Fully Delocalized (Ethynyl)(vinyl)phenylene Bridged Triruthenium Complexes in up to Five Different Oxidation States
Evelyn Wuttke; Florian Pevny; Yves-Marie Hervault; Lucie Norel; Malte Drescher; Rainer F. Winter; Stéphane Rigaut; Inorganic Chemistry 51 (2012) 1902–1915; doi:10.1021/ic2022177

data_4328266
_publ_section_title
;
 Fully Delocalized (Ethynyl)(vinyl)phenylene Bridged Triruthenium
 Complexes in up to Five Different Oxidation States
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1902
_journal_page_last               1915
_journal_paper_doi               10.1021/ic2022177
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C50 H96 Cl2 O4 P4 Ru2, 4(C H Cl3)'
_chemical_formula_sum            'C54 H100 Cl14 O4 P4 Ru2'
_chemical_formula_weight         1635.66
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.58(3)
_cell_angle_beta                 93.34(3)
_cell_angle_gamma                110.62(3)
_cell_formula_units_Z            1
_cell_length_a                   9.2229(18)
_cell_length_b                   11.547(2)
_cell_length_c                   18.729(4)
_cell_measurement_reflns_used    42238
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.79
_cell_volume                     1844.0(8)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26143
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.8038
_exptl_absorpt_correction_T_min  0.7268
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         2.225
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0195P)^2^+21.0247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1705
_reflns_number_gt                6878
_reflns_number_total             7799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2022177_si_002_3.cif
_cod_data_source_block           ewbw10
_cod_original_cell_volume        1844.1(6)
_cod_database_code               4328266