Di- and Tri-Cobalt Silicotungstates: Synthesis, Characterization, and Stability Studies
Guibo Zhu; Yurii V. Geletii; Jie Song; Chongchao Zhao; Elliot N. Glass; John Bacsa; Craig L. Hill; Inorganic Chemistry 52 (2013) 1018–1024; doi:10.1021/ic302279m

data_4333618
_publ_section_title
;
 Di- and Tri-Cobalt Silicotungstates: Synthesis, Characterization, and
 Stability Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1018
_journal_page_last               1024
_journal_paper_doi               10.1021/ic302279m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Co2 H12 Na3 O72 Si2 W18, K5, Na4, (H2O)37'
_chemical_formula_sum            'Co2 H86 K5 Na7 O109 Si2 W18'
_chemical_formula_weight         5670.37
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.166(5)
_cell_angle_beta                 87.147(6)
_cell_angle_gamma                81.561(6)
_cell_formula_units_Z            2
_cell_length_a                   12.846(5)
_cell_length_b                   18.671(7)
_cell_length_c                   20.889(7)
_cell_measurement_reflns_used    9788
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.70
_cell_measurement_theta_min      2.17
_cell_volume                     4632(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            94080
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    22.988
_exptl_absorpt_correction_T_max  0.1690
_exptl_absorpt_correction_T_min  0.1115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    3.760
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         12.199
_refine_diff_density_min         -7.053
_refine_diff_density_rms         0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         28073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+142.5901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                22316
_reflns_number_total             28073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302279m_si_002_1.cif
_cod_data_source_block           Co2Na3Si2W18
_cod_database_code               4333618