20-Oxopregn-5-ene-3β,16α-diyl diacetate
Andrade, L. C. R.; Paixão, J. A.; de Almeida, M. J. M.; Cruz Silva, M. M.; Moreno, M. J. S. M; Sá e Melo, M. L.; Campos Neves, A. S.; Acta Crystallographica Section E 58 (2002) o898–o900; doi:10.1107/S1600536802012862

data_2201441
_publ_section_title
;
 20-Oxopregn-5-ene-3\b,16\a-diyl diacetate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o898
_journal_page_last               o900
_journal_paper_doi               10.1107/S1600536802012862
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C25 H36 O5'
_chemical_formula_moiety         'C25 H36 O5'
_chemical_formula_sum            'C25 H36 O5'
_chemical_formula_weight         416.54
_chemical_name_systematic
;
 20-Oxopregn-5-ene-3\b,16\a-diyl diacetate
;
_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                 99.18(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.892(2)
_cell_length_b                   9.375(3)
_cell_length_c                   17.119(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      10.20
_cell_volume                     2359.4(13)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius MACH3'
_diffrn_measurement_method       'profile data from \w-2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7913
_diffrn_reflns_theta_full        71.91
_diffrn_reflns_theta_max         71.91
_diffrn_reflns_theta_min         4.29
_diffrn_standards_decay_%        5.7
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.210
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         4918
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0752P)^2^+0.3449P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                4607
_reflns_number_total             4918
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6128.cif
_cod_data_source_block           I
_cod_original_cell_volume        2359.3(13)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2201441
_cod_database_fobs_code          2201441