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Preparation and characterization of neutral double- and monoalkynyl bridged diplatinum complexes

Preparation and characterization of neutral double- and monoalkynyl bridged diplatinum complexes. Berenguer, Jesus R.; Fornies, Juan; Lalinde, Elena; Martin, Antonio; Serrano, Blanca (Departamento de Quimica-Grupo de Sintesis Quimica de La Rioja, UA-CSIC Universidad de La Rioja, Logrono 26001, Spain). Journal of the Chemical Society, Dalton Transactions, (19), 2926-2936 (English) 2001 Royal Society of Chemistry. CODEN: JCSDAA. ISSN: 1472-7773. DOCUMENT TYPE: Journal CA Section: 29 (Organometallic and Organometalloidal Compounds) Section cross-reference(s): 75 The novel acetylide complexes [trans-Pt(CYCR)2(PPh3)2] [R = (Z)-CMe:CHMe 2a and C(OMe)EtMe 3] have been prepd. starting from [trans-Pt{CYCC(OH)EtMe}2(PPh3)2] 1 by dehydration (2a) and etherification (3) reactions, resp. The analogous a-hydroxyacetylide, R = C(OH)Ph2 4, has been obtained by reaction of [cis-PtCl2(PPh3)2] with HCYCC(OH)Ph2 in NEt2H, in presence of CuI. These bis(acetylide) complexes react with [cis-Pt(C6F5)2(THF)2] leading to sym. diplatinum species [trans,trans-(PPh3)(C6F5)Pt(m-1kCa:h2-CYCR)(m-2kCa:h2-C:CR)Pt(C6 F5)(PPh3)] [R = C(OH)EtMe 5, (Z)-CMe:CHMe 6, C(OMe)EtMe 7, C(OH)Ph2 8] contg. a double alkynyl bridging system. Complexes 5 and 7 have been obtained as mixts. of the corresponding RR/SS and RS/SR diastereomers (1: 1 molar ratio). Treatment of 4-8 with 2 equiv. of PPh3 produces bridge splitting to yield the corresponding mixed mononuclear derivs. [trans-Pt(CYCR)(C6F5)(PPh3)2] [R = C(OH)EtMe 9, (Z)-CMe:CHMe 10, C(OMe)EtMe 11, C(OH)Ph2 12]. Treatment of the hydroxyalkynyl complex 9 with HBF4 in Et2O also produces the dehydrated enynyl deriv. 10. The mononuclear complexes [trans-Pt(CYCR)2(PPh3)2] (1, 3, 4) react with [cis-Pt(C6F5)2(CO)(THF)] to afford, under alkynylation of the carbonyl fragment "Pt(C6F5)2(CO)", the m-h2-acetylide-bridged zwitterionic derivs. [cis,trans-(CO)(C6F5)2Pt(m-1kCa:h2-CYCR)Pt(CYCR)(PPh3)2] [R = C(OH)EtMe 13, C(OMe)EtMe 14, C(OH)Ph2 15]. On the other hand, while the analogous reaction with the bis-enynyl complex 2a is not clean, the related mixed pentafluorophenyl enynyl complex 10 produces the simple displacement of THF from [cis-Pt(C6F5)2(CO)(THF)] by the alkynyl fragment and formation of the adduct [trans,cis-(PPh3)2(C6F5){m-1kCa:h2-C3,4-CYC-(Z)-CMe:CHMe}Pt(C6F5 )2(CO)] 16. The crystal structures of 7, 8 and 13 have also been detd. For complex 8, the dimer units are linked via unusual intermol. hydrogen bonds (O-H Y F-C) leading to an extended polymeric chain along the crystallog. c axis. Keywords alkynyl bridged platinum dinuclear complex prepn crystal mol structure enynyl platinum dinuclear complex prepn crystal mol structure bisalkynyl bridged diplatinum complex hydrogen bond bisalkynylol bridged diplatinum complex Index Entries Crystal structure Molecular structure of bisalkynyl bridged diplatinum complexes Hydrogen bond of bisalkynylol bridged diplatinum complexes 391230-82-3 mol. structure; prepn. and characterization of neutral double- and monoalkynyl bridged diplatinum complexes 204853-08-7 390775-24-3 prepn. and bridge splitting reaction with triphenylphosphine 77-75-8 3923-52-2 15604-36-1 97877-52-6 122619-63-0 60974-81-4 204853-10-1 204933-71-1 390775-21-0 390775-22-1 390775-23-2 390775-27-6 390775-28-7 390775-29-8 prepn. and characterization of neutral double- and monoalkynyl bridged diplatinum complexes 391230-83-4 391231-06-4 prepn. and crystal structure of 390775-30-1 390775-31-2 390775-32-3 390775-33-4 390775-34-5 390775-35-6 390775-36-7 391231-09-7 391231-10-0 prepn. of 390775-25-4 390775-26-5 prepn., mol. structure, and bridge splitting reaction with triphenylphosphine