6β-Hydroxy-5β-methyl-20-oxo-19-norpregn-9(10)-en-3β-yl acetate
Pinto, R. M. A.; Ramos Silva, M.; Matos Beja, A.; Salvador, J. A. R.; Paixão, J. A.; Acta Crystallographica Section C 65 (2009) o214–o216; doi:10.1107/S0108270109010233

data_2017119
_publ_section_title
;
 6\b-Hydroxy-5\b-methyl-20-oxo-19-norpregn-9(10)-en-3\b-yl acetate
;
_journal_coeditor_code           SK3302
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o214
_journal_page_last               o216
_journal_paper_doi               10.1107/S0108270109010233
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C23 H34 O4'
_chemical_formula_moiety         'C23 H34 O4'
_chemical_formula_sum            'C23 H34 O4'
_chemical_formula_weight         374.50
_chemical_melting_point          411
_chemical_name_systematic
;
6\b-Hydroxy-5\b-methyl-20-oxo-19-norpregn-9(10)-en-3\b-yl acetate
;
_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                   5.8903(2)
_cell_length_b                   9.6929(2)
_cell_length_c                   36.9988(8)
_cell_measurement_reflns_used    6566
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2890
_cell_measurement_theta_min      2.3722
_cell_volume                     2112.41(10)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_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 0.999
_diffrn_measurement_device_type  'Bruker 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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            59317
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat hexagonal prism'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0779P)^2^+0.1174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                2885
_reflns_number_total             3729
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3302.cif
_cod_data_source_block           I
_cod_database_code               2017119
_cod_database_fobs_code          2017119