Structure of Palladium( Ⅱ ) Complex with 2-Hydroxy-propane 1, 3-diamine-N,N,N'''' N'''',-tetraacetic Acid

The reaction of PdCl2 in water with 2-hydroxypropane-1, 3-diaminetetraacetic acid (HPDTA) gave the complex Pd (C11H16N2O9)·1. 5H2O, which was characterized by elemental analysis, IR, NMR and single-crystal X-ray diffraction. The spectroscopic and X-ray diffraction data show that Pd ( Ⅱ ) is coordinated by two nitrogen atoms and two car-boxylic oxygen atoms. The complex crystallizes in monoclinic space group Pc with a = 1. 1240(2), b=1. 1183(2), c=1. 2597(3) nm, β=96. 33(2)°V=1. 5737(6) nm3, Z = 4, R= 0.038. The structure contains two crystallographically independent molecules which have slightly different orientations and are connected by hydrogen bonds.     

A Y(Ⅲ)-organic Coordination Polymer Constructed from 2-(Pyridine-4-yl)-1H-imidazole-4,5-dicarboxylate and Oxalate Ligands: Structure and Luminescent Property

A novel compound, {[Y(HPIDC)(OX)1/2(H2O)]·2H2O}n (1, H3PIDC = 2-(pyridin-4- yl)-1H-imidazole-4,5-dicarboxylic acid, H2OX = oxalic acid), has been synthesized under hydrothermal conditions and characterized by thermal analysis (TGA), powder X-ray diffraction (PXRD), and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic space group P21/c with a = 8.342(8), b = 14.61(1), c = 11.487(1), β = 90.78(9)°, V = 1400.4(2)3, Z = 4, C11H11N3O9Y, Mr = 418.14, Dc = 1.983 g/cm3, F(000) = 836, Rint = 0.0509, T = 293(2) K, μ = 4.240 mm-1, the final R = 0.0477 and wR = 0.1125 for 2770 observed reflections with I > 2σ(I). Compound 1 exhibits a 3D framework and generates the 1D open channels filled with free water molecules. The structure of 1 can be rationalized as a diamondoid network when the atom yttrium is regarded as a 4-connected node linking four surrounding yttrium atoms. The luminescent property of compound 1 is also investigated.     

Synthesis and Crystal Structure of a New Iron Complex with Cyclic Water Hexamers [Fe(CDTA)(H_2O)]·[Fe(1,10-phen)_3]·10H_2O·2OH

The title complex [Fe(CDTA)(H2O)]·[Fe(1,10-phen)3]·10H2O·2OH (CDTA = transcyclohexane-1,2-diamine-N,N,N,N′-tetraacetate) has been prepared and characterized by single-crystal X-ray diffraction analysis. The crystal adopts space group P with a = 12.793(4), b = 14.104(5), c = 17.880(5), V = 2792.2(1)3, Dc = 1.459 g/cm3, C50H66Fe2N8O21, Mr = 1226.81, F(000) = 1284, μ = 0.604 mm-1, Z = 2, R = 0.1055 and wR = 0.2581 for 8675 observed reflections (I > 2σ(I)). X-ray crystallography analysis exhibits that the title compound consists of two crystallographically independent molecules [Fe(CDTA)(H2O)] and [Fe(1,10-phen)3], and they are connected through O-H···O hydrogen bonds and π···π stacking interactions forming a 3D supramolecular structure. Interestingly, there is a cyclic water hexamer with chair conformation in this complex.     

Synthesis and Crystal Structure of a Co(Ⅱ) Complex with Taurine-5-methyl-2-hydroxyisophthalaldehyde Schiff Bases [Co(C_(13)H_(16)N_2O_7S_2)(H_2O)_3]_2·H_2O

The title complex CoL(H2O)32·H2O(C26H46N4O21S4Co2),where L = taurine-5-methyl-2-hydroxyisophthalaldehydes,has been synthesized and characterized by IR and X-ray diffraction analysis.The crystal of the complex belongs to the triclinic system,space group P1,with a = 11.197(4),b = 13.309(5),c = 14.486(5),α = 78.827(13),β = 70.547(11),γ = 81.058(13)°,Mr = 996.77,S = 1.08,V = 1987.2(13)3,Z = 2,Dc = 1.666 g/cm3,F(000)= 1032,μ = 1.131 mm?1,R = 0.0633 and wR = 0.1293.According to the structural analysis,the Co(Ⅱ)ion adopts a slightly distorted six-coordinated octahedral geometry.One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom.Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds,thus generating an infinite chain constructed by hydrogen bonds.     

Syntheses and Crystal Structures of Two Cadmium(Ⅱ) Compounds Linked by N,N-Bis(3-pyridylmethyl)amine

Two cadmium(Ⅱ) compounds linked by a flexible dipyridyl ligand {[Cd2(Hbpma) Cl5(H2O)]·2H2O}n 1 and [Cd(Hbpma)Cl(H2O)2]2·2SO4·3H2O 2 (bpma = N,N-bis(3-pyridylmethyl)amine) have been synthesized and structurally characterized by single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic, space group P with a = 9.5612(6), b = 11.3401(7), c = 11.5069(12), α = 112.8540(10), β = 106.5330(10), γ = 101.6680(10)°, V = 1030.77(14)3, C12H20Cd2Cl5N3O3, Mr = 656.36, Z = 2, Dc = 2.115 g/cm3, μ(MoKα) = 2.727 mm-1, F(000) = 636, S = 1.059, the final R = 0.0319 and wR = 0.0822 for 3443 observed reflections (I > 2σ(I)). For complex 2, it belongs to triclinic, space group P with a = 10.9487(4), b = 11.4197(4), c = 15.4288(5), α = 94.7470(10), β = 104.1000(10), γ = 104.42°, V = 1790.76(11)3, C24H42Cd2Cl2N6O15S2, Mr = 1014.46, Z = 2, Dc = 1.881 g/cm3, μ(MoKα) = 1.529 mm-1, F(000) = 1020, S = 1.050, the final R = 0.0178 and wR = 0.0451 for 6026 observed reflections (I > 2σ(I)). Complex 1 is found to have tetranuclear Cd(Ⅱ) clusters which are bridged by the protonated bpma ligands leading to one-dimensional coordination polymers, whereas complex 2 consists of binuclear Cd(Ⅱ) structures linked by the protonated bpma ligands. Both complexes are assembled into three-dimensional supramolecular structures through hydrogen bonding interactions.     

Synthesis and Crystal Structure of a New Zn(Ⅱ) Coordination Polymer Constructed by 1,2,4,5-Benzenetetracarboxylate

A new Zn(Ⅱ) coordination polymer [Zn3(btec)(OH)2(H2O)2]n (1, btec = 1,2,4,5- benzenetetracarboxylate) has been synthesized by hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in mono- clinic, space group C2/c, with a = 19.580(3), b = 5.0137(8), c = 15.975(3), β = 121.629(2)°, V = 1335.3(4)3, C10H8O12Zn3, Mr = 516.27, Z = 4, Dc = 2.568g/cm3, μ = 5.419 mm-1, F(000) = 1016, R = 0.0590 and Rw = 0.1279 for 1110 observed reflections (I > 2σ(I)). X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn(Ⅱ) atoms which are connected through the bridging carboxylate oxygen atoms of the btec ligands and μ2-bridging oxygen atoms of water molecules to generate an infinite one-dimensional chain. The adjacent chains are linked together through the benzene rings of the btec ligands to form a two-dimensional polymeric network. The adjacent two-dimensional layers are further connected together by the benzene rings of btec ligands to give the final three-dimensional structure. The benzene rings act as pillars between two layers.     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H_2O)_3}·2H_2O]_n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc = 5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 9.599(3), b = 18.699(5), c = 7.557(2) , β = 108.198(4)°, V = 1288.6(6) 3, Z = 4, Mr = 382.60, Dc = 1.972 g/cm3, F(000) = 760, μ = 1.740, the final R = 0.0555 and wR = 0.0995 for 1732 observed reflections with I > 2σ(I). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.     

Synthesis, Structure and Luminescent Properties of a New Terbium（Ⅲ） Complex with 5-Bromoisophthalic Acid

The self-assembly of 5-bromoisophthalic acid (H2BIPA) with Tb(NO3)3·6H2O under hydrothermal conditions gives rise to a 3D coordination polymer, [Tb2(BIPA)3(CH3CH2OH)]n (1), which was characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a = 19.2591(17), b = 8.2537(7), c = 18.5663(17), β = 104.4720(10)°, V = 2857.6(4)3, C26H15Br3O13Tb2, Mr = 1092.95, Dc = 2.540 g/cm3, F(000) = 2040, μ = 9.173 mm-1 and Z = 4. The final R = 0.0324 and wR = 0.0767 for 5299 observed reflections (I > 2σ(I)). Complex 1 displays an unusual three-dimensional (4,6)-connected network with (48.66.8)2(44.62)2(42.84) topology, which is different from [Tb(HBDC)(BDC)(H2O)4]·3.3H2O (BDC = isophthalate) because the -Br substituent of isophthalate results in different electronic effect and steric hindrance to change the coordination modes of carboxylate groups in the assembly process. Moreover, luminescent properties of 1 have also been investigated in the solid state.     

Synthesis, Structure, and Magnetic Properties of One Polyoxometalate (W/Mo) Compound: H_8K{[Ni(H_2O)_5]_2(H_2Mo_(1.80)W_(10.20)O_(42))}Cl_3·16H_2O

One new polyoxometalate compound connected via nickel/potassium cations, H8K{[Ni(H2O)5]2(H2Mo1.80W10.20O42)}Cl3·16H2O 1, was prepared and characterized by elemental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis results reveal that clusters of [Ni(H2O)5]2(H2Mo1.80W10.20O42)}6-in compound 1 are linked by potassium cations to form one- dimiensional chains, based on which a three-dimensional network is further constructed via the hydrogen bonds of O…O and O…Cl. Magnetic measurements show that compound 1 has para- magnetic properties. Crystal data: H62Cl3KMo1.80Ni2O68W10.20, Mr = 3461.33, monoclinic, space group C2/c, a = 18.9291(19), b = 16.6758(17), c = 19.1064(19), β = 106.6880(10)°, V = 5777.1(10)3, Z = 4, Dc = 3.980 g/cm3, F(000) = 6250, μ = 21.574 mm?1, R = 0.0579 and wR = 0.1623 (I > 2σ(I)).     

Synthesis and Crystal Structure of 2-(4-Nitrophenyl)-1,2-benzisoselenazol-3(2H)-one DMF (1:1) Solvate

The title compound (C13H8N2O3Se-C3H7NO) has been synthesized by a simple synthetic route and by recrystallization from DMF. The molecular structure of this compound was obtained by single-crystal X-ray diffraction. The compound crystallized in the triclinic space group P with a = 7.450(6), b = 8.150(7), c = 13.859(12) , α = 75.014(14), β = 83.072(18), γ = 84.409(14)°, V = 805.0(12)3, Z = 2 and R = 0.0271 for 2575 observed reflections with I > 2σ(I). X-ray analysis reveals that not only intermolecular Se…O and C-H…O interactions, but also π…π stacking interactions exist in the adjacent molecules. The above three kinds of intermolecular interactions extend the complex into an infinite three-dimensional layered network.     

Hydrothermal Synthesis and Structure of One New Polyoxotungsate [Ni(trien)]_4[Ni_4(H_2O)_2(HPW_9O_(34))_2]·4H_2O

One new sandwich-type tetra-nickel substituted polyoxotungsate,[Ni(trien)]4-[Ni4(H2O)2(HPW9O34)2]·4H2O(1,trien=triethylenetetramine),has been hydrothermally synthesized and characterized by IR,elemental analysis,TGA,and single-crystal X-ray diffraction analysis.Crystal data for 1:triclinic,space group P with a=13.279(3),b=13.816(3),c=14.494(4),α=95.403(1),β=113.173(4),γ=93.809(3)o,V=2418.0(10)3,Z=1 and Dc=3.861 g/cm3.X-ray crystallographic study shows that compound 1 is a relatively rare inorganic-organic hybrid polyoxo tungstate constructed from sandwich Ni-substituted polyoxo-anions and nickel complexes.     

Synthesis and Crystal Structure of 5,5-Dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexene-1-one

The title compound 5,5-dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexen-1-one has been synthesized,and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic,space group P21/c with a=9.4193(13),b=26.915(4),c=21.188(3),β =101.906(3)°,V =5256.2(13)3,Z =4,C60H68Cl2N2O8,Mr=1016.06,Dc=1.284 g/cm3,F(000)=2160,λ(MoKα)=0.71073,μ=0.182 mm–1,R=0.0530 and wR=0.1131 for 4128 observed reflections (I>2σ(I)). X-ray analysis reveals that there are two independent molecules in the unit and the cyclohexenone rings adopt different conformations. In addition,there are four intramolecular hydrogen bonds in the title molecule.     

Synthesis and Structural Characterization of One New Polyoxotungstate Connected via Potassium Cations with aThree-dimensional Framework: H_6Na_2K_4(H_2W_(12)O_(42))Cl_2·14H_2O

One new polyoxotungstate complex H_6Na_2K_4(H_2W_(12)O_(42))Cl_2·14H_2O 1 has been prepared in the beaker solution and characterized by elemental analysis and IR spectroscopy. Crystal data: H36Cl2K4W12Na2O56, Mr = 3411.77, monoclinic, space group P21/c, a = 11.5734(16), b = 14.3136(19), c = 15.459(2) , β = 105.601(2)°, V = 2466.5(6)3, Z = 2, Dc = 4.594 g/cm3, F(000) = 3008, μ = 28.447 mm-1, R = 0.0574 and wR = 0.1239 (I > 2σ(I)). Single-crystal X-ray diffraction analysis results reveal that a three-dimensional architecture in the title compound is constructed from the H2W12O4210- units linked by potassium.     

Synthesis and Structure of a La(Ⅲ) Complex of 1,10-Phenanthroline-2,9-dicarboxylate:a Three-dimensional Network via Hydrogen Bonding Interactions

A new La(Ⅲ) complex, {[La(L)(NO3)(H2O)3]·H2O}n (L = 1,10-phenanthroline- 2,9-dicarboxylate), has been synthesized and structurally determined by X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P21/c with a = 7.7358(17), b = 8.1664(18), c = 28.271(6) , β = 95.184(4)°, V = 1778.6(7)3, Z = 4, C14H14LaN3O11, Mr = 539.19, Dc = 2.014 g/cm3, μ = 2.471 mm–1, F(000) = 1056, the final R = 0.0350 and wR = 0.0659. In this complex, each metal center adopts a ten-coordination geometry formed by two N atoms from a ligand L and eight O atoms from three H2O molecules, a nitrate ion and carboxylates of two ligands. Each ligand adopts a N2,O3-pentdentate coordination mode using two N and two O atoms chelating a La(III), and using another O atom of carboxylate to bridge another La(III) center resulting in a 1D helical chain molecule. Intermolecular strong O–H···O and weak C–H···O hydrogen bonds extend the 1D chain structure into a 3D supramolecular architecture.     

Syntheses, Crystal Structures and Antibacterial Activities of Copper（Ⅱ） and Zinc（Ⅱ） Complexes Based on （E）-4-fluoro-2-（（3-morpholinopropylimino）methyl）phenol

Two Schiff base complexes [Cu(L)2] (1) and [Zn(L)2]·3H2O(2) of (E)-4-fluoro-2-((3-morpholino propylimino)methyl)phenol (HL) have been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. Crystal data for 1: triclinic, space group Pī with a=4.8000(10), b=11.109(2), c=13.921(3),α=66.55(3),β=80.35(3),γ=81.09(3)°, V=668.2(2)3 , Z=1, Dc=1.477g/cm 3 , F(000)=311, and the final R=0.0744 and wR=0.1601 for 2301 observed reflections with I > 2σ(I). And those for 2: monoclinic, space group P21 /c with a=14.789(3), b=11.713(2), c=18.846(4),β=107.85(3)°, V=3107.4(11)3 , Z=4, D c=1.389 g/cm 3 , F(000)=1368, and the final R=0.0749 and wR=0.1348 for 5423 observed reflections with I > 2σ(I). Both 1 and 2 are four-coordinated complexes, with a square-planar geometry of copper(Ⅱ) in 1 and a slightly distorted tetrahedral geometry of zinc(Ⅱ) in 2. An asymmetric unit consists of only one half of a Cu ion and one L ligand in 1, while an asymmetric unit is composed of one Zn ion, two L ligands and three water molecules in 2. Non-classical C-H···O and C-H F hydrogen bonds play important roles in the formation of a 1D chain of 1, but O-H O and O-H N hydrogen bonds play dominant roles in the self-assembly of a 3D network of 2. The antibacterial activities of 1 and 2 against B. subtilis, S. aureus, S. faecalis, P. aeruginosa, E. coli and E. cloacae have been evaluated by MTT method.     

Synthesis,Crystal Structure and Magnetic Properties of a Co(Ⅱ) Complex Containing 2′-(l′-Methyl)benzimidazolyl-substituted Nitronyl Nitroxide

A new complex [Co(NIT-1′-MeBzIm)2Cl2](NIT-1′-MeBzIm = 2-{2′-[(l′-methyl)-benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method.The complex crystallizes in the monoclinic system,space group C2/c,Z = 4.Crystal data:C30H38Cl2CoN8O4,Mr = 704.51,a = 17.074(3),b = 21.350(3),c = 11.6962(19),β = 108.879(2)°,V = 4034.3(11)3,Dc = 1.160 g/cm3,μ(MoKα) = 0.597 mm-1,F(000) = 1468,R = 0.0422 and wR = 0.1141 for 2577 observed reflections with I > 2σ(I).X-ray analysis reveals that the Co(Ⅱ) ion is six-coordinated with a distorted octahedral geometry.Temperature dependence of susceptibility measurements shows the existence of antiferromagnetic interactions between the Co(Ⅱ) ion and the radicals(J =-52.88 cm-1).     

Syntheses and Crystal Structures of Two Supramolecular Architectures:(H_2tfbdc)·(tfbdc)·(Hbipy)_2 and (tfbdc)·(H_2pz)(tfbdc=Tetrafluoroterephthalate,bipy=4,4'-Bipyridine,pz=Pyrazine)

Two new supramolecular compounds,2C 10 H 9 N 2 + ·C 8 HF 4 O 4 2-·C 8 H 2 F 4 O 4 /(H 2 tfbdc)· (tfbdc)·(Hbipy) 2 (1) and C 4 H 6 N 2 2+ ·C 8 HF 4 O 4 2-/(tfbdc)·(H 2 pz) (2),were synthesized and characterized by elemental analysis,IR spectra,and single-crystal X-ray diffraction.Compound 1 crystallizes in the triclinic system,space group P1,with a=8.3453(12),b=10.1798(15),c=10.6626(16),α=87.591(2),β=74.047(2),γ=69.006(2)°,V=834.53(12) 3,D c=1.614 g/cm 3,F(000)=400,u=1.45 cm-1,Z=2,the final R=0.0353 and wR=0.1005 for 5882 observed reflections with I > 2σ(I);and compound 2 crystallizes in the monoclinic system,space group P2 1 /c,with a=10.471(4),b=5.4419(19),c=12.249(4),β=114.909(6)°,V=633(4)3,D c=1.669 g/cm 3,F(000)=320,u=1.63 cm-1,Z=2,the final R=0.0794 and wR=0.2923 for 3213 observed reflections with I > 2σ(I).Both compounds 1 and 2 crystallize as charge-transfer organic salts with the dianionic or neutral acid components lying at the inversion centers.Hbipy + cations and anionic acid in compound 1 are linked to form a chain by means of C-H···O hydrogen bonds.Adjacent chains are further extended into a two-dimensional layer network via N-H···O and O-H···N hydrogen bonds.In compound 2,the acid and base subunits are arranged alternately to generate a linear tape motif via N-H O hydrogen bonds;these tapes are further combined into a three-dimensional array with CdSO 4 topology via C-H O intermolecular hydrogen bonds.     

Simple Preparation,Structure and Conductivity of Nickel(Ⅱ) Benzenetricarboxylate Ni_3(BTC)_2·12H_2O

Proton-conductive crystalline metal-organic framework nickel(Ⅱ) benzenetricarboxylate Ni3(BTC)2·12H2O(MOF-Ni) was prepared by the reaction of nickel(Ⅱ) nitrate and 1,3,5-benzenetricarboxylic(BTC) acid in a mixed solvent of N,N-dimethylformamide(DMF)/C2H5OH/ H2O(1:1:1, ν/ν) at low temperature and short reaction time. It was characterized by thermogravimetric analyses(TG), FT-IR and N2 adsorption-desorption. Single-crystal X-ray diffraction analysis indicated that the complex belongs to monoclinic system, space group C2 with a = 17.407(6), b = 12.878(5), c = 6.542(2) , β = 112.07°, V = 1359.0(8)3, Dc = 1.971 g/cm3, μ = 2.166 mm-1 and Z = 2. Linear polarization resistance(LPR) analysis showed that the complex possesses semiconducting properties.     

Synthesis and Crystal Structure of Picrates of 3,5-Diamino-1,2,4-triazole

The title compound C2N5H6+C6N3O7H2-was synthesized by the reaction of 3,5-diamino-1,2,4-triazole and picric acid in the mixture of ethanol and water solution.Single crystals suitable for X-ray measurement were obtained at room temperature.The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis.Crystallographic data:C8N8H8O7,Mr = 328.22,monoclinic,space group C2/c with a = 22.815(2),b = 4.8086(5),c = 22.564(2),β = 93.976(2)°,V = 2469.6(4)3,Dc = 1.766 g/cm3,Z = 8,μ = 0.156 mm-1,F(000) = 1344,the final R= 0.0309,wR= 0.0864.     

Synthesis and Crystal Structure of [Zn(FcCOO)_2(2,2'-bipy)(H_2O)]_2·H_2O

A novel complex [Zn(FcCOO)2(2,2'-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2'-bipy = 2,2'-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) A, α = 90, β = 97.7420(10), γ = 90o, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) A3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I > 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2'-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.