A Diruthenium Catalyst for Selective, Intramolecular Allylic C-H Amination: Reaction Development and Mechanistic Insight Gained through Experiment and Theory
Mark Edwin Harvey; Djamaladdin G. Musaev; J. Du Bois; Journal of the American Chemical Society 133 (2011) 17207–17216; doi:10.1021/ja203576p

data_4107022
_publ_contact_author_address     'Dept. of Chemistry, Stanford Univeristy'
_publ_contact_author_email       harveym@stanford.edu
_publ_contact_author_name        'Mark Harvey'
_publ_contact_author_phone       '+1 650 724 4558'
_publ_section_title
;
 A Diruthenium Catalyst for Selective, Intramolecular Allylic C-H
 Amination: Reaction Development and Mechanistic Insight Gained through
 Experiment and Theory
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17207
_journal_page_last               17216
_journal_paper_doi               10.1021/ja203576p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C23 H23 Cl N5 O5 Ru2'
_chemical_formula_sum            'C23 H23 Cl N5 O5 Ru2'
_chemical_formula_weight         687.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.915(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.1203(10)
_cell_length_b                   10.6090(3)
_cell_length_c                   14.8811(5)
_cell_measurement_reflns_used    9108
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.68
_cell_measurement_theta_min      2.37
_cell_volume                     4825.1(3)
_computing_cell_refinement       'Bruker SAINT v7.66A'
_computing_data_collection       'Bruker APEX-II v2009-9'
_computing_data_reduction        'Bruker SAINT v7.66A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74094
_diffrn_reflns_theta_full        35.12
_diffrn_reflns_theta_max         35.12
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.6869
_exptl_absorpt_correction_T_min  0.5721
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.376
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.118
_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     327
_refine_ls_number_reflns         10597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+7.0304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                8910
_reflns_number_total             10597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203576p_si_003.cif
_cod_data_source_block           su031a
_cod_database_code               4107022