Novel solid forms of insomnia drug suvorexant with improved solubility and dissolution: accessing salts from a salt solvate route
Gundlapalli, Suman; Devarapalli, Ramesh; Mudda, Ramesh Reddy; Chennuru, Ramanaiah; Rupakula, Ravichandrababu; CrystEngComm 23 (2021) 7739–7749; doi:10.1039/D1CE01269J

data_7243674
_publ_section_title
;
 Novel solid forms of insomnia drug suvorexant with improved solubility
 and dissolution: accessing salts from a salt solvate route
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7739
_journal_page_last               7749
_journal_paper_doi               10.1039/D1CE01269J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C23 H24 Cl N6 O2, C6 H5 O3 S'
_chemical_formula_sum            'C29 H29 Cl N6 O5 S'
_chemical_formula_weight         609.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.993(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4711(18)
_cell_length_b                   7.0655(6)
_cell_length_c                   13.0349(12)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.7
_cell_volume                     1376.4(2)
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.1269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11028
_diffrn_reflns_point_group_measured_fraction_full 0.846
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.726
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 912 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.02(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4538
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.681
_reflns_Friedel_fraction_full    0.691
_reflns_Friedel_fraction_max     0.683
_reflns_number_gt                3300
_reflns_number_total             4538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01269j2.txt
_cod_data_source_block           SRX-BSA
_cod_depositor_comments
'Adding full bibliography for 7243671--7243675.cif.'
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7243674
_shelxl_version_number           2013-4
_shelx_res_checksum              56713
_shelx_hkl_checksum              40448