Temperature-dependent structural properties of a solid urea inclusion compound containing chiral guest molecules: 2-bromotetradecane/urea

1999 ◽  
Vol 77 (12) ◽  
pp. 2105-2118 ◽  
Author(s):  
Lily Yeo ◽  
Kenneth DM Harris
Keyword(s):  
High Temperature ◽  
Structural Properties ◽  
Inclusion Compound ◽  
High Temperature Phase ◽  
Temperature Phase ◽  
Tunnel Structure ◽  
X Ray Diffraction ◽  
Guest Molecules ◽  
Urea Inclusion Compound ◽  
Urea Inclusion

Periodic structural properties of the 2-bromotetradecane/urea inclusion compound have been investigated as a function of temperature. Differential scanning calorimetry between 298 and 98 K identified three well-defined regimes, denoted the high-, intermediate-, and low-temperature phases. The structural properties of each phase (at 293, 207, and 142 K, respectively) have been investigated by single crystal X-ray diffraction. In the high-temperature phase, the inclusion compound has the hexagonal urea tunnel structure (P6122) characteristic of the conventional urea inclusion compounds, with substantial orientational disorder of the guest molecules. In the intermediate-temperature phase, the symmetry is lowered to orthorhombic (C2221), although the host structure remains close to the hexagonal tunnel structure of the high-temperature phase and there is no clear evidence for increased orientational ordering of the guest molecules. In the low-temperature phase, the urea tunnel structure is monoclinic (P21), and is based on a 2 × 2 × 1 supercell of the hexagonal cell of the high-temperature structure. There are four independent types of tunnel, three of which are strongly distorted from hexagonal geometry. Within these distorted tunnels, there is a comparatively narrow distribution of guest molecule orientations, which correlate well with the observed distortions of the tunnels. The 2-bromotetradecane/urea inclusion compound highlights several issues of wider relevance concerning the structural properties of solid inclusion compounds.Key words: urea inclusion compounds, X-ray diffraction, phase transitions, chiral recognition, incommensurate solid, 2-bromotetradecane/urea.

Definitive Structural Characterization of the Conventional Low-Temperature Host Structure in Urea Inclusion Compounds

1997 ◽  
Vol 53 (5) ◽  
pp. 822-830 ◽  
Author(s):  
L. Yeo ◽  
K. D. M. Harris
Keyword(s):  
Low Temperature ◽  
Inclusion Compounds ◽  
Temperature Phase ◽  
Temperature Structure ◽  
Tunnel Structure ◽  
X Ray Diffraction ◽  
Guest Molecules ◽  
Urea Inclusion Compounds ◽  
Urea Inclusion ◽  
Low Temperature Phase

Structural properties of the 1,10-dibromodecane/urea and 1,12-dibromododecane/urea inclusion compounds have been determined by single-crystal X-ray diffraction for both the high- and low-temperature phases. In the high-temperature phase both inclusion compounds have the conventional hexagonal urea tunnel structure, with substantial orientational disorder of the guest molecules. In the low-temperature phase the urea tunnel structure distorts to an orthorhombic structure, based on a distorted form of the orthohexaganol cell of the high-temperature structure and with the loss of the C centre. Within this tunnel structure there is evidence that the guest molecules have a narrow distribution of orientations (with respect to rotation about the tunnel axis) and the preferred orientation of the guest molecules correlates well with the observed distortion of the host tunnel. This represents the first accurate and reliable report of the conventional low-temperature structure of urea inclusion compounds. Previous powder X-ray diffraction studies have confirmed that the host structure in the low-temperature phase of 1,10-dibromodecane/urea is the same as that in the low-temperature phase of the alkane/urea inclusion compounds.

scholarly journals High-temperature phase transition of SrRuO3and SrHfO5: X-ray diffraction and PAC spectroscopy

1996 ◽  
Vol 52 (a1) ◽  
pp. C364-C364
Author(s):  
J. A. Guevara ◽  
S. L. Cuffini ◽  
Y. P. Mascarenhas ◽  
P. de la Presa ◽  
A. Ayala ◽  
...  
Keyword(s):  
Phase Transition ◽  
High Temperature ◽  
High Temperature Phase ◽  
Temperature Phase ◽  
Pac Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Temperature Phase Transition

Structural properties of the guest species in diacyl peroxide/urea inclusion compounds: an X-ray diffraction investigation

1990 ◽  
Vol 431 (1882) ◽  
pp. 245-269 ◽  
Keyword(s):  
Single Crystal ◽  
Structural Properties ◽  
Inclusion Compounds ◽  
X Ray Diffraction ◽  
Channel Axis ◽  
Guest Molecules ◽  
X Ray ◽  
Urea Inclusion Compounds ◽  
Diacyl Peroxide ◽  
Urea Inclusion

In this paper we report single crystal X-ray diffraction studies of urea inclusion compounds containing diacyl peroxides (dioctanoyl peroxide (OP), diundecanoyl peroxide (UP), lauroyl peroxide (LP)) as the guest component. In these inclusion compounds, the host (urea) molecules crystallize in a hexagonal structure that contains linear, parallel, non-intersecting channels (tunnels). The guest (diacyl peroxide) molecules are closely packed inside these channels with a periodic repeat distance that is incommensurate with the period of the host structure along the channel axis. Furthermore, there is pronounced inhomogeneity within the guest structure: within each single crystal, there are regions in which the guest molecules are three-dimensionally ordered, and other regions in which they are only one-dimensionally ordered (along the channel axis). Although it has not proven possible to ‘determine’ the guest structures in the conventional sense, substantial information concerning their average periodicities and their orientational relationships with respect to the host has been deduced from single crystal X-ray diffraction photographs recorded at room temperature. For OP/urea, UP/urea and LP/urea, the guest structure in the three-dimensionally ordered regions is monoclinic, and six types of domain of this monoclinic structure can be identified within each single crystal. The relative packing of diacyl peroxide molecules is the same in each domain, and the different domains are related by 60° rotation about the channel axis. For each of these inclusion compounds, the offset between the ‘heights’ of the guest molecules in adjacent channels is the same ( ca . 4.6 Å (4.6 x 10 -10 m)) within experimental error, suggesting that the relative interchannel packing of the guest molecules is controlled by a property of the diacyl peroxide group. In addition to revealing these novel structural properties, the work discussed in this paper has more general relevance concerning the measurement and interpretation of single crystal X-ray diffraction patterns that are based on more than one three-dimensionally periodic reciprocal lattice. Seven separate reciprocal lattices are required to rationalize the complete X-ray diffraction pattern from each diacyl peroxide/urea crystal studied here.

scholarly journals Study of the High Temperature Phase of 1,16-Hexadecanediol by Polarized Light Microscopy and Glancing Incidence X-Ray Diffraction

2018 ◽  
Vol 24 (S1) ◽  
pp. 2248-2249
Author(s):  
M. Ramírez-Cardona ◽  
M.P. Falcón-León ◽  
G. Luis-Raya ◽  
G. Mejía-Hernández ◽  
R. Arceo ◽  
...  
Keyword(s):  
High Temperature ◽  
Light Microscopy ◽  
Polarized Light ◽  
High Temperature Phase ◽  
Polarized Light Microscopy ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
X Ray

35Cl NQR and Structural Studies of Chloroacetanilides C6H3Cl2NHCOCH3-xClx, 1 ≤ x ≤ 3

1992 ◽  
Vol 47 (1-2) ◽  
pp. 160-170
Author(s):  
Dirk Groke ◽  
Shi-Qi Dou ◽  
Alarich Weiss
Keyword(s):  
High Temperature ◽  
Low Temperature ◽  
Temperature Dependence ◽  
Phenyl Group ◽  
High Temperature Phase ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Chlorine Atoms ◽  
Space Group ◽  
Low Temperature Phase

AbstractThe temperature dependence of 35Cl NQR frequencies and the phase transition behaviour of chloroacetanilides (N-[2,6-dichlorophenyl]-2-chloroacetamide, -2,2-dichloroacetamide, -2,2,2-trichloroacetamide) were investigated. The crystal structure determination of N-[2,6-dichlorophenyl]- 2-chloroacetamide leads to the following: a = 1893.8 pm, b = 1110.7 pm, c = 472.1 pm, space group P212121 = D24 with Z = 4 molecules per unit cell. The arrangement of the molecules and their geometry is comparable to the high temperature phase of the acetyl compound N-[2,6-dichlorophenyl]- acetamide. For N-[2,6-diclorophenyl]-2,2,2-trichloroacetamide it was found: a = 1016.6 pm, b = 1194.3 pm, c = 1006.7 pm, ß= 101.79°, space group P21/c = C52h, Z = 4. The structure is similar to the low temperature phase of N-[2,6-dichlorophenyl]-acetamide. Parallelism between the temperature dependence of the 35C1 NQR lines of the CCl3 group and the X-ray diffraction results concerning the different behaviour of the chlorine atoms was observed. The structures of the compounds show intermolecular hydrogen bonding of the N - H • • • O - C type. The phenyl group and the HNCO function are nearly planar. A bleaching out of several 35Cl NQR lines at a temperature far below the melting point of the substances was observed. The different types of chlorine atoms (aromatic, chloromethyl) can be distinguished by their temperature coefficients of the 35Cl NQR frequencies. All the resonances found show normal "Bayer" temperature behaviour. N-[2,6-dichlorophenyl]-2,2-diehloroacetamide shows several solid phases. One stable low temperature phase and an instable high temperature phase (at room temperature) were observed. The different phases were detected by means of 35Cl NQR spectroscopy and thermal analysis

Investigation on the Thermal Stability of the Compounds Y3Fe29-xCrx

2013 ◽  
Vol 820 ◽  
pp. 71-74
Author(s):  
Xiao Hua Wang ◽  
Wei He ◽  
Ling Min Zeng
Keyword(s):  
Thermal Stability ◽  
High Temperature ◽  
Single Phase ◽  
Binary Compound ◽  
High Temperature Phase ◽  
Temperature Phase ◽  
Transition Elements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermal Stability Of

Binary compound Y3Fe29cannot be directly formed by rare earth Y and Fe and the third element M (non-iron transition elements) must be introduced to form ternary compound Y3(Fe,M)29. In this work, six alloys with compositions of the Y3Fe29-xCrx(x=1,2,3,4,5,6) were prepared and investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and differential thermal analysis (DTA). The study on the thermal stability of these compounds points to that the compoundY3(Fe,Cr)29is a high temperature phase and exists above 1100K. The alloys with single-phase of Y3(Fe,Cr)29was decomposed into Y2(Fe,Cr)17and Y(Fe,Cr)12annealed at high temperature 1100K.

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