Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The title salt crystallizes in an almost identical cell to that of (NH4)6[H6W12O42]·10H2O [Averbuch-Pouchot, Tordjman, Durif & Guitel (1979). Acta Cryst. B35, 1675-1677]. While the centrosymmetric anion coordinates are isomorphous, refinement confirms the different ammonium cation and water content, even though the H atoms cannot be unambig­uously determined.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016963/tk6075sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016963/tk6075Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 168 K
  • Mean [sigma](W-O) = 0.012 Å
  • H-atom completeness 1%
  • Disorder in solvent or counterion
  • R factor = 0.051
  • wR factor = 0.128
  • Data-to-parameter ratio = 28.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
ABSTM_02 Alert A Crystal and compound unsuitable for non-numerical corrections. Product of mu and tmid > 3.0 Value of mu given = 26.200 tmid = 0.140
Author response: The collection of a full sphere of data, used in the analytical correction, was considered adequate for the purposes of the required structural solution and identification.

Yellow Alert Alert Level C:
ABSMU_01 Alert C The ratio of given/expected absorption coefficient lies outside the range 0.99 <> 1.01 Calculated value of mu = 27.155 Value of mu given = 26.200 DIFMX_01 Alert C The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 6.040 Test value = 5.550 DIFMX_02 Alert C The minimum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 33 PLAT_302 Alert C Anion/Solvent Disorder ....................... 3.00 Perc. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H60 N10 O51 W12 Atom count from the _atom_site data: N10 O51 W12 CELLZ_01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum H60 N10 O51 W12 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 120.00 0.00 120.00 N 20.00 20.00 0.00 O 102.00 102.00 0.00 W 24.00 24.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional? CHEMW_03 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 3222.78 TEST: Calculate formula weight from _atom_site_* atom mass num sum O 16.00 51.00 815.95 H 1.01 0.00 0.00 N 14.01 10.00 140.07 W 183.85 12.00 2206.20 Calculated formula weight 3162.22 The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
5 Alert Level C = Please check

Comment top

The title compound, (I), was prepared as a by-product while attempting to use aniline as an organic amine inter-layer spacer molecule for new inorganic oxide-layered compounds. The crystal structure comprises [H2W12O42]10− anions (Fig. 1) bound in an infinite three-dimensional network through hydrogen bonding with NH4+ cations and water molecules. There are at least 42 contacts between the anion O atoms, amine N atoms and water O atoms within normal hydrogen-bonding distances, e.g. O22···O2W 2.76 (2) Å.

The two independent anions per cell are centrosymmetric and are essentially identical (truly isomorphic) with those in (NH4)6[H6W12O42].10H2O (Averbuch-Pouchot et al., 1979, hereafter AVEPOU). The final cell composition is inferred from the consistency of the refined displacement parameters of the water O atoms and ammonium cation N atoms, the analytical data and the proximity of cations to each other, since the X-ray scattering of the H atoms cannot be determined unambiguously in the presence of the W atoms. The atom-numbering scheme for the anions follows that in AVEPOU, with the coordinates transformed into one asymmetric unit. The cell volume here is slightly larger [2542 (2) Å3 at 168 K compared with 2540 Å3 at 293 K for AVEPOU], as expected from the greater total number of cations and water molecules. Other structures found on the Cambridge Structural Database (Allen & Kennard, 1993; Conquest, 2002) containing the same [H2W12O42]10− anion are the closely related (NH4)10[H2W12O42].10H2O, which crystallizes in space group Pbca, as reported by Allman (1971) and a decasodium diglycine salt (Naruke et al., 2000). A summary of the expected geometry of the anions is given in the paper reporting Na10[H2W12O42].20H2O (Evans & Rollins, 1976). The internally self-consistent range of W—O distances are indicated in Table 1 by those found for W1.

A larger crystal from another preparation was also examined; it had a slightly smaller cell [2510 (1) Å3 at 168 K], but the diffraction data was not as good with an internal agreement Rint of 0.068 and the subsequent refinement was less stable. The isomorphicity of the anion coordinates reported here with those in the six-cation structure AVEPOU suggest that this larger crystal could be made up of plate-like twins, possibly with variable cation/water composition.

Experimental top

The compound was prepared as a by-product of the reaction of H2WO4 with aniline in an ammonia (0.1 N) solution and recrystallized from water [N% calculated (H60N10O51W12): 4.35%; found 4.33%].

Refinement top

No H atoms were included in the refinement. One disordered water O atom (O9WA) was refined over two sites with final occupancies 0.52 (3)/0.48 (3) and a common U value of 0.045 (6) Å2. The largest residual electron-density peak was located 0.99 Å from W6 and the deepest hole 1.07 Å from W7.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996) and SADABS (Sheldrick, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 in WinGX (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of one of the two independent [H2W12O42]10− anions. Displacement ellipsoids are drawn at the 50% probablity level (Farrugia, 1997) and centrosymmetrically related atom labels have been omitted.
(I) top
Crystal data top
(NH4)10[H2W12O42]·9H2OZ = 2
Mr = 3222.78F(000) = 2852
Triclinic, P1Dx = 4.211 Mg m3
a = 11.945 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.225 (5) ÅCell parameters from 8000 reflections
c = 16.780 (6) Åθ = 2.3–26.3°
α = 76.159 (5)°µ = 26.20 mm1
β = 80.985 (5)°T = 168 K
γ = 88.763 (5)°Plate, colourless
V = 2541.6 (15) Å30.44 × 0.14 × 0.06 mm
Data collection top
Siemens CCD area-detector
diffractometer
10192 independent reflections
Radiation source: fine-focus sealed tube7208 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
Detector resolution: 8.192 pixels mm-1θmax = 26.5°, θmin = 2.3°
ϕ and ω scansh = 1414
Absorption correction: multi-scan
(Blessing, 1995)
k = 1616
Tmin = 0.355, Tmax = 0.592l = 2020
32370 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128 w = 1/[σ2(Fo2) + (0.0765P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.99(Δ/σ)max = 0.001
10192 reflectionsΔρmax = 6.04 e Å3
357 parametersΔρmin = 5.45 e Å3
0 restraints
Crystal data top
(NH4)10[H2W12O42]·9H2Oγ = 88.763 (5)°
Mr = 3222.78V = 2541.6 (15) Å3
Triclinic, P1Z = 2
a = 11.945 (4) ÅMo Kα radiation
b = 13.225 (5) ŵ = 26.20 mm1
c = 16.780 (6) ÅT = 168 K
α = 76.159 (5)°0.44 × 0.14 × 0.06 mm
β = 80.985 (5)°
Data collection top
Siemens CCD area-detector
diffractometer
10192 independent reflections
Absorption correction: multi-scan
(Blessing, 1995)
7208 reflections with I > 2σ(I)
Tmin = 0.355, Tmax = 0.592Rint = 0.047
32370 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.051357 parameters
wR(F2) = 0.1280 restraints
S = 0.99Δρmax = 6.04 e Å3
10192 reflectionsΔρmin = 5.45 e Å3
Special details top

Experimental. Crystal decay was monitored by repeating the initial 10 frames at the end of the data collection and analyzing duplicate reflections. The standard 0.8 mm diameter collimator was used.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. No hydrogen atoms were located and refined. The final fourier difference map peaks and troughs are all within 1.2 Å of W or anion oxygen atoms.

Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
W10.74798 (6)0.95682 (6)0.37941 (4)0.01354 (17)
W20.73015 (6)0.54717 (5)0.00374 (4)0.01202 (16)
W30.79439 (6)0.26622 (6)0.03953 (4)0.01433 (17)
W40.24171 (5)0.83230 (6)0.50908 (4)0.01244 (16)
W50.63869 (6)0.33572 (6)0.19582 (4)0.01309 (17)
W60.77893 (6)0.71536 (6)0.49179 (4)0.01443 (17)
W70.57800 (6)0.61552 (6)0.15959 (4)0.01321 (17)
W80.48069 (6)0.27743 (5)0.03180 (4)0.01227 (16)
W90.72927 (6)0.36805 (6)0.85211 (4)0.01396 (17)
W100.97795 (6)0.69413 (6)0.61159 (4)0.01386 (17)
W110.03978 (6)0.86744 (6)0.38909 (4)0.01235 (16)
W120.79219 (6)0.93179 (5)0.60835 (4)0.01192 (16)
O10.7572 (10)0.8874 (9)0.5149 (7)0.019 (3)*
O20.6321 (10)0.6984 (10)0.5222 (8)0.023 (3)*
O30.8168 (10)0.6752 (9)0.6027 (7)0.018 (3)*
O40.9111 (10)0.8465 (9)0.6200 (7)0.018 (3)*
O50.6818 (10)0.6890 (9)0.9529 (7)0.016 (3)*
O60.8752 (10)0.5646 (9)0.0285 (7)0.017 (3)*
O70.4692 (10)0.1441 (9)0.0742 (7)0.018 (3)*
O80.6864 (10)0.8690 (9)0.6871 (7)0.015 (3)*
O90.9183 (10)0.2845 (10)0.0789 (8)0.023 (3)*
O100.2561 (9)0.9151 (9)0.5909 (7)0.013 (3)*
O110.5484 (10)0.2561 (10)0.2756 (7)0.019 (3)*
O120.5721 (10)0.4637 (10)0.2057 (8)0.021 (3)*
O130.3526 (10)0.7403 (9)0.5225 (7)0.016 (3)*
O140.7209 (9)0.4136 (9)0.0713 (7)0.012 (2)*
O150.7613 (11)0.3456 (10)0.2401 (8)0.024 (3)*
O161.0314 (10)0.5834 (10)0.5767 (7)0.020 (3)*
O170.1193 (9)0.7646 (9)0.5937 (7)0.012 (2)*
O180.6916 (9)0.2266 (9)0.1419 (7)0.014 (3)*
O190.8407 (10)0.3489 (9)0.0705 (7)0.016 (3)*
O200.4125 (9)0.5979 (9)0.1860 (7)0.012 (3)*
O210.3147 (9)0.9435 (9)0.4289 (7)0.014 (3)*
O220.6330 (9)0.2925 (9)0.0215 (7)0.013 (3)*
O230.7434 (10)0.2434 (10)0.8315 (8)0.021 (3)*
O240.1003 (9)0.9479 (8)0.4842 (7)0.008 (2)*
O250.1766 (10)0.7846 (9)0.4322 (7)0.015 (3)*
O260.1567 (9)0.9705 (9)0.3326 (7)0.014 (3)*
O270.8166 (10)0.4451 (9)0.7695 (7)0.018 (3)*
O280.0291 (10)0.8051 (9)0.3120 (7)0.017 (3)*
O290.8118 (10)0.1420 (9)0.0179 (7)0.016 (3)*
O300.6922 (10)0.4991 (9)0.0899 (7)0.017 (3)*
O310.5434 (9)0.5611 (9)0.0472 (7)0.012 (2)*
O320.9556 (9)0.7730 (9)0.4819 (7)0.014 (3)*
O330.6062 (10)0.6618 (10)0.2421 (8)0.022 (3)*
O340.5994 (10)0.9378 (10)0.3947 (7)0.020 (3)*
O350.7828 (9)0.8110 (9)0.3847 (7)0.014 (3)*
O360.5550 (9)0.7400 (9)0.0831 (7)0.013 (3)*
O370.9281 (9)0.9651 (8)0.3834 (6)0.008 (2)*
O380.7754 (10)0.9995 (9)0.2702 (7)0.019 (3)*
O390.7213 (9)0.5994 (9)0.1060 (7)0.013 (3)*
O400.8211 (11)0.6054 (10)0.4563 (8)0.028 (3)*
O410.5052 (10)0.3325 (10)0.1132 (7)0.019 (3)*
O420.9603 (10)0.6513 (10)0.7193 (8)0.020 (3)*
O1W0.1030 (13)0.7632 (12)1.0322 (10)0.043 (4)*
O2W0.3456 (12)0.8820 (11)0.2535 (9)0.033 (3)*
O3W0.5940 (11)0.9221 (11)0.1167 (8)0.029 (3)*
O4W0.4676 (12)0.9492 (11)0.7699 (9)0.036 (4)*
O5W0.0691 (12)0.8292 (11)0.7559 (9)0.037 (4)*
O6W0.8432 (12)0.6733 (12)0.2592 (9)0.038 (4)*
O7W0.8190 (11)0.9533 (11)0.1215 (8)0.030 (3)*
O8W0.1458 (15)1.0431 (14)0.0771 (11)0.058 (5)*
O9WA0.483 (3)0.533 (2)0.548 (2)0.045 (6)*0.52 (3)
O9WB0.485 (3)0.541 (3)0.606 (2)0.045 (6)*0.48 (3)
N10.0376 (14)0.5051 (13)0.8531 (10)0.028 (4)*
N20.4886 (14)0.7698 (13)0.3589 (10)0.030 (4)*
N30.5117 (12)0.8746 (12)0.5726 (9)0.019 (3)*
N40.1081 (14)0.5867 (13)0.4019 (10)0.031 (4)*
N50.6703 (14)0.6391 (13)0.7488 (10)0.030 (4)*
N60.3588 (14)0.9477 (13)0.0542 (10)0.029 (4)*
N70.0286 (14)0.8380 (13)0.1376 (10)0.027 (4)*
N80.8216 (14)0.8202 (14)0.8280 (11)0.033 (4)*
N90.359 (2)0.574 (2)0.3631 (17)0.087 (9)*
N100.2488 (15)0.5320 (14)0.6392 (11)0.036 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.0086 (3)0.0164 (4)0.0148 (4)0.0019 (3)0.0054 (3)0.0000 (3)
W20.0076 (3)0.0139 (4)0.0131 (4)0.0011 (3)0.0025 (3)0.0003 (3)
W30.0097 (3)0.0176 (4)0.0141 (4)0.0033 (3)0.0034 (3)0.0000 (3)
W40.0063 (3)0.0140 (4)0.0157 (4)0.0025 (3)0.0036 (3)0.0000 (3)
W50.0101 (3)0.0148 (4)0.0125 (4)0.0015 (3)0.0033 (3)0.0013 (3)
W60.0094 (3)0.0145 (4)0.0186 (4)0.0009 (3)0.0043 (3)0.0010 (3)
W70.0102 (3)0.0156 (4)0.0133 (4)0.0019 (3)0.0041 (3)0.0011 (3)
W80.0085 (3)0.0133 (4)0.0136 (4)0.0011 (3)0.0037 (3)0.0007 (3)
W90.0099 (3)0.0174 (4)0.0133 (4)0.0029 (3)0.0027 (3)0.0007 (3)
W100.0092 (3)0.0148 (4)0.0152 (4)0.0008 (3)0.0033 (3)0.0018 (3)
W110.0072 (3)0.0157 (4)0.0130 (4)0.0011 (3)0.0026 (3)0.0005 (3)
W120.0068 (3)0.0139 (4)0.0133 (4)0.0010 (3)0.0025 (3)0.0009 (3)
Geometric parameters (Å, º) top
W1—O381.764 (12)W8—O221.889 (11)
W1—O341.768 (12)W8—O5iii1.972 (11)
W1—O10i1.874 (12)W8—O36iv2.104 (11)
W1—O351.947 (12)W8—O31iv2.267 (11)
W1—O372.168 (10)W9—O271.722 (12)
W1—O12.258 (12)W9—O231.763 (13)
W2—O61.725 (12)W9—O20iii1.910 (11)
W2—O301.832 (12)W9—O19v1.972 (11)
W2—O141.902 (11)W9—O30v2.188 (12)
W2—O5ii1.952 (12)W9—O22v2.257 (11)
W2—O392.103 (11)W10—O421.740 (12)
W2—O312.281 (11)W10—O161.774 (12)
W3—O91.757 (12)W10—O17vi1.893 (11)
W3—O291.766 (12)W10—O31.979 (12)
W3—O191.911 (11)W10—O42.179 (12)
W3—O181.916 (11)W10—O322.232 (11)
W3—O142.265 (11)W11—O281.714 (12)
W3—O222.304 (11)W11—O37vii1.835 (10)
W4—O131.783 (12)W11—O32vii1.905 (11)
W4—O251.842 (11)W11—O261.938 (11)
W4—O211.864 (11)W11—O252.075 (11)
W4—O171.938 (11)W11—O242.326 (11)
W4—O101.979 (11)W12—O81.740 (12)
W4—O242.273 (10)W12—O41.800 (12)
W5—O111.728 (12)W12—O11.906 (12)
W5—O151.763 (12)W12—O26i1.964 (12)
W5—O121.886 (12)W12—O21i2.099 (11)
W5—O181.925 (12)W12—O24i2.208 (11)
W5—O142.183 (11)O5—W2v1.952 (12)
W5—O412.278 (12)O5—W8iii1.972 (11)
W6—O401.735 (14)O10—W1i1.874 (12)
W6—O21.752 (12)O17—W10vii1.893 (11)
W6—O351.929 (11)O19—W9ii1.972 (11)
W6—O31.931 (12)O20—W9iii1.910 (11)
W6—O322.228 (11)O21—W12i2.099 (11)
W6—O12.400 (12)O22—W9ii2.257 (11)
W7—O331.721 (13)O24—W12i2.208 (11)
W7—O391.838 (11)O26—W12i1.964 (12)
W7—O361.875 (11)O30—W9ii2.188 (12)
W7—O201.964 (11)O31—W8iv2.267 (11)
W7—O121.970 (12)O32—W11vi1.905 (11)
W7—O312.270 (11)O36—W8iv2.104 (11)
W8—O71.736 (12)O37—W11vi1.835 (10)
W8—O411.759 (12)O9WA—O9WB1.01 (4)
O38—W1—O34100.1 (5)O7—W8—O5iii98.7 (5)
O38—W1—O10i100.4 (5)O41—W8—O5iii92.2 (5)
O34—W1—O10i95.9 (5)O22—W8—O5iii155.8 (5)
O38—W1—O3596.4 (5)O7—W8—O36iv91.9 (5)
O34—W1—O3594.8 (5)O41—W8—O36iv162.3 (5)
O10i—W1—O35158.1 (5)O22—W8—O36iv84.8 (5)
O38—W1—O3789.7 (5)O5iii—W8—O36iv81.9 (5)
O34—W1—O37169.9 (5)O7—W8—O31iv162.1 (5)
O10i—W1—O3784.4 (4)O41—W8—O31iv89.8 (5)
O35—W1—O3781.8 (4)O22—W8—O31iv85.8 (4)
O38—W1—O1165.8 (5)O5iii—W8—O31iv71.0 (4)
O34—W1—O192.4 (5)O36iv—W8—O31iv72.5 (4)
O10i—W1—O184.8 (5)O27—W9—O23103.1 (6)
O35—W1—O175.7 (5)O27—W9—O20iii98.6 (5)
O37—W1—O177.6 (4)O23—W9—O20iii97.8 (5)
O6—W2—O30103.5 (5)O27—W9—O19v95.4 (5)
O6—W2—O14100.4 (5)O23—W9—O19v96.4 (5)
O30—W2—O1494.5 (5)O20iii—W9—O19v157.3 (5)
O6—W2—O5ii100.0 (5)O27—W9—O30v91.5 (5)
O30—W2—O5ii93.9 (5)O23—W9—O30v164.9 (5)
O14—W2—O5ii155.4 (5)O20iii—W9—O30v83.6 (5)
O6—W2—O3993.5 (5)O19v—W9—O30v78.2 (5)
O30—W2—O39163.0 (5)O27—W9—O22v165.5 (5)
O14—W2—O3983.0 (5)O23—W9—O22v88.3 (5)
O5ii—W2—O3982.2 (5)O20iii—W9—O22v88.7 (4)
O6—W2—O31163.8 (5)O19v—W9—O22v74.1 (4)
O30—W2—O3190.9 (5)O30v—W9—O22v76.8 (4)
O14—W2—O3185.7 (4)O42—W10—O16103.5 (6)
O5ii—W2—O3171.0 (4)O42—W10—O17vi99.1 (5)
O39—W2—O3172.2 (4)O16—W10—O17vi96.2 (5)
O9—W3—O29103.5 (6)O42—W10—O395.4 (5)
O9—W3—O1996.9 (5)O16—W10—O397.7 (5)
O29—W3—O1998.3 (5)O17vi—W10—O3157.0 (5)
O9—W3—O1899.3 (5)O42—W10—O491.4 (5)
O29—W3—O1898.2 (5)O16—W10—O4165.0 (5)
O19—W3—O18153.5 (5)O17vi—W10—O482.9 (5)
O9—W3—O1490.7 (5)O3—W10—O478.9 (5)
O29—W3—O14164.2 (5)O42—W10—O32163.7 (5)
O19—W3—O1486.8 (4)O16—W10—O3289.7 (5)
O18—W3—O1472.2 (4)O17vi—W10—O3288.9 (4)
O9—W3—O22163.9 (5)O3—W10—O3273.0 (4)
O29—W3—O2291.2 (5)O4—W10—O3275.3 (4)
O19—W3—O2274.0 (4)O28—W11—O37vii105.9 (5)
O18—W3—O2285.0 (4)O28—W11—O32vii100.3 (5)
O14—W3—O2275.8 (4)O37vii—W11—O32vii93.5 (5)
O13—W4—O2598.9 (5)O28—W11—O26100.5 (5)
O13—W4—O21102.1 (5)O37vii—W11—O2692.6 (5)
O25—W4—O2192.8 (5)O32vii—W11—O26155.8 (5)
O13—W4—O17102.2 (5)O28—W11—O2596.7 (5)
O25—W4—O1788.6 (5)O37vii—W11—O25157.4 (5)
O21—W4—O17155.1 (5)O32vii—W11—O2582.9 (5)
O13—W4—O10103.4 (5)O26—W11—O2582.6 (5)
O25—W4—O10157.4 (5)O28—W11—O24166.3 (5)
O21—W4—O1086.5 (5)O37vii—W11—O2485.0 (4)
O17—W4—O1082.8 (5)O32vii—W11—O2487.0 (4)
O13—W4—O24176.5 (5)O26—W11—O2470.2 (4)
O25—W4—O2478.0 (4)O25—W11—O2472.6 (4)
O21—W4—O2476.7 (4)O8—W12—O4103.5 (5)
O17—W4—O2479.2 (4)O8—W12—O1101.9 (5)
O10—W4—O2479.8 (4)O4—W12—O193.6 (5)
O11—W5—O15103.7 (6)O8—W12—O26i97.4 (5)
O11—W5—O1297.4 (6)O4—W12—O26i95.5 (5)
O15—W5—O1299.0 (6)O1—W12—O26i156.1 (5)
O11—W5—O1895.2 (5)O8—W12—O21i91.5 (5)
O15—W5—O1896.7 (5)O4—W12—O21i164.8 (5)
O12—W5—O18156.9 (5)O1—W12—O21i84.7 (5)
O11—W5—O14161.3 (5)O26i—W12—O21i80.8 (4)
O15—W5—O1492.8 (5)O8—W12—O24i163.2 (5)
O12—W5—O1488.4 (5)O4—W12—O24i91.0 (5)
O18—W5—O1474.0 (4)O1—W12—O24i85.4 (5)
O11—W5—O4187.4 (5)O26i—W12—O24i72.5 (4)
O15—W5—O41168.1 (5)O21i—W12—O24i73.8 (4)
O12—W5—O4183.6 (5)W12—O1—W1138.3 (6)
O18—W5—O4177.7 (5)W12—O1—W6126.5 (6)
O14—W5—O4175.5 (4)W1—O1—W691.7 (4)
O40—W6—O2104.3 (6)W6—O3—W10115.8 (6)
O40—W6—O3597.5 (6)W12—O4—W10145.6 (7)
O2—W6—O3599.9 (5)W2v—O5—W8iii119.9 (6)
O40—W6—O3100.2 (6)W1i—O10—W4150.5 (6)
O2—W6—O395.9 (5)W5—O12—W7145.1 (7)
O35—W6—O3152.5 (5)W2—O14—W5139.9 (6)
O40—W6—O3293.9 (5)W2—O14—W3124.9 (5)
O2—W6—O32160.6 (5)W5—O14—W394.9 (4)
O35—W6—O3284.0 (4)W10vii—O17—W4144.0 (6)
O3—W6—O3274.0 (5)W3—O18—W5117.1 (6)
O40—W6—O1166.0 (5)W3—O19—W9ii117.3 (6)
O2—W6—O187.4 (5)W9iii—O20—W7146.1 (6)
O35—W6—O172.7 (4)W4—O21—W12i113.8 (5)
O3—W6—O185.8 (5)W8—O22—W9ii137.7 (6)
O32—W6—O175.5 (4)W8—O22—W3127.7 (5)
O33—W7—O39102.0 (5)W9ii—O22—W393.3 (4)
O33—W7—O36101.1 (5)W12i—O24—W495.7 (4)
O39—W7—O3693.3 (5)W12i—O24—W1196.2 (4)
O33—W7—O20100.9 (5)W4—O24—W1192.9 (4)
O39—W7—O20156.4 (5)W4—O25—W11116.5 (6)
O36—W7—O2087.7 (5)W11—O26—W12i119.8 (6)
O33—W7—O12102.3 (5)W2—O30—W9ii139.2 (6)
O39—W7—O1287.6 (5)W8iv—O31—W795.6 (4)
O36—W7—O12155.8 (5)W8iv—O31—W296.7 (4)
O20—W7—O1282.0 (5)W7—O31—W294.6 (4)
O33—W7—O31177.6 (5)W11vi—O32—W6126.6 (5)
O39—W7—O3177.3 (4)W11vi—O32—W10137.3 (6)
O36—W7—O3176.7 (4)W6—O32—W1095.9 (4)
O20—W7—O3180.1 (4)W6—O35—W1119.2 (6)
O12—W7—O3180.0 (5)W7—O36—W8iv115.2 (6)
O7—W8—O41105.5 (6)W11vi—O37—W1132.9 (6)
O7—W8—O22101.8 (5)W7—O39—W2116.0 (5)
O41—W8—O2294.4 (5)W8—O41—W5140.2 (7)
O8—W12—O1—W1137.3 (9)O41—W8—O22—W339.8 (7)
O4—W12—O1—W1118.1 (9)O5iii—W8—O22—W3145.4 (9)
O26i—W12—O1—W15.8 (18)O36iv—W8—O22—W3157.9 (7)
O21i—W12—O1—W146.8 (9)O31iv—W8—O22—W3129.3 (7)
O24i—W12—O1—W127.3 (9)O9—W3—O22—W8104.1 (18)
O8—W12—O1—W670.4 (7)O29—W3—O22—W8100.3 (7)
O4—W12—O1—W634.3 (7)O19—W3—O22—W8161.4 (8)
O26i—W12—O1—W6146.6 (9)O18—W3—O22—W82.2 (7)
O21i—W12—O1—W6160.8 (7)O14—W3—O22—W870.7 (7)
O24i—W12—O1—W6125.0 (7)O9—W3—O22—W9ii64.9 (19)
O38—W1—O1—W1295 (2)O29—W3—O22—W9ii90.7 (5)
O34—W1—O1—W12113.3 (9)O19—W3—O22—W9ii7.5 (4)
O10i—W1—O1—W1217.6 (9)O18—W3—O22—W9ii171.2 (5)
O35—W1—O1—W12152.3 (10)O14—W3—O22—W9ii98.2 (4)
O37—W1—O1—W1267.8 (9)O25—W4—O24—W12i96.6 (5)
O38—W1—O1—W663 (2)O21—W4—O24—W12i0.7 (4)
O34—W1—O1—W688.6 (5)O17—W4—O24—W12i172.6 (5)
O10i—W1—O1—W6175.7 (5)O10—W4—O24—W12i88.1 (4)
O35—W1—O1—W65.8 (4)O25—W4—O24—W110.0 (4)
O37—W1—O1—W690.3 (4)O21—W4—O24—W1195.8 (5)
O40—W6—O1—W12110 (2)O17—W4—O24—W1190.9 (4)
O2—W6—O1—W12102.7 (8)O10—W4—O24—W11175.4 (5)
O35—W6—O1—W12156.1 (8)O28—W11—O24—W12i57 (2)
O3—W6—O1—W126.6 (7)O37vii—W11—O24—W12i86.7 (4)
O32—W6—O1—W1267.9 (7)O32vii—W11—O24—W12i179.5 (5)
O40—W6—O1—W152 (2)O26—W11—O24—W12i7.9 (4)
O2—W6—O1—W195.3 (5)O25—W11—O24—W12i96.1 (5)
O35—W6—O1—W15.9 (4)O28—W11—O24—W439 (2)
O3—W6—O1—W1168.6 (5)O37vii—W11—O24—W4177.3 (4)
O32—W6—O1—W194.1 (4)O32vii—W11—O24—W483.5 (4)
O40—W6—O3—W1081.2 (7)O26—W11—O24—W488.2 (5)
O2—W6—O3—W10173.1 (7)O25—W11—O24—W40.0 (4)
O35—W6—O3—W1048.1 (14)O13—W4—O25—W11178.5 (6)
O32—W6—O3—W1010.0 (6)O21—W4—O25—W1175.7 (6)
O1—W6—O3—W1086.2 (6)O17—W4—O25—W1179.3 (6)
O42—W10—O3—W6178.4 (7)O10—W4—O25—W1112.0 (16)
O16—W10—O3—W677.2 (7)O24—W4—O25—W110.0 (5)
O17vi—W10—O3—W649.3 (15)O28—W11—O25—W4171.3 (6)
O4—W10—O3—W688.0 (6)O37vii—W11—O25—W47.2 (16)
O32—W10—O3—W610.1 (6)O32vii—W11—O25—W489.1 (7)
O8—W12—O4—W1066.4 (12)O26—W11—O25—W471.5 (6)
O1—W12—O4—W1036.7 (12)O24—W11—O25—W40.0 (5)
O26i—W12—O4—W10165.4 (11)O28—W11—O26—W12i179.7 (6)
O21i—W12—O4—W10119.5 (18)O37vii—W11—O26—W12i73.6 (6)
O24i—W12—O4—W10122.1 (11)O32vii—W11—O26—W12i30.8 (15)
O42—W10—O4—W12106.3 (12)O25—W11—O26—W12i84.2 (6)
O16—W10—O4—W1267 (2)O24—W11—O26—W12i10.1 (5)
O17vi—W10—O4—W12154.7 (12)O6—W2—O30—W9ii59.9 (10)
O3—W10—O4—W1211.1 (11)O14—W2—O30—W9ii41.9 (10)
O32—W10—O4—W1264.0 (11)O5ii—W2—O30—W9ii161.3 (9)
O13—W4—O10—W1i140.8 (13)O39—W2—O30—W9ii122.6 (14)
O25—W4—O10—W1i50 (2)O31—W2—O30—W9ii127.7 (9)
O21—W4—O10—W1i39.1 (13)O39—W7—O31—W8iv96.7 (5)
O17—W4—O10—W1i118.3 (13)O36—W7—O31—W8iv0.1 (4)
O24—W4—O10—W1i38.0 (12)O20—W7—O31—W8iv89.9 (4)
O11—W5—O12—W7178.4 (12)O12—W7—O31—W8iv173.5 (5)
O15—W5—O12—W776.3 (12)O39—W7—O31—W20.5 (4)
O18—W5—O12—W756 (2)O36—W7—O31—W297.1 (5)
O14—W5—O12—W716.3 (12)O20—W7—O31—W2172.9 (5)
O41—W5—O12—W791.9 (12)O12—W7—O31—W289.4 (5)
O33—W7—O12—W5117.9 (12)O6—W2—O31—W8iv66.6 (17)
O39—W7—O12—W516.1 (12)O30—W2—O31—W8iv85.8 (5)
O36—W7—O12—W576.8 (17)O14—W2—O31—W8iv179.7 (5)
O20—W7—O12—W5142.6 (12)O5ii—W2—O31—W8iv8.1 (4)
O31—W7—O12—W561.3 (11)O39—W2—O31—W8iv95.8 (5)
O6—W2—O14—W5128.4 (9)O6—W2—O31—W729.6 (18)
O30—W2—O14—W5127.0 (9)O30—W2—O31—W7178.0 (5)
O5ii—W2—O14—W517.4 (17)O14—W2—O31—W783.5 (4)
O39—W2—O14—W536.0 (8)O5ii—W2—O31—W788.2 (5)
O31—W2—O14—W536.5 (9)O39—W2—O31—W70.4 (4)
O6—W2—O14—W359.6 (7)O40—W6—O32—W11vi92.6 (8)
O30—W2—O14—W345.0 (7)O2—W6—O32—W11vi107.5 (15)
O5ii—W2—O14—W3154.6 (9)O35—W6—O32—W11vi4.6 (7)
O39—W2—O14—W3152.0 (7)O3—W6—O32—W11vi168.0 (8)
O31—W2—O14—W3135.5 (6)O1—W6—O32—W11vi78.2 (7)
O11—W5—O14—W2107.8 (16)O40—W6—O32—W1091.5 (5)
O15—W5—O14—W299.6 (9)O2—W6—O32—W1068.5 (16)
O12—W5—O14—W20.7 (9)O35—W6—O32—W10171.4 (5)
O18—W5—O14—W2164.2 (10)O3—W6—O32—W108.0 (4)
O41—W5—O14—W283.1 (9)O1—W6—O32—W1097.8 (5)
O11—W5—O14—W365.7 (16)O42—W10—O32—W11vi121.3 (17)
O15—W5—O14—W387.0 (5)O16—W10—O32—W11vi94.5 (9)
O12—W5—O14—W3174.1 (5)O17vi—W10—O32—W11vi1.7 (9)
O18—W5—O14—W39.2 (4)O3—W10—O32—W11vi167.4 (10)
O41—W5—O14—W390.3 (4)O4—W10—O32—W11vi84.7 (9)
O9—W3—O14—W294.9 (7)O42—W10—O32—W653.9 (19)
O29—W3—O14—W2111.3 (17)O16—W10—O32—W690.2 (5)
O19—W3—O14—W22.0 (7)O17vi—W10—O32—W6173.6 (5)
O18—W3—O14—W2165.5 (8)O3—W10—O32—W67.9 (4)
O22—W3—O14—W276.3 (6)O4—W10—O32—W690.6 (5)
O9—W3—O14—W590.2 (5)O40—W6—O35—W1177.7 (7)
O29—W3—O14—W563.6 (18)O2—W6—O35—W176.3 (7)
O19—W3—O14—W5172.9 (5)O3—W6—O35—W147.9 (13)
O18—W3—O14—W59.3 (4)O32—W6—O35—W184.5 (6)
O22—W3—O14—W598.5 (4)O1—W6—O35—W17.9 (5)
O13—W4—O17—W10vii107.1 (11)O38—W1—O35—W6176.2 (6)
O25—W4—O17—W10vii8.4 (11)O34—W1—O35—W683.0 (7)
O21—W4—O17—W10vii85.2 (15)O10i—W1—O35—W636.2 (16)
O10—W4—O17—W10vii150.6 (11)O37—W1—O35—W687.4 (6)
O24—W4—O17—W10vii69.7 (10)O1—W1—O35—W68.3 (6)
O9—W3—O18—W575.9 (7)O33—W7—O36—W8iv179.1 (6)
O29—W3—O18—W5179.0 (6)O39—W7—O36—W8iv76.2 (6)
O19—W3—O18—W551.1 (14)O20—W7—O36—W8iv80.3 (6)
O14—W3—O18—W511.9 (5)O12—W7—O36—W8iv15.5 (15)
O22—W3—O18—W588.5 (6)O31—W7—O36—W8iv0.1 (5)
O11—W5—O18—W3176.6 (6)O38—W1—O37—W11vi96.5 (8)
O15—W5—O18—W378.8 (7)O34—W1—O37—W11vi71 (3)
O12—W5—O18—W353.8 (15)O10i—W1—O37—W11vi162.9 (8)
O14—W5—O18—W312.2 (5)O35—W1—O37—W11vi0.1 (7)
O41—W5—O18—W390.5 (6)O1—W1—O37—W11vi77.0 (8)
O9—W3—O19—W9ii176.1 (7)O33—W7—O39—W2178.2 (6)
O29—W3—O19—W9ii79.1 (7)O36—W7—O39—W276.1 (6)
O18—W3—O19—W9ii48.7 (14)O20—W7—O39—W215.8 (15)
O14—W3—O19—W9ii85.8 (6)O12—W7—O39—W279.7 (6)
O22—W3—O19—W9ii9.7 (5)O31—W7—O39—W20.6 (5)
O33—W7—O20—W9iii124.8 (11)O6—W2—O39—W7172.7 (6)
O39—W7—O20—W9iii69.2 (18)O30—W2—O39—W74.8 (19)
O36—W7—O20—W9iii23.9 (11)O14—W2—O39—W787.2 (6)
O12—W7—O20—W9iii134.1 (12)O5ii—W2—O39—W773.1 (6)
O31—W7—O20—W9iii53.0 (11)O31—W2—O39—W70.6 (5)
O13—W4—O21—W12i177.5 (6)O7—W8—O41—W565.4 (11)
O25—W4—O21—W12i77.8 (6)O22—W8—O41—W538.2 (10)
O17—W4—O21—W12i14.8 (14)O5iii—W8—O41—W5165.1 (10)
O10—W4—O21—W12i79.5 (6)O36iv—W8—O41—W5124.9 (14)
O24—W4—O21—W12i0.8 (5)O31iv—W8—O41—W5123.9 (10)
O7—W8—O22—W9ii129.5 (9)O11—W5—O41—W8106.4 (11)
O41—W8—O22—W9ii123.6 (9)O15—W5—O41—W853 (3)
O5iii—W8—O22—W9ii18.1 (17)O12—W5—O41—W8155.9 (11)
O36iv—W8—O22—W9ii38.6 (8)O18—W5—O41—W810.5 (10)
O31iv—W8—O22—W9ii34.2 (8)O14—W5—O41—W865.9 (10)
O7—W8—O22—W367.0 (8)
Symmetry codes: (i) x+1, y+2, z+1; (ii) x, y, z1; (iii) x+1, y+1, z+1; (iv) x+1, y+1, z; (v) x, y, z+1; (vi) x+1, y, z; (vii) x1, y, z.

Experimental details

Crystal data
Chemical formula(NH4)10[H2W12O42]·9H2O
Mr3222.78
Crystal system, space groupTriclinic, P1
Temperature (K)168
a, b, c (Å)11.945 (4), 13.225 (5), 16.780 (6)
α, β, γ (°)76.159 (5), 80.985 (5), 88.763 (5)
V3)2541.6 (15)
Z2
Radiation typeMo Kα
µ (mm1)26.20
Crystal size (mm)0.44 × 0.14 × 0.06
Data collection
DiffractometerSiemens CCD area-detector
diffractometer
Absorption correctionMulti-scan
(Blessing, 1995)
Tmin, Tmax0.355, 0.592
No. of measured, independent and
observed [I > 2σ(I)] reflections
32370, 10192, 7208
Rint0.047
(sin θ/λ)max1)0.628
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.128, 0.99
No. of reflections10192
No. of parameters357
Δρmax, Δρmin (e Å3)6.04, 5.45

Computer programs: SMART (Siemens, 1996), SMART, SAINT (Siemens, 1996) and SADABS (Sheldrick, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 in WinGX (Farrugia, 1997), SHELXL97.

Selected bond lengths (Å) top
W1—O381.764 (12)W1—O372.168 (10)
W1—O341.768 (12)W1—O12.258 (12)
W1—O10i1.874 (12)W6—O12.400 (12)
W1—O351.947 (12)
Symmetry code: (i) x+1, y+2, z+1.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds