| 1 | Author
| Srb^sioogThomas Berger, Klaus-Jürgen Range | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0172.pdf | | | Identifier
| ZNB-1996-51b-0172 | | | Volume
| 51 | |
2 | Author
| Karl Peters3, Eva-Maria Peters3, Gerhard Bringmannb, Sven Harmsenb | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0144_n.pdf | | | Identifier
| ZNB-1996-51b-0144_n | | | Volume
| 51 | |
3 | Author
| D. Frerichs, C. H. Park, Hk Müller-Buschbaum | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0233.pdf | | | Identifier
| ZNB-1996-51b-0233 | | | Volume
| 51 | |
4 | Author
| Silke Busche, K. Arsten Bluhm | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0309.pdf | | | Identifier
| ZNB-1996-51b-0309 | | | Volume
| 51 | |
5 | Author
| D. Frerichs, C. H. Park, HkM. Üller-B, Uschbaum | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0333.pdf | | | Identifier
| ZNB-1996-51b-0333 | | | Volume
| 51 | |
6 | Author
| Karl Peters3, Eva-M Aria Peters3, G.Erhard Bringmannb, O. La, F. Schuppb | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0431_n.pdf | | | Identifier
| ZNB-1996-51b-0431_n | | | Volume
| 51 | |
7 | Author
| J. Feldmann, Hk Müller-Buschbaum | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0489.pdf | | | Identifier
| ZNB-1996-51b-0489 | | | Volume
| 51 | |
8 | Author
| Rolf Minkwitz, RaimUnd Bröchler, Hans Preut | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0599_n.pdf | | | Identifier
| ZNB-1996-51b-0599_n | | | Volume
| 51 | |
9 | Author
| Na2z, New Sodium, ZincateD. Trinschek, M. Jansen | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0711.pdf | | | Identifier
| ZNB-1996-51b-0711 | | | Volume
| 51 | |
10 | Author
| Z. Naturforsch | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0733.pdf | | | Identifier
| ZNB-1996-51b-0733 | | | Volume
| 51 | |
11 | Author
| H. V., A. Fischerb, P. G. Jonesb | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0865.pdf | | | Identifier
| ZNB-1996-51b-0865 | | | Volume
| 51 | |
12 | Author
| N. Stock, W. Schnick | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-1079.pdf | | | Identifier
| ZNB-1996-51b-1079 | | | Volume
| 51 | |
13 | Author
| Wolfgang Czado, Ulrich Müller | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-1245.pdf | | | Identifier
| ZNB-1996-51b-1245 | | | Volume
| 51 | |
14 | Author
| Joachim Pickardt, B. Ritta Kühn | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-1469.pdf | | | Identifier
| ZNB-1996-51b-1469 | | | Volume
| 51 | |
15 | Author
| StefanH. Orstm, AnnW. Olfgang Schnick | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-1732.pdf | | | Identifier
| ZNB-1996-51b-1732 | | | Volume
| 51 | |
16 | Author
| G. Rebe, Frank Weller, Kurt Dehnicke, Prof | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-1739.pdf | | | Identifier
| ZNB-1996-51b-1739 | | | Volume
| 51 | |
17 | Author
| Ute Berger, Wolfgang Schnick | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0001.pdf | | | Identifier
| ZNB-1996-51b-0001 | | | Volume
| 51 | |
18 | Author
| E. Kemnitz3, C. Werner3, A. Stiewe3, H. Worzalab, S. Trojanov3 | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0014.pdf | | | Identifier
| ZNB-1996-51b-0014 | | | Volume
| 51 | |
19 | Author
| S. Trojanov, A. Stiewe, E. Kemnitz | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0019.pdf | | | Identifier
| ZNB-1996-51b-0019 | | | Volume
| 51 | |
20 | Author
| D. Frerichs, Hk Müller-Buschbaum | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0025.pdf | | | Identifier
| ZNB-1996-51b-0025 | | | Volume
| 51 | |
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