EPR study of the magnetic states of mixed-valence VIV4 - VV2 alkoxypolyoxovanadium cluster
Yurii, Yablokov; Maria A. Augustyniak-Jablokow; .; Serguei Borshch; .; Daniel, Charles; Hartl, Hans; New J.Chem.(Nouv.J.Chim.) 29 (2005) 1064–; doi:10.1039/b412427h

data_7050041
_publ_section_title
;
EPR study of the magnetic states of mixed-valence
VIV4 - VV2 alkoxypolyoxovanadium cluster
;
_journal_issue                   8
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'
_journal_page_first              1064
_journal_paper_doi               10.1039/b412427h
_journal_volume                  29
_journal_year                    2005
_chemical_formula_sum            'C12 H36 O19 V6'
_chemical_formula_weight         790.05
_chemical_name_systematic
;
\m6-oxo-dodeca-\m-methoxo-hexakis(oxovanadium)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8343(12)
_cell_length_b                   10.0830(6)
_cell_length_c                   13.5064(8)
_cell_measurement_reflns_used    7344
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.462
_cell_measurement_theta_min      4.938
_cell_volume                     2837.3(3)
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32332
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  '20 sec / frame'
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    1.971
_exptl_absorpt_correction_T_max  0.647652
_exptl_absorpt_correction_T_min  0.413253
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.483(14)
_refine_ls_extinction_coef       0.00000(5)
_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   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          3.431
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                7402
_reflns_number_total             8265
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               7050041