K~6~H~2~[TiW~11~CoO~40~].13H~2~O, with a monotitanoundecatungstocobaltate(II) anion
Werner Kraus; Holger Stephan; Anita Röllich; Zdenek Matĕjka; Günter Reck; Acta Crystallographica, Section E 61 (2005) i35–i37; doi:10.1107/S1600536805005180

data_2205377
_publ_section_title
;
K~6~H~2~[TiW~11~CoO~40~].13H~2~O, with a monotitanoundecatungstocobaltate(II)
anion
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              i35
_journal_page_last               i37
_journal_paper_doi               10.1107/S1600536805005180
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'K6 H2 [Ti W11 Co O40], 13H2 O'
_chemical_formula_moiety         'H28 Co K6 O53 Ti W11'
_chemical_formula_structural     'K6 H2 [Ti W11 Co O40], 13H2 O'
_chemical_formula_sum            'Co H28 K6 O53 Ti W11'
_chemical_formula_weight         3240.00
_chemical_name_systematic
;
Hexapotassium dihydrogen monotitanoundecatungstocobaltate(II) tridecahydrate
;
_space_group_IT_number           215
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P -4 2 3'
_symmetry_space_group_name_H-M   'P -4 3 m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.6850(16)
_cell_length_b                   10.6850(16)
_cell_length_c                   10.6850(16)
_cell_measurement_reflns_used    942
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.133
_cell_measurement_theta_min      2.696
_cell_volume                     1219.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.091
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8248
_diffrn_reflns_theta_full        30.44
_diffrn_reflns_theta_max         30.44
_diffrn_reflns_theta_min         2.70
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.929
_exptl_absorpt_correction_T_max  0.390
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    4.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1429
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.638
_refine_diff_density_min         -1.659
_refine_ls_abs_structure_details 'Flack (1983), 315 Friedel pairs'
_refine_ls_abs_structure_Flack   0.43(6)
_refine_ls_extinction_coef       0.0093(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0494P)^2^+8.0204P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                516
_reflns_number_total             730
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm6053.cif
_cod_data_source_block           I
_cod_database_code               2205377