Raman spectrum of crystalline aminosulphonic acid

The Raman spectrum of a single crystal of sulphamic acid has been recorded withλ 2537 excitation. Thirty-eight lines have been observed, of which twenty-nine have been recorded for the first time. Seven Raman lines with shifts in the region 50–155 cm.−1 have been assigned to the lattice oscillations, two at 177 and 240 cm.−1 have been attributed to the low-frequency hydrogen bond vibrations.. The splitting of the degenerate modes and the appearance of N-H....O bonded stretching vibrations are consistent with the structural data which expect the presence of the free molecule as a Zwitter ion with only slight distortion from C3v symmetry.

Raman spectrum of crystalline cadmium acetate dihydrate

The Raman spectrum of a single crystal of cadmium acetate dihydrate has been recorded for the first time using λ 2537 excitation. Twenty-three lines have been observed out of which ten have been attributed to the internal oscillations of the acetate ion, nine to the lattice modes, two to low-frequency hydrogen bond vibrations. A line at 308 cm.−1 and the continuum 3250–3560 cm.−1 have been assigned to the Cd-O6 and internal vibrations of the water molecules.

Raman spectra of ferro-electric crystals Part IV. Lithium hydrazinium sulphate (LiN2H5SO4)

The Raman spectrum of lithium hydrazinium sulphate has been recorded both in the single crystal form and in aqueous solutions. The crystal exhibits thirty-eight Raman lines having the frequency shifts 52, 70, 104, 146, 174, 220, 260, 302, 350, 454, 470, 610, 630, 715, 977, 1094, 1115, 1132, 1177, 1191, 1260, 1444, 1493, 1577, 1630, 1670, 2205, 2484, 2553, 2655, 2734, 2848, 2894, 2939, 3028, 3132, 3290 and 3330 cm.−1 The aqueous solution gave rise to six Raman lines at 452, 980, 1050–1200, 1260, 1425 and 1570 cm.−1 apart from a maximum at 180 cm.−1 in the ‘wing’ accompanying the Rayleigh line. The observed Raman lines have been assigned as arising from the vibrations of the SO4 ion, N2H5+ ion, Li-O4 group, hydrogen bond and the lattice. The influence of the hydrogen bond on the N-H stretching vibrations has been pointed out. The various features of the observed spectrum strongly support the hypothesis that the NH3 group in the crystal is rotating around the N-N axis at room temperature.

Raman spectrum of hydroxylamine hydrochloride (NH3OH.Cl)

The Raman spectrum of hydroxylamine hydrochloride (NH3OH.Cl) in the form of a single crystal has been photographed usingλ 2536·5 excitation. 32 Raman lines with frequency shifts 40, 57, 78, 88, 111, 125, 135, 156, 187, 217, 250, 330, 550, 575, 1004, 1168, 1204, 1470, 1496, 1565, 1590, 1979, 2636, 2710, 2750, 2789, 2926, 2970, 3000, 3050, 3141 and 3220 cm.−1 have been recorded. Of these, the first 8 low-frequency lines belong to the external oscillation, while the four lines at 187, 217, 250 and 330 cm.−1 should be attributed to the vibrations of the hydrogen bond valence vibrations. The remaining Raman lines have been assigned to the vibrations of the NH3OH ion. The O-H and N-H stretching vibrations are very much influenced by the presence of the hydrogen bonds in the crystal.

Raman spectrum of diglycine barium chloride monohydrate

The Raman spectrum of diglycine barium chloride monohydrate in the single crystal form has been recorded using λ 2536·5 excitation. 43 Raman lines (9 lattice and 34 internal) have been recorded. Satisfactory assignments have been given for most of the observed Raman lines. It is concluded from a comparison of the Raman spectrum of this compound with those of glycine and of other addition compounds of glycine, that the glycine unit exists in the zwitterion form in the structure of diglycine barium chloride monohydrate.

Raman spectrum of triglycine selenate (G3Se), [(NH2CH2COOH)3 H2SeO4]

The Raman spectrum of a single crystal of triglycine selenate G3Se which is ferroelectric below 22° C. has been photographed using λ 2537 excitation. 42 Raman lines have been recorded of which 6 belong to the lattice spectrum, 3 are due to NH...O oscillations and the remaining 33 are due to internal oscillations of the ions of glycine and SeO4--. There is a close similarity between the spectrum of triglycine selenate and the spectrum of its isomorph, triglycine sulphate, the frequency shifts due to the SO4-- ion being replaced by the frequency shifts due to the SeO4-- ion. The existence of glycine in the zwitterion form in the structure of G3Se is substantiated by the appearance in the Raman spectrum of lines which are attributable to NH3+ groups and COO- groups. The appearance of the additional C-H line at 2982 cm.-1 in the spectrum of triglycine selenate which is absent in the spectrum of α-glycine indicates the existence of planar monoprotonated glycine also in the structure, as indicated by X-ray studies.

Raman spectrum of sodium iodide

Raman spectrum of a single crystal of sodium iodide has been recorded for the first time using lambda 2537 excitation. The general features of the spectrum are discussed in the light of the existing theories on the dynamics of the alkali halides. The authors wish to thank Professor D.Y.Phadke of the Tata Institute of Fundamental Research, Bombay, for presenting the crystal of Nal used in the present investigation.

Raman spectrum of lanthanum ethyl sulphate nonahydrate

Raman spectrum of a single crystal of lanthanum ethyl sulphate has been recorded for the first time using the λ 2537 radiation Forty-one lines have been identified out of which eight belong to the lattice oscillations, seven to the internal vibrations of the water molecule and the remaining twenty-six to the internal vibrations of the ethyl sulphate group. The Raman spectrum of ethyl sulphate (liquid) has also been recorded using the λ 4358 excitation and is compared with the spectrum of lanthanum ethyl sulphate. Thirty Raman lines could be identified in the spectrum of ethyl sulphate, of which fourteen are recorded for the first time. Probable assignments of the observed frequencies are also given. The sulphate group is found to have O-SO3 structure in lanthanum ethyl sulphate, while it has a co-ordination {Mathematical expression} in ethyl sulphate.

Transition metal complexes of 3-aryl-2-substituted 1,2-dihydroquinazolin-4(3H)-one derivatives: New class of analgesic and anti-inflammatory agents

Five-coordinate, neutral transition metal complexes of newly designed pyridine-2-ethyl-(3-carboxyhdeneamino)-3-(2-phenyl)-1,2-dihydroquinazoli n-4(3H)-one (L) were synthesized and characterized The structure of ligand is confirmed by single crystal X-ray diffraction studies The compounds were evaluated for the anti-inflammatory activity by carrageenan-induced rat paw edema model while their analgesic activity was determined by acetic acid-induced writhing test in mice wherein the transition metal complexes were found to be more active than the free ligand (C) 2010 Elsevier Masson SAS All rights reserved.

Raman spectrum of l-asparagine monohydrate

The Raman spectrum of l-asparagine monohydrate in the form of a single crystal has been recorded for the first time. λ 2537 excitation has been used. Fifty-three Raman frequency shifts have been recorded. They are grouped as follows: Eight Raman lines coming under the lattice spectrum, three Raman lines arising from low-frequency vibrations of the hydrogen bonds and the remaining forty-two arising from the internal oscillations of the asparagine molecule. Appropriate assignments have been given for the observed Raman lines

New Solid State Forms of the Anti-HIV Drug Efavirenz. Conformational Flexibility and High Z ` Issues

Structural information on the solid forms of efavirenz, a non-nucleoside reverse transcriptase inhibitor, is limited, although various polymorphic forms of this drug have been patented. We report here structural studies of four new crystal forms a pure form, a cyclohexane solvate, and cocrystals with 1,4-cyclohexanedione and 4,4'-bipyridine. Temperature dependent single-crystal to single-crystal phase transitions are observed for the pure form and for the cyclohexane solvate with an increase in the number of symmetry independent molecules, Z', upon a lowering of temperature. Other issues related to these solid forms, such as thermal stability, conformational flexibility, and high Z' occurrences, are addressed by using a combined experimental and computational approach.

A Method for Purifying Bulk Gallium Arsenide by Chemical Vapour Transport

The need for high purity materials for the growth of epitaxial layers of GaAs and the limitations of present source materials are discussed. A for purifying bulk quantitites of GaAs using chemical vapour transport is presented. GaAs is contained in a silica capsule which has a small orifice allow movement of gas between inside and outside. The capsule is contained in a heated tube and hydrogen chloride is used as the transporting agent. Growth rates of 0.1 g/h have been obtained and evidence for the purification is presented along with a discussion of the principles involved. The potentialities of the method for both purification and for the growth of single crystal substrate material are stressed.--AA

An electron paramagnetic resonance study of Pr0.6Ca0.4MnO3 across the charge-ordering transition

We report the first electron paramagnetic resonance studies of single crystals and powders of Pr0.6Ca0.4MnO3 in the 300-4.2 K range, covering the charge-ordering transition (Tco) at ~240 K and antiferromagnetic transition (TN) at ~170 K. The asymmetry parameter for the Dysonian single-crystal spectra shows an anomalous increase at Tco. Below Tco the g-value increases continuously, suggesting a gradual strengthening of the orbital ordering. The linewidth undergoes a sudden increase at Tco and continues to increase down to TN. The intensity increases as the temperature is decreased until Tco is reached, due to the renormalization of the magnetic susceptibility arising from the build-up of ferromagnetic correlations.

Cryptosin, a cardenolide from the leaves of Cryptolepis buchanani

A new cardenolide named cryptosin was isolated from the leaves of Cryptolepis buchanani. By spectral studies and single crystal X-ray crystallography, cryptosin was found to possess a novel structure. The structure thus established was 3β-(d-deoxy glucose-oxy)-14β,11β-dihydroxy-7α,8α-epoxy-12-oxo-5β- card-20 (22)-enolide.

Amido binding to ReO3+ core: Synthesis, structure and intermolecular interactions

The light green coloured complexes of general formula [(ReO)-O-V(L)CI(OH2)]Cl have been synthesised in good yields by reacting [RcvOCl(3)(AsPh3)21 with HL in dichloromethane in dinitrogen atmosphere. Here, L- is the deprotonated form of N',N'-bis(2-pyridylmethyl)amine (HL1); N-(2-pyridylmethyl)-N',N'-dimethylethylenediamine (HL2) and N-(2-pyridylmethyl)-N',N-diethylethylenediamine (HL3). Single crystal X-ray structure determination of [(ReO)-O-V(L-1)Cl(OH2)Cl confirms the amido binding of ReO3+ species. In the solid state of [(ReO)-O-V(L-1)Cl(OH2)]Cl, the coordinated and counter chloride ions are engaged in Re-Cl... H-C(ring), Cl...H-C(ring) and Re(OH2)...Cl hydrogen bonding and forming of a supramolecular network in the solid state. The subunit of the supramolecular network consists of one eight-membered and two nine-membered hydrogen bonded rings. The average diameters of eight-membered and nine-membered rings are similar to 3.70 and similar to 5.26 angstrom, respectively.