(25<i>R</i>)-3β-Bromo-5α-spirostan-6,23-dione
Angel Dago Morales; Santiago García-Granda; Martín Andrés Iglesias-Arteaga; Francisco Coll-Manchado; Acta Crystallographica Section C 55 (1999) IUC9900042–; doi:10.1107/S0108270199099436

data_2008501
_publ_section_title
;
 (25<i>R</i>)-3\b-Bromo-5\a-spirostan-6,23-dione
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900042
_journal_paper_doi               10.1107/S0108270199099436
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C27 H39 Br O4'
_chemical_formula_weight         507.49
_chemical_name_systematic
;
(25R)-3\b-Bromo-5\a-spirostan-6,23-dione
;
_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'
_audit_creation_method           SHELX-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.361(10)
_cell_length_b                   13.044(10)
_cell_length_c                   18.806(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     2542(3)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'REFLEX (local program)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  'PARST93 (Nardelli, 1983) and  SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w-2\q
_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  0.088
_diffrn_reflns_av_sigmaI/netI    0.3477
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5629
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        4.3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.647
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.456
_refine_ls_abs_structure_details
;
The absolute stereochemistry was known before X-ray analysis and the results
of the Friedel refinement are in complete accord with it. 2482 Friedel pairs
were used in the refinement (Flack, 1983).
;
_refine_ls_abs_structure_Flack   0.007(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment
;
All H-atom parameters were refined as riding atoms with isotropic common
displacement parameter
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.305
_refine_ls_R_factor_gt           0.041
_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^)+(0.0296P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.107
_reflns_number_gt                1407
_reflns_number_total             4969
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qb0083.cif
_cod_data_source_block           QB0083
_cod_database_code               2008501
_cod_database_fobs_code          2008501