Reactions of Diazo Compounds at μ-Vinyliminium Ligands: Synthesis of Novel Dinuclear Azine−Bis(alkylidene) Complexes
Busetto, Luigi; Marchetti, Fabio; Zacchini, Stefano; Zanotti, Valerio; Organometallics 26 (2007) 3577–; doi:10.1021/om700334h

data_4073443
_publ_section_title
;
 Reactions of Diazo Compounds at \m-Vinyliminium Ligands:&#x00A0;
 Synthesis of Novel Dinuclear Azine&#x2212;Bis(alkylidene) Complexes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3577
_journal_paper_doi               10.1021/om700334h
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C29 H31 Fe2 N3 O4'
_chemical_formula_weight         597.27
_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                96.29(3)
_cell_angle_beta                 95.75(3)
_cell_angle_gamma                96.76(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0593(18)
_cell_length_b                   11.785(2)
_cell_length_c                   12.541(3)
_cell_measurement_reflns_used    4264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.746
_cell_measurement_theta_min      2.252
_cell_volume                     1312.9(5)
_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_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15791
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.8560
_exptl_absorpt_correction_T_min  0.7627
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0593P)^2^+0.0234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                5566
_reflns_number_total             6761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700334h-file002.cif
_cod_data_source_block           z40p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073443