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1998 (237)
101Author    Requires cookie*
 Title    Neuartige  
 Abstract    Synthese und M olekül­ struktur von Benzylkalium (thf) [KCH2C6H 5]2 N o v el S y nthesis a n d M o le c u la r S tru c tu re o f B enzyl P o tassiu m (th f)[K C H 2C 6H 5]2 
  Reference    Z. Naturforsch. 53b, 625 (1998) 
  Published    1998 
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 Identifier    ZNB-1998-53b-0625_n 
 Volume    53 
102Author    Requires cookie*
 Title    Weitere Verbindungen zum Ba6N d2A l40 15-Typ: Ba4Nd4Z n 3 P t0 15 und Ba4Eu4Zn3P tO |5  
 Abstract    F u rth e r C o m p o u n d s o f th e B a 6N d 2A l4O j5 T ype: B a 4N d 4Z n 3P t 0 15 an d B a4E u 4Z n 3P t 0 15 
  Reference    Z. Naturforsch. 53b, 628 (1998) 
  Published    1998 
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 Identifier    ZNB-1998-53b-0628_n 
 Volume    53 
103Author    Requires cookie*
 Title    Fe[B2P 2 0 7( 0 H ) 5]: Ein neues Boro- phosphat mit unverzweigten Vierer-Einfach Tetraederketten  
  Reference    Z. Naturforsch. 53b, 631 (1998) 
  Published    1998 
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 Identifier    ZNB-1998-53b-0631_n 
 Volume    53 
104Author    Requires cookie*
 Title    Polysulfonylamine, CIII [1] Ein Hydroxylamin mit bemerkenswert kurzer O -N -B indung: Kristall-und Molekülstruktur von M e0 -N (S 0 2Me)2  
  Reference    Z. Naturforsch. 53b, 634 (1998) 
  Published    1998 
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 Identifier    ZNB-1998-53b-0634_n 
 Volume    53 
105Author    Requires cookie*
 Title      
 Abstract    -methylethyl) -[29H,31H-tetrapyrido[2,3-b:2',3'-g: 2' '-3"-I:2'' ',3'' '-q]porphyrazinato-(2-)N29,N30,N31,N32]-nickel-[E u(fod)3]4 -Ein lösliches Pyridoporphyrazin 
  Reference    Z. Naturforsch. 53b, 637 (1998) 
  Published    1998 
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 Identifier    ZNB-1998-53b-0637_n 
 Volume    53 
106Author    Kristallstruktur, Ethyl Arista Gräfe-Kavoosian, Shida Nafepour, Klaus Nagel, Karl-Friedrich TebbeRequires cookie*
 Title    Untersuchungen an Polyhalogeniden, XXXVI. Zur Kenntnis des Oktaiodid-Ions I82-: Darstellung  
 Abstract    des [(Crypt-2.2.2)H2]l8> des [Ni(phen)3]I8*2CHCl3 und der Bis(N-alkyluro-tropinium)oktaiodide (UrR)2I8 mit R = Methyl und Ethyl Studies on Polyhalides, XXXVI. On the Octaiodide Ion I82~: Preparation and Crystal Structure of [(Crypt-2.2.2)H2]I8, of [Ni(phen)3]I8-2CHCl3 and of the Bis(N-alkylurotropinium)octaiodides (UrR)2I8 with R = methyl Cryptate, N-Alkyl-Urotropinium Cation, Tris(l,10-phenanthroline)nickel(II), Octaiodide, Crystal Structure The new compound [(Crypt-2.2.2)H 2]I8 has been prepared by the reaction of [(Crypt-2.2.2)H2](I3)2 with iodine in methanol. It crystallizes in the orthorhombic space group Pbcn with a = 11.476 (2), b = 13.589 (2), c = 22.888 (2) A and Z = 4. The crystal structure has been refined to R F = 0.031 for 1618 reflections. It may be described as a layerlike packing of octaiodide anions I82-and diprotonated 2.2.2-Crypt as cations. The non planar octaiodide anion is built up from two triiodide groups and a bridging iodine molecule. Tris(1, lO-phenanthroline)nickel(II) octaiodide bis(chloroform) crystallizes in the monoclinic space group P2,/n with a = 11.683 (8), b = 21.717 {8), c = 20.752 (5) Ä, ß = 95.03 (5)° and Z = 4 formula units. The crystal structure has been refined to RF = 0.058 for 3894 reflections. The structure consists of two chloroform molecules, octahedrally coordinated complex cations [Ni(phen)3]2+ and nonplanar octaiodide anions I82~ each composed of two asymmetric triiodide units I3~ weakly associated with an elongated bridging iodine molecule I2. The already known structure of bis(N-methylurotropinium) octaiodide, (UrMe)2I8, has been verified and more accurate crystal data have been collected. The crystal structure has been refined to RF = 0.045 for 1908 reflections. The compound crystallizes in the monoclinic space group P 2,/c with a = 11.302 (2), b = 9.850 (2), c = 14.188 (2) A , ß = 92.59 (1)° and Z = 2. The anion has the shape of a stretched Z. The structure of bis(N-ethylurotropinium) octaiodide (UrEt)2I8 has been determined and a new configuration (I3" -I5-) for octaiodide ions between Z (I3_ -I2-I3_) and a "broken" confi­ guration (I3~, I5_) has been observed. The compound crystallizes in the triclinic space group P i with a = 9.741 (3), b = 11.815 (3), c = 15.426 (3) A, a = 91.80 (2), ß = 107.14 (2), 7 = 90.04 (2)° and Z = 2. The crystal structure has been refined to RF = 0.037 for 3657 reflections. 
  Reference    Z. Naturforsch. 53b, 641—652 (1998); eingegangen am 2. März 1998 
  Published    1998 
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 Identifier    ZNB-1998-53b-0641 
 Volume    53 
107Author    PeterG. Jones, Birte AhrensRequires cookie*
 Title    Gold(I)-Komplexe mit Aminliganden, II [1]. (Methylpyridin)-Komplexe von Gold(I) Gold(I) Complexes with Amine Ligands, II. Methylpyridine Complexes of Gold(I)  
 Abstract    Gold(I) complexes of overall formula LAuCl (L = various methylpyridines) are non-con­ ducting in acetone. X-ray structure analyses show that the solid state structure of the cor­ responding complex 1 (L = 2-picoline) is molecular; the 3-picoline derivative 2 is however ionic (L2A u)+(AuCl2)-. 3-Picoline forms a molecular complex LAuC6F5 (3) and also the ionic (L2Au)+(SbF6)_ (4). Complexes 1, 2 and 4 display short A u--A u contacts, leading to chains of gold atoms; additionally, complexes 3 and 4 show weak Au-F contacts. The (3-picoline)-gold(III) complex /rans-(L2AuCl2)+(SbF6)_ (5) was obtained as a by-product; it too contains short Au-F contacts. 
  Reference    Z. Naturforsch. 53b, 653—662 (1998); eingegangen am 6. April 1998 
  Published    1998 
  Keywords    Gold(l), Pyridine, Amine Complexes, X-Ray Data 
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 Identifier    ZNB-1998-53b-0653 
 Volume    53 
108Author    ChlorotrimethylsilaneJan Schneider3, Eckhard Popowski, Hans FuhrmannbRequires cookie*
 Title    Reaktionen von Lithiumhydridosilylamiden mit Carbonylverbindungen und Gemischen von Carbonylverbindungen und Chlortrimethylsilan Reactions of Lithium Hydridosilylamides with Carbonyl Compounds and Mixtures of Carbonyl Compounds  
 Abstract    The lithium hydridosilylamides Me2(H)SiN(Li)R (1: R = CM e3, 2: R = SiMe3) were allowed to react either with the non-enolizable carbonyl compounds CH2=C(Me)CHO, PhCHO and Ph2CO followed by trapping with chlorotrimethylsilane (A), or with mixtures of these carbonyl compounds and chlorotrimethylsilane (B). In the second case the course of the reactions is determined by the carbonyl compound. The composition of the reaction mixtures is nearly the same according to A and B. Main products in the reactions with the aldehydes are the corresponding imines R'CH=NR (R' = CH2=C(Me), Ph) 3 , 4 , 8 ,9 formed by addition of the hydridosilylamides to the C = 0 group of the aldehydes and subsequent LiOSiM e2H elimination. Partial hydrosilylation of the alde­ hydes by the hydridosilanolate followed by the trimethylsilylation yields the alkoxydisiloxanes R'CH2OSiMe2OSiMe3 6 , 11. In some cases 2 partially reacts under hydrosilylation to give the alkoxydisilazanes R'CH2OSiM e2NHSiM e3 7,12. The hydrosilylation is the preferred reaction of 1 and 2 with benzophenone. The compounds Ph2CHOSiMe2NHR 13, 14 are obtained. This difference in the reaction behaviour of 1 and 2 towards the aldehydes and benzophenone is mainly due to steric reasons. Depending on the conditions the imines Ph2C=NR 20, 21 may be formed. Ph2CHOSiM e2OSiMe3 (22) is a secondary product of imine formation. In all reactions of 1 and 2 with the carbonyl compounds the corresponding alkoxysilanes R'CH2OSiMe3 (5: R' = CH 2=C(Me), 6 : R' = Ph) and Ph2CHOSiM e3 (15) are generated. Compounds resulting from a reaction of 1 and 2 with chlorotrimethylsilane are produced to minor extent, but only if the molar ratio of amide to carbonyl compounds is not greater than one. The formation of a silanimine intermediate in reaction according to B is not observed. 
  Reference    Z. Naturforsch. 53b, 663—672 (1998); eingegangen am 9. April 1998 
  Published    1998 
  Keywords    Hydridosilylamides, Reaction Behaviour, Imines, Hydrosilylation 
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 Identifier    ZNB-1998-53b-0663 
 Volume    53 
109Author    V. Erena, M.T T Hiede, W. Olfgang, JeitschkoRequires cookie*
 Title    Ternary Intermetallic Compounds L«Mn2Ali0 (Ln = Y, La-Nd, Sm, Gd-Dy) and L«Re2Al10 (Ln = Ce, Pr, Sm) with CaCr2Al10-Type Structure  
 Abstract    The twelve title compounds have been prepared for the first time. Their CaCnA lio-type structure (PA/nm m, Z = 4) was refined from single-crystal X-ray data for the three representatives TbM mAlio (a = 1274.3(2) pm, c = 511.4(2) pm, R = 0.025 for 680 structure factors F and 43 variable parameters VO, CeRe2Alio (a -1295.5(5) pm, c -517.2(4) pm, R = 0.054 for 810 F a n d 46 V), and SmReaAlio (a = 1291.5(2) pm, c = 516.5(1) pm, R = 0.021 for 622 F and 46 V). The atomic positions of the lanthanoid and transition metal atoms are fully occupied. Significant deviations from the full occupancies were observed for two aluminum sites in TbM mAlio and for all five aluminum sites of the two rhenium-containing compounds, resulting in the compositions TbMn2Al9.63(2), CeRe2Al9.52(8), and SmRe2Al9.i6< 9)-The cell volume of CeRe2Alio and to a smaller extent also that of CeMm A1 io indicate mixed or intermediate +III/+IV valencies of the cerium atoms in these compounds. The structural relationships between the three closely related body-centered tetragonal structures of ThM ni2, CeMn-iAlx, DyFeöAU, and the primitive tetragonal structure of CaCnA lio are briefly discussed. 
  Reference    Z. Naturforsch. 53b, 673—678 (1998); received February 2 1998 
  Published    1998 
  Keywords    Intermetallic Compounds, Crystal Structure, X-Ray Data 
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 Identifier    ZNB-1998-53b-0673 
 Volume    53 
110Author    Bor-Jih Lee, Shigeo Kitsukawa, Hidemoto Nakagawa, Shukuji Asakura, Kenzo FukudaRequires cookie*
 Title    The Partial Oxidation of Methane to Methanol with Nitrite and Nitrate Melts  
 Abstract    The effect of reduced oxygen species on the partial oxidation of methane to methanol was examined with nitrite melts. The experimental results support the suggestion that the formation of methanol or C2 compounds depends on different reduced oxygen species, as observed in our previous work using nitrate melts. It has been suggested that the partial oxidation of methane proceeds to CH3OH or C2 compounds via parallel pathways. This suggestion was verified by increasing the oxygen concentration to carry out the partial oxidation of methane in 25 mol% NaNC>3 -75 mol% KNO3 melts. A methanol selectivity of 8.2% and a methanol yield of 0.43% were observed with CH4/O 2 = 15/1 at 575 °C, whereas with CH4/O 2 = 7/1 methanol selectivity and yield increased to 23.7% and 1.1%, respectively. The results further confirm the contribution of the superoxide ion O 2-on methanol formation. 
  Reference    Z. Naturforsch. 53b, 679—682 (1998); received February 26 1998 
  Published    1998 
  Keywords    Superoxide Ion, Nitrite, Nitrate, Partial Oxidation, Methanol 
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 Identifier    ZNB-1998-53b-0679 
 Volume    53 
111Author    JuliaA. Manskayaa, KonstantinV. Domasevitcha ', VeraV. Ponomareva2, Joachim Sielerb, VolodimirN. Kokozay2Requires cookie*
 Title    Crystal Engineering towards Design of Macrocyclic Coordination Compounds: Crystal Structure of Rubidium Tetrachloro-and Tetracyanoaurate(III) Complexes with 18-Crown-6  
 Abstract    The new macrocyclic complexes of composition Rb(18-crown-6)AuX4 (X = Cl (1) and CN (2)) have been prepared and characterized by X-ray crystallography (1: monoclinic, space group P2\/n, with a = 8.747(1), b = 8.366(1), c = 15.404(1) Ä; ß = 104.37(1)°, V = 1092.0(3) A , Z = 2; final R 1 =0.025 for 2030 independent reflections used; 2: monoclinic, space group P2\/c, with a = 14.765(3), 6 = 17.134(3), c = 8.855(2) k \ ß = 90.20(1)°, V = 2240.2(8) Ä3, Z = 4; final R 1 = 0.080 for 2034 independent reflections used). Both structures consist of Rb(18-crown-6)+ cations (A) and complex aurate(III) anions AuX4_ (B). Complex 1 has a linear polymeric array -A-B-A-B-(Rb-Cl 3.604(3), 3.654(3) Ä) with the rubidium ions disordered 0.276(2) A above and below the crown ether plane (Rb-O 2.819(5)-2.884(5) A, av. 2.846(5) A). The positioning of the rubidium atom away from the center of the 18-crown-6 is effected by the packing of the Rb(18-crown-6)+ and AuCU-moieties, and by the resemblance in the charge and symmetry of the cationic and anionic parts of the structure. Complex 2 has a zig-zag polymeric array -A-B-A-B-(Rb-N 2.92(2), 2.94(1) A) with orthogonal disposition of Rb(18-crown-6)+ and Au(CN)4-planes. The rubidium atom is situated 0.90(2) A above the mean plane of the macrocyclic oxygen atoms (Rb-O 2.93(5)-3.15(4) A) and adopts a typical "sunrise coordination". 
  Reference    Z. Naturforsch. 53b, 683—688 (1998); received January 5 1998 
  Published    1998 
  Keywords    18-Crown-6, Rubidium Macrocyclic Complexes, Gold(III), Crystal Structure 
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 Identifier    ZNB-1998-53b-0683 
 Volume    53 
112Author    Wolfgang Banße, Jana Fliegner, Stefan Sawusch, Uwe Schilde, Erhard UhlemannRequires cookie*
 Title    Dioxomolybdän(VI)-Komplexe mit dreizähnigen diaciden Liganden Dioxomolybdenum(VI) Complexes with Tridentate Diacidic Ligands  
 Abstract    Dioxomolybdenum(VI) complexes have been synthesized by ligand exchange reactions o f M o(CO)6, M o(NO)2(acac)2 and M o 0 2(acac)2 with tridentate diacidic ligands. X-ray structure analyses were performed on single crystals. The complexes salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (lb) and 2,2'-dihydroxy-azobenzenato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2) are isomorphous. In all chelates the Mo atom is in a distorted octahedral environment. Structural data: Salicylaldehyde-2-hydroxyanilato(2-)-tetrahydrofurane-dioxomolybdenum (VI) (la): a = 23.381(6) Ä, b = 6.756(2) A, c = 28.380(8) A, ß = 124.47(2)°; Salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum (VI) (lb): a = 9.4208(14) A, b = 30.550(5) A, c = 10.461(2) Ä, ß = 111.005(17)°; 2,2'-Dihydroxy-azobenzenato(2-o)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2): a = 9.392(2) A, b = 31.012(13) A, c = 10.350(2) Ä, /3 = 110.968(17)°; Salicylaldehyde-salicylhydrazonato(2-0)-triphenylphosphaneoxide-dioxomolybdenum(VI) (3): a = 9.321(2) A, b = 12.048(2) A, c — 13.858(3) A, a = 101.90(2)°, ß = 94.94(2)°, 7 = 105.479(17)°. 
  Reference    Z. Naturforsch. 53b, 689—693 (1998); eingegangen am 6. März 1998 
  Published    1998 
  Keywords    Ligand Exchange Reactions, Dioxomolybdenum(VI) Complexes, Tridentate Diacidic Ligands, Crystal Structure 
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 Identifier    ZNB-1998-53b-0689 
 Volume    53 
113Author    Martin Mutz, HansPeter LatschaRequires cookie*
 Title    Strukturuntersuchungen an DihaIogen(diphosphan)nickel-KompIexen in Lösung mit Differential-Puls-Polarographie Structure Analysis of Dihalogeno(diphosphine)nickel Complexes in Solution with Differential Puls Polarography  
 Abstract    Dihalogeno(diphosphine)nickel Complexes, NMR Data The structures of twelve dihalogeno(diphosphine)nickel complexes of the general formula [NiX2(PR'2R")2] (X = Cl, Br and I; R' resp. R" = -C2H 5 or -C6H5) were analyzed in solution by differential puls polarography and 1H-NMR spectroscopy as a function of temperature. 
  Reference    Z. Naturforsch. 53b, 694—698 (1998); eingegangen am 20. Februar 1998 
  Published    1998 
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 Identifier    ZNB-1998-53b-0694 
 Volume    53 
114Author    Abdel-Fattah Shihada, Frank WellerbRequires cookie*
 Title    Synthesis, Spectroscopic Studies, and Crystal Structure of Diethylchlorotin Dimethylphosphinate Et2C lSn02PMe2  
 Abstract    Diethylchlorotin dimethylphosphinate has been synthesized by treating (E tiC lS n^O with H02PMe2 in toluene. Single crystal X-ray analysis shows that Ü 2PM e2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The S n-C l bond lies on a C2 axis of symmetry in the (C2V) OCClSnCO unit. Et2ClSn02PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, /5 = 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSn0 2 PMe2 are assigned and the mass spectrum is reported and discussed. 
  Reference    Z. Naturforsch. 53b, 699—703 (1998); received December 29 1997 
  Published    1998 
  Keywords    Crystal Structure, IR Data, Mass Spectroscopic Data, Diethylchlorotin Dimethylphosphinate 
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 Identifier    ZNB-1998-53b-0699 
 Volume    53 
115Author    Michael Malchus, Martin JansenRequires cookie*
 Title    Studies on Tetramethylammonium Selenate(VI) and Chromate(VI)  
 Abstract    Tetramethylammonium Selenate(VI), Tetramethylammonium Chromate(VI), Crystal Structure, Vibrational Spectra, Thermal Analysis [N(CH3)4]2Se04 and [N tC H .^ h C rO j have been investigated by Infrared and Raman spec­ troscopy, coupled thermogravimetric and differential thermal analysis combined with mass spectroscopy of the evolved gases and temperature dependent X-ray diffraction. The crystal structure of [N(CH3)4]2Se04 has been determined from single crystal data (cubic, Fm3m. a -11.1077(7) A, Z = 4) and reveals [N(CH3)4]+ cations and SeC>42~ anions to be arranged in a LiiO -type of structure. While the cation framework of regular tetrahedra is orientationally fixed, the selenate anions are disordered. Powder diffraction data show [N(CH3)4]2Cr04 to be isostructural (cubic, Fm3m, a = 11,039(1) Ä, Z = 4). 
  Reference    Z. Naturforsch. 53b, 704—710 (1998); received March 5 1998 
  Published    1998 
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 Identifier    ZNB-1998-53b-0704 
 Volume    53 
116Author    Francoanellite K^alschpo^cpo, Stefan Dicka, Thomas ZeiskebRequires cookie*
 Title    Francoanellit K3A15HP04)6(P04)2*12H20: Struktur und Synthese durch topochemische Entwässerung von Taranakit-I 2 H2O: Structure and Synthesis by Topochemical Dehydration of Taranakite  
 Abstract    Single crystals of synthetic francoanellite K3Al5(HP0 4)6(P0 4)2-12H20 could be obtained for the first time by topochemical dehydration of taranakite crystals. An X-ray structure de­ termination showed francoanellite to be the mineral with the second longest crystallographic axis described hitherto. Crystal data: space group R3c, a = 869.0(2), c = 8227(1)pm, Z = 6 , R g = 0.042. Francoanellite is a layer structure mineral having six layers of composition [K3Al5(HP04)6(P04)2(H2 0)i2], connected by hydrogen bonds. The rigid layer is formed by columns of corner sharing hydrogen phosphate tetrahedra and AIOö-octahedra which are inter­ connected by additional six-coordinated A1 ions. In trigonal holes of the layer orthophosphate ions are situated. The structure of francoanellite is very similar to the structure of taranakite K3H6Al5(P04)8-18H20 which has planar water interlayers between the Al-phosphate layers. A neutron scattering experiment with subsequent Rietveld refinement of the powder pattern gave the H-atom positions. Hydrogen bonds in francoanellite are formed within the rigid layers and between them. During the reaction taranakite —► francoanellite crystals in an intermediate stage of dehy­ dration could be obtained. From the c-axis of 8858 pm and one-dimensional electron density projections it can be proposed that in these crystals every second water interlayer was lost and a first order staging product of the deintercalation of water from taranakite was formed. 
  Reference    Z. Naturforsch. 53b, 711—719 (1998); eingegangen am 2. März 1998 
  Published    1998 
  Keywords    Crystal Structure, Neutron Scattering, Francoanellite, Taranakite, Topochemical Reaction 
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 Identifier    ZNB-1998-53b-0711 
 Volume    53 
117Author    Norbert Kuhn, Joanna Fahl, Riad Fawzi, Cäcilia Maichle-Mößmer, Manfred SteimannRequires cookie*
 Title    Stable Carbene Adducts of Chlorine [1]  
 Abstract    The carbene adducts 3a-c (R 1 = Me, Et, iso-Pr; R2 = Me) are formed from the 2,3-dihydro-imidazol-2-ylidenes la-c and 1,2-dichloroethane as air-sensitive solids in good yields. The compounds exhibit a reactive Cl-Cl bond. Benzene is chlorinated by 3a,b to give chlorobenzene and the imidazolium salts 10a,b under mild conditions. 3c acts as a chloride donor to give with AICI3 and S 0 2 the 2-chloroimidazolium salts 12c andl3c (X = A1C14, S 0 2C1). On hydrolysis, the less reactive hydrate salt 14c is formed from 3c. The X-ray structures of 10a and 14c are reported. 
  Reference    Z. Naturforsch. 53b, 720—726 (1998); eingegangen am 23. Februar 1998 
  Published    1998 
  Keywords    Carbene, Chlorine, X-Ray Data 
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 Identifier    ZNB-1998-53b-0720 
 Volume    53 
118Author    Michael Schmidt, Andreas Bauer, Annette Schier, Hubert SchmidbaurRequires cookie*
 Title    Complexation of Beryllium(II) by Maleic and Succinic Acid  
 Abstract    Beryllium succinate dihydrate [Be(C4H404)](H20)2 is formed in the reaction of equimolar quantities of beryllium sulfate, succinic acid and barium hydroxide in aqueous solution at pH 3.2. Sodium, potassium, and ammonium bis(succinato)beryllates M 2[Be(C4H4C>4)2] are obtained using the same reagents in the molar ratio 1:2 :1 and adjusting the pH to 6.3-6.5 with NaOH, KOH or concentrated aqueous ammonia, respectively. The corresponding potassium bis(maleato)beryllate is prepared similarly and obtained as a crystalline monohydrate, the structure of which has been determined by X-ray methods. The lattice contains spiro-bicyclic dianions with the Be atom chelated by two dicarboxylate ligands. The compounds undergo slow hydrolysis in water as shown by time-and pH-dependent }Be NMR spectroscopy. In the neutral region (pH 6.5-6.9) the maleinato complexes are in an equilibrium with trinuclear compounds M 3{[Be(C4H204)0 H]3} as the predominating species, while in acid solution (at pH 1.3) only the aquo complex [Be(H20)4]2+ remains. In the intermediate pH region various complexes of the above types coexist, with only very slow ligand exchange (on the NMR time scale). 
  Reference    Z. Naturforsch. 53b, 727—733 (1998); received April 23 1998 
  Published    1998 
  Keywords    Beryllium(II), Maleic Acid, Succinic Acid, X-Ray Data 
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 Identifier    ZNB-1998-53b-0727 
 Volume    53 
119Author    JonesRequires cookie*
 Title    Polysulfonylamine, CV [1] Die ersten N,N-disulfonylierten Sulfinsäureamide: Synthese und Kristallstrukturen von R S ( 0 )-N (S 0 2Me)2 (R = Me, CC13)  
 Abstract    P o ly su lfo n y lam in es, C V [1] T h e F irst N ,N -D isu lfo n y lated S ulfinic A m id es: S y nthesis a n d C ry sta l S tru c tu re s o f R S (0) -N (S 0 2M e)2 (R = M e, CC13) M a rtin a N äv e k e, A rm a n d B lasc h ette* , P e te r G. The novel sulfinamides R S (0) -N (S 0 2M e)2, where R = Me (la) or CC13 (lb), were ob­ tained by treating the corresponding sulfinyl chlorides with Me3S iN (S 02Me)2 or AgN-(S 0 2Me)2, respectively. A presumedly ionic 1:1 adduct of lb with 4-dimethylaminopyridine was isolated and analytically characterized. In the crystals of la (monoclinic, space group P2\!ri) and lb (monoclinic, P l j c) , the molecules feature approximately planar NS3 moieties, unusually long S (0) -N bonds and, in the case of lb, an extremely long S (0) -C bond [for la and lb, in order: sum of bond angles at nitrogen 359.5 and 357.1°, S (0) -N 178.2(2) and 173.6(2) pm, S (0) -C 178.8(2) and 194.1(2) pm]. In both molecular structures, an attractive S (0) --0 1,4-interaction leads to a 7.3° discrepancy in the S (0) -N -S 0 2 angles. The crystal packing of la displays a tape (double-chain) motif generated by two prominent intermolecu-lar C -H -O interactions involving one M e S 0 2 group and the sulfinyl oxygen atoms of two adjacent molecules, whereas in lb the molecules are associated into parallel chains via a bonding C l-"0(sulfonyl) interaction. 
  Reference    Z. Naturforsch. 53b, 734—741 (1998); eingegangen am 6. April 1998 
  Published    1998 
  Keywords    N, N-Bis(organosulfonyl)sulfinamides, Synthesis, Crystal Structure, Long S ( 0 ) -N Bond 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0734.pdf 
 Identifier    ZNB-1998-53b-0734 
 Volume    53 
120Author    H. M. Öhrle, E. Tot, S. R. ÜdigerRequires cookie*
 Title    .2.3.4-Tetrahydroquinolines as Substrates for M annich C om pounds  
 Abstract    A m inals, Im inium Salts, C-and N -A m in om eth ylation s, N aphthols The product o f the reaction o f 1,2,3,4-tetrahydroquinoline (1) w ith 2-naphthol (2) and form aldehyde reported as the N -substitu ted tetrahyd roq uinoline 3 sh ow s really the structure o f the ph en ylogous bis-substituted tetrahyd roq uinoline 4. The function o f 1, 6 -m eth y l-l,2,3,4-tetrahydroquinoline (9) and l-m eth yl-l,2 ,3 ,4 -tetra h y d ro q u in o lin e (17) as am ines or C -nucleo-philic com poun ds in M annich con d en sation s w ere exam in ed . 
  Reference    Z. Naturforsch. 53b, 742 (1998); ein gegan gen am 6. Mai 1998 
  Published    1998 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0742.pdf 
 Identifier    ZNB-1998-53b-0742 
 Volume    53 
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