Abstract
The structure of cis-(CH3)2Au(O,O′-acac) was investigated by single-crystal X-ray diffraction. It crystallizes in the orthorhombic space group Cmca with unit cell dimensions a = 6.7831(13) Å, b = 15.080(3) Å, c = 18.073(3) Å and α = β = γ = 90°. The molecule is planar but lacks a C2 axis in the solid-state, with two Au–C bond lengths that differ by 0.078(21) Å due to crystal packing effects. The inequivalence of the crystallographic carbon positions is evident in the solid-state 13C CP-MAS NMR spectrum, which was recorded at low temperature due to the thermal sensitivity of the compound during magic-angle spinning. Head-to-tail stacking, which creates short intermolecular paths, was reproduced computationally in a dimer model.
Graphical Abstract
Solid-state Spectroscopic and Structural Investigation of cis -(CH 3 ) Au 2 ( O , O ′-acac)
Miyako Hisamoto • Swarup Chattopadhyay • Juergen Eckert • Guang Wu • Susannah L. Scott
In the solid state, cis-(CH3)2Au(O,O′-acac) has no C2 axis, two different Au–C bond lengths (1.960, 2.038 Å; Δd = 0.078(21) Å) and a close Au–C…C–Au contact; these features give rise to additional features in the 13C CP-MAS NMR spectrum.
Similar content being viewed by others
References
Vicente J, Chicote MT (1999) Coord Chem Rev 193–195:1143
Vicente J, Chicote M-T, Abrisqueta MD, Alvarez-Falcon MM (2003) Organometallics 22:4327
Brain FH, Gibson CS (1939) J Chem Soc 762
Usón R, Laguna A, Laguna M, Abad M (1983) J Organomet Chem 249:437
Vicente J, Bermúdez MD, Carrión FJ, Jones PG (1996) J Organomet Chem 508:53
Usón R, Vicente J, Cirac JA, Chicote MT (1980) J Organomet Chem 198:105
Usón R, Vicente J, Chicote MT (1981) J Organomet Chem 209:271
Vicente J, Bermudez MD, Escribano J, Carrillo MP, Jones PG (1990) J Chem Soc Dalton Trans 3083
Komiya S, Kochi JK (1977) J Am Chem Soc 99:3695
Baum TH, Jones CR (1985) Appl Phys Lett 47:538
Glass GE, Tobias RS (1968) J Organomet Chem 15:481
Klassen RB, Baum TH (1989) Organometallics 8:2477
Semyannikov PP, Zharkova GI, Grankin VM, Tyukalevskaya NM, Igumenov IK (1988) Metalloorg Khim 1:1105
Semyannikov PP, Grankin VM, Igumenov IK, Zharkova GI (1995) J Phys IV C5:213
Okumura M, Tanaka K, Ueda A, Haruta M (1997) Solid State Ionics 95:143
Okumura M, Nakamura S-I, Tsubota S, Nakamura T, Azuma M, Haruta M (1998) Catal Lett 51:53
Guzman J, Gates BC (2003) Langmuir 19:3897
Guzman J, Kuba S, Fierro-Gonzalez JC, Gates BC (2004) Catal Lett 95:77
Guzman J, Anderson BG, Vinod CP, Ramesh K, Niemantsverdriet JW, Gates BC (2005) Langmuir 21:3675
Okumura M, Nakamura S-I, Tsubota S, Nakamura T, Haruta M (1998) Prep Catal VII:277
Sinha AK, Seelan S, Tsubota S, Haruta M (2002) Stud Surf Sci Catal 143:167
Haruta M (2002) Cattech 6:102
Zharkova GI, Baidina IA, Igumenov IK (2006) J Struct Chem 47:1117. Unfortunately, the crystal structure of (CH3)2Au(acac) described in this paper is not available from the Cambridge Crystallographic Database
Shibata S, Iijima K (1990) J Chem Soc Dalton Trans 1519
Hisamoto M, Scott SL (2008) Spectrochim Acta A (in press)
Fung BM, Khitrin AK, Ermolaev K (2000) J Magn Reson 142:97
SMART (1999) Bruker Advanced X-ray Solutions. Inc, Madison, WI
SAINT (1999) Bruker advanced x-ray solutions. Madison, WI
Sheldrick GM (2001) SHELXTL. Bruker Advanced X-ray Solutions, Inc., Madison, WI
Frisch MJ, Trucks GW, Schlegel HB, Scuseri GE, Robb MA, Cheeseman JR JA, Montgomery J, Vreven T, Kudin KN, Burant JC, Millam JM, Iyengar SS, Tomasi J, Barone V, Mennucci B, Cossi M, Scalmani G, Rega N, Petersson GA, Nakatsuji H, Hada M, Ehara M, Toyota K, Fukuda R, Hasegawa J, Ishida M, Nakajima T, Honda Y, Kitao O, Nakai H, Klene M, Li X, Knox JE, Hratchian HP, Cross JB, Bakken V, Adamo C, Jaramillo J, Gomperts R, Stratmann RE, Yazyev O, Austin AJ, Cammi R, Pomelli C, Ochterski JW, Ayala PY, Morokuma K, Voth GA, Salvador P, Dannenberg JJ, Zakrzewski VG, Dapprich S, Daniels AD, Strain MC, Farkas O, Malick DK, Rabuck AD, Raghavachari K, Foresman JB, Ortiz JV, Cui Q, Baboul AG, Clifford S, Cioslowski J, Stefanov BB, Liu G, Liashenko A, Piskorz P, Komaromi I, Martin RL, Fox DJ, Keith T, Al-Laham MA, Peng CY, Nanayakkara A, Challacombe M, Gill PMW, Johnson B, Chen W, Wong MW, Gonzalez C, Pople JA (2004) Gaussian 03, revision c.02. Gaussian Inc., Wallingford, CT
Grimmer A-R, Kretschmer A, Cajipe VB (1998) Magn Res Chem 35:86
Grässle U, Strähle J (1985) Z Anorg Allg Chem 531:26
Chen HW, Paparizos C, Fackler JP Jr (1985) Inorg Chim Acta 96:137
Glass GE, Konnert JH, Miles MG, Britton D, Tobias RS (1968) J Am Chem Soc 90:1131
Hisamoto M, Scott SL (submitted)
Vaarkamp M (1998) The accepted error for EXAFS distances, in the absence of systematic fitting errors, is ± 0.02 Å. Catal Today 39:271
Becker B, Dolega A, Konitz A, Wojnowski W (2001) Polyhedron 20:949
Bridson JH, Henderson W, Nicholson BK, Hor TSA (2006) Inorg Chim Acta 359:680
Acknowledgements
This work was funded by the U.S. Department of Energy, Basic Energy Sciences, Catalysis Science Grant No. DE-FG02-03ER15467. The authors thank George Athens for assistance in recording the solid-state NMR spectrum. This work also made use of MRL Central Facilities supported by the MRSEC Program of the National Science Foundation, under award No. DMR05-20415.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Hisamoto, M., Chattopadhyay, S., Eckert, J. et al. Solid-state Spectroscopic and Structural Investigation of cis-(CH3)2Au(O,O′-acac). J Chem Crystallogr 39, 173–177 (2009). https://doi.org/10.1007/s10870-008-9449-0
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10870-008-9449-0