Synthesis and crystal structures of C24-epimeric 20(<i>R</i>)-ocotillol-type saponins
Xu, Yang-Rong; Yang, Jing-Jing; Liu, Juan; Hou, Gui-Ge; Meng, Qing-Guo; Acta Crystallographica Section C 72 (2016) –; doi:10.1107/S2053229616007270

data_2020516
_publ_section_title
;
 Synthesis and crystal structures of C24-epimeric
 20(<i>R</i>)-ocotillol-type saponins
;
_journal_coeditor_code           LF3031
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229616007270
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C30 H52 O4, H2 O1'
_chemical_formula_moiety         'C30 H52 O4, H2 O1'
_chemical_formula_sum            'C30 H54 O5'
_chemical_formula_weight         494.73
_chemical_name_systematic
;
(20<i>R</i>,24<i>R</i>)-20,24-Epoxydammarane-3\b,12\b,25-triol
monohydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 102.700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8503(6)
_cell_length_b                   29.1839(18)
_cell_length_c                   14.8014(9)
_cell_measurement_reflns_used    2016
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2886.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9666
_diffrn_reflns_theta_full        66.193
_diffrn_reflns_theta_max         66.193
_diffrn_reflns_theta_min         3.028
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.8203
_exptl_absorpt_correction_T_min  0.7774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.293
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 581 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.7(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0925
_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^)+(0.1333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2772
_reflns_number_gt                3528
_reflns_number_total             6932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3031sup1.cif
_cod_data_source_block           IV
_cod_database_code               2020516
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.820