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_4071882
_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            'C38.5 H40 Cl3 Fe2 N3 O4'
_chemical_formula_weight         826.79
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.56(3)
_cell_angle_beta                 93.89(3)
_cell_angle_gamma                95.94(3)
_cell_formula_units_Z            2
_cell_length_a                   11.013(2)
_cell_length_b                   11.506(2)
_cell_length_c                   14.818(3)
_cell_measurement_reflns_used    6461
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.921
_cell_measurement_theta_min      2.235
_cell_volume                     1856.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19454
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.8266
_exptl_absorpt_correction_T_min  0.7183
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8185
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0451P)^2^+1.8184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                7457
_reflns_number_total             8185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800445k_si_007.cif
_cod_data_source_block           z38p-1
_cod_original_cell_volume        1856.1(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C38.50 H40 Cl3 Fe2 N3 O4'
_cod_database_code               4071882