Synthesis and Crystal Structure of (PCl4)[Re2Cl9]
β Scribed by A. I. Baranov; G. V. Khvorykh; S. I. Troyanov
- Publisher
- John Wiley and Sons
- Year
- 1999
- Tongue
- German
- Weight
- 83 KB
- Volume
- 625
- Category
- Article
- ISSN
- 0372-7874
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β¦ Synopsis
The reaction between PCl 3 and ReCl 5 yielded at 200 Β°C the ionic tetrachlorophosphonium dirhenium nonachloride, (PCl 4 )[Re 2 Cl 9 ]. Single crystal X-ray diffraction analysis revealed a monoclinic unit cell: a = 8.616(3) A Γ , b = 10.449(4) A Γ , c = 9.397(3) A Γ , b = 99.72(3)Β°, V = 833.9(5) A Γ 3 , Z = 2, sp. gr. P2 1 /m, wR 2 = 0.1083 and R 1 = 0.0527. The ionic compound is built from tetrahedra PCl 4 + and face-sharing bioctahedra Re 2 Cl 9 Β± . The ReΒ±Re distance, 2.724 A Γ , indicates the presence of direct Re-Re interaction.
π SIMILAR VOLUMES
An ampule reaction between Mo and PCl 5 at 200 Β°C yielded (PCl 4 ) 2 [Mo 2 Cl 10 ], the first ternary compound in MoΒ±PΒ±Cl system. Single crystal X-ray diffraction gave a triclinic unit cell: a = 6.870(1), b = 8.892(2), c = 9.423(2) A Γ , Ξ± = 100.24(2), b = 95.55(2), c = 96.12(2)Β°(V = 559.3(2) A Γ 3
The crystal structures of Ni(NCNH 2 ) 4 Cl 2 and Co(NCNH 2 ) 4 Cl 2 , the first complexes with cyanamide as a neutral ligand, have been determined from single crystal data (Im3m, Z = 6, a = 1259.3(2) pm, R 1 = 0.0245 for Ni(NCNH 2 ) 4 Cl 2 and a = 1266.3(2) pm, R 1 = 0.0241 for Co(NCNH 2 ) 4 Cl 2 ;