3β,11α-Dihydroxy-17a-oxa-<small>D</small>-homoandrost-5-en-17-one
Świzdor, Alina; Białońska, Agata; Kołek, Teresa; Panek, Anna; Acta Crystallographica Section E 66 (2010) o2003–; doi:10.1107/S1600536810026516

data_2227118
_publ_section_title
;
 3\b,11\a-Dihydroxy-17a-oxa-<small>D</small>-homoandrost-5-en-17-one
;
_journal_coeditor_code           WN2398
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2003
_journal_paper_doi               10.1107/S1600536810026516
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C19 H28 O4'
_chemical_formula_moiety         'C19 H28 O4'
_chemical_formula_sum            'C19 H28 O4'
_chemical_formula_weight         320.41
_chemical_name_systematic
;
3\b,11\a-Dihydroxy-17a-oxa-D-homoandrost-5-en-17-one
;
_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                 102.66(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.915(3)
_cell_length_b                   9.854(2)
_cell_length_c                   14.246(3)
_cell_measurement_reflns_used    1957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      3.06
_cell_volume                     1632.0(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'XP (Bruker, 1999)'
_computing_publication_material  'SHELXTL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       '\w scan'
_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  0.1175
_diffrn_reflns_av_sigmaI/netI    0.1358
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8286
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         2921
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                2062
_reflns_number_total             2921
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wn2398.cif
_cod_data_source_block           I
_cod_original_cell_volume        1632.0(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2227118
_cod_database_fobs_code          2227118