| 81 | Author
| Tetraazadibenzo Macrocycle, Ralf Feldhaus, Jens Köppe, Rainer Mattes, Ulrich Voet | Requires cookie* | | Title
| Synthesis and Structures of the Vanadyl, Cobalt(III), Nickel(II), Copper(II), Zinc(II) and Palladium(II) Complexes of a 14-Membered Unsaturated  | | | Abstract
| The synthesis and structural characterisation of complexes of the 14-membered macrocyclic trans-N4 dibenzo ligand 7,8,9,16,17.18-hexahydrodibenzo[e,l][ 1,4, 8.11 ]-tetraazacyclotetra-decine (L 1) is described. The crystal structures of six compounds were determined by single crystal X-ray diffraction. In [CuL1 ]2+ the metal atom is tightly bound within the macrocyclic cavity. The Cu-N bonds [201.2(3) and 191.8(3) pm] are rather short. Zn(II) is penta-coordinated in [Zn(L')C l]+ with the metal center outside the cavity. L 1 is deprotonated at one or both secondary amine functions in the complexes [N i(L '-H)]+, [Co(L -2H)]+, [VO(L'-2H)] and [Pd(L'-2H)]. With the exception of [VO (L'-2H)] the metal ions assume nearly square planar N4-coordination, which is very rare for Co(III). Salts of [Co(L'-2H)]+ display a temperature independent magnetic moment of 0,64 B. M. The nickel, cobalt and palladium complexes show remarkably short metal-nitrogen bond distances: Ni-N [183.8(8)], Co-N [181.8(2)] and Pd-N [194.5(6) pm], respectively. The UV/Vis and EPR spectra, and the electrochemical behaviour of some of these complexes are also discussed. | | |
Reference
| Z. Naturforsch. 51b, 1449—1458 (1996); eingegangen am 1. April 1996 | | |
Published
| 1996 | | |
Keywords
| Macrocyclic N4-Donor Ligands, Transition Metal Complexes, Crystal Structure | | |
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| default:Reihe_B/51/ZNB-1996-51b-1449.pdf | | | Identifier
| ZNB-1996-51b-1449 | | | Volume
| 51 | |
82 | Author
| Cl Walter, Frank, GuidoJ. Reiß | Requires cookie* | | Title
| Spezielle Alkylammoniumhexachlorometallate, II [1] Synthese und Kristallstruktur von Bis(l,2-diammoniopropan)hexachlororhodat(III)-chlorid, [H3N-CH(CH3)-CH2-NH3]2[RhCl6]Cl Alkylammonium Hexachlorometallates, II [1] Synthesis, and Crystal Structure of Bis( 1,2-diammoniopropane) Hexachlororhodate(III) Chloride, (H3N-CH(CH3)-CH9-NH3]-,|RhCl6]  | | | Abstract
| Bis(1,2-diammoniopropane) hexachlororhodate(III) chloride, [H ^N -CH tCI-fO -CH i-N H ^ [RhCl6]Cl (1) has been obtained by the reaction of rhodium(III) chloride with rac-1,2-diammoniopropane dihydrochloride in hydrochloric acid solution. The quasi-ternary com pound, which crystallizes in the orthorhombic space group Pbca (a -11.0007(13) A, b = 22.181(2) A, c = 14.638(2) A, V = 3571.7(7) Ä \ T = -1 2 0 °C, Z -8) contains two crystallographically independent 1,2-diammoniopropane ions beside one hexachlororhodate and one chloride ion. One of the cations shows a R/S-S/R-disorder of enantiomeric pairs in the centrosymmetric crystal lattice. The packing scheme is determined by a complex framework of hydrogen bonds. | | |
Reference
| Z. Naturforsch. 51b, 1459—1463 (1996); eingegangen am 9. April 1996 | | |
Published
| 1996 | | |
Keywords
| Hexachlororhodate, Alkylammonium Salt, Crystal Structure, Hydrogen Bonding | | |
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| default:Reihe_B/51/ZNB-1996-51b-1459.pdf | | | Identifier
| ZNB-1996-51b-1459 | | | Volume
| 51 | |
83 | Author
| Walter Frank, GuidoJ. Reiß | Requires cookie* | | Title
| Spezielle Alkylammoniumhexachlorometallate, III [1] Synthese und Kristallstruktur von Tris(guanidinium)- hexachlororhodat(III)-monohydrat, [C(NH2)3 ]3 [RhCl6] * H20 Alkylammonium Hexachlorometallates, III [1] Synthesis, and Crystal Structure of Tris(guanidinium) Hexachlororhodate(III) Monohydrate, [C(NH2)3]3[RhCl6] * H20  | | | Abstract
| Tris(guanidinium) hexachlororhodate(III) monohydrate, [C(NH2)3]3[RhCl6] • H20 (1) has be en obtained by the reaction of rhodium(III) chloride with guanidine hydrochloride in hydrochlo ric acid solution. 1 crystallizes in the triclinic space group P i (o = 7.6013(9) A, b = 8.6912(10) A, c = 15.956(2) Ä, q = 93.177(10)°, ß = 101.691(10)°, 7 = 113.995(9)°, V = 931.8(2), Z = 2). Two crystallographically independent hexachlororhodate ions, three crystallographically independent guanidinium ions and one water molecule are linked by a complex framework of hydrogen bonds. | | |
Reference
| Z. Naturforsch. 51b, 1464—1468 (1996); eingegangen am 9. April 1996 | | |
Published
| 1996 | | |
Keywords
| Hexachlororhodate, Guanidinium Salt, Crystal Structure, Hydrogen Bonding | | |
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| default:Reihe_B/51/ZNB-1996-51b-1464.pdf | | | Identifier
| ZNB-1996-51b-1464 | | | Volume
| 51 | |
84 | 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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| default:Reihe_B/51/ZNB-1996-51b-0009.pdf | | | Identifier
| ZNB-1996-51b-0009 | | | Volume
| 51 | |
85 | 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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| default:Reihe_B/51/ZNB-1996-51b-0178.pdf | | | Identifier
| ZNB-1996-51b-0178 | | | Volume
| 51 | |
86 | 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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| default:Reihe_B/51/ZNB-1996-51b-0257.pdf | | | Identifier
| ZNB-1996-51b-0257 | | | Volume
| 51 | |
87 | 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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| default:Reihe_B/51/ZNB-1996-51b-0263.pdf | | | Identifier
| ZNB-1996-51b-0263 | | | Volume
| 51 | |
88 | 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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| default:Reihe_B/51/ZNB-1996-51b-0517.pdf | | | Identifier
| ZNB-1996-51b-0517 | | | Volume
| 51 | |
89 | 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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| default:Reihe_B/51/ZNB-1996-51b-0536.pdf | | | Identifier
| ZNB-1996-51b-0536 | | | Volume
| 51 | |
90 | 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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| default:Reihe_B/51/ZNB-1996-51b-0567.pdf | | | Identifier
| ZNB-1996-51b-0567 | | | Volume
| 51 | |
91 | 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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| default:Reihe_B/51/ZNB-1996-51b-0609_n.pdf | | | Identifier
| ZNB-1996-51b-0609_n | | | Volume
| 51 | |
92 | 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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| default:Reihe_B/51/ZNB-1996-51b-0778.pdf | | | Identifier
| ZNB-1996-51b-0778 | | | Volume
| 51 | |
93 | 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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| default:Reihe_B/51/ZNB-1996-51b-0811.pdf | | | Identifier
| ZNB-1996-51b-0811 | | | Volume
| 51 | |
94 | 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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| default:Reihe_B/51/ZNB-1996-51b-0905_n.pdf | | | Identifier
| ZNB-1996-51b-0905_n | | | Volume
| 51 | |
95 | 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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| default:Reihe_B/51/ZNB-1996-51b-0934.pdf | | | Identifier
| ZNB-1996-51b-0934 | | | Volume
| 51 | |
96 | Author
| ]. C. Nachtigal, W. Preetz | Requires cookie* | | Title
| Darstellung, n B-NMR  | | | Abstract
| , Schwingungsspektren und Kristallstruktur von Bis(tetraphenylphosphonium)-2-[2-(2-pyridyl-amino)-pyrid-5-yl]-c/oso-decaborat, [P(C6H5)4]2[2-{2-(2-(C5H4N)-NH)-(C5H3N)-5}B10H9] Preparation, 11B NMR, Vibrational Sprectra and Crystal Structure of Bis(tetraphenylphosphonium) 2-[2-(2-Pyridyl-amino)-pyrid-5-yl]-c/fxw-decaborate, [P(C6H5)4]2 [2 2-[2-(2-Pyridyl-am ino)-pyrid-5 -yl]-c7r« 0-decaborate( | | |
Reference
| Z. Naturforsch. 51b, 1559—1562 (1996); eingegangen am 29. Mai 1996 | | |
Published
| 1996 | | |
Keywords
| ), Crystal Structure, n B NMR Spectra, Vibrational Spectra | | |
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| default:Reihe_B/51/ZNB-1996-51b-1559.pdf | | | Identifier
| ZNB-1996-51b-1559 | | | Volume
| 51 | |
97 | Author
| Hristoph Linke, M. Artin, Jansen | Requires cookie* | | Title
| C  | | | Abstract
| Ag8Ge3O 10 was obtained from a mixture of the binary oxides by solid state reaction in the presence of a small amount of water which is acting as an accelerator. Conditions applied were T = 500 °C and p (0 2) = 1,2 kbar. According to an X-ray crystal structure analysis the title compound contains four crystallographically independent trigermanate [Ge3O 10]8-ions per unit cell (Pc, a = 12.1549(11), b = 10.7375(14), c = 18.5169(20) Ä, ß = 92.326(10)°, 13448 independent reflections, R 1 = 6 ,1 %, wR2 = 13,0%, Z = 8). Thermal decomposition, as recorded by DTA and temperature dependent Guinier photographs, occurs at 520 °C. Ag8Ge3O ,0 is diamagnetic with a molar susceptibility of -330-10" cm3 mol" 1. Darstellung, Kristallstruktur und physikalische Eigenschaften von Oktasilbertrigermanat, Ag8Ge3O10 | | |
Reference
| Z. Naturforsch. 51b, 1591—1597 (1996); eingegangen am 18. April 1996 | | |
Published
| 1996 | | |
Keywords
| Octasilver Trigermanate, High Oxygen Pressure Synthesis, Crystal Structure, Physical Properties | | |
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| default:Reihe_B/51/ZNB-1996-51b-1591.pdf | | | Identifier
| ZNB-1996-51b-1591 | | | Volume
| 51 | |
98 | Author
| Rolf Minkwitz, Ulrike Lohmann, Hans Preut | Requires cookie* | | Title
| Methansulfinylchlorid-Lewissäure  | | | Abstract
| Addukte CH3S(Cl)OMF5 (M = As, Sb) und Kristallstruktur von CH3S(Cl)OSbCl5 [1] Methanesulfinylchloride Lewis Acid Adducts CH3S(Cl)OMF5 (M = As, Sb) and Crystal Structure of CH3S(Cl)OSbCl5 [1] CH 3S(0)C1 reacts in HF as solvent with MF5 (M = As, Sb) to give products CH 3S(Cl)OMF5 (M = As, Sb). The new compounds are stable below 253 K and were charac terized by Raman and N M R spectroscopy. In addition, the crystal structure of C H 3S(Cl)OSbCl5 has been determinated. The complex crystallizes in the monoclinic space group P2x !n with a = 644.3(5), b = 1905.9(14), c = 900.0(7) pm, ß = 99.27(6)° with four formula units per unit cell. | | |
Reference
| Z. Naturforsch. 51b, 133—138 (1996); eingegangen am 6. Juni 1995 | | |
Published
| 1996 | | |
Keywords
| Methanesulfinylchloride Lewis Acid Complexes, Preparation, Raman Spectra, N M R Spectra, Crystal Structure | | |
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| default:Reihe_B/51/ZNB-1996-51b-0133.pdf | | | Identifier
| ZNB-1996-51b-0133 | | | Volume
| 51 | |
99 | Author
| Hans Bock, Sabine Nick, Wolfgang Seitz, Christian Näther, JanW. Bats | Requires cookie* | | Title
| Structures of Charge-Perturbed or Sterically Overcrowed Molecules, 80 [1 -3] Structural Changes of /?-Benzoquinone by Donor and Acceptor Substituents  | | |
Reference
| Z. Naturforsch. 51b, 153—171 (1996); eingegangen am 29. Mai 1995 | | |
Published
| 1996 | | |
Keywords
| Crystal Structure, Oxo-and Alkylamino-Substituted p-Benzoquinone Derivatives, Substituent Effects, Cyanine Distortion, AM 1 Calculations | | |
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| default:Reihe_B/51/ZNB-1996-51b-0153.pdf | | | Identifier
| ZNB-1996-51b-0153 | | | Volume
| 51 | |
100 | 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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| default:Reihe_B/51/ZNB-1996-51b-0277.pdf | | | Identifier
| ZNB-1996-51b-0277 | | | Volume
| 51 | |
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