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Self-assembled Transition Metal Coordination Frameworks of ...

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Chapter6A, 0 0 _, 0 0 _* 4, W 0 0 0<br />

g (47%). Elemental Anal. Found (Calc.): C, 44.92 (44.77); H, 3.10 (3.16); N, 12.67<br />

(12.53); S, 5.05 (4.78)%.<br />

[Z~(HL2)1.(BF.).~ #140 (25)<br />

2<br />

To a hot solution <strong>of</strong> H2L (0.220 g, 0.5 mmol) in 10 ml chlor<strong>of</strong>orm was added<br />

an equimolar amount <strong>of</strong> Zn(BF4)2~ 2H20 (0.120 g) dissolved in 10 ml hot methanol.<br />

The yellow colored solution was then refluxed for 2 h and allowed to stand at room<br />

temperature for slow evaporation. The yellow solid mass precipitated alter<br />

evaporation was washed with methanol and ether and dried in vacuo over P4010.<br />

Yield: 0.146 g (47%). Elemental Anal. Found (Calc.): C, 48.59 (48.49); H, 3.88<br />

(3.66); N, 13.77 (13.57); S, 5.40 (5.l8)%.<br />

[Zn(H2L3)Br;]2- 61140 (26)<br />

A solution <strong>of</strong> ZnBr2 (0.229 g, 1 mmol) in 10 ml <strong>of</strong> methanol was added to a<br />

solution <strong>of</strong> HZL3 (0.398 g, 1 mmol) in 50 ml boiling methanol and refluxed for 1 h and<br />

allowed to stand at room temperature. Orange yellow powder separated out was<br />

filtered, washed with methanol followed by ether and dried over P4010 in vacuo.<br />

Yield: 0.411 g (62%). Elemental Anal. Found (Calc.): C, 38.10 (38.00); H, 2.83<br />

(3.34); N, 12.69 (12.66); S, 4.92 (4.83)%.<br />

[Zn (HL3)]4(BF4)4' ZCH, 011- 211140 (2 7)<br />

To a hot solution <strong>of</strong> HZL3 (0.298 g, 0.75 mmol) in 50 ml methanol was added<br />

an equimolar amount <strong>of</strong> Zn(BF4);' 21120 (0.180 g) dissolved in 10 ml hot methanol.<br />

The orange colored solution was then stirred for 3 h and allowed to stand at room<br />

temperature for slow evaporation. The orange powder precipitated after evaporation<br />

was washed with methanol and ether and dried in vacuo over P4010. Yield: 0.326 g<br />

(77%). Elemental Anal. Found (Calc.): C, 46.18 (46.06); H, 3.72 (3.24); N, 15.35<br />

(14.99); S, 5.93 (5.72)%.<br />

232

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