Synthesis, vibrational spectra, and crystal and molecular structure of 1,5-bis[2-(dihydroxyphosphinyl)phenoxy]-3-oxapentane dihydrate [(HO)2(O)P(C6H4)(OCH2CH2)2O(C6H4)P(O)(OH)2(H2O)] · H2O

• Published in: Russian journal of inorganic chemistry 2011-08, Vol.56 (8), p.1222-1231
• Main Authors: Baulin, V. E., Minacheva, L. Kh, Ivanova, I. S., Pyatova, E. N., Churakov, A. V., Baulin, D. V., Sergienko, V. S., Tsivadze, A. Yu
• Format: Article
• Language: English
• Subjects: Chemistry; Chemistry and Materials Science; Coordination Compounds; Ethers; Hydrogen bonds; Hydroxyl groups; Inorganic Chemistry; Locks; Molecular structure; Reflection; Rings (mathematics); Synthesis
• ISSN: 0036-0236; 1531-8613
• DOI: 10.1134/S0036023611080043

A modified method of synthesis of a phosphoryl podand, 1,5-bis[2-(dihydroxyphosphinyl)phenoxy]-3-oxapentane (L), has been developed. The IR spectra of this podand and its dehydrate (L [L · H 2 O] · H 2 O ( I ) have been studied, the structure of I has been determined by X-ray crystallography. The crystals are orthorhombic, a = 9.4006(19) Å, b = 25.494(5) Å, c = 8.4264(17) Å, V = 2019.5(7) Å 3 , Z = 4, space group Pna 2 1 , R = 0.0512 for 3016 reflections with I > 2σ( I ). Compound I is a host-guest molecular complex. Phosphoryl podand L acts as a host molecule, and one of the water molecules (H 2 O(11)) is a guest. This molecule forms one donor and one acceptor intramolecular hydrogen bond with hydroxyl groups of two phosphoryl groups (O(8)H(4) and O(3)H(2)) and combines them into an 18-membered macrocyclic ring, acting as a kind of “lock.” The H 2 O(11) molecule forms a second donor intramolecular hydrogen bond with the O(5) ether atom. The neutral molecular complexes are linked by hydrogen bonds directly and through the second water molecule (H 2 O(10)) into chains running along the c axis.