3β,6β-Diacetoxy-5,9α-dihydroxy-5α-cholest-7-en-11-one acetic acid 0.04-solvate
Piccialli, Vincenzo; Oliviero, Giorgia; Borbone, Nicola; Centore, Roberto; Tuzi, Angela; Acta Crystallographica Section E 69 (2013) o879–o880; doi:10.1107/S1600536813012646

data_2237926
_publ_section_title
;
 3\b,6\b-Diacetoxy-5,9\a-dihydroxy-5\a-cholest-7-en-11-one acetic acid
 0.04-solvate
;
_journal_coeditor_code           KP2452
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o879
_journal_page_last               o880
_journal_paper_doi               10.1107/S1600536813012646
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C31 H48 O7, 0.04C2 H4 O2'
_chemical_formula_moiety         'C31 H48 O7, 0.04(C2 H4 O2)'
_chemical_formula_sum            'C31.09 H48.18 O7.09'
_chemical_formula_weight         535.45
_chemical_name_systematic
;
3\b,6\b-Diacetoxy-5,9\a-dihydroxy-5\a-cholest-7-en-11-one acetic acid
0.04-solvate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   10.242(2)
_cell_length_b                   28.556(5)
_cell_length_c                   30.214(6)
_cell_measurement_reflns_used    454
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.839
_cell_measurement_theta_min      4.899
_cell_volume                     8837(3)
_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) and SADABS (Bruker,
2001)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            82574
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.9632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3498
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         11048
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1850
_reflns_number_gt                6969
_reflns_number_total             11048
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2452.cif
_cod_data_source_block           I
_cod_database_code               2237926
_cod_database_fobs_code          2237926