Aryl C-H Amination by Diruthenium Nitrides in the Solid State and in Solution at Room Temperature: Experimental and Computational Study of the Reaction Mechanism
Amanda Kae Musch Long; George H. Timmer; József S. Pap; Jamie Lynn Snyder; Renyuan Pony Yu; John F. Berry; Journal of the American Chemical Society 133 (2011) 13138–13150; doi:10.1021/ja203993p

data_4106601
_publ_contact_author_address
;Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John Ferguson Berry'
_publ_contact_author_phone       809-608-262-7534
_publ_section_title
;
 Aryl C-H Amination by Diruthenium Nitrides in the Solid State and in
 Solution at Room Temperature: Experimental and Computational Study of the
 Reaction Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13138
_journal_page_last               13150
_journal_paper_doi               10.1021/ja203993p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         Ru2(C13H7N2Cl4)3NH(C13H6N2Cl4)(C6H14)
_chemical_formula_sum            'C58 H42 Cl16 N9 Ru2'
_chemical_formula_weight         1634.35
_chemical_name_common            Ru2(D(3,5-Cl2)PhF)3NH(C13H6N2Cl4)(Hexane)
_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
_audit_update_record
;
2010-05-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.191(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.6125(9)
_cell_length_b                   12.1901(4)
_cell_length_c                   21.7234(7)
_cell_measurement_reflns_used    9379
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1259
_cell_measurement_theta_min      2.8120
_cell_volume                     6801.0(4)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'microfocus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            77230
_diffrn_reflns_theta_full        29.20
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.9577
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             3252
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.983
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         9186
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0633P)^2^+42.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                8152
_reflns_number_total             9186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203993p_si_001.cif
_cod_data_source_block           berry126
_cod_database_code               4106601