Structural Studies of the 1:1 Complex of <Emphasis Type="Italic">o</Emphasis>-3,4-Dimethyltetrathiafulvalene (<Emphasis Type="Italic">o</Emphasis>-Me<Subscript>2</Subscript>TTF) and 1,2,4,5-Tetracyanobenzene (TCNB)

Abstract  

The synthesis and crystal structure of the 1:1 complex o-Me₂TTF-TCNB is reported. The complex crystallizes in the triclinic space group P-1 with a = 6.920(1) ?, b = 7.928(2) ?, c = 17.453(4) ?, α = 100.53(3)°, β = 99.66(3)°, and γ = 97.32(3)°. The bond length of the central C=C bond in o-Me₂TTF is 1.342(2) ?, indicating a neutral state for the o-Me₂TTF donor.     

Metal Ion Interactions with Pyridinecarboxylates in Tripodal tris(2-Aminoethyl)amine Ligand System: Crystal Structures of [Ni(tren)(pic)]2(ClO4)2·CH3OH and [Co(tren)(dipic)]ClO4·CH3OH

Abstract  

Two new complexes [Ni(tren)(pic)]₂(ClO₄)₂·CH₃OH (1) and [Co(tren)(dipic)]ClO₄·CH₃OH (2), (tren is tris(2-aminoethyl)amine, pic is the anion of picolinic acid, dipic is the dianion of 2,6-pyridinedicarboxylic acid) have been synthesized and structurally characterized. X-ray analysis indicates that the two complexes are mononuclear with tren acting as a quadridentate ligand. In complex 1, the nickel(II) ion is further coordinated with picolinate in μ₂-N, O bidentate chelating mode. In complex 2, the cobalt(III) ion is coordinated with the pyridine nitrogen and one carboxylic oxygen of 2,6-pyridinedicarboxylate in μ₂-N, O chelating form. The metal atoms in both cases have distorted octahedral geometry. Crystal data: [Ni(tren)(pic)]₂(ClO₄)₂·CH₃OH (1), Mr = 869.03, monoclinic, C2/c, a = 26.354(5) ?, b = 10.407(2) ?, c = 25.839(5) ?, β = 96.24(3)°, Z = 8, V = 7045(2) ?³, R ₁ = 0.0418, wR ₂ = 0.1063 [I > 2σ(I)]; [Co(tren)(dipic)]ClO₄·CH₃OH (2), Mr = 501.77, Triclinic, P-1, a = 8.3667(2) ?, b = 10.4434(2) ?, c = 11.9431(16) ?, α = 73.9590(10)°, β = 88.0240(10)°, γ = 75.5890°, Z = 2, V = 969.97(4) ?³, R ₁ = 0.0408, wR ₂ = 0.1063 [I > 2σ(I)].     

Synthesis,Characterization and Crystal Structure of 4,5-Bis(Cyclohexanecarbonylthio)-1,3-dithiolane-2-thione Crystal

Abstract  

A new crystal of 4,5-bis(cyclohexanecarbonylthio)-1,3-dithiolane-2-thione has been prepared at room temperature and characterized by elemental analysis, UV–Vis–NIR absorption spectrum and X-ray single crystal determination. The complex crystallized in triclinic space group P-1 with unit cell dimensions a = 5.37370(10) ?, b = 12.8618(2) ?, c = 15.2481(2) ?, α = 74.8530(10)°, β = 80.6000(10)°, γ = 85.9550(10)°, V = 1003.18(3) ?³, Z = 2, D _x = 1.3861(1) g cm⁻³. The X-ray structure determination revealed that the crystal is centered-symmetrical and the molecules form dimers with a long intermolecular S···S interaction in the crystal.     

Crystal Forms of the Antiepileptic Lamotrigine: Molecular Salts and Solvates with Fluorobenzoic Acid,Nicotinic Acid, 2-Thiobarbituric Acid, 3-Picoline and Butyl Alcohol

Abstract  

The crystal structures of three salts and two solvated multicomponent crystals of lamotrigine with 4-fluorobenzoic acid, nicotinic acid, 2-thiobarbituric acid, 3-picoline and butyl alcohol are reported. Compound 1a crystallizes in monoclinc system, space group P2₁ with a = 13.3860(5) ?, b = 8.3420(3) ?, c = 15.5200(6) ?, β = 93.524(1)°, V = 1729.78(11) ?³, and Z = 2. Compound 1b crystallizes in monoclinic system, space group P2₁/c with a = 10.6625(7) ?, b = 16.2575(11) ?, c = 13.6346(9) ?, β = 100.904(1)°, V = 2320.8(3) ?³, and Z = 4. Compound 1c crystallizes in triclinic system, space group P[`1] \overline{1} , with a = 10.1309(7) ?, b = 12.0260(8) ?, c = 14.0826(10) ?, α = 71.783(1)°, β = 86.451(1)°, γ = 80.902(1)°, V = 1609.10(19) ?<sup>3</sup>, and Z = 1. Compound 1d crystallizes in monoclinic system, space group P2<sub>1</sub>/c with a = 14.9570(10) ?, b = 8.0230(6) ?, c = 13.8162(10) ?, β = 102.884(1)°, V = 1616.2(2) ?<sup>3</sup>, and Z = 4. Compound 1e crystallizes in triclinic system, space group P[`1] \overline{1} , with a = 7.5710(6) ?, b = 8.5721(7) ?, c = 13.5532(11) ?, α = 85.364(1)°, β = 79.632(1) (1)°, γ = 86.188(1)°, V = 861.19(12) ?³, and Z = 2. Characteristic R₂²(8) dimer is observed in all five structures. A complete hydrogen bonded motif analysis is described. Lamotrigine-lamotrigine base pair is observed in all the structures, except in (1b). In (1c), the R₂²(7) dimer is noticed while, in all other structures R₂²(8) dimer exist between the lamotrigine-lamotrigine base pair. In all the six structures, chlorine atoms of the lamotrigine molecules are not involved in any interactions.     

Crystal Structure of Bis[hydrobis(3-phenylpyrazolyl)(5-phenylpyrazolyl)borato]-zinc(II)

Abstract  

The X-ray crystal structure of (C₅₄ H₄₂ B₂ N₁₂ Zn)*2(C H Cl₃) is reported. The title compound is a chloroform-solvated neutral complex crystallizing in the Triclinic space group, P − 1, with two half complexes (each located on a crystallographic center of inversion) and two full chloroform molecules appearing in the asymmetric unit. The capping ligands are related by symmetry and together form, essentially, an octahedral coordination sphere. Strain is apparent in the complex as indicated by asymmetric bond distances and angles. Final statistical data: R = 4.60% with I > 2σ(I), a = 11.2912(8) ?, b = 14.7912(11) ?, c = 17.0047(13) ?, α = 72.3560(10)°, β = 89.8950(10)°, γ = 88.1010(10)°, Z = 2.     

Synthesis,Crystal Structure and DNA Binding Property of Diaquadi(4-methylbenzoyloxy)bis[2-(4-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl 3-oxide]cobalt(II)

Abstract  

A novel cobalt(II) complex of [Co(4-MePhCOO)₂(NITpPy)₂(H₂O)₂] (1), where NITpPy is short for 2-(4-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxy 3-oxide(C₁₂H₁₆N₃O₂), was synthesized and structurally characterized by X-ray diffraction analysis. The X-ray diffraction analysis reveals that 1 crystallizes in the triclinic space group P-1 with a = 6.7910(10) ?, b = 12.4421(15) ?, c = 12.9169(16) ?, α = 89.8470(10)°, β = 89.8480(10)°, γ = 76.991(2)°, and Z = 1. The Co atom in the complex is located on the center of inversion and lies in a distorted octahedral geometry defined by an N₂O₄ donor set. The interaction of 1 with calf thymus DNA (CT-DNA) was investigated by UV–vis absorption and emission spectroscopy, which indicating that 1 could bind to DNA through electrostatic interaction.     

Synthetic and structural studies of the trans bis(2-N-H-pyrrolylcarbaldimine) complexes of nickel(II) and palladium(II)

The molecular bis(2-N-H-pyrrolylcarbaldimine)nickel(II) and palladium(II) complexes are isolated in moderate yield (30–35%) from in situ assembly of the Schiff base with metal(II) salt, base, and pyrrole-2-carbaldehyde in aqueous ammonia solution. The nickel(II) complex, 1, is monoclinic, space group P2₁/c, with a=11.289(6) ?, b=5.611(3) ?, c=8.287(5) ?, β=111.620(6)°, and V=488.0(5) ?³ with Z=2, for d _calc=1.667 Mg/m³. The palladium analog, 2, is isomorphous, space group P2₁/c, with a=11.481(3) ?, b=5.5738(10) ?, c=8.276(2) ?, β=110.923(12)°, and V=494.7(2) ?³ with Z=2, for d _calc=1.965 Mg/m³. In both crystal structures, the metal resides on an inversion center. In the IR spectra, ν(C=N) appears at 1561 cm⁻¹ in 1, and 1557 cm⁻¹ in 2, while ν(N–H) shows at 3345 cm⁻¹ and 3335 cm⁻¹, respectively. The ¹H-nmr spectra reveal the C–H and N–H protons of the imine group as sharp and broad doublets, respectively, at 7.62 and 8.38 δ in 1 and at 7.92 and 9.73 δ in 2.     

Synthesis and Crystal Structures of the Five-Coordinate Diorganotin(IV) Complex [Ph<Subscript>2</Subscript>Sn(L)]·DMF and its 5-Hydroxypyrazoline Ligand (H<Subscript>2</Subscript>L)

Abstract  

A five-coordinate diorganotin(IV) complex [Ph₂Sn(L)]·DMF and its ligand, 5-hydroxy-3-methyl-5-phenyl-(N ⁴-phenylthiosemicarbazone)pyrazoline (H₂L), were synthesized and characterized by elemental analysis, IR, NMR (¹H, ¹³C) spectroscopies and X-ray crystallography techniques. Our studies revealed that H₂L has formed as 5-hydroxy-4,5-dihydropyrazoline derivative in orthorhombic, Pbca space group with a = 15.4330(3) ?, b = 11.5427(2) ?, c = 18.1440(3) ? whereas [Ph₂Sn(L)]·DMF crystallizes with two independent molecules (a and b) in the asymmetric unit in triclinic system, Pī space group with a = 9.2795(1) ?, b = 15.8315(2) ?, c = 19.9895(3) ?, α = 100.855(1)°, β = 92.985(1)°, γ = 102.243(1)°. In molecule a, the central Sn(IV) atom adopts a distorted tetragonal–pyramidal (TTP) geometry with N2 atom at apical position, while in molecule b the Sn(IV) occupies the centre of a trigonal-bipyramid (TBP) with N2 atom of the ONS-tridentate ligand and both Ph groups occupying equatorial positions. One molecule of DMF (crystallization solvent) helps in stabilizing the crystal structure.     

Structures and Characterization of [Zn(n-chlorosalicylato)2(N-methylnicotinamide)2(H2O)2] (n?=?4 or 5) Ligand Isomers

Abstract  

Two ligand isomers [Zn{4-ClC₆H₃-2-(OH)COO}₂(Menia)₂(H₂O)₂] (I) and [Zn{5-ClC₆H₃-2-(OH)COO}₂(Menia)₂(H₂O)₂] (II) (Menia = N-methylnicotinamide) were prepared and characterized by elemental analysis, IR spectroscopy and thermal analysis. The X-ray crystal structures of complexes (I) and (II) were determined. Compound (I) crystallizes in the triclinic space group P[`1] P\bar{1} with a = 8.105(1) ?, b = 10.036(2) ?, c = 10.545(2) ?, α = 109.088(9)°, β = 91.416(8)°, γ = 102.757(9)°, V = 786.2(2) ?<sup>3</sup>, Z = 1. Compound (II) crystallizes in the triclinic space group P[`1] P\bar{1} . Its cell parameters are: a = 8.133(1) ?, b = 10.119(2) ?, c = 10.428(1) ?, α = 66.44(1)°, β = 74.32(1)°, γ = 80.16(1)°, V = 755.5(2) ?³, Z = 1. The molecular structure of both isomers is monomeric. Each Zn(II) atom is hexacoordinated by three pairs of unidentate ligands in trans-positions (ZnO₄N₂). The 5-Clsal complex is somewhat less distorted than 4-Clsal complex (Cl-sal = chlorosalicylate). The structural data are compared with those found in similar [Zn(RCOO)₂(NL)₂(H₂O)₂].     

Inclusion of Caffeine by a Diol Host

Abstract  

The host compound 9,9′-(ethyne-1,2-diyl)-bis(fluoren-9-ol), H, forms inclusion compounds with caffeine (H·CAF) and methanol (H·MeOH). The host and guest ratios were 1:2 and 1:1, respectively. Both of these structures were successfully solved in P-1 with unit cell dimensions for H·CAF: a = 7.2121(14) ?, b = 9.2782(19) ?, c = 15.206(3) ?, α = 73.23(3)°, β = 84.20(3)°, γ = 73.39(3)°, Z = 2 and for H·MeOH : a = 9.7592(10) ?, b = 11.2584(11) ?, c = 20.7854(19) ?, α = 97.161(2)°, β = 99.263(2)°, γ = 95.257(2) ?, Z = 2. These crystal structures were studied together with that of a mixed clathrate, H·CAF·MeOH with stoichiometry 2:1:1.5. For H·CAF·MeOH which was solved in P2₁/c : a = 12.2051(5) ?, b = 46.8023(19) ?, c = 9.0121(4) ?, β = 91.9650(10)°, Z = 4. The kinetics of desolvation of the methanol solvate (H·MeOH) yielded an activation energy of 69.6–83.9 kJ mol⁻¹.     

Synthesis and Crystal Structure of the Coordination Polymer [Cu(ppca′)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)(HgI<Subscript>2</Subscript>)](H<Subscript>2</Subscript>O) (ppca′ = 3,4′-bipyridine-6-carboxylic acid)

Abstract  

The coordination complex Cu(ppca′)₂(H₂O)₂ (1) was synthesized hydrothermally using the ligand 3,4′-bipyridine-6-carboxylic acid (ppca′). Complex 1 consists of pseudo-octahedral copper (II) units hydrogen bonded into a three-dimensional network that crystallizes in the monoclinic P2₁/n space group. In complex 1, a = 5.3429(4) ?, b = 29.343(2) ?, c = 6.7940(5) ?, and β = 110.635(2)°.     

C–H···F Hydrogen-Bonded Assembly of Ni(II) and Cu(II) Complexes Generate 3D Supramolecular Frameworks

Abstract  Syntheses and X-ray structural characterizations of two new complexes [Ni(imi)₆](pfbz)₂ (1) and Cu(imi)₂(pfbz)₂ (2) (imi = imidazole, pfbz = pentafluorobenzoate) are reported. The first complex crystallizes in the triclinic space group P-1 with the crystal cell parameters a = 9.180(2) ?, b = 9.742(3) ?, c = 11.466(3) ?, α = 76.947(18)°, β = 80.629(18)°, γ = 78.043(19)°, V = 970.0(4) ?³ and Z = 1. The second complex crystallizes in the triclinic space group P-1 with the crystal cell parameters a = 7.3250(12) ?, b = 7.6685(10) ?, c = 10.888(4) ?, α = 92.80(2)°, β = 101.92(2)°, γ = 115.038(12)°, V = 535.7(2) ?³ and Z = 1. Examination of the structures shows that both complexes form three-dimensional hydrogen bonded networks in which C–H···F hydrogen bonds play significant roles. Index Abstract   C–H···F Hydrogen-Bonded Assembly of Ni(II) and Cu(II) Complexes Generate 3D Supramolecular Frameworks Chun-Hua Ge, Xiao-Yan Zhang, Fang Yu, Ya-Nan Guo, Xiang-Dong Zhang* and Qi-Tao Liu C–H···F interactions link simple complexes to form intricate three-dimensional supramolecular networks.      

Synthesis and Crystal Structures of the Coordination Polymers Pb(PYTAC)<Subscript>2</Subscript> and Pb<Subscript>2</Subscript>(PYTAC)<Subscript>3</Subscript>(NO<Subscript>3</Subscript>) (PYTAC = 2-(pyridin-4-yl)thiazole-5-carboxylate)

Abstract  

Two lead coordination compounds, Pb(PYTAC)₂ (1), and Pb(PYTAC)₂(NO₃) (2), were grown as single crystals via hydrothermal synthesis (PYTAC = 2-(4-pyridyl) thiazole-4-carboxylate). Both compounds have been identified via single crystal X-ray diffraction. Coordination polymer 1 crystallizes in a triclinic space group P-1 (a = 5.5097(4) ?, b = 7.2822(5) ?, c = 11.3134(8) ?, α = 103.5580(10)°, β = 99.4330(10)°, γ = 97.1050(10)°), and forms 2-D layers parallel to the crystallographic (ac) plane. Coordination polymer 2 crystallizes in a triclinic space group P-1 (a = 9.8102(5) ?, b = 10.5972(6) ?, c = 14.8076(8) ?, α = 91.9350(10)°, β = 100.8050(10)°, γ = 103.1350(10)°), and forms an infinite 1-D chains along the a axis.     

Preparation, Characterisation and Crystal and Molecular Structure of [N2H5Cu(HEDTA)]H2O

Abstract  

New hydrazinium copper(II) hydrogen ethylenediaminetetraacetate monohydrate, [N₂H₅Cu(HEDTA)]H₂O has been prepared and characterized by analytical, spectral and thermal techniques. The conductivity value indicates the non-electrolyte nature of the complex. Analytical and bond length measurements indicate the distorted octahedral geometry around the copper ion with EDTA acting as pentadentate ligand. The crystal structure of the complex has been determined from single crystal X-ray analysis. The complex crystallizes in orthorhombic system; space group Pccn. The unit cell parameters are a = 25.1858(14) ?, B = 7.3305(4) ?, C = 15.8291(9) ?, α = 90°, β = 90°, γ = 90°, V = 2,922.4(3) ?³ and Z = 8. The copper ion is six coordinated, three carboxylate oxygen atoms and two nitrogen atoms from EDTA occupy five coordination sites, while the sixth site is occupied by hydrazinium cation and a water molecule present outside coordination sphere as lattice water. The complex undergo multi-step degradation to give copper oxide as the final residue.     

Synthesis and Characterization of Some Transition Metal Complexes with Mixed Adenine and Acetylacetonate Ligands: Crystal Structures of Solvated Complex {[Cu(acac)<Subscript>2</Subscript>(adenine)]·EtOH} and {[Cu(acac)<Subscript>2</Subscript>(adenine)]·DMF·H<Subscript>2</Subscript>O}

Abstract  

Metal complexes of divalent copper (1–2), cobalt (3), and nickel (4) with mixed ligands acetylacetone (acac) and adenine were prepared and characterized by IR, mass spectra, elemental and thermal analysis. The X-ray crystal structures of {[Cu(acac)₂(adenine)]·EtOH} complex (1) and {[Cu(acac)₂(adenine)]·DMF·H₂O} (2) were determined. Compound (1) crystallizes in the triclinic space group P − 1 with a = 7.547(3) ?, b = 7.828(3) ?, c = 17.791(6) ?, α = 79.538(6)°, β = 82.240(7)°, γ = 86.010(6)°, V = 1023.1(6) ?³, and Z = 2. Complex (1) forms a hydrogen bonded 2:2 complex {[Cu(acac)₂(adenine)]₂:[EtOH]₂} arranged in bilayers. Complex (2) crystallizes in the triclinic space group P − 1 with a = 7.828(2) ?, b = 8.095(2) ?, c = 16.995(5) ?, α = 78.508(5)°, β = 84.949(5)°, γ = 89.285(5)°, V = 1051.2(5) ?³, and Z = 2. Complex (2) also forms bilayers with H-bonded DMF. Thermal analysis TG and DSC of the compounds (25–800 °C, under N₂) reveals the disproportionation of ligands with the associated heat.     

Dichloro-{bis(Pyrazol-1-yl)}Palladium(II) Complexes: Structures of a DMSO Solvated Dichloro-{bis(3,5-Dimethylpyrazol-1-yl)Acetic Acid}Palladium(II) and Dichloro-{bis(3,5-Ditertbutylpyrazol-1-yl)Methane}Palladium(II)

Abstract  Two new palladium(II) complexes, dichloro-{bis(3,5-dimethylpyrazol-1-yl)acetic acid}palladium(II)PdCl₂(3,5-Me₂bpza)], (1) (3,5-Me₂bpza = 3,5-dimethylpyrazol-1-yl)acetic acid) and dichloro-{bis(3,5-ditertbutylpyrazol-1-yl)acetic acid}palladium(II), [PdCl₂(3,5-^tBu₂bpza)], (2a) [3,5- ^t Bu₂bpza = 3,5-ditertiarybutylpyrazol-1-yl)acetic acid] complexes, were synthesized from the reactions of pyrazol-1-yl ligands with palladium salts. Attempts to crystallize 2a led to a hydrolyzed product, dichloro-{3,5-ditertbutylpyrazol-1-yl}palladium(II) (2b), in which the acetic acid moiety in the ligand backbone of 1 is lost. Both complexes 1 and 2b have been characterized by single-crystal X-ray crystallography. Both complexes crystallized in triclinic system (P − 1 space group). The cell parameters are: complex 1 (a = 8.7960(14) Å, b = 16.238(2) Å, c = 16.430(2) Å, α = 78.038(10)°, β = 77.817(11)°, γ = 89.970(10)°) and complex 2b (a = 10.1492(2) Å, b = 12.4001(2) Å, c = 13.108(3) Å, α = 103.0690(10)°, β = 97.4120(10)°, γ = 107.2450(10)°). The asymmetric unit of 1 contains two crystallographic independent monomeric units of 1 and three molecules of DMSO solvent, whilst that of 2b has got one monomeric unit with one molecule of chloroform solvent. Index Abstract  Two palladium complexes, dichloro-{bis(3,5-dimethylpyrazol-1-yl)acetic acid}palladium(II), PdCl₂(3,5-Me₂bpza)], (1) (3,5-Me₂bpza = 3,5-dimethylpyrazol-1-yl)acetic acid) and dichloro-{bis(3,5-ditertbutylpyrazol-1-yl)acetic acid}palladium(II), [PdCl₂(3,5- ^t Bu₂bpza)], (3,5- ^t Bu₂bpza = 3,5-ditertiarybutylpyrazol-1-yl)acetic acid) complexes, were synthesized from the reactions of pyrazol-1-yl ligands with palladium salts. Attempt to obtain crystals of tertiarybutylpyrazolyl analogue led to hydrolysis, the crystal structure of the hydrolysis product was established by single crystal X-ray crystallography.      

Synthesis and Characterization of a Novel Unsymmetrical Tetradentate Schiff Base Complex of Zinc(II) Derived from N,N′-bis (5-Bromosalicylidene) 2,3-Diaminopyridine (H2L): Crystal Structure of [Zn(II)L]Pyridine

Abstract  

Yellow crystals of [Zn(N,N′-bis (5-bromosalicylidene) 2,3-diaminopyridine)] Pyridine, [Zn(C₁₉H₁₁Br₂N₃O₂)]C₅H₅N, have been obtained and characterized by elemental analysis, FT-IR, UV–Vis, ¹H NMR spectroscopy and MALDI-TOF mass spectrometry. The structure has been determined by single crystal X-ray crystallography. The complex crystallizes in the triclinic space group P-1 with two molecules in the asymmetric unit and with unit cell dimensions a = 8.0103(3) ?, b = 12.8340(5) ?, c = 22.3682(11) ?, α = 91.715(2)°, β = 93.918(2)°, γ = 103.708(2)°. V = 2226.30(16) ?³, Z = 4, R ₁ = 0.0780 and wR ₂ = 0.1192. X-ray structure determination revealed that the complex consists of a [Zn(C₁₉H₁₁Br₂N₃O₂)] moiety with a coordinated pyridine molecule on the metallic centre. The zinc atom adopts a distorted square pyramidal geometry as it is shown in the crystal structure.     

A New Lanthanide Coordination Polymer with 4,4′-Oxybis (Benzoic Acid) Ligand: Hydrothermal Synthesis, Crystal Structure and Photoluminescence

Abstract  

Self-assemblies of the organic ligand 4,4′-oxybis(benzoic acid) with metal salt (Eu³⁺) have led to one new complex, namely, Eu(oba)₂(phen) (1) (oba = 4,4′-oxybis (benzoic acid), phen = 1,10-phenanthroline). The structure was determined by single crystal X-ray crystallography and further characterized by elemental analysis and IR spectra. X-ray diffraction analysis reveals that it crystallizes in the monoclinic C2/c space group with a = 13.4943(12) ?, b = 19.3737(18) ?, c = 27.359(2) ?, β = 99.539°, V = 7053.7(1) ?³, Z = 8, μ = 1.862, F(000) = 3376. The Eu(III) ions along the a-axis are bridged by oba ligand into infinite oval-like one-dimensional chain. Interestingly, because of the existing of hydrogen bonging (O5–H5···O6), the title complex further formed a 2D layer structure with an interlayer separation of ca. 19.3737(18) ?. The complex exhibits excellent fluorescence property.     

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.     

The Coordination Behaviour of the Peroxodisulfate Anion with Group XII Metal Ions: [Zn(H2O)(C12H8N2)2(S2O8)]·H2O and Related Compounds

Abstract  

The title compound is monomeric with a Zn(II) hexacoordinated center. The coordination sphere is formed by four nitrogens from two phenanthroline molecules, one oxygen from a monodentate peroxodisulfate ion, and one oxygen from a water molecule. A non-coordinated water molecule completes the formula with an important role in the stabilization of the structure through the formation of two O_HW–H···O_pds bridges (acting as a donor) and one O_CW–H···O_HW bridge where it is an acceptor group (HW: hydration water; pds: peroxodisulfato; CW: coordinated water). The compound is triclinic, space group P-1 with a = 8.763 (3) ?, b = 9.068 (3) ?, c = 17.531 (6) ?, α = 96.48 (2)°, β = 103.94 (3)°, γ = 104.57 (3)°, V = 1286.0 (7) ?³ and Z = 2. The structure was solved by direct methods with a conventional R (on F) = 0.050 for 4534 reflections with Fo > 4σ(Fo). The compound is isomorphous with the Cd analogue (in Harvey et al. Aust J Chem 54:307, 2001). An eventual dependence of conformation and coordination mode of the peroxodisulfate anion on the ancillary organic ligand taking part in the coordination compounds analyzed is discussed.