#------------------------------------------------------------------------------ #$Date: 2026-09-30 23:19:14 +0200 (Wed, 30 Sep 2026) $ #$Revision: 306930 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023581.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_2023581 loop_ _publ_author_name 'Gurbanov, Atash V.' 'Akkurt, Mehmet' 'Karmakar, Anirban' 'Manahelohe, Gizachew Mulugeta' _publ_section_title ; Synthesis and structure of 5-[(4-fluorobenzyl)amino]isophthalic acid featuring O---H...O and N---H...\p interactions ; _journal_coeditor_code HB8253 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 1201 _journal_page_last 1204 _journal_paper_doi 10.1107/S205698902600959X _journal_volume 82 _journal_year 2026 _chemical_formula_iupac 'C15 H12 F N O4' _chemical_formula_moiety 'C15 H12 F N O4' _chemical_formula_sum 'C15 H12 F N O4' _chemical_formula_weight 289.26 _chemical_name_common ; 5-[(4-Fluorobenzyl)amino]isophthalic acid ; _chemical_name_systematic ; 5-{[(4-Fluorophenyl)methyl]amino}benzene-1,3-dicarboxylic acid ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 102.838(4) _cell_angle_beta 96.181(4) _cell_angle_gamma 108.027(4) _cell_formula_units_Z 2 _cell_length_a 8.4674(9) _cell_length_b 9.2193(11) _cell_length_c 9.2749(11) _cell_measurement_reflns_used 2691 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.40 _cell_measurement_theta_min 2.29 _cell_volume 659.01(13) _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_collection ; APEX4 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _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 0.0355 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 8198 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.480 _diffrn_reflns_theta_min 2.294 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_correction_T_min 0.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.458 _exptl_crystal_description prism _exptl_crystal_F_000 300 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.210 _refine_diff_density_max 0.239 _refine_diff_density_min -0.259 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 2722 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0388 _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^)+(0.0457P)^2^+0.1305P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.1022 _reflns_number_gt 2050 _reflns_number_total 2722 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8253.cif _cod_data_source_block I _cod_database_code 2023581 _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 0.961 _shelx_estimated_absorpt_t_max 0.976 _shelx_hkl_file ; -1 0 0 11.60 0.90 -1 0 0 10.80 0.60 -1 0 0 10.20 0.70 -1 0 0 11.50 0.60 1 0 0 11.80 0.90 1 0 0 12.00 0.70 1 0 0 11.50 0.60 1 0 0 11.60 0.60 -2 0 0 125.69 5.00 -2 0 0 127.59 4.80 -2 0 0 128.29 5.30 -2 0 0 124.29 4.70 2 0 0 125.39 5.00 2 0 0 126.79 5.30 2 0 0 121.69 4.80 2 0 0 126.69 4.70 -3 0 0 78.09 3.50 -3 0 0 82.79 4.20 -3 0 0 81.89 3.40 -3 0 0 84.79 3.70 3 0 0 79.69 3.40 3 0 0 82.99 3.50 3 0 0 80.39 4.10 3 0 0 82.39 3.10 3 0 0 79.49 3.80 -4 0 0 95.79 4.10 -4 0 0 100.39 4.70 -4 0 0 100.59 4.30 -4 0 0 98.89 5.20 4 0 0 94.59 4.60 4 0 0 97.79 3.70 4 0 0 93.99 4.20 4 0 0 98.29 4.20 -5 0 0 74.59 3.70 -5 0 0 84.39 5.00 -5 0 0 82.19 3.90 5 0 0 82.69 3.20 5 0 0 78.29 3.90 5 0 0 81.29 3.80 -6 0 0 118.49 6.60 -6 0 0 105.19 5.10 6 0 0 109.29 5.00 6 0 0 110.69 4.10 -7 0 0 719.33 26.00 -7 0 0 687.53 27.90 7 0 0 701.73 25.70 -8 0 0 -0.80 1.40 8 0 0 -1.10 0.70 -9 0 0 9.70 2.90 9 0 0 13.20 2.00 -10 1 0 3.20 2.50 9 -1 0 0.30 1.00 -9 1 0 1.90 2.00 -9 1 0 1.10 1.20 8 -1 0 80.49 4.10 -8 1 0 74.89 4.40 -8 1 0 79.09 6.10 7 -1 0 276.57 10.70 -7 1 0 278.07 11.20 -7 1 0 270.17 10.70 -7 1 0 278.87 13.00 6 -1 0 110.99 4.80 -6 1 0 106.89 6.40 -6 1 0 107.59 4.70 -6 1 0 115.19 5.20 5 -1 0 25.60 1.10 5 -1 0 25.50 1.60 5 -1 0 24.10 1.10 5 -1 0 27.40 1.90 -5 1 0 26.20 2.60 -5 1 0 26.00 1.60 -5 1 0 21.60 1.80 4 -1 0 200.88 7.90 4 -1 0 203.38 7.20 4 -1 0 201.78 7.60 -4 1 0 210.88 8.00 -4 1 0 199.58 8.90 -4 1 0 201.78 8.20 -4 1 0 206.28 7.60 3 -1 0 53.09 2.70 3 -1 0 53.19 2.50 3 -1 0 51.89 2.20 3 -1 0 52.99 2.00 -3 1 0 54.29 2.70 -3 1 0 53.09 2.20 -3 1 0 51.49 2.50 2 -1 0 1918.61 63.69 2 -1 0 1791.82 63.59 2 -1 0 1755.52 63.19 2 -1 0 1810.12 63.29 -2 1 0 1784.92 63.09 -2 1 0 1892.31 63.49 -2 1 0 1763.22 63.09 -2 1 0 1762.12 63.49 1 -1 0 139.59 5.00 1 -1 0 138.59 5.10 1 -1 0 144.29 5.10 -1 1 0 142.19 5.00 -1 1 0 135.19 5.10 -1 1 0 140.49 5.10 0 -1 0 324.17 12.20 0 -1 0 299.37 12.50 0 -1 0 361.96 12.30 0 -1 0 365.66 12.10 0 1 0 360.46 12.20 0 1 0 354.36 12.20 0 1 0 355.46 12.10 -1 -1 0 53.09 2.20 -1 -1 0 53.09 2.30 -1 -1 0 53.09 2.30 -1 -1 0 57.19 2.70 1 1 0 59.89 2.70 1 1 0 54.09 2.30 1 1 0 51.79 2.30 1 1 0 52.59 2.20 -2 -1 0 3.40 0.60 -2 -1 0 3.20 0.90 -2 -1 0 3.30 0.50 -2 -1 0 3.00 0.70 2 1 0 3.30 0.90 2 1 0 3.10 0.50 2 1 0 3.60 0.80 2 1 0 2.70 0.60 2 1 0 4.00 0.60 -3 -1 0 0.30 0.50 -3 -1 0 0.50 0.60 -3 -1 0 0.90 0.90 3 1 0 0.50 0.50 3 1 0 -0.10 0.40 3 1 0 0.80 0.70 3 1 0 -0.20 0.60 3 1 0 0.10 0.60 -4 -1 0 31.80 2.00 -4 -1 0 30.80 2.30 -4 -1 0 31.60 2.70 4 1 0 31.40 1.70 4 1 0 31.30 2.00 4 1 0 29.00 2.60 4 1 0 30.90 2.00 -5 -1 0 16.90 2.50 5 1 0 15.00 1.60 5 1 0 14.50 1.70 5 1 0 14.60 1.10 5 1 0 13.90 2.60 -6 -1 0 110.79 6.50 6 1 0 102.19 5.10 6 1 0 107.29 4.30 -7 -1 0 108.59 6.90 7 1 0 103.39 5.30 7 1 0 106.49 4.20 -8 -1 0 3.30 2.00 8 1 0 2.90 1.30 -9 -1 0 10.90 3.00 9 1 0 14.40 2.20 -10 2 0 0.70 1.90 -10 2 0 -0.20 1.10 -9 2 0 2.70 1.70 -9 2 0 2.40 1.30 -8 2 0 13.60 2.90 -8 2 0 11.60 1.90 7 -2 0 0.60 0.70 -7 2 0 0.40 1.00 -7 2 0 0.70 0.60 -7 2 0 0.70 1.40 6 -2 0 100.49 3.70 6 -2 0 101.69 4.30 -6 2 0 106.19 6.30 -6 2 0 99.79 4.20 -6 2 0 109.09 5.00 5 -2 0 228.18 9.10 5 -2 0 226.88 8.40 5 -2 0 229.38 8.30 -5 2 0 237.28 10.50 -5 2 0 227.58 8.40 -5 2 0 228.28 9.20 -5 2 0 234.28 9.40 4 -2 0 421.86 14.80 4 -2 0 429.66 15.40 4 -2 0 419.06 14.70 -4 2 0 430.36 15.50 -4 2 0 416.76 14.80 -4 2 0 412.16 14.70 -4 2 0 398.96 15.40 3 -2 0 136.59 5.10 3 -2 0 132.19 5.40 -3 2 0 132.89 5.10 -3 2 0 137.99 5.40 -3 2 0 134.99 4.80 -3 2 0 130.99 5.40 2 -2 0 22.00 1.20 2 -2 0 18.50 1.30 -2 2 0 20.70 1.20 -2 2 0 20.10 1.10 -2 2 0 21.40 1.40 1 -2 0 0.90 0.30 1 -2 0 0.30 0.50 1 -2 0 0.20 0.50 -1 2 0 0.30 0.10 -1 2 0 1.10 0.30 -1 2 0 1.00 0.50 -1 2 0 0.60 0.40 0 -2 0 0.50 0.70 0 -2 0 0.40 0.40 0 -2 0 0.60 0.50 0 -2 0 0.70 0.30 0 2 0 0.00 0.70 0 2 0 1.00 0.50 0 2 0 -0.50 0.40 -1 -2 0 357.66 13.00 -1 -2 0 355.86 12.90 -1 -2 0 361.56 13.00 -1 -2 0 349.57 13.70 1 2 0 339.67 12.90 1 2 0 357.36 13.00 1 2 0 381.06 13.70 1 2 0 371.86 13.00 -2 -2 0 1040.30 36.50 -2 -2 0 962.50 36.70 -2 -2 0 1054.69 36.70 -2 -2 0 1076.89 37.60 2 2 0 1059.19 36.70 2 2 0 1026.60 36.80 2 2 0 1040.70 36.60 2 2 0 1072.69 37.50 -3 -2 0 276.07 10.70 -3 -2 0 281.37 11.70 -3 -2 0 285.97 10.90 3 2 0 285.67 10.50 3 2 0 281.27 10.60 3 2 0 269.77 10.70 3 2 0 289.07 11.70 -4 -2 0 35.20 3.10 4 2 0 34.60 2.40 4 2 0 34.40 2.20 4 2 0 35.80 2.00 4 2 0 35.30 3.00 -5 -2 0 1.60 1.30 5 2 0 -0.20 0.70 5 2 0 0.30 0.60 5 2 0 0.50 0.70 -6 -2 0 29.60 3.20 6 2 0 27.20 1.90 6 2 0 34.70 2.70 -7 -2 0 0.70 1.60 7 2 0 0.50 1.10 7 2 0 1.10 0.70 -8 -2 0 14.60 3.20 8 2 0 13.70 2.30 -9 -2 0 45.10 5.80 9 2 0 49.20 4.30 -10 3 0 2.90 2.30 -10 3 0 3.70 1.80 -9 3 0 -0.50 1.10 -9 3 0 0.30 1.30 -8 3 0 6.30 1.60 -8 3 0 7.40 2.30 7 -3 0 6.60 0.60 -7 3 0 4.10 1.90 -7 3 0 6.30 0.80 -7 3 0 7.00 1.50 6 -3 0 21.20 1.30 -6 3 0 20.50 2.20 -6 3 0 21.10 1.20 5 -3 0 146.09 6.40 5 -3 0 148.49 5.70 -5 3 0 145.39 6.30 -5 3 0 145.69 5.30 -5 3 0 149.49 6.40 -5 3 0 146.39 5.70 4 -3 0 77.89 3.40 4 -3 0 83.69 3.90 -4 3 0 84.99 4.00 -4 3 0 80.19 3.80 -4 3 0 82.79 3.50 3 -3 0 24.70 1.60 3 -3 0 25.30 1.80 -3 3 0 26.60 1.50 -3 3 0 26.30 1.80 -3 3 0 25.80 1.60 2 -3 0 28.90 1.70 2 -3 0 28.40 1.20 2 -3 0 27.20 1.60 -2 3 0 27.80 1.70 -2 3 0 25.90 1.20 -2 3 0 27.70 1.20 -2 3 0 27.50 1.80 1 -3 0 11.20 1.20 1 -3 0 11.20 0.90 -1 3 0 13.10 1.80 -1 3 0 15.10 1.30 -1 3 0 9.70 1.00 -1 3 0 13.80 0.90 0 -3 0 73.69 4.00 0 -3 0 72.49 3.10 0 -3 0 70.39 2.80 0 -3 0 69.89 3.30 0 3 0 68.49 3.10 0 3 0 70.99 3.30 -1 -3 0 197.58 8.00 -1 -3 0 203.28 7.80 -1 -3 0 212.08 8.10 1 3 0 222.28 9.00 1 3 0 211.28 8.10 1 3 0 209.58 8.10 -2 -3 0 76.59 3.70 -2 -3 0 77.99 4.60 -2 -3 0 74.89 3.50 -2 -3 0 72.69 3.60 2 3 0 79.19 3.60 2 3 0 73.29 4.40 2 3 0 76.79 3.70 -3 -3 0 114.19 4.90 -3 -3 0 118.89 6.20 -3 -3 0 107.59 5.10 3 3 0 110.79 4.90 3 3 0 119.39 6.10 3 3 0 108.99 5.10 -4 -3 0 24.50 2.80 4 3 0 23.90 2.30 4 3 0 21.90 1.80 4 3 0 22.90 1.80 -5 -3 0 22.50 3.20 5 3 0 25.90 2.60 5 3 0 23.60 1.90 -6 -3 0 2.60 1.80 6 3 0 0.40 1.20 6 3 0 1.80 0.90 -7 -3 0 -0.90 1.50 7 3 0 0.40 1.20 -8 -3 0 58.99 5.70 8 3 0 65.69 4.50 -10 4 0 0.80 1.40 -10 4 0 4.10 2.40 -9 4 0 1.20 1.80 -9 4 0 0.60 1.20 -8 4 0 3.70 2.00 -8 4 0 2.40 1.30 7 -4 0 7.40 0.90 -7 4 0 5.80 1.50 6 -4 0 0.30 0.50 -6 4 0 1.30 0.60 -6 4 0 1.10 1.00 5 -4 0 18.00 1.40 -5 4 0 16.80 1.70 -5 4 0 18.80 1.40 -5 4 0 17.80 2.00 4 -4 0 15.50 1.50 4 -4 0 14.70 1.60 -4 4 0 14.50 1.70 -4 4 0 14.50 1.20 -4 4 0 14.40 1.40 3 -4 0 32.70 2.00 3 -4 0 27.00 1.90 3 -4 0 30.30 1.30 -3 4 0 31.70 1.30 -3 4 0 29.50 2.10 -3 4 0 30.20 2.00 -3 4 0 29.30 1.60 2 -4 0 107.59 4.80 2 -4 0 109.29 4.30 2 -4 0 113.09 4.80 -2 4 0 110.49 3.90 -2 4 0 107.19 4.80 -2 4 0 112.79 4.30 -2 4 0 117.49 4.90 1 -4 0 171.38 7.00 1 -4 0 174.08 6.70 -1 4 0 180.98 7.10 -1 4 0 159.28 8.00 -1 4 0 177.98 6.70 -1 4 0 176.28 7.00 0 -4 0 223.78 9.10 0 -4 0 193.98 7.70 0 -4 0 201.38 7.00 0 -4 0 188.88 7.40 0 4 0 186.38 7.40 0 4 0 180.08 7.60 0 4 0 157.68 8.50 -1 -4 0 12.10 1.30 -1 -4 0 10.10 2.10 -1 -4 0 12.60 1.50 -1 -4 0 12.50 1.20 1 4 0 10.70 1.30 1 4 0 15.00 2.10 1 4 0 13.40 1.50 -2 -4 0 0.00 1.00 -2 -4 0 0.70 0.60 -2 -4 0 0.70 0.70 2 4 0 1.20 0.90 2 4 0 0.00 0.80 2 4 0 1.50 0.70 -3 -4 0 102.09 4.90 -3 -4 0 101.99 6.30 -3 -4 0 99.29 4.80 3 4 0 109.69 5.00 3 4 0 101.59 5.00 -4 -4 0 22.40 3.40 4 4 0 22.10 2.30 4 4 0 20.70 2.10 -5 -4 0 14.30 2.90 5 4 0 14.70 1.80 5 4 0 14.70 2.10 -6 -4 0 19.20 3.50 6 4 0 18.40 2.10 6 4 0 16.80 2.40 -7 -4 0 13.80 3.30 7 4 0 11.70 2.30 -10 5 0 6.00 2.70 -10 5 0 4.30 1.80 -9 5 0 11.70 2.20 -9 5 0 12.50 3.20 -8 5 0 4.30 1.50 7 -5 0 57.09 3.00 -7 5 0 57.69 3.00 -7 5 0 56.99 3.80 6 -5 0 129.19 5.50 -6 5 0 127.29 5.70 -6 5 0 129.99 5.50 -6 5 0 122.39 6.20 5 -5 0 12.40 1.50 -5 5 0 8.80 1.20 -5 5 0 6.10 1.40 -5 5 0 9.60 1.20 4 -5 0 92.79 4.50 -4 5 0 103.49 4.60 -4 5 0 93.79 4.80 -4 5 0 97.59 4.10 3 -5 0 1.80 0.50 3 -5 0 2.00 0.80 -3 5 0 3.60 1.10 -3 5 0 2.30 0.50 -3 5 0 2.60 0.40 -3 5 0 3.10 1.00 2 -5 0 53.79 2.50 2 -5 0 55.49 3.00 -2 5 0 45.20 3.00 -2 5 0 55.59 4.10 -2 5 0 52.59 2.50 -2 5 0 53.39 3.10 1 -5 0 281.67 11.20 1 -5 0 299.17 10.90 -1 5 0 291.37 11.20 -1 5 0 288.97 10.90 -1 5 0 281.47 11.30 0 -5 0 87.09 4.00 0 -5 0 97.99 5.70 0 -5 0 85.99 3.40 0 5 0 80.59 4.30 0 5 0 74.19 5.10 0 5 0 80.39 3.90 -1 -5 0 34.60 1.90 -1 -5 0 27.50 3.20 1 5 0 32.60 2.30 1 5 0 30.90 2.30 -2 -5 0 28.70 2.00 -2 -5 0 17.70 3.20 2 5 0 26.10 2.40 2 5 0 26.60 2.50 -3 -5 0 142.79 9.20 3 5 0 202.28 8.10 3 5 0 198.18 8.20 -4 -5 0 14.40 3.10 4 5 0 17.60 2.20 4 5 0 16.40 2.20 -5 -5 0 30.90 4.60 5 5 0 38.10 3.50 5 5 0 38.50 2.90 -6 -5 0 26.80 4.40 6 5 0 22.20 2.50 6 5 0 25.80 3.10 7 5 0 13.70 2.50 -10 6 0 13.30 3.40 -10 6 0 9.30 2.30 -9 6 0 2.30 1.60 -8 6 0 6.10 1.70 -8 6 0 7.80 1.90 7 -6 0 1.20 1.00 -7 6 0 3.10 1.20 -7 6 0 3.00 1.00 -6 6 0 22.20 2.00 -6 6 0 21.00 2.60 -6 6 0 18.40 2.00 -5 6 0 36.80 2.60 -5 6 0 33.30 2.80 -5 6 0 36.00 2.10 4 -6 0 28.70 1.40 -4 6 0 27.90 1.40 -4 6 0 25.60 2.60 -4 6 0 28.10 1.50 -4 6 0 29.90 2.30 3 -6 0 35.30 1.90 -3 6 0 33.70 1.90 -3 6 0 32.70 2.50 -3 6 0 32.20 2.40 2 -6 0 82.59 3.70 -2 6 0 81.39 3.70 -2 6 0 71.19 4.10 -2 6 0 83.59 4.40 1 -6 0 0.60 0.70 -1 6 0 0.80 0.80 -1 6 0 1.80 0.80 -1 6 0 1.20 1.10 0 -6 0 5.30 0.70 0 6 0 4.60 1.40 0 6 0 3.40 1.20 0 6 0 6.30 1.10 -1 -6 0 170.98 9.00 -1 -6 0 153.88 6.20 1 6 0 145.59 6.80 1 6 0 146.09 7.00 -2 -6 0 2.30 1.80 -2 -6 0 1.90 1.00 2 6 0 3.30 1.30 2 6 0 4.00 1.40 -3 -6 0 23.40 4.10 3 6 0 36.90 2.90 3 6 0 36.50 2.90 -4 -6 0 2.60 2.40 4 6 0 1.60 1.30 4 6 0 2.80 1.50 -5 -6 0 4.80 2.50 5 6 0 6.30 1.70 5 6 0 6.70 1.70 -6 -6 0 5.10 2.70 6 6 0 -0.40 1.30 6 6 0 -1.10 1.00 -10 7 0 18.00 3.00 -10 7 0 16.30 3.90 -9 7 0 10.40 2.30 -8 7 0 52.09 3.20 -8 7 0 37.90 4.00 -7 7 0 25.60 2.50 -7 7 0 28.60 3.20 -6 7 0 0.30 0.90 -6 7 0 -0.90 0.70 -5 7 0 136.69 6.70 -5 7 0 135.79 5.30 -5 7 0 129.29 6.30 4 -7 0 24.80 1.60 -4 7 0 26.80 2.60 -4 7 0 24.20 1.50 -4 7 0 25.40 2.60 3 -7 0 137.29 5.60 -3 7 0 138.89 5.60 -3 7 0 123.49 6.40 -3 7 0 138.29 6.50 2 -7 0 77.39 3.70 -2 7 0 70.19 4.10 -2 7 0 75.89 4.40 -2 7 0 72.39 3.70 -1 7 0 1.50 1.00 -1 7 0 -0.30 0.70 -1 7 0 0.40 0.80 0 -7 0 11.30 0.90 0 7 0 9.50 1.70 0 7 0 12.10 1.90 0 7 0 12.50 1.80 -1 -7 0 437.66 18.50 -1 -7 0 381.76 14.70 1 7 0 386.26 15.90 1 7 0 396.56 15.70 -2 -7 0 5.20 2.60 2 7 0 8.70 1.90 2 7 0 7.60 1.80 -3 -7 0 11.90 3.30 3 7 0 14.50 2.30 3 7 0 15.40 2.40 -4 -7 0 16.70 3.90 4 7 0 13.70 2.30 4 7 0 13.90 2.60 -5 -7 0 7.70 3.30 5 7 0 6.60 1.90 5 7 0 4.40 1.90 -9 8 0 1.60 1.60 -8 8 0 8.30 2.30 -8 8 0 10.90 1.90 -7 8 0 26.20 3.20 -7 8 0 25.80 2.70 -6 8 0 0.80 1.30 -6 8 0 1.40 1.10 -5 8 0 52.39 3.80 -5 8 0 41.80 3.40 4 -8 0 13.80 1.40 -4 8 0 10.80 1.20 -4 8 0 11.30 2.00 -4 8 0 9.80 2.00 3 -8 0 1.20 0.70 -3 8 0 -0.20 1.10 -3 8 0 -0.20 0.70 -3 8 0 -0.50 1.00 -2 8 0 -0.30 1.20 -2 8 0 -0.70 1.10 -2 8 0 0.30 0.80 -1 8 0 281.37 12.00 -1 8 0 305.17 12.50 -1 8 0 283.27 11.70 0 8 0 0.80 1.10 0 8 0 -0.50 0.80 0 8 0 1.80 1.20 1 8 0 6.00 1.60 1 8 0 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95.99 5.50 6 -5 4 101.59 5.60 6 -5 4 104.09 4.30 -7 5 -4 1.50 1.10 7 -5 4 1.20 0.70 7 -5 4 -1.10 1.30 -8 5 -4 0.60 1.50 8 -5 4 3.10 1.70 -9 5 -4 30.90 4.30 -9 5 -4 30.30 3.60 9 -5 4 35.40 4.10 -8 -4 4 8.30 3.00 -7 -4 4 2.10 2.30 6 4 -4 19.70 1.90 -6 -4 4 20.90 4.00 5 4 -4 1034.90 35.70 -5 -4 4 963.10 35.60 -5 -4 4 989.40 38.90 4 4 -4 80.99 4.00 -4 -4 4 79.49 3.90 -4 -4 4 74.39 5.70 3 4 -4 9.70 1.40 -3 -4 4 6.80 1.90 -3 -4 4 7.70 1.20 2 4 -4 61.99 2.50 2 4 -4 62.99 3.40 -2 -4 4 68.09 4.80 -2 -4 4 58.59 3.30 1 4 -4 52.39 4.40 1 4 -4 54.79 2.30 1 4 -4 52.09 3.00 -1 -4 4 51.39 2.30 -1 -4 4 53.69 4.30 -1 -4 4 46.00 2.90 -1 -4 4 51.49 3.10 0 4 -4 44.80 3.30 0 4 -4 39.30 2.50 0 4 -4 39.30 2.00 0 -4 4 39.90 2.40 0 -4 4 37.60 2.00 0 -4 4 41.90 2.60 0 -4 4 34.80 2.30 0 -4 4 26.90 2.90 -1 4 -4 107.79 4.70 -1 4 -4 112.99 6.00 -1 4 -4 111.79 5.10 1 -4 4 105.09 4.60 1 -4 4 108.79 6.00 1 -4 4 108.19 5.00 1 -4 4 104.19 4.80 -2 4 -4 1491.15 53.49 -2 4 -4 1528.55 53.29 -2 4 -4 1520.35 53.29 2 -4 4 1499.55 53.19 2 -4 4 1530.05 53.29 2 -4 4 1500.35 53.49 -3 4 -4 37.40 2.40 -3 4 -4 35.30 2.40 -3 4 -4 29.80 3.00 3 -4 4 31.70 2.40 -4 4 -4 4.20 1.10 -4 4 -4 4.20 1.60 4 -4 4 5.20 0.90 4 -4 4 5.70 1.40 -5 4 -4 48.30 3.40 5 -4 4 45.50 2.50 5 -4 4 53.69 3.60 -6 4 -4 1.10 1.20 6 -4 4 1.10 1.40 6 -4 4 1.20 0.70 -7 4 -4 -0.30 0.90 7 -4 4 0.40 0.70 7 -4 4 0.20 1.50 -8 4 -4 22.80 3.40 -8 4 -4 18.20 2.90 8 -4 4 23.90 3.20 -9 4 -4 152.68 8.20 -9 4 -4 137.69 9.40 9 -4 4 155.98 8.50 -8 -3 4 0.60 2.20 -7 -3 4 54.59 5.40 -6 -3 4 125.39 8.30 -5 -3 4 172.58 6.90 -5 -3 4 169.58 9.50 4 3 -4 4.90 0.90 -4 -3 4 3.40 0.90 -4 -3 4 2.70 1.40 3 3 -4 112.49 5.00 -3 -3 4 115.39 6.70 -3 -3 4 111.49 4.90 2 3 -4 64.49 3.40 2 3 -4 64.29 4.40 -2 -3 4 69.59 4.70 -2 -3 4 69.39 3.90 -2 -3 4 70.69 3.40 1 3 -4 113.69 4.40 1 3 -4 114.89 5.20 1 3 -4 115.69 6.00 -1 -3 4 108.29 4.40 -1 -3 4 135.19 6.60 -1 -3 4 119.29 5.20 0 3 -4 1.20 0.50 0 3 -4 0.50 0.90 0 -3 4 -0.50 0.70 0 -3 4 0.10 1.10 0 -3 4 0.80 0.80 0 -3 4 0.20 0.50 -1 3 -4 546.05 20.20 -1 3 -4 594.24 21.20 -1 3 -4 555.14 20.40 1 -3 4 569.44 20.50 1 -3 4 558.54 20.50 1 -3 4 534.05 21.20 1 -3 4 561.34 20.20 -2 3 -4 615.34 22.20 -2 3 -4 617.94 22.10 2 -3 4 600.44 22.00 2 -3 4 610.44 22.20 2 -3 4 590.44 22.10 -3 3 -4 51.89 3.50 -3 3 -4 55.29 3.10 -3 3 -4 50.09 3.00 3 -3 4 58.29 3.30 3 -3 4 55.39 3.00 3 -3 4 55.69 2.70 -4 3 -4 36.30 2.70 4 -3 4 35.60 2.60 4 -3 4 32.20 2.00 4 -3 4 35.60 2.40 -5 3 -4 3.10 1.30 5 -3 4 1.10 0.70 5 -3 4 1.90 1.20 -6 3 -4 0.80 1.00 -6 3 -4 1.00 1.00 6 -3 4 -0.90 1.40 6 -3 4 1.10 0.70 -7 3 -4 29.80 3.20 -7 3 -4 33.00 3.30 7 -3 4 31.40 2.30 7 -3 4 34.00 3.80 -8 3 -4 158.38 8.10 -8 3 -4 154.98 8.50 8 -3 4 157.28 8.50 8 -3 4 157.78 6.90 -9 3 -4 17.30 3.00 9 -3 4 10.30 2.70 -9 -2 4 5.70 3.10 -8 -2 4 6.50 2.90 -7 -2 4 4.70 2.30 6 2 -4 -0.40 0.30 -6 -2 4 0.70 1.30 -5 -2 4 14.70 1.30 -5 -2 4 13.60 2.70 -4 -2 4 371.86 13.50 -4 -2 4 358.86 15.70 3 2 -4 77.99 5.40 -3 -2 4 73.49 3.50 -3 -2 4 77.09 4.10 -3 -2 4 75.39 4.90 2 2 -4 744.73 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9 7.70 2.60 5 -3 9 0.70 2.00 5 -3 9 3.60 1.60 -7 -2 9 0.90 1.80 -6 -2 9 4.70 2.50 -5 -2 9 8.60 2.70 -4 -2 9 95.49 6.80 -4 -2 9 89.69 5.70 -3 -2 9 22.20 3.50 -3 -2 9 24.70 3.10 -2 -2 9 33.90 3.80 -2 -2 9 42.50 3.80 -1 -2 9 5.00 1.70 -1 -2 9 4.70 1.50 0 -2 9 3.30 1.30 0 -2 9 4.90 1.60 1 -2 9 70.69 4.60 1 -2 9 76.79 5.20 2 -2 9 20.80 2.70 2 -2 9 17.60 3.00 3 -2 9 1.00 1.30 3 -2 9 -0.10 1.60 4 -2 9 9.40 2.10 4 -2 9 7.00 2.20 5 -2 9 3.70 2.40 5 -2 9 -1.40 1.30 -7 -1 9 6.50 3.00 -6 -1 9 20.30 4.00 -5 -1 9 16.30 3.30 -5 -1 9 17.70 2.80 -4 -1 9 16.50 2.70 -4 -1 9 9.80 2.60 -3 -1 9 168.88 8.40 -3 -1 9 156.68 8.70 -2 -1 9 24.90 3.10 -2 -1 9 20.20 2.90 -1 -1 9 42.10 3.30 -1 -1 9 37.20 3.90 0 -1 9 1.80 1.30 0 -1 9 1.50 1.30 1 -1 9 0.00 1.30 1 -1 9 -0.20 1.00 2 -1 9 2.80 1.60 2 -1 9 3.60 1.30 3 -1 9 -0.90 1.30 3 -1 9 0.70 1.40 4 -1 9 73.89 4.90 4 -1 9 67.89 5.60 5 -1 9 17.00 2.80 -7 0 9 28.90 4.90 -6 0 9 4.20 2.30 -5 0 9 2.40 1.90 -5 0 9 3.60 1.70 -4 0 9 15.70 1.80 -4 0 9 19.20 2.90 -4 0 9 18.90 3.20 -3 0 9 27.80 3.20 -3 0 9 29.60 3.50 -2 0 9 19.50 2.70 -2 0 9 16.20 2.70 -1 0 9 3.60 1.40 -1 0 9 3.00 1.20 0 0 9 26.40 3.00 0 0 9 22.00 3.10 1 0 9 -0.10 1.30 1 0 9 0.40 1.30 2 0 9 16.90 3.10 2 0 9 16.20 2.60 3 0 9 18.30 2.80 3 0 9 15.00 2.80 4 0 9 2.00 1.60 4 0 9 -0.50 1.80 -7 1 9 8.30 3.00 -6 1 9 -0.80 1.40 -6 1 9 0.10 1.40 -5 1 9 50.79 4.90 -5 1 9 53.09 4.30 -4 1 9 25.00 3.60 -4 1 9 23.40 3.20 -3 1 9 15.90 2.70 -3 1 9 12.90 2.30 -3 1 9 18.40 2.50 -2 1 9 39.50 3.40 -2 1 9 37.00 3.90 -2 1 9 37.00 3.60 -1 1 9 12.60 2.20 -1 1 9 8.50 2.20 0 1 9 0.40 1.30 0 1 9 2.40 1.50 1 1 9 3.40 1.90 1 1 9 1.30 1.50 2 1 9 7.40 2.40 2 1 9 6.50 2.00 3 1 9 19.50 2.80 3 1 9 19.10 3.30 -7 2 9 29.50 3.90 -7 2 9 31.90 5.10 -6 2 9 2.40 1.90 -6 2 9 2.70 1.50 -6 2 9 2.50 1.50 -5 2 9 0.30 1.30 -5 2 9 0.00 1.10 -5 2 9 1.20 1.00 -5 2 9 -1.30 1.40 -4 2 9 53.19 4.20 -4 2 9 54.39 4.60 -4 2 9 47.60 3.80 -3 2 9 9.80 2.20 -3 2 9 12.90 2.20 -3 2 9 16.40 2.60 -2 2 9 6.20 1.90 -2 2 9 5.10 1.70 -1 2 9 0.70 1.30 -1 2 9 1.30 1.40 0 2 9 -0.70 1.20 0 2 9 -1.60 0.80 1 2 9 1.30 1.60 1 2 9 1.90 1.50 2 2 9 2.90 1.90 2 2 9 0.40 1.50 3 2 9 16.80 2.90 3 2 9 16.40 3.20 -6 3 9 6.40 1.80 -6 3 9 6.90 2.70 -6 3 9 4.40 1.90 -6 3 9 4.20 1.60 -5 3 9 -0.30 1.10 -5 3 9 -0.10 0.90 -5 3 9 0.20 1.10 -5 3 9 0.40 1.20 -5 3 9 -0.10 1.40 -4 3 9 3.50 1.60 -4 3 9 2.30 1.70 -4 3 9 3.00 1.60 -4 3 9 1.50 1.40 -4 3 9 2.60 1.30 -3 3 9 3.50 1.60 -3 3 9 5.10 1.90 -3 3 9 5.40 1.50 -2 3 9 7.60 2.00 -2 3 9 5.10 1.60 -1 3 9 9.00 2.20 -1 3 9 5.50 1.80 0 3 9 37.30 4.20 0 3 9 40.80 4.00 0 3 9 36.00 4.10 1 3 9 1.80 1.70 1 3 9 2.10 1.40 1 3 9 2.60 1.60 2 3 9 0.00 1.70 -6 4 9 16.00 3.60 -6 4 9 17.00 2.50 -6 4 9 23.10 3.00 -6 4 9 15.20 2.70 -6 4 9 18.40 2.60 -5 4 9 1.20 1.70 -5 4 9 4.00 1.50 -5 4 9 4.40 1.70 -5 4 9 5.50 1.70 -5 4 9 4.70 1.70 -4 4 9 1.20 1.30 -4 4 9 0.90 1.40 -4 4 9 1.20 1.40 -4 4 9 1.00 1.40 -3 4 9 53.49 4.10 -3 4 9 40.70 4.30 -3 4 9 50.39 4.00 -2 4 9 5.30 1.80 -2 4 9 3.80 1.60 -2 4 9 4.70 1.80 -1 4 9 54.69 4.40 -1 4 9 56.29 4.20 -1 4 9 48.40 4.20 0 4 9 0.10 1.60 0 4 9 0.60 1.60 0 4 9 0.60 1.70 -4 5 9 25.40 3.40 -4 5 9 29.20 3.40 -4 5 9 37.50 3.90 -4 5 9 20.70 3.00 -3 5 9 62.59 4.50 -3 5 9 52.09 4.30 -3 5 9 57.29 4.70 -2 5 9 11.90 2.70 -2 5 9 8.00 2.20 -2 5 9 7.90 2.30 -2 -7 10 -0.20 1.50 -2 -7 10 1.00 2.60 -1 -7 10 1.20 2.30 -1 -7 10 5.30 2.00 0 -7 10 3.20 2.40 0 -7 10 3.50 1.90 1 -7 10 7.50 2.20 2 -7 10 0.70 1.70 3 -7 10 2.10 2.10 -3 -6 10 3.60 2.00 -3 -6 10 1.60 1.90 -2 -6 10 0.40 1.90 -2 -6 10 -0.90 1.30 -1 -6 10 1.20 2.00 -1 -6 10 -0.40 1.40 0 -6 10 1.70 1.60 0 -6 10 1.40 1.90 1 -6 10 0.50 1.50 2 -6 10 3.00 1.90 3 -6 10 11.50 2.70 3 -6 10 6.10 1.90 4 -6 10 4.70 2.00 4 -6 10 4.00 1.60 -4 -5 10 2.20 2.40 -4 -5 10 3.20 1.90 -3 -5 10 2.80 2.60 -3 -5 10 0.70 1.60 -2 -5 10 0.40 1.50 -2 -5 10 0.10 1.90 -1 -5 10 16.10 3.50 -1 -5 10 30.10 3.70 0 -5 10 1.50 1.80 0 -5 10 0.80 1.20 1 -5 10 5.90 2.20 2 -5 10 -1.10 1.40 3 -5 10 2.50 1.90 3 -5 10 -0.10 1.30 4 -5 10 2.50 1.50 4 -5 10 2.70 2.40 -5 -4 10 3.70 1.80 -5 -4 10 5.00 2.90 -4 -4 10 6.00 2.30 -4 -4 10 12.10 3.40 -3 -4 10 1.20 1.30 -3 -4 10 -2.80 1.40 -2 -4 10 -1.90 1.50 -2 -4 10 0.10 1.00 -1 -4 10 7.30 2.00 -1 -4 10 2.20 1.90 0 -4 10 0.30 1.50 1 -4 10 0.50 1.60 2 -4 10 20.00 3.10 2 -4 10 19.00 2.60 3 -4 10 0.70 1.80 3 -4 10 1.40 1.40 4 -4 10 5.10 2.20 4 -4 10 3.80 1.70 -5 -3 10 1.90 1.80 -5 -3 10 3.30 2.30 -4 -3 10 -0.80 1.40 -4 -3 10 -1.00 1.70 -3 -3 10 9.50 2.70 -3 -3 10 7.40 2.00 -2 -3 10 55.69 4.40 -2 -3 10 56.29 5.10 -1 -3 10 0.10 1.10 -1 -3 10 0.20 1.30 0 -3 10 13.20 2.70 1 -3 10 6.30 2.30 1 -3 10 7.60 1.80 2 -3 10 50.99 4.00 2 -3 10 44.60 4.70 3 -3 10 12.00 2.30 3 -3 10 14.30 3.10 4 -3 10 3.10 1.90 4 -3 10 1.30 1.60 -6 -2 10 48.30 5.20 -6 -2 10 39.40 5.70 -5 -2 10 1.90 1.70 -5 -2 10 1.40 2.00 -4 -2 10 124.19 8.20 -4 -2 10 125.49 7.50 -3 -2 10 28.00 3.60 -3 -2 10 32.30 4.30 -2 -2 10 62.79 5.00 -2 -2 10 70.29 4.90 -1 -2 10 0.70 1.60 0 -2 10 2.90 1.60 0 -2 10 3.70 1.70 1 -2 10 -2.50 1.20 1 -2 10 -2.00 1.10 2 -2 10 -0.10 1.70 2 -2 10 1.20 1.40 3 -2 10 8.50 2.00 3 -2 10 13.40 2.90 -6 -1 10 50.79 5.20 -6 -1 10 40.80 5.60 -5 -1 10 4.40 2.10 -5 -1 10 2.70 2.00 -4 -1 10 4.50 2.20 -4 -1 10 3.70 1.60 -3 -1 10 126.19 7.60 -3 -1 10 125.99 7.30 -2 -1 10 4.00 1.80 -1 -1 10 5.80 1.60 -1 -1 10 1.90 1.70 0 -1 10 10.30 2.30 0 -1 10 10.60 2.30 1 -1 10 1.60 1.80 1 -1 10 4.30 1.70 2 -1 10 0.90 1.50 2 -1 10 -0.30 1.40 3 -1 10 25.60 3.40 3 -1 10 33.10 4.40 -6 0 10 24.00 4.40 -6 0 10 23.80 3.60 -5 0 10 6.50 2.40 -5 0 10 4.90 2.00 -4 0 10 11.40 2.60 -4 0 10 17.70 3.30 -3 0 10 144.79 7.80 -3 0 10 126.29 10.00 -2 0 10 1.20 1.50 -2 0 10 0.30 1.50 -1 0 10 17.80 2.60 -1 0 10 20.00 3.20 0 0 10 10.60 2.30 0 0 10 9.60 2.20 1 0 10 2.30 1.80 1 0 10 0.40 1.10 2 0 10 3.00 1.80 2 0 10 2.80 1.70 -6 1 10 -0.10 1.60 -6 1 10 2.20 1.40 -5 1 10 16.90 3.30 -5 1 10 14.90 2.90 -4 1 10 9.70 2.20 -4 1 10 9.90 2.40 -4 1 10 10.30 2.70 -3 1 10 1.70 1.60 -3 1 10 0.70 1.30 -2 1 10 0.20 1.40 -2 1 10 0.10 1.40 -1 1 10 33.60 3.60 -1 1 10 26.80 3.60 0 1 10 53.69 4.20 0 1 10 54.09 4.60 1 1 10 2.50 1.60 1 1 10 4.50 2.00 2 1 10 24.10 3.30 2 1 10 31.60 4.30 -5 2 10 -0.40 1.50 -5 2 10 -0.40 1.30 -5 2 10 1.30 1.40 -4 2 10 28.30 3.70 -4 2 10 29.40 3.40 -3 2 10 3.20 1.70 -3 2 10 10.30 2.40 -2 2 10 10.30 2.20 -2 2 10 9.30 2.10 -1 2 10 6.40 2.20 -1 2 10 9.70 2.30 0 2 10 2.60 1.70 0 2 10 0.30 1.20 1 2 10 0.40 1.20 1 2 10 2.20 2.00 -4 3 10 -0.50 1.30 -4 3 10 2.30 1.40 -4 3 10 0.50 1.10 -4 3 10 1.30 1.60 -3 3 10 2.40 1.70 -3 3 10 2.70 1.80 -3 3 10 3.70 1.90 -2 3 10 6.10 1.90 -2 3 10 5.50 1.90 -2 3 10 6.20 2.20 -1 3 10 10.90 2.50 -1 3 10 11.00 2.40 -1 3 10 9.80 2.70 0 -6 11 1.80 2.00 -2 -5 11 2.60 1.60 -2 -5 11 -0.30 1.70 -1 -5 11 1.00 1.80 0 -5 11 2.90 1.90 1 -5 11 -0.10 1.30 2 -5 11 -0.30 1.40 -3 -4 11 4.30 1.80 -3 -4 11 2.00 2.20 -2 -4 11 2.50 1.90 -1 -4 11 39.00 4.50 0 -4 11 0.00 1.70 1 -4 11 -0.40 1.70 1 -4 11 -0.50 1.40 2 -4 11 18.40 3.40 2 -4 11 13.10 2.50 -4 -3 11 -1.30 1.80 -4 -3 11 0.90 1.80 -3 -3 11 0.60 1.90 -3 -3 11 0.40 1.30 -2 -3 11 40.50 4.60 -1 -3 11 6.80 2.50 0 -3 11 3.10 2.10 1 -3 11 2.80 1.80 1 -3 11 -0.10 1.30 2 -3 11 2.60 2.10 2 -3 11 -0.20 1.50 -4 -2 11 20.90 3.90 -4 -2 11 22.60 3.70 -3 -2 11 13.20 2.70 -2 -2 11 17.20 3.20 -1 -2 11 12.20 2.80 0 -2 11 17.70 2.70 0 -2 11 13.50 2.80 1 -2 11 12.30 2.80 1 -2 11 8.50 2.30 -4 -1 11 10.50 2.50 -3 -1 11 16.30 3.20 -2 -1 11 0.00 1.40 -2 -1 11 1.90 1.90 -1 -1 11 43.40 4.20 -1 -1 11 34.80 4.40 0 -1 11 -2.10 1.50 0 -1 11 -0.70 1.40 1 -1 11 -1.30 1.10 1 -1 11 -0.80 1.00 -4 0 11 2.90 1.80 -3 0 11 1.80 1.90 -3 0 11 -0.70 1.30 -2 0 11 20.80 2.90 -2 0 11 20.50 3.40 -1 0 11 -0.60 1.70 -1 0 11 4.30 1.90 0 0 11 7.60 2.50 0 0 11 0.30 1.30 -3 1 11 10.80 2.60 -3 1 11 6.60 1.90 -2 1 11 9.30 2.60 -2 1 11 8.00 2.20 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 7036 _shelx_res_file ; TITL revised-nu2019 in P-1 shelx.res created by SHELXL-2019/3 at 21:33:02 on 20-Aug-2026 CELL 0.71073 8.4674 9.2193 9.2749 102.838 96.181 108.027 ZERR 2.00 0.0009 0.0011 0.0011 0.004 0.004 0.004 LATT 1 SFAC C H N O F UNIT 30 24 2 8 2 TEMP -123.000 SIZE 0.210 0.300 0.350 DFIX 0.86 0.01 N1 H1N DFIX 0.85 0.01 O1 H1O O4 H4O DFIX 0.95 0.01 C2 H2 C4 H4 C6 H6 C9 H9 C10 H10 C12 H12 C13 H13 DFIX 0.99 0.01 C7 H7A C7 H7B EQIV $1 -x, -y, -z HTAB O1 O2_$1 EQIV $2 -x+2, -y+1, -z HTAB O4 O3_$2 EQIV $3 -x+2, -y+3, -z+1 HTAB C12 F1_$3 EQIV $4 -x+2, -y+2, -z+1 HTAB C12 O3_$4 HTAB O1 O2_$1 HTAB O4 O3_$2 HTAB C12 F1_$3 HTAB C12 O3_$4 FMAP 2 PLAN 5 L.S. 13 ACTA BOND $H CONF HTAB WGHT 0.045700 0.130500 FVAR 0.69665 F1 5 0.904254 1.378216 0.337630 11.00000 0.04916 0.02938 = 0.04712 0.01775 0.01705 0.01518 O1 4 0.063667 0.186705 0.136945 11.00000 0.01811 0.03521 = 0.04755 -0.00646 0.01402 -0.00465 H1O 2 -0.021381 0.101948 0.093178 11.00000 -1.50000 O2 4 0.201808 0.070496 -0.012961 11.00000 0.02652 0.03108 = 0.06076 -0.01619 0.01701 -0.00367 O3 4 0.920153 0.603993 0.118205 11.00000 0.01630 0.02294 = 0.02794 0.00143 0.00772 0.00210 O4 4 0.790972 0.352499 -0.018999 11.00000 0.01760 0.02463 = 0.03446 -0.00074 0.01147 0.00438 H4O 2 0.887879 0.370294 -0.047613 11.00000 -1.50000 N1 3 0.493794 0.706869 0.437565 11.00000 0.01929 0.02472 = 0.03375 -0.00189 0.01175 0.00369 H1N 2 0.400604 0.700344 0.470497 11.00000 0.04336 C1 1 0.495541 0.586450 0.320821 11.00000 0.01981 0.02027 = 0.02373 0.00615 0.00701 0.00706 C2 1 0.349178 0.452346 0.259926 11.00000 0.01582 0.02343 = 0.02627 0.00820 0.00963 0.00589 H2 2 0.247353 0.446296 0.296783 11.00000 0.02410 C3 1 0.350704 0.327874 0.145173 11.00000 0.01580 0.01993 = 0.02355 0.00774 0.00406 0.00343 C4 1 0.496405 0.333610 0.086169 11.00000 0.01887 0.01877 = 0.02037 0.00414 0.00482 0.00622 H4 2 0.498634 0.249109 0.008117 11.00000 0.02129 C5 1 0.639553 0.467457 0.142451 11.00000 0.01517 0.02108 = 0.02033 0.00831 0.00439 0.00676 C6 1 0.639458 0.593418 0.257524 11.00000 0.01516 0.01886 = 0.02352 0.00519 0.00349 0.00282 H6 2 0.737571 0.686545 0.289790 11.00000 0.01708 C7 1 0.645136 0.828709 0.530837 11.00000 0.02588 0.02505 = 0.02217 0.00119 0.00587 0.00722 H7A 2 0.738240 0.784320 0.542554 11.00000 0.02662 H7B 2 0.623106 0.861688 0.633572 11.00000 0.02921 C8 1 0.711481 0.974709 0.475563 11.00000 0.02195 0.02437 = 0.02249 0.00312 0.00758 0.00987 C9 1 0.641427 0.985656 0.337487 11.00000 0.02808 0.02568 = 0.02286 -0.00098 0.00263 0.00954 H9 2 0.546422 0.897461 0.276199 11.00000 0.03381 C10 1 0.705484 1.120908 0.289659 11.00000 0.03820 0.03074 = 0.02189 0.00430 0.00515 0.01780 H10 2 0.660005 1.128078 0.194072 11.00000 0.03873 C11 1 0.839250 1.244350 0.383009 11.00000 0.03172 0.02371 = 0.03298 0.01090 0.01475 0.01404 C12 1 0.911213 1.239753 0.520795 11.00000 0.02351 0.02450 = 0.03821 0.00510 0.00036 0.00458 H12 2 0.999828 1.331041 0.585148 11.00000 0.04165 C13 1 0.846489 1.103700 0.566260 11.00000 0.02829 0.02924 = 0.02871 0.00789 -0.00075 0.00898 H13 2 0.893084 1.094454 0.660898 11.00000 0.02913 C14 1 0.196416 0.184217 0.083480 11.00000 0.01723 0.02505 = 0.02729 0.00433 0.00737 0.00384 C15 1 0.796596 0.481527 0.080012 11.00000 0.01758 0.02256 = 0.01930 0.00574 0.00337 0.00666 HKLF 4 REM revised-nu2019 in P-1 REM wR2 = 0.1022, GooF = S = 1.051, Restrained GooF = 1.050 for all data REM R1 = 0.0388 for 2050 Fo > 4sig(Fo) and 0.0564 for all 2722 data REM 236 parameters refined using 12 restraints END WGHT 0.0457 0.1305 REM Instructions for potential hydrogen bonds HTAB O1 O2_$1 HTAB O4 O3_$2 HTAB C12 F1_$3 HTAB C12 O3_$4 REM Highest difference peak 0.239, deepest hole -0.259, 1-sigma level 0.049 Q1 1 0.2858 0.2624 0.1212 11.00000 0.05 0.24 Q2 1 0.4159 0.3291 0.1281 11.00000 0.05 0.21 Q3 1 0.7170 0.4702 0.1132 11.00000 0.05 0.20 Q4 1 0.9286 1.2142 0.4249 11.00000 0.05 0.17 Q5 1 0.6343 0.5417 0.1756 11.00000 0.05 0.17 ; _shelx_res_checksum 32715 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 _atom_site_disorder_assembly _atom_site_disorder_group F F1 0.90425(13) 1.37822(11) 0.33763(12) 0.0396(3) Uani d 1 . . O O1 0.06367(14) 0.18670(14) 0.13695(15) 0.0393(3) Uani d 1 . . H H1O -0.021(2) 0.1019(17) 0.093(2) 0.059 Uiso d 1 . . O O2 0.20181(15) 0.07050(14) -0.01296(16) 0.0469(4) Uani d 1 . . O O3 0.92015(12) 0.60399(12) 0.11820(12) 0.0242(3) Uani d 1 . . O O4 0.79097(13) 0.35250(12) -0.01900(13) 0.0272(3) Uani d 1 . . H H4O 0.8879(15) 0.370(2) -0.048(2) 0.041 Uiso d 1 . . N N1 0.49379(17) 0.70687(15) 0.43757(16) 0.0280(3) Uani d 1 . . H H1N 0.4006(16) 0.700(2) 0.470(2) 0.043(6) Uiso d 1 . . C C1 0.49554(18) 0.58645(17) 0.32082(17) 0.0210(3) Uani d 1 . . C C2 0.34918(19) 0.45235(17) 0.25993(18) 0.0213(3) Uani d 1 . . H H2 0.2474(14) 0.4463(18) 0.2968(17) 0.024(4) Uiso d 1 . . C C3 0.35070(18) 0.32787(17) 0.14517(17) 0.0201(3) Uani d 1 . . C C4 0.49641(18) 0.33361(17) 0.08617(17) 0.0195(3) Uani d 1 . . H H4 0.4986(18) 0.2491(14) 0.0081(14) 0.021(4) Uiso d 1 . . C C5 0.63955(17) 0.46746(16) 0.14245(16) 0.0182(3) Uani d 1 . . C C6 0.63946(18) 0.59342(17) 0.25752(17) 0.0200(3) Uani d 1 . . H H6 0.7376(14) 0.6865(13) 0.2898(16) 0.017(4) Uiso d 1 . . C C7 0.6451(2) 0.82871(18) 0.53084(18) 0.0255(4) Uani d 1 . . H H7A 0.7382(16) 0.7843(17) 0.5426(18) 0.027(4) Uiso d 1 . . H H7B 0.623(2) 0.8617(19) 0.6336(12) 0.029(4) Uiso d 1 . . C C8 0.71148(19) 0.97471(17) 0.47556(17) 0.0227(4) Uani d 1 . . C C9 0.6414(2) 0.98566(18) 0.33749(18) 0.0269(4) Uani d 1 . . H H9 0.5464(16) 0.8975(15) 0.2762(17) 0.034(5) Uiso d 1 . . C C10 0.7055(2) 1.12091(19) 0.28966(19) 0.0294(4) Uani d 1 . . H H10 0.660(2) 1.128(2) 0.1941(14) 0.039(5) Uiso d 1 . . C C11 0.8393(2) 1.24435(18) 0.38301(19) 0.0271(4) Uani d 1 . . C C12 0.9112(2) 1.23975(19) 0.5208(2) 0.0306(4) Uani d 1 . . H H12 0.9998(18) 1.3310(15) 0.5851(18) 0.042(5) Uiso d 1 . . C C13 0.8465(2) 1.10370(19) 0.5663(2) 0.0295(4) Uani d 1 . . H H13 0.8931(19) 1.0945(19) 0.6609(13) 0.029(4) Uiso d 1 . . C C14 0.19642(19) 0.18422(18) 0.08348(18) 0.0242(4) Uani d 1 . . C C15 0.79660(18) 0.48153(17) 0.08001(17) 0.0199(3) Uani 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 F1 0.0492(6) 0.0294(5) 0.0471(7) 0.0152(5) 0.0171(5) 0.0177(5) O1 0.0181(6) 0.0352(7) 0.0475(8) -0.0046(5) 0.0140(6) -0.0065(6) O2 0.0265(7) 0.0311(7) 0.0608(9) -0.0037(5) 0.0170(6) -0.0162(6) O3 0.0163(5) 0.0229(5) 0.0279(6) 0.0021(4) 0.0077(5) 0.0014(5) O4 0.0176(6) 0.0246(6) 0.0345(7) 0.0044(5) 0.0115(5) -0.0007(5) N1 0.0193(7) 0.0247(7) 0.0337(8) 0.0037(6) 0.0118(6) -0.0019(6) C1 0.0198(8) 0.0203(7) 0.0237(8) 0.0071(6) 0.0070(6) 0.0062(6) C2 0.0158(8) 0.0234(8) 0.0263(8) 0.0059(6) 0.0096(6) 0.0082(6) C3 0.0158(7) 0.0199(7) 0.0235(8) 0.0034(6) 0.0041(6) 0.0077(6) C4 0.0189(8) 0.0188(7) 0.0204(8) 0.0062(6) 0.0048(6) 0.0041(6) C5 0.0152(7) 0.0211(7) 0.0203(8) 0.0068(6) 0.0044(6) 0.0083(6) C6 0.0152(7) 0.0189(7) 0.0235(8) 0.0028(6) 0.0035(6) 0.0052(6) C7 0.0259(9) 0.0250(8) 0.0222(8) 0.0072(7) 0.0059(7) 0.0012(7) C8 0.0219(8) 0.0244(8) 0.0225(8) 0.0099(6) 0.0076(6) 0.0031(6) C9 0.0281(9) 0.0257(8) 0.0229(9) 0.0095(7) 0.0026(7) -0.0010(7) C10 0.0382(10) 0.0307(9) 0.0219(9) 0.0178(8) 0.0051(7) 0.0043(7) C11 0.0317(9) 0.0237(8) 0.0330(9) 0.0140(7) 0.0148(8) 0.0109(7) C12 0.0235(9) 0.0245(8) 0.0382(10) 0.0046(7) 0.0004(7) 0.0051(7) C13 0.0283(9) 0.0292(9) 0.0287(9) 0.0090(7) -0.0007(7) 0.0079(7) C14 0.0172(8) 0.0250(8) 0.0273(9) 0.0038(6) 0.0074(7) 0.0043(7) C15 0.0176(8) 0.0226(8) 0.0193(8) 0.0067(6) 0.0034(6) 0.0057(6) 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' F F 0.0171 0.0103 '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_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C14 O1 H1O . . 111.3(15) ? C15 O4 H4O . . 108.2(12) ? C1 N1 C7 . . 123.58(13) ? C1 N1 H1N . . 119.1(13) ? C7 N1 H1N . . 116.0(13) ? N1 C1 C6 . . 121.89(13) ? N1 C1 C2 . . 120.03(13) ? C6 C1 C2 . . 118.07(14) ? C3 C2 C1 . . 120.61(14) ? C3 C2 H2 . . 119.2(9) ? C1 C2 H2 . . 120.2(9) ? C2 C3 C4 . . 120.87(13) ? C2 C3 C14 . . 120.43(13) ? C4 C3 C14 . . 118.69(13) ? C5 C4 C3 . . 118.82(13) ? C5 C4 H4 . . 119.8(9) ? C3 C4 H4 . . 121.4(9) ? C4 C5 C6 . . 120.82(13) ? C4 C5 C15 . . 120.91(13) ? C6 C5 C15 . . 118.26(13) ? C5 C6 C1 . . 120.73(13) ? C5 C6 H6 . . 118.9(9) ? C1 C6 H6 . . 120.3(9) ? N1 C7 C8 . . 115.64(13) ? N1 C7 H7A . . 110.0(9) ? C8 C7 H7A . . 107.8(9) ? N1 C7 H7B . . 108.8(10) ? C8 C7 H7B . . 108.6(10) ? H7A C7 H7B . . 105.5(14) ? C9 C8 C13 . . 118.46(15) ? C9 C8 C7 . . 122.41(14) ? C13 C8 C7 . . 119.12(14) ? C10 C9 C8 . . 121.07(15) ? C10 C9 H9 . . 120.6(10) ? C8 C9 H9 . . 118.3(10) ? C11 C10 C9 . . 118.13(15) ? C11 C10 H10 . . 120.4(11) ? C9 C10 H10 . . 121.5(11) ? F1 C11 C12 . . 118.15(15) ? F1 C11 C10 . . 118.95(15) ? C12 C11 C10 . . 122.90(16) ? C11 C12 C13 . . 118.20(15) ? C11 C12 H12 . . 120.2(11) ? C13 C12 H12 . . 121.5(11) ? C12 C13 C8 . . 121.23(16) ? C12 C13 H13 . . 121.3(10) ? C8 C13 H13 . . 117.5(10) ? O2 C14 O1 . . 123.59(14) ? O2 C14 C3 . . 119.88(14) ? O1 C14 C3 . . 116.53(13) ? O3 C15 O4 . . 123.33(13) ? O3 C15 C5 . . 122.30(13) ? O4 C15 C5 . . 114.37(12) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 C11 . 1.3651(18) ? O1 C14 . 1.2809(19) ? O1 H1O . 0.861(10) ? O2 C14 . 1.2341(19) ? O3 C15 . 1.2273(17) ? O4 C15 . 1.3156(17) ? O4 H4O . 0.868(9) ? N1 C1 . 1.3728(19) ? N1 C7 . 1.4460(19) ? N1 H1N . 0.866(9) ? C1 C6 . 1.399(2) ? C1 C2 . 1.405(2) ? C2 C3 . 1.385(2) ? C2 H2 . 0.952(9) ? C3 C4 . 1.394(2) ? C3 C14 . 1.490(2) ? C4 C5 . 1.384(2) ? C4 H4 . 0.945(9) ? C5 C6 . 1.392(2) ? C5 C15 . 1.488(2) ? C6 H6 . 0.953(9) ? C7 C8 . 1.514(2) ? C7 H7A . 1.001(9) ? C7 H7B . 0.990(9) ? C8 C9 . 1.390(2) ? C8 C13 . 1.391(2) ? C9 C10 . 1.387(2) ? C9 H9 . 0.961(9) ? C10 C11 . 1.371(2) ? C10 H10 . 0.952(9) ? C11 C12 . 1.371(2) ? C12 C13 . 1.382(2) ? C12 H12 . 0.958(9) ? C13 H13 . 0.955(9) ? 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 C9 H9 N1 . 0.961(9) 2.521(14) 2.890(2) 102.8(10) yes O1 H1O O2 2 0.861(10) 1.772(10) 2.6326(16) 177(2) yes O4 H4O O3 2_765 0.868(9) 1.785(10) 2.6518(15) 176.0(18) yes N1 H1N Cg2 2_676 0.866(9) 2.705(16) 3.4071(17) 139.3(15) yes C12 H12 F1 2_786 0.958(9) 2.456(13) 3.2661(19) 142.2(14) yes C12 H12 O3 2_776 0.958(9) 2.646(16) 3.298(2) 125.7(13) 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C7 N1 C1 C6 . . . . -16.8(2) ? C7 N1 C1 C2 . . . . 164.21(15) ? N1 C1 C2 C3 . . . . -178.04(14) ? C6 C1 C2 C3 . . . . 2.9(2) ? C1 C2 C3 C4 . . . . -0.9(2) ? C1 C2 C3 C14 . . . . 178.51(14) ? C2 C3 C4 C5 . . . . -1.1(2) ? C14 C3 C4 C5 . . . . 179.50(14) ? C3 C4 C5 C6 . . . . 1.0(2) ? C3 C4 C5 C15 . . . . -178.08(13) ? C4 C5 C6 C1 . . . . 1.1(2) ? C15 C5 C6 C1 . . . . -179.77(13) ? N1 C1 C6 C5 . . . . 177.92(14) ? C2 C1 C6 C5 . . . . -3.1(2) ? C1 N1 C7 C8 . . . . 89.38(19) ? N1 C7 C8 C9 . . . . -5.7(2) ? N1 C7 C8 C13 . . . . 173.68(14) ? C13 C8 C9 C10 . . . . 0.8(2) ? C7 C8 C9 C10 . . . . -179.75(14) ? C8 C9 C10 C11 . . . . -0.5(2) ? C9 C10 C11 F1 . . . . 179.82(14) ? C9 C10 C11 C12 . . . . -0.3(2) ? F1 C11 C12 C13 . . . . -179.42(14) ? C10 C11 C12 C13 . . . . 0.7(3) ? C11 C12 C13 C8 . . . . -0.3(3) ? C9 C8 C13 C12 . . . . -0.4(2) ? C7 C8 C13 C12 . . . . -179.85(15) ? C2 C3 C14 O2 . . . . -176.06(16) ? C4 C3 C14 O2 . . . . 3.3(2) ? C2 C3 C14 O1 . . . . 3.2(2) ? C4 C3 C14 O1 . . . . -177.37(14) ? C4 C5 C15 O3 . . . . 173.38(14) ? C6 C5 C15 O3 . . . . -5.7(2) ? C4 C5 C15 O4 . . . . -6.4(2) ? C6 C5 C15 O4 . . . . 174.48(13) ?