Polymorphs of Neutral Red, a Redox-Mediating Phenazine in Biological Systems

2017 ◽  
Vol 70 (9) ◽  
pp. 1032 ◽  
Author(s):  
Mackenzie Labine-Romain ◽  
Sabrina Beckmann ◽  
Mohan Bhadbhade ◽  
Saroj Bhattacharyya ◽  
Michael Manefield ◽  
...  
Keyword(s):  
Room Temperature ◽  
Control Method ◽  
Scale Up ◽  
Industrial Process ◽  
Neutral Red ◽  
Crystalline Solid ◽  
Temperature Structure ◽  
X Ray Diffraction ◽  
Methane Generation ◽  
Raman And Infrared Spectroscopy

Neutral red 1 is a heterocyclic phenazine that, as a crystalline solid, has been observed to accelerate microbial methane generation from coal. Scale-up to an industrial process will require large quantities of neutral red crystals, hence an understanding of any polymorphic behaviour is essential for careful control of this process. A room-temperature structure of 1 (Form I) has been reported previously, and this study describes a new polymorph (Form II) crystallising from aqueous solution at 50°C, or transforming from Form I over an incubation time of one week at 70°C. Single-crystal X-ray diffraction has been used to study the molecular arrangements and intermolecular interactions in the new polymorph, and compared with those found in the room temperature form. Both polymorphs have been characterised using Raman and infrared spectroscopy, and a synthetic mixture of polymorphs successfully imaged using Raman spectroscopy. Raman imaging is proposed as a quality control method for small quantities of sample to ensure the correct polymorph is produced as a feedstock for this new methanogenesis process.

Influence of Molecular Conformation on the Solid State Packing of 1,2-Diglycerides Study of 1,2-Dipalmitin and Some Structural Analogs by Electron Diffraction, X-Ray Diffraction, and Infrared Spectroscopy

1978 ◽  
Vol 33 (1-2) ◽  
pp. 39-49 ◽  
Author(s):  
Douglas L. Dorset ◽  
Walter A. Pangborn ◽  
Anthony J. Hancock ◽  
Iris S. Lee
Keyword(s):  
Infrared Spectroscopy ◽  
Solid State ◽  
Room Temperature ◽  
Molecular Conformation ◽  
Crystalline Solid ◽  
X Ray Diffraction ◽  
Chain Packing ◽  
X Ray ◽  
Monoclinic Form ◽  
Extended Chain

Abstract Diffraction studies on natural 1,2-dipalmitin and on analogs, including those based on the configurational isomers of cyclopentane-1,2,3-triol reveal that the 1,2-diglycerides crystallize from solvent with chain methylene packing identical to the monoclinic form of even-chain alkanes. The chains probably are folded back in “hairpin” fashion as found in phospholipid crystal structures. Acyl shifts are observed to occur in the crystalline solid state at room temperature to give the 1,3-diglyceride. Analogs based on the above-mentioned cyclitols show that isomers with adjacent chains trans to the ring (possibly extended chain packing) or with chains cis to the ring (“hair­ pin”) crystallize readily. Both possibly extended chain configurational isomers have the α-form as well as β′-forms and a β-polymorph. The hairpin isomers each give a β′-polymorph but only the all-cts isomer gives an α-form.

Single-Crystal X-Ray Diffraction Study of the Room Temperature Structure and Orientational Disorder of C 70

1994 ◽  
Vol 27 (5) ◽  
pp. 359-364 ◽  
Author(s):  
E Blanc ◽  
H.-B Bürgi ◽  
R Restori ◽  
D Schwarzenbach ◽  
P Stellberg ◽  
...  
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
Room Temperature ◽  
Temperature Structure ◽  
X Ray Diffraction ◽  
Orientational Disorder ◽  
X Ray

Order and disorder in acenaphthylene

1973 ◽  
Vol 334 (1596) ◽  
pp. 19-48 ◽  
Keyword(s):  
Low Temperature ◽  
Room Temperature ◽  
Temperature Structure ◽  
Intermediate Form ◽  
X Ray Diffraction ◽  
Space Group ◽  
Order And Disorder ◽  
Temperature Form ◽  
Diffraction Effects

Acenaphthylene, C 12 H 8 , occurs in space group Pbam (or Pba2) at room temperatures (23 °C) with a = 7.705 (5), b = 7.865 (5), c = 14.071 (5) Å and Z = 4, and is disordered. At about 130 K it undergoes a reversible transition to space group P2 1 nm with a = 7.588 (13), b = 7.549 (10), c = 27.822 (2) Å and Z = 8 (85 K) with an ordered structure. A general study of the system has revealed that the structure of both forms consists of layers of closely packed molecules stacked in the c direction. The room temperature structure has a two-layer repeat and the low temperature form a four-layer repeat. Observation of diffuse X-ray diffraction effects at temperatures close to the transition indicates that an intermediate form having a six-layer repeat is formed. A preliminary structure determination of the low-temperature form reveals that the four layers though having a similar packing scheme differ in the orientation of the constituent molecules relative to c . It is proposed that the almost circular shape of the molecules allows each layer to change its identity under thermal agitation by a rotation of its constituent molecules in their own planes. The transition can be explained in terms of changes of the correlations between neighbouring layers. A simple model based on short-range order parameters is described, which explains the occurrence of the six-layer intermediate and the observed sequence of diffuse diffraction phenomena. The nature of the structure of the disordered room temperature form, which is predicted by this model, is confirmed as far as possible with the data available which are limited because of the dearth of high-angle diffraction maxima.

Investigation into the Crystal Structure of the Perovskite Lead Hafnate, PbHfO3

1998 ◽  
Vol 54 (1) ◽  
pp. 18-28 ◽  
Author(s):  
D. L. Corker ◽  
A. M. Glazer ◽  
W. Kaminsky ◽  
R. W. Whatmore ◽  
J. Dec ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Room Temperature ◽  
Lead Zirconate ◽  
Crystal Structure Analysis ◽  
Temperature Structure ◽  
X Ray Diffraction ◽  
Neutron Data ◽  
X Ray

The room-temperature crystal structure of the perovskite lead hafnate PbHfO3 is investigated using both low-temperature single crystal X-ray diffraction (Mo Kα radiation, λ = 0.71069 Å) and polycrystalline neutron diffraction (D1A instrument, ILL, λ = 1.90788 Å). Single crystal X-ray data at 100 K: space group Pbam, a = 5.856 (1), b = 11.729 (3), c = 8.212 (2) Å, V = 564.04 Å3 with Z = 8, μ = 97.2 mm−1, F(000) = 1424, final R = 0.038, wR = 0.045 over 439 reflections with F >1.4σ(F). Polycrystalline neutron data at 383 K: a = 5.8582 (3), b = 11.7224 (5), c = 8.2246 (3) Å, V = 564.80 Å3 with χ2 = 1.62. Although lead hafnate has been thought to be isostructural with lead zirconate, no complete structure determination has been reported, as crystal structure analysis in both these materials is not straightforward. One of the main difficulties encountered is the determination of the oxygen positions, as necessary information lies in extremely weak l = 2n + 1 X-ray reflections. To maximize the intensity of these reflections the X-ray data are collected at 100 K with unusually long scans, a procedure which had previously been found successful with lead zirconate. In order to establish that no phase transitions exist between room temperature and 100 K, and hence that the collected X-ray data are relevant to the room-temperature structure, birefringence measurements for both PbZrO3 and PbHfO3 are also reported.

Synthesis and structural characterization of BaV4O9

2007 ◽  
Vol 63 (2) ◽  
pp. 270-276 ◽  
Author(s):  
Thomas Reeswinkel ◽  
Sebastian Prinz ◽  
Karine M. Sparta ◽  
Georg Roth
Keyword(s):  
Crystal Structure ◽  
Thermal Expansion ◽  
Structural Characterization ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
Temperature Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermal Expansion Tensor

The new spin ½ V4+ barium oxovanadate BaV4O9 was synthesized and studied by means of single-crystal X-ray diffraction. Its room-temperature structure is monoclinic, space group P2/c. We discuss the temperature evolution of the crystal structure and thermal expansion tensor of the material between 293 and 100 K.

scholarly journals The modulated low-temperature structure of malayaite, CaSnOSiO4

2020 ◽  
Vol 76 (3) ◽  
pp. 316-321
Author(s):  
Thomas Malcherek ◽  
Bianca Paulenz ◽  
Michael Fischer ◽  
Carsten Paulmann
Keyword(s):  
Crystal Structure ◽  
Density Functional ◽  
Room Temperature ◽  
Phonon Dispersion ◽  
Temperature Structure ◽  
X Ray Diffraction ◽  
Static Displacement ◽  
X Ray ◽  
First Order ◽  
Density Functional Perturbation Theory

The crystal structure of the mineral malayaite has been studied by single-crystal X-ray diffraction at a temperature of 20 K and by calculation of its phonon dispersion using density functional perturbation theory. The X-ray diffraction data show first-order satellite diffraction maxima at positions q = 0.2606 (8)b*, that are absent at room temperature. The computed phonon dispersion indicates unstable modes associated with dynamic displacements of the Ca atoms. The largest-frequency modulus of these phonon instabilities is located close to a wavevector of q = 0.3b*. These results indicate that the malayaite crystal structure is incommensurately modulated by static displacement of the Ca atoms at low temperatures, caused by the softening of an optic phonon with Bg symmetry.

Low-temperature behaviour of K2Sc[Si2O6]F: determination of the lock-in phase and its relationships with fresnoite- and melilite-type compounds

2017 ◽  
Vol 73 (5) ◽  
pp. 923-930
Author(s):  
C. Hejny ◽  
L. Bindi
Keyword(s):  
Low Temperature ◽  
Room Temperature ◽  
Temperature Structure ◽  
X Ray Diffraction ◽  
Temperature Behaviour ◽  
Modulated Structure ◽  
Incommensurate Structure ◽  
Commensurate Phase ◽  
Lock In

K2Sc[Si2O6]F exhibits, at room temperature, a (3 + 2)-dimensional incommensurately modulated structure [a= 8.9878 (1),c= 8.2694 (2) Å,V= 668.01 (2) Å3; superspace groupP42/mnm(α,α,0)000s(−α,α,0)0000] with modulation wavevectorsq1= 0.2982 (4)(a* +b*) andq2= 0.2982 (4)(−a* +b*). Its low-temperature behaviour has been studied by single-crystal X-ray diffraction. Down to 45 K, the irrational component α of the modulation wavevectors is quite constant varying from 0.2982 (4) (RT), through 0.2955 (8) (120 K), 0.297 (1) (90 K), 0.298 (1) (75 K), to 0.299 (1) (45 K). At 25 K it approaches the commensurate value of one-third [i.e.0.332 (3)]: thus indicating that the incommensurate–commensurate phase transition takes place between 45 K and 25 K. The commensurate lock-in phase of K2Sc[Si2O6]F has been solved and refined with a 3 × 3 × 1 supercell compared with the tetragonal incommensurately modulated structure stable at room temperature. This corresponds to a 3 × 1 × 3 supercell in the pseudo-orthorhombic monoclinic setting of the low-temperature structure, space groupP2/m, with lattice parametersa= 26.786 (3),b= 8.245 (2)c= 26.824 (3) Å, β = 90.00 (1)°. The structure is a mixed tetrahedral–octahedral framework composed of chains of [ScO4F2] octahedra that are interconnected by [Si4O12] rings with K atoms in fourfold to ninefold coordination. Distorted [ScO4F2] octahedra are connected to distorted Si tetrahedra to form octagonal arrangements closely resembling those observed in the incommensurate structure of fresnoite- and melilite-type compounds.

scholarly journals The behavior of the lattice parameters in the Bi-Sn-Zn system

2007 ◽  
Vol 43 (2) ◽  
pp. 151-159 ◽  
Author(s):  
Helena Braga ◽  
J. Ferreira ◽  
L.F. Malheiros
Keyword(s):  
Room Temperature ◽  
Mass Density ◽  
Phase Region ◽  
Argon Atmosphere ◽  
Lattice Parameters ◽  
Crystalline Solid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Three Phase ◽  
Expansion Coefficients

Lattice parameters, coefficients of thermal expansion and mass density were determined by means of X-ray powder diffraction between 30 and 180?C (or 240?C - depending on samples' composition). Rietveld refinement was performed in order to obtain phases' lattice parameters at each temperature. The Panalytical X' Pert Pro MPD was used for room temperature X-ray diffraction experiments (RTXRD) with bulk samples. The aim was to identify the phases that were present in the sample, as well as, their lattice parameters. For some samples, powder high temperature X-ray diffraction measurements (HT-XRD) were also performed, under a vacuum of 10-5 mbar or an argon atmosphere. It was found that the lattice parameters of (Bi), (Sn) and (Zn) don't change with the composition, at room temperature, as expected since all samples belong to the three phase region. It was also concluded that (Bi) behaves like an isometric crystalline solid on the contrary of (Zn) that has different expansion coefficients for different crystallographic directions a (= b) and c.

scholarly journals Yttrium orthoferrite powder obtained by the mechanochemical synthesis

2017 ◽  
Vol 49 (3) ◽  
pp. 277-284 ◽  
Author(s):  
Zorica Lazarevic ◽  
Cedomir Jovalekic ◽  
Martina Gilic ◽  
Valentin Ivanovski ◽  
Ana Umicevic ◽  
...  
Keyword(s):  
Infrared Spectroscopy ◽  
Crystallite Size ◽  
Mechanochemical Synthesis ◽  
Ball Mill ◽  
Room Temperature ◽  
Average Crystallite Size ◽  
X Ray Diffraction ◽  
X Ray ◽  
Yttrium Orthoferrite ◽  
Raman And Infrared Spectroscopy

Yttrium orthoferrite (YFeO3) powder was prepared by a mechanochemical synthesis from a mixture of Y2O3 and ?-Fe2O3 powders in a planetary ball mill for 2.5 h. The obtained YFeO3 powder sample was characterized by X-ray diffraction (XRD), Raman and infrared spectroscopy. The average crystallite size calculated by the Scherrer equation was 12 nm. The M?ssbauer spectroscopy at room temperature confirms the superparamagnetic character of YFeO3 orthoferrite sample.

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