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Facet section ZfN Section B:Volume 051 [X]

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41	Author	A. Nne, M. Witte, Wolfgang Jeitschko	Requires cookie*
	Title	Preparation and Crystal Structure of the Isotypic Carbides Ln3.67TC6 (Ln = rare earth elements; T = Mn, Fe, Ru) and Eu3 ,i6NiC6
	Abstract	The 14 carbides Ln367MnC6 (Ln = La-Nd) and Ln367TC6 (Ln = La-Nd, Sm; T = Fe, Ru) were prepared from the elem ental components by arc-melting and subsequent annealing. Eu3 16N iC 6 was obtained from a lithium flux. The crystal structures of these nearly isotypic, hexagonal compounds (P63/m, Z = 2) were determined from single-crystal X-ray data; La3 67. FeC6: a = 878.7(2), c = 535.1(1) pm, R = 0.052 for 548 structure factors and 25 variable parameters; Eu316NiC6: a -860.0(1), c = 548.2(2) pm, R = 0.015 for 606 structure factors and 25 variables. The structures differ from the previously reported Gd3Mn2C6 structure by the occupancy of one manganese position by rare earth atoms. Since the lanthanum atoms are larger than the manganese atoms, only two thirds o f these manganese positions can be occupied by the lanthanum atoms in La3 67FeC6. Eu316NiC6 has similar atomic positions. The C-C bond distances in the C2 pairs are 130(2) and 126.5(5) pm in the La and Eu compounds, respectively. Magnetic susceptibility measurements with a SQ U ID m agnetom eter indicate La3 67FeC6 to be Pauli paramagnetic. A test for superconductivity was negative down to 3 K.
	Reference	Z. Naturforsch. 51b, 249 (1996); received June 12 1995
	Published	1996
	Keywords	Lithium Flux, Crystal Structure, Ternary Carbides with C2 Pairs
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	Volume	51

42	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

43	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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	Volume	51

44	Author	G. Jochem, A. Schmidpeter, H. Nöth	Requires cookie*
	Title	Bis(triphenylphosphoniumyIidyl)phosphane Bis(triphenylphosphoniumylidyl)phosphanes
	Abstract	Bis(ylidyl)phosphanes can be prepared from ylides and dichlorophosphanes or from bis-(ylidyl)phosphenium chlorides and organolithium compounds. By substituting in bis(ylidyl)-phosphenium chlorides the chloride ion for more basic anions, a large variety o f bis(ylidyl)-phosphanes is accessible. They can be protonated at the ylidic carbon atoms, but alkylated and oxidized at the central phosphorus atom. A s shown by 3IP NM R in solution and by X-ray investigation of the crystal, the lone pair at the tervalent phosphorus is generally oriented synperiplanar to both phosphonio groups.
	Reference	Z. Naturforsch. 51b, 267—2 (1996); eingegangen am 10. Juli 1995
	Published	1996
	Keywords	Ylides, Transylidation, Phosphenium Ions, M ichaelis Arbusov Rearrangement, Diphosphanes
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	Volume	51

45	Author	Rolf Minkwitz, Ulrike Lohmann, Hans Preut	Requires cookie*
	Title	Primäre und sekundäre Ethyl-und /-Propylsulfoniumsalze sowie Kristallstruktur von /-C3H7SH2+SbF6 [1] Prim ary and Secondary Ethyl and /-Propyl Sulfonium Salts and Crystal Structure of /-C3H 7SH2+SbF6-[1]
	Abstract	The synthesis of salts of the type R"SH3_"+MF6~ (R = C2H 5, i-C3H 7; n = 1, 2; M = As, Sb) by protonation of the corresponding thiols and sulfides in the superacid systems HF/M F5 is reported. The salts have been characterized by vibrational and NM R spectroscopic methods. Isopropylsulfonium hexafluoroantimonate is the first known example of a sulfonium salt, for which a SH bond distance has been determined by a crystal structure analysis, i-C3H 7SH 2+SbF6" crystallizes in the monoclinic space group P2i/m with a = 568.0(4), b = 801.1(6), c = 1019.7(8) pm, ß = 82.63(6) °, with two formula units per unit cell.
	Reference	Z. Naturforsch. 51b, 277 (1996); eingegangen am 6. Juli 1995
	Published	1996
	Keywords	Primary and Secondary Sulfonium Salts, Vibrational Spectra, NM R Spectra, Crystal Structure
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	Volume	51

46	Author	G. Erhard, Koßmehl* Bettina Labahn	Requires cookie*
	Title	Liquid Crystalline Compounds in the Thiophene Series, Part 12+ Synthesis and Characterization of Side Chain Polysiloxanes with Low Transition Temperatures
	Abstract	Polysiloxanes as side chain polymers containing the 2.2'-bithiophene unit, hexyl and octyl terminal groups and spacer units with 3, 5. 6 and 10 m ethylene groups were prepared and characterized. These polymers have monotropic liquid crystalline phases with transition tem peratures below 0 °C (e. g. for polymer 6p: isotropic — * ■ liquid crystalline transition: -20 °C; liquid crystalline — * ■ solid transition: -43 °C). Polymers with a trimethylene spacer group must contain an octyl terminal group for forming liquid crystalline phase; a hexyl group does not form such a phase.
	Reference	Z. Naturforsch. 51b, 286—2 (1996); received July 7 1995
	Published	1996
	Keywords	Liquid Crystalline Thiophene Compounds, Liquid Crystalline Polysiloxanes, Bithiophene Derivatives, Liquid Crystalline Side Chain Polymers
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	Identifier	ZNB-1996-51b-0286
	Volume	51

47	Author	Kuhn3, Thomas Kratz3, G. Erald, H. Enkelb	Requires cookie*
	Title	N orbert
	Abstract	The carbene adduct 5 is formed from the 2-tel-luroimidazoline 4 and iodine. The X-ray structure analysis reveals a dimeric structure in the solid state.
	Reference	Z. Naturforsch. 51b, 295 (1996); eingegangen am 21. Juli 1995
	Published	1996
	Keywords	Tellurium, Carbene, Iodine Reaction, X-Ray
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	Volume	51

48	Author	TabI. Kristalldaten, Frank Weller, Hans-Joachim Mai, Kurt Dehnicke	Requires cookie*
	Title	D ie Kristallstruktur von [M n(C H 3C N )6][M n I4]
	Abstract	und Angaben zur Kristallstruktur-bestimmung von [M n(CH3C N)6][MnI4], Crystal Structure of [M n(CH3CN)6][MnI4] M anganese(II) Complex, Crystal Structure, IR Spectra [M n(CH3C N)6][MnI4] crystallizes from aceto-nitrile solutions of M nl2 as yellow single crystals which were characterized by their IR spectrum and by a crystal-structure analysis. Space group P2Jn, Z -4, structure solution with 3742 observed unique reflections with F0 >5cr(F0), R = 0.050. Lattice dim ensions at 20°C: a = 1258.0(5), b = 1244.7(2), c = 1753.3(6) pm, ß = 92.22(3)°. The compound forms octahedral cations [M n(CH3C N)6]2+ with site symmetry Q with average Mn-N bond lengths of 222.3 pm and te trahedral anions [M nl4]2' without symmetry with average bond lengths M nl of 271.3 pm.
	Reference	Z. Naturforsch. 51b, 298 (1996); eingegangen am 13. Juli 1995
	Published	1996
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	Volume	51

49	Author	Yoshimitsu Yamazaki, MidoriG. Oto1, ^. Yu-Ichi, Takenori Kageyama, Hiroaki Tomohiro, Okuno	Requires cookie*
	Title	Structure of Chloro(cyclopentadienone)- (cyclopentadienyl)ruthenium and its Cytotoxic Activity
	Abstract	The structure of R u(cpO)(cp)C l com plex (3), which was precipitated from aqueous solutions of R u(cp)2Cl+PF6' (1), was determined by X-ray crystallographic analysis. The Ru-halogen bond distance was shorter and the dihedral angle be tween the rings was larger than the values re ported for the corresponding Br analogue, R u(cpO)(cp)Br (4). The com plex 3 (IC50 1 09 /iM) was more cytotoxic than 1 (IC50 163 //M) against mouse sarcoma S I80 cells, but less toxic than 4 (IC50 72 ,/M).
	Reference	Z. Naturforsch. 51b, 301 (1996); received September 21 1995
	Published	1996
	Keywords	Ruthenium Complex, Cytotoxicity, X-Ray, Cyclic Voltammetry
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	Identifier	ZNB-1996-51b-0301_n
	Volume	51

50	Author	AnneU. Tzolino, K. Arsten Bluhm	Requires cookie*
	Title	Synthese und röntgenographische Charakterisierung von zwei neuen Verbindungen des Ludwigit-Strukturtyps: Co5Sn(B0 3)2 0 4 und Co5Mn(B0 3 )20 4
	Abstract	Synthesis and X -R ay C haracterization o f Two New Com pounds with Ludw igite-Structure: C o5S n (B 0 3)20 4 and C o5M n (B 0 3)20 4 The compounds Co5Sn(B 03)20 4 (I) and Co5M n(B03)20 4 (II) were prepared by using a B20 3 flux technique. Single crystals were investigated by X-ray diffraction and showed orthorhombic symmetry, space group D2h-Pbam (No. 55), I a = 944.4; b = 1233.8; c = 310.5 pm; Z = 2 and II a = 925.07; b = 1241.67; c = 305.24 pm; Z = 2. Both compounds are isotypic to the mineral Ludwigite. All metal point positions show an octahedral oxygen coordination. Co2+ and M4+ (M = Sn or Mn) occupy one point position statistically. Both structures contain isolated, trigonal planar B 0 3 units and oxygen atoms that are not coordinated to boron.
	Reference	Z. Naturforsch. 51b, 305—308 (1996); eingegangen am 28. September 1995
	Published	1996
	Keywords	Cobalt, Tin, Manganese, Borate Oxide, Crystal Structure
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	Identifier	ZNB-1996-51b-0305
	Volume	51

51	Author	Silke Busche, K. Arsten Bluhm	Requires cookie*
	Title	Synthese und Kristallstruktur von Dibariumzink-bis(cyclotriborat) Ba2Zn(B30 6)2
	Abstract	Single crystals of the new compound Ba2Zn(B30 6)2 were obtained by using a B20 3 flux technique. They crystallize in an as yet unknown structure type. X-ray investigations led to space group Cj'-Pl (Nr.2) with lattice parameters a = 715.5(2), b = 720.5(2), c = 1178.9(4), a = 78.96(2)°, /3 = 85.45(2)°, j = 60.12(1)°, Z = 2. The structure is characterized by iso lated (B30 6)3_-rings and contains two ninefold coordinated Ba-sites. Zn2+ is tetrahedrally coordinated by oxygen. The relation to the crystal structures of high-temperature BaB20 4 and Ba2Ca(B30 6)2 is discussed.
	Reference	Z. Naturforsch. 51b, 309—312 (1996); eingegangen am 26. September 1995
	Published	1996
	Keywords	Barium, Zinc, Borate, Crystal Structure
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	Volume	51

52	Author	Park, K. Arsten Bluhm	Requires cookie*
	Title	Pb6(A s0 4)
	Abstract	[B (A s04)4] -ein neuartiger Kristallstrukturtyp im System Pb0 /B2 0 3 /As2 0 5 mit einem Beitrag über P b(B A s05) Pb6(A s 0 4)[B (A s 0 4)4] -a New Crystal Structure Type in the System P b 0 /B 20 3/A s20 3 w ith R em arks about P b (B A s0 5) C heong- Single crystals of Pb6(A s04)[B(As04)4] (I) and Pb(BAs05) (II) were obtained by melting B->03, As20 5 and PbO at 800 °C. X-ray investigation led to the space group (I): S4 -P4 (Nr. 81) with a = 715.4(1), c = 976.2(3) pm, Z = 1 and (II): C \| -P3, (Nr. 144) with a = 712.2(1), c = 693.5(2) pm, Z = 3. While (II) is isotypic to the Stillwellite structure, Pb^(As04)[B(As04)4] represents a completely novel type of crystal structure. Boron and arsenic are tetrahedrally coordinated by oxygen. These polyhedra form two kinds of isolated anions: A s04'~ and B(A s04)49_. Lead is eightfold coordinated by oxygen.
	Reference	Z. Naturforsch. 51b, 313—318 (1996); eingegangen am 16. Oktober 1995
	Published	1996
	Keywords	Lead, Arsenic, Borate, Synthesis, Crystal Structure
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	Identifier	ZNB-1996-51b-0313
	Volume	51

53	Author	Silke Busche, K. Arsten Bluhm	Requires cookie*
	Title	Ba2KZn3(B306)(B60 13)
	Abstract	Single crystals of the new compound Ba2KZn3(B30 6)(B60 \| 3) were obtained by using a B20 3 flux technique; they crystallize in an as yet unknown structure type. X-ray investigations led to the space group C '-P l (Nr.2) with lattice parameters a = 705.2(2), b = 712.5(2), c = 1880.3(6), a = 93.43(3)°, ß = 90.72(2)°, 7 = 119.57(2)°, Z = 2. The structure contains (B30 6)3~-rings and a new discrete (B60 13)8~ anion, which is composed of two B 0 4 and two B20 5 units. Zn-+ is tetrahedrally coordinated by oxygen and two out of three tenfold coordinated Ba-sites are statistically occupied by Ba2+ and K+.
	Reference	Z. Naturforsch. 51b, 319—324 (1996); eingegangen am 26. September 1995
	Published	1996
	Keywords	Barium, Potassium, Zinc, Borate, Crystal Structure
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	Identifier	ZNB-1996-51b-0319
	Volume	51

54	Author	H. Einer, Homborg	Requires cookie*
	Title	Inin -Phthalocyanine: Darstellung, Eigenschaften und Kristallstruktur von £-Bis(triphenylphosphin)iminium-as-di(cyanato(N))phthalocyaninato- (2-)indat(III)
	Abstract	In111 Phthalocyanines: Synthesis, Properties and Crystal Structure of Z?-Bis(triphenylphosphine)iminium c/5-D i(cyanato(N))phthalocyaninato(2-)indate(III) B arbara Aßm ann, A ndreas Franken, [In(Cl)Pc2~] reacts with bis(triphenylphosphine)iminium cyanate ((PNP)OCN) in dichlo-romethane to yield green-blue *(PNP) [In(NCO)2Pc2_] • CH2C12, which crystallizes in the triclinic space group Pi (No. 2) with Z = 2. The two cyanato(N) ligands are in a mutually cis coordination (Z (NNCO-In -N NCO) = 84.2(3)°). The In atom is displaced out of the plane of the four N,.vo atoms towards the two cyanato(N) ligands (d(In-Ct(N,JO)4) = 0.988 A). The average In-N NC0 and In-N,.so bond distances are 2.16(1) and 2.216(8) A, respectively. The NNco-In -NNCO moiety deviates by ~ 4° from the staggered conformation relative to the In-(N,,")4 sceleton. Though the cyanato(N) ligands are essentially linear, there are different In-N -C angles (164.4(9) and 147.1(8)°) probably due to crystal packing effects. The Pc2~ ligand is distorted in an asymmetrically convex manner. The PNP cation adopts the bent conformation (Z(P-N(K)-P) = 143.5(6)°). The cyclic voltammogram shows three electrode processes, which are assigned to the redox pairs: Pc ~/Pc2~ (-0.87 V) < In'/In111 (-0.63 V) < Pc~_ /Pc~ (0.69 V). The UV-VIS-NIR spectra and the vibrational spectra are discussed.
	Reference	Z. Naturforsch. 51b, 325—332 (1996); eingegangen am 21. August 1995
	Published	1996
	Keywords	Indium(III) Phthalocyanines, Cyanato(N) Complex, Cyclic Voltammetry, Crystal Structure, Optical and Vibrational Spectra
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	Identifier	ZNB-1996-51b-0325
	Volume	51

55	Author	D. Frerichs, C. H. Park, HkM. Üller-B, Uschbaum	Requires cookie*
	Title	Zur Kenntnis zweier Formen des Zinkorthoarsenates: a-Z n 3(A s04)2 und /3-Zn3(A s0 4)2 On Two Forms o f Zinc O rthoarsenate: a -Z n 3(A s 0 4)2 and /3-Zn3(A s 0 4)2
	Abstract	Single crystals of two forms of zinc orthoarsenate (a-Z n3(A s04)2 (I) and /3-Zn3(A s04)2 (II)) have been prepared by flux techniques. Both compounds crystallize monoclinically, space groups (I): Cih-P2l/c, (II): Cih-P21/n, with the lattice parameters (I): a = 6.306(2), b = 8.652(2), c = 'ol 1.321(4) A, ß = 92.25(5) °, Z = 4 and (II): a = 5.281(1), b = 8.494(2), c = 7.726(3) A, ß = 96.39(3)°, Z = 2. ct-Zn3(A s04)2 is isotypic to I-Cu3(A s04)2 and ß-Zn3(A s04)2 to 7-Zn3(P 0 4)2. Similarities and differences of the crystal structures are discussed.
	Reference	Z. Naturforsch. 51b, 333—337 (1996); eingegangen am 31. August 1995
	Published	1996
	Keywords	Zinc, Arsenic, Oxide, Crystal Structure
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	Identifier	ZNB-1996-51b-0333
	Volume	51

56	Author	O. Sfreddo, Ch Rabbow, HkM. Üller-B, Uschbaum	Requires cookie*
	Title	Eine neue Verbindung im System Ba/Ln/Zn/Pt/O: Bs^Sn^Zi^PtOis On a New Com pound in the System B a/Ln/Zn/Pt/O : Ba4Sm 4Z n3P tO \|5
	Abstract	Reactions of mixtures of B aC 03, ZnO, Sm20 3 (3:5: 1) heated in platinum crucibles up to 1250 °C led to big black single crystals of Ba4Sm4Zn3P t0 15. The new compound crystallizes with hexagonal symmetry, space group C^-Pö^mc, a = 1 L657, c = 6,789 A , Z = 2. It is isotypic with Ba6Nd2Al4O l5 but shows an ordered Pt4+ and Zn2+ distribution over the aluminium positions. The octahedrally coordinated barium sites of the Ba6Nd2Al40 15 type are occupied by Sm3+. In comparison to compounds of the composition Ba6Ln2M40 15 (M = Al, Fe, Co), Ba4Sm4Zn3PtOi5 is the first example containing different oxidation states at the M '+ positions.
	Reference	Z. Naturforsch. 51b, 338—342 (1996); eingegangen am 22. August 1995
	Published	1996
	Keywords	Barium Rare Earth, Zinc, Platinum, Oxide, Crystal Structure
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	Volume	51

57	Author	Ch Rabbow, HkM. Üller-B, Uschbaum	Requires cookie*
	Title	Zur Kenntnis eines Barium-Lanthanoid-Aluminat-Zinkats: BaLuAlZn30 7 mit einem Anhang zu Ba2Er2Zn80 13
	Abstract	Reactions of B aC 03, ZnO, Lu20 3 and A120 3 mixtures at temperatures up to 1500 °C led to small and colourless rods of BaLuAlZn30 7. The new compound crystallizes with hexagonal symmetry, space group CöV -P63mc, a = 6.273, c =10.161 A, Z = 2. In spite of small differences in the oxygen content BaLuAlZn30 7 is isotypic to Ba2Ln2Zn80 13. The crystal structure shows Zn2+ with tetrahedral, Lu '+ with octahedral and Ba:+ with anticuboctahedral coordination by 0 2~. It has been shown that parts of the [Zn3A107]5_ network are fragments of the ZnO structure. In consequence one oxygen atom is fourfold coordinated by zinc/aluminium. The space group of Ba2Ln2ZnxO i3 must be corrected to C6V -P63mc.
	Reference	Z. Naturforsch. 51b, 343—347 (1996); eingegangen am 27. Juli 1995
	Published	1996
	Keywords	Barium, Rare Earth, Zinc, Aluminium, Crystal Structure
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	Identifier	ZNB-1996-51b-0343
	Volume	51

58	Author	Jörg Laue, G. Unther Seitz, H. Ans, W. Aßmuth	Requires cookie*
	Title	Synthese und [4+2
	Abstract	]-Cycloadditionen von 4a, 8a-Methanophthalazin, das erste Propellan mit einem elektronenreichen und einem elektronenarmen 47r-Diensystem Synthesis and [4+2] C ycloaddition Reactions o f 4a, 8a-M ethanophthalazine, the First Propellane w ith an E lectronrich and an Electrondeficient 47r-Diene System Cyclopropabenzene 3 reacts with 3,6-bis(trifluoro)-l,2,4,5-tetrazine 4 to afford in high yield the 4a,8a-methanophthalazine 6, the first propellane, containing an electron rich cyclohexadiene system on the one hand and an electron deficient diazadiene system on the other hand. According to the principle of Diels-Alder reactions with inverse electron demand, electron rich dienophiles like ketene acetals, enamines or dimethyl hydrazones react predominantly with the diazadiene system to yield the azo-bridged cycoadducts of type 19 and/or the tricyclic tetrahydropyridazines like 20. In the same fashion several more or less angle strained cycloalkenes cycloadd to the diazadiene of the propellane 6 to give the novel polycyclic azo compounds 34, 36, 38,40, 42 and 44 with exo-configuration of the annulated cycloalkanes. Attack apparently occurs from less hindered face anti to the methano bridge of 6 with high stereo-and site-selectivity. As anticipated the electron deficient dienophiles 1,2,4-triazoline-3,5-dione 45 and the benzoquinone 46 add with different site selectiviy to 6 furnishing the polycyclic pyridazines 47 and 48 resp. again by exclusive anti attack. Treatment of 6 with both an electron rich and an electron deficient dienophile like 49 and 45 resp. affords the heptacyclic anti-anti-bis adduct 51 with analogously high site-and stereoselectivity.
	Reference	Z. Naturforsch. 51b, 348—358 (1996); eingegangen am 31. August 1995
	Published	1996
	Keywords	Diels-Alder Reactions, Valence Tautomerism, Propellane, Bivalent, 7r-Facial Selectivity, Site Selectivity
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	Volume	51

59	Author	W. Lübbe, W. Preetz	Requires cookie*
	Title	Darstellung, n B-, 13C-, ^ -N M R -und Schwingungsspektren von ji-Pentamethylen-bis
	Abstract	hexahydro-c/oso-hexaborat, [B6H6(CH2)5B6H6]2', und ji-Hexamethylen-bis-hexahydro-c/oso-hexaborat, [B6H6(CH2)6B6H6]2 Preparation, n B, l3C, 'H NMR and Vibrational Spectra of /x-Pentamethylene-bis-hexahydro-c/oso-hexaborate, [B6H6(CH2)5B6H6]2_, and /i-Hexamethylene-bis-hexahydro-c/<m>-hexaborate, [BftH ötC^^BftH ö]2- /i-Pentamethylene-bis-hexahydro-c/o5<7-hexaborate(2-), /u-Hexamethylene-bis-hexahydro-c/cw-hexaborate(2-), '
	Reference	Z. Naturforsch. 51b, 359—362 (1996); eingegangen am 7. September 1995
	Published	1996
	Keywords	H NMR Spectra, l3C NMR Spectra, "B NMR Spectra
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	TEI-XML for	default:Reihe_B/51/ZNB-1996-51b-0359.pdf
	Identifier	ZNB-1996-51b-0359
	Volume	51

60	Author	W. Lübbe, W. Preetz	Requires cookie*
	Title	Darstellung, n B -,13C -,1 H-NMR-und Schwingungsspektren von ja-Dimethylen-bis
	Abstract	hexahydro-c/oso-hexaborat, [B6H6(CH2)2B6H6]2', sowie Kristallstrukturen von [As(C6H5)4]2[B6H6(CH2)2B6H6] [(CH3)2CO] und [P(C6H5)4]2[B6H6(CH2)2B6H6][C 2H5OH] Preparation, " B , 13C, 'H NM R and Vibrational Spectra of /i-Dimethylene-bis-hexahydro-c/oso-hexaborate, [BeHöCCI^hBöHö]2" , and the Crystal Structures o f [As(C6H5)4]t[B 6H6(CH2)2B 6H6] [(CH3)?CO] and [P(C6H5)4]2 [B6H6(CH2)2B6H6] • [C2H5OH] ^-Dimethylene-bis-hexahydro-c/as'o-hexaborate(2- By reaction of [B6H6]2~ with dibromoethane in acetonitrile /j-dimethylene-bis-hexa-hydro-c/oso-hexaborate(2-), JBfiHötCfLbBfcHö]2 -, is formed. The compound was sepa rated from excess [B6H6]'_ by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of [AstCfiH.^MBöHötCHbhBöHftl-IXCI-L^CO] (I) and [P(Cf,H5)4]2[BftH^CHT^BftHf,]■ [C2H5OH] (II) have been determined by single crystal X-ray ana lysis: I is triclinic, space group PI with a = 10.264(2), b = 13.804(2) and c = 20.242(2) A, a = 97.857(10)°, ß = 92.734(11)° and 7 = 103.024(13)°; II is monoclinic, space group P2iIn with a = 12.742(2), b = 7.532(2) and c = 26.887(3) Ä, ß = 95.765(10)°. The 11B NMR spectrum of this compound reveals the feature of monosubstituted octahedral B6 cages. The l3C NMR spectrum exhibits a triplet at 16.20 ppm with '7(C,H) = 120.4 Hz. In the 'H NMR spectrum a singulet at 0.72 ppm of the CH2-groups and two singulets at 1.72 and -4.95 ppm of the BH fragments are observed. The IR and Raman spectra exhibit strong CH stretching bands between 2908 and 2789 cm-1, BH stretching bands between 2463 and 2396 cm-1, and the BC stretching vibration at 1144 in the IR and at 1150 cm" 1 in the Raman spectrum.
	Reference	Z. Naturforsch. 51b, 363—369 (1996); eingegangen am 3. August 1995
	Published	1996
	Keywords	), Crystal Structure, 'H NMR Spectra, Vibrational Spectra, l3C NMR Spectra, "B NMR Spectra
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	Identifier	ZNB-1996-51b-0363
	Volume	51

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