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Syntheses and structural studies of molybdenum‐iron‐sulfur compounds: I. The synthesis and crystal structure of (Et 4 N) 1 [Mo 2 Fe 7 S 8 (SPh) 12 ]
Author(s) -
BeiSheng Kang,
JingHua Cai,
ChangNeng Cheng,
JiaXi Lu
Publication year - 1986
Publication title -
acta chimica sinica english edition
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.28
H-Index - 41
eISSN - 1614-7065
pISSN - 0256-7660
DOI - 10.1002/cjoc.19860040305
Subject(s) - cubane , chemistry , triclinic crystal system , molybdenum , acetonitrile , cluster (spacecraft) , crystal structure , crystallography , stereochemistry , ferrous , sulfur , inorganic chemistry , organic chemistry , computer science , programming language
Through the reactions of ferrous thiolates with tetrathiomolybdate, we discussed the reaction pathways and possible intermediates during the formation of double‐cubane type Mo‐Fe‐S cluster compounds. We also reported the synthesis, crystal structure, IR and magnetic susceptibility measurements of the title compound 2. The crystal of 2 belongs to triclinic system, M r = 2670.3;\documentclass{article}\pagestyle{empty}\begin{document}$$ P\bar 1 $$\end{document} ; a = 12.755(4) Å, b = 13.076(3) Å, c = 20.576(4) Å; α = 80.00 (2)°, β = 81.39(2)°, γ = 61.51(2)°; V = 2966.3(14) Å 3 ; Z = 1; D c = 1.495 g/cm 2 . Final R factor is 0.077 for 4031 observed reflections. The compound was obtained through the reaction of (Et 4 N) 2 [Fe 4 (SPh) 10 ] (1) with (Et 4 N) 2 MoS 4 in acetonitrile solution. The structure of anion 2 is two cubane clusters bridged by a Fe(SPh) 6 group. The Mo… Mo' distance of 7.188 Å is the longest among all double‐cubane cluster compounds of known structures.