(25<i>R</i>)-16β-Acetoxy-3β-bromo-23',26-epoxy-23',25-dimethyl-5α-cholest-23,23'-en-6-one dichloromethane monosolvate
Rincón, Susana; Yépez, Rebeca; Ochoa, M. Eugenia; López, Yliana; Santillan, Rosa; Farfán, Norberto; Acta Crystallographica Section E 68 (2012) o3260–o3261; doi:10.1107/S1600536812043590

data_2237030
_publ_section_title
;
 (25<i>R</i>)-16\b-Acetoxy-3\b-bromo-23',26-epoxy-23',25-dimethyl-5\a-cholest-23,23'-en-6-one
 dichloromethane monosolvate
;
_journal_coeditor_code           SU2514
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3260
_journal_page_last               o3261
_journal_paper_doi               10.1107/S1600536812043590
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C31 H45 Br O5, C H2 Cl2'
_chemical_formula_moiety         'C31 H45 Br O5, C H2 Cl2'
_chemical_formula_sum            'C32 H47 Br Cl2 O5'
_chemical_formula_weight         662.51
_chemical_melting_point          468(2)
_chemical_name_systematic
'(25<i>R</i>)-16\b-Acetoxy-3\b-bromo-23',26-epoxy-23',25-dimethyl-5\a-cholest-23,23'-en-6-one dichloromethane monosolvate'
_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            4
_cell_length_a                   7.44230(10)
_cell_length_b                   15.6578(2)
_cell_length_c                   26.8496(3)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      3.46
_cell_volume                     3128.79(7)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \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  0.0883
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            37310
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.523
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.677
_refine_ls_abs_structure_details 'Flack (1983), 3453 Friedel pairs'
_refine_ls_abs_structure_Flack   0.031(13)
_refine_ls_extinction_coef       0.0038(10)
_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   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0870P)^2^+3.6522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                5668
_reflns_number_total             7934
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2514.cif
_cod_data_source_block           I
_cod_database_code               2237030
_cod_database_fobs_code          2237030