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1996[X]
1Author    Srb^sioogThomas Berger, Klaus-Jürgen RangeRequires cookie*
 Title    Hochdrucksynthese und Strukturverfeinerung von Strontium-Danburit, SrB2Si20 8 High-Pressure Synthesis and Structure Refinement of Strontium Danburite  
 Abstract    of strontium danburite, SrB2Si20 8, were found after high-pressure treatment of SrSi03/Si02/Al20 3 mixtures at 40 kbar and 1400°C, obviously formed by an unwanted side reaction with the boron oxide-containing boron nitride capsules used. The crystals are orthorhombic, space group Pnma, with a = 8.1891 (5), b = 7.9311 (6), c = 8.9284(5) A and Z = 4. The structure was refined to R = 0.031, Rw = 0.028 for 590 independent, absorption-corrected reflections. SrB2Si20 8 is isostructural with danburite (CaB2Si20 8). The structure comprises a tetrahedral framework of ordered B20 7 and Si2Ov groups which contains Sr in irregular coordination. Die Kristallstruktur des seit 1839 bekannten Dan-burits, CaB2Si20 8, wurde 1931 von Dunbar und Machatschki [1] bestimmt und später von Johann-son [2], Bakakin, Kravchenko und Belov [3] sowie von Phillips, Gibbs und Ribbe [4] verfeinert. Ob­ wohl Dunbar und Machatschki die Positionen der Boratome nur ungenau festlegen konnten, haben sie das Grundprinzip der Danburitstruktur korrekt be­ schrieben; es liegt ein dreidimensionales Netzwerk aus geordnet verteilten, eckenverknüpften B20 7-und Si20 7-Gruppen vor, das die Ca-Atome in irre­ gulärer Koordination durch Sauerstoff enthält. Eine 1'B-NMR-Studie von Brun und Ghose [5] belegt, daß die geordnete B-Si-Verteilung in Danburit bis zu dessen Zersetzungstemperatur erhalten bleibt. Während also CaB2Si2Ö 8 strukturell gut charak­ terisiert ist, lagen von der homologen Verbindung SrB2Si20 8 bisher nur Pulverdaten vor. SrB->Sio08 wurde erstmals von Verstegen et al. erwähnt, die die Lumineszenz der Eu-aktivierten Verbindung un­ tersuchten [6]. Auf sie geht auch die Bestimmung der Zellparameter zurück. Aufgrund der vermute­ ten Ähnlichkeit zum Danburit schlugen Verstegen et al. [6] für SrB2Si2Og den Namen Strontium-Dan-burit vor. Eine weitere Erwähnung der Verbindung SrB2Si20 8 erfolgt bei Baylor und Brown [7], die Phasengleichgewichte im ternären System SiCX-B20 3-Sr0 untersuchten. * Sonderdruckanforderungen an Prof. Dr. K.-J. Range. 
  Reference    Z. Naturforsch. 51b, 172—174 (1996); eingegangen am 20. Juli 1995 
  Published    1996 
  Keywords    Stontium Danburite, High-Pressure Synthesis, Crystal Structure Single crystals 
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 Identifier    ZNB-1996-51b-0172 
 Volume    51 
2Author    D. Frerichs, C. H. Park, Hk Müller-BuschbaumRequires cookie*
 Title    Zur Kenntnis der Tief-und Hochtemperaturform eines Oxidarsenats des Zinks: Zn0Z n3(A s0 4)2 On the Low and High Temperature Form o f an Oxidearsenate of Zinc: Z n 0 Z n 3( A s 0 4)2  
 Abstract    Single crystals of the low (t-) and high (h-) temperature form o f Z n 0 Z n 3(A s 0 4)2 have been prepared by flux and by C 0 2-L A SER techniques respectively. Both compounds crystal­ lizes monoclinic, space group C2h-P2;/n with the lattice parameters t-Z n 0 Z n 3(A s 0 4)2: a = 9.807(3), b = 8.180(2), c = 9.967(2) A , ß = 116.53(2)°, Z = 4 and h -Z n 0 Z n 3(A s 0 4)2: a = 9.743(3), b = 8.163(8), c = 17.933(2) A , ß = 91.55(2)°, Z = 8. Similarities and differences of the crystal structures will be discussed. 
  Reference    Z. Naturforsch. 51b, 233 (1996); eingegangen am 10. Juli 1995 
  Published    1996 
  Keywords    Zinc, Arsenic, Oxide, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0233.pdf 
 Identifier    ZNB-1996-51b-0233 
 Volume    51 
3Author    Silke Busche, K. Arsten BluhmRequires cookie*
 Title    Synthese und Kristallstruktur von Dibariumzink-bis(cyclotriborat) Ba2Zn(B30 6)2  
 Abstract    Single crystals of the new compound Ba2Zn(B30 6)2 were obtained by using a B20 3 flux technique. They crystallize in an as yet unknown structure type. X-ray investigations led to space group Cj'-Pl (Nr.2) with lattice parameters a = 715.5(2), b = 720.5(2), c = 1178.9(4), a = 78.96(2)°, /3 = 85.45(2)°, j = 60.12(1)°, Z = 2. The structure is characterized by iso­ lated (B30 6)3_-rings and contains two ninefold coordinated Ba-sites. Zn2+ is tetrahedrally coordinated by oxygen. The relation to the crystal structures of high-temperature BaB20 4 and Ba2Ca(B30 6)2 is discussed. 
  Reference    Z. Naturforsch. 51b, 309—312 (1996); eingegangen am 26. September 1995 
  Published    1996 
  Keywords    Barium, Zinc, Borate, Crystal Structure 
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 Identifier    ZNB-1996-51b-0309 
 Volume    51 
4Author    Karl Peters3, Eva-Maria Peters3, Gerhard Bringmannb, Sven HarmsenbRequires cookie*
 Title    l,4-Dibromonaphthalene-2,3-diyI- bis(l'-bromo-2'-naphthoate) * CHC13, a Potential Precursor to Lactone-Bridged Teraryls  
 Abstract    The title compound was prepared from 1,4-di-bromo-2,3-dihydroxynaphthalene by two-fold es-terification with l-bromo-2-naphthoic acid. It crystallizes from chloroform in the triclinic sys­ 
  Reference    Z. Naturforsch. 51b, 144—146 (1996); received June 20 1995 
  Published    1996 
  Keywords    Crystal Structure, Biaryl Coupling, Teraryls 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0144_n.pdf 
 Identifier    ZNB-1996-51b-0144_n 
 Volume    51 
5Author    D. Frerichs, C. H. Park, HkM. Üller-B, UschbaumRequires cookie*
 Title    Zur Kenntnis zweier Formen des Zinkorthoarsenates: a-Z n 3(A s04)2 und /3-Zn3(A s0 4)2 On Two Forms o f Zinc O rthoarsenate: a -Z n 3(A s 0 4)2 and /3-Zn3(A s 0 4)2  
 Abstract    Single crystals of two forms of zinc orthoarsenate (a-Z n3(A s04)2 (I) and /3-Zn3(A s04)2 (II)) have been prepared by flux techniques. Both compounds crystallize monoclinically, space groups (I): Cih-P2l/c, (II): Cih-P21/n, with the lattice parameters (I): a = 6.306(2), b = 8.652(2), c = 'ol 1.321(4) A, ß = 92.25(5) °, Z = 4 and (II): a = 5.281(1), b = 8.494(2), c = 7.726(3) A, ß = 96.39(3)°, Z = 2. ct-Zn3(A s04)2 is isotypic to I-Cu3(A s04)2 and ß-Zn3(A s04)2 to 7-Zn3(P 0 4)2. Similarities and differences of the crystal structures are discussed. 
  Reference    Z. Naturforsch. 51b, 333—337 (1996); eingegangen am 31. August 1995 
  Published    1996 
  Keywords    Zinc, Arsenic, Oxide, Crystal Structure 
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 Identifier    ZNB-1996-51b-0333 
 Volume    51 
6Author    Karl Peters3, Eva-M Aria Peters3, G.Erhard Bringmannb, O. La, F. SchuppbRequires cookie*
 Title    l,3-Dimethoxy-677- benzo[b]naphtho[l,2-d]pyran-6-thione, a Thionolactone-Bridged Axially Prostereogenic Biaryl  
 Abstract    The title compound was prepared from the cor­ responding " ordinary" oxolactone bridged biaryl using Lawesson's reagent. It crystallizes from di-chloromethane / petroleum ether in the mono­ clinic system, space group P2xla; a = 1115.7(2), 
  Reference    Z. Naturforsch. 51b, 431—432 (1996); received September 9 1995 
  Published    1996 
  Keywords    Crystal Structure, Stereochemistry, Biaryl Coupling 
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 Identifier    ZNB-1996-51b-0431_n 
 Volume    51 
7Author    J. Feldmann, Hk Müller-BuschbaumRequires cookie*
 Title    Kristallstrukturuntersuchung am Barium-Yanadyl-Vanadat: Ba2(V 0)V 20 8 Crystal Structure Investigation of the Barium Vanadyl-Vanadate: Ba2(V 0 )V 20 8  
 Abstract    Single crystals of Ba2(V 0)V 20 8 have been prepared by solid state reactions of Ba2V 20 7, V 9O 1 and V ^ 05 in sealed silica tubes. This compound crystallizes with monoclinic symmetry, space group C 1 -P 2 ,, a = 8.1174(9), b = 5.9699(9), c = 9.2903(9) A , ß = 113.94(1)°, Z = 2. V 5+ shows tetrahedral coordination. V 4+ inside ^ [V (3)0 4] chains is characterized by a square pyramidal coordination with a short apical V-O distance of 1.6 A typically for vanadyl groups. Ba2(V 0)V 20 8 represents a new structure type and is not isotypic to Sr2(V 0)V 20 8. 
  Reference    Z. Naturforsch. 51b, 489—4 (1996); eingegangen am 22. August 1995 
  Published    1996 
  Keywords    Barium, Vanadium, Oxide, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0489.pdf 
 Identifier    ZNB-1996-51b-0489 
 Volume    51 
8Author    Rolf Minkwitz, RaimUnd Bröchler, Hans PreutRequires cookie*
 Title    Low-Temperature Crystal Structure of the Inclusion Compound {[N(CH3)4+C1]2] * CH 3CN * h 2o  
 Abstract    The crystal structure of {[N(CH3)4+C1]2}-CFI3C N H 20 is reported. Cry-stalls are orthorhombic, space group Pnma, with a = 1622.9(15), b = 671.3(6), c = 1511.2(11) pm, V = 1646(2) 106 pm3 and Z = 4. 
  Reference    Z. Naturforsch. 51b, 599—601 (1996); eingegangen am 3. August 1995 
  Published    1996 
  Keywords    Preparation, Crystal Structure, Inclusion Compound 
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 Identifier    ZNB-1996-51b-0599_n 
 Volume    51 
9Author    Na2z, New Sodium, ZincateD. Trinschek, M. JansenRequires cookie*
 Title    Na2Zn02, ein neues Natriumzinkat  
 Abstract    By reacting Na20 , which was produced in situ from NaN3 and NaN02, with reactive ZnO in the solid state, the synthesis of Na2Z n02 has been achieved. Na2Zn02 is metastable up to about 750°C. The novel sodium zincate crystallizes in the spaceogroup P2,/c (No. 14) with the lattice parameters a = 7.7352(2), b = 5.9782(2), c = 5.7248(2)Ä, ß = 94.934(3)°, Z = 4. According to a single crystal structure determination it is an representative of the anti type of the Ln2S20 (Ln = Er, Tm, Yb, Dy) structure. 
  Reference    Z. Naturforsch. 51b, 711—714 (1996); eingegangen am 10. August 1995 
  Published    1996 
  Keywords    Sodium Zincates, Crystal Structure, Metastability 
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 Identifier    ZNB-1996-51b-0711 
 Volume    51 
10Author    Z. NaturforschRequires cookie*
 Title    A -P r 2S3, D -H o2S3 und E -Y b 2S3: Synthese und Einkristallstrukturuntersuchungen  
 Abstract    The oxidation of reduced chlorides (MC12) or chloride-hydrides (MC1HV) of the lanthani­ des with sulfur (700-850 °C, 7 d, sealed tantalum capsules or evacuated silica vessels) usually results in the formation of the sesquisulfides M2S3 as the main products. In the presence of appropriate fluxes (e.g., alkali halides), the products often are obtained as single crystals, and the flux decides which modification is favoured. Ternary halides of the trivalent lanthanides with the corresponding alkali metal can mostly be found as the second components. Crystal growth and structural investigations of thus produced single crystals of Pr2S3 (from PrClH() 67 + S + NaCl, 5:5:1, A type: orthorhombic, Pnma (No. 62), Z = 4, a = 748.22(5), b = 405.51(3), c = 1560.74(9) pm, R = 0.024, Rw = 0.020), Ho^S, (from U -H o^S , + KI, 1:1, D type: mono­ clinic, P 2xim (No. 12), Z = 6, a = 1746.15(9), b = 400.23(3), c = 1012.43(6) pm, ß = 98.529(4)°, R = 0.041, Rw = 0.035), and YbiS3 (from T-Yb^S^ + KI, 1:1, E type: trigonal, R 3c (No. 167), Z = 6, a = 674.97(2), c = 1820.11(9) pm'. R = 0.019, Rw = 0.018) are reported here. In accordance with the lanthanide contraction, the trivalent cations (M3+) exhibit sulfur coordination numbers of 7 and 8 in A -P r 2S3, 6 and 7 in D -H o 2S3, and 6 in E -Y b 2S3 (corundum-type structure). 
  Reference    Z. Naturforsch. 51b, 733—738 (1996); eingegangen am 4. Oktober 1994 
  Published    1996 
  Keywords    Lanthanides, Sesquisulfides, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0733 
 Volume    51 
11Author    H. V., A. Fischerb, P. G. JonesbRequires cookie*
 Title    Eine unerwartete Synthese des Triphenyphosphazenium-chlorids, [(C6H5)3PNH2]+CI_ und eine Neubestimmung seiner Kristallstruktur  
 Abstract    Triphenylphosphazenium chloride has been prepared by the reaction of triphenylphos-phine with trimethylsilylazide in impure, wet dichloromethane. Yields are improved as stoi­ chiometric quantities of w ater are added. Colourless crystals are obtained by recrystallization from the same solvent. The crystals are triclinic, space group P I, Z=2, a = 894,6(3), b -979,8(3), c = 1142,9(4) pm, a = 107,27(3), ß = 93,70(3), y = 92,97(3)°. In the solid state the compound exists as [(C6H 5)3PNH2]+ cations, and Cl-anions. Dimeric units are formed by H-bonding. The crystal structure contains one molecule CH 2C12 per one molecule (C6H 5)3PNH2C1. The cation has a slightly irregular tetrahedral geometry around the P-atom with a relatively short P-N bond. 
  Reference    Z. Naturforsch. 51b, 865—868 (1996); eingegangen am 21. O ktober 1995 
  Published    1996 
  Keywords    Triphenylphosphazenium Chloride, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0865 
 Volume    51 
12Author    N. Stock, W. SchnickRequires cookie*
 Title    Synthese, Kristallstruktur und Eigenschaften von l,l>3 ?3 ?3 -Pentaam*n° -l  
 Abstract    oxo-lA 5 ,3A 5 -diphosphaz-2-en, (NH2)2 (0)P-N=P(NH2)3 Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaam ino-l-oxo-l A 5 , 3 A 5 -diphosphaz-2-ene, (NH2)2(0)P-N =P(N H i)3 Coarse crystalline (NH2)2(0)P-N=P(NH2)3 is obtained from a NH;* saturated CH2C12 suspen­ sion of (NH2)2(0)P-N=P(NH2)3 NH4C1 at room temperature. (NH2)2(0)P-N=P(NH2)3 NH4C1 is synthesized" by slow addition of C12(0)P-N=PC13 to a solution of NH3 in CH2C12 at -78 °C. Excess NH4C1 is removed by treatment with HNEt2 followed by extraction with CH2C12. The crystal structure of (NH2)2(0)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P2(/c; a = 1462.8(3), b = 944.8(2), c = 1026.9(2) pm, /3 = 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H- • N > 313 pm. N-H • 0 > 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80 °C. 
  Reference    Z. Naturforsch. 51b, 1079—1083 (1996); eingegangen am 7. Dezember 1995 
  Published    1996 
  Keywords    Aminophosphazene, Synthesis, Crystal Structure Precursor 
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 Identifier    ZNB-1996-51b-1079 
 Volume    51 
13Author    Wolfgang Czado, Ulrich MüllerRequires cookie*
 Title    (PPh4)4Sb8Br28 Tetraphenylphosphonium Ikosioctabromooctaantimonate(III), (PPh4)4Sb8Br28  
 Abstract    The title compound was obtained by the reaction of PPh4Br, Sb2Se3, and bromine in dichloro-methane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1249.1(2), b = 1307.8(2), c = 2152.3(4) pm, a = 102.93(2), ß = 100.83(2), 7 = 100.42(2)°, Z = 2, triclinic, space group P I . (PPh4)4Sb8Br28 is isotypic with (PPh4)4Sb8I28. The Sb8Br284~ ion can be taken as the association product of eight SbBr3 molecules with four B r-ions. Each Sb atom has a distorted octahedral coordination with three shorter (252 to 274 pm) and three longer (300 to 353 pm) Sb-Br bonds. The octahedra share common edges in two parallel rows of four octahedra each. The arrangement of the 28 bromine atoms corresponds to a section of a closest packing of spheres. Tetraphenylphosphonium-ikosioctabromooctaantimonat(III), 
  Reference    Z. Naturforsch. 51b, 1245—1247 (1996); eingegangen am 22. März 1996 
  Published    1996 
  Keywords    Ocataikosabromooctaantimonate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1245 
 Volume    51 
14Author    Joachim Pickardt, B. Ritta KühnRequires cookie*
 Title    Metallkomplexe mit Guanidinderivaten als Liganden  
 Abstract    Kristallstrukturen von [Zn(cnge)2(SCN)2] 2H20 und Zn(eoge)Br2 (enge = Cyanoguanidin; eoge = 1-Ethoxyiminomethylguanidin) M etal C om plexes with G uanidine D erivatives as Ligands: Crystal Structures o f [Zn(cnge)2(SC N)2]-2H20 und Z n(eoge)B r2 (cnge = C yanoguanidine; eoge = 1-Ethoxyim inom ethylguanidine) Crystals of |Zn(cnge)2(SCN)2]-2H20 (1) were obtained by evaporation of an aqueous solution 
  Reference    Z. Naturforsch. 51b, 1469—1472 (1996); eingegangen am 3. April 1996 
  Published    1996 
  Keywords    Cyanoguanidine, Zinc Complexes, Crystal Structures 
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 Identifier    ZNB-1996-51b-1469 
 Volume    51 
15Author    StefanH. Orstm, AnnW. Olfgang SchnickRequires cookie*
 Title    Synthese  
 Abstract    , K rista llstru k tu r und Eigenschaften von 1 ,1 , 1 > 3 * 3 , 3 -H e x a a m i n o -lA 5,3A5-diphosphazenium ehlorid[(N H 2)3PNP(NH2)3]Cl Synthesis, C rystal Structure, and Properties of 1,1,1,3,3,3-Hexaam ino-1 A5,3A5-diphosphazenium Chloride [(N H 2)3PN P(N H 2)3]C1 [(NH2)3PNP(NH2)3 ]C1 has been prepared by a three step synthesis. The last step is the ammo-nolysis of [C13PNPC13]C1. Single crystals of 1,1,1,3,3,3-hexaamino-1 A \ 3As-diphosphazenium chloride were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. Between room temperature and -1 0 0 °C [(NH2)3PNP(NH2)3]C1 is sub­ ject to a phase transition. Therefore, the crystal structure was determined by single crystal X-ray methods at room temperature (P i, a = 584.7(1) pm, b = 732.1(1) pm, c = 1092.0(2) pm. q = 71.05(3)°, ß = 76.36(3)°, 7 = 89.83(3)°, Z = 2, R = 4.75 %, wR = 2.47 %). The cation [(NH2)3PNP(NH2)3]+ is built up by two corner sharing PN4 tetrahedra. Remarkably short P-N bonding distances have been observed and both PN4 tetrahedra exhibit a significant distortion resulting in two large and four small N-P-N bond angles. 
  Reference    Z. Naturforsch. 51b, 1732—1738 (1996); eingegangen am 26. Juni 1996 
  Published    1996 
  Keywords    Aminophosphazenes, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1732 
 Volume    51 
16Author    G. Rebe, Frank Weller, Kurt Dehnicke, ProfRequires cookie*
 Title    Jutta  
 Abstract    N-Iodo-triphenylphosphaneimine, Ph3PNI, has been prepared by thermolysis of the donor acceptor complex [Me3SiNPPh3-ICl] in boiling acetonitrile in the presence of potassium fluo­ ride. Both compounds have been characterized by IR spectroscopy and by crystal structure determinations. [Me3SiNPPh3 ICl]: Space group P I, Z = 2, a = 888.3(1), b = 1070.7(1), c = 1310.2(1) pm, a = 9 5 .15(1)°, ß = 108.67(1)°, 7 = 97.78(1)° at 20°C. The complex has a molecular structure in which the N atom of the phosphaneimine is connected with the iodine atom of the IC1 molecule in a linear arrangement N-I-Cl with bond lengths N-I = 232.7 pm, I-Cl = 255.37 pm. Ph3PNI: Space group P2,/n, Z = 4, a = 952.8(1), b = 1800.8(2), c = 1003.6(1) pm, ß = 110.25(1)° at -50°C. The compound forms monomeric molecules with bond lengths PN = 159.1 pm, I-N = 205.6 pm and an INP bond angle of 113.3°. N-Iod-triphenylphosphanimin. Synthese und Kristallstrukturen von [Me3SiNPPh3 ICl] und Ph3PNI 
  Reference    Z. Naturforsch. 51b, 1739—1743 (1996); eingegangen am 12. April 1996 
  Published    1996 
  Keywords    Phosphaneimine Complexes, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1739 
 Volume    51 
17Author    Ute Berger, Wolfgang SchnickRequires cookie*
 Title    Ba2Na(CN2)(CN)3, ein neues Cyanamid-cyanid mit interpenetrierenden Teilstrukturen Ba2Na(CN2)(CN)3, a Novel Cyanamide Cyanide with Interpenetrating Substructures  
 Abstract    Ba2Na(CN2)(CN)3 was obtained by the reaction of Ba2N with melamine and NaCN at 700 °C. The compound was structurally characterized by single-crystal X-ray investigations (Fd3m, a = 1518.8(3) pm, Z = 16). In the crystal structure the Ba"+ ions form a cubic close packed arrangement, the Na+ and the CN2_ ions occupy the octahedral interstices. The CN-ions are located within the close packed Ba2+ layers. The unit cell of Ba2Na(CN2)(CN)3 contains two interpenetrating substructures of the zinc-blende structure type, building up a variant of NaTl. A reversible phase transition has been observed during cooling of the compound. Whereas the Ba2(CN2)(CN)3 sublattice remains nearly unaffected in this process, the Na+ ions of the low-temperature phase are statistically distributed on two crystallographic positions. 
  Reference    (Z. Naturforsch. 51b, 1—8 [1996]; eingegangen am 7. Juni 1995) 
  Published    1996 
  Keywords    Cyanamide Cyanides, Synthesis, Crystal Structure, Vibrational Spectra 
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 Identifier    ZNB-1996-51b-0001 
 Volume    51 
18Author    E. Kemnitz3, C. Werner3, A. Stiewe3, H. Worzalab, S. Trojanov3Requires cookie*
 Title    Synthese und Struktur von Zn(HS0 4)2(H2S0 4)2 und Cd(H S04)2 Synthesis and Structure of Z n(H S04)2(H2S 0 4)2 and C d(H S 04)2  
 Abstract    From the binary systems M2S 0 4/H2S 0 4 (M = Zn, Cd), two new hydrogen sulfates, (Zn(HS0 4)2(H2S04)2 and Cd(HS04)2, have been synthesized and structurally characteri­ zed. Both compounds crystallize in the monoclinic space group P2,/c with cell parameters a = 5.047(2), b = 15.430(4), c = 7.958(3) A and ß = 104.16(4)° (Z= 2) for Zn(HS04)2(H2S 0 4)2 and a = 5.339(1), b = 13.351(3), c = 8.508(2) A and ß = 92.22(3)° (Z = 4) for Cd(H S04)2. In the zinc compound there are slightly distorted centrosymmetric Z n 06 octahedra with Z n -0 distances of 2.05 -2.13 A which are sharing corners with S 0 4 tetrahedra. H S 04 and H2S 0 4 tetrahedra are linked via hydrogen bonds to form layers perpendicular to the c-axis. In the crystal structure of C d(HS04)2there exist two crystallographically different H S 04 tetrahedra. The C d06 octahedra with C d -0 distances between 2.24 and 2.31 A are strongly angle-distorted. Besides hydrogen bonds of medium strength (d0...o = 2.66 A) there are also much more weaker ones (d0...0 = 3.04 A). Considering these latter ones zigzag chains in z-direction can be recognized. The relatively low stability of Cd(H S04)2 in comparison with other metal-II-hydrogen sulfates is discussed with respect to its structural pecularities. 
  Reference    (Z. Naturforsch. 51b, 14—18 [1996]; eingegangen am 13. Juni 1995) 
  Published    1996 
  Keywords    Synthesis, Crystal Structure Zinc, Cadmium, Hydrogen Sulfate 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0014.pdf 
 Identifier    ZNB-1996-51b-0014 
 Volume    51 
19Author    S. Trojanov, A. Stiewe, E. KemnitzRequires cookie*
 Title    Synthese und Struktur saurer Ubergangsmetallsulfate - Ti(H50 2)(S 0 4)2(H20 ) 2 und Zr(H30 ) 2(S 0 4)3 Synthesis and Structure of Acid Transition Metal Sulfates - Ti(H50 2)(S 0 4)2(H20 )2 and Zr(H30 ) 2(S 0 4)3  
 Abstract    From the ternary system Mn(S 0 4)n/2 / S 0 3 / H20 (Mn+ = Zr4+, Ti3+) two new acid metal sulfates, Ti(H50 2)(S 0 4)2(H20)2 and Zr(H30) 2(S 0 4)3, have been synthesized and structurally characterized. Ti(H50 2)(S 0 4)2(H->0)i crystallizes in the orthorhombic space group Pnma with cell parameters a = 9.858(5), b = 18.32(2), c = 5.437(7)Ä (Z = 4); Zr(H30) 2(S 0 4)3 crystallizes in the triclinic space group PI with cell parameters a = 5.092(2), b = 8.533(3), c = 12.388(6)A, a = 92.95(3)°, ß = 90.89(3)°, 7 = 94.35(3)° (Z= 2). In the titanium compound there are slightly distorted T i0 6 octahedra with T i-0 distances between 1.99 and 2.09 A which are sharing corners with S 0 4 tetrahedra. Through hydrogen bonds layers are formed perpendicular to the 6-axis. These layers are connected by H30 + ions only. The structure of Zr(H30) 2(S 0 4)3 consists of three different S 0 4 tetrahedra and distorted Zr07 polyhedra which are connected via common corners and edges to form columns parallel to the a-axis. The Z r-0 distances vary from 2.13o to 2.18A for equatorial positions, significantly longer than the axial Zr-O distances with 2.05A. 
  Reference    (Z. Naturforsch. 51b, 19—24 [1996]; eingegangen am 13. Juni 1995) 
  Published    1996 
  Keywords    Synthesis, Crystal Structure, Titanium, Zirconium, Hydrogen Sulfates 
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 Identifier    ZNB-1996-51b-0019 
 Volume    51 
20Author    D. Frerichs, Hk Müller-BuschbaumRequires cookie*
 Title    Vier verschiedene Koordinationspolyeder um Cu2+ im Oxid-Arsenat-Phosphat Cu0  
 Abstract    (Cu,M g)3(As1_xPJt:0 4)2 (x = 0,3) Four Different Coordination Polyhedra Around Copper in the Oxide-Arsenate-Phosphate C u0(C u,M g)3(A s,_xP,.04)2 (x = 0.3) Single crystals of CuO(Cu,Mg)3[(As0.7P0.3)O4]2 have been prepared by crystallization from melts. The compound crystallizes with triclinic symmetry, space group C '-P l, a = 6.372(4), b = 7.643(7), c = 8.175(5) A, a = 98.59(6), ß = 112.26(3), 7 = 99.03(3)°, Z = 2. CuO(Cu,Mg)3[(Aso)7Po 3)0 4]2 is isotypic to Cu4(P 0 4)20 . X-ray investigations show square planar C u 04 polygons, twisted tetragonal C u 0 5 pyramids, C u 05 bipyramids and elongated (Cu,M g)06 octahedra. 
  Reference    (Z. Naturforsch. 51b, 25—28 [1996]; eingegangen am 27. Juli 1995) 
  Published    1996 
  Keywords    Copper, Magnesium, Arsenate, Phosphate, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0025.pdf 
 Identifier    ZNB-1996-51b-0025 
 Volume    51 
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