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_7132620
_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         'C70 H134 N4 O6 Si6'
_chemical_formula_sum            'C70 H134 N4 O6 Si6'
_chemical_formula_weight         1296.34
_chemical_name_systematic        4c
_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                79.449(2)
_cell_angle_beta                 65.041(2)
_cell_angle_gamma                78.584(2)
_cell_formula_units_Z            2
_cell_length_a                   15.9929(3)
_cell_length_b                   16.1504(3)
_cell_length_c                   17.3188(4)
_cell_measurement_reflns_used    25405
_cell_measurement_temperature    93
_cell_measurement_theta_max      78.8360
_cell_measurement_theta_min      3.7700
_cell_volume                     3950.26(15)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_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    -88.00  25.00   0.50    5.38    --    0.00 -38.00  60.00  226
  2  \w     12.00  38.00   0.50    5.38    --    0.00  57.00 150.00   52
  3  \w     -4.00  89.00   0.50    5.38    --    0.00  57.00  60.00  186
  4  \w    -54.00   7.00   0.50    5.38    --    0.00 -57.00   0.00  122
  5  \w    -25.00  78.00   0.50    5.38    --    0.00  57.00  30.00  206
  6  \w      8.00  45.00   0.50    5.38    --    0.00  57.00-150.00   74
  7  \w     79.00 195.00   0.50   11.86    --  105.20  45.00  30.00  232
  8  \w    106.00 132.00   0.50   11.86    --  105.20 -82.00  90.00   52
  9  \w     74.00 130.00   0.50   11.86    --  105.20 -61.00-120.00  112
 10  \w     16.00  56.00   0.50   11.86    --  105.20 -61.00-120.00   80
 11  \w     16.00 130.00   0.50   11.86    --  105.20 -82.00-180.00  228
 12  \w     72.00 108.00   0.50   11.86    --  105.20 -82.00   0.00   72
 13  \w     18.00  50.00   0.50   11.86    --  105.20 -61.00 150.00   64
 14  \w     59.00  85.00   0.50   11.86    --  105.20 -61.00 150.00   52
 15  \w     80.00 175.00   0.50   11.86    --  105.20  45.00 120.00  190
 16  \w     96.00 123.00   0.50   11.86    --  105.20 -82.00 -60.00   54
 17  \w     18.00  61.00   0.50   11.86    --  105.20 -82.00 -60.00   86
 18  \w     16.00 116.00   0.50   11.86    --  105.20 -61.00  60.00  200
 19  \w     90.00 137.00   0.50   11.86    --  105.20 -82.00 120.00   94
 20  \w     46.00 141.00   0.50   11.86    --  105.20 -82.00 -90.00  190
 21  \w     20.00 141.00   0.50   11.86    --  105.20 -82.00  60.00  242
 22  \w     75.00 101.00   0.50   11.86    --  105.20 -61.00-180.00   52
 23  \w     99.00 193.00   0.50   11.86    --  105.20  45.00   0.00  188
 24  \w    114.00 191.00   0.50   11.86    --  105.20  45.00  90.00  154
;
_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      0.0102772000
_diffrn_orient_matrix_UB_12      -0.0287214000
_diffrn_orient_matrix_UB_13      -0.0839926000
_diffrn_orient_matrix_UB_21      0.0420122000
_diffrn_orient_matrix_UB_22      0.0813652000
_diffrn_orient_matrix_UB_23      -0.0502892000
_diffrn_orient_matrix_UB_31      0.0981289000
_diffrn_orient_matrix_UB_32      -0.0463157000
_diffrn_orient_matrix_UB_33      -0.0128643000
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47578
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.579
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87776
_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_density_diffrn    1.090
_exptl_crystal_description       needle
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         16502
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0593P)^2^+2.0057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14478
_reflns_number_total             16502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06023c2.cif
_cod_data_source_block           tips_hex
_cod_depositor_comments
'Adding full bibliography for 7132619--7132620.cif.'
_cod_original_cell_volume        3950.27(15)
_cod_database_code               7132620
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.819
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 Si1-O10
 1.684 with sigma of 0.001
3.a Ternary CH refined with riding coordinates:
 C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C018(H018), C01A(H01J), C01C(H01N),
 C01M(H4), C01R(H9), C01T(H11), C01X(H15), C020(H020), C023(H023)
3.b Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00P(H00P), C00R(H00R), C00T(H00T), C00U(H00U),
 C00Y(H00Y), C010(H010)
3.c Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C), C017(H01D,H01E,H01F), C019(H01G,H01H,H01I), C01B(H01K,
 H01L,H01M), C01D(H01O,H01P,H01Q), C01E(H01R,H01S,H01T), C01F(H01U,H01V,H01W),
 C01G(H01X,H01Y,H), C01H(H01Z,HA,HB), C01I(H01,HC,HD), C01J(H1,HE,HF), C01K(H2,
 HG,HH), C01L(H3,HI,HJ), C01N(H5,HK,HL), C01O(H6,HM,HN), C01P(H7,HO,HP),
 C01Q(H8,HQ,HR), C01S(H10,HS,HT), C01U(H12,HU,HV), C01V(H13,HW,HX), C01W(H14,HY,
 HZ), C01Y(H16,H20,H21), C01Z(H17,H22,H23), C021(H02A,H02B,H02C), C022(H02D,
 H02E,H02F), C024(H02G,H02H,H02I), C025(H02J,H02K,H02L), C026(H02M,H02N,H02O),
 C027(H02P,H02Q,H02R), C028(H02S,H02T,H02U), C029(H02V,H02W,H02X), C02A(H02Y,
 H24,H25), C02B(H02Z,H26,H27), C02C(H02,H28,H29), C02D(H18,H30,H31), C02E(H19,
 H32,H33)
;
_shelx_res_checksum              6980
_shelx_hkl_checksum              33869
_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 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.833