Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806034362/wm2028sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806034362/wm2028Isup2.hkl |
Data collection: XSCANS (Bruker, 2000); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 2000) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.
K2NaH[GeW12O40]·7H2O | Dx = 3.973 Mg m−3 |
Mr = 3147.12 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P6222 | Cell parameters from 250 reflections |
Hall symbol: P62 2c | θ = 2.5–25° |
a = 19.057 (3) Å | µ = 26.92 mm−1 |
c = 12.557 (3) Å | T = 293 K |
V = 3949.3 (13) Å3 | Block, colourless |
Z = 3 | 0.10 × 0.08 × 0.06 mm |
F(000) = 4087 |
Bruker P4 diffractometer | 2165 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.091 |
Graphite monochromator | θmax = 25.1°, θmin = 2.1° |
ω scans | h = −22→22 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −22→22 |
Tmin = 0.174, Tmax = 0.295 | l = 0→14 |
12980 measured reflections | 3 standard reflections every 97 reflections |
2318 independent reflections | intensity decay: none |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0394P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max = 0.001 |
2318 reflections | Δρmax = 1.73 e Å−3 |
155 parameters | Δρmin = −1.25 e Å−3 |
74 restraints | Absolute structure: Flack (1983), with how many Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.61 (3) |
Experimental. IR spectrum (KBr disk, cm-1): 979, 880, 825, 769. |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
K1 | −1.62856 (13) | −0.2571 (3) | 0.5000 | 0.0152 (10) | |
Ge1 | −1.5000 | −0.5000 | 0.3333 | 0.0065 (6) | |
W1 | −1.62679 (4) | −0.63466 (4) | 0.53271 (4) | 0.01136 (15) | |
W2 | −1.70650 (3) | −0.55520 (4) | 0.32408 (5) | 0.01000 (15) | |
W3 | −1.56860 (4) | −0.41735 (4) | 0.53160 (4) | 0.00986 (15) | |
O1 | −1.6984 (7) | −0.6857 (6) | 0.6270 (7) | 0.015 (2) | |
O2 | −1.8049 (7) | −0.5831 (7) | 0.3523 (8) | 0.017 (2) | |
O3 | −1.6228 (6) | −0.3971 (6) | 0.6223 (7) | 0.012 (2) | |
O4 | −1.6861 (7) | −0.6205 (6) | 0.4210 (8) | 0.016 (2) | |
O5 | −1.5913 (7) | −0.5254 (6) | 0.5683 (8) | 0.015 (2) | |
O6 | −1.7240 (7) | −0.6318 (7) | 0.2112 (7) | 0.015 (2) | |
O7 | −1.6819 (6) | −0.4755 (7) | 0.2140 (7) | 0.014 (2) | |
O8 | −1.6473 (6) | −0.4696 (6) | 0.4214 (7) | 0.009 (2) | |
O9 | −1.4674 (6) | −0.3744 (7) | 0.6046 (7) | 0.015 (2) | |
O10 | −1.5822 (6) | −0.5216 (6) | 0.2524 (7) | 0.007 (2) | |
O1W | −1.6527 (9) | −0.1231 (9) | 0.5176 (11) | 0.039 (3) | |
O2W | −1.5000 | −0.5000 | −0.1192 (11) | 0.021 (4) | |
Na1 | −1.790 (2) | −0.131 (2) | 0.435 (3) | 0.039 (8)* | 0.25 |
O3W | −1.757 (3) | 0.0000 | 0.5000 | 0.083 (16)* | 0.50 |
H1WA | −1.661 (12) | −0.082 (8) | 0.526 (15) | 0.039 (3)* | |
H1WB | −1.699 (6) | −0.138 (12) | 0.487 (13) | 0.039 (3)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
K1 | 0.0145 (19) | 0.013 (2) | 0.018 (2) | 0.0063 (12) | 0.0004 (17) | 0.000 |
Ge1 | 0.0063 (11) | 0.0063 (11) | 0.0090 (14) | 0.0046 (13) | 0.000 | 0.000 |
W1 | 0.0119 (3) | 0.0108 (3) | 0.0167 (3) | 0.0096 (3) | 0.0057 (2) | 0.0073 (2) |
W2 | 0.0045 (3) | 0.0113 (3) | 0.0173 (3) | 0.0063 (3) | 0.0010 (2) | 0.0028 (2) |
W3 | 0.0123 (3) | 0.0108 (3) | 0.0122 (3) | 0.0100 (3) | 0.0034 (2) | 0.0000 (2) |
O1 | 0.015 (2) | 0.015 (2) | 0.015 (2) | 0.0075 (14) | 0.0002 (10) | 0.0011 (10) |
O2 | 0.016 (3) | 0.017 (2) | 0.017 (3) | 0.0085 (14) | 0.0001 (10) | 0.0000 (10) |
O3 | 0.012 (2) | 0.013 (2) | 0.013 (2) | 0.0066 (14) | 0.0003 (10) | −0.0003 (10) |
O4 | 0.016 (3) | 0.016 (3) | 0.016 (3) | 0.0081 (15) | 0.0004 (10) | 0.0000 (10) |
O5 | 0.015 (3) | 0.015 (3) | 0.015 (3) | 0.0074 (15) | −0.0005 (10) | 0.0006 (10) |
O6 | 0.015 (2) | 0.015 (2) | 0.015 (2) | 0.0077 (14) | 0.0000 (10) | −0.0003 (10) |
O7 | 0.014 (2) | 0.014 (2) | 0.015 (2) | 0.0075 (14) | 0.0002 (10) | 0.0000 (10) |
O8 | 0.009 (2) | 0.009 (2) | 0.009 (2) | 0.0045 (13) | −0.0001 (10) | −0.0001 (10) |
O9 | 0.015 (2) | 0.015 (2) | 0.016 (2) | 0.0081 (14) | −0.0001 (10) | 0.0000 (10) |
O10 | 0.008 (2) | 0.007 (2) | 0.007 (2) | 0.0036 (13) | 0.0002 (10) | 0.0005 (10) |
O1W | 0.039 (3) | 0.039 (3) | 0.039 (3) | 0.0198 (19) | 0.0002 (7) | 0.0000 (7) |
O2W | 0.016 (9) | 0.025 (10) | 0.032 (8) | 0.016 (8) | 0.000 | 0.000 |
K1—O3i | 2.708 (9) | W2—O6 | 1.940 (10) |
K1—O3ii | 2.708 (9) | W2—O10 | 2.306 (10) |
K1—O7iii | 2.819 (11) | W3—O3 | 1.706 (10) |
K1—O7iv | 2.819 (11) | W3—O9 | 1.911 (10) |
K1—O1Wv | 2.822 (15) | W3—O8 | 1.914 (9) |
K1—O1W | 2.822 (15) | W3—O7iii | 1.917 (10) |
K1—O3v | 3.127 (10) | W3—O5 | 1.937 (11) |
K1—O3 | 3.127 (10) | W3—O10iii | 2.268 (10) |
K1—W3v | 3.778 (3) | O3—K1iv | 2.708 (9) |
K1—W3 | 3.778 (3) | O6—W1vii | 1.921 (10) |
K1—K1ii | 4.719 (4) | O6—Na1ii | 2.89 (4) |
K1—K1iv | 4.719 (4) | O7—W3iii | 1.917 (10) |
Ge1—O10vi | 1.734 (10) | O7—K1ii | 2.819 (11) |
Ge1—O10 | 1.734 (10) | O9—W1vi | 1.938 (10) |
Ge1—O10vii | 1.734 (10) | O10—W3iii | 2.268 (10) |
Ge1—O10iii | 1.734 (10) | O10—W1vii | 2.286 (10) |
W1—O1 | 1.697 (10) | O1W—Na1 | 2.76 (4) |
W1—O5 | 1.893 (11) | O1W—H1WA | 0.87 (5) |
W1—O4 | 1.903 (10) | O1W—H1WB | 0.87 (5) |
W1—O6vii | 1.921 (10) | O2W—O2Wviii | 1.19 (3) |
W1—O9vi | 1.938 (10) | Na1—O3W | 2.39 (4) |
W1—O10vii | 2.286 (10) | Na1—O6iv | 2.89 (4) |
W2—O2 | 1.711 (11) | Na1—Na1iii | 2.96 (6) |
W2—O8 | 1.893 (9) | Na1—H1WA | 2.4 (2) |
W2—O4 | 1.915 (10) | Na1—H1WB | 1.93 (10) |
W2—O7 | 1.929 (10) | O3W—Na1ix | 2.39 (4) |
O3i—K1—O3ii | 157.9 (5) | O1—W1—O10vii | 169.1 (4) |
O3i—K1—O7iii | 109.8 (3) | O5—W1—O10vii | 85.4 (4) |
O3ii—K1—O7iii | 78.3 (3) | O4—W1—O10vii | 84.9 (4) |
O3i—K1—O7iv | 78.3 (3) | O6vii—W1—O10vii | 72.7 (4) |
O3ii—K1—O7iv | 109.8 (3) | O9vi—W1—O10vii | 72.2 (4) |
O7iii—K1—O7iv | 138.1 (5) | O2—W2—O8 | 102.8 (5) |
O3i—K1—O1Wv | 88.3 (4) | O2—W2—O4 | 102.3 (5) |
O3ii—K1—O1Wv | 74.3 (4) | O8—W2—O4 | 85.6 (4) |
O7iii—K1—O1Wv | 72.7 (4) | O2—W2—O7 | 101.0 (5) |
O7iv—K1—O1Wv | 149.0 (4) | O8—W2—O7 | 88.8 (4) |
O3i—K1—O1W | 74.3 (4) | O4—W2—O7 | 156.7 (5) |
O3ii—K1—O1W | 88.3 (4) | O2—W2—O6 | 99.6 (5) |
O7iii—K1—O1W | 149.0 (4) | O8—W2—O6 | 157.5 (4) |
O7iv—K1—O1W | 72.7 (4) | O4—W2—O6 | 89.4 (4) |
O1Wv—K1—O1W | 76.8 (6) | O7—W2—O6 | 87.2 (4) |
O3i—K1—O3v | 126.1 (2) | O2—W2—O10 | 169.0 (4) |
O3ii—K1—O3v | 72.2 (3) | O8—W2—O10 | 85.8 (4) |
O7iii—K1—O3v | 93.0 (3) | O4—W2—O10 | 85.0 (4) |
O7iv—K1—O3v | 54.5 (3) | O7—W2—O10 | 72.0 (4) |
O1Wv—K1—O3v | 145.6 (3) | O6—W2—O10 | 72.0 (4) |
O1W—K1—O3v | 109.5 (3) | O3—W3—O9 | 100.3 (4) |
O3i—K1—O3 | 72.2 (3) | O3—W3—O8 | 101.2 (4) |
O3ii—K1—O3 | 126.1 (2) | O9—W3—O8 | 158.5 (4) |
O7iii—K1—O3 | 54.5 (3) | O3—W3—O7iii | 98.0 (4) |
O7iv—K1—O3 | 93.0 (3) | O9—W3—O7iii | 88.6 (5) |
O1Wv—K1—O3 | 109.5 (3) | O8—W3—O7iii | 89.0 (4) |
O1W—K1—O3 | 145.6 (3) | O3—W3—O5 | 104.1 (4) |
O3v—K1—O3 | 84.7 (4) | O9—W3—O5 | 89.0 (5) |
O3i—K1—W3v | 100.8 (2) | O8—W3—O5 | 85.3 (4) |
O3ii—K1—W3v | 94.6 (2) | O7iii—W3—O5 | 157.9 (4) |
O7iii—K1—W3v | 111.8 (2) | O3—W3—O10iii | 168.7 (4) |
O7iv—K1—W3v | 29.5 (2) | O9—W3—O10iii | 73.1 (4) |
O1Wv—K1—W3v | 167.3 (3) | O8—W3—O10iii | 85.8 (4) |
O1W—K1—W3v | 97.0 (3) | O7iii—W3—O10iii | 73.0 (4) |
O3v—K1—W3v | 26.52 (17) | O5—W3—O10iii | 85.2 (4) |
O3—K1—W3v | 82.0 (2) | O3—W3—K1 | 54.9 (3) |
O3i—K1—W3 | 94.6 (2) | O9—W3—K1 | 110.7 (4) |
O3ii—K1—W3 | 100.8 (2) | O8—W3—K1 | 82.5 (3) |
O7iii—K1—W3 | 29.5 (2) | O7iii—W3—K1 | 46.3 (3) |
O7iv—K1—W3 | 111.8 (2) | O5—W3—K1 | 152.6 (3) |
O1Wv—K1—W3 | 97.0 (3) | O10iii—W3—K1 | 118.1 (3) |
O1W—K1—W3 | 167.3 (3) | W3—O3—K1iv | 141.1 (5) |
O3v—K1—W3 | 82.0 (2) | W3—O3—K1 | 98.5 (4) |
O3—K1—W3 | 26.52 (17) | K1iv—O3—K1 | 107.7 (3) |
W3v—K1—W3 | 91.16 (10) | W1—O4—W2 | 152.7 (6) |
O3i—K1—K1ii | 158.2 (3) | W1—O5—W3 | 151.7 (6) |
O3ii—K1—K1ii | 39.1 (2) | W1vii—O6—W2 | 121.1 (6) |
O7iii—K1—K1ii | 83.1 (2) | W1vii—O6—Na1ii | 120.8 (8) |
O7iv—K1—K1ii | 80.5 (2) | W2—O6—Na1ii | 106.0 (8) |
O1Wv—K1—K1ii | 112.7 (3) | W3iii—O7—W2 | 120.9 (5) |
O1W—K1—K1ii | 103.9 (3) | W3iii—O7—K1ii | 104.2 (4) |
O3v—K1—K1ii | 33.13 (17) | W2—O7—K1ii | 132.9 (5) |
O3—K1—K1ii | 104.3 (2) | W2—O8—W3 | 152.8 (6) |
W3v—K1—K1ii | 57.58 (8) | W3—O9—W1vi | 120.4 (5) |
W3—K1—K1ii | 88.65 (5) | Ge1—O10—W3iii | 123.1 (5) |
O3i—K1—K1iv | 39.1 (2) | Ge1—O10—W1vii | 122.5 (5) |
O3ii—K1—K1iv | 158.2 (3) | W3iii—O10—W1vii | 94.3 (3) |
O7iii—K1—K1iv | 80.5 (2) | Ge1—O10—W2 | 121.2 (5) |
O7iv—K1—K1iv | 83.1 (2) | W3iii—O10—W2 | 94.1 (4) |
O1Wv—K1—K1iv | 103.9 (3) | W1vii—O10—W2 | 94.1 (4) |
O1W—K1—K1iv | 112.7 (3) | Na1—O1W—K1 | 120.3 (9) |
O3v—K1—K1iv | 104.3 (2) | Na1—O1W—H1WA | 60 (10) |
O3—K1—K1iv | 33.13 (17) | K1—O1W—H1WA | 178 (10) |
W3v—K1—K1iv | 88.65 (5) | Na1—O1W—H1WB | 15 (10) |
W3—K1—K1iv | 57.58 (8) | K1—O1W—H1WB | 105 (10) |
K1ii—K1—K1iv | 132.86 (14) | H1WA—O1W—H1WB | 75 (10) |
O10vi—Ge1—O10 | 108.3 (6) | O3W—Na1—O1W | 93.7 (17) |
O10vi—Ge1—O10vii | 109.6 (7) | O3W—Na1—O6iv | 120.6 (14) |
O10—Ge1—O10vii | 110.5 (6) | O1W—Na1—O6iv | 97.5 (11) |
O10vi—Ge1—O10iii | 110.5 (6) | O3W—Na1—Na1iii | 129.0 (14) |
O10—Ge1—O10iii | 109.6 (7) | O1W—Na1—Na1iii | 125.5 (9) |
O10vii—Ge1—O10iii | 108.3 (6) | O6iv—Na1—Na1iii | 88.3 (15) |
O1—W1—O5 | 102.0 (5) | O3W—Na1—H1WA | 76 (2) |
O1—W1—O4 | 103.4 (5) | O1W—Na1—H1WA | 18.0 (16) |
O5—W1—O4 | 86.0 (4) | O6iv—Na1—H1WA | 107 (4) |
O1—W1—O6vii | 100.0 (5) | Na1iii—Na1—H1WA | 139 (4) |
O5—W1—O6vii | 157.9 (4) | O3W—Na1—H1WB | 100 (6) |
O4—W1—O6vii | 89.1 (4) | O1W—Na1—H1WB | 7 (6) |
O1—W1—O9vi | 99.7 (4) | O6iv—Na1—H1WB | 94 (6) |
O5—W1—O9vi | 89.2 (5) | Na1iii—Na1—H1WB | 120 (6) |
O4—W1—O9vi | 156.9 (4) | H1WA—Na1—H1WB | 25 (6) |
O6vii—W1—O9vi | 87.0 (5) | Na1ix—O3W—Na1 | 150 (3) |
Symmetry codes: (i) x, x−y+1, −z+4/3; (ii) −y−2, x−y+1, z−1/3; (iii) −y−2, −x−2, −z+2/3; (iv) −x+y−3, −x−2, z+1/3; (v) −x+y−3, y, −z+1; (vi) −x−3, −y−1, z; (vii) y−1, x+1, −z+2/3; (viii) −y−2, −x−2, −z−1/3; (ix) x−y, −y, −z+1. |