#------------------------------------------------------------------------------ #$Date: 2019-12-14 09:04:55 +0200 (Sat, 14 Dec 2019) $ #$Revision: 245192 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556578.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_1556578 loop_ _publ_author_name 'Broadhurst, Edward T.' 'Xu, Hongyi' 'Clabbers, Max T. B.' 'Lightowler, Molly' 'Nudelman, Fabio' 'Zou, Xiaodong' 'Parsons, Simon' _publ_section_title ; Polymorph evolution during crystal growth studied by 3D electron diffraction ; _journal_issue 1 _journal_name_full IUCrJ _journal_paper_doi 10.1107/S2052252519016105 _journal_volume 7 _journal_year 2020 _chemical_formula_moiety C2H5NO2 _chemical_formula_sum 'C2 H5 N O2' _chemical_formula_weight 75.07 _chemical_name_common beta-glycine _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 difmap _atom_sites_solution_primary 'Dual space' _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 112.86(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.3110(11) _cell_length_b 6.4540(13) _cell_length_c 5.6940(11) _cell_measurement_temperature 103(2) _cell_volume 179.84(7) _computing_cell_refinement REDp _computing_data_reduction XDS _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 103(2) _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measurement_method 'Phi scan' _diffrn_radiation_type electrons _diffrn_radiation_wavelength 0.02508 _diffrn_reflns_av_R_equivalents 0.2086 _diffrn_reflns_av_unetI/netI 0.1954 _diffrn_reflns_Laue_measured_fraction_full 0.955 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 2516 _diffrn_reflns_point_group_measured_fraction_full 0.968 _diffrn_reflns_point_group_measured_fraction_max 0.961 _diffrn_reflns_theta_full 0.862 _diffrn_reflns_theta_max 0.957 _diffrn_reflns_theta_min 0.137 _diffrn_source ;? JEOL JEM-2100 LaB6 transmission electron microscope ; _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.386 _exptl_crystal_description shard _exptl_crystal_F_000 27 _refine_diff_density_max 0.215 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.080 _refine_ls_abs_structure_details ; All f" are zero, so absolute structure could not be determined ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_hydrogen_treatment idealised+riding _refine_ls_matrix_type full _refine_ls_number_parameters 54 _refine_ls_number_reflns 859 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.179 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.1276 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1642P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2894 _refine_ls_wR_factor_ref 0.2964 _reflns_Friedel_coverage 0.843 _reflns_Friedel_fraction_full 0.983 _reflns_Friedel_fraction_max 0.963 _reflns_number_gt 745 _reflns_number_total 859 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yc5021.cif _cod_data_source_block beta _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 1556578 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL Beta glycine in P2(1) solved Shelxt BETA.res created by SHELXL-2018/3 at 07:59:49 on 06-Aug-2019 CELL 0.02508 5.311 6.454 5.694 90 112.863 90 ZERR 2 0.0011 0.0013 0.0011 0 0.03 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C 0.731 36.995 1.195 11.297 0.456 2.814 0.125 0.346 0 0 0 0 0.77 12.011 SFAC H 0.375 15.495 0.141 4.126 0.022 0.025 -0.101 46.884 0 0 0 0 0.32 1.008 SFAC N 0.572 28.846 1.043 9.054 0.465 2.421 0.131 0.317 0 0 0 0 0.75 14.007 SFAC O 0.455 23.78 0.917 7.622 0.472 2.144 0.138 0.296 0 0 0 0 0.73 15.999 UNIT 4 10 2 4 TEMP -170 L.S. 20 FMAP 2 PLAN 10 ACTA LIST 4 WGHT 0.164200 FVAR 64.43245 N1 3 -0.148262 0.434608 0.235859 11.00000 0.00864 0.01074 = 0.01335 -0.00397 0.00678 -0.00223 AFIX 138 H1 2 -0.155003 0.468355 0.032484 11.00000 0.01041 H2 2 -0.169277 0.256966 0.259893 11.00000 0.01964 H3 2 0.058885 0.492319 0.387708 11.00000 0.05244 AFIX 0 C1 1 -0.384622 0.548158 0.272080 11.00000 0.01119 0.01186 = 0.01576 0.00179 0.00715 0.00117 AFIX 24 H4 2 -0.594252 0.473999 0.135185 11.00000 0.06565 H5 2 -0.384018 0.724051 0.213227 11.00000 0.02075 AFIX 0 C2 1 -0.364244 0.536691 0.559551 11.00000 0.00966 0.01186 = 0.01281 0.00035 0.00950 -0.00044 O1 4 -0.119458 0.509509 0.741903 11.00000 0.00426 0.02471 = 0.00990 0.00313 0.00381 0.00015 O2 4 -0.590964 0.564417 0.598984 11.00000 0.00628 0.01464 = 0.02011 -0.00461 0.00836 -0.00138 HKLF 4 REM Beta glycine in P2(1) solved Shelxt REM wR2 = 0.296444, GooF = S = 1.17978, Restrained GooF = 1.17905 for all data REM R1 = 0.127617 for 745 Fo > 4sig(Fo) and 0.137915 for all 859 data REM 54 parameters refined using 1 restraints END WGHT 0.1647 0.0000 REM Highest difference peak 0.215, deepest hole -0.293, 1-sigma level 0.080 Q1 1 0.2177 0.3515 0.2986 11.00000 0.05 0.21 Q2 1 -0.2898 0.9087 0.2096 11.00000 0.05 0.17 Q3 1 -0.1625 0.3755 0.0141 11.00000 0.05 0.16 Q4 1 -0.7543 0.3026 0.0639 11.00000 0.05 0.16 Q5 1 0.0038 0.7093 0.1132 11.00000 0.05 0.16 Q6 1 -0.2326 0.8343 0.4317 11.00000 0.05 0.15 Q7 1 -0.2995 0.2003 0.2347 11.00000 0.05 0.15 Q8 1 0.0346 0.3623 0.1653 11.00000 0.05 0.14 Q9 1 -0.2505 0.2491 -0.0085 11.00000 0.05 0.14 Q10 1 -0.0361 0.2264 0.0529 11.00000 0.05 0.14 ; _shelx_res_checksum 25816 _shelx_hkl_file ; 0 0 1 69972. 18689. 1 0 0 2 86969. 23274. 1 0 0 -2 70053. 18770. 1 0 0 5 14945. 3331.04 1 0 0 -5 11327. 2658.03 1 0 0 6 19624. 4957.50 1 0 0 -6 14091. 3705.78 1 0 -1 1 58478. 15824. 1 0 -1 1 49535. 16904. 1 0 1 -1 35103. 12044. 1 0 -1 2 81344. 17669. 1 0 -1 2 77256. 26269. 1 0 -1 -2 88264. 18984. 1 0 1 2 104087. 22388. 1 0 1 -2 79765. 27135. 1 0 -1 3 40550. 16139. 1 0 -1 3 57507. 11663. 1 0 -1 -3 53622. 10761. 1 0 1 3 63699. 12756. 1 0 1 -3 35180. 14059. 1 0 1 -3 52125. 10639. 1 0 -1 4 15953. 3871.71 1 0 1 4 17624. 4091.46 1 0 1 -4 14302. 3564.95 1 0 1 -4 17119. 4160.25 1 0 -1 5 1938.08 815.459 1 0 -2 0 167462. 44800. 1 0 -2 0 403723. 88588. 1 0 -2 0 999999. 460542. 1 0 2 0 288102. 44759. 1 0 2 0 823957. 379482. 1 0 2 0 344395. 75556. 1 0 2 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1 -2 3 -3 4601.37 1487.66 1 2 -3 4 5499.79 2104.41 1 2 -3 4 7021.44 1964.39 1 -2 3 -4 6070.41 1922.70 1 -2 3 -4 6673.40 2454.47 1 2 -3 5 774.99 403.885 1 -2 3 -5 191.18 412.383 1 -2 3 -5 405.10 332.092 1 2 -4 -6 140.95 260.825 1 -2 -4 6 94.13 345.771 1 -2 -4 6 140.02 221.327 1 -2 -4 6 237.92 319.506 1 2 4 -6 318.66 457.709 1 2 4 -6 613.52 488.466 1 -2 4 6 149.21 255.281 1 -2 -4 5 6624.84 2026.71 1 -2 -4 5 4285.71 702.549 1 -2 -4 5 15415. 5333.87 1 2 4 -5 5681.90 844.596 1 2 4 -5 8251.71 3043.70 1 2 4 -5 8223.38 2295.42 1 -2 4 5 4013.35 710.238 1 2 -4 -4 1627.68 377.741 1 -2 -4 4 2022.26 931.606 1 -2 -4 4 2569.81 430.999 1 -2 -4 4 1169.16 684.742 1 2 4 -4 2209.22 401.497 1 2 4 -4 3755.16 1337.92 1 2 4 -4 3040.87 1124.64 1 2 -4 -3 21437. 5026.30 1 2 -4 -3 25362. 4200.72 1 -2 -4 3 13460. 5908.53 1 -2 -4 3 17863. 4354.51 1 2 4 -3 15269. 3752.32 1 -2 4 3 19470. 4548.76 1 2 -4 -2 9388.90 1902.87 1 -2 -4 2 5159.85 407.527 1 -2 -4 2 4099.55 1286.12 1 -2 -4 2 3172.40 1343.99 1 2 4 -2 6552.00 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3853.90 1 -4 4 0 16038. 4204.77 1 4 -4 1 2468.63 1180.49 1 4 -4 1 2050.58 568.595 1 -4 4 -1 5184.13 2070.41 1 -4 4 -1 1750.30 505.463 1 4 -4 2 2819.50 1000.40 1 4 -4 2 2946.58 1185.35 1 -4 4 -2 2606.23 907.324 1 -4 4 -2 2131.93 1008.90 1 4 -4 3 431.81 605.018 1 4 -4 3 1849.86 736.948 1 4 -5 -5 5018.21 972.075 1 4 5 -5 5787.12 550.384 1 -4 5 5 4508.29 845.001 1 -4 5 5 3166.73 739.376 1 4 -5 -4 6632.94 1390.93 1 4 -5 -4 4273.57 958.316 1 -4 -5 4 5285.30 792.796 1 -4 -5 4 2792.39 1256.98 1 4 5 -4 5123.43 813.840 1 -4 5 4 3942.12 907.729 1 -4 5 4 4091.46 909.752 1 4 -5 -3 6418.45 808.579 1 4 -5 -3 7365.43 1106.03 1 4 -5 -3 4985.83 1048.97 1 -4 -5 3 3955.48 893.969 1 -4 -5 3 5418.85 849.048 1 4 5 -3 6171.58 1367.06 1 -4 5 3 5301.49 661.675 1 -4 5 3 6062.32 940.509 1 -4 5 3 6641.03 1323.75 1 4 -5 -2 1827.19 488.870 1 -4 -5 2 2033.99 515.580 1 -4 -5 2 1415.22 405.908 1 4 5 -2 1149.74 319.101 1 4 5 -2 1928.37 523.674 1 4 5 -2 1277.62 235.613 1 -4 5 2 1510.72 330.230 1 -4 5 2 1906.11 587.211 1 -4 5 2 1757.18 461.351 1 4 -5 -1 4787.53 1180.09 1 -4 -5 1 5038.44 1287.74 1 -4 -5 1 3492.91 806.555 1 4 5 -1 4123.83 1047.75 1 4 5 -1 3444.76 797.247 1 -4 5 1 6264.66 1498.58 1 4 -5 0 10320. 3093.89 1 4 -5 0 1305.95 817.077 1 -4 -5 0 5422.90 1201.94 1 -4 -5 0 7211.65 2137.59 1 4 5 0 4528.53 1390.53 1 -4 5 0 10121. 3035.61 1 4 -5 1 4536.62 1516.79 1 4 -5 1 3825.57 1155.81 1 -4 5 -1 4957.50 1641.44 1 4 -5 2 738.97 442.735 1 4 -5 2 1048.16 679.077 1 -4 5 -2 447.59 326.264 1 4 -6 -4 255.81 184.945 1 -4 -6 4 395.59 143.666 1 -4 6 4 439.09 339.781 1 -4 6 4 243.42 176.568 1 4 -6 -3 843.38 405.503 1 4 -6 -3 105.42 229.421 1 4 -6 -3 636.18 167.058 1 -4 -6 3 39.36 161.594 1 -4 -6 3 426.14 219.223 1 -4 -6 3 605.02 226.143 1 4 6 -3 556.86 232.618 1 4 6 -3 270.50 283.691 1 -4 6 3 1526.10 558.883 1 -4 6 3 325.13 268.636 1 -4 6 3 1261.43 544.718 1 4 -6 -2 3002.02 805.341 1 4 -6 -2 1430.19 632.132 1 4 -6 -2 1543.91 496.964 1 4 -6 -2 810.60 208.944 1 -4 -6 2 718.74 364.548 1 -4 -6 2 1214.08 446.378 1 4 6 -2 1059.89 441.117 1 4 6 -2 1001.62 356.535 1 -4 6 2 1477.13 264.306 1 -4 6 2 4200.72 1023.88 1 4 -6 -1 4743.01 1439.50 1 -4 -6 1 3166.33 951.031 1 -4 -6 1 4641.84 1499.80 1 4 6 -1 4196.68 1343.99 1 4 6 -1 4245.24 1197.89 1 -4 6 1 4969.64 1519.63 1 4 -6 0 3437.88 1186.56 1 4 -6 0 2095.10 727.640 1 -4 -6 0 4989.88 1569.40 1 -4 -6 0 5851.88 1208.82 1 4 6 0 6191.82 1955.48 1 -4 6 0 842.57 479.158 1 -4 6 0 3611.09 1264.26 1 4 -6 1 4856.33 1752.33 1 -4 6 -1 1131.52 504.249 1 4 -7 -2 173.33 102.914 1 4 -7 -2 462.57 368.879 1 -4 -7 2 225.01 165.884 1 -4 -7 2 107.12 201.173 1 4 7 -2 237.51 138.851 1 -4 7 2 1018.61 577.903 1 -4 7 2 358.19 130.919 1 -4 7 2 331.57 401.659 1 4 -7 -1 7875.35 2363.82 1 -4 -7 1 3785.10 1249.70 1 -4 -7 1 4079.32 1258.60 1 4 7 -1 4087.41 1323.35 1 -4 7 1 5252.93 1673.41 1 5 0 -7 472.68 237.920 1 -5 0 7 431.00 229.097 1 5 0 -6 156.21 232.213 1 -5 0 6 441.52 335.815 1 5 0 -5 2440.71 529.340 1 5 0 -4 432.21 267.260 1 5 0 -4 445.16 185.714 1 -5 0 4 420.88 273.816 1 -5 0 4 615.13 177.094 1 5 0 -3 7345.20 1241.20 1 5 0 -3 6863.61 1477.54 1 -5 0 3 10348. 2215.70 1 -5 0 3 9178.46 1539.46 1 5 0 -2 17216. 2692.83 1 5 0 -2 15945. 3405.10 1 5 0 -2 19935. 5532.17 1 -5 0 2 14650. 2295.42 1 -5 0 2 11611. 2481.99 1 -5 0 2 13468. 3734.52 1 5 0 -1 2439.90 826.385 1 5 0 -1 2468.23 857.142 1 -5 0 1 1653.18 603.399 1 -5 0 1 3402.26 1101.17 1 5 0 0 3648.72 1104.81 1 5 0 0 2783.89 805.746 1 -5 0 0 2952.24 852.690 1 -5 0 0 2816.27 888.708 1 5 0 1 8097.93 2428.97 1 5 0 1 5131.52 1927.56 1 -5 0 -1 5487.65 1677.86 1 5 -1 -6 1492.92 593.686 1 -5 -1 6 4245.24 1168.76 1 -5 1 6 2509.91 838.526 1 5 -1 -5 55.60 139.377 1 -5 -1 5 107.81 122.906 1 5 1 -5 133.63 160.947 1 -5 1 5 66.41 130.311 1 -5 1 5 206.92 182.517 1 5 -1 -4 1886.68 346.620 1 5 -1 -4 1031.16 413.597 1 -5 -1 4 2118.98 328.773 1 -5 -1 4 1422.50 468.636 1 5 1 -4 2095.10 363.253 1 -5 1 4 1747.06 282.760 1 -5 1 4 1545.53 520.437 1 5 -1 -3 25836. 4006.07 1 5 -1 -3 18895. 2573.45 1 -5 -1 3 23314. 2904.08 1 -5 -1 3 27892. 4301.90 1 5 1 -3 29599. 6317.27 1 5 1 -3 29717. 4556.85 1 -5 1 3 27689. 4293.80 1 -5 1 3 24407. 3006.07 1 5 -1 -2 20830. 4443.54 1 5 -1 -2 19385. 3013.76 1 5 -1 -2 30255. 8377.17 1 -5 -1 2 20482. 3143.66 1 -5 -1 2 18737. 4002.02 1 5 1 -2 22687. 4840.14 1 -5 1 2 21429. 3314.85 1 -5 1 2 18600. 3968.03 1 -5 1 2 25722. 7130.71 1 5 -1 -1 15451. 4540.67 1 5 -1 -1 11437. 3321.73 1 -5 -1 1 29150. 8381.21 1 -5 -1 1 18110. 3863.61 1 5 1 -1 17216. 4989.88 1 -5 1 1 15176. 4297.85 1 -5 1 1 27454. 8008.90 1 5 -1 0 26050. 6665.31 1 5 -1 0 36394. 9433.42 1 -5 -1 0 21562. 5495.75 1 5 1 0 33007. 8389.31 1 -5 1 0 41198. 10526. 1 -5 1 0 30987. 8021.04 1 5 -1 1 152.61 265.277 1 5 -1 1 2380.01 1091.06 1 -5 -1 -1 121.65 186.281 1 -5 1 -1 1208.42 529.340 1 5 -2 -6 3518.41 842.573 1 -5 -2 6 2668.96 749.493 1 5 2 -6 7029.54 1431.00 1 -5 2 6 4419.26 989.882 1 5 -2 -5 369.28 265.803 1 5 -2 -5 153.54 197.167 1 -5 -2 5 683.53 254.512 1 5 2 -5 685.96 287.414 1 5 2 -5 6386.07 2169.97 1 -5 2 5 1591.66 515.176 1 -5 2 5 418.05 231.202 1 5 -2 -4 948.60 324.322 1 5 -2 -4 1193.44 379.158 1 -5 -2 4 1272.76 370.133 1 5 2 -4 757.18 231.121 1 -5 2 4 1663.70 460.137 1 5 -2 -3 1132.33 475.111 1 -5 -2 3 1103.20 240.712 1 -5 2 3 1566.17 285.350 1 -5 2 3 1545.53 550.384 1 5 -2 -2 12185. 2307.16 1 5 -2 -2 5325.77 1555.24 1 5 -2 -2 5600.97 1553.22 1 5 -2 -2 11194. 2398.62 1 -5 -2 2 10045. 1910.56 1 -5 -2 2 10635. 2211.65 1 5 2 -2 12234. 2321.73 1 -5 2 2 11578. 2469.44 1 -5 2 2 4605.42 1332.66 1 -5 2 2 8255.76 1565.76 1 5 -2 -1 19535. 5192.22 1 5 -2 -1 15836. 4144.07 1 -5 -2 1 16552. 3133.55 1 5 2 -1 20409. 3860.38 1 -5 2 1 14868. 3996.76 1 5 -2 0 6102.79 1405.10 1 5 -2 0 6017.80 2303.11 1 -5 -2 0 5034.39 1097.13 1 -5 2 0 3669.77 912.585 1 5 -2 1 1182.52 768.514 1 5 -2 1 1271.55 554.836 1 -5 2 -1 923.11 668.959 1 5 -2 2 95.10 238.082 1 5 -2 2 379.24 389.397 1 5 -3 -6 787.13 308.943 1 -5 -3 6 646.30 469.040 1 -5 3 6 1205.58 373.775 1 5 -3 -5 1004.86 439.093 1 5 -3 -5 2098.34 694.860 1 -5 -3 5 1473.09 315.378 1 5 3 -5 1547.55 394.051 1 -5 3 5 456.90 297.774 1 -5 3 5 1553.62 612.302 1 5 -3 -4 8106.02 1164.71 1 5 -3 -4 6863.61 1374.75 1 5 3 -4 2828.41 1065.96 1 5 3 -4 5418.85 925.131 1 -5 3 4 6402.26 851.881 1 -5 3 4 7025.49 1396.60 1 5 -3 -3 18745. 3260.62 1 -5 -3 3 17127. 2876.16 1 -5 -3 3 17904. 4516.39 1 5 3 -3 18231. 4589.23 1 5 3 -3 15662. 2633.75 1 -5 3 3 14298. 2549.98 1 5 -3 -2 3142.04 819.101 1 5 -3 -2 4330.23 1091.46 1 5 -3 -2 2682.31 604.613 1 -5 -3 2 3332.25 863.617 1 -5 -3 2 3350.46 631.727 1 5 3 -2 5560.50 1411.57 1 -5 3 2 1959.12 499.797 1 -5 3 2 3360.98 708.619 1 -5 3 2 3852.69 951.436 1 -5 3 2 2693.24 901.254 1 5 -3 -1 6968.83 2561.31 1 5 -3 -1 10453. 2335.49 1 -5 -3 1 11967. 3013.35 1 5 3 -1 9526.50 2397.41 1 -5 3 1 8555.23 1947.79 1 -5 3 1 11611. 4055.03 1 5 -3 0 7486.84 2309.59 1 5 -3 0 10907. 3930.79 1 5 -3 1 1475.11 825.171 1 5 -3 1 696.07 365.034 1 -5 3 -1 1925.13 663.698 1 5 -3 2 1526.10 628.490 1 5 -4 -5 1522.46 486.442 1 5 -4 -5 1051.40 350.829 1 -5 -4 5 1205.58 227.438 1 5 4 -5 1097.94 242.614 1 -5 4 5 1010.52 333.104 1 -5 4 5 1612.30 515.985 1 5 -4 -4 900.85 419.263 1 -5 -4 4 1799.67 390.611 1 5 4 -4 2031.97 758.801 1 5 4 -4 1671.39 388.911 1 -5 4 4 1155.40 455.686 1 -5 4 4 1910.16 736.543 1 -5 4 4 1365.84 265.317 1 5 -4 -3 904.49 314.731 1 5 -4 -3 163.74 211.291 1 -5 -4 3 -28.51 122.541 1 -5 -4 3 400.73 157.547 1 5 4 -3 142.98 91.946 1 5 4 -3 263.33 130.797 1 -5 4 3 55.93 191.704 1 -5 4 3 262.48 183.650 1 5 -4 -2 4192.63 1448.00 1 5 -4 -2 2158.64 549.575 1 5 -4 -2 3844.59 842.168 1 -5 -4 2 2411.57 557.668 1 5 4 -2 2742.61 617.968 1 -5 4 2 3176.85 1143.67 1 -5 4 2 2259.00 554.836 1 5 -4 -1 15382. 4540.67 1 5 -4 -1 4965.60 1942.94 1 -5 -4 1 16046. 3515.98 1 5 4 -1 19421. 5495.75 1 5 4 -1 13695. 2995.55 1 -5 4 1 16487. 4848.23 1 5 -4 0 5892.35 1678.27 1 5 -4 0 6458.92 2029.14 1 -5 4 0 5471.46 1778.63 1 -5 4 0 10129. 2775.80 1 5 -4 1 193.57 245.204 1 5 -4 1 370.74 407.932 1 5 -5 -4 3093.48 687.575 1 -5 -5 4 3323.75 428.166 1 5 5 -4 2444.35 373.897 1 5 5 -4 3784.70 792.391 1 -5 5 4 3068.80 332.335 1 -5 5 4 3674.62 749.089 1 -5 5 4 5224.60 1107.65 1 5 -5 -3 6268.71 1150.55 1 -5 -5 3 4783.48 1016.19 1 5 5 -3 5301.49 1102.79 1 5 5 -3 4022.66 658.842 1 -5 5 3 5269.12 1002.43 1 -5 5 3 7033.58 636.988 1 5 -5 -2 135.53 182.436 1 5 -5 -2 700.93 411.574 1 -5 -5 2 876.57 337.474 1 5 5 -2 858.76 309.308 1 5 5 -2 312.99 212.586 1 -5 5 2 233.27 197.936 1 -5 5 2 305.14 326.952 1 5 -5 -1 3087.82 940.509 1 5 -5 -1 6766.48 2222.98 1 -5 -5 1 3789.56 1153.78 1 5 5 -1 3815.05 1153.38 1 5 5 -1 3163.90 658.033 1 -5 5 1 4658.03 1580.33 1 -5 -5 0 634.16 284.257 1 -5 5 0 349.09 319.263 1 5 -6 -2 396.76 430.594 1 5 -6 -2 338.65 314.245 1 -5 -6 2 310.24 250.101 1 5 6 -2 550.79 307.567 1 5 6 -2 402.23 187.171 1 -5 6 2 374.22 411.169 1 -5 6 2 618.37 450.829 1 -5 6 2 311.13 104.371 1 6 0 -6 636.99 244.880 1 6 0 -5 795.63 285.147 1 -6 0 5 554.43 224.524 1 -6 0 5 785.51 246.621 1 6 0 -4 104.09 169.850 1 6 0 -4 155.85 179.725 1 -6 0 4 399.15 220.073 1 -6 0 4 799.68 308.094 1 6 0 -3 2118.57 483.205 1 6 0 -3 3331.04 715.094 1 6 0 -3 5123.43 1772.56 1 -6 0 3 2720.35 643.868 1 -6 0 3 3912.58 1384.86 1 6 0 -2 1624.44 747.875 1 6 0 -2 619.18 155.605 1 -6 0 2 566.57 147.147 1 -6 0 2 749.90 427.762 1 6 0 -1 898.83 599.352 1 6 0 -1 623.63 299.190 1 -6 0 1 718.74 448.806 1 -6 0 1 486.85 287.414 1 6 0 0 529.74 402.752 1 6 0 0 192.15 188.223 1 -6 0 0 524.08 386.119 1 6 0 1 2420.88 798.057 1 -6 -1 6 4204.77 589.639 1 6 1 -6 5572.64 770.133 1 -6 1 6 4892.75 962.767 1 6 -1 -5 148.04 150.951 1 6 -1 -5 354.31 152.570 1 -6 -1 5 217.85 111.534 1 -6 -1 5 521.65 197.086 1 6 1 -5 217.20 130.676 1 -6 1 5 316.67 191.825 1 6 -1 -4 2532.58 518.008 1 6 -1 -4 2491.70 732.496 1 -6 -1 4 3573.45 874.139 1 -6 -1 4 2795.63 497.369 1 6 1 -4 1983.81 454.471 1 6 1 -4 2242.41 611.493 1 -6 1 4 2794.82 796.438 1 -6 1 4 3395.38 535.006 1 6 -1 -3 965.60 309.834 1 6 -1 -3 571.02 155.929 1 6 -1 -3 646.30 470.659 1 -6 -1 3 488.87 242.088 1 6 1 -3 859.97 288.830 1 6 1 -3 733.31 193.403 1 6 1 -3 386.73 266.936 1 -6 1 3 1094.29 372.561 1 -6 1 3 1012.95 246.823 1 -6 1 3 1516.79 668.150 1 6 -1 -2 1586.40 608.660 1 6 -1 -2 2121.00 970.456 1 6 -1 -2 2947.39 652.772 1 6 1 -2 2771.75 618.777 1 -6 1 2 2106.84 469.850 1 -6 1 2 4075.27 1538.24 1 6 -1 -1 560.10 283.529 1 6 -1 -1 1736.95 771.347 1 -6 -1 1 916.63 354.431 1 6 1 -1 760.82 296.965 1 -6 1 1 855.52 445.163 1 -6 1 1 1294.62 487.252 1 6 -1 0 1513.15 579.927 1 6 -1 0 780.25 384.783 1 -6 -1 0 776.61 317.037 1 6 1 0 876.16 368.433 1 6 -1 1 2138.81 787.130 1 6 1 1 1256.58 442.331 1 6 -2 -5 2175.64 513.557 1 -6 -2 5 3075.67 403.116 1 -6 -2 5 3450.42 893.969 1 6 2 -5 3683.12 478.348 1 6 2 -5 3226.63 825.576 1 -6 2 5 2403.07 315.742 1 -6 2 5 1975.72 484.014 1 6 -2 -4 377.01 285.633 1 6 -2 -4 399.76 213.152 1 -6 -2 4 323.92 220.963 1 -6 -2 4 387.01 201.861 1 6 2 -4 472.68 205.706 1 -6 2 4 598.95 364.387 1 -6 2 4 462.57 204.573 1 6 -2 -3 2977.33 961.148 1 6 -2 -3 3562.52 872.925 1 -6 -2 3 3180.09 779.441 1 6 2 -3 3064.75 1003.24 1 -6 2 3 2824.76 790.772 1 -6 2 3 4625.65 1476.73 1 6 -2 -2 1044.92 549.575 1 6 -2 -2 1101.58 362.565 1 6 2 -2 486.44 192.594 1 -6 2 2 622.42 214.366 1 -6 2 2 557.67 398.583 1 6 -2 -1 1911.77 875.353 1 6 2 -1 911.37 298.138 1 -6 2 1 1453.66 681.909 1 6 -2 0 2050.99 775.799 1 -6 -2 0 1948.20 632.537 1 6 2 0 2101.17 685.552 1 6 -3 -5 834.48 640.226 1 -6 -3 5 1263.86 338.446 1 6 3 -5 1312.02 386.483 1 -6 3 5 911.37 718.332 1 6 -3 -4 1118.98 359.490 1 -6 -3 4 1370.70 278.794 1 -6 -3 4 865.64 248.523 1 6 3 -4 1020.23 248.523 1 6 3 -4 1180.49 264.872 1 -6 3 4 1035.21 378.389 1 6 -3 -3 2129.90 603.804 1 6 -3 -3 1387.29 298.543 1 -6 -3 3 2499.80 623.229 1 6 3 -3 2391.34 511.938 1 -6 3 3 2459.73 732.901 1 6 -3 -2 6276.81 2043.30 1 6 -3 -2 2459.33 888.303 1 6 3 -2 3532.57 734.520 1 -6 3 2 4649.93 953.055 1 6 -3 -1 395.71 327.276 1 6 -3 -1 474.71 323.958 1 6 -3 0 1108.46 495.750 1 6 -4 -4 1004.05 745.042 1 -6 -4 4 1562.93 432.618 1 -6 -4 4 1166.33 563.739 1 6 4 -4 979.76 336.301 1 6 4 -4 1532.98 530.149 1 -6 4 4 1607.44 983.002 1 6 -4 -3 2785.51 1275.60 1 6 -4 -3 543.10 363.415 1 -6 -4 3 3623.63 1394.17 1 6 4 -3 3030.35 1002.43 1 -6 4 3 2919.06 1411.17 1 6 -4 -2 651.56 428.571 1 6 -4 -2 311.09 382.476 1 6 4 -2 394.46 162.970 1 -6 4 2 533.39 177.337 1 -6 4 2 351.40 488.061 1 6 -4 -1 2244.84 807.365 1 6 4 -1 2338.32 761.230 1 7 0 -3 1477.13 501.821 1 -7 0 3 1503.44 577.498 1 -7 0 3 962.36 582.759 1 7 0 -2 4354.51 1278.43 1 7 0 -2 8429.78 2697.29 1 7 0 -2 4908.94 1646.30 1 -7 0 2 4229.05 1412.79 1 7 -1 -3 671.79 409.955 1 7 -1 -3 238.49 133.792 1 -7 -1 3 443.95 370.902 1 7 1 -3 298.91 151.598 1 7 1 -3 282.56 256.212 1 -7 1 3 1107.24 521.246 1 -7 1 3 291.50 341.198 1 0 0 0 0. 0.00 0 ; _shelx_hkl_checksum 3452 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 N1 N -0.1483(10) 0.4346(8) 0.2359(11) 0.0101(13) Uani 1 1 d . H1 H -0.155(3) 0.468(3) 0.032(4) 0.010(6) Uiso 1 1 calc R H2 H -0.169(3) 0.257(3) 0.260(5) 0.020(7) Uiso 1 1 calc R H3 H 0.059(4) 0.492(3) 0.388(4) 0.052(15) Uiso 1 1 calc R C1 C -0.3846(12) 0.5482(9) 0.2721(13) 0.0124(14) Uani 1 1 d . H4 H -0.594(7) 0.474(3) 0.135(4) 0.066(19) Uiso 1 1 calc R H5 H -0.3840(12) 0.724(5) 0.213(2) 0.021(8) Uiso 1 1 calc R C2 C -0.3642(12) 0.5367(8) 0.5596(14) 0.0099(14) Uani 1 1 d . O1 O -0.1195(10) 0.5095(9) 0.7419(9) 0.0126(13) Uani 1 1 d . O2 O -0.5910(9) 0.5644(8) 0.5990(11) 0.0127(12) Uani 1 1 d . 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 N1 0.009(2) 0.011(2) 0.013(3) -0.004(2) 0.007(2) -0.002(2) C1 0.011(3) 0.012(3) 0.016(3) 0.002(3) 0.007(3) 0.001(3) C2 0.010(3) 0.012(3) 0.013(3) 0.000(3) 0.009(3) 0.000(2) O1 0.004(2) 0.025(3) 0.010(3) 0.003(2) 0.004(2) 0.0002(17) O2 0.006(2) 0.015(2) 0.020(3) -0.005(2) 0.008(2) -0.0014(17) 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' H H 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C1 C2 112.4(5) O2 C2 O1 124.6(6) O2 C2 C1 117.7(6) O1 C2 C1 117.7(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C1 1.535(6) C1 C2 1.600(9) C2 O2 1.320(6) C2 O1 1.323(8)