16α-Bromo-17β-hydroxy-5α-androstan-3β-yl acetate
Shi, Rui; Zhang, Chun-Sheng; Wei, Kun; Acta Crystallographica Section E 66 (2010) o750–; doi:10.1107/S1600536810007555

data_2225549
_publ_section_title
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 16\a-Bromo-17\b-hydroxy-5\a-androstan-3\b-yl acetate
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_journal_coeditor_code           HB5324
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o750
_journal_paper_doi               10.1107/S1600536810007555
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C21 H33 Br O3'
_chemical_formula_moiety         'C21 H33 Br O3'
_chemical_formula_sum            'C21 H33 Br O3'
_chemical_formula_weight         413.38
_chemical_name_systematic
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16\a-Bromo-17\b-hydroxy-5\a-androstan-3\b-yl acetate
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_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 93.036(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1010(12)
_cell_length_b                   7.6637(8)
_cell_length_c                   24.383(3)
_cell_measurement_reflns_used    9114
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.213
_cell_volume                     2071.5(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.1563
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13607
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_T_max  0.7953
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.288
_refine_ls_abs_structure_details 'Flack (1983), 3537 Friedel pairs'
_refine_ls_abs_structure_Flack   0.016(9)
_refine_ls_extinction_coef       0.0010(4)
_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   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         9114
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.1701
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                3737
_reflns_number_total             9114
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5324.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
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_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2225549
_cod_database_fobs_code          2225549