Bis(imino)pyridine Iron Dinitrogen Compounds Revisited: Differences in Electronic Structure Between Four- and Five-Coordinate Derivatives.
E Stieber, S Chantal; Milsmann, Carsten; Hoyt, Jordan M.; Turner, Zoë R; Finkelstein, Kenneth D.; Wieghardt, Karl; Debeer, Serena; Chirik, Paul J.; Organometallics 31 (2012) 2275–2285; doi:10.1021/om201212m

data_4076438
_publ_section_title
;
 Bis(imino)pyridine Iron Dinitrogen Compounds Revisited: Differences in
 Electronic Structure Between Four- and Five-Coordinate Derivatives.
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2275
_journal_page_last               2285
_journal_paper_doi               10.1021/om201212m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C37 H51 Fe N7'
_chemical_formula_sum            'C37 H51 Fe N7'
_chemical_formula_weight         649.70
_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                99.7520(10)
_cell_angle_beta                 94.9880(10)
_cell_angle_gamma                100.8610(10)
_cell_formula_units_Z            4
_cell_length_a                   12.44830(10)
_cell_length_b                   13.06560(10)
_cell_length_c                   24.0716(3)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.61
_cell_measurement_theta_min      3.64
_cell_volume                     3760.74(7)
_computing_cell_refinement       'BRUKER, APEX II SOFTWARE SUITE'
_computing_data_collection       'BRUKER, APEX II SOFTWARE SUITE'
_computing_data_reduction        'BRUKER, APEX II SOFTWARE SUITE'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 'acta 50'
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39567
_diffrn_reflns_theta_full        'acta 50'
_diffrn_reflns_theta_max         66.30
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    3.464
_exptl_absorpt_correction_T_max  0.7233
_exptl_absorpt_correction_T_min  0.5904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The unit cell contains half of a molecule of disorded diethyl ether. This has been treated with the PLATON-SQUEEZE routine accordingly.
;
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.520
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         12442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.520
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1494P)^2^+6.7159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                10934
_reflns_number_total             12442
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om201212m_si_002.cif
_cod_data_source_block           jmd23
_cod_depositor_comments
'Adding full bibliography for 4076435--4076439.cif.'
_cod_original_cell_volume        3760.74(6)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4076438