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186 Chapter 7 7.4 Experimental data on chapter 5 All chemicals (Cu(NO3)2∙3H2O, Pd(OOCCH3)2, PdCl2, benzene-1,3,5-tricarboxylic acid (H3BTC), p-nitrophenol (PNP) (99%), Sodium borohydrate (NaBH4) (98%)) and all solvents (H2O, ethanol, and acetone) were used as commercially received unless otherwise noted. Before further manipulations, all activated samples were stored in an Ar-filled glove-box. 7.4.1 Synthesis of [Cu3-XPdx(BTC)2]n Cu/Pd-BTC_1-3 For Cu/Pd-BTC_1-3, 2.0 mmol of H3BTC (420 mg) was combined with 1.8 molar equivalents of a mixture of Cu(NO3)2∙3H2O and Pd acetate and then placed into a Teflon vessel. Subsequently 15ml of H2O/ethanol (1:1) solution was added. The molar percentage and amount of each metal salts in the total metal source as well as their weight used in the starting reactant are for Cu/Pd-BTC_1, Cu(NO3)2∙3H2O (90%, 3.24 mmol, 783 mg) / Pd acetate (10%, 0.36 mmol. 80.8 mg); for Cu/Pd-BTC_2, Cu(NO3)2∙3H2O (85%, 3.06 mmol, 739 mg) / Pd acetate (15%, 0.54 mmol. 121.2 mg); for Cu/Pd-BTC_3, Cu(NO3)2∙3H2O (80%, 2.88 mmol, 696 mg) / Pd acetate (20%, 0.72 mmol. 161.6 mg). The Teflon vessel was sealed in an autoclave and kept in the oven at 125 °C for 12h. The resulting power product was collected by filtration and washed several times with distilled water and acetone, respectively. After dried under ambient conditions the obtained powder was further activated by heating at 120 °C for 24 h under dynamic vacuum (ca. 10 -3 mbar).
Chapter 7 187 Figure 7.24. XPS survey scans of the activated samples Cu/Pd-BTC_1 and 3. Figure is provided by P. Guo. Figure 7.25. PXRD patterns of the sample obtained using 50% feeding of Pd(II)-acetate under the same conditions as [Cu 3-X Pd x (BTC) 2 ] n with 10%, 15% and 20% feeding .
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Controlled Modification of Metal-Or
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This thesis is based on the work pe
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Bochum) for the study of XPS and UH
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Zhang, for their continuous support
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II 3.2.1 Synthesis and characteriza
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IV 7.3.4 Synthesis of Cu-DEMOF samp
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VI DMSO dobdc e.g. EA EDX EtOH EXAF
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VIII TOF UHV UiO UMCM vs WCA XANES
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2 Chapter 1 limitations of the (non
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4 Chapter 2 For the synthesis of CP
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6 Chapter 2 cavities is able to rev
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8 Chapter 2 2.2.2 MOF features Adva
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10 Chapter 2 Figure 2.5. A series o
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12 Chapter 2 the material is retain
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14 Chapter 2 2.3 Synthetic approach
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16 Chapter 2 Expansion of this stru
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18 Chapter 2 (H2BPDC) [75] or other
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20 Chapter 2 Cr III CUSs of MIL-101
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22 Chapter 2 Figure 2.14. Schematic
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24 Chapter 2 adsorbate-surface inte
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3 Controlled secondary building uni
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28 Chapter 3 3.1 Preparation and in
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30 Chapter 3 formula of [Ru3 II,III
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Intensity, a. u. 32 Chapter 3 quali
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34 Chapter 3 After activating the R
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36 Chapter 3 presence of the residu
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Intensity, a. u. 38 Chapter 3 the a
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40 Chapter 3 extent than acetic aci
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42 Chapter 3 Ru-nodes. Therefore, r
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44 Chapter 3 decomposition of [BF4]
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deriv. normalized E) 46 Chapter 3 F
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48 Chapter 3 3.1.6 Summary Applying
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50 Chapter 3 3.2 Elaboration of Ru
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52 Chapter 3 with that of the Ru II
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54 Chapter 3 Figure 3.20. (a) XANES
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4 Linker-based MOF solid solutions:
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58 Chapter 4 4.1 Introduction 4.1.1
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60 Chapter 4 framework [Cu2(ndc)2(d
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62 Chapter 4 partial replacing of B
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64 Chapter 4 in the case of ip intr
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66 Chapter 4 4.2.1.1 Crystallinity
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68 Chapter 4 suggesting the absence
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70 Chapter 4 Table 4.1. The molar f
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72 Chapter 4 Figure 4.11. IR spectr
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74 Chapter 4 taking into account th
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76 Chapter 4 As quantitative digest
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78 Chapter 4 (Figure 4.16). Notably
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80 Chapter 4 framework Ru-species (
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82 Chapter 4 Figure 4.20. XANES spe
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84 Chapter 4 It is important to not
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86 Chapter 4 Ru δ+ have been obser
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88 Chapter 4 Figure 4.25. UHV-IR sp
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90 Chapter 4 Table 4.5. Possible de
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CO 2 adsorbed, mmol/g 92 Chapter 4
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H 2 adsorbed, mmol/g 94 Chapter 4 F
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CO 2 adsorbed, mmol/g 96 Chapter 4
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H 2 adsorbed, mmol/g 98 Chapter 4 8
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H 2 adsorbed, mmol/g 100 Chapter 4
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102 Chapter 4 presence of H2. [236]
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104 Chapter 4 reactive metal center
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106 Chapter 4 4.2.6 Conclusions App
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108 Chapter 4 4.3 Defects Engineeri
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Intensity, a. u. 110 Chapter 4 as-s
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weight loss, % 112 Chapter 4 100 Cu
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weight loss, % 114 Chapter 4 record
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116 Chapter 4 4.3.2 Composition and
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V, cm 3 /g 118 Chapter 4 500 400 30
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120 Chapter 4 Figure 4.50. From lef
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5 Simultaneous introduction of vari
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124 Chapter 5 preferred like Cu 2+
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126 Chapter 5 5.2 Preparation and S
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128 Chapter 5 Figure 5.5. Pawley Fi
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130 Chapter 5 5.3 Compositional cha
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132 Chapter 5 Table 5.3. The assign
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134 Chapter 5 framework are dominan
Page 154 and 155: 136 Chapter 5 5.4 Synthesis, compos
Page 156 and 157: 138 Chapter 5 obtained Pd-doped sol
Page 158 and 159: 140 Chapter 5 Figure 5.18. Deconvol
Page 160 and 161: V, cm 3 /g 142 Chapter 5 sorption i
Page 162 and 163: 144 Chapter 5 time as well as the i
Page 164 and 165: 146 Chapter 5 5.6 Conclusions In su
Page 166 and 167: 148 Chapter 6 coordinating anion),
Page 168 and 169: 7 Experimental Section In this Chap
Page 170 and 171: 152 Chapter 7 as water and hydroxyl
Page 172 and 173: 154 Chapter 7 internal standards an
Page 174 and 175: 156 Chapter 7 Uppermost layer is in
Page 176 and 177: 158 Chapter 7 to the more tightly b
Page 178 and 179: 160 Chapter 7 7.2 Experimental data
Page 180 and 181: 162 Chapter 7 [Ru2(OOCC(CH3)3)4(H2O
Page 182 and 183: 164 Chapter 7 Figure 7.7. The PXRD
Page 184 and 185: 166 Chapter 7 [Ru2(OOCCH3)4(H2O)2]B
Page 186 and 187: 168 Chapter 7 [Ru2(OOCCH3)4](THF)2
Page 188 and 189: 170 Chapter 7 [Ru3(BTC)2(OH)1.5]n·
Page 190 and 191: 172 Chapter 7 [Ru3(BTC)2]n∙(AcOH)
Page 192 and 193: 174 Chapter 7 Table 7.3. Feeding mo
Page 194 and 195: 176 Chapter 7 For comparison of the
Page 196 and 197: 178 Chapter 7 7.3.4 Synthesis of Cu
Page 198 and 199: 180 Chapter 7 D3 The mixture of H3B
Page 200 and 201: 182 Chapter 7 D5 This sample was re
Page 202 and 203: 184 Chapter 7 The synthesis of D7 a
Page 206 and 207: 188 Chapter 7 Figure 7.26. PXRD pat
Page 208 and 209: 190 Chapter 7 7.4.2 Hydrogenation o
Page 210 and 211: 192 Chapter 7 7.5 Supplementary det
Page 212 and 213: 8 Bibliography [1] A. J. Ihde, The
Page 214 and 215: 196 Bibliography [61] S. Ma, D. Sun
Page 216 and 217: 198 Bibliography [121] T. K. Prasad
Page 218 and 219: 200 Bibliography [180] Y. Kobayashi
Page 220 and 221: 202 Bibliography [239] A. L. Harreu
Page 222 and 223: 204 Bibliography [297] A. P. Hammer
Page 224 and 225: 206 Appendix List of Presentations
Page 226: 208 Appendix 05. 2015 Grant from th
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