Westphalen's diol diacetate: 19(10→ 5)-<i>abeo</i>-5β-cholest-9-ene-3β,6β-diyl diacetate
Ramírez Hernández, Johana; Sandoval-Ramírez, Jesús; Meza-Reyes, Socorro; Vega Báez, José Luis; Bernès, Sylvain; Acta Crystallographica Section E 68 (2012) o3331–; doi:10.1107/S1600536812045278

data_2236855
_publ_section_title
;
 Westphalen's diol diacetate: 19(10\\rightarrow
 5)-<i>abeo</i>-5\b-cholest-9-ene-3\b,6\b-diyl diacetate
;
_journal_coeditor_code           FF2087
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3331
_journal_paper_doi               10.1107/S1600536812045278
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C31 H50 O4'
_chemical_formula_moiety         'C31 H50 O4'
_chemical_formula_sum            'C31 H50 O4'
_chemical_formula_weight         486.71
_chemical_melting_point          393
_chemical_name_common
;
3\b,6\b-diacetoxy-5\b-methyl-19-norcholest-9(10)-ene
;
_chemical_name_systematic
;
19(10\\rightarrow 5)-<i>abeo</i>-5\b-cholest-9-ene-3\b,6\b-diyl diacetate
;
_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            4
_cell_length_a                   9.2846(15)
_cell_length_b                   10.7203(18)
_cell_length_c                   29.982(4)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      12.55
_cell_measurement_theta_min      4.43
_cell_volume                     2984.2(8)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            4350
_diffrn_reflns_theta_full        26.24
_diffrn_reflns_theta_max         26.24
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.131
_refine_ls_extinction_coef       0.0087(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     364
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.3625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                2827
_reflns_number_total             3393
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ff2087.cif
_cod_data_source_block           I
_cod_database_code               2236855
_cod_database_fobs_code          2236855