A Spironolactone−Saccharin 1:1 Cocrystal Hemihydrate
Takata, Noriyuki; Takano, Ryusuke; Uekusa, Hidehiro; Hayashi, Yoshiki; Terada, Katsuhide; Crystal Growth & Design 10 (2010) 2116–; doi:10.1021/cg901242q

data_4502457
_publ_section_title
;
 A Spironolactone&#x2212;Saccharin 1:1 Cocrystal Hemihydrate
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2116
_journal_paper_doi               10.1021/cg901242q
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C24 H32 O4 S, 0.33(H2 O)'
_chemical_formula_sum            'C24 H32.67 O4.33 S'
_chemical_formula_weight         422.53
_chemical_name_common            'spironolactone saccharin 1/3 hydrate'
_chemical_name_systematic
;
7a-Acetylthio-3-oxo-17a-pregn-4-ene-21,17- carbolactone
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            12
_cell_length_a                   14.0133(3)
_cell_length_b                   15.6692(3)
_cell_length_c                   30.9146(6)
_cell_measurement_reflns_used    36803
_cell_measurement_temperature    223.2
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.2
_cell_volume                     6788.1(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            71139
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2727.72
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5502 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00099(5)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     795
_refine_ls_number_reflns         12255
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0200P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                7500
_reflns_number_total             12255
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            cg901242q_si_003.cif
_cod_data_source_block           SPI_hydrate
_cod_original_formula_sum        'C24 H32.67 O4.33 S '
_cod_database_code               4502457