A Mixed-Valence VIV/VV Alkoxo-polyoxovanadium Cluster Series [V6O8(OCH3)11]n+/-: Exploring the Influence of a μ-Oxo Ligand in a Spin Frustrated Structure
Charles Daniel; Hans Hartl; Journal of the American Chemical Society 131 (2009) 5101–5114; doi:10.1021/ja8073648

data_4104153
_publ_section_title
;
 A Mixed-Valence VIV/VV Alkoxo-polyoxovanadium Cluster Series
 [V6O8(OCH3)11]n+/-: Exploring the Influence of a \m-Oxo Ligand in a Spin
 Frustrated Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5101
_journal_page_last               5114
_journal_paper_doi               10.1021/ja8073648
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         '(CH3O)11 V6O8'
_chemical_formula_sum            'C11 H33 O19 V6'
_chemical_formula_weight         775.01
_chemical_name_systematic
;
 undeca-methoxo-octa-oxo-hexavanadium 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.720(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1160(19)
_cell_length_b                   13.004(3)
_cell_length_c                   10.385(2)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.52
_cell_volume                     1353.7(5)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    DIAMOND
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans with 0.3 deg in omega'
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0101
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27410
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       SHELXL
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.0588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                3615
_reflns_number_total             4137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8073648_si_001.cif
_cod_data_source_block           onc
_cod_original_cell_volume        1353.8(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4104153