Chelate-Assisted Oxidative Coupling Reaction of Arylamides and Unactivated Alkenes: Mechanistic Evidence for Vinyl C-H Bond Activation Promoted by an Electrophilic Ruthenium-Hydride Catalyst.
Kwon, Ki-Hyeok; Lee, Do W.; Yi, Chae S.; Organometallics 29 (2010) 5748–5750; doi:10.1021/om100764c

data_4067002
_publ_section_title
;
 Chelate-Assisted Oxidative Coupling Reaction of Arylamides and
 Unactivated Alkenes: Mechanistic Evidence for Vinyl C-H Bond Activation
 Promoted by an Electrophilic Ruthenium-Hydride Catalyst.
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5748
_journal_page_last               5750
_journal_paper_doi               10.1021/om100764c
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C38 H55 B Cl2 F4 N O2 P Ru'
_chemical_formula_weight         847.58
_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                100.1596(12)
_cell_angle_beta                 102.3207(11)
_cell_angle_gamma                103.8371(12)
_cell_formula_units_Z            2
_cell_length_a                   10.23664(13)
_cell_length_b                   12.0713(2)
_cell_length_c                   16.7295(2)
_cell_measurement_reflns_used    59128
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.741
_cell_measurement_theta_min      3.3682
_cell_volume                     1903.84(5)
_computing_cell_refinement
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
 1 omega -57.00 25.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - 31.5067 0.0000 90.0000 82
 2 omega 24.00 108.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - 31.5067 37.0000 -90.0000 84
 3 omega 5.00 84.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - 31.5067 37.0000 60.0000 79
 4 omega 13.00 96.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - 31.5067 -140.0000 135.0000 83
 5 omega 6.00 86.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - 31.5067 77.0000 -180.0000 80
 6 omega -90.00 -29.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 129.0000 -128.0000 61
 7 omega 5.00 108.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - 31.5067 37.0000 150.0000 103
 8 omega -28.00 44.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 37.0000 30.0000 72
 9 omega -98.00 -32.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 140.0000 44.0000 66
 10 omega -111.00 2.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 -77.0000 -90.0000 113
 11 omega -28.00 44.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 37.0000 -120.0000 72
 12 omega -111.00 2.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 -77.0000 30.0000 113
 13 omega -28.00 44.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 37.0000 -150.0000 72
 14 omega -111.00 2.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 -77.0000 150.0000 113
 15 omega -98.00 -65.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 140.0000 -135.0000 33
 16 omega -28.00 44.00 1.0000 11.2200
 omega____ theta____ kappa____ phi______ frames
 - -31.8192 37.0000 -60.0000 72
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0121916
_diffrn_orient_matrix_UB_12      0.0273754
_diffrn_orient_matrix_UB_13      0.043129
_diffrn_orient_matrix_UB_21      -0.0202818
_diffrn_orient_matrix_UB_22      0.0484006
_diffrn_orient_matrix_UB_23      -0.0116185
_diffrn_orient_matrix_UB_31      -0.0701755
_diffrn_orient_matrix_UB_32      -0.0281672
_diffrn_orient_matrix_UB_33      -0.0017637
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            95037
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         37.83
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
 Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4281
_exptl_crystal_size_mid          0.2686
_exptl_crystal_size_min          0.1765
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         19744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                17207
_reflns_number_total             19744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100764c_si_002.cif
_cod_data_source_block           YI1W
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4067002