Synthesis and Crystal Structure of SrFe[BP2O8(OH)2]

SrFe[BP₂O₈(OH)₂] was synthesised under mild hydrothermal conditions. The crystal structure was determined from single–crystal X–ray diffraction data: triclinic, space group P (No. 2), a = 6.6704(12) Å, b = 6.6927(13) Å, c = 9.3891(19) Å, α = 109.829(5)°, β = 102.068(6)°, γ = 103.151(3)°, V = 364.74(12) ų and Z = 2. The crystal structure of SrFe[BP₂O₈(OH)₂] contains isolated borophosphate oligomers, [BP₂O₈(OH)₂]^5–, which are interconnected by Fe^IIIO₄(OH)₂ coordination octahedra. The resulting three–dimensional framework is characterised by elliptical channels running along [011]. Strontium takes positions inside the channels.     

Synthesis,Crystal Structure and Characterization of a new Protonated Magnesium Borophosphate: (H3O)Mg(H2O)2[BP2O8]·H2O

A new protonated borophosphate (H₃O)Mg(H₂O)₂[BP₂O₈]·H₂O ( 1 ) was synthesized under mild hydrothermal conditions and characterized by single‐crystal X‐ray diffraction, FTIR spectroscopy and TG‐DTA. The compound crystallizes in the hexagonal system, space group P6(1)22 (No 178), a = 9.4462(7) Å, c = 15.759(2) Å, V = 1217.8(2) Å³, and Z = 6. There exist infinite helical $^1_\infty$ {[BP₂O₈]^3–} ribbons built up from corner‐sharing PO₄ and BO₄ tetrahedra, which are connected by MgO₄(H₂O)₂ leading to an infinite three‐dimensional open‐framework. The H₃O⁺ ions are located at the free thread of the helical ribbons, whereas crystallized water occupy the channels of the helical ribbons. The dehydration of the compound occurs at a higher temperature which is presumably due to the anisotropic hydrogen bonds in the crystal structure. The luminescent properties of the compound were studied.     

Na1.89Ag0.11[BP2O7(OH)] und Na2[BP2O7(OH)] – Isotype Borophosphate mit Tetraeder-Schichtpaketen

Na_1.89Ag_0.11[BP₂O₇(OH)] and Na₂[BP₂O₇(OH)] – Isotypic Borophosphates Containing Layered Tetrahedral Blocks The isotypic borophosphates Na_1.89Ag_0.11[BP₂O₇(OH)] and Na₂[BP₂O₇(OH)] were grown under mild hydrothermal conditions (T = 165–170 °C). The crystal structures were solved by single crystal methods in the case of Na_1.89Ag_0.11[BP₂O₇(OH)] and by refinement of powder data (Rietveld method) for Na₂[BP₂O₇(OH)], respectively (orthorhombic, Pna2₁ (No. 33); a = 683.98(14)/682.36(1) pm, b = 2086.5(4)/2079.11(4) pm, c = 1318.9(3)/1314.46(3) pm; Z = 12). The compounds contain a complex two-dimensional structure consisting of layered tetrahedral blocks, which are formed by six- and eight-membered rings of tetrahedra. The Na⁺/Ag⁺-ions are located inside and near the surface of the ‘layer blocks' and are five-, six- and sevenfold coordinated by oxygen.     

[Co(phen)3]2[PMo12O40](OH)的水热合成及晶体结构

利用水热合成法制备了Keggin结构阴离子有机一无机复合物[Co（phen）3]2[PMo12O40]（OH）,通过元素分析,红外光谱和X射线单晶衍射等对其进行了表征．结果表明,该化合物属于单斜晶系,C2／c空间群．=1．97225（18）nm,b=1．81079（16）nm,c=2．5117（2）nm,β=100．5380（10）°,V=8．819O（14）nm^3,Z=4,R1=0．0587,wR2=0．1211．该化合物分子由一个多阴离子[PMo12O40]^3-,两个[Co（phen）3]^2＋及一个羟基组成．     

Co(en)3[B4O5(OH)4]Cl·3H2O和[Ni(en)3][B5O6(OH)4]2·2H2O的合成、结构以及热力学性质

利用水热法合成了两种过渡金属配合物为模板剂的含水硼酸盐晶体Co(en)3[B4O5(OH)4]Cl·3H2O(1) 和 [Ni(en)3][B5O6(OH)4]2·2H2O (2),并通过元素分析、X射线单晶衍射、红外光谱及热重分析对其进行了表征。化合物1晶体结构的主要特点是在所有组成Co(en)33+, [B4O5(OH)4]2–, Cl– 和 H2O之间通过O–H…O、O–H…Cl、N–H…Cl和N–H…O四种氢键连接形成网状超分子结构。化合物2晶体结构的特点是[B5O6(OH)4]–阴离子通过O–H…O氢键连接形成沿a方向有较大通道的三维超分子骨架,模板剂[Ni(en)3]2+阳离子和结晶水分子填充在通道中。     

一维链状高价锰配合物[Mn_2(C_7H_4O_3)_4(CH_3OH)_2]·4H_2O_2CH_3OH的合成与结构

合成了一维链状高价锰配合物[Mn2(C7H4O3)4(CH3OH)2]4H2O2CH3OH,并对其进行了IR、X-射线衍射、UV-Vis和TG-DSC等表征。单晶衍射结果表明,该配合物晶体属三斜晶型,空间群P?晶胞参数a=7.653(5),b=10.486(7),c=12.943(8),=103.24(1),?=104.55(1),?=110.11(1),V=885.4(9)3,Z=1。UV-Vis光谱在547nm有一个吸收峰,相应于Mn(Ⅳ)的d-d电子跃迁光谱。     

Synthesis,Crystal Structure of a New Structure Type,and Thermal Analysis of the Ammonium Borophosphate (NH4)2[B2P3O11(OH)]

(NH₄)₂[B₂P₃O₁₁(OH)] was synthesized as a crystalline colorless powder by reaction of (NH₄)₂HPO₄, H₃BO₃, and H₃PO₄ under hydrothermal conditions at 180 °C. According to X‐ray single‐crystal investigations (NH₄)₂[B₂P₃O₁₁(OH)] crystallizes in a new structure type in the orthorhombic space group P2₁2₁2₁ (no. 19) [Z = 4, a = 4.509(3), b = 14.490(11), c = 16.401(12) Å, R₁ = 0.046, wR₂ = 0.093, 1682 data, 200 parameters]. The crystal structure comprises infinite layers of corner‐sharing borate, phosphate and hydroxo‐phosphate tetrahedra with ammonium ions in‐between. The loop‐Branched (lB) zweier‐single layer reveals an open‐Branched (oB) vierer‐single ring as fundamental building unit (FBU), which was observed in (NH₄)₂Mn^II[B₂P₃O₁₁(OH)₂]Cl^[1] for the first time. Besides the spectroscopic properties the thermal behavior is presented as well.     

Synthesis and Crystal Structure of [C10N2H10]2[P2Mo5O21(OH)2]·2H2O

The crystal structure of [C₁₀N₂H₁₀]₂[P₂Mo₅O₂₁(OH)₂] · 2H₂O, contains the heteropolyanion, [P₂Mo₅O₂₁(OH)₂]^4—, together with diprotonated 4, 4′‐bipyridine. The heteropolyanion is built up from five MoO₆ octahedra sharing four common edges and one common corner, capped by two PO₃(OH) tetrahedra. The structure is stabilized by hydrogen bonds involving the hydrogen atoms of the 4, 4′‐bipyridine, water molecules and the oxygen atoms of the pentamolybdatobisphosphate. This is the first example that this kind of cluster could be isolated in the presence of a poly‐functional aromatic molecule ion. Crystal data: triclinic, P1¯ (No. 2), a = 9.983(2)Å, b = 11.269(2)Å, c = 17.604(4)Å, α = 73.50(3)°, β = 84.07(3)°, γ = 67.96(3)°; V = 1760.0(6)ų; Z = 2; R₁ = 0.037 and wR₂ = 0.081, for 9138 reflections [I > 2σ(I)].     

[Nd(4-PYA)_3(H_2O)_2]_n的合成及其晶体结构

3-(4-吡啶基)丙烯酸(4-HPYA)和Nd(NO3)3通过水热法合成了一种新的一维链状配位聚合物[Nd(4-PYA)3(H2O)2]n(1),其结构经IR,元素分析和X-射线单晶衍射表征。1属三斜晶系,P-1空间群,晶胞参数:a=0.829 23(13)nm,b=1.272 60(2)nm,c=1.435 00(12)nm,α=112.371(2)°,β=98.856(3)°,γ=100.239(2)°,V=1.336 6(3)nm3,Mr=660.72,Z=2,Dc=1.642 g.cm-3,F(000)=662,μ=2.002mm-1,R1=0.052 3,wR2=0.141 9。1通过分子间氢键作用将一维链紧密堆积成三维网状结构。     

Structural Patterns and Dimensionality in Magnesium Borophosphates: The Crystal Structures of Mg2(H2O)[BP3O9(OH)4] and Mg(H2O)2[B2P2O8(OH)2]·H2O

Hydrothermal investigations in the system MgO/B₂O₃/P₂O₅(/H₂O) yielded two new magnesium borophosphates, Mg₂(H₂O)[BP₃O₉(OH)₄] and Mg(H₂O)₂[B₂P₂O₈(OH)₂]·H₂O. The crystal structures were solved by means of single crystal X‐ray diffraction. While the acentric crystal structure of Mg₂(H₂O)[BP₃O₉(OH)₄] (orthorhombic, P2₁2₁2₁ (No. 19), a = 709.44(5) pm, b = 859.70(4) pm, c = 1635.1(1) pm, V = 997.3(3) × 10⁶ pm³, Z = 4) contains 1D infinite chains of magnesium coordination octahedra interconnected by a borophosphate tetramer, Mg(H₂O)₂[B₂P₂O₈(OH)₂]·H₂O (monoclinic, P2₁/c (No. 14), a = 776.04(5) pm, b = 1464.26(9) pm, c = 824.10(4) pm, β = 90.25(1)°, V = 936.44(9) × 10⁶ pm³,Z = 4) represents the first layered borophosphate with 6³ net topology. The structures are discussed and classified in terms of structural systematics.     

钴的二膦酸配合物[ Co(en) 3 ] [ Co2 (Hedbbp) 2 ]· 7H2O的合成与晶体结构

水热条件下合成了一个新的有机二膦酸钴配合物[Co(en)3][Co2(Hedbbp)2]·7H2O,[H4edbbp=N,N'-二(苄基膦酸)乙二胺].X射线单晶衍射结构分析表明配合物属三斜晶系,空间群P-1,晶胞参数a=1.505.6(3)nm,b=1.524 8(3)nm,c=1.649 7(3)nm,α=63.10(3)°,β=78.12(3)°,γ=75.62(3)°,晶胞 体积为V=3.2524(11)nm3,Z=2.配合物结构单元中包含一个二膦酸钴的二聚单元阴离子[Co2(Hedbbp)2]2-和一个三乙二胺合钴螯合阳离子单元[Co(en)3]2+和七个水分子.     

Synthesis,Crystal Structure,and Characterization of a New Metal Borophosphate: PbII4{Co2[B(OH)2P2O8](PO4)2}Cl

A new metal borophosphate Pb^II₄{Co₂[B(OH)₂P₂O₈](PO₄)₂}Cl ( 1 ), containing both Pb²⁺ cations and Cl^– anions, was hydrothermally synthesized and characterized by powder X‐ray diffraction, ICP, TG/DTA, and FTIR spectroscopic analyses. The crystal structure determination from single‐crystal X‐ray diffraction reveals that compound 1 crystallizes in the trigonal space group R c (No. 167), a = 9.7513(7) Å, c = 91.060(13) Å, V = 7498.7(13) Å³ and Z = 18. Its structure features a new cobalt borophosphate layer {Co₂[B(OH)₂P₂O₈](PO₄)₂}^7– built up from CoO₅ square pyramids, [B(OH)₂P₂O₈]^5– borophosphate trimers and PO₄ tetrahedra. Extra‐framework Pb²⁺ and Cl^– ions are located at the vacancy of layers to achieve the charge neutrality of the framework. Magnetic measurements indicate that antiferromagnetic interactions exist between Co²⁺ ions with a negative Weiss constant of –20.3 K.     

Hydrothermal Synthesis and Characterization of Nb3O7(OH)

Triniobium hydroxide heptaoxide, Nb₃O₇(OH), was prepared hydrothermally by treating niobic acid or triniobium chloride heptaoxide with 3.0 mol/dm³ sulfuric acid at 250–350°C and 15 MPa. The hydroxide oxide was isomorphous with the low-pressure form of triniobium fluoride heptaoxide which is built up of 3 X ∞ blocks of the ReO₃ structure with crystallographic shear in one dimension. When heated in air, Nb₃O₇(OH) dehydrated up to 460°C to give poorly crystallized Nb₂O₅, which, on further heating, changed slowly into a less ordered precursor of M? Nb₂O₅(¹). Hydrothermal treatment of Nb₃O₇(OH) with pure water at 400–500°C afforded P? and R? Nb₂O₅; the conversion of Nb₃O₇(OH) is explained in terms of the close structural relation among these three forms.     

配合物Nd(C7H7N2O2)3(H2O)3的合成及其晶体结构

用水热法合成了3,5-二氨基苯甲酸与Nd(Ⅲ)的配合物Nd(C7H7N2O2)3(H2O)3(1),其结构经IR,元素分析和X-射线单晶衍射仪表征。1为单核结构,属六方晶系,R3空间群,晶胞参数:a=1.887 29(18)nm,b=1.887 29(18)nm,c=0.603 53(12)nm,β=90,°γ=120°,V=1.861 7(4)nm3,Z=3,μ=2.154 mm-1,Dc=1.744 g.cm-3,R1=0.014 3,wR2=0.033 2。1中Nd(Ⅲ)与来自3个3,5-二氨基苯甲酸的6个氧原子及3个配位水的氧原子进行配位,形成9配位化合物。     

[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构

氯化钆;甘氨酸;固态配合物;[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构     

NaSc3[HPO3]2[HPO2(OH)]6: Synthesis,Crystal Structure,and Thermal Decomposition

NaSc₃[HPO₃]₂[HPO₂(OH)]₆ was prepared by use of a phosphorus acid flux route. The crystal structure was determined from single‐crystal X‐ray diffraction data: triclinic, space group P$\bar{1}$ (No. 2), a = 7.4507(11) Å, b = 9.6253(17) Å, c = 9.6141(16) Å, α = 115.798(4)°, β = 101.395(4)°, γ = 101.136(3)°, V = 577.29(16) Å³ and Z = 1. The crystal structure of NaSc₃[HPO₃]₂[HPO₂(OH)]₆ contains two kinds of phosphate(III) groups: HPO₃^2– and HPO₂(OH)^–. Phosphate(III)‐tetrahedra, NaO₆ and ScO₆ octahedra together form a (3,6)‐connected net. During heating hydrogen and water are released and Sc[PO₃]₃ is formed as the main crystalline decomposition product.     

[Ni(C13H10O2N3)2]2·CH3OH配合物的合成、晶体结构及其电化学性质

合成了含吡啶甲醛缩水杨酰腙(HL)的镍配合物[(NiL2)2·CH3OH(1,L=C13H10O2N3],其结构经X-射线单晶衍射,IR和元素分析表征.1属于单斜晶系,P2(1)/n空间群,晶胞参数a=12.458(2)A,b=17.920(3)A,c=13.885(8)A,β=119.923(10)°,V=2 686.70(7)A3,Z=2,Mr=710.73,Dc=1.368 Mg·m3,μ=0.767 mm1,F(000)=1 140,R=0.060 3,wR=0.161 1.中心Ni(Ⅱ)与两个HL中的两个亚氨基氮、两个吡啶氮及两个羰基氧配位,形成了六配位的八面体构型.其中甲醛缩水杨酰腙三啮配体以负一价的阴离子形式存在.对1的电化学性质进行了讨论.