A Series of Enthalpy/Entropy-Driven Reversible Dissolution/Reorganization Equilibriums in the System of Cu(NO3)2–HL–GdX3–H2O (HL=5-methylpyrazine-2-carboxylic acid; X=Cl, Br, NO3, ClO4)

2014 ◽  
Vol 67 (11) ◽  
pp. 1679
Author(s):  
Sheng Zhang ◽  
Qi Yang ◽  
Xiangyu Liu ◽  
Gang Xie ◽  
Qing Wei ◽  
...  

Five coordination polymers, [Cu(L)2]n (1), {[Cu(L)(Cl)(H2O)]·H2O}2n (2), [KCu(L)(μ-Cl)2]n (3), [Cu(L)(Br)H2O]n (4), and {[Cu0.5(HL)(H2O)](NO3)·H2O}2n (5) (HL = 5-methylpyrazine-2-carboxylic acid) were obtained by reactions of a pyramidal CuII-containing ligand, {[Cu(L)2(H2O)]·3H2O}n (LCu), with Gd(ClO4)3·6H2O, GdCl3·6H2O, GdCl3·6H2O/KCl, GdBr3·6H2O, or Gd(NO3)3·6H2O in water. Structural analysis reveals that the structures of these compounds range from a 0D block to a 2D network with modification of the environment of the CuII ions compared with LCu. Interestingly, there occurred a series of reversible dissolution/reorganization equilibriums between the initial reactants and the final products 1–5, which were determined as enthalpy/entropy driven chemical equilibriums by single crystal X-ray diffraction and microcalorimetry. In addition, the thermal stability of 1–4 and the magnetic property of 2 are discussed.

Author(s):  
Jacky S. Bouanga Boudiombo ◽  
Ayesha Jacobs

Mefenamic acid (MA) formed solvates with 2-picoline (2PIC), 3-picoline (3PIC), 4-picoline (4PIC) and 3-chloropyridine (3CLPYR). The solvates crystallized in the space group P\bar 1 with the carboxylic acid of MA hydrogen-bonded to the nitrogen of the substituted pyridine. Tolfenamic acid (TFA) formed solvates with 2PIC and 3PIC, the crystal structures successfully solved in the space groupsP21/nandPbca, respectively. The fenamate conformation varied depending on the acid and the included solvent. Similarities were observed in the structures involving MA. The two solvate structures of TFA had different packing arrangements. Grinding and slurry experiments were also successful for the preparation of all of the compounds except MA·2PIC. Recrystallization, grinding and slurry investigations of MA and 2PIC yielded a polymorph; the structure was successfully solved inP21/n. Additionally, the thermal stability of the solvates was determined. Desolvation experiments were also performed and the resultant powders were analysed using powder X-ray diffraction.


2014 ◽  
Vol 67 (4) ◽  
pp. 603 ◽  
Author(s):  
Fang-Hua Zhao ◽  
Xin Zheng ◽  
Yun-Xia Che

Two new NiII complexes, [Ni2(AIP)2(bib)1.5]·4H2O (1) and [Ni(AIP)(bibp)(H2O)]·H2O (2) (AIP = 5-aminoisophthalic acid, bib = 1,4-bis(1-imidazolyl)benzene and bibp = 4,4′-bis(1-imidazolyl)biphenyl), have been synthesised hydrothermally and characterised by IR, elemental, single-crystal X-ray diffraction, and powder X-ray diffraction analyses. Topology analysis reveals that complex 1 is a 2D bilayer network, containing a new tetranodal (3,3,4,5)-connected (63)2(65·8)(68·82) configuration. Complex 2 exhibits a 2D→3D inclined polycatenate framework based on the 2D 44-sql net. In addition, the thermal stability of the two complexes was also studied.


2013 ◽  
Vol 66 (11) ◽  
pp. 1378 ◽  
Author(s):  
Wei Luo ◽  
Di Yao ◽  
Haiye Li ◽  
Fuping Huang ◽  
Qing Yu ◽  
...  

Eight different complexes with three positional isomeric dipyridyl ligands (3,3′-Hbpt, 3,4′-Hbpt, and 4,4′-Hbpt) (here, 3,3′-Hbpt = 1H-3,5-bis(3-pyridyl)-1,2,4-triazole, 3,4′-Hbpt = 1H-3-(3-pyridyl)-5-(4-pyridyl)-1,2,4-triazole, and 4,4′-Hbpt = 1H-3,5-bis(4-pyridyl)-1,2,4-triazole), as well as 3,3′,4,4′-biphenyltetracarboxylic acid (H4bptc), namely, {[M(bptc)0.5(3,3′-Hbpt)(H2O)2]·H2O}n (M = Co (1), M = Ni (2)), {[Zn2(bptc)(3,3′-Hbpt)2]·3H2O}n (3), [Co(bptc)0.5(3,4′-Hbpt)(H2O)]n (4), [Ni(bptc)0.5(3,4′-Hbpt)2(H2O)2]n (5), {[Cu(bptc)0.5(3,4′-Hbpt)(H2O)]·H2O}n (6), and {[M(bptc)0.5(4,4′-Hbpt)2(H2O)]·4H2O}n (M = Co (7), and Ni (8)) were synthesised and characterised by single-crystal X-ray diffraction. The crystallographic analysis demonstrates that bptc influences the MII (M = Co, Ni, Cu, and Zn) ions to form 2D layers, which are further connected via the isomeric bpt connectors, leading to many types of coordination polymers, such as 2D layers(for 1–3, 5), 3D four-connected nets with a short Schläfli symbol of (64.82) (for 4, 6), and 3D four-connected nets with a short Schläfli symbol of (64.82)(5.63.72)0.5 (for 7–8). This work demonstrates that the isomeric effects of the bpt ligands influence the construction of these frameworks. The thermal stability of complexes 1–6 was investigated.


Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 1101
Author(s):  
Anirban Karmakar ◽  
Anup Paul ◽  
Elia Pantanetti Sabatini ◽  
M. Fátima C. Guedes da Silva ◽  
Armando J. L. Pombeiro

The new coordination polymers (CPs) [Zn(μ-1κO1:1κO2-L)(H2O)2]n·n(H2O) (1) and [Cd(μ4-1κO1O2:2κN:3,4κO3-L)(H2O)]n·n(H2O) (2) are reported, being prepared by the solvothermal reactions of 5-{(pyren-4-ylmethyl)amino}isophthalic acid (H2L) with Zn(NO3)2.6H2O or Cd(NO3)2.4H2O, respectively. They were synthesized in a basic ethanolic medium or a DMF:H2O mixture, respectively. These compounds were characterized by single-crystal X-ray diffraction, FTIR spectroscopy, thermogravimetric and elemental analysis. The single-crystal X-ray diffraction analysis revealed that compound 1 is a one dimensional linear coordination polymer, whereas 2 presents a two dimensional network. In both compounds, the coordinating ligand (L2−) is twisted due to the rotation of the pyrene ring around the CH2-NH bond. In compound 1, the Zn(II) metal ion has a tetrahedral geometry, whereas, in 2, the dinuclear [Cd2(COO)2] moiety acts as a secondary building unit and the Cd(II) ion possesses a distorted octahedral geometry. Recently, several CPs have been explored for the cyanosilylation reaction under conventional conditions, but microwave-assisted cyanosilylation of aldehydes catalyzed by CPs has not yet been well studied. Thus, we have tested the solvent-free microwave-assisted cyanosilylation reactions of different aldehydes, with trimethylsilyl cyanide, using our synthesized compounds, which behave as highly active heterogeneous catalysts. The coordination polymer 1 is more effective than 2, conceivably due to the higher Lewis acidity of the Zn(II) than the Cd(II) center and to a higher accessibility of the metal centers in the former framework. We have also checked the heterogeneity and recyclability of these coordination polymers, showing that they remain active at least after four recyclings.


1998 ◽  
Vol 514 ◽  
Author(s):  
M. F. Wu ◽  
A. Vantomne ◽  
S. Hogg ◽  
H. Pattyn ◽  
G. Langouche ◽  
...  

ABSTRACTThe Nd-disilicide, which exists only in a tetragonal or an orthorhombic structure, cannot be grown epitaxially on a Si(111) substrate. However, by adding Y and using channeled ion beam synthesis, hexagonal Nd0.32Y0.68Si1.7 epilayers with lattice constant of aepi = 0.3915 nm and cepi = 0.4152 nm and with good crystalline quality (χmin of Nd and Y is 3.5% and 4.3 % respectively) are formed in a Si(111) substrate. This shows that the addition of Y to the Nd-Si system forces the latter into a hexagonal structure. The epilayer is stable up to 950 °C; annealing at 1000 °C results in partial transformation into other phases. The formation, the structure and the thermal stability of this ternary silicide have been studied using Rutherford backscattering/channeling, x-ray diffraction and transmission electron microscopy.


2021 ◽  
Vol 875 ◽  
pp. 116-120
Author(s):  
Muhammad Alamgir ◽  
Faizan Ali Ghauri ◽  
Waheed Qamar Khan ◽  
Sajawal Rasheed ◽  
Muhammad Sarfraz Nawaz ◽  
...  

In this study, the effect of SBR concentration (10 Phr, 20 Phr & 30 Phr ) on the thermal behavior of EPDM/SBR blends was studied. Thermogravimetric analysis (TGA) was used to check weight loss of samples as function of temperature by heating upto 600°C. X-ray diffraction (XRD) was performed to determine quality and % crystallinity of the elastomer blends. It was seen that % crystallinity improved with an increase in the content of SBR in EPDM/SBR blends. TGA revealed that the thermal stability of EPDM/SBR blends has improved by 17% than neat EPDM. Carbon nano-coatings produced by sputtering have no beneficial influence on thermal behaviour of elastomers.


2005 ◽  
Vol 60 (5) ◽  
pp. 505-510 ◽  
Author(s):  
Tong-Lai Zhang ◽  
Jiang-Chuang Song ◽  
Jian-Guo Zhang ◽  
Gui-Xia Ma ◽  
Kai-Bei Yu

Cobalt(II) and zinc(II) complexes of ethyl carbazate (ECZ), [Co(ECZ)3](NO3)2 and [Zn(ECZ)3] (NO3)2, were synthesized. Single crystals of these two compounds were grown from aqueous solutions using a slow evaporation method. Their structures have been determined by X-ray diffraction analysis. Both of them are monoclinic with space group P21/n. The complexes are further characterized by element analysis and IR measurements. Their thermal stabilities are studied by using TG-DTG, DSC techniques. When heated to 350 °C, only metal oxide was left for both complexes.


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