Crystal Structure and Synthesis of 17α-Acetoxy-6,7-epoxypregn-4-ene-3,20-dione
SORIANO-GARCIA, Manuel; ZAMBRANO, Armando; CABEZA, Marisa; BRATOEFF, Eugene; X-ray Structure Analysis Online 25 (2009) 61–; doi:10.2116/xraystruct.25.61

data_1551801
_publ_section_title
;
 Crystal Structure and Synthesis of
 17\a-Acetoxy-6,7-epoxypregn-4-ene-3,20-dione
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              61
_journal_paper_doi               10.2116/xraystruct.25.61
_journal_volume                  25
_journal_year                    2009
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C23 H30 O5'
_chemical_formula_sum            'C23 H30 O5'
_chemical_formula_weight         386.47
_chemical_name_systematic
;
17\a-acetoxy-6,7-epoxypregn-4-ene-3,20-dione
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.031(1)
_cell_length_b                   12.143(2)
_cell_length_c                   24.150(3)
_cell_measurement_reflns_used    8046
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.38
_cell_volume                     2061.9(5)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL V 6.14 (Sheldrick, 2006)'
_computing_publication_material  'SHELXTL V 6.14 (Sheldrick, 2006)'
_computing_structure_refinement  'SHELXTL V 6.14 (Sheldrick, 2006)'
_computing_structure_solution    'SHELXTL V 6.14 (Sheldrick, 2006)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX AXS CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22840
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      1.243
_exptl_crystal_density_method    'by flotation'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.9(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                2756
_reflns_number_total             3787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            25_61_1.cif
_cod_data_source_block           119sgm08
_cod_original_cell_volume        2062.0(5)
_cod_database_code               1551801