| | 1 | Author
| Jörn Müller, PetraEscarpa Gaede, Ke Qiao | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1645.pdf | | | | Identifier
| ZNB-1994-49b-1645 | | | | Volume
| 49 | |
| 2 | Author
| Z. Naturforsch | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0015.pdf | | | | Identifier
| ZNB-1994-49b-0015 | | | | Volume
| 49 | |
| 3 | Author
| Dieter Sellmann+, Helge Friedrich, Falk Knoch, Matthias Moll | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0076.pdf | | | | Identifier
| ZNB-1994-49b-0076 | | | | Volume
| 49 | |
| 4 | Author
| Thom As Schleid, Falk Lissner | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0340.pdf | | | | Identifier
| ZNB-1994-49b-0340 | | | | Volume
| 49 | |
| 5 | Author
| Frank Weller, Fritjof Schmock, Kurt Dehnicke, Kurt Findeisen Bayer-Werk | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0360.pdf | | | | Identifier
| ZNB-1994-49b-0360 | | | | Volume
| 49 | |
| 6 | Author
| Andreas Ahle, K. Urt Dehnicke, CäciliaM. Aichle-Mössmer, Joachim Strähle | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0434_n.pdf | | | | Identifier
| ZNB-1994-49b-0434_n | | | | Volume
| 49 | |
| 7 | Author
| Dieter Sellm, Helge Friedrich, Falk Knoch | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0660.pdf | | | | Identifier
| ZNB-1994-49b-0660 | | | | Volume
| 49 | |
| 9 | Author
| YueQing Zheng, Arnold Adam | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1368.pdf | | | | Identifier
| ZNB-1994-49b-1368 | | | | Volume
| 49 | |
| 10 | Author
| M. Arkus Wieber, Stefan Lang, StefanRalph Rohse, Christian Habersack, Burschka | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1654.pdf | | | | Identifier
| ZNB-1994-49b-1654 | | | | Volume
| 49 | |
| 11 | Author
| Z. Naturforsch | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1789.pdf | | | | Identifier
| ZNB-1994-49b-1789 | | | | Volume
| 49 | |
| 12 | Author
| Jones | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0036.pdf | | | | Identifier
| ZNB-1994-49b-0036 | | | | Volume
| 49 | |
| 13 | Author
| Meyer Zu Köcker, Andreas Behrendt, K. Urt Dehnicke, Dieter Fenske | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0301.pdf | | | | Identifier
| ZNB-1994-49b-0301 | | | | Volume
| 49 | |
| 14 | Author
| Mitra Ghassemzadeh, Kurt Dehnicke, Helmut Goesmann, Dieter Fenske | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0602.pdf | | | | Identifier
| ZNB-1994-49b-0602 | | | | Volume
| 49 | |
| 15 | Author
| Blaschette, PeterG. Jones, Karin Linoh, Ilona Lange, M. Artina Näveke, Dagmar Henschel, Axel Chrapkowski, Dietm Ar, Schomburg | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0999.pdf | | | | Identifier
| ZNB-1994-49b-0999 | | | | Volume
| 49 | |
| 16 | Author
| Oliver Seeger, Joachim Strähle | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1169.pdf | | | | Identifier
| ZNB-1994-49b-1169 | | | | Volume
| 49 | |
| 17 | Author
| Stefan Horstmann, Wolfgang Schnick | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1381.pdf | | | | Identifier
| ZNB-1994-49b-1381 | | | | Volume
| 49 | |
| 18 | Author
| Z. Naturforsch | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1763.pdf | | | | Identifier
| ZNB-1994-49b-1763 | | | | Volume
| 49 | |
| 19 | Author
| 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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| default:Reihe_B/49/ZNB-1994-49b-0089.pdf | | | | Identifier
| ZNB-1994-49b-0089 | | | | Volume
| 49 | |
| 20 | Author
| Peter Dierkes, Kurt Dehnicke, Dieter Fenske | Requires cookie* | | | Title
| Diinkomplexe | | | | Abstract
| von Wolfram(VI). D ie Kristallstruktur von [(Et2S)WCl4(Me3S i-C = C -(C H 2)4 -C = C -S iM e 3)WCl4(SEt2)] Diyne Complexes of Tungsten(VI). The Crystal Structure of [(Et2 S)WCl4 (M e3Si -C = C -(C H 2)4-C ^ C -SiMe3) WCl4 (SEt2)] The diyne complexes [(Et2S)W C l4(R -C ^ C -(C H 2)" -C = C -R)W C l4(SEt2)] (R = SiM e3, n = 3, 4, 8; R = C6H 5, n = 4, 8) have been prepared by the reaction o f /rarcs-[WCl4(SEt2)2] with the corresponding diyne in toluene solutions. The com plexes form green or orange, diamagne tic, moisture sensitive crystal powders, which were characterized by their IR and 13C NM R spec tra. The crystal structure of the com plex with R = SiM e3 and n = 4 has been determined. [(Et2S)WCl4(M e3S i-C = C -(C H 2)4-C = C -S iM e 3)W Cl4(SE t2)]: Space group P2j/c, Z -2, 3620 observed unique reflections with I>2a(I), R = 0.027. Lattice dimensions at -7 0 °C: a -1431.8(11), b -839.6(8), c = 1731.3(11) pm, ß = 112.74(2)°. The structure consists o f m ole cules in which both tungsten atom s are surrounded by four chlorine atoms in equatorial positions, both alkyne groups are bonded side on (rj2) to the tungsten atoms, whereas the sulfur atoms of the diethylsulfide molecules are located trans to the alkyne groups. | | | |
Reference
| Z. Naturforsch. 49b, 1391—1396 (1994); eingegangen am 17. Mai 1994 | | | |
Published
| 1994 | | | |
Keywords
| Diyne Complexes of Tungsten(VI), Synthesis, IR Spectra, NM R Spectra, Crystal Structure | | | |
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| default:Reihe_B/49/ZNB-1994-49b-1391.pdf | | | | Identifier
| ZNB-1994-49b-1391 | | | | Volume
| 49 | |
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