#------------------------------------------------------------------------------ #$Date: 2019-07-12 07:21:08 +0300 (Fri, 12 Jul 2019) $ #$Revision: 216970 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552087.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1552087 loop_ _publ_author_name 'Wang, Bin' 'Zou, Xiaodong' 'Smeets, Stef' _publ_section_title ; Automated serial rotation electron diffraction combined with cluster analysis: an efficient multi-crystal workflow for structure determination ; _journal_coeditor_code FC5033 _journal_issue 5 _journal_name_full IUCrJ _journal_page_first ; ; _journal_paper_doi 10.1107/S2052252519007681 _journal_volume 6 _journal_year 2019 _chemical_formula_moiety 'O192 Si96' _chemical_formula_sum 'O192 Si96' _chemical_formula_weight 5768.06 _chemical_name_common ZSM-5 _chemical_name_systematic Si-MFI _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 19.980 _cell_length_b 20.430 _cell_length_c 13.610 _cell_measurement_reflns_used 4734 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 1.80 _cell_measurement_theta_min 0.072 _cell_volume 5555.485 _computing_cell_refinement 'XDS-20180126 (Kabsch, 2018)' _computing_data_collection 'Instamatic-1.0.0 (Smeets et al., 2018)' _computing_data_reduction 'XDS-20180126 (Kabsch, 2018)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2013)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.906 _diffrn_measured_fraction_theta_max 0.851 _diffrn_measurement_device_type 'JEOL JEM-2100 LAB6' _diffrn_measurement_method 'Continuous rotation electron diffraction' _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.0251 _diffrn_reflns_av_R_equivalents 0.2527 _diffrn_reflns_av_unetI/netI 0.2794 _diffrn_reflns_Laue_measured_fraction_full 0.906 _diffrn_reflns_Laue_measured_fraction_max 0.851 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 17584 _diffrn_reflns_point_group_measured_fraction_full 0.906 _diffrn_reflns_point_group_measured_fraction_max 0.851 _diffrn_reflns_theta_full 0.863 _diffrn_reflns_theta_max 0.883 _diffrn_reflns_theta_min 0.064 _diffrn_source 'electron microscope' _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_density_diffrn 1.724 _exptl_crystal_description cuboid _exptl_crystal_F_000 939 _refine_diff_density_max 0.386 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.057 _refine_ls_extinction_coef 2062(32) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.405 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 4734 _refine_ls_number_restraints 348 _refine_ls_restrained_S_all 1.392 _refine_ls_R_factor_all 0.2603 _refine_ls_R_factor_gt 0.2178 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.5024 _refine_ls_wR_factor_ref 0.5448 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2692 _reflns_number_total 4734 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file fc5033.cif _cod_data_source_block zsm5_cluster3 _cod_original_cell_volume 5555.5 _cod_database_code 1552087 _shelx_shelxl_version_number 2014/7 _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_res_file ; shelx_a15_UCtoLit.res created by SHELXL-2014/7 TITL shelx_a.res in Pnma REM Old TITL 16 REM SHELXT solution in Pnma REM R1 0.362, Rweak 0.198, Alpha 0.203, Orientation a'=b, b'=c, c'=a REM Formula found by SHELXT: Si24 O49 CELL 0.02510 19.9800 20.4300 13.6100 90.000 90.000 90.000 ZERR 1.000 0.0000 0.0000 0.0000 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, -Z SYMM 1/2+X, 1/2-Y, 1/2-Z SFAC SI 2.1293 57.7748 2.5333 16.4756 = 0.8349 2.8796 0.3216 0.3860 0.0000 = 0.0000 0.0000 0.0000 1.1100 28.0860 SFAC O 0.4548 23.7803 0.9173 7.6220 = 0.4719 2.1440 0.1384 0.2959 0.0000 = 0.0000 0.0000 0.0000 0.7300 15.9990 UNIT 96 192 L.S. 10 BOND $H LIST 6 EQIV $1 x, -y+3/2, z EQIV $2 x+1/2, y, -z+1/2 EQIV $3 -x+1/2, -y+1, z+1/2 EQIV $4 -x+1/2, -y+1, z-1/2 EQIV $5 x, -y+1/2, z EQIV $6 x-1/2, y, -z+1/2 DFIX 21 0.02 Si1 O1 Si1 O19 Si1 O7 Si1 O4 DFIX 21 0.02 Si2 O11 Si2 O12 Si2 O6 Si2 O21 DFIX 21 0.02 Si3 O18 Si3 O23 Si3 O20 Si3 O9_$6 DFIX 21 0.02 Si4 O16 Si4 O25 Si4 O1_$6 Si4 O13_$4 DFIX 21 0.02 Si5 O4 Si5 O24 Si5 O9 Si5 O5_$4 DFIX 21 0.02 Si6 O24 Si6 O13 Si6 O8 Si6 O6 DFIX 21 0.02 Si7 O14 Si7 O22 Si7 O17 Si7 O15 DFIX 21 0.02 Si8 O14 Si8 O21 Si8 O7_$3 Si8 O3_$3 DFIX 21 0.02 Si9 O10 Si9 O5 Si9 O22 Si9 O2_$3 DFIX 21 0.02 Si10 O17 Si10 O26 Si10 O3 Si10 O16 DFIX 21 0.02 Si11 O20 Si11 O25 Si11 O19_$4 Si11 O15_$4 DFIX 21 0.02 Si12 O11 Si12 O23 Si12 O26 Si12 O2 RIGU FMAP 2 PLAN 20 ACTA WGHT 0.200000 EXTI 2061.602783 FVAR 1.32507 1.61017 SI1 1 0.428964 0.472972 0.311651 11.00000 0.02320 0.03298 = 0.02710 0.00244 -0.00813 0.00361 SI2 1 0.225238 0.672954 0.526989 11.00000 0.02736 0.02644 = 0.05479 0.00158 0.00401 -0.00031 SI3 1 0.078059 0.672304 0.169596 11.00000 0.01729 0.03773 = 0.04298 -0.00680 0.00248 -0.00118 SI4 1 0.077700 0.444063 0.158815 11.00000 0.01979 0.04160 = 0.04069 -0.00741 0.00574 0.00340 SI5 1 0.430539 0.629788 0.313908 11.00000 0.02327 0.03601 = 0.04431 -0.00079 -0.01309 0.00013 SI6 1 0.380017 0.673545 0.525837 11.00000 0.03187 0.02187 = 0.05477 0.00255 0.00015 -0.00194 SI7 1 0.220080 0.437740 0.527069 11.00000 0.02455 0.03702 = 0.04358 0.00252 0.00411 0.00171 SI8 1 0.182693 0.559518 0.663626 11.00000 0.02995 0.04256 = 0.04034 0.00276 0.01025 0.00096 SI9 1 0.184752 0.327649 0.674447 11.00000 0.02792 0.03683 = 0.04370 -0.00227 0.00971 -0.00770 SI10 1 0.194850 0.471410 0.304388 11.00000 0.02487 0.03282 = 0.05127 0.00379 -0.00593 -0.00325 SI11 1 0.122143 0.564109 0.023662 11.00000 0.03506 0.02714 = 0.04528 -0.00794 0.00211 0.00143 SI12 1 0.194207 0.628425 0.311370 11.00000 0.02813 0.03448 = 0.04493 -0.00055 -0.00072 -0.00090 O1 2 0.505301 0.450360 0.292586 11.00000 0.03572 0.04207 = 0.06140 0.01333 -0.00228 0.00619 O2 2 0.259014 0.653047 0.252345 11.00000 0.03785 0.08057 = 0.07868 0.02391 0.00345 -0.00482 O3 2 0.259932 0.445990 0.245887 11.00000 0.04504 0.08955 = 0.04885 -0.00487 -0.00012 0.00278 O4 2 0.421109 0.552090 0.319340 11.00000 0.04698 0.04614 = 0.06797 0.00364 -0.01520 0.00007 O5 2 0.115071 0.344426 0.725274 11.00000 0.03082 0.05365 = 0.06646 -0.01029 0.02271 0.00307 O6 2 0.302485 0.653902 0.525543 11.00000 0.03233 0.03609 = 0.08700 0.00231 -0.00031 -0.00033 O7 2 0.387551 0.446783 0.217386 11.00000 0.03317 0.06870 = 0.03725 -0.01087 -0.02898 0.00325 O8 2 0.391324 0.750000 0.557359 10.50000 0.03754 0.03248 = 0.05416 0.00000 -0.00227 0.00000 O9 2 0.506115 0.650457 0.292544 11.00000 0.04111 0.08898 = 0.06346 -0.00378 -0.00841 -0.01939 O10 2 0.187483 0.250000 0.648930 10.50000 0.06875 0.03586 = 0.06285 0.00000 0.02596 0.00000 O11 2 0.193515 0.659198 0.419698 11.00000 0.05444 0.06755 = 0.06428 -0.00810 -0.00282 -0.00673 O12 2 0.213527 0.750000 0.552038 10.50000 0.03884 0.03087 = 0.04151 0.00000 -0.00625 0.00000 O13 2 0.420484 0.624834 0.598454 11.00000 0.04918 0.04953 = 0.07916 0.01809 -0.00594 0.00230 O14 2 0.190748 0.500856 0.583839 11.00000 0.05131 0.04981 = 0.04823 0.00041 0.01376 0.00623 O15 2 0.299102 0.439737 0.527322 11.00000 0.02470 0.09520 = 0.07306 -0.00680 0.00645 0.00086 O16 2 0.129574 0.443854 0.246765 11.00000 0.03609 0.06731 = 0.06755 -0.00050 -0.01616 -0.00313 O17 2 0.193532 0.439365 0.413588 11.00000 0.04364 0.04866 = 0.05340 0.00949 -0.00617 -0.00236 O18 2 0.077920 0.750000 0.145167 10.50000 0.07525 0.03725 = 0.04443 0.00000 0.00503 0.00000 O19 2 0.401510 0.436403 0.409327 11.00000 0.07295 0.04721 = 0.04344 0.00601 0.00183 -0.01205 O20 2 0.097519 0.633032 0.072346 11.00000 0.06871 0.03839 = 0.05727 -0.00907 0.00532 0.01399 O21 2 0.186704 0.630720 0.611466 11.00000 0.04723 0.05395 = 0.06194 0.01184 0.00433 -0.00554 O22 2 0.194321 0.370903 0.578675 11.00000 0.06090 0.04606 = 0.05198 0.00897 0.00951 -0.00050 O23 2 0.129093 0.658384 0.257702 11.00000 0.02987 0.07423 = 0.05162 0.00493 -0.00518 0.00000 O24 2 0.407896 0.664400 0.412867 11.00000 0.06917 0.07572 = 0.06365 -0.00881 0.00449 0.00435 O25 2 0.089799 0.501511 0.079566 11.00000 0.06120 0.04724 = 0.05265 0.00395 0.00560 -0.00083 O26 2 0.193716 0.549845 0.310767 11.00000 0.09503 0.04485 = 0.07289 0.00444 -0.00473 -0.00472 HKLF 4 REM shelx_a.res in Pnma REM R1 = 0.2178 for 2692 Fo > 4sig(Fo) and 0.2603 for all 4734 data REM 333 parameters refined using 348 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.386, deepest hole -0.199, 1-sigma level 0.057 Q1 1 0.5645 0.7500 0.6787 10.50000 0.05 0.33 Q2 1 0.3087 0.7500 0.8182 10.50000 0.05 0.26 Q3 1 0.4310 0.4567 0.3214 11.00000 0.05 0.24 Q4 1 0.5021 0.6676 0.2950 11.00000 0.05 0.21 Q5 1 0.2009 0.6312 0.6221 11.00000 0.05 0.20 Q6 1 0.1926 0.2500 0.6157 10.50000 0.05 0.20 Q7 1 0.5016 0.5555 0.0336 11.00000 0.05 0.20 Q8 1 0.0760 0.7500 0.1057 10.50000 0.05 0.19 Q9 1 0.5023 0.4348 0.2985 11.00000 0.05 0.19 Q10 1 0.1906 0.5112 0.5605 11.00000 0.05 0.19 Q11 1 0.3057 0.6197 0.5411 11.00000 0.05 0.17 Q12 1 0.1179 0.4416 0.2845 11.00000 0.05 0.17 Q13 1 0.0481 0.3623 0.6787 11.00000 0.05 0.17 Q14 1 0.0693 0.3296 0.4419 11.00000 0.05 0.17 Q15 1 0.0677 0.7099 0.2625 11.00000 0.05 0.16 Q16 1 0.1894 0.7500 0.5618 10.50000 0.05 0.16 Q17 1 0.0516 0.3518 0.3560 11.00000 0.05 0.16 Q18 1 0.3880 0.6326 0.4313 11.00000 0.05 0.16 Q19 1 0.1104 0.3315 0.7112 11.00000 0.05 0.15 Q20 1 0.0988 0.7500 0.3500 10.50000 0.05 0.15 ; _shelx_res_checksum 33783 _shelx_hkl_file ; 0 -3 0 169.53 81.42 0 4 0 2832.67 1350.37 0 -4 0 3095.47 1475.95 0 5 0 153.11 74.49 0 -5 0 48.65 26.97 0 6 0 4338.96 2068.95 0 -6 0 4259.59 2030.14 0 7 0 94.45 49.51 0 -7 0 197.37 95.86 0 9 0 198.25 96.94 0 -9 0 157.87 78.98 0 -10 0 7930.05 3779.83 0 11 0 216.95 104.77 0 -11 0 162.32 79.27 0 12 0 1855.52 884.54 0 -12 0 2086.58 994.61 0 13 0 28.45 18.18 0 -13 0 16.30 14.20 0 14 0 1036.24 494.39 0 -14 0 468.99 224.18 0 15 0 51.84 28.38 0 -15 0 66.09 35.54 0 16 0 6138.03 2926.15 0 17 0 110.79 55.95 0 18 0 1295.86 618.39 0 19 0 11.03 14.43 0 20 0 649.44 310.08 0 21 0 8.95 11.06 0 22 0 65.30 32.79 0 23 0 7.74 10.00 0 24 0 143.81 69.60 -1 4 0 29.77 13.71 1 -4 0 13.66 8.22 1 5 0 189.25 91.42 -1 -5 0 92.30 46.19 -1 6 0 40.44 18.54 -1 -6 0 7.29 13.75 1 -6 0 47.16 21.68 1 7 0 82.90 41.77 -1 -7 0 45.24 25.43 1 8 0 173.45 83.85 -1 8 0 246.05 101.00 -1 8 0 190.67 92.19 -1 -8 0 817.35 389.98 1 -8 0 210.07 101.35 1 9 0 4.67 9.79 -1 9 0 3.78 8.04 -1 9 0 15.63 16.63 1 -9 0 11.79 16.43 -1 10 0 111.79 46.65 -1 10 0 98.51 49.02 -1 -10 0 25.96 16.71 1 -10 0 51.82 29.68 1 11 0 8.58 10.25 -1 -11 0 20.60 15.08 1 -11 0 17.88 15.98 1 12 0 8.45 9.54 -1 12 0 400.91 191.72 -1 -12 0 9.29 11.78 1 -12 0 35.70 20.14 1 13 0 39.33 20.83 -1 13 0 13.64 12.79 -1 13 0 0.50 8.59 -1 -13 0 10.51 11.94 1 14 0 56.67 28.66 -1 14 0 9.85 13.13 -1 14 0 28.59 16.65 -1 -14 0 11.28 12.04 1 15 0 407.97 195.08 -1 15 0 14.16 13.16 -1 -15 0 130.74 63.87 1 16 0 16.09 13.27 -1 16 0 27.06 17.15 -1 16 0 174.21 83.96 -1 -16 0 23.18 16.37 1 -16 0 66.07 32.86 1 17 0 19.53 15.89 -1 17 0 4.95 12.52 -1 17 0 4.29 13.05 1 -17 0 10.55 16.47 1 18 0 87.41 43.62 -1 18 0 17.23 14.63 -1 18 0 58.42 31.43 1 -18 0 118.74 51.82 1 19 0 39.39 21.96 -1 19 0 2.79 10.77 -1 19 0 15.34 13.30 1 -19 0 32.61 19.23 -1 20 0 38.05 20.37 1 -20 0 28.91 18.94 1 21 0 54.13 27.76 -1 21 0 26.25 18.96 -1 21 0 7.38 10.13 1 -21 0 11.32 19.60 1 -21 0 -2.21 9.55 1 22 0 24.99 14.65 -1 22 0 28.45 20.07 -1 22 0 5.84 9.00 1 -22 0 6.85 19.75 1 23 0 3.73 8.12 -1 23 0 12.84 10.82 1 -23 0 3.46 19.07 1 24 0 25.79 14.91 -1 24 0 52.56 27.64 1 -24 0 4.89 12.97 -2 1 0 1065.33 276.03 -2 3 0 117.72 48.70 -2 4 0 661.25 270.03 -2 5 0 1382.29 564.41 -2 7 0 184.14 75.58 -2 8 0 721.93 294.91 2 9 0 60.09 31.91 -2 9 0 78.17 32.95 -2 -9 0 14.99 16.33 2 10 0 713.11 340.42 -2 10 0 621.21 253.81 -2 -10 0 529.32 253.10 2 11 0 5.11 13.01 -2 11 0 68.86 29.38 -2 12 0 198.78 81.70 -2 -12 0 320.48 153.73 -2 13 0 256.63 105.62 -2 -13 0 290.14 139.57 2 14 0 34.06 21.27 -2 14 0 24.43 13.84 -2 14 0 58.22 31.27 -2 -14 0 8.95 14.91 2 15 0 30.90 21.32 -2 15 0 27.25 14.25 -2 15 0 140.67 68.82 -2 -15 0 49.65 27.85 2 16 0 204.95 99.65 -2 16 0 203.72 84.15 -2 16 0 165.55 80.54 -2 -16 0 173.33 84.19 2 17 0 116.98 59.67 -2 17 0 86.43 36.95 -2 17 0 76.67 40.69 2 -17 0 64.78 29.40 2 18 0 166.48 81.36 -2 18 0 81.06 35.12 -2 18 0 47.27 28.66 2 -18 0 53.44 25.66 2 19 0 10.43 14.13 -2 19 0 1.81 8.91 2 -19 0 7.54 11.07 2 20 0 16.94 14.41 -2 20 0 24.39 17.24 2 -21 0 13.30 15.08 2 -22 0 9.30 15.73 -2 23 0 -0.71 8.83 2 -23 0 3.90 13.52 2 24 0 3.87 7.88 -2 24 0 7.35 9.93 2 -24 0 1.40 11.10 -3 0 0 21.31 9.59 3 0 0 25.52 9.73 -3 1 0 33.34 11.23 3 -1 0 19.23 7.93 -3 2 0 45.37 14.54 -3 5 0 40.59 17.96 -3 6 0 7.15 6.42 -3 7 0 427.72 174.81 -3 8 0 68.22 28.61 -3 9 0 9.60 7.14 -3 10 0 15.21 9.40 -3 12 0 4.85 7.49 -3 13 0 103.24 43.18 -3 -13 0 27.22 21.22 3 14 0 5.97 14.74 -3 -14 0 2.25 14.52 3 -14 0 46.35 21.66 3 15 0 28.80 20.16 -3 15 0 14.91 9.76 -3 -15 0 43.83 26.93 3 -15 0 9.56 9.22 3 16 0 48.38 29.26 -3 16 0 7.42 10.04 3 17 0 23.97 23.18 -3 17 0 12.15 10.23 3 -17 0 26.49 14.95 3 18 0 20.72 19.24 -3 18 0 4.65 9.24 -3 -18 0 38.35 25.49 3 -18 0 13.66 11.87 -3 19 0 6.03 8.16 -3 -19 0 7.21 17.23 3 -19 0 1.99 9.18 3 -20 0 4.00 9.76 3 21 0 4.37 13.11 -3 21 0 13.36 12.76 -3 21 0 1.64 11.49 3 -21 0 6.07 11.61 3 22 0 2.94 12.09 -3 22 0 6.34 13.17 -3 22 0 -6.94 12.66 3 -22 0 6.18 14.40 3 23 0 3.79 11.63 -3 23 0 2.94 12.98 3 24 0 8.75 12.64 -3 24 0 1.86 11.62 -4 0 0 2520.47 652.61 4 0 0 2479.90 642.03 -4 2 0 189.78 50.83 4 -2 0 127.74 34.24 -4 8 0 268.98 110.10 4 -8 0 180.26 74.17 -4 9 0 288.20 118.00 -4 10 0 136.31 56.11 -4 12 0 198.25 81.40 -4 13 0 2017.79 824.23 4 -13 0 2254.14 920.18 -4 14 0 24.39 12.39 4 -14 0 15.41 10.85 -4 15 0 410.61 167.95 4 -15 0 586.29 239.70 -4 16 0 254.69 104.61 4 -16 0 226.83 93.62 -4 17 0 16.96 11.13 -4 -17 0 -0.34 19.44 4 -17 0 15.71 11.07 -4 18 0 52.46 23.19 -4 -18 0 7.86 17.17 4 -18 0 82.93 35.33 4 19 0 14.32 20.67 -4 -19 0 1.14 15.84 4 -19 0 18.13 11.51 4 20 0 12.79 18.10 -4 20 0 45.35 21.18 -4 -20 0 -2.26 17.07 4 -20 0 17.40 10.85 4 21 0 25.68 19.35 -4 21 0 76.55 33.53 4 22 0 55.67 29.65 -4 22 0 7.42 12.77 4 -22 0 10.73 11.54 4 23 0 25.22 17.17 4 -23 0 31.52 15.89 4 -24 0 13.04 10.76 -5 0 0 7.58 10.31 5 0 0 3.31 8.93 -5 1 0 8.12 7.89 5 -1 0 5.24 22.84 5 -1 0 10.03 7.43 -5 3 0 12.81 10.73 5 -3 0 11.84 9.28 -5 7 0 64.86 29.56 5 -7 0 5.76 13.92 -5 8 0 14.66 10.00 5 -8 0 16.25 12.77 -5 9 0 76.85 32.35 5 -10 0 10.51 9.49 -5 11 0 198.43 81.51 5 -11 0 60.52 26.39 5 -12 0 14.30 8.97 -5 14 0 75.21 31.71 5 -14 0 17.99 11.48 -5 15 0 26.03 13.11 5 -15 0 115.20 48.05 -5 16 0 16.83 10.81 5 -16 0 27.41 14.57 -5 17 0 13.11 9.66 5 -17 0 29.93 15.40 5 -18 0 25.08 13.63 -5 19 0 6.20 7.91 5 -19 0 3.78 7.54 -5 20 0 12.44 9.70 -5 21 0 37.16 17.83 5 -21 0 13.95 9.96 5 -22 0 -2.59 8.01 5 -23 0 14.24 9.95 -6 0 0 3929.75 1017.19 6 0 0 3860.97 999.37 6 1 0 600.57 279.91 -6 1 0 661.95 171.81 -6 -1 0 436.02 204.07 6 -1 0 674.48 175.02 -6 2 0 189.43 50.22 6 -2 0 175.53 46.39 -6 3 0 3220.70 833.75 6 -3 0 2356.44 610.10 -6 4 0 36.65 14.47 6 -4 0 15.40 10.25 -6 9 0 14.56 10.01 -6 10 0 388.74 159.04 6 -10 0 428.78 175.58 -6 11 0 108.37 45.12 6 -11 0 30.50 14.44 6 -12 0 60.59 26.07 -6 13 0 316.96 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7.98 9 -22 0 13.35 9.66 -10 0 0 7353.29 1903.14 10 0 0 5850.53 1514.23 10 -1 0 168.09 44.50 -10 2 0 561.06 299.32 -10 2 0 963.74 249.94 10 -2 0 1022.13 264.92 -10 3 0 188.55 49.88 10 -3 0 144.20 38.56 10 -4 0 327.19 85.37 -10 5 0 59.95 17.61 10 -5 0 51.77 16.06 -10 6 0 339.54 88.56 10 -6 0 270.74 70.76 -10 7 0 40.96 12.67 10 -7 0 72.23 20.41 -10 14 0 64.57 28.49 -10 15 0 81.58 34.76 10 -15 0 82.19 35.82 -10 16 0 480.28 196.66 10 -16 0 591.93 242.35 10 -17 0 23.95 14.53 -10 18 0 134.95 55.95 -10 19 0 4.22 8.21 10 -19 0 6.68 9.01 10 -20 0 9.49 9.86 10 -21 0 2.31 8.14 -11 0 0 9.70 9.95 11 0 0 18.03 10.31 11 1 0 28.38 24.78 11 -1 0 4.26 6.89 11 2 0 68.77 39.14 -11 2 0 18.31 8.72 -11 -2 0 26.53 25.95 11 -2 0 14.15 7.86 -11 3 0 7.80 7.53 11 -3 0 4.53 7.00 -11 4 0 24.80 9.92 11 -4 0 50.30 15.03 -11 5 0 7.58 7.70 11 -5 0 0.93 5.91 11 -6 0 2.26 6.93 -11 7 0 16.94 8.22 11 -7 0 15.41 8.43 11 -8 0 1.80 6.85 -11 17 0 2.10 9.04 -11 18 0 15.57 10.36 11 -18 0 14.15 12.30 -11 19 0 8.18 8.44 11 -19 0 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5.20 17.53 19 -4 0 32.58 12.34 -19 5 0 7.24 8.37 -19 6 0 3.98 8.67 19 -6 0 0.95 8.19 -19 7 0 7.25 8.97 19 -7 0 6.59 8.22 -19 8 0 13.07 9.29 -19 9 0 4.23 7.86 19 -9 0 0.58 7.59 19 -10 0 1.01 8.67 -19 11 0 -1.20 7.30 -19 12 0 -3.01 8.18 19 -12 0 3.80 9.43 -19 13 0 -3.39 7.12 19 -13 0 -1.05 8.93 19 -14 0 -2.55 8.90 20 1 0 16.37 23.76 -20 1 0 29.30 11.42 20 -1 0 35.03 13.56 -20 2 0 7.71 7.54 20 -2 0 9.93 8.27 20 3 0 74.94 43.34 -20 3 0 21.57 9.78 -20 -3 0 46.93 31.06 20 -3 0 21.71 9.94 -20 4 0 17.90 14.72 -20 4 0 3.82 7.63 -20 -4 0 29.95 25.61 20 -4 0 4.22 7.71 -20 5 0 120.17 32.84 20 -5 0 81.17 23.25 -20 6 0 12.51 8.95 20 -6 0 11.87 8.68 -20 7 0 22.28 10.46 20 -7 0 30.28 11.94 -20 8 0 299.14 78.70 20 -8 0 308.67 81.21 -20 9 0 7.03 8.50 20 -9 0 0.43 6.83 -20 10 0 81.63 24.02 20 -10 0 29.31 12.74 -20 11 0 3.95 8.57 20 -11 0 -2.19 9.35 -20 12 0 14.88 9.60 -21 0 0 -3.50 8.33 21 1 0 102.72 53.87 -21 1 0 3.18 7.03 21 -1 0 13.38 8.96 21 -2 0 7.70 7.78 21 3 0 8.19 21.59 -21 3 0 5.52 7.29 -21 -3 0 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14.47 -3 -8 -15 32.77 15.25 3 8 15 40.87 17.55 3 8 15 13.93 12.02 -3 8 -15 6.95 10.04 -3 9 15 -1.77 7.41 3 -9 15 0.89 8.97 3 -9 15 1.55 4.62 -3 -9 -15 4.16 7.25 3 9 15 0.52 9.03 -3 9 -15 3.54 10.67 3 10 15 1.40 8.95 -4 0 -15 193.66 79.78 -4 0 -15 92.71 45.22 4 -1 15 15.90 10.52 4 -1 15 4.15 7.94 -4 -1 -15 2.07 7.21 4 1 15 5.56 6.98 4 1 15 11.79 10.61 -4 1 -15 6.99 8.71 -4 1 -15 1.99 6.58 4 -2 15 43.05 19.88 4 -2 15 59.53 29.44 -4 -2 -15 19.17 12.05 4 2 15 52.54 22.77 4 2 15 39.40 20.90 -4 2 -15 51.19 22.66 4 -2 -15 77.15 37.34 4 -3 15 6.13 8.07 4 -3 15 12.97 8.98 -4 -3 -15 11.07 9.03 -4 -3 -15 16.11 11.03 4 3 15 4.27 6.40 4 3 15 15.32 11.31 4 -4 15 6.99 8.94 4 -4 15 10.53 7.33 -4 -4 -15 18.40 10.96 -4 -4 -15 1.02 11.69 -4 -4 -15 4.91 8.32 4 4 15 7.73 9.54 -4 4 -15 9.76 8.17 -4 5 15 0.95 11.91 4 -5 15 2.79 5.49 -4 -5 -15 8.57 8.70 -4 -5 -15 8.68 11.13 4 5 15 14.57 8.07 4 5 15 29.86 16.55 -4 5 -15 3.19 8.53 4 -6 15 3.38 5.40 4 6 15 30.14 13.68 4 6 15 10.55 9.49 -4 6 -15 2.26 8.50 4 -7 15 -2.71 9.77 4 -7 15 12.97 8.10 -4 -7 -15 11.01 8.59 4 7 15 38.35 20.62 -4 7 -15 4.98 9.35 4 -8 15 96.07 41.01 4 -8 15 29.42 15.10 -4 -8 -15 70.57 30.21 4 8 15 63.88 26.77 -4 8 -15 53.39 24.43 4 -9 15 -0.32 10.79 5 0 15 90.36 37.85 -5 0 -15 129.02 53.60 5 -1 15 6.19 8.10 -5 -1 -15 33.90 16.67 -5 -1 -15 4.90 7.63 5 1 15 8.37 6.71 5 1 15 4.48 8.29 5 -2 15 35.77 16.53 5 -2 15 4.13 7.36 -5 -2 -15 4.88 8.12 5 2 15 5.85 8.23 -5 2 -15 10.88 9.19 5 -2 -15 26.39 16.59 5 -3 15 3.03 7.22 -5 -3 -15 13.10 9.34 -5 -3 -15 2.40 7.51 5 3 15 6.45 6.62 5 3 15 4.14 8.32 -5 3 -15 9.21 8.75 5 -4 15 4.54 7.86 -5 -4 -15 0.46 11.28 -5 -4 -15 19.63 11.41 -5 -4 -15 1.86 8.22 5 4 15 25.77 12.32 5 4 15 3.86 9.33 -5 4 -15 5.42 8.94 -5 5 15 -1.83 13.60 5 -5 15 87.66 37.50 5 -5 15 3.49 7.76 -5 -5 -15 4.85 8.31 5 5 15 3.10 8.69 -5 5 -15 9.18 9.86 5 -6 15 10.48 10.27 5 -6 15 3.61 7.53 -5 -6 -15 30.07 15.05 5 6 15 15.33 8.54 5 6 15 2.83 8.68 -5 6 -15 17.08 11.36 5 -7 15 0.14 9.89 5 -7 15 4.00 7.36 5 7 15 3.63 5.95 5 7 15 2.83 8.79 5 -8 15 133.95 56.12 -5 -8 -15 194.55 80.25 -5 8 -15 222.59 91.79 5 9 15 2.57 8.21 6 0 15 21.13 10.75 6 0 15 3.15 11.73 -6 0 -15 23.93 13.30 -6 1 15 4.31 10.17 6 -1 15 2.29 9.65 6 1 15 5.70 7.09 6 1 15 0.84 10.48 -6 1 -15 1.20 8.24 6 -2 15 6.50 7.90 6 -2 15 6.47 9.60 6 2 15 84.70 35.42 6 2 15 1.69 11.36 -6 2 -15 10.58 9.95 6 -2 -15 11.59 14.34 6 -3 15 5.30 8.59 -6 -3 -15 1.88 8.98 6 3 15 6.12 11.65 6 3 15 9.59 9.42 -6 3 -15 9.45 9.28 6 -4 15 -2.29 7.90 -6 -4 -15 3.03 8.70 6 4 15 15.52 9.19 6 4 15 5.23 11.10 6 -5 15 13.51 10.25 6 -5 15 7.49 8.43 6 5 15 14.64 8.72 6 5 15 28.41 17.26 -6 5 -15 5.19 8.90 6 -6 15 2.68 7.77 -6 -6 -15 4.45 9.53 6 6 15 5.47 10.00 6 -7 15 2.94 9.89 6 -7 15 1.37 7.82 -6 -7 -15 3.75 9.68 6 7 15 2.93 6.23 6 7 15 4.56 9.37 6 8 15 2.40 8.52 7 0 15 22.65 12.04 7 0 15 -1.65 10.97 -7 1 15 10.02 12.17 7 -1 15 14.10 9.60 7 1 15 14.88 13.15 7 -2 15 8.94 8.35 7 -2 15 -0.43 9.35 7 2 15 6.27 7.58 7 2 15 1.48 11.22 7 -3 15 -0.23 9.25 7 3 15 33.53 15.26 7 3 15 29.56 16.54 7 -4 15 0.44 9.19 -7 -4 -15 11.13 13.88 7 4 15 2.61 7.21 7 4 15 4.10 11.92 7 -5 15 80.13 34.43 7 5 15 82.18 34.38 7 5 15 137.83 67.25 7 -6 15 0.18 9.37 7 6 15 1.67 7.21 7 6 15 -2.68 11.51 8 0 15 3.67 7.52 8 1 15 35.36 16.40 8 1 15 -0.01 11.72 8 -2 15 5.12 8.62 8 2 15 7.40 6.94 8 2 15 6.42 12.41 8 3 15 22.28 11.51 8 3 15 4.50 9.57 8 3 15 11.44 13.06 8 -4 15 8.00 9.13 -8 -4 -15 7.90 13.11 8 4 15 2.87 7.47 8 4 15 -2.04 11.46 8 5 15 7.91 12.74 9 0 15 1.99 8.03 9 -1 15 3.04 9.19 9 -1 -15 11.62 18.64 9 -2 15 -0.43 8.67 9 2 15 0.85 6.98 0 0 16 34.59 17.52 0 1 16 2.19 9.24 0 1 16 12.90 19.24 0 -1 16 1.71 10.91 0 2 16 17.63 11.36 0 2 16 58.84 34.59 0 -2 16 11.00 11.10 0 -2 16 2.84 16.05 0 3 16 0.89 8.15 0 3 16 5.46 20.18 0 -3 16 30.83 20.76 0 -3 -16 2.62 9.78 0 4 16 11.04 8.36 0 4 16 11.82 20.02 0 -4 -16 5.56 9.79 0 5 16 -9.89 17.92 0 -5 16 0.38 9.52 0 -5 -16 -0.05 8.94 0 6 16 6.38 13.95 0 7 16 -2.35 12.94 -1 0 16 14.22 11.66 -1 1 16 -0.36 9.46 1 -1 16 0.01 7.81 1 1 16 3.03 8.55 1 1 16 -0.22 8.70 -1 -1 16 0.39 10.06 -1 2 16 13.65 9.94 -1 2 16 15.61 8.91 1 -2 16 9.44 10.09 -1 -2 -16 3.72 11.13 1 2 16 12.14 10.56 1 2 16 -0.56 9.82 -1 -2 16 10.29 10.45 1 -2 -16 3.24 12.46 1 -3 16 2.91 10.09 -1 -3 -16 19.53 13.70 1 3 16 4.22 8.39 1 3 16 0.27 9.90 -1 -3 16 -0.28 10.40 1 -3 -16 0.26 11.49 -1 4 16 29.37 23.72 1 -4 16 8.41 11.18 1 -4 16 0.65 9.46 1 4 16 0.91 7.19 1 4 16 8.30 10.96 -1 -4 16 5.54 10.27 1 -4 -16 -4.20 10.69 -1 5 16 54.33 23.88 -1 5 16 13.44 20.28 1 -5 16 1.44 12.71 1 -5 16 26.16 15.70 -1 -5 -16 0.96 8.88 1 5 16 3.13 7.04 1 5 16 2.92 9.57 -1 -5 16 -3.32 11.60 1 -5 -16 2.12 9.54 1 6 16 -2.52 9.06 1 7 16 -2.63 8.98 2 0 16 129.84 54.01 2 -1 16 6.28 9.30 2 -1 16 3.17 8.35 2 1 16 6.39 8.49 2 1 16 -0.92 8.53 -2 2 16 13.37 12.21 2 -2 16 11.76 10.14 2 -2 16 6.09 8.15 2 2 16 4.13 9.00 -2 -2 16 -5.57 11.13 2 -2 -16 0.34 13.33 -2 3 16 -0.23 8.06 2 -3 16 3.31 9.53 2 -3 16 6.67 7.77 2 3 16 5.63 8.85 2 3 16 1.78 8.63 -2 -3 16 -2.07 10.14 2 -3 -16 -1.41 11.94 -2 4 16 0.45 7.72 2 -4 16 1.83 10.79 2 -4 16 2.93 6.35 2 4 16 1.83 6.92 2 4 16 6.96 9.43 -2 -4 16 0.16 10.95 2 -4 -16 -2.01 12.11 -2 5 16 7.73 8.63 2 -5 16 32.22 16.63 2 5 16 7.32 9.53 -2 -5 16 0.52 11.58 2 -5 -16 0.50 11.07 2 -6 16 3.54 5.65 2 6 16 1.28 9.43 2 -7 16 0.59 5.57 3 0 16 13.12 9.44 -3 0 16 -1.11 10.25 -3 1 16 -3.20 9.79 3 -1 16 5.86 8.92 3 1 16 4.51 7.86 3 1 16 0.82 9.26 -3 -1 16 -1.65 10.40 -3 2 16 1.44 9.34 3 -2 16 11.13 9.20 3 -2 16 2.83 7.69 3 2 16 11.35 8.96 3 2 16 7.42 10.34 -3 -2 16 -6.68 11.09 -3 3 16 -3.96 9.30 3 -3 16 7.81 10.09 3 -3 16 2.86 6.68 3 3 16 25.58 12.90 3 3 16 13.02 11.76 -3 -3 16 -3.39 11.09 -3 4 16 -1.24 9.32 3 -4 16 3.39 10.57 3 -4 16 0.33 5.67 3 4 16 2.48 9.47 -3 -4 16 -1.47 11.57 3 -5 16 5.54 6.27 3 5 16 13.01 11.50 3 -6 16 2.80 5.56 3 6 16 3.66 9.81 4 0 16 18.96 11.05 4 -1 16 10.97 9.79 4 -1 16 3.59 7.12 4 1 16 1.02 6.86 4 -2 16 1.52 8.65 4 -2 16 11.81 8.63 4 2 16 5.06 7.23 4 2 16 14.43 11.20 4 -3 16 1.36 8.53 4 -3 16 9.82 7.97 4 3 16 54.92 23.99 4 -4 16 2.26 6.00 4 -5 16 22.81 12.70 5 0 16 27.30 14.28 5 0 16 2.98 8.55 5 -1 16 4.48 8.35 5 -1 16 4.07 7.16 5 1 16 6.12 8.07 5 1 16 3.86 7.99 5 -2 16 -0.16 6.76 5 2 16 0.02 7.95 5 3 16 23.81 14.47 5 4 16 1.91 9.21 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 17791 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, 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 Si1 Si 0.4290(2) 0.4730(2) 0.3117(3) 0.0278(12) Uani 1 1 d D U . Si2 Si 0.2252(2) 0.6730(2) 0.5270(4) 0.0362(13) Uani 1 1 d D U . Si3 Si 0.0781(2) 0.6723(2) 0.1696(4) 0.0327(13) Uani 1 1 d D U . Si4 Si 0.0777(2) 0.4441(2) 0.1588(4) 0.0340(13) Uani 1 1 d D U . Si5 Si 0.4305(2) 0.6298(2) 0.3139(4) 0.0345(13) Uani 1 1 d D U . Si6 Si 0.3800(2) 0.6735(2) 0.5258(4) 0.0362(13) Uani 1 1 d D U . Si7 Si 0.2201(3) 0.4377(2) 0.5271(4) 0.0351(13) Uani 1 1 d D U . Si8 Si 0.1827(3) 0.5595(3) 0.6636(4) 0.0376(14) Uani 1 1 d D U . Si9 Si 0.1848(2) 0.3276(3) 0.6744(4) 0.0362(13) Uani 1 1 d D U . Si10 Si 0.1949(2) 0.4714(3) 0.3044(4) 0.0363(13) Uani 1 1 d D U . Si11 Si 0.1221(3) 0.5641(2) 0.0237(4) 0.0358(13) Uani 1 1 d D U . Si12 Si 0.1942(2) 0.6284(3) 0.3114(4) 0.0358(13) Uani 1 1 d D U . O1 O 0.5053(4) 0.4504(4) 0.2926(7) 0.046(2) Uani 1 1 d D U . O2 O 0.2590(4) 0.6530(5) 0.2523(8) 0.066(3) Uani 1 1 d D U . O3 O 0.2599(5) 0.4460(5) 0.2459(7) 0.061(3) Uani 1 1 d D U . O4 O 0.4211(5) 0.5521(4) 0.3193(8) 0.054(2) Uani 1 1 d D U . O5 O 0.1151(4) 0.3444(4) 0.7253(7) 0.050(2) Uani 1 1 d D U . O6 O 0.3025(3) 0.6539(4) 0.5255(8) 0.052(2) Uani 1 1 d D U . O7 O 0.3876(4) 0.4468(4) 0.2174(6) 0.046(2) Uani 1 1 d D U . O8 O 0.3913(6) 0.7500 0.5574(9) 0.041(2) Uani 1 2 d DS TU P O9 O 0.5061(4) 0.6505(6) 0.2925(8) 0.065(3) Uani 1 1 d D U . O10 O 0.1875(7) 0.2500 0.6489(11) 0.056(3) Uani 1 2 d DS TU P O11 O 0.1935(4) 0.6592(6) 0.4197(7) 0.062(2) Uani 1 1 d D U . O12 O 0.2135(6) 0.7500 0.5520(8) 0.037(2) Uani 1 2 d DS TU P O13 O 0.4205(5) 0.6248(4) 0.5985(8) 0.059(2) Uani 1 1 d D U . O14 O 0.1907(4) 0.5009(4) 0.5838(7) 0.050(2) Uani 1 1 d D U . O15 O 0.2991(4) 0.4397(6) 0.5273(10) 0.064(3) Uani 1 1 d D U . O16 O 0.1296(4) 0.4439(4) 0.2468(8) 0.057(2) Uani 1 1 d D U . O17 O 0.1935(4) 0.4394(4) 0.4136(7) 0.049(2) Uani 1 1 d D U . O18 O 0.0779(7) 0.7500 0.1452(9) 0.052(3) Uani 1 2 d DS TU P O19 O 0.4015(5) 0.4364(4) 0.4093(6) 0.055(2) Uani 1 1 d D U . O20 O 0.0975(5) 0.6330(4) 0.0723(7) 0.055(2) Uani 1 1 d D U . O21 O 0.1867(4) 0.6307(4) 0.6115(8) 0.054(2) Uani 1 1 d D U . O22 O 0.1943(5) 0.3709(4) 0.5787(7) 0.053(2) Uani 1 1 d D U . O23 O 0.1291(4) 0.6584(5) 0.2577(7) 0.052(2) Uani 1 1 d D U . O24 O 0.4079(5) 0.6644(5) 0.4129(7) 0.070(3) Uani 1 1 d D U . O25 O 0.0898(5) 0.5015(4) 0.0796(6) 0.054(2) Uani 1 1 d D U . O26 O 0.1937(6) 0.5498(4) 0.3108(10) 0.071(3) Uani 1 1 d 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 Si1 0.023(2) 0.033(2) 0.027(2) 0.0024(17) -0.008(2) 0.0036(19) Si2 0.027(3) 0.026(2) 0.055(3) 0.0016(19) 0.004(2) 0.000(2) Si3 0.017(2) 0.038(3) 0.043(3) -0.0068(19) 0.002(2) -0.001(2) Si4 0.020(2) 0.042(3) 0.041(3) -0.0074(19) 0.006(2) 0.0034(19) Si5 0.023(2) 0.036(3) 0.044(3) -0.0008(19) -0.013(2) 0.000(2) Si6 0.032(3) 0.022(2) 0.055(3) 0.0026(19) 0.000(2) -0.0019(19) Si7 0.025(3) 0.037(3) 0.044(3) 0.0025(19) 0.004(2) 0.002(2) Si8 0.030(3) 0.043(3) 0.040(3) 0.003(2) 0.010(2) 0.001(2) Si9 0.028(3) 0.037(3) 0.044(3) -0.002(2) 0.010(2) -0.008(2) Si10 0.025(3) 0.033(3) 0.051(3) 0.004(2) -0.006(2) -0.0032(19) Si11 0.035(3) 0.027(2) 0.045(3) -0.0079(19) 0.002(3) 0.001(2) Si12 0.028(3) 0.034(3) 0.045(3) -0.001(2) -0.001(2) -0.0009(19) O1 0.036(4) 0.042(4) 0.061(5) 0.013(3) -0.002(4) 0.006(3) O2 0.038(4) 0.081(6) 0.079(6) 0.024(5) 0.003(4) -0.005(4) O3 0.045(4) 0.090(7) 0.049(5) -0.005(4) 0.000(4) 0.003(4) O4 0.047(5) 0.046(4) 0.068(6) 0.004(3) -0.015(4) 0.000(3) O5 0.031(4) 0.054(5) 0.066(5) -0.010(4) 0.023(4) 0.003(3) O6 0.032(3) 0.036(4) 0.087(6) 0.002(4) 0.000(3) 0.000(3) O7 0.033(4) 0.069(5) 0.037(4) -0.011(3) -0.029(4) 0.003(3) O8 0.038(5) 0.032(4) 0.054(6) 0.000 -0.002(5) 0.000 O9 0.041(4) 0.089(7) 0.063(6) -0.004(5) -0.008(4) -0.019(4) O10 0.069(8) 0.036(5) 0.063(8) 0.000 0.026(7) 0.000 O11 0.054(5) 0.068(6) 0.064(4) -0.008(4) -0.003(3) -0.007(4) O12 0.039(5) 0.031(4) 0.042(5) 0.000 -0.006(5) 0.000 O13 0.049(5) 0.050(5) 0.079(6) 0.018(4) -0.006(5) 0.002(4) O14 0.051(5) 0.050(4) 0.048(4) 0.000(3) 0.014(4) 0.006(3) O15 0.025(4) 0.095(8) 0.073(7) -0.007(5) 0.006(4) 0.001(3) O16 0.036(4) 0.067(6) 0.068(5) -0.001(4) -0.016(4) -0.003(3) O17 0.044(5) 0.049(5) 0.053(4) 0.009(3) -0.006(3) -0.002(3) O18 0.075(8) 0.037(5) 0.044(6) 0.000 0.005(6) 0.000 O19 0.073(6) 0.047(5) 0.043(4) 0.006(3) 0.002(4) -0.012(4) O20 0.069(6) 0.038(4) 0.057(5) -0.009(3) 0.005(4) 0.014(4) O21 0.047(5) 0.054(5) 0.062(5) 0.012(4) 0.004(4) -0.006(3) O22 0.061(5) 0.046(4) 0.052(4) 0.009(3) 0.010(4) -0.001(3) O23 0.030(3) 0.074(5) 0.052(4) 0.005(4) -0.005(3) 0.000(3) O24 0.069(6) 0.076(6) 0.064(4) -0.009(4) 0.004(4) 0.004(5) O25 0.061(5) 0.047(4) 0.053(4) 0.004(3) 0.006(4) -0.001(4) O26 0.095(8) 0.045(4) 0.073(7) 0.004(3) -0.005(5) -0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0000 0.0000 'International Tables Vol C Tables 4.3.2.2 and 4.3.2.3' O O 0.0000 0.0000 'International Tables Vol C Tables 4.3.2.2 and 4.3.2.3' 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 O1 Si1 O7 105.1(5) . . O1 Si1 O19 108.6(6) . . O7 Si1 O19 109.0(6) . . O1 Si1 O4 112.7(5) . . O7 Si1 O4 109.3(5) . . O19 Si1 O4 111.9(6) . . O6 Si2 O11 109.1(6) . . O6 Si2 O12 112.2(6) . . O11 Si2 O12 107.5(6) . . O6 Si2 O21 109.7(6) . . O11 Si2 O21 111.1(6) . . O12 Si2 O21 107.2(6) . . O9 Si3 O20 110.3(6) 6_556 . O9 Si3 O23 106.5(6) 6_556 . O20 Si3 O23 112.2(6) . . O9 Si3 O18 109.8(7) 6_556 . O20 Si3 O18 108.8(6) . . O23 Si3 O18 109.2(7) . . O16 Si4 O1 106.3(6) . 6_556 O16 Si4 O25 114.2(6) . . O1 Si4 O25 110.8(5) 6_556 . O16 Si4 O13 111.4(6) . 2_564 O1 Si4 O13 107.4(5) 6_556 2_564 O25 Si4 O13 106.7(6) . 2_564 O24 Si5 O9 107.9(6) . . O24 Si5 O5 109.3(6) . 2_564 O9 Si5 O5 108.3(6) . 2_564 O24 Si5 O4 111.7(6) . . O9 Si5 O4 112.5(6) . . O5 Si5 O4 107.1(5) 2_564 . O6 Si6 O13 109.3(5) . . O6 Si6 O8 112.0(6) . . O13 Si6 O8 111.0(6) . . O6 Si6 O24 107.3(6) . . O13 Si6 O24 109.4(6) . . O8 Si6 O24 107.9(6) . . O15 Si7 O14 110.0(6) . . O15 Si7 O22 109.8(6) . . O14 Si7 O22 110.5(6) . . O15 Si7 O17 109.0(6) . . O14 Si7 O17 108.6(5) . . O22 Si7 O17 108.9(5) . . O7 Si8 O3 107.7(6) 2_565 2_565 O7 Si8 O21 108.6(5) 2_565 . O3 Si8 O21 109.4(6) 2_565 . O7 Si8 O14 109.6(5) 2_565 . O3 Si8 O14 110.1(6) 2_565 . O21 Si8 O14 111.4(6) . . O22 Si9 O5 110.0(6) . . O22 Si9 O2 108.9(6) . 2_565 O5 Si9 O2 105.9(6) . 2_565 O22 Si9 O10 111.4(7) . . O5 Si9 O10 109.4(6) . . O2 Si9 O10 111.1(7) 2_565 . O26 Si10 O3 111.1(6) . . O26 Si10 O16 111.2(6) . . O3 Si10 O16 107.3(6) . . O26 Si10 O17 110.7(7) . . O3 Si10 O17 109.6(6) . . O16 Si10 O17 106.8(5) . . O15 Si11 O25 110.1(6) 2_564 . O15 Si11 O19 108.7(7) 2_564 2_564 O25 Si11 O19 109.1(5) . 2_564 O15 Si11 O20 109.3(6) 2_564 . O25 Si11 O20 111.7(6) . . O19 Si11 O20 107.8(5) 2_564 . O2 Si12 O11 110.1(6) . . O2 Si12 O26 108.4(7) . . O11 Si12 O26 113.4(7) . . O2 Si12 O23 107.8(6) . . O11 Si12 O23 105.1(6) . . O26 Si12 O23 111.9(6) . . Si4 O1 Si1 144.4(7) 6_656 . Si9 O2 Si12 168.3(8) 2_564 . Si8 O3 Si10 160.6(8) 2_564 . Si5 O4 Si1 166.2(8) . . Si9 O5 Si5 153.6(7) . 2_565 Si2 O6 Si6 151.3(7) . . Si8 O7 Si1 147.6(7) 2_564 . Si6 O8 Si6 145.5(9) . 7_575 Si3 O9 Si5 150.6(8) 6_656 . Si9 O10 Si9 155.0(11) . 7_565 Si12 O11 Si2 153.6(7) . . Si2 O12 Si2 150.6(9) 7_575 . Si6 O13 Si4 148.2(7) . 2_565 Si7 O14 Si8 161.0(7) . . Si11 O15 Si7 175.2(9) 2_565 . Si4 O16 Si10 152.9(7) . . Si10 O17 Si7 150.2(6) . . Si3 O18 Si3 156.3(9) 7_575 . Si1 O19 Si11 152.4(6) . 2_565 Si3 O20 Si11 147.6(7) . . Si8 O21 Si2 143.8(7) . . Si9 O22 Si7 149.8(8) . . Si3 O23 Si12 157.1(7) . . Si5 O24 Si6 160.0(8) . . Si4 O25 Si11 161.3(7) . . Si12 O26 Si10 177.0(10) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 O1 1.615(8) . Si1 O7 1.618(8) . Si1 O19 1.621(8) . Si1 O4 1.627(8) . Si2 O6 1.592(8) . Si2 O11 1.616(10) . Si2 O12 1.627(5) . Si2 O21 1.631(9) . Si3 O9 1.591(8) 6_556 Si3 O20 1.596(8) . Si3 O23 1.600(8) . Si3 O18 1.622(5) . Si4 O16 1.583(9) . Si4 O1 1.596(9) 6_556 Si4 O25 1.612(9) . Si4 O13 1.630(8) 2_564 Si5 O24 1.587(10) . Si5 O9 1.595(9) . Si5 O5 1.601(8) 2_564 Si5 O4 1.600(8) . Si6 O6 1.600(8) . Si6 O13 1.619(9) . Si6 O8 1.636(5) . Si6 O24 1.646(10) . Si7 O15 1.579(8) . Si7 O14 1.613(9) . Si7 O22 1.619(9) . Si7 O17 1.633(10) . Si8 O7 1.588(8) 2_565 Si8 O3 1.606(10) 2_565 Si8 O21 1.621(9) . Si8 O14 1.625(9) . Si9 O22 1.586(9) . Si9 O5 1.592(8) . Si9 O2 1.594(9) 2_565 Si9 O10 1.625(6) . Si10 O26 1.605(9) . Si10 O3 1.611(9) . Si10 O16 1.623(8) . Si10 O17 1.624(9) . Si11 O15 1.576(8) 2_564 Si11 O25 1.622(9) . Si11 O19 1.626(9) 2_564 Si11 O20 1.632(8) . Si12 O2 1.605(9) . Si12 O11 1.603(10) . Si12 O26 1.605(9) . Si12 O23 1.613(8) . O1 Si4 1.596(9) 6_656 O2 Si9 1.594(9) 2_564 O3 Si8 1.606(10) 2_564 O5 Si5 1.601(8) 2_565 O7 Si8 1.588(8) 2_564 O8 Si6 1.636(5) 7_575 O9 Si3 1.591(8) 6_656 O10 Si9 1.625(6) 7_565 O12 Si2 1.627(5) 7_575 O13 Si4 1.630(8) 2_565 O15 Si11 1.576(8) 2_565 O18 Si3 1.622(5) 7_575 O19 Si11 1.626(9) 2_565