Diosgenin-3,6-dione: second polymorph in space group <i>P</i>2~1~2~1~2~1~
Guerrero-Luna, Gabriel; Reyes Melchor, Jaquelin; Bernès, Sylvain; Hernández-Linares, María-Guadalupe; IUCrData 5 (2020) x201200–; doi:10.1107/S2414314620012006

data_1559020
_publ_section_title
;
 Diosgenin-3,6-dione: second polymorph in space group <i>P</i>2~1~2~1~2~1~
;
_journal_coeditor_code           ZQ4041
_journal_issue                   9
_journal_name_full               IUCrData
_journal_page_first              x201200
_journal_paper_doi               10.1107/S2414314620012006
_journal_volume                  5
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_iupac          'C27 H38 O4'
_chemical_formula_moiety         'C27 H38 O4'
_chemical_formula_sum            'C27 H38 O4'
_chemical_formula_weight         426.57
_chemical_melting_point          453
_chemical_name_systematic
;
(25<i>R</i>)-Spirost-4-en-3,6-dione
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4768(3)
_cell_length_b                   16.2190(9)
_cell_length_c                   19.4101(10)
_cell_measurement_reflns_used    25730
_cell_measurement_temperature    295.0(10)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.30
_cell_volume                     2353.8(2)
_computing_cell_refinement
;
X-AREA  (Stoe & Cie, 2018)
;
_computing_data_collection
;
X-AREA  (Stoe & Cie, 2018)
;
_computing_data_reduction
;
X-AREA  (Stoe & Cie, 2018)
;
_computing_molecular_graphics
;
XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      295.0(10)
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47703
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         20.998
_diffrn_reflns_theta_min         2.303
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_current           0.600
_diffrn_source_power             0.039
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2018)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.206
_refine_ls_extinction_coef       0.0162(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                3345
_reflns_number_total             5150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq4041sup1.cif
_cod_data_source_block           I
_cod_database_code               1559020
_cod_database_fobs_code          1559020
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              46452
_shelx_res_checksum              56491