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1994[X]
1Author    M. Arkus Brylak, Wolfgang JeitschkoRequires cookie*
 Title    U3TiSb5, U3VSb5, U3CrSb5, and U3MnSb5 with "Anti"-Hf5Sn3Cu Type Structure  
 Abstract    The title compounds have been prepared from the elem ental com ponents by arc-melting and subsequent annealing. Single crystals of U 3TiSb5 and U 3M nSb5 were obtained from a tin flux and their structures were determined from single-crystal X-ray data: P 63/mcm, Z = 2; a = 913.9(2), c = 611.2(1) pm, R = 0.011 (233 structure factors, 14 variables) for U 3TiSb5 and a = 916.8(2), c = 613.2(1) pm, R = 0.015 (427 structure factors, 14 variables) for U 3MnSb5. The lattice constants of the isotypic compounds are: a -908.2(2), c = 608.3(2) pm for U 3VSb5 and a -911.0(1), c = 611.5(1) pm for U^CrSb^. The structure of these antimonides may be regarded as an "anti"-type structure of Hf5Sn3Cu with the antimony atoms on the hafnium sites, while the positions of the uranium and transition metal atoms correspond to the posi­ tions of the tin and copper atoms. A comparison o f the interatomic distances of UVTiSbs with those of U 3Sb4, USb2, and a-antimony suggests oxidation numbers according to (U +III)3Ti+,v(S b l_III)3(S b 2_,I)2, where the Sb2 atoms form weakly bonded chains. 
  Reference    Z. Naturforsch. 49b, 747—752 (1994); received D ecem ber 16 1993 
  Published    1994 
  Keywords    Lattice Constants, Antimonides, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0747.pdf 
 Identifier    ZNB-1994-49b-0747 
 Volume    49 
2Author    W. Olfgang Eikens, P. Eter, G. Jones, Jü Rg, L. Au Tn Er, C. Arsten, ThöneRequires cookie*
 Title    Complexes of Copper, Silver, and Gold with Urea Homologues. Crystal Structures of I{/i2-SeC(NH2)2} Ag{SeC(NH2)2}2]22+2 Cl~ * 4 DMF and [Ph3PAu{SC(NHMe)2}]+Cl" * SC(NHMe)2  
 Abstract    The title compounds were prepared from chloro(organophosphine)metal(I) complexes and the urea homologues SeC(NH2)2 and SC(NHMe)2 in good yields. Recrystallization of [Ph,PAg{SeC(NH2)2}]+C r from D M F/C H 2C12 leads in low yield to the dinuclear complex [{/r-SeC(NH2)2}Ag{SeC(NH2)2}2]22+2 C r-4 D M F . The crystal structure reveals short A g-A g contacts and unexpectedly acute angles at the bridging selenium atom. The crystal structure of [Ph3PAu{SC(NHMe)2}]+Cl_ • SC(NHMe)2 shows short N --C1 and N -S con­ tacts that probably correspond to hydrogen bonding. 
  Reference    (Z. Naturforsch. 49b, 21—26 [1994]; received August 12 1993) 
  Published    1994 
  Keywords    Coinage Metal Complexes, X-Ray, Urea Homologues 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0021.pdf 
 Identifier    ZNB-1994-49b-0021 
 Volume    49 
3Author    Dieter Sellmann+, Helge Friedrich, Falk Knoch, Matthias MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, C*. Unerwartet einfache Bildung von Diazen-Komplexen und ein neuer Typ von Diastereomerie: [/#-N2H2{Fe(PPr3)('S4')}2] und analoge Komplexe mit [FeS]-Zentren. ( 'S /2-= l,2-Bis(2-mercaptophenylthio)ethan(2-)) Transition Metal Complexes with Sulfur Ligands, C*. Unexpectedly Facile Formation of Diazene Complexes and a New Type of Diastereomerism: [a-N2H2{Fe(PPr3)('S4')}2] and Analogous Complexes with [FeS]-Centers. ('S4'2~ = l,2-Bis(2-mercaptophenylthio)ethane(2-))  
 Abstract    Single pot reactions of FeCl2-4H20 with the tetradentate thioether-thiol 'S4-H 2' = 1,2-bis(2-mercaptophenylthio)ethane, phosphines such as PEt3, PPr3 or PBu3, and a ca. 40-fold excess of N2H4-H20 yield, in the presence of air, diazene complexes of the general formula [M-N2H2{Fe(PR3)('S4')}2]. In contrast to previous syntheses of diazene complexes, the yields can excel 80%, and the syntheses can be carried out on a 10 g scale. [M-N2H2{Fe(PPr3)('S4')}2], 1 and [M-N2H2{Fe(PEt3)('buS4')}2], 2 were characterized by X-ray structure analysis. 2 contains 'buS4'2-= l,2-bis(3,5-ditertiarybutyl-2-mercaptophenylthio)-ethane(2-), which is the tertiary-butyl derivative of 'S4'2-. 1 and 2 contain fram-HN=NH which bridges enantiomeric [Fe(PPr3)('S4')] or [Fe(PEt3)('buS4')] fragments. HN=NH is stabilized by 4c -6 e~-jr bonds, strong tricentric N -H — (S)2 bridges, and steric shielding. NMR studies show that centrosymmetric 1 isomerizes in solution at temperatures around 0 °C in order to give a diastereomerie diazene complex which is also centrosymmetric. The diastereomerism is traced back to bridging the chiral [Fe(PPr3)('S4')] fragments by frara-HN=NH in a differ­ ent way. The two different bridging modes are verified by X-ray structure analyses of analo­ gous ruthenium complexes. Because this new type of diastereomerism is basically caused by a different position only of the N -H — (S)2 bridges, it is termed hydrogen bridge diastereo­ merism. A mechanism for the isomerization is suggested. 1 exhibits three anodic waves in the cyclovoltammogram. The second wave indicates formation of the dication [1]2+, which is a redox isomer of the diprotonated (and as yet hypothetical) dinitrogen complex [a-N2{Fe(PPr3)('S4')}2]. The significance of [1]2+ and of its Lewis basic thiolate donors with respect to electrochemical reduction of molecular dinitrogen under mild conditions is dis­ cussed. 
  Reference    (Z. Naturforsch. 49b, 76—88 [1994]; eingegangen am 9. Juli 1993) 
  Published    1994 
  Keywords    Diazene, Iron Sulfur Complexes, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0076.pdf 
 Identifier    ZNB-1994-49b-0076 
 Volume    49 
4Author    Ulrich Behrens3, ReinhardH. Oppenheitb+, Wilhelm Isenbergb, Enno Lorka, Jan Petersen3, Rüdiger MewsRequires cookie*
 Title    Thiazyltrifluorid-Komplexe von Mg und Zn Thiazyltrifluoride Complexes of Mg and Zn  
 Abstract    The preparations of [Mg(NSF3)4](AsF6)2 (2a) and [Zn(NSF3)4](AsF6)2 (2b) are reported. The structure of 2 b was determined by X-ray diffraction. The ligand properties of NSF3 are discussed. 
  Reference    Z. Naturforsch. 49b, 238—242 (1994); eingegangen am 11. Oktober 1993 
  Published    1994 
  Keywords    Thiazyltrifluoride, X-Ray, Magnesium Complexes, Zinc Complexes 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0238.pdf 
 Identifier    ZNB-1994-49b-0238 
 Volume    49 
5Author    Dieter Sellm, Helge Friedrich, Falk KnochRequires cookie*
 Title    Synthese und Struktur von *1,33N2H4 Transition Metal Com plexes with Sulfur Ligands, Cl*. Synthesis and Structure of N 2H 5[Fe(N 2H4)(S2C6H4)2] * 1,33 N 2H 4  
 Abstract    A ttem pts to coordinate N2H4 to [Fe(S2C6H 4)2] fragments lead to N2H 5[Fe(N2H 4)(S2C6H4)2], which crystallizes from M eOH/N2H 4 solutions as the solvate [(N2H 5){Fe(N2H4)(S2C6H4)2} T.33 N2H 4], 1, and has been characterized by X-ray structure analysis. 1 contains three discrete N2H 5+ cations, four N2H4 solvate molecules and three independent [Fe(N2H4)(S2C6H4)2] anions which are connected via an extended network of N -H —N and N -H —S bridges. N2H 5[Fe(N2H 4)(S2C6H4)2] and 1 contain high-spin Fe(III) centers and labile N2H4 ligands. Ubergangsmetallkomplexe mit Schwefelliganden, CI*. 
  Reference    Z. Naturforsch. 49b, 660—664 (1994); eingegangen am 22. Dezember 1993 
  Published    1994 
  Keywords    Iron Sulfur Hydrazine Complexes, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0660.pdf 
 Identifier    ZNB-1994-49b-0660 
 Volume    49 
6Author    D. Ieter Sellmann, Thomas Hofmann, Falk KnochRequires cookie*
 Title    Ni(II)-und Ni(III)-Komplexe mit dem fünfzähnigen Thioether- Thiolat-Amin-Liganden 'NMeS4'2_ ('NMeS4'2_ = Dianion von 2,2'-Bis(2-mercaptophenylthio)diethylmethylamin) Transition Metal Complexes with Sulfur Ligands, CV* Ni(II) and Ni(III) Complexes with the Pentadentate Thioether- Thiolate-Amine-Ligand 'N MeS4'2_ ('N MeS4'2-= Dianion of 2.2'-Bis(2-m ercaptophenylthio)diethylmethylamine)  
 Abstract    Paramagnetic [N i('N MeS4')]2 1 ('N MeS4'2_ = 2.2'-Bis(2-m ercaptophenylthio)diethylm ethyl-a m in e(2 -)) was synthesized from N i(ac)2 and N a2-'N MeS4' and characterized by X-ray structure analysis. In solid state, 1 contains two pseudo-octahedral [N i('N MeS4')] fragments bridged via thiolate donors. In contrast to the parent com plex [N i('N HS4')]2, the thiolate and thioether donors coordinate cis to the Ni center forming m eso [N i('N MeS4')] fragments of Cs symmetry. 1 readily dissociates in solution to give mononuclear [N i('N MeS4')]. Reaction of [N i('N MeS4')]2 1 with PM e3 yielded [N i(PM e3)('N MeS4')] 2, oxidation by io­ dine gave the Ni(III) complex [N i(I)('N MeS4')] 3. Ubergangsmetallkomplexe mit Schwefel-Liganden, CY* 
  Reference    Z. Naturforsch. 49b, 821 (1994); eingegangen am 15. Februar 1994 
  Published    1994 
  Keywords    Nickel Complexes, Thioether-Thiolate-Amine-Ligands, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0821.pdf 
 Identifier    ZNB-1994-49b-0821 
 Volume    49 
7Author    E. Ndre Kövári, Roland KrämerRequires cookie*
 Title    Metallkomplexe 6,6'-Dialkinyl-substituierter 2,2'-Bipyridin  
 Abstract    Liganden: Synthese und Struktur von [{6,6'-(CH3CH2CH2C = C)2bpy}Cu(Cl)(^-Cl)]2 Metal Complexes of 6 ,6 '-Dialkynyl-Substituted 2,2'-Bipyridine Ligands: Synthesis and Structure of [{6 ,6 '-(C H 3 CH2CH2C = C)2bpy}Cu(Cl)(a-Cl)] 2 The bipyridyldiacetylene 6,6'-(C H 3CH2CH2C = C)2bpy (1) was prepared by palladium catalyzed C -C -cou p lin g reaction of 6,6'-dibromo-2,2'-bipyridine with pentyne. Reaction of 1 with anhydrous CuCl2 in acetonitrile gave the dimeric, chloro-bridged complex (1)C u(C1)(m-C1)2Cu(C1)(1) (2), which was characterized by X-ray crystallography. The copper atoms in 2 are square-pyramidally coordinated with normal in-plane C u -N and C u -C l bond distances and one longer, apical bond to the second bipyridyl nitrogen atom. The influence of steric hindrance o f the bipyridyl 6,6'-substituents on the structure o f the complex is discussed. 
  Reference    Z. Naturforsch. 49b, 1324—1328 (1994); eingegangen am 9. Mai 1994 
  Published    1994 
  Keywords    Copper Bipyridine Complexes, Bipyridylacetylenes, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1324.pdf 
 Identifier    ZNB-1994-49b-1324 
 Volume    49 
8Author    N. Orbert Kuhn3, Hans Bohnen3, GeraldH. EnkelbRequires cookie*
 Title    Zur Reaktion von Carben-Addukten des Kohlenstoffdisulfids mit Brom und Iod [1] On the Reaction of Carbene Adducts of Carbon Disulfide with Bromine and Iodine [1]  
 Abstract    The carbene adducts 3 are obtained as stable solids from the im idazol-2-ylidenes 1 and CS2. 3 c reacts with bromine to give the cationic bromosulfane 4, whereas iodine forms the charge-transfer adduct 5. Oxidative coupling to the dicationic disulfane 6 is observed with excess of iodine. The X-ray structure analyses of 3b, 4, 5 and 6 are reported. 
  Reference    Z. Naturforsch. 49b, 1473—1480 (1994); eingegangen am 7. Juli 1994 
  Published    1994 
  Keywords    Carbene Adducts, X-Ray, Iodine Reaction, Bromine Reaction 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1473.pdf 
 Identifier    ZNB-1994-49b-1473 
 Volume    49 
9Author    Oliver Seeger, Joachim SträhleRequires cookie*
 Title    BaCeN2, ein Bariumnitridocerat(IV) mit einer Struktur vom awf/-TiP-Typ BaCeN2, a Barium nitridocerate(IV ) with a Structure of the anti-TiP Type  
 Abstract    Reaction of Ba3N 2 with CeN in the stoichiometric ratio 1:3 at 850 °C under an atmosphere of N 2 followed by quenching yields air and moisture sensitive BaCeN 2. The product crystalli­ zes isotypically to /?-R bSc02 with the anti-TiP type structure in the hexagonal space group P 63/mmc with a = 365.06(2), c = 1266.03(3) pm, Z = 2. The structure was determined using X-ray and neutron powder diffraction data. In the structure the Ba2+ cations occupy trigonal prismatic holes with distances B a -N = 288(1) pm while the Ce atoms are in octahedral positions with distances C e -N = 242.4(8) pm. 
  Reference    Z. Naturforsch. 49b, 1169—1174 (1994); eingegangen am 27. April 1994 
  Published    1994 
  Keywords    Bariumnitridocerate(IV), Synthesis, Structure, X-Ray, Neutron Powder Diffraction 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1169.pdf 
 Identifier    ZNB-1994-49b-1169 
 Volume    49 
10Author    Z. NaturforschRequires cookie*
 Title    Structure and Magnetic Properties of a Dinuclear Complex with Iron(III) in Octahedral and Pyramidal Coordination  
 Abstract    [FeL(M eO H)C l]2 (L = N-(2-hydroxyphenyl)salicylaldimine) was synthesized and its crystal structure determ ined, [C27H 20N 2O5Cl2Fe2], monoclinic, space group P 2 a/c, a = 9.528(1), b = 7.684(1), c = 18.365(2) Ä , ß = 109.83(1)°, V = 1264.8 Ä 3, Z = 2. Two identical [FeL(M eOH)Cl] fragments, related by an inversion centre, are combined by the two bridging O atoms, to form a binuclear unit. The iron(III) centers are separated by 3.163(2) A and weakly antiferro-magnetically coupled (J = -8 .0 (1) cm -1), which follows from temperature -dependent mag­ netic susceptibility m easurements in the range 4.2 to 288 K. The effective magnetic moment per iron(III) is /ueff = 7.4 /uB at 288 K. 
  Reference    Z. Naturforsch. 49b, 1239—1242 (1994); received March 28 1994 
  Published    1994 
  Keywords    Dinuclear Iron(III) Complex, X-Ray, Structure, Magnetic Properties, Antiferromagnetic Coupling 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1239.pdf 
 Identifier    ZNB-1994-49b-1239 
 Volume    49 
11Author    RolfW. Saalfrank3, Oliver Struck3, Karl Petersb, HansG. Eorg, Von SchneringbRequires cookie*
 Title    Synthese und Struktur diastereomerer, zweikerniger Kupferkomplexe [1] Synthesis and Structure of Diastereomerie Dinuelear C opper Complexes [1]  
 Abstract    Depolym erisation of a copper(II)/pyrrolidine-based 2D -polym er 2 by 4.4'-bipyridyl [molar ratio: 2 (C u L 2) : l (Bipy)] and recrystallisation o f the reaction product leads to two visually distinguishable crystal charges, composed of dark green octahedra m eso-4 and light green rod-shaped crystals racem-5. Separation of the conglom erate of the morphologically different crystals is accomplished by pick out. The structure of the dinuelear complex racem-5 has been established unambigously by X-ray structure analysis. EPR and susceptibility measure­ ments of mixtures of complex meso-4 and racem-S indicate that there is no interaction be­ tween the two copper(II) centres. 
  Reference    Z. Naturforsch. 49b, 1410—1414 (1994); eingegangen am 17. März 1994 
  Published    1994 
  Keywords    Coordination Polymers, Depolymerisation, Dinuelear Copper Complexes, Diastereomers, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1410.pdf 
 Identifier    ZNB-1994-49b-1410 
 Volume    49 
12Author    Z. NaturforschRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 114 [1]  
 Abstract    Synthese und Struktur eines ionischen und nichtionischen, cyclischen Carbaphosphazens und eines Cobalt(III)phosphazen-Komplexes C hem istry of Polyfunctional M olecules, 114 [1] Synthesis and Structure of an Ionic and N on Ionic Cyclic C arbaphosphazene and of a C o b alt(III)phosphazene Com plex Jochen E llerm ann3 *, Jörg S u tter3, Falk A. K noch3, M atthias M oll3, W alter B au e rb Reaction of Ph2 P -N -P (P h 2) -N -(Ph2)PCoP(Ph2) -N -P (P h 2) -N -PPh2 (1) in CH2 C12 with benzimidazole yields (CH2 -PPh2 = N -PPh2 = N -PPh2)+C l" ([4]+C L). The salt [4]+BPh4" has been prepared in THF by metathesis of [4]+C l_ with N aBPh4. D eprotonation of the cationic ring in [4]+BPh4_ was accomplished using l,8-diazabicyclo[5.4.01 7 ]undec-7-ene and resulted in the six-membered carbacyclophosphazene CH=PPh2 -N = P P h 2 -N = P P h 2 (6). Treating 1 with 8 -hydroxyquinoline in CH2 C12 yields the octahedral c/s-complex (N 0) 2 CoP(Ph2) -N -P (P h 2) -N -P P h 2 (7) (N O = 8 -oxyquinolinate group). The com ­ pounds [4]+BPh4~, 6 and 7 are characterized by their IR, Raman, 3 1 P{1H) NM R, 1 3 C{1 H} N M R , !H NMR and mass spectra. Crystals suitable for X-ray structure analyses have been obtained for [4]+BPh4_ and_7x0.5 CH2 C12. The colourless plates of [4]+BPh4_ crystallize in the triclinic space group P I, with the lattice constants a = 1172.7(3), b = 1326.2(3), c = 1806.1(6) pm; a = 100.79(2), ß = 103.71(3), y = 108.18(2)°. The black blocks o f 7 x 0 .5 C H 2 C12 crystallize in the monoclinic space group P 2 x!c with the lattice constants a = 1159.0(10), b = 2008.9(10), c = 2034.6(12) pm; ß = 105.86(5)°. 
  Reference    Z. Naturforsch. 49b, 1763—1773 (1994); eingegangen am 25. April 1994 
  Published    1994 
  Keywords    Cyclic Carbaphosphazene Systems, Cobalt Complexes, Syntheses, NM R Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1763.pdf 
 Identifier    ZNB-1994-49b-1763 
 Volume    49 
13Author    Z. NaturforschRequires cookie*
 Title      
 Abstract    C om plexes of the types R3 P b -F e (C O)2Cp [R = Me (la), Et (lb), 'Pr (lc), 'Bu (Id)]. R2 Pb[Fe(CO)2 Cp] 2 [R = Me (2a), Et (2b)], 'Pr2 (B r)P b -F e(C O)2Cp (3c) and [R2 PbFe(CO) 4 ] 2 [R = Me (4a), Et (4b), 'Pr (4c)], as well as the spiro-complexes Pb[Fe(C O)4 PbR2 ] 2 [R = Me (5a), Et (5b), 'Pr (5c)] and Pb[Fe(CO) 4 ] 4 (6) were studied by multinuclear magnetic reso­ 
  Reference    Z. Naturforsch. 49b, 1781—1788 (1994); received July 28 1994 
  Published    1994 
  Keywords    Carbonyliron-Lead Complexes, NM R Spectra, Coupling Sign Determination, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1781.pdf 
 Identifier    ZNB-1994-49b-1781 
 Volume    49 
14Author    Matthias Westerhausen, Bernd Radem, Wolfgang Schwarz, Sonja HenkelRequires cookie*
 Title    Lithium-zinkate mit heteroleptischem Triorganylzinkat-Anion Lithium Zincates with Heteroleptic Triorganylzincate Anion  
 Abstract    -, bis[bis(trimethylsilyl)methyl]-as well as bis(2,2,4,4,6,6-hexa-methyl-2,4,6-trisila-cyc/o-hexyl)zinc react with methyl lithium or phenyl lithium in the pres­ ence of the tridentate l,3,5-trimethyl-l,3,5-triazinane (TMTA) to yield zincates of the type LiZnR2R'-2TMTA. The compounds are colorless and insoluble in aliphatic or aromatic hydrocarbons. These zincates exist in solution as well as in the crystalline state as separated ions, as confirmed for lithium-methyl-bis(2,2,4,4,6,6-hexamethyl-2,4,6-trisila-cyc/o-hexyl)-zincate • 2TMTA by X-ray diffraction (PI; a -1139,5(3); b = 1482,4(4); c = 1528,6(5) pm; a = 95,33(2); ß = 100,13(2); y = 106,91(2)°; Z = 2). The lithium cation is six-coordinated by two TMTA ligands in a distorted anti-prismatic complex. The zinc atom displays a trigonal planar coordination with Z n -C bond lengths of 207 pm to the 2,2,4,4,6,6-hexamethyl-2,4,6-trisila-cyc/o-hexyl ligands and of 202 pm to the methyl group. One trisila-cyc/o-hexyl substi­ tuent exists in the chair, the other one in the twist conformation. The reaction of lithium bis(trimethylsilyl)amide with bis(trimethylsilylmethyl)zinc yields the benzene soluble lithium-bis(trimethylsilyl)amino-bis(trimethylsilylmethyl)zincate TMTA. The molecular structure was confirmed by X-ray diffraction a -1024,8(3); b = 1775,4(7), c = 1918,2(8) pm; Z = 4). The bridging bis(trimethylsilyl)amino ligand displays long Z n -N and L i-N distances of 213 and 208 pm, respectively, due to the steric inter-ligand repulsion. During the reaction of lithium bis(trimethylsilyl)amide with bis[bis(trimethylsilyl)methyl]-zinc no zincate formations observed. The decomposition products lithium bis(trimethylsilyl)-methanide and the heteroleptic bis(trimethylsilyl)amino-bis(trimethylsilyl)methylzinc were detected. 
  Reference    Z. Naturforsch. 49b, 199—210 (1994); eingegangen am 9. Juli 1993 
  Published    1994 
  Keywords    Lithium Zincate, Heteroleptic Triorganylzincate, Zincate, X-Ray, NMR Spectra Bis(trimethylsilylmethyl) 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0199.pdf 
 Identifier    ZNB-1994-49b-0199 
 Volume    49 
15Author    WolfPeter Fehlhammer, Thomas Bliß, Wilfried Sperber, Joachim FuchsRequires cookie*
 Title    Homoleptische Carbenkomplexe, V [1] Chelatartige Percarbenkomplexe des Palladiums und Platins Homoleptic Carbene Complexes, V [1] Chelating Percarbene Complexes of Palladium and Platinum  
 Abstract    Ten palladium and platinum complexes each containing two chelating bis(diaminocarbe-ne) ligands have been synthesized in a one pot-reaction from P dl2, P tl2 or K2PtCl4, a tenfold excess (forty equivalents) of isocyanide and 1,2-or 1,3-diamines. A n X-ray investigation of 
  Reference    Z. Naturforsch. 49b, 494—500 (1994); eingegangen am 10. N ovem ber 1993 
  Published    1994 
  Keywords    Isocyanide Complexes, Reactions at Coordinated Ligands, Chelating Bis(diam inocarbene) Ligands, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0494.pdf 
 Identifier    ZNB-1994-49b-0494 
 Volume    49 
16Author    JensR. Goerlich, Axel Fischer, PeterG. Jones, Reinhard Schmutzler+Requires cookie*
 Title    Organophosphorverbindungen mit tertiären Alkylsubstituenten. III*: Synthese und Reaktionen Di-l-adamantylsubstituierter Phosphorverbindungen; Kristallstruktur von Di-l-Adamantylphosphinsäurechlorid Organophosphorus Compounds with Tertiary Alkyl Substituents. Ill: Synthesis and Reactions of D i-l-adam antyl-Substituted Phosphorus Compounds; Crystal Structure of Di-l-adam antylphosphinic Chloride  
 Abstract    The reaction of adamantane with PC13/A1C13, followed by hydrolysis, gave (l-Ad)2P(: 0)C1 1, which was converted to (l-Ad)2P(:Ö)F 2 and (l-Ad)2P(:S)Cl 3 by standard procedures. The structure of 1 was confirmed by a single crystal X-ray structure determination; despite the bulky substituents the P-C bond lengths are normal (184.0(3), 185.0(3) pm). Whereas chlorine-fluorine exchange in 3 with AsF3 furnished (l-Ad)2P(: S)F 4, desulfuration of 3 with Ph3P to give (l-Ad)2PCl 5 failed. The secondary phosphine oxides R 'R 2P(:0)H (R1, R2 = 1-Ad: 6; R1 = 1-Ad, R2 = 'Bu: 7; R1, R2 = 'Bu: 8) were synthesized by reaction of 1, l-AdP(:0)Cl2 and 'BuP(:0)Cl2 with 'BuLi. 6 and 8 reacted readily with chloral to give the adducts R2P(:0)CH(0H)CC13 (R = 1-Ad: 9; R = 'Bu: 10). Silylation of 6 with Me2NSiMe3 in the presence of dry air led to (l-Ad)2P(:0)0SiM e3 11, which was hydrolyzed to give (l-Ad)2P (:0)0H 12. (l-Ad)2POSiMe3 13 was obtained by the reaction of 6 with /z-BuLi, followed by Me3SiCl. No reaction took place upon heating 6 with Mo(CO)6. (l-Ad)2PCl 5 was synthesized in low yield by the reaction of 6 with PC13. The action of tetrachloro-o-benzoquinone (TOB) upon 6 furnished (l-Ad)2P(: 0)(o-OH)C6Cl4 15, whereas the 'butyl analogue of 15, 16, was synthesized by hydrolysis of the TOB-adduct of di-'butylfluorophos-phine. Analogous 1-adamantyl-and 'butyl-phosphorus compounds are compared with regard to their 31P NMR data. 
  Reference    Z. Naturforsch. 49b, 801—811 (1994); eingegangen am 17. Dezember 1993 
  Published    1994 
  Keywords    Di-l-adamantyl Phosphorus Compounds, Secondary Phosphine Oxides, Di-l-adamantyl Phosphinic Acid, NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0801.pdf 
 Identifier    ZNB-1994-49b-0801 
 Volume    49 
17Author    Axel Fischer, Ion Neda, Thomas Kaukorat, Ralf Sonnenburg, PeterG. Jones, R.Einhard SchmutzlerRequires cookie*
 Title    Chemistry of the 4,5-Benzo-3-methyl-l,3,2-oxazaphosphorinan-6-one Ring System: X-Ray Crystal Structure Analysis of a Bis(2-chloroethyl)amino-and of an Acetam ido-Substituted Derivative  
  Reference    Z. Naturforsch. 49b, 939—949 (1994); eingegangen am 14. Februar 1994 
  Published    1994 
  Keywords    4, 5-Benzo-3-m ethyl-l, 3, 2-oxazaphosphorinan-6-one Derivatives, H alogen Substitution, Oxidation, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0939.pdf 
 Identifier    ZNB-1994-49b-0939 
 Volume    49