10.1002/chem.201904253
Chemistry - A European Journal
NMR (400 MHz, CD3CN, ppm): δ 9.40 (d, 2H), δ 7.27 (dd, 2H), δ 7.17 (dd, 2H), δ 6.69 (t,
2H), δ 4.65 (t, 2H), δ 4.55 (m, 2H), δ 4.20 (m, 2H), δ 4.10 (s, 6H), δ 3.54 (m, 2H).
Complex 4. Yield 0.228 g (60%) C20H23ClN3NaO10U (760.87). Calculated C, 31.53; H, 3.04;
N, 5.52; Found C, 31.59; H, 2.96; N, 5.56; IR: ν(N–H) = 3241 cm–1, ν(C=N) = 1631 cm–1, ν(UO2
asymmetric stretching) = 898 cm–1, ν(ClO4) = 1089 cm–1. ESI-MS (positive ion mode, CH3CN)
calcd. m/z = 640.22 and 662.20; found at m/z = 640.22 and 662.20 which are assigned as
[UO2L2 + H]+ and [UO2L2 + Na]+ respectively. 1H NMR (400 MHz, CD3CN, ppm): δ 9.41 (s,
2H), δ 7.24 (d, 2H), δ 7.15 (d, 2H), δ 6.65 (t, 2H), δ 4.64 (t, 2H), δ 4.54 (m, 2H), δ 4.16 (m,
2H), δ 4.08 (s, 6H), δ 3.52 (m, 2H).
Complex 5. Yield 0.252 g (61%) C20H25AgN4O10U (827.34). Calculated C, 29.03; H, 3.05;
N, 6.77; Found C, 28.95; H, 3.01; N, 6.82; IR: ν(N–H) = 3186 cm–1, ν(C=N) = 1627 cm–1, ν(UO2
asymmetric stretching) = 892 cm–1, ν(NO3) = 1384 cm–1. ESI-MS (positive ion mode, CH3CN)
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calcd. m/z = 746.11; found at m/z = 746.12, which are assigned as [UO2L2 +Ag]+. H NMR
(400 MHz, CD3CN, ppm): δ 9.41 (s, 2H), δ 7.22 (dd, 2H), δ 7.14 (dd, 2H), δ 6.63 (t, 2H), δ
4.64 (t, 2H), δ 4.53 (m, 2H), δ 4.16 (m, 2H), δ 4.07 (s, 6H), δ 3.51 (m, 2H).
Complex 6. Yield 0.225 g (60%) C40H50F6KN6O14PU2 (1498.67). Calculated C, 32.05; H,
3.36; N, 5.61; Found C, 32.09; H, 3.31; N, 5.65; IR: ν(N–H) = 3233 cm–1, ν(C=N) = 1629 cm–1,
ν(UO2 asymmetric stretching) = 872 cm–1, ν(PF6) = 845 cm–1. ESI-MS (positive ion mode,
CH3CN) calcd m/z = 678.17 and 640.22; found at m/z, 678.58 and 640.59 which are assigned
as [UO2L2 + K]+ and [UO2L2 +H]+ respectively. 1H NMR (400 MHz, CD3CN, ppm): δ 9.45
(s, 2H), δ 7.19 (d, 2H), δ 7.17 (d, 2H), δ 6.67 (t, 2H), δ 4.66 (m, 2H), δ 4.56 (m, 2H), δ 4.23
(m, 2H), δ 3.96 (s, 6H), δ 3.56 (m, 2H).
Physical measurements
Elemental analyses (C, H and N) were performed using a Perkin–Elmer 2400 series II CHN
analyzer. IR spectra in KBr pellets (4000–400 cm−1) were recorded using a Perkin-Elmer RXI
FTIR spectrophotometer. The electronic absorption spectra (500–250 nm) in acetronitrile
solution were collected in a Hitachi U-3501 spectrophotometer. ESI mass spectra were
recorded on a WATERS Xevo G2-S QTof mass spectrometer in HRMS grade acetronitrile.
1H NMR spectra were recorded in CD3CN solvent for complexes 1−6 in a Bruker 400 MHz
NMR instrument, where tetramethylsilane was used as an internal standard.
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