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C12H36Br20O6Si6Zr5, monoclinic, P121/c1 (no. 14), a = 9.8087(2) Å, b = 22.7606(4) Å, c = 13.6501(2) Å, 3 = 97.645(1)°, V = 3020.3 Å, Z = 2, Rgt(F) = 0.042, wRref(F) = 0.088, T = 150 K. Source of material The compoundwas prepared as abyproduct from the bromination of Zr(C5H5)2Br2 in the presence of silicone grease [1,2], which in other cases can lead to [(CH3)2SiO]7 [3,4] and other related ligand systems [5]. Single crystals were formed directly from the unstirred reaction mixture over a period of two days. Discussion The title compound exists as a salt, with the dication possessing crystallographically imposed inversion symmetry, and being comprised of a trans-ZrBr2 unitwith equatorial coordination arising from the oxygen atoms of a [Me2SiO]6 ring. The Zr—Br distance for the dication is 2.5338(6) Å, while four short and two longZr—O distances are observed, averaging 2.258(3)Å forO1, O2, and 2.577(6) Å for O3. The O1–Zr1–O2 angle is 63.52(1)°, while the O3–Zr1–O1(O2) angles average 58.40(3)°. One sees a corresponding difference in Si–O–Si angles, with the angle about O3 being 159.6(4)°, and the others averaging 145.0(3)°. The O–Si–O and C–Si–C angles fall in narrower ranges, being 90.1(2)° – 91.2(3)° and 116.5(3)° – 118.8(3)°. The coordination of Zr1 may be described as intermediate between octahedral and hexagonal bipyramidal. Compensating for the half-independent dication is a [Zr2Br9] counterion. The Zr—Br (terminal) and Zr—Br (bridging) distances average 2.511(5)Å and 2.752(11)Å, the former being slightly shorter than that found in the dication. The cis Br–Zr–Br angles for pairs of terminal bromides average 98.4(3)°, while for pairs of bridging bromides the average is 79.0(2)°. The /trans/ Br–Zr–Br angles average 166.1(6)°, while the Zr–Br–Zr angles average 85.5°. Z. Kristallogr. NCS 222 (2007) 333-334 / DOI 10.1524/ncrs.2007.0140 333 © by OldenbourgWissenschaftsverlag,München Crystal: colorless plate, size 0.08 × 0.23 × 0.30 mm Wavelength: Mo K2 radiation (0.71073 Å) &: 142.08 cm−1 Diffractometer, scan mode: Nonius KappaCCD, $/* 2(max: 55.74° N(hkl)measured, N(hkl)unique: 13614, 7177 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 5273 N(param)refined: 230 Programs: SIR97 [6], SHELXL-97 [7] Table 1. Data collection and handling. H(1A) 4e 0.4331 −0.1419 0.2215 0.054 H(1B) 4e 0.3873 −0.1821 0.3076 0.054 H(1C) 4e 0.5307 −0.1477 0.3248 0.054 H(2A) 4e 0.1387 −0.0342 0.3249 0.056 H(2B) 4e 0.1140 −0.1036 0.3160 0.056 H(2C) 4e 0.1560 −0.0674 0.2240 0.056 H(3A) 4e 0.6879 0.0147 0.1663 0.053 H(3B) 4e 0.5815 −0.0388 0.1500 0.053 H(3C) 4e 0.6948 −0.0372 0.2458 0.053 H(4A) 4e 0.3353 0.0943 0.2436 0.054 H(4B) 4e 0.3268 0.0514 0.1502 0.054 H(4C) 4e 0.4358 0.1040 0.1618 0.054 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso  * Correspondence author (e-mail: ernst@chem.utah.edu) 5 8 % 2 % / & / %

Crystal structure of hexakis(dimethyl-μ-oxosilane)dibromozirconium(IV) bis(nonabromodizirconate(IV)), [Zr{(CH 3 ) 2 SiO} 6 Br 2 ][Zr 2 Br 9 ] 2