| | 41 | Author
| KurtO. Klepp, Andreas Kolb | Requires cookie* | | | Title
| Komplexe Chalkogenide der IVa Metalle mit niedrigdimensionalen anionischen Partialstrukturen. Darstellung und Kristallstruktur von K2ZrTe3 und Rb2ZrTe3 Complex Chalcogenides of the IVa Metals with Low Dimensional Anionic Partial Structures. Preparation and Crystal Structures of K2ZrTe3 and Rb2ZrTe3  | | | | Abstract
| The isostructural compounds K2ZrTe3 and Rb2ZrTe3 were obtained at 1000°C by reacting K7Te and Rb9Te with stoichiometric amounts of Zr and Te. The compounds are monoclinic, mP24, space group P2,/c, Z = 4 with a = 9.089(3), b = 14.148(4), c = 6.986(3)Ä, ß = 105.90(1)° and a = 9.735(4), b = 14.300(7), c = 6.952(8) Ä, ß = 108.61(2)°, respectively. The crystal structure was determined from diffractometer data and refined to R = 0.030 for 1452 Fo's for K2ZrTe3 and R = 0.038 for 1131 Fo's for Rb2ZrTe3. The crystal structure is of a new type, characterized by infinite anionic chains, ^-[ZrTe3]2_ built up by octahedra sharing opposite faces which run along [001]. The mean Zr-Te bond lengths are 2.921 and 2.920 A, respectively. The alkali cations separating the chains are characterized by two different -distorted octahedral and pentagonal bipyramidal -chalcogen environments. E inleitung | | | |
Reference
| Z. Naturforsch. 54b, 441 (1999); eingegangen am 9. November 1998 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, Complex Chalcogenides, Tellurides, Zirconium, Pseudo-one-dimensional solids | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0441.pdf | | | | Identifier
| ZNB-1999-54b-0441 | | | | Volume
| 54 | |
| 42 | Author
| F. K. Ubela, H. Billb, H. H. Ag, Em An | Requires cookie* | | | Title
| Low Temperature Crystal Growth and Structure of Ordered Ba7F12Cl2 | | | | Abstract
| of composition Ba7F12Cl2 were obtained by a reaction at room temperature be tween Ba2+/Cl"/F_ in a gel of agar-agar/water. The hexagonal crystals have space group P6, «=1064.69(8), c=417.89(5)pm, V=410.24(8) 106 pm3 and Z=l. The anions form a propeller type network located in tunnels parallel to the chex axis; the chloride ions are located at the center on the propeller axes. The Ba2+ ions are coordinated by a (distorted) tricapped trigo nal environment of fluoride and chloride anions. Disorder is present for one particular Ba2+ site. The average structure is isotypic with the structure of Pb7F)2Cl2. | | | |
Reference
| Z. Naturforsch. 54b, 515—518 (1999); received November 30 1998 | | | |
Published
| 1999 | | | |
Keywords
| Bariumfluorochloride, Hexagonal Crystal Structure, Crystal Growth, Low Temperature Gel Method Crystals | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0515.pdf | | | | Identifier
| ZNB-1999-54b-0515 | | | | Volume
| 54 | |
| 43 | Author
| Karna Wijaya, Oliver Moers, Blaschette Arm, PeterG. Jones | Requires cookie* | | | Title
| Polysulfonylamine, CXII [1] Neues aus der Festkörperchemie der 2-Pyridone: Isolierung und Röntgenstrukturen von Bis(2-pyridon)hydrogen(I)-und Bis(6-methyl-2-pyridon)hydrogen(I)-dimesylamid Polysulfonylamines, CXII [1] A Novel Solid-State Aspect of 2-Pyridones: Isolation and X-Ray Structures of Bis(2-pyridone)hydrogen(I) and Bis(6-methyl-2-pyridone)hydrogen(I) Dimesylamides | | | | Abstract
| The compounds (2-pyridone)2H +(M e S 0 2)2N~ (1, monoclinic, space group V ljn) and ( | | | |
Reference
| Z. Naturforsch. 54b, 643 (1999); eingegangen am 11. Januar 1999 | | | |
Published
| 1999 | | | |
Keywords
| 2-Pyridones, 2-Hydroxypyridines, Dimesylamide, Hom oconjugate Cations, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0643.pdf | | | | Identifier
| ZNB-1999-54b-0643 | | | | Volume
| 54 | |
| 44 | Author
| Rolf-Dieter Hoffmann3, Dirk Kußmanna, Ute Ch, Rainer Rodewald3, Pöttgen3, Carsten Rosenhahnb, BerndD. Moselb | Requires cookie* | | | Title
| New Stannides CaTSn2 (T = Rh, Pd, Ir) and Ca2Pt3 Sn5 -Synthesis, Structure and Chemical Bonding | | | | Abstract
| New stannides CaTSm (T = Rh, Pd, Ir) and Ca2P hSn5 were prepared as single phase materials by a reaction o f the elements in glassy carbon crucibles under flowing purified argon. The four compounds were investigated by X-ray diffraction both on powders and single crystals and their structures were refined from single crystal data. The stannides CaTSn2 (T = Rh, Pd, Ir) adopt | | | |
Reference
| Z. Naturforsch. 54b, 709 (1999); received February 25 1999 | | | |
Published
| 1999 | | | |
Keywords
| Intermetallic Calcium Compounds, Crystal Structure, Mössbauer Spectroscopy, Chemical Bonding | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0709.pdf | | | | Identifier
| ZNB-1999-54b-0709 | | | | Volume
| 54 | |
| 46 | Author
| Christoph Mockenhaupt, Ralf Eßmanna, HeinzDieter Lutz | Requires cookie* | | | Title
| [Ni(NH3 )6]S0 4 : Kristallstruktur und Infrarotspektren [Ni(NH3)6]S 0 4: Crystal Structure and Infrared Spectra | | | | Abstract
| The crystal structure of [Ni(NH3)6]S 0 4 has been determined by single-crystal X-ray dif fraction (P2,/c; Z = 4; a = 705.0(1), b = 1195.2(2), c = 1180.0(2) pm, ß = 96.14(3)°; 2271 reflections; R x = 3.94%). In the hitherto unknown structure type, both the [Ni(NH3)6]2+ and the S 0 42-ions form chains along [100], The six crystallographically different ammine ligands of the distorted [Ni(NH3)6]2+ octahedra are involved in hydrogen bonds to six crystallographically equivalent S 0 42-ions (site symmetry C |). The strength of the hydrogen bonds differs strongly (i'od ° f matrix isolated N H 2D molecules: 2378 -2494 cm -1 , N -O distances: 272 -340 pm). The temperature evolution of the IR bands reveals the decrease of the dynamic orientational disorder of the N H 3 molecules with decreasing temperature. | | | |
Reference
| Z. Naturforsch. 54b, 843—848 (1999); eingegangen am 8. März 1999 | | | |
Published
| 1999 | | | |
Keywords
| Hexammine Nickel Sulfate, Ammoniates, Crystal Structure, IR Data, Hydrogen Bonding | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0843.pdf | | | | Identifier
| ZNB-1999-54b-0843 | | | | Volume
| 54 | |
| 48 | Author
| Bernd Ziegler, Michael Witzel, Martin Schwarten, Dietrich Babel | Requires cookie* | | | Title
| Neutronen-und Röntgenbeugungsuntersuchungen an Pulvern und Einkristallen von Strukturverwandten des Berliner Blaus: CsMnnCrln (CN)6 * D20 , NMe4MnII(Cr,M)6Mn0>»4)III(CN)6 * 8 H20 , NMe4MnIICoI1I(CN)6 * 8 H20 , Mn3ll[MnI1I(CN)6]2 * 15 H20 und Cd3[Fen l(CN)6]2 * 15 H20 Neutron and X-Ray Diffraction Studies on Powders and Single Crystals of Compounds Structurally Related to Prussian Blue: CsMn1ICrIII(CN)6 * D^O, NMe4MnII(Cr006Mn0 94)III(CN)6 * 8 H.O, NMe4MnnCoin(CN)6 * 8 H .O " Mn3II[MnIII(CN)6]2 * 15 H20 and Cd3[Fem(CN)6]2 * 15 H20 | | | | Abstract
| The results of a Rietveld refinement of CsMnCr(CN)6 • D20 neutron powder data (a = 1084.3(1) pm, F43m, Z = 4) and of a neutron single crystal structure refinement of tetragonal NMe4M nII(Cro.o6Mno.94)III(CN)6 • 8 H20 (a = 1065.8(21), c = 1064.6(26) pm, P4/n, Z = 2) at ambient temperature are reported. Single crystal X-ray analyses of the isostructural octahydrate NMe4M nCo(CN)6 • 8 H20 (a = 1062.1 (1), c = 1046.2(1) pm) and of gel-grown crystals of cubic M n31I[M nI1I(CN)6]2 -15 H20 (a = 1062.6(3) pm, Fm3m, Z = 4/3) and Cd3[Fe(CN)6]2 • 15 H20 (a = 1067.7(3) pm) were performed as well. The latter "Prussian Blues" are highly disordered and intermediate with respect to cyano-bridging between the above three-dimensional cesium and one-dimensional tetramethylammonium compounds. | | | |
Reference
| Z. Naturforsch. 54b, 870—876 (1999); eingegangen am 6. April 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, Neutron Diffraction, Prussian Blue, Hexacyanometallate(III) | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0870.pdf | | | | Identifier
| ZNB-1999-54b-0870 | | | | Volume
| 54 | |
| 49 | Author
| M. Athias, O. Senge, W. Erner, W. Kalisch | Requires cookie* | | | Title
| Structure and Conformation of Tetra-meso-, O c t a -ß and Dodecasubstituted 22,24-Dihydroporphyrins (Porphyrin Dications) | | | | Abstract
| A comparative crystallographic analysis of the conformation of porphyrin diacids with various substituent types reveals considerable differences in the degree of nonplanarity and distortion modes. Diacids of 5,10,15,20-tetraarylporphyrins generally exhibit typical saddle-distorted macrocycles with displacements of the Cb positions in the range of 0.7-1.0 A. Adding peripheral substituents, i.e., using dodecasubstituted porphyrins for the diacid forma tion yields similar distortion types albeit with larger out-of-plane displacements. As a result of the combined effect of both peripheral (interaction between the Cb and Cm substituents) and core (interaction between the four inner hydrogen atoms) steric strain the maximum Cb displacements reach 1.3-1.5 A. Quite a different situation is observed for the diacids of 2,3,7,8,12,13,17,18-octaalkylporphyrins. Here, macrocycles with pair-wise displacement of neighboring pyrrole rings and significant NH pyramidalization and those with classic saddle distortion are found. Generally, octa-/?-substituted porphyrin diacids show smaller degrees of nonplanarity; Cb displacements ranged from 0.06 to 0.72 A. On the basis of the overall degree of conformational distortion (ZI24 = average deviation of the 24 macrocycles atoms from the mean plane), the three different types of porphyrin macrocycles studied differ considerably in their degree of conformational flexibility. For several porphyrin crystal structures with different counterions and/or solvate molecules were obtained. Taking into account results from the literature 2,3,7,8,12,13,17,18-octaethyl-22,24-dihydro-5,10,15.,20-tetraphenylporphy-rin (13) shows the smallest degree of flexibility (ZI24 = 0.61-0.63 A; four different X-ray structures),o while 22,24-dihydro-5,10,15,20-tetraphenylporphyrin (1) is more flexible (ZI24 = 0.42-0.52 A; four structures). The largest flexibility is observed for 2,3,7,8,12,13,18-octaethyl-22,24-dihydroporphyrin (7) (A24 = 0.02-0.33 A; four structures). | | | |
Reference
| Z. Naturforsch. 54b, 943—959 (1999); received May 4 1999 | | | |
Published
| 1999 | | | |
Keywords
| Porphyrins, Steric Strain, Porphyrin Dications, Crystal Structure, 22, 24-Dihydroporphyrins | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0943.pdf | | | | Identifier
| ZNB-1999-54b-0943 | | | | Volume
| 54 | |
| 51 | Author
| Dirk Kußmann3, Rainer Pöttgen, Ute Ch, Carsten Rodewald3, BerndD. Rosenhahnb, Gunter Moselb, Bernd Kotzyba3, Künnen3 | Requires cookie* | | | Title
| Structure and Properties of the Stannide Eu2Au2Sn5, and its Relationship with the Family of BaAl4-Related Structures | | | | Abstract
| The stannide Eu2Au2Sn.i was prepared by high-frequency melting of the elements in a sealed tantalum tube. The structure of Eu-iAu^Sn^ was refined from single crystal X-ray data: P2\/m, a = 928.6(2), b = 465.8(2), c = 1042.9(3) pm, ß = 92.28(2)°, wR2 = 0.0653, 1220 F2 values and 56 variables. The structure of Eu2Au2Sns is of a new type, it can be considered as an ordered defect variant of the BaAU type. Due to the ordered defects, the coordination number (CN) of the two crystallographically different europium sites is reduced from CN 16 to CN 14. The gold and tin atoms in Eu2Au2Sn_s form a complex three-dimensional [A ^Sns] polyanion in which the europium atoms are embedded. Within the polyanion short Au-Sn and Sn-Sn distances are indicative of strongly bonding Au-Sn and Sn-Sn interactions. A detailed group-subgroup scheme for various ordered and defect variants of the BaAU family is presented. EuiA^Sn? shows Curie-Weiss behavior above 50 K with an experimental magnetic moment of 7.90(5) /ub/Eu, indicating divalent europium. Antiferromagnetic ordering is detected at 5.8(5) K at low fields and a metamagnetic transition occurs at a critical field of 1.4(2) T. Eu2Au2Sns is a metal with a specific resistivity of 150±20 p f i cm at room temperature. The results of l:i|Eu and 119Sn Mössbauer spectroscopic experiments are compatible with divalent europium and show complex hyperfine field splitting with a transferred magnetic hyperfine field at the tin nuclei at low temperature. | | | |
Reference
| Z. Naturforsch. 54b, 1155—1164 (1999); received June 7 1999 | | | |
Published
| 1999 | | | |
Keywords
| Europium Gold Stannide, Crystal Structure, Mössbauer Spectroscopy, Group-Subgroup Relations | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1155.pdf | | | | Identifier
| ZNB-1999-54b-1155 | | | | Volume
| 54 | |
| 52 | Author
| Dietrich Gudata, AndreasW. Holderberg3, Nikolaus Korberb, Martin Nieger3, Martin Schrott3 | Requires cookie* | | | Title
| Bis-phosphonio-isophosphindolide Copper Complexes | | | | Abstract
| Bis-triphenylphosphonio-isophosphindolide salts 1[X] react with Cu(I)-halides CuX to give isolable products of composition [(l)Cu2X3]. X-ray crystal structure analyses confirmed that for X = Br, Cl dinuclear complexes [(/y-1)(/i-X)Cu2X2] with /i2j;'(P)-bridging cations 1 are formed, while for X = I a solid phase containing a salt (l^lC u*^] and a complex [(l^ C u .^ ] with a terminal ?/(P)-coordinated ligand 1 was obtained. The bonding parameters in the two types of complexes suggest that l i s a hybrid between a phosphenium cation and a phospholide anion whose 7T-system is less nucleophilic than the phosphorus lone-pair.31P NMR studies revealed that in solution in all cases binuclear complexes [(l)Cu2X3] are in dynamic equilibrium with small amounts of mononuclear species and free 1. The same equilibria were detected in the system l[OTf]/CuOTf. NMR studies of ligand exchange reactions indicated that the stability of complexes [(l)Cu2X3] increases in the order X = OTf < 1 < Br, Cl, and titration of [(l)Cu2Bn] with EuNBr allowed to determine the equilibrium constant of the complex formation reaction. | | | |
Reference
| Z. Naturforsch. 54b, 1244—1252 (1999); received July 6 1999 | | | |
Published
| 1999 | | | |
Keywords
| Phosphorus Heterocycles, Copper Complexes, Crystal Structure, '' P NMR Data | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1244.pdf | | | | Identifier
| ZNB-1999-54b-1244 | | | | Volume
| 54 | |
| 53 | Author
| A.B M Shamsur, Rahman, H. Boiler, K. O. Klepp | Requires cookie* | | | Title
| Synthesis and Structural Characterization of [Me4N]2[W202(/i-S)(r72-S2)4]*MeCN, a Novel Oxo-thiotungstate(VI) | | | | Abstract
| Orange red crystals of the new compound [Me4 N]2 [W2 0 2 (^ -S 2)(?/2 -S2)4 ] MeCN were ob tained from the reaction of a solution of [Me4 N ]2 [WOS3 ] in MeCN with solid AuCN at room temperature. They are monoclinic, space group P2|//?, with a = 9.264(2), b = 17.736(3), c = 18.742(5) A, ß = 95.19(1)°; Z = 4. The crystal structure was determined from single crystal diffractometer data (M oKa-radiation) and refined to R = 0.050 (2955 reflections, 221 variable parameters). It is characterized by binuclear complex anions [(S2)2 0 WSWO(S2)2 r with close to C2 symmetry. Each metal center is surrounded by two end-on coordinating disulfide groups at distances ranging from 2.37 to 2.42 A which together with a bridging sulfur atom (dw-s = 2.445 A) occupy the equatorial positions of a pentagonal bipyramid whose apices are defined by a terminal oxygen atom (dw -o ~ 1 -725 A) and one sulfur atom of the neighboring component at a distinctly larger distance (dw -s ~ 2.82 A). Infrared spectra of the complex (KBr powder) showed z/(W-O) and i^(W-S) of bridging W-S-W at 931 (vs) and 454 (m) cm -1, respectively, u{ W-S) of the W S2 unit appeared in the range between 465 and 438 crrT 1. The mass spectrum of the anion showed the molecular mass at m/z 6 8 8 for [W2 0 2 S9 ]~ as well as peaks for other fragments. | | | |
Reference
| Z. Naturforsch. 54b, 1318—1322 (1999); received April 19 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, IR Data, Chalcogenides, Complex Sulfides, Tungsten Compounds | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1318.pdf | | | | Identifier
| ZNB-1999-54b-1318 | | | | Volume
| 54 | |
| 54 | Author
| Wilhelm Klein3, Martin Jansenb | Requires cookie* | | | Title
| Darstellung und Kristallstruktur von Lithiumozonid-Ammoniakat (1/5) Li(> 3 * 5 NH3 Synthesis and Crystal Structure of Lithiumozonide-Ammonia (1/5) L i0 3 * 5 NH3 | | | | Abstract
| Lithium ozonide has been synthezised starting from cesium ozonide via cation exchange in liquid ammonia and crystallizes at -78°C as an ammoniate, L i0 3 • 5NH3. The coarse, ruby red crystals decompose above the boiling temperature of ammonia and are extremely sensitive to moisture. The crystal structure of L i0 3 • 5NH3 (P c2\n; a = 1231.9(5), b = 637.4(2), c = 1104.8(4) pm; Z = 4; /?, = 4.57%; 1318 independent reflections) consists of lithium tetramine complexes, ozonide anions and non coordinating ammonia molecules. With respect to the arrangement of the complex cations and of the anions there is similarity to the WC type of structure. The central oxygen atom of the ozonide anion is disordered. | | | |
Reference
| Z. Naturforsch. 54b, 1345—1349 (1999); eingegangen am 28. Juni 1999 | | | |
Published
| 1999 | | | |
Keywords
| Lithium Ozonide Ammonia, Ionic Ozonides, Lithium Tetramine Complex, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1345.pdf | | | | Identifier
| ZNB-1999-54b-1345 | | | | Volume
| 54 | |
| 55 | Author
| Kristallstruktur Neuer, Kai Landskron, Wolfgang Schnick | Requires cookie* | | | Title
| Synthese und | | | | Abstract
| -diphosphazenium bromide [(NH->)3PNP(NHi)3]Br, nitrate 1(NH2)3PNP(NH2)3][N03], and toluene-4-sulfonate [(NH2)3PNP(NH2)3][CH3C6H4S0 3] have been prepared by anion exchange in aqueous solution. Single crystals were obtained from acetonitrile solutions in a temperature gradient between 60 °C and room temperature. The crystal structures were determined by single crystal X-ray methods at room temperature. ([(NH2)3PNP(NH2)3]Br: P i, Z = 2, a = 596.2(1),b = 744.5(1), c = 1114.4(1) pm, a = 108.78(1), ß = 104.18(1), 7 = 90.64(1)°, R 1 = 0.048, wR2 = 0.104; [(NH2)3PNP(NH2)3][N03]: Pi, Z = 2, a = 550.9(1), b = 796.3(1), c = 1115.7(1) pm, a = 94.45(1), ß = 99.55(1), 7 = 101,53(1)°, R l = 0.033, wR2 = 0.095; [(NH2)3PNP(NH2)3][CH3C6H4S 0 3]: P2,/c, Z = 4, a = 804.1(1), b = 596.1(1), c = 3218.7(3) pm, ß = 94.59(1)°, /?1 = 0.052, wR2 = 0.136). In the solid the three salts consist of discrete [(NHi)3PNP(NH2)3]+ cations and their corresponding anions. The PN4 tetrahedra in [(NH2)3PNP(NH2j3]Br are staggered, while in [(NH2)3PNP(NH2)3][N03] the eclipsed conformation is preferred. The PN4 tetrahedra of [(NH2)3PNP(NH2)3][CH3C 6H4S 0 3] show gauche conformation. | | | |
Reference
| Z. Naturforsch. 54b, 1363—1370 (1999); eingegangen am 13. Juli 1999 | | | |
Published
| 1999 | | | |
Keywords
| 3, 3, 3-Hexaamino-lA5, 3A5-diphosphazenium-Salze Synthesis and Crystal Structure of Novel l, l, l, 3, 3, 3-Hexaamino-lA5, 3A5-diphosphazenium Salts Phosphazenes, Ion Exchange, Crystal Structure 1, 1, 1, 3, 3, 3-Hexaamino-lA\3A5 | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1363.pdf | | | | Identifier
| ZNB-1999-54b-1363 | | | | Volume
| 54 | |
| 56 | Author
| Michael Schur, Astrid Gruhl, Christian Näther, Inke Jeß, Wolfgang Bensch | Requires cookie* | | | Title
| (CH3NH3)2Sb2S4, a New Thioantimonate(III) with Building Groups Stabilized by Hydrogen Bonds | | | | Abstract
| (CH3NH3)2Sb2S4 has been isolated from the reaction of antimony with sulfur in the presence of manganese in an ethanolic solution of methylamine under solvothermal conditions. Two pyramidal SbS? units are linked via common S-S edges to give dimeric Sb2S42-anions, which are joined via secondary Sb --S contacts of 3.074(2) and 2.975(2) A forming infinite 1 [SbS2]-^n chains consisting of edge-linked xp-SbS4 trigonal bipyramids. The cis configuration o? the Sb2S42-anions in the title compound is observed for the first time. A specific hydrogen-bonding pattern between the amino-hydrogen and the sulfur atoms stabilizes this configuration and gives rise to anionic layers separated by the methyl groups. | | | |
Reference
| Z. Naturforsch. 54b, 1524—1528 (1999); received July 21 1999 | | | |
Published
| 1999 | | | |
Keywords
| Thioantimonates, Solvothermal Synthesis, Crystal Structure, Hydrogen Bonding, Polymerie Anions | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1524.pdf | | | | Identifier
| ZNB-1999-54b-1524 | | | | Volume
| 54 | |
| 58 | Author
| Saalfrank, JochenN. Achtrab, Stephan Reck, Frank Hampel | Requires cookie* | | | Title
| Synthese und Aggregatbildung eines 5-Hydroxy-2,5-dihydropyrrols. Enantiomerenreine, eindimensionale Stränge durch Wasserstoff- brückenbindungen und chiroselektive Selbstorganisation [1] | | | | Abstract
| Synthesis and A ggregation o f a 5-H ydroxy-2,5-dihydropyrrole. E nantiom erically Pure, O ne-dim ensional Strands via Hydrogen Bonds and Chiroselective S eif O rganization [ 1 ] R olf W. Reaction of dimethyl 1,3-acetonedicarboxylate 8 with oxalylchloride 2 and magnesium chlo ride as catalyst yielded 2,3-dioxo-2,3-dihydrofuran 9, which is in equilibrium with tautomer 10 (9:10 = 1:2). Addition of thionyl chloride to a mixture of 9/10 afforded 3-chloro-2(5H)-furanone 11. The structure of 11 was unequivocally established by X-ray diffraction, which indirectly pro ved the structure of 10 as well. Ring opening of 11 by nucleophilic attack with benzylamine 14 in C2-position and subsequent recyclization led to racemic 3-chloro-5-hydroxy-2-oxo-2,5-di-hydropyrrole 15. According to a single crystal X-ray analysis, 15 aggregates via stereospecific self selection through hydrogen bonds to give chiroselectively the one-dimensional strands 1 1(S)-15] and I [(R)-1SI | | | |
Reference
| Z. Naturforsch. 54b, 179—186 (1999); eingegangen am 28. September 1998 | | | |
Published
| 1999 | | | |
Keywords
| 2(5H)-Furanones, Hydrogen-Bonding, Chiral Recognition, One-Dimensional Strand, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0179.pdf | | | | Identifier
| ZNB-1999-54b-0179 | | | | Volume
| 54 | |
| 59 | Author
| Hans-JoachimD. Rexler3, Ines Starkeb, M. Anuela, G. Rotjahnb, Helmut Reinke3, Erich Kleinpeterb, Hans-JürgenH. Oldt3 | Requires cookie* | | | Title
| SbCI3, BiCl3 and Na+ Complexes of Maleonitrile-Dithiacrown Ethers: Synthesis, Crystal Structures and DEP-MS Experiments | | | | Abstract
| The reactions of MC13 (M = Sb, Bi) with maleonitrile-dithia-15-crown-5 (mn-15S20 3) and maleonitrile-dithia-18-crown-6 (mn-18S20 4) in MeCN yielded the complexes [MCl3(mn-15S20 3)] {M = S b (l), Bi(2)} and [MCl3(mn-18S20 4)] {M = Sb(3), Bi(4)}, respec tively. The pyramidal MC13 units are coordinated very weakly to the three oxygen and two sulphur donor atoms of mn-15S20 3 in 1 and 2, and to the four oxygen donor atoms o f mn-18S20 4 in 3 and 4. Both mn-15S20 3 com plexes, 1 and 2, crystallize isotypically in the m ono clinic space group P2(\)ln with four formula units per unit cell, while the isotypic mn-18S20 4 complexes, 3 and 4, are triclinic, space group P-1, with two formula units per unit cell. In the SbCl3 complexes, 1 and 3, the mean contact distances between the Sb centres and the macro-cyclic donor atoms are longer than the corresponding distances in their isostructural BiCl3 analogues, 2 and 4, which may reflect a stereochem ical activity of the Sb,n lone pair. Under the conditions of DEP-M S experim ents with 1 and 3 the monocationic SbCl2+ complexes [SbCl2(L)]+ (L = mn-15S20 3, mn-18S20 4) were detected. NaSbCl6 and mn-18S20 4 in M eCN furnished the 2:1 complex [Na(mn-18S20 4)2]SbCl6 {(5)SbCl6). In the com plex cation 5 the sodium atom is coordinated sandwich-like through the eight oxygen atoms of two mn-18S20 4 molecules. Compound (5)SbCl6 crystallize in the triclinic space group P -1 with two formula units per unit cell. | | | |
Reference
| Z. Naturforsch. 54b, 799 (1999); received September 24 1998 | | | |
Published
| 1999 | | | |
Keywords
| Maleonitrile-Dithiacrown Ether Complexes, Antim ony and Bismuth Trichlorides, Sodium, Crystal Structure, D EP-M S | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0799.pdf | | | | Identifier
| ZNB-1999-54b-0799 | | | | Volume
| 54 | |
| 60 | Author
| Karsten Schweiger, Heiner Hückstädt, Heiner Homborg | Requires cookie* | | | Title
| Darstellung | | | | Abstract
| und Eigenschaften von Tetra(w-butyl)ammonium-c/s-diacidooxophthalocyaninato(2-)niobaten(V) und -tantalaten(V); Kristallstruktur von (wBu4N)CIS[Nb(F)20pc2'] Preparation and Properties of Tetra(«-butyl)ammonium c/'s-Diacidooxophthalocyanina-to(2-)niobates(V) and -tantalates(V); Crystal Structure of ("Bu4N)m [Nb(F)2Opc2~j Tetra(n-butyl)ammonium ds-diacidooxophthalocyaninato(2-)niobates(V) and -tantalates(V), (''Bu4N)m [M(X)2Opc2~] (M = Nb, Ta; X = F, Cl, NCS, N3), are obtained by the reaction of m [M(Cl)3pc2~] or m [M(Cl}Opc2~] (M = Nb, Ta) with the respective tetra(n-butyl)ammonium salt. ('!Bu4N)c'v[Nb(F)oOpc'_ ] crystallizes in the monoclinic space group P2\tn with cell pa rameters a = 13.460(5'), b = 13.820(5), c = 23.360(5) Ä, ß = 92.640(5)°, Z = 4. The hepta-coordinated Nb(V) atom is surrounded by four isoindole nitrogen atoms (Niso) of the pc2~ ligand, two fluorine atoms and one oxygen atom in a distorted square-base-trigonal-cap poly hedron. Nb(V) is displaced out o fothe centre of the (N,.s")4 plane (Ct(N,.so)) towards the acido ligands (d(Nb-Ct(Niso)) = 1.241 A). The average (Nb-NIJO), (Nb-F), and (Nb-O) distances are 2.300, 1.957, and 1.720(5) A, the (F-Nb-F) and the average (O-Nb-F) angles are 79.8(2) and 91.8°, respectively. The pc2_ ligand is concavely distorted. Typical 7r-7r*-transitions of the pc2~ligand are observed in the UV/Vis spectra at ca. 14500 and 29300 cm-1 . Vibration frequencies t/asiS(M-X), ^(M-O) and (5(X-M-0) have been assigned. | | | |
Reference
| Z. Naturforsch. 54b, 963—969 (1999); eingegangen am 23. April 1999 | | | |
Published
| 1999 | | | |
Keywords
| Phthalocyaninates, Niobium and Tantalum Compounds, Optical Spectra, Vibrational Spectra, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0963.pdf | | | | Identifier
| ZNB-1999-54b-0963 | | | | Volume
| 54 | |
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