3β,4β-Epoxy-7-oxo-7a-oxa-7a-homo-5β-cholan-24-oic acid
Angel Dago Morales; Santiago García-Granda; Roxana Pérez Gil; Francisco Coll-Manchado; Acta Crystallographica Section C 55 (1999) IUC9900043–; doi:10.1107/S0108270199099448

data_2008500
_publ_section_title
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 3\b,4\b-Epoxy-7-oxo-7a-oxa-7a-homo-5\b-cholan-24-oic acid
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900043
_journal_paper_doi               10.1107/S0108270199099448
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C24 H36 O5'
_chemical_formula_weight         404.53
_chemical_name_systematic
;
3\b,4\b-epoxy-7-oxo-7a-oxa-5\b-cholanoic acid
;
_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           SHELX-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.48(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.318(4)
_cell_length_b                   15.69(4)
_cell_length_c                   11.161(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      10
_cell_volume                     1076(3)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1994)'
_computing_data_reduction        'REFLEX (local program)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  'PARST93 (Nardelli, 1983) and SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w-2\q
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4138
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        2.7
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.244
_refine_ls_abs_structure_details
'Absolute structure could not be determined reliably Flack (1983)'
_refine_ls_abs_structure_Flack   0.0(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment
;
All H-atom parameters were refined as riding atoms with common isotropic
displacement parameter
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.107
_refine_ls_R_factor_gt           0.053
_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^)+(0.0841P)^2^+0.1625P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.155
_reflns_number_gt                2390
_reflns_number_total             3783
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qb0082.cif
_cod_data_source_block           QB0082
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2008500