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 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 tris-(2,2′,2″)-triaminoethylamino-salicylidene iron(III) complex

Tris-(2,2,2)-triaminoethylamino-salicylidene iron(III) crystallizes in the monoclinic crystal system witha=7.766(2),b=25.423(5),c=13.318(5) Å, =118.04(3)°, space group P2₁/c,V=2320.8(6) ų,Z=4, andD _x=1.464 g cm^–3. The center of the axially distorted octahedron is occupied by the Fe atom which is coordinated by six donor nitrogen and oxygen atoms infac positions. The planes of coordinated atoms (N and O) with the Fe(III) atom are almost planar and the maximum elevated atom from these planes is O(1) (–0.1065 Å).     

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.     

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.     

Synthesis and Crystal Structure of Nickel(II) Complex with 2,2′-Biimidazole and 4-Aminobenzoic Acid

Abstract  The Ni(II) complex, [Ni(H₂biim)₂(PABA)₂]Cl₂·2H₂O, H₂biim being 2,2′-biimidazole, PABA being 4-aminobenzoic acid has been synthesized and the crystal structure determined using X-ray crystallography. The complex crystallizes in triclinic system, space group P − 1 with unit cell parameters a = 8.3920(9) ?, b = 9.8436(11) ?, c = 9.8874(11) ?, α = 94.862(2)°, β = 109.142(2)°, γ = 90.992(2)°, V = 767.95(15) ?³ and Z = 1. The molecules of the complex in the crystal assemble by way of N–H⋯Cl, O–H⋯Cl, O–H⋯O hydrogen bonds as well as π–π stacking interactions to provide a two-dimensional supramolecular structure. Index Abstract  Synthesis and Crystal Structure of Nickel(II) Complex with 2,2′-Biimidazole and 4-Aminobenzoic Acid Yanping Li and Pin Yang* The molecules of the title complex [Ni(H₂biim)₂(PABA)₂]Cl₂·2H₂O in the crystal assemble by way of N–H⋯Cl, O–H⋯Cl, O–H⋯O hydrogen bonds as well as π–π stacking interactions to provide a two-dimensional supramolecular structure.      

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 the inclusion compound between 1,1′-binaphthyl-2,2′-dicarboxylic acid and acetylacetone (1∶1)

The lattice type crystalline inclusion compound of 1,1-binaphthyl-2,2-dicarboxylic acid (BNDA) with acetylacetone (AcAc) 11 has been investigated by single crystal X-ray diffraction. AcAc is present as the enolic tautomer, stabilized by a notably short intramolecular hydrogen bond. This H-bond closes a six-membered ring with delocalization of the system of conjugated double bonds. In the crystal the AcAc molecules are incorporated into channels, delimited by bulky binaphyl moieties, in a hydrogen-bonded framework of BNDA, and they do not show any disorder. The strictly stoichiometric host:guest ratio seems to be enforced by packing forces only.     

Crystal and molecular structure of 1,1′-ferrocene-dicarbaldehyde

The crystal and molecular structure of 1,1-ferrocene-dicarbaldehyde 1 is reported. Crystal data for 1: monoclinic, space group P2₁/n, a = 5.876(1), b = 11.349(1), c = 29.460(3) Å, = 95.067(2)°, V = 1956.9(3) ų, and D _c = 1.64 g/cm³, for Z = 8. The complex crystallizes such that two molecules are located in the asymmetric unit in which the complexes display different degrees of twisting of the cyclopentadienyl (Cp) rings and formyl substituents about the Cp—Fe—Cp and Cp—COH axes, respectively. The molecule self-assembles in the solid state to form a 2D layered structure held together by - interactions and C—H···O hydrogen bonds.     

Crystal and molecular structures of three 2,2′-thio- and 2,2′-sulfonyl-bis(1,3-diarylprop-2-en-1-ones)

The X-ray crystal structures of 2,2-thio- and 2,2-sulfonylbis(1,3-diarylprop-2-en-1-ones) are determined [1: 2,2-thiobis(3-(p-chlorophenyl)-1-phenylprop-2-en-1-one), C₃₀H₂₀Cl₂O₂S, space group C2/c, a = 14.275(3), b = 6.280(1), c = 26.533(5) Å, = 94.55(3)°, Z = 1/2; 2: 2,2-sulfonylbis(1,3-diphenylprop-2-en-1-one), C₃₀H₂₂O₄S, space group P , a = 9.652(1), b = 12.044(1), c = 12.182(1) Å, = 61.985(6), = 77.511(5), = 74.340(6)°, Z = 1; 3: 2,2-sulfonylbis(3-(p-chlorophenyl)-1-phenylprop-2-en-1-one), C₃₀H₂₀Cl₂O₄S, space group P , a = 8.294(1), b = 13.175(2), c = 13.470(1) Å, = 62.870(9), = 83.796(7), = 85.282(8)°, Z = 1]. The C=C double bonds are all clearly defined. The sulfide 1 crystallizes on a crystallographic twofold axis, leading to a symmetric molecular conformation. The sulfones 2 and 3 crystallize on general positions, with different and irregular conformations.     

Crystal and molecular structure of 2-(2′-chloro-5′-nitrostyryl)benzoselenazole

The title compound C₁₅H₉ClN₂O₂Se (nsbse) is orthorhombic, witha=6.823(2),b=7.860(2),c=26.349(5) Å,Z=4,D _x =1.709,(MoK)=28.3 cm^–1,F(000)=720,T=298K in space groupP2₁2₁2₁. The structure was solved by heavy atom and Fourier methods and refined toR=0.045 for 1095 unique observed reflections. The molecule is almost planar, with a dihedral angle of 4.8(2)° between the benzoselenazole and phenyl rings. The C-Se-C angle in the selenazole ring is very small, 84.6(4)°, while the C-N-C angle in that ring is 113.7(7)°.     

Heteropolymetallic complexes of 1,1′-bis(diphenylphosphino) ferrocene (dppf). II. Crystal structure of dppf and NiCl2(dppf)

The crystal structures of dppf [dppf=1,1-bis(diphenylphoshino)ferrocene] and (dppf)NiCl₂ were determined by X-ray crystallography and refined toR=0.043 (both). The molecule of dppf is centrosymmetric, with the inversion center at the Fe atom. The ferrocene rings are parallel and staggered. In (dppf)NiCl₂ the coordination around nickel is tetrahedral, with a significantly large Cl-Ni-Cl angle (125°) due to repulsion of the chlorine atoms. The ferrocene ligand exhibits a slightly distorted (9°) eclipsed conformation, very similar to that observed in (dppf)NiBr₂.     

Crystal structures of 3,5,5′-trichloro-2,2′-bithiophene and 3,3′,5,5′-tetrachloro-2,2′-bithiophene

The crystal structures of 3,5,5-trichloro-2,2-bithiophene (I) and 3,3,5,5-tetrachloro-2,2-bithiophene (II) have been determined by single crystal X-ray diffraction techniques. BothI andII crystallize in the monoclinic crystal system. ForI,a=3.895(2),b=11.928(2),c=10.701(2)Å,=97.70(1)°, space groupP2₁,Z=2 and forII,a=8.942(2),b=3.900(2),c=15.180(2)Å,=92.30(1)°, space groupP2₁/n,Z=2. The structures have been solved by direct methods and all nonhydrogen atoms refined with anisotropic thermal parameters. ForI the final residual is 0.035 (all 1185 independent reflections, MoK radiation) and forII, 0.034 (all 1209 independent reflections, MoK radiation). BothI andII have theanti conformation butI has a torsion angle of 3.4(5)° between the two thiophene rings whileII is completely planar.     

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.     

Syntheses and Crystal Structures of Two New Cadmium(II) and Nickel(II) Complexes with 1,4-Phenylenediacetate and 2,2′-Bipyridyl-Like Ligands

Abstract  

Two new complexes, namely [Cd(PDA)_0.5(2,2′-bpy)Cl](H₂PDA) (1) and [Ni(PDA)(phen)(H₂O)]₂ (2) (H₂PDA = 1,4-phenylenediacetic acid, 2,2′-bpy = 2,2′-bipyridine, phen = 1,10-phenanthroline), have been synthesized and characterized by elemental analysis, IR spectra and X-ray crystal diffraction. Single-crystal X-ray diffraction analysis shows that complex 1 crystallizes in the triclinic space group P-1 with unit cell dimensions a = 8.760 (4) ?, b = 11.190 (5) ?, c = 13.917 (7) ?, α = 110.383 (5)°, β = 101.736 (5)°, γ = 100.612 (5)°, V = 1202.8 (10) ?³, Z = 2, R ₁ = 0.0314 and wR ₂ = 0.0898. Complex 2 crystallizes in the monoclinic space group P2(1)/n with unit cell dimensions a = 9.911 (3) ?, b = 17.924 (6) ?, c = 10.638 (4) ?, β = 94.998 (5)°, V = 1882.7 (11) ?³, Z = 2, R ₁ = 0.0397 and wR ₂ = 0.1150. In complex 1, Cd(II) ions are alternately bridged by PDA ligands and chloride ions into 1D chains and the PDA ligands display trans-configuration. Complex 2 is a dimer and two Ni(II) ions are linked by two PDA ligands with cis-configuration, resulting in a cyclic structure. In spite of these differences, both in complexes 1 and 2 there are π–π stacking interactions and hydrogen bonding to make them 3D supramolecular frameworks.     

Crystal and molecular structure of 2,2′-di-N-methylamino-1,1′ -di-p-hydroxyphenyldiethyleneether dihydrobromide, (C9H12ON·HBr)2O

The structure of the title compound (C₉H₁₂ON·HBr)₂O was determined by X-ray diffraction methods. The crystals are monoclinic:C2/c,a=7.645(2),b=19.777(3),c=13.704(3) Å,=98.32(2)°,V _c =2050.2 ų,Z=4,F(000)=968,D _m =1.62,D _c =1.615 Mg m^–3; MoK radiation (graphite crystal monochromator, =0.71073 Å),(MoK)=4.39 mm^–1. FinalR factor=0.061 andR _w =0.045 for 1566 reflections. The structure was solved by the heavy-atom Fourier method and refined by least-squares procedures. Each asymmetric unit in the unit cell contains one-half of the molecule, with oxygen atom O(2) at a special position with half-occupancy. The molecules are protonated at their nitrogen sites. The structure is stabilized by a three-dimensional network of hydrogen bonds. The ethylamine side chain in the molecular fragment in the asymmetric unit exhibits an extended (trans) conformation that is also found in most of the other adrenergic phenylethylamines.     

X-ray Crystal Structures of Silver Based Molecules Containing 5,5′-Dimethyl-2,2′-bipyridine and 2,2′-bipyridine

Abstract  

The reaction of AgBF₄ with 5,5′-dimethy-2,2′-bipyridine and 2,2′-bipyridine yields three previously unreported compounds. The molecular structures of these compounds were obtained by single-crystal X-ray diffraction. Crystallization of 1 occurs in the centrosymmetric triclinic space group P-1 (No. 2) with a = 13.0069(6), b = 13.5903(6), c = 13.9489(6); and α = 95.677(2), β = 98.995(2), γ = 101.716(2) and Z = 6. Crystallization of 2 occurs in the centrosymmetric monoclinic space group C2/c (No. 15) with a = 23.413(3), b = 11.2116(13), c = 13.0653(13) and β = 123.074(3), and Z = 4. Crystallization of 3 occurs in the centrosymmetric triclinic space group P-1 (No. 2) with a = 12.6843(12), b = 12.8834(13), c = 12.9887(13), and α = 96.172(5), β = 95.149(5), γ = 98.051(6) and Z = 2. Details of the synthesis and the structural characterization of the title compounds are presented and discussed.     

Crystal and molecular structure of 4′-hexyloxyphenyl 4-pentylbenzoate

The molecular and crystal structure of 4??-hexyloxyphenyl 4-pentylbenzoate, C₆H₁₃O-C₆H₄-COO-C₆H₄-C₅H₁₁, which is a liquid-crystal compound, was determined by X-ray diffraction. This compound forms a nematic phase upon melting. The crystal contains three crystallographically independent molecules. In one of them, the alkyl chain is disordered. This is indicative of the looseness of the crystal packing in the aliphatic region. The crystal structure is stabilized by the following two types of weak directional interactions: hydrogen bonds with the participation of the terminal O atom of the ester group and the C-H group of one of the benzene rings and C-H????-system interactions. Only one of the three independent molecules is involved in the latter type of interactions. Hence, the structurization of the mesophase is most likely determined by hydrogen bonding.     

Crystal and molecular structure,and infrared study of bis(2,2′-bipyridine) [N-(toluene-p-sulfonyl)glycinato-NO] cadmium(II) complex and related compounds

A series of complexes of formula [M(II)(bpy)₂(ArSO₂-N-aminoacidato-NO)]·3H₂O [bpy=2,2-bipyridine, M(II)=Zn(II), ArSO₂-N-aminoacidato-NO=N(toluene-p-sulfonyl)- and N(benzenesulfonyl)-glycinate-NO dianion, hereafter abbreviated as tsgly-NO and bsgly-NO, respectively, M(II)=Cd(II), ArSO₂-N-aminoacidato-NO=tsgly-NO] was separated and investigated by spectroscopic and X-ray methods. The crystal structure of [Cd(bpy)₂(tsgly-NO)]·3H₂O was determined. The compound crystallizes in the monoclinic space groupP2/n,Z=4,a=15.427(4),b=13.580(2),c=15.546(4)Å, =110.97(3),R=0.041,R _w =0.043. The structure consists of monomeric, approximately octahedral [Cd(bpy)₂(tsgly-NO)] units with a N₅O donor atom set, which gives rise to three almost orthogonal five-membered chelate rings. The IR spectra suggest similar environments for all the complexes.