| | 1 | Author
| Stefan Horstmann, Wolfgang Schnick | Requires cookie* | | | Title
| Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumchlorid [P(NH2)4]C1 Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Chloride [P(NH2)4]C1  | | | | Abstract
| [P(NH2)4]C1 has been prepared by ammonolysis of phosphorus pentachloride in liquid ammonia. The product was purified by reacting the byproduct, ammonium chloride, with diethylamine and removing the diethylamine hydrochloride. Suitable single crystals were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. The crystal structure of [P(NH2)4]C1 has been determined by single crystal X-ray methods (Pbcn, a = 470.8(2), b = 1622.3(3), c = 756.3(2) pm, Z = 4). In the solid, [PfNH2)4]+ and Cl~ ions are found, resembling a Til-analogous structure. The N -H -C l distances indicate N -H — Cl hydrogen bonding interactions. The distortion of the P-N sceleton of the cation and the very short P -N H 2 distances (mean value: 161.2 pm) have been confirmed by ab initio calculations, which show a generalized anomeric effect of the electron pairs at nitrogen and pjrdjr bonding. | | | |
Reference
| (Z. Naturforsch. 51b, 127—132 [1996]; eingegangen am 18. Mai 1995) | | | |
Published
| 1996 | | | |
Keywords
| Tetraaminophosphonium Salt, Synthesis, Crystal Structure, Vibrational Spectroscopic Data | | | |
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| default:Reihe_B/51/ZNB-1996-51b-0127.pdf | | | | Identifier
| ZNB-1996-51b-0127 | | | | Volume
| 51 | |
| 2 | Author
| Stefan Horstmann, Wolfgang Schnick | Requires cookie* | | | Title
| Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumiodid [P(NH2)4]I Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Iodide [P(NH2)4]I | | | | Abstract
| The title compound has been prepared starting from phosphorothionic triamide SP(N H 2)3 by methylation of the sulfur atom and subsequent ammonolysis reaction in dry acetonitrile and dichloromethane, respectively, both at room temperature. Suitable single crystals are obtained from an acetonitrile solution in a temperature gradient between 70 °C and room temperature. The crystal structure o f [P(N H 2)4]I has been determined by single crystal X-ray methods (P 4!nbm\ a = 842.6(2), c = 486.7(2) pm, Z = 2). In the solid [P(NH2)4]+-and I~-ions are found with significant N -H -I -h y d r o g e n bonding interactions between anions and cations (H —I: 276.4 pm). The P -N -b o n d length in the cation (160.7(2) pm) represents the shortest P -N H 2 bond distance reported to date indicating a significant electrostatic strengthening. The condensation behaviour of [P(N H 2)4]I in solution and in the solid has been investigated. | | | |
Reference
| Z. Naturforsch. 49b, 1381—1386 (1994); eingegangen am 5. Mai 1994 | | | |
Published
| 1994 | | | |
Keywords
| Tetraaminophosphonium Salt, Synthesis, Crystal Structure, Hydrogen Bonding, Condensation Reactions | | | |
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| default:Reihe_B/49/ZNB-1994-49b-1381.pdf | | | | Identifier
| ZNB-1994-49b-1381 | | | | Volume
| 49 | |
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