Self-assembled Transition Metal Coordination Frameworks of ...

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1.6.4. IR spectra _ __g W ___ M Introduction Infrared spectra of organic ligands and their metal complexes in the range 4000-400 cm'1 were recorded on a Thermo Nicolet, Avatar 370 .DTGS model FT-IR spectrophotometer with KBr pellets and ATR technique at SAIF, Kochi. The far IR spectra of metal complexes were recorded using polyethylene pellets in the 500-100 cm" region on a Nicolet Magna 550 FTIR instrument at the Sophisticated Analytical Instrumentation Facility, Indian Institute of Technology, Bombay, India. 1.6.5. Single crystal X-ray crystallography The technique of single crystal X-ray crystallography is used to determine the arrangement of atoms within a crystal, which provides positions of atoms very precisely. This has led to a better understanding of chemical bonds and non-covalent interactions. The first atomic-resolution structure to be solved (in 1913) was that of table salt [88], which proved the existence of ionic compounds and that crystals are not necessarily comprised of molecules. X-Ray crystallography had a pioneering role in the development of supramolecular chemistry, particularly in clarifying the structures of the crown ethers and the principles of host-guest chemistry. As of 1“ January 2007 the Cambridge Structural Database (C SD), the principal product of the Cambridge Crystallographic Data Centre (CCDC) contains 400977 structures [89]. The crystallographic data of present work were collected at (i) the X-ray Crystallography Unit, School of Physics, Universiti Sains Malaysia, Penang, Malaysia, (ii) the Analytical Sciences Division, Central Salt and Marine Chemicals Research Institute, Bhavnagar, Gujarat, India, (iii) the Department of Inorganic and Physical Chemistry, Indian Institute of Science, Bangalore, India and (iv) the National Single Crystal X-ray Diffraction Facility, Indian Institute of Technology, Bombay, India. 23
Chapter I W__‘ _ 1.6.6. MALDI MS spectrometry MALDI (matrix-assisted laser desorption/ionization), a laser based soft ionization method, developed in the late 1980s, has proven to be one of the most successful ionization methods for mass spectrometric analysis and investigation of large molecules. The most important applications of MALDI mass spectrometry are (in decreasing order of importance): peptides and proteins, synthetic polymers, oligonucleotidcs, oligosaccharides, lipids, inorganics. Compared to the large number of applications for organic (especially bioorganic) compounds the use of the matrix assisted laser ionization method for the analysis of inorganic compounds is relatively rare [90]. Nevertheless there is a good chance to get useful MALDI mass spectra from many inorganic compounds with the appropriate choice of the matrix. However, with metal complexes the matrix may occupy a coordination site and additional peaks are expected. Also the acidic nature of many matrices is destructive to proton sensitive compounds. In the present study, High-resolution MAL-DI spectra were measured by the MS-service, Laboratorium fur Organische Chemie, ETH Zurich, Switzerland on an IonSpec HiResMALDI apparatus in a DCTB {T-2-[3-(4-t-butyl-phenyl)-2—methyl-2 propenylidene]malononitrile} matrix and dichloromethane solvent. All spectra were taken in positive ion mode. Simulation of isotropic distribution patterns were carried out using a free demo version of ChemSW Mass Spec Calculator. 1. 6. 7. EPR spectroscopy Electron Paramagnetic Resonance {EPR) phenomenon was discovered by Zavoisky in 1944 and in the beginning it was used by physicists to study the paramagnetic metal ions in crystal lattices. lt is based on the absorption of electromagnetic radiation, usually in the microwave region, which causes transitions between energy levels produced by the action of a magnetic field on an unpaired electron. For example, in the case of a Cu(ll) ion, it has an effective spin of S I % and 24
Page 1 and 2: 7,2/H5 Self-assembled Transition Me
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Page 7 and 8: PREFACE In its method, chemistry is
Page 9 and 10: CONTENTS CHAPTER 1 Introduction to
Page 11 and 12: 4.3.5. Magnetochemistry 4.3.6. Char
Page 13 and 14: Chapter I__ _ _ irreducible, is a n
Page 15 and 16: Chapter I W 7 _ W _ 7 pg _ jg to pr
Page 17 and 18: Chapter I H_ g g 7 g 7 7 __ harvest
Page 19 and 20: Chapter I _ _ ______g__H _ g involv
Page 21 and 22: Chapter I _ g plays a pivotal role
Page 23 and 24: Chapter I g g _ exhibit considerabl
Page 25 and 26: Chapter I _, assemblies to generate
Page 27 and 28: Chapter I _ ,_ of mono or dinuclear
Page 29 and 30: Chapter I M W 7 7 _ __ 1.3.1.1. Ant
Page 31 and 32: Chapter I _ _ _ _ \_ 4- Jm _. _.
Page 33: Chapter In g_ g _ E __ _ E __( > es
Page 37 and 38: Chapter I ,,_ g electron spin (the
Page 39 and 40: Chapter I W _ _ Traditional magnets
Page 41 and 42: Chapter I L.K. Thompson, O. Waldman
Page 43 and 44: Chapter I i __ _ Org. Chem. 31 (200
Page 45 and 46: Chapter In _g , g H g 85. S. Padhye
Page 47 and 48: Chapter 2 1 g anticipation of Cu(H)
Page 49 and 50: Chapter 2 _. M_ _ up 1. Quinoline-2
Page 51 and 52: Chapter 2 chloroform solution and d
Page 53 and 54: Chapter2 V _ _ _ _, 7 _ with aceton
Page 55: Chapter 2 _ 7 f __ i 2.3. Results a
Page 58 and 59: 100s0- I > J 20
Page 60 and 61: — — 1 Ligands 1
Page 62 and 63: Ligands The ‘H and "C NMR spectra
Page 64 and 65: Ligands The ‘H NMR spectrum of HZ
Page 66 and 67: M1 1‘ 11 IL; Fig. 2.11. 'H NMR sp
Page 68 and 69: ' | Ligands uo no 1&0 150 no no no
Page 70 and 71: Ligands Table 2. 3. Crystal data an
Page 72 and 73: Ligands The C-S bond distances of 1
Page 74 and 75: ligands between the planes of Cg(2)
Page 76 and 77: " F Ligands A indicates a typical d
Page 78 and 79: ' ' Q 0' ¢ ¢" .~ 0~ I Q Q Q \ ' Q
Page 80 and 81: 2.4.2. M TT Cell Proliferation Assa
Page 82 and 83: Table 2.9. Cell proliferation effec
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7 y _ i _ W Ligands B. Moubaraki, K
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CHAPTER Ni(II) complexes of carbohy
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_ _ __ g_ g W g H__ Ni(ll) complexe
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_ g A __ Ni(lI) complexes The reddi
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3.3. Results and discussion g_g _ N
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3.3.1. MALDI MS spectral studies of
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Ni(Il) complexes In the case of com
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100 U-
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3.3.2. IR and electronic spectral s
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Chapter 3 The electronic spectra of
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t§hqphw*3 v(Ni—S), further suppo
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Chapter 3 charge transfer bands. Fo
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Chapter 3 were refined anisotropica
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Chapter 3 3.3.3.1. Crystal structur
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Chapter 3 Table 3.7. Selected bond
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Chapter 3 N(l3)—C(35), N(2l)-C(58
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3.3.3.2. Crystal structures 0f[Ni(H
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Table 3.10. Selected bond lengths (
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Ni(lI) complexes significant 1t---1
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3.3.4. Magnetochemistry of the mole
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Ni(Il) complexes The allowed values
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in xn In
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g 7 Ni(Il) complexes 3.4. Concludin
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11 12 13 14 15 16 17 18 19 20 21 22
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41 42 43 44 45 46 47 48 49 50 51 52
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_ g “FOUR CHAPTER Cu(II) complexe
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_g C0pper(II) complexes complex of
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_ _ , p f 7, Copper-(II) complexes
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pp g _g _4_,_ C0pper(II) complexes
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g _,_,_ g g Copperfll) complexes in
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i ____ 3+ i --—- C 0pper(H) 2+ co
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C0pper(Il) complexes 499 100i ~04 7
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.04Copper(II) complexes 385 50.1I 1
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100-I 4 -1 U ” Q 7°-J 59-: "1
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C0pper(lI) complexes confirm the po
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C0pper(ll) complexes 100 80" I
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C0pper(1l) complexes state, similar
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2 5 2.5MW 20 Q 1.51 2oo'aoo'45o's
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Copper(lI) complexes F1 = g",3B:S:
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Chapter 4 for both species consider
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Chapter 4 The spectrum of compound
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Chapter 4 stability alone could not
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Chapter 4 zénzénzénzénénaloeé
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Chapter 4 164 | | | 252 272 2Q 31 B
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Chapter 4 The shifting of g values
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Chapter 4 _|“. / "| 1' '| |' | 1'
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Chapter 4 The solid state and some
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Chapter 4 U 1 .I - O i I . I II I
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_ I Chapter 4 — I I I — I '
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. , Chapter 4 2.5 I I ' I ' I ' I '
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Chapter 4 The field dependence of m
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Chapter 4 Where ,1’ M is the magn
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Chapter 4 g e The powder and frozen
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Chapter 4 various aspects like bond
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C0pper(ll) complexes Table 4.6. Sel
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,____ p _p C0pper(H) complexes from
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Ed. Engl. 31 (1992) 733. 7___7 7 7
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__ ,_ f W C 0pper(l1) complexes Che
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-_ FIVE CHAPTER Spectral and magnet
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__ g_ _g g H g __ Manganese(II) com
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q H _ Manganesefll) complexes [Mn2(
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Manganese(Il) complexes lcmzmoll in
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1W3 "l U 70 60 40 30 10 490 740 979
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Manganese(II) complexes MALDI MS sp
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5.3.2. EPR spectral studies Mangane
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Manganese(II) complexes D and E , e
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the pattern is uncertain and it is
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__ I . l r Manganese(II) complexes
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" |\ Man ganese(II) complexes 80" 6
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Chapter 5 thiocarbohydrazone comple
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Chapter 5 To fit and interpret the
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Chapter 5 #1 IT 0.00 1 — ‘ I '
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Chapter 5 The temperature dependenc
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Chapter 5 ___ M _ 357 (2004) 2694.
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Chapter5 p _ _ S. Sivakumar, Struct
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Chapter 6 _ _ __ 7 the latter have
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Chapter6A, 0 0 _, 0 0 _* 4, W 0 0 0
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Chapter 6 g _ _ [Cd(HL2) ].,(1v0_.)
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Chapter 6 / ‘~ ' if‘ . l \ N N/
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1 | Chapter 6 100m__ ‘ 76$ mi, 16
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3 - i El Q I Chapter 6 - '3“ 1999
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Chapter 6 The compound 27 exhibits
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(T71aq7tew'¢5 centered at 1711.9 c
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1 . 1 Chapter 6 1244 100--1-; 1245
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Chapter 6 6.3.2. Electronic and IR
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Chapter 6 band at 19160 and 23920 c
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Zinc(II) & Cadmium(II) complexes Th
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.- 60- I ‘J TZinc(Il) & Cadmium(l
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Zinc(Il) & Cadmium(Il) complexes re
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Zinc(II) & C admium(ll) complexes T
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Fig. 6.25. The molecular structure
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Zinc(lI) & Cadmium(ll) complexes Al
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Zi!lC(II) & Cadmlum(II) C0mlexes Ta
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V _ i Zinc(1I) & Cadmium(lI) comple
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_ g _ g g V Zinc(lI) & Cadmiumfll)
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_, _ g pg L Summary and conclusion
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W g _ g mm Summary and conclusion a
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__ ,_ _ W A _ _ Summary and conclus
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Curriculum Vitae PERSONAL PROFILE N
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2-Hydroxyacetophenone 4-phenylthios
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