Solvates and polymorphs of rebamipide: preparation, characterization, and physicochemical analysis
Xiong, Xinnuo; Du, Qiaohong; Zeng, Xia; He, Jiawei; Yang, Hongqin; Li, Hui; RSC Adv. 7 (2017) 23279–; doi:10.1039/C7RA02895D

data_7228138
_publ_section_title
;
 Solvates and polymorphs of rebamipide: preparation, characterization, and
 physicochemical analysis
;
_journal_issue                   38
_journal_name_full               'RSC Adv.'
_journal_page_first              23279
_journal_paper_doi               10.1039/C7RA02895D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C19 H15 Cl N2 O4, C H2 Cl2'
_chemical_formula_sum            'C20 H17 Cl3 N2 O4'
_chemical_formula_weight         455.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-22 deposited with the CCDC.
2017-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 136.08(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3285(16)
_cell_length_b                   9.7542(4)
_cell_length_c                   21.475(2)
_cell_measurement_reflns_used    2179
_cell_measurement_temperature    142.95(10)
_cell_measurement_theta_max      27.4520
_cell_measurement_theta_min      3.4340
_cell_volume                     2081.9(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      142.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -21.00  10.00   1.00    7.50    --  -14.97 -99.00-150.00   31
  2  \w    -47.00  45.00   1.00    7.50    --   16.69 -19.00  30.00   92
  3  \w    -52.00  32.00   1.00    7.50    --   16.69 -19.00 -60.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407074000
_diffrn_orient_matrix_UB_12      -0.0112349000
_diffrn_orient_matrix_UB_13      0.0070693000
_diffrn_orient_matrix_UB_21      0.0428028000
_diffrn_orient_matrix_UB_22      -0.0545278000
_diffrn_orient_matrix_UB_23      0.0298331000
_diffrn_orient_matrix_UB_31      0.0400471000
_diffrn_orient_matrix_UB_32      0.0467860000
_diffrn_orient_matrix_UB_33      0.0364481000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8491
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         8491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1059P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                4598
_reflns_number_total             8491
_reflns_threshold_expression     >2sigma(I)
_twin_special_details
;
Component 2 rotated by 4.0599\% 
 around [0.44 0.06 -0.90] (reciprocal) or [0.03 0.30 -0.95] (direct)
;
_cod_data_source_file            c7ra02895d2.cif
_cod_data_source_block           twin_twin1_hklf4
_cod_original_cell_volume        2081.9(3)
_cod_database_code               7228138
_chemical_oxdiff_formula         c8h4o4n2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5891(10) 0.4109(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3.a Ternary CH refined with riding coordinates:
 C11(H11)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C5(H5), C6(H6), C7(H7), C8(H8), C15(H15), C16(H16), C18(H18),
  C19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.084
_oxdiff_exptl_absorpt_empirical_full_min 0.853
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2