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_4107031
_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         'C41 H58 Fe N4'
_chemical_formula_sum            'C41 H58 Fe N4'
_chemical_formula_weight         662.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.764(5)
_cell_length_b                   14.825(3)
_cell_length_c                   21.812(4)
_cell_measurement_temperature    293(2)
_cell_volume                     7328(3)
_computing_cell_refinement       HKL2000
_computing_data_collection       'CHESS A1 station'
_computing_data_reduction        HKL2000
_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      293(2)
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.713
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         CHESS
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.97820
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7129
_diffrn_reflns_theta_full        32.28
_diffrn_reflns_theta_max         32.28
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.9363
_exptl_absorpt_correction_T_min  0.8598
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         7129
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.445
_refine_ls_shift/su_mean         0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1602P)^2^+14.5387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2243
_refine_ls_wR_factor_ref         0.2304
_reflns_number_gt                7000
_reflns_number_total             7129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205736m_si_002_2.cif
_cod_data_source_block           iPrPDIFeNCyOct
_cod_database_code               4107031