Activation of Nitriles by Metal Ligand Cooperation. Reversible Formation of Ketimido- and Enamido-Rhenium PNP Pincer Complexes and Relevance to Catalytic Design
Matthias Vogt; Alexander Nerush; Mark A. Iron; Gregory Leitus; Yael Diskin-Posner; Linda J. W. Shimon; Yehoshoa Ben-David; David Milstein; Journal of the American Chemical Society 135 (2013) 17004–17018; doi:10.1021/ja4071859

data_4121113
_publ_section_title
;
 Activation of Nitriles by Metal Ligand Cooperation. Reversible Formation
 of Ketimido- and Enamido-Rhenium PNP Pincer Complexes and Relevance to
 Catalytic Design
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17004
_journal_page_last               17018
_journal_paper_doi               10.1021/ja4071859
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C34 H49 F3 N2 O2 P2 Re, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C36 H51 Cl2 F6 N2 O5 P2 Re S'
_chemical_formula_weight         1056.89
_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                 94.6930(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.75800(10)
_cell_length_b                   9.28100(10)
_cell_length_c                   35.6750(4)
_cell_measurement_reflns_used    68980
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     4210.01(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.112
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            41887
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    3.208
_exptl_absorpt_correction_T_max  0.5663
_exptl_absorpt_correction_T_min  0.3602
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Numabs, Higashi 1999'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         5.936
_refine_diff_density_min         -2.680
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+6.4086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                6447
_reflns_number_total             7671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4071859_si_001_7.cif
_cod_data_source_block           complex10
_cod_database_code               4121113