Search

Abstract: A series of new polyoxometalates based on [Ni6(μ3-OH)3(H2O)6(en)3(B-α-PW9O34)] (en=ethylenediamine) clusters capped by different tripodal alcohol ligands have been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray diffraction, respectively. The experimental results indicate that the tripodal alcohol ligands can substitute three hydroxyl groups located on the axial positions of the Ni6 cluster to form new polyoxometalates with different substituted modes. [Copyright &y& Elsevier]

Abstract: A novel hybrid borate B3O4(OH)·0.5(C4H10N2) 1 was synthesized under milder hydrothermal conditions. The product was characterized by a combination of elemental analysis, FT-IR, thermogravimetric analysis and powder X-ray diffraction, as well as single-crystal X-ray diffraction studies. The structure consists of two types of inorganic borate helices cohered by piperazine rings, giving rise to a neutral hybrid sheet. The adjacent layers are stacked in a parallel fashion and further stabilized by hydrogen bonding interactions. [Copyright &y& Elsevier]

Abstract: Two new arsenic–vanadium clusters, [Zn(2,2′-bpy)3]2[As8V14O42(H2O)]·4H2O (1, 2,2′-bpy =2,2′-bipyridine) and [Zn(2,2′-bpy)(dien)]2[As8V14O42(H2O)]·2H2O (2, dien=diethylenetriamine), have been hydrothermally synthesized and characterized by IR, elemental analysis, EPR, XRD, TGA, magnetic measurements, and single-crystal X-ray diffraction analysis. Crystal data: 1, triclinic,, a=14.3793(2)Å, b=16.7706(2)Å, c=24.7077(1)Å, α=93.740(1)°, β=93.182(1)°, γ=113.363(1)°, Z=2; 2 orthorhombic, P4(3)2(1)2, a=21.3442(7)Å, b=21.3442(7)Å, c=15.8837(7)Å, Z=4. X-ray crystallographic study showed that compound 1 is composed of the discrete [As8V14O42(H2O)]4- polyoxoanions and chiral [Zn(2,2′-bpy)3]2+ cations, while compound 2 is constructed from [As8V14O42(H2O)]4− cluster anions and novel [Zn(2,2′-bpy)(dien)]2+ complex fragments linked through hydrogen bonds into a network. Variable temperature susceptibility measurements demonstrate the presence of antiferromagnetic interaction between VIV cations in 1 and 2. [Copyright &y& Elsevier]

Abstract: Two new hybrid vanadium arsenates (2,2′-bpy)2(VVO2)2(AsO4)⋅H3O⋅H2O 1 and (2,2′-bpy)2V4O7(HAsO4)2 2 (2,2′-bpy=2,2′-bipyridine) were synthesized under hydrothermal reaction conditions and structurally characterized by single-crystal X-ray diffraction, thermogravimetric analysis (TGA), IR, powder XRD and elemental analyses. Crystal data for 1: monoclinic, , , , , , , . Crystal data for 2: triclinic, P-1, , , , , , , , . Compound 1 is composed of discrete {(VO2)2(AsO4)} 3-membered rings bonded to two 2,2′-bpy ligands. Compound 2 exhibits a 2D arsenic vanadate network decorated with 2,2′-bpy ligands. [Copyright &y& Elsevier]

Abstract: A new arsenic–vanadium clusters, [NH2(CH2CH2)2NH2]3[As8V14O42(SO4)]·6.5H2O (1), have been hydrothermally synthesized and characterized by IR, elemental analysis, TGA, magnetic property, and single crystal X-ray diffraction analysis. Crystal data: Monoclinic, P2(1)/n, a=21.963(2)Å, b=14.508(1)Å, c=23.054(3)Å, β=118.316(3)°, Z=4. X-ray crystallographic study showed that crystal 1 is composed of the discrete cluster anions [As8V14O42(SO4)]6-, organic amine molecules providing charge-compensation, space-filling, and structure-directing roles, and lattice water molecules occupying in the structure. The study of the magnetic susceptibility of 1 demonstrates the presence of antiferromagnetic interaction between VIV cations in 1. [Copyright &y& Elsevier]

A new inorganic–organic hybrid open-framework zinc phosphite, (C6N3H12)2·Zn5(HPO3)6, has been hydrothermally synthesized in the presence of 1-(3-aminopropyl)imidazole amine as a structure-directing agent. Its structure was determined by single-crystal X-ray diffraction and further characterized by powder X-ray diffraction (PXRD), IR spectroscopy, ICP, elemental, and TG analyses. This compound crystallizes in the orthorhombic system, space group C2221 (no. 20), a=9.9512(4), b=14.7129(6), c=22.50660(10) Å, V=3295.21(19) Å3, Z=4. The connectivity of the strictly alternating Zn-centered tetrahedra and HPO3 pseudopyramids results in a 3D framework with intersecting 8- and 12-membered ring channels, where organic amines reside. It is worth noting that the title compound is the first metal phosphite to be prepared with a metal: phosphorus ratio of 5:6. [Copyright &y& Elsevier]

Abstract: An unexpected 3D manganese vanadate (en)Mn2(V2O7) (1) (en=ethylenediamine) has been hydrothermally obtained by H2E2Ge2O3 (E=−CH2CH2COO−) ligands and well-prepared mixture of V–Mn-amine and characterized by IR spectroscopy, elemental analysis, thermal stability and powder X-ray diffraction. Single-crystal X-ray diffraction analysis reveals that the structure is a novel pillared-layer, in which MnO5N octahedra are corner-linked to form an infinite sheet with 4-membered rings (MRs) and further condensed to the 3D framework. The most prominent feature of 1 is the connection between the sheets via double bridges, namely, inorganic V2O7 dimeric units and organic en molecules. It is noteworthy that inorganic and organic double bridges between sheets have not been seen in manganese vanadates. [Copyright &y& Elsevier]

CaYGaO 4 was synthesized by conventional solid-state method. Its crystal structure was determined by single-crystal X-ray diffraction technique to be olivine structure type. CaYGaO 4 comprises an orthorhombic space group Pnma , with lattice constants of a = 11.3484(1) Å, b = 6.5712(6) Å and c = 5.2818(8) Å. All three cations occupy their specific atomic positions and the structure is fully ordered. The crystallographic ordering scheme in the new gallate system, is different from those reported for the previously studied silicate and germanate olivines. The partial replacement of the Ga 3+ by Fe 3+ ions could be achieved, resulting in a series of solid solutions with the chemical composition of CaYGa 1− x Fe x O 4 (0 < x ⩽ 0.50). The unit cell volumes of the doped variants are consistent with Vegard’s law. [ABSTRACT FROM AUTHOR]

Abstract: A novel di-copperII-complex substituted monovacant Keggin polyoxotungstate [Cu(2,2′-bpy)(H2O)][H2PW11O39Cu2(2,2′-bpy)2(H2O)(OH)]·1.5H2O (1) (2,2′-bpy=2,2′-bipyridine) with a 1D polymeric chain has been hydrothermally synthesized and structurally characterized. To our knowledge, 1 is the rare magnetic di-transition metal-complex substituted monovacant Keggin polyoxotungstate with a unique 1D dual-bridging chain structure. Its magnetic behavior has been quantitatively analyzed by the Bleaney–Bowers equation, indicating the presence of weak antiferromagnetic interactions within dinuclear CuII centers. [Copyright &y& Elsevier]

Abstract: Two new zinc phosphates, Zn6P8O26(OH)6[H3dien]2 (I) and Zn6P8O29(OH)3[H3dien]3 (II) (dien=diethylenetriamine), were solvothermally synthesized in the presence of a mixture of organic amines. Both two structures are built by the alternate linkages between ZnO4 and (H)PO4 tetrahedral moieties producing two intimately related (3,4)-connected framework structures with the 16-ring large channels. The successful synthesis of the two compounds illustrates that a specific “secondary” organic additive governs the resulting open-framework structures besides a “primary” organic amine plays a structure-directing role. Crystal data: triclinic, , a =8.5619(1), b =13.5037(2), c =16.9251(1)Å, α =69.545(1)°, β =89.573(1)°, γ =86.684(1)°, V =1830.21(4)Å3, Z =2 for I, and monoclinic, P21/c, a =31.9204(3), b =8.3759(2), c =15.7894(3)Å, β =97.062(1)°, V =4189.46(13)Å3, Z =4 for II. [Copyright &y& Elsevier]

Abstract: A new inorganic–organic hybrid solid, Cd(phen)(H2PO4)2⋅H2O (phen=1,10-phenanthroline), has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis, ICP analysis, powder X-ray diffraction and fluorescent spectrum. The compound crystallizes in the triclinic system, space group P-1 (No. 2), , , , , , , , . The structure is built from strictly alternating CdO4N2 octahedra and H2PO4 tetrahedra through their vertices, forming an infinite ladder-like architecture. This compound shows intense photoluminescence upon photoexcitation at 358 nm. [Copyright &y& Elsevier]

Two new open-framework germanates, [Cd2(C2N2H8)3][Ge9O18(OH)4] (1) and (C8N4H26)[Ge9O18(OH)4] (2), have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic space group, Pbca, with a=14.318(3), b=13.106(3), c=14.580(3) Å, V=2736.0(9) Å3, Z=4. The compound is the first organically templated cadmium germanate. The structure of 1 is constructed from two distinct motifs, a body-centered [Ge9O18(OH)4] cluster and a cadmium complex [Cd2(C2N2H8)3O6], which integrate to generate a 3D architecture with neutral framework. The structures of 2 is closely related to that of 1 and has identical Ge9O18(OH)4 clusters. It crystallizes in the orthorhombic space group, Pbca, with a=14.158(3), b=13.213(3), c=14.553(3) Å, V=2722.5(9) Å3, Z=4. The connectivity between the Ge9 clusters result in a 3D open-framework structure. The quadruply protonated N,N′-bis(3-aminopropyl)ethylene diamine molecules are located in the free voids and interact with the macroanionic inorganic framework by extensive hydrogen bonds. [Copyright &y& Elsevier]

A new layered inorganic–organic hybrid gallium phosphate, Ga2(phen)(HPO4)3 (phen=1,10-phenanthroline), has been hydrothermally synthesized and characterized by single crystal X-ray diffraction, FTIR, elemental analysis, ICP, power X-ray diffraction and thermogravimetric analysis. This compound crystallizes in the triclinic system, space group P-1 (No. 2), a=7.7730(6) Å, b=11.7968(10) Å, c=12.1458(9) Å, α=114.089(2)°, β=102.310(2)°, γ=102.905(2)°, V=931.28(13) Å3, Z=2. The structure is built from strictly alternating GaO4N2 octahedra, GaO4 tetrahedra and HPO4 tetrahedra through their vertices, forming a neutral layered architecture grafted with phen ligands. The adjacent sheets are stacked in an AAAA sequence along [0 0 1] direction and held together by strong π–π interactions. [Copyright &y& Elsevier]

Two organically templated zinc phosphites, (C2N2H10)Zn2(HPO3)3 (1) and (C4N2H12)Zn3(HPO3)4 (2), were hydrothermally synthesized and structurally characterized. Compound 1 crystallized in the triclinic system, space group P-1 (No. 2), a=8.6357(14) A˚, b=8.8197(14) A˚, c=9.9665(16) A˚, α=64.645(2), β=65.922(2), γ=81.049(2)°, V=626.12(17) A˚3, Z=2. The connectivity of the strictly alternating ZnO4 and HPO3 polyhedra results in infinite macroanionic layers with 4.8-net. The organic cations locate in the interlayer region and hold the macroanionic sheets together by strong H-bonds. Compound 2 crystallized in the monoclinic system, space group P21/c (No. 14), a=9.9352(14) A˚, b=10.1487(14) A˚, c=17.8257(13) A˚, β=95.701(7), V=1788.5(4) A˚3, Z=4. The structure of 2 consists of ZnO4 tetrahedra and HPO3 pseudo-pyramids with shared vertices, forming a 3D framework with 8-ring channels. Both compounds were characterized by FTIR, elemental analysis, ICP analysis and thermogravimetric analysis. [Copyright &y& Elsevier]

A new inorganic–organic hybrid solid, (4,4′-bipy)[Zn(HPO3)]2 (4,4′-bipy=4,4′-bipyridine), has been hydrothermally synthesized in the presence of 4,4′-bipy ligand. Its structure was determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, ICP analysis, powder X-ray diffraction, thermogravimetric analysis and fluorescent spectrum. It crystallized in the monoclinic space group, P21/c, with a=9.741(2), b=7.4423(16), c=10.271(2) A˚, β=100.038(4)°, V=733.3(3) A˚3, Z=2. The structure consists of neutral sheets of zinc phosphite which is pillared through 4,4′-bipy ligands to generate a 3D framework. The compound shows relatively high thermal stability and exhibits intense photoluminescence upon photo-excitation at 362 nm. [Copyright &y& Elsevier]

The hydrothermal synthesis, crystal structure and some properties of a zinc phosphite with a neutral cluster, [Zn(2,2′-bipy)]2(H2PO3)4, are reported. This compound crystallizes in the triclinic system of space group P-1 (No. 2), a=8.3067(5) A˚, b=8.9545(4) A˚, c=10.0893(6) A˚, α=95.448(2)°, β=99.7530(10)°, γ=103.461(2)°, V=712.23(7) A˚3, Z=1. The cluster consists of 4-membered rings formed by alternating ZnO3N2 square pyramids and H2PO3 pseudo pyramids, with two “hanging” H2PO3 groups attached to each of the Zn centers. The clusters are linked together by extensive multipoint hydrogen bonding involving the phosphite units to form a sheet-like structure. This compound represents the first example of zinc phosphite with P&z.sbnd;OH bonds. An intense photoluminescence was observed from this compound upon photoexcitation at 388 nm. [Copyright &y& Elsevier]

A neutral zincophosphate monomer [Zn(2,2′-bipy)]2(H2PO4)4 has been synthesized under hydrothermal condition in the presence of 2,2′-bipyridine ligands. The structure consists of a 4-membered ring formed by vertex-sharing ZnO3N2 square pyramids and H2PO4 tetrahedra, with two H2PO4 groups hanging from the zinc atoms. This compound exhibits intense photoluminescence upon photoexcitation at 388 nm. [Copyright &y& Elsevier]

Abstract: An organically-templated chiral borogermanate (CH3NH3)2[Ge(B4O9)] (1), has been solvothermally synthesized and characterized by elemental analysis, IR, PXRD, TGA, single-crystal X-ray diffraction and UV–vis spectrum. It crystallized in the monoclinic space group C2 (No. 5) with a =10.249(1)Å, b =9.449(1)Å, c =6.956(2)Å, β =131.76(2)°, V =502.43(19)Å3, Z =2. The structure is constructed by alternate linkage of GeO4 tetrahedra and B4O9 clusters to form a zeotype framework with diamond topology. Four intersecting channels with different sizes are observed. Large circular 10-ring channels are clearly extended along the [001] direction, 9-ring channels are running along the [101], [110], and [112] directions, respectively. Additionally, two pairs of the right- and left-handed channels couple together along the [100] and [010] directions, respectively. The preliminary investigations show that compound 1 exhibits second-harmonic generation (SHG) response and ferroelectric properties. [Copyright &y& Elsevier]

A novel manganese oxyborate, K7{(BO3)[B12O18(OH)6]} · H2O (1), which is the first example showing the edge-sharing between boron and transition metal, has been solvothermally synthesized. The structure consists of [B12O20(OH)4] and [BO3] which are linked through unusual MnO5 polyhedron via vertexes and edges. This compound exhibits NLO properties and the intensity of the green light (frequency-doubled output: λ=532 nm) produced by 1 is as large as that of KDP. [Copyright &y& Elsevier]

Two new hollow 3D tubular polyoxoniobate frameworks are built from { SiNb 18 O 54 } clusters, copper-organic complexes and helical heterometallic Ba 2 K 4 O 13 / Ba 2 NaO 7 cluster chains. [Display omitted] • Two new hollow 3D tubular polyoxoniobate frameworks are synthesized hydrothermally. • The nanotubes enrich the structures of the heteropolyoxoniobate family. • The compounds 1 and 2 show excellent proton conduction properties. Two new 3D tubular polyoxoniobate frameworks, [Cu(en) 2 ] 2 {[Cu(en) 2 ] 2 K 4 Ba 2 (H 2 O) 13 (SiNb 18 O 54)} 2 ·3en·52H 2 O (1) and H 6 [Cu(en) 2 ] 2 {[Cu(en) 2 ] 2 NaBa 2 (H 2 O) 7 (SiNb 18 O 54)} 2 ·3en·50H 2 O (2) (en = ethylenediamine) have been synthesized by hydrothermal reactions. Interestingly, their frameworks both consist of rare inorganic-organic hybrid polyoxoniobate nanotubes and helical heterometallic Ba 2 K 4 O 13 / Ba 2 NaO 7 cluster chains. The nanotubes are both built from { SiNb 18 O 54 } clusters and copper-organic complexes. Compounds 1 and 2 present excellent proton conduction properties. [ABSTRACT FROM AUTHOR]