Tuning the Reactivity of TEMPO by Coordination to a Lewis Acid: Isolation and Reactivity of MCl3(η1-TEMPO) (M = Fe, Al)
Jeremiah J. Scepaniak; Ashley M. Wright; Richard A. Lewis; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 134 (2012) 19350–19353; doi:10.1021/ja309499h

data_4118931
_publ_section_title
;
 Tuning the Reactivity of TEMPO by Coordination to a Lewis Acid: Isolation
 and Reactivity of MCl3(\h1-TEMPO) (M = Fe, Al)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19350
_journal_page_last               19353
_journal_paper_doi               10.1021/ja309499h
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C9 H19 Cl3 Fe N O'
_chemical_formula_weight         319.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5724(3)
_cell_length_b                   12.7487(3)
_cell_length_c                   9.3096(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1373.47(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23908
_diffrn_reflns_theta_full        33.29
_diffrn_reflns_theta_max         33.29
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.9217
_exptl_absorpt_correction_T_min  0.4912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.3473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                2513
_reflns_number_total             2748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309499h_si_001_3.cif
_cod_data_source_block           Complex_3
_cod_database_code               4118931