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1	Author	M. Arkus Brylak, Wolfgang Jeitschko	Requires 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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	Identifier	ZNB-1994-49b-0747
	Volume	49

2	Author	E. Ndre Kövári, Roland Krämer	Requires 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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	Identifier	ZNB-1994-49b-1324
	Volume	49

3	Author	N. Orbert Kuhn3, Hans Bohnen3, GeraldH. Enkelb	Requires 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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	Identifier	ZNB-1994-49b-1473
	Volume	49

4	Author	W. Olfgang Eikens, P. Eter, G. Jones, Jü Rg, L. Au Tn Er, C. Arsten, Thöne	Requires 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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	Identifier	ZNB-1994-49b-0021
	Volume	49

5	Author	Dieter Sellmann+, Helge Friedrich, Falk Knoch, Matthias Moll	Requires 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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	Identifier	ZNB-1994-49b-0076
	Volume	49

6	Author	Ulrich Behrens3, ReinhardH. Oppenheitb+, Wilhelm Isenbergb, Enno Lorka, Jan Petersen3, Rüdiger Mews	Requires 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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	Identifier	ZNB-1994-49b-0238
	Volume	49

7	Author	Dieter Sellm, Helge Friedrich, Falk Knoch	Requires 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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	Identifier	ZNB-1994-49b-0660
	Volume	49

8	Author	D. Ieter Sellmann, Thomas Hofmann, Falk Knoch	Requires 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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	Identifier	ZNB-1994-49b-0821
	Volume	49

9	Author	Oliver Seeger, Joachim Strähle	Requires 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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	Identifier	ZNB-1994-49b-1169
	Volume	49

10	Author	Z. Naturforsch	Requires 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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	Identifier	ZNB-1994-49b-1239
	Volume	49

11	Author	RolfW. Saalfrank3, Oliver Struck3, Karl Petersb, HansG. Eorg, Von Schneringb	Requires 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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	Identifier	ZNB-1994-49b-1410
	Volume	49

12	Author	Z. Naturforsch	Requires 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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	Identifier	ZNB-1994-49b-1763
	Volume	49

13	Author	Z. Naturforsch	Requires 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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	Identifier	ZNB-1994-49b-1781
	Volume	49

14	Author	Matthias Westerhausen, Bernd Radem, Wolfgang Schwarz, Sonja Henkel	Requires 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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	Identifier	ZNB-1994-49b-0199
	Volume	49

15	Author	WolfPeter Fehlhammer, Thomas Bliß, Wilfried Sperber, Joachim Fuchs	Requires 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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	Identifier	ZNB-1994-49b-0494
	Volume	49

16	Author	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

17	Author	Axel Fischer, Ion Neda, Thomas Kaukorat, Ralf Sonnenburg, PeterG. Jones, R.Einhard Schmutzler	Requires 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