Komplexbildung und Metallextraktion mit heterocyclischen β-Dicarbonylverbindungen im Vergleich. Struktur von 3-Phenyl-4-benzoyl-isoxazol-5-on / Complex Formation and Metal Extraction with Heterocyclic β-Dicarbonyl Compounds as Comparison. Structure of 3-Phenyl-4-benzoyl-5-isoxazolone

1995 ◽  
Vol 50 (1) ◽  
pp. 37-42 ◽  
Author(s):  
Erhard Uhlemann ◽  
Alwin Friedrich ◽  
Gerald Hinsche ◽  
Wulfhard Mickler ◽  
Uwe Schilde

Acid constants and stability constants of nickel and zinc chelates with 2-thenoyltrifluoroacetone, dibenzoylmethane, 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone and 3-phenyl-4-benzoyl-5-isoxazolone were compared. The extraction of copper was studied. Thermoanalytic measurements were made using the ligands and their copper compounds in the solid state. The molecular structure of 3-phenyl-4-benzoyl-5-isoxazolone was determined by X-ray analysis. Crystal data: a = 874,7(2), b = 1959,2(7), c = 897,38(7) pm; β = 101,030(7)°; space group P 121/c 1; Z = 4; R = 0,043; 1920 observed, unique reflexions.

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2


1983 ◽  
Vol 36 (2) ◽  
pp. 253 ◽  
Author(s):  
AC McDonell ◽  
TW Hambley ◽  
MR Snow ◽  
AG Wedd

The salts Ph4As [ReO(SPh)4].MeCN and Ph4As [ReO(SePh)4] have been synthesized and characterized. The crystal and molecular structure of the thiolate compound has been determined by X-ray crystallography which reveals a square-pyramidal arrangement of ligand atoms around the central rhenium atom of the [ReO(SPh)4]- anion. Crystal data: a 9.756(4), b 18.171(3), c 25.684(4) �, space group P212121, Z 4.


1997 ◽  
Vol 52 (6) ◽  
pp. 693-695 ◽  
Author(s):  
Heike Hefele ◽  
Erhard Uhlemann ◽  
Frank Weller

A new binuclear vanadium( V) complex was synthesized by reaction of an aqueous oxovanadium(IV) sulfate solution with 2-(2′-hydroxyphenyl)-8-quinolinol dissolved in methanol. The molecular structure of the complex was determined by X-ray structure analysis. Crystal data: a = 10.004(3), b = 9.325(2), c = 15.089(3) Å; β = 91.95(2)°; space group P21/n, Z = 4.


1996 ◽  
Vol 74 (11) ◽  
pp. 2209-2216 ◽  
Author(s):  
Neil Burford ◽  
Charles L.B. Macdonald ◽  
Trenton M. Parks ◽  
Gang Wu ◽  
Borzena Borecka ◽  
...  

1,3-Dimethyldiaza-2-arsenanium tetrachlorogallate (crystal data: C5H12AsCl4GaN2, M = 386.61, orthorhombic, space group Pca21, a = 14.432(3) Å, b = 6.7580(14) Å, c = 13.905(3) Å, V = 1356.2(5) Å3) is synthesized by the routine chloride ion abstraction procedure from 2-chloro-1,3-dimethyldiaza-2-arsenane (crystal data: C5H12AsClN2, M = 210.54, monoclinic, space group P21/n, a = 7.206(1) Å, b = 9.650(1) Å, c = 13.021(2) Å, β = 99.61(2)°, V = 892.8(2) Å3). X-ray crystallographic studies of both compounds are described together with that for 2-chloro-1,3-dimethyldiaza-2-arsolidine (crystal data: C4H10AsClN2, M = 196.51, monoclinic, space group P21/n, a = 6.959(7) Å, b = 9.23(2) Å, c = 12.14(2) Å, β = 95.4(1)°, V = 777(4) Å3) providing useful structural comparisons. In contrast to the closely related arsolidinium salts, the diazarsenanium gallate exhibits a monomeric solid state structure. Rapid and quantitative cycloaddition reactions of the diazarsolidinium and diazarsenanium cations with 2,4-dimethylbutadiene give similar cycloadducts. The Diels–Alder type arsolidinium adduct is structurally characterized (crystal data: C10H20AsCl4GaN2, M = 454.73, orthorhombic, space group Pca21, a = 18.471(2) Å, b = 7.000(2) Å, c = 13.738(1) Å, V = 1776.2(8) Å3), and the related structure of the arsenanium cycloadduct is confirmed by 2D NMR. Key words: arsenium, cycloadditions, arsenanium, Diels–Alder, cyclochloroarsines.


2000 ◽  
Vol 55 (11) ◽  
pp. 1005-1010 ◽  
Author(s):  
Ulrich Jürgen Bildmann ◽  
Martin Winkler ◽  
Gerhard Müller Fachbereich

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.


1995 ◽  
Vol 10 (1) ◽  
pp. 2-6 ◽  
Author(s):  
N. R. Khasanova ◽  
A. V. Mironov ◽  
E. V. Antipov

The incommensurately modulated structure of Bi2Sr2Eu1.3Ce0.7Cu2O10.17, with a = 5.4752(4) Å, b = 5.4522(3) Å, c = 17.860(1) Å, Z = 2, was refined by the GJANA program [Gao et al., Acta Cryst. A 49, 141 (1993)] from X-ray powder data in C:C2mb: 111 four-dimensional space group (Rov = 0.064, Rm = 0.041, Rsat = 0.202, Rp = 0.049, Rwp = 0.065). Displacive modulation parameters of all cations and oxygen atoms in the Bi-layer were involved in the refinement. Obtained results including the modulation parameters are in agreement with those found for the similar phase Bi2Sr1.7Nd1.8Ce0.5Cu2O10+δ from single-crystal data [Mironov et al., J. Solid State Chem. 109, 74 (1994)].


Author(s):  
SVEND SIEVERTSEN ◽  
MORTEN WEIDEMANN ◽  
HEINER HÜCKSTÄDT ◽  
HEINER HOMBORG

Tetra(n-butyl)ammonium nitrite reacts with ‘dichlorophthalocyaninatoruthenium(III) acid’ to yield bis(tetra(n-butyl)ammonium) bisnitrophthalocyaninatoruthenate(II). It crystallizes monoclinic with crystal data: a = 15.114(4) Å, b = 22.34(3) Å, c = 18.206 (11) Å, β = 90.88(5)°; space group P1 21/n 1, Z = 4, and its X-ray crystal structure has been determined. Ru is located in the centre of the slightly distorted phthalocyaninate dianion, and is coordinated to two nitrite ions through their nitrogen (N) atoms in a staggered trans-configuration. The average Ru - N p ( Np pyrrolic N atoms) and Ru -N distance is 1.978(6) and 2.068(5) Å, respectively. The electrochemical and spectroscopic properties (IR, resonance Raman, UV/vis) of the compound are in full agreement with its molecular structure.


1978 ◽  
Vol 33 (7) ◽  
pp. 753-755 ◽  
Author(s):  
G. Struckmeier ◽  
J. Engel ◽  
U. Thewalt

Abstract The crystal and molecular structure of the title compound has been determined by X-ray diffraction. The compound possesses an (almost) planar Z configuration. The ions form ion pairs in the solid state: each bromide anion is connected via two hydrogen bonds with a cation. The crystal data are: space group P21/n with Z = 4; cell dimensions a = 14.097(2), b = 11.591(2), c = 14.133(3) Å, β = 106,22(2)°.


2014 ◽  
Vol 38 (1) ◽  
pp. 97-101
Author(s):  
Jagodish C Sarker ◽  
Md Saifur Rahman ◽  
Shariff E Kabir ◽  
Tasneem A Siddiquee

The solid-state molecular structure determination of the bimetallic osmium-tin compound [(?-H)Os2(CO)4(SnPh3)2(?-HSnPh2)(?-dppf)] (1) was carried out to determine the relative orientationof the coordinated ligands. Compound 1 crystallizes in the monoclinic space group P 21/c with a =22.366(7), b = 14.217(4), c = 25.213(8) Å, ? = 98.865(7)°, Z = 8 and V = 7921(4) Å3. It is a 34-electron bimetallic cluster with the Os-Os edge concomitantly bridged by a dppf and two HSnPh2 ligands DOI: http://dx.doi.org/10.3329/jbas.v38i1.20218 Journal of Bangladesh Academy of Sciences, Vol. 38, No. 1, 97-101, 2014


1996 ◽  
Vol 51 (9) ◽  
pp. 1240-1244 ◽  
Author(s):  
Heide Kraudelt ◽  
Uwe Schilde ◽  
Heike Hefele ◽  
Eberhard Ludwig ◽  
Erhard Ludwig

By reaction of 1-phenyl-3-methyl-4-benzoyl-pyrazol-5-one with benzoylhydrazine the tridentate diacidic ligand 4-[1-(N′-benzoylhydrazino)-1-phenyl-m ethylidene]-3-m ethyl-lphenyl-1-pyrazol-5-one (H2L) is formed which gives complexes ML2 with tetravalent titanium and vanadium ions. The ligand and its complexes were characterized by mass spectroscopy. The vanadium(IV) complex can be oxidised and reduced electrochemicallv. The chemical bonding in the titanium(IV) complex and in the ligand was studied by IR and 13C NMR spectroscopy.The molecular structure of 4-[1-(N′-benzoylhydrazino)-1-phenyl-methylidenel-3-m ethyl-lphenyl- pyrazol-5-one was determined by X-ray analysis. Crystal data: a = 9.159(3) Å, b = 11.014(4) Å, c = 11.136(5) Å, a = 90.11 (2)°, β = 101.84(3)°, γ = 113.01 (2)°; space group P1̄, Z = 2.


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