Crystal structure and EPR spectra of glycilglycilglycinocopper(II)bromide sesquihydrate

The title compound, Cu(glyglygly)Br·1·5H₂O, crystallizes in the space group C2/c, with a = 21.468(7), b = 6.716(5), c = 16.166(6) Å, = 98.39°, and Z = 8. The tripeptide is bonded to one Cu(II) ion through the nitrogen [Cu–N=1.97(1)Å] and oxygen [Cu–O=2.019(8)Å] atoms of the amino end glycine residue and to another Cu(II) through one oxygen atom [Cu–O=1.931(9)Å] of the terminal carboxyl group. This give rise to covalently bonded and infinite ···–Cu–tripeptide–Cu–··· chains. These chains are linked to one another by a network of H-bonds involving the water molecules and bromide ions. The Cu(II) ion is in a distorted tetragonal pyramidal coordination polyhedron. At the corner of the base of the pyramid are the terminal glycine nitrogen and oxygen atoms of one tripeptide, a carboxylic oxygen of another tripeptide and a bromide ion. The fivefold coordination is completed with a water molecule at the top of the pyramid [Cu–Ow=2.286(9)Å]. For all orientations of the applied magnetic field the single crystal EPR spectra display a single anisotropic exchange collapsed resonance without hyperfine structure. Its position was measured in three perpendicular planes and the crystal g-tensor evaluated from the data. This tensor is interpreted in terms of the contributing Cu(II) complexes in the unit cell to deduce the principal values g₁ = 2.273, g₂ = 2.050 and g₃ = 2.131 for the molecular gyromagnetic tensor. We also discuss the magnitude of the exchange interaction between neighboring copper ions in the lattice on the basis of the features in the EPR spectra and the structural information.     

Crystal of catena-(μ2-terephthalato)-bis (N-methylimidazole)-copper(II)

A new one-dimensional chain complex [Cu(ta) (N-MeIm)₂]n (where ta = terephthalic acid dianion,N-MeIm =N-methylimidazole) has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the Monoclinic space groupP2₁/c with the parameters:a = 5.2930(11)Å,b = 14.679(3)Å,c = 11.007(3)Å, β = 104.84(3)^°,V = 826.7(3)ų, withZ = 4 formula units. In the structure, each Cu atom is coordinated by a pair ofN-methylimidazole ligands and a pair of monodentate carboxylate groups, affording a square planar N₂O₂ geometry. Both carboxylate groups of the terephthalate dianion coordinate in a monodentate mode bridging two Cu(II) ions with formation of 1D zigzag chain along thec axis. This supramolecular compound exhibits a three-dimensional solid state structure constituted by hydrogen bonds and C–H–π stacking interactions.     

Crystal structure of a macrocyclic tetraamine isocyanato zinc(II) complex

The complex, [Zn(L)(NCO)]Cl · 3H₂O (1) (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18,0^7.12]docosane), has been synthesized and structurally characterized. 1 crystallizes in the monoclinic system, space group P2₁/n with a = 10.530(3), b = 9.315(2), c = 27.188(3) Å, = 92.58(1)°, V = 2664.1(9)ų, and Z = 4. The zinc atom is in a distorted squarepyramidal environment with the four nitrogen atoms of the macrocycle and one nitrogen atom of the isocyanate ligand.     

Synthesis,Characterization and Crystal Structure of Bis(isothiocyanato)-bis(pyridine) Zinc(II) Crystal

Abstract  Bis(isothiocyanato)-bis(pyridine) zinc(II) crystal has been prepared at room temperature and characterized by elemental analysis, IR spectrum and X-ray single crystal determination. The complex crystallizes in monoclinic space group P2₁/m with unit cell parameters: a = 5.5786(3), b = 11.0587(5), c = 12.1616(6) ?, β = 96.776(3)°, V = 745.03(6) ?³, Z = 2, D _x  = 1.514 g cm⁻³. The X-ray structure determination has revealed that the crystal is centered-symmetrical and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation. Index Abstract  The title compound, bis(isothiocyanato)-bis(pyridine) zinc(II), was synthesized by zinc compound, KSCN and C₅H₅N (pyridine) and its crystal structure was determined. Single crystal X-ray structure determination reveals that the crystal is centered-symmetrical, and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation.      

Crystal structure of a nickel(II) complex with macrocyclic tetraamine

A new compound [Ni(cyclen)(²-CH₃CO₂)]BF₄ (cyclen = 1,4,7,10-tetraazacyclodode- cane) has been synthesized and characterized structurally. It crystallizes in the orthorhombic system, space group Pnnm with a =12.045(5), b =14.906(6), c =8.913(4) Å, V =1600.4(12) ų, and Z =4. The nickel(II) ion has a distorted octahedral geometry with four secondary amines of the macrocycle and two oxygen atoms of the bidentate acetate group. TGA curve shows its thermal stability is up to 280°C.     

Crystal structure of chloritopentamminecobalt(III) tetracyanopalladate(II)

The X-ray crystal structure of [(NH₃)₅Co(ClO₂)][Pd(CN)₄]·H₂O consists of two discrete complex ions and a water of hydration. The red crystals are triclinic, P , with lattice parameters a = 7.1992(5), b = 9.4873(7), c = 11.7752(8) Å. = 66.680(1), = 75.784(1), = 82.203(1)°, and Z = 2 giving a cell volume of 715.27(9) ų and a calculated density of 2.043 g/cm³ at 293°. The chlorite ion is O-bonded to the cobalt atom with amine N—Co distances all equal. The chlorite ion is bent with a O—Cl—O angle of 110.8(2)° and the Cl—O distances being 1.601(3) and 1.558(3) Å, the longer value for the O atom also coordinated to Co. The Pd(CN)^–2 ₄ ions are planar, C-coordinated and stack along the x-axis, separated by 3.599(1) Å and alternatively rotated by 29.9(5)°.     

Crystal and molecular structure of [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II)

The silver(II) complex of the chlorin-like derivativev [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II) (1Ag), formally formed by substitution of one pyrrolic subunit in silvermeso-tetraphenylporphyrin by one ethoxy-substituted hydrooxazole moiety, crystallizes in the tetragonal space groupI4/m witha = 13.4811(10) Å,c = 9.7361(13) Å, andZ = 2. The molecule, which is asymmetric, accommodates the high-symmetry space group by rotational disorder with the silver atom located on the four-fold axis.     

Crystal and molecular structure of benzophenone azine: evidence for an Fe(II) carbene intermediate

Benzophenone azine crystallizes in the monoclinic space groupA2/a (No. 15) witha=16.303(3) Å,b=5.4864(2) Å,c=21.973(5) Å, =85.52(2)°,V=1959.4(8) ų, andD _calc=1.22 g cm^–3 forZ=4. The structure was solved by direct methods and refined againstF to a finalR value of 0.047. The unit cell contains four molecules of the title compound; the asymmetric unit consists of half a molecule. Despite the high crystallographic symmetry, the two halves of the molecule arenot related by a center of symmetry; instead, the molecule adopts C₂ symmetry; the molecular C₂ axis is coincident with the crystallographic twofold axis. The formation of benzophenone azine from the reaction of the iron-containing Lewis acid complex [(⁵-C₅H₅)Fe(CO)₂(THF)]⁺ [BF₄]^– and diphenyldiazomethane provides strong evidence for an Fe(II) carbene intermediate.     

Synthesis and crystal structure of a macrocyclic azidotetraamine copper(II) complex

The complex [Cu(L)N₃](H₂O)(ClO₄) (1) (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18, 0^7.12]docosane) has been prepared and characterized by X-ray crystallography. 1 crystallizes in the monoclinic space group P2₁/c, with a = 8.907(5), b = 20.036(3), c = 14.773(2) Å, = 103.78(2)°, V = 2560.6(15) ų, and Z = 4. The coordination geometry around the Cu(II) ion is a distorted square-pyramidal with four nitrogen atoms of the macrocycle and one nitrogen atom of the axial azido group.     

Crystal structure and vibrational spectra of polyamine-copper(II) complexes

The structures of [Cu(en)(H₂O)₂]SO₄ (I), [Cu(en)₂](NO₃)₂ (II) and [Cu(trien)I]I (III) have been determined by single crystal X-ray diffraction. ComplexI is monoclinic, space group C2/c, with unit cell parametera=7.232(1),b=11.725(2),c=9.768(1), =105.50(1)°, andZ=4. ComplexII is also monoclinic, space group P2₁/a, witha=7.978(2),b=9.982(4),c=8.218(3), =111.11(2)°, andZ=2. ComplexIII is orthorhombic, space group P2₁2₁2₁, witha=8.098(1),b=11.902(1),c=13.682(2), andZ=4. The structures were solved by direct methods and refined by full-matrix least-squares to finalR values of 0.031, 0.043 and 0.036 for complexesI, II, andIII, respectively. ComplexesI andII show an octahedral coordination geometry. ComplexIII shows a square pyramidal coordination geometry. ComplexI forms infinite monodimensional chains where the SO ₄ ^2– ions acts as a bridge between two neighboringen molecules. The vibrational spectra of these complexes agree well with their crystal structures. Structure and stability of seven other related Cu(II) complexes of (trien), (dien)₂, (en)₂ and (en) are inferred in this study.     

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 and spectroscopy of a hydrogen-bridged one-dimensional Cu(II) complex containing both octahedral and square pyramidal geometries in the same unit cell

Single crystals of the helical hydrogen-bridged one-dimensional Cu(II) complex, [Cu(stpy)₂(CH₃COO)₂(H₂O)₂] (1) [Cu(stpy)₂(CH₃COO)₂(H₂O)] (2), are prepared and characterized by elemental and thermal analyses, IR, electronic and X-ray crystal structure determination. The crystals are monoclinic, of space group C2/c, with unit cell parameters a = 31.842(7) Å, b = 5.9829(10) Å, c = 30.970(14) Å, = 111.78(3)°, Z = 4. The asymmetric unit contains two different types of Cu(II) polyhedra, namely, octahedron and square pyramid within the same unit cell. 1 has elongated octahedral geometry with two nitrogen atoms from stpy and two oxygen atoms from synmonodentate acetate ligands, transcoordinated to Cu(II) in the basal plane. The oxygen atoms of the two water molecules occupy the axial positions. 2 has Cu(II) coordination polyhedra similar to 1, except that only one of the apical positions is occupied by a water molecule. The structure consists of two independent linear chains, one involving octahedral (1) and the other involving square-pyramidal (2) polyhedra, held by hydrogen bridges. The Cu–Cu intra- and interchain separations in both 1 and 2 are 5.983 and 8.214 Å. The unit cell packing shows weak -stacking between adjacent coordinated stpy ligands in the chain, resulting in ladder-type structure. Further, the extended packing reveals helical arrangement of Cu(II) polyhedra in the lattice.     

Spectroscopic and crystal structure analysis of diamminebis(2,4,6‐triiodophenolato‐O) copper(II)

The crystal structure of [Cu(C₆H₂I₃O)₂(NH₃)₂] (CCDC 238896) has been determined by x‐ray diffraction. This monomeric centrosymmetric Cu(II) complex crystallizes in the monoclinic system. The CuO₂N₂ coordination sphere is trans ‐planar, [Cu–O: 1.943(5) Å and Cu‐N: 1.972(7)] with the fifth and sixth coordination sites occupied by I atoms from the phenoxide ions [Cu–I₁: 3.3552(8) Å] to form a tetragonally elongated octahedral structure for CuO₂N₂I₂ coordination. The complex molecules hold together in a one dimensional chain true [100] direction by intermolecular hydrogen bonds. Differantial scanning calorimeter, FTIR and magnetic susceptibility measurements were also performed in order to identify the title complex. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystallographic characterization of a six coordinate Cu(II) complex based on hexamethylenetetramine ligand

The title compound, Cu(H₂O)₆]Cl₂.2{(CH₂)₆N₄}.4H₂O ( 1 ), has been prepared under mild hydrothermal conditions. Each Cu^II atom, located on a centre of symmetry, is coordinated by six water molecules in distorted octahedral coordination geometry. The hexamethylenetetramine molecule does not coordinate to the Cu atom but links with the Cu complex via three O—H…N hydrogen bonds. The remaining N atom of the hexamethylenetetramine is hydrogen‐bonded to the solvent water molecule. In the crystal structure, intermolecular O—H…O, O—H…N and O—H…Cl hydrogen bonds link the components into a three‐dimensional network. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

二维异核铜-钠配位聚合物的合成和晶体结构

合成了铜-钠混合金属配位聚合物 [(CuL)2(CH3OO)Na(H2O)4]2 (简写为1)并进行了元素分析和单晶X射线衍射分析,L为{2-(2′-酚基)- Δ 2-噻唑-4-羧酸}.晶体结构分析表明配合物形成Cu4Na2的六核混合金属大环.相邻的Cu4Na2环之间通过进一步的配位作用连结成包含更大的Cu8Na4大环的二维网状结构.该晶体属于三斜晶系Pī空间群,晶胞参数分别为:a = 1.0777(4) nm, b = 1.5221(6) nm, c = 1.6994(6) nm, α = 84.58(1)°, β = 76.31(1)°, γ = 89.97(1) °, V = 2.696 (2) nm3, Z = 2, Mr= 1447.26, dc = 1.783 g·cm-3, T = 293(2) K, μ = 1.816 mm-1, F(000) = 1472, R1 = 0.0794, wR2 = 0.1819 [I>2σ(I)].     

Crystal structure and characterization of 1,2-N,N-disallicydene-phenylamineato nickel(II) complex

A new complex has been synthesized and characterized by elemental analysis, IR, TGA, and single-crystal X-ray analysis. The crystal is orthorhombic and the space group is chiral (P2₁2₁2₁) with a = 6.620(3) Å, b = 17.300(4) Å,, c = 5.450(1) Å,, = 90°, = 90°, = 90°, z = 4. In the crystal lattice, the molecules create a two-dimensional network structure through hydrogen bonds. The C–HO intermolecular hydrogen bonds connect the title complex to form a supermolecular structure.     

Synthesis,Characterization and Crystal Structure Determination of a Hepta-coordinated Cadmium(II) Complex with Thiocyanato-bridges

Abstract  A new cadmium(II) complex [(C₂₈H₂₄N₆)Cd(SCN)₂]₂(CH₃OH)₂ (1) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single crystal X-ray diffraction analysis. The crystallographic data for compound 1: triclinic P1ˉ, a = 9.630(2) Å, b = 11.123(3) Å, c = 15.396(4) Å, α = 106.93(1)°, β = 91.60(1)°, γ = 99.99(1)°, V = 1,548.5(6) Å³, Z = 1, Dc = 1.512 mg/m³, F(000) = 716, R ₁ = 0.0332, wR ₂ = 0.0907. The molecule contains a symmetrical dinuclear unit in which two Cd(II) ions are double bridged by two di-μ-1,3-SCN⁻ anoins with a cadmium–cadmium separation of 6.48 Å. Each Cd(II) ion is seven-coordinated with six nitrogen atoms and a sulfur atom to form a monocapped trigonal prism coordination geometry. In addition, the molecule is further connected by multiform intermolecular C–H···π, π···π interactions and hydrogen bonds to form a three-dimensional supramolecular structure. Graphical Abstract  A hepta-coordinated Cd(II) complex which exhibits a distorted a monocapped trigonal prism coordination geometry has been achieved by using bisbidentate Schiff-base ligand and thiocyanate anion.      

Synthesis and Crystal Structure of the Hydrated Nickel(II) Complex of Tartrate

Abstract  A new dinuclear hydrated nickel(II) tartrate has been isolated and structurally characterized by single-crystal X-ray diffraction. The title compound formulated as [Ni₄(C₄H₄O₆)₄(H₂O)₈](EtOH)_0.5(H₂O)_10.25 (C₁₇H_55.5Ni₄O_42.75) crystallizes in monoclinic system, space group P2(1)/c with a = 13.684(5), b = 17.143(6), c = 18.586(6) ?, β = 96.638(6)°, V = 4331(3) ?³, Z = 4. The unit cell contains two crystallographic independent dimeric units of [Ni₂(C₄H₄O₆)₂(H₂O)₄] without significant structural difference, half of menthol molecule and ten and a quarter packing water molecules. In each dimeric unit, one (R,R)-tartrato dianion chelates two Ni(II) ions by the use of two hydroxy oxygen and two carboxyl oxygen atoms as donor atoms, and another tartrato dianion chelates the same pair of Ni(II) cations in the same way. Each Ni(II) atom is six-coordinated by six O atoms from two tartrate units and two water molecules. Index Abstract  The crystal structure of complex [Ni₄(C₄H₄O₆)₄(H₂O)₈](EtOH)_0.5(H₂O)_10.25 contains two crystallographic independent dimeric units of [Ni₂(C₄H₄O₆)₂(H₂O)₄] without significant structural difference. In each dimeric unit, one (R,R)-tartrato dianion chelates two Ni(II) ions by the use of two hydroxy oxygen and two carboxyl oxygen atoms as donor atoms, and another tartrato dianion chelates the same pair of Ni(II) cations in the same way.      

Crystal structure of bis[dihydrobis(3,5-dimethy-1-pyrazolyl)borato]cadmium(II)

The structure of [H₂B(3,5-Me₂pz)₂]₂Cd shows the four nitrogen donor atoms form a pseudotetrahedral arrangement about the cadmium(II). The intraligand N—Cd—N angles are restricted to an average of 91.4° by the chelate rings forcing the interligand N—Cd—N bond angles to average 119.4°. The Cd—N bond distances average 2.21 Å with a range of 0.04 Å. The crystal is in the triclinic space group, P with a = 7.6793(2) Å, b = 8.5992(2) Å, c = 25.0874(4) Å, = 91.0791(2)°, = 97.9769(4)°, = 110.2344(6)°, and Z = 2.     

Synthesis and crystal structure of tetraiminediphenolate diiron(II) macrocyclic complex

The crystal structure of the binuclear tetraiminediphenolate diiron(II) macrocyclic complex [Fe₂(tidf)(CH₃OH)₄](ClO₄)₂ (tidf = tetraiminediphenolate ligand) is presented. The molecular structure (monoclinic, space group C2/c, Z = 4, a = 20.6903(14)Å, b = 11.0827(11) Å, c = 16.0494(15) Å, = 99.911(6) shows two iron(II) cores occupying distorted octahedral geometries with four methanol molecules bound axially. Main equatorial bond distances are 2.050(3) Å for Fe—O1 and 2.067(4) Å for Fe—N1 with a Fe Fe distance of 3.108(1) Å. Contrasting to the monoiron complex the macrocycle does not adopt a bent conformation being nearly coplanar with the maximum deviation from the least-squares plane of 0.18 Å.