Crystal Structures of Diphosphinated Chromium Fischer Amino Carbenes

The crystal structures of four new diphosphinated chromium Fischer amino carbenes with the compositions fac-[(P-P)(CO)₃Cr=C(NR₂′)(R)] (R = Me, NR₂′ = pyrrolidino, P-P = dppe, 1; R = Me, NR₂′ = pyrrolidino, P-P = dppp, 2; R = Me, R′ = Me, P-P = dppe, 3; R = Me, R′ = Me, P-P = dppp, 4) have been determined at 243 K. Compound 1 crystallizes in the monoclinic system, space group P2₁ /n with a = 12.1597(11) Å, b = 20.1556(17) Å, c = 14.0557(12) Å, β = 114.163(3)°, V = 3143.0(5) Å³, and Z = 4. Compound 2 crystallizes in the triclinic system, space group P ? 1 with a = 7.4424(3) Å, b = 10.8830(5) Å, c = 20.6040(9) Å, α = 100.9880(10)°, β = 91.7650(10)°, γ = 97.6610(10)°, V = 1620.90(12) Å³, and Z = 2. Compound 3 crystallizes in the monoclinic system as a mono-solvate of d⁵-pyridine, space group P2₁ /c with a = 11.485(2) Å, b = 22.825(5) Å, c = 14.092(3) Å, β = 108.53(3)°, V = 3502.7(12) Å³, and Z = 4. Compound 4 crystallizes in the orthorhombic system, space group P2 ₁ 2 ₁ 2 ₁ with a = 8.359(3) Å, b = 15.364(6) Å, c = 23.784(9) Å, V = 3055(2) Å³, and Z = 4. Steric repulsions with the diphosphine ligand favor a conformation with the amino moiety directed away from the diphosphine backbone in 1–4.     

X-Ray Crystal Structure of <Emphasis Type="Italic">trans</Emphasis>-PdCl<Subscript>2</Subscript>(PPh<Subscript>2</Subscript>C<Subscript>12</Subscript>H<Subscript>7</Subscript>S<Subscript>3</Subscript>)<Subscript>2</Subscript>, a New Morphology

Herein we report the crystal structure of trans-PdCl₂(PPh₂C₁₂H₇S₃)₂, 1, in a different morphology than has previously been reported [Stott et al. (Dalton Trans (4):652–653, 2005]. This structure crystallizes in a P-1 space group with a = 9.4249(19) Å, b = 11.540(2) Å, c = 12.559(3) Å, α = 79.07(3)°, β = 78.04(3)°, γ = 69.44(3)°, Z = 1. The earlier structure possessed a P2₁/n space group. Additionally the terthienyl moieties of 1 demonstrate the anti orientation exclusively while the P2₁/n space group structure has some syn and even syn/anti mixed geometries included.     

Solvent-induced Polymorphism of 2-[(2-Amino-phenylimino)-phenyl-methyl]-phenol

The title compound C₁₉H₁₆N₂O crystallize as either triclinic or monoclinic polymorph depending on the solvent used. Polymorph [1] crystallizes from methanol in the space group P \( \mathop 1\limits^ - \) with unit cell dimensions: a = 8.723(2), b = 9.344(2), c = 10.544(2) Å, α = 71.54(2), ß = 78.74(2), γ = 74.15(2)°, and Z = 2. Polymorph [2] crystallizes from benzene with space group P2₁/n with unit cell dimensions: a = 10.230(3), b = 20.536(7), c = 14.563(4) Å, ß = 97.14(3)°, and Z = 8. The only similarity between molecules of [1] and two independent molecules of [2] can be found in almost co-planar phenyl moiety with chelate ring. Both structures are characterized with strong intramolecular O-H···N hydrogen bond. Whereas the molecular interconnections in [2] are based on van der Waals attractions between discrete molecules, molecules of [1] associate in dimers via intermolecular N-H···O hydrogen bonding by the operation of crystallographic centre of inversion.     

Stereoselective Synthesis and X-Ray Structure Determination of Labeled [1, 2, 3-<Superscript>13</Superscript>C<Subscript>3</Subscript>]-1-(Phenylsulfinyl)-3-Benzyloxyacetone

[1,2,3-¹³C₃]-1-(Phenylsulfinyl)-3-benzyloxyacetone, C₁₆H₁₆O₃S, (3) has been synthesized and its crystal structure has been determined by a single-crystal X-ray diffraction analysis. The X-ray diffraction study revealed that compound 3 crystallizes in the monoclinic crystal system in the acentric space group Pc, with cell constants at T = 100 K: a = 16.073(5), b = 5.5079(16), c = 7.949(2) Å, β = 100.221(4)^°, V = 692.6(3) ų, Z = 2, d _calc = 1.383 g/cm³. Compound 3 contains the chiral tetravalent three-coordinated sulfur atom, which has a distorted tetrahedral configuration with a lone electron pair occupying one of the tetrahedron vertices. In the crystal, the molecules are packed in stacks along the b axis; the stacks consist of the molecules of the same chirality. Furthermore, the stacks of the molecules of the opposite chirality alternate along the c axis. The molecules in neighboring stacks are arranged by head-to-tail orientations. There are no short intermolecular contacts in the crystal of 3.     

Synthesis and structural characterization of 2,5-dihalo-3,4-dinitrothiophenes

Using new nitration protocols, we have been able to efficiently dinitrate 2,5-dihalothiophenes with yields of ～80–95%. The resulting products 2,5-dibromo-3,4-dinitrothiophene (1), 2,5-dichloro-3,4-dinitrothiophene (2), 2-bromo-5-chloro-3,4-dinitrothiophene (3), as well as the analogous 2-bromo-3,4-dinitrothiophene (4), all crystallize easily allowing their characterization via X-ray crystallography. Crystallization of 1 occurs in the monoclinic space group C2/c with a = 14.547(3) Å, b = 7.3534(15) Å, c = 10.775(2) Å, β = 128.89(3)°, and Z = 4. Crystallization of 2 occurs in the tetragonal space group I-42d with a = 9.9398(14) Å, b = 9.9398(14) Å, c = 16.866(3) Å, and Z = 8. Crystallization of 3 occurs as a pseudo-merohedral twin in the triclinic space group P-1 with a = 7.340(5) Å, b = 8.094(5) Å, c = 9.112(5) Å, α = 82.059(5)°, β = 66.232(5)°, γ = 63.021(5)°, and Z = 2. Crystallization of 4 occurs in the triclinic space group P-1 with a = 7.1787(14) Å, b = 7.4092(15) Å, c = 8.3151(17) Å, α = 101.67(3)°, β = 96.00(3)°, γ = 116.13(3)°, and Z = 2. The structures of all compounds exhibit the formation of interesting solid-state assemblies due to halogen-bonding interactions between the halogen and nitro groups.     

Molecular structures of chalcone podands: A prognosis of photoinduced transformations in the crystals

A series of chalcone podands with the propenone group in the ortho position of the bridging aryl substituent with respect to the oxyethylene fragment is synthesized. The influence of the preorganization of the chalcone podand molecules in crystals on their ability to participate in topochemical reactions is investigated. From analyzing the X-ray structural data, the highest probability of the solid-state photochemical [2 + 2]cycloaddition is predicted for podands with phenyl substituents and the oxyethylene fragment containing two or three oxygen atoms. The X-ray structural data for the chalcone podand C₃₂H₂₆O₄ (3a) are as follows: a = 7.904(9) Å, b = 14.92(2) Å, c = 21.30(3) Å, β = 91.7(1)°, monoclinic system, space group P2₁/c, Z = 4, V = 2510(5) ų, ρ = 1.26 g/cm³, and R = 0.046; C₃₄H₃₀O₅ (3b): a = 15.738(9) Å, b = 11.889(2) Å, c = 15.0830(15) Å, β = 105.47(14)°, monoclinic system, space group C2/c, Z = 4, V = 2720.0(9) ų, ρ = 1.266 g/cm³, and R = 0.0418; C₃₂H₂₄N₂O₈ (4a): a = 17.9416(18) Å, b = 10.9703(8) Å, c = 41.699(2) Å, β = 105.970(11)°, monoclinic system, space group P2₁/c, Z = 4, V = 2781.4(5) ų, ρ = 1.348 g/cm³, and R = 0.0426; C₃₆H₃₂N₂O₁₀ (4c): a = 7.6286(5)Å, b = 17.9398(10) Å, c = 11.5890(3)Å, β = 95.287(4)°, monoclinic system, space group P2₁/n, Z = 2, V = 1579.27(14) ų, ρ = 1.372 g/cm³, and R = 0.0377; and C₂₈H₂₂O₆ (5a): a = 15.6032(10) Å, b = 8.1131(5) Å, c = 17.7334(11) Å, β = 91.381(5)°, monoclinic system, space group C2/c, Z = 4, V = 2244.2(2) ų, ρ = 1.345 g/cm³, and R = 0.0309.     

Crystal structures of complexes of the <Emphasis Type="Italic">cys-syn-cys</Emphasis> isomer of dicyclohexano-18-crown-6 with oxonium hexafluorotantalate and oxonium hexafluoroniobate

The crystal structures of [(cys-syn-cys-dicyclohexano-18-crown-6 · H₃O)][TaF₆] and [(cys-syn-cys-dicyclohexano-18-crown-6 · H₃O)][NbF₆] complex compounds are determined using X-ray diffraction analysis. The tantalum complex has two polymorphic modifications, namely, the monoclinic (I) and triclinic (II) modifications. The unit cell parameters of these compounds are as follows: a = 8.507(4) Å, b = 11.947(5) Å, c = 27.392(12) Å, β = 93.11(1)°, Z = 4, and space group P2₁/n for modification I; and a = 10.828(1) Å, b = 11.204(1) Å, c = 12.378(1) Å, α = 72.12(1)°, β = 79.40(1)°, γ = 73.70(1)°, Z = 2, and space group P-1 for modification II. The triclinic niobium complex [(cys-syn-cys-dicyclohexano-18-crown-6 · H₃O)][NbF₆] (III) with the unit cell parameters a = 10.796(3) Å, b = 11.183(3) Å, c = 12.352(3) Å, α = 72.364(5)°, β = 79.577(5)°, γ = 73.773(4)°, Z = 2, and space group P-1 is isostructural with tantalum complex II. The structures of all three complexes are ionic in character. The oxonium cation in complexes I–III is encapsulated by the crown ether and thus forms one ordinary and two bifurcated hydrogen bonds with the oxygen atoms of the crown ether. This macrocyclic cation is bound to the anions through the C-H...F contacts (H...F, 2.48–2.58 Å). The conformation of the macrocycle in complex I differs substantially from that in complex II (III).     

Crystal and molecular structures of dimethyl 4-phenylthiosemicarbazidediacetate and its adduct with rhodium(II) acetate

The crystal structures of dimethyl 4-phenylthiosemicarbazidediacetate C₁₃H₁₇N₃O₄S (I) and its adduct [C₈H₁₂O₈Rh₂ (C₁₃H₁₇N₃O₄S)₂] (II) with rhodium(II) acetate are determined by X-ray diffraction analysis. The unit cell parameters of crystals I are as follows: a = 8.066(6) Å, b = 15.812(6) Å, c = 24.977(8) Å, β = 94.88(3)°, space group P2₁/n, and Z = 8. The unit cell parameters of crystals II are a = 8.513(1) Å, b = 16.055(1) Å, c = 16.071(3) Å, β = 104.99(1)°, space group P2₁/c, and Z = 2. In structure I, two crystallographically independent molecules considerably differ from each other in the mutual orientation of the structural fragments containing the ester groups. In the centrosymmetric dimeric complex II, the organic molecule I acts as a monodentate thio ligand and adopts only one conformation.     

Synthesis and structure of Cs[UO<Subscript>2</Subscript>(SeO<Subscript>4</Subscript>)(OH)] · <Emphasis Type="Italic">n</Emphasis>H<Subscript>2</Subscript>O (<Emphasis Type="Italic">n</Emphasis> = 1.5 or 1)

The synthesis and single-crystal X-ray diffraction study of Cs[UO₂(SeO₄)(OH)] · 1.5H₂O (I) and Cs[UO₂(SeO₄)(OH)] · H₂O (II) are performed. Compound I crystallizes in the monoclinic crystal system, a = 7.2142(2) Å, b = 14.4942(4) Å, c = 8.9270(3) Å, β = 112.706(1)°, space group P2₁/m, Z = 4, and R = 0.0222. Compound II is monoclinic, a = 8.4549(2) Å, b = 11.5358(3) Å, c = 9.5565(2) Å, β = 113.273(1)°, space group P2₁/c, Z = 4, and R = 0.0219. The main structural units of crystals I and II are [UO₂(SeO₄)(OH)]^? layers which belong to the AT ³ M ² crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , T ³ = SeO₄ ^2?, and M ² = OH^?). In structure I, johannite-like layers are found. Structure II is a topological isomer of I. The two structures differ in the number of U(VI) atoms bound to the central atom by all bridging ligands.     

Synthesis and Crystal Structure of Tert-butyl 2-((phenylthio)-carbonyl)pyrrolidine-1-carboxylate

Tert-butyl 2-((phenylthio)carbonyl)pyrrolidine-1-carboxylate, was synthesized by using iso-butoxycarbonyl chloride (i-BuOCOCl) via mixed anhydride method. The obtained product was characterized spectroscopically and finally confirmed by X-ray diffraction studies. The title compound C₁₆ H₂₁ N O₃ S crystallizes in the triclinic space group P1 with the cell parameters a = 6.0250(7) Å, b = 8.2820(13) Å, c = 8.7700(14) Å, α = 102.352(4)°, β = 102.993(11)°, γ = 90.279(8)°, V = 415.89(10) Å³ and Z = 1. The proline ring in the structure is in a envelope conformation. The structure exhibits intermolecular hydrogen bonds of the type C–H...O.     

Synthesis,Crystal Structure and Spectral Properties of [Fe<Subscript>3</Subscript>(2,2′-bipy)<Subscript>6</Subscript>(ox)<Subscript>3</Subscript>]·12.25H<Subscript>2</Subscript>O Complex

A novel iron (II) complex of formula [Fe₃(2,2′-bipy)₆(ox)₃]·12.25H₂O (2,2′-bipy = 2,2′-bipyridine, ox = oxalate) has been prepared and structurally characterized by X-ray crystallography. In the complex, the metal atoms are six-coordinated in distorted octahedral environment. In the complex [Fe(ox)₃]^4? anions and water molecules are linked together into 1D chain structure by hydrogen interaction. The red crystal of the complex is monoclinic, space group P2₁/c, with a = 22.932(6) Å, b = 13.715(4) Å, c = 22.493(6) Å, β = 93.177(5)°, and V = 7063(3) Å³ with Z = 4.     

Crystal structures of dioxonium hexafluorotantalate and dioxonium hexafluoroniobate complexes with tetrabenzo-30-crown-10

Two isostructural complexes of dioxonium [H₅O₂]⁺ with tetrabenzo-30-crown-10 of the compositions [(tetrabenzo-30-crown-10 · H₅O₂)][TaF₆] (I) and [(tetrabenzo-30-crown-10 · H₅O₂)][NbF₆] (II) are studied using X-ray diffraction. The complexes crystallize in the monoclinic crystal system (space group C2/c, Z = 4). The unit cell parameters of these compounds are as follows: a = 15.6583(12) Å, b = 15.2259(13) Å, c = 16.4473(13) Å, and β = 99.398(6)° for complex I and a = 15.7117(12) Å, b = 15.2785(15) Å, c = 16.5247(15) Å, and β = 99.398(7)° for complex II. These complexes belong to the ionic type. The dioxonium cation [H₅O₂]⁺ in the form of the two-unit cluster [H₃O · H₂O]⁺ is stabilized by the strong hydrogen bond OH?O [O?O, 2.353(4) Å] and encapsulated by the crown ether. Each oxygen atom of the dioxonium cation also forms two oxygen bonds O?O(crown). The crown ether adopts an unusual two-level (pocket-like) conformation, which provides a complete encapsulation of the oxonium associate. The interaction of the cationic complex with the anion in the crystal occurs through contacts of the C-H?F type.     

X-ray mapping in heterocyclic design: XV. Tricyclic heterocycles based on 2-oxo-2,5,6,7-tetrahydro-1<Emphasis Type="Italic">H</Emphasis>-cyclopenta[<Emphasis Type="Italic">b</Emphasis>]pyridine-3-carbonitrile

The structures of five compounds are studied using single-crystal X-ray diffraction: 2-oxo-2,5,6,7-tetrahydro-1H-cyclopenta[b]pyridine-3-carbonitrile [a = 15.641(8) Å, b = 9.373(5) Å, c = 7.387(4) Å, β = 92.91(5)°, Z = 4, space group P2₁/c]; 1-[2-(4-chlorophenyl)-2-oxoethyl]-2-oxo-2,5,6,7-tetrahydro-1H-cyclopenta[b]pyridine-3-carbonitrile [a = 4.728(4) Å, b = 28.035(11) Å, c = 11.184(3) Å, Z = 4, space group P2₁2₁2₁]; 2-[2-(4-chlorophenyl)-2-oxoethoxy]-6,7-dihydro-5H-cyclopenta[b]pyridine-3-carbonitrile [a = 10.1202(13) Å, b = 11.2484(18) Å, c = 13.4323(19) Å, β = 102.05(1)°, Z = 4, space group P2₁/c]; 2-(4-chlorophenyl)-3a, 6,7,8-tetrahydrocyclopenta[e][1.3]oxazolo[3.2-a]pyridine-4-carboxamide perchlorate [a = 7.702(2) Å, b = 9.599(3) Å, c = 23.798(5) Å, β = 93.44(2)°, Z = 4, space group P2₁/c]; and (3-amino-6,7-dihydro-5H-cyclopenta[b]furo[3.2-e]pyridin-2-yl)(4-chlorophenyl)methanone [a = 7.3273(2) Å, b = 13.390(3) Å, c = 28.792(8) Å, Z = 8, space group Pbca]. The structures are solved using direct methods and refined by the full-matrix least-squares procedure in the anisotropic approximation to R = 0.0580, 0.0724, 0.0469, 0.0477, and 0.0418, respectively.     

C–H...O,C–H...π and π–π stacking interactions in 3-(2,4-dimethylphenyloxymethyl)-3,4-dihydroisocoumarin

3-(2,4-Dimethylphenyloxymethyl)-3,4-dihydroisocoumarin (C₁₈H₁₈O₃) was prepared by the alkylation of o-lithio N-methyl benzamide with 2-(2,4-dimethylphenoxy)methyl oxirane, followed by alkaline hydrolysis. The compound crystallizes in the orthorhombic space group Pbca with unit cell parameters : a = 8.239(2) Å, b = 14.918(5) Å, c = 24.831(9) Å, Z = 8. The crystal structure was solved by direct methods and refined to R = 0.0514 for 1564 observed reflections. The heterocyclic ring adopts a distorted half-chair conformation. Molecules are connected by π–π interactions between phenyl rings of the isocoumarin nucleus forming dimers. Dimers are connected via C–H...O hydrogen bonds forming chains. Further intermolecular C–H...π hydrogen bonds link the dimer chains to form supramolecular structure.     

Synthesis and crystal structure of <Emphasis Type="Italic">catena</Emphasis>-bis(nicotinamide)aqua(μ-phthalato)copper(II) hemihydrate

The copper(II) phthalate complex with nicotinamide [CuL ₂(μ-Pht)(H₂O)] · 0.5H₂O(I) (where L is nicotinamide and Pht ^2? is an anion of phthalic acid) is synthesized and investigated using IR spectroscopy and X-ray diffraction. The crystals of compound I are monoclinic, a = 13.368(2) Å, b = 7.891(3) Å, c = 20.480(2) Å, β = 108.69(2)°, Z = 4, and space group P2₁/c. The structural units of crystal I are linear chains formed by bridging phthalate anions and crystallization water molecules. The copper atom is coordinated by two pyridine nitrogen atoms of two nicotinamide ligands (Cu-N, 2.001 and 2.045 Å), two oxygen atoms of different phthalate anions (Cu-O, 1.964 and 2.235 Å), and the oxygen atom of the H₂ O molecule (Cu-O, 2.014 Å). The coordination polyhedron of the copper atom is completed to an elongated (4 + 1 + 1) tetragonal bipyramid by the second (chelating) oxygen atom of the carboxyl group (Cu-O, 2.587 Å), which is one of the anions of phthalic acid. The linear polymer molecules are joined into complex macromolecular dimers with the closest internal contacts of the specific type. The macromolecular dimers are the main supramolecular ensembles of the crystal structure.     

Crystal structure of zinc(II) hydrated trinuclear complex with monoprotonated ethylenediaminetetraacetate anion(3−), [Zn<Subscript>3</Subscript>(H<Emphasis Type="Italic">Edta</Emphasis>)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)<Subscript>6</Subscript>]

The crystal structure of the [Zn₃(HEdta)₂(H₂O)₆] complex (I) is determined by X-ray diffraction analysis. The crystals are orthorhombic, a = 14.780 Å, b = 29.699 Å, c = 7.032 Å, Z = 4, and space group Pna2₁. The structural units of crystals I are trinuclear linear molecules, in which the peripheral atoms Zn(1) and Zn(2) each coordinate two N atoms and three O atoms of the HEdta ^3? ligand and the O(w) atom of the H₂O molecule, whereas the central Zn(3) atom coordinates four O(w) atoms of the H₂O molecules and two terminal O atoms of the two HEdta ^3? ligands. The HEdta ^3? ligand fulfills a hexadentate chelating—bridging function. The bond lengths are as follows: Zn-O(HEdta), 2.006(4)–2.123(4) Å; Zn-N, 2.214(6) and 2.128(5) Å; and Zn-O(w), 2.006(6)–2.225(5) Å. In structure I, there is a specific contact formed by hydrogen bonds, owing to which the distance between the central atoms of individual molecules appears to be shorter than that in covalently bonded complexes.     

Unclassical hydrogen bonds of C—H⋅<Emphasis Type="Italic">s</Emphasis>O and C—H⋅<Emphasis Type="Italic">s</Emphasis>N in the crystals of 2-amino-3-cyano-4-(3,4-dichlorophenyl)-5-oxo-1,4,5,6-tetrahydro-4H-pyrano[2,3-<Emphasis Type="Italic">d</Emphasis>]pyrimidine

The 2-amino-3-cyano-4-(3,4-dichlorophenyl)-5-oxo-1,4,5,6-tetrahydro-4H-pyrano[2,3-d] pyrimidine (1, C₁₇H₁₅Cl₂N₅O₃) was synthesized and characterized by IR,¹H NMR and elemental analysis. The molecular structure of1 was further studied by using X-ray crystallography. The crystals of compound1 are triclinic, space groupP-1,a = 6.0090(4) Å,b = 10.4056(7) Å,c = 15.6021(11) Å, α = 70.983(4), β = 84.056(6), γ = 84.611(6),Z = 2,V = 915.47(11) ų. Two types of unclassical hydrogen bonds C–H?sO and C–H?sN were presented in the crystals. In addition, there were classical hydrogen bonds in the crystal structure.     

X-ray mapping in heterocyclic design: VI. X-ray diffraction study of 3-(isonicotinoyl)-2-oxooxazolo[3,2-<Emphasis Type="Italic">a</Emphasis>]pyridine and the product of its hydrolysis

The structure of 3-(isonicotinoyl)-2-oxooxazolo[3,2-a]pyridine, C₁₃H₈N₂O₃, (I) is determined by X-ray powder diffraction analysis. Crystals I are orthorhombic, a = 16.610(2) Å, b = 3.853(1) Å, c = 16.431(2) Å, Z = 4, and space group Pna2₁. The structure is solved by the grid search procedure and refined by the Reitveld method (R_p = 0.086, R_wp = 0.115, R_e = 0.030, and χ² = 11.138). The structure of the product of hydrolysis of compound I, C₁₂H₁₀N₂O₂, (II) is determined by the single-crystal X-ray diffraction technique. Crystals II are orthorhombic, a = 8.755(4) Å, b = 10.526(17) Å, c = 23.088(6) Å, Z = 8, and space group Pc2₁b. The structure is solved by the direct method and refined by the full-matrix least-squares procedure to R = 0.0464. A fragment of two fused heterocycles in I is planar. The dihedral angle between the plane of the pyridine ring in the isonicotinoyl fragment and the plane of the bicyclic system is 51.2(2)°. Both exocyclic CO groups that are adjacent to the five-membered fragment contain double bonds. The structures of two crystallographically independent molecules II are almost identical to each other, and the isonicotinoyl fragment is nearly perpendicular to the plane of the pyridone fragment [84.3(1)° and 87.0(1)°].     

Crystal structure of SrFe(<Emphasis Type="Italic">EDTA</Emphasis>)Cl · 5H<Subscript>2</Subscript>O

The crystal structure of the SrFe(Edta)Cl · 5H₂O (I) complex is determined. The crystals are monoclinic, a = 7.530(4) Å, b = 10.575(3) Å, c = 23.308(10) Å, β = 95.75(4)°, Z = 4, and space group P2₁/c. The structural units of I are infinite ribbons of the molecular type that are formed by tetranuclear fragments. A tetranuclear fragment involves the centrosymmetric positively charged dimer group [Sr(H₂O)₄Cl] ₂ ²⁺ at the center and the [Fe(Edta)(H₂O)]_? anionic complexes, which compensate for the positive charge of the dimer group, at the periphery. These constituents are bound via bridging oxygen atoms of the Edta ligands. The coordination number of the Sr atom is nine. The Sr-O bond lengths lie in the range between 2.552 and 2.766 Å, the Sr-Cl bond length is 3.216(3) Å, and the Sr?Sr distance is 4.371(1) Å. The parameters of the [Fe(Edta)(H₂O)]^? group are within the range of values observed in such complexes: Fe-O, 1.996–2.086(3) Å; Fe-O(w), 2.110(4) Å; and Fe-N, 2.289(4) and 2.327(4) Å. Separate ribbons are linked by hydrogen bonds involving all H₂O molecules and terminal oxygen atoms of the Edta ligand.     

Synthesis and structure of oxovanadium(IV) complexes [VO(<Emphasis Type="Italic">Acac</Emphasis>)<Subscript>2</Subscript>] and [VO(<Emphasis Type="Italic">Sal</Emphasis>: <Emphasis Type="Italic">L</Emphasis>-alanine)(H<Subscript>2</Subscript>O)]

Bis(acetylacetonato)oxovanadium C₁₀H₁₄O₅V (I) and (S)-[2-(N-salicylidene)aminopropionate]oxovanadium monohydrate C₁₀H₉NO₅V (II) are synthesized. The crystal structures of compounds I and II are determined using single-crystal X-ray diffraction. Crystals of compound I are triclinic, a = 7.4997(19) Å, b = 8.2015(15) Å, c = 11.339(3) Å, α = 91.37(2)°, β = 110.36(2)°, γ = 113.33(2)°, Z = 2, and space group \(P\bar 1\). Crystals of compound II are monoclinic, a = 8.5106(16) Å, b = 7.373(2) Å, c = 9.1941(16) Å, β = 101.88(1)°, Z = 2, and space group P2₁. The structures of compounds I and II are solved by direct methods and refined to R₁ = 0.0382 and 0.0386, respectively. The oxovanadium complexes synthesized are investigated by vibrational spectroscopy.