 109.5 H62A C62 H62C 109.5 H62B C62 H62C 109.5 C63 C64 H64A 109.5 C63 C64 H64B 109.5 H64A C64 H64B 109.5 C63 C64 H64C 109.5 H64A C64 H64C 109.5 H64B C64 H64C 109.5 O7 C65 C68 121.6(3) O7 C65 Ge3 114.7(2) C68 C65 Ge3 123.65(19) O8 C66 C77 121.2(3) O8 C66 Ge3 121.7(2) C77 C66 Ge3 117.0(2) O9 C67 C86 123.0(3) O9 C67 Ge3 113.1(2) C86 C67 Ge3 123.4(2) C69 C68 C73 121.2(3) C69 C68 C65 119.6(2) C73 C68 C65 119.3(2) C70 C69 C68 118.0(3) C70 C69 C74 119.7(3) C68 C69 C74 122.3(3) C71 C70 C69 121.9(3) C71 C70 H70 119.0 C69 C70 H70 119.0 C72 C71 C70 118.6(3) C72 C71 C75 121.2(3) C70 C71 C75 120.1(3) C71 C72 C73 121.8(3) C71 C72 H72 119.1 C73 C72 H72 119.1 C72 C73 C68 118.5(3) C72 C73 C76 120.6(3) C68 C73 C76 120.8(3) C69 C74 H74A 109.5 C69 C74 H74B 109.5 H74A C74 H74B 109.5 C69 C74 H74C 109.5 H74A C74 H74C 109.5 H74B C74 H74C 109.5 C73 C76 H76A 109.5 C73 C76 H76B 109.5 H76A C76 H76B 109.5 C73 C76 H76C 109.5 H76A C76 H76C 109.5 H76B C76 H76C 109.5 C71 C75 H75A 109.5 C71 C75 H75B 109.5 H75A C75 H75B 109.5 C71 C75 H75C 109.5 H75A C75 H75C 109.5 H75B C75 H75C 109.5 C82 C77 C78 121.4(3) C82 C77 C66 120.0(3) C78 C77 C66 118.6(3) C79 C78 C77 118.4(3) C79 C78 C83 120.2(3) C77 C78 C83 121.4(3) C80 C79 C78 121.4(3) C80 C79 H79 119.3 C78 C79 H79 119.3 C77 C82 C81 118.1(3) C77 C82 C85 121.2(3) C81 C82 C85 120.7(3) C80 C81 C82 121.3(3) C80 C81 H81 119.3 C82 C81 H81 119.3 C79 C80 C81 119.3(3) C79 C80 C84 119.9(3) C81 C80 C84 120.8(3) C78 C83 H83A 109.5 C78 C83 H83B 109.5 H83A C83 H83B 109.5 C78 C83 H83C 109.5 H83A C83 H83C 109.5 H83B C83 H83C 109.5 C91 C86 C87 120.7(3) C91 C86 C67 120.0(3) C87 C86 C67 119.2(3) C82 C85 H85A 109.5 C82 C85 H85B 109.5 H85A C85 H85B 109.5 C82 C85 H85C 109.5 H85A C85 H85C 109.5 H85B C85 H85C 109.5 C80 C84 H84A 109.5 C80 C84 H84B 109.5 H84A C84 H84B 109.5 C80 C84 H84C 109.5 H84A C84 H84C 109.5 H84B C84 H84C 109.5 C88 C87 C86 117.8(3) C88 C87 C92 119.3(3) C86 C87 C92 122.8(3) C89 C88 C87 122.3(3) C89 C88 H88 118.9 C87 C88 H88 118.9 C88 C89 C90 118.7(3) C88 C89 C93 121.2(3) C90 C89 C93 120.1(3) C89 C90 C91 121.3(3) C89 C90 H90 119.3 C91 C90 H90 119.3 C86 C91 C90 119.1(3) C86 C91 C94 121.6(3) C90 C91 C94 119.3(3) C87 C92 H92A 109.5 C87 C92 H92B 109.5 H92A C92 H92B 109.5 C87 C92 H92C 109.5 H92A C92 H92C 109.5 H92B C92 H92C 109.5 C89 C93 H93A 109.5 C89 C93 H93B 109.5 H93A C93 H93B 109.5 C89 C93 H93C 109.5 H93A C93 H93C 109.5 H93B C93 H93C 109.5 C91 C94 H94A 109.5 C91 C94 H94B 109.5 H94A C94 H94B 109.5 C91 C94 H94C 109.5 H94A C94 H94C 109.5 H94B C94 H94C 109.5 C96 C95 Ge3 115.9(3) C96 C95 H95A 108.3 Ge3 C95 H95A 108.3 C96 C95 H95B 108.3 Ge3 C95 H95B 108.3 H95A C95 H95B 107.4 C95 C96 H96A 109.5 C95 C96 H96B 109.5 H96A C96 H96B 109.5 C95 C96 H96C 109.5 H96A C96 H96C 109.5 H96B C96 H96C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ge1 C31 1.973(4) Ge1 C2 2.030(3) Ge1 C3 2.031(3) Ge1 C1 2.032(3) C1 O1 1.216(4) C1 C4 1.495(4) Ge2 C63 1.958(3) Ge2 C33 2.030(3) Ge2 C34 2.033(4) Ge2 C35 2.044(3) C2 O2 1.213(4) C2 C13 1.503(4) Ge3 C95 1.956(3) Ge3 C67 2.027(3) Ge3 C65 2.028(3) Ge3 C66 2.035(3) C3 O3 1.214(4) C3 C22 1.496(4) O4 C33 1.214(4) C4 C5 1.400(4) C4 C9 1.404(4) O5 C34 1.213(4) C5 C6 1.401(4) C5 C10 1.505(4) O6 C35 1.217(4) C6 C7 1.388(5) C6 H6 0.9500 O7 C65 1.218(4) C7 C8 1.398(5) C7 C11 1.513(5) O8 C66 1.210(3) C8 C9 1.389(5) C8 H8 0.9500 O9 C67 1.220(4) C9 C12 1.504(4) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C13 C18 1.395(4) C13 C14 1.406(4) C14 C15 1.400(4) C14 C19 1.513(4) C15 C16 1.386(5) C15 H15 0.9500 C16 C17 1.396(5) C16 C20 1.505(4) C17 C18 1.394(4) C17 H17 0.9500 C18 C21 1.508(5) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C22 C27 1.402(4) C22 C23 1.403(4) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C23 C24 1.395(4) C23 C28 1.503(4) C24 C25 1.390(4) C24 H24 0.9500 C25 C26 1.387(5) C25 C29 1.519(4) C26 C27 1.396(4) C26 H26 0.9500 C27 C30 1.510(4) C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C31 C32 1.507(6) C31 H31A 0.9900 C31 H31B 0.9900 C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 C33 C36 1.500(4) C34 C45 1.498(5) C35 C54 1.506(4) C36 C41 1.398(4) C36 C37 1.406(4) C37 C38 1.394(4) C37 C42 1.508(4) C38 C39 1.394(4) C38 H38 0.9500 C39 C40 1.387(4) C39 C43 1.510(5) C40 C41 1.391(4) C40 H40 0.9500 C41 C44 1.516(4) C42 H42A 0.9800 C42 H42B 0.9800 C42 H42C 0.9800 C44 H44A 0.9800 C44 H44B 0.9800 C44 H44C 0.9800 C43 H43A 0.9800 C43 H43B 0.9800 C43 H43C 0.9800 C45 C50 1.400(5) C45 C46 1.417(4) C46 C47 1.397(5) C46 C51 1.506(4) C47 C48 1.391(5) C47 H47 0.9500 C48 C49 1.391(4) C48 C52 1.507(5) C49 C50 1.381(5) C49 H49 0.9500 C50 C53 1.512(4) C51 H51A 0.9800 C51 H51B 0.9800 C51 H51C 0.9800 C54 C59 1.399(4) C54 C55 1.408(5) C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C52 H52A 0.9800 C52 H52B 0.9800 C52 H52C 0.9800 C55 C56 1.391(5) C55 C60 1.503(5) C56 C57 1.392(5) C56 H56 0.9500 C57 C58 1.387(5) C57 C61 1.514(4) C58 C59 1.394(5) C58 H58 0.9500 C59 C62 1.514(5) C60 H60A 0.9800 C60 H60B 0.9800 C60 H60C 0.9800 C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 C63 C64 1.473(6) C63 H63A 0.9900 C63 H63B 0.9900 C62 H62A 0.9800 C62 H62B 0.9800 C62 H62C 0.9800 C64 H64A 0.9800 C64 H64B 0.9800 C64 H64C 0.9800 C65 C68 1.501(4) C66 C77 1.507(4) C67 C86 1.497(4) C68 C69 1.403(4) C68 C73 1.408(4) C69 C70 1.397(4) C69 C74 1.506(4) C70 C71 1.393(4) C70 H70 0.9500 C71 C72 1.387(4) C71 C75 1.511(4) C72 C73 1.391(4) C72 H72 0.9500 C73 C76 1.506(4) C74 H74A 0.9800 C74 H74B 0.9800 C74 H74C 0.9800 C76 H76A 0.9800 C76 H76B 0.9800 C76 H76C 0.9800 C75 H75A 0.9800 C75 H75B 0.9800 C75 H75C 0.9800 C77 C82 1.400(4) C77 C78 1.402(4) C78 C79 1.396(4) C78 C83 1.511(5) C79 C80 1.382(5) C79 H79 0.9500 C82 C81 1.401(4) C82 C85 1.512(5) C81 C80 1.390(5) C81 H81 0.9500 C80 C84 1.513(4) C83 H83A 0.9800 C83 H83B 0.9800 C83 H83C 0.9800 C86 C91 1.396(4) C86 C87 1.417(4) C85 H85A 0.9800 C85 H85B 0.9800 C85 H85C 0.9800 C84 H84A 0.9800 C84 H84B 0.9800 C84 H84C 0.9800 C87 C88 1.395(5) C87 C92 1.514(5) C88 C89 1.387(5) C88 H88 0.9500 C89 C90 1.389(4) C89 C93 1.512(5) C90 C91 1.397(4) C90 H90 0.9500 C91 C94 1.506(4) C92 H92A 0.9800 C92 H92B 0.9800 C92 H92C 0.9800 C93 H93A 0.9800 C93 H93B 0.9800 C93 H93C 0.9800 C94 H94A 0.9800 C94 H94B 0.9800 C94 H94C 0.9800 C95 C96 1.523(5) C95 H95A 0.9900 C95 H95B 0.9900 C96 H96A 0.9800 C96 H96B 0.9800 C96 H96C 0.9800