Ligand-Promoted Carbene Insertion into the Aryl Substituent of an N-Heterocyclic Carbene Ligand in Ruthenium-Based Metathesis Catalysts
Brandon R. Galan; Mateusz Pitak; Milan Gembicky; Jerome B. Keister; Steven T. Diver; Journal of the American Chemical Society 131 (2009) 6822–6832; doi:10.1021/ja809984k

data_4104377
_publ_contact_author_address
;
Department of Chemistry
State University of New York at Buffalo
Buffalo, NY
14260-3000, USA
;
_publ_contact_author_email       mpitak@buffalo.edu
_publ_contact_author_name        'Mateusz Pitak'
_publ_contact_author_phone       (716)645-6800x2235
_publ_section_title
;
 Ligand-Promoted Carbene Insertion into the Aryl Substituent of an
 N-Heterocyclic Carbene Ligand in Ruthenium-Based Metathesis Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6822
_journal_page_last               6832
_journal_paper_doi               10.1021/ja809984k
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C52 H50 Cl5 N5 O Ru, C6 H6'
_chemical_formula_sum            'C58 H56 Cl5 N5 O Ru'
_chemical_formula_weight         1117.40
_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                117.3980(10)
_cell_angle_beta                 112.8420(10)
_cell_angle_gamma                90.063(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4404(7)
_cell_length_b                   15.3105(8)
_cell_length_c                   16.4038(9)
_cell_measurement_reflns_used    8834
_cell_measurement_temperature    90(1)
_cell_measurement_theta_max      21.25
_cell_measurement_theta_min      2.51
_cell_volume                     2694.4(3)
_computing_cell_refinement       'Bruker Saint v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'Bruker Saint v7.23A (Bruker, 2005)'
_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      90(1)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34122
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.55
_diffrn_source_type              'RIGAKU RU-2000BEH'
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.8972
_exptl_absorpt_correction_T_min  0.8823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2004/1; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.297
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         10220
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0859P)^2^+5.7360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1677
_reflns_number_gt                7381
_reflns_number_total             10220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809984k_si_006.cif
_cod_data_source_block           C58H56Cl5N5ORu
_cod_original_cell_volume        2694.4(2)
_cod_database_code               4104377