Two Coordination Novel Polymers Based on a Flexible Ligand N,N?-diacetic Acid Imidazolium

{[Cu_3(cis-DAM)_4(OH)_2]·12H_2O}_n 1 and [Ag_3(trans-DAM)_2(NO_3)]_n 2 with a flexible ligand N,N?-diacetic acid imidazolium(HDAM) were synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic I222 space group with a = 12.033(2),b = 12.498(3),c = 14.963(3) ?,V = 2250.4(8) ?~3,Z = 8,C_7H_(13.5)N_2O_(7.5)Cu_(0.75),M_r = 293.35,D_c = 1.732 g·cm~(-3),F(000) = 1210,GOF = 1.087,the final R(I 2σ(I)) = 0.0521 and w R(all data) = 0.1386. Compound 2 crystallizes in the monoclinic C2/c space group with a = 21.601(4),b = 8.321(2),c = 13.589(3) ?,β = 126.95(3)°,V = 1951.9(7) ?~3,Z = 8,C_7H_7N_(2.5)O_(5.5)Ag_(1.5),M_r = 375.96,D_c = 2.559 g·cm~(-3),F(000) = 1448,GOF = 1.017,R(I 2σ(I)) = 0.0222 and w R(all data) = 0.0633. Compound 1 displays a novel 2D layer,consisting of a couple of left-helical chains with a pitch of 12.498(3) ? formed by μ_3-cis-DAM~– ligands and Cu(1) ions,which are stabilized by hydrogen bonding interactions to give a 3D supramolecular framework. As for 2,Ag(1) ions are doubly bridged by trans-DAM~– and NO_3~– to form [Ag(1)_2O_4] chains,which are further connected by Ag(2) and trans-DAM~– to build a 3D framework. Additionally,thermogravimetric analyses,FT-IR spectroscopy,UV-visible spectroscopy,and the fluorescent properties were discussed.     

Synthesis, Crystal Structure and Fluorescent Property of a New One-dimensional Cadmium(Ⅱ) Coordination Polymer Based on 3,4-Thiophenedicarboxylic Acid and 1,10-Phenanthroline

A new cadmium(Ⅱ) polymer [Cd(tdc)(Phen)]n 1 (H2tdc = thiophene-3,4-dicar-boxylic acid, Phen = 1,10-phenanthroline) was synthesized under hydrothermal conditions. The compound crystallizes in the triclinic system, space group P , with a = 7.3150(10), b = 10.3598(14), c = 10.8784(15) , α = 82.2740(10), β = 72.9730(10), γ = 80.236(2)°, V = 773.68(18) 3, Z = 2, Mr = 462.74, Dc = 1.986 Mg/m3, μ = 1.58 mm-1, F(000) = 456, the final R = 0.0218 and wR = 0.0465 for 3361 observed reflections with Ⅰ > 2σ(Ⅰ). The compound presents a one-dimensional (1-D) double-stranded structure and exhibits fluorescent emission at room temperature. Furthermore, infrared spectroscopy, elemental analyses, thermogravimetric analysis and powder X-ray diffraction properties of the compound are also investigated.     

Syntheses and Crystal Structures of Two Zn(Ⅱ) Coordination Polymers Constructed with 4,4’-(Dihydroxymethylene)dibenzoic Acid

Two new isomorphous metal-organic coordination polymers, [Zn(dhmdb)(2,2'- bpy)]n 1 and [Zn(dhmdb)(1,10-phen)]n 2, have been obtained under hydrothermal reactions from 4,4'-(dihydroxymethylene)dibenzoic acid (H2dhmdb), Zn(NO3)2·6H2O and 2,2'-pyridine or 1,10- phenanthroline, respectively. Compounds 1 and 2 have been characterized by FT-IR spectroscopy, thermal analysis and single-crystal X-ray diffraction. The zigzag chains of 1 and 2 are linked into three-dimensional supramolecular networks by both O-H…O hydrogen bonds and π…π stacking interactions. Crystal data for 1: ZnC25H18N2O6, Mr = 507.78, orthorhombic, space group Pbca, a = 14.031(3), b = 10.826(2), c = 27.343(6), V = 4153.5(14)3, Z = 8, Dc = 1.624 g/cm3, F(000) = 2080, μ = 1.231 mm-1, R = 0.0699 and wR = 0.1829. Crystal data for 2: ZnC27H18N2O6, Mr = 531.80, orthorhombic, space group Pbca, a = 13.796(3), b = 10.809(2), c = 28.612(6), V = 4266.8(15)3, Z = 8, Dc = 1.656 g/cm3, F(000) = 2176, μ = 1.203 mm-1, R = 0.0454 and wR = 0.1399.     

Syntheses and Crystal Structure of Erbium(Ⅲ) Coordination Polymers with Two Flexible Double Betaine Ligands

1INTR0DUCTI0NLanthanidecarboxylatecomplexeshavebeenwidelystudiedt1iandm0starefoundtoexhibitavarietyofdimericorinfinitechainstructures.Recentstudiesinourlaboratoryhavedem0nstratedthattheprototypetertiaryaminebetaine(Me,N CHzC0z-)anditsderivativesareusefulinthegenerationoflanthanidecarb0xylate-likecomplexeswithnewstructuralfeaturesduetotheiroverallchargeneutralityandpossibleinclusionofvariouskindsofcounteranionsinthestructuret2~4i.Thelan-thanidecomplexesisolatedsofarhavebeenfoundtobemononu…     

Two New Coordination Polymers Assembled with a Functionalized Ligand：Syntheses and Crystal Structures

Two new transition-metal organic coordination polymers [M(mna)2](M = Cd(1),Zn(2);mna = 2-mercaptonicotinic anion) have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction along with IR and elemental analyses.Compound 1 is generally a one-dimensional linear structure bridged through the sulfur donor of mna ligand,while 2 is a one-dimensional zigzag chain ligated via the oxygen donor of mna ligand.These compounds further result in three-dimensional structures via intermolecular π...π stacking interactions and/or hydrogen bonding interactions.The two compounds were structurally determined by single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic space group P21/c with a = 3.730(3),b = 13.973(12),c = 12.380(11) ,β = 97.953(18)°,V = 639.0(10) 3,Z = 2,CdC12H8O4N2S2,Mr = 420.72,Dc = 2.187 g/cm3,F(000) = 412,Rint = 0.0252,T = 293(2) K,μ = 2.052 mm?1,the final R = 0.0269 and wR = 0.0586 for 1377 observed reflections with I > 2σ(I).Complex 2 belongs to monoclinic space group P21/c with a = 13.376(2),b = 12.8429(14),c = 7.4856(10) ,β = 96.190(10)°,V = 1278.5(3) 3,Z = 4,ZnC12H8O4N2S2,Mr = 373.69,Dc = 1.941 g/cm3,F(000) = 752,Rint = 0.0414,T = 293(2) K,μ = 2.264 mm?1,the final R = 0.0418 and wR = 0.0966 for 2396 observed reflections with I > 2σ(I).     

Syntheses and Crystal Structures of Two Copper~Ⅱ Complexes with Tetracyanonickelate~Ⅱ

Two copper-nickel complexes, {[Cu(i-Pr3TACN)][Ni(CN)4]}2·2H2O (1) and {[Cu(DACH)][Ni(CN)4]}n (2), have been synthesized by the self-assembly reactions of K2[Ni(CN)4] with CuCl2 and the corresponding chelating ligand 1,4,7-triisopropyl-1,4,7- triazacyclononane (i-Pr3TACN) or 1,4-diazacycloheptane (DACH), respectively. The complexes were structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectra and magnetic properties. Complex 1 presents a [2+2] type of molecular square structure and 2 features a 2D β-pucker structure. The magnetic susceptibility measurements reveal a weak antiferromagnetic interaction between the Cu(Ⅱ) ions, with the J values of-22.11 and -32.50 cm-1 for 1 and 2. Moreover, by changing the size of macrocyclic ligands we have successfully constructed two different strictures, which may provide useful information for the construction of the structure.     

Two Cd(Ⅱ) Coordination Polymers Based on a Flexible Tricarboxylate Ligand: Syntheses,Structures, and Photoluminescence and Catalytic Properties

Studies on the synthesis and design of coordination polymers(CPs) with flexible ligands are of great interest owing to their dynamic structures and promising applications. The title coordination polymers, {[Cd·(HTTTA)·(phen)]·2H_2 O}n(1) and [Cd·(HTTTA)·(phen)]n(2)(H3 TTTA = 2,2',2'-[1,3,5-triazine-2,4,6-triyltris(thio)] tris-acetic acid, phen = 1,10-phenanthroline) have been synthesized and characterized by elemental analysis, IR, powder XRD and single-crystal X-ray diffraction. Complex 1 consists of one CdII ion, one HTTTA2-ligand and one phen co-ligand. The Cd(Ⅱ) metal clusters were bridged by the tridentate HTTTA2-ligands into infinite 1D chains, which are further connected into the 3D architecture by abundant hydrogen bonds. In 2, three carboxyl groups of HTTTA2-ligand show different coordination directions because of the C–S–C flexible bond angle, which leads to different 1D chains of 2. The strong π-π stacking interaction and four C–H···O hydrogen bonds connect the 1D chains into a 3D framework. The solid-state photoluminescence and catalytic properties were studied as well.     

Syntheses and Crystal Structures of Cd(Ⅱ) and Ni(Ⅱ) Complexes Containing Flexible Sulfide and Nitrogen Heterocyclic Ligands

Two new coordination polymers [Cd(EBLA)(ip)(H2O)](1) and [Ni(EBSA)(im)2(H2O)]n(2) were synthesized by hydrothermal and solution methods using 2,2'-dithiosalicylicacid(EBSA), 1H-imidazo[4,5-f][1,10]phenanthroline(ip), imidazole(im), Cd(NO3)2·4H2O and Ni(NO3)2·6H2O. The complexes were characterized by elemental analysis and FT-IR. Meanwhile, the crystal structures, fluorescence properties of complex 1 and thermogravimetrie analysis of complex 2 have been studied. In complex 1, 2,2'-dicarboxydiphenylthioether(EBLA) was prepared with 2,2'-dithiosalicylicacid(EBSA) in situ reaction by hydrothermal method. Complex 1 is a dinuclear structure and Cd2+ is five-coordinated in a distorted trigonal bipyramidal geometry. Complex 2 is a one-dimensional infinite linear chain and Ni2+ is six-coordinated to form a distorted octahedral geometry. Hydrogen bonding and π-π interactions are observed in these complexes.     

Syntheses and Crystal Structures of Copper（Ⅱ） and Nickel Complexes with 1,2,3-Triazole-carboxylic Acid

Three novel complexes [Cu(L1)2(H2O)2] (1), [Ni(L1)2(H2O)2]·(H2O)4(2,HL1=5-methyl-1-(4-methylphenyl)-1,2,3-triazole-4-carboxylic acid) and [Ni2 (HL2)2(CH3OH)6]·(CH3OH)2(3,H3L2=1,2,3-triazole-4,5-dicarboxylic acid) were synthesized and characterized by elemental analysis, IR and X-ray diffraction. Complexes 1 and 2 are mononuclear structures, and are assembled into a two-dimensional sheet by C(7) H(7)···O(3) weak interactions or hydrogen-bonding interaction. Complex 3 is a centrosymmetric dinuclear structure, and is assembled into a three-dimensional supramolecular structure by hydrogen-bonding interaction.     

Two New Copper(Ⅱ) Complexes with p-Cyanobenzoic Acid: Synthesis,Crystal Structures and Properties

The complexes of [Cu(bpy)(H2O)(CBA)2]n 1 and [Cu(phen)(H2O)(CBA)2]·H2O 2 based on p-cyanobenzoic acid(HCBA) have been synthesized in aqueous ethanolic solution at room temperature. The single-crystal X-ray diffraction studies demonstrated that complex 1 crystallizes in orthorhombic and complex 2 is of triclinic system. The results indicate the complex 1 shows a 1D chain structure bridged by two carboxylic oxygen atoms from CBA–, and complex 2 is a mononuclear structure. Through intermolecular hydrogen bonding and π...π stacking interactions, the complexes are assembled into supramolecular structures. Complex 1 has been characterized by magnetic measurements. The magnetic measurement indicates that weak ferromagnetic interaction(zJ= 0.038(5)) between the Cu2+ ions is dominant in the structure. The IR spectrum and results of thermal and elemental analyses are also presented.     

Syntheses and Crystal Structures of Two One-dimensional Cobalt(Ⅱ) Compounds with the Flexible Dipyridyl Ligan

Two one-dimensional cobalt(Ⅱ) compounds {[Co(Hbpma)(H2O)4 ] 2 ·3SO 4 ·4.5H2O} n1 and {[Co(Hbpma)(NCS) 3 (H2O)]·2.85H2O}n2 (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 P1 with a = 15.8780(5), b = 16.2187(5), c = 16.4858(5) , α = 91.0420(10), β = 94.5190(10), γ = 101.4360(10)°, V = 4145.7(2) 3 , C 24 H 53 Co 2 N 6 O 24.50 S 3 , M r = 1031.76, Z = 4, D c = 1.653 g/cm 3 , μ(MoKα) = 1.046 mm -1 , F(000) = 2148, S = 1.017, the final R = 0.0269 and wR = 0.0644 for 13032 observed reflections (I > 2σ(I)). For complex 2, it belongs to triclinic, space group P1 with a = 9.3761(11), b = 10.5814(13), c = 11.2972(14) , α = 85.472(2), β = 88.058(2), γ = 76.203(2)°, V = 1085.0(2) 3 , C 15 H 21.70 CoN 6 O 3.85 S 3 , M r = 502.79, Z = 2, D c = 1.539 g/cm 3 , μ(MoKα) = 1.112 mm -1 , F(000) = 519, S = 1.070, the final R = 0.0358 and wR = 0.0899 for 3466 observed reflections (I > 2σ(I)). Two complexes 1 and 2 are both found to be one-dimensional coordination polymers bridged by the protonated bpma ligands, which are assembled into three-dimensional supramolecular structures through the hydrogen bonding interactions and π-π packing interactions.     

Syntheses,Structures and Properties of Two 2D Coordination Polymers from 5-（Pyridin-2-yl-methyl）aminoisophthalate

Hydrothermal reactions of 5-(pyridin-2-yl-methyl)aminoisophthalic acid(H2paip) with Mn(OAc)2·4H2O and Cu(NO3)2·3H2O produced two 2D complexes, [Mn(paip)]n·nH2O(1) and [Cu(paip)(H2O)]n(2). In complex 1, paip serves as a μ4-bridge, and its two carboxylate groups in μ2,η2-bridging and chelating modes connect Mn(Ⅱ) into 1D chains, which are further extended into a 2D layer through coordination of two chelating nitrogen atoms. However, paip in complex 2 acts as a μ3-bridge to link Cu(Ⅱ) into a 2D layer, in which two carboxylate groups function in a monodentate mode, and hydrogen bonds between the coordinated water and carboxylate oxygen atoms further extend the 2D layers into a 3D supramolecular network. The frameworks of complexes 1 and 2 are stable up to 470 and 250 ℃, respectively. Magnetic measurement shows that complex 2 possesses a weak antiferromagnetic interaction.     

Synthesis and Crystal Structure of a New Cadmium（Ⅱ） Coordination Polymer with Ethylenediaminetetraacetic Acid

A new cadmium(Ⅱ) coordination polymer,namely,[KCd2(edta)I]n(1,H4edta = ethylenediaminetetraacetic acid),has been prepared and structurally characterized by single-crystal X-ray diffraction.Crystallographic data for 1:C10H12Cd2IKN2O8,Mr = 679.02,monoclinic,space group P21/n,a = 9.870(5),b = 8.989(4),c = 19.082(10) ,β = 104.581(10)o,V = 1638.5(13) 3,Z = 4,Dc = 2.753 g/cm3,μ = 4.776 mm-1,F(000) = 1272,the final R = 0.0473 and wR = 0.1311 for 2846 observed reflections with I > 2σ(I).Polymer 1 features a 2-D layered structure,in which each edta4-ligand chelates/bridges five adjacent six-/seven-coordinated Cd(Ⅱ) centers with all ten donors(eight oxygen and two nitrogen) involved with coordination.Additional iodide I-ions as counterions are bound to the Cd(Ⅱ) centers in a terminal mode and the potassium K+ ions are located in the layers and surrounded by O and I atoms from neighboring environment.The thermal stability of 1 has been discussed.     

Syntheses, Crystal Structures and Magnetic Properties of a New Nitronyl Nitroxide Radical and Its Cu(Ⅱ) Complex

A new compound (NIT-mNO2 = 4,4,5,5-tetramethylimidazoline-2-yl-(2'-chlor-5'- nitrophenyl)-3-oxide-1-oxyl) 1 and its complex (Cu(NIT-mNO2)(hfac)2) 2 have been synthesized and structurally and magnetically characterized. Complex 1 crystallizes in monoclinic, space group P21/n with a = 10.6798(9), b = 11.2705(9), c = 12.9559(10) , β = 107.3770(10)o, V = 1488.3(2) 3, C13H15ClN3O4, Mr = 312.73, Z = 4, Dc = 1.396 g/cm3, μ(MoKa) = 0.276 mm-1, F(000) = 652, the final R = 0.0606 and wR = 0.1773 for 3405 independent reflections with Rint = 0.0203. The nitronyl nitroxide unit (imidazoline ring) is not coplanar with the phenyl ring with the dihedral angle between them of 55.75o. The compound results in a 1-D zig-zag chain structure by intermolecular H-bond interaction. Compound 2 crystallizes in triclinic, space group P1 with a = 10.3699(10), b = 10.6286(11), c = 15.1683(15), α = 77.5330(10), β = 773080(10), γ = 87.3420(10)o, V = 1592.5(3) 3, C23H17ClF12N3O8Cu, Mr = 790.39, Z = 2, Dc = 1.648 g/cm3, μ(MoKa) = 0.888 mm-1, F(000) = 788, the final R = 0.0793 and wR = 0.2153 for 5794 independent reflections with Rint = 0.0196. The Cu(II) ion is located at a center of symmetry, and each Cu(II) is surrounded by six oxygen atoms at the vertices of a distorted tetragonal octahedron. Four of the six oxygen atoms belong to two hfac ligands and occupy the equatorial coordination sites, while the other two of NIT-mNO2 act as μ-1,5 bridge between the Cu(II) ion, thus forming a 1-D chain structure. The magnetic susceptibility data indicate intermolecular antiferromagnetic interactions between compound 1 and intrachain ferromagnetic behaviors.     

Syntheses and Crystal Structures of Two New Nickel（Ⅱ） Complexes with Salicylidene-2-ethanolamine

Two new Schiff base complexes of nickle(Ⅱ) [C18H20NiN2O4]·1.5H2O(1) and [C18H20N2NiO4]·H2O(2) were synthesized and characterized by elemental analysis,IR,UV-Vis and X-ray crystal structure analysis.Both 1 and 2 crystallize in the orthorhombic system.Crystal 1:space group Pbcn with a = 12.8591(19),b = 14.779(2),c = 19.749(3) ,V = 3753.3(10) 3,C18H23N2NiO5.5,Mr = 414.07,Z = 8,Dc = 1.445 g/cm3,μ = 1.067 mm-1,F(000) = 1712,S = 1.037,the final R = 0.0741 and wR = 0.2101 for 4353 observed reflections(I > 2σ(I)) and R = 0.1157 and wR = 0.2380 for all data.Crystal 2:space group P21 with a = 9.4673(17),b = 11.559(2),c = 16.347(3) ,V = 1788.9(6) 3,C18H22N2NiO5,Mr = 405.07,Z = 4,Dc = 1.497 g/cm3,μ = 1.116 mm-1,F(000) = 840,S = 1.085,the final R = 0.0330 and wR = 0.0869 for 3151 observed reflections(I > 2σ(I)) and R = 0.0362 and wR = 0.0887 for all data.Each Ni atom of 1 and 2 is six-coordinated with two nitrogen atoms and four oxygen atoms from two salicylidene-2-ethanolamine ligands yielding a distorted octahedral geometry.Dimer structure is observed in the packing diagram of 1.The thermal stability of complex 2 is also studied.     

Syntheses,Crystal Structures and Properties of Mn(Ⅱ) and Co(Ⅱ) Coordination Complexes Based on 1,10-Phenanthroline Derivative

Two new coordination complexes[Mn(L)₂(DNSA)](1) and[Co(L)(1,4-bdc)]_n (2) have been achieved under hydrothermal conditions (H₂DNSA=3,5-dinitro-salicylic acid,1,4-bdc=1,4-benzenedicarboxylic acid and L=2-(2-fluoro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline).1 crystallizes in monoclinic,space group P2_1/c with a=15.871(3),b=17.274(4),c=16.078(3)A,β=113.03(3)^o,V=4056.6(16)A³,Z=4,C₄₅H₂₂Cl₂F₂Mn N₁₀O₇,M_r=978.57,D_c=1.602 g/cm³,F(000)=1980,μ(Mo Ka)=0.536 mm^–1,R=0.0437 and w R=0.1065.2 belongs to the monoclinic system,space group C2/c with a=14.665(2),b=30.856(4),c=11.237(2)A,β=111.166(2)^o,V=4742.0(12)A³,Z=8,C₂₇H₁₄Cl Co FN₄O₄,M_r=517.80,D_c=1.602 g/cm³,F(000)=2312,μ(Mo Ka)=0.889 mm^–1,R=0.0364 and w R=0.0862.The central Mn(II) ion in 1 is six-coordinated by four nitrogen atoms from two L ligands and two oxygen atoms from one DNSA anion.In 2,the two kinds of 1,4-bdc ligands link neighboring Co(II) atoms to yield a two-dimensional layer structure.The luminescence of 1 has been studied in detail.Moreover,thermal behaviors of 1 and 2 are also investigated.     

Syntheses,Crystal Structures and Luminescent and Magnetic Properties of Cerium(Ⅲ) and Zinc(Ⅱ) Coordination Compounds Constructed from 3,5-Dibromobenzoic Acid

Two coordination compounds, namely [Ce(3,5-Br2BC)3(3,5-HBr2BC)]n(1) and [Zn(3,5-Br2BC)2(phen)](2, 3,5-HBr2 BC = 3,5-dibromobenzoic acid, phen = 1,10-phenanthroline), were assembled. Single-crystal X-ray diffraction studies show that compound 1 possesses a 1D chain coordination network, which is further extended into a 3D supramolecular architecture via Br···Br and Br···O halogen bonding. Compound 2 consists of a mononuclear molecule, which is assembled to a 3D supramolecular framework through C–H···O hydrogen bond, π-π stacking interactions and Br···π halogen bonding. Luminescent and magnetic properties of both compounds have also been studied.     

A New Terbium(Ⅲ) Coordination Compound with 2-Thiophenecarboxylic Ligand:Synthesis and Crystal Structure

A new coordination compound with formula [Tb(2-TC)3(DMF)]n(1, 2-TC = 2-thiophenecarboxylic ligand and DMF = dimethylformamide) was synthesized by solvothermal method. The structure of compound 1 was determined by single-crystal X-ray diffraction analyses, and characterized by elemental analyses, IR and powder X-ray diffraction. Structure analysis reveals compound 1, exhibiting a one-dimensional chain structure, crystallizes in triclinic space group P21/c, with a = 9.2751(19), b = 16.490(3), c = 15.865(5) A, β = 118.98(2)o, V = 2122.7(9) A3, Dc = 1.916 g/cm3, Mr = 612.45(C18H15NO7S3Tb), F(000) = 1196, μ(MoKα) = 3.67 mm–1, Z = 4, R = 0.0616 and wR = 0.0962 for 3865 observed reflections(I 2σ(I)), and R = 0.1092 for all data. Meanwhile, the photoluminescent properties of compound 1 were also investigated in the solid state at room temperature.     

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.     

Syntheses,Crystal Structures and Antibacterial Activities of 5-Chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic Acid and Its Copper(Ⅱ) Compound

The title compounds 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic acid(C11H9Cl N2O2, HL)(1) and [Cu(L)2(H2O)](2) were prepared and structurally characterized by elemental analysis, IR and single-crystal X-ray diffraction. Compound 1(C11H9Cl N2O2) crystallizes in the monoclinic system, space group P21/n with a = 7.249(3), b = 20.515(10), c = 7.249(3),β= 96.30°, V = 1071.6(9) ?3, Z = 4, Mr = 236.65, Dc = 1.467 g/cm3, F(000) = 488, GOOF = 1.029, μ= 0.341 mm-1, the final R = 0.0736 and w R = 0.1966 for 1500 observed reflections with I 2σ(I). Compound 2(C22H18Cl2Cu N4O5) crystallizes in the monoclinic system, space group P21/c with a = 7.2931(6), b = 24.548(2), c = 13.2726(11), β= 99.4040(10)°, V = 2344.2(3) ?3, Z = 4, Mr = 552.84, Dc = 1.566 g/cm3, F(000) = 1124, GOOF = 1.050, μ= 1.201 mm-1, the final R = 0.0376 and w R = 0.1000 for 3626 observed reflections with I 2σ(I). 1 and 2 are connected through hydrogen bonding interactions to generate 2D and 3D supramolecular structures, respectively. Moreover, the preliminary antibacterial activities of 1 and 2 against the gram positive bacteria(S. aureus, C. albicans and B. subtilis) and gram negative bacteria(E. coli and P. aeruginosa) have been tested by using the microdilution method, and the results indicate that 2 is more active than 1 against the tested bacteria.