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21	Author	Peter Kaiser, Wolfgang Jeitschko	Requires cookie*
	Title	Preparation and Crystal Structures of the Ternary Compounds Ag2SiP2 and AuSiP
	Abstract	The title compounds were prepared by solid state reaction of the elemental components. Their crystal structures were determined from single-crystal X-ray diffractometer data. Ag2SiP2: 142d, a = 652.75(5) pm, c = 855.0(1) pm, Z = 4, R = 0.024 for 611 structure factors and 14 variable parameters; AuSiP: R3m, a = 345.9(1) pm, c = 1720.0(3) pm, Z = 3, R = 0.023 (352 F values, 11 variables). The silicon atoms in Ag2SiP2 are tetrahedrally coordinated by phosphorus atoms. The compound might therefore be considered as a phosphidosilicate and its formula can be rationalized as (Ag+l)2Si+4(P_3)2. However, Ag2SiP2 is not a tetrahedral compound since the phosphorus atoms have five near neighbors (3Ag + 2Si) and the silver atoms are coordinated by three phosphorus atoms in almost trigonal planar coordination. Weak silver-silver bonding is assumed for the shortest Ag-Ag contacts of 318 pm. In AuSiP the gold atoms are in a linear coordination of one silicon (235.5 pm) and one phosphorus atom (232.6 pm). The silicon and phosphorus atoms are tetrahedrally coordinated (3Si + 1 Au and 3P + 1 Au, respectively). Thus, the elements can be assigned oxidation numbers according to the formula Au+lSi+2P-3 . This structure was also refined in the centrosymmetric space group R3m, but in this improper setting the silicon and phosphorus atoms occupy one crystallographic site with random occupancy.
	Reference	Z. Naturforsch. 52b, 462 (1997); received September 13 1996
	Published	1997
	Keywords	Crystal Structure, Two-Electron Bonds, Zintl Compounds
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0462.pdf
	Identifier	ZNB-1997-52b-0462
	Volume	52

22	Author	Teodor Silviu Balabana ', NinaG. Furmanovab	Requires cookie*
	Title	7T-7T Interactions between Pyrylium and Phenyl Rings in the Crystal
	Abstract	The crystal structures of two isomeric phenyl-substituted pyrylium perchlorates, 2,6-di-methyl-4-phenylpyrylium (1) and 2,4-dim ethyl-6-phenylpyrylium (2), have been determined. Both cations are planar in the crystal so that the electron deficient pyrylium rings can interact strongly with the phenyl rings of adjacent molecules forming stacks along the shortest crys-tallographic axis. The phenyl rings may act as donors in a charge transfer interaction which is more pronounced in 1 than in 2. Charge transfer appears as a non-mandatory consequence of the 7T-7T stacking. The structures demonstrate the electrostatic nature of these interactions conforming to the model of Hunter and Sanders [ 1 ].
	Reference	Z. Naturforsch. 52b, 485 (1997); received January 13 1997
	Published	1997
	Keywords	Pyrylium Salt, Crystal Engineering, Charge Transfer, Crystal Structure
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0485.pdf
	Identifier	ZNB-1997-52b-0485
	Volume	52

23	Author	Stefan Horstmann, Wolfgang Schnick	Requires cookie*
	Title	Synthese, Kristallstruktur und Eigenschaften von 1,1,3,3,3-Pentaamino- l-th io -l A \3 A 5-diphosphaz-2-en (NH2)2P(S)N=P(NH2)3 Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaam ino-l-thio-l A5,3A5-diphosphaz-2-ene (N H 2)2P(S)N =P(NH 2)3
	Abstract	(NH2)2P(S)N=P(NH2)3 has been prepared by a two step synthesis. Suitable single crystals were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. The crystal structure of (NH->)tP(S)N=P(NH->)3 has been determined by single cry stal X-ray methods (P2,/c, a = 9 9 8 .2 7 (9)> '= 762.78(8), c = 1007.70(15) pm, ß = 107.340(7)°, Z = 4). In the crystal structure each hydrogen atom is subject to a hydrogen bond. Four N-H -N hydrogen bonding interactions per molecule build up a framework connecting two molecules in eight-membered rings. Each sulfur atom shows six distances N -H -S in the range of weak hydrogen bonding interactions.
	Reference	Z. Naturforsch. 52b, 490—95 (1997); eingegangen am 18. Dezember 1996
	Published	1997
	Keywords	Aminophosphazenes, Synthesis, Crystal Structure, Hydrogen Bonding
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0490.pdf
	Identifier	ZNB-1997-52b-0490
	Volume	52

24	Author	M. Enders, R. Rudolph, H. Pritzkow	Requires cookie*
	Title	Synthese und Kristallstruktur von Pentakis(dimethylsulfoxid)- oxo-titan(IV)chlorid Synthesis and Crystal Structure o f Pentakis(dimethylsulfoxide)-oxo-titanium(IV) Chloride
	Abstract	Pentakis(dimethylsulfoxide)-oxo-titanium(IV) chloride is obtained by reaction of titanium tetrachloride with a stoichiometric amount of water in dimethylsulfoxide. A single crystal structure determination (P i, a = 9.564(6), b = 10.504(7), c = 12.510(8) A. a = 70.21(5), ß = 83.48(5), 7 = 89.82(5)°, V = 1174 Ä 3, Z = 2) shows a dicationic titanium(IV) complex with five dimethylsulfoxide ligands and one oxygen atom. The two chlorine anions are not bonded to the complex cation. The T i0 6-fragment is a distorted octahedron, where five of the six oxygen atoms belong to the coordinated dimethylsulfoxide molecules.
	Reference	Z. Naturforsch. 52b, 496—499 (1997); eingegangen am 23. Dezember 1996
	Published	1997
	Keywords	Titanium Oxo Complexes, Dimethylsulfoxide, Crystal Structure
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0496.pdf
	Identifier	ZNB-1997-52b-0496
	Volume	52

25	Author	Ch Rabbow, S. Panzer, H.K M Üller-, Busch-Baum	Requires cookie*
	Title	Röntgenstrukturanalyse von zwei Verbindungen des
	Abstract	Kupfertyps BaMLn20 5 (M = Zn, Ln = Sm, Tm) und von BaSmAIZn30 7 X -R ay A nalysis of Two C om pounds of the C o p p er Type B aM L n20 5 (M = Z n, Ln = Sm, Tm) and of B aS m A lZ n 30 7 The barium zinc lanthanoide oxides BaZnSm20 5 (I) and BaZnTm20 5 (II) crystallize in the BaCuLn20 3 copper type with orthorhom bic symmetry, space group D^-Pnma, (I): a = 12.575(2), b = 5.804(1), c = 7.198(1) A and (II): a = 12.258(2), b = 5.684(1), c = 7.010(2) A, Z = 4. Zinc shows square pyramidal oxygen coordina tion, but the strong elongation of the C u 0 5 pyra mid in the copper type is missing. BaSmAlZn30 7 crystallizes in the space group C6V -P63mc, a = 6.346(1), c = 10.237(3) Ä, Z = 2. The metal coordi nation of oxygen and the shifts of the ratio Al : Zn at the sites (6c) and (2a) depending on the size of the lanthanoid ions are discussed.
	Reference	Z. Naturforsch. 52b, 546—548 (1997); eingegangen am 30. Dezember 1996
	Published	1997
	Keywords	Barium, Rare Earth, Zinc, Aluminium, Oxide, Crystal Structure
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0546_n.pdf
	Identifier	ZNB-1997-52b-0546_n
	Volume	52

26	Author	S. Meyer, Hk Müller-Buschbaum	Requires cookie*
	Title	Kantenverknüpfte V 0 6-0ktaeder und P 0 4-Tetraeder in BaC a(V 0)(P04)2 Edge-Connected V 0 6 Octahedra and P 0 4 Tetrahedra in BaCa(V0)(P04)2
	Abstract	Single crystals of the new compound BaCa(V0)(P04)2 have been prepared by solid state reactions below the melting point of the reactants in evacuated quartz tubes. X-ray investigations led to monoclinic symmetry, space group C2h-P2 i/c, a = 7.300(1), b = 7.053(1), c = 14.460(1) A, ß = 101,43(1)°, Z = 4. The crystal structure is characterized by layers of corner-and edge-connected P 0 4 tetrahedra and VO,+5 octahedra. There is an unusually short 0 (1)-0(4) distance in a V 0 6 octahedron of 2.44 A associated with the sharing of edges with P 0 4 tetrahedra. The short V-0 distance of 1.61 A indicates a vanadyl group.
	Reference	Z. Naturforsch. 52b, 549—552 (1997); eingegangen am 25. Februar 1997
	Published	1997
	Keywords	Barium, Zinc, Vanadium Phosphate, Crystal Structure
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0549.pdf
	Identifier	ZNB-1997-52b-0549
	Volume	52

27	Author	Tristram Chivers, Masood Parvez, Peter Zoricak	Requires cookie*
	Title	Preparation and X-Ray Structure of 4-BrC6H4CNSC(Cl)N
	Abstract	The title compound was obtained in 82% yield by the intramolecular cyclization of 4-BrC6H4C(NSCCl3)[N(SiMe3)2] in CH2CI2 at 23°C. It crystallizes in the triclinic system, space group PI, a = 7.957(3) Ä, b = 10.864(5) A, c = 5.625(1) A, a = 95.94(3)°, ß = 97.79(2)°, 7 = 100.72(3)°, V = 469.2(3) A3, and Z -2. The bond lengths of the planar C2N2S ring indicate partial 7r-delocalization.
	Reference	Z. Naturforsch. 52b, 557—559 (1997); received September 5 1996
	Published	1997
	Keywords	Crystal Structure, 1, 2, 4-Thiadiazole, Intramolecular Cyclization
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	Identifier	ZNB-1997-52b-0557
	Volume	52

28	Author	Heiner Hückstädt, Heiner Homborg	Requires cookie*
	Title	Synthese von Bis[pyridin-phthalocyaninato(l,5-)iridium(II)]iodid und Pyridin-iodo-phthalocyaninato(2-)iridium(III)-Pyridin durch schrittweise Oxydation von Bis[pyridin-phthalocyaninato(2-)iridium(II)]
	Abstract	Synthesis of Bis[pyridine-phthalocyaninato(l,5-)iridium(II)] Iodide and Pyridine-iodo-phthalocyaninato(2-)iridium(III)-Pyridine by Successive Oxidation of Bis[pyridine-phthalocyaninato(2-)iridium(II)] Successive oxidation of bis[pyridine-phthalocyaninato(2-)iridium(II)] with iodine first yields mixed-valent bis[pyridine-phthalocyaninato(l,5-)iridium(II)] iodide ([(Ir(py)pc1 5'}2]I) and then pyridine-iodo-phthalocyaninato(2-)iridium(III)-pyridine ([Ir(py)(I)pc2_]-py). The latter crystallizes monoclinically with the following cell parameters: a = 10.258(1) A. b = 17.589(3) Ä, c = 19.723(2) Ä, ß = 92.95(1)°, space group P2j/n, Z = 4. Irm is in the centre of a slightly distorted pc2 ligand and coordinates pyridine and iodide in a fra/zs-arrangement. The average Ir-Niso distance is 1.995(5) A (Niso: isoindole N atom), the Ir-Npy and Ir-I distan ces are 2.102(5) and 2.657(1) A, respectively. By a similar oxidation of [{Rh(py)pc2 }2] only [Rh(py)(I)pc2~ ] py is obtained. Solid state spectral properties with diagnostic absorption bands at 1360. 1456, 5620 and 19800 cm-1 confirm the mixed-valent diphthalocyaninate(1.5-).
	Reference	Z. Naturforsch. 52b, 728—734 (1997); eingegangen am 18. März 1997
	Published	1997
	Keywords	Phthalocyaninates, Iridium Compounds, Rhodium Compounds, Crystal Structure
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0728.pdf
	Identifier	ZNB-1997-52b-0728
	Volume	52

29	Author	Hans Hartl, Michael Hoyer	Requires cookie*
	Title	Synthese und Strukturuntersuchungen von Iodocupraten(I), X V III. Darstellung und Kristallstruktur von PbCu2I4 * 2C H 3CN [1] Synthesis and Structure Investigations of Iodocuprates(I), X V III. Preparation and Crystal Structure of PbCu2I4 * 2C H 3CN [1]
	Abstract	Single crystals of PbCu2I4-2(CH3CN) are formed by reaction of Pbl2 with Cul in ace-tonitril. The compound crystallizes in the mono clinic space group C2/m; a = 1625.8(3), b = 436.6(1), c = 1025.8(2)pm; ß = 94.77(3)°; V = 725.7 pm3 TO6; Z = 2. The crystal structure is built up by chains of trans-edge sharing ^[PbI6/3] octahe-dra and corner sharing ^[CuI-y^CH^CN)] tetra hedra connected by common I-I edges.
	Reference	Z. Naturforsch. 52b, 766—768 (1997); eingegangen am 14. März 1997
	Published	1997
	Keywords	Iodometallates, Lead-Copper-Iodide, Synthesis, Crystal Structure
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0766_n.pdf
	Identifier	ZNB-1997-52b-0766_n
	Volume	52

30	Author	R. Rettich, Hk Müller-Buschbaum	Requires cookie*
	Title	Ein [Ba(Ca,Mn)06]-Gerüst mit eingelagerten V-O-V-Gruppen in der Kristallstruktur von Ba(Ca0,6Mn0,4)V20 7 A [Ba(Ca,Mn)06] Framework with Incorporated V-O-V Groups in the Crystal Structure of Ba(CaQ 6Mn0 4)V20
	Abstract	Single crystals of Ba(Ca<).6Mn0 4)V20 7 have been prepared by crystallization from melts. X-ray investigations revealed a new quaternary vanadium oxide of the type BaMV20 7. The M positions are occupied statistically by Ca2+ and Mn2+. The compound crystallizes wi\|h orthorhombic symmetry, space group D^-Pnma, a = 15.429(2), b -5.7005(12), c = 7.364(2) A, Z = 4. The crystal structure can be interpreted as a [Ba(Ca,Mn)06] network with incorporated V-O-V groups. Considering the nearest O2-neighbours of the incorporated vanadium, the V-O-V groups are complemented to give V20 7 divanadate units. Ba(Ca« 6Mn0 4)V20 7 is isotypic to BaMV20 7 (M=Ca,Cd) but not to BaMnV20 7.
	Reference	Z. Naturforsch. 52b, 785—789 (1997); eingegangen am 14. April 1997
	Published	1997
	Keywords	Barium, Calcium, Manganese, Vanadium Oxide, Crystal Structure
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0785.pdf
	Identifier	ZNB-1997-52b-0785
	Volume	52

31	Author	Bernd Schwarze, Wolfgang Milius, Wolfgang Schnick	Requires cookie*
	Title	Synthese und Kristallstruktur von [(CXjSi^N^TiC^ -ein perchloriertes N-Silyl-titanamid Synthesis and Crystal Structure of [(Cl3Si)2N]2TiCl2 -a Fully Chlorinated N-Silyl Titanium Amide
	Abstract	The chlorinated titanium amides [(Cl3Si)2N]2TiCl2 (1) and (Cl3Si)2NTiCl3 have been syn thesized selectively from hexachlorodisilazane lithium and TiCl4. The crystal structure of 1 was determined by single crystal X-ray methods at room temperature (P2\|2j 2 \|, a = 1232.4(2), b = 1265.5(2), c -1469.1(2) pm, Z = 4). The central titanium atom of 1 is bound to two nitrogen atoms and two Cl atoms and is weakly coordinated further by two Cl atoms of the trichlorosilyl groups.
	Reference	Z. Naturforsch. 52b, 819—822 (1997); eingegangen am 1. April 1997
	Published	1997
	Keywords	N-Silyl Titanium Amides, Trichlorosilyl Groups, Crystal Structure, Titanium
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0819.pdf
	Identifier	ZNB-1997-52b-0819
	Volume	52

32	Author	Joachim Pickardt, Sven Wiese	Requires cookie*
	Title	Reaktionen von Azacoronanden mit Quecksilber(II)iodid: Kristallstrukturen zweier Komplexe von Hgl2 mit Diaza-15-krone-5 und Diaza-18-krone-6 Reactions of Azacoronands with M ercury(II) Iodide: Crystal Structures of Two Complexes of H gl2 with Diaza-15-crown-5, and Diaza-18-crown-6
	Abstract	The reactions of diaza-15-crown-5 ("2.1"), and diaza-18-crown-6 ("2.2"), resp., with H gl2
	Reference	Z. Naturforsch. 52b, 847—850 (1997); eingegangen am 7. April 1997
	Published	1997
	Keywords	Crown Complexes, Mercuric Iodide, Crystal Structures
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	Identifier	ZNB-1997-52b-0847
	Volume	52

33	Author	Stephan Strojek, Martin Jansen	Requires cookie*
	Title	Darstellung und Kristallstruktur von P4 0 8 Preparation and Crystal Structure o f P4 Og
	Abstract	P4O x was synthesized for the first time in a pure state. Its crystal structure has been refined using X-ray diffractometer datao (monoclinic, C2/c with a = 970.0(2); b = 1017.9(2); c = 692.3(1) pm; ß = 96.95(2)°; V = 678.5 A3; R ] = 0.033; wR2 = 0.073). Molecular geometry and packing in the solid state are discussed.
	Reference	Z. Naturforsch. 52b, 906—910 (1997); eingegangen am 16. Mai 1997
	Published	1997
	Keywords	Tetraphosphorus Octaoxide, Preparation, Crystal Structure, Molecular Geometry
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0906.pdf
	Identifier	ZNB-1997-52b-0906
	Volume	52

34	Author	Einar Möller, Joachim Sieler, Reinhard Kirmse	Requires cookie*
	Title	Synthese, Struktur-und EPR-Untersuchungen an 57Fe-markiertem Tetra- w-butylammonium-bis(l,l-dicyanoethen-2,2-dithiolato)nitrosyleisen(I), («-Bu4N)2 [57Fe(NO)(/-mnt)2] Synthesis, Structural, and EPR Investigations on 57Fe Enriched Tetra-n-butylammonium- bis(l,l-dicyanoethene-2,2-dithiolato)nitrosyliron(I), («-Bu4N )2[57Fe(NO)(/-mnt)2]
	Abstract	The molecular structure and X-as well as Q-band EPR studies of tetra-«-butylammonium-bis(l,l-dicyanoethene-2,2-dithiolato)nitrosyliron(I) enriched with 57Fe are reported, (n-Bu4N)2[Fe(NO)(/-mnt)2] crystallizes triclinically, space group P i with a = 9,5147(7) A, b = 10,4841(8) A, c = 25,840(2) A, a = 92,510(1)°, ß = 92,895(1)°, 7 = 1 1 1 ,1 5 6 (1)° , Z = 2. The g and the hyperfine coupling tensors AN and AFe derived from the EPR spectra are rhombically-symmetric: g, = 2,043, g~> = 2 039, g3 = 2,031, A ,N = 13 ,8 1 0 ~ 4cm _ l , Ai N = 1 l ,6 1 0 _4cm _lI A3N = 15,2-10_4cm _T, A ,Fe = ll,4 -1 0 ~ 4cm _ l , A2Fe = 1 5 ,7 1 0 '4c m " r and A 3Fe = -2,6-10_4cm _1. The spin-density distribution within the first coordination sphere is discussed.
	Reference	Z. Naturforsch. 52b, 919—926 (1997); eingegangen am 1. April 1997
	Published	1997
	Keywords	Nitrosyliron(I) Complexes, Crystal Structure, EPR Spectra
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	Identifier	ZNB-1997-52b-0919
	Volume	52

35	Author	M. Höhling, W. Preetz	Requires cookie*
	Title	Synthesis and Crystal Structure of Tetraphenylarsonium Pentachlorocarbonylosmate(IV), (Ph4As)[OsCl5(CO)]
	Abstract	The structure of tetraphenylarsonium pentachlorocarbonylosmate(IV), (Ph4As)[OsCl<;(CO)], the first example of a halogenocarbonyl complex with osmium in the oxidation state +IV, has been determined at 208oK by single crystal X-ray diffraction: tetragonal, space group P4/n with a = 12.821 , c = 8.084 A, Z = 2. There are short intermolecular contacts between neighbouring anions along the tetragonal axis c and unusually large displacement ellipsoids of the carbonyl group and the four equatorial Cl ligands arising from a positional disorder of the complex anion. By analogy with a variety of reported structures of the (Ph4As)[RuNCl4] structure type this is attributed to the close packing of the cation sublattice. Compared to other monocarbonylosmates the Os-C bond of 1.94(2) A is extraordinaryly long while the bond between Os and the trans coordinated Cl ligand of 2.286(3) A is rather short.
	Reference	Z. Naturforsch. 52b, 978—980 (1997); received June 2 1997
	Published	1997
	Keywords	Pentachloromonocarbonylosmate(IV), Crystal Structure, Positional Disorder
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	TEI-XML for	default:Reihe_B/52/ZNB-1997-52b-0978.pdf
	Identifier	ZNB-1997-52b-0978
	Volume	52

36	Author	S. Meyer, Hk Müller-Buschbaum	Requires cookie*
	Title	Kurze O-O-Abstände einer gemeinsamen Polyederkante bei Verknüpfung von P 0 4-Tetraedern mit V 0 6-0ktaedern im Vanadyl-Orthophosphat C aN i(V 0)(P04)2 Short 0 -0 Distances in Edge Sharing P 0 4 Tetrahedra and V 0 6 Octahedra o f the Vanadyl- Orthophosphate C a N i(V 0 )(P 0 4)2
	Abstract	Single crystals of the new compound C aN i(V 0)(P 04)2 have been prepared by solid state reactions below the melting point of the oxide mixture in evacuated quartz tubes. X-ray inve stigations ledoto orthorhom bic symmetry, space group D2£-Pnma, a -14.113(1), b -6.408(1), c = 7.364(1) A, Z = 4. The crystal structure shows J. [N i0 4] and J. [V 0 6P20 3] polyhedra chains closely related to analogous chains in the isotypic compound CdV20 (P 0 4)2. The short V -0 distance of 1.66 A indicates a vanadyl group as the main difference to CdV20 (P 0 4)2. The short 0 -0 distance of 2,395 A of the edge-sharing P 0 4 tetrahedra and V 0 6 octahedra is discussed.
	Reference	Z. Naturforsch. 52b, 981—984 (1997); eingegangen am 12. Mai 1997
	Published	1997
	Keywords	Calcium, Nickel, Vanadium Phosphate, Crystal Structure
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	Identifier	ZNB-1997-52b-0981
	Volume	52

37	Author	B. Mertens, Hk Müller-Buschbaum	Requires cookie*
	Title	Uber ein cadmiumreiches Orthovanadat Ba2,5Cd11(V 04)9 mit Cadmium in oktaedrischer und tetragonal pyramidaler Koordination On a Cadmium Rich Orthovanadate Ba-, 3Cd, \|( V 0 4)9 Showing Cadmium in Octahedral and Square Pyramidal Coordination
	Abstract	Single crystals of Ba2 ^C di^V O ^g have been prepared by solid state reactions. The new compound crystallizes with orthorhombic symmetry, space group D ^-Pbcn, a = 20.842(6), b = 13.471(3), c = 11.838(9) A, Z = 4. The crystal structure is characterized and dominated by C d 0 6 octahedra and unusual square pyramids of 0 2~ around Cd2+ forming a three-dimensional [C d ]\|0 36] network. The interstices are occupied by V 5+ and Ba2+ ions. This results in V 0 4 tetrahedra and irregular BaO 10 polyhedra isolated from each other. Occupation of the barium positions is deficient in agreement with the valence state V5+ and calculations of the coulomb terms of lattice energy.
	Reference	Z. Naturforsch. 52b, 989—993 (1997); eingegangen am 26. Mai 1997
	Published	1997
	Keywords	Barium, Cadmium, Vanadium Oxide, Crystal Structure
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	Identifier	ZNB-1997-52b-0989
	Volume	52

38	Author		Requires cookie*
	Title	Synthese und Eigenschaften von fra/zs-Bisnitro-phthalocyaninato(2-)iridat(III) und Pyridin-nitro-phthalocyaninato(2-)iridium(III)
	Abstract	Kristallstruktur von linear-Bis(triphenylphosphin)iminium-fra/is-Bisnitro-phthalocyaninato(2-)iridat(III) S y nthesis a n d P ro p e rtie s o f /raA zs-B isn itro -p h th alo cy a n in ato (2 -)irid a te (III) an d P y rid in e -n itro -p h th a lo c y a n in a to (2 -)irid iu m (III); C ry sta l S tru c tu re o f linear-B is (trip h e n y lp h o sp h in e)im in iu m /ra « 5 -B isn itro -p h th a lo c y a n in a to (2 -)irid a te (III) H e in e r H ü c k stä d t, H e in e r H o m b o rg * Reaction of bis[phthalocyaninato(2-)iridium(II)] ([(Irpc2")2]) with nitric oxide in pyridine yields nitrosyl-containing intermediates that are immediately oxidized by air yielding pyri-dine-nitro-phthalocyaninato(2-)iridium(III) ([Ir(py)(,/V02)pc2 ]). Linear-bis(triphenylphos-phine)iminium frans-bisnitro-phthalocyaninatoiridate(III) (l(PNPy™,,v[Ir(/V02)2pc2"]) is pre pared by air-oxidation of [(Irpc2')2] in dichloromethane in the presence of (P N P)N 0 2. It crystallizes in the triclinic space group P I (no. 2) with the following cell parameters: a -10.649(1) Ä, b = 12.357(1) A, c = 12.841(1) A, a = 75.47(1)°, ß = 67.88(1)°, y = 65.31(1)°, Z = 1. Ir111 is in the centre of a slightly waving pc2~ ligand coordinating two nitro ligands in an eclipsed fram-arrangement. The average Ir-Niso distance is 1.993(2) A (N iso: isoindole N atom), the Ir-N distance is 2.189(3) A (N: nitrite N atom), respectively. The structural data of the nitrite ion are: d(ZV-O) = 1.194(4) and 1.042(5) A, Z(O -N -O) = 131.7(4)°). Spectral properties with diagnostic IR absorption bands at 820, 1331 and 1398 cm -1 confirm the nitro coordination.
	Reference	Z. Naturforsch. 52b, 1003—1010 (1997); eingegangen am 6. Juni 1997
	Published	1997
	Keywords	Phthalocyaninates, Iridium Compounds, Nitro Compounds, Crystal Structure
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	Identifier	ZNB-1997-52b-1003
	Volume	52

39	Author	Ho, Er, Ho Dy, Er, Y. O. Sfreddo, Hk Müller-Buschbaum	Requires cookie*
	Title	Weitere Verbindungen des Bai7Lnj6Zn8Pt4057-Typs mit Ln = Dy More Compounds of the B a17Ln16Zn8Pt40 57 Type with Ln =
	Abstract	Single crystals of B a\|7D y16Zn8Pt40 57 (I), Ba17HO\|6Zn8Pt40 57 (II), BaI7Er16Zn8Pt4057 (III) and Ba17Y 16Zn8Pt40 57 (IV) have been prepared by high temperature reactions using platinum crucibles. X-ray investigations led to tetragonal symmetry, space group C4h -I4/m, (I) -(IV): a = 22.905(1), 22.840(1), 22.795(1), 22.848(1) Ä and c = 5.728(1), 5.722(1), 5.700(1), 5.709(1) A, Z = 2. The crystal structure is characterized by small square, medium-sized quadrangular and large rectangular tunnels, which are filled by oxygen, barium and zinc. The polyhedra network is discussed with respect to the network of compounds of the Ba13D y8Zn4Pt40 37 type.
	Reference	Z. Naturforsch. 52b, 1067—1071 (1997); eingegangen am 6. Mai 1997
	Published	1997
	Keywords	Barium, Rare Earth, Zinc, Platinum, Crystal Structure
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	Identifier	ZNB-1997-52b-1067
	Volume	52

40	Author	Z. Naturforsch	Requires cookie*
	Title	Die unterschiedlichen Strukturen des im Kristall verdrillten 1,4-Bis(tricyanvinyl)- benzols sowie des eingeebneten 1-Tricyanvinylbenzols, Dichtefunktional- Berechnungen und cyclovoltammetrisch sowie ESR/ENDOR-spektroskopisch charakterisiertes Reduktionsverhalten
	Abstract	In te ra c tio n s in M o le cu lar C rystals, 127 [1] T h e D iffe re n t S tru c tu re s in th e C rystal o f T w isted l,4 -B is(tric y a n o v in y l)b e n z e n e as w ell as o f P la n a r 1-T ricyanovinyl-benzene, D e n sity F u n c tio n a l C a lc u la tio n s a n d R e d u c tio n B e h a v io u r S tu d ie d by C y c lo v o ltam m e try a n d E S R /E N D O R S p ec tro sc o p y H a n s B o c k 3, W olfgang S eitz3, N o rb e rt N a g e l3, R ü d ig e r B a u rb, Jan W. B a ts3, Z d e n e k H a v la sc, R o d n e y F. C. C la rid g e d The attem pted crystal growth of l,4-bis(tricyanovinyl)benzene dianion salts, although wi thout success so far, has provided information of general interest. The crystal structures of the related mono and l,4-bis(tricyanovinyl)benzene derivatives differ considerably in their substituent group twisting angles: The two tricyanovinylbenzenes in split-positions exhibit dihedral angles of only 6° or 11°, whereas the two C2(CN)3 groups of the disubstituted benzene are conrotationally twisted by 48° out of the benzene plane. Density functional calculations with 6 -3 1 1 ++G* basis sets, however, predict identical values of 32° for both com pounds and, therefore, their crystal arrangements are discussed in detail for packing-enforced additional interactions. Cyclovoltammetric and ESR /EN D O R -m easurem ents pro vide inform ation on the redox behaviour, a prerequisite for attem pts to crystallize molecular anion salts: The 1,4-disubstituted derivative with a cyclovoltammetrically determ ined half wave reduction potential of +.14 V in aprotic TH F solution proves to be one of the strongest polycyano-substituted ^--acceptors and its radical anion can be selectively generated by T1 metal reduction as confirmed by its ESR/EN D O R spectra. Wechselwirkungen in Molekülkristallen, 127 [1] Ausgangspunkte
	Reference	Z. Naturforsch. 52b, 1125—1138 (1997); eingegangen am 2. Juni 1997
	Published	1997
	Keywords	Tricyanovinyl Benzene Derivatives, Crystal Structure, Density Functional Calculations
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	Identifier	ZNB-1997-52b-1125
	Volume	52

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