Dinuclear Ru/Ni, Ir/Ni, and Ir/Pt Complexes with Bridging Phenanthroline-5,6-dithiolate: Synthesis, Structure, and Electrochemical and Photophysical Behavior.
Schallenberg, David; Neubauer, Antje; Erdmann, Elisa; Tänzler, Marco; Villinger, Alexander; Lochbrunner, Stefan; Seidel, Wolfram W.; Inorganic chemistry 53 (2014) 8859–8873; doi:10.1021/ic4031206

data_4340866
_publ_section_title
;
 Dinuclear Ru/Ni, Ir/Ni, and Ir/Pt Complexes with Bridging
 Phenanthroline-5,6-dithiolate: Synthesis, Structure, and Electrochemical
 and Photophysical Behavior.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8859
_journal_page_last               8873
_journal_paper_doi               10.1021/ic4031206
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
;
C61 H50 N2 Ni P3 Ru S2 +, F6 P -, 1.5(C6 H5 F)
;
_chemical_formula_sum            'C70 H57.5 F7.5 N2 Ni P4 Ru S2'
_chemical_formula_weight         1416.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                115.0290(10)
_cell_angle_beta                 90.898(2)
_cell_angle_gamma                99.323(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0988(4)
_cell_length_b                   14.6087(4)
_cell_length_c                   16.5442(5)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.711
_cell_measurement_theta_min      4.963
_cell_volume                     3033.21(15)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96341
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_correction_T_min  0.7139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1446
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The unit cell contains three fluorobenzene molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         21423
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                12850
_reflns_number_total             21423
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic4031206_si_004.cif
_cod_data_source_block           is_schal237cp
_cod_depositor_comments
'Adding full bibliography for 4340865--4340867.cif.'
_cod_original_formula_sum        'C70 H57.50 F7.50 N2 Ni P4 Ru S2'
_cod_database_code               4340866