#------------------------------------------------------------------------------ #$Date: 2016-05-11 07:50:53 +0300 (Wed, 11 May 2016) $ #$Revision: 182867 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543284.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_1543284 loop_ _publ_author_name 'Mazzanti, M.' 'Andrez, Julie' 'PECAUT, Jacques' 'Scopelliti, Rosario' 'Maron, Laurent' 'Kefalidis, Christos E.' 'Meyer, Karsten' 'Rosenzweig, Michael W.' _publ_section_title ; Synthesis and reactivity of a terminal uranium(IV) sulfide supported by siloxide ligands ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C6SC00675B _journal_year 2016 _chemical_formula_sum 'C51.5 H112 K2 O16 S Si4 U' _chemical_formula_weight 1448.05 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _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 76.530(4) _cell_angle_beta 74.270(4) _cell_angle_gamma 65.093(4) _cell_formula_units_Z 2 _cell_length_a 13.2622(7) _cell_length_b 15.3715(6) _cell_length_c 20.3762(10) _cell_measurement_reflns_used 8308 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 31.2760 _cell_measurement_theta_min 3.2490 _cell_volume 3592.7(3) _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 0.997 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_details ; 1 omega -4.00 96.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 25.8739 77.0000 -180.0000 100 2 omega -98.00 3.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -27.4364 -77.0000 -120.0000 101 3 omega -98.00 3.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -27.4364 -77.0000 -30.0000 101 4 omega -57.00 43.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -27.4364 77.0000 90.0000 100 5 omega -53.00 39.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -27.4364 37.0000 -60.0000 92 ; _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 0.0499 _diffrn_reflns_av_unetI/netI 0.0833 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 43383 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.508 _diffrn_reflns_theta_min 3.231 _exptl_absorpt_coefficient_mu 2.525 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'translucent intense green' _exptl_crystal_density_diffrn 1.339 _exptl_crystal_description block _exptl_crystal_F_000 1502 _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.700 _exptl_crystal_size_min 0.600 _refine_diff_density_max 2.712 _refine_diff_density_min -2.218 _refine_diff_density_rms 0.131 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1017 _refine_ls_number_reflns 21655 _refine_ls_number_restraints 42 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0449 _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^)+(0.0233P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.0857 _reflns_Friedel_coverage 0.000 _reflns_number_gt 17658 _reflns_number_total 21655 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6sc00675b2.cif _cod_data_source_block 1 _cod_original_cell_volume 3592.8(3) _cod_original_formula_sum 'C51.50 H112 K2 O16 S Si4 U' _cod_database_code 1543284 _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 0.237 _shelx_estimated_absorpt_t_max 0.313 _shelxl_version_number 2013-4 _shelx_res_file ; TITL CF solution in P-1 CELL 0.71073 13.262224 15.37152 20.376187 76.5301 74.2704 65.0935 ZERR 2 0.000663 0.000643 0.000995 0.0039 0.0043 0.0044 LATT 1 SFAC C H K O S Si U UNIT 103 224 4 32 2 8 2 SIMU 0.01 0.02 1.7 C86 C83 C82 C84 C81 C85 C87 L.S. 5 PLAN 50 SIZE 0.6 0.7 0.8 TEMP -123 FREE K1 C42 FREE K2 C62 FREE K2 C68 FREE K2 C31 BOND $H fmap 2 acta SHEL 999 0.7 REM C:/Users/JP154903/structure/2014/andrez/ja294/struct/ja294.hkl WGHT 0.023300 FVAR 2.65388 U1 7 0.852165 0.327885 0.198748 11.00000 0.01819 0.01541 = 0.01879 -0.00018 -0.00424 -0.00854 PART 1 K1 3 0.794954 0.111739 0.256393 11.00000 0.02789 0.02078 = 0.02693 0.00003 -0.00868 -0.01105 K2 3 0.982159 0.574674 0.069628 11.00000 0.04062 0.03743 = 0.02333 -0.00269 0.00192 -0.02406 PART 0 S1 5 0.971841 0.373013 0.086205 11.00000 0.03380 0.02817 = 0.02337 -0.00044 0.00161 -0.01729 SI4 6 0.805392 0.574018 0.223676 11.00000 0.02363 0.01801 = 0.01940 -0.00213 -0.00360 -0.01056 SI2 6 0.715631 0.234147 0.104662 11.00000 0.02111 0.02158 = 0.02092 -0.00216 -0.00543 -0.01033 SI1 6 0.641524 0.288399 0.360252 11.00000 0.02323 0.02091 = 0.02009 -0.00086 -0.00256 -0.01230 SI3 6 1.076000 0.088182 0.255783 11.00000 0.02120 0.01999 = 0.02612 -0.00079 -0.00979 -0.00632 O61 4 0.798418 0.471260 0.231384 11.00000 0.02989 0.01962 = 0.02653 -0.00419 -0.00478 -0.01206 O62 4 0.935656 0.568577 0.211670 11.00000 0.02375 0.02362 = 0.02645 0.00145 -0.00704 -0.01127 O64 4 0.724868 0.625461 0.290179 11.00000 0.03383 0.02174 = 0.02564 -0.00674 -0.00067 -0.01567 O63 4 0.773787 0.644577 0.152033 11.00000 0.02823 0.02365 = 0.02523 0.00213 -0.01117 -0.01203 O21 4 0.768091 0.268167 0.150596 11.00000 0.02750 0.03115 = 0.02572 -0.00106 -0.01037 -0.01712 O22 4 0.698405 0.135824 0.150403 11.00000 0.03079 0.02320 = 0.02454 -0.00322 -0.00875 -0.01502 O23 4 0.597077 0.314491 0.085216 11.00000 0.02410 0.02910 = 0.02231 -0.00242 -0.00619 -0.01026 O24 4 0.796642 0.200441 0.032656 11.00000 0.03030 0.02547 = 0.02153 -0.00250 -0.00395 -0.01042 O1 4 0.737919 0.292877 0.294928 11.00000 0.02550 0.02162 = 0.02384 -0.00312 -0.00059 -0.01262 O2 4 0.631672 0.184268 0.361774 11.00000 0.03198 0.02666 = 0.02386 -0.00118 -0.00136 -0.02057 O4 4 0.516783 0.371135 0.355970 11.00000 0.02334 0.02652 = 0.02841 -0.00513 -0.00659 -0.00894 O3 4 0.667798 0.292858 0.432387 11.00000 0.02387 0.02672 = 0.02135 -0.00262 -0.00534 -0.01115 O41 4 0.984305 0.192135 0.235026 11.00000 0.02318 0.02476 = 0.02521 0.00114 -0.00794 -0.00474 O42 4 1.012225 0.012426 0.266229 11.00000 0.02790 0.02155 = 0.04238 -0.00046 -0.01687 -0.01035 O43 4 1.111110 0.072588 0.329220 11.00000 0.02538 0.02569 = 0.02693 -0.00089 -0.01077 -0.01222 O44 4 1.194902 0.055889 0.201153 11.00000 0.02491 0.03269 = 0.02782 -0.00297 -0.00761 -0.00668 C61 1 1.025953 0.509031 0.248386 11.00000 0.03041 0.02648 = 0.03132 0.00493 -0.01488 -0.01313 C64 1 0.983878 0.458684 0.317050 11.00000 0.04421 0.04441 = 0.03017 0.01106 -0.01042 -0.01486 H64A 2 0.963289 0.413612 0.312428 11.00000 -1.50000 H64B 2 0.930063 0.501361 0.348789 11.00000 -1.50000 H64C 2 1.046667 0.423880 0.346218 11.00000 -1.50000 C62 1 1.113280 0.435055 0.203502 11.00000 0.02459 0.04296 = 0.04793 -0.00650 -0.00570 -0.00354 H62A 2 1.176449 0.397658 0.225888 11.00000 -1.50000 H2A 2 1.144715 0.472024 0.161217 11.00000 -1.50000 H62B 2 1.085211 0.392000 0.192350 11.00000 -1.50000 C63 1 1.076267 0.575312 0.259546 11.00000 0.07051 0.04818 = 0.08341 0.01055 -0.05104 -0.03580 H63A 2 1.033210 0.611787 0.289743 11.00000 -1.50000 H63B 2 1.093111 0.605814 0.217738 11.00000 -1.50000 H63C 2 1.139142 0.539605 0.281541 11.00000 -1.50000 C69 1 0.700224 0.714034 0.315922 11.00000 0.03975 0.02666 = 0.03318 -0.01402 -0.00199 -0.01414 C72 1 0.765606 0.772414 0.267240 11.00000 0.05409 0.03377 = 0.06085 -0.01533 0.00089 -0.02714 H72A 2 0.749701 0.828160 0.287606 11.00000 -1.50000 H72B 2 0.742260 0.790019 0.219853 11.00000 -1.50000 H72C 2 0.842095 0.741073 0.267126 11.00000 -1.50000 C71 1 0.575361 0.773483 0.321084 11.00000 0.03716 0.03587 = 0.08550 -0.03218 0.00093 -0.00796 H71A 2 0.550519 0.832588 0.341573 11.00000 -1.50000 H71B 2 0.534230 0.734167 0.348233 11.00000 -1.50000 H71C 2 0.553748 0.795217 0.273796 11.00000 -1.50000 C70 1 0.730415 0.686216 0.385446 11.00000 0.09728 0.05457 = 0.03590 -0.02019 -0.02221 -0.01551 H70A 2 0.793314 0.660462 0.386676 11.00000 -1.50000 H70B 2 0.697162 0.639687 0.409548 11.00000 -1.50000 H70C 2 0.708986 0.752261 0.413452 11.00000 -1.50000 C65 1 0.675976 0.676832 0.120753 11.00000 0.03584 0.02490 = 0.03098 -0.00047 -0.01580 -0.00966 C66 1 0.578865 0.654657 0.170476 11.00000 0.03304 0.04548 = 0.04800 -0.00300 -0.01547 -0.01693 H66A 2 0.599224 0.593920 0.188646 11.00000 -1.50000 H66B 2 0.509723 0.682223 0.148178 11.00000 -1.50000 H66C 2 0.547078 0.687180 0.209734 11.00000 -1.50000 C67 1 0.641528 0.785437 0.100247 11.00000 0.04812 0.03230 = 0.04913 0.00385 -0.02357 -0.00740 H67A 2 0.584551 0.813466 0.076432 11.00000 -1.50000 H67B 2 0.704728 0.797232 0.072786 11.00000 -1.50000 H67C 2 0.612121 0.816804 0.142664 11.00000 -1.50000 C68 1 0.711715 0.627152 0.057935 11.00000 0.05136 0.04050 = 0.04059 -0.00645 -0.02457 -0.01235 H68A 2 0.739381 0.561179 0.068083 11.00000 -1.50000 H2B 2 0.765119 0.643785 0.022078 11.00000 -1.50000 H68B 2 0.646571 0.651540 0.037156 11.00000 -1.50000 C21 1 0.669458 0.065227 0.130833 11.00000 0.03833 0.02767 = 0.03247 -0.00797 -0.00695 -0.01949 C24 1 0.599588 0.109028 0.075508 11.00000 0.06098 0.05097 = 0.04426 -0.00558 -0.02046 -0.03726 H24A 2 0.581025 0.062427 0.060614 11.00000 -1.50000 H24B 2 0.638375 0.129274 0.033239 11.00000 -1.50000 H24C 2 0.531807 0.163050 0.088117 11.00000 -1.50000 C23 1 0.600875 0.030024 0.196173 11.00000 0.06201 0.03903 = 0.04320 -0.00413 -0.00182 -0.03771 H23A 2 0.526215 0.084662 0.211908 11.00000 -1.50000 H23B 2 0.640604 0.003579 0.234729 11.00000 -1.50000 H23C 2 0.579046 -0.019369 0.187867 11.00000 -1.50000 C22 1 0.779392 -0.015759 0.107732 11.00000 0.05318 0.03793 = 0.05612 -0.01750 -0.00093 -0.02022 H22A 2 0.825514 -0.043761 0.145802 11.00000 -1.50000 H22B 2 0.824142 0.007335 0.069635 11.00000 -1.50000 H22C 2 0.769547 -0.065160 0.092756 11.00000 -1.50000 C25 1 0.498904 0.377064 0.126357 11.00000 0.02699 0.03016 = 0.02831 -0.00224 -0.00335 -0.00877 C27 1 0.403390 0.402618 0.089306 11.00000 0.02883 0.08385 = 0.04274 -0.00157 -0.01418 0.00079 H27A 2 0.420158 0.425314 0.049918 11.00000 -1.50000 H27B 2 0.335855 0.454477 0.112608 11.00000 -1.50000 H27C 2 0.384436 0.347737 0.083170 11.00000 -1.50000 C26 1 0.472348 0.327021 0.198410 11.00000 0.03424 0.03931 = 0.02873 -0.00429 0.00013 -0.00848 H26A 2 0.458089 0.279336 0.197559 11.00000 -1.50000 H26B 2 0.407789 0.369122 0.225830 11.00000 -1.50000 H26C 2 0.526512 0.309641 0.219161 11.00000 -1.50000 PART 2 C28 1 0.519275 0.465565 0.129486 11.00000 0.06118 0.03639 = 0.07592 -0.02036 0.01616 -0.01670 AFIX 137 H28A 2 0.581351 0.446351 0.153867 11.00000 -1.50000 H28B 2 0.450216 0.511683 0.153969 11.00000 -1.50000 H28C 2 0.539459 0.496011 0.082649 11.00000 -1.50000 AFIX 66 PART 0 PART -1 C81 1 -0.020141 0.551061 0.495857 10.50000 0.07647 0.11227 = 0.07091 -0.01695 -0.03694 -0.05175 C82 1 -0.089199 0.502405 0.534656 10.50000 0.06553 0.12252 = 0.06278 -0.01328 -0.01490 -0.06293 AFIX 43 H82 2 -0.163886 0.537708 0.557137 10.50000 -1.20000 AFIX 65 C83 1 -0.048978 0.402096 0.540561 10.50000 0.08438 0.12287 = 0.06528 -0.02049 -0.01593 -0.06206 AFIX 43 H83 2 -0.096177 0.368843 0.567078 10.50000 -1.20000 AFIX 65 C84 1 0.060300 0.350443 0.507667 10.50000 0.09350 0.12704 = 0.07905 -0.01857 -0.03705 -0.04587 AFIX 43 H84 2 0.087789 0.281886 0.511704 10.50000 -1.20000 AFIX 65 C85 1 0.129359 0.399097 0.468868 10.50000 0.06791 0.13208 = 0.06845 -0.01488 -0.02600 -0.04427 AFIX 43 H85 2 0.204046 0.363794 0.446387 10.50000 -1.20000 AFIX 65 C86 1 0.089140 0.499406 0.462963 10.50000 0.06070 0.12743 = 0.06772 -0.01277 -0.02354 -0.05113 AFIX 43 H86 2 0.136338 0.532660 0.436445 10.50000 -1.20000 AFIX 0 C87 1 -0.062239 0.654791 0.492714 10.50000 0.13660 0.08377 = 0.12577 -0.01118 -0.09287 -0.04123 AFIX 137 H87A 2 -0.066166 0.685166 0.445029 10.50000 -1.50000 H87B 2 -0.011071 0.671887 0.509331 10.50000 -1.50000 H87C 2 -0.138084 0.677803 0.521647 10.50000 -1.50000 AFIX 0 PART 0 C5 1 0.771470 0.248884 0.458585 11.00000 0.03072 0.03483 = 0.03068 -0.00002 -0.01402 -0.01465 C6 1 0.735031 0.245482 0.536092 11.00000 0.05429 0.05024 = 0.02909 -0.00183 -0.02071 -0.01597 H6A 2 0.687084 0.310213 0.549144 11.00000 -1.50000 H6B 2 0.796595 0.223726 0.558516 11.00000 -1.50000 H6C 2 0.695720 0.207216 0.551429 11.00000 -1.50000 C42 1 0.985154 -0.128895 0.264159 11.00000 0.07962 0.03383 = 0.11691 -0.00513 -0.05854 -0.02399 C30 1 0.759632 0.245170 -0.080869 11.00000 0.11719 0.09641 = 0.03311 0.00711 -0.02659 -0.07337 C51 1 1.253063 0.164610 0.109666 11.00000 0.04773 0.05905 = 0.04154 0.00750 0.00049 -0.01638 H51A 2 1.182868 0.218993 0.117073 11.00000 -1.50000 H51B 2 1.281525 0.174281 0.064108 11.00000 -1.50000 H51C 2 1.311191 0.160113 0.139861 11.00000 -1.50000 C29 1 0.824036 0.252457 -0.033433 11.00000 0.03563 0.03607 = 0.02283 -0.00298 -0.00437 -0.01519 PART 2 C31 1 0.793821 0.357079 -0.028355 11.00000 0.04709 0.03663 = 0.03228 0.00395 -0.00137 -0.02027 H31A 2 0.715436 0.389366 -0.016481 11.00000 -1.50000 H31B 2 0.816368 0.392684 -0.073688 11.00000 -1.50000 H31C 2 0.824979 0.363174 0.007500 11.00000 -1.50000 PART 0 C32 1 0.951065 0.203592 -0.056160 11.00000 0.04249 0.06186 = 0.06210 0.00259 0.01867 -0.00029 H32A 2 0.970392 0.227617 -0.103036 11.00000 -1.50000 H32B 2 0.964312 0.141410 -0.059459 11.00000 -1.50000 H32C 2 0.986398 0.204817 -0.024583 11.00000 -1.50000 C1 1 0.549646 0.145447 0.405456 11.00000 0.04575 0.03742 = 0.03133 0.00144 -0.00111 -0.03232 C2 1 0.606303 0.036908 0.402640 11.00000 0.07748 0.03961 = 0.05541 -0.01027 0.01550 -0.03979 H2C 2 0.629633 0.017012 0.353469 11.00000 -1.50000 H2D 2 0.557807 0.004555 0.424930 11.00000 -1.50000 H2E 2 0.680823 0.006332 0.408382 11.00000 -1.50000 C4 1 0.443691 0.188665 0.374549 11.00000 0.05321 0.07297 = 0.06430 0.00596 -0.01337 -0.04919 H4A 2 0.412956 0.245841 0.373604 11.00000 -1.50000 H4B 2 0.388924 0.160542 0.403870 11.00000 -1.50000 H4C 2 0.468437 0.173425 0.325941 11.00000 -1.50000 C3 1 0.523695 0.164381 0.478353 11.00000 0.05502 0.05056 = 0.03710 -0.00526 0.00890 -0.03744 H3A 2 0.595146 0.133737 0.495905 11.00000 -1.50000 H3B 2 0.460363 0.142144 0.507492 11.00000 -1.50000 H3C 2 0.491868 0.227290 0.481714 11.00000 -1.50000 C9 1 0.462050 0.466070 0.376604 11.00000 0.02765 0.02936 = 0.02311 -0.00166 -0.00410 -0.00724 C11 1 0.370857 0.521732 0.333890 11.00000 0.03841 0.04344 = 0.04318 -0.00197 -0.01577 -0.00021 H11A 2 0.403290 0.533798 0.284153 11.00000 -1.50000 H11B 2 0.327288 0.583003 0.348430 11.00000 -1.50000 H11C 2 0.315558 0.487828 0.341284 11.00000 -1.50000 C10 1 0.410046 0.455805 0.452867 11.00000 0.03848 0.03867 = 0.03063 -0.01009 0.00089 -0.01058 H10A 2 0.362087 0.427557 0.460365 11.00000 -1.50000 H10B 2 0.376491 0.509973 0.466641 11.00000 -1.50000 H10C 2 0.467241 0.416313 0.483816 11.00000 -1.50000 C12 1 0.545582 0.514860 0.362532 11.00000 0.04158 0.02730 = 0.05113 -0.00299 -0.00245 -0.01748 H12A 2 0.597102 0.484140 0.391281 11.00000 -1.50000 H12B 2 0.506011 0.577170 0.372169 11.00000 -1.50000 H12C 2 0.582030 0.516889 0.314311 11.00000 -1.50000 C7 1 0.840084 0.149027 0.437949 11.00000 0.03383 0.03661 = 0.04661 -0.00367 -0.01308 -0.00877 H7A 2 0.797983 0.114660 0.449966 11.00000 -1.50000 H7B 2 0.902379 0.121956 0.460910 11.00000 -1.50000 H7C 2 0.868611 0.152320 0.388248 11.00000 -1.50000 C8 1 0.837028 0.314516 0.429293 11.00000 0.03837 0.05449 = 0.05405 -0.00829 -0.01186 -0.02610 H8A 2 0.901227 0.294044 0.446959 11.00000 -1.50000 H8B 2 0.791007 0.374488 0.442022 11.00000 -1.50000 H8C 2 0.856725 0.315159 0.379836 11.00000 -1.50000 C41 1 1.044485 -0.088248 0.296497 11.00000 0.04230 0.02076 = 0.05930 0.00353 -0.02498 -0.01375 C44 1 1.171432 -0.142539 0.279127 11.00000 0.04217 0.02382 = 0.07054 -0.00694 -0.01591 -0.00387 H44A 2 1.201416 -0.140567 0.229373 11.00000 -1.50000 H44B 2 1.189850 -0.208559 0.298789 11.00000 -1.50000 H44C 2 1.211260 -0.121932 0.296126 11.00000 -1.50000 C43 1 1.001786 -0.091908 0.373052 11.00000 0.05044 0.03034 = 0.06252 0.01072 -0.01065 -0.01525 H43A 2 1.023528 -0.159959 0.393779 11.00000 -1.50000 H43B 2 0.927795 -0.063076 0.383259 11.00000 -1.50000 H43C 2 1.030608 -0.066154 0.393156 11.00000 -1.50000 C45 1 1.194967 0.094683 0.347313 11.00000 0.02511 0.02439 = 0.03484 -0.00276 -0.01292 -0.01090 C47 1 1.311291 0.015844 0.327468 11.00000 0.02699 0.04065 = 0.06077 -0.00841 -0.02116 -0.00700 H47A 2 1.313217 -0.047240 0.353635 11.00000 -1.50000 H47B 2 1.367463 0.021405 0.342277 11.00000 -1.50000 H47C 2 1.330716 0.012374 0.276728 11.00000 -1.50000 C46 1 1.162869 0.094122 0.423916 11.00000 0.04086 0.06145 = 0.04055 -0.00431 -0.02013 -0.02205 H46A 2 1.156062 0.035431 0.446962 11.00000 -1.50000 H46B 2 1.088538 0.144806 0.436646 11.00000 -1.50000 H46C 2 1.220305 0.099794 0.435979 11.00000 -1.50000 C48 1 1.191500 0.193127 0.310631 11.00000 0.05275 0.03153 = 0.05740 0.00735 -0.03103 -0.02303 H48A 2 1.235685 0.213673 0.323916 11.00000 -1.50000 H48B 2 1.114200 0.244164 0.322134 11.00000 -1.50000 H48C 2 1.209478 0.195574 0.264389 11.00000 -1.50000 C49 1 1.230137 0.071528 0.127954 11.00000 0.03263 0.05242 = 0.02663 -0.00901 -0.00569 -0.00555 C50 1 1.338717 -0.014902 0.110645 11.00000 0.04175 0.06570 = 0.05441 -0.02815 -0.00110 0.00746 H50A 2 1.388985 -0.018408 0.138996 11.00000 -1.50000 H50B 2 1.371733 -0.017209 0.063477 11.00000 -1.50000 H50C 2 1.329140 -0.070666 0.121283 11.00000 -1.50000 C52 1 1.140294 0.079883 0.091795 11.00000 0.04849 0.07677 = 0.04021 -0.02277 -0.01787 -0.00174 H52A 2 1.120707 0.019888 0.102840 11.00000 -1.50000 H52B 2 1.168063 0.084076 0.041383 11.00000 -1.50000 H52C 2 1.069834 0.133093 0.102878 11.00000 -1.50000 H1 2 0.885897 -0.091018 0.290038 11.00000 -1.50000 H42A 2 1.002238 -0.192470 0.286196 11.00000 -1.50000 H42B 2 1.001040 -0.123671 0.217832 11.00000 -1.50000 H30A 2 0.791303 0.179025 -0.087021 11.00000 -1.50000 H30B 2 0.778704 0.274961 -0.127311 11.00000 -1.50000 H30C 2 0.685946 0.267503 -0.062781 11.00000 -1.50000 HKLF 4 REM CF solution in P-1 REM R1 = 0.0449 for 17658 Fo > 4sig(Fo) and 0.0637 for all 21655 data REM 1017 parameters refined using 42 restraints END WGHT 0.0234 0.0000 REM Highest difference peak 2.712, deepest hole -2.218, 1-sigma level 0.131 Q1 1 0.8759 0.3052 0.1583 11.00000 0.05 2.71 Q2 1 0.8304 0.3397 0.2387 11.00000 0.05 2.67 Q3 1 0.8368 0.2999 0.2093 11.00000 0.05 1.31 Q4 1 0.4428 0.0123 0.4066 11.00000 0.05 1.19 Q5 1 0.9199 0.3082 0.2132 11.00000 0.05 0.84 Q6 1 0.9203 0.2791 0.1969 11.00000 0.05 0.83 Q7 1 0.9059 0.5475 0.1422 11.00000 0.05 0.77 Q8 1 0.9022 0.3218 0.1117 11.00000 0.05 0.72 Q9 1 0.8145 0.3283 0.2810 11.00000 0.05 0.69 Q10 1 0.8419 0.0784 0.2185 11.00000 0.05 0.66 Q11 1 0.7424 0.2027 0.0698 11.00000 0.05 0.65 Q12 1 0.7741 0.2312 0.0597 11.00000 0.05 0.64 Q13 1 0.9030 0.0861 0.1748 11.00000 0.05 0.63 Q14 1 0.6427 0.3034 0.4022 11.00000 0.05 0.62 Q15 1 0.7561 0.3753 0.2702 11.00000 0.05 0.61 Q16 1 0.6983 0.3137 0.2181 11.00000 0.05 0.60 Q17 1 0.7409 0.6285 0.2418 11.00000 0.05 0.59 Q18 1 0.7879 0.5985 0.2615 11.00000 0.05 0.59 Q19 1 0.9179 0.2971 0.1184 11.00000 0.05 0.59 Q20 1 0.8588 0.3626 0.1202 11.00000 0.05 0.57 Q21 1 -0.0003 0.3675 0.5354 11.00000 0.05 0.57 Q22 1 0.9561 0.6159 0.0983 11.00000 0.05 0.55 Q23 1 0.7515 0.2568 0.4971 11.00000 0.05 0.55 Q24 1 0.8188 0.3912 0.2694 11.00000 0.05 0.55 Q25 1 1.0050 0.3510 0.0497 11.00000 0.05 0.55 Q26 1 0.6866 0.2785 0.3930 11.00000 0.05 0.54 Q27 1 0.9440 0.2723 0.1265 11.00000 0.05 0.53 Q28 1 0.9200 0.3444 0.0977 11.00000 0.05 0.53 Q29 1 1.4422 0.0167 0.3223 11.00000 0.05 0.53 Q30 1 1.0655 0.1026 0.2996 11.00000 0.05 0.52 Q31 1 0.5024 0.4541 0.0537 11.00000 0.05 0.51 Q32 1 0.6363 0.0226 0.3683 11.00000 0.05 0.51 Q33 1 0.9825 0.3697 0.0435 11.00000 0.05 0.51 Q34 1 0.8542 0.2765 0.2626 11.00000 0.05 0.50 Q35 1 0.7436 0.4452 0.2701 11.00000 0.05 0.50 Q36 1 0.6595 0.2704 0.0907 11.00000 0.05 0.50 Q37 1 1.0219 0.5347 0.0393 11.00000 0.05 0.50 Q38 1 0.9929 0.4179 0.2910 11.00000 0.05 0.50 Q39 1 0.9549 0.3835 0.1297 11.00000 0.05 0.49 Q40 1 0.9968 0.5655 0.0263 11.00000 0.05 0.49 Q41 1 0.9430 0.0273 0.2903 11.00000 0.05 0.49 Q42 1 0.7562 0.4837 0.1961 11.00000 0.05 0.48 Q43 1 1.1371 0.0574 0.2887 11.00000 0.05 0.48 Q44 1 0.8830 0.2649 0.1317 11.00000 0.05 0.48 Q45 1 0.6351 0.1284 0.2766 11.00000 0.05 0.48 Q46 1 0.4078 0.0161 0.4542 11.00000 0.05 0.48 Q47 1 0.7831 0.2410 0.1128 11.00000 0.05 0.48 Q48 1 0.4241 0.0630 0.4348 11.00000 0.05 0.48 Q49 1 0.9368 0.1912 0.3214 11.00000 0.05 0.47 Q50 1 0.5802 0.0230 0.0914 11.00000 0.05 0.47 ; _shelx_res_checksum 85169 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.85217(2) 0.32789(2) 0.19875(2) 0.01698(4) Uani 1 1 d . . . . . K1 K 0.79495(6) 0.11174(5) 0.25639(4) 0.02448(16) Uani 1 1 d . . . A 1 K2 K 0.98216(7) 0.57467(6) 0.06963(4) 0.03260(19) Uani 1 1 d . . . B 1 S1 S 0.97184(8) 0.37301(7) 0.08620(5) 0.0286(2) Uani 1 1 d . . . . . Si4 Si 0.80539(8) 0.57402(6) 0.22368(5) 0.01964(19) Uani 1 1 d . . . . . Si2 Si 0.71563(8) 0.23415(7) 0.10466(5) 0.02030(19) Uani 1 1 d . . . . . Si1 Si 0.64152(8) 0.28840(7) 0.36025(5) 0.02076(19) Uani 1 1 d . . . . . Si3 Si 1.07600(8) 0.08818(7) 0.25578(5) 0.0223(2) Uani 1 1 d . . . . . O61 O 0.79842(19) 0.47126(16) 0.23138(13) 0.0244(5) Uani 1 1 d . . . . . O62 O 0.93566(19) 0.56858(16) 0.21167(13) 0.0243(5) Uani 1 1 d . . . . . O64 O 0.7249(2) 0.62546(16) 0.29018(13) 0.0258(5) Uani 1 1 d . . . . . O63 O 0.77379(19) 0.64458(16) 0.15203(13) 0.0247(5) Uani 1 1 d . . . . . O21 O 0.76809(19) 0.26817(17) 0.15060(13) 0.0255(5) Uani 1 1 d . . . . . O22 O 0.69840(19) 0.13582(16) 0.15040(12) 0.0238(5) Uani 1 1 d . . . . . O23 O 0.59708(19) 0.31449(17) 0.08522(12) 0.0250(5) Uani 1 1 d . . . . . O24 O 0.79664(19) 0.20044(17) 0.03266(12) 0.0262(5) Uani 1 1 d . . . . . O1 O 0.73792(18) 0.29288(16) 0.29493(12) 0.0233(5) Uani 1 1 d . . . . . O2 O 0.6317(2) 0.18427(17) 0.36177(12) 0.0255(5) Uani 1 1 d . . . . . O4 O 0.51678(19) 0.37113(17) 0.35597(13) 0.0257(5) Uani 1 1 d . . . . . O3 O 0.66780(19) 0.29286(17) 0.43239(12) 0.0234(5) Uani 1 1 d . . . . . O41 O 0.98430(19) 0.19214(17) 0.23503(13) 0.0261(5) Uani 1 1 d . . . . . O42 O 1.0122(2) 0.01243(17) 0.26623(14) 0.0289(6) Uani 1 1 d . . . . . O43 O 1.11111(19) 0.07259(17) 0.32922(13) 0.0244(5) Uani 1 1 d . . . . . O44 O 1.19490(19) 0.05589(18) 0.20115(13) 0.0297(6) Uani 1 1 d . . . . . C61 C 1.0260(3) 0.5090(3) 0.2484(2) 0.0283(8) Uani 1 1 d . . . . . C64 C 0.9839(4) 0.4587(4) 0.3170(2) 0.0426(11) Uani 1 1 d . . . . . H64A H 0.963(4) 0.414(4) 0.312(3) 0.064 Uiso 1 1 d . U . . . H64B H 0.930(4) 0.501(4) 0.349(3) 0.064 Uiso 1 1 d . U . . . H64C H 1.047(4) 0.424(4) 0.346(3) 0.064 Uiso 1 1 d . U . . . C62 C 1.1133(3) 0.4351(3) 0.2035(3) 0.0420(11) Uani 1 1 d . . . . . H62A H 1.176(4) 0.398(4) 0.226(3) 0.063 Uiso 1 1 d . U . . . H2A H 1.145(4) 0.472(3) 0.161(3) 0.063 Uiso 1 1 d . U . . . H62B H 1.085(4) 0.392(3) 0.192(3) 0.063 Uiso 1 1 d . U . . . C63 C 1.0763(5) 0.5753(4) 0.2595(4) 0.0586(17) Uani 1 1 d . . . . . H63A H 1.033(5) 0.612(5) 0.290(3) 0.088 Uiso 1 1 d . U . . . H63B H 1.093(5) 0.606(4) 0.218(3) 0.088 Uiso 1 1 d . U . . . H63C H 1.139(5) 0.540(4) 0.282(3) 0.088 Uiso 1 1 d . U . . . C69 C 0.7002(3) 0.7140(3) 0.3159(2) 0.0320(9) Uani 1 1 d . . . . . C72 C 0.7656(4) 0.7724(3) 0.2672(3) 0.0469(12) Uani 1 1 d . . . . . H72A H 0.750(4) 0.828(4) 0.288(3) 0.070 Uiso 1 1 d . U . . . H72B H 0.742(4) 0.790(4) 0.220(3) 0.070 Uiso 1 1 d . U . . . H72C H 0.842(4) 0.741(4) 0.267(3) 0.070 Uiso 1 1 d . U . . . C71 C 0.5754(4) 0.7735(4) 0.3211(3) 0.0534(14) Uani 1 1 d . . . . . H71A H 0.551(4) 0.833(4) 0.342(3) 0.080 Uiso 1 1 d . U . . . H71B H 0.534(4) 0.734(4) 0.348(3) 0.080 Uiso 1 1 d . U . . . H71C H 0.554(4) 0.795(4) 0.274(3) 0.080 Uiso 1 1 d . U . . . C70 C 0.7304(5) 0.6862(5) 0.3854(3) 0.0628(16) Uani 1 1 d . . . . . H70A H 0.793(5) 0.660(5) 0.387(4) 0.094 Uiso 1 1 d . U . . . H70B H 0.697(5) 0.640(4) 0.410(3) 0.094 Uiso 1 1 d . U . . . H70C H 0.709(5) 0.752(4) 0.413(3) 0.094 Uiso 1 1 d . U . . . C65 C 0.6760(3) 0.6768(3) 0.1208(2) 0.0299(8) Uani 1 1 d . . . . . C66 C 0.5789(4) 0.6547(4) 0.1705(3) 0.0405(11) Uani 1 1 d . . . . . H66A H 0.599(4) 0.594(4) 0.189(3) 0.061 Uiso 1 1 d . U . . . H66B H 0.510(4) 0.682(3) 0.148(3) 0.061 Uiso 1 1 d . U . . . H66C H 0.547(4) 0.687(4) 0.210(3) 0.061 Uiso 1 1 d . U . . . C67 C 0.6415(4) 0.7854(3) 0.1002(3) 0.0447(11) Uani 1 1 d . . . . . H67A H 0.585(4) 0.813(4) 0.076(3) 0.067 Uiso 1 1 d . U . . . H67B H 0.705(4) 0.797(4) 0.073(3) 0.067 Uiso 1 1 d . U . . . H67C H 0.612(4) 0.817(4) 0.143(3) 0.067 Uiso 1 1 d . U . . . C68 C 0.7117(4) 0.6272(4) 0.0579(3) 0.0425(11) Uani 1 1 d . . . . . H68A H 0.739(4) 0.561(4) 0.068(3) 0.064 Uiso 1 1 d . U . . . H2B H 0.765(4) 0.644(3) 0.022(3) 0.064 Uiso 1 1 d . U . . . H68B H 0.647(4) 0.652(3) 0.037(3) 0.064 Uiso 1 1 d . U . . . C21 C 0.6695(3) 0.0652(3) 0.1308(2) 0.0297(8) Uani 1 1 d . . . . . C24 C 0.5996(4) 0.1090(4) 0.0755(3) 0.0445(12) Uani 1 1 d . . . . . H24A H 0.581(4) 0.062(4) 0.061(3) 0.067 Uiso 1 1 d . U . . . H24B H 0.638(4) 0.129(4) 0.033(3) 0.067 Uiso 1 1 d . U . . . H24C H 0.532(4) 0.163(4) 0.088(3) 0.067 Uiso 1 1 d . U . . . C23 C 0.6009(4) 0.0300(3) 0.1962(3) 0.0437(11) Uani 1 1 d . . . . . H23A H 0.526(4) 0.085(4) 0.212(3) 0.066 Uiso 1 1 d . U . . . H23B H 0.641(4) 0.004(4) 0.235(3) 0.066 Uiso 1 1 d . U . . . H23C H 0.579(4) -0.019(4) 0.188(3) 0.066 Uiso 1 1 d . U . . . C22 C 0.7794(4) -0.0158(4) 0.1077(3) 0.0482(12) Uani 1 1 d . . . . . H22A H 0.826(4) -0.044(4) 0.146(3) 0.072 Uiso 1 1 d . U . . . H22B H 0.824(4) 0.007(4) 0.070(3) 0.072 Uiso 1 1 d . U . . . H22C H 0.770(4) -0.065(4) 0.093(3) 0.072 Uiso 1 1 d . U . . . C25 C 0.4989(3) 0.3771(3) 0.1264(2) 0.0300(8) Uani 1 1 d . . . . . C27 C 0.4034(4) 0.4026(5) 0.0893(3) 0.0594(16) Uani 1 1 d . . . . . H27A H 0.420(5) 0.425(4) 0.050(3) 0.089 Uiso 1 1 d . U . . . H27B H 0.336(5) 0.454(4) 0.113(3) 0.089 Uiso 1 1 d . U . . . H27C H 0.384(5) 0.348(4) 0.083(3) 0.089 Uiso 1 1 d . U . . . C26 C 0.4723(4) 0.3270(3) 0.1984(2) 0.0375(10) Uani 1 1 d . . . . . H26A H 0.458(4) 0.279(4) 0.198(3) 0.056 Uiso 1 1 d . U . . . H26B H 0.408(4) 0.369(3) 0.226(3) 0.056 Uiso 1 1 d . U . . . H26C H 0.527(4) 0.310(3) 0.219(3) 0.056 Uiso 1 1 d . U . . . C28 C 0.5193(4) 0.4656(3) 0.1295(3) 0.0625(16) Uani 1 1 d . . . C 2 H28A H 0.5814 0.4464 0.1539 0.094 Uiso 1 1 calc R U . C 2 H28B H 0.4502 0.5117 0.1540 0.094 Uiso 1 1 calc R U . C 2 H28C H 0.5395 0.4960 0.0826 0.094 Uiso 1 1 calc R U . C 2 C81 C -0.0201(8) 0.5511(6) 0.4959(6) 0.075(3) Uani 0.5 1 d G U P D -1 C82 C -0.0892(6) 0.5024(7) 0.5347(5) 0.074(4) Uani 0.5 1 d G U P D -1 H82 H -0.1639 0.5377 0.5571 0.088 Uiso 0.5 1 calc R U P D -1 C83 C -0.0490(8) 0.4021(7) 0.5406(5) 0.081(3) Uani 0.5 1 d G U P D -1 H83 H -0.0962 0.3688 0.5671 0.098 Uiso 0.5 1 calc R U P D -1 C84 C 0.0603(8) 0.3504(6) 0.5077(6) 0.093(6) Uani 0.5 1 d G U P D -1 H84 H 0.0878 0.2819 0.5117 0.112 Uiso 0.5 1 calc R U P D -1 C85 C 0.1294(6) 0.3991(7) 0.4689(5) 0.084(3) Uani 0.5 1 d G U P D -1 H85 H 0.2040 0.3638 0.4464 0.101 Uiso 0.5 1 calc R U P D -1 C86 C 0.0891(7) 0.4994(7) 0.4630(5) 0.078(5) Uani 0.5 1 d G U P D -1 H86 H 0.1363 0.5327 0.4364 0.093 Uiso 0.5 1 calc R U P D -1 C87 C -0.0622(14) 0.6548(11) 0.4927(10) 0.102(6) Uani 0.5 1 d . U P D -1 H87A H -0.0662 0.6852 0.4450 0.153 Uiso 0.5 1 calc R U P D -1 H87B H -0.0111 0.6719 0.5093 0.153 Uiso 0.5 1 calc R U P D -1 H87C H -0.1381 0.6778 0.5216 0.153 Uiso 0.5 1 calc R U P D -1 C5 C 0.7715(3) 0.2489(3) 0.4586(2) 0.0304(8) Uani 1 1 d . . . . . C6 C 0.7350(4) 0.2455(4) 0.5361(2) 0.0439(11) Uani 1 1 d . . . . . H6A H 0.687(4) 0.310(4) 0.549(3) 0.066 Uiso 1 1 d . U . . . H6B H 0.797(4) 0.224(4) 0.559(3) 0.066 Uiso 1 1 d . U . . . H6C H 0.696(4) 0.207(4) 0.551(3) 0.066 Uiso 1 1 d . U . . . C42 C 0.9852(6) -0.1289(4) 0.2642(4) 0.069(2) Uani 1 1 d . . . . . C30 C 0.7596(7) 0.2452(5) -0.0809(3) 0.071(2) Uani 1 1 d . . . . . C51 C 1.2531(4) 0.1646(4) 0.1097(3) 0.0554(14) Uani 1 1 d . . . . . H51A H 1.183(5) 0.219(4) 0.117(3) 0.083 Uiso 1 1 d . U . . . H51B H 1.282(4) 0.174(4) 0.064(3) 0.083 Uiso 1 1 d . U . . . H51C H 1.311(5) 0.160(4) 0.140(3) 0.083 Uiso 1 1 d . U . . . C29 C 0.8240(3) 0.2525(3) -0.0334(2) 0.0315(8) Uani 1 1 d . . . . . C31 C 0.7938(4) 0.3571(3) -0.0284(2) 0.0401(11) Uani 1 1 d . . . E 2 H31A H 0.715(4) 0.389(3) -0.016(3) 0.060 Uiso 1 1 d . U . F 2 H31B H 0.816(4) 0.393(3) -0.074(3) 0.060 Uiso 1 1 d . U . G 2 H31C H 0.825(4) 0.363(3) 0.008(3) 0.060 Uiso 1 1 d . U . H 2 C32 C 0.9511(5) 0.2036(5) -0.0562(3) 0.071(2) Uani 1 1 d . . . . . H32A H 0.970(5) 0.228(5) -0.103(4) 0.106 Uiso 1 1 d . U . . . H32B H 0.964(5) 0.141(5) -0.059(4) 0.106 Uiso 1 1 d . U . . . H32C H 0.986(5) 0.205(5) -0.025(4) 0.106 Uiso 1 1 d . U . . . C1 C 0.5496(3) 0.1454(3) 0.4055(2) 0.0349(9) Uani 1 1 d . . . . . C2 C 0.6063(5) 0.0369(4) 0.4026(3) 0.0568(15) Uani 1 1 d . . . . . H2C H 0.630(5) 0.017(4) 0.353(3) 0.085 Uiso 1 1 d . U . . . H2D H 0.558(5) 0.005(4) 0.425(3) 0.085 Uiso 1 1 d . U . . . H2E H 0.681(5) 0.006(4) 0.408(3) 0.085 Uiso 1 1 d . U . . . C4 C 0.4437(5) 0.1887(4) 0.3745(3) 0.0571(16) Uani 1 1 d . . . . . H4A H 0.413(5) 0.246(4) 0.374(3) 0.086 Uiso 1 1 d . U . . . H4B H 0.389(4) 0.161(4) 0.404(3) 0.086 Uiso 1 1 d . U . . . H4C H 0.468(5) 0.173(4) 0.326(3) 0.086 Uiso 1 1 d . U . . . C3 C 0.5237(4) 0.1644(4) 0.4784(2) 0.0454(12) Uani 1 1 d . . . . . H3A H 0.595(4) 0.134(4) 0.496(3) 0.068 Uiso 1 1 d . U . . . H3B H 0.460(4) 0.142(3) 0.507(3) 0.068 Uiso 1 1 d . U . . . H3C H 0.492(4) 0.227(4) 0.482(3) 0.068 Uiso 1 1 d . U . . . C9 C 0.4620(3) 0.4661(3) 0.37660(19) 0.0285(8) Uani 1 1 d . . . . . C11 C 0.3709(4) 0.5217(4) 0.3339(3) 0.0462(11) Uani 1 1 d . . . . . H11A H 0.403(4) 0.534(4) 0.284(3) 0.069 Uiso 1 1 d . U . . . H11B H 0.327(4) 0.583(4) 0.348(3) 0.069 Uiso 1 1 d . U . . . H11C H 0.316(4) 0.488(4) 0.341(3) 0.069 Uiso 1 1 d . U . . . C10 C 0.4100(4) 0.4558(3) 0.4529(2) 0.0381(10) Uani 1 1 d . . . . . H10A H 0.362(4) 0.428(3) 0.460(2) 0.057 Uiso 1 1 d . U . . . H10B H 0.376(4) 0.510(4) 0.467(3) 0.057 Uiso 1 1 d . U . . . H10C H 0.467(4) 0.416(3) 0.484(3) 0.057 Uiso 1 1 d . U . . . C12 C 0.5456(4) 0.5149(3) 0.3625(3) 0.0403(11) Uani 1 1 d . . . . . H12A H 0.597(4) 0.484(4) 0.391(3) 0.060 Uiso 1 1 d . U . . . H12B H 0.506(4) 0.577(4) 0.372(3) 0.060 Uiso 1 1 d . U . . . H12C H 0.582(4) 0.517(3) 0.314(3) 0.060 Uiso 1 1 d . U . . . C7 C 0.8401(4) 0.1490(3) 0.4379(3) 0.0399(10) Uani 1 1 d . . . . . H7A H 0.798(4) 0.115(3) 0.450(3) 0.060 Uiso 1 1 d . U . . . H7B H 0.902(4) 0.122(3) 0.461(3) 0.060 Uiso 1 1 d . U . . . H7C H 0.869(4) 0.152(3) 0.388(3) 0.060 Uiso 1 1 d . U . . . C8 C 0.8370(4) 0.3145(4) 0.4293(3) 0.0453(12) Uani 1 1 d . . . . . H8A H 0.901(4) 0.294(4) 0.447(3) 0.068 Uiso 1 1 d . U . . . H8B H 0.791(4) 0.374(4) 0.442(3) 0.068 Uiso 1 1 d . U . . . H8C H 0.857(4) 0.315(4) 0.380(3) 0.068 Uiso 1 1 d . U . . . C41 C 1.0445(3) -0.0882(3) 0.2965(2) 0.0386(10) Uani 1 1 d . . . . . C44 C 1.1714(4) -0.1425(3) 0.2791(3) 0.0475(12) Uani 1 1 d . . . . . H44A H 1.201(4) -0.141(4) 0.229(3) 0.071 Uiso 1 1 d . U . . . H44B H 1.190(4) -0.209(4) 0.299(3) 0.071 Uiso 1 1 d . U . . . H44C H 1.211(4) -0.122(4) 0.296(3) 0.071 Uiso 1 1 d . U . . . C43 C 1.0018(4) -0.0919(4) 0.3731(3) 0.0510(14) Uani 1 1 d . . . . . H43A H 1.024(4) -0.160(4) 0.394(3) 0.077 Uiso 1 1 d . U . . . H43B H 0.928(5) -0.063(4) 0.383(3) 0.077 Uiso 1 1 d . U . . . H43C H 1.031(5) -0.066(4) 0.393(3) 0.077 Uiso 1 1 d . U . . . C45 C 1.1950(3) 0.0947(2) 0.3473(2) 0.0263(8) Uani 1 1 d . . . . . C47 C 1.3113(4) 0.0158(3) 0.3275(3) 0.0419(11) Uani 1 1 d . . . . . H47A H 1.313(4) -0.047(4) 0.354(3) 0.063 Uiso 1 1 d . U . . . H47B H 1.367(4) 0.021(3) 0.342(3) 0.063 Uiso 1 1 d . U . . . H47C H 1.331(4) 0.012(4) 0.277(3) 0.063 Uiso 1 1 d . U . . . C46 C 1.1629(4) 0.0941(4) 0.4239(3) 0.0446(11) Uani 1 1 d . . . . . H46A H 1.156(4) 0.035(4) 0.447(3) 0.067 Uiso 1 1 d . U . . . H46B H 1.089(4) 0.145(4) 0.437(3) 0.067 Uiso 1 1 d . U . . . H46C H 1.220(4) 0.100(4) 0.436(3) 0.067 Uiso 1 1 d . U . . . C48 C 1.1915(4) 0.1931(3) 0.3106(3) 0.0429(12) Uani 1 1 d . . . . . H48A H 1.236(4) 0.214(3) 0.324(3) 0.064 Uiso 1 1 d . U . . . H48B H 1.114(4) 0.244(4) 0.322(3) 0.064 Uiso 1 1 d . U . . . H48C H 1.209(4) 0.196(4) 0.264(3) 0.064 Uiso 1 1 d . U . . . C49 C 1.2301(3) 0.0715(3) 0.1280(2) 0.0404(10) Uani 1 1 d . . . . . C50 C 1.3387(5) -0.0149(5) 0.1106(3) 0.0619(16) Uani 1 1 d . . . . . H50A H 1.389(5) -0.018(4) 0.139(3) 0.093 Uiso 1 1 d . U . . . H50B H 1.372(5) -0.017(4) 0.063(3) 0.093 Uiso 1 1 d . U . . . H50C H 1.329(5) -0.071(4) 0.121(3) 0.093 Uiso 1 1 d . U . . . C52 C 1.1403(5) 0.0799(5) 0.0918(3) 0.0583(14) Uani 1 1 d . . . . . H52A H 1.121(5) 0.020(4) 0.103(3) 0.087 Uiso 1 1 d . U . . . H52B H 1.168(4) 0.084(4) 0.041(3) 0.087 Uiso 1 1 d . U . . . H52C H 1.070(5) 0.133(4) 0.103(3) 0.087 Uiso 1 1 d . U . . . H1 H 0.886(5) -0.091(4) 0.290(3) 0.087 Uiso 1 1 d . U . . . H42A H 1.002(5) -0.192(4) 0.286(3) 0.087 Uiso 1 1 d . U . . . H42B H 1.001(5) -0.124(4) 0.218(3) 0.087 Uiso 1 1 d . U . . . H30A H 0.791(5) 0.179(4) -0.087(3) 0.087 Uiso 1 1 d . U . . . H30B H 0.779(4) 0.275(4) -0.127(3) 0.087 Uiso 1 1 d . U . . . H30C H 0.686(5) 0.268(4) -0.063(3) 0.087 Uiso 1 1 d . 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 0.01819(6) 0.01541(6) 0.01879(6) -0.00018(4) -0.00424(4) -0.00854(4) K1 0.0279(4) 0.0208(4) 0.0269(4) 0.0000(3) -0.0087(3) -0.0111(3) K2 0.0406(5) 0.0374(5) 0.0233(4) -0.0027(3) 0.0019(3) -0.0241(4) S1 0.0338(5) 0.0282(5) 0.0234(5) -0.0004(4) 0.0016(4) -0.0173(4) Si4 0.0236(4) 0.0180(4) 0.0194(5) -0.0021(4) -0.0036(4) -0.0106(4) Si2 0.0211(4) 0.0216(5) 0.0209(5) -0.0022(4) -0.0054(4) -0.0103(4) Si1 0.0232(5) 0.0209(5) 0.0201(5) -0.0009(4) -0.0026(4) -0.0123(4) Si3 0.0212(4) 0.0200(5) 0.0261(5) -0.0008(4) -0.0098(4) -0.0063(4) O61 0.0299(13) 0.0196(12) 0.0265(14) -0.0042(10) -0.0048(10) -0.0121(11) O62 0.0237(12) 0.0236(12) 0.0265(14) 0.0015(10) -0.0070(10) -0.0113(10) O64 0.0338(13) 0.0217(12) 0.0256(14) -0.0067(10) -0.0007(10) -0.0157(11) O63 0.0282(12) 0.0237(12) 0.0252(14) 0.0021(10) -0.0112(10) -0.0120(11) O21 0.0275(12) 0.0311(13) 0.0257(14) -0.0011(11) -0.0104(10) -0.0171(11) O22 0.0308(13) 0.0232(12) 0.0245(14) -0.0032(10) -0.0087(10) -0.0150(11) O23 0.0241(12) 0.0291(13) 0.0223(13) -0.0024(10) -0.0062(10) -0.0103(11) O24 0.0303(13) 0.0255(13) 0.0215(13) -0.0025(10) -0.0040(10) -0.0104(11) O1 0.0255(12) 0.0216(12) 0.0238(13) -0.0031(10) -0.0006(10) -0.0126(10) O2 0.0320(13) 0.0267(13) 0.0239(14) -0.0012(10) -0.0014(10) -0.0206(11) O4 0.0233(12) 0.0265(13) 0.0284(14) -0.0051(11) -0.0066(10) -0.0089(11) O3 0.0239(12) 0.0267(13) 0.0213(13) -0.0026(10) -0.0053(9) -0.0112(10) O41 0.0232(12) 0.0248(13) 0.0252(14) 0.0011(10) -0.0079(10) -0.0047(10) O42 0.0279(13) 0.0215(12) 0.0424(17) -0.0005(11) -0.0169(11) -0.0104(11) O43 0.0254(12) 0.0257(13) 0.0269(14) -0.0009(10) -0.0108(10) -0.0122(11) O44 0.0249(12) 0.0327(14) 0.0278(15) -0.0030(11) -0.0076(10) -0.0067(11) C61 0.0304(19) 0.0265(18) 0.031(2) 0.0049(15) -0.0149(15) -0.0131(16) C64 0.044(3) 0.044(3) 0.030(2) 0.011(2) -0.0104(19) -0.015(2) C62 0.025(2) 0.043(3) 0.048(3) -0.007(2) -0.0057(18) -0.0035(19) C63 0.071(4) 0.048(3) 0.083(5) 0.011(3) -0.051(3) -0.036(3) C69 0.040(2) 0.0267(19) 0.033(2) -0.0140(16) -0.0020(17) -0.0141(17) C72 0.054(3) 0.034(2) 0.061(3) -0.015(2) 0.001(2) -0.027(2) C71 0.037(3) 0.036(3) 0.085(4) -0.032(3) 0.001(3) -0.008(2) C70 0.097(5) 0.055(4) 0.036(3) -0.020(3) -0.022(3) -0.016(3) C65 0.036(2) 0.0249(19) 0.031(2) -0.0005(16) -0.0158(16) -0.0097(16) C66 0.033(2) 0.045(3) 0.048(3) -0.003(2) -0.015(2) -0.017(2) C67 0.048(3) 0.032(2) 0.049(3) 0.004(2) -0.024(2) -0.007(2) C68 0.051(3) 0.041(3) 0.041(3) -0.006(2) -0.025(2) -0.012(2) C21 0.038(2) 0.0277(19) 0.032(2) -0.0080(16) -0.0069(16) -0.0195(17) C24 0.061(3) 0.051(3) 0.044(3) -0.006(2) -0.020(2) -0.037(3) C23 0.062(3) 0.039(2) 0.043(3) -0.004(2) -0.002(2) -0.038(2) C22 0.053(3) 0.038(3) 0.056(3) -0.017(2) -0.001(2) -0.020(2) C25 0.0270(18) 0.030(2) 0.028(2) -0.0022(16) -0.0033(15) -0.0088(16) C27 0.029(2) 0.084(4) 0.043(3) -0.002(3) -0.014(2) 0.001(3) C26 0.034(2) 0.039(2) 0.029(2) -0.0043(19) 0.0001(17) -0.008(2) C28 0.061(3) 0.036(3) 0.076(4) -0.020(3) 0.016(3) -0.017(2) C81 0.076(5) 0.112(6) 0.071(6) -0.017(6) -0.037(4) -0.052(6) C82 0.066(6) 0.123(7) 0.063(6) -0.013(6) -0.015(6) -0.063(6) C83 0.084(6) 0.123(8) 0.065(6) -0.020(6) -0.016(5) -0.062(6) C84 0.093(8) 0.127(9) 0.079(8) -0.019(8) -0.037(7) -0.046(8) C85 0.068(6) 0.132(8) 0.068(6) -0.015(7) -0.026(5) -0.044(6) C86 0.061(6) 0.127(8) 0.068(7) -0.013(7) -0.024(6) -0.051(7) C87 0.137(12) 0.084(10) 0.126(13) -0.011(10) -0.093(11) -0.041(10) C5 0.0307(19) 0.035(2) 0.031(2) 0.0000(16) -0.0140(16) -0.0147(17) C6 0.054(3) 0.050(3) 0.029(2) -0.002(2) -0.021(2) -0.016(2) C42 0.080(4) 0.034(3) 0.117(6) -0.005(3) -0.059(4) -0.024(3) C30 0.117(5) 0.096(5) 0.033(3) 0.007(3) -0.027(3) -0.073(5) C51 0.048(3) 0.059(3) 0.042(3) 0.008(3) 0.000(2) -0.016(3) C29 0.036(2) 0.036(2) 0.023(2) -0.0030(16) -0.0044(15) -0.0152(18) C31 0.047(3) 0.037(2) 0.032(2) 0.0040(19) -0.0014(19) -0.020(2) C32 0.042(3) 0.062(4) 0.062(4) 0.003(3) 0.019(3) 0.000(3) C1 0.046(2) 0.037(2) 0.031(2) 0.0014(17) -0.0011(17) -0.032(2) C2 0.077(4) 0.040(3) 0.055(3) -0.010(2) 0.015(3) -0.040(3) C4 0.053(3) 0.073(4) 0.064(4) 0.006(3) -0.013(3) -0.049(3) C3 0.055(3) 0.051(3) 0.037(3) -0.005(2) 0.009(2) -0.037(3) C9 0.0277(18) 0.0294(19) 0.023(2) -0.0017(15) -0.0041(14) -0.0072(16) C11 0.038(2) 0.043(3) 0.043(3) -0.002(2) -0.016(2) 0.000(2) C10 0.038(2) 0.039(2) 0.031(2) -0.0101(19) 0.0009(18) -0.011(2) C12 0.042(2) 0.027(2) 0.051(3) -0.003(2) -0.002(2) -0.017(2) C7 0.034(2) 0.037(2) 0.047(3) -0.004(2) -0.013(2) -0.0088(19) C8 0.038(3) 0.054(3) 0.054(3) -0.008(3) -0.012(2) -0.026(2) C41 0.042(2) 0.0208(19) 0.059(3) 0.0035(18) -0.025(2) -0.0137(18) C44 0.042(3) 0.024(2) 0.071(4) -0.007(2) -0.016(2) -0.004(2) C43 0.050(3) 0.030(2) 0.063(4) 0.011(2) -0.011(2) -0.015(2) C45 0.0251(17) 0.0244(18) 0.035(2) -0.0028(15) -0.0129(15) -0.0109(15) C47 0.027(2) 0.041(2) 0.061(3) -0.008(2) -0.021(2) -0.0070(19) C46 0.041(2) 0.061(3) 0.041(3) -0.004(2) -0.020(2) -0.022(2) C48 0.053(3) 0.032(2) 0.057(3) 0.007(2) -0.031(2) -0.023(2) C49 0.033(2) 0.052(3) 0.027(2) -0.0090(19) -0.0057(17) -0.006(2) C50 0.042(3) 0.066(4) 0.054(4) -0.028(3) -0.001(2) 0.007(3) C52 0.048(3) 0.077(4) 0.040(3) -0.023(3) -0.018(2) -0.002(3) 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 O41 U1 O61 125.97(9) . . O41 U1 O21 99.78(9) . . O61 U1 O21 132.12(9) . . O41 U1 O1 84.98(8) . . O61 U1 O1 87.42(8) . . O21 U1 O1 82.90(8) . . O41 U1 S1 98.00(6) . . O61 U1 S1 92.07(6) . . O21 U1 S1 95.01(6) . . O1 U1 S1 176.64(6) . . O41 U1 K1 60.03(6) . . O61 U1 K1 138.95(6) . . O21 U1 K1 51.44(6) . . O1 U1 K1 51.56(6) . . S1 U1 K1 128.77(3) . . O2 K1 O42 123.38(8) . . O2 K1 O22 108.33(8) . . O42 K1 O22 127.82(8) . . O2 K1 O21 104.24(8) . . O42 K1 O21 112.04(7) . . O22 K1 O21 55.81(7) . . O2 K1 O1 55.54(6) . . O42 K1 O1 105.36(7) . . O22 K1 O1 109.28(7) . . O21 K1 O1 63.55(7) . . O2 K1 O41 109.04(7) . . O42 K1 O41 51.93(6) . . O22 K1 O41 119.07(7) . . O21 K1 O41 69.39(6) . . O1 K1 O41 60.53(6) . . O2 K1 Si2 110.19(6) . . O42 K1 Si2 122.21(6) . . O22 K1 Si2 28.41(5) . . O21 K1 Si2 27.51(5) . . O1 K1 Si2 86.86(5) . . O41 K1 Si2 93.17(5) . . O2 K1 Si1 28.21(5) . . O42 K1 Si1 116.43(6) . . O22 K1 Si1 112.27(6) . . O21 K1 Si1 83.81(6) . . O1 K1 Si1 27.35(4) . . O41 K1 Si1 83.82(5) . . Si2 K1 Si1 100.07(3) . . O2 K1 U1 93.89(5) . . O42 K1 U1 89.29(5) . . O22 K1 U1 94.11(5) . . O21 K1 U1 38.30(5) . . O1 K1 U1 38.71(4) . . O41 K1 U1 37.68(4) . . Si2 K1 U1 65.753(19) . . Si1 K1 U1 65.925(19) . . O2 K1 Si3 117.60(6) . . O42 K1 Si3 25.70(5) . . O22 K1 Si3 129.44(6) . . O21 K1 Si3 91.97(5) . . O1 K1 Si3 82.17(5) . . O41 K1 Si3 26.33(4) . . Si2 K1 Si3 110.69(3) . . Si1 K1 Si3 99.68(3) . . U1 K1 Si3 63.948(19) . . O2 K1 H1 107.7(12) . . O42 K1 H1 57.6(11) . . O22 K1 H1 102.5(11) . . O21 K1 H1 146.0(12) . . O1 K1 H1 147.4(12) . . O41 K1 H1 109.6(11) . . Si2 K1 H1 125.6(12) . . Si1 K1 H1 130.2(12) . . U1 K1 H1 146.6(11) . . Si3 K1 H1 83.3(11) . . O63 K2 O62 53.26(7) . . O63 K2 S1 123.95(6) . 2_765 O62 K2 S1 167.26(6) . 2_765 O63 K2 S1 91.92(5) . . O62 K2 S1 90.65(5) . . S1 K2 S1 102.01(3) 2_765 . O63 K2 Si4 28.83(5) . . O62 K2 Si4 29.06(5) . . S1 K2 Si4 152.05(4) 2_765 . S1 K2 Si4 79.65(3) . . O63 K2 K2 117.83(6) . 2_765 O62 K2 K2 141.05(6) . 2_765 S1 K2 K2 51.59(3) 2_765 2_765 S1 K2 K2 50.42(3) . 2_765 Si4 K2 K2 123.52(3) . 2_765 O63 K2 H2A 106.6(9) . . O62 K2 H2A 53.7(10) . . S1 K2 H2A 128.8(9) 2_765 . S1 K2 H2A 82.6(9) . . Si4 K2 H2A 79.1(9) . . K2 K2 H2A 113.0(10) 2_765 . O63 K2 H2B 56.1(10) . . O62 K2 H2B 108.7(10) . . S1 K2 H2B 71.8(10) 2_765 . S1 K2 H2B 83.6(9) . . Si4 K2 H2B 80.8(10) . . K2 K2 H2B 70.4(10) 2_765 . H2A K2 H2B 157.4(13) . . U1 S1 K2 151.91(4) . 2_765 U1 S1 K2 114.88(4) . . K2 S1 K2 77.99(3) 2_765 . O61 Si4 O64 108.33(12) . . O61 Si4 O63 114.24(13) . . O64 Si4 O63 111.20(13) . . O61 Si4 O62 113.54(13) . . O64 Si4 O62 112.01(13) . . O63 Si4 O62 97.29(12) . . O61 Si4 K2 100.23(10) . . O64 Si4 K2 151.41(8) . . O63 Si4 K2 53.23(9) . . O62 Si4 K2 55.08(9) . . O21 Si2 O24 115.60(13) . . O21 Si2 O23 114.22(14) . . O24 Si2 O23 105.74(13) . . O21 Si2 O22 104.77(13) . . O24 Si2 O22 105.17(13) . . O23 Si2 O22 111.02(12) . . O21 Si2 K1 54.51(9) . . O24 Si2 K1 120.14(10) . . O23 Si2 K1 133.18(10) . . O22 Si2 K1 50.51(9) . . O1 Si1 O4 115.45(13) . . O1 Si1 O3 114.63(12) . . O4 Si1 O3 105.75(13) . . O1 Si1 O2 103.88(13) . . O4 Si1 O2 106.21(12) . . O3 Si1 O2 110.64(13) . . O1 Si1 K1 54.26(9) . . O4 Si1 K1 126.96(10) . . O3 Si1 K1 126.27(10) . . O2 Si1 K1 49.68(9) . . O41 Si3 O44 115.35(13) . . O41 Si3 O43 115.50(14) . . O44 Si3 O43 105.03(13) . . O41 Si3 O42 104.83(12) . . O44 Si3 O42 111.16(14) . . O43 Si3 O42 104.54(13) . . O41 Si3 K1 60.61(8) . . O44 Si3 K1 133.79(11) . . O43 Si3 K1 118.12(9) . . O42 Si3 K1 44.50(9) . . Si4 O61 U1 152.80(14) . . C61 O62 Si4 131.2(2) . . C61 O62 K2 118.1(2) . . Si4 O62 K2 95.86(11) . . C69 O64 Si4 135.5(2) . . C65 O63 Si4 132.0(2) . . C65 O63 K2 117.2(2) . . Si4 O63 K2 97.93(11) . . Si2 O21 U1 170.65(14) . . Si2 O21 K1 97.98(10) . . U1 O21 K1 90.26(8) . . C21 O22 Si2 129.8(2) . . C21 O22 K1 127.1(2) . . Si2 O22 K1 101.08(10) . . C25 O23 Si2 131.0(2) . . C29 O24 Si2 133.2(2) . . Si1 O1 U1 169.33(15) . . Si1 O1 K1 98.38(10) . . U1 O1 K1 89.73(8) . . C1 O2 Si1 129.2(2) . . C1 O2 K1 128.6(2) . . Si1 O2 K1 102.10(10) . . C9 O4 Si1 131.5(2) . . C5 O3 Si1 131.0(2) . . Si3 O41 U1 173.32(16) . . Si3 O41 K1 93.06(10) . . U1 O41 K1 82.30(7) . . C41 O42 Si3 130.4(2) . . C41 O42 K1 117.36(19) . . Si3 O42 K1 109.79(12) . . C45 O43 Si3 131.0(2) . . C49 O44 Si3 136.2(2) . . O62 C61 C62 107.7(3) . . O62 C61 C63 106.8(3) . . C62 C61 C63 110.2(4) . . O62 C61 C64 112.0(3) . . C62 C61 C64 110.0(4) . . C63 C61 C64 110.1(4) . . C61 C64 H64A 113(3) . . C61 C64 H64B 115(3) . . H64A C64 H64B 114(4) . . C61 C64 H64C 112(3) . . H64A C64 H64C 106(4) . . H64B C64 H64C 97(4) . . C61 C62 H62A 109(3) . . C61 C62 H2A 107(3) . . H62A C62 H2A 104(4) . . C61 C62 H62B 114(3) . . H62A C62 H62B 110(4) . . H2A C62 H62B 113(4) . . C61 C63 H63A 113(4) . . C61 C63 H63B 105(4) . . H63A C63 H63B 115(6) . . C61 C63 H63C 111(3) . . H63A C63 H63C 99(5) . . H63B C63 H63C 114(5) . . O64 C69 C70 107.4(4) . . O64 C69 C71 107.8(3) . . C70 C69 C71 110.5(4) . . O64 C69 C72 111.2(3) . . C70 C69 C72 111.3(4) . . C71 C69 C72 108.6(4) . . C69 C72 H72A 108(3) . . C69 C72 H72B 109(3) . . H72A C72 H72B 113(4) . . C69 C72 H72C 111(3) . . H72A C72 H72C 100(4) . . H72B C72 H72C 116(4) . . C69 C71 H71A 113(3) . . C69 C71 H71B 109(3) . . H71A C71 H71B 110(4) . . C69 C71 H71C 112(3) . . H71A C71 H71C 106(4) . . H71B C71 H71C 108(4) . . C69 C70 H70A 117(5) . . C69 C70 H70B 105(4) . . H70A C70 H70B 105(6) . . C69 C70 H70C 114(3) . . H70A C70 H70C 99(6) . . H70B C70 H70C 117(5) . . O63 C65 C68 108.0(3) . . O63 C65 C66 111.6(3) . . C68 C65 C66 110.6(4) . . O63 C65 C67 106.1(3) . . C68 C65 C67 110.3(4) . . C66 C65 C67 110.2(4) . . C65 C66 H66A 113(3) . . C65 C66 H66B 110(3) . . H66A C66 H66B 116(4) . . C65 C66 H66C 116(3) . . H66A C66 H66C 102(4) . . H66B C66 H66C 99(4) . . C65 C67 H67A 114(3) . . C65 C67 H67B 108(3) . . H67A C67 H67B 108(4) . . C65 C67 H67C 109(3) . . H67A C67 H67C 105(4) . . H67B C67 H67C 112(4) . . C65 C68 H68A 113(3) . . C65 C68 H2B 116(3) . . H68A C68 H2B 108(4) . . C65 C68 H68B 106(3) . . H68A C68 H68B 112(4) . . H2B C68 H68B 102(4) . . O22 C21 C22 107.0(3) . . O22 C21 C24 112.2(3) . . C22 C21 C24 111.5(4) . . O22 C21 C23 105.2(3) . . C22 C21 C23 110.9(4) . . C24 C21 C23 109.8(4) . . C21 C24 H24A 114(3) . . C21 C24 H24B 114(3) . . H24A C24 H24B 99(4) . . C21 C24 H24C 113(3) . . H24A C24 H24C 109(4) . . H24B C24 H24C 107(4) . . C21 C23 H23A 111(3) . . C21 C23 H23B 114(3) . . H23A C23 H23B 107(4) . . C21 C23 H23C 111(3) . . H23A C23 H23C 105(4) . . H23B C23 H23C 109(4) . . C21 C22 H22A 110(3) . . C21 C22 H22B 111(3) . . H22A C22 H22B 106(4) . . C21 C22 H22C 113(3) . . H22A C22 H22C 111(4) . . H22B C22 H22C 105(4) . . O23 C25 C28 108.6(3) . . O23 C25 C27 104.7(4) . . C28 C25 C27 111.7(4) . . O23 C25 C26 111.9(3) . . C28 C25 C26 110.0(4) . . C27 C25 C26 109.8(3) . . C25 C27 H27A 109(4) . . C25 C27 H27B 107(3) . . H27A C27 H27B 108(5) . . C25 C27 H27C 118(3) . . H27A C27 H27C 102(6) . . H27B C27 H27C 113(4) . . C25 C26 H26A 111(4) . . C25 C26 H26B 112(3) . . H26A C26 H26B 107(4) . . C25 C26 H26C 111(3) . . H26A C26 H26C 110(5) . . H26B C26 H26C 106(4) . . 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 . . C82 C81 C86 120.0 . . C82 C81 C87 118.9(10) . . C86 C81 C87 121.0(10) . . C83 C82 C81 120.0 . . C83 C82 H82 120.0 . . C81 C82 H82 120.0 . . C82 C83 C84 120.0 . . C82 C83 H83 120.0 . . C84 C83 H83 120.0 . . C83 C84 C85 120.0 . . C83 C84 H84 120.0 . . C85 C84 H84 120.0 . . C86 C85 C84 120.0 . . C86 C85 H85 120.0 . . C84 C85 H85 120.0 . . C85 C86 C81 120.0 . . C85 C86 H86 120.0 . . C81 C86 H86 120.0 . . C81 C87 H87A 109.5 . . C81 C87 H87B 109.5 . . H87A C87 H87B 109.5 . . C81 C87 H87C 109.5 . . H87A C87 H87C 109.5 . . H87B C87 H87C 109.5 . . O3 C5 C7 110.6(3) . . O3 C5 C6 105.5(3) . . C7 C5 C6 111.7(4) . . O3 C5 C8 107.4(3) . . C7 C5 C8 110.8(4) . . C6 C5 C8 110.6(4) . . C5 C6 H6A 111(3) . . C5 C6 H6B 113(3) . . H6A C6 H6B 105(4) . . C5 C6 H6C 108(3) . . H6A C6 H6C 109(4) . . H6B C6 H6C 111(4) . . C41 C42 H1 104(3) . . C41 C42 H42A 104(3) . . H1 C42 H42A 101(4) . . C41 C42 H42B 116(4) . . H1 C42 H42B 116(5) . . H42A C42 H42B 114(5) . . C29 C30 H30A 105(4) . . C29 C30 H30B 112(3) . . H30A C30 H30B 101(5) . . C29 C30 H30C 110(4) . . H30A C30 H30C 114(5) . . H30B C30 H30C 114(5) . . C49 C51 H51A 109(3) . . C49 C51 H51B 110(4) . . H51A C51 H51B 105(5) . . C49 C51 H51C 109(3) . . H51A C51 H51C 112(5) . . H51B C51 H51C 111(4) . . O24 C29 C30 108.1(3) . . O24 C29 C31 111.2(3) . . C30 C29 C31 110.2(4) . . O24 C29 C32 105.4(3) . . C30 C29 C32 112.5(5) . . C31 C29 C32 109.4(4) . . C29 C31 H31A 111(3) . . C29 C31 H31B 112(3) . . H31A C31 H31B 105(4) . . C29 C31 H31C 111(3) . . H31A C31 H31C 106(4) . . H31B C31 H31C 112(4) . . C29 C32 H32A 108(4) . . C29 C32 H32B 106(4) . . H32A C32 H32B 101(6) . . C29 C32 H32C 110(5) . . H32A C32 H32C 121(6) . . H32B C32 H32C 111(6) . . O2 C1 C3 111.8(3) . . O2 C1 C4 108.3(3) . . C3 C1 C4 111.8(4) . . O2 C1 C2 104.8(3) . . C3 C1 C2 109.7(4) . . C4 C1 C2 110.3(4) . . C1 C2 H2C 115(3) . . C1 C2 H2D 113(3) . . H2C C2 H2D 101(4) . . C1 C2 H2E 117(4) . . H2C C2 H2E 91(4) . . H2D C2 H2E 117(5) . . C1 C4 H4A 113(4) . . C1 C4 H4B 108(3) . . H4A C4 H4B 107(5) . . C1 C4 H4C 107(3) . . H4A C4 H4C 108(6) . . H4B C4 H4C 114(4) . . C1 C3 H3A 108(3) . . C1 C3 H3B 111(3) . . H3A C3 H3B 114(4) . . C1 C3 H3C 112(4) . . H3A C3 H3C 111(4) . . H3B C3 H3C 101(4) . . O4 C9 C12 111.0(3) . . O4 C9 C11 105.4(3) . . C12 C9 C11 110.5(4) . . O4 C9 C10 108.1(3) . . C12 C9 C10 110.8(4) . . C11 C9 C10 111.0(3) . . C9 C11 H11A 112(3) . . C9 C11 H11B 109(3) . . H11A C11 H11B 106(4) . . C9 C11 H11C 111(3) . . H11A C11 H11C 111(4) . . H11B C11 H11C 106(4) . . C9 C10 H10A 110(3) . . C9 C10 H10B 111(3) . . H10A C10 H10B 109(4) . . C9 C10 H10C 114(3) . . H10A C10 H10C 107(4) . . H10B C10 H10C 105(4) . . C9 C12 H12A 110(3) . . C9 C12 H12B 108(3) . . H12A C12 H12B 107(4) . . C9 C12 H12C 110(3) . . H12A C12 H12C 112(4) . . H12B C12 H12C 108(4) . . C5 C7 H7A 110(3) . . C5 C7 H7B 106(3) . . H7A C7 H7B 112(4) . . C5 C7 H7C 111(3) . . H7A C7 H7C 109(4) . . H7B C7 H7C 109(4) . . C5 C8 H8A 112(3) . . C5 C8 H8B 107(3) . . H8A C8 H8B 107(4) . . C5 C8 H8C 107(3) . . H8A C8 H8C 110(4) . . H8B C8 H8C 113(4) . . O42 C41 C43 108.2(4) . . O42 C41 C44 111.2(3) . . C43 C41 C44 111.4(4) . . O42 C41 C42 104.8(3) . . C43 C41 C42 111.2(4) . . C44 C41 C42 109.8(4) . . C41 C44 H44A 113(3) . . C41 C44 H44B 109(3) . . H44A C44 H44B 108(4) . . C41 C44 H44C 114(4) . . H44A C44 H44C 107(4) . . H44B C44 H44C 105(4) . . C41 C43 H43A 109(3) . . C41 C43 H43B 112(4) . . H43A C43 H43B 109(4) . . C41 C43 H43C 114(4) . . H43A C43 H43C 106(5) . . H43B C43 H43C 108(5) . . O43 C45 C46 105.6(3) . . O43 C45 C48 109.5(3) . . C46 C45 C48 111.0(4) . . O43 C45 C47 108.6(3) . . C46 C45 C47 110.6(4) . . C48 C45 C47 111.2(4) . . C45 C47 H47A 110(3) . . C45 C47 H47B 113(3) . . H47A C47 H47B 100(4) . . C45 C47 H47C 111(3) . . H47A C47 H47C 110(4) . . H47B C47 H47C 112(4) . . C45 C46 H46A 112(3) . . C45 C46 H46B 111(3) . . H46A C46 H46B 106(4) . . C45 C46 H46C 106(3) . . H46A C46 H46C 109(4) . . H46B C46 H46C 115(4) . . C45 C48 H48A 113(3) . . C45 C48 H48B 111(3) . . H48A C48 H48B 103(4) . . C45 C48 H48C 113(3) . . H48A C48 H48C 109(4) . . H48B C48 H48C 107(4) . . O44 C49 C52 111.1(4) . . O44 C49 C50 105.5(4) . . C52 C49 C50 111.5(5) . . O44 C49 C51 107.7(4) . . C52 C49 C51 110.3(4) . . C50 C49 C51 110.5(4) . . C49 C50 H50A 106(4) . . C49 C50 H50B 116(4) . . H50A C50 H50B 114(5) . . C49 C50 H50C 113(4) . . H50A C50 H50C 107(5) . . H50B C50 H50C 100(5) . . C49 C52 H52A 114(3) . . C49 C52 H52B 111(3) . . H52A C52 H52B 102(5) . . C49 C52 H52C 113(4) . . H52A C52 H52C 106(4) . . H52B C52 H52C 110(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 O41 2.208(2) . U1 O61 2.216(2) . U1 O21 2.219(2) . U1 O1 2.239(2) . U1 S1 2.5440(8) . U1 K1 3.5800(7) . K1 O2 2.665(3) . K1 O42 2.672(2) . K1 O22 2.677(3) . K1 O21 2.799(2) . K1 O1 2.804(2) . K1 O41 3.129(2) . K1 Si2 3.4047(12) . K1 Si1 3.4178(13) . K1 Si3 3.5867(11) . K1 H1 2.82(6) . K2 O63 2.727(3) . K2 O62 2.779(3) . K2 S1 3.0455(12) 2_765 K2 S1 3.0962(12) . K2 Si4 3.3711(12) . K2 K2 3.8649(18) 2_765 K2 H2A 2.93(5) . K2 H2B 2.97(5) . S1 K2 3.0455(12) 2_765 Si4 O61 1.590(2) . Si4 O64 1.614(3) . Si4 O63 1.641(2) . Si4 O62 1.646(2) . Si2 O21 1.588(2) . Si2 O24 1.614(3) . Si2 O23 1.621(3) . Si2 O22 1.651(2) . Si1 O1 1.587(2) . Si1 O4 1.618(3) . Si1 O3 1.622(3) . Si1 O2 1.653(2) . Si3 O41 1.593(2) . Si3 O44 1.618(3) . Si3 O43 1.622(3) . Si3 O42 1.653(2) . O62 C61 1.441(4) . O64 C69 1.449(4) . O63 C65 1.447(4) . O22 C21 1.456(4) . O23 C25 1.433(4) . O24 C29 1.436(4) . O2 C1 1.451(4) . O4 C9 1.436(4) . O3 C5 1.442(4) . O42 C41 1.449(4) . O43 C45 1.445(4) . O44 C49 1.432(5) . C61 C62 1.507(6) . C61 C63 1.516(6) . C61 C64 1.518(5) . C64 H64A 0.88(5) . C64 H64B 0.95(5) . C64 H64C 1.04(5) . C62 H62A 0.96(5) . C62 H2A 1.01(5) . C62 H62B 0.98(5) . C63 H63A 0.85(6) . C63 H63B 0.89(6) . C63 H63C 0.95(6) . C69 C70 1.494(7) . C69 C71 1.505(6) . C69 C72 1.522(5) . C72 H72A 0.96(5) . C72 H72B 1.03(6) . C72 H72C 0.92(5) . C71 H71A 0.98(6) . C71 H71B 0.96(5) . C71 H71C 1.02(6) . C70 H70A 0.76(6) . C70 H70B 0.97(6) . C70 H70C 1.17(6) . C65 C68 1.506(6) . C65 C66 1.517(6) . C65 C67 1.519(5) . C66 H66A 0.87(5) . C66 H66B 1.02(5) . C66 H66C 0.95(5) . C67 H67A 0.91(5) . C67 H67B 0.94(5) . C67 H67C 0.99(6) . C68 H68A 0.91(5) . C68 H2B 0.94(5) . C68 H68B 0.96(5) . C21 C22 1.506(6) . C21 C24 1.507(6) . C21 C23 1.522(5) . C24 H24A 0.98(5) . C24 H24B 0.93(5) . C24 H24C 0.95(5) . C23 H23A 1.02(5) . C23 H23B 0.98(5) . C23 H23C 0.98(5) . C22 H22A 1.02(6) . C22 H22B 0.94(5) . C22 H22C 0.95(5) . C25 C28 1.512(6) . C25 C27 1.513(6) . C25 C26 1.514(5) . C27 H27A 0.81(6) . C27 H27B 1.00(6) . C27 H27C 1.02(6) . C26 H26A 0.84(5) . C26 H26B 0.95(5) . C26 H26C 0.85(5) . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C81 C82 1.3900 . C81 C86 1.3900 . C81 C87 1.442(13) . C82 C83 1.3900 . C82 H82 0.9500 . C83 C84 1.3900 . C83 H83 0.9500 . C84 C85 1.3900 . C84 H84 0.9500 . C85 C86 1.3900 . C85 H85 0.9500 . C86 H86 0.9500 . C87 H87A 0.9800 . C87 H87B 0.9800 . C87 H87C 0.9800 . C5 C7 1.509(6) . C5 C6 1.516(6) . C5 C8 1.519(5) . C6 H6A 0.98(5) . C6 H6B 0.94(5) . C6 H6C 0.89(5) . C42 C41 1.527(6) . C42 H1 1.21(6) . C42 H42A 0.93(6) . C42 H42B 0.90(6) . C30 C29 1.502(7) . C30 H30A 0.95(6) . C30 H30B 0.97(6) . C30 H30C 0.89(6) . C51 C49 1.528(7) . C51 H51A 0.96(6) . C51 H51B 0.91(6) . C51 H51C 1.08(6) . C29 C31 1.507(6) . C29 C32 1.513(6) . C31 H31A 0.93(5) . C31 H31B 1.00(5) . C31 H31C 0.97(5) . C32 H32A 0.95(7) . C32 H32B 0.91(7) . C32 H32C 0.90(7) . C1 C3 1.500(6) . C1 C4 1.520(7) . C1 C2 1.522(6) . C2 H2C 1.04(6) . C2 H2D 0.93(5) . C2 H2E 0.93(6) . C4 H4A 0.80(6) . C4 H4B 0.99(5) . C4 H4C 1.01(6) . C3 H3A 0.99(5) . C3 H3B 1.03(5) . C3 H3C 0.89(5) . C9 C12 1.516(5) . C9 C11 1.518(6) . C9 C10 1.520(6) . C11 H11A 0.99(5) . C11 H11B 0.94(5) . C11 H11C 1.03(5) . C10 H10A 0.87(4) . C10 H10B 0.84(5) . C10 H10C 1.02(5) . C12 H12A 0.92(5) . C12 H12B 0.92(5) . C12 H12C 0.97(5) . C7 H7A 0.87(4) . C7 H7B 0.95(5) . C7 H7C 0.98(5) . C8 H8A 0.92(5) . C8 H8B 0.92(5) . C8 H8C 0.97(6) . C41 C43 1.505(7) . C41 C44 1.512(6) . C44 H44A 0.98(6) . C44 H44B 0.95(5) . C44 H44C 0.89(5) . C43 H43A 0.98(5) . C43 H43B 0.88(5) . C43 H43C 0.87(5) . C45 C46 1.501(6) . C45 C48 1.511(5) . C45 C47 1.526(6) . C47 H47A 0.99(5) . C47 H47B 0.92(5) . C47 H47C 1.00(5) . C46 H46A 0.94(5) . C46 H46B 0.98(5) . C46 H46C 0.90(5) . C48 H48A 0.89(5) . C48 H48B 1.00(5) . C48 H48C 0.90(5) . C49 C52 1.511(6) . C49 C50 1.515(7) . C50 H50A 0.97(6) . C50 H50B 0.94(6) . C50 H50C 0.89(6) . C52 H52A 1.02(5) . C52 H52B 0.99(6) . C52 H52C 0.96(6) .