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_4119389
_publ_contact_author_address
;Department of Chemistry
Texas A&M University
College Station, TX 77842-3255, USA
;
_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_absolute_configuration unk
_chemical_formula_moiety         'Fe4 C64 H56 N32 8+, 8(B F4 1-)'
_chemical_formula_sum            'C64 H56 B8 F32 Fe4 N32'
_chemical_formula_weight         2191.29
_chemical_name_common            'Fe(II) Square with bptz and [BF4]-'
_chemical_name_systematic
;        
tetrakis(3,6-bis(Pyrid-2-yl)-1,2,4,5-tetrazine-N,N',N'',N''')-
octakis(acetonitrile-N)-tetrairon(II)-tetrafluoroborate clathrate 
heptakis(tetrafluoroborate)acetonitrile solvate
;
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.364(3)
_cell_angle_beta                 84.223(3)
_cell_angle_gamma                76.651(3)
_cell_formula_units_Z            2
_cell_length_a                   14.678(3)
_cell_length_b                   18.363(4)
_cell_length_c                   20.780(5)
_cell_measurement_reflns_used    1025
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      18.75
_cell_measurement_theta_min      1.44
_cell_volume                     5412(2)
_computing_cell_refinement       'APEX2 v2011.6-1 (Bruker AXS 2011)'
_computing_data_collection       'APEX2 v2011.6-1 (Bruker AXS 2011)'
_computing_data_reduction        'APEX2 v2011.6-1 (Bruker AXS 2011)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker APEX2 CCD area-detector, SMART 3 circle goniometer'
;
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.1359
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50883
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS Scale (Bruker 2011)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       needle
_exptl_crystal_F_000             2192
_exptl_crystal_recrystallization_method
'layered acetonitrile solution over toluene'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         18430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1748
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2478
_refine_ls_wR_factor_ref         0.2813
_reflns_number_gt                7081
_reflns_number_total             18430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3082473_si_002.cif
_cod_data_source_block           p-1-sr
_cod_database_code               4119389