3β,6α-Diacetoxy-5,9α-dihydroxy-5α-cholest-7-en-11-one
Piccialli, Vincenzo; Tuzi, Angela; Oliviero, Giorgia; Borbone, Nicola; Centore, Roberto; Acta Crystallographica Section E 69 (2013) o1109–o1110; doi:10.1107/S1600536813016206

data_2238154
_publ_section_title
;
 3\b,6\a-Diacetoxy-5,9\a-dihydroxy-5\a-cholest-7-en-11-one
;
_journal_coeditor_code           FJ2632
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1109
_journal_page_last               o1110
_journal_paper_doi               10.1107/S1600536813016206
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C31 H48 O7'
_chemical_formula_moiety         'C31 H48 O7'
_chemical_formula_sum            'C31 H48 O7'
_chemical_formula_weight         532.69
_chemical_name_systematic
;
3\b,6\a-Diacetoxy-5,9\a-dihydroxy-5\a-cholest-7-en-11-one
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.964(2)
_cell_length_b                   9.1550(10)
_cell_length_c                   14.740(2)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.374
_cell_measurement_theta_min      3.718
_cell_volume                     1477.5(4)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>, 2000)'
_computing_data_collection       '<i>COLLECT</i> (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method
;
CCD rotation images, thick slices
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9976
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9959
_exptl_absorpt_correction_T_min  0.9518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         3498
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.6674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                2502
_reflns_number_total             3498
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2632.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2238154
_cod_database_fobs_code          2238154