Slow Hydrogen Atom Transfer Reactions of Oxo- and Hydroxo-Vanadium Compounds: The Importance of Intrinsic Barriers
Christopher R. Waidmann; Xin Zhou; Erin A. Tsai; Werner Kaminsky; David A. Hrovat; Weston Thatcher Borden; James M. Mayer; Journal of the American Chemical Society 131 (2009) 4729–4743; doi:10.1021/ja808698x

data_4104116
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       wernerka@u.washington.edu
_publ_contact_author_name        'Werner Kaminsky'
_publ_section_title
;
 Slow Hydrogen Atom Transfer Reactions of Oxo- and Hydroxo-Vanadium
 Compounds: The Importance of Intrinsic Barriers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4729
_journal_page_last               4743
_journal_paper_doi               10.1021/ja808698x
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C20 H16 N4 O2 V, B F4'
_chemical_formula_sum            'C20 H16 B F4 N4 O2 V'
_chemical_formula_weight         482.12
_chemical_name_common            etsai1
_chemical_name_systematic        etsai1
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.3310(11)
_cell_angle_beta                 100.9180(11)
_cell_angle_gamma                94.6080(14)
_cell_formula_units_Z            2
_cell_length_a                   8.0920(2)
_cell_length_b                   9.3510(3)
_cell_length_c                   13.3910(4)
_cell_measurement_reflns_used    304
_cell_measurement_temperature    130(2)
_cell_volume                     983.53(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7668
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.8756
_exptl_absorpt_correction_T_min  0.7799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.072
_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     289
_refine_ls_number_reflns         4700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.3006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                3704
_reflns_number_total             4700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808698x_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4104116