| 122 | Author
| K. Barlos, H. Nöth, B. Wrackmeyer | Requires cookie* | | Title
| 4 N-NMR-Untersuchungen an Aminophosphinen 14 N NMR Studies on Aminophosphines  | | | Abstract
| Aminophosphines, Cyclic Noncyclic, 14 N NMR 14 N chemical shifts of a series of cyclic and noncyclic aminophosphines are reported. The nuclear shielding of nitrogen decreases with increasing number of halogen substituents at phosphorus as well as with increasing number of phosphinyl groups attached to nitrogen. In addition to the influence of electronegativity PN(jr)-interactions may account for the observed shielding. Steric effects are discussed. | | |
Reference
| Z. Naturforsch. 33b, 515—520 (1978); eingegangen am 2. März 1978 | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0515.pdf | | | Identifier
| ZNB-1978-33b-0515 | | | Volume
| 33 | |
125 | Author
| Tetraphenylphosphonium-Isopolymolybdates, Roger Grase, Joachim Fuchs | Requires cookie* | | Title
| Über Tetraphenylphosphonium-Isopolymolybdate  | | | Abstract
| From acidified sodium molybdate solutions mixtures of two polymolybdates are precipitated by addition of tetraphenylphosphonium ions. The pure compounds obtainable by separation with selective organic solvents were identified analytically and by their vibrational spectra as octamolybdate, [P(C6Hs)4]4Mo8026, with "Lindqvist structure" and as hexamolybdate, [P(C6Hs)4Mo60i9. They are characterized by their UV-VIS spectra and X-ray powder patterns. The precipitation of the hexamolybdate from strong acidic solution can be used analytically for the determination of molybdenum. | | |
Reference
| Z. Naturforsch. 33b, 533—536 (1978); eingegangen am 20. Januar 1978 | | |
Published
| 1978 | | |
Keywords
| Isopolymolybdates, Preparation, Vibrational Spectra, X-ray, UV | | |
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| default:Reihe_B/33/ZNB-1978-33b-0533.pdf | | | Identifier
| ZNB-1978-33b-0533 | | | Volume
| 33 | |
127 | Author
| Dieter Sellmann, Alfred Brandl, Ralf Endeil | Requires cookie* | | Title
| Wolfram-Carbonylkomplexe mit Stickstoff-Wasserstoff-Liganden [1] Tungsten Carbonyl Complexes with Nitrogen Hydride Ligands [1]  | | | Abstract
| Tungsten Nitrogen Hydride Complexes Synthesis, properties and reactions of [(OC)5W]2N2H2, [(OC)5W]2N2H4, (OC)5WN2H4, (OC)5WNH3, [(OC)4P03W]2N2H4, [(OC)4P03WN2H4], [(OC)5W-N2H2-W(CO)4P03], [(OC)5W-N2H2-W(CO)4P(CH3)3] and [(OC^WNHCHgNHCeHs] are reported. The hydrazine complexes are synthesized by ligand exchange from the corresponding tetra-hydrofuran complexes. Oxidation by various oxidizing agents yields the diazene complexes, in most cases very low yields. Substitution of CO by phosphanes leads to reduced stability of the compounds. All complexes undergo base catalysed H-D exchange yielding the corresponding ND derivatives; the diazene complexes show a much faster exchange than the corresponding hydrazine and ammonia complexes, which is explained by the higher acidity of the N2H2 protons. The diazene complexes disproportionate under base catalysis to hydrazine and dinitrogen compounds, the latter of which loose the N2 ligand immedi-ately. The diazene ligand of [(OC)sW]2N2H2 cannot be alkylated by reactions with (CH3)2S04, LiCH3 or CH2N2; instead, LiCH3 as well as CH2N2 cause disproportionation to N2H4 and N2 complexes. UV irradiation of [(OC)sW]2N2H2 in THF leads to substitution of CO by THF. The THF complexes can be converted to the phosphane substituted diazene complexes. The IR, UV-VIS and *H NMR spectra of the (OC)sW complexes are nearly identical to those of the analogous Cr and Mo compounds. The unsymmetrical phosphane diazene complexes, however, show a quartet of the N2H2 protons in the X H NMR spectra with coupling constants of 25-26 Hz for the protons on the NN double bond. This value points to a trans configuration of the diazene ligand and its complexes respectively. | | |
Reference
| Z. Naturforsch. 33b, 542—553 (1978); eingegangen am 1. Februar 1978 | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0542.pdf | | | Identifier
| ZNB-1978-33b-0542 | | | Volume
| 33 | |
128 | Author
| A. Zayed, J. Metri | Requires cookie* | | Title
| Benzo-benzothiopyranoquinoline Derivatives of Possible Antiparasitic Activity  | | | Abstract
| Benzo-benzothiopyranoquinoline, Benzoquinoline, Synthesis, Reactions, Antiparasitic Activity For possible antiparasitic activity, benzo-benzothiopyranoquinoline-6-malonaldehyde was synthesized and condensed with hydrazine hydrate, Phenylhydrazine and/or O-phenyle-nediamine. This afforded pyrazole, phenylpyrazole and diazepin derivatives respectively. | | |
Reference
| Z. Naturforsch. 33b, 554—556 (1978); received January 5 1978 | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0554.pdf | | | Identifier
| ZNB-1978-33b-0554 | | | Volume
| 33 | |
129 | Author
| Ivan Juchnovski, Rositza Kuzmanova, Jordan Tsenov, Jose Kaneti, Ivan Binev | Requires cookie* | | Title
| Structural Effects on Nitrile Infrared Integrated Intensities of Alpha,Beta-Diaryl Cyanoethylenes: Hammett and Quantum Chemical Approaches  | | | Abstract
| Cyanostilbenes, IR The nitrile infrared intensities of a series of a,)S-diaryl cyanoethylenes were juxtaposed to the associated substituent constants, HMO and SCF-MO indices and fair to excellent correlations were established. The competitive resonance of the nitrile group with alpha-and beta-aryl substituents is discussed. HMO calculations were used to estimate the steric hindrance to conjugation caused by polycyclic substituents and SCF-MO calculations were made to obtain uniform predictions of nitrile intensities and frequencies for hetero-cyclic derivatives of acrylonitrile. | | |
Reference
| Z. Naturforsch. 33b, 557—563 (1978); received December 30 1977 | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0557.pdf | | | Identifier
| ZNB-1978-33b-0557 | | | Volume
| 33 | |
133 | Author
| Hubert Schmidbaur, Peter Holl | Requires cookie* | | Title
| Die Reaktion eines gemischten Doppelylids mit Ethylenoxid Reaction of a Mixed Double Ylide with Ethylene Oxide  | | | Abstract
| Dimethyl-trimethylphosphinimino-methylene-phosphorane, (CH3)3P=N-P(CH3)2 = CH2 was found to react with ethylene oxide to form a 1:1 adduct, that was identified as 2,2-dimethyl-2-trimethylphosphinimino -1,2 A 5 -oxaphospholane. According to its 1 H, 13 C, 31 P NMR spectra it is assigned a rigid trigonal bipyramidal structure with nitrogen and oxygen atoms in axial positions. | | |
Reference
| Z. Naturforsch. 33b, 572—573 (1978); eingegangen am 28. Februar 1978 | | |
Published
| 1978 | | |
Keywords
| Ylides, Ethylenoxide, 1, 2-Oxaphospholane | | |
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| default:Reihe_B/33/ZNB-1978-33b-0572_n.pdf | | | Identifier
| ZNB-1978-33b-0572_n | | | Volume
| 33 | |
135 | Author
| Nils Wiberg, Gerhard Hübler | Requires cookie* | | Title
| Über Derivate des Hydrazins, VIII [1] Bis(trimethylsilyl)amino-isocyanat und -isothiocyanat  | | | Abstract
| Aminoisocyanate, Aminoisothiocyanate, Adducts of Heterocumulenes, Lithium Silylhydrazides Bis(trimethylsilyl)aminoisocyanate (1) is formed by reaction of the hydrazides LiN2(SiMe3)3 or Li2N2(SiMe3)2 with phosgene. Bis(trimethylsilyl)aminoisothiocyanate (2) is obtained by thermolysis of the hydrazide (Me3Si)3N2CSSLi, which is readily prepared from LiN2(SiMe3)3 and carbon disulfide. (It is generally found that LiN2(SiMe3)3 and Li2N2(SiMe3)2 add to heterocumulenes X=C=Y (X = TosN, O, S; Y = 0, S), and that reaction of the addition products with Me3SiCl yields (Me3Si)3N2CXYSiMe3. While 1 is obtained solely as a thermostable dimer, 2 is a thermolabile monomer). Thermolysis of 2 at ambient temperature yields (Me3Si)4NiC2S and (Me3Si)4NiC2S3. Thermolysis of 2 in ether solution at elevated temperatures mainly yields bis(trimethylsilyl)carbodiimide and sulfur. | | |
Reference
| Z. Naturforsch. 33b, 575—582 (1978); eingegangen am 27. Februar 1978 | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0575.pdf | | | Identifier
| ZNB-1978-33b-0575 | | | Volume
| 33 | |
136 | Author
| WilliamS. Sheldrick, Alfred Schmidpeter, Thomas Von Criegern | Requires cookie* | | Title
| Die Kristallstruktur von 2.2'-Bipyridin-bis(brenzkatechyl)phosphoniiim- hexafluorophosphat Crystal Structure of 2,2'-Bipyridine-bis(o-phenylenedioxy)phosphonium Hexafluorophosphate  | | | Abstract
| 2,2'-Bipyridine-bis(o-phenylenedioxy)phosphonium hexafluorophosphate crystallises in the monoclinic space group C2/c (Z = 8) with a = 18.654(4), b = 10.131(2), c = 24.344(4) A, ß = 99.53(4)°. The cationic phosphorus atom displays an octahedral coordination slightly distorted towards the tetrahedral one of an uncomplexed phosphonium center. The OPO bond angles are between 91.6 and 95.7(2)°, the NPN angle of the bipyridine chelate ring in contrast is only 81.7(2)°. The ring systems of the bipyridine ligand are inclined slightly to one another at an angle of 4.7°. The bond lengths to the cationic phosphorus are P-0 1.668-1.672(3), P-N 1.896(4) and 1.898(4) A. The hexafluorophosphate anion is disordered. | | |
Reference
| Z. Naturforsch. 33b, 583—587 (1978); eingegangen am 30. März 1978 | | |
Published
| 1978 | | |
Keywords
| Hexacoordinate Cationic Phosphorus, Octahedral Distortion, Bipyridine Chelate, Benzodioxaphosphole Ring, Coordinative PN Bond Distance | | |
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| default:Reihe_B/33/ZNB-1978-33b-0583.pdf | | | Identifier
| ZNB-1978-33b-0583 | | | Volume
| 33 | |
140 | Author
| Gerhard Thiele, Peter Hilfrich | Requires cookie* | | Title
| Über Cyanatomercurate M2Hg3(NCO)8 (M = K, Rb, Cs) - Synthesen, Kristallstrukturen und Schwingungsspektren On Cyanatomercurates M2Hg3(NCO)8 (M = K, Rb, Cs) - Syntheses, Crystal Structures and Vibrational Spectra  | | | Abstract
| By mixing aqueous solutions of Hg(CH3COO)2 and MOCN (M = K, Rb, Cs) the tri-clinic compounds M2Hg3(NCO)8 are formed. In a first approximation the crystal structure analysis indicates isolated Hg(NCO)2 molecules besides K+ and NCO~ ions. As in the range of van der Waals radii additional NCO-neighbours are noticed the mercury atoms are surrounded by distorted octahedra. The octahedra around 2/3 of the Hg form infinite chains as in KHg(NCO)3 which are linked together by additional Hg(NCO)2 molecules. Therefore the compound can be formulated as a double salt 2 KHg(NCO)3 • Hg(NCO)2. The vibrational spectrum is discussed. Rb2Hg3(NCO)8 is isotypous while the caesium salt has a double cell volume. | | |
Reference
| Z. Naturforsch. 33b, 597—602 (1978); eingegangen am 20. März 1978 | | |
Published
| 1978 | | |
Keywords
| Cyanatomercurate, Cyanato Complexes, Crystal Structure, Vibrational Spectra | | |
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| default:Reihe_B/33/ZNB-1978-33b-0597.pdf | | | Identifier
| ZNB-1978-33b-0597 | | | Volume
| 33 | |
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