Terminating high-spin bands in 101Rh

High spin states of ¹⁰¹Rh have been populated using the reaction ⁷⁰Zn+³⁶S at 130 MeV. γ-rays were detected with the EUROGAM2 array. New high-spin bands have been observed in this nucleus up to 45/2⁻, 57/2⁻ and 65/2⁺ states. They have been interpreted using the Nilsson-Strutinsky cranking formalism as terminating configurations. Two of the bands were observed up to the predicted terminating states which are built up from g_9/2 protons as well as d_5/2, g_7/2 and h_11/2 neutrons relative to a ⁹⁰Zr core. Received: 30 October 1998     

High-spin study of Xe

High-spin states have been populated in ₅₄¹¹⁹Xe via the ⁹⁶Mo(²⁷Al,p3n) reaction at 133 MeV, using the γ-ray spectrometer to record triple γ-ray coincidences. The known level scheme has been significantly extended and several band crossings identified. In particular, the νh_11/2 yrast band has been extended to I^π = (83/2⁻) and shows features which are consistent with those of smooth band termination at high spin. Theoretical results for ¹¹⁹Xe at high spin are discussed within the framework of cranked Nilsson-Strutinsky calculations, together with results for ¹¹⁷Xe.     

Functionalized pyridylboronic acids and their Suzuki cross-coupling reactions to yield novel heteroarylpyridines

2-Bromo-5-pyridylboronic acid 2a, 2-chloro-5-pyridylboronic acid 2b, 2-methoxy-5-pyridylboronic acid 2c, and 5-chloro-2-methoxy-4-pyridylboronic acid 4 have been synthesized and shown to undergo palladium-catalyzed cross-coupling reactions with heteroaryl bromides to yield novel heteroarylpyridine derivatives. The X-ray crystal structures of 2a and 2b have been obtained.     

Sub‐millisecond transient vertical chevron formation during the electroclinic effect in the smectic A∗ phase

X‐ray diffraction studies are carried out in order to probe the smectic layer structure in liquid crystal devices filled with FLC mixture SCE8 and AFLC mixture CS4001, at a temperature just above the SmA?–SmC? phase transtion. The data gathered are time‐resolved in synchronization with a bipolar voltage pulse applied across the device. The layers are observed to move dynamically and reversibly with voltage application and removal, giving evidence for temporary vertical chevron formation due to the electroclinic effect on a timescale consistent with this phenomenon.     

Bis(fluoroalkyl)acrylic and methacrylic phosphate monomers, their polymers and some of their properties

Ten fluoromonomers of structure (R_FO)₂P(O)OCH₂CH₂OC(O)CRCH₂ were made in 30-64% yield by treating the chloridates (R_FO)₂P(O)Cl with HOCH₂CH₂OC(O)CRCH₂ in chloroform in the presence of triethylamine [R_F=CF₃CH₂, C₂F₅CH₂, C₃F₇CH₂, C₄F₉CH₂, C₄F₉CH₂CH₂ or C₆F₁₃CH₂CH₂; R  H or Me]. The chloromonomer (CCl₃CH₂O)₂P(O)OCH₂CH₂OC(O)CHCH₂ was obtained analogously in 29% yield. Polymerisation of the acrylate monomers, but not the methacrylate monomers, could be effected using α-azoisobutyronitrile as a radical initiator. Acrylic polymers having CF₃CH₂O, CCl₃CH₂O and C₆F₁₃CH₂CH₂O side-chains were obtained as translucent rubbers. Specimens of cotton fabric were treated with solutions of the polymers, and average water and oil repellency ratings measured. Fabric coated with the polymer with the C₆F₁₃CH₂CH₂O side-chain afforded protection from penetration of the test liquids. Treated fabrics were subjected to the limiting oxygen index (LOI) test according to BS EN ISO 4589-2 (1999): this test determines the point at which a material just burns in a volumetric flow of oxygen and nitrogen. The treated fabrics were more fire-resistant (LOI 22-29%) than the untreated fabric (LOI 18%). Fabric coated with the CCl₃CH₂O-based polymer can be considered fire-retardant (LOI 29%). The fluoromonomers were tested for anti-acetylcholinesterase activity and were found to be poor enzyme inhibitors; they are predicted to possess low acute toxicity.     

5-Formyl-2-furylboronic acid as a versatile bifunctional reagent for the synthesis of pi-extended heteroarylfuran systems

5-Formyl-2-furylboronic acid reacts cleanly with a range of heteroaryl bromides under Suzuki-Miyaura cross-coupling conditions to produce 2-formyl-5-heteroarylfuran derivatives. Subsequent Wittig olefination reactions afford pi-conjugated alkene-pyridyl-furan derivatives.     

Templating and selection in the formation of macrocycles containing [[P(micro-NtBu)(2)](micro-NH)](n) frameworks: observation of halide ion coordination

Amination of [ClP(micro-NtBu)](2) (1) using NH(3) in THF gives the cyclophospha(III)zane dimer [H(2)NP(micro-NtBu)](2) (2), in good yield. (31)P NMR spectroscopic studies of the reaction of 1 with 2 in THF/Et(3)N show that almost quantitative formation of the cyclic tetramer [[P(micro-NtBu)](2)(micro-NH)](4) (3) occurs. The remarkable selectivity of this reaction can (in part) be attributed to pre-organisation of 1 and 2, which prefer cis arrangements in the solid state and solution. The macrocycle 3 can be isolated in yields of 58-67 % using various reaction scales. The isolation of the major by-product of the reaction (ca. 0.5-1 % of samples of 3), the pentameric, host-guest complex [[P(micro-NtBu)(2)](2)(micro-NH)](5)(HCl).2 THF] (4.2 THF), gives a strong indication of the mechanism involved. In situ (31)P NMR spectroscopic studies support a stepwise condensation mechanism in which Cl(-) ions play an important role in templating and selection of 3 and 4. Amplification of the pentameric arrangement occurs in the presence of excess LiX (X=Cl, Br, I). In addition, the cyclisation reaction is solvent- and anion-dependent. The X-ray structures of 2 and 4.2 THF are reported.