3,17-Dioxo-4-oxaandrostane-5α-carbaldehyde
Andrade, L. C. R.; Paixão, J. A.; de Almeida, M. J.; Tavares da Silva, E. J.; Sá e Melo, M. L.; Campos Neves, A. S.; Acta Crystallographica Section C 55 (1999) 637–639; doi:10.1107/S0108270198015728

data_2008420
_publ_section_title
;
 3,17-Dioxo-4-oxaandrostane-5\a-carbaldehyde
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              637
_journal_page_last               639
_journal_paper_doi               10.1107/S0108270198015728
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C19 H26 O4'
_chemical_formula_sum            'C19 H26 O4'
_chemical_formula_weight         318.40
_chemical_name_systematic
;
 4-oxa-3,17-dioxoandrostane-5\a-carbaldehyde
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.05(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.893(4)
_cell_length_b                   18.222(8)
_cell_length_c                   6.981(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.63
_cell_measurement_theta_min      8.03
_cell_volume                     833.7(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'SDP-Plus (Frenz, 1985)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'profile data from \w-2\q 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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3648
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         4.99
_diffrn_standards_decay_%        3.6
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.166
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -3.2(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         1955
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0505P)^2^+0.1143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                1385
_reflns_number_total             1955
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1231.cif
_cod_data_source_block           and22
_cod_original_cell_volume        833.8(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2008420
_cod_database_fobs_code          2008420