Ruthenium Induced C-N Bond Activation of an N-Heterocyclic Carbene: Isolation of C- and N-Bound Tautomers
Suzanne Burling; Mary F. Mahon; Rachael E. Powell; Michael K. Whittlesey; Jonathan M. J. Williams; Journal of the American Chemical Society 128 (2006) 13702–13703; doi:10.1021/ja065582k

data_4111014
_publ_section_title
;
 Ruthenium Induced C-N Bond Activation of an N-Heterocyclic Carbene:
 Isolation of C- and N-Bound Tautomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13702
_journal_page_last               13703
_journal_paper_doi               10.1021/ja065582k
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C46 H46 Cl4 N2 O P2 Ru'
_chemical_formula_weight         947.66
_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                 114.462(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9960(1)
_cell_length_b                   27.7130(2)
_cell_length_c                   14.4600(1)
_cell_measurement_reflns_used    83946
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     4375.65(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  kappaCCD
_diffrn_measurement_method       kappaCCD
_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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            79030
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         3.70
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       tabloid
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         12745
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+4.0511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                9686
_reflns_number_total             12745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065582ksi20060920_075008.cif
_cod_data_source_block           c:\x-ray\kappa\k06mkw2\maxus\k06mkw2
_cod_original_cell_volume        4375.65(6)
_cod_database_code               4111014