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3.55 13 C NMR spectrum of polyanion 2 . . . . . . . . . . . . . . . . . . . . . . 131 3.56 31 P NMR spectrum of polyanion 3 . . . . . . . . . . . . . . . . . . . . . . 132 3.57 119 Sn NMR spectrum of polyanion 3 . . . . . . . . . . . . . . . . . . . . . 133 3.58 13 C NMR spectrum of polyanion 3 . . . . . . . . . . . . . . . . . . . . . . 134 3.59 1 H NMR spectrum of polyanion 3 . . . . . . . . . . . . . . . . . . . . . . 135 3.60 1 H NMR spectrum of polyanion 5 . . . . . . . . . . . . . . . . . . . . . . 136 3.61 13 C NMR spectrum of polyanion 5 . . . . . . . . . . . . . . . . . . . . . . 137 3.62 119 Sn NMR spectrum of polyanion 5 . . . . . . . . . . . . . . . . . . . . . 138 3.63 1 H NMR spectrum of polyanion 6 . . . . . . . . . . . . . . . . . . . . . . 138 3.64 13 C NMR spectrum of polyanion 6 . . . . . . . . . . . . . . . . . . . . . . 139 3.65 119 Sn NMR spectrum of polyanion 6 . . . . . . . . . . . . . . . . . . . . . 139 3.66 1 H NMR spectrum of polyanion 7 . . . . . . . . . . . . . . . . . . . . . . 140 3.67 13 C NMR spectrum of polyanion 7 . . . . . . . . . . . . . . . . . . . . . . 140 3.68 183 W NMR spectrum of polyanion 7 . . . . . . . . . . . . . . . . . . . . . 141 3.69 1 H NMR spectrum of polyanion 8 . . . . . . . . . . . . . . . . . . . . . . 141 3.70 13 C NMR spectrum of polyanion 8 . . . . . . . . . . . . . . . . . . . . . . 142 3.71 119 Sn NMR spectrum of polyanion 8 in presence of sodium chloride . . . . 142 3.72 FTIR spectra of compound K-18(red) and Na 9 [A-PW 9 O 34 ](blue) . . . . . 143 3.73 31 P NMR spectrum of polyanion 18 . . . . . . . . . . . . . . . . . . . . . 145 3.74 Size distribution by intensity of polyanion 18 . . . . . . . . . . . . . . . . 145 3.75 Size distribution by number of polyanion 18 . . . . . . . . . . . . . . . . . 146 3.76 Size distribution by volume of polyanion 18 . . . . . . . . . . . . . . . . . 146 3.77 Ball/stick and polyhedron representation of solid state of 18 showing 1-D chain . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146 3.78 FTIR spectra of compound K-19(red) and K 12 [H 2 P 2 W 12 O 48 ](blue) . . . . 147 3.79 Ball/stick and polyhedron representation of solid state of 19 showing 1-D chain . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149 3.80 FTIR spectra of compound K-20(red) and K 14 [P 2 W 19 O 69 (H 2 O)](blue) . . 150 3.81 Ball/stick and polyhedral representation of polyanion 20 . . . . . . . . . . 151 xvi
List of Tables 1.1 Selected M-M distances (in angstrom units) of corner- and edgesharing octahedra in POMs. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 1.2 List of common metal cations, M n+ , taking part in POM frameworks. We especially highlight W and Mo for being the most typical as addenda atoms 4 3.1 Crystal Data and Structure Refinement for compounds CsNa-1 and CsNa- 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 3.2 Crystal Data and Structure Refinement for compound KLi-3 . . . . . . . . 36 3.3 Reduction peak potentials measured from CVs and number (n 1 or n 2 ) of electrons corresponding to each wave of 3, [H 2 P 4 W 24 O 94 ] 22− and [H 7 P 8 W 48 O 184 ] 33− The scan rate was 10 mV s −1 , the working electrode was glassy carbon and the reference electrode was SCE . . . . . . . . . . . . . . . . . . . . . . . . 41 3.4 Crystal Data and Structure Refinement for compound CsNa-4 . . . . . . 45 3.5 Crystal Data and Structure Refinement for compound KNH4-5 . . . . . . 52 3.6 Crystal Data and Structure Refinement for compounds Cs-6 and Cs-7 . . 58 3.7 Crystal Data and Structure Refinement for compound NH4-8 . . . . . . . 72 3.8 Crystal Data and Structure Refinement for compound Cs-9 . . . . . . . . 85 3.9 Crystal Data and Structure Refinement for compound RbK-10 . . . . . . 90 3.10 Crystal Data and Structure Refinement for compound K-11 . . . . . . . . 93 3.11 Crystal Data and Structure Refinement for compound CsKNa-12 . . . . . 101 3.12 Crystal Data and Structure Refinement for compounds NH4-14, NH4Na- 15, RbNa-16 and KNa-17 . . . . . . . . . . . . . . . . . . . . . . . . . . 113 3.13 Selected bond lengths and angles in polyanions 14 and 15 . . . . . . . . . 115 3.14 Selected bond lengths and angles in polyanions 16 and 17 . . . . . . . . . 119 3.15 Crystal Data and Structure Refinement for compound K-18 . . . . . . . . 144 3.16 Crystal Data and Structure Refinement for compound K-19 . . . . . . . . 148 3.17 Crystal Data and Structure Refinement for compound K-20 . . . . . . . . 150 xvii
Page 1 and 2: Hybrid Organic-Inorganic Polyoxomet
Page 3 and 4: Abstract Polyoxometalates (POMs) ar
Page 5 and 6: the cubic system (space group I m¯
Page 7 and 8: AsW 9 O 32 OH) 2 ]·36H 2 O (RbNa-1
Page 9 and 10: Paris-Sud, Orsay Cedex, France) for
Page 11 and 12: 2.2.9 Synthesis of K 12 [H 2 P 2 W
Page 13 and 14: Bibliography . . . . . . . . . . .
Page 15 and 16: 3.5 Left: combined polyhedral and b
Page 17: 3.33 Combined polyhedron and ball/s
Page 21 and 22: MO 6 octahedra surrounding a centra
Page 23 and 24: 1.1.1 The clathrate-like structure
Page 25 and 26: 7(MoO 4 ) 2− + 8H + → [Mo 7 O 2
Page 27 and 28: Fig. 1.4: Combined polyhedral/ball
Page 29 and 30: This planar structure was originall
Page 31 and 32: [X 2 M 18 O 62 ] 6− , the D 3h We
Page 33 and 34: [P 2 W 19 O 68 (HO)] 14− , [P 2 W
Page 35 and 36: Fig. 1.11: Monomeric (left) and dim
Page 37 and 38: Chapter 2 Experimental 2.0.1 Reagen
Page 39 and 40: 2.2 Preparation of starting materia
Page 41 and 42: as Cs 6 [P 2 W 5 O 23 ]·7H 2 O by
Page 43 and 44: was adjusted between 5-6 by additio
Page 45 and 46: Chapter 3 Results 3.1 The hybrid or
Page 47 and 48: Fig. 3.2: FTIR spectra of compound
Page 49 and 50: Fig. 3.3: W 183 NMR spectra of (CsN
Page 51 and 52: Fig. 3.5: Left: combined polyhedral
Page 53 and 54: formed upon crystallization and bot
Page 55 and 56: X-ray Crystallography A crystal of
Page 57 and 58: the presence of the four (CH 3 ) 2
Page 59 and 60: Fig. 3.10: Cyclic voltammogram of 2
Page 61 and 62: as a function of electrolyte compos
Page 63 and 64: was observed that could be traced t
Page 65 and 66: electrochemical set-up was an EG &
Page 67 and 68: Fig. 3.14: The central core of Sn(C
Page 69 and 70:
of these fragments [88, 90]. For co
Page 71 and 72:
diffractometer using Mo K α radiat
Page 73 and 74:
Fig. 3.18: Side view of [{Sn(CH 3 )
Page 75 and 76:
host−guest systems with large cav
Page 77 and 78:
X-ray Crystallography Single crysta
Page 79 and 80:
3.5.2 Results and discussions Polya
Page 81 and 82:
Fig. 3.26: Ball and stick represent
Page 83 and 84:
can distinguish between different m
Page 85 and 86:
Fig. 3.28: STM pictures of {Sn(CH 3
Page 87 and 88:
Fig. 3.31: Size distribution by int
Page 89 and 90:
3.6 The bis-phenyltin substituted,
Page 91 and 92:
Table 3.7: Crystal Data and Structu
Page 93 and 94:
tral belt in-between the two tin at
Page 95 and 96:
Fig. 3.35: 183 W NMR spectra of com
Page 97 and 98:
whereas they are five-coordinated (
Page 99 and 100:
investigated by scanning tunneling
Page 101 and 102:
3.8 The di-titanium substituted, lo
Page 103 and 104:
Fig. 3.37: Ball/stick (left), polyh
Page 105 and 106:
[As 2 W 19 O 67 (H 2 O)] 14− , [A
Page 107 and 108:
3.9 The cyclic trimeric-titanium su
Page 109 and 110:
Table 3.9: Crystal Data and Structu
Page 111 and 112:
Fig. 3.40: FTIR spectra of compound
Page 113 and 114:
Fig. 3.42: Side-view of compound 11
Page 115 and 116:
11 by 183 W-NMR (at 16.66 MHz on a
Page 117 and 118:
3.11 Structure and solution propert
Page 119 and 120:
472(w), 444(w) cm −1 . This proce
Page 121 and 122:
MHz in 10 mm tubes and the 111 Cd N
Page 123 and 124:
Fig. 3.47: 111 Cd NMR spectra of [C
Page 125 and 126:
in aqueous solution, so that the nu
Page 127 and 128:
of cadmium ions in 12 and 13 and it
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doubtedly 183 W-NMR, but the parama
Page 131 and 132:
K): (relative intensities in parent
Page 133 and 134:
Fig. 3.49: Combined polyhedral/ball
Page 135 and 136:
Fig. 3.50: 183 W NMR spectrum of [I
Page 137 and 138:
(17) are isostructural. They consis
Page 139 and 140:
Fig. 3.53: 183 W NMR spectrum of [I
Page 141 and 142:
3.12.4 Conclusion We have synthesiz
Page 143 and 144:
[37] D. Gatteschi, O. Kahn, J. Mill
Page 145 and 146:
94:226403, 2005. [123] R. J. Hamers
Page 147 and 148:
[206] I. Loose, E. Droste, M. Bösi
Page 149 and 150:
NMR Spectra Fig. 3.54: 13 C NMR spe
Page 151 and 152:
Fig. 3.56: 31 P NMR spectrum of pol
Page 153 and 154:
Fig. 3.58: 13 C NMR spectrum of pol
Page 155 and 156:
Fig. 3.60: 1 H NMR spectrum of poly
Page 157 and 158:
Fig. 3.62: 119 Sn NMR spectrum of p
Page 159 and 160:
Fig. 3.66: 1 H NMR spectrum of poly
Page 161 and 162:
Fig. 3.70: 13 C NMR spectrum of pol
Page 163 and 164:
were applied and an absorption corr
Page 165 and 166:
Fig. 3.75: Size distribution by num
Page 167 and 168:
Table 3.16: Crystal Data and Struct
Page 169 and 170:
Fig. 3.80: FTIR spectra of compound
Page 171 and 172:
FIRASAT HUSSAIN International Unive
Page 173 and 174:
Publications 1. Observation of a Ha
Page 175 and 176:
PAPERS IN CONFERENCE/ SYMPOSIA / WO
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