Mechanism of Catalytic Aziridination with Manganese Corrole: The Often Postulated High-Valent Mn(V) Imido Is Not the Group Transfer Reagent
Michael J. Zdilla; Mahdi M. Abu-Omar; Journal of the American Chemical Society 128 (2006) 16971–16979; doi:10.1021/ja0665489

data_4111293
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfanwick@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Phillip E. Fanwick'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Mechanism of Catalytic Aziridination with Manganese Corrole: The Often
 Postulated High-Valent Mn(V) Imido Is Not the Group Transfer Reagent
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16971
_journal_page_last               16979
_journal_paper_doi               10.1021/ja0665489
_journal_volume                  128
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H16 F15 Mn1 N4 O2,C4 H8 O2'
_chemical_formula_structural     '(Mn +2) (C37 H8 F15 N4 -3) (C4 H8 O2)2'
_chemical_formula_sum            'C45 H24 F15 Mn N4 O4'
_chemical_formula_weight         1024.63
_chemical_name_systematic
; 
Manganese(III) 5,10,15-tris(pentafluorophenyl)corrole 
Ethyl Acetate, Ethyl Acetate solvate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             1-03-06
_audit_creation_method           SHELXL_and_local_programs
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.103(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8543(4)
_cell_length_b                   38.0136(15)
_cell_length_c                   7.4550(2)
_cell_measurement_reflns_used    21357
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     4064.2(2)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 1997)
    XP (Sheldrick, 1997)
;
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    direct_methods_(SIR2004,_Burla_et_al.,_2005)
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9909
_diffrn_measured_fraction_theta_max 0.9909
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.273
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            21357
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.9788
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_type   multi-scan_(Otwinowski_&_Minor,_1997)
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       needle
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_d_res_high            0.841
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         6321
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.060
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0071P)^2^+15.3405P] where P=(Fo^2^+2Fc^2^)/3 '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.105
_refine_ls_wR_factor_ref         0.108
_reflns_Friedel_coverage         1.0000
_reflns_number_gt                5724
_reflns_number_total             6321
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ja0665489si20061022_083609.cif
_cod_data_source_block           MZ120B
_cod_original_formula_sum        'C45 H24 F15 Mn1 N4 O4'
_cod_database_code               4111293