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1994[X]
1Author    Jörn Müller, PetraEscarpa Gaede, Ke QiaoRequires cookie*
 Title    ^-Olefin-Iridium-Komplexe, XXII [1] C -H -Aktivierung von aromatischen und aliphatischen Solvensmolekülen RH bei der Reaktion von [Cp*IrCI2 ] 2 mit Butadienmagnesium unter Bildung von [Cp*Ir(773-C4H 7)R] sowie Kristallstruktur von [Cp*Ir(i/3-C4H 7)C6H 5] jr-Olefin Iridium Complexes, XXII [1] C -H Activation of Aromatic and Aliphatic Solvent Molecules RH in the Reaction of [Cp*IrCl2 ] 2 with Butadienemagnesium with Formation of [Cp*Ir(?;3 -C4 H 7 )R], and Crystal Structure of [Cp*Ir(773 -C4 H 7 )C6 H 5] Activation of C -H , (l-Methylallyl)(pentamethylcyclopentadienyl)iridium-a-organyl Com­ plexes  
 Abstract    Reactions of [Cp*IrCl2]2 (Cp* = ^3-C5M e5) with [MgC4H6 -2 THF]" at low temperature give [Cp*Ir(^4-C4H6)] together with [Cp*Ir(/73-C4H 7)R] compounds, the latter being formed via C -H activation of solvent molecules RH (RH = benzene, toluene, anisole, thiophene, furane, N-methylpyrrole, pentane, cyclohexane. THF). In the case of pyrrole, C -N -activation occurs. The ratio of syn and anti isomers of the 1-methylallyl com plexes as well as the sites o f C -H activation of RH were investigated by NM R spectrometry. An enantiomorphous crystal of [Cp*Ir(773-C4H7)C6Hs] was characterized by X-ray diffraction analysis which reveals trigonal planar coordination at the Ir atom and an exo, syn conformation o f the 1-methylallyl ligand. A mechanism of the reaction which involves 16-electron intermediates is discussed. The corresponding system [Cp*RhCl2]2/butadienemagnesium/RH gives only [Cp*Rh(>/4-C4H6)], and no C -H activation is observed. 
  Reference    Z. Naturforsch. 49b, 1645—1653 (1994) 
  Published    1994 
  Keywords    Synthesis, NMR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1645.pdf 
 Identifier    ZNB-1994-49b-1645 
 Volume    49 
2Author    Z. NaturforschRequires cookie*
 Title    Die isoelektronischen Molekülkomplexe TiCl3(NPPh3) und TiCl3(OSiPh3)  
 Abstract    The Isoelectronic M olecular C om plexes TiC l3(N P P h 3) and T iC l3(O SiPh3) Thilo R übenstahl, D o ro th ea W olff von G udenberg, F ra n k W eller, K u rt D ehnicke* TiCl3(NPPh3) and TiCl3(OSiPh3) have been prepared from titanium tetrachloride and Me3SiNPPh3 and HOSiPh3, respectively. Both complexes were characterized by IR spectrosco­ py and by crystal structure determmations. TiCl3(N PPhj): Space group R3, Z = 6, structure analysis with 959 observed unique reflec­ tions, R = 0.039. Lattice dimensions at -6 8 °C: a = b = 1370.5(7), c = 1845.9(9) pm. TiCl}(OSiPh3): Space group P2,/c, Z = 8, structure analysis with 4549 observed unique re­ flections, R = 0.049. Lattice dimensions at 19 °C: a = 2127.7(2), b = 947.2(1), c = 2136.8(1) pm, ß = 105.081(5)°. Both complexes form monomeric molecules in which the titanium atom is tetrahedrally coordinated by three chlorine atoms, the nitrogen atom of the phosphorone iminato ligand and the oxygen atom of the silyloxy group, respectively. The bond lengths TiN of 171.9(4) pm and TiO of 171.0(3) (in average) correspond to double bonds. 
  Reference    (Z. Naturforsch. 49b, 15—20 [1994]; eingegangen am 7. September 1993) 
  Published    1994 
  Keywords    Monomerie Titanium Complexes, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0015.pdf 
 Identifier    ZNB-1994-49b-0015 
 Volume    49 
3Author    Dieter Sellmann+, Helge Friedrich, Falk Knoch, Matthias MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, C*. Unerwartet einfache Bildung von Diazen-Komplexen und ein neuer Typ von Diastereomerie: [/#-N2H2{Fe(PPr3)('S4')}2] und analoge Komplexe mit [FeS]-Zentren. ( 'S /2-= l,2-Bis(2-mercaptophenylthio)ethan(2-)) Transition Metal Complexes with Sulfur Ligands, C*. Unexpectedly Facile Formation of Diazene Complexes and a New Type of Diastereomerism: [a-N2H2{Fe(PPr3)('S4')}2] and Analogous Complexes with [FeS]-Centers. ('S4'2~ = l,2-Bis(2-mercaptophenylthio)ethane(2-))  
 Abstract    Single pot reactions of FeCl2-4H20 with the tetradentate thioether-thiol 'S4-H 2' = 1,2-bis(2-mercaptophenylthio)ethane, phosphines such as PEt3, PPr3 or PBu3, and a ca. 40-fold excess of N2H4-H20 yield, in the presence of air, diazene complexes of the general formula [M-N2H2{Fe(PR3)('S4')}2]. In contrast to previous syntheses of diazene complexes, the yields can excel 80%, and the syntheses can be carried out on a 10 g scale. [M-N2H2{Fe(PPr3)('S4')}2], 1 and [M-N2H2{Fe(PEt3)('buS4')}2], 2 were characterized by X-ray structure analysis. 2 contains 'buS4'2-= l,2-bis(3,5-ditertiarybutyl-2-mercaptophenylthio)-ethane(2-), which is the tertiary-butyl derivative of 'S4'2-. 1 and 2 contain fram-HN=NH which bridges enantiomeric [Fe(PPr3)('S4')] or [Fe(PEt3)('buS4')] fragments. HN=NH is stabilized by 4c -6 e~-jr bonds, strong tricentric N -H — (S)2 bridges, and steric shielding. NMR studies show that centrosymmetric 1 isomerizes in solution at temperatures around 0 °C in order to give a diastereomerie diazene complex which is also centrosymmetric. The diastereomerism is traced back to bridging the chiral [Fe(PPr3)('S4')] fragments by frara-HN=NH in a differ­ ent way. The two different bridging modes are verified by X-ray structure analyses of analo­ gous ruthenium complexes. Because this new type of diastereomerism is basically caused by a different position only of the N -H — (S)2 bridges, it is termed hydrogen bridge diastereo­ merism. A mechanism for the isomerization is suggested. 1 exhibits three anodic waves in the cyclovoltammogram. The second wave indicates formation of the dication [1]2+, which is a redox isomer of the diprotonated (and as yet hypothetical) dinitrogen complex [a-N2{Fe(PPr3)('S4')}2]. The significance of [1]2+ and of its Lewis basic thiolate donors with respect to electrochemical reduction of molecular dinitrogen under mild conditions is dis­ cussed. 
  Reference    (Z. Naturforsch. 49b, 76—88 [1994]; eingegangen am 9. Juli 1993) 
  Published    1994 
  Keywords    Diazene, Iron Sulfur Complexes, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0076.pdf 
 Identifier    ZNB-1994-49b-0076 
 Volume    49 
4Author    Thom As Schleid, Falk LissnerRequires cookie*
 Title    Oxidsulfidchloride der Lanthanide vom Typ M 4OS4Cl2 (M = L a-N d ) M 4OS4Cl2-Type Oxysulfide Chlorides of the Lanthanides (M = L a -N d )  
 Abstract    Oxysulfide chlorides, M4OS4Cl2, o f the lanthanides (M = L a -N d) are obtained upon the oxi­ dation o f the metals with sulfur in the presence o f MOC1 (or M 20 3) and MC13 in appropriate molar ratios. Additional NaCl or an excess o f MC13 serving as a flux provide even single crys­ talline material after reactions at 850 °C for seven days in sealed tantalum capsules. The crys­ tal structure o f M4OS4Cl2 (hexagonal, P 6 3mc, no. 186, Z = 2; M = La: a = 933.19(3), c = 701.22(4) pm, c/a = 0.7514, R = RH = 0.020; M = Ce: a = 925.49(3), c = 694.13(3) pm, c/a = 0.7500; M = Pr: a = 919.72(4), c = 688.53(4) pm, c/a = 0.7486; M = Nd: a = 914.25(4), c = 683.12(4) pm, c/a = 0.7472, R = 0.022, Rw = 0.019) contains isolated 0 2--centered (M 3+)4 te-trahedra which are surrounded by twelve S2-and six Cl-, capping vertices, edges, and faces o f each tetrahedron and linking to other [OM4] units. Basically, the structure is identical to that o f Ba4OCl6 if Ba2+ is substituted by M 3+ and 2/3 o f the CL anions are replaced by S2-to secure charge neutrality in M4OS4Cl2. Different models for the C L /S 2-replacement are presented on the basis o f comparisons o f the Madelung part o f the lattice energy (M A PLE) with the M APLE sum o f the binaries (M 20 3, M 2S3, and MC13). 
  Reference    Z. Naturforsch. 49b, 340 (1994); eingegangen am 27. September 1993 
  Published    1994 
  Keywords    Lanthanides, Oxysulfide Chlorides, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0340.pdf 
 Identifier    ZNB-1994-49b-0340 
 Volume    49 
5Author    Frank Weller, Fritjof Schmock, Kurt Dehnicke, Kurt Findeisen Bayer-WerkRequires cookie*
 Title    Synthese, IR-Spektrum und Kristallstruktur von 1.3.5-Trichlortriazinium-hexachloroantimonat, [HC3N3C13]SbCl6 Synthesis, IR Spectrum and Crystal Structure of 1.3.5-Trichlortriazinium Hexachloroantim onate, [HC3N3Cl3]SbCl6  
 Abstract    ,3,5-Trichlortriazinium hexachloroantimonate has been prepared by the reaction of CCl2 = N-COCl with antimony pentachloride in boiling dichloromethane. The compound was characterized by IR spectroscopy and by a crystal structure determination. [HC3N3Cl3]SbCl6 crystallizes in the monoclinic space group P 2 Jn with four formula units per unit cell. 2503 observed unique reflections, R = 0.029. Lattice dimensions at 19 °C: a = 1314.1(1), b = 958.2(1), c = 1329.1(1) pm, ß = 117.113(5)°). The compound forms ion pairs via a linear N -H • • • Cl bridge, thus distorting the SbCl6~ ion from octahedral geometry. The C3N3 skeleton of the [HC3N3C13]+ ion is nearly planar, but the hydrogen atom lies about 30 pm out of this plane. 
  Reference    Z. Naturforsch. 49b, 360—364 (1994); eingegangen am 3. November 1993 1.3. 
  Published    1994 
  Keywords    5-Trichlortriazinium Salt, Synthesis, IR Spectra, Crystal Structure 1 
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 Identifier    ZNB-1994-49b-0360 
 Volume    49 
6Author    Andreas Ahle, K. Urt Dehnicke, CäciliaM. Aichle-Mössmer, Joachim SträhleRequires cookie*
 Title    Synthesis and Crystal Structure of [Na( 12-Crown-4)2]2[Fe4Se4Cl4]  
 Abstract    [N a(12-crow n-4)2]2[Fe4Se4Cl4] has been pre­ pared by the reaction o f FeCl2 with N a2Se4 in di-methylform amide solution in the presence o f 12-crown-4 as dark red crystals, which were char­ acterized by a_ crystal structure determination. Space group P 1, Z = 2, 6295 observed unique re­ flections, R = 0.085. Lattice dim ensions at 20 °C: a = 1397.3(3), b = 1501.8(4), c = 1570.1(4) pm, a = 85.86(2)°, ß = 64.06(2)°, y = 65.01(2)°. The structure consists o f [Na(12-crown-4)2]+ cations and cuban-like anions [Fe4Se4Cl4]2" with Fe — Fe contacts o f 282.8(3) pm. 
  Reference    Z. Naturforsch. 49b, 434 (1994); eingegangen am 30. September 1993 
  Published    1994 
  Keywords    Tetranuclear Iron Selenium Cluster Dianion, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0434_n.pdf 
 Identifier    ZNB-1994-49b-0434_n 
 Volume    49 
7Author    Dieter Sellm, Helge Friedrich, Falk KnochRequires cookie*
 Title    Synthese und Struktur von *1,33N2H4 Transition Metal Com plexes with Sulfur Ligands, Cl*. Synthesis and Structure of N 2H 5[Fe(N 2H4)(S2C6H4)2] * 1,33 N 2H 4  
 Abstract    A ttem pts to coordinate N2H4 to [Fe(S2C6H 4)2] fragments lead to N2H 5[Fe(N2H 4)(S2C6H4)2], which crystallizes from M eOH/N2H 4 solutions as the solvate [(N2H 5){Fe(N2H4)(S2C6H4)2} T.33 N2H 4], 1, and has been characterized by X-ray structure analysis. 1 contains three discrete N2H 5+ cations, four N2H4 solvate molecules and three independent [Fe(N2H4)(S2C6H4)2] anions which are connected via an extended network of N -H —N and N -H —S bridges. N2H 5[Fe(N2H 4)(S2C6H4)2] and 1 contain high-spin Fe(III) centers and labile N2H4 ligands. Ubergangsmetallkomplexe mit Schwefelliganden, CI*. 
  Reference    Z. Naturforsch. 49b, 660—664 (1994); eingegangen am 22. Dezember 1993 
  Published    1994 
  Keywords    Iron Sulfur Hydrazine Complexes, Synthesis, X-Ray 
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 Identifier    ZNB-1994-49b-0660 
 Volume    49 
8Author    S. Möhr, Hk Müller-BuschbaumRequires cookie*
 Title    Uber ein gemischtvalentes Oxoniobat mit planaren Polygonen um Niob und Barium: BaNb2+Nb2+0 6 On a Mixed Valent Oxoniobate Containing Planar Polygons A round Niobium and Barium: BaNb2 +N b^+0 6  
 Abstract    Single crystals of B aN b30 6 were prepared by C 0 2-LA SER high temperature technique. The compound crystallizes with trigonal symmetry C fv-R 3 m , a = 11.4333, c -3.4949Ä , Z = 3. The new structure type is characterized by planar N b 0 4 and planar B a 0 6 polygons. The results are discussed with respect to related compounds like Ca0.75 Nb3O6 or N aNb30 6. 
  Reference    Z. Naturforsch. 49b, 915 (1994); eingegangen am 17. Februar 1994 
  Published    1994 
  Keywords    Barium, Niobium, Oxide, Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-0915 
 Volume    49 
9Author    YueQing Zheng, Arnold AdamRequires cookie*
 Title    Ein neues Carbonat mit Baylissit-Struktur: Rb2[M g(C 03)2(H 20 )4] A New Carbonate with Baylissite Structure: Rb2 [Mg(C0 3 )2(H 2 0 )4]  
 Abstract    The new complex carbonate Rb2[M g (C 0 3)2(HoC))4] crystallizes in the Baylissite-tvpe structure with a = 1130,4(3), b = 641,9(1), c = 703,3(2) pm, ß = 99,62(1)°, V EZ = 503,2(2), space group P2l/n (No. 14) and Z = 2. In comparison with the isostructural potassium compound the cell dimensions increase in b-and c-and decrease in ö-direction. This effect depends on the greater coordination number of Rb+ and the rigidity of strong hydrogen bonds. The carbonate anion exhibits significant deviations from D 3h-symmetry (C -O : 127,1(5)-130,2(5) pm, Z_ O -C -O : 117.9(4)-121,1(3)°). 
  Reference    Z. Naturforsch. 49b, 1368—1372 (1994); eingegangen am 25. April 1994 
  Published    1994 
  Keywords    M etal-Carbonato-Complex, Baylissite Type, Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-1368 
 Volume    49 
10Author    M. Arkus Wieber, Stefan Lang, StefanRalph Rohse, Christian Habersack, BurschkaRequires cookie*
 Title    Synthese und Kristallstruktur von Triphenyltelluroniumsulfid Synthesis and Crystal Structure of Triphenyltelluroniumsulfide  
 Abstract    The synthesis of triphenyltelluroniumsulfide (Ph3TeS)4 is described together with a NMR-spectroscopic characterization. The structure of the title compound was determined by single crystal X-ray diffraction. Crystals of triphenyltelluroniumsulfide are triclinic (space group P I) with the cell parameters a = 1178.0(3) pm. b = 1295.8(6) pm. c = 1298.7(4) pm, a = 77.67(3)°, ß = 82.18(2)°, y = 66.00(2)° (V = 1766(1) x 106 pm3) and Z = 2. The compound appears to form a step-like structure of two [Ph3TeS]2 units and crystallizes with two m ole­ cules of CH2C12 per unit cell. 
  Reference    Z. Naturforsch. 49b, 1654—1658 (1994); eingegangen am 5. Mai 1994 
  Published    1994 
  Keywords    Triphenyltelluroniumsulfide, Synthesis, NMR Data, Crystal Structure, Secondary Bonding 
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 Identifier    ZNB-1994-49b-1654 
 Volume    49 
11Author    Z. NaturforschRequires cookie*
 Title    Lanthanoiden-Komplexe, IX [1]  
 Abstract    Reaktivitätsbestimmender Einfluß der Ligandenkonstitution bei Seltenerdamiden: Herstellung und Struktur sterisch überladener Alkoxid-Komplexe L anthanoid Com plexes, IX [1] Reactivity C ontrol o f L an th an o id A m ides through Ligand Effects: Synthesis and S tructures of Sterically C ongested Alkoxy Com plexes W olfgang A. H errm an n * , R ein er A nw ander, Florian C. M unck, W olfgang Scherer, V eronique D u fau d 3, N o rb ert W. H u b e rb, G eorg R. J. A rtus It is shown that the introduction o f sterically demanding ligands in lanthanoid metal com ­ plexes can depend more on the precise composition of the lanthanoid precursor than on the size of the new ligand. Thus, tris(r-butyl)methanol ("tritox-H ") does not react with the amides Ln[N(SiM e3) 2 ] 3 of the "late" (small) lanthanoid metals. However, fast and clean reactions occur with the sterically less demanding derivatives Ln[N(SiHM e2)2]3, with new homoleptic com plexes Ln(tritox)3 (Ln = Y, Nd) being formed with practically all metals o f this group of elements. The molecular and crystal structures of some lanthanoid amides and alkoxides are described. 
  Reference    Z. Naturforsch. 49b, 1789—1797 (1994); eingegangen am 30. März 1994 
  Published    1994 
  Keywords    Lanthanoid Complexes, Alkoxides, Amides, Synthesis, Structure 
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 Identifier    ZNB-1994-49b-1789 
 Volume    49 
12Author    JonesRequires cookie*
 Title    Polysulfonylamine  
 Abstract    , LIV [1] (12-Krone-4)lithiumdimesylamid-Acetonitril (3/2): Ein Kristall mit zwei prinzipiell unterschiedlichen Konformationen des gleichen Coronanden Polysulfonylam ines, L IV [1] (12-Crow n-4)lithium D im esylam ide-A cetonitrile (3/2): A Crystal w ith Two F undam entally D ifferent C onform ations of the Sam e C oronand A rm an d Blaschette*, K arl-H einz N agel, P e te r G. [Li(12-crown-4){N(S02CH3)2}] is obtained from equimolar amounts of lithium dimesyl­ amide and 12-crown-4 in methanol and crystallizes from acetonitrile as a 3/2 solvate. The crystallographic data of the latter at -130 °C are: monoclinic, space group P 2In, a = 1053.4(3), b = 904.3(3), c = 2791.2(8) pm, ß = 95.66(3)°, V = 2.646 nm3, Z = 6, Dx = 1.441 Mgm~3. Apart from CH3CN molecules residing in lattice cavities, the structure consists of two crystallogra-phically independent [Li(12-crown-4){N(S02CH3)2}] ion pairs A and B in the ratio 2:1. In B, the Li and N atoms lie on a crystallographic twofold axis. In both ion pairs, Li is hexa-coordinated by the four crown oxygen atoms O(C) and by one oxygen O(S) from each sul-fonyl group of the anionic ligand. The coordination geometry of Li in A closely resembles that of Cu11 in the known structure of [Cu(12-crown-4)Cl2] and can be pictured as a distorted octahedron, where two cis sites are occupied by the O(S) atoms and the remaining vertices by the four oxygens of the macrocycle, which displays a [4 8] conformation. The lithium atom, the two O(S) and two O(C) atoms are arranged in an approximately square-planar pattern with L i-O (S) 203.6 and 205.1, L i-O (C) 206.9 and 219.1 pm, trans angles of 173.7 and 174.8°, and cis angles in the range 87.1 -93.6°. The angle between the remaining two Li -O(C) bonds with distances 214.7 and 221.5 pm is only 146.5° compared with 180° in an ideal octahedron. In ion pair B, the coronand assumes a [3 3 3 3] conformation close to C4 symmetry, as observ­ ed e. g. in the known structures of [Li(12-crown-4)NCS] with a square-pyramidal 0 4N-co-ordination and [Ca(12-crown-4)(H20) 4]Cl2-4 H zO with a square-antiprismatic 0 8-geometry. The coordination polyhedron in B can be viewed as an incomplete cube in which two verti­ ces related by a face diagonal are unoccupied. Important bond lengths and angles in B are: L i-O (S) 216.8, L i-O (C) 214.0 and 228.7pm; 0 (S) -L i-0 (S) 82.0, 0 (C) -L i-0 (C) 75.7/76.3 for adjacent and 120.4/121.9° for opposite ring oxygens. 
  Reference    (Z. Naturforsch. 49b, 36—42 [1994]; eingegangen am 2. September 1993) 
  Published    1994 
  Keywords    Polysulfonylamines, (12-Crown-4)lithium Dimesylamide, Synthesis, Crystal Structure, Coronand Conformation 
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 Identifier    ZNB-1994-49b-0036 
 Volume    49 
13Author    Meyer Zu Köcker, Andreas Behrendt, K. Urt Dehnicke, Dieter FenskeRequires cookie*
 Title    Phosphaniminato-Cluster des  
 Abstract    Kupfers. Synthese und Kristallstrukturen von ICu6Cl6(NPM e3)4|Cl[Me3SiNPM e3| • CH2C12 und ICu6Cl6(NPM e3)4l[Cu(Me3SiNPM e3)2lCl2 Phosphoraneim inato Clusters o f Copper. Syntheses and Crystal Structures of [Cu6Cl6(N PM e3)4]Cl[Me3SiNPM e3] • C H 2C12 and [Cu6Cl6(NPM e3)4][Cu(Me3SiNPM e3)2]Cl2 R olf The title com pounds have been prepared as black-blue crystals with metallic lustre by the reaction o f CuCl2 and CuCl, respectively, with M e3SiN P M e3 in C H 2C12 suspensions. The com ­ plexes have been characterized by cyclic voltammetry and by crystal structure determinations. [Cu6Cl6(N P M e3)4]Cl[M e3SiN P M e3] • C H 2C12: Space group P 2,2,2,, Z = 4, structure solution with 4407 unique observed reflections, R = 0.057. Lattice dimensions at -7 0 °C: a -1159.3(8), b = 2027.1(14), c = 2063.3(12) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, in which the copper atom s form a regular octahedron. Four planes o f the octahedra are capped by //3-nitrogen atom s o f the (N P M e3)~ groups. Each o f the Cu atom s is connected with a terminal chlorine atom . Another chloride ion serves for charge com pensa­ tion; this ion occupies another Cu3 plane o f the octahedron. W ithout bonding interaction one M e3SiN P M e3 molecule and one C H 2C12 molecule are included in the lattice. [Cu6Cl6(N P M e3)4][Cu(M e3SiN P M e3)2]Cl2: Space group Pna2,, Z = 4, structure solution with 5676 unique observed reflections, R = 0.071. Lattice dimensions at -7 0 °C: a = 3117.2(21), b = 1927.4(11), c = 1002.7(8) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, the com plex ion [Cu(M e3SiN PM e3)2]+, and chloride ions. In the cation [Cu(Me3SiN P M e3)2]+ the copper atom is linearly coordinated by the nitrogen atom s o f the phosphaneimine m olecules. 
  Reference    Z. Naturforsch. 49b, 301—3 (1994); eingegangen am 18. November 1993 
  Published    1994 
  Keywords    Phosphoraneim inato Clusters o f Copper, Synthesis, Cyclic Voltammetry, Crystal Structure 
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 Identifier    ZNB-1994-49b-0301 
 Volume    49 
14Author    Mitra Ghassemzadeh, Kurt Dehnicke, Helmut Goesmann, Dieter FenskeRequires cookie*
 Title    //2-Halogenokomplexe von N-Iodsuccinimid. Die Kristallstrukturen von PPh4[X(N-Iodsuccinimid)2] * CH3CN mit X = Cl, Br, I /^2-Halogeno Complexes of N-Iodosuccinimide. The Crystal Structures of PPh4 [X(N-Iodosuccinimide)2] * CH 3CN with X = Cl, Br, I  
 Abstract    The ,a2-halogeno complexes PPh4[X(N-Iodosuccinimide)2] • CH 3CN with X = Cl. Br, I have been prepared by reactions of N-Iodosuccinimide with the corresponding tetraphenylphos-phonium halides PPh4X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determina­ tions. PPh4[Cl(N-Iodosuccinimide)2] C H 3CN (1): Space group Pna2!, Z = 4, 4461 observed unique reflections, R -0.027. Lattice dimensions at -6 0 °C: a = 1840.5(9), b = 2589(1), c = 728.2(4) pm. 
  Reference    Z. Naturforsch. 49b, 602—608 (1994); eingegangen am 22. Dezember 1993 
  Published    1994 
  Keywords    Halogeno Complexes of N-Iodosuccinimide, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1994-49b-0602 
 Volume    49 
15Author    Blaschette, PeterG. Jones, Karin Linoh, Ilona Lange, M. Artina Näveke, Dagmar Henschel, Axel Chrapkowski, Dietm Ar, SchomburgRequires cookie*
 Title    Arm  
  Reference    Z. Naturforsch. 49b, 999—1011 (1994); eingegangen am 1. Februar 1994 
  Published    1994 
  Keywords    Polysulfonylamines, 18-Crown-6-Dimesylamine (3/2), Synthesis, Crystal Structure, Coronand Conformation 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0999.pdf 
 Identifier    ZNB-1994-49b-0999 
 Volume    49 
16Author    Oliver Seeger, Joachim SträhleRequires cookie*
 Title    BaCeN2, ein Bariumnitridocerat(IV) mit einer Struktur vom awf/-TiP-Typ BaCeN2, a Barium nitridocerate(IV ) with a Structure of the anti-TiP Type  
 Abstract    Reaction of Ba3N 2 with CeN in the stoichiometric ratio 1:3 at 850 °C under an atmosphere of N 2 followed by quenching yields air and moisture sensitive BaCeN 2. The product crystalli­ zes isotypically to /?-R bSc02 with the anti-TiP type structure in the hexagonal space group P 63/mmc with a = 365.06(2), c = 1266.03(3) pm, Z = 2. The structure was determined using X-ray and neutron powder diffraction data. In the structure the Ba2+ cations occupy trigonal prismatic holes with distances B a -N = 288(1) pm while the Ce atoms are in octahedral positions with distances C e -N = 242.4(8) pm. 
  Reference    Z. Naturforsch. 49b, 1169—1174 (1994); eingegangen am 27. April 1994 
  Published    1994 
  Keywords    Bariumnitridocerate(IV), Synthesis, Structure, X-Ray, Neutron Powder Diffraction 
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 Identifier    ZNB-1994-49b-1169 
 Volume    49 
17Author    Stefan Horstmann, Wolfgang SchnickRequires cookie*
 Title    Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumiodid [P(NH2)4]I Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Iodide [P(NH2)4]I  
 Abstract    The title compound has been prepared starting from phosphorothionic triamide SP(N H 2)3 by methylation of the sulfur atom and subsequent ammonolysis reaction in dry acetonitrile and dichloromethane, respectively, both at room temperature. Suitable single crystals are obtained from an acetonitrile solution in a temperature gradient between 70 °C and room temperature. The crystal structure o f [P(N H 2)4]I has been determined by single crystal X-ray methods (P 4!nbm\ a = 842.6(2), c = 486.7(2) pm, Z = 2). In the solid [P(NH2)4]+-and I~-ions are found with significant N -H -I -h y d r o g e n bonding interactions between anions and cations (H —I: 276.4 pm). The P -N -b o n d length in the cation (160.7(2) pm) represents the shortest P -N H 2 bond distance reported to date indicating a significant electrostatic strengthening. The condensation behaviour of [P(N H 2)4]I in solution and in the solid has been investigated. 
  Reference    Z. Naturforsch. 49b, 1381—1386 (1994); eingegangen am 5. Mai 1994 
  Published    1994 
  Keywords    Tetraaminophosphonium Salt, Synthesis, Crystal Structure, Hydrogen Bonding, Condensation Reactions 
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 Identifier    ZNB-1994-49b-1381 
 Volume    49 
18Author    Z. NaturforschRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 114 [1]  
 Abstract    Synthese und Struktur eines ionischen und nichtionischen, cyclischen Carbaphosphazens und eines Cobalt(III)phosphazen-Komplexes C hem istry of Polyfunctional M olecules, 114 [1] Synthesis and Structure of an Ionic and N on Ionic Cyclic C arbaphosphazene and of a C o b alt(III)phosphazene Com plex Jochen E llerm ann3 *, Jörg S u tter3, Falk A. K noch3, M atthias M oll3, W alter B au e rb Reaction of Ph2 P -N -P (P h 2) -N -(Ph2)PCoP(Ph2) -N -P (P h 2) -N -PPh2 (1) in CH2 C12 with benzimidazole yields (CH2 -PPh2 = N -PPh2 = N -PPh2)+C l" ([4]+C L). The salt [4]+BPh4" has been prepared in THF by metathesis of [4]+C l_ with N aBPh4. D eprotonation of the cationic ring in [4]+BPh4_ was accomplished using l,8-diazabicyclo[5.4.01 7 ]undec-7-ene and resulted in the six-membered carbacyclophosphazene CH=PPh2 -N = P P h 2 -N = P P h 2 (6). Treating 1 with 8 -hydroxyquinoline in CH2 C12 yields the octahedral c/s-complex (N 0) 2 CoP(Ph2) -N -P (P h 2) -N -P P h 2 (7) (N O = 8 -oxyquinolinate group). The com ­ pounds [4]+BPh4~, 6 and 7 are characterized by their IR, Raman, 3 1 P{1H) NM R, 1 3 C{1 H} N M R , !H NMR and mass spectra. Crystals suitable for X-ray structure analyses have been obtained for [4]+BPh4_ and_7x0.5 CH2 C12. The colourless plates of [4]+BPh4_ crystallize in the triclinic space group P I, with the lattice constants a = 1172.7(3), b = 1326.2(3), c = 1806.1(6) pm; a = 100.79(2), ß = 103.71(3), y = 108.18(2)°. The black blocks o f 7 x 0 .5 C H 2 C12 crystallize in the monoclinic space group P 2 x!c with the lattice constants a = 1159.0(10), b = 2008.9(10), c = 2034.6(12) pm; ß = 105.86(5)°. 
  Reference    Z. Naturforsch. 49b, 1763—1773 (1994); eingegangen am 25. April 1994 
  Published    1994 
  Keywords    Cyclic Carbaphosphazene Systems, Cobalt Complexes, Syntheses, NM R Spectra, X-Ray 
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 Identifier    ZNB-1994-49b-1763 
 Volume    49 
19Author    Paolo Ghigna, M. Arco, ScaviniRequires cookie*
 Title    Kinetics and Mechanism of Nd2C u04 Synthesis  
 Abstract    The reaction N d20 3 -I-C uO -*■ N d 2C u 0 4 was investigated on the basis of the Wagner-Schmalz-ried theory of diffusion-driven reactions between crystalline solids, with the help of monodimen­ sional chemical diffusion measurements. It was found that the kinetics of the process is governed by C u2+ diffusion, and the chemical diffusion coefficient Z)(Cu2+) in the N d 2C u 0 4 matrix was obtained (9.9 • 10-13, 1.97 • 10-12 and 1.98 • 10" 11 cm 2 s -1 at 1223, 1273 and 1323 K, respectively). The rela­ tively low value of D (C u2+) was interpreted on the basis of the crystal structures of the compound and related materials, which in addition may suggest an alternative rationale for the interpretation of neodymium immobility. 
  Reference    Z. Naturforsch. 49a, 611—616 (1994); received M arch 14 1994 
  Published    1994 
  Keywords    N d 2C u 0 4 superconductor, Synthesis, Reaction mechanism, Kinetics, Chemical diffu­ sion 
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 Identifier    ZNA-1994-49a-0611 
 Volume    49 
20Author    Unsymmetrische Diorganomagnesiumverbindungen, Heiko Viebrock, Dirk Abein, Erwin Weiss+Requires cookie*
 Title    Über Metallalkyl-und -arylverbindungen, 51. Mittig.* On Metal Alkyl and Aryl Compounds, Part 51 Unsymmetrical Diorganomagnesium Compounds. MgRR'(L) and Solvens Separated Ion Pairs with R = Me  
 Abstract    Amine adducts of diorganomagnesium compounds MgR2(L) are soluble in hydrocarbons and therefore valuable synthons for reactions in non-polar solvents. In this way unsymmetri-cally substituted derivatives MgRR'(L) become available by substituting one organic group by a different carbanion via acid-base reactions, according to eq. (1): R2Mg(L) + HR' -> RR'Mg(L) + HR (1) with HR' being stronger CH-acids than HR. Using the amin adducts R2Mg(L) (R = Me, Et) with chelating amines (L = tetramethyl­ ethylenediamine, TMED A, pentamethylethylenetriamine, PMDTA) and the strong CH-acids cyclopentadiene, indene, fluorene and alkynes the following compounds have been synthe­ sized and their structures derived by X-ray analyses: MgMe(?/3-cyclopentadienyl)(tmeda) (1), MgMe(?73-indenyl)(tmeda) (2), MgMe(^1-fluorenyl)(tmeda) (3), [Mg2Me2(pmdta)2]2+[fluo-renyl]2-benzene (4) and [Mg2Et(phenylethynyl)3(tmeda)]2-benzene (5). It is remarkable, that cyclopentadienyl, indenyl, and fluorenyl ligands have a lower hapticity than rj5 to the metal, due to steric repulsion by the other ligands. In 4 the bulky tridentate base PMDTA prevents any direct interaction between the fluorenide anion and magnesium, giving solvens separated ion pairs with the unusual and hitherto rare example of an organomagnesium cation [Mg2Me2(pmdt)2]2+. The 1:3 compound 5 has a more complicated structure, related to that of alkali metal alkynyl magnesates. 
  Reference    (Z. Naturforsch. 49b, 89—99 [1994]; eingegangen am 17. August 1993) 
  Published    1994 
  Keywords    Unsymmetrical Diorganomagnesium Compounds, Synthesis, Crystal Structure, Base Adducts, Chelating Di-and Triamines 
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 Identifier    ZNB-1994-49b-0089 
 Volume    49 
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