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1996 (295)
201Author    Z. NaturforschRequires cookie*
 Title    E nan tioselective Catalysis  
 Abstract    , 101 [1] Synthesis and C oordination Properties o f (3 'S ,4 'S)-(+)-l,2 -B is(3 ',4 '-d im eth o x y -p h osp h olan o)b en zene, a N ew Chiral D iphosphane H e n ri B ru n n e r* , G e m m a N e t A new bisphospholane, BDPB, derived from 1,2-bisphosphanobenzene and tartaric acid as well as the complex [Rh(CO D)(BD PB)]PF6 were syn­ thesized. The strong binding of BDPB to metals and the presence of four functional groups in the periphery of the molecule make this bisphospho­ lane a good starting point for new expanded bis­ phosphanes. 
  Reference    Z. Naturforsch. 51b, 1210—1212 (1996); received February 5. 1996 
  Published    1996 
  Keywords    Chiral Bisphosphanes Expanded Phosphanes, Rhodium Complexes, Cyclic Sulfates 
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 Identifier    ZNB-1996-51b-1210_n 
 Volume    51 
202Author    N.Requires cookie*
 Title    N eu e Verbindungen mit C eN iSi2-Struktur  
 Abstract    ew C o m p o u n d s w ith C e N iS i2-Type S tru c tu re D irk Jo h re n d t, C h ristin e Lux, A lb re c h t M ew is The compounds BaPdA s, (a = 4 .6 7 8 (1). b -1 7 .3 3 0 (2). c = 4 .5 7 4 (1) A), BaPdSb2 (,a = 4 .8 7 7 (1). b = 1 8 .5 8 3 (2). c = 4 .8 8 9 (1) Ä) and BaPtA s, {a = 4 .6 6 0 (1), b = 1 7 .1 1 9 (2). c = 4 .6 0 8 (1) Ä) were pre­ pared by heating mixtures of the elements and investigated by X-ray methods. They are isotypic and crystallize in the CeNiSi2-type structure (Cmcm), also called the BaCuSn2-type. 
  Reference    Z. Naturforsch. 51b, 1213—1214 (1996); eingegangen am 1. März 1996 
  Published    1996 
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 Identifier    ZNB-1996-51b-1213_n 
 Volume    51 
203Author    Z. NaturforschRequires cookie*
 Title    Elektronentransfer und Ionenpaar-Bildung  
 Abstract    , 47 [1] Titrationen von 1,2,4,5-Tetracyanbenzol und 7,7,8,8-Tetracyan-/;-chino-dimethan mit Natriummetall in aprotischen Lösungen E le ctro n T ran sfer an d Ion P air F o rm atio n , 47 [ 1 ] T itratio n s o f 1,2 ,4 ,5 -T etracy an o b en zen e and 7 ,7 ,8 ,8 -T etracy an o -/?-q u in o d im eth an e w ith S o d iu m M etal in A p ro tic S o lu tio n s H an s B ock*, M a rk u s K leine 
  Reference    Z. Naturforsch. 51b, 1215—1221 (1996); eingegangen am 25. Januar 1996 
  Published    1996 
  Keywords    1, 2, 4, 5-Tetracyanobenzene, 7, 7, 8, 8-Tetracyano-/?-quinodimethane, Sodium Metal Reduction, UV/VIS Spectra 
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 Identifier    ZNB-1996-51b-1215 
 Volume    51 
204Author    Hans Bock, Markus KleineRequires cookie*
 Title    Elektronentransfer und Ionenpaar-Bildung, 48 [1] Titrationen von Tetraphenyl-/?-benzochinon mit Natrium-und Kaliummetall in aprotischen Lösungen Electron Transfer and Ion Pair Formation, 48 [ 1 ] Titrations of Tetraphenyl-/?-benzoquinone with Sodium and Potassium Metals in Aprotic Solutions  
  Reference    Z. Naturforsch. 51b, 1222—1228 (1996); eingegangen am 25. Januar 1996 
  Published    1996 
  Keywords    benzoquinone Reduction, Alkaline and Alkaline Earth Metals, Aprotic Solution, UV/VIS Spectra 
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 Identifier    ZNB-1996-51b-1222 
 Volume    51 
205Author    WilhelmV. Dahlhoffd, Karin Radkowskia, Ingo Dierkingb, Peter ZugenmaierbRequires cookie*
 Title    Amphiphilic Carbohydrate-Based Mesogens, 12 [1] High-Yield Synthesis of Mesogenic l-O-Alkanoyl-D/L-Xylitols  
 Abstract    The equilibrium mixture of 1,2:3,4-and l,3:2,4-di-0-ethylboranediyl-D /L-xylitols 1 and 1' obtained on reaction o f three equivalents of xylitol with two equivalents of triethylboroxin, reacts with alkanoyl chlorides (heptanoyl-dodecanoyl) to give equilibrium mixtures of the O-ethylboranediyl protected l-O-alkanoyl-D.L-xylitols 2,2' after vacuum distillation. Depro­ tection of the latter affords the title amphiphilic esters 3 which melt to give the smectic A liquid-crystalline phase. 
  Reference    Z. Naturforsch. 51b, 1229—1234 (1996); received April 26 1996 
  Published    1996 
  Keywords    Carbohydrates, Amphiphiles, Liquid Crystals (Smectic), 1-0-A lkanoyl-D, L-X ylitols, X-Ray 
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 Identifier    ZNB-1996-51b-1229 
 Volume    51 
206Author    M. Wachhold, W. S. SheldrickRequires cookie*
 Title    Methanolothermale Synthese von Cs4As2Te6, des ersten Alkalimetall- Telluridoarsenats mit As-As-und Te-Te-Bindungen Methanolothermal Synthesis of Cs4As2Te6, the First Alkali Metal Telluridoarsenate with As-As and Te-Te Bonds  
 Abstract    Reaction of Cs2C 0 3 and As2Te3 in methanol at 145°C affords the telluridoarsenate(II) Cs4As2Te(,. A trans conformation is observed for the centrosymmetric As2Te^~ anions, which consist of two t/>-tetrahedralo As(As)(Te2)Te units with a common As-As bond. The terminal As-Te distance of 2.554(2) A is much shorter than the As-Te distance of 2.691(2) A to the Te2 unit, which exhibits a Te-Te bond length of 2.744(2) A. Both of the independent cations are coordinated in an irregular manner by eight Te atoms. 
  Reference    Z. Naturforsch. 51b, 1235—1239 (1996); eingegangen am 29. April 1996 
  Published    1996 
  Keywords    Cesium, Telluridoarsenate(II), Methanolothermal Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1235 
 Volume    51 
207Author    Heide Kraudelt, Uwe Schilde, Heike Hefele, Eberhard Ludwig, Erhard UhlemannRequires cookie*
 Title    Titan-und Vanadiumkomplexe mit 4-[l-(N '-Benzoylhydrazino)-l-phenyl- methyliden]-3-methyl-l-phenyl-pyrazol-5-on. Röntgenkristallstruktur von 4-[l-(N ,-Benzoylhydrazino)-l-phenyl-methyliden]-3-methyl-l- phenyl-pyrazol-5-on Titanium-and Vanadium Complexes of 4-[l-(N'-Benzoylhydrazino)-l-phenyl- methylidene]-3-methyl-l-phenyl-pyrazol-5-one. Structure of 4-[l-(N'-Benzoyl- hydrazino)-1 -phenyl-methylidene]-3-methyl-1 -phenyl-pyrazol-5-one  
 Abstract    Benzoylhydrazone of l-Phenyl-3-methyl-4-benzoyl-pyrazol-5-one, Titanium(IV) and Vanadi-um(IV) Chelates, IR Spectra, n C NMR Spectra, Crystal Structure By reaction of l-phenyl-3-methyl-4-benzoyl-pyrazol-5-one with benzoylhydrazine the tridentate diacidic ligand 4-[l-(N'-benzoylhydrazino)-l-phenyl-m ethylidene]-3-m ethyl-l-phenyl-pyrazol-5-one (H2L) is formed which gives complexes M L2 with tetravalent titanium and vanadium ions. The ligand and its complexes were characterized by mass spectroscopy. The vanadium(IV) complex can be oxidised and reduced electrochemicallv. The chemical bonding in the titanium(IV) complex and in the ligand was studied by IR and C NMR spectroscopy. The molecular structure of 4-[l-(N '-benzoylhydrazino)-l-phenyl-m ethylidenel-3-m ethyl-l-phenyl-pyrazol-5-one was determined by X-ray analysis. Crystal data: a = 9.159(3) A, b = 11.014(4) A, c = 11.136(5) Ä, a = 90.11 (2)°, ß = 101.84(3)°, 7 = 113.01 (2)°; space group PI, Z = 2. 
  Reference    Z. Naturforsch. 51b, 1240—1244 (1996); eingegangen am 18. März 1996 
  Published    1996 
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 Identifier    ZNB-1996-51b-1240 
 Volume    51 
208Author    Wolfgang Czado, Ulrich MüllerRequires cookie*
 Title    (PPh4)4Sb8Br28 Tetraphenylphosphonium Ikosioctabromooctaantimonate(III), (PPh4)4Sb8Br28  
 Abstract    The title compound was obtained by the reaction of PPh4Br, Sb2Se3, and bromine in dichloro-methane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1249.1(2), b = 1307.8(2), c = 2152.3(4) pm, a = 102.93(2), ß = 100.83(2), 7 = 100.42(2)°, Z = 2, triclinic, space group P I . (PPh4)4Sb8Br28 is isotypic with (PPh4)4Sb8I28. The Sb8Br284~ ion can be taken as the association product of eight SbBr3 molecules with four B r-ions. Each Sb atom has a distorted octahedral coordination with three shorter (252 to 274 pm) and three longer (300 to 353 pm) Sb-Br bonds. The octahedra share common edges in two parallel rows of four octahedra each. The arrangement of the 28 bromine atoms corresponds to a section of a closest packing of spheres. Tetraphenylphosphonium-ikosioctabromooctaantimonat(III), 
  Reference    Z. Naturforsch. 51b, 1245—1247 (1996); eingegangen am 22. März 1996 
  Published    1996 
  Keywords    Ocataikosabromooctaantimonate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1245 
 Volume    51 
209Author    Rainer Pöttgen, Gunter KotzybaRequires cookie*
 Title    Ti2Ni2In, Zr2Co2In, and Zr2Pd2In -Intermetallic Compounds with Ordered U3Si2 and Zr3Al2 Type Structure  
 Abstract    T i:N i2ln, Zr2Co2ln, and Zr^Pd^In were synthesized by reacting the elements in an arc-melting furnace and subsequent annealing at 1070 K. The compounds were investigated by X-ray diffraction on both powders as well as single crystals. Z rC o iIn adopts the ordered U jSi: type structure: P4/mbm, a = 720.54(7), c = 331.59(4) pm. The structure consists of planar [Co2lnj layers with C02 dumb-bells which are separated by the zirconium atoms. Ti2Ni2ln and Z n P d 2ln crystallize with the ordered Z riA b type structure (space group P42/mnm), a superstructure of U?Si2: a = 694.3(2), c = 623.2(2) pm for TioNi^In and a = 746.0(1), c = 686.1(1) pm for Zr2Pd2ln. The Ni2 and Pd2 dumb-bells in the Ni2ln and Pd2ln layers of Ti2Ni2In and Z n P ^ I n are shifted from the mirror planes of the subcell resulting in puckered layers with weak interlayer Ni-Ni and Pd-Pd contacts, respectively. The indium atoms in these compounds occupy [Tis] and [Zr*] square prisms while the transition metal atoms are surrounded by [Tia] and [Zr6] trigonal prisms. These structural fragments are derived from the CsCl and AIB2 type structures. Chemical bonding in these intermetallic compounds is briefly discussed. Magnetic susceptibility measurements of compact polycrystalline samples indicate Pauli paramagnetism. 
  Reference    Z. Naturforsch. 51b, 1248—1254 (1996); received February 29 1996 
  Published    1996 
  Keywords    Intermetallic Compounds, Crystal Structure, Pauli Paramagnetism 
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 Identifier    ZNB-1996-51b-1248 
 Volume    51 
210Author    H. Schumann, B. Neumann, H.-G StammlerRequires cookie*
 Title    Spektroskopische und strukturelle Aspekte der Protonierung von Tetraaza[14]annulen-Dianionen Spectroscopic and Structural Aspects of the Protonation of Tetraaza[14]annulene Dianions  
 Abstract    The effects of increasing protonation upon two [ 14]annulene dianions prepared by reaction of LiCH3 with 5,14-dihydro-6,8,15,17-tetram ethyldibenzo[b,i][l,4,8,l l]tetraazacyclotetradecine 
  Reference    Z. Naturforsch. 51b, 1255—1266 (1996); eingegangen am 8. Februar 1996 
  Published    1996 
  Keywords    Nickel Complexes, Macrocyclic Ligands, Protonation, 7r-Conjugation, X-Ray 
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 Identifier    ZNB-1996-51b-1255 
 Volume    51 
211Author    Norbert Kuhna, Hans Bohnena, Gerald Henkelb, Jörg KreutzbergbRequires cookie*
 Title    5-Tetramethyl-2-methylenimidazoline -an Olefin with Ylidic Properties [ 1]  
 Abstract    A facile synthesis of l,3,4,5-tetramethyl-2-methylenimidazoline 5 (Im) starting from the pentamethylimidazolium ion (8) and KH is described. Boranes react with 5 to give the adducts ImBHi (11) and ImBF3 (18). With Mel and CH3C(0)C1 the imidazolium salts ImMe+ (19) and Im C (0)M e+ (20) are obtained. CS2 gives the zwitterionic compound ImCS2 (24) which is transformed into the cationic thiocarboxylic ester ImC(S)SCH2Cl+ on treatment with CH2C12. Reaction with chlorotrimethylsilane gives the imidazolium ion ImSiMe^ (26) which may be transferred into the disilylated imidazolium ion 28 via deprotonation and subsequent silylation, the silylated olefin 27 being the intermediate. Similarly, the cations ImSiR2Cl+ (29; R = Me, Ph) are obtained from 5 and the silanes R2SiCl2. The neutral adduct ImSnPh2Cl2 (32) is formed in the reaction of 5 with Ph2SnCl2. Iodine reacts with 5 to give the charge-transfer adduct Im l2 (35), which can be further transferred into the imidazolium salt Im l+I^ (36). verhilft Imidazolin-Derivaten des Typs 1 durch die Dominanz der Grenzstruktur 2 zu einer Ylid-artigen Bindungssituation. Als Belege können die Eigen­ schaften der 2-Chalkogenoimidazoline 1 (X = S [3,41, Se [4 -6 ], Te [4,7]) sowie des 2-Iminoimi-dazolins 3 (1 ,8 ] gelten. Die bekannte Polarisierung der olefinischen Dop­ pelbindung durch Substituenten mit +M-Charak-ter ist im Falle der Enamine [9] gut untersucht; durch Einbindung der Stickstoff-Atome des 1,1-Endiamins 4 in ein fünfgliedriges Ringsystem wird eine bemerkenswert hohe Basizität des Methylen­ kohlenstoffs erreicht [10]. Hierzu analog läßt sich durch Einbau eines olefinischen Kohlenstoffs in ein System zyklisch konjugierter 7 r-Elektronen gleich­ falls eine starke Polarisierung der olefinischen Dop­ pelbindung erreichen [11]. Die Kombination beider Effekte führt zum System des 2-Methylenimidaz-olins. Synthese und strukturelle Charakterisierung des Tetramethyl-Derivats 5 sind Gegenstand einer vorläufigen Mitteilung [12]. Über die Kupplungsre­ aktion von 5 zum Methinium-Kation 6 [13] sowie seine koordinationschemische Fixierung an Metall­ zentren (7) [14, 15] haben wir bereits an anderer Stelle berichtet. 
  Reference    Z. Naturforsch. 51b, 1267—1278 (1996); eingegangen am 8. März 1996 
  Published    1996 
  Keywords    Imidazoles, Olefins, X-Ray 
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 Identifier    ZNB-1996-51b-1267 
 Volume    51 
212Author    M. Staack, Hk Müller-BuschbaumRequires cookie*
 Title    Zur Kenntnis des Kupfer-Oxid-Arsenats Cu40 (A s 0 4)2 On the Copper Oxide Arsenate Cu40 (A s 0 4)2  
 Abstract    The copper oxide arsenate Cu40 (A s0 4)2 has been prepared and investigated by single crystal X-ray techniques. The compound crystallizes with triclinic symmetry, space group C '-P l, a = 6.4148(7), b = 7.6549(5), c = 8.2241(7) A, a = 98.52(1), ß = 112.39(1), 7 = 98.38(1)°, Z = 2. Cu40 (A s 0 4)2 is isotypic to C u^(P04)20 . Copper ions on one of the four specified sites show nearly planar coordination by 0 ~~ and may be assigned to the anionic part of the crystal structure. One of the nine different types of oxygen atoms is coordinated by copper exclusively. The compound is therefore classified as an oxide arsenate. 
  Reference    Z. Naturforsch. 51b, 1279—1282 (1996) 
  Published    1996 
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 Identifier    ZNB-1996-51b-1279 
 Volume    51 
213Author    Max Herberhold, E. Bertholdt, WolfgangM. Iliu, BerndW. RackmeyerRequires cookie*
 Title    N-Functionalization of the Tetrahedrane Fe2(CO)6(/z-SNH)  
 Abstract    The azadiferrathia tetrahedrane, Fe2(CO)6(£/-SNH) (1), was deprotonated to give the anion [Fe2(CO)6(/J-SN)]_ (2) which reacts with halides of phosphorus, arsenic, silicon, germanium, tin and boron by formation of element-nitrosen bonds. The new compounds were characterized by their IR. N M R ('H , mB, i3C, i5N, 29S i,3 P, m S n)and mass spectra. The molecular structure of [Fe2(CO)6(A/-SN-SiMe2CH2-)]2 (11) was determined by X-ray structure analysis (space group P i; triclinic; a = 799.8(2), b = 958.5(2), c = 1035.7(2) pm, a = 86.30(2)°, (3 = 81.27(2)°, 7 = 69.90(2)°). 
  Reference    Z. Naturforsch. 51b, 1283—1289 (1996); received March 27 1996 
  Published    1996 
  Keywords    Azadiferrathia, Tetrahedrane, Cluster Anion, Element-Nitrogen Bonds, NMR Spectra 
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 Identifier    ZNB-1996-51b-1283 
 Volume    51 
214Author    C. Wadewitz, Hk Müller-BuschbaumRequires cookie*
 Title    Strukturelle Unterschiede zwischen Sr2(V 0)(A s04)2 und Ba2(V 0)(P 04)2 Strucural Differences between Sr2(V 0 )(A s0 4)2 and Ba2(V 0 )(P 0 4)2  
 Abstract    Two new alkaline earth vanadyl compounds, Sr2(V 0)(A s 0 4)2 (I) and Ba2(V 0)(P 0 4)2 (II), have been prepared by solid state reactions in closed quartz tubes and characterized by sin­ gle crystal X-ray diffraction methods. Crystal data: (I): monoclinic, C ,h -12/a, a = 6.873(2), b = 16.307(4), c = 7.196(2) A, ß = 115.67(2), Z = 4; (II): monoclinic, C^-I2, a = 9.471(2), b = 5.443(1), c = 16.972(4) Ä, ß = 101.65(2), Z = 4. (I) is isotypic to Sr2(V 0)V 20 8 and Sr2(V 0)(P 0 4)2. (II) shows significant differences to the strontium compounds as well as to Ba2(V 0)(V 0 4)2. The differences of the crystal chemistry and the similarity of (II) to Ba2(V 0)(P 0 4)2 H20 are discussed. 
  Reference    Z. Naturforsch. 51b, 1290—1294 (1996); eingegangen am 26. April 1996 
  Published    1996 
  Keywords    Barium, Strontium, Vanadium, Phosphorus, Arsenic, Oxygen, Crystal Structure 
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 Identifier    ZNB-1996-51b-1290 
 Volume    51 
215Author    Stephan Friederichs, Jens Kudnig, Günter KlarRequires cookie*
 Title    Elementorganische Verbindungen mit o-Phenylenresten, XXVIII [1] Charge-transfer  
 Abstract    Komplexe von 2,3,7,8-Tetraalkoxy-chalkogenanthrenen mit 7,7,8,8-Tetracyan-2,3?5,6-tetrafluor-chinodimethan Organometalloidal Compounds with o-Phenylene Substituents, Part XXVIII [1] Charge-Transfer Complexes of 2,3,7,8-Tetraalkoxy-chalcogenanthrenes wjth 7.7.8.8-Tetracyano-2,3,5,6-tetrafluoro-quinodimethane -selenanthrene, as well as -tetraethoxythianthrene gi­ ve isostructural 1:1 charge-transfer complexes with 7,7,8,8-tetracyano-2,3,5,6-tetrafluoro-quinodimethane. In the columnar crystal structures there are alternating donor and acceptor molecules. The chalcogenanthrene molecules which are folded at their E -E axes in the pure state, are planar in the complexes indicating a charge-transfer according to [donor]+ [acceptor]-. Consecutive molecules of the stacks are arranged in such a way that an optimum overlap of the HOMO of the donor and the LUMO of the acceptor, both of which are of 7T-type character according to MNDO calculations, is secured. 
  Reference    Z. Naturforsch. 51b, 1295—1300 (1996); eingegangen am 1. April 
  Published    1996 
  Keywords    Tetracyano-2, 3, 5, 6-tetrafiuoro-quinodi-methane, 1:1 Charge-Transfer Complexes, Columnar Structures, MNDO Calculations 2, 3, 7, 8-Tetramethoxythianthrene and 
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 Identifier    ZNB-1996-51b-1295 
 Volume    51 
216Author    Matthias Asbrand, Brigitte EisenmannRequires cookie*
 Title    Ein neues Baumuster für ein heteronukleares 11 -Valenzelektronensystem: gefaltete ^ [SnBi]2~-Zickzack-Ketten in der Struktur von K2[SnBi] A Novel Structure Pattern for a Heteronuclear 11 Valence Electron System: Folded ^ [SnBi]2" Zigzag Chains in the Structure of K2[SnBi]  
 Abstract    The compound K2[SnBi] was prepared by reaction of stoichiometric amounts of the elements in graphitized quartz ampoules. K2[SnBi] crystallizes in the orthorhombic system, space group Pbcm (No 57), Z = 4, with a = 680,4(3), b = 1339,(4) and c = 649,9(3) pm. The crystal structure of K2[SnBi] is characterized by folded infinite [SnBi] zigzag chains of alternating Sn and Bi atoms. The chains are bent at each Bi atom, the Sn atoms are located at the fold of the chain. Apart from the two covalent Sn-Bi bonds, each Sn atom has two additional collinear Sn-Sn contacts in direction of the fold of the chain which in terms of partial bonds can be assigned a bond order of one half. The repeating unit of the chain [Sn2Bi2]4_ is strongly related to the isoelectronic butterfly [Si4]6-in Ba3Si4. 
  Reference    Z. Naturforsch. 51b, 1301—1304 (1996); eingegangen am 8. März 1996 
  Published    1996 
  Keywords    Dipotassium Bismutidostannate, Preparation, Crystal Structure, Tin-Bismuth Chain 
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 Identifier    ZNB-1996-51b-1301 
 Volume    51 
217Author    S.Requires cookie*
 Title    Stereoselektive Pudovik-Reaktion von 5,6-Benzo-2//-l-methyl-3- (2'-chlorethyl)-2-oxo-l,3,2i4-diazaphosphorin-4-on mit einem 3-Thiazolin und MPL-chromatographische Isolierung des Überschußdiastereomers  
 Abstract    te re o se le c tiv e Pudovik R e a c tio n o f 5 ,6 -B e n z o -2 //-l-m e th y l-3 -(2 '-c h lo ro eth y l)-2 -o x o -l,3 ,2 A 4-d ia z a p h o sp h o rin -4 -o n e w ith a 3 -T h iaz o lin e an d M P L -C h ro m a to g ra p h ic a l Iso latio n o f th e M a jo r D ia s te re o m e r H a ra ld G rö g e r, Jö rg W ilk e n , Jü rg e n M a rte n s* Io n N e d a , V asily P in ch u k , H o lg e r T h ö n n e sse n , P e te r G. Jones, R e in h a rd S chm u tzler* 5,6-Benzo-2f/-l-m ethyl-3-(2'-chloroethyl)-2-oxo-l,3,2A4-diazaphosphorin-4-one, 3-Thiazoline Adducts, Pudovik Reaction, MPLC Technique, X-Ray The modified Pudovik reaction of 5,6-benzo-2//-l-methyl-3-(2'-chloroethyl)-2-oxo-l,3,2A4-diazaphosphorin-4-one with a 3-thiazoline furnishing the corresponding 5,6-benzo-2/Y-l-me-thyl-3-(2'-chloroethyl)-2-oxo-2-(3-thiazolidin-4-yl)-l,3,2)i4-diazaphosphorin-4-one 4 and the medium pressure liquid column chromatographical (MPLC) isolation of the major diastereo­ mer is described. The relative stereochemistry at the centres PI and Cl was determ ined by X-ray structure determ ination of three racemic modifications (a total of seven independent molecules). 
  Reference    Z. Naturforsch. 51b, 1305—1312 (1996); eingegangen am 4. März 1996 
  Published    1996 
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 Identifier    ZNB-1996-51b-1305 
 Volume    51 
218Author    G. Jo, EsRequires cookie*
 Title    Polysulfonylamine  
 Abstract    , LXXVI [1] Zwei supramolekulare Isomere im gleichen Kristall: Darstellung und Struktur des monomeren 18-Krone-6-Komplexes (CH2CH20) 6-2 M eN (S02M e)(S02Ph) P o lysulfonylam ines, L X X V I [1] O c c u rre n c e o f Two S u p ra m o le c u la r Iso m ers in O n e C rystal: S y nthesis a n d S tru c tu re o f th e M o n o m e rie 18-C row n-6 C o m p lex (C H 2C H 20) 6 -2 M e N (S 0 2M e) (S 0 2P h) D a g m a r H en sc h el, O liv er H iem isch , A rm a n d B lasc h ette* , P e te r N-M ethyl(benzenesulfonyl)(methanesulfonyl)amine, N-M ethyldi(fluorosulfonyl)amine, 18-Crown-6, Binary Complexes of Uncharged Molecules, Supramolecular Isomerism The title complex, obtained by co-crystallization of its molecular com ponents from m etha­ nol, was characterized by low-temperature X-ray diffraction. The crystal structure (triclinic, space group P I, Z = 2) consists of two monomeric and crystallographically centrosymmetric formula units A and B which may be classified as supramolecular stereo-and/or linkage isomers. In both units, the receptor rings adopt the frequently observed D ?(/ pseudosymmetry, and the symmetry-related substrate molecules are situated above and below the polyether rings. The isomerism of the supermolecules arises from markedly different confomations of their substrate components. In B, the methyl groups display a transoid orientation (torsional angle for C -N -S -C : 135.5°) and the N-methyldisulfonylamine is solely attached by three S -C -H -O interactions to a set of three alternating crown oxygen atoms. In isomer A, the C — N — S — Cmethyi sequence is cisoid (torsional angle: 83.1°) and the substrate is connected to the crown ether by three S -C -H — O bonds and an additional N -C -H -O interaction. The H -O distances and C -H -O angles of the seven independent hydrogen bonds lie within the intervals 230-260 pm and 140-180°, respectively. A supermolecule in­ volving M eN (S 02Ph)2 and 18-crown-6 could not be isolated, whereas the binary complex (CH 2CH 20) 6-2 M eN (S02F)2 is readily obtained by co-crystallization of the components. The latter complex showed severe disorder of the N (S 0 2F)2 moieties and its structure could not be refined satisfactorily. 
  Reference    Z. Naturforsch. 51b, 1313—1319 (1996); eingegangen am 30. April 1996 
  Published    1996 
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 Identifier    ZNB-1996-51b-1313 
 Volume    51 
219Author    Z. NaturforschRequires cookie*
 Title    ,1-Organoboration of Sterically Hindered Tetra-l-alkynylsilanes and the Crystal Structure of Tetrakis[l-(3,3-dimethyl)butynyl]silane  
 Abstract    Tetra-l-alkynylsilanes, Si(C sC R *)4 with R 1 = 'Bu (1) and SiMe3 (2) react with triethyl-borane, E t3B. by intermolecular 1,1-ethyloboration followed by intramolecular 1.1-vinylo-boration. to give the substituted siloles 3 and 5 with two R 'C = C groups linked to silicon. The formation of 5 (R 1 = SiMe3) requires exactly one equivalent of E t3B, whereas 3 (R 1 = 'Bu) is formed after = 2 0 d in boiling toluene in the presence of a large excess of E t3B, and the remaining 'B u -C = C groups in 3 do not react with E t3B. The 1,1-organoboration of 2 using one equivalent of 9-ethyl-9-borabicyclo[3.3.1]nonane, Et-9-BBN, proceeds similar to the E t3B-reaction, to give mainly the silole derivative 6, in which the bicyclic ring system is enlarged by two carbon atoms. This product is the result of a kinetically controlled reaction. The single crystal X-ray analysis of 1 has been carried out (space group Pnm a; a = 990.0(2), b = 1668.0(3), c = 1479.0(3) pm), and its crystal structure is com pared with that of the corre­ sponding tin compound 1 (Sn). 
  Reference    Z. Naturforsch. 51b, 1320—1324 (1996); received March 14 1996 
  Published    1996 
  Keywords    Tetra-l-alkynylsilanes, 1, 1-Organoboration, Siloles, X-Ray 
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 Identifier    ZNB-1996-51b-1320 
 Volume    51 
220Author    Z. NaturforschRequires cookie*
 Title    Thermolyse und Photolyse von cyclischen Diazoverbindungen [1]  
 Abstract    T h erm o ly sis a n d P hotolysis o f Cyclic D iazo C o m p o u n d s [1] H a n s-D ie tric h S tachel*, H e rm a n n P o sch e n rie d er, J u tta R e d lin The rhodium-catalyzed decomposition of the diazoketones 4 in teAY-butyl alcohol at 130 °C furnishes the m onoenolethers 5 and, after deprotection, the ac/-reductones 6. In absence of intercepting agents the intermediate carbenes preferentially undergo Wolff rearrangem ent with ring contraction. In this case the /J-thiolactone 10b or the /J-lactone 13 or the /M actam 14 are thermolysis products of the corresponding diazoketones. During photolysis of the diazoketones 4d/4g in presence of alcohols the 2-azetidinones lOc/d are formed. 
  Reference    Z. Naturforsch. 51b, 1325—1333 (1996); eingegangen am 9. Mai 1996 
  Published    1996 
  Keywords    Diazoketones, Reductones, 2-Oxetanones, 2-Thietanones, 2-Azetidinones 
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 Identifier    ZNB-1996-51b-1325 
 Volume    51 
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