#------------------------------------------------------------------------------ #$Date: 2019-01-16 05:24:05 +0200 (Wed, 16 Jan 2019) $ #$Revision: 213112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242814.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_2242814 loop_ _publ_author_name 'Kamaal, Saima' 'Faizi, Md. Serajul Haque' 'Ali, Arif' 'Ahmad, Musheer' 'Gupta, Mayank' 'Dege, Necmi' 'Iskenderov, Turganbay' _publ_section_title ; Crystal structure of 4-[(2-hydroxy-3-methoxybenzyl)amino]benzoic acid hemihydrate ; _journal_coeditor_code LD2147 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 159 _journal_page_last 162 _journal_paper_doi 10.1107/S2056989018018455 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '2C15 H15 N O4, H2 O' _chemical_formula_moiety '2(C15 H15 N O4), H2 O' _chemical_formula_sum 'C30 H32 N2 O9' _chemical_formula_weight 564.57 _chemical_name_systematic ; 4-[(2-Hydroxy-3-methoxybenzyl)amino]benzoic acid hemihydrate ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 98.292(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 24.742(3) _cell_length_b 5.5002(6) _cell_length_c 19.387(2) _cell_measurement_reflns_used 6409 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.17 _cell_measurement_theta_min 2.50 _cell_volume 2610.7(5) _computing_cell_refinement ; SAINT (Bruker, 2014) ; _computing_data_collection ; APEX2 (Bruker, 2014) ; _computing_data_reduction ; SAINT (Bruker, 2014) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_unetI/netI 0.0402 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 16146 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 2.880 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2014) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.436 _exptl_crystal_description prism _exptl_crystal_F_000 1192 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.257 _refine_diff_density_min -0.218 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 203 _refine_ls_number_reflns 2570 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0417 _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^)+(0.0366P)^2^+3.8398P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.1073 _reflns_number_gt 2138 _reflns_number_total 2570 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ld2147sup1.cif _cod_data_source_block I _cod_original_cell_volume 2610.8(5) _cod_database_code 2242814 _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_estimated_absorpt_t_min 0.975 _shelx_estimated_absorpt_t_max 0.979 _shelx_hkl_file ; -1 1 0 2850.81 166.88 -1 1 0 2714.33 172.78 1 -1 0 2744.03 172.68 1 -1 0 2849.31 167.18 -2 2 0 1377.16 90.89 -2 2 0 1100.49 79.09 -2 2 0 1372.26 77.99 2 -2 0 1231.08 88.59 2 -2 0 1298.17 78.59 -3 3 0 11.30 4.10 -3 3 0 10.90 7.00 -3 3 0 20.20 2.70 3 -3 0 14.60 4.00 -4 4 0 753.92 53.69 -4 4 0 771.12 48.90 -4 4 0 791.92 72.49 4 -4 0 779.92 59.19 4 -4 0 738.93 51.19 -5 5 0 156.98 35.50 -5 5 0 159.88 13.60 -5 5 0 188.28 19.20 5 -5 0 147.99 21.80 5 -5 0 160.78 15.70 -6 6 0 38.60 10.90 -6 6 0 -16.10 16.50 6 -6 0 26.50 6.70 -7 7 0 45.40 20.90 -7 7 0 61.99 16.00 7 -7 0 56.69 17.60 5 -7 0 28.10 11.20 -5 7 0 10.10 7.70 -5 7 0 15.00 21.50 4 -6 0 4.60 4.60 4 -6 0 -3.90 5.60 -4 6 0 6.40 13.70 3 -5 0 186.98 19.10 -3 5 0 235.58 37.10 -3 5 0 231.38 21.30 2 -4 0 140.89 14.30 -2 4 0 177.18 28.40 -2 4 0 156.68 12.70 -2 4 0 151.88 15.50 1 -3 0 907.21 56.99 -1 3 0 769.82 56.89 -1 3 0 952.80 55.59 -1 3 0 863.81 72.29 0 -2 0 1618.64 113.29 0 -2 0 1745.03 103.19 0 2 0 1431.46 102.79 0 2 0 1790.02 115.69 0 2 0 1843.32 102.59 -1 -1 0 2711.73 174.58 1 1 0 2682.83 174.98 1 1 0 3043.40 168.98 -3 1 0 38.90 4.60 -3 1 0 41.60 3.80 -3 1 0 44.80 5.10 -3 1 0 50.89 7.70 3 -1 0 49.10 5.50 3 -1 0 39.30 7.60 3 -1 0 42.60 3.80 -4 2 0 772.72 58.39 -4 2 0 767.02 46.90 -4 2 0 671.03 48.80 4 -2 0 707.63 56.89 4 -2 0 782.22 47.30 4 -2 0 795.02 51.59 -5 3 0 798.52 65.99 -5 3 0 682.93 51.99 -5 3 0 779.92 48.70 5 -3 0 809.02 49.99 5 -3 0 788.82 56.09 -6 4 0 303.97 39.60 -6 4 0 276.87 25.50 -6 4 0 301.67 20.90 6 -4 0 297.87 29.80 6 -4 0 305.17 22.60 -7 5 0 -1.70 10.40 -7 5 0 8.10 5.30 7 -5 0 6.90 3.50 7 -5 0 -3.00 6.00 -8 6 0 42.50 21.30 -8 6 0 42.90 11.60 8 -6 0 33.00 14.20 8 -6 0 29.50 5.80 -9 7 0 -10.00 17.60 9 -7 0 5.10 10.80 3 -7 0 -0.20 6.00 -3 7 0 12.80 16.70 -3 7 0 6.60 4.70 2 -6 0 383.46 33.30 2 -6 0 453.55 44.80 -2 6 0 392.16 56.59 -2 6 0 433.46 36.10 1 -5 0 355.76 30.00 -1 5 0 367.26 49.10 -1 5 0 400.76 31.40 0 -4 0 15.20 4.80 0 4 0 13.20 13.00 0 4 0 13.30 4.60 -1 -3 0 712.73 53.09 1 3 0 922.91 52.89 1 3 0 856.31 70.29 1 3 0 795.62 53.19 -2 -2 0 1255.27 91.89 -2 -2 0 1391.46 82.19 2 2 0 1400.56 81.59 2 2 0 1185.18 92.39 -3 -1 0 48.70 7.60 -3 -1 0 52.69 4.90 3 1 0 42.80 3.50 3 1 0 49.90 9.50 3 1 0 51.69 4.80 -4 0 0 436.16 27.70 -4 0 0 342.47 25.30 -4 0 0 423.06 26.00 4 0 0 433.86 27.80 4 0 0 415.66 25.40 4 0 0 410.86 25.90 -5 1 0 1569.44 90.19 -5 1 0 1352.36 87.29 -5 1 0 1442.86 87.49 -5 1 0 1246.08 88.49 5 -1 0 1527.35 94.99 5 -1 0 1524.45 87.29 5 -1 0 1457.55 90.09 -6 2 0 1077.29 75.29 -6 2 0 891.51 64.89 -6 2 0 988.30 62.59 6 -2 0 1048.40 62.49 6 -2 0 1071.79 67.79 6 -2 0 1013.20 74.29 -7 3 0 105.29 21.90 -7 3 0 73.59 7.10 -7 3 0 61.29 9.20 7 -3 0 85.79 11.90 7 -3 0 73.59 7.20 -8 4 0 139.09 10.90 -8 4 0 134.89 28.60 -8 4 0 152.28 16.80 8 -4 0 124.69 11.40 8 -4 0 147.09 19.10 -9 5 0 72.09 6.80 -9 5 0 56.69 20.80 -9 5 0 88.79 15.80 9 -5 0 68.39 7.60 9 -5 0 74.79 16.40 -10 6 0 108.99 20.00 10 -6 0 74.19 18.70 1 -7 0 35.50 9.00 1 -7 0 33.70 11.80 -1 7 0 46.50 12.00 -1 7 0 34.40 23.90 0 -6 0 57.89 12.30 0 6 0 90.19 12.90 0 6 0 68.19 25.80 -1 -5 0 396.06 32.20 1 5 0 407.76 31.90 1 5 0 393.76 51.49 -2 -4 0 146.89 14.80 2 4 0 159.38 14.60 2 4 0 150.28 31.40 -3 -3 0 11.50 3.60 -3 -3 0 21.80 3.80 3 3 0 12.20 3.80 3 3 0 20.80 9.80 3 3 0 13.90 3.30 -4 -2 0 840.42 49.20 -4 -2 0 723.83 58.09 4 2 0 656.43 46.40 4 2 0 733.63 59.89 4 2 0 805.42 48.60 -5 -1 0 1598.04 102.69 -5 -1 0 1611.94 96.39 5 1 0 1596.04 103.69 5 1 0 1489.25 96.19 -6 0 0 176.48 14.10 -6 0 0 147.69 11.70 -6 0 0 150.58 11.20 6 0 0 155.58 11.90 6 0 0 184.48 14.70 -7 1 0 857.51 62.79 -7 1 0 984.50 61.89 -7 1 0 963.90 64.29 -7 1 0 1063.19 62.09 7 -1 0 1015.50 65.09 7 -1 0 1113.39 61.79 -8 2 0 1609.24 99.79 -8 2 0 1402.16 97.79 -8 2 0 1422.36 94.99 -8 2 0 1545.35 94.79 8 -2 0 1622.74 100.69 8 -2 0 1681.53 94.69 8 -2 0 1585.14 108.19 -9 3 0 181.68 14.10 -9 3 0 185.18 18.10 9 -3 0 186.38 13.70 9 -3 0 183.78 20.00 -10 4 0 21.40 3.70 -10 4 0 31.00 8.90 10 -4 0 23.40 4.20 10 -4 0 21.60 7.10 -11 5 0 167.88 19.80 -11 5 0 140.29 10.10 -11 5 0 122.29 10.40 11 -5 0 139.19 20.80 11 -5 0 132.39 10.30 -12 6 0 41.70 12.70 12 -6 0 -3.60 9.00 -1 -7 0 26.90 8.90 1 7 0 18.80 17.10 1 7 0 24.30 9.40 -2 -6 0 394.26 34.30 2 6 0 311.07 51.59 2 6 0 457.85 34.40 -3 -5 0 199.98 20.70 3 5 0 223.78 19.60 3 5 0 170.78 38.60 -4 -4 0 742.03 53.49 4 4 0 804.82 51.49 4 4 0 756.82 73.69 -5 -3 0 805.12 55.39 -5 -3 0 864.91 52.49 5 3 0 847.82 52.79 5 3 0 773.02 70.79 -6 -2 0 1166.58 69.69 -6 -2 0 1085.39 65.89 6 2 0 1016.10 80.99 6 2 0 1107.29 65.89 6 2 0 1039.60 68.99 -7 -1 0 1054.59 64.39 -7 -1 0 1067.89 70.79 7 1 0 964.10 71.29 7 1 0 982.90 64.19 -8 0 0 157.08 11.30 -8 0 0 129.49 10.90 -8 0 0 130.59 10.30 -8 0 0 133.99 13.20 8 0 0 133.09 13.80 8 0 0 134.19 11.10 -9 1 0 22.70 4.10 -9 1 0 11.90 4.00 -9 1 0 25.50 4.80 -9 1 0 23.50 4.00 9 -1 0 26.80 3.90 9 -1 0 18.40 5.10 -10 2 0 163.68 12.80 -10 2 0 148.79 15.10 -10 2 0 166.58 18.40 -10 2 0 152.68 12.80 10 -2 0 168.88 12.40 10 -2 0 180.18 25.40 10 -2 0 178.08 17.50 -11 3 0 43.60 5.00 -11 3 0 42.20 5.20 -11 3 0 36.50 8.80 11 -3 0 29.90 8.40 11 -3 0 41.50 4.70 -12 4 0 2.30 2.00 -12 4 0 5.60 4.50 -12 4 0 6.70 2.70 12 -4 0 10.20 7.10 12 -4 0 8.30 2.50 -13 5 0 29.50 3.20 -13 5 0 22.20 9.20 -13 5 0 29.40 3.20 13 -5 0 36.60 12.80 -14 6 0 129.99 22.90 14 -6 0 97.99 22.90 -3 -7 0 11.00 5.50 3 7 0 10.90 11.40 3 7 0 1.30 4.60 -4 -6 0 6.90 4.10 4 6 0 12.70 3.50 4 6 0 7.80 13.40 -5 -5 0 174.38 18.30 5 5 0 110.29 33.00 5 5 0 183.68 16.40 -6 -4 0 286.07 25.40 -6 -4 0 307.67 22.20 6 4 0 254.27 39.00 6 4 0 328.17 22.80 -7 -3 0 85.59 7.30 -7 -3 0 86.89 10.10 7 3 0 86.39 7.40 7 3 0 82.59 20.80 -8 -2 0 1738.23 103.49 8 2 0 1520.55 115.79 -9 -1 0 19.40 2.00 -9 -1 0 14.40 5.60 -9 -1 0 18.10 4.00 9 1 0 15.00 5.80 9 1 0 19.10 4.30 -10 0 0 217.18 19.00 -10 0 0 165.58 15.20 -10 0 0 221.58 15.20 10 0 0 200.48 19.60 10 0 0 208.08 16.00 -11 1 0 3063.09 190.38 -11 1 0 3018.80 188.08 -11 1 0 3056.79 186.68 -11 1 0 2962.90 186.58 11 -1 0 3297.17 192.38 -12 2 0 408.16 31.80 -12 2 0 466.05 35.20 -12 2 0 525.05 32.20 12 -2 0 480.35 37.80 -13 3 0 101.89 13.70 -13 3 0 95.59 10.20 -13 3 0 135.29 10.70 13 -3 0 118.99 16.30 -14 4 0 10.90 2.80 -14 4 0 7.90 4.40 -14 4 0 14.90 3.70 14 -4 0 4.20 5.00 -15 5 0 719.93 58.99 15 -5 0 746.43 63.39 -16 6 0 4.50 4.60 16 -6 0 -8.70 7.10 -5 -7 0 15.70 8.90 5 7 0 17.00 7.20 5 7 0 -12.90 20.20 -6 -6 0 35.00 9.10 6 6 0 24.40 7.30 6 6 0 8.00 18.50 -7 -5 0 7.20 4.80 7 5 0 15.80 4.40 7 5 0 20.40 9.90 -8 -4 0 152.28 15.70 -8 -4 0 123.59 10.90 8 4 0 148.19 11.70 8 4 0 79.39 24.00 -9 -3 0 173.28 12.50 -9 -3 0 204.98 17.70 9 3 0 185.18 12.60 9 3 0 170.18 27.50 -10 -2 0 165.88 15.00 10 2 0 159.88 23.90 -11 -1 0 3012.00 182.28 -11 -1 0 3096.19 186.18 11 1 0 3013.60 195.98 -12 0 0 2572.54 165.18 -12 0 0 2802.72 164.28 12 0 0 2725.43 172.08 -13 1 0 114.59 11.60 -13 1 0 120.59 10.90 -13 1 0 102.69 10.30 13 -1 0 103.19 13.80 -14 2 0 20.20 3.70 -14 2 0 14.40 3.90 -14 2 0 8.70 4.70 14 -2 0 14.50 6.60 -15 3 0 2.20 1.90 -15 3 0 3.60 4.60 -15 3 0 7.70 2.90 15 -3 0 4.60 5.00 -16 4 0 1243.48 87.99 -16 4 0 1588.74 100.49 -16 4 0 1389.26 87.89 16 -4 0 1554.24 104.09 -17 5 0 12.70 7.80 17 -5 0 1.90 6.40 -18 6 0 221.98 28.00 18 -6 0 145.49 28.70 -7 -7 0 47.80 13.30 7 7 0 72.89 26.60 7 7 0 51.09 12.40 -8 -6 0 17.30 7.60 8 6 0 34.50 21.20 8 6 0 44.40 8.70 -9 -5 0 57.89 12.30 9 5 0 56.99 7.70 9 5 0 22.60 16.70 -10 -4 0 28.00 3.60 -10 -4 0 24.00 7.60 10 4 0 30.10 15.10 10 4 0 29.00 3.90 -11 -3 0 38.10 8.00 11 3 0 27.80 11.10 -12 -2 0 464.95 34.50 12 2 0 477.15 47.10 -13 -1 0 93.49 8.10 -13 -1 0 109.49 11.20 13 1 0 112.09 17.30 -14 0 0 379.66 28.50 -14 0 0 378.06 27.20 14 0 0 409.46 35.30 -15 1 0 258.67 22.10 -15 1 0 280.07 21.50 15 -1 0 276.77 26.90 -16 2 0 37.60 8.60 -16 2 0 36.50 6.70 16 -2 0 36.50 10.60 -17 3 0 841.32 61.09 -17 3 0 833.02 53.99 17 -3 0 788.12 63.59 -18 4 0 36.90 6.60 -18 4 0 38.20 10.60 -18 4 0 31.30 5.60 18 -4 0 38.10 11.30 -19 5 0 27.60 10.20 19 -5 0 57.89 13.90 -9 -7 0 11.70 6.50 9 7 0 31.60 22.20 -10 -6 0 83.69 16.00 10 6 0 78.69 10.70 10 6 0 75.69 30.10 -11 -5 0 120.09 10.10 -11 -5 0 125.79 16.40 11 5 0 104.69 27.80 11 5 0 116.29 10.60 -12 -4 0 7.70 5.10 12 4 0 8.30 10.00 -13 -3 0 128.29 14.30 13 3 0 96.39 23.60 -14 -2 0 11.20 4.40 14 2 0 7.60 9.10 -15 -1 0 258.37 19.80 -15 -1 0 297.77 23.80 15 1 0 216.58 28.90 15 1 0 337.47 19.50 -16 0 0 10.40 3.90 -16 0 0 9.50 3.40 16 0 0 12.60 4.10 16 0 0 7.40 5.90 -17 1 0 836.02 56.89 -17 1 0 814.42 55.69 17 -1 0 837.52 63.69 -18 2 0 791.02 60.79 -18 2 0 930.11 58.19 18 -2 0 859.81 66.69 -19 3 0 136.69 17.20 -19 3 0 104.89 11.60 19 -3 0 94.69 19.70 -20 4 0 91.59 17.90 -20 4 0 41.90 7.20 20 -4 0 69.19 18.10 -21 5 0 59.69 16.40 21 -5 0 30.00 12.80 -12 -6 0 55.19 12.50 12 6 0 66.29 30.60 -13 -5 0 30.90 8.90 13 5 0 6.30 15.10 -14 -4 0 8.20 4.80 14 4 0 3.80 7.60 -15 -3 0 5.40 3.70 15 3 0 4.90 8.70 -16 -2 0 28.60 7.20 16 2 0 31.50 13.80 -17 -1 0 791.62 53.19 -17 -1 0 727.03 48.30 17 1 0 721.53 63.89 17 1 0 762.62 47.30 -18 0 0 33.00 6.10 -18 0 0 34.20 7.60 18 0 0 51.49 13.80 -19 1 0 65.29 9.50 -19 1 0 75.39 10.60 19 -1 0 82.19 17.30 -20 2 0 97.19 13.20 -20 2 0 69.79 9.90 20 -2 0 89.59 18.20 -21 3 0 9.60 4.20 -21 3 0 8.70 6.10 21 -3 0 10.90 6.20 -22 4 0 68.39 9.20 -22 4 0 76.29 17.00 22 -4 0 81.89 18.40 -23 5 0 3.20 3.20 23 -5 0 9.80 12.10 -14 -6 0 126.99 18.00 14 6 0 141.49 41.70 -15 -5 0 624.44 49.99 15 5 0 590.54 73.79 -16 -4 0 1403.26 91.89 16 4 0 1190.68 114.89 -17 -3 0 765.82 54.79 17 3 0 684.33 72.59 -18 -2 0 929.21 61.29 18 2 0 747.83 73.99 -19 -1 0 67.59 10.20 -19 -1 0 60.59 7.40 19 1 0 80.59 7.00 19 1 0 62.29 17.70 -20 0 0 112.59 11.80 -20 0 0 112.79 13.20 20 0 0 79.09 18.10 -21 1 0 67.69 11.80 -21 1 0 59.49 10.80 21 -1 0 64.59 17.30 -22 2 0 486.25 39.10 -22 2 0 439.56 35.20 22 -2 0 484.65 46.20 -23 3 0 67.09 9.50 -23 3 0 76.99 16.60 23 -3 0 77.59 19.40 -24 4 0 3.20 8.50 -24 4 0 9.30 4.60 24 -4 0 -11.60 8.70 -16 -6 0 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334.17 33.20 7 1 -24 -0.60 7.00 -7 -1 24 -0.80 5.70 -7 -1 24 -7.60 7.00 6 2 -24 11.30 7.70 6 2 -24 12.20 7.00 -6 -2 24 -5.20 7.90 -6 -2 24 1.00 5.00 8 -2 -24 57.79 16.70 -8 2 24 31.30 9.70 7 -1 -24 -12.60 6.50 -7 1 24 0.00 5.70 6 0 -24 20.50 9.90 -6 0 24 -2.90 8.40 -6 0 24 9.00 6.20 5 1 -24 45.30 12.00 -5 -1 24 3.60 6.60 -5 -1 24 25.10 9.90 4 2 -24 8.00 5.90 4 2 -24 -4.30 7.30 -4 -2 24 2.90 7.90 -4 -2 24 1.30 5.70 6 -2 -24 -6.80 6.00 -6 2 24 1.20 6.20 5 -1 -24 30.00 11.90 -5 1 24 18.30 10.40 -5 1 24 37.60 11.40 4 0 -24 0.90 9.30 -4 0 24 3.90 7.80 -4 0 24 -7.80 4.30 3 1 -24 2.80 5.40 3 1 -24 5.70 6.80 -3 -1 24 -0.50 5.70 -3 -1 24 9.40 8.90 2 2 -24 -4.60 3.40 2 2 -24 2.40 6.20 -2 -2 24 12.80 6.70 -2 -2 24 5.50 6.10 4 -2 -24 4.00 9.20 -4 2 24 2.40 7.10 3 -1 -24 4.50 7.10 -3 1 24 -10.60 8.50 -3 1 24 4.70 6.00 2 0 -24 101.39 20.80 -2 0 24 92.09 19.10 -2 0 24 91.49 20.70 1 1 -24 5.00 7.10 1 1 -24 -5.90 6.50 -1 -1 24 -10.00 4.50 -1 -1 24 5.00 8.40 0 2 -24 112.89 16.90 0 2 -24 103.99 18.40 0 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42.20 12 0 -25 2.00 7.00 -12 0 25 -9.00 6.10 -11 -1 25 103.69 21.70 -11 1 25 134.69 25.30 10 0 -25 2.80 5.90 -10 0 25 19.30 9.10 9 1 -25 244.48 30.40 -9 -1 25 235.58 27.70 -9 -1 25 300.87 31.50 9 -1 -25 260.37 32.90 -9 1 25 260.77 31.30 8 0 -25 -2.80 5.90 -8 0 25 -11.80 4.90 7 1 -25 4.20 7.90 -7 -1 25 15.90 8.60 -7 -1 25 -3.60 6.40 7 -1 -25 -8.40 5.90 -7 1 25 0.90 7.60 6 0 -25 -3.10 6.90 -6 0 25 -6.10 6.60 -6 0 25 -4.30 5.40 5 1 -25 2.60 5.20 -5 -1 25 -12.50 7.70 -5 -1 25 6.80 8.40 -5 1 25 9.40 5.90 4 0 -25 3.10 6.60 -4 0 25 3.40 8.50 -4 0 25 1.10 4.90 3 1 -25 66.39 17.10 -3 -1 25 61.99 14.10 -3 -1 25 61.49 16.90 3 -1 -25 87.89 18.10 -3 1 25 62.29 13.40 2 0 -25 -3.20 6.80 -2 0 25 8.40 9.00 -2 0 25 -3.90 3.40 1 1 -25 12.80 10.10 1 1 -25 12.10 8.90 -1 -1 25 21.20 10.40 -1 -1 25 4.00 7.10 1 -1 -25 9.10 6.10 -1 1 25 0.90 6.50 -1 1 25 4.60 10.40 0 0 -25 5.50 11.20 0 0 25 -3.50 3.10 0 0 25 13.80 10.50 -1 1 -25 44.00 10.90 -1 1 -25 33.80 12.50 1 -1 25 22.00 11.10 -1 -1 -25 11.80 11.70 1 1 25 23.90 9.70 1 1 25 31.90 11.70 -2 0 -25 7.50 9.40 2 0 25 4.70 9.50 2 0 25 -10.90 7.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 21988 _shelx_res_file ; TITL shelxt_a.res in C2/c shelx.res created by SHELXL-2018/3 at 19:36:57 on 27-Dec-2018 CELL 0.71073 24.7422 5.5002 19.3873 90.000 98.292 90.000 ZERR 4.00 0.0027 0.0006 0.0022 0.000 0.006 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 120 128 8 36 MERG 2 OMIT -2.00 52.00 DFIX 0.82 O5 H5 EQIV $2 -x+3/2, y+1/2, -z+3/2 HTAB O5 O2_$2 EQIV $3 x+1/2, y+1/2, z HTAB O2 O3_$3 HTAB O4 O5 FMAP 2 PLAN 5 ACTA BOND $H CONF LIST 6 L.S. 25 TEMP 0.00 WGHT 0.036600 3.839800 FVAR 0.47194 O2 4 0.956346 0.706969 0.672601 11.00000 0.01223 0.02346 = 0.02620 0.00428 0.00286 -0.00249 O5 4 0.500000 0.790319 0.750000 10.50000 0.01498 0.02438 = 0.02774 0.00000 0.00435 0.00000 O1 4 0.973145 1.083078 0.591822 11.00000 0.01986 0.02123 = 0.03126 0.00634 0.00669 -0.00519 O3 4 0.562420 0.250369 0.659327 11.00000 0.01361 0.02696 = 0.04105 -0.00114 0.00551 -0.00317 O4 4 0.589889 0.607601 0.707366 11.00000 0.01727 0.03656 = 0.05242 -0.01872 0.01265 -0.00005 N1 3 0.817742 0.258287 0.635120 11.00000 0.01372 0.01855 = 0.02800 -0.00336 0.00706 -0.00197 C14 1 0.749746 0.505574 0.680827 11.00000 0.01504 0.01627 = 0.01907 -0.00068 0.00204 -0.00377 AFIX 43 H14 2 0.775566 0.623501 0.696467 11.00000 -1.20000 AFIX 0 C9 1 0.765114 0.298505 0.646272 11.00000 0.01319 0.01687 = 0.01729 0.00305 0.00254 0.00006 C12 1 0.656254 0.362108 0.668728 11.00000 0.01480 0.01923 = 0.01844 0.00239 0.00375 0.00036 C15 1 0.598578 0.398088 0.677922 11.00000 0.01660 0.02201 = 0.02006 0.00129 0.00419 0.00100 C7 1 0.869734 0.625878 0.606214 11.00000 0.01565 0.01839 = 0.02074 -0.00228 0.00838 0.00122 C10 1 0.724765 0.123909 0.623074 11.00000 0.01761 0.01448 = 0.02237 -0.00021 0.00352 0.00038 AFIX 43 H10 2 0.734254 -0.014204 0.599877 11.00000 -1.20000 AFIX 0 C13 1 0.695998 0.533996 0.691604 11.00000 0.01763 0.01715 = 0.01782 -0.00107 0.00393 0.00121 AFIX 43 H13 2 0.686232 0.671711 0.714756 11.00000 -1.20000 AFIX 0 C5 1 0.925427 0.956545 0.572977 11.00000 0.01612 0.01801 = 0.02360 -0.00100 0.00832 0.00001 C6 1 0.917278 0.764066 0.617386 11.00000 0.01488 0.01867 = 0.01978 -0.00203 0.00565 0.00299 C2 1 0.831047 0.678133 0.548202 11.00000 0.01586 0.02323 = 0.02300 -0.00331 0.00377 -0.00072 AFIX 43 H2 2 0.799081 0.587223 0.539822 11.00000 -1.20000 AFIX 0 C8 1 0.863353 0.418723 0.656237 11.00000 0.01162 0.01959 = 0.02461 0.00030 0.00432 -0.00116 AFIX 23 H8A 2 0.896629 0.323016 0.662065 11.00000 -1.20000 H8B 2 0.859392 0.487346 0.701326 11.00000 -1.20000 AFIX 0 C4 1 0.886901 1.005112 0.515418 11.00000 0.02489 0.02151 = 0.02106 0.00339 0.00822 0.00278 AFIX 43 H4 2 0.892432 1.131150 0.485232 11.00000 -1.20000 AFIX 0 C11 1 0.671657 0.155352 0.634318 11.00000 0.01566 0.01503 = 0.02388 0.00093 0.00257 -0.00403 AFIX 43 H11 2 0.645659 0.037923 0.618889 11.00000 -1.20000 AFIX 0 C3 1 0.839971 0.864125 0.503162 11.00000 0.02166 0.02870 = 0.02022 -0.00015 0.00245 0.00180 AFIX 43 H3 2 0.814245 0.895045 0.464242 11.00000 -1.20000 AFIX 0 C1 1 0.984947 1.276508 0.547259 11.00000 0.02904 0.01798 = 0.03505 0.00433 0.01594 -0.00295 AFIX 137 H1A 2 0.986748 1.213811 0.501435 11.00000 -1.50000 H1B 2 1.019360 1.348797 0.565539 11.00000 -1.50000 H1C 2 0.956674 1.397043 0.544826 11.00000 -1.50000 AFIX 0 H5 2 0.515923 0.890523 0.777191 11.00000 0.07562 H1 2 0.824586 0.120279 0.607618 11.00000 0.03829 H2A 2 0.989971 0.770558 0.665138 11.00000 0.05046 H4A 2 0.553555 0.630351 0.714540 11.00000 0.07304 HKLF 4 REM shelxt_a.res in C2/c REM wR2 = 0.1073, GooF = S = 1.054, Restrained GooF = 1.054 for all data REM R1 = 0.0417 for 2138 Fo > 4sig(Fo) and 0.0521 for all 2570 data REM 203 parameters refined using 1 restraints END WGHT 0.0355 4.0667 REM Highest difference peak 0.257, deepest hole -0.218, 1-sigma level 0.051 Q1 1 0.8496 0.8695 0.6005 11.00000 0.05 0.26 Q2 1 0.6308 0.3600 0.6737 11.00000 0.05 0.24 Q3 1 0.7722 0.2740 0.5727 11.00000 0.05 0.22 Q4 1 0.8319 0.0885 0.5589 11.00000 0.05 0.22 Q5 1 0.6669 0.2454 0.6663 11.00000 0.05 0.22 ; _shelx_res_checksum 49012 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy O O2 0.95635(5) 0.7070(2) 0.67260(6) 0.0206(3) Uani d 1 O O5 0.500000 0.7903(3) 0.750000 0.0222(4) Uani d 1 O O1 0.97314(5) 1.0831(2) 0.59182(6) 0.0238(3) Uani d 1 O O3 0.56242(5) 0.2504(2) 0.65933(7) 0.0271(3) Uani d 1 O O4 0.58989(5) 0.6076(3) 0.70737(8) 0.0347(4) Uani d 1 N N1 0.81774(6) 0.2583(3) 0.63512(8) 0.0197(3) Uani d 1 C C14 0.74975(6) 0.5056(3) 0.68083(8) 0.0168(3) Uani d 1 H H14 0.775566 0.623501 0.696467 0.020 Uiso calc 1 C C9 0.76511(6) 0.2985(3) 0.64627(8) 0.0158(3) Uani d 1 C C12 0.65625(6) 0.3621(3) 0.66873(8) 0.0174(4) Uani d 1 C C15 0.59858(7) 0.3981(3) 0.67792(9) 0.0194(4) Uani d 1 C C7 0.86973(6) 0.6259(3) 0.60621(9) 0.0177(4) Uani d 1 C C10 0.72476(7) 0.1239(3) 0.62307(9) 0.0181(4) Uani d 1 H H10 0.734254 -0.014204 0.599877 0.022 Uiso calc 1 C C13 0.69600(7) 0.5340(3) 0.69160(8) 0.0174(3) Uani d 1 H H13 0.686232 0.671711 0.714756 0.021 Uiso calc 1 C C5 0.92543(7) 0.9565(3) 0.57298(9) 0.0187(4) Uani d 1 C C6 0.91728(6) 0.7641(3) 0.61739(8) 0.0175(4) Uani d 1 C C2 0.83105(7) 0.6781(3) 0.54820(9) 0.0206(4) Uani d 1 H H2 0.799081 0.587223 0.539822 0.025 Uiso calc 1 C C8 0.86335(6) 0.4187(3) 0.65624(9) 0.0184(4) Uani d 1 H H8A 0.896629 0.323016 0.662065 0.022 Uiso calc 1 H H8B 0.859392 0.487346 0.701326 0.022 Uiso calc 1 C C4 0.88690(7) 1.0051(3) 0.51542(9) 0.0220(4) Uani d 1 H H4 0.892432 1.131150 0.485232 0.026 Uiso calc 1 C C11 0.67166(7) 0.1554(3) 0.63432(9) 0.0182(4) Uani d 1 H H11 0.645659 0.037923 0.618889 0.022 Uiso calc 1 C C3 0.83997(7) 0.8641(3) 0.50316(9) 0.0236(4) Uani d 1 H H3 0.814245 0.895045 0.464242 0.028 Uiso calc 1 C C1 0.98495(8) 1.2765(3) 0.54726(10) 0.0262(4) Uani d 1 H H1A 0.986748 1.213811 0.501435 0.039 Uiso calc 1 H H1B 1.019360 1.348797 0.565539 0.039 Uiso calc 1 H H1C 0.956674 1.397043 0.544826 0.039 Uiso calc 1 H H5 0.5159(12) 0.891(5) 0.7772(13) 0.076(10) Uiso d 1 H H1 0.8246(9) 0.120(4) 0.6076(12) 0.038(6) Uiso d 1 H H2A 0.9900(10) 0.771(5) 0.6651(13) 0.050(7) Uiso d 1 H H4A 0.5536(12) 0.630(6) 0.7145(15) 0.073(9) Uiso d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O2 0.0122(6) 0.0235(7) 0.0262(6) -0.0025(5) 0.0029(5) 0.0043(5) O5 0.0150(8) 0.0244(10) 0.0277(10) 0.000 0.0043(7) 0.000 O1 0.0199(6) 0.0212(7) 0.0313(7) -0.0052(5) 0.0067(5) 0.0063(5) O3 0.0136(6) 0.0270(7) 0.0411(8) -0.0032(5) 0.0055(5) -0.0011(6) O4 0.0173(7) 0.0366(8) 0.0524(9) 0.0000(6) 0.0127(6) -0.0187(7) N1 0.0137(7) 0.0186(7) 0.0280(8) -0.0020(6) 0.0071(6) -0.0034(6) C14 0.0150(8) 0.0163(8) 0.0191(8) -0.0038(6) 0.0020(6) -0.0007(6) C9 0.0132(7) 0.0169(8) 0.0173(8) 0.0001(6) 0.0025(6) 0.0030(6) C12 0.0148(8) 0.0192(8) 0.0184(8) 0.0004(7) 0.0037(6) 0.0024(7) C15 0.0166(8) 0.0220(9) 0.0201(8) 0.0010(7) 0.0042(6) 0.0013(7) C7 0.0156(8) 0.0184(8) 0.0207(8) 0.0012(7) 0.0084(6) -0.0023(7) C10 0.0176(8) 0.0145(8) 0.0224(8) 0.0004(7) 0.0035(7) -0.0002(7) C13 0.0176(8) 0.0172(8) 0.0178(8) 0.0012(7) 0.0039(6) -0.0011(7) C5 0.0161(8) 0.0180(8) 0.0236(9) 0.0000(7) 0.0083(7) -0.0010(7) C6 0.0149(8) 0.0187(8) 0.0198(8) 0.0030(7) 0.0057(6) -0.0020(7) C2 0.0159(8) 0.0232(9) 0.0230(9) -0.0007(7) 0.0038(7) -0.0033(7) C8 0.0116(7) 0.0196(9) 0.0246(9) -0.0012(7) 0.0043(6) 0.0003(7) C4 0.0249(9) 0.0215(9) 0.0211(9) 0.0028(7) 0.0082(7) 0.0034(7) C11 0.0157(8) 0.0150(8) 0.0239(9) -0.0040(6) 0.0026(6) 0.0009(7) C3 0.0217(9) 0.0287(10) 0.0202(9) 0.0018(8) 0.0025(7) -0.0001(7) C1 0.0290(10) 0.0180(9) 0.0351(10) -0.0029(8) 0.0159(8) 0.0043(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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_site_symmetry_3 _geom_angle C6 O2 H2A . 109.7(15) H5 O5 H5 2_656 96(4) C5 O1 C1 . 117.37(14) C15 O4 H4A . 113.6(19) C9 N1 C8 . 125.37(15) C9 N1 H1 . 117.7(13) C8 N1 H1 . 116.7(13) C13 C14 C9 . 119.78(15) C13 C14 H14 . 120.1 C9 C14 H14 . 120.1 N1 C9 C14 . 122.47(15) N1 C9 C10 . 119.03(15) C14 C9 C10 . 118.50(14) C13 C12 C11 . 118.44(15) C13 C12 C15 . 121.46(15) C11 C12 C15 . 120.06(15) O3 C15 O4 . 123.39(15) O3 C15 C12 . 123.62(16) O4 C15 C12 . 112.98(15) C6 C7 C2 . 118.60(16) C6 C7 C8 . 118.28(15) C2 C7 C8 . 123.08(15) C11 C10 C9 . 120.84(15) C11 C10 H10 . 119.6 C9 C10 H10 . 119.6 C14 C13 C12 . 121.73(15) C14 C13 H13 . 119.1 C12 C13 H13 . 119.1 O1 C5 C4 . 125.57(16) O1 C5 C6 . 114.50(15) C4 C5 C6 . 119.92(16) O2 C6 C7 . 118.78(15) O2 C6 C5 . 120.42(15) C7 C6 C5 . 120.79(15) C3 C2 C7 . 120.46(16) C3 C2 H2 . 119.8 C7 C2 H2 . 119.8 N1 C8 C7 . 115.22(14) N1 C8 H8A . 108.5 C7 C8 H8A . 108.5 N1 C8 H8B . 108.5 C7 C8 H8B . 108.5 H8A C8 H8B . 107.5 C5 C4 C3 . 119.45(16) C5 C4 H4 . 120.3 C3 C4 H4 . 120.3 C10 C11 C12 . 120.71(15) C10 C11 H11 . 119.6 C12 C11 H11 . 119.6 C2 C3 C4 . 120.72(16) C2 C3 H3 . 119.6 C4 C3 H3 . 119.6 O1 C1 H1A . 109.5 O1 C1 H1B . 109.5 H1A C1 H1B . 109.5 O1 C1 H1C . 109.5 H1A C1 H1C . 109.5 H1B C1 H1C . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance O2 C6 . 1.371(2) O2 H2A . 0.93(3) O5 H5 . 0.823(17) O5 H5 2_656 0.823(17) O1 C5 . 1.374(2) O1 C1 . 1.427(2) O3 C15 . 1.224(2) O4 C15 . 1.317(2) O4 H4A . 0.94(3) N1 C9 . 1.368(2) N1 C8 . 1.445(2) N1 H1 . 0.96(2) C14 C13 . 1.384(2) C14 C9 . 1.401(2) C14 H14 . 0.9300 C9 C10 . 1.411(2) C12 C13 . 1.390(2) C12 C11 . 1.399(2) C12 C15 . 1.477(2) C7 C6 . 1.391(2) C7 C2 . 1.398(2) C7 C8 . 1.519(2) C10 C11 . 1.374(2) C10 H10 . 0.9300 C13 H13 . 0.9300 C5 C4 . 1.385(2) C5 C6 . 1.397(2) C2 C3 . 1.383(3) C2 H2 . 0.9300 C8 H8A . 0.9700 C8 H8B . 0.9700 C4 C3 . 1.388(3) C4 H4 . 0.9300 C11 H11 . 0.9300 C3 H3 . 0.9300 C1 H1A . 0.9600 C1 H1B . 0.9600 C1 H1C . 0.9600 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O5 H5 O2 4_656 0.823(17) 2.063(19) 2.8640(19) 164(3) yes O2 H2A O3 3 0.93(3) 1.82(3) 2.6844(17) 154(2) yes O4 H4A O5 . 0.94(3) 1.81(3) 2.6776(15) 153(3) yes N1 H1 Cg1 1_545 0.96(2) 2.40(2) 3.3008(18) 157(2) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C8 N1 C9 C14 -0.4(3) C8 N1 C9 C10 -179.51(15) C13 C14 C9 N1 -178.88(15) C13 C14 C9 C10 0.2(2) C13 C12 C15 O3 -179.11(16) C11 C12 C15 O3 3.0(3) C13 C12 C15 O4 1.8(2) C11 C12 C15 O4 -176.06(15) N1 C9 C10 C11 178.86(15) C14 C9 C10 C11 -0.3(2) C9 C14 C13 C12 -0.3(2) C11 C12 C13 C14 0.3(2) C15 C12 C13 C14 -177.56(15) C1 O1 C5 C4 -2.0(2) C1 O1 C5 C6 177.78(14) C2 C7 C6 O2 -177.34(14) C8 C7 C6 O2 0.3(2) C2 C7 C6 C5 2.2(2) C8 C7 C6 C5 179.87(15) O1 C5 C6 O2 -3.0(2) C4 C5 C6 O2 176.85(15) O1 C5 C6 C7 177.53(14) C4 C5 C6 C7 -2.7(2) C6 C7 C2 C3 -0.2(2) C8 C7 C2 C3 -177.81(16) C9 N1 C8 C7 -83.9(2) C6 C7 C8 N1 -170.01(14) C2 C7 C8 N1 7.6(2) O1 C5 C4 C3 -179.06(16) C6 C5 C4 C3 1.2(2) C9 C10 C11 C12 0.4(3) C13 C12 C11 C10 -0.4(2) C15 C12 C11 C10 177.54(15) C7 C2 C3 C4 -1.3(3) C5 C4 C3 C2 0.8(3) _cod_database_fobs_code 2242814