[V16O38(CN)]9-: A Soluble Mixed-Valence Redox-Active Building Block with Strong Antiferromagnetic Coupling
Tony D. Keene; Deanna M. D'Alessandro; Karl W. Krämer; Jason R. Price; David J. Price; Silvio Decurtins; Cameron J. Kepert; Inorganic Chemistry 51 (2012) 9192–9199; doi:10.1021/ic3001834

data_4330142
_publ_section_title
;
 [V16O38(CN)]9-: A Soluble Mixed-Valence Redox-Active Building Block with
 Strong Antiferromagnetic Coupling
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9192
_journal_page_last               9199
_journal_paper_doi               10.1021/ic3001834
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'O38 V16, O2, C N, 11(O), 9(K)'
_chemical_formula_sum            'C K9 N O51 V16'
_chemical_formula_weight         2008.96
_chemical_name_common            K9[V16O38(CN)].13(H2O)
_chemical_name_systematic
;
 K9[V16O38(CN)].13(H2O)
;
_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   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.978(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3351(9)
_cell_length_b                   20.1302(16)
_cell_length_c                   22.5130(16)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.089
_cell_measurement_theta_min      5.422
_cell_volume                     5117.6(7)
_computing_cell_refinement       'SAINT Ver. 7.60A  (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2009.3-0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.60A'
_computing_molecular_graphics    'Diamond 3.2g (Crystal Impact, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius FR591 Kappa APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61311
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.622
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.090
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         9012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+54.4326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                7877
_reflns_number_total             9012
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3001834_si_002.cif
_cod_data_source_block           09tdks01
_cod_database_code               4330142