A Coordination Chemistry Study of Hydrated and Solvated Cationic Vanadium Ions in Oxidation States +III, +IV, and +V in Solution and Solid State
Joanna Krakowiak; Daniel Lundberg; Ingmar Persson; Inorganic Chemistry 51 (2012) 9598–9609; doi:10.1021/ic300202f

data_4330289
_publ_contact_author_address
;Department of Chemistry
Uppsala Biocenter
P.O. Box 7015
Swedish University of Agricultural Sciences
SE-750 07 Uppsala
SWEDEN
;
_publ_contact_author_email       daniel.lundberg@kemi.slu.se
_publ_contact_author_name        'Daniel Lundberg'
_publ_contact_author_phone       +46-18-671549
_publ_section_title
;
 A Coordination Chemistry Study of Hydrated and Solvated Cationic Vanadium
 Ions in Oxidation States +III, +IV, and +V in Solution and Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9598
_journal_page_last               9609
_journal_paper_doi               10.1021/ic300202f
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        synthesized
_chemical_formula_moiety         '2(C F3 O3 S), H10 O6 V'
_chemical_formula_sum            'C2 H10 F6 O12 S2 V'
_chemical_formula_weight         455.16
_chemical_name_common            'pentaaquaoxovanadium(IV) triflate'
_chemical_name_systematic
'pentaaquaoxovanadium(IV) trifluoromethanesulfonate'
_chemical_properties_physical    hygroscopic
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 102.555(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7598(11)
_cell_length_b                   7.8650(9)
_cell_length_c                   10.2154(11)
_cell_measurement_reflns_used    4904
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      2.97
_cell_volume                     765.39(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 2.0'
_computing_publication_material  'Diamond 2.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4087
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX-II'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_description       block
_exptl_crystal_F_000             454
_exptl_crystal_recrystallization_method 'from saturated aqueous solution'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.086(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1561
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                1275
_reflns_number_total             1561
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300202f_si_002_2.cif
_cod_data_source_block           voaqm
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4330289