Synthesis of Pd Complexes Combined with Photosensitizing of a Ruthenium(II) Polypyridyl Moiety through a Series of Substituted Bipyrimidine Bridges. Substituent Effect of the Bridging Ligand on the Photocatalytic Dimerization of α-Methylstyrene
Akiko Inagaki; Shinichi Yatsuda; Shinichi Edure; Akiko Suzuki; Takeshi Takahashi; Munetaka Akita; Inorganic Chemistry 46 (2007) 2432–2445; doi:10.1021/ic0612909

data_4306942
_publ_contact_author_email       akiko_inagaki@res.titech.ac.jp
_publ_contact_author_fax         '+81 45 924 5230'
_publ_contact_author_name        'Akiko Inagaki'
_publ_contact_author_phone       '+81 45 924 5229'
_publ_section_title
;
Synthesis of Pd Complexes Combined with Photosensitizing of a Ruthenium(II)
Polypyridyl Moiety through a Series of Substituted Bipyrimidine Bridges.
Substituent Effect of the Bridging Ligand on the Photocatalytic
Dimerization of \a-Methylstyrene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2432
_journal_page_last               2445
_journal_paper_doi               10.1021/ic0612909
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C29 H24 B3 Br2 F12 N9 O2 Ru'
_chemical_formula_weight         1051.89
_chemical_name_systematic
; 
complex 3 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                63.27(3)
_cell_angle_beta                 89.01(3)
_cell_angle_gamma                83.05(3)
_cell_formula_units_Z            2
_cell_length_a                   10.872(8)
_cell_length_b                   13.654(11)
_cell_length_c                   14.259(11)
_cell_measurement_temperature    213(2)
_cell_volume                     1875(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'imaging plate area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode X-ray generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_sigmaI/netI    0.1351
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14367
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.653
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.381
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         7720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.290
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2387
_refine_ls_wR_factor_ref         0.2742
_reflns_number_gt                4147
_reflns_number_total             7720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0612909si20060713_085308.cif
_cod_data_source_block           string
_cod_database_code               4306942