A Unique Dinuclear Mixed V(V) Oxo-peroxo Complex in the Structural Speciation of the Ternary V(V)-Peroxo-citrate System. Potential Mechanistic and Structural Insight into the Aqueous Synthetic Chemistry of Dinuclear V(V)-Citrate Species with H2O2
M. Kaliva; C. Gabriel; C. P. Raptopoulou; A. Terzis; G. Voyiatzis; M. Zervou; C. Mateescu; A. Salifoglou; Inorganic Chemistry 50 (2011) 11423–11436; doi:10.1021/ic201204s

data_4326845
_publ_section_title
;
 A Unique Dinuclear Mixed V(V) Oxo-peroxo Complex in the Structural
 Speciation of the Ternary V(V)-Peroxo-citrate System. Potential
 Mechanistic and Structural Insight into the Aqueous Synthetic Chemistry
 of Dinuclear V(V)-Citrate Species with H2O2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11423
_journal_page_last               11436
_journal_paper_doi               10.1021/ic201204s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C12 H29 N4 O20.5 V2'
_chemical_formula_weight         659.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 95.193(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.833(8)
_cell_length_b                   9.235(4)
_cell_length_c                   25.678(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.0
_cell_measurement_theta_min      5.5
_cell_volume                     4920(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       '\q/2\q 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  0.0117
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4443
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0420P)^2^+13.9441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                3783
_reflns_number_total             4331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201204s_si_002.cif
_cod_data_source_block           salv184
_cod_original_formula_sum        'C12 H29 N4 O20.50 V2'
_cod_database_code               4326845