Chapter 4 - Jacobs University

2.1.2 Single crystal X-ray diffraction……………………………………………………49
2.1.3 Multinuclear magnetic resonance spectroscopy…………………………………...50
2.1.5 Elemental and thermogravimetric analyses………………………………………..50
2.2 Preparation of starting materials……………………………………………………………..51
2.2.1 Synthesis of Na 9 [AsW 9 O 33 ]·27H 2 O……………………………………………….51
2.2.2 Synthesis of Na 9 [SbW 9 O 33 ]·27H 2 O.........................................................................51
2.2.3 Synthesis of K 14 [As 2 W 19 O 67 (H 2 O)]..........................................................................52
2.2.4 Synthesis of A & B Na 8 [HAsW 9 O 34 ]·11H 2 O (A & B-Type AsW 9 O 34 )...................52
2.2.5 Synthesis of A-Na 9 [PW 9 O 34 ]·7H 2 O..........................................................................53
2.2.6 Synthesis of K 7 [PW 11 O 39 ]·12H 2 O.............................................................................53
2.2.7 Synthesis of K 14 [P 2 W 19 O 69 (OH 2 )]·24H 2 O................................................................54
2.2.8 Synthesis of K 8 [a-SiW 11 O 39 ]·13H 2 O........................................................................54
2.2.9 Synthesis of K 8-x Na x [GeW 11 O 39 ]………………………………………………..…55
2.2.10 Synthesis of K 12 [H 2 P 2 W 12 O 48 ]·24H 2 O……………………………………………55
2.2.11 Synthesis of K 16 Li 2 [H 6 P 4 W 24 O 94 ]·33H 2 O...............................................................56
2.2.12 Synthesis of K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O………………………………………..56
2.2.13 Synthesis of K 8 [b 2 -SiW 11 O 39 ]·14H 2 O………………………………...…………..56
2.2.14 Synthesis of K 8 [g-SiW 10 O 36 ]·20H 2 O……………………………………..……….57
2.3References…………………………………………………………………………….………58
Chapter 3: The Wheel-Shaped Cu 20 Tungstophosphate
[Cu 20 Cl(OH) 24 (H 2 O) 12 (P 8 W 48 O 184 )] 25- 59
3.1 Introduction…………………………………………………………………………………..59
3.2 Synthesis……………………………………………………………………………………..61
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