#------------------------------------------------------------------------------ #$Date: 2016-09-10 02:12:59 +0300 (Sat, 10 Sep 2016) $ #$Revision: 186333 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543285.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_1543285 loop_ _publ_author_name 'Andrez, Julie' 'P\'ecaut, Jacques' 'Scopelliti, Rosario' 'Kefalidis, Christos E.' 'Maron, Laurent' 'Rosenzweig, Michael W.' 'Meyer, Karsten' 'Mazzanti, Marinella' _publ_section_title ; Synthesis and reactivity of a terminal uranium(iv) sulfide supported by siloxide ligands ; _journal_issue 9 _journal_name_full 'Chem. Sci.' _journal_page_first 5846 _journal_paper_doi 10.1039/C6SC00675B _journal_volume 7 _journal_year 2016 _chemical_formula_sum 'C122 H256 K4 O38 S2 Si8 U2' _chemical_formula_weight 3252.55 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2016-01-18 deposited with the CCDC. 2016-04-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.476(9) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 16.3304(14) _cell_length_b 26.8000(19) _cell_length_c 18.8582(15) _cell_measurement_reflns_used 2365 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 19.7910 _cell_measurement_theta_min 3.0720 _cell_volume 8250.6(11) _computing_cell_refinement ; Agilent Technologies, (2013), CrysAlisPro Software system, version 1.171. 36.28, Agilent Technologies UK Ltd, Oxford, UK ; _computing_data_collection ; Agilent Technologies, (2013), CrysAlisPro Software system, version 1.171.37.31, Agilent Technologies UK Ltd, Oxford, UK ; _computing_data_reduction ; Agilent Technologies, (2013), CrysAlisPro Software system, version 1.171. 36.28, Agilent Technologies UK Ltd, Oxford, UK ; _computing_molecular_graphics ; Mercury 3.1 New software for searching the Cambridge Structural Database and visualizing crystal structures (I.J. Bruno, J.C. Cole, P.R. Edgington, M. Kessler, C.F. Macrae, P. McCabe, J. Pearson, R. Taylor, Acta Cryst., 2002, B58, 389-397) ; _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement ; OLEX2: a complete structure solution, refinement and analysis program (O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann. J. Appl. Cryst. 2009, 42, 339-34). ; _computing_structure_solution ; SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007, 40, 786-790) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 15.9653 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; 1 omega -25.00 67.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 -99.0000 -120.0000 92 2 omega -5.00 95.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 77.0000 30.0000 100 3 omega -97.00 -38.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - -26.9676 -77.0000 0.0000 59 ; _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1343 _diffrn_reflns_av_unetI/netI 0.2296 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 37944 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.093 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.209 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'translucent pale green' _exptl_crystal_density_diffrn 1.309 _exptl_crystal_description plate _exptl_crystal_F_000 3392 _exptl_crystal_size_max 0.216 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.422 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.152 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 870 _refine_ls_number_reflns 16850 _refine_ls_number_restraints 66 _refine_ls_restrained_S_all 0.930 _refine_ls_R_factor_all 0.1642 _refine_ls_R_factor_gt 0.0778 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1000 _refine_ls_wR_factor_ref 0.1282 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9046 _reflns_number_total 16850 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6sc00675b2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 1543284--1543292.cif.' _cod_database_code 1543285 _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 0.647 _shelx_estimated_absorpt_t_max 0.957 _shelxl_version_number 2013-4 _shelx_res_file ; TITL CF solution in P21/n CELL 0.71073 16.330426 26.799962 18.858158 90 91.4758 90 ZERR 2 0.001381 0.001886 0.00153 0 0.0092 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H K O S Si U UNIT 244 512 8 76 4 16 4 SIMU 0.01 0.02 1.7 C84B C84 C83B C83 ISOR 0.01 0.02 C97 ISOR 0.05 0.01 C32 C31 ISOR 0.01 0.02 C32B C31B L.S. 4 PLAN 20 SIZE 0.02 0.095 0.216 TEMP -123 FREE K2 C64 FREE K2 C66 FREE K2 C83 FREE K2 C84B FREE C82 C83B BOND $H ACTA fmap 2 SHEL 999 0.8 REM C:\Users\JP154903\structure\2014\andrez\ja326\struct\tmp\ja326.hkl WGHT 0.000000 FVAR 0.28230 0.69054 0.61915 U1 7 0.728194 0.390530 0.767474 11.00000 0.01896 0.01793 = 0.02205 -0.00029 0.00200 0.00154 K1 3 0.920892 0.337201 0.725809 11.00000 0.02272 0.02691 = 0.03223 -0.00253 0.00335 0.00255 K2 3 0.506763 0.474409 0.890970 11.00000 0.03465 0.03128 = 0.03634 -0.00330 0.00851 0.00659 S1 5 0.686063 0.434693 0.879636 11.00000 0.03188 0.02939 = 0.02800 -0.00655 0.00429 0.00431 SI1 6 0.781288 0.329469 0.590204 11.00000 0.02688 0.02474 = 0.02660 -0.00374 0.00349 0.00420 SI2 6 0.924192 0.465052 0.758669 11.00000 0.02183 0.02897 = 0.03663 -0.00368 0.00945 -0.00278 SI3 6 0.822532 0.278592 0.862522 11.00000 0.02968 0.02326 = 0.02825 0.00335 0.00331 0.00476 SI4 6 0.513016 0.419344 0.720444 11.00000 0.02286 0.02546 = 0.02024 -0.00223 0.00225 0.00423 O1 4 0.763336 0.351021 0.667096 11.00000 0.02192 0.02546 = 0.03350 -0.00811 0.00124 0.00521 O2 4 0.878216 0.311695 0.593819 11.00000 0.02413 0.02430 = 0.03046 -0.00585 0.01019 0.00729 O3 4 0.776758 0.369662 0.525522 11.00000 0.02930 0.02920 = 0.02663 0.00204 0.00339 0.00331 O4 4 0.722134 0.283500 0.564122 11.00000 0.03161 0.02914 = 0.02360 -0.00201 -0.00055 -0.01193 O21 4 0.841606 0.434174 0.750406 11.00000 0.01882 0.04198 = 0.02689 -0.00215 -0.00334 -0.00640 O22 4 0.997788 0.423242 0.750986 11.00000 0.02823 0.02352 = 0.05576 -0.01039 0.00424 -0.00508 O23 4 0.933941 0.508996 0.699388 11.00000 0.04056 0.02303 = 0.03852 -0.00175 0.01031 -0.00663 O24 4 0.941347 0.492014 0.834203 11.00000 0.03711 0.04403 = 0.03445 -0.01133 0.00109 -0.01005 O41 4 0.785320 0.324947 0.819959 11.00000 0.03459 0.02202 = 0.02189 -0.00454 0.00388 0.00204 O42 4 0.911199 0.267436 0.826315 11.00000 0.02767 0.02573 = 0.04731 0.01535 0.00619 0.01298 O43 4 0.832877 0.286079 0.946666 11.00000 0.03500 0.04453 = 0.02162 -0.00040 0.00501 0.00357 O44 4 0.770243 0.226842 0.851549 11.00000 0.03772 0.03113 = 0.04617 0.00554 0.00975 0.00271 O61 4 0.604034 0.398344 0.720754 11.00000 0.02678 0.02527 = 0.01953 -0.01069 0.00734 0.00494 O62 4 0.507084 0.479643 0.738104 11.00000 0.03475 0.02446 = 0.02852 0.00100 0.00362 0.00218 O63 4 0.457409 0.399789 0.786176 11.00000 0.02158 0.02109 = 0.03301 0.00526 0.00885 0.00199 O64 4 0.470440 0.406444 0.643779 11.00000 0.02821 0.04094 = 0.02057 -0.00459 0.00061 0.01086 O81 4 0.537574 0.576567 0.951751 11.00000 0.04646 0.03053 = 0.04468 -0.00104 0.00892 -0.00496 O82 4 0.390193 0.547840 0.882304 11.00000 0.03706 0.04897 = 0.09149 0.00756 -0.00254 0.00778 O83 4 0.345706 0.458096 0.952490 11.00000 0.03628 0.04473 = 0.07651 0.01528 0.00410 -0.00963 C1 1 0.932049 0.297118 0.538452 11.00000 0.02584 0.01918 = 0.03541 -0.00102 0.00240 0.00689 C2 1 0.887899 0.267169 0.480351 11.00000 0.05168 0.03639 = 0.04340 -0.01375 0.01121 0.02133 AFIX 137 H2C 2 0.860661 0.238394 0.501478 11.00000 -1.50000 H2D 2 0.927680 0.255515 0.446020 11.00000 -1.50000 H2E 2 0.846973 0.288344 0.456205 11.00000 -1.50000 AFIX 0 C3 1 0.969162 0.342893 0.506122 11.00000 0.06025 0.04988 = 0.04624 0.00444 0.02484 0.00528 AFIX 137 H3A 2 0.925489 0.364361 0.486698 11.00000 -1.50000 H3B 2 1.005452 0.332964 0.468015 11.00000 -1.50000 H3C 2 1.000722 0.361173 0.542593 11.00000 -1.50000 AFIX 0 C4 1 0.997200 0.265797 0.573633 11.00000 0.03916 0.04471 = 0.06476 0.00309 0.01593 0.01912 AFIX 137 H4A 2 1.025769 0.285419 0.610481 11.00000 -1.50000 H4B 2 1.036413 0.255007 0.538270 11.00000 -1.50000 H4C 2 0.972072 0.236456 0.595181 11.00000 -1.50000 AFIX 0 C5 1 0.708621 0.388135 0.481141 11.00000 0.03556 0.04099 = 0.03412 0.00412 -0.00654 0.01769 C6 1 0.740411 0.436318 0.449918 11.00000 0.11040 0.03506 = 0.06220 0.02482 -0.02987 0.00448 AFIX 137 H6A 2 0.761852 0.457775 0.488162 11.00000 -1.50000 H6B 2 0.695676 0.453527 0.424370 11.00000 -1.50000 H6C 2 0.784250 0.428791 0.417045 11.00000 -1.50000 AFIX 0 C7 1 0.691139 0.350721 0.422164 11.00000 0.05959 0.04917 = 0.01997 0.00229 -0.00440 -0.00799 AFIX 137 H7A 2 0.740451 0.346118 0.394358 11.00000 -1.50000 H7B 2 0.646518 0.363184 0.391256 11.00000 -1.50000 H7C 2 0.675171 0.318725 0.442828 11.00000 -1.50000 AFIX 0 C8 1 0.632509 0.395494 0.525517 11.00000 0.07313 0.13098 = 0.05278 0.00716 -0.00476 0.07117 AFIX 137 H8A 2 0.618165 0.363863 0.548126 11.00000 -1.50000 H8B 2 0.586774 0.406612 0.494774 11.00000 -1.50000 H8C 2 0.643802 0.420723 0.562093 11.00000 -1.50000 AFIX 0 C9 1 0.690111 0.240856 0.599930 11.00000 0.02959 0.03637 = 0.05311 0.00096 0.01065 -0.00432 C10 1 0.668985 0.202679 0.541708 11.00000 0.07668 0.04635 = 0.05678 -0.00867 0.00241 -0.03183 AFIX 137 H10A 2 0.631760 0.217922 0.506339 11.00000 -1.50000 H10B 2 0.642405 0.173648 0.562770 11.00000 -1.50000 H10C 2 0.719288 0.192072 0.518809 11.00000 -1.50000 AFIX 0 C11 1 0.614178 0.256121 0.637543 11.00000 0.04188 0.06124 = 0.05543 -0.01105 0.01180 -0.00950 AFIX 137 H11A 2 0.627828 0.282296 0.672159 11.00000 -1.50000 H11B 2 0.591589 0.227195 0.662105 11.00000 -1.50000 H11C 2 0.573546 0.268838 0.602922 11.00000 -1.50000 AFIX 0 C12 1 0.754183 0.219824 0.651515 11.00000 0.05959 0.04732 = 0.06299 0.02023 0.00483 -0.00977 AFIX 137 H12A 2 0.807027 0.217801 0.628206 11.00000 -1.50000 H12B 2 0.737551 0.186409 0.666580 11.00000 -1.50000 H12C 2 0.759317 0.241688 0.693046 11.00000 -1.50000 AFIX 0 C21 1 1.086003 0.425720 0.766209 11.00000 0.02397 0.05431 = 0.06445 -0.00548 -0.00361 -0.00241 C22 1 1.122526 0.386790 0.718725 11.00000 0.02892 0.04810 = 0.12178 -0.00361 0.01344 -0.01334 AFIX 137 H1 2 1.103567 0.353638 0.732849 11.00000 -1.50000 H22A 2 1.182413 0.388178 0.723061 11.00000 -1.50000 H22B 2 1.105335 0.393251 0.669405 11.00000 -1.50000 AFIX 0 C23 1 1.118211 0.476985 0.745806 11.00000 0.03044 0.04497 = 0.10496 -0.01414 0.01092 -0.01729 AFIX 137 H23A 2 1.100245 0.484839 0.697093 11.00000 -1.50000 H23B 2 1.178202 0.476906 0.749032 11.00000 -1.50000 H23C 2 1.096897 0.502175 0.778173 11.00000 -1.50000 AFIX 0 C24 1 1.100142 0.413482 0.841932 11.00000 0.02722 0.10569 = 0.07944 0.00062 -0.01191 0.00912 AFIX 137 H24A 2 1.069629 0.436879 0.871205 11.00000 -1.50000 H24B 2 1.158755 0.416070 0.853849 11.00000 -1.50000 H24C 2 1.081422 0.379381 0.850966 11.00000 -1.50000 AFIX 0 C25 1 0.909814 0.511064 0.625800 11.00000 0.05586 0.02922 = 0.03808 0.00967 0.01608 0.00506 C26 1 0.822728 0.523127 0.618450 11.00000 0.06826 0.05030 = 0.05024 -0.00266 0.00713 0.01510 AFIX 137 H26A 2 0.790184 0.494855 0.634827 11.00000 -1.50000 H26B 2 0.808823 0.529972 0.568531 11.00000 -1.50000 H26C 2 0.810782 0.552644 0.647063 11.00000 -1.50000 AFIX 0 C27 1 0.927914 0.461365 0.589639 11.00000 0.07967 0.04628 = 0.04343 -0.01423 0.02733 -0.01479 AFIX 137 H27A 2 0.986756 0.454366 0.593588 11.00000 -1.50000 H27B 2 0.911080 0.463246 0.539454 11.00000 -1.50000 H27C 2 0.897509 0.434621 0.612694 11.00000 -1.50000 AFIX 0 C28 1 0.962935 0.551174 0.593637 11.00000 0.07366 0.05550 = 0.05262 0.01229 0.02157 -0.01687 AFIX 137 H28A 2 0.952035 0.583249 0.616496 11.00000 -1.50000 H28B 2 0.950270 0.553748 0.542690 11.00000 -1.50000 H28C 2 1.020805 0.542425 0.600956 11.00000 -1.50000 AFIX 0 C29 1 0.908356 0.537489 0.864194 11.00000 0.03318 0.06340 = 0.05152 -0.04590 0.00863 -0.00582 C30 1 0.826763 0.550335 0.833412 11.00000 0.06848 0.03415 = 0.05369 -0.00893 -0.00073 0.01010 AFIX 137 H30A 2 0.830754 0.554677 0.782018 11.00000 -1.50000 H30B 2 0.807459 0.581426 0.854641 11.00000 -1.50000 H30C 2 0.788056 0.523408 0.843199 11.00000 -1.50000 AFIX 0 PART 1 C31 1 0.906228 0.537443 0.937497 31.00000 0.04884 0.04367 = 0.04560 -0.00616 0.00486 -0.00158 AFIX 137 H31A 2 0.864241 0.513989 0.952946 31.00000 -1.50000 H31B 2 0.893148 0.571046 0.954291 31.00000 -1.50000 H31C 2 0.959788 0.527263 0.957171 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C31B 1 0.892829 0.511199 0.947372 -31.00000 0.02984 0.05848 = 0.03108 -0.00141 -0.00970 0.00593 AFIX 137 H31D 2 0.842744 0.491045 0.945646 -31.00000 -1.50000 H31E 2 0.887384 0.537806 0.982586 -31.00000 -1.50000 H31F 2 0.939633 0.489974 0.960624 -31.00000 -1.50000 AFIX 0 PART 0 PART 1 C32 1 0.964802 0.582373 0.836756 31.00000 0.04863 0.04453 = 0.05225 -0.01484 0.00589 -0.02131 AFIX 137 H32A 2 1.020551 0.578512 0.856475 31.00000 -1.50000 H32B 2 0.942145 0.614312 0.852241 31.00000 -1.50000 H32C 2 0.966088 0.581633 0.784840 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C32B 1 0.980857 0.566589 0.875905 -31.00000 0.05355 0.04046 = 0.07216 -0.02529 -0.00427 -0.00058 AFIX 137 H32D 2 1.022833 0.546156 0.900012 -31.00000 -1.50000 H32E 2 0.968202 0.595514 0.905468 -31.00000 -1.50000 H32F 2 1.001217 0.578037 0.830259 -31.00000 -1.50000 AFIX 0 PART 0 C41 1 0.966777 0.226240 0.831701 11.00000 0.03482 0.02452 = 0.04951 0.00437 0.01138 0.01162 C42 1 0.947799 0.192704 0.770616 11.00000 0.08405 0.02911 = 0.06568 0.00490 -0.00467 0.03618 AFIX 137 H42A 2 0.892439 0.179125 0.774999 11.00000 -1.50000 H42B 2 0.987469 0.165272 0.770306 11.00000 -1.50000 H42C 2 0.950984 0.211619 0.726298 11.00000 -1.50000 AFIX 0 C43 1 1.051410 0.247855 0.826603 11.00000 0.02742 0.06116 = 0.10946 0.04096 0.01782 0.02599 AFIX 137 H43A 2 1.057290 0.263483 0.780029 11.00000 -1.50000 H43B 2 1.092095 0.221208 0.832616 11.00000 -1.50000 H43C 2 1.059992 0.272959 0.863842 11.00000 -1.50000 AFIX 0 C44 1 0.958272 0.197506 0.899661 11.00000 0.05732 0.04099 = 0.05489 0.01841 0.00551 0.01617 AFIX 137 H44A 2 0.963474 0.220405 0.940043 11.00000 -1.50000 H44B 2 1.001323 0.172091 0.903287 11.00000 -1.50000 H44C 2 0.904479 0.181308 0.899918 11.00000 -1.50000 AFIX 0 C45 1 0.866960 0.325041 0.992171 11.00000 0.04674 0.04617 = 0.02497 -0.00507 0.01120 -0.00160 C46 1 0.917806 0.360943 0.949118 11.00000 0.08118 0.08094 = 0.05023 -0.03245 -0.00051 -0.02943 AFIX 137 H46A 2 0.961395 0.342495 0.925815 11.00000 -1.50000 H46B 2 0.942166 0.386274 0.980645 11.00000 -1.50000 H46C 2 0.882646 0.377216 0.913129 11.00000 -1.50000 AFIX 0 C47 1 0.917372 0.299818 1.048951 11.00000 0.09057 0.06899 = 0.04985 -0.01334 -0.03701 0.03994 AFIX 137 H47A 2 0.925304 0.322560 1.089238 11.00000 -1.50000 H47B 2 0.970762 0.290698 1.030231 11.00000 -1.50000 H47C 2 0.889091 0.269665 1.064596 11.00000 -1.50000 AFIX 0 C48 1 0.796175 0.353144 1.023456 11.00000 0.07123 0.06576 = 0.04743 -0.00215 0.00509 0.03111 AFIX 137 H48A 2 0.760886 0.366398 0.985084 11.00000 -1.50000 H48B 2 0.817332 0.380756 1.052657 11.00000 -1.50000 H48C 2 0.764432 0.330492 1.052900 11.00000 -1.50000 AFIX 0 C49 1 0.695420 0.210453 0.883092 11.00000 0.03202 0.05028 = 0.04734 0.02509 0.00593 -0.00843 C50 1 0.653232 0.177494 0.827857 11.00000 0.08847 0.07872 = 0.08166 0.01989 -0.00102 -0.04584 AFIX 137 H50A 2 0.634480 0.197979 0.787570 11.00000 -1.50000 H50B 2 0.606121 0.160961 0.848835 11.00000 -1.50000 H50C 2 0.691852 0.152258 0.811497 11.00000 -1.50000 AFIX 0 C51 1 0.641109 0.253289 0.901353 11.00000 0.03115 0.06675 = 0.10439 0.03230 0.02266 0.01171 AFIX 137 H51A 2 0.670606 0.275868 0.933931 11.00000 -1.50000 H51B 2 0.591952 0.240682 0.924105 11.00000 -1.50000 H51C 2 0.625198 0.271372 0.857982 11.00000 -1.50000 AFIX 0 C52 1 0.719099 0.181075 0.948184 11.00000 0.06305 0.06914 = 0.06831 0.04047 -0.00186 -0.01098 AFIX 137 H52A 2 0.757769 0.154759 0.935583 11.00000 -1.50000 H52B 2 0.670072 0.165975 0.968037 11.00000 -1.50000 H52C 2 0.744920 0.203306 0.983441 11.00000 -1.50000 AFIX 0 C61 1 0.544273 0.522817 0.706494 11.00000 0.03820 0.01997 = 0.02177 0.00595 0.01366 -0.00434 C62 1 0.593846 0.508795 0.644072 11.00000 0.11638 0.05026 = 0.05953 0.00212 0.03790 -0.00985 AFIX 137 H62A 2 0.638880 0.486876 0.659583 11.00000 -1.50000 H62B 2 0.616234 0.538998 0.622601 11.00000 -1.50000 H62C 2 0.558947 0.491313 0.609080 11.00000 -1.50000 AFIX 0 C63 1 0.476665 0.556497 0.683311 11.00000 0.07669 0.03533 = 0.09413 0.01567 -0.02467 0.00021 AFIX 137 H63A 2 0.442264 0.539672 0.647300 11.00000 -1.50000 H63B 2 0.499577 0.587015 0.663180 11.00000 -1.50000 H63C 2 0.443482 0.565055 0.724134 11.00000 -1.50000 AFIX 0 C64 1 0.598451 0.546803 0.762583 11.00000 0.07025 0.03800 = 0.04780 0.01739 -0.01397 -0.02593 AFIX 137 H2B 2 0.566164 0.554247 0.804376 11.00000 -1.50000 H64A 2 0.621344 0.577816 0.743981 11.00000 -1.50000 H64B 2 0.643112 0.523959 0.775902 11.00000 -1.50000 AFIX 0 C65 1 0.446163 0.350589 0.817562 11.00000 0.03618 0.02295 = 0.03168 0.00351 0.00821 -0.00555 C66 1 0.491324 0.351111 0.887606 11.00000 0.04447 0.02565 = 0.03818 -0.00340 0.01181 0.00052 AFIX 137 H66A 2 0.549181 0.358774 0.880324 11.00000 -1.50000 H66B 2 0.486746 0.318320 0.910158 11.00000 -1.50000 H2A 2 0.467627 0.376582 0.918213 11.00000 -1.50000 AFIX 0 C67 1 0.482173 0.309981 0.769599 11.00000 0.06357 0.02162 = 0.04838 0.00025 -0.00222 0.00250 AFIX 137 H67A 2 0.454727 0.311152 0.722799 11.00000 -1.50000 H67B 2 0.473726 0.277113 0.790980 11.00000 -1.50000 H67C 2 0.540961 0.315861 0.764522 11.00000 -1.50000 AFIX 0 C68 1 0.356355 0.343433 0.826688 11.00000 0.04411 0.04284 = 0.04158 0.00639 0.00835 -0.00946 AFIX 137 H68A 2 0.334467 0.371515 0.853564 11.00000 -1.50000 H68B 2 0.346958 0.312296 0.852484 11.00000 -1.50000 H68C 2 0.328707 0.341792 0.780003 11.00000 -1.50000 AFIX 0 C69 1 0.387734 0.410002 0.613710 11.00000 0.04330 0.04317 = 0.02982 -0.00045 -0.00723 0.00525 C70 1 0.398234 0.433903 0.541503 11.00000 0.03971 0.08043 = 0.04380 0.01898 -0.00799 0.00271 AFIX 137 H70A 2 0.427017 0.465790 0.547264 11.00000 -1.50000 H70B 2 0.344287 0.439684 0.519037 11.00000 -1.50000 H70C 2 0.430175 0.411660 0.511608 11.00000 -1.50000 AFIX 0 C71 1 0.354433 0.358579 0.604430 11.00000 0.06968 0.06493 = 0.06052 -0.02684 -0.02203 0.00363 AFIX 137 H71A 2 0.388317 0.340039 0.571335 11.00000 -1.50000 H71B 2 0.298070 0.360398 0.585475 11.00000 -1.50000 H71C 2 0.355011 0.341484 0.650379 11.00000 -1.50000 AFIX 0 C72 1 0.332800 0.441303 0.659441 11.00000 0.03862 0.06216 = 0.03981 0.00558 -0.00721 -0.00294 AFIX 137 H72A 2 0.327744 0.425401 0.705920 11.00000 -1.50000 H72B 2 0.278499 0.444125 0.636440 11.00000 -1.50000 H72C 2 0.356596 0.474642 0.665567 11.00000 -1.50000 AFIX 0 C81 1 0.477901 0.610981 0.924920 11.00000 0.07184 0.02241 = 0.03432 -0.00187 0.01455 0.00847 AFIX 23 H81A 2 0.490375 0.619686 0.875335 11.00000 -1.20000 H81B 2 0.480339 0.641974 0.953460 11.00000 -1.20000 AFIX 0 C82 1 0.394136 0.589501 0.927352 11.00000 0.04742 0.05889 = 0.04205 0.00680 0.01579 0.03020 AFIX 23 H82A 2 0.381963 0.579412 0.976470 11.00000 -1.20000 H82B 2 0.353187 0.614694 0.911690 11.00000 -1.20000 AFIX 0 PART 1 C83 1 0.313096 0.521828 0.867402 21.00000 0.03424 0.05352 = 0.03767 -0.02185 -0.00142 0.00883 AFIX 23 H83A 2 0.321014 0.495945 0.830754 21.00000 -1.20000 H83B 2 0.271259 0.545713 0.849377 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C83B 1 0.307916 0.537765 0.905427 -21.00000 0.03121 0.05514 = 0.03737 -0.01837 -0.00437 0.00709 AFIX 23 H83C 2 0.267239 0.555849 0.875271 -21.00000 -1.20000 H83D 2 0.301733 0.548475 0.955245 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C84 1 0.284726 0.497806 0.935529 21.00000 0.03191 0.05334 = 0.03678 -0.02015 -0.00576 0.00384 AFIX 23 H84A 2 0.283244 0.522688 0.974276 21.00000 -1.20000 H84B 2 0.229327 0.483319 0.928625 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C84B 1 0.295989 0.483683 0.898885 -21.00000 0.03137 0.05355 = 0.03420 -0.02072 -0.00232 0.00486 AFIX 23 H84C 2 0.237501 0.475423 0.904967 -21.00000 -1.20000 H84D 2 0.311758 0.472538 0.851083 -21.00000 -1.20000 AFIX 0 PART 0 C85 1 0.324534 0.440814 1.018778 11.00000 0.03799 0.04100 = 0.05738 -0.02001 0.02268 -0.01013 AFIX 23 H85A 2 0.268834 0.426257 1.015801 11.00000 -1.20000 H85B 2 0.323554 0.469138 1.052445 11.00000 -1.20000 AFIX 0 C86 1 0.382837 0.402765 1.045608 11.00000 0.06403 0.03750 = 0.02934 -0.00322 0.01197 -0.01581 AFIX 23 H86A 2 0.367363 0.391848 1.093593 11.00000 -1.20000 H86B 2 0.381496 0.373309 1.013919 11.00000 -1.20000 AFIX 0 C91 1 0.751723 0.308230 1.213330 11.00000 0.10439 0.10938 = 0.05703 0.02633 0.00421 -0.02194 C92 1 0.830764 0.298116 1.230759 11.00000 0.11492 0.08597 = 0.10460 0.04682 0.00264 0.01934 AFIX 43 H92 2 0.850796 0.265382 1.222666 11.00000 -1.20000 AFIX 0 C93 1 0.884190 0.333443 1.260022 11.00000 0.19383 0.07195 = 0.10582 0.01704 0.02849 0.02702 AFIX 43 H93 2 0.939852 0.325179 1.270095 11.00000 -1.20000 AFIX 0 C94 1 0.857069 0.377446 1.273223 11.00000 0.11149 0.19748 = 0.12712 -0.02320 -0.00096 -0.07119 AFIX 43 H94 2 0.892705 0.402376 1.292210 11.00000 -1.20000 AFIX 0 C95 1 0.776705 0.387771 1.259622 11.00000 0.18299 0.10622 = 0.05844 0.00560 0.03668 -0.00017 AFIX 43 H95 2 0.757585 0.419924 1.272456 11.00000 -1.20000 AFIX 0 C96 1 0.719142 0.354575 1.227916 11.00000 0.11830 0.11221 = 0.04817 0.00938 0.02793 0.02917 AFIX 43 H96 2 0.663696 0.363284 1.217695 11.00000 -1.20000 AFIX 0 C97 1 0.705102 0.269447 1.180915 11.00000 0.12754 0.16638 = 0.08657 0.01059 0.00763 -0.06556 AFIX 137 H97A 2 0.735127 0.255656 1.141076 11.00000 -1.50000 H97B 2 0.652446 0.282800 1.163534 11.00000 -1.50000 H97C 2 0.695505 0.243073 1.215726 11.00000 -1.50000 AFIX 0 HKLF 4 REM CF solution in P21/n REM R1 = 0.0778 for 9046 Fo > 4sig(Fo) and 0.1642 for all 16850 data REM 870 parameters refined using 66 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 1.422, deepest hole -1.071, 1-sigma level 0.152 Q1 1 0.7733 0.3261 0.7333 11.00000 0.05 1.42 Q2 1 0.8171 0.3905 0.6940 11.00000 0.05 1.26 Q3 1 0.7584 0.3743 0.7200 11.00000 0.05 1.15 Q4 1 0.7918 0.3919 0.7391 11.00000 0.05 1.13 Q5 1 0.6605 0.3799 0.7557 11.00000 0.05 0.77 Q6 1 0.6717 0.3873 0.7373 11.00000 0.05 0.75 Q7 1 0.7064 0.4167 0.8175 11.00000 0.05 0.75 Q8 1 0.7523 0.4207 0.7207 11.00000 0.05 0.74 Q9 1 0.5222 0.6105 0.9959 11.00000 0.05 0.71 Q10 1 0.7075 0.3959 0.8382 11.00000 0.05 0.68 Q11 1 0.6574 0.3932 0.8748 11.00000 0.05 0.68 Q12 1 1.0228 0.3526 1.0188 11.00000 0.05 0.68 Q13 1 0.6410 0.4167 0.7041 11.00000 0.05 0.67 Q14 1 0.6601 0.4035 0.7694 11.00000 0.05 0.66 Q15 1 0.7850 0.3913 0.8017 11.00000 0.05 0.65 Q16 1 0.7388 0.3444 0.6213 11.00000 0.05 0.63 Q17 1 0.7032 0.3605 0.8021 11.00000 0.05 0.63 Q18 1 0.8953 0.4254 0.7647 11.00000 0.05 0.62 Q19 1 0.8791 0.4061 0.6207 11.00000 0.05 0.61 Q20 1 0.4595 0.5306 0.6010 11.00000 0.05 0.61 ; _shelx_res_checksum 92829 loop_ _space_group_symop_operation_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' 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.72819(2) 0.39053(2) 0.76747(2) 0.01962(9) Uani 1 1 d . . . . . K1 K 0.92089(13) 0.33720(7) 0.72581(11) 0.0272(5) Uani 1 1 d . . . . . K2 K 0.50676(14) 0.47441(7) 0.89097(11) 0.0340(6) Uani 1 1 d . . . . . S1 S 0.68606(16) 0.43469(8) 0.87964(13) 0.0297(6) Uani 1 1 d . . . . . Si1 Si 0.78129(17) 0.32947(9) 0.59020(14) 0.0260(6) Uani 1 1 d . . . . . Si2 Si 0.92419(18) 0.46505(9) 0.75867(15) 0.0290(7) Uani 1 1 d . . . . . Si3 Si 0.82253(18) 0.27859(9) 0.86252(14) 0.0270(7) Uani 1 1 d . . . . . Si4 Si 0.51302(17) 0.41934(9) 0.72044(13) 0.0228(6) Uani 1 1 d . . . . . O1 O 0.7633(4) 0.3510(2) 0.6671(3) 0.0270(16) Uani 1 1 d . . . . . O2 O 0.8782(4) 0.31169(19) 0.5938(3) 0.0261(16) Uani 1 1 d . . . . . O3 O 0.7768(4) 0.3697(2) 0.5255(3) 0.0283(16) Uani 1 1 d . . . . . O4 O 0.7221(4) 0.2835(2) 0.5641(3) 0.0281(16) Uani 1 1 d . . . . . O21 O 0.8416(4) 0.4342(2) 0.7504(3) 0.0293(16) Uani 1 1 d . . . . . O22 O 0.9978(4) 0.4232(2) 0.7510(4) 0.0358(18) Uani 1 1 d . . . . . O23 O 0.9339(4) 0.5090(2) 0.6994(3) 0.0339(17) Uani 1 1 d . . . . . O24 O 0.9413(4) 0.4920(2) 0.8342(3) 0.0385(18) Uani 1 1 d . . . . . O41 O 0.7853(4) 0.32495(19) 0.8200(3) 0.0261(15) Uani 1 1 d . . . . . O42 O 0.9112(4) 0.2674(2) 0.8263(3) 0.0335(17) Uani 1 1 d . . . . . O43 O 0.8329(4) 0.2861(2) 0.9467(3) 0.0336(17) Uani 1 1 d . . . . . O44 O 0.7702(4) 0.2268(2) 0.8515(3) 0.0382(18) Uani 1 1 d . . . . . O61 O 0.6040(4) 0.39834(19) 0.7208(3) 0.0237(15) Uani 1 1 d . . . . . O62 O 0.5071(4) 0.4796(2) 0.7381(3) 0.0292(16) Uani 1 1 d . . . . . O63 O 0.4574(4) 0.39979(19) 0.7862(3) 0.0251(15) Uani 1 1 d . . . . . O64 O 0.4704(4) 0.4064(2) 0.6438(3) 0.0299(16) Uani 1 1 d . . . . . O81 O 0.5376(5) 0.5766(2) 0.9518(4) 0.0404(19) Uani 1 1 d . . . . . O82 O 0.3902(5) 0.5478(3) 0.8823(4) 0.059(2) Uani 1 1 d . . . . . O83 O 0.3457(5) 0.4581(2) 0.9525(4) 0.052(2) Uani 1 1 d . . . . . C1 C 0.9320(6) 0.2971(3) 0.5385(5) 0.027(2) Uani 1 1 d . . . . . C2 C 0.8879(7) 0.2672(3) 0.4804(5) 0.044(3) Uani 1 1 d . . . . . H2C H 0.8607 0.2384 0.5015 0.065 Uiso 1 1 calc R U . . . H2D H 0.9277 0.2555 0.4460 0.065 Uiso 1 1 calc R U . . . H2E H 0.8470 0.2883 0.4562 0.065 Uiso 1 1 calc R U . . . C3 C 0.9692(7) 0.3429(3) 0.5061(5) 0.052(3) Uani 1 1 d . . . . . H3A H 0.9255 0.3644 0.4867 0.078 Uiso 1 1 calc R U . . . H3B H 1.0055 0.3330 0.4680 0.078 Uiso 1 1 calc R U . . . H3C H 1.0007 0.3612 0.5426 0.078 Uiso 1 1 calc R U . . . C4 C 0.9972(6) 0.2658(3) 0.5736(6) 0.049(3) Uani 1 1 d . . . . . H4A H 1.0258 0.2854 0.6105 0.074 Uiso 1 1 calc R U . . . H4B H 1.0364 0.2550 0.5383 0.074 Uiso 1 1 calc R U . . . H4C H 0.9721 0.2365 0.5952 0.074 Uiso 1 1 calc R U . . . C5 C 0.7086(6) 0.3881(4) 0.4811(5) 0.037(3) Uani 1 1 d . . . . . C6 C 0.7404(8) 0.4363(3) 0.4499(6) 0.070(4) Uani 1 1 d . . . . . H6A H 0.7619 0.4578 0.4882 0.105 Uiso 1 1 calc R U . . . H6B H 0.6957 0.4535 0.4244 0.105 Uiso 1 1 calc R U . . . H6C H 0.7842 0.4288 0.4170 0.105 Uiso 1 1 calc R U . . . C7 C 0.6911(7) 0.3507(3) 0.4222(5) 0.043(3) Uani 1 1 d . . . . . H7A H 0.7405 0.3461 0.3944 0.065 Uiso 1 1 calc R U . . . H7B H 0.6465 0.3632 0.3913 0.065 Uiso 1 1 calc R U . . . H7C H 0.6752 0.3187 0.4428 0.065 Uiso 1 1 calc R U . . . C8 C 0.6325(7) 0.3955(5) 0.5255(6) 0.086(5) Uani 1 1 d . . . . . H8A H 0.6182 0.3639 0.5481 0.129 Uiso 1 1 calc R U . . . H8B H 0.5868 0.4066 0.4948 0.129 Uiso 1 1 calc R U . . . H8C H 0.6438 0.4207 0.5621 0.129 Uiso 1 1 calc R U . . . C9 C 0.6901(7) 0.2409(4) 0.5999(6) 0.040(3) Uani 1 1 d . . . . . C10 C 0.6690(7) 0.2027(4) 0.5417(5) 0.060(4) Uani 1 1 d . . . . . H10A H 0.6318 0.2179 0.5063 0.090 Uiso 1 1 calc R U . . . H10B H 0.6424 0.1736 0.5628 0.090 Uiso 1 1 calc R U . . . H10C H 0.7193 0.1921 0.5188 0.090 Uiso 1 1 calc R U . . . C11 C 0.6142(7) 0.2561(4) 0.6375(6) 0.053(3) Uani 1 1 d . . . . . H11A H 0.6278 0.2823 0.6722 0.079 Uiso 1 1 calc R U . . . H11B H 0.5916 0.2272 0.6621 0.079 Uiso 1 1 calc R U . . . H11C H 0.5735 0.2688 0.6029 0.079 Uiso 1 1 calc R U . . . C12 C 0.7542(7) 0.2198(4) 0.6515(6) 0.057(4) Uani 1 1 d . . . . . H12A H 0.8070 0.2178 0.6282 0.085 Uiso 1 1 calc R U . . . H12B H 0.7376 0.1864 0.6666 0.085 Uiso 1 1 calc R U . . . H12C H 0.7593 0.2417 0.6930 0.085 Uiso 1 1 calc R U . . . C21 C 1.0860(7) 0.4257(4) 0.7662(6) 0.048(3) Uani 1 1 d . . . . . C22 C 1.1225(6) 0.3868(4) 0.7187(6) 0.066(4) Uani 1 1 d . . . . . H1 H 1.1036 0.3536 0.7328 0.099 Uiso 1 1 calc R U . . . H22A H 1.1824 0.3882 0.7231 0.099 Uiso 1 1 calc R U . . . H22B H 1.1053 0.3933 0.6694 0.099 Uiso 1 1 calc R U . . . C23 C 1.1182(7) 0.4770(3) 0.7458(6) 0.060(4) Uani 1 1 d . . . . . H23A H 1.1002 0.4848 0.6971 0.090 Uiso 1 1 calc R U . . . H23B H 1.1782 0.4769 0.7490 0.090 Uiso 1 1 calc R U . . . H23C H 1.0969 0.5022 0.7782 0.090 Uiso 1 1 calc R U . . . C24 C 1.1001(7) 0.4135(4) 0.8419(6) 0.071(4) Uani 1 1 d . . . . . H24A H 1.0696 0.4369 0.8712 0.107 Uiso 1 1 calc R U . . . H24B H 1.1588 0.4161 0.8538 0.107 Uiso 1 1 calc R U . . . H24C H 1.0814 0.3794 0.8510 0.107 Uiso 1 1 calc R U . . . C25 C 0.9098(7) 0.5111(3) 0.6258(6) 0.041(3) Uani 1 1 d . . . . . C26 C 0.8227(7) 0.5231(4) 0.6184(6) 0.056(4) Uani 1 1 d . . . . . H26A H 0.7902 0.4949 0.6348 0.084 Uiso 1 1 calc R U . . . H26B H 0.8088 0.5300 0.5685 0.084 Uiso 1 1 calc R U . . . H26C H 0.8108 0.5526 0.6471 0.084 Uiso 1 1 calc R U . . . C27 C 0.9279(7) 0.4614(3) 0.5896(5) 0.056(4) Uani 1 1 d . . . . . H27A H 0.9868 0.4544 0.5936 0.084 Uiso 1 1 calc R U . . . H27B H 0.9111 0.4632 0.5395 0.084 Uiso 1 1 calc R U . . . H27C H 0.8975 0.4346 0.6127 0.084 Uiso 1 1 calc R U . . . C28 C 0.9629(7) 0.5512(4) 0.5936(5) 0.060(4) Uani 1 1 d . . . . . H28A H 0.9520 0.5832 0.6165 0.090 Uiso 1 1 calc R U . . . H28B H 0.9503 0.5537 0.5427 0.090 Uiso 1 1 calc R U . . . H28C H 1.0208 0.5424 0.6010 0.090 Uiso 1 1 calc R U . . . C29 C 0.9084(7) 0.5375(4) 0.8642(6) 0.049(3) Uani 1 1 d . . . . . C30 C 0.8268(7) 0.5503(3) 0.8334(5) 0.052(3) Uani 1 1 d . . . . . H30A H 0.8308 0.5547 0.7820 0.078 Uiso 1 1 calc R U . . . H30B H 0.8075 0.5814 0.8546 0.078 Uiso 1 1 calc R U . . . H30C H 0.7881 0.5234 0.8432 0.078 Uiso 1 1 calc R U . . . C31 C 0.9062(15) 0.5374(10) 0.9375(11) 0.046(7) Uani 0.62(4) 1 d . U P A 1 H31A H 0.8642 0.5140 0.9529 0.069 Uiso 0.62(4) 1 calc R U P A 1 H31B H 0.8931 0.5710 0.9543 0.069 Uiso 0.62(4) 1 calc R U P A 1 H31C H 0.9598 0.5273 0.9572 0.069 Uiso 0.62(4) 1 calc R U P A 1 C31B C 0.893(2) 0.5112(17) 0.9474(16) 0.040(10) Uani 0.38(4) 1 d . U P A 2 H31D H 0.8427 0.4910 0.9456 0.060 Uiso 0.38(4) 1 calc R U P A 2 H31E H 0.8874 0.5378 0.9826 0.060 Uiso 0.38(4) 1 calc R U P A 2 H31F H 0.9396 0.4900 0.9606 0.060 Uiso 0.38(4) 1 calc R U P A 2 C32 C 0.9648(14) 0.5824(8) 0.8368(14) 0.048(7) Uani 0.62(4) 1 d . U P A 1 H32A H 1.0206 0.5785 0.8565 0.073 Uiso 0.62(4) 1 calc R U P A 1 H32B H 0.9421 0.6143 0.8522 0.073 Uiso 0.62(4) 1 calc R U P A 1 H32C H 0.9661 0.5816 0.7848 0.073 Uiso 0.62(4) 1 calc R U P A 1 C32B C 0.981(2) 0.5666(14) 0.876(3) 0.055(12) Uani 0.38(4) 1 d . U P A 2 H32D H 1.0228 0.5462 0.9000 0.083 Uiso 0.38(4) 1 calc R U P A 2 H32E H 0.9682 0.5955 0.9055 0.083 Uiso 0.38(4) 1 calc R U P A 2 H32F H 1.0012 0.5780 0.8303 0.083 Uiso 0.38(4) 1 calc R U P A 2 C41 C 0.9668(7) 0.2262(3) 0.8317(6) 0.036(3) Uani 1 1 d . . . . . C42 C 0.9478(8) 0.1927(3) 0.7706(5) 0.060(4) Uani 1 1 d . . . . . H42A H 0.8924 0.1791 0.7750 0.090 Uiso 1 1 calc R U . . . H42B H 0.9875 0.1653 0.7703 0.090 Uiso 1 1 calc R U . . . H42C H 0.9510 0.2116 0.7263 0.090 Uiso 1 1 calc R U . . . C43 C 1.0514(6) 0.2479(4) 0.8266(7) 0.066(4) Uani 1 1 d . . . . . H43A H 1.0573 0.2635 0.7800 0.099 Uiso 1 1 calc R U . . . H43B H 1.0921 0.2212 0.8326 0.099 Uiso 1 1 calc R U . . . H43C H 1.0600 0.2730 0.8638 0.099 Uiso 1 1 calc R U . . . C44 C 0.9583(7) 0.1975(3) 0.8997(5) 0.051(3) Uani 1 1 d . . . . . H44A H 0.9635 0.2204 0.9400 0.076 Uiso 1 1 calc R U . . . H44B H 1.0013 0.1721 0.9033 0.076 Uiso 1 1 calc R U . . . H44C H 0.9045 0.1813 0.8999 0.076 Uiso 1 1 calc R U . . . C45 C 0.8670(7) 0.3250(4) 0.9922(5) 0.039(3) Uani 1 1 d . . . . . C46 C 0.9178(8) 0.3609(4) 0.9491(6) 0.071(4) Uani 1 1 d . . . . . H46A H 0.9614 0.3425 0.9258 0.106 Uiso 1 1 calc R U . . . H46B H 0.9422 0.3863 0.9806 0.106 Uiso 1 1 calc R U . . . H46C H 0.8826 0.3772 0.9131 0.106 Uiso 1 1 calc R U . . . C47 C 0.9174(8) 0.2998(4) 1.0490(5) 0.070(4) Uani 1 1 d . . . . . H47A H 0.9253 0.3226 1.0892 0.106 Uiso 1 1 calc R U . . . H47B H 0.9708 0.2907 1.0302 0.106 Uiso 1 1 calc R U . . . H47C H 0.8891 0.2697 1.0646 0.106 Uiso 1 1 calc R U . . . C48 C 0.7962(7) 0.3531(4) 1.0235(6) 0.061(4) Uani 1 1 d . . . . . H48A H 0.7609 0.3664 0.9851 0.092 Uiso 1 1 calc R U . . . H48B H 0.8173 0.3808 1.0527 0.092 Uiso 1 1 calc R U . . . H48C H 0.7644 0.3305 1.0529 0.092 Uiso 1 1 calc R U . . . C49 C 0.6954(7) 0.2105(4) 0.8831(6) 0.043(3) Uani 1 1 d . . . . . C50 C 0.6532(8) 0.1775(4) 0.8279(6) 0.083(5) Uani 1 1 d . . . . . H50A H 0.6345 0.1980 0.7876 0.125 Uiso 1 1 calc R U . . . H50B H 0.6061 0.1610 0.8488 0.125 Uiso 1 1 calc R U . . . H50C H 0.6919 0.1523 0.8115 0.125 Uiso 1 1 calc R U . . . C51 C 0.6411(7) 0.2533(4) 0.9014(6) 0.067(4) Uani 1 1 d . . . . . H51A H 0.6706 0.2759 0.9339 0.101 Uiso 1 1 calc R U . . . H51B H 0.5920 0.2407 0.9241 0.101 Uiso 1 1 calc R U . . . H51C H 0.6252 0.2714 0.8580 0.101 Uiso 1 1 calc R U . . . C52 C 0.7191(8) 0.1811(4) 0.9482(6) 0.067(4) Uani 1 1 d . . . . . H52A H 0.7578 0.1548 0.9356 0.100 Uiso 1 1 calc R U . . . H52B H 0.6701 0.1660 0.9680 0.100 Uiso 1 1 calc R U . . . H52C H 0.7449 0.2033 0.9834 0.100 Uiso 1 1 calc R U . . . C61 C 0.5443(6) 0.5228(3) 0.7065(5) 0.026(2) Uani 1 1 d . . . . . C62 C 0.5938(9) 0.5088(4) 0.6441(6) 0.075(5) Uani 1 1 d . . . . . H62A H 0.6389 0.4869 0.6596 0.112 Uiso 1 1 calc R U . . . H62B H 0.6162 0.5390 0.6226 0.112 Uiso 1 1 calc R U . . . H62C H 0.5589 0.4913 0.6091 0.112 Uiso 1 1 calc R U . . . C63 C 0.4767(8) 0.5565(4) 0.6833(6) 0.069(4) Uani 1 1 d . . . . . H63A H 0.4423 0.5397 0.6473 0.104 Uiso 1 1 calc R U . . . H63B H 0.4996 0.5870 0.6632 0.104 Uiso 1 1 calc R U . . . H63C H 0.4435 0.5651 0.7241 0.104 Uiso 1 1 calc R U . . . C64 C 0.5985(7) 0.5468(3) 0.7626(5) 0.052(3) Uani 1 1 d . . . . . H2B H 0.5662 0.5542 0.8044 0.078 Uiso 1 1 calc R U . . . H64A H 0.6213 0.5778 0.7440 0.078 Uiso 1 1 calc R U . . . H64B H 0.6431 0.5240 0.7759 0.078 Uiso 1 1 calc R U . . . C65 C 0.4462(6) 0.3506(3) 0.8176(5) 0.030(2) Uani 1 1 d . . . . . C66 C 0.4913(6) 0.3511(3) 0.8876(5) 0.036(3) Uani 1 1 d . . . . . H66A H 0.5492 0.3588 0.8803 0.054 Uiso 1 1 calc R U . . . H66B H 0.4867 0.3183 0.9102 0.054 Uiso 1 1 calc R U . . . H2A H 0.4676 0.3766 0.9182 0.054 Uiso 1 1 calc R U . . . C67 C 0.4822(7) 0.3100(3) 0.7696(5) 0.045(3) Uani 1 1 d . . . . . H67A H 0.4547 0.3112 0.7228 0.067 Uiso 1 1 calc R U . . . H67B H 0.4737 0.2771 0.7910 0.067 Uiso 1 1 calc R U . . . H67C H 0.5410 0.3159 0.7645 0.067 Uiso 1 1 calc R U . . . C68 C 0.3564(6) 0.3434(3) 0.8267(5) 0.043(3) Uani 1 1 d . . . . . H68A H 0.3345 0.3715 0.8536 0.064 Uiso 1 1 calc R U . . . H68B H 0.3470 0.3123 0.8525 0.064 Uiso 1 1 calc R U . . . H68C H 0.3287 0.3418 0.7800 0.064 Uiso 1 1 calc R U . . . C69 C 0.3877(7) 0.4100(4) 0.6137(5) 0.039(3) Uani 1 1 d . . . . . C70 C 0.3982(7) 0.4339(4) 0.5415(5) 0.055(3) Uani 1 1 d . . . . . H70A H 0.4270 0.4658 0.5473 0.082 Uiso 1 1 calc R U . . . H70B H 0.3443 0.4397 0.5190 0.082 Uiso 1 1 calc R U . . . H70C H 0.4302 0.4117 0.5116 0.082 Uiso 1 1 calc R U . . . C71 C 0.3544(8) 0.3586(4) 0.6044(6) 0.065(4) Uani 1 1 d . . . . . H71A H 0.3883 0.3400 0.5713 0.098 Uiso 1 1 calc R U . . . H71B H 0.2981 0.3604 0.5855 0.098 Uiso 1 1 calc R U . . . H71C H 0.3550 0.3415 0.6504 0.098 Uiso 1 1 calc R U . . . C72 C 0.3328(7) 0.4413(4) 0.6594(5) 0.047(3) Uani 1 1 d . . . . . H72A H 0.3277 0.4254 0.7059 0.071 Uiso 1 1 calc R U . . . H72B H 0.2785 0.4441 0.6364 0.071 Uiso 1 1 calc R U . . . H72C H 0.3566 0.4746 0.6656 0.071 Uiso 1 1 calc R U . . . C81 C 0.4779(7) 0.6110(3) 0.9249(5) 0.043(3) Uani 1 1 d . . . . . H81A H 0.4904 0.6197 0.8753 0.051 Uiso 1 1 calc R U . . . H81B H 0.4803 0.6420 0.9535 0.051 Uiso 1 1 calc R U . . . C82 C 0.3941(7) 0.5895(4) 0.9274(6) 0.049(3) Uani 1 1 d . . . . . H82A H 0.3820 0.5794 0.9765 0.059 Uiso 1 1 calc R U . . . H82B H 0.3532 0.6147 0.9117 0.059 Uiso 1 1 calc R U . . . C83 C 0.3131(10) 0.5218(6) 0.8674(10) 0.042(4) Uani 0.691(19) 1 d . U P B 1 H83A H 0.3210 0.4959 0.8308 0.050 Uiso 0.691(19) 1 calc R U P B 1 H83B H 0.2713 0.5457 0.8494 0.050 Uiso 0.691(19) 1 calc R U P B 1 C83B C 0.308(2) 0.5378(14) 0.905(2) 0.041(4) Uani 0.309(19) 1 d . U P B 2 H83C H 0.2672 0.5558 0.8753 0.050 Uiso 0.309(19) 1 calc R U P B 2 H83D H 0.3017 0.5485 0.9552 0.050 Uiso 0.309(19) 1 calc R U P B 2 C84 C 0.2847(10) 0.4978(6) 0.9355(10) 0.041(4) Uani 0.691(19) 1 d . U P B 1 H84A H 0.2832 0.5227 0.9743 0.049 Uiso 0.691(19) 1 calc R U P B 1 H84B H 0.2293 0.4833 0.9286 0.049 Uiso 0.691(19) 1 calc R U P B 1 C84B C 0.296(2) 0.4837(15) 0.899(2) 0.040(4) Uani 0.309(19) 1 d . U P B 2 H84C H 0.2375 0.4754 0.9050 0.048 Uiso 0.309(19) 1 calc R U P B 2 H84D H 0.3118 0.4725 0.8511 0.048 Uiso 0.309(19) 1 calc R U P B 2 C85 C 0.3245(7) 0.4408(4) 1.0188(5) 0.045(3) Uani 1 1 d . . . . . H85A H 0.2688 0.4263 1.0158 0.054 Uiso 1 1 calc R U . . . H85B H 0.3236 0.4691 1.0524 0.054 Uiso 1 1 calc R U . . . C86 C 0.3828(7) 0.4028(3) 1.0456(5) 0.043(3) Uani 1 1 d . . . . . H86A H 0.3674 0.3918 1.0936 0.052 Uiso 1 1 calc R U . . . H86B H 0.3815 0.3733 1.0139 0.052 Uiso 1 1 calc R U . . . C91 C 0.7517(14) 0.3082(8) 1.2133(8) 0.090(5) Uani 1 1 d . . . . . C92 C 0.8308(13) 0.2981(7) 1.2308(9) 0.102(6) Uani 1 1 d . . . . . H92 H 0.8508 0.2654 1.2227 0.122 Uiso 1 1 calc R U . . . C93 C 0.8842(16) 0.3334(7) 1.2600(10) 0.123(9) Uani 1 1 d . . . . . H93 H 0.9399 0.3252 1.2701 0.148 Uiso 1 1 calc R U . . . C94 C 0.8571(15) 0.3774(11) 1.2732(11) 0.145(10) Uani 1 1 d . . . . . H94 H 0.8927 0.4024 1.2922 0.175 Uiso 1 1 calc R U . . . C95 C 0.7767(17) 0.3878(8) 1.2596(9) 0.115(7) Uani 1 1 d . . . . . H95 H 0.7576 0.4199 1.2725 0.138 Uiso 1 1 calc R U . . . C96 C 0.7191(12) 0.3546(8) 1.2279(7) 0.092(6) Uani 1 1 d . . . . . H96 H 0.6637 0.3633 1.2177 0.111 Uiso 1 1 calc R U . . . C97 C 0.7051(11) 0.2694(6) 1.1809(8) 0.127(7) Uani 1 1 d . U . . . H97A H 0.7351 0.2557 1.1411 0.190 Uiso 1 1 calc R U . . . H97B H 0.6524 0.2828 1.1635 0.190 Uiso 1 1 calc R U . . . H97C H 0.6955 0.2431 1.2157 0.190 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 U1 0.01896(17) 0.01793(16) 0.02205(17) -0.00029(18) 0.00200(14) 0.00154(18) K1 0.0227(12) 0.0269(11) 0.0322(12) -0.0025(10) 0.0033(11) 0.0025(9) K2 0.0347(14) 0.0313(12) 0.0363(13) -0.0033(11) 0.0085(12) 0.0066(10) S1 0.0319(16) 0.0294(13) 0.0280(14) -0.0066(11) 0.0043(13) 0.0043(12) Si1 0.0269(17) 0.0247(14) 0.0266(15) -0.0037(12) 0.0035(14) 0.0042(13) Si2 0.0218(16) 0.0290(15) 0.0366(17) -0.0037(14) 0.0095(14) -0.0028(13) Si3 0.0297(17) 0.0233(14) 0.0283(16) 0.0034(12) 0.0033(14) 0.0048(12) Si4 0.0229(16) 0.0255(14) 0.0202(14) -0.0022(12) 0.0022(13) 0.0042(12) O1 0.022(4) 0.025(3) 0.033(4) -0.008(3) 0.001(3) 0.005(3) O2 0.024(4) 0.024(3) 0.030(4) -0.006(3) 0.010(3) 0.007(3) O3 0.029(4) 0.029(3) 0.027(4) 0.002(3) 0.003(3) 0.003(3) O4 0.032(4) 0.029(3) 0.024(4) -0.002(3) -0.001(3) -0.012(3) O21 0.019(4) 0.042(4) 0.027(4) -0.002(3) -0.003(3) -0.006(3) O22 0.028(4) 0.024(3) 0.056(5) -0.010(3) 0.004(4) -0.005(3) O23 0.041(5) 0.023(3) 0.039(4) -0.002(3) 0.010(4) -0.007(3) O24 0.037(5) 0.044(4) 0.034(4) -0.011(3) 0.001(4) -0.010(4) O41 0.035(4) 0.022(3) 0.022(3) -0.005(3) 0.004(3) 0.002(3) O42 0.028(4) 0.026(3) 0.047(4) 0.015(3) 0.006(4) 0.013(3) O43 0.035(5) 0.045(4) 0.022(4) 0.000(3) 0.005(3) 0.004(3) O44 0.038(5) 0.031(4) 0.046(4) 0.006(3) 0.010(4) 0.003(3) O61 0.027(4) 0.025(3) 0.020(3) -0.011(3) 0.007(3) 0.005(3) O62 0.035(4) 0.024(3) 0.029(4) 0.001(3) 0.004(4) 0.002(3) O63 0.022(4) 0.021(3) 0.033(4) 0.005(3) 0.009(3) 0.002(3) O64 0.028(4) 0.041(4) 0.021(4) -0.005(3) 0.001(3) 0.011(3) O81 0.046(5) 0.031(4) 0.045(5) -0.001(3) 0.009(4) -0.005(4) O82 0.037(5) 0.049(5) 0.091(7) 0.008(5) -0.003(5) 0.008(4) O83 0.036(5) 0.045(5) 0.077(6) 0.015(4) 0.004(5) -0.010(4) C1 0.026(6) 0.019(5) 0.035(6) -0.001(5) 0.002(5) 0.007(4) C2 0.052(8) 0.036(6) 0.043(7) -0.014(5) 0.011(6) 0.021(6) C3 0.060(9) 0.050(7) 0.046(7) 0.004(6) 0.025(7) 0.005(6) C4 0.039(7) 0.045(7) 0.065(8) 0.003(6) 0.016(7) 0.019(6) C5 0.036(6) 0.041(6) 0.034(6) 0.004(6) -0.007(5) 0.018(6) C6 0.110(13) 0.035(7) 0.062(8) 0.025(6) -0.030(9) 0.004(7) C7 0.060(9) 0.049(7) 0.020(6) 0.002(5) -0.004(6) -0.008(6) C8 0.073(11) 0.131(12) 0.053(8) 0.007(9) -0.005(8) 0.071(10) C9 0.030(7) 0.036(6) 0.053(7) 0.001(6) 0.011(6) -0.004(5) C10 0.077(10) 0.046(7) 0.057(8) -0.009(6) 0.002(8) -0.032(7) C11 0.042(8) 0.061(8) 0.055(8) -0.011(6) 0.012(7) -0.009(6) C12 0.060(9) 0.047(7) 0.063(8) 0.020(6) 0.005(8) -0.010(6) C21 0.024(7) 0.054(7) 0.064(9) -0.005(7) -0.004(7) -0.002(6) C22 0.029(7) 0.048(7) 0.122(11) -0.004(8) 0.013(8) -0.013(6) C23 0.030(7) 0.045(7) 0.105(10) -0.014(7) 0.011(8) -0.017(6) C24 0.027(8) 0.106(11) 0.079(10) 0.001(8) -0.012(8) 0.009(7) C25 0.056(8) 0.029(6) 0.038(7) 0.010(5) 0.016(7) 0.005(6) C26 0.068(10) 0.050(7) 0.050(8) -0.003(6) 0.007(8) 0.015(7) C27 0.080(10) 0.046(7) 0.043(7) -0.014(6) 0.027(7) -0.015(7) C28 0.074(10) 0.056(7) 0.053(8) 0.012(6) 0.022(8) -0.017(7) C29 0.033(7) 0.063(8) 0.052(8) -0.046(7) 0.009(6) -0.006(6) C30 0.068(10) 0.034(6) 0.054(8) -0.009(6) -0.001(7) 0.010(6) C31 0.049(10) 0.044(10) 0.046(10) -0.006(8) 0.005(8) -0.002(8) C31B 0.030(16) 0.058(18) 0.031(15) -0.001(14) -0.010(12) 0.006(14) C32 0.049(10) 0.045(9) 0.052(10) -0.015(8) 0.006(8) -0.021(7) C32B 0.054(18) 0.040(16) 0.07(2) -0.025(15) -0.004(15) -0.001(13) C41 0.035(7) 0.025(5) 0.050(7) 0.004(5) 0.011(6) 0.012(5) C42 0.084(11) 0.029(6) 0.066(8) 0.005(6) -0.005(8) 0.036(6) C43 0.027(7) 0.061(8) 0.109(11) 0.041(8) 0.018(8) 0.026(6) C44 0.057(9) 0.041(6) 0.055(8) 0.018(6) 0.006(7) 0.016(6) C45 0.047(8) 0.046(7) 0.025(6) -0.005(5) 0.011(6) -0.002(6) C46 0.081(11) 0.081(9) 0.050(8) -0.032(7) -0.001(8) -0.029(8) C47 0.091(11) 0.069(8) 0.050(8) -0.013(7) -0.037(8) 0.040(8) C48 0.071(10) 0.066(8) 0.047(8) -0.002(6) 0.005(8) 0.031(7) C49 0.032(7) 0.050(7) 0.047(7) 0.025(6) 0.006(6) -0.008(6) C50 0.088(12) 0.079(9) 0.082(10) 0.020(8) -0.001(10) -0.046(9) C51 0.031(8) 0.067(8) 0.104(11) 0.032(8) 0.023(8) 0.012(6) C52 0.063(10) 0.069(8) 0.068(9) 0.040(7) -0.002(8) -0.011(7) C61 0.038(7) 0.020(5) 0.022(5) 0.006(4) 0.014(5) -0.004(5) C62 0.116(14) 0.050(8) 0.060(9) 0.002(7) 0.038(9) -0.010(8) C63 0.077(11) 0.035(7) 0.094(10) 0.016(7) -0.025(9) 0.000(7) C64 0.070(9) 0.038(6) 0.048(7) 0.017(6) -0.014(7) -0.026(6) C65 0.036(7) 0.023(5) 0.032(6) 0.004(5) 0.008(5) -0.006(5) C66 0.044(7) 0.026(5) 0.038(6) -0.003(5) 0.012(6) 0.001(5) C67 0.064(9) 0.022(5) 0.048(7) 0.000(5) -0.002(7) 0.003(5) C68 0.044(8) 0.043(6) 0.042(7) 0.006(5) 0.008(6) -0.009(6) C69 0.043(8) 0.043(6) 0.030(6) 0.000(5) -0.007(6) 0.005(6) C70 0.040(8) 0.080(9) 0.044(7) 0.019(6) -0.008(6) 0.003(7) C71 0.070(10) 0.065(8) 0.061(9) -0.027(7) -0.022(8) 0.004(7) C72 0.039(7) 0.062(7) 0.040(7) 0.006(6) -0.007(6) -0.003(6) C81 0.072(9) 0.022(5) 0.034(6) -0.002(5) 0.015(6) 0.008(6) C82 0.047(8) 0.059(8) 0.042(7) 0.007(6) 0.016(7) 0.030(6) C83 0.034(7) 0.054(9) 0.038(10) -0.022(7) -0.001(8) 0.009(7) C83B 0.031(8) 0.055(10) 0.037(11) -0.018(8) -0.004(9) 0.007(8) C84 0.032(7) 0.053(9) 0.037(10) -0.020(7) -0.006(8) 0.004(7) C84B 0.031(8) 0.054(10) 0.034(11) -0.021(8) -0.002(9) 0.005(8) C85 0.038(7) 0.041(7) 0.057(8) -0.020(6) 0.023(7) -0.010(6) C86 0.064(9) 0.038(7) 0.029(6) -0.003(5) 0.012(6) -0.016(6) C91 0.104(17) 0.109(15) 0.057(11) 0.026(10) 0.004(11) -0.022(12) C92 0.115(19) 0.086(13) 0.105(15) 0.047(12) 0.003(14) 0.019(12) C93 0.19(3) 0.072(12) 0.106(16) 0.017(12) 0.028(17) 0.027(16) C94 0.11(2) 0.20(3) 0.127(18) -0.023(19) -0.001(18) -0.07(2) C95 0.18(2) 0.106(15) 0.058(11) 0.006(11) 0.037(15) 0.000(18) C96 0.118(18) 0.112(15) 0.048(10) 0.009(10) 0.028(11) 0.029(14) C97 0.128(14) 0.166(13) 0.087(11) 0.011(10) 0.008(11) -0.066(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O61 U1 O41 129.0(2) . . O61 U1 O21 130.9(2) . . O41 U1 O21 98.0(2) . . O61 U1 O1 87.7(2) . . O41 U1 O1 83.63(19) . . O21 U1 O1 83.9(2) . . O61 U1 S1 91.29(14) . . O41 U1 S1 96.78(15) . . O21 U1 S1 96.91(16) . . O1 U1 S1 178.99(17) . . O61 U1 K1 139.48(13) . . O41 U1 K1 54.20(16) . . O21 U1 K1 55.57(15) . . O1 U1 K1 51.79(15) . . S1 U1 K1 129.18(7) . . O2 K1 O22 120.1(2) . . O2 K1 O42 117.77(19) . . O22 K1 O42 121.1(2) . . O2 K1 O1 56.44(17) . . O22 K1 O1 112.36(19) . . O42 K1 O1 107.6(2) . . O2 K1 O41 111.07(19) . . O22 K1 O41 110.72(19) . . O42 K1 O41 54.86(18) . . O1 K1 O41 63.10(17) . . O2 K1 O21 105.59(17) . . O22 K1 O21 54.20(18) . . O42 K1 O21 118.15(18) . . O1 K1 O21 62.76(16) . . O41 K1 O21 69.94(16) . . O2 K1 Si1 28.60(13) . . O22 K1 Si1 119.52(16) . . O42 K1 Si1 116.23(16) . . O1 K1 Si1 27.85(12) . . O41 K1 Si1 86.88(14) . . O21 K1 Si1 83.27(13) . . O2 K1 Si3 117.83(15) . . O22 K1 Si3 119.18(16) . . O42 K1 Si3 27.58(14) . . O1 K1 Si3 85.12(14) . . O41 K1 Si3 27.28(12) . . O21 K1 Si3 93.96(13) . . Si1 K1 Si3 102.65(9) . . O2 K1 Si2 114.98(14) . . O22 K1 Si2 27.25(15) . . O42 K1 Si2 124.31(15) . . O1 K1 Si2 87.14(13) . . O41 K1 Si2 90.63(12) . . O21 K1 Si2 26.96(12) . . Si1 K1 Si2 101.63(8) . . Si3 K1 Si2 108.68(8) . . O2 K1 U1 95.62(14) . . O22 K1 U1 91.63(15) . . O42 K1 U1 93.18(14) . . O1 K1 U1 39.29(12) . . O41 K1 U1 38.33(11) . . O21 K1 U1 38.46(12) . . Si1 K1 U1 67.04(6) . . Si3 K1 U1 65.61(6) . . Si2 K1 U1 64.89(6) . . O82 K2 O62 85.7(2) . . O82 K2 O63 105.9(2) . . O62 K2 O63 50.42(15) . . O82 K2 O83 60.1(2) . . O62 K2 O83 115.3(2) . . O63 K2 O83 86.03(19) . . O82 K2 O81 58.5(2) . . O62 K2 O81 109.39(18) . . O63 K2 O81 157.75(18) . . O83 K2 O81 97.3(2) . . O82 K2 S1 152.93(19) . . O62 K2 S1 85.56(14) . . O63 K2 S1 87.89(13) . . O83 K2 S1 145.73(16) . . O81 K2 S1 100.85(16) . . O82 K2 O81 100.3(2) . 3_667 O62 K2 O81 155.10(17) . 3_667 O63 K2 O81 104.93(16) . 3_667 O83 K2 O81 51.3(2) . 3_667 O81 K2 O81 94.10(16) . 3_667 S1 K2 O81 98.35(15) . 3_667 O82 K2 Si4 106.3(2) . . O62 K2 Si4 27.46(11) . . O63 K2 Si4 27.29(11) . . O83 K2 Si4 110.12(17) . . O81 K2 Si4 135.83(15) . . S1 K2 Si4 75.36(8) . . O81 K2 Si4 130.07(12) 3_667 . O82 K2 K2 77.15(19) . 3_667 O62 K2 K2 158.62(14) . 3_667 O63 K2 K2 147.07(14) . 3_667 O83 K2 K2 66.74(16) . 3_667 O81 K2 K2 50.48(13) . 3_667 S1 K2 K2 104.04(9) . 3_667 O81 K2 K2 43.61(11) 3_667 3_667 Si4 K2 K2 173.67(9) . 3_667 U1 S1 K2 119.38(10) . . O1 Si1 O3 115.8(3) . . O1 Si1 O4 115.2(4) . . O3 Si1 O4 105.0(3) . . O1 Si1 O2 105.4(3) . . O3 Si1 O2 104.3(3) . . O4 Si1 O2 110.7(3) . . O1 Si1 K1 55.1(2) . . O3 Si1 K1 122.8(2) . . O4 Si1 K1 130.9(2) . . O2 Si1 K1 50.3(2) . . O21 Si2 O24 116.6(4) . . O21 Si2 O23 114.0(4) . . O24 Si2 O23 105.3(3) . . O21 Si2 O22 104.8(3) . . O24 Si2 O22 105.7(4) . . O23 Si2 O22 110.2(4) . . O21 Si2 K1 57.3(2) . . O24 Si2 K1 126.8(3) . . O23 Si2 K1 126.1(2) . . O22 Si2 K1 47.5(2) . . O41 Si3 O43 115.5(3) . . O41 Si3 O44 114.0(4) . . O43 Si3 O44 105.8(4) . . O41 Si3 O42 105.2(3) . . O43 Si3 O42 111.2(4) . . O44 Si3 O42 104.8(3) . . O41 Si3 K1 56.4(2) . . O43 Si3 K1 130.0(3) . . O44 Si3 K1 122.8(3) . . O42 Si3 K1 48.7(2) . . O61 Si4 O64 107.9(3) . . O61 Si4 O63 114.8(3) . . O64 Si4 O63 111.8(3) . . O61 Si4 O62 113.9(3) . . O64 Si4 O62 111.2(3) . . O63 Si4 O62 97.1(3) . . O61 Si4 K2 101.1(2) . . O64 Si4 K2 151.0(3) . . O63 Si4 K2 54.4(2) . . O62 Si4 K2 53.6(2) . . Si1 O1 U1 171.7(4) . . Si1 O1 K1 97.1(3) . . U1 O1 K1 88.93(19) . . C1 O2 Si1 130.7(5) . . C1 O2 K1 126.9(5) . . Si1 O2 K1 101.1(3) . . C5 O3 Si1 132.3(6) . . C9 O4 Si1 132.8(6) . . Si2 O21 U1 166.0(4) . . Si2 O21 K1 95.7(3) . . U1 O21 K1 85.97(18) . . C21 O22 Si2 131.8(6) . . C21 O22 K1 122.1(6) . . Si2 O22 K1 105.2(3) . . C25 O23 Si2 131.4(6) . . C29 O24 Si2 131.4(7) . . Si3 O41 U1 175.9(4) . . Si3 O41 K1 96.3(3) . . U1 O41 K1 87.46(18) . . C41 O42 Si3 132.4(6) . . C41 O42 K1 122.8(6) . . Si3 O42 K1 103.7(3) . . C45 O43 Si3 134.7(6) . . C49 O44 Si3 130.6(7) . . Si4 O61 U1 152.6(3) . . C61 O62 Si4 132.3(6) . . C61 O62 K2 117.6(5) . . Si4 O62 K2 98.9(3) . . C65 O63 Si4 132.3(5) . . C65 O63 K2 112.4(5) . . Si4 O63 K2 98.3(2) . . C69 O64 Si4 134.8(6) . . C86 O81 C81 112.3(7) 3_667 . C86 O81 K2 121.0(6) 3_667 . C81 O81 K2 110.4(6) . . C86 O81 K2 110.3(6) 3_667 3_667 C81 O81 K2 114.5(5) . 3_667 K2 O81 K2 85.90(16) . 3_667 C82 O82 C83B 89.7(17) . . C82 O82 C83 121.5(10) . . C82 O82 K2 121.0(6) . . C83B O82 K2 119.8(16) . . C83 O82 K2 105.2(8) . . C85 O83 C84B 129.6(19) . . C85 O83 C84 104.6(10) . . C85 O83 K2 130.8(6) . . C84B O83 K2 98.3(17) . . C84 O83 K2 114.2(8) . . O2 C1 C4 105.8(7) . . O2 C1 C3 109.5(7) . . C4 C1 C3 110.4(9) . . O2 C1 C2 112.3(8) . . C4 C1 C2 109.9(7) . . C3 C1 C2 109.0(8) . . C1 C2 H2C 109.5 . . C1 C2 H2D 109.5 . . H2C C2 H2D 109.5 . . C1 C2 H2E 109.5 . . H2C C2 H2E 109.5 . . H2D C2 H2E 109.5 . . C1 C3 H3A 109.5 . . C1 C3 H3B 109.5 . . H3A C3 H3B 109.5 . . C1 C3 H3C 109.5 . . H3A C3 H3C 109.5 . . H3B C3 H3C 109.5 . . C1 C4 H4A 109.5 . . C1 C4 H4B 109.5 . . H4A C4 H4B 109.5 . . C1 C4 H4C 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . O3 C5 C6 104.3(8) . . O3 C5 C7 108.8(7) . . C6 C5 C7 109.7(8) . . O3 C5 C8 110.4(8) . . C6 C5 C8 113.2(9) . . C7 C5 C8 110.2(9) . . C5 C6 H6A 109.5 . . C5 C6 H6B 109.5 . . H6A C6 H6B 109.5 . . C5 C6 H6C 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C5 C7 H7A 109.5 . . C5 C7 H7B 109.5 . . H7A C7 H7B 109.5 . . C5 C7 H7C 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C5 C8 H8A 109.5 . . C5 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . C5 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . O4 C9 C11 108.7(8) . . O4 C9 C12 110.1(9) . . C11 C9 C12 111.2(9) . . O4 C9 C10 105.8(8) . . C11 C9 C10 110.3(9) . . C12 C9 C10 110.5(9) . . C9 C10 H10A 109.5 . . C9 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . C9 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C9 C11 H11A 109.5 . . C9 C11 H11B 109.5 . . H11A C11 H11B 109.5 . . C9 C11 H11C 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 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 . . O22 C21 C24 107.9(10) . . O22 C21 C22 104.7(8) . . C24 C21 C22 111.5(10) . . O22 C21 C23 109.6(9) . . C24 C21 C23 113.4(10) . . C22 C21 C23 109.2(10) . . C21 C22 H1 109.5 . . C21 C22 H22A 109.5 . . H1 C22 H22A 109.5 . . C21 C22 H22B 109.5 . . H1 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . C21 C23 H23A 109.5 . . C21 C23 H23B 109.5 . . H23A C23 H23B 109.5 . . C21 C23 H23C 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C21 C24 H24A 109.5 . . C21 C24 H24B 109.5 . . H24A C24 H24B 109.5 . . C21 C24 H24C 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . O23 C25 C26 110.0(9) . . O23 C25 C28 105.6(9) . . C26 C25 C28 111.7(9) . . O23 C25 C27 110.3(8) . . C26 C25 C27 110.4(10) . . C28 C25 C27 108.7(9) . . C25 C26 H26A 109.5 . . C25 C26 H26B 109.5 . . H26A C26 H26B 109.5 . . C25 C26 H26C 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C25 C27 H27A 109.5 . . C25 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . C25 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C25 C28 H28A 109.5 . . C25 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . C25 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . C31 C29 O24 114.0(14) . . C32B C29 O24 101.8(15) . . C31 C29 C30 110.3(13) . . C32B C29 C30 132(2) . . O24 C29 C30 112.4(8) . . C31 C29 C32 110.6(13) . . O24 C29 C32 106.3(10) . . C30 C29 C32 102.6(14) . . C32B C29 C31B 103(2) . . O24 C29 C31B 94.3(15) . . C30 C29 C31B 107.2(13) . . C29 C30 H30A 109.5 . . C29 C30 H30B 109.5 . . H30A C30 H30B 109.5 . . C29 C30 H30C 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . C29 C31 H31A 109.5 . . C29 C31 H31B 109.5 . . H31A C31 H31B 109.5 . . C29 C31 H31C 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C29 C31B H31D 109.5 . . C29 C31B H31E 109.5 . . H31D C31B H31E 109.5 . . C29 C31B H31F 109.5 . . H31D C31B H31F 109.5 . . H31E C31B H31F 109.5 . . C29 C32 H32A 109.5 . . C29 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C29 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . C29 C32B H32D 109.5 . . C29 C32B H32E 109.5 . . H32D C32B H32E 109.5 . . C29 C32B H32F 109.5 . . H32D C32B H32F 109.5 . . H32E C32B H32F 109.5 . . O42 C41 C42 107.0(8) . . O42 C41 C43 106.3(7) . . C42 C41 C43 110.9(10) . . O42 C41 C44 112.5(8) . . C42 C41 C44 109.2(8) . . C43 C41 C44 110.9(10) . . C41 C42 H42A 109.5 . . C41 C42 H42B 109.5 . . H42A C42 H42B 109.5 . . C41 C42 H42C 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . C41 C43 H43A 109.5 . . C41 C43 H43B 109.5 . . H43A C43 H43B 109.5 . . C41 C43 H43C 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 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 . . O43 C45 C47 107.1(8) . . O43 C45 C48 107.7(9) . . C47 C45 C48 111.0(9) . . O43 C45 C46 110.2(8) . . C47 C45 C46 111.7(11) . . C48 C45 C46 109.1(9) . . C45 C46 H46A 109.5 . . C45 C46 H46B 109.5 . . H46A C46 H46B 109.5 . . C45 C46 H46C 109.5 . . H46A C46 H46C 109.5 . . H46B C46 H46C 109.5 . . C45 C47 H47A 109.5 . . C45 C47 H47B 109.5 . . H47A C47 H47B 109.5 . . C45 C47 H47C 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . C45 C48 H48A 109.5 . . C45 C48 H48B 109.5 . . H48A C48 H48B 109.5 . . C45 C48 H48C 109.5 . . H48A C48 H48C 109.5 . . H48B C48 H48C 109.5 . . O44 C49 C51 112.0(8) . . O44 C49 C52 107.1(9) . . C51 C49 C52 110.9(10) . . O44 C49 C50 105.6(9) . . C51 C49 C50 110.1(10) . . C52 C49 C50 111.0(9) . . C49 C50 H50A 109.5 . . C49 C50 H50B 109.5 . . H50A C50 H50B 109.5 . . C49 C50 H50C 109.5 . . H50A C50 H50C 109.5 . . H50B C50 H50C 109.5 . . C49 C51 H51A 109.5 . . C49 C51 H51B 109.5 . . H51A C51 H51B 109.5 . . C49 C51 H51C 109.5 . . H51A C51 H51C 109.5 . . H51B C51 H51C 109.5 . . C49 C52 H52A 109.5 . . C49 C52 H52B 109.5 . . H52A C52 H52B 109.5 . . C49 C52 H52C 109.5 . . H52A C52 H52C 109.5 . . H52B C52 H52C 109.5 . . O62 C61 C63 107.0(8) . . O62 C61 C62 111.5(7) . . C63 C61 C62 109.6(9) . . O62 C61 C64 107.3(7) . . C63 C61 C64 111.5(8) . . C62 C61 C64 109.9(9) . . C61 C62 H62A 109.5 . . C61 C62 H62B 109.5 . . H62A C62 H62B 109.5 . . C61 C62 H62C 109.5 . . H62A C62 H62C 109.5 . . H62B C62 H62C 109.5 . . C61 C63 H63A 109.5 . . C61 C63 H63B 109.5 . . H63A C63 H63B 109.5 . . C61 C63 H63C 109.5 . . H63A C63 H63C 109.5 . . H63B C63 H63C 109.5 . . C61 C64 H2B 109.5 . . C61 C64 H64A 109.5 . . H2B C64 H64A 109.5 . . C61 C64 H64B 109.5 . . H2B C64 H64B 109.5 . . H64A C64 H64B 109.5 . . O63 C65 C68 107.3(8) . . O63 C65 C66 106.6(7) . . C68 C65 C66 111.3(9) . . O63 C65 C67 110.3(7) . . C68 C65 C67 111.6(8) . . C66 C65 C67 109.7(8) . . C65 C66 H66A 109.5 . . C65 C66 H66B 109.5 . . H66A C66 H66B 109.5 . . C65 C66 H2A 109.5 . . H66A C66 H2A 109.5 . . H66B C66 H2A 109.5 . . C65 C67 H67A 109.5 . . C65 C67 H67B 109.5 . . H67A C67 H67B 109.5 . . C65 C67 H67C 109.5 . . H67A C67 H67C 109.5 . . H67B C67 H67C 109.5 . . C65 C68 H68A 109.5 . . C65 C68 H68B 109.5 . . H68A C68 H68B 109.5 . . C65 C68 H68C 109.5 . . H68A C68 H68C 109.5 . . H68B C68 H68C 109.5 . . O64 C69 C71 108.5(8) . . O64 C69 C72 111.8(8) . . C71 C69 C72 111.1(10) . . O64 C69 C70 104.6(9) . . C71 C69 C70 109.5(9) . . C72 C69 C70 111.1(9) . . C69 C70 H70A 109.5 . . C69 C70 H70B 109.5 . . H70A C70 H70B 109.5 . . C69 C70 H70C 109.5 . . H70A C70 H70C 109.5 . . H70B C70 H70C 109.5 . . C69 C71 H71A 109.5 . . C69 C71 H71B 109.5 . . H71A C71 H71B 109.5 . . C69 C71 H71C 109.5 . . H71A C71 H71C 109.5 . . H71B C71 H71C 109.5 . . C69 C72 H72A 109.5 . . C69 C72 H72B 109.5 . . H72A C72 H72B 109.5 . . C69 C72 H72C 109.5 . . H72A C72 H72C 109.5 . . H72B C72 H72C 109.5 . . O81 C81 C82 111.1(8) . . O81 C81 H81A 109.4 . . C82 C81 H81A 109.4 . . O81 C81 H81B 109.4 . . C82 C81 H81B 109.4 . . H81A C81 H81B 108.0 . . O82 C82 C81 108.5(8) . . O82 C82 H82A 110.0 . . C81 C82 H82A 110.0 . . O82 C82 H82B 110.0 . . C81 C82 H82B 110.0 . . H82A C82 H82B 108.4 . . O82 C83 C84 108.6(14) . . O82 C83 H83A 110.0 . . C84 C83 H83A 110.0 . . O82 C83 H83B 110.0 . . C84 C83 H83B 110.0 . . H83A C83 H83B 108.3 . . O82 C83B C84B 106(3) . . O82 C83B H83C 110.5 . . C84B C83B H83C 110.5 . . O82 C83B H83D 110.5 . . C84B C83B H83D 110.5 . . H83C C83B H83D 108.7 . . O83 C84 C83 105.5(14) . . O83 C84 H84A 110.6 . . C83 C84 H84A 110.6 . . O83 C84 H84B 110.6 . . C83 C84 H84B 110.6 . . H84A C84 H84B 108.8 . . O83 C84B C83B 110(3) . . O83 C84B H84C 109.7 . . C83B C84B H84C 109.7 . . O83 C84B H84D 109.7 . . C83B C84B H84D 109.7 . . H84C C84B H84D 108.2 . . O83 C85 C86 111.5(9) . . O83 C85 H85A 109.3 . . C86 C85 H85A 109.3 . . O83 C85 H85B 109.3 . . C86 C85 H85B 109.3 . . H85A C85 H85B 108.0 . . O81 C86 C85 109.0(8) 3_667 . O81 C86 H86A 109.9 3_667 . C85 C86 H86A 109.9 . . O81 C86 H86B 109.9 3_667 . C85 C86 H86B 109.9 . . H86A C86 H86B 108.3 . . C92 C91 C96 120.1(18) . . C92 C91 C97 117(2) . . C96 C91 C97 123(2) . . C91 C92 C93 123(2) . . C91 C92 H92 118.5 . . C93 C92 H92 118.5 . . C94 C93 C92 119(3) . . C94 C93 H93 120.5 . . C92 C93 H93 120.5 . . C93 C94 C95 119(2) . . C93 C94 H94 120.5 . . C95 C94 H94 120.5 . . C94 C95 C96 125(2) . . C94 C95 H95 117.3 . . C96 C95 H95 117.3 . . C91 C96 C95 113.2(19) . . C91 C96 H96 123.4 . . C95 C96 H96 123.4 . . C91 C97 H97A 109.5 . . C91 C97 H97B 109.5 . . H97A C97 H97B 109.5 . . C91 C97 H97C 109.5 . . H97A C97 H97C 109.5 . . H97B C97 H97C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 O61 2.200(6) . U1 O41 2.212(5) . U1 O21 2.221(6) . U1 O1 2.256(6) . U1 S1 2.534(2) . U1 K1 3.562(2) . K1 O2 2.657(6) . K1 O22 2.662(6) . K1 O42 2.670(6) . K1 O1 2.799(6) . K1 O41 2.892(6) . K1 O21 2.946(6) . K1 Si1 3.388(3) . K1 Si3 3.451(3) . K1 Si2 3.482(3) . K2 O82 2.740(7) . K2 O62 2.886(6) . K2 O63 2.911(6) . K2 O83 2.935(8) . K2 O81 3.006(6) . K2 S1 3.128(3) . K2 O81 3.361(7) 3_667 K2 Si4 3.542(3) . K2 K2 4.346(4) 3_667 Si1 O1 1.595(6) . Si1 O3 1.628(6) . Si1 O4 1.634(6) . Si1 O2 1.653(6) . Si2 O21 1.587(6) . Si2 O24 1.615(6) . Si2 O23 1.634(6) . Si2 O22 1.652(7) . Si3 O41 1.591(6) . Si3 O43 1.604(6) . Si3 O44 1.639(7) . Si3 O42 1.644(7) . Si4 O61 1.589(6) . Si4 O64 1.625(6) . Si4 O63 1.641(6) . Si4 O62 1.653(6) . O2 C1 1.436(10) . O3 C5 1.461(10) . O4 C9 1.433(10) . O22 C21 1.463(12) . O23 C25 1.434(11) . O24 C29 1.453(11) . O42 C41 1.431(10) . O43 C45 1.453(11) . O44 C49 1.441(11) . O62 C61 1.443(10) . O63 C65 1.459(9) . O64 C69 1.454(12) . O81 C86 1.412(12) 3_667 O81 C81 1.425(11) . O81 K2 3.361(7) 3_667 O82 C82 1.403(11) . O82 C83B 1.45(4) . O82 C83 1.460(17) . O83 C85 1.385(11) . O83 C84B 1.45(4) . O83 C84 1.487(17) . C1 C4 1.497(12) . C1 C3 1.504(12) . C1 C2 1.524(12) . C2 H2C 0.9800 . C2 H2D 0.9800 . C2 H2E 0.9800 . C3 H3A 0.9800 . C3 H3B 0.9800 . C3 H3C 0.9800 . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . C5 C6 1.516(13) . C5 C7 1.519(12) . C5 C8 1.529(14) . C6 H6A 0.9800 . C6 H6B 0.9800 . C6 H6C 0.9800 . C7 H7A 0.9800 . C7 H7B 0.9800 . C7 H7C 0.9800 . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 C11 1.501(13) . C9 C12 1.519(13) . C9 C10 1.534(12) . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 H11C 0.9800 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . C21 C24 1.478(14) . C21 C22 1.508(13) . C21 C23 1.524(13) . C22 H1 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C24 H24A 0.9800 . C24 H24B 0.9800 . C24 H24C 0.9800 . C25 C26 1.462(15) . C25 C28 1.518(13) . C25 C27 1.529(12) . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 C31 1.38(2) . C29 C32B 1.43(3) . C29 C30 1.480(14) . C29 C32 1.61(2) . C29 C31B 1.74(4) . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C31B H31D 0.9800 . C31B H31E 0.9800 . C31B H31F 0.9800 . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . C32B H32D 0.9800 . C32B H32E 0.9800 . C32B H32F 0.9800 . C41 C42 1.487(13) . C41 C43 1.504(14) . C41 C44 1.505(12) . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 0.9800 . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . C45 C47 1.495(13) . C45 C48 1.512(14) . C45 C46 1.520(14) . C46 H46A 0.9800 . C46 H46B 0.9800 . C46 H46C 0.9800 . C47 H47A 0.9800 . C47 H47B 0.9800 . C47 H47C 0.9800 . C48 H48A 0.9800 . C48 H48B 0.9800 . C48 H48C 0.9800 . C49 C51 1.496(14) . C49 C52 1.501(13) . C49 C50 1.518(14) . C50 H50A 0.9800 . C50 H50B 0.9800 . C50 H50C 0.9800 . C51 H51A 0.9800 . C51 H51B 0.9800 . C51 H51C 0.9800 . C52 H52A 0.9800 . C52 H52B 0.9800 . C52 H52C 0.9800 . C61 C63 1.483(13) . C61 C62 1.494(13) . C61 C64 1.506(12) . C62 H62A 0.9800 . C62 H62B 0.9800 . C62 H62C 0.9800 . C63 H63A 0.9800 . C63 H63B 0.9800 . C63 H63C 0.9800 . C64 H2B 0.9800 . C64 H64A 0.9800 . C64 H64B 0.9800 . C65 C68 1.493(13) . C65 C66 1.496(12) . C65 C67 1.541(12) . C66 H66A 0.9800 . C66 H66B 0.9800 . C66 H2A 0.9800 . C67 H67A 0.9800 . C67 H67B 0.9800 . C67 H67C 0.9800 . C68 H68A 0.9800 . C68 H68B 0.9800 . C68 H68C 0.9800 . C69 C71 1.490(13) . C69 C72 1.514(13) . C69 C70 1.519(12) . C70 H70A 0.9800 . C70 H70B 0.9800 . C70 H70C 0.9800 . C71 H71A 0.9800 . C71 H71B 0.9800 . C71 H71C 0.9800 . C72 H72A 0.9800 . C72 H72B 0.9800 . C72 H72C 0.9800 . C81 C82 1.486(14) . C81 H81A 0.9900 . C81 H81B 0.9900 . C82 H82A 0.9900 . C82 H82B 0.9900 . C83 C84 1.52(3) . C83 H83A 0.9900 . C83 H83B 0.9900 . C83B C84B 1.47(6) . C83B H83C 0.9900 . C83B H83D 0.9900 . C84 H84A 0.9900 . C84 H84B 0.9900 . C84B H84C 0.9900 . C84B H84D 0.9900 . C85 C86 1.476(13) . C85 H85A 0.9900 . C85 H85B 0.9900 . C86 O81 1.413(12) 3_667 C86 H86A 0.9900 . C86 H86B 0.9900 . C91 C92 1.35(2) . C91 C96 1.38(2) . C91 C97 1.418(18) . C92 C93 1.39(2) . C92 H92 0.9500 . C93 C94 1.29(3) . C93 H93 0.9500 . C94 C95 1.36(2) . C94 H94 0.9500 . C95 C96 1.42(2) . C95 H95 0.9500 . C96 H96 0.9500 . C97 H97A 0.9800 . C97 H97B 0.9800 . C97 H97C 0.9800 .