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In K4Sn9, which crystallizes with a new structure type, the Sn atoms form isolated Wade nido-[Sn9]4- clusters of approxi­mate C4v symmetry (monocapped square antiprisms), with Sn-Sn distances ranging from 2.9264 (9) to 3.348 (1) Å. The cluster anions are separated by K+ cations and are in a hexagonal close-packed arrangement.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102002032/br1356sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102002032/br1356Isup2.hkl
Contains datablock I

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP (Johnson, 1968) and DRAWxtl (Finger & Kroeker, 1999); software used to prepare material for publication: SHELXL97.

Tetrapotassium nonastannide top
Crystal data top
K4Sn9F(000) = 2104
Mr = 1224.61Dx = 4.165 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71070 Å
a = 14.238 (2) ÅCell parameters from 980 reflections
b = 8.3554 (13) Åθ = 2.7–28.8°
c = 16.487 (3) ŵ = 12.12 mm1
β = 95.261 (3)°T = 293 K
V = 1953.2 (5) Å3Irregular, metallic light silver
Z = 40.08 × 0.06 × 0.03 mm
Data collection top
Bruker AXS CCD
diffractometer
4575 independent reflections
Radiation source: fine-focus sealed tube3176 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω scansθmax = 28.0°, θmin = 1.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1818
Tmin = 0.432, Tmax = 0.695k = 119
11888 measured reflectionsl = 2116
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.027Secondary atom site location: difference Fourier map
wR(F2) = 0.058 w = 1/[σ2(Fo2) + (0.0174P)2 + 3.425P]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max < 0.001
4575 reflectionsΔρmax = 1.22 e Å3
118 parametersΔρmin = 0.85 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
Sn10.29271 (4)0.61971 (7)0.24040 (4)0.04424 (15)
Sn20.12208 (4)0.60221 (6)0.12012 (3)0.03745 (13)
Sn30.18159 (4)0.32550 (6)0.25293 (3)0.03628 (13)
Sn40.39013 (4)0.31956 (7)0.20216 (3)0.03980 (14)
Sn50.32767 (4)0.61046 (6)0.06830 (4)0.04254 (14)
Sn60.07469 (3)0.25753 (6)0.09188 (3)0.03736 (13)
Sn70.17431 (4)0.43065 (7)0.03032 (3)0.04244 (14)
Sn80.35443 (4)0.26749 (6)0.02620 (3)0.03940 (14)
Sn90.25244 (4)0.07640 (6)0.14252 (3)0.03556 (13)
K10.07578 (12)0.5710 (2)0.76158 (11)0.0464 (5)
K20.50822 (13)0.4386 (2)0.38471 (11)0.0499 (5)
K30.16211 (14)0.5654 (2)0.44653 (12)0.0557 (5)
K40.61160 (13)0.4697 (2)0.14277 (11)0.0483 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0509 (4)0.0366 (3)0.0445 (4)0.0048 (3)0.0003 (3)0.0147 (2)
Sn20.0362 (3)0.0318 (3)0.0455 (4)0.0073 (2)0.0100 (2)0.0015 (2)
Sn30.0416 (3)0.0361 (3)0.0329 (3)0.0011 (2)0.0128 (2)0.0024 (2)
Sn40.0302 (3)0.0431 (3)0.0442 (4)0.0024 (2)0.0065 (2)0.0066 (2)
Sn50.0443 (3)0.0337 (3)0.0521 (4)0.0077 (2)0.0176 (3)0.0004 (2)
Sn60.0281 (3)0.0384 (3)0.0458 (3)0.0065 (2)0.0046 (2)0.0048 (2)
Sn70.0411 (3)0.0568 (4)0.0295 (3)0.0032 (3)0.0035 (2)0.0034 (2)
Sn80.0472 (3)0.0373 (3)0.0363 (3)0.0140 (2)0.0176 (2)0.0065 (2)
Sn90.0339 (3)0.0272 (3)0.0469 (3)0.0016 (2)0.0111 (2)0.0023 (2)
K10.0444 (10)0.0439 (11)0.0535 (12)0.0068 (8)0.0183 (9)0.0017 (8)
K20.0536 (12)0.0516 (12)0.0435 (12)0.0201 (9)0.0007 (9)0.0000 (8)
K30.0570 (13)0.0637 (13)0.0454 (12)0.0131 (10)0.0007 (9)0.0058 (9)
K40.0565 (12)0.0467 (11)0.0437 (11)0.0016 (9)0.0149 (9)0.0087 (8)
Geometric parameters (Å, º) top
Sn1—Sn52.9264 (9)Sn7—K1viii3.773 (2)
Sn1—Sn32.9409 (8)Sn7—K4vi3.8025 (19)
Sn1—Sn42.9616 (9)Sn7—K3iv4.165 (2)
Sn1—Sn22.9955 (9)Sn8—Sn92.9742 (8)
Sn1—K4i3.6926 (19)Sn8—K2v3.6061 (18)
Sn1—K24.003 (2)Sn8—K4vi3.6146 (18)
Sn1—K34.046 (2)Sn8—K2iv3.7604 (19)
Sn1—K1ii4.0669 (19)Sn8—K3iv4.038 (2)
Sn2—Sn62.9847 (9)Sn9—K1iv3.5499 (18)
Sn2—Sn73.0163 (8)Sn9—K3iv3.569 (2)
Sn2—Sn53.1243 (9)Sn9—K2v3.6632 (19)
Sn2—Sn33.2431 (8)Sn9—K4v3.977 (2)
Sn2—K1ii3.6897 (19)K1—Sn9ix3.5499 (18)
Sn2—K1iii3.8526 (19)K1—Sn3ix3.6472 (19)
Sn2—K3ii4.065 (2)K1—Sn6iii3.6647 (18)
Sn3—Sn62.9913 (8)K1—Sn2x3.6897 (19)
Sn3—Sn93.0000 (8)K1—Sn3iii3.7515 (19)
Sn3—Sn43.1584 (9)K1—Sn7xi3.772 (2)
Sn3—K1iv3.6473 (19)K1—Sn2iii3.8526 (19)
Sn3—K1iii3.7514 (19)K1—Sn6ix3.9183 (19)
Sn3—K33.801 (2)K1—Sn1x4.0669 (19)
Sn4—Sn92.9299 (8)K2—Sn8i3.6061 (18)
Sn4—Sn82.9314 (9)K2—Sn5v3.640 (2)
Sn4—Sn53.3480 (9)K2—Sn9i3.6632 (19)
Sn4—K23.4565 (19)K2—Sn8ix3.7604 (19)
Sn4—K43.6113 (19)K2—Sn4i3.8283 (19)
Sn4—K2v3.8282 (19)K3—Sn9ix3.569 (2)
Sn4—K4v3.885 (2)K3—Sn6xii3.735 (2)
Sn5—Sn82.9812 (9)K3—Sn6ix3.889 (2)
Sn5—Sn73.0029 (9)K3—Sn5x4.007 (2)
Sn5—K2i3.640 (2)K3—Sn8ix4.038 (2)
Sn5—K4vi3.723 (2)K3—Sn2x4.065 (2)
Sn5—K3ii4.007 (2)K3—Sn7ix4.165 (2)
Sn6—Sn72.9475 (8)K4—Sn8vi3.6145 (18)
Sn6—Sn93.0008 (8)K4—Sn1v3.6926 (19)
Sn6—K1iii3.6646 (18)K4—Sn5vi3.723 (2)
Sn6—K3vii3.735 (2)K4—Sn7vi3.8025 (19)
Sn6—K3iv3.889 (2)K4—Sn4i3.885 (2)
Sn6—K1iv3.9183 (19)K4—Sn9i3.977 (2)
Sn7—Sn82.9775 (8)
Sn5—Sn1—Sn3100.75 (2)Sn3—Sn4—Sn587.933 (19)
Sn5—Sn1—Sn469.30 (2)Sn1—Sn5—Sn8106.73 (2)
Sn3—Sn1—Sn464.70 (2)Sn1—Sn5—Sn7111.00 (2)
Sn5—Sn1—Sn263.67 (2)Sn8—Sn5—Sn759.68 (2)
Sn3—Sn1—Sn266.222 (19)Sn1—Sn5—Sn259.240 (19)
Sn4—Sn1—Sn2100.66 (2)Sn8—Sn5—Sn2100.69 (2)
Sn6—Sn2—Sn1107.96 (2)Sn7—Sn5—Sn258.94 (2)
Sn6—Sn2—Sn758.832 (19)Sn7—Sn6—Sn261.118 (19)
Sn1—Sn2—Sn7108.75 (2)Sn7—Sn6—Sn3106.02 (2)
Sn6—Sn2—Sn5100.53 (2)Sn2—Sn6—Sn365.734 (18)
Sn1—Sn2—Sn557.09 (2)Sn7—Sn6—Sn989.49 (2)
Sn7—Sn2—Sn558.523 (18)Sn2—Sn6—Sn9105.69 (2)
Sn6—Sn2—Sn357.232 (19)Sn3—Sn6—Sn960.087 (18)
Sn1—Sn2—Sn356.081 (18)Sn6—Sn7—Sn890.92 (2)
Sn7—Sn2—Sn398.49 (2)Sn6—Sn7—Sn5104.30 (2)
Sn5—Sn2—Sn390.40 (2)Sn8—Sn7—Sn559.80 (2)
Sn1—Sn3—Sn6109.24 (2)Sn6—Sn7—Sn260.05 (2)
Sn1—Sn3—Sn9108.92 (2)Sn8—Sn7—Sn2103.32 (2)
Sn6—Sn3—Sn960.114 (19)Sn5—Sn7—Sn262.54 (2)
Sn1—Sn3—Sn457.968 (19)Sn4—Sn8—Sn959.482 (19)
Sn6—Sn3—Sn4100.13 (2)Sn4—Sn8—Sn7107.94 (2)
Sn9—Sn3—Sn456.747 (17)Sn9—Sn8—Sn789.44 (2)
Sn1—Sn3—Sn257.696 (19)Sn4—Sn8—Sn568.97 (2)
Sn6—Sn3—Sn257.035 (19)Sn9—Sn8—Sn5106.59 (2)
Sn9—Sn3—Sn299.58 (2)Sn7—Sn8—Sn560.525 (19)
Sn4—Sn3—Sn291.49 (2)Sn4—Sn9—Sn859.53 (2)
Sn9—Sn4—Sn860.985 (18)Sn4—Sn9—Sn364.35 (2)
Sn9—Sn4—Sn1110.28 (2)Sn8—Sn9—Sn3103.30 (2)
Sn8—Sn4—Sn1107.11 (2)Sn4—Sn9—Sn6105.36 (2)
Sn9—Sn4—Sn358.900 (18)Sn8—Sn9—Sn689.95 (2)
Sn8—Sn4—Sn3100.53 (2)Sn3—Sn9—Sn659.800 (19)
Sn1—Sn4—Sn357.332 (19)
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x, y+3/2, z1/2; (iii) x, y+1, z+1; (iv) x, y+1/2, z1/2; (v) x+1, y1/2, z+1/2; (vi) x+1, y+1, z; (vii) x, y1/2, z+1/2; (viii) x, y, z1; (ix) x, y+1/2, z+1/2; (x) x, y+3/2, z+1/2; (xi) x, y, z+1; (xii) x, y+1/2, z+1/2.
 

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