TY - JOUR A1 - Franco, O. A1 - Reck, Günter A1 - Orgzall, I. A1 - Schulz, Burkhard A1 - Schulz, B. T1 - Characterization of a new non-centrosymmetric polymorph of diphenyl-1,3,4-oxadiazole N2 - Diphenyl-1,3,4-oxadiazole (DPO) crystallization experiments from solutions clearly reveal the polymorphism of the substance. Besides the formerly known centrosymmetric monoclinic structure with space group P21/c (DPO I) a new monoclinic structure with the non-centrosymmetric space group Cc is found (DPO II): a=2.4134(4) nm, b=2.4099(3) nm, c=1.2879(2) nm,?=110.048(3)°, and V=7.0363(17) nm3. The asymmetric unit contains six independent molecules in a complex packing motif. A re-determination of the crystal structure of DPO I at room temperature gives lattice parameters a=0.51885(6) nm, b=1.8078(2) nm, c=1.21435(14) nm, ?=93.193(3)°, and V=1.1373(2) nm3. X-ray measurements at 363 K show a significant increase of the unit cell volume by 1.6%. Differences between both structures concerning morphology and characteristic Raman bands are outlined in detail. DSC investigations show an irreversible transition from DPO I to DPO II at 97 °C. DPO II does not show any transition in the temperature range up to the melting point at 141 °C. The non-centrosymmetric DPO II structure shows triboluminescence. KW - Diphenyl-1,3,4-oxadiazole KW - X-ray structure KW - Polymorphism KW - Non-centrosymmetric structure PY - 2003 DO - https://doi.org/10.1016/S0022-2860(02)00569-0 SN - 0022-2860 SN - 1872-8014 SN - 0377-046X VL - 649 SP - 219 EP - 230 PB - Elsevier CY - Amsterdam AN - OPUS4-2465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Orgzall, I. A1 - Dietzel, B. A1 - Schulz, Burkhard A1 - Reck, Günter A1 - Schulz, B. T1 - Structural studies on trifluoromethyl substituted 2,5-diphenyl-1,3,4-oxadiazoles N2 - Three new compounds have been synthesized based on the molecular motif 2-[2,6-bis(trifluoromethyl)phenyl]-5-phenyl-1,3,4-oxadiazole, with subsequent CF3-substitution in the ortho-positions of the phenylene ring. The crystal structures of the compounds have been determined by single crystal X-ray diffraction. All compounds have a monoclinic structure. The solid state structure of the compounds is influenced by the electronic properties of the fluorine atoms, leading to the occurrence of C–H...F, and C–F...ϖ interactions, partly replacing ϖ–ϖ interactions usually observed in the crystal structures of 2,5-diphenyl-1,3,4-oxadiazole derivatives. Other significant interactions than those involving fluorine appear only in rare cases. The strong impact of the fluorine atoms on the intra- and intermolecular interactions, and the molecular conformation lead to novel inputs for the understanding of molecular recognition, supramolecular assembly, and crystal packing of fluorine containing compounds. KW - Crystal structure KW - 1,3,4-oxadiazole KW - Molecular conformation KW - Weak interactions PY - 2007 SN - 0022-2860 SN - 1872-8014 SN - 0377-046X VL - 832 IS - 1-3 SP - 124 EP - 131 PB - Elsevier CY - Amsterdam AN - OPUS4-14644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Orgzall, I. A1 - Reck, Günter A1 - Schulz, Burkhard A1 - Stockhause, S. A1 - Schulz, B. T1 - Structures of substituted di-aryl-1,3,4-oxadiazole derivatives: 2,5-bis(pyridyl)- and 2,5-bis(aminophenyl)-substitution N2 - Crystal structures of four different di-aryl-1,3,4-oxadiazole compounds (aryl = 2-pyridyl-, 3-pyridyl-, 2-aminophenyl-, 3-aminophenyl-) are determined. Crystallization of di(2-pyridyl)-1,3,4-oxadiazole yielded monoclinic and triclinic polymorphs. The structures are characterized by the occurrence of π–π interactions. Additionally, in case of the aminophenyl compounds intra- as well as intermolecular hydrogen bonds are found that influence the packing motif as well. Since these molecules are often used as ligands in metal–organic complexes similarities and differences of the molecular conformation between the molecules in the pure crystals and that of the ligands in the complexes are discussed. KW - Crystal structure KW - 1,3,4-Oxadiazole KW - Molecular conformation KW - Hydrogen bonds PY - 2006 DO - https://doi.org/10.1016/j.molstruc.2006.03.076 SN - 0022-2860 SN - 1872-8014 SN - 0377-046X VL - 800 IS - 1-3 SP - 74 EP - 84 PB - Elsevier CY - Amsterdam AN - OPUS4-13799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudert, R. A1 - Schulz, Burkhard A1 - Reck, Günter A1 - Vollhardt, D. A1 - Kriwanek, J. T1 - (Carboxymethyl)dimethylundecylammonium bromide N2 - The title compound, C₁₅H₃₂NO₂⁺.Br⁻, crystallizes to form layers with interdigitating hydrocarbon chains stabilized by Br⁻۰۰۰H—O hydrogen bonds and Br⁻۰۰۰N⁺ contacts. KW - (Carboxymethyl)dimethylundecylammonium bromide KW - Crystal structure PY - 1995 DO - https://doi.org/10.1107/s0108270194011443 SN - 0108-2701 VL - 51 SP - 768 EP - 770 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-56998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vossmeyer, T. A1 - Reck, Günter A1 - Katsikas, L. A1 - Haupt, E. T. K. A1 - Schulz, Burkhard A1 - Weller, H. T1 - A "double-diamond superlattice" built up of Cd17S4(SCH2CH20H)26 clusters N2 - A simple preparation of Cd17S4(SCH2CH2OH)26 clusters in aqueous solution leads to the formation of colorless blocky crystals. X-ray structure determinations revealed a superlattice framework built up of covalently linked clusters. This superlattice is best described as two enlarged and interlaced diamond or zinc blende lattices. Because both the superlattice and the clusters display the same structural features, the crystal structure resembles the self-similarities known from fractal geometry. The optical spectrum of the cluster solution displays a sharp transition around 290 nanometers with a large Absorption coefficient (~84,000 per molar per centimeter). KW - superlattice KW - cluster KW - X-ray structure determination PY - 1995 DO - https://doi.org/10.1126/science.267.5203.1476 SN - 0036-8075 SN - 1095-9203 VL - 267 IS - 5203 SP - 1476 EP - 1479 PB - AAAS, American Association for the Advancement of Science CY - Washington, DC AN - OPUS4-44409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Rikowski, E. T1 - Zur Charakterisierung von Si-Polymeren durch flüssigchromatographische Verfahren in Kopplung mit der MALDI-TOF-MS N2 - Summary. The coupling of the three liquid chromatographic modes with MALDI-TOF mass spectrometry is suitable for the determination of the molecular, functional, and chemical heterogeneities of Si polymers. Silsesquioxanes and siloxanes serve as examples for this method of structure identification. The substance specific construction of the SEC calibration curve by means of MALDI-MS is shown. Zusammenfassung. Die Kopplung der drei flüssigchromatographischen Modi mit MALDI-TOF-Massenspektrometrie ist zur Bestimmung der molekularen, funktionalen und chemischen Verteilungen von Si-Polymeren geeignet. Silsesquioxane und Siloxane dienen als Beispiele für diese Art der Strukturerkennung. Die substanzspezifische Konstruktion einer SEC-Eichkurve mit Hilfe der MALDI-MS wird gezeigt. KW - Si polymer characterization KW - LC/MALDI-TOF-MS PY - 1999 DO - https://doi.org/10.1007/PL00010162 SN - 0026-9247 SN - 1434-4475 VL - 130 IS - 1 SP - 163 EP - 174 PB - Springer CY - Wien AN - OPUS4-2163 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Hauser, K. A1 - Krüger, Ralph-Peter A1 - Schulz, Günter T1 - Macrocycles 12. Ring-Opening Polycondensations of Tin-Containing Macrocycles with Bis(Thioarylester)s N2 - 2,2-Dibutyl-2-stanna-1,3-dioxepane (DSDOP) was polycondensed with bis(4-chlorothiophenyl) suberat under various reaction conditions, but only moderate molecular weights (Mn 10000) were obtained. The MALDI-TOF mass spectrosmetry revealed the formation of cyclic oligo- and polyesters in addition to linear species having OH, CO2H, and unreacted 4-chlorothiophenyl ester endgroups. Furthermore, -Caprolactone (-CL) was polymerized with DSDOP as the initiator at monomer/initiator (M/I) ratios of 20 and 50. The resulting tin-containing macrocyclic polylactones were reacted with sebacic acid bis(4-thiocresyl)ester at three different temperatures and with different reaction times. Analogous polycondensations were conducted with suberic acid bis(4-chlorothiophenyl) ester. The presence of thioarylester endgroups in the isolated polyesters was checked by 1H NMR spectroscopy. The highest conversions were found at long reaction times (24 or 72 hours), or after the addition of pyridine and N,N-dimethylaminopyridine as catalysts. Despite high conversions, the number average molecular weights (Mn's) did not exceed values around 20000. Even in the samples having the highest molecular weights, unreacted 4-chlorothiophenylester endgroups were detected by GPC measurements evaluated with a UV-detector. It is concluded that both factors, cyclization and incomplete conversion, contribute to the limitation of the chain growth. KW - Ring-Opening Polycondensations KW - Macrocycles KW - Polyesters PY - 2000 DO - https://doi.org/10.1081/MA-100101099 SN - 1060-1325 SN - 1520-5738 VL - 37 IS - 4 SP - 379 EP - 394 PB - Taylor & Francis CY - Philadelphia, PA AN - OPUS4-2167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Probst, N. A1 - Schwarz, G. A1 - Schulz, Günter A1 - Krüger, Ralph-Peter T1 - New Polymer Syntheses - 107. Aliphatic Poly(thio ester)s by Ring-Opening Polycondensation of 2-Stanna-1,3-Dithiacycloalkanes N2 - We prepared 2,2-dibutyl-2-stanna-1,3-dithiacycloalkanes from dibutyltin oxide and ,-dimercaptoalkanes. Heterocycles with five-, six-, seven-, or nine-ring members were used as bifunctional monomers for polycondensations with aliphatic dicarboxylic acid chlorides. These polycondensations conducted in bulk were highly exothermic and yielded poly(thio ester)s with number average molecular weights (Mn's) in the range of 5000-30,000 Da. These poly(thio ester)s proved to be rapidly crystallizing materials with melting temperatures in the range of 90-150 °C. In addition to the success of the new synthetic approach, two interesting and unpredictable results were obtained. All volatile species detectable by matrix assisted laser desorption induced-time of flight (MALDI-TOF) mass spectrometry were cyclic oligo- and poly(thio ester)s. Second, several polyesters showed a reversible first-order change of the crystal modification as identified by differential scanning calorimetry measurements and X-ray scattering with variation of the temperature. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 3656-3664, 2000 KW - Poly(thio-ester)s KW - Ring-opening polycondensation KW - Macrocycles KW - Change of crystal structure PY - 2000 DO - https://doi.org/10.1002/1099-0518(20001001)38:19<3656::AID-POLA190>3.0.CO;2-M SN - 0360-6376 SN - 0887-624X VL - 38 IS - 19 SP - 3656 EP - 3664 PB - Wiley CY - Hoboken, NJ AN - OPUS4-2170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reuther, F. A1 - Krüger, Ralph-Peter A1 - Schulz, Günter A1 - Baehr, G. A1 - Westerwelle, U. A1 - Gruetzner, G. ED - Houlihan, F. M. T1 - Tailored novolak resins for advanced photoresists by a two-step procedure - new insight into the molecular structure by coupling GPC and MALDI-TOF-MS T2 - 17th Annual SPIE Conference on Advances in Resist Technology and Processing CY - Santa Clara, CA, USA DA - 2000-02-28 KW - Novolak KW - Structure KW - Synthesis KW - Gel permeation KW - Chromatography KW - MALDI-TOF-MS PY - 2000 SN - 0-8194-3617-8 SN - 1605-7422 N1 - Serientitel: SPIE proceedings series – Series title: SPIE proceedings series IS - 3999 SP - 464 EP - 471 PB - SPIE CY - Bellingham AN - OPUS4-2171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reck, Günter A1 - Orgzall, I. A1 - Schulz, B. A1 - Dietzel, B. T1 - Two polymorphic forms of 2,5-bis(4-methoxycarbonylphenyl)-1,3,4-oxadiazole N2 - In the title compound, C13H14BN3O, the aziridine ring is an almost equilateral triangle, the C—C distance being slightly shorter than the C—N distances, probably because of the dative B—N bond. The five-membered ring, composed of two C atoms and N, B and O atoms, is fused with the aziridine ring to form a six-membered ring with a chair conformation. PY - 2003 DO - https://doi.org/10.1107/S0108270103022698 SN - 0108-2701 SN - 1600-5759 VL - 59 SP - o634 EP - o635 PB - Blackwell Publ. CY - Oxford AN - OPUS4-2694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Günter A1 - Starfinger, Käthe T1 - Pilzwidrige Wirksamkeit verschiedener Steinkohlenteeröle PY - 1961 SN - 0417-2000 VL - 48 SP - 53 EP - 56 PB - Deutsche Gesellschaft für Holzforschung CY - München AN - OPUS4-10112 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Determination of functionality and molar mass distribution of aliphatic polyesters by orthogonal liquid chromatography, Part I: Off-line investigation of poly-(1,6-hexanediol adipates) PY - 1994 SN - 0148-3919 VL - 17 SP - 3069 EP - 3090 PB - Dekker CY - New York, NY AN - OPUS4-2139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - New Results of Determination of Polymer Heterogeneity by Two-Dimensional Orthogonal Liquid Chromatography T2 - International GPC Symposium CY - Lake Buena Vista, FL, USA DA - 1994-06-05 PY - 1994 SP - 273 EP - 275 PB - Gordon and Breach CY - St. Helier, Jersey AN - OPUS4-2140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachsen, O. A1 - Reichert, K.H. A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Thermal decomposition of biodegradable polyesters - III. Studies on the mechanisms of thermal degradation of oligo-L-lactide using SEC, LACCC and MALDI-TOF-MS PY - 1997 SN - 0141-3910 SN - 1873-2321 VL - 55 SP - 225 EP - 231 PB - Applied Science Publ. CY - London AN - OPUS4-2154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leitner, M.B. A1 - Schinkel, G. A1 - Springer, J. A1 - Ruhmann, R. A1 - Schulz, Günter A1 - Niesel, F.T. T1 - Methacrylate copolymers containing azoanthraquinone units: synthesis by direct copolymerization and by polymer-analogous esterfication reaction PY - 1997 SN - 1381-5148 SN - 1873-166X VL - 33 SP - 137 PB - Elsevier CY - Amsterdam AN - OPUS4-2155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Determination of polymer heterogeneity by two-dimensional orthogonal liquid chromatography KW - Orthogonal chromatography KW - Size exclusion chromatography KW - Liquid adsorption chromatography at critical conditions KW - Matrix-assisted laser desorption ionization time-of-flight mass spectrometry KW - Polyester KW - Polyether PY - 1996 SN - 1023-666X SN - 1563-5341 VL - 2 SP - 221 EP - 235 PB - Gordon and Breach Publ. CY - Amsterdam AN - OPUS4-2146 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leukel, J. A1 - Burchard, W. A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Mechanism of the anionic copolymerization of anhydride- cured epoxies-analysisted by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF-MS) PY - 1996 SN - 1022-1336 SN - 1521-3927 VL - 17 SP - 359 EP - 366 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-2148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Bestimmung der Polymerheterogenität durch Kopplung von HPLC und MALDI-TOF-MS KW - Zweidimensionale Flüssigchromatographie KW - Flugzeit-Massenspektrometrie KW - Synthetische Polymere PY - 1996 SN - 0016-3538 VL - 40 IS - 4 SP - 398 EP - 402 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-2149 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Wachsen, O. T1 - New aspects of determination of polymer heterogeneity by 2-dimensional orthogonal liquid chromatography and MALDI-TOF-MS PY - 1996 SN - 1022-1360 SN - 0258-0322 SN - 1521-3900 VL - 110 SP - 155 EP - 176 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-2150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mix, Renate A1 - Gähde, J. A1 - Goering, Harald A1 - Schulz, Günter T1 - Segmented polyurethanes with 4,4-bis-(6-hydroxyhexoxy)biphenyl as chain extender - Part 2. Synthesis and properties of MDI-polyurethanes in comparison with 2,4-TDI-polyurethanes N2 - Linear segmented polyurethanes based on poly(butylene adipate)s (PBA) of different molecular weight (Mn 2000, 1000, and 600), 4,4-diphenylmethane diisocyanate (MDI) and the mesogenic diol 4,4-bis-(6-hydroxyhexoxy)biphenyl (BHHBP) as well as the unsegmented polyurethane consisting of MDI/BHHBP units have been synthesized and characterized by elemental analysis, 13C-NMR and SEC. The thermal behavior and the morphology were studied by DSC, polarizing microscopy, and DMA. The properties of the MDI-polyurethanes were discussed in relation to the BHHBP chain extended 2,4-TDI-polyurethanes and common 1,4-butanediol chain-extended MDI products. MDI polyurethanes based on PBA (Mn 2000) exhibit a glass transition temperature Tg of about -40°C independent of the hard segment content up to 50% hard segments. At higher hard segment contents increasing Tgs were observed. Polyurethanes, based on the shorter polyester soft segments PBA (Mn 1000 or 600), reveal an increase in the glass transition temperatures with growing hard segment content. The thermal transitions caused by melting of the MDI/BHHBP hard segment domains are found at 50 K higher temperatures in comparison with the analogous TDI products with mesogenic BHHBP/TDI hard segments. Shortening of the PBA chain length causes a shift of the thermal transitions to lower temperatures. Polarizing microscopy experiments indicate that liquid crystalline behavior is influenced by both the content of mesogenic hard segments and the chain length of the polyester. © 1996 John Wiley & Sons, Inc. PY - 1996 DO - https://doi.org/10.1002/(SICI)1099-0518(19960115)34:1<33::AID-POLA3>3.0.CO;2-4 SN - 0360-6376 SN - 0887-624X VL - 34 IS - 1 SP - 33 EP - 44 PB - Wiley CY - Hoboken, NJ AN - OPUS4-2151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter ED - Günther, W. T1 - Strukturaufklärung von heterogenen Polymeren durch zweidimensionale Flüssigchromatographie und MALDI-TOF-Massenspektrometrie T2 - InCom '94 - International Symposium on Instrumentalized Analytical Chemistry and Computer Technology CY - Düsseldorf, Deutschland DA - 1994-03-14 PY - 1994 VL - 94 PB - InCom-Bureau CY - Düsseldorf AN - OPUS4-2195 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -