Role of Fe(IV)-Oxo Intermediates in Stoichiometric and Catalytic Oxidations Mediated by Iron Pyridine-Azamacrocycles
Wanhua Ye; Douglas M. Ho; Simone Friedle; Taryn D. Palluccio; Elena V. Rybak-Akimova; Inorganic Chemistry 51 (2012) 5006–5021; doi:10.1021/ic202435r

data_4329028
_publ_contact_author_address
;
Department of Chemistry
Tufts University
Medford MA 02155
USA
;
_publ_contact_author_email       erybakak@tufts.edu
_publ_contact_author_fax         617-627-3443
_publ_contact_author_name
;
Rybak-Akimova, Elena V. 
;
_publ_contact_author_phone       617-627-3413
_publ_section_title
;
 Role of Fe(IV)-Oxo Intermediates in Stoichiometric and Catalytic
 Oxidations Mediated by Iron Pyridine-Azamacrocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5006
_journal_page_last               5021
_journal_paper_doi               10.1021/ic202435r
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'chemical synthesis'
_chemical_formula_iupac
;
(Fe (C2 H3 N)2 (C16 H28 N4)) (C F3 O3 S)2
;
_chemical_formula_moiety         'C20 H34 Fe N6 2+, 2(C F3 O3 S 1-)'
_chemical_formula_structural
;
(Fe (C2 H3 N)2 (C16 H28 N4)) (C F3 O3 S)2
;
_chemical_formula_sum            'C22 H34 F6 Fe N6 O6 S2'
_chemical_formula_weight         712.52
_chemical_name_common            WH60
_chemical_name_systematic
; 
Bis(Acetonitrile)(2,7,12-trimethyl-3,7,11,17-tetraaza-
bicyclo[11.3.1]heptadeca-1(17),13,15-triene)iron(II) Triflate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 100.968(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4722(6)
_cell_length_b                   14.1244(5)
_cell_length_c                   13.3541(5)
_cell_measurement_reflns_used    1845
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      17.50
_cell_measurement_theta_min      2.52
_cell_volume                     3050.21(19)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006b)'
_computing_data_collection       'APEX2 v2.1-0 (Bruker AXS, 2006a)'
_computing_data_reduction
;
SAINT V7.34A (Bruker AXS, 2006b), SADABS (Bruker AXS, 2004)
;
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXTL v6.12 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w scans, 861 0.5\% rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18820
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.8703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         5365
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+3.0881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                3164
_reflns_number_total             5365
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic202435r_si_002_1.cif
_cod_data_source_block           era08001
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329028