9α-Fluoro-16α-methyl-3,17-dioxoandrosta-1,4-dien-11β-yl 2-Butynoate
Brock, C. P.; Song, J.; Acta Crystallographica Section C 51 (1995) 2437–2439; doi:10.1107/S0108270195006020

data_2004116
_publ_section_title
;
 9\a-Fluoro-16\a-methyl-3,17-dioxoandrosta-1,4-dien-11\b-yl 2-Butynoate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2437
_journal_page_last               2439
_journal_paper_doi               10.1107/S0108270195006020
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C24 H27 F O4'
_chemical_formula_sum            'C24 H27 F O4'
_chemical_formula_weight         398.47
_chemical_melting_point          .226E-224
_chemical_name_systematic
;
9\a-fluoro-11\b-hydroxy-16\a-methylandrosta-1,4-diene-3,17-dione
2-butynoate
;
_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'
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   7.6922(5)
_cell_length_b                   14.1688(8)
_cell_length_c                   19.3663(11)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.9
_cell_measurement_theta_min      12.2
_cell_volume                     2110.7(2)
_computing_cell_refinement       'CAD-4--VAX Users Manual'
_computing_data_collection       'CAD-4--VAX Users Manual (Enraf-Nonius, 1988)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4--VAX'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5140
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        <0.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description
;
Needles (major faces are {011}, {012}, {110}, {101} and {010}).
;
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.156
_refine_ls_abs_structure_details
;
the absolute structure of the crystal was assigned on the basis of the
synthetic pathway
;
_refine_ls_abs_structure_Flack   -2.0(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.000
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment    'H atoms refined as riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_obs          0.0387
_refine_ls_shift/esd_max         0.005
_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^) + (0.0630P)^2^ + 0.0117P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1065
_refine_ls_wR_factor_obs         0.0897
_reflns_number_observed          1698
_reflns_number_total             2752
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cr1188.cif
_cod_data_source_block           jsi82
_cod_database_code               2004116