N-H Activation of Amines and Ammonia by Ru via Metal-Ligand Cooperation
Eugene Khaskin; Mark A. Iron; Linda J. W. Shimon; Jing Zhang; David Milstein; Journal of the American Chemical Society 132 (2010) 8542–8543; doi:10.1021/ja103130u

data_4102596
_publ_section_title
;
 N-H Activation of Amines and Ammonia by Ru via Metal-Ligand Cooperation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8542
_journal_page_last               8543
_journal_paper_doi               10.1021/ja103130u
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         '4(C30 H49 N3 O3 P2 Ru), 3(C4 H8 O)'
_chemical_formula_sum            'C132 H220 N12 O15 P8 Ru4'
_chemical_formula_weight         2867.24
_chemical_name_systematic
; 
 ? 
;
_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                 94.6278(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.2908(2)
_cell_length_b                   19.3330(2)
_cell_length_c                   22.0646(4)
_cell_measurement_reflns_used    14478
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     7776.96(18)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            49488
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_correction_T_min  0.9168
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.563
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         14683
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0704P)^2^+27.2023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                12064
_reflns_number_total             14683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103130u_si_001.cif
_cod_data_source_block           m1069a
_cod_database_code               4102596