Four-Electron Oxidative Dehydrogenation Induced by Proton-Coupled Electron Transfer in Ruthenium(III) Complex with 2-(1,4,5,6-Tetrahydropyrimidin-2-yl)phenolate
Ryoji Mitsuhashi; Takayoshi Suzuki; Yukinari Sunatsuki; Inorganic Chemistry 52 (2013) 10183–10190; doi:10.1021/ic401667v

data_4335915
_publ_section_title
;
 Four-Electron Oxidative Dehydrogenation Induced by Proton-Coupled
 Electron Transfer in Ruthenium(III) Complex with
 2-(1,4,5,6-Tetrahydropyrimidin-2-yl)phenolate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10183
_journal_page_last               10190
_journal_paper_doi               10.1021/ic401667v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C30 H27 N6 O Ru 1+, B F4 1-, C H4 O'
_chemical_formula_sum            'C31 H31 B F4 N6 O2 Ru'
_chemical_formula_weight         707.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.006(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9379(7)
_cell_length_b                   10.0441(8)
_cell_length_c                   30.4265(19)
_cell_measurement_reflns_used    31126
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3025.5(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'ortep-3 for win'
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            27312
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.8002
_exptl_absorpt_correction_T_min  0.7592
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0388P)^2^+3.7032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                6024
_reflns_number_total             6909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401667v_si_002_02.cif
_cod_data_source_block           2_BF4_CH3OH
_cod_database_code               4335915