Sintesi di {Pt 3 }-(CA &-C 4 H 2 S-CA & 2 {Pt 3 } (22)

Ad una sospensione di CuCl (5.4 mg, 0.059 mmoli) in acetone (10 ml) è stato aggiunto TMEDA (10 µl, 0.059 mmoli), e la risultante miscela è stata mantenuta sotto

vigorosa agitazione per 30 minuti; la soluzione verde sopranatante è stata aggiunta ad una soluzione del complesso 15 (114 mg, 0.094 mmoli) in acetone (25 ml), sotto battente di O2. La soluzione risultante è stata lasciata in agitazione per 3 ore; il residuo ottenuto per evaporazione del solvente è stato estratto con CH2Cl2 e purificato tramite cromatografia su silice (eluente: n-esano). Sono stati ottenuti 86 mg di {Pt3}-(CA&- C5H2S-CA&2-{Pt3} (resa del 76 %).

Analisi elementare calcolato (%) per C68H112O4P6Pt6S2: C 33.8, H 4.7; trovato C 33.6, H 4.5.

31_P{1_{H} NMR (81 MHz, CDCl} 3. /SSPG 2JPP = 129 Hz; P1, P3), 100.0 (t, 2JPP = 129 Hz; P2). 1_{H NMR (200 MHz, CDCl} 3. /SSPG 2JHH = 8.3 Hz, 4H, H2H5, C6H4), 6.8 (d, 2_J HH = 8.3 Hz, 4H, H3H4, C6H4), 1.4 (3JHP + 5JHP = 8.1 Hz, 18 H, CCH3), 1.3 (d, 3_J HP =15.6 Hz, 36 H,CCH3). 13_{C NMR (50.3 MHz, CDCl} 3, 293 K) / (ppm); 175.1 (s, CO), 134.6, 127.2 (s, C4H2S), 122.1 (s, Pt-CA&V3W -CAC), 113.6 (s, Ar-CA&-), 98.7 (s, Ar-CAC-), 38.9 (s, -

195_{Pt {}1_{H }(42.3 MHz, CDCl}

3, 293 K) / (ppm) –5726.9 (ddd, 1JPPt =1894 Hz, 1816 Hz, 2_J

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Nel documento Cluster molecolari di platino come sintoni nella sintesi organometallica (pagine 85-93)