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_4104019
_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         'C24 H20 Co N6, C4 H8 O, C F3 O3 S'
_chemical_formula_sum            'C29 H28 Co F3 N6 O4 S'
_chemical_formula_weight         672.56
_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                 126.141(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.8068(12)
_cell_length_b                   14.4243(5)
_cell_length_c                   18.5224(7)
_cell_measurement_reflns_used    3338
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      2.20
_cell_volume                     6646.9(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28729
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.9390
_exptl_absorpt_correction_T_min  0.7846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic black'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6783
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.145
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                4835
_reflns_number_total             6783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8089747_si_005.cif
_cod_data_source_block           bf18
_cod_original_cell_volume        6646.9(4)
_cod_database_code               4104019