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Self-assembled Transition Metal Coordination Frameworks of ...

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Zinc(Il) & Cadmium(Il) complexes<br />

refinement was carried out by full-matrix least squares on F2 (SHELXTL-97). H atoms<br />

were placed at calculated positions and allowed to ride on their parent atoms.<br />

The crystallographic data and structure refinement parameters <strong>of</strong><br />

[Zn(HL5)]4(BF4)4- 10H20 (29) are given in Table 6.3. The graphics tools used include<br />

ORTEP-III [39], PLATON [40], MERCURY [41] and DIAMOND version 3.0 [42].<br />

Table 6.3. Crystal data and structural refinement parameters <strong>of</strong> complex 29.<br />

Parameters [Zn(I-IL5)]4(BF4)4- 101120 (29)<br />

FO1Tl1Lll3 C|QQI‘I96B4F|6N24O|4Zfl4<br />

Formula weight (M) 2466.73<br />

Temperature (T) K 100.0(1) K<br />

Wavelength (Mo Ka) (A) 0.71073<br />

Crystal system Orthorhombic<br />

a b<br />

Z<br />

(A) 25.4580(l3) l5.4680(7)<br />

4<br />

c a (A) (°) 27.31 90.00 1o(14)<br />

,3 ;/(°) (°) 90.00<br />

Volume v (A3) 107s4.9(9)<br />

1»... cm (Mg or’) 1.523<br />

Space group P2(1)2( I )2( I )<br />

Lattice constants<br />

F(000) 5056<br />

Absorption coefficient;1(mm") 0.983<br />

Crystal size (mms) o.ss>< 0.39>< 0.28<br />

6 Range for data collection 1.09 to 30.l4°<br />

Limiting Indices -21 S h S 21,<br />

-35 S k S 35,<br />

-38 S I S 38<br />

Tm, and Tm," 0.759 and 0.638<br />

Reflections collected 124835<br />

Independent Reflections 31705 [R(int) = 0.0912]<br />

Refinement method Full-matrix least-squares on F2<br />

Data / restraints / parameters 31705 / 0/ 1463<br />

Goodness-<strong>of</strong>-fit on F2 1.074<br />

Final R indices [I > 20(1)] R] = 0.0575, wR2 = 0.1323<br />

R indices (all data) R, = 0.0962, wR; = 0.1556<br />

Largest difference peak and hole (e 13(3) 1.227 and -0.947<br />

257

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