Isomorphous Salts of Anti-HIV Saquinavir Mesylate: Exploring the Effect of Anion-Exchange on Its Solid-State and Dissolution Properties
Fandaruff, Cinira; Chelazzi, Laura; Braga, Dario; Cuffini, Silvia Lucia; Silva, Marcos Antônio Segatto; Resende, Jackson A. L. C.; Dichiarante, Elena; Grepioni, Fabrizia; Crystal Growth & Design 15 (2015) 5233–; doi:10.1021/acs.cgd.5b00696

data_4516371
_publ_section_title
;
 Isomorphous Salts of Anti-HIV Saquinavir Mesylate: Exploring the Effect
 of Anion-Exchange on Its Solid-State and Dissolution Properties
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5233
_journal_paper_doi               10.1021/acs.cgd.5b00696
_journal_volume                  15
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_sum            'C38 H55 Br N6 O7'
_chemical_formula_weight         787.79
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 111.404(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3053(7)
_cell_length_b                   9.7478(4)
_cell_length_c                   15.84700(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2057.38(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10264
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.614
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.279
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.051
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 904 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6901
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.377
_reflns_Friedel_fraction_full    0.500
_reflns_Friedel_fraction_max     0.356
_reflns_number_gt                4168
_reflns_number_total             6901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00696_si_002.cif
_cod_data_source_block           3_SQVBr
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4516371
_shelx_shelxl_version_number     2014/7