Solvothermal Synthesis and Crystal Structure Determination of Tris- (ethyleneamine-ammonium) Tetraselenoantimonat: Non-Centrosymmetry Mediated by an Extended Unusual N-H···N Hydrogen Bonded Network?

1998 ◽  
Vol 53 (10) ◽  
pp. 1144-1148 ◽  
Author(s):  
Frank Wendland ◽  
Christian Näther ◽  
Michael Schur ◽  
Wolfgang Bensch

AbstractThe title compound has been synthesized under solvothermal conditions by the reaction of elemental chromium, antimony and selenium in a solution of 40% 1,2-ethanediamine (en) in methanol. The crystal structure consists of tetrahedral SbSe43- anions which are connected by monoprotonated 1,2-ethanediamine (enH+) cations via N-H--Se hydrogen bonding. The enH+ cations are joined via strong N-H -N hydrogen bonds between the ammonium hydrogen and the amino nitrogen atom forming four distinct chains, each built up of three crystallographically independent enH+ cations. Two of these chains are running parallel to [100], the other two are parallel to [010]. Based on this arrangement different centrosymmetric or non-centrosymmetric hydrogen bonding patterns are possible, but only in one chain the sequence of NH2 and NH3+ groups was determined by X-ray diffraction

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Runmei Ding ◽  
Zixin He ◽  
Meilin Wang ◽  
Danian Tian ◽  
Peipei Cen

AbstractBased on 2-(4-pyridyl)-terephthalate (H2pta) and oxalate ligands, two new lanthanide-containing coordination polymers (CPs), [Tb(pta)(C2O4)0.5(H2O)2)]·2H2O (1) and [Sm(pta)(C2O4)0.5(H2O)2)]·2H2O (2), have been synthesized under solvothermal conditions. The structures of both 1 and 2 have been determined by single-crystal X-ray diffraction. Infrared, elemental analysis, powder X-ray diffraction and thermogravimetric analysis data are also presented. The crystals of 1 and 2 exhibit isostructural layer-like networks, crystallizing in the triclinic space group P$‾{1}$. The layers are further stabilized and associated into 3D architectures through hydrogen bonding. Remarkably, the CPs 1 and 2 exhibit excellent water stability and remarkable thermostability with thermal decomposition temperatures of more than 420 °C.


2000 ◽  
Vol 65 (8) ◽  
pp. 1317-1328 ◽  
Author(s):  
Alexandr Jegorov ◽  
Ladislav Cvak ◽  
Aleš Husek ◽  
Petr Šimek ◽  
Anna Heydová ◽  
...  

Acid-catalyzed degradation of cyclosporin A was studied in various solvents and products of reaction were monitored by HPLC. Identification of amino acids and their chirality were determined after hydrolysis and derivatization by GC-MS. Cyclosporin H was isolated as the principal product and its structure was determined by X-ray diffraction: Cyclosporin H- diethyl ether-water (1 : 0.5 : 1) crystallizes in the monoclinic space group I2 with a = 12.338(2) Å, b = 18.963(2) Å, c = 34.074(3) Å, β = 96.47(2)°, Z = 4, and V = 7 921.4(17) Å3.


1997 ◽  
Vol 52 (8) ◽  
pp. 901-905 ◽  
Author(s):  
Vera V Ponomareva ◽  
Victor V Skopenko ◽  
Konstantin V Domasevitch ◽  
Joachim Sieler ◽  
Thomas Gelbrich

Abstract The caesium hydrogen benzoylcyanoximate (L-) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [monoclinic, space group P21/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Å, β = 90.13(1)°, V = 3434.3(9) Å, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of Cs(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}-, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O - - - O ca. 2.456(5)Å]. The caesium atom deviates by 1.492(3) Å from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical “sunrise coordination” [Cs-O (ether) 3.040(9)-3.312(7) Å]. The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (Cs-O ca. 3.040(9), 3.312(7) Å; Cs-N ca. 3.469(5), 3.679(6) Å). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism.


2009 ◽  
Vol 64 (7) ◽  
pp. 821-825 ◽  
Author(s):  
Xiuhong Xu ◽  
Ling Zhang ◽  
Yi Zhang ◽  
Bin Qi ◽  
Fang Luo

The sandwich-type complex Na(H2O)6(C6H16O3N)2[Na2(H2O)7(C6H16O3N)]2[(Na(H2O)2)3- (Cu(H2O))3(BiW9O33)2]・14H2O (1) (C6H16O3N+ = protonated triethanolamine) has been synthesized and structurally characterized by single-crystal X-ray diffraction, IR spectroscopy and TG analysis. The basic framework of 1 is built from a sandwich-type [(Na(H2O)2)3- (Cu(H2O))3(BiW9O33)2]9− anion, two [Na2(H2O)7(C6H16O3N)]3+ cations, a free Na(H2O)6+ cation, and two free C6H16O3N+ units. In compound 1, the [(Na(H2O)2)3(Cu(H2O))3- (BiW9O33)2]9− anion links two bi-nuclear units [Na2(H2O)7(C6H16O3N)]3+ to form a [Na2- (H2O)7(C6H16O3N)]2[(Na(H2O)2)3(Cu(H2O))3(BiW9O33)2]3− cluster, and a new 3D supramolecular structure is further constructed by hydrogen bonding interactions among this cluster, the free Na(H2O)6+ cation, and the free C6H16O3N+ cations. Crystal data: Cu3Na8Bi2W18C24H150O121N4, monoclinic, C2/c, a = 14.5668(13), b = 23.0405(13), c = 37.412(2) Å , β = 91.569(10)° , Z = 4.


RSC Advances ◽  
2020 ◽  
Vol 10 (53) ◽  
pp. 31947-31960 ◽  
Author(s):  
Francisco Colmenero ◽  
Jakub Plášil ◽  
Vicente Timón ◽  
Jiří Čejka

The determination of the full crystal structure of the uranyl sulfate mineral uranopilite, including the positions of the H atoms in the corresponding unit cell, has not been feasible to date due to the poor quality of its X-ray diffraction pattern.


1992 ◽  
Vol 47 (4) ◽  
pp. 460-464 ◽  
Author(s):  
Klaus Brodersen ◽  
Jürgen Hofmann

The structure of bis(m-aminobenzonitrile)dimercury(I) dinitrate, [Hg2(m -NH2C6H4CN)2](NO3)2 has been determined by single crystal X-ray diffraction techniques and refined to an Rw-value of 0.022. The crystals are triclinic, space group P1 with a = 5.4878(1) Å, b = 8.4085(1) Å, c = 9.6062(1) Å, α = 92.599(3)°, β = 94.763(3)°, γ = 89.614(3)° and Z = 1.The Hg22+-ion [Hg-Hg 2.524(1) Å] is approximately axially coordinated to amino nitrogen atoms [Hg - N 2.209(4) Å, Hg - Hg - N 169.5(3)°]. Additional amino hydrogen bonds to oxygen are building chains along the b-axis containing units of L - Hg - Hg - L groups.


2001 ◽  
Vol 56 (6) ◽  
pp. 517-520 ◽  
Author(s):  
Alfonso Castiñeiras ◽  
Ricardo Domínguez ◽  
Leandro Bresolin ◽  
Jairo Bordinhão ◽  
Adaílton João Bortoluzzi ◽  
...  

AbstractA novel heptacoordinated thiosemicarbazonato lead(II) complex [Pb(4ML)(SCN)] (4ML = 2-Acetylpyridine-4N-methylthiosemicarbazonato) was synthesized and characterized by conventional methods (IR and elemental analysis) and single-crystal X-ray diffraction. [Pb(4ML)(SCN)] shows an unusual polymeric structure in which the lead atom is hexa-coordinate, the deprotonated thiosemicarbazone both chelates and bridges, and the thiocyanate group acts as bridge between lead(II)-thiosemicarbazonate fragments. There is hydrogen-bonding between the polymeric chains. The complex crystallizes in the triclinic space group P 1̅̅ with a = 7.461(2), b = 9.572(2), c = 11.235(2) Å, α = 66.51(3), β = 84.01(3), γ = 68.75(3)°, V = 685.1(2) Å3, Z = 2.


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