A derivative of diosgenin: (25<i>R</i>)-23-acetyl-3β-bromo-16β-acetoxy-22,26-epoxy-5α-cholest-22-en-6-one
Castro-Méndez, Albina; Sandoval-Ramírez, Jesús; Bernès, Sylvain; Acta Crystallographica Section E 58 (2002) o606–o608; doi:10.1107/S1600536802007754

data_2201065
_publ_section_title
;A derivative of diosgenin:
 (25<i>R</i>)-23-acetyl-3\b-bromo-16\b-acetoxy-22,26-epoxy-5\a-cholest-22-en-6-one
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o606
_journal_page_last               o608
_journal_paper_doi               10.1107/S1600536802007754
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C31 H45 Br O5'
_chemical_formula_moiety         'C31 H45 Br O5'
_chemical_formula_sum            'C31 H45 Br O5'
_chemical_formula_weight         577.58
_chemical_melting_point          491
_chemical_name_systematic
;
(25R)-23-acetyl-3-\b-bromo-16-\b-acetoxy-22,26-epoxy-5-\a-cholest-22-en-6-one
;
_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                   8.5963(11)
_cell_length_b                   12.4609(8)
_cell_length_c                   27.7642(15)
_cell_measurement_reflns_used    67
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      13.22
_cell_measurement_theta_min      4.67
_cell_volume                     2974.0(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'RASTEP-3D (Merritt & Bacon, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7094
_diffrn_reflns_theta_full        26.25
_diffrn_reflns_theta_max         26.25
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XSCANS; Fait, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.524
_refine_ls_abs_structure_details 'Flack (1983); 2511 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.008(12)
_refine_ls_extinction_coef       0.0014(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0489P)^2^+2.0696P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                3490
_reflns_number_total             5918
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6172.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_database_code               2201065
_cod_database_fobs_code          2201065