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.

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.

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 Schwingungsspektren von Fluoro-Chloro- Platinaten(IV) einschließlich der Stereoisomeren / Preparation and Vibrational Spectra of Fluoro-Chloro-Platinates(IV) Including Stereoisomers

1989 ◽  
Vol 44 (4) ◽  
pp. 412-418 ◽  
Author(s):  
W. Preetz ◽  
P. Erlhöfer
Keyword(s):  
Ion Exchange ◽  
Vibrational Spectra ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Mixed Ligand ◽  
Trans Isomers ◽  
Trans Effect ◽  
Diethylaminoethyl Cellulose ◽  
Point Groups ◽  
Stretching Vibrations

The reaction of [PtCI6]2- with BrF3 generates the mixed complexes [PtFnC6-n]2- , n = 1- 5, of which the species with n = 2. 3, 4 are cis-configurated. Due to the stronger trans-effect of Cl compared to F, on treatment of [PtF5Cl]2- and cis-[PtF4Cl2]2- with Cl- the trans-isomers are formed stereospecifically. The pure fluoro-chloro-platinates(IV) are separated by ion exchange chromatography on diethylaminoethyl-cellulose. The vibrational spectra o f the mixed ligand complexes are completely assigned according to point groups D4h, C4v, C3v and C2v. The Pt-Cl stretching vibrations of [PtF5Cl]2-, trans-[PtF4Cl2]2-, mer-[PtF3Cl3]2- and [PtFCl5]2- are split by the isotopes 35Cl and 37Cl, showing well resolved sharp Raman lines in the expected ratio of intensities.

Darstellung und Schwingungsspektren von Chloro-Bromo-Ruthenaten(IV) einschließlich der Stereoisomeren / Preparation and Vibrational Spectra of Chloro-Bromo-Ruthenates(IV) Including Stereoisomers

1987 ◽  
Vol 42 (4) ◽  
pp. 381-386 ◽  
Author(s):  
W. Preetz ◽  
H. N. v. Allwörden
Keyword(s):  
Ion Exchange ◽  
Force Field ◽  
Vibrational Spectra ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Mixed Ligand ◽  
Mixed Ligand Complexes ◽  
Trans Effect ◽  
Point Groups ◽  
First Time

Abstract The mixed chloro-bromo complexes [RuClnBr6-n]2-, n = 1-5, have been separated for the first time by ion exchange chromatography on diethylaminoethylcellulose. Due to the stronger trans-effect of Br compared with Cl, on treatment of [RuBr6]2- with Cl- in the presence of Br2 nearly pure cis/fac-isomers,and by reaction of [RuCl6]2- withBr-/Br2 nearly purer tranS/mer-isomersforn = 2,3,4 are formed. The vibrational spectra of the mixed ligand complexes are completely assigned according to point groups D4h, C4v, C3v and C2v, respectively. The bands are observed in the characteristic regions: ν(RuCl): 340-270 > ν(RuBr): 245-190 > δ(ClRuCl) ≥ δ(ClRubr) ≥ δ(BrRuBr): 125-90 > νʟ: < 100 cm-1. The lower stability of the hexahalogeno complexes of Ru(IV), 4d, compared with the homologous complexes of Os(IV), 5d, is confirmed by a decrease of the force field constants by approximately 15%.

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

1984 ◽  
Vol 39 (8) ◽  
pp. 1100-1109 ◽  
Author(s):  
W. Preetz ◽  
D. Ruf ◽  
D. Tensfeldt
Keyword(s):  
Ion Exchange ◽  
Electric Field ◽  
Vibrational Spectra ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Mixed Ligand ◽  
Deformation Bands ◽  
Trans Isomers ◽  
Trans Effect ◽  
Point Groups

AbstractThe stepwise replacement of ligands in [OsCl6]2- by oxidation with BrF3 generates the mixed complexes [OsFnCl6-n]2-, n = 1 - 5, of which the species with n = 2,3,4 are cw-configurated. Due to the stronger trans-effect of Cl compared to F on treatment of [OsF5Cl]2- and cis-[OsF4Cl2]2- with Cl- the trans-isomers are formed stereospecifically. The pure fluoro-chloro-osmates(IV) are separated by ion exchange chromatography on diethylaminoethylcellulose. From the pairs of stereoisomers the cis-compounds are always first eluted, whereas the trans-complexes are moving faster in an electric field by 3 to 5% . The vibrational spectra of octahedral mixed ligand complexes are generally discussed according to point groups Oh, D4h, C4v, C3v and C2v. For the fluoro-chloroosmates(IV) all stretching and deformation bands are assigned. They are observed in the characteristic regions; ν(OsF): 625-490 > ν(OsCl): 360-300 > δ (FOsF): 275-210 > δ (FOsCl) > δ (ClOsCl): 190-150 > νL: < 100 cm -1.

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.

Darstellung, 11B-, 13C-, 1H-NMR - und Schwingungsspektren von μ-Pentamethylen-bis-hexahydro-closo-hexaborat, [B6H6(CH2)5B6H6]2-, und μ-Hexamethylen-bis-hexahydro-closo-hexaborat, [B6H6(CH2)6B6H6]2/Preparation, 11B, 13C, 1H NMR and Vibrational Spectra of μ-Pentamethylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)5 B6H6 ]2-, and μ-Hexamethylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)6B6H6]2-

1996 ◽  
Vol 51 (3) ◽  
pp. 359-362 ◽  
Author(s):  
W. Lübbe ◽  
W. Preetz
Keyword(s):  
Ion Exchange ◽  
Vibrational Spectroscopy ◽  
1H Nmr ◽  
Vibrational Spectra ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
H Nmr ◽  
Diethylaminoethyl Cellulose

Abstract In the reaction of [B6H6]2- with diiodopentane or diiodohexane in dichloromethane μ-pentamethylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)5B6H6]2- (I), and μ-hexamethylene-bishexahydro-closo-hexaborate, [B6H6(CH2)6B6H6]2- (II), are formed, respectively. The products were separated from excess [B6H6]2- by ion exchange chromatography on diethylaminoethyl cellulose and have been identified and characterized by 11B, 13C, 1H NMR and vibrational spectroscopy.

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.

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

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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