3β-Acetoxy-5α-chloro-6β-hydroxyandrostan-17-one
Chun-Nian Xia; Bi-Wen Li; Wei-xiao Hu; Wei Zhou; Acta Crystallographica Section E 63 (2007) o3107–o3107; doi:10.1107/S1600536807026803

data_2214083
_publ_section_title
;
 3\b-Acetoxy-5\a-chloro-6\b-hydroxyandrostan-17-one
;
_journal_coeditor_code           BT2381
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3107
_journal_page_last               o3107
_journal_paper_doi               10.1107/S1600536807026803
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H31 Cl O4'
_chemical_formula_moiety         'C21 H31 Cl O4'
_chemical_formula_sum            'C21 H31 Cl O4'
_chemical_formula_weight         382.91
_chemical_name_systematic
;
3\b-Acetoxy-5\a-chloro-6\b-hydroxyandrostan-17-one
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                100.521(2)
_cell_angle_beta                 99.211(2)
_cell_angle_gamma                110.470(2)
_cell_formula_units_Z            2
_cell_length_a                   7.1025(12)
_cell_length_b                   9.9840(16)
_cell_length_c                   15.552(3)
_cell_measurement_reflns_used    2891
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.08
_cell_measurement_theta_min      2.42
_cell_volume                     985.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2005)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5701
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.9622
_exptl_absorpt_correction_T_min  0.9378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.137
_refine_diff_density_min         -0.167
_refine_ls_abs_structure_details 'Flack (1983), with 983 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0442P)^2^+0.1280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                4372
_reflns_number_total             4861
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2381.cif
_cod_data_source_block           I
_cod_database_code               2214083
_cod_database_fobs_code          2214083