#------------------------------------------------------------------------------ #$Date: 2020-02-05 07:55:53 +0200 (Wed, 05 Feb 2020) $ #$Revision: 247895 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556579.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1556579 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_page_first 5 _journal_page_last 9 _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 gamma-glycine _space_group_crystal_system trigonal _space_group_IT_number 144 _space_group_name_Hall 'P 31' _space_group_name_H-M_alt 'P 31' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 7.3950(10) _cell_length_b 7.3950(10) _cell_length_c 5.7500(12) _cell_measurement_temperature 103(2) _cell_volume 272.32(8) _computing_cell_refinement REDp _computing_data_reduction XDS _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 103(2) _diffrn_measured_fraction_theta_full 0.677 _diffrn_measured_fraction_theta_max 0.663 _diffrn_measurement_method 'Phi scan' _diffrn_radiation_type electrons _diffrn_radiation_wavelength 0.02508 _diffrn_reflns_av_R_equivalents 0.2475 _diffrn_reflns_av_unetI/netI 0.3990 _diffrn_reflns_Laue_measured_fraction_full 0.677 _diffrn_reflns_Laue_measured_fraction_max 0.663 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 769 _diffrn_reflns_point_group_measured_fraction_full 0.610 _diffrn_reflns_point_group_measured_fraction_max 0.560 _diffrn_reflns_theta_full 0.862 _diffrn_reflns_theta_max 1.026 _diffrn_reflns_theta_min 0.112 _diffrn_source ; JEOL JEM-2100 LaB6 transmission electron microscope ; _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.373 _exptl_crystal_description block _exptl_crystal_F_000 40 _refine_diff_density_max 0.154 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.068 _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 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 18 _refine_ls_number_reflns 625 _refine_ls_number_restraints 9 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.4088 _refine_ls_R_factor_gt 0.3064 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.3883P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.6299 _refine_ls_wR_factor_ref 0.7029 _reflns_Friedel_coverage 0.689 _reflns_Friedel_fraction_full 0.544 _reflns_Friedel_fraction_max 0.457 _reflns_number_gt 160 _reflns_number_total 625 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yc5021.cif _cod_data_source_block gamma _cod_depositor_comments 'Adding full bibliography for 1556577--1556579.cif.' _cod_original_cell_volume 272.32(9) _cod_database_code 1556579 _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 gamma glycine P3(1) SOLVED SHELXT gamma.res created by SHELXL-2018/3 at 09:48:40 on 06-Aug-2019 CELL 0.02508 7.395 7.395 5.75 90 90 120 ZERR 3 0.001 0.001 0.0012 0 0 0 LATT -1 SYMM -Y,+X-Y,0.333+Z SYMM +Y-X,-X,0.667+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 6 15 3 6 TEMP -170 OMIT -1 -1 0 OMIT 2 2 0 OMIT -1 -3 4 OMIT -1 2 0 L.S. 20 DFIX 1.27 0.02 O1 C2 O2 C2 DFIX 1.50 0.02 C1 C2 DFIX 1.48 0.02 C1 N1 DFIX 2.40 0.02 O1 C1 O2 C1 DFIX 2.50 0.02 C2 N1 FLAT 0.05 O1 O2 C1 C2 EADP N1 C1 C2 O1 O2 FMAP 2 PLAN 10 ACTA LIST 4 BOND WGHT 0.388300 FVAR 10.14842 N1 3 0.760719 0.786852 0.758056 11.00000 0.03813 AFIX 137 1.0500 H1 2 0.780745 0.744100 0.926119 11.00000 -1.20000 H3 2 0.706135 0.893163 0.769362 11.00000 -1.20000 H2 2 0.904223 0.856791 0.669761 11.00000 -1.20000 AFIX 0 C1 1 0.610075 0.602257 0.632121 11.00000 0.03813 AFIX 23 1.0890 H5 2 0.454281 0.560896 0.691718 11.00000 -1.20000 H4 2 0.635517 0.473784 0.677852 11.00000 -1.20000 AFIX 0 C2 1 0.615139 0.620848 0.373780 11.00000 0.03813 O1 4 0.760608 0.795150 0.283842 11.00000 0.03813 O2 4 0.482913 0.469338 0.249153 11.00000 0.03813 HKLF 4 REM gamma glycine P3(1) SOLVED SHELXT REM wR2 = 0.702857, GooF = S = 1.01292, Restrained GooF = 1.01036 for all data REM R1 = 0.306383 for 160 Fo > 4sig(Fo) and 0.408787 for all 625 data REM 18 parameters refined using 9 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.154, deepest hole -0.230, 1-sigma level 0.068 Q1 1 0.9869 1.0416 0.7268 11.00000 0.05 0.15 Q2 1 1.0387 0.9774 0.4939 11.00000 0.05 0.15 Q3 1 0.4019 0.3500 0.1219 11.00000 0.05 0.15 Q4 1 1.0258 0.8025 0.7286 11.00000 0.05 0.14 Q5 1 0.6316 0.9583 0.7346 11.00000 0.05 0.13 Q6 1 0.5940 0.8583 0.8738 11.00000 0.05 0.13 Q7 1 0.3204 0.3554 0.6479 11.00000 0.05 0.13 Q8 1 0.4381 0.4769 0.7548 11.00000 0.05 0.13 Q9 1 0.3993 0.4406 0.2667 11.00000 0.05 0.13 Q10 1 0.6208 0.3045 0.5147 11.00000 0.05 0.12 ; _shelx_res_checksum 56261 _shelx_hkl_file ; 1 -1 0 465.35 128.49 -1 0 -1 5007.90 1220.38 1 0 1 4315.57 1051.79 1 -2 0 9999.00 2436.46 2 -1 0 4050.29 993.40 -1 2 0 7866.51 1917.11 1 -2 -1 1423.06 354.56 -2 1 -1 1825.12 450.15 2 -1 1 1870.51 462.45 -1 2 1 1992.80 490.45 -2 1 -2 728.73 185.68 2 -1 2 585.94 152.98 0 2 1 2868.21 700.33 2 -2 1 3587.14 878.11 -2 2 -1 2470.15 605.94 2 -2 0 5565.14 1359.86 -2 2 0 5181.58 1266.67 2 -2 -1 68.09 70.69 -2 0 -1 207.28 70.99 2 0 1 317.67 94.79 -2 2 1 197.18 85.49 -2 0 -2 2590.84 634.24 2 1 2 388.66 104.29 1 -3 0 5080.29 1241.18 -3 2 0 4696.73 1149.69 3 -2 0 4607.54 1129.19 -1 3 0 5408.36 1320.97 1 -3 -1 1865.71 463.15 -3 2 -1 984.00 250.37 3 -2 1 1105.29 284.37 -1 3 1 1290.07 322.27 1 2 2 872.31 213.68 -1 -2 -2 910.21 222.78 2 -3 1 2530.55 624.84 -2 3 -1 2795.82 686.83 2 -3 0 6216.48 1524.35 2 -3 -1 593.64 168.18 -3 1 -1 537.45 150.68 3 -1 1 512.85 148.89 -2 3 1 528.55 157.98 -3 1 -2 812.92 211.38 3 -1 2 744.43 197.08 -3 1 -3 1761.02 433.96 3 -1 3 1372.56 341.57 0 3 2 375.36 100.09 3 -3 2 706.33 185.88 0 -3 -2 349.57 96.59 3 -3 1 2723.53 675.23 -3 3 -1 2617.34 647.44 3 -3 0 1227.88 315.27 -3 3 0 1197.48 307.07 3 -3 -1 265.57 112.39 -3 3 1 154.18 81.19 -3 0 -2 4175.68 1022.10 -3 0 -3 459.75 123.89 3 0 3 406.26 109.39 -3 -1 -4 2353.46 576.34 3 1 3 155.88 57.09 -3 -1 -3 256.17 74.59 -4 3 1 114.09 96.89 4 -3 -1 36.60 90.19 -4 3 0 1342.17 343.77 4 -3 0 797.32 222.98 -4 3 -1 294.57 101.09 4 -3 1 164.78 85.49 1 -4 -2 3097.39 759.92 -4 3 -2 4542.35 1115.89 4 -3 2 4897.01 1202.78 -1 4 2 3596.74 881.21 1 -4 -3 46.90 64.19 -1 4 3 25.00 66.99 -2 -2 -3 313.37 79.59 -2 4 -1 1988.00 493.05 2 -4 0 3866.91 947.61 -4 2 0 1787.02 450.15 4 -2 0 1053.69 275.27 2 -4 -1 452.35 129.99 -4 2 -1 261.77 114.29 4 -2 1 250.67 108.99 -2 4 1 380.46 119.29 2 -4 -2 225.48 93.19 4 -2 2 423.16 127.29 -2 4 2 250.87 89.49 -4 2 -3 520.55 147.99 4 -2 3 524.45 142.49 -4 2 -4 1966.30 487.05 4 -2 4 1972.30 489.95 -1 -3 -3 353.66 91.49 3 -4 2 3845.22 944.41 -3 4 -2 3695.63 907.51 3 -4 1 1693.23 422.16 -3 4 -1 1471.05 367.66 3 -4 0 1126.59 289.77 -3 4 0 943.91 245.38 3 -4 -1 422.36 131.49 -4 1 -1 96.49 88.49 4 -1 1 100.49 77.99 3 -4 -2 108.09 76.49 -4 1 -2 291.87 101.39 4 -1 2 488.05 143.29 -3 4 2 137.19 93.39 -4 1 -3 365.26 117.99 4 -1 3 301.07 99.79 4 -1 4 1871.51 463.65 0 4 3 22.60 47.80 4 -4 3 93.69 65.09 -4 4 -3 187.78 76.99 0 -4 -3 33.90 48.20 0 4 2 511.15 133.49 4 -4 2 1498.25 376.56 -4 4 -2 799.22 212.08 0 -4 -2 622.14 158.48 4 -4 1 905.81 242.48 -4 4 -1 917.21 242.68 4 -4 0 2489.45 618.74 -4 4 0 2078.69 521.75 4 -4 -1 235.28 113.99 -4 4 1 252.77 104.19 4 -4 -2 -5.30 80.99 -4 0 -2 6.20 41.30 4 0 2 51.29 66.09 -4 4 2 83.09 102.29 -4 0 -3 144.39 59.89 4 0 3 133.89 65.59 -4 0 -4 190.88 68.39 4 0 4 229.38 71.99 4 1 5 69.59 35.70 -4 -1 -5 -10.20 38.80 4 1 4 79.79 49.70 -4 -1 -4 24.20 41.10 -4 -1 -3 13.60 24.90 5 -4 -1 461.95 144.69 5 -4 0 66.39 107.29 1 -5 -1 214.48 74.89 -5 4 -1 191.18 89.69 5 -4 1 170.08 90.19 -1 5 1 411.76 117.89 1 -5 -2 310.27 99.19 -5 4 -2 250.67 109.39 -1 5 2 153.08 76.99 1 -5 -3 43.80 57.79 -5 4 -3 374.36 120.49 5 -4 3 334.07 107.99 -1 5 3 64.29 57.29 -5 4 -4 660.23 177.28 5 -4 4 365.46 112.99 3 2 4 425.26 108.39 -3 -2 -4 353.86 92.89 3 2 3 -8.50 34.00 2 -5 0 953.60 244.58 -5 3 0 205.58 96.49 5 -3 0 166.88 103.89 2 -5 -1 365.96 112.69 -5 3 -1 359.46 132.89 5 -3 1 276.67 125.09 -2 5 1 316.47 104.29 2 -5 -2 558.44 156.38 -5 3 -2 348.87 115.09 5 -3 2 463.85 151.38 -2 5 2 679.33 183.88 -5 3 -3 121.59 79.79 5 -3 3 102.89 73.19 -2 5 3 62.99 64.99 -3 5 -1 2834.42 698.83 3 -5 0 768.52 205.58 -3 5 0 793.42 214.98 3 -5 -1 101.49 73.89 5 -2 1 47.30 77.49 -3 5 1 107.59 69.09 3 -5 -2 42.70 83.59 5 -2 2 89.09 91.19 -3 5 2 35.60 83.29 -5 2 -3 115.99 65.89 5 -2 3 142.39 86.69 -3 5 3 13.30 80.89 -5 2 -4 625.54 174.28 5 -2 4 553.34 149.59 -5 2 -5 120.89 59.29 5 -2 5 93.29 53.39 1 4 3 143.99 47.80 -4 5 -3 111.69 68.39 -1 -4 -3 55.79 35.20 4 -5 2 343.07 112.89 -4 5 -2 338.97 108.99 4 -5 1 165.28 84.49 -4 5 -1 290.17 110.89 4 -5 0 405.56 128.79 -4 5 0 289.47 110.59 4 -5 -1 164.38 83.59 5 -1 1 -2.20 66.79 -4 5 1 248.98 113.19 4 -5 -2 14.10 73.89 -5 1 -2 -12.60 43.40 4 -5 -3 -0.60 38.60 -5 1 -3 50.79 56.79 5 -1 3 -0.50 69.29 -5 1 -4 119.99 74.79 5 -1 4 230.58 86.09 -5 1 -5 13.20 43.70 0 5 4 46.80 48.20 5 -5 4 377.56 116.59 0 -5 -4 22.10 51.09 0 5 3 172.78 69.09 5 -5 3 682.23 184.78 0 -5 -3 210.18 75.39 0 5 2 293.07 84.69 5 -5 2 298.37 108.99 -5 5 -2 171.78 95.09 0 -5 -2 429.36 116.89 5 -5 1 105.79 85.19 -5 5 -1 91.59 74.49 5 -5 0 1823.22 460.55 5 -5 -1 -3.70 92.59 -5 5 1 125.79 98.79 5 -5 -2 50.49 75.09 5 0 2 44.40 69.49 -5 0 -3 161.58 76.59 -5 0 -4 26.00 45.40 5 0 4 33.30 49.10 -5 0 -5 39.60 47.40 -5 0 -6 81.39 46.20 -5 -1 -6 51.79 39.20 -5 -1 -5 8.00 38.90 5 1 4 34.20 53.39 -5 -1 -4 8.30 53.99 5 1 3 10.20 53.49 -6 5 2 211.08 114.59 6 -5 -2 21.20 96.39 -6 5 1 83.89 97.89 6 -5 -1 60.09 84.39 -6 5 0 115.59 98.99 6 -5 0 88.79 98.79 -6 5 -1 212.08 100.39 6 -5 1 112.19 85.59 -1 6 1 259.57 82.79 1 -6 -2 159.48 63.29 -6 5 -2 36.70 65.49 6 -5 2 10.80 88.49 -1 6 2 214.38 74.89 1 -6 -3 11.30 53.19 -6 5 -3 18.90 68.09 6 -5 3 20.10 79.49 -1 6 3 -1.20 50.29 1 -6 -4 -20.40 64.49 -6 5 -4 63.09 63.79 6 -5 4 63.69 58.79 -1 6 4 31.80 53.79 -6 5 -5 10.00 54.89 4 2 5 119.69 40.80 -4 -2 -5 41.60 36.50 4 2 4 4.50 43.90 6 -4 -1 42.70 82.09 2 -6 0 2424.36 599.24 -6 4 0 835.92 235.08 6 -4 0 919.81 250.17 2 -6 -1 631.74 167.78 -6 4 -1 207.58 100.49 -2 6 1 573.84 157.38 -6 4 -2 31.00 68.59 6 -4 2 44.00 80.39 -2 6 2 65.69 56.79 2 -6 -3 164.38 79.39 -6 4 -3 119.59 92.49 6 -4 3 207.28 95.39 -2 6 3 82.09 63.09 2 -6 -4 29.20 82.59 -6 4 -4 290.17 111.09 6 -4 4 434.96 127.69 -2 6 4 59.99 68.29 2 -6 -5 1.30 35.70 -6 4 -6 26.70 48.60 3 -6 1 220.88 82.59 -3 6 -1 405.06 120.19 -6 3 0 48.90 67.39 6 -3 0 151.38 96.29 3 -6 -1 48.40 75.59 -6 3 -1 44.40 56.49 6 -3 1 57.49 108.79 -3 6 1 100.49 75.89 3 -6 -2 67.49 66.59 -6 3 -2 75.09 71.19 6 -3 2 67.09 96.19 -3 6 2 150.88 85.79 3 -6 -3 25.30 86.59 -6 3 -3 56.99 63.29 6 -3 3 77.79 71.49 -3 6 3 90.89 76.89 6 -3 4 166.48 80.09 -3 6 4 -35.50 68.99 -6 3 -6 170.88 73.39 2 4 4 334.07 86.19 4 -6 2 105.29 67.39 -4 6 -2 159.68 74.39 4 -6 1 582.84 161.48 -4 6 -1 896.61 237.38 4 -6 0 420.96 135.79 -4 6 0 598.24 178.38 4 -6 -1 91.79 70.59 -6 2 -1 210.48 81.79 6 -2 1 176.48 101.29 -4 6 1 77.39 89.39 4 -6 -2 287.27 113.89 6 -2 2 197.28 101.49 -4 6 2 380.16 126.99 4 -6 -3 -22.10 74.29 -6 2 -3 82.49 69.49 6 -2 3 89.69 73.09 -4 6 3 36.50 74.99 4 -6 -4 3.80 34.70 -6 2 -4 15.20 56.99 6 -2 4 -98.19 72.09 -6 2 -5 34.60 63.29 -6 2 -6 91.99 58.49 1 5 4 42.10 33.90 -5 6 -4 113.49 67.19 -1 -5 -4 32.40 40.90 1 5 3 229.18 65.79 5 -6 3 99.99 66.89 5 -6 2 431.36 130.09 -5 6 -2 323.77 115.19 5 -6 1 308.27 115.79 5 -6 0 71.19 93.59 -5 6 0 53.69 70.29 5 -6 -1 86.99 77.19 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60.29 1 -7 -3 86.39 63.29 -7 6 -3 101.99 89.19 7 -6 3 148.59 95.19 -1 7 3 64.99 52.89 -7 6 -4 124.29 84.29 7 -6 4 96.99 71.89 -1 7 4 14.90 51.89 -7 6 -5 37.30 58.29 -1 7 5 -3.80 48.70 5 2 4 9.80 44.70 7 -5 -2 52.69 75.99 7 -5 -1 -82.59 83.49 -7 5 0 97.79 97.89 7 -5 0 58.29 110.69 -2 7 0 335.07 101.49 -7 5 -1 34.00 90.09 7 -5 1 104.69 87.19 -2 7 1 119.49 58.69 -7 5 -2 309.07 120.89 7 -5 2 131.89 88.29 -2 7 2 324.67 107.89 2 -7 -3 46.50 58.69 -7 5 -3 9.40 62.09 7 -5 3 70.29 77.89 -2 7 3 37.20 51.09 -7 5 -4 38.80 63.99 -2 7 4 30.10 60.19 -7 5 -5 -22.00 51.19 -2 7 5 -10.10 65.39 -7 5 -6 34.00 55.29 -4 -3 -6 26.00 25.20 4 3 5 3.70 25.70 3 -7 1 50.09 57.49 7 -4 -1 25.50 77.59 -3 7 -1 103.59 64.19 3 -7 0 45.20 62.89 7 -4 0 -3.00 86.49 -3 7 0 60.29 61.89 3 -7 -1 285.87 102.19 -7 4 -1 -49.00 93.39 7 -4 1 43.10 104.39 -3 7 1 174.78 80.39 3 -7 -2 207.18 86.09 -7 4 -2 182.78 86.19 7 -4 2 223.68 114.79 -3 7 2 102.29 66.59 -7 4 -3 35.70 66.89 7 -4 3 -48.80 72.29 -3 7 3 51.99 70.89 -7 4 -4 68.99 87.39 -3 7 4 34.10 67.29 -7 4 -6 81.69 63.49 4 -7 2 568.14 160.18 -4 7 -2 832.72 222.58 4 -7 1 142.49 70.59 -4 7 -1 179.18 77.29 4 -7 0 471.65 151.08 -4 7 0 465.55 141.79 4 -7 -1 30.60 72.29 -7 3 -1 -14.30 55.29 7 -3 1 51.99 96.59 4 -7 -2 17.80 65.19 -7 3 -2 97.19 96.89 7 -3 2 23.00 86.69 -4 7 2 112.59 86.59 4 -7 -3 56.49 90.49 -7 3 -3 -12.60 69.79 7 -3 3 33.90 75.69 -4 7 3 31.30 76.69 -4 7 4 -12.40 84.39 -7 3 -5 -6.30 60.89 -7 3 -6 25.40 49.90 2 5 5 11.20 23.80 -2 -5 -5 -14.70 25.70 5 -7 3 77.69 63.49 -5 7 -3 80.49 67.29 5 -7 2 130.39 69.29 -5 7 -2 188.48 83.19 5 -7 1 96.09 82.29 -5 7 -1 29.70 68.99 5 -7 0 205.18 96.39 -5 7 0 187.88 85.79 5 -7 -1 35.20 71.39 -7 2 -1 -31.60 47.80 7 -2 1 24.80 77.89 -5 7 1 147.69 88.39 5 -7 -2 -28.80 83.79 -7 2 -2 23.20 43.80 7 -2 2 -7.10 74.19 -5 7 2 83.19 81.49 -7 2 -3 45.20 82.29 7 -2 3 -1.50 81.59 -5 7 3 6.30 70.49 -7 2 -4 21.50 58.69 -5 7 4 -0.90 76.99 -7 2 -5 22.70 62.59 1 6 5 0.00 36.80 -6 7 -5 3.50 53.89 -1 -6 -5 -40.40 33.00 1 6 4 63.09 37.10 6 -7 4 33.00 56.29 -6 7 -4 85.19 63.39 -1 -6 -4 46.50 36.60 6 -7 3 106.59 67.59 -6 7 -3 127.59 71.79 6 -7 2 34.00 71.89 -6 7 -2 98.29 76.19 6 -7 1 -34.90 85.19 -6 7 -1 -6.20 79.19 6 -7 0 367.16 137.39 -6 7 0 447.76 143.59 6 -7 -1 -83.09 83.49 -6 7 1 23.40 87.79 6 -7 -2 4.80 91.19 -7 1 -2 -4.60 44.10 7 -1 2 1.70 79.99 -6 7 2 59.69 88.99 -7 1 -3 -0.40 38.70 -6 7 3 107.19 99.49 -7 1 -4 4.30 71.89 -7 1 -5 17.30 50.89 0 7 5 -1.90 42.30 -7 7 -5 -1.50 50.39 0 7 4 24.50 44.40 7 -7 4 22.90 56.39 -7 7 -4 19.20 54.59 0 7 3 48.70 42.40 7 -7 3 46.70 65.99 -7 7 -3 60.19 65.79 0 -7 -3 21.70 42.20 7 -7 2 20.00 94.89 -7 7 -2 16.30 72.29 7 -7 1 100.79 86.29 -7 7 -1 90.79 77.59 7 -7 0 160.88 97.29 -7 7 0 231.18 118.09 7 -7 -1 -5.30 93.09 -7 7 1 41.10 98.69 7 -7 -2 22.30 80.69 -7 7 2 95.79 83.19 -7 0 -3 25.70 44.20 -7 7 3 -45.60 81.49 -7 0 -4 10.10 40.70 -7 0 -5 -21.90 53.59 -7 -1 -4 22.00 38.10 -8 7 3 62.49 88.99 8 -7 -2 53.69 87.99 -8 7 1 53.89 84.89 8 -7 -1 49.10 100.79 -8 7 0 40.00 84.39 8 -7 0 0.80 102.39 -8 7 -1 47.60 76.29 8 -7 1 33.80 80.09 -8 7 -2 54.49 77.19 8 -7 2 -20.70 78.49 -1 8 2 77.99 48.70 -8 7 -3 27.90 71.49 8 -7 3 16.10 73.39 -1 8 3 28.40 47.10 -8 7 -4 34.10 58.79 -1 8 4 4.10 41.60 -6 -2 -5 -3.40 23.20 -8 6 2 23.00 58.09 8 -6 -2 -2.30 79.39 8 -6 -1 49.00 97.69 -8 6 0 59.79 99.29 8 -6 0 -7.80 104.69 -8 6 -1 -12.10 95.39 8 -6 1 45.30 83.29 -2 8 1 46.60 49.10 -8 6 -2 80.99 76.89 8 -6 2 3.10 75.19 -2 8 2 75.39 59.09 -8 6 -3 8.10 59.79 8 -6 3 -0.70 80.69 -2 8 3 25.90 52.09 -8 6 -4 73.79 70.99 -2 8 4 14.90 57.09 -2 8 5 -15.00 42.90 8 -5 -1 72.29 80.49 3 -8 0 308.07 101.79 -8 5 0 76.99 89.89 8 -5 0 25.90 93.79 3 -8 -1 207.28 81.29 -8 5 -1 24.10 88.39 8 -5 1 -33.60 105.89 -3 8 1 89.69 65.09 -8 5 -2 50.19 72.29 8 -5 2 31.30 90.49 -3 8 2 7.90 61.49 -8 5 -3 11.80 62.99 -3 8 3 103.09 70.99 -8 5 -4 42.40 76.69 -3 8 4 39.00 63.19 -8 5 -5 38.90 61.09 -3 8 5 -10.50 55.49 -4 8 -2 267.77 95.39 4 -8 1 44.10 54.99 4 -8 0 199.88 82.59 -8 4 0 38.90 70.59 8 -4 0 -58.59 83.89 -4 8 0 193.08 84.79 4 -8 -1 58.99 69.69 -8 4 -1 59.59 82.19 8 -4 1 19.70 85.19 -8 4 -2 14.30 100.59 8 -4 2 22.00 90.59 -4 8 2 21.10 67.89 -8 4 -3 19.60 70.59 -4 8 3 6.90 68.49 -8 4 -4 2.10 62.59 -4 8 4 9.30 72.29 -8 4 -5 -4.30 75.39 -4 8 5 7.90 77.29 5 -8 3 44.70 58.49 -5 8 -3 17.40 56.69 5 -8 2 46.80 58.49 5 -8 1 93.79 69.39 -5 8 -1 139.19 74.79 5 -8 0 60.59 71.99 -5 8 0 8.50 61.19 5 -8 -1 71.79 72.69 -8 3 -1 33.00 54.59 8 -3 1 22.50 77.19 -5 8 1 21.60 63.49 -8 3 -2 40.70 44.60 -8 3 -3 81.29 80.99 -5 8 3 -6.90 87.59 -5 8 4 18.30 72.09 -8 3 -5 -14.20 53.79 -5 8 5 20.00 78.29 6 -8 4 91.19 63.39 -6 8 -4 152.58 77.69 6 -8 3 46.30 63.59 -6 8 -3 56.89 60.19 6 -8 2 201.88 85.99 -6 8 -2 91.39 73.79 6 -8 1 -24.30 74.79 -6 8 -1 16.50 70.79 6 -8 0 69.19 77.49 -6 8 0 8.30 61.09 6 -8 -1 21.70 82.79 -6 8 1 32.80 74.29 -8 2 -2 5.60 54.99 -6 8 2 94.19 80.69 -6 8 3 -10.20 82.29 -8 2 -4 10.40 79.19 -6 8 4 -101.49 91.39 -7 8 -4 57.89 60.89 7 -8 3 86.89 69.09 -7 8 -3 42.00 70.49 7 -8 2 84.79 83.69 -7 8 -2 41.60 72.09 7 -8 1 21.30 88.39 -7 8 -1 -11.50 57.19 7 -8 0 16.70 77.29 -7 8 0 67.99 84.59 7 -8 -1 81.29 92.89 -7 8 1 37.30 83.09 -7 8 2 40.00 81.89 -7 8 3 -63.89 73.89 -8 1 -4 6.50 63.49 -7 8 4 -34.70 76.49 0 8 3 26.30 35.50 8 -8 3 25.40 71.59 -8 8 -3 4.30 60.59 8 -8 2 13.10 77.69 -8 8 -2 26.80 60.99 8 -8 1 5.70 94.89 -8 8 -1 -34.50 59.69 8 -8 0 80.89 85.49 -8 8 0 35.80 87.19 8 -8 -1 56.59 94.69 -8 8 1 -1.10 79.09 -8 8 2 9.00 81.49 -8 8 3 32.00 90.59 -9 8 2 38.40 75.89 -9 8 1 16.80 84.69 9 -8 -1 52.39 102.39 -9 8 0 28.10 75.39 9 -8 0 -76.59 84.59 -9 8 -1 13.50 72.39 9 -8 1 9.10 77.09 -9 8 -2 38.80 64.09 9 -8 2 33.10 79.39 -1 9 2 49.30 44.30 -9 7 2 -57.19 56.49 9 -7 -2 62.29 80.09 -9 7 1 77.89 87.19 9 -7 -1 59.29 86.89 -9 7 0 -46.10 87.99 9 -7 0 32.40 106.29 -9 7 -1 36.50 88.09 9 -7 1 -56.09 79.89 -2 9 1 89.39 54.49 -9 7 -2 15.10 69.69 9 -7 2 25.10 75.19 -2 9 2 2.20 43.00 -9 7 -3 9.50 55.29 -2 9 3 19.50 44.00 9 -6 -2 82.79 79.99 -9 6 1 -82.49 71.29 9 -6 -1 1.70 80.79 -9 6 0 -29.60 83.69 9 -6 0 44.20 88.29 9 -6 1 9.10 94.89 -3 9 1 51.49 53.29 -9 6 -2 -19.00 69.19 -3 9 2 26.20 50.29 -9 6 -3 39.90 73.89 -3 9 3 26.50 47.70 -9 6 -4 40.20 66.89 -9 5 1 -16.70 49.00 9 -5 -1 45.50 78.59 -4 9 -1 79.29 60.29 9 -5 0 5.20 86.79 -4 9 0 130.69 67.79 -9 5 -1 19.00 90.59 9 -5 1 -23.10 109.09 -4 9 1 11.80 53.69 -9 5 -2 16.60 79.79 -4 9 2 59.69 57.29 -9 5 -3 -28.30 71.99 -4 9 3 -12.30 68.99 -9 5 -4 7.80 67.89 -4 9 4 -19.30 65.59 -5 9 -3 94.89 62.29 5 -9 2 18.00 52.19 -5 9 -2 17.70 53.39 -5 9 -1 -5.10 48.80 -9 4 0 -12.40 53.09 9 -4 0 4.10 83.59 -5 9 0 27.10 54.99 -5 9 1 15.70 67.39 -9 4 -2 -33.00 57.69 -5 9 2 -12.10 58.09 -9 4 -3 71.29 79.59 -5 9 3 -18.30 65.49 -9 4 -4 -56.89 64.39 -5 9 4 -14.70 59.99 -6 9 -4 74.59 69.99 6 -9 3 4.30 52.29 -6 9 -3 22.50 51.69 6 -9 2 95.39 64.69 -6 9 -2 63.29 56.69 -6 9 -1 41.80 59.19 -6 9 0 64.99 65.39 -9 3 -1 26.30 48.70 -6 9 1 -43.20 67.89 -9 3 -2 10.90 55.39 -6 9 2 100.59 89.89 -9 3 -3 7.90 79.39 7 -9 3 28.30 53.99 -7 9 -3 1.40 49.30 -7 9 -2 98.99 68.59 7 -9 1 73.79 79.39 -7 9 -1 55.39 78.39 -7 9 0 -13.70 54.19 -7 9 1 33.10 73.09 -9 2 -2 0.40 46.20 -7 9 2 17.60 71.49 -7 9 3 -5.90 78.49 8 -9 2 54.69 77.39 8 -9 1 12.30 73.79 -8 9 -1 9.80 52.49 -8 9 0 19.70 69.69 -8 9 1 74.29 79.19 -8 9 2 80.39 83.39 -9 9 0 8.40 85.99 -9 9 1 -10.50 79.89 10 -7 -1 0.00 88.09 -10 7 0 35.20 87.39 10 -7 0 -1.70 108.39 -10 7 -1 57.19 92.99 10 -7 1 20.90 101.09 -10 6 1 22.80 70.39 10 -6 -1 15.10 75.09 -4 10 -1 72.99 55.19 10 -6 0 -1.50 96.89 -4 10 0 36.20 50.19 -10 6 -1 -1.90 78.19 -4 10 1 -9.40 55.89 -10 6 -2 11.60 81.99 -5 10 -2 125.99 75.29 -5 10 -1 36.10 52.49 -10 5 0 62.59 71.59 -5 10 0 60.29 62.19 -10 5 -1 19.60 89.19 -5 10 1 1.90 49.00 -10 5 -2 28.00 85.59 -6 10 -2 47.20 56.69 -6 10 -1 55.69 61.29 -6 10 0 26.10 54.29 -10 4 -1 43.80 55.99 -6 10 1 4.20 50.69 -10 4 -2 -18.10 52.39 -7 10 -1 -15.10 56.29 -7 10 0 18.30 55.09 -7 10 1 43.40 56.79 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 61805 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 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 N1 N 0.761(4) 0.787(3) 0.758(4) 0.038(4) Uiso 1 1 d D . H1 H 0.780745 0.744100 0.926119 0.046 Uiso 1 1 calc R U H3 H 0.706135 0.893163 0.769362 0.046 Uiso 1 1 calc R U H2 H 0.904223 0.856791 0.669761 0.046 Uiso 1 1 calc R U C1 C 0.610(4) 0.602(4) 0.632(2) 0.038(4) Uiso 1 1 d D . H5 H 0.454281 0.560896 0.691718 0.046 Uiso 1 1 calc R U H4 H 0.635517 0.473784 0.677852 0.046 Uiso 1 1 calc R U C2 C 0.615(3) 0.621(3) 0.374(3) 0.038(4) Uiso 1 1 d D . O1 O 0.761(3) 0.795(3) 0.284(4) 0.038(4) Uiso 1 1 d D . O2 O 0.483(4) 0.469(3) 0.249(4) 0.038(4) Uiso 1 1 d D . 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 116.0(17) O1 C2 O2 122(2) O1 C2 C1 117.2(16) O2 C2 C1 120.4(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C1 1.45(2) C1 C2 1.491(19) C2 O1 1.30(2) C2 O2 1.28(2)