Structure Cristalline du Phosphite Acide de Calcium,Ca(HPO3H)2 · H2O

Crystal Structure of Calcium Hydrogenphosphite Monohydrate, Ca(HPO₃H)₂ · H₂O Ca(HPO₃H)₂ · H₂O is triclinic, space group P1 , with a = 7.007(1), b = 8.100(1), c = 6.773(1) Å, α = 84.92(1), β = 95.72(2) and γ = 112.00(1)°; V = 354.1 ų, Z = 2; ?_x = 2.251 g/cm³ and ?_ob = 2.21(1) g³/cm³. The structure was refined to R = 0.019 for 1640 independent reflections. HPO₃H^? ions are linked together by hydrogen bonds (with acid hydrogen atoms) to form parallelograms. Chains of parallelograms are parallel to c axis. The coordination number of the calcium ion is seven; the mean values of Ca? O is 2.409 Å.     

C4H8N2H4·Zn(HPO3)2的水热合成和结构表征

在过去的十几年中 ,人们对含有机模板的、由 Zn O4 四面体和 PO4 四面体基本结构单元组成的磷酸锌盐进行了深入广泛的研究 ,发现其结构具有多样性 [1] .近年来 ,人们又开始探索用亚磷酸氢根( HPO3)替代磷酸根 ( PO4 ) ,形成结构新颖的含有机模板的亚磷酸盐 .与磷酸根相比 ,亚磷酸氢根只能与 3个邻近的阳离子通过 P— O— M( M=Zn等 )键相连 ,结构同 [PO3( OH) ]相似 .鉴于此 ,HPO3完全可以作为搭建空旷骨架化合物的结构基元 .与磷酸盐的研究相比 ,以有机胺为模板的过渡金属亚磷酸盐合成研究相对较少 .Harrison等 [2 ,3] 报道了通过…     

Synthesis and Crystal Structure of （H3O）2[Cu3Cl3（H2O）3（NC9H12.5O6）2]

1 INTRODUCTION The polydentate ligand nitrilotripropionic acid, H3ntp[N(CH2CH2COOH)3], has attracted conside- rable research interest in constructing coordination polymers, designing organic-inorganic hybrid mate- rials[1], synthesizing supramolecular compounds[2], etc. due to its high degree of flexibility with three carboxylic acid moieties allowing for a variety of coordination through oxygen atoms[3]. It also pro- vides other versatile properties such as the possibili- ty of inter-…     

配合物[Cu（C8H6CIO3）2（H2O）2]的合成与晶体结构

以硝酸铜和对氯苯氧乙酸为原料,合成了标题化合物[Cu（C8H6ClO3）2（H2O）2],并用元素分析仪、红外光谱仪、X射线单晶衍射仪表征了其组成和晶体结构．结果表明,所合成的晶体属三斜晶系,Pi空间群,a=0．51146（6）nm,b=0．70640（8）nm,c=1．326410（15）nm,a=81．7770（10）°,β=86．361（2）°,γ=76．3970（10）°,F（000）=239,Z=1;最终偏离因子R=0．0264,wR=0．0674．在配合物中,铜离子与来自两个对氯苯氧乙酸根的两个羧基氧原子、两个醚氧原子以及来自两个水分子的氧原子配位,形成变形八面体结构．     

Hydrothermal Synthesis and Structure of a New Two- dimensional Zincophosphite:Zn2(HPO3)3(H2DACH (DACH = 1,2-diaminocyclohexane)

A new open-framework zincophosphite, Zn2(HPO3)3(H2DACH 1, was hydrothermally synthesized in the presence of 1,2-diaminocyclohexane (DACH) as structure-directing agent. Its structure was determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, powder X-ray diffraction and thermogravimetric analysis. Crystal data for 1: Mr = 486.88, monoclinic, space group P21/c with a = 10.2287(11), b = 9.7624(11), c = 16.1686(18) A,β = 92.573(2), V = 1612.9(3) A3, Z = 4, Dc = 2.005 g/cm3, F(000) = 984, μ = 3.314 mm-1 and S = 1.152. The final R = 0.0473 and wR = 0.1121 for 2456 observed reflections with I > 2σ(I). The inorganic layer consisting of four- and eight-membered rings is constructed of alternating ZnO4 tetrahedra and HPO3 pseudo pyramids by sharing vertices. The organic template molecules reside in the interlayer region and interact with the inorganic network through H-bonds.     

Syntheses and structures of two chiral zincophosphite compounds: [Zn(C8H8N2)(HPO3)] and (C6H13N2)[Zn3(C6H12N2)(HPO3)3(H2PO3)

Employing achiral organic amines (2-methylbenzimidazole and 1,4-diazabicyclo[2.2.2]octane) as the structure-directing agent and ligand, two chiral zincophosphites, [Zn(C(8)H(8)N(2))(HPO(3))] 1 and (C(6)H(13)N(2))[Zn(3)(C(6)H(12)N(2))(HPO(3))(3)(H(2)PO(3))] 2, have been hydro(solvo)-thermally synthesized, crystallizing in the chiral space group P2(1)2(1)2(1). Single-crystal structural analysis reveals that compound 1 consists of alternating ZnO(3)N and HPO(3) units exhibiting a neutral one-dimensional chiral chain. Interestingly, the organic ligands interact with the inorganic chain via hydrogen-bonds in hydrogen-bonded helix fashion. Compound 2, a three-dimensional chiral open framework with 16-MR channels, is formed by the distorted {Zn(3)P(4)} secondary building unit (SBU). The organic amine molecules play dual roles as both ligands and countercations.     

AgCo3PO4(HPO4)2

The structure of the hydro­thermally synthesized compound AgCo₃PO₄(HPO₄)₂, silver tricobalt phosphate bis­(hydrogen phosphate), consists of edge‐sharing CoO₆ chains linked together by the phosphate groups and hydrogen bonds. The three‐dimensional framework delimits two types of tunnels which accommodate Ag⁺ cations and OH groups. The title compound is isostructural with the compounds AM₃H₂(XO₄)₃ (A = Na or Ag, M = Co or Mn, and X = P or As) of the alluaudite structure type.     

Preparation and Crystal Structure of Potassium Iron Hydrogen Phosphate,KFe3(HPO4)2(H2PO4)6 · 4 H2O

Single crystals of potassium iron hydrogen phosphate, KFe₃(HPO₄)₂(H₂PO₄)₆ · 4 H₂O, were prepared hydrothermally by heating a mixture of Fe₂O₃, H₃PO₄ and K₂CO₃ with a small amount of water. It crystallizes monoclinic, space group C2/c (N° 15 Int. Tab.) with Z = 4 and a = 1701(2), b = 960.4(5), c = 1750(1) pm, β = 90.88(7)°. The crystal structure was solved by using 1716 unique reflections F₀ > 4σ(F₀) with a final wR2 value of 0.126 (SHELXL-93). The main feature of the crystal structure are layers formed by PO₄-tetrahedra around the FeO₆-octahedra parallel to (001). K⁺ and H₂O molecules connect these layers. Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), Charge Distribution (CHARDI) and the Madelung Part of Lattice Energy (MAPLE) are calculated for the title compound. The existence of hydrogen bonds is confirmed by these calculations.     

Ferromagnetism in malonato-bridged copper(II) complexes. Synthesis,crystal structures,and magnetic properties of [[Cu(H2O)3][Cu(mal)2(H2O)]]n and [[Cu(H2O)4]2[Cu(mal)2(H2O)]][Cu(mal)2(H2O)2][[Cu(H2O)4][Cu(mal)2(H2O)2][(H2mal = malonic acid)

Three malonato-bridged copper(II) complexes of the formulas [[Cu(H2O)3][Cu(C3H2O4)2(H2O)]]n (1), [[Cu(H2O)4]2[Cu(C3H2O4)2(H2O)]] [Cu(C3H2O4)2(H2O)2][[Cu(H2O)4][Cu(C3H2O4)2(H2O)2]] (2), and [Cu(H2O)4][Cu(C3H2O4)2(H2O)2] (3) (C3H2O4 = malonate dianion) have been prepared, and the structures of the two former have been solved by X-ray diffraction methods. The structure of compound 3 was already known. Complex 1 crystallizes in the orthorhombic space group Pcab, Z = 8, with unit cell parameters of a = 10.339(1) A, b = 13.222(2) A, and c = 17.394(4) A. Complex 2 crystallizes in the monoclinic space group P2/c, Z = 4, with unit cell parameters of a = 21.100(4) A, b = 21.088(4) A, c = 14.007(2) A, and beta = 115.93(2) degrees. Complex 1 is a chain compound with a regular alternation of aquabis(malonato)copper(II) and triaquacopper(II) units developing along the z axis. The aquabis(malonato)copper(II) unit acts as a bridging ligand through two slightly different trans-carboxylato groups exhibiting an anti-syn coordination mode. The four carboxylate oxygens, in the basal plane, and the one water molecule, in the apical position, describe a distorted square pyramid around Cu1, whereas the same metal surroundings are observed around Cu2 but with three water molecules and one carboxylate oxygen building the equatorial plane and a carboxylate oxygen from another malonato filling the apical site. Complex 2 is made up of discrete mono-, di-, and trinuclear copper(II) complexes of the formulas [Cu(C3H2O4)2(H2O)2]2-, [[Cu(H2O)4] [Cu(C3H2O4)2(H2O)2]], and [[Cu(H2O)4]2[Cu(C3H2O4)2(H2O)]]2+, respectively, which coexist in a single crystal. The copper environment in the mononuclear unit is that of an elongated octahedron with four carboxylate oxygens building the equatorial plane and two water molecules assuming the axial positions. The neutral dinuclear unit contains two types of copper atoms, one that is six-coordinated, as in the mononuclear entity, and another that is distorted square pyramidal with four water molecules building the basal plane and a carboxylate oxygen in the apical position. The overall structure of this dinuclear entity is nearly identical to that of compound 3. Finally, the cationic trimer consists of an aquabis(malonato)copper(II) complex that acts as a bismonodentate ligand through two cis-carboxylato groups (anti-syn coordination mode) toward two tetraaqua-copper(II) terminal units. The environment of the copper atoms is distorted square pyramidal with four carboxylate oxygens (four water molecules) building the basal plane of the central (terminal) copper atom and a water molecule (a carboxylate oxygen) filling the axial position. The magnetic properties of 1-3 have been investigated in the temperature range 1.9-290 K. Overall, ferromagnetic behavior is observed in the three cases: two weak, alternating intrachain ferromagnetic interactions (J = 3.0 cm-1 and alpha J = 1.9 cm-1 with H = -J sigma i[S2i.S2i-1 + alpha S2i.S2i+1]) occur in 1, whereas the magnetic behavior of 2 is the sum of a magnetically isolated spin doublet and ferromagnetically coupled di- (J3 = 1.8 cm-1 from the magnetic study of the model complex 3) and trinuclear (J = 1.2 cm-1 with H = -J (S1.S2 + S1.S3) copper(II) units. The exchange pathway that accounts for the ferromagnetic coupling, through an anti-syn carboxylato bridge, is discussed in the light of the available magneto-structural data.     

Structure and spectral characteristics of (NH4)2[Re2(HPO4)4 · 2H2O]

The compound (NH₄)₂[Re₂(HPO₄)₄ · 2H₂O] has been synthesized and characterized by electronic and vibrational spectroscopy. The molecular structure has been determined by X-ray diffraction (MoK _α radiation, λ = 0.71073 Å). The (NH₄)₂[Re₂(HPO₄)₄ · 2H₂O] coordination units form centrosymmetrical binuclear ordering with each metal atom being coordinated in a distorted octahedron incorporating one rhenium atom, one oxygen atom of the water molecule, and four phosphate oxygen atoms in the equatorial plane. The rhenium-rhenium bond length (2.2207 Å) corresponds to a quadruple bond between the atoms. The [Re₂(HPO₄)₄ · 2H₂O]^2- complex anions in the crystal are associated through strong hydrogen bonds formed by the phosphate O-H···O groups. The stability of dirhenium(III) tetra-μ-phosphates in aqueous solutions is considered.     

新型磷酸钒孔道结构化合物(H3NCH2CH2NH3)3- [ (VO)4(PO4)2 (HPO4)4]的水热 合成及结构表征

以有机分子乙二胺作为模板剂合成了新型磷酸钒孔道化合物(H3NCH2CH2NH3)3^-[(VO)4(PO4)2(HPO4)4,并通过X射线单晶衍射实验进行了结构表征,晶体学数据为：C2/c,a=1.8505(9)nm,b=0.7089(4)nm,c=2.3304(10)nm,β=96.43(3)°,V-3.038(3)nm^3,Z=8,R=0.067,Rw^b=0.1635,该化合物具有非常独特和规整的二维孔道骨架结构,进一步的晶体化学研究表明该化合物为一新的VPO物相。