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_4065484
_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         'C44 H39 Cl2 P Ru, C H Cl3'
_chemical_formula_sum            'C45 H40 Cl5 P Ru'
_chemical_formula_weight         890.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.285(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3714(4)
_cell_length_b                   15.9421(4)
_cell_length_c                   19.4262(5)
_cell_measurement_reflns_used    10444
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.4781
_cell_measurement_theta_min      2.9661
_cell_volume                     4013.0(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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 0.979
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24621
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.9247
_exptl_absorpt_correction_T_min  0.8320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Wed Nov 24 12:31:49 2010'
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8516
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                5912
_reflns_number_total             8516
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200843f_si_002.cif
_cod_data_source_block           sd303_(compound_9)
_cod_original_cell_volume        4013.01(19)
_cod_database_code               4065484