Open-framework Borophosphate:(NH4)_(0.5)Fe~II_(0.5)Fe~III_(0.5)(H_2O)_2BP_2O_8·0.5H_2O

We are investigating the synthesis and properties of a new class of open framework borophosphate solids with the goal of being able to use in optical devices and magnetic materials. Only a few open-framework ferric borophosphate compounds with a chiral tetraheda-tetraheda helices, KFe(H2O)2BP2O8)H2O(1), Fe(H2O)2BP2O8H2O(2), (NH4)0.4-FeII0.55FeIII0.5(H2O)[BP2O8]0.6H2O(3) have been reported by Boy et al.1, Ylmaze et al.2 and Huang and Schfer et al.3. However, Huang and Schfer et…     

Synthesis and Crystal Structure of Na_(10)[LaSiW_(11)O_(39)(H_2O)_4]_2·22H_2O

1 INTRODUCTION The pseudoliquid character of heteropoly compounds as catalysts is determined by their crystallographic properties. Study on the crystal structures of the heteropoly compounds could provide interesting information to enrich heteropoly acid and catalytic chemistry[1]. In the past, Zhuo Ying-Li抯 group has synthesized the carbamidine salts of 1:1 LnL(Ln=lanthanide, L=[SiW11O39]n－)[2], and Pope抯 group has reported that -SiW11O39 units are connected by lanthanide catio…     

Synthesis and Crystal Structure of a Novel Heptanuclear Ruthenium- and Sodium-containing Polyoxomolybdate [{Na(H_2O)_3}_2{Ru(dmso)_3}_2(MoO_4)_3]·_3H_2O

1 INTRODUCTION Polyoxomolybdates have been of great interest due to their unique structural varieties, associated multitude of properties and applications as catalysis, medicine and material[1, 2]. One of the most impor- tant aspects is the synthesis and investigation of the materials on polyoxomolybdates containing organo- metallic groups[3～5]. Such materials can provide molecular models for heterogeneous catalysis and display cooperative effects or bifunctional catalytic activity[6]. O…     

Synthesis and Crystal Structure of a Novel 1D Coordination Polymer:[Pr(BYBA)_3(H_2O)_2]·[Pr(BYBA)_3(H_2O)]

The novel coordination polymer [Pr(BYBA)3(H2O)2]·[Pr(BYBA)3(H2O)] (BYBAH=2-benzoylbenzoic acid) was yielded by hydrothermal synthesis,determined by single-crystal X-ray diffraction,and characterized by FT-IR and UV-Vis spectra. The crystal crystallizes in the triclinic system,space group P1 with a=9.112(3),b=14.644(5),c=27.076(11),α=84.223(3),β= 87.816(4),γ=88.902(4)o,V=3592(2)3,C84H60O21Pr2,Mr=1687.14,Z=2,F(000)=1700,Dc= 1.560 g/cm3,μ=1.419 mm-1,the final R=0.0485 and wR=0.1258 for 13035 observed reflections with I > 2σ(I). The compound contains two different building units,[Pr2(BYBA)6(H2O)4] and [Pr2(BYBA)6(H2O)2]. It is noticeable that [Pr2(BYBA)6(H2O)4] is an isolated binuclear building block,in which the Pr3+ ion centers are both located in an eight-coordinated environment. However,in [Pr2(BYBA)6(H2O)2] the Pr3+ ion centers are located in a nine-coordinated environment and connected by BYBA ligands to form 1D chains.     

Synthesis and Structure of One Novel Polyoxometalate Compound Connected via Cerium(III) Cation with Three-dimensional Framework H_2{[K(H_2O)_2]_2[Ce(H_2O)_5]_2(H_2Mo_(1.16)W_(10.84)O_(42))}·8H_2O

One novel polyoxometalate compound connected via trivalent cerium cation as bridge H2{[K(H2O)2]2[Ce(H2O)5]2(H2Mo1.16W10.84O42)}·8H2O 1 was designed and synthesized in aqueous solution. X-ray diffraction analysis reveals that the structure of 1 is a three-dimensional framework assembled from the arrangement of H2Mo1.16W10.84O42 (named paradodecmetalate-B) and Ce(H2O)53+ containing two planes, which are constructed through the unification of H2Mo1.16W10.84O4210- and Ce(H2O)53+ along the [100] and [001] directions. Crystal data: H96Ce4K4Mo2.32O128W21.68, Mr = 7074.89, monoclinic, P21/n, a = 12.5037(17), b = 17.002(2), c = 12.7473(17) A, β = 105.966(2)°, V = 2605.4(6) 3, Z = 1, Dc = 4.509 g/cm3, F(000) = 3132, μ = 26.098 mm-1, R = 0.0377 and wR = 0.0789 (I > 2σ(I)).     

Water-induced reversible dissolution/reorganization transformations of Cu(Ⅱ)-K(I) heterometallic coordination polymers

Three new heterometallic coordination compounds, namely, [KCu(I3)(L)2(H2O)2]n(1), [KCu(I3)(L)2(H2O)]n(2) and [CuK4(I3)2(L′)4]n(3), were prepared and characterized(HL=5-methylpyrazine-2-carboxylic acid, HL′=p-tolylacetic acid). Structural studies revealed that 1 and 2 exhibit 3D frameworks with rectangular channels occupied by triiodide ions. Both compounds can be symbolized as a 5-connected net with pcu topology. In compound 3, a one-dimensional polyhedral chain is connected by hexanuclear mask like clusters [Cu2K4O8]. These chains are further linked each other via rare(1,1,3,3)-triiodide ion-bridging units to generate a 3D(4,5,6)-connected net with the point symbol of {12}2{4·122}4{46}{48·62}4{49·66}4. It is noteworthy that water-induced reversible dissolution/reorganization processes occur between 1/2 and [Cu(L)2(H2O)]n·3nH2O. The thermal and photoluminescence properties of compounds 1, 2, and 3 were investigated as well.     

CRYSTAL STRUCTURE OF (NH_4)_(11)[Na(H_2O)_2P_4W_(14)O_(58)] ·12H_2O

<正> (NH4)11[Na(H2O)2P4W14O58)·12H2O, Mr = 4099. 39, triclinic, space group P1, a = 14. 376(2), b = 19.861(9), c=13. 010(3)(?) , α=104. 68(2), β=91. 37(1), γ= 104. 05(2)°, V = 3471. 1 (?)3, Z = 2, Dc=3. 922g/cm3, μ (MoKα) = 238. 274cm-1, F(000) = 3664, R = 0.0510, Rw = 0. 0665 for 9260 observed reflections with I> 3σ(I). The polyanion [Na(H2O)2P4W14O58]11- consists of two PW7O29 subunits anisostructurally, two linkage phosphorous atoms and one sodium ion with two water ligands as well. The geometries of tungsten atoms within these two subunits are almost the same as those in K12P4W14O58· 21H2O[2]. The four phosphorous atoms are in PO4 coordinations. The sodium ion locates nearly at the center of the polyanion, and is coordinated by two water molecules, five oxygen atoms of the anion and one phosphorous atom with Na-P = 3. 053(3) (?). Due to the presence of the sodium atom, the interactions between oxygen and tungsten atoms in the polyanion are somewhat weakened.     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex[La(betaine)_2(H_2O)_6Fe(CN)_6]·2H_2O

1 INTRODUCTION In the last decade, cyano-bridged Prussian Blueanalogues[1] have been intensively studied from theviewpoint of application as functionalized molecule-based magnets[2], chemical sensor materials[3], fluo-rescent materials[4] and zeolitic-type materials[5, , 6]etc. In 1976, a series of cyano-bridged three-dimen-sional rare earth hexacyanometalates(IIILnM(CN)6?nH2O (M = Fe or Cr, n = 4 or 5) were crystallized andsubjected to single-crystal X-ray analysis[7]. …     

Synthesis and Structure Characterization of Aqua-(μ_2-carbonato-O,O'''')-(2,2''''-bipyridyl)-copper(Ⅱ) Dihydrate

1 INTRODUCTION The class of materials of carbonato metal- organic compounds has received much attention as a consequence of their potential applications in biochemical and environmental protection[1～3]. Many carbonato compounds of Cu2+, Co3+ and Zn2+ etc. have been studied[4～6]. The carbonate anion is a versatile bridging ligand, which can bind metal cations in different modes to generate mononuclear, binuclear, trinuclear, tetranuclear and even 1D, 2D and 3D structures[4, 7, 8]. We…     

STRUCTURE OF PENTAAQUO PYROMEL DIZINE (Ⅱ)-DIHYDROUS [C_6H_2(COO)_4Zn_2(H_2O)_5]·2H_2O

Crystal and molecular structure of [C6H2(COO)4Zn2(H2O)5]·2H2O has been determined by X-ray diffraction technique, Mr = 507. 0,monoclinic,space group P21/n,a = 5. 925(1), 6 = 23. 613(9) ,c= 11. 790(5) A ,β= 96. 36 (3)°, V=1639. 3 (1. 0) A3,Z=4,DC = 2. 05g/cm3,λ=0. 71069 A,μ(MoKa) = 30. 9/cm-1,F(000) = 1024e. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0. 055(Re = 0. 059)for 1557(I>3σ(I))reflections. Both atoms Zn(1) and Zn(2) are bridged by the Z,E-type of the car-boxyl group, in addition, Zn (1) is monodentate-bonded to the three remaining carboxyl and Zn(2) is bonded to five water molecules. The crystal structure shows a 2-dimensional polymeric network along(010)face. The Zn(l) -O distances are in the range of 1. 94~ 2. 01 A (average 1. 98 A ). The Zn(2) -O distances are in the range of 2. 06~2. 21 A (average 2. 12A).     

SYNTHESIS, STRUCTURE AND PROPERTIES OF Na_3[V_2O_3(nta)_2]·5H_2O

<正> Compound Na3 [V2O3 (nta )2 ]·5H2O (1) (ntaH3 = N (CH2CO2H)3) has been prepared by reduction of a mixture of (NH4)2[VO(O2)2Cl] and H3(nta) in H2O with Na2S2O4. The compound crystallizes in the triclinic system, space group P1 with Mr = 685. 2, a = 11. 050(6), b=12. 179(4), c=9. 792 (3)A,α=111.71(2),β= 98. 23(3), γ= 89. 36(2)°, Z=2, V = 1210. 5A3,λ(MoKa) = 0. 71069 A, F(000) = 694 and DC = 1. 880g/cm3. The structure was solved by direct methods and refined by full-matrix least squares to final R and Rw values of 0. 055 and 0. 065, respectively.The structure of the anion can be considered as two [VO(nta)] fragments connected by one μ2-O atom. Each vanadium atom in the fragment is coordinated by one vanadyl oxygen atom, one bridging-oxygen atom, three oxygen atoms and one nitrogen atom from (nta) ligand in a distorted octahedral geometry. In this paper, we have studied the conversion of compound 1 to mononuclear compound Na2[VO(O2) (nta)]·5H2O (2) by oxidation with hydrogen peroxide, as well as thei     

Synthesis and Characterization of a One-dimensional Chain Polymer{[Cu(4-CPOA)(3-PyOH)_2(H_2O)_2]·H_2O}_n

1 INTRODUCTION Molecular self-assembly of coordination architec- tures is a rapidly developing research area of supra- molecular chemistry in recent years[1～6]. 4-Carboxy- phenoxyacetic acid (4-CPOAH2) is a multidentate flexible and rigid ligand, which is capable of coor- dinating to metal centers in versatile binding fashi- ons and can also form regular hydrogen bonds as both hydrogen-bond donors and acceptors. To date, only Na(I), Ni(II), Mn(II) and Co(II) complexes con- taining…     

CRYSTAL AND MOLECULAR STRUCTURE OF GUANIDINIUM BIS (o-AMINOPHENYLARSENIC) HEXAMOLYBDATE (CN_3H_6)_4[(o NH_2C_6H_4 As)_2Mo_6O_(24)]

<正> Guanidinium bis (o - aminophenylarsenic) hexamolybdate belongs to monoclinic space group P21/c,with a=10. 217(2),b= 18. 870(2),c= 10. 939(2)A,β = 102. 82(3)°,Z = 2,V=2056. 4A3,and Dc=2. 477 g·cm-3. Each molecule contains one [(o-NH2C6H4As)2Mo6O24]4- anion and four CN3H6+ cations. In the anion,six distorted MoO6 octahedra are connected with edges-sharing to form a six-membered Mo ring which is capped above and below by two o - aminophenylarsenic groups. There is half a molecule in an asymmetric unit. It is interesting that both phenyl planes are almost perpendicular to the plane of the Mo atoms. The structure of the anion is similar to that of [ (CH3 As)2Mo6O24]4-,[(n-C3H7As)2Mo6O24]4- or [(C6H5CH2As)2Mo6O24]4-. This is the first example of this type of compounds in which the As atom is directly connected to a substituted phenyl group.     

Crystal Structure of a Three-dimensional Coordination Polymer {[Ca_3(μ_5-OOCCH_2OCH_2COO)_3(H_2O)_4]·4H_2O}_n

A novel three-dimensional coordination polymer, {[Ca3(μ5-OOCCH2OCH2COO)3(H2O)4]- 4H2O}n, has been synthesized with oxydiacetate as bridge ligand and structurally determined by X-ray crystallography. The crystal belongs to monoclinic, space group C2/c with a = 17.805(2), b = 9.3923(12), c = 17.255(2) A, β = 107.838(5)°, V = 2746.8(6) A3, Mr = 660.58, C12H28Ca3O23, Dc = 1.597 g/cm3, μ = 0.695 mm-1, Z = 4, F(000) = 1376, GOOF = 1.027, R = 0.0303 and wR = 0.0660. In the complex there are two coordination modes for Ca(II) ions, one coordinated by three μ5-OOCCH2OCH2COO2- bridge ligands together with two H2O molecules, and the other by five μ-5-OOCCH2OCH2COO2 bridge ligands. In both coordination modes each Ca(II) ion assumes a distorted dipentapyramidal CaO7 geometry; whereas each oxydiacetate is coordinated with five Ca(II) ions and acts as a pentdentates bridge ligand.     

Synthesis and Structural Characterization of a Cyano-bridged 1-D Lanthanum(Ⅲ)-iron(Ⅲ) Complex [La(DMSO)_5(H_2O)](μ-CN)_2[Fe(CN)_4]·H_2O

A new lanthanumⅢ-ironⅢ complex [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4]·H2O 1 (DMSO=dimethylsulfoxide) has been prepared by a facile approach,ball-milling method,and characterized by X-ray diffraction. The crystal belongs to monoclinic,space group P21/n with a= 9.7125(3),b=21.5336(7),c=14.3804(5),β=93.242(3)o,C16H34FeLaN6O7S5,Mr=777.55,V =3002.8(2)3,Z=4,Dc=1.720 g/cm3,S=1.053,μ(MoKα)=2.278 mm–1,F(000)=1564,R= 0.0490 and wR=0.1270. The crystal structure analysis of 1 reveals a slightly distorted square-antiprism eightfold-coordinated La(Ⅲ) ion and a 1-D zigzag chain structure extending through the Fe-CN-La-NC-Fe linkages. The [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4] species are held together via hydrogen bonds to form a three-dimensional framework.     

Syntheses and Crystal Structures of Two New Metal Phosphonates:[Mn(H_2O)_2(C_(12)H_8N_2)(HO_3PCH_2CH_2CO_2)] and [Co(H_2O)_4(C_(10)H_8N_2)]·(HO_3PCH_2CH_2CO_2)

By the reactions of manganese(II) acetate, 2-sulfoethylphosphonic acid, 1,10-phen (1,10-phen = 1, 10-phenanthroline) or cobalt(II) acetate, 4,4'-bipy and 2-carboxyethylphosphonic acid, two novel compounds of [Mn(H2O)2(C12H8N2)(HO3PCH2CH2CO2)] (1) and[Co(H2O)4 (C10H8N2)]· (HO3PCH2CH2CO2) (2) have been synthesized and characterized by IR spectroscopy, elemental analyses and single-crystal X-ray diffraction. Compound 1 has a 0D structure. Two Mn(II) ions are linked by two 2-carboxyethylphosphonic acid ligands, forming a centrosymmetric dimer. These dimers are further interlinked into a 2D layer structure by π-π stacking interactions and hydrogen bonds. Compound 2 has a 1D chain structure. The 2-carbo- xyethylphosphonic acid remains uncoor- dinated and acts as the organic template. By the bridge of 4,4'-bipy, the [Co(4,4'-bipy)]2+ chains are formed.     

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…     

Hydrothermal Synthesis and Crystal Structure of a Bivanadyl Capped Keggin Polyoxomet alate[Zn(2,2''''-bpy)_2(H_2O)]_2[HPMo_(12)O_(40)(VO)_2]

1 INTRODUCTION The design and synthesis of organic-inorganic hy-brid compounds are of great interest owing to theirextensive theoretical and practical applications in ca-talysis, medicine, analytical chemistry, nanotechno-logy, electrochromism, magnetism and photochemis-try[1～5]. In heteropolyoxometalate chemistry, a newadvance is the decoration of polyoxoanions with va-rious organic and transition metal complex moieties.In contrast to a large number of known organic andtransition-metal-s…     

Hydrogen-bonded Three-Dimensional Networks Encapsulating One-dimensional Covalent Chains: [Cu(3-ampy)(H_2O)_4](SO_4)·(H_2O) (3-ampy = 3-Aminopyridine)

A three-dimensional complex [Cu(3-ampy)(H2O)4](SO4)·(H2O) (3-ampy = 3-amino- pyridine) has been synthesized. Crystallographic data: C5H16CuN2O9S, Mr = 343.80, triclinic, space group P1, a = 7.675(2), b = 8.225(3), c = 10.845(3) A, α = 86.996(4), β = 76.292(4), γ = 68.890(4)°, V = 620.0(3) A3, Z = 2, Dc = 1.841 g/cm3, F(000) = 354 and μ = 1.971 mm-1. The structure was refined to R = 0.0269 and wR = 0.0659 for 1838 observed reflections (I > 2σ(I)). The structure consists of [Cu(3-ampy)(H2O)4]2+ cations, SO42- anions and lattice water molecules. 3-Ampy acting as a bidentate bridging ligand generates a 1D covalent chain. A supramolecular 2D framework is formed through π-π stacking of pyridine rings. The lattice water molecules and SO42- anions are located between the adjacent 2D frameworks. The hydrogen bonding interactions from lattice water molecules and SO42- anions to coordinate water extend the 2D framework into a 3D network.     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Mo(V) Phosphate [Zn(Mo~v_6P_4O_(31)H_(10))_2(C_4H_(14)N_3)_2]·2C_4H_(13)N_3·8H_2O

1 INTRODUCTION Hydrothermal synthesis of Mo(V) phosphates has allowed various structures, all characterized by the presence of identical clusters with the composition Mo12MP8X62 (X = O, OH) to be stabilized[1～6]. Many Mo(V) phosphates with such clusters have been iso- lated to date. The first compound was discovered by Haushalter and Lai[1] for M = Na with the formula (PPh4)2[(H3O)2NaMo6P4O24(OH)7]?5H2O. Recently, a second type of structure has been observed for M = Na (Na8(…