#------------------------------------------------------------------------------ #$Date: 2016-09-10 02:12:59 +0300 (Sat, 10 Sep 2016) $ #$Revision: 186333 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543291.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_1543291 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_moiety 'C48 H108 K2 O16 S2 Si4 U, C7 H8' _chemical_formula_sum 'C55 H116 K2 O16 S2 Si4 U' _chemical_formula_weight 1526.18 _chemical_name_systematic ; ? ; _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-10-26 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _audit_update_record ; 2016-01-18 deposited with the CCDC. 2016-04-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.2882(5) _cell_length_b 19.3780(5) _cell_length_c 40.5378(9) _cell_measurement_reflns_used 13392 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.2600 _cell_measurement_theta_min 3.6210 _cell_volume 15151.7(6) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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 0.999 _diffrn_measurement_details ; 1 omega -44.00 47.50 0.7500 40.0000 omega____ theta____ kappa____ phi______ frames - 25.5614 -37.0000 -30.0000 122 2 omega -96.00 -6.00 0.7500 40.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 -57.0000 120.0000 120 3 omega -97.00 -31.00 0.7500 40.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 -77.0000 -30.0000 88 ; _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 0.0718 _diffrn_reflns_av_unetI/netI 0.0759 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_number 89393 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.508 _diffrn_reflns_theta_min 3.324 _exptl_absorpt_coefficient_mu 2.425 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'translucent pale yellow' _exptl_crystal_density_diffrn 1.338 _exptl_crystal_description plate _exptl_crystal_F_000 6336 _exptl_crystal_size_max 0.288 _exptl_crystal_size_mid 0.171 _exptl_crystal_size_min 0.018 _refine_diff_density_max 2.555 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 832 _refine_ls_number_reflns 23090 _refine_ls_number_restraints 266 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0550 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+37.6122P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1153 _reflns_Friedel_coverage 0.000 _reflns_number_gt 14501 _reflns_number_total 23090 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL CF solution in Pbca CELL 0.71073 19.288225 19.378044 40.537768 90 90 90 ZERR 8 0.000471 0.000496 0.000894 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H K O S Si U UNIT 440 928 16 128 16 32 8 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 DFIX 2.5 C86B C87B C82B C87B SIMU 0.02 0.04 1.7 C30B C30 C31 C31B SIMU 0.02 0.04 1.7 C81 > C87B EADP C27 C27b ISOR 0.01 0.02 C30 C30b ISOR 0.005 0.01 C23 C2 C43 C44 C52 C67 C68 SHEL 999 0.7 SIZE 0.018 0.171 0.288 FREE K2 C63 FREE K2 C68 FREE K1 C43 WGHT 0.029900 35.949000 FVAR 0.811510 0.634790 0.700150 0.767150 TEMP -123 U1 7 0.440059 0.442263 0.609365 11.000000 0.023710 0.024000 = 0.015890 0.001760 -0.002390 -0.001780 K1 3 0.511998 0.416768 0.690931 11.000000 0.031240 0.035340 = 0.021360 0.002180 -0.001440 0.002480 K2 3 0.401227 0.471714 0.494667 11.000000 0.059360 0.049420 = 0.027820 0.008480 0.002390 -0.015650 S1 5 0.474024 0.529505 0.557263 11.000000 0.052300 0.033350 = 0.026220 0.007850 0.001030 -0.003550 S2 5 0.517272 0.430279 0.552549 11.000000 0.044820 0.036160 = 0.025850 0.003240 0.007810 0.000210 Si1 6 0.535309 0.281081 0.636785 11.000000 0.031970 0.032410 = 0.022300 0.002270 0.001210 0.007220 O1 4 0.489675 0.348212 0.628853 11.000000 0.028940 0.031750 = 0.021820 0.002750 -0.000380 0.003010 O2 4 0.567342 0.295532 0.673624 11.000000 0.053940 0.040130 = 0.027150 0.000650 -0.009010 0.022290 O3 4 0.602083 0.268960 0.613521 11.000000 0.031940 0.047310 = 0.036990 -0.004270 0.005720 0.006080 O4 4 0.490832 0.210027 0.636658 11.000000 0.046920 0.030320 = 0.035720 0.000980 0.009780 0.003780 C1 1 0.620762 0.258228 0.691777 11.000000 0.067780 0.060770 = 0.041030 0.001860 -0.019170 0.036350 C2 1 0.608026 0.275395 0.727409 11.000000 0.138770 0.113150 = 0.054500 -0.000840 -0.039770 0.065680 AFIX 137 H2A 2 0.560963 0.261293 0.733535 11.000000 -1.500000 H2B 2 0.613140 0.325233 0.730718 11.000000 -1.500000 H2C 2 0.641669 0.250857 0.741214 11.000000 -1.500000 AFIX 0 C3 1 0.690604 0.282624 0.680888 11.000000 0.067210 0.099690 = 0.129370 0.025580 -0.053410 0.005900 AFIX 137 H3A 2 0.694167 0.332551 0.684343 11.000000 -1.500000 H3B 2 0.696902 0.272209 0.657422 11.000000 -1.500000 H3C 2 0.726544 0.259109 0.693758 11.000000 -1.500000 AFIX 0 C4 1 0.614550 0.180962 0.686813 11.000000 0.076200 0.057630 = 0.073390 0.015290 -0.025920 0.034820 AFIX 137 H4A 2 0.620450 0.170018 0.663378 11.000000 -1.500000 H4B 2 0.568714 0.165484 0.694165 11.000000 -1.500000 H4C 2 0.650468 0.157419 0.699685 11.000000 -1.500000 AFIX 0 C5 1 0.613638 0.245450 0.580373 11.000000 0.043930 0.044100 = 0.035620 0.000210 0.014320 0.018520 C6 1 0.659360 0.298509 0.563781 11.000000 0.061790 0.070500 = 0.067670 0.010140 0.028050 0.011150 AFIX 137 H6A 2 0.704650 0.299616 0.574725 11.000000 -1.500000 H6B 2 0.637558 0.344070 0.565353 11.000000 -1.500000 H6C 2 0.665498 0.286222 0.540513 11.000000 -1.500000 AFIX 0 C7 1 0.650305 0.176749 0.582996 11.000000 0.061960 0.055150 = 0.059270 -0.005190 0.002350 0.028330 AFIX 137 H7A 2 0.621458 0.144458 0.595557 11.000000 -1.500000 H7B 2 0.694780 0.183019 0.594294 11.000000 -1.500000 H7C 2 0.658454 0.158220 0.560839 11.000000 -1.500000 AFIX 0 C8 1 0.545805 0.238478 0.562136 11.000000 0.056980 0.057110 = 0.031530 -0.002240 0.001810 0.017580 AFIX 137 H8A 2 0.521954 0.283129 0.561873 11.000000 -1.500000 H8B 2 0.516625 0.204228 0.573254 11.000000 -1.500000 H8C 2 0.554780 0.223550 0.539437 11.000000 -1.500000 AFIX 0 C9 1 0.422630 0.195470 0.650016 11.000000 0.051780 0.032250 = 0.045060 0.005320 0.014030 -0.004420 C10 1 0.424379 0.120312 0.661142 11.000000 0.105260 0.046050 = 0.091500 0.021400 0.039360 -0.007000 AFIX 137 H10A 2 0.461114 0.114158 0.677582 11.000000 -1.500000 H10B 2 0.433567 0.090535 0.642097 11.000000 -1.500000 H10C 2 0.379581 0.107947 0.670896 11.000000 -1.500000 AFIX 0 C11 1 0.370846 0.205775 0.623489 11.000000 0.056270 0.071500 = 0.062760 0.000750 0.010780 -0.016950 AFIX 137 H11A 2 0.381011 0.174492 0.605120 11.000000 -1.500000 H11B 2 0.372899 0.253628 0.615730 11.000000 -1.500000 H11C 2 0.324364 0.196022 0.632066 11.000000 -1.500000 AFIX 0 C12 1 0.406755 0.240154 0.680243 11.000000 0.060340 0.057300 = 0.046860 0.004950 0.020320 0.001200 AFIX 137 H12A 2 0.403357 0.288624 0.673537 11.000000 -1.500000 H12B 2 0.444021 0.234990 0.696489 11.000000 -1.500000 H12C 2 0.362727 0.225444 0.690048 11.000000 -1.500000 AFIX 0 Si2 6 0.569476 0.561366 0.651016 11.000000 0.030130 0.034420 = 0.026180 0.000510 -0.005100 -0.009350 O21 4 0.515956 0.505260 0.637294 11.000000 0.032390 0.034700 = 0.020860 -0.000880 -0.004130 -0.009500 O22 4 0.580749 0.537533 0.689713 11.000000 0.038590 0.045600 = 0.027750 -0.003270 -0.011930 -0.008620 O23 4 0.642632 0.565203 0.631646 11.000000 0.032830 0.043390 = 0.047170 0.003560 0.001430 -0.013070 O24 4 0.541145 0.639633 0.653103 11.000000 0.046310 0.036790 = 0.037220 0.000230 -0.004130 -0.007600 C21 1 0.617121 0.571424 0.716573 11.000000 0.047130 0.063460 = 0.036540 -0.000220 -0.022220 -0.016030 C22 1 0.569810 0.621789 0.732543 11.000000 0.089260 0.113950 = 0.063310 -0.051980 -0.029370 -0.000420 AFIX 137 H22A 2 0.527264 0.598237 0.739461 11.000000 -1.500000 H22B 2 0.558256 0.658475 0.716837 11.000000 -1.500000 H22C 2 0.592682 0.641899 0.751871 11.000000 -1.500000 AFIX 0 C23 1 0.680941 0.607792 0.704569 11.000000 0.086070 0.130800 = 0.058040 -0.002330 -0.019450 -0.058810 AFIX 137 H23A 2 0.667982 0.642207 0.687963 11.000000 -1.500000 H23B 2 0.712763 0.574147 0.694745 11.000000 -1.500000 H23C 2 0.703786 0.630790 0.723155 11.000000 -1.500000 AFIX 0 C24 1 0.635401 0.513895 0.739752 11.000000 0.100980 0.107350 = 0.061020 0.012140 -0.053160 -0.029170 AFIX 137 H24A 2 0.667996 0.482392 0.728930 11.000000 -1.500000 H24B 2 0.593266 0.488645 0.745819 11.000000 -1.500000 H24C 2 0.656885 0.533064 0.759651 11.000000 -1.500000 AFIX 0 C25 1 0.689470 0.515440 0.617377 11.000000 0.028310 0.060260 = 0.056620 -0.001880 0.005990 -0.004730 PART 1 C26 1 0.683463 0.522429 0.580101 11.000000 0.068440 0.104210 = 0.057300 -0.010630 0.018520 -0.007980 AFIX 137 H26A 2 0.692188 0.570432 0.573726 11.000000 -1.500000 H26B 2 0.636720 0.509028 0.573119 11.000000 -1.500000 H26C 2 0.717609 0.492329 0.569452 11.000000 -1.500000 PART 1 41 AFIX 0 C27 1 0.672605 0.442852 0.630316 41.000000 0.037990 0.030940 = 0.074530 -0.001020 0.012800 0.006790 AFIX 137 H27A 2 0.671621 0.443523 0.654484 41.000000 -1.500000 H27B 2 0.708198 0.410379 0.622789 41.000000 -1.500000 H27C 2 0.627236 0.428345 0.621929 41.000000 -1.500000 PART 2 -41 AFIX 0 C27B 1 0.677751 0.441858 0.614407 -41.000000 0.037990 0.030940 = 0.074530 -0.001020 0.012800 0.006790 AFIX 137 H27D 2 0.640213 0.428024 0.629297 -41.000000 -1.500000 H27E 2 0.720229 0.416989 0.620288 -41.000000 -1.500000 H27F 2 0.664881 0.430785 0.591627 -41.000000 -1.500000 PART 0 AFIX 0 C28 1 0.761838 0.535536 0.628276 11.000000 0.032800 0.088020 = 0.096370 0.001630 0.002300 -0.009070 AFIX 137 H28A 2 0.795950 0.507040 0.616638 11.000000 -1.500000 H28B 2 0.766403 0.528282 0.652103 11.000000 -1.500000 H28C 2 0.769974 0.584286 0.623139 11.000000 -1.500000 AFIX 0 C29 1 0.543551 0.700102 0.632716 11.000000 0.061800 0.033820 = 0.053830 0.004040 0.007680 -0.005490 PART 2 -21 C30B 1 0.480512 0.688418 0.606094 -21.000000 0.095690 0.043170 = 0.100090 0.022260 -0.045800 -0.036080 AFIX 137 H30D 2 0.483330 0.641627 0.597019 -21.000000 -1.500000 H30E 2 0.484773 0.722100 0.588175 -21.000000 -1.500000 H30F 2 0.435797 0.694551 0.617192 -21.000000 -1.500000 AFIX 0 C31B 1 0.607847 0.710072 0.611847 -21.000000 0.094690 0.083680 = 0.114470 0.068580 0.038310 0.007500 AFIX 137 H31D 2 0.647268 0.721207 0.626140 -21.000000 -1.500000 H31E 2 0.600216 0.747940 0.596240 -21.000000 -1.500000 H31F 2 0.617687 0.667522 0.599648 -21.000000 -1.500000 PART 0 AFIX 0 C32 1 0.504600 0.754083 0.650136 11.000000 0.178420 0.043350 = 0.084830 0.003410 0.007270 0.023570 AFIX 137 H32A 2 0.506473 0.797052 0.637418 11.000000 -1.500000 H32B 2 0.525127 0.761616 0.671955 11.000000 -1.500000 H32C 2 0.456209 0.739599 0.652657 11.000000 -1.500000 PART 1 21 AFIX 0 C30 1 0.530150 0.686526 0.599474 21.000000 0.153170 0.051420 = 0.054600 0.019670 -0.011850 0.002820 AFIX 137 H30A 2 0.569924 0.662560 0.589726 21.000000 -1.500000 H30B 2 0.522334 0.730085 0.587768 21.000000 -1.500000 H30C 2 0.488791 0.657411 0.597611 21.000000 -1.500000 AFIX 0 C31 1 0.618727 0.728967 0.638091 21.000000 0.068540 0.061800 = 0.154070 0.049010 -0.002620 -0.028830 AFIX 137 H31A 2 0.652263 0.698648 0.627147 21.000000 -1.500000 H31B 2 0.628868 0.730808 0.661763 21.000000 -1.500000 H31C 2 0.621994 0.775471 0.628718 21.000000 -1.500000 PART 0 AFIX 0 Si3 6 0.333899 0.451153 0.688886 11.000000 0.027280 0.031840 = 0.024420 0.001280 0.002810 0.001080 O41 4 0.378469 0.449965 0.656003 11.000000 0.030220 0.033680 = 0.024440 -0.001780 -0.000340 -0.001610 O42 4 0.387403 0.426387 0.718535 11.000000 0.033880 0.046630 = 0.024340 0.003830 0.005640 0.004800 O43 4 0.299928 0.526024 0.697079 11.000000 0.031560 0.028490 = 0.036010 -0.003660 0.004270 0.001850 O44 4 0.269880 0.397087 0.690841 11.000000 0.038120 0.038530 = 0.043710 0.006080 0.002740 -0.005190 C41 1 0.374854 0.408060 0.752588 11.000000 0.049740 0.070880 = 0.025380 0.010180 0.008270 0.014220 C42 1 0.351182 0.333778 0.753908 11.000000 0.161170 0.091730 = 0.060240 0.036020 0.004250 -0.019720 AFIX 137 H42A 2 0.386112 0.304242 0.743474 11.000000 -1.500000 H42B 2 0.307040 0.329105 0.742147 11.000000 -1.500000 H42C 2 0.345040 0.319813 0.776958 11.000000 -1.500000 AFIX 0 C43 1 0.442580 0.411957 0.769656 11.000000 0.075910 0.158060 = 0.042240 0.032720 -0.004160 -0.001440 AFIX 137 H43A 2 0.459422 0.459664 0.769275 11.000000 -1.500000 H43B 2 0.476017 0.381999 0.758420 11.000000 -1.500000 H43C 2 0.437142 0.396789 0.792572 11.000000 -1.500000 AFIX 0 C44 1 0.322242 0.453309 0.768059 11.000000 0.117350 0.122350 = 0.051180 0.013030 0.027030 0.045180 AFIX 137 H44A 2 0.279107 0.451134 0.755327 11.000000 -1.500000 H44B 2 0.339320 0.500933 0.768403 11.000000 -1.500000 H44C 2 0.313473 0.437809 0.790690 11.000000 -1.500000 AFIX 0 C45 1 0.326057 0.595283 0.692745 11.000000 0.040220 0.031680 = 0.031580 -0.008180 0.002330 -0.003450 C46 1 0.398865 0.600752 0.705056 11.000000 0.045970 0.055260 = 0.057660 -0.004200 -0.001430 -0.011950 AFIX 137 H46A 2 0.429323 0.572308 0.691289 11.000000 -1.500000 H46B 2 0.401024 0.584554 0.727935 11.000000 -1.500000 H46C 2 0.414002 0.648979 0.704020 11.000000 -1.500000 AFIX 0 C47 1 0.277992 0.640362 0.712859 11.000000 0.059760 0.039930 = 0.055040 -0.009580 0.011720 0.002620 AFIX 137 H47A 2 0.280333 0.626638 0.736100 11.000000 -1.500000 H47B 2 0.230380 0.634931 0.704830 11.000000 -1.500000 H47C 2 0.292119 0.688726 0.710681 11.000000 -1.500000 AFIX 0 C48 1 0.320701 0.614203 0.656722 11.000000 0.084480 0.040930 = 0.034650 0.004510 0.000190 0.001120 AFIX 137 H48A 2 0.273093 0.606645 0.649089 11.000000 -1.500000 H48B 2 0.352503 0.585361 0.643862 11.000000 -1.500000 H48C 2 0.333028 0.662888 0.653821 11.000000 -1.500000 AFIX 0 C49 1 0.209643 0.386652 0.670935 11.000000 0.038540 0.045890 = 0.039080 -0.006440 0.003640 -0.012050 C50 1 0.225733 0.323540 0.649547 11.000000 0.125980 0.042950 = 0.061580 -0.004540 -0.020820 0.013710 AFIX 137 H50A 2 0.242819 0.285986 0.663549 11.000000 -1.500000 H50B 2 0.261204 0.335602 0.633227 11.000000 -1.500000 H50C 2 0.183475 0.308634 0.638172 11.000000 -1.500000 AFIX 0 C51 1 0.194952 0.446373 0.648729 11.000000 0.056210 0.036400 = 0.107740 0.000970 -0.039680 0.001750 AFIX 137 H51A 2 0.235684 0.455680 0.634980 11.000000 -1.500000 H51B 2 0.184278 0.487209 0.662055 11.000000 -1.500000 H51C 2 0.155253 0.435423 0.634578 11.000000 -1.500000 AFIX 0 C52 1 0.152875 0.369489 0.693588 11.000000 0.061360 0.143920 = 0.086340 -0.016510 0.012260 -0.032590 AFIX 137 H52A 2 0.138866 0.410979 0.705698 11.000000 -1.500000 H52B 2 0.168510 0.334198 0.709224 11.000000 -1.500000 H52C 2 0.113333 0.351829 0.680972 11.000000 -1.500000 AFIX 0 Si4 6 0.296008 0.400702 0.551631 11.000000 0.032620 0.023750 = 0.023560 0.001070 -0.007220 -0.004780 O61 4 0.348651 0.405434 0.581830 11.000000 0.029240 0.028360 = 0.023840 0.005070 -0.004340 -0.004740 O62 4 0.327239 0.362236 0.518967 11.000000 0.041360 0.032330 = 0.027460 -0.004050 -0.003930 -0.003430 O63 4 0.283003 0.475665 0.533559 11.000000 0.051050 0.028110 = 0.031610 0.003950 -0.014500 -0.003740 O64 4 0.224748 0.366968 0.565268 11.000000 0.028130 0.040010 = 0.032720 -0.000490 -0.007040 -0.008160 C61 1 0.356961 0.295709 0.511118 11.000000 0.044440 0.032870 = 0.029860 -0.008160 -0.004910 -0.004530 C62 1 0.308337 0.261554 0.486388 11.000000 0.066560 0.043180 = 0.044450 -0.015990 -0.010720 -0.008930 AFIX 137 H62A 2 0.302255 0.291902 0.467267 11.000000 -1.500000 H62B 2 0.263262 0.253269 0.496817 11.000000 -1.500000 H62C 2 0.328226 0.217530 0.479178 11.000000 -1.500000 AFIX 0 C63 1 0.427250 0.307404 0.494804 11.000000 0.057750 0.049300 = 0.034580 -0.008030 0.004900 0.003240 AFIX 137 H63A 2 0.455780 0.337080 0.508907 11.000000 -1.500000 H63B 2 0.420555 0.329696 0.473339 11.000000 -1.500000 H63C 2 0.450572 0.262951 0.491684 11.000000 -1.500000 AFIX 0 C64 1 0.364985 0.252873 0.542175 11.000000 0.049250 0.031990 = 0.043800 -0.001130 -0.001660 0.003180 AFIX 137 H64A 2 0.319534 0.246580 0.552553 11.000000 -1.500000 H64B 2 0.396100 0.276632 0.557546 11.000000 -1.500000 H64C 2 0.384509 0.207716 0.536504 11.000000 -1.500000 AFIX 0 C65 1 0.257103 0.542833 0.543354 11.000000 0.057840 0.030210 = 0.055160 0.001910 -0.020230 0.004550 C66 1 0.286470 0.564656 0.576022 11.000000 0.075540 0.038110 = 0.043940 -0.003780 -0.006710 0.010080 AFIX 137 H66A 2 0.337188 0.562165 0.575215 11.000000 -1.500000 H66B 2 0.269198 0.533904 0.593365 11.000000 -1.500000 H66C 2 0.272194 0.612146 0.580812 11.000000 -1.500000 AFIX 0 C67 1 0.178897 0.539983 0.545110 11.000000 0.079120 0.058810 = 0.152330 -0.021750 -0.025670 0.024670 AFIX 137 H67A 2 0.164846 0.508955 0.562991 11.000000 -1.500000 H67B 2 0.160481 0.522806 0.524128 11.000000 -1.500000 H67C 2 0.160646 0.586340 0.549349 11.000000 -1.500000 AFIX 0 C68 1 0.281976 0.590761 0.516539 11.000000 0.150260 0.045190 = 0.054080 0.009670 -0.005310 0.007200 AFIX 137 H68A 2 0.266086 0.573734 0.495068 11.000000 -1.500000 H68B 2 0.332748 0.592600 0.516773 11.000000 -1.500000 H68C 2 0.263257 0.637094 0.520353 11.000000 -1.500000 AFIX 0 C69 1 0.160705 0.339938 0.551985 11.000000 0.034600 0.038530 = 0.044460 -0.006630 -0.006980 -0.011330 C70 1 0.163088 0.261959 0.555899 11.000000 0.053220 0.041290 = 0.074350 -0.008560 0.001660 -0.016500 AFIX 137 H70A 2 0.173517 0.250370 0.578902 11.000000 -1.500000 H70B 2 0.199209 0.242940 0.541533 11.000000 -1.500000 H70C 2 0.118075 0.242296 0.549786 11.000000 -1.500000 AFIX 0 C71 1 0.101778 0.368281 0.573118 11.000000 0.032050 0.058370 = 0.065050 -0.012260 -0.005250 -0.004570 AFIX 137 H71A 2 0.100856 0.418721 0.571427 11.000000 -1.500000 H71B 2 0.109063 0.354891 0.596171 11.000000 -1.500000 H71C 2 0.057561 0.349436 0.565330 11.000000 -1.500000 AFIX 0 C72 1 0.151312 0.361176 0.516197 11.000000 0.045270 0.063760 = 0.055870 -0.011120 -0.026510 -0.007490 AFIX 137 H72A 2 0.190035 0.343411 0.503050 11.000000 -1.500000 H72B 2 0.150166 0.411635 0.514671 11.000000 -1.500000 H72C 2 0.107672 0.342185 0.507778 11.000000 -1.500000 PART 1 AFIX 0 C81 1 0.445545 0.029885 0.398774 31.000000 0.089260 0.075260 = 0.121010 0.011240 0.016630 -0.038080 C82 1 0.472790 -0.022556 0.418175 31.000000 0.120750 0.093680 = 0.126990 0.014510 0.008910 -0.052330 AFIX 43 H82 2 0.492505 -0.059806 0.406170 31.000000 -1.200000 AFIX 0 C83 1 0.475643 -0.028808 0.448634 31.000000 0.124260 0.102230 = 0.133000 -0.003670 0.026690 -0.027760 AFIX 43 H83 2 0.498766 -0.065948 0.459262 31.000000 -1.200000 AFIX 0 C84 1 0.440194 0.026163 0.466632 31.000000 0.131370 0.114070 = 0.152360 -0.000260 0.040960 -0.008210 AFIX 43 H84 2 0.436752 0.023616 0.489978 31.000000 -1.200000 AFIX 0 C85 1 0.412607 0.079837 0.450799 31.000000 0.125060 0.106570 = 0.172700 -0.015800 0.036490 -0.025520 AFIX 43 H85 2 0.393852 0.117116 0.463128 31.000000 -1.200000 AFIX 0 C86 1 0.410819 0.082163 0.416085 31.000000 0.102920 0.093710 = 0.161780 -0.004280 0.023070 -0.028710 AFIX 43 H86 2 0.386913 0.117913 0.404782 31.000000 -1.200000 AFIX 0 C87 1 0.445752 0.029776 0.361865 31.000000 0.134560 0.194850 = 0.083550 0.015590 -0.005280 -0.058960 AFIX 137 H87A 2 0.420854 0.070459 0.353748 31.000000 -1.500000 H87B 2 0.422852 -0.012102 0.353806 31.000000 -1.500000 H87C 2 0.493686 0.030901 0.353867 31.000000 -1.500000 PART 2 AFIX 7 C81B 1 0.432725 0.012503 0.440984 -31.000000 0.129980 0.107700 = 0.154900 -0.002590 0.021110 -0.026380 C82B 1 0.386806 0.065475 0.444315 -31.000000 0.128250 0.107280 = 0.164190 -0.009950 0.029510 -0.023390 AFIX 43 H82B 2 0.367968 0.076039 0.465371 -31.000000 -1.200000 AFIX 7 C83B 1 0.367580 0.103944 0.416985 -31.000000 0.114220 0.096310 = 0.171220 -0.002910 0.027490 -0.020490 AFIX 43 H83B 2 0.334250 0.139748 0.419165 -31.000000 -1.200000 AFIX 7 C84B 1 0.397065 0.090165 0.386344 -31.000000 0.108470 0.084190 = 0.151580 0.001160 0.019760 -0.035560 AFIX 43 H84B 2 0.384000 0.116700 0.367645 -31.000000 -1.200000 AFIX 7 C85B 1 0.446389 0.036759 0.383045 -31.000000 0.107420 0.100400 = 0.141490 -0.001440 0.008570 -0.040350 AFIX 43 H85B 2 0.468411 0.028411 0.362467 -31.000000 -1.200000 AFIX 7 C86B 1 0.462042 -0.003156 0.410315 -31.000000 0.114550 0.099090 = 0.140810 0.006340 0.014490 -0.045120 AFIX 43 H86B 2 0.492732 -0.041250 0.408227 -31.000000 -1.200000 AFIX 7 C87B 1 0.474477 -0.012044 0.471534 -31.000000 0.155370 0.136590 = 0.188360 0.001150 0.049810 -0.037660 AFIX 137 H87D 2 0.521912 0.005872 0.470245 -31.000000 -1.500000 H87E 2 0.475661 -0.062594 0.471985 -31.000000 -1.500000 H87F 2 0.452221 0.005090 0.491664 -31.000000 -1.500000 AFIX 0 PART 0 HKLF 4 END ; _cod_data_source_file c6sc00675b2.cif _cod_data_source_block ojc115 _cod_depositor_comments 'Adding full bibliography for 1543284--1543292.cif.' _cod_database_code 1543291 _shelxl_version_number 2013-4 _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_max 0.958 _shelx_estimated_absorpt_t_min 0.542 _olex2_refinement_description ; 1. Others Fixed Uiso: H2A(0.153) H2B(0.153) H2C(0.153) H3A(0.148) H3B(0.148) H3C(0.148) H4A(0.104) H4B(0.104) H4C(0.104) H6A(0.1) H6B(0.1) H6C(0.1) H7A(0.088) H7B(0.088) H7C(0.088) H8A(0.073) H8B(0.073) H8C(0.073) H10A(0.121) H10B(0.121) H10C(0.121) H11A(0.095) H11B(0.095) H11C(0.095) H12A(0.082) H12B(0.082) H12C(0.082) H22A(0.133) H22B(0.133) H22C(0.133) H23A(0.137) H23B(0.137) H23C(0.137) H24A(0.135) H24B(0.135) H24C(0.135) H26A(0.115) H26B(0.115) H26C(0.115) H27A(0.072) H27B(0.072) H27C(0.072) H27D(0.072) H27E(0.072) H27F(0.072) H28A(0.109) H28B(0.109) H28C(0.109) H30D(0.119) H30E(0.119) H30F(0.119) H31D(0.146) H31E(0.146) H31F(0.146) H32A(0.153) H32B(0.153) H32C(0.153) H30A(0.13) H30B(0.13) H30C(0.13) H31A(0.142) H31B(0.142) H31C(0.142) H42A(0.157) H42B(0.157) H42C(0.157) H43A(0.138) H43B(0.138) H43C(0.138) H44A(0.145) H44B(0.145) H44C(0.145) H46A(0.079) H46B(0.079) H46C(0.079) H47A(0.077) H47B(0.077) H47C(0.077) H48A(0.08) H48B(0.08) H48C(0.08) H50A(0.115) H50B(0.115) H50C(0.115) H51A(0.1) H51B(0.1) H51C(0.1) H52A(0.146) H52B(0.146) H52C(0.146) H62A(0.077) H62B(0.077) H62C(0.077) H63A(0.071) H63B(0.071) H63C(0.071) H64A(0.063) H64B(0.063) H64C(0.063) H66A(0.079) H66B(0.079) H66C(0.079) H67A(0.145) H67B(0.145) H67C(0.145) H68A(0.125) H68B(0.125) H68C(0.125) H70A(0.084) H70B(0.084) H70C(0.084) H71A(0.078) H71B(0.078) H71C(0.078) H72A(0.082) H72B(0.082) H72C(0.082) H82(0.137) H83(0.144) H84(0.159) H85(0.162) H86(0.143) H87A(0.206) H87B(0.206) H87C(0.206) H82B(0.16) H83B(0.153) H84B(0.138) H85B(0.14) H86B(0.142) H87D(0.24) H87E(0.24) H87F(0.24) Fixed X: H2A(0.561) H2B(0.6131) H2C(0.6417) H3A(0.6942) H3B(0.6969) H3C(0.7265) H4A(0.6204) H4B(0.5687) H4C(0.6505) H6A(0.7046) H6B(0.6376) H6C(0.6655) H7A(0.6215) H7B(0.6948) H7C(0.6585) H8A(0.522) H8B(0.5166) H8C(0.5548) H10A(0.4611) H10B(0.4336) H10C(0.3796) H11A(0.381) H11B(0.3729) H11C(0.3244) H12A(0.4034) H12B(0.444) H12C(0.3627) H22A(0.5273) H22B(0.5583) H22C(0.5927) H23A(0.668) H23B(0.7128) H23C(0.7038) H24A(0.668) H24B(0.5933) H24C(0.6569) H26A(0.6922) H26B(0.6367) H26C(0.7176) H27A(0.6716) H27B(0.7082) H27C(0.6272) H27D(0.6402) H27E(0.7202) H27F(0.6649) H28A(0.7959) H28B(0.7664) H28C(0.77) H30D(0.4833) H30E(0.4848) H30F(0.4358) H31D(0.6473) H31E(0.6002) H31F(0.6177) H32A(0.5065) H32B(0.5251) H32C(0.4562) H30A(0.5699) H30B(0.5223) H30C(0.4888) H31A(0.6523) H31B(0.6289) H31C(0.622) H42A(0.3861) H42B(0.307) H42C(0.345) H43A(0.4594) H43B(0.476) H43C(0.4371) H44A(0.2791) H44B(0.3393) H44C(0.3135) H46A(0.4293) H46B(0.401) H46C(0.414) H47A(0.2803) H47B(0.2304) H47C(0.2921) H48A(0.2731) H48B(0.3525) H48C(0.333) H50A(0.2428) H50B(0.2612) H50C(0.1835) H51A(0.2357) H51B(0.1843) H51C(0.1553) H52A(0.1389) H52B(0.1685) H52C(0.1133) H62A(0.3023) H62B(0.2633) H62C(0.3282) H63A(0.4558) H63B(0.4206) H63C(0.4506) H64A(0.3195) H64B(0.3961) H64C(0.3845) H66A(0.3372) H66B(0.2692) H66C(0.2722) H67A(0.1648) H67B(0.1605) H67C(0.1606) H68A(0.2661) H68B(0.3327) H68C(0.2633) H70A(0.1735) H70B(0.1992) H70C(0.1181) H71A(0.1009) H71B(0.1091) H71C(0.0576) H72A(0.19) H72B(0.1502) H72C(0.1077) H82(0.4925) H83(0.4988) H84(0.4368) H85(0.3939) H86(0.3869) H87A(0.4209) H87B(0.4229) H87C(0.4937) H82B(0.368) H83B(0.3342) H84B(0.384) H85B(0.4684) H86B(0.4927) H87D(0.5219) H87E(0.4757) H87F(0.4522) Fixed Y: H2A(0.2613) H2B(0.3252) H2C(0.2509) H3A(0.3326) H3B(0.2722) H3C(0.2591) H4A(0.17) H4B(0.1655) H4C(0.1574) H6A(0.2996) H6B(0.3441) H6C(0.2862) H7A(0.1445) H7B(0.183) H7C(0.1582) H8A(0.2831) H8B(0.2042) H8C(0.2235) H10A(0.1142) H10B(0.0905) H10C(0.1079) H11A(0.1745) H11B(0.2536) H11C(0.196) H12A(0.2886) H12B(0.235) H12C(0.2254) H22A(0.5982) H22B(0.6585) H22C(0.6419) H23A(0.6422) H23B(0.5741) H23C(0.6308) H24A(0.4824) H24B(0.4886) H24C(0.5331) H26A(0.5704) H26B(0.509) H26C(0.4923) H27A(0.4435) H27B(0.4104) H27C(0.4283) H27D(0.428) H27E(0.417) H27F(0.4308) H28A(0.507) H28B(0.5283) H28C(0.5843) H30D(0.6416) H30E(0.7221) H30F(0.6946) H31D(0.7212) H31E(0.7479) H31F(0.6675) H32A(0.7971) H32B(0.7616) H32C(0.7396) H30A(0.6626) H30B(0.7301) H30C(0.6574) H31A(0.6986) H31B(0.7308) H31C(0.7755) H42A(0.3042) H42B(0.3291) H42C(0.3198) H43A(0.4597) H43B(0.382) H43C(0.3968) H44A(0.4511) H44B(0.5009) H44C(0.4378) H46A(0.5723) H46B(0.5846) H46C(0.649) H47A(0.6266) H47B(0.6349) H47C(0.6887) H48A(0.6066) H48B(0.5854) H48C(0.6629) H50A(0.286) H50B(0.3356) H50C(0.3086) H51A(0.4557) H51B(0.4872) H51C(0.4354) H52A(0.411) H52B(0.3342) H52C(0.3518) H62A(0.2919) H62B(0.2533) H62C(0.2175) H63A(0.3371) H63B(0.3297) H63C(0.263) H64A(0.2466) H64B(0.2766) H64C(0.2077) H66A(0.5622) H66B(0.5339) H66C(0.6121) H67A(0.509) H67B(0.5228) H67C(0.5863) H68A(0.5737) H68B(0.5926) H68C(0.6371) H70A(0.2504) H70B(0.2429) H70C(0.2423) H71A(0.4187) H71B(0.3549) H71C(0.3494) H72A(0.3434) H72B(0.4116) H72C(0.3422) H82(-0.0598) H83(-0.0659) H84(0.0236) H85(0.1171) H86(0.1179) H87A(0.0705) H87B(-0.0121) H87C(0.0309) H82B(0.076) H83B(0.1397) H84B(0.1167) H85B(0.0284) H86B(-0.0412) H87D(0.0059) H87E(-0.0626) H87F(0.0051) Fixed Z: H2A(0.7335) H2B(0.7307) H2C(0.7412) H3A(0.6843) H3B(0.6574) H3C(0.6938) H4A(0.6634) H4B(0.6942) H4C(0.6997) H6A(0.5747) H6B(0.5654) H6C(0.5405) H7A(0.5956) H7B(0.5943) H7C(0.5608) H8A(0.5619) H8B(0.5733) H8C(0.5394) H10A(0.6776) H10B(0.6421) H10C(0.6709) H11A(0.6051) H11B(0.6157) H11C(0.6321) H12A(0.6735) H12B(0.6965) H12C(0.69) H22A(0.7395) H22B(0.7168) H22C(0.7519) H23A(0.688) H23B(0.6947) H23C(0.7232) H24A(0.7289) H24B(0.7458) H24C(0.7597) H26A(0.5737) H26B(0.5731) H26C(0.5695) H27A(0.6545) H27B(0.6228) H27C(0.6219) H27D(0.6293) H27E(0.6203) H27F(0.5916) H28A(0.6166) H28B(0.6521) H28C(0.6231) H30D(0.597) H30E(0.5882) H30F(0.6172) H31D(0.6261) H31E(0.5962) H31F(0.5996) H32A(0.6374) H32B(0.672) H32C(0.6527) H30A(0.5897) H30B(0.5878) H30C(0.5976) H31A(0.6271) H31B(0.6618) H31C(0.6287) H42A(0.7435) H42B(0.7421) H42C(0.777) H43A(0.7693) H43B(0.7584) H43C(0.7926) H44A(0.7553) H44B(0.7684) H44C(0.7907) H46A(0.6913) H46B(0.7279) H46C(0.704) H47A(0.7361) H47B(0.7048) H47C(0.7107) H48A(0.6491) H48B(0.6439) H48C(0.6538) H50A(0.6635) H50B(0.6332) H50C(0.6382) H51A(0.635) H51B(0.6621) H51C(0.6346) H52A(0.7057) H52B(0.7092) H52C(0.681) H62A(0.4673) H62B(0.4968) H62C(0.4792) H63A(0.5089) H63B(0.4733) H63C(0.4917) H64A(0.5526) H64B(0.5575) H64C(0.5365) H66A(0.5752) H66B(0.5934) H66C(0.5808) H67A(0.563) H67B(0.5241) H67C(0.5493) H68A(0.4951) H68B(0.5168) H68C(0.5204) H70A(0.5789) H70B(0.5415) H70C(0.5498) H71A(0.5714) H71B(0.5962) H71C(0.5653) H72A(0.5031) H72B(0.5147) H72C(0.5078) H82(0.4062) H83(0.4593) H84(0.49) H85(0.4631) H86(0.4048) H87A(0.3537) H87B(0.3538) H87C(0.3539) H82B(0.4654) H83B(0.4192) H84B(0.3676) H85B(0.3625) H86B(0.4082) H87D(0.4702) H87E(0.472) H87F(0.4917) ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -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 0.44006(2) 0.44226(2) 0.60937(2) 0.02120(4) Uani 1 1 d . . . . . K1 K 0.51200(5) 0.41677(5) 0.69093(2) 0.0293(2) Uani 1 1 d . . . . . K2 K 0.40123(7) 0.47171(7) 0.49467(3) 0.0455(3) Uani 1 1 d . . . . . S1 S 0.47402(8) 0.52951(7) 0.55726(3) 0.0373(3) Uani 1 1 d . . . . . S2 S 0.51727(7) 0.43028(6) 0.55255(3) 0.0356(3) Uani 1 1 d . . . . . Si1 Si 0.53531(7) 0.28108(7) 0.63679(3) 0.0289(3) Uani 1 1 d . . . . . O1 O 0.48968(16) 0.34821(16) 0.62885(7) 0.0275(7) Uani 1 1 d . . . . . O2 O 0.56734(19) 0.29553(18) 0.67362(8) 0.0404(9) Uani 1 1 d . . . . . O3 O 0.60208(18) 0.26896(18) 0.61352(9) 0.0387(8) Uani 1 1 d . . . . . O4 O 0.49083(19) 0.21003(17) 0.63666(9) 0.0377(8) Uani 1 1 d . . . . . C1 C 0.6208(4) 0.2582(3) 0.69178(15) 0.0565(18) Uani 1 1 d . . . . . C2 C 0.6080(5) 0.2754(5) 0.72741(18) 0.102(3) Uani 1 1 d . U . . . H2A H 0.5610 0.2613 0.7335 0.153 Uiso 1 1 calc R U . . . H2B H 0.6131 0.3252 0.7307 0.153 Uiso 1 1 calc R U . . . H2C H 0.6417 0.2509 0.7412 0.153 Uiso 1 1 calc R U . . . C3 C 0.6906(4) 0.2826(5) 0.6809(2) 0.099(3) Uani 1 1 d . . . . . H3A H 0.6942 0.3326 0.6843 0.148 Uiso 1 1 calc R U . . . H3B H 0.6969 0.2722 0.6574 0.148 Uiso 1 1 calc R U . . . H3C H 0.7265 0.2591 0.6938 0.148 Uiso 1 1 calc R U . . . C4 C 0.6145(4) 0.1810(3) 0.68681(17) 0.069(2) Uani 1 1 d . . . . . H4A H 0.6204 0.1700 0.6634 0.104 Uiso 1 1 calc R U . . . H4B H 0.5687 0.1655 0.6942 0.104 Uiso 1 1 calc R U . . . H4C H 0.6505 0.1574 0.6997 0.104 Uiso 1 1 calc R U . . . C5 C 0.6136(3) 0.2454(3) 0.58037(13) 0.0412(13) Uani 1 1 d . . . . . C6 C 0.6594(4) 0.2985(4) 0.56378(17) 0.067(2) Uani 1 1 d . . . . . H6A H 0.7046 0.2996 0.5747 0.100 Uiso 1 1 calc R U . . . H6B H 0.6376 0.3441 0.5654 0.100 Uiso 1 1 calc R U . . . H6C H 0.6655 0.2862 0.5405 0.100 Uiso 1 1 calc R U . . . C7 C 0.6503(3) 0.1767(3) 0.58300(16) 0.0588(18) Uani 1 1 d . . . . . H7A H 0.6215 0.1445 0.5956 0.088 Uiso 1 1 calc R U . . . H7B H 0.6948 0.1830 0.5943 0.088 Uiso 1 1 calc R U . . . H7C H 0.6585 0.1582 0.5608 0.088 Uiso 1 1 calc R U . . . C8 C 0.5458(3) 0.2385(3) 0.56214(14) 0.0485(15) Uani 1 1 d . . . . . H8A H 0.5220 0.2831 0.5619 0.073 Uiso 1 1 calc R U . . . H8B H 0.5166 0.2042 0.5733 0.073 Uiso 1 1 calc R U . . . H8C H 0.5548 0.2235 0.5394 0.073 Uiso 1 1 calc R U . . . C9 C 0.4226(3) 0.1955(3) 0.65002(14) 0.0430(14) Uani 1 1 d . . . . . C10 C 0.4244(4) 0.1203(3) 0.6611(2) 0.081(3) Uani 1 1 d . . . . . H10A H 0.4611 0.1142 0.6776 0.121 Uiso 1 1 calc R U . . . H10B H 0.4336 0.0905 0.6421 0.121 Uiso 1 1 calc R U . . . H10C H 0.3796 0.1079 0.6709 0.121 Uiso 1 1 calc R U . . . C11 C 0.3708(3) 0.2058(4) 0.62349(17) 0.0635(19) Uani 1 1 d . . . . . H11A H 0.3810 0.1745 0.6051 0.095 Uiso 1 1 calc R U . . . H11B H 0.3729 0.2536 0.6157 0.095 Uiso 1 1 calc R U . . . H11C H 0.3244 0.1960 0.6321 0.095 Uiso 1 1 calc R U . . . C12 C 0.4068(3) 0.2402(3) 0.68024(15) 0.0548(16) Uani 1 1 d . . . . . H12A H 0.4034 0.2886 0.6735 0.082 Uiso 1 1 calc R U . . . H12B H 0.4440 0.2350 0.6965 0.082 Uiso 1 1 calc R U . . . H12C H 0.3627 0.2254 0.6900 0.082 Uiso 1 1 calc R U . . . Si2 Si 0.56948(7) 0.56137(7) 0.65102(3) 0.0302(3) Uani 1 1 d . . . . . O21 O 0.51596(17) 0.50526(16) 0.63729(7) 0.0293(7) Uani 1 1 d . . . . . O22 O 0.58075(18) 0.53753(18) 0.68971(8) 0.0373(8) Uani 1 1 d . . . . . O23 O 0.64263(18) 0.56520(18) 0.63165(9) 0.0411(9) Uani 1 1 d . . . . . O24 O 0.54115(19) 0.63963(18) 0.65310(9) 0.0401(9) Uani 1 1 d . . . . . C21 C 0.6171(3) 0.5714(3) 0.71657(14) 0.0490(15) Uani 1 1 d . . . . . C22 C 0.5698(4) 0.6218(5) 0.73254(19) 0.089(3) Uani 1 1 d . . . . . H22A H 0.5273 0.5982 0.7395 0.133 Uiso 1 1 calc R U . . . H22B H 0.5583 0.6585 0.7168 0.133 Uiso 1 1 calc R U . . . H22C H 0.5927 0.6419 0.7519 0.133 Uiso 1 1 calc R U . . . C23 C 0.6809(4) 0.6078(5) 0.70457(18) 0.092(3) Uani 1 1 d . U . . . H23A H 0.6680 0.6422 0.6880 0.137 Uiso 1 1 calc R U . . . H23B H 0.7128 0.5741 0.6947 0.137 Uiso 1 1 calc R U . . . H23C H 0.7038 0.6308 0.7232 0.137 Uiso 1 1 calc R U . . . C24 C 0.6354(4) 0.5139(4) 0.73975(18) 0.090(3) Uani 1 1 d . . . . . H24A H 0.6680 0.4824 0.7289 0.135 Uiso 1 1 calc R U . . . H24B H 0.5933 0.4886 0.7458 0.135 Uiso 1 1 calc R U . . . H24C H 0.6569 0.5331 0.7597 0.135 Uiso 1 1 calc R U . . . C25 C 0.6895(3) 0.5154(3) 0.61738(15) 0.0484(15) Uani 1 1 d . . . . . C26 C 0.6835(4) 0.5224(4) 0.58010(17) 0.077(2) Uani 1 1 d . . . A 1 H26A H 0.6922 0.5704 0.5737 0.115 Uiso 1 1 calc R U . A 1 H26B H 0.6367 0.5090 0.5731 0.115 Uiso 1 1 calc R U . A 1 H26C H 0.7176 0.4923 0.5695 0.115 Uiso 1 1 calc R U . A 1 C27 C 0.6726(5) 0.4429(5) 0.6303(5) 0.048(3) Uani 0.77(3) 1 d . . P A 1 H27A H 0.6716 0.4435 0.6545 0.072 Uiso 0.77(3) 1 calc R U P A 1 H27B H 0.7082 0.4104 0.6228 0.072 Uiso 0.77(3) 1 calc R U P A 1 H27C H 0.6272 0.4283 0.6219 0.072 Uiso 0.77(3) 1 calc R U P A 1 C27B C 0.678(2) 0.442(2) 0.6144(14) 0.048(3) Uani 0.23(3) 1 d . . P A 2 H27D H 0.6402 0.4280 0.6293 0.072 Uiso 0.23(3) 1 calc R U P A 2 H27E H 0.7202 0.4170 0.6203 0.072 Uiso 0.23(3) 1 calc R U P A 2 H27F H 0.6649 0.4308 0.5916 0.072 Uiso 0.23(3) 1 calc R U P A 2 C28 C 0.7618(3) 0.5355(4) 0.6283(2) 0.072(2) Uani 1 1 d . . . . . H28A H 0.7959 0.5070 0.6166 0.109 Uiso 1 1 calc R U . . . H28B H 0.7664 0.5283 0.6521 0.109 Uiso 1 1 calc R U . . . H28C H 0.7700 0.5843 0.6231 0.109 Uiso 1 1 calc R U . . . C29 C 0.5436(3) 0.7001(3) 0.63272(16) 0.0498(15) Uani 1 1 d . . . . . C30B C 0.4805(17) 0.6884(12) 0.6061(7) 0.080(8) Uani 0.37(2) 1 d . U P B 2 H30D H 0.4833 0.6416 0.5970 0.119 Uiso 0.37(2) 1 calc R U P B 2 H30E H 0.4848 0.7221 0.5882 0.119 Uiso 0.37(2) 1 calc R U P B 2 H30F H 0.4358 0.6946 0.6172 0.119 Uiso 0.37(2) 1 calc R U P B 2 C31B C 0.6078(16) 0.7101(16) 0.6118(9) 0.098(9) Uani 0.37(2) 1 d . U P B 2 H31D H 0.6473 0.7212 0.6261 0.146 Uiso 0.37(2) 1 calc R U P B 2 H31E H 0.6002 0.7479 0.5962 0.146 Uiso 0.37(2) 1 calc R U P B 2 H31F H 0.6177 0.6675 0.5996 0.146 Uiso 0.37(2) 1 calc R U P B 2 C32 C 0.5046(6) 0.7541(4) 0.6501(2) 0.102(3) Uani 1 1 d . . . . . H32A H 0.5065 0.7971 0.6374 0.153 Uiso 1 1 calc R U . . . H32B H 0.5251 0.7616 0.6720 0.153 Uiso 1 1 calc R U . . . H32C H 0.4562 0.7396 0.6527 0.153 Uiso 1 1 calc R U . . . C30 C 0.5301(13) 0.6865(7) 0.5995(3) 0.086(5) Uani 0.63(2) 1 d . U P B 1 H30A H 0.5699 0.6626 0.5897 0.130 Uiso 0.63(2) 1 calc R U P B 1 H30B H 0.5223 0.7301 0.5878 0.130 Uiso 0.63(2) 1 calc R U P B 1 H30C H 0.4888 0.6574 0.5976 0.130 Uiso 0.63(2) 1 calc R U P B 1 C31 C 0.6187(7) 0.7290(8) 0.6381(6) 0.095(6) Uani 0.63(2) 1 d . U P B 1 H31A H 0.6523 0.6986 0.6271 0.142 Uiso 0.63(2) 1 calc R U P B 1 H31B H 0.6289 0.7308 0.6618 0.142 Uiso 0.63(2) 1 calc R U P B 1 H31C H 0.6220 0.7755 0.6287 0.142 Uiso 0.63(2) 1 calc R U P B 1 Si3 Si 0.33390(7) 0.45115(7) 0.68889(3) 0.0278(3) Uani 1 1 d . . . . . O41 O 0.37847(16) 0.44996(16) 0.65600(8) 0.0294(7) Uani 1 1 d . . . . . O42 O 0.38740(17) 0.42639(18) 0.71853(8) 0.0350(8) Uani 1 1 d . . . . . O43 O 0.29993(17) 0.52602(16) 0.69708(8) 0.0320(8) Uani 1 1 d . . . . . O44 O 0.26988(19) 0.39709(18) 0.69084(9) 0.0401(9) Uani 1 1 d . . . . . C41 C 0.3749(3) 0.4081(3) 0.75259(13) 0.0487(15) Uani 1 1 d . . . . . C42 C 0.3512(6) 0.3338(4) 0.7539(2) 0.104(3) Uani 1 1 d . . . . . H42A H 0.3861 0.3042 0.7435 0.157 Uiso 1 1 calc R U . . . H42B H 0.3070 0.3291 0.7421 0.157 Uiso 1 1 calc R U . . . H42C H 0.3450 0.3198 0.7770 0.157 Uiso 1 1 calc R U . . . C43 C 0.4426(4) 0.4120(5) 0.76966(17) 0.092(3) Uani 1 1 d . U . . . H43A H 0.4594 0.4597 0.7693 0.138 Uiso 1 1 calc R U . . . H43B H 0.4760 0.3820 0.7584 0.138 Uiso 1 1 calc R U . . . H43C H 0.4371 0.3968 0.7926 0.138 Uiso 1 1 calc R U . . . C44 C 0.3222(5) 0.4533(5) 0.76806(18) 0.097(3) Uani 1 1 d . U . . . H44A H 0.2791 0.4511 0.7553 0.145 Uiso 1 1 calc R U . . . H44B H 0.3393 0.5009 0.7684 0.145 Uiso 1 1 calc R U . . . H44C H 0.3135 0.4378 0.7907 0.145 Uiso 1 1 calc R U . . . C45 C 0.3261(3) 0.5953(2) 0.69274(12) 0.0345(11) Uani 1 1 d . . . . . C46 C 0.3989(3) 0.6008(3) 0.70506(16) 0.0530(16) Uani 1 1 d . . . . . H46A H 0.4293 0.5723 0.6913 0.079 Uiso 1 1 calc R U . . . H46B H 0.4010 0.5846 0.7279 0.079 Uiso 1 1 calc R U . . . H46C H 0.4140 0.6490 0.7040 0.079 Uiso 1 1 calc R U . . . C47 C 0.2780(3) 0.6404(3) 0.71286(15) 0.0516(16) Uani 1 1 d . . . . . H47A H 0.2803 0.6266 0.7361 0.077 Uiso 1 1 calc R U . . . H47B H 0.2304 0.6349 0.7048 0.077 Uiso 1 1 calc R U . . . H47C H 0.2921 0.6887 0.7107 0.077 Uiso 1 1 calc R U . . . C48 C 0.3207(4) 0.6142(3) 0.65672(13) 0.0534(16) Uani 1 1 d . . . . . H48A H 0.2731 0.6066 0.6491 0.080 Uiso 1 1 calc R U . . . H48B H 0.3525 0.5854 0.6439 0.080 Uiso 1 1 calc R U . . . H48C H 0.3330 0.6629 0.6538 0.080 Uiso 1 1 calc R U . . . C49 C 0.2096(3) 0.3867(3) 0.67094(14) 0.0412(13) Uani 1 1 d . . . . . C50 C 0.2257(4) 0.3235(3) 0.64955(17) 0.077(2) Uani 1 1 d . . . . . H50A H 0.2428 0.2860 0.6635 0.115 Uiso 1 1 calc R U . . . H50B H 0.2612 0.3356 0.6332 0.115 Uiso 1 1 calc R U . . . H50C H 0.1835 0.3086 0.6382 0.115 Uiso 1 1 calc R U . . . C51 C 0.1950(3) 0.4464(3) 0.64873(19) 0.067(2) Uani 1 1 d . . . . . H51A H 0.2357 0.4557 0.6350 0.100 Uiso 1 1 calc R U . . . H51B H 0.1843 0.4872 0.6621 0.100 Uiso 1 1 calc R U . . . H51C H 0.1553 0.4354 0.6346 0.100 Uiso 1 1 calc R U . . . C52 C 0.1529(4) 0.3695(5) 0.6936(2) 0.097(3) Uani 1 1 d . U . . . H52A H 0.1389 0.4110 0.7057 0.146 Uiso 1 1 calc R U . . . H52B H 0.1685 0.3342 0.7092 0.146 Uiso 1 1 calc R U . . . H52C H 0.1133 0.3518 0.6810 0.146 Uiso 1 1 calc R U . . . Si4 Si 0.29601(7) 0.40070(6) 0.55163(3) 0.0266(3) Uani 1 1 d . . . . . O61 O 0.34865(16) 0.40543(15) 0.58183(7) 0.0271(7) Uani 1 1 d . . . . . O62 O 0.32724(18) 0.36224(16) 0.51897(8) 0.0337(8) Uani 1 1 d . . . . . O63 O 0.28300(19) 0.47567(17) 0.53356(8) 0.0369(8) Uani 1 1 d . . . . . O64 O 0.22475(17) 0.36697(17) 0.56527(8) 0.0336(8) Uani 1 1 d . . . . . C61 C 0.3570(3) 0.2957(3) 0.51112(12) 0.0357(12) Uani 1 1 d . . . . . C62 C 0.3083(3) 0.2616(3) 0.48639(14) 0.0514(16) Uani 1 1 d . . . . . H62A H 0.3023 0.2919 0.4673 0.077 Uiso 1 1 calc R U . . . H62B H 0.2633 0.2533 0.4968 0.077 Uiso 1 1 calc R U . . . H62C H 0.3282 0.2175 0.4792 0.077 Uiso 1 1 calc R U . . . C63 C 0.4272(3) 0.3074(3) 0.49480(14) 0.0472(15) Uani 1 1 d . . . . . H63A H 0.4558 0.3371 0.5089 0.071 Uiso 1 1 calc R U . . . H63B H 0.4206 0.3297 0.4733 0.071 Uiso 1 1 calc R U . . . H63C H 0.4506 0.2630 0.4917 0.071 Uiso 1 1 calc R U . . . C64 C 0.3650(3) 0.2529(3) 0.54218(13) 0.0417(13) Uani 1 1 d . . . . . H64A H 0.3195 0.2466 0.5526 0.063 Uiso 1 1 calc R U . . . H64B H 0.3961 0.2766 0.5575 0.063 Uiso 1 1 calc R U . . . H64C H 0.3845 0.2077 0.5365 0.063 Uiso 1 1 calc R U . . . C65 C 0.2571(3) 0.5428(3) 0.54335(15) 0.0477(15) Uani 1 1 d . . . . . C66 C 0.2865(3) 0.5647(3) 0.57602(14) 0.0525(16) Uani 1 1 d . . . . . H66A H 0.3372 0.5622 0.5752 0.079 Uiso 1 1 calc R U . . . H66B H 0.2692 0.5339 0.5934 0.079 Uiso 1 1 calc R U . . . H66C H 0.2722 0.6121 0.5808 0.079 Uiso 1 1 calc R U . . . C67 C 0.1789(4) 0.5400(4) 0.5451(2) 0.097(3) Uani 1 1 d . U . . . H67A H 0.1648 0.5090 0.5630 0.145 Uiso 1 1 calc R U . . . H67B H 0.1605 0.5228 0.5241 0.145 Uiso 1 1 calc R U . . . H67C H 0.1606 0.5863 0.5493 0.145 Uiso 1 1 calc R U . . . C68 C 0.2820(5) 0.5908(3) 0.51654(17) 0.083(2) Uani 1 1 d . U . . . H68A H 0.2661 0.5737 0.4951 0.125 Uiso 1 1 calc R U . . . H68B H 0.3327 0.5926 0.5168 0.125 Uiso 1 1 calc R U . . . H68C H 0.2633 0.6371 0.5204 0.125 Uiso 1 1 calc R U . . . C69 C 0.1607(3) 0.3399(3) 0.55199(14) 0.0392(13) Uani 1 1 d . . . . . C70 C 0.1631(3) 0.2620(3) 0.55590(17) 0.0563(17) Uani 1 1 d . . . . . H70A H 0.1735 0.2504 0.5789 0.084 Uiso 1 1 calc R U . . . H70B H 0.1992 0.2429 0.5415 0.084 Uiso 1 1 calc R U . . . H70C H 0.1181 0.2423 0.5498 0.084 Uiso 1 1 calc R U . . . C71 C 0.1018(3) 0.3683(3) 0.57312(16) 0.0518(16) Uani 1 1 d . . . . . H71A H 0.1009 0.4187 0.5714 0.078 Uiso 1 1 calc R U . . . H71B H 0.1091 0.3549 0.5962 0.078 Uiso 1 1 calc R U . . . H71C H 0.0576 0.3494 0.5653 0.078 Uiso 1 1 calc R U . . . C72 C 0.1513(3) 0.3612(3) 0.51620(15) 0.0550(17) Uani 1 1 d . . . . . H72A H 0.1900 0.3434 0.5031 0.082 Uiso 1 1 calc R U . . . H72B H 0.1502 0.4116 0.5147 0.082 Uiso 1 1 calc R U . . . H72C H 0.1077 0.3422 0.5078 0.082 Uiso 1 1 calc R U . . . C81 C 0.4455(8) 0.0299(8) 0.3988(4) 0.095(4) Uani 0.700(11) 1 d . U P C 1 C82 C 0.4728(9) -0.0226(9) 0.4182(5) 0.114(4) Uani 0.700(11) 1 d . U P C 1 H82 H 0.4925 -0.0598 0.4062 0.137 Uiso 0.700(11) 1 calc R U P C 1 C83 C 0.4756(9) -0.0288(9) 0.4486(5) 0.120(5) Uani 0.700(11) 1 d . U P C 1 H83 H 0.4988 -0.0659 0.4593 0.144 Uiso 0.700(11) 1 calc R U P C 1 C84 C 0.4402(9) 0.0262(10) 0.4666(5) 0.133(5) Uani 0.700(11) 1 d . U P C 1 H84 H 0.4368 0.0236 0.4900 0.159 Uiso 0.700(11) 1 calc R U P C 1 C85 C 0.4126(10) 0.0798(10) 0.4508(5) 0.135(5) Uani 0.700(11) 1 d . U P C 1 H85 H 0.3939 0.1171 0.4631 0.162 Uiso 0.700(11) 1 calc R U P C 1 C86 C 0.4108(9) 0.0822(9) 0.4161(5) 0.119(5) Uani 0.700(11) 1 d . U P C 1 H86 H 0.3869 0.1179 0.4048 0.143 Uiso 0.700(11) 1 calc R U P C 1 C87 C 0.4458(6) 0.0298(7) 0.3619(3) 0.138(6) Uani 0.700(11) 1 d . U P C 1 H87A H 0.4209 0.0705 0.3537 0.206 Uiso 0.700(11) 1 calc R U P C 1 H87B H 0.4229 -0.0121 0.3538 0.206 Uiso 0.700(11) 1 calc R U P C 1 H87C H 0.4937 0.0309 0.3539 0.206 Uiso 0.700(11) 1 calc R U P C 1 C81B C 0.4327(11) 0.0125(8) 0.4410(3) 0.131(5) Uani 0.300(11) 1 d R U P C 2 C82B C 0.3868(7) 0.0655(9) 0.4443(3) 0.133(6) Uani 0.300(11) 1 d DR U P C 2 H82B H 0.3680 0.0760 0.4654 0.160 Uiso 0.300(11) 1 calc R U P C 2 C83B C 0.3676(8) 0.1039(9) 0.4170(3) 0.127(6) Uani 0.300(11) 1 d R U P C 2 H83B H 0.3342 0.1397 0.4192 0.153 Uiso 0.300(11) 1 calc R U P C 2 C84B C 0.3971(9) 0.0902(8) 0.3863(3) 0.115(6) Uani 0.300(11) 1 d R U P C 2 H84B H 0.3840 0.1167 0.3676 0.138 Uiso 0.300(11) 1 calc R U P C 2 C85B C 0.4464(10) 0.0368(7) 0.3830(3) 0.116(7) Uani 0.300(11) 1 d R U P C 2 H85B H 0.4684 0.0284 0.3625 0.140 Uiso 0.300(11) 1 calc R U P C 2 C86B C 0.4620(12) -0.0032(9) 0.4103(3) 0.118(6) Uani 0.300(11) 1 d DR U P C 2 H86B H 0.4927 -0.0412 0.4082 0.142 Uiso 0.300(11) 1 calc R U P C 2 C87B C 0.4745(11) -0.0120(10) 0.4715(3) 0.160(12) Uani 0.300(11) 1 d DR U P C 2 H87D H 0.5219 0.0059 0.4702 0.240 Uiso 0.300(11) 1 calc R U P C 2 H87E H 0.4757 -0.0626 0.4720 0.240 Uiso 0.300(11) 1 calc R U P C 2 H87F H 0.4522 0.0051 0.4917 0.240 Uiso 0.300(11) 1 calc R U P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02371(8) 0.02400(7) 0.01589(7) 0.00176(7) -0.00239(7) -0.00178(7) K1 0.0312(5) 0.0353(5) 0.0214(5) 0.0022(4) -0.0014(4) 0.0025(4) K2 0.0594(8) 0.0494(7) 0.0278(6) 0.0085(5) 0.0024(6) -0.0156(6) S1 0.0523(8) 0.0334(6) 0.0262(6) 0.0079(5) 0.0010(6) -0.0036(6) S2 0.0448(8) 0.0362(7) 0.0259(6) 0.0032(5) 0.0078(6) 0.0002(6) Si1 0.0320(7) 0.0324(7) 0.0223(7) 0.0023(5) 0.0012(6) 0.0072(6) O1 0.0289(17) 0.0317(17) 0.0218(17) 0.0027(13) -0.0004(14) 0.0030(14) O2 0.054(2) 0.0401(19) 0.0271(18) 0.0006(15) -0.0090(17) 0.0223(18) O3 0.0319(19) 0.047(2) 0.037(2) -0.0043(17) 0.0057(17) 0.0061(16) O4 0.047(2) 0.0303(18) 0.036(2) 0.0010(15) 0.0098(17) 0.0038(16) C1 0.068(5) 0.061(4) 0.041(4) 0.002(3) -0.019(3) 0.036(3) C2 0.139(7) 0.113(6) 0.054(4) -0.001(4) -0.040(5) 0.066(5) C3 0.067(6) 0.100(7) 0.129(8) 0.026(6) -0.053(5) 0.006(5) C4 0.076(5) 0.058(4) 0.073(5) 0.015(3) -0.026(4) 0.035(4) C5 0.044(3) 0.044(3) 0.036(3) 0.000(2) 0.014(3) 0.019(3) C6 0.062(4) 0.070(5) 0.068(5) 0.010(4) 0.028(4) 0.011(4) C7 0.062(4) 0.055(4) 0.059(4) -0.005(3) 0.002(3) 0.028(3) C8 0.057(4) 0.057(4) 0.032(3) -0.002(3) 0.002(3) 0.018(3) C9 0.052(4) 0.032(3) 0.045(3) 0.005(2) 0.014(3) -0.004(2) C10 0.105(6) 0.046(4) 0.091(6) 0.021(4) 0.039(5) -0.007(4) C11 0.056(4) 0.072(5) 0.063(5) 0.001(4) 0.011(4) -0.017(4) C12 0.060(4) 0.057(4) 0.047(4) 0.005(3) 0.020(3) 0.001(3) Si2 0.0301(7) 0.0344(7) 0.0262(7) 0.0005(6) -0.0051(5) -0.0093(6) O21 0.0324(18) 0.0347(17) 0.0209(17) -0.0009(13) -0.0041(14) -0.0095(15) O22 0.039(2) 0.046(2) 0.0277(19) -0.0033(15) -0.0119(16) -0.0086(16) O23 0.0328(19) 0.043(2) 0.047(2) 0.0036(17) 0.0014(17) -0.0131(17) O24 0.046(2) 0.0368(19) 0.037(2) 0.0002(16) -0.0041(17) -0.0076(17) C21 0.047(3) 0.063(4) 0.037(3) 0.000(3) -0.022(3) -0.016(3) C22 0.089(6) 0.114(7) 0.063(5) -0.052(5) -0.029(4) 0.000(5) C23 0.086(5) 0.131(6) 0.058(4) -0.002(4) -0.019(4) -0.059(5) C24 0.101(6) 0.107(6) 0.061(5) 0.012(4) -0.053(5) -0.029(5) C25 0.028(3) 0.060(4) 0.057(4) -0.002(3) 0.006(3) -0.005(3) C26 0.068(5) 0.104(6) 0.057(5) -0.011(4) 0.019(4) -0.008(5) C27 0.038(4) 0.031(3) 0.075(9) -0.001(6) 0.013(6) 0.007(3) C27B 0.038(4) 0.031(3) 0.075(9) -0.001(6) 0.013(6) 0.007(3) C28 0.033(3) 0.088(5) 0.096(6) 0.002(4) 0.002(4) -0.009(4) C29 0.062(4) 0.034(3) 0.054(4) 0.004(3) 0.008(3) -0.005(3) C30B 0.096(14) 0.043(9) 0.100(14) 0.022(9) -0.046(12) -0.036(11) C31B 0.095(17) 0.084(15) 0.114(19) 0.069(15) 0.038(17) 0.007(13) C32 0.178(10) 0.043(4) 0.085(6) 0.003(4) 0.007(6) 0.024(5) C30 0.153(14) 0.051(6) 0.055(7) 0.020(5) -0.012(9) 0.003(9) C31 0.069(9) 0.062(8) 0.154(17) 0.049(11) -0.003(11) -0.029(7) Si3 0.0273(7) 0.0318(7) 0.0244(7) 0.0013(5) 0.0028(5) 0.0011(6) O41 0.0302(17) 0.0337(18) 0.0244(17) -0.0018(14) -0.0003(14) -0.0016(15) O42 0.0339(19) 0.047(2) 0.0243(18) 0.0038(15) 0.0056(15) 0.0048(16) O43 0.0316(19) 0.0285(16) 0.036(2) -0.0037(14) 0.0043(15) 0.0018(15) O44 0.038(2) 0.0385(19) 0.044(2) 0.0061(16) 0.0027(17) -0.0052(17) C41 0.050(4) 0.071(4) 0.025(3) 0.010(3) 0.008(3) 0.014(3) C42 0.161(9) 0.092(6) 0.060(5) 0.036(5) 0.004(6) -0.020(6) C43 0.076(5) 0.158(7) 0.042(4) 0.033(4) -0.004(4) -0.001(5) C44 0.117(6) 0.122(6) 0.051(4) 0.013(4) 0.027(4) 0.045(5) C45 0.040(3) 0.032(3) 0.032(3) -0.008(2) 0.002(2) -0.003(2) C46 0.046(4) 0.055(4) 0.058(4) -0.004(3) -0.001(3) -0.012(3) C47 0.060(4) 0.040(3) 0.055(4) -0.010(3) 0.012(3) 0.003(3) C48 0.084(5) 0.041(3) 0.035(3) 0.005(2) 0.000(3) 0.001(3) C49 0.039(3) 0.046(3) 0.039(3) -0.006(2) 0.004(3) -0.012(3) C50 0.126(7) 0.043(4) 0.062(5) -0.005(3) -0.021(5) 0.014(4) C51 0.056(4) 0.036(3) 0.108(6) 0.001(4) -0.040(4) 0.002(3) C52 0.061(5) 0.144(7) 0.086(5) -0.017(5) 0.012(4) -0.033(5) Si4 0.0326(7) 0.0237(6) 0.0236(7) 0.0011(5) -0.0072(6) -0.0048(5) O61 0.0292(18) 0.0284(16) 0.0238(17) 0.0051(13) -0.0043(14) -0.0047(14) O62 0.041(2) 0.0323(17) 0.0275(18) -0.0041(14) -0.0039(16) -0.0034(16) O63 0.051(2) 0.0281(17) 0.0316(19) 0.0040(14) -0.0145(17) -0.0037(16) O64 0.0281(18) 0.0400(19) 0.0327(19) -0.0005(15) -0.0070(15) -0.0082(15) C61 0.044(3) 0.033(3) 0.030(3) -0.008(2) -0.005(2) -0.005(2) C62 0.067(4) 0.043(3) 0.044(3) -0.016(3) -0.011(3) -0.009(3) C63 0.058(4) 0.049(3) 0.035(3) -0.008(2) 0.005(3) 0.003(3) C64 0.049(3) 0.032(3) 0.044(3) -0.001(2) -0.002(3) 0.003(3) C65 0.058(4) 0.030(3) 0.055(4) 0.002(2) -0.020(3) 0.005(3) C66 0.076(4) 0.038(3) 0.044(3) -0.004(3) -0.007(3) 0.010(3) C67 0.079(5) 0.059(4) 0.152(7) -0.022(4) -0.026(5) 0.025(4) C68 0.150(7) 0.045(4) 0.054(4) 0.010(3) -0.005(4) 0.007(4) C69 0.035(3) 0.039(3) 0.044(3) -0.007(2) -0.007(2) -0.011(2) C70 0.053(4) 0.041(3) 0.074(5) -0.009(3) 0.002(3) -0.016(3) C71 0.032(3) 0.058(4) 0.065(4) -0.012(3) -0.005(3) -0.005(3) C72 0.045(4) 0.064(4) 0.056(4) -0.011(3) -0.027(3) -0.007(3) C81 0.089(7) 0.075(6) 0.121(9) 0.011(7) 0.017(7) -0.038(6) C82 0.121(9) 0.094(8) 0.127(10) 0.015(8) 0.009(8) -0.052(7) C83 0.124(9) 0.102(8) 0.133(10) -0.004(9) 0.027(9) -0.028(7) C84 0.131(10) 0.114(9) 0.152(11) 0.000(9) 0.041(9) -0.008(8) C85 0.125(9) 0.107(8) 0.173(11) -0.016(9) 0.036(9) -0.026(8) C86 0.103(9) 0.094(8) 0.162(10) -0.004(9) 0.023(9) -0.029(7) C87 0.135(13) 0.195(15) 0.084(11) 0.016(11) -0.005(10) -0.059(11) C81B 0.130(10) 0.108(10) 0.155(11) -0.003(10) 0.021(10) -0.026(9) C82B 0.128(11) 0.107(10) 0.164(12) -0.010(10) 0.030(11) -0.023(10) C83B 0.114(12) 0.096(11) 0.171(13) -0.003(11) 0.027(12) -0.020(11) C84B 0.108(11) 0.084(10) 0.152(13) 0.001(11) 0.020(12) -0.036(10) C85B 0.107(11) 0.100(11) 0.141(14) -0.001(13) 0.009(13) -0.040(11) C86B 0.115(10) 0.099(11) 0.141(12) 0.006(10) 0.014(10) -0.045(10) C87B 0.16(2) 0.14(2) 0.19(2) 0.00(2) 0.05(2) -0.04(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1 -1 0 0.1103 1.0000 -1.0000 0.0001 -0.0110 0.0089 -0.0499 -1 1 0 0.0603 -1.0000 1.0000 -0.0001 0.0110 -0.0089 0.0499 0 0 -1 0.0099 0.0000 -0.0000 -1.0000 0.0141 0.0103 -0.0013 0 0 1 0.0079 -0.0000 0.0000 1.0000 -0.0141 -0.0103 0.0013 -1 -1 0 0.1291 -1.0000 -1.0000 -0.0002 -0.0288 0.0408 0.0139 1 1 0 0.1581 1.0000 1.0000 0.0002 0.0288 -0.0408 -0.0139 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 S1 U1 K1 133.30(3) . . S2 U1 K1 123.05(3) . . S2 U1 S1 44.68(4) . . O1 U1 K1 52.66(8) . . O1 U1 S1 132.20(9) . . O1 U1 S2 89.73(8) . . O1 U1 O21 89.17(12) . . O1 U1 O41 89.02(11) . . O1 U1 O61 105.12(11) . . O21 U1 K1 49.88(8) . . O21 U1 S1 84.13(8) . . O21 U1 S2 96.69(9) . . O21 U1 O41 83.24(11) . . O41 U1 K1 56.00(8) . . O41 U1 S1 136.51(9) . . O41 U1 S2 178.74(9) . . O61 U1 K1 136.44(8) . . O61 U1 S1 90.04(8) . . O61 U1 S2 88.95(9) . . O61 U1 O21 164.70(12) . . O61 U1 O41 91.42(11) . . Si1 K1 U1 64.75(3) . . Si1 K1 Si3 104.93(4) . . O1 K1 U1 37.53(6) . . O1 K1 Si1 27.45(6) . . O1 K1 Si2 90.74(7) . . O1 K1 Si3 85.43(7) . . O1 K1 O41 63.84(9) . . O2 K1 U1 91.91(8) . . O2 K1 Si1 27.46(8) . . O2 K1 O1 54.89(10) . . O2 K1 Si2 117.79(9) . . O2 K1 O21 109.08(11) . . O2 K1 O22 124.24(12) . . O2 K1 Si3 123.56(9) . . O2 K1 O41 113.96(10) . . Si2 K1 U1 65.18(3) . . Si2 K1 Si1 106.31(4) . . Si2 K1 Si3 98.68(4) . . O21 K1 U1 37.73(6) . . O21 K1 Si1 88.22(7) . . O21 K1 O1 66.64(9) . . O21 K1 Si2 27.46(7) . . O21 K1 Si3 83.72(8) . . O21 K1 O41 61.44(9) . . O22 K1 U1 93.07(8) . . O22 K1 Si1 125.89(9) . . O22 K1 O1 117.34(10) . . O22 K1 Si2 28.23(7) . . O22 K1 O21 55.50(10) . . O22 K1 Si3 108.53(9) . . O22 K1 O41 103.14(10) . . Si3 K1 U1 64.92(3) . . O41 K1 U1 38.07(6) . . O41 K1 Si1 88.58(7) . . O41 K1 Si2 83.09(7) . . O41 K1 Si3 26.88(6) . . O42 K1 U1 91.63(8) . . O42 K1 Si1 116.02(9) . . O42 K1 O1 105.38(10) . . O42 K1 O2 122.21(12) . . O42 K1 Si2 115.78(8) . . O42 K1 O21 108.18(10) . . O42 K1 O22 113.11(11) . . O42 K1 Si3 27.01(7) . . O42 K1 O41 53.77(9) . . S1 K2 K2 49.79(4) 5_666 5_666 S1 K2 K2 51.76(4) . 5_666 S1 K2 S1 101.55(5) . 5_666 S1 K2 S2 87.50(5) 5_666 . S1 K2 S2 37.88(4) . . S1 K2 S2 93.09(5) . 5_666 S1 K2 C26 156.99(15) . 5_666 S1 K2 C26 77.16(12) 5_666 5_666 S1 K2 Si4 81.94(4) . . S1 K2 Si4 154.40(6) 5_666 . S2 K2 K2 54.41(4) 5_666 5_666 S2 K2 K2 49.45(4) . 5_666 S2 K2 S1 38.89(4) 5_666 5_666 S2 K2 S2 103.86(5) 5_666 . S2 K2 C26 71.29(13) 5_666 5_666 S2 K2 C26 160.66(14) . 5_666 S2 K2 Si4 166.54(6) 5_666 . S2 K2 Si4 79.86(4) . . C26 K2 K2 122.64(13) 5_666 5_666 Si4 K2 K2 127.85(5) . 5_666 Si4 K2 C26 109.32(13) . 5_666 O62 K2 K2 132.18(9) . 5_666 O62 K2 S1 128.53(9) . 5_666 O62 K2 S1 102.75(8) . . O62 K2 S2 162.54(8) . 5_666 O62 K2 S2 84.86(8) . . O62 K2 C26 95.44(15) . 5_666 O62 K2 Si4 28.76(7) . . O62 K2 O63 52.32(10) . . O63 K2 K2 135.75(9) . 5_666 O63 K2 S1 173.38(9) . 5_666 O63 K2 S1 84.11(8) . . O63 K2 S2 99.11(8) . . O63 K2 S2 138.24(9) . 5_666 O63 K2 C26 96.28(14) . 5_666 O63 K2 Si4 29.09(7) . . U1 S1 K2 132.24(5) . 5_666 U1 S1 K2 107.11(5) . . K2 S1 K2 78.45(5) . 5_666 S2 S1 U1 66.88(5) . . S2 S1 K2 77.04(6) . . S2 S1 K2 68.60(6) . 5_666 U1 S2 K2 137.25(5) . 5_666 U1 S2 K2 101.82(5) . . K2 S2 K2 76.14(5) 5_666 . S1 S2 U1 68.44(5) . . S1 S2 K2 72.51(6) . 5_666 S1 S2 K2 65.08(6) . . O1 Si1 K1 55.83(12) . . O1 Si1 O2 104.53(17) . . O1 Si1 O3 116.05(19) . . O1 Si1 O4 113.43(19) . . O2 Si1 K1 48.74(12) . . O3 Si1 K1 125.88(15) . . O3 Si1 O2 104.9(2) . . O3 Si1 O4 107.26(19) . . O4 Si1 K1 125.39(14) . . O4 Si1 O2 110.3(2) . . U1 O1 K1 89.81(10) . . Si1 O1 U1 168.77(19) . . Si1 O1 K1 96.72(14) . . Si1 O2 K1 103.80(15) . . C1 O2 K1 125.8(3) . . C1 O2 Si1 129.9(3) . . C5 O3 Si1 135.8(3) . . C9 O4 Si1 130.1(3) . . O2 C1 C2 105.1(5) . . O2 C1 C3 109.3(5) . . O2 C1 C4 111.5(5) . . C2 C1 C4 109.5(6) . . C3 C1 C2 111.2(7) . . C3 C1 C4 110.2(6) . . C1 C2 H2A 109.5 . . C1 C2 H2B 109.5 . . C1 C2 H2C 109.5 . . H2A C2 H2B 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . C1 C3 H3A 109.5 . . C1 C3 H3B 109.5 . . C1 C3 H3C 109.5 . . H3A C3 H3B 109.5 . . H3A C3 H3C 109.5 . . H3B C3 H3C 109.5 . . C1 C4 H4A 109.5 . . C1 C4 H4B 109.5 . . C1 C4 H4C 109.5 . . H4A C4 H4B 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . O3 C5 C6 106.9(5) . . O3 C5 C7 106.6(4) . . O3 C5 C8 110.6(4) . . C7 C5 C6 110.9(5) . . C8 C5 C6 110.4(5) . . C8 C5 C7 111.2(5) . . C5 C6 H6A 109.5 . . C5 C6 H6B 109.5 . . C5 C6 H6C 109.5 . . H6A C6 H6B 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C5 C7 H7A 109.5 . . C5 C7 H7B 109.5 . . C5 C7 H7C 109.5 . . H7A C7 H7B 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C5 C8 H8A 109.5 . . C5 C8 H8B 109.5 . . C5 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . O4 C9 C10 106.0(5) . . O4 C9 C11 108.3(5) . . O4 C9 C12 111.7(5) . . C10 C9 C12 107.9(5) . . C11 C9 C10 111.0(6) . . C11 C9 C12 111.7(5) . . C9 C10 H10A 109.5 . . C9 C10 H10B 109.5 . . C9 C10 H10C 109.5 . . H10A C10 H10B 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C9 C11 H11A 109.5 . . C9 C11 H11B 109.5 . . C9 C11 H11C 109.5 . . H11A C11 H11B 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . C9 C12 H12A 109.5 . . C9 C12 H12B 109.5 . . C9 C12 H12C 109.5 . . H12A C12 H12B 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . O21 Si2 K1 53.01(12) . . O21 Si2 O22 103.03(18) . . O21 Si2 O23 115.20(19) . . O21 Si2 O24 116.01(19) . . O22 Si2 K1 50.47(12) . . O23 Si2 K1 123.40(15) . . O23 Si2 O22 111.1(2) . . O24 Si2 K1 129.43(15) . . O24 Si2 O22 104.94(19) . . O24 Si2 O23 106.1(2) . . U1 O21 K1 92.39(11) . . Si2 O21 U1 168.0(2) . . Si2 O21 K1 99.53(14) . . Si2 O22 K1 101.30(15) . . C21 O22 K1 128.2(3) . . C21 O22 Si2 130.5(3) . . C25 O23 Si2 135.3(3) . . C29 O24 Si2 136.6(4) . . O22 C21 C22 109.1(5) . . O22 C21 C23 111.5(5) . . O22 C21 C24 104.3(5) . . C22 C21 C23 109.7(7) . . C22 C21 C24 111.1(7) . . C23 C21 C24 111.1(6) . . C21 C22 H22A 109.5 . . C21 C22 H22B 109.5 . . C21 C22 H22C 109.5 . . H22A C22 H22B 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C21 C23 H23A 109.5 . . C21 C23 H23B 109.5 . . C21 C23 H23C 109.5 . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C21 C24 H24A 109.5 . . C21 C24 H24B 109.5 . . C21 C24 H24C 109.5 . . H24A C24 H24B 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . O23 C25 C26 106.9(5) . . O23 C25 C27 110.0(7) . . O23 C25 C28 106.8(5) . . C26 C25 C27 113.9(8) . . C27B C25 O23 126.4(16) . . C27B C25 C28 114.9(18) . . C28 C25 C26 109.7(5) . . C28 C25 C27 109.3(6) . . K2 C26 H26A 79.5 5_666 . K2 C26 H26B 47.0 5_666 . K2 C26 H26C 87.2 5_666 . C25 C26 K2 155.9(4) . 5_666 C25 C26 H26A 109.5 . . C25 C26 H26B 109.5 . . C25 C26 H26C 109.5 . . H26A C26 H26B 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C25 C27 H27A 109.5 . . C25 C27 H27B 109.5 . . C25 C27 H27C 109.5 . . H27A C27 H27B 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C25 C27B H27D 109.5 . . C25 C27B H27E 109.5 . . C25 C27B H27F 109.5 . . H27D C27B H27E 109.5 . . H27D C27B H27F 109.5 . . H27E C27B H27F 109.5 . . C25 C28 H28A 109.5 . . C25 C28 H28B 109.5 . . C25 C28 H28C 109.5 . . H28A C28 H28B 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . O24 C29 C30B 104.0(8) . . O24 C29 C31B 116.9(10) . . O24 C29 C32 106.8(5) . . O24 C29 C31 103.9(7) . . C31B C29 C30B 104.9(17) . . C32 C29 C30B 92.0(14) . . C32 C29 C31B 126.6(14) . . C32 C29 C31 98.7(10) . . C30 C29 O24 113.3(7) . . C30 C29 C32 120.2(10) . . C30 C29 C31 111.8(10) . . C29 C30B H30D 109.5 . . C29 C30B H30E 109.5 . . C29 C30B H30F 109.5 . . H30D C30B H30E 109.5 . . H30D C30B H30F 109.5 . . H30E C30B H30F 109.5 . . C29 C31B H31D 109.5 . . C29 C31B H31E 109.5 . . C29 C31B H31F 109.5 . . H31D C31B H31E 109.5 . . H31D C31B H31F 109.5 . . H31E C31B H31F 109.5 . . C29 C32 H32A 109.5 . . C29 C32 H32B 109.5 . . C29 C32 H32C 109.5 . . H32A C32 H32B 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . C29 C30 H30A 109.5 . . C29 C30 H30B 109.5 . . C29 C30 H30C 109.5 . . H30A C30 H30B 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . C29 C31 H31A 109.5 . . C29 C31 H31B 109.5 . . C29 C31 H31C 109.5 . . H31A C31 H31B 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . O41 Si3 K1 59.02(12) . . O41 Si3 O42 105.55(18) . . O41 Si3 O43 113.76(18) . . O41 Si3 O44 116.39(19) . . O42 Si3 K1 46.82(12) . . O43 Si3 K1 124.09(13) . . O43 Si3 O42 111.20(18) . . O44 Si3 K1 128.56(14) . . O44 Si3 O42 104.60(19) . . O44 Si3 O43 105.05(19) . . U1 O41 K1 85.92(10) . . Si3 O41 U1 176.9(2) . . Si3 O41 K1 94.10(14) . . Si3 O42 K1 106.17(15) . . C41 O42 K1 122.4(3) . . C41 O42 Si3 131.3(3) . . C45 O43 Si3 131.6(3) . . C49 O44 Si3 133.1(3) . . O42 C41 C42 108.6(5) . . O42 C41 C43 106.6(5) . . O42 C41 C44 111.9(5) . . C43 C41 C42 107.4(7) . . C43 C41 C44 112.1(7) . . C44 C41 C42 110.0(7) . . C41 C42 H42A 109.5 . . C41 C42 H42B 109.5 . . C41 C42 H42C 109.5 . . H42A C42 H42B 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . C41 C43 H43A 109.5 . . C41 C43 H43B 109.5 . . C41 C43 H43C 109.5 . . H43A C43 H43B 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . C41 C44 H44A 109.5 . . C41 C44 H44B 109.5 . . C41 C44 H44C 109.5 . . H44A C44 H44B 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . O43 C45 C46 110.7(4) . . O43 C45 C47 104.9(4) . . O43 C45 C48 108.6(4) . . C46 C45 C47 110.8(5) . . C46 C45 C48 111.7(5) . . C48 C45 C47 109.8(5) . . C45 C46 H46A 109.5 . . C45 C46 H46B 109.5 . . C45 C46 H46C 109.5 . . H46A C46 H46B 109.5 . . H46A C46 H46C 109.5 . . H46B C46 H46C 109.5 . . C45 C47 H47A 109.5 . . C45 C47 H47B 109.5 . . C45 C47 H47C 109.5 . . H47A C47 H47B 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . C45 C48 H48A 109.5 . . C45 C48 H48B 109.5 . . C45 C48 H48C 109.5 . . H48A C48 H48B 109.5 . . H48A C48 H48C 109.5 . . H48B C48 H48C 109.5 . . O44 C49 C50 105.5(5) . . O44 C49 C51 112.6(4) . . O44 C49 C52 106.6(5) . . C51 C49 C50 108.4(5) . . C52 C49 C50 108.9(6) . . C52 C49 C51 114.3(6) . . C49 C50 H50A 109.5 . . C49 C50 H50B 109.5 . . C49 C50 H50C 109.5 . . H50A C50 H50B 109.5 . . H50A C50 H50C 109.5 . . H50B C50 H50C 109.5 . . C49 C51 H51A 109.5 . . C49 C51 H51B 109.5 . . C49 C51 H51C 109.5 . . H51A C51 H51B 109.5 . . H51A C51 H51C 109.5 . . H51B C51 H51C 109.5 . . C49 C52 H52A 109.5 . . C49 C52 H52B 109.5 . . C49 C52 H52C 109.5 . . H52A C52 H52B 109.5 . . H52A C52 H52C 109.5 . . H52B C52 H52C 109.5 . . O61 Si4 K2 96.85(13) . . O61 Si4 O62 114.45(19) . . O61 Si4 O63 112.85(17) . . O61 Si4 O64 107.57(18) . . O62 Si4 K2 53.76(12) . . O62 Si4 O63 95.63(18) . . O63 Si4 K2 54.98(14) . . O64 Si4 K2 155.56(13) . . O64 Si4 O62 113.91(18) . . O64 Si4 O63 112.26(19) . . Si4 O61 U1 156.50(19) . . Si4 O62 K2 97.48(15) . . C61 O62 K2 113.9(3) . . C61 O62 Si4 137.0(3) . . Si4 O63 K2 95.93(16) . . C65 O63 K2 117.6(3) . . C65 O63 Si4 136.3(3) . . C69 O64 Si4 138.1(3) . . O62 C61 C62 106.7(4) . . O62 C61 C63 108.4(4) . . O62 C61 C64 110.2(4) . . C62 C61 C63 109.0(5) . . C64 C61 C62 111.8(5) . . C64 C61 C63 110.5(5) . . C61 C62 H62A 109.5 . . C61 C62 H62B 109.5 . . C61 C62 H62C 109.5 . . H62A C62 H62B 109.5 . . H62A C62 H62C 109.5 . . H62B C62 H62C 109.5 . . C61 C63 H63A 109.5 . . C61 C63 H63B 109.5 . . C61 C63 H63C 109.5 . . H63A C63 H63B 109.5 . . H63A C63 H63C 109.5 . . H63B C63 H63C 109.5 . . C61 C64 H64A 109.5 . . C61 C64 H64B 109.5 . . C61 C64 H64C 109.5 . . H64A C64 H64B 109.5 . . H64A C64 H64C 109.5 . . H64B C64 H64C 109.5 . . O63 C65 C66 111.4(4) . . O63 C65 C67 108.9(5) . . O63 C65 C68 104.2(5) . . C66 C65 C67 110.2(6) . . C66 C65 C68 110.0(5) . . C68 C65 C67 112.0(6) . . C65 C66 H66A 109.5 . . C65 C66 H66B 109.5 . . C65 C66 H66C 109.5 . . H66A C66 H66B 109.5 . . H66A C66 H66C 109.5 . . H66B C66 H66C 109.5 . . C65 C67 H67A 109.5 . . C65 C67 H67B 109.5 . . C65 C67 H67C 109.5 . . H67A C67 H67B 109.5 . . H67A C67 H67C 109.5 . . H67B C67 H67C 109.5 . . C65 C68 H68A 109.5 . . C65 C68 H68B 109.5 . . C65 C68 H68C 109.5 . . H68A C68 H68B 109.5 . . H68A C68 H68C 109.5 . . H68B C68 H68C 109.5 . . O64 C69 C70 107.2(4) . . O64 C69 C71 107.3(4) . . O64 C69 C72 111.1(4) . . C70 C69 C71 108.8(5) . . C72 C69 C70 111.9(5) . . C72 C69 C71 110.5(5) . . C69 C70 H70A 109.5 . . C69 C70 H70B 109.5 . . C69 C70 H70C 109.5 . . H70A C70 H70B 109.5 . . H70A C70 H70C 109.5 . . H70B C70 H70C 109.5 . . C69 C71 H71A 109.5 . . C69 C71 H71B 109.5 . . C69 C71 H71C 109.5 . . H71A C71 H71B 109.5 . . H71A C71 H71C 109.5 . . H71B C71 H71C 109.5 . . C69 C72 H72A 109.5 . . C69 C72 H72B 109.5 . . C69 C72 H72C 109.5 . . H72A C72 H72B 109.5 . . H72A C72 H72C 109.5 . . H72B C72 H72C 109.5 . . C82 C81 C86 115.2(17) . . C82 C81 C87 124.4(17) . . C86 C81 C87 120.2(16) . . C81 C82 H82 114.7 . . C83 C82 C81 131(2) . . C83 C82 H82 114.7 . . C82 C83 H83 123.1 . . C82 C83 C84 114(2) . . C84 C83 H83 123.1 . . C83 C84 H84 119.5 . . C85 C84 C83 121.0(19) . . C85 C84 H84 119.5 . . C84 C85 H85 119.5 . . C84 C85 C86 121(2) . . C86 C85 H85 119.5 . . C81 C86 C85 117.7(18) . . C81 C86 H86 121.1 . . C85 C86 H86 121.1 . . C81 C87 H87A 109.5 . . C81 C87 H87B 109.5 . . C81 C87 H87C 109.5 . . H87A C87 H87B 109.5 . . H87A C87 H87C 109.5 . . H87B C87 H87C 109.5 . . C82B C81B C86B 120.9(4) . . C82B C81B C87B 119.3(3) . . C86B C81B C87B 115.7(6) . . C81B C82B H82B 120.0 . . C81B C82B C83B 120.0 . . C83B C82B H82B 120.0 . . C82B C83B H83B 120.0 . . C82B C83B C84B 120.1 . . C84B C83B H83B 120.0 . . C83B C84B H84B 120.0 . . C83B C84B C85B 120.0 . . C85B C84B H84B 120.0 . . C84B C85B H85B 120.6 . . C86B C85B C84B 118.8(7) . . C86B C85B H85B 120.6 . . C81B C86B H86B 120.0 . . C85B C86B C81B 120.06(14) . . C85B C86B H86B 120.0 . . C81B C87B H87D 109.5 . . C81B C87B H87E 109.5 . . C81B C87B H87F 109.5 . . H87D C87B H87E 109.5 . . H87D C87B H87F 109.5 . . H87E C87B H87F 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 K1 3.6197(10) . U1 S1 2.7836(12) . U1 S2 2.7526(13) . U1 O1 2.205(3) . U1 O21 2.217(3) . U1 O41 2.238(3) . U1 O61 2.205(3) . K1 Si1 3.4545(17) . K1 O1 2.878(3) . K1 O2 2.674(3) . K1 Si2 3.4203(17) . K1 O21 2.770(3) . K1 O22 2.690(4) . K1 Si3 3.5002(17) . K1 O41 3.009(3) . K1 O42 2.657(3) . K2 K2 3.988(3) 5_666 K2 S1 3.1973(19) 5_666 K2 S1 3.1088(18) . K2 S2 3.1212(17) 5_666 K2 S2 3.3407(19) . K2 C26 3.445(8) 5_666 K2 Si4 3.3682(18) . K2 O62 2.740(3) . K2 O63 2.773(4) . S1 K2 3.1972(19) 5_666 S1 S2 2.1047(18) . S2 K2 3.1212(17) 5_666 Si1 O1 1.603(3) . Si1 O2 1.640(4) . Si1 O3 1.613(4) . Si1 O4 1.622(4) . O2 C1 1.458(6) . O3 C5 1.436(6) . O4 C9 1.450(6) . C1 C2 1.502(9) . C1 C3 1.494(10) . C1 C4 1.515(9) . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 H2C 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 1.512(8) . C5 C7 1.511(7) . C5 C8 1.509(8) . 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 C10 1.525(8) . C9 C11 1.481(9) . C9 C12 1.531(8) . 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 . Si2 O21 1.599(3) . Si2 O22 1.650(4) . Si2 O23 1.617(4) . Si2 O24 1.614(4) . O22 C21 1.452(6) . O23 C25 1.442(7) . O24 C29 1.435(6) . C21 C22 1.485(9) . C21 C23 1.500(9) . C21 C24 1.500(9) . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 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 1.522(9) . C25 C27 1.536(13) . C25 C27B 1.45(4) . C25 C28 1.515(8) . C26 K2 3.445(8) 5_666 C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C27B H27D 0.9800 . C27B H27E 0.9800 . C27B H27F 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 C30B 1.64(2) . C29 C31B 1.51(3) . C29 C32 1.469(9) . C29 C30 1.397(14) . C29 C31 1.569(15) . C30B H30D 0.9800 . C30B H30E 0.9800 . C30B H30F 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 . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . Si3 O41 1.586(3) . Si3 O42 1.655(4) . Si3 O43 1.626(3) . Si3 O44 1.621(4) . O42 C41 1.446(6) . O43 C45 1.444(6) . O44 C49 1.429(6) . C41 C42 1.511(10) . C41 C43 1.480(9) . C41 C44 1.481(9) . 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 C46 1.494(8) . C45 C47 1.512(7) . C45 C48 1.509(7) . 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 C50 1.531(8) . C49 C51 1.493(8) . C49 C52 1.467(9) . 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 . Si4 O61 1.593(3) . Si4 O62 1.635(3) . Si4 O63 1.646(3) . Si4 O64 1.619(4) . O62 C61 1.446(6) . O63 C65 1.450(6) . O64 C69 1.446(6) . C61 C62 1.524(7) . C61 C63 1.525(8) . C61 C64 1.516(7) . 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 H64A 0.9800 . C64 H64B 0.9800 . C64 H64C 0.9800 . C65 C66 1.501(8) . C65 C67 1.511(10) . C65 C68 1.508(9) . C66 H66A 0.9800 . C66 H66B 0.9800 . C66 H66C 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 C70 1.520(7) . C69 C71 1.526(8) . C69 C72 1.519(8) . 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 1.39(2) . C81 C86 1.40(2) . C81 C87 1.50(2) . C82 H82 0.9500 . C82 C83 1.24(2) . C83 H83 0.9500 . C83 C84 1.46(2) . C84 H84 0.9500 . C84 C85 1.33(2) . C85 H85 0.9500 . C85 C86 1.41(2) . C86 H86 0.9500 . C87 H87A 0.9800 . C87 H87B 0.9800 . C87 H87C 0.9800 . C81B C82B 1.362(12) . C81B C86B 1.399(4) . C81B C87B 1.552(7) . C82B H82B 0.9500 . C82B C83B 1.386(2) . C83B H83B 0.9500 . C83B C84B 1.3920(10) . C84B H84B 0.9500 . C84B C85B 1.412(13) . C85B H85B 0.9500 . C85B C86B 1.383(4) . C86B H86B 0.9500 . C87B H87D 0.9800 . C87B H87E 0.9800 . C87B H87F 0.9800 .