Synthesis and Crystal Structure of a Two-dimensional Zinc(II) Coordination Polymer: [Zn_2(DTB)(DMF)_4(H_2O)_2]_n (DTM= 1,4-Dinitro-2,3,5,6-tetracarboxylatebenzene Tetravalent Anion; DMF = Dimethylformamide)

1 INTRODUCTION For a long time much research interest has beenfocused on coordination polymers because they mayafford new materials with useful properties, such ascatalytic activity, microporosity, electrical conduc-tivity, non-linear optical activit…     

[Cu(Phen)_3][DTB]·6H_2O的合成与晶体结构

利用螯合配体1,10-邻菲咯啉(Phen)与2,2′-二硫代二苯甲酸(H2DTB)的钠盐及氢氧化铜反应合成了一种新型配合物[Cu(Phen)3][DTB].6H2O,通过元素分析、红外光谱和X射线单晶衍射等技术对其进行了表征.配合物属单斜晶系,空间群P2(1)/c,晶胞参数:a=1.822(2)nm,b=3.053(4)nm,c=2.016(3)nm,α=90°,β=106.28(4)°,γ=90°,Z=8,V=10.762(25)nm3,Dc=1.255 g/cm3,Mr=1016.57.该配合物晶体结构由配阳离子[Cu(Phen)3]2+和未配位的反荷阴离子[DTB]2-和晶格水分子组成.每个Cu(Ⅱ)原子与来自三个Phen的6个N原子配位,形成畸变的八面体结构单元.     

Di-tert-butyl phosphate as synthon for metal phosphate materials via single-source coordination polymers [M(dtbp)(2)](n) (M = Mn,Cu) and [Cd(dtbp)(2)(H2O)](n) (dtbp-H = (tBuO)(2)P(O)OH)

Reaction of M(OAc)(2).xH(2)O (M = Mn, Cu, or Cd) with di-tert-butyl phosphate (dtbp-H) in a 1:2 molar ratio in methanol followed by slow crystallization of the resultant solid in MeOH/THF medium results in the formation of three new polymeric metal phosphates [M(dtbp)(2)](n)() [M = Mn, 1 (beige); M = Cu, 2 (blue)] and [Cd(dtbp)(2)(H(2)O)](n)(), 3 (colorless)] in good yields. The formation of [Mn(dtbp)(2)](n) (1) proceeds via tetrameric manganese phosphate [Mn(4)(O)(dtbp)(6)] (4), which has been isolated in an analytically pure form. Perfectly air- and moisture-stable compounds 1-4 were characterized with the aid of analytical, thermoanalytical, and spectroscopic techniques. The molecular structures of 1-3 were further established by single-crystal X-ray diffraction studies. Crystal data for 1: C(32)H(72)Mn(2)O(16)P(4), monoclinic, P2(1)/c, a = 19.957(4) A, b = 13.419(1) A, c = 18.083(2) A, beta = 91.25(2) degrees, Z = 4. Crystal data for 2: C(16)H(36)CuO(8)P(2), orthorhombic, Pccn, a = 23.777(2) A, b = 10.074(1) A, c = 10.090(1) A, Z = 4. Crystal data for 3: C(48)H(114)Cd(3)O(27)P(6), triclinic, P1, a = 12.689(3) A, b = 14.364(3) A, c = 22.491(5) A, alpha = 84.54(3) degrees, beta = 79.43(3) degrees, gamma = 70.03(3) degrees, Z = 2. The diffraction studies reveal three different structural forms for the three compounds investigated, each possessing a one-dimensional coordination polymeric structure. While alternating triple and single dtbp bridges are found between the adjacent Mn(2+) ions in 1, uniform double dtbp bridges across the adjacent Cu(2+) ions are present in 2. The cadmium ions in the structure of 3 are pentacoordinated. Thermal analysis (TGA and DSC) indicates that compounds 1-3 convert to the corresponding crystalline metaphosphate materials M(PO(3))(2), in each case at temperatures below 500 degrees C. Similarly, the thermal decomposition of 4 results in the formation of Mn(PO(3))(3) and Mn(2)P(2)O(7). The final materials obtained by independent thermal decomposition of bulk samples have been characterized using IR spectroscopic, powder diffraction, and N(2) adsorption studies.     

Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O: a layered cadmium phosphonate with reversible dehydration/hydration properties

In a recent systematic study on the influence of the reaction temperature on the structure formation in the system CdCl2/H(HO3PCH2)2NH-CH2C6H4-COOH (H5L) /NaOH, [Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O was obtained as a microcrystalline compound. We have now been able to elucidate the structure from single-crystal data: triclinic, P; a=5.4503(9), b=12.880(2), and c=16.417(3) A; alpha=67.841(6) degrees, beta=80.633(6) degrees, gamma=87.688(8) degrees, V=1052.9(3) A3; Z=1; R1=0.1143, R2=0.2108 (all data); 0.0705, 0.1823 ((I>2sigmaI)). The structure of [Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O is built up of cadmium phosphonate layers connected by water-mediated hydrogen bonds between aryl-carboxylic acid groups and water molecules coordinated to Cd2+ ions of adjacent layers (C-OH...H2O...H2O-Cd2+). The title compound was characterized by IR spectroscopy and energy dispersive X-ray, elemental, and thermogravimetric analyses. Furthermore, temperature-dependent X-ray diffraction data are presented. [Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O can be reversibly dehydrated, and mechanical stress and grinding in the presence of water leads to the intercalation of additional water molecules.     

Cd(II)(bpdc).H(2)O](n): a robust, thermally stable porous framework through a combination of a 2-D grid and a cadmium dicarboxylate cluster chain (H(2)bpdc = 2,2'-Bipyridyl-4,4'-dicarboxylic acid)

The synthesis and characterization of a cadmium(II) coordination polymer, [Cd(C(12)H(6)N(2)O(4)) x H(2)O](n)() (1), is reported. A single-crystal X-ray analysis shows that compound 1 presents a non-interpenetrating three-dimensional porous host containing one-dimensional hydrophilic channels, where guest water molecules reside. The strategy in designing the 3-D framework architecture is based on a combination of two building subunits: a porous two-dimensional grid of (4,4) topology and a metal dicarboxylate cluster chain. Both subunits are assembled from the coordination of a cadmium ion with a three-connecting organic modular ligand, 2,2'-bipyridyl-4,4'-dicarboxylic acid (H(2)bpdc). The results of thermogravimetric analysis and powder X-ray diffraction study show that the framework rigidity of compound 1 remains intact upon the removal of guest molecules, and maintains the thermal stability up to 440 degrees C. The second-row transition-metal ions are capable of engaging higher coordination modes (e.g., hepta- and octacoordination) because of their atomic sizes and intrinsic electron configurations. Our results show that the heptacoordinated cadmium center plays an important role in the overall framework rigidity and high thermal stability of compound 1. Crystal data for 1: Cd(C(12)H(6)N(2)O(4)) x H(2)O, triclinic, space group P1 macro, a = 6.7843(5) A, b = 9.3299(7) A, c = 9.4439(7) A, alpha = 104.629(1) degrees, beta = 92.324(1) degrees, gamma = 100.416(1) degrees, Z = 2.     

Synthesis and Crystal Structure of Cadmium（Ⅱ） Complex [Cd（H2O）（CH3OC6H4COO）2]n

1 INTRODUCTION Cadmium (Ⅱ) complexes have been exten- sively studied from both chemical and structural views, mainly due to the capability of cadmium (Ⅱ) (shared by most d10 metal ions) to adopt different modes of coordination determined by the consideration of size, as well as electrostatic and covalent bonding forces[1]. And the field of coordination polymers has witnessed tremendous growth over the last decade[2]. Many coordination polymeric networks have been shown to posses intere…     

Synthesis and Crystal Structure of DinuclearCadmium Complex [Cd2（phen）4（fca）2]（ClO4）2-（H2O）2

1 INTRODUCTION During the search of molecule-based materials with interesting properties such as catalysis, cla- thration etc., much attention has been focused on the synthesis of one-, two- and three-dimensional extended solids involving cadmium[1], as its d10 configuration permits a wide variety of geometries and coordination numbers. Rigid bridged ligands such as carboxylate groups are frequently used to construct these materials. Therefore, the coordi- nation chemistry of Cd(Ⅱ) ca…     

Crystal structure and quantum chemical investigation of [Cd(NTO)_4Cd(H_2O)_6]·4H_2O

The common explosives, RDX (1,3,5-trinitro-1,3,5-triazacyclohexane), HMX (1,3,5,7- tetranitro-1,3,5,7-tetraazacyclooctane) and TNT (trinitrotoluene), were considered adequately for all weapons applications. Due to many catastrophic explosions resulting from unintentional initia-tion of impact, friction or shock, these explosives have become less attractive. TATB (1,3,5-tria- mino-2,4,6-trinitrobenzene) is noted for its insensitivity, however, it does not have the energetic performance of e…     

一维Z型链状配合物[Cd(BDC)(H2C2EIm)(H2O)]的水热合成、晶体结构和荧光性质研究

水热合成了1个新配合物[Cd(BDC)(H2C2EIm)(H2O)]n(BDC=对二苯甲酸;H2C2EIm=2,2'-乙基双苯丙咪唑).通过元素分析、红外光谱、热重以及X-射线单晶洐射对其进行了表征.该晶体属三斜晶系,P(1)空间群.Cd(Ⅱ)原子通过BDC和H2C2EIm 2种配体连接成一维Z型带状结构,带与带之间通过N-H…D,O-H…O连接成三维超分子结构.室温下配合物具有较强的荧光发射光谱.     

Synthesis and Structural Characterization of a Novel Coordination Polymer [Cd(C_4H_2O_4)(C_3H_4N_2)_3]_n·2nH_2O

1 INTRODUCTION In recent years, the design and synthesis of metalorganic coordination polymers have attracted considerable attention, for such supramolecular assemblies have interesting structures as well as potentiaapplications as smart optoelectronic, magnetic andporous materials. By judicious selection of ligandand metal coordination geometries, control over thetopology and geometry of the infinite networks canbe gained. As neutral donor ligands, 4,4?-bpy, pyrazine and imidazole which …     

Synthesis and Crystal Structure of a 2-D Framework Supramolecular Complex [Cd2（phen）2（adip）（NO3）2]

1 INTRODUCTION In the design of crystal molecule, inorganic crystal engineering is one of the focused fields that are ever developing[1]. The introduction of different metal ions and bridging ligands often gives rise to novel physical and chemical properties[2~4]. Conse- quently, the supramolecular compounds constructed from weak interactions, such as hydrogen bond, π-π stacking, C–H???O interaction, ion-π interaction and hy- drophobing interaction, have become the new focus of cryst…     

Synthesis, Crystal Structure and Luminescent Property of a Novel 1-D Cadmium(II) Complex: [Cd_2(C_8H_3NO_6)_2(H_2O)_4]_n·2nH_2O

A novel one-dimensional chain-like coordination polymer constructed from 3-nitro- benzene-1,2-dicarboxylic acid, [Cd2(C8H3NO6)2(H2O)4]n·2nH2O, has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to monoclinic, space group P21/c with a = 6.1252(8), b = 20.706(3), c = 8.8067(11) , β = 95.608(2)°, V = 1111.6(2) 3, Mr = 751.12, Dc = 2.244 g/cm3, F(000) = 736, μ = 2.011 mm-1, Z = 2, the final R = 0.0262 and wR = 0.0692 for 2338 observed reflections with I > 2σ(I). The structure of the title compound presents a 1-D chain-like structure constructed by dimer units, [Cd2(C8H3NO6)2(H2O)4]n, through two carboxylate oxygen atoms. The fluorescence of the title compound has been also discussed in this paper.     

Synthesis,Crystal Structure and Antitumor Activity of a New Coordination Polymer [Cd（C（14）H（10）N3O5）2（C5H5N）2]n

A new cadmium coordination polymer,[Cd(C14H10N3O5)2(C5H5N)2]n,has been synthesized by the reaction of 2-hydroxy-N'-(4-nitrobenzoyl)benzohydraizide with cadmium acetate in pyridine and ethanol mixture solution.Its molecular structure was characterized by elemental analysis,IR spectra and X-ray crystal structure determination.Crystal data for this compound:tetragonal,space group I41/a,Mr=871.10,a=16.960(6),b=16.960(6),c=28.612(6) ,V= 8230(4)3,Z=8,Dc=1.406 g·m-3 and F(000)=3536.the final R=0.0326,wR=0.0847 for 2682 observed reflections with I 2σ(I) and R=0.0460,wR=0.0896 for all reflections.In the molecular structure of the complex,the cadmium atoms are coordinated to four N and two O atoms forming a slightly distorted octahedral geometry.The intermolecular hydrogen bonds link the neighboring molecules to form a coordination polymer which was then evaluated for its anti-tumor activities against two kinds of cell lines (K562 and BGC) by MTT method.A preliminary bioactivity study indicates that the complex has distinct inhibitory effect on K562 cell lines.     

Hydrothermal Assembly and Structural Characterization of a Novel 3D Coordination Polymer: [Cd_2Zn(BTC)_2(H_2O)_4]_n·2nH_2O

1INTRODUCTIONThehydrothermalsynthesisofmetalsaltsofaro-maticpolycarboxylicacidisattractinginterestinthefieldofcrystalengineeringasaconsequenceoftheirnovelstructuresandpropertiessuchasporosityandmagneticinteractionsbetweenparamagneticmetal-ions[1~7].1,3,5-Benzenetricarboxylicacid(H3-BTC)hasreceivedconsiderableattentionasatridentatearomaticpolycarboxylicligandcapableofformingcoordinationpolymers.Manyscientistshavesuc-ceededinsynthesizingvarietyofporouscoordina-tionpolymerswithhighdimension…     

Synthesis and Crystal Structure of One-dimensional Chain Zinc(II) Coordination Polymer:{Na[ZnL(H2O)2]}n(L=2-Hydroxyl-2-hydroxylate-malonate Trivalent Anion)

1 INTRODUCTION For a long time much research interest has been focused on coordination polymers because such new coordination polymers may afford new materials with useful properties such as catalytic activity, mi- croporosity, electrical conductivity, …     

Hydrothermal Synthesis and Crystal Structure of a Cd~(2+) Supramolecular Coordination Complex{[Cd_2(HCAM)_2(H_2O)_4]·3.5H_2O}_n with a 3D Metal-organic Open Framework

<正>A three-dimensional coordination polymer {[Cd_2(HCAM)_2(H_2O)_4]·3.5H_2O}_n was synthesized by the hydrothermal reaction of H_3CAM(H_3CAM=4-hydroxypyridine-2,6-dicerboxylic acid)and Cd(NO_3)_2·4H_2O.The structure was characterized by elemental analysis,thermal gravimetric analysis,infrared spectroscopy and single-crystal X-ray diffraction.It crystallizes in triclinic,space group P_1~-with a= 9.4389(19),b=11.009(2),c=11.192(2)(?),α=87.87(3),β= 74.63(3),γ=81.22(3)°,V=1108.2(4)(?)~3,Z=2,D_c=2.164g/cm~3,μ=2.011 mm~(-1),F(000)=710,R =0.0419 and wR=0.1170.X-ray analysis reveals that the title compound adopts a one-dimensional staircase structure by carboxyl of H_3CAM and water molecules,and it is further linked by hydrogen bonds to form a 3-D metal-organic open framework.The thermal gravimetric analysis displays that the framework exists stably below 300℃.     

Structural diversity within analogous compounds: syntheses and studies of M(SCH2CH2NH2)Cl (M = Zn, Cd, Hg)

The novel complexes [Zn(L)Cl] (1), [Cd(L)Cl] (2), [Hg(L)Cl] (3), {[Hg(L)Cl].NaOH.2H2O} (3.NaOH.2H2O), and {[Hg3(HL)2Cl6].2H2O} (4) (L = -SCH2CH2NH2) were prepared and investigated by means of IR spectroscopy and single-crystal X-ray diffraction. The crystal structures of 1, 2, and 3.NaOH.2H2O show chelating N,S-coordination of the cysteaminate ligand, bridging S, and terminally coordinating Cl. Apart from these common features, the coordination geometries and modes of intermolecular association are different. 1 forms a cyclic tetramer with a Zn4S4 ring, and 3.NaOH.2H2O contains one-dimensional [Hg(L)Cl]n chains with S-bridged Hg atoms. Zn and Hg atoms in 1 and 3.NaOH.2H2O are tetracoordinate with a distorted tetrahedral M(ClNS2) geometry (M = Zn, Hg). Each Cd atom of 2 binds to three S atoms and vice versa, such that layers of distorted Cd3S3 hexagons are formed. 2 is the first example for a compound exhibiting a group 12-group 16 layer structure, which can be described as an analogue of a graphite layer. Additionally, each Cd atom binds to a chlorine atom and a nitrogen atom from a cysteaminate ligand resulting in pentacoordination with a distorted trigonal bipyramidal Cd(ClNS3) geometry. 4 contains two differently coordinate Hg atoms. One displays a distorted trans-octahedral Hg(Cl4S2) geometry, while the other is coordinated by four Cl atoms and one S atom and additionally forms a long Hg...Cl contact.     

Reactions and reactivity of Co-bpdc coordination polymers (bpdc = 4,4'-biphenyldicarboxylate)

By choosing a suitable metal center, ligand, and solvents, we have revealed several structural transformations involving a polymer precursor. infinity 1[Co(bpdc)(H2O)2].H2O (1) was prepared by reaction of Na2bpdc and Co(NO3)2 in aqueous solution. Immersing 1 in pyridine/water solutions of (2:1) and (8:1) ratios yielded a second one-dimensional structure infinity 1[Co(bpdc)(py)2(H2O)2].2py (2) and a two-dimensional structure infinity 2[Co(bpdc)(py)2].H2O (3), respectively. After heating 1 under N2 to remove all water within the structure, the compound Co(bpdc) (IR) was obtained. When IR was immersed in solutions of pyridine/water (5:4) and in pure pyridine (in air), a third one-dimensional structure of infinity 1[Co(bpdc)(py)2(H2O)2].2py.H2O (4) and 3, respectively, were obtained. Compounds 2-4 easily transformed to 1 when immersed in water. Crystal data for 1: monoclinic, space group C2/c with a = 6.950(1), b = 31.585(6), and c = 6.226(1) A, beta = 95.84(3) degrees, Z = 4. Crystal data for 2: triclinic, space group P1 with a = 9.646(2), b = 10.352(2), and c = 17.031(3) A, alpha = 79.02(3) degrees, beta = 86.88(3) degrees, gamma = 77.16(3) degrees, Z = 2. Crystal data for 3: triclinic, space group P1 with a = 9.137(2), b = 10.480(2), and c = 12.254(2) A, alpha = 102.10(3) degrees, beta = 100.80(3) degrees, gamma = 99.43(3) degrees, Z = 2. Crystal data for 4: orthorhombic, space group Pbcn with a = 13.468(3), b = 16.652 (3), and c = 14.977(3) A, Z = 4.     

Hydrothermal synthesis, structures, and luminescent properties of zinc(II) and cadmium(II) phosphonates with a 3D framework structure using terephthalate as second linkers

By introduction of 1,4-benzenedicarboxylic acid as a second organic ligand, two new divalent metal(II) phosphonates with a 3D framework structure, namely, [Zn(HL1)(bdc)(0.5)] (1) and [Cd(1.5)(HL2)(bdc)(0.5)] (2) (H(2)L1 = H(2)O(3)PCH(NH(2))C(6)H(5), H(3)L2 = H(2)O(3)PCH(2)-NC(5)H(9)-COOH, H(2)bdc = HOOCC(6)H(4)COOH), have been synthesized under hydrothermal conditions. The two compounds show three-dimensional (3D) framework structure with infinite two-dimensional (2D) networks pillared by H(2)bdc. For compound 1, the {ZnO(4)} polyhedra are interconnected by phosphonate groups into a 2D layer, and the adjacent layers are further cross-linked via the bdc(2-) anions to generate a three-dimensional framework structure with two types of channel system along the c-axis. A notable feature of compound 1 is the presence of alternate left- and right-handed helical chains in the structure. In compound 2, the inorganic chains, composed of {Cd(1)O(7)}, {Cd(2)O(4)} and {CPO(3)} polyhedra, are linked by HL2(2-) ligands to form a double layer structure in the ab plane, and the adjacent layers are further linked by the bdc(2-) anions to form a 3D framework structure with one-dimensional channel systems along the a-axis. Luminescence properties of compounds 1 and 2 have also been studied.     

Three-, two-, and one-dimensional metal phosphonates based on [hydroxy(4-pyridyl)methyl]phosphonate: M{(4-C5H4N)CH(OH)PO3}(H2O) (M = Ni, Cd) and Gd{(4-C5H4N)CH(OH)P(OH)O2}3.6H2O

Based on the [hydroxy(4-pyridyl)methyl]phosphonate ligand, three compounds with formula Ni{(4-C(5)H(4)N)CH(OH)PO(3)}(H(2)O) (1), Cd{(4-C(5)H(4)N)CH(OH)PO(3)}(H(2)O) (2), and Gd{(4-C(5)H(4)N)CH(OH)P(OH)O(2)}(3).6H(2)O (3) have been synthesized under hydrothermal conditions. The crystal data for 1 are as follows: orthorhombic, space group Pbca, a = 8.7980(13) A, b = 10.1982(15) A, and c = 17.945(3) A. For 2 the crystal data are as follows: monoclinic, space group C2/c, a = 23.344(6) Angstroms, b = 5.2745(14) Angstroms, c = 16.571(4) Angstroms, and beta = 121.576(4) degrees. The crystal data for 3 are as follows: rhombohedral, space group R, a = 22.2714(16) Angstroms, b = 22.2714(16) Angstroms, and c = 9.8838(11) Angstroms. Compound 1 adopts a three-dimensional pillared layered structure in which the inorganic layers made up of corner-sharing {NiO(5)N} octahedra and {CPO(3)} tetrahedra are connected by pyridyl groups. A two-dimensional layer structure is found in compound 2, which contains alternating inorganic double chains and pyridyl rings. Compound 3 has a one-dimensional chain structure where the Gd atoms are triply bridged by O-P-O linkages. The pyridyl nitrogen atom in 3 remains uncoordinated and is involved in the interchain hydrogen bonds. Magnetic susceptibility studies of 1 and 3 reveal that weak ferromagnetic interactions are mediated between Ni(II) centers in compound 1. For compound 3, the behavior is principally paramagnetic.