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Non-order-disorder allotwinning of the rhenium pincer complex cis-Re[(PNPCH2-iPr)(CO)2Cl].

ABSTRACT: Crystals of cis-Re[(PNPCH2-iPr)(CO)2Cl] (1) are made up of two geometrically non-equivalent polytypes with respective symmetries of P21/c and I2/a. The structures were determined in a concurrent refinement, taking into account overlap of diffraction spots. The polytypes are composed of layers with px121/c1 symmetry and are of the non-order-disorder (OD) type (the layer interfaces are non-equivalent). Whereas the molecules of (1) differ in both polytypes, the Re atoms are located at nearly identical positions.

SUBMITTER: Glatz M

PROVIDER: S-EPMC5628399 | biostudies-other | 2017 Oct

REPOSITORIES: biostudies-other

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Non-order-disorder allotwinning of the rhenium pincer complex cis-Re[(PNPCH2-iPr)(CO)2Cl].

Glatz Mathias M Stöger Berthold B Kirchner Karl K

Acta crystallographica Section B, Structural science, crystal engineering and materials 20170927 Pt 5

Crystals of cis-Re[(PNPCH2-iPr)(CO)2Cl] (1) are made up of two geometrically non-equivalent polytypes with respective symmetries of P21/c and I2/a. The structures were determined in a concurrent refinement, taking into account overlap of diffraction spots. The polytypes are composed of layers with px121/c1 symmetry and are of the non-order-disorder (OD) type (the layer interfaces are non-equivalent). Whereas the molecules of (1) d ...[more]

PMID: 28981000

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Project description:This report describes a synthetic protocols and the crystal structures involving a novel pincer-type H3[NNN] ligand, namely di-?-bromido-?-{2-(2,2-di-methylpropanimido-yl)-N-[2-(2,2-di-methyl-propanimido-yl)-4-methyl-phen-yl]-4-methylaniline}-bis-[(diethyl ether)lithium], [Li2Br2(C24H33N3)(C4H10O)2] (1) and a dinuclear metal complex, namely di-?-bromido-2:3?4Br:Br-bis-{2-(2,2-di-methylpropanimido-yl)-N-[2-(2,2-di-methyl-propanimido-yl)-4-methyl-phen-yl]-4-methylaniline}-1?3N,N',N'';4?3N,N',N''-tetra-?-iso-propano-lato-1:2?4O:O;3:4?4O:O-diiso-propano-lato-1?O,4?O-2,3-dilithium-1,4-dititanium, [Li2Ti2Br2(C24H32N3)2(C3H7O)6] or {[NHNNH]Ti(O i Pr)3(LiBr)2}2 (2). Complex 1, which sits on a twofold rotation axis, is a rare example of a pincer-type ligand which bears ketimine side arms. A unique feature of complex 1 is that the ketimine N atoms have an LiBr(Et2O) fragment bonded to them, with the Li atom adopting a distorted tetra-hedral geometry. This particular fragment creates an LiBr bridge between the two ketimine sidearms, which leads to a cage-type appearance of the ligand. Complex 2 consists of the previously described ligand and a TiIV metal atom in an octa-hedral environment, and is located on an inversion center. Complex 2 crystallizes as a dinuclear species with the metal atoms being bridged by an LiBr entity [the Br atoms are disordered and refined in two positions with their site occupation factors refining to 0.674?(12)/0.372?(12)], and the Li cation being bonded to the isopropoxide O atoms (Li having a tetra-hedral coordination as in 1). The organic ligand of compound 2 exhibits disorder in its periphery groups; isopropyl and tert-butyl groups (occupation factors fixed at 0.6/0.4). The novel [NNN]H3 pincer-type ligand was characterized by multinuclear and multidimensional NMR, HRMS and X-ray crystallography. The dinuclear metal complex 2 was characterized by X-ray crystallography. Although each structure exhibits donor N-H groups, no hydrogen bonding is found in either one, perhaps due to the bulky groups around them. One of the ethyl groups of the ether ligand of 1 is disordered and refined in two parts with site-occupation factors of 0.812?(8) and 0.188?(8). One and a half toluene solvent mol-ecules are also present in the asymmetric unit of 2. The toluene mol-ecules were significantly disordered and could not be modeled properly, thus SQUEEZE [Spek (2015 ?). Acta Cryst. C71, 9-18] was used to remove their contributions to the overall intensity data.

Dataset Information

Non-order-disorder allotwinning of the rhenium pincer complex cis-Re[(PNPCH2-iPr)(CO)2Cl].

Publications

Non-order-disorder allotwinning of the rhenium pincer complex cis-Re[(PNP<sup>CH<sub>2</sub></sup>-iPr)(CO)<sub>2</sub>Cl].

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