F. F. Chausov

Synthesis, structure, and properties of nickel complexes with nitrilotris(methylenephosphonic acid) [Ni(H2O)3N(CH2PO3H)3] and Na4[Ni(H2O)N(CH2PO3)3] ∙ 11H2O

Nitrilotris(methylenephosphonato)triaquanickel and tetrasodium nitrilotris(methylenephosphonato) aquanickelate undecahydrate were synthesized and characterized. The crystal of [Ni(H2O)3N(CH2PO3H)3] is composed of linear coordination polymers and belongs to sp. gr. P21/c, Z = 4, a = 9.17120(10) Å, b = 16.05700(10) Å, c = 9.70890(10) Å, β = 115.830(2)°. The Ni atom is in an octahedral coordination formed by two oxygen atoms of one phosphonate ligand, one oxygen atom of another ligand molecule, and three water molecules in a meridional configuration. The crystal of Na4[Ni(H2O)N(CH2PO3)3] ∙ 11H2O has an island dimeric chelate structure and belongs to sp. gr. С2/c, Z = 8, a = 18.7152(2) Å, b = 12.05510(10) Å, c = 21.1266(2) Å, β = 104.4960(10)°. The Ni atom has a slightly distorted octahedral coordination involving one nitrogen atom and closes three five-membered N–C–P–O–Ni rings sharing the Ni–N bond.

Nitrilotris(methylenephosphonato)potassium K[μ6-NH(CH2PO3)3H4]: Synthesis, structure, and the nature of the K–O chemical bond

The crystal structure of nitrilotris(methylenephosphonato)potassium K[μ6-NH(CH2PO3)3H4]—a three-dimensional coordination polymer—was determined. The potassium atom is coordinated by seven oxygen atoms belonging to the six nearest ligand molecules, resulting in distorted monocapped octahedral coordination geometry. The complex contains the four-membered chelate ring K–O–P–O. The K–O chemical bond is predominantly ionic. Meanwhile, the bonds of the potassium atom with some oxygen atoms have a noticeable covalent component. In addition to coordination bonds, the molecules in the crystal packing are linked by hydrogen bonds.

Chelate complexes of lead(II) with nitrilotris(methylenephosphonic) acid [Pb{μ5-NH(CH2PO3H)3}] and Na4[Pb2(H2O)2{μ3-N(CH2PO3)3H2}2] · 10H2O: Synthesis, structure, and asymmetry of lone 6s pair

Two complexes of Pb(II) with nitrilotris(methylenephosphonic) acid are synthesized and their crystal structures are determined. Nitrilotris(methylenephosphonato)lead(II) [Pb{μ5-NH(CH2PO3H)3}] is a coordination 3D polymer; space group Pī, Z = 2. The coordination polyhedron of Pb is a distorted pentagonal bipyramid with the N atom at one of the equatorial positions. Tetrasodium bis[aquanitrilotris(methylenephosphonatoplumbate( II)] decahydrate Na4[Pb2(H2O)2{μ3-N(CH2PO3)3H2}2] · 10H2O crystallizes in space group Pī, Z = 2. The degree of asymmetry of the coordination polyhedra of lead atoms characterizing the localization of the lone 6s electron pair is estimated.

The trisodium monohydrogen-nitrilo-tris-methylenephosphonato-hydroxylaminato-nitrosyl-molybdate octahydrate Na3[Mo(NO)(NH2O){N(CH2PO3)3H}] · 8H2O: Synthesis, structure, and nature of coordination bond of transition metal with non-innocent ligand

The sodium salt of heteroleptic molybdenum complex with nitrilotris(methylenephosphonic) acid (NTP), hydroxylamine, and nitrogen(II) oxide Na3[Mo(NO)(NH2O){N(CH2PO3)3H}]· 8H2O was synthesized, isolated, and studied (space group P21/c, Z = 4, a = 9.7385(2), b = 10.2542(2), c =21.6517(3) Å, β = 93.7060(10)°). The nitrilotris(methylenephosphonate) ion is monoprotonated at the PO3 group. The nitrogen atom is deprotonated and coordinates the Mo atom; the NTP denticity is 4. Hydroxylamine is ionized according to the acid type and is bidentate. The Mo–NO group is almost linear (176.31(19)° angle; Mo–N, 1.7599(13) Å; ν(N–O), 1756 cm–1), the electron density distribution attests to the formation of an Mo–N π-bond. The Mo coordination polyhedron is a distorted pentagonal bipyramid. Two Na ions are coordinated at the vertices of a distorted octahedron and the third one forms a distorted tetrahedral geometry. (CIF file CCDC no. 1543700.)

Aquanitrilotris(methylenephosphonato)dirubidium [Rb2(H2O){μ12-NH(CH2PO3H)3}]: Synthesis and structure

Aquanitrilotris(methylenephosphonato)dirubidium is a 3D coordination polymer with a layer structure. Space group

Aqua{pentahydrogennitrilotris(methylenephosphonato)}lithium hydrate [Li(H2O){N(CH2PO3)3H5}] • H2O: Synthesis and structure

P\bar 1

Dihydronitrilotris(methylenephosphonato)dimercury(II)mercury(I) [(Hg 2 I )Hg II N(CH 2 PO 3 ) 3 H 2 ]: Synthesis and Structure

P1¯, Z = 2; a = 8.0380(3) Å, b = 9.0522(4) Å, and c = 10.7837(4) Å; α = 113.252(4)°, β = 105.391(3)°, and γ = 96.182(3)°. Rb atoms populate two symmetrically inequivalent positions with c.n. = 8 and 10; significant difference in O–Rb–O angles in the coordination polyhedra is indicative of the ionic type of Rb–O bonds. In the crystal packing, molecules are connected by not only coordination bonds but hydrogen bonds as well.

Bis(nitrilo)tris(methylenephosphonato)dodecaaquatrihydrohexasodium Europium(III) [EuNa6H3(H2O)12{N(CH2PO3)3}2]: Synthesis and Structure

Abstract3D coordination polymers cesium nitrilotris(methylenephosphonate) and dicesium nitrilotris( methylenephosphonate) are synthesized and their crystal structure is determined. In the crystal of [Cs-μ6-NH(CH2PO3)3H4] (space group P, Z = 2), cesium atoms occupy two crystallographically inequivalent positions with c.n. = 10 and c.n. = 14. The phosphonate ligand plays the bridging function; its denticity is nine. The crystal packing consists of alternating layers of Cs atoms in different environments with layers of ligand molecules between them. A ligand is bound to three Cs atoms of one layer and three Cs atoms of another layer. In the crystal of [Cs2-μ10-NH(CH2PO3H)3] · H2O (space group P, Z = 2), the complex has a dimeric structure: the bridging phosphonate ligand coordinates Cs to form a three-dimensional Cs4О6 cluster. The denticity of the ligand is equal to nine; the coordination numbers of cesium atoms are seven and nine. Two-dimensional corrugated layers of Cs4О6 clusters lie in the (002) plane, and layers of ligand molecules are located between them. Each ligand molecule coordinates eight Cs atoms of one layer and two Cs atoms of the neighboring layer.