Crystal structure of (−)-β-D-19-glucopiranosyl-9,15-dihydroxy kaurenoate, C26H40O9
Wang, Lei; Li, Guang-Jie; Ye, Jiang-Hai; He, Kang; Zou, Juan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 197–199; doi:10.1515/ncrs-2022-0551

data_8107393
_publ_section_title
;
 Crystal structure of (&#x2212;)-\b-D-19-glucopiranosyl-9,15-dihydroxy
 kaurenoate, C26H40O9
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              197
_journal_page_last               199
_journal_paper_doi               10.1515/ncrs-2022-0551
_journal_volume                  238
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C26 H40 O9, 2(H2 O)'
_chemical_formula_sum            'C26 H44 O11'
_chemical_formula_weight         532.61
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6816(12)
_cell_length_b                   7.3911(3)
_cell_length_c                   15.6072(8)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      32.90
_cell_measurement_theta_min      2.99
_cell_volume                     2616.4(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX2 (Brucker, 2012)[1]'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)[4]'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)[4]'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)[3]'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)[2]'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29960
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.992
_diffrn_reflns_theta_min         2.994
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0563 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.9418.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 3154 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(17)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         9512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.1926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.796
_reflns_number_gt                8250
_reflns_number_total             9512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0551_suppl.cif
_cod_data_source_block           a
_cod_database_code               8107393
_olex2_refinement_description
;
1.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
1.b Ternary CH refined with riding coordinates:
 C5(H5A), C13(H13), C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
1.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,
 H11B), C12(H12A,H12B), C14(H14A,H14B), C26(H26A,H26B)
1.d X=CH2 refined with riding coordinates:
 C17(H17A,H17B)
1.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
1.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O5(H5), O6(H6), O7(H7), O9(H9)
;
_shelx_res_checksum              31057
_shelx_hkl_checksum              44876
_olex2_submission_special_instructions 'No special instructions were received'