Synthesis and Electronic Structure Determination of N-Alkyl-Substituted Bis(imino)pyridine Iron Imides Exhibiting Spin Crossover Behavior
Amanda C. Bowman; Carsten Milsmann; Eckhard Bill; Zoë R. Turner; Emil Lobkovsky; Serena DeBeer; Karl Wieghardt; Paul J. Chirik; Journal of the American Chemical Society 133 (2011) 17353–17369; doi:10.1021/ja205736m

data_4107032
_publ_section_title
;
 Synthesis and Electronic Structure Determination of N-Alkyl-Substituted
 Bis(imino)pyridine Iron Imides Exhibiting Spin Crossover Behavior
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17353
_journal_page_last               17369
_journal_paper_doi               10.1021/ja205736m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C43 H58 Fe N4'
_chemical_formula_sum            'C43 H58 Fe N4'
_chemical_formula_weight         686.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 94.477(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.160(4)
_cell_length_b                   14.6320(19)
_cell_length_c                   20.850(3)
_cell_measurement_reflns_used    2784
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      19.18
_cell_measurement_theta_min      2.52
_cell_volume                     8869(2)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26619
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  0.9640
_exptl_absorpt_correction_T_min  0.9640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_description       'cube like'
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0783P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                3818
_reflns_number_total             5970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205736m_si_002_3.cif
_cod_data_source_block           iPrPDIFeN2Ad
_cod_database_code               4107032