| | 61 | Author
| StefanD. Icka, Gisbert Großmannb, G. Isela, Ohm Sb, Thom As Zeiskec | Requires cookie* | | | Title
| Aluminiumphosphate mit nichtzentrosymmetrischen Schicht-und Raumnetzstrukturen aus topologisch verwandten Motiven: 1. KA12(P 0 4)2(0H)*4H20 Aluminum Phosphates with Non-Centrosym metric Layer-and Framework-Structures o f Topologically Related Motifs  | | | | Abstract
| KAl2(P04)2(0 H)-4H20 could be obtained by the reaction of gibbsite with a potassium-phosphate solution of pH = 5.5 at 333 K. A single crystal X-ray structure analysis showed that KAl2(P04)2(0 H)-4H20 is isotypic with the mineral minyulite. Crystal data: orthorhombic space group P b a l, a = 934.7(1), b = 982, 1 (1), c = 551,0(1) pm, Z = 2. It possesses dimeric units of Al-octahedra which are bridged by an OH-and two bidentate phosphate groups. The dimers are linked by phosphate to plane polar layers. Cavities in the layers are occupied by K ions. One corner of each phosphate tetrahedron is not connected to Al but accepts four hydrogen bonds from water molecules bound to Al of the adjacent layer. A powder neutron scattering experiment with KAl2(P04)2(0 D)-4D20 showed that four D atoms and P coordinate the hydrogen bond accepting O in KAl2(P04)2(0 D)-4D20 like a square pyramid. Analogous dimeric building units are found in the Al phosphate minerals minyulite and morinite; similar dimers of Fe octahedra occur in the mineral copiapite, a number of Fe containing enzymes and numerous synthetic iron complexes. High-resolution 31P solid-state NMR spectra show only one isotropic line at <5;so = —9.6 ppm and confirm the presence of one symmetry independent phosphorus site in the unit cell. In the 'H-MAS-NMR spectra the water molecules and the bridging OH groups show signals at 5.4 and 1.4 ppm, respectively. | | | |
Reference
| Z. Naturforsch. 52b, 1439—1446 (1997); eingegangen am 9. September 1997 | | | |
Published
| 1997 | | | |
Keywords
| Crystal Structure, Neutron Scattering, MAS NMR, Minyulite, Aluminium Phosphate | | | |
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| default:Reihe_B/52/ZNB-1997-52b-1439.pdf | | | | Identifier
| ZNB-1997-52b-1439 | | | | Volume
| 52 | |
| 62 | Author
| Angela Bayler, Andreas Bauer, Hubert Schmidbaur | Requires cookie* | | | Title
| Chiral Phosphine Ligands in the Structural Chemistry of Gold | | | | Abstract
| The reaction of chloro(dimethylsulfide)gold(I) with (2-hydroxybutyl)diphenylphosphine (L) (racemic mixture) in dichloromethane affords high yields of the racemic chiral complex (L)AuCl. Metathesis reactions with KBr or KI, respectively, in a two-phase solvent mix ture (CH2CI2/H2O) lead to a conversion into the corresponding bromide and iodide complexes (L)AuBr and (L)AuI. Treatment of silver chloride with the ligand L in acetonitrile yields the analogous 1:1 adduct (L)AgCl. The compounds have been characterized by their analytical and spectroscopic data, and the structures of (L)AuCl and (L)AuBr have been determined by single-crystal X-ray diffraction. The compounds build isomorphous crystal lattices (monoclinic, P2i/c) in which pairs of enantiomers (R-and S-configuration of L) are aggregated by two long hydrogen bonds between the hydroxyl group of the ligand and the halogen substituent of the neighbouring molecule. Cationic, linear two-coordinate 1:2 complexes (L)2Au+ X-(X = BF4, CIO4, SO3CF3) and (L)2Ag+ X-(X = BF4) are obtained in good yields by reaction of L with Me2SAuCl and AgX (molar ratio 2:1:1) or with AgBF4 (molar ratio 2:1), respectively. 31P NMR studies at variable temperature show an equilibrium between all possible stereoisomers (RR, SS, RS, SR) in solution with rapid ligand exchange at ambient temperatures. | | | |
Reference
| Z. Naturforsch. 52b, 1477—1483 (1997); received October 14 1997 | | | |
Published
| 1997 | | | |
Keywords
| Gold Complexes, Phosphane Complexes, Chiral Phosphanes, Crystal Structure, Diastereomers | | | |
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| default:Reihe_B/52/ZNB-1997-52b-1477.pdf | | | | Identifier
| ZNB-1997-52b-1477 | | | | Volume
| 52 | |
| 63 | Author
| R. Pöttgen, K. H. Wachtmann, W. Jeitschko, A. Lang, T. Ebel | Requires cookie* | | | Title
| Er5Re2C7, Tm5Re2C7, and Lu5Re2C7 with Sc5Re2C7 Type, and Yb2ReC2 with Pr2ReC2 Type Structures | | | | Abstract
| ErsReiCy, TmsRe2C7, and LusReaC? were prepared by arc-melting of the elemental compo nents and subsequent annealing at 800 °C. ErsRe^Cy forms only after the annealing process, whereas the other two carbides were already present in the as cast samples. They crystallize with a ScsReiC? type structure, which was refined from single-crystal X-ray data of LusRe2C7: Cmmm, a = 791.44(5), b = 1418.08(8), c = 332.79(2) pm, Z = 2, R = 0.037 for 544 structure factors and 21 variable parameters. The structure contains linear centrosymmetric C3 units with a C-C bond length of 133(2) pm and isolated carbon atoms in octahedral coordination of four lutetium and two rhenium atoms. The rhenium atoms within the two-dimensionally infinite polymeric sheets [ReiC-tln are electronically saturated as is indicated by the diamagnetism and the semiconductivity of this carbide. Yf>2ReC2 was prepared by reacting the elements in a sealed tantalum tube with a high-frequency furnace. It crystallizes with a Pr2ReC2 type structure: Pnma, a = 645.91(6), b = 498.64(6), and c = 966.05(6) pm. Magnetic susceptibility measurements indicate the ytterbium atoms to be trivalent in this compound. | | | |
Reference
| Z. Naturforsch. 52b, 231—236 (1997); received November 15 1996 | | | |
Published
| 1997 | | | |
Keywords
| Crystal Structure, Magnetic Properties, Rare Earth Metal Rhenium Carbides, Polymeric Rhenium-Carbon Polyanions | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0231.pdf | | | | Identifier
| ZNB-1997-52b-0231 | | | | Volume
| 52 | |
| 64 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| Zinn(IV) | | | | Abstract
| Komplexe mit diaciden Azo(hydrazono)verbindungen. Kristallstruktur von Bis[4-(2'-hydroxyphenylazo)-3-methyl-l-phenyl-pyrazol-5-onato(2-)]zinn(IV) Tin(IV) Complexes with Diacidic Azo(hydrazono) Compounds. Crystal Structure of Bis[4-(2'-hydroxyphenylazo)-3-methyl-l-phenyl-pyrazol-5-onato(2-)]tin(IV) Wolfgang Banße3, Tin(IV) complexes of diacidic azo and hydrazono compounds were synthesized by the reaction of these ligands with SnCl2acac2 and SnCl2 • 2H20 , respectively. The complexes were further characterized by Mössbauer spectroscopy. For bis[4-(2'-hydroxyphenylazo)-3-methyl-l-phenyl-pyrazol-5-onato(2-)]tin(IV) force field calculations have been performed and the crystal structure was determined by X-ray analysis. | | | |
Reference
| Z. Naturforsch. 52b, 237—242 (1997); eingegangen am 16. Oktober 1996 | | | |
Published
| 1997 | | | |
Keywords
| Tin(I V) Complexes, Diacidic Azo Compounds, Mössbauer Spectroscopy, Molecular Mechanics Study, Crystal Structure | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0237.pdf | | | | Identifier
| ZNB-1997-52b-0237 | | | | Volume
| 52 | |
| 65 | Author
| W. Preetz, A. Krull | Requires cookie* | | | Title
| Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalysen von Tetrahalogenooxalatoosmaten (IV), [OsX4(ox)]2', X = Cl, Br, I Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of Tetrahalogenooxalatoosmates (IV), [OsX4(ox)]2~, X = Cl, Br, I | | | | Abstract
| The crystal structures of [(C5H5N)iC H 2][OsCl4(ox)] (monoclinic, space group I2/m, a = 10.260(5), b = 13.841(5), c = " 12.273(5) Ä, ß = 92.050(5)°, Z = 4), [(C5H5N)2CH2j[O sBr4(o x)]H 20(m onoclinic, space g ro u p P 2 ,/n ,a = 11.666(3),b = 11.591(5), c = 14.926(2) A, ß = 102.45(2)°, Z = 4) and [P(C6H5)4M O sI4(ox)]-2CH2C12 (triclinic, space group P i, a = 14.597(2), b = 11.9185(9), c = 22.5624(14) A, a = 80.284(8), ß = 78.903(8), 7 = 69.432(8)°, Z = 2) have been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra of the three complexes were measured at room temperature. Using the molecular parameters of the X-ray determinations normal coordinate analyses based on a modified valence force field have been performed and the normal modes o f vibration are assigned. With a set of 25 force constants and taking into account the innerligand vibrations a good agreement between observed and calculated frequencies has been achieved. The valence force constants of the X-Os-X axis are fd(OsCl) = 1.77, fd(OsBr) = 1.48, fd(OsI)o= 1.0 mdyn/A, of the X'-Os-O* axes are fd(O sCl') = 1.88, fd(OsBr') = 1.6, fd(OsI') =1.1 mdyn/A and fd(OsO*) ranges from 2.7 to 2.8 mdyn/A. | | | |
Reference
| Z. Naturforsch. 52b, 315—322 (1997); eingegangen am 27. November 1996 | | | |
Published
| 1997 | | | |
Keywords
| Tetrachlorooxalatoosmate(IV), Tetrabromooxalatoosmate(IV), Tetraiodooxalatoosmate(IV), Crystal Structure, Vibrational Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0315.pdf | | | | Identifier
| ZNB-1997-52b-0315 | | | | Volume
| 52 | |
| 67 | Author
| T. Koch, W. Preetz | Requires cookie* | | | Title
| Darstellung, n B-, 'H-NMR und Schwingungsspektren von 4-Aminopyridylundecahydro-c/oso-dodecaborat(l-) sowie Kristallstruktur von (Ph4As)[(4-(NH)-C5H4N)B12H11]*2CH3CN Synthesis, " B , 'H NM R and Vibrational Spectra o f 4-Aminopyridylundecahydro-c/oso- dodecaborate( 1-) and Crystal Structure o f (Ph4A s)[(4-(N H )-C5H4N )B 12H n ]-2CH3CN | | | |
Reference
| Z. Naturforsch. 52b, 939—942 (1997); eingegangen am 9. Juni 1997 | | | |
Published
| 1997 | | | |
Keywords
| 4-Am inopyridylundecahydro-c7(wododecaborate(l-), Crystal Structure, " B NMR Data, 1H NMR Data, Vibrational Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0939.pdf | | | | Identifier
| ZNB-1997-52b-0939 | | | | Volume
| 52 | |
| 68 | Author
| K. Dallmann, W. Preetz | Requires cookie* | | | Title
| Kristallstrukturen, Schwingungsspektren und Normalkoordinaten- analysen von cis-und ^rans-[OsX2(acac)2], X = Cl, Br, I Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of cis-and rrarcs-[OsX2(acac)2l, X = Cl, Br, I | | | | Abstract
| The crystal structures of frans-tOsCM acac)?] (triclinic, space group P i, a = 7.4114(5), | | | |
Reference
| Z. Naturforsch. 52b, 965—974 (1997); eingegangen am 12. Mai 1997 | | | |
Published
| 1997 | | | |
Keywords
| Crystal Structure, IR Spectra, Raman Spectra, Normal Coordinate Analysis, trans Influence | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0965.pdf | | | | Identifier
| ZNB-1997-52b-0965 | | | | Volume
| 52 | |
| 70 | Author
| Michael Feista, Sergej Trojanov3, Anja Stiewe3, Erhard Kemnitz3, Ralf Kunzeb | Requires cookie* | | | Title
| Synthese, Kristallstrukturen und thermisches Verhalten von (trienH2)[Mn(H20)3X 3]X * H20 (X=Cl,Br)* Synthesis, Crystal Structures and Thermal Behavior of (trienH2)[Mn(H20 ) 3X 3]X * H20 (X=Cl,Br) | | | |
Reference
| Z. Naturforsch. 52b, 1094—1102 (1997); eingegangen am 12. Mai 1997 | | | |
Published
| 1997 | | | |
Keywords
| Triethylenediammonium Triaquatrichloromanganate(II) Chloride Monohydrate, Triethylene-diammonium Triaquatribromomanganate(II) Bromide Monohydrate, Crystal Structures, Hy drogen Bonding, Thermal Analysis, DTA-TG, TG-MS | | | |
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| default:Reihe_B/52/ZNB-1997-52b-1094.pdf | | | | Identifier
| ZNB-1997-52b-1094 | | | | Volume
| 52 | |
| 71 | Author
| T. Koch, W. Preetz | Requires cookie* | | | Title
| Darstellung, n B-, 13C -,1 H-NMR-und Schwingungsspektren | | | | Abstract
| von 2,2' -Bipyridylundecahydro-c/oso-dodecaborat(1-) sowie Kristallstruktur von (Ph4As)[(2,2-C10H8N2)B12Hn ] CH3CN Synthesis, n B, 13C, 'H NMR and Vibrational Spectra of 2 ,2 '-Bipyridyl-undecahydro-c/o5o-dodecaborate(l-) and Crystal Structure of (Ph4As)[(2 ,2 '-C10H8N2)B 12H 1 1 ]-CH3CN | | | |
Reference
| Z. Naturforsch. 52b, 1165—1168 (1997); eingegangen am 17. Juli 1997 | | | |
Published
| 1997 | | | |
Keywords
| 2, 2'-Bipyridyl-undecahydro-c/oso-dodecaborate(l-), Crystal Structure, n B NMR Spectra, 1H NMR Spectra, 13C NMR Spectra, Vibrational Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-1165.pdf | | | | Identifier
| ZNB-1997-52b-1165 | | | | Volume
| 52 | |
| 72 | Author
| Karl Hensen3, Frank Gebhardta, Michael Bolteb | Requires cookie* | | | Title
| Synthese und Kristallstrukturbestimmung von Additionsverbindungen aus Alkyldimethylbromsilanen und N-Trimethylsilylimidazol Syntheses and Crystal Structure Determination of Addition Compounds of Alkyldimethylbromosilanes and N-Trimethylsilylimidazole | | | | Abstract
| The bromosilanes RMe2SiBr (R = Me, Et, n-Pr and /-Pr) form ionic l:l-compounds with N-trimethylsilylimidazole (NTMSI), stable at room temperature. Crystals of the compounds with R = Et, n-Pr and i-Pr are obtained by sublimation. From the product of the reaction of 1,1-dibromosilacyclopentane with NTMSI single crystals of N,N'-bis(trimethylsilyl)imidazolium-bromide (R = Me) were obtained. In the new adducts both silicon atoms are tetracoordinated. | | | |
Reference
| Z. Naturforsch. 52b, 1491—1496 (1997); eingegangen am 31. Juli 1997 | | | |
Published
| 1997 | | | |
Keywords
| Alkyldimethylbromosilanes (alkyl = Me, Et, «-Pr and /-Pr), N-Trimethylsilylimidazole, Lewis-Acid-Base Adducts, Crystal Structure | | | |
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| default:Reihe_B/52/ZNB-1997-52b-1491.pdf | | | | Identifier
| ZNB-1997-52b-1491 | | | | Volume
| 52 | |
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