Abstract
C18H28Mo8N12O26, monoclinic, P21/n (no. 14), a = 11.4563(4) A, b = 12.6941(4) A, c = 14.2248(5) A, ) = 96.385(3)°, V = 2055.9 A, Z = 2, Rgt(F) = 0.054, wRref(F ) = 0.166, T = 293 K. Source of material The pH value of a mixture of (NH4)6Mo7O24.·.4H2O (0.12 g, 0.0001 mol), imidazole (0.27 g, 0.025 mol) in 10 mL distilled water was adjusted to between 2 and 3 by the addition of hydrochloric acid. The resulting solution was heated at 150 °C in a Teflon-lined stainless steel autoclave for 3 days. The reaction system was then slowly cooled to room temperature. Colorless crystals suitable for X-ray diffraction analysis were collected by filtration. Experimental details The carbonand nitrogen-bonded hydrogen atoms were placed at calculated positions (d(C—H) = 0.95 A and d(N—H) = 0.86.A), andwere included in the refinement in a ridingmodel approximation, with Uiso(H) = 1.2 Ueq(C,N). Because of series termination errors, there are still some high residual peaks of differnce electron density after structure refinement (*max = 2.994 e·A and *min = –1.720 e·A). Discussion Polyoxometalates (POMs), a unique class of metal-oxide clusters, have many properties that make them attractive for applications in catalysis, biology,magnetism, optics,medicine, etc. [1]. The anion of the title salt is a centrosymmetricMo8O26 species in which eachMo atom is coordinated by an imidazole heterocycle. The anion is made up of twoMoNO5 and sixMoO6 edge-sharing octahedra. The cations interact with the tetraimidazolium anion to give rise to a three-dimensional hydrogen-bonded network. Z. Kristallogr. NCS 225 (2010) 183-184 / DOI 10.1524/ncrs.2010.0079 183 © by Oldenbourg Wissenschaftsverlag, Munchen Crystal: colorless block, size 0.15 × 0.18 × 0.20 mm Wavelength: Mo K+ radiation (0.71073 A) .: 24.62 cm−1 Diffractometer, scan mode: Oxford Diffraction Gemini R Ultra, % 2,max: 58.52° N(hkl)measured, N(hkl)unique: 9154, 4756 Criterion for Iobs, N(hkl)gt: Iobs > 2 ((Iobs), 2944 N(param)refined: 289 Programs: SHELXS-97 [2], SHELXL-97 [3] Table 1. Data collection and handling.
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