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The crystal structure of the title compound, disilver(I) tetra­hydro­dodioxotellurate(VI), has been redetermined; it confirms the previous study [Fischer (1969). Monatsh. Chem. 100, 1809–1822] which was based on film data, but with higher precision, with all displacement factors refined anisotropically for non-H atoms and with the localization of the H atoms, which leads to a different hydrogen-bonding scheme from that originally proposed. The structure of Ag2[TeO2(OH)4] can be derived from a distorted hexa­gonal close packing of [TeO2(OH)4]2− octa­hedra (Te site symmetry 2) with the Ag+ cations located in the inter­stices. O—H...O hydrogen bonds help to stabilize the structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807007970/hb2295sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807007970/hb2295Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](g-Ag) = 0.001 Å
  • R factor = 0.033
  • wR factor = 0.039
  • Data-to-parameter ratio = 22.9

checkCIF/PLATON results

No syntax errors found



Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.107 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 34.92 From the CIF: _reflns_number_total 1167 Count of symmetry unique reflns 614 Completeness (_total/calc) 190.07% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 553 Fraction of Friedel pairs measured 0.901 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CAD-4 Software (Enraf–Nonius, 1989); cell refinement: CAD-4 Software; data reduction: HELENA implemented in PLATON (Spek, 2003); program(s) used to solve structure: coordinates taken from a previous refinement; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2006); software used to prepare material for publication: SHELXL97.

Disilver(I) tetrahydroxodioxotellurate(VI) top
Crystal data top
Ag2[TeO2(OH)4]F(000) = 1584
Mr = 443.37Dx = 5.561 Mg m3
Orthorhombic, Fdd2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: F 2 -2dCell parameters from 25 reflections
a = 18.5845 (18) Åθ = 11.3–16.2°
b = 6.4186 (7) ŵ = 12.75 mm1
c = 8.879 (1) ÅT = 293 K
V = 1059.1 (2) Å3Prism, light yellow
Z = 80.18 × 0.15 × 0.14 mm
Data collection top
Enraf–Nonius CAD-4
diffractometer
1140 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.107
Graphite monochromatorθmax = 34.9°, θmin = 4.1°
ω/2θ scansh = 2929
Absorption correction: numerical
(HABITUS; Herrendorf, 1997)
k = 1010
Tmin = 0.226, Tmax = 0.337l = 1414
4417 measured reflections3 standard reflections every 300 min
1167 independent reflections intensity decay: none
Refinement top
Refinement on F2Hydrogen site location: difference Fourier map
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.033 w = 1/[σ2(Fo2) + (0.0192P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.039(Δ/σ)max = 0.001
S = 1.09Δρmax = 1.91 e Å3
1167 reflectionsΔρmin = 3.14 e Å3
51 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
3 restraintsExtinction coefficient: 0.00918 (18)
Primary atom site location: isomorphous structure methodsAbsolute structure: Flack (1983), 554 Friedel pairs
Secondary atom site location: noneAbsolute structure parameter: 0.22 (2)
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*/Ueq
Te0.00000.00000.002000 (11)0.00736 (6)
Ag0.079916 (12)0.52615 (4)0.98669 (4)0.02515 (9)
O10.04247 (9)0.8207 (4)0.8601 (2)0.0109 (3)
O20.04460 (9)0.8320 (5)0.1599 (2)0.0161 (4)
O30.08359 (8)0.1808 (3)0.0064 (2)0.0130 (3)
H10.022 (4)0.787 (10)0.254 (5)0.037 (11)*
H20.129 (3)0.126 (9)0.040 (6)0.037 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Te0.00781 (8)0.00498 (9)0.00931 (8)0.00088 (5)0.0000.000
Ag0.02056 (11)0.00880 (12)0.04609 (18)0.00267 (6)0.00392 (9)0.00486 (12)
O10.0108 (6)0.0072 (10)0.0146 (6)0.0001 (6)0.0029 (5)0.0048 (7)
O20.0125 (7)0.0199 (12)0.0159 (7)0.0019 (7)0.0007 (5)0.0099 (8)
O30.0087 (5)0.0071 (8)0.0232 (7)0.0014 (5)0.0030 (6)0.0018 (7)
Geometric parameters (Å, º) top
Te—O1i1.8799 (19)Ag—Agiv2.9893 (5)
Te—O1ii1.8799 (19)Ag—Agviii3.2110 (3)
Te—O3iii1.9395 (17)Ag—Agix3.2110 (3)
Te—O31.9395 (17)O1—Tex1.8799 (19)
Te—O2iv1.953 (2)O2—Texi1.953 (2)
Te—O2v1.953 (2)O2—Agxii2.4561 (17)
Ag—O3vi2.225 (2)O2—Agxiii2.579 (3)
Ag—O12.307 (2)O2—H10.98 (4)
Ag—O2vii2.4561 (17)O3—Agxiii2.225 (2)
Ag—O2vi2.579 (3)O3—H20.95 (4)
O1i—Te—O1ii95.84 (13)O2vii—Ag—Agiv163.72 (4)
O1i—Te—O3iii89.06 (9)O2vi—Ag—Agiv80.36 (4)
O1ii—Te—O3iii92.49 (9)O3vi—Ag—Agviii115.31 (5)
O1i—Te—O392.49 (9)O1—Ag—Agviii94.85 (5)
O1ii—Te—O389.06 (9)O2vii—Ag—Agviii67.88 (5)
O3iii—Te—O3177.69 (12)O2vi—Ag—Agviii48.71 (4)
O1i—Te—O2iv175.61 (11)Agiv—Ag—Agviii125.079 (9)
O1ii—Te—O2iv87.99 (9)O3vi—Ag—Agix62.64 (5)
O3iii—Te—O2iv88.62 (9)O1—Ag—Agix103.31 (4)
O3—Te—O2iv89.72 (9)O2vii—Ag—Agix52.08 (6)
O1i—Te—O2v87.99 (9)O2vi—Ag—Agix157.75 (5)
O1ii—Te—O2v175.61 (11)Agiv—Ag—Agix117.545 (10)
O3iii—Te—O2v89.72 (9)Agviii—Ag—Agix117.084 (15)
O3—Te—O2v88.62 (9)Tex—O1—Ag107.56 (9)
O2iv—Te—O2v88.27 (14)Texi—O2—Agxii133.07 (10)
O3vi—Ag—O1149.79 (7)Texi—O2—Agxiii95.76 (8)
O3vi—Ag—O2vii97.94 (8)Agxii—O2—Agxiii79.21 (7)
O1—Ag—O2vii91.80 (7)Texi—O2—H1127 (4)
O3vi—Ag—O2vi136.02 (7)Agxii—O2—H197 (4)
O1—Ag—O2vi65.78 (6)Agxiii—O2—H1113 (4)
O2vii—Ag—O2vi107.23 (10)Te—O3—Agxiii124.75 (9)
O3vi—Ag—Agiv85.33 (4)Te—O3—H2119 (4)
O1—Ag—Agiv78.01 (4)Agxiii—O3—H2115 (4)
Symmetry codes: (i) x, y1, z1; (ii) x, y+1, z1; (iii) x, y, z; (iv) x, y+1, z; (v) x, y1, z; (vi) x, y, z+1; (vii) x+1/4, y1/4, z+3/4; (viii) x+1/4, y+1/4, z+1/4; (ix) x+1/4, y1/4, z1/4; (x) x, y+1, z+1; (xi) x, y+1, z; (xii) x+1/4, y+1/4, z3/4; (xiii) x, y, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H1···O1xiv0.98 (4)1.68 (4)2.596 (2)155 (6)
O3—H2···O1xv0.95 (4)1.63 (4)2.579 (3)171 (6)
Symmetry codes: (xiv) x, y+3/2, z1/2; (xv) x+1/4, y3/4, z3/4.
 

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