Investigation of the solid forms of deferasirox: solvate, co-crystal, and amorphous form
Du, Qiaohong; Xiong, Xinnuo; Suo, Zili; Tang, Peixiao; He, Jiawei; Zeng, Xia; Hou, Quan; Li, Hui; RSC Adv. 7 (2017) 43151–; doi:10.1039/C7RA08077H

data_7229082
_publ_section_title
;
 Investigation of the solid forms of deferasirox: solvate, co-crystal, and
 amorphous form
;
_journal_issue                   68
_journal_name_full               'RSC Adv.'
_journal_page_first              43151
_journal_paper_doi               10.1039/C7RA08077H
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C21 H15 N3 O4, C6 H6 N2 O'
_chemical_formula_sum            'C27 H21 N5 O5'
_chemical_formula_weight         495.49
_chemical_name_systematic        DFX-INA
_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     iterative
_audit_creation_date             2017-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-06-12 deposited with the CCDC.
2017-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.206(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3205(3)
_cell_length_b                   36.1503(10)
_cell_length_c                   7.1171(3)
_cell_measurement_reflns_used    5258
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5110
_cell_measurement_theta_min      3.1750
_cell_volume                     2360.08(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -28.00   54.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106   44.0000  106.0000 164

  2 omega  -83.00    1.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106  -44.0000  -43.0000 168

  3 omega  -33.00   -8.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.6856  -44.0000  -43.0000 50

  4 omega  -76.00  -35.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106 -178.0000  150.0000 82

  5 omega  -79.00  -35.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106 -178.0000   60.0000 88

  6 omega  -64.00  -38.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106    0.0000 -150.0000 52

  7 omega  -27.00   -2.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106    0.0000 -150.0000 50

  8 omega   29.00   54.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106    0.0000 -150.0000 50

  9 omega  -25.00   23.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106  -99.0000 -120.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0529269000
_diffrn_orient_matrix_UB_12      -0.0093059000
_diffrn_orient_matrix_UB_13      0.0429456000
_diffrn_orient_matrix_UB_21      0.0552382000
_diffrn_orient_matrix_UB_22      -0.0056185000
_diffrn_orient_matrix_UB_23      0.0764391000
_diffrn_orient_matrix_UB_31      -0.0111752000
_diffrn_orient_matrix_UB_32      0.0163302000
_diffrn_orient_matrix_UB_33      0.0507087000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            20181
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.962
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0482P)^2^+0.6851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3876
_reflns_number_total             4815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra08077h2.cif
_cod_data_source_block           161206_s3_dqh
_cod_original_cell_volume        2360.06(13)
_cod_database_code               7229082
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.966
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26)
2.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'