(NH4)(CN3H6)2[UO2(C2O4)2(NCS)] · 2H2O: Synthesis and crystal structure

A single-crystal X-ray diffraction study (NH₄)(CN₃H₆)₂[(UO₂(C₂O₄)₂(NCS)] · 2H₂O (I) was carried out. The crystals are orthorhombic, space group P2₁2₁2₁, Z = 4, with the unit cell parameters a = 6.668(2) Å, b = 13.463(4) Å, c = 23.086(6) Å. The main structural units of the crystals of I are insular complex anions [(UO₂)(C₂O₄)₂(NCS)]^3?. They belong to the crystal-chemical group AB ₂ ⁰¹ M¹ (A = UO ₂ ²⁺ ) of uranyl complexes and are linked into a three-dimensional framework through electrostatic interactions and hydrogen bonds with the participation of ammonium and guanidinium cations and crystal water molecules.     

Synthesis and crystal structure of Ba2[(UO2)(C2O4)2(NCS)]NCS·7H2O

Single crystals of Ba₂[(UO₂)(C₂O₄)₂(NCS)]NCS · 7H₂O were prepared and studied by X-ray diffraction. The crystals are monoclinic, space group P2₁/c, Z = 4, a = 13.508(5) Å, b = 12.268(4) Å, c = 14.965(5) Å, β = 115.38(1)°, V = 2240.6(13) ų. The main structural units in the crystal are the island complex species [(UO₂)(C₂O₄)₂(NCS)]^3? corresponding to the crystal chemical group AB ₂ ⁰¹ M¹ (A = UO ₂ ²⁺ , B⁰¹ = C₂O ₄ ^2? , M¹ = NCS^?) of uranyl complexes, which are united into a three-dimensional framework through electrostatic interactions and through hydrogen bonds involving oxalate and isocyanate ions and water molecules.     

Synthesis and crystal structure of [UO2CrO4(C5NH5COO)] · 0.25H2O

[UO₂CrO₄(C₅NH₅COO)] · 0.25H₂O crystals have been synthesized and studied by X-ray diffraction and IR spectroscopy. The compound crystallizes in monoclinic system with the unit cell parameters a = 7.2362(3) ?, b = 13.8847(6) ?, c = 10.7204(5) ?, ?? = 90.037(2)°, space group P2₁/n, Z = 4, R = 0.0236. The structure consists of [UO₂CrO₄(C₅NH₅COO)] chains, which run in the direction [100] and correspond to the AT³B⁰¹ crystallochemical formula, where A = UO ₂ ²⁺ , T³ = CrO ₄ ^2? , and B⁰¹ is nicotinic acid molecules in the form of zwitter ions. The results of analyzing nonbonded interactions in the crystal structure by the method of molecular Voronoi-Dirichlet polyhedra (MMVDP) are presented.     

Synthesis and crystal structure of Cs2[(UO2)2(C2O4)3] and Cs2[UO2(C3H2O4)2] · H2O

Cs₂[(UO₂)₂(C₂O₄)₃] (I) and Cs₂[UO₂(C₃H₂O₄)₂] · H₂O (II) have been synthesized and studied by X-ray diffraction. The crystals of complexes I and II are monoclinic: a = 8.1453(2) Å, b = 8.9831(2) Å, c = 11.3897(4) Å, β = 104.0950(10)°, V = 808.29(4) ų, space group P2₁/n, Z = 2, and R ₁ = 0.0255 for I and a = 9.6998(2) Å, b = 17.8686(3) Å, c = 8.2074(2) Å, β = 97.5780(10)°, V = 1410.10(5) ų, space group P2₁/c, Z = 4, and R ₁ = 0.0287 for II. The uranium-containing structural units of complexes I and II are [(UO₂)₂(C₂O₄)₃]^2? chains and [UO₂(C₃H₂O₄)₂] ₂ ^4? dimers, which belong to the AK _0.5 ⁰² T¹¹ and AT¹¹B⁰¹ crystallochemical groups (A = UO ₂ ²⁺ , K⁰² and T¹¹ = C₂O ₄ ^2? , T¹¹ and B⁰¹ = C₃H₂O ₄ ^2? ) of uranyl complexes.     

Synthesis and structure of [UO2(SeO4)(C2H4N4)2] · 0.5H2O

The single-crystal X-ray diffraction analysis of [UO₂(SeO₄)(C₂H₄N₄)₂] · 0.5H₂O (I) is performed. The crystals are monoclinic: space group C2/c, Z = 8, a = 19.035(2), b = 7.1326(8), c = 21.477(2) Å, β = 109.683(4)°. The main structural units of the crystal are chains of [UO₂(SeO₄)(C₂H₄N₄)₂]. Compound I belongs to the crystal-chemical group AT³M ₂ ¹ (A = UO ₂ ²⁺ , T³ = SeO ₄ ^2? , M¹ is a cyanoguanidine molecule) of the uranyl complexes. The chains are united into three-dimensional framework through hydrogen bonds involving the oxygen atoms of the selenate and uranyl groups, the nitrogen atoms of cyanoguanidine, and the hydrogen atoms of the cyanoguanidine or water molecules.     

Synthesis and structure of (NH4)2[(UO2)2(C2O4)(CH3COO)4] · 2H2O

Single crystals of (NH₄)₂[(UO₂)₂C₂O₄(CH₃COO)₄] · 2H₂O have been synthesized and studied. The compound crystallizes in the orthorhombic system with the unit cell parameters a = 6.9225(14) Å, b = 12.327(3) Å, c = 14.619(3) Å, space group Immm, Z = 2, and V = 1247.6(5) ų. The main structural units of the crystals are the isle binuclear groups [(UO₂)₂C₂O₄(CH₃COO)₄]^2? belonging to the crystal-chemical group A₂K⁰²B ₄ ⁰¹ (A = UO ₂ ²⁺ , K⁰² = C₂O ₄ ^2? , B⁰¹ = CH₃COO^?) of the uranyl complexes. The uranium-containing groups are linked into a three-dimensional framework due to electrostatic interaction with the ammonium cations and through a system of hydrogen bonds involving atoms of the water molecules, oxalate and acetate ions, and ammonium and uranyl cations.     

Rhenium complexes with pyrazoles. Synthesis and crystal structure of trans-[Re(O)(OMe)L4]Br2·L·4H2O (L is 3,5-dimethylpyrazole)

The first mononuclear Re^V complex with four pyrazole ligands, viz., [Re(O)(OMe)L₄]Br₂ (L is 3,5-dimethylpyrazole), and its molecular adduct with L, viz., [Re(O)(OMe)L₄]Br₂·L·4H₂O, were synthesized. The complex is resistant to hydrolysis in a neutral aqueous solution. The structure of the adduct was established by X-ray diffraction analysis.     

Synthesis and structure of Na[UO2(SeO3)(HSeO3)] · 4H2O

Compound Na[UO₂(SeO₃)(HSeO₃)] · 4H₂O (I) has been synthesized and studied by single-crystal X-ray diffraction. The crystals of I are monoclinic with the unit cell parameters a = 8.8032(5) Å, b = 10.4610(7) Å, c = 13.1312(7) Å, β = 105.054(2)°, space group P2₁/n, Z = 4, V = 1167.76(12) ų, R = 0.0394. The main structural units of crystals I are the [UO₂(SeO₃)(HSeO₃)]^? layers belonging to the AT³B² crystal-chemical group (A = UO ₂ ²⁺ , T³ = SeO ₃ ^2? , B² =HSeO ₃ ^? ) of the uranyl complexes. The sodium ions are linked with oxygen atoms of two uranyl ions of the same layer and with four water molecules. Electroneutral packets that formed are linked into a three-dimensional framework through a system of hydrogen bonds.     

The crystal structure of Fe(SeO2OH)(SeO4)·H2O

Summary The crystal structure of the hydrothermally synthesized compound Fe(SeO₂OH) (SeO₄) · H₂O was determined by single crystal diffraction methods:a=8.355(2) Å,b=8.696(2) Å,c=9.255(2) Å, =93.72(1)°,V=670.95 ų;Z=4, space group P2₁/c,R=0.029,R _w=0.027 for 2430 independent reflections (sin /0.76 Å^–1). Isolated FeO₅(H₂O)-octahedra share five corners with [SeO₂OH] and [SeO₄] groups to form sheets parallel to (100). These sheets are interconnected via hydrogen bonds only.

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Die Kristallstruktur von Fe(SeO₂OH)(SeO₄)·H₂O

Zusammenfassung Die Kristallstruktur der hydrothermal dargestellten Verbindung Fe(SeO₂OH) (SeO₄)·H₂O wurde mittels Einkristallbeugungsmethoden bestimmt:a=8.355(2) Å,b=8.696(2) Å,c=9.255(2) Å, =93.72(1)°,V=670.95 ų;Z=4, Raumgruppe P2₁/c,R=0.029,R _w=0.027 für 2 430 unabhängige Reflexe (sin / 0.76 Å^–1). Isolierte FeO₅(H₂O)-Oktaeder teilen fünf Ecken mit [SeO₂OH]- und [SeO₄]-Gruppen, wobei sie Schichten parallel (100) bilden. Diese Schichten sind nur über Wasserstoffbrücken miteinander verbunden.

     

Synthesis, crystal structure, and IR spectral study of Na[(UO2)(C3H7COO)3] · 0.25H2O and K[(UO2)(C3H7COO)3]

Synthesis, IR spectral study and X-ray diffraction analysis of single crystals of Na[(UO₂)(C₃H₇COO)₃] · 0.25H₂O (I) and K[(UO₂)(C₃H₇COO)₃] (II) were carried out. Compound I is monoclinic, unit cell parameters are: a = 13.5671(15) ?, b = 20.070(2) ?, c = 13.6139(15) ?, ?? = 106.839(2)°, space group P2₁, Z = 8, R = 0.0493. Compound II is orthorhombic, unit cell parameters are: a = 17.1325(9) ?, b = 19.6966(11) ?, c = 21.9686(11) ?, space group P2₁2₁2₁, Z = 16, R = 0.0563. Mononuclear groups [UO₂(C₃H₇COO)₃]^? related to the A ₃ ⁰¹ crystal-chemical group (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₇COO^?) of uranyl complexes are the uranium-containing structural units of crystals I and II. The data of IR spectral study agree well with X-ray diffraction data.     

Synthesis and crystal structure of (H3O)2{(Na2(OH)CB[5])2[HV4O12]}Cl · 14H2O

The compound (H₃O)₂{(Na₂(OH)CB[5])₂[HV₄O₁₂]}Cl · 14H₂O is synthesized by heating (120°C) of a mixture of sodium vanadate, cucurbit[5]uril (CB[5]), rubidium chloride, and water in a sealed ampule. According to the X-ray diffraction data, the binding of the [Na₂(OH)]⁺ binuclear cation with CB[5] occurs due to the bidentate coordination of the oxygen atoms of the portals of cucurbit[5]uril to the sodium atoms. The tetranuclear vanadium complex [HV₄O₁₂]^3? serves as a bridge, joining infinite chains {Na₂(OH)CB[5]} _∞ ⁺ in pairs.     

Synthesis,Structure, and Properties of Cesium Polyuranate [Cs2(H2O)3][(UO2)6O3(OH)8]·2H2O

Russian Journal of General Chemistry - Cesium uranate [Cs2(Н2О)3][(UO2)6O3(OH)8]·2H2O was obtained by reacting hydrated uranium(VI) oxide UO3·2.25H2O with a cesium nitrate...     

Synthesis, crystal structure, and fluorescence properties of a novel coordination polymer [Zn(L)(4,4′-bipyridine)(H2O)] n · (H2O)4

In this work, a novel and rare coordination polymer, [Zn(L)(Bipy)(H₂O)] _n · (H₂O)₄ (H₂L??sphenylpropylmalonate acid, Bipy??4,4??-bipyridine), has been synthesized and characterized by elemental analysis, FT-IR spectroscopy, and solid fluorimetry studies. In the crystal, the Zn²⁺ ion of the complex is hexacoordinated in a slightly distorted octahedral configuration forming the unit structure, 2D structure, and 3D framework. The supramolecular architecture was constructed by a unit of (H₂O)₄ discrete water cluster. Besides, the coordination polymer displays strong emission spectra due to the metal-to-ligand charge-transfer transition, having potential applications as fluorescent materials.     

Crystal structure of Na6[(UO2)3O(OH)3(SeO4)2]2 · 10H2O

The complex Na₆[(UO₂)₃O(OH)₃(SeO₄)₂]₂ · 10H₂O (I) is synthesized and studied by X-ray diffraction. The compound crystallizes in the orthorhombic crystal system with the unit cell parameters: a = 14.2225(7) Å, b = 18.3601(7) Å, c = 16.5406(6) Å, V = 4319.2(3) ų, Z = 4, space group Cmcm, R ₁ = 0.0406. Compound I is found to be a representative of the crystal-chemical group A₃M³M² ₃T³ ₂ (A = UO²⁺ ₂, M³ = O^2?, M² = OH^?, T³ = SeO^2? ₄) of the uranyl complexes; it contains layer uranium-containing groups [(UO₂)₃O(OH)₃(SeO₄)₂]^3?. These layers linked to form a three-dimensional cage through bonds formed by the sodium atoms with the oxygen atoms of the uranyl ions and SeO₄ groups that belong to different layers.     

Synthesis and crystal structure of KBi(C6H4O7) · 3.5H2O

A novel compound, KBi(C₆H₄O₇) · 3.5H₂O (I), has been synthesized in the Bi(NO₃)₂-K₃(HCit) system (HCit^3? is an anion of citric acid C₆H₈O₇) at a component ratio (n) of 8 in a water-glycerol mixture, and its crystal structure has been determined. The crystals are unstable in air. The crystals are triclinic: a = 7.462 Å, b = 10.064 Å, c = 17.582 Å, α = 100.27°, β = 99.31°, γ = 105.48°, V = 1221.2 ų, Z = 2, space group $P\bar 1$ . In the structure of I, asymmetric binuclear fragments [Bi₂(Cit^4?)₂(H₂O)₂]^2? are linked through inversion centers into polymeric chain anions. Ions K⁺ and crystal water molecules are arranged in channels between the chains. The Bi(1)...Bi(2) distances in the binuclear fragment are 4.62 Å, and the Bi(1)...Bi(1) and Bi(2)...Bi(2) distances between bismuth atoms in the chain are 5.83 and 5.95 Å, respectively. The chains are linked through bridging oxygen atoms of the ligands Cit to form layers. In the centrosymmetric four-membered chelate ring Bi₂O₂ formed through Bi-O(Cit) bonds, the distances Bi(1)-Bi(1) are equal to 4.55 Å, and Bi(1)-O are 2.66 and 2.84 Å. The Bi-O bond lengths in I are in the range 2.12–3.16 Å. The Cit ligands act as hexadentate chelating/bridging ligands.     

Synthesis and X-ray diffraction study of cs3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)] and Cs5[UO2(CH3COO)3]3[UO2(NCS)4(H2O)] · 2H2O

Cs₃[UO₂(CH₃COO)₃]₂[UO₂(CH₃COO)(NCS)₂(H₂O)] (I) and Cs₅[UO₂(CH₃COO)₃]₃[UO₂ (NCS)₄(H₂O)] · 2H₂O (II) have been synthesized via the reaction between uranyl acetate and cesium thiocyanate in aqueous solution. According to single-crystal X-ray diffraction data, both compounds crystallize in monoclinic system with the unit cell parameters a = 18.7036(5) Å, b = 16.7787(3) Å, c = 12.9636(3) Å, β = 92.532(1)°, space group C2/c, Z = 4, R = 0.0434 (I); and a = 21.7843(3) Å, b = 24.6436(5) Å, c = 13.1942(2) Å, β = 126.482(1)°, space group Cc, Z = 4, R = 0.0273 (II). Uranium-containing structural units of compound (I) are mononuclear [UO₂(CH₃COO)₃]^? and [UO₂(CH₃COO)(NCS)₂(H₂O)]^? moieties, which correspond to the AB ₃ ⁰¹ and AB⁰¹M ₃ ¹ crystallochemical groups (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?, M¹ = NCS^? and H₂O). The structure of compound II is built of [UO₂(CH₃COO)₃]^? and [UO₂(NCS)₄(H₂O)]^2? complexes, which belong to the AB ₃ ⁰¹ and AM ₅ ¹ crystallochemical groups, respectively. Uranium-containing complexes in both structures are linked into a framework by hydrogen bonds and electrostatic interactions with cesium cations. The IR spectra of compounds I and II agree well with X-ray diffraction data.