#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/53/2205377.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2205377
loop_
_publ_author_name
'Werner Kraus'
'Holger Stephan'
'Anita Röllich'
'Zdenek Matĕjka '
'Günter Reck'
_publ_section_title
;
K₆H₂[TiW₁₁CoO₄₀].13H₂O, 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       ω
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0494P)²+8.0204P] where P = (Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            wm6053.cif
_cod_data_source_block           I
_cod_database_code               2205377
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
W1 0.26855(4) 0.26855(4) 0.49996(19) 0.0358(3) Uani d SP 0.91666 W
Ti1 0.26855(4) 0.26855(4) 0.49996(19) 0.0358(3) Uani d SP 0.08333 Ti
Co1 0.5000 0.5000 0.5000 0.0252(11) Uani d S 1 Co
K1 0.0000 0.5000 0.5000 0.0423(13) Uani d S 1 K
K2 0.0000 0.0000 0.3680(12) 0.069(3) Uani d SP 0.50 K
O1 0.2273(13) 0.3999(10) 0.6001(10) 0.045(3) Uani d S 1 O
O2 0.3970(9) 0.3970(9) 0.3970(9) 0.027(4) Uani d S 1 O
O3 0.1555(7) 0.1555(7) 0.492(3) 0.059(4) Uani d S 1 O
O4 0.1779(13) 0.3594(9) 0.3594(9) 0.049(4) Uani d S 1 O
O5 0.0187(19) 0.2204(12) 0.2204(12) 0.078(6) Uani d S 1 O
O6 0.0000 0.0000 0.0000 0.108(19) Uani d S 1 O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 W1 O1 . 8_656 113.8(8) ?
O3 W1 O1 . . 113.8(8) ?
O1 W1 O1 8_656 . 91.6(9) ?
O3 W1 O4 . 5 87.9(10) ?
O1 W1 O4 8_656 5 87.2(5) ?
O1 W1 O4 . 5 156.5(6) ?
O3 W1 O4 . . 87.9(10) ?
O1 W1 O4 8_656 . 156.5(6) ?
O1 W1 O4 . . 87.2(5) ?
O4 W1 O4 5 . 84.8(7) ?
O3 W1 O2 . . 147.6(13) ?
O1 W1 O2 8_656 . 88.0(5) ?
O1 W1 O2 . . 88.0(5) ?
O4 W1 O2 5 . 68.6(4) ?
O4 W1 O2 . . 68.6(4) ?
O3 W1 K1 . . 85.762(10) ?
O1 W1 K1 8_656 . 137.9(5) ?
O1 W1 K1 . . 46.6(5) ?
O4 W1 K1 5 . 132.3(4) ?
O4 W1 K1 . . 47.8(3) ?
O2 W1 K1 . . 93.69(2) ?
O3 W1 K1 . 5 85.762(9) ?
O1 W1 K1 8_656 5 46.6(5) ?
O1 W1 K1 . 5 137.9(5) ?
O4 W1 K1 5 5 47.8(3) ?
O4 W1 K1 . 5 132.3(4) ?
O2 W1 K1 . 5 93.69(2) ?
K1 W1 K1 . 5 171.512(16) ?
O2 Co1 O2 . 4_566 109.4710(10) ?
O2 Co1 O2 . 2_665 109.4710(10) ?
O2 Co1 O2 4_566 2_665 109.471(3) ?
O2 Co1 O2 . 3_656 109.4710(10) ?
O2 Co1 O2 4_566 3_656 109.4710(10) ?
O2 Co1 O2 2_665 3_656 109.471(3) ?
O4 K1 O4 4_566 . 96.3(6) ?
O4 K1 O4 4_566 3_556 116.4(4) ?
O4 K1 O4 . 3_556 116.4(4) ?
O4 K1 O4 4_566 2_565 116.4(4) ?
O4 K1 O4 . 2_565 116.4(4) ?
O4 K1 O4 3_556 2_565 96.3(6) ?
O4 K1 O1 4_566 3_556 163.7(3) ?
O4 K1 O1 . 3_556 99.9(5) ?
O4 K1 O1 3_556 3_556 55.5(3) ?
O4 K1 O1 2_565 3_556 55.5(3) ?
O4 K1 O1 4_566 . 55.5(3) ?
O4 K1 O1 . . 55.5(3) ?
O4 K1 O1 3_556 . 99.9(5) ?
O4 K1 O1 2_565 . 163.7(3) ?
O1 K1 O1 3_556 . 136.1(3) ?
O4 K1 O1 4_566 4_566 55.5(3) ?
O4 K1 O1 . 4_566 55.5(3) ?
O4 K1 O1 3_556 4_566 163.7(3) ?
O4 K1 O1 2_565 4_566 99.9(5) ?
O1 K1 O1 3_556 4_566 136.1(3) ?
O1 K1 O1 . 4_566 63.8(5) ?
O4 K1 O1 4_566 2_565 99.9(5) ?
O4 K1 O1 . 2_565 163.7(3) ?
O4 K1 O1 3_556 2_565 55.5(3) ?
O4 K1 O1 2_565 2_565 55.5(3) ?
O1 K1 O1 3_556 2_565 63.8(5) ?
O1 K1 O1 . 2_565 136.1(3) ?
O1 K1 O1 4_566 2_565 136.1(3) ?
O4 K1 W1 4_566 4_566 31.88(16) ?
O4 K1 W1 . 4_566 80.7(3) ?
O4 K1 W1 3_556 4_566 148.11(15) ?
O4 K1 W1 2_565 4_566 99.3(3) ?
O1 K1 W1 3_556 4_566 152.51(3) ?
O1 K1 W1 . 4_566 66.5(2) ?
O1 K1 W1 4_566 4_566 27.50(3) ?
O1 K1 W1 2_565 4_566 113.5(2) ?
O4 K1 Ti1 4_566 11_566 31.88(16) ?
O4 K1 Ti1 . 11_566 80.7(3) ?
O4 K1 Ti1 3_556 11_566 99.3(3) ?
O4 K1 Ti1 2_565 11_566 148.11(15) ?
O1 K1 Ti1 3_556 11_566 152.51(3) ?
O1 K1 Ti1 . 11_566 27.50(3) ?
O1 K1 Ti1 4_566 11_566 66.5(2) ?
O1 K1 Ti1 2_565 11_566 113.5(2) ?
W1 K1 Ti1 4_566 11_566 54.97(5) ?
O4 K1 W1 4_566 11_566 31.88(16) ?
O4 K1 W1 . 11_566 80.7(3) ?
O4 K1 W1 3_556 11_566 99.3(3) ?
O4 K1 W1 2_565 11_566 148.11(15) ?
O1 K1 W1 3_556 11_566 152.51(3) ?
O1 K1 W1 . 11_566 27.50(3) ?
O1 K1 W1 4_566 11_566 66.5(2) ?
O1 K1 W1 2_565 11_566 113.5(2) ?
W1 K1 W1 4_566 11_566 54.97(5) ?
Ti1 K1 W1 11_566 11_566 0.000(9) ?
O4 K1 Ti1 4_566 4_566 31.88(16) ?
O4 K1 Ti1 . 4_566 80.7(3) ?
O4 K1 Ti1 3_556 4_566 148.11(15) ?
O4 K1 Ti1 2_565 4_566 99.3(3) ?
O1 K1 Ti1 3_556 4_566 152.51(3) ?
O1 K1 Ti1 . 4_566 66.5(2) ?
O1 K1 Ti1 4_566 4_566 27.50(3) ?
O1 K1 Ti1 2_565 4_566 113.5(2) ?
W1 K1 Ti1 4_566 4_566 0.00(6) ?
Ti1 K1 Ti1 11_566 4_566 54.97(5) ?
W1 K1 Ti1 11_566 4_566 54.97(5) ?
O3 K2 O3 . 2 121.2(14) ?
O3 K2 O3 . 4_556 74.7(2) ?
O3 K2 O3 2 4_556 74.7(2) ?
O3 K2 O3 . 3_556 74.7(2) ?
O3 K2 O3 2 3_556 74.7(2) ?
O3 K2 O3 4_556 3_556 115.0(14) ?
O3 K2 K2 . 3_556 60.6(7) ?
O3 K2 K2 2 3_556 60.6(7) ?
O3 K2 K2 4_556 3_556 57.5(7) ?
O3 K2 K2 3_556 3_556 57.5(7) ?
O3 K2 O5 . 7 145.7(5) ?
O3 K2 O5 2 7 73.7(6) ?
O3 K2 O5 4_556 7 138.6(5) ?
O3 K2 O5 3_556 7 81.1(6) ?
K2 K2 O5 3_556 7 123.7(4) ?
O3 K2 O5 . 2 145.7(5) ?
O3 K2 O5 2 2 73.7(6) ?
O3 K2 O5 4_556 2 81.1(6) ?
O3 K2 O5 3_556 2 138.6(5) ?
K2 K2 O5 3_556 2 123.7(4) ?
O5 K2 O5 7 2 64.9(8) ?
O3 K2 O5 . . 73.7(6) ?
O3 K2 O5 2 . 145.7(5) ?
O3 K2 O5 4_556 . 138.6(5) ?
O3 K2 O5 3_556 . 81.1(6) ?
K2 K2 O5 3_556 . 123.7(4) ?
O5 K2 O5 7 . 78.9(8) ?
O5 K2 O5 2 . 112.5(8) ?
O3 K2 O5 . 5 73.7(6) ?
O3 K2 O5 2 5 145.7(5) ?
O3 K2 O5 4_556 5 81.1(6) ?
O3 K2 O5 3_556 5 138.6(5) ?
K2 K2 O5 3_556 5 123.7(4) ?
O5 K2 O5 7 5 112.5(8) ?
O5 K2 O5 2 5 78.9(8) ?
O5 K2 O5 . 5 64.9(8) ?
Ti1 O1 W1 11_566 11_566 0.000(15) ?
Ti1 O1 W1 11_566 . 148.1(9) ?
W1 O1 W1 11_566 . 148.1(9) yes
Ti1 O1 K1 11_566 . 105.9(5) ?
W1 O1 K1 11_566 . 105.9(5) ?
W1 O1 K1 . . 105.9(5) ?
Co1 O2 W1 . . 115.2(4) ?
Co1 O2 Ti1 . 9 115.2(4) ?
W1 O2 Ti1 . 9 103.2(5) ?
Co1 O2 W1 . 5 115.2(4) ?
W1 O2 W1 . 5 103.2(5) ?
Ti1 O2 W1 9 5 103.2(5) ?
Co1 O2 W1 . 9 115.2(4) ?
W1 O2 W1 . 9 103.2(5) ?
Ti1 O2 W1 9 9 0.000(15) ?
W1 O2 W1 5 9 103.2(5) ?
Co1 O2 Ti1 . 5 115.2(4) ?
W1 O2 Ti1 . 5 103.2(5) ?
Ti1 O2 Ti1 9 5 103.2(5) ?
W1 O2 Ti1 5 5 0.00(3) ?
W1 O2 Ti1 9 5 103.2(5) ?
W1 O3 K2 . . 153.5(18) ?
W1 O3 K2 . 3_556 144.6(19) ?
K2 O3 K2 . 3_556 61.9(5) ?
Ti1 O4 W1 9 9 0.00(8) ?
Ti1 O4 W1 9 . 118.6(7) ?
W1 O4 W1 9 . 118.6(7) yes
Ti1 O4 K1 9 . 100.4(4) ?
W1 O4 K1 9 . 100.4(4) ?
W1 O4 K1 . . 100.4(4) ?
K2 O5 K2 9 . 156.3(8) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 O3 . 1.711(11) yes
W1 O1 8_656 1.819(4) yes
W1 O1 . 1.819(4) ?
W1 O4 5 2.034(8) yes
W1 O4 . 2.034(8) ?
W1 O2 . 2.231(7) yes
W1 K1 . 3.7881(6) ?
W1 K1 5 3.7881(6) ?
Co1 O2 . 1.906(17) yes
Co1 O2 4_566 1.906(17) ?
Co1 O2 2_665 1.906(17) ?
Co1 O2 3_656 1.906(17) ?
K1 O4 4_566 2.851(12) ?
K1 O4 . 2.851(12) yes
K1 O4 3_556 2.851(12) ?
K1 O4 2_565 2.851(12) ?
K1 O1 3_556 2.861(15) ?
K1 O1 . 2.861(15) yes
K1 O1 4_566 2.861(16) ?
K1 O1 2_565 2.861(15) ?
K1 W1 4_566 3.7881(6) ?
K1 Ti1 11_566 3.7881(6) ?
K1 W1 11_566 3.7881(6) ?
K1 Ti1 4_566 3.7881(6) ?
K2 O3 . 2.70(2) yes
K2 O3 2 2.70(2) ?
K2 O3 4_556 2.78(2) yes
K2 O3 3_556 2.78(2) ?
K2 K2 3_556 2.82(3) ?
K2 O5 7 2.841(8) ?
K2 O5 2 2.841(8) ?
K2 O5 . 2.841(8) ?
K2 O5 5 2.841(8) ?
O1 Ti1 11_566 1.819(4) ?
O1 W1 11_566 1.819(4) ?
O2 Ti1 9 2.231(7) ?
O2 W1 5 2.231(7) ?
O2 W1 9 2.231(7) ?
O2 Ti1 5 2.231(7) ?
O3 K2 3_556 2.78(2) ?
O4 Ti1 9 2.034(8) ?
O4 W1 9 2.034(8) ?
O5 K2 9 2.841(8) ?
