#------------------------------------------------------------------------------ #$Date: 2025-01-18 02:50:49 +0200 (Sat, 18 Jan 2025) $ #$Revision: 297373 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/37/1573714.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_1573714 loop_ _publ_author_name 'Greijer, Bj\"orn' 'Nefedova, Alexandra' 'Agback, Tatiana' 'Agback, Peter' 'Kisand, Vambola' 'Rausalu, Kai' 'Vanetsev, Alexander' 'Seisenbaeva, Gulaim A.' 'Ivask, Angela' 'Kessler, Vadim G.' _publ_section_title ; Molecular Mechanisms behind the Anti Corona Virus Activity of Small Metal Oxide Nanoparticles ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR03730H _journal_year 2025 _chemical_formula_sum 'C24 H42 N12 O58 Si W12' _chemical_formula_weight 3660.98 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-08-30 deposited with the CCDC. 2025-01-17 downloaded from the CCDC. ; _cell_angle_alpha 99.7051(8) _cell_angle_beta 91.9863(9) _cell_angle_gamma 103.7460(9) _cell_formula_units_Z 1 _cell_length_a 10.8473(5) _cell_length_b 12.4152(5) _cell_length_c 13.1760(6) _cell_measurement_reflns_used 9993 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 34.75 _cell_measurement_theta_min 2.59 _cell_volume 1693.76(13) _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device_type 'Bruker D8 Quest ECO' _diffrn_measurement_method 'Omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_unetI/netI 0.0462 _diffrn_reflns_Laue_measured_fraction_full 0.962 _diffrn_reflns_Laue_measured_fraction_max 0.962 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 16418 _diffrn_reflns_point_group_measured_fraction_full 0.962 _diffrn_reflns_point_group_measured_fraction_max 0.962 _diffrn_reflns_theta_full 25.024 _diffrn_reflns_theta_max 25.024 _diffrn_reflns_theta_min 2.837 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 20.424 _exptl_absorpt_correction_T_max 0.32 _exptl_absorpt_correction_T_min 0.24 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Bruker SADABS' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.589 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1636 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_transmission_factor_max 0.32 _exptl_transmission_factor_min 0.24 _refine_diff_density_max 4.514 _refine_diff_density_min -2.369 _refine_diff_density_rms 0.355 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 503 _refine_ls_number_reflns 5757 _refine_ls_number_restraints 590 _refine_ls_restrained_S_all 1.154 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0655 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+128.9648P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1564 _refine_ls_wR_factor_ref 0.1570 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5605 _reflns_number_total 5757 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4nr03730h2.cif _cod_data_source_block shelx _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Empirical' was changed to 'empirical' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 1573714 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.059 _shelx_estimated_absorpt_t_max 0.106 _exptl_absorpt_special_details 'Bruker SADABS' _shelx_res_file ; TITL Gly3SiPW_230726_0m in P1 shelx.res created by SHELXL-2018/3 at 09:22:47 on 30-Aug-2024 CELL 0.71073 10.84730 12.41520 13.17600 99.7051 91.9863 103.7460 ZERR 1.00 0.00050 0.00050 0.00060 0.0008 0.0009 0.0009 LATT 1 SFAC C H N O W SI UNIT 24 42 12 58 12 1 LIST 4 TEMP 23 ACTA L.S. 256 OMIT 0 50.05 OMIT -3 4 1 OMIT -4 1 2 OMIT -2 4 1 OMIT 6 -3 1 SIZE 0.32 0.24 0.20 SIMU DELU BOND TWIN FMAP 2 PLAN 80 ISOR 0.001 O2 O2A O4 O16 O22 O18 O5 O6 O13 O14 O15 O7 O1Y WGHT 0.019700 128.964798 BASF 1.24650 FVAR 0.06635 W2 5 0.495435 0.737340 0.385286 11.00000 0.03393 0.04229 = 0.02227 0.01640 0.00830 0.02301 W3 5 0.211217 0.314814 0.540276 11.00000 0.01829 0.05471 = 0.02241 0.00619 0.00544 -0.00665 W4 5 0.404151 0.224843 0.351076 11.00000 0.02715 0.03497 = 0.03578 -0.01477 -0.00486 0.01159 W5 5 0.206121 0.553333 0.429648 11.00000 0.01775 0.02399 = 0.02543 0.01079 -0.00002 0.00560 W6 5 0.396146 0.461355 0.236717 11.00000 0.02650 0.02371 = 0.01812 0.00646 -0.00312 0.00504 W1 5 0.308992 0.588691 0.692311 11.00000 0.02759 0.02042 = 0.02849 0.00352 0.01578 0.00456 SI1 6 0.500000 0.500000 0.500000 10.50000 0.01271 0.01770 = 0.01791 0.00249 0.00244 0.00300 O19 4 0.073074 0.229068 0.560014 11.00000 0.02570 0.03567 = 0.04759 0.01272 -0.00255 -0.00197 O20 4 0.361143 0.094478 0.281215 11.00000 0.03208 0.03283 = 0.03933 0.00280 -0.00779 0.00123 O1 4 0.220280 0.628034 0.786141 11.00000 0.07235 0.07026 = 0.04658 0.02800 0.03606 0.06061 O2 4 0.349623 0.447543 0.113170 11.00000 0.04800 0.05000 = 0.04535 0.00861 0.00417 0.00983 O3 4 0.489127 0.848089 0.329155 11.00000 0.06176 0.02644 = 0.06480 0.01862 0.03115 0.01311 O4 4 0.669400 0.740352 0.383304 11.00000 0.06260 0.06402 = 0.06305 0.01090 0.00495 0.01615 O5 4 0.320914 0.689951 0.413768 11.00000 0.04419 0.04352 = 0.04404 0.00775 0.00455 0.01032 O6 4 0.247392 0.217128 0.419461 11.00000 0.05852 0.05940 = 0.05842 0.00992 0.00527 0.01505 O7 4 0.569007 0.453333 0.226538 11.00000 0.05572 0.05606 = 0.05699 0.01046 0.00413 0.01419 O8 4 0.069050 0.578296 0.393659 11.00000 0.03040 0.06820 = 0.07961 -0.01662 -0.01765 0.03107 O9 4 0.247131 0.483043 0.299855 11.00000 0.05610 0.02722 = 0.05362 -0.00008 0.02878 -0.00201 O10 4 0.358109 0.495926 0.528338 10.50000 0.02732 0.04210 = 0.03918 0.01190 0.01072 0.01620 O11 4 0.460974 0.620220 0.267287 11.00000 0.05146 0.03317 = 0.05991 0.00174 0.02702 -0.00292 O12 4 0.574374 0.458602 0.582541 10.50000 0.01580 0.03867 = 0.01725 0.00358 0.00403 0.00401 O13 4 0.221752 0.609450 0.575286 11.00000 0.05042 0.04953 = 0.04919 0.00947 0.00346 0.01188 O14 4 0.428048 0.726154 0.689615 11.00000 0.05029 0.04986 = 0.05137 0.00956 0.00394 0.01228 O15 4 0.350878 0.312747 0.260030 11.00000 0.05157 0.05094 = 0.05228 0.00985 0.00394 0.01274 O16 4 0.153234 0.405761 0.458440 11.00000 0.05182 0.05047 = 0.05030 0.00982 0.00390 0.01161 O17 4 0.229788 0.432290 0.656696 11.00000 0.09589 0.03101 = 0.03589 0.01281 0.00044 -0.01593 O18 4 0.524462 0.803449 0.529785 11.00000 0.06530 0.06629 = 0.06507 0.01114 0.00487 0.01668 N2 3 0.753163 1.120120 0.435192 11.00000 0.04373 0.02421 = 0.03167 0.00591 0.00981 0.01803 AFIX 43 H2A 2 0.730365 1.179087 0.463938 11.00000 -1.20000 AFIX 0 O3X 4 0.938381 0.650643 0.009239 11.00000 0.05711 0.05791 = 0.02107 0.01318 0.00747 0.02441 N1 3 0.920273 1.201644 0.288108 11.00000 0.03771 0.03360 = 0.03191 0.00231 0.01001 0.00446 AFIX 43 H1A 2 0.936943 1.222655 0.353757 11.00000 -1.20000 AFIX 0 O1X 4 1.116754 1.187297 0.070874 11.00000 0.08015 0.07364 = 0.03578 0.02508 0.02406 0.04382 O2X 4 1.092562 1.087690 0.194297 11.00000 0.04946 0.05382 = 0.05026 0.03014 0.01735 0.02250 N3 3 0.914724 1.055978 0.657489 11.00000 0.04084 0.03305 = 0.03730 0.01234 -0.00034 0.00555 AFIX 33 H3A 2 0.917483 1.077889 0.725594 11.00000 -1.50000 H3B 2 0.889857 0.981090 0.641772 11.00000 -1.50000 H3C 2 0.991736 1.079337 0.635892 11.00000 -1.50000 AFIX 0 O3A 4 0.789101 1.086088 0.160889 11.00000 0.07827 0.04824 = 0.02560 0.00614 -0.00376 0.01220 O4X 4 0.867361 0.994585 0.452677 11.00000 0.06010 0.04364 = 0.04438 -0.00456 -0.00813 0.03303 O1A 4 0.682884 0.864445 0.122273 11.00000 0.05307 0.05656 = 0.04498 0.00072 -0.00615 0.01160 C3 1 0.811519 1.123394 0.250393 11.00000 0.03274 0.03138 = 0.02385 0.00357 0.00208 0.01440 C5 1 0.817435 1.069343 0.491667 11.00000 0.03506 0.02809 = 0.03556 0.00644 0.00358 0.00801 C4 1 0.721362 1.077717 0.326829 11.00000 0.02459 0.03938 = 0.03806 0.00931 0.00336 0.00969 AFIX 43 H4A 2 0.646435 1.022968 0.303940 11.00000 -1.20000 AFIX 0 N1A 3 0.828135 0.637427 0.149809 11.00000 0.06221 0.04285 = 0.04131 0.02076 0.02166 0.01402 AFIX 43 H1AA 2 0.823473 0.614411 0.207900 11.00000 -1.20000 AFIX 0 C6 1 0.823134 1.105385 0.606125 11.00000 0.03165 0.04574 = 0.03248 0.01177 0.00897 0.01076 AFIX 23 H6A 2 0.849446 1.187003 0.623826 11.00000 -1.20000 H6B 2 0.739320 1.080804 0.630182 11.00000 -1.20000 AFIX 0 C1 1 1.073388 1.167672 0.161758 11.00000 0.03315 0.03969 = 0.02955 0.01765 0.00518 0.00864 O21 4 0.500645 0.566779 0.613634 10.50000 0.03731 0.04112 = 0.02391 -0.00009 0.00447 0.01358 O4A 4 1.166638 0.780557 0.175360 11.00000 0.06912 0.05544 = 0.04655 -0.00376 0.01223 0.01795 C2 1 1.009092 1.250356 0.218022 11.00000 0.04157 0.04021 = 0.03723 0.00841 0.01099 0.00760 AFIX 23 H2B 2 1.073007 1.313453 0.257132 11.00000 -1.20000 H2C 2 0.963464 1.279056 0.168315 11.00000 -1.20000 AFIX 0 C2A 1 0.729227 0.688306 0.118756 11.00000 0.04339 0.05456 = 0.04097 0.01303 0.01626 0.00940 AFIX 23 H2AA 2 0.651634 0.658254 0.149791 11.00000 -1.20000 H2AB 2 0.712061 0.668994 0.044320 11.00000 -1.20000 AFIX 0 C3A 1 0.923701 0.624022 0.096029 11.00000 0.05592 0.04103 = 0.02416 0.01345 0.00516 0.01471 N2A 3 1.136504 0.597163 0.108874 11.00000 0.06288 0.04796 = 0.04324 0.01087 -0.00777 0.02093 AFIX 43 H2AC 2 1.170434 0.546615 0.076732 11.00000 -1.20000 AFIX 0 C5A 1 1.202738 0.705314 0.125890 11.00000 0.05937 0.04522 = 0.02917 0.01114 0.00310 0.02416 O2A 4 0.867266 0.865077 0.192077 11.00000 0.05954 0.05935 = 0.06033 0.01029 0.00350 0.01505 C1A 1 0.766881 0.813138 0.150639 11.00000 0.04832 0.05508 = 0.03292 0.01378 0.01095 0.01775 N3A 3 1.393648 0.847158 0.108305 11.00000 0.06257 0.07225 = 0.04840 0.01790 0.00564 0.00699 AFIX 33 H3A1 2 1.468063 0.860463 0.080368 11.00000 -1.50000 H3A2 2 1.345577 0.888652 0.085962 11.00000 -1.50000 H3A3 2 1.406703 0.865094 0.176781 11.00000 -1.50000 AFIX 0 C4A 1 1.017527 0.564564 0.140659 11.00000 0.06664 0.04591 = 0.04336 0.02403 0.00115 0.01765 AFIX 23 H4AA 2 1.021725 0.581635 0.215487 11.00000 -1.20000 H4AB 2 0.985974 0.483616 0.119281 11.00000 -1.20000 AFIX 0 C6A 1 1.328943 0.727707 0.078424 11.00000 0.07668 0.05727 = 0.04300 0.01526 0.02076 0.02899 AFIX 23 H6AA 2 1.381335 0.682069 0.102023 11.00000 -1.20000 H6AB 2 1.315223 0.707548 0.003793 11.00000 -1.20000 AFIX 0 O1Y 4 1.243639 0.981439 0.055146 10.50000 0.01670 0.01652 = 0.01604 0.00300 0.00139 0.00494 O22 4 0.570983 0.634136 0.494472 11.00000 0.05298 0.05261 = 0.05294 0.01030 0.00401 0.01285 HKLF 4 REM Gly3SiPW_230726_0m in P1 REM wR2 = 0.1570, GooF = S = 1.181, Restrained GooF = 1.154 for all data REM R1 = 0.0655 for 5605 Fo > 4sig(Fo) and 0.0666 for all 5757 data REM 503 parameters refined using 590 restraints END WGHT 0.0000 127.9848 REM Highest difference peak 4.514, deepest hole -2.369, 1-sigma level 0.355 Q1 1 0.2768 0.2780 0.4188 11.00000 0.05 4.51 Q2 1 1.5003 0.8808 -0.0783 11.00000 0.05 4.01 Q3 1 0.5453 0.8570 0.5231 11.00000 0.05 3.59 Q4 1 0.6877 0.7884 0.3724 11.00000 0.05 3.35 Q5 1 0.6416 0.6869 0.3843 11.00000 0.05 3.24 Q6 1 0.0933 0.4084 0.4561 11.00000 0.05 3.04 Q7 1 0.5014 0.7500 0.5291 11.00000 0.05 3.02 Q8 1 0.2072 0.4003 0.4576 11.00000 0.05 2.86 Q9 1 0.2788 0.5983 0.5701 11.00000 0.05 2.76 Q10 1 0.1683 0.6174 0.5828 11.00000 0.05 2.66 Q11 1 0.4325 0.7428 0.7395 11.00000 0.05 2.61 Q12 1 0.5626 0.4686 0.2749 11.00000 0.05 2.60 Q13 1 0.4327 0.7100 0.6421 11.00000 0.05 2.33 Q14 1 0.5708 0.4389 0.1784 11.00000 0.05 2.26 Q15 1 0.3530 0.3006 0.2124 11.00000 0.05 2.16 Q16 1 0.3581 0.6798 0.4474 11.00000 0.05 2.05 Q17 1 0.3659 0.3283 0.3084 11.00000 0.05 1.87 Q18 1 1.1979 0.9411 0.0474 11.00000 0.05 1.86 Q19 1 0.2302 0.1717 0.4205 11.00000 0.05 1.73 Q20 1 0.2867 0.7040 0.3816 11.00000 0.05 1.69 Q21 1 0.2783 0.4794 0.3374 11.00000 0.05 1.47 Q22 1 1.2732 1.0183 0.0603 11.00000 0.05 1.44 Q23 1 0.1374 0.4933 0.2158 11.00000 0.05 1.24 Q24 1 0.3613 0.3973 0.1094 11.00000 0.05 1.23 Q25 1 0.1814 0.4361 0.6750 11.00000 0.05 1.20 Q26 1 0.2813 0.4331 0.6430 11.00000 0.05 1.18 Q27 1 0.3538 0.5000 0.1169 11.00000 0.05 1.17 Q28 1 1.0091 0.5394 0.0192 11.00000 0.05 1.17 Q29 1 1.4029 0.6363 -0.0365 11.00000 0.05 1.16 Q30 1 0.7862 0.9190 0.3415 11.00000 0.05 1.15 Q31 1 0.3673 0.5106 0.6172 11.00000 0.05 1.12 Q32 1 0.2046 0.4808 0.2726 11.00000 0.05 1.11 Q33 1 0.3924 0.4366 0.5197 11.00000 0.05 1.07 Q34 1 0.6331 1.1792 0.5082 11.00000 0.05 1.06 Q35 1 0.2957 0.5760 0.3797 11.00000 0.05 1.03 Q36 1 0.4989 0.6177 0.2995 11.00000 0.05 1.01 Q37 1 -0.0091 0.4083 0.4739 11.00000 0.05 1.00 Q38 1 0.7036 0.4794 0.1955 11.00000 0.05 0.99 Q39 1 0.3877 0.0999 0.3623 11.00000 0.05 0.98 Q40 1 0.5274 0.5397 0.3164 11.00000 0.05 0.96 Q41 1 0.4028 0.5261 0.1323 11.00000 0.05 0.96 Q42 1 0.2505 0.6651 0.7802 11.00000 0.05 0.96 Q43 1 0.4703 0.4580 0.2375 11.00000 0.05 0.96 Q44 1 0.3837 0.1642 0.3397 11.00000 0.05 0.96 Q45 1 0.3616 0.5946 0.7416 11.00000 0.05 0.96 Q46 1 0.2588 0.3379 0.4948 11.00000 0.05 0.95 Q47 1 0.1641 0.6432 0.8377 11.00000 0.05 0.94 Q48 1 0.3129 0.1853 0.1982 11.00000 0.05 0.94 Q49 1 0.5675 0.9320 0.4845 11.00000 0.05 0.93 Q50 1 1.2476 1.1226 0.0803 11.00000 0.05 0.91 Q51 1 0.5179 0.8605 0.3998 11.00000 0.05 0.91 Q52 1 0.1446 0.3193 0.5420 11.00000 0.05 0.91 Q53 1 0.3175 0.4861 0.1864 11.00000 0.05 0.90 Q54 1 0.4572 0.4386 0.2973 11.00000 0.05 0.90 Q55 1 0.2726 0.4042 0.3235 11.00000 0.05 0.89 Q56 1 0.2299 0.3584 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91.67 5.49 -1 4 -5 206.68 12.02 -2 4 -5 138.36 7.47 -2 4 -5 115.44 7.42 -3 4 -5 22.50 1.44 -3 4 -5 19.00 1.27 -3 4 -5 20.81 1.28 3 -4 5 19.60 1.22 -4 4 -5 4.19 0.34 -4 4 -5 3.60 0.32 4 -4 5 3.38 0.31 -5 4 -5 65.75 3.85 -5 4 -5 67.96 4.18 -5 4 -5 64.81 3.81 5 -4 5 64.71 3.80 5 -4 5 63.82 3.83 -6 4 -5 92.81 5.63 6 -4 5 89.51 5.25 6 -4 5 89.31 5.28 -7 4 -5 4.67 0.35 -7 4 -5 4.58 0.76 7 -4 5 4.05 0.34 7 -4 5 4.03 0.40 -8 4 -5 7.44 1.02 -8 4 -5 6.39 0.49 8 -4 5 7.05 0.55 -9 4 -5 9.70 1.21 -9 4 -5 8.61 0.62 9 -4 5 8.84 0.67 -10 4 -5 40.02 2.45 -10 4 -5 37.22 2.93 10 -4 5 43.57 2.50 -11 4 -5 23.68 2.11 11 -4 5 26.24 1.64 -12 4 -5 13.28 1.70 12 -4 5 19.66 1.24 -13 4 -5 7.27 1.26 13 -4 5 9.43 0.79 -14 4 -5 1.64 0.83 14 -4 5 1.69 0.42 -15 4 -5 0.38 0.71 16 -4 5 1.43 0.76 15 3 -5 -0.05 0.70 14 3 -5 11.22 1.05 13 3 -5 3.44 0.54 -13 -3 5 2.62 0.86 12 3 -5 94.29 5.78 11 3 -5 77.90 4.30 -11 -3 5 60.88 4.64 10 3 -5 22.25 1.44 -10 -3 5 19.46 1.85 9 3 -5 1.12 0.30 9 3 -5 1.04 0.27 -9 -3 5 1.87 0.67 8 3 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1.95 1.14 6 4 -19 -0.53 0.71 5 4 -19 17.75 1.75 4 4 -19 0.96 0.80 3 4 -19 3.48 0.72 2 4 -19 6.32 0.93 -2 -4 19 9.37 0.90 1 4 -19 0.60 0.53 -1 -4 19 0.64 0.39 0 4 -19 0.70 0.52 0 -4 19 0.86 0.42 -1 4 -19 26.47 1.99 1 -4 19 27.07 1.89 -2 4 -19 58.02 3.61 2 -4 19 52.87 3.51 -3 4 -19 0.90 0.54 3 -4 19 0.19 0.41 -4 4 -19 0.04 0.47 4 -4 19 0.36 0.49 5 -4 19 7.02 0.90 -6 4 -19 0.83 0.64 6 -4 19 0.98 0.53 7 3 -19 0.96 0.83 6 3 -19 2.33 0.82 5 3 -19 3.31 0.89 4 3 -19 1.42 0.71 3 3 -19 0.97 0.58 -3 -3 19 0.69 0.45 2 3 -19 11.54 1.26 -2 -3 19 13.41 1.13 1 3 -19 -0.25 0.47 -1 -3 19 0.48 0.38 0 3 -19 1.27 0.56 0 -3 19 0.28 0.41 -1 3 -19 51.74 3.20 1 -3 19 44.70 3.07 -2 3 -19 36.19 2.57 2 -3 19 37.27 2.47 -3 3 -19 -0.87 0.44 3 -3 19 0.83 0.49 -4 3 -19 0.60 0.60 4 -3 19 0.82 0.52 -5 3 -19 4.90 0.92 5 -3 19 3.60 0.67 -6 3 -19 5.14 0.85 6 -3 19 4.17 0.74 -7 3 -19 3.54 0.79 7 2 -19 0.45 0.70 6 2 -19 4.13 0.91 5 2 -19 17.25 1.77 4 2 -19 7.42 1.07 -4 -2 19 9.32 0.95 3 2 -19 1.08 0.58 -3 -2 19 1.51 0.49 2 2 -19 1.71 0.57 -2 -2 19 0.65 0.42 1 2 -19 2.00 0.61 -1 -2 19 1.81 0.49 0 2 -19 1.03 0.53 0 -2 19 0.41 0.43 -1 2 -19 2.81 0.66 1 -2 19 1.87 0.51 -2 2 -19 1.72 0.59 2 -2 19 -0.20 0.37 -3 2 -19 2.40 0.64 4 -2 19 3.34 0.62 -5 2 -19 4.77 0.84 5 -2 19 5.55 0.77 -6 2 -19 5.84 0.94 6 -2 19 6.93 0.94 7 1 -19 4.82 0.99 6 1 -19 11.88 1.31 5 1 -19 21.01 1.87 -5 -1 19 18.96 1.55 4 1 -19 1.10 0.75 -4 -1 19 2.43 0.58 3 1 -19 2.49 0.67 -3 -1 19 4.07 0.63 2 1 -19 2.60 0.66 -2 -1 19 3.07 0.58 1 1 -19 1.04 0.52 -1 -1 19 0.28 0.43 0 1 -19 0.88 0.53 0 -1 19 1.47 0.48 -1 1 -19 6.01 0.87 1 -1 19 6.24 0.77 -2 1 -19 0.33 0.50 2 -1 19 -0.11 0.41 3 -1 19 2.03 0.60 -4 1 -19 4.36 0.79 4 -1 19 4.94 0.72 -5 1 -19 10.65 1.24 5 -1 19 13.56 1.20 -6 1 -19 2.64 0.86 7 0 -19 9.39 1.17 6 0 -19 4.10 0.83 -6 0 19 4.82 0.94 5 0 -19 3.23 0.78 -5 0 19 2.60 0.60 -4 0 19 2.12 0.57 3 0 -19 3.64 0.76 -3 0 19 6.25 0.77 2 0 -19 1.79 0.59 -2 0 19 2.59 0.56 1 0 -19 37.68 2.66 -1 0 19 39.62 2.58 0 0 -19 2.86 0.68 0 0 19 3.85 0.61 -1 0 -19 0.27 0.55 1 0 19 0.71 0.46 2 0 19 18.57 2.03 -3 0 -19 10.64 1.17 3 0 19 10.74 1.07 -4 0 -19 8.71 1.06 4 0 19 7.42 0.90 -5 0 -19 4.85 0.84 5 0 19 3.39 0.68 7 -1 -19 1.56 0.65 -7 1 19 0.94 0.87 6 -1 -19 0.49 0.58 -6 1 19 -0.01 0.55 5 -1 -19 2.59 0.69 4 -1 -19 1.02 0.92 -4 1 19 1.18 0.57 -3 1 19 3.37 0.65 2 -1 -19 25.19 2.17 -2 1 19 22.62 1.74 1 -1 -19 70.24 4.72 -1 1 19 68.84 4.39 0 1 19 5.03 1.10 -1 -1 -19 0.76 0.83 1 1 19 -0.39 0.63 -2 -1 -19 8.61 0.99 2 1 19 6.87 0.84 -3 -1 -19 0.81 0.56 3 1 19 0.63 0.44 -4 -1 -19 8.59 1.05 4 1 19 7.47 0.89 7 -2 -19 2.09 0.71 -7 2 19 1.49 0.59 6 -2 -19 0.63 0.55 -6 2 19 -0.27 0.44 5 -2 -19 0.87 0.54 -5 2 19 0.32 0.46 4 -2 -19 2.29 0.62 -4 2 19 2.36 0.62 -3 2 19 3.08 1.01 2 -2 -19 5.82 1.05 -2 2 19 8.44 1.34 1 -2 -19 12.12 1.44 -1 2 19 11.31 1.22 0 -2 -19 -0.72 0.47 0 2 19 0.48 0.46 -1 -2 -19 3.90 0.74 1 2 19 3.61 0.64 -2 -2 -19 4.22 0.77 2 2 19 3.65 0.63 -3 -2 -19 5.83 0.88 3 2 19 5.69 0.76 -7 3 19 0.25 0.56 6 -3 -19 0.98 0.56 -6 3 19 -0.13 0.47 5 -3 -19 2.36 0.63 -5 3 19 1.57 0.54 4 -3 -19 3.13 0.68 -4 3 19 3.06 0.62 3 -3 -19 1.53 0.60 -3 3 19 2.18 0.56 2 -3 -19 3.32 0.69 -2 3 19 2.84 0.59 1 -3 -19 0.18 0.47 -1 3 19 -0.22 0.39 0 -3 -19 0.97 0.55 0 3 19 0.76 0.45 -1 -3 -19 2.40 0.64 1 3 19 3.34 0.61 -2 -3 -19 6.93 0.97 2 3 19 7.87 0.89 6 -4 -19 0.50 0.57 5 -4 -19 3.96 0.74 -5 4 19 3.05 0.69 4 -4 -19 3.24 0.67 -4 4 19 1.50 0.55 3 -4 -19 1.28 0.59 -3 4 19 0.24 0.45 2 -4 -19 2.18 0.63 -2 4 19 2.35 0.55 1 -4 -19 5.78 0.86 -1 4 19 7.35 0.86 0 -4 -19 33.43 2.36 0 4 19 31.14 2.23 -1 -4 -19 1.36 0.68 1 4 19 1.22 0.54 4 -5 -19 29.54 2.26 3 -5 -19 8.21 1.02 -3 5 19 8.83 1.40 2 -5 -19 0.75 0.55 -2 5 19 -0.20 0.80 1 -5 -19 22.36 2.38 3 8 -20 3.27 0.84 2 8 -20 1.66 0.63 1 8 -20 1.08 0.56 3 -8 20 1.11 0.47 4 -8 20 1.10 0.56 3 7 -20 15.86 1.53 2 7 -20 0.80 0.55 1 7 -20 0.26 0.51 0 7 -20 31.00 2.26 -1 7 -20 40.69 2.99 2 -7 20 1.52 0.47 3 -7 20 1.02 0.48 4 -7 20 6.45 0.85 4 6 -20 1.47 0.71 3 6 -20 2.28 0.68 2 6 -20 0.12 0.50 1 6 -20 0.14 0.49 0 6 -20 6.67 1.01 0 -6 20 6.15 1.11 -1 6 -20 5.25 0.92 1 -6 20 5.40 0.79 -2 6 -20 0.06 0.56 2 -6 20 0.19 0.40 3 -6 20 3.03 0.62 4 -6 20 2.92 0.63 4 5 -20 4.04 0.85 3 5 -20 0.68 0.60 2 5 -20 0.10 0.51 1 5 -20 0.42 0.53 -1 -5 20 -0.05 0.42 0 5 -20 4.83 0.93 -1 5 -20 0.05 0.58 1 -5 20 1.07 0.56 -2 5 -20 1.42 0.60 2 -5 20 0.77 0.46 -3 5 -20 12.16 1.16 3 -5 20 8.71 1.01 -4 5 -20 13.45 1.32 4 -5 20 13.31 1.25 5 4 -20 0.64 0.82 4 4 -20 2.67 0.74 3 4 -20 0.15 0.54 2 4 -20 24.45 1.94 -2 -4 20 25.48 1.87 1 4 -20 2.33 0.66 -1 -4 20 2.66 0.66 0 4 -20 7.17 1.01 -1 4 -20 5.52 0.87 1 -4 20 4.38 0.76 -2 4 -20 6.42 0.87 2 -4 20 5.59 0.76 -3 4 -20 6.53 0.89 3 -4 20 7.10 0.84 -4 4 -20 6.23 0.88 4 -4 20 5.59 0.81 -5 4 -20 0.84 0.56 5 3 -20 2.78 0.82 4 3 -20 1.04 0.60 3 3 -20 8.56 1.09 -3 -3 20 9.71 1.17 2 3 -20 63.77 4.05 -2 -3 20 60.23 4.31 1 3 -20 8.77 1.06 0 3 -20 0.16 0.50 0 -3 20 -0.48 0.67 -1 3 -20 14.05 1.34 1 -3 20 13.46 1.21 -2 3 -20 4.50 0.76 2 -3 20 4.03 0.66 -3 3 -20 5.81 0.84 3 -3 20 6.46 0.82 -4 3 -20 0.66 0.55 4 -3 20 1.30 0.59 -5 3 -20 7.74 1.48 5 2 -20 0.75 0.64 4 2 -20 4.48 0.83 3 2 -20 6.23 0.93 2 2 -20 22.49 1.81 1 2 -20 0.99 0.57 -1 -2 20 1.04 0.51 0 2 -20 -0.46 0.48 0 -2 20 0.22 0.41 -1 2 -20 2.09 0.63 1 -2 20 2.23 0.55 -2 2 -20 2.13 0.62 2 -2 20 2.50 0.54 -3 2 -20 6.64 0.91 3 -2 20 7.12 0.86 -4 2 -20 0.46 0.56 5 1 -20 4.79 0.88 4 1 -20 2.70 0.71 -4 -1 20 3.20 0.63 3 1 -20 1.97 0.63 -3 -1 20 1.23 0.49 2 1 -20 -0.09 0.49 -2 -1 20 0.36 0.40 1 1 -20 0.93 0.57 -1 -1 20 0.87 0.45 0 1 -20 1.80 0.62 0 -1 20 1.87 0.51 -1 1 -20 10.29 1.14 1 -1 20 10.78 1.06 -2 1 -20 7.38 0.95 2 -1 20 7.48 0.89 -3 1 -20 3.68 0.76 3 -1 20 4.55 0.77 5 0 -20 0.49 0.73 -5 0 20 1.25 0.50 4 0 -20 0.96 0.60 -4 0 20 0.43 0.45 3 0 -20 3.72 0.75 -3 0 20 4.38 0.67 2 0 -20 1.37 0.58 -2 0 20 0.48 0.44 1 0 -20 17.99 1.53 -1 0 20 16.12 1.38 0 0 -20 1.84 0.63 0 0 20 1.15 0.49 -1 0 -20 10.78 1.16 1 0 20 10.35 1.04 -2 0 -20 1.34 0.57 2 0 20 0.48 0.45 -6 1 20 -0.13 0.55 -5 1 20 30.86 2.20 4 -1 -20 15.02 1.49 -4 1 20 13.51 1.25 3 -1 -20 0.36 0.53 -3 1 20 0.55 0.46 2 -1 -20 13.65 1.32 -2 1 20 11.83 1.15 1 -1 -20 38.72 2.54 -1 1 20 32.37 2.38 0 -1 -20 0.20 0.51 0 1 20 0.14 0.43 -1 -1 -20 3.96 0.77 1 1 20 4.25 0.70 -4 2 20 7.66 1.04 3 -2 -20 0.06 0.60 -3 2 20 0.12 0.42 2 -2 -20 1.98 0.69 -2 2 20 1.13 0.51 1 -2 -20 4.05 0.83 -1 2 20 3.01 0.64 0 -2 -20 1.52 1.01 0 2 20 2.03 0.90 0 6 -21 4.40 0.96 -1 6 -21 0.64 0.59 1 -6 21 1.79 0.56 0 5 -21 9.05 1.18 0 -5 21 7.79 0.88 -1 5 -21 10.26 1.26 1 -5 21 8.93 1.14 -1 -4 21 1.52 0.50 0 4 -21 17.74 1.82 0 -4 21 15.59 1.34 -1 4 -21 5.16 1.04 1 -4 21 5.28 1.09 -2 -3 21 29.30 2.06 -1 -3 21 1.86 0.53 0 -3 21 4.21 0.72 -3 -2 21 2.76 0.63 -2 -2 21 8.83 1.00 -1 -2 21 0.11 0.49 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 13507 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W2 W 0.49544(8) 0.73734(7) 0.38529(6) 0.0291(2) Uani 1 1 d . U . . . W3 W 0.21122(7) 0.31481(8) 0.54028(6) 0.0345(2) Uani 1 1 d . U . . . W4 W 0.40415(8) 0.22484(7) 0.35108(7) 0.0347(2) Uani 1 1 d . U . . . W5 W 0.20612(6) 0.55333(6) 0.42965(6) 0.0216(2) Uani 1 1 d . U . . . W6 W 0.39615(7) 0.46135(6) 0.23672(5) 0.0228(2) Uani 1 1 d . U . . . W1 W 0.30899(7) 0.58869(6) 0.69231(6) 0.0255(2) Uani 1 1 d . U . . . Si1 Si 0.500000 0.500000 0.500000 0.0163(12) Uani 1 2 d S U P . . O19 O 0.0731(13) 0.2291(12) 0.5600(12) 0.037(3) Uani 1 1 d . U . . . O20 O 0.3611(14) 0.0945(12) 0.2812(12) 0.037(3) Uani 1 1 d . U . . . O1 O 0.2203(18) 0.6280(16) 0.7861(13) 0.053(4) Uani 1 1 d . U . . . O2 O 0.3496(16) 0.4475(15) 0.1132(13) 0.048(3) Uani 1 1 d . U . . . O3 O 0.4891(17) 0.8481(13) 0.3292(14) 0.049(4) Uani 1 1 d . U . . . O4 O 0.6694(19) 0.7404(17) 0.3833(16) 0.063(3) Uani 1 1 d . U . . . O5 O 0.3209(15) 0.6900(14) 0.4138(13) 0.044(2) Uani 1 1 d . U . . . O6 O 0.2474(18) 0.2171(16) 0.4195(15) 0.059(3) Uani 1 1 d . U . . . O7 O 0.5690(18) 0.4533(16) 0.2265(15) 0.056(3) Uani 1 1 d . U . . . O8 O 0.0690(15) 0.5783(16) 0.3937(16) 0.060(4) Uani 1 1 d . U . . . O9 O 0.2471(16) 0.4830(13) 0.2999(13) 0.048(3) Uani 1 1 d . U . . . O10 O 0.358(3) 0.496(2) 0.528(2) 0.034(3) Uani 0.5 1 d . U P . . O11 O 0.4610(16) 0.6202(13) 0.2673(14) 0.051(3) Uani 1 1 d . U . . . O12 O 0.574(2) 0.459(2) 0.5825(18) 0.024(4) Uani 0.5 1 d . U P . . O13 O 0.2218(17) 0.6095(15) 0.5753(14) 0.050(3) Uani 1 1 d . U . . . O14 O 0.4280(17) 0.7262(15) 0.6896(14) 0.050(3) Uani 1 1 d . U . . . O15 O 0.3509(17) 0.3127(15) 0.2600(14) 0.052(3) Uani 1 1 d . U . . . O16 O 0.1532(17) 0.4058(15) 0.4584(14) 0.051(3) Uani 1 1 d . U . . . O17 O 0.230(2) 0.4323(14) 0.6567(13) 0.059(4) Uani 1 1 d . U . . . O18 O 0.524(2) 0.8034(18) 0.5298(16) 0.066(3) Uani 1 1 d . U . . . N2 N 0.7532(17) 1.1201(14) 0.4352(13) 0.031(3) Uani 1 1 d . U . . . H2A H 0.730365 1.179087 0.463938 0.038 Uiso 1 1 calc R U . . . O3X O 0.9384(16) 0.6506(14) 0.0092(11) 0.043(4) Uani 1 1 d . U . . . N1 N 0.9203(17) 1.2016(15) 0.2881(14) 0.035(4) Uani 1 1 d . U . . . H1A H 0.936943 1.222655 0.353757 0.042 Uiso 1 1 calc R U . . . O1X O 1.1168(19) 1.1873(17) 0.0709(13) 0.057(5) Uani 1 1 d . U . . . O2X O 1.0926(16) 1.0877(14) 0.1943(13) 0.047(4) Uani 1 1 d . U . . . N3 N 0.9147(17) 1.0560(15) 0.6575(14) 0.037(4) Uani 1 1 d . U . . . H3A H 0.917483 1.077889 0.725594 0.056 Uiso 1 1 calc R U . . . H3B H 0.889857 0.981090 0.641772 0.056 Uiso 1 1 calc R U . . . H3C H 0.991736 1.079337 0.635892 0.056 Uiso 1 1 calc R U . . . O3A O 0.7891(18) 1.0861(14) 0.1609(12) 0.052(4) Uani 1 1 d . U . . . O4X O 0.8674(17) 0.9946(14) 0.4527(13) 0.048(4) Uani 1 1 d . U . . . O1A O 0.6829(17) 0.8644(16) 0.1223(13) 0.053(4) Uani 1 1 d . U . . . C3 C 0.8115(19) 1.1234(17) 0.2504(15) 0.028(3) Uani 1 1 d . U . . . C5 C 0.817(2) 1.0693(17) 0.4917(16) 0.033(4) Uani 1 1 d . U . . . C4 C 0.7214(19) 1.0777(18) 0.3268(16) 0.033(4) Uani 1 1 d . U . . . H4A H 0.646435 1.022968 0.303940 0.040 Uiso 1 1 calc R U . . . N1A N 0.828(2) 0.6374(17) 0.1498(16) 0.047(4) Uani 1 1 d . U . . . H1AA H 0.823473 0.614411 0.207900 0.056 Uiso 1 1 calc R U . . . C6 C 0.823(2) 1.1054(19) 0.6061(16) 0.036(4) Uani 1 1 d . U . . . H6A H 0.849446 1.187003 0.623826 0.043 Uiso 1 1 calc R U . . . H6B H 0.739320 1.080804 0.630182 0.043 Uiso 1 1 calc R U . . . C1 C 1.073(2) 1.1677(18) 0.1618(16) 0.033(4) Uani 1 1 d . U . . . O21 O 0.501(3) 0.567(2) 0.614(2) 0.034(4) Uani 0.5 1 d . U P . . O4A O 1.1666(19) 0.7806(16) 0.1754(14) 0.058(4) Uani 1 1 d . U . . . C2 C 1.009(2) 1.2504(19) 0.2180(18) 0.040(4) Uani 1 1 d . U . . . H2B H 1.073007 1.313453 0.257132 0.048 Uiso 1 1 calc R U . . . H2C H 0.963464 1.279056 0.168315 0.048 Uiso 1 1 calc R U . . . C2A C 0.729(2) 0.688(2) 0.1188(19) 0.046(4) Uani 1 1 d . U . . . H2AA H 0.651634 0.658254 0.149791 0.055 Uiso 1 1 calc R U . . . H2AB H 0.712061 0.668994 0.044320 0.055 Uiso 1 1 calc R U . . . C3A C 0.924(2) 0.6240(19) 0.0960(16) 0.039(4) Uani 1 1 d . U . . . N2A N 1.137(2) 0.5972(18) 0.1089(16) 0.050(4) Uani 1 1 d . U . . . H2AC H 1.170434 0.546615 0.076732 0.060 Uiso 1 1 calc R U . . . C5A C 1.203(2) 0.705(2) 0.1259(17) 0.042(4) Uani 1 1 d . U . . . O2A O 0.8673(19) 0.8651(17) 0.1921(15) 0.060(4) Uani 1 1 d . U . . . C1A C 0.767(2) 0.813(2) 0.1506(18) 0.044(4) Uani 1 1 d . U . . . N3A N 1.394(2) 0.847(2) 0.1083(18) 0.062(6) Uani 1 1 d . U . . . H3A1 H 1.468063 0.860463 0.080368 0.093 Uiso 1 1 calc R U . . . H3A2 H 1.345577 0.888652 0.085962 0.093 Uiso 1 1 calc R U . . . H3A3 H 1.406703 0.865094 0.176781 0.093 Uiso 1 1 calc R U . . . C4A C 1.018(3) 0.565(2) 0.141(2) 0.050(5) Uani 1 1 d . U . . . H4AA H 1.021725 0.581635 0.215487 0.059 Uiso 1 1 calc R U . . . H4AB H 0.985974 0.483616 0.119281 0.059 Uiso 1 1 calc R U . . . C6A C 1.329(3) 0.728(2) 0.078(2) 0.056(5) Uani 1 1 d . U . . . H6AA H 1.381335 0.682069 0.102023 0.067 Uiso 1 1 calc R U . . . H6AB H 1.315223 0.707548 0.003793 0.067 Uiso 1 1 calc R U . . . O1Y O 1.244(2) 0.9814(18) 0.0551(17) 0.016(5) Uani 0.5 1 d . U P . . O22 O 0.5710(17) 0.6341(15) 0.4945(14) 0.053(3) Uani 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W2 0.0339(4) 0.0423(5) 0.0223(4) 0.0164(3) 0.0083(3) 0.0230(4) W3 0.0183(4) 0.0547(5) 0.0224(4) 0.0062(4) 0.0054(3) -0.0066(3) W4 0.0272(4) 0.0350(5) 0.0358(5) -0.0148(4) -0.0049(3) 0.0116(3) W5 0.0178(4) 0.0240(4) 0.0254(4) 0.0108(3) 0.0000(3) 0.0056(3) W6 0.0265(4) 0.0237(4) 0.0181(4) 0.0065(3) -0.0031(3) 0.0050(3) W1 0.0276(4) 0.0204(4) 0.0285(4) 0.0035(3) 0.0158(3) 0.0046(3) Si1 0.013(3) 0.018(3) 0.018(3) 0.002(2) 0.002(2) 0.003(2) O19 0.026(6) 0.036(7) 0.048(8) 0.013(6) -0.003(5) -0.002(5) O20 0.032(7) 0.033(6) 0.039(8) 0.003(5) -0.008(6) 0.001(6) O1 0.072(10) 0.070(10) 0.047(7) 0.028(7) 0.036(8) 0.061(9) O2 0.048(4) 0.050(4) 0.045(3) 0.009(2) 0.004(2) 0.010(2) O3 0.062(9) 0.026(6) 0.065(9) 0.019(6) 0.031(8) 0.013(6) O4 0.063(4) 0.064(4) 0.063(4) 0.0109(12) 0.0049(11) 0.0162(13) O5 0.044(3) 0.044(3) 0.044(3) 0.0077(11) 0.0046(10) 0.0103(11) O6 0.059(3) 0.059(3) 0.058(3) 0.0099(11) 0.0053(11) 0.0150(13) O7 0.056(3) 0.056(4) 0.057(4) 0.0105(12) 0.0041(11) 0.0142(13) O8 0.030(6) 0.068(10) 0.080(11) -0.017(9) -0.018(7) 0.031(6) O9 0.056(7) 0.027(6) 0.054(6) 0.000(5) 0.029(6) -0.002(5) O10 0.027(6) 0.042(7) 0.039(8) 0.012(5) 0.011(5) 0.016(5) O11 0.051(8) 0.033(5) 0.060(6) 0.002(5) 0.027(5) -0.003(5) O12 0.016(9) 0.039(11) 0.017(11) 0.004(8) 0.004(7) 0.004(8) O13 0.050(3) 0.050(3) 0.049(3) 0.0095(11) 0.0035(10) 0.0119(12) O14 0.050(3) 0.050(3) 0.051(3) 0.0096(12) 0.0039(11) 0.0123(12) O15 0.052(3) 0.051(3) 0.052(3) 0.0098(12) 0.0039(11) 0.0127(12) O16 0.052(3) 0.050(3) 0.050(3) 0.0098(11) 0.0039(10) 0.0116(12) O17 0.096(11) 0.031(5) 0.036(6) 0.013(4) 0.000(7) -0.016(6) O18 0.065(4) 0.066(4) 0.065(4) 0.0111(12) 0.0049(11) 0.0167(13) N2 0.044(9) 0.024(8) 0.032(6) 0.006(6) 0.010(6) 0.018(7) O3X 0.057(10) 0.058(10) 0.021(7) 0.013(6) 0.007(6) 0.024(8) N1 0.038(8) 0.034(9) 0.032(8) 0.002(6) 0.010(6) 0.004(6) O1X 0.080(13) 0.074(12) 0.036(8) 0.025(8) 0.024(8) 0.044(10) O2X 0.049(9) 0.054(9) 0.050(9) 0.030(8) 0.017(8) 0.023(8) N3 0.041(10) 0.033(9) 0.037(9) 0.012(8) 0.000(7) 0.006(8) O3A 0.078(12) 0.048(9) 0.026(6) 0.006(6) -0.004(7) 0.012(8) O4X 0.060(10) 0.044(9) 0.044(9) -0.005(7) -0.008(8) 0.033(8) O1A 0.053(9) 0.057(9) 0.045(10) 0.001(8) -0.006(7) 0.012(8) C3 0.033(8) 0.031(9) 0.024(6) 0.004(7) 0.002(6) 0.014(6) C5 0.035(10) 0.028(9) 0.036(7) 0.006(7) 0.004(7) 0.008(7) C4 0.025(9) 0.039(10) 0.038(7) 0.009(8) 0.003(6) 0.010(7) N1A 0.062(11) 0.043(9) 0.041(10) 0.021(8) 0.022(8) 0.014(8) C6 0.032(10) 0.046(11) 0.032(7) 0.012(8) 0.009(8) 0.011(8) C1 0.033(10) 0.040(10) 0.030(9) 0.018(8) 0.005(7) 0.009(8) O21 0.037(7) 0.041(10) 0.024(8) 0.000(7) 0.004(6) 0.014(7) O4A 0.069(12) 0.055(9) 0.047(10) -0.004(8) 0.012(8) 0.018(9) C2 0.042(10) 0.040(10) 0.037(10) 0.008(8) 0.011(8) 0.008(7) C2A 0.043(10) 0.055(8) 0.041(12) 0.013(9) 0.016(9) 0.009(7) C3A 0.056(10) 0.041(11) 0.024(8) 0.013(8) 0.005(8) 0.015(9) N2A 0.063(9) 0.048(8) 0.043(11) 0.011(8) -0.008(9) 0.021(8) C5A 0.059(11) 0.045(8) 0.029(10) 0.011(8) 0.003(9) 0.024(7) O2A 0.060(4) 0.059(5) 0.060(5) 0.010(2) 0.003(2) 0.015(2) C1A 0.048(10) 0.055(9) 0.033(11) 0.014(9) 0.011(8) 0.018(8) N3A 0.063(13) 0.072(12) 0.048(13) 0.018(11) 0.006(11) 0.007(10) C4A 0.067(10) 0.046(12) 0.043(12) 0.024(9) 0.001(10) 0.018(8) C6A 0.077(14) 0.057(11) 0.043(13) 0.015(11) 0.021(11) 0.029(9) O1Y 0.017(5) 0.017(5) 0.016(5) 0.003(2) 0.001(2) 0.005(2) O22 0.053(3) 0.053(3) 0.053(3) 0.0103(12) 0.0040(10) 0.0129(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' W W -0.8490 6.8722 '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' 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 O3 W2 O4 101.2(9) . . ? O3 W2 O11 100.1(8) . . ? O4 W2 O11 89.3(8) . . ? O3 W2 O5 99.9(8) . . ? O4 W2 O5 158.8(8) . . ? O11 W2 O5 88.2(7) . . ? O3 W2 O18 102.8(9) . . ? O4 W2 O18 88.9(9) . . ? O11 W2 O18 157.0(8) . . ? O5 W2 O18 85.2(8) . . ? O3 W2 O22 158.4(8) . . ? O4 W2 O22 64.0(8) . . ? O11 W2 O22 95.6(7) . . ? O5 W2 O22 95.3(7) . . ? O18 W2 O22 63.2(8) . . ? O3 W2 O12 156.2(9) . 2_666 ? O4 W2 O12 95.8(8) . 2_666 ? O11 W2 O12 63.4(8) . 2_666 ? O5 W2 O12 64.4(7) . 2_666 ? O18 W2 O12 94.0(8) . 2_666 ? O22 W2 O12 45.4(7) . 2_666 ? O19 W3 O16 100.8(7) . . ? O19 W3 O17 100.8(8) . . ? O16 W3 O17 89.3(8) . . ? O19 W3 O4 101.0(8) . 2_666 ? O16 W3 O4 158.2(8) . 2_666 ? O17 W3 O4 86.2(9) . 2_666 ? O19 W3 O6 96.4(8) . . ? O16 W3 O6 91.9(8) . . ? O17 W3 O6 162.2(9) . . ? O4 W3 O6 86.1(8) 2_666 . ? O19 W3 O22 156.9(7) . 2_666 ? O16 W3 O22 96.9(7) . 2_666 ? O17 W3 O22 94.1(8) . 2_666 ? O4 W3 O22 62.3(8) 2_666 2_666 ? O6 W3 O22 68.1(7) . 2_666 ? O19 W3 O10 156.0(8) . . ? O16 W3 O10 62.9(9) . . ? O17 W3 O10 63.7(8) . . ? O4 W3 O10 96.2(9) 2_666 . ? O6 W3 O10 101.3(9) . . ? O22 W3 O10 47.0(8) 2_666 . ? O20 W4 O18 100.3(8) . 2_666 ? O20 W4 O14 100.4(7) . 2_666 ? O18 W4 O14 88.1(8) 2_666 2_666 ? O20 W4 O15 102.5(7) . . ? O18 W4 O15 157.2(9) 2_666 . ? O14 W4 O15 87.6(8) 2_666 . ? O20 W4 O6 96.3(8) . . ? O18 W4 O6 87.5(9) 2_666 . ? O14 W4 O6 163.3(8) 2_666 . ? O15 W4 O6 90.2(8) . . ? O20 W4 O22 155.5(7) . 2_666 ? O18 W4 O22 62.2(8) 2_666 2_666 ? O14 W4 O22 96.3(7) 2_666 2_666 ? O15 W4 O22 96.0(7) . 2_666 ? O6 W4 O22 67.4(7) . 2_666 ? O20 W4 O21 156.7(8) . 2_666 ? O18 W4 O21 96.1(9) 2_666 2_666 ? O14 W4 O21 63.7(8) 2_666 2_666 ? O15 W4 O21 62.0(8) . 2_666 ? O6 W4 O21 100.7(8) . 2_666 ? O22 W4 O21 47.8(8) 2_666 2_666 ? O8 W5 O16 102.1(9) . . ? O8 W5 O5 100.3(9) . . ? O16 W5 O5 157.6(7) . . ? O8 W5 O9 99.5(9) . . ? O16 W5 O9 85.9(7) . . ? O5 W5 O9 89.3(7) . . ? O8 W5 O13 101.9(9) . . ? O16 W5 O13 88.3(8) . . ? O5 W5 O13 88.2(7) . . ? O9 W5 O13 158.5(8) . . ? O8 W5 O10 159.6(10) . . ? O16 W5 O10 64.6(9) . . ? O5 W5 O10 94.1(9) . . ? O9 W5 O10 94.9(9) . . ? O13 W5 O10 64.0(9) . . ? O8 W5 O12 157.0(10) . 2_666 ? O16 W5 O12 92.7(8) . 2_666 ? O5 W5 O12 65.7(8) . 2_666 ? O9 W5 O12 63.7(8) . 2_666 ? O13 W5 O12 96.0(8) . 2_666 ? O10 W5 O12 43.3(9) . 2_666 ? O2 W6 O15 103.0(8) . . ? O2 W6 O11 98.9(8) . . ? O15 W6 O11 158.1(8) . . ? O2 W6 O9 101.0(8) . . ? O15 W6 O9 87.6(7) . . ? O11 W6 O9 87.6(7) . . ? O2 W6 O7 100.5(8) . . ? O15 W6 O7 90.4(8) . . ? O11 W6 O7 86.3(8) . . ? O9 W6 O7 158.4(8) . . ? O2 W6 O21 159.7(9) . 2_666 ? O15 W6 O21 65.8(9) . 2_666 ? O11 W6 O21 93.5(9) . 2_666 ? O9 W6 O21 95.5(9) . 2_666 ? O7 W6 O21 64.2(9) . 2_666 ? O2 W6 O12 157.6(9) . 2_666 ? O15 W6 O12 93.5(8) . 2_666 ? O11 W6 O12 65.3(8) . 2_666 ? O9 W6 O12 64.4(8) . 2_666 ? O7 W6 O12 94.3(8) . 2_666 ? O21 W6 O12 42.4(9) 2_666 2_666 ? O1 W1 O13 101.8(8) . . ? O1 W1 O14 101.4(9) . . ? O13 W1 O14 88.5(8) . . ? O1 W1 O7 98.7(8) . 2_666 ? O13 W1 O7 159.4(8) . 2_666 ? O14 W1 O7 89.2(8) . 2_666 ? O1 W1 O17 100.6(9) . . ? O13 W1 O17 88.3(8) . . ? O14 W1 O17 158.0(8) . . ? O7 W1 O17 86.2(8) 2_666 . ? O1 W1 O21 156.8(10) . . ? O13 W1 O21 97.4(9) . . ? O14 W1 O21 66.0(9) . . ? O7 W1 O21 63.2(9) 2_666 . ? O17 W1 O21 92.8(10) . . ? O1 W1 O10 158.5(10) . . ? O13 W1 O10 63.8(9) . . ? O14 W1 O10 94.4(9) . . ? O7 W1 O10 96.0(9) 2_666 . ? O17 W1 O10 64.8(9) . . ? O21 W1 O10 44.5(9) . . ? O12 Si1 O12 180.0(17) 2_666 . ? O12 Si1 O21 66.4(14) 2_666 2_666 ? O12 Si1 O21 113.6(14) . 2_666 ? O12 Si1 O21 113.6(14) 2_666 . ? O12 Si1 O21 66.4(14) . . ? O21 Si1 O21 180.0 2_666 . ? O12 Si1 O10 111.3(13) 2_666 2_666 ? O12 Si1 O10 68.7(13) . 2_666 ? O21 Si1 O10 70.2(15) 2_666 2_666 ? O21 Si1 O10 109.8(15) . 2_666 ? O12 Si1 O10 68.7(13) 2_666 . ? O12 Si1 O10 111.3(13) . . ? O21 Si1 O10 109.8(15) 2_666 . ? O21 Si1 O10 70.2(15) . . ? O10 Si1 O10 180.0 2_666 . ? O12 Si1 O22 70.3(11) 2_666 . ? O12 Si1 O22 109.7(11) . . ? O21 Si1 O22 104.7(13) 2_666 . ? O21 Si1 O22 75.3(13) . . ? O10 Si1 O22 72.6(12) 2_666 . ? O10 Si1 O22 107.4(12) . . ? O12 Si1 O22 109.7(11) 2_666 2_666 ? O12 Si1 O22 70.3(11) . 2_666 ? O21 Si1 O22 75.3(13) 2_666 2_666 ? O21 Si1 O22 104.7(13) . 2_666 ? O10 Si1 O22 107.4(12) 2_666 2_666 ? O10 Si1 O22 72.6(12) . 2_666 ? O22 Si1 O22 180.0 . 2_666 ? W2 O4 W3 136.1(11) . 2_666 ? W5 O5 W2 136.9(9) . . ? W4 O6 W3 129.8(10) . . ? W1 O7 W6 135.9(11) 2_666 . ? W6 O9 W5 137.2(10) . . ? Si1 O10 O12 54.8(12) . 2_666 ? Si1 O10 W5 124.8(15) . . ? O12 O10 W5 70.0(12) 2_666 . ? Si1 O10 W1 122.4(16) . . ? O12 O10 W1 135.1(18) 2_666 . ? W5 O10 W1 94.8(9) . . ? Si1 O10 W3 120.0(15) . . ? O12 O10 W3 128.5(17) 2_666 . ? W5 O10 W3 93.6(10) . . ? W1 O10 W3 93.3(9) . . ? W6 O11 W2 138.0(10) . . ? Si1 O12 O21 57.5(13) . . ? Si1 O12 O10 56.5(12) . 2_666 ? O21 O12 O10 95.9(19) . 2_666 ? Si1 O12 W6 124.8(14) . 2_666 ? O21 O12 W6 67.3(12) . 2_666 ? O10 O12 W6 133.4(17) 2_666 2_666 ? Si1 O12 W5 123.2(13) . 2_666 ? O21 O12 W5 134.9(17) . 2_666 ? O10 O12 W5 66.7(11) 2_666 2_666 ? W6 O12 W5 94.2(8) 2_666 2_666 ? Si1 O12 W2 120.7(13) . 2_666 ? O21 O12 W2 127.7(15) . 2_666 ? O10 O12 W2 128.0(16) 2_666 2_666 ? W6 O12 W2 93.1(8) 2_666 2_666 ? W5 O12 W2 92.4(9) 2_666 2_666 ? W1 O13 W5 137.2(10) . . ? W1 O14 W4 138.0(10) . 2_666 ? W6 O15 W4 138.1(10) . . ? W3 O16 W5 138.3(10) . . ? W1 O17 W3 137.8(9) . . ? W4 O18 W2 138.0(12) 2_666 . ? C5 N2 C4 120.8(17) . . ? C3 N1 C2 120.3(18) . . ? O3A C3 N1 122(2) . . ? O3A C3 C4 120(2) . . ? N1 C3 C4 118.0(17) . . ? O4X C5 N2 122(2) . . ? O4X C5 C6 121.2(19) . . ? N2 C5 C6 116.4(18) . . ? N2 C4 C3 119.0(18) . . ? C3A N1A C2A 124.7(19) . . ? N3 C6 C5 110.1(17) . . ? O2X C1 O1X 119(2) . . ? O2X C1 C2 124.3(19) . . ? O1X C1 C2 117.0(18) . . ? Si1 O21 O12 56.0(12) . . ? Si1 O21 W6 126.3(15) . 2_666 ? O12 O21 W6 70.3(13) . 2_666 ? Si1 O21 W1 122.8(15) . . ? O12 O21 W1 135.9(18) . . ? W6 O21 W1 95.6(10) 2_666 . ? Si1 O21 W4 118.1(15) . 2_666 ? O12 O21 W4 129.1(17) . 2_666 ? W6 O21 W4 93.5(10) 2_666 2_666 ? W1 O21 W4 92.2(9) . 2_666 ? N1 C2 C1 112.6(18) . . ? N1A C2A C1A 111(2) . . ? O3X C3A N1A 124(2) . . ? O3X C3A C4A 119(2) . . ? N1A C3A C4A 117.0(19) . . ? C5A N2A C4A 122(2) . . ? O4A C5A N2A 124(2) . . ? O4A C5A C6A 121(2) . . ? N2A C5A C6A 115(2) . . ? O2A C1A O1A 121(2) . . ? O2A C1A C2A 124(2) . . ? O1A C1A C2A 114(2) . . ? N2A C4A C3A 112.2(19) . . ? N3A C6A C5A 109(2) . . ? Si1 O22 W2 123.5(9) . . ? Si1 O22 W3 120.3(9) . 2_666 ? W2 O22 W3 97.3(7) . 2_666 ? Si1 O22 W4 118.8(9) . 2_666 ? W2 O22 W4 96.0(7) . 2_666 ? W3 O22 W4 94.5(6) 2_666 2_666 ? 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 W2 O3 1.681(15) . ? W2 O4 1.88(2) . ? W2 O11 1.900(17) . ? W2 O5 1.914(16) . ? W2 O18 1.93(2) . ? W2 O22 2.328(18) . ? W2 O12 2.48(3) 2_666 ? W3 O19 1.676(14) . ? W3 O16 1.880(18) . ? W3 O17 1.899(17) . ? W3 O4 1.93(2) 2_666 ? W3 O6 1.944(19) . ? W3 O22 2.378(18) 2_666 ? W3 O10 2.46(3) . ? W4 O20 1.671(14) . ? W4 O18 1.85(2) 2_666 ? W4 O14 1.903(18) 2_666 ? W4 O15 1.912(18) . ? W4 O6 1.942(19) . ? W4 O22 2.412(18) 2_666 ? W4 O21 2.50(3) 2_666 ? W5 O8 1.659(15) . ? W5 O16 1.892(18) . ? W5 O5 1.899(16) . ? W5 O9 1.902(15) . ? W5 O13 1.915(18) . ? W5 O10 2.37(3) . ? W5 O12 2.43(2) 2_666 ? W6 O2 1.656(17) . ? W6 O15 1.874(18) . ? W6 O11 1.897(16) . ? W6 O9 1.898(16) . ? W6 O7 1.909(19) . ? W6 O21 2.35(3) 2_666 ? W6 O12 2.40(2) 2_666 ? W1 O1 1.672(14) . ? W1 O13 1.868(17) . ? W1 O14 1.886(18) . ? W1 O7 1.893(19) 2_666 ? W1 O17 1.898(16) . ? W1 O21 2.41(3) . ? W1 O10 2.41(3) . ? Si1 O12 1.56(3) 2_666 ? Si1 O12 1.56(3) . ? Si1 O21 1.58(3) 2_666 ? Si1 O21 1.58(3) . ? Si1 O10 1.59(3) 2_666 ? Si1 O10 1.59(3) . ? Si1 O22 1.675(18) . ? Si1 O22 1.675(18) 2_666 ? O10 O12 1.77(4) 2_666 ? O12 O21 1.72(4) . ? N2 C5 1.33(3) . ? N2 C4 1.44(3) . ? O3X C3A 1.25(2) . ? N1 C3 1.35(3) . ? N1 C2 1.46(3) . ? O1X C1 1.34(3) . ? O2X C1 1.20(3) . ? N3 C6 1.48(3) . ? O3A C3 1.19(2) . ? O4X C5 1.23(3) . ? O1A C1A 1.31(3) . ? C3 C4 1.51(3) . ? C5 C6 1.49(3) . ? N1A C3A 1.30(3) . ? N1A C2A 1.45(3) . ? C1 C2 1.49(3) . ? O4A C5A 1.20(3) . ? C2A C1A 1.49(4) . ? C3A C4A 1.55(3) . ? N2A C5A 1.34(3) . ? N2A C4A 1.36(3) . ? C5A C6A 1.51(4) . ? O2A C1A 1.19(3) . ? N3A C6A 1.46(4) . ?