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Synthesis and Structural Characterization of ... - Jacobs University

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Amal H. Ismail<br />

Ph.D. Thesis<br />

1.6.1 Photocatalysis .............................................................................................................. 22<br />

1.6.2 Acid catalysis .............................................................................................................. 24<br />

1.6.3 Oxidation catalysis ...................................................................................................... 25<br />

1.7 Lanthanide-containing polyoxotungstates .......................................................................... 26<br />

1.7.1 Lanthanide-containing isopolyoxotungstates .............................................................. 26<br />

1.7.2 Lanthanide-containing heteropolytungstates ............................................................... 29<br />

1.7.3 Mixed lanthanide / d-transition metal ions containing POMs ..................................... 33<br />

1.8 References .......................................................................................................................... 35<br />

Chapter II<br />

Experimental ........................................................................................................................... 41<br />

2.1 Reagents ............................................................................................................................. 41<br />

2.2 Instrumentation ................................................................................................................... 42<br />

2.2.1 Fourier transform infrared spectroscopy ..................................................................... 42<br />

2.2.2 Single crystal X-ray diffraction ................................................................................... 42<br />

2.2.3 Thermogravimetry ....................................................................................................... 43<br />

2.2.4 Multinuclear magnetic resonance spectroscopy .......................................................... 43<br />

2.3 Preparation <strong>of</strong> starting materials ........................................................................................ 43<br />

2.3.1 <strong>Synthesis</strong> <strong>of</strong> K 14 [As 2 W 19 O 67 (H 2 O)] ............................................................................ 43<br />

2.3.2 <strong>Synthesis</strong> <strong>of</strong> Na 9 [B-α-AsW 9 O 33 ]·27H 2 O ..................................................................... 44<br />

2.3.3 <strong>Synthesis</strong> <strong>of</strong> Na 9 [B-α-SbW 9 O 33 ]·27H 2 O ..................................................................... 44<br />

2.3.4 <strong>Synthesis</strong> <strong>of</strong> Na 12 [Sb 2 W 22 O 74 (OH) 2 ]........................................................................... 44<br />

2.3.5 <strong>Synthesis</strong> <strong>of</strong> K 8 [β 2 -GeW 11 O 39 ]·14H 2 O........................................................................ 44<br />

2.3.6 <strong>Synthesis</strong> <strong>of</strong> K 8 [γ-GeW 10 O 36 ]·6H 2 O ........................................................................... 45<br />

2.3.7 <strong>Synthesis</strong> <strong>of</strong> K 8 Na 2 [A--GeW 9 O 34 ]·25H 2 O ................................................................ 45<br />

2.3.8 <strong>Synthesis</strong> <strong>of</strong> Na 10 [A--GeW 9 O 34 ]·4H 2 O ..................................................................... 46<br />

2.3.9 <strong>Synthesis</strong> <strong>of</strong> K 8 [BW 11 O 39 H]·13H 2 O ........................................................................... 46<br />

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