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_7243671
_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_absolute_configuration rm
_chemical_formula_moiety         'C7 H7 O3 S, C23 H24 Cl N6 O2'
_chemical_formula_sum            'C30 H31 Cl N6 O5 S'
_chemical_formula_weight         623.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 92.42(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.247(6)
_cell_length_b                   7.6192(16)
_cell_length_c                   15.469(10)
_cell_measurement_reflns_used    1100
_cell_measurement_temperature    394(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      2.6
_cell_volume                     1559.9(13)
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      394(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.3514
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.146
_diffrn_reflns_theta_min         2.636
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       Block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.205
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_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.4052
_refine_ls_R_factor_gt           0.0956
_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^)+(0.0244P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.2293
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                1092
_reflns_number_total             5302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01269j4.txt
_cod_data_source_block           SRX-PTSA
_cod_depositor_comments
'Adding full bibliography for 7243671--7243675.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7243671
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              93072
_shelx_hkl_checksum              47243