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Sue-Lein Wang

Publications and source records attributed to Sue-Lein Wang.

18 recordsLinked to original sources

Hydrothermal synthesis and characterization of two cobalt phosphates based on double-four-ring units with fluorine-occlusion and phosphite-substitution modifications.

Two new fluorinated microporous cobalt phosphates, (H2en)0.5[F(0.25)Co(H(0.5)PO4)0.5(PO4)0.5].0.25H2O (1) and (H2en)0.5[Fx(H2O)0.25(-x)Co(HPO3)x(PO4)1-x].0.25H2O (x = 0.17; 2), have been synthesized from different P sources, H3PO4 and H3PO3, in the presence of ethylenediamine and F ions. Both structures of 1 and 2 are based on the similar secondary building unit of a double four ring (D4R). 1 crystallizes in the orthorhombic space group Cmcm with a = 14.895(1) A, b = 9.7133(9) A, c = 13.688(1) A, V = 1980.4(3) A(3), and Z = 16 and is built up from fully F-occluded double-four-ring units via corner-sharing Co and P polyhedra and edge-sharing Co polyhedra. 2 crystallizes in the tetragonal space group /42m with a = 10.2033(4) A, c = 9.5545(9) A, V = 994.7(1) A(3), and Z = 8 and adopts an ACO-type framework with strict alternation of corner-sharing Co and P polyhedra. On the basis of the evidence from ion chromatography studies and elemental analyses, 2 contains both phosphate and phosphite ions, and the amount of F ions in 2 is the same as the amount of phosphite ions. This implies that some PO4(3-) groups in 2 are substituted by HPO3(2-) groups with the same amount of F(-) occlusion in the center of D4R as charge compensation. Magnetic susceptibility measurements of both 1 and 2 appear that they contain mainly antiferromagnetic interaction (theta = -27.8 K for 1 and -35.0 K for 2). However, the magnetic coupling is much more complicated in compound 1 because of the Co-O-Co linkages in it. Low-field temperature-dependent magnetization curves of 1 showed spontaneous magnetization in the form of two continuous bumps, one sharp and one broad. This may be related to the temperature dependence of two related but different types of spin canting. At 2 K, 1 also showed a large coercive field of about 5000 Oe.

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Hydrothermal synthesis of a three-dimensional organic-inorganic hybrid network formed by poly(oxomolybdophosphate) anions and nickel coordination cations.

A novel organic-inorganic hybrid nickel molybdenum(V) phosphate has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and magnetic susceptibility. The structure consists of poly(oxomolybdophosphate) anions linked by both Ni(II) cations and 4,4-bipyridine bridging ligands to form a three-dimensional open-framework structure with large cavities where the uncoordinated 4,4'-bipyridinium cations and lattice water molecules are located. This is the first example of an extended framework solid containing poly(oxomolybdophosphate) anions interconnected by both transition-metal complexes and organic moieties. Crystal data: (4,4'-H2bpy)[Ni(4,4'-bpy)(H2O)2Ni(0.5)Mo6(OH)3O12(HPO4)4].2H2O, orthorhombic, space group Pccn (No. 56), a = 27.745(2) A, b = 16.158(1) A, c = 22.819(2) A, V =10230.3(1) A(3), and Z = 8.

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Rb6(InCo)2(Si9O26): a mixed-metal silicate containing 20-membered-ring silicate single layers with a very low Si:O ratio.

A new cobalt-indium silicate, Rb6(InCo)2(Si9O26), has been synthesized via a high-temperature, high-pressure hydrothermal method and characterized by single-crystal X-ray diffraction. It crystallizes in the noncentrosymmetric orthorhombic space group Aba2 (No. 41) with a = 20.779(1) A, b = 12.0944(6) A, c = 10.7761(5) A, V =2708.1(2) A(3), and Z = 4. The structure consists of 20-membered-ring silicate single layers of corner-sharing SiO4 tetrahedra interconnected by dimers of edge-sharing CoO4 tetrahedra and InO6 octahedra into a 3D framework. The Si:O ratio for the title compound is the lowest among the known single-layer silicates. Magnetic susceptibility confirms the divalent state of the cobalt ion. The powder sample has a second-harmonic-generation signal, confirming the absence of a center of symmetry in the structure.

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Discrete water hexamers and template-assisted molecular recognition in an elastic zincophosphate lattice.

Water molecules and terephthalic acid, respectively, exist as a self-assembled monolayer of cyclic (H2O)6 clusters and (TA)infinity chiral chains between the zincophosphate sheets (in blue wires); the irremovable template H3tren3+ ions (in purple wires) are dynamic and could translate back and forth on the sheets during the conversion of the supramolecule contained in one another.

Crystallography, X-Ray↗

Direct white light phosphor: a porous zinc gallophosphate with tunable yellow-to-white luminescence.

A nanoporous zinc gallophosphate framework, NTHU-4, possessing 14-ring channels, disordered rims, and two luminant analogues, NTHU-4Y and NTHU-4W, has been synthesized and characterized; NTHU-4Y is an intrinsic yellow phosphor, while NTHU-4W is a white phosphor. The unique tetrahedral framework can be excited by wavelengths longer than 254 nm to give intense yellow-to-white luminescence. Subtle changes in disorderliness were observed to be related to the distinct photoluminescence property.

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Rb3In(H2O)Si5O13: a novel indium silicate with a CdSO4-topological-type structure.

A novel indium silicate, Rb3In(H2O)Si5O13, has been synthesized using a high-temperature, high-pressure hydrothermal method and characterized by single-crystal X-ray diffraction. The structure consists of five-membered rings of corner-sharing SiO4 tetrahedra connected via corner sharing to four adjacent five-membered rings to form a 3D silicate framework that belongs to the CdSO4 topological type. The InO6 octahedron shares five of its corners with five different SiO4 tetrahedra to form a 3D frame-work that delimits two types of channels to accommodate the rubidium cations. The sixth corner of InO6 is coordinated H2O. The structure is related to that of the titanium silicate ETS-10, and these are the only two metal silicates that have the CdSO4-topological-type structure. In addition, the crystal of Rb3In(H2O)Si5O13 shows an intense second harmonic generation signal. Crystal data: H2Rb3InSi5O14, monoclinic, space group Cc (No. 9), a = 9.0697(5) A, b = 11.5456(6) A, c = 13.9266(8) A, beta = 102.300(1) degrees, V = 1424.8(1) A3, and Z = 4.

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New titanium and nickel gallophosphates with layered structures.

Two new transition-metal gallophosphates, (H(2)C(4)H(10)N(2))(3)[(Ti(2.5)(H(2)O)(4)Ga(5.5)(PO(4))(10)].2H(2)O (TGP-1) and [H(3.5)(C(4)H(13)N(3))(2)][(Ni(0.5)(OH)(4)Ga(5.5)(PO(4))(3)(HPO(4))(4)].2H(2)O (NGP-1), have been synthesized under mild hydrothermal conditions and characterized by single-crystal X-ray diffraction, thermogravimetric analysis, electron paramagnetic resonance, electron probe microanalysis, and magnetic susceptibility data. TGP-1 exhibits a unique two-dimensional structure consisting of tetrahedral and octahedral metals centers and is the foremost paramagnetic TiGaPO material ever prepared. NGP-1 as well represents the first NiGaPO compound and adopts a layer structure that is constructed from hexameric M-O clusters of trigonal bipyramids and octahedra. In both compounds, the transition metals incorporate with gallium into octahedral sites only, while the four- and five-coordinated metals centers are only Ga(3+) ions. The unique sites for Ti(3+) and Ni(2+) ions have been initially elucidated from single-crystal structure refinements and further confirmed by bond-valence-sum calculations, EPR, and magnetic susceptibility studies. Crystal data: TGP-1, monoclinic, P2(1)/c; a = 25.692(2) A, b = 9.6552(8) A, c = 9.8418(8) A, beta = 96.737(2)(o) , V = 2424.5(3) A(3), and Z = 2; NGP-1, monoclinic, C2/c, a = 20.8363(12) A, b = 11.9546(7) A, c = 16.4577(9) A, beta = 117.285(1)(o) , V = 3643.3(1) A(3), Z = 4.

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Metamagnetism in cobalt phosphates with pillared layer structures: [Co3(pyz)(HPO4)2F2] and [Co3(4,4'-bpy)(HPO4)2F2].xH2O.

Two new cobalt phosphates, [Co(3)(pyz)(HPO(4))(2)F(2)] (1) and [Co(3)(4,4'-bpy)(HPO(4))(2)F(2)].xH(2)O (x approximately 0.7) (2), have been synthesized by hydrothermal methods in the presence of aromatic amines, and characterized by single-crystal X-ray diffraction and magnetic susceptibility. Their structures consist of neutral sheets of fluorinated cobalt phosphate which are pillared through pyrazine and 4,4'-bipyridine molecules to form 3D frameworks. The structures are related to that of the mineral lazulite. Both compounds show long-range antiferromagnetic ordering below 15 K and metamagnetic behaviors. Compound 1 reveals a two-step magnetic phase transition. Crystal data for 1: monoclinic, space group C2/c (No. 15), a = 21.809(4) A, b = 7.370(1) A, c = 7.395(1) A, beta = 103.753(3) degrees, and Z = 4. Crystal data for 2 are the same as those for 1 except a = 29.940(2) A, b = 7.4421(5) A, c = 7.4170(5) A, and beta = 93.444(1) degrees.

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Cs2Pd3(P2O7)2 and Cs2Pd3(As2O7)2: a 3D palladium phosphate with a tunnel structure and a 2D palladium arsenate containing strings of palladium atoms.

Cs(2)Pd(3)(P(2)O(7))(2) (1) and Cs(2)Pd(3)(As(2)O(7))(2) (2) have been synthesized by molten flux reactions and characterized by single-crystal X-ray diffraction. The structure of 1 consists of discrete Pd(II)O(4) squares which are linked by P(2)O(7) groups via corner-sharing to generate a 3D framework containing 12-ring channels in which Cs(+) cations are located. Compound 2 adopts a 2D layer structure with the interlayer space filled with Cs(+) cations. Within a layer there are PdO(4) squares and As(2)O(7) groups fused together via corner-sharing. Adjacent layers are stacked such that strings of Pd atoms are formed. The PdO(4) squares show eclipsed and staggered stacks with alternate short and long Pd...Pd distances. The two compounds adopt considerably different structures although they have the same general formula: Cs(2)Pd(3)(X(2)O(7))(2). Compound 2 is the first palladium arsenate reported. Crystal data for 1: orthorhombic, space group Cmc2(1) (No. 36), a = 7.6061(4) A, b = 14.2820(7) A, c = 14.1840(7) A, and Z = 4. Crystal data for 2: tetragonal, space group P4/n (No. 85), a = 16.251(1) A, c = 5.9681(5) A, and Z = 4.

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A zeolitic organo-metallophosphate hybrid material with bimodal porosity.

The first metal carboxylatophosphate, NTHU-2, contains inorganic ZnHPO4 layers linked by BDC units (BDC = 1,4-benzene dicarboxylate or terephthalic anion); the three-dimensional anionic framework has large pores with the smallest diameter being 1.36 nm; N2 sorption isotherms reveal both micro- and mesoporosity; the new material is photoluminescent and disassembles in water wherein the discharged organic fragments form mixed crystals.

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Novel transition metal oxalatophosphates with a two-dimensional honeycomb structure: (H3TREN)[M2(HPO4)(C2O4)2.5] x 3H2O (M = Mn(II) and Fe(II), TREN = tris(2-aminoethyl)amine).

Two new layered transition metal oxalatophosphates, (H(3)TREN)[M(2)(HPO(4))(C(2)O(4))(2.5)].3H(2)O (M = Mn(II) and Fe(II)), have been synthesized by hydrothermal methods in the presence of a structure-directing organic amine, tris(2-aminoethyl)amine, and characterized by single-crystal X-ray diffraction and magnetic susceptibility. They are the first metal oxalatophosphates which adopt a two-dimensional honeycomb structure with the organic cations and water molecules intercalated in between. Within a layer, there are 12-membered pores made from 6 Mn, 1 phosphate, and 5 oxalate units. Measurements of field dependence of magnetization and variable-temperature susceptibilities under different fields were performed on a polycrystalline sample of the manganese compound. The results indicate a phase transition from a paramagnetic to an antiferromagnetic coupled state at about 12 K. Crystal data for the manganese compound follow: triclinic, space group Ponemacr; (No. 2), a = 8.8385(6) A, b = 9.0586(6) A, c = 16.020(1) A, alpha = 77.616(1) degrees, beta = 83.359(1) degrees, gamma = 68.251(1) degrees, and Z = 2. Crystal data for the iron compound are the same as those for the manganese compound except a = 8.7776(9) A, b = 8.9257(9) A, c = 15.884(2) A, alpha = 78.630(2) degrees, beta = 84.018(2) degrees, and gamma = 67.372(2) degrees.

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Hydrothermal synthesis, crystal structure, and solid-state NMR spectroscopy of a new indium silicate: K2In(OH)(Si4O10).

A new indium(III) silicate, K(2)In(OH)(Si(4)O(10)), has been synthesized by a high-temperature, high-pressure hydrothermal method. It crystallizes in the monoclinic space group P2(1)/m (No. 11) with a = 11.410(1) A, b = 8.373(1) A, c = 11.611(1) A, beta = 112.201(2) degrees, and Z = 4. The structure, which is analogous to that of K(2)CuSi(4)O(10), consists of unbranched vierer 4-fold chains of corner-sharing SiO(4) tetrahedra running along the b axis linked together via corner sharing by chains of trans-corner-sharing InO(4)(OH)(2) octahedra to form a 3-D framework which delimits 8-ring and 6-ring channels to accommodate K(+) cations. The presence of hydroxyl groups is confirmed by IR spectroscopy. The (29)Si MAS NMR exhibits four resonances at -88.6, -90.1, -97.4, and -98.2 ppm corresponding to four distinct crystallographic Si sites. A (1)H --> (29)Si CP/MAS NMR experiment was performed to assign the four resonances.

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Synthesis, crystal structure, and solid state NMR spectroscopy of NH(4)[(V(2)O(3))(2)(4,4'-bpy)(2)(H(2)PO(4))(PO(4))(2)].0.5H(2)O, a mixed-valence vanadium(IV,V) phosphate with a pillared layer structure.

A mixed-valence vanadium phosphate, NH(4)[(V(2)O(3))(2)(4,4'-bpy)(2)(H(2)PO(4))(PO(4))(2)].0.5H(2)O, has been synthesized under hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group C2/c (No. 15) with a = 12.6354(8) A, b = 9.9786(6) A, c = 23.369(1) A, beta = 92.713(1) degrees, and Z = 4 with R(1) = 0.0389. The structure consists of dimers of edge-sharing vanadium(IV,V) octahedra that are connected by corner-sharing phosphate tetrahedra to form layers in the ab-plane, which are further linked through 4,4'-bipyridine pillars to generate a 3-D framework. Magnetic susceptibility confirms the valence of the vanadium atoms. The (31)P MAS NMR spectrum shows a resonance centered at 80 ppm with a shoulder at ca. 83 ppm in an intensity ratio close to 1:2, which correspond to two distinct P sites. The observed large downfield (31)P NMR shifts can be ascribed to magnetic exchange coupling involving phosphorus atoms. The unpaired electron spin density at the phosphorus nucleus was determined from variable-temperature (31)P NMR spectra. The (1)H MAS NMR spectrum was fitted to six components in accordance with the structure as determined from X-ray diffraction.

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Synthesis and Chemistry of Fullerene Derivatives Bearing Phosphorus Substituents. Unusual Reaction of Phosphines with Electron-Deficient Acetylenes and C(60).

A unique method to introduce phosphorus substituents onto C(60) is based on the reaction of phosphines with acetylenes and C(60). Treatment of C(60) with phosphines (PR(3)) and electron-deficient acetylenes (A) in toluene at ambient temperature gave fullerene derivatives (1, R = C(6)H(5) and A = MeO(2)CC&tbd1;CCO(2)Me; 2, R = C(6)D(5) and A = MeO(2)CC&tbd1;CCO(2)Me; 3, R = C(6)H(5) and A = EtO(2)CC&tbd1;CCO(2)Et; 4, R = p-CH(3)C(6)H(5) and A = MeO(2)CC&tbd1;CCO(2)Me; 6, R = C(6)H(5) and A = trans-MeO(2)CC&tbd1;CCH=CHCO(2)Me) consisting of a phosphorus ylide group and a cyclopropane ring on the fullerene moiety in good to excellent yields. The structures of these ylide derivatives are determined on the basis of their spectral data and single-crystal X-ray diffraction measurements. All these ylides show temperature-dependent NMR spectra that can be rationalized on the basis of interchange between two Z,E isomers and restricted rotation of the substituents on the fullerene moiety. Based on the known chemistry of phosphines and acetylenes, we propose a mechanism to account for the formation of these ylide derivatives. Phosphine ylides 1 and 4 readily undergo protonation and decarboxylation in the presence of acid to give phosphonium salts 7 and 8, respectively.

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Layered Iron(III) Arsenates: Synthesis and Characterization of A(2)Fe(2)O(AsO(4))(2) (A = K, Rb).

Two new iron(III) arsenates K(2)Fe(2)O(AsO(4))(2) (1) and Rb(2)Fe(2)O(AsO(4))(2) (2) have been synthesized and characterized by single-crystal X-ray diffraction, magnetic susceptibilities, and Mossbauer spectroscopy. The two compounds are isostructural and exhibit a sheet structure consisting of infinite slabs of edge-sharing FeO(6) octahedra linked into sheets by AsO(4) tetrahedra, with the alkali-metal cations in the interlayer region. Crystal data for 1: orthorhombic, space group Pnma (No. 62), a = 8.5219(3) Å, b = 5.7612(2) Å, c = 17.9452(6) Å, Z = 4. Crystal data for 2: As above, except a = 8.5330(2) Å, b = 5.7945(2) Å, c = 18.6157(1) Å. Room-temperature Mossbauer data confirm the presence of Fe(III). Magnetic susceptibility measurements on compound 2 show that it undergoes a transition to a weak ferromagnetic state near 25 K.

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Cs(5)Mo(8)O(24)(OH)(2)AsO(4).2H(2)O and Cs(7)Mo(8)O(26)AsO(4): Two Novel Molybdenum(VI) Arsenates Containing Heteropolyanions [AsMo(8)O(30)H(2)](5)(-) and [AsMo(8)O(30)](7)(-).

Two novel molybdenum(VI) arsenates, Cs(5)Mo(8)O(24)(OH)(2)AsO(4).2H(2)O and Cs(7)Mo(8)O(26)AsO(4), have been prepared and their structures determined. Cs(5)Mo(8)O(24)(OH)(2)AsO(4).2H(2)O was synthesized by a high-temperature, high-pressure hydrothermal method and characterized by single-crystal X-ray diffraction, IR spectroscopy, and thermogravimetric analysis. Diffraction measurements were performed on a CCD area detector system. It crystallizes in the orthorhombic space group Cmcm with a = 8.8048(3) Å, b = 23.4314(9) Å, c = 16.0499(6) Å, and Z = 4. The structure consists of [AsMo(8)O(30)H(2)](5)(-) cluster anions which are made up of two tetranuclear {Mo(4)O(15)H} cores linked by an arsenic(V) atom. Upon heating, half of the structural unit first transforms to Cs(7)Mo(8)O(26)AsO(4), and the other half decomposes to Cs(3)AsO(4) and MoO(3) at higher temperature. Cs(7)Mo(8)O(26)AsO(4) crystallizes in the orthorhombic space group Ibca with a = 12.1247(4) Å, b = 22.9153(7) Å, c = 24.3777(7) Å, and Z = 8. It possesses [AsMo(8)O(30)](7)(-) cluster anions resembling to those found in the original structure. Cs(7)Mo(8)O(26)AsO(4) may be viewed as a dehydrated form of Cs(5)Mo(8)O(24)(OH)(2)AsO(4).2H(2)O from which the lability of [AsMo(8)O(30)H(2)](5)(-) with respect to dissociation of AsO(4)(3)(-) is first shown in the solid state. Structural differences between [AsMo(8)O(30)H(2)](5)(-) and [AsMo(8)O(30)](7)(-) are closely correlated with the cesium cations and water molecules present in the crystals. The title compounds are also the first structurally characterized examples in the Cs-Mo-As-O system.

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