UNSPECIFIED (2000) Crown ether complexation of p-block metal halides: synthesis and structural characterisation of [InI2(dibenzo-24-crown-8)(H2O)][InI4], [(SnBr4)(2)(dibenzo-24-crown-8)]center dot MeCN, [(SbCl3)(2)(dibenzo-24-crown-8)]center dot MeCN, [(BiCl3)(2)(dibenzo-24-crown-8)]center dot MeCN and [(SbBr3)(2)(dibenzo-24-crown-8)]. Inorganica Chimica Acta, 300 . pp. 1004-1013. ISSN 0020-1693

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Abstract

The reactions of the large crown ether 6,7,9,10,12, 13,20,21,23,24,26,27-dodecahydrodibenzo[b,n][1,4,7,10,13,16, 19,22]octaoxycyclotetracosine (dibenzo-24-crown-8) with p-block metal halides have been studied, leading to the isolation and structural characterisation of [InI2(dibenzo-24-crown-8)(H2O)][InI4] (I), [(SnBr4)(2)(dibenzo-24-crown-8)]. MeCN (II), [(SbCl3)(2)(dibento-24-crown-8)] (III), [(BiCl3)(2)(dibenzo-24-crown-(8))]. MeCN (IV) and [(SbBr3)(2)(dibenzo-24-crown-8)]. MeCN (V). Compound I was isolated as colourless block crystals; crystals are triclinic, space group P (1) over bar, Z = 2, R = 0.0372. The structure consists of [InI2(dibenzo-24-crown-8)(H2O)](+) cations and [InI4](-) anions. For the cation, the threaded near-linear InI2+ unit (In-I 2.6977(5), 2.6919(5) A) is located off-centre within the cavity and is bonded to four ring oxygen atoms (In-O-crown 2.344(4)-2.560(4) Angstrom) and a single water molecule (In-O-water 2.271(4) Angstrom). The latter forms intracavity hydrogen bonds of the type M-OH2...O-crown to two more of the oxygen atoms of the crown (O-water...O-crown 2.89, 2.94 Angstrom). Compound II was isolated as orange block crystals, crystals are monoclinic, space group I2/m, Z = 2, R = 0.0391. The structure features the two metal centres in exocyclic locations each bound to two oxygens of the ring (Sn-O-crown 2.262(3) Angstrom). The metal geometry is distorted octahedral (Sn-Br 2.5235(7), 2.5187(6) Angstrom). Compound III was isolated as colourless block crystals; crystals are monoclinic, space group C2/c, Z = 4, R = 0.0311. The two SbCl3 moieties (Sb-Cl 2.3807(8), 2.3874(8), 2.4015(9) Angstrom) are coordinated to opposite sides of the crown which adopts a sigmoidal conformation to create two O-5 donor cavities. Each Sb(III) centre is bound to five oxygens of the ring (Sb-O-crown 2.852(2)-3.153(2) Angstrom). Crystals of IV are monoclinic, space group C2/c, Z = 4, R = 0.0325. The structure is directly similar to that of III with two BiCl3 units (Bi-Cl 2.5034(12), 2.5054(13), 2.5389(12) Angstrom) coordinated to opposite sides of the ring which exhibits a sigmoidal conformation. Each Bi(III) centre is bonded to five crown oxygen atoms (Bi-O-crown 2.733(3)-3.221(4) Angstrom). Compound V crystallises in the triclinic space group P (1) over bar, Z = 2, R = 0.0693. The two SbBr3 groups are located on opposite sides of the ring (Sb-Br 2.5268(15), 2.5478(15), 2.5558(14) Angstrom) and each one is bound to four of the ring oxygen atoms (Sb-O-crown 2.893(7)-3.183(8) Angstrom). (C) 2000 Elsevier Science S.A. All rights reserved.

Item Type:	Journal Article
Subjects:	Q Science > QD Chemistry
Journal or Publication Title:	Inorganica Chimica Acta
Publisher:	ELSEVIER SCIENCE SA
ISSN:	0020-1693
Date:	30 April 2000
Volume:	300
Number of Pages:	10
Page Range:	pp. 1004-1013
Publication Status:	Published
URI:	http://wrap.warwick.ac.uk/id/eprint/13322

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