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_7043139
_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'
_chemical_formula_sum            'C29 H15 F15 N4 O'
_chemical_formula_weight         720.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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            8
_cell_length_a                   9.78405(18)
_cell_length_b                   10.07442(18)
_cell_length_c                   55.2622(12)
_cell_measurement_reflns_used    28130
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      74.0710
_cell_measurement_theta_min      4.6510
_cell_volume                     5447.12(18)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(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    -69.00  21.00   1.00    4.00    --  -41.90  57.00  60.00   90
  2  \w   -122.00  -1.00   1.00    4.00    --  -41.90 -19.00 -90.00  121
  3  \w   -101.00 -76.00   1.00    4.00    --  -41.90-149.00  98.00   25
  4  \w     14.00 118.00   1.00    4.00    --   41.90  77.00  30.00  104
  5  \w     69.00 116.00   1.00    4.00    --   41.90  37.00 120.00   47
  6  \w      9.00  94.00   1.00    4.00    --   41.90  77.00 -30.00   85
  7  \w     23.00  95.00   1.00    4.00    --   41.90-125.00-180.00   72
  8  \w     13.00  87.00   1.00    4.00    --   41.90  77.00-180.00   74
  9  \w     10.00  55.00   1.00    4.00    --   41.90  77.00  90.00   45
 10  \w      2.00  58.00   1.00    4.00    --   41.90 -99.00 -60.00   56
 11  \w     14.00  64.00   1.00    4.00    --   41.90  57.00 150.00   50
 12  \w     10.00 108.00   1.00    4.00    --   41.90  77.00-120.00   98
 13  \w     72.00 114.00   1.00    4.00    --   41.90  57.00 150.00   42
 14  \w     18.00  61.00   1.00    4.00    --   41.90  37.00 120.00   43
 15  \w     74.00 100.00   1.00   16.00    --  106.66  77.00 -60.00   26
 16  \w     25.00 102.00   1.00   16.00    --  106.66 -94.00 -60.00   77
 17  \w    107.00 177.00   1.00   16.00    --  106.66  71.00 -76.71   70
 18  \w     78.00 110.00   1.00   16.00    --  106.66  60.00-110.78   32
 19  \w     78.00 104.00   1.00   16.00    --  106.66  60.00-138.88   26
 20  \w     76.00 102.00   1.00   16.00    --  106.66  71.00 -76.71   26
 21  \w     78.00 108.00   1.00   16.00    --  106.66  60.00-116.45   30
 22  \w    109.00 178.00   1.00   16.00    --  106.66  77.00  30.00   69
 23  \w     78.00 104.00   1.00   16.00    --  106.66  61.00  90.00   26
 24  \w     78.00 139.00   1.00   16.00    --  106.66  61.00 -90.00   61
 25  \w     79.00 106.00   1.00   16.00    --  106.66  61.00 -30.00   27
 26  \w    107.00 149.00   1.00   16.00    --  106.66  61.00 -30.00   42
 27  \w     74.00 146.00   1.00   16.00    --  106.66  77.00 150.00   72
 28  \w     78.00 105.00   1.00   16.00    --  106.66  61.00  60.00   27
 29  \w     74.00  99.00   1.00   16.00    --  106.66  77.00  30.00   25
 30  \w     79.00 104.00   1.00   16.00    --  106.66  61.00-180.00   25
 31  \w     78.00 104.00   1.00   16.00    --  106.66  61.00 122.14   26
 32  \w     53.00  80.00   1.00   16.00    --  106.66-125.00-150.00   27
 33  \w     74.00 100.00   1.00   16.00    --  106.66  77.00-150.00   26
 34  \w     77.00 149.00   1.00   16.00    --  106.66  65.00 -16.30   72
 35  \w     77.00 103.00   1.00   16.00    --  106.66  63.00 127.47   26
 36  \w     74.00 178.00   1.00   16.00    --  106.66  77.00-180.00  104
 37  \w     34.00 108.00   1.00   16.00    --  106.66 -94.00  30.00   74
 38  \w     24.00 105.00   1.00   16.00    --  106.66 -94.00-150.00   81
 39  \w     77.00 107.00   1.00   16.00    --  106.66  65.00  28.95   30
 40  \w    116.00 178.00   1.00   16.00    --  106.66  77.00-150.00   62
 41  \w     74.00 144.00   1.00   16.00    --  106.66  77.00  60.00   70
 42  \w     97.00 122.00   1.00   16.00    --  106.66-125.00-150.00   25
 43  \w     78.00 104.00   1.00   16.00    --  106.66  61.00-150.00   26
 44  \w    114.00 178.00   1.00   16.00    --  106.66  77.00   0.00   64
 45  \w     74.00 177.00   1.00   16.00    --  106.66  77.00  90.00  103
 46  \w     74.00 100.00   1.00   16.00    --  106.66  77.00   0.00   26
 47  \w     79.00 139.00   1.00   16.00    --  106.66  61.00 150.00   60
 48  \w     74.00 100.00   1.00   16.00    --  106.66  77.00 120.00   26
 49  \w    115.00 178.00   1.00   16.00    --  106.66  77.00 120.00   63
 50  \w     74.00 100.00   1.00   16.00    --  106.66  77.00-120.00   26
 51  \w     24.00 102.00   1.00   16.00    --  106.66 -94.00 120.00   78
 52  \w     80.00 106.00   1.00   16.00    --  106.66  47.00 -57.19   26
 53  \w    124.00 149.00   1.00   16.00    --  106.66  60.00-116.45   25
 54  \w     78.00 104.00   1.00   16.00    --  106.66  58.00   6.86   26
 55  \w     78.00 104.00   1.00   16.00    --  106.66  58.00 -50.55   26
;
_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      -0.0767846000
_diffrn_orient_matrix_UB_12      -0.1069902000
_diffrn_orient_matrix_UB_13      0.0145560000
_diffrn_orient_matrix_UB_21      -0.0613256000
_diffrn_orient_matrix_UB_22      -0.0551971000
_diffrn_orient_matrix_UB_23      -0.0236310000
_diffrn_orient_matrix_UB_31      0.1230332000
_diffrn_orient_matrix_UB_32      -0.0942847000
_diffrn_orient_matrix_UB_33      -0.0026849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            82852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.746
_diffrn_reflns_theta_max         66.746
_diffrn_reflns_theta_min         4.389
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75971
_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    1.757
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 4105 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0522P)^2^+1.8624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8985
_reflns_number_total             9628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00983f2.cif
_cod_data_source_block           3
_cod_database_code               7043139
_chemical_oxdiff_formula         'C20 H20 N4 F15'
_reflns_odcompleteness_completeness 99.93
_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 N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N4A(H4AA), C1(H1), C1A(H1A), C2(H2), C2A(H2A), C3(H3), C3A(H3A),
 C4(H4A), C4A(H4AB), C7(H7), C7A(H7A), C9(H9), C9A(H9A), C12(H12), C12A(H12A),
 C13(H13), C13A(H13A), C14(H14), C14A(H14A), C15(H15), C15A(H15A), C17(H17),
 C17A(H17A), C18(H18), C18A(H18A), C20(H20), C20A(H20A), C21(H21), C21A(H21A)
;
_shelx_res_checksum              65567
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.835