Synthesis of Tridentate 2,6-Bis(imino)pyridyl Ruthenium(II) Complexes with N-Heterocyclic Carbene Ligands: Activation of Imidazolium Salts.
Yoo, Hyojong; Berry, Donald H.; Inorganic chemistry 53 (2014) 11447–11456; doi:10.1021/ic501248c

data_4341364
_publ_section_title
;
 Synthesis of Tridentate 2,6-Bis(imino)pyridyl Ruthenium(II) Complexes
 with N-Heterocyclic Carbene Ligands: Activation of Imidazolium Salts.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11447
_journal_page_last               11456
_journal_paper_doi               10.1021/ic501248c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C39 H47 N5 O3 Ru S'
_chemical_formula_weight         766.95
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.672(6)
_cell_angle_beta                 75.450(6)
_cell_angle_gamma                77.123(6)
_cell_formula_units_Z            2
_cell_length_a                   10.2854(8)
_cell_length_b                   12.4186(11)
_cell_length_c                   15.7211(13)
_cell_measurement_temperature    143(1)
_cell_volume                     1873.7(3)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22546
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6945
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       prism
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.614
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         8267
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+2.7621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                7274
_reflns_number_total             8267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501248c_si_003.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4341363--4341365.cif.'
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               4341364