4 of 11
KARMAN AND ROMANOWSKI
(DMSO-d6, ppm) mer-isomer (65%): 8.70 (1H, s)
5.6 Hz) (methylene); fac-isomer (35%): 10.27 (1H, s)
(hydroxyl); 8.59 (1H, s) (azomethine); 8.26 (2H, d, J =
3
3
3
(azomethine); 8.24 (2H, d, J = 8.7 Hz), 7.81 (1H, t, J =
3
3
3
3
2.6 Hz), 7.73 (2H, d, J = 8.7 Hz), 7.58 (1H, t, J = 2.6
Hz), 6.87 (1H, d, 3J = 8.8 Hz) (aromatic); 5.25 (1H, t, 3J =
5.2 Hz) (hydroxyl); 5.42 (1H, d, 3J = 6.9 Hz), 3.89 (1H, m)
8.7 Hz), 7.64 (2H, d, J = 8.7 Hz), 7.29 (1H, t, J = 7.4
3
Hz), 6.46 (1H, d, J = 8.2 Hz), 6.27 (1H, s) (aromatic);
5.98 (1H, d, 3J = 4.7 Hz) (hydroxyl); 4.16 (1H, dd, 3J = 9.1
Hz, 4J = 4.1 Hz), 4.06 (1H, ov) (methine); 4.90 (1H, dd, 3J
= 9.3 Hz, 4J = 4.7 Hz), 4.03 (1H, ov) (methylene).
3
4
(methine); 4.03 (1H, ov), 3.62 (1H, dt, J = 12.4 Hz, J =
5.6 Hz) (methylene); fac-isomer (35%): 8.77 (1H, s)
3
3
(azomethine); 8.27 (2H, d, J = 8.7 Hz), 7.85 (1H, t, J =
3
3
2.6 Hz), 7.65 (2H, d, J = 8.7 Hz), 7.60 (1H, t, J = 2.6
Hz), 6.89 (1H, d, 3J = 8.8 Hz) (aromatic); 5.95 (1H, d, 3J =
4.7 Hz) (hydroxyl); 4.13 (1H, dd, J = 9.1 Hz, J = 4.1
Hz), 4.03 (1H, ov) (methine); 4.87 (1H, dd, 3J = 9.3 Hz, 4J
= 4.7 Hz), 4.00 (1H, ov) (methylene).
2.2.9 | MoO2L9
3
4
Yield 78%. Anal. calc for C20H22N2O7Mo: C, 48.2; H,
4.5; N, 5.6. Found: C, 48.3; H, 4.6; N, 5.5%. IR (KBr,
cm−1): 3393 (νO–H); 1633 (νC=N); 1587, 1482 (νC=C); 1528,
1347 (νNO2); 1237 (νC–O); 930, 902 (νMo=O). UV–vis spec-
2.2.7 | MoO2L7
trum in DMSO [λmax (nm), ɛ (M cm−1)]: 280 (10850),
−1
−1
352 (1680). CD spectrum in DMSO [λmax (nm), Δɛ (M
Yield 86%. Anal. calc for C16H13N3O9Mo: C, 39.4; H,
2.7; N, 8.6. Found: C, 39.5; H, 2.6; N, 8.6%. IR (KBr,
cm−1): 3440 (νO–H); 1642 (νC=N); 1609, 1465 (νC=C); 1518,
1348 (νNO2); 1287 (νC–O); 949, 916 (νMo=O). UV–vis spec-
cm−1)]: 286 (5.86), 309 (−0.78), 360 (5.12). 1H NMR
(DMSO-d6, ppm) mer-isomer (65%): 8.68 (1H, s)
(azomethine); 8.22 (2H, d, J = 8.7 Hz), 7.70 (2H, d, J =
8.7 Hz), 7.12 (1H, d, J = 7.5 Hz), 7.06 (1H, d, J = 7.5
Hz), 6.89 (1H, t, J = 7.5 Hz) (aromatic); 5.23 (1H, t, J =
5.2 Hz) (hydroxyl); 5.41 (1H, d, 3J = 6.9 Hz), 3.89 (1H, m)
(methine); 4.02 (1H, ov), 3.61 (1H, dt, J = 12.4 Hz, J =
5.6 Hz) (methylene); 1.38 (9H, s) (tert-butyl); fac-isomer
(35%): 8.75 (1H, s) (azomethine); 8.25 (2H, d, J = 8.7
Hz), 7.62 (2H, d, J = 8.7 Hz), 7.14 (1H, d, J = 7.5 Hz),
3
3
3
3
−1
3
3
trum in DMSO [λmax (nm), ɛ (M cm−1)]: 275 (11400),
−1
339 (7620). CD spectrum in DMSO [λmax (nm), Δɛ (M
cm−1)]: 281 (3.78), 331 (3.30). H NMR (DMSO-d6, ppm)
1
3
4
mer-isomer (65%): 9.02 (1H, s) (azomethine); 8.69 (1H, t,
3J = 2.6 Hz), 8.28 (2H, d, 3J = 8.7 Hz), 7.77 (2H, d, 3J = 8.7
3
3
3
3
3
Hz), 7.61 (1H, t, J = 2.6 Hz), 7.14 (1H, d, J = 8.7 Hz)
3
3
3
(aromatic); 5.23 (1H, t, J = 5.2 Hz) (hydroxyl); 5.40 (1H,
7.08 (1H, d, J = 7.5 Hz), 6.91 (1H, t, J = 7.5 Hz) (aro-
matic); 5.92 (1H, d, 3J = 4.7 Hz) (hydroxyl); 4.12 (1H, dd,
d, 3J = 6.9 Hz), 3.87 (1H, m) (methine); 4.02 (1H, ov), 3.61
(1H, dt, 3J = 12.4 Hz, 4J = 5.6 Hz) (methylene); fac-isomer
(35%): 9.09 (1H, s) (azomethine); 8.72 (1H, t, 3J = 2.6 Hz),
3J = 9.1 Hz, J = 4.1 Hz), 4.02 (1H, ov) (methine); 4.86
4
3
4
(1H, dd, J = 9.3 Hz, J = 4.7 Hz), 3.99 (1H, ov) (methy-
lene); 1.40 (9H, s) (tert-butyl).
3
3
8.31 (2H, d, J = 8.7 Hz), 7.69 (2H, d, J = 8.7 Hz), 7.63
3
3
(1H, t, J = 2.6 Hz), 7.16 (1H, d, J = 8.7 Hz) (aromatic);
5.93 (1H, d, 3J = 4.7 Hz) (hydroxyl); 4.12 (1H, dd, 3J = 9.1
Hz, 4J = 4.1 Hz), 4.02 (1H, ov) (methine); 4.86 (1H, dd, 3J
= 9.3 Hz, 4J = 4.7 Hz), 3.99 (1H, ov) (methylene).
2.2.10 | MoO2L10
Yield 81%. Anal. calc for C20H16N2O7Mo: C, 48.8; H,
3.3; N, 5.7. Found: C, 48.7; H, 3.5; N, 5.8%. IR (KBr,
cm−1): 3329 (νO–H); 1621 (νC=N); 1606, 1456 (νC=C); 1517,
1339 (νNO2); 1251 (νC–O); 929, 898 (νMo=O). UV–vis spec-
2.2.8 | MoO2L8
−1
Yield 82%. Anal. calc for C16H14N2O8Mo: C, 41.9; H,
3.1; N, 6.1. Found: C, 41.8; H, 3.0; N, 6.2%. IR (KBr,
cm−1): 3414 (νO–H); 1631 (νC=N); 1608, 1491 (νC=C); 1522,
1350 (νNO2); 1232 (νC–O); 931, 902 (νMo=O). UV–vis spec-
trum in DMSO [λmax (nm), ɛ (M cm−1)]: 271 (11720),
302 (9740), 380 (2840). CD spectrum in DMSO [λmax
−1
1
(nm), Δɛ (M cm−1)]: 316 (−6.14), 383 (7.51). H NMR
(DMSO-d6, ppm) mer-isomer (65%): 9.53 (1H, s)
−1
3
3
trum in DMSO [λmax (nm), ɛ (M cm−1)]: 288 (11290),
(azomethine); 8.44 (1H, d, J = 8.5 Hz), 8.28 (2H, d, J =
−1
3
3
339 (3410). CD spectrum in DMSO [λmax (nm), Δɛ (M
8.7 Hz), 8.05 (1H, d, J = 8.8 Hz), 7.89 (1H, d, J = 8.0
Hz), 7.76 (2H, d, J = 8.7 Hz), 7.61 (1H, t, J = 7.3 Hz),
3
3
cm−1)]: 276 (−3.91), 347 (8.63). 1H NMR (DMSO-d6,
ppm) mer-isomer (65%): 10.24 (1H, s) (hydroxyl); 8.57
3
3
7.42 (1H, t, J = 7.3 Hz), 7.14 (1H, d, J = 8.9 Hz) (aro-
matic); 5.28 (1H, t, 3J = 5.2 Hz) (hydroxyl); 5.45 (1H, d, 3J
= 6.9 Hz), 3.92 (1H, m) (methine); 4.07 (1H, ov), 3.65
(1H, dt, J = 12.4 Hz, J = 5.6 Hz) (methylene); fac-
isomer (35%): 9.55 (1H, s) (azomethine); 8.46 (1H, d, 3J =
3
(1H, s) (azomethine); 8.24 (2H, d, J = 8.7 Hz), 7.72 (2H,
d, 3J = 8.7 Hz), 7.27 (1H, t, 3J = 7.4 Hz), 6.43 (1H, d, 3J =
3
3
4
8.2 Hz), 6.25 (1H, s) (aromatic); 5.27 (1H, t, J = 5.2 Hz)
(hydroxyl); 5.45 (1H, d, 3J = 6.9 Hz), 3.92 (1H, m)
3
4
3
3
(methine); 4.06 (1H, ov), 3.65 (1H, dt, J = 12.4 Hz, J =
8.5 Hz), 8.30 (2H, d, J = 8.7 Hz), 8.07 (1H, d, J = 8.8