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_7229079
_publ_section_title
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 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, H2 O'
_chemical_formula_sum            'C21 H17 N3 O5'
_chemical_formula_weight         391.38
_chemical_name_systematic        DFX-H2O
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-10 deposited with the CCDC.
2017-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.790(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9201(2)
_cell_length_b                   29.7303(8)
_cell_length_c                   7.20740(19)
_cell_measurement_reflns_used    2945
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6070
_cell_measurement_theta_min      3.4860
_cell_volume                     1893.74(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   -6.00   45.00   0.3000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       16.6856  -19.0000  -60.0000 170

  2 omega  -21.00    9.00   0.3000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000 -120.0000 100

  3 omega  -11.00   83.20   0.3000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       16.6856   19.0000  150.0000 314

  4 omega  -87.00  -48.00   0.3000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669 -178.0000   90.0000 130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0065786000
_diffrn_orient_matrix_UB_12      0.0189971000
_diffrn_orient_matrix_UB_13      -0.0579106000
_diffrn_orient_matrix_UB_21      -0.0691282000
_diffrn_orient_matrix_UB_22      0.0085569000
_diffrn_orient_matrix_UB_23      0.0237603000
_diffrn_orient_matrix_UB_31      0.0402239000
_diffrn_orient_matrix_UB_32      0.0116206000
_diffrn_orient_matrix_UB_33      0.0771390000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8581
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89445
_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            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.3557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                3107
_reflns_number_total             3848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra08077h2.cif
_cod_data_source_block           160419_s4_dqh
_cod_original_cell_volume        1893.75(8)
_cod_database_code               7229079
_chemical_oxdiff_formula         c12h12n2o3
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b 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)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'