Two-Step Binding of O2 to a Vanadium(III) Trisanilide Complex To Form a Non-Vanadyl Vanadium(V) Peroxo Complex
Anthony F. Cozzolino; Daniel Tofan; Christopher C. Cummins; Manuel Temprado; Taryn D. Palluccio; Elena V. Rybak-Akimova; Subhojit Majumdar; Xiaochen Cai; Burjor Captain; Carl D. Hoff; Journal of the American Chemical Society 134 (2012) 18249–18252; doi:10.1021/ja309621h

data_4118875
_publ_contact_author_address
;
Department of Chemistry, Massachusetts Institute of Technology, 
77 Massachusetts Avenue, Cambridge, Massachusetts 02139, 
United States
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 Two-Step Binding of O2 to a Vanadium(III) Trisanilide Complex To Form a
 Non-Vanadyl Vanadium(V) Peroxo Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18249
_journal_page_last               18252
_journal_paper_doi               10.1021/ja309621h
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C36 H54 N3 O2 V'
_chemical_formula_sum            'C36 H54 N3 O2 V'
_chemical_formula_weight         611.76
_chemical_name_common
tris(3,5-dimethylphenyl(tertbutyl)amido)-(eta-2-peroxo)-vanadium
_chemical_name_systematic
tris(3,5-dimethylphenyl(tertbutyl)amido)-(eta-2-peroxo)-vanadium
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      220
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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            16
_cell_length_a                   23.919(2)
_cell_length_b                   23.919(2)
_cell_length_c                   23.919(2)
_cell_measurement_reflns_used    9352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.398
_cell_measurement_theta_min      2.408
_cell_volume                     13685(2)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_molecular_graphics    'WINGX (Farrugia, 1999)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            151622
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_correction_T_min  0.9380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             5280
_exptl_crystal_recrystallization_method pentane
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
'Flack H D (1983), 1576 Friedel pairs Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3356
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+6.0216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                3066
_reflns_number_total             3356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309621h_si_001.cif
_cod_data_source_block           O2VX3_Cmp_3
_cod_database_code               4118875