Investigation of Copper Halide:Hydrothermal Syntheses and Characterization of CuBr2(C12H8N2) and Cu3Br3(C12H8N2)2

The reaction of CuBr₂ with 1,10‐phen‐H₂O (1,10‐phen = 1,10‐phenanthroline) gave two compounds: CuBr₂(C₁₂H₈N₂) and Cu₃Br₃(C₁₂H₈N₂)₂. Their structures have been characterized by single‐crystal X‐ray diffraction analysis, elemental analyses, thermogravimetric analyses (TGA) and measurement of variable temperature magnetic susceptibility. Crystal data for CuBr₂(C₁₂‐H₈N₂): monoclinic, space group P2₁/n, a = 0.9977(3) nm, b = 0.65138(14) nm, c = 1.8207(4) nm, β = 91.624(18)°, V = 1.1828(5) nm³, Z = 2. Crystal data for Cu₃Br₃(C₁₂H₈N₂)₂: monoclinic, space group C2/c, a = 1.00167(11) nm, b = 1.4523(4) nm, c = 1.6295(3) nm, β = 94.386(14)°, V = 2.3635(8) nm³, Z = 3.     

{[Cu2Br3]n[Cu(H-Leof)2]·2H2O}(Leof是左氟沙星)

C om m ent Levofloxacin (S-(-)9-fluoro-2,3-dihydro-3-m ethyl- 10-(4-m ethyl-1-piperazinyl)-7-oxo-7H -pyrido[1,2,3-de]- 1,4-benzoxaxin-6-carboxilic acid)(Leof),is a synthetic fluorinated quinolone derivative, having activity a- gainstboth Gram ( )and Gram …     

金属配位聚合物[Mn2（C8H3NO6）2(C12H8N2)2]n的合成及其催化氧化性能

以5-硝基间苯二甲酸,1,10-邻菲啰啉,硫酸锰(MnSO4.H2O)为原料合成了一种结构新颖的金属配位聚合物——[Mn2(C8H3NO6)2(C12H8N2)2]n(1),其结构经IR,XRD,TG-DTG和元素分析表征。X-射线单晶衍射测试结果表明,1属三斜晶系,空间群Pī,晶胞参数a=10.060 2(1),b=14.343 5(2),c=14.663 7(2),α=104.052(1)°,β=102.633(1)°,γ=110.460(1)°,Mr=888.52,V=1 812.69(4)3,Z=2,Dc=1.628 g.cm-3,F(000)=900。以30%H2O2为氧化剂,初步研究了1在苯乙烯氧化反应中的催化氧化性能。     

Hydrothermal Synthesis and Characterization of a One-Dimensional Copper(I) Halide Cluster with 1,10-Phenanthroline

ＩｎｔｒｏｄｕｃｔｉｏｎＣｏｐｐｅｒ(Ｉ)ｈａｌｉｄｅｓｃａｎｆｏｒｍｏｌｉｇｏｍｅｒｉｃ (ｎｏｒｍａｌｌｙｄｉｍｅｒｓｏｒｔｅｔｒａｍｅｒｓ)ａｎｄｐｏｌｙｍｅｒｉｃｆｒａｍｅｗｏｒｋｓｔｈｅｍ ｓｅｌｖｅｓ .Ａｌｌｔｈｅｃｏｐｐｅｒ(Ｉ)ｈａｌｉｄｅｐｏｌｙｍｅｒｉｃｓｐｅｃｉｅｓａｒｅｂａｓｅｄｏｎｏｎｅ ｄｉｍｅｎｓｉｏｎａｌｃｈａｉｎｓ ,ｎｏｅｘａｍｐｌｅｓｏｆｔｗｏ ｄｉ ｍｅｎｓｉｏｎａｌｓｈｅｅｔｓｈａｖｅｂｅｅｎｆｏｕｎｄｓｏｆａｒ .Ｉｎｏｒｄｅｒｔｏｉｎ ｃｒｅａｓｅｔｈｅｄｉｍｅｎｓ…     

Hydrothermal Synthesis and Characterization of a One—Dimen—sional Copper（Ⅰ） Halide Cluster with 1,10—Phenanthroline

The title compound Cu₂Cl₂phen (phen = 1,10‐phenanthroline, C₁₂H₈N₂) 1 was synthesized from CuCl₂·2H₂O, CuCl and phen by hydrothermal method and its structure was determined by single crystal X‐ray analysis. With phen, CuG forms one‐dimensional chains, which comprise two zigzag chains based on fused Cu‐X units and connected via covalent bonds. The compound contains two crystallographically unique monovalent copper ions, Cu(1) and Cu(2). The Cu(1) atom in the tetrahedral site, is coordinated to two bridging Cl^? and two N atoms in phen. The Cu(2) atom with a slightly distorted triangular planar geometry, is coordinated to three Cl^?. The compound 1 was crystallized in monoclinic, space group P2₁/n with a = 0.37338(4), b = 1.9510(2), c = 1.68008(19) nm, β = 95.605 (3)°, R = 0.0458, and was characterized by elemental analysis, IR spectrum and TGA analysis.     

配合物[Cu2(C4H2O6)(Phen)2(H2O)]·8H2O的合成、晶体结构和抗菌活性

在pH≈10的乙醇-水溶液中以硫酸铜、酒石酸和邻菲咯啉反应合成了分子式为[Cu₂(C₄H₂O₆)(Phen)₂(H₂O)]·8H₂O的配合物单晶。用X-射线单晶衍射测定了晶体结构，并研究了配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌的抗菌活性。晶体属单斜晶系，空间群P2₁。标题化合物为双核铜配合物，2个铜原子配位数不同。Cu(1)是五配位的，具有扭曲的四方锥结构，5个配位原子分别是酒石酸的去质子的羟基氧和羧基氧、邻菲咯啉的2个氮原子及1个水分子的氧原子。Cu(2)为四配位的，配位原子分别是酒石酸的去质子的羟基氧和羧基氧和邻菲咯啉的2个氮原子。分子中Cu(1)…Cu(2)间的距离为0.354 8 nm。存在分子内邻菲咯啉-邻菲咯啉的面—面π-π相互作用，面间距为0.381 3 nm。配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌具有较强的抗菌活性。     

Hydrothermal Synthesis and Characterization Properties of C7H12N2[H2PO4]2.1/2H2O

An orthophosphoric hybrid material was successfully prepared by a hydrothermal reaction at 110 °C. A single crystal X-ray structure, thermal behavior, IR, and NMR spectroscopy investigations are given for a new organic cation bis dihydrogenomonophosphate C₇H₁₂N₂[H₂PO₄]₂.1/2H₂O. The latter has been synthesized hydrothermally using 2,4-diaminotoluene (DAT) and orthophosphoric acid. The atomic arrangement can be described as inorganic sheets alternating with inorganic-organic layers. The organic group C₇H₁₂N⁺ ₂ is located between inorganic groups to build multiple hydrogen bonds to ensure the three-dimensional cohesion network. The thermal behavior and IR, NMR and impedance spectroscopy studies are discussed for the powder samples of this compound.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Hydrothermal synthesis and crystal structure of a layered coordination polymer: [Zn2(C2O4)2(C3N2H4)2] n

A new metal-organic coordination polymer [Zn₂(C₂O₄)₂(C₃N₂H₄)₂] _n (1) has been hydrothermally synthesized with ZnCl₂·2H₂O, oxalic acid and imidazole. The compound has a 2D network, consisting of infinite zinc(II) oxalate chains connected to each other by three-coordinate oxygen atoms. Within the chains, the zinc atoms are each octahedrally coordinated by one nitrogen atom from imidazole and five oxygen atoms from oxalate groups. Furthermore, there are two coordination modes of oxalate to zinc ions: chelate bis-bidentate and chelate/bridging bis-bidentate in compound 1, and the latter is rare among related compounds. Crystal data: monoclinic, P2(1)/c, a?=?8.4310(17), b?=?9.4060(19), c?=?8.2790(17)?Å, β?=?93.15(3)°, V?=?655.5(2)?ų, Z?=?2, R ₁?=?0.0322, wR ₂?=?0.0850.     

Solid State Synthesis and Structural Characterization of Binuclear Cu(I)-SbPh3 Complex [Cu(SbPh3)2I]2

Dimeric complex [Cu(SbPh3)2I]2 has been synthesized by a solid state reaction at a low heating temperature and its crystal structure has been analyzed by X-ray crystallography. The crystal is monoclinic, space group P21/a (#14), a = 20.436(5), b=14.125(3), c=24.683(3)(A), β=110.67(1)°, Z=4, V=6666(2)(A)3; C72H60Sb4I2Cu2, Mr = 1792, Dc = 1.787 g.cm-3, μ(MoKα) = 31.88 cm-1, F(000)=3440, R=0.038 and Rw=0.043 for 5632 observed reflections (I≥3.0σ(I)) and 361 refined parameters. The result reveals the copper and the bridging iodide atoms form an approximately planar rhomboid array. Effects of the bulkiness of the ligands upon the structures of the analogous complexes are discussed.     

新型磷-钒-氧层状化合物[H2en]2[H3O]6[Co(H2O)2(VO)8(OH)4(PO4)8]的水热合成与晶体结构

金属磷酸盐材料在吸附、离子交换、离子传导和催化剂方面有潜在的应用前景[1～5]. 近年来, 通过水热反应合成了一些A-V-P-O化合物. 在这些化合物中, A一般为碱金属或有机阳离子, 如层状结构的[H2N(C4H8)2NH2][(VO)4(OH)4(PO4)2][6] 和[H2N(C2H4)3NH2][(VO)8(HPO4)3(PO4)4*(OH)2]*2H2O[6], 一维链状结构的 [H2NCH2CH2NH3(VO)(PO4)][7], 手性双螺旋结构的 [(CH3)2NH2]K4[(VO)10(H2O)2(OH)4(PO4)7]*H2O[8]以及具有三维骨架结构的化合物 [H3N(CH2)3NH3K(VO)3(PO4)3][9], [H3N(CH2)3NH3]2[V(H2O)2(VO)6(OH)2(HPO4)3(PO4)5]*3H2O[10]和[H3N(CH2)2NH3][(VO)3(H2O)2(PO4)2(HPO4)4][11].     

亚乙基硫脲配位聚合物[Cu3(etu)3 Br3]n的合成与晶体结构

CuB r2和亚乙基硫脲反应生成Cu(I)配位聚合物[Cu3(etu)3B r3]n(etu=亚乙基硫脲),单晶X射线衍射测得该晶体为三斜晶系,Pī空间群.晶胞参数:a=0.762 46(6)nm,b=1.198 48(10)nm,c=1.224 52(7)nm,α=68.202(5),°β=74.607(6),°γ=87.652(7)°,V=0.999 61(13)nm3,Z=2,Mr=736.82,Dc=2.448 g.cm-3,μ=9.477 mm-1,F(000)=708,偏差因子R1=0.030 6,wR2=0.071 0.配合物由环状[Cu(etu)B r]3单元聚合而成,形成Cu4S2B r2和Cu2S4B r2聚合体,两聚合体通过μ2-S桥键交替连接,形成平行于晶胞b轴的[Cu3(μ3-etu)(μ2-etu)2(μ2-B r)2B r]n一维链.Cu(I)均为变形四面体配位,亚乙基硫脲以S原子与Cu(I)结合,形成μ2-S和μ3-S两种配位方式.     

一价铜配合物〔Cu（C_8H_4F_3O_2S）（PPh_3）_2〕的合成和晶体

室温下，铜粉和２－噻吩甲酰三氟丙酮、三苯基膦在甲醇和四氢呋喃混合溶剂中反应，生成一价铜的配合物［Ｃｕ（Ｃ_８Ｈ_４Ｆ_３Ｏ_２Ｓ）（ＰＰｈ_３）_２］，测定了该配合物的晶体结构，结果表明，晶体属单斜晶系，Ｐ２_１／ｎ空间群，晶胞参数：ａ＝１０．５８４（１），ｂ＝１６．７３８（１），ｃ＝２２．７２８（９）Ａ；β＝９４．２２（２）°，Ｖ＝４０１５．２Ａ３，Ｍｒ＝７８５．２９，Ｚ＝４，Ｄｃ＝１０２９９ｇ／ｃｍ３，μ＝９．８６ｃｍ－１。晶体结构由直接法解出，使用块对角矩阵和全矩阵最小二乘法对原子参数进行修正，最后偏离因子Ｒ＝０．０４８，Ｒｗ＝０．０５４，其中４３９１个Ｉ＞３σ（Ｉ）的可观察衍射点参加了结构修正，结果表明，Ｃｕ原子由２个Ｏ原子和２个Ｐ原子配位，形成畸变四面体构型。     

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…     

Syntheses and Crystal Structures of Complexes [Cu(C14H8N3O4Br)](C4H9NO) and [Ni(C14H9N2O3Br)](C4H9NO)

The title compounds, Cu(L1)(C4H8NHO) and Ni(L2)(C4H8NHO) (H2L1 = 5-bro- mosalicylaldehyde-p-nitrobenzoylhydrazone, H2L2 = 5-bromosalicylaldehyde-p-hydroxybenzo- ylhydrazone), have been obtained and characterized by single-crystal X-ray diffraction. Complex 1 belongs to the triclinic system, space group P1 with a = 8.6960(2), b = 9.957(2), c = 11.878(2) , α = 73.36(3), β = 78.25(3), γ = 82.64(3)o, V = 962.1(3) 3, Mr = 512.81, Z = 2, F(000) = 514, Dc = 1.770 g/cm3, μ(MoKα) = 3.251, R = 0.0337 and wR = 0.0846. Complex 2 is of monoclinic, space group P21/c with a = 13.313(2), b = 8.2096(1), c = 21.890(3) , β = 125.737(3)o, V = 1941.9(4) 3, Mr = 478.97, Z = 4, F(000) = 968, Dc = 1.638 g/cm3, μ(MoKα) = 3.085, R = 0.0356 and wR = 0.0817. The ligands form a satisfactory N2O2 square plane around the metal centers in two compounds. Different patterns of hydrogen bonds are observed owing to the presence of different substituents on aromatic ring of the acylhydrazone Schiff bases. In complex 1, square-planar copper(II) complexes are linked by intermolecular hydrogen bonds leading to zigzag infinite chains. In complex 2, the metal complexes are linked via hydrogen bonds to form corrugated sheets in a staggered fashion; 3D channels along the b axis are constructed through other non-covalent interactions between the neighboring layers.     

Synthesis and Crystal Structure of [Cu (C_8H_4O_2F_3S) (2, 2' -bipy) ]

1INTRODUCTIONCoppercomplexesarewidelyusedascatalystsinthedecompositionofdisubsti-tutedperoxides"'-Theelectronicstructureandbondingatthecatalystscanbeprof-itablypursuedbystudyingmodelcomplexes.Generally,theCu(I)complexesareob-tainedbyreactionofCu(l)saltswithligands.Wereporthereamethodofpreparingcopper(I)complexbythereactionofCupowderwith2-thenoyltrifluoroacetone,2,2'-bipyinmethanol.2EXPERIMENTALReactionwascarriedoutundernitrogenatmosphere.2,2-bipy(1mmol)wasaddedtoamixtureof2-thenoyl…     

新型层状氟化磷酸铝[C4H12N2][Al2(PO4)2(H2O)2F2]的水热合成与表征

自从1982年Wilson等发现一类新型微孔材料磷酸铝分子筛(AlPO4-n)以来,大量具有新颖结构的磷酸铝化合物被合成出来,它们在催化、离子交换、吸附和主-客体组装等方面均具有潜在的应用前景,这类化合物大多是在水热或溶剂热体系中和有机模板剂存在条件下合成的,1978年,Flanigen等首先在反应体系中加入氟离子作矿化剂合成了硅晶体,后来,氟离子方法在硅铝体系和金属磷酸盐体系中也得到了广泛的应用,氟离子在反应过程中起到矿化剂或结构导向剂的作用,     

[C4N2H12]1.5[Zn2(PO4)(HPO4)2]·H2O晶体的合成与表征

由于在电学、磁学、光学、吸附、离子交换和催化等领域具有潜在的应用价值,具有开放骨架结构的金属磷酸盐的合成一直受到人们的广泛关注。在这些磷酸盐微孔化合物中,磷酸锌晶体是拓扑结构最为丰富的一种犤1犦。自从Stucky等犤2犦报道具有SOD、Li-ABW、FAU等已知结构磷酸锌的合成以来,已经有近百种具有0-D犤3,4犦,1-D犤5,6犦,2-D犤7～9犦,3-D犤10～13犦结构的磷酸锌被成功地合成出来。其中令人瞩目的是具有螺旋孔道的手性磷酸锌犤14犦以及具有二十四元环孔道的两种微孔磷酸锌化合物犤15,16犦的合成。这些化合物大多是采用水热技术以有…     

以哌嗪为模板剂的二维层状硫酸铈[C4N2H12]3[Ce2(SO4)6(H2O)2]·H2O的水热合成与晶体结构表征

以哌嗪为模板剂, 在水热条件下合成了一个新的具有二维拓展骨架结构的稀土硫酸盐[C4N2H12]3[Ce2(SO4)6(H2O)2]·H2O, 并对其进行了结构表征和热分析. 单晶结构解析结果表明, 该化合物晶体属于单斜晶系, P21/c空间群, 晶体学参数a=0.66335(10) nm, b=2.8088(4) nm, c=1.02212(15) nm, β=96.160(2)°, V=1.8935(5) nm3, R1=0.0466, wR2=0.1226. 该化合物由[—Ce—S3—Ce—S1—Ce— S3—Ce—S1—]八元环连接形成二维层状结构, 无机层间通过氢键连接成三维无限结构.     

配合物[Cu2(bpe)X2] n (bpe =1, 2–trans–(4–pyridyl)ethene, X=Cl, Br, I )的合成、晶体结构及热稳定性研究

以1,2-反式-二（4-吡啶基）乙烯桥连卤化铜分别得到配合物[Cu₂(bpe)Cl ₂] _n (1), [Cu₂(bpe)Br₂] _n (2) 和 [Cu₂(bpe)I₂] _n (3)。通过X-射线单晶衍射法对配合物1的结构进行了研究,晶体学数据：单斜晶系, P 2(1)/c空间群, a = 0.3788(8) nm, b = 1.5059(3) nm, c = 1.0875(2)nm, β = 96.262(4) °, V = 616.5(2)ų, Z = 2, S = 1.002,最终残差因子( I >2 σ ( I )) R ₁ = 0.0288, wR ₂ = 0.0579,对于全部数据 R ₁ = 0.0509, wR ₂ = 0.0615。元素分析及红外光谱分析表明,该类配合物为同晶化合物。另外,通过热重分析对配合物的热稳定性进行了研究。     

An Organically Templated Copper Pentaborate with Infinite Metallo-chains:[Cu(C3N2H4)4][Cu(CH3COO)2(C3N2H4)2(H2O)2][B5O6(OH)4]2

A novel organically templated copper pentaborate, [Cu(C₃N₂H₄)₄][Cu(CH₃COO)₂(C₃N₂H₄)₂(H₂O)₂]‐ [B₅O₆(OH)₄]₂, was synthesized by hydrothermal reaction and characterized by elemental analysis, single‐crystal X‐ray diffraction, FT‐IR spectroscopy, Raman spectroscopy and TGA. The crystal structure of this compound consists of two copper‐centered polyhedra and two discrete [B₅O₆(OH)₄]^? pentaborate anions, which are linked together through intensive hydrogen bonding interactions, forming a 3D framework with large channels along c axis. The discrete pentaborate anions form infinite layers by hydrogen bonds. Moreover, the two crystallographically different octahedral coppers are connected by common oxygen atom to form an infinite chain.