Hans Reuter - Profile on Academia.edu (original) (raw)
Papers by Hans Reuter
Zeitschrift für Naturforschung B, Feb 1, 2007
Strontium hydroxide octahydrate Sr(OH) 2 • 8 H 2 O crystallizes in the tetragonal space group P4/... more Strontium hydroxide octahydrate Sr(OH) 2 • 8 H 2 O crystallizes in the tetragonal space group P4/ncc with cell constants a = 9.017(1) and c = 11.603(1) Å. The crystal structure has been refined from 2656 diffractometer data up to 2ϑ = 60 • to an R value of 0.0303. With the new diffraction data it was possible to localize the positions of all hydrogen atoms for the first time and to describe the hydrogen bonding scheme in detail. The Sr 2+ ions are square antiprismatically coordinated by eight water molecules. These {Sr(H 2 O) 8 } 2+ coordination polyhedra are linked with each other via hydrogen bonds in a way that linear columns parallel to the c axis result. The two hydroxyl anions of the asymmetric unit are linked by weak hydrogen bonds and are not coordinated to strontium atoms. Like the strontium atoms, they form linear chains parallel to the c axis. Both, {Sr(H 2 O) 8 } 2+ columns and OH -chains, are interconnected through two types of additional hydrogen bonds.
The Journal of Organic Chemistry, 2017
A de novo Palladium carbon catalyzed synthesis of tri-substituted nicotinonitriles from easily sy... more A de novo Palladium carbon catalyzed synthesis of tri-substituted nicotinonitriles from easily synthesized homopropagylic or homoallylic aromatic alcohols in presence of nitriles has been explored. The mechanism proceeds with an interesting generation of Pd(II) -C palladacycle followed by an oxidative aromatization to generate the pyridine core. The pyridine core is generated with a noteworthy C-C bond cleavage incase with the substituted nitriles. The moderate yields and easy separation of the products delivers a unique importance to this one pot methodology.
Observations to the Structural Evolution of Tin(IV)-Oxygen-Gels
Eurogel '91, 1992
ABSTRACT In order to isolate the different intermediates formed during the formation of tin(IV)-o... more ABSTRACT In order to isolate the different intermediates formed during the formation of tin(IV)-oxygen-gels, the normal sol-gel-process was modified by a slow and incomplete addition of water, by use of dipolar aprotic solvents and monoorganotin compounds, respectively. The characterization of the different oligomers by single crystal X-ray diffraction gives a first raw model on the structural evolution and on the inclusion of ions and sovent molecules during gelation.
Thia- and oxa-[2.2]metacyclophanes: synthesis, helicity, and stereoselective formation of sulphoxides
J. Chem. Soc., Chem. Commun., 1986
2'-Deoxyimmunosine: a thiazolo[4,5-d]pyrimidine nucleoside adopting the syn conformation
Acta crystallographica. Section C, Crystal structure communications, 2007
The title compound [systematic name: 5-amino-3-(2-deoxy-beta-D-erythro-pentofuranosyl)thiazolo[4,... more The title compound [systematic name: 5-amino-3-(2-deoxy-beta-D-erythro-pentofuranosyl)thiazolo[4,5-d]pyrimidine-2,7-(3H,6H)-dione], C(10)H(12)N(4)O(5)S, exhibits a syn glycosylic bond conformation, with a torsion angle chi of 61.0 (3) degrees. The furanose moiety adopts the N-type sugar pucker ((3)T4), with P = 33.0 (5) degrees and tau(m) = 15.1 (1) degrees. The conformation at the exocyclic C4'-C5' bond is +ap (trans), with the torsion angle gamma = 176.71 (14) degrees. The extended structure is a three-dimensional hydrogen-bond network involving O-H...O and N-H...O hydrogen bonds.
Tetrahedron, 1999
Crystallization of 1-deaza-2'-deoxyadenosine (c~Ad, 1) from propanol-2 gives two forms of crystal... more Crystallization of 1-deaza-2'-deoxyadenosine (c~Ad, 1) from propanol-2 gives two forms of crystals: type A formed firstly as plates, then, on the surface of the plates, type B appeared as needles. Single crystal X-ray analyses shows that the crystals A and B differ mainly in the sugar ring conformation: A adopts the S-type (P = 179.8°; C.2'-endo-C-Y-exo; 2%) conformation associated with an high-anti base orientation (g = -90.7 °) and the y = 152.3 ° across the exocyclic C(4')-C(5') bond; B shows N-type (P = 21.2; C-3'-endo; 3E) conformation accompanied by a somewhat different anti base orientation (g = -116.5 °) an eclipsed orientation of the exocyclic C(4')-C(5') bond (y = 84.5°). No intramolecular hydrogen bonds in both types of crystals can be detected. Unlike CtAd, the ribonucleoside (etA, 2) is in the syn conformation (g = 56.1 °) in the solid state which is caused by an intramolecular (5')CH2OH.-.N(3) hydrogen bond. The compounds I and 2 display very similar conformation in D20 solution with a strong preference for the S-type conformation of the furanose ring accompanied by the intramolecular (5')CH2OH...N(3) hydrogen bond.
The N(1)-(2'-deoxyribofuranoside) of 3-iodo-5-nitroindole: a universal nucleoside forming nitro-iodo interactions
Acta crystallographica. Section C, Crystal structure communications, 2009
The title compound [systematic name: 1-(2-deoxy-beta-D-erythro-pentofuranosyl)-3-iodo-5-nitro-1H-... more The title compound [systematic name: 1-(2-deoxy-beta-D-erythro-pentofuranosyl)-3-iodo-5-nitro-1H-indole], C(13)H(13)IN(2)O(5), exhibits an anti glycosylic bond conformation with a chi torsion angle of -114.9 (3) degrees . The furanose moiety shows a twisted C2'-endo sugar pucker (S-type), with P = 141.3 degrees and tau(m) = 40.3 degrees . The orientation of the exocyclic C4'-C5' bond is +ap (gauche, trans), with a gamma torsion angle of 177.4 (2) degrees . The extended crystal structure is stabilized by hydrogen bonding and I...O contacts, as well as by stacking interactions. The O atoms of the nitro group act as acceptors, forming bifurcated hydrogen bonds within the ac plane. Additionally, the iodo substituent forms an interplanar contact with an O atom of the nitro group, and another contact with the O atom of the 5'-hydroxy group of the sugar moiety within the ac plane is observed. These contacts can be considered as the structure-determining factors for the mole...
Zeitschrift für anorganische und allgemeine Chemie, 1997
Farblose Kristalle von Li2[Sn(OH)6] · 2 H2O wurden durch Umsetzung von SnCl4 mit LiOH in wäßriger... more Farblose Kristalle von Li2[Sn(OH)6] · 2 H2O wurden durch Umsetzung von SnCl4 mit LiOH in wäßriger Phase erhalten. Die Kristallstruktur der Verbindung konnte an Einkristallen aufgeklärt werden.Li2[Sn(OH)6] · 2 H2O: monoklin, P21/n (Nr. 14), a = 502.3(1), b = 692.3(1), c = 1020.2(3) pm, β = 99.78(1)°, V = 349.6(2) · 106 pm3, Z = 2, R/Rw = 0.0192/0.0472, N(I) > 2σ(I) = 1527, N(Par.) = 54.Innerhalb des Kristallverbandes sind nur wenig verzerrte, oktaedrische [Sn(OH)6]2−‐Ionen über Wasserstoffbrückenbindungen mit Wassermolekülen zu Schichten verknüpft, die ihrerseits untereinander über tetraedrisch koordinierte Lithium‐Ionen verbunden sind; die Struktur ist in Übereinstimmung mit den IR‐Daten und Ergebnissen der 119Sn‐Festkörper‐NMR‐Spektroskopie; Hydratwasser wird bei 117.1°C abgespalten, die Kondensationsreaktion zum ternären Oxid erfolgt bei 257.7°C.
Phosphorus, Sulfur, and Silicon and the Related Elements, 2011
The title compound Et 2 SnCl 2 • H 2 O was prepared and characterized by IRspectroscopy and singl... more The title compound Et 2 SnCl 2 • H 2 O was prepared and characterized by IRspectroscopy and single crystal X-ray diffraction, showing the typical trigonal bipyramidal structure of a S N 2 transition state with the water molecule in an axial position. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.
Zeitschrift für Kristallographie - New Crystal Structures, 1998
Gel-to-Solid Transition in Polyethylene from the Viewpoint of the Crystallization Process
Macromolecules, 2003
ABSTRACT The crystalline phase in gels and solid gel-derived samples of ultrahigh molecular weigh... more ABSTRACT The crystalline phase in gels and solid gel-derived samples of ultrahigh molecular weight polyethylene was studied using the infrared spectroscopy, low-frequency Raman spectroscopy and wide-angle X-ray scattering methods. The spectroscopic data evidence the presence in gels of tiny crystallites whose thickness (3-5 nm) depends on the sort of the solvent used and it is insensitive neither to the concentration of the diluted solution, nor to the molecular weight of the polymer. After removal of the solvent, there appear crystalline clusters composed of closely attached folded platelets. The total thickness of these stacked entities is about 10-20 nm while their transverse size reaches similar to50 nm. In addition, the crystalline domains in the gelled material exhibit a kind of mosaic structure which is much more pronounced in solid xerogels than in wet gels.
Journal of Organometallic Chemistry, 1991
High-resolution "'Sn spectra of solid trimethyltin fluoride (I), tri-isobutyltin fluoride (II), a... more High-resolution "'Sn spectra of solid trimethyltin fluoride (I), tri-isobutyltin fluoride (II), and triphenyltin fluoride (III) show that all the compounds are five-coordinate in the solid state, with the "'Sn nucleus apparently equally coupled to two fluorines. In contrast, the spectrum of trimesityltin fluoride (IV) indicates, in conformity with X-ray results, that the tin is four-coordinate and couples to only one fluorine, but that there are two molecules in the asymmetric unit.
The Journal of Organic Chemistry, 1991
A series of pyridino macrocycles 1-3(a-e) incorporating rigid bi-and triaryl ether segments in di... more A series of pyridino macrocycles 1-3(a-e) incorporating rigid bi-and triaryl ether segments in different ring positions have been synthesized. The effect of incorporation of these building blocks into a given macroring framework on the host properties for uncharged-molecule inclusion has been studied. Symmetric 21-membered macrorings IC, Id, or 2c, 2d with tri-o-phenylene, tri-e,&naphthylene, or mixed phenylene naphthylene ether units are efficient hosts in solid-state complexation of dipolar-aprotic and apolar guests such as nitro compounds and nitriles as well as DMF, DMSO, THF, dioxane, or benzene. X-ray analyses of the solid-state complexes of Id with PhNOz (1:l) and MeCN (1:l) have been studied. It is shown that the presence of the triaryl ether segment induces a biconcave nonequally sided host conformation suitable for guest inclusion. The packing characterizes the host-guest topologies of the two inclusion compounds to be of (H-bonded) cavitate-type for the MeCN case and of interstitial channel type for the PhNOz case. A comparative discussion of the present and previous results support the interpretation of hemispherand preorganization for the new host structures.
Monoorganotin–polyoxometal-compounds. Part IV: Na2[(iPrSn3)(OV)4O10(OH)3]·5H2O·3DMSO, a novel branched tetravanadate(V) stabilized by a trimeric monoorganotin-oxo-hydroxo unit
Inorganica Chimica Acta, 2010
Via self-assembly of the molecular precursors sodium orthovanadate and isopropyltin-dihydroxide-c... more Via self-assembly of the molecular precursors sodium orthovanadate and isopropyltin-dihydroxide-chloride the unprecedented organic–inorganic hybrid polyoxoanion [(iPrSn)3(OV)4O10(OH)3]2− was synthesized in dimethylsulfoxide (DMSO) and isolated as its sodium salt Na2[(iPrSn)3(OV)4O10(OH)3]·5H2O·3DMSO. This spherical nanosized anion is composed of two different structural subunits, a well-known trinuclear monoorganotin-polyoxo-hydroxo unit with octahedrally coordinated tin atoms and a new open-chain, branched isopolyoxo tetravanadate(V) with tetrahedrally coordinated vanadium atoms.
N ‐Tosylaza[2.2]metacyclophan — Darstellung, Struktur, Helicität, Chiroptik, Racemisierung
Chemische Berichte, 1988
Synthesis, structure, helicity, and chiroptical properties of the ten-membered helical N-tosylaza... more Synthesis, structure, helicity, and chiroptical properties of the ten-membered helical N-tosylaza[2.2]metacyclophane 7a are described for the first time. 7a exist in a strained anti conformation, the inner (Hi-) protons of which absorb at high field (4.13, 4.34 ppm). The enantiomers of 7a were enriched by low-pressure chromatography on triacetylcellulose (TAC). Specific rotations, barrier of racemization, and circular dichrograms are discussed with respect to comparison compounds.
Angewandte Chemie, 1995
Achim Miiller Abb. 3. Zusammenstellung einiger in der anorganischen Wirt-Gast-Chemie gebrauchlich... more Achim Miiller Abb. 3. Zusammenstellung einiger in der anorganischen Wirt-Gast-Chemie gebrauchlicher Tektone und Tektonaquivalente. Die Zielverbindung (Zentrum) wird retrosynthetisch in die Tektone (mittlerer Ring) zerlegt, die ihrerseits uber einfache Reaktionen aus den in der Anorganischen Chemie bekannten, stabilen oder als Intermediat vennuteten Tektoniquivalenten (iulierer Ring) zuganglich sein sollten.
Angewandte Chemie, 2002
Die Festkˆrperstruktur des 7-Desaza-2'-desoxyxanthosin-Dihydrats 1 ¥ 2 H 2 O deckt einige interes... more Die Festkˆrperstruktur des 7-Desaza-2'-desoxyxanthosin-Dihydrats 1 ¥ 2 H 2 O deckt einige interessante Befunde auf: Neben einer intramolekularen Wasserstoffbr¸cke (N3-H ¥¥¥ OH-5') treten weitere Wasserstoffbr¸cken auf, die ein supramolekulares Aggregat aus vier Molek¸len 1 stabilisieren. Dabei entsteht ein nahezu flaches Tetramer (Abbildung 1) mit einem ovalen Hohlraum der ungef‰hren Abmessung 9.5 Â 6.5 Â 3.0 ä (AE 0.5 ä). ‹bereinander gestapelte Tetramere bilden eine columnare, Nanorˆhren-artige Struktur (Abbildung 2). Abbildung 1. L‰nge der Wasserstoffbr¸cken im H 2 O-haltigen Tetramer aus vier Molek¸len 1. Abbildung 2. Nanorˆhre aus gestapelten Tetrameren (siehe Abbildung 1). Die Synthese von 1 wurde wie fr¸her beschrieben durchgef¸hrt. 1 kristallisiert aus iPrOH/H 2 O/MeOH (3:1:1) in Gegenwart geringer Anteile Essigs‰ure als Dihydrat in der monoklinen Raumgruppe P2 1 (siehe Hintergrundinformationen). Die Molek¸lstruktur im Kristall zeigt, dass 1 in der 2,4-Dioxoform vorliegt (Abbildung 3); die beiden Oxogruppen liegen etwas au˚erhalb der Ringebene. Der Torsionswinkel c 1 (O4'-C1'-N9-C4), der die Orientierung der Base relativ zum Zuckerrest beschreibt (syn/anti), betr‰gt 61.98; damit liegt das Nucleosid 1 in der syn-Konformation vor. Aus einer ‹bersicht ¸ber nahezu 300 Kristallstrukturanalysen von Nucleosiden geht hervor, dass 1 [
Angewandte Chemie, 1991
Um ein Natrium‐Ion als Templat baut sich die kugelförmige Schale des dodecameren Organozinn‐Sauer... more Um ein Natrium‐Ion als Templat baut sich die kugelförmige Schale des dodecameren Organozinn‐Sauerstoff‐Kations der Titelverbindung auf ‐ siehe Polyederdarstellung rechts, bei der schwarze Punkte Isopropylgruppen symbolisieren. Neben dieser neuartigen anorganischen Wirt‐Gast‐Verbindung ist auch die Struktur des [Ag7I11]‐Anions recht bemerkenswert, das als eindimensionales, verdrilltes Doppelband flächenverknüpfter Iodid‐Tetraeder vorliegt und eine hohe Silber‐Ionen‐Leitfähigkeit erwarten läßt.magnified image
Trimethylene-Bridged Tri- and Tetratin Compounds as Building Blocks for Unusual Double and Triple Ladders
Angewandte Chemie International Edition in English, 1997
Zeitschrift für Naturforschung B, Feb 1, 2007
Strontium hydroxide octahydrate Sr(OH) 2 • 8 H 2 O crystallizes in the tetragonal space group P4/... more Strontium hydroxide octahydrate Sr(OH) 2 • 8 H 2 O crystallizes in the tetragonal space group P4/ncc with cell constants a = 9.017(1) and c = 11.603(1) Å. The crystal structure has been refined from 2656 diffractometer data up to 2ϑ = 60 • to an R value of 0.0303. With the new diffraction data it was possible to localize the positions of all hydrogen atoms for the first time and to describe the hydrogen bonding scheme in detail. The Sr 2+ ions are square antiprismatically coordinated by eight water molecules. These {Sr(H 2 O) 8 } 2+ coordination polyhedra are linked with each other via hydrogen bonds in a way that linear columns parallel to the c axis result. The two hydroxyl anions of the asymmetric unit are linked by weak hydrogen bonds and are not coordinated to strontium atoms. Like the strontium atoms, they form linear chains parallel to the c axis. Both, {Sr(H 2 O) 8 } 2+ columns and OH -chains, are interconnected through two types of additional hydrogen bonds.
The Journal of Organic Chemistry, 2017
A de novo Palladium carbon catalyzed synthesis of tri-substituted nicotinonitriles from easily sy... more A de novo Palladium carbon catalyzed synthesis of tri-substituted nicotinonitriles from easily synthesized homopropagylic or homoallylic aromatic alcohols in presence of nitriles has been explored. The mechanism proceeds with an interesting generation of Pd(II) -C palladacycle followed by an oxidative aromatization to generate the pyridine core. The pyridine core is generated with a noteworthy C-C bond cleavage incase with the substituted nitriles. The moderate yields and easy separation of the products delivers a unique importance to this one pot methodology.
Observations to the Structural Evolution of Tin(IV)-Oxygen-Gels
Eurogel '91, 1992
ABSTRACT In order to isolate the different intermediates formed during the formation of tin(IV)-o... more ABSTRACT In order to isolate the different intermediates formed during the formation of tin(IV)-oxygen-gels, the normal sol-gel-process was modified by a slow and incomplete addition of water, by use of dipolar aprotic solvents and monoorganotin compounds, respectively. The characterization of the different oligomers by single crystal X-ray diffraction gives a first raw model on the structural evolution and on the inclusion of ions and sovent molecules during gelation.
Thia- and oxa-[2.2]metacyclophanes: synthesis, helicity, and stereoselective formation of sulphoxides
J. Chem. Soc., Chem. Commun., 1986
2'-Deoxyimmunosine: a thiazolo[4,5-d]pyrimidine nucleoside adopting the syn conformation
Acta crystallographica. Section C, Crystal structure communications, 2007
The title compound [systematic name: 5-amino-3-(2-deoxy-beta-D-erythro-pentofuranosyl)thiazolo[4,... more The title compound [systematic name: 5-amino-3-(2-deoxy-beta-D-erythro-pentofuranosyl)thiazolo[4,5-d]pyrimidine-2,7-(3H,6H)-dione], C(10)H(12)N(4)O(5)S, exhibits a syn glycosylic bond conformation, with a torsion angle chi of 61.0 (3) degrees. The furanose moiety adopts the N-type sugar pucker ((3)T4), with P = 33.0 (5) degrees and tau(m) = 15.1 (1) degrees. The conformation at the exocyclic C4'-C5' bond is +ap (trans), with the torsion angle gamma = 176.71 (14) degrees. The extended structure is a three-dimensional hydrogen-bond network involving O-H...O and N-H...O hydrogen bonds.
Tetrahedron, 1999
Crystallization of 1-deaza-2'-deoxyadenosine (c~Ad, 1) from propanol-2 gives two forms of crystal... more Crystallization of 1-deaza-2'-deoxyadenosine (c~Ad, 1) from propanol-2 gives two forms of crystals: type A formed firstly as plates, then, on the surface of the plates, type B appeared as needles. Single crystal X-ray analyses shows that the crystals A and B differ mainly in the sugar ring conformation: A adopts the S-type (P = 179.8°; C.2'-endo-C-Y-exo; 2%) conformation associated with an high-anti base orientation (g = -90.7 °) and the y = 152.3 ° across the exocyclic C(4')-C(5') bond; B shows N-type (P = 21.2; C-3'-endo; 3E) conformation accompanied by a somewhat different anti base orientation (g = -116.5 °) an eclipsed orientation of the exocyclic C(4')-C(5') bond (y = 84.5°). No intramolecular hydrogen bonds in both types of crystals can be detected. Unlike CtAd, the ribonucleoside (etA, 2) is in the syn conformation (g = 56.1 °) in the solid state which is caused by an intramolecular (5')CH2OH.-.N(3) hydrogen bond. The compounds I and 2 display very similar conformation in D20 solution with a strong preference for the S-type conformation of the furanose ring accompanied by the intramolecular (5')CH2OH...N(3) hydrogen bond.
The N(1)-(2'-deoxyribofuranoside) of 3-iodo-5-nitroindole: a universal nucleoside forming nitro-iodo interactions
Acta crystallographica. Section C, Crystal structure communications, 2009
The title compound [systematic name: 1-(2-deoxy-beta-D-erythro-pentofuranosyl)-3-iodo-5-nitro-1H-... more The title compound [systematic name: 1-(2-deoxy-beta-D-erythro-pentofuranosyl)-3-iodo-5-nitro-1H-indole], C(13)H(13)IN(2)O(5), exhibits an anti glycosylic bond conformation with a chi torsion angle of -114.9 (3) degrees . The furanose moiety shows a twisted C2'-endo sugar pucker (S-type), with P = 141.3 degrees and tau(m) = 40.3 degrees . The orientation of the exocyclic C4'-C5' bond is +ap (gauche, trans), with a gamma torsion angle of 177.4 (2) degrees . The extended crystal structure is stabilized by hydrogen bonding and I...O contacts, as well as by stacking interactions. The O atoms of the nitro group act as acceptors, forming bifurcated hydrogen bonds within the ac plane. Additionally, the iodo substituent forms an interplanar contact with an O atom of the nitro group, and another contact with the O atom of the 5'-hydroxy group of the sugar moiety within the ac plane is observed. These contacts can be considered as the structure-determining factors for the mole...
Zeitschrift für anorganische und allgemeine Chemie, 1997
Farblose Kristalle von Li2[Sn(OH)6] · 2 H2O wurden durch Umsetzung von SnCl4 mit LiOH in wäßriger... more Farblose Kristalle von Li2[Sn(OH)6] · 2 H2O wurden durch Umsetzung von SnCl4 mit LiOH in wäßriger Phase erhalten. Die Kristallstruktur der Verbindung konnte an Einkristallen aufgeklärt werden.Li2[Sn(OH)6] · 2 H2O: monoklin, P21/n (Nr. 14), a = 502.3(1), b = 692.3(1), c = 1020.2(3) pm, β = 99.78(1)°, V = 349.6(2) · 106 pm3, Z = 2, R/Rw = 0.0192/0.0472, N(I) > 2σ(I) = 1527, N(Par.) = 54.Innerhalb des Kristallverbandes sind nur wenig verzerrte, oktaedrische [Sn(OH)6]2−‐Ionen über Wasserstoffbrückenbindungen mit Wassermolekülen zu Schichten verknüpft, die ihrerseits untereinander über tetraedrisch koordinierte Lithium‐Ionen verbunden sind; die Struktur ist in Übereinstimmung mit den IR‐Daten und Ergebnissen der 119Sn‐Festkörper‐NMR‐Spektroskopie; Hydratwasser wird bei 117.1°C abgespalten, die Kondensationsreaktion zum ternären Oxid erfolgt bei 257.7°C.
Phosphorus, Sulfur, and Silicon and the Related Elements, 2011
The title compound Et 2 SnCl 2 • H 2 O was prepared and characterized by IRspectroscopy and singl... more The title compound Et 2 SnCl 2 • H 2 O was prepared and characterized by IRspectroscopy and single crystal X-ray diffraction, showing the typical trigonal bipyramidal structure of a S N 2 transition state with the water molecule in an axial position. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.
Zeitschrift für Kristallographie - New Crystal Structures, 1998
Gel-to-Solid Transition in Polyethylene from the Viewpoint of the Crystallization Process
Macromolecules, 2003
ABSTRACT The crystalline phase in gels and solid gel-derived samples of ultrahigh molecular weigh... more ABSTRACT The crystalline phase in gels and solid gel-derived samples of ultrahigh molecular weight polyethylene was studied using the infrared spectroscopy, low-frequency Raman spectroscopy and wide-angle X-ray scattering methods. The spectroscopic data evidence the presence in gels of tiny crystallites whose thickness (3-5 nm) depends on the sort of the solvent used and it is insensitive neither to the concentration of the diluted solution, nor to the molecular weight of the polymer. After removal of the solvent, there appear crystalline clusters composed of closely attached folded platelets. The total thickness of these stacked entities is about 10-20 nm while their transverse size reaches similar to50 nm. In addition, the crystalline domains in the gelled material exhibit a kind of mosaic structure which is much more pronounced in solid xerogels than in wet gels.
Journal of Organometallic Chemistry, 1991
High-resolution "'Sn spectra of solid trimethyltin fluoride (I), tri-isobutyltin fluoride (II), a... more High-resolution "'Sn spectra of solid trimethyltin fluoride (I), tri-isobutyltin fluoride (II), and triphenyltin fluoride (III) show that all the compounds are five-coordinate in the solid state, with the "'Sn nucleus apparently equally coupled to two fluorines. In contrast, the spectrum of trimesityltin fluoride (IV) indicates, in conformity with X-ray results, that the tin is four-coordinate and couples to only one fluorine, but that there are two molecules in the asymmetric unit.
The Journal of Organic Chemistry, 1991
A series of pyridino macrocycles 1-3(a-e) incorporating rigid bi-and triaryl ether segments in di... more A series of pyridino macrocycles 1-3(a-e) incorporating rigid bi-and triaryl ether segments in different ring positions have been synthesized. The effect of incorporation of these building blocks into a given macroring framework on the host properties for uncharged-molecule inclusion has been studied. Symmetric 21-membered macrorings IC, Id, or 2c, 2d with tri-o-phenylene, tri-e,&naphthylene, or mixed phenylene naphthylene ether units are efficient hosts in solid-state complexation of dipolar-aprotic and apolar guests such as nitro compounds and nitriles as well as DMF, DMSO, THF, dioxane, or benzene. X-ray analyses of the solid-state complexes of Id with PhNOz (1:l) and MeCN (1:l) have been studied. It is shown that the presence of the triaryl ether segment induces a biconcave nonequally sided host conformation suitable for guest inclusion. The packing characterizes the host-guest topologies of the two inclusion compounds to be of (H-bonded) cavitate-type for the MeCN case and of interstitial channel type for the PhNOz case. A comparative discussion of the present and previous results support the interpretation of hemispherand preorganization for the new host structures.
Monoorganotin–polyoxometal-compounds. Part IV: Na2[(iPrSn3)(OV)4O10(OH)3]·5H2O·3DMSO, a novel branched tetravanadate(V) stabilized by a trimeric monoorganotin-oxo-hydroxo unit
Inorganica Chimica Acta, 2010
Via self-assembly of the molecular precursors sodium orthovanadate and isopropyltin-dihydroxide-c... more Via self-assembly of the molecular precursors sodium orthovanadate and isopropyltin-dihydroxide-chloride the unprecedented organic–inorganic hybrid polyoxoanion [(iPrSn)3(OV)4O10(OH)3]2− was synthesized in dimethylsulfoxide (DMSO) and isolated as its sodium salt Na2[(iPrSn)3(OV)4O10(OH)3]·5H2O·3DMSO. This spherical nanosized anion is composed of two different structural subunits, a well-known trinuclear monoorganotin-polyoxo-hydroxo unit with octahedrally coordinated tin atoms and a new open-chain, branched isopolyoxo tetravanadate(V) with tetrahedrally coordinated vanadium atoms.
N ‐Tosylaza[2.2]metacyclophan — Darstellung, Struktur, Helicität, Chiroptik, Racemisierung
Chemische Berichte, 1988
Synthesis, structure, helicity, and chiroptical properties of the ten-membered helical N-tosylaza... more Synthesis, structure, helicity, and chiroptical properties of the ten-membered helical N-tosylaza[2.2]metacyclophane 7a are described for the first time. 7a exist in a strained anti conformation, the inner (Hi-) protons of which absorb at high field (4.13, 4.34 ppm). The enantiomers of 7a were enriched by low-pressure chromatography on triacetylcellulose (TAC). Specific rotations, barrier of racemization, and circular dichrograms are discussed with respect to comparison compounds.
Angewandte Chemie, 1995
Achim Miiller Abb. 3. Zusammenstellung einiger in der anorganischen Wirt-Gast-Chemie gebrauchlich... more Achim Miiller Abb. 3. Zusammenstellung einiger in der anorganischen Wirt-Gast-Chemie gebrauchlicher Tektone und Tektonaquivalente. Die Zielverbindung (Zentrum) wird retrosynthetisch in die Tektone (mittlerer Ring) zerlegt, die ihrerseits uber einfache Reaktionen aus den in der Anorganischen Chemie bekannten, stabilen oder als Intermediat vennuteten Tektoniquivalenten (iulierer Ring) zuganglich sein sollten.
Angewandte Chemie, 2002
Die Festkˆrperstruktur des 7-Desaza-2'-desoxyxanthosin-Dihydrats 1 ¥ 2 H 2 O deckt einige interes... more Die Festkˆrperstruktur des 7-Desaza-2'-desoxyxanthosin-Dihydrats 1 ¥ 2 H 2 O deckt einige interessante Befunde auf: Neben einer intramolekularen Wasserstoffbr¸cke (N3-H ¥¥¥ OH-5') treten weitere Wasserstoffbr¸cken auf, die ein supramolekulares Aggregat aus vier Molek¸len 1 stabilisieren. Dabei entsteht ein nahezu flaches Tetramer (Abbildung 1) mit einem ovalen Hohlraum der ungef‰hren Abmessung 9.5 Â 6.5 Â 3.0 ä (AE 0.5 ä). ‹bereinander gestapelte Tetramere bilden eine columnare, Nanorˆhren-artige Struktur (Abbildung 2). Abbildung 1. L‰nge der Wasserstoffbr¸cken im H 2 O-haltigen Tetramer aus vier Molek¸len 1. Abbildung 2. Nanorˆhre aus gestapelten Tetrameren (siehe Abbildung 1). Die Synthese von 1 wurde wie fr¸her beschrieben durchgef¸hrt. 1 kristallisiert aus iPrOH/H 2 O/MeOH (3:1:1) in Gegenwart geringer Anteile Essigs‰ure als Dihydrat in der monoklinen Raumgruppe P2 1 (siehe Hintergrundinformationen). Die Molek¸lstruktur im Kristall zeigt, dass 1 in der 2,4-Dioxoform vorliegt (Abbildung 3); die beiden Oxogruppen liegen etwas au˚erhalb der Ringebene. Der Torsionswinkel c 1 (O4'-C1'-N9-C4), der die Orientierung der Base relativ zum Zuckerrest beschreibt (syn/anti), betr‰gt 61.98; damit liegt das Nucleosid 1 in der syn-Konformation vor. Aus einer ‹bersicht ¸ber nahezu 300 Kristallstrukturanalysen von Nucleosiden geht hervor, dass 1 [
Angewandte Chemie, 1991
Um ein Natrium‐Ion als Templat baut sich die kugelförmige Schale des dodecameren Organozinn‐Sauer... more Um ein Natrium‐Ion als Templat baut sich die kugelförmige Schale des dodecameren Organozinn‐Sauerstoff‐Kations der Titelverbindung auf ‐ siehe Polyederdarstellung rechts, bei der schwarze Punkte Isopropylgruppen symbolisieren. Neben dieser neuartigen anorganischen Wirt‐Gast‐Verbindung ist auch die Struktur des [Ag7I11]‐Anions recht bemerkenswert, das als eindimensionales, verdrilltes Doppelband flächenverknüpfter Iodid‐Tetraeder vorliegt und eine hohe Silber‐Ionen‐Leitfähigkeit erwarten läßt.magnified image
Trimethylene-Bridged Tri- and Tetratin Compounds as Building Blocks for Unusual Double and Triple Ladders
Angewandte Chemie International Edition in English, 1997