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Synthesis, Crystal Structure, and Bonding of (PCl 4 ) 2 [Mo 2 Cl 10 ], the First Compound in Mo–P–Cl System
Author(s) -
Khvorykh G. V.,
Troyanov S. I.,
Baranov A. I.,
Serov A. A.
Publication year - 1998
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/(sici)1521-3749(199806)624:6<1026::aid-zaac1026>3.0.co;2-r
Subject(s) - triclinic crystal system , crystallography , bond length , crystal structure , chemistry , ionic bonding , single crystal , ion , organic chemistry
An ampule reaction between Mo and PCl 5 at 200 °C yielded (PCl 4 ) 2 [Mo 2 Cl 10 ], the first ternary compound in Mo–P–Cl system. Single crystal X‐ray diffraction gave a triclinic unit cell: a  = 6.870(1), b  = 8.892(2), c  = 9.423(2) Å, α = 100.24(2), β = 95.55(2), γ = 96.12(2)° ( V  = 559.3(2) Å 3 , Z  = 1, sp. gr. P 1, w R 2  = 0.0575 and R 1  = 0.0279. The ionic compound is built from edge sharing bioctahedra [Mo 2 Cl 10 ] 2– and two tetrahedra PCl 4 + . The averaged Mo–Cl b distance, 2.503(1) Å, is longer than the Mo–Cl t distance, 2.33(2) Å. The Mo … Mo distance, 3.77 Å, indicates the absence of a direct Mo–Mo interaction. Semiempirical and ab initio calculations showed the possibility for [Mo 2 Cl 10 ] 2– to exist with long and short Mo to Mo distances, the letter corresponding to the Mo–Mo bond.

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