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_4071526
_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            'C85.5 H72.5 Cl4.5 Fe N2 O3 P2 Re Ru'
_chemical_formula_weight         1740.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 91.512(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.5669(5)
_cell_length_b                   11.3780(3)
_cell_length_c                   53.1036(11)
_cell_measurement_reflns_used    27266
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.2219
_cell_measurement_theta_min      2.8189
_cell_volume                     15442.5(6)
_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  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.1441
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            86133
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77206
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             7000
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.840
_refine_diff_density_min         -2.381
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1907
_refine_ls_number_reflns         30035
_refine_ls_number_restraints     535
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.1036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+350.0074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.2347
_reflns_number_gt                19279
_reflns_number_total             30035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800206k-file006.cif
_cod_data_source_block           rico53
_cod_depositor_comments
;

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C171 H145 Cl9 Fe2 N4 O6 P4 Re2 Ru2'
_cod_original_formula_weight         3481.08
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4071526