Apinpus Rujiwatra

Microwave-assisted facile synthesis and crystal structure of cis-9,10,11,15-tetrahydro-9,10[3'4']-furanoanthracene-12,14-dione

Abstract A facile synthesis and crystal structure of cis‐9,10,11,15‐tetrahydro‐9,10[3′,4′]‐furanoanthracene‐12,14‐dione from the reaction of anthracene and maleic anhydride in xylene in a short time and high yield using a modified commercial domestic microwave oven is reported.

Bis(1,10-phenanthroline-κ2N,N′)(sulfato-κO)copper(II) ethanol monosolvate

The crystal structure of the title compound, [Cu(SO4)(C12H8N2)2]·C2H5OH, arises from the assembly of the neutral complex [Cu(SO4)(C12H8N2)2] and an ethanol solvent molecule. The CuII ion is five-coordinate, surrounded by two pairs of N atoms from two independent N,N′-chelating 1,10-phenanthroline ligands, and one O atom of monodentate sulfate ligand, in a distorted trigonal-bipyramidal fashion. Spatial orientation of the ligands and the assembly in the solid state are stabilized by the C—H⋯O hydrogen-bonding interactions, established between the O atoms (from the sulfate ligand and the ethanol molecule) and the neighbouring 1,10-phenanthroline molecules. There is also an offset face-to-face π–π stacking between the 1,10-phenanthroline ligands. The ethanol solvent molecule is disordered over two orientations in the ratio 0.663 (10):0.337 (10). The crystal examined was subject to racemic twinning and the refined twin fraction was 0.346 (19).

Lanthanide Coordination Polymers of Mixed Phthalate/Adipate for Ratiometric Temperature Sensing in the Upper-Intermediate Temperature Range

Based on the mixed phthalate (phth2-) and adipate (ad2-), [Nd2(ad)(phth)2(H2O)4] (I) and [Ln(ad)0.5(phth)(H2O)2] (Ln = EuIII (II), GdIII (III), TbIII (IV), DyIII (V), ErIII (VI), TmIII (VII), 1EuIII:10TbIII (VIII), 3EuIII:10TbIII (IX), and 5EuIII:10TbIII (X)) were synthesized and characterized. Complexes VIII-X show excellent ratiometric temperature sensing behavior in physiological and higher temperature ranges (303-423 K) rendered by the TbIII-to-EuIII energy transfer process. The efficiency of the process as illustrated through the lifetime measurements depends on both the EuIII:TbIII mole ratio and the temperature. The performance of X in terms of relative sensitivity ( Sr), temperature resolution, and measurement repeatability were determined, revealing the maximum Sr ( Sm) of 1.21%·K-1 at 303 K with reliable temperature resolution and excellent repeatability.

A New 1D Coordination Polymer of Lanthanum-Sulfate-1,10-Phenanthroline: Synthesis, Structure, and Photoluminescence Property

A 1D coordination framework, {[La2(o-phen)2(SO4)3(H2O)2]}n (1) (o-phen = 1,10-phenanthroline) was hydrothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, IR, and UV-Vis spectroscopy. The crystal of 1 crystallized in the triclinic P,1. space group, a = 10.3228(5) Å, b = 12.3644(7) Å, c = 12.6579(6) Å, α = 72.323(2)°, β = 75.610(2)°, γ = 82.785(2)°, V = 1488.82(13) Å3, Z = 2. The structure exhibits a neutral 1D framework representing a five-connected uninodal 1-periodic net of (3,6)(0,2) topology. The framework structure comprises TPRS-9 {LaO7N2} units, chelating o-phen ligands and bridging sulfates of 3.1110 and 4.2211 coordination modes. These 1D chains are extended into a 3D supramolecular structure by hydrogen bonding interactions of, R22 (n) patterns. Thermogravimetric analysis shows the structure to be thermally stable up to approximately 400°C. Photoluminescence investigations on Eu3+ and Tb3+ doped samples suggest the competition between the ligand-to-metal charge-transfer and energy-transfer processes.

Tris(ethyl­enediamine)cobalt(II) sulfate

The structure of the title compound, [CoII(C2H8N2)3]SO4, the cobalt example of [M(C2H8N2)3]SO4, is reported. The Co and S atoms are located at the 2d and 2c Wyckoff sites (point symmetry 32), respectively. The Co atom is coordinated by six N atoms of three chelating ethylenediamine molecules generated from half of the ethylenediamine molecule in the asymmetric unit. The O atoms of the sulfate anion are disordered mostly over two crystallographic sites. The third disorder site of O (site symmetry 3) has a site occupancy approaching zero. The H atoms of the ethylenediamine molecules interact with the sulfate anions via intermolecular N—H⋯O hydrogen-bonding interactions.

Influence of secondary ligand on structures and topologies of lanthanide coordination polymers with 1,3,5-triazine-2,4,6-triamine hexaacetic acid

A series of new lanthanide coordination polymers has been synthesized and structurally characterized; [Ln4(TTHA)2(pzac)(H3O)2(H2O)]·5H2O (Ln = Pr (1a) and Nd (1b)), [Sm8(TTHA)4(pzac)0.5(H3O)(H2O)7.5]·4H2O (2), [Ln4(HTTHA)2(SO4)(H2O)4]·5H2O (Ln = Pr (3a) and Nd (3b)), where H6TTHA = 1,3,5-triazine-2,4,6-triamine hexaacetic acid, and H2pzac = 2,5-dioxo-piperazine-1,4-diacetic acid. The compounds feature 3-D frameworks comprising the deprotonated H6TTHA as the primary ligand and either the in situ generated pzac2− or sulfate as the secondary ligands. The influence of the deprotonated H6TTHA in directing the framework structures through preferential coordination modes and molecular conformation is described. The effect of the secondary ligands in increasing the compactness of the frameworks and in the alternation of the framework topologies based on the four-connected pts type is described. Graphical abstract

Unsaturated Mn(II)-Centered [Mn(BDC)]n Metal–Organic Framework with Strong Water Binding Ability and Its Potential for Dehydration of an Ethanol/Water Mixture

An unsaturated Mn(II)-centered metal-organic framework was synthesized. The presence of an unsaturated Mn(II) center, together with a guest-responsive structural changing feature, plays a crucial role for strong binding with water, leading to its potential application for water/ethanol separation. In addition, the present framework is thermally stable up to 400 °C, which is beneficial for the regeneration process after adsorption.

catena-Poly[[bis­(pyridine-κN)zinc]-μ-5-carb­oxy­benzene-1,3-di­carboxyl­ato-κ2O1:O3]

The title one-dimensional coordination polymer, [Zn(C9H4O6)(C5H5N)2]n or [Zn(HBTC)(py)2]n, (I), where BTC is benzene-1,3,5-tricarboxylate and py is pyridine, is a solvent-free polymorph of [Zn(HBTC)(py)2]·2C2H5OH [Yaghi et al. (1997 ▶). Chem. Mater. 9, 1074–1076]. Differences in the spatial arrangements and supramolecular packing of the [Zn(HBTC)(py)2]n chains in the two structures are described. The chain in (I) extends parallel to [100] and is severely puckered, with a Zn⋯Zn distance of 8.3599 (3) Å and a Zn⋯Zn⋯Zn angle of 107.516 (3)°, as a result of hydrogen-bonding interactions of the types O—H⋯O and C—H⋯O. There is no evidence for π–π interactions in (I). The differences between the solvent-free and solvent-containing structures can be accounted for by the absence of the ethanol solvent molecule and the use of the converging pair of O atoms in the bis-monodentate bridging HBTC2− ligand in (I).

μ3-Methoxido-κ3O:O:O-tris­(μ-l-p-tyrosinato-κ3N,O:O)tris­(l-p-tyrosinato-κ2N,O)trinickel(II,III) methanol tetra­solvate

A trinuclear nickel complex, [Ni3(C9H10NO3)6(CH3O)]·4CH4O, was synthesized and characterized as a neutral cluster containing the incomplete cubane {Ni3(μ1-O)(μ2-O)2(μ3-O)} core of 2M3–1 topology. The three nickel cations show similar octahedral coordination, {Ni(μ1-O)(μ2-O)2(μ3-O)(μ1-N)2}; the positive charge is balanced by six tyrosinate ligands and one methoxide ion. The mean oxidation state of each NiII ion is therefore +2.33. The common coordination modes, chelating (via the amino N and the carboxylate O atoms) and bridging (via the carboxylate O atom), are exhibited by the tyrosinates. Three interligand (intracluster) N—H⋯O hydrogen-bonding interactions stabilize the incomplete cubane-type moiety. Additional N—H⋯O, O—H⋯O and C—H⋯O interactions are formed between clusters, and between the clusters and methanol molecules to regulate the spatial orientation of the tyrosinate and the assembly of the clusters in the crystal. The approximate equilateral triangular arrangement of the three nickel cations in the incomplete cubane-type moiety suggests the possible magnetic frustration, and the proximity of these metal cations indicates weak metallic bonds. The structure contains approximately 39% solvent-accessible volume between the clusters. This is filled with 17 molecules of disordered methanol and was modelled with SQUEEZE [Spek (2009 ▶). Acta Cryst. D65, 148–155]; the reported unit-cell characteristics do not take these molecules into account. The H atoms of the solvent molecules have not been included in the crystal data.

(1-Butyl-1,4-diaza­bicyclo­[2.2.2]octon-1-ium-κN4)trichloridocobalt(II)

The title compound, [Co(C10H21N2)Cl3], was obtained as the by-product of the attempted synthesis of a cobalt sulfate framework using 1,4-diazabicyclo[2.2.2]octane as an organic template. The asymmetric unit comprises two distinct molecules, and in each, the cobalt(II) ions are tetrahedrally coordinated by three chloride anions and one 1-butyldiazabicyclo[2.2.2]octan-1-ium cation. The organic ligands are generated in situ, and exhibit two forms differentiated by the eclipsed and staggered conformations of the butyl groups. These molecules interact by way of C—H⋯Cl hydrogen bonds, forming a three-dimensional hydrogen-bonding array.