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1996 (114)
81Author    M. Itra, G. Hassem Zadeha, JörgM. Agullb, D. Ieter Fenskeb, KurtD. EhnickeaRequires cookie*
 Title    PPh4[Cl-I-C6H5] und PPh4[Br-I-C6H5] Iodobenzene as Lewis-Acid: Synthesis and Crystal Structures of PPh4[Cl-I-C6H5] and PPh4[Br-I-C6H 5]  
 Abstract    The donor-acceptor complexes [X-I-C6H5]~ with X" = Cl-and Br-have been prepared as tetraphenylphosphonium salts from iodobenzene and PPh4X in acetonitrile solutions. They form colourless single crystals, which were characterized by crystal structure determinations. PPh4[Cl-I-C6H5]: Space group P2,/c, Z = 4. Lattice dimensions at -70°C: a = 1301.1(5), 
  Reference    Z. Naturforsch. 51b, 1579—1582 (1996); eingegangen am 18. Juni 1996 
  Published    1996 
  Keywords    Halide Complexes of Iodobenzene, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1579 
 Volume    51 
82Author    M. M. Om, K. D. Ertza, Ehnickea ', J. M. AgullbRequires cookie*
 Title     
 Abstract    Colourless single crystals of the title compound are obtained from a saturated solution of NaOSiPh, in toluene in a humid atmosphere. We have characterized [N a ^ O S iP h ^ H iO),] by IR spectroscopy and by a crystal structure determination. Space group R3, Z = 6 , R -0.056. Lattice dimensions at -70°C: a -b = 1540.3 pm, c = 2639.6 pm. The compound has the structure of a Na40 4 heterocubane which is only slighty distorted and in which one of the sodium atoms is not hydrated and shows coordination number three. Die Kristallstruktur von [Na4(0SiPh3)4(H20)3] 
  Reference    Z. Naturforsch. 51b, 1583—1586 (1996); eingegangen am 9. Juli 1996 
  Published    1996 
  Keywords    Sodium Triphenylsilanolate Hydrate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1583.pdf 
 Identifier    ZNB-1996-51b-1583 
 Volume    51 
83Author    Z. NaturforschRequires cookie*
 Title    Über ein Blei-Kupfer-Tellurat PbC^TeOy mit Cu2+ in deformiert tetragonal pyramidaler und tetraedrischer Sauerstoffkoordination  
 Abstract    On a Lead C opper Tellurate P b C u 3T e 0 7 Containing C u2+ in D istorted Square Pyram idal and Tetrahedral O xygen C oordination B. W edel, Hk. M üller-B uschbaum * PbCu3T e07 has been prepared from the element oxides by solid state reaction in air. Single crystal X-ray work led too orthorhombic symmetry, space group D^-Pnma, a = 10.488(1), b = 6.353(2), c = 8.813(2) A, Z = 4. Cu(1)0 5 square pyramids and Te06 octahedra are members of the anionic part of the crystal structure, Cu(2) atoms show tetrahedral coordination by oxygen. The C u (2)2+ and the Pb2+ cations are incorporated into a [Cu(l)2Te07] network. PbCu,Te07 can thus be viewed as a lead copper oxocuprate(II) tellurate. Calculations of the Coulomb terms of lattice energy reveal two possible positions for the lone pair of electrons at Pb'+. 
  Reference    Z. Naturforsch. 51b, 1587—1590 (1996); eingegangen am 21. Mai 1996 
  Published    1996 
  Keywords    Lead, Copper, Tellurium, Oxide, Crystal Structure 
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 Identifier    ZNB-1996-51b-1587 
 Volume    51 
84Author    Herrn Prof, K. DrRequires cookie*
 Title    Reaktion  
 Abstract    von Ph3P=C=PPh3 mit Fe(CO)5; Molekülstrukturen von (CO)4Fe=C=C=PPh3 und Fe3(CO)9(/X3-r72-C=C-PPh3) Reaction o f Ph3P= C =P Ph3 w ith Fe(C O)5; M olecular Structures of (CO)4F e= C =C = P P h3 and Fe3(C O)9(/i3-/72-C = C -P P h 3). W olfgang P e tz * a, Frank W eller5 aGmelin- The ylide Ph3P=C=PPh3 reacts with Fe(CO)5 in toluene to give the metallacumulene (CO)4Fe=C=C=PPh3 (1) and 0=PPh3. A mixture of the ylide with its hydrolysis product Ph2P(0)-CH=PPh3 produces the trinuclear cluster Fe3(CO)9(^ 3-?/2-C=CPPh3) (2) in low yields which can also be obtained from 1 and Fe2(CO)9. Both compounds contain the same ligand bonded in a terminal (1) and in a bridging (2) manner. 1 and 2 crystallize in the monoclinic space groups P2(l)/n and P2(l)/c, respectively, with the unit cell parameters a = 1008.35(10), b= 1167.89(10), c = 1875.10(10) pm, ß = 99.824(10)° for 1 and a = 853.6(2), b = 1966.6(4), c = 1770.2(4) pm; ß = 99.05(3)° for 2. The compounds are further characterized by IR and NMR (l3C , 31P) spectroscopy and elemental analyses. 
  Reference    Z. Naturforsch. 51b, 1598—1604 (1996); eingegangen am 7. Juni 1996 
  Published    1996 
  Keywords    Crystal Structure, Hexaphenylcarbodiphosphorane, Iron Acetylide Complex, Metallacumulene 
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 Identifier    ZNB-1996-51b-1598 
 Volume    51 
85Author    Z. NaturforschRequires cookie*
 Title    On the Structure o f f-B utylam inotriphenylphosphonium Iodine D ichloride  
 Abstract    A del A m e ra, A n d rea M ayerb, D ouglas H o c, H ans Z im m erb * The structures of f-butylaminotriphenylphos-phonium iodine dibromide and iodine dichloride were determ ined by Raman spectroscopy and X-ray crystallographic structure analysis. The iodine dibromide [IBr2]~ species was assigned a centro­ symmetric nature, whereas the iodine dichloride [IC12]" possesses a non-centrosymmetric structure. 
  Reference    Z. Naturforsch. 51b, 1663—1665 (1996); received August 30 1995 
  Published    1996 
  Keywords    /-Butylaminotriphenylphosphonium Iodine D i­ chloride, Raman Spectra, Crystal Structure 
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 Identifier    ZNB-1996-51b-1663_n 
 Volume    51 
86Author    P. Eter, G. JonesRequires cookie*
 Title     
 Abstract    o ly su lfo n y la m in e, L X X V III [1] l-M e sy l-4 -d im e th y la m in o p y r id in iu m -d im esylam id : D a r ste llu n g und F estkörperstru ktur Polysulfonylam ines, L X X V III [1] l-M esyl-4-dim ethylam inopyridinium D im esylam ide: Synthesis and Solid State Structure A n d reas W irth, A rm an d B laschette Treating (MeSC^X^N with 4-dimethylaminopy-ridine in MeCN afforded the ionic title compound (monoclinic, space group P2j/c). The bond lengths of the 4-dimethylaminopyridinium moiety suggest a semiquinoid resonance form with a dou­ ble bond to the exocyclic nitrogen and two local­ ized carbon-carbon double bonds in the ring. The ring and the exocyclic N and S atoms of the cation are essentially coplanar. The S -N bond distances in the cation (173.4 pm) and the anion (159.1 and 159.6 pm) correlate with Pauling bond orders of 1.0 and 1.7, respectively. The anion displays a staggered conformation with approximate C2 symmetry (S -N -S 120.4°). 
  Reference    Z. Naturforsch. 51b, 1666—1668 (1996); eingegangen am 20. August 1996 
  Published    1996 
  Keywords    l-Mesyl-4-dimethylaminopyridinium Dimesylamide, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1666_n 
 Volume    51 
87Author    Klaus Kopka, RainerM. AttesRequires cookie*
 Title    Ein  
 Abstract    zweikerniger Vanadium(V)-Komplex mit (r/1)-und (/x-772:?72)-gebundenen Hydrazido(2-)-Liganden A D inuclear V anadium (V) C om plex w ith (r/1)-and (^ -//2://2)-Bonded H ydrazido(2-) L igands The title complex was obtained by reaction of guanidinium dioxodipicolinatovanadate(V) and N-methyl-N-phenylhydrazine. According to the single crystal structure analysis the dinuclear anion [(/i-PhN NH)(/t-O CH 3){(M ePhN N (dipic)V)}2]~ with sevenfold coordinated metal cen­ ters contains two types of hydrazido ligands. The ligand [MePhNN]: ~ is terminally bonded, and the VNN unit is linear with extensive electron delocalisation. The V-N and N-N bond lengths are 167.9(5) and 131.9(6) pm, respectively. The bonding of the bridging ligand is of the hitherto unknown fi-rf'.rf type, with V-N and N-N bond lengths of 202.5(5) and 136.5(5) pm, respectively. The V (N 2)V moiety is not planar. The compound was also characterized by H and 1V NMR spectroscopy. 
  Reference    Z. Naturforsch. 51b, 1675—1678 (1996); eingegangen am 30. Juli 1996 
  Published    1996 
  Keywords    Vanadium(V) Compounds, Hydrazido(2-) Complexes, Crystal Structure 
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 Identifier    ZNB-1996-51b-1675 
 Volume    51 
88Author    Joachim Pickardt, Britta KühnRequires cookie*
 Title     
 Abstract    etallkom plexe m it C yanoguanidin als L iganden: K ristallstru k tu ren von [Cd(cnge)2F2]*3H20 , C d(cnge)2B r2 und Hg(cnge)Cl2 (enge = C yanoguanidin) M etal C om plexes with C yanoguanidine as Ligand: Crystal Structures o f [Cd(cnge)2F2]-3H 20 , C d(cnge)2 Br^ and H g(cnge)C l2 (cnge = Cyanoguanidine) Crystals of [Cd(cnge)2F2]-3H20 (1), Cd(cnge): Br2 (2) and Hg(cnge)Cl2 (3) (cnge = cya­ noguanidine) were obtained by crystallisation from solutions of CdF2, CdBr2 or HgCl2 and cyanoguanidine in water/ethanol or methanol. 1 crystallizes monoclinically, space group C2, Z = 2,a = 1629.2(4), b = 1056.6(4), c -353.9(1) pm, 3 = 101.05(2)°; 2 is monoclinic, space group P2,/n, Z = 2 , a = 3 9 1.9(I), b = 850.7(2), c = 1722.1(4) pm, ß = 94.06(2)°, 3 is triclinic, space group P I, Z = 1, a = 686.7(1), b = 693.0(5), c = 387.2(4) pm, a = 94.45(5)°, ß = 95.05(4)°, 7 = 78.58(5)°. In 1 and 2 each Cd atom is bonded to four halogen atoms to form polymeric (CdF2)" and (CdBr2)" chains, resp., and to two cyanoguanidine molecules. In 3 each Hg atom is bonded to four chlorine atoms also forming (HgCl2)" chains, which are connected via cyanoguanidine molecules acting as a bidentate bridging ligands to form a network. 
  Reference    Z. Naturforsch. 51b, 1701—1706 (1996); eingegangen am 30. Juli 1996 
  Published    1996 
  Keywords    Cyanoguanidine, Cadmium Halide Complexes, Mercuric Chloride Complex, Crystal Structure 
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 Identifier    ZNB-1996-51b-1701 
 Volume    51 
89Author    Michael Feist, Sergej Trojanov, Erhard KemnitzRequires cookie*
 Title    Die Kristallstrukturen von 1,4-Dimethylpiperazinium-tetrabromo- cobaltat(II) und -zinkat(II), (dmpipzH2) [Mn Br4] (M = Co, Zn)  
 Abstract    The Crystal Structures of 1,4-Dimethylpiperazinium Tetrabromocobaltate(II) and -Zincate(II), (dmpipzH2) [MHBr4] (M = Co, Zn) The compounds (dmpipzH2)[MnBr4] (M = Co, Zn) crystallize at room temperature from equi-molar solutions of 1,4-dimethylpiperazine and MBr2 • n H20 in 3M HBr. (dmpipzH2)[CoBr4] is isotypic with the homologous chlorometalates of Co and Zn and crystallizes in the mono­ clinic space group P2,/m with a = 6.424(3), b = 14.588(6), c = 7.102(6) A, ß = 90.87(6)°, Z = 2. (dmpipzH2)[ZnBr4], however, crystallizes in the monoclinic space group P2,/c with a = 7,605(5), b = 13,760(9), c = 13,286(7) Ä, ß = 93,03(6)°, Z = 4. Both structures con­ tain centrosymmetric cations (dmpipzH2)2+ in the chair form and slightly distorted tetrahedra [MBr4]2~ with a mirror plane in the case ofM = Co. Several distances N- • -Brin both structures are interpreted in terms of N-H- • Br hydrogen bonds which are favoured by the packing in the case of M = Zn. 
  Reference    (Z. Naturforsch. 51b, 9—13 [1996]; eingegangen am 12. Juni 1995) 
  Published    1996 
  Keywords    1, 4-Dimethylpiperazinium Tetrabromometalates(II), Cobalt, Zinc, Crystal Structure 
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 Identifier    ZNB-1996-51b-0009 
 Volume    51 
90Author    Martin Köckerling, Gerald HenkelRequires cookie*
 Title    Nickelkomplexe  
 Abstract    mit Thioether-Chelatliganden: Elektrochemische Eigenschaften und Kristallstrukturen von [Ni(MeSCH2CH2SMe)2 (NCS)2], [Ni(EtSCH2CH2SEt)2(NCS)2] und [Ni(MeSCH2CH2SMe)2Br2] Nickel Complexes with Chelating Thioether Ligands: Electrochemical Properties and Crystal Structures of [Ni(MeSCH2CH2SMe)2(NCS)2], [Ni(EtSCH2CH,SEt)2(NCS)2] and [Ni(MeSCH2CH2SMe)2Br2] interest in nickel complexes with sulfur donor ligands as models for the active sites of nickel-containing hydrogenases has prompted us to investigate the structural and elec­ trochemical behaviour of nickel complexes with bifunctional thioether ligands. Crystals of [Ni(MeSCH,CH,SMe),(NCS),] (1) and [Ni(EtSCH2CH,SEt)2(NCS)2], (2) are triclinic, space group Pi, Z = 1, 1: a = 7.293(3) A, b = 7.567(3) A, c = 8.784(3) A, a = 72.81(3)°, ß = 78.41(3)°, 7 = 85.14(3)°; 2: a = 8.611(1) A, b = 8.101(1) Ä, c = 9.163(1) ßrbÄ, a = 66.54(1)°, ß = 76.19(1)°, 7 = 67.88(1)ßrb°. [Ni(MeSCH2CH2SMe^Br2] (3) crystallizes in the mono­ clinic space group P2,/n, a = 6.757(2) A, b = 7.881(2) A, c = 14.674(4) Ä, ß = 94.05(2)°, Z = 2. In crystals of 1, 2 and 3 mononuclear neutral complex molecules are observed which have pseudo-octahedral rran5-NiS4L2 coordination sites. The cyclovoltammograms of 1 and 3 in MeCN (Ag/AgCl/KCl, 3 mol/1) show only irreversible oxidation waves at +837 mV for 1 and +846 mV for 3, respectively, which are characteristic features of NCSe and Bre ions. In addition, a reduction wave at +393 mV is observed in 3. No redox response is found in the potential region between -700 and +100 mV which is used by the NiFe hydrogenase enzymes. 
  Reference    Z. Naturforsch. 51b, 178—186 (1996); eingegangen am 18. Juli 1995 
  Published    1996 
  Keywords    Nickel-Sulfur Complexes, Thioether Ligands, Crystal Structure, Electrochemistry, Bioinorganic Chemistry Current 
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 Identifier    ZNB-1996-51b-0178 
 Volume    51 
91Author    JörgH. Albering, Wolfgang JeitschkoRequires cookie*
 Title    Quaternary Thorium Transition Metal Pnictide Oxides: ThCu^j-PO, ThCuAsO, and Th2Ni3 _xP3 0  
 Abstract    The new compounds T h C u ^ P O and ThCuAsO with ZrCuSiAs-type structure were pre­ pared in well crystallized form by chemical vapor transport reactions. Th2N i3.A :P30 with a new structure type was obtained by reaction o f T h 0 2 with the other elem ental components in an alumina crucible at high temperatures. The crystal structures of the three compounds were determined from single-crystal X-ray data. ThCuj.xPO: P4/nmm, a = 389.43(4), c -828.3(1) pm, R = 0.024 for 13 variable parameters and 338 structure factors; ThCuAsO: P4/ nmm, a = 396.14(5), c = 844.0(1) pm, R = 0.028 (13 variables and 379 F values); Th2Ni3_JP30 : P4/nmm, a = 394.62(4), c = 1723.2(3) pm, R = 0.018 (27 variables and 374 F values). The refinement of the occupancy parameters revealed significant deviations from the ideal values for the transition metal sites for two compounds resulting in the exact compositions ThCu0938(4)PO and Th2N i2 45(nP30 . Magnetic susceptibility measurements indicate Pauli paramagnetism for T hC u^P O . The crystal structures of these compounds are closely related. They belong to a large family o f tetragonal structures of which the ThCr2Si2-and the PbFCl-type structures are well known examples. 
  Reference    Z. Naturforsch. 51b, 257 (1996); received July 6 1995 
  Published    1996 
  Keywords    Crystal Structure, Quaternary Thorium-Transition Metal-Pnictide Oxides, Chemical Vapor Transport 
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 Identifier    ZNB-1996-51b-0257 
 Volume    51 
92Author    PaulK. Baker3, DavidJ M Uldoona, MichaelB. Hursthouseb, SimonJ. Colesb, AidanJ. Laveryc, Andrew ShawcrosscRequires cookie*
 Title    The Crystal Structure and Low Temperature 13C NMR Spectrum of the Seven-Coordinate Complex of Tungsten(II), [WI2(CO)3(NCPh)2]  
 Abstract    The crystal structure of [WI2(C O)3(N C Ph)2] (1) has been determined by X-ray methods. The crystals are orthorhombic, space group Pnam, a = 7.815(3), b = 13.839(5), c = 18.475(3) Ä, Z = 8, R -0.0346 for 1497 observed data. The complex [WI2(C O)3(NCPh)2] has a seven-coordinate geometry, which may be described as a distorted capped octahedron, with the two iodo-ligands mutually trans, while each nitrile is trans to a carbonyl group. The capped octahedral geometry consists of a capping carbonyl (C(10)} on the face defined by 1(1), C(20) and C(20)#. However, the geom etry may also be described as a capped trigonal prism, which has one triangular face occupied by three carbonyl groups and the second triangular face occupied by N (l) , N (l)# and 1(1) atoms, respectively. The iodide 1(2) occupies the capping position on the rectangular face defined by the atoms C(20), C(20)#, N (l), and N (l)# . The low temperature 13C NM R spectrum (203 K, C D 2C12) of 1 shows a single carbonyl resonance at 219.27 ppm which indicates that the com plex is undergoing a rapid fluxional process in solution at 203 K. 
  Reference    Z. Naturforsch. 51b, 263 (1996); received July 7 1995 
  Published    1996 
  Keywords    Crystal Structure, Benzonitrile, Carbonyl, D iiodo, Tungsten(II) 
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 Identifier    ZNB-1996-51b-0263 
 Volume    51 
93Author    DietrichK. Breitinger, Roman BreiterRequires cookie*
 Title      
 Abstract    ?ram-(NH4)2[R u (S 0 3)2(N H 3)4]-4 H 20 (1) (m onoclinic, P l x!n\ a = 629.8(3), b = 1000.6(2), c = 1345.7(5) pm, ß = 112.25(4)°, Z = 2; R = 0.021; R w = 0.017) is obtained as pale greenish-yellow crystals by reaction of /ra « s-[R u (S 0 3H)2(N H 3)4] (2) with aqueous ammonia, and crys­ tallization at +5 °C. The compound, when isolated, is stable at room temperature for only a few days even under inert gas, but persists under the mother liquor. In the centrosymmetric anion frö/?s-[Ru(S03)2(N H 3)4]2~ the bonds Ru-S = 230.5(1) pm are significantly longer than in the neutral complex 2 (227.6(1) pm), whereas the Ru-N bonds are the same in both com ­ plexes within experimental error (averages 214.1 and 214.0 pm). Hence, the mutual trans-influence of the sulfite ligands is weakened on protonation; the bonding of the co-ligands in c/s-position is not affected. The internal structure o f the sulfite ligand in 1 with long S-O bonds (average 151.2(5) pm) and small angles O-S-O (average 106.1(6)°) and the weakened Ru-S bond are a good match. The structure of 1 is held together by a complex network of hydrogen bonds, in which all potential hydrogen-bond donors (O H 2, N H 4+, N H 3) and accep­ tors (H 20 , S 0 3) are involved. The structural findings are reflected in the vibrational spectra. 
  Reference    Z. Naturforsch. 51b, 517 (1996); received August 25 1995 
  Published    1996 
  Keywords    Ruthenium(II) Sulfito Complex, Crystal Structure, m ws-Influence, Hydrogen Bonding 
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 Identifier    ZNB-1996-51b-0517 
 Volume    51 
94Author    Thomas Dahlems, Dietrich Mootz, Michaela SchillingRequires cookie*
 Title    Zweidimensionales Eis und H50 2+-Ionen. Zur Bildung und Struktur tiefschmelzender molekularer und ionischer Hemi-bis Hexahydrate halogenierter Essigsäuren CCl"F3."COOH (n = 1 bis 3) [1] Two-Dimensional Ice and H 50 2+ Ions. On Formation and Structure of Low-Melting Molecular and Ionic Hemi-through Hexahydrates of Haloacetic Acids CCl"F3."COOH (n = 1 to 3) [1]  
 Abstract    Hydrate formation o f haloacetic acids CCl"F3_"COOH (n = 1, 2, 3) has been studied by D TA and tem perature-dependent X-ray powder diffraction, and evidence obtained for five phases, all melting at temperatures below ambient. The hydrates have been confirmed and further characterized by their crystal structures at -1 5 0 °C. Three lower hydrates, CC12F C O O H 0.5H -> 0 (space group P2,/c and Z = 8 formula unites per unit cell), CC1F2C 0 0 H H 20 (P2,/c, Z = 4), and CC1F2C 0 0 H -4 H 20 (P I, Z = 2), have molecular structures with the acid and water m olecules hydrogen-bonded in two-dimensional arrays. The structures of the remaining hydrates, CCl2F C O O H -6H 20 and CC13C 0 0 H -6 H 20 (sim i­ lar, but not isotypic, both P 1 and Z = 2), are ionic, as (H s0 2+)(C X 3C 0 Ö) -4 H 20 , and three-dimensional. The neutral water molecules are hydrogen-bonded in ice-like layers rare in crystal chemistry. A lso, CCl2FCOOH is established only as the second acid o f which a lower hydrate is molecular and a higher one ionic. 
  Reference    Z. Naturforsch. 51b, 536 (1996); eingegangen am 16. Oktober 1995 
  Published    1996 
  Keywords    Crystal Structure, Haloacetic Acid Hydrate, Hydrogen Bonding, Melting Diagram 
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 Identifier    ZNB-1996-51b-0536 
 Volume    51 
95Author    G. O. Stendorp3, O. Tterb, H. HomRequires 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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0567.pdf 
 Identifier    ZNB-1996-51b-0567 
 Volume    51 
96Author    D. Bublitz, A. Franken, W. Preetz, H. ThomsenRequires 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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 Identifier    ZNB-1996-51b-0609_n 
 Volume    51 
97Author    JosephG. Robe, Duc Le Van, JostW. Innemöller, Bernt Krebs, M. Echtild LägeRequires cookie*
 Title    Reaktive E=C(p-p)7r-Systeme, XLIII [1] Darstellung und Charakterisierung P-Phosphino-oder P-Arsino-substituierter Fluorphosphaalkene des Typs R2E-P=C(F)NEt2 (R = Me, CF3, Me2N; E = P, As)  
 Abstract    Reactive E=C(p-p)-7r System s XLIII [1] Synthesis and Characterization o f P -Phosphino or P-A rsino Substituted Fluoro-phosphaalkenes of the Type R 2E -P=C (F)N Et2 (R = Me, C F 3, M e7N; E = R As) The easily accessible phosphaalkene HP=C(F)NEt2 (lb) reacts with halophosphanes or -arsanes R2EX (X = Cl, I) in the presence of NEt3 to give P-phosphino-or -P-arsino sub­ stituted fluorophosphaalkenes of the type RiE-P=C(F)NEti (2 -6) in high yields (60 -85 %) [R2E: (CF3)2P (2), Me2N(CF3)P (3), Me2P (4), (CF3)2As (5), M e2As (6)]. The analogous re-action of ib with CF3PI2 (molar ratio 1:2) unexpectedly leads to the triphosphetene Et2N 
  Reference    Z. Naturforsch. 51b, 778—784 (1996); eingegangen am 30. November 1995 
  Published    1996 
  Keywords    Phosphaalkenes, 1, 2, 3-Triphosphetenes, NMR Spectra, Crystal Structure 
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 Identifier    ZNB-1996-51b-0778 
 Volume    51 
98Author    M. Steiner, A. Artina, Klaus-Jürgen Ndratschke, RangeRequires cookie*
 Title    C laudia  
 Abstract    Single crystals of Nd4Au20 9 and Gd4Au20 9 have been prepared by oxidizing mixtures of gold metal and Nd20 3 or Gd20 3, rsp., with K 0 2 under high-pressure high-temperature conditions (40 kbar, 1200°C) in a modified Belt-type apparatus. The X-ray structure analyses have been carried out on twinned crystals. The compounds crystallize in the orthorhombic space group Pbcn (Nd4A u ,0 9: a = 11.938(7) , b = 6.126(2),c = 11.928(3) A ,Z = 4,/?1 = 0.0443; Gd4A u ,0 9: a = 11.922(2), 6 = 6.1242(7), c = 11.917(2) A, Z = 4. R\ =0.0232). The title compounds are isostructural with La4Au20 9. Their structure comprises isolated square-planar A u04 groups, stacked along [010] to form a columnar structure. The Au-Au distance along the columnar direction is 3.10 A. Structural relations to Bi2C u04 und (Nd, Pr)2A u05 are discussed. Hochdrucksynthese und K ristallstruktur von Nd4Au2 C>9 und Gd4Au2 C>9 
  Reference    Z. Naturforsch. 51b, 811—816 (1996); eingegangen am 1. Dezember 1995 
  Published    1996 
  Keywords    Lanthanoide Aurates(III), High-Pressure Synthesis, Crystal Structure, Columnar Stacking 
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 Identifier    ZNB-1996-51b-0811 
 Volume    51 
99Author    D. Irk Johrendt, R. Einer, M. Iericke, A.Lbrecht MewisRequires 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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 Identifier    ZNB-1996-51b-0905_n 
 Volume    51 
100Author    Stephan Pitter, EckhardD. Injus, Beate Jung, H. Elm, Ar GörlsRequires 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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0934.pdf 
 Identifier    ZNB-1996-51b-0934 
 Volume    51 
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