Bis(imino)pyridine Iron Dinitrogen Compounds Revisited: Differences in Electronic Structure Between Four- and Five-Coordinate Derivatives.
S. Chantal E. Stieber; Carsten Milsmann; Jordan M. Hoyt; Zoë R. Turner; Kenneth D. Finkelstein; Karl Wieghardt; Serena DeBeer; Paul J. Chirik; Inorganic Chemistry 51 (2012) 3770–3785; doi:10.1021/ic202750n

data_4328688
_publ_section_title
;
 Bis(imino)pyridine Iron Dinitrogen Compounds Revisited: Differences in
 Electronic Structure Between Four- and Five-Coordinate Derivatives.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3770
_journal_page_last               3785
_journal_paper_doi               10.1021/ic202750n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C37 H51 Fe N5'
_chemical_formula_sum            'C37 H51 Fe N5'
_chemical_formula_weight         621.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.3410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7394(2)
_cell_length_b                   13.6105(2)
_cell_length_c                   24.6266(4)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.55
_cell_measurement_theta_min      3.64
_cell_volume                     3882.64(11)
_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_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_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            38146
_diffrn_reflns_theta_full        65.99
_diffrn_reflns_theta_max         65.99
_diffrn_reflns_theta_min         3.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.320
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.5911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The squeeze procedure was used to acount for 3 molecules of hexane present
within the unit cell.
;
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.706
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.706
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1801P)^2^+9.1158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1851
_refine_ls_wR_factor_ref         0.2018
_reflns_number_gt                5261
_reflns_number_total             6661
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202750n_si_001_1.cif
_cod_data_source_block           jmh2
_cod_database_code               4328688