Dehydrogenative Coupling of 4-Substituted Pyridines Catalyzed by Diruthenium Complexes
Takashi Kawashima; Toshiro Takao; Hiroharu Suzuki; Journal of the American Chemical Society 129 (2007) 11006–11007; doi:10.1021/ja074224u

data_4109918
_publ_section_title
;
 Dehydrogenative Coupling of 4-Substituted Pyridines Catalyzed by
 Diruthenium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11006
_journal_page_last               11007
_journal_paper_doi               10.1021/ja074224u
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C37 H56 N2 O2 Ru2'
_chemical_formula_weight         762.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 93.5110(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1058(4)
_cell_length_b                   13.1552(6)
_cell_length_c                   13.5335(5)
_cell_measurement_reflns_used    17165
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.02
_cell_volume                     1795.82(13)
_computing_cell_refinement       'PROCESS-AUTO (T.Higashi, 1998)'
_computing_data_collection       'PROCESS-AUTO (T.Higashi, 1998)'
_computing_data_reduction        'PROCESS-AUTO (T.Higashi, 1998)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       'oscillation photograph'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating Anode ultraX18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17165
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6159
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0599P)^2^+2.4607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                3304
_reflns_number_total             4283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074224usi20070610_095731_1.cif
_cod_data_source_block           3
_cod_database_code               4109918