Crystal structure of copper(II) ?-thiopicolinanilidate

Neverov, V. A.; Biyushkin, V. N.; Mazus, M. D.

doi:10.1007/bf00747534

Cited by 2 publications

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“…We report here the twinned crystal structures of tris(ethylenediamine)zinc(II) sulfate, (I), and tris(ethylenediamine)copper(II) sulfate, (II), both measured at 110 (2) K. At room temperature, the corresponding complexes of vanadium (Daniels et al, 1995), cobalt (Yotnoi et al, 2010), nickel (Mazhar-ul-Haque et al, 1970), copper (Cullen & Lingafelter, 1970) and zinc (Neverov et al, 1990) are isostructural in the trigonal space group P31c and the metal complex is a racemic mixture of the and isomers. There has also been a report of an isostructural manganese complex (Lu, 2009), but because of the positive residual electron density on the site of the metal and the unusually short metal-nitrogen distance we regard this structure with due care.…”

Section: Commentmentioning

confidence: 97%

Twinned low-temperature structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate

Lutz

2010

Acta Crystallogr C

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Tris(ethylenediamine)zinc(II) sulfate, [Zn(C(2)H(8)N(2))(3)]SO(4), (I), undergoes a reversible solid-solid phase transition during cooling, accompanied by a lowering of the symmetry from high-trigonal P31c to low-trigonal P3 and by merohedral twinning. The molecular symmetries of the cation and anion change from 32 (D(3)) to 3 (C(3)). This lower symmetry allows an ordered sulfate anion and generates in the complex cation two independent N atoms with significantly different geometries. The twinning is the same as in the corresponding Ni complex [Jameson et al. (1982). Acta Cryst. B38, 3016-3020]. The low-temperature phase of tris(ethylenediamine)copper(II) sulfate, [Cu(C(2)H(8)N(2))(3)]SO(4), (II), has only triclinic symmetry and the unit-cell volume is doubled with respect to the room-temperature structure in P31c. (II) was refined as a nonmerohedral twin with five twin domains. The asymmetric unit contains two independent formula units, and all cations and anions are located on general positions with 1 (C(1)) symmetry. Both molecules of the Cu complex are in elongated octahedral geometries because of the Jahn-Teller effect. This is in contrast to an earlier publication, which describes the complex as a compressed octahedron [Bertini et al. (1979). J. Chem. Soc. Dalton Trans. pp. 1409-1414].

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Section: Commentmentioning

confidence: 97%

Twinned low-temperature structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate

Lutz

2010

Acta Crystallogr C

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“…The crystal structure of (1) was first determined by Neverov et al (1990). It was found to crystallize in the trigonal space group P " 3 31c.…”

Section: Introductionmentioning

confidence: 99%

Temperature-dependent analysis of thermal motion, disorder and structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate

Smeets

Parois

Bürgi

et al. 2011

Acta Crystallogr Sect B

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The crystal structures of the title compounds have been determined in the temperature range 140-290 K for the zinc complex, and 190-270 K for the copper complex. The two structures are isostructural in the trigonal space group P " 3 31c with the sulfate anion severely disordered on a site with 32 (D 3 ) symmetry. This sulfate disorder leads to a disordered three-dimensional hydrogen-bond network, with the N-H atoms acting as donors and the sulfate O atoms as acceptors. The displacement parameters of the N and C atoms in both compounds contain disorder contributions in the out-of-ligand plane direction owing to ring puckering and/or disorder in hydrogen bonding. In the Zn compound the vibrational amplitudes in the bond directions are closely similar. Their differences show no significant deviations from rigid-bond behaviour. In the Cu compound, a (presumably) dynamic Jahn-Teller effect is identified from a temperature-independent contribution to the displacement ellipsoids of the N atom along the N-Cu bond. These conclusions derive from analyses of the atomic displacement parameters with the Hirshfeld test, with rigid-body models at different temperatures, and with a normal coordinate analysis. This analysis considers the atomic displacement parameters (ADPs) from all different temperatures simultaneously and provides a detailed description of both the thermal motion and the disorder in the cation. The Jahn-Teller radii of the Cu compound derived on the basis of the ADP analysis and from the bond distances in the statically distorted low-temperature phase [Lutz (2010). Acta Cryst. C66, m330-m335] are found to be the same.

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Crystal structure of copper(II) ?-thiopicolinanilidate

Cited by 2 publications

References 1 publication

Twinned low-temperature structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate

Twinned low-temperature structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate

Temperature-dependent analysis of thermal motion, disorder and structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate

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