Joachim Scholz | Universität Koblenz (original) (raw)
Papers by Joachim Scholz
Zeitschrift Fur Anorganische Und Allgemeine Chemie, Aug 1, 1995
... Wie in Pe C,". Abb. 1 Molekiilstruktur von Dichloro(tetramethylcyc1obuta-dien)platin(II)... more ... Wie in Pe C,". Abb. 1 Molekiilstruktur von Dichloro(tetramethylcyc1obuta-dien)platin(II) (1) (ORTEP II-Darstellung [21], 50%-Wahr-scheinlichkeitsellipsoide, H-Atome in willkurlich gewahlter GroBe dargestellt) Tabelle 1 Bindungslangen ...
Organometallics, 2001
Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdC... more Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdCHN(tBu)] (≡Li 2 (tBu-DAD); 2) prepared by reduction of tBu-DAD by 2 equiv of lithium in THF surprisingly results in the formation of the samarium(III) iodide complex [(THF) 2 Li(tBu-DAD)][(THF)Li(tBu-DAD)]SmI (5). The characteristic structural feature of 5 is formed by two (Z)-1,4-diaza-but-2-ene-1,4-diyl units bridging the Sm 3+ with two Li + ions. Complex 5 and the analogous chloride complex [(THF)Li(tBu-DAD)] 2 Sm(µ-Cl) 2 Li(THF) 2 (4b) react with 2 equiv of benzophenone to give the structurally very similar samarium complexes {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 SmX(THF) (X) Cl (6), I (7)) in high yield. The reaction formally proceeds via a 1,3-dipolar cycloaddition of the benzophenone CdO bond across a Sm-N-Cd fragment of the enediamide samarium complexes 4b and 5, including the formation of a new CC bond, and results in the formation of the novel tripodal ligand [OC(Ph) 2 CH{CHdN(tBu)}N(tBu)] 2-. X-ray structure determinations of 6 and 7 revealed that the two tripodal ligands and the halogen atom form a slightly distorted octahedral coordination geometry around the Sm 3+ ion and that the Li + ions are retained within the ligand sphere by close contacts to their N and O atoms. By controlled hydrolysis of the cycloaddition product 6, the new tripodal ligands can be separated from the samarium and isolated in the form of the lithium compound {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 (8). The crystal structure of 8, which is dimeric in the solid state, is reported.
Journal f�r Praktische Chemie, 1988
Die Dnrstellung spezieller Organyliibergangsmetallverbindungen ist besonders dann von Interesse, ... more Die Dnrstellung spezieller Organyliibergangsmetallverbindungen ist besonders dann von Interesse, wenn bei geeigneter Wahl der Reaktionspartner imd-bedingungen die Synthese der Zielverbindung in nur einem Reaktionsschritt bei gleichzeitig hoher Ausbeute gelingt. Dieses Prinzip konnten wir bei der Darstellung von Metallocengl ycolaten des Titaniums und Zirconiums, vom Typ (q5-CCjH5)2M(OCR1ReCR1R20) (M = Ti, Zr), verwirklichen. Setzt man (~5-C,H5)2TiC12 bzw. ($-C5H5)2ZrC12 mit Magnesium in Gegenwart von Ketonen K1R3C=0 um, dann entstehen zwischenzeitlich schwarzgriine bzw. tiefrote Beaktionsltisungen, und es bilden sich gemail3 G1. (1) die Metallocenglycolate 1-4.
J Organomet Chem, 2001
Reduction of [(t-Bu-DAD)TiCl(m-Cl)] 2 (1) (t-Bu-DAD: t-BuN CHCH Nt-Bu) with magnesium in the pres... more Reduction of [(t-Bu-DAD)TiCl(m-Cl)] 2 (1) (t-Bu-DAD: t-BuN CHCH Nt-Bu) with magnesium in the presence of benzophenone yields the MgCl 2-bridged dimeric titanium ketone complex [(t-Bu-DAD)Ti(m,h 2-OCPh 2)] 2 Mg(m-Cl) 2 (THF) (2) whose molecular structure largely conforms with the assumptions about the structure of the first step of the reductive coupling of ketones at low-valent titanium.
The reactions of (η5-C5Me5)2Ln(μ-Cl)2ML2 (Ln = Y, La, Lu; M = Li, K; L = Et2O, dme) 3a-c with the... more The reactions of (η5-C5Me5)2Ln(μ-Cl)2ML2 (Ln = Y, La, Lu; M = Li, K; L = Et2O, dme) 3a-c with the sodium iminoacetylacetonates 2a-b yield monomeric metallocene chelate complexes , (Ln = Y, La, Lu; R = C6H5, C6H4-4-Me) 4a-d which have been characterized by IR, NMR and mass spectrometry. In the case of the lanthanum complex 4c, the chelating structure was confirmed by an X-ray structure analysis. 4c crystallizes monoclinically in space group P21/c with a = 10.232(3), b = 10.216(1), c = 29.047(7)Å, α = γ = 90.0°, β = 97.76(3)°, Ζ = 4, and R = Rw = 0.0378 for 4026 observed reflections. The new complexes are sensitive to oxygen and moisture and soluble in all common organic solvents.
Angewandte Chemie-international Edition, 1996
... tantalum compounds [I] a) S. L Liite\ky. AK McMullen. G. P Niccolai. IP Rothwell. JC Huff-1n.... more ... tantalum compounds [I] a) S. L Liite\ky. AK McMullen. G. P Niccolai. IP Rothwell. JC Huff-1n.m Or,~(iii(iritclol/t~~s 1985. ... J E. Hill. P. E. Fanwick. I. P. Roth\iell. Or,qiii~ofiicru//i~.~ 1990. Y. 75-80, [9] [:PtCl,(PBu,)~,(l~-r'.i~'-~Bu-dad)]: C=W 1.27(3). VC' 1 4X(2) .a: H. vim der Pod. ...
Ceramic Engineering and Science Proceedings, 2012
Polyhedron, 2002
The new 1,4-diaza-1,3-diene niobium complexes (t-Bu-DAD)NbCl 3 (THF) (2) and (t-Bu-DAD) 2 NbCl (3... more The new 1,4-diaza-1,3-diene niobium complexes (t-Bu-DAD)NbCl 3 (THF) (2) and (t-Bu-DAD) 2 NbCl (3) [t-Bu-DAD (t-Bu)N CHCH N(t-Bu)] have been prepared in 75-82% isolated yields by replacing of two or four chlorine atoms of NbCl 5 by the sterically demanding t-Bu-DAD ligand. In addition, we also describe the ionic Nb(V) complex [(t-Bu-DAD)NbCl 4 ](H 3 Nt-Bu) (6) which was formed as a byproduct during the preparation of 2. The new compounds have been characterized in solution by NMR measurements as well as by X-ray analyses in solid state. The structural parameters within the t-Bu-DAD ligand of 6 are in agreement with a chelating enediamido dianion. On the other hand the N C and C C bond distances of the t-Bu-DAD ligand of 2 are rather comparable to those found in complexes having a radical-anionic t-Bu-DAD ligand. The higher steric crowding at the niobium center caused by two 1,4-diaza-1,3-diene ligands in 3 leads to a significant asymmetric distortion of the 1,3-diaza-2-niobacyclopent-4-ene rings. However, none of the 1,4-diaza-1,3-diene ligands of 2, 3 or 6 is coordinated in the sterically less demanding p2-C,N bonding mode as found in the binuclear complex (t-Bu-DAD) 5 Nb 2 (4).
Zeitschrift f�r anorganische und allgemeine Chemie, 1983
Zeitschrift f�r anorganische und allgemeine Chemie, 1995
Page 1. Z. anorg. allg. Chem. 621 (1995) 365-372 Zeitschrift fur anorganische und allgemeine Chem... more Page 1. Z. anorg. allg. Chem. 621 (1995) 365-372 Zeitschrift fur anorganische und allgemeine Chemie 0 Johann Ambrosius Barth 1995 1,4-Diaza-l,3-dien-Verbindungen elektronenarmer Ubergangsmetalle o-Donor-und It-Akzeptor-Komplexe des Zirconiums und Hafniums ...
Organometallics, 2001
Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdC... more Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdCHN(tBu)] (≡Li 2 (tBu-DAD); 2) prepared by reduction of tBu-DAD by 2 equiv of lithium in THF surprisingly results in the formation of the samarium(III) iodide complex [(THF) 2 Li(tBu-DAD)][(THF)Li(tBu-DAD)]SmI (5). The characteristic structural feature of 5 is formed by two (Z)-1,4-diaza-but-2-ene-1,4-diyl units bridging the Sm 3+ with two Li + ions. Complex 5 and the analogous chloride complex [(THF)Li(tBu-DAD)] 2 Sm(µ-Cl) 2 Li(THF) 2 (4b) react with 2 equiv of benzophenone to give the structurally very similar samarium complexes {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 SmX(THF) (X) Cl (6), I (7)) in high yield. The reaction formally proceeds via a 1,3-dipolar cycloaddition of the benzophenone CdO bond across a Sm-N-Cd fragment of the enediamide samarium complexes 4b and 5, including the formation of a new CC bond, and results in the formation of the novel tripodal ligand [OC(Ph) 2 CH{CHdN(tBu)}N(tBu)] 2-. X-ray structure determinations of 6 and 7 revealed that the two tripodal ligands and the halogen atom form a slightly distorted octahedral coordination geometry around the Sm 3+ ion and that the Li + ions are retained within the ligand sphere by close contacts to their N and O atoms. By controlled hydrolysis of the cycloaddition product 6, the new tripodal ligands can be separated from the samarium and isolated in the form of the lithium compound {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 (8). The crystal structure of 8, which is dimeric in the solid state, is reported.
Organometallics, 1999
ABSTRACT
Journal of Organometallic Chemistry, 1997
Tris[2-(dimethylaminomethyl)ferrocenyl]-thallium (FcN)3Tl (I) reacts with the vanadium(IV)/(V) ch... more Tris[2-(dimethylaminomethyl)ferrocenyl]-thallium (FcN)3Tl (I) reacts with the vanadium(IV)/(V) chlorides VCl4(THF)2, Cp2VCl2, CpVOCl2, VOCl3 with substitution of, in each case, a chlorine atom by an FcN-ligand to form bis[2-(dimethylaminomethyl)ferrocenyl]-thallium chloride (FcN)2TlCl (II) and thermally unstable (not isolable) FcN-derivatives of four/five-valent vanadium. A detailed characterization of II has been carried out by IR, mass, 1H NMR, UV-vis and Mössbauer spectroscopies. X-ray crystal structure
Journal of Organometallic Chemistry, 1995
... Chemistry 501 (1995) 71-77 of~reg ~ metallic Chemistry Synthese and Struktur des heterobimeta... more ... Chemistry 501 (1995) 71-77 of~reg ~ metallic Chemistry Synthese and Struktur des heterobimetallischen thalliumorganischen Chelatkomplexes Tris[2-(dimethylaminomethy ferrocenyl]thallium Klaus Jacob a * , Joachim ScholZ a, Claus ... [14] ME O'Neill and K. Wade, in ...
Zeitschrift Fur Anorganische Und Allgemeine Chemie, Aug 1, 1995
... Wie in Pe C,". Abb. 1 Molekiilstruktur von Dichloro(tetramethylcyc1obuta-dien)platin(II)... more ... Wie in Pe C,". Abb. 1 Molekiilstruktur von Dichloro(tetramethylcyc1obuta-dien)platin(II) (1) (ORTEP II-Darstellung [21], 50%-Wahr-scheinlichkeitsellipsoide, H-Atome in willkurlich gewahlter GroBe dargestellt) Tabelle 1 Bindungslangen ...
Organometallics, 2001
Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdC... more Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdCHN(tBu)] (≡Li 2 (tBu-DAD); 2) prepared by reduction of tBu-DAD by 2 equiv of lithium in THF surprisingly results in the formation of the samarium(III) iodide complex [(THF) 2 Li(tBu-DAD)][(THF)Li(tBu-DAD)]SmI (5). The characteristic structural feature of 5 is formed by two (Z)-1,4-diaza-but-2-ene-1,4-diyl units bridging the Sm 3+ with two Li + ions. Complex 5 and the analogous chloride complex [(THF)Li(tBu-DAD)] 2 Sm(µ-Cl) 2 Li(THF) 2 (4b) react with 2 equiv of benzophenone to give the structurally very similar samarium complexes {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 SmX(THF) (X) Cl (6), I (7)) in high yield. The reaction formally proceeds via a 1,3-dipolar cycloaddition of the benzophenone CdO bond across a Sm-N-Cd fragment of the enediamide samarium complexes 4b and 5, including the formation of a new CC bond, and results in the formation of the novel tripodal ligand [OC(Ph) 2 CH{CHdN(tBu)}N(tBu)] 2-. X-ray structure determinations of 6 and 7 revealed that the two tripodal ligands and the halogen atom form a slightly distorted octahedral coordination geometry around the Sm 3+ ion and that the Li + ions are retained within the ligand sphere by close contacts to their N and O atoms. By controlled hydrolysis of the cycloaddition product 6, the new tripodal ligands can be separated from the samarium and isolated in the form of the lithium compound {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 (8). The crystal structure of 8, which is dimeric in the solid state, is reported.
Journal f�r Praktische Chemie, 1988
Die Dnrstellung spezieller Organyliibergangsmetallverbindungen ist besonders dann von Interesse, ... more Die Dnrstellung spezieller Organyliibergangsmetallverbindungen ist besonders dann von Interesse, wenn bei geeigneter Wahl der Reaktionspartner imd-bedingungen die Synthese der Zielverbindung in nur einem Reaktionsschritt bei gleichzeitig hoher Ausbeute gelingt. Dieses Prinzip konnten wir bei der Darstellung von Metallocengl ycolaten des Titaniums und Zirconiums, vom Typ (q5-CCjH5)2M(OCR1ReCR1R20) (M = Ti, Zr), verwirklichen. Setzt man (~5-C,H5)2TiC12 bzw. ($-C5H5)2ZrC12 mit Magnesium in Gegenwart von Ketonen K1R3C=0 um, dann entstehen zwischenzeitlich schwarzgriine bzw. tiefrote Beaktionsltisungen, und es bilden sich gemail3 G1. (1) die Metallocenglycolate 1-4.
J Organomet Chem, 2001
Reduction of [(t-Bu-DAD)TiCl(m-Cl)] 2 (1) (t-Bu-DAD: t-BuN CHCH Nt-Bu) with magnesium in the pres... more Reduction of [(t-Bu-DAD)TiCl(m-Cl)] 2 (1) (t-Bu-DAD: t-BuN CHCH Nt-Bu) with magnesium in the presence of benzophenone yields the MgCl 2-bridged dimeric titanium ketone complex [(t-Bu-DAD)Ti(m,h 2-OCPh 2)] 2 Mg(m-Cl) 2 (THF) (2) whose molecular structure largely conforms with the assumptions about the structure of the first step of the reductive coupling of ketones at low-valent titanium.
The reactions of (η5-C5Me5)2Ln(μ-Cl)2ML2 (Ln = Y, La, Lu; M = Li, K; L = Et2O, dme) 3a-c with the... more The reactions of (η5-C5Me5)2Ln(μ-Cl)2ML2 (Ln = Y, La, Lu; M = Li, K; L = Et2O, dme) 3a-c with the sodium iminoacetylacetonates 2a-b yield monomeric metallocene chelate complexes , (Ln = Y, La, Lu; R = C6H5, C6H4-4-Me) 4a-d which have been characterized by IR, NMR and mass spectrometry. In the case of the lanthanum complex 4c, the chelating structure was confirmed by an X-ray structure analysis. 4c crystallizes monoclinically in space group P21/c with a = 10.232(3), b = 10.216(1), c = 29.047(7)Å, α = γ = 90.0°, β = 97.76(3)°, Ζ = 4, and R = Rw = 0.0378 for 4026 observed reflections. The new complexes are sensitive to oxygen and moisture and soluble in all common organic solvents.
Angewandte Chemie-international Edition, 1996
... tantalum compounds [I] a) S. L Liite\ky. AK McMullen. G. P Niccolai. IP Rothwell. JC Huff-1n.... more ... tantalum compounds [I] a) S. L Liite\ky. AK McMullen. G. P Niccolai. IP Rothwell. JC Huff-1n.m Or,~(iii(iritclol/t~~s 1985. ... J E. Hill. P. E. Fanwick. I. P. Roth\iell. Or,qiii~ofiicru//i~.~ 1990. Y. 75-80, [9] [:PtCl,(PBu,)~,(l~-r'.i~'-~Bu-dad)]: C=W 1.27(3). VC' 1 4X(2) .a: H. vim der Pod. ...
Ceramic Engineering and Science Proceedings, 2012
Polyhedron, 2002
The new 1,4-diaza-1,3-diene niobium complexes (t-Bu-DAD)NbCl 3 (THF) (2) and (t-Bu-DAD) 2 NbCl (3... more The new 1,4-diaza-1,3-diene niobium complexes (t-Bu-DAD)NbCl 3 (THF) (2) and (t-Bu-DAD) 2 NbCl (3) [t-Bu-DAD (t-Bu)N CHCH N(t-Bu)] have been prepared in 75-82% isolated yields by replacing of two or four chlorine atoms of NbCl 5 by the sterically demanding t-Bu-DAD ligand. In addition, we also describe the ionic Nb(V) complex [(t-Bu-DAD)NbCl 4 ](H 3 Nt-Bu) (6) which was formed as a byproduct during the preparation of 2. The new compounds have been characterized in solution by NMR measurements as well as by X-ray analyses in solid state. The structural parameters within the t-Bu-DAD ligand of 6 are in agreement with a chelating enediamido dianion. On the other hand the N C and C C bond distances of the t-Bu-DAD ligand of 2 are rather comparable to those found in complexes having a radical-anionic t-Bu-DAD ligand. The higher steric crowding at the niobium center caused by two 1,4-diaza-1,3-diene ligands in 3 leads to a significant asymmetric distortion of the 1,3-diaza-2-niobacyclopent-4-ene rings. However, none of the 1,4-diaza-1,3-diene ligands of 2, 3 or 6 is coordinated in the sterically less demanding p2-C,N bonding mode as found in the binuclear complex (t-Bu-DAD) 5 Nb 2 (4).
Zeitschrift f�r anorganische und allgemeine Chemie, 1983
Zeitschrift f�r anorganische und allgemeine Chemie, 1995
Page 1. Z. anorg. allg. Chem. 621 (1995) 365-372 Zeitschrift fur anorganische und allgemeine Chem... more Page 1. Z. anorg. allg. Chem. 621 (1995) 365-372 Zeitschrift fur anorganische und allgemeine Chemie 0 Johann Ambrosius Barth 1995 1,4-Diaza-l,3-dien-Verbindungen elektronenarmer Ubergangsmetalle o-Donor-und It-Akzeptor-Komplexe des Zirconiums und Hafniums ...
Organometallics, 2001
Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdC... more Treatment of SmI 2 (THF) n with the dilithium 1,4-diaza-1,3-diene (DAD) compound Li 2-[(tBu)NCHdCHN(tBu)] (≡Li 2 (tBu-DAD); 2) prepared by reduction of tBu-DAD by 2 equiv of lithium in THF surprisingly results in the formation of the samarium(III) iodide complex [(THF) 2 Li(tBu-DAD)][(THF)Li(tBu-DAD)]SmI (5). The characteristic structural feature of 5 is formed by two (Z)-1,4-diaza-but-2-ene-1,4-diyl units bridging the Sm 3+ with two Li + ions. Complex 5 and the analogous chloride complex [(THF)Li(tBu-DAD)] 2 Sm(µ-Cl) 2 Li(THF) 2 (4b) react with 2 equiv of benzophenone to give the structurally very similar samarium complexes {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 SmX(THF) (X) Cl (6), I (7)) in high yield. The reaction formally proceeds via a 1,3-dipolar cycloaddition of the benzophenone CdO bond across a Sm-N-Cd fragment of the enediamide samarium complexes 4b and 5, including the formation of a new CC bond, and results in the formation of the novel tripodal ligand [OC(Ph) 2 CH{CHdN(tBu)}N(tBu)] 2-. X-ray structure determinations of 6 and 7 revealed that the two tripodal ligands and the halogen atom form a slightly distorted octahedral coordination geometry around the Sm 3+ ion and that the Li + ions are retained within the ligand sphere by close contacts to their N and O atoms. By controlled hydrolysis of the cycloaddition product 6, the new tripodal ligands can be separated from the samarium and isolated in the form of the lithium compound {[OC(Ph) 2 CH{CHdN(tBu)}N(tBu)]Li} 2 (8). The crystal structure of 8, which is dimeric in the solid state, is reported.
Organometallics, 1999
ABSTRACT
Journal of Organometallic Chemistry, 1997
Tris[2-(dimethylaminomethyl)ferrocenyl]-thallium (FcN)3Tl (I) reacts with the vanadium(IV)/(V) ch... more Tris[2-(dimethylaminomethyl)ferrocenyl]-thallium (FcN)3Tl (I) reacts with the vanadium(IV)/(V) chlorides VCl4(THF)2, Cp2VCl2, CpVOCl2, VOCl3 with substitution of, in each case, a chlorine atom by an FcN-ligand to form bis[2-(dimethylaminomethyl)ferrocenyl]-thallium chloride (FcN)2TlCl (II) and thermally unstable (not isolable) FcN-derivatives of four/five-valent vanadium. A detailed characterization of II has been carried out by IR, mass, 1H NMR, UV-vis and Mössbauer spectroscopies. X-ray crystal structure
Journal of Organometallic Chemistry, 1995
... Chemistry 501 (1995) 71-77 of~reg ~ metallic Chemistry Synthese and Struktur des heterobimeta... more ... Chemistry 501 (1995) 71-77 of~reg ~ metallic Chemistry Synthese and Struktur des heterobimetallischen thalliumorganischen Chelatkomplexes Tris[2-(dimethylaminomethy ferrocenyl]thallium Klaus Jacob a * , Joachim ScholZ a, Claus ... [14] ME O'Neill and K. Wade, in ...