Addition of Isocyanides at Diiron μ-Vinyliminium Complexes: Synthesis of Novel Ketenimine−Bis(alkylidene) Complexes
Busetto, Luigi; Marchetti, Fabio; Zacchini, Stefano; Zanotti, Valerio; Organometallics 27 (2008) 5058–; doi:10.1021/om800445k

data_4071884
_publ_section_title
;
 Addition of Isocyanides at Diiron \m-Vinyliminium Complexes: Synthesis of
 Novel Ketenimine&#x2212;Bis(alkylidene) Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5058
_journal_paper_doi               10.1021/om800445k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C24 H32 Fe2 N3 O2.5'
_chemical_formula_weight         514.23
_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                 99.670(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.013(3)
_cell_length_b                   14.6744(17)
_cell_length_c                   11.5698(13)
_cell_measurement_reflns_used    7362
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0385
_cell_measurement_theta_min      2.275
_cell_volume                     5023.2(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26607
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  0.8521
_exptl_absorpt_correction_T_min  0.7811
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5129
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+0.4401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                3901
_reflns_number_total             5129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800445k_si_009.cif
_cod_data_source_block           z119
_cod_original_cell_volume        5023.1(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C24 H32 Fe2 N3 O2.50'
_cod_database_code               4071884