scholarly journals A phase transition caught in mid-course: independent and concomitant analyses of the monoclinic and triclinic structures of ( n Bu4N)[Co(orotate)2(bipy)]·3H2O

2017 ◽  
Vol 73 (9) ◽  
pp. 731-742 ◽  
Author(s):  
Miguel Castro ◽  
Larry R. Falvello ◽  
Elena Forcén-Vázquez ◽  
Pablo Guerra ◽  
Nuha A. Al-Kenany ◽  
...  
Keyword(s):  
Phase Transition ◽  
Single Crystal ◽  
Room Temperature ◽  
Structural Changes ◽  
Energy Content ◽  
Single Crystal Diffraction ◽  
Two Phase ◽  
Reverse Transition ◽  
Crystal Phase Transition

The preparation and characterization of the n Bu4N+ salts of two bis-orotate(2−) complexes of cobalt, namely bis(tetra-n-butylammonium) diaquabis(2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-ide-6-carboxylato-κ2 N 1,O 6)cobalt(II) 1.8-hydrate, (C16H36N)2[Co(C5H2N2O4)2(H2O)2]·1.8H2O, (1), and tetra-n-butylammonium (2,2′-bipyridine-κ2 N,N′)bis(2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-ide-6-carboxylato-κ2 N 1,O 6)cobalt(III) trihydrate, (C16H36N)[Co(C5H2N2O4)2(C10H8N2)]·3H2O, (2), are reported. The CoIII complex, (2), which is monoclinic at room temperature, presents a conservative single-crystal-to-single-crystal phase transition below 200 K, producing a triclinic twin. The transition, which involves a conformational change in one of the n Bu groups of the cation, is reversible and can be cycled. Both end phases have been characterized structurally and the system was also characterized structurally in a two-phase intermediate state, using single-crystal diffraction techniques, with both the monoclinic and triclinic phases present. Thermal analysis allows a rough estimate of the small energy content, viz. 0.25 kJ mol−1, for both the monoclinic-to-triclinic transformation and the reverse transition, in agreement with the nature of the structural changes involving only the n Bu4N+ cation.

Single-crystal to single-crystal phase transition of cucurbit[5]uril hydrochloride hydrates: large water-filled channels transforming to layers of unusual stability

2008 ◽  
pp. 4927 ◽  
Author(s):  
David Bardelang ◽  
Konstantin A. Udachin ◽  
Roberto Anedda ◽  
Igor Moudrakovski ◽  
Donald M. Leek ◽  
...  
Keyword(s):  
Phase Transition ◽  
Single Crystal ◽  
Crystal Phase ◽  
Crystal Phase Transition ◽  
Large Water

Thermo-Optical Properties of Perfluorinated Sulfonic Acid Membranes: An Investigation of Hydration Based on Absorption Spectra

2017 ◽  
Vol 71 (11) ◽  
pp. 2504-2511 ◽  
Author(s):  
Daniele T. Dias ◽  
Guy Lopes ◽  
Tales Ferreira ◽  
Ivanir L. Oliveira ◽  
Caroline D. Rosa
Keyword(s):  
Sulfonic Acid ◽  
Room Temperature ◽  
Water Retention ◽  
Structural Changes ◽  
Optical Characterization ◽  
Scanning Calorimetry ◽  
Experimental Procedure ◽  
Nafion Membranes ◽  
Perfluorinated Sulfonic Acid

The Nafion membranes are widely used in electrochemical applications such as fuel cells, chlor-alkali cells, and actuators–sensors. In this work, the thermal-optical characterization of Nafion in acid form was performed by photoacoustic spectroscopy, thermogravimetry, and differential scanning calorimetry. In the experimental procedure three distinct hydration levels were considered: (1) pristine membrane (λ ≅ H2O/–SO3H ≅ 5.6); (2) swelling process (λ ≅ 17.4); and (3) drying at controlled room temperature after swelling process (λ ≅ 6.5). The discovered behaviors showed significant irreversible structural changes induced by water retention in the membrane. These structural changes depend on the water population present in the clusters and also affect the directional thermal diffusivity of the membrane irreversibly.

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

RBS/Channeling Characterization of Ba Implanted Mg

1992 ◽  
Vol 279 ◽  
Author(s):  
R. C. Da Silva ◽  
Th. Hauser ◽  
A. A. Melo ◽  
J. C. Soares ◽  
M. F. Da Silva ◽  
...  
Keyword(s):  
Melting Point ◽  
Single Crystal ◽  
Room Temperature ◽  
Surface Segregation

ABSTRACTThe behaviour of 300 keV Ba ions implanted at room temperature with doses between 1015 and 1017 cm−2 in Mg single crystal and foils was investigated. The results show that the Ba ions do not occupy substitutions sites in Mg, either after the implantation or the annealing treatments. However, pronounced migration of Ba to the surface is observed above 380 °C. The remaining fraction overlaps with the aa-implanted distribution and forms small precipitates. This behaviour is not correlated with the recovery of the Mg lattice which is already complete at about 250 °C. The surface segregation of Ba delays the evaporation of Mg to temperatures near the melting point.

scholarly journals Mixed Ca/Sr salt forms of salicylic acid: tuning structure and aqueous solubility

2018 ◽  
Vol 74 (2) ◽  
pp. 131-138 ◽  
Author(s):  
Pamela Allan ◽  
Jean-Baptiste Arlin ◽  
Alan R. Kennedy ◽  
Aiden Walls
Keyword(s):  
Salicylic Acid ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Structural Feature ◽  
Structural Changes ◽  
Aqueous Solubility ◽  
Single Crystal Diffraction ◽  
One Dimensional ◽  
The One ◽  
Salt Forms

Ten isostructural single-crystal diffraction studies of mixed cation Ca/Sr salt forms of the salicylate anion are presented, namely catena-poly[[diaquacalcium(II)/strontium(II)]-bis(μ2-2-hydroxybenzoato)], [Ca1–x Sr x (C7H5O3)2(H2O)2] n , where x = 0, 0.041, 0.083, 0.165, 0.306, 0.529, 0.632, 0.789, 0.835 and 1. The structure of an isostructural Sr/Ba species, namely catena-poly[[diaquastrontium(II)/barium(II)]-bis(μ2-2-hydroxybenzoato)], [Sr0.729Ba0.271(C7H5O3)2(H2O)2], is also described. The Ca/Sr structures form a series where, with increasing Sr content, the unit cell expands in both the crystallographic a and c directions (by 1.80 and 3.18%, respectively), but contracts slightly in the b direction (−0.31%). The largest percentage structural expansion lies parallel to the direction of propagation of the one-dimensional coordination polymer that is the primary structural feature. This structural expansion is thus associated with increased M—O distances. Aqueous solubility measurements show that solubility generally increases with increasing Sr content. Thus, tuning the composition of these mixed counter-ion salt forms leads to systematic structural changes and allows solubility to be tuned to values between those for the pure Ca and Sr species.

An irreversible phase transition in 1-n-butylindeno[2,1-c]pyran-3,9-dione

2012 ◽  
Vol 68 (10) ◽  
pp. o413-o416 ◽  
Author(s):  
Andrei S. Batsanov ◽  
Judith A. K. Howard ◽  
Na Wu ◽  
Zhen Yang ◽  
Todd B. Marder
Keyword(s):  
Phase Transition ◽  
Ambient Temperature ◽  
Single Crystal ◽  
Title Compound ◽  
Room Temperature ◽  
Side Chain ◽  
Compound C ◽  
Planar Conformation ◽  
Triclinic Phase ◽  
Out Of Plane

At ambient temperature, the title compound, C16H14O3, is triclinic, with then-butyl side chain disordered in an out-of-plane orientation. On cooling below 240 K, it converts into a different triclinic phase with an ordered planar conformation and denser packing, which is retained on warming to room temperature. The transition (occasionally) proceeds from single crystal to single crystal.

scholarly journals Applications with a brighter X-ray source and new detectors from Agilent

2014 ◽  
Vol 70 (a1) ◽  
pp. C1734-C1734
Author(s):  
Zoltan Gal ◽  
Tadeusz Skarzynski ◽  
Fraser White ◽  
Oliver Presly ◽  
Adrian Jones ◽  
...  
Keyword(s):  
Data Quality ◽  
Single Crystal ◽  
Measurement System ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Vacuum Technology ◽  
Intelligent Measurement ◽  
Wide Range

Agilent Technologies develop and supply X-ray systems for single-crystal diffraction research, including the SuperNova; a compact, highly reliable and very low maintenance instrument providing X-ray data of the highest quality; and the PX Scanner for testing and characterization of protein crystals in their original crystallization drops (in-situ). The SuperNova and PX Scanner are constantly improving, with recent enhancements including a new range of detectors using an Intelligent Measurement System. The Eos S2, Atlas S2 and Titan S2 detector range employs a smart sensitivity control of the electronic gain and is capable of instantaneously switching its binning modes thus providing unprecedented flexibility in tuning every exposure to provide the highest data quality for a wide range of experiments. We have also developed a completely new micro-focus X-ray source based on Gradient Vacuum technology, with novel filament and target designs. This novel source is an integral part of the new Agilent GV1000 X-ray diffractometer, which has been designed for applications that require even higher brightness of the X-ray beam.

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