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_4335921
_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         'C9 H10 N2 O'
_chemical_formula_sum            'C9 H10 N2 O'
_chemical_formula_weight         162.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.718(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.9475(19)
_cell_length_b                   7.4571(14)
_cell_length_c                   21.436(4)
_cell_measurement_reflns_used    8148
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.34
_cell_volume                     1579.2(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'ortep-3 for win'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS 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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15039
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.33
_diffrn_standards_number         15039
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9729
_exptl_absorpt_correction_T_min  0.9555
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       platelet
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                3022
_reflns_number_total             3608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401667v_si_002_08.cif
_cod_data_source_block           H2imn
_cod_database_code               4335921