Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.     

Synthesis and characterization of single crystals of the layered copper hydroxide acetate Cu2(OH)3(CH3COO)·H2O

Single‐crystals of the layered copper hydroxide acetate Cu₂(OH)₃(CH₃COO)·H₂O were synthesized by heating copper acetate solution at 60 °C. The standard synthesis of the title compound based on slow titration of copper acetate solution with NaOH yielded materials with worse morphology and an additional phase present. The obtained products were characterized with powder X‐ray diffraction, high temperature powder X‐ray diffraction, scanning electron microscopy and infrared spectroscopy. The crystal structure was determined from single‐crystal X‐ray diffraction data, collected both at 120 K and at 293 K. The title compound crystallizes in the monoclinic botallackite‐type layered structure, space group P 2₁, with the lattice parameters a = 5.5776(3) Å, b = 6.0733(2) Å, c = 18.5134(8) Å, β = 91.802(4)° and a = 5.5875(4)Å, b = 6.0987(4) Å, c = 18.6801(10)Å, β = 91.934(5)° for 120 K and for 293 K, respectively. Acetate groups and water molecules are interlayered between corrugated sheets of edge‐sharing CuO6 octahedra exhibiting strong distortion resulted from the Jahn‐Teller effect. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a novel Ni(II) coordination polymer with dipyrido[3,2‐a:2′,3′‐c]phenazine and 4,4′‐oxy(bisbenzoate)

A novel coordination polymer, [Ni(dppz)(oba)(H₂O)]·0.5H₂O (dppz = dipyrido[3,2‐a:2′,3′‐c]phenazine and oba = 4,4′‐oxy(bisbenzoate)) has been synthesized through hydrothermal method and characterized by IR, and single‐crystal X‐ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 23.163(5), b = 18.211(4), c = 14.460(3) Å, α = γ = 90°, β = 100.45(3)°, V = 5998(2) ų, Z = 2. The structure was solved by direct methods and refined to R = 0.0866 (wR₂ = 0.1836). The compound exhibits interesting one‐dimensional chain structures, which are further stacked through π‐π interactions to form supramolecular double chains. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)     

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.     

Structure and conformation of a nickel complex: {2‐Hydroxo‐3‐piperidine‐1‐yl‐methyl‐N,N′(bis‐5‐bromobenzylpropylenediimine)nickel(II)perchlorate}

The title compound, a nickel complex [C₂₃H₂₆N₃O₂Br₂Ni.(ClO₄)] (CCDC 199520) crystallizes in triclinic space group P with the cell parameters a = 10.2560(4), b = 10.8231(4), c = 12.0888(5)Å, α = 99.404(1), β = 99.780(1), γ = 92.252(1)° and V = 1301.49(9)ų. The structure was solved by Patterson method and refined by full‐matrix least‐squares procedures to a final R = 0.0497 using 6287 observed reflections. In the complex, the piperidine ring takes chair conformation and the geometry around the Ni ion is slightly distorted square planar. The dihedral angle between the planes [N‐Ni‐N and O‐Ni‐O] is 9.4(1)°. The chelate ring containing both the nitrogen atoms adopts twisted boat conformation. The molecules in the crystal are stabilized by N‐H…O and C‐H…O types of hydrogen bonds in addition to a C‐H…π interaction. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,crystal structure and photophysical studies on a ruthenium(II) carbonyl hydrido compound based on 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid (H2bpdc)

A novel complex, namely [Ru^II(PPh₃)(CO)(H)(Hbpdc)]·2MeOH ( 1 ) (H₂bpdc = 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid), has been synthesized from the reaction of H₂bpdc with [Ru^II(PPh₃)₃(CO)(H)₂] in methanol under mild condition and characterized by elemental analysis, IR spectrum, ESI mass spectrometry, and single crystal X‐ray diffraction. The structure shows that the complex crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 11.8984(13) Å, b = 16.5180(18) Å, c = 25.5322(19) Å, β = 115.302(4)°, V = 4536.6(8) ų, Z = 4. This compound features a 1‐D supramolecular chain constructed via hydrogen bonds. Its photophysical properties have been investigated in MeOH solution and in the solid state at room temperature.     

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     

The Crystal Structure of [La(NO3)6{Cu(2,2′-bipy)2}2][La(NO3)6Cu(2,2′-bipy)2]CH3CN with the Most Profuse Modes of Nitrate Coordination

The title compound [La(NO₃)₆{Cu(2,2′-bipy)₂}₂][La(NO₃)₆Cu(2,2′-bipy)₂] CH₃CN was synthesized, the crystal and molecular structures were determined at room temperature. The complex formed monoclinic crystals, space group P21/n (No.14), a = 10.354 (3) A, b = 23.440 (9) A, c = 32.817 (9) A, b = 90.39 (2)°, Z = 4. The crystal structure consisted of a discrete [La(NO₃)₆{Cu(2,2′-bipy)₂}₂]⁺ cation and [La(NO₃)₆Cu(2,2′-bipy)₂]^- anion and a non-coordinated CH₃CN molecule. Each La(III) ion was 12-coordinate with twelve oxygen atoms from six chelating nitrate ligands. There were four modes of nitrate coordination and the coordination geometry of all three copper ions was different in the crystal structure.     

Synthesis and structural characterization of [Ni(Me2NCH2CH2CH2N=CHC6H4O)2]

The synthesis, properties, and X-ray crystal structure of a Ni(II) complex of the tridentate Schiff base ligand Me₂NCH₂CH₂CH₂N=CHC₆H₄OH(LH) are described. The complex crystallizes in the monoclinic space group P2₁/c, with a = 10.180(2), b = 15.169(3), c = 15.293(4) Å, = 106.69(2)°, and Z = 4. The Ni atom shows a distorted fac-octahedral geometry, with the two Ni—N(Me₂) bonds being significantly longer than the two Ni—N(imino) bonds, 2.284(9), 2.310(9) vs. 2.051(2), 2.055(2) Å.     

Self‐assembly of a cadmium(II) diamondoid net with 2‐fold interpenetrating microporous structure

Assembly of 5‐methoxyisophthalic acid (H₂moip) with cadmium(II) ions in the presence of neutral ancillary 1,3‐bis(4‐pyridyl)propane (bpp) yields a new coordination polymer, [Cd(moip)(bpp)(H₂O)]_n·nH₂O ( 1 ). X‐ray single‐crystal diffraction determination reveals that complex 1 crystallizes in the space group C2/c of monoclinic crystal system: a = 14.545(2), b = 18.749(3), c = 17.359(3) Å, β = 105.480(2)º. Complex 1 is a 4‐connected 3D diamondoid topological framework with a 2‐fold interpenetration. Interestingly, the dense adamantine cages with inherent microporous structure are filled with free water molecules to further stabilize the coordination network.     

A hexagonal columnar packing structure of C7 symmetric supramolecules: a superstructure of a 2:3 complex of heptakis‐(6‐O‐tert‐butyldimethylsilyl)‐β‐cyclodextrin and ethyl acetate

The recrystallization of Heptakis[6‐O‐tert ‐butyldimethylsilyl)]‐β ‐cyclodextrin ( 1 ) from ethyl acetate gave single crystals of 1 ₂·(ethyl acetate)₃ complex. The superstructure of 1₂·(ethyl acetate)₃ complex was investigated by ¹H NMR spectroscopy, molecular modeling, and single crystal/powder X‐ray diffractions. Encapsulation of ethyl acetate molecules with 1 and a unique hexagonal columnar superstructure in its crystal were found. (© 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.     

Structural analysis of bis{(N,N′–dimethylformamide) (μ‐formato)[μ‐bis(salicylidene)–1,3‐propanediaminato] nickel(II)} copper(II) and zinc(II) monohydrate hetero‐trinuclear complexes

The two linear hetero‐trinuclear metallic complexes with Cu²⁺, Ni²⁺ and Zn²⁺ ions, [CuNi₂ {(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(I) and [ZnNi₂{(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(II), form crystals which belong to the monoclinic system, space group P2₁/c, with unit cell dimensions a=10.537(4), b=16.612(5), c=13.837(3) Å, β=111.09(5)°, V=2259.8(12) ų in (I) and a=10.525(4), b=16.658(5), c=13.826(3) Å, β=111.11(5) °, V=2261.4(8) ų in (II), respectively. The coordinations around the M (Ni²⁺, Cu²⁺, Zn²⁺) ions in the title complexes are distorted octahedrals. The stereochemistries of the bridge ligands, linking to the metal ions each other, are changed between Ni…M (Cu²⁺, Zn²⁺) distances. The Ni…M (Cu²⁺, Zn²⁺) distances are 3.0469(13) and 3.0645(14), respectively. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Interaction in the molten system Rb2O‐P2O5‐TiO2‐NiO. Crystal structure of the langbeinite‐related Rb2Ni0.5Ti1.5(PO4)3

The interaction in the molten system Rb₂O‐P₂O₅‐TiO₂‐NiO was investigated at different molar ratios Rb/P = 0.5‐1.3, fixed Ti/P = 0.15, Ti/Ni = 1.0 at temperature range 1073–953 K. The conditions of formation of complex phosphates RbTi₂(PO₄)₃, Rb₂Ni_0.5Ti_1.5(PO₄)₃ and RbNiPO₄ have been determined. The new phosphate Rb₂Ni_0.5Ti_1.5(PO₄)₃ (space group P2₁3, a = 9.9386(2) Å) has been obtained and investigated by the single crystal X‐ray diffraction and FTIR‐spectroscopy. It has langbeinite‐like structure, that is built up from mixed (Ni/Ti)O₆‐octahedra and РО₄‐tetrahedra. Rubidium atoms are located in closed cavities of 3D‐framework.     

Synthesis,crystal structure and spectral analysis of diaquatetrakis(N‐methylimidazole)Ni(II)(2,4,6‐tribromophenol)

Diaquatetrakis(N‐methylimidazole)Ni(II)(2,4,6‐tribromophenol), Ni(H₂O)₂(C₃N₂(CH₃))₄^.2(C₆H₃Br₃O), was synthesized via reaction of nickel sulphate and 2,4,6‐tribromophenolate in aqueous media in the presence of N‐methyl imidazole and sodium hydroxide. The complex crystalizes in the triclinic space group P1 with one formula unit of Ni(C₃H₃N₂(CH₃))₄(H₂O)₂.2(C₆H₃Br₃O) in the cell. The coordination around the Ni(II) ion is a slightly distorted octahedron, involving four N atoms from four different di(N‐methyl imidazole) ligand in the basal plane. The two oxygen atoms of the water molecules located at the apical positions result in an octahedral coordination. The two tribomophenol groups in the unit cell are connected via hydrogen‐bonds to the atoms of the coordination sphere, to build one dimensional chains along the a‐axis. For characterization of complex FTIR, UV spectroscopy, DSC and TGA thermal analysis were performed. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of 4‐(1‐methyl‐1‐mesitylcyclobutane‐3‐yl)‐2‐aminothiazole

The crystal structure of 4‐(1‐methyl‐1‐mesitylcyclobutane‐3‐yl)‐2‐aminothiazole (C₁₇H₂₂N₂S₁) has been determined by X‐ray crystallographic techniques. The compound crystallizes in the triclinic space group P‐1 with Z = 6. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.052 for 2298 observed reflections [I > 2σ ( I ) ]. There are three crystallographically independent molecules, I, II and III. These molecules are held together by intermolecular N‐H...N hydrogen bonds. © 2006 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     

Crystal and Molecular Structure of bis[diaaqua(1H‐cyclopenta(2,1‐b:3,4‐b')(dipyridine ‐2,5‐dione))N ickel(II)]dihydrate

The title compound [Ni(CPDD)(H₂O)₂]₂(H ₂O )₂, {]Ni₂(C₄₄H₂₈N₈O₁₂)] (H₂O)₂ }, where CPDD = 1H‐cyclopenta(2,1‐b:3,4‐b')(dipyridine‐2,5‐dione) has been prepared and its crystal structure determined by single crystal X‐ray diffraction at room temperature. The complex crystallizes in the triclinic space group P1 w ith two molecules in the asymmetric unit. The cell dimensions are a=10.452(1),b=14.098(1) & c=16.023 Å; D=110.13(1), E=100.63(1) & J=100.85(1)°. The two independent molecules in the asymmertic unit are related by pseudo two fold symmetry. In both the molecules the coordination environment around the Ni(II) may be best described as a distorted octahedral. Due to some delocalization of charge towards one of the oxygens(O1a) from the O2a atom some degree of bond localization has been observed. The individual diones of both the molecules are almost right angles at the metal atom. A long the y‐axis inversion related molecules are forming pseudo‐dimers through hydrogen bonding.     

Synthesis,Crystal Growth,Structural and Physical Properties of bis(thallium) bis(nitrilotriacetato) zirconate dihydrate,Tl2Zr(N[CH2COO]3)2 · 2H2O

Single crystals of Tl₂Zr(N[CH₂COO]₃)₂ · 2H₂O having optical quality and dimensions up to 30 × 25 × 12 mm have been grown from aqueous solutions by controlled lowering of temperature. The raw material was synthesized as the first fraction of crystallization during evaporation of an aqueous solution of (CH₃NH₃)₂Zr(N[CH₂COO]₃)₂ · 2H₂O and TlNH₂SO₃. A crystal structure analysis revealed an isotypy to the K₂Zr(N[CH₂COO]₃)₂ · 2H₂O family, space group Ccc2, a₁ = 14.780(2)Å, a₂ = 14.933(2)Å, a₃ = 8.901(1)Å, Z = 4, ρ_calc. = 3.145 gcm^‐3. Thermal stability, thermal expansion and pyroelectric, dielectric, piezoelectric, elastic and thermoelastic properties have been determined. All properties are closely related to those of Rb₂Zr(N[CH₂COO]₃)₂ · 2H₂O.