Synthesis,crystal structure,and catalytic performance of two 3-D supramolecular compounds: (C7N2H7)3(C7N2H6) · PMo12O40 · 2H2O and (C7N2H7)3(C7N2H6)2 · AsMo12O40 · 3H2O

Two organic–inorganic compounds based on Keggin building blocks have been synthesized by hydrothermal methods, (C₇N₂H₇)₃(C₇N₂H₆)?·?PMo₁₂O_40?·?2H₂O (1) and (C₇N₂H₇)₃(C₇N₂H₆)_2?·?AsMo₁₂O_40?·?3H₂O (2) (C₇N₂H₆?=?benzimidazole). Single-crystal X-ray analysis revealed that 1 crystallized in the triclinic system, P-1 space group with a?=?9.8980(4)?Å, b?=?11.2893(4)?Å, c?=?25.8933(9)?Å, α?=?93.307(2)°, β?=?90.630(2)°, γ?=?108.330(2)°, V?=?2740.68(18)?ų, Z?=?2, R ₁(F)?=?0.0740, ωR ₂(F ²)?=?0.1511, and S?=?1.037; 2 crystallized in the triclinic system, P-1 space group with a?=?12.3353(4)?Å, b?=?13.2649(4)?Å, c?=?20.2878(6)?Å, α?=?95.6630(10)°, β?=?100.1720(10)°, γ?=?99.3940(10)°, V?=?3195.72(17)?ų, Z?=?2, R ₁(F)?= 0.0329, ωR₂ (F ²)?=?0.1236, and S?=?1.088. The two compounds show a layer framework constructed from Keggin-polyoxoanion clusters and benzimidazole via hydrogen bonds and π–π stacking interactions, resulting in a 3-D supramolecular network. Both have high catalytic activity for oxidation of methanol. When the initial concentration of the methanol is 5.37?g?m^?3 in air and the flow velocity is 4.51?mL?min^?1, methanol is completely eliminated at 150°C for 1 (160°C for 2).     

Two binuclear complexes containing the enrofloxacinate anion: Cd2(C19H21N3O3F)4(H2O)2 · 4H2O and Pb2(C19H21N3O3F)4 · 4H2O

The syntheses and crystal structures of the closely related but non-isostructural Cd₂(C₁₉H₂₁N₃O₃F)₄(H₂O)₂?·?4H₂O (1) and Pb₂(C₁₉H₂₁N₃O₃F)₄?·?4H₂O (2) are described, where C₁₉H₂₁N₃O₃F^? is enrofloxacinate (enro). Both compounds contain centrosymmetric, binuclear, neutral complexes incorporating a central diamond-shaped M₂O₂ (M?=?Cd, Pb) structural unit. The Cd²⁺ coordination polyhedron in 1 is a CdO₆ trigonal prism, including one coordinated water. The Pb²⁺ coordination polyhedron in 2 can be described as a very distorted square-based PbO₅ pyramid, although two additional short Pb?···?O (<3.1?Å) contacts are also present. In the crystal of the cadmium complex, O–H?···?O hydrogen bonds lead to a layered structure. In the lead compound, O–H?···?O and O–H?···?N interactions lead to chains in the crystal. Crystal data: 1: C₇₆H₉₆Cd₂F₄N₁₂O₁₈, M _r?=?1766.45, triclinic, P 1, a?=?12.185(2)?Å, b?=?12.306(3)?Å, c?=?14.826(3)?Å, α?=?68.15(3)°, β?=?70.28(3)°, γ?=?86.11(3)°, V?=?1938.2(7)?ų, Z?=?1, T?=?298 K, R(F)?=?0.030, wR(F ²)?=?0.079. 2: C₇₆H₈₈F₄N₁₂O₁₆Pb₂, M _r?=?1920.00, triclinic, P 1, a?=?12.0283(4)?Å, b?=?12.7465(4)?Å, c?=?13.0585(4)?Å, α?=?83.751(1)°, β?=?74.635(1)°, γ?=?81.502(1)°, V?=?1904.3(1)?ų, Z?=?1, T?=?298?K, R(F)?=?0.021, wR(F ²)?=?0.049.     

Syntheses and structural determinations of the nine-coordinate rare earth metal: Na4[DyIII(dtpa)(H2O)]2·16H2O,Na[DyIII(edta)(H2O)3]·3.25H2O and Na3[DyIII(nta)2(H2O)]·5.5H2O

Three complexes, Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O, Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O and Na₃[Dy^III (nta)₂(H₂O)]?·?5.5H₂O, have been synthesized in aqueous solution and characterized by FT–IR, elemental analyses, TG–DTA and single-crystal X-ray diffraction. Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O crystallizes in the monoclinic system with P2₁/n space group, a?=?18.158(10)?Å, b?=?14.968(9)?Å, c?=?20.769(12)?Å, β?=?108.552(9)°, V?=?5351(5)?ų, Z?=?4, M?=?1517.87?g?mol^?1, D _c?=?1.879?g?cm^?3, μ?=?2.914?mm^?1, F(000)?=?3032, and its structure is refined to R ₁(F)?=?0.0500 for 9384 observed reflections [I?>?2σ(I)]. Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O crystallizes in the orthorhombic system with Fdd2 space group, a?=?19.338(7)?Å, b?=?35.378(13)?Å, c?=?12.137(5)?Å, β?=?90°, V?=?8303(5)?ų, Z?=?16, M?=?586.31?g?mol^?1, D _c?=?1.876?g?cm^?3, μ?=?3.690?mm^?1, F(000)?=?4632, and its structure is refined to R ₁(F)?=?0.0307 for 4027 observed reflections [I?>?2σ(I)]. Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O crystallizes in the orthorhombic system with Pccn space group, a?=?15.964(12)?Å, b?=?19.665(15)?Å, c?=?14.552(11)?Å, β?=?90°, V?=?4568(6)?ų, Z?=?8, M?=?724.81?g?mol^?1, D _c?=?2.102?g?cm^?3, μ?=?3.422?mm^?1, F(000)?=?2848, and its structure is refined to R ₁(F)?=?0.0449 for 4033 observed reflections [I?>?2?σ(I)]. The coordination polyhedra are tricapped trigonal prism for Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O and Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O, but monocapped square antiprism for Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O. The crystal structures of these three complexes are completely different from one another. The three-dimensional geometries of three polymers are 3-D layer-shaped structure for Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O, 1-D zigzag type structure for Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O and a 2-D parallelogram for Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O. According to thermal analyses, the collapsing temperatures are 356°C for Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O, 371°C for Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O and 387°C for Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O, which indicates that their crystal structures are very stable.     

Solid state structures of the chiral heterobimetallic complexes [Cu(dach)2][Pt(CN)4] · 2H2O, [Ni(dach)3][Pt(CN)4] · 2DMF · H2O,and [Pd(dach)2][Pt(CN)4] · H2O (dach = 1 R , 2 R -diaminocyclohexane)

The chiral dinuclear heterometallic complexes [Cu(dach)₂][Pt(CN)₄]?·?2H₂O (1), [Ni(dach)₃][Pt(CN)₄]?·?2DMF?·?H₂O (2), and [Pd(dach)₄][Pt(CN)₄]?·?H₂O (3) (dach?=?1R,2R-cyclohexanediamine) have been prepared and characterized by X-ray diffraction analysis. Crystal data: 1, monoclinic, P2₁, a?=?8.108(3), b?=?15.552(6), c?=?9.914(4)?Å, β?=?110.931(6)°, V?=?1167.6(8)?ų, Z?=?2, R ₁?=?0.0420, wR ₂?=?0.1122; 2, monoclinic, P2₁, a?=?13.264(11), b?=?9.285(7), c?=?16.211(13)?Å, β?=?111.640(9)°, V?=?1856(3)?ų, Z?=?2, R ₁?=?0.0276, wR ₂?=?0.0698; 3, monoclinic, P2₁, a?=?6.887(2), b?=?12.809(4), c?=?12.975(4)?Å, β?=?94.865(4)°, V?=?1140.6(6)?ų, Z?=?2, R ₁?=?0.057, wR ₂?=?0.156. In complex 1, the Pt and Cu atoms are linked by a CN bridge that presents a very bent C=N–Cu angle [136.8(8)°].     

Effects on Coordination of Thioether Sites. 4. Structural Analysis of η3-Tripodal Ligand Manganese(I) Complexes

Crystal structures of a series of manganese(I) complexes containing tripodal ligands were determined. For [η³-{CH₃C(CH₂PPh₂)₂(CH₂SPh)-P,P′,S}Mn(CO)₃]PF₆ ( 1 ): a = 10.856(3) Å, b = 19.698(3) Å, c = 17.596(5) Å, β = 96.17(2)°, monoclinic, Z = 4, P2₁/c, R(F_o) = 0.068, R_w(F_o) = 0.055 for 3617 reflections with I_o > 2σ(I_o). For [η³-{CH₃C(CH₂PPh₂)(CH₂SPh)₂-P,P′,S}Mn(CO)₃]PF₆ ( 2 ): a = 9.890(2) Å, b = 20.403(4) Å, c = 10.269(3) Å, β = 117.44(2)°, monoclinic, Z = 2, P2_l, R(F_o) = 0.050, R_w(F_o) = 0.037 for 1760 reflections with I_o > 2σ(I_o). For [η³-{CH₃C(CH₂PPh₂)₂(CH₂S)-P,P′,S}Mn(CO)₃] ( 4 ): a = 8.191(7) Å, b = 10.495(3) Å, c = 19.858(6) Å, α = 99.61(2)°, β = 96.17(2)°, γ = 92.70(4)°, triclinic, Z = 2, P-I, R(F_o) = 0.048, R_w(F_o) = 0.039 for 2973 reflections with I_o > 2σ(I_o). There is no significant difference in the bond lengths of Mn-S bonds among three species in their crystal structures [2.325(2) Å in 1; 2.358(4) in 2; 2.380(2) in 4], but the better donating ability of thiolate in complex 4 appears on the lower frequencies of its carbonyl stretching absorptions.     

Synthesis and structures of two cobalt complexes [NaCoII(NTA)(H2O)] n and NH4[CoIII(IDA)2] · 2H2O

Two cobalt complexes [NaCo^II(nta)(H₂O)] _n (H₃nta?=?nitrilotriacetic acid) (1) and NH₄[Co^III(ida)₂]?·?2H₂O (H₂ida?=?iminodiacetic acid) (2) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the orthorhombic system, space group P2₁2₁2₁ with a?=?7.9770(12)?Å, b?=?9.7613(15)?Å, c?=?12.1945(18)?Å, V?=?949.5(2)?ų, Z?=?4, and R ₁?=?0.0705 for 1597 observed reflections. Compound 2 crystallizes in the monoclinic system, space group P2(1)/c with a?=?5.1801(3)?Å, b?=?11.2073(6)?Å, c?=?12.2891(7)?Å, V?=?707.09(7)?ų, Z?=?2, and R ₁?=?0.0349 for 1143 observed reflections. In compound 1, the Co is coordinated by a nitrogen and five oxygen atoms in a distorted octahedral geometry {CoNO₅}, and the Na is coordinated by one water molecule and four carboxyl oxygen atoms in slightly distorted square pyramidal geometry. The entire structure shows a three-dimensional network. In compound 2, Co atom is equatorially coordinated by two ida ligands in a distorted octahedral geometry {CoN₂O₄}. The discrete [Co(ida)₂]^2? anions are linked by hydrogen bonding to a three-dimensional supramolecular network.     

Synthesis and structures of three triphosphonate compounds containing d10 transition metal ions

Three new triphosphonate compounds, [Zn(APTPH₄)(2,2′-bipy)(H₂O)]?·?2H₂O (1), [Cd(APTPH₄)(2,2′-bipy)(H₂O)]?·?2H₂O (2), and [Zn(APTPH₄)(phen)₂]?·?phen?·?4H₂O (3) (APTPH₆?=?1-aminopropane-1,1,3-triphosphonic acid, 2,2′-bipy?=?2,2′-bipyridine, phen?=?1,10-phenanthroline), are synthesized by a low-temperature hydrothermal method. Compounds 1 and 2 are isomorphous, both one-dimensional (1D) coordination polymers expanded into three-dimensional (3D) supramolecular structures by hydrogen bonds and π–π stacking interactions. Compound 3 is a molecular complex and forms a 3D network through an S-shaped water hexamer. Crystal data for 1: Triclinic, space group P 1, a?=?6.6814(5)?Å, b?=?10.0929(7)?Å, c?=?15.438(2)?Å, α?=?81.544(2)°, β?=?79.066(2)°, γ?=?82.278(2)°, Z?=?2; for 2: Triclinic, space group P 1, a?=?6.9380(8)?Å, b?= 10.043(2)?Å, c?=?15.681(2)?Å, α?=?81.357(2)°, β?=?78.510(2)°, γ?=?81.902(2)°, Z?=?2; Crystal data for 3: Triclinic, space group P 1, a?=?12.540(2)?Å, b?=?12.596(2)?Å, c?=?14.997(2)?Å, α?=?100.795(2)°, β?=?113.328(2)°, γ?=?101.358(2)°, Z?=?2.     

An open-framework cobalt molybdate possessing {Mo2O7} building block: hydrothermal synthesis and structural characterization of [CoMo2O7(4,4′-bipy)1.5]

The hydrothermal reaction of Co(COO)₂?·?4H₂O, MoO₃, H₃PO₄ and 4,4′-bipyridine yields bipyridine-ligated cobalt dimolybdate [CoMo₂O₇(4,4′-bipy)_1.5] (1) (4,4′-bipy?=?4,4′-bipyridine) in the triclinic system with space group of P 1 and cell parameters of a?=?7.1951(8)?Å, b?=?11.1708(17)?Å, c?=?11.4514(11)?Å, α?=?98.545(7)°, β?=?90.315(2)°, γ?=?105.777(5)°, V?=?874.88(19)?ų, and Z?=?2. Its structure consists of Co/Mo/O bimetal oxide layers with {Mo₂O₇} building blocks, linked by the coordination of 4,4′-bipy ligand with Co and Mo atoms, into a 3D porous hybrid framework.     

Synthesis and structural determination of the first eight-coordinate rare earth metal complex with a six-member ring, (NH4)[EuIII(pdta)(H2O)] · H2O

(NH₄)[Eu^III(pdta)(H₂O)]?·?H₂O has been synthesized and characterized by infrared spectrum, fluorescence spectrum, elemental analyses and single-crystal X-ray diffraction techniques. It crystallizes in the monoclinic system with space group P2₁/n, a?=?12.7700(15)?Å, b?=?9.3885(11)?Å, c?=?14.4070(18)?Å, α?=?90°, β?=?95.950(2)°, γ?=?90°, V?=?1718.0(4)?ų, Z?=?4, M?=?508.28, D _c?=?1.965?g?cm^?3, μ?=?3.708?mm^?1, F(000)?=?1108. The structure was refined to R ₁?=?0.0238 for 3469 observed reflections (I?>?2σ(I)). The Eu^IIIN₂O₆ part in the [Eu^III(pdta)(H₂O)]^? complex anion has an eight-coordinate structure with a distorted square anti-prismatic conformation, in which six coordination positions, two nitrogen atoms and four oxygen atoms are from one pdta (=propylenediaminetetraacetic acid) ligand, the seventh position is an oxygen (O(8A)) from another pdta and the eighth coordination site is occupied by a water molecule. (NH₄)[Eu^III(pdta)(H₂O)]?·?H₂O is the first eight-coordinate complex with a six-member ring in the rare earth metal complexes with aminopolycarboxylic acid ligands.     

Bis(2-Amino-5-bromopyrimidinium) Tetrahalometallates: Crystal structures of (2-amino-5-bromopyrimidinium)2 MCl4 (M = Co,Zn)

The reactions of metal(II) chlorides and bromides with 2-amino-5-bromopyrimidine (2-abpm) in neutral and acidic solution were investigated. The reaction with ZnCl₂, ZnBr₂, CoCl₂, CoBr₂ and MnCl₂ in acidic nitromethane solution gave complexes of the formula (2-abpmH)₂MX₄ (1, M?=?Zn, X?=?Cl; 2, M?=?Zn, X?=?Br; 3, M?=?Co, X?=?Cl; 4, M?=?Co, X?=?Br; 5, M?=?Mn, X?=?Cl). Crystals of 1 and 3 suitable for single crystal X-ray diffraction were obtained. Crystal data: For (1): triclinic, P-1, a?=?6.2485(13), b?=?9.0520(14), c?=?15.334(4)?Å, α?=?94.81(2), β?=?95.224(17), γ?=?98.027(17)°, V?=?851.1(3)?ų, Z?=?2, R?=?0.0596 for [|I|?≥?2σ(I)]. For (3): triclinic, P-1, a?=?6.2438(13), b?=?9.0597(15), c?=?15.318(3)?Å, α?=?94.749(18), β?=?95.343(15), γ?=?98.021(17)°, V?=?850.2(3)?ų, Z?=?2, R?=?0.0452 for [|I|?≥?2σ(I) ]. Variable temperature magnetic susceptibility data indicates weak antiferromagnetic interactions in the cobalt and manganese complexes.     

Hydrothermal synthesis,characterization, and luminescence of two new arsenic–vanadium compounds with a γ-[As8V14O42(H2O)]4− anion

Two new compounds, [Zn(phen)₃]₂[γ-As₈V₁₄O₄₂(H₂O)]?·?4H₂O (1) and [Cd(phen)₃]₂[γ-As₈V₁₄O₄₂(H₂O)]?·?2H₂O (2) (phen?=?1,10′-phenanthroline), have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, infrared spectrum, and thermogravimetric analysis. Compound 1 crystallizes in the triclinic space group P 1 with a?=?11.429(4)?Å, b?=?15.760(5)?Å, c?=?15.952(5)?Å, α?=?108.825(5)°, β?=?92.194(5)°, γ?=?104.155(5)°, V?=?2615.6(15)?ų, Z?=?1; 2 crystallizes in the triclinic space group P 1 with a?=?11.450(4)?Å, b?=?15.629(6)?Å, c?=?16.302(6)?Å, α?=?109.177(5)°, β?=?92.628(5)°, γ?=?104.251(4)°, V?=?2644.8(17)?ų, Z?=?1. Single-crystal structural analysis shows that both 1 and 2 consist of a new type of [γ-As₈V₁₄O₄₂(H₂O)]^4? cluster anion.     

A dimeric luminescent lanthanide complex [Eu(PAA)2(phen)(NO3)]2: hydrothermal synthesis,crystal structure and fluorescence

A lanthanide coordination complex [Eu(PAA)₂(phen)(NO₃)]₂ (PAA?=?phenylacetic acid, phen?=?1,10-phenanthroline) has been synthesized by the hydrothermal method. Single crystal X-ray diffractions show that it forms a dimeric molecular structure. The title complex crystallizes in the triclinic system, space group P 1, with lattice parameters a?=?8.9473(8)?Å, b?=?13.3659(12)?Å, c?=?13.4745(12)?Å, α?=?60.7590(10)°, β?=?89.5100(10)°, γ?=?71.9850(10)°, V?=?1317.3(2)?ų, D _c?= 1.675?Mg?m^?3, Z?=?1, F(000)?=?660, GOF?=?1.003, R ₁?=?0.0206, wR ₂?=?0.0575. The fluorescence excitation and emission spectra have been investigated.     

Synthesis and crystal structure of a Cu(II) complex with mixed malonate/1,10-phenanthroline ligands

A Cu(II) complex with mixed ligands, [Cu₃(mal)₃(phen)₃(H₂O)₂]?·?11H₂O (mal?=?malonate, phen?=?1,10-phenanthroline) was synthesized and characterized by elemental analysis, IR, UV, electron paramagnetic resonance (EPR) and luminescence spectra and single-crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group Cc with a?=?13.1631(10)?Å, b?=?20.1089(10)?Å, c?=?20.1267(13)?Å, β?=?103.500(3)°, V?=?5180.2(6)?ų, Z?=?4, and R ₁?=?0.0476 for 7993 observed reflections. In the complex, one Cu is coordinated by a mal dianion and a phen molecule, exhibiting N₂O₂ square-planar geometry, while the other two Cu atoms are coordinated, respectively, by a mal dianion, a phen and water molecules, exhibiting N₂O₃ square pyramidal coordination geometry.     

Syntheses,crystal structures,and antimicrobial activities of nickel(II) and cadmium(II) complexes with 4-methylsulfonyl cinnamate and diamines

Two metal complexes, [Ni^II(mscinn)₂(pda)₂] (1) and [Cd^II(mscinn)₂(dmeda)₂·2H₂O] (2) (mscinn?=?4-methylsulfonyl cinnamate, pda?=?propane-1,3-diamine, dmeda?=?N′,N′-dimethylethane-1,2-diamine), were synthesized by reacting 4-methylsulfonyl cinnamate with the diamines and metal salts. Their structures were determined by single-crystal X-ray diffraction analysis. Crystal parameters of 1: C₂₆H₃₈N₄NiO₈S₂, M?=?657.43, monoclinic, P2₁/c, a?=?16.6123(8)?Å, b?=?8.5956(4)?Å, c?=?11.2047(5)?Å, β?=?107.423(1)°, V?=?1526.54(12)?ų, Z?=?2, D _calcd?=?1.430?g?cm^?3, F(000)?=?692, μ?=?0.825?mm^?1, R ₁?=?0.0257, wR ₂?=?0.0669. Crystal data of 2: C₂₈H₄₂CdN₄O₈S_2?·?2(H₂O), M?=?775.24, monoclinic, P2₁/c, a?=?9.8278(4)?Å, b?=?11.6611(5)?Å, c?=?15.3972(7)?Å, β?=?96.195(1)°, V?=?1754.26(13)?ų, Z?=?2, D _calcd?=?1.468?g?cm^?3, F(000)?=?804, μ?=?0.798?mm^?1, R ₁?=?0.0299, wR ₂?=?0.0770. Antimicrobial activities for 1 and 2 against Escherichia coli, Pseudomonas putida, Bacillus subtilis, and Bacillus cereus had better antibacterial activity than their parent carboxylic acid against Gram-positive bacteria (B. subtilis and B. cereus). The cadmium complex of the cinnamate displayed high inhibitory activity with an MIC value of 5?µg?mL^?1 against P. putida, while the nickel complex also exhibited good inhibitory potency with an MIC value of 5?µg?mL^?1 against B. subtilis.     

A novel Anderson-type polyoxometalate: hydrothermal synthesis,crystal structure,and catalytic performance of (H3O)[(3-C5H7N2)2(Cr(OH)6Mo6O18)] · 3H2O

A new Anderson polyoxometalate (H₃O)[(3-C₅H₇N₂)₂(Cr(OH)₆Mo₆O₁₈)]?·?3H₂O (3-C₅H₆N₂?=?3-aminopyridine) was hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Crystal data: triclinic, P 1, a?=?7.8482(8)?Å, b?=?10.1800(10)?Å, c?=?10.4103(10)?Å, α?=?88.031(3)°, β?=?78.308(2)°, γ?=?88.842(3)°, V?=?813.91?ų, Z?=?1, R(F)?=?0.0397, wR _ref(F ²)?=?0.1022, and S?=?1.076. The X-ray crystallographic study showed that the structure contains Anderson-type [Cr(OH)₆Mo₆O₁₈]^3? polyoxoanions. The title compound has high catalytic activity for the oxidation of acetone tested in a continuous-flow fixed-bed micro-reactor. When the initial concentration is 18.3?g?m^?3 in air and the flow velocity is 8.5?mL?min^?1, the acetone is completely eliminated at 160°C.     

Hydrothermal synthesis,structures and characterization of two new copper(II) triphosphonate compounds

Two copper(II) triphosphonate compounds, Cu[(APTPH₄)(phen)(H₂O)]?·?2.16H₂O (1) and [Cu(APTPH₄)(2,2′-bipy)(H₂O)]?·?2.63H₂O (2), have been prepared by a low temperature hydrothermal reaction from 1-aminopropane-1,1,3-triphosphonic acid (APTPH₆), CuO and a second ligand, phen?=?1,10-phenanthroline, or 2,2′-bipy?=?2,2′-bipyridyl. These two compounds were characterized by single crystal X-ray diffraction, elemental analysis, IR and TG. Crystal data for 1: Monoclinic, space group P2₁ /c, a?=?14.4830(7)?Å, b?=?9.1721(5)?Å, c?=?16.7403(8)?Å, β?=?90.101(2)°. For compound 2: Triclinic, space group P 1, a?=?7.1215(7)?Å, b?=?10.460(2)?Å, c?=?14.671(2)?Å, α?=?82.983(2)°, β?=?83.882(2)°, γ?=?80.617(2)°. In both compounds, each Cu²⁺ ion is five-coordinate with two oxygen atoms from the triphosphonate, two nitrogen atoms from the second ligand and one water molecule, to form a distorted square-pyramidal geometry. Both complexes have 3D supramolecular structures constructed by hydrogen bonds and π–π stacking interactions.     

Synthesis,structure and characterization of copper(II) and zinc(II) complexes based on 3-carboxyl-1,2,4-triazole

Two complexes [CuL₂(H₂O)₂] (1) and [ZnL₂(H₂O)₂] (2) (L?=?3-carboxyl-1,2,4-triazole (L)) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group P ₂(1)/n, a?=?8.632(8)?Å, b?=?9.153(8)?Å, c?=?6.991(7)?Å, β?=?94.279(12)°, Z?=?2, R ₁?=?0.0296, wR ₂?=?0.0918. Compound 2 also crystallizes in the monoclinic space group P ₂(1)/n, a?=?4.937(3)?Å, b?=?18.107(10)?Å, c?=?6.344(4)?Å, β?=?106.839(7)°, Z?=?2, R ₁?=?0.0230, wR ₂?=?0.0556. Extensive intermolecular hydrogen bonds assemble 1 and 2 into three-dimensional (3D) supramolecular architectures, with eight-member H-bonded synthons. Compounds 1 and 2 were also characterized by element analysis, FT–IR, luminescence and EPR studies.     

Synthesis and crystal structure of a trinuclear titanium(IV) β -diketonate complex with a six-membered [Ti–(μ-O)]3 ring

The trinuclear titanium(IV) β-diketonate complex, [Ti₃(μ-O)₃(dppd)₆]?·?(DMF)(0.5EtOH) (1) (H-dppd?=?1,3-diphenylpropane-1,3-dione) has been synthesized and its crystal structure and spectroscopic properties have been studied. Complex 1 crystallizes in monoclinic system with space group C2/c and a?=?20.954(5)?Å, b?=?18.705(4)?Å, c?=?24.617(6)?Å, β?=?111.957(4)°, Z?=?4. The complex consists of a six-membered [Ti–(μ-O)]₃ ring, of which three titanium(IV) ions are linked together by bridging oxygen atoms. Each titanium(IV) possesses an octahedral geometry, with four oxygen atoms from the two β-diketonate ligands and two bridging oxygen atoms.     

Bidentate coordination of a diketo phosphorus ylide: synthesis and structure of [(C6H5)3PC(COCH3)(COC6H5)-κO,O′]UO2(NO3)2

A 1?:?1 chelate complex [(C₆H₅)₃PC(COCH₃)(COC₆H₅)-κO,O′]UO₂(NO₃)₂ has been synthesized by reaction of (C₆H₅)₃PC(COCH₃)(COC₆H₅) with UO₂(NO₃)₂?·?6H₂O in methanol at room temperature and characterized by elemental analysis, spectroscopy as well as by single-crystal X-ray diffraction. The complex crystallizes in P2₁/n space group with a?=?10.007(2)?Å, b?=?15.285(7)?Å, c?=?19.20(1)?Å, β?=?91.22(3)°, V?=?2936(2)?ų, Z?=?4, D _c?=?1.847?g?cm^?3. In the solid state structure, the dihedral angle [88.1(4)°] between the planes defined by the two quartets of atoms O1 O8 O2 O4 and O6 O5 O3 O7 is close to 90°, as expected for a triangulated dodecahedral geometry around uranium.