Crystal Structure and Physical Stability of Ginsenoside Compound-K Solvates
Chen, Jinyao; Zhu, Wenming; Ji, Weijie; Zhu, Bin; Guo, Chunyang; Qi, Ming-Hui; Ren, Guo-Bin; CrystEngComm  (2019) –; doi:10.1039/C9CE00965E

data_7234739
_publ_section_title
;
 Crystal Structure and Physical Stability of Ginsenoside Compound-K
 Solvates
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE00965E
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H62 O8, 2(C2 H6 O), H2 O'
_chemical_formula_sum            'C40 H76 O11'
_chemical_formula_weight         733.00
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-12 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.00
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.77470(10)
_cell_length_b                   12.45640(10)
_cell_length_c                   14.17900(10)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    170
_cell_measurement_theta_max      66.074
_cell_measurement_theta_min      3.791
_cell_volume                     2059.40(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11355
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        66.179
_diffrn_reflns_theta_max         66.179
_diffrn_reflns_theta_min         3.791
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0514 before and 0.0244 after correction. The Ratio of minimum to maximum transmission is 0.9082. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 2782 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         6506
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0615P)^2^+0.3475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.825
_reflns_Friedel_fraction_max     0.825
_reflns_number_gt                6470
_reflns_number_total             6506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00965e2.cif
_cod_data_source_block           s268_0m
_cod_original_cell_volume        2059.39(3)
_cod_database_code               7234739
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C39-C40 \\sim C38-C37
 with sigma of 0.02
3.a Free rotating group:
 O11(H11C)
3.b Ternary CH refined with riding coordinates:
 C31(H31), C35(H35), C32(H32), C3(H3), C5(H5A), C34(H34), C33(H33), C17(H17),
 C12(H12), C13(H13), C9(H9)
3.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C7(H7A,H7B), C2(H2A,H2B), C1(H1A,H1B), C6(H6A,H6B), C23(H23A,
 H23B), C22(H22A,H22B), C16(H16A,H16B), C15(H15A,H15B), C37(H37A,H37B)
3.d Aromatic/amide H refined with riding coordinates:
 C24(H24)
3.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C28(H28A,
 H28B,H28C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C)
3.f Idealised tetrahedral OH refined as rotating group:
 O6(H6), O2(H2), O4(H4), O5(H5), O1(H1), O8(H8), O9(H9A)
;
_olex2_submission_special_instructions 'No special instructions were received'