Ruthenium Complexes of κ(P)- and κ(P)-η6-Coordinated KITPHOS Monophosphines: Efficient Catalysts for the Direct Ortho Arylation of 2-Phenylpyridine andN-Phenylpyrazole with Aryl Chlorides
Doherty, Simon; Knight, Julian G.; Addyman, Carrie R.; Smyth, Catherine H.; Ward, Nicholas A. B.; Harrington, Ross W.; Organometallics 30 (2011) 6010–; doi:10.1021/om200843f

data_4065486
_publ_section_title
;
 Ruthenium Complexes of \k(P)- and \k(P)-\h6-Coordinated KITPHOS
 Monophosphines: Efficient Catalysts for the Direct Ortho Arylation of
 2-Phenylpyridine andN-Phenylpyrazole with Aryl Chlorides
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6010
_journal_paper_doi               10.1021/om200843f
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C38 H35 Cl2 P Ru'
_chemical_formula_sum            'C38 H35 Cl2 P Ru'
_chemical_formula_weight         694.60
_chemical_name_systematic
;
 ?
;
_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                81.524(5)
_cell_angle_beta                 79.600(4)
_cell_angle_gamma                89.921(4)
_cell_formula_units_Z            4
_cell_length_a                   12.1151(5)
_cell_length_b                   13.6674(7)
_cell_length_c                   20.0357(13)
_cell_measurement_reflns_used    6319
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.6008
_cell_measurement_theta_min      2.2656
_cell_volume                     3226.3(3)
_computing_cell_refinement
;
'Thu Sep 01 13:31:17 2011'
;
_computing_data_collection
;
'Thu Sep 01 13:31:17 2011'
;
_computing_data_reduction
;
'Thu Sep 01 13:31:17 2011'
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'sealed tube with Enhance Ultra optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19146
_diffrn_reflns_theta_full        62.69
_diffrn_reflns_theta_max         62.69
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    6.112
_exptl_absorpt_correction_T_max  0.8875
_exptl_absorpt_correction_T_min  0.5801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Thu Sep 01 13:31:17 2011'
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.594
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         10025
_refine_ls_number_restraints     680
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0870P)^2^+9.5235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                7848
_reflns_number_total             10025
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200843f_si_002.cif
_cod_data_source_block           sd309_compound_13
_cod_database_code               4065486