A Combined Spectroscopic and Computational Study of a High-Spin S=7/2 Diiron Complex with a Short Iron-Iron Bond
Christopher M. Zall; Danylo Zherebetskyy; Allison L. Dzubak; Eckhard Bill; Laura Gagliardi; Connie C. Lu; Inorganic Chemistry 51 (2012) 728–736; doi:10.1021/ic202384b

data_4327918
_publ_section_title
;
 A Combined Spectroscopic and Computational Study of a High-Spin S=7/2
 Diiron Complex with a Short Iron-Iron Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              728
_journal_page_last               736
_journal_paper_doi               10.1021/ic202384b
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C39 H33 Fe2 N6, 0.5(C6 H6)'
_chemical_formula_sum            'C42 H36 Fe2 N6'
_chemical_formula_weight         736.48
_chemical_name_common            Fe2(DPhF)3(C6H6)0.5
_chemical_name_systematic        'Diiron tris-N,N'diphenylformamidinate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                108.303(2)
_cell_angle_beta                 91.290(2)
_cell_angle_gamma                95.539(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3170(18)
_cell_length_b                   11.9544(18)
_cell_length_c                   13.948(2)
_cell_measurement_reflns_used    4095
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.31
_cell_volume                     1780.4(5)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19037
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.9195
_exptl_absorpt_correction_T_min  0.7837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                4528
_reflns_number_total             7222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202384b_si_002.cif
_cod_data_source_block           10106m
_cod_database_code               4327918