An Azophenine Radical-Bridged Fe2 Single-Molecule Magnet with Record Magnetic Exchange Coupling
Ie-Rang Jeon; Jesse G. Park; Dianne J. Xiao; T. David Harris; Journal of the American Chemical Society 135 (2013) 16845–16848; doi:10.1021/ja409927v

data_4121143
_publ_contact_author
;
        T. David Harris
        Department of Chemistry
    Northwestern University
    2145 Sheridan Road
    Evanston, IL 60201-3113
    USA
;
_publ_contact_author_email       dharris@northwestern.edu
_publ_contact_author_phone       '(1)847 467 4176'
_publ_section_title
;
 An Azophenine Radical-Bridged Fe2 Single-Molecule Magnet with Record
 Magnetic Exchange Coupling
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16845
_journal_page_last               16848
_journal_paper_doi               10.1021/ja409927v
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C66 H58 Fe2 N12, C F3 O3 S, 6(C2 H3 N)'
_chemical_formula_sum            'C79 H76 F3 Fe2 N18 O3 S'
_chemical_formula_weight         1526.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   35.9492(8)
_cell_length_b                   35.9492(8)
_cell_length_c                   14.0374(4)
_cell_measurement_reflns_used    5296
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.46
_cell_measurement_theta_min      3.45
_cell_volume                     15710.7(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38426
_diffrn_reflns_theta_full        65.19
_diffrn_reflns_theta_max         65.19
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    4.219
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_correction_T_min  0.9204
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             7155
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains 36 acetonitrile molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
These molecules were included in the final molecular formula directly.
;
_refine_diff_density_max         0.823
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5948
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0694
_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^)+(0.1158P)^2^+50.9264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.1955
_reflns_number_gt                4908
_reflns_number_total             5948
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja409927v_si_003.cif
_cod_data_source_block           compound_2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4121143