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The title compound, trisilver niobium niobate tetraoxide bis(arsenate), contains (NbAsO8)n corrugated layers crosslinked via NbO6 polyhedra to form a three-dimensional framework that delimits elliptical tunnels running along the a axis where the highly disordered Ag+ cations are located.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680604462X/hb2153sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680604462X/hb2153Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](As-O) = 0.005 Å
  • R factor = 0.032
  • wR factor = 0.086
  • Data-to-parameter ratio = 10.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT213_ALERT_2_C Atom Ag1 has ADP max/min Ratio ............. 3.10 prolat PLAT213_ALERT_2_C Atom Ag2 has ADP max/min Ratio ............. 3.10 prolat PLAT213_ALERT_2_C Atom Ag3 has ADP max/min Ratio ............. 3.10 prolat PLAT213_ALERT_2_C Atom Ag4 has ADP max/min Ratio ............. 3.10 prolat PLAT213_ALERT_2_C Atom Ag5 has ADP max/min Ratio ............. 3.10 prolat PLAT213_ALERT_2_C Atom Ag6 has ADP max/min Ratio ............. 3.10 prolat PLAT213_ALERT_2_C Atom Ag7 has ADP max/min Ratio ............. 3.10 prolat PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.34 PLAT301_ALERT_3_C Main Residue Disorder ......................... 9.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

trisilver niobium niobate tetraoxide bis(arsenate) top
Crystal data top
Ag3Nb(NbO)2O4(AsO4)2F(000) = 884
Mr = 976.18Dx = 5.392 Mg m3
Dm = non Mg m3
Dm measured by not measured
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 5.087 (1) Åθ = 10–16°
b = 8.713 (1) ŵ = 13.09 mm1
c = 13.740 (1) ÅT = 298 K
β = 99.11 (1)°Prism, colourless
V = 601.3 (1) Å30.20 × 0.10 × 0.07 mm
Z = 2
Data collection top
Enraf–Nonius CAD-4
diffractometer
1169 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.035
Graphite monochromatorθmax = 27.0°, θmin = 2.8°
ω/2θ scansh = 62
Absorption correction: ψ scan
(North et al., 1968)
k = 111
Tmin = 0.226, Tmax = 0.400l = 1717
1962 measured reflections2 standard reflections every 120 min
1299 independent reflections intensity decay: 1%
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)] = 0.032 w = 1/[σ2(Fo2) + (0.0366P)2 + 6.6131P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.086(Δ/σ)max = 0.007
S = 1.12Δρmax = 1.20 e Å3
1299 reflectionsΔρmin = 1.40 e Å3
123 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.0049 (4)
Special details top

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. 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)
Nb10.00000.00000.00000.0073 (2)
Nb20.44754 (11)0.26212 (7)0.37485 (4)0.00598 (19)
As10.12198 (13)0.08243 (8)0.23368 (5)0.00501 (19)
Ag10.544 (3)0.3606 (7)0.1152 (3)0.0155 (4)0.433 (11)
Ag20.003 (2)0.4912 (11)0.0141 (3)0.0155 (4)0.295 (9)
Ag30.461 (3)0.3376 (11)0.1093 (3)0.0155 (4)0.361 (10)
Ag40.378 (4)0.3092 (17)0.1072 (7)0.0155 (4)0.098 (9)
Ag50.022 (3)0.4553 (18)0.0066 (11)0.0155 (4)0.132 (10)
Ag60.0225 (18)0.4223 (9)0.0463 (7)0.0155 (4)0.091 (2)
Ag70.634 (5)0.3762 (17)0.1147 (10)0.0155 (4)0.087 (9)
O10.3248 (9)0.0710 (5)0.0833 (3)0.0100 (9)
O20.0838 (10)0.1251 (6)0.1156 (3)0.0101 (10)
O30.1654 (10)0.0933 (6)0.3122 (4)0.0128 (10)
O40.2388 (9)0.0968 (5)0.2425 (3)0.0086 (9)
O50.3465 (10)0.2162 (6)0.2564 (3)0.0111 (10)
O60.1933 (9)0.3210 (6)0.4590 (3)0.0100 (10)
O70.6287 (10)0.1112 (6)0.4462 (4)0.0125 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0077 (4)0.0093 (4)0.0052 (4)0.0007 (3)0.0025 (3)0.0003 (3)
Nb20.0056 (3)0.0082 (3)0.0034 (3)0.0021 (2)0.0017 (2)0.0002 (2)
As10.0046 (3)0.0068 (3)0.0033 (3)0.0002 (2)0.0005 (2)0.0012 (2)
Ag10.0182 (12)0.0132 (16)0.0139 (6)0.0122 (16)0.0010 (18)0.0029 (8)
Ag20.0182 (12)0.0132 (16)0.0139 (6)0.0122 (16)0.0010 (18)0.0029 (8)
Ag30.0182 (12)0.0132 (16)0.0139 (6)0.0122 (16)0.0010 (18)0.0029 (8)
Ag40.0182 (12)0.0132 (16)0.0139 (6)0.0122 (16)0.0010 (18)0.0029 (8)
Ag50.0182 (12)0.0132 (16)0.0139 (6)0.0122 (16)0.0010 (18)0.0029 (8)
Ag60.0182 (12)0.0132 (16)0.0139 (6)0.0122 (16)0.0010 (18)0.0029 (8)
Ag70.0182 (12)0.0132 (16)0.0139 (6)0.0122 (16)0.0010 (18)0.0029 (8)
O10.010 (2)0.007 (2)0.012 (2)0.0026 (19)0.0020 (18)0.0032 (18)
O20.014 (2)0.013 (2)0.005 (2)0.0020 (19)0.0041 (18)0.0009 (18)
O30.012 (2)0.012 (2)0.011 (2)0.000 (2)0.0080 (19)0.0015 (19)
O40.010 (2)0.010 (2)0.004 (2)0.0036 (19)0.0030 (17)0.0008 (18)
O50.012 (2)0.012 (2)0.009 (2)0.0039 (19)0.0038 (18)0.0003 (19)
O60.010 (2)0.012 (2)0.009 (2)0.0024 (19)0.0034 (17)0.0009 (19)
O70.013 (2)0.013 (2)0.010 (2)0.001 (2)0.0036 (19)0.0037 (19)
Geometric parameters (Å, º) top
Nb1—O1i1.955 (5)Ag1—O7iv2.452 (6)
Nb1—O11.955 (5)Ag2—O7vii2.149 (11)
Nb1—O2i2.026 (5)Ag2—O7iv2.166 (11)
Nb1—O22.026 (5)Ag3—O5v2.353 (7)
Nb1—O6ii1.973 (5)Ag3—O7iv2.522 (9)
Nb1—O6iii1.973 (5)Ag3—O4vi2.545 (8)
Nb2—O71.804 (5)Ag3—O7ii2.560 (10)
Nb2—O61.935 (5)Ag4—O4vi2.429 (12)
Nb2—O1iv1.891 (5)Ag4—O5v2.430 (11)
Nb2—O5v2.109 (5)Ag4—O6ii2.390 (13)
Nb2—O32.138 (5)Ag5—O7vii2.123 (16)
Nb2—O4vi2.168 (5)Ag5—O7iv2.248 (16)
As1—O31.676 (5)Ag6—O7vii2.262 (10)
As1—O41.682 (5)Ag6—O7iv2.410 (9)
As1—O51.695 (5)Ag7—O3iv2.304 (17)
As1—O21.706 (5)Ag7—O7ii2.315 (14)
Ag1—O5v2.306 (6)Ag7—O5v2.383 (17)
Ag1—O7ii2.441 (6)Ag7—O7iv2.514 (18)
O1i—Nb1—O1180.0 (4)O7—Nb2—O5v90.4 (2)
O1i—Nb1—O2i88.6 (2)O6—Nb2—O5v166.4 (2)
O1—Nb1—O2i91.4 (2)O1iv—Nb2—O5v91.5 (2)
O1i—Nb1—O291.4 (2)O7—Nb2—O388.3 (2)
O1—Nb1—O288.6 (2)O6—Nb2—O387.3 (2)
O2i—Nb1—O2180.0 (3)O1iv—Nb2—O3172.3 (2)
O1i—Nb1—O6ii89.8 (2)O5v—Nb2—O386.7 (2)
O1—Nb1—O6ii90.2 (2)O7—Nb2—O4vi165.0 (2)
O2i—Nb1—O6ii91.44 (19)O6—Nb2—O4vi89.95 (19)
O2—Nb1—O6ii88.56 (19)O1iv—Nb2—O4vi89.7 (2)
O1i—Nb1—O6iii90.2 (2)O5v—Nb2—O4vi77.18 (18)
O1—Nb1—O6iii89.8 (2)O3—Nb2—O4vi82.66 (19)
O2i—Nb1—O6iii88.56 (19)O3—As1—O4106.7 (2)
O2—Nb1—O6iii91.44 (19)O3—As1—O5112.8 (2)
O6ii—Nb1—O6iii180.0 (3)O4—As1—O5111.6 (2)
O7—Nb2—O6101.6 (2)O3—As1—O2112.4 (2)
O7—Nb2—O1iv99.2 (2)O4—As1—O2111.5 (2)
O6—Nb2—O1iv92.8 (2)O5—As1—O2101.9 (2)
Symmetry codes: (i) x, y, z; (ii) x, y+1/2, z1/2; (iii) x, y1/2, z+1/2; (iv) x+1, y+1/2, z+1/2; (v) x+1, y, z; (vi) x, y+1/2, z+1/2; (vii) x1, y+1/2, z1/2.
 

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