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_7234738
_publ_section_title
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 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         '2(C36 H62 O8), H2 O'
_chemical_formula_sum            'C72 H126 O17'
_chemical_formula_weight         1263.72
_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
_audit_creation_date             2019-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-27 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.1605(7)
_cell_length_b                   7.4488(3)
_cell_length_c                   26.1220(10)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    170
_cell_measurement_theta_max      66.79
_cell_measurement_theta_min      3.16
_cell_volume                     3504.9(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47095
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.960
_diffrn_reflns_theta_max         66.960
_diffrn_reflns_theta_min         4.910
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1294 before and 0.0796 after correction. The Ratio of minimum to maximum transmission is 0.5996. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 4906 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_coef       0.0032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12291
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0658P)^2^+1.0909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                11719
_reflns_number_total             12291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00965e2.cif
_cod_data_source_block           sc264_183_38_6_0m_a
_cod_database_code               7234738
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.878
_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.a Ternary CH refined with riding coordinates:
 C3A(H3A), C5A(H5A), C9A(H9A), C12A(H12A), C13A(H13A), C17A(H17A), C32A(H32A),
 C33A(H33A), C34A(H34A), C35A(H35A), C31A(H31A), C17(H17), C13(H13), C12(H12),
 C9(H9), C5(H5B), C3(H3), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C1A(H1AA,H1AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C11A(H11A,
 H11B), C16A(H16A,H16B), C15A(H15A,H15B), C23A(H23A,H23B), C22A(H22A,H22B),
 C36A(H36A,H36B), C23(H23C,H23D), C22(H22C,H22D), C16(H16C,H16D), C15(H15C,
 H15D), C11(H11C,H11D), C7(H7A,H7B), C6(H6B,H6C), C1(H1B,H1C), C2(H2B,H2C),
 C36(H36C,H36D)
2.c Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C24(H24)
2.d Idealised Me refined as rotating group:
 C29A(H29A,H29B,H29C), C28A(H28A,H28B,H28C), C30A(H30A,H30B,H30C), C19A(H19A,
 H19B,H19C), C18A(H18A,H18B,H18C), C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C),
 C21A(H21A,H21B,H21C), C27(H27D,H27E,H27F), C26(H26D,H26E,H26F), C21(H21D,H21E,
 H21F), C19(H19D,H19E,H19F), C18(H18D,H18E,H18F), C30(H30D,H30E,H30F), C29(H29D,
 H29E,H29F), C28(H28D,H28E,H28F)
2.e Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O2A(H2A), O6A(H6A), O8A(H8A), O4A(H4A), O5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'