Hexaarsabenzene as Complex Ligand
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Di Maio A.‐J., J. Chem. soc. Chem. Commun., 1987, 404
1H‐NMR (200 MHz C6D6 293 K TMS int.):2a: δ = −0.1 (s 30H) [2].—2b: δ = 0.0l (s 12H) −0.02 (s 12 H) 0.13 (q 3J(H H) = 7.6 Hz 4H) ‐0.4 (t 6H).—3a|4a[2].—3b: δ = 1.66 (s 6H) 1.62 (s 6H) 2.06 (q 3J(H H) = 7.6 Hz 2H) 0.68 (t 3H).—4b: δ = 1.78 (s 12H) 1.75 (s 12H) 2.20 (q 3J(H H) = 7.6 Hz 4H) 0.68 (t 3 H)—IR (n‐heptane) of3b: ṽ(CO) = 1981 (vs) 1924 (vs) cm−1.—IR of4b: ṽ(CO) = 1967 (vs) 1930 (m).—EI‐MS (70 eV 300°C) of2a:m/z912 (M⊕ 73%) 837 (M⊕–As 100) 762 (M⊕‐2 As 22) 456 (M⊕/2 33) 300 (As 32) 225 (As 5) 150 (As 10).
2b: monoclinic P21/n a= 9.174(l) b= 19.854(3) c= 15.174(5)Å β = 94.11(2)° Z= 4; 4610 independent reflections (MoKα 1.5°<θ>26°) 3487 observed withF≥ 2.0σ(F) 301 parameters R= 0.057 Rw= 0.064. One C5Me4Et ring is rotationally disordered. The two orientations differ by a 72° rotation in the ring plane with 50% population each. Further details of the crystal structure investigation are available on request from the Fachinformationszentrum Energie Physik Mathematik GmbH D‐7514 Eggenstein‐Leopoldshafen 2 (FRG) on quoting the depository number CSD‐53417 the names of the authors and the journal citation.
(b)W.Tremel R.Hoffmann M.Kertesz J. Am. Chem. Soc. in press.