[(Zr6B)Cl11- x I2+ x ] (0 ≤ x ≤ 6):  A New Mixed-Halide Structure with Zigzag Chains of Clusters in Multiply Twinned Crystals

[(Zr6B)Cl11- x I2+ x ] (0 ≤ x ≤ 6):  A New Mixed-Halide Structure with Zigzag Chains of Clusters in Multiply Twinned Crystals

The new [(Zr6B)Cl11 - x I2+ x ] phase (with 0 ≤ x ≤ 6) is obtained from reactions of ZrI4, ZrCl4, and elemental Zr and B for 2−4 weeks in sealed Ta tubing at 800−850 °C. Single crystals of [(Zr6B)Cl6.44(7)I6.56] have been characterized by X-ray diffraction at room temperature (orthorhombic Pbcn, Z =...

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Veröffentlicht in:Inorganic chemistry 2001-03, Vol.40 (7), p.1439-1444
Hauptverfasser: Köckerling, Martin, Willems, Johannes B, Boyle, Paul D
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Willems, Johannes B
Boyle, Paul D
description The new [(Zr6B)Cl11 - x I2+ x ] phase (with 0 ≤ x ≤ 6) is obtained from reactions of ZrI4, ZrCl4, and elemental Zr and B for 2−4 weeks in sealed Ta tubing at 800−850 °C. Single crystals of [(Zr6B)Cl6.44(7)I6.56] have been characterized by X-ray diffraction at room temperature (orthorhombic Pbcn, Z = 4, a = 12.365(2) Å, b = 15.485(3) Å, c = 13.405(2) Å). This structure contains zigzag chains of boron-centered (Zr6B) octahedra that are interconnected by Cli-i halides. Further three-dimensional connectivity is achieved by Ia-a-a bridges. The noncluster interconnecting two-bonded Xi sites are occupied statistically by a mixture of Cl and I. For each site both positions were resolved. This structure forms within a phase width of 0 ≤ x ≤ 6 at temperatures between 800 and 850 °C. Crystals of this phase appear to be always multiply twinned.
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Single crystals of [(Zr6B)Cl6.44(7)I6.56] have been characterized by X-ray diffraction at room temperature (orthorhombic Pbcn, Z = 4, a = 12.365(2) Å, b = 15.485(3) Å, c = 13.405(2) Å). This structure contains zigzag chains of boron-centered (Zr6B) octahedra that are interconnected by Cli-i halides. Further three-dimensional connectivity is achieved by Ia-a-a bridges. The noncluster interconnecting two-bonded Xi sites are occupied statistically by a mixture of Cl and I. For each site both positions were resolved. This structure forms within a phase width of 0 ≤ x ≤ 6 at temperatures between 800 and 850 °C. 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Chem</addtitle><description>The new [(Zr6B)Cl11 - x I2+ x ] phase (with 0 ≤ x ≤ 6) is obtained from reactions of ZrI4, ZrCl4, and elemental Zr and B for 2−4 weeks in sealed Ta tubing at 800−850 °C. Single crystals of [(Zr6B)Cl6.44(7)I6.56] have been characterized by X-ray diffraction at room temperature (orthorhombic Pbcn, Z = 4, a = 12.365(2) Å, b = 15.485(3) Å, c = 13.405(2) Å). This structure contains zigzag chains of boron-centered (Zr6B) octahedra that are interconnected by Cli-i halides. Further three-dimensional connectivity is achieved by Ia-a-a bridges. The noncluster interconnecting two-bonded Xi sites are occupied statistically by a mixture of Cl and I. For each site both positions were resolved. This structure forms within a phase width of 0 ≤ x ≤ 6 at temperatures between 800 and 850 °C. 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Chem</addtitle><date>2001-03-26</date><risdate>2001</risdate><volume>40</volume><issue>7</issue><spage>1439</spage><epage>1444</epage><pages>1439-1444</pages><issn>0020-1669</issn><eissn>1520-510X</eissn><abstract>The new [(Zr6B)Cl11 - x I2+ x ] phase (with 0 ≤ x ≤ 6) is obtained from reactions of ZrI4, ZrCl4, and elemental Zr and B for 2−4 weeks in sealed Ta tubing at 800−850 °C. Single crystals of [(Zr6B)Cl6.44(7)I6.56] have been characterized by X-ray diffraction at room temperature (orthorhombic Pbcn, Z = 4, a = 12.365(2) Å, b = 15.485(3) Å, c = 13.405(2) Å). This structure contains zigzag chains of boron-centered (Zr6B) octahedra that are interconnected by Cli-i halides. Further three-dimensional connectivity is achieved by Ia-a-a bridges. The noncluster interconnecting two-bonded Xi sites are occupied statistically by a mixture of Cl and I. For each site both positions were resolved. This structure forms within a phase width of 0 ≤ x ≤ 6 at temperatures between 800 and 850 °C. 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title [(Zr6B)Cl11- x I2+ x ] (0 ≤ x ≤ 6):  A New Mixed-Halide Structure with Zigzag Chains of Clusters in Multiply Twinned Crystals
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