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21	Author	C. H. Rüscher, M. Zimmermann, M. Götte	Requires cookie*
	Title	Investigations of the Anisotropic Optical Reflectivity of Binary and Ternary Nb-W Oxides Possessing Block-Type Crystal Structure
	Abstract	We have studied the anisotropic optical properties of binary Nb0 2 5 _ a (0 < Ö < 0.083) and ternary Nb 18 _ £ W 8+£ 0 6? (e = 0,1,..., 9) compounds using the polarized regular-reflection method. We observed strong anisotropic behaviour for all reduced phases. The anisotropic effect can be related to the crystallographical structure principle and to the doping of charge carriers by the reduction of oxygen (<5) or substitution of W for Nb (e) in the binary and ternary oxides, respectively. Our results indicate that the charge carriers are confined to the structural block units. For increasing 3 and e, metal-like properties occur (<5 > 0.1, e > 8) in the infinite block direction only.
	Reference	Z. Naturforsch. 48a, 443—446 (1993); received December 31 1991
	Published	1993
	Keywords	Optical reflectivity, Block-type crystal structure, Niobium oxide, Niobium tungsten oxide
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	TEI-XML for	default:Reihe_A/48/ZNA-1993-48a-0443.pdf
	Identifier	ZNA-1993-48a-0443
	Volume	48

22	Author	K. Arl Hensen, PeterW. Ag, N. Er+	Requires cookie*
	Title	Die Kristallstruktur der Verbindung N-Trimethylsilyl-3,4-Dimethylpyridiniumbromid The C rystal Structure o f N -T rim ethylsilyl-3,4-dim ethylpyridinium Brom ide
	Abstract	Trimethylbromosilane and 3,4-lutidine form a 1:1 com pound which is stable at room tem perature. Single crystals of this com pound can be isolated by sublimation. It crystallizes in the orthorhom bic space group P 2,2,2, with lattice constants a = 737,08(9) pm, b = 1295,7(1) pm, c = 1318,8(3) pm. The crystal structure was refined to Rw = 0,042 and proves an ionic struc ture.
	Reference	(Z. Naturforsch. 48b, 79—81 [1993]; eingegangen am 21. Februar 1992)
	Published	1993
	Keywords	Trimethylbromosilane, 3, 4-Dimethylpyridine, Addition Com pound, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0079.pdf
	Identifier	ZNB-1993-48b-0079
	Volume	48

23	Author	Michael Plate, Gerlinde Frenzen, K. Urt Dehnicke	Requires cookie*
	Title	Synthese und Kristallstrukturen der ionischen Kronenetherkomplexe [TiCl3(15-Krone-5)(CH3CN)l[SbCl6l und \| V Cl(OH)( 18-Krone-6)(CH3CN)2] [SbCl6l * V2(18-Krone-6 * CH3CN) Synthesis and Crystal Structures of the Ionic Crown Ether Complexes [TiCl3( 15-Crown-5)(CH3CN)][SbCl6] and [VCl(OH)( 18-Crown-6)(CH3C N )2][SbCl6] ■ 'A( 18-Crown-6 * C H 3CN)
	Abstract	The title compounds were prepared by the reaction o f titanium tetrachloride with 15-crown-5 and antimony pentachloride, and by the reaction o f vanadium trichloride with 18-crown-6 and antimony pentachloride in the presence o f traces o f water in acetonitrile solution, respectively. The complexes were characterized by IR spectroscopy and by X-ray structure determinations. [TiCl3(15-crown-5)(CH1CN)][SbCl6]: Space group Pnma, Z = 4, 1355 observed unique reflec tions, R = 0.035. Lattice dim ensions at -8 0 °C: a = 1987(1), b = 1742.2(6), c = 111.0(2) pm. The com pound consists o f SbCl6~ anions and cations [TiCl3(15-crown-5)(CH3C N)]+, in which the titanium atom is coordinated octahedrally by three chlorine atom s in facial arrangement, by the nitrogen atom o f the acetonitrile m olecule, and by two oxygen atom s o f the crown ether molecule. [VCl(OH)(18 -crown-6)(C H 3C N)2][SbCl6] ■ 'A(18-crow n-6 • C H 3 CN); Space group P I, 3936 observed unique reflections, R = 0.014. Lattice dim ensions at -8 0 °C: a = 1194.2(6), b = 1349.8(6), c = 1365.5(6) pm, « = 93.55(4)°, ß = 111.23(4)°, y = 93.15(4)°. The com pound con sists o f SbCl6-anions, included 18-crown-6 and acetonitrile molecules, and cations [VCl(OH)(18-crown-6)(CH3C N)2]+, in which the vanadium atom is octahedrally coordinated by two nitrogen atoms o f the acetonitrile molecules in trans positions, by a chlorine atom and a hydroxyl group in cis position, and by two oxygen atom s o f the crown ether molecule. One o f the acetonitrile molecules forms weak hydrogen bridges with two oxygen atom s o f the includ ed crown ether molecule as well as with one chlorine atom o f the SbCl6" ion.
	Reference	Z. Naturforsch. 48b, 149—155 (1993); eingegangen am 4. September 1992
	Published	1993
	Keywords	Crown Ether Complexes, Titanium, Vanadium, IR Spectra, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0149.pdf
	Identifier	ZNB-1993-48b-0149
	Volume	48

24	Author	Lothar Ohse, Mehmet Somer, Wolfgang Blase, Gerhard Cordier	Requires cookie*
	Title	Verbindungen mit SiS2-isosteren Anionen i
	Abstract	[AlX4/2 3 ] und i \|InP4/23 ]: Synthesen, Kristallstrukturen und Schwingungsspektren von Na3\|AlX2], K2Na[AlX2] und K3IInP2] (X = P, As) Com pounds with SiS2 Isoelectronic Anions l [A1X4 23-] and i [InP4/23-]: Synthesis, Crystal Structures and Vibrational Spectra of N a3[AlX2], K 2Na[AlX2] and K 3[InP2] (X = P, As) The title compounds were prepared from stoichiometric mixtures o f the elements or from alkali metals (Na, K), NaX (KX) and MX (M = Al, In; X = P, As) at 1000 K. The crystal structures (Ibam, No. 72) are characterized by infinite chains o f edge sharing tetrahedra j, [MX4;,3'] (M = Al, In; X = P, As) which are isoelectronic to SiS2. The vibrational spectra can be interpreted with respect to the symmetry P(2/m 2/c) 42/ m -D 4h of the isolated polymeric chain ][M X 4(23"]. The assignment of the observed frequen cies is supported by a normal coordinate analysis using the fragment method.
	Reference	Z. Naturforsch. 48b, 1027—1034 (1993); eingegangen am 29. März 1993
	Published	1993
	Keywords	Zintl Phases, Preparation, Crystal Structure, V ibrational Spectra, Force Constants
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	Identifier	ZNB-1993-48b-1027
	Volume	48

25	Author	Gerhard Cordier, Volker Müller	Requires cookie*
	Title	Darstellung und Kristallstruktur von K49T1108 Preparation and Crystal Structure of K49T1108
	Abstract	K49TI 10g was prepared from the elements (molar ratio K:T1 = 1:2) at 700 K. The crystal structure was determined by single crystal X-ray diffraction methods (a = 1728.7(1) pm, Pm 3, Z — 1, R = 0.086). It contains T l12 icosahedra and T l12 truncated tetrahedra (Kasper polyhed-ra). 20 truncated tetrahedra form Tlg4-polyhedra (Sam son polyhedra) by sharing hexagonal faces. These polyhedra are connected by com m on edges. Folded T l3-chains connect the icosa hedra and the Samson polyhedra to a framework. The truncated tetrahedra are occupied by potassium atoms.
	Reference	Z. Naturforsch. 48b, 1035—1040 (1993); eingegangen am 5. April 1993
	Published	1993
	Keywords	Intermetallic Compound, Potassium Thallide, Synthesis, Crystal Structure, Cluster Framework
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	Identifier	ZNB-1993-48b-1035
	Volume	48

26	Author	Hans-Jörg Hemmerling, Margarete Janoschka, Hartmut Wunderlich	Requires cookie*
	Title	Amidinadditionsprodukte des 1,2,3-Indantrionhydrats: Synthese und Strukturzuordnung durch Kristallstrukturanalyse, spektrale Daten und Blei(IV)acetatoxidation Products o f Am idinaddition to 1,2,3-Triketohydrindenhydrat: Synthesis and Determination by Crystal Structure, Spectral Data and Oxidation with Lead(IV)acetate
	Abstract	The addition o f amidines to 1,2,3-triketohydrindenhydrat gives cyclic dihydroxyindenoimi-dazoles. From N-substituted amidines mixtures o f regioisomeric derivatives were obtained. Analysis o f crystals revealed the major product o f 2 k to be 4 k. They belong to the monoclinic space group P 2 ,/c (a = 889.1(2); b = 1186.6(3); c = 2783.5(7) pm; ß = 91.26(2)°) with Z = 8 molecules including four molecules o f ethanole per unit cell. These results were confirmed by oxidation with lead(IV)acetate, which lead to derivatives o f isoindols.
	Reference	Z. Naturforsch. 48b, 1094—1104 (1993); eingegangen am 26. März 1993
	Published	1993
	Keywords	Indeno[l, 2-d]im idazoles, Triketohydrinden, Crystal Structure, Amidines, Isoindoles
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	Identifier	ZNB-1993-48b-1094
	Volume	48

27	Author	Andreas Korn, Sabine Rudolph-Böhner, Luis Moroder	Requires cookie*
	Title	Synthesis and Crystal Structure of Benzyl (-)-(2 S)-l-trityl-2-aziridinecarboxylate
	Abstract	Benzyl (-)-(2S)-l-trityl-2-aziridinecarboxylate (1) has been prepared by the reaction of N-trityl-L-serine benzyl ester and triethylam ine in toluene with S 0 2C12. X-ray, 'H N M R and gas chromatographic configuration analysis allowed to define the structure o f the compound as a rrans-isomer regarding ring substituents and as a (2 S)-enantiom er o f the chiral C2.
	Reference	Z. Naturforsch. 48b, 1146 (1993); received April 131993
	Published	1993
	Keywords	Aziridine, Synthesis, Crystal Structure, N M R Spectra, A bsolute Configuration
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-1146.pdf
	Identifier	ZNB-1993-48b-1146
	Volume	48

28	Author	Gerhard Müller, Joachim Lachmann	Requires cookie*
	Title	Sterisch belastete cyclische Phosphanborane Sterically Crowded Cyclic Phosphine-Boranes
	Abstract	A The anionic phosphine o-(diphenylphosphinomethyl)phenyl L has been used to prepare the sterically crowded cyclic phosphine-boranes BL3, 'BuBL2, and 'Bu2BL by reaction o f the lith-iated ligand LiL with B(OM e)3, 'BuB(OM e)2, and 'Bu2BOMe, respectively. In the new com pounds 'BuBL-, and 'Bu^BL one ligand L is bonded to the boron center by both its carbanionic and its phosptiino function with formation o f five-membered rings. In solution 11B and 31P N M R spectroscopy does not indicate substantial B -P dissociation, i.e., the existence o f three-coordinate boron. The steric bulk o f L in BL3 leads to the formation o f oligom ers in solution, presumably by a bridging coordination mode o f L to two boron centers. N o conclusive evi dence as to the monom eric or oligomeric nature o f BL3 in the solid state can be given, however. Five-membered ring form ation is proven for the solid state by X-ray structure determinations o f 'BuBL2 and 'Bu2BL which in addition confirm that the steric bulk o f L is superior to that o f a tert. butyl group.
	Reference	Z. Naturforsch. 48b, 1248 (1993); eingegangen am 13. Mai 1993
	Published	1993
	Keywords	nionic Benzylphosphines, Cyclic Phosphine-Boranes, Crystal Structure, Steric Hindrance
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-1248.pdf
	Identifier	ZNB-1993-48b-1248
	Volume	48

29	Author	DietrichM. Ootz, Dieter Stäben	Requires cookie*
	Title	Die Hydrate von terf-Butanol: Kristallstruktur von Me3COH * 2 H20 und Me3COH * 7 H20 [ 1 ]
	Abstract	The system /er/-butanol-water has been confirmed by X-ray powder diffraction and single crystal structure analysis to contain two hydrates, a dihydrate and a higher hydrate. The com position o f the latter, contradictory in the literature, could be resolved in favor o f the new one o f a heptahydrate. The dihydrate (m.p. 0.7 °C) is m onoclinic with space group P2, and Z = 2 formula units per unit cell o f dim ensions a = 6.017, b = 6.055, c = 10.377 A and ß -106.60° at -150 °C. The heptahydrate (m.p. -6 °C, dec.) is orthorhombic with space group Pnma, Z = 4, a -12.589, b = 15.251 and c = 6.645 A at -150 °C. Both hydrates contain characteristic layers o f hydrogen-bonded O atom s, which in the heptahydrate are further linked into a three-di-m ensional semi-clathrate structure.
	Reference	Z. Naturforsch. 48b, 1325—1330 (1993); eingegangen am 17. Mai 1993
	Published	1993
	Keywords	te/7-Butanol Hydrates, Melting Diagram, Crystal Structure, Hydrogen Bonding
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-1325.pdf
	Identifier	ZNB-1993-48b-1325
	Volume	48

30	Author	Henning Von Arnim, Kurt Dehnicke, Klaus Maczek, D. Ieter Fenske	Requires cookie*
	Title	Ionische Kronenetherkomplexe von Thallium(I), Blei(II) und Indium(III). Die Kristallstrukturen von [Tl(12-Krone-4)2][SbCl6], [Pb(15-Krone-5)2][SbCl6]2* [SbCl3(15-Krone-5>] und [In(12-Krone-4)2][SbCl6]3* 3 CH3CN
	Abstract	Ionic Crown E ther Complexes of Thallium(I), Lead(II), and Indium(III). Crystal Structures of [Tl(12-Crown-4)2][SbCl6], [Pb(15-Crown-5)2][SbCl6]2-[SbCl3(15-Crown-5)], and [In(12-Crown-4)2][SbCl6]3 -3 CH3CN T he ionic crown ether com plexes [Tl(12-crown-4)2][SbCl6] (1) and [In(12-crown-4)2][SbCl6]3-3 C H 3CN (3) have been prepared by reaction o f T1C1 and InCl3, respectively, with SbCl5 in the presence o f 12-crown-4 in acetonitrile solution. The lead com
	Reference	Z. Naturforsch. 48b, 1331 (1993); eingegangen am 3. Juni 1993
	Published	1993
	Keywords	Ionic Crown Ether Com plexes o f Thallium, Lead, Indium, Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-1331.pdf
	Identifier	ZNB-1993-48b-1331
	Volume	48

31	Author	Hans Wolkers, Ralf Stegmann, G. Ernot, Frenking, Kurt Dehnicke, D. Ieter Fenske, G.Erhard Baum	Requires cookie*
	Title	Das Methylviologen-Radikalkation. Synthese, Kristallstruktur und ab Rechnungen von N,N'-Dimethyl-4,4'-bipyridinium-chlorid-dihydrat The Methylviologen Radical Cation. Synthesis, Crystal Structure and ab initio Calculations of N,N' -Dimethyl-4,4'-bipyridinium Chloride Dihydrate
	Abstract	The title compound has been prepared by the reduction of N,N'-dimethyl-4,4'-bipyridinium dichloride with dilithium tritelluride in dimethylformamide solution. It forms deep blue crystal needles, which were characterized by a crystal structure determination. Space group Pna21; Z -8, 3450 observed unique reflections, R = 0.045. Lattice dimensions at -70 °C: a = 1707.6(8), b = 2323.9(11), c -664.6(3) pm. The N,N'-dimethyl-4,4'-bipyridinium radical cations are planar and form ion pairs in the lattice. The chloride ions together with the water molecules form an infinite network of hydrogen bridges along the crystallographic «-axis. The structural parameters of the radical cation are in excellent agreement with ab initio calculations.
	Reference	Z. Naturforsch. 48b, 1341—1347 (1993); eingegangen am 25. Juni 1993 N
	Published	1993
	Keywords	N'-Dimethyl-4, 4'-bipyridinium Chloride Dihydrate, Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-1341.pdf
	Identifier	ZNB-1993-48b-1341
	Volume	48

32	Author	Indium Gallium, ThalliumG. Erhard Müller, Joachim Lachmann	Requires cookie*
	Title	Vier-und fünffach koordinierte Organometall-Phosphankomplexe von Aluminium, Gallium, Indium und Thallium Four-and Five-Coordinate Organom etal Phosphine Complexes of Aluminum
	Abstract	A The organom etal phosphine complexes M L3 (L = [o-(Ph2PCH2)C6H4]"; M = A l3+, G a3+, In3+) are obtained from MC13 and the lithiated ligand in diethyl ether. Tl[o-(Ph2PC H 2)C6H 4]3 is prepared from T1C1 by a disproportionation reaction. M 1 species could not be detected with L as ligand. Al[o-(Ph2PCH 2)C6H4]3 is the first triorganoaluminum bis(phosphine) adduct where C3P2 pentacoordination at aluminum has been definitely proven for both the solution (<5(27A1) = 131 ppm, w 1/2 = 12 kHz) and the solid state (d (A l-P) = 2.676(3)/2.782(2) Ä). The trigonal-bipyramidal coordination geometry (C3P2) at Al is achieved by two o f the anionic phosphines acting as chelating ligands, spanning equatorial (C atoms) and axial sites (P atom s), while the third phosphine is only carbon-bonded. Like A1L3, the heavier congeners M L3 (M = G a, In, Tl) are stereochemically nonrigid molecules in solution. Surprisingly, in the solid state only InL3 resembles the aluminum complex (C3P2 penta-coordination) while G aL 3 and T1L3 contain four-coordinate metal centers (C3P). This may be rationalized by the notice ably less polar G a -P bonds as compared to A l-P and I n -P bonds, while in T1L3 the span o f the ligand is not sufficient to allow for chelating coordination at a five-(or six-)coordinate Tl center.
	Reference	Z. Naturforsch. 48b, 1544—1554 (1993); eingegangen am 12. Juli 1993
	Published	1993
	Keywords	nionic Benzylphosphines, Main Group Metals, Phosphine Complexes, Crystal Structure
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	Identifier	ZNB-1993-48b-1544
	Volume	48

33	Author	Ekkehard Lindner, Walter Wassing, R. Fawzi, M. Steimann	Requires cookie*
	Title	Zweikernige Mangan-und Rheniumkomplexe mit gemischt aliphatischen-aromatischen Kohlenwasserstoffbrücken Dinuclear Manganese and Rhenium Complexes with Mixed Aliphatic-Aromatic Hydrocarbon Bridges
	Abstract	The symmetrically hydrocarbon-bridged complexes (OC)5M -(C H 2)n+1-X -(C H 2)n+\|-M (CO)5 [n = 1, X = 1,4-C6H4, M = Mn (2a), M = Re (3a); n = 2, X = 1,4-C6H4, M = Mn (2b), M = Re (3b); n = 1, X = 1,3-C6H4, M = Mn (5a), M = Re (6a); n = 2, X = 1,3-C6H4, M = Mn (5b), M = Re (6b); n = 1, X = 1,2-C6H4, M = Mn (8a), M = Re (9a); n = 2, X = 1,2-C 6H4, M = Mn (8 b), M = Re (9b)] are obtained by the reaction of the bistriflates X[(CH2)"-C H 2-0 S 0 2CF3]2 [X = 1,4-C6H4, n = 1 (la), n = 2 (lb); X = 1,3-C6H4, n = 1 (4a), n = 2 (4b); X = 1,2-C6H4, n = 1 (7 a), n = 2 (7 b)] with the carbonyl metalates [M(CO)5]" (M = Mn, Re) in THF and dimethyl ether, respectively. According to an X-ray structural analysis 8a crystallizes in the triclinic space group PI with Z = 2. Depending on the solvent, the reaction of 7 a with [Mn(CO)5]" affords also the cyclic carbene complex 10 a. The behavior of the manganese compounds toward CO has been investigated exemplarily in the case of 8 a and leads to the diacyl complex l,2-C6H4[CH2CH2C (0)M n(C 0)5]2 (11). Upon reaction with Na2C 0 3/CH30 H 11 is con verted to give the corresponding diester 1,2-C6H4[CH2CH2C (0)0 C H 3]2 (12).
	Reference	Z. Naturforsch. 48b, 1651—1660 (1993); eingegangen am 2. Juli 1993
	Published	1993
	Keywords	Bistriflates, Hydrocarbon-Bridged Complexes, Manganese Complexes, Rhenium Complexes, Crystal Structure
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	Identifier	ZNB-1993-48b-1651
	Volume	48

34	Author	Hansjürgen Mattausch, Horst Borrmann, A.Rndt Simon, *. Sonderdruckanforderungen, ProfA. Dr, Simon	Requires cookie*
	Title	Y 7I6C30 : Ein Carbidoxid mit kondensierten Y 6C -O ktaedem und Y 40-T etraed em Y7I6C30 : A Carbide Oxide with Condensed Y6C-Octahedra and Y40 -T etrahedra
	Abstract	The new compound Y7I6C30 is prepared by re action of stoichiometric amounts of Y, YI3, Y20 3 and C in closed Ta capsules at 1370 K. Y,I6C30 forms bronze coloured, metallic, air and moisture sensitive crystals. It crystallizes in the space group Pmma (No. 51) with the lattice constants a = 2249.4(4), b = 383.7(1), c = 1079.1(1) pm. Within the crystal structure the C atoms and the O atoms are surrounded by Y atoms octahedrally and tetrahedrally, respectively. The Y6C octahedra and Y40 tetrahedra are condensed to form ondulated layers, which are separated by double layers of I atoms. Einleitung Metallreiche Halogenide der Seltenerdmetalle mit einem Halogen/M etallverhältnis kleiner als 2 [1] sind mit Ausnahm e der Sesquihalogenide SE2X3 [2,3,4] ternäre Verbindungen. In ihren Strukturen treten Nichtmetallatome wie H, B, C, N, Si oder Übergangsmetallatome wie zum Beispiel Fe, Co, Pt, Ru, A u durch SE-Atom e koordiniert auf. H [5] und N [6,7] bevorzugen tetraedrische, B, C, Si [1,8] und die Übergangsmetallatome [9,10,11] oktaedrische Plätze im Metallgerüst. Für Fe und Co wurde auch trigonal-prismatische Koordination durch SE-Atom e gefunden [12]. Ü ber den Einbau von O als interstitiellem Atom ist bisher nichts bekannt. Bei Untersuchungen im System Y/I/C erhielten wir durch Nebenreaktion bronzefarbene, lattenför
	Reference	Z. Naturforsch. 48b, 1828—1830 (1993); eingegangen am 1. Juli 1993
	Published	1993
	Keywords	Yttrium Iodide Carbide Oxide, Crystal Structure, Condensed Clusters, Metallic Behaviour
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	Identifier	ZNB-1993-48b-1828_n
	Volume	48

35	Author	Axel Deeg, Dietrich Mootz	Requires cookie*
	Title	Addukte Aromat/Chlorwasserstoff bei tiefen Temperaturen: Beiträge zu Bildung und Kristallstruktur [ 1 ] Adducts Arene/Hydrogen Chloride at Low Temperatures: C ontributions to Form ation and Crystal Structure [1]
	Abstract	The melting diagrams o f the systems benzene-HCl, toluene-HCl and mesitylene-HCl have been established and the crystal structures o f two adducts determined. The adduct tolu ene-2 HC1, melting incongruently at -1 1 5 °C, is monoclinic with space group C 2 /c and Z = 4 formula units per unit cell; the adduct mesitylene-HCl, m .p. -6 4 °C, is orthorhom bic with space group P bca and Z = 8. The HC1 molecules are situated on both sides and one side, respectively, o f the plane o f the aromatic system and are linked to it by weak hydrogen bonds o f the type C l-H — it.
	Reference	Z. Naturforsch. 48b, 571—5 (1993); eingegangen am 14. Dezember 1992
	Published	1993
	Keywords	Adducts Arene/HCl, Melting Diagrams, Crystal Structure, Hydrogen Bonding C l-H — it
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	Identifier	ZNB-1993-48b-0571
	Volume	48

36	Author	Karlheinz Sünkel, Adrian Blum, Barbara Wagner	Requires cookie*
	Title	Koordinationschemie perhalogenierter Cyclopentadiene und Alkine, XI [ 1 ]
	Abstract	Darstellung einiger Cymantrenyl-mono-und bis-thioether mit einer weiteren funktionellen Gruppe am Cyclopentadienylring. Molekülstruktur von [C5Cl2(SM e)2(PPh2)lM n(CO)3 C oordination Chemistry of Perhalogenated Cyclopentadienes and Alkynes, XI [1] Synthesis of Some Cymantrene Mono-and Bis-Thioethers with One Additional Functional G roup on the Cyclopentadienyl Ring. M olecular Structure of [C5Cl2(SMe)2(PPh2)]Mn(CO)3 The reaction o f [C5Cl4(SM e)]M n(CO)3 (la) with «-butyllithium and the electrophiles SiM e3Cl, C 0 2, or PPh,Cl regiospecifically yields the chiral 1,3-disubstituted functional cym an trene thioethers [C5Cl3(SM e)R]M n(CO)3 (R = SiM e3 (2), COOLi (3a), PPh2 (4)). 3 a can be protonated to give the corresponding carboxylic acid (3 b), which in turn can be transformed to the acid chloride [C5Cl3(SM e)(COCl)]M n(CO)3 (3c). 3c reacts with N a N 3 to yield after work-up the urea derivative O C [[N H -C 5Cl3(SM e)]M n(CO)3]2 (3d). U sing the cymantrene bis-thioethers [C5Cl3(SR)2]M n(CO)3 (R = Me, 5a, Ph, 5b) as starting materials, the carboxyl de rivatives [C5Cl2(SM e)2(COR)]M n(CO)3 (R = OLi, 6a, OH, 6b, Cl, 6 c) and the potential organometallic S,P-chelate ligands [C5Cl2(SR)2(PPh2)]M n(CO)3 (R = Me, 7 a , Ph, 7b) can be obtained. The crystal structure determination o f 7a (C " H 160 3PS-,CLMn, m onoclinic, P 2,/c, a = 18.714(6) A, b = 9.506(3) A, c = 14.475(3) A, ß = 109.18(2)°, V = 2432.1(12) A \ Z = 4) shows an orientation o f the neighbouring PPh2-and SMe groups, that allows chelation o f an additional metal fragment.
	Reference	Z. Naturforsch. 48b, 583—5 (1993); eingegangen am 16. N ovem ber 1992
	Published	1993
	Keywords	M ultifunctional Cymantrene Thioethers, Organometallic P -S -C h elate Ligand, Chiral Cyclopentadienyl Complexes, Crystal Structure
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	Identifier	ZNB-1993-48b-0583
	Volume	48

37	Author	". B. Preparation, 13cN., M. R., Vibrational Spectra, W. Preetz, A. Franken, M. R. Ath	Requires cookie*
	Title	Darstellung, UB-, 13C-NM R-und Schwingungsspektren der c/öso-Hexaborate [B6H 5(C N )\|2~ und m -[B 6H4(CN)2l2_ sowie Kristallstruktur von Cs2[B6H 5(CN)\|
	Abstract	of the c/oso-Hexaborates [B6H 5(CN)]2~ and c/s-[B6H 4(C N)2]2-, and the Crystal Structure o f Cs2[B6H 5(CN)] By reaction o f Cs2[B6H 6] with in situ generated dicyanogen in aqueous alkaline solution the m onocyanohydrohexaborate C s2[B6H5(CN)] and the dicyanohydrohexaborate cis-Cs,[B6H4(C N)2] are formed. The com pounds have been separated by ion exchange chrom atog raphy on diethylaminoethyl cellulose. The crystal structure o f Cs2[B6H5(CN)] was determined from single crystal X-ray diffraction analysis; monoclinic, space group P 2 Ja with a = 9.540(8), b = 9.977(3), c = 10.578(2) Ä, ß = 105.06(2)°. The B6 octahedron is compressed in the direction o f the nearly linear B -C N bond by about 5%, with bond lengths between 1.71 and 1.76Ä . The "B N M R spectra o f the two com pounds reveal the features o f substituted B6 cages with C4v and C2v point symmetry. In the l3C N M R spectrum o f Cs2[B6H 5(CN)] a quartet at -139 ppm with '/(C ,B) 92 Hz is observed. The IR and Raman spectra exhibit very strong CN stretching bands for Cs2[B6H5(CN)] at 2149, and for m -C s2[B6H4(C N)2] at 2170 c tr r 1.
	Reference	Z. Naturforsch. 48b, 598—6 (1993); eingegangen am 7. Dezember 1992
	Published	1993
	Keywords	M onocyanohydrohexaborate, m -Dicyanohydrohexaborate, Crystal Structure, 11B N M R Spectra, Vibrational Spectra
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	Identifier	ZNB-1993-48b-0598
	Volume	48

38	Author	Tetramethylammoniumfluorid Bildung, Wasserstoffbrückenbindung Struktur, Dieter Stäben, Dietrich Mootz	Requires cookie*
	Title	Die kristallinen Hydrate
	Abstract	The melting diagram of the system M e4N F -H 20 in the region 50-100 mol% H zO has been investigated for the first time, using D T A , D SC and tem perature-dependent X-ray powder diffraction. Four crystalline hydrates M e4N F\*H 20 were found, with x = 1 ,2 .3 3 ,4 and 5, which decom pose irreversibly above ca. 160 °C and m elt incongruently at 36 °C, congruently at 46 °C and again incongruently at 10 °C, respectively. The crystal structure o f each hydrate, except the already known one of the tetrahydrate, has b een determ ined with M oK a diffractom eter data. The monohydrate is rhombohedral with space group R3m and Z = 6 formula units per unit cell (hexagonal axes), the 2.33-hydrate m onoclinic with P2j/n and Z = 12, and the pen-tahydrate tetragonal with 142 m and Z = 2. The hydrogen-bonded H 20/F ~ structure is an iso lated centrosymmetric [F2(H 20) 2]2_ four-m em bered ring in the m onohydrate, a rather open three-dim ensional network in the 2.33-hydrate and a corrugated dense layer o f fused five-mem bered rings in the pentahydrate.
	Reference	Z. Naturforsch. 48b, 1057—57 (1993); eingegangen am 5. April 1993
	Published	1993
	Keywords	Tetramethylamm onium Fluoride, Fluoride Hydrates, M elting Diagram, Crystal Structure, Hydrogen Bonding
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	Volume	48

39	Author	Klaus Schulbert, R.Ainer Mattes	Requires cookie*
	Title	Kupfer-und Goldkomplexe von Dithiocarbaminsäureestern. Strukturen von [CuC1(L1)3] * CH2C12, [AuC1(L1)2], [CuI(L1)(PPh3)]2 und [Cu2ICuIICl4(L2)2]IJ (L1 = N-Phenyl-S-methyldithiocarbaminsäureester, L2 = N,N-Dimethyl-S-methyldithiocarbaminsäureester) N-Phenyl-S-methyldithiocarbamate, L2 = N,N-Dimethyl-S-methyldithiocarbamate)
	Abstract	Copper and Gold Complexes of Dithiocarbam ate Esters. X-Ray Structures of [CuC1(L1)3] ■ CH2C12, [A uC ^L 1^], [CuI(L1)(PPh3)]2 and [Cu2ICuIICl4(L2)2]n (L 1 = Reactions of N-phenyl-S-methyldithiocarbamate (L1) and N,N-dimethyl-S-methyldithio-carbamate (L2) with CuCl2, [CUjI^PPhj^] and HAuC14 yield the complexes [CuC1(L1)3] • CH2C12 (1), [AuCKL1),] (2), [CuI(L1)(PPh3)]2 (3) and [Cu2ICuIICl4(L2)2]" (4). Their structures have been determined by single crystal X-ray crystallography. 1 and 2 are monomeric, with Cu(I) tetrahedrally four-coordinate and Au(I) two-coordinate with an S-Au-S angle of 158.2(1)°. 3 is dimeric with a central CuI2Cu core, the Cu— Cu distance of which [314.9(1) pm] is rather large. The mixed valence complex 4 has a chain structure with the identity period CuI1(a-Cl)2CuI(a-S)2CuI(a-Cl)2. Cu1 is in a tetrahedral, Cu11 in a square planar environment. The (m-S)2 bridged Cu1---Cu1 distance is only 259.1(1) pm. The structures of the CuX2Cu cores of 3 and 4 are mainly determined by steric interactions of the donor atoms within the coordination spheres of the metal centers.
	Reference	Z. Naturforsch. 48b, 1227—1233 (1993); eingegangen am 4. Mai 1993
	Published	1993
	Keywords	Crystal Structure, Copper(I) Complexes, Dithiocarbamic Acid Esters, Gold(I) Complexes, Dithiocarbamic Acid Esters
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	Identifier	ZNB-1993-48b-1227
	Volume	48

40	Author	Hermann Irngartingera, Jochen Lichtenthälera, Dieter Fenskeb, Gerhard Baumb	Requires cookie*
	Title	Synthesen und Strukturen von 2,5-Bis(2-arylvinyl)-l,4-benzochinonen und deren photochemisches Verhalten im Kristall Syntheses and Crystal Structures of 2,5-Bis(2-arylvinyl)-l,4-benzoquinones and their Photochemical Reactivity in the Crystalline State
	Reference	Z. Naturforsch. 48b, 1411—1418 (1993); eingegangen am 14. Mai 1993
	Published	1993
	Keywords	2, 5-D istyryl-l, 4-benzoquinones, Synthesis, Crystal Structure, Solid State Photochemistry
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	Identifier	ZNB-1993-48b-1411
	Volume	48

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