Thermodynamic and Kinetic Study of Cleavage of the N-O Bond of N-Oxides by a Vanadium(III) Complex: Enhanced Oxygen Atom Transfer Reaction Rates for Adducts of Nitrous Oxide and Mesityl Nitrile Oxide
Taryn D. Palluccio; Elena V. Rybak-Akimova; Subhojit Majumdar; Xiaochen Cai; Megan Chui; Manuel Temprado; Jared S. Silvia; Anthony F. Cozzolino; Daniel Tofan; Alexandra Velian; Christopher C. Cummins; Burjor Captain; Carl D. Hoff; Journal of the American Chemical Society 135 (2013) 11357–11372; doi:10.1021/ja405395z

data_4120219
_publ_section_title
;
 Thermodynamic and Kinetic Study of Cleavage of the N-O Bond of N-Oxides
 by a Vanadium(III) Complex: Enhanced Oxygen Atom Transfer Reaction Rates
 for Adducts of Nitrous Oxide and Mesityl Nitrile Oxide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11357
_journal_page_last               11372
_journal_paper_doi               10.1021/ja405395z
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C36 H54 N3 O V'
_chemical_formula_weight         595.76
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_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                   24.0912(9)
_cell_length_b                   24.0912(9)
_cell_length_c                   24.0912(9)
_cell_measurement_reflns_used    6521
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.76
_cell_measurement_theta_min      2.39
_cell_volume                     13982.2(9)
_computing_cell_refinement       'SAINT+  V7.46A (Bruker, 2007)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2007)'
_computing_data_reduction        'SAINT+  V7.46A (Bruker, 2007)'
_computing_molecular_graphics    'XSHELL v4.02 (Bruker, 2000)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29806
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/4 Bruker)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       Block
_exptl_crystal_F_000             5152
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+1.6405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                2304
_reflns_number_total             2775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405395z_si_002.cif
_cod_data_source_block           collect_0m
_cod_database_code               4120219