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_7229081
_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, 2(C6 H6 N2 O)'
_chemical_formula_sum            'C33 H27 N7 O6'
_chemical_formula_weight         617.61
_chemical_name_systematic        DFX-2INA
_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
_atom_sites_solution_primary     direct
_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                 101.377(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5782(6)
_cell_length_b                   8.4837(2)
_cell_length_c                   37.8874(12)
_cell_measurement_reflns_used    6191
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8440
_cell_measurement_theta_min      3.4960
_cell_volume                     6799.5(3)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega  -20.00   52.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6336   57.0000  -90.0000 360

  2 omega    2.00   79.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3523   57.0000 -120.0000 385

  3 omega   -2.00   23.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6336  -99.0000 -150.0000 125

  4 omega   25.00   50.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3523 -150.0000 -104.0000 125

  5 omega    7.00   32.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3523 -122.0000   57.0000 125

  6 omega  -24.00   19.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6336  -99.0000   60.0000 215

  7 omega  -65.00  -40.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6336 -178.0000  120.0000 125

  8 omega  -55.00  -30.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6336  122.0000  138.0000 125

  9 omega   36.00   72.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3523  178.0000  150.0000 180

 10 omega  -72.00  -47.00   0.2000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6336  150.0000  -59.0000 125
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018591000
_diffrn_orient_matrix_UB_12      -0.0827772000
_diffrn_orient_matrix_UB_13      -0.0026353000
_diffrn_orient_matrix_UB_21      0.0027226000
_diffrn_orient_matrix_UB_22      -0.0111930000
_diffrn_orient_matrix_UB_23      0.0187881000
_diffrn_orient_matrix_UB_31      -0.0333800000
_diffrn_orient_matrix_UB_32      0.0037400000
_diffrn_orient_matrix_UB_33      -0.0021055000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            24099
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41426
_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    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0602P)^2^+2.8861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5564
_reflns_number_total             6852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra08077h2.cif
_cod_data_source_block           161128_s2_dqh
_cod_database_code               7229081
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.967
_reflns_odcompleteness_completeness 98.07
_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) 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),
  C29(H29), C30(H30), C31(H31), C32(H32)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'