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_4329029
_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          '(Ni (C16 H28 N4)) (Cl O4)2'
_chemical_formula_moiety         '(C16 H28 N4 Ni 2+), 2(Cl O4 1-)'
_chemical_formula_structural     '(Ni (C16 H28 N4)) (Cl O4)2'
_chemical_formula_sum            'C16 H28 Cl2 N4 Ni O8'
_chemical_formula_weight         534.03
_chemical_name_common            'Nickel macrocycle complex'
_chemical_name_systematic
;
N,N,N,N-{2,7,12-Trimethyl-3,7,11,17-tetraazabicyclo[11.3.1]heptadeca-
1(16),13(17),14-triene}nickel(II) Perchlorate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 98.308(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6611(1)
_cell_length_b                   10.2788(2)
_cell_length_c                   12.5195(2)
_cell_measurement_reflns_used    4219
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.38
_cell_volume                     1102.86(3)
_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)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w scans, 1290 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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10587
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.85614
_exptl_absorpt_correction_T_min  0.69131
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       Needle
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         2045
_refine_ls_number_restraints     1134
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+0.2959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                1656
_reflns_number_total             2045
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic202435r_si_002_2.cif
_cod_data_source_block           era001
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4329029