Microwave assisted synthesis of molybdenum and tungsten tetracarbonyl complexes with a pyrazolylpyridine ligand. Crystal structure of cis-[Mo(CO)4{ethyl[3-(2-pyridyl)-1-pyrazolyl]acetate}]

• Published in: Molecules (Basel, Switzerland) Vol. 11; no. 12; pp. 940 - 952
• Main Authors: Coelho, Ana C, Almeida Paz, Filipe A, Klinowski, Jacek, Pillinger, Martyn, Gonçalves, Isabel S
• Format: Journal Article
• Language: English
• Published: Switzerland MDPI AG 06-12-2006
• Subjects: Acetates - chemistry; Crystal structure; Crystallography, X-Ray; Hydrogen Bonding; Ligands; microwave synthesis; Microwaves; Models, Molecular; Molybdenum; Molybdenum - chemistry; Organometallic Compounds - chemical synthesis; Organometallic Compounds - chemistry; pyrazolylpyridine ligand; Pyridines - chemistry; Single crystals; Tetracarbonyl metal complexes; Tungsten - chemistry; X-ray structure
• ISSN: 1420-3049; 1420-3049
• DOI: 10.3390/11120940

We report the one-step syntheses in good yields of the complexes cis-[M(CO)4(pzpy)] {M = Mo, W; pzpy = ethyl[3-(2-pyridyl)-1-pyrazolyl]acetate} directly from the corresponding M(CO)6 starting materials by using microwave-assisted heating and reaction times of either 30 s (M = Mo) or 15 min (M = W). The structure of the molybdenum tetracarbonyl complex was determined by single crystal X-ray diffraction. The compound is monomeric and the molybdenum atom has a highly distorted octahedral geometry. The close packing of the individual cis-[Mo(CO)4(pzpy)] species is essentially driven by the need to fill the space effectively, closely mediated by weak C-H-O and pi-pi interactions.