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A. MARGARITI ET AL.
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.65 g (ꢂ50%, based on oxalylchloride). H-NMR (300 MHz, DMSO-d , d, ppm): 12.80 (s,
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H), 8.70 (d, 1H), 8.08 (d, 1H), 7.71 (t, 1H), 7.29 (t, 1H). IR (KBr pellets, cm ): 3268 m,
975 br, 2677 w, 2493 w, 1700 s, 1676 s, 1603 s, 1581 s, 1510 s, 1467 m, 1456 m, 1406 s,
322 m, 1298 m, 1269 s, 1171 m, 1147 m, 1091 m, 1054 w, 1041 w, 961 w, 905 m, 875
w, 864 w, 832 m, 775 m, 753 s, 698 m, 660 m, 561 sh, 545 m, 488 m.
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.2.2. Synthesis of [Mg(H L)(H O) ] (1)
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2 n
An aqueous solution (10 mL) of MgCl ꢀ6H O (43 mg, 0.2 mmol) was added to a 10 mL
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DMF solution of H L (33 g, 0.1 mmol) resulting in a white turbid suspension. The slurry
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was then sealed in a glass vial and heated in an isotemp oven at 100 C for 2 days
and colorless well-shaped, needle-like single crystals were formed and collected by
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vacuum filtration. Yield: 70%. IR (KBr pellet, cm ): 3457 s, 3385 sh, 3161 w, 3130 sh,
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686 s, 1611 m, 1584 s, 1506 s, 1456 m, 1442 s, 1393 s, 1299 m, 1220 m, 1170 w, 1150 w,
092 w, 1048 w, 874 w, 851 sh, 844 m, 818 w, 766 m, 717 w, 704 w, 664 m, 617 br w,
41 m, 529 sh, 492 w.
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.2.3. Synthesis of [Mn(H L)(H O) ] (2)
2 2 2 n
An aqueous solution (10 mL) of MnCl ꢀ4H O (40 mg, 0.2 mmol) was added to a 10 mL
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DMF solution of H L (33 mg, 0.1 mmol) producing a white turbid suspension. The sus-
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pension was sealed in a glass vial and heated in an isotemp oven at 85 C for 1 day.
Pale yellow needle-like single crystals were formed and collected by vacuum filtration.
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Yield: 84%. IR (KBr pellet, cm ): 3445 s, 3111 br w, 1686 s, 1607 w, 1583 s, 1564 br w,
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501 s, 1454 w, 1437 s, 1384 s, 1297 m, 1220 m, 1170 m, 1148 w, 1047 w, 874 w, 848 m,
66 m, 717 sh, 702 w, 664 m, 597 br w, 539 m, 529 sh, 492 w.
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.2.4. Synthesis of [Co(H L)(H O) ] (3)
2 2 2 n
A pink clear aqueous solution (10 mL) of Co(NO ) ꢀ6H O (59 mg, 0.2 mmol) was added
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to a 10 mL DMF solution of H L (33 mg, 0.1 mmol) producing a pink-whitish turbid sus-
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pension. The suspension was sealed in a glass vial and heated in an isotemp oven at
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5 C for 3 days. Pink needle-like single crystals were formed and collected by vacuum
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filtration. Yield: 83%. IR (KBr pellet, cm ): 3447 s, 3361 sh, 3148 w, 3130 sh, 1685 s,
1606 m, 1582 s, 1560 m, 1501 s, 1455 m, 1438 s, 1384 s, 1298 m, 1221 m, 1171 w, 1150
w, 1092 w, 1047 w, 874 w, 851 sh, 842 m, 818 w, 766 m, 717 w, 705 w, 666 m, 617 br
w, 540 m, 516 sh, 490 w.
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.2.5. Synthesis of [Ni(H L)(H O) ] (4)
2 2 2 n
An aqueous solution (20 mL) of Ni(NO ) ꢀ6H O (66 mg, 0.2 mmol) was added to a
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0 mL DMF solution of H L (33 mg, 0.1 mmol) producing a green-whitish turbid sus-
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pension. The suspension was sealed in a glass vial and heated in an isotemp oven at
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5 C for 3 days. Green needle-like single crystals were formed and collected by vac-
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uum filtration. Yield: 60%. IR (KBr pellet, cm ): 3434 s, 3316 w, 3153 w, 1701 w,
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684 s, 1606 m, 1583 s, 1559 m, 1501 s, 1455 w, 1438 s, 1383 s, 1309 sh, 1298 m, 1221 m,
171 m, 1148 w, 1091 w, 1047 w, 957 w, 874 w, 851 sh, 839 m, 814 w, 766 s, 706 w,
69 w, 665 w, 617 br w, 541 m, 534 m, 516 sh, 491 m.