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_7043135
_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
'C64 H38 F34 N8 Ni O2, 2(Cl), 2(C2 H6 O S), H2 O'
_chemical_formula_sum            'C68 H52 Cl2 F34 N8 Ni O5 S2'
_chemical_formula_weight         1900.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                95.396(6)
_cell_angle_beta                 91.534(6)
_cell_angle_gamma                90.814(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4507(7)
_cell_length_b                   13.2384(8)
_cell_length_c                   26.961(2)
_cell_measurement_reflns_used    3482
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.4820
_cell_measurement_theta_min      3.5710
_cell_volume                     3711.7(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)'
_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 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -107.00 -17.00   1.50   21.00    --  -41.90 -37.00   0.00   60
  2  \w    -66.00  28.50   1.50   21.00    --  -41.90  37.00-180.00   63
  3  \w    -96.00  -6.00   1.50   21.00    --  -41.90 125.00 -90.00   60
  4  \w    -96.00  -3.00   1.50   21.00    --  -41.90 125.00-180.00   62
  5  \w     44.00 135.50   1.50   84.00    --  112.00 -77.00  30.00   61
  6  \w     88.00 178.00   1.50   84.00    --  112.00  45.00  90.00   60
  7  \w     58.00 136.00   1.50   84.00    --  112.00 -30.00  30.00   52
  8  \w     93.00 174.00   1.50   84.00    --  112.00  30.00-150.00   54
  9  \w     43.00 115.00   1.50   84.00    --  112.00-111.00-150.00   48
 10  \w     38.00 122.00   1.50   84.00    --  112.00 -89.00 -59.00   56
 11  \w     51.00 135.00   1.50   84.00    --  112.00 -45.00 150.00   56
 12  \w     39.00 117.00   1.50   84.00    --  112.00 -30.00 -90.00   52
;
_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      -0.0650949000
_diffrn_orient_matrix_UB_12      -0.0174057000
_diffrn_orient_matrix_UB_13      -0.0521106000
_diffrn_orient_matrix_UB_21      0.0084789000
_diffrn_orient_matrix_UB_22      -0.1155978000
_diffrn_orient_matrix_UB_23      0.0021465000
_diffrn_orient_matrix_UB_31      -0.1320712000
_diffrn_orient_matrix_UB_32      -0.0010368000
_diffrn_orient_matrix_UB_33      0.0240112000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.1108
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20793
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.746
_diffrn_reflns_theta_max         66.746
_diffrn_reflns_theta_min         3.354
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77879
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.941
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         13059
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1066P)^2^+2.4553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8000
_reflns_number_total             13059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00983f2.cif
_cod_data_source_block           Ni42_Cl2
_cod_database_code               7043135
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12'
_reflns_odcompleteness_completeness 99.20
_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 C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) = Uanis(C29)
Uanis(C25) = Uanis(C24)
3. Others
 Sof(F3)=Sof(F4)=Sof(F7)=Sof(F8)=Sof(H23C)=Sof(H23D)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(C26)=Sof(C29)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F5)=Sof(F6)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(C27)=Sof(C28)=FVAR(1)
 Fixed Sof: S1(0.5) S2(0.5) F22(0.5) F23(0.5) F24(0.5) F25(0.5) F26(0.5)
 F27(0.5) F28(0.5) F29(0.5) F30(0.5) F31(0.5) F32(0.5) F33(0.5) F34(0.5)
 F35(0.5) F36(0.5) F37(0.5) F38(0.5) F39(0.5) F40(0.5) F41(0.5) F42(0.5)
 F43(0.5) F44(0.5) F45(0.5) F46(0.5) F47(0.5) F48(0.5) F49(0.5) F50(0.5)
 F51(0.5) F52(0.5) F53(0.5) F54(0.5) F55(0.5) C67(0.5) C68(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) H71D(0.5) H71E(0.5) H71F(0.5) C72(0.5) H72A(0.5) H72B(0.5)
 H72C(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5)
4.a Riding coordinates:
 O5(H5A,H5B), N7(H7), N8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C23(H23C,H23D), C24(H24A,H24B), C25(H25A,H25B), C58(H58A,
 H58B), C59(H59A,H59B)
4.c Me refined with riding coordinates:
 C71(H71A,H71B,H71C), C71(H71D,H71E,H71F)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7A), C9(H9), C12(H12), C13(H13), C14(H14),
  C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C36(H36), C37(H37),
 C38(H38), C39(H39), C42(H42), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50),
  C52(H52), C53(H53), C55(H55), C56(H56)
4.e Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C)
;
_shelx_res_checksum              17144
_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 1.365
_oxdiff_exptl_absorpt_empirical_full_min 0.669