| 3 | Author
| Z. Naturforsch | Requires cookie* | | Title
| Über Sulfide und Oxidsulfide des Samariums  | | | Abstract
| Stoichiometric oxidation o f SmCl2 with sulfur in the presence o f NaCl (evacuated silica ves sel, 850 °C, 7 d) results in the formation o f A -S m -,S 3 (orthorhombic, Pnma (no. 62), a = 737.64(5), b = 397.44(3), c = 1536.26(9) pm, Z = 4, /?w = 0.017). In contrast, C ~ S m 2S3 (cubic, I4 3 d (no. 220), a = 844.71(3) pm, Z = 5.333, Rw = 0.017) is obtained upon reaction o f the | | |
Reference
| Z. Naturforsch. 47b, 1614 (1992); eingegangen am 1. Juli 1992 | | |
Published
| 1992 | | |
Keywords
| Samarium, Sulfides, Oxysulfides, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-1614.pdf | | | Identifier
| ZNB-1992-47b-1614 | | | Volume
| 47 | |
4 | Author
| A. Dalbert Lossin, Gerd Meyer, R. Obert Fuchs, Joachim Strähle | Requires cookie* | | Title
| [Sm(CH3C 0 0 )3 (H 20)2] * CH 3COOH, ein Essigsäureaddukt des Samarium(III)-acetatdihydrates [Sm(CH3C0 0 )3(H 20 )2] * CH 3COOH, an Acetic Acid Adduct o f Sam arium (III) Acetate Dihydrate  | | | Abstract
| The crystal structure o f the acetic acid adduct o f the so far unknown samarium(III) acetate dihydrate was determined from single-crystal four-circle diffractometer data. It has the com position [Sm (CH 3C 0 0)3 (H 20) 2] C H 3C 0 0 H containing {[Sm (CH3C 0 0)3 (H 20) 2]}2 dimers and crystallizes in the trigonal system, R 3, a = 2695.1(3), c = 1030.8(4) pm, Vm = 216.97(5) cm 3/m ol, R = 0.041, Rw = 0.030. | | |
Reference
| Z. Naturforsch. 47b, 179—182 (1992); eingegangen am 5. September 1991 | | |
Published
| 1992 | | |
Keywords
| Samarium Acetate, Acetic Acid Adduct, Synthesis, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0179.pdf | | | Identifier
| ZNB-1992-47b-0179 | | | Volume
| 47 | |
6 | Author
| Volker Müller, Gerlinde Frenzen, K. Urt Dehnicke, Dieter Fenske | Requires cookie* | | Title
| Synthese, FIR-Spektren und Kristallstrukturen der Pentaselenide K2Se5 und [Na(15-Krone-5)l2Se5 Syntheses, F IR Spectra, and Crystal Structures of the Pentaselenides K 2Se5 and [Na( 15-crown-5)]2Se5  | | | Abstract
| K2Se5 has been prepared by crystallization from a potassium polyselenide solution in D M F. In a similar way [Na(15-crown-5)]2Se5 can be prepared by crystallization from a sodium p oly selenide solution in D M F in the presence o f 15-crown-5. Both com pounds were characterized by FIR spectroscopy as well as by X-ray structure determinations. K2Se5: Space group P 2,2,2,, Z -4, 1659 observed independent reflections, R = 0.061. Lat tice dim ensions at -9 0 °C; a = 671.5(5), b = 694.9(5), c = 1776.4(9) pm. The com pound crys tallizes with the K2S5 type structure. [Na(15-crown-5)]2Se5: Space group P 1, Z = 2, 3026 observed indenpendent reflections, R = 0.140. Lattice dim ensions at -1 0 0 °C: a = 853.7(5), b = 1042.8(10), c = 2011.0(10) pm; a = 88.95(5)°, ß = 79.42(5)°, y = 66.15(5)°. The compound forms an ion triple, in which the sodium ions are coordinated by the five oxygen atoms o f the crown ether molecules as well as by the terminal selenium atom s o f the pentaselenide chain. The rather high R value is a result o f the disordered crown ether molecules. | | |
Reference
| Z. Naturforsch. 47b, 205 (1992); eingegangen am 23. August 1991 | | |
Published
| 1992 | | |
Keywords
| Pentaselenides, Syntheses, FIR Spectra, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0205.pdf | | | Identifier
| ZNB-1992-47b-0205 | | | Volume
| 47 | |
7 | Author
| Kerstin Müller3, AntonM. Heynsb, Klaus-Jürgen Range3, M. Anfred Zabela | Requires cookie* | | Title
| The Polymorphism of Alkali Metal Formates, Part 3 A Raman Spectroscopic, X-Ray and Thermoanalytical Study of the Polymorphism of Lithium Formate  | | | Abstract
| The crystal structure o f anhydrous lithium formate, published recently by Kansikas and Hermansson, is in fact that o f a quenchable high-temperature m odification (L iH C O O -I). The low-temperature modification L iH C O O -II can be obtained by thermal dehydration o f the monohydrate, LiHCOO-H20 , or by drying it over P4O 10. L iH C O O -II persists up to 228 C, at which temperature it transforms to L iH C O O -I, which in turn is stable up to its melting point at 272 °C. L iH C O O -I is also the m odification which crystallizes when a melt o f lithium formate is cooled down, in spite o f the fact that solidification occurs only at 165 "C, i.e. at a temperature well within the stability region o f L iH C O O -II. The Raman spectra o f the differ ent forms o f lithium formate are discussed in some detail. | | |
Reference
| Z. Naturforsch. 47b, 238 (1992); received June 10 1991 | | |
Published
| 1992 | | |
Keywords
| Lithium Formate, Polymorphism, Raman Spectra, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0238.pdf | | | Identifier
| ZNB-1992-47b-0238 | | | Volume
| 47 | |
8 | Author
| M. Onika Paulus, G.Erhard Thiele | Requires cookie* | | Title
| Synthese und Kristallstruktur von Tris-//-chlorodichloro- tetrakis(dichlorsulfan)diruthenium(II, III), eines unsymmetrisch substituierten, gemischtvalenten Ruthenium(II, III)-Komplexes mit SCl2-Liganden Synthesis and Crystal Structure o f Tris-//-chlorodichlorotetrakis(disulfane)diruthenium(II, III) - an Unsymmetrically Substituted Mixed-Valence Ruthenium(II, III) Complex with SC12 Ligands  | | | Abstract
| Black crystals o f Ru2S4C113 have been obtained by reaction o f Ru with SC12 in closed quartz ampoules at 125 °C. The crystal structure o f the mixed-valence ruthenium(II, III) com pound (m onoclinic, a = 8.0262(15)Ä , b = 14.9612(33)Ä , c = 32.8876(55)Ä, ß = 97.03(1)°, space group P 2,/c, Z = 4) consists o f m olecules Ru2C15(SC12)4, in which the two Ru atom s are un symmetrically substituted by Cl and SC12 ligands. Octahedral units o f RuC15(SC12) and RuC13(SC12) 3 are Cl bridged to binuclear complexes C12(SC12)Ru(//-C1)3Ru(SC12)3. | | |
Reference
| Z. Naturforsch. 47b, 253 (1992); eingegangen am 12. Juli/9. September 1991 | | |
Published
| 1992 | | |
Keywords
| Ruthenium Complex, M ixed-Valence, Sulphurdichloride, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0253.pdf | | | Identifier
| ZNB-1992-47b-0253 | | | Volume
| 47 | |
10 | Author
| Rainer Pöttgen, Wolfgang Jeitschko | Requires cookie* | | Title
| Sc5Re2C7, a Complex Carbide with C3-Units  | | | Abstract
| The title com pound was obtained by arc melting o f the elemental com ponents and subse quent annealing in a high frequency furnace. It crystallizes with the orthorhombic space group Cmmm, a = 779.26(7) pm, b = 1362.0(1) pm, c = 320.62(3) pm, V = 0.3403 nm3, Z -2. The structure was determined from single-crystal X-ray data and refined to a residual o f R = 0.021 (692 F values and 21 variables). It is closely related to the NaCl-structure. Three o f the seven carbon atom s per formula unit form linear C3-units with C -C bond lengths o f 134 pm. They are coordinated to ten Sc atom s forming bicapped quadratic prisms. Additional isolated C atoms are located in octahedral voids formed by four Sc and two Re atoms. Together with the Re atom s they form tw o-dim ensionally infinite [Re2C4"~]" polyanions. The Re atoms have highly distorted tetrahedral carbon coordination with R e -C bond lengths o f 200 and 208 pm corresponding to bond orders o f about two. This coordination seems to be compatible with the 18-electron rule. The near-neighbour coordination o f the Re atoms is assymmetric. It is suggested that this is due to the space requirements o f nonbonding electrons. Samples o f Sc5Re2C7 are sem iconducting and weakly paramagnetic. | | |
Reference
| Z. Naturforsch. 47b, 358 (1992); received September 2 1991 | | |
Published
| 1992 | | |
Keywords
| Crystal Structure, Scandium Rhenium Carbide, 18-Electron Rule | | |
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| default:Reihe_B/47/ZNB-1992-47b-0358.pdf | | | Identifier
| ZNB-1992-47b-0358 | | | Volume
| 47 | |
12 | Author
| A. Lfred, D. Bacher, Irin, Sens Und, U. Lrich, M. Üller | Requires cookie* | | Title
| Ein neuer Zugang zu Tetrathiooxalaten. Die Kristallstruktur von (NEt4)2[C2S4]  | | | Abstract
| (N E t4)2S5 was prepared from N E t4Cl and N a 2S4 in ethanol. Its reaction with boiling acetoni-trile yielded tetraethylammonium tetrathiooxalate. (N E t4)2[C2S4] was also obtained by heating (N E t4)2S5 with tetraethylammonium dithioacetate in ethanol. Benzyltriethylammonium tetra thiooxalate, (N E t3Bz)2[C2S4] • 2 toluene, crystallized after N E t3BzCl and N a 2S4 were heated in acetonitrile on subsequent addition o f toluene. The crystal structure o f (N E t4)2[C2S4] was de termined by X-ray diffraction (454 independent observed reflexions, R = 0.047). Crystal data: tetragonal, a = 871.2(1) pm, c = 1566.0(3) pm, space group P 4 2/nmc, Z = 2. The [C2S4]2-ion has point symmetry 4 m 2 (D 2d), i.e. the dihedral angle between the two CS2 groups is 90°. The ethyl groups o f the N E t4+ ions are disordered in two orientations. | | |
Reference
| Z. Naturforsch. 47b, 702 (1992); eingegangen am 21. Oktober 1991 | | |
Published
| 1992 | | |
Keywords
| Tetraethylammoniun Pentasulfide, Tetraethylammonium Tetrathiooxalate, Benzyltriethylammonium Tetrathiooxalate, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0702.pdf | | | Identifier
| ZNB-1992-47b-0702 | | | Volume
| 47 | |
13 | Author
| Irina Sens, AlfredDirk Bacher, Ulrich Müller | Requires cookie* | | Title
| Natrium-tetraethylammonium-tetrasulfid, N a+NEt4+S42 Synthese und Kristallstruktur Synthesis and Crystal Structure  | | | Abstract
| N aN E t4S4 was obtained from an equimolar solution of N a2S4 and N E t4Cl in ethanol. Its crystal structure was determined by X-ray diffraction with 4175 observed unique reflexions, R = 0.044. Crystal data: a = 713.4(4), b = 1744.5(9), c = 1204.0(5) pm, ß = 105.8(3)°, space group P 2 ,/«, Z = 4. In the structure, chains consisting of N a + and S42~ ions run in the a direc tion, every N a+ being coordinated by four terminal S atom s of S42~ ions (two terminal, one chelating). The chains are separated by the N E t4+ ions. | | |
Reference
| Z. Naturforsch. 47b, 819—822 (1992); eingegangen am 16. Januar 1992 | | |
Published
| 1992 | | |
Keywords
| Sodium Tetraethylammonium Tetrasulfide, Synthesis, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0819.pdf | | | Identifier
| ZNB-1992-47b-0819 | | | Volume
| 47 | |
14 | Author
| Henry Strasdeit | Requires cookie* | | Title
| Synthesis, Spectroscopic and X-Ray Structural Characterization of |Cd(linpen)l2+, a Model for M etal Complexes of the Chelating Polymer Polyethyleneimine (linpen = Linear Pentaethylenehexamine)  | | | Abstract
| The isolation of 3,6,9,12-tetraazatetradecane-l,14-diam ine (linear isomer o f pentaethylene hexamine, linpen) from a technical polyamine mixture is described. In methanol, linpen acts as a hexadentate ligand tow ards cadmium(II). The solid compounds [Cd(linpen)](BPh4)2 (1), [Cd(linpen)](BPh4)2-2D M SO (2) and [Cd(linpen)](BF4)2 (3) have been isolated and character ized by elemental analysis, spectroscopy and X-ray powder diffraction. The 113Cd N M R reso nance of 1 is at 351 ppm (0.30 M in DM SO -d6, standard: 0.10 M Cd(C104)2 in D 20). 2 and 3 have been structurally characterized by single-crystal X-ray diffraction. 2: C2/c; a = 19.337(1) A, b = 17.937(1)Ä, c = 18.584(1)Ä, ß = 1 1 1.54(1)°; Z = 4, R = 0.034, Rw = 0.033. 3: P2,/h; a = 8.607(1)Ä, b = 14.851(2)Ä, c = 15.703(2)Ä, ß = 91.21(2)°; Z = 4, R = 0.083, R" = 0.072. Both com pounds contain discrete [Cd(linpen)]2+ complexes. The hexamine wraps ar ound the metal ion in a helical manner. This results in a strong distortion of the coordination polyhedron. The mean C d -N bond lengths are 2.38Ä and 2.37Ä for 2 and 3, respectively. Models for M N 6 centers in metal-polyethyleneimine (PEI) complexes are derived from the structure of [Cd(linpen)]2+. F or example, loops at the M N 6 site in molecules of linear PEI are proposed. | | |
Reference
| Z. Naturforsch. 47b, 829—836 (1992); received December 12 1991 | | |
Published
| 1992 | | |
Keywords
| Pentaethylenehexamine, Cadmium Complex, Synthesis, Crystal Structure, Polyethyleneimine | | |
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| default:Reihe_B/47/ZNB-1992-47b-0829.pdf | | | Identifier
| ZNB-1992-47b-0829 | | | Volume
| 47 | |
15 | Author
| Brigitte Tecklenburg, Uwe Klingebiel, M. Athias, N. Oltem, Eyer+, Dieter Schmidt-Bäse+ | Requires cookie* | | Title
| Tetrafluorcyclodi-und Hexafluorcyclotrisilazane Tetrafluorocyclodi-and Hexafluorocyclotrisilazanes  | | | Abstract
| Bis(silylamino)difluorosilanes (1,2) are prepared in the reaction o f lithiated di-Je/7-butyl-methyl-and ter/-butyl-dimethylsilylamine with tetrafluorosilane. The dilithium derivative o f 1 reacts with SiF4 to give the tetrafluoro-substituted four-membered (S i -N) ring system [(C M ej^M eSiN-SiFJj (3). Two four-membered rings [(R N -S iF 2)2 (4), (R N -S iF N R S iF 3)2 (5), R = CM e3SiM e2] are obtained in the reaction o f dilithiated 2 with SiF4. The dilithiated silyl-amines and SiF4 also react with formation o f 3 and 4. However, besides 4 the six-membered ring (C M e3SiM e2N -S i F 2)3 (6) is obtained. Crystal structures o f 3, 5, and 6 were determined. A transannular Si • • • Si ring distance o f 237,5 pm is found in 3. | | |
Reference
| Z. Naturforsch. 47b, 855 (1992); eingegangen am 9. Dezem ber 1991 | | |
Published
| 1992 | | |
Keywords
| Cyclosilazanes, Ring Distance Si — Si, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0855.pdf | | | Identifier
| ZNB-1992-47b-0855 | | | Volume
| 47 | |
16 | Author
| K. Urt, O. Klepp | Requires cookie* | | Title
| Darstellung und Kristallstruktur von Na4Ga2S5. Ein Thiogallat mit i -[Ga2S5]4_ -Z weier-Doppelketten Preparation and Crystal Structure of N a4G a2S5. A Thiogallate with ],-[Ga2S5]4~-zweier-Double Chains  | | | Abstract
| T ransparent single crystals of N a4G a2S5 were obtained from a melt of N a2S, G a and S. N a4G a2S5 is monoclinic, space group P 2 l/c with a = 7.967(1), b = 6.133(2), c = 19.852(9) Ä, ß = 91.61(2)°, Z = 4. Its crystal structure was refined to a conventional R o f 0.033 for 1150 observed reflections. The structure of N a4G a2S5 is of a new type. It is characterized by infinite ribbon like thiogal late anions, ,J,-[Ga2S5] , which are built up by G aS4-tetrahedra (mean G a -S bond length 2.28 Ä) sharing apices and edges. The four crystallographically independent alkali cations are coordinated to six sulphur atoms in distorted octahedral configurations. | | |
Reference
| Z. Naturforsch. 47b, 937—941 (1992); eingegangen am 1. O ktober 1991 /7. Februar 1992 | | |
Published
| 1992 | | |
Keywords
| Thiogallate(III), Crystal Structure, Chain Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-0937.pdf | | | Identifier
| ZNB-1992-47b-0937 | | | Volume
| 47 | |
17 | Author
| Alfred-Dirk Bacher, Ulrich Müller | Requires cookie* | | Title
| Synthese und Kristallstruktur von INa(15-Krone-5)]2S6 Synthesis and Crystal Structure of [Na(15-crown-5)]2S6  | | | Abstract
| [Na(15-crown-5)]2S6 was obtained from N a 2S4 und 15-crown-5 in acetonitrile. Its crystal structure was determined by X-ray diffraction with 2968 observed reflexions, R = 0.119. Crys tal data: a = 861.4(9), 6 = 1006(1), c = 2097(1) pm, a = 89.7(1), ß = 100.20(8), y = 114.6(1)°, Z = 2, space group P 1. The chain-like S62-ion has transoid conform ations, each o f its terminal atom s is in contact with one N a + ion which in turn is coordinated with one crown ether m ole cule. | | |
Reference
| Z. Naturforsch. 47b, 1063—1066 (1992); eingegangen am 6. Februar 1992 | | |
Published
| 1992 | | |
Keywords
| Sodium -Crown Hexasulfide, Synthesis, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-1063.pdf | | | Identifier
| ZNB-1992-47b-1063 | | | Volume
| 47 | |
18 | Author
| Siegfried Pohl, Ulrich Bierbach | Requires cookie* | | Title
| |Fe4S4I2(C6H 10(N HCSNHMe)2)]: ein neutraler Eisen-Schwefel-Cluster mit zweizähnigem Liganden [Fe4S4l2(C6H 10(NHCSNHMe)2)]: A Neutral Iron-Sulfur Cluster with a Bidentate Ligand  | | | Abstract
| The reaction o f [Fe4S4I2(SC (N M e2)2)2 ] with racemic l,2-bis(3-m ethylthioureido)-cyclohexane in tetrahydrofuran (thf) yields [Fe4S4I2(C 6H 10(N H C S N H M e)2)]-4 th f (2). 2 crys tallizes in the monoclinic space group C 2/c with a = 1471.7(2), b = 1329.7(2), c = 2339.3(3) pm, ß = 107.70(1), V = 4362.3 x 106pm 3, Z = 4, R -0.057. The cluster exhibits C2 symmetry in the solid state. The replacement o f the m onodentate neutral ligands results in a cluster in which the bifunctional thiourea derivative bridges tw o different iron sites o f the slightly com pressed [Fe4S4] core. The most striking feature are the differences o f the F e -F e distances which are 269.8 pm between thiourea coordinated atom s and 280.7 pm between Fe atom s with iodide ligation. The F e -S thiourea distance was found to be 229.3 pm. | | |
Reference
| Z. Naturforsch. 47b, 1266—1270 (1992); eingegangen am 13. März 1992 | | |
Published
| 1992 | | |
Keywords
| Neutral [Fe4S4] Cluster, Crystal Structure, Subsite Specific Reactions | | |
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| default:Reihe_B/47/ZNB-1992-47b-1266.pdf | | | Identifier
| ZNB-1992-47b-1266 | | | Volume
| 47 | |
20 | Author
| Viktor Keimes, Albrecht Mewis | Requires cookie* | | Title
| Strukturvarianten des MgCu2 -Typs: Die Verbindungen Mg2 Ni3P und Mg2 Ni3As  | | | Abstract
| Variants of the M gC u2 Type: The C om pounds M g2N i3P and M g2N i3As The com pounds M g2N i3P and M g2N i3A s were prepared by heating the elements. Their structures have been determined from single-crystal X-ray data. The structure o f the phosphide is a rhombohedral ternary variant o f the cubic Laves structure type M gCu2 (R 3m ; hexagonal lattice constants: a = 4.971(0)Ä , c = 10.961 (2) Ä). The ordered substitution o f one quarter o f the metal atom s by phosphorus and the resulting shorter distances are responsible for the rhombohedral symmetry. The arsenide crystallizes in the M gC u2 type structure (F d3m ; a = 6.891(1)A , com position M g2N i3A s) with a statistic distribution o f the N i and As atoms; the relevant hom ogeneity range extends from M g2N i2 9A s , , to M g2N i3 5A s0 5. | | |
Reference
| Z. Naturforsch. 47b, 1351—1354 (1992); eingegangen am 23. März 1992 | | |
Published
| 1992 | | |
Keywords
| M agnesium, N ickel, Phosphide, Arsenide, Crystal Structure | | |
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| default:Reihe_B/47/ZNB-1992-47b-1351.pdf | | | Identifier
| ZNB-1992-47b-1351 | | | Volume
| 47 | |
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