11β,17,21-Trihydroxy-6α-methyl-3,20-dioxopregna-1,4-dien-21-yl 3-carboxypropionate
An, Hui-Mei; Gong, Ning-Bo; Lu, Yang; Acta Crystallographica Section E 65 (2009) o987–; doi:10.1107/S1600536809011969

data_2221801
_publ_section_title
;
 11\b,17,21-Trihydroxy-6\a-methyl-3,20-dioxopregna-1,4-dien-21-yl
 3-carboxypropionate
;
_journal_coeditor_code           SJ2598
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o987
_journal_paper_doi               10.1107/S1600536809011969
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C26 H34 O8'
_chemical_formula_moiety         'C26 H34 O8'
_chemical_formula_sum            'C26 H34 O8'
_chemical_formula_weight         474.53
_chemical_name_systematic
;
11\b,17,21-Trihydroxy-6\a-methyl-3,20-dioxopregna-1,4-dien-21-yl
3-carboxypropionate
;
_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'
_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                   8.31250(10)
_cell_length_b                   10.17650(10)
_cell_length_c                   28.8472(3)
_cell_measurement_reflns_used    8346
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      58.80
_cell_measurement_theta_min      3.06
_cell_volume                     2440.25(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            8346
_diffrn_reflns_theta_full        58.80
_diffrn_reflns_theta_max         58.80
_diffrn_reflns_theta_min         3.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.129
_refine_ls_abs_structure_details 'Flack (1983), 1388 Friedel pairs'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.0070(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max_lt       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^)+(0.0538P)^2^+0.6209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                3365
_reflns_number_total             3397
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2598.cif
_cod_data_source_block           I
_cod_database_code               2221801
_cod_database_fobs_code          2221801