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The title compound (C31H55N2O13P3) crystallizes in the triclinic space group P$\bar 1$ with a=12.676(4) Å, b=13.733(3)Å, c=14.042(2)Å, α=67.94(4)°, β=77.15(4)°, γ=61.95(4)°, V=1996.2(8)Å3, Z=2, Dx =1.259 g.cm‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R=0.055). The macrocyclic ligand is an 18‐membered lariat ether containing two N and three etheral O atoms and two phosphonate side groups. The title compound consists of the macrocyclic ligand, one ethyl phosphonic acid and one water molecule, as a whole. In the macrocyclic ring, the mean N...O distance is 5.481(6) Å. The relative macrocyclic inner hole size, estimated as twice the mean distance of the donor atoms from their centroid is approximately 2.29 Å.

The title compound, C(45)H(55)NO(6)P(2), consists of an acyclic P=N-P(O) monophosphazene chain and five bulky 2,4,6-trimethylphenoxy side groups which predominantly determine the molecular shape. Although the P-N single [1.586 (3) A] and P=N double [1.517 (3) A] bonds are significantly different from each other, both are substantially shorter than the ideal P-N single bond. The P-N-P angle [146.0 (2) degrees ] corresponds to the upper limit reported for acyclic phosphazene derivatives in the literature.

Macrocyclic multidentate N2O2 donor-type ligands have been investigated previously as potential metal-ion-selective reagents. 1,2 A series of these investigations have involved the synthetic, thermodynamic and structural properties of selective complex formation of a number of transition metal ions. 3 There are only a few reports about the structures of the free macrocyclic multidentate N2O2 and N2O3 donor-type ligands. [4][5][6] The title compound was prepared from the reduction of the reaction product of 1,5-bis(2-formylphenyl)-1,5-dioxapentane (2.84 g, 0.01 mol) and 1,3-diaminopropane (0.74 g, 0.01 mol) by NaBH4 (2.00 g, 0.05 mol) in THF-MeOH mixture (1:1). The residue was dissolved in CHCl3-light petroleum (1:1) and set aside for crystallization at ambient temperature [m.p. 91˚C and yield 1.4 g (49%)].The structure determination was carried out in order to estimate the relative macrocyclic ring hole size of the molecule. The intramolecular distances N1···O1 4.057 (3)