Crystal Structure Investigation of 2-Pheny limidazo [f]1,10-phenanthroline

The crystal structure of the title compound (PIP) has been determined by single crystal X-ray diffraction methods. C₁₉H₁₂N₄. C₂H₅OH crystallizes in the monoclinic space group P2₁/n with a = 11.4414(8), b = 12.6052(9), c = 12.4627(8) Å, β = 100.345(2)°, Z = 4, V = 1768.17 ų, D_cal = 1.286 Mg. m⁻³, μ (MoKα) = 0.80 cm^-1, F(000) = 720. The structure was solved by the direct methods and refined by full-matrix least-squares method to a final R = 0.0337 and R_w = 0.0332 for 2306 reflections with F₀ > 4σ(F₀). The phenl ring and the imidazo[f]1,10-phenanthroline moiety are coplanar in the crystal. The packing of the molecules involves hydrogen bonded association of the hydroxyl group of ethanol both with the N H of the imidazole moiety of one PIP and one nitrogen atom of the phenanthroline moiety of another PIP.     

Crystal structure of dinitro(2,9-dimethyl-1,10-phenanthroline)-palladium(II)

Dinitro(2,9-dimethyl-1,10-phenanthroline)-palladium(II) crystallizes in the orthorhombic system, space groupP2₁ nb, with cell dimensionsa = 6·790,b = 19·807,c = 10·625 Å andZ = 4. The structure was determined from three-dimensional Fourier syntheses and refined by full-matrix least squares, the finalR for 1155 measured reflexions being 0·07.     

Synthesis and crystal structure of a new dysprosium(III) complex with 2-fluorobenzoato and 1,10-phenanthroline

The dysprosium complex with 2-fluorobenzoato (2-FBA) and 1,10-phenanthroline (phen) was synthesized and characterized by X-ray diffraction. The complex crystallizes in the triclinic system with space group , lattice parameters: a = 11.233(7)  Å, b = 12.598(8)  Å, c = 22.718(14)  Å, α = 81.045(13)°, β = 78.213(12)°, γ = 80.506(11)°, V = 3079(3) ų, Z= 2, Dcalc = 1.689 Mg/m³. The complex contains two independent binuclear molecules, namely, [Dy(2-FBA)₃·phen·CH₃CH₂OH]₂ (I) and [Dy(2-FBA)₃·phen]₂ (II). In molecule (I), Dy1³⁺ ion is coordinated by eight atoms, five O atoms from five 2-FBA groups, one O atom from an ethanol molecule and two N atoms from the phen ligand. The 2-FBA groups adopt monodentate and bridging two-coordination modes. In molecule (II), the Dy2³⁺ ion is coordinated by nine atoms, seven O atoms from five 2-FBA groups and two N atoms from the phen ligand. The 2-FBA groups adopt chelating, bridging and chelating-bridging three-coordination modes.Supplementary material CCDC-257186 for the compound contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from CCDC, 12 Union Road, Cambridge, CB2 1EZ, UK; fax: (44(0) 1223-336033; email: deposit@ccdc.cam.ac.uk.     

Structure of {Pb[S2CN(C2H5)2]2(1,10-phenanthroline)}2

Lead (II) nitrate reacts with 1,10-phenanthroline and sodium diethyldithiocarbamate in water to produce yellow bisdiethyldithiocarbamata 1,10-phenanthroline lead(II). Crystals from water are triclinic, space group $P\bar 1$ (#2),a=10.53(2) Å,b=11.050(12)Å,c=24.74 (3) Å, α=94.71 (9)⁰, β=98.15(11)^o, γ=114.11(9)^o,V=2569(6) ų,Z=2. Each lead atom has approximate pentagonal pyramid coordination geometry through the nitrogens of a phenathroline and sulfurs of two dithiocarbamates. Additionally, complexes form loose dimers in which lead atoms are weakly coordinated to a sulfur in an adjacent complex. IR and proton nmr spectrum of the complex are consistent with the solid state structure.     

Crystal structures of salicylideneguanylhydrazinium chloride and its copper(II) and cobalt(III) chloride complexes

The crystal structures of salicylideneguanylhydrazinium chloride hydrate hemiethanol solvate (I), salicylideneguanylhydrazinium trichloroaquacuprate(II) (II), and bis(salicylideneguanylhydrazino)cobalt(III) chloride trihydrate (III) are determined using X-ray diffraction. The structures of compounds I, II, and III are solved by direct methods and refined using the least-squares procedure in the anisotropic approximation for the non-hydrogen atoms to the final factors R = 0.0597, 0.0212, and 0.0283, respectively. In the structure of compound I, the monoprotonated molecules and chlorine ions linked by hydrogen bonds form layers aligned parallel to the (010) plane. In the structure of compound II, the salicylaldehyde guanylhydrazone cations and polymer chains consisting of trichloroaquacuprate(II) anions are joined by an extended three-dimensional network of hydrogen bonds. In the structure of compound III, the [Co(LH)₂]⁺ cations, chloride ions, and molecules of crystallization water are linked together by a similar network.     

Crystal structure of tris (phenylammonium) chloride pentachloroantimonate (III) monohydrate

The tris (phenylammonium) chloride pentachloroantimonate (III) monohydrate salt is triclinic with the following cell parameters: a = 9.4283(3), b = 11.4482(3), c = 13.1748(3)Å, = 113.493(2), = 90.381(2), = 97.331(1)°, V = 1290.86(6)ų, with Z = 2 formula units. The structure consists of [C₆H₅NH₃]⁺ cations, water molecules, Cl^– anions, and SbCl₅ square pyramids. Hydrogen bonds, established through water molecule, link the anions [SbCl₅]^2– and Cl^– and make an infinite chain in the [011] direction. Chains are linked together via another hydrogen bond network originating from the ammonium groups. A distortion of the SbCl₅ square pyramid can be attributed to the stereo activity of the Sb(III) lone electron pair.     

Crystal structure and emission study of [(PPh3)2Cu(dmp)-O-(dmp)Cu(PPh3)2]2+ (dmp = 2,9-dimethyl-1,10-phenanthroline)

The synthesis and crystal structure of a luminescent dinuclear Cu(I) complex as the BF^– ₄ salt from toluene and methanol containing triphenylphosphine and -oxo-bis(2,9-dimethyl-1,10-phenanthroline) is described. The coordination geometry about the Cu(I) center is distorted tetrahedral. An unusual feature of the structure is a pseudo-inversion center located near the oxygen atom at approximately 0.51, 0.26, 0.25, such that all of the atoms except for the oxygen are related by a pseudo-inversion center to another atom in the same molecule, as well as by crystallographic inversion to the other molecule in the unit cell. The complex displays luminescence from an MLCT band in fluid solution and emission from both a metal-centered charge-transfer and intraligand (phenanthroline) state at 77K in a chloroform snow. Crystal data: triclinic, P , a = 15.163(2), b = 16.985(2), c = 18.731(2) Å, = 106.458(9), = 91.416(8), = 102.557(9)°, V = 4496(1) ų, and Z = 2.     

Fluoro-containing complexes of chromium (III). II. Crystal structure oftrans-difluorodiaquo-ethylenediaminechromium(III) chloride

The results of an X-ray structure determination of one of the three possible chloride salts of [Cr(en) F₂(OH₂)₂]⁺ show the two fluoro ligands to betrans to each other. The purple crystals are monoclinic in the space groupC2/c-C _2h ⁶ , witha=11.409(3),b=9.319(2),c=10.260(3) Å,β=128.73(2)° andD _c =1.73 g cm^?3 forZ=4. Least-squares refinement based on 1341 independent observed reflections resulted in a finalR of 0.026. The molecule lies on a crystallographic two-fold axis, and the Cr-F, Cr-N, and Cr-O bond lengths are 1.885(1), 2.044(2), and 1.997(2) Å respectively. It is suggested that the ill-defined shoulder in the visible electronic spectrum of this complex is indicative of atrans dihalo geometry.     

Crystal and molecular structure of Bis(N-[pyrid-2-yl]-1-imino-2-carbethoxy-3-oxo-butan-2-ido)-palladium (II)

The crystal and molecular structure of the title compound has been determined by X-ray diffraction techniques. It crystallizes in the orthorhombic space group Pbca with 4 formula units C₂₄H₂₆N₄O₆Pd in the unit cell. The lattice constants are a = 17.259, b = 19.070, and c = 7.480 Å. The structure was solved by the heavy atom technique and refined by least-squares calculations to the conventional R = 0.057. The coordination sphere of palladium as well as the molecular geometry of the ligands are discussed in the paper.     

Improved Photobleaching for (1,10-phenanthroline)tris[4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedionato]europium(III) Particle Embedded in Sol-Gel Derived Glass Film

In this research, we investigated improved photobleaching characteristics of (1,10-phenanthroline)tris[4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedionato]europium(III) by forming nano-particles embedded into a sol-gel derived silica glass film by a conventional sol-gel process. The relative photoluminescence intensities after the UV irradiation for 90 min were 88, 76, and 67% for nano-particles in the sol-gel derived glass film, powders in the sol-gel derived glass film, and raw powders, respectively. This result indicates that the phtobleaching of this Eu-complex can improved by forming nano-partcile structures by a reprecipitation method and embedding in the sol-gel derived silica glass.     

Crystal and molecular structure of trans-bis(dodecylamine) bis(dimethylglyoximato)cobalt(III) nitrite

An octahedral geometry for the molecule of the title complex with very slight distortions around Co(III) is confirmed by single-crystal X-ray diffraction study. The molecular structure of the complex has been shown to contain two dodecylamine moieties in the trans orientations, two N-bonded dimethylglyoximato (DMG) groups and an uncoordinated nitrite ion.     

Coordination properties of sulfonyl-N-aminoacids: Crystal and molecular structure of the [Zn(II) (N-(p-toluenesulfonyl)-L-glutaminate)2(H2O)2] complex

The coordination behavior of N-tosyl-L-glutamine (hereafter abbreviated as tsglnH, tosyl =toluenesulfonyl group) toward the Zn(II) ion is investigated by means of structural and spectroscopic techniques. From aqueous solution, at acidic pH the Zn(II) ion separates a compound of empirical formula Zn(tsgln)₂·2H₂O whose crystal structure is determined. The crystal is monoclinic, space group C2, with cell dimensions:a=19.775(5),b=5.3146(3),c=16.543(8) Å, =119.93(3)°,Z=2. The Zn(II) is tetrahedrally coordinated by two symmetry-related tsgln monoanions acting as monodentate carboxylate ligands and two symmetry related water molecules. The Zn–O bond distances are similar while the angles at Zn(II) ion differ significantly from those of regular tetrahedron. The side chain amide group does not participate in metal coordination and forms intermolecular hydrogen bonds.     

Crystal structure of 2-mercaptobenzimidazole and bis[2-mercaptobenzimidazole]dichlorocobalt(II)

Delocalization of the imidazole electron density is observed in both structures. In the dichlorocobalt complex structure, the two crystallographically independent mercaptobenzimidazole molecules are attached together through the direct bonding of the Co(II) ion with two S atoms. The cohesion of the molecules in the crystals is due to intermolecular N–H...S, and; intra and intermolecular N–H...Cl hydrogen bonds, respectively.     

Crystal and molecular structure of diaquabis(thiocyanato-N)bis(5-methyl-[1,2,4]triazolo[1,5-a]pyridine-N3)cobalt(II), [Co(NCS)2(C6H6N4)2(H2O)2]

The X-ray crystal structure of the title compound, [Co(NCS)₂(C₆H₆N₄)₂(H₂O)₂], has been determined. The crystals are monoclinic, space groupC2/c, with cell dimensionsa=15.6901(5),b=7.9248(10),c=16.1278(12) Å,=94.4(8)°V _c=1999.44 ų,M _r=479.18,Z=4,D _x=1.5918 Mg m³,Cu K radiation (graphite crystal monochromator, =1.54051 Å), (CuK)=39.08 cm^–1,F(000)=980.00 andT=290 K. Final conventionalR-factor=0.051, andR _w=0.053 for 1430 observed reflections and 141 variables. The structure was solved using the programsPatsys andDirdif. The Co atom is octahedrally coordinated (CoN₂O₂N₂ chromophore), with only the 5-methyl-[1,2,4]-triazolo[1,5-a]pyrimidine (5mtp) ligands in thetrans positions. The triazolo pyrimidine rings are planar and coordinated through their N(3) atoms. The H₂O ligands are also H-bond donors to N(4) (intramolecularly) and to the S atoms of the NSC anions (intermolecularly).     

Synthesis and the crystal and molecular structure of two modifications of bis(1,10-phenanthroline)trinitratoerbium(III) Er(NO3)3(Phen)2

Two crystalline modifications (I and II) of the phenanthroline complex of erbium nitrate with the same chemical composition, Er(NO₃)₃(Phen)₂, are synthesized by a procedure similar to that used for preparing the phenanthroline complexes of europium nitrate. The crystal structures of these modifications are determined using X-ray diffraction. Crystals of compound I belong to the isostructural family Ln(NO₃)₃(Phen)₂ (Ln = La-Lu). Crystals of compound II are isostructural to those of modification II (new phase) of the Eu(NO₃)₃(Phen)₂ compound. Crystals of I and II are monoclinic, space group C2/c, and Z = 4. The unit cell parameters are as follows: a = 11.126 Å, b = 17.815 Å, c = 12.976 Å, β = 100.45°, and V = 2529 ų for modification I and a = 9.459 Å, b = 15.463 Å, c = 17.076 Å, β = 93.52°, and V = 2493 ų for modification II. The molecular complexes in the structures of compounds I and II are nearly identical. The mean lengths of the Er-N and Er-O bonds are equal to 2.500 and 2.466 Å in compound I and 2.508 and 2.457 Å in compound II, respectively. The difference between the structures of compounds I and II is associated with the difference between intermolecular interactions in the unit cell.     

Crystal structure of 4-methyl-2-phenylbenzo[de]cyclobut[i] isoquinoline-3,5(2H)-dione

4-Methyl-2-phenylbenzo[de]cyclobut[i]isoquinoline-3,5(2H)-dione, C₂₁H₁₅NO₂, resulted from the photochemical reaction of N-methyl-1,8-naphthalenedicarboximide with phenylacetylene, has been characterized by ¹H NMR, IR, and MS spectra and established by single-crystal X-ray crystallography. The crystal structure belongs to the monoclinic space group P2₁/n with cell parameters a = 12.530(2) Å, b = 9.324(2) Å, c = 13.296(2) Å, = 96.85(1), V = 1542.3(4) ų, and Z = 4.     

X-ray crystal and molecular structure of cis-dichlorobis[1,2-ethanebis(diphenylphosphineoxide)] iron(III)tetrachloroferrate(III), [FeCl2(L-L)2] [FeCl4]

Reaction of iron(III) chloride with 1,2-ethanebis(diphenylphosphine oxide) in an ethanol/chloroform mixture formed a 11 adduct of stoichiometry FeCl₃(L-L) which has been characterized by X-ray crystallography as [FeCl₂(L-L)₂] [FeCl₄]. The structure was solved by the heavy atom method, using MoK diffractometer data and refined by full-matrix least squares toR=0.044 for 8506 observed reflections. The coordination is slightly distorted octahedral for the cation with acis-arrangement of the chlorine atoms and a seven-membered chelate ring formation by Ph₂P(O)CH₂CH₂P(O)Ph₂ with the donor O atoms also in acis arrangement. The Fe-Cl distances are equal at 2.306(1) Å but the Fe-O distances differ significantly in each of the two ligands, (avg. 2.076(2) Å; avg. 1.975(3) Å).