(+)-14bα-3-Oxoglycyrrhetinic acid: catemeric hydrogen bonding in a non-racemic triterpenoid diketo acid
Thompson, Hugh W.; Lalancette, Roger A.; Kikolski, Elizabeth M.; Acta Crystallographica Section E 62 (2006) o5482–o5484; doi:10.1107/S1600536806045788

data_2211500
_publ_section_title
;
 (+)-14b\a-3-Oxoglycyrrhetinic acid: catemeric hydrogen bonding in a
 non-racemic triterpenoid diketo acid
;
_journal_coeditor_code           LH2223
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o5482
_journal_page_last               o5484
_journal_paper_doi               10.1107/S1600536806045788
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C30 H44 O4'
_chemical_formula_moiety         'C30 H44 O4'
_chemical_formula_sum            'C30 H44 O4'
_chemical_formula_weight         468.65
_chemical_melting_point          598
_chemical_name_common            '(+)-14b\a-3-Oxoglycyrrhetinic acid'
_chemical_name_systematic
;
(+)-10,13-dioxo-2\a,4a\b,6a\a,6b\b,9,9,12a\b-heptamethyl-
1,2,3,4,4a,5,6,6a,6 b,7,8,8a\a,9,10,11,12,12a,12b\a,13,14b\a-
eicosahydropicene-2\b-carboxylic acid
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.085(2)
_cell_angle_beta                 96.287(2)
_cell_angle_gamma                114.225(2)
_cell_formula_units_Z            1
_cell_length_a                   6.6054(2)
_cell_length_b                   7.2228(2)
_cell_length_c                   14.5495(3)
_cell_measurement_reflns_used    8622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.71
_cell_measurement_theta_min      3.06
_cell_volume                     628.39(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART CCD APEX-II area-detector'
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8622
_diffrn_reflns_theta_full        67.71
_diffrn_reflns_theta_max         67.71
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details 'Flack (1983), 1651 Friedel pairs'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3702
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.3681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                3345
_reflns_number_total             3702
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2223.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_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 (2
times).

'_geom_angle_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 (2 times).

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

The following automatic conversions were performed:

'_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 (2
times).

'_geom_angle_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 (2 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2211500
_cod_database_fobs_code          2211500