Crystal structure analysis of Bis{(N,N′‐dimethylformamide)‐[μ‐bis‐N,N′‐(2‐oxybenzyl)‐1,3‐propanediaminato](μ‐asetato) nickel(II)}nickel(II)

The title compound, a homotrinuclear Ni^II complex has been synthesized from ONNO type Schiff base reduced with the help of NaBH₄. The structure of the complex, [Ni{Ni(CH₃CO₂) (C₁₇H₂₀N₂O₂) (C₃H₇NO)}₂], was identified using elemental analysis, thermal analysis, IR spectroscopy and x‐ray diffraction techniques. It was established that although some bond lengths and angles changed with respect to previous complexes, the Ni…Ni distance was approximately the same.     

Crystal Structure Analysis of {[μ‐N,N′‐Bis(salicylidene)‐2,2′‐dimethyl‐1,3‐propanediaminato](dimethylformamide) zinc(II)}diiodomercury(II)

The title compound, a hetero‐dinuclear complex with Zn^II and Hg^II ions, forms crystals which belong to the monoclinic system, space group P2₁/n, with unit cell dimensions a = 11.2217(12), b = 17.7493(11), c = 13.9293(13) Å, β = 94.830(3)°, V = 2764.5(4) ų. The cell contains four molecules. The Zn…Hg distance is 3.5362(15) Å.     

Crystal structure analysis of {[μ‐N,N′‐Bis(salicylidene)‐1,3‐propanediaminato]nickel(II)}dichloromercury(II)

The title compound, a hetero‐dinuclear complex with Ni(II) and Hg(II) ions, forms crystals which belong to the triclinic system, space group P1, with unit cell dimensions a = 8.9620(12), b = 9.2370(11), c = 12.0810(13) Å, α = 92.100(3)° , β = 105.317(5)°, γ = 110.502(3)°, V = 894.2(2) ų. The cell contains two molecules. The Ni…Hg distance is 3.4859(7) Å. The distance Hg...Hg^a (symmetry code: ‐x,‐y,‐z) between the neighbouring molecules is 4.7514(7) Å. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure analysis of N,N′‐bis(salicylidene)‐2‐methyl‐1,2‐propanediaminato‐nickel(II)

In the title compound, N,N′‐Bis(salicylidene)‐2‐methyl‐1,2‐propanediaminato‐nickel(II), [NiC₁₈H₁₈N₂O₂], (CCDC 235278), the Ni^II atom is coordinated by two iminic N and two phenolic O atoms of the N,N′‐Bis(salicylidene)‐2‐methyl‐1,2‐propanediaminate (SALPD^2‐) ligand. The geometry of the coordination sphere around the Ni atom is distorted square‐planar. Ni(II) ion, forms crystals which belong to the orthorhombic system, space group P cab, with unit cell dimensions a=11.5531(1), b=15.985(4), c=17.418(1) Å, V=3210.5(9) ų. The cell contains eight molecules. The contact distance Ni...Ni^a between the neighbouring molecules is 4.4704(8) Å. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Structure and electrochemical behaviour of Bis[N‐(4‐methylphenyl)salicylaldimine]copper(II) N,N′dimethylformamide solvate

The molecular model of mononuclear complex formed, through a reaction between N‐(4‐methylphenyl)salicylaldimine and Cu^II ion was determined using x‐ray diffraction method. The Cu^II coordination was found to have a distorted square‐planar structure and a cis coordination geometry was observed within the surrounding of the copper. The electro chemical behaviour of the mononuclear copper complex was studied with cyclic voltammetry.     

Schiff bases and their complexes with metal ions. Part II. Structures of N-n-butyl-2-hydroxy-1-naphthaldimine and bis[N-n-pentyl-2-hydroxy-1-naphthaldiminato]nickel(II)

The Schiff base ligand (1), [C₁₅H₁₇NO] crystallizes in the monoclinic space group P2₁/c witha=10.054(3),b=10.313(3), c=13.173(4)Å, =107.42(4)°,V=1303.2(7)ų,Z=4,Dx=1.159 g cm^–3, and (MoK)=0.674 cm^–1. The C2-O[1.23(1)Å] and C3–C4 [1.33(2)Å] bond lengths are short, due to its quinoidal structure. In the Schiff base nickel complex (2), [Ni(C₁₆H₁₈NO)₂] the asymmetric unit is comprised of two half-complexes. It crystallizes in the triclinic space group witha=5.124(3),b=16.227(3),c=16.886(4)Å, =95.47(8), =96.00(1), =90.71(4)°,V=1389.6(9) ų,Z=2,Dx=1.289 g cm^–3, and (MoK) =12.1 cm^–1. The coordination of the Ni(II) ions are square planar with bond angles between 87.9(1) and 92.1(1)°. The Ni–O and Ni–N distances are 1.819(2), 1.922(2) and 1.823(2), 1.914(3)Å in these two complexes.     

Synthesis,crystal and molecular structure of trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II)

Trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II), [Ni(sac)₂(pypr)₂], where sac and pypr are the saccharinate anion and the 2‐pyridinepropanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 8.1981(8), b = 9.9680(10), c = 10.4956(10) Å, α = 90.740(3)° β = 108.142(3)°, γ = 111.025(3)°, Z = 1, V = 1.537 ų. The structure of the nickel(II) complex consists of neutral molecules in which the nickel(II) ion sits on a center of symmetry and is octahedrally coordinated by two sac ligands, and two neutral pypr ligands. The pypr acts as a bidentate N‐ and O‐donor ligand forming a seven‐membered chelate ring, while sac behaves as a monodentate O‐donor ligand via the carbonyl O atom. The Ni‐N bond distance is 2.1016(15) Å, whereas the Ni‐O_pypr and Ni‐O_sac bond distances are 2.1280(12) and 2.0792(11) Å, respectively. The individual molecules are held together with a strong hydrogen bond between the hydroxyl O atom of pypr and N atom of sac and the C‐H…O type weak hydrogen bonds between some ring hydrogen atoms of pypr and sac, and the carbonyl and sulfonyl O atoms of sac in the neighbouring molecules. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,crystal structure and third order nonlinear optical properties of bis(tetra‐n‐propylammonium) bis(2‐thioxo‐1,3‐dithiole‐4,5‐dithiolato)cuprate(II)

A novel bis (dmit) complex of copper (II), [(C₃H₇)₄N]₂[Cu(dmit)₂] ( 1 ), where dmit is 2‐thioxo‐1,3‐dithiole‐4,5‐dithiolate, was prepared and structurally characterized by X‐ray single crystal diffraction. The copper (II) atom is tetracoordinated by four dmit S atoms, forming a nearly square planar arrangement. The [Cu(dmit)₂]^2‐ anions and the [(C₃H₇)₄N]⁺ counter‐cations form a three‐dimensional solid‐state structure by C–H…S hydrogen bonds. The third‐order nonlinear optical properties of the complex were determined by picosecond Z‐scan technique at a wavelength of 1064 nm. The results indicate the compound exhibits reverse saturation absorption and self‐defocusing performance. The molecular second‐order hyperpolarizability γ is calculated to be as high as (1.8±0.2)×10^‐30 esu. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of a ternary mononuclear copper (II) complex: 4‐chloro‐3‐methyl‐6[(N‐2‐picolyl)‐1′‐iminomethyl]phenolato copper(II)perchlorate

The complex crystallizes in monoclinic space group P2₁/n with unit cell parameters a = 7.295(4), b = 19.627(5), c = 12.770(4) Å, β = 101.25(4)º, V = 1793.2(12) ų, Z = 4, ρ = 1.684 Mg/m³ at T = 293(2)K. The structure was solved by Patterson method and refined by full‐matrix least‐squares procedures to final R = 0.0387 using 2906 observed reflections. The asymmetric unit of the complex contains a mononuclear tridentate ligand, a perchlorate group and a methanol molecule. The compound crystallizes as parallel layers of polymeric complex bridged through perchloarate groups. The molecular CuN₂OO′O′′₂ chromophore involves an elongated rhombic octahedral structure and the Cu‐ligand bond shows greater disparity. The five‐membered chelate ring and the pyridine ring lie in the same plane while the six membered chelate ring assumes sofa conformation. A strong O‐H…O inter molecular interaction plays a key role in the formation of dimer along b‐axis. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of (μ‐terephthlato) bis [(N‐Salicylidene ‐N'‐(2‐hydroxyethyl) ethylenediamine) Copper(II)]

The title compound [[Cu(shen)]₂(tp)], {[Cu(C₁₅H₁₇O₄N₂)]2}, where tp = dianion of terephthalic acid and shen = (N‐salicylidene‐N'‐(2‐hydroxyethyl ethylene‐diamine)) has been prepared and its crystal structure determined by single crystal X‐ray diffraction at room temperature. The complex crystallizes in the orthorhombic space group Pbca with four formula units in a unit cell of dimensions a = 12.298(2), b = 14.214(2) and c = 16.436(2)Å. The structure consists of binuclear units with Cu(II) ion bridged by the tp ligand in a bis‐unidentate fashion. The five coordinate Cu(II) complex adopts a distorted square‐based pyramid. A crystallographic inversion center has been located at the center of the benzene ring of the tp bridging ligand. The Cu … Cu distance inside a same binuclear entity is 11.069Å. Intermolecular aromatic ring stacking interactions were observed with the shortest atom to atom contact being 3.423Å.     

Preparation,single crystal growth and characterization of bis(tetrabutylammonium)bis(4,5‐dithiolato‐1,3‐dithiole‐2‐thione)copper

The preparation and single crystal growth of bis(tetrabutylammonium)bis(4,5‐dithiolato‐1,3‐dithiole‐2‐thione)copper, (I), are described. The energy gap Eg of (I) is about 2.38 eV. The nonlinear optical susceptibility χ⁽³⁾ is about 1.3×10^‐3 esu at 1064 nm. The characterization of (I) has been performed by electronic absorption, infrared and X‐ray powder diffraction spectroscopy. The thermal behavior of (I) has been investigated by means of thermogravimetric analysis (TGA) and differential thermal analysis (DTA) measurements in air. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure analysis of {bis‐2,6‐(3,5‐dimethylprazolyl) pyridine‐dicyanato}copper(II)monohydrate

A mononuclear copper(II) complex, [Cu(dmpp)(OCN)₂(H₂O)], was synthesized using 2,6‐bis (3,5‐dimethylpyrazolyl) pyridine (dmpp) and cyanate anion (OCN), and characterized by single crystal X‐ray diffraction. The coordination around the Cu atom is a distorted square‐pyramid involving three N atoms from the dmpp ligand and one N atom from OCN at the basal plane. The O atom of the OCN group is located at the apical position. The Cu atom is located 0.2782(1) Å above the basal plane. The Cu atom is coordinated by different donor atoms of the OCN groups. The complex crystalizes in monoclinic space group P2₁/n, with unit cell dimensions a= 12.4413(12), b=11.1457(13), c=14.2203(12) Å, β=108.817(3)°, V= 1866.5(3) ų. The cell containes 4 molecules. In the crystal, there are three intermolcular and three intramolecular hydrogen bonds interactions. The Cu atom and crystal water O interactions is 5.574 Å. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Nickel(II) complexes with N,N,O-donor Schiff bases. Self-assembly to two-dimensional network via hydrogen bonding

The syntheses, characterization and crystal structures of two mononuclear nickel(II) complexes are described. Reactions of Ni(O₂CCH₃)₂⋅4H₂O with the Schiff bases derived from 2-pyridinecarbaldehyde and ortho-aminophenol (Hpaap) and 2-pyridinecarbaldehyde and ortho-aminobenzoic acid (Hpaab) in methanolic media afford the complexes in good yields. The elemental analysis, magnetic moments, and spectral features of the complexes are consistent with the formulae [Ni(paap)₂]⋅CH₃COOH⋅H₂O and [Ni(paab)₂]⋅2H₂O. Crystal data for [Ni(paap)₂]⋅CH₃COOH⋅H₂O: monoclinic, P2₁/c, a = 9.675(2) Å, b = 17.109(5) Å, c = 14.403(4) Å, β = 92.903(11)^∘, V = 2381.1(11) ų, and Z = 4 and for [Ni(paab)₂]⋅2H₂O: triclinic, P 1, a = 9.834(3) Å, b = 11.319(3) Å, c = 13.130(4) Å, α = 84.68(3), β = 67.54(3), γ = 85.49(2)^∘, V = 1343.4(6) ų, and Z = 2. In each complex, two tridentate monoanionic meridionally spanning ligands form a distorted octahedral N₄O₂ coordination sphere around the metal ion. In [Ni(paap)₂]⋅CH₃COOH⋅H₂O, two metal coordinated phenolate-O atoms are hydrogen bonded to CH₃COOH and H₂O, respectively. Intramolecular C–H⋅ < eqid1 > ⋅O interactions involving the water molecule and the C–H from azomethine and aromatic fragments lead to a two-dimensional network of [Ni(paap)₂]⋅CH₃COOH⋅H₂O in the crystal lattice. An uncoordinated carboxylate O-atom in [Ni(paab)₂]⋅2H₂O is hydrogen bonded to both water molecules. One of the water molecules is again hydrogen bonded to the corresponding symmetry related water molecule forming a dimer. The azomethine groups and the metal coordinated carboxylate-O atoms in [Ni(paab)₂] are involved in intermolecular C–H⋅ < eqid2 > ⋅O interactions forming a chain-like arrangement of the molecules. The water dimers act as bridges between these chains and a two-dimensional network of [Ni(paab)₂]⋅2H₂O is formed.     

Synthesis and crystallographic characterization of a chiral complex of (R)‐2‐(pyridin‐2‐ylmethylene)amino‐2′‐hydroxy‐1,1′‐binaphthyl(L) with hydrated nickel(II) acetate

A chiral complex of (R)‐2‐((pyridin‐2‐ylmethylene)amino)‐2′‐hydroxy‐1,1′‐binaphthyl ( L ) with hydrated nickel (II) acetate has been synthesized and spectroscopically characterized. The crystal structure of [NiL₂(CH₃OH)(CH₃COO)]CH₃COO·CH₃OH has been determined by single‐crystal X‐ray diffraction. The complex crystallizes in the orthorhombic space group P 2(1) 2(1) 2(1) with cell constants a = 15.1035 (19), b = 17.836 (2), c = 18.730 (2)Å, α = β = γ = 90.00°, Z = 4. The structure was solved by direct methods and refined to R = 0.0346 (wR₂ = 0.0863). The analytical result of the crystal structure indicates that a pair of L ligands chelate to a Ni (II) atom in an asymmetric fashion with one Ni‐N bond being longer than the other, the Ni (II) atom is further coordinated by one methanol molecule and one acetate anion to form a distorted octahedral geometry. In the crystal of the complex, the coordination cation [NiL₂(CH₃OH)(CH₃COO)]⁺, the uncoordinated methanol molecule and uncoordinated acetate anion are further assembled into one‐dimensional chain structure via intermolecular hydrogen bonds along the a‐axis. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure of bis[N-(2-fluoro-3-methoxy)-salicylideneaminato]copper(II)

The title compound, bis[N-(2-fluoro-3-methoxy)-salicylideneaminato]copper(II) [Cu(C₁₄H₁₂O₂FN)₂] was synthesized and its crystal structure was determined. The title compound is triclinic, space group P with a = 8.552(1), b = 9.645(1), c = 7.871(1) Å, = 108.708(1), = 93.769(1), = 79.429(1), V = 1208.98(1) ų, Z = 2, D _c = 1.696 gcm_–3, (Mo K) = 1.815 mm^–1, R = 0.0369 for 2963 reflections [I>2(I)]. The title compound has crystallographic inversion symmetry with two bidentate Schiff base ligand coordinated to the Cu atom in a square-planar arrangement. The Cu–N1 and Cu–O2 distances are 1.995(1) and 1.885(1) Å, respectively.     

Synthesis,crystal structure and vibrational characterization of bis‐μ‐peroxo‐hexacarbonatodicerate(IV) complexes of rubidium and cesium

The new compounds Rb₈[Ce(O₂)(CO₃)₃]₂ · 12 H₂O (1) and Cs₈[Ce(O₂)(CO₃)₃]₂ · 10 H₂O (2) were obtained from the reaction of hydrogen peroxide and Ce(III) in saturated alkali carbonate solutions. The crystal structures and the unit cell parameters of (1) triclinic, P‐1 with a = 8.973(2) Å, b = 10.815(2) Å, c = 11.130(3) Å, α = 66.992(2)°, β = 68.337(2)°, γ = 74.639(2)°, V_EZ = 914.7(4) ų, Z = 2, and (2) orthorhombic, Pbca, a = 19.3840(16) Å, b = 18.528(2) Å, c = 10.487(3) Å, V_EZ = 3766.4(13) ų, Z = 8, were determined. Both compounds contain the bis‐µ‐peroxo‐hexacarbonatodicerate(IV)‐ion, [(CO₃)₃Ce(O₂)₂Ce(CO₃)₃]^8‐. IR and Raman spectra were measured and discussed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and X‐ray structure of two conformational isomers of [Zn(medpt)(SCN)2], medpt = bis (3 – aminopropyl)methylamine

Two conformational isomers of [Zn (medpt)(NCS)₂], medpt=bis(3‐aminopropyl) methylamine, (1) and (2) have been synthesised and the crystal structures are determined using single crystal X‐ray diffraction. The structures of the complexes have been solved by Patterson method and refined by full‐matrix least‐ squares techniques to R1 = 0.0524 for (1) and R1 = 0.0506 for (2), respectively. The geometry around the Zn(II) centre in both isomers is distorted trigonal bipyramidal. The two pendent thiocyanate moieties in (1), with Zn–N–C angles 167.9(4)–173.9(4)º, coordinate the mental centre almost linearly while the corresponding coordinations in (2) are significantly bent [Zn–N–C angles 150.8(3)–153.1(2)°]. Intermolecular N–H…S hydrogen bonds stabilise the crystal packing in the complexes forming infinite chains parallel to the [100] direction. The combinations of molecular chains generate three/two dimensional supramolecular framework in complexes (1) and (2). (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

X-ray structure of {[μ-N,N′-Bis(salicylidene)-1, 3-propane-diamine] (dimethylformamide) zinc(II)} dibromo cadmium(ii)

The title compound, forms crystals which are the orthorhombic system, space group P2 ₁2₁2₁, with unit cell dimensions a = 10.3928(12) Å, b = 14.6298(13) Å, c = 15.9514(11) Å, V = 2425.3(4) ų. The cell contains four molecules. The structure is a heteronuclear dimeric complex with Zn^II and Cd^II ions. The coordination around the Zn^II ion is distorted square–pyramid and the Cd^II ion is distorted tetrahedral coordination. The Zn·sCd distance is 3.3594(7) Å.