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_2020815
_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, 0.5H2 O1'
_chemical_formula_moiety         'C32 H54 O5, 0.5(H2 O1)'
_chemical_formula_sum            'C32 H55 O5.5'
_chemical_formula_weight         527.76
_chemical_name_systematic
;
(20<i>S</i>,24<i>R</i>)-3-Acetyl-20,24-epoxydammarane-3\b,12\b,25-triol
hemihydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.524(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.0091(18)
_cell_length_b                   7.7205(3)
_cell_length_c                   29.9984(18)
_cell_measurement_reflns_used    4093
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.3270
_cell_measurement_theta_min      3.5570
_cell_volume                     6112.5(6)
_computing_cell_refinement
;
FRAMBO (Bruker, 2004)
;
_computing_data_collection
;
FRAMBO (Bruker, 2004)
;
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker FRAMBO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19762
_diffrn_reflns_theta_full        66.40
_diffrn_reflns_theta_max         66.40
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.8041
_exptl_absorpt_correction_T_min  0.7657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.400
_refine_ls_abs_structure_details
;
Flack (1983), <b>???? Friedel pairs</b>
;
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_coef       0.00059(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         8185
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+1.5622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                6202
_reflns_number_total             8185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lf3050sup1.cif
_cod_data_source_block           IIIa
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2020815
_cod_database_fobs_code          2020815