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Table (1); Elemental analysis of Zr(IV) and Hf (IV) Complex of

N(4)–alkyl, N(4)–dialkyl and 3-azacyclothiosemicarbazones


Found (calc.) %

No No Complex C H M H2O(a)
1 Zr8(DA4-M)2(OH)32.26H2O 10(10.7) 4.4(4.9) 33.2(32.4) 20.3 (20.8)
2 Hf8(DA4-M)2(OH)32.24H2O 7. 4(8.2) 2.8(3.6) 49.8(49.0) 13.9(14.8)
3 Zr8(DA3-Pip)2(OH)32.26H2O 13.8(14.1) 4.2(4.7) - -
4 Hf8(DA3-Pip)2(OH)32.26H2O 12. 5(13.2) 3.8(4.4) - -
5 Zr8(DA3-hexim)2(OH)3236H2O 13.3(14.0) (4.8)5.6 - -
6 Hf8(DA3-hexim)2(OH)3236H2O 10.3(11.0) (3.8)4.4 44.9(43.8) -
7 Zr8(DA4-Et)2(OH)32.36H2O 19.9(10.7) 4.9(5.5) - -
8 Hf(DA4-Et)2(OH)32.36.H2O 17.9(8.4) 3.9(4.2) - -
9 Zr8(DA4-DEt)2(OH)32..36H2O 11.8(12.4) 4.8(5.6) - -
10 Hf8(DA4-DEt)2(OH)32.36.H2O 8.9(9.7) 4.1(4.4) - -
11 Zr8(DA4-Ph)2(OH)32.36H2O 13.7(14.1) 4.6(5.2) - -
12 Hf8(DA4-Ph)2(OH)32.36H2O 10.4(11.1) 3.6(4.1) - -

* a = Water of hydration
Table2: Infrared Spectral bands for
dehydroacetic acid N(4)-alkyl,N(4)-dialkyl and
3-azacyclothiosemicarbazones and their Zr(IV) and Hf(IV) Complexes.
No Compowd γ(H2O) γ (C=O) γ (C=N) γ (CS) γ (M-O) γ (M-N)
1 DA4-M - 1680,1650 1565 858
3415 1630, 1540(sh) 847
3412 1630 1540(sh) 847
2 DA3-Pip - 1680,1650 1583 883
3418 1625,- 1563 847
3417 1625 1566 849
1682, 1580 868
3 DA3-Hexim
1670(sh)
3405 1627 1561 849
3402 1630 1564 847
- 1717, 1570 850
4 DA4-Et
3405 1651
1627 1560 845
3412 1630 1555 845
- 1684 1583 855
5 DA4-DEt
3420 1658
1626 1563 846
3409 1605 1564 847
6 DA4-Ph 1716, 1600 851
1652
3418 1600 1562 846
3403 1635 1563 884