Supramolecular Architectures with π-Acidic 3,6-Bis(2-pyridyl)-1,2,4,5-tetrazine Cavities: Role of Anion-π Interactions in the Remarkable Stability of Fe(II) Metallacycles in Solution
Helen T. Chifotides; Ian D. Giles; Kim R. Dunbar; Journal of the American Chemical Society 135 (2013) 3039–3055; doi:10.1021/ja3082473

data_4119390
_publ_contact_author_address
;
Department of Chemistry
Texas A&M University
College Station, TX 77843-3255
;
_publ_contact_author_email       dunbar@chem.tamu.edu
_publ_contact_author_fax         +1(979)845-7177
_publ_contact_author_name        'Kim R. Dunbar'
_publ_contact_author_phone       +1(979)845-5235
_publ_section_title
;
 Supramolecular Architectures with \p-Acidic
 3,6-Bis(2-pyridyl)-1,2,4,5-tetrazine Cavities: Role of Anion-\p
 Interactions in the Remarkable Stability of Fe(II) Metallacycles in
 Solution
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3039
_journal_page_last               3055
_journal_paper_doi               10.1021/ja3082473
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C80 H70 N40 Fe5, 10(Sb F6)'
_chemical_formula_sum            'C80 H70 F60 Fe5 N40 Sb10'
_chemical_formula_weight         4228.51
_chemical_name_systematic
; 
pentakis(3,6-bis(pyrid-2-yl)-1,2,4,5-tetrazine-N,N',N'',N''')
-decakis(acetonitrile-N)-pentairon(II)bis hexafluoroantimonate(V) clathrate 
octakis(hexafluoroantimonate(V)) acetonitrile solvate 
;
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.824(11)
_cell_length_b                   37.92(4)
_cell_length_c                   34.12(3)
_cell_measurement_reflns_used    196
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      2.9
_cell_volume                     15298(3)
_computing_cell_refinement       'SAINT v7.60A (Bruker 2008)'
_computing_data_collection       'APEXII (Bruker 2008)'
_computing_data_reduction        'SAINT v7.60A, XPREP v2008/2 (Bruker 2008)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Bruker APEX2 CCD area-detector, 3 circle goniometer'
;
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1421
_diffrn_reflns_av_sigmaI/netI    0.3100
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            30355
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    2.314
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS Scale, SADABS (Bruker 2008)'
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_description       plate
_exptl_crystal_F_000             8040
_exptl_crystal_recrystallization_method
;
layered acetonitrile solution over toluene
;
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.426
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.714
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         15658
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.715
_refine_ls_R_factor_all          0.2411
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1952
_refine_ls_wR_factor_ref         0.2404
_reflns_number_gt                4022
_reflns_number_total             15658
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3082473_si_003.cif
_cod_data_source_block           pbcn_4
_cod_original_cell_volume        15299(25)
_cod_database_code               4119390