Two anhydrous forms and one monohydrate of a cocrystal of axitinib and glutaric acid: characterization, property evaluation and phase transition study
Ren, Bo-Ying; Dai, Xia-Lin; Chen, Jia-Mei; Lu, Tong-Bu; CrystEngComm  (2022) –; doi:10.1039/D1CE01740C

data_7244533
_publ_section_title
;
 Two anhydrous forms and one monohydrate of a cocrystal of axitinib and
 glutaric acid: characterization, property evaluation and phase transition
 study
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01740C
_journal_year                    2022
_chemical_formula_moiety         'C22 H18 N4 O S, C5 H8 O4'
_chemical_formula_sum            'C27 H26 N4 O5 S'
_chemical_formula_weight         518.58
_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
_audit_creation_date             2021-11-28
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2021-11-28 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                65.633(3)
_cell_angle_beta                 83.024(2)
_cell_angle_gamma                77.802(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6975(2)
_cell_length_b                   12.7075(3)
_cell_length_c                   14.7757(4)
_cell_measurement_reflns_used    10522
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      79.1230
_cell_measurement_theta_min      3.2670
_cell_volume                     1285.88(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14648
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.314
_diffrn_reflns_theta_min         3.286
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68363
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5413
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.4355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4971
_reflns_number_total             5413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01740c2.cif
_cod_data_source_block           axi-ga
_cod_original_cell_volume        1285.88(6)
_cod_database_code               7244533
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C24(H24A,H24B), C26(H26A,H26B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C16(H16), C7(H7), C11(H11), C19(H19), C14(H14), C4(H4A),
 C18(H18), C17(H17), C6(H6), C1(H1), C13(H13), C3(H3A), C2(H2)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              69283
_shelx_hkl_checksum              57159
_olex2_submission_special_instructions 'No special instructions were received'