Elucidating the Protonation Site of Vanadium Peroxide Complexes and the Implications for Biomimetic Catalysis
Curtis J. Schneider; James E. Penner-Hahn; Vincent L. Pecoraro; Journal of the American Chemical Society 130 (2008) 2712–2713; doi:10.1021/ja077404c

data_4107479
_publ_section_title
;
 Elucidating the Protonation Site of Vanadium Peroxide Complexes and the
 Implications for Biomimetic Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2712
_journal_page_last               2713
_journal_paper_doi               10.1021/ja077404c
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C6 H9 N O7 V, H4 N'
_chemical_formula_sum            'C6 H13 N2 O7 V'
_chemical_formula_weight         276.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 109.437(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.340(6)
_cell_length_b                   7.644(2)
_cell_length_c                   14.309(4)
_cell_measurement_reflns_used    5230
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      23.33
_cell_measurement_theta_min      2.87
_cell_volume                     2098.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-1K'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42667
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.8297
_exptl_absorpt_correction_T_min  0.5937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  TWINABS  (Version 1.05), Bruker Nonius scaling and
  corrections for twinned crystals University of Gottingen, Germany 2003.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.020
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         7558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1413P)^2^+11.5124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2211
_reflns_number_gt                7081
_reflns_number_total             7558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077404c-file004.cif
_cod_data_source_block           cs4
_cod_database_code               4107479