Probing the Relationship between Crystallization and Gelation by Using Ammonium Salts of Bile Acids
Li, Puzhen; Zhang, Meng; Maris, Thierry; Zhu, X. X.; Wuest, James D.; Crystal Growth & Design 22 (2022) 3505–3517; doi:10.1021/acs.cgd.2c00310

data_4519427
_publ_contact_author_id_orcid    0000-0001-9731-4046
_publ_section_title
;
 Probing the Relationship between Crystallization and Gelation by Using
 Ammonium Salts of Bile Acids
;
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3505
_journal_page_last               3517
_journal_paper_doi               10.1021/acs.cgd.2c00310
_journal_volume                  22
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H39 O5, 3.5(H2 O), C10 H18 N'
_chemical_formula_sum            'C34 H64 N O8.5'
_chemical_formula_weight         622.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_contact_author_email      thierry.maris@umontreal.ca
_audit_contact_author_name       'Thierry Maris'
_audit_contact_author_phone      '+1 514 340 4711 2579'
_audit_creation_date             2021-09-10
_audit_creation_method
;
FinalCif V88 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_cell_angle_alpha                90
_cell_angle_beta                 113.990(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.0367(16)
_cell_length_b                   7.5296(4)
_cell_length_c                   17.7558(10)
_cell_measurement_reflns_used    2542
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.148
_cell_measurement_theta_min      2.724
_cell_volume                     3424.5(3)
_computing_cell_refinement
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEX2 CCD'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Quazar MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22267
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.933
_diffrn_reflns_theta_min         2.724
_diffrn_source                   'Microfocus Source'
_diffrn_source_current           0.65
_diffrn_source_power             0.02912
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mS High Brilliance Microsource'
_diffrn_source_voltage           44.8
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.5863
_exptl_absorpt_correction_T_min  0.4705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1781 before and 0.0855 after correction.
The Ratio of minimum to maximum transmission is 0.8025.
The \l/2 correction factor is Not present.
;
_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    1.208
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         5990
_refine_ls_number_restraints     583
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0671P)^2^+3.1277P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.655
_reflns_Friedel_fraction_full    0.785
_reflns_Friedel_fraction_max     0.765
_reflns_number_gt                5305
_reflns_number_total             5990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CA_1-AdamantylNH3_3_5H2O.cif
_cod_data_source_block           zhu31
_cod_original_formula_sum        'C34 H64 N O8.50'
_cod_database_code               4519427
_cod_database_fobs_code 4519427