CuO nanoparticles were successfully prepared by a one-step solid-state reaction under ambient conditions. Three pellet samples with different grain sizes were obtained by annealing at high temperature. The room temperature Raman spectra of these samples show that as the grain size decreases, the Raman peaks shift to lower wavenumber and become broader owing to size effects. The dependences of the Raman spectra on the wavelength of the excitation laser and temperature were also investigated.

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Three new thiostannates [M(en) 3 ] 2 Sn 2 S 6 (en ϭ ethylenediamine, M ϭ Mn(1), Co(2) and Zn(3)) were synthesized by solvothermal method. The crystals were grown up in a Teflon-lined steel autoclave at temperature about 180°C. All the three compounds consist of discrete [Sn 2 S 6 ] 4Ϫ anions, which are dimer of two tetrahedral SnS 4 sharing a common edge. The transition metal cations are six-coordinated by three ethylenediamine molecules forming octahedral complex ions. Although the synthetic procedures, the mole ratio of the reactants and the solvent are essentially the same, the compound of Mn II is quite different in structure from that of compounds of Co II and Zn II . Compound 1 crystallizes in monoclinic Solvothermale Synthesen und Charakterisierung der Thiostannate [M(en) 3 ] 2 Sn 2 S 6 (M ‫؍‬ Mn, Co, Zn), der Einfluß der Metallionen auf die Kristallstruktur Inhaltsübersicht. Drei neue Thiostannate [M(en) 3 ] 2 Sn 2 S 6 (en ϭ ethylenediamine, M ϭ Mn(1), Co(2) und Zn(3)) wurden durch solvothermale Synthesen präpariert. Die Kristalle wurden in einem teflonausgekleideten Stahlautoklaven bei 180°C gezüchtet. Die drei Verbindungen bestehen aus diskreten [Sn 2 S 6 ] 4Ϫ -Anionen, die Dimere durch zwei über eine gemeinsame Kante verknüpfte SnS 4 ϪTetraeder bilden. Die Übergangsmetallkationen sind sechsfach koordiniert von drei Ethylendiamin-Molekülen unter Bildung eines oktaedrischen, komplexen Ions. Obwohl die synthetische Prozedur, das Molverhältnis der Edukte und das Lösungsmittel völlig gleich

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A two-step solvothermal synthetic method was used for preparation of a one-dimensional compound, [{Mn(en) 2 } 2 (µ-en)(µ-Sn 2 S 6 )] ∞ (1), in which the Mn(II) ions are bridged by thiostannate [Sn 2 S 6 ] 4anions and linear coordinating ethylenediamine (en) molecules. At first, a clear yellow solution containing [Sn 2 S 6 ] 4anions was previously obtained from a SnCl 4 /S/en mixture under solvothermal conditions. Then MnCl 2 ‚6H 2 O was added to the resulted solution, and the solvothermal reaction went on for additional days. Finally pale-yellow crystals of 1 were obtained. Using the same starting materials and in the same molar ratio, however, we obtained a colorless [Mn(en) 3 ] 2 Sn 2 S 6 (2) by the one-step, one-portion solvothermal reaction from a MnCl 2 /SnCl 4 /S/en mixture.