Novel glucocorticoid antedrugs possessing a C16,17-fused γ-lactone ring
Keith Biggadike; Sean M. Lynn; Panayiotis A. Procopiou; Rupert E. Shaw; Christopher Williamson; J. Chem. Soc., Perkin Trans. 1  (2000) 813–818; doi:10.1039/a908358h

data_7203935
_publ_section_title
;
 Novel glucocorticoid antedrugs possessing a C16,17-fused \g-lactone
 ring
;
_journal_issue                   5
_journal_name_full               'J. Chem. Soc., Perkin Trans. 1'
_journal_page_first              813
_journal_page_last               818
_journal_paper_doi               10.1039/a908358h
_journal_year                    2000
_chemical_formula_sum            'C25 H31 F O6'
_chemical_formula_weight         446.50
_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                 94.418(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1029(16)
_cell_length_b                   13.105(2)
_cell_length_c                   14.153(2)
_cell_measurement_reflns_used    59
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      18.35
_cell_volume                     1128.6(4)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device_type  'Stoe-Siemens diffractometer'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3304
_diffrn_reflns_theta_max         59.92
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(4)
_refine_ls_extinction_coef       0.0037(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_obs          0.0730
_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^)+(0.1068P)^2^+0.6411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1973
_refine_ls_wR_factor_obs         0.1707
_reflns_number_total             3171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908358h.txt
_cod_data_source_block           c2182_274_3
_cod_original_cell_volume        1128.5(4)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7203935
_reflns_number_obs               2320