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 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 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%.

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 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.

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, Schwingungsspektren und Normalkoordinatenanalyse von Chloro-Bromo-Rhodaten(III) / Preparation, Vibration Spectra and Normal Coordinate Analysis of Chloro-Bromo-Rhodates(III)

1989 ◽  
Vol 44 (10) ◽  
pp. 1221-1227 ◽  
Author(s):  
W. Preetz ◽  
W. Kuhr
Keyword(s):  
Exchange Chromatography ◽  
Trans Isomers ◽  
Normal Coordinate ◽  
Valence Force ◽  
Trans Influence ◽  
Diethylaminoethyl Cellulose ◽  
Point Groups ◽  
First Time ◽  
Ir And Raman ◽  
Good Agreement

The mixed chloro-bromo-rhodates(III) [RhClnBr6-n]3-, n = 1-5, have been separated for the first time by ion exchange chromatography on diethylaminoethyl-cellulose. Due to the stronger trans-effect of Br, as compared with Cl, on treatment of [RhBr6]3- with conc. HCl nearly pure cis/fac-isomers for n = 2, 3, 4 are formed. The reaction of [RhCl6]3- with conc. HBr yields mixtures of the cis/trans-isomers for n = 2, 4, which cannot be separated, but mer-[RhCl3Br3]3 is formed stereospecifically. The IR and Raman spectra of all isolated mixed ligand complexes are completely assigned according to point groups Oh, D3d, C4v, C3v and C2v, supported by normal coordinate analyses based on a general valence force field. The good agreement of calculated and observed frequencies confirms the assignments. Due to the stronger trans-influence of Br as compared to Cl, in all asymmetric Cl—Rh—Br axes the Rh—Br bonds are strengthened and the Rh—Cl bonds are weakened, indicated by valence force constants for Rh—Br approximately 14% higher, for Rh—Cl 10% lower, as compared with the values calculated for symmetric Br—Rh—Br and Cl—Rh—Cl axes, respectively.

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 von Fluoro-Chloro-Osmaten(V)/ Preparation and Vibrational Spectra of Fluoro-Chloro-Osm ates(V)

1986 ◽  
Vol 41 (7) ◽  
pp. 885-889 ◽  
Author(s):  
W. Preetz ◽  
Th. Groth
Keyword(s):  
Bond Strength ◽  
Vibrational Spectra ◽  
Trifluoroacetic Acid ◽  
Mixed Ligand ◽  
Mixed Ligand Complexes ◽  
Significant Shift ◽  
Stretching Vibration ◽  
Point Groups

AbstractBy oxidation of the pure fluoro-chloro-osmates(IV ) with BrF3 in dichlorom ethane the mixed pentavalent complexes [OsF5Cl]-, cis-[OsF4Cl2]-, fac-[OsF3Cl3]- and cis-[OsF2Cl4]- are formed without replacement of ligands. Trans-[OsF4Cl2]- and trans-[OsF2Cl4]- are generated from the corresponding osmates(IV) by oxidation with PbO2 in dichloromethane under addition of trifluoroacetic acid. The vibrational spectra o f the mixed ligand complexes are assigned according to point groups D4h, C4v, C3v and C2v. The increased bond strength com pared with the corresponding Os(IV ) complexes is indicated by a significant shift to higher energy by about 5 -15% . The Os -Cl stretching vibration of [OsF5Cl]- and also the symmetric ClOsCl of trans-[OsF4Cl2]- is split by the isotopes 35Cl and 37Cl, showing two and three well resolved sharp Raman lines in the expected ratio of intensities, respectively.

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

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