X-ray structure of 18-crown-6-KClO₄ at room temperature and 20 K

Abstract

Abstract

Syntheses, Vibrational Spectra, and Theoretical Studies of the Adamantanoid Sn4Ch104- (Ch = Se, Te) Anions: X-ray Crystal Structures of [18-Crown-6-K]4[Sn4Se10]·5en and [18-Crown-6-K]4[Sn4Te10]·3en·2THF

“…The geometrical parameters of the Sn 4 Se 10 4-anion are in agreement with those previously reported for [2,2,2-crypt-K] 4 -[Sn 4 Se 10 ] (Sn-Se b , 2.533(2)-2.562(2) Å, and Sn-Se t , 2.416-(2)-2.433(2) Å; ∠Se b -Sn-Se b , 107.16(6)-113.06(6) o , and ∠Se t -Sn-Se b , 103.55(7)-12.96(6) o ) 2 and for [Å; ∠Se b -Sn-Se b , 109.22(9)-110.17(10) o , and ∠Se tSn-Se b , 106.50(12)-111.87(12) o ). 3The C-O and C-C bond distances within the crown ether moieties are in good agreement with those reported previously36 and are not discussed further. Each structural unit contains four 18-crown-6 molecules chelated to K + cations which complete their coordination by bridging to the nitrogen atoms of en and/ Views of (a) the Sn4Te10 4-anion and (b) the solvated 18-crown-6-K + cations in[18-crown-6-K]4[Sn4Te10]‚3en‚2THF with displacement ellipsoids drawn at the 70% probability level.…”

“…The K + ions of the Sn 4 Te 10 4-salt are located well inside the cavity of the macrocycle; that is, their distance from the least-squares plane through the six O atoms of 18-crown-6 is -0.019 to 0.099 Å. In Sn 4 Se 10 4-, two K + ions are located inside the cavity of the macrocycle (-0.112 to 0.082 Å from the O 6 -plane), whereas one K + ion is slightly displaced from the O 6 -plane (-0.278 Å), which likely results from a weak K(3)‚‚‚N interaction at 3.273 (7) 36 The (18-crown-6-K(3)) + and (18-crown-6-K(4)) + anions of the Sn 4 Te 10 4-salt are positionally disordered and occupy the same site in two equally populated orientations. In each case, the two orientations are related by a 30°rotation about an axis that passes through K(3) or K(4) and is perpendicular to the least-squares planes defined by the six crown oxygen atoms.…”

Color modulation for intramolecular charge‐transfer‐induced chemiluminescence of 1,2‐dioxetanes

“…Therefore, the order of interaction between the anthrylphenoxide anion and the central potassium ion may be reversed: 34a < 34b < 34d < 34c . In any event, the sizes of crown ethers 34a–34c are apparently only slightly different from each other, although 34d , which has benzyl groups, is far bulkier than the others 45–47. Thus, the color change of the chemiluminescence observed for 32 apparently reflects the steric interaction of the anthracene ring of 33 (32) with the [K⊂(crown ether)] + .…”

Polysulfonylamine, LI [1]. Synthese von zwei Kronenether-Komplexen des Kaliumdimesylamids und Kristallstruktur von [K(18-Krone-6)] [N(SO2CH3)2] • 2 CH3OH bei —95°C / Polysulfonylamines, LI. Synthesis of Two Crown Ether Complexes of Potassium Dimesylamide and Crystal Structure of [K(18-Crown-6)][N(SO2CH3)2] • 2 CH3OH at –95°C

“…290,56(30) K -0 (6 ) 297,05(30) K -0 (8 ) 283,78(28) K -0 (9 ) 284,54(29) 0 ( l) -K -0 ( 8 ) 82,44 (8) (9) 76,65(7) 0 (5 )-K -0 (9) 79,35(7) 0 (6 ) -K -0 ( 9 ) 114,19(8) 0 (8 )-K -0 (9) 63,79(7) K -O -C 104,74(21) bis 123,77(22) S (l)-0 (7 ) 143,94(28) S (l)-0 (8 ) 145,31(25) S (2)-0 (9) 145,23(26) S (2)-0(10) 144,35(26) 0 (7 ) -S ( l)-0 (8 ) 116,05(16) 0 (9 ) Die Bindungslängen und -winkel des Dimesylamid-Liganden (Tab. II) unterscheiden sich nur ge ringfügig von denen des gleichen Anions im ein gangs erwähnten Natrium-Komplex; bezüglich ei niger Einzelheiten wird daher auf Lit.…”

“…III) weist die für Kronenether-Strukturen charakteristischen [6] V erkür zungen der C -C -A bstände (147,2, M ittel wert 148,6 pm) gegenüber dem Standardwert 153,0 pm für C(sp3) -C(sp3) [7] auf, während die C -O -A bstände (142,5,Mittelwert 143,0 pm) erwartungsgemäß nicht wesentlich vom Standard wert 142,6 pm für C(sp3) -0 abweichen. Die V er kürzung der C -C -A bstände ist vermutlich nicht, wie früher angenommen, ein therm ischer Effekt, denn sie wird auch in der bei 20 K durch R öntgen beugung ermittelten Struktur von ]-C104 beobachtet (M ittelwert 149,6 pm) [8]. D er E r wartung entsprechend [6] liegen die O -C -C -W inkel im Bereich 108,0-109,9°, die C -O -C -W in k e l im Bereich 111,2-112,4°.…”