M. D. Surazhskaya

Synthesis and crystal structure of phosphate Ba1.5Fe2(PO4)3

Double phosphate Ba1.5Fe2(PO4)3 was synthesized and structurally studied. Single crystals were synthesized by the fusion method. Cubic crystals, Z = 4, space group P213, a = 9.866(1) Å. This structure is built of polyhedrons of four types: PO4 tetrahedrons, two virtually regular FeO6 octahedrons, BaO12 twelve-vertex polyhedrons, and BaO9 nine-vertex polyhedrons. These polyhedrons share common oxygen vertices to form three-dimensional [Fe2(PO4)3]3∞ framework containing barium atoms in cavities.

Molybdenum(VI) complexes with N-substituted hydroxylamines

New molybdenum(VI) complexes with N-monoalkylsubstituted hydroxylamines have been synthesized and studied. The structure of [MoO2(C2H5NHO)2] and [MoO2(i-C3H7NHO)2], whose distinguishing feature is the bidentate chelate coordination of the ligand to molybdenum with the formation of the three-membered NMoO chelate ring, has been determined by X-ray diffraction.

Reaction between uranyl dihydroxylaminate and benzaldehyde

Reactions of coordinated ligands in uranyl hydroxylaminate complexes with benzaldehyde were studied. Methods of the synthesis of uranyl complexes containing E and Z isomers of benzaldehydoxime were developed. The structures of [UO2((E)-C7H6NO)2{(CH3)2SO}2] and [UO2((Z)-C7H6NO)2{(CH3)2SO}2] were determined by X-ray diffraction.

Bis(Thiosemicarbazide)Copper(II) 1,5-Naphthalenedisulfonate Complex [Cu(Тsc)2](1,5-Nds): Synthesis and Crystal and Molecular Structures

The synthesis, analysis, and IR spectroscopic, thermogravimetric, and X-ray diffraction study of [Cu(Тsc)2](Nds) (I), where Тsc is thiosemicarbazide NH2NHС(=S)NH2, and 1,5-Nds2– is the doubly deprotonated 1,5-naphthalenedisulfoacid anion C10H6(SO3)22–, have been performed. Crystal structure units in complex I are [Cu(Тsc)2]2+ centrosymmetric complex cations and (Nds)2– anions (including those in inversion centers). The copper atom is coordinated to the vertices of a square via the two sulfur and two nitrogen atoms of the two bidentate-chelate (S,N) ligands Тsc. Crystal structure units in complex I are linked together by a branched network of weak nonlinear N–Н···О hydrogen bonds with participation of donors (all the five independent hydrogen atoms of the two NH2 groups and NH group of the [Cu(Tsc)]2+ complex cation) and acceptors (all the three independent oxygen atoms of the sulfato group of the 1,5-Nds2– anion).

Nickel(II) tetraaqua bis(benzoate) tris(phenylacethydrazide) complex [Ni(HL1)3](L2)2 · 4H2O: Synthesis and crystal and molecular structure

The synthesis, IR and Raman spectroscopic study, and X-ray diffraction analysis of [Ni(HL1)3](L2)2 · 4H2O (I), where HL1 is phenylacetic acid hydrazide and L2 is the benzoate monoanion, have been performed. The structural units of a crystal of complex I are complex [Ni(HL1)3]2+ cations, (L2)– anions, and crystallization water molecules. The nickel atom is coordinated to the three oxygen atoms at octahedron apices and the three nitrogen atoms of three bidentate chelate (О, N) ligands HL1 in cis,trans-meredianal (fac) conformation. The structural units of a crystal of complex I are bonded by a branched network of О–Н···О and N–H···O hydrogen bonds.

Complex [MoO 2 (L)(CH 3 OH)] (L 2- = 3-methoxysalicylidenemonoethanolimine anion): Synthesis, crystal and molecular structures

The complex [MoO2(L)(CH3OH)] (where L2- is 3-methoxysalicylidenemonoethanolimine anion) has been prepared and structurally characterized by X-ray diffraction. The molybdenum atom has an octahedral coordination to two ligands in cis-positions to each other, two oxygen atoms, the nitrogen atom of the tridentate bis(chelate) L2- ligand, and also the oxygen atom of methanol. Strong O-H⋯O hydrogen bonds (O⋯O, 2.598 Å) link pairs of molecules into centrosymmetric pseudo-dimers.

Crystal and molecular structure of diaquadinitratouranyl dihydrate [UO2(NO3)2(H2O)2] · 2H2O

Single crystals of previously unknown diaquadinitratouranyl dihydrate [UO2(NO3)2(H2O)2] · 2H2O (I) were obtained by evaporation of aqueous solution of [UO2(NO3)2(H2O)2] · 4H2O containing nitric acid in air at ambient temperature. The structure of the complex was studied by X-ray diffraction analysis. Crystals are monoclinic, a = 7.6820(15) Å, b = 9.887(2) Å, c = 7.1990(14) Å, β = 105.08(3)°, space group P21/c, Z = 2, V = 527.95(18) Å3. Structural units of crystal are neutral centrosymmetrical molecular complexes [UO2(NO3)2(H2O)2] and crystal water molecules united by a hydrogen bond system. Certain structural and spectral characteristics of new complex I and known diaquadinitratouranyl complexes were compared.

Synthesis and crystal and molecular structure of the [MoO2(L)(H2O)] · H2O complex (L 2− is the anion of 2-[N-(hydroxynaphtylidene)amino]propan-1,2,3-triol)

A new compound of dioxomolybdenum(VI)—[MoO2(L)(H2O)] · H2O, where L2− = 2-[N-(hydroxynaphtylidene)amino]propan-1,2,3-triol)—is synthesized. Its structure is determined by X-ray diffraction. The Mo atom has an octahedral coordination formed by two oxo ligands located cis with respect to one another, two O atoms and the N atom of the tridentate bis(chelate) L2− ligand, and the O atom of a water molecule. The crystallization water molecule is connected with two complex molecules by O-H…O hydrogen bonds.

The Insertion of Carbon Dioxide in Combination with RNCS (R Is Et, Ph) or N,N′-Dihexylcarbodiimide into the Re–O(R) Bonds

The heteromolecular insertion of carbon dioxide in combination with heterocumulenes, iso(thio)cyanates or N,N′-dicyclohexylcarbodiimide, into rhenium–alkoxy group bond was accomplished for the first time in relation to reactivity of rhenium oxoalkoxides. The ease of combined insertion of iso(thio)cyanate and carbon dioxide into Re–O(Me) bond is determined by the nature of the heterocumulene organic group. Indeed, if ethyl iso(thio)cyanate is used in the reaction, the insertion is reversible, whereas the reaction with PhNCS (unlike PhNCO) together with carbon dioxide leads to complete insertion into two Re–O(R) bonds to give the insertion product (OMe)10O6Re4[OC(O){N(Ph)C(S)}2-OMe]2. In similar reactions carried out with N,N′-dicyclohexylcarbodiimide, a dependence of the number of bonds participating in the inner-sphere condensation of the inserted moieties on the duration of the experiment was found for the first time. An increase in the time of synthesis from 3 to 5 h results in insertion involving six rather than three bonds, the heteromolecular insertion products being (OMe),O6Re4{OC(O)[(Hex)N=C=N(Hex)]2}3 and (OMe)6O6Re4{OC(O)[(Hex)N=C=N(Hex)]2}6, respectively.

Crystal Structure of (H3O)2[(UO2)2(SO4)3(H2O)] · 6.86H2O, a New Hydroxonium Diuranyltrisulfate Aqua Complex

Single crystals of earlier unknown hydroxonium monoaquatrisulfatodiuranylate 6.86-hydrate (H3O)2[(UO2)2(SO4)3(H2O)] · 6.86H2O (I) have been synthesized via the evaporation of an aqueous [UO2(NO3)2(H2O)2] · nH2O (n = 2, 4) solution containing sulfuric and nitric acids in air at room temperature. The structure of complex I has been studied by X-ray diffraction. Crystals are monoclinic, а = 15.0903(12) Å, b = 9.9191(8) Å, c = 15.6099(13) Å, β = 112.560(1)°, space group P21/n, Z = 4, V = 2157.7(3) Å3. The complex is formed due to electrostatic attraction forces between counterions and stabilized by hydrogen bonds. Its main structural element is the [(UO2)2(SO4)3H2O] n2- framework. The structure contains two types of uranium atoms surrounded by oxygen atoms according to a pentagonal bipyramid motif. The coordination polyhedra of all the three crystallographically different S atoms are SO42- tetrahedra. The U(1) atom in the equatorial bipyramid plane is monodentately bonded to the oxygen atoms of five SO42- tetrahedra, while the U(2) atom is monodentately coordinated to four sulfate groups and one water molecule.