Acta Crystallographica Section C

Crystal Structure Communications

Volume 69, Part 12 (December 2013)

crystallography, spectroscopy and theory

Acta Cryst. (2013). C69, 1421-1426    [ doi:10.1107/S0108270113024505 ]

RuII-hydride-trop complexes: X-ray single-crystal determination and quantum-chemical calculations

G. Santiso-Quinones, R. Rodriguez-Lugo, V. Sacchetti and H. Grützmacher

Abstract: As part of our search for catalytically active RuII-hydride complexes, we have synthesized and crystallographically characterized three different ruthenium species, namely dihydrido[(SR)-(10,11-[eta])-N-(pyridin-2-ylmethyl-[kappa]N)-5H-di­benzo[a,d]cyclo­hepten-5-amine](tri­phenyl­phosphane-[kappa]P)ruthenium(II) tetra­hydro­furan monosolvate, [RuH2(C21H18N2)(C18H15P)]·C4H8O or (SR)-[RuII(H)2{N-(pyridin-2-yl­meth­yl)tropNH}(PPh3)]·THF, (1), chlorido­{(1SR,2RS)-N,N'-bis­[(10,11-[eta])-5H-dibenzo[a,d]cyclo­hepten-5-amine]­ethane-1,2-di­amine-[kappa]2N,N'}hydridoruthenium(II) di­meth­oxy­ethane hemisolvate, [RuClH(C32H28N2)]·0.5C4H10O2 or (1SR,2RS)-[RuII(H)(Cl){tropNH(CH2)2HNtrop}]·DME, (2), and chlo­rido­{(1SR,2RS)-N,N'-bis­[(10,11-[eta])-5H-dibenzo[a,d]cyclo­hep­ten-5-amine]­propane-1,3-di­amine-[kappa]2N,N'}hydridoruthenium(II), [RuClH(C33H30N2)] or (1SR,2RS)-[RuII(H)(Cl){tropNH(CH2)3HNtrop}], (3), where trop is 5H-dibenzo[a,d]cyclo­hep­tene. In all three complexes, the RuII center resides in an octa­hedral coordination environment. For (1)-(3), the hydride atoms were located in a difference Fourier map and were refined freely. In solution, the 1H NMR spectra of all species show the presence of the hydride resonance. Comparison with quantum-chemical calculations reveals that the crystallographic data sets are plausible. In every case, the prediction is in very good agreement with the observed X-ray data. Not only the observed geometry is predicted well but also the Ru-H(hydride) bond lengths are reproduced remarkably well. Complexes (1) and (2) crystallized in the triclinic P\overline{1} space group, while (3) crystallized in the tetra­gonal space group I41/a. For (3), there is disorder of the axial ligands producing two isomers (in a 98.7:1.3 ratio). Details of the synthesis, characterization, X-ray analysis, and theoretical calculations for complexes (1)-(3) are presented.

Formula: [RuH2(C21H18N2)(C18H15P)]·C4H8O and two analogues

Keywords: crystal structure; quantum-chemical calculations; RuII-hydride-tropamine complexes.

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Structure factor file (CIF format) (368.4 kbytes)
[ doi:10.1107/S0108270113024505/fa3321Isup2.hkl ]
Contains datablock I

hkldisplay filedownload file

Structure factor file (CIF format) (223.5 kbytes)
[ doi:10.1107/S0108270113024505/fa3321IIsup3.hkl ]
Contains datablock II

hkldisplay filedownload file

Structure factor file (CIF format) (319.2 kbytes)
[ doi:10.1107/S0108270113024505/fa3321IIIsup4.hkl ]
Contains datablock III


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