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_7234741
_publ_section_title
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 Crystal Structure and Physical Stability of Ginsenoside Compound-K
 Solvates
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE00965E
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H62 O8, 2(C H4 O), H2 O'
_chemical_formula_sum            'C38 H71 O11'
_chemical_formula_weight         703.94
_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             2019-08-12
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-08-12 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 96.646(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4907(6)
_cell_length_b                   12.3599(6)
_cell_length_c                   14.0787(8)
_cell_measurement_reflns_used    9132
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      66.59
_cell_measurement_theta_min      3.58
_cell_volume                     1986.08(18)
_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      170.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            28599
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.916
_diffrn_reflns_theta_max         66.916
_diffrn_reflns_theta_min         3.873
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1202 before and 0.0784 after correction.
The Ratio of minimum to maximum transmission is 0.7807.
The \l/2 correction factor is Not present.
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_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details
;
 Flack x determined using 2777 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(9)
_refine_ls_extinction_coef       0.0123(5)
_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   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7011
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0264P)^2^+0.3523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                6560
_reflns_number_total             7011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00965e2.cif
_cod_data_source_block           sc208_183_25_4_0m_a
_cod_database_code               7234741
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
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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, All O(H,H) groups
2. Restrained distances
 O10-C38 \\sim O10-C38A
 with sigma of 0.02
 C25-C26 \\sim C25-C26A \\sim C25-C27 \\sim C25-C27A
 with sigma of 0.02
 C24-C26 \\sim C24-C26A \\sim C24-C27 \\sim C24-C27A
 with sigma of 0.02
3. Rigid bond restraints
 C26, C27, C38, C26A, C27A, C38A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C38 \\sim C26A \\sim C27A \\sim C38A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(H10A)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(H10)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5A), C9(H9), C12(H12), C13(H13), C17(H17), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C15(H15A,
 H15B), C16(H16A,H16B), C22(H22A,H22B), C23(H23A,H23B), C36(H36A,H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C24(H24)
6.d Tetrahedral OH refined with riding coordinates:
 O10(H10), O10(H10A)
6.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C38(H38A,H38B,H38C), C26A(H26D,H26E,
 H26F), C27A(H27D,H27E,H27F), C38A(H38D,H38E,H38F), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C)
6.f Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O8(H8), O9(H9A)
6.g Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O1(H1), O2(H2), O4(H4)
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_olex2_submission_special_instructions 'No special instructions were received'