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_4333619
_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         'Co3 Na3 O66 Si2 W18 (H2O)7, K6, Na, (H2O)24'
_chemical_formula_sum            'Co3 H62 K6 Na4 O97 Si2 W18'
_chemical_formula_weight         5483.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.3640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3935(12)
_cell_length_b                   16.1715(15)
_cell_length_c                   20.3596(18)
_cell_measurement_reflns_used    5178
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.76
_cell_measurement_theta_min      2.44
_cell_volume                     4231.1(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1308
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            82692
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    25.390
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.4292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    4.164
_exptl_crystal_description       needle
_exptl_crystal_F_000             4635
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.860
_refine_diff_density_min         -3.256
_refine_diff_density_rms         0.598
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         13265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0462P)^2^+40.9220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                8727
_reflns_number_total             13265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302279m_si_002_2.cif
_cod_data_source_block           Co3NaSi2W18
_cod_database_code               4333619