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81	Author	M. Itra, G. Hassem Zadeha, JörgM. Agullb, D. Ieter Fenskeb, KurtD. Ehnickea	Requires cookie*
	Title	PPh4[Cl-I-C6H5] und PPh4[Br-I-C6H5] Iodobenzene as Lewis-Acid: Synthesis and Crystal Structures of PPh4[Cl-I-C6H5] and PPh4[Br-I-C6H 5]
	Abstract	The donor-acceptor complexes [X-I-C6H5]~ with X" = Cl-and Br-have been prepared as tetraphenylphosphonium salts from iodobenzene and PPh4X in acetonitrile solutions. They form colourless single crystals, which were characterized by crystal structure determinations. PPh4[Cl-I-C6H5]: Space group P2,/c, Z = 4. Lattice dimensions at -70°C: a = 1301.1(5),
	Reference	Z. Naturforsch. 51b, 1579—1582 (1996); eingegangen am 18. Juni 1996
	Published	1996
	Keywords	Halide Complexes of Iodobenzene, Synthesis, Crystal Structure
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	Identifier	ZNB-1996-51b-1579
	Volume	51

82	Author	M. M. Om, K. D. Ertza, Ehnickea ', J. M. Agullb	Requires cookie*
	Title	A
	Abstract	Colourless single crystals of the title compound are obtained from a saturated solution of NaOSiPh, in toluene in a humid atmosphere. We have characterized [N a ^ O S iP h ^ H iO),] by IR spectroscopy and by a crystal structure determination. Space group R3, Z = 6 , R -0.056. Lattice dimensions at -70°C: a -b = 1540.3 pm, c = 2639.6 pm. The compound has the structure of a Na40 4 heterocubane which is only slighty distorted and in which one of the sodium atoms is not hydrated and shows coordination number three. Die Kristallstruktur von [Na4(0SiPh3)4(H20)3]
	Reference	Z. Naturforsch. 51b, 1583—1586 (1996); eingegangen am 9. Juli 1996
	Published	1996
	Keywords	Sodium Triphenylsilanolate Hydrate, Synthesis, Crystal Structure
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	Identifier	ZNB-1996-51b-1583
	Volume	51

83	Author	Z. Naturforsch	Requires cookie*
	Title	Über ein Blei-Kupfer-Tellurat PbC^TeOy mit Cu2+ in deformiert tetragonal pyramidaler und tetraedrischer Sauerstoffkoordination
	Abstract	On a Lead C opper Tellurate P b C u 3T e 0 7 Containing C u2+ in D istorted Square Pyram idal and Tetrahedral O xygen C oordination B. W edel, Hk. M üller-B uschbaum * PbCu3T e07 has been prepared from the element oxides by solid state reaction in air. Single crystal X-ray work led too orthorhombic symmetry, space group D^-Pnma, a = 10.488(1), b = 6.353(2), c = 8.813(2) A, Z = 4. Cu(1)0 5 square pyramids and Te06 octahedra are members of the anionic part of the crystal structure, Cu(2) atoms show tetrahedral coordination by oxygen. The C u (2)2+ and the Pb2+ cations are incorporated into a [Cu(l)2Te07] network. PbCu,Te07 can thus be viewed as a lead copper oxocuprate(II) tellurate. Calculations of the Coulomb terms of lattice energy reveal two possible positions for the lone pair of electrons at Pb'+.
	Reference	Z. Naturforsch. 51b, 1587—1590 (1996); eingegangen am 21. Mai 1996
	Published	1996
	Keywords	Lead, Copper, Tellurium, Oxide, Crystal Structure
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	Identifier	ZNB-1996-51b-1587
	Volume	51

84	Author	Herrn Prof, K. Dr	Requires cookie*
	Title	Reaktion
	Abstract	von Ph3P=C=PPh3 mit Fe(CO)5; Molekülstrukturen von (CO)4Fe=C=C=PPh3 und Fe3(CO)9(/X3-r72-C=C-PPh3) Reaction o f Ph3P= C =P Ph3 w ith Fe(C O)5; M olecular Structures of (CO)4F e= C =C = P P h3 and Fe3(C O)9(/i3-/72-C = C -P P h 3). W olfgang P e tz * a, Frank W eller5 aGmelin- The ylide Ph3P=C=PPh3 reacts with Fe(CO)5 in toluene to give the metallacumulene (CO)4Fe=C=C=PPh3 (1) and 0=PPh3. A mixture of the ylide with its hydrolysis product Ph2P(0)-CH=PPh3 produces the trinuclear cluster Fe3(CO)9(^ 3-?/2-C=CPPh3) (2) in low yields which can also be obtained from 1 and Fe2(CO)9. Both compounds contain the same ligand bonded in a terminal (1) and in a bridging (2) manner. 1 and 2 crystallize in the monoclinic space groups P2(l)/n and P2(l)/c, respectively, with the unit cell parameters a = 1008.35(10), b= 1167.89(10), c = 1875.10(10) pm, ß = 99.824(10)° for 1 and a = 853.6(2), b = 1966.6(4), c = 1770.2(4) pm; ß = 99.05(3)° for 2. The compounds are further characterized by IR and NMR (l3C , 31P) spectroscopy and elemental analyses.
	Reference	Z. Naturforsch. 51b, 1598—1604 (1996); eingegangen am 7. Juni 1996
	Published	1996
	Keywords	Crystal Structure, Hexaphenylcarbodiphosphorane, Iron Acetylide Complex, Metallacumulene
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	Identifier	ZNB-1996-51b-1598
	Volume	51

85	Author	Z. Naturforsch	Requires cookie*
	Title	On the Structure o f f-B utylam inotriphenylphosphonium Iodine D ichloride
	Abstract	A del A m e ra, A n d rea M ayerb, D ouglas H o c, H ans Z im m erb * The structures of f-butylaminotriphenylphos-phonium iodine dibromide and iodine dichloride were determ ined by Raman spectroscopy and X-ray crystallographic structure analysis. The iodine dibromide [IBr2]~ species was assigned a centro symmetric nature, whereas the iodine dichloride [IC12]" possesses a non-centrosymmetric structure.
	Reference	Z. Naturforsch. 51b, 1663—1665 (1996); received August 30 1995
	Published	1996
	Keywords	/-Butylaminotriphenylphosphonium Iodine D i chloride, Raman Spectra, Crystal Structure
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	Identifier	ZNB-1996-51b-1663_n
	Volume	51

86	Author	P. Eter, G. Jones	Requires cookie*
	Title	P
	Abstract	o ly su lfo n y la m in e, L X X V III [1] l-M e sy l-4 -d im e th y la m in o p y r id in iu m -d im esylam id : D a r ste llu n g und F estkörperstru ktur Polysulfonylam ines, L X X V III [1] l-M esyl-4-dim ethylam inopyridinium D im esylam ide: Synthesis and Solid State Structure A n d reas W irth, A rm an d B laschette Treating (MeSC^X^N with 4-dimethylaminopy-ridine in MeCN afforded the ionic title compound (monoclinic, space group P2j/c). The bond lengths of the 4-dimethylaminopyridinium moiety suggest a semiquinoid resonance form with a dou ble bond to the exocyclic nitrogen and two local ized carbon-carbon double bonds in the ring. The ring and the exocyclic N and S atoms of the cation are essentially coplanar. The S -N bond distances in the cation (173.4 pm) and the anion (159.1 and 159.6 pm) correlate with Pauling bond orders of 1.0 and 1.7, respectively. The anion displays a staggered conformation with approximate C2 symmetry (S -N -S 120.4°).
	Reference	Z. Naturforsch. 51b, 1666—1668 (1996); eingegangen am 20. August 1996
	Published	1996
	Keywords	l-Mesyl-4-dimethylaminopyridinium Dimesylamide, Synthesis, Crystal Structure
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	Identifier	ZNB-1996-51b-1666_n
	Volume	51

87	Author	Klaus Kopka, RainerM. Attes	Requires cookie*
	Title	Ein
	Abstract	zweikerniger Vanadium(V)-Komplex mit (r/1)-und (/x-772:?72)-gebundenen Hydrazido(2-)-Liganden A D inuclear V anadium (V) C om plex w ith (r/1)-and (^ -//2://2)-Bonded H ydrazido(2-) L igands The title complex was obtained by reaction of guanidinium dioxodipicolinatovanadate(V) and N-methyl-N-phenylhydrazine. According to the single crystal structure analysis the dinuclear anion [(/i-PhN NH)(/t-O CH 3){(M ePhN N (dipic)V)}2]~ with sevenfold coordinated metal cen ters contains two types of hydrazido ligands. The ligand [MePhNN]: ~ is terminally bonded, and the VNN unit is linear with extensive electron delocalisation. The V-N and N-N bond lengths are 167.9(5) and 131.9(6) pm, respectively. The bonding of the bridging ligand is of the hitherto unknown fi-rf'.rf type, with V-N and N-N bond lengths of 202.5(5) and 136.5(5) pm, respectively. The V (N 2)V moiety is not planar. The compound was also characterized by H and 1V NMR spectroscopy.
	Reference	Z. Naturforsch. 51b, 1675—1678 (1996); eingegangen am 30. Juli 1996
	Published	1996
	Keywords	Vanadium(V) Compounds, Hydrazido(2-) Complexes, Crystal Structure
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	Identifier	ZNB-1996-51b-1675
	Volume	51

88	Author	Joachim Pickardt, Britta Kühn	Requires cookie*
	Title	M
	Abstract	etallkom plexe m it C yanoguanidin als L iganden: K ristallstru k tu ren von [Cd(cnge)2F2]*3H20 , C d(cnge)2B r2 und Hg(cnge)Cl2 (enge = C yanoguanidin) M etal C om plexes with C yanoguanidine as Ligand: Crystal Structures o f [Cd(cnge)2F2]-3H 20 , C d(cnge)2 Br^ and H g(cnge)C l2 (cnge = Cyanoguanidine) Crystals of [Cd(cnge)2F2]-3H20 (1), Cd(cnge): Br2 (2) and Hg(cnge)Cl2 (3) (cnge = cya noguanidine) were obtained by crystallisation from solutions of CdF2, CdBr2 or HgCl2 and cyanoguanidine in water/ethanol or methanol. 1 crystallizes monoclinically, space group C2, Z = 2,a = 1629.2(4), b = 1056.6(4), c -353.9(1) pm, 3 = 101.05(2)°; 2 is monoclinic, space group P2,/n, Z = 2 , a = 3 9 1.9(I), b = 850.7(2), c = 1722.1(4) pm, ß = 94.06(2)°, 3 is triclinic, space group P I, Z = 1, a = 686.7(1), b = 693.0(5), c = 387.2(4) pm, a = 94.45(5)°, ß = 95.05(4)°, 7 = 78.58(5)°. In 1 and 2 each Cd atom is bonded to four halogen atoms to form polymeric (CdF2)" and (CdBr2)" chains, resp., and to two cyanoguanidine molecules. In 3 each Hg atom is bonded to four chlorine atoms also forming (HgCl2)" chains, which are connected via cyanoguanidine molecules acting as a bidentate bridging ligands to form a network.
	Reference	Z. Naturforsch. 51b, 1701—1706 (1996); eingegangen am 30. Juli 1996
	Published	1996
	Keywords	Cyanoguanidine, Cadmium Halide Complexes, Mercuric Chloride Complex, Crystal Structure
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	Identifier	ZNB-1996-51b-1701
	Volume	51

89	Author	Michael Feist, Sergej Trojanov, Erhard Kemnitz	Requires cookie*
	Title	Die Kristallstrukturen von 1,4-Dimethylpiperazinium-tetrabromo- cobaltat(II) und -zinkat(II), (dmpipzH2) [Mn Br4] (M = Co, Zn)
	Abstract	The Crystal Structures of 1,4-Dimethylpiperazinium Tetrabromocobaltate(II) and -Zincate(II), (dmpipzH2) [MHBr4] (M = Co, Zn) The compounds (dmpipzH2)[MnBr4] (M = Co, Zn) crystallize at room temperature from equi-molar solutions of 1,4-dimethylpiperazine and MBr2 • n H20 in 3M HBr. (dmpipzH2)[CoBr4] is isotypic with the homologous chlorometalates of Co and Zn and crystallizes in the mono clinic space group P2,/m with a = 6.424(3), b = 14.588(6), c = 7.102(6) A, ß = 90.87(6)°, Z = 2. (dmpipzH2)[ZnBr4], however, crystallizes in the monoclinic space group P2,/c with a = 7,605(5), b = 13,760(9), c = 13,286(7) Ä, ß = 93,03(6)°, Z = 4. Both structures con tain centrosymmetric cations (dmpipzH2)2+ in the chair form and slightly distorted tetrahedra [MBr4]2~ with a mirror plane in the case ofM = Co. Several distances N- • -Brin both structures are interpreted in terms of N-H- • Br hydrogen bonds which are favoured by the packing in the case of M = Zn.
	Reference	(Z. Naturforsch. 51b, 9—13 [1996]; eingegangen am 12. Juni 1995)
	Published	1996
	Keywords	1, 4-Dimethylpiperazinium Tetrabromometalates(II), Cobalt, Zinc, Crystal Structure
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	Identifier	ZNB-1996-51b-0009
	Volume	51

90	Author	Martin Köckerling, Gerald Henkel	Requires cookie*
	Title	Nickelkomplexe
	Abstract	mit Thioether-Chelatliganden: Elektrochemische Eigenschaften und Kristallstrukturen von [Ni(MeSCH2CH2SMe)2 (NCS)2], [Ni(EtSCH2CH2SEt)2(NCS)2] und [Ni(MeSCH2CH2SMe)2Br2] Nickel Complexes with Chelating Thioether Ligands: Electrochemical Properties and Crystal Structures of [Ni(MeSCH2CH2SMe)2(NCS)2], [Ni(EtSCH2CH,SEt)2(NCS)2] and [Ni(MeSCH2CH2SMe)2Br2] interest in nickel complexes with sulfur donor ligands as models for the active sites of nickel-containing hydrogenases has prompted us to investigate the structural and elec trochemical behaviour of nickel complexes with bifunctional thioether ligands. Crystals of [Ni(MeSCH,CH,SMe),(NCS),] (1) and [Ni(EtSCH2CH,SEt)2(NCS)2], (2) are triclinic, space group Pi, Z = 1, 1: a = 7.293(3) A, b = 7.567(3) A, c = 8.784(3) A, a = 72.81(3)°, ß = 78.41(3)°, 7 = 85.14(3)°; 2: a = 8.611(1) A, b = 8.101(1) Ä, c = 9.163(1) ßrbÄ, a = 66.54(1)°, ß = 76.19(1)°, 7 = 67.88(1)ßrb°. [Ni(MeSCH2CH2SMe^Br2] (3) crystallizes in the mono clinic space group P2,/n, a = 6.757(2) A, b = 7.881(2) A, c = 14.674(4) Ä, ß = 94.05(2)°, Z = 2. In crystals of 1, 2 and 3 mononuclear neutral complex molecules are observed which have pseudo-octahedral rran5-NiS4L2 coordination sites. The cyclovoltammograms of 1 and 3 in MeCN (Ag/AgCl/KCl, 3 mol/1) show only irreversible oxidation waves at +837 mV for 1 and +846 mV for 3, respectively, which are characteristic features of NCSe and Bre ions. In addition, a reduction wave at +393 mV is observed in 3. No redox response is found in the potential region between -700 and +100 mV which is used by the NiFe hydrogenase enzymes.
	Reference	Z. Naturforsch. 51b, 178—186 (1996); eingegangen am 18. Juli 1995
	Published	1996
	Keywords	Nickel-Sulfur Complexes, Thioether Ligands, Crystal Structure, Electrochemistry, Bioinorganic Chemistry Current
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	Identifier	ZNB-1996-51b-0178
	Volume	51

91	Author	JörgH. Albering, Wolfgang Jeitschko	Requires cookie*
	Title	Quaternary Thorium Transition Metal Pnictide Oxides: ThCu^j-PO, ThCuAsO, and Th2Ni3 _xP3 0
	Abstract	The new compounds T h C u ^ P O and ThCuAsO with ZrCuSiAs-type structure were pre pared in well crystallized form by chemical vapor transport reactions. Th2N i3.A :P30 with a new structure type was obtained by reaction o f T h 0 2 with the other elem ental components in an alumina crucible at high temperatures. The crystal structures of the three compounds were determined from single-crystal X-ray data. ThCuj.xPO: P4/nmm, a = 389.43(4), c -828.3(1) pm, R = 0.024 for 13 variable parameters and 338 structure factors; ThCuAsO: P4/ nmm, a = 396.14(5), c = 844.0(1) pm, R = 0.028 (13 variables and 379 F values); Th2Ni3_JP30 : P4/nmm, a = 394.62(4), c = 1723.2(3) pm, R = 0.018 (27 variables and 374 F values). The refinement of the occupancy parameters revealed significant deviations from the ideal values for the transition metal sites for two compounds resulting in the exact compositions ThCu0938(4)PO and Th2N i2 45(nP30 . Magnetic susceptibility measurements indicate Pauli paramagnetism for T hC u^P O . The crystal structures of these compounds are closely related. They belong to a large family o f tetragonal structures of which the ThCr2Si2-and the PbFCl-type structures are well known examples.
	Reference	Z. Naturforsch. 51b, 257 (1996); received July 6 1995
	Published	1996
	Keywords	Crystal Structure, Quaternary Thorium-Transition Metal-Pnictide Oxides, Chemical Vapor Transport
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	Identifier	ZNB-1996-51b-0257
	Volume	51

92	Author	PaulK. Baker3, DavidJ M Uldoona, MichaelB. Hursthouseb, SimonJ. Colesb, AidanJ. Laveryc, Andrew Shawcrossc	Requires cookie*
	Title	The Crystal Structure and Low Temperature 13C NMR Spectrum of the Seven-Coordinate Complex of Tungsten(II), [WI2(CO)3(NCPh)2]
	Abstract	The crystal structure of [WI2(C O)3(N C Ph)2] (1) has been determined by X-ray methods. The crystals are orthorhombic, space group Pnam, a = 7.815(3), b = 13.839(5), c = 18.475(3) Ä, Z = 8, R -0.0346 for 1497 observed data. The complex [WI2(C O)3(NCPh)2] has a seven-coordinate geometry, which may be described as a distorted capped octahedron, with the two iodo-ligands mutually trans, while each nitrile is trans to a carbonyl group. The capped octahedral geometry consists of a capping carbonyl (C(10)} on the face defined by 1(1), C(20) and C(20)#. However, the geom etry may also be described as a capped trigonal prism, which has one triangular face occupied by three carbonyl groups and the second triangular face occupied by N (l) , N (l)# and 1(1) atoms, respectively. The iodide 1(2) occupies the capping position on the rectangular face defined by the atoms C(20), C(20)#, N (l), and N (l)# . The low temperature 13C NM R spectrum (203 K, C D 2C12) of 1 shows a single carbonyl resonance at 219.27 ppm which indicates that the com plex is undergoing a rapid fluxional process in solution at 203 K.
	Reference	Z. Naturforsch. 51b, 263 (1996); received July 7 1995
	Published	1996
	Keywords	Crystal Structure, Benzonitrile, Carbonyl, D iiodo, Tungsten(II)
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	Identifier	ZNB-1996-51b-0263
	Volume	51

93	Author	DietrichK. Breitinger, Roman Breiter	Requires cookie*
	Title
	Abstract	?ram-(NH4)2[R u (S 0 3)2(N H 3)4]-4 H 20 (1) (m onoclinic, P l x!n\ a = 629.8(3), b = 1000.6(2), c = 1345.7(5) pm, ß = 112.25(4)°, Z = 2; R = 0.021; R w = 0.017) is obtained as pale greenish-yellow crystals by reaction of /ra « s-[R u (S 0 3H)2(N H 3)4] (2) with aqueous ammonia, and crys tallization at +5 °C. The compound, when isolated, is stable at room temperature for only a few days even under inert gas, but persists under the mother liquor. In the centrosymmetric anion frö/?s-[Ru(S03)2(N H 3)4]2~ the bonds Ru-S = 230.5(1) pm are significantly longer than in the neutral complex 2 (227.6(1) pm), whereas the Ru-N bonds are the same in both com plexes within experimental error (averages 214.1 and 214.0 pm). Hence, the mutual trans-influence of the sulfite ligands is weakened on protonation; the bonding of the co-ligands in c/s-position is not affected. The internal structure o f the sulfite ligand in 1 with long S-O bonds (average 151.2(5) pm) and small angles O-S-O (average 106.1(6)°) and the weakened Ru-S bond are a good match. The structure of 1 is held together by a complex network of hydrogen bonds, in which all potential hydrogen-bond donors (O H 2, N H 4+, N H 3) and accep tors (H 20 , S 0 3) are involved. The structural findings are reflected in the vibrational spectra.
	Reference	Z. Naturforsch. 51b, 517 (1996); received August 25 1995
	Published	1996
	Keywords	Ruthenium(II) Sulfito Complex, Crystal Structure, m ws-Influence, Hydrogen Bonding
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	Identifier	ZNB-1996-51b-0517
	Volume	51

94	Author	Thomas Dahlems, Dietrich Mootz, Michaela Schilling	Requires cookie*
	Title	Zweidimensionales Eis und H50 2+-Ionen. Zur Bildung und Struktur tiefschmelzender molekularer und ionischer Hemi-bis Hexahydrate halogenierter Essigsäuren CCl"F3."COOH (n = 1 bis 3) [1] Two-Dimensional Ice and H 50 2+ Ions. On Formation and Structure of Low-Melting Molecular and Ionic Hemi-through Hexahydrates of Haloacetic Acids CCl"F3."COOH (n = 1 to 3) [1]
	Abstract	Hydrate formation o f haloacetic acids CCl"F3_"COOH (n = 1, 2, 3) has been studied by D TA and tem perature-dependent X-ray powder diffraction, and evidence obtained for five phases, all melting at temperatures below ambient. The hydrates have been confirmed and further characterized by their crystal structures at -1 5 0 °C. Three lower hydrates, CC12F C O O H 0.5H -> 0 (space group P2,/c and Z = 8 formula unites per unit cell), CC1F2C 0 0 H H 20 (P2,/c, Z = 4), and CC1F2C 0 0 H -4 H 20 (P I, Z = 2), have molecular structures with the acid and water m olecules hydrogen-bonded in two-dimensional arrays. The structures of the remaining hydrates, CCl2F C O O H -6H 20 and CC13C 0 0 H -6 H 20 (sim i lar, but not isotypic, both P 1 and Z = 2), are ionic, as (H s0 2+)(C X 3C 0 Ö) -4 H 20 , and three-dimensional. The neutral water molecules are hydrogen-bonded in ice-like layers rare in crystal chemistry. A lso, CCl2FCOOH is established only as the second acid o f which a lower hydrate is molecular and a higher one ionic.
	Reference	Z. Naturforsch. 51b, 536 (1996); eingegangen am 16. Oktober 1995
	Published	1996
	Keywords	Crystal Structure, Haloacetic Acid Hydrate, Hydrogen Bonding, Melting Diagram
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	Identifier	ZNB-1996-51b-0536
	Volume	51

95	Author	G. O. Stendorp3, O. Tterb, H. Hom	Requires cookie*
	Title	Syntheses and Properties of Cerium Diphthalocyanines in High Oxidation States; Crystal Structure of [C e(Pc)2](BF4) 0.33
	Abstract	Ring oxidized green Cerium(IV)diphthalocyanines, [Ce(Pc)2]X (X = (poly)halide, N 0 3_) are prepared by chemical oxidation of ("Bu4N)[Ce(Pc2~)2] with the corresponding halogen in solution or of solid [Ce(Pc2_)2] with aqueous HNO> Electrochemical oxidation of ("Bu4N)[Ce(Pc2_)2] in solution in the presence of ("Bu4N)BF4 yields [Ce(Pc)2](BF4)0.;p, which crystallizes in the tetragonal space group P4/nnc (a, b = 19.643(3) A, c = 6.525(3) A, Z = 2). The CeIV ion is eightfold coordinated by the isoindole N atoms (Niso) of the two staggered (ca. 41°), slightly distorted Pc ligands. The "[Ce(Pc)2]<)33+" subunits are arranged in infinite columns along [001] with the Ce atoms statistically disordered over two positions and C e -N iso bond lengths of 2.45(1) and 2.69(1) A, respectively The UV-VIS spectrum is dominated by the transitions of the Pc2-ligand at ca. 15,000 (B band), 30,000 and 36,000 cm -1 (Q, N region). A low energy ("metallic") band at ca. 2800 cm -1 typical for partially oxidized systems is present. The UV-VIS-NIR spectrum of [Ce(Pc)2]N 0 3 indicates a cofacial Pc2" -P c -complex. In addition to the jt-jz' transitions of the Pc2-moiety at ca. 14,000, 30,000 and 36,000 cm-1, the Ch transition of the Pc-ring is observed at ca. 19,200 cm -1 and the typical N IR band at 6380 cm -1. Oxidation of a thin film of (PNP)[Ce(Pc2_)2] with dry Br2/ N2 gas yields purple [Ce(Pc_)2]B rv, whose UV-VIS-NIR spectrum shows the diagnostic fea tures of dimeric Pc~ radicals with intense bands at ca. 14,000 and 18,000 cm -1 assigned as B and Qi bands, respectively. A t ca. 9000 cm 1 the typical Q D absorption is observed. The vibrational spectra are dom inated by the transitions of the Pc-ligand at 1305/1445 cm -1 (IR) and 560/1120/1172/1591 cm-1 (resonance Raman). Excitation with 1064 nm strongly enhances the sym. C e -N stretch at 163 c m '1.
	Reference	Z. Naturforsch. 51b, 567—573 (1996); received September 14 1995
	Published	1996
	Keywords	Diphthalocyanines, Cerium Compounds, Crystal Structure, UV-VIS-NIR Spectra, Vibrational Spectra
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	Identifier	ZNB-1996-51b-0567
	Volume	51

96	Author	D. Bublitz, A. Franken, W. Preetz, H. Thomsen	Requires cookie*
	Title	Darstellung, U B-NMR-Spektren, Schwingungsspektren und Normalkoordi- natenanalyse von cowy'HWcto-Bis-hexahydro-c/oso-hexaborat, [B6H6-B 6H6]2_, sowie Kristallstruktur von [P(C6H5)4 ]2-cöW7 ww^o-[B6H6-B 6H6 ] Preparation, 11B NMR Spectra, Vibrational Spectra and Normal Coordinate Analysis of con ju ncto-B is-h exah ydro-closo-h exaboratQ , [B6H6-B 6H6]2_, and the Crystal Structure of [ P(C6 H5 )4 ] 2 -conjuncto-[B6 H6-B 6 H6 ]
	Abstract	By reaction of [B6H6]2-with dibenzoylperoxide in dichloromethane conjuncto-[B6H6-b 6h 6]2-is formed. The product could be separated from excess [B6H6]2 by ion exchange chro matography on diethylaminoethyl cellulose. The crystal structure of [P(C6H^ ^ -con ju n cto-[B6H6-B 6H6 ] has been determined by single crystal X-ray diffraction analysis; triclinic, space group PI with a = 10.8315(10), b = 11,2422(12), c = 20.340(2) Ä, a = 91.278° (9), ß = 9 0 .\78° (9), 7 = 105.662°(9). The 1 'B NMR spectrum reveals three signals with the intensity ratio 1:1:4, for two equivalent moieties of the conjuncto molecule ion with local C4v symmetry. The IR and Raman spectra of the deprotonated Cs salts of the 1()B, n B and their respective D isotopomers of conjuncto-[B6H5-B6HS]4_ exhibit characteristic shifts. Using averaged crystallographic data and assuming idealized D4h symmetry, normal coordinate analyses have been performed based on a modified valence force field. With a set of eleven force constants (e.g. fd(BB)C 0njU IK.t0 = 2.9, fd(BB)cage = 1.6 mdyn/A) very good agreement between observed and calculated frequencies has been achieved. From strong vibrational coupling with the B6 clusters two vibrations result for the conjuncto B-B bond at 1142/1198 and 292/304cm-1 for 1 'B/I(IB species, respectively. They can be assigned as anti-phase and in-phase motions of the conjuncto B atoms related to the equatorial B4 planes.
	Reference	Z. Naturforsch. 51b, 609—618 (1996); eingegangen am 7. September 1995
	Published	1996
	Keywords	Crystal Structure, n B NMR Spectra, Vibra tional Spectra, Normal Coordinate Analysis
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	Volume	51

97	Author	JosephG. Robe, Duc Le Van, JostW. Innemöller, Bernt Krebs, M. Echtild Läge	Requires cookie*
	Title	Reaktive E=C(p-p)7r-Systeme, XLIII [1] Darstellung und Charakterisierung P-Phosphino-oder P-Arsino-substituierter Fluorphosphaalkene des Typs R2E-P=C(F)NEt2 (R = Me, CF3, Me2N; E = P, As)
	Abstract	Reactive E=C(p-p)-7r System s XLIII [1] Synthesis and Characterization o f P -Phosphino or P-A rsino Substituted Fluoro-phosphaalkenes of the Type R 2E -P=C (F)N Et2 (R = Me, C F 3, M e7N; E = R As) The easily accessible phosphaalkene HP=C(F)NEt2 (lb) reacts with halophosphanes or -arsanes R2EX (X = Cl, I) in the presence of NEt3 to give P-phosphino-or -P-arsino sub stituted fluorophosphaalkenes of the type RiE-P=C(F)NEti (2 -6) in high yields (60 -85 %) [R2E: (CF3)2P (2), Me2N(CF3)P (3), Me2P (4), (CF3)2As (5), M e2As (6)]. The analogous re-action of ib with CF3PI2 (molar ratio 1:2) unexpectedly leads to the triphosphetene Et2N
	Reference	Z. Naturforsch. 51b, 778—784 (1996); eingegangen am 30. November 1995
	Published	1996
	Keywords	Phosphaalkenes, 1, 2, 3-Triphosphetenes, NMR Spectra, Crystal Structure
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	Identifier	ZNB-1996-51b-0778
	Volume	51

98	Author	M. Steiner, A. Artina, Klaus-Jürgen Ndratschke, Range	Requires cookie*
	Title	C laudia
	Abstract	Single crystals of Nd4Au20 9 and Gd4Au20 9 have been prepared by oxidizing mixtures of gold metal and Nd20 3 or Gd20 3, rsp., with K 0 2 under high-pressure high-temperature conditions (40 kbar, 1200°C) in a modified Belt-type apparatus. The X-ray structure analyses have been carried out on twinned crystals. The compounds crystallize in the orthorhombic space group Pbcn (Nd4A u ,0 9: a = 11.938(7) , b = 6.126(2),c = 11.928(3) A ,Z = 4,/?1 = 0.0443; Gd4A u ,0 9: a = 11.922(2), 6 = 6.1242(7), c = 11.917(2) A, Z = 4. R\ =0.0232). The title compounds are isostructural with La4Au20 9. Their structure comprises isolated square-planar A u04 groups, stacked along [010] to form a columnar structure. The Au-Au distance along the columnar direction is 3.10 A. Structural relations to Bi2C u04 und (Nd, Pr)2A u05 are discussed. Hochdrucksynthese und K ristallstruktur von Nd4Au2 C>9 und Gd4Au2 C>9
	Reference	Z. Naturforsch. 51b, 811—816 (1996); eingegangen am 1. Dezember 1995
	Published	1996
	Keywords	Lanthanoide Aurates(III), High-Pressure Synthesis, Crystal Structure, Columnar Stacking
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	Identifier	ZNB-1996-51b-0811
	Volume	51

99	Author	D. Irk Johrendt, R. Einer, M. Iericke, A.Lbrecht Mewis	Requires cookie*
	Title	Neue Pnictide mit modifizierten A1B2-Strukturen New Pnictides with M odified A1B2-Type Structures
	Abstract	Nine new compounds A M X with A: Ca, Sr, Ba, M: Pd, Au and X : P, As were prepared by heating mixtures of the elements and investigated by X-ray methods. They crystallize in modified A1B2-type structures, for the present examples in the ZrBeSi-and SrPtSb-types, with an ordered distri bution of the atoms.
	Reference	Z. Naturforsch. 51b, 905—906 (1996); eingegangen am 6. November 1995
	Published	1996
	Keywords	Ternary Pnictides, Alkaline Earth Metals, Palladium, Gold, Crystal Structure
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	Volume	51

100	Author	Stephan Pitter, EckhardD. Injus, Beate Jung, H. Elm, Ar Görls	Requires cookie*
	Title	Phosphinoalkylnitrile: Synthese und Koordinationsverhalten an Palladiumzentren Phosphinoalkylnitnles: Synthesis and Coordination Behaviour at Palladium C entres
	Abstract	Phosphinoalkylnitriles R2P-(CH2)"-CN {R = isopropyl ('pr), phenyl (ph), cyclohexyl (' hex), n -3, 6, 10} have been prepared starting from the corresponding secondary phosphines in an easy three step synthesis. All new compounds were characterized by their 'H -, i3C and 31P NMR data. Some of these new P, N ligands were used to prepare complexes [{R2P-(CH2)"-CN}2PdCl2] which were also identified by their NMR data. In addition the crystal structures of three derivatives, [{'pr2P-(CH2)3-CN }2PdCl2] 7a, [{ph2P-(CH2)3-CN }2PdCl2) 7b and [{ph2P-(CH 2)6-CN}2PdCl2] 8b were determined by X-ray analysis. The coordination mode of the phosphinoalkylnitriles in these complexes was found to be P-bonded resulting in a trans configuration. Palladium catalysts with 5a as ligand show high activies in the co-oligomerization of butadiene and carbon dioxide. The ^-lactone 11a is formed under very mild conditions.
	Reference	Z. Naturforsch. 51b, 934—946 (1996); eingegangen am 11. Juli 1995
	Published	1996
	Keywords	Phosphinoalkylnitriles, Phosphine Complexes of Palladium, Crystal Structure, Catalysis, -Lactones
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	Identifier	ZNB-1996-51b-0934
	Volume	51

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