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_7234744
_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, C2 H6 O'
_chemical_formula_sum            'C38 H68 O9'
_chemical_formula_weight         668.92
_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             2019-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-16 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.607(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2329(19)
_cell_length_b                   11.8682(12)
_cell_length_c                   20.210(3)
_cell_measurement_reflns_used    8326
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      2.80
_cell_volume                     3784.3(8)
_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 0.994
_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  0.0720
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59016
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.149
_diffrn_reflns_theta_max         67.149
_diffrn_reflns_theta_min         3.153
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1220 before and 0.0937 after correction. The Ratio of minimum to maximum transmission is 0.8773. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 4501 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         13402
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0634P)^2^+0.4190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                11476
_reflns_number_total             13402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00965e2.cif
_cod_data_source_block           sc173_183_15_5_0m_a
_cod_original_cell_volume        3784.2(8)
_cod_database_code               7234744
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O10-C39 \\sim O0AA-C39
 with sigma of 0.02
3. Rigid bond restraints
 O0AA, O10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O0AA \\sim O10: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O10) \\sim Ueq, Uanis(C26A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: C26A(0.5) H26A(0.5) H26B(0.5) H26C(0.5) O10(0.65) H10(0.65)
 H39A(0.65) H39B(0.65) H39C(0.35) H39D(0.35) C0AA(0.5) H0AA(0.5) H0AB(0.5)
 H0AC(0.5) O0AA(0.35) H0AD(0.35)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C31A(H31A), C13(H13), C35(H35), C9A(H9A), C9(H9), C17(H17),
 C12(H12), C13A(H13A), C32(H32), C17A(H17A), C5(H5B), C5A(H5AA), C35A(H35A),
 C12A(H12A), C32A(H32A), C3A(H3A), C34(H34), C3(H3), C33(H33), C33A(H33A),
 C34A(H34A)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C22(H22C,H22D), C11A(H11A,H11B), C11(H11C,H11D), C7A(H7AA,
 H7AB), C36(H36C,H36D), C15A(H15A,H15B), C1(H1B,H1C), C2(H2B,H2C), C6A(H6AA,
 H6AB), C22A(H22A,H22B), C7(H7A,H7B), C1A(H1AA,H1AB), C15(H15C,H15D), C16A(H16A,
 H16B), C6(H6B,H6C), C16(H16C,H16D), C23A(H23A,H23B), C2A(H2AA,H2AB), C23(H23C,
 H23D), C36A(H36A,H36B), C39(H39A,H39B), C39(H39C,H39D)
6.c Me refined with riding coordinates:
 C38(H38A,H38B,H38C)
6.d Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C24(H24)
6.e Idealised Me refined as rotating group:
 C26A(H26A,H26B,H26C), C19(H19D,H19E,H19F), C28(H28D,H28E,H28F), C21(H21D,H21E,
 H21F), C18(H18D,H18E,H18F), C30(H30D,H30E,H30F), C28A(H28A,H28B,H28C),
 C18A(H18A,H18B,H18C), C30A(H30A,H30B,H30C), C19A(H19A,H19B,H19C), C29A(H29A,
 H29B,H29C), C29(H29D,H29E,H29F), C21A(H21A,H21B,H21C), C27(H27D,H27E,H27F),
 C40(H40A,H40B,H40C), C27A(H27A,H27B,H27C), C26(H26D,H26E,H26F), C0AA(H0AA,H0AB,
 H0AC)
6.f Idealised tetrahedral OH refined as rotating group:
 O5(H5), O4A(H4A), O5A(H5A), O10(H10), O9(H9B), O0AA(H0AD)
6.g Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O2(H2), O4(H4), O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'