Solubility, crystallization process optimization, and thermal properties of afoxolaner and the single-crystal structure of its hydrate
Fang, Zong-Bin; Xiao, Yue-Feng; Sun, Chong; Chen, Xinyao; Zhou, Lingyu; Chen, Li; Lu, Qiaomei; Xiao, Wang-Dong; Wu, Shu-Ting; CrystEngComm 27 (2025) 795–800; doi:10.1039/D4CE00975D

data_7249687
_publ_section_title
;
 Solubility, crystallization process optimization, and thermal properties
 of afoxolaner and the single-crystal structure of its hydrate
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              795
_journal_page_last               800
_journal_paper_doi               10.1039/D4CE00975D
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C52 H34 Cl2 F18 N6 O7'
_chemical_formula_weight         1267.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2024-11-13 deposited with the CCDC.	2024-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.354(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5511(3)
_cell_length_b                   37.3176(14)
_cell_length_c                   16.5685(5)
_cell_measurement_reflns_used    99.9(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.8040
_cell_measurement_theta_min      2.5370
_cell_volume                     5271.9(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type
'CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.269
_diffrn_reflns_theta_min         2.059
_exptl_absorpt_coefficient_mu    1.445
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       needle
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.556
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1432
_refine_ls_number_reflns         11714
_refine_ls_number_restraints     1061
_refine_ls_restrained_S_all      1.560
_refine_ls_R_factor_all          0.1876
_refine_ls_R_factor_gt           0.1374
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3951
_refine_ls_wR_factor_ref         0.4182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7721
_reflns_number_total             11714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00975d2.cif
_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 7249687.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7249687
_shelx_estimated_absorpt_t_min   0.478
_shelx_estimated_absorpt_t_max   0.869
_shelxl_version_number           2014-3
_shelx_res_checksum              56811
_shelx_hkl_checksum              85248