Isolation, structural elucidation, and bioactivity of cholestane derivatives from Ypsilandra thibetica
Xie, Jing; Zhang, Shi-Juan; Yue, Grace Gar-Lee; Yu, Ling-Ling; Liu, Hui; Ma, Wen-Yi; Yan, Huan; Ni, Wei; Lau, Clara Bik-San; Liu, Hai-Yang; New Journal of Chemistry 47 (2023) 324–332; doi:10.1039/D2NJ04576A

data_7062076
_publ_section_title
;
 Isolation, structural elucidation, and bioactivity of cholestane
 derivatives from Ypsilandra thibetica
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              324
_journal_page_last               332
_journal_paper_doi               10.1039/D2NJ04576A
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_compound_source        'Ypsilandra thibetica Franch'
_chemical_formula_moiety         'C33 H52 O9, C H4 O, H2 O'
_chemical_formula_sum            'C34 H58 O11'
_chemical_formula_weight         642.80
_chemical_name_common            18-hydroxylypsilanogenin
_chemical_name_systematic
(23R,24S)-5\a-cholest-16\b,23-epoxy-23,24-(\b-D-fucopyranose-2,1-di-O-yl)-3\b,18-diol-6-one
_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'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2022-08-15 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0479(3)
_cell_length_b                   7.6358(2)
_cell_length_c                   17.9880(5)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      72.2936
_cell_measurement_theta_min      3.6825
_cell_volume                     1648.63(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.9'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON II'
_diffrn_radiation_monochromator  'Helixos MX multilayer Optic'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19289
_diffrn_reflns_theta_full        72.36
_diffrn_reflns_theta_max         72.36
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'Ius Diamond'
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             700
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform-Methanol'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.207
_refine_ls_abs_structure_details
;

Flack x determined using 2641 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6224
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0377P)^2^+0.3226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                6145
_reflns_number_total             6224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04576a2.cif
_cod_data_source_block           cxj18
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7062074--7062076.cif.
;
_cod_database_code               7062076
_shelx_res_checksum              22290