Reactions of Gold(III) Oxo Complexes with Cyclic Alkenes†
Maria A. Cinellu Prof.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorGiovanni Minghetti Prof.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorFabio Cocco
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorSergio Stoccoro Dr.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorAntonio Zucca Dr.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorMario Manassero Prof.
Dipartimento di Chimica Strutturale e Stereochimica Inorganica, Università di Milano, Centro CNR via Venezian 21, 20133 Milano, Italy
Search for more papers by this authorMaria A. Cinellu Prof.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorGiovanni Minghetti Prof.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorFabio Cocco
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorSergio Stoccoro Dr.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorAntonio Zucca Dr.
Dipartimento di Chimica, Università di Sassari via Vienna 2, 07100 Sassari, Italy, Fax: (+39) 079-229-559
Search for more papers by this authorMario Manassero Prof.
Dipartimento di Chimica Strutturale e Stereochimica Inorganica, Università di Milano, Centro CNR via Venezian 21, 20133 Milano, Italy
Search for more papers by this authorSupport from the University of Sassari (60 %) is gratefully acknowledged. We thank Mrs. E. Azara (ICB, CNR, Sassari) and Dr. A. Furesi (PMP, USSL, Sassari) for performing GC-MS and LC-MS analyses. Thanks are also due to Dr. G. A. Chelucci (Dipartimento di Chimica, Università di Sassari) for support in the organic syntheses and simulation of NMR spectra.
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Supporting Information
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(no. 2), a=6.466(1), b=8.822(1), c=17.548(1) Å, α=103.45(1), β=90.38(1), γ=100.97(1)°, V=954.4(2) Å3, Z=2, ρcalcd=2.165 g cm−3, T=150 K, μ(MoKα)=78.4 cm−1, F(000)=596. Reflections measured 19 839, independent 5795 with Rint=0.043. Final R2 (F 2, all reflections)=0.113, wR2=0.165, conventional R1=0.052 for 262 variables. Bruker SMART CCD area detector, MoKα radiation (λ=0.71073 Å), ω-scan mode, θmin=3°, θmax=26°. Structure solved by direct methods and refined by full-matrix least squares. The program used to refine the structure was Personal SDP. CCDC-272640 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from the Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
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- 241H NMR spectra were recorded soon after workup of the reaction mixture. Aldehyde signals (CDCl3): 7: 9.64 (d, 2.0 Hz; 2 H); 8 or 9: 9.63 (d, 2.4 Hz; 1 H); 9 or 8: 9.62 ppm (d, 2.4 Hz; 1 H). Intensities: 7≥(8 + 9); 7≤6 (molar ratio based on CHH-7 of the epoxide at δ=0.70 ppm).
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- 27Complex 3 a and 6 also form upon addition of nb and a catalytic amount (5 %) of HBF4⋅Et2O to 4 a; in this case small amounts of diols 10 and 11 are formed.
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