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_7043137
_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, C H Cl3'
_chemical_formula_sum            'C30 H16 Cl3 F15 N4 O'
_chemical_formula_weight         839.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-11
_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                 99.250(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.62249(13)
_cell_length_b                   60.950(3)
_cell_length_c                   9.3539(3)
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    123.0(3)
_cell_measurement_theta_max      73.9290
_cell_measurement_theta_min      4.3280
_cell_volume                     3163.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -49.00  -11.20   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 126

  2 omega -115.00  -13.90   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -57.0000  -30.0000 337

  3 omega   -3.00   30.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 110

  4 omega   35.00   96.20   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -45.0000  -60.0000 204

  5 omega   22.00  157.00   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601    0.0000 -150.0000 450

  6 omega   44.00   88.10   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -45.0000 -150.0000 147

  7 omega   30.00   99.00   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000  -30.0000 230

  8 omega   31.00   67.00   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000    0.0000 120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.2531690000
_diffrn_orient_matrix_UB_12      -0.0052497000
_diffrn_orient_matrix_UB_13      -0.0339747000
_diffrn_orient_matrix_UB_21      0.1119021000
_diffrn_orient_matrix_UB_22      0.0071203000
_diffrn_orient_matrix_UB_23      0.1542058000
_diffrn_orient_matrix_UB_31      -0.0224298000
_diffrn_orient_matrix_UB_32      -0.0236773000
_diffrn_orient_matrix_UB_33      0.0537749000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -72
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9579
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.746
_diffrn_reflns_theta_max         66.746
_diffrn_reflns_theta_min         4.352
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82305
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.763
_exptl_crystal_description       needle
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.0833
_exptl_crystal_size_mid          0.0409
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         5545
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0554P)^2^+1.7779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4423
_reflns_number_total             5545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00983f2.cif
_cod_data_source_block           3_CHCl3
_cod_original_cell_volume        3163.84(19)
_cod_database_code               7043137
_chemical_oxdiff_formula         'C28 H20 N4 O F20'
_reflns_odcompleteness_completeness 98.95
_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. Restrained distances
 F25-C34
 1.32 with sigma of 0.02
 F26-C35
 1.32 with sigma of 0.02
 C34-F23
 1.32 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.01
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C34) = Uanis(C35)
Uanis(C25) = Uanis(C24)
4. Others
 Sof(C25)=Sof(F3)=Sof(F5)=1-FVAR(1)
 Sof(C24)=Sof(F4)=Sof(F6)=FVAR(1)
 Sof(C27)=Sof(F8)=Sof(F10)=1-FVAR(2)
 Sof(C26)=Sof(F7)=Sof(F9)=FVAR(2)
 Sof(C29)=Sof(F13)=Sof(F14)=1-FVAR(3)
 Sof(C28)=Sof(F11)=Sof(F12)=FVAR(3)
 Sof(C32)=Sof(F19)=Sof(F20)=1-FVAR(4)
 Sof(C33)=Sof(F21)=Sof(F22)=FVAR(4)
 Sof(C35)=Sof(F25)=Sof(F27)=Sof(F28)=1-FVAR(5)
 Sof(C34)=Sof(F23)=Sof(F24)=Sof(F26)=FVAR(5)
 Sof(C30)=Sof(F17)=Sof(F18)=1-FVAR(6)
 Sof(C31)=Sof(F15)=Sof(F16)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C36(H36)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), N4(H4A)
;
_shelx_res_checksum              86213
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'