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_7243675
_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, C H4 O'
_chemical_formula_sum            'C31 H35 Cl N6 O6 S'
_chemical_formula_weight         655.16
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.725(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5891(8)
_cell_length_b                   7.5159(3)
_cell_length_c                   15.6522(9)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      2.6
_cell_volume                     1571.22(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Mova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6669
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.630
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       Needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 1398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5283
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0318P)^2^+0.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.583
_reflns_Friedel_fraction_full    0.716
_reflns_Friedel_fraction_max     0.685
_reflns_number_gt                4571
_reflns_number_total             5283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01269j3.txt
_cod_data_source_block           SRX-PTSA-MeOH
_cod_depositor_comments
'Adding full bibliography for 7243671--7243675.cif.'
_cod_original_cell_volume        1571.22(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7243675
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              4317
_shelx_hkl_checksum              17517