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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) A, b = 9.9191(8) A, c = 15.6099(13) A, β = 112.560(1)°, space group P21/n, Z = 4, V = 2157.7(3) A3. 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] n 2- 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 SO 4 2- tetrahedra. The U(1) atom in the equatorial bipyramid plane is monodentately bonded to the oxygen atoms of five SO 4 2- tetrahedra, while the U(2) atom is monodentately coordinated to four sulfate groups and one water molecule.

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.

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) 2 2– , 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).

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.

New complexes of uranyl with diethylglyoxime have been synthesized and studied. A feature of these complexes is the tetradentate bridging coordination of the ligand in both cis- and trans-conformations. The structure of organic ligand C6H12N2O2 and binuclear complex (CN3H6)4[(UO2)2(C6H10N2O2)(CO3)(C2O4)2] ∙ H2O have been determined by X-ray diffraction.

Single crystals of diaquadinitratouranyl tetrahydrate [UO2(NO3)2(H2O)2] • 4H2O (I) have been synthesized by evaporating an aqueous [UO2(NO3)2(H2O)2] • 2H2O solution containing nitric acid under air at room temperature. An experimental X-ray diffraction intensity set has been obtained from a single crystal of I. Crystals are ortorhombic, a = 13.113(2) A, b = 7.9847(12) A, c = 11.3323(17) A, space group Cmc21, Z = 4, V = 1186.5(3) A3. The structural units of a crystal of complex I are neutral molecular complexes [UO2(NO3)2(H2O)2] and crystal water molecules linked by a network of hydrogen bonds. The uranium atom is in a hexagonal bipyramidal surrounding. Axial positions are occupied by uranyl oxygen atoms, and two nonequivalent bidentate cyclic nitrato groups and two equivalent water molecules are coordinated in the equatorial plane in trans-positions to each other. Coordinated and outer-sphere water molecules in the molecular structure of complex I are linked by hydrogen bonds as O-H(H2Ocoord)⋯O(H2Oout). Outer-sphere water molecules are linked to each other and the terminal oxygen atoms of nitrato groups by hydrogen bonds as O-H(H2Oout)⋯O(H2Oout) and O-H(H2Oout)⋯O(ONO2-). Hydrogen bonds of the first type are stronger than those of the second and third types.

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) A, b = 9.887(2) A, c = 7.1990(14) A, β = 105.08(3)°, space group P21/c, Z = 2, V = 527.95(18) A3. 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.

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.

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 A) link pairs of molecules into centrosymmetric pseudo-dimers.

A new compound of dioxomolybdenum(VI)—[MoO2(L)(H2O)] · H2O, where L 2− = 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) L 2− 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.

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.

We demonstrate that the previously synthesized product of ethyl isothiocyanate insertion into tungsten hexachloride, WCl5{N(Et)C(S)N(Et)C(S)Cl}, whose partial hydrolysis yields {N(Et)C(S)-S-S-C=NH(Et)}[WOCl5] (I), can be used as a source of biologically active heterocyclic compounds. 1H and 13C NMR and gas chromatography-mass spectrometry data show that reaction of I with a saturated aqueous Na2CO3 solution yields a number of thiazolidine heterocycles, mostly 4-ethyl-5-ethylimino-[1,2,4]-dithiazolidin-3-trithione. The thermal Dimroth rearrangement leads to the formation of 2,4-diethyl-[1,2,4]-dithiazolidin-3,5-dithione and the products of partial hydrolysis of both heterocycles: 4-ethyl-5-ethylimino-[1,2,4]-dithiazolidin-3-on and 2,4-diethyl-3-thioxo-[1,2,4]-dithiazolidin-5-on.

Ten new dioxomolybdenum(VI) compounds with o-oxyazomethines, derivatives of substituted salicylaldehydes (I–X) and tris(hydroxymethyl)aminomethane, are synthesized. The structures of two of them, [MoO2(L)] · CH3OH; L = Z-substituted salicylalimines, Z = 3-NO2 (IV) and 3-OCH3 (V), are determined by X-ray diffraction analysis. Compounds IV and V have similar structures and geometric parameters. The Mo atoms are coordinated through the octahedral mode by two oxo ligands in the cis positions to each other, two O atoms, one N atom of the tridentate bis(chelating) ligand L, and the O atom of the MeOH molecule.

The reaction of diaquadinitratouranyl with ammonium nitrate in ethanol gave the single crystals of ((NH4)2[}UO2(NO3)2}2(μ4-C2O4)] · 2H2O (I).The structure of the complex was studied by X-ray diffraction. The crystals are monoclinic, a = 8.6497(10) A, b = 11.7001(10) A, c = 20.2135(10) A, β = 93.924(10)°, space group P21/c, Z = 4, V = 2040.9(3) A3. The structural units of the crystal are island binuclear groups [{UO2(NO3)2}2(μ4-C2O4)]2−, ammonium cations, and crystal water molecules. The structure has a complex three-dimensional packing provided by electrostatic attraction forces of the counterions and the hydrogen bond system involving water molecules, oxalate, nitrate, and uranyl ions. The IR spectra of I confirm the X-ray diffraction data.

A reaction of uranyl dioxalate complexes with methyl derivatives of alicyclic α-dioximes, 3-methyl-1,2-cyclohexanedione dioxime and 3-methyl-1,2-cyclopentanedione dioxime, was studied. The structure of (CN3H6)4[(UO2)2(C6H8N2O2)(CO3)(C2O4)2] · (C6H10N2O2) · 2H2O and NH4(CN3H6)3[(UO2)2(C7H10N2O2)(CO3)(C2O4)2] · 2H2O based on binuclear complex anions with carbonate-dioximate fragment was studied by X-ray diffraction.

Single crystals of diammonium tetranitratouranylate (NH4)2[UO2(NO3)4] (I) and a new diammonium tetranitratouranylate complex with 18-crown-6 [(NH4)(18C6)]2[UO2(NO3)4] (II) have been synthesized by the reaction of diaquadinitratouranyl tetrahydrate with ammonium nitrate in a nitric acid solution and the reaction of the same reagents with 18C6 in an ethanol solution, respectively. The X-ray diffraction analysis of compounds I and II has been performed. Crystals of compounds I and II are monoclinic, Z = 2, space group P21/n, a = 6.4075(5) A, b = 7.7851(7) A, c = 12.4461(12) A, β = 101.239(1)°, V = 608. 94(9) A3 for compound I and a = 10.542(9) A, b = 8.590(8) A, c = 22.5019(19) A, β = 101.632(1)°, V = 2058.3(3) A3 for compound II. The [UO2(NO3)4]2− complex anion in compounds I and II contains two monodentate and two bidentate cyclic nitrato groups, and the coordination number of uranyl is 6. The 18C6 molecule in the structure of compound II has the classic crown conformation and combined with the ammonium ion by three hydrogen bonds. Compounds I and II formed by electrostatic attraction forces between counterions are stabilized by (NH 4 + )NH...O(NO 3 − ) interionic hydrogen bonds.

Ammonium trinitratouranylate NH4[UO2(NO3)3] (I) single crystals have been synthesized by the reaction of aqueous solutions of diaquadinitratouranyl tetrahydrate and ammonium nitrate in the presence of nitric acid. The structure of the complex has been studied by X-ray diffraction analysis: space group \(R\bar 3c\), a = 9.361(2), c = 18.883(4) A; V = 1433.0(5) A3, and Z = 6. The structural units of the NH4[UO2(NO3)3] crystal—NH4+ cations and [UO2(NO3)3]− complex anions with three bidentate cyclic nitrato groups—are on crystallographic axes \(\bar 3\). A complex three-dimensional packing arranged by the electrostatic attraction forces between counterions and the N-H...O hydrogen bonds between ammonium cations and trinitratouranylate anions is realized in the structure. X-ray diffraction analysis results are confirmed by IR spectra of NH4[UO2(NO3)3].

The reactions of coordinated ligands in uranyl complexes were studied for the first time. The reaction of uranyl hydroxylaminate complexes with aldehyde and ketones of different structure was shown to result in the formation of corresponding oxime complexes.

The compound Cs3ZnBr5 was synthesized from cesium and zinc bromides. The single crystals were grown by the Bridgman method. The structure of Cs3ZnBr5 was studied. The compound crystallizes in the tetragonal system with the unit cell parameters: a = b = 9.633(2) A, c = 15.141(5) A, V = 1404.8(6) A3, Z = 4, space group I4/mcm; ρcalcd = 4.083 g/cm3, ρexp = 4.074 ± 0.001 g/cm3. The compound Cs3ZnBr5 is not hygroscopic and congruently melts at 530°C; it is transparent at 2.5 to 25 μm. The refractive indices are N p = 1.682, N g = 1.686. The microhardness is 560 MPa.

Uranyl complexes with ethylmethylglyoxime were studied. The structure of (CN3H6)4[(UO2)2(CO3)(C2O4)2(C5H8N2O2)] · 1.5H2O was determined by X-ray crystallography. The structure of the complex is binuclear with a double carbonate dioximate bridging fragment.

Comparing the geometry of [UO2(NO3)2(H2O)2] · 2H2O · 18C6 (18C6 = C12H24O6) and IR spectroscopic data, we propose correlations between the conformation of an ethylene oxide unit of 18-crown-6 and the conformation-sensitive frequency in the IR spectrum. Spectral conformational analysis verifies the composition of the 18-crown-6 conformer in the [UO2(NO3)2(H2O)2] · 18C6 complex whose structure is known. The distribution character of hydrogen bonds that retain crown ether molecules in aquanitratouranyl complexes is shown to influence the conformational uniformity of ethylene oxide units of the macrocycle.

The cation influence on substitution reactions in aqua dioxalate uranyl complexes with the participation of a fluoride ion as an attacking ligand and two-charge cations of ethylene diammonium and propylene diammonium was considered. The structure of (C2H10N2)3[UO2(C2O4)2F]2 · 6H2O and (C3H12N2)[UO2(C2O4)2(H2O)] complexes was determined by X-ray crystallography.

Uranylaqua complexes with N-methyl-, N-ethyl-, N-isopropyl-, and N,N-dimethylhydroxylamines were studied. The structure of [UO2{(CH3)2NO}2(H2O)2] was determined by X-ray crystallography. The N, N -dimethylhydroxylaminate ion is coordinated to uranyl through the nitrogen and oxygen atoms with the formation of a three-membered chelate ring.

Unusual coordination modes of 1,2-cyclohexane dionedioxime in uranyl complexes, i.e., tridentate chelating/bridging and (E, Z)-pentadentate chelating/bridging ones, were established by X-ray crystallography of single crystals of (CN3H6)3[(UO2)2(C6H9N2O2)(C6H8N2O2)(C2O4)2] · 2H2O and [(UO2)2(C6H8N2O2)2(H2O)3] · 2H2O. The conditions of the emergence of such coordination modes were determined. The possibility of (E/Z) izomerization of α-dioximes in reactions of uranyl complexes.

The interaction of uranyl compounds with different α-dioximes has been studied. Uranyl complexes with glyoxime, methylglyoxime, dimethylglyoxime, and 1,2-cyclohexanedionedioxime have been synthesized. The X-ray diffraction study of single crystals of [UO2(C3H5N2O2)2{(NH2)2CO}2], [UO2(C6H9N2O2)2(H2O)2] · H2O, [UO2(C6H9N2O2)2(H2O)2] · 6H2O, and [UO2(C6H9N2O2)2(H2O)2]2(CH3CONH2)2 · 6H2O showed a bidentate cyclic coordination of α-dioximes to the central atom through only one oxime group

The complexes [UO2(C6H4NO2)2(C6H5NO2) (I) and [UO2SO4(C6H5NO2)(H2O)] · H2O (II) were synthesized and studied by X-ray diffraction analysis. Crystals I are monoclinic: a = 7.0081(3), b = 14.9624(7), c = 9.1837(5) A, β = 96.594(2)°, Z = 2, space group P21/m. Crystals II are triclinic: a = 6.8097(6), b = 9.3837(8), c = 10.4556(10) A, α = 85.279(3), β = 75.434(3), γ = 69.180(3)°, Z = 2, space group $$P\bar 1$$ . The main structural unit of crystal I is a mononuclear fragment, which belongs to the crystal chemical group AB 2 01 M1 (A = UO 2 2+ , B01 are ions of pyridine-2-carboxylic (picolinic) acid, M1 are molecules of picolinic acid) of the uranyl complexes. The main structural unit of crystal II is a chain, which belongs to the crystal chemical group AT3M 2 1 (where T3-SO 4 2− , M1 are water and picolinic acid molecules) of the uranyl complexes. Picolinic acid in complexes I, II was found to have a zwitterion structure.

Rubidium hexanitratothorate was synthesized, and its crystal structure was determined by X-ray diffraction analysis: space group P21/n; a = 8.347(1) A, b = 6.890(1) A, c = 13.069(1) A, β = 91.88(1)°, Z = 2; 1812 independent reflections, R = 0.0165.

The crystal structure of a new bismuth aluminoborate Bi0.96Al2.37(B4O10)O is studied by single-crystal X-ray diffraction. The Bi0.96Al2.37(B4O10)O single crystals are hexagonal (space group $$P\bar 6$$ 2m). The unit cell parameters are as follows: a = b = 4.587(4) A, c = 2.253(9) A, α = β = 90°, γ = 120°, V = 168.60 A3, Z = 1.

The interaction of uranyl compounds with acetophenone oxime has been studied. Mixed-ligand uranyl acetophenone oximates have been synthesized. X-ray crystallography shows that, in single crystals of [UO2(C8H8NO)2{(CH3)2SO}2] and [UO2(C8H8NO)(NO3){(CH3)2SO}2], acetophenone oxime is coordinated to uranyl as a bidentate chelating ligand.

An energy analysis of small-angle neutron scattering in Fe x Ni1−x (x = 0.50, 0.57, 0.65 at %) alloys is performed at various temperatures and wavevectors. Low-energy long-wavelength magnetic excitations other than spin waves of the Holstein-Primakoff type are detected. These data and the data obtained earlier for the Fe0.65Ni0.35 alloy indicate that the density of states of the low-energy long-wavelength magnetic excitations correlates with the inhomogeneity of the magnetic structure of the alloys, which is caused by the iron concentration and a competing exchange interaction (J NiNi > 0, J FeNi > 0, J FeFe < 0).

The single crystals of K3[UO2(C2O4)2(NCS)] · 3H2O were studied by X-ray diffraction. The compound crystallizes in the monoclinic system, space group P21/n, Z = 4, a = 10.673 A, b = 12.041 A, c = 13.856 A, β = 110.18°, R = 0.0290. The basic structural units of the crystals of I are the island complex groups [UO2(C2O4)2NCS]3− corresponding to the crystal-chemical group AB01 2M1 (A = UO 2 2+ , B01 = C2O 4 2− , M1 = NCS−) of uranyl complexes and connected into a three-dimensional framework through electrostatic interactions and through hydrogen bonds involving potassium ions and water molecules.

A procedure for the synthesis of uranyltricarbonatetetrarubidium Rb4UO2(CO3)3 was developed. Its crystal structure was determined by X-ray diffraction analysis: space group C2/c; a=10.778(5) A, b=9.381(2) A, c=12.509(3) A. β=94.42(3)°, Z=4; 1178 independent reflections, R=0.0662.

The temperature dependences of the intensity of elastic diffuse neutron scattering from γ-FexNi100−x (x=57 and 68 at. %) alloy single crystals near basic reciprocal-lattice sites in the (110) plane are measured using a triaxial neutron spectrometer. New effects of instability of the γ-phase lattice with respect to long-wavelength (transverse and longitudinal) static atomic displacements have been detected. The displacements are found to depend on the iron concentration in the alloys and on temperature. The relations of these structural distortions to premartensitic phenomena and the invar effect in γ-FeNi alloys are discussed

A theoretical analysis of small-angle neutron scattering is performed for the Fe65Ni35 alloy at a temperature T=0.9TC=450 K. The results obtained indicate the existence of long-wavelength magnetic excitations that do not correspond to spin waves of the Holstein-Primakoff type. The possible nature of these excitations is discussed.

The crystal structures of complex antimony(III) fluorides RbSbF4 (I) and (C2N4H5)SbF4 (II) were determined. The crystals of I and II are monoclinic; for I: a = 4.628(1) A, b = 6.167(1) A, c = 7.922(1) A, β = 100.582(3)°, V = 222.24(7) A3, Z = 2, ρ(calcd.) = 4.23 g/cm3, ρ(exp.) = 4.25 g/cm3, F(000) = 248, space group P21/m, R = 0.0395; for II: a = 4.678(1) A, b = 7.339(4) A, c = 10.185(1) A, β = 90.88(2)°, V = 349.6(2) A3, Z = 2, ρ(calcd.) = 2.69 g/cm3, ρ(exp.) = 2.70 g/cm3, F(000) = 264, space group P21. The structure of I is formed by Rb+ cations and [SbF4]n−n anionic chains composed of SbF5E octahedra with two bridging fluorine atoms. The structure of IIis formed by (C2N4H5)+ cations and isolated [SbF4]− anions in which the antimony polyhedra are SbF4E trigonal bipyramids. The relationship between the crystal structures and electrophysical and biological properties of single-charged cation tetrafluoroantimonates(III) was studied.

The (C10H10N2)0.5[SnF(SO4)] compound was synthesized via reaction of SnF2 with 4,4"-bipyridine (C10H8N2) in a diluted sulfuric acid solution (pH 3) and its X-ray diffraction analysis was carried out. The Sn2+ atoms coordinate one fluorine atom (Sn–F 2.062(2) A) and two oxygen atoms of two sulfate groups (Sn–O 2.149(2) and 2.313(3) A) thus forming the coordination polyhedron as a trigonal bipyramid with a stereochemically active unshared electron pair in its vertex. The sulfate groups act as bidentate bridges and join the neighboring Sn2+ complexes into infinite chains of [SnF(SO4)] n– n anions combined in pairs through the Sn–F contacts (2.450(2) A) to form ribbons whose voids contain two-charge 4,4"-bipyridinium cations.

The reaction of tungsten hexachloride with excess ethyl isocyanate in dichloroethane leads to the insertion of three ligand molecules at one of the tungsten–chlorine bonds. The data of elemental analysis and IR spectroscopy confirm that the thermolysis of the reaction mixture affords the WCl4(L3Cl) complex (I), where L = –N(Et)C(O)–. The structure of the chain of inserted molecules in I is established on the basis of IR and NMR data, and the results of X-ray diffraction analysis of crystals of an organic product (II) of the hydrolysis of I. According to the latter, compound (II) is a derivative of s-triazine—1,3,5-triethyl-1,3,5-triazine-2,4,6-(1H,3H,5H)-trione.

Antimony(III) fluoride complexes with compositions (NH4)3Sb4F15(I) and Cs3Sb4F15(II) are structurally characterized. Crystals Iare triclinic: a= 8.317(3) A, b= 10.419(6) A, c= 10.826(3) A, α = 63.71(4)°, β = 73.24(3)°, γ = 77.42(5)°, Z= 2, ρcalcd= 3.42 g/cm3, ρexp= 3.45 g/cm3, space group P\(\overline {\text{1}} \), R= 0.051; crystals IIare monoclinic: a= 8.079(2) A, b= 29.116(8) A, c= 8.162(2) A, β = 117.08(2)°, Z= 4, ρcalcd= 4.549 g/cm3, ρexp= 4.50 g/cm3, space group P21/c, R= 0.036. Structure Iis composed of SbF4E and SbF5E polyhedra combined into tetranuclear chains; crystals IIconsist of SbF4E polyhedra, two of which form a dimer Sb2F7E2, while the other two are isolated (E is the antimony lone electron pair).

The features of the environment of actinide atoms (Pa, Pu, Am, Cm, Bk, Cf) in the crystal structure of their oxygen-containing compounds were analyzed in terms of Voronoi-Dirichlet (VD) polyhedra. The volume of the VD polyhedra of actinide atoms surrounded by the oxygen atoms is determined by their valence state and is practically independent of their coordination number. In going to higher oxidation states, the volume of the VD polyhedra of actinide atoms regularly decreases.

The NH4[SnF2(NCS)] compound was obtained and its structure was determined. The tin atom is surrounded by two fluorine atoms (Sn–F 2.060 A) and one nitrogen atom of the NCS group (Sn–N 2.351 A). The coordination polyhedron of tin(II) is a distorted trigonal pyramid with a stereochemically active lone electron pair at the vertex.

The crystal structure of a novel antimony(III) fluoride complex, ammonium undecafluorotriantimonate(III) (NH4)2Sb3F11, was determined. The crystals are triclinic: a = 7.780(2) A, b = 8.370(2) A, c = 10.620(1) A, α = 71.06(1)°, β = 89.03(1)°, γ = 63.58(1)°, V = 579.1(2) A3, Z = 2, ρ(calcd) = 3.500 g/cm3, ρ(exp) = 3.51 g/cm3, F(000) = 548.0, space group P\(\overline 1\). The structure consists of anionic [Sb3F11]2– chains and ammonium cations combined into a framework by the N–H···F hydrogen bonds.

The crystal structure of thallium fluoroantimonate(III) complex TlSb4F13 (I), which is isostructural to KSb4F13 (II), is determined. Crystals I are tetragonal: a = 9.634(2) A, c = 6.590(2) A, V = 611.7(2) A3, Z = 2, ρ(calcd) = 5.094 g/cm3, F(000) = 804.0, space group I4¯. The structure consists of tetrameric [Sb4F13]– anions formed by SbF3 groups connected by the fluoride ion and the Тl+ cations.