Synthesis,Crystal Structure and Bioactivity of a Pd(Ⅱ) Complex with Demethylcantharate and 2,2′-Bipyridine

A novel crystal with the molecular formula [Pd(DCA)(bipy)]2 [Pd(bipy)Cl2 ]·6.75H2O was formed by PdCl2 with disodium demethylcantharate (Na2 (DCA),DCA2= 7-oxa-bicyclo[2.2.1]heptane-2,3-bicarboxylate) and 2,2-bipyidine (bipy) through the hydrothermal method.The complex was characterized by elemental analysis and infrared spectroscopy.The structure of the complex was determined by single-crystal X-ray diffraction,which is of triclinic system,space group P1 with a=13.6818(7),b=14.8426(8),c=15.0043(8),α=97.319(3),β=92.521(3),γ=105.776(2)°,V=2898.4(3) 3,Dc=1.545 g·cm-3,Z=1,F(000)=1420,S=0.852,the final R=0.0525 and wR=0.1777 for 13634 observer reflections (I>2σ(I)).The binding reaction of the complex with ct-DNA and bovine serum albumin (BSA) was studied by fluorescence spectroscopy.The results indicated that the complex binds to ct-DNA via the partial intercalation.The binding constant K A of the complex interaction with BSA was 3.98×10 5 L·mol-1 and one binding site would be formed.The antiproliferative activity of the complex against human hepatoma cells (SMMC7721) in vitro is much higher than that of Na 2 (DCA).     

Synthesis and Crystal Structure of [Cd(NBA)(μ_3-OH)(4,4′-bipy)_(1/2)]_n

A new cadmium polymer [Cd(NBA)(μ3-OH)(4,4′-bipy)1/2]n 1 (NBA = m-nitrobenzoic acid and 4,4′-bipy = 4,4-bipyridine) has been synthesized by hydrothermal reaction. Its structure was determined by single-crystal X-ray diffraction method, and characterized by elemental analysis and IR spectrum. The crystal is of monoclinic, space group C2/c, with a = 15.6912(9), b = 25.9394(15), c = 6.7332(4) ′, β = 114.7700(10)°, V = 2488.4(3) 3, C12H9CdN2O5, Mr = 373.61, Z = 8, Dc = 1.995 g/cm3, μ = 1.776 mm-1, F(000) = 1464, R = 0.0411 and wR = 0.1128 for 2130 observed reflections (I > 2σ(I)). X-ray diffraction studies reveal that the compound features a layered structure, in which 4,4′-bipy ligands bridge Z type of double chains [Cd(μ3-OH)]n and NBA ligands locate at the two sides of the layer. The π-π interactions between the benzene rings of NBA ligands of two adjacent layers lead to the 3D framework.     

Synthesis, Characterization and Crystal Structure Determination of a Thiocyanato Bridged One-dimensional Polymeric Complex of Cadmium(Ⅱ)

A new one-dimensional polymeric complex [Cd(SCN)2(H2O)]L (L = N,N?-bis(furan- 2-ylmethylene)hydrazine) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, pace group P1 with a = 5.9268(8), b = 10.8678(15), c = 13.3671(19) , α = 109.295(2), β = 95.092(2), γ = 97.8580(10)°, V = 796.70(19) 3, Z = 2, C12H10CdN4O3S2, Mr = 434.76, μ = 1.648 mm–1, Dc = 1.812 g/cm3, F(000) = 428, R = 0.0308 and wR = 0.0769. The crystal structure reveals that the structure of [Cd(SCN)2(H2O)]n features di-μ-1,3-thiocyante bridges and 1D chains. The octahedrally coordinated Cd atom is surrounded by one oxygen atom from water molecule, three S atoms and two Natoms from five di-μ-1,3 thiocyanato bridges. The Cd atoms are connected by two di-μ-1,3 thiocyanato bridges with the Cd(1)…Cd(1A) separation of 4.239(1)  and Cd(1)…Cd(1B) of 5.852(1). In addition, the one-dimensional straight chain structure is further connected by multiform intermolecular N-H…O hydrogen bonds and π…π interactions to form a three-dimensional supramolecular structure.     

Synthesis, Crystal Structure and Fluorescene of a One-dimensional Compound {CdI2（2,2＇-bipy）}n

The title compound, {CdI2(2,2'-bipy)}n, was prepared by the hydrothermal reaction of CdI2 and 2,2'-bipy in an aqueous solution, and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: C10H8N2CdI2, monoclinic system, space group C2/c, a = 16.927(1), b = 10.0925(7), c = 7.7422(3) (A), β = 106.0629(4)°, V = 1271.00(14)(A)3, Z = 4, F(000) = 944, μ = 6.546 mm-1, Dc= 2.730 g/cm3, Mr = 522.38, the final R = 0.0309 and wR = 0.0805 for 1310 observed reflections (I＞2σ(Ⅰ)). X-ray crystal structure analysis shows that the Cd atom is coordinated by four iodines and two N atoms from one 2,2'-bipy to form an 1-D chain-like structure through bridging iodines. The fluorescene of the title compound was also discussed.     

A Cadmium(II) Coordination Polymer: Crystal Structure and Fluorescent Property of [CdCl_2(4,4''''-bipyridine)]_ ∞

1 INTRODUCTION The metal-organic coordination polymers have proved to be promising in developing new mate- rials[1]. It is crucial to select or synthesize the suita- ble bridging organic ligand. Some simple rigid li- gands are skillfully employed[2～4].…     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

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 = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, 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.     

Synthesis and Crystal Structure of Copper(Ⅱ) Compound with Didentate Schiff-base Ligand

1INTRODUCTIONTransitionmetalcomplexesofSchiff-baseligandswhichbindtwoormoremetalcentersincloseproximityareimportantaspotentialcatalysts[1]andasmodelsforanumberofmetalloproteins[2]duetotheopportunitytheyprovidefortheinvesti-gationofmagneticinteractions.The…     

Hydrothermal Syntheses and Crystal Structures of Two Complexes with 3,5- Dinitrosalicylate and 2,2′-Bipyridine Ligands

The two title complexes,[Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5-(NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal=3,5-dinitrosalicylate,2,2′-bipy=2,2′-bipyridine),were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic,space group P1,a=5.581(4),b=12.071(8),c=12.88(1),α=92.10(3),β=96.73(3),γ =102.02(2)°,C17H10N4O7Cd,Mr=494.69,V=841(1)3,Z=2,Dc=1.954 g/cm3,F(000)=488,μ =1.353 mm-1,R=0.0248 and wR=0.0761. Complex 2 crystallizes in monoclinic with space group P21/c,a=8.604(3),b=23.88(1),c=8.894(3),β=102.45(1)°,C17H10N4O7Mn,Mr=437.23,V= 1785(1) 3,Z=4,Dc=1.627 g/cm3,F(000)=884,μ=0.791 mm-1,R=0.0471 and wR=0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units (Cd2O2) and eight-membered ring units (CdOCO)2. Compound 2 displays a linear 1D chain through Mn(Ⅱ) atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472(2). The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported.     

Synthesis and Crystal Structure of N,N~′-Bis(p-nitrophenyl)-2,2~′-(p-phenylene-dioxy)diacetamide DMF Monohydrate

1 INTRODUCTION Many crown ethers have been synthesized[1, 2] and widely used[3～5]. The amide-type acyclic poly- ethers with versatile molecular structures offer many advantages over the traditional crown ethers, such as their potential activity for ion-selective electrodes[6] and the extraction of metal ions[7], so they have attracted much scientific attention[8～10]. In an effort to investigate the effect of skeleton of acyclic polyether on the extractability of metal ions, and to find …     

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.     

Synthesis and Crystal Structure of aNovel Polymer Copper（ Ⅱ） Complex

1 INTRODUCTION One-dimensional coordination polymers of metal complexes have been extensively studied for many years owing to their unusual properties, and many efforts have been made to prepare these kinds of complexes. Study on these polymer complexes has an active field of coordination chemistry in recent years[1～5]. In this study we obtained a com- plex C14H9CuNO3CH3OH, of which the carboxy- late oxygen atom acts as the bridging ligands to coordinate to the second metal atom, fo…     

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.     

Synthesis,Crystal Structure,Theoretical Calculation,and Photophysical Property of a New Cd(Ⅱ) Complex Based on N-heterocyclic Ligand and Isophthalic Acid

A new metal-organic coordination complex[Cd(imp)(m-bdc)]_n (1,ipm=5-(1H-imidazo[4,5-f][1,10]phenanthrolin-2-yl)-2-methoxyphenol,m-bdc=isophthalic acid) has been synthesized by hydrothermal reaction and characterized by elemental analysis,thermogravimetric (TG) analysis,infrared spectrum (IR) and single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic,space group C2/c with a=15.373(5),b=16.719(5),c=19.406(6)A,β=106.995(5)°,V=4770(2)A³,C₂₈H₁₈Cd N₄O₆,M_r=618.86,D_c=1.724 g/cm³,μ(Mo Kα)=0.971 mm^–1,F(000)=2480,Z=8,the final R=0.0391 and w R=0.1044 for 4701 observed reflections (I>2σ(I)).Single-crystal X-ray diffraction reveals that 1 exhibits a one-dimensional (1D) double-chain architecture,and the H-bond intersections link the 1D double-chain architecture into a 2D layer structure.TG analysis shows clear courses of weight loss,which corresponds to the decomposition of different ligands.We also study the luminescent properties of complex 1.In addition,to elucidate the essential electronic characters of this complex,theoretical calculation analysis was performed by the PBE0/LANL2DZ method in Gaussian 03 Program.     

Synthesisand Crystal Structure of a Cu（II） Complex with Reduced Schiff-base N-（2-Hydroxybenzyl）-D,L-alanine and 4,4＇-Bipyridine

A new complex [Cu2(sala)2(H2O)2(4,4'-bipy)]·H2O (sala = N-(2-hydroxybenzyl)- D,L-alaninate, 4,4'-bipy = 4,4'-bipyridine) has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis and single-crystal X-ray diffraction. The complex crystallizes in monoclinic system, space group C2/c with a = 42.44(3), b = 10.416(8), c = 15.487(13), β = 97.455(14)o, C30H36Cu2N4O9, Mr = 723.71, V = 6789(9)3, Dc = 1.416 g/cm3, Z = 8, F(000) = 2992, μ(MoKα) = 1.308 mm-1, R = 0.0493 and wR = 0.1004 for 4878 observed reflections (I > 2σ(I)). Structural analysis shows that each copper(II) atom displays a distorted square-based pyramidal coordination geometry with two oxygen atoms and one nitrogen atom from one N-(2-hydroxybenzyl)-D,L-alaninate, one nitrogen atom from 4,4'-bipyridine ligand and one water molecule. 4,4'-Bipyridine ligand bridges two Cu(II) ions to form a dinuclear compound. The molecular structure is extended into a one-dimensional wavy chain through hydrogen bonds. These 1D chains are further expanded into 2D networks through hydrogen bonds.     

Hydrothermal Synthesis,Crystal Structure and Electrochemical Properties of Complex [Cd(phen)_3]·(ClO_4)_2·(p-MBA)_2·(H_2O)_2

One new cadmium complex [Cd(phen)3]·(ClO4)2·(p-MBA)2·(H2O)2 has been hydro-thermally synthesized by reacting p-methylbenzoic acid (p-MBA),1,10-phenanthroline (phen) and cadmium perchlorate. It crystallizes in the triclinic system,space group P1,with a=1.2809(3),b= 1.3431(3),c=1.3734(3) nm,α=84.259(4),β=71.603(3),γ=74.424(3)o,V=2.1594(8) nm3,Dc= 1.532 g/cm3,Z=2,F(000)=1008,μ=0.697 mm-1,R=0.0646 and wR=0.1648. The crystal structure shows that the cadmium ion is coordinated with six nitrogen atoms from three 1,10-phenanthroline molecules,forming a distorted octahedral coordination geometry. The result of electrochemical property analysis shows that the electron transfer in the electrode reaction is irreversible.     

Hydrothermal Synthesis and Crystal Structure of a New One-dimensional Nickel(Ⅱ) Complex with 2-Pyridinecarboxyic Acid and 4,4′-Bipyridine Ligands

A new metal-organic coordination polymer [Ni[(2-pya)2(4,4′-bipy)]n·6nH2O (2-pya = 2-pyridinecarboxylic acid, 4,4′-bipy = 4,4′-pyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I41/a with a = b = 22.5642(19), c = 10.7118(18), V = 5453.8(11) 3, C22H28N4NiO10, Mr = 567.19, Dc = 1.382 g/cm3, μ(MoKα) = 0.769 mm-1, F(000) = 2368, Z = 8, the final R = 0.0572 and wR = 0.1254 for 1401 observed reflections (I > 2σ(I)). It exhibits a one-dimensional chain-like structure by mixed ligands of 2-pyridinedicarboxylic acid and 4,4′-pyridine.     

A Fluorescent Cobalt（II） Complex for the Recognition of Cations and Small Molecules： Synthesis, Structure and Characterization

A fluorescent cobalt(Ⅱ) complex, 1 [Co(H2bibim)2(5-nipa)], for the recognition of cations and small molecules constructed with 5-nitroisophthalic acid (5-H2nipa) and 2,2-biben-zimidazole(H2bibim) has been synthesized by hydrothermal methods and structurally characterized by elemental analysis, IR spectroscopy, PL and single-crystal X-ray diffraction. The cobalt units are six-coordinated by two H2bibim ligands and one 5-nitroisophthalic acid group, which are further connected into a three-dimensional (3D) network by intermolecular hydrogen bonds. Complex 1 exhibits fluorescence and thus has detection capabilities for different cations and small solvent molecules in the solution state at room temperature.     

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.     

Crystal Structure of a Cadmium（II） Complex Containing an Amide Type Ligand

The compound [Cd(L)2(NO3)]NO3·0.5H2O (L = N-benzyl-2-(quinolin-8-yloxy)aceta- mide) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction, elemental analysis, IR and UV spectroscopy. The crystal belongs to the triclinic system, space group P1 with a = 11.7175(13), b = 11.8873(13), c = 14.0958(16) , α = 74.889(2), β = 78.228(2), γ = 78.831(2)o, V = 1835.0(4) 3, Z = 1, Dc = 1.502 Mg/m3, Mr = 1660.17,μ = 0.662 mm-1, F(000) = 846, λ(MoKα) = 0.71073 , the final R = 0.0585 and wR = 0.0577 for all observed reflections. The results show that the Cd(Ⅱ) ion with a square antiprismatic geometry is coordinated by a N2O6 donor set, two NO2 sets from two ligands and two O atoms from a bidendate nitrate group. In the crystal, the O-H···O and N-H···O hydrogen bonds are helpful to consolidate the three- dimensional network.