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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110022869/fa3227sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110022869/fa3227Isup2.hkl
Contains datablock I

Computing details top

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)2WTe2O8F(000) = 520
Mr = 603.1Dx = 4.912 Mg m3
Monoclinic, P21Synchrotron radiation, λ = 0.3978 Å
Hall symbol: P 2ybCell parameters from 1027 reflections
a = 6.443 (1) Åθ = 1.8–21.2°
b = 6.883 (1) ŵ = 4.24 mm1
c = 9.301 (1) ÅT = 295 K
β = 98.8 (2)°Irregular plate shape, colourless
V = 407.7 (2) Å30.03 × 0.01 × 0.01 mm
Z = 2
Data collection top
Huber
diffractometer
599 independent reflections
Radiation source: Beamline D3, Hasylab599 reflections with I > 3σ(I)
ROMO monochromatorRint = 0.142
rotation method scansθmax = 21.2°, θmin = 1.8°
Absorption correction: numerical
(JANA2006; Petricek et al., 2006)
h = 1010
Tmin = 0.471, Tmax = 0.610k = 1110
1027 measured reflectionsl = 89
Refinement top
Refinement on FH-atom parameters not defined?
R[F > 3σ(F)] = 0.112Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
wR(F) = 0.095(Δ/σ)max = 0.006
S = 2.27Δρmax = 4.55 e Å3
599 reflectionsΔρmin = 4.06 e Å3
48 parametersAbsolute structure: refinement as inversion twin
0 restraintsAbsolute 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
xyzUiso*/Ueq
W10.3239 (6)0.42530.2616 (11)0.017 (3)
Te10.5450 (9)0.2104 (8)0.0057 (16)0.0052 (14)*
Te20.4640 (10)0.4748 (8)0.6432 (18)0.0073 (16)*
O10.180 (9)0.255 (7)0.296 (15)0.006 (5)*
O20.127 (8)0.593 (7)0.169 (14)0.006 (5)*
O30.441 (9)0.572 (7)0.442 (15)0.006 (5)*
O40.290 (9)0.274 (7)0.084 (14)0.006 (5)*
O50.566 (9)0.240 (7)0.290 (14)0.006 (5)*
O60.565 (9)0.564 (7)0.157 (15)0.006 (5)*
O70.509 (8)0.385 (6)0.148 (16)0.006 (5)*
O80.177 (7)0.391 (6)0.591 (13)0.006 (5)*
N10.034 (10)0.964 (9)0.107 (17)0.007*
N20.868 (11)0.519 (8)0.402 (19)0.007*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.0070 (14)0.0070 (12)0.037 (9)0.0018 (19)0.000 (3)0.003 (3)
Geometric parameters (Å, º) top
W1—O11.55 (7)O2—O42.60 (10)
W1—O21.83 (7)O2—O62.85 (9)
W1—O32.00 (11)O2—N12.67 (8)
W1—O41.93 (12)O2—N1vii2.76 (18)
W1—O52.00 (5)O2—N2vi2.96 (19)
W1—O62.18 (9)O3—O52.87 (12)
Te1—O2i2.97 (10)O3—O5ii2.75 (18)
Te1—O41.95 (9)O3—O62.88 (19)
Te1—O52.64 (13)O3—O82.66 (13)
Te1—O62.81 (8)O3—N22.86 (11)
Te1—O6i1.87 (11)O4—O52.42 (14)
Te1—O71.85 (12)O4—O62.69 (8)
Te1—O7i2.65 (9)O4—O6i2.94 (16)
Te2—O1ii2.98 (6)O4—O72.86 (17)
Te2—O31.97 (13)O4—N1v2.72 (9)
Te2—O3iii2.97 (6)O4—N1vii2.84 (13)
Te2—O5ii1.94 (6)O5—O62.55 (11)
Te2—O7iv2.02 (14)O5—O7i2.79 (11)
Te2—O81.93 (5)O5—N22.82 (9)
O1—O22.61 (10)O6—O7viii2.25 (7)
O1—O32.95 (10)O6—N22.78 (17)
O1—O42.19 (18)O7—O8ix2.98 (14)
O1—O52.49 (9)O7—N1i2.96 (8)
O1—O82.90 (18)O8—N2vi2.60 (13)
O1—N1v2.73 (14)O8—N2iii2.58 (7)
O1—N2vi2.99 (12)
O1—W1—O2100 (3)O6i—Te1—O774 (4)
O1—W1—O3112 (6)O6i—Te1—O7i84 (4)
O1—W1—O477 (5)O7—Te1—O7i157 (3)
O1—W1—O588 (3)O1ii—Te2—O385 (3)
O1—W1—O6156 (4)O1ii—Te2—O3iii118.1 (17)
O2—W1—O3103 (3)O1ii—Te2—O5ii56 (2)
O2—W1—O487 (4)O1ii—Te2—O7iv91 (3)
O2—W1—O5159 (5)O1ii—Te2—O8157.0 (17)
O2—W1—O690 (3)O3—Te2—O3iii93 (3)
O3—W1—O4165 (3)O3—Te2—O5ii89 (4)
O3—W1—O591 (3)O3—Te2—O7iv176 (2)
O3—W1—O687 (4)O3—Te2—O886 (4)
O4—W1—O576 (4)O3iii—Te2—O5ii174 (2)
O4—W1—O682 (4)O3iii—Te2—O7iv88 (3)
O5—W1—O675 (3)O3iii—Te2—O883 (2)
O2i—Te1—O4168 (4)O5ii—Te2—O7iv89 (4)
O2i—Te1—O5130 (2)O5ii—Te2—O8103 (2)
O2i—Te1—O6122 (2)O7iv—Te2—O898 (4)
O2i—Te1—O6i68 (3)W1—O1—Te2iii94 (3)
O2i—Te1—O777 (3)W1—O2—Te1viii86 (2)
O2i—Te1—O7i102 (2)W1—O3—Te2126 (3)
O4—Te1—O562 (4)W1—O3—Te2ii108 (5)
O4—Te1—O666 (2)Te2—O3—Te2ii126 (4)
O4—Te1—O6i101 (4)W1—O4—Te1117 (3)
O4—Te1—O797 (4)W1—O5—Te190 (4)
O4—Te1—O7i80 (3)W1—O5—Te2iii122 (4)
O5—Te1—O656 (3)Te1—O5—Te2iii105 (4)
O5—Te1—O6i144 (3)W1—O6—Te181.9 (16)
O5—Te1—O7135 (3)W1—O6—Te1viii113 (3)
O5—Te1—O7i64 (3)Te1—O6—Te1viii94 (5)
O6—Te1—O6i149 (3)Te1—O7—Te1viii100 (6)
O6—Te1—O780 (4)Te1—O7—Te2ix158 (5)
O6—Te1—O7i119 (4)
Symmetry codes: (i) x+1, y1/2, z; (ii) x+1, y+1/2, z+1; (iii) x+1, y1/2, z+1; (iv) x, y, z+1; (v) x, y1, z; (vi) x1, y, z; (vii) x, y1/2, z; (viii) x+1, y+1/2, z; (ix) x, y, z1.
Selected bond lengths in (Å) at ambient pressure and 5.09 GPa top
ambient5.09 GPa
W1-O11.733 (9)1.55 (7)
W1-O21.759 (9)1.83 (7)
W1-O31.834 (9)2.00 (11)
W1-O42.097 (8)1.93 (12)
W1-O52.110 (8)2.00 (5)
W1-O62.151 (8)2.18 (9)
Te1-O41.882 (8)1.95 (9)
Te1-O6i1.890 (8)1.87 (11)
Te1-O71.965 (9)1.85 (12)
Te1-O72.349 (9)2.65 (9)
Te2-O32.145 (9)1.97 (13)
Te2-O5ii1.878 (7)1.94 (6)
Te2-O7iv2.152 (8)2.02 (14)
Te2-O81.832 (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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