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_4333620
_publ_contact_author_name
;
;
_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         'K11[Co2(H2O)8 K Si2 W18 O66].17(H2O)'
_chemical_formula_sum            'Co2 H50 K12 O91 Si2 W18'
_chemical_formula_weight         5458.94
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-02
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Sep 14 2012 15:46:11, GUI svn.r4346)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.8800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2891(3)
_cell_length_b                   23.5596(5)
_cell_length_c                   30.7185(7)
_cell_measurement_reflns_used    9004
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      40.247
_cell_measurement_theta_min      2.446
_cell_volume                     8847.0(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            160685
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.371
_exptl_absorpt_correction_T_max  0.0249
_exptl_absorpt_correction_T_min  0.0017
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0834 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.0683.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    4.098
_exptl_crystal_description       needle
_exptl_crystal_F_000             9680
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         6.087
_refine_diff_density_min         -3.296
_refine_diff_density_rms         0.407
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         28156
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+266.7097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                23948
_reflns_number_total             28156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302279m_si_002_3.cif
_cod_data_source_block           KCo2Si2W18
_cod_database_code               4333620
_shelx_res_file_md5              f60ddea27637b9d9703ff1df429e7aad