3-Methoxy-16,16-dimethyl-5α-androstan-17-one
Wölfling, János; Schneider, Gyula; Noltemeyer, Mathias; Tietze, Lutz F.; Acta Crystallographica Section C 50 (1994) 964–965; doi:10.1107/S0108270193012557

data_2009784
_publ_section_title
;
 3-Methoxy-16,16-dimethyl-5\a-androstan-17-one
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              964
_journal_page_last               965
_journal_paper_doi               10.1107/S0108270193012557
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C22 H36 O2'
_chemical_formula_weight         332.51
_chemical_name_systematic        ' 3-methoxy-16,16-dimethyl-5\a-andrstan-17-one'
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5620(10)
_cell_length_b                   13.583(3)
_cell_length_c                   22.488(4)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2004.4(6)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1989)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1989)'
_computing_structure_refinement  'SHELXL92 (Sheldrick, 1992)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe AED-2 four-circle'
_diffrn_measurement_method       'Profile fitting collection method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71072
_diffrn_reflns_av_R_equivalents  0.0108
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            2055
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       needles
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.119
_refine_diff_density_min         -0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3.(3)
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_method
'F~c~^*^ = kF~c~[1 + 0.001\cF~c~^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   0.968
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         1768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      0.968
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_obs          0.0363
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^) + (0.0610P)^2^ + 0.5000P] where
P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1105
_refine_ls_wR_factor_obs         0.0960
_reflns_number_observed          1574
_reflns_number_total             1769
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ka1056.cif
_cod_data_source_block           tie13
_cod_database_code               2009784