Synthesis, Structure Characterization, and Reversible Transformation of a Cobalt Salt of a Dilacunary γ-Keggin Silicotungstate and Sandwich-Type Di- and Tetracobalt-Containing Silicotungstate Dimers
Yuji Kikukawa; Kosuke Suzuki; Kazuya Yamaguchi; Noritaka Mizuno; Inorganic Chemistry 52 (2013) 8644–8652; doi:10.1021/ic4008075

data_4335548
_publ_contact_author_address
;
Department of Applied Chemistry
School of Engineering
the University of Tokyo
7-3-1 Hongo, Bunkyoku
Tokyo, JAPAN
;
_publ_contact_author_email       tmizuno@mail.ecc.u-tokyo.ac.jp
_publ_contact_author_fax         81-3-5841-7220
_publ_contact_author_name        'Noritaka Mizuno'
_publ_contact_author_phone       81-3-5841-7272
_publ_section_title
;
 Synthesis, Structure Characterization, and Reversible Transformation of a
 Cobalt Salt of a Dilacunary \g-Keggin Silicotungstate and Sandwich-Type
 Di- and Tetracobalt-Containing Silicotungstate Dimers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8644
_journal_page_last               8652
_journal_paper_doi               10.1021/ic4008075
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C196 Co4 N16 O152 Si4 W40'
_chemical_formula_sum            'C196 Co4 N16 O152 Si4 W40'
_chemical_formula_weight         12712.2
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2013-02-26T13:07:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.9830(10)
_cell_angle_beta                 97.0030(10)
_cell_angle_gamma                96.09
_cell_formula_units_Z            2
_cell_length_a                   24.29700(10)
_cell_length_b                   25.1429(2)
_cell_length_c                   27.2971(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    123
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     16214.6(2)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.926
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            84219
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    14.416
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.604
_exptl_crystal_description       prism
_exptl_crystal_F_000             11256
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         10.781
_refine_diff_density_min         -4.604
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2115
_refine_ls_number_reflns         84219
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+549.4132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1516
_reflns_number_gt                67398
_reflns_number_total             84219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4008075_si_001_3.cif
_cod_data_source_block           Co2
_cod_original_cell_volume        16214.75(19)
_cod_database_code               4335548