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#$Date: 2017-01-11 11:14:44 +0200 (Wed, 11 Jan 2017) $
#$Revision: 190383 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/43/7204312.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7204312
loop_
_publ_author_name
'Dusek, Michal'
'Lüdecke, Jens'
'van Smaalen, Sander'
_publ_section_title
;
 Crystal structure of monophosphate tungsten bronze K1.33P4W8O32 at 110
 K
;
_journal_issue                   5
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1408
_journal_paper_doi               10.1039/b109982p
_journal_volume                  12
_journal_year                    2002
_chemical_formula_sum            'K1.33 O32 P4 W8'
_chemical_formula_weight         2158.7
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 100.65(4)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            1
_cell_length_a                   13.373(7)
_cell_length_b                   5.3282(11)
_cell_length_c                   8.926(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    110
_cell_measurement_theta_max      33.6
_cell_measurement_theta_min      15.2
_cell_volume                     625.1(5)
_diffrn_ambient_temperature      110
_diffrn_measurement_device       'six-circle diffractometer'
_diffrn_measurement_device_details 'limited to four circles'
_diffrn_measurement_device_type  KUMA
_diffrn_measurement_method       'ω-2θ scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.59
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0029
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2883
_diffrn_reflns_theta_max         22.80
_diffrn_reflns_theta_min         1.29
_diffrn_standards_decay_%        4.9
_diffrn_standards_interval_count 30
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    22.7833
_exptl_absorpt_correction_T_max  0.8020
_exptl_absorpt_correction_T_min  0.4769
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    5.733
_exptl_crystal_description       platelet
_exptl_crystal_F_000             933
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.14
_refine_diff_density_min         -3.86
_refine_ls_extinction_coef       0.26(3)
_refine_ls_extinction_method     'B-C type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_obs   2.48
_refine_ls_goodness_of_fit_ref   2.19
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1634
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(σ²(F)+0.0004F²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0597
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_observed          1094
_reflns_number_total             1634
_reflns_observed_criterion       4
_cod_data_source_file            b109982p.txt
_cod_data_source_block           kpwo
_cod_depositor_comments
;
 Moving the _atom_site_adp_type data item from the _atom_site_aniso
 loop to the _atom_site loop.
 
 Antanas Vaitkus,
 2017-01-11
;
_cod_original_cell_volume        625.0(4)
_cod_original_sg_symbol_H-M      P21
_cod_original_formula_sum        'K1.33 P4 W8 O32'
_cod_database_code               7204312
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
W1-1 W -0.06944(5) 0.253898 0.08820(7) Uani -0.0024(3) 2 1
W1-2 W 0.43070(4) 0.24604(16) 0.08763(7) Uani -0.0035(2) 2 1
O1-1 O 0.007(2) 0.025(5) -0.004(3) Uani 0.007(4) 2 1
O1-2 O 0.499(2) 0.006(5) -0.004(3) Uani -0.003(3) 2 1
O2-1 O 0.0365(11) 0.283(4) 0.2789(16) Uani 0.004(4) 2 1
O2-2 O 0.5380(8) 0.263(4) 0.2787(14) Uani -0.005(3) 2 1
W2-1 W -0.21773(5) 0.7545(4) 0.24932(7) Uani -0.0029(3) 2 1
W2-2 W 0.28242(5) 0.7472(3) 0.24799(7) Uani -0.0032(2) 2 1
O3-1 O -0.1377(19) -0.018(5) 0.180(2) Uani 0.014(6) 2 1
O3-2 O 0.3433(13) 0.020(4) 0.176(2) Uani -0.001(4) 2 1
O4-1 O -0.1364(12) 0.511(3) 0.198(2) Uani -0.005(4) 2 1
O4-2 O 0.3627(12) 0.509(3) 0.1986(17) Uani -0.016(3) 2 1
O5-1 O -0.1764(8) 0.262(6) -0.0746(12) Uani 0.001(4) 2 1
O5-2 O 0.3103(8) 0.271(4) -0.0779(13) Uani -0.003(3) 2 1
P-2 P 0.1454(3) 0.244(2) 0.3708(5) Uani -0.0002(13) 2 1
P-1 P 0.6454(3) 0.257(2) 0.3711(4) Uani -0.0044(11) 2 1
O6-1 O 0.1282(8) 0.256(3) 0.5369(15) Uani 0.002(3) 2 1
O6-2 O 0.6347(9) 0.266(4) 0.5389(11) Uani 0.004(3) 2 1
O7-1 O 0.2072(15) 0.458(4) 0.3360(17) Uani 0.005(5) 2 1
O7-2 O 0.6850(12) 0.516(3) 0.3339(16) Uani -0.006(3) 2 1
O8-1 O 0.2017(12) 0.010(3) 0.343(2) Uani 0.002(4) 2 1
O8-2 O 0.7056(12) 0.019(3) 0.334(2) Uani -0.001(4) 2 1
K-1 K -0.0678(8) 0.246(3) 0.5087(12) Uani 0.001(3) 2 0.32672
K-2 K 0.4322(8) 0.266(4) 0.4925(15) Uani 0.014(4) 2 0.32672
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
K 0 3 0.153 0.175 International_Tables_Vol_C 18.962999 18.854 18.683001 18.462
18.204 17.924 17.629999 17.332001 17.032
P 0 8 0.074 0.065 International_Tables_Vol_C 14.977 14.909 14.798 14.646 14.458
14.237 13.99 13.721 13.435
W 0 16 -0.379 5.095 International_Tables_Vol_C 73.947998 73.792999 73.539001
73.194 72.766998 72.268997 71.710999 71.102997 70.
O 0 64 0.007 0.004 International_Tables_Vol_C 7.992 7.967 7.926 7.869 7.798
7.712 7.612 7.501 7.378
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 1 4
6 0 -7
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
O1-1 W1-1 O1-1 90.3(13) . . 2_555
O1-1 W1-1 O2-1 93.9(10) . . .
O1-1 W1-1 O3-1 92.2(12) . . .
O1-1 W1-1 O4-1 173.9(10) . . .
O1-1 W1-1 O5-1 94.3(11) . . .
O1-1 W1-1 O1-1 90.3(13) 2_555 . .
O1-1 W1-1 O2-1 89.0(10) 2_555 . .
O1-1 W1-1 O3-1 177.5(12) 2_555 . .
O1-1 W1-1 O4-1 86.7(11) 2_555 . .
O1-1 W1-1 O5-1 90.3(11) 2_555 . .
O2-1 W1-1 O3-1 90.7(8) . . .
O2-1 W1-1 O4-1 80.7(7) . . .
O2-1 W1-1 O5-1 171.8(9) . . .
O3-1 W1-1 O4-1 90.8(9) . . .
O3-1 W1-1 O5-1 89.7(10) . . .
O4-1 W1-1 O5-1 91.1(8) . . .
O1-2 W1-2 O1-2 90.6(12) . . 2_655
O1-2 W1-2 O2-2 94.1(9) . . .
O1-2 W1-2 O3-2 97.8(11) . . .
O1-2 W1-2 O4-2 176.6(8) . . .
O1-2 W1-2 O5-2 96.7(9) . . .
O1-2 W1-2 O1-2 90.6(12) 2_655 . .
O1-2 W1-2 O2-2 88.5(9) 2_655 . .
O1-2 W1-2 O3-2 171.0(11) 2_655 . .
O1-2 W1-2 O4-2 89.1(10) 2_655 . .
O1-2 W1-2 O5-2 92.9(9) 2_655 . .
O2-2 W1-2 O3-2 94.2(7) . . .
O2-2 W1-2 O4-2 82.5(6) . . .
O2-2 W1-2 O5-2 169.1(7) . . .
O3-2 W1-2 O4-2 82.7(8) . . .
O3-2 W1-2 O5-2 82.9(7) . . .
O4-2 W1-2 O5-2 86.7(6) . . .
O3-1 W2-1 O4-1 88.6(10) 1_565 . .
O3-1 W2-1 O5-2 92.1(9) 1_565 . 2_555
O3-1 W2-1 O6-1 92.0(8) 1_565 . 2_556
O3-1 W2-1 O7-2 175.7(10) 1_565 . 1_455
O3-1 W2-1 O8-2 91.9(10) 1_565 . 1_465
O4-1 W2-1 O5-2 100.0(8) . . 2_555
O4-1 W2-1 O6-1 87.8(7) . . 2_556
O4-1 W2-1 O7-2 95.7(8) . . 1_455
O4-1 W2-1 O8-2 171.8(7) . . 1_465
O5-2 W2-1 O6-1 171.3(6) 2_555 . 2_556
O5-2 W2-1 O7-2 87.7(7) 2_555 . 1_455
O5-2 W2-1 O8-2 88.2(7) 2_555 . 1_465
O6-1 W2-1 O7-2 87.7(6) 2_556 . 1_455
O6-1 W2-1 O8-2 84.0(6) 2_556 . 1_465
O7-2 W2-1 O8-2 83.8(7) 1_455 . 1_465
O3-2 W2-2 O4-2 98.7(8) 1_565 . .
O3-2 W2-2 O5-1 89.6(9) 1_565 . 2_555
O3-2 W2-2 O6-2 95.1(8) 1_565 . 2_656
O3-2 W2-2 O7-1 175.9(8) 1_565 . .
O3-2 W2-2 O8-1 84.7(8) 1_565 . 1_565
O4-2 W2-2 O5-1 102.9(9) . . 2_555
O4-2 W2-2 O6-2 91.1(7) . . 2_656
O4-2 W2-2 O7-1 85.4(8) . . .
O4-2 W2-2 O8-1 170.0(7) . . 1_565
O5-1 W2-2 O6-2 164.4(6) 2_555 . 2_656
O5-1 W2-2 O7-1 89.9(9) 2_555 . .
O5-1 W2-2 O8-1 86.5(8) 2_555 . 1_565
O6-2 W2-2 O7-1 84.3(7) 2_656 . .
O6-2 W2-2 O8-1 79.2(7) 2_656 . 1_565
O7-1 W2-2 O8-1 91.2(8) . . 1_565
O2-1 P-2 O6-1 102.2(7) . . .
O2-1 P-2 O7-1 107.1(12) . . .
O2-1 P-2 O8-1 118.5(11) . . .
O6-1 P-2 O7-1 111.2(10) . . .
O6-1 P-2 O8-1 111.0(11) . . .
O7-1 P-2 O8-1 106.8(11) . . .
O2-2 P-1 O6-2 106.3(7) . . .
O2-2 P-1 O7-2 101.1(11) . . .
O2-2 P-1 O8-2 112.0(11) . . .
O6-2 P-1 O7-2 106.2(12) . . .
O6-2 P-1 O8-2 112.1(11) . . .
O7-2 P-1 O8-2 118.0(9) . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
W1-1 O1-1 1.88(3) . .
W1-1 O1-1 1.89(3) . 2_555
W1-1 O2-1 2.009(13) . .
W1-1 O3-1 1.97(2) . .
W1-1 O4-1 1.99(2) . .
W1-1 O5-1 1.841(10) . .
W1-2 O1-2 1.85(2) . .
W1-2 O1-2 1.90(2) . 2_655
W1-2 O2-2 2.018(10) . .
W1-2 O3-2 1.94(2) . .
W1-2 O4-2 2.026(16) . .
W1-2 O5-2 1.978(10) . .
W2-1 O3-1 1.80(2) . 1_565
W2-1 O4-1 1.804(19) . .
W2-1 O5-2 1.783(10) . 2_555
W2-1 O6-1 2.056(12) . 2_556
W2-1 O7-2 2.060(18) . 1_455
W2-1 O8-2 1.977(18) . 1_465
W2-2 O3-2 1.84(2) . 1_565
W2-2 O4-2 1.770(16) . .
W2-2 O5-1 1.898(10) . 2_555
W2-2 O6-2 2.020(9) . 2_656
W2-2 O7-1 2.07(2) . .
W2-2 O8-1 2.05(2) . 1_565
P-2 O2-1 1.548(15) . .
P-2 O6-1 1.543(15) . .
P-2 O7-1 1.47(2) . .
P-2 O8-1 1.50(2) . .
P-1 O2-2 1.518(10) . .
P-1 O6-2 1.531(11) . .
P-1 O7-2 1.54(2) . .
P-1 O8-2 1.57(2) . .
