(+)-3-Oxo-23,24-dinor-5α-cholan-22-oic Acid: Hydrogen-Bonding Patterns in a Steroidal Keto Acid and its Monohydrate
Lalancette, Roger A.; Thompson, Hugh W.; Brunskill, Andrew P. J.; Acta Crystallographica Section C 54 (1998) 421–424; doi:10.1107/S0108270197016296

data_2007077
_publ_section_title
;
 (+)-3-Oxo-23,24-dinor-5\a-cholan-22-oic Acid: Hydrogen-Bonding
 Patterns in a Steroidal Keto Acid and its Monohydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              421
_journal_page_last               424
_journal_paper_doi               10.1107/S0108270197016296
_journal_volume                  54
_journal_year                    1998
_chemical_formula_analytical     'C22 H36 O4'
_chemical_formula_iupac          'C22 H34 O3, H2 O1'
_chemical_formula_moiety         'C22 H36 O4'
_chemical_formula_structural     'C22 H36 O4'
_chemical_formula_sum            'C22 H36 O4'
_chemical_formula_weight         364.51
_chemical_melting_point          526
_chemical_name_common
;
22,23-Bisnor-5\a-cholanic acid-3-one Monohydrate
;
_chemical_name_systematic
;
(+)-22,23-Bisnor-3-oxo-5\a-cholanic Acid Monohydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_audit_creation_method           SHELXTL/PC
_cell_angle_alpha                90.00
_cell_angle_beta                 101.26(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.696(3)
_cell_length_b                   6.168(2)
_cell_length_c                   26.784(7)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.74
_cell_measurement_theta_min      10.07
_cell_volume                     2057.1(10)
_computing_cell_refinement       XSCANS
_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, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\q 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  0.047
_diffrn_reflns_av_sigmaI/netI    0.057
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            7240
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0.4
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_meas      1.180(10)
_exptl_crystal_density_method    'flotation in hexane/CCl~4~'
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.146
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -1.0(10)
_refine_ls_goodness_of_fit_all   1.05
_refine_ls_goodness_of_fit_obs   1.09
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.20
_refine_ls_restrained_S_obs      1.09
_refine_ls_R_factor_all          0.062
_refine_ls_R_factor_obs          .044
_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^)+(0.0608P)^2^+0.0737P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.131
_refine_ls_wR_factor_obs         .106
_reflns_number_observed          2910
_reflns_number_total             3624
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            fg1381.cif
_cod_data_source_block           II
_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.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (3 times).

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 '526K' was changed to '526' - 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 '526K' was changed to '526' - the
value should be numeric and without a unit
designator.

'_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_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^)+(0.0608P)^2^+0.0737P] 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^)+(0.0608P)^2^+0.0737P] 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      'C 2'
_cod_database_code               2007077