1,2,3-Dithiazolyl and 1,2,35-Dithiadiazolyl Radicals as Spin-Bearing ...

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Compound Name: [μ-4-(2′-pyrimidyl)-1,2,3,5-dithiadiazolyl] di[bis(1,1,1,5,5,5- hexafluoroacetylacetonate) zinc(II)] : 4-(2′-pyrimidyl)-1,2,3,5-dithiadiazolyl bis(1,1,1,5,5,5-hexafluoroacetylacetonate) zinc(II)] 1:2 MW: 2467.7 g/mol Synthesis and Structure: Appearance: Dark blue needles Lit. and/or notebook # and page: DM07-57, p87 DM08-15, p18 First made on date: Nov 11, 2010 Made by: Dan J. MacDonald Experimental Data: A clear, colourless solution of Zn(hfac) 2·2THF (1.0294 g, 1.6504 mmol) in 20 mL of dry methylene chloride was added to a clear, dark purple solution of pymDTDA (0.1693g, 0.8186 mmol) in 30 mL of dry methylene chloride. The resulting darkened solution was stirred at room temperature for 30 minutes after which time the solvent was removed by flash distillation and the residue was sublimed at 120 °C to give dark blue needles of the title compound (37% yield based on 2:1 ratio of complexes). FTIR 3138w, 2961w, 2914w, 2851w, 1647s, 1586w, 1560m, 1532m, 1487s, 1463m, 1389m, 1348w, 1319w, 1259s, 1208s, 1150s, 1137s, 1097m, 861w, 841w, 813m, 796m, 763w, 743w, 716w, 669m, 647w, 586m, 526w. EA Calculated for [Zn 2 hfac 4·pymDTDA]:2[Znhfac 2·pymDTDA]: C, 26.770; H, 0.6944; N, 6.8113%. Found: C, 27.12; H, 0.89; N, 6.75%. 199
Crystallography: P2 1 /n a = 19.884, b = 8.8599, c = 23.216 α = 90.00, β = 100.73, γ = 90.00 volume: 4018.46 Z = 2 R-Factor = 5.09% 200
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1,2,3-Dithiazolyl and 1,2,35-Dithia
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an individual binuclear coordinatio
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weren’t sure about something our
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2.1 General........................
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5.3 Reverse oDTANQ.................
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LIST OF FIGURES AND SCHEMES Figure
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Figure 2-12. Magnetic susceptibilit
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GLOSSARY OF ABBREVIATIONS ° Degree
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K k k B LMCT ls LUMO Kelvin Exchang
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LIST OF STRUCTURES I-1 I-2 I-3 I-4
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I-16a I-16b I-16c I-16d I-16e I-16f
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I-22 I-23 I-24 I-25 exo I-26 endo x
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I-34 I-35 II-3 II-4 II-1 xxv
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III-2 III-1 III-3 III-4 III-5 III-6
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V-7 V-8 V-9 V-10 V-11 V-12 V-13 V-1
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Chapter 1 - General Introduction 1.
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linear relationship shown in Figure
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A plot of χT vs. T is an important
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examination of phenyl methylene. In
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different atomic nuclei. Qualitativ
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3) 14 and a variety of thiazyl base
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with one another with an energy bar
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magnetic properties and undergoes a
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heteroatoms which could facilitate
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Figure 1-5. Qualitative molecular o
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temperature. 64 This was a very imp
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dimerization and therefore a quench
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e enough to overcome the energetica
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eaches the lower end of the investi
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DTDAs has been to exploit the rearr
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1.3.4 1,2,3-Dithiazolyl Radicals (I
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aromatic ring not only protects the
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is quite similar to the spin-polari
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compound there are many competing m
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a b c d e Figure 1-16. a) Nonorthog
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would result in non-orthogonal over
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platinum center as well as the phos
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substantial amount of unpaired elec
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I-28 I-29 I-30 The metals manganese
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gave a combination of 2 mononuclear
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changes related to geometric, chemi
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Finally, the last chapter reviews t
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(23) Rajca, A. Chem. Rev. 1994, 94,
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(53) Azuma, N.; Tsutsui, K.; Miura,
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(79) Decken, A.; Cameron, T. S.; Pa
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(102) Herz, R.; Leopold Cassella &
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(128) Aliaga-Alcalde, N., 2003. (12
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Chapter 2 - Structural and Magnetic
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2.2.2 pymDSDA Coordination Complexe
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2.2.3 DTDA Coordination Complexes o
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indicators tend to be very weak str
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In Figure 2-1a, the nickel complex
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2.2.3 Cyclic Voltametry The cyclic
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propensity for intermolecular Se-N
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dimerization motif. One possible ex
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the bridging ligand such that the D
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contacts into four different intera
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e acting as a closed-shell, S = 0,
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2.3.4 [Zn(hfac) 2 ] 2·pymDTDA (II-
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ancillary ligands and the nearly oc
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single molecular unit. Upon closer
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across the entire temperature regim
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2.5 Conclusions and Future Work It
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therefore chain formation. However
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The work presented in this chapter
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736(s), 723(s), 646(s), 632(s), 469
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(0.2023 g, 1.104 mmol) in 30 mL of
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(6) Chattoraj, S. C.; Cupka Jr, A.
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Chapter 3 - 5-oxo-5H-naphtho[1,2-d]
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triethylammonium chloride which was
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3.3.2 Mass Spectrometry A sample of
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3.3.4 X-ray Crystallography Crystal
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a 2-fold screw axis across half of
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number of electrons that this compo
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often generated in situ although wa
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similar to compounds II-1 and II-2,
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3.6 Experimental General All reacti
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Chapter 4 - The Polymorphism of Tri
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4.3 Discussion Prior to the discove
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(derived from angles ranging from 4
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a b c Figure 4-2. Packing diagrams
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polymorphs observed and are therefo
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Chapter 5 5.1 Overview There are se
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success and so a Herz ring closure
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did not immediately precipitate, bu
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Figure 5-2 shows the IR spectra for
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comparison of the infrared data obt
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discussed in section 5.2.2. As the
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Page 179 and 180: equired to obtain a decent agreemen
Page 181 and 182: Considerations have been put toward
Page 183 and 184: chelation pocket is similar to that
Page 185 and 186: the mixture was filtered to remove
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Page 189 and 190: spectrum from about 1900 to 400 cm
Page 191 and 192: doublets of triplets associated wit
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Page 197 and 198: changed substantially after the tra
Page 199 and 200: The reaction to produce V-15 was qu
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Page 203 and 204: which is parallel to the mean plane
Page 205 and 206: of the 1,2,3-DTA rings could act as
Page 207 and 208: mixture was refluxed for 20 h yield
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Page 211 and 212: 1085(w), 1059(w), 1008(w), 917(w),
Page 213 and 214: ___________________________________
Page 215 and 216: Crystallography P 2 1 /c a = 9.1678
Page 217 and 218: Compound Name: 4-(2′-pyrimidyl)-1
Page 219 and 220: Compound Name: [μ-4-(2′-pyrimidy
Page 221 and 222: Magnetometry 192
Page 223 and 224: Crystallography P-1 a = 8.9576, b =
Page 225 and 226: Compound Name: [μ-4-(2′-pyrimidy
Page 227: Magnetometry: 198
Page 231 and 232: Compound Name: 5-oxo-5H-naphtho[1,2
Page 233 and 234: 204
Page 235 and 236: 206
Page 237 and 238: MS (EI + ): 208
Page 239 and 240: Compound Name: 5-chloro-1H-[1,2,5]t
Page 241 and 242: Compound Name: 3-nitro-1,2-naphthaq
Page 243 and 244: Compound Name: 3,4-dioxo-3,4-dihydr
Page 245 and 246: Compound Name: 4,5-dioxo-4,5-dihydr
Page 247 and 248: Compound Name: 6,6′-dinitro-1,1
Page 249 and 250: 220
Page 251: 222
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1,2,3-Dithiazolyl and 1,2,35-Dithiadiazolyl Radicals as Spin-Bearing ...

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