Ruthenium-Mediated C-H Functionalization of Pyridine: The Role of Vinylidene and Pyridylidene Ligands
David G. Johnson; Jason M. Lynam; Neetisha S. Mistry; John M. Slattery; Robert J. Thatcher; Adrian C. Whitwood; Journal of the American Chemical Society 135 (2013) 2222–2234; doi:10.1021/ja3097256

data_4119312
_publ_contact_author_address
;Department of Chemistry
University of York
Heslington
York
YO10 5DD
UK
;
_publ_contact_author_email       jason.lynam@york.ac.uk
_publ_contact_author_fax         +44(0)1904322516
_publ_contact_author_name        'Jason M Lynam'
_publ_contact_author_phone       +44(0)1904322534
_publ_section_title
;
 Ruthenium-Mediated C-H Functionalization of Pyridine: The Role of
 Vinylidene and Pyridylidene Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2222
_journal_page_last               2234
_journal_paper_doi               10.1021/ja3097256
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C33 H30 N2 P Ru, F6 P, C H2 Cl2'
_chemical_formula_sum            'C34 H32 Cl2 F6 N2 P2 Ru'
_chemical_formula_weight         816.53
_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                106.655(3)
_cell_angle_beta                 98.593(3)
_cell_angle_gamma                101.394(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2663(14)
_cell_length_b                   10.8938(17)
_cell_length_c                   18.206(3)
_cell_measurement_reflns_used    4704
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.30
_cell_volume                     1684.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17562
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10; (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8314
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0426P)^2^+0.1799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                6971
_reflns_number_total             8314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3097256_si_002_2.cif
_cod_data_source_block           '[6]PF6.CH2Cl2'
_cod_original_cell_volume        1684.0(4)
_cod_database_code               4119312