#------------------------------------------------------------------------------ #$Date: 2021-11-03 01:37:29 +0200 (Wed, 03 Nov 2021) $ #$Revision: 270215 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/38/7243820.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_7243820 loop_ _publ_author_name 'Shi, Jianhang' 'Zhang, Hongxu' 'Wang, Peisen' 'Wang, Pai' 'Zha, Junjie' 'Liu, Yi' 'Gautam, Jagadis' 'Zhang, Lu-Nan' 'Wang, Yue' 'Xie, Ju' 'Ni, Lubin' 'Diao, Guowang' 'Wei, Yongge' _publ_section_title ; Inorganic--Organic Hybrid Supramolecular Architectures Based on Keggin Polyoxometalates and Crown Ether:Synthesis, Crystal Structure and Electrochemical Properties ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE01203G _journal_year 2021 _chemical_formula_moiety 'C52 H102 K4 N2 O64 Si W12' _chemical_formula_sum 'C52 H102 K4 N2 O64 Si W12' _chemical_formula_weight 4170.04 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-12-17 _audit_creation_method ; Olex2 1.3 (compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132) ; _audit_update_record ; 2021-05-28 deposited with the CCDC. 2021-10-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.730(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.9948(7) _cell_length_b 25.5334(13) _cell_length_c 14.1995(7) _cell_measurement_reflns_used 9860 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 27.44 _cell_measurement_theta_min 2.20 _cell_volume 4859.2(4) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_unetI/netI 0.0603 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 49529 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.567 _diffrn_reflns_theta_min 1.969 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 14.426 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1380 before and 0.0662 after correction. The Ratio of minimum to maximum transmission is 0.5656. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.850 _exptl_crystal_description block _exptl_crystal_F_000 3836 _exptl_crystal_size_max 0.292 _exptl_crystal_size_mid 0.266 _exptl_crystal_size_min 0.263 _refine_diff_density_max 1.617 _refine_diff_density_min -1.505 _refine_diff_density_rms 0.229 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 602 _refine_ls_number_reflns 11169 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0423 _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^)+(0.0134P)^2^+44.2829P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.0799 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8168 _reflns_number_total 11169 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01203g2.cif _cod_data_source_block 2CH3CN-4Crown@SiW12 _cod_database_code 7243820 _shelx_shelxl_version_number 2017/1 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N1-C25 1.15 with sigma of 0.01 C25-C26 1.5 with sigma of 0.01 3. Others Fixed Sof: W6(0.33333) W6'(0.33333) W6''(0.33333) O19(0.5) O19'(0.5) O20(0.5) O20'(0.5) 4.a Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A, H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B) 4.b Idealised Me refined as rotating group: C26(H26A,H26B,H26C) ; _shelx_res_file ; TITL nice_a.res in P2(1)/n Nice.res created by SHELXL-2017/1 at 22:28:28 on 17-Dec-2020 REM Old TITL Nice in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.182, Rweak 0.011, Alpha 0.029, Orientation as input REM Formula found by SHELXT: O80 K5 W12 CELL 0.71073 13.9948 25.5334 14.1995 90 106.73 90 ZERR 2 0.0007 0.0013 0.0007 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H K N O Si W UNIT 104 204 8 4 128 2 24 DFIX 1.15 0.01 N1 C25 DFIX 1.5 0.01 C25 C26 L.S. 40 PLAN 20 TEMP 0 CONF list 4 MORE -1 fmap 2 acta BOND $H OMIT 0 2 0 OMIT 0 1 1 OMIT 1 1 0 OMIT 0 1 2 REM REM REM WGHT 0.013400 44.282906 FVAR 0.10478 W1 7 0.757848 0.520797 0.604279 11.00000 0.01871 0.04550 = 0.04129 -0.01429 -0.00253 0.00467 W2 7 0.637563 0.570683 0.368060 11.00000 0.04349 0.03004 = 0.02588 0.00406 0.01578 0.00350 W3 7 0.539726 0.445890 0.285737 11.00000 0.03050 0.03809 = 0.02070 -0.00218 0.00806 -0.00669 W4 7 0.376869 0.553383 0.266772 11.00000 0.02538 0.03024 = 0.02029 0.00369 0.00449 0.00230 W5 7 0.329959 0.604810 0.480760 11.00000 0.02397 0.02618 = 0.05494 0.00790 0.00854 0.00680 W6 7 0.597279 0.623682 0.587084 10.33333 0.04553 0.01743 = 0.03000 0.00311 -0.01693 -0.00527 W6' 7 0.572963 0.627728 0.580165 10.33333 0.02032 W6'' 7 0.597014 0.626494 0.564507 10.33333 0.01979 K1 3 0.960903 0.642516 0.706219 11.00000 0.05864 0.04765 = 0.04337 -0.00552 0.01566 0.00589 SI1 6 0.500000 0.500000 0.500000 10.50000 0.01370 0.01460 = 0.01782 -0.00063 0.00281 0.00105 O1 5 0.880589 0.531541 0.652653 11.00000 0.03193 0.08272 = 0.03703 -0.00818 0.00760 -0.02150 O2 5 0.631677 0.685871 0.616132 11.00000 0.05872 0.03232 = 0.05137 -0.01430 0.02724 -0.01689 O3 5 0.706743 0.585144 0.630744 11.00000 0.17537 0.10020 = 0.02338 -0.01565 -0.01022 0.10399 O4 5 0.740885 0.543296 0.471496 11.00000 0.15648 0.09603 = 0.02698 -0.00998 -0.00538 0.09741 O5 5 0.701954 0.604046 0.303672 11.00000 0.04114 0.04701 = 0.09068 0.02160 0.02517 -0.00619 O6 5 0.559938 0.419627 0.184935 11.00000 0.03969 0.09219 = 0.04696 -0.04158 0.00322 0.01806 O7 5 0.449973 0.397293 0.311607 11.00000 0.04509 0.14405 = 0.09885 0.09166 -0.02267 -0.04892 O8 5 0.432133 0.491005 0.230515 11.00000 0.02824 0.03177 = 0.10250 -0.01797 0.01915 -0.00691 O9 5 0.275829 0.508132 0.288738 11.00000 0.09782 0.05094 = 0.12287 -0.04297 0.09232 -0.03799 O10 5 0.241241 0.547910 0.447037 11.00000 0.10201 0.05662 = 0.10022 -0.05154 0.08180 -0.04564 O11 5 0.251618 0.655331 0.469572 11.00000 0.06869 0.03895 = 0.06382 0.01791 0.03718 0.03067 O12 5 0.356897 0.587526 0.613970 11.00000 0.04532 0.12219 = 0.08717 0.07453 -0.03207 -0.04680 O13 5 0.343115 0.601840 0.350517 11.00000 0.09266 0.06445 = 0.10575 -0.05113 0.07991 -0.04722 O14 5 0.318559 0.579008 0.156977 11.00000 0.09738 0.04305 = 0.05233 0.00659 -0.03917 0.00029 O15 5 0.503333 0.584428 0.291519 11.00000 0.02682 0.03437 = 0.10627 -0.01729 0.02094 -0.00673 O16 5 0.626347 0.504710 0.307679 11.00000 0.02344 0.03592 = 0.09978 -0.01702 0.01463 -0.00367 O17 5 0.454868 0.641293 0.513470 11.00000 0.04592 0.14855 = 0.08513 0.08672 -0.02568 -0.04957 O18 5 0.615710 0.622930 0.455401 11.00000 0.16430 0.09137 = 0.03067 -0.01403 -0.01196 0.08712 O19 5 0.595341 0.541232 0.504876 10.50000 0.01881 O19' 5 0.474074 0.553309 0.554652 10.50000 0.01777 O20 5 0.505977 0.512902 0.395831 10.50000 0.02008 O20' 5 0.400773 0.525983 0.429166 10.50000 0.01872 O21 5 0.875415 0.738915 0.598059 11.00000 0.04783 0.05837 = 0.06689 -0.00601 0.01037 0.00930 O22 5 0.908392 0.650764 0.500511 11.00000 0.06598 0.05982 = 0.04165 0.00898 0.02061 0.01574 O23 5 1.075349 0.591779 0.595725 11.00000 0.04684 0.05564 = 0.05666 -0.00544 0.01463 0.00494 O24 5 1.139162 0.587628 0.800918 11.00000 0.04607 0.07247 = 0.06173 -0.00684 0.01010 0.00705 O25 5 1.100430 0.677776 0.895094 11.00000 0.09710 0.06771 = 0.05141 -0.02071 0.01743 -0.00379 O26 5 0.936028 0.740019 0.803760 11.00000 0.11584 0.05395 = 0.06508 -0.02555 0.01070 0.00963 N1 4 0.865428 0.607469 0.845171 11.00000 0.13587 C13 1 1.191296 0.563581 0.740835 11.00000 0.04610 0.08332 = 0.07797 0.02029 0.02605 0.02656 AFIX 23 H13A 2 1.227849 0.533505 0.774687 11.00000 -1.20000 H13B 2 1.238989 0.588120 0.728041 11.00000 -1.20000 AFIX 0 C14 1 1.121933 0.546871 0.648089 11.00000 0.04948 0.06032 = 0.07963 -0.00998 0.02427 0.01744 AFIX 23 H14A 2 1.157503 0.527887 0.609458 11.00000 -1.20000 H14B 2 1.071932 0.523763 0.660599 11.00000 -1.20000 AFIX 0 C15 1 1.011719 0.577778 0.501903 11.00000 0.05781 0.07554 = 0.06429 -0.02037 0.03031 0.00577 AFIX 23 H15A 2 0.959573 0.554577 0.509551 11.00000 -1.20000 H15B 2 1.049684 0.559398 0.464819 11.00000 -1.20000 AFIX 0 C16 1 0.966545 0.625602 0.448104 11.00000 0.07280 0.07314 = 0.04353 -0.00492 0.02611 0.00106 AFIX 23 H16A 2 1.018641 0.649024 0.441093 11.00000 -1.20000 H16B 2 0.925122 0.616293 0.382894 11.00000 -1.20000 AFIX 0 C17 1 0.861474 0.694919 0.450032 11.00000 0.04557 0.06670 = 0.05281 0.00847 0.00535 -0.01320 AFIX 23 H17A 2 0.814433 0.684209 0.388475 11.00000 -1.20000 H17B 2 0.910926 0.717406 0.434859 11.00000 -1.20000 AFIX 0 C18 1 0.808502 0.724293 0.508689 11.00000 0.03662 0.06210 = 0.06128 0.01864 0.00771 0.00490 AFIX 23 H18A 2 0.777925 0.755258 0.472935 11.00000 -1.20000 H18B 2 0.756112 0.702695 0.520529 11.00000 -1.20000 AFIX 0 C19 1 0.830942 0.771135 0.656612 11.00000 0.08616 0.05791 = 0.10882 -0.01049 0.00989 0.03353 AFIX 23 H19A 2 0.803029 0.802363 0.620072 11.00000 -1.20000 H19B 2 0.777249 0.752147 0.671914 11.00000 -1.20000 AFIX 0 C20 1 0.903519 0.785445 0.744660 11.00000 0.12352 0.04867 = 0.13419 -0.03125 0.02267 0.01452 AFIX 23 H20A 2 0.875342 0.810556 0.780487 11.00000 -1.20000 H20B 2 0.959909 0.801755 0.729459 11.00000 -1.20000 AFIX 0 C21 1 1.008180 0.754410 0.892750 11.00000 0.10961 0.08268 = 0.08242 -0.06224 0.01732 -0.01312 AFIX 23 H21A 2 0.977860 0.776486 0.931810 11.00000 -1.20000 H21B 2 1.062011 0.773810 0.878559 11.00000 -1.20000 AFIX 0 C22 1 1.047290 0.706081 0.947284 11.00000 0.11083 0.10501 = 0.05885 -0.04736 0.00908 -0.01318 AFIX 23 H22A 2 1.090641 0.714881 1.011946 11.00000 -1.20000 H22B 2 0.992529 0.685083 0.955606 11.00000 -1.20000 AFIX 0 C23 1 1.144557 0.632551 0.946864 11.00000 0.11542 0.07841 = 0.04813 -0.00582 -0.01365 0.00017 AFIX 23 H23A 2 1.093613 0.608473 0.954318 11.00000 -1.20000 H23B 2 1.186981 0.641853 1.011657 11.00000 -1.20000 AFIX 0 C24 1 1.204061 0.608419 0.887734 11.00000 0.07305 0.06795 = 0.07655 0.01443 -0.00854 -0.00337 AFIX 23 H24A 2 1.247169 0.634510 0.871507 11.00000 -1.20000 H24B 2 1.245646 0.580786 0.925163 11.00000 -1.20000 AFIX 0 C25 1 0.804944 0.636595 0.852538 11.00000 0.18292 C26 1 0.725686 0.668173 0.879773 11.00000 0.25942 AFIX 137 H26A 2 0.756390 0.690268 0.934879 11.00000 -1.50000 H26B 2 0.679432 0.644911 0.896901 11.00000 -1.50000 H26C 2 0.690813 0.689431 0.824865 11.00000 -1.50000 AFIX 0 K2 3 0.200064 0.357437 -0.159242 11.00000 0.04523 0.08111 = 0.07515 -0.01743 0.00482 0.00676 O27 5 0.366381 0.403254 -0.028349 11.00000 0.06030 0.06412 = 0.05687 -0.00016 0.01170 -0.00517 O28 5 0.182916 0.455594 -0.080388 11.00000 0.08916 0.07759 = 0.09423 0.00746 0.02787 0.03014 O29 5 0.007866 0.394425 -0.157651 11.00000 0.06289 0.14291 = 0.10126 0.02763 0.01447 0.04108 O30 5 0.023373 0.296402 -0.236718 11.00000 0.04812 0.14319 = 0.09489 0.05144 0.01450 -0.02076 O31 5 0.209748 0.248439 -0.172501 11.00000 0.07711 0.05797 = 0.16731 -0.00975 0.02060 -0.00842 O32 5 0.382834 0.304370 -0.103281 11.00000 0.06416 0.07853 = 0.08422 0.00158 0.01180 0.01603 C1 1 0.462024 0.328833 -0.032199 11.00000 0.05636 0.11600 = 0.07577 -0.00473 0.00012 0.02538 AFIX 23 H1A 2 0.525416 0.316168 -0.038043 11.00000 -1.20000 H1B 2 0.458172 0.320577 0.033289 11.00000 -1.20000 AFIX 0 C2 1 0.454879 0.386053 -0.047982 11.00000 0.05283 0.14294 = 0.03866 0.00057 0.01029 -0.01089 AFIX 23 H2A 2 0.512432 0.403329 -0.004257 11.00000 -1.20000 H2B 2 0.452673 0.394280 -0.115267 11.00000 -1.20000 AFIX 0 C3 1 0.359620 0.458205 -0.025632 11.00000 0.09297 0.07466 = 0.06950 -0.00161 0.00562 -0.02192 AFIX 23 H3A 2 0.358925 0.473015 -0.088734 11.00000 -1.20000 H3B 2 0.416342 0.472438 0.024303 11.00000 -1.20000 AFIX 0 C4 1 0.265352 0.471081 -0.002287 11.00000 0.12541 0.05190 = 0.12036 -0.01424 0.01541 0.00216 AFIX 23 H4A 2 0.263727 0.453180 0.057485 11.00000 -1.20000 H4B 2 0.262187 0.508473 0.008506 11.00000 -1.20000 AFIX 0 C5 1 0.088533 0.468137 -0.066938 11.00000 0.13107 0.07983 = 0.14585 0.03351 0.09024 0.04092 AFIX 23 H5A 2 0.083711 0.505608 -0.058025 11.00000 -1.20000 H5B 2 0.081095 0.450643 -0.008818 11.00000 -1.20000 AFIX 0 C6 1 0.006173 0.450171 -0.158073 11.00000 0.09192 0.15824 = 0.15565 0.07140 0.04526 0.07434 AFIX 23 H6A 2 -0.058314 0.462855 -0.155357 11.00000 -1.20000 H6B 2 0.018623 0.463526 -0.217404 11.00000 -1.20000 AFIX 0 C7 1 -0.070595 0.372685 -0.232348 11.00000 0.03705 0.26982 = 0.06253 0.02940 0.00268 0.04379 AFIX 23 H7A 2 -0.066114 0.384488 -0.295870 11.00000 -1.20000 H7B 2 -0.133855 0.384540 -0.224859 11.00000 -1.20000 AFIX 0 C8 1 -0.066582 0.316055 -0.228420 11.00000 0.04716 0.26010 = 0.05921 0.00402 0.01842 -0.03182 AFIX 23 H8A 2 -0.075948 0.304414 -0.166655 11.00000 -1.20000 H8B 2 -0.120860 0.301985 -0.281260 11.00000 -1.20000 AFIX 0 C9 1 0.035198 0.242336 -0.218192 11.00000 0.10412 0.13937 = 0.11186 0.03926 0.01194 -0.08275 AFIX 23 H9A 2 -0.018423 0.223826 -0.264985 11.00000 -1.20000 H9B 2 0.029581 0.235265 -0.152877 11.00000 -1.20000 AFIX 0 C10 1 0.132057 0.221766 -0.225045 11.00000 0.12730 0.09278 = 0.12534 0.04221 0.01662 -0.03197 AFIX 23 H10A 2 0.138790 0.185596 -0.203238 11.00000 -1.20000 H10B 2 0.131963 0.222269 -0.293378 11.00000 -1.20000 AFIX 0 C11 1 0.302387 0.227128 -0.169443 11.00000 0.09246 0.07106 = 0.14763 0.01771 0.03038 0.01605 AFIX 23 H11A 2 0.316700 0.233896 -0.231230 11.00000 -1.20000 H11B 2 0.300738 0.189493 -0.160733 11.00000 -1.20000 AFIX 0 C12 1 0.380859 0.249888 -0.088750 11.00000 0.08341 0.09374 = 0.15245 0.03013 0.02858 0.04029 AFIX 23 H12A 2 0.367818 0.242543 -0.026567 11.00000 -1.20000 H12B 2 0.444880 0.234719 -0.087052 11.00000 -1.20000 AFIX 0 HKLF 4 REM nice_a.res in P2(1)/n REM R1 = 0.0423 for 8168 Fo > 4sig(Fo) and 0.0729 for all 11169 data REM 602 parameters refined using 2 restraints END WGHT 0.0134 44.2915 REM Highest difference peak 1.617, deepest hole -1.505, 1-sigma level 0.229 Q1 1 0.7430 0.5974 0.6266 11.00000 0.05 1.62 Q2 1 0.7986 0.7226 0.9654 11.00000 0.05 1.57 Q3 1 0.7804 0.5527 0.4749 11.00000 0.05 1.53 Q4 1 0.1853 0.3418 -0.1010 11.00000 0.05 1.42 Q5 1 0.3448 0.6011 0.6383 11.00000 0.05 1.38 Q6 1 0.6763 0.5743 0.6441 11.00000 0.05 1.35 Q7 1 0.7140 0.5312 0.5056 11.00000 0.05 1.34 Q8 1 0.6400 0.6365 0.4433 11.00000 0.05 1.32 Q9 1 0.4600 0.6226 0.4995 11.00000 0.05 1.29 Q10 1 0.5854 0.6125 0.4537 11.00000 0.05 1.18 Q11 1 0.4395 0.6529 0.5403 11.00000 0.05 1.16 Q12 1 0.5221 0.4749 0.2543 11.00000 0.05 1.13 Q13 1 0.7777 0.5199 0.6731 11.00000 0.05 1.10 Q14 1 0.6032 0.5427 0.3261 11.00000 0.05 1.08 Q15 1 0.3613 0.5650 0.6004 11.00000 0.05 1.06 Q16 1 0.4604 0.3867 0.2771 11.00000 0.05 1.05 Q17 1 0.7888 0.5335 0.5966 11.00000 0.05 1.05 Q18 1 0.3752 0.5983 0.3762 11.00000 0.05 1.04 Q19 1 0.4718 0.3724 0.3218 11.00000 0.05 1.04 Q20 1 0.5563 0.4759 0.3207 11.00000 0.05 0.99 ; _shelx_res_checksum 11026 _shelx_hkl_file ; 1 0 0 -0.31 0.42 1 0 0 -0.13 0.45 -1 0 0 -0.25 0.37 -1 0 0 0.98 0.50 2 0 0 5.02 1.19 -2 0 0 3.18 1.14 -2 0 0 5.49 1.37 2 0 0 3.10 1.39 3 0 0 -1.62 1.36 3 0 0 0.74 1.78 -3 0 0 1.94 1.58 -3 0 0 2.31 1.87 4 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375.08 28.21 -2 -22 0 370.15 24.91 2 -22 0 383.40 28.31 -2 -22 0 379.97 28.68 2 22 0 381.62 24.56 -2 22 0 404.63 33.23 -2 22 0 393.32 27.26 3 -22 0 833.04 48.34 -3 -22 0 789.02 48.47 -3 -22 0 766.49 43.25 -3 22 0 733.81 50.90 -3 22 0 786.12 47.14 3 22 0 789.15 43.76 4 -22 0 -11.76 10.10 -4 -22 0 -4.02 5.49 -4 -22 0 -5.36 8.80 -4 22 0 0.09 9.55 -4 22 0 0.91 14.26 4 22 0 6.52 7.16 5 -22 0 103.13 16.82 -5 -22 0 91.18 15.36 -5 22 0 77.15 14.48 -5 22 0 71.20 16.77 -6 -22 0 -2.89 11.04 6 -22 0 -14.32 12.96 -6 22 0 1.36 11.29 7 -22 0 48.23 16.47 -7 22 0 48.31 13.96 8 -22 0 90.93 18.88 -8 -22 0 78.45 16.65 -8 22 0 52.94 15.04 9 -22 0 0.95 14.50 -9 -22 0 11.30 14.46 -9 22 0 -1.78 14.33 -10 -22 0 137.20 23.73 -10 22 0 116.82 21.22 -11 -22 0 14.29 18.88 11 -22 0 -35.61 16.30 -11 22 0 0.69 17.02 12 -22 0 81.43 23.44 -12 -22 0 96.19 24.00 -12 22 0 89.19 24.57 13 -22 0 5.45 23.44 -13 -22 0 -4.75 23.77 -13 22 0 22.28 22.29 0 -23 0 -0.20 8.76 0 -23 0 8.35 8.96 0 23 0 26.18 17.24 0 23 0 3.80 7.15 -1 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3 234.41 18.95 3 10 -3 242.26 13.74 -2 -10 3 673.83 37.05 2 -10 -3 712.56 38.52 -2 -10 3 670.59 36.78 -2 10 3 700.52 38.44 -2 10 3 634.31 40.81 2 10 -3 712.58 36.91 2 10 -3 699.65 36.70 -1 -10 3 2069.35 107.00 1 -10 -3 2400.88 111.72 1 -10 -3 2188.71 108.91 -1 -10 3 2207.73 108.18 -1 10 3 2098.33 108.86 1 10 -3 2018.48 108.99 -1 10 3 1757.75 110.58 0 -10 3 1875.03 98.69 0 -10 3 2014.58 100.57 0 10 -3 1996.35 100.53 0 10 3 2211.83 104.35 0 10 3 1947.94 100.75 0 10 -3 1668.04 99.26 -1 -10 -3 6.02 3.74 -1 -10 -3 -1.10 3.54 1 -10 3 3.01 2.41 1 -10 3 7.22 4.03 -1 10 -3 6.00 3.39 -1 10 -3 2.28 2.43 1 10 3 3.85 4.92 -2 -10 -3 12.15 4.43 -2 -10 -3 8.53 4.86 -2 -10 -3 13.04 5.95 2 -10 3 4.88 3.59 2 -10 3 7.60 2.57 2 -10 3 8.38 4.91 -2 10 -3 7.21 3.90 2 10 3 7.03 4.17 -3 -10 -3 173.60 14.76 3 -10 3 185.12 14.30 -3 -10 -3 167.03 13.03 3 -10 3 178.10 11.63 3 -10 3 181.70 13.47 -3 -10 -3 196.60 15.59 -3 10 -3 185.07 14.32 3 10 3 176.63 13.36 -4 -10 -3 -5.47 5.34 4 -10 3 -5.67 5.39 -4 -10 -3 -9.97 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7 -12 -3 98.54 12.87 7 12 -3 87.82 12.02 -7 12 3 84.33 11.91 6 -12 -3 -5.95 6.38 -6 -12 3 3.98 5.32 6 -12 -3 5.55 6.49 -6 12 3 0.75 8.30 -6 12 3 -1.49 5.66 6 12 -3 -4.53 4.99 5 -12 -3 87.34 11.43 -5 -12 3 88.20 10.13 5 -12 -3 75.52 11.00 5 12 -3 80.10 5.67 5 12 -3 79.04 5.19 -5 12 3 97.93 14.17 -5 12 3 80.69 10.65 5 12 -3 95.13 10.30 -4 -12 3 1522.79 77.78 4 -12 -3 1441.86 79.91 -4 -12 3 1430.37 78.85 4 -12 -3 1497.71 81.15 4 12 -3 1497.53 76.39 -4 12 3 1424.73 79.83 -4 12 3 1621.31 83.84 4 12 -3 1575.74 79.10 3 -12 -3 7.23 6.55 3 -12 -3 26.47 6.55 -3 -12 3 17.05 4.83 -3 -12 3 26.06 4.94 -3 12 3 13.28 7.99 -3 12 3 25.79 5.64 3 12 -3 21.80 4.80 3 12 -3 16.46 3.60 2 -12 -3 13.58 6.18 -2 -12 3 4.52 3.86 2 -12 -3 3.74 4.56 -2 -12 3 8.56 4.79 -2 12 3 8.70 4.47 2 12 -3 10.31 3.62 -2 12 3 6.73 6.95 2 12 -3 13.70 4.03 1 -12 -3 149.28 12.00 -1 -12 3 122.76 12.01 1 -12 -3 156.20 13.91 -1 -12 3 137.80 10.06 -1 12 3 139.81 11.43 -1 12 3 155.37 15.60 1 12 -3 135.44 10.56 0 -12 3 444.28 24.60 0 -12 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3 207.88 20.15 -4 13 3 180.31 14.80 4 13 -3 179.20 13.79 -3 -13 3 584.43 32.28 3 -13 -3 561.51 33.38 3 -13 -3 491.78 34.95 -3 -13 3 568.70 31.49 3 13 -3 548.52 30.54 3 13 -3 576.98 32.11 -3 13 3 586.84 37.90 -3 13 3 612.96 33.72 -2 -13 3 173.50 12.39 2 -13 -3 164.98 13.72 -2 -13 3 174.20 12.63 2 -13 -3 198.64 16.52 2 13 -3 169.96 13.78 -2 13 3 148.62 17.29 -2 13 3 173.63 13.64 1 -13 -3 88.92 11.95 1 -13 -3 87.54 9.90 -1 -13 3 86.22 8.91 1 13 -3 77.42 8.31 -1 13 3 92.90 13.73 -1 13 3 73.90 8.72 0 -13 -3 303.43 19.52 0 -13 3 308.07 19.50 0 -13 3 313.64 17.98 0 13 -3 257.75 18.96 0 13 -3 300.83 19.05 0 13 3 339.90 19.91 -1 -13 -3 2027.04 100.92 -1 -13 -3 1679.80 102.88 1 -13 3 1918.28 99.55 1 -13 3 2080.65 101.78 -1 13 -3 2022.86 100.41 1 13 3 2008.82 101.38 1 13 3 1767.14 103.56 -1 13 -3 2033.58 101.64 -2 -13 -3 854.38 52.36 -2 -13 -3 924.76 50.65 2 -13 3 957.73 50.94 -2 13 -3 907.68 49.04 -2 13 -3 922.01 50.76 2 13 3 924.77 51.72 3 -13 3 511.02 31.88 -3 -13 -3 527.20 33.89 -3 -13 -3 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6.86 -4 -3 -6 9.68 7.46 -4 -3 -6 7.86 5.02 4 3 6 11.18 7.67 -4 3 -6 7.69 6.81 -4 3 -6 5.90 4.28 4 3 6 2.28 4.00 -5 -3 -6 721.74 42.77 5 -3 6 713.06 42.84 5 -3 6 715.72 39.20 -5 -3 -6 716.21 42.24 -5 3 -6 685.33 42.53 -5 3 -6 740.49 40.57 5 3 6 685.35 43.23 5 3 6 723.19 40.15 -6 -3 -6 116.07 14.87 -6 -3 -6 145.14 14.97 6 -3 6 111.74 11.30 6 -3 6 127.17 15.84 -6 3 -6 113.19 12.44 -6 3 -6 121.70 15.27 6 3 6 109.46 12.29 6 3 6 96.77 14.17 7 -3 6 104.30 11.98 -7 -3 -6 93.63 13.81 -7 -3 -6 106.40 14.38 7 3 6 126.49 15.73 -7 3 -6 99.63 14.85 7 3 6 100.63 12.15 -7 3 -6 93.07 13.27 8 -3 6 0.35 6.88 -8 -3 -6 14.30 9.76 -8 -3 -6 -2.54 8.44 -8 3 -6 -0.75 8.73 -8 3 -6 -10.31 7.05 8 3 6 -0.57 10.78 8 3 6 4.51 8.32 -9 -3 -6 325.68 27.23 -9 -3 -6 306.23 25.36 9 -3 6 275.37 23.29 9 3 6 298.28 32.97 -9 3 -6 290.07 25.04 -9 3 -6 286.24 25.24 -10 -3 -6 234.94 25.60 -10 -3 -6 215.10 23.10 -10 3 -6 198.84 23.54 -10 3 -6 234.74 23.60 -11 -3 -6 26.72 14.93 -11 -3 -6 0.69 12.30 -11 3 -6 19.79 12.52 -12 -3 -6 319.30 33.67 -12 -3 -6 279.34 31.10 -12 3 -6 343.54 34.11 -12 3 -6 360.30 34.38 -13 -3 -6 433.84 40.99 -13 3 -6 322.08 37.41 -13 3 -6 479.99 39.71 -14 -3 -6 72.58 23.99 -14 -3 -6 34.84 20.27 -14 3 -6 31.74 20.96 -14 3 -6 49.66 21.60 -18 -4 6 2.38 17.48 18 -4 -6 -28.07 30.37 -18 4 6 3.16 24.10 -17 -4 6 117.78 22.49 -17 -4 6 118.98 21.76 17 -4 -6 178.93 34.16 -17 4 6 141.22 25.13 16 -4 -6 8.45 21.02 -16 -4 6 18.01 15.62 -16 -4 6 16.52 15.56 -16 4 6 21.27 17.51 -15 -4 6 4.21 13.39 -15 -4 6 -11.42 12.95 15 -4 -6 -31.39 19.12 -14 -4 6 68.23 14.86 -14 -4 6 138.49 16.85 -14 4 6 91.10 16.84 14 4 -6 80.98 15.29 -13 -4 6 171.78 19.96 13 4 -6 157.41 19.04 -13 4 6 170.54 21.47 -12 -4 6 81.44 12.99 -12 -4 6 85.44 13.02 -12 4 6 127.77 16.17 12 4 -6 102.75 13.12 11 -4 -6 2042.92 110.78 -11 -4 6 2021.40 107.13 11 -4 -6 1884.01 107.14 -11 -4 6 2010.49 105.92 -11 4 6 2014.84 107.54 11 4 -6 1971.71 104.94 -10 -4 6 896.55 50.72 10 -4 -6 889.23 54.41 -10 -4 6 904.40 51.10 10 -4 -6 835.43 51.22 -10 4 6 898.99 51.67 10 4 -6 852.47 52.56 10 4 -6 914.33 49.84 9 -4 -6 495.11 32.32 -9 -4 6 492.45 31.28 9 -4 -6 521.88 34.00 -9 -4 6 512.77 31.25 9 -4 -6 461.03 32.66 9 4 -6 499.52 30.20 9 4 -6 496.85 32.71 -9 4 6 512.56 32.11 -8 -4 6 425.40 27.13 8 -4 -6 420.41 29.07 8 -4 -6 439.03 29.74 -8 -4 6 441.92 27.89 8 -4 -6 428.75 28.62 8 4 -6 402.33 28.40 -8 4 6 453.45 28.80 8 4 -6 466.17 27.08 7 -4 -6 359.52 24.67 -7 -4 6 361.15 22.97 7 -4 -6 389.42 25.58 7 -4 -6 348.09 25.21 7 4 -6 355.21 25.07 7 4 -6 381.07 24.56 7 4 -6 376.84 23.58 -7 4 6 360.33 24.32 6 -4 -6 321.07 22.34 6 -4 -6 285.74 21.78 6 -4 -6 316.92 22.27 -6 -4 6 332.44 20.53 6 4 -6 363.85 22.07 6 4 -6 319.52 23.16 -6 4 6 326.00 21.85 6 4 -6 340.67 21.53 5 -4 -6 159.80 15.09 -5 -4 6 159.48 11.92 5 -4 -6 166.66 14.41 5 -4 -6 154.99 13.57 -5 4 6 187.67 14.65 5 4 -6 165.68 14.38 5 4 -6 172.54 13.08 5 4 -6 162.39 15.22 -5 4 6 164.96 17.13 4 -4 -6 117.66 10.95 4 -4 -6 116.53 11.90 -4 4 6 124.92 11.58 4 4 -6 110.05 13.16 -4 4 6 119.74 14.44 4 4 -6 135.06 13.25 4 4 -6 124.24 10.02 3 -4 -6 224.01 16.89 -3 -4 6 200.99 17.75 3 -4 -6 216.90 15.37 3 4 -6 229.56 17.35 -3 4 6 220.50 16.40 3 4 -6 217.14 13.58 -3 4 6 218.30 17.53 3 4 -6 200.83 13.54 2 -4 -6 137.08 13.12 2 -4 -6 123.03 12.32 2 -4 -6 139.63 13.57 -2 -4 6 144.58 14.29 2 4 -6 137.27 9.19 -2 4 6 161.52 14.41 2 4 -6 140.86 13.25 2 4 -6 146.45 9.31 1 -4 -6 389.93 24.56 -1 -4 6 352.50 23.42 1 -4 -6 352.76 23.71 1 4 -6 311.86 18.79 1 4 -6 353.40 18.53 -1 4 6 306.28 22.42 1 4 -6 341.94 23.38 0 -4 -6 456.69 29.14 0 -4 -6 372.24 25.74 0 -4 6 444.20 28.00 0 -4 -6 465.01 28.35 0 -4 6 468.84 23.57 0 4 -6 430.33 22.86 0 4 6 418.35 28.40 0 4 -6 409.39 27.22 1 -4 6 922.51 43.47 -1 -4 -6 770.14 45.91 -1 -4 -6 862.53 48.64 1 -4 6 825.81 47.34 -1 4 -6 799.57 47.04 1 4 6 732.41 45.44 -1 4 -6 858.60 42.94 1 4 6 838.32 48.53 -2 -4 -6 1544.03 77.94 -2 -4 -6 1352.90 74.96 2 -4 6 1414.75 71.46 2 -4 6 1367.89 75.95 -2 4 -6 1419.86 72.16 2 4 6 1353.73 76.45 2 4 6 1364.05 73.50 -2 4 -6 1399.70 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3 -17 64.62 28.80 7 -3 -17 469.27 49.62 7 -3 -17 482.67 35.55 7 3 -17 336.38 44.65 6 -3 -17 65.11 25.37 6 3 -17 52.19 29.04 5 -3 -17 89.88 14.87 5 -3 -17 51.72 27.52 5 3 -17 77.97 32.52 4 -3 -17 -4.67 11.28 4 -3 -17 -27.18 22.57 4 3 -17 21.16 25.15 3 -3 -17 33.56 13.17 3 -3 -17 13.87 28.95 3 3 -17 29.49 26.87 2 -3 -17 28.73 28.08 2 -3 -17 16.49 13.66 2 3 -17 23.32 26.05 1 -3 -17 33.58 26.15 1 -3 -17 36.09 15.94 1 3 -17 12.46 28.06 0 -3 -17 -22.24 27.45 0 3 -17 -5.98 26.08 -1 -3 -17 67.53 28.49 -1 3 -17 126.88 29.89 11 -4 -17 17.20 20.49 11 -4 -17 4.32 28.25 11 4 -17 53.33 32.90 11 4 -17 27.00 17.71 10 -4 -17 265.25 38.54 10 -4 -17 321.06 36.50 10 4 -17 299.13 43.77 9 -4 -17 6.76 26.82 9 -4 -17 18.77 18.28 9 4 -17 -27.76 29.37 8 -4 -17 32.07 28.46 8 -4 -17 66.00 17.73 8 4 -17 47.87 28.08 7 -4 -17 32.56 15.19 7 -4 -17 19.64 25.72 7 4 -17 24.26 28.88 6 -4 -17 233.96 36.08 6 4 -17 261.33 39.20 5 -4 -17 25.28 16.51 5 -4 -17 21.22 25.78 5 4 -17 0.19 26.21 4 -4 -17 6.89 12.26 4 -4 -17 0.83 21.99 4 4 -17 -20.08 25.93 3 -4 -17 -25.12 25.63 3 -4 -17 -10.65 12.06 3 4 -17 -14.67 26.47 2 -4 -17 -0.55 27.75 2 -4 -17 -3.02 13.55 2 4 -17 7.83 25.46 1 -4 -17 -11.01 14.75 1 -4 -17 17.10 26.62 1 4 -17 24.29 29.18 0 -4 -17 188.92 24.64 0 -4 -17 188.34 33.84 0 4 -17 126.55 31.00 -1 -4 -17 82.06 31.24 -1 4 -17 142.00 30.68 11 -5 -17 178.09 26.37 11 -5 -17 174.53 35.55 11 5 -17 75.22 35.67 10 -5 -17 50.91 20.04 10 -5 -17 16.34 26.29 10 5 -17 34.29 34.19 9 -5 -17 44.59 28.18 9 -5 -17 61.47 20.69 9 5 -17 80.20 32.18 8 -5 -17 -34.05 26.11 8 -5 -17 27.44 16.20 8 5 -17 -53.13 28.30 7 -5 -17 355.39 32.10 7 -5 -17 324.11 42.01 7 5 -17 266.92 42.15 6 -5 -17 -15.61 26.77 6 -5 -17 44.76 14.47 6 5 -17 -11.51 26.43 5 -5 -17 83.21 15.38 5 -5 -17 111.37 29.68 5 5 -17 76.04 27.43 4 -5 -17 -8.30 23.78 4 -5 -17 -3.28 11.70 4 5 -17 16.46 24.77 3 -5 -17 -15.34 23.68 3 -5 -17 3.34 13.31 3 5 -17 -30.53 23.88 2 -5 -17 -21.01 23.29 2 -5 -17 -19.00 18.25 2 5 -17 -24.71 26.32 1 -5 -17 27.39 26.45 1 -5 -17 56.14 20.39 1 5 -17 50.02 27.17 0 -5 -17 -4.97 16.81 0 -5 -17 25.33 28.18 0 5 -17 11.92 28.20 -1 -5 -17 166.59 36.03 -1 -5 -17 194.57 40.54 -1 5 -17 138.80 32.99 10 -6 -17 67.05 23.28 10 -6 -17 61.18 32.24 10 6 -17 134.24 36.44 9 -6 -17 0.35 29.38 9 -6 -17 -9.83 19.08 9 6 -17 -43.17 30.65 8 -6 -17 73.86 28.34 8 6 -17 36.43 30.66 7 -6 -17 52.91 16.07 7 -6 -17 62.55 28.96 7 6 -17 -16.02 28.37 6 -6 -17 95.99 16.12 6 -6 -17 42.08 28.63 6 6 -17 85.76 29.62 5 -6 -17 77.90 15.38 5 -6 -17 54.42 25.46 5 6 -17 32.40 28.59 4 -6 -17 64.02 29.51 4 -6 -17 61.80 14.74 4 6 -17 34.08 29.33 3 -6 -17 110.19 17.90 3 -6 -17 104.69 30.63 3 6 -17 105.01 31.64 2 -6 -17 10.17 14.42 2 -6 -17 -64.94 26.48 2 6 -17 -2.13 24.49 1 -6 -17 -0.10 15.95 1 -6 -17 4.22 27.52 1 6 -17 -3.01 25.93 0 -6 -17 125.49 33.66 0 -6 -17 215.82 26.34 0 6 -17 235.82 39.51 -1 -6 -17 9.48 30.14 -1 -6 -17 -24.71 19.28 -1 6 -17 -28.00 27.30 10 -7 -17 20.46 29.56 10 -7 -17 0.14 22.89 10 7 -17 -36.73 31.22 9 -7 -17 -3.80 25.88 9 -7 -17 20.32 20.84 9 7 -17 36.53 33.29 8 -7 -17 48.95 18.26 8 -7 -17 -27.72 26.39 8 7 -17 27.39 32.57 7 -7 -17 65.82 27.10 7 -7 -17 30.50 15.47 7 7 -17 34.34 28.46 6 -7 -17 148.58 31.78 6 -7 -17 185.10 26.71 6 7 -17 203.43 36.19 5 -7 -17 41.86 14.29 5 -7 -17 12.30 26.50 5 7 -17 10.29 28.82 4 -7 -17 50.59 13.91 4 -7 -17 66.79 26.51 4 7 -17 22.29 27.36 3 -7 -17 74.96 28.42 3 -7 -17 49.88 15.81 3 7 -17 40.99 29.14 2 -7 -17 113.82 32.32 2 -7 -17 134.47 20.38 2 7 -17 159.24 32.11 1 -7 -17 -24.79 25.46 1 -7 -17 13.20 16.22 1 7 -17 -4.53 27.44 0 -7 -17 13.40 18.27 0 -7 -17 -49.02 26.94 0 7 -17 -15.54 26.17 10 -8 -17 19.55 22.14 10 -8 -17 29.40 31.08 10 8 -17 35.35 33.01 9 -8 -17 25.09 22.08 9 -8 -17 30.86 29.62 9 8 -17 40.83 33.42 8 -8 -17 7.43 26.21 8 -8 -17 -9.17 16.76 8 8 -17 -2.18 30.22 7 -8 -17 123.35 32.65 7 -8 -17 165.71 21.70 7 8 -17 125.48 31.61 6 -8 -17 -7.76 27.52 6 -8 -17 25.54 15.18 6 8 -17 2.22 28.19 5 -8 -17 34.89 14.54 5 -8 -17 56.79 27.43 5 8 -17 -12.89 27.34 4 -8 -17 200.05 33.14 4 -8 -17 190.42 25.95 4 8 -17 90.00 29.52 3 -8 -17 181.14 33.84 3 -8 -17 285.45 29.86 3 8 -17 243.86 36.57 2 -8 -17 -44.55 25.39 2 -8 -17 23.38 15.51 2 8 -17 -16.60 24.81 1 -8 -17 8.08 28.93 1 -8 -17 39.96 16.87 1 8 -17 35.15 28.23 0 -8 -17 -2.39 18.13 0 -8 -17 -17.25 25.71 0 8 -17 -3.95 28.32 9 -9 -17 23.84 21.29 9 -9 -17 26.48 26.66 9 9 -17 -35.08 30.30 8 -9 -17 107.88 22.25 8 -9 -17 48.49 29.36 8 9 -17 106.72 30.66 7 -9 -17 81.26 28.45 7 -9 -17 18.86 16.47 7 9 -17 -26.88 28.18 6 -9 -17 119.62 30.28 6 -9 -17 205.27 27.22 6 9 -17 151.78 36.20 5 -9 -17 13.07 14.64 5 -9 -17 12.28 27.51 5 9 -17 4.73 27.05 4 -9 -17 47.71 15.55 4 -9 -17 31.11 25.62 4 9 -17 14.87 27.89 3 -9 -17 16.72 24.65 3 -9 -17 25.18 15.74 3 9 -17 29.41 28.86 2 -9 -17 131.96 20.88 2 -9 -17 93.70 28.56 2 9 -17 113.81 32.44 1 -9 -17 59.26 29.16 1 -9 -17 62.52 18.51 1 9 -17 51.96 31.74 0 -9 -17 31.91 19.03 0 -9 -17 -5.96 28.71 0 9 -17 -23.18 29.27 9 -10 -17 116.18 34.42 9 -10 -17 116.86 23.56 9 10 -17 125.69 37.82 8 -10 -17 -17.89 26.11 8 -10 -17 24.35 19.35 8 10 -17 -35.25 30.05 7 -10 -17 174.48 24.33 7 -10 -17 142.29 30.27 7 10 -17 109.61 35.04 6 -10 -17 40.54 26.75 6 -10 -17 66.98 17.50 6 10 -17 57.14 31.16 5 -10 -17 -8.81 13.89 5 -10 -17 54.96 26.95 5 10 -17 15.29 28.51 4 -10 -17 58.06 28.30 4 -10 -17 76.66 17.01 4 10 -17 8.56 28.38 3 -10 -17 83.08 18.12 3 -10 -17 121.44 31.61 3 10 -17 42.07 30.72 2 -10 -17 6.54 28.83 2 -10 -17 33.30 17.25 2 10 -17 -18.04 28.76 1 -10 -17 15.14 17.20 1 -10 -17 14.12 28.07 1 10 -17 1.96 30.28 8 -11 -17 13.92 28.31 8 -11 -17 63.21 21.62 8 11 -17 77.11 32.42 7 -11 -17 88.68 31.09 7 -11 -17 103.43 21.24 7 11 -17 47.77 30.46 6 -11 -17 6.06 28.68 6 -11 -17 25.75 16.94 6 11 -17 -4.20 27.87 5 -11 -17 0.96 15.73 5 -11 -17 13.77 25.93 5 11 -17 10.01 28.18 4 -11 -17 -48.68 27.62 4 -11 -17 28.39 15.94 4 11 -17 -26.10 27.54 3 -11 -17 23.00 28.59 3 -11 -17 -5.27 15.67 3 11 -17 -20.77 29.31 2 -11 -17 12.67 29.13 2 -11 -17 -4.08 16.52 2 11 -17 -17.92 27.85 7 -12 -17 2.84 28.41 7 -12 -17 57.37 19.92 7 12 -17 20.97 31.85 6 -12 -17 234.91 37.93 6 -12 -17 269.83 31.67 6 12 -17 145.10 37.09 5 -12 -17 -8.99 24.68 5 -12 -17 8.72 15.78 5 12 -17 34.76 31.71 4 -12 -17 42.26 17.10 4 -12 -17 35.98 29.77 4 12 -17 46.07 30.88 3 -12 -17 -6.24 26.56 3 -12 -17 2.25 16.51 3 12 -17 7.61 30.65 8 0 -18 -1.97 29.73 7 0 -18 3.10 29.43 6 0 -18 -30.58 30.68 5 0 -18 11.91 31.07 4 0 -18 317.46 45.17 3 0 -18 51.13 29.14 2 0 -18 230.21 38.28 8 -1 -18 22.83 28.57 8 -1 -18 15.66 16.53 8 1 -18 -19.54 31.74 7 -1 -18 -23.00 30.86 7 1 -18 34.19 29.28 6 -1 -18 -5.49 31.52 6 1 -18 41.75 31.71 5 -1 -18 14.74 32.18 5 1 -18 5.60 32.19 4 -1 -18 32.26 31.74 4 1 -18 71.68 30.23 3 -1 -18 286.67 40.38 3 1 -18 263.04 38.88 2 -1 -18 -35.07 28.91 2 1 -18 53.37 31.76 8 -2 -18 8.28 15.76 8 -2 -18 -32.32 28.88 8 2 -18 31.00 32.01 7 -2 -18 91.85 17.12 7 -2 -18 138.70 36.37 7 2 -18 133.02 36.09 6 -2 -18 22.19 30.03 6 -2 -18 5.46 13.51 6 2 -18 -31.08 27.51 5 -2 -18 30.96 29.95 5 2 -18 35.21 28.84 4 -2 -18 85.88 32.80 4 2 -18 100.16 30.21 3 -2 -18 195.15 34.82 3 2 -18 151.25 33.21 2 -2 -18 106.71 31.64 2 2 -18 54.71 32.88 8 -3 -18 -53.29 28.49 8 -3 -18 20.99 16.72 8 3 -18 37.53 33.91 7 -3 -18 -8.01 29.59 7 -3 -18 26.09 15.09 7 3 -18 -36.21 30.86 6 -3 -18 23.32 31.08 6 -3 -18 48.24 14.80 6 3 -18 19.18 30.66 5 -3 -18 14.66 13.14 5 -3 -18 35.04 30.13 5 3 -18 -20.89 28.02 4 -3 -18 131.34 33.68 4 3 -18 60.07 30.33 3 -3 -18 98.34 31.51 3 3 -18 58.07 31.64 2 -3 -18 34.48 28.03 2 3 -18 103.22 33.75 8 -4 -18 -9.80 15.78 8 -4 -18 -10.98 31.92 8 4 -18 1.84 34.48 7 -4 -18 75.42 16.98 7 -4 -18 35.98 29.01 7 4 -18 50.14 34.23 6 -4 -18 21.40 13.93 6 -4 -18 25.77 29.83 6 4 -18 -34.34 30.46 5 -4 -18 -17.63 27.96 5 -4 -18 5.30 13.25 5 4 -18 15.38 30.81 4 -4 -18 -50.41 26.38 4 -4 -18 8.60 14.34 4 4 -18 2.01 31.57 3 -4 -18 202.57 38.47 3 4 -18 157.05 37.42 2 -4 -18 -10.63 28.99 2 4 -18 -3.30 30.98 7 -5 -18 -18.74 27.38 7 -5 -18 10.83 15.01 7 5 -18 28.29 34.06 6 -5 -18 -8.59 12.95 6 -5 -18 8.30 28.63 6 5 -18 55.52 33.09 5 -5 -18 -7.48 26.42 5 -5 -18 22.57 13.28 5 5 -18 -7.29 27.62 4 -5 -18 105.20 18.60 4 -5 -18 89.35 32.38 4 5 -18 29.81 29.76 3 -5 -18 27.54 16.69 3 -5 -18 -15.10 29.37 3 5 -18 10.00 28.06 7 -6 -18 -38.74 30.21 7 -6 -18 13.39 15.31 7 6 -18 -7.35 33.41 6 -6 -18 -4.87 29.94 6 -6 -18 -10.25 13.45 6 6 -18 10.60 29.74 5 -6 -18 -15.67 29.38 5 -6 -18 19.06 13.47 5 6 -18 -3.55 33.33 4 -6 -18 52.72 16.30 4 -6 -18 39.64 28.09 4 6 -18 12.51 32.21 3 -6 -18 44.17 33.30 3 6 -18 3.56 31.11 6 -7 -18 19.42 29.28 6 7 -18 50.80 36.61 5 -7 -18 49.74 27.40 5 -7 -18 47.35 14.37 5 7 -18 -5.50 30.25 4 -7 -18 -49.29 29.29 4 7 -18 -0.89 29.35 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4217 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71055 14.001 25.544 14.207 90.034 106.628 89.915 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 24756 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.75785(2) 0.52080(2) 0.60428(3) 0.03750(10) Uani 1 1 d . . . . . W2 W 0.63756(3) 0.57068(2) 0.36806(3) 0.03192(9) Uani 1 1 d . . . . . W3 W 0.53973(3) 0.44589(2) 0.28574(2) 0.02962(9) Uani 1 1 d . . . . . W4 W 0.37687(2) 0.55338(2) 0.26677(2) 0.02574(8) Uani 1 1 d . . . . . W5 W 0.32996(3) 0.60481(2) 0.48076(3) 0.03562(10) Uani 1 1 d . . . . . W6 W 0.5973(6) 0.62368(15) 0.5871(5) 0.0368(7) Uani 0.3333 1 d . . P . . W6' W 0.5730(2) 0.62773(11) 0.5802(4) 0.0203(6) Uiso 0.3333 1 d . . P . . W6'' W 0.5970(4) 0.62649(12) 0.56451(18) 0.0198(6) Uiso 0.3333 1 d . . P . . K1 K 0.96090(17) 0.64252(9) 0.70622(17) 0.0497(6) Uani 1 1 d . . . . . Si1 Si 0.500000 0.500000 0.500000 0.0157(6) Uani 1 2 d S . P . . O1 O 0.8806(4) 0.5315(3) 0.6527(5) 0.0510(18) Uani 1 1 d . . . . . O2 O 0.6317(5) 0.6859(2) 0.6161(5) 0.0451(17) Uani 1 1 d . . . . . O3 O 0.7067(8) 0.5851(4) 0.6307(5) 0.108(4) Uani 1 1 d . . . . . O4 O 0.7409(8) 0.5433(3) 0.4715(5) 0.100(4) Uani 1 1 d . . . . . O5 O 0.7020(5) 0.6040(3) 0.3037(6) 0.058(2) Uani 1 1 d . . . . . O6 O 0.5599(5) 0.4196(3) 0.1849(5) 0.062(2) Uani 1 1 d . . . . . O7 O 0.4500(6) 0.3973(4) 0.3116(7) 0.105(4) Uani 1 1 d . . . . . O8 O 0.4321(4) 0.4910(2) 0.2305(6) 0.054(2) Uani 1 1 d . . . . . O9 O 0.2758(6) 0.5081(3) 0.2887(7) 0.078(3) Uani 1 1 d . . . . . O10 O 0.2412(6) 0.5479(3) 0.4470(6) 0.075(3) Uani 1 1 d . . . . . O11 O 0.2516(5) 0.6553(2) 0.4696(5) 0.0534(19) Uani 1 1 d . . . . . O12 O 0.3569(5) 0.5875(4) 0.6140(6) 0.096(4) Uani 1 1 d . . . . . O13 O 0.3431(6) 0.6018(3) 0.3505(6) 0.077(3) Uani 1 1 d . . . . . O14 O 0.3186(6) 0.5790(3) 0.1570(6) 0.077(3) Uani 1 1 d . . . . . O15 O 0.5033(4) 0.5844(2) 0.2915(6) 0.055(2) Uani 1 1 d . . . . . O16 O 0.6263(4) 0.5047(2) 0.3077(6) 0.0537(19) Uani 1 1 d . . . . . O17 O 0.4549(5) 0.6413(4) 0.5135(6) 0.103(4) Uani 1 1 d . . . . . O18 O 0.6157(8) 0.6229(4) 0.4554(5) 0.104(4) Uani 1 1 d . . . . . O19 O 0.5953(7) 0.5412(4) 0.5049(7) 0.019(2) Uiso 0.5 1 d . . P . . O19' O 0.4741(7) 0.5533(4) 0.5547(7) 0.018(2) Uiso 0.5 1 d . . P . . O20 O 0.5060(7) 0.5129(4) 0.3958(7) 0.020(2) Uiso 0.5 1 d . . P . . O20' O 0.4008(7) 0.5260(4) 0.4292(7) 0.019(2) Uiso 0.5 1 d . . P . . O21 O 0.8754(5) 0.7389(3) 0.5981(6) 0.059(2) Uani 1 1 d . . . . . O22 O 0.9084(5) 0.6508(3) 0.5005(5) 0.0547(19) Uani 1 1 d . . . . . O23 O 1.0753(5) 0.5918(3) 0.5957(5) 0.0531(18) Uani 1 1 d . . . . . O24 O 1.1392(5) 0.5876(3) 0.8009(6) 0.061(2) Uani 1 1 d . . . . . O25 O 1.1004(7) 0.6778(3) 0.8951(6) 0.073(2) Uani 1 1 d . . . . . O26 O 0.9360(7) 0.7400(3) 0.8038(6) 0.081(3) Uani 1 1 d . . . . . N1 N 0.8654(12) 0.6075(7) 0.8452(12) 0.136(5) Uiso 1 1 d D . . . . C13 C 1.1913(8) 0.5636(5) 0.7408(9) 0.067(3) Uani 1 1 d . . . . . H13A H 1.227849 0.533505 0.774687 0.081 Uiso 1 1 calc R U . . . H13B H 1.238989 0.588120 0.728041 0.081 Uiso 1 1 calc R U . . . C14 C 1.1219(8) 0.5469(4) 0.6481(9) 0.062(3) Uani 1 1 d . . . . . H14A H 1.157503 0.527887 0.609458 0.074 Uiso 1 1 calc R U . . . H14B H 1.071932 0.523763 0.660599 0.074 Uiso 1 1 calc R U . . . C15 C 1.0117(9) 0.5778(5) 0.5019(9) 0.063(3) Uani 1 1 d . . . . . H15A H 0.959573 0.554577 0.509551 0.076 Uiso 1 1 calc R U . . . H15B H 1.049684 0.559398 0.464819 0.076 Uiso 1 1 calc R U . . . C16 C 0.9665(9) 0.6256(5) 0.4481(8) 0.061(3) Uani 1 1 d . . . . . H16A H 1.018641 0.649024 0.441093 0.073 Uiso 1 1 calc R U . . . H16B H 0.925122 0.616293 0.382894 0.073 Uiso 1 1 calc R U . . . C17 C 0.8615(8) 0.6949(4) 0.4500(8) 0.057(3) Uani 1 1 d . . . . . H17A H 0.814433 0.684209 0.388475 0.068 Uiso 1 1 calc R U . . . H17B H 0.910926 0.717406 0.434859 0.068 Uiso 1 1 calc R U . . . C18 C 0.8085(7) 0.7243(4) 0.5087(8) 0.055(3) Uani 1 1 d . . . . . H18A H 0.777925 0.755258 0.472935 0.066 Uiso 1 1 calc R U . . . H18B H 0.756112 0.702695 0.520529 0.066 Uiso 1 1 calc R U . . . C19 C 0.8309(11) 0.7711(5) 0.6566(11) 0.088(5) Uani 1 1 d . . . . . H19A H 0.803029 0.802363 0.620072 0.106 Uiso 1 1 calc R U . . . H19B H 0.777249 0.752147 0.671914 0.106 Uiso 1 1 calc R U . . . C20 C 0.9035(13) 0.7854(5) 0.7447(13) 0.105(6) Uani 1 1 d . . . . . H20A H 0.875342 0.810556 0.780487 0.126 Uiso 1 1 calc R U . . . H20B H 0.959909 0.801755 0.729459 0.126 Uiso 1 1 calc R U . . . C21 C 1.0082(11) 0.7544(6) 0.8928(11) 0.094(5) Uani 1 1 d . . . . . H21A H 0.977860 0.776486 0.931810 0.112 Uiso 1 1 calc R U . . . H21B H 1.062011 0.773810 0.878559 0.112 Uiso 1 1 calc R U . . . C22 C 1.0473(12) 0.7061(6) 0.9473(10) 0.095(5) Uani 1 1 d . . . . . H22A H 1.090641 0.714881 1.011946 0.114 Uiso 1 1 calc R U . . . H22B H 0.992529 0.685083 0.955606 0.114 Uiso 1 1 calc R U . . . C23 C 1.1446(12) 0.6326(6) 0.9469(9) 0.088(5) Uani 1 1 d . . . . . H23A H 1.093613 0.608473 0.954318 0.106 Uiso 1 1 calc R U . . . H23B H 1.186981 0.641853 1.011657 0.106 Uiso 1 1 calc R U . . . C24 C 1.2041(10) 0.6084(5) 0.8877(10) 0.079(4) Uani 1 1 d . . . . . H24A H 1.247169 0.634510 0.871507 0.095 Uiso 1 1 calc R U . . . H24B H 1.245646 0.580786 0.925163 0.095 Uiso 1 1 calc R U . . . C25 C 0.8049(17) 0.6366(9) 0.853(2) 0.183(10) Uiso 1 1 d D . . . . C26 C 0.726(2) 0.6682(11) 0.880(2) 0.259(15) Uiso 1 1 d D . . . . H26A H 0.756390 0.690268 0.934879 0.389 Uiso 1 1 calc R U . . . H26B H 0.679432 0.644911 0.896901 0.389 Uiso 1 1 calc R U . . . H26C H 0.690813 0.689431 0.824865 0.389 Uiso 1 1 calc R U . . . K2 K 0.20006(18) 0.35744(11) -0.1592(2) 0.0698(8) Uani 1 1 d . . . . . O27 O 0.3664(6) 0.4033(3) -0.0283(5) 0.062(2) Uani 1 1 d . . . . . O28 O 0.1829(8) 0.4556(4) -0.0804(7) 0.087(3) Uani 1 1 d . . . . . O29 O 0.0079(7) 0.3944(5) -0.1577(8) 0.104(3) Uani 1 1 d . . . . . O30 O 0.0234(6) 0.2964(5) -0.2367(7) 0.097(3) Uani 1 1 d . . . . . O31 O 0.2097(8) 0.2484(4) -0.1725(9) 0.104(3) Uani 1 1 d . . . . . O32 O 0.3828(6) 0.3044(4) -0.1033(7) 0.078(2) Uani 1 1 d . . . . . C1 C 0.4620(9) 0.3288(6) -0.0322(10) 0.087(4) Uani 1 1 d . . . . . H1A H 0.525416 0.316168 -0.038043 0.104 Uiso 1 1 calc R U . . . H1B H 0.458172 0.320577 0.033289 0.104 Uiso 1 1 calc R U . . . C2 C 0.4549(9) 0.3861(6) -0.0480(9) 0.079(4) Uani 1 1 d . . . . . H2A H 0.512432 0.403329 -0.004257 0.094 Uiso 1 1 calc R U . . . H2B H 0.452673 0.394280 -0.115267 0.094 Uiso 1 1 calc R U . . . C3 C 0.3596(11) 0.4582(5) -0.0256(10) 0.083(4) Uani 1 1 d . . . . . H3A H 0.358925 0.473015 -0.088734 0.099 Uiso 1 1 calc R U . . . H3B H 0.416342 0.472438 0.024303 0.099 Uiso 1 1 calc R U . . . C4 C 0.2654(13) 0.4711(5) -0.0023(13) 0.103(5) Uani 1 1 d . . . . . H4A H 0.263727 0.453180 0.057485 0.124 Uiso 1 1 calc R U . . . H4B H 0.262187 0.508473 0.008506 0.124 Uiso 1 1 calc R U . . . C5 C 0.0885(14) 0.4681(6) -0.0669(14) 0.108(6) Uani 1 1 d . . . . . H5A H 0.083711 0.505608 -0.058025 0.130 Uiso 1 1 calc R U . . . H5B H 0.081095 0.450643 -0.008818 0.130 Uiso 1 1 calc R U . . . C6 C 0.0062(13) 0.4502(9) -0.1581(16) 0.133(8) Uani 1 1 d . . . . . H6A H -0.058314 0.462855 -0.155357 0.160 Uiso 1 1 calc R U . . . H6B H 0.018623 0.463526 -0.217404 0.160 Uiso 1 1 calc R U . . . C7 C -0.0706(11) 0.3727(10) -0.2323(12) 0.126(9) Uani 1 1 d . . . . . H7A H -0.066114 0.384488 -0.295870 0.151 Uiso 1 1 calc R U . . . H7B H -0.133855 0.384540 -0.224859 0.151 Uiso 1 1 calc R U . . . C8 C -0.0666(11) 0.3161(10) -0.2284(12) 0.122(8) Uani 1 1 d . . . . . H8A H -0.075948 0.304414 -0.166655 0.146 Uiso 1 1 calc R U . . . H8B H -0.120860 0.301985 -0.281260 0.146 Uiso 1 1 calc R U . . . C9 C 0.0352(13) 0.2423(8) -0.2182(13) 0.122(7) Uani 1 1 d . . . . . H9A H -0.018423 0.223826 -0.264985 0.147 Uiso 1 1 calc R U . . . H9B H 0.029581 0.235265 -0.152877 0.147 Uiso 1 1 calc R U . . . C10 C 0.1321(15) 0.2218(7) -0.2250(14) 0.119(6) Uani 1 1 d . . . . . H10A H 0.138790 0.185596 -0.203238 0.143 Uiso 1 1 calc R U . . . H10B H 0.131963 0.222269 -0.293378 0.143 Uiso 1 1 calc R U . . . C11 C 0.3024(12) 0.2271(6) -0.1694(14) 0.105(5) Uani 1 1 d . . . . . H11A H 0.316700 0.233896 -0.231230 0.126 Uiso 1 1 calc R U . . . H11B H 0.300738 0.189493 -0.160733 0.126 Uiso 1 1 calc R U . . . C12 C 0.3809(12) 0.2499(6) -0.0888(14) 0.111(6) Uani 1 1 d . . . . . H12A H 0.367818 0.242543 -0.026567 0.133 Uiso 1 1 calc R U . . . H12B H 0.444880 0.234719 -0.087052 0.133 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01871(17) 0.0455(2) 0.0413(2) -0.01429(18) -0.00253(15) 0.00467(16) W2 0.0435(2) 0.03004(19) 0.02588(19) 0.00406(15) 0.01578(16) 0.00350(16) W3 0.03050(18) 0.0381(2) 0.02070(18) -0.00218(15) 0.00806(14) -0.00669(16) W4 0.02538(17) 0.03024(18) 0.02029(17) 0.00369(14) 0.00449(13) 0.00230(15) W5 0.02397(18) 0.02618(19) 0.0549(3) 0.00790(17) 0.00854(17) 0.00680(15) W6 0.046(2) 0.0174(11) 0.0300(18) 0.0031(11) -0.0169(11) -0.0053(11) K1 0.0586(14) 0.0476(13) 0.0434(13) -0.0055(11) 0.0157(11) 0.0059(11) Si1 0.0137(13) 0.0146(14) 0.0178(15) -0.0006(12) 0.0028(11) 0.0011(11) O1 0.032(4) 0.083(5) 0.037(4) -0.008(4) 0.008(3) -0.022(4) O2 0.059(4) 0.032(3) 0.051(4) -0.014(3) 0.027(3) -0.017(3) O3 0.175(10) 0.100(7) 0.023(4) -0.016(4) -0.010(5) 0.104(7) O4 0.156(9) 0.096(7) 0.027(4) -0.010(4) -0.005(5) 0.097(6) O5 0.041(4) 0.047(4) 0.091(6) 0.022(4) 0.025(4) -0.006(3) O6 0.040(4) 0.092(6) 0.047(4) -0.042(4) 0.003(3) 0.018(4) O7 0.045(5) 0.144(9) 0.099(7) 0.092(6) -0.023(4) -0.049(5) O8 0.028(3) 0.032(4) 0.103(6) -0.018(4) 0.019(4) -0.007(3) O9 0.098(6) 0.051(5) 0.123(7) -0.043(5) 0.092(6) -0.038(4) O10 0.102(6) 0.057(5) 0.100(7) -0.052(5) 0.082(5) -0.046(5) O11 0.069(5) 0.039(4) 0.064(5) 0.018(3) 0.037(4) 0.031(4) O12 0.045(4) 0.122(7) 0.087(6) 0.075(6) -0.032(4) -0.047(5) O13 0.093(6) 0.064(5) 0.106(7) -0.051(5) 0.080(5) -0.047(5) O14 0.097(6) 0.043(4) 0.052(5) 0.007(4) -0.039(4) 0.000(4) O15 0.027(3) 0.034(4) 0.106(6) -0.017(4) 0.021(4) -0.007(3) O16 0.023(3) 0.036(4) 0.100(6) -0.017(4) 0.015(3) -0.004(3) O17 0.046(5) 0.149(9) 0.085(6) 0.087(6) -0.026(4) -0.050(5) O18 0.164(9) 0.091(7) 0.031(4) -0.014(4) -0.012(5) 0.087(7) O21 0.048(4) 0.058(5) 0.067(5) -0.006(4) 0.010(4) 0.009(4) O22 0.066(5) 0.060(5) 0.042(4) 0.009(4) 0.021(4) 0.016(4) O23 0.047(4) 0.056(5) 0.057(5) -0.005(4) 0.015(4) 0.005(4) O24 0.046(4) 0.072(5) 0.062(5) -0.007(4) 0.010(4) 0.007(4) O25 0.097(7) 0.068(5) 0.051(5) -0.021(5) 0.017(5) -0.004(5) O26 0.116(7) 0.054(5) 0.065(6) -0.026(5) 0.011(5) 0.010(5) C13 0.046(7) 0.083(9) 0.078(9) 0.020(7) 0.026(6) 0.027(6) C14 0.049(7) 0.060(7) 0.080(9) -0.010(7) 0.024(6) 0.017(6) C15 0.058(7) 0.076(8) 0.064(8) -0.020(7) 0.030(6) 0.006(6) C16 0.073(8) 0.073(8) 0.044(7) -0.005(6) 0.026(6) 0.001(7) C17 0.046(6) 0.067(8) 0.053(7) 0.008(6) 0.005(5) -0.013(6) C18 0.037(6) 0.062(7) 0.061(8) 0.019(6) 0.008(5) 0.005(5) C19 0.086(10) 0.058(8) 0.109(12) -0.010(8) 0.010(9) 0.034(7) C20 0.124(14) 0.049(8) 0.134(15) -0.031(9) 0.023(12) 0.015(9) C21 0.110(12) 0.083(10) 0.082(11) -0.062(9) 0.017(9) -0.013(9) C22 0.111(12) 0.105(12) 0.059(9) -0.047(9) 0.009(8) -0.013(10) C23 0.115(12) 0.078(10) 0.048(8) -0.006(7) -0.014(8) 0.000(9) C24 0.073(9) 0.068(9) 0.077(10) 0.014(8) -0.009(8) -0.003(7) K2 0.0452(14) 0.0811(19) 0.0751(19) -0.0174(15) 0.0048(13) 0.0068(13) O27 0.060(5) 0.064(5) 0.057(5) 0.000(4) 0.012(4) -0.005(4) O28 0.089(7) 0.078(6) 0.094(7) 0.007(6) 0.028(6) 0.030(6) O29 0.063(6) 0.143(10) 0.101(8) 0.028(7) 0.014(6) 0.041(7) O30 0.048(5) 0.143(10) 0.095(7) 0.051(7) 0.014(5) -0.021(6) O31 0.077(7) 0.058(6) 0.167(11) -0.010(6) 0.021(7) -0.008(5) O32 0.064(6) 0.079(6) 0.084(7) 0.002(5) 0.012(5) 0.016(5) C1 0.056(8) 0.116(13) 0.076(10) -0.005(9) 0.000(7) 0.025(8) C2 0.053(8) 0.143(14) 0.039(7) 0.001(8) 0.010(6) -0.011(8) C3 0.093(11) 0.075(10) 0.069(10) -0.002(7) 0.006(8) -0.022(8) C4 0.125(15) 0.052(8) 0.120(15) -0.014(9) 0.015(12) 0.002(9) C5 0.131(15) 0.080(11) 0.146(17) 0.034(11) 0.090(14) 0.041(11) C6 0.092(13) 0.158(19) 0.156(19) 0.071(16) 0.045(13) 0.074(14) C7 0.037(8) 0.27(3) 0.063(10) 0.029(15) 0.003(7) 0.044(14) C8 0.047(9) 0.26(3) 0.059(10) 0.004(15) 0.018(7) -0.032(14) C9 0.104(13) 0.139(16) 0.112(14) 0.039(12) 0.012(11) -0.083(13) C10 0.127(16) 0.093(12) 0.125(16) 0.042(11) 0.017(13) -0.032(12) C11 0.092(12) 0.071(10) 0.148(17) 0.018(10) 0.030(12) 0.016(9) C12 0.083(11) 0.094(12) 0.152(17) 0.030(12) 0.029(11) 0.040(10) 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 _geom_angle_publ_flag O1 W1 O3 100.3(4) . . ? O1 W1 O4 100.1(4) . . ? O1 W1 O9 101.5(4) . 3_666 ? O1 W1 O10 100.9(4) . 3_666 ? O1 W1 O19 154.6(3) . . ? O1 W1 O20' 157.6(3) . 3_666 ? O3 W1 O4 89.3(3) . . ? O3 W1 O10 158.7(4) . 3_666 ? O3 W1 O19 64.5(4) . . ? O3 W1 O20' 95.2(4) . 3_666 ? O4 W1 O19 61.4(4) . . ? O4 W1 O20' 96.1(4) . 3_666 ? O9 W1 O3 89.0(4) 3_666 . ? O9 W1 O4 158.2(4) 3_666 . ? O9 W1 O10 88.7(3) 3_666 3_666 ? O9 W1 O19 98.5(4) 3_666 . ? O9 W1 O20' 62.4(3) 3_666 3_666 ? O10 W1 O4 85.0(4) 3_666 . ? O10 W1 O19 94.9(4) 3_666 . ? O10 W1 O20' 65.2(3) 3_666 3_666 ? O19 W1 O20' 47.8(3) . 3_666 ? O4 W2 O15 157.5(4) . . ? O4 W2 O16 88.1(3) . . ? O4 W2 O18 89.0(3) . . ? O4 W2 O19 63.0(4) . . ? O4 W2 O20 95.4(4) . . ? O5 W2 O4 101.6(4) . . ? O5 W2 O15 100.9(3) . . ? O5 W2 O16 101.1(3) . . ? O5 W2 O18 102.1(4) . . ? O5 W2 O19 157.6(4) . . ? O5 W2 O20 157.5(3) . . ? O15 W2 O19 95.2(3) . . ? O15 W2 O20 63.0(3) . . ? O16 W2 O15 88.0(3) . . ? O16 W2 O18 156.7(4) . . ? O16 W2 O19 94.8(3) . . ? O16 W2 O20 64.5(3) . . ? O18 W2 O15 85.8(3) . . ? O18 W2 O19 63.5(4) . . ? O18 W2 O20 92.7(4) . . ? O19 W2 O20 44.9(3) . . ? O6 W3 O7 100.9(5) . . ? O6 W3 O8 101.6(3) . . ? O6 W3 O12 100.4(4) . 3_666 ? O6 W3 O16 101.5(4) . . ? O6 W3 O19' 156.3(4) . 3_666 ? O6 W3 O20 159.0(4) . . ? O7 W3 O8 89.2(3) . . ? O7 W3 O12 88.0(3) . 3_666 ? O7 W3 O16 157.4(4) . . ? O7 W3 O19' 64.4(4) . 3_666 ? O7 W3 O20 94.2(4) . . ? O8 W3 O12 158.0(4) . 3_666 ? O8 W3 O16 88.9(3) . . ? O8 W3 O19' 96.9(3) . 3_666 ? O8 W3 O20 63.9(3) . . ? O12 W3 O19' 62.4(4) 3_666 3_666 ? O12 W3 O20 94.6(4) 3_666 . ? O16 W3 O12 85.4(3) . 3_666 ? O16 W3 O19' 93.5(3) . 3_666 ? O16 W3 O20 64.8(3) . . ? O19' W3 O20 44.7(3) 3_666 . ? O8 W4 O9 85.2(3) . . ? O8 W4 O20 64.7(3) . . ? O8 W4 O20' 93.6(3) . . ? O9 W4 O20 92.5(4) . . ? O9 W4 O20' 64.1(4) . . ? O13 W4 O8 157.3(4) . . ? O13 W4 O9 87.8(3) . . ? O13 W4 O15 89.9(3) . . ? O13 W4 O20 94.1(4) . . ? O13 W4 O20' 64.0(4) . . ? O14 W4 O8 101.7(4) . . ? O14 W4 O9 101.7(4) . . ? O14 W4 O13 100.9(4) . . ? O14 W4 O15 101.0(4) . . ? O14 W4 O20 159.6(4) . . ? O14 W4 O20' 158.4(4) . . ? O15 W4 O8 88.2(3) . . ? O15 W4 O9 157.3(4) . . ? O15 W4 O20 65.0(3) . . ? O15 W4 O20' 94.7(3) . . ? O20' W4 O20 42.1(3) . . ? O10 W5 O13 87.9(3) . . ? O10 W5 O17 157.9(4) . . ? O10 W5 O19' 95.7(4) . . ? O10 W5 O20' 65.4(3) . . ? O11 W5 O10 101.8(4) . . ? O11 W5 O12 102.4(4) . . ? O11 W5 O13 100.5(4) . . ? O11 W5 O17 100.1(4) . . ? O11 W5 O19' 156.5(3) . . ? O11 W5 O20' 156.6(3) . . ? O12 W5 O10 90.1(4) . . ? O12 W5 O13 157.0(4) . . ? O12 W5 O17 88.0(3) . . ? O12 W5 O19' 61.7(4) . . ? O12 W5 O20' 97.3(4) . . ? O13 W5 O17 85.3(4) . . ? O13 W5 O19' 95.7(4) . . ? O13 W5 O20' 61.2(3) . . ? O17 W5 O19' 64.2(4) . . ? O17 W5 O20' 93.0(4) . . ? O19' W5 O20' 46.7(3) . . ? O2 W6 O3 106.3(5) . . ? O2 W6 O7 103.1(6) . 3_666 ? O2 W6 O17 95.0(5) . . ? O2 W6 O18 97.9(5) . . ? O2 W6 O19 155.7(7) . . ? O2 W6 O19' 151.8(7) . . ? O3 W6 O7 92.0(5) . 3_666 ? O3 W6 O17 158.3(5) . . ? O3 W6 O18 89.4(6) . . ? O3 W6 O19 64.7(4) . . ? O3 W6 O19' 98.6(5) . . ? O7 W6 O17 86.9(6) 3_666 . ? O7 W6 O18 157.6(5) 3_666 . ? O7 W6 O19 99.8(5) 3_666 . ? O7 W6 O19' 62.4(4) 3_666 . ? O17 W6 O19 94.1(4) . . ? O17 W6 O19' 61.8(4) . . ? O18 W6 O17 83.7(4) . . ? O18 W6 O19 60.9(4) . . ? O18 W6 O19' 95.3(4) . . ? O19 W6 O19' 49.8(3) . . ? O2 W6' O3 92.5(4) . . ? O2 W6' O7 104.2(5) . 3_666 ? O2 W6' O18 94.4(4) . . ? O2 W6' O19 141.8(4) . . ? O2 W6' O19' 167.7(5) . . ? O3 W6' O19 58.9(3) . . ? O3 W6' O19' 93.6(4) . . ? O7 W6' O3 83.3(4) 3_666 . ? O7 W6' O18 154.8(5) 3_666 . ? O7 W6' O19 97.3(5) 3_666 . ? O7 W6' O19' 65.9(4) 3_666 . ? O17 W6' O2 107.4(4) . . ? O17 W6' O3 158.3(5) . . ? O17 W6' O7 99.6(4) . 3_666 ? O17 W6' O18 90.6(5) . . ? O17 W6' O19 99.4(5) . . ? O17 W6' O19' 68.7(4) . . ? O18 W6' O3 79.0(4) . . ? O18 W6' O19 58.1(4) . . ? O18 W6' O19' 97.3(4) . . ? O19' W6' O19 49.8(3) . . ? O2 W6'' O3 101.3(4) . . ? O2 W6'' O7 90.9(4) . 3_666 ? O2 W6'' O17 97.0(5) . . ? O2 W6'' O19 164.6(5) . . ? O2 W6'' O19' 142.7(4) . . ? O3 W6'' O7 80.1(4) . 3_666 ? O3 W6'' O17 153.6(5) . . ? O3 W6'' O19 65.1(4) . . ? O3 W6'' O19' 93.3(4) . . ? O7 W6'' O19 93.5(4) 3_666 . ? O7 W6'' O19' 57.8(3) 3_666 . ? O17 W6'' O7 80.7(4) . 3_666 ? O17 W6'' O19 98.2(4) . . ? O17 W6'' O19' 61.0(4) . . ? O18 W6'' O2 110.7(5) . . ? O18 W6'' O3 96.4(5) . . ? O18 W6'' O7 158.3(5) . 3_666 ? O18 W6'' O17 94.7(5) . . ? O18 W6'' O19 66.1(4) . . ? O18 W6'' O19' 101.4(5) . . ? O19 W6'' O19' 49.6(3) . . ? O1 K1 C25 81.8(4) . . ? O21 K1 O1 125.1(2) . . ? O21 K1 O25 106.2(2) . . ? O21 K1 C25 96.8(4) . . ? O22 K1 O1 81.0(2) . . ? O22 K1 O21 56.8(2) . . ? O22 K1 O23 58.8(2) . . ? O22 K1 O24 117.4(2) . . ? O22 K1 O25 145.6(2) . . ? O22 K1 O26 113.5(2) . . ? O22 K1 N1 135.6(4) . . ? O22 K1 C25 127.8(5) . . ? O23 K1 O1 70.58(19) . . ? O23 K1 O21 107.4(2) . . ? O23 K1 O25 107.9(2) . . ? O23 K1 O26 144.1(3) . . ? O23 K1 C25 150.5(4) . . ? O24 K1 O1 82.6(2) . . ? O24 K1 O21 145.4(2) . . ? O24 K1 O23 58.7(2) . . ? O24 K1 O25 57.4(2) . . ? O24 K1 O26 113.9(2) . . ? O24 K1 C25 108.5(4) . . ? O25 K1 O1 127.2(2) . . ? O25 K1 C25 80.4(5) . . ? O26 K1 O1 145.3(2) . . ? O26 K1 O21 56.8(2) . . ? O26 K1 O25 56.6(2) . . ? O26 K1 C25 64.2(5) . . ? N1 K1 O1 70.6(4) . . ? N1 K1 O21 115.0(4) . . ? N1 K1 O23 133.8(4) . . ? N1 K1 O24 92.3(4) . . ? N1 K1 O25 77.6(4) . . ? N1 K1 O26 78.1(4) . . ? N1 K1 C25 18.3(4) . . ? O19 Si1 O19 180.0 3_666 . ? O19' Si1 O19 75.2(5) 3_666 3_666 ? O19' Si1 O19 104.8(5) . 3_666 ? O19' Si1 O19 104.8(5) 3_666 . ? O19' Si1 O19 75.2(5) . . ? O19' Si1 O19' 180.0(6) 3_666 . ? O20 Si1 O19 69.2(5) . . ? O20 Si1 O19 69.2(5) 3_666 3_666 ? O20 Si1 O19 110.8(5) 3_666 . ? O20 Si1 O19 110.8(5) . 3_666 ? O20 Si1 O19' 110.7(5) . . ? O20 Si1 O19' 110.7(5) 3_666 3_666 ? O20 Si1 O19' 69.3(5) 3_666 . ? O20 Si1 O19' 69.3(5) . 3_666 ? O20 Si1 O20 180.0 . 3_666 ? O20 Si1 O20' 65.6(5) . . ? O20 Si1 O20' 65.6(5) 3_666 3_666 ? O20 Si1 O20' 114.4(5) 3_666 . ? O20 Si1 O20' 114.4(5) . 3_666 ? O20' Si1 O19 107.4(5) 3_666 3_666 ? O20' Si1 O19 72.6(5) . 3_666 ? O20' Si1 O19 107.4(5) . . ? O20' Si1 O19 72.6(5) 3_666 . ? O20' Si1 O19' 108.2(5) 3_666 . ? O20' Si1 O19' 71.8(5) . . ? O20' Si1 O19' 71.8(5) 3_666 3_666 ? O20' Si1 O19' 108.2(5) . 3_666 ? O20' Si1 O20' 180.0 . 3_666 ? W1 O1 K1 120.8(4) . . ? W6 O2 W6' 11.6(4) . . ? W6 O2 W6'' 11.1(4) . . ? W6'' O2 W6' 15.39(10) . . ? W1 O3 W6' 137.6(5) . . ? W1 O3 W6'' 134.2(5) . . ? W6 O3 W1 139.2(6) . . ? W6 O3 W6' 2.8(4) . . ? W6 O3 W6'' 9.8(4) . . ? W6'' O3 W6' 11.38(10) . . ? W2 O4 W1 136.9(6) . . ? W2 O5 K2 166.9(4) . 3_665 ? W3 O7 W6'' 137.0(6) . 3_666 ? W6 O7 W3 139.7(6) 3_666 . ? W6 O7 W6'' 3.2(3) 3_666 3_666 ? W6' O7 W3 134.8(5) 3_666 . ? W6' O7 W6 10.8(3) 3_666 3_666 ? W6' O7 W6'' 8.22(13) 3_666 3_666 ? W3 O8 W4 137.6(4) . . ? W1 O9 W4 137.8(5) 3_666 . ? W5 O10 W1 137.2(4) . 3_666 ? W5 O12 W3 138.3(6) . 3_666 ? W4 O13 W5 139.0(5) . . ? W4 O15 W2 138.4(4) . . ? W2 O16 W3 138.7(4) . . ? W5 O17 W6 135.5(5) . . ? W5 O17 W6'' 139.3(6) . . ? W6' O17 W5 135.6(5) . . ? W6' O17 W6 2.8(5) . . ? W6' O17 W6'' 11.79(17) . . ? W6'' O17 W6 9.3(4) . . ? W2 O18 W6 135.9(5) . . ? W2 O18 W6' 138.9(6) . . ? W6 O18 W6' 9.6(3) . . ? W6'' O18 W2 138.6(6) . . ? W6'' O18 W6 3.0(3) . . ? W6'' O18 W6' 7.6(2) . . ? W1 O19 W6 91.7(4) . . ? W1 O19 W6' 99.0(3) . . ? W2 O19 W1 98.0(3) . . ? W2 O19 W6 98.8(4) . . ? W2 O19 W6' 99.5(4) . . ? W2 O19 W6'' 91.3(3) . . ? W6 O19 W6' 7.6(2) . . ? W6'' O19 W1 94.7(4) . . ? W6'' O19 W6 7.7(2) . . ? W6'' O19 W6' 9.91(8) . . ? Si1 O19 W1 120.1(5) . . ? Si1 O19 W2 124.0(5) . . ? Si1 O19 W6 117.7(5) . . ? Si1 O19 W6' 111.9(5) . . ? Si1 O19 W6'' 121.5(5) . . ? W3 O19' W5 97.3(3) 3_666 . ? W3 O19' W6 93.5(4) 3_666 . ? W3 O19' W6'' 100.7(4) 3_666 . ? W5 O19' W6 98.0(4) . . ? W5 O19' W6'' 95.3(3) . . ? W6 O19' W6'' 7.4(2) . . ? W6' O19' W3 93.1(4) . 3_666 ? W6' O19' W5 90.5(3) . . ? W6' O19' W6 7.7(2) . . ? W6' O19' W6'' 9.71(8) . . ? Si1 O19' W3 123.6(5) . 3_666 ? Si1 O19' W5 121.2(5) . . ? Si1 O19' W6 117.1(5) . . ? Si1 O19' W6' 123.0(5) . . ? Si1 O19' W6'' 113.4(5) . . ? W3 O20 W2 91.5(3) . . ? W4 O20 W2 93.0(3) . . ? W4 O20 W3 93.1(3) . . ? Si1 O20 W2 121.9(5) . . ? Si1 O20 W3 122.4(5) . . ? Si1 O20 W4 125.9(5) . . ? Si1 O20 O20' 59.0(5) . . ? O20' O20 W2 131.9(6) . . ? O20' O20 W3 130.8(6) . . ? O20' O20 W4 66.9(4) . . ? W1 O20' W5 92.1(3) 3_666 . ? W4 O20' W1 95.2(3) . 3_666 ? W4 O20' W5 95.4(3) . . ? Si1 O20' W1 119.6(5) . 3_666 ? Si1 O20' W4 126.4(5) . . ? Si1 O20' W5 120.3(5) . . ? Si1 O20' O20 55.4(4) . . ? O20 O20' W1 131.2(6) . 3_666 ? O20 O20' W4 71.0(5) . . ? O20 O20' W5 134.5(6) . . ? C18 O21 K1 108.3(6) . . ? C18 O21 C19 113.1(9) . . ? C19 O21 K1 110.7(7) . . ? C16 O22 K1 119.9(6) . . ? C17 O22 K1 122.6(6) . . ? C17 O22 C16 110.8(8) . . ? C14 O23 K1 108.9(6) . . ? C15 O23 K1 109.3(6) . . ? C15 O23 C14 111.0(8) . . ? C13 O24 K1 117.7(6) . . ? C24 O24 K1 119.1(7) . . ? C24 O24 C13 112.2(9) . . ? C22 O25 K1 109.0(7) . . ? C22 O25 C23 111.6(11) . . ? C23 O25 K1 107.3(7) . . ? C20 O26 K1 118.4(8) . . ? C21 O26 K1 119.4(8) . . ? C21 O26 C20 109.7(11) . . ? C25 N1 K1 111.4(18) . . ? O24 C13 H13A 109.6 . . ? O24 C13 H13B 109.6 . . ? O24 C13 C14 110.3(9) . . ? H13A C13 H13B 108.1 . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? O23 C14 C13 108.8(9) . . ? O23 C14 H14A 109.9 . . ? O23 C14 H14B 109.9 . . ? C13 C14 H14A 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? O23 C15 H15A 109.7 . . ? O23 C15 H15B 109.7 . . ? O23 C15 C16 109.6(9) . . ? H15A C15 H15B 108.2 . . ? C16 C15 H15A 109.7 . . ? C16 C15 H15B 109.7 . . ? O22 C16 C15 109.2(9) . . ? O22 C16 H16A 109.8 . . ? O22 C16 H16B 109.8 . . ? C15 C16 H16A 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O22 C17 H17A 109.4 . . ? O22 C17 H17B 109.4 . . ? O22 C17 C18 111.2(9) . . ? H17A C17 H17B 108.0 . . ? C18 C17 H17A 109.4 . . ? C18 C17 H17B 109.4 . . ? O21 C18 C17 109.7(8) . . ? O21 C18 H18A 109.7 . . ? O21 C18 H18B 109.7 . . ? C17 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? O21 C19 H19A 109.7 . . ? O21 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C20 C19 O21 109.9(11) . . ? C20 C19 H19A 109.7 . . ? C20 C19 H19B 109.7 . . ? O26 C20 H20A 109.7 . . ? O26 C20 H20B 109.7 . . ? C19 C20 O26 109.7(11) . . ? C19 C20 H20A 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? O26 C21 H21A 110.1 . . ? O26 C21 H21B 110.1 . . ? O26 C21 C22 108.2(11) . . ? H21A C21 H21B 108.4 . . ? C22 C21 H21A 110.1 . . ? C22 C21 H21B 110.1 . . ? O25 C22 C21 109.2(12) . . ? O25 C22 H22A 109.8 . . ? O25 C22 H22B 109.8 . . ? C21 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? O25 C23 H23A 110.5 . . ? O25 C23 H23B 110.5 . . ? O25 C23 C24 106.2(11) . . ? H23A C23 H23B 108.7 . . ? C24 C23 H23A 110.5 . . ? C24 C23 H23B 110.5 . . ? O24 C24 C23 109.1(11) . . ? O24 C24 H24A 109.9 . . ? O24 C24 H24B 109.9 . . ? C23 C24 H24A 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? N1 C25 K1 50.3(15) . . ? N1 C25 C26 169(3) . . ? C26 C25 K1 140.9(19) . . ? 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 . . ? O5 K2 C2 68.3(2) 3_665 . ? O27 K2 O5 81.8(2) . 3_665 ? O27 K2 O29 117.6(3) . . ? O27 K2 O30 161.7(3) . . ? O27 K2 O31 114.6(3) . . ? O27 K2 O32 59.6(3) . . ? O27 K2 C2 22.0(3) . . ? O28 K2 O5 95.2(3) . 3_665 ? O28 K2 O27 60.4(3) . . ? O28 K2 O29 60.6(3) . . ? O28 K2 O30 118.7(3) . . ? O28 K2 O31 159.2(3) . . ? O28 K2 O32 119.9(3) . . ? O28 K2 C2 80.0(3) . . ? O29 K2 O5 121.6(3) . 3_665 ? O29 K2 O30 58.1(4) . . ? O29 K2 C2 139.4(4) . . ? O30 K2 O5 116.0(3) . 3_665 ? O30 K2 C2 158.9(4) . . ? O31 K2 O5 104.1(3) . 3_665 ? O31 K2 O29 113.2(4) . . ? O31 K2 O30 59.0(3) . . ? O31 K2 O32 58.6(3) . . ? O31 K2 C2 100.0(4) . . ? O32 K2 O5 77.8(2) . 3_665 ? O32 K2 O29 160.6(3) . . ? O32 K2 O30 117.6(3) . . ? O32 K2 C2 41.6(3) . . ? C2 O27 K2 110.4(7) . . ? C3 O27 K2 112.8(7) . . ? C3 O27 C2 112.6(11) . . ? C4 O28 K2 115.1(8) . . ? C4 O28 C5 114.4(13) . . ? C5 O28 K2 116.6(9) . . ? C6 O29 K2 110.2(9) . . ? C7 O29 K2 113.4(9) . . ? C7 O29 C6 112.6(14) . . ? C8 O30 K2 118.3(11) . . ? C8 O30 C9 113.5(13) . . ? C9 O30 K2 114.9(8) . . ? C10 O31 K2 120.3(10) . . ? C10 O31 C11 115.1(14) . . ? C11 O31 K2 116.7(8) . . ? C1 O32 K2 117.0(7) . . ? C12 O32 K2 117.7(8) . . ? C12 O32 C1 112.1(12) . . ? O32 C1 H1A 109.9 . . ? O32 C1 H1B 109.9 . . ? O32 C1 C2 108.9(11) . . ? H1A C1 H1B 108.3 . . ? C2 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? K2 C2 H2A 157.6 . . ? K2 C2 H2B 82.1 . . ? O27 C2 K2 47.5(5) . . ? O27 C2 C1 107.6(11) . . ? O27 C2 H2A 110.2 . . ? O27 C2 H2B 110.2 . . ? C1 C2 K2 83.0(7) . . ? C1 C2 H2A 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O27 C3 H3A 110.3 . . ? O27 C3 H3B 110.3 . . ? O27 C3 C4 107.3(11) . . ? H3A C3 H3B 108.5 . . ? C4 C3 H3A 110.3 . . ? C4 C3 H3B 110.3 . . ? O28 C4 C3 109.9(13) . . ? O28 C4 H4A 109.7 . . ? O28 C4 H4B 109.7 . . ? C3 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O28 C5 H5A 110.0 . . ? O28 C5 H5B 110.0 . . ? O28 C5 C6 108.7(14) . . ? H5A C5 H5B 108.3 . . ? C6 C5 H5A 110.0 . . ? C6 C5 H5B 110.0 . . ? O29 C6 C5 106.7(13) . . ? O29 C6 H6A 110.4 . . ? O29 C6 H6B 110.4 . . ? C5 C6 H6A 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? O29 C7 H7A 109.5 . . ? O29 C7 H7B 109.5 . . ? O29 C7 C8 110.7(14) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? O30 C8 C7 112.5(14) . . ? O30 C8 H8A 109.1 . . ? O30 C8 H8B 109.1 . . ? C7 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? O30 C9 H9A 108.9 . . ? O30 C9 H9B 108.9 . . ? O30 C9 C10 113.3(12) . . ? H9A C9 H9B 107.7 . . ? C10 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? O31 C10 C9 113.6(17) . . ? O31 C10 H10A 108.8 . . ? O31 C10 H10B 108.8 . . ? C9 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O31 C11 H11A 109.5 . . ? O31 C11 H11B 109.5 . . ? O31 C11 C12 110.6(14) . . ? H11A C11 H11B 108.1 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? O32 C12 C11 108.7(13) . . ? O32 C12 H12A 110.0 . . ? O32 C12 H12B 110.0 . . ? C11 C12 H12A 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.679(6) . ? W1 O3 1.873(7) . ? W1 O4 1.919(8) . ? W1 O9 1.868(8) 3_666 ? W1 O10 1.901(6) 3_666 ? W1 O19 2.364(9) . ? W1 O20' 2.444(9) 3_666 ? W2 O4 1.875(7) . ? W2 O5 1.688(6) . ? W2 O15 1.913(6) . ? W2 O16 1.876(6) . ? W2 O18 1.905(7) . ? W2 O19 2.313(10) . ? W2 O20 2.478(10) . ? W3 O6 1.677(6) . ? W3 O7 1.876(7) . ? W3 O8 1.879(6) . ? W3 O12 1.914(7) 3_666 ? W3 O16 1.899(6) . ? W3 O19' 2.329(9) 3_666 ? W3 O20 2.454(10) . ? W4 O8 1.905(6) . ? W4 O9 1.920(6) . ? W4 O13 1.869(7) . ? W4 O14 1.671(7) . ? W4 O15 1.878(6) . ? W4 O20 2.405(10) . ? W4 O20' 2.340(10) . ? W5 O10 1.881(7) . ? W5 O11 1.671(6) . ? W5 O12 1.872(8) . ? W5 O13 1.912(8) . ? W5 O17 1.916(7) . ? W5 O19' 2.383(9) . ? W5 O20' 2.447(9) . ? W6 O2 1.676(7) . ? W6 O3 1.776(10) . ? W6 O7 1.828(13) 3_666 ? W6 O17 2.017(10) . ? W6 O18 1.960(13) . ? W6 O19 2.404(11) . ? W6 O19' 2.441(11) . ? W6' O2 1.702(6) . ? W6' O3 2.105(8) . ? W6' O7 1.777(10) 3_666 ? W6' O17 1.687(8) . ? W6' O18 2.030(11) . ? W6' O19 2.512(10) . ? W6' O19' 2.317(10) . ? W6'' O2 1.693(6) . ? W6'' O3 1.878(9) . ? W6'' O7 2.136(9) 3_666 ? W6'' O17 1.948(10) . ? W6'' O18 1.646(9) . ? W6'' O19 2.334(10) . ? W6'' O19' 2.517(10) . ? K1 O1 3.062(7) . ? K1 O21 2.965(8) . ? K1 O22 2.807(7) . ? K1 O23 2.855(7) . ? K1 O24 2.840(7) . ? K1 O25 2.967(8) . ? K1 O26 2.918(8) . ? K1 N1 2.828(17) . ? K1 C25 3.42(2) . ? Si1 O19 1.685(9) 3_666 ? Si1 O19 1.685(9) . ? Si1 O19' 1.658(9) . ? Si1 O19' 1.658(9) 3_666 ? Si1 O20 1.541(10) 3_666 ? Si1 O20 1.541(10) . ? Si1 O20' 1.605(9) 3_666 ? Si1 O20' 1.605(9) . ? O5 K2 2.945(7) 3_665 ? O20 O20' 1.704(13) . ? O21 C18 1.394(12) . ? O21 C19 1.433(14) . ? O22 C16 1.406(12) . ? O22 C17 1.395(12) . ? O23 C14 1.419(12) . ? O23 C15 1.419(13) . ? O24 C13 1.413(13) . ? O24 C24 1.408(14) . ? O25 C22 1.394(15) . ? O25 C23 1.412(15) . ? O26 C20 1.427(16) . ? O26 C21 1.420(14) . ? N1 C25 1.154(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.457(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.482(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.470(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.413(19) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.476(19) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.477(18) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.509(10) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? K2 O27 2.784(8) . ? K2 O28 2.783(10) . ? K2 O29 2.857(9) . ? K2 O30 2.861(9) . ? K2 O31 2.795(10) . ? K2 O32 2.800(8) . ? K2 C2 3.536(12) . ? O27 C2 1.415(14) . ? O27 C3 1.408(15) . ? O28 C4 1.407(16) . ? O28 C5 1.424(16) . ? O29 C6 1.42(2) . ? O29 C7 1.40(2) . ? O30 C8 1.391(19) . ? O30 C9 1.406(19) . ? O31 C10 1.317(18) . ? O31 C11 1.395(16) . ? O32 C1 1.412(15) . ? O32 C12 1.408(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.477(18) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.49(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.53(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.45(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.48(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.46(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag W2 O20 O20' W1 152.1(5) . . . 3_666 ? W2 O20 O20' W4 72.2(7) . . . . ? W2 O20 O20' W5 -6.4(13) . . . . ? W2 O20 O20' Si1 -106.8(7) . . . . ? W3 O20 O20' W1 6.8(12) . . . 3_666 ? W3 O20 O20' W4 -73.1(6) . . . . ? W3 O20 O20' W5 -151.6(5) . . . . ? W3 O20 O20' Si1 107.9(7) . . . . ? W4 O20 O20' W1 80.0(7) . . . 3_666 ? W4 O20 O20' W5 -78.5(7) . . . . ? W4 O20 O20' Si1 -178.9(5) . . . . ? K1 O21 C18 C17 -61.3(9) . . . . ? K1 O21 C19 C20 59.7(14) . . . . ? K1 O22 C16 C15 30.2(12) . . . . ? K1 O22 C17 C18 -23.2(11) . . . . ? K1 O23 C14 C13 -63.4(9) . . . . ? K1 O23 C15 C16 61.4(10) . . . . ? K1 O24 C13 C14 -31.1(12) . . . . ? K1 O24 C24 C23 37.1(13) . . . . ? K1 O25 C22 C21 -65.1(12) . . . . ? K1 O25 C23 C24 64.7(11) . . . . ? K1 O26 C20 C19 38.7(17) . . . . ? K1 O26 C21 C22 -32.9(15) . . . . ? K1 N1 C25 C26 -169(15) . . . . ? Si1 O20 O20' W1 -101.1(7) . . . 3_666 ? Si1 O20 O20' W4 178.9(5) . . . . ? Si1 O20 O20' W5 100.4(8) . . . . ? O1 W1 O3 W6 157.7(10) . . . . ? O1 W1 O3 W6' 161.1(8) . . . . ? O1 W1 O3 W6'' 145.5(9) . . . . ? O2 W6 O3 W1 -155.1(9) . . . . ? O2 W6 O3 W6' 150(9) . . . . ? O2 W6 O3 W6'' -91.2(16) . . . . ? O2 W6' O17 W5 -156.1(8) . . . . ? O2 W6' O17 W6 113(6) . . . . ? O2 W6' O17 W6'' 89.3(7) . . . . ? O2 W6'' O3 W1 -159.4(8) . . . . ? O2 W6'' O3 W6 75.6(13) . . . . ? O2 W6'' O3 W6' 87.8(6) . . . . ? O2 W6'' O18 W2 155.7(8) . . . . ? O2 W6'' O18 W6 129(7) . . . . ? O2 W6'' O18 W6' -107.9(12) . . . . ? O3 W1 O1 K1 -14.2(4) . . . . ? O3 W6 O2 W6' -171(3) . . . . ? O3 W6 O2 W6'' 103(3) . . . . ? O3 W6' O2 W6 7(2) . . . . ? O3 W6' O2 W6'' 53.5(6) . . . . ? O3 W6' O17 W5 48(2) . . . . ? O3 W6' O17 W6 -42(5) . . . . ? O3 W6' O17 W6'' -66.1(14) . . . . ? O3 W6'' O2 W6 -64(3) . . . . ? O3 W6'' O2 W6' -113.3(7) . . . . ? O3 W6'' O18 W2 51.1(10) . . . . ? O3 W6'' O18 W6 25(7) . . . . ? O3 W6'' O18 W6' 147.4(11) . . . . ? O4 W1 O1 K1 77.0(4) . . . . ? O4 W1 O3 W6 57.6(11) . . . . ? O4 W1 O3 W6' 60.9(9) . . . . ? O4 W1 O3 W6'' 45.3(10) . . . . ? O4 W2 O5 K2 107.2(16) . . . 3_665 ? O4 W2 O16 W3 104.9(7) . . . . ? O5 W2 O4 W1 154.2(7) . . . . ? O5 W2 O16 W3 -153.6(6) . . . . ? O6 W3 O7 W6 160.3(9) . . . 3_666 ? O6 W3 O7 W6' 146.1(8) . . . 3_666 ? O6 W3 O7 W6'' 157.5(8) . . . 3_666 ? O6 W3 O8 W4 -154.9(6) . . . . ? O6 W3 O16 W2 155.0(6) . . . . ? O7 W3 O8 W4 104.1(6) . . . . ? O7 W3 O16 W2 -31.8(12) . . . . ? O7 W6 O2 W6' -75(3) 3_666 . . . ? O7 W6 O2 W6'' -161(3) 3_666 . . . ? O7 W6 O3 W1 100.6(11) 3_666 . . . ? O7 W6 O3 W6' 45(8) 3_666 . . . ? O7 W6 O3 W6'' 164.5(14) 3_666 . . . ? O7 W6' O2 W6 91(2) 3_666 . . . ? O7 W6' O2 W6'' 137.3(8) 3_666 . . . ? O7 W6' O17 W5 -47.7(11) 3_666 . . . ? O7 W6' O17 W6 -139(6) 3_666 . . . ? O7 W6' O17 W6'' -162.3(8) 3_666 . . . ? O7 W6'' O2 W6 16(2) 3_666 . . . ? O7 W6'' O2 W6' -33.2(6) 3_666 . . . ? O7 W6'' O3 W1 111.7(10) 3_666 . . . ? O7 W6'' O3 W6 -13.4(13) 3_666 . . . ? O7 W6'' O3 W6' -1.1(6) 3_666 . . . ? O7 W6'' O18 W2 -28(2) 3_666 . . . ? O7 W6'' O18 W6 -55(6) 3_666 . . . ? O7 W6'' O18 W6' 68.0(14) 3_666 . . . ? O8 W3 O7 W6 -98.1(9) . . . 3_666 ? O8 W3 O7 W6' -112.3(9) . . . 3_666 ? O8 W3 O7 W6'' -100.9(8) . . . 3_666 ? O8 W3 O16 W2 53.4(6) . . . . ? O8 W4 O13 W5 -18.0(12) . . . . ? O8 W4 O15 W2 -54.5(6) . . . . ? O9 W1 O1 K1 -105.3(3) 3_666 . . . ? O9 W1 O3 W6 -100.7(11) 3_666 . . . ? O9 W1 O3 W6' -97.3(9) 3_666 . . . ? O9 W1 O3 W6'' -113.0(9) 3_666 . . . ? O9 W4 O13 W5 54.1(7) . . . . ? O9 W4 O15 W2 18.6(12) . . . . ? O10 W1 O1 K1 163.8(3) 3_666 . . . ? O10 W1 O3 W6 -16.6(19) 3_666 . . . ? O10 W1 O3 W6' -13.3(17) 3_666 . . . ? O10 W1 O3 W6'' -28.9(17) 3_666 . . . ? O10 W5 O12 W3 102.7(7) . . . 3_666 ? O11 W5 O10 W1 154.9(7) . . . 3_666 ? O11 W5 O12 W3 -155.2(7) . . . 3_666 ? O12 W3 O7 W6 60.1(9) 3_666 . . 3_666 ? O12 W3 O7 W6' 45.9(9) 3_666 . . 3_666 ? O12 W3 O7 W6'' 57.3(8) 3_666 . . 3_666 ? O12 W3 O8 W4 21.5(11) 3_666 . . . ? O12 W3 O16 W2 -105.3(7) 3_666 . . . ? O12 W5 O10 W1 -102.5(8) . . . 3_666 ? O13 W4 O15 W2 102.8(7) . . . . ? O13 W5 O10 W1 54.6(8) . . . 3_666 ? O13 W5 O12 W3 17.9(13) . . . 3_666 ? O14 W4 O13 W5 155.5(7) . . . . ? O14 W4 O15 W2 -156.0(6) . . . . ? O15 W2 O4 W1 -24.5(13) . . . . ? O15 W2 O5 K2 -73.3(16) . . . 3_665 ? O15 W2 O16 W3 -52.9(6) . . . . ? O15 W4 O13 W5 -103.3(7) . . . . ? O16 W2 O4 W1 -104.8(8) . . . . ? O16 W2 O5 K2 16.9(17) . . . 3_665 ? O16 W3 O7 W6 -12.9(16) . . . 3_666 ? O16 W3 O7 W6' -27.1(15) . . . 3_666 ? O16 W3 O7 W6'' -15.7(14) . . . 3_666 ? O16 W3 O8 W4 -53.4(6) . . . . ? O17 W5 O10 W1 -17.6(15) . . . 3_666 ? O17 W5 O12 W3 -55.3(8) . . . 3_666 ? O17 W6 O2 W6' 13(2) . . . . ? O17 W6 O2 W6'' -73(2) . . . . ? O17 W6 O3 W1 14(3) . . . . ? O17 W6 O3 W6' -41(7) . . . . ? O17 W6 O3 W6'' 78.0(17) . . . . ? O17 W6' O2 W6 -164(3) . . . . ? O17 W6' O2 W6'' -117.6(11) . . . . ? O17 W6'' O2 W6 97(3) . . . . ? O17 W6'' O2 W6' 47.5(8) . . . . ? O17 W6'' O3 W1 67.7(14) . . . . ? O17 W6'' O3 W6 -57.4(16) . . . . ? O17 W6'' O3 W6' -45.1(11) . . . . ? O17 W6'' O18 W2 -104.9(9) . . . . ? O17 W6'' O18 W6 -131(7) . . . . ? O17 W6'' O18 W6' -8.6(10) . . . . ? O18 W2 O4 W1 52.0(8) . . . . ? O18 W2 O5 K2 -161.2(16) . . . 3_665 ? O18 W2 O16 W3 21.7(12) . . . . ? O18 W6 O2 W6' 97(2) . . . . ? O18 W6 O2 W6'' 11(2) . . . . ? O18 W6 O3 W1 -57.0(11) . . . . ? O18 W6 O3 W6' -112(8) . . . . ? O18 W6 O3 W6'' 6.9(12) . . . . ? O18 W6' O2 W6 -72(2) . . . . ? O18 W6' O2 W6'' -25.6(7) . . . . ? O18 W6' O17 W5 109.2(10) . . . . ? O18 W6' O17 W6 18(6) . . . . ? O18 W6' O17 W6'' -5.4(6) . . . . ? O18 W6'' O2 W6 -166(3) . . . . ? O18 W6'' O2 W6' 145.3(10) . . . . ? O18 W6'' O3 W1 -46.7(10) . . . . ? O18 W6'' O3 W6 -171.8(15) . . . . ? O18 W6'' O3 W6' -159.5(8) . . . . ? O19 W1 O1 K1 36.2(9) . . . . ? O19 W1 O3 W6 -0.8(10) . . . . ? O19 W1 O3 W6' 2.6(7) . . . . ? O19 W1 O3 W6'' -13.1(8) . . . . ? O19 W2 O4 W1 -8.5(6) . . . . ? O19 W2 O5 K2 151.5(13) . . . 3_665 ? O19 W2 O16 W3 42.2(7) . . . . ? O19 W6 O2 W6' 124(3) . . . . ? O19 W6 O2 W6'' 39(2) . . . . ? O19 W6 O3 W1 0.8(9) . . . . ? O19 W6 O3 W6' -55(8) . . . . ? O19 W6 O3 W6'' 64.7(13) . . . . ? O19 W6' O2 W6 -32(2) . . . . ? O19 W6' O2 W6'' 14.9(7) . . . . ? O19 W6' O17 W5 51.4(10) . . . . ? O19 W6' O17 W6 -39(6) . . . . ? O19 W6' O17 W6'' -63.1(6) . . . . ? O19 W6'' O2 W6 -91(3) . . . . ? O19 W6'' O2 W6' -139.7(14) . . . . ? O19 W6'' O3 W1 13.2(8) . . . . ? O19 W6'' O3 W6 -111.9(14) . . . . ? O19 W6'' O3 W6' -99.6(6) . . . . ? O19 W6'' O18 W2 -8.0(8) . . . . ? O19 W6'' O18 W6 -34(7) . . . . ? O19 W6'' O18 W6' 88.4(10) . . . . ? O19 Si1 O19' W3 -118.3(6) . . . 3_666 ? O19 Si1 O19' W3 61.7(6) 3_666 . . 3_666 ? O19 Si1 O19' W5 -63.8(6) 3_666 . . . ? O19 Si1 O19' W5 116.2(6) . . . . ? O19 Si1 O19' W6 -3.3(5) . . . . ? O19 Si1 O19' W6 176.7(5) 3_666 . . . ? O19 Si1 O19' W6' -177.7(5) 3_666 . . . ? O19 Si1 O19' W6' 2.3(5) . . . . ? O19 Si1 O19' W6'' -176.2(4) 3_666 . . . ? O19 Si1 O19' W6'' 3.8(4) . . . . ? O19 Si1 O20 W2 1.4(5) . . . . ? O19 Si1 O20 W2 -178.6(5) 3_666 . . . ? O19 Si1 O20 W3 116.9(7) . . . . ? O19 Si1 O20 W3 -63.1(7) 3_666 . . . ? O19 Si1 O20 W4 59.6(7) 3_666 . . . ? O19 Si1 O20 W4 -120.4(7) . . . . ? O19 Si1 O20 O20' 58.4(6) 3_666 . . . ? O19 Si1 O20 O20' -121.6(6) . . . . ? O19 Si1 O20' W1 178.5(5) . . . 3_666 ? O19 Si1 O20' W1 -1.5(5) 3_666 . . 3_666 ? O19 Si1 O20' W4 -124.7(7) 3_666 . . . ? O19 Si1 O20' W4 55.3(7) . . . . ? O19 Si1 O20' W5 -69.2(6) . . . . ? O19 Si1 O20' W5 110.8(6) 3_666 . . . ? O19 Si1 O20' O20 56.5(6) . . . . ? O19 Si1 O20' O20 -123.5(6) 3_666 . . . ? O19' W3 O7 W6 0.0(8) 3_666 . . 3_666 ? O19' W3 O7 W6' -14.3(7) 3_666 . . 3_666 ? O19' W3 O7 W6'' -2.9(7) 3_666 . . 3_666 ? O19' W3 O8 W4 40.0(6) 3_666 . . . ? O19' W3 O16 W2 -43.4(7) 3_666 . . . ? O19' W5 O10 W1 -40.9(8) . . . 3_666 ? O19' W5 O12 W3 6.3(6) . . . 3_666 ? O19' W6 O2 W6' -20.2(19) . . . . ? O19' W6 O2 W6'' -106(2) . . . . ? O19' W6 O3 W1 38.3(12) . . . . ? O19' W6 O3 W6' -17(8) . . . . ? O19' W6 O3 W6'' 102.2(13) . . . . ? O19' W6' O2 W6 126(4) . . . . ? O19' W6' O2 W6'' 173(2) . . . . ? O19' W6' O17 W5 11.5(8) . . . . ? O19' W6' O17 W6 -79(6) . . . . ? O19' W6' O17 W6'' -103.0(6) . . . . ? O19' W6'' O2 W6 47(2) . . . . ? O19' W6'' O2 W6' -2.3(7) . . . . ? O19' W6'' O3 W1 55.2(9) . . . . ? O19' W6'' O3 W6 -69.9(14) . . . . ? O19' W6'' O3 W6' -57.6(6) . . . . ? O19' W6'' O18 W2 -43.6(10) . . . . ? O19' W6'' O18 W6 -70(7) . . . . ? O19' W6'' O18 W6' 52.7(10) . . . . ? O19' Si1 O19 W1 113.4(6) . . . . ? O19' Si1 O19 W1 -66.6(6) 3_666 . . . ? O19' Si1 O19 W2 -120.9(6) . . . . ? O19' Si1 O19 W2 59.1(6) 3_666 . . . ? O19' Si1 O19 W6 3.4(5) . . . . ? O19' Si1 O19 W6 -176.6(5) 3_666 . . . ? O19' Si1 O19 W6' 178.1(4) 3_666 . . . ? O19' Si1 O19 W6' -1.9(4) . . . . ? O19' Si1 O19 W6'' -4.4(5) . . . . ? O19' Si1 O19 W6'' 175.6(5) 3_666 . . . ? O19' Si1 O20 W2 -114.4(6) 3_666 . . . ? O19' Si1 O20 W2 65.6(6) . . . . ? O19' Si1 O20 W3 -178.9(5) . . . . ? O19' Si1 O20 W3 1.1(5) 3_666 . . . ? O19' Si1 O20 W4 -56.2(7) . . . . ? O19' Si1 O20 W4 123.8(7) 3_666 . . . ? O19' Si1 O20 O20' 122.6(6) 3_666 . . . ? O19' Si1 O20 O20' -57.4(6) . . . . ? O19' Si1 O20' W1 -114.1(6) . . . 3_666 ? O19' Si1 O20' W1 65.9(6) 3_666 . . 3_666 ? O19' Si1 O20' W4 -57.3(7) 3_666 . . . ? O19' Si1 O20' W4 122.7(7) . . . . ? O19' Si1 O20' W5 -1.8(5) . . . . ? O19' Si1 O20' W5 178.2(5) 3_666 . . . ? O19' Si1 O20' O20 -56.1(6) 3_666 . . . ? O19' Si1 O20' O20 123.9(6) . . . . ? O20 W2 O4 W1 -40.6(8) . . . . ? O20 W2 O5 K2 -31(2) . . . 3_665 ? O20 W2 O16 W3 8.0(6) . . . . ? O20 W3 O7 W6 -34.3(9) . . . 3_666 ? O20 W3 O7 W6' -48.5(9) . . . 3_666 ? O20 W3 O7 W6'' -37.1(8) . . . 3_666 ? O20 W3 O8 W4 8.9(5) . . . . ? O20 W3 O16 W2 -8.1(6) . . . . ? O20 W4 O13 W5 -38.4(7) . . . . ? O20 W4 O15 W2 8.3(5) . . . . ? O20 Si1 O19 W1 52.8(7) 3_666 . . . ? O20 Si1 O19 W1 -127.2(7) . . . . ? O20 Si1 O19 W2 -1.5(5) . . . . ? O20 Si1 O19 W2 178.5(5) 3_666 . . . ? O20 Si1 O19 W6 -57.2(6) 3_666 . . . ? O20 Si1 O19 W6 122.8(6) . . . . ? O20 Si1 O19 W6' 117.5(6) . . . . ? O20 Si1 O19 W6' -62.5(6) 3_666 . . . ? O20 Si1 O19 W6'' 115.0(7) . . . . ? O20 Si1 O19 W6'' -65.0(7) 3_666 . . . ? O20 Si1 O19' W3 1.2(5) 3_666 . . 3_666 ? O20 Si1 O19' W3 -178.8(5) . . . 3_666 ? O20 Si1 O19' W5 -124.3(7) 3_666 . . . ? O20 Si1 O19' W5 55.7(7) . . . . ? O20 Si1 O19' W6 -63.8(6) . . . . ? O20 Si1 O19' W6 116.2(6) 3_666 . . . ? O20 Si1 O19' W6' -58.2(7) . . . . ? O20 Si1 O19' W6' 121.8(7) 3_666 . . . ? O20 Si1 O19' W6'' -56.7(6) . . . . ? O20 Si1 O19' W6'' 123.3(6) 3_666 . . . ? O20 Si1 O20' W1 -58.0(7) 3_666 . . 3_666 ? O20 Si1 O20' W1 122.0(7) . . . 3_666 ? O20 Si1 O20' W4 -1.2(5) . . . . ? O20 Si1 O20' W4 178.8(5) 3_666 . . . ? O20 Si1 O20' W5 54.3(7) 3_666 . . . ? O20 Si1 O20' W5 -125.7(7) . . . . ? O20 Si1 O20' O20 179.999(3) 3_666 . . . ? O20' W1 O1 K1 -147.1(7) 3_666 . . . ? O20' W1 O3 W6 -38.5(11) 3_666 . . . ? O20' W1 O3 W6' -35.1(9) 3_666 . . . ? O20' W1 O3 W6'' -50.8(9) 3_666 . . . ? O20' W4 O13 W5 -8.0(6) . . . . ? O20' W4 O15 W2 39.0(6) . . . . ? O20' W5 O10 W1 -4.5(6) . . . 3_666 ? O20' W5 O12 W3 37.5(7) . . . 3_666 ? O20' Si1 O19 W1 -1.6(5) 3_666 . . . ? O20' Si1 O19 W1 178.4(5) . . . . ? O20' Si1 O19 W2 124.2(7) 3_666 . . . ? O20' Si1 O19 W2 -55.8(7) . . . . ? O20' Si1 O19 W6 68.4(6) . . . . ? O20' Si1 O19 W6 -111.6(6) 3_666 . . . ? O20' Si1 O19 W6' -116.8(6) 3_666 . . . ? O20' Si1 O19 W6' 63.2(6) . . . . ? O20' Si1 O19 W6'' 60.7(6) . . . . ? O20' Si1 O19 W6'' -119.3(6) 3_666 . . . ? O20' Si1 O19' W3 127.3(7) . . . 3_666 ? O20' Si1 O19' W3 -52.7(7) 3_666 . . 3_666 ? O20' Si1 O19' W5 -178.2(5) 3_666 . . . ? O20' Si1 O19' W5 1.8(5) . . . . ? O20' Si1 O19' W6 -117.7(6) . . . . ? O20' Si1 O19' W6 62.3(6) 3_666 . . . ? O20' Si1 O19' W6' -112.1(7) . . . . ? O20' Si1 O19' W6' 67.9(7) 3_666 . . . ? O20' Si1 O19' W6'' -110.6(6) . . . . ? O20' Si1 O19' W6'' 69.4(6) 3_666 . . . ? O20' Si1 O20 W2 123.0(7) . . . . ? O20' Si1 O20 W2 -57.0(7) 3_666 . . . ? O20' Si1 O20 W3 58.5(7) 3_666 . . . ? O20' Si1 O20 W3 -121.5(7) . . . . ? O20' Si1 O20 W4 1.2(5) . . . . ? O20' Si1 O20 W4 -178.8(5) 3_666 . . . ? O20' Si1 O20 O20' 179.997(3) 3_666 . . . ? O21 C19 C20 O26 -66.2(17) . . . . ? O22 C17 C18 O21 57.9(12) . . . . ? O23 C15 C16 O22 -61.8(12) . . . . ? O24 C13 C14 O23 64.2(12) . . . . ? O25 C23 C24 O24 -69.7(13) . . . . ? O26 C21 C22 O25 66.5(15) . . . . ? C13 O24 C24 C23 -179.7(10) . . . . ? C14 O23 C15 C16 -178.4(9) . . . . ? C15 O23 C14 C13 176.2(9) . . . . ? C16 O22 C17 C18 -174.5(9) . . . . ? C17 O22 C16 C15 -177.7(9) . . . . ? C18 O21 C19 C20 -178.6(12) . . . . ? C19 O21 C18 C17 175.6(10) . . . . ? C20 O26 C21 C22 -174.4(13) . . . . ? C21 O26 C20 C19 -179.4(13) . . . . ? C22 O25 C23 C24 -176.0(11) . . . . ? C23 O25 C22 C21 176.5(11) . . . . ? C24 O24 C13 C14 -174.9(10) . . . . ? K2 O27 C2 C1 -62.5(10) . . . . ? K2 O27 C3 C4 55.5(12) . . . . ? K2 O28 C4 C3 43.4(14) . . . . ? K2 O28 C5 C6 -42.9(15) . . . . ? K2 O29 C6 C5 -58.2(15) . . . . ? K2 O29 C7 C8 54.7(17) . . . . ? K2 O30 C8 C7 31.8(18) . . . . ? K2 O30 C9 C10 -38.3(18) . . . . ? K2 O31 C10 C9 -38.1(18) . . . . ? K2 O31 C11 C12 47.4(17) . . . . ? K2 O32 C1 C2 -35.6(14) . . . . ? K2 O32 C12 C11 44.5(17) . . . . ? O27 C3 C4 O28 -66.6(15) . . . . ? O28 C5 C6 O29 68.6(17) . . . . ? O29 C7 C8 O30 -57.9(19) . . . . ? O30 C9 C10 O31 51(2) . . . . ? O31 C11 C12 O32 -59.9(18) . . . . ? O32 C1 C2 K2 24.5(9) . . . . ? O32 C1 C2 O27 65.7(13) . . . . ? C1 O32 C12 C11 -175.4(13) . . . . ? C2 O27 C3 C4 -178.7(11) . . . . ? C3 O27 C2 K2 -127.1(10) . . . . ? C3 O27 C2 C1 170.4(10) . . . . ? C4 O28 C5 C6 178.8(13) . . . . ? C5 O28 C4 C3 -177.6(11) . . . . ? C6 O29 C7 C8 -179.3(15) . . . . ? C7 O29 C6 C5 174.2(13) . . . . ? C8 O30 C9 C10 -178.8(14) . . . . ? C9 O30 C8 C7 170.9(15) . . . . ? C10 O31 C11 C12 -163.5(14) . . . . ? C11 O31 C10 C9 173.9(14) . . . . ? C12 O32 C1 C2 -176.0(12) . . . . ?