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_4107034
_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                 94.196(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.832(2)
_cell_length_b                   14.4148(12)
_cell_length_c                   20.7661(14)
_cell_measurement_reflns_used    9727
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.40
_cell_measurement_theta_min      3.43
_cell_volume                     8607.4(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, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.940
_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  0.1186
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37459
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         65.09
_diffrn_reflns_theta_min         3.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.030
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs 2008/2'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The PLATON-SQUEEZE routine was used to treat approximately
6 molecules of disordered diethyl ether present within the 
unit cell.
;
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6898
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1911
_refine_ls_R_factor_gt           0.1711
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1249P)^2^+228.1829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4043
_refine_ls_wR_factor_ref         0.4151
_reflns_number_gt                5130
_reflns_number_total             6898
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja205736m_si_002_5.cif
_cod_data_source_block           cm27
_cod_database_code               4107034