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| FrankW. Eller, Harald Borgholte, H. Arald Stenger, Stefan Vogler, Kurt Dehnicke | Requires cookie* | | | Title
| Synthesen und Kristallstrukturen der Kronenether-Komplexe (18-Krone-6) * 2 CH3CN, [Na-15-Krone-5][Re04] CH3CN und [Na-15-Krone-5]PF6 Syntheses and Crystal Structures of the Crown E ther Complexes (18-C row n-6)-2C H 3CN, [N a-15-Crow n-5][Re04] * C H 3CN, and [Na-15-Crown-5]PF6  | | | | Abstract
| Single crystals o f (18-crow n -6)-2C H 3CN were obtained by cooling a solution o f 18-crown-6 in acetonitrile to 4 °C. Space group P 2 x/n, Z = 2, 629 observed independent reflexions, R = 0.062. Lattice dim ensions at 19 °C: a = 911.7(1), b = 852.0(1), c = 1370.0(2) pm; ß — 104.61(1)°. The com pound forms a m olecular structure with approximate D 3d symmetry o f the crown ether m olecule, and C —H -O interactions of the acetonitrile m olecules with the crown ether, the H ---0 distances being 243, 253, and 267 pm , respectively. [N a-15-crow n-5][R e04] • C H 3CN is formed as a by-product o f the reaction o f R eN C l4 with sodium fluoride in acetonitrile in the presence o f 15-crown-5 and traces o f water. Space group P 1, Z = 2, 3107 observed independent reflexions, R = 0.045. Lattice dim ensions at 19 °C: a — 823.4(1), b = 1078.8(1), c = 1204.0(1) pm; a = 112.40(1)°, ß = 94.35(1)°, y = 104.63(1)°. The com pound forms ion pairs, in which the sodium atom is sixfold coordinated by the five oxygen atoms o f the crown ether m olecule, as well as by one oxygen atom o f the R e 0 4~ ion, which is only slightly distorted. The bond length Na — 0 R e 0 3 is 237.8(8) pm , the bond angle N aO R e is 164.3(5)°. [Na-15-crown-5]PF6 is formed in the reaction o f [R eC l3(N SC l)2 • PO C l3] with sodium fluoride in acetonitrile solution in the presence o f 15-crown-5. Space group P na2,, Z = 4, 1130 observed independent reflexions, R = 0.123. The high R value is due to disorder of the skeletal atoms of the crown ether m olecule. The com pound forms ion pairs, in which the sodium atom is sevenfold coordinated by the five oxygen atom s o f the crown ether m olecule, as well as by two fluorine atom s o f the PF6~ ion with N a —F bond lengths o f 240(2), and 246(2) pm, respectively. | | | |
Reference
| Z. Naturforsch. 44b, 1524 (1989); eingegangen am 25. Juli/5. September 1989 | | | |
Published
| 1989 | | | |
Keywords
| Crown Ether C om plexes, Syntheses, IR Spectra, Crystal Structure | | | |
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| ZNB-1989-44b-1524 | | | | Volume
| 44 | |
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