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1.
Dalton Trans ; 45(29): 11644-9, 2016 Aug 07.
Artigo em Inglês | MEDLINE | ID: mdl-27221148

RESUMO

A new synthetic approach to highly flexible bis-phospholanes from 1-benzylphospholane (1) as starting material is described. Silver(i) macrocycles containing 16 ([Ag2(µ-3a)2](BF4)2, 4), 20 ([Ag2(µ-3b)2](BF4)2, 5), 24 ([Ag2(µ-3c)2](BF4)2, 6), and 28 ([Ag2(µ-3d)2](BF4)2, 7) atoms in the ring were obtained in one step from AgBF4 and the respective bis-phospholane (C4H8P)(CH2)n(PC4H8) (n = 5, 7, 9, 11; 3a-d) in excellent yields. Comparison of 6 with the previously reported isomorphous complex [Au2(µ-3c)2](BF4)2 gave further evidence that gold(i) is significantly smaller than silver(i). All complexes were fully characterized by NMR and IR spectroscopy, mass spectrometry, and X-ray diffraction.

2.
Dalton Trans ; 44(43): 18760-8, 2015 Nov 21.
Artigo em Inglês | MEDLINE | ID: mdl-26243459

RESUMO

The two highly flexible ligands 1,1'-bis(4-phospholanobutyl)ferrocene (5a) and 1,1'-bis(5-phospholanopentyl)ferrocene (5b) reacted with [PtCl2(cod)] (cod = 1,5-cyclooctadiene), [AuCl(tht)] (tht = tetrahydrothiophene) and [{RhCl(CO)2}2] to give the respective chelate complexes cis-[PtCl2(5a,b-κ(2)P,P')] (7a,b), [AuCl(5a,b-κ(2)P,P')] (8a,b) and trans-[RhCl(CO)(5b-κ(2)P,P')] (9b). Treatment of 5a,b with selenium gave the corresponding selenides 6a,b. All compounds have been fully characterised by NMR ((1)H, (13)C, (31)P) and IR spectroscopy and mass spectrometry. In addition, crystal structures of 6a, 7b, 8a,b and 9b were determined by X-ray crystallography. Furthermore, the rhodium-catalysed hydroformylation of 1-octene has been studied with ligand 5b.

3.
Inorg Chem ; 53(13): 6794-804, 2014 Jul 07.
Artigo em Inglês | MEDLINE | ID: mdl-24945973

RESUMO

A series of highly flexible bis-phospholane ligands 3a-g with 5-11 methylene groups in the backbone was synthesized and fully characterized by mass spectrometry and NMR ((1)H, (13)C, (31)P) and IR spectroscopy. Gold bis-phospholane macrocycles containing 16 ([Au2Cl2(µ-3a)2], 4), 20 ([Au2Cl2(µ-3c)2], 5), 24 ([Au2Cl(µ-3e)2]Cl, 6), and 28 ([Au2Cl2(µ-3g)2], 7) atoms in the ring were obtained in one step from [AuCl(tht)] (tht = tetrahydrothiophene) and 3a,c,e,g in excellent yield. In addition, three polymers resulting from aurophilic interactions, i.e., zigzag chains in [Au2Cl2(µ-3b)]x (8) and nanotubes in [Au2Cl2(µ-3d)]x (9) and [Au2Cl2(µ-3f)]x (10), with Au···Au distances of 309.41(2), 330.24(6), and 335.82(3) pm, respectively, were obtained. Halide abstraction of 4-7 with AgBF4 led to macrocycles [Au2(µ-3a)2](BF4)2 (11), [Au2(µ-3c)2](BF4)2 (12), [Au2(µ-3e)2](BF4)2 (13), and [Au2(µ-3g)2](BF4)2 (14). In 12, the monomers are connected by strong aurophilic interactions (Au···Au 296.57(1) pm) in the solid state with formation of a polymeric chain. All complexes were fully characterized by NMR ((1)H, (13)C, (31)P) and IR spectroscopy, mass spectrometry, and X-ray diffraction.

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