Unusual Electronic Features and Reactivity of the Dipyridylazaallyl Ligand: Characterizations of (smif)2M [M = Fe, Co, Co+, Ni; smif = {(2-py)CH}2N] and [(TMS)2NFe]2(smif)2
Brenda A. Frazier; Peter T. Wolczanski; Emil B. Lobkovsky; Thomas R. Cundari; Journal of the American Chemical Society 131 (2009) 3428–3429; doi:10.1021/ja8089747

data_4104017
_publ_section_title
;
 Unusual Electronic Features and Reactivity of the Dipyridylazaallyl
 Ligand: Characterizations of (smif)2M [M = Fe, Co, Co+, Ni; smif =
 {(2-py)CH}2N] and [(TMS)2NFe]2(smif)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3428
_journal_page_last               3429
_journal_paper_doi               10.1021/ja8089747
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C18 H28 Fe N4 Si2'
_chemical_formula_sum            'C18 H28 Fe N4 Si2'
_chemical_formula_weight         412.47
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.491(3)
_cell_angle_beta                 85.244(4)
_cell_angle_gamma                81.614(4)
_cell_formula_units_Z            2
_cell_length_a                   8.0558(5)
_cell_length_b                   10.8367(7)
_cell_length_c                   14.3114(9)
_cell_measurement_reflns_used    6155
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1177.73(13)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32284
_diffrn_reflns_theta_full        30.69
_diffrn_reflns_theta_max         30.69
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.8959
_exptl_absorpt_correction_T_min  0.7537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                5519
_reflns_number_total             7293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8089747_si_003.cif
_cod_data_source_block           bf8
_cod_database_code               4104017