Synthesis and crystal structures of a 3-acetylated (20<i>S</i>,24<i>S</i>)-ocotillol-type saponin and its C-24 epimer
Liu, Juan; Xu, Yang-Rong; An, Xing-Si; Hou, Gui-Ge; Meng, Qing-Guo; Acta Crystallographica Section C 73 (2017) 464–469; doi:10.1107/S2053229617006507

data_2020817
_publ_section_title
;
 Synthesis and crystal structures of a 3-acetylated
 (20<i>S</i>,24<i>S</i>)-ocotillol-type saponin and its C-24 epimer
;
_journal_coeditor_code           LF3050
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              464
_journal_page_last               469
_journal_paper_doi               10.1107/S2053229617006507
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C32 H54 O5'
_chemical_formula_moiety         'C32 H54 O5'
_chemical_formula_sum            'C32 H54 O5'
_chemical_formula_weight         518.75
_chemical_name_systematic
;
(20<i>S</i>,24<i>S</i>)-3-Acetyl-20,24-epoxydammarane-3,12,25-triol
;
_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   geom
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.910(2)
_cell_length_b                   8.0370(16)
_cell_length_c                   17.018(3)
_cell_measurement_reflns_used    2872
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      47.8430
_cell_measurement_theta_min      1.5620
_cell_volume                     1490.8(5)
_computing_cell_refinement
;
XSCANS (Bruker, 1997)
;
_computing_data_collection
;
XSCANS (Bruker, 1997)
;
_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      153
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31738
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         6.743
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS;Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.225
_refine_ls_abs_structure_details
;
Flack (1983), <b>???? Friedel pairs</b>
;
_refine_ls_abs_structure_Flack   0.19(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5480
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+0.7202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                4294
_reflns_number_total             5480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3050sup1.cif
_cod_data_source_block           IV
_cod_database_code               2020817
_cod_database_fobs_code          2020817
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.861
_shelx_hkl_file                  {9b1e1925-86b8-4406-b8a0-99bce375bfbd}
_shelx_hkl_checksum              97928
_shelx_res_file                  {a51e6b85-d4c5-4020-8897-cb10570a3bb2}
_shelx_res_checksum              26458