Geometrische Isomerie bei bindungsisomeren Hexakis(thiocyanatoisothiocyanato)osmaten(III) / Geometrie Isomerism of Bond Isomerie Hexakis(thiocyanatoisothiocyanato)osmates (III)

1980 ◽  
Vol 35 (8) ◽  
pp. 994-999 ◽  
Author(s):  
G. Peters ◽  
W. Preetz
Keyword(s):  
Ion Exchange ◽  
Raman Spectra ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Geometric Isomers ◽  
Complex Ions ◽  
Diethylaminoethyl Cellulose ◽  
Ir And Raman ◽  
Bond Isomers ◽  
Reflux Temperature

Abstract From the system of isomeric complex ions [Os(NCS)n(SCN)6-n]3-, 9 of 10 possible species, n = 1-6, are isolated, including for n = 2, 3, 4 the first representatives of pure geometric bond isomers. By reaction of K2[OsCl6] with aqueous KSCN solution at reflux temperature, trans(mer)-complexes, and on treatment at 60 °C exclusively cis(fac)- complexes are formed. By ion exchange chromatography on diethylaminoethyl-cellulose columns, from mixtures of pairs of geometric isomers the pure trans(mer)-compounds are enriched in front, the cis(fac)-species at the end of the zones. Characterization and assignment of the configuration of the geometric isomers is based upon the reproducible differences in the IR and Raman spectra.

scholarly journals Darstellung von trans-[PtCl4Br2] 2 -und [PtCl5Br] 2- durch oxidative Addition an [PtCl4]2-/Preparation of trans-[PtCl4Br2] 2--and [PtCl5Br] 2 -by Oxidative Addition to [PtCl4]2-

1983 ◽  
Vol 38 (4) ◽  
pp. 442-445 ◽  
Author(s):  
W. Preetz ◽  
G. Rimkus
Keyword(s):  
Ion Exchange ◽  
Raman Spectra ◽  
Vibrational Spectra ◽  
Oxidative Addition ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Mixed Ligand ◽  
Diethylaminoethyl Cellulose ◽  
Ir And Raman ◽  
Stereospecific Reaction

Abstract The oxidative addition of Br2 to [PtCl4]2-in HBr yields almost pure trans-[PtCl4Br2]2-, in HCl nearly pure [PtCl5Br]2-, and in CH2Cl2 by a quantitative and stereospecific reaction completely pure trans-[PtCl4Br2]2-. This is confirmed by ion exchange chromatography on diethylaminoethyl cellulose and by analysis of the vibrational spectra in comparison with the IR and Raman spectra of the well-known species of the series [PtClnBr6-n]2- , n = 0-6. The literature concerning trans-[PtCl4Br2]2- and other mixed ligand complexes is critically discussed.

Darstellung, 11 B-NMR- und Schwingungsspektren von cis-Dinitrotetrahydro-closo-hexaborat(2–), cis-[B6H4( NO2)2]2- sowie Kristallstruktur von cis-Cs2[B6H4(NO2)2] / Preparation, 11 B NMR and Vibrational Spectra of cis-Dinitrotetrahydro-closo-hexaborate(2–),cis-[B6H4(NO2)2]2-, and the Crystal Structure of cis-Cs2[B6H4(NO2)2]

1995 ◽  
Vol 50 (7) ◽  
pp. 1030-1034 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Dichloromethane Solution ◽  
X Ray ◽  
Diethylaminoethyl Cellulose ◽  
Ir And Raman

By electrochemical oxidation of [B6H6,]2 in the presence of nitrite ions and of the base DBU in dichloromethane solution apart from [B6H5 (NO2)]2- and [B6H5(NO)B 6H5]3- the dinitro anion cis-[B6H4( NO2)2]2- is formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of the Cs salt has been determined from single crystal X-ray diffraction analyses. cis-Cs2[B6H4 ( NO2)2] is tetragonal, space group P4̄21 m with a = 10.0656(4), c = 11.0127(13) Å. The 11B NMR spectrum is consistent with a disubstituted octahedral B6 cage with local C2v symmetry. The IR and Raman spectra exhibit characteristic NO2, B - H and B6 vibrations.

Bindungsisomere Hexakis(thiocyanato-isothiocyanato)osmate(III) /Bond-Isomeric Hexakis(thiocyanato-isothiocyanato)osmates(III)

1979 ◽  
Vol 34 (9) ◽  
pp. 1243-1248 ◽  
Author(s):  
W. Preetz ◽  
G. Peters
Keyword(s):  
Reaction Times ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Individual Species ◽  
Diethylaminoethyl Cellulose ◽  
Characteristic Group ◽  
Intensity Ratios ◽  
The Individual ◽  
Ir And Raman ◽  
Bond Isomers

AbstractOn treatment of K2[OsX6], X = Cl, Br, I with KSCN in aqueous solution mixtures of bond-isomeric hexakis(thiocyanato-isothiocyanato)complexes, [Os(NCS)n(SCN)6-n] 3-, n = 1-6, are formed. At low temperatures and short reaction times species with more S-bonded, after longer boiling species with more N-bonded ligands are preferred, indicating the increase of thermodynamic stability with growing n-values. The isolation of the pure bond isomers n = 1-6, is achieved by ion exchange chromatography on diethylaminoethyl-cellulose. The assignment of the individual species is based upon the intensity ratios of characteristic group frequencies in the IR and Raman spectra. The UV-VIS spectra also show significant shifts within the series.

Darstellung von Mononitropentahydrohexaborat(2-) und Kristallstruktur von M2[B6H5(NO2)], M = K, Cs / Preparation of Mononitropentahydrohexaborate(2—) and Crystal Structure of M2[B6H5(NO2)], M = K, Cs

1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.

Darstellung und Schwingungsspektren der 35Cl/37Cl-markierten Fluoro-Chloro-Platinate(IV) / Preparation and Vibrational Spectra of 35Cl/37Cl Labelled Fluoro-Chloro-Platinates(IV)

1989 ◽  
Vol 44 (6) ◽  
pp. 619-626 ◽  
Author(s):  
P. Erlhöfer ◽  
W. Preetz
Keyword(s):  
Low Temperature ◽  
Mutual Exclusion ◽  
Deae Cellulose ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Vibrational Modes ◽  
Geometric Isomers ◽  
Deformation Bands ◽  
Isotopic Shifts ◽  
Ir And Raman

All components of the two series Cs2[PtF„35Cl6-n] and Cs2[PtFn37Cl6-n], including the pairs of geometric isomers for n = 2,3, 4, have been prepared and isolated by ion exchange chromatography on DEAE cellulose. The highly resolved low temperature (80 K) IR and Raman spectra of the pure isotopomers show distinctive isotopic shifts for different vibrational modes up to 10 cm-1. The excellent agreement of the observed values with Teller-Redlich calculations verifies the assignment of all stretching and especially of the narrow deformation bands. For transcomplexes containing 35Cl-Pt-37Cl axes, the lowered symmetry affects the restriction of the rule of mutual exclusion

scholarly journals Darstellung von μ-Nitroso-bis(pentahydro-closo-hexaborat)(3-) und Kristallstruktur von Cs3[B6H5(NO)B6H5] / Preparation of μ-nitroso-bis(pentahydro-closo-hexaborate)(3-) and crystal structure of Cs3[B6H5(NO)B6H5]

1994 ◽  
Vol 49 (9) ◽  
pp. 1263-1266 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and of the base DBU in dichlorom ethane solution the μ-nitroso-bis(pentahydrohexaborate) [B6H5(NO)B6H5]3- ion is formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of the Cs salt has been determined from single crystal X-ray diffraction analysis. Cs3[B6H5(NO)B6H5] is orthorhombic, space group Pnma with a = 16.2303(13), b = 12.245(6), c = 25.444(2) Å. The unit cell contains three crystallographically independent anions with nearly C2v symmetry but differently distorted B6 cages

Darstellung und Schwingungsspektren von Fluoro-Chloro-Iridaten(IV) einschließlich der Stereoisomeren / Preparation and Vibrational Spectra of Fluoro-Chloro-Iridates(IV) Including Stereoisomers

1984 ◽  
Vol 39 (9) ◽  
pp. 1185-1192 ◽  
Author(s):  
D. Tensfeldt ◽  
W. Preetz
Keyword(s):  
Ion Exchange ◽  
Vibrational Spectra ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Mixed Ligand ◽  
Trans Isomers ◽  
Trans Effect ◽  
Diethylaminoethyl Cellulose ◽  
Stretching Vibration ◽  
Point Groups

The reaction of [IrCl6]2- with BrF3 generates the mixed complexes [IrFnCl6-n]2-, n = 1-5, of which the species with n = 2, 3, 4 are ds-configurated. Due to the stronger trans-effect of Cl as compared to F on treatment of [IrF5Cl]2- and cis-[IrF4Cl2]2- with SOCl2 the trans-isomers are formed stereospecifically. The pure fluoro-chloro-iridates(IV) are separated by ion exchange chromatography on diethylaminoethyl-cellulose. The vibrational spectra of the mixed ligand complexes are completely assigned according to point groups D4h, C4v, C3v, and C2v. The IrCl stretching vibration of [IrF5Cl]2- is split by the isotopes 35C1 and 37Cl, showing two well resolved sharp Raman lines at 361 and 355 cm-1.

Darstellung und spektroskopische Charakterisierung von Tetrakis (chloro -iodo ) oxalato -osmaten (IV )/Preparation and Spectroscopical Characterisation of Tetrakis(chloro-iodo)oxalato-osmates(IV)

1981 ◽  
Vol 36 (1) ◽  
pp. 62-69 ◽  
Author(s):  
W. Preetz ◽  
H. Schulz
Keyword(s):  
Mutual Influence ◽  
Complete Separation ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Vibrational Modes ◽  
Spin Orbit ◽  
Geometric Isomers ◽  
Trans Effect ◽  
Diethylaminoethyl Cellulose ◽  
Point Groups

Abstract On treatment of [OsI4ox]2- with Cl- the mixed complexes [OsClnI4-nox]2-, n = 1, 2, 3, are formed. The isolation and complete separation of the differently coloured geometric isomers is achieved by ion exchange chromatography on diethylaminoethyl cellulose. The IR and Ra spectra are assigned according to point groups C2v, Cs, C1. The mutual influence of ligands, especially by the high trans effect of I, is indicated by shifts of the distinct vibrational and electronic bands. The observed splittings of I→Os transitions are attributed to the different groupings I-Os-I, I-Os-Cl, and I-Os-O, important for the distinction of stereoisomers. The CT-bands as well as the d-d-transitions show batho-chromic shifts with increasing number of I-ligands. Up to five spin-orbit components in the NIR region are well resolved. The assignment is improved by the electronic Ra spectra. The fine structure of some d-d-bands originates from coupling with symmetric vibrational modes.

Separation of Creatine Kinase Isoenzymes in Serum by Ion-Exchange Column Chromatography (Mercer's Method, Modified to Increase Sensitivity)

1975 ◽  
Vol 21 (3) ◽  
pp. 392-397 ◽  
Author(s):  
Daniel A Nealon ◽  
Arthur R Henderson
Keyword(s):  
Creatine Kinase ◽  
Ionic Strength ◽  
Ion Exchange ◽  
Cardiac Disease ◽  
Significant Proportion ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Serum Creatine Kinase ◽  
Diethylaminoethyl Cellulose ◽  
Ion Exchange Column

Abstract We describe our experience with Mercer's method [Clin. Chem. 20, 36 (1974)] for separating isoenzymes of creatine kinase (EC 2.7.3.2) in serum by ion-exchange chromatography. By using diethylaminoethyl cellulose rather than diethylaminoethyl Sephadex in the column and by changing the ionic strength of the eluting buffer, we could detect a significant proportion of the MB isoenzyme of serum creatine kinase at normal activities of creatine kinase in serum, even in the absence of cardiac disease.

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