Synthesis, crystal structure and ab initio/DFT calculations of a derivative of dithiophosphonates.

The compound 2 has been synthesized from the reaction of 2,4-Bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide and (R)-1-[3,5-Bis(trifloromethyl)phenyl]ethanol in toluene. The obtained crude dithiophosphonic acid 1 has been treated with the excess of N(C2H5)3 to give rise to 2, [(+HN(C2H5)3][O-CH3CH-C6H3(CF3)2)(CH3OC6H4)PS2(-)]. The compound 2 has been characterized by using the spectroscopic methods such as IR, (1)H, (13)C, (31)P NMR and structural analysing method such as X-ray crystallography. It crystallizes in the orthorhombic system, whose space group is P212121. It consists of a dithiophosphonate bridged methoxyphenyl and bis(triflorophenylethyl) groups and a triethylammonium moiety linked by N-H⋯S and C-H⋯F hydrogen bonds. In the crystal structure, the C17H14F6O2PS2 molecule is elongated along the b-axis and stacked along the a-axis. The triethylammonium, N(CH2CH3)3, molecule fill in the cavities between the C17H14F6O2PS2 molecule. Moreover, ab initio methods based on Hartree-Fock (HF) and Density Functional Theory (DFT) calculations with the basis set of 6-31G(d) are also carried out to determine the molecular structural properties and to calculate FT-IR and NMR spectrum of the compound 2. The experimental results and theoretical calculations have been compared, and they are found to be in good agreement.

Diaqua-bis(2-chloro-benzoato-κO)bis-(N,N-diethyl-nicotinamide-κN)manganese(II).

In the monomeric title complex, [Mn(C(7)H(4)ClO(2))(2)(C(10)H(14)N(2)O)(2)(H(2)O)(2)], the Mn(II) atom is located on a crystallographic centre of inversion. The asymmetric unit contains one 2-chloro-benzoate (CB) ligand, one diethyl-nicotinamide (DENA) ligand and one coordinated water mol-ecule, all ligands being monodentate. The four O atoms in the equatorial plane around the Mn atom form a slightly distorted square-planar arrangement, while the slightly distorted octa-hedral coordination is completed by the two pyridine N atoms of the DENA ligands in the axial positions. The dihedral angle between the carboxyl group and the adjacent benzene ring is 77.9 (11)°, while the pyridine and benzene rings are oriented at a dihedral angle of 45.94 (5)°. In the crystal structure, inter-molecular O-H⋯O hydrogen bonds link the mol-ecules into infinite chains.

trans-2,4,4,6,8,8-Hexamorpholino-2,6-bis(n-propylamino)cyclo-2lambda5,4lambda5,6lambda5,8lambda5-tetraphosphazatetraene.

The title compound, C(30)H(64)N(12)O(6)P(4), consists of a centrosymmetric chair-shaped cyclic tetrameric phosphazene ring with six bulky morpholino and two n-propylamino side groups. The two n-propylamino side groups are in trans positions. The bulky substituents mainly determine the eight-membered-ring conformation. The endocyclic N-P-N angles around the P atoms having different substituents are not the same as the P-N-P angles of the macrocyclic ring.

4-Methylcarbazole-3-carboxylic acid.

The title compound, C(14)H(11)NO(2), consists of a carbazole skeleton with carboxylic acid and methyl groups at positions 3 and 4, respectively. Molecules are linked about inversion centres by O-H.O hydrogen bonds [O.O 2.620 (3) A] to form centrosymmetric dimers.

N-[Bis(2,4,6-trimethylphenoxy)phosphinoyl]-P,P,P-tris(2,4, 6-trimethylphenoxy)phosphazene.

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.