The crystal structure of iguratimod-dimethylformamide (1/1), C17H14N2O6S·C3H7NO
Ma, Wen-Jing; Wang, Hao; Wang, Zhen-Yu; Long, Yu-Xuan; Wang, Xin-Qi; Ma, Qian; Xu, Cui-Ran; Ma, Yu-Heng; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 577–578; doi:10.1515/ncrs-2023-0101

data_8107499
_publ_section_title
;
 The crystal structure of iguratimod-dimethylformamide (1/1),
 C17H14N2O6S&#x00B7;C3H7NO
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              577
_journal_page_last               578
_journal_paper_doi               10.1515/ncrs-2023-0101
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C17 H14 N2 O6 S, C3 H7 N O'
_chemical_formula_sum            'C20 H21 N3 O7 S'
_chemical_formula_weight         447.46
_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   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                85.238(2)
_cell_angle_beta                 86.674(2)
_cell_angle_gamma                78.959(2)
_cell_formula_units_Z            2
_cell_length_a                   5.4146(4)
_cell_length_b                   11.7925(8)
_cell_length_c                   16.9527(12)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    295.78
_cell_measurement_theta_max      68.3211
_cell_measurement_theta_min      4.7974
_cell_volume                     1057.77(13)
_computing_cell_refinement       'APEX2-2008 [1]'
_computing_data_collection       'APEX2-2008 [1]'
_computing_data_reduction        'SAINT- 2008 [1]'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)[2]'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)[2]'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)[3,4]'
_computing_structure_solution    'Olex2 1.5 (Dolomanov et al., 2009)[2]'
_diffrn_ambient_temperature      295.78
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-AXS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24753
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.406
_diffrn_reflns_theta_min         4.797
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       needle
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0087(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3854
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.3786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3546
_reflns_number_total             3854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0101_suppl_001.cif
_cod_data_source_block           1
_cod_database_code               8107499
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.674
_olex2_refinement_description
;
1. Restrained distances
 O1-O7
 2.9 with sigma of 0.01
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C11(H11), C8(H8), C15(H15), C16(H16), C18(H18), C4(H4), C6(H6),
 C2(H2A), C5(H5), C3(H3)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              53230
_shelx_hkl_checksum              9317