Solid-state supramolecular architecture of carbenoxolone ‒ comparative studies with glycyrrhetinic and glycyrrhizic acids
Tykarska, Ewa; Gdaniec, Maria; Acta Crystallographica Section B 71 (2015) –; doi:10.1107/S2052520614026419

data_2106006
_publ_section_title
;
 Solid-state supramolecular architecture of carbenoxolone -- comparative
 studies with glycyrrhetinic and glycyrrhizic acids
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520614026419
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety
;
 C34 H50 O7, C34 H49 Na O7, 2.0(H2 O), 2.0(C4 H8 O)
;
_chemical_formula_sum            'C76 H119 Na O18'
_chemical_formula_weight         1343.69
_chemical_name_systematic
;
(2S,4aS,6aR,6aS,6bR,8aR,10S,12aS,14bR)-10-(3-carboxypropanoyloxy)-
2,4a,6a,6b,9,9,12a-heptamethyl-13-oxo-3,4,5,6,6a,7,8,8a,10,11,12,14b-
dodecahydro-1H-picene-2-carboxylic acid :  monosodium
(2S,4aS,6aR,6aS,6bR,8aR,10S,12aS,14bR)-10-(3-carboxylatopropanoyloxy)-
2,4a,6a,6b,9,9,12a-heptamethyl-13-oxo-3,4,5,6,6a,7,8,8a,10,11,12,14b-
dodecahydro-1H-picene-2-carboxylic acid water/butan-2-one solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 92.4760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.34970(10)
_cell_length_b                   11.80610(10)
_cell_length_c                   42.4208(4)
_cell_measurement_reflns_used    26715
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      76.2410
_cell_measurement_theta_min      3.1270
_cell_volume                     3677.47(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
 Mercury CSD 2.4 - new features for the visualization and investigation
 of crystal structures, C. F. Macrae, I. J. Bruno, J. A. Chisholm,
 P. R. Edgington, P. McCabe, E. Pidcock, L. Rodriguez-Monge, R. Taylor,
 J. van de Streek and P. A. Wood, J. Appl. Cryst., 41, 466-470, 2008.
;
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla et al.,2005)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 5.2679
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            34807
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         76.468
_diffrn_reflns_theta_min         3.128
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.565
_refine_ls_abs_structure_details
;
 Flack x determined using 4731 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         12866
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+2.3843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                12732
_reflns_number_total             12866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bm5069sup1.cif
_cod_data_source_block           CBX_4
_cod_database_code               2106006
_cod_database_fobs_code          2106006
_shelx_hkl_checksum              6415
_shelx_res_checksum              28313
_shelxl_version_number           20.14