(+)-3,11-Dioxo-5α-androstanecarboxylic acid: catemeric hydrogen bonding in a steroidal diketo acid
Kikolski, Elizabeth M.; Thompson, Hugh W.; Lalancette, Roger A.; Acta Crystallographica Section C 62 (2006) o397–o398; doi:10.1107/S0108270106017677

data_2015455
_publ_section_title
;
 (+)-3,11-Dioxo-5\a-androstanecarboxylic acid: catemeric hydrogen
 bonding in a steroidal diketo acid
;
_journal_coeditor_code           SK3023
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o397
_journal_page_last               o398
_journal_paper_doi               10.1107/S0108270106017677
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C20 H28 O4'
_chemical_formula_moiety         'C20 H28 O4'
_chemical_formula_sum            'C20 H28 O4'
_chemical_formula_weight         332.42
_chemical_melting_point          559
_chemical_name_systematic
;
 (+)-3,11-Dioxo-5\a-androstanecarboxylic acid
;
_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                   6.36840(10)
_cell_length_b                   11.61020(10)
_cell_length_c                   22.7430(2)
_cell_measurement_reflns_used    8793
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.95
_cell_measurement_theta_min      3.89
_cell_volume                     1681.58(3)
_computing_cell_refinement       'SMART WNT/2000'
_computing_data_collection       'SMART WNT/2000 (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker,2000)'
_computing_molecular_graphics    'SHELXTL (Bruker,2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_sigmaI/netI    0.026
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8793
_diffrn_reflns_theta_full        64.95
_diffrn_reflns_theta_max         64.95
_diffrn_reflns_theta_min         3.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.17
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.040
_refine_ls_R_factor_gt           0.035
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.4552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.082
_refine_ls_wR_factor_ref         0.085
_reflns_number_gt                2503
_reflns_number_total             2741
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3023.cif
_cod_data_source_block           I
_cod_database_code               2015455
_cod_database_fobs_code          2015455