Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889806004328/ks5080sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0021889806004328/ks5080Isup2.fcf |
Data collection: CAD-4-PC (Kretschmar, 1996); cell refinement: CAD-4-PC; data reduction: CFEO (Solans, 1978); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3.2 (Brueggemann & Schmid, 1990); software used to prepare material for publication: PLATON (Spek, 1990).
LuO8W2·K | F(000) = 1208 |
Mr = 709.77 | Dx = 7.686 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 25 reflections |
a = 10.576 (7) Å | θ = 9–21° |
b = 10.214 (7) Å | µ = 54.07 mm−1 |
c = 7.487 (2) Å | T = 293 K |
β = 130.68 (4)° | Sphere, colourless |
V = 613.3 (6) Å3 | 0.2 × 0.2 × 0.2 mm |
Z = 4 |
Enraf-Nonius CAD4 diffractometer | 664 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.034 |
Graphite monochromator | θmax = 30.0°, θmin = 3.2° |
ω/2θ scans | h = −14→11 |
Absorption correction: spherical ? | k = 0→14 |
Tmin = 0.242, Tmax = 0.264 | l = 0→10 |
1875 measured reflections | 3 standard reflections every 120 min. min |
899 independent reflections | intensity decay: none |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.036 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.083 | w = 1/[σ2(Fo2) + (0.0275P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.21 | (Δ/σ)max = 0.002 |
899 reflections | Δρmax = 0.77 e Å−3 |
56 parameters | Δρmin = −0.67 e Å−3 |
LuO8W2·K | V = 613.3 (6) Å3 |
Mr = 709.77 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.576 (7) Å | µ = 54.07 mm−1 |
b = 10.214 (7) Å | T = 293 K |
c = 7.487 (2) Å | 0.2 × 0.2 × 0.2 mm |
β = 130.68 (4)° |
Enraf-Nonius CAD4 diffractometer | 664 reflections with I > 2σ(I) |
Absorption correction: spherical ? | Rint = 0.034 |
Tmin = 0.242, Tmax = 0.264 | 3 standard reflections every 120 min. min |
1875 measured reflections | intensity decay: none |
899 independent reflections |
R[F2 > 2σ(F2)] = 0.036 | 56 parameters |
wR(F2) = 0.083 | 0 restraints |
S = 1.21 | Δρmax = 0.77 e Å−3 |
899 reflections | Δρmin = −0.67 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
W1 | 0.19691 (3) | 0.00005 (2) | 0.73532 (5) | 0.01801 (16) | |
Lu | 0.0000 | 0.72841 (3) | 0.2500 | 0.01989 (19) | |
K | 0.5000 | 0.2027 (3) | 0.7500 | 0.0249 (6) | |
O1 | 0.3768 (7) | −0.0828 (7) | 0.8121 (13) | 0.0462 (16) | |
O2 | 0.0239 (7) | −0.1070 (6) | 0.4722 (11) | 0.0334 (12) | |
O3 | 0.2835 (7) | 0.1522 (6) | 0.8784 (13) | 0.0418 (16) | |
O4 | 0.2003 (6) | −0.0749 (8) | 0.9536 (12) | 0.0402 (14) |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.01930 (19) | 0.0183 (2) | 0.0168 (3) | −0.00007 (7) | 0.0119 (2) | −0.00015 (10) |
Lu | 0.0213 (2) | 0.0194 (2) | 0.0196 (3) | 0.000 | 0.0136 (2) | 0.000 |
K | 0.0237 (8) | 0.0325 (8) | 0.0218 (15) | 0.000 | 0.0162 (9) | 0.000 |
O1 | 0.040 (2) | 0.049 (3) | 0.053 (4) | −0.004 (3) | 0.032 (3) | 0.003 (4) |
O2 | 0.041 (2) | 0.031 (2) | 0.032 (3) | −0.004 (2) | 0.026 (2) | −0.002 (3) |
O3 | 0.042 (2) | 0.040 (3) | 0.039 (4) | 0.002 (3) | 0.025 (2) | 0.005 (4) |
O4 | 0.043 (2) | 0.041 (3) | 0.033 (3) | 0.003 (3) | 0.023 (3) | 0.000 (4) |
W1—O3 | 1.767 (7) | K—O4ii | 2.739 (6) |
W1—O4 | 1.784 (8) | K—O4iv | 2.739 (6) |
W1—O1 | 1.801 (6) | K—O4xiv | 2.786 (8) |
W1—O2 | 1.930 (6) | K—O4xi | 2.786 (8) |
W1—O2i | 2.081 (6) | K—O1ii | 2.894 (8) |
W1—O4ii | 2.265 (8) | K—O1iv | 2.894 (8) |
W1—Luiii | 3.5128 (18) | K—O2xi | 2.976 (7) |
W1—Kiv | 3.648 (3) | K—O2xiv | 2.976 (7) |
W1—Kv | 3.725 (3) | K—O3xv | 3.050 (8) |
W1—K | 3.756 (2) | K—O3 | 3.050 (8) |
W1—Kvi | 4.110 (3) | K—O1 | 3.348 (7) |
Lu—O1vii | 2.217 (7) | K—O1xv | 3.348 (7) |
Lu—O1vi | 2.217 (7) | O1—Luvi | 2.217 (7) |
Lu—O2viii | 2.260 (7) | O1—Kiv | 2.894 (8) |
Lu—O2ix | 2.260 (7) | O2—W1i | 2.081 (6) |
Lu—O3x | 2.299 (7) | O2—Luxvi | 2.260 (7) |
Lu—O3xi | 2.299 (7) | O2—Kv | 2.976 (7) |
Lu—O3xii | 2.765 (6) | O3—Luxvii | 2.299 (7) |
Lu—O3iii | 2.765 (6) | O3—Luiii | 2.765 (6) |
Lu—W1xii | 3.5128 (18) | O4—W1xviii | 2.265 (8) |
Lu—W1iii | 3.5128 (18) | O4—Kiv | 2.739 (6) |
Lu—Kx | 3.7527 (10) | O4—Kv | 2.786 (8) |
Lu—Kxiii | 3.7527 (10) | ||
O3—W1—O4 | 97.4 (3) | O3xii—Lu—Kx | 70.88 (17) |
O3—W1—O1 | 101.4 (3) | O3iii—Lu—Kx | 112.91 (17) |
O4—W1—O1 | 96.9 (3) | W1xii—Lu—Kx | 68.82 (4) |
O3—W1—O2 | 152.7 (2) | W1iii—Lu—Kx | 118.16 (4) |
O4—W1—O2 | 97.6 (3) | O1vii—Lu—Kxiii | 50.3 (2) |
O1—W1—O2 | 99.3 (3) | O1vi—Lu—Kxiii | 123.0 (2) |
O3—W1—O2i | 82.9 (2) | O2viii—Lu—Kxiii | 52.46 (18) |
O4—W1—O2i | 104.6 (2) | O2ix—Lu—Kxiii | 135.52 (17) |
O1—W1—O2i | 157.4 (3) | O3x—Lu—Kxiii | 122.41 (19) |
O2—W1—O2i | 71.3 (3) | O3xi—Lu—Kxiii | 54.30 (19) |
O3—W1—O4ii | 87.2 (4) | O3xii—Lu—Kxiii | 112.91 (17) |
O4—W1—O4ii | 174.1 (2) | O3iii—Lu—Kxiii | 70.88 (17) |
O1—W1—O4ii | 78.5 (3) | W1xii—Lu—Kxiii | 118.16 (4) |
O2—W1—O4ii | 79.7 (3) | W1iii—Lu—Kxiii | 68.82 (4) |
O2i—W1—O4ii | 79.6 (3) | Kx—Lu—Kxiii | 171.96 (8) |
O3—W1—Luiii | 51.0 (2) | O4ii—K—O4iv | 123.1 (3) |
O4—W1—Luiii | 88.2 (2) | O4ii—K—O4xiv | 153.79 (16) |
O1—W1—Luiii | 152.4 (2) | O4iv—K—O4xiv | 83.1 (2) |
O2—W1—Luiii | 107.00 (19) | O4ii—K—O4xi | 83.1 (2) |
O2i—W1—Luiii | 37.74 (18) | O4iv—K—O4xi | 153.79 (16) |
O4ii—W1—Luiii | 97.58 (19) | O4xiv—K—O4xi | 70.7 (3) |
O3—W1—Kiv | 96.2 (2) | O4ii—K—O1ii | 56.8 (2) |
O4—W1—Kiv | 46.34 (19) | O4iv—K—O1ii | 98.3 (2) |
O1—W1—Kiv | 51.5 (3) | O4xiv—K—O1ii | 125.8 (2) |
O2—W1—Kiv | 110.63 (19) | O4xi—K—O1ii | 96.0 (2) |
O2i—W1—Kiv | 150.7 (2) | O4ii—K—O1iv | 98.3 (2) |
O4ii—W1—Kiv | 129.70 (16) | O4iv—K—O1iv | 56.8 (2) |
Luiii—W1—Kiv | 123.07 (4) | O4xiv—K—O1iv | 96.0 (2) |
O3—W1—Kv | 141.1 (3) | O4xi—K—O1iv | 125.8 (2) |
O4—W1—Kv | 45.6 (2) | O1ii—K—O1iv | 130.0 (3) |
O1—W1—Kv | 95.9 (2) | O4ii—K—O2xi | 107.26 (19) |
O2—W1—Kv | 52.6 (2) | O4iv—K—O2xi | 109.0 (2) |
O2i—W1—Kv | 94.20 (17) | O4xiv—K—O2xi | 57.7 (2) |
O4ii—W1—Kv | 130.63 (18) | O4xi—K—O2xi | 57.94 (19) |
Luiii—W1—Kv | 106.78 (6) | O1ii—K—O2xi | 152.57 (17) |
Kiv—W1—Kv | 68.24 (5) | O1iv—K—O2xi | 70.4 (2) |
O3—W1—K | 53.3 (2) | O4ii—K—O2xiv | 109.0 (2) |
O4—W1—K | 134.64 (19) | O4iv—K—O2xiv | 107.26 (19) |
O1—W1—K | 63.0 (2) | O4xiv—K—O2xiv | 57.94 (19) |
O2—W1—K | 124.4 (2) | O4xi—K—O2xiv | 57.7 (2) |
O2i—W1—K | 104.69 (18) | O1ii—K—O2xiv | 70.4 (2) |
O4ii—W1—K | 46.39 (15) | O1iv—K—O2xiv | 152.57 (17) |
Luiii—W1—K | 94.36 (6) | O2xi—K—O2xiv | 98.4 (3) |
Kiv—W1—K | 97.83 (7) | O4ii—K—O3xv | 112.0 (2) |
Kv—W1—K | 158.64 (6) | O4iv—K—O3xv | 57.6 (2) |
O3—W1—Kvi | 69.5 (2) | O4xiv—K—O3xv | 81.4 (2) |
O4—W1—Kvi | 145.4 (2) | O4xi—K—O3xv | 115.1 (2) |
O1—W1—Kvi | 116.8 (2) | O1ii—K—O3xv | 56.46 (15) |
O2—W1—Kvi | 85.36 (19) | O1iv—K—O3xv | 114.18 (19) |
O2i—W1—Kvi | 43.69 (19) | O2xi—K—O3xv | 138.94 (17) |
O4ii—W1—Kvi | 40.00 (18) | O2xiv—K—O3xv | 57.77 (17) |
Luiii—W1—Kvi | 58.35 (4) | O4ii—K—O3 | 57.6 (2) |
Kiv—W1—Kvi | 160.58 (4) | O4iv—K—O3 | 112.0 (2) |
Kv—W1—Kvi | 131.12 (5) | O4xiv—K—O3 | 115.1 (2) |
K—W1—Kvi | 63.25 (5) | O4xi—K—O3 | 81.4 (2) |
O1vii—Lu—O1vi | 95.7 (4) | O1ii—K—O3 | 114.2 (2) |
O1vii—Lu—O2viii | 98.3 (3) | O1iv—K—O3 | 56.46 (15) |
O1vi—Lu—O2viii | 148.7 (2) | O2xi—K—O3 | 57.77 (17) |
O1vii—Lu—O2ix | 148.7 (2) | O2xiv—K—O3 | 138.94 (17) |
O1vi—Lu—O2ix | 98.3 (3) | O3xv—K—O3 | 160.6 (3) |
O2viii—Lu—O2ix | 83.9 (3) | O4ii—K—O1 | 49.3 (2) |
O1vii—Lu—O3x | 76.6 (3) | O4iv—K—O1 | 79.8 (2) |
O1vi—Lu—O3x | 77.1 (2) | O4xiv—K—O1 | 149.3 (2) |
O2viii—Lu—O3x | 133.5 (2) | O4xi—K—O1 | 124.09 (17) |
O2ix—Lu—O3x | 79.4 (2) | O1ii—K—O1 | 81.97 (14) |
O1vii—Lu—O3xi | 77.1 (2) | O1iv—K—O1 | 53.3 (2) |
O1vi—Lu—O3xi | 76.6 (3) | O2xi—K—O1 | 104.71 (19) |
O2viii—Lu—O3xi | 79.4 (2) | O2xiv—K—O1 | 152.15 (18) |
O2ix—Lu—O3xi | 133.5 (2) | O3xv—K—O1 | 109.67 (18) |
O3x—Lu—O3xi | 140.4 (3) | O3—K—O1 | 50.88 (19) |
O1vii—Lu—O3xii | 151.1 (2) | O4ii—K—O1xv | 79.8 (2) |
O1vi—Lu—O3xii | 73.5 (2) | O4iv—K—O1xv | 49.3 (2) |
O2viii—Lu—O3xii | 80.8 (2) | O4xiv—K—O1xv | 124.09 (17) |
O2ix—Lu—O3xii | 60.24 (19) | O4xi—K—O1xv | 149.3 (2) |
O3x—Lu—O3xii | 124.7 (3) | O1ii—K—O1xv | 53.3 (2) |
O3xi—Lu—O3xii | 74.3 (3) | O1iv—K—O1xv | 81.97 (14) |
O1vii—Lu—O3iii | 73.5 (2) | O2xi—K—O1xv | 152.15 (18) |
O1vi—Lu—O3iii | 151.1 (2) | O2xiv—K—O1xv | 104.71 (19) |
O2viii—Lu—O3iii | 60.24 (19) | O3xv—K—O1xv | 50.88 (19) |
O2ix—Lu—O3iii | 80.8 (2) | O3—K—O1xv | 109.67 (18) |
O3x—Lu—O3iii | 74.3 (3) | O1—K—O1xv | 58.8 (3) |
O3xi—Lu—O3iii | 124.7 (3) | W1—O1—Luvi | 153.1 (4) |
O3xii—Lu—O3iii | 127.7 (3) | W1—O1—Kiv | 99.3 (3) |
O1vii—Lu—W1xii | 167.9 (2) | Luvi—O1—Kiv | 93.5 (3) |
O1vi—Lu—W1xii | 94.68 (18) | W1—O1—K | 88.4 (3) |
O2viii—Lu—W1xii | 69.61 (17) | Luvi—O1—K | 102.7 (2) |
O2ix—Lu—W1xii | 34.30 (14) | Kiv—O1—K | 126.7 (2) |
O3x—Lu—W1xii | 111.87 (18) | W1—O2—W1i | 108.7 (3) |
O3xi—Lu—W1xii | 99.33 (17) | W1—O2—Luxvi | 138.5 (3) |
O3xii—Lu—W1xii | 29.77 (14) | W1i—O2—Luxvi | 108.0 (3) |
O3iii—Lu—W1xii | 99.89 (15) | W1—O2—Kv | 96.5 (3) |
O1vii—Lu—W1iii | 94.68 (18) | W1i—O2—Kv | 107.4 (2) |
O1vi—Lu—W1iii | 167.9 (2) | Luxvi—O2—Kv | 90.5 (2) |
O2viii—Lu—W1iii | 34.30 (14) | W1—O3—Luxvii | 138.2 (3) |
O2ix—Lu—W1iii | 69.61 (17) | W1—O3—Luiii | 99.3 (2) |
O3x—Lu—W1iii | 99.33 (17) | Luxvii—O3—Luiii | 105.7 (3) |
O3xi—Lu—W1iii | 111.87 (18) | W1—O3—K | 99.0 (3) |
O3xii—Lu—W1iii | 99.89 (15) | Luxvii—O3—K | 87.95 (19) |
O3iii—Lu—W1iii | 29.77 (14) | Luiii—O3—K | 133.1 (2) |
W1xii—Lu—W1iii | 75.71 (5) | W1—O4—W1xviii | 134.8 (4) |
O1vii—Lu—Kx | 123.0 (2) | W1—O4—Kiv | 105.5 (3) |
O1vi—Lu—Kx | 50.3 (2) | W1xviii—O4—Kiv | 96.8 (2) |
O2viii—Lu—Kx | 135.52 (17) | W1—O4—Kv | 107.1 (3) |
O2ix—Lu—Kx | 52.46 (18) | W1xviii—O4—Kv | 108.5 (3) |
O3x—Lu—Kx | 54.30 (19) | Kiv—O4—Kv | 96.9 (2) |
O3xi—Lu—Kx | 122.41 (19) |
Symmetry codes: (i) −x, −y, −z+1; (ii) x, −y, z−1/2; (iii) −x, −y+1, −z+1; (iv) −x+1, −y, −z+2; (v) x−1/2, y−1/2, z; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z−1/2; (viii) x, y+1, z; (ix) −x, y+1, −z+1/2; (x) x−1/2, y+1/2, z−1; (xi) −x+1/2, y+1/2, −z+3/2; (xii) x, −y+1, z−1/2; (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 | LuO8W2·K |
Mr | 709.77 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 10.576 (7), 10.214 (7), 7.487 (2) |
β (°) | 130.68 (4) |
V (Å3) | 613.3 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 54.07 |
Crystal size (mm) | 0.2 × 0.2 × 0.2 |
Data collection | |
Diffractometer | Enraf-Nonius CAD4 diffractometer |
Absorption correction | Spherical |
Tmin, Tmax | 0.242, 0.264 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1875, 899, 664 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.703 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.083, 1.21 |
No. of reflections | 899 |
No. of parameters | 56 |
Δρmax, Δρmin (e Å−3) | 0.77, −0.67 |
Computer programs: CAD-4-PC (Kretschmar, 1996), CAD-4-PC, CFEO (Solans, 1978), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3.2 (Brueggemann & Schmid, 1990), PLATON (Spek, 1990).