Synthesis and Structure of a Novel Silver(I) Perchlorate 2,2′:6′,2″-Terpyridine Adduct Solvated With Acetonitrile

1994 ◽  
Vol 47 (8) ◽  
pp. 1545 ◽  
Author(s):  
S Binsilong ◽  
JD Kildea ◽  
WC Patalinghug ◽  
BW Skelton ◽  
AH White

Recrystallization of an equimolar mixture of silver(I) perchlorate and 2,2′:6′,2″-terpyridine ( terpy ) from acetonitrile solution yields the golden yellow crystalline adduct shown by a room-temperature single-crystal X-ray study to be [Ag3( terpy )4][( MeCN )Ag( terpy )](ClO4)4. Crystals are triclinic, Pī , a 21.48(1), b 14.525(7), c 13.506(8) Ǻ, α 68.50(4), β 80.71(4), γ 81.66(4)°, Z 2 formula units; R was 0.045 for 9681 'observed' reflections. The complex helical cation is quasi- centrosymmetric with a collinear Ag3 array. The environment of the central silver atom is planar four-coordinate, two short Ag-N distances [(2.198(5), 2.188(5)Ǻ] arising from the nitrogen atoms of outer rings of a pair of twisted terpy ligands ; the other two sites are occupied by the nitrogen atoms of the central terpy rings which bifurcate to the other silver atoms [Ag(central)-N(central) 2.624(5), 2.818(5)Ǻ; Ag(outer)-N(central) 2.704(4), 2.640(4)Ǻ], which are also coordinated by the outer ring nitrogen of the two ligands [Ag-N, 2.266(5), 2.304(4) Ǻ]. Coplanar with the latter, each outer silver atom has a further tridentate terpy coordinated [Ag-N(central) 2.362(4), 2.381(4)Ǻ; Ag-N(outer) 2.403(6)-2.573(5)Ǻ]. The [( MeCN )Ag( terpy )]+ species is also quasi-planar, Ag- NCMe being 2.174(7)Ǻ, opposed to the central ring nitrogen [2.331(5)Ǻ; Ag-N(outer) being 2.399(7), 2.433(7)Ǻ].

2003 ◽  
Vol 56 (7) ◽  
pp. 718
Author(s):  
A. Hamid bin Othman ◽  
Brian W. Skelton ◽  
Allan H. White

A room-temperature single-crystal X-ray structure determination of the 1 : 1 adduct of silver(I) 2-hydroxy-3,5-dinitrobenzoate/triphenyl-phosphine (AgL/PPh3) was recorded, showing it to be a binuclear centrosymmetric system with the silver atoms bridged by one of the carboxy oxygen atoms of each ligand, [(PPh3)Ag(μ-O)2Ag(PPh3)] as in the parent acetate; the phenolic oxygen, retaining its protonation, is hydrogen bonded within the ligand to the other feebly chelating carboxylate oxygen.


2013 ◽  
Vol 717 ◽  
pp. 113-116
Author(s):  
Sani Klinsanit ◽  
Itsara Srithanachai ◽  
Surada Ueamanapong ◽  
Sunya Khunkhao ◽  
Budsara Nararug ◽  
...  

The effect of soft X-ray irradiation to the Schottky diode properties was analyzed in this paper. The built-in voltage, leakage current, and work function of Schottky diode were investigated. The current-voltage characteristics of the Schottky diode are measured at room temperature. After irradiation at 70 keV for 55 seconds the forward current and leakage current are increase slightly. On the other hand, the built-in voltage is decrease from the initial value about 0.12 V. Consequently, this method can cause the Schottky diode has low power consumption. The results show that soft X-ray can improve the characteristics of Schottky diode.


1998 ◽  
Vol 51 (8) ◽  
pp. 785 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Brian W. Skelton ◽  
Allan H. White

Room-temperature single-crystal X-ray structure determinations are recorded for a number of Group 2 4-nitrophenoxide acid salts, variously hydrated M(4-np)2.x(4-npH).yH2O. Ca(4-np)2.2(4-npH).8H2O is monoclinic, P 21/n, a 30·52(1), b 10·027(1), c 23·65(2) Å, β 116·3(5)°, Z = 8, conventional R on |F| being 0·058 for No 5092 independent ‘observed’ (I > 3s(I)) reflections. Sr(4-np)2.2(4-npH).8H2O, based on a subcell of the former, is monoclinic, P 21/c, a 15·576(5), b10·081(6), c 24·20(2) Å, β 117·99(5)° , Z = 4, R 0·054 for No 2908. Ba(4-np)2.2(4-npH).4H2O is orthorhombic, Fdd2, a 28·01(1), b 19·90(1), c 10·692(7)Å, Z = 8, R 0·028 for No 1967. The strontium array (and that of the calcium salt developed from it) may be represented as [(H2O)6Sr(4-npH.4-np)] (4-npH.4-np), a neutral ligand being unsymmetrically chelated to the strontium through the nitro group, with a quasi-parallel counter ion hydrogen-bonded to it by phenoxide confrontation. The other two 4-np residues make up a similar phenoxide-confronting pair (4-npH.4-np), the hydrogen being more intimately associated with one moiety. The barium salt is also an interesting array: the 10-coordinate barium lies on a crystallographic 2 axis, in an environment of two pairs of symmetry-related nitro-chelating ligand anions, and a pair of nitro-O coordinating neutral 4-npH ligands; the whole [(H2O)4Ba(4-np)2(4-npH)2] array may be envisaged as a single neutral (super)molecule. Hydrogen bonds between confronting phenoxides of the neutral 4-npH components of the parent and the 4-np- components of neighbouring molecules link the whole into a three-dimensional array.


2007 ◽  
Vol 546-549 ◽  
pp. 301-304
Author(s):  
Wei Qiu ◽  
En Hou Han ◽  
Lu Liu

Addition of RE elements to Al-containing Mg alloys can improve properties of Mg alloys at elevated temperatures. In the present investigation, hot-extruded AZ31+x%Nd. (x=0.1,0.3,0.6and1.0 wt%) wrought Mg alloy were prepared .The effects of Nd on microstructures and mechanical properties at room temperature of new alloy were investigated. The investigation found that Nd can bring about two kind of precipitation phases . One is AlNd phase, the other is AlNdMn phase, which were identified as Al11Nd3 and Al8NdMn4 by X-ray diffraction and TEM.


1993 ◽  
Vol 48 (10) ◽  
pp. 1360-1364
Author(s):  
Michel Mégnamisi-Bélombé ◽  
Irene Jokwi ◽  
Emmanuel Ngameni ◽  
Robert Roux ◽  
Bernhard Nuber

The structure of the cobaloximatic acid, hydro-trans-diiodobis(ethanedioximato(1-)-N,N′)cobaltate(III), has been determined by X-ray diffraction. Crystal data: C4H7CoI2N4O4, Mr = 487.87; monoclinic space group P21/a (C2h5 ); a = 10.795(7), b = 9.003(7), c = 11.881(6) Å; β = 97.29(6)°; V = 1145.35 Å3; Z = 4; dc = 2.83 Mg m-3. Rw (R) = 3.6 (3.9)% for 3064 observed independent reflections and 148 parameters. The coordination geometry around CoIII is a distorted (4 + 2) octahedron of four chelating equatorial N atoms and two apical iodides. The compound is most adequately formulated as a monovalent strong acid: H(Co(GH)2I2) (GH- = ethanedioximate or glyoximate). The H atoms of the oxime groups are involved in the usual intramolecular, as well as in much stronger intermolecular O-H-O bridgings (O ••• Ointramol = 2.613-2.631, O ••• Ointramol = 2.454 A). The “acidic” H atom of each molecule participates in the intermolecular bridging which extends throughout the structure, and propagates nearly parallel to the [101] crystallographic direction. The redox properties of the present compound were examined by cyclic voltammetry in acetonitrile solution at room temperature. Redox waves attributed to the reduction of CoIII and to the oxidation of I- were observed, along with a wave which may be linked to the reduction of the “acidic” proton


2009 ◽  
Vol 152-153 ◽  
pp. 79-84 ◽  
Author(s):  
Joan Josep Suñol ◽  
L. Escoda ◽  
C. García ◽  
V.M. Prida ◽  
Victor Vega ◽  
...  

Glass-coated Cu-Mn-Ga microwires were fabricated by Taylor-Ulitovsky technique. By means of energy dispersive spectroscopy microanalysis, an average alloy composition of Cu56Ga28Mn16 was determined. The temperature dependence of magnetization measured at a low magnetic field showed the coexistence of two ferromagnetic phases. The Curie temperature of one phase is 125 K and above room temperature for the other one. X-ray diffraction at room temperature and at 100 K reflects the presence of the same three crystalline phases corresponding to the cubic B2 Cu-Mn-Ga structure as a main phase and the minor phases of fcc Cu rich solid solution with Mn and Ga and the monoclinic CuO.


X-ray measurements recently carried out by the author on the lattice expansion of silver and quartz showed that the coefficients of thermal expansion, over the ranges investigated, are the same as those observed for the specimen as a whole using optical methods. Goetz and Hergenrother, on the other hand, from X-ray measurements on the coefficients of thermal expansion of single crystals of bismuth, claimed to have found a large difference between values obtained by the two methods of measurement. A possible explanatiion of this that their accuracy is not sufficient to establish definitely the deviation of the X-ray measurements from the optical expansion curve. The author has since made X-ray measurements on the expansion of the bismuth lattice from room temperature to just below the melting point, and finds no evidence of such a discrepancy as Goetz and Hergenrother record.


1996 ◽  
Vol 51 (1) ◽  
pp. 127-132 ◽  
Author(s):  
Stefan Horstmann ◽  
Wolfgang Schnick

Abstract [P(NH2)4]Cl has been prepared by ammonolysis of phosphorus pentachloride in liquid ammonia. The product was purified by reacting the byproduct, ammonium chloride, with diethylamine and removing the diethylamine hydrochloride. Suitable single crystals were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. The crystal structure of [P(NH2)4]Cl has been determined by single crystal X-ray methods (Pbcn, a = 470.8(2), b = 1622.3(3), c = 756.3(2) pm, Z = 4). In the solid, [P(NH2)4]+ and Cl- ions are found, resembling a TlI-analogous structure. The N-H···Cl distances indicate N-H···Cl hydrogen bonding interactions. The distortion of the P-N sceleton of the cation and the very short P-NH2 distances (mean value: 161.2 pm) have been confirmed by ab initio calculations, which show a generalized anomeric effect of the electron pairs at nitrogen and pπdπ bonding.


2017 ◽  
Vol 865 ◽  
pp. 25-29 ◽  
Author(s):  
Yun Gao Cai ◽  
Xin Qi Li

Various sizes SiO2 colloidal particles in the size range of 260-950 nm were synthesized by the stöber method by adjusting the amount of ammonia from 9.0 ml to 3.0 ml while keeping 20.0 ml tetraethyl orthosilicate (TEOS), 125.0 ml ethanol, 6.0 ml ammonia and 18.0 ml distilled water fixed. In addition, X-ray diffraction (XRD) and scanning electron microscopy (SEM) were employed to analyze the crystallinity and morphology of the synthesized SiO2 colloidal particles; the XRD result show that the SiO2 colloidal particles are amorphous at room temperature; the SEM results demonstrated that the amount of ammonia could have significant effects on the size, size distribution and sphericity of the SiO2 colloidal particles. SiO2 colloidal particles were resulted with good monodispersity when the amount of ammonia was in the range of 6.0-90 ml, while SiO2 colloidal particles with double size distribution were obtained when the range is 3.0-4.5 ml; on the other hand, SiO2 spheres were resulted with good sphericity when the ammonia is in the range of 6.0-7.5 ml.


1982 ◽  
Vol 21 ◽  
Author(s):  
J.M. Launay ◽  
J.Y. Laval ◽  
A. Gibaud ◽  
A. Bulou ◽  
J. Nouet

ABSTRACTIt is shown that the detailed investigation of an irreversible SPT implies the combination of X-ray, neutron and electron diffraction data. This diffraction analysis is applied to K Al F4 and Rb Al F4. There is a good agreement between the three diffraction techniques in the case of Rb Al F4 where the SPT is reversible. On the other hand, for K Al F4 room temperature quadratic phase, electron diffraction exhibits exta spots which are not evidenced by X-ray and neutron diffraction. Finally the assumption of an orthorombic lattice from neutron scattering for the low temperature phase is consistant with electron diffraction results.


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