Acta Crystallographica Section C

Crystal Structure Communications

Volume 69, Part 9 (September 2013)


Acta Cryst. (2013). C69, 947-953    [ doi:10.1107/S0108270113015898 ]

Improved syntheses, and structural and electronic characterization of carboxamide-substituted TpCONHPh,Me and TpCONHt-Bu,Me ligands

E. R. Sirianni, G. P. A. Yap, E. S. Akturk and K. H. Theopold

Abstract: Improvements in the syntheses of the carboxamide-substituted tris­(pyrazol­yl)borate ligands TpCONHPh,Me [tris­(3-anilino­carbonyl-5-methyl­pyrazol-1-yl)borate] and TpCONHt-Bu,Me [tris­(3-tert-butyl­amino­carbonyl-5-methyl­pyrazol-1-yl)borate] are reported. Their TlI salts, namely [tris­(3-anilino­carbonyl-5-methyl­pyrazol-1-yl-[kappa]N2)borato]thallium(I), [Tl(C33H31BN9O3)], (II), and [tris­(3-tert-butyl­amino­carbonyl-5-methyl­pyrazol-1-yl-[kappa]N2)borato]thallium(I), [Tl(C27H43BN9O3)], (III), as well as the CuI carbonyl complexes (TpCONHPh,Me)Cu(CO), namely carbonyl[tris­(3-anilino­carbonyl-5-methyl­pyrazol-1-yl-[kappa]N2)borato]cop­per(I) tetra­hydro­furan tri­solvate, [Cu(C33H31BN9O3)(CO)]·3C4H8O, (IV), and (TpCONHt-Bu,Me)Cu(CO), namely carbon­yl[tris­(3-tert-butyl­amino­carbonyl-5-methyl­pyrazol-1-yl-[kappa]N2)borato]copper(I) tetra­hydro­furan hemi­solvate, [Cu(C27H43BN9O3)(CO)]·0.5C4H8O, (V), have been prepared. Their spectroscopic properties and structures are compared with those of related compounds. The mol­ecules of (II)-(V) show hydrogen bonding to either solvent mol­ecules or neighboring complex mol­ecules via amide groups. The title compounds feature the ability to engage other ligands in hydrogen bonding and they show strong electron-withdrawing character. Compound (V) displays voids of ca 800 Å3 in the crystal structure.

Formula: [Tl(C33H31BN9O3)], [Tl(C27H43BN9O3)], [Cu(C33H31BN9O3)(CO)]·3C4H8O and [Cu(C27H43BN9O3)(CO)]·0.5C4H8O

Keywords: crystals structure; scorpionates; hydrogen bonding.

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Structure factor file (CIF format) (296.9 kbytes)
[ doi:10.1107/S0108270113015898/eg3122IIsup2.hkl ]
Contains datablock II

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Structure factor file (CIF format) (491.2 kbytes)
[ doi:10.1107/S0108270113015898/eg3122IIIsup3.hkl ]
Contains datablock III

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Structure factor file (CIF format) (1047.7 kbytes)
[ doi:10.1107/S0108270113015898/eg3122IVsup4.hkl ]
Contains datablock IV

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Structure factor file (CIF format) (1052.1 kbytes)
[ doi:10.1107/S0108270113015898/eg3122Vsup5.hkl ]
Contains datablock V


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