#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:57:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179712 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/14/7001419.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_7001419
loop_
_publ_author_name
'Redrup, Kate V.'
'Weller, Mark T.'
_publ_section_title
;
 Hydrothermal routes to new sodium hydrogen polytungstates
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4468
_journal_page_last               4472
_journal_paper_doi               10.1039/b818103a
_journal_year                    2009
_chemical_formula_sum            'H40 Na5 O62 W12'
_chemical_formula_weight         3353.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.260(2)
_cell_angle_beta                 76.107(2)
_cell_angle_gamma                87.059(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8677(4)
_cell_length_b                   12.4370(4)
_cell_length_c                   12.5313(4)
_cell_measurement_reflns_used    6948
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1565.58(9)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28074
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.089
_exptl_absorpt_correction_T_max  0.6664
_exptl_absorpt_correction_T_min  0.2061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    3.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1479
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.962
_refine_diff_density_min         -3.270
_refine_diff_density_rms         0.448
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5498
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0727P)²+20.7159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                4392
_reflns_number_total             5498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818103a.txt
_cod_data_source_block           2007kvb0028mtw
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001419
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.03146(6) 0.26243(5) 1.06262(5) 0.01358(17) Uani 1 1 d . . .
W2 W 0.76133(6) 0.31771(5) 1.22835(5) 0.01483(17) Uani 1 1 d . . .
W3 W 0.73786(6) 0.32936(5) 0.93575(5) 0.01431(17) Uani 1 1 d . . .
W4 W 0.99835(6) 0.27036(5) 0.76916(5) 0.01455(17) Uani 1 1 d . . .
W5 W 1.26227(6) 0.38405(5) 0.77565(5) 0.01480(17) Uani 1 1 d . . .
W6 W 0.96684(6) 0.57007(5) 0.77083(5) 0.01337(17) Uani 1 1 d . . .
Na1 Na 0.7667(6) 0.6194(5) 0.5256(5) 0.0241(14) Uani 1 1 d . . .
Na2 Na 0.7575(11) 0.0189(9) 0.9283(10) 0.081(3) Uani 1 1 d . . .
Na3 Na 1.0000 0.0000 1.5000 0.046(3) Uani 1 2 d S . .
O1 O 1.0809(9) 0.2883(9) 1.1930(8) 0.019(2) Uani 1 1 d U . .
O2 O 1.0947(9) 0.1283(8) 1.0762(8) 0.016(2) Uani 1 1 d U . .
O3 O 0.9282(9) 0.2729(8) 0.9575(9) 0.017(2) Uani 1 1 d U . .
O4 O 0.9283(9) 0.4155(8) 1.0984(8) 0.011(2) Uani 1 1 d U . .
O5 O 0.8652(9) 0.2042(8) 1.1870(8) 0.015(2) Uani 1 1 d U . .
O6 O 0.6861(10) 0.5911(9) 0.3724(9) 0.022(2) Uani 1 1 d U . .
O7 O 0.8640(9) 0.3374(8) 1.3211(8) 0.016(2) Uani 1 1 d U . .
O8 O 0.6318(11) 0.2412(9) 1.3267(10) 0.026(3) Uani 1 1 d U . .
O9 O 0.7044(10) 0.4708(9) 1.2154(9) 0.022(2) Uani 1 1 d U . .
O10 O 0.7051(10) 0.3445(9) 1.0835(9) 0.020(2) Uani 1 1 d U . .
O11 O 0.6814(10) 0.1911(9) 0.9690(9) 0.022(2) Uani 1 1 d U . .
O12 O 0.6122(10) 0.4135(9) 0.8903(9) 0.021(2) Uani 1 1 d U . .
O13 O 0.8358(9) 0.3359(8) 0.7810(8) 0.014(2) Uani 1 1 d U . .
O14 O 0.8450(9) 0.4895(9) 0.8891(9) 0.017(2) Uani 1 1 d U . .
O15 O 0.9539(10) 0.1277(9) 0.8154(9) 0.019(2) Uani 1 1 d U . .
O16 O 1.0397(10) 0.3034(9) 0.6193(9) 0.022(2) Uani 1 1 d U . .
O17 O 1.1593(10) 0.2477(8) 0.8044(8) 0.017(2) Uani 1 1 d U . .
O18 O 1.0694(9) 0.4420(9) 0.7600(8) 0.016(2) Uani 1 1 d U . .
O19 O 1.3888(9) 0.3135(8) 0.8259(8) 0.015(2) Uani 1 1 d U . .
O20 O 1.1559(10) 0.3565(9) 0.9581(9) 0.020(2) Uani 1 1 d U . .
O21 O 0.9007(9) 0.5992(8) 0.6519(9) 0.015(2) Uani 1 1 d U . .
O1W O 0.8384(11) 0.4346(10) 0.5242(10) 0.028(3) Uani 1 1 d U . .
O2W O 0.5852(11) 0.5439(11) 0.6718(10) 0.032(3) Uani 1 1 d U . .
O3W O 0.719(2) 0.8180(18) 0.5000(19) 0.095(6) Uani 1 1 d U . .
O4W O 0.5713(19) -0.1069(17) 1.0255(18) 0.088(6) Uani 1 1 d U . .
O5W O 0.8738(17) 0.0217(15) 0.7330(15) 0.075(5) Uani 1 1 d U . .
O6W O 0.6752(18) 0.0439(16) 0.7644(16) 0.079(5) Uani 1 1 d U . .
O7W O 0.8263(18) 0.0021(15) 1.0926(16) 0.072(5) Uani 1 1 d U . .
O8W O 0.9108(11) -0.0008(10) 1.3425(10) 0.029(3) Uani 1 1 d U . .
O9W O 1.0929(12) -0.1711(10) 1.4734(11) 0.036(3) Uani 1 1 d U . .
O10W O 1.1687(13) 0.1091(10) 1.3516(11) 0.036(3) Uani 1 1 d U . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 W1 O20 103.8(5) . . ?
O2 W1 O3 102.2(4) . . ?
O20 W1 O3 94.9(5) . . ?
O2 W1 O1 97.5(4) . . ?
O20 W1 O1 92.7(4) . . ?
O3 W1 O1 156.5(4) . . ?
O2 W1 O5 94.5(4) . . ?
O20 W1 O5 161.5(4) . . ?
O3 W1 O5 84.0(4) . . ?
O1 W1 O5 81.8(4) . . ?
O2 W1 O4 164.1(4) . . ?
O20 W1 O4 88.8(4) . . ?
O3 W1 O4 86.2(4) . . ?
O1 W1 O4 71.8(4) . . ?
O5 W1 O4 72.7(4) . . ?
O8 W2 O7 103.5(5) . . ?
O8 W2 O5 102.6(5) . . ?
O7 W2 O5 91.9(4) . . ?
O8 W2 O9 100.5(5) . . ?
O7 W2 O9 87.9(5) . . ?
O5 W2 O9 156.3(4) . . ?
O8 W2 O10 100.2(5) . . ?
O7 W2 O10 155.9(4) . . ?
O5 W2 O10 87.6(4) . . ?
O9 W2 O10 83.1(4) . . ?
O8 W2 O4 178.9(4) . . ?
O7 W2 O4 77.5(4) . . ?
O5 W2 O4 76.9(4) . . ?
O9 W2 O4 79.9(4) . . ?
O10 W2 O4 78.9(4) . . ?
O11 W3 O12 103.7(5) . . ?
O11 W3 O10 100.0(5) . . ?
O12 W3 O10 97.0(5) . . ?
O11 W3 O13 94.7(4) . . ?
O12 W3 O13 95.8(4) . . ?
O10 W3 O13 157.6(4) . . ?
O11 W3 O3 92.6(4) . . ?
O12 W3 O3 162.1(4) . . ?
O10 W3 O3 87.4(4) . . ?
O13 W3 O3 75.0(4) . . ?
O11 W3 O14 169.1(4) . . ?
O12 W3 O14 86.3(4) . . ?
O10 W3 O14 82.8(4) . . ?
O13 W3 O14 79.8(4) . . ?
O3 W3 O14 76.9(4) . . ?
O16 W4 O15 103.7(5) . . ?
O16 W4 O17 101.4(5) . . ?
O15 W4 O17 95.9(5) . . ?
O16 W4 O13 96.8(5) . . ?
O15 W4 O13 99.8(4) . . ?
O17 W4 O13 152.4(4) . . ?
O16 W4 O18 91.3(4) . . ?
O15 W4 O18 163.3(4) . . ?
O17 W4 O18 73.6(4) . . ?
O13 W4 O18 85.4(4) . . ?
O16 W4 O3 165.7(4) . . ?
O15 W4 O3 88.6(4) . . ?
O17 W4 O3 84.4(4) . . ?
O13 W4 O3 73.5(4) . . ?
O18 W4 O3 77.6(3) . . ?
O19 W5 O6 102.3(5) . 2_766 ?
O19 W5 O9 98.7(5) . 2_767 ?
O6 W5 O9 99.5(5) 2_766 2_767 ?
O19 W5 O17 96.1(4) . . ?
O6 W5 O17 95.8(5) 2_766 . ?
O9 W5 O17 155.9(4) 2_767 . ?
O19 W5 O18 163.4(4) . . ?
O6 W5 O18 91.8(4) 2_766 . ?
O9 W5 O18 87.5(4) 2_767 . ?
O17 W5 O18 73.4(4) . . ?
O19 W5 O20 88.8(4) . . ?
O6 W5 O20 168.0(4) 2_766 . ?
O9 W5 O20 82.9(4) 2_767 . ?
O17 W5 O20 78.4(4) . . ?
O18 W5 O20 76.6(4) . . ?
O21 W6 O14 104.3(5) . . ?
O21 W6 O18 103.2(4) . . ?
O14 W6 O18 94.4(4) . . ?
O21 W6 O1 96.4(5) . 2_767 ?
O14 W6 O1 92.8(4) . 2_767 ?
O18 W6 O1 156.7(4) . 2_767 ?
O21 W6 O7 94.8(4) . 2_767 ?
O14 W6 O7 160.7(4) . 2_767 ?
O18 W6 O7 83.9(4) . 2_767 ?
O1 W6 O7 82.0(4) 2_767 2_767 ?
O21 W6 O4 163.5(4) . 2_767 ?
O14 W6 O4 88.1(4) . 2_767 ?
O18 W6 O4 86.3(4) . 2_767 ?
O1 W6 O4 71.8(4) 2_767 2_767 ?
O7 W6 O4 72.7(4) 2_767 2_767 ?
O21 Na1 O2W 95.0(4) . . ?
O21 Na1 O1W 83.0(4) . . ?
O2W Na1 O1W 91.5(5) . . ?
O21 Na1 O6 158.3(5) . . ?
O2W Na1 O6 95.1(4) . . ?
O1W Na1 O6 77.6(4) . . ?
O21 Na1 O3W 97.9(6) . . ?
O2W Na1 O3W 97.1(7) . . ?
O1W Na1 O3W 171.3(7) . . ?
O6 Na1 O3W 99.8(6) . . ?
O21 Na1 O16 82.4(4) . 2_766 ?
O2W Na1 O16 177.4(5) . 2_766 ?
O1W Na1 O16 88.3(4) . 2_766 ?
O6 Na1 O16 87.4(4) . 2_766 ?
O3W Na1 O16 83.2(6) . 2_766 ?
O7W Na2 O6W 176.0(8) . . ?
O7W Na2 O2 79.3(6) . 2_757 ?
O6W Na2 O2 104.6(7) . 2_757 ?
O7W Na2 O11 78.9(6) . . ?
O6W Na2 O11 97.5(7) . . ?
O2 Na2 O11 153.7(7) 2_757 . ?
O7W Na2 O4W 95.7(8) . . ?
O6W Na2 O4W 83.1(8) . . ?
O2 Na2 O4W 95.4(6) 2_757 . ?
O11 Na2 O4W 101.2(7) . . ?
O7W Na2 O5W 131.4(8) . . ?
O6W Na2 O5W 52.0(7) . . ?
O2 Na2 O5W 65.8(6) 2_757 . ?
O11 Na2 O5W 120.8(7) . . ?
O4W Na2 O5W 119.4(8) . . ?
O7W Na2 O15 88.3(7) . . ?
O6W Na2 O15 93.3(6) . . ?
O2 Na2 O15 78.8(5) 2_757 . ?
O11 Na2 O15 86.0(5) . . ?
O4W Na2 O15 172.3(7) . . ?
O5W Na2 O15 53.7(5) . . ?
O9W Na3 O9W 180.000(3) . 2_758 ?
O9W Na3 O10W 89.2(4) . 2_758 ?
O9W Na3 O10W 90.8(4) 2_758 2_758 ?
O9W Na3 O10W 90.8(4) . . ?
O9W Na3 O10W 89.2(4) 2_758 . ?
O10W Na3 O10W 180.000(1) 2_758 . ?
O9W Na3 O8W 96.9(4) . 2_758 ?
O9W Na3 O8W 83.1(4) 2_758 2_758 ?
O10W Na3 O8W 84.4(4) 2_758 2_758 ?
O10W Na3 O8W 95.6(4) . 2_758 ?
O9W Na3 O8W 83.1(4) . . ?
O9W Na3 O8W 96.9(4) 2_758 . ?
O10W Na3 O8W 95.6(4) 2_758 . ?
O10W Na3 O8W 84.4(4) . . ?
O8W Na3 O8W 180.000(2) 2_758 . ?
O9W Na3 O5W 122.7(5) . 1_556 ?
O9W Na3 O5W 57.3(5) 2_758 1_556 ?
O10W Na3 O5W 49.2(4) 2_758 1_556 ?
O10W Na3 O5W 130.8(4) . 1_556 ?
O8W Na3 O5W 49.8(5) 2_758 1_556 ?
O8W Na3 O5W 130.2(5) . 1_556 ?
O9W Na3 O5W 57.3(5) . 2_757 ?
O9W Na3 O5W 122.7(5) 2_758 2_757 ?
O10W Na3 O5W 130.8(4) 2_758 2_757 ?
O10W Na3 O5W 49.2(4) . 2_757 ?
O8W Na3 O5W 130.2(5) 2_758 2_757 ?
O8W Na3 O5W 49.8(5) . 2_757 ?
O5W Na3 O5W 180.000(2) 1_556 2_757 ?
W1 O1 W6 118.7(5) . 2_767 ?
W1 O2 Na2 161.4(6) . 2_757 ?
W1 O3 W3 139.0(5) . . ?
W1 O3 W4 125.9(5) . . ?
W3 O3 W4 93.4(4) . . ?
W2 O4 W6 95.6(4) . 2_767 ?
W2 O4 W1 95.5(3) . . ?
W6 O4 W1 96.2(4) 2_767 . ?
W2 O5 W1 114.9(5) . . ?
W5 O6 Na1 137.4(6) 2_766 . ?
W2 O7 W6 114.2(5) . 2_767 ?
W5 O9 W2 147.6(6) 2_767 . ?
W3 O10 W2 147.8(6) . . ?
W3 O11 Na2 137.6(6) . . ?
W4 O13 W3 116.9(5) . . ?
W6 O14 W3 137.3(5) . . ?
W4 O15 Na2 134.5(6) . . ?
W4 O16 Na1 132.9(6) . 2_766 ?
W4 O17 W5 116.8(5) . . ?
W6 O18 W5 138.2(5) . . ?
W6 O18 W4 126.0(5) . . ?
W5 O18 W4 94.5(4) . . ?
W1 O20 W5 137.7(5) . . ?
W6 O21 Na1 166.0(6) . . ?
Na2 O5W Na3 173.4(8) . 1_554 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O2 1.747(10) . ?
W1 O20 1.814(10) . ?
W1 O3 1.897(10) . ?
W1 O1 1.955(10) . ?
W1 O5 2.077(9) . ?
W1 O4 2.268(9) . ?
W2 O8 1.731(11) . ?
W2 O7 1.865(10) . ?
W2 O5 1.880(10) . ?
W2 O9 1.942(10) . ?
W2 O10 1.980(10) . ?
W2 O4 2.242(10) . ?
W3 O11 1.748(11) . ?
W3 O12 1.774(10) . ?
W3 O10 1.866(10) . ?
W3 O13 1.955(10) . ?
W3 O3 2.203(10) . ?
W3 O14 2.206(10) . ?
W4 O16 1.744(11) . ?
W4 O15 1.745(10) . ?
W4 O17 1.892(10) . ?
W4 O13 1.900(10) . ?
W4 O18 2.268(10) . ?
W4 O3 2.309(10) . ?
W5 O19 1.736(10) . ?
W5 O6 1.738(11) 2_766 ?
W5 O9 1.901(10) 2_767 ?
W5 O17 1.971(10) . ?
W5 O18 2.215(10) . ?
W5 O20 2.230(11) . ?
W6 O21 1.740(10) . ?
W6 O14 1.801(10) . ?
W6 O18 1.917(10) . ?
W6 O1 1.964(10) 2_767 ?
W6 O7 2.103(10) 2_767 ?
W6 O4 2.261(9) 2_767 ?
Na1 O21 2.349(11) . ?
Na1 O2W 2.353(13) . ?
Na1 O1W 2.392(13) . ?
Na1 O6 2.414(12) . ?
Na1 O3W 2.44(2) . ?
Na1 O16 2.441(12) 2_766 ?
Na2 O7W 2.30(2) . ?
Na2 O6W 2.36(2) . ?
Na2 O2 2.377(15) 2_757 ?
Na2 O11 2.410(15) . ?
Na2 O4W 2.45(2) . ?
Na2 O5W 2.46(2) . ?
Na2 O15 2.463(15) . ?
Na3 O9W 2.390(12) . ?
Na3 O9W 2.390(12) 2_758 ?
Na3 O10W 2.396(13) 2_758 ?
Na3 O10W 2.396(13) . ?
Na3 O8W 2.401(11) 2_758 ?
Na3 O8W 2.401(11) . ?
Na3 O5W 3.000(18) 1_556 ?
Na3 O5W 3.000(18) 2_757 ?
O1 W6 1.964(10) 2_767 ?
O2 Na2 2.377(15) 2_757 ?
O4 W6 2.261(9) 2_767 ?
O6 W5 1.738(11) 2_766 ?
O7 W6 2.103(10) 2_767 ?
O9 W5 1.901(10) 2_767 ?
O16 Na1 2.441(12) 2_766 ?
O5W Na3 3.000(18) 1_554 ?
