Crystal structure of new complexes of praseodymium(III) nitrate and ytterbium(III) nitrate with 2,2′: 6,2′′-terpyridine

The crystal structure of new complexes of praseodymium(III) and ytterbium(III) (elements from the initial and final parts of the lanthanide series), namely, [Pr(NO₃)₃ (Terpy)((CH₃)₂CO)] (I) and [Yb(NO₃)₂(Terpy)(H₂O)₂]NO₃ · 2H₂O (II), is investigated. The structure of compound I consists of [Pr(NO₃)₃(Terpy)((CH₃)₂CO)] neutral complexes. The coordination number of the praseodymium atom is 10. The coordination polyhedron of the praseodymium atom can be described as a distorted bicapped tetragonal antiprism. The structure of compound II is composed of [Yb(NO₃)₂(Terpy)(H₂O)₂]⁺ cationic complexes, nitrate anions, and molecules of crystallization water. The structural components are joined together via a three-dimensional system of hydrogen bonds. The coordination polyhedron of the ytterbium atom can be represented as a distorted tricapped trigonal prism. The coordination number of the ytterbium atom is 9.     

Crystal and molecular structure of 2′,4′-dimethoxyflavone

C₁₇H₁₄O₄,M _r =282.3, triclinic,P-1,a=8.469(3),b=8.516(2),c=20.425(8)Å,=84.95(3),=81.98(3), =70.47(2)°,V=1373(13)ų,Z=4,D _x =1.365 g cm^–3, (MoK )=0.71069 Å,=0.91 cm^–1,F(000)=592,T=294K,R=0.038 for 3577 observed reflections (F>3 (F)). The asymmetric unit is composed of two molecules. These two molecules, which are in planar conformations, differ in 4-methoxyl group orientation. Short intramolecular contacts are found between the -benzopyran portion and the dimethoxyphenyl ring.     

Synthesis and crystal structure of Nd(III)–Zn(II) complex

A novel heteronuclear complex, [NdZn₂L₆(NO ₃)(phen)₂] (HL = -methylacrylic acid, phen = 1,10-phenanthroline), was synthesized and characterized by elemental analysis, infrared absorption spectra (IR) and its molecular structure was also determined by X-ray structure analysis. The title complex contains a discrete trinuclear ZnNdZn molecule bridged by carboxylate groups between Zn and Nd ions and crystallizes in space group P¯1 with the cell dimensions: a = 13.601(3) Å, b = 16.859(2) Å, c = 12.575(2) Å, = 110.09(1), = 112.21(1), = 81.10(2).     

Crystal and molecular structure of β-resorcylidene aminoguanidine copper(II) complex

The tridentate Schiff base, -resorcylidene aminoguanidine (RAG)1 was synthesized from 2,4-dihydroxybenzaldehyde and aminoguanidine and complexed with copper(II) to form a copper(II)--resorcylidene aminoguanidine (Cu-RAG)2 complex. X-ray diffraction analysis of compound2 (orthorhombic, Pnma,a=11.674(1);b=6.7198(7);c=17.836(2) ) revealed a square-planar copper(II) cation with a tridentate·ligand bound through two nitrogen atoms (N1 and N3) of the aminoguanidine moiety and an oxygen (O1) of the monodeprotonated dihydroxybenzaldehyde function. The remaining coordination site was occupied by chloride and the structure was rigidly planar as demanded by the restrictions of the crystallographic space group. The unit cell contents exhibited an extended sheet-like structure constructed via hydrogen bonds both intermolecularly and involving two water molecules (O3 and O4) also restricted by the same mirror symmetry. The remaining water (O5) provided for interlayer hydrogen bonding.     

Crystal structure of zinc iodide complex with carbamide, ZnI2 · 2CO(NH2)2

The structure of ZnI₂ · 2CO(NH₂)₂ is determined by single-crystal X-ray diffraction. The crystals are monoclinic, a = 12.694(3) Å, b = 6.886(2) Å, c = 13.161(3) Å, β = 110.58(2)°, Z = 4, space group P2₁/a, and R = 0.0337 for 2481 reflections. Similar to the chloride analogue, the structure consists of discrete molecules with tetrahedrally coordinated Zn atoms. The bond lengths and angles are as follows: Zn-I, 2.5749(8) and 2.5473(8) Å; Zn-O, 1.954(3) and 1.985(4) Å; IZnI, 113.74(3)°; OZnO, 100.5(2)°; and IZnO, 108.5°–113.1(1)°. The crystal structure agrees with the IR and electronic absorption spectra of the crystals.     

Crystal structure of a (μ-bis(carbene))dimetal complex of tungsten

The (-bis(carbene))ditungsten complex, (CO)₅W{(C(OCH₂Ph)C(CH₂C₂H₃)(Me)CH₂CH₂C(OCH₂Ph)}W(CO)₅ (1) is only the fifth such complex to be crystallographically characterized. The steric demands of one side of the bis(carbene) ligand gives rise to small, but statistically significant differences in the bonding parameters to W. The W=C distances are 2.195(4) and 2.171(6)Å. The carbonyltrans to the longest W=C bond has the shortest of the ten W-CO separations (1.994(5)Å) and the longest CO bond length (1.156(6)Å). The planes defined by the two carbene groups have a dihedral angle of 44.5°.     

Crystal structure of phenyl bis(O-isopropylxanthato s,s′)arsenic(III)

The crystal structure of the title compound PhAs(S₂COPrⁱ)₂ has been determined by single crystal X-ray diffraction and refined by full matrix least squares analysis with anisotropic temperature factors. The crystal is monoclinic, space groupP2₁/c,a=8.889(6),b=16.174(19),c=13.506(14) Å,=102.02(7)°,V=1899.2 ų,Z=4,D _c=1.478 g cm^–3, monochromated Mo-K radiation, =0.71069 Å,=22.07 cm^–1.The geometry around the arsenic atom is square pyramidal. Each ligand is bonded to an arsenic atom through two unequal As-S bonds measuring 2.298 and 3.041 Å. The apical position is occupied by a phenyl group and a lone pair of electrons is presenttrans to the phenyl group.     

Crystal and molecular structure of aquabis(2,2′-bipyridine)nitratomanganese(II) nitrate monohydrate

A new monomeric manganese(II) nitrate complex with 2,2-bipyridine (bpy), [Mn(bpy)₂(NO₃)(H₂O)](NO₃)·H₂O, has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group witha=9.721(3),b=14.691(5),c=8.578(3) Å, =106.79(3), =96.05(3), =82.55(3)°,V=1159.9 ų andZ=2. The structure comprises discrete cation [Mn(bpy)₂(NO₃)(H₂O)]⁺ in which the metal atom is coordinated by a pair of bidentate bpy ligands [Mn–N=2.261(4)–2.299(4) Å], a unidentate nitrato [Mn–O=2.284(4) Å] and aqua [Mn–O=2.160(3) Å] ligands in a highly distorted octahedral arrangement.     

Crystal structure of jinshajiangite from the Norra Kärr complex (Sweden)

The structure of the mineral jinshajiangite from the Norra Kärr alkaline complex (Sweden) was determined by single-crystal X-ray diffraction and refined to R = 6.7%. The monoclinic unit-cell parameters are a = 5.350(2) Å, b = 6.909(6) Å, c = 20.96(1) Å, β = 99.83(4)°, sp. gr. P2/m. This mineral is an Fe-rich analogue of surkhobite and perraultite, but it crystallizes in a different space group, and the unit-cell parameters a and b are two times smaller than those of these two minerals. The framework of jinshajiangite from Norra Kärr contains narrow and wide channels, which are occupied by Ca, Na, Ba, and K atoms in an ordered fashion.     

Synthesis and Crystal Structure of μ-oxo-bis[(octaethyloxoporphinato)iron(III)] Tetrafluoroborate

Exposure of dichloromethane solution of [OEOPFe(BF₄)], where OEOP is the monoanion of octaethyloxoporphyrin, to dioxygen results in its transformation into the μ-oxo bridged compound, [(OEOPFe)₂O)](BF₄)₂. The molecular structure of the title compound, [(OEOPFe)₂O](BF₄)₂, was determined by single-crystal X-ray diffraction. It contains a binuclear centrosymmetric [(OEOPFe)₂O]²⁺ cation (the bridging O atom lies on an inversion centre) and two tetrafluoroborate anions. The Fe atom is five-coordinate to four N atoms of the porphyrin ring and to one bridging O atom. The compound is characterized by an average Fe–N bond length of 2.064 Å. The Fe–O bond distance is 1.7665(11) Å and the Fe–O–Fe bond angle is 180.0° and the two porphyrin rings are parallel. Crystal data: crystal system, monoclinic, a = 8.867(3), b = 26.104(9), c = 15.748(6) Å, β = 105.40(3)°, space group, P2₁/c, V = 3514(2) Å³, Z = 2.     

Crystal structure and spectroscopy of a new dmg2−-bridged dinuclear cobalt(III) compound

A new dinuclear complex of formula [Co₂(dien)₂(dmg)₂](ClO₄)₂4.5H₂O (dien = diethlyenetriamine, dmg^2– = dianion of dimethylglyoxime) has been synthesized and characterized by single crystal X-ray diffraction analysis. It crystallizes in the monoclinic space group c2/c, with a = 20.868(7) Å, b = 11.408(4) Å, c = 15.816(4) Å, = 116.97(2), V = 3355.8(17) ų, Z = 4, F(000) = 1732. The structure consists of a dmg^2–-bridged Co(III) dimer. The coordination environments of two Co(III) ions are identical. Each cobalt(III) ion is coordinated by five nitrogen of one dien molecule and one dmg^2– ligand, and the coordination sphere is completed by an oxygen atom of the bridging dmg^2–. The compound is characterized by means of room temperature magnetic susceptibility measurement and infrared spectroscopy.     

Crystal and molecular structure of 4-(3-indolyl)butyric acid-picric acid 2/2 π complex

The title compound, IBA-PIC, is 2C₁₂H₁₃NO₂·2C₆H₃N₃O₇, triclinic,P¯1,a=7.137(1),b=15.355(4),c=18.282(5) Å,=79.72(2),=79.85(2), =76.87(2)°. The structure was solved by direct methods and refined by least-squares techniques to anR factor of 0.068 for 3395 observed reflections. The IBA-PIC complex occurs as two independent molecules with different conformations. The crystallographic evidence for a prominent overlapping between the phenyl and indole rings corroborates earlier conclusions from UV spectroscopy. Molecules of both IBA and picric acid lie approximately parallel to (100) in layers and -bonding interactions across the 3.55 Å spacing. The angles between the indole ring and carboxyl-group planes are 82.9 and 86.9° for the A and B molecules, respectively.     

Crystal structure of 3,3′-dimethoxybenzydine (2-hydroxybenzal)diimine

Molecular and crystal structure of 3,3'-dimethoxybenzydine(2-hydroxybenzal)diimine, C₂₈H₂₄N₂O₄, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a= 18.045(2) Å, b= 11.725(4) Å, c= 12.436(6) Å, = 120.03(3)°, Z=4, D _x =1.32 g/cm³, (MoK) =0.089 mm^–1, and space group is C2/c. The structure was solved by direct methods and refined to a final R=0.056 for 2325 reflections with I > 2(I). There is half independent molecule in the asymmetric unit. The molecule has a twofold symmetry on the mid point of the C4 C4 ⁱ bond. The N1-C8 imine bond length of 1.284(3) Å is typical of a double bond. The molecule of the title compound is not planar. There is a strong intramolecular hydrogen bond between hydroxy oxygen atom and imine nitrogen atom. The crystal structure is stabilized by a weak intermolecular hydrogen bond of the C H O type forming three-dimensional cage.     

Crystal and molecular structure of the photocatalyst tris(2,2′-bipyrazine)ruthenium(II) hexafluorophosphate

The X-ray structure determination of the complex tris(2,2-bipyrazine)ruthenium(II) hexafluorophosphate, [Ru(C₈N₄H₆)₃](PF₆)₂, has shown that the compound crystallizes in the monoclinic space group P2₁/c witha=13.459(5),b=23.486(8),c=17.913(10) Å,=139.85(1)°, andZ=4. Each asymmetric unit also contains one dimethylformamide and one water molecule. Least-squares refinement led to an R factor of 0.074 based on 3463 reflections for which I>2(I). The [Ru(C₈N₄H₆)₃]²⁺ cation has no crystallographic symmetry, but the requirements for point symmetry 32 are nearly met. The six Ru-N bond lengths agree within experimental error and have an average length of 2.05(1) Å.     

Crystal structure and magnetic properties of bis(2,2′-bipyridine) azido copper(II) perchlorate

The title compound has been synthesized and its crystal structure has been solved at room temperature. It crystallizes in the triclinic system, space groupP, witha=7.853(1) Å,b=10.177(1) Å,c=13.651(4) Å,=74.57(1)°,=88.49(1)°, =80.675(4)°, andZ=2. The structure consists of isolated [Cu(bipy)₂N₃]⁺ cations (bipy=2,2-bipyridine) and perchlorate anions. The metallic cation environment has a distorted trigonal-bipyramidal geometry. The EPR spectrum is rhombic, which indicates that the distortion with respect to the perfect trigonal bipyramid is sufficiently pronounced to mixz ²- andx ²–y ²-type orbitals in the ground state. The temperature dependence of the molar magnetic susceptibility has been investigated in the 300-2.2 K temperature range.     

Crystal structure of (ethylenediammonium-N,N′-di-3-propanoic acid) tetrachloropalladate(II) complex

The title compound was obtained by a synthesis from ethylenediamine-N,N-di-3-propanoic acid dihydrochloride (H₂eddp2HCl) and potassium hexachloropalladate(IV) (molar ratio 1:1, in water). Its structure has been determined by single-crystal X-ray diffraction: monoclinic space group P2₁/n, a = 8.198(1), b = 10.282(1), c = 9.080(1) Å, = 103.62(1)°, V = 743.9(2) ų, and Z = 2. The dianionic complex has a square-planar coordination geometry with four chloro ligands, and ethylenediamine-N,N-di-3-propanoic acid as dication in the second coordination sphere. This is the first reported Pd(II) structure with uncoordinated H₂eddp.     

Synthesis and characterization of ternary L-histidine complexes. Crystal structure of (2,2′-dipyridyl)-(L-histidinato-N,N′,O)copper(II) perchlorate 1.5 hydrate

A series of ternary complexes of copper(II), cobalt(II) and zinc(II) with L-histidine, 1,10-phenanthroline, 2,2-dipyridyl or imidazole having perchlorate or acetate as counterions were synthesized and characterized by conventional methods and for [Cu(bipy)(L-hist)]ClO₄·1.5H₂O and X-ray crystal structure was determined. The crystals belong to the monoclinic space groupC2 witha=18.843(3),b=10.582(2),c=11.020(2), =115.20(10)°,Z=4,R=0.0535. The structure is consistent of [Cu(bipy)(L-hist)]⁺ cations, perchlorate ions and water molecules. The geometry around copper is trigonal bipyramidal with one N,N,O tridentate L-histidine molecule and one 2,2-dipyridyl ligand, the apical sites are occupied by the -amino nitrogen [Cu–N(71) 1.995(8)] and by N(11) of 2,2-dipyridyl [Cu–N(11) 1.983(7)], the equatorial plane is formed by the N(3) imidazole -nitrogen [Cu–N(3) 2.140(6)], O(82) carboxylic oxygen [Cu–O(82) 2.009(5)] and N(22) [Cu–N(22) 2.010(7)].     

Crystal and molecular structure of dipotassium-aquapentachlororhodate (III): (K2)++ [RhCl5(H2O)]2−

The structure of K₂[RhCl₅(H₂O)] has been established by X-ray crystallography. It crystallizes in the orthorhombic space groupPcmn, with cell dimensionsa=7.065(1),b=9.453(1),c=13.567(1) Å,V=906.1(3) ų,Z=4,M _r =376.4,D _x =2.76 g cm^–3,F(000)=712,T=293 K. The final wasR=0.046. The rhodium atom has a distorted octahedral coordination involving five chlorine atoms and an oxygen of the water molecule with Rh, O, and three chlorine atoms on the mirror plane. Rh-Cl distances range from 2.284(7) Å to 2.345(7) Å. The Cl(4)O intermolecular distance, 3.140(12) Å indicates strong hydrogen bonding between oxygen and chlorine atoms of the neighboring octahedra.N. C. L. Communication No. 5353.     

Crystal and molecular structure of aqua(2,2′-bipyridine)bis(betaine)copper(II) perchlorate monohydrate

A new monomeric copper(II) complex with 2,2-bipyridine (bpy) and betaine (bet), [Cu(byy)(bet)₂(H₂O)](ClO₄)₂ · H₂O, has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space groupP-1 witha=8.859(2),b=11.191(2),c=14.850(3) Å, =91.41(1), =97.19(1), =91.97(1)°,V=1459.2(7) ų, andZ=2. The structure comprises discrete cations [Cu(bpy)(bet)₂(H₂O)]²⁺ in which the metal atom is coordinated in a distorted square-pyramidal environment by two oxygen atoms from a pair of monodentate carboxylato ligands [Cu–O=1.950(2) Å] and two nitrogen atoms of a bidentate bpy ligand [Cu–N=1.997(3)–2.005(3) Å] on the basal plane, and one aqua [Cu–O=2.267(3) Å] ligand at the apical position.     

The synthesis and crystal structure of one novel ternary complex of 2,2′-bipyridine N-salicylidenetyrosinatocopper(II)

The crystal structure of copper(II)—salicylidene-aminoacidate Schiff base—nitrogen-donor chelating ligand, [Cu(sal-tyr)(bipy)] (sal-tyr: N-salicylidenetyrosinato; bipy: 2,2-bipyridine) which is obtained by means of one-step synthesis, is presented. It crystallizes in space group P2₁2₁2₁ with a = 9.0356(18) Å, b = 11.992(2) Å, c = 20.618(4) Å. The Cu^II ion is five coordinated by one oxygen atom of carboxylate, the imine nitrogen atom, and the hydroxyl oxygen atom of the salicylidene in the Schiff base anion as well as two nitrogen atoms of bipy, resulting in a seriously distorted square pyramid coordination polyhedron. The phenol group and the apical coordination bond Cu(1)–N(2) are in the same side of the Schiff base chelating plane which could be attributed to the intramolecular C–H s interaction between the H(17) of the bipy and the benzene ring of the phenol. The hydrogen bond between the hydroxyl hydrogen atom of the phenol group and the coordinated oxygen atom of the carboxylate from neighboring molecule is helpful to stabilize the crystal.