The crystal structure of monoclinic KYb(WO
4)
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}, {
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 (
= 16.68 × 10
−6 K
−1),
, was located 12° from the
c axis. Its principal
,
and
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
Program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Ytterbium potassium wolframate
top
Crystal data top
YbKO8W2 | F(000) = 1204 |
Mr = 707.84 | Dx = 7.610 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71069 Å |
a = 10.590 (4) Å | Cell parameters from 25 reflections |
b = 10.290 (6) Å | θ = 12–21° |
c = 7.478 (2) Å | µ = 52.84 mm−1 |
β = 130.70 (2)° | T = 293 K |
V = 617.8 (5) Å3 | 0.2 × 0.1 × 0.1 mm |
Z = 4 | |
Data collection top
Radiation source: fine-focus sealed tube | 837 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
Absorption correction: phi scan ? | θmax = 30.1°, θmin = 3.2° |
Tmin = 0.47, Tmax = 0.63 | h = −14→11 |
1875 measured reflections | k = 0→14 |
976 independent reflections | l = 0→10 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.045 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.113 | Calculated w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.007 |
909 reflections | Δρmax = 0.47 e Å−3 |
56 parameters | Δρmin = −0.14 e Å−3 |
Crystal data top
YbKO8W2 | V = 617.8 (5) Å3 |
Mr = 707.84 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.590 (4) Å | µ = 52.84 mm−1 |
b = 10.290 (6) Å | T = 293 K |
c = 7.478 (2) Å | 0.2 × 0.1 × 0.1 mm |
β = 130.70 (2)° | |
Data collection top
Absorption correction: phi scan ? | 976 independent reflections |
Tmin = 0.47, Tmax = 0.63 | 837 reflections with I > 2σ(I) |
1875 measured reflections | Rint = 0.046 |
Refinement top
R[F2 > 2σ(F2)] = 0.045 | 56 parameters |
wR(F2) = 0.113 | 0 restraints |
S = 1.00 | Δρmax = 0.47 e Å−3 |
909 reflections | Δρmin = −0.14 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Yb | 0.0000 | 0.72860 (6) | 0.2500 | 0.0060 (2) | |
W | 0.19722 (5) | −0.00004 (3) | 0.73560 (6) | 0.0045 (2) | |
K | 0.5000 | 0.2049 (4) | 0.7500 | 0.0145 (6) | |
O1 | 0.3736 (8) | −0.0860 (8) | 0.8115 (11) | 0.0110 (13) | |
O2 | 0.0241 (8) | −0.1103 (7) | 0.4636 (11) | 0.0067 (11) | |
O3 | 0.2783 (7) | 0.1584 (6) | 0.8732 (10) | 0.0050 (11) | |
O4 | 0.1907 (8) | −0.0784 (7) | 0.9378 (11) | 0.0091 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Yb | 0.0055 (3) | 0.0057 (3) | 0.0044 (3) | 0.000 | 0.0022 (2) | 0.000 |
W | 0.0037 (3) | 0.0047 (3) | 0.0029 (3) | −0.00003 (9) | 0.0012 (2) | −0.00014 (9) |
K | 0.0138 (14) | 0.0138 (15) | 0.0150 (14) | 0.000 | 0.0090 (13) | 0.000 |
O1 | 0.010 (3) | 0.012 (4) | 0.008 (3) | −0.002 (2) | 0.004 (3) | 0.000 (2) |
O2 | 0.005 (3) | 0.007 (3) | 0.004 (3) | −0.002 (2) | 0.001 (2) | −0.003 (2) |
O3 | 0.005 (3) | 0.003 (3) | 0.003 (3) | 0.000 (2) | 0.001 (2) | 0.0008 (19) |
O4 | 0.007 (3) | 0.011 (3) | 0.008 (3) | −0.001 (2) | 0.005 (2) | 0.000 (2) |
Geometric parameters (Å, º) top
Yb—O2i | 2.198 (7) | K—O4xiv | 2.706 (8) |
Yb—O2ii | 2.198 (7) | K—O4vi | 2.706 (8) |
Yb—O1iii | 2.226 (7) | K—O4xi | 2.811 (7) |
Yb—O1iv | 2.226 (7) | K—O4xii | 2.811 (7) |
Yb—O3v | 2.312 (6) | K—O1xi | 2.884 (7) |
Yb—O3vi | 2.312 (6) | K—O1xii | 2.884 (7) |
Yb—O3vii | 2.711 (6) | K—O2vi | 2.997 (7) |
Yb—O3viii | 2.711 (6) | K—O2xiv | 2.997 (7) |
Yb—Wvii | 3.5311 (15) | K—O3xv | 3.068 (6) |
Yb—Wviii | 3.5311 (15) | K—O3 | 3.068 (6) |
Yb—Kv | 3.7469 (10) | K—O1 | 3.430 (8) |
Yb—Kix | 3.7469 (10) | K—O1xv | 3.430 (8) |
W—O4 | 1.755 (6) | O1—Ybiv | 2.226 (7) |
W—O1 | 1.792 (7) | O1—Kxii | 2.884 (7) |
W—O3 | 1.817 (6) | O2—Wx | 2.109 (6) |
W—O2 | 1.980 (6) | O2—Ybxvi | 2.198 (7) |
W—O2x | 2.109 (6) | O2—Kxiii | 2.997 (7) |
W—O4xi | 2.327 (6) | O3—Ybxvii | 2.312 (6) |
W—Ybviii | 3.5311 (15) | O3—Ybviii | 2.711 (6) |
W—Kxii | 3.666 (3) | O4—Wxviii | 2.327 (6) |
W—Kxiii | 3.726 (4) | O4—Kxiii | 2.706 (8) |
W—K | 3.780 (3) | O4—Kxii | 2.811 (7) |
W—Kiv | 4.109 (3) | | |
| | | |
O2i—Yb—O2ii | 82.1 (4) | O2x—W—K | 104.55 (19) |
O2i—Yb—O1iii | 98.5 (3) | O4xi—W—K | 47.86 (17) |
O2ii—Yb—O1iii | 147.8 (2) | Ybviii—W—K | 93.75 (6) |
O2i—Yb—O1iv | 147.8 (2) | Kxii—W—K | 98.38 (7) |
O2ii—Yb—O1iv | 98.5 (3) | Kxiii—W—K | 159.19 (8) |
O1iii—Yb—O1iv | 97.5 (4) | O4—W—Kiv | 144.9 (2) |
O2i—Yb—O3v | 131.7 (2) | O1—W—Kiv | 117.9 (2) |
O2ii—Yb—O3v | 78.8 (2) | O3—W—Kiv | 67.51 (19) |
O1iii—Yb—O3v | 77.1 (2) | O2—W—Kiv | 85.4 (2) |
O1iv—Yb—O3v | 79.1 (2) | O2x—W—Kiv | 44.57 (18) |
O2i—Yb—O3vi | 78.8 (2) | O4xi—W—Kiv | 38.45 (17) |
O2ii—Yb—O3vi | 131.7 (2) | Ybviii—W—Kiv | 58.15 (4) |
O1iii—Yb—O3vi | 79.1 (2) | Kxii—W—Kiv | 160.96 (6) |
O1iv—Yb—O3vi | 77.1 (2) | Kxiii—W—Kiv | 131.02 (5) |
O3v—Yb—O3vi | 143.6 (3) | K—W—Kiv | 62.98 (3) |
O2i—Yb—O3vii | 81.0 (2) | O4xiv—K—O4vi | 69.0 (3) |
O2ii—Yb—O3vii | 60.6 (2) | O4xiv—K—O4xi | 152.1 (2) |
O1iii—Yb—O3vii | 151.6 (2) | O4vi—K—O4xi | 83.1 (2) |
O1iv—Yb—O3vii | 71.7 (2) | O4xiv—K—O4xii | 83.1 (2) |
O3v—Yb—O3vii | 124.3 (2) | O4vi—K—O4xii | 152.1 (2) |
O3vi—Yb—O3vii | 72.9 (2) | O4xi—K—O4xii | 124.8 (3) |
O2i—Yb—O3viii | 60.6 (2) | O4xiv—K—O1xi | 125.1 (2) |
O2ii—Yb—O3viii | 81.0 (2) | O4vi—K—O1xi | 97.1 (2) |
O1iii—Yb—O3viii | 71.7 (2) | O4xi—K—O1xi | 55.52 (19) |
O1iv—Yb—O3viii | 151.6 (2) | O4xii—K—O1xi | 100.0 (2) |
O3v—Yb—O3viii | 72.9 (2) | O4xiv—K—O1xii | 97.1 (2) |
O3vi—Yb—O3viii | 124.3 (2) | O4vi—K—O1xii | 125.1 (2) |
O3vii—Yb—O3viii | 129.2 (3) | O4xi—K—O1xii | 100.0 (2) |
O2i—Yb—Wvii | 68.58 (18) | O4xii—K—O1xii | 55.52 (19) |
O2ii—Yb—Wvii | 34.12 (16) | O1xi—K—O1xii | 129.8 (3) |
O1iii—Yb—Wvii | 167.08 (18) | O4xiv—K—O2vi | 59.3 (2) |
O1iv—Yb—Wvii | 93.90 (19) | O4vi—K—O2vi | 57.70 (19) |
O3v—Yb—Wvii | 111.15 (16) | O4xi—K—O2vi | 106.92 (18) |
O3vi—Yb—Wvii | 97.69 (16) | O4xii—K—O2vi | 107.25 (18) |
O3vii—Yb—Wvii | 30.37 (13) | O1xi—K—O2vi | 152.77 (19) |
O3viii—Yb—Wvii | 100.59 (14) | O1xii—K—O2vi | 69.5 (2) |
O2i—Yb—Wviii | 34.12 (16) | O4xiv—K—O2xiv | 57.70 (19) |
O2ii—Yb—Wviii | 68.58 (18) | O4vi—K—O2xiv | 59.3 (2) |
O1iii—Yb—Wviii | 93.90 (19) | O4xi—K—O2xiv | 107.25 (18) |
O1iv—Yb—Wviii | 167.08 (18) | O4xii—K—O2xiv | 106.92 (18) |
O3v—Yb—Wviii | 97.69 (16) | O1xi—K—O2xiv | 69.5 (2) |
O3vi—Yb—Wviii | 111.15 (16) | O1xii—K—O2xiv | 152.77 (19) |
O3vii—Yb—Wviii | 100.59 (14) | O2vi—K—O2xiv | 101.2 (3) |
O3viii—Yb—Wviii | 30.37 (13) | O4xiv—K—O3xv | 80.00 (19) |
Wvii—Yb—Wviii | 75.44 (4) | O4vi—K—O3xv | 115.54 (19) |
O2i—Yb—Kv | 134.30 (19) | O4xi—K—O3xv | 112.57 (19) |
O2ii—Yb—Kv | 53.10 (18) | O4xii—K—O3xv | 58.10 (17) |
O1iii—Yb—Kv | 123.66 (18) | O1xi—K—O3xv | 58.05 (17) |
O1iv—Yb—Kv | 50.21 (18) | O1xii—K—O3xv | 113.37 (19) |
O3v—Yb—Kv | 54.85 (15) | O2vi—K—O3xv | 138.8 (2) |
O3vi—Yb—Kv | 122.35 (15) | O2xiv—K—O3xv | 56.35 (17) |
O3vii—Yb—Kv | 70.09 (12) | O4xiv—K—O3 | 115.54 (19) |
O3viii—Yb—Kv | 113.35 (12) | O4vi—K—O3 | 80.00 (19) |
Wvii—Yb—Kv | 68.66 (6) | O4xi—K—O3 | 58.10 (17) |
Wviii—Yb—Kv | 117.82 (5) | O4xii—K—O3 | 112.57 (19) |
O2i—Yb—Kix | 53.10 (19) | O1xi—K—O3 | 113.37 (19) |
O2ii—Yb—Kix | 134.30 (19) | O1xii—K—O3 | 58.05 (17) |
O1iii—Yb—Kix | 50.21 (18) | O2vi—K—O3 | 56.35 (17) |
O1iv—Yb—Kix | 123.66 (18) | O2xiv—K—O3 | 138.8 (2) |
O3v—Yb—Kix | 122.35 (15) | O3xv—K—O3 | 162.0 (3) |
O3vi—Yb—Kix | 54.85 (15) | O4xiv—K—O1 | 150.91 (17) |
O3vii—Yb—Kix | 113.35 (12) | O4vi—K—O1 | 124.36 (19) |
O3viii—Yb—Kix | 70.09 (12) | O4xi—K—O1 | 50.36 (19) |
Wvii—Yb—Kix | 117.82 (5) | O4xii—K—O1 | 80.2 (2) |
Wviii—Yb—Kix | 68.66 (5) | O1xi—K—O1 | 81.36 (15) |
Kv—Yb—Kix | 172.54 (12) | O1xii—K—O1 | 53.8 (2) |
O4—W—O1 | 96.8 (3) | O2vi—K—O1 | 103.62 (17) |
O4—W—O3 | 101.2 (3) | O2xiv—K—O1 | 150.69 (18) |
O1—W—O3 | 104.7 (3) | O3xv—K—O1 | 110.2 (2) |
O4—W—O2 | 95.2 (3) | O3—K—O1 | 51.80 (18) |
O1—W—O2 | 96.8 (3) | O4xiv—K—O1xv | 124.36 (19) |
O3—W—O2 | 151.0 (3) | O4vi—K—O1xv | 150.91 (17) |
O4—W—O2x | 101.9 (3) | O4xi—K—O1xv | 80.2 (2) |
O1—W—O2x | 159.8 (3) | O4xii—K—O1xv | 50.36 (19) |
O3—W—O2x | 79.3 (3) | O1xi—K—O1xv | 53.8 (2) |
O2—W—O2x | 74.0 (3) | O1xii—K—O1xv | 81.36 (15) |
O4—W—O4xi | 172.3 (2) | O2vi—K—O1xv | 150.69 (18) |
O1—W—O4xi | 81.3 (3) | O2xiv—K—O1xv | 103.62 (17) |
O3—W—O4xi | 86.5 (3) | O3xv—K—O1xv | 51.80 (18) |
O2—W—O4xi | 77.6 (3) | O3—K—O1xv | 110.2 (2) |
O2x—W—O4xi | 79.1 (2) | O1—K—O1xv | 58.4 (2) |
O4—W—Ybviii | 88.9 (2) | W—O1—Ybiv | 154.5 (4) |
O1—W—Ybviii | 153.6 (2) | W—O1—Kxii | 100.6 (3) |
O3—W—Ybviii | 48.97 (19) | Ybiv—O1—Kxii | 93.4 (3) |
O2—W—Ybviii | 108.4 (2) | W—O1—K | 86.8 (3) |
O2x—W—Ybviii | 35.77 (17) | Ybiv—O1—K | 102.0 (2) |
O4xi—W—Ybviii | 96.06 (18) | Kxii—O1—K | 126.2 (2) |
O4—W—Kxii | 48.0 (2) | W—O2—Wx | 106.0 (3) |
O1—W—Kxii | 50.7 (2) | W—O2—Ybxvi | 140.3 (3) |
O3—W—Kxii | 98.90 (19) | Wx—O2—Ybxvi | 110.1 (3) |
O2—W—Kxii | 109.8 (2) | W—O2—Kxiii | 94.7 (2) |
O2x—W—Kxii | 149.26 (17) | Wx—O2—Kxiii | 105.8 (2) |
O4xi—W—Kxii | 131.58 (16) | Ybxvi—O2—Kxiii | 91.0 (2) |
Ybviii—W—Kxii | 123.57 (4) | W—O3—Ybxvii | 134.4 (3) |
O4—W—Kxiii | 42.5 (2) | W—O3—Ybviii | 100.7 (2) |
O1—W—Kxiii | 94.4 (2) | Ybxvii—O3—Ybviii | 107.1 (2) |
O3—W—Kxiii | 141.40 (18) | W—O3—K | 98.2 (2) |
O2—W—Kxiii | 53.3 (2) | Ybxvii—O3—K | 87.10 (19) |
O2x—W—Kxiii | 94.20 (19) | Ybviii—O3—K | 134.9 (2) |
O4xi—W—Kxiii | 130.01 (18) | W—O4—Wxviii | 132.2 (4) |
Ybviii—W—Kxiii | 106.85 (5) | W—O4—Kxiii | 111.5 (3) |
Kxii—W—Kxiii | 67.93 (4) | Wxviii—O4—Kxiii | 109.2 (2) |
O4—W—K | 137.9 (2) | W—O4—Kxii | 104.4 (3) |
O1—W—K | 64.9 (2) | Wxviii—O4—Kxii | 94.3 (2) |
O3—W—K | 53.44 (19) | Kxiii—O4—Kxii | 96.9 (2) |
O2—W—K | 123.27 (19) | | |
Symmetry codes: (i) x, y+1, z; (ii) −x, y+1, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) −x+1/2, −y+1/2, −z+1; (v) x−1/2, y+1/2, z−1; (vi) −x+1/2, y+1/2, −z+3/2; (vii) x, −y+1, z−1/2; (viii) −x, −y+1, −z+1; (ix) x−1/2, y+1/2, z; (x) −x, −y, −z+1; (xi) x, −y, z−1/2; (xii) −x+1, −y, −z+2; (xiii) x−1/2, y−1/2, z; (xiv) x+1/2, y+1/2, z; (xv) −x+1, y, −z+3/2; (xvi) x, y−1, z; (xvii) x+1/2, y−1/2, z+1; (xviii) x, −y, z+1/2. |
Experimental details
Crystal data |
Chemical formula | YbKO8W2 |
Mr | 707.84 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 10.590 (4), 10.290 (6), 7.478 (2) |
β (°) | 130.70 (2) |
V (Å3) | 617.8 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 52.84 |
Crystal size (mm) | 0.2 × 0.1 × 0.1 |
|
Data collection |
Diffractometer | ? |
Absorption correction | Phi scan |
Tmin, Tmax | 0.47, 0.63 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1875, 976, 837 |
Rint | 0.046 |
(sin θ/λ)max (Å−1) | 0.705 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.113, 1.00 |
No. of reflections | 909 |
No. of parameters | 56 |
Δρmax, Δρmin (e Å−3) | 0.47, −0.14 |