#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/19/2011945.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_2011945
loop_
_publ_author_name
'Fletcher, Heath'
'Allen, Christine C.'
'Burns, Robert C.'
'Craig, Donald C.'
_publ_section_title
;
 Pentapotassium dodecatungstoborate(III) hexadecahydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              505
_journal_page_last               507
_journal_paper_doi               10.1107/S0108270101002840
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'K5 [BW12 O40 ](H2 O)16 '
_chemical_formula_moiety         'B1 O40 W12 5-, 5K 1+, 16H2  O'
_chemical_formula_sum            'B H32 K5 O56 W12'
_chemical_formula_weight         3340.72
_space_group_IT_number           180
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 62 2 (0 0 4)'
_symmetry_space_group_name_H-M   'P 62 2 2'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.970(4)
_cell_length_b                   18.970(4)
_cell_length_c                   12.414(5)
_cell_measurement_reflns_used    10
_cell_measurement_temperature    294
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     3868.8(19)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'local software (University of New South Wales)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'RAELS (Rae, 1989)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .047
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5003
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        21
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    27.740
_exptl_absorpt_correction_T_max  .11
_exptl_absorpt_correction_T_min  .04
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.30
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4404.0
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .10
_refine_diff_density_max         1.79
_refine_diff_density_min         -2.70
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.54
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     78
_refine_ls_number_reflns         2122
_refine_ls_R_factor_gt           .036
_refine_ls_shift/su_max          .006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0016F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .048
_reflns_number_gt                2122
_reflns_number_total             2288
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            br1308.cif
_cod_data_source_block           I
_cod_original_cell_volume        3869(2)
_cod_original_sg_symbol_Hall     'P 62 2 (0 0 -2)'
_cod_database_code               2011945
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,2/3+z
3 y-x,-x,1/3+z
4 -x,-y,z
5 y,y-x,2/3+z
6 x-y,x,1/3+z
7 y,x,2/3-z
8 -x,y-x,1/3-z
9 x-y,-y,-z
10 -y,-x,2/3-z
11 x,x-y,1/3-z
12 y-x,y,-z
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_occupancy
_atom_site_type_symbol
B .5000000 .0000000 .5000000 .0229(2) Uani 1 B
W1 .37332(4) .00723(4) .30232(5) .03110(10) Uani 1 W
W2 .56844(4) .14873(4) .30205(5) .0295(2) Uani 1 W
W3 .44594(4) .15078(4) .49093(5) .0298(2) Uani 1 W
O123 .4809(6) .0551(6) .4274(8) .0243(2) Uani 1 O
O2 .6199(7) .2225(6) .2064(8) .0374(4) Uani 1 O
O1 .3008(7) -.0106(7) .2090(9) .0409(2) Uani 1 O
O3 .4190(7) .2230(7) .5132(11) .0382(4) Uani 1 O
O12 .4675(7) .0910(7) .2268(8) .0329(2) Uani 1 O
O32 .5236(7) .2046(6) .3797(8) .0309(2) Uani 1 O
O21 .5934(7) .0669(6) .2612(8) .0300(2) Uani 1 O
O13 .3112(6) -.0673(6) .4078(8) .0304(2) Uani 1 O
O23 .6489(6) .1798(6) .4084(8) .0285(2) Uani 1 O
O31 .3678(7) .0918(6) .3806(9) .0333(2) Uani 1 O
K1 .3687(2) .7374(3) .0000000 .0400(10) Uani 1 K
OKW1 .5000000 .0000000 .0448(13) .069(7) Uani 1 O/K1
OKW2 .4701(11) .3488(11) .3425(14) .123(7) Uani 1 O/K2
OKW3 .1305(11) .261(2) .0000000 .205(9) Uani 1 O/K3
OW1 .1995(16) .399(3) .5000000 .051(9) Uani 1 O
OW2 .725(3) .0000000 .0000000 .058(9) Uani 1 O
OW3 .204(3) .0000000 .5000000 .075(9) Uani 1 O
loop_
_atom_type_symbol
_atom_type_description
O/K1 0.83K+0.17O
O/K2 0.30K+0.70O
O/K3 0.48K+0.52O
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O123 B O123 1_555 1_555 4_655 109.1(7) no
O123 B O123 1_555 1_555 9_556 110.5(7) no
O123 B O123 1_555 1_555 12_656 108.8(7) no
O123 B O123 4_655 1_555 9_556 108.8(7) no
O123 B O123 4_655 1_555 12_656 110.5(7) no
O123 B O123 9_556 1_555 12_656 109.1(7) no
O123 W1 O1 1_555 1_555 1_555 170.4(4) no
O123 W1 O12 1_555 1_555 1_555 74.7(4) no
O123 W1 O13 1_555 1_555 1_555 85.7(4) no
O123 W1 O31 1_555 1_555 1_555 75.1(4) no
O123 W1 O21 1_555 1_555 4_655 85.3(4) no
O1 W1 O12 1_555 1_555 1_555 99.0(5) no
O1 W1 O13 1_555 1_555 1_555 100.8(5) no
O1 W1 O31 1_555 1_555 1_555 97.7(5) no
O1 W1 O21 1_555 1_555 4_655 102.0(5) no
O12 W1 O13 1_555 1_555 1_555 160.2(4) no
O12 W1 O31 1_555 1_555 1_555 88.4(5) no
O12 W1 O21 1_555 1_555 4_655 88.0(5) no
O13 W1 O31 1_555 1_555 1_555 90.0(5) no
O13 W1 O21 1_555 1_555 4_655 86.8(4) no
O31 W1 O21 1_555 1_555 4_655 160.3(5) no
O123 W2 O2 1_555 1_555 1_555 169.7(5) no
O123 W2 O12 1_555 1_555 1_555 76.1(4) no
O123 W2 O32 1_555 1_555 1_555 75.0(4) no
O123 W2 O21 1_555 1_555 1_555 85.9(4) no
O123 W2 O23 1_555 1_555 1_555 85.8(4) no
O2 W2 O12 1_555 1_555 1_555 97.3(5) no
O2 W2 O32 1_555 1_555 1_555 97.2(5) no
O2 W2 O21 1_555 1_555 1_555 102.0(5) no
O2 W2 O23 1_555 1_555 1_555 100.9(5) no
O12 W2 O32 1_555 1_555 1_555 88.2(5) no
O12 W2 O21 1_555 1_555 1_555 89.4(5) no
O12 W2 O23 1_555 1_555 1_555 161.8(4) no
O32 W2 O21 1_555 1_555 1_555 160.8(4) no
O32 W2 O23 1_555 1_555 1_555 89.3(4) no
O21 W2 O23 1_555 1_555 1_555 87.1(5) no
O123 W3 O3 1_555 1_555 1_555 169.8(5) no
O123 W3 O32 1_555 1_555 1_555 74.3(4) no
O123 W3 O31 1_555 1_555 1_555 75.2(4) no
O123 W3 O13 1_555 1_555 9_556 84.9(4) no
O123 W3 O23 1_555 1_555 12_656 85.3(4) no
O3 W3 O32 1_555 1_555 1_555 98.6(5) no
O3 W3 O31 1_555 1_555 1_555 97.5(5) no
O3 W3 O13 1_555 1_555 9_556 102.3(5) no
O3 W3 O23 1_555 1_555 12_656 102.3(5) no
O32 W3 O31 1_555 1_555 1_555 87.7(5) no
O32 W3 O13 1_555 1_555 9_556 159.1(4) no
O32 W3 O23 1_555 1_555 12_656 90.3(4) no
O31 W3 O13 1_555 1_555 9_556 89.1(5) no
O31 W3 O23 1_555 1_555 12_656 160.2(4) no
O13 W3 O23 9_556 1_555 12_656 85.8(4) no
B O123 W1 1_555 1_555 1_555 124.9(5) no
B O123 W2 1_555 1_555 1_555 125.8(5) no
B O123 W3 1_555 1_555 1_555 125.0(5) no
W1 O123 W2 1_555 1_555 1_555 90.2(3) no
W1 O123 W3 1_555 1_555 1_555 89.7(3) no
W2 O123 W3 1_555 1_555 1_555 90.2(3) no
W1 O12 W2 1_555 1_555 1_555 118.9(5) no
W2 O32 W3 1_555 1_555 1_555 120.5(5) no
W2 O21 W1 1_555 1_555 4_655 148.4(6) no
W1 O13 W3 1_555 1_555 9_556 150.3(6) no
W2 O23 W3 1_555 1_555 12_656 149.3(6) no
W1 O31 W3 1_555 1_555 1_555 120.0(6) no.........................
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
B O123 1_555 1_555 1.554(10) yes
B O123 1_555 4_655 1.554(10) no
B O123 1_555 9_556 1.554(10) no
B O123 1_555 12_656 1.554(10) no
W1 O123 1_555 1_555 2.354(10) yes
W1 O1 1_555 1_555 1.699(11) yes
W1 O12 1_555 1_555 1.938(10) yes
W1 O13 1_555 1_555 1.853(10) yes
W1 O31 1_555 1_555 1.923(11) yes
W1 O21 1_555 4_655 1.876(10) yes
W2 O123 1_555 1_555 2.320(9) yes
W2 O2 1_555 1_555 1.719(10) yes
W2 O12 1_555 1_555 1.908(10) yes
W2 O32 1_555 1_555 1.917(10) yes
W2 O21 1_555 1_555 1.905(10) yes
W2 O23 1_555 1_555 1.876(11) yes
W3 O123 1_555 1_555 2.358(10) yes
W3 O3 1_555 1_555 1.708(10) yes
W3 O32 1_555 1_555 1.902(10) yes
W3 O31 1_555 1_555 1.914(11) yes
W3 O13 1_555 9_556 1.923(10) yes
W3 O23 1_555 12_656 1.891(10) yes
