Rapid self-healing and anion selectivity in metallosupramolecular gels assisted by fluorine–fluorine interactions
Arnedo-Sánchez, Leticia; Nonappa, Nonappa; Bhowmik, Sandip; Hietala, Sami; Puttreddy, Rakesh; Lahtinen, Manu; De Cola, Luisa; Rissanen, Kari; Dalton Trans.  (2017) –; doi:10.1039/C7DT00983F

data_7043136
_publ_section_title
;
 Rapid self-healing and anion selectivity in metallosupramolecular gels
 assisted by fluorine--fluorine interactions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00983F
_journal_year                    2017
_chemical_formula_moiety         'C29 H15 F15 N4 O, C4 H8 O'
_chemical_formula_sum            'C33 H23 F15 N4 O2'
_chemical_formula_weight         792.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2n 2a'
_space_group_name_H-M_alt        'P 21 c n'
_symmetry_space_group_name_Hall  'P -2n 2a'
_symmetry_space_group_name_H-M   'P 21 c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-02-16 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7081(5)
_cell_length_b                   10.0000(7)
_cell_length_c                   56.029(4)
_cell_measurement_reflns_used    8131
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.2260
_cell_measurement_theta_min      4.4720
_cell_volume                     3198.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -116.00 -17.00   1.50   10.00    --  -41.65 -37.00 150.00   66
  2  \w   -114.00 -72.00   1.50   10.00    --  -41.65-143.00 -91.00   28
  3  \w   -117.00 -54.00   1.50   10.00    --  -41.65 -19.00-120.00   42
  4  \w    -50.00 -14.00   1.50   10.00    --  -41.65 -19.00-120.00   24
  5  \w    -92.00  46.00   1.50   10.00    --  -41.65   0.00 -60.00   92
  6  \w     23.00  86.00   1.50   10.00    --   41.65-125.00 -30.00   42
  7  \w      9.00 117.00   1.50   10.00    --   41.65  77.00 120.00   72
  8  \w     11.00  83.00   1.50   10.00    --   41.65  68.00 -43.54   48
  9  \w      2.00  81.50   1.50   10.00    --   41.65 -99.00 150.00   53
 10  \w      9.00  67.50   1.50   10.00    --   41.65  77.00  30.00   39
 11  \w      9.00  67.50   1.50   10.00    --   41.65  77.00-150.00   39
 12  \w     63.00 108.00   1.50   40.00    --  106.66 -94.00 -90.00   30
 13  \w     75.00 100.50   1.50   40.00    --  106.66  75.00-127.03   17
 14  \w     24.00 108.00   1.50   40.00    --  106.66 -94.00 150.00   56
 15  \w     34.00  61.00   1.50   40.00    --  106.66 -94.00 -90.00   18
 16  \w     80.00 140.00   1.50   40.00    --  106.66  61.00 -60.00   40
 17  \w    124.00 178.00   1.50   40.00    --  106.66  77.00 -34.80   36
 18  \w     75.00 102.00   1.50   40.00    --  106.66  72.00  -3.06   18
 19  \w     78.00 118.50   1.50   40.00    --  106.66  61.00 120.00   27
 20  \w     91.00 118.00   1.50   40.00    --  106.66-125.00  90.00   18
 21  \w     74.00 101.00   1.50   40.00    --  106.66  77.00-150.00   18
 22  \w     78.00 105.00   1.50   40.00    --  106.66  61.00  90.00   18
 23  \w     74.00 107.00   1.50   40.00    --  106.66  77.00-180.00   22
 24  \w     74.00  99.50   1.50   40.00    --  106.66  77.00  90.00   17
 25  \w    121.00 175.00   1.50   40.00    --  106.66  77.00  90.00   36
 26  \w     74.00 110.00   1.50   40.00    --  106.66  77.00   0.00   24
 27  \w    114.00 141.00   1.50   40.00    --  106.66  77.00   0.00   18
 28  \w     78.00 105.00   1.50   40.00    --  106.66  61.00-180.00   18
 29  \w     78.00 177.00   1.50   40.00    --  106.66  61.00 150.00   66
 30  \w     78.00 105.00   1.50   40.00    --  106.66  61.00-150.00   18
 31  \w     34.00  61.00   1.50   40.00    --  106.66-125.00  90.00   18
 32  \w     74.00 101.00   1.50   40.00    --  106.66  77.00 -34.80   18
 33  \w     74.00 129.50   1.50   40.00    --  106.66  77.00 -90.00   37
 34  \w     78.00 123.00   1.50   40.00    --  106.66  61.00  30.00   30
 35  \w     94.00 178.00   1.50   40.00    --  106.66 125.00   0.00   56
 36  \w     34.00 139.00   1.50   40.00    --  106.66 -77.00 -30.00   70
 37  \w     74.00 176.00   1.50   40.00    --  106.66  77.00  60.00   68
 38  \w     78.00 177.00   1.50   40.00    --  106.66  61.00-120.00   66
 39  \w     78.00 111.00   1.50   40.00    --  106.66  61.00  60.00   22
 40  \w     74.00 101.00   1.50   40.00    --  106.66  77.00 -60.00   18
 41  \w     74.00 101.00   1.50   40.00    --  106.66  77.00  30.00   18
 42  \w     78.00 105.00   1.50   40.00    --  106.66  61.00   0.00   18
 43  \w    110.00 176.00   1.50   40.00    --  106.66  61.00-150.00   44
 44  \w     74.00 143.00   1.50   40.00    --  106.66  77.00 120.00   46
 45  \w     76.00 101.50   1.50   40.00    --  106.66  70.00 154.78   17
 46  \w    152.00 177.50   1.50   40.00    --  106.66  61.00  90.00   17
 47  \w     76.00 101.50   1.50   40.00    --  106.66  68.00  62.35   17
 48  \w     77.00 102.50   1.50   40.00    --  106.66  66.00-102.16   17
 49  \w     75.00 112.50   1.50   40.00    --  106.66  74.00 -48.11   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1940384000
_diffrn_orient_matrix_UB_12      -0.0829171000
_diffrn_orient_matrix_UB_13      0.0120670000
_diffrn_orient_matrix_UB_21      0.1047273000
_diffrn_orient_matrix_UB_22      -0.0330875000
_diffrn_orient_matrix_UB_23      -0.0246461000
_diffrn_orient_matrix_UB_31      0.1556910000
_diffrn_orient_matrix_UB_32      0.1256274000
_diffrn_orient_matrix_UB_33      0.0015021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            44193
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.728
_diffrn_reflns_theta_max         66.728
_diffrn_reflns_theta_min         4.491
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81665
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 1656 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5656
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0726
_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^)+(0.0392P)^2^+7.8485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4925
_reflns_number_total             5656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00983f2.cif
_cod_data_source_block           3_THF
_cod_database_code               7043136
_chemical_oxdiff_formula         'C30 H30 N3 F15 O1'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C3(H3), C4(H4A), C7(H7), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21)
;
_shelx_res_checksum              81852
_shelx_shelxl_version_number     2014/7
_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 1.552
_oxdiff_exptl_absorpt_empirical_full_min 0.782