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_4073444
_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            'C35 H42 Cl2 F3 Fe2 N3 O7 S'
_chemical_formula_weight         888.38
_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                107.03(3)
_cell_angle_beta                 98.26(3)
_cell_angle_gamma                110.62(3)
_cell_formula_units_Z            2
_cell_length_a                   11.814(2)
_cell_length_b                   12.577(3)
_cell_length_c                   15.404(3)
_cell_measurement_reflns_used    1004
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4165
_cell_measurement_theta_min      2.5895
_cell_volume                     1968.8(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21139
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.8578
_exptl_absorpt_correction_T_min  0.7830
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.276
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8694
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+2.0471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1901
_reflns_number_gt                6334
_reflns_number_total             8694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700334h-file003.cif
_cod_data_source_block           z89p-1
_cod_original_cell_volume        1968.8(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073444