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A transparent Yb3+:NaY(WO4)2 single crystal with dimensions of 30 mm (diameter) × 40 mm has been grown by the Czochralski method. The high crystalline quality of the as-grown Yb3+:NaY(WO4)2 crystals was confirmed by high-resolution X-ray diffraction. The effective segregation coefficients of elemental Yb, Na, Y and W in Yb3+:NaY(WO4)2 were measured using the X-ray fluorescence method. Powder and single-crystal X-ray diffraction data of NaYb0.05Y0.95(WO4)2 are reported. The structure refinement shows that NaYb0.05Y0.95(WO4)2 crystallizes in the tetragonal space group I41/a, with a = b = 5.2039 (2), c = 11.2838 (9) Å, α = β = γ = 90°, V = 305.57 (3) Å3 and Z = 2. A series of possible growth faces (hkl) were determined from the crystal lattice and symmetry according to the Bravais–Friedel Donnay–Harker theory, and the relationship among crystal structure, growth habits and crystal morphology is discussed. In addition, the thermal properties of the crystal, including the specific heat, thermal expansion, thermal diffusion and thermal conductivity, were carefully investigated. The anisotropy of the crystal thermal conductivities is explained from the point of view of the crystal structure.
Supporting information
Data collection: APEX2 Software Suite (Bruker,2005); cell refinement: APEX2 Software Suite (Bruker,2005); data reduction: APEX2 Software Suite (Bruker,2005); program(s) used to solve structure: SIR97 (Altomare,1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: WinGX (Farrugia,1999).
Crystal data top
NaO8W2Y0.95Yb0.05 | Dx = 6.649 Mg m−3 |
Mr = 611.81 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41/a | Cell parameters from 995 reflections |
Hall symbol: -I 4ad | θ = 4.3–33.1° |
a = 5.2039 (2) Å | µ = 47.33 mm−1 |
c = 11.2838 (9) Å | T = 293 K |
V = 305.57 (3) Å3 | Plate, colourless |
Z = 2 | 0.23 × 0.15 × 0.03 mm |
F(000) = 527 | |
Data collection top
Bruker APEX2 CCD area-detector diffractometer | 292 independent reflections |
Radiation source: fine-focus sealed tube | 257 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
ϕ and ω scans | θmax = 33.4°, θmin = 4.3° |
Absorption correction: numerical APEX2 Software Suite (Bruker,2005) | h = −6→5 |
Tmin = 0.032, Tmax = 0.313 | k = −7→8 |
1208 measured reflections | l = −17→12 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.028 | w = 1/[σ2(Fo2) + (0.0221P)2 + 2.0193P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.065 | (Δ/σ)max < 0.001 |
S = 1.23 | Δρmax = 2.09 e Å−3 |
292 reflections | Δρmin = −3.04 e Å−3 |
15 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.038 (2) |
Crystal data top
NaO8W2Y0.95Yb0.05 | Z = 2 |
Mr = 611.81 | Mo Kα radiation |
Tetragonal, I41/a | µ = 47.33 mm−1 |
a = 5.2039 (2) Å | T = 293 K |
c = 11.2838 (9) Å | 0.23 × 0.15 × 0.03 mm |
V = 305.57 (3) Å3 | |
Data collection top
Bruker APEX2 CCD area-detector diffractometer | 292 independent reflections |
Absorption correction: numerical APEX2 Software Suite (Bruker,2005) | 257 reflections with I > 2σ(I) |
Tmin = 0.032, Tmax = 0.313 | Rint = 0.044 |
1208 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.028 | 15 parameters |
wR(F2) = 0.065 | 0 restraints |
S = 1.23 | Δρmax = 2.09 e Å−3 |
292 reflections | Δρmin = −3.04 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 | Occ. (<1) |
W1 | 0.5000 | 1.2500 | 0.8750 | 0.0111 (2) | |
Y1 | 0.0000 | 0.7500 | 0.8750 | 0.0090 (4) | 0.475 |
Na1 | 0.0000 | 0.7500 | 0.8750 | 0.0090 (4) | 0.50 |
Yb1 | 0.0000 | 0.7500 | 0.8750 | 0.0090 (4) | 0.025 |
O1 | 0.3443 (7) | 1.0072 (7) | 0.7891 (4) | 0.0195 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
W1 | 0.0110 (2) | 0.0110 (2) | 0.0111 (3) | 0.000 | 0.000 | 0.000 |
Y1 | 0.0108 (5) | 0.0108 (5) | 0.0054 (8) | 0.000 | 0.000 | 0.000 |
Na1 | 0.0108 (5) | 0.0108 (5) | 0.0054 (8) | 0.000 | 0.000 | 0.000 |
Yb1 | 0.0108 (5) | 0.0108 (5) | 0.0054 (8) | 0.000 | 0.000 | 0.000 |
O1 | 0.0173 (17) | 0.0246 (19) | 0.0165 (16) | −0.0035 (16) | 0.0012 (15) | −0.0045 (16) |
Geometric parameters (Å, º) top
W1—O1 | 1.787 (4) | Y1—O1x | 2.424 (4) |
W1—O1i | 1.787 (4) | Y1—O1xi | 2.437 (4) |
W1—O1ii | 1.787 (4) | Y1—O1 | 2.437 (4) |
W1—O1iii | 1.787 (4) | Y1—O1xii | 2.437 (4) |
W1—Yb1iv | 3.6797 (1) | Y1—O1xiii | 2.437 (4) |
W1—Na1iv | 3.6797 (1) | Y1—Na1xiv | 3.8377 (2) |
W1—Na1v | 3.6797 (1) | Y1—Na1xv | 3.8377 (2) |
W1—Yb1v | 3.6797 (1) | Y1—Y1xiv | 3.8377 (2) |
W1—Yb1vi | 3.6797 (1) | Y1—Yb1xv | 3.8377 (2) |
W1—Na1vi | 3.6797 (1) | O1—Yb1viii | 2.424 (4) |
Y1—O1vii | 2.424 (4) | O1—Na1viii | 2.424 (4) |
Y1—O1viii | 2.424 (4) | O1—Y1viii | 2.424 (4) |
Y1—O1ix | 2.424 (4) | | |
| | | |
O1—W1—O1i | 107.10 (13) | O1viii—Y1—O1xii | 73.40 (8) |
O1—W1—O1ii | 107.10 (13) | O1ix—Y1—O1xii | 153.25 (18) |
O1i—W1—O1ii | 114.3 (3) | O1x—Y1—O1xii | 75.74 (14) |
O1—W1—O1iii | 114.3 (3) | O1xi—Y1—O1xii | 99.09 (7) |
O1i—W1—O1iii | 107.10 (13) | O1—Y1—O1xii | 99.09 (7) |
O1ii—W1—O1iii | 107.10 (13) | O1vii—Y1—O1xiii | 75.74 (14) |
O1—W1—Yb1iv | 145.17 (13) | O1viii—Y1—O1xiii | 153.25 (18) |
O1i—W1—Yb1iv | 79.66 (12) | O1ix—Y1—O1xiii | 73.40 (8) |
O1ii—W1—Yb1iv | 100.34 (12) | O1x—Y1—O1xiii | 68.83 (9) |
O1iii—W1—Yb1iv | 34.83 (13) | O1xi—Y1—O1xiii | 99.09 (7) |
O1—W1—Na1iv | 145.17 (13) | O1—Y1—O1xiii | 99.09 (7) |
O1i—W1—Na1iv | 79.66 (12) | O1xii—Y1—O1xiii | 133.2 (2) |
O1ii—W1—Na1iv | 100.34 (12) | O1vii—Y1—Na1xiv | 159.36 (8) |
O1iii—W1—Na1iv | 34.83 (13) | O1viii—Y1—Na1xiv | 70.43 (9) |
Yb1iv—W1—Na1iv | 0.0 | O1ix—Y1—Na1xiv | 37.99 (9) |
O1—W1—Na1v | 79.66 (12) | O1x—Y1—Na1xiv | 100.80 (10) |
O1i—W1—Na1v | 34.83 (13) | O1xi—Y1—Na1xiv | 37.75 (9) |
O1ii—W1—Na1v | 145.17 (13) | O1—Y1—Na1xiv | 101.90 (10) |
O1iii—W1—Na1v | 100.34 (12) | O1xii—Y1—Na1xiv | 131.64 (10) |
Yb1iv—W1—Na1v | 90.0 | O1xiii—Y1—Na1xiv | 85.41 (9) |
Na1iv—W1—Na1v | 90.0 | O1vii—Y1—Na1xv | 37.99 (9) |
O1—W1—Yb1v | 79.66 (12) | O1viii—Y1—Na1xv | 159.36 (8) |
O1i—W1—Yb1v | 34.83 (13) | O1ix—Y1—Na1xv | 100.80 (10) |
O1ii—W1—Yb1v | 145.17 (13) | O1x—Y1—Na1xv | 70.43 (9) |
O1iii—W1—Yb1v | 100.34 (12) | O1xi—Y1—Na1xv | 131.64 (10) |
Yb1iv—W1—Yb1v | 90.0 | O1—Y1—Na1xv | 85.41 (9) |
Na1iv—W1—Yb1v | 90.0 | O1xii—Y1—Na1xv | 101.90 (10) |
Na1v—W1—Yb1v | 0.0 | O1xiii—Y1—Na1xv | 37.75 (9) |
O1—W1—Yb1vi | 100.34 (12) | Na1xiv—Y1—Na1xv | 122.705 (3) |
O1i—W1—Yb1vi | 145.17 (13) | O1vii—Y1—Y1xiv | 159.36 (8) |
O1ii—W1—Yb1vi | 34.83 (13) | O1viii—Y1—Y1xiv | 70.43 (9) |
O1iii—W1—Yb1vi | 79.66 (12) | O1ix—Y1—Y1xiv | 37.99 (9) |
Yb1iv—W1—Yb1vi | 90.0 | O1x—Y1—Y1xiv | 100.80 (10) |
Na1iv—W1—Yb1vi | 90.0 | O1xi—Y1—Y1xiv | 37.75 (9) |
Na1v—W1—Yb1vi | 180.0 | O1—Y1—Y1xiv | 101.90 (10) |
Yb1v—W1—Yb1vi | 180.0 | O1xii—Y1—Y1xiv | 131.64 (10) |
O1—W1—Na1vi | 100.34 (12) | O1xiii—Y1—Y1xiv | 85.41 (9) |
O1i—W1—Na1vi | 145.17 (13) | Na1xiv—Y1—Y1xiv | 0.0 |
O1ii—W1—Na1vi | 34.83 (13) | Na1xv—Y1—Y1xiv | 122.705 (3) |
O1iii—W1—Na1vi | 79.66 (12) | O1vii—Y1—Yb1xv | 37.99 (9) |
Yb1iv—W1—Na1vi | 90.0 | O1viii—Y1—Yb1xv | 159.36 (8) |
Na1iv—W1—Na1vi | 90.0 | O1ix—Y1—Yb1xv | 100.80 (10) |
Na1v—W1—Na1vi | 180.0 | O1x—Y1—Yb1xv | 70.43 (9) |
Yb1v—W1—Na1vi | 180.0 | O1xi—Y1—Yb1xv | 131.64 (10) |
Yb1vi—W1—Na1vi | 0.0 | O1—Y1—Yb1xv | 85.41 (9) |
O1vii—Y1—O1viii | 125.70 (12) | O1xii—Y1—Yb1xv | 101.90 (10) |
O1vii—Y1—O1ix | 125.70 (12) | O1xiii—Y1—Yb1xv | 37.75 (9) |
O1viii—Y1—O1ix | 80.4 (2) | Na1xiv—Y1—Yb1xv | 122.705 (3) |
O1vii—Y1—O1x | 80.4 (2) | Na1xv—Y1—Yb1xv | 0.0 |
O1viii—Y1—O1x | 125.70 (12) | Y1xiv—Y1—Yb1xv | 122.705 (3) |
O1ix—Y1—O1x | 125.70 (12) | W1—O1—Yb1viii | 130.77 (18) |
O1vii—Y1—O1xi | 153.25 (18) | W1—O1—Na1viii | 130.77 (18) |
O1viii—Y1—O1xi | 68.83 (9) | Yb1viii—O1—Na1viii | 0.0 |
O1ix—Y1—O1xi | 75.74 (14) | W1—O1—Y1viii | 130.77 (18) |
O1x—Y1—O1xi | 73.40 (8) | Yb1viii—O1—Y1viii | 0.0 |
O1vii—Y1—O1 | 73.40 (8) | Na1viii—O1—Y1viii | 0.0 |
O1viii—Y1—O1 | 75.74 (14) | W1—O1—Y1 | 120.4 (2) |
O1ix—Y1—O1 | 68.83 (9) | Yb1viii—O1—Y1 | 104.26 (14) |
O1x—Y1—O1 | 153.25 (18) | Na1viii—O1—Y1 | 104.26 (14) |
O1xi—Y1—O1 | 133.2 (2) | Y1viii—O1—Y1 | 104.26 (14) |
O1vii—Y1—O1xii | 68.83 (9) | | |
| | | |
O1i—W1—O1—Yb1viii | −68.56 (13) | O1xi—Y1—O1—W1 | 160.0 (2) |
O1ii—W1—O1—Yb1viii | 168.4 (3) | O1xii—Y1—O1—W1 | −88.3 (3) |
O1iii—W1—O1—Yb1viii | 49.9 (2) | O1xiii—Y1—O1—W1 | 48.3 (2) |
Yb1iv—W1—O1—Yb1viii | 27.9 (4) | Na1xiv—Y1—O1—W1 | 135.48 (19) |
Na1iv—W1—O1—Yb1viii | 27.9 (4) | Na1xv—Y1—O1—W1 | 13.00 (19) |
Na1v—W1—O1—Yb1viii | −46.9 (2) | Y1xiv—Y1—O1—W1 | 135.48 (19) |
Yb1v—W1—O1—Yb1viii | −46.9 (2) | Yb1xv—Y1—O1—W1 | 13.00 (19) |
Yb1vi—W1—O1—Yb1viii | 133.1 (2) | O1vii—Y1—O1—Yb1viii | 134.75 (16) |
Na1vi—W1—O1—Yb1viii | 133.1 (2) | O1viii—Y1—O1—Yb1viii | 0.0 |
O1i—W1—O1—Na1viii | −68.56 (13) | O1ix—Y1—O1—Yb1viii | −85.0 (2) |
O1ii—W1—O1—Na1viii | 168.4 (3) | O1x—Y1—O1—Yb1viii | 146.5 (2) |
O1iii—W1—O1—Na1viii | 49.9 (2) | O1xi—Y1—O1—Yb1viii | −41.50 (10) |
Yb1iv—W1—O1—Na1viii | 27.9 (4) | O1xii—Y1—O1—Yb1viii | 70.18 (5) |
Na1iv—W1—O1—Na1viii | 27.9 (4) | O1xiii—Y1—O1—Yb1viii | −153.18 (17) |
Na1v—W1—O1—Na1viii | −46.9 (2) | Na1xiv—Y1—O1—Yb1viii | −66.00 (13) |
Yb1v—W1—O1—Na1viii | −46.9 (2) | Na1xv—Y1—O1—Yb1viii | 171.52 (13) |
Yb1vi—W1—O1—Na1viii | 133.1 (2) | Y1xiv—Y1—O1—Yb1viii | −66.00 (13) |
Na1vi—W1—O1—Na1viii | 133.1 (2) | Yb1xv—Y1—O1—Yb1viii | 171.52 (13) |
O1i—W1—O1—Y1viii | −68.56 (13) | O1vii—Y1—O1—Na1viii | 134.75 (16) |
O1ii—W1—O1—Y1viii | 168.4 (3) | O1viii—Y1—O1—Na1viii | 0.0 |
O1iii—W1—O1—Y1viii | 49.9 (2) | O1ix—Y1—O1—Na1viii | −85.0 (2) |
Yb1iv—W1—O1—Y1viii | 27.9 (4) | O1x—Y1—O1—Na1viii | 146.5 (2) |
Na1iv—W1—O1—Y1viii | 27.9 (4) | O1xi—Y1—O1—Na1viii | −41.50 (10) |
Na1v—W1—O1—Y1viii | −46.9 (2) | O1xii—Y1—O1—Na1viii | 70.18 (5) |
Yb1v—W1—O1—Y1viii | −46.9 (2) | O1xiii—Y1—O1—Na1viii | −153.18 (17) |
Yb1vi—W1—O1—Y1viii | 133.1 (2) | Na1xiv—Y1—O1—Na1viii | −66.00 (13) |
Na1vi—W1—O1—Y1viii | 133.1 (2) | Na1xv—Y1—O1—Na1viii | 171.52 (13) |
O1i—W1—O1—Y1 | 83.5 (3) | Y1xiv—Y1—O1—Na1viii | −66.00 (13) |
O1ii—W1—O1—Y1 | −39.6 (2) | Yb1xv—Y1—O1—Na1viii | 171.52 (13) |
O1iii—W1—O1—Y1 | −158.0 (3) | O1vii—Y1—O1—Y1viii | 134.75 (16) |
Yb1iv—W1—O1—Y1 | 180.0 | O1viii—Y1—O1—Y1viii | 0.0 |
Na1iv—W1—O1—Y1 | 180.0 | O1ix—Y1—O1—Y1viii | −85.0 (2) |
Na1v—W1—O1—Y1 | 105.20 (19) | O1x—Y1—O1—Y1viii | 146.5 (2) |
Yb1v—W1—O1—Y1 | 105.20 (19) | O1xi—Y1—O1—Y1viii | −41.50 (10) |
Yb1vi—W1—O1—Y1 | −74.80 (19) | O1xii—Y1—O1—Y1viii | 70.18 (5) |
Na1vi—W1—O1—Y1 | −74.80 (19) | O1xiii—Y1—O1—Y1viii | −153.18 (17) |
O1vii—Y1—O1—W1 | −23.8 (2) | Na1xiv—Y1—O1—Y1viii | −66.00 (13) |
O1viii—Y1—O1—W1 | −158.5 (3) | Na1xv—Y1—O1—Y1viii | 171.52 (13) |
O1ix—Y1—O1—W1 | 116.45 (14) | Y1xiv—Y1—O1—Y1viii | −66.00 (13) |
O1x—Y1—O1—W1 | −12.0 (4) | Yb1xv—Y1—O1—Y1viii | 171.52 (13) |
Symmetry codes: (i) −y+7/4, x+3/4, −z+7/4; (ii) y−3/4, −x+7/4, −z+7/4; (iii) −x+1, −y+5/2, z; (iv) x+1, y+1, z; (v) x+1, y, z; (vi) x, y+1, z; (vii) y−3/4, −x+5/4, z+1/4; (viii) −x+1/2, −y+3/2, −z+3/2; (ix) x−1/2, y, −z+3/2; (x) −y+3/4, x+1/4, z+1/4; (xi) −x, −y+3/2, z; (xii) y−3/4, −x+3/4, −z+7/4; (xiii) −y+3/4, x+3/4, −z+7/4; (xiv) −x−1/2, −y+3/2, −z+3/2; (xv) −x, −y+2, −z+2. |
Experimental details
Crystal data |
Chemical formula | NaO8W2Y0.95Yb0.05 |
Mr | 611.81 |
Crystal system, space group | Tetragonal, I41/a |
Temperature (K) | 293 |
a, c (Å) | 5.2039 (2), 11.2838 (9) |
V (Å3) | 305.57 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 47.33 |
Crystal size (mm) | 0.23 × 0.15 × 0.03 |
|
Data collection |
Diffractometer | Bruker APEX2 CCD area-detector diffractometer |
Absorption correction | Numerical APEX2 Software Suite (Bruker,2005) |
Tmin, Tmax | 0.032, 0.313 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1208, 292, 257 |
Rint | 0.044 |
(sin θ/λ)max (Å−1) | 0.774 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.065, 1.23 |
No. of reflections | 292 |
No. of parameters | 15 |
Δρmax, Δρmin (e Å−3) | 2.09, −3.04 |
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