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_2106005
_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, C4 H10 O2'
_chemical_formula_sum            'C38 H60 O9'
_chemical_formula_weight         660.86
_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 dimethoxyethan solvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2834(2)
_cell_length_b                   11.6425(3)
_cell_length_c                   41.9069(15)
_cell_measurement_reflns_used    6575
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      75.5015
_cell_measurement_theta_min      2.1068
_cell_volume                     3553.58(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.965
_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  0.0467
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            14172
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         75.686
_diffrn_reflns_theta_min         2.109
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45217
_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    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.291
_refine_ls_abs_structure_details
;
 Flack x determined using 1686 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0486P)^2^+2.8826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                5265
_reflns_number_total             6397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bm5069sup1.cif
_cod_data_source_block           CBX_3
_cod_database_code               2106005
_cod_database_fobs_code          2106005
_shelx_hkl_checksum              45345
_shelx_res_checksum              86264
_shelxl_version_number           20.14