(+)-3-Oxo-5α-cholan-24-oic acid: catemeric hydrogen bonding in a steroidal keto acid
Brunskill, Andrew P. J.; Lalancette, Roger A.; Thompson, Hugh W.; Acta Crystallographica Section C 55 (1999) 419–422; doi:10.1107/S0108270198012931

data_2008250
_publ_section_title
;
 (+)-3-Oxo-5\a-cholan-24-oic acid: catemeric hydrogen bonding in a
 steroidal keto acid
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              419
_journal_page_last               422
_journal_paper_doi               10.1107/S0108270198012931
_journal_volume                  55
_journal_year                    1999
_chemical_formula_analytical     'C24 H38 O3'
_chemical_formula_moiety         'C24 H38 O3'
_chemical_formula_structural     'C24 H38 O3'
_chemical_formula_sum            'C24 H38 O3'
_chemical_formula_weight         374.54
_chemical_melting_point          462
_chemical_name_common
;
(+)-3-Oxo-5\a-cholan-24-oic  Acid
;
_chemical_name_systematic
;
(+)-3-Oxo-5\a-cholan-24-oic  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           SHELXTL/PC
_cell_angle_alpha                90.00
_cell_angle_beta                 91.940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.458(2)
_cell_length_b                   7.619(2)
_cell_length_c                   13.280(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.79
_cell_measurement_theta_min      5.98
_cell_volume                     1057.5(4)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4695
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        -1.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   'Face-indexed numerical (Sheldrick, 1994)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      1.175(3)
_exptl_crystal_density_method    'flotation in cyclohexane/ CCl~4~'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.118
_refine_diff_density_min         -0.119
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   '1.0(16) using 1910 Friedel pairs'
_refine_ls_extinction_coef       'refined to 0.0'
_refine_ls_extinction_method     'SHELXTL/PC (Sheldrick, 1995)'
_refine_ls_goodness_of_fit_all   1.07
_refine_ls_goodness_of_fit_obs   1.10
_refine_ls_hydrogen_treatment    'For hydrogen treatment, see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4151
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.16
_refine_ls_restrained_S_obs      1.10
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_obs          0.046
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.045P)^2^+0.094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.122
_refine_ls_wR_factor_obs         0.101
_reflns_number_observed          3202
_reflns_number_total             4153
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1512.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '462K' was changed to '462' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '462K' was changed to '462' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.045P)^2^+0.094P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.045P)^2^+0.094P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2008250