10.1002/ejic.201900480
European Journal of Inorganic Chemistry
(C5 or C2), 59.56 (C7a), 46.74 (C9), 33.87 (C7), 32.78 (C7’), 27.37 (C8). MALDI MS
(anthracene matrix): calcd m/z 525.14 [M]●+, obsd m/z 525.14. IR: ν(O-H) 2920 cm-1.
[Pt(CH2CMe2C6H4)(L3)], 3.
This was prepared similarly from [Pt2(CH2CMe2C6H4)2(μ-SMe2)2] (0.196 g, 0.252 mmol) and 2-
C5H4N-CH2-NH-4-C6H4OH, L3 (0.100 g, 0.504 mmol). Yield: 0.187 g, 0.356 mmol, 71%.
NMR in (CD3)2CO at 25°C: δ(1H, 600 MHz) 9.03 (d, 1H, J = 6 Hz, H6a), 8.14 (t, 1H, J = 7 Hz,
H4a), 7.68 (d, 1H, J = 7 Hz, H3a), 7.53 (dd, 1H, J = 6 Hz, 7 Hz, H5a), 7.17(d, 1H, J = 7 Hz,
H6’), 7.13 (t, 1H, H4’), 7.12 (d, 2H, J = 7 Hz, H2, H6), 6.93 (t, J = 6 Hz, NH), 6.73 (d, 2H, J = 7
Hz, H3, H5), 6.71 (t, 1H, J = 7 Hz, H5’), 6.70 (d, 1H, J = 7 Hz, H3’), 4.68 (dd, 1H, J = 16 Hz, 6
Hz, H7a), 4.48 (dd, 1H, J = 16 Hz, 6 Hz, H7a’), 1.93 (d, 1H, J = 9 Hz, H8), 1.69 (d, 1H, J = 9
Hz, H8’), 1.15 (s, 3H, H7), 1.05 (s, 3H, H7’). δ(13C, 151 MHz) 161.19 (C6a), 154.62 (C2a),
148.94, 140.25, 136.62, 133.23, 124.35, 122.70 (C3, C5), 121.49 (C5a), 121.12 (C3a), 115.12
(C2, C6), 61.28 (C7a), 54.05 (C9), 33.65 (C7), 32.88 (C7’), 26.71 (C8). MALDI MS
(anthracene matrix): calcd m/z 525.14 [M]●+, obsd m/z 525.13. IR: ν(O-H) 2920 cm-1.
[Pt(CH2CMe2C6H4)(L4)], 4.
To a stirred solution of [Pt2(CH2CMe2C6H4)2(μ-SMe2)2], (0.196 g, 0.252 mmol) in ether (50 mL)
was added a solution of 2-C5H4NCH=N-2-C6H4OH, L4 (0.100 g, 0.504 mmol) in ether (20 mL).
An immediate color change from yellow to red was observed, and a red precipitate of 4 was
formed. After 3h., the product was separated by filtration, washed with hexane (30 mL) and cold
acetone (10 mL), and dried under vacuum. Yield: 0.220 g, 0.418 mmol, 83%. NMR in CD2Cl2 at
-20°C: δ(1H) 9.38 (s, 1H, 3JPtH = 27 Hz, H7a), 9.19 (d, 1H, J = 6 Hz, H6a), 8.15 (t, 1H, J = 7 Hz,
H4a), 7.94 (d, 1H, J = 7 Hz, H3a), 7.69 (dd, 1H, J = 6 Hz, 7 Hz, H5a), 7.35 (t, 1H, J = 8 Hz, H5),
7.28 (d, 1H, J = 8 Hz, H3), 7.12 (t, 1H, J = 8 Hz, H4), 6.92 (d, 1H, J = 8 Hz, H6), 6.83 (m, 2H,
H3’, H6’), 6.48 (m, 2H, H5’, H4’), 3.38 (d, 1H, J = 12 Hz, 2JPtH = 100 Hz, H8), 2.48 (d, 1H, J =
2
13
12 Hz, JPtH = 94 Hz, H8’), 1.35 (s, 3H, H7), 1.34 (s, 3H, H7’). C{1H} NMR (CD2Cl2, 151
MHz, -20°C) δ: 168.55 (C2’), 165.46 (C7a), 155.60 (C2a), 151.62 (C2), 149.65 (C6a), 141.36
(C1’), 138.07 (C4a), 137.45 (C1), 134.18 (C4’ or C5’), 129.89 (C5), 128.51 (C5a), 127.96 (C3a),
123.75 (C3’ or C6’), 123.39 (C4’ or C5’), 121.51 (C3’ or C6’), 121.06 (C3), 120.83 (C4),
117.84 (C6), 70.82 (C8), 47.38 (C9), 34.51 (C7,C7’). At room temperature, the 1H spectrum was
similar except that no resonances were observed for the CH2 protons (H8, H8’) and a single
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