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_4071881
_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            'C35 H34 Fe2 N2 O4'
_chemical_formula_weight         658.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.71(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.849(3)
_cell_length_b                   13.765(3)
_cell_length_c                   17.266(4)
_cell_measurement_reflns_used    4992
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5265
_cell_measurement_theta_min      2.436
_cell_volume                     3036.3(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32638
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.8567
_exptl_absorpt_correction_T_min  0.7815
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6961
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0645P)^2^+0.7714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                5370
_reflns_number_total             6961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800445k_si_006.cif
_cod_data_source_block           z45p21c
_cod_original_cell_volume        3036.4(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4071881