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1996[X]
1Author    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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1267.pdf 
 Identifier    ZNB-1996-51b-1267 
 Volume    51 
2Author    Frank Borkenhagen, Ion Neda, H. Olger Thönnessen, PeterG. Jones, R. Einhard, Schm UtzlerRequires cookie*
 Title    Synthesis and Characterization o f 2-Substituted 5 Darstellung und Charakterisierung von 2-substituierten 5,6-Benzo-l-methyl  
 Abstract    ,6 -B en zo -l-m eth y l-3 -R -l,3 ,2 -diazaphosphorin-4-ones (R = 2-M orpholinoethyl, 1-Adam antyl) C ontaining Phosphorus w ith Coordination N um bers T hree, Four and Five The reaction of N-methylisatoic anhydride with 2-morpholinoethylamine or 1-amino-adamantane furnished N-methyl-N'-(2-morpholinoethyl)anthranilamide 1 and N-methyl-N'-(l-adamantyl)anthranilamide 2, respectively. 1 and 2 are intermediates in the synthesis of the 2-chloro-3-methyl-1,3,2 A'-diazaphosphorinones 3 and 4 by reaction of 1 and 2 with PCI,. The reaction of 3 with bis(2-chloroethyl)amine hydrochloride/triethylamine or (2-chloroethyl)amine hydrochloride/triethylamine formed the 2-substituted diazaphosphorinones 5 and 6. Hydrolysis of 3 led to the 2-oxo-A4P-compound 7. The reaction of 6 with hexafluoroacetone furnished the (A5) phosphorane 8. 5 reacted with C7H8Cr(CO)4 to form complex 9 whereas oxidation of 5 with the H20 2: urea 1:1 adduct yielded the phosphoryl compound 10. The crystal structure of 1 displays two independent molecules that show different chain conformations. Both molecules form chains parallel to the y-axis by intermolecular N (am ide)-H -0(am ide) bonds. The crystal structure of 6 shows a half-boat conformation for the phosphorinone ring; the P atom lies out of the plane. Again the molecules are linked by H-bonds into chains parallel to the y-axis. 
  Reference    Z. Naturforsch. 51b, 1627—1638 (1996); eingegangen am 14. März 1996 
  Published    1996 
  Keywords    Diazaphosphorinones, Oxidative Addition, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1627.pdf 
 Identifier    ZNB-1996-51b-1627 
 Volume    51 
3Author    Jochen Ellermann, Peter Gabold, FalkA. Knoch, MatthiasM. Oll, Astrid Schmidt, Martin SchützRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 120 [1] Synthesen und Kristallstrukturanalysen von Tris(imido-tetraphenyl- diphosphinato-0,0')eisen(III) und des PP-verknüpften Phosphazens Ph2P-N=PPh2-PPh2=N-PPh2 Chemistry o f Polyfunctional M olecules, 120 [11 Syntheses and Crystal Structures o f Tris(imido-tetraphenyl-diphosphinato-0,0')iron(III) and o f the PP-Connected Phosphazene Ph2P-N=PPh2-PPh2=N-PPh2  
 Abstract    While the reaction of anhydrous iron(III) chloride with the chelate ligand [(C6H5)2P(0)]2NH (6) is an efficient way to synthesize the new tricyclic compound imido-tetraphenyl-diphosphinato-0,0'iron(III), [Fe{0-P(Ph2)=N-P(Ph2)= 0 }3] (4), treatment of [(C6H5)2P]2NLi (1) with anhydrous iron(III) fluoride in THF represents a simple route to obtain the phosphorus-phosphorus connected species Ph2P-N=PPh2-PPh2=N-PPh2(7). Both compounds were charac­ terized by X-ray crystallography, 'H ,31 P {1H}, 13C {1H} NMR, IR, Raman and mass spectra. 
  Reference    Z. Naturforsch. 51b, 201—208 (1996); eingegangen am 24. Juli 1995 
  Published    1996 
  Keywords    Phosphazene, Iron Complexes, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0201.pdf 
 Identifier    ZNB-1996-51b-0201 
 Volume    51 
4Author    Kuhn3, Thomas Kratz3, G. Erald, H. EnkelbRequires cookie*
 Title    N orbert  
 Abstract    The carbene adduct 5 is formed from the 2-tel-luroimidazoline 4 and iodine. The X-ray structure analysis reveals a dimeric structure in the solid state. 
  Reference    Z. Naturforsch. 51b, 295 (1996); eingegangen am 21. Juli 1995 
  Published    1996 
  Keywords    Tellurium, Carbene, Iodine Reaction, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0295_n.pdf 
 Identifier    ZNB-1996-51b-0295_n 
 Volume    51 
5Author    Yoshimitsu Yamazaki, MidoriG. Oto1, ^. Yu-Ichi, Takenori Kageyama, Hiroaki Tomohiro, OkunoRequires cookie*
 Title    Structure of Chloro(cyclopentadienone)- (cyclopentadienyl)ruthenium and its Cytotoxic Activity  
 Abstract    The structure of R u(cpO)(cp)C l com plex (3), which was precipitated from aqueous solutions of R u(cp)2Cl+PF6' (1), was determined by X-ray crystallographic analysis. The Ru-halogen bond distance was shorter and the dihedral angle be­ tween the rings was larger than the values re­ ported for the corresponding Br analogue, R u(cpO)(cp)Br (4). The com plex 3 (IC50 1 09 /iM) was more cytotoxic than 1 (IC50 163 //M) against mouse sarcoma S I80 cells, but less toxic than 4 (IC50 72 ,/M). 
  Reference    Z. Naturforsch. 51b, 301 (1996); received September 21 1995 
  Published    1996 
  Keywords    Ruthenium Complex, Cytotoxicity, X-Ray, Cyclic Voltammetry 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0301_n.pdf 
 Identifier    ZNB-1996-51b-0301_n 
 Volume    51 
6Author    Max Herberhold, Guo-Xin Jina, ArnoldL. RheingoldbRequires cookie*
 Title    Sulfur and Selenium Complexes of the Hydrido-tri(3,5-dimethyl-l- pyrazolyl)borate Nitrosylmolybdenum Fragment, [Tp*Mo(NO)]. An X-Ray Crystal Structure Determination of Tp*Mo(NO)(Se5)  
 Abstract    The reactions of hydrido-tri(3,5-dimethyl-l-pyrazolyl)borate nitrosylmolybdenum diiodide, Tp*Mo(NO)L (2), with the oligochalcogenides (N H ^Sio and (NEuteSeö in THF solution lead to mononuclear cvc/o-pentachalcogenido complexes, Tp*Mo(NO)(E5) (E = S (3a), Se (3b)). In the presence of either H2S or H^Se (generated by slow "in situ" hydrolysis of AI2E3 in moist THF solution) 2 is converted into binuclear chalcogenido-bridged products, Tp2Mo2(NO)2(//-E)2 (E = S (4a), Se (4b)) which are more conveniently obtained from 3a,b by dechalcogenation with tri(''butyl)phosphane (1:4,5). The new chalcogen complexes 3a,b and 4a,b were characterized by IR, NMR and mass spectroscopy and compared with the related chalcogen compounds derived from pentamethylcyclopentadienyl nitrosylmolybdenum diiodide, Cp*Mo(NO)l2. The molecular structure of Tp*Mo(NO)(Ses) (3b) has been determined; the complex contains a six-membered MoSe«; metallacycle in the chair conformation and a linearly coordinated nitrosyl ligand (angle M o -N -0 178.9(17)°). 
  Reference    Z. Naturforsch. 51b, 681—685 (1996); received August 28 1995 
  Published    1996 
  Keywords    Molybdenum-chalcogenido Complexes, Nitrosyl Compounds, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0681.pdf 
 Identifier    ZNB-1996-51b-0681 
 Volume    51 
7Author    Utzolino, Karsten BluhmRequires cookie*
 Title    A nne  
 Abstract    The compounds M nCo(B20 ?) (I) and M nM g(B20 5) (II) were prepared by using B20 3 flux techniques in an argon atmosphere. X-ray investigations on single crystals showed triclinic symmetry, space group C' -P i, I: a = 320.94(10), b = 619.20(11), c = 939.0(2) pm, a = 104.38(2)°, ß = 90.76(2)°, 7 = 92.046(14)° and II: a = 318.97(7), b = 619.8(2), c = 936.7(2) pm, q = 104.47(2)°, ß = 90.60(2)°, 7 = 91.98(2)° Z = 2. Their structures are isotypic with C o2(B20 5). All metal ions are octahedrally coordinated by six oxygen atoms. The structures contain diborate anions B ^ 4 -. Each boron atom is threefold coordinated by oxygen. Synthese und Kristallstruktur von manganhaltigen Pyroboraten: MnCo(B20 5) und MnMg(B20 5) 
  Reference    Z. Naturforsch. 51b, 912—916 (1996); eingegangen am 25. Januar 1996 
  Published    1996 
  Keywords    Manganese, Cobalt Magnesium, Pyroborate Crystal Structure, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0912.pdf 
 Identifier    ZNB-1996-51b-0912 
 Volume    51 
8Author    Stephan Von, B. Eckeratha, Ingo-Peter Lorenz, Riad Fawzib, M. Anfred, Steim AnnbRequires cookie*
 Title     
 Abstract    p(C O)2M nN (Bz)C H 2CH2 , der erste einzähnig koordinierte A ziridin-K om plex C p(C O)2M nN (B z)C H 2C H 2, the First M ono-C oordinate A ziridine Com plex The photolytically induced CO-substitution reaction of CpM n(CO b with N-benzyl-aziridine leads to the first mono coordinate aziridine complex, Cp(CO)2MnN(Bz)CH2CH2. It is stable against thermal C2H4 elimination up to 135°C. No nitrene complexes {Cp(CO)2Mn}"NBz (/? = 1, 2) were detected. The X-ray structure analysis of Cp(CO)2MnN(Bz)CH2CH2 shows the intact three-membered ring ligand and the pyramidal configuration of the nitrogen atom. 
  Reference    Z. Naturforsch. 51b, 959—962 (1996); eingegangen am 12. Januar 1996 
  Published    1996 
  Keywords    N-Benzyl-aziridine, Substitution, Cymantrene, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0959.pdf 
 Identifier    ZNB-1996-51b-0959 
 Volume    51 
9Author    Eva-M Struckb, Karl Aria Peters0, H. Petersc, Georg Ans, Von SchneringcRequires cookie*
 Title    Verknüpfung koordinativ ungesättigter Kupfer(II)-Monomere via Cyano-versus Tetrazolyl-Donor [1]  
 Abstract    Reaction of a methanolic copper(II) acetate solution with tetrazolyl enol derivatives 2a (HL2) or 2b (HL3) leads to the formation of the corresponding 2D-coordination polymers 4 (^ [CuL^]) and 5 (^ [CuL2]), respectively. Single-crystal X-ray diffraction of the supramolecular species 4 and 5 established unequivocally the structures of the regioisomeric coordination polymers. On the contrary, reactions of 2c (HL4) with methanolic copper(II) acetate solution and 2b (HL3) with methanolic zinc(II) acetate solution yield mononuclear chelate complexes 11 ([CuL2]) and 12 ([ZnL2(MeOH)2]). The structures of 11 and 12 have been established by X-ray structure analysis. 
  Reference    Z. Naturforsch. 51b, 399—408 (1996); eingegangen am 14. August 1995 
  Published    1996 
  Keywords    Tetrazolyl Enols, Coordination Polymers 2D Copper Complexes, Spontaneous Self-Assembly, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0399.pdf 
 Identifier    ZNB-1996-51b-0399 
 Volume    51 
10Author    Ayhan Elmalia, Yalcin Elerman3, Ingrid Svoboda, Hartmut Fuessb, Klaus Griesar0, Wolfgang HaasecRequires cookie*
 Title    Structure and Spin-Spin Interactions in a Linear Trinuclear Ni(II) Complex  
 Abstract    [Ni3(C2H302)2(C3H8N0)2L2] 1(L=N,N'-1,3-propyl-disalicylaldimine), (C2H30 2)=acetate, (C3H><NO)=hydroxymethyl-dimethylamine] has been synthesized and its crystal structure de­ termined, [C44H54N6OioNi3], triclinic, space group Pi, a = 9.560(1), b = 10.681(1), c = 12.200(1) A ,a = 112.17(1), ß = 101.25(1), 7 = 90.32(1)°, V = 1127.3 A \ Z = l.The molecule is linearly trinuclear with octahedral coordination of each nickel ion. The Ni-Ni distance is 3.048(1) A. Each nickel(II) atom is in an octahedral coordination. Magnetic susceptibility mea­ surements in the range 4.2 < T < 280 K have revealed antiferromagnetic coupling between adjacent Ni atoms (J\ = -2.2 cm-1) and between the terminal Ni atoms (/2 = -1 .7 cm-1). 
  Reference    Z. Naturforsch. 51b, 665—670 (1996); received October 20 1994 
  Published    1996 
  Keywords    X-Ray, Linear Trinuclear Nickel Complex, Magnetic Properties, Antiferromagnetic Coupling 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0665.pdf 
 Identifier    ZNB-1996-51b-0665 
 Volume    51 
11Author    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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1255.pdf 
 Identifier    ZNB-1996-51b-1255 
 Volume    51 
12Author    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 
13Author    B. Ernd, W. Rackm Eyer, D. Örfler, W. Olfgang Milius, M. Ax, H. ErberholdRequires cookie*
 Title    ,1-Organoboration of Trimethyl-l-propynyltin Using Diorganoboryl-Substituted Ferrocenes  
 Abstract    The reactions of various diorganoborylferrocenes, F c -B R 2 [1, R = Me (a), Et (b), 'Pr (c), 'Bu (d), Ph (f), R2B = 9-borabicyclo[3.3.1]nonyl (e)] and 1,1 '-bis(9-borabicyclo[3.3.1]nonyl)-ferrocene (2) with trimethyl-l-propynyltin (3) were studied, and the products of the 1,1-organoboration were characterized as the alkenyltin compounds 4 -6 by 'H, UB, 13C and 119Sn NMR. In the cases of l a -I d and If, there is competition between the transfer of a ferrocenyl group and the other organyl groups R from boron to carbon, whereas in the case of the 9-borabicyclo[3.3.1]nonane derivatives le and 2, the enlargement of the bicyclic system takes place selectively (compounds 4e and 6). The molecular structure of the product 6, obtained from the reaction between the l,l'-diborylated ferrocene 2 and two equivalents of 3, was determined by single crystal X-ray analysis (space group P2x!c\ monoclinic; Z = 4, a = 958.3(2), b = 1610.4(3), c = 2405.3(5) pm and ß = 90.33(3)°). 
  Reference    Z. Naturforsch. 51b, 851 (1996); received October 26. 1995 
  Published    1996 
  Keywords    Ferrocenes, Trimethyl-l-propynyltin, 1, 1-Organoboration, Alkenyltin Compounds, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0851.pdf 
 Identifier    ZNB-1996-51b-0851 
 Volume    51 
14Author    RolfW. Saalfrank3 ', BerndH. Örner1, Stephan Recka, Jochen Nachtraba, Eva-Maria Petersb, Karl Petersb, Hans Georg Von SchneringbRequires cookie*
 Title    Synthese und Umsetzungen von 4-Acyl/Carbamoyl-N-aryl-3-chloro- pyrrol-2,5-dionen: Kristallstruktur eines auf Wasserstoffbrückenbindungen basierenden supramolekularen Bandes [1] Synthesis and Reactions of 4-Acyl/Carbamoyl-N-aryl-3-chloro-pyrrol-2,5-diones: Crystal Structure of a Supramolecular Ribbon Based on Hydrogen Bonds [ 1]  
  Reference    Z. Naturforsch. 51b, 1084—1098 (1996); eingegangen am 14. August 1995 
  Published    1996 
  Keywords    2, 3-Dioxo-2, 3-dihydrofurans, Pyrrol-2, 5-diones, Intermolecular H-Bridges, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1084.pdf 
 Identifier    ZNB-1996-51b-1084 
 Volume    51 
15Author    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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1229.pdf 
 Identifier    ZNB-1996-51b-1229 
 Volume    51 
16Author    FredR. Oschea, G. Ernot, H. Eckm, Anna, FrankW. Ellerb, Ekkehard Fluck0Requires cookie*
 Title    Ein neuer Heterocyclus  
 Abstract    , 2A3,4A5-[l,2,4]-O xadiphosphinin (2), als Ligand eines zw eikernigen Eisenkom plexes A New H eterocycle, 2A3,4A5-[l,2,4]-O xadiphosphinine (2), as L igand o f a Binuclear Iron C om plex Preparation and properties of a coordination compound are described, in which a carbonyl group in bis[(dicarbonyl)(/;;i-cyclopentadienyl)iron] is substituted by hitherto unknown octa-Af-methyl-2A',4A:i-[l,2,4]-oxadiphosphinine-2,4,4,6-tetramine (2). The 'H , '1P, and l3C NMR spectra are recorded and discussed in detail. The molecular structure of the iron complex 4 is described and interpreted. 
  Reference    Z. Naturforsch. 51b, 1725—1731 (1996); eingegangen am 27. Juni 1996 
  Published    1996 
  Keywords    [l, 2, 4]-Oxadiphosphinine, Binuclear Iron Complex, NMR Spectra, X-Ray 
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 Identifier    ZNB-1996-51b-1725 
 Volume    51 
17Author    VasilyRequires cookie*
 Title    Chemistry of the l,3>5-Triaza-2-phosphorin-4,6-diones, Part XII*. Synthesis and Characterization of 2-PhenyI-2-(/?-tolylthio)-l,3?5- trimethyI-l,3,5-triaza-4,6-dione-2-phosphorinonium Salts  
 Abstract    A . P in ch u k , Io n N e d a , C h ristian M üller, H o lg e r T h ö n n e ss e n , P e te r G. Jones, R e in h a rd S chm utzler The reaction of l,5-bis(trimethylsilyl)-l,3.5-trimethylbiuret (1) with/M olylsulfenyl chloride (2) furnished l-(/?-tolylthio)-5-trimethylsilyl-l,3,5-trimethylbiuret (3). In the reaction of 3 with phenyldichlorophosphine, 2-phenyl-2-(/?-tolylthio)-l,3,5-trimethyl-l,3,5-triaza-4,6-dione-2-phosphorinonium chloride (4) was formed. The same product was obtained from the reac­ tion of 2-phenyl-l,3,5-trimethyl-l,3,5-triaza-2/.3-phosphorin-4,6-dione (6) with p-tolylsulfenyl chloride (2). Compound 4 was isolated and characterized in the form of the hexachloroanti-m onate (4a). The spirophosphorane 2-phenyl-l,3,5-trimethyl-l,3,5-triaza-7,10-dioxa-8,9-perchlorobenzo-2As-phosphaspiro-[4.5]decan-4,6-dione (7) was prepared by the reaction of 4 with tetrachloroorthobenzoquinone. The new products were characterized by 'H -and 13C NMR spectroscopy, elemental analysis, 31P NMR spectroscopy in the case of 4a. 6 and 7, and mass spectrometry (4a). Single-crystal X-ray structural analyses of compounds 4a and 7 were conducted. The phosphorus atom of 4a has the expected tetrahedral geometry, with a rather short P-S bond of 204.9(2) pm. In 7 the geometry at phosphorus is almost ideal trigonal bipyramidal. Weak hydrogen bonds are formed from a C (:0) group to deuterochloroform of solvation. 
  Reference    Z. Naturforsch. 51b, 1494—1500 (1996); received February 13 1996 
  Published    1996 
  Keywords    1, 3, 5-Trimethyl-Substituted 1, 3, 5-Triaza-4, 6-dione-2-phosphorinonium Derivatives, Intram olecular Rearrangem ent, NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1494.pdf 
 Identifier    ZNB-1996-51b-1494 
 Volume    51