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The crystal structure of monoclinic KYb(WO4)2 (KYbW) crystals has been refined (in space group C2/c) at room temperature by using single-crystal X-ray diffraction data. KYbW undoped crystals were grown by the TSSG (top-seeded-solution growth) slow-cooling method. The crystals show {110}, {\bar{1}11}, {010} and {310} faces, which basically define their habit. The linear thermal expansion tensor has been determined and the principal axis with maximum thermal expansion (\alpha ^{\,\prime}_{33} = 16.68 × 10−6 K−1), {\bf X}^{\,\prime}_{3}, was located 12° from the c axis. Its principal {\bf X}^{\,\prime}_{1}, {\bf X}^{\,\prime}_{2} and {\bf X}^{\,\prime}_{3} axes are [302], [010] and [106] directions, respectively, in the crystallographic system. The optical tensor has been studied at λ = 632.8 nm at room temperature; two principal axes, Ng and Nm, are located in the ac plane, while the other, Np, is parallel to [010]. The principal axis with maximum refractive index (ng = 2.45), Ng, was located 19° from the c axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889801019914/pd0023sup1.cif
Contains datablock magec40a

sft

Structure factor file (SHELXL table format) https://doi.org/10.1107/S0021889801019914/pd0023magec40asup2.sft
Supplementary material

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0021889801019914/pd0023sup3.pdf
Supplementary material

Computing details top

Program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
Ytterbium potassium wolframate top
Crystal data top
YbKO8W2F(000) = 1204
Mr = 707.84Dx = 7.610 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
a = 10.590 (4) ÅCell parameters from 25 reflections
b = 10.290 (6) Åθ = 12–21°
c = 7.478 (2) ŵ = 52.84 mm1
β = 130.70 (2)°T = 293 K
V = 617.8 (5) Å30.2 × 0.1 × 0.1 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tube837 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
Absorption correction: phi scan
?
θmax = 30.1°, θmin = 3.2°
Tmin = 0.47, Tmax = 0.63h = 1411
1875 measured reflectionsk = 014
976 independent reflectionsl = 010
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.045Secondary atom site location: difference Fourier map
wR(F2) = 0.113Calculated w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.007
909 reflectionsΔρmax = 0.47 e Å3
56 parametersΔρmin = 0.14 e Å3
Crystal data top
YbKO8W2V = 617.8 (5) Å3
Mr = 707.84Z = 4
Monoclinic, C2/cMo Kα radiation
a = 10.590 (4) ŵ = 52.84 mm1
b = 10.290 (6) ÅT = 293 K
c = 7.478 (2) Å0.2 × 0.1 × 0.1 mm
β = 130.70 (2)°
Data collection top
Absorption correction: phi scan
?
976 independent reflections
Tmin = 0.47, Tmax = 0.63837 reflections with I > 2σ(I)
1875 measured reflectionsRint = 0.046
Refinement top
R[F2 > 2σ(F2)] = 0.04556 parameters
wR(F2) = 0.1130 restraints
S = 1.00Δρmax = 0.47 e Å3
909 reflectionsΔρmin = 0.14 e Å3
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
Yb0.00000.72860 (6)0.25000.0060 (2)
W0.19722 (5)0.00004 (3)0.73560 (6)0.0045 (2)
K0.50000.2049 (4)0.75000.0145 (6)
O10.3736 (8)0.0860 (8)0.8115 (11)0.0110 (13)
O20.0241 (8)0.1103 (7)0.4636 (11)0.0067 (11)
O30.2783 (7)0.1584 (6)0.8732 (10)0.0050 (11)
O40.1907 (8)0.0784 (7)0.9378 (11)0.0091 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb0.0055 (3)0.0057 (3)0.0044 (3)0.0000.0022 (2)0.000
W0.0037 (3)0.0047 (3)0.0029 (3)0.00003 (9)0.0012 (2)0.00014 (9)
K0.0138 (14)0.0138 (15)0.0150 (14)0.0000.0090 (13)0.000
O10.010 (3)0.012 (4)0.008 (3)0.002 (2)0.004 (3)0.000 (2)
O20.005 (3)0.007 (3)0.004 (3)0.002 (2)0.001 (2)0.003 (2)
O30.005 (3)0.003 (3)0.003 (3)0.000 (2)0.001 (2)0.0008 (19)
O40.007 (3)0.011 (3)0.008 (3)0.001 (2)0.005 (2)0.000 (2)
Geometric parameters (Å, º) top
Yb—O2i2.198 (7)K—O4xiv2.706 (8)
Yb—O2ii2.198 (7)K—O4vi2.706 (8)
Yb—O1iii2.226 (7)K—O4xi2.811 (7)
Yb—O1iv2.226 (7)K—O4xii2.811 (7)
Yb—O3v2.312 (6)K—O1xi2.884 (7)
Yb—O3vi2.312 (6)K—O1xii2.884 (7)
Yb—O3vii2.711 (6)K—O2vi2.997 (7)
Yb—O3viii2.711 (6)K—O2xiv2.997 (7)
Yb—Wvii3.5311 (15)K—O3xv3.068 (6)
Yb—Wviii3.5311 (15)K—O33.068 (6)
Yb—Kv3.7469 (10)K—O13.430 (8)
Yb—Kix3.7469 (10)K—O1xv3.430 (8)
W—O41.755 (6)O1—Ybiv2.226 (7)
W—O11.792 (7)O1—Kxii2.884 (7)
W—O31.817 (6)O2—Wx2.109 (6)
W—O21.980 (6)O2—Ybxvi2.198 (7)
W—O2x2.109 (6)O2—Kxiii2.997 (7)
W—O4xi2.327 (6)O3—Ybxvii2.312 (6)
W—Ybviii3.5311 (15)O3—Ybviii2.711 (6)
W—Kxii3.666 (3)O4—Wxviii2.327 (6)
W—Kxiii3.726 (4)O4—Kxiii2.706 (8)
W—K3.780 (3)O4—Kxii2.811 (7)
W—Kiv4.109 (3)
O2i—Yb—O2ii82.1 (4)O2x—W—K104.55 (19)
O2i—Yb—O1iii98.5 (3)O4xi—W—K47.86 (17)
O2ii—Yb—O1iii147.8 (2)Ybviii—W—K93.75 (6)
O2i—Yb—O1iv147.8 (2)Kxii—W—K98.38 (7)
O2ii—Yb—O1iv98.5 (3)Kxiii—W—K159.19 (8)
O1iii—Yb—O1iv97.5 (4)O4—W—Kiv144.9 (2)
O2i—Yb—O3v131.7 (2)O1—W—Kiv117.9 (2)
O2ii—Yb—O3v78.8 (2)O3—W—Kiv67.51 (19)
O1iii—Yb—O3v77.1 (2)O2—W—Kiv85.4 (2)
O1iv—Yb—O3v79.1 (2)O2x—W—Kiv44.57 (18)
O2i—Yb—O3vi78.8 (2)O4xi—W—Kiv38.45 (17)
O2ii—Yb—O3vi131.7 (2)Ybviii—W—Kiv58.15 (4)
O1iii—Yb—O3vi79.1 (2)Kxii—W—Kiv160.96 (6)
O1iv—Yb—O3vi77.1 (2)Kxiii—W—Kiv131.02 (5)
O3v—Yb—O3vi143.6 (3)K—W—Kiv62.98 (3)
O2i—Yb—O3vii81.0 (2)O4xiv—K—O4vi69.0 (3)
O2ii—Yb—O3vii60.6 (2)O4xiv—K—O4xi152.1 (2)
O1iii—Yb—O3vii151.6 (2)O4vi—K—O4xi83.1 (2)
O1iv—Yb—O3vii71.7 (2)O4xiv—K—O4xii83.1 (2)
O3v—Yb—O3vii124.3 (2)O4vi—K—O4xii152.1 (2)
O3vi—Yb—O3vii72.9 (2)O4xi—K—O4xii124.8 (3)
O2i—Yb—O3viii60.6 (2)O4xiv—K—O1xi125.1 (2)
O2ii—Yb—O3viii81.0 (2)O4vi—K—O1xi97.1 (2)
O1iii—Yb—O3viii71.7 (2)O4xi—K—O1xi55.52 (19)
O1iv—Yb—O3viii151.6 (2)O4xii—K—O1xi100.0 (2)
O3v—Yb—O3viii72.9 (2)O4xiv—K—O1xii97.1 (2)
O3vi—Yb—O3viii124.3 (2)O4vi—K—O1xii125.1 (2)
O3vii—Yb—O3viii129.2 (3)O4xi—K—O1xii100.0 (2)
O2i—Yb—Wvii68.58 (18)O4xii—K—O1xii55.52 (19)
O2ii—Yb—Wvii34.12 (16)O1xi—K—O1xii129.8 (3)
O1iii—Yb—Wvii167.08 (18)O4xiv—K—O2vi59.3 (2)
O1iv—Yb—Wvii93.90 (19)O4vi—K—O2vi57.70 (19)
O3v—Yb—Wvii111.15 (16)O4xi—K—O2vi106.92 (18)
O3vi—Yb—Wvii97.69 (16)O4xii—K—O2vi107.25 (18)
O3vii—Yb—Wvii30.37 (13)O1xi—K—O2vi152.77 (19)
O3viii—Yb—Wvii100.59 (14)O1xii—K—O2vi69.5 (2)
O2i—Yb—Wviii34.12 (16)O4xiv—K—O2xiv57.70 (19)
O2ii—Yb—Wviii68.58 (18)O4vi—K—O2xiv59.3 (2)
O1iii—Yb—Wviii93.90 (19)O4xi—K—O2xiv107.25 (18)
O1iv—Yb—Wviii167.08 (18)O4xii—K—O2xiv106.92 (18)
O3v—Yb—Wviii97.69 (16)O1xi—K—O2xiv69.5 (2)
O3vi—Yb—Wviii111.15 (16)O1xii—K—O2xiv152.77 (19)
O3vii—Yb—Wviii100.59 (14)O2vi—K—O2xiv101.2 (3)
O3viii—Yb—Wviii30.37 (13)O4xiv—K—O3xv80.00 (19)
Wvii—Yb—Wviii75.44 (4)O4vi—K—O3xv115.54 (19)
O2i—Yb—Kv134.30 (19)O4xi—K—O3xv112.57 (19)
O2ii—Yb—Kv53.10 (18)O4xii—K—O3xv58.10 (17)
O1iii—Yb—Kv123.66 (18)O1xi—K—O3xv58.05 (17)
O1iv—Yb—Kv50.21 (18)O1xii—K—O3xv113.37 (19)
O3v—Yb—Kv54.85 (15)O2vi—K—O3xv138.8 (2)
O3vi—Yb—Kv122.35 (15)O2xiv—K—O3xv56.35 (17)
O3vii—Yb—Kv70.09 (12)O4xiv—K—O3115.54 (19)
O3viii—Yb—Kv113.35 (12)O4vi—K—O380.00 (19)
Wvii—Yb—Kv68.66 (6)O4xi—K—O358.10 (17)
Wviii—Yb—Kv117.82 (5)O4xii—K—O3112.57 (19)
O2i—Yb—Kix53.10 (19)O1xi—K—O3113.37 (19)
O2ii—Yb—Kix134.30 (19)O1xii—K—O358.05 (17)
O1iii—Yb—Kix50.21 (18)O2vi—K—O356.35 (17)
O1iv—Yb—Kix123.66 (18)O2xiv—K—O3138.8 (2)
O3v—Yb—Kix122.35 (15)O3xv—K—O3162.0 (3)
O3vi—Yb—Kix54.85 (15)O4xiv—K—O1150.91 (17)
O3vii—Yb—Kix113.35 (12)O4vi—K—O1124.36 (19)
O3viii—Yb—Kix70.09 (12)O4xi—K—O150.36 (19)
Wvii—Yb—Kix117.82 (5)O4xii—K—O180.2 (2)
Wviii—Yb—Kix68.66 (5)O1xi—K—O181.36 (15)
Kv—Yb—Kix172.54 (12)O1xii—K—O153.8 (2)
O4—W—O196.8 (3)O2vi—K—O1103.62 (17)
O4—W—O3101.2 (3)O2xiv—K—O1150.69 (18)
O1—W—O3104.7 (3)O3xv—K—O1110.2 (2)
O4—W—O295.2 (3)O3—K—O151.80 (18)
O1—W—O296.8 (3)O4xiv—K—O1xv124.36 (19)
O3—W—O2151.0 (3)O4vi—K—O1xv150.91 (17)
O4—W—O2x101.9 (3)O4xi—K—O1xv80.2 (2)
O1—W—O2x159.8 (3)O4xii—K—O1xv50.36 (19)
O3—W—O2x79.3 (3)O1xi—K—O1xv53.8 (2)
O2—W—O2x74.0 (3)O1xii—K—O1xv81.36 (15)
O4—W—O4xi172.3 (2)O2vi—K—O1xv150.69 (18)
O1—W—O4xi81.3 (3)O2xiv—K—O1xv103.62 (17)
O3—W—O4xi86.5 (3)O3xv—K—O1xv51.80 (18)
O2—W—O4xi77.6 (3)O3—K—O1xv110.2 (2)
O2x—W—O4xi79.1 (2)O1—K—O1xv58.4 (2)
O4—W—Ybviii88.9 (2)W—O1—Ybiv154.5 (4)
O1—W—Ybviii153.6 (2)W—O1—Kxii100.6 (3)
O3—W—Ybviii48.97 (19)Ybiv—O1—Kxii93.4 (3)
O2—W—Ybviii108.4 (2)W—O1—K86.8 (3)
O2x—W—Ybviii35.77 (17)Ybiv—O1—K102.0 (2)
O4xi—W—Ybviii96.06 (18)Kxii—O1—K126.2 (2)
O4—W—Kxii48.0 (2)W—O2—Wx106.0 (3)
O1—W—Kxii50.7 (2)W—O2—Ybxvi140.3 (3)
O3—W—Kxii98.90 (19)Wx—O2—Ybxvi110.1 (3)
O2—W—Kxii109.8 (2)W—O2—Kxiii94.7 (2)
O2x—W—Kxii149.26 (17)Wx—O2—Kxiii105.8 (2)
O4xi—W—Kxii131.58 (16)Ybxvi—O2—Kxiii91.0 (2)
Ybviii—W—Kxii123.57 (4)W—O3—Ybxvii134.4 (3)
O4—W—Kxiii42.5 (2)W—O3—Ybviii100.7 (2)
O1—W—Kxiii94.4 (2)Ybxvii—O3—Ybviii107.1 (2)
O3—W—Kxiii141.40 (18)W—O3—K98.2 (2)
O2—W—Kxiii53.3 (2)Ybxvii—O3—K87.10 (19)
O2x—W—Kxiii94.20 (19)Ybviii—O3—K134.9 (2)
O4xi—W—Kxiii130.01 (18)W—O4—Wxviii132.2 (4)
Ybviii—W—Kxiii106.85 (5)W—O4—Kxiii111.5 (3)
Kxii—W—Kxiii67.93 (4)Wxviii—O4—Kxiii109.2 (2)
O4—W—K137.9 (2)W—O4—Kxii104.4 (3)
O1—W—K64.9 (2)Wxviii—O4—Kxii94.3 (2)
O3—W—K53.44 (19)Kxiii—O4—Kxii96.9 (2)
O2—W—K123.27 (19)
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z+1/2; (iii) x1/2, y+1/2, z1/2; (iv) x+1/2, y+1/2, z+1; (v) x1/2, y+1/2, z1; (vi) x+1/2, y+1/2, z+3/2; (vii) x, y+1, z1/2; (viii) x, y+1, z+1; (ix) x1/2, y+1/2, z; (x) x, y, z+1; (xi) x, y, z1/2; (xii) x+1, y, z+2; (xiii) x1/2, y1/2, z; (xiv) x+1/2, y+1/2, z; (xv) x+1, y, z+3/2; (xvi) x, y1, z; (xvii) x+1/2, y1/2, z+1; (xviii) x, y, z+1/2.

Experimental details

Crystal data
Chemical formulaYbKO8W2
Mr707.84
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)10.590 (4), 10.290 (6), 7.478 (2)
β (°) 130.70 (2)
V3)617.8 (5)
Z4
Radiation typeMo Kα
µ (mm1)52.84
Crystal size (mm)0.2 × 0.1 × 0.1
Data collection
Diffractometer?
Absorption correctionPhi scan
Tmin, Tmax0.47, 0.63
No. of measured, independent and
observed [I > 2σ(I)] reflections
1875, 976, 837
Rint0.046
(sin θ/λ)max1)0.705
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.113, 1.00
No. of reflections909
No. of parameters56
Δρmax, Δρmin (e Å3)0.47, 0.14

Computer programs: SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997).

 

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