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_7234743
_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 rmad
_chemical_formula_moiety         '2(C36 H62 O8), 4(H2O)'
_chemical_formula_sum            'C72 H132 O20'
_chemical_formula_weight         1317.80
_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   geom
_audit_creation_date             2019-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-18 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.98
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.99620(10)
_cell_length_b                   11.95430(10)
_cell_length_c                   20.1400(2)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      67.11
_cell_measurement_theta_min      2.243
_cell_volume                     3767.36(5)
_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)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.964
_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  0.0200
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25800
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.781
_diffrn_reflns_theta_min         3.222
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0675 before and 0.0367 after correction. The Ratio of minimum to maximum transmission is 0.8813. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 5078 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         12553
_refine_ls_number_restraints     789
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0880P)^2^+0.4905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                11898
_reflns_number_total             12553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00965e2.cif
_cod_data_source_block           s280_0m
_cod_original_cell_volume        3767.41(5)
_cod_database_code               7234743
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.868
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O12(0.5) O11(0.5) O10(0.5) O1AA(0.5) O0AA(0.5)
4.a Ternary CH refined with riding coordinates:
 C9A(H9A), C5A(H5AA), C13A(H13A), C17A(H17A), C35A(H35A), C32A(H32A),
 C31A(H31A), C34A(H34A), C33A(H33A), C12A(H12A), C3A(H3A), C5(H5), C9(H9),
 C3(H3), C31(H31), C32(H32), C13(H13), C17(H17), C12(H12), C35(H35), C34(H34),
 C33(H33)
4.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C11A(H11A,H11B), C36A(H36A,H36B), C22A(H22A,H22B), C15A(H15A,
 H15B), C1A(H1AA,H1AB), C7A(H7AA,H7AB), C6A(H6AA,H6AB), C23A(H23A,H23B),
 C16A(H16A,H16B), C2(H2B,H2C), C1(H1B,H1C), C6(H6B,H6C), C11(H11C,H11D), C7(H7A,
 H7B), C22(H22C,H22D), C16(H16C,H16D), C23(H23C,H23D), C36(H36C,H36D), C15(H15C,
 H15D)
4.c Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C24(H24)
4.d Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C), C30A(H30A,H30B,H30C), C28A(H28A,
 H28B,H28C), C29A(H29A,H29B,H29C), C21A(H21A,H21B,H21C), C27A(H27A,H27B,H27C),
 C28(H28D,H28E,H28F), C21(H21D,H21E,H21F), C18(H18D,H18E,H18F), C19(H19D,H19E,
 H19F), C30(H30D,H30E,H30F), C29(H29D,H29E,H29F), C27(H27D,H27E,H27F),
 C26A(H26A,H26B,H26C), C26(H26D,H26E,H26F)
4.e Idealised tetrahedral OH refined as rotating group:
 O2A(H2A), O8A(H8A), O5A(H5A), O1A(H1A), O6A(H6A), O4A(H4A), O6(H6), O1(H1),
 O2(H2), O4(H4), O5(H5B), O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'