#------------------------------------------------------------------------------ #$Date: 2025-02-11 05:41:48 +0200 (Tue, 11 Feb 2025) $ #$Revision: 297679 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573875.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_1573875 loop_ _publ_author_name 'Vlahakis, Niko' 'Clauss, Arden' 'Rodriguez, Jose A.' _publ_section_title ; Accounting for electron-beam-induced warping of molecular nanocrystals in MicroED structure determination. ; _journal_coeditor_code NF5001SUP1 _journal_issue 2 _journal_name_full IUCrJ _journal_paper_doi 10.1107/S2052252524012132 _journal_volume 12 _journal_year 2025 _chemical_absolute_configuration rm _chemical_formula_sum 'C20 H40 N4 O8 S4 Zn2' _chemical_formula_weight 723.60 _chemical_name_common Zn(II)-methionine _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2024-04-12 # Formatted by publCIF ; _cell_angle_alpha 90 _cell_angle_beta 106.94(5) _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 9.070(2) _cell_length_b 4.9100(19) _cell_length_c 14.970(3) _cell_measurement_reflns_used 13658 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 0.918 _cell_measurement_theta_min 0.083 _cell_volume 637.7(4) _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.842 _diffrn_measured_fraction_theta_max 0.832 _diffrn_measurement_device_type TEM _diffrn_radiation_type Electron _diffrn_radiation_wavelength 0.0251 _diffrn_reflns_av_R_equivalents 0.2219 _diffrn_reflns_av_unetI/netI 0.1765 _diffrn_reflns_Laue_measured_fraction_full 0.842 _diffrn_reflns_Laue_measured_fraction_max 0.832 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13658 _diffrn_reflns_point_group_measured_fraction_full 0.860 _diffrn_reflns_point_group_measured_fraction_max 0.845 _diffrn_reflns_theta_full 0.863 _diffrn_reflns_theta_max 0.918 _diffrn_reflns_theta_min 0.083 _diffrn_source FEG _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.884 _exptl_crystal_description Plate _exptl_crystal_F_000 129 _refine_diff_density_max 0.206 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.063 _refine_ls_abs_structure_details ; All f" are zero, so absolute structure could not be determined ; _refine_ls_extinction_coef 15704(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2019/2 (Sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.404 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 175 _refine_ls_number_reflns 2345 _refine_ls_number_restraints 280 _refine_ls_restrained_S_all 1.363 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_gt 0.1482 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 _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 0.3730 _refine_ls_wR_factor_ref 0.3815 _reflns_Friedel_coverage 0.812 _reflns_Friedel_fraction_full 0.882 _reflns_Friedel_fraction_max 0.861 _reflns_number_gt 1823 _reflns_number_total 2345 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nf5001.cif _cod_data_source_block ZnIImethionine _cod_original_cell_volume 637.8(4) _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 1573875 _shelx_shelxl_version_number 2019/3 _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_res_file ; TITL znmet_cryo_apollo_merge01_a.res in P2(1) a.res created by SHELXL-2019/3 at 10:50:03 on 12-Apr-2024 REM Old TITL GGYMLG in space group P 1 21 1 . REM SHELXT solution in P2(1): R1 0.256, Rweak 0.250, Alpha 0.123 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = -0.746 ( 0.149 ) from 735 Parsons' quotients REM Formula found by SHELXT: C9 N3 O7 S CELL 0.02510 9.0700 4.9100 14.9700 90.000 106.936 90.000 ZERR 1.000 0.0020 0.0019 0.0033 0.000 0.0500 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C 0.600 40.938 0.136 0.374 0.547 3.278 1.225 13.013 0 0 0 0 0.76 12.011 SFAC N 0.482 31.526 0.135 0.324 0.519 2.607 1.075 10.017 0 0 0 0 0.71 14.007 SFAC O 0.392 25.675 0.144 0.306 0.511 2.272 0.937 8.270 0 0 0 0 0.66 15.999 SFAC S 1.390 40.169 0.348 0.365 0.915 2.890 2.506 13.043 0 0 0 0 1.05 32.065 SFAC Zn 1.665 60.120 0.600 0.360 1.776 2.769 2.018 15.492 0 0 0 0 1.22 65.39 SFAC H 0.129 37.737 0.036 0.553 0.127 3.772 0.236 13.518 0 0 0 0 0.31 1.008 UNIT 20 4 8 4 2 40 L.S. 1 ACTA RIGU 0.004 SIMU 0.005 BOND LIST 4 FMAP 2 PLAN 20 TEMP -173 SADI 0.0001 C1 C2 C2 C3 C3 C4 C6 C7 C7 C8 C8 C9 WGHT 0.200000 EXTI15703.725586 FVAR 7.84726 ZN1 5 0.768228 0.359835 0.517554 11.00000 0.03879 0.02788 = 0.06813 0.00670 0.02385 0.01231 S1 4 0.858465 0.672699 0.889318 11.00000 0.03849 0.04106 = 0.09301 -0.01226 0.01525 -0.00269 S2 4 0.617826 0.583312 0.151047 11.00000 0.04504 0.03179 = 0.08179 0.00389 0.01223 0.00214 O4 3 1.052499 0.097720 0.389389 11.00000 0.01831 0.01415 = 0.07430 0.00184 0.02178 0.00791 O1 3 0.598230 0.579299 0.537021 11.00000 0.03099 0.02323 = 0.07182 0.00668 0.02104 0.00125 C6 1 0.942957 0.178604 0.409891 11.00000 0.01723 0.01255 = 0.07145 0.00506 0.01863 0.00840 N2 2 0.775838 0.549105 0.400822 11.00000 0.02730 0.01996 = 0.06763 0.00496 0.02032 0.00448 AFIX 23 H6A 6 0.679136 0.598200 0.366595 11.00000 -1.20000 H6B 6 0.834424 0.702306 0.415317 11.00000 -1.20000 AFIX 0 O3 3 0.913857 0.107464 0.481058 11.00000 0.02461 0.02243 = 0.07071 0.00787 0.01669 0.00611 C1 1 0.549753 0.479361 0.599039 11.00000 0.02356 0.02014 = 0.07577 0.00189 0.02357 -0.00404 O2 3 0.426175 0.559996 0.613503 11.00000 0.03065 0.02356 = 0.09019 0.00866 0.03228 -0.00028 C9 1 0.804914 0.707508 0.219050 11.00000 0.03784 0.03118 = 0.07646 0.00778 0.01566 0.00137 AFIX 23 H9A 6 0.861657 0.767946 0.175223 11.00000 -1.20000 H9B 6 0.788821 0.869875 0.254294 11.00000 -1.20000 AFIX 0 C7 1 0.838199 0.374932 0.350717 11.00000 0.02093 0.02352 = 0.07005 0.00722 0.01801 0.00223 AFIX 13 H7 6 0.749924 0.265524 0.311541 11.00000 -1.20000 AFIX 0 N1 2 0.705437 0.104314 0.601882 11.00000 0.02505 0.01841 = 0.07496 0.00056 0.02227 -0.00195 AFIX 23 H1A 6 0.638014 -0.020748 0.567948 11.00000 -1.20000 H1B 6 0.789300 0.014558 0.638268 11.00000 -1.20000 AFIX 0 C8 1 0.902467 0.516690 0.284995 11.00000 0.03189 0.02683 = 0.07119 0.00690 0.01754 -0.00293 AFIX 23 H8A 6 0.938331 0.376996 0.248405 11.00000 -1.20000 H8B 6 0.994734 0.617539 0.321761 11.00000 -1.20000 AFIX 0 C5 1 0.774245 0.902392 0.943538 11.00000 0.04305 0.04046 = 0.09610 -0.02262 0.00660 -0.01175 AFIX 137 H5A 6 0.851585 0.975857 0.998365 11.00000 -1.50000 H5B 6 0.692277 0.812993 0.963257 11.00000 -1.50000 H5C 6 0.730200 1.051071 0.900327 11.00000 -1.50000 AFIX 0 C10 1 0.681678 0.338311 0.082397 11.00000 0.05980 0.02264 = 0.09072 -0.00488 0.00933 -0.00783 AFIX 137 H10A 6 0.592270 0.258891 0.036259 11.00000 -1.50000 H10B 6 0.739429 0.194154 0.123079 11.00000 -1.50000 H10C 6 0.748395 0.427360 0.050159 11.00000 -1.50000 AFIX 0 C2 1 0.631373 0.264362 0.661170 11.00000 0.02271 0.02042 = 0.07805 0.00060 0.02565 -0.00752 AFIX 13 H2 6 0.557683 0.148726 0.682799 11.00000 -1.20000 AFIX 0 C4 1 0.696619 0.558612 0.802563 11.00000 0.03393 0.03684 = 0.08777 -0.01078 0.01834 -0.00601 AFIX 23 H4A 6 0.626694 0.459056 0.831022 11.00000 -1.20000 H4 6 0.639803 0.715254 0.767051 11.00000 -1.20000 AFIX 0 C3 1 0.749034 0.378740 0.740505 11.00000 0.03667 0.03210 = 0.08360 -0.00372 0.01926 -0.01076 AFIX 23 H3A 6 0.823105 0.481121 0.716125 11.00000 -1.20000 H3B 6 0.806137 0.225846 0.778211 11.00000 -1.20000 AFIX 0 HKLF 4 REM znmet_cryo_apollo_merge01_a.res in P2(1) REM wR2 = 0.3815, GooF = S = 1.404, Restrained GooF = 1.363 for all data REM R1 = 0.1482 for 1823 Fo > 4sig(Fo) and 0.1684 for all 2345 data REM 175 parameters refined using 280 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.206, deepest hole -0.261, 1-sigma level 0.063 Q1 1 0.5171 0.3748 0.0663 11.00000 0.05 0.21 Q2 1 0.5624 -0.0062 0.5690 11.00000 0.05 0.20 Q3 1 0.7395 0.0465 0.7346 11.00000 0.05 0.19 Q4 1 0.9740 0.6844 0.4496 11.00000 0.05 0.18 Q5 1 0.7954 0.8573 0.3931 11.00000 0.05 0.18 Q6 1 0.8906 0.8990 0.2013 11.00000 0.05 0.18 Q7 1 0.6934 0.2765 0.4756 11.00000 0.05 0.18 Q8 1 0.2763 0.4678 0.6350 11.00000 0.05 0.18 Q9 1 0.8953 0.3937 0.0809 11.00000 0.05 0.16 Q10 1 1.0225 1.0096 0.9502 11.00000 0.05 0.16 Q11 1 0.8728 0.0644 0.7338 11.00000 0.05 0.16 Q12 1 1.0392 0.7610 1.0846 11.00000 0.05 0.16 Q13 1 0.8282 -0.0963 0.6911 11.00000 0.05 0.15 Q14 1 0.8591 -0.0241 0.7160 11.00000 0.05 0.15 Q15 1 0.5705 0.4174 0.3212 11.00000 0.05 0.15 Q16 1 0.6146 0.9950 0.7880 11.00000 0.05 0.15 Q17 1 0.8903 0.6959 0.4553 11.00000 0.05 0.15 Q18 1 0.6577 1.1104 0.8968 11.00000 0.05 0.15 Q19 1 0.6098 0.6519 0.2845 11.00000 0.05 0.14 Q20 1 0.6351 0.0971 0.4921 11.00000 0.05 0.14 ; _shelx_res_checksum 90778 _shelx_hkl_file ; 0 -1 1 1082.57 238.64 0 -1 1 1440.04 371.18 0 -1 1 1107.51 231.53 0 -1 -1 1470.06 379.22 0 -1 -1 1034.08 232.45 0 -1 -1 969.88 200.72 0 1 1 811.47 171.76 0 1 1 1119.06 249.96 0 1 1 1362.92 351.84 0 1 -1 1109.82 243.86 0 1 -1 1016.53 213.05 0 1 -1 1610.92 413.45 0 -1 2 2284.76 493.25 0 -1 2 2038.60 520.04 0 -1 2 1909.28 409.11 0 -1 -2 2881.92 739.88 0 -1 -2 2482.89 489.56 0 -1 -2 2050.61 454.68 0 1 2 3244.48 701.08 0 1 2 2014.12 404.86 0 1 2 2539.70 652.13 0 1 -2 1946.23 422.78 0 1 -2 2360.97 599.48 0 1 -2 2050.14 432.89 0 -1 -3 8562.65 1843.24 0 -1 -3 3446.31 907.53 0 1 3 8197.80 1773.95 0 1 3 2599.74 702.93 0 -1 -4 7976.11 1791.04 0 -1 -4 6558.23 1682.51 0 1 4 5523.69 1310.72 0 1 4 5782.33 1489.92 0 -1 -5 304.63 403.61 0 -2 0 3524.36 753.28 0 -2 0 3723.88 704.78 0 -2 0 4272.56 962.49 0 -2 0 3602.87 953.72 0 -2 0 3329.46 840.57 0 2 0 3871.67 975.42 0 2 0 3208.45 687.23 0 2 0 4316.42 1142.61 0 2 0 5320.48 1198.03 0 2 0 4341.37 821.17 0 -2 1 2315.24 451.28 0 -2 1 2550.79 647.51 0 -2 1 2204.86 475.24 0 -2 1 1821.99 484.48 0 -2 -1 2385.90 606.41 0 -2 -1 2213.63 598.55 0 -2 -1 2264.90 434.46 0 -2 -1 1670.50 386.80 0 -2 -1 1837.23 398.80 0 2 1 1846.01 471.54 0 2 1 1631.71 379.50 0 2 1 2042.29 393.63 0 2 1 1873.25 407.17 0 2 -1 1542.11 337.24 0 2 -1 1472.37 392.06 0 2 -1 2469.97 478.93 0 2 -1 2219.18 564.37 0 -2 2 762.04 209.13 0 -2 2 428.60 105.30 0 -2 2 443.33 117.13 0 -2 -2 323.30 108.40 0 -2 -2 544.06 124.89 0 -2 -2 265.97 79.30 0 2 2 311.61 90.85 0 2 2 381.16 95.00 0 2 2 283.20 97.96 0 2 -2 330.41 85.81 0 2 -2 507.57 146.09 0 2 -2 392.15 105.16 0 -2 3 2108.33 538.98 0 -2 3 1975.32 430.35 0 -2 -3 1648.34 430.08 0 -2 -3 991.58 231.25 0 -2 -3 1191.56 253.69 0 2 3 1109.82 256.37 0 2 3 1643.72 428.14 0 2 3 1122.29 236.52 0 2 -3 2095.86 454.82 0 2 -3 1821.53 410.81 0 2 -3 2214.10 564.37 0 -2 4 3013.09 649.82 0 -2 4 3864.74 976.34 0 -2 4 4733.94 945.41 0 -2 -4 5228.11 1328.74 0 -2 -4 4114.60 794.84 0 -2 -4 4430.96 960.18 0 2 4 4237.91 915.38 0 2 4 3957.57 766.20 0 2 4 5325.10 1349.98 0 2 -4 3407.97 731.57 0 2 -4 3783.46 955.11 0 2 -4 4594.00 926.01 0 -2 5 1816.45 419.50 0 -2 -5 4094.74 1066.40 0 -2 -5 4083.66 883.05 0 -2 -5 2592.35 512.19 0 2 5 3909.07 857.66 0 2 5 2991.84 782.37 0 2 5 2646.85 524.20 0 2 -5 2398.37 526.97 0 -2 -6 1405.40 375.25 0 -2 -6 621.65 293.83 0 2 6 1779.96 486.79 0 2 6 895.52 406.33 0 -2 -7 3350.71 912.15 0 -2 -7 2454.72 688.15 0 2 7 5066.47 1287.63 0 2 7 3129.94 880.28 0 -2 -8 164.09 359.41 0 -2 -8 68.08 286.62 0 2 8 432.15 440.10 0 2 8 293.27 298.26 0 -2 -9 421.16 432.48 0 2 9 1000.82 469.70 0 2 9 1657.11 527.43 0 -2 -10 89.18 338.31 0 -3 1 176.24 55.51 0 -3 1 360.01 106.09 0 -3 1 73.99 36.49 0 -3 1 127.10 34.64 0 -3 1 84.98 30.04 0 -3 -1 73.90 34.92 0 -3 -1 85.16 54.78 0 -3 -1 124.05 49.42 0 -3 -1 44.31 36.01 0 3 1 102.62 53.39 0 3 1 180.53 67.48 0 3 1 269.85 142.58 0 3 1 220.49 68.91 0 3 1 187.28 52.74 0 3 -1 102.58 44.62 0 3 -1 199.84 58.19 0 3 -1 327.50 96.71 0 -3 2 655.37 149.09 0 -3 2 586.08 134.45 0 -3 2 641.05 173.70 0 -3 -2 827.63 168.76 0 -3 -2 942.63 248.89 0 -3 -2 228.06 434.32 0 -3 -2 590.70 139.44 0 -3 -2 770.82 204.37 0 3 2 506.19 124.75 0 3 2 783.75 208.43 0 3 2 1083.95 215.92 0 3 2 368.14 128.12 0 3 2 -267.91 849.80 0 3 -2 808.23 184.60 0 3 -2 735.73 158.46 0 3 -2 1601.22 408.14 0 -3 3 83.27 34.53 0 -3 3 126.64 60.64 0 -3 3 109.64 62.58 0 -3 -3 66.23 61.66 0 -3 -3 48.86 42.62 0 -3 -3 300.06 76.90 0 3 3 93.02 41.30 0 3 3 106.36 53.07 0 3 3 87.80 52.79 0 3 -3 111.77 41.71 0 3 -3 175.45 62.67 0 3 -3 205.11 75.28 0 -3 4 291.89 86.41 0 -3 4 246.68 67.66 0 -3 4 490.48 127.43 0 -3 -4 539.90 158.13 0 -3 -4 337.71 93.06 0 -3 -4 179.66 71.08 0 3 4 205.48 70.34 0 3 4 249.45 67.80 0 3 -4 287.64 77.08 0 3 -4 368.18 104.70 0 3 -4 192.68 89.28 0 -3 5 364.07 105.30 0 -3 5 556.52 130.71 0 -3 5 469.70 153.61 0 -3 -5 141.56 102.76 0 -3 -5 273.60 87.10 0 -3 -5 311.19 96.34 0 3 5 259.97 94.03 0 3 5 318.35 94.26 0 3 5 164.88 96.06 0 3 -5 495.56 118.65 0 3 -5 428.37 165.01 0 -3 6 1285.78 331.06 0 -3 6 1430.81 312.67 0 -3 6 1874.17 425.83 0 -3 -6 2402.07 630.89 0 -3 -6 1029.46 250.74 0 -3 -6 1620.62 330.22 0 3 6 1436.35 297.89 0 3 6 1762.88 402.50 0 3 6 2205.78 574.54 0 3 -6 1235.91 271.66 0 3 -6 2006.26 442.78 0 3 -6 1485.30 377.00 0 -3 7 546.37 153.28 0 -3 7 377.42 167.65 0 -3 -7 438.07 209.96 0 -3 -7 196.52 78.93 0 3 7 226.95 89.74 0 3 7 1334.28 363.93 0 3 -7 506.19 179.19 0 -3 -8 1465.44 340.11 0 -3 -8 1615.54 477.55 0 3 8 1445.12 355.39 0 3 8 1360.61 388.00 0 -3 -9 139.25 119.85 0 -3 -9 514.50 249.36 0 3 9 285.56 172.22 0 3 9 1595.22 486.79 0 -3 -10 20.62 124.61 0 -3 -10 95.74 179.75 0 3 10 22.64 141.93 0 3 10 194.67 270.55 0 -3 -11 70.57 135.00 0 -3 -11 -0.97 228.02 0 3 11 139.16 152.22 0 3 11 -8.91 278.54 0 -3 -12 0.56 113.62 0 -3 -12 103.87 203.21 0 3 12 4.91 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29.31 11 0 -8 46.74 30.72 11 0 -8 76.53 40.84 11 0 -8 38.14 15.48 11 0 -8 31.96 54.45 -11 0 8 71.08 97.27 -11 0 8 39.52 81.79 -11 0 8 56.58 31.25 -11 0 8 66.60 19.04 11 0 -7 32.08 32.98 11 0 -7 48.91 20.62 11 0 -7 32.85 14.94 11 0 -7 -25.16 62.49 -11 0 7 43.79 26.44 -11 0 7 21.67 68.72 -11 0 7 32.11 24.58 11 0 -6 186.91 48.77 11 0 -6 174.25 39.08 11 0 -6 239.52 61.43 11 0 -6 184.74 74.36 11 0 -6 260.80 65.77 -11 0 6 193.61 42.74 -11 0 6 177.21 46.83 -11 0 6 193.79 94.96 -11 0 6 166.35 43.69 11 0 -5 47.48 22.50 11 0 -5 40.92 21.48 11 0 -5 15.13 45.05 11 0 -5 79.62 26.52 -11 0 5 16.07 20.81 -11 0 5 55.98 14.72 -11 0 5 63.09 76.34 -11 0 5 44.37 22.18 11 0 -4 6.31 13.95 11 0 -4 174.07 63.60 11 0 -4 47.06 19.93 11 0 -4 35.31 38.40 -11 0 4 7.08 25.76 -11 0 4 33.72 10.29 -11 0 4 15.50 53.02 -11 0 4 10.47 13.66 11 0 -3 140.96 33.81 11 0 -3 45.83 44.76 11 0 -3 78.01 28.27 11 0 -3 231.34 76.20 -11 0 3 0.08 46.06 -11 0 3 206.72 80.08 -11 0 3 168.02 37.60 11 0 -2 350.78 70.71 11 0 -2 87.66 80.82 11 0 -2 248.89 64.43 11 0 -2 394.00 116.53 -11 0 2 90.34 56.25 -11 0 2 414.92 127.10 -11 0 2 338.17 69.37 11 0 -1 15.00 45.97 11 0 -1 35.63 13.69 11 0 -1 30.52 34.02 -11 0 1 43.03 59.67 -11 0 1 48.68 16.51 11 0 0 18.36 33.41 -11 0 0 32.99 61.15 11 -1 -10 56.67 41.36 11 -1 -10 22.29 78.75 11 1 -10 9.24 82.30 -11 1 10 11.92 40.70 11 -1 -9 34.74 15.13 11 -1 -9 44.85 32.79 11 -1 -9 47.85 32.29 11 -1 -9 21.78 69.74 -11 -1 9 24.88 30.81 -11 -1 9 31.80 13.93 -11 -1 9 4.73 119.44 -11 -1 9 33.45 18.32 11 1 -9 26.99 12.70 11 1 -9 42.79 14.38 11 1 -9 18.12 72.23 11 1 -9 35.29 36.95 -11 1 9 73.66 36.87 -11 1 9 20.83 23.52 11 -1 -8 23.24 12.74 11 -1 -8 46.06 33.53 11 -1 -8 58.42 58.79 -11 -1 8 74.03 22.70 -11 -1 8 57.36 36.28 -11 -1 8 19.62 79.35 -11 -1 8 56.21 20.20 11 1 -8 26.27 14.53 11 1 -8 96.99 44.49 11 1 -8 86.69 24.79 11 1 -8 25.34 55.74 -11 1 8 51.50 21.42 -11 1 8 16.98 6.84 -11 1 8 50.71 26.87 11 -1 -7 33.28 25.89 11 -1 -7 44.27 16.89 11 -1 -7 57.78 53.76 11 -1 -7 87.98 22.73 -11 -1 7 78.38 37.59 -11 -1 7 48.68 18.03 -11 -1 7 91.95 27.45 -11 -1 7 28.46 69.37 11 1 -7 74.08 66.60 11 1 -7 77.54 24.14 11 1 -7 105.67 30.59 11 1 -7 104.42 38.39 -11 1 7 64.01 22.62 -11 1 7 84.43 30.76 -11 1 7 41.71 11.85 11 -1 -6 95.28 30.87 11 -1 -6 47.71 21.73 11 -1 -6 29.52 54.08 -11 -1 6 32.31 17.82 -11 -1 6 55.84 28.51 -11 -1 6 3.71 61.98 -11 -1 6 51.31 19.45 11 1 -6 47.57 20.34 11 1 -6 53.76 31.87 11 1 -6 51.77 52.47 11 1 -6 103.08 31.96 -11 1 6 69.97 20.00 -11 1 6 62.67 25.47 11 -1 -5 64.38 25.27 11 -1 -5 29.34 18.84 11 -1 -5 48.91 16.93 11 -1 -5 9.87 47.20 -11 -1 5 42.72 24.21 -11 -1 5 27.48 23.98 -11 -1 5 -11.08 65.40 -11 -1 5 37.63 16.78 11 1 -5 32.16 20.26 11 1 -5 -6.12 43.97 11 1 -5 32.95 17.27 11 1 -5 83.36 32.21 -11 1 5 17.06 8.97 -11 1 5 17.88 14.72 -11 1 5 69.79 24.20 11 -1 -4 20.53 19.20 11 -1 -4 56.76 21.29 11 -1 -4 -13.40 38.73 -11 -1 4 14.80 29.59 -11 -1 4 27.13 18.68 -11 -1 4 70.89 46.69 -11 -1 4 2.29 49.97 -11 -1 4 37.91 17.19 11 1 -4 92.42 35.96 11 1 -4 52.56 22.92 11 1 -4 44.48 39.44 11 1 -4 74.50 23.93 -11 1 4 32.15 12.03 -11 1 4 93.11 26.30 -11 1 4 53.94 46.65 11 -1 -3 32.68 17.55 11 -1 -3 84.84 23.65 11 -1 -3 76.34 19.46 11 -1 -3 78.84 46.79 -11 -1 3 51.22 18.34 -11 -1 3 52.37 37.35 -11 -1 3 98.23 52.23 -11 -1 3 50.06 20.02 11 1 -3 130.15 59.58 11 1 -3 86.50 46.10 11 1 -3 48.31 22.83 11 1 -3 44.43 16.13 -11 1 3 36.64 12.36 -11 1 3 89.18 24.93 -11 1 3 172.36 61.19 11 -1 -2 25.78 20.97 11 -1 -2 51.27 16.55 11 -1 -2 32.50 14.22 11 -1 -2 -1.01 34.55 -11 -1 2 45.30 15.02 -11 -1 2 59.16 48.08 -11 -1 2 78.24 44.49 -11 -1 2 59.76 22.76 11 1 -2 46.88 45.75 11 1 -2 40.26 35.53 11 1 -2 10.23 18.38 11 1 -2 35.96 13.77 -11 1 2 67.34 18.90 -11 1 2 49.19 17.48 11 -1 -1 38.69 39.25 -11 -1 1 -6.18 64.61 11 1 -1 54.82 38.61 11 1 -1 75.14 44.54 -11 1 1 8.64 11.65 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 88131 _publcif_funding_html ; ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Zn1 Zn 0.7682(5) 0.3598(13) 0.5176(5) 0.0432(13) Uani 1 1 d . U . . . S1 S 0.8585(9) 0.6727(19) 0.8893(11) 0.058(3) Uani 1 1 d . U . . . S2 S 0.6178(9) 0.5833(17) 0.1510(10) 0.054(3) Uani 1 1 d . U . . . O4 O 1.0525(10) 0.0977(19) 0.3894(11) 0.034(2) Uani 1 1 d . U . . . O1 O 0.5982(12) 0.579(2) 0.5370(13) 0.041(2) Uani 1 1 d . U . . . C6 C 0.9430(7) 0.1786(9) 0.4099(5) 0.033(2) Uani 1 1 d D U . . . N2 N 0.7758(13) 0.549(2) 0.4008(14) 0.037(2) Uani 1 1 d . U . . . H6A H 0.679136 0.598200 0.366595 0.044 Uiso 1 1 calc R U . . . H6B H 0.834424 0.702306 0.415317 0.044 Uiso 1 1 calc R U . . . O3 O 0.9139(11) 0.107(2) 0.4811(13) 0.039(2) Uani 1 1 d . U . . . C1 C 0.5498(9) 0.4794(9) 0.5990(5) 0.038(2) Uani 1 1 d D U . . . O2 O 0.4262(12) 0.560(2) 0.6135(14) 0.045(3) Uani 1 1 d . U . . . C9 C 0.8049(8) 0.7075(10) 0.2190(5) 0.049(3) Uani 1 1 d D U . . . H9A H 0.861657 0.767946 0.175223 0.058 Uiso 1 1 calc R U . . . H9B H 0.788821 0.869875 0.254294 0.058 Uiso 1 1 calc R U . . . C7 C 0.8382(5) 0.3749(7) 0.3507(2) 0.037(2) Uani 1 1 d D U . . . H7 H 0.749924 0.265524 0.311541 0.045 Uiso 1 1 calc R U . . . N1 N 0.7054(12) 0.104(2) 0.6019(13) 0.038(2) Uani 1 1 d . U . . . H1A H 0.638014 -0.020748 0.567948 0.045 Uiso 1 1 calc R U . . . H1B H 0.789300 0.014558 0.638268 0.045 Uiso 1 1 calc R U . . . C8 C 0.9025(6) 0.5167(7) 0.2850(2) 0.043(3) Uani 1 1 d D U . . . H8A H 0.938331 0.376996 0.248405 0.051 Uiso 1 1 calc R U . . . H8B H 0.994734 0.617539 0.321761 0.051 Uiso 1 1 calc R U . . . C5 C 0.774(2) 0.902(4) 0.944(2) 0.063(5) Uani 1 1 d . U . . . H5A H 0.851585 0.975857 0.998365 0.094 Uiso 1 1 calc R U . . . H5B H 0.692277 0.812993 0.963257 0.094 Uiso 1 1 calc R U . . . H5C H 0.730200 1.051071 0.900327 0.094 Uiso 1 1 calc R U . . . C10 C 0.682(2) 0.338(3) 0.082(2) 0.060(5) Uani 1 1 d . U . . . H10A H 0.592270 0.258891 0.036259 0.091 Uiso 1 1 calc R U . . . H10B H 0.739429 0.194154 0.123079 0.091 Uiso 1 1 calc R U . . . H10C H 0.748395 0.427360 0.050159 0.091 Uiso 1 1 calc R U . . . C2 C 0.6314(5) 0.2644(8) 0.6612(3) 0.038(2) Uani 1 1 d D U . . . H2 H 0.557683 0.148726 0.682799 0.046 Uiso 1 1 calc R U . . . C4 C 0.6966(7) 0.5586(11) 0.8026(3) 0.053(3) Uani 1 1 d D U . . . H4A H 0.626694 0.459056 0.831022 0.063 Uiso 1 1 calc R U . . . H4 H 0.639803 0.715254 0.767051 0.063 Uiso 1 1 calc R U . . . C3 C 0.7490(6) 0.3787(8) 0.7405(2) 0.050(3) Uani 1 1 d D U . . . H3A H 0.823105 0.481121 0.716125 0.061 Uiso 1 1 calc R U . . . H3B H 0.806137 0.225846 0.778211 0.061 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0388(17) 0.0279(14) 0.068(4) 0.0067(19) 0.0238(19) 0.0123(14) S1 0.038(3) 0.041(3) 0.093(8) -0.012(4) 0.015(4) -0.003(3) S2 0.045(3) 0.032(3) 0.082(8) 0.004(4) 0.012(4) 0.002(3) O4 0.018(3) 0.014(3) 0.074(7) 0.002(4) 0.022(4) 0.008(3) O1 0.031(3) 0.023(3) 0.072(6) 0.007(4) 0.021(4) 0.001(3) C6 0.017(3) 0.013(3) 0.071(6) 0.005(3) 0.019(3) 0.008(3) N2 0.027(3) 0.020(3) 0.068(6) 0.005(4) 0.020(4) 0.004(3) O3 0.025(3) 0.022(3) 0.071(5) 0.008(4) 0.017(3) 0.006(3) C1 0.024(4) 0.020(3) 0.076(6) 0.002(4) 0.024(4) -0.004(3) O2 0.031(4) 0.024(4) 0.090(11) 0.009(5) 0.032(5) 0.000(3) C9 0.038(4) 0.031(4) 0.076(8) 0.008(5) 0.016(5) 0.001(4) C7 0.021(3) 0.024(3) 0.070(6) 0.007(4) 0.018(4) 0.002(3) N1 0.025(3) 0.018(3) 0.075(6) 0.001(4) 0.022(4) -0.002(3) C8 0.032(4) 0.027(4) 0.071(7) 0.007(4) 0.018(4) -0.003(4) C5 0.043(7) 0.040(7) 0.096(14) -0.023(8) 0.007(8) -0.012(6) C10 0.060(8) 0.023(5) 0.091(13) -0.005(7) 0.009(8) -0.008(5) C2 0.023(3) 0.020(3) 0.078(6) 0.001(4) 0.026(4) -0.008(3) C4 0.034(4) 0.037(4) 0.088(8) -0.011(5) 0.018(5) -0.006(4) C3 0.037(4) 0.032(4) 0.084(7) -0.004(5) 0.019(5) -0.011(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.0000 0.0000 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N1 82.5(5) . . ? O1 Zn1 N2 95.9(6) . . ? N1 Zn1 N2 160.6(7) . . ? O1 Zn1 O3 170.6(7) . . ? N1 Zn1 O3 96.7(5) . . ? N2 Zn1 O3 81.7(6) . . ? O1 Zn1 O4 94.8(5) . 2_756 ? N1 Zn1 O4 103.6(7) . 2_756 ? N2 Zn1 O4 95.8(6) . 2_756 ? O3 Zn1 O4 94.5(5) . 2_756 ? C5 S1 C4 99.9(9) . . ? C10 S2 C9 98.2(8) . . ? C6 O4 Zn1 123.0(11) . 2_746 ? C1 O1 Zn1 111.0(8) . . ? O4 C6 O3 122.6(9) . . ? O4 C6 C7 120.6(9) . . ? O3 C6 C7 116.8(7) . . ? C7 N2 Zn1 108.3(7) . . ? C6 O3 Zn1 112.9(7) . . ? O1 C1 O2 122.0(9) . . ? O1 C1 C2 122.7(8) . . ? O2 C1 C2 115.3(9) . . ? C8 C9 S2 116.6(5) . . ? N2 C7 C8 112.5(6) . . ? N2 C7 C6 112.4(8) . . ? C8 C7 C6 114.1(5) . . ? C2 N1 Zn1 108.1(6) . . ? C7 C8 C9 118.7(5) . . ? C1 C2 C3 110.8(4) . . ? C1 C2 N1 103.6(7) . . ? C3 C2 N1 109.8(6) . . ? C3 C4 S1 108.0(5) . . ? C2 C3 C4 117.1(5) . . ? 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 Zn1 O1 1.971(11) . ? Zn1 N1 1.978(15) . ? Zn1 N2 1.998(18) . ? Zn1 O3 2.000(11) . ? Zn1 O4 2.152(13) 2_756 ? S1 C5 1.70(2) . ? S1 C4 1.745(12) . ? S2 C10 1.78(2) . ? S2 C9 1.811(11) . ? O4 C6 1.190(12) . ? O1 C1 1.238(17) . ? C6 O3 1.221(18) . ? C6 C7 1.458(3) . ? N2 C7 1.364(14) . ? C1 O2 1.265(13) . ? C1 C2 1.458(3) . ? C9 C8 1.458(3) . ? C7 C8 1.458(3) . ? N1 C2 1.485(14) . ? C2 C3 1.458(3) . ? C4 C3 1.458(3) . ? loop_ _publcif_info_cif.paper_type ?