Fluoride-triggered phase transition of metallogels for on-demand <i>in situ</i> containment of fluids.
Kim, Junghwan; Kim, Chungryeol; Lee, Dongwhan; Chemical communications (Cambridge, England) 60 (2024) 1762–1765; doi:10.1039/d3cc06023c

data_7132619
_publ_section_title
;
 Fluoride-triggered phase transition of metallogels for on-demand <i>in
 situ</i> containment of fluids.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1762
_journal_page_last               1765
_journal_paper_doi               10.1039/d3cc06023c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C52 H98 N4 O6 Si6'
_chemical_formula_sum            'C52 H98 N4 O6 Si6'
_chemical_formula_weight         1043.88
_chemical_name_systematic        4b
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-05-30 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.5290(10)
_cell_angle_beta                 98.8760(10)
_cell_angle_gamma                109.3500(10)
_cell_formula_units_Z            2
_cell_length_a                   11.96430(10)
_cell_length_b                   16.5858(2)
_cell_length_c                   17.56880(10)
_cell_measurement_reflns_used    35681
_cell_measurement_temperature    93
_cell_measurement_theta_max      79.2740
_cell_measurement_theta_min      3.6810
_cell_volume                     3243.16(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  89.00   0.50    1.80    --    0.00  57.00   0.00  232
  2  \w    -27.00  89.00   0.50    1.80    --    0.00  38.00 120.00  232
  3  \w    -69.00  46.00   0.50    1.80    --   20.00 -46.00 -83.57  230
  4  \w     -5.00 117.00   0.50    1.80    --   28.00  77.00 167.99  244
  5  \w     17.00 141.00   0.50    1.80    --   52.00  81.00 178.37  248
  6  \w     53.00 177.00   0.50    2.92    --   88.00  82.00  72.60  248
  7  \w     79.00 195.00   0.50    2.92    --  105.20  45.00-120.00  232
  8  \w     16.00 134.00   0.50    2.92    --  105.20 -61.00  30.00  236
  9  \w     16.00 141.00   0.50    2.92    --  105.20 -82.00  90.00  250
 10  \w     16.00 141.00   0.50    2.92    --  105.20 -82.00   0.00  250
 11  \w     79.00 195.00   0.50    2.92    --  105.20  45.00 -90.00  232
 12  \w     79.00 195.00   0.50    2.92    --  105.20  45.00-180.00  232
 13  \w     16.00 141.00   0.50    2.92    --  105.20 -82.00-150.00  250
 14  \w     16.00 141.00   0.50    2.92    --  105.20 -82.00 -90.00  250
 15  \w     96.00 195.00   0.50    2.92    --  105.20  45.00 150.00  198
 16  \w     92.00 118.00   0.50    2.92    --  105.20 -82.00 120.00   52
 17  \w     17.00  58.00   0.50    2.92    --  105.20 -45.00 -60.00   82
 18  \w     99.00 132.00   0.50    2.92    --  105.20 -45.00 -60.00   66
 19  \w     72.00 137.00   0.50    2.92    --  105.20 -82.00  60.00  130
 20  \w     19.00  91.00   0.50    2.92    --  105.20 -61.00 -60.00  144
 21  \w     17.00 119.00   0.50    2.92    --  105.20 -61.00-150.00  204
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0000084000
_diffrn_orient_matrix_UB_12      0.0148237000
_diffrn_orient_matrix_UB_13      -0.0864339000
_diffrn_orient_matrix_UB_21      -0.0738074000
_diffrn_orient_matrix_UB_22      -0.0952907000
_diffrn_orient_matrix_UB_23      -0.0204260000
_diffrn_orient_matrix_UB_31      -0.1170894000
_diffrn_orient_matrix_UB_32      0.0207907000
_diffrn_orient_matrix_UB_33      -0.0046659000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53203
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.663
_diffrn_reflns_theta_min         2.551
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.069
_exptl_crystal_description       needle
_exptl_crystal_F_000             1140
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         13663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0525P)^2^+1.6470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12737
_reflns_number_total             13663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06023c2.cif
_cod_data_source_block           tbs_hex
_cod_depositor_comments
'Adding full bibliography for 7132619--7132620.cif.'
_cod_database_code               7132619
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C6(H6), C2(H2), C41(H41), C23(H23), C51(H51), C13(H13), C8(H8)
2.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C49(H49A,H49B,H49C), C21(H21A,H21B,H21C), C59(H59A,H59B,
 H59C), C22(H22A,H22B,H22C), C60(H60A,H60B,H60C), C50(H50A,H50B,H50C), C48(H48A,
 H48B,H48C), C67(H67A,H67B,H67C), C58(H58A,H58B,H58C), C31(H31A,H31B,H31C),
 C68(H68A,H68B,H68C), C66(H66A,H66B,H66C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C), C56(H56A,H56B,H56C), C39(H39A,H39B,H39C), C32(H32A,H32B,H32C), C37(H37A,
 H37B,H37C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C64(H64A,H64B,H64C),
 C57(H57A,H57B,H57C), C30(H30A,H30B,H30C), C20(H20A,H20B,H20C), C18(H18A,H18B,
 H18C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C65(H65A,H65B,H65C), C19(H19A,
 H19B,H19C)
;
_shelx_res_checksum              6363
_shelx_hkl_checksum              69713
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.626
_oxdiff_exptl_absorpt_empirical_full_min 0.756