Diosgenin hemihydrate
Hernández Linares, María-Guadalupe; Bernès, Sylvain; Flores-Alamo, Marcos; Guerrero-Luna, Gabriel; Martínez-Gallegos, Anselmo A.; Acta Crystallographica Section E 68 (2012) o2357–; doi:10.1107/S1600536812027912

data_2235806
_publ_section_title
;
 Diosgenin hemihydrate
;
_journal_coeditor_code           GG2085
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2357
_journal_paper_doi               10.1107/S1600536812027912
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C27 H42 O3, 0.5H2 O'
_chemical_formula_moiety         'C27 H42 O3, 0.5(H2 O)'
_chemical_formula_sum            'C27 H43 O3.5'
_chemical_formula_weight         423.61
_chemical_melting_point          590
_chemical_name_common
;
Diosgenin hemihydrate
;
_chemical_name_systematic
;
(25<i>R</i>)-Spirost-5-en-3-ol hemihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.3483(5)
_cell_length_b                   19.698(2)
_cell_length_c                   33.440(3)
_cell_measurement_reflns_used    1880
_cell_measurement_temperature    136(2)
_cell_measurement_theta_max      67.6627
_cell_measurement_theta_min      3.4644
_cell_volume                     4840.3(7)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      136(2)
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Atlas Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.1313
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            17450
_diffrn_reflns_theta_full        67.40
_diffrn_reflns_theta_max         67.40
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2009); based on expressions derived
by
Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.5031
_exptl_crystal_size_mid          0.1715
_exptl_crystal_size_min          0.0309
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     570
_refine_ls_number_reflns         4918
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0722
_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^)+(0.05P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                3573
_reflns_number_total             4918
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg2085.cif
_cod_data_source_block           I
_cod_original_cell_volume        4840.3(8)
_cod_original_formula_sum        'C27 H43 O3.50'
_cod_database_code               2235806
_cod_database_fobs_code          2235806