17α-Ethynyl-17β-hydroxyandrosta-1,4-dien-3-one
Liu-Qing Sheng; Wan-Gen Liang; Gang Chen; Hua-Feng Shen; Acta Crystallographica Section E 63 (2007) o1182–o1183; doi:10.1107/S1600536807005223

data_2212521
_publ_section_title
;
 17\a-Ethynyl-17\b-hydroxyandrosta-1,4-dien-3-one
;
_journal_coeditor_code           CV2190
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1182
_journal_page_last               o1183
_journal_paper_doi               10.1107/S1600536807005223
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H26 O2'
_chemical_formula_moiety         'C21 H26 O2'
_chemical_formula_sum            'C21 H26 O2'
_chemical_formula_weight         310.42
_chemical_name_systematic
;
17\a-Ethynyl-17\b-hydroxyandrosta-1,4-diene-3-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                 107.777(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.480(3)
_cell_length_b                   20.758(8)
_cell_length_c                   6.697(3)
_cell_measurement_reflns_used    690
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.135
_cell_measurement_theta_min      3.301
_cell_volume                     857.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4306
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.413
_refine_ls_extinction_coef       0.097(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         1931
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0791P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                1684
_reflns_number_total             1931
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2190.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2212521
_cod_database_fobs_code          2212521