Heterotrimetallic M−M′−M′′ Transition Metal Complexes Based on 1,3,5-Triethynylbenzene: Synthesis, Solid State Structure, and Electrochemical and UV−Vis Characterization. EPR Analysis of thein SituGenerated Associated Radical Cations
Packheiser, Rico; Ecorchard, Petra; Rüffer, Tobias; Lohan, Manja; Bräuer, Björn; Justaud, Frédéric; Lapinte, Claude; Lang, Heinrich; Organometallics 27 (2008) 3444–; doi:10.1021/om800206k

data_4071524
_publ_section_title
;
 Heterotrimetallic M&#x2212;M&#x2032;&#x2212;M&#x2032;&#x2032; Transition
 Metal Complexes Based on 1,3,5-Triethynylbenzene: Synthesis, Solid State
 Structure, and Electrochemical and UV&#x2212;Vis Characterization. EPR
 Analysis of thein SituGenerated Associated Radical Cations
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3444
_journal_paper_doi               10.1021/om800206k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C43 H37 Fe N2 O3 Re'
_chemical_formula_weight         871.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.457(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0242(9)
_cell_length_b                   12.0532(9)
_cell_length_c                   19.8283(16)
_cell_measurement_reflns_used    10433
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.9999
_cell_measurement_theta_min      2.7975
_cell_volume                     3753.4(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_publication_material  shelxtl
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34504
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    3.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71715
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         7356
_refine_ls_number_restraints     684
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                4677
_reflns_number_total             7356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800206k-file004.cif
_cod_data_source_block           rico47
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4071524