11β,17aα-Dihydroxy-17aβ-methyl-<small>D</small>-homoandrosta-1,4-diene-3,17-dione monohydrate
Qiu, Ya; Chen, Ying; Xia, Peng; Acta Crystallographica Section E 65 (2009) o935–; doi:10.1107/S1600536809010770

data_2221353
_publ_section_title
;11\b,17a\a-Dihydroxy-17a\b-methyl-<small>D</small>-homoandrosta-1,4-diene-3,17-dione
 monohydrate
;
_journal_coeditor_code           GK2193
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o935
_journal_paper_doi               10.1107/S1600536809010770
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C21 H28 O4, H2 O'
_chemical_formula_moiety         'C21 H28 O4, H2 O'
_chemical_formula_sum            'C21 H30 O5'
_chemical_formula_weight         362.45
_chemical_name_systematic
;
11\b,17a\a-Dihydroxy-17a\b-methyl-D-homoandrosta-1,4-diene-3,17-dione
monohydrate
;
_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                 103.797(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.641(2)
_cell_length_b                   18.642(6)
_cell_length_c                   8.017(3)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.054
_cell_measurement_theta_min      2.836
_cell_volume                     963.9(6)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4866
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_correction_T_min  0.9784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0626P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                1778
_reflns_number_total             2182
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2193.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2221353
_cod_database_fobs_code          2221353