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_4104154
_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 SbCl6 CH2Cl2'
_chemical_formula_sum            'C12 H35 Cl8 O19 Sb V6'
_chemical_formula_weight         1194.39
_chemical_name_systematic
;
 Dodeca-methoxo-hepta-oxo-hexa-vanadium-hexochloroantimonat
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.041(5)
_cell_angle_beta                 103.880(5)
_cell_angle_gamma                91.872(5)
_cell_formula_units_Z            2
_cell_length_a                   10.074(2)
_cell_length_b                   13.066(3)
_cell_length_c                   15.085(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      1.39
_cell_volume                     1926.5(7)
_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, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16279
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    2.701
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rodshaped
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.776
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0000(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   0.977
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                4444
_reflns_number_total             6777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8073648_si_002.cif
_cod_data_source_block           oncsbcl6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4104154