Gas-Phase C-H and N-H Bond Activation by a High Valent Nitrido-Iron Dication and NH-Transfer to Activated Olefins
Maria Schlangen; Johannes Neugebauer; Markus Reiher; Detlef Schröder; Jesús Pitarch López; Marco Haryono; Frank W. Heinemann; Andreas Grohmann; Helmut Schwarz; Journal of the American Chemical Society 130 (2008) 4285–4294; doi:10.1021/ja075617w

data_4107608
_publ_contact_author
;                                                    
        Prof. Dr. A. GROHMANN
        Technische Universit\"at Berlin
        Fakult\"at II       
        Institut f\"ur Chemie, Sekr. C2
        Str. des 17. Juni 135
        D-10623 Berlin
        Bundesrepublik Deutschland                             
;
_publ_contact_author_email       andreas.grohmann@chem.tu-berlin.de
_publ_contact_author_fax         '049 30 314 22168'
_publ_contact_author_phone       '049 30 314 79877'
_publ_section_title
;
 Gas-Phase C-H and N-H Bond Activation by a High Valent Nitrido-Iron
 Dication and NH-Transfer to Activated Olefins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4285
_journal_page_last               4294
_journal_paper_doi               10.1021/ja075617w
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C13 H25 Fe N8, F6 P, H2 O, Br'
_chemical_formula_sum            'C13 H27 Br F6 Fe N8 O P'
_chemical_formula_weight         592.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom except water bound hydrogens difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.476(2)
_cell_angle_beta                 85.090(2)
_cell_angle_gamma                89.894(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6579(2)
_cell_length_b                   10.7787(2)
_cell_length_c                   13.3012(3)
_cell_measurement_reflns_used    162
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     1053.72(4)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
; 
 \w-scans with 2.0 \% and 20 sec per frame
;
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22821
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    2.764
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_description       block
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0417P)^2^+1.4783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                4193
_reflns_number_total             5229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075617w-file002.cif
_cod_data_source_block           jp0206
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4107608