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1

1	Author	Abdussalam Maihub, HuiBi Xu, GerhardN. Schrauzer	Requires cookie*
	Title	Studies on Vitamin B12 and Related Compounds, 51 [1] Direct Syntheses of Alkylcobalamins from Alkanes and Vitamin B12r under "Oxidizing-Reducing" Conditions
	Abstract	Syntheses of methylcobalamin from methane, and of n-alkylcobalamins from n-alkanes (C2 C10) and vitamin Bi2r are described. The compounds are formed under "oxidizing-reducing" conditions: Oxygen radicals (02~, HOO -, and HO') are generated from the reaction of O2 with reducing metal ions, notably V +3 (aq) and abstract hydrogen from the alkane substrates. The resulting alkyl radicals are captured by vitamin Bj2r with high efficiency to yield alkylcobalamins. The reactions take place at room temperature in mildly alkaline or acidic solutions. In addition to n-alkylcobalamins, the preparation of neopentylcobalamin from neopentane, of isobutylcobalamin from isobutane, and of several cycloalkylcobalamins from cycloalkanes, is also reported. Methyl radicals generated in D20 from CH4 under "oxidizing-reducing" conditions are reduced to yield CH3D.
	Reference	Z. Naturforsch. 35b, 1435—1438 (1980); received April 25 1980
	Published	1980
	Keywords	Alkylcobalamins, Synthesis, Alkanes
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	Identifier	ZNB-1980-35b-1435
	Volume	35

2	Author	Ulrich Wannagat, Thomas Blumenthal, Gerd Eisele, Axel König, Reinhard Schächter, Braunschweig	Requires cookie*
	Title	Synthese von neuen Silazangerüstsystemen * Synthesis of Some Silazane Frameworks
	Abstract	Some novel silazane frameworks (scheme 1: H,J, K, M, P) were synthesized and charac-terized by mainly methyl substituted derivatives. Synthetic routes are given in Scheme 2 and 3, respectively, as well as in equations (13) and (14). Compounds are described in their properties, physical data and elemental and structure analysis.
	Reference	Z. Naturforsch. 36b, 1479—1485 (1981); eingegangen am 7. Mai 1981
	Published	1981
	Keywords	Silazanes, Cyclosilazanes, Synthesis
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	Identifier	ZNB-1981-36b-1479
	Volume	36

3	Author	Wolfgang Haubold, Armin Gemmler, Ullrich Kraatz	Requires cookie*
	Title	Tetramethylsilan -ein Methylierungsreagenz für Bortrihalogenide Tetramethylsilane -a Methylating Agent for Borontrihalides
	Abstract	The interaction of tetramethylsilane and BY3 (Y = Br, I) in a 1:1 ratio at elevated temperature yields quantitatively MesSiY (Me = CH3) and MeBY2, while a 2:1 ratio gives 2 moles MesSiY and Me2BY. Except for MeBl2 the reactions are convenient routes for the preparation of these compounds. -Using CD3BI2 the reaction path of the formation of MP2BI was studied.
	Reference	Z. Naturforsch. 33b, 140—141 (1978); eingegangen am 21. Dezember 1977
	Published	1978
	Keywords	Tetramethylsilane, Tribromoborane, Triiodoborane, Synthesis, Methylboronhalides
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	TEI-XML for	default:Reihe_B/33/ZNB-1978-33b-0140.pdf
	Identifier	ZNB-1978-33b-0140
	Volume	33

4	Author	Dieter Weber	Requires cookie*
	Title	CHsNHsSnBraJa-z = 0-3), a Sn(II)-System with Cubic Perovskite Structure
	Abstract	CH3NH3SnBr^l3 -.x [x = 0—3) has the cubic perovskite structure with the unit cell parameters a = 5.89 A {x = 3), a = 6.01 A (x = 2) and a = 6.24 A (x = 0) and Z = 1. The compounds show intense colour and conducting property. The U9 Sn Mössbauer data are consistent with the high symmetry environment of the Sn(II)-ion. A bonding model, using a "p-resonance-bonding", can explain the properties of the cubic system. The synthesis is described.
	Reference	Z. Naturforsch. 33b, 862—865 (1978); eingegangen am 5. Mai 1978
	Published	1978
	Keywords	Synthesis, X-ray, Mössbauer Spectra
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	TEI-XML for	default:Reihe_B/33/ZNB-1978-33b-0862.pdf
	Identifier	ZNB-1978-33b-0862
	Volume	33

5	Author	S. Sarkar, A. Midler	Requires cookie*
	Title	von Nitrosyl-Komplexen. Direkte Darstellung von Thiocyanatonitro- syl-Komplexen und von [Mo(NO)(CN)5] 3 - A Contribution on the Synthesis and Reactivity of Nitrosyl Complexes. Direct Preparation of Thiocyanatonitrosvl Complexes and of [Mo(NO)(CN)5] 3
	Abstract	Some new aspects of the synthesis and reacti-vity of nitrosyl complexes are given. The com-plexes [Cr(NO)(NCS5] 3 -, [Mo(NO)(NCS)4] 2 -[3a], [Os(NO)(NCS)5] 2 -and [Mo(NO)(CN)5] 3 -have been isolated as tetraphenylphosphonium salts.
	Reference	Z. Naturforsch. 33b, 1053—1055 (1978); eingegangen am 8. Mai/5. Juni 1978
	Published	1978
	Keywords	Synthesis, Reactivity, Nitrosyl Complexes
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	Identifier	ZNB-1978-33b-1053_n
	Volume	33

6	Author	OttoJ. Scherer, Norbert Kuhn, Heribert Jungmann	Requires cookie*
	Title	Elementorganische Amin/Imin-Verbindungen, XIX [1] Phospha(III)azen-Komplexe des Platins Elementorganic Amino/Imino Compounds, XIX [1] Phospha(III)azene Complexes of Platinum
	Abstract	Reacting Zeise's salt with the phospha(III)azene (R3C)(R3Si)N-P = N-CR3 (R = CH3) (1) one gets the platinum phospha(III)azene complex (2), Cl2PtI<2 (L = 1). 2 adds water and methanol to the P=N bond of the phospha(III)azene ligand with formation of 3, Cl2Pt(PRR2 1)2 (R = (CH3)3SiO, R 1 = (CH3)3CNH) and 4, Cl2Pt(PRR 1 R 2)2 (R = CH30, R 1 = (CH3)3CNH, R2 = (CH3)3SiNC(CH3)3). 2, 3 and 4 have trans configuration, 4 also forms a mixture of the meso and d, 1 isomers. For 2 a P-a coordination of the phospha(III)-azene ligand is proposed. Die inzwischen in größerer Anzahl bekanntge-wordenen Phospha(III)azene des Typs A [la] /Py -W X N-A I
	Reference	Z. Naturforsch. 33b, 1321—1324 (1978); eingegangen am 12. Juli 1978
	Published	1978
	Keywords	Synthesis, Addition Reactions, Diastereoisomers, NMR
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	TEI-XML for	default:Reihe_B/33/ZNB-1978-33b-1321.pdf
	Identifier	ZNB-1978-33b-1321
	Volume	33

7	Author	AbdelKader Fathy, El-Sayed Amer, Mohamed Afsah, MohamedAbbas Tawfik El-Zimaity, Metwally	Requires cookie*
	Title	Synthesis of Hexahydro-bisfbenzo-dipyrazolones, benzo-diazepinone] and Dithiopyrimidoquinazolinetetrone
	Abstract	A new series of hexahydro-bis-benzodipyrazolones (2a-e) were obtained by the inter-action of 1 with hydrazines. These pyrazolones underwent coupling reaction with different diazonium salts to give 7a-g. Compound 1 when treated with acid hydrazides gave 3 a, b, and when subjected to Japp-Klingemann reaction in alkaline medium gave 6a-e. The hexahydro-bis-benzodiazepine (8), and dithiopyrimidoquinazolinetetrone (10) were obtained by the interaction of 1 with o-phenylenediamine and thiourea respectively.
	Reference	(Z. Naturforsch. 34b, 95—98 [1979]; received June 5 1978)
	Published	1979
	Keywords	Pyrazolones, Diazonium Salts, Synthesis
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	TEI-XML for	default:Reihe_B/34/ZNB-1979-34b-0095.pdf
	Identifier	ZNB-1979-34b-0095
	Volume	34

8	Author	P. Rodighiero, A. Guiotto, P. Manzini, G. Pastorini	Requires cookie*
	Title	Synthesis of Isoponcimarin
	Abstract	Synthesis of isoponcimarin, 7-(3'-methyl-2',3'-epoxy-butiloxy)-8-(3"-methyl-2"-oxo-butyl) coumarin, a natural coumarin isolated from Poncirus trifoliata L., was obtained starting from acetyl osthenol. From the intermediate 7-acetoxy-8-(3'-methyl-2'-oxobutyl) coumarin, the coumarin derivatives isomeranzin and dihydrooroselone were also prepared. In a previous paper [1] we reported the isolation and identification from unripe fruits of Poncirus trifoliata L. (fam. Rutaceae; subfam. Aurantioideae) of a new coumarin, which was named isoponcimarin. This compound is a neutral coumarinic derivative, optically active [a]»j5 — 6,94° (CHCls), m.p. 85 °C (from w-hexane), violet-blue fluorescent to UV light (365 nm) and has molecular formula C18H22O5. On the basis of the chemical and spectroscopical evi-dences to isoponcimarin was assigned the structure
	Reference	Z. Naturforsch. 34b, 1010—1014 (1979); received February 19 1979
	Published	1979
	Keywords	Isoponcimarin, Isomeranzin, Dihydrooroselone, Synthesis
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	TEI-XML for	default:Reihe_B/34/ZNB-1979-34b-1010.pdf
	Identifier	ZNB-1979-34b-1010
	Volume	34

9	Author	Dirk Dahmann, Hans Rose, Wolfgang Walz	Requires cookie*
	Title	Darstellung und Struktur von Phosphazenylcyclophosphazenen Synthesis and Structure of Phosphazenylcyclophosphazenes
	Abstract	Various phosphazenylcyclophosphazenes N3P3Xn(N = PA3)e-n with X = Cl, F, A = Me, Ph, NMe2, OEt, OPr», OBut" and n = 1-3 were obtained by desilylation methods. Chemical and spectroscopical properties dependent on the substituents are discussed. Isomers of di-and tri-substituted compounds were isolated and their structures elucidated by NMR spectroscopy.
	Reference	Z. Naturforsch. 35b, 964—969 (1980); eingegangen am 14. Dezember 1979
	Published	1980
	Keywords	Phosphazenylcyclophosphazenes, Molecular Structure, Synthesis
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	TEI-XML for	default:Reihe_B/35/ZNB-1980-35b-0964.pdf
	Identifier	ZNB-1980-35b-0964
	Volume	35

10	Author	El-Sayed Afsah, FathyA. Amer, MohamedA. Metwally, MohamedT. El-Zimaity	Requires cookie*
	Title	Synthesis of Hexahydroindazole, Tetrahydro-[pyrimidoquinazolinone, benzodiisoxazolone] Derivatives and Anils from Diethyl l,4-Cyclohexanedione-2,5-dicarboxylate
	Abstract	Treatment of diethyl l,4-cyclohexanedione-2,5-dicarboxylate (1) with hydrazine hydrate in glacial acetic acid afforded the diazobicycloocatdienedicarboxylate (2) and the azine (3). On the other hand, condensation of 1 with benzenesulphonylhydrazide in ethanolic solution gave the indazole derivative (4). Interaction of 1 with urea or hydroxyl-amine afforded the tetrahydropyrimidoquinazolinone (5) and the tetrahydrobenzodi-isoxazolone (6), respectively. Treatment of 1 with aniline gave the mono-anil (7) which, when subjected to Japp-Klingemann reaction with ja-anisidine gave the dihydrazonoanil (8) and their condensation with benzidine in acetic acid gave the hydrazonoketoester (9). On the other hand condensation of 7 with hydrazine hydrate in ethanolic solution af-forded the azobis (5-anilinoterephthalate) (10) and the hexahydrobenzodipyrazolone (11).
	Reference	Z. Naturforsch. 35b, 1310—1312 (1980); received February 8/April 10 1980
	Published	1980
	Keywords	Indazolones, Isoxazolones, Quinazlinones, Synthesis
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	Identifier	ZNB-1980-35b-1310
	Volume	35

11	Author	FathyA. Amer, El-Sayed Afsah, MohamedA. Metwally, MohamedT. El-Zimaity	Requires cookie*
	Title	Related Compounds from l,4-Bis(ethoxycarbonyl)-2,5-diamino-l,4-cyclohexadiene
	Abstract	Interaction of o-phenylenediamine with l,4-Bis-(ethoxycarbonyl)-2,5-diamino-l,4-cyclo-hexadiene (1) gave 2, which cyclised to the hexahydrobenzodiazepinone (3). On the other hand, interaction of 1 with o-aminophenol, gave compound 4 which on treatment with polyphosphoric acid gave the tetrahydrobis-benzooxazepinone (11). Treatment of 1 with phenylisothiocyanate and formamide afforded the dithiopyrimidoquinazolinone (8) and the tetrahydropyrimidoquinazolinone (9), while the interaction of 1 with benzenesulphonyl-chloride gave dibenzenesulphonamido-cyclohexadiene dicarboxylate (10). The structure of these compounds was established by chemical and spectroscopic methods.
	Reference	Z. Naturforsch. 35b, 1395—1397 (1980); received July 13/October 11 1979/May 2 1980
	Published	1980
	Keywords	Diazepinones, Oxazepinones, Pyrimidoquinazolinones, Synthesis
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	Identifier	ZNB-1980-35b-1395
	Volume	35

12	Author	Ingrid Riess-Maurer, Hildebert Wagner, András Lipták	Requires cookie*
	Title	Synthesis of Kaempferol-3-0-(3",4'' -di-O-a-L-rhamnopyranosy^-^-D-galactopyranoside and its Comparison with the Natural Ascaside Isolated from Astragalus caucasicus
	Abstract	The trisaccharide, 3,4-di-0-(a-L-rhamnopyranosyl)-D-galactose was synthesized using benzyl 2,6-di-0-benzyl-/?-D-galactopyranoside as starting compound. Its acetobromo derivative was coupled with 4',7-di-O-benzyl-kaempferol. The structure of the synthetic kaempferol trioside was characterised by different spectroscopic methods (UV, IR, X H, 13 C NMR and MS). Chromatographic and mass spectrometric comparison of the synthetic product with ascaside precluded their identity.
	Reference	Z. Naturforsch. 36b, 257—261 (1981); received October 21 1980
	Published	1981
	Keywords	Trisaccharide, Synthesis, Synthetic Kaempferol Trioside
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	TEI-XML for	default:Reihe_B/36/ZNB-1981-36b-0257.pdf
	Identifier	ZNB-1981-36b-0257
	Volume	36

13	Author	Birgit Lehnis, Joachim Strähle	Requires cookie*
	Title	Synthese und Kristallstruktur von C83(AuBr 4 ) 2 Br3 Synthesis and Crystal Structure of Cs3(AuBr4) 2 Br 3
	Abstract	Cs3(AuBr4)2Br3 is obtained in the form of red needles by adding the stoichiometric amount of CsBr to a solution of HAuBr4 and Br3~ in aqueous HBr. The salt decomposes slowly at room temperature to form a mixed-valent, cubic bromo aurate(I,III), in which the linear AuBr 2 ~ ions are partially substituted by Br3~ ions. At 140 °C Cs 2 Au 2 Bre and CsBr are formed. Cs3(AuBr4) 2 Br3 crystallizes monoclinic with four formula units in the space group P2i/c. The structure is built up by AuBr 4 ~ and Br3~ anions and Cs+ cations. An average Au-Br distance of 242.2 pm was found for the square planar AuBr 4 ~ ion. The linear Br3~ groups are almost symmetrical with Br-Br distances of 254.0 and 256.2 pm. Therefore only two vibrations are observed in the IR spectrum: Vas = 172, <5 = 56 cm -1 . The absorptions of the AuBr 4 _ groups are: vas = 250, <5as= 113, y — 102 cm -1 .
	Reference	Z. Naturforsch. 36b, 1504—1508 (1981); eingegangen am 8. September 1981
	Published	1981
	Keywords	Synthesis, IR Spectra, Crystal Structure
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	Identifier	ZNB-1981-36b-1504
	Volume	36

14	Author	BharatB. Kaul, D. Sellmann	Requires cookie*
	Title	Transition Metal Complexes with Sulfur Ligands, IV [1] Synthesis and Reactions of Mo (IV) Complexes with the Tetradentate Thioether-thiol Ligand 2,3,8,9-Dibenzo-l,4,7,10-tetrathiadecane
	Abstract	Synthesis and characterization of non-oxo Mo(IV) complexes with the tetradentate thioether-thiol ligand 2,3,8,9-dibenzo-l,4,7,10-tetrathiadecane(dttd-H2) are reported. MoCl4(THF)2 reacts with dttd-H2 in THF at room temperature to give the paramagnetic (2.61 BM, 295 K) [Mo(dttd)Cl2]. The chlorine ligands in [Mo(dttd)Cl2] can be substituted by sulfur ligands yielding diamagnetic complexes as [Mo(dttd)(CeH4S2)], [Mo(dttd)(SC2HiS)] and [Mo(dttd)(SC2H5)2]; with Na2S, NaHS or H2S, the di-^-sulfido bridged complex [(dttd)Mo(S)2Mo(dttd)] is obtained. The reduction of [Mo(dttd)Cl2] by various reducing agents in the presence of CO or NO yields labile carbonyl and nitrosyl species in solution. In contrast to [Mo(dttd)Cl2], the complexes with MoSe cbromophores showed no reactivity to CO or NO under reducing conditions.
	Reference	Z. Naturforsch. 38b, 562—567 (1983); received January 19 1982
	Published	1983
	Keywords	Molybdenum(IV) Sulfur Complexes, Synthesis, Reactions
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	TEI-XML for	default:Reihe_B/38/ZNB-1983-38b-0562.pdf
	Identifier	ZNB-1983-38b-0562
	Volume	38

15	Author	CorneliusG. Kreiter, Ulrich Koemm	Requires cookie*
	Title	Gehinderte Ligandbewegungen in Übergangsmetallkomplexen, XIX [1] Oktaedrische Wolfram-Olefin-Komplexe mit Bisphospbinoethan-Liganden Hindered Ligand Motions in Transition Metal Complexes, XIX [I] Octahedral Tungsten Olefin Complexes with Bisphosphinoethane Ligands
	Abstract	(OC-6-32)-W(CO)3[(CH3)2PC2H4P(CH3)2](olefin) complexes (9-14) were prepared photochemicallyfromW(CO)4[(CH3)2PC2H4P(CH3)2](l)viaW(CO)3[(CH3)2PC2H4P(CH3)2]-(THF) (2) and the electron poor olefins dimethyl malonate(3), fumarate (4), methylfuma-rate (5), fiuorofumarate (6), chlorofumarate (7) and bromofumarate (8). The stereoche-mistry of 9-14 was elucidated by IR and NMR spectroscopy. The hindered rotations of the olefin ligands in 9-14 were studied by D-NMR spectroscopy. 11-14 form two diastereomeric isomers when the olefin rotation is freezed. The spectroscopic behaviour of the dimethyl fumarate complex 10 gives unambiguous proof for the rotation of the olefin ligand around the metal-olefin-bond. Alternative motions are ruled out.
	Reference	Z. Naturforsch. 38b, 943—952 (1983); eingegangen am 7. Februar/15. März 1983
	Published	1983
	Keywords	Olefin Complexes, Synthesis, Ligand Rotations
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	TEI-XML for	default:Reihe_B/38/ZNB-1983-38b-0943.pdf
	Identifier	ZNB-1983-38b-0943
	Volume	38

16	Author	Bernhard Czeska, Kurt Dehnicke	Requires cookie*
	Title	[P(C 6 H 5 ) 4 ] 2 S 8 : Synthesis and IR Spectrum
	Abstract	[P(C 6 H 5)4] 2 S g was prepared from Na 2 S 4 and PPh 4 Cl in ethanol solution and characterized by its IR spectrum.
	Reference	(Z. Naturforsch. 40b, 120—121 [1985]; eingegangen am 28. September 1984)
	Published	1985
	Keywords	Tetraphenylphosphonium Octasulfide, Synthesis, IR Spectra
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	Identifier	ZNB-1985-40b-0120_n
	Volume	40

17	Author	Karl Häberle, Martin Dräger	Requires cookie*
	Title	Über Polygermane, XVIII [1] Drucksynthese der mehrfach funktionellen Digermane Ph 6 _"Ge 2 Cl" (n = 2, 3, 4) und von Ph 2 GeCl 2 On Polygermanes, XVIII [1] Synthesis of the Multifunctional Digermanes Ph 6 _"Ge 2 Cl" (n = 2, 3, 4) and of Ph 2 GeCl 2 under Pressure
	Abstract	Reaction of Ph 6 Ge 2 with liquid HCl under pressure leads to di-, tri-and tetrachloro phenyl-digermanes. The yield of higher chlorinated products increases with increasing pressure. The analogous reaction of Ph 4 Ge yields Ph 2 GeCl 2 quantitatively. The Ge-Ge bond is most unstable in the case of Ph 3 Ge 2 Cl 3 both chemically and thermally. The crystal structure of Ph 2 Ge 2 Cl 4 has been determined (R = 0.057), Ge-Ge 241.3(1) pm.
	Reference	Z. Naturforsch. 42b, 323 (1987); eingegangen am 15. September/24. November 1986
	Published	1987
	Keywords	Functional Digermanes, Synthesis, Structure
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	TEI-XML for	default:Reihe_B/42/ZNB-1987-42b-0323.pdf
	Identifier	ZNB-1987-42b-0323
	Volume	42

18	Author	Dieter Sellmann, Gerhard Binker	Requires cookie*
	Title	Übergangsmetall-Komplexe mit Schwefelliganden, XXVII* Synthese und Reaktivität der Nitrosyl-und Nitrido-Ruthenium-Komplexe mit 1,2-Benzoldithiolat-Liganden [Ru(NO)(S 2 C 6 H 4 ) 2 r bzw. [Ru(N)(S 2 C 6 H 4 ) 2 r Transition Metal Complexes with Sulfur Ligands, XXVII* Synthesis and Reactivity of the Nitrosyl-and Nitrido-Ruthenium Complexes with 1,2-Benzenedithiolate Ligands [Ru(NO)(S 2 C 6 H 4 ) 2 ]~ and [Ru(N)(S 2 C 6 H 4 ) 2 ]~, Respectively
	Abstract	The reaction of [Ru(NO) 2 (PPh 3) 2 ], [RuCl(NO) 2 (PPh 3) 2 ]PF 6 or [RuCl 3 (NO)(PPh 3) 2 ] with 1,2-benzenedithiolate(—2), C 6 H 4 S 2 : ~, leads to the 16e"-complex [Ru(NO)(S 2 C 6 H 4) 2 ]~, which was isolated as the NBu 4 + salt (1). The square pyramidal anion in [NBu 4 ][Ru(NO)(S 2 C 6 H 4) 2 ] coordi-nates PMe 3 with rearrangement of the sulfur ligands to give the six-coordinate cis-[NBu 4 ][Ru(NO)(PMe 3)(S 2 C 6 H 4) 2 ] (3); the rearrangement of the C 6 H 4 S 2 2 "-ligands from trans to eis coordination is proved by 13 C NMR spectroscopy. [Ru(NO)(S 2 C 6 H 4) 2 ]~ is rapidly reduced even under mild conditions. Reaction of 1 with NaBH 4 in MeOH leads to the reduction of NO to a nitrido ligand and the concomitant oxidation of (formal) Ru(III) to Ru(VI) yielding [NBu 4 ][Ru(N)(S^C 6 H 4)->] (2). This compound is also formed when the nitrosyl complex is reacted with SiMe 3 N 3 . [Ru(NO) 2 (PPh 3) 2 ] and [RuCl(NO) 2 (PPh 3) 2 ]PF 6 are denitrosylatedby dttd 2 ~ (dttd 2 " = 2,3,8,9-dibenzo-l,4,7,lÖ-tetrathiadecane(—2)) to give [Ru(dttd)(PPh 3) 2 ],
	Reference	Z. Naturforsch. 42b, 341—347 (1987); eingegangen am 10. November 1986
	Published	1987
	Keywords	Ruthenium Sulfur Complexes, Synthesis, Reactions
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	TEI-XML for	default:Reihe_B/42/ZNB-1987-42b-0341.pdf
	Identifier	ZNB-1987-42b-0341
	Volume	42

19	Author	Siegfried Pohl, Wolfgang Saak, Detlev Haase	Requires cookie*
	Title	Darstellung und Kristallstrukturen von (Ph4P)4Sb8I28 und (Ph4P)Sb3l 10 (Ph = C6H5) Synthesis and Crystal Structures of (Ph4P)4Sb8I28 and (Ph4P)Sb3 l 1 0 (Ph = C6H 5)
	Abstract	The compounds (Ph4P)4Sb8l 28 (1) and (Ph4P)Sb,Iio (2) were prepared by the reaction of Sbl3 and Ph4PI in acetonitrile (molar ratios 2:1 and 3:1 respectively). The structures of 1 and 2 were determined from single crystal X-ray diffraction data. 1 crystallizes in the triclinic space group P I with a = 1321.7(5), b = 1346.7(5), c = 2201.8(8) pm, a = 104.18(2), ß = 99.92(2), y = 100.33(2)°; 2: monoclinic, C2/c, a = 2371.1(2), b = 745.0(1), c = 2495.1(2) pm, ß = 100.75(1)°. Whereas 1 exhibits isolated SbsI284' ions, the anions of 2 are built up of polymeric chains [Sb3I 10_]x. In both compounds the distorted Sbl6 octahedra are linked by common edges. The Sb—I distances are in the range between 277.4 and 354.8 pm (1) and between 277.4 and 342.4 pm (2). The observed structures do not only depend on stoichiometry. the nature of the counter cations, and the possibility of oligomerisation but also on the wide variety of the Sb—I bond strengths and the different bridges formed by iodine. The lone pair of Sb(III) seems to be predominantly 5s: .
	Reference	Z. Naturforsch. 42b, 1493—1499 (1987); eingegangen am 30. Juni 1987
	Published	1987
	Keywords	Iodoantimonates, Synthesis, Crystal Structure
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	Identifier	ZNB-1987-42b-1493
	Volume	42

20	Author	ManfredL. Ziegler, Klaus Blechschmitt, Harald Bock, Ernst Guggolz, RichardP. Korswagen	Requires cookie*
	Title	Über die Reaktivität von [(CH 3 ) 2 N] 6 W 2 (W=W) gegenüber CS 2 /S 8 und CS 2 /Se, Röntgenstrukturanalyse von [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 ) Reactivity of [(CH 3 ) 2 N] 6 W 2 (W=W) Towards CS 2 /S 8 and CS 2 /Se 8 . X-Ray Structure Analysis of [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 )
	Abstract	In this paper we report two improved preparation methods for [(CH 3) 2 N] 6 W 2 (W=W) (1), one starting from WC1 4 (yield 51%), and a second one starting from W 2 C1 6 (THF) 4 (ca. 60% yield). We have studied the reactions of 1 with different nucleophiles, among them triphenylalkylidenphos-phoranes (like Ph 3 P=CH 2 and Ph 3 P=CHPh • LiCl; Ph = phenyl), sulfur and CS 2 . 1 reacts with S 8 and CS 2 in hexane to yield the two new compounds (Me 2 NCS 2) 2 WS(S 2) (4) and W(CS 2 H)(Me 2 NCS 2) 2 (5), both containing dithiocarbamato ligands formed by insertion of CS 2 into the W-N bond. The two mononuclear compounds were characterized spectroscopically, in the case of 4 an X-ray diffraction structure analysis was performed. The reaction of 1 with Se and CS 2 , leads to the compounds 4, (Me 2 NCS 2) 2 W 2 S 4 (6) and [(Me 2 N) 2 C]CS 2 (7), which were also characterized spectroscopically. No Se-containing compounds could be isolated. 4 crystallizes monoclinically, C 5 2h -P2Jn, with a = 648.6(3), b = 1346.7(6) and c = 1745.9(7) pm, ß = 91.85(3)°, V = 1524xl0 6 pm 3 , Z = 4. The structure of the seven-coordinate tungsten compound is discussed and compared to complexes with similar ligands and geometry.
	Reference	Z. Naturforsch. 43b, 590—598 (1988); eingegangen am 28. Dezember 1987
	Published	1988
	Keywords	Reactivity, Synthesis, X-Ray
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	Identifier	ZNB-1988-43b-0590
	Volume	43

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