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C22H34CuN10O8, monoclinic, P21/n (no. 14), a = 10.083(1) Å, b = 25.486(3) Å, c = 11.055(1) Å, * = 95.853(1)°, V = 2826.1 Å, Z = 2, Rgt(F) = 0.041, wRref(F) = 0.106, T = 291 K. Source of material The imino nitroxide radical, 2-(2-methylimidazol)-4,4,5,5tetramethyl-2-imidazoline-1-oxyl (IM-MeIm) was prepared according to [1]. The [Cu(IM-MeImz)2(NO3)](NO3) complex was synthesized by adding Cu(NO3)2 · 3H2O (0.240 g, 1 mmol) to 20 mL of an ethanol solution containing IM-MeImz (0.234 g, 1 mmol). The mixture was stirred for 2 h and then filtered; the dark yellow filtrate was allowed to stand at room temperature. Dark yellow crystals suitable for X-ray diffraction analysis were obtained after one week. Discussion During the past decade, nitronyl nitroxide radicals (NITR) have been widely employed as molecular units in the design and synthesis of molecular magnetic materials, due to their exceptional stability and rich chemistry [2-4]. Among many different types of organic radicals, research has focused on the NITR family because of their flexibility and functionality [5,6]. These radicals are especially attractive due to their donor atoms and their ability to assemble extended arrangements with changing magnetic coupling. The family of +-nitronyl nitroxides, such as NITR (R = methyl, ethyl, phenyl, pyridyl, etc.) has been widely studied for a long time. However, +-imidazol-4-yl derivatives have rarely been reported so far. The symmetry independent part of the title crystal structure consists of [Cu(IM-MeImz)2(NO3)] moiety and one uncoordinated NO3 anion. In this complex, copper atom is five-coordinated in a distorted square-pyramidal CuN2O3 environment. The imino nitroxide radical (IM-MeImz) coordinates Cu(II) ion as an unusual six-membered chelate "2N(MeImz) in a O(IM) mode, namely, binding to the metal center through the imino O and imidazole N atom, and forms trans-MN2O2 unit. The squareplanar coordination sites at Cu(II) are occupied by two O atoms (O1, O2) and two N atoms (N1, N5) from the imino nitroxide radical. The bond lengths of Cu1—O1 and Cu1—O2 are 1.919(2) Å and 1.946(2) Å, respectively; the bond lengths of Cu1—N1 and Cu1—N5 are 1.963(2) Å and 1.968(2) Å, respectively, all are in the normal range [7]. The oxygen atom from NO3 occupies axial position. Because Cu(II) ion is Jahn-Teller active, the axial Cu—O distance is longer (2.442 Å). These values correspond well to the literature [8]. The bond angles ∠O1–Cu1–O2, ∠N1–Cu1–O1 and ∠N5–Cu1–O1 are 160.3(1)°, 91.17(9)° and 87.61(9)°, respectively. The Cu(II) ion is slightly displaced by 0.2401 Å out of the basal plane O1–N1–O2–N5. The N—O bond distance is 1.339(3) Å. The dihedral angles between the imino nitroxide moiety (O1, N3, C5, N4) and the imidazole ring of the radical are 15.68° and 8.40°, respectively. There are no significant intermolecular interactions in the structure of the title complex. 768 Z. Kristallogr. NCS 225 (2010) 768-770 / DOI 10.1524/ncrs.2010.0338 © by Oldenbourg Wissenschaftsverlag, München Crystal: yellow block, size 0.14 × 0.22 × 0.38 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 8.37 cm−1 Diffractometer, scan mode: Bruker SMART CCD, #/% 2,max: 51° N(hkl)measured, N(hkl)unique: 21470, 5246 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 3871 N(param)refined: 380 Programs: SHELXS-97, SHELXL-97, SHELXTL [9] Table 1. Data collection and handling.

zeitschrift für kristallographie. new crystal structures/zeitschrift für kristallographie. new crystal structures

Crystal structure of nitratobis[2-(2-methylimidazol)-4,4,5,5-tetramethyl-2-imidazoline-1-oxyl]copper(II) nitrate, [Cu(C 11 H 17 N 4 O) 2 (NO 3 )](NO 3 )