Issue 5, 2011

Synthetic, spectroscopic, and structural studies on organoimido molybdenum, tungsten, and rhenium phthalocyanines

Abstract

Unprecedented imido phthalocyaninato complexes of pentavalent refractory metals [PcM(NR)Cl] (M = Mo, W, Re; R = tBu: 1, 3, 6, Mes: 2, 4, 7 or Ts: 5) have been synthesized by reductive cyclotetramerization of phthalonitrile in the presence of appropriate bis(imido) complexes of Mo, W and Re as templates. While d1Mo(V) and W(V) species 1–5 show distinctive EPR spectra corresponding to metal centered radicals with hyperfine coupling of two magnetically non-equivalent nitrogen atoms (4 equatorial and 1 axial N), corresponding d2Re(V) compounds 6 and 7 are diamagnetic. [PcMo(NtBu)Cl] 1 crystallizes from 1-chloronaphthalene in the tetragonal space groupP4/n. The molecular structure reveals, that the metal center is located above the plane of the equatorial N4 and displaced towards the axial π-donor ligand. Due to the thermodynamic trans effect the Mo–Cl bond trans to the imido group is elongated to about 2.600(2) Å.

Graphical abstract: Synthetic, spectroscopic, and structural studies on organoimido molybdenum, tungsten, and rhenium phthalocyanines

Supplementary files

Article information

Article type
Paper
Submitted
03 Sep 2010
Accepted
11 Nov 2010
First published
20 Dec 2010

Dalton Trans., 2011,40, 1183-1188

Synthetic, spectroscopic, and structural studies on organoimido molybdenum, tungsten, and rhenium phthalocyanines

W. Darwish, E. Seikel, K. Harms, O. Burghaus and J. Sundermeyer, Dalton Trans., 2011, 40, 1183 DOI: 10.1039/C0DT01166E

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