6β-Chloro-5α-hydroxy-20-oxopregnan-3β-yl acetate
Pinto, Rui M. A.; Salvador, Jorge A. R.; Paixão, José A.; Matos Beja, Ana; Ramos Silva, Manuela; Acta Crystallographica Section E 64 (2008) o1420–; doi:10.1107/S1600536808019478

data_2219063
_publ_section_title
;
 6\b-Chloro-5\a-hydroxy-20-oxopregnan-3\b-yl acetate
;
_journal_coeditor_code           IM2073
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1420
_journal_paper_doi               10.1107/S1600536808019478
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C23 H35 Cl O4'
_chemical_formula_moiety         'C23 H35 Cl O4'
_chemical_formula_sum            'C23 H35 Cl O4'
_chemical_formula_weight         410.96
_chemical_melting_point          506
_chemical_name_systematic
;
6\b-Chloro-5\a-hydroxy-20-oxopregnan-3\b-yl acetate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.094(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6862(6)
_cell_length_b                   27.484(2)
_cell_length_c                   11.1863(9)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1215
_cell_measurement_theta_min      2.4403
_cell_volume                     2219.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97(Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97(Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            55742
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS;  Sheldrick, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.259
_refine_ls_abs_structure_details 'Flack (1983), 5188 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         10978
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0626P)^2^+0.2390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                7889
_reflns_number_total             10978
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2073.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2219063
_cod_database_fobs_code          2219063