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The polar crystal structure of diammonium [octaoxidoditellurato(IV)]tungstate, (NH4)2WTe2O8, was studied at high pressures using single-crystal X-ray diffraction in a diamond-anvil cell at the HASYLAB synchrotron (DESY, Hamburg, Germany). No phase transition was observed up to 7.16 GPa. However, a full structure determination at 5.09 GPa shows that the coordination number of one of the two non-equivalent Te atoms has decreased from four to three.
Supporting information
Data collection: XDS (Kabsch, 2010); cell refinement: XDS (Kabsch, 2010); data reduction: XDS (Kabsch, 2010)
JANA2006 (Petricek et al., 2006); program(s) used to solve structure: SIR97 (Altomare et al., 1997); program(s) used to refine structure: JANA2006 (Petricek et al., 2006); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: JANA2006 (Petricek et al., 2006).
Diammonium [oxtaoxidoditellurato(IV)]tungstate
top
Crystal data top
(NH4)2WTe2O8 | F(000) = 520 |
Mr = 603.1 | Dx = 4.912 Mg m−3 |
Monoclinic, P21 | Synchrotron radiation, λ = 0.3978 Å |
Hall symbol: P 2yb | Cell parameters from 1027 reflections |
a = 6.443 (1) Å | θ = 1.8–21.2° |
b = 6.883 (1) Å | µ = 4.24 mm−1 |
c = 9.301 (1) Å | T = 295 K |
β = 98.8 (2)° | Irregular plate shape, colourless |
V = 407.7 (2) Å3 | 0.03 × 0.01 × 0.01 mm |
Z = 2 | |
Data collection top
Huber diffractometer | 599 independent reflections |
Radiation source: Beamline D3, Hasylab | 599 reflections with I > 3σ(I) |
ROMO monochromator | Rint = 0.142 |
rotation method scans | θmax = 21.2°, θmin = 1.8° |
Absorption correction: numerical (JANA2006; Petricek et al., 2006) | h = −10→10 |
Tmin = 0.471, Tmax = 0.610 | k = −11→10 |
1027 measured reflections | l = −8→9 |
Refinement top
Refinement on F | H-atom parameters not defined? |
R[F > 3σ(F)] = 0.112 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
wR(F) = 0.095 | (Δ/σ)max = 0.006 |
S = 2.27 | Δρmax = 4.55 e Å−3 |
599 reflections | Δρmin = −4.06 e Å−3 |
48 parameters | Absolute structure: refinement as inversion twin |
0 restraints | Absolute structure parameter: 0.0 (1) |
0 constraints | |
Special details top
Experimental. Synchrotron data: Beamline D3, Hasylab, Hamburg, Germany |
Refinement. Te, O and N isotropic. Displacement parameters of O restricted to be equal.
Displacement parameters of N not refined. No H-atoms taken into account. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
W1 | 0.3239 (6) | 0.4253 | 0.2616 (11) | 0.017 (3) | |
Te1 | 0.5450 (9) | 0.2104 (8) | 0.0057 (16) | 0.0052 (14)* | |
Te2 | 0.4640 (10) | 0.4748 (8) | 0.6432 (18) | 0.0073 (16)* | |
O1 | 0.180 (9) | 0.255 (7) | 0.296 (15) | 0.006 (5)* | |
O2 | 0.127 (8) | 0.593 (7) | 0.169 (14) | 0.006 (5)* | |
O3 | 0.441 (9) | 0.572 (7) | 0.442 (15) | 0.006 (5)* | |
O4 | 0.290 (9) | 0.274 (7) | 0.084 (14) | 0.006 (5)* | |
O5 | 0.566 (9) | 0.240 (7) | 0.290 (14) | 0.006 (5)* | |
O6 | 0.565 (9) | 0.564 (7) | 0.157 (15) | 0.006 (5)* | |
O7 | 0.509 (8) | 0.385 (6) | −0.148 (16) | 0.006 (5)* | |
O8 | 0.177 (7) | 0.391 (6) | 0.591 (13) | 0.006 (5)* | |
N1 | 0.034 (10) | 0.964 (9) | 0.107 (17) | 0.007* | |
N2 | 0.868 (11) | 0.519 (8) | 0.402 (19) | 0.007* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
W1 | 0.0070 (14) | 0.0070 (12) | 0.037 (9) | −0.0018 (19) | 0.000 (3) | 0.003 (3) |
Geometric parameters (Å, º) top
W1—O1 | 1.55 (7) | O2—O4 | 2.60 (10) |
W1—O2 | 1.83 (7) | O2—O6 | 2.85 (9) |
W1—O3 | 2.00 (11) | O2—N1 | 2.67 (8) |
W1—O4 | 1.93 (12) | O2—N1vii | 2.76 (18) |
W1—O5 | 2.00 (5) | O2—N2vi | 2.96 (19) |
W1—O6 | 2.18 (9) | O3—O5 | 2.87 (12) |
Te1—O2i | 2.97 (10) | O3—O5ii | 2.75 (18) |
Te1—O4 | 1.95 (9) | O3—O6 | 2.88 (19) |
Te1—O5 | 2.64 (13) | O3—O8 | 2.66 (13) |
Te1—O6 | 2.81 (8) | O3—N2 | 2.86 (11) |
Te1—O6i | 1.87 (11) | O4—O5 | 2.42 (14) |
Te1—O7 | 1.85 (12) | O4—O6 | 2.69 (8) |
Te1—O7i | 2.65 (9) | O4—O6i | 2.94 (16) |
Te2—O1ii | 2.98 (6) | O4—O7 | 2.86 (17) |
Te2—O3 | 1.97 (13) | O4—N1v | 2.72 (9) |
Te2—O3iii | 2.97 (6) | O4—N1vii | 2.84 (13) |
Te2—O5ii | 1.94 (6) | O5—O6 | 2.55 (11) |
Te2—O7iv | 2.02 (14) | O5—O7i | 2.79 (11) |
Te2—O8 | 1.93 (5) | O5—N2 | 2.82 (9) |
O1—O2 | 2.61 (10) | O6—O7viii | 2.25 (7) |
O1—O3 | 2.95 (10) | O6—N2 | 2.78 (17) |
O1—O4 | 2.19 (18) | O7—O8ix | 2.98 (14) |
O1—O5 | 2.49 (9) | O7—N1i | 2.96 (8) |
O1—O8 | 2.90 (18) | O8—N2vi | 2.60 (13) |
O1—N1v | 2.73 (14) | O8—N2iii | 2.58 (7) |
O1—N2vi | 2.99 (12) | | |
| | | |
O1—W1—O2 | 100 (3) | O6i—Te1—O7 | 74 (4) |
O1—W1—O3 | 112 (6) | O6i—Te1—O7i | 84 (4) |
O1—W1—O4 | 77 (5) | O7—Te1—O7i | 157 (3) |
O1—W1—O5 | 88 (3) | O1ii—Te2—O3 | 85 (3) |
O1—W1—O6 | 156 (4) | O1ii—Te2—O3iii | 118.1 (17) |
O2—W1—O3 | 103 (3) | O1ii—Te2—O5ii | 56 (2) |
O2—W1—O4 | 87 (4) | O1ii—Te2—O7iv | 91 (3) |
O2—W1—O5 | 159 (5) | O1ii—Te2—O8 | 157.0 (17) |
O2—W1—O6 | 90 (3) | O3—Te2—O3iii | 93 (3) |
O3—W1—O4 | 165 (3) | O3—Te2—O5ii | 89 (4) |
O3—W1—O5 | 91 (3) | O3—Te2—O7iv | 176 (2) |
O3—W1—O6 | 87 (4) | O3—Te2—O8 | 86 (4) |
O4—W1—O5 | 76 (4) | O3iii—Te2—O5ii | 174 (2) |
O4—W1—O6 | 82 (4) | O3iii—Te2—O7iv | 88 (3) |
O5—W1—O6 | 75 (3) | O3iii—Te2—O8 | 83 (2) |
O2i—Te1—O4 | 168 (4) | O5ii—Te2—O7iv | 89 (4) |
O2i—Te1—O5 | 130 (2) | O5ii—Te2—O8 | 103 (2) |
O2i—Te1—O6 | 122 (2) | O7iv—Te2—O8 | 98 (4) |
O2i—Te1—O6i | 68 (3) | W1—O1—Te2iii | 94 (3) |
O2i—Te1—O7 | 77 (3) | W1—O2—Te1viii | 86 (2) |
O2i—Te1—O7i | 102 (2) | W1—O3—Te2 | 126 (3) |
O4—Te1—O5 | 62 (4) | W1—O3—Te2ii | 108 (5) |
O4—Te1—O6 | 66 (2) | Te2—O3—Te2ii | 126 (4) |
O4—Te1—O6i | 101 (4) | W1—O4—Te1 | 117 (3) |
O4—Te1—O7 | 97 (4) | W1—O5—Te1 | 90 (4) |
O4—Te1—O7i | 80 (3) | W1—O5—Te2iii | 122 (4) |
O5—Te1—O6 | 56 (3) | Te1—O5—Te2iii | 105 (4) |
O5—Te1—O6i | 144 (3) | W1—O6—Te1 | 81.9 (16) |
O5—Te1—O7 | 135 (3) | W1—O6—Te1viii | 113 (3) |
O5—Te1—O7i | 64 (3) | Te1—O6—Te1viii | 94 (5) |
O6—Te1—O6i | 149 (3) | Te1—O7—Te1viii | 100 (6) |
O6—Te1—O7 | 80 (4) | Te1—O7—Te2ix | 158 (5) |
O6—Te1—O7i | 119 (4) | | |
Symmetry codes: (i) −x+1, y−1/2, −z; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y−1/2, −z+1; (iv) x, y, z+1; (v) x, y−1, z; (vi) x−1, y, z; (vii) −x, y−1/2, −z; (viii) −x+1, y+1/2, −z; (ix) x, y, z−1. |
Selected bond lengths in (Å) at ambient pressure and 5.09 GPa top | ambient | 5.09 GPa |
W1-O1 | 1.733 (9) | 1.55 (7) |
W1-O2 | 1.759 (9) | 1.83 (7) |
W1-O3 | 1.834 (9) | 2.00 (11) |
W1-O4 | 2.097 (8) | 1.93 (12) |
W1-O5 | 2.110 (8) | 2.00 (5) |
W1-O6 | 2.151 (8) | 2.18 (9) |
Te1-O4 | 1.882 (8) | 1.95 (9) |
Te1-O6i | 1.890 (8) | 1.87 (11) |
Te1-O7 | 1.965 (9) | 1.85 (12) |
Te1-O7 | 2.349 (9) | 2.65 (9) |
Te2-O3 | 2.145 (9) | 1.97 (13) |
Te2-O5ii | 1.878 (7) | 1.94 (6) |
Te2-O7iv | 2.152 (8) | 2.02 (14) |
Te2-O8 | 1.832 (8) | 1.93 (5) |
Notes: Ambient pressure data from Kim et al. (2007).
Symmetry Codes: (i) -x+1,y-1/2,-z; (ii) -x+1,y+1/2,-z+1;
(iv) x,y,z+1. |
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