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1	Author	Gudrun Stieglitz, Bernhard Neumüller, K. Urt Dehnicke	Requires cookie*
	Title	Synthesen und Kristallstrukturen der Lithiumphosphide { Li(DME)[P(f-Bu)2]} 2 und [Li(DM E)PPh2l00 Syntheses and Crystal Structures of the Lithium Phosphides {Li(DME)[P(/-Bu)2]}2 and [Li(DM E)PPh2]0 0
	Abstract	The title com pounds have been prepared by the reaction o f rc-butyllithium with the corre sponding diorganophosphanes H PR 2 (R = r-Bu, Ph) in D M E solutions. Both compounds were characterized by crystal structure determinations. {Li(DM E)[P(f-Bu)2]}2: Space group P 1, Z = 1, 2027 observed unique reflections, R = 0.055. Lattice dimensions at —80 °C: a = 879.9(3), b = 986.3(1), c = 1064.0(2) pm, a = 70.69(1)°, ß = 70.63(2)°, y -69.89(2)°. The com pound forms centrosymmetric dimers o f symmetry Q with L i-P bond lengths o f 260.0 and 257.3 pm for the Li2P2 four-membered ring. [Li(DM E)PPh2]0C : Space group P 2 ,/«, Z = 4. 3437 observed unique reflections, R = 0.055. Lattice dimensions at -8 0 °C: a = 1034.8(2), b = 812.48(9), c = 1978.4(3) pm, ß = 103.30(2)°. The com pound forms polymeric chains via LiP bridges with L i-P bond lengths o f 256.3 and 254.1 pm.
	Reference	Z. Naturforsch. 48b, 156 (1993); eingegangen am 8. Oktober 1992
	Published	1993
	Keywords	Lithium Phosphides, Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0156.pdf
	Identifier	ZNB-1993-48b-0156
	Volume	48

2	Author	Jorge Blanco, Eduardo Gayoso, JoseManuel Vila, Miguel Gayoso, CäciliaM. Aichle, -. M. Össmer, Joachim Strähle	Requires cookie*
	Title	Synthesis and Structure of Di-I/i-acetato(0,0')-ferrocenylmethyliden- 2,4,6-trimethylaniline(N,C)-palladium(II)l
	Abstract	Di-[//-acetato(0,0')-ferrocenylmethylidene-2,4,6-trimethylaniline(N,C)-palladium(II)],
	Reference	Z. Naturforsch. 48b, 906—910 (1993); received M arch 8 1993
	Published	1993
	Keywords	Cyclometallation, Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0906.pdf
	Identifier	ZNB-1993-48b-0906
	Volume	48

3	Author	Sabine Kühnei, Klaus-Jürgen Range	Requires cookie*
	Title	Darstellung und Kristallstruktur von Rubidiumdicyanoargentat(I), Rb\|Ag(CN)2] * 0,4 H 20 Synthesis and Crystal Structure o f Rubidium Dicyanoargentate(I), Rb[Ag(CN)2] * 0,4 H 20
	Abstract	Rb[A g(C N)2] 0 ,4 H 20 was synthesized by reaction o f silver cyanide with RbOH and liquid
	Reference	Z. Naturforsch. 48b, 133—139 (1993); eingegangen am 3. September 1992
	Published	1993
	Keywords	Rubidium Dicyanoargentate(I), Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0133.pdf
	Identifier	ZNB-1993-48b-0133
	Volume	48

4	Author	Peter Rögner, Ulrike Schießl, Klaus-Jürgen Range	Requires cookie*
	Title	On the Space Group of Cesium Perbromate, CsBrÖ4
	Abstract	The correct space group of cesium perbromate, C sB r04, is 14,/amd and not 14,/a as previously reported. The com pound is isostructural with a-C sR e 0 4, the high-temperature modification of cesium perrhenate. By analogy with C sR e04 and C s I0 4, a phase transform ation to a low-tempera-ture modification is predicted for C sB r04.
	Reference	Z. Naturforsch. 48b, 235—236 (1993); received September 18 1992
	Published	1993
	Keywords	Cesium Perbromate, Space G roup, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0235_n.pdf
	Identifier	ZNB-1993-48b-0235_n
	Volume	48

5	Author	Klaus-Jürgen Range, Alexandra Atzesdorfer	Requires cookie*
	Title	Ein Orthoperrhenat mit flächenverknüpften R e 0 6-0ktaedern: Hochdrucksynthese und Kristallstruktur von K3NaRe20 9 An Orthoperrhenate with Face-Sharing R e 0 6 Octahedra: High-Pressure Synthesis and Crystal Structure of K 3N aR e20 9
	Abstract	The title com pound was prepared by high-pres sure reaction of rhenium metal with technical grade (i.e., N a containing) K O , in a modified Belt-type apparatus (20 kbar, 1Ö00 °C, 60 min, Au capsule). The amber-coloured crystals are very hygroscopic and decompose rapidly when exposed to air. K 3N aR e20 9 crystallizes hexago-nally, space group P 63/mmc, with a = 6.012(1), c = 14.342(14)Ä, c/a = 2.386 and Z = 2. The structure was refined to R = 0.031, R w = 0.023 for 422 independent, absorption-corrected reflections with l> a (I). K 3N aR e20 9 is isostructural with 6 H -B a T i0 3, a perowskite variant, and contains Na and Re in octaedral coordination. Two R e 0 6 octahedra are face-sharing, thus creating a Re20 9 double octahedron with a R e -R e distance of 2.92Ä.
	Reference	Z. Naturforsch. 48b, 237—239 (1993); eingegangen am 30. September 1992
	Published	1993
	Keywords	Tripotassium Sodium D iorthoperrhenate, High-Pressure Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0237_n.pdf
	Identifier	ZNB-1993-48b-0237_n
	Volume	48

6	Author	Christian Robl, M. Ona Frost	Requires cookie*
	Title	Na6[TeMo60 24l ' 22 H20 -A Layered Heteropoly Compound with the Chain-Like Polycation {N a3(H 20 ) n }^/,+
	Abstract	Colourless triclinic single crystals of N a6[TeMo60 24] • 22 H-,0 were grown from aqueous so lution (space group P i, a = 1030.89(9), 6 = 1056.7(1), c = 1106.32(9) pm, a = 90.120(7), ß = 115.220(6), 7 = 105.195(7) , Z = 1, 295 K, 336 param eters, 3181 reflections, Rg = 0.0186). There are three crystallographically independent N a+ cations. Two of them are coordinated octahedrally by water molecules only. The third N a+ cation is bound to five H 20 and one oxy gen atom (0(4)) belonging to the Anderson-Evans type anion [TeMo60 24]6~. The sodium-cen tered coordination octahedra are linked by common edges exclusively formed by water mole cules to yield chain-like polycations {Na-,(H20) ,,} ^ + which are bound by the N a (l) -0 (4) con tact to the anions situated on crystallographic centers o f inversion forming a layer-like arrangement. Further connections "between the polycations and the [TeM o60 24]6" anions are established by hydrogen bonds involving all the oxygen atom s of the anion except 0(4) as al most equivalent proton acceptors regardless of their bonding mode to Te or Mo.
	Reference	Z. Naturforsch. 48b, 404—408 (1993); received November 12 1992
	Published	1993
	Keywords	Hexamolybdotellurate, Layer Structure, Polycations, Crystal Structure Hydrogen Bonding
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	Identifier	ZNB-1993-48b-0404
	Volume	48

7	Author	Emerich Eichhorn, Anton Rieker, Bernd Speiser, Jürgen Sieglen, Joachim Strähle	Requires cookie*
	Title	Electrochemistry of Oxygenation Catalysts, Part 2 + Improved Synthesis, Crystal Structure, and Electrochemical Properties of N,N-Bis(salicylidene)ethylenediaminatocobalt(III) Chloride
	Abstract	N,N'-Bis(salicylidene)ethylenediaminatocobalt(III) hydroxide is treated with chloroform in methanol to yield the corresponding chloride in pure, crystalline form. Results of the crystal structure determination compare well with those in earlier reports of dimeric [Co(salen)Cl]2 units and incorporated CHC13 molecules. Electrochemical experiments in D M F and pyridine show that the chloride fully dissociates in these donor solvents. Thus, the quasireversible one-electron reduction to Co(salen) is observed in cyclic voltammograms.
	Reference	Z. Naturforsch. 48b, 418—424 (1993)
	Published	1993
	Keywords	Oxygenation Catalyst, Cobalt Schiff-Base Complex, Crystal Structure, Electrochemistry
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	Identifier	ZNB-1993-48b-0418
	Volume	48

8	Author	W. Olfgang Hönle	Requires cookie*
	Title	Single-Crystal Structure Refinement of LiZnAs
	Reference	Z. Naturforsch. 48b, 683—6 (1993); received January 18 1993
	Published	1993
	Keywords	Crystal Structure, Filled-up Zinc Blende, Ternary Arsenide
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0683_n.pdf
	Identifier	ZNB-1993-48b-0683_n
	Volume	48

9	Author	Alexander Lichtblau, Hans-Dieter Hausen, Wolfgang Kaim	Requires cookie*
	Title	First Structural Characterization of an Easily Oxidized Derivative o f 1,4-Dihydroquinoxaline
	Abstract	The first crystal structure analysis o f a 1,4-dihydroquinoxaline is described by example o f the l,4-bis(re/-/-butyldimethylsilyl) derivative. In the solid state, this molecule exhibits a non-planar heterocycle with a dihedral angle o f 156.3° along the N -N axis in the boat-shaped 87r electron ring system. The alkyl groups o f the Si(/er/-Bu)M e2 substituents are arranged as to minimize steric repulsion. Despite the reduced n electron conjugation due to non-planarity, the com pound is oxidized reversibly to an EPR detectable radical cation at -0 .5 9 V vs. ferro cene in dichloromethane. However, the second oxidation to the fully aromatic dication is elec-trochemically irreversible. A comparison with previously obtained results illustrates the struc tural flexibility o f the non-aromatic 1,4-dihydro-1,4-diazine ring system which is strongly affected by rather weak non-bonded interactions.
	Reference	Z. Naturforsch. 48b, 713 (1993); eingegangen am 21. Dezember 1992
	Published	1993
	Keywords	Heterocycles, Organosilicon Compounds, Crystal Structure, Cyclic Voltammetry, Conformation
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0713.pdf
	Identifier	ZNB-1993-48b-0713
	Volume	48

10	Author	Adalbert Lossin, Gerd Meyer	Requires cookie*
	Title	CsPr2(CH3COO)7, ein caesiumarmes wasserfreies ternäres Caesium-Praseodym-Acetat CsPr2(C H 3COO)7, a Cesium Poor Anhydrous Ternary Cesium Praseodymium (III) Acetate
	Abstract	Single crystals of CsPr2(CH 3CO O)7 were obtained from an acetic acid solution of Pr(CH 3COO)3-H-,0 and C s ^ O j in a m olar ratio of 4:1 at 120 °C. It crystallizes in the triclinic system', PT (no. 2), Z = 2, a = 1028.1(5), b = 1034.6(5), c = 1199.4(6) pm, a = 84.82(2), ß = 67.07(3), y = 76.01(2)°, Vm = 343.3(3) cm3/mol, R = 0.031, R w = 0.027. The crystal structure contains infinite chains, i[P r2(CH 3COO)6], running along the [1 1 0] direction. The chains are built up by bridging acetate ions coordinated to two crystallographically different P r3+ ions which are both surrounded by 9 oxygen ligands. These chains are linked by "intercalated" Cs(CH3COO) to layers parallel (100). C s+ has contacts to oxygen atoms of neighbouring layers, such that a three-dimensional network is formed.
	Reference	Z. Naturforsch. 48b, 886—892 (1993); eingegangen am 8. M ärz 1993
	Published	1993
	Keywords	Cesium Praseodym Acetate, Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0886.pdf
	Identifier	ZNB-1993-48b-0886
	Volume	48

11	Author	Blaschette Arm, Karl-Heinz Nagel, PeterG. Jones	Requires cookie*
	Title	Polysulfonylamine, XLIV [1] Synthese von \|Na(15-Krone-5)][N(S02CH3)2l und Kristallstruktur bei -9 5 °C Polysulfonylamines, XLIV [1] Synthesis of [Na(15-Crown-5)][N(S02C H 3)2] and Crystal Structure at -9 5 °C
	Abstract	The complex [Na(15-crown-5)][N(S02C H 3)2] crystallizes at -2 5 °C from a methanol solu tion containing equimolar am ounts of N aN (S 0 2C H 3)2 and 15-crown-5. Its crystallographic data at -9 5 °C are: monoclinic, space group P2,/c, a = 852.1(5), b = 2731.9(12), c = 909.2(4) pm, ß = 115.53(4)°, V = 1.910 nm3, Z = 4, D v = 1.445 M gm 3. The structure in the solid state consists of ion pairs. The sodium cation is coordinated to the five oxygen atoms of the crown ether, one oxygen atom o f the anion, and to the nitrogen atom of the anion. The bond distances are N a-O (crow n) 238.7-247.2, Na sodium ion lies 78 pm out of the plane o f the crown the coronand is described.
	Reference	Z. Naturforsch. 48b, 893—897 (1993); eingegangen am 5. Februar 1993
	Published	1993
	Keywords	Polysulfonylamines, (15-Crown-5)sodium Dimesylamide, Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0893.pdf
	Identifier	ZNB-1993-48b-0893
	Volume	48

12	Author	Jürgen Stuhrm, Arnold Adam, Hans-Uwe Schuster	Requires cookie*
	Title	Na8TiAs4, eine neue Zintl-Phase mit idealen isolierten TiAs4-Tetraedern N a8TiAs4, a New Zintl-Com pound with Ideal Isolated TiAs4-Tetrahedra
	Abstract	The new cubic com pound N a8TiAs4, a = 1376.7(1) pm, space group F d3m , is isostructural to N agSnSb4 [1]. The structure is characterized by ideal isolated TiAs4 tetrahedra. The com pound is in agreement with the Zintl concept.
	Reference	Z. Naturforsch. 48b, 898—900 (1993); eingegangen am 4. M ärz 1993
	Published	1993
	Keywords	Crystal Structure, Preparation, Zintl-Com pound
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0898.pdf
	Identifier	ZNB-1993-48b-0898
	Volume	48

13	Author	Shan-Jia Chen, Ulrich Behrens, Rüdiger Mews	Requires cookie*
	Title	Oxothiatriazine (NSCl)"(NS(0)Cl)3_n (n = 1,2)
	Abstract	A modified m ethod for the preparation of (C1SN)2(C1S(0)N) (1) and (C1SN)(C1S(0)N)2 (2) as well as the crystal structures of 1 and 2 are reported.
	Reference	Z. Naturforsch. 48b, 901—905 (1993); eingegangen am 4. M ärz 1993
	Published	1993
	Keywords	Oxothiatriazines, Crystal Structure, Bond Properties, Stabilities
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0901.pdf
	Identifier	ZNB-1993-48b-0901
	Volume	48

14	Author	MichaelW. Iebcke, ClemensC., F. Reyhardt3, Jürgen Felsche3, G. Ünter Engelhardtb	Requires cookie*
	Title	Clathrates with Three-Dimensional Host Structures of Hydrogen-Bonded Pentaborate \|B50 6(0 H )4]~ Ions: Pentaborates with the Cations NMe4+, NEt4+, NPhMe3+ and pipH+ (pipH+ = Piperidinium) [1]
	Abstract	X-ray structure analyses of crystalline [NMe4][B50 6(0 H)4] «H 20 with n ~ 0.25-0.50 (1), [NEt4][B50 6(0 H)4] (2), [NPhM e3][B50 6(0 H)4] (3), and [pipH][B50 6(0 H)4] (4) reveal that these materials are novel clathrates with closely related three-dimensional host structures built up of hydrogen-bonded oligomeric pentaborate [B50 6(0 H)4]~ ions. The organic cations and water molecules (in 1) occupy as guest species large straight channel-like voids of nearly rectangular cross-section. Com pound 1 crystallizes monoclinically with space group P2,/c (Z = 4); the com pounds 2, 3 and 4, which possess the same host-structure topology, crystallize triclinically with space group P i (Z = 2). "B-M AS N M R spectra allow the detection of small angular distortions in the pentaborate anions caused by the specific hydrogen bonding in the host frameworks. U pon heating the com pounds on a therm obalance in a dynamic inert gas atm os phere dehydration occurs at temperatures of 563 K (1), 543 K (2), 558 K (3) and 523 K (4) before degradation of the organic cations starts at tem peratures o f 633 K (1), 623 K (2), 623 K (3) and 613 K (4).
	Reference	Z. Naturforsch. 48b, 978—985 (1993); received February 17 1993
	Published	1993
	Keywords	Pentaborate, Tetraalkylammonium, Piperidinium, Clathrate, Crystal Structure
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	TEI-XML for	default:Reihe_B/48/ZNB-1993-48b-0978.pdf
	Identifier	ZNB-1993-48b-0978
	Volume	48

15	Author	WilliamS. Sheldrick, Thomas Häusler	Requires cookie*
	Title	Synthesis and Structure of the Hexaethylcyclohexaarsoxane Complexes [{M(CO)3}2{cjc/o-(C2H5AsO)6}], M = Cr, Mo, W
	Abstract	The hexaethylcyclohexaarsoxane complexes [{M (CO)3}2{c>'c/o-(C2H 5A sO)6}], M = Cr, M o, W, 2 -4 have been prepared by the reaction o f (C2H 5AsO)n with the respective metal hexacar-bonyl in toluene and characterized by their IR and N M R spectroscopic data. For 2 the m olec ular structure was established by X-ray structural analysis. The 12 atom s o f the A s60 6 ring form a flattened cuboctahedron in which the 6 oxygen atoms lie in the central equatorial plane. Cr(CO)3 groups are coordinated facially by the upper and lower three arsenic atoms. An ap proximately S6 symmetry is displayed by the Cr2A s60 6 core. Average values o f respectively 116.3 and 98.9° are observed for the A s -O -A s and O -A s -O angles in the hexadentate li gand. The E l-M S and 'H N M R data for (C2H 5AsO)" suggest that this alkylcycloarsoxane is present in solution as a mixture o f species including trimers and tetramers so that a metal as sisted ring expansion is required for the formation o f 2 -4 .
	Reference	Z. Naturforsch. 48b, 1069—1074 (1993); received April 5 1993
	Published	1993
	Keywords	Ethylcycloarsoxane, Tricarbonyl Metal Complexes, Crystal Structure
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	Identifier	ZNB-1993-48b-1069
	Volume	48

16	Author	Michael Plate, Peter Hofacker, WernerM. Assa, Birgit Schwarz, Bernhard Neumüller, Kurt Dehnicke	Requires cookie*
	Title	Synthese und Kristallstrukturen der Wolfram(VI)-Alkinkomplexe \|WCl4(P h -C = C -I)(T H F )l und [WCl4( P h -C = C -T e -C 4H9)(THF)\| Synthesis and Crystal Structures o f the Tungsten(VI) Alkyne Complexes [WCl4(P h -C = C -I)(T H F )] and [WCl4( P h -C = C -T e -C 4H 9)(THF)]
	Abstract	[WCl4(P h -C = C -I)(T H F)] has been prepared by the reaction o f mrns-[WCl4(SEt2)2] with P h -C = C -I in TH F solution, whereas [WCl4(P h -C = C -T e -n C 4H 9)(THF)] has been syn thesized by the reaction o f P h -C = C -T e -« C 4H 9 with tungsten hexacloride in the presence o f C2C14 and THF. Both complexes were characterized by IR spectroscopy and by crystal struc ture determinations. [WCl4(P h -C = C -I)(T H F)]: Space group P 2,/c, Z = 4, 2617 observed unique reflections, R = 0.064. Lattice dimensions at -7 0 °C: a = 1518.2(3), b = 714.5(1), c = 1540.0(3) pm, ß = 90.09(3)°. [WCl4(P h -C = C -T e -« C 4H9)(TH F)]. Space group P 1, Z = 2, 3911 observed unique reflec tions, R = 0.067. Lattice dimensions at 20 °C: a = 844.0(3), b = 974.6(4), c = 1002.4(3) pm, a = 76.00(4),/? = 105.14(1), y = 82.03(3)°. Both complexes have molecular structures, in which the tungsten atom s are seven-coordi nate by four chlorine ligands, by the two alkyne carbon atom s, and in trans position to the latter by the oxygen atom o f the T H F molecule. The WC bond lengths are 198 and 200(1) in the telluro complex and 206 and 196(1) pm in the iodine derivative.
	Reference	Z. Naturforsch. 48b, 1105—1111 (1993); eingegangen am 21. April 1993
	Published	1993
	Keywords	Tungsten Alkyne Complexes, Synthesis, IR Spectra, Crystal Structure
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	Identifier	ZNB-1993-48b-1105
	Volume	48

17	Author	Minkwitz, Hans Preut, M. Athias, Seifert, Dirk Lamek	Requires cookie*
	Title	Die Darstellung von Trifluormethylnitrylhexafluorometallaten CF2N (0 )H +MF6~, Trifluormethylhydroxylammoniumhexafluorometallaten CF3N H 2O H +MF6
	Abstract	(M = As, Sb) und Kristallstruktur von CF3NH 2O H +AsF6" Preparation of Trifluoromethylnitryl-Hexafluorometallates C F 3N (0)H + M F 6~, Trifluorom ethylhydroxylamm onium -Hexafluorom etallates C F 3N H 2O H +M F 6_ (M = As, Sb) and Crystal Structure of C F 3N H 2O H +A sF6~ R olf The preparation o f C F 3N (0)H + M F6~ and C F 3N H ,O H +M F 6' (M = As, Sb) and the crystal structure o f C F 3N H 2O H +A sF 6_ are reported. C F 3N (Ö)H +M F 6~ is prepared by protonation o f C F 3N O in the superacid system H F /M F 5 (M = As, Sb). With an excess o f C F 3N O the cation C F 3N H 2O H +M F6" is formed. C F3NH-,OH+A sF 6~ crystallizes in the triclinic space group P 1 with a = 5.071(2), b = 8.297(3), c = 8.882(4)Ä, a = 90.93(4)°, ß = 95.49(4)°, y = 102.96(4)° and Z = 2. It is formed by a redox reaction between C F 3N (0) H + and excess C F 3N O.
	Reference	Z. Naturforsch. 48b, 1241—1247 (1993); eingegangen am 23. April 1993
	Published	1993
	Keywords	Nitryl Salts, Trifluoromethylhydroxylammonium Salts, Preparation, Spectra, Crystal Structure
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	Identifier	ZNB-1993-48b-1241
	Volume	48

18	Author	Herrn Prof, Dr	Requires cookie*
	Title	Zur Struktur des Pentaazadienidions [tol-N =N -N -N =N -tol]
	Abstract	_. Synthese und Kristallstruktur von Cs2(18-Krone-6)(tolN5tol)2 und (NH4)[Cr(NH3)6(H20) 4](tolN5tol)4 T h e S tru c tu re o f th e P e n ta a z a d ie n id e A n io n [ to l-N = N -N -N = N -to l] _. S yn th esis a n d C ry sta l S tru c tu re o f C s2(1 8 -C ro w n -6)(to lN 5to l)2 an d (N H 4)[C r(N H 3)6(H 20) 4] (to lN 5to l)4 S u san n e D ie te ric h , Jo a c h im S träh le* A concentrated solution of CsCl, 18-crown-6, and to l-N = N -N (H)-N = N -to l in aqueous am m onia affords Cs2(18-crown-6)(tolN5tol)2, which crystallizes in the triclinic space group P 1 with a = 852.6(2), b = 1139.4(3), c -1373.9(4) pm, a = 104.17(3),ß = 95.94(2), y = 110.74(2)°, Z = 1. In the structure centrosym m etrical [Cs2(18-crown-6)]2+ moieties are packed with pairs of l,5-bis(tolyl)pentaazadienide anions to built up columns along [100]. The N -N distances N 1 -N 2 = 128 pm and N 4 -N 5 = 129 pm in the pentaazadienide anions indicate localized double bonds, while the distances N 2 -N 3 and N 3 -N 4 of 134 pm can be assigned to single bonds. A m ixture of C r(N H 3)^+ and tolN N N (H)N N tol in concentrated aqueous am monia yields triclinic (N H 4)[C r(N H 3)6(H 20) 4](tolN 5tol)4 crystallizing in the space group P 1 with the lattice param eters a = 1561.1(1), b = 1619.3(3), c = 1703.3(2) pm, a = 107.03(1), ß = 116.81(1), y = 101.75(1)°, Z = 2. The structure contains tolN5toh anions, NH^ cations and [C r(N H 3)6(H 2Ö)4]3+ complexes in which four triangular faces of the Cr(N H 3)6 octahedron are capped by w ater molecules which are linked via hydrogen bonds. Within the pentaazadienide anions which are connected with the [Cr(N H 3)6(H 20) 4]3+ complexes also via hydrogen bonds an indication for localized double bonds N 1=N2 and N 4=N 5 has been obtained.
	Reference	Z. Naturforsch. 48b, 1574—1580 (1993); eingegangen am 26. Juli 1993
	Published	1993
	Keywords	Pentaazadienide A nion, Synthesis, Crystal Structure
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	Identifier	ZNB-1993-48b-1574
	Volume	48

19	Author	H.R G Bender, M. Nieger, E. Niecke	Requires cookie*
	Title	Synthese amino-und silylsubstituierter Triphosphane -Struktur des 1.1.3.3-Tetrakis(di-is0-propylamino)-2-trimethylsilyl-und des 1.1.3.3-T etraphenyl-2-tri-fStf-propylsilyl-triphosphans Synthesis of Amino-and Silyl-Substituted Triphosphines -Structure of 1.1.3.3-Tetrakis(dwso-propylamino)-2-trimethylsilyl-and 1.1.3 .3 -Tetraphenyl-2 -tri-/s0 -propylsilyl-triphosphine
	Abstract	A variety o f triphosphines [(Et2N)2 P]2PR 4 a -h , [('Pr2 N)2P]2PR 5 a -e and [Ph,P]-,PR 9 e -g [R = Cy (a), rBu (b), Mes (c), M e3Si (d), 'BuM e2Si (e), ThexM e2Si (f), 'Pr3Si (g), Äd"(h), H (i)] has been obtained by the reaction o f the dilithiated primary phosphines R PH 2 l a -h with 2 equiv. o f the chlorophosphines (Et2 N)2PCl 2, ('Pr2N)2PCl 3 or Ph2PCl 8 . M ethanolysis o f the trimethylsilyl substituted derivative [('Pr2 N)2 P]2P(SiM e3) 5d yields the hydrogen substituted triphosphine [('Pr2 N)2 P]2PH 5i. The lithiated diphosphine ('Pr2 N)2 P -P (S iM e 3)Li 6 reacts with the chlorophosphine 2 to give the unsymmetrically substituted triphosphine ('Pr2N)2 P -P (S iM e 3)-P (N E t2) 2 7d. The com pounds have been chracterized by their N M R and mass spectra. The structures o f 4d and 9g have been determined by X-ray diffraction, repre senting the first structures o f uncomplexed triphosphines.
	Reference	Z. Naturforsch. 48b, 1742—1752 (1993); eingegangen am 7. Juni 1993
	Published	1993
	Keywords	Triphosphines, Aminotriphosphines, Silyltriphosphines, N M R Spectra, Crystal Structure
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	Identifier	ZNB-1993-48b-1742
	Volume	48

20	Author	Sabine Niemann, Wolfgang Jeitschko	Requires cookie*
	Title	The Crystal Structures of Re2Al, Re4Alu, and ReAl6
	Abstract	of the rhenium aluminides Re4Aln and ReAl6 were obtained by reaction of rhenium with an excess of aluminum. Re4Aln was found to be isotypic with Mn4Alu. The MnAl6 type structure of ReAl6 was confirmed. The crystal structures of both compounds were refined from single-crystal X-ray data. Re4Aln :P l, Z = 1, a = 516.0(1) pm, b = 896.3(2) pm, c = 516.9(1) pm, a = 90.44(1)°, ß = 99.76(1)°, y = 105.17(1)°, V = 0.2271 nm3, R = 0.036 for 2315 structure factors and 74 variable parameters. ReAl6: Cmcm, Z = 4, a -761.0(1) pm, b = 660.5(1) pm, c = 903.4(1) pm, V = 0.4541 nm3, R = 0.013 for 711 F values and 23 variables. In both structures the rhenium atoms have ten aluminum neighbors at distances from 245 to 277 pm. The A l-A l distances cover the whole range from 251 to 362 pm rather continuously. The previously reported compound Re2Al with the tetragonal MoSi2-type struc ture has the lattice constants a = 298.1(1) pm, c = 958.4(4) pm, V = 0.08519 nm3. ReAl6 shows Pauli-paramagnetism.
	Reference	Z. Naturforsch. 48b, 1767—1773 (1993); received June 161993
	Published	1993
	Keywords	Crystal Structure, Magnetic Susceptibility, Rhenium, Aluminum Well-crystallized samples
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	Identifier	ZNB-1993-48b-1767
	Volume	48

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