Structure and Bonding of the Vanadium(III) Hexa-Aqua Cation. 1. Experimental Characterization and Ligand-Field Analysis
Philip L.W. Tregenna-Piggott; David Spichiger; Graham Carver; Beatrice Frey; Roland Meier; Høgni Weihe; John A. Cowan; Garry J. McIntyre; Gernot Zahn; Anne-Laure Barra; Inorganic Chemistry 43 (2004) 8049–8060; doi:10.1021/ic049292l

data_4312179
_publ_contact_author
;
Philip L.W. Tregenna-Piggott
Department of Chemistry and Biochemistry
University of Bern 
Freiestrasse 3 
CH-3000 Bern 9
Switzerland
;
_publ_contact_author_email       tregenna@iac.unibe.ch
_publ_contact_author_fax         '+41 31 631 4322'
_publ_contact_author_phone       '+41 31 631 4317'
_publ_section_title
;
 Structure and Bonding of the Vanadium(III) Hexa-Aqua Cation. 1.
 Experimental Characterization and Ligand-Field Analysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8049
_journal_page_last               8060
_journal_paper_doi               10.1021/ic049292l
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C H18 N3 O14 S2 V'
_chemical_formula_weight         411.24
_chemical_name_systematic
; 
Guanidinium Hexaaqua Vanadium Disulphate 
;
_space_group_IT_number           157
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2'
_symmetry_space_group_name_H-M   'P 3 1 m'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.8116(4)
_cell_length_b                   11.8116(4)
_cell_length_c                   9.0311(3)
_cell_measurement_reflns_used    9521
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      33.73
_cell_measurement_theta_min      1.99
_cell_volume                     1091.16(6)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-7 with Mercury CCD'
_diffrn_measurement_method       oscillation
_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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0139
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15473
_diffrn_reflns_theta_full        30.98
_diffrn_reflns_theta_max         30.98
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7687
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_coef       0.016(2)
_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   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2487
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                2444
_reflns_number_total             2487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049292lsi20040531_020941.cif
_cod_data_source_block           ghvs
_cod_database_code               4312179