Diffraction studies, x-ray

Detailed x-ray diffraction studies on polar liquid crystals have demonstrated tire existence of multiple smectic A and smectic C phases [M, 15 and 16]. The first evidence for a smectic A-smectic A phase transition was provided by tire optical microscopy observations of Sigaud etal [17] on binary mixtures of two smectogens. Different stmctures exist due to tire competing effects of dipolar interactions (which can lead to alternating head-tail or interdigitated stmctures) and steric effects (which lead to a layer period equal to tire molecular lengtli). These... 

Li J and Abruna FI D 1997 Coadsorption of sulphate/bisulphate anions with Fig cations during Fig underpotential deposition on Au (111) An In situ x-ray diffraction study J. Phys. Chem. B 101 244-52... 

Zegenhagen J, Kazimirov A, Scherb G, Kolb D M, Smilgies D-M and Feidenhans l R 1996 X-ray diffraction study of a semiconductor/electrolyte interface n-GaAs(001)/H2S04( Cu) 1996 Surf. Sc/. 352-354 346-51... 

X-Ray diffraction studies of the oxoacid anions indicate the following probable arrangements for the acids ... 

The same reaction performed in ether at 0°C (336) gives the same major adduct, but the structure proposed by Acheson et al. corresponds to 86, although such a structure is hardly compatible with the presence of an isolated low-field proton. Very recently, in a reinvestigation of these cyclo-additions of DMA to azoles (338, 339), Acheson et al. were able to establish the correct structure of the adducts on the base of CNMR spectra and X-ray diffraction studies. The adduct of thiazole is represented by formula 87, and it results from the rearrangement of the... 

The thickness of the crystal plates or lamellae can be measured by x-ray diffraction studies and other methods. It is a well-established fact that thinner lamellae are formed at lower temperatures of crystallization. 

The stmcture of DPXN was determined in 1953 from x-ray diffraction studies (22). There is considerable strain energy in the buckled aromatic rings and distorted bond angles. The strain has been experimentally quantified at 130 kj/mol (31 kcal/mol) by careful determination of the formation enthalpy through heat of combustion measurements (23). The release of this strain energy is doubtiess the principal reason for success in the particularly convenient preparation of monomer in the parylene process. 

Poly(vinyl fluoride) [24981-14-4] (PVF) is a semicrystaltiae polymer with a planar, zig-zag configuration (50). The degree of crystallinity can vary significantly from 20—60% (51) and is thought to be primarily a function of defect stmctures. Wide-line nmr and x-ray diffraction studies show the unit cell to contain two monomer units and have the dimensions of a = 0.857 nm, b = 0.495 nm, and c = 0.252 nm (52). Similarity to the phase I crystal form of poly (vinytidene fluoride) suggests an orthorhombic crystal (53). 

A left-handed double-heUcal stmcture has been proposed for geUan in the crystalline state, based on x-ray diffraction studies (227). The presence of acetyl groups presumably dismpts interchain aggregation, since these groups are postulated to be on the outside of the heUces. The role played by acetyl and glyceryl ester groups and their influence on the double-heUcal stmcture has been studied using computet models (232). 

These hydrated salts contain bidentate carbonate ligands and no water molecules are bound directly to the central metal atom. The only single-crystal x-ray diffraction studies available are those for salts of (4) (52—54) and the mineral tuliokite [128706 2-3], Na2BaTh(C03)2 -6H20], which contains the unusual Th(C02) 2 anion (5) (55). 

Trialkyl- and triarylarsine sulfides have been prepared by several different methods. The reaction of sulfur with a tertiary arsine, with or without a solvent, gives the sulfides in almost quantitative yields. Another method involves the reaction of hydrogen sulfide with a tertiary arsine oxide, hydroxyhahde, or dihaloarsorane. X-ray diffraction studies of triphenylarsine sulfide [3937-40-4], C gH AsS, show the arsenic to be tetrahedral the arsenic—sulfur bond is a tme double bond (137). Triphenylarsine sulfide and trimethylarsine sulfide [38859-90-4], C H AsS, form a number of coordination compounds with salts of transition elements (138,139). Both trialkyl- and triarylarsine selenides have been reported. The trialkyl compounds have been prepared by refluxing trialkylarsines with selenium powder (140). The preparation of triphenylarsine selenide [65374-39-2], C gH AsSe, from dichlorotriphenylarsorane and hydrogen selenide has been reported (141), but other workers could not dupHcate this work (140). 

A single-crystal x-ray diffraction study has shown that the borate anion in anhydrous borax is polymeric in nature and is formed via oxygen bridging of triborate and pentaborate groups (83). The chemistry of anhydrous borax has been reviewed (73,84). 

A single-crystal x-ray diffraction study gives a stmctural formula of Na2 [B5 0g (0H)4]-3H2 0 and contains the pentaborate ion analogous to that found in the corresponding potassium compound (86). 

The composition varies with the heat treatment and the end point according to x-ray diffraction studies it is a form of carbon that reconverts to weU-ordered graphite on heating to 1800°C. Before the use of x-rays, chemists used the Brodie reaction to differentiate between graphitic carbons and turbostratic carbons. Turbostratic carbons yield a brown solution of humic acids, whereas further oxidation of graphite oxide produces mellitic acid (benzenehexacarboxyhc acid) [517-60-2] ... 

X-Ray diffraction studies have been carried out on other 1,2-benzisothiazoles (72JCS(P2)2125, 74CSC535, 76G769) and complexes of substituted 1,2-benzisothiazoles with... 

X-Ray diffraction studies on the 3-imino-l-azetine (205 Ar = p-FC6H4), show that the four-membered ring is planar with an unusually long endocyclic C=N bond (74ZN(B)399). The structure of the 1-azetine A7-oxide (275) has also been determined by X-ray crystallographic techniques (79CC993). 

Confirmation of the structure of benzylpenicillin by X-ray diffraction studies (B-49MI51101). 

Wark, Whitlock, and co-workers [72]-[75] extend these ideas in shock compression of < 111 >-oriented silicon single crystals. The method of producing the shock wave differs from previous X-ray diffraction studies, but the basic concepts are the same. Higher X-ray fluences result in a time resolution of 0.05-0.1 ns. This permits a sequence of exposures at various irradiances and delay times, thus mapping the interatomic spacing of the shock-compressed surface as a function of time. 

Q. Johnson, A.C. Mitchell, and L. Evans, X-Ray Diffraction Study of Single... 

Kennard, O., Hunter, W.N. Oligonucleotide structure a decade of results from single crystal x-ray diffraction studies. Q. Rev. Biophys. 22 327-379, 1989. 

Satow, Y., et al. Phosphorylcholine-binding immunoglobulin Fab McPC603. An x-ray diffraction study at 2.7 A. 

As described in Chapter 2, the first complete protein structure to be determined was the globular protein myoglobin. However, the a helix that was recognized in this structure, and which has emerged as a persistent structural motif in the many hundreds of globular proteins determined subsequently, was first observed in x-ray diffraction studies of fibrous proteins. 

A. Segmuller, I, C. Noyan, V. S. Speriosu. X-Ray Diffraction Studies of Thin Films and Multilayer Structures. Prog. Cryst. Growth and Charact. 18,21, 1989. 

---