Cationic diiron and diruthenium μ-allenyl complexes: synthesis, X-ray structures and cyclization reactions with ethyldiazoacetate/amine affording unprecedented butenolide- and furaniminium-substituted bridging carbene ligands.
Boni, Adriano; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 39 (2010) 10866–10875; doi:10.1039/c0dt00697a

data_7026785
_publ_section_title
;
 Cationic diiron and diruthenium \m-allenyl complexes: synthesis, X-ray
 structures and cyclization reactions with ethyldiazoacetate/amine
 affording unprecedented butenolide- and furaniminium-substituted bridging
 carbene ligands.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10866
_journal_page_last               10875
_journal_paper_doi               10.1039/c0dt00697a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C19 H17 F3 Fe2 O6 S'
_chemical_formula_weight         542.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6193(15)
_cell_length_b                   21.194(3)
_cell_length_c                   9.5464(14)
_cell_measurement_reflns_used    4065
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      21.9975
_cell_measurement_theta_min      2.340
_cell_volume                     2148.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16383
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.506
_exptl_absorpt_correction_T_max  0.8518
_exptl_absorpt_correction_T_min  0.7732
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4221
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0471P)^2^+2.7080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                2758
_reflns_number_total             4221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00697a.txt
_cod_data_source_block           '[4a][CF3SO3]'
_cod_original_cell_volume        2148.5(5)
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_database_code               7026785