Multilateral Solid-State Metathesis Reactions for the Preparation of Materials with Heteroanions: The [Si(CN2)4]4− Ion
✍ Scribed by Jochen Glaser; H.-Jürgen Meyer
- Publisher
- John Wiley and Sons
- Year
- 2008
- Tongue
- English
- Weight
- 357 KB
- Volume
- 47
- Category
- Article
- ISSN
- 0044-8249
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✦ Synopsis
Experimental section
All manipulations of the starting materials were carried out in a glove box under an Ar atmosphere. Rare-earth trichlorides (RECl 3 , ABCR, 99.9 %), A 2 SiF 6 (Chempur, 99 %), and Li 2 CN 2 (for the preparation of which, see Ref. [19]) were mixed thoroughly in a mortar according to their molar fractions in the formula A(RE)[Si(CN 2 ] 4 ] [see Eq. ( 2); total amount: ca. 200 mg). The mixture was placed in a dry quartzglass ampoule. The ampoule was closed with a quickfit stopper and sealed by melting under vacuum. The reaction mixture was then heated to 550 8C (within 5 h) in a tubular furnace, held at this temperature for 3 days, and then cooled to room temperature by switching off the oven. The glass ampoule with the reaction product was opened in air. The product was then washed with water, rinsed with acetone, and dried at 100 8C in air. Single crystals of ALa[Si(CN 2 ) 4 ] with A = K, Rb were selected under a microscope for X-ray crystal-structure investigations.