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Polynuclear cyclometallated palladium(II) complexes. Crystal and molecular structures of [(PPh 3 )(Cl)PdN(Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy) Pd(Cl)(PPh 3 )] and [{PdN(Cy) Ä /C(H)C 6 H 2 C(H) Ä / N(Cy)Pd}{Ph 2 PC(H) Ä /C(H)PPh 2 -P ,P } 2 ][ClO 4 ] 2 Margarit a Lo ´ pez-Torre s a, *, Alberto Ferna ´ ndez a , Jesu ´ s J. Ferna ´ ndez a , Antonio Sua ´ rez a , Samuel Castr o-Ju iz a , M a Teres a Perei ra b , Jos e ´ M. Vila b, * a Departamento de Quı ´mica Fundamental, Uni versidad de La Corun ˜ a, E-15071 La Corun˜ a, Spain b Departamento de Quı ´mica Inorga ´ nica, Uni versidad de Santiago de Compostela, E-15782 Santiago de Compostela, Spain Received 22 Febr uary 2002; acce pted 8 April 2002 Dedicated to Professor Joachim Stra ¨ hle on the occasion of his 65th birthday Abstract Treatment of N ,N -terephthalylidenebis(cyclohexylamine) ( L) with palladium(II) acetate in toluene at room temperature ga ve the dicyclometallated acetato-bridged complex [(OAc)PdN(Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy)Pd(OAc)] n (1). Reaction of 1 with lithiu m chloride or bromide in acetone produced the chloro- or bromo-bridged complexes [(Cl)PdN(Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy)Pd(Cl)] n (2) and [( Br)PdN(Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy)Pd(Br)] n (3), respec tivel y. R ea c ti on of  2 wit h tri phe nyl pho sph ine gave [(PPh 3 )(Cl)PdN(Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy)Pd(Cl)(PPh 3 )] (4). Treatment of 2 and 3 with bis(diphenylphosphino)methane and 1, 5- bi s( di phenylp hosphi no)pentane in a 1:1 molar rati o af forded [{(Cl) PdN( Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy)Pd(Cl)} 2 {m- Ph 2 PCH 2 PPh 2 } 2 ] (5) and [{(Br)PdN(Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy)Pd(Br)} 2 {m-Ph 2 P(CH 2 ) 5 PPh 2 } 2 ] (6), respectively. Reaction of 2 and 3 with bis(diphenylphosphino)methane or cis -1,5-bis(diphenylphosphino)ethene, in a 1:2 molar ratio, and sodium perchlorate, gave di nu cl ear c yc lo me t al late d co m po un ds wi th two ch e la te d p ho sp hi ne l ig an ds [ {P d N( Cy) Ä /C(H)C 6 H 2 C(H) Ä / N(Cy)Pd}{Ph 2 PCH 2 PPh 2 -P ,P } 2 ][ClO 4 ] 2 (7) a nd [{ Pd N( Cy) Ä /C(H)C 6 H 2 C(H) Ä /N(Cy)Pd}{Ph 2 PC(H) Ä /C(H)PPh 2 -P ,P } 2 ][ClO 4 ] 2 (8). The compounds ha ve been fully character ized by elemental analysis, mass spectrometry, IR and NMR spectrosco py, and complexes 4 and 8 by X-ray crystallography. # 2002 Elsevier Science B.V. All rights reserved. Keywords: Cyclometallation; Palladium(II); Phosphines; Schiff-base 1. Introd uction There has been a growing interest in the synthesis of cyclometallated compounds, due to their successful use in, e.g. organi c [1] and asymmetric synthesis [2]; they are also very promising as photoluminiscent compounds [3] and potentially biologically active complexes [4]. Liga nds bearing two don or atoms, whi ch may un- dergo double metallation on the same phenyl ring ha ve been studied by us and by others [5,6]. These ligands are capabl e of binding to two diff er ent metal ce nt er s simulta neousl y in a tetrad entate fashion with format ion of two sMà/C bonds, and consequently gi ve rise to two independent cyclometallated rings: one per each metal atom. Mor e rec entl y, we have been intereste d in the synthesis of doubly cyclometallated complexes deri ved from one of these ligands, namely N ,N -terephthalylide- nebis(cyclohexylamine), which was used in the prepara- tion of new self-assembly supramolecular species [7] and in the synthesis of a no vel pentacoordinated palladiu- m(II) compou nd [8]. As a continuation of our work related to tetradentate [C, N, C, N] Schiff-base ligands, in the present paper we report the synthesis and characterization of new poly- * Correspond ing author. Fax: ' /34-98-159-5012. E-mail address: [email protected] (Jose ´ M. Vi la). Journal of Organometallic Chemistry 655 (2002) 127 Á /133 www.elsevier.com/locate/jorganchem 0022-328X/02/$ - see front matter # 2002 Elsevier Science B.V. All rights reserved. PII: S 0 0 22-3 28X(0 2)014 68-7

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