(22<i>S</i>)-21-Acetoxy-11β-hydroxy-16α,17α-methylorthoacetoxypregna-1,4-diene-3,20-dione
Pniewska, B.; Anulewicz, R.; Uszycka-Horawa, T.; Acta Crystallographica Section C 52 (1996) 212–215; doi:10.1107/S0108270195009589

data_2004423
_publ_section_title
(22<i>S</i>)-21-Acetoxy-11\b-hydroxy-16\a,17\a-methylorthoacetoxypregna-1,4-diene-3,20-dione
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              212
_journal_page_last               215
_journal_paper_doi               10.1107/S0108270195009589
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C26 H34 O8'
_chemical_formula_weight         474.53
_chemical_name_systematic
;
 Methyl 21-acetoxy-11\b-hydroxy-1,4-pregnadiene-(22S)-16\a,17\a-orthoacetate
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 107.26(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.524(2)
_cell_length_b                   14.819(3)
_cell_length_c                   11.763(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      17
_cell_volume                     1252.5(5)
_computing_cell_refinement       'Kuma KM-4 Software'
_computing_data_collection       'Kuma KM-4 Software (Kuma, 1991)'
_computing_data_reduction        'Kuma KM-4 Software'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990b)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Kuma KM-4 computer-controlled four-circle'
_diffrn_measurement_method       \w/\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2529
_diffrn_reflns_theta_max         80.32
_diffrn_reflns_theta_min         3.94
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.203
_refine_ls_abs_structure_details 'Flack (1983) parameter = -0.14(26)'
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_coef       0.0094(15)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         2474
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_obs          0.0475
_refine_ls_shift/esd_max         0.022
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.1130P)^2^ + 0.0314P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1355
_refine_ls_wR_factor_obs         0.1320
_reflns_number_observed          2304
_reflns_number_total             2474
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1177.cif
_cod_data_source_block           pniewska
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2004423