Understanding the thermal stability of apalutamide crystalline solvates through crystal structure analyses and computational studies
Prashanth, Jupally; Arikatla, Sivalakshmi Devi; Surov, Artem; Voronin, Alexander P.; Andrei, Churakov; Perlovich, German L.; Balasubramanian, Sridhar; CrystEngComm  (2022) –; doi:10.1039/D2CE00216G

data_7244688
_publ_section_title
;
 Understanding the thermal stability of apalutamide crystalline solvates
 through crystal structure analyses and computational studies
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00216G
_journal_year                    2022
_chemical_formula_moiety         '2(C21 H15 F4 N5 O2 S), C4 H8 O2'
_chemical_formula_sum            'C46 H38 F8 N10 O6 S2'
_chemical_formula_weight         1042.98
_chemical_name_common            Apalutamide-1,4-dioxane-2:1
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-15 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.9090(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.7833(6)
_cell_length_b                   13.6224(2)
_cell_length_c                   17.4061(3)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.50
_cell_volume                     9254.9(3)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36635
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         2.165
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9440
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0832
_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^)+(0.0679P)^2^+56.7028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.2010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6534
_reflns_number_total             9440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00216g2.cif
_cod_data_source_block           KA1156_0m_APA-DOX-2-1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7244688
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              5429