New lanthanide dimethyl‐N‐benzoylamidophosphate (HL) based tetrakis‐complexes NEt4[LnL4] (Ln3+=La, Nd, Sm, Eu, Gd, Tb, Dy) are reported. The complexes are characterized by means of NMR, IR, absorption, and luminescent spectroscopy as well as by elemental, X‐Ray, and thermal gravimetric analyses. The phenyl groups of the four ligands of the complex anion are directed towards one side, while the methoxy groups are directed in the opposite side, which makes the complexes under consideration structurally similar to calixarenes. The effect of changing the alkali metal counterion to the organic cation NEt4+ on the structure and properties of the tetrakis‐complex [LnL4]‐ is analyzed. The complexes exhibit bright characteristic for respective lanthanides luminescence. Rather high intensity of the band of 5D0→7F4 transition, observed in the luminescence spectrum of NEt4[EuL4], is discussed based on theoretical calculations.

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A series of pentanuclear lanthanide complexes Ln 5 L 6 (μ-L) 4 (μ 3 -OH) 4 (μ 4 -OH) (Ln III = Nd, Dy, Ho, Er, Yb; L − = dimethyl N-benzoylamidophosphate ion, [C 6 H 5 C(O)−N−P(O)(OCH 3 ) 2 ] − ) was obtained by the reaction of sodium dimethyl N-benzoylamidophosphate with the corresponding lanthanide nitrates. The pentanuclear cores formed as a result of selfarrangement and their composition did not depend on the lanthanide ion. The complexes and sodium dimethyl Nbenzoylamidophosphate have been characterized by single-crystal X-ray diffraction. The absorption spectra of the complexes were measured at 300 and 4 K. The dysprosium and ytterbium complexes exhibited weak emission in the visible and IR regions, respectively. Temperature dependences of magnetic susceptibility (χ M ) of the dysprosium, holmium, and erbium compounds were studied. It was found that χ M vs T dependences were governed by the crystal field splitting effects with the Δ parameter being in the range 5−17 cm −1 . Slow magnetic relaxation was found for the dysprosium complex by ac magnetic measurements, while no significant out-of-phase signals were detected for holmium and erbium complexes.

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