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_4107021
_publ_contact_author_address     'Dept. of Chemistry, Stanford University'
_publ_contact_author_email       harverym@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         'C38 H54 N2 O10 Ru2, F6 Sb '
_chemical_formula_sum            'C38 H54 F6 N2 O10 Ru2 Sb'
_chemical_formula_weight         1136.72
_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                 97.5080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5171(3)
_cell_length_b                   12.5434(3)
_cell_length_c                   25.7609(5)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.22
_cell_volume                     4330.32(16)
_computing_cell_refinement       'Bruker SAINT v7.68A'
_computing_data_collection       'Bruker APEX-II v2010-7'
_computing_data_reduction        'Bruker SAINT v7.68A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_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 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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28726
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.9435
_exptl_absorpt_correction_T_min  0.8632
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             2276
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0190
_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^)+(0.0191P)^2^+8.1153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                4121
_reflns_number_total             4455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203576p_si_002.cif
_cod_data_source_block           su036a
_cod_database_code               4107021