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나노크기의 카르복실레이토 은(I) 카벤 착체 화합물의 합성 및 특성
Synthesis and Characterization of Nano-sized Carboxylato Silver carbene Complexes
삼성정밀화학연구소 전자재료팀, 대전305-380
Electronic Materials Team, Samsung Fine Chemical, R & D Center, Daejeon 305-380, Korea
ruthenium@korea.com
HWAHAK KONGHAK, August 2002, 40(4), 422-426(5), NONE
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Abstract
본 연구에는 은 carboxylate 착체와 1,3,4,5-tetramethylimidazol-2-ylidenes 배위자와의 반응으로부터 다양한 은 착체화합물(착체1-5)을 얻었다. 합성된 착체는 1H/13C-NMR, FT-IR, UV, 원소분석을 통해 특성을 파악하였다. 특히 착체 2는 X-ray 결정구조해석을 통해 분자구조를 알 수가 있었다. 얻어진 착체 2는 단분자 구조를 보였고, carboxylates가 은 원자를 중심으로 1,3,4,5-tetramethylimidazol-2-ylidene 배위자와 동일 평면상에 존재하고, carboxylates 배위자는 은 원자에 비대칭으로 존재함을 알 수가 있었다. 그리고 착체 2의 1,3,4,5-tetramethylimidazol-2-ylidene중 carbenenic 탄소원자의 화학이동은 free-1,3,4,5-tetramethylimidazol-2-ylidene 보다 34.5-39.7 ppm 정도 고자기장쪽으로 이동됨을 알 수가 있었다.
The complexes of (carboxylato) Ag(I) (1,3,4,5-tetramethylimidazol-2-ylidenes) (complexes 1-5) were prepared by the reaction of silver carboxylates with 1,3,4,5-tetramethylimidazol-2-ylidenes as ligands. The products were characterized by 1H/13C-NMR, FT-IR, UV and elemental analysis. Especially complex 2 consisted of the monomeric units arranged on the same plane on the basis of the result for X-ray crystallographic analysis. The oxygen in carboxylates moiety is asymmetric with respect to silver atom. In the 13C-NMR spectrum, the carbenenic carbon atom in the complexes is shifted upfield by ca. 34.5-39.7 ppm.
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Arduengo AJ, Dias HVR, Harlow RL, Kline M, J. Am. Chem. Soc., 114, 5530 (1992)
Arduengo AJ, Dias HV, Dixon DA, Harlow RL, Klooster WT, Koetzle TF, J. Am. Chem. Soc., 116(15), 6812 (1994)
Arduengo AJ, Goerlich JR, Marshall WJ, J. Am. Chem. Soc., 117(44), 11027 (1995)
Arduengo AJ, Davidson F, Dias HVR, Goerlich JR, Khasnis D, Marshall WJ, Prakasha TK, J. Am. Chem. Soc., 119(52), 12742 (1997)
Arduengo AJ, Davidson F, Krafczyk R, Marshall WJ, Tamm M, Organometallics, 17, 3375 (1998)
Arduengo AJ, Krafczyk R, Schmutzler R, Tetrahedron, 55, 14523 (1999)
Arduengo AJ, Accounts Chem. Res., 32(11), 913 (1999)
Hamilton JG, Frenzel U, Kohl FJ, Weskamp T, Rooney JJ, Herrmann WA, Nuyken O, J. Org. Chem., 606, 8 (2000)
Bohm VPW, Gstottmayr CWK, Weskamp T, Herrmann WA, J. Org. Chem., 595, 186 (2000)
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Weskamp T, Bohm VPW, Herrmann WA, J. Org. Chem., 585, 348 (1999)
Gerdiner MG, Herrmann WA, Reisinger CP, Schwarz J, Spiegler M, J. Org. Chem., 572, 239 (1999)
Herrmann WA, Goossen LJ, Kocher C, Artus GRJ, Angew. Chem.-Int. Edit., 35(23-24), 2805 (1996)
Chung MC, Submitted for Publication
Private Communication with Dr. Byun
Kuhn N, Kratz T, Synthesis, 56 (1993)
Edwards DA, Longley M, J. Inorg. Nucl. Chem., 40, 1599 (1978)
Oldham C, Sandford WF, J. Chem. Soc.-Dalton Trans., 2068 (1977)