#------------------------------------------------------------------------------ #$Date: 2019-07-12 07:21:08 +0300 (Fri, 12 Jul 2019) $ #$Revision: 216970 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552088.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_1552088 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_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 20.580 _cell_length_b 19.600 _cell_length_c 13.740 _cell_measurement_reflns_used 5407 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 1.80 _cell_measurement_theta_min 0.072 _cell_volume 5542.276 _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 0.992 _diffrn_measured_fraction_theta_max 0.962 _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 0.3516 _diffrn_reflns_av_unetI/netI 0.3313 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.962 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 37050 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.962 _diffrn_reflns_theta_full 0.863 _diffrn_reflns_theta_max 0.887 _diffrn_reflns_theta_min 0.063 _diffrn_source 'electron microscope' _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_density_diffrn 1.728 _exptl_crystal_description cuboid _exptl_crystal_F_000 939 _refine_diff_density_max 0.232 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef 1225(23) _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 1.597 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 5407 _refine_ls_number_restraints 348 _refine_ls_restrained_S_all 1.586 _refine_ls_R_factor_all 0.3058 _refine_ls_R_factor_gt 0.2385 _refine_ls_shift/su_max 0.133 _refine_ls_shift/su_mean 0.006 _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 0.5479 _refine_ls_wR_factor_ref 0.5875 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3425 _reflns_number_total 5407 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file fc5033.cif _cod_data_source_block zsm5_cluster10 _cod_original_cell_volume 5542.3 _cod_database_code 1552088 _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_a11_UCtoLit.res created by SHELXL-2014/7 TITL shelx_a.res in Pnma REM Old TITL 16 REM SHELXT solution in Pnma REM R1 0.625, Rweak 0.163, Alpha 0.184, Orientation a'=c, b'=-b, c'=a REM Formula found by SHELXT: Si O2 CELL 0.02510 20.5800 19.6000 13.7400 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 ACTA FMAP 2 PLAN 20 WGHT 0.200000 EXTI 1224.682861 FVAR 1.10682 1.61010 SI1 1 0.428576 0.470921 0.311677 11.00000 0.02294 0.04715 = 0.03660 -0.00163 -0.01533 0.00093 SI2 1 0.224795 0.673169 0.526630 11.00000 0.02410 0.04879 = 0.03674 0.00307 0.00278 -0.00076 SI3 1 0.078023 0.670695 0.169544 11.00000 0.02001 0.06109 = 0.04213 0.00238 0.00187 -0.00575 SI4 1 0.078612 0.443700 0.160320 11.00000 0.02018 0.04029 = 0.04154 -0.00514 0.00530 0.00312 SI5 1 0.431072 0.631128 0.314043 11.00000 0.01892 0.05740 = 0.04167 -0.00645 -0.00168 0.00263 SI6 1 0.379494 0.673257 0.524900 11.00000 0.02008 0.05341 = 0.04325 -0.00115 -0.00040 0.00274 SI7 1 0.220145 0.437834 0.527158 11.00000 0.02507 0.04198 = 0.04432 -0.00524 0.00290 0.00158 SI8 1 0.183956 0.557772 0.666034 11.00000 0.02734 0.04721 = 0.03830 0.00003 0.01792 -0.00029 SI9 1 0.185136 0.327552 0.677309 11.00000 0.02527 0.05116 = 0.04707 0.00305 0.00220 0.00208 SI10 1 0.194419 0.469817 0.304105 11.00000 0.02757 0.06345 = 0.04074 -0.00361 -0.00254 0.00427 SI11 1 0.122886 0.564042 0.023881 11.00000 0.01982 0.06002 = 0.04459 0.00128 0.00153 0.00053 SI12 1 0.193729 0.631062 0.310401 11.00000 0.02729 0.07016 = 0.04073 -0.00505 -0.01013 -0.00211 O1 2 0.505821 0.451920 0.296282 11.00000 0.03704 0.08050 = 0.04052 0.00274 -0.01158 0.01137 O2 2 0.258741 0.654297 0.253771 11.00000 0.04661 0.09578 = 0.06188 0.00213 0.00169 -0.00883 O3 2 0.259373 0.445491 0.246739 11.00000 0.04134 0.08871 = 0.06871 -0.00827 0.00371 0.00295 O4 2 0.421729 0.551454 0.326574 11.00000 0.05537 0.06187 = 0.07937 -0.00299 -0.00126 0.00377 O5 2 0.114695 0.345868 0.723189 11.00000 0.02610 0.07711 = 0.06987 -0.01296 0.00851 0.00372 O6 2 0.301661 0.656602 0.527610 11.00000 0.02762 0.06523 = 0.08553 0.00404 0.00079 0.00694 O7 2 0.386782 0.445499 0.219088 11.00000 0.03484 0.07233 = 0.03806 -0.00397 -0.01447 0.00100 O8 2 0.389271 0.750000 0.559290 10.50000 0.05186 0.05624 = 0.07820 0.00000 0.00277 0.00000 O9 2 0.505370 0.649217 0.294160 11.00000 0.03604 0.09095 = 0.03535 -0.00012 -0.00869 -0.01086 O10 2 0.186762 0.250000 0.645515 10.50000 0.08978 0.06143 = 0.04913 0.00000 0.04088 0.00000 O11 2 0.191978 0.658491 0.422245 11.00000 0.05703 0.06973 = 0.04636 -0.00437 -0.00403 -0.00736 O12 2 0.213154 0.750000 0.554521 10.50000 0.03687 0.05277 = 0.05897 0.00000 0.02429 0.00000 O13 2 0.419426 0.626172 0.598775 11.00000 0.04024 0.07188 = 0.05313 0.00403 -0.00949 0.00375 O14 2 0.189818 0.499237 0.584704 11.00000 0.06938 0.05727 = 0.05489 -0.00385 0.01069 0.01125 O15 2 0.298072 0.440132 0.528127 11.00000 0.03169 0.08656 = 0.08572 -0.00051 0.00404 0.00062 O16 2 0.129940 0.445073 0.247339 11.00000 0.04100 0.11023 = 0.06183 0.00268 -0.01790 -0.00884 O17 2 0.194168 0.440634 0.413542 11.00000 0.05314 0.07892 = 0.04941 0.00227 -0.00482 -0.00822 O18 2 0.076757 0.750000 0.140246 10.50000 0.11904 0.06415 = 0.04915 0.00000 0.00487 0.00000 O19 2 0.400381 0.436537 0.411185 11.00000 0.06569 0.05426 = 0.04150 -0.00146 0.00113 -0.00241 O20 2 0.098428 0.633913 0.068440 11.00000 0.06539 0.06584 = 0.05973 -0.00345 0.00367 0.00571 O21 2 0.187426 0.630908 0.611860 11.00000 0.05250 0.04563 = 0.04065 -0.00681 0.02540 -0.00024 O22 2 0.193115 0.368230 0.576026 11.00000 0.06226 0.05553 = 0.05472 0.00163 0.01289 -0.00130 O23 2 0.128955 0.656494 0.258375 11.00000 0.04053 0.09787 = 0.05462 0.00823 -0.00364 -0.00505 O24 2 0.409251 0.662239 0.416362 11.00000 0.06159 0.08867 = 0.06919 -0.02039 0.01767 -0.00724 O25 2 0.088285 0.502725 0.081593 11.00000 0.05979 0.06729 = 0.06631 0.01794 -0.00169 -0.00702 O26 2 0.194217 0.549696 0.309924 11.00000 0.09445 0.07490 = 0.08958 -0.00424 -0.00342 -0.00168 HKLF 4 REM shelx_a.res in Pnma REM R1 = 0.2385 for 3425 Fo > 4sig(Fo) and 0.3058 for all 5407 data REM 333 parameters refined using 348 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.232, deepest hole -0.332, 1-sigma level 0.077 Q1 1 0.1079 0.7500 0.1791 10.50000 0.05 0.23 Q2 1 0.3071 0.7500 0.3571 10.50000 0.05 0.23 Q3 1 0.1907 0.5505 0.2352 11.00000 0.05 0.23 Q4 1 0.2281 0.6233 0.5505 11.00000 0.05 0.22 Q5 1 0.1789 0.6825 0.1472 11.00000 0.05 0.21 Q6 1 0.1103 0.2878 0.4441 11.00000 0.05 0.21 Q7 1 0.4310 0.4246 0.3145 11.00000 0.05 0.21 Q8 1 0.3124 0.3602 0.3324 11.00000 0.05 0.21 Q9 1 0.0789 0.3493 0.3268 11.00000 0.05 0.20 Q10 1 0.1680 0.6952 0.1537 11.00000 0.05 0.20 Q11 1 0.0774 0.4874 0.5552 11.00000 0.05 0.20 Q12 1 0.5135 0.7500 0.1745 10.50000 0.05 0.20 Q13 1 0.0492 0.7153 0.3759 11.00000 0.05 0.20 Q14 1 0.0937 0.5623 0.0503 11.00000 0.05 0.20 Q15 1 0.2240 0.4849 0.5140 11.00000 0.05 0.20 Q16 1 0.0427 0.7500 0.3991 10.50000 0.05 0.20 Q17 1 0.3383 0.4312 0.6631 11.00000 0.05 0.19 Q18 1 0.1698 0.6771 0.5351 11.00000 0.05 0.19 Q19 1 0.1199 0.2500 0.4817 10.50000 0.05 0.19 Q20 1 0.1606 0.4395 0.5584 11.00000 0.05 0.19 ; _shelx_res_checksum 83523 _shelx_hkl_file ; 2 0 0 2007.45 1010.22 3 0 0 60.96 23.64 3 0 0 74.60 39.04 -3 0 0 64.71 33.98 4 0 0 2115.79 1064.77 4 0 0 1770.37 622.88 4 0 0 1170.94 608.10 5 0 0 19.86 13.36 5 0 0 38.22 19.25 -5 0 0 14.30 9.28 6 0 0 3048.77 1534.58 6 0 0 2512.18 884.04 -6 0 0 2818.07 1418.60 -6 0 0 1733.42 900.23 7 0 0 15.52 12.92 7 0 0 86.94 43.77 7 0 0 20.34 13.84 -7 0 0 69.97 35.23 -7 0 0 34.90 19.87 8 0 0 5132.69 2583.55 8 0 0 3940.97 1386.73 -8 0 0 4045.48 2035.49 9 0 0 117.82 59.31 9 0 0 49.70 21.04 9 0 0 55.81 30.60 -9 0 0 77.67 39.10 10 0 0 3752.33 1319.18 10 0 0 4471.19 2250.89 10 0 0 2932.79 1523.11 -10 0 0 4190.79 2109.41 -10 0 0 2993.96 1554.98 11 0 0 24.15 12.51 11 0 0 41.30 20.80 11 0 0 34.41 18.95 -11 0 0 25.84 13.01 -11 0 0 78.76 41.47 12 0 0 454.76 160.72 12 0 0 620.84 312.53 12 0 0 510.85 265.49 -12 0 0 724.98 364.91 -12 0 0 531.75 276.32 13 0 0 0.79 7.18 13 0 0 3.62 1.88 13 0 0 1.19 4.41 -13 0 0 4.33 2.22 -13 0 0 2.69 5.19 14 0 0 223.31 79.48 14 0 0 385.17 193.86 14 0 0 206.10 107.23 -14 0 0 426.86 214.89 -14 0 0 227.39 118.29 15 0 0 11.60 9.49 15 0 0 46.74 23.53 15 0 0 94.06 49.44 -15 0 0 61.55 30.98 -15 0 0 32.90 18.25 16 0 0 3478.31 1223.46 16 0 0 4738.85 2384.72 16 0 0 2802.78 1455.56 -16 0 0 4309.32 2169.32 -16 0 0 2860.14 1484.87 17 0 0 17.44 11.68 17 0 0 62.28 31.35 17 0 0 13.24 9.98 -17 0 0 33.22 16.72 -17 0 0 25.95 15.01 18 0 0 419.84 148.87 18 0 0 393.08 197.81 18 0 0 300.80 156.64 -18 0 0 445.59 224.33 -18 0 0 329.86 171.55 19 0 0 3.84 1.99 19 0 0 2.26 8.26 -19 0 0 2.48 1.32 -19 0 0 2.09 4.91 20 0 0 561.44 282.57 20 0 0 598.15 211.58 -20 0 0 538.76 271.23 -20 0 0 659.46 342.61 21 0 0 0.64 0.50 21 0 0 1.58 8.08 -21 0 0 3.27 1.68 -21 0 0 2.59 3.95 22 0 0 22.88 11.73 22 0 0 26.55 13.37 -22 0 0 37.17 18.71 -22 0 0 13.13 7.74 -22 0 0 22.36 13.13 23 0 0 -0.65 9.07 23 0 0 1.20 0.69 -23 0 0 -1.67 9.99 -23 0 0 -1.44 3.68 24 0 0 20.65 13.13 -24 0 0 19.00 13.96 -24 0 0 5.72 5.62 -25 0 0 0.79 6.49 2 1 0 301.44 177.29 -2 1 0 413.98 230.19 -2 -1 0 392.44 230.70 3 1 0 11.02 6.47 -3 -1 0 7.15 4.62 4 -1 0 642.39 240.77 4 -1 0 731.61 258.10 4 1 0 548.45 284.74 4 1 0 633.97 223.56 -4 1 0 570.88 214.00 -4 1 0 603.13 212.85 -4 -1 0 622.76 219.61 5 -1 0 31.06 18.76 5 1 0 66.43 34.82 6 -1 0 1213.52 427.49 6 1 0 772.51 272.25 -6 1 0 1224.74 431.32 -6 -1 0 747.92 263.58 7 -1 0 50.83 20.60 7 1 0 30.39 20.75 7 1 0 42.79 17.81 -7 1 0 44.33 18.20 -7 -1 0 61.01 23.46 8 -1 0 56.46 22.08 8 1 0 17.55 9.79 -8 1 0 47.21 19.26 -8 -1 0 28.13 12.41 9 -1 0 1.66 8.48 9 -1 0 18.11 11.07 -9 1 0 5.26 6.45 -9 1 0 1.00 8.84 -9 -1 0 1.24 6.83 10 -1 0 133.45 48.10 10 -1 0 73.77 38.76 10 1 0 150.28 53.80 -10 1 0 121.32 63.60 -11 1 0 38.08 20.79 12 1 0 53.07 20.57 -12 1 0 31.39 14.28 -12 -1 0 87.26 32.17 13 -1 0 20.72 11.94 13 1 0 22.24 10.65 -13 1 0 11.44 8.43 -13 -1 0 5.36 6.81 14 -1 0 55.38 21.46 14 -1 0 125.94 65.67 14 1 0 86.35 31.65 -14 1 0 69.39 26.14 -14 1 0 94.89 49.77 -14 -1 0 96.47 35.18 15 -1 0 3.29 6.55 15 -1 0 26.78 14.71 15 1 0 1.49 6.82 -15 1 0 -0.35 7.49 -15 1 0 22.09 12.92 -15 -1 0 5.60 7.34 16 -1 0 41.60 17.33 16 1 0 46.16 19.08 -16 1 0 59.54 23.54 -16 1 0 62.16 33.28 -16 -1 0 63.77 24.60 17 -1 0 1.31 8.37 17 -1 0 35.82 19.55 17 1 0 5.92 8.39 -17 1 0 2.57 8.53 -17 1 0 6.80 7.52 -17 -1 0 6.95 8.66 -17 -1 0 3.27 5.45 18 -1 0 32.28 14.89 18 -1 0 33.99 18.42 18 1 0 37.36 16.19 -18 1 0 42.20 18.44 -18 1 0 30.60 17.09 -18 -1 0 27.91 13.48 -18 -1 0 50.51 26.93 19 -1 0 2.00 8.12 19 -1 0 3.59 4.40 19 1 0 -1.44 8.05 -19 1 0 0.41 8.28 -19 1 0 1.76 5.17 -19 -1 0 -0.64 7.59 -19 -1 0 3.97 5.84 20 -1 0 7.59 8.31 20 -1 0 6.07 4.97 20 1 0 4.43 8.06 -20 1 0 7.26 9.24 -20 1 0 10.33 7.21 -20 -1 0 11.15 9.09 -20 -1 0 19.49 11.07 21 -1 0 1.23 7.81 21 -1 0 28.67 15.41 21 1 0 8.82 8.41 -21 1 0 1.01 8.26 -21 1 0 2.56 4.21 -21 -1 0 6.33 8.07 22 -1 0 3.28 7.42 22 -1 0 4.45 3.93 22 1 0 6.35 8.57 -22 1 0 3.50 8.62 -22 1 0 2.36 3.72 -22 -1 0 9.54 9.00 23 -1 0 1.80 8.25 23 -1 0 2.44 3.71 23 1 0 5.96 8.77 -23 1 0 1.92 9.18 -23 1 0 5.50 4.81 -23 -1 0 6.63 9.45 -23 -1 0 21.94 12.43 24 -1 0 29.12 14.62 24 -1 0 27.45 15.01 24 1 0 29.14 14.48 -24 1 0 32.36 17.58 -24 1 0 26.65 15.98 -24 -1 0 35.28 17.10 -24 -1 0 33.32 17.79 25 -1 0 1.21 5.36 -25 -1 0 -0.08 3.15 1 -2 0 316.35 175.89 -1 2 0 371.41 206.48 2 -2 0 68.07 29.80 2 2 0 153.96 80.23 3 2 0 31.86 16.95 3 2 0 11.67 10.07 -3 2 0 38.21 19.09 -3 2 0 27.58 16.14 -3 -2 0 14.40 11.13 -3 -2 0 37.38 19.69 4 -2 0 101.84 39.98 4 2 0 134.73 70.02 4 2 0 294.81 173.47 -4 2 0 110.76 41.40 -4 2 0 115.82 64.70 -4 -2 0 220.63 130.01 5 2 0 51.26 26.88 -5 2 0 42.80 24.55 -5 2 0 21.09 14.42 -5 2 0 12.50 9.65 -5 -2 0 66.12 34.53 6 2 0 37.82 20.11 6 2 0 182.01 65.39 -6 -2 0 44.09 23.22 -6 -2 0 239.37 85.15 7 -2 0 20.80 10.66 7 2 0 53.62 28.24 7 2 0 66.32 25.56 7 2 0 62.96 37.97 -7 2 0 123.10 45.32 -7 2 0 0.87 7.59 -7 -2 0 58.02 35.18 -7 -2 0 46.75 24.78 8 -2 0 1631.45 611.41 8 -2 0 1932.25 680.36 8 2 0 1239.27 643.28 8 2 0 1187.51 417.93 8 2 0 2465.02 1447.91 -8 2 0 2004.90 750.98 -8 2 0 1600.86 563.61 -8 -2 0 1373.98 483.57 9 -2 0 15.37 9.85 9 -2 0 2.61 13.82 9 2 0 57.32 30.22 9 2 0 9.48 7.49 -9 2 0 9.96 8.48 -9 2 0 0.56 11.82 -9 -2 0 58.85 31.01 -9 -2 0 10.58 7.88 10 2 0 729.31 378.67 -10 -2 0 600.19 311.63 11 2 0 12.18 7.92 11 2 0 8.14 8.07 -11 2 0 29.62 14.21 -11 -2 0 12.61 8.28 -11 -2 0 7.76 8.68 12 -2 0 38.86 17.27 12 2 0 111.73 40.53 -12 2 0 43.26 18.32 -12 -2 0 81.83 42.81 13 -2 0 17.72 10.71 13 2 0 11.02 12.55 13 2 0 13.75 8.80 -13 2 0 26.43 12.52 -13 -2 0 16.20 9.40 14 -2 0 106.98 38.90 14 2 0 163.14 96.82 14 2 0 63.42 23.78 -14 2 0 112.74 40.90 -14 -2 0 80.21 29.60 15 -2 0 1.52 6.95 15 2 0 8.97 7.63 -15 2 0 1.72 6.75 -15 -2 0 22.22 17.26 -15 -2 0 17.21 10.04 16 -2 0 233.63 83.28 16 -2 0 177.16 92.58 16 2 0 252.61 89.77 -16 2 0 318.52 119.82 -16 2 0 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2.19 -4 -5 -14 12.70 9.72 -4 -5 -14 9.92 5.02 5 5 14 12.31 9.20 5 5 14 10.13 9.35 5 -5 -14 10.44 5.28 5 -5 -14 79.41 46.99 -5 -5 14 -0.04 6.40 -5 -5 14 22.50 11.90 -5 5 -14 -1.52 6.88 5 -5 14 -2.94 7.42 5 5 -14 -3.54 8.33 5 5 -14 5.52 4.08 -5 5 14 11.52 13.89 -5 -5 -14 8.94 9.07 -5 -5 -14 16.93 8.54 6 5 14 35.33 18.20 6 -5 -14 4.80 2.47 6 -5 -14 37.84 22.76 -6 -5 14 -1.28 6.35 -6 -5 14 10.54 5.94 -6 5 -14 -1.59 6.60 6 -5 14 2.97 7.66 6 5 -14 2.30 8.67 -6 5 14 24.04 18.72 -6 -5 -14 4.04 7.71 -6 -5 -14 36.54 18.65 -6 -5 -14 11.48 5.81 7 -5 -14 50.86 25.61 -7 -5 14 99.77 51.93 -7 5 -14 44.65 24.56 7 -5 14 73.29 39.18 7 5 -14 16.34 12.21 7 5 -14 44.65 23.54 -7 -5 -14 44.29 27.24 -7 -5 -14 73.72 37.12 8 5 14 0.37 4.88 8 5 14 2.29 1.32 8 5 14 14.28 11.44 8 -5 -14 2.58 1.44 -8 -5 14 25.99 13.91 -8 -5 14 -0.41 4.77 8 5 -14 9.52 6.05 8 5 -14 0.39 6.95 -8 -5 -14 17.27 10.80 -8 -5 -14 11.35 5.75 9 5 14 1.83 1.12 9 5 14 9.22 10.01 9 -5 -14 5.16 5.70 -9 -5 14 13.61 7.74 -9 -5 14 -1.14 4.91 9 5 -14 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83.29 -9 0 -15 12.50 6.72 10 0 -15 26.15 17.31 -10 0 15 34.57 19.36 -10 0 -15 16.94 9.07 11 0 15 44.06 23.82 -11 0 15 52.98 28.60 0 1 -15 13.97 8.60 0 1 15 29.28 17.02 0 -1 -15 24.98 9.75 0 -1 -15 41.44 22.53 1 1 15 6.55 6.75 1 -1 -15 15.23 6.16 1 -1 -15 11.84 8.34 -1 1 -15 5.59 5.09 1 1 -15 4.58 4.85 -1 1 15 4.47 11.46 -1 -1 -15 4.54 5.79 2 1 15 11.54 8.97 2 -1 -15 20.20 12.06 -2 -1 15 3.47 5.55 -2 1 -15 10.70 7.06 2 1 -15 5.34 5.28 -2 -1 -15 2.02 5.04 3 1 15 2.98 6.81 3 -1 -15 2.95 5.37 -3 -1 15 3.55 5.15 -3 1 -15 7.12 5.60 3 -1 15 4.05 5.52 3 1 -15 14.89 9.14 -3 1 15 2.56 1.70 -3 -1 -15 3.60 13.43 -3 -1 -15 1.53 4.65 4 1 15 2.68 5.92 4 -1 -15 3.75 5.72 -4 -1 15 7.53 6.21 -4 1 -15 1.72 4.54 4 -1 15 2.85 2.75 4 -1 15 7.10 5.90 4 1 -15 3.16 4.73 -4 1 15 10.91 9.25 -4 -1 -15 1.80 12.25 5 1 15 8.07 7.59 5 -1 -15 3.86 6.42 -5 -1 15 14.98 9.34 -5 1 -15 2.93 4.07 5 -1 15 0.93 2.73 5 -1 15 3.85 2.16 5 -1 15 6.89 6.08 5 1 -15 4.40 5.27 -5 1 15 5.00 6.75 6 1 15 3.44 2.29 6 1 15 3.99 6.42 6 -1 -15 1.40 5.33 6 -1 -15 5.31 6.03 -6 -1 15 4.51 5.80 -6 1 -15 1.99 2.96 -6 1 -15 4.27 4.61 -6 1 -15 7.31 3.97 6 -1 15 5.08 2.85 6 -1 15 9.83 7.18 6 -1 15 3.66 3.08 6 1 -15 2.85 5.42 -6 1 15 2.60 7.14 7 1 15 3.77 2.66 7 1 15 4.56 6.08 -7 -1 15 12.68 8.78 -7 1 -15 5.81 3.97 -7 1 -15 5.73 3.24 -7 1 -15 12.07 7.80 7 -1 15 10.18 5.50 7 -1 15 3.21 5.01 -7 1 15 4.16 7.24 -7 -1 -15 -5.09 7.09 -7 -1 -15 5.10 6.43 8 1 15 20.05 10.52 8 1 15 2.26 5.94 8 -1 -15 16.79 11.08 -8 -1 15 18.53 11.32 -8 1 -15 16.63 8.80 -8 1 -15 6.03 4.05 8 -1 15 21.43 11.30 8 -1 15 10.77 7.68 -8 1 15 4.43 6.95 -8 -1 -15 16.17 8.84 9 -1 -15 5.05 5.26 -9 -1 15 17.28 10.59 -9 1 -15 0.57 1.95 -9 1 -15 4.91 4.12 9 -1 15 5.09 3.33 -9 1 15 5.37 6.96 10 1 15 1.15 5.69 -10 -1 15 3.71 5.25 -10 1 -15 0.48 2.52 10 -1 15 5.40 5.53 -10 1 15 3.88 6.28 -10 -1 -15 6.58 3.81 11 1 15 1.46 5.18 -11 -1 15 3.71 4.95 11 -1 15 3.16 4.89 -11 1 15 12.35 9.01 0 -2 15 0.35 4.07 0 2 -15 0.43 3.52 0 2 15 0.09 0.46 0 2 15 6.82 7.79 0 -2 -15 4.73 5.74 1 2 15 0.88 0.65 1 2 15 3.13 6.83 1 -2 -15 0.69 5.49 -1 -2 15 0.79 4.24 -1 2 -15 0.37 3.39 1 -2 15 0.66 4.50 1 2 -15 0.03 3.67 -1 2 15 2.03 1.13 -1 2 15 2.10 6.96 -1 -2 -15 4.41 6.09 2 2 15 4.59 2.36 2 2 15 0.33 6.90 2 -2 -15 2.64 4.99 2 -2 -15 6.49 6.37 -2 -2 15 8.64 6.55 -2 2 -15 5.47 4.62 2 -2 15 1.88 4.08 2 2 -15 0.37 4.09 -2 2 15 6.40 7.77 -2 2 15 3.07 1.61 -2 -2 -15 3.72 5.39 3 2 15 2.70 1.45 3 2 15 -0.16 5.96 3 -2 -15 24.19 13.99 -3 -2 15 6.32 5.79 -3 2 -15 4.47 4.32 3 -2 15 13.55 8.32 -3 2 15 3.72 1.92 -3 2 15 9.26 8.64 -3 -2 -15 8.33 7.23 4 2 15 36.45 18.37 4 2 15 12.35 8.82 4 -2 -15 61.26 32.64 -4 -2 15 10.18 7.24 -4 2 -15 28.83 15.82 4 -2 15 38.82 20.83 -4 2 15 27.52 13.87 -4 2 15 7.40 7.92 -4 -2 -15 31.16 17.32 5 2 15 14.91 13.65 5 2 15 16.98 8.56 5 -2 -15 5.71 5.33 -5 -2 15 3.74 4.59 -5 2 -15 14.39 7.53 -5 2 -15 4.52 4.58 5 -2 15 4.32 4.70 -5 2 15 5.71 7.49 -5 -2 -15 3.08 5.23 6 2 15 -1.48 10.46 6 2 15 9.31 4.72 6 -2 -15 7.08 7.76 -6 -2 15 28.07 15.65 -6 2 -15 1.09 1.52 -6 2 -15 1.02 3.85 6 -2 15 1.56 4.10 -6 2 15 1.40 6.75 -6 2 15 1.46 0.86 -6 -2 -15 0.20 5.46 7 2 15 3.09 1.65 7 2 15 12.32 14.22 7 2 15 2.90 2.24 -7 -2 15 1.52 4.77 -7 2 -15 1.37 2.08 -7 2 -15 1.30 4.10 7 -2 15 0.99 3.84 7 -2 15 0.16 2.54 -7 2 15 -0.46 6.30 -7 2 15 0.90 0.62 -7 -2 -15 0.44 5.25 8 2 15 0.90 1.92 -8 -2 15 5.04 5.45 -8 2 -15 -1.14 2.14 8 -2 15 5.34 3.66 8 -2 15 4.55 4.58 -8 2 15 2.80 6.47 -8 -2 -15 -6.86 6.90 -9 -2 15 1.57 4.67 9 -2 15 2.32 3.22 -9 2 15 2.00 6.07 -9 -2 -15 2.98 2.74 -10 -2 15 3.93 5.05 10 -2 15 9.28 4.92 10 -2 15 4.78 4.69 -10 2 15 3.61 5.88 -10 -2 -15 12.83 6.93 -11 -2 15 0.79 5.12 11 -2 15 4.52 3.49 11 -2 15 -0.03 4.39 0 -3 15 6.51 3.80 0 -3 15 5.54 4.82 0 3 -15 8.86 6.74 0 3 15 3.34 1.76 0 -3 -15 2.74 1.45 0 -3 -15 4.06 5.67 1 3 15 7.96 4.04 1 -3 -15 0.58 0.51 1 -3 -15 2.48 5.52 1 -3 -15 1.59 5.27 -1 -3 15 0.82 3.57 -1 3 -15 2.38 4.75 1 -3 15 21.90 11.43 1 -3 15 -0.55 3.46 1 3 -15 2.10 4.81 -1 3 15 8.48 4.30 -1 -3 -15 1.45 4.85 -1 -3 -15 1.93 1.06 2 3 15 8.52 4.32 2 -3 -15 6.91 3.50 2 -3 -15 13.10 9.49 2 -3 -15 4.56 5.85 -2 -3 15 7.10 5.45 -2 3 -15 13.17 8.70 2 -3 15 17.24 8.99 2 -3 15 10.21 6.89 2 3 -15 7.34 6.24 -2 3 15 7.06 3.59 -2 -3 -15 8.58 8.47 -2 -3 -15 7.40 3.75 3 3 15 14.36 7.26 3 -3 -15 5.18 9.29 3 -3 -15 12.52 6.32 3 -3 -15 4.40 6.00 -3 -3 15 3.56 4.28 -3 3 -15 6.73 6.28 3 -3 15 4.89 4.78 3 3 -15 7.15 6.25 -3 3 15 11.10 5.61 -3 -3 -15 0.02 6.65 -3 -3 -15 11.01 5.56 4 3 15 5.09 2.62 4 3 15 2.89 5.83 4 -3 -15 1.98 5.62 4 -3 -15 0.82 0.59 -4 -3 15 1.36 3.71 -4 3 -15 5.73 6.01 4 -3 15 2.04 4.06 4 3 -15 4.69 5.55 -4 3 15 4.22 2.19 -4 3 15 0.40 6.84 -4 -3 -15 1.30 0.79 5 3 15 5.34 2.74 5 -3 -15 10.07 11.40 5 -3 -15 1.48 0.87 5 -3 -15 1.32 6.49 -5 -3 15 -0.45 3.68 -5 3 -15 2.20 4.92 5 3 -15 3.24 5.62 -5 3 15 -0.67 5.79 -5 -3 -15 0.45 0.55 6 3 15 4.19 2.17 -6 -3 15 1.04 3.87 -6 3 -15 4.34 5.41 6 3 -15 3.28 6.25 -6 3 15 6.46 3.29 -6 3 15 1.61 6.94 7 3 15 5.96 3.05 -7 -3 15 5.69 5.74 -7 3 -15 13.46 8.86 -7 3 15 16.21 8.18 -7 3 15 0.49 6.60 8 -3 -15 20.38 12.85 -8 -3 15 19.40 11.51 -8 3 15 2.77 6.61 9 -3 -15 13.73 9.32 -9 -3 15 6.14 5.83 -9 3 15 2.96 6.50 -9 -3 -15 -0.55 5.68 10 3 15 4.64 6.60 -10 -3 15 1.48 4.99 -10 3 15 -0.18 5.66 11 3 15 12.20 8.91 -11 -3 15 18.18 11.30 11 -3 15 20.74 8.71 -11 3 15 26.45 10.14 0 -4 15 2.46 1.75 0 -4 15 0.87 4.93 0 4 -15 0.34 1.28 0 4 15 2.47 1.34 0 -4 -15 -1.87 13.54 1 4 15 2.78 1.49 -1 -4 15 6.99 3.88 -1 -4 15 -0.18 4.85 -1 4 -15 2.29 1.48 1 -4 15 3.89 2.32 1 -4 15 0.64 4.80 1 4 -15 1.47 2.14 -1 4 15 3.95 2.05 -1 -4 -15 2.20 7.12 2 4 15 5.84 2.99 2 -4 -15 11.75 8.89 -2 -4 15 5.16 3.26 -2 -4 15 -0.43 4.12 -2 4 -15 2.45 1.69 2 -4 15 -0.97 4.95 2 4 -15 0.39 2.02 -2 4 15 3.31 1.74 -2 -4 -15 1.78 7.30 3 4 15 4.33 2.24 -3 -4 15 15.37 8.29 -3 -4 15 1.40 4.23 3 -4 15 10.28 7.49 3 4 -15 -1.81 2.95 -3 4 15 4.58 2.36 -3 -4 -15 5.15 6.99 4 4 15 5.48 2.82 4 4 15 3.23 7.89 -4 -4 15 6.84 4.46 -4 -4 15 6.23 5.53 4 -4 15 4.68 5.51 -4 4 15 13.09 6.62 5 4 15 9.27 4.71 5 -4 -15 3.51 5.68 -5 -4 15 -0.40 4.01 -5 -4 15 7.43 4.56 5 -4 15 10.61 7.48 6 4 15 1.72 1.06 6 -4 -15 18.19 11.79 -6 -4 15 9.06 5.47 -6 -4 15 0.04 4.84 6 -4 15 0.12 4.51 -6 4 15 1.51 0.90 -6 -4 -15 -2.15 6.84 -6 -4 -15 2.23 5.68 7 -4 -15 6.54 6.11 -7 -4 15 3.97 3.10 -7 -4 15 0.37 4.85 7 -4 15 1.02 4.63 -7 -4 -15 -2.53 6.99 -7 -4 -15 1.66 5.21 8 4 15 3.90 6.01 8 -4 -15 9.71 6.93 -8 -4 15 1.75 4.93 8 -4 15 -1.12 4.65 -8 -4 -15 6.26 6.18 9 4 15 3.57 6.11 -9 -4 15 -0.21 4.52 -9 -4 -15 0.60 6.42 10 4 15 0.95 6.19 -10 -4 15 1.05 4.75 10 -4 15 0.24 4.82 -10 -4 -15 4.58 5.98 -11 -4 15 -0.01 4.88 11 -4 15 -0.96 4.88 -11 -4 -15 0.77 6.40 0 -5 15 26.08 13.65 0 -5 15 3.56 6.07 0 5 -15 25.33 15.23 0 5 -15 63.58 33.02 0 5 15 43.68 22.00 0 -5 -15 52.54 26.46 1 5 15 4.02 2.11 1 -5 -15 14.95 7.55 -1 -5 15 7.99 4.32 -1 -5 15 -0.85 5.52 -1 5 -15 -2.07 6.26 1 -5 15 -1.67 5.47 1 5 -15 13.57 7.18 1 5 -15 -3.88 7.34 -1 5 15 0.59 0.65 -1 -5 -15 9.72 9.44 -1 -5 -15 12.55 6.34 2 5 15 31.80 16.02 2 -5 -15 38.89 19.58 -2 -5 15 2.51 5.99 -2 -5 15 49.38 25.70 -2 5 -15 5.88 7.20 2 -5 15 -0.21 5.50 2 5 -15 39.41 20.55 2 5 -15 5.57 8.34 -2 5 15 28.74 14.48 -2 -5 -15 40.66 20.48 3 5 15 6.93 3.54 3 -5 -15 13.38 6.76 3 -5 -15 19.07 12.41 -3 -5 15 -0.74 4.58 -3 5 -15 2.27 6.00 3 -5 15 -1.79 5.08 3 5 -15 9.00 5.19 3 5 -15 0.47 7.50 -3 5 15 9.66 4.90 -3 -5 -15 9.41 4.77 4 5 15 1.90 1.16 4 -5 -15 12.15 6.14 -4 -5 15 -0.08 4.48 -4 -5 15 3.19 2.31 -4 5 -15 -0.03 5.43 4 -5 15 -1.46 4.67 4 5 -15 2.73 2.99 4 5 -15 0.15 6.21 -4 5 15 0.71 0.63 -4 -5 -15 83.76 39.64 5 5 15 3.85 2.05 5 -5 -15 8.16 7.11 -5 -5 15 3.61 2.87 -5 -5 15 -0.11 4.46 -5 5 -15 -1.82 5.21 5 -5 15 -1.49 4.97 -5 -5 -15 9.98 9.01 6 5 15 2.68 6.17 6 -5 -15 20.80 13.04 -6 -5 15 8.79 5.10 -6 -5 15 -1.44 4.94 -6 5 -15 0.61 5.43 6 -5 15 -1.79 4.87 6 5 -15 3.40 3.45 -6 -5 -15 3.83 8.10 7 5 15 86.22 40.67 7 -5 -15 34.49 20.85 -7 -5 15 16.93 10.40 7 -5 15 -1.87 4.47 -7 -5 -15 26.64 29.51 -7 -5 -15 79.24 37.41 8 5 15 12.78 8.39 -8 -5 15 -1.05 4.85 8 -5 15 -3.53 4.42 8 5 -15 33.32 17.77 -8 -5 -15 40.66 20.25 -9 -5 15 75.14 39.19 -9 -5 -15 94.29 44.42 10 -5 15 -1.51 3.66 -10 -5 -15 30.97 16.10 0 -6 15 0.76 1.54 0 -6 15 -0.49 7.46 0 6 -15 1.52 1.90 1 -6 -15 3.06 7.38 -1 -6 15 0.73 7.39 -1 -6 15 0.52 1.65 1 -6 15 0.06 7.45 1 6 -15 1.98 1.82 -2 -6 15 3.39 2.23 -2 -6 15 0.54 7.46 2 -6 15 -1.19 6.84 2 6 -15 2.50 2.12 -2 -6 -15 33.70 17.19 3 -6 -15 9.32 8.47 -3 -6 15 2.00 7.52 -3 -6 15 12.90 6.87 3 -6 15 0.40 6.67 3 6 -15 4.32 2.90 -3 -6 -15 12.15 22.64 4 6 15 -0.97 5.41 4 -6 -15 21.11 13.36 -4 -6 15 3.32 2.43 -4 -6 15 3.91 8.12 4 -6 15 -1.87 6.45 4 6 -15 8.21 4.76 -4 -6 -15 2.29 8.62 5 6 15 13.06 8.59 5 -6 -15 16.82 11.09 -5 -6 15 3.54 7.71 5 -6 15 0.17 5.94 5 6 -15 2.65 2.58 -5 -6 -15 1.25 5.83 -6 -6 15 3.95 2.81 -6 -6 15 4.51 7.45 6 -6 15 0.34 5.49 6 6 -15 0.66 2.30 -6 -6 -15 1.05 5.70 7 6 15 -1.06 4.50 7 -6 -15 2.88 5.45 -7 -6 15 3.00 2.39 -7 -6 15 4.30 6.54 7 -6 15 -0.77 5.19 7 6 -15 0.57 3.03 -7 -6 -15 0.45 6.24 -7 -6 -15 3.85 6.05 -8 -6 15 1.74 2.37 -8 -6 15 2.65 6.25 8 -6 15 -0.88 4.73 8 6 -15 -0.04 3.60 -8 -6 -15 3.22 7.81 -8 -6 -15 3.07 6.28 -9 -6 15 -0.56 5.34 -9 -6 -15 1.22 4.60 0 7 -15 -4.86 7.46 0 -7 -15 13.99 11.38 1 7 15 32.78 16.54 1 -7 -15 30.73 19.69 -1 -7 15 16.58 8.75 1 7 -15 16.44 8.88 -1 -7 -15 16.67 12.55 2 7 15 2.02 5.63 -2 -7 15 7.01 4.17 2 7 -15 15.78 8.55 3 -7 -15 7.87 7.31 -3 -7 15 15.61 8.30 3 7 -15 7.68 4.40 -3 -7 -15 7.19 7.35 -4 -7 15 4.34 2.70 -4 -7 -15 5.66 6.91 5 -7 -15 8.82 8.15 -5 -7 15 5.60 3.44 5 7 -15 4.39 3.14 -5 -7 -15 -2.32 5.71 6 -7 -15 8.62 7.31 -6 -7 15 5.91 3.66 6 7 -15 10.75 6.08 -6 -7 -15 6.26 8.70 -7 -7 15 5.47 3.60 7 7 -15 3.16 2.93 0 8 15 1.22 4.90 0 -8 -15 13.47 10.52 1 -8 -15 12.58 10.04 1 8 -15 52.02 28.19 -1 8 15 19.42 10.54 -1 -8 -15 55.51 33.80 -1 -8 -15 2.55 6.13 2 -8 -15 28.68 18.21 -2 -8 15 1.74 1.72 2 8 -15 2.20 3.01 -2 -8 -15 44.60 27.61 3 8 -15 40.14 21.06 -3 -8 -15 49.15 30.21 4 -8 -15 35.99 22.27 -4 -8 15 75.30 39.17 4 8 -15 100.61 52.35 -4 -8 -15 25.24 16.54 5 -8 15 120.75 43.21 -6 -8 15 21.41 11.30 6 8 -15 13.46 7.44 0 -9 -15 7.66 8.52 0 -9 -15 14.42 9.23 1 -9 -15 3.86 6.03 -1 -9 -15 0.23 6.47 2 -9 -15 3.21 7.81 2 -9 -15 2.55 4.94 -2 -9 15 -0.24 1.67 2 -9 15 -0.72 3.81 2 9 -15 -4.76 7.42 -2 9 15 2.06 4.61 -2 -9 -15 3.19 7.33 -3 -9 15 2.30 1.91 3 9 -15 -1.14 2.95 -3 9 15 4.22 4.87 -3 -9 -15 6.80 8.83 4 9 -15 1.19 3.00 -4 9 15 4.05 5.43 4 -10 -15 1.64 4.67 -5 10 15 6.29 5.21 0 0 16 92.11 34.69 0 0 16 187.11 98.05 1 0 16 65.36 24.73 1 0 16 59.62 32.28 -1 0 16 38.34 21.80 2 0 16 23.82 9.47 2 0 16 21.81 13.63 -2 0 16 28.52 17.05 3 0 16 79.33 42.25 -3 0 16 41.45 23.44 -3 0 -16 9.60 4.67 4 0 16 32.27 18.38 4 0 -16 -1.99 11.80 -4 0 16 15.89 11.38 -4 0 -16 7.04 4.00 5 0 16 10.73 8.96 -5 0 16 21.41 13.66 -5 0 -16 15.82 6.91 7 0 16 43.50 23.82 -7 0 16 37.34 21.06 -8 0 16 24.56 15.24 0 -1 -16 5.61 3.09 1 1 16 6.64 7.05 1 -1 -16 1.19 2.07 2 1 16 23.77 14.35 2 -1 16 15.54 10.03 3 1 16 10.70 8.59 3 -1 16 4.34 5.44 -3 1 16 3.42 1.87 -3 -1 -16 2.90 13.12 4 1 16 5.31 7.11 -4 -1 16 9.91 8.27 4 -1 16 0.19 2.31 4 -1 16 1.98 5.33 -4 1 16 27.81 16.44 -4 -1 -16 3.08 14.11 5 1 16 4.17 6.21 -5 -1 16 11.65 8.48 5 -1 16 78.99 29.90 5 -1 16 5.70 3.09 5 -1 16 6.09 6.11 -5 1 16 5.38 6.75 6 1 16 8.15 7.66 -6 -1 16 7.76 6.92 -6 1 -16 3.22 2.44 6 -1 16 6.95 6.37 6 -1 16 18.51 7.62 -6 1 16 6.12 7.68 7 1 16 3.51 6.20 -7 -1 16 7.27 6.82 -7 1 -16 6.42 4.41 7 -1 16 7.43 6.82 -7 1 16 3.65 6.93 -8 -1 16 13.85 9.49 8 -1 16 5.68 6.16 0 -2 16 6.98 6.42 0 2 16 3.65 7.06 1 2 16 1.98 6.79 -1 -2 16 3.24 5.49 1 -2 16 1.77 4.78 -1 2 16 2.52 6.89 2 2 16 2.07 6.71 2 -2 -16 2.42 8.54 -2 -2 16 3.94 5.68 2 -2 16 4.71 5.75 -2 2 16 1.46 6.74 3 2 16 -0.56 6.98 3 -2 -16 -4.41 17.17 -3 -2 16 3.29 5.64 3 -2 16 9.61 7.00 -3 2 16 2.32 6.82 4 2 16 0.61 5.99 4 -2 -16 2.64 1.61 -4 -2 16 3.73 5.64 4 -2 16 3.63 5.09 -4 2 16 5.86 7.55 5 2 16 -0.83 5.78 5 -2 -16 86.87 52.08 -5 -2 16 3.05 5.55 -5 2 -16 4.25 2.44 5 -2 16 6.65 3.57 5 -2 16 1.05 4.41 -5 2 16 2.45 6.71 -6 -2 16 3.00 5.87 6 -2 16 1.08 4.88 -6 2 16 0.32 6.27 -7 -2 16 10.20 8.40 7 -2 16 4.06 3.05 7 -2 16 6.13 5.99 -7 2 16 4.80 7.79 8 -2 16 1.17 2.92 8 -2 16 3.82 5.77 1 -3 16 1.88 1.51 -1 -3 -16 -2.67 25.01 2 -3 -16 0.17 5.33 2 -3 16 8.42 4.45 -2 -3 -16 -0.37 6.75 3 -3 -16 3.02 5.17 -3 3 16 -2.27 6.16 -4 3 16 0.38 6.99 -5 3 16 3.15 7.28 6 -3 16 10.44 8.69 -6 3 16 13.06 10.61 7 -3 16 6.04 6.32 0 -4 16 7.23 4.00 0 -4 16 -2.34 5.39 0 4 -16 -0.06 1.46 0 -4 -16 3.51 6.79 -1 -4 16 3.32 2.25 -1 -4 16 -0.09 5.43 -1 4 -16 2.81 1.74 1 -4 16 5.31 2.91 1 -4 16 0.85 5.12 1 4 -16 -0.85 1.59 -1 -4 -16 -0.35 6.76 -2 -4 16 22.62 11.90 -2 -4 16 -0.31 5.50 -2 4 -16 4.82 2.61 2 -4 16 -1.81 5.24 -2 -4 -16 1.54 6.52 3 -4 -16 3.43 5.64 -3 -4 16 -0.06 5.49 3 -4 16 -0.68 5.02 -4 -4 16 2.15 2.47 -4 -4 16 -0.48 5.47 4 -4 16 -0.63 4.93 -5 -4 16 1.15 5.95 5 -4 16 -1.27 5.23 -6 -4 16 5.27 6.99 6 -4 16 0.62 5.48 -7 -4 16 4.51 6.67 7 -4 16 0.28 5.50 0 -5 16 2.91 1.86 0 5 -16 3.08 1.94 0 -5 -16 17.91 12.95 -1 -5 16 4.06 2.46 -1 5 -16 1.57 1.30 1 -5 16 4.42 2.51 1 5 -16 3.99 2.40 -2 -5 16 47.48 24.73 -2 5 -16 18.40 10.20 2 5 -16 9.27 5.23 -3 -5 -16 4.10 7.15 6 5 16 8.44 7.34 0 -6 16 9.04 4.85 0 -6 16 10.22 8.51 -1 -6 16 -0.12 6.29 -1 6 -16 0.22 3.03 1 -6 16 0.63 6.11 -2 -6 16 -0.58 5.99 2 -6 16 -0.70 5.58 -3 -6 16 0.95 5.18 3 -6 16 -0.11 5.29 4 6 16 2.68 5.32 -4 -6 16 -0.83 5.31 4 -6 16 -0.64 5.14 5 6 16 -2.29 5.64 -5 -6 16 -2.23 5.14 5 -6 16 0.39 5.07 2 7 16 1.89 5.50 -3 -7 16 2.40 6.32 4 7 16 166.46 77.37 -4 -7 16 11.16 8.76 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30540 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 0.42858(18) 0.4709(3) 0.3117(3) 0.0356(12) Uani 1 1 d D U . Si2 Si 0.22479(19) 0.6732(3) 0.5266(3) 0.0365(13) Uani 1 1 d D U . Si3 Si 0.07802(19) 0.6707(3) 0.1695(4) 0.0411(14) Uani 1 1 d D U . Si4 Si 0.0786(2) 0.4437(2) 0.1603(4) 0.0340(13) Uani 1 1 d D U . Si5 Si 0.43107(18) 0.6311(3) 0.3140(3) 0.0393(14) Uani 1 1 d D U . Si6 Si 0.37949(19) 0.6733(3) 0.5249(4) 0.0389(14) Uani 1 1 d D U . Si7 Si 0.2201(2) 0.4378(3) 0.5272(4) 0.0371(13) Uani 1 1 d D U . Si8 Si 0.1840(2) 0.5578(3) 0.6660(4) 0.0376(14) Uani 1 1 d D U . Si9 Si 0.1851(2) 0.3276(3) 0.6773(4) 0.0412(15) Uani 1 1 d D U . Si10 Si 0.19442(19) 0.4698(4) 0.3041(4) 0.0439(15) Uani 1 1 d D U . Si11 Si 0.1229(2) 0.5640(3) 0.0239(4) 0.0415(14) Uani 1 1 d D U . Si12 Si 0.1937(2) 0.6311(3) 0.3104(4) 0.0461(16) Uani 1 1 d D U . O1 O 0.5058(3) 0.4519(5) 0.2963(6) 0.053(2) Uani 1 1 d D U . O2 O 0.2587(4) 0.6543(6) 0.2538(7) 0.068(3) Uani 1 1 d D U . O3 O 0.2594(4) 0.4455(5) 0.2467(8) 0.066(3) Uani 1 1 d D U . O4 O 0.4217(4) 0.5515(4) 0.3266(8) 0.066(2) Uani 1 1 d D U . O5 O 0.1147(3) 0.3459(5) 0.7232(6) 0.058(2) Uani 1 1 d D U . O6 O 0.3017(3) 0.6566(6) 0.5276(8) 0.059(2) Uani 1 1 d D U . O7 O 0.3868(3) 0.4455(4) 0.2191(5) 0.048(2) Uani 1 1 d D U . O8 O 0.3893(6) 0.7500 0.5593(10) 0.062(3) Uani 1 2 d DS TU P O9 O 0.5054(3) 0.6492(6) 0.2942(6) 0.054(2) Uani 1 1 d D U . O10 O 0.1868(7) 0.2500 0.6455(10) 0.067(4) Uani 1 2 d DS TU P O11 O 0.1920(4) 0.6585(6) 0.4222(6) 0.058(2) Uani 1 1 d D U . O12 O 0.2132(5) 0.7500 0.5545(8) 0.050(3) Uani 1 2 d DS TU P O13 O 0.4194(4) 0.6262(5) 0.5988(6) 0.055(2) Uani 1 1 d D U . O14 O 0.1898(4) 0.4992(5) 0.5847(7) 0.061(2) Uani 1 1 d D U . O15 O 0.2981(3) 0.4401(6) 0.5281(9) 0.068(3) Uani 1 1 d D U . O16 O 0.1299(4) 0.4451(6) 0.2473(7) 0.071(3) Uani 1 1 d D U . O17 O 0.1942(4) 0.4406(5) 0.4135(7) 0.060(3) Uani 1 1 d D U . O18 O 0.0768(8) 0.7500 0.1402(9) 0.077(4) Uani 1 2 d DS TU P O19 O 0.4004(4) 0.4365(4) 0.4112(6) 0.054(2) Uani 1 1 d D U . O20 O 0.0984(5) 0.6339(5) 0.0684(7) 0.064(2) Uani 1 1 d D U . O21 O 0.1874(4) 0.6309(4) 0.6119(6) 0.0463(19) Uani 1 1 d D U . O22 O 0.1931(4) 0.3682(5) 0.5760(7) 0.058(2) Uani 1 1 d D U . O23 O 0.1290(3) 0.6565(6) 0.2584(6) 0.064(2) Uani 1 1 d D U . O24 O 0.4093(5) 0.6622(6) 0.4164(7) 0.073(3) Uani 1 1 d D U . O25 O 0.0883(4) 0.5027(5) 0.0816(7) 0.064(2) Uani 1 1 d D U . O26 O 0.1942(6) 0.5497(5) 0.3099(11) 0.086(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 0.0229(19) 0.047(3) 0.037(2) -0.002(2) -0.0153(15) 0.0009(17) Si2 0.024(2) 0.049(4) 0.037(2) 0.003(2) 0.0028(16) -0.0008(17) Si3 0.0200(19) 0.061(4) 0.042(3) 0.002(2) 0.0019(16) -0.0057(18) Si4 0.020(2) 0.040(4) 0.042(2) -0.005(2) 0.0053(16) 0.0031(15) Si5 0.0189(19) 0.057(4) 0.042(3) -0.006(2) -0.0017(15) 0.0026(17) Si6 0.0201(19) 0.053(4) 0.043(3) -0.001(2) -0.0004(16) 0.0027(17) Si7 0.025(2) 0.042(3) 0.044(3) -0.005(2) 0.0029(17) 0.0016(16) Si8 0.027(2) 0.047(4) 0.038(3) 0.000(2) 0.0179(18) -0.0003(16) Si9 0.025(2) 0.051(4) 0.047(3) 0.003(2) 0.0022(17) 0.0021(18) Si10 0.028(2) 0.063(4) 0.041(3) -0.004(3) -0.0025(16) 0.0043(19) Si11 0.020(2) 0.060(4) 0.045(3) 0.001(2) 0.0015(17) 0.0005(18) Si12 0.027(2) 0.070(4) 0.041(3) -0.005(2) -0.0101(17) -0.0021(19) O1 0.037(3) 0.081(7) 0.041(4) 0.003(4) -0.012(3) 0.011(3) O2 0.047(4) 0.096(8) 0.062(5) 0.002(5) 0.002(3) -0.009(4) O3 0.041(4) 0.089(8) 0.069(5) -0.008(5) 0.004(3) 0.003(3) O4 0.055(4) 0.062(4) 0.079(6) -0.003(3) -0.001(4) 0.004(3) O5 0.026(3) 0.077(7) 0.070(5) -0.013(5) 0.009(3) 0.004(3) O6 0.028(3) 0.065(6) 0.086(6) 0.004(5) 0.001(3) 0.007(3) O7 0.035(3) 0.072(6) 0.038(3) -0.004(3) -0.014(3) 0.001(3) O8 0.052(5) 0.056(6) 0.078(7) 0.000 0.003(5) 0.000 O9 0.036(3) 0.091(7) 0.035(4) 0.000(4) -0.009(3) -0.011(3) O10 0.090(8) 0.061(6) 0.049(7) 0.000 0.041(6) 0.000 O11 0.057(4) 0.070(6) 0.046(4) -0.004(3) -0.004(3) -0.007(4) O12 0.037(4) 0.053(5) 0.059(6) 0.000 0.024(4) 0.000 O13 0.040(3) 0.072(6) 0.053(4) 0.004(4) -0.009(3) 0.004(3) O14 0.069(5) 0.057(5) 0.055(5) -0.004(4) 0.011(3) 0.011(3) O15 0.032(4) 0.087(9) 0.086(7) -0.001(5) 0.004(3) 0.001(3) O16 0.041(4) 0.110(9) 0.062(5) 0.003(4) -0.018(3) -0.009(4) O17 0.053(4) 0.079(7) 0.049(4) 0.002(3) -0.005(3) -0.008(3) O18 0.119(11) 0.064(7) 0.049(6) 0.000 0.005(6) 0.000 O19 0.066(5) 0.054(6) 0.041(4) -0.001(3) 0.001(3) -0.002(3) O20 0.065(5) 0.066(6) 0.060(5) -0.003(4) 0.004(4) 0.006(4) O21 0.053(4) 0.046(5) 0.041(4) -0.007(3) 0.025(3) 0.000(3) O22 0.062(5) 0.056(5) 0.055(4) 0.002(3) 0.013(3) -0.001(3) O23 0.041(3) 0.098(7) 0.055(4) 0.008(4) -0.004(3) -0.005(4) O24 0.062(4) 0.089(7) 0.069(4) -0.020(4) 0.018(4) -0.007(4) O25 0.060(4) 0.067(6) 0.066(5) 0.018(4) -0.002(4) -0.007(4) O26 0.094(7) 0.075(5) 0.090(8) -0.004(4) -0.003(5) -0.002(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 O4 Si1 O7 111.0(6) . . O4 Si1 O19 105.6(6) . . O7 Si1 O19 110.1(5) . . O4 Si1 O1 109.0(5) . . O7 Si1 O1 110.1(5) . . O19 Si1 O1 111.0(5) . . O12 Si2 O6 109.9(6) . . O12 Si2 O11 108.9(7) . . O6 Si2 O11 112.5(6) . . O12 Si2 O21 103.9(5) . . O6 Si2 O21 110.8(5) . . O11 Si2 O21 110.6(5) . . O18 Si3 O20 102.7(6) . . O18 Si3 O9 108.2(7) . 6_556 O20 Si3 O9 112.6(5) . 6_556 O18 Si3 O23 111.3(7) . . O20 Si3 O23 113.5(6) . . O9 Si3 O23 108.4(5) 6_556 . O25 Si4 O13 104.9(6) . 2_564 O25 Si4 O16 114.4(6) . . O13 Si4 O16 113.0(6) 2_564 . O25 Si4 O1 107.0(5) . 6_556 O13 Si4 O1 107.5(5) 2_564 6_556 O16 Si4 O1 109.5(6) . 6_556 O4 Si5 O9 110.8(6) . . O4 Si5 O24 104.3(7) . . O9 Si5 O24 109.6(5) . . O4 Si5 O5 106.6(6) . 2_564 O9 Si5 O5 111.2(5) . 2_564 O24 Si5 O5 114.0(6) . 2_564 O8 Si6 O13 107.0(6) . . O8 Si6 O24 110.5(7) . . O13 Si6 O24 108.2(6) . . O8 Si6 O6 107.8(6) . . O13 Si6 O6 111.9(5) . . O24 Si6 O6 111.3(6) . . O14 Si7 O15 111.8(6) . . O14 Si7 O22 107.5(6) . . O15 Si7 O22 111.3(6) . . O14 Si7 O17 108.8(6) . . O15 Si7 O17 109.3(6) . . O22 Si7 O17 108.0(6) . . O21 Si8 O14 108.0(6) . . O21 Si8 O3 108.7(6) . 2_565 O14 Si8 O3 113.3(6) . 2_565 O21 Si8 O7 106.3(5) . 2_565 O14 Si8 O7 110.5(5) . 2_565 O3 Si8 O7 109.7(5) 2_565 2_565 O10 Si9 O2 112.3(8) . 2_565 O10 Si9 O22 103.6(6) . . O2 Si9 O22 112.5(6) 2_565 . O10 Si9 O5 109.8(6) . . O2 Si9 O5 109.9(5) 2_565 . O22 Si9 O5 108.5(5) . . O26 Si10 O17 107.9(8) . . O26 Si10 O16 108.8(7) . . O17 Si10 O16 110.0(6) . . O26 Si10 O3 108.7(7) . . O17 Si10 O3 110.6(6) . . O16 Si10 O3 110.7(7) . . O20 Si11 O25 108.4(6) . . O20 Si11 O19 106.4(5) . 2_564 O25 Si11 O19 109.6(6) . 2_564 O20 Si11 O15 110.3(6) . 2_564 O25 Si11 O15 112.8(6) . 2_564 O19 Si11 O15 109.2(6) 2_564 2_564 O26 Si12 O23 108.4(7) . . O26 Si12 O2 106.0(7) . . O23 Si12 O2 112.9(6) . . O26 Si12 O11 109.5(8) . . O23 Si12 O11 107.6(6) . . O2 Si12 O11 112.4(5) . . Si4 O1 Si1 150.2(6) 6_656 . Si9 O2 Si12 167.8(7) 2_564 . Si8 O3 Si10 160.4(8) 2_564 . Si5 O4 Si1 161.8(8) . . Si9 O5 Si5 151.3(6) . 2_565 Si2 O6 Si6 156.8(8) . . Si1 O7 Si8 147.2(6) . 2_564 Si6 O8 Si6 142.3(10) . 7_575 Si5 O9 Si3 152.2(6) . 6_656 Si9 O10 Si9 147.8(10) 7_565 . Si2 O11 Si12 152.8(6) . . Si2 O12 Si2 146.6(7) . 7_575 Si4 O13 Si6 146.8(6) 2_565 . Si7 O14 Si8 158.2(7) . . Si7 O15 Si11 174.8(9) . 2_565 Si4 O16 Si10 155.7(8) . . Si10 O17 Si7 153.4(7) . . Si3 O18 Si3 150.9(10) 7_575 . Si11 O19 Si1 155.3(7) 2_565 . Si11 O20 Si3 143.1(7) . . Si8 O21 Si2 143.5(5) . . Si7 O22 Si9 144.1(7) . . Si12 O23 Si3 157.9(7) . . Si5 O24 Si6 164.5(9) . . Si4 O25 Si11 158.8(7) . . Si10 O26 Si12 177.3(12) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 O4 1.598(10) . Si1 O7 1.614(7) . Si1 O19 1.631(8) . Si1 O1 1.646(7) . Si2 O12 1.572(6) . Si2 O6 1.615(7) . Si2 O11 1.611(9) . Si2 O21 1.628(8) . Si3 O18 1.606(6) . Si3 O20 1.620(9) . Si3 O9 1.631(7) 6_556 Si3 O23 1.633(8) . Si4 O25 1.596(9) . Si4 O13 1.610(9) 2_564 Si4 O16 1.596(8) . Si4 O1 1.620(7) 6_556 Si5 O4 1.583(10) . Si5 O9 1.593(7) . Si5 O24 1.597(9) . Si5 O5 1.628(8) 2_564 Si6 O8 1.589(7) . Si6 O13 1.599(8) . Si6 O24 1.627(9) . Si6 O6 1.635(7) . Si7 O14 1.569(9) . Si7 O15 1.604(7) . Si7 O22 1.619(9) . Si7 O17 1.651(9) . Si8 O21 1.617(9) . Si8 O14 1.606(10) . Si8 O3 1.611(9) 2_565 Si8 O7 1.629(7) 2_565 Si9 O10 1.582(7) . Si9 O2 1.601(8) 2_565 Si9 O22 1.612(10) . Si9 O5 1.621(7) . Si10 O26 1.568(11) . Si10 O17 1.609(10) . Si10 O16 1.614(8) . Si10 O3 1.623(8) . Si11 O20 1.582(10) . Si11 O25 1.606(9) . Si11 O19 1.621(8) 2_564 Si11 O15 1.630(8) 2_564 Si12 O26 1.595(11) . Si12 O23 1.593(8) . Si12 O2 1.613(8) . Si12 O11 1.628(9) . O1 Si4 1.620(7) 6_656 O2 Si9 1.601(8) 2_564 O3 Si8 1.611(9) 2_564 O5 Si5 1.628(8) 2_565 O7 Si8 1.629(7) 2_564 O8 Si6 1.589(7) 7_575 O9 Si3 1.632(7) 6_656 O10 Si9 1.582(7) 7_565 O12 Si2 1.572(6) 7_575 O13 Si4 1.610(9) 2_565 O15 Si11 1.630(8) 2_565 O18 Si3 1.606(6) 7_575 O19 Si11 1.621(8) 2_565