Synthesis and Crystal Structure of 3,3'-Bis(5-(N-(4-hydroxylphenyl)imidomethyl)- pyrrol-2-yl)pentane·2CH_3OH

3,3'-Bis(5-(N-(4-hydroxylphenyl)imidomethyl)pyrrol-2-yl)pentane 1 has been synthesized and characterized. The crystal of its methanol complex, 1·(CH3OH)2, belongs to the orthorhombic system, space group Pccn with a = 18.094(2), b = 11.6890(16), c = 13.3629(19) , V = 2826.3(7) 3, Z = 8, C14.5H18N2O2, Mr = 252.31, Dc = 1.186 g/cm3, F(000) = 1080 and μ(MoKα) = 0.080 mm-1. The final R = 0.0662 and wR = 0.1801 for 1908 observed reflections with I 2σ(I), and R = 0.0800 and wR = 0.1948 for all reflections. In the solid state, bridged by included methanol molecules, the molecules of compound 1 form interpenetrated grid structure through N–H···O and O–H···O hydrogen bonds.     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Novel Water Cluster [Mn(phen)_2·H_2O·Cl]·p-FBA·3H_2O

A novel water cluster [Mn(phen)2·H2O·Cl]·p-FBA·3H2O (p-FBA = p-fluorobenzoic acid and phen = 1,10-phenanthroline) was synthesized by the hydrothermal reaction of MnCl2 with p-FBA and phen at 150 ℃ and characterized by elemental analysis,IR spectra and TG. Its crystal structure was determined by X-ray single-crystal diffraction study. The crystal belongs to the triclinic system,space group P1,with a = 10.5768(1),b = 11.5960(1),c = 12.9916(2) ,α = 101.816(2),β = 95.397(2),γ = 103.052(2)o,V = 1502.8(3) 3,Z = 2,Dc = 1.463 g/cm3,R = 0.0399 and wR = 0.0997. The crystal structure shows that the manganese(Ⅱ ) ion is six-coordinated by four nitrogen atoms,one chloride ion and one oxygen atom forming a distorted octahedral coordination geometry. The structure includes three acyclically connected water molecules and one coordinated water molecule thus forming a (H2O)4 water cluster. This water pattern forms a cross-linked discrete ring. The steady (H2O)4 is further extended into a cage-like structure by the hydrogen-bonding interaction formed by dissociative aqua molecule and Cl-ligand. The dimer structure is further extended into a one-dimensional (1D) structure through C-H···O interaction. π···π Stacking interaction among adjacent phen aromatic rings further stabilizes the crystal structure.     

Synthesis and Crystal Structure of 3-（1-Ethyl-1H-indole-3-carbonyl）aminopropionic Acid

3-(1-Ethyl-1H-indole-3-carbonyl)aminopropionic acid has been synthesized by alkylation of 3-(1H-indole-3-carbonyl)aminopropionic acid methyl ester with bromoethane,follo-wed by saponifying and acidating,in 89.0% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of orthorhombic,space group P212121 with a = 8.9490(12),b = 11.1010(15),c = 13.0475(18) ,V = 1296.2(3) 3,Z = 4,Dc = 1.334 g/cm3,λ = 0.71073 ,μ(MoKα) = 0.095 mm-1,Mr = 260.29 and F(000) = 552.The structure was refined to R = 0.0306 and wR = 0.1445 for 2612 observed reflections with I 2σ(I).In the crystal structure,molecules are linked to each other through hydrogen bonds of N(2)-H(2)···O(1) and O(3)-H(3)···O(1),generating a three-dimensional network.     

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.     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

Synthesis and Crystal Structure of an Unusual Dodecacoordinated Lanthanum Complex by Phenanthroline and Nitrate （phenH）_2[La（NO_3）_5（phen）]·CH_3OH

Lanthanum complex (phenH)2[La(NO3)5(phen)]·CH3OH (1, phen=phenanthroline) was synthesized and characterized by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a=20.3040(3), b=10.7091(1), c=19.0771(2), β=102.090(1)°, V=4056.07(8)3, Z=4, Dc=1.676 g/cm3, μ= 1.142 mm-1, F(000)=2056, the final R=0.0346 and wR=0.0793 for 9981 (Rint=0.0358) independent reflections. The mononuclear complex 1 consists of four parts: two phenH+ cations formed by the protonation of phen, one complex anion [La(NO3)5(phen)]2-, and one solvent methanol molecule. The complex anion contains one phen and five nitrate ligands which both chelate the center La(III) ion, adopting a distorted twelve-coordinated icosahedral geometry. The cations, anion and solvent molecule are linked together by hydrogen bonds. One of the protonated phenanthrolines (phenH+) acting as cation connects to the anion via N–H…O hydrogen bond directly, and the other one links to the anion through an intermediate solvent CH3OH via N–H…O and O–H…O hydrogen bonds. By the plentiful additional weak C–H…O intermolecular hydrogen bonds, the compound molecules construct a two-dimensional layer structure.     

Synthesis and Crystal Structure of a 1-D Coordination Polymer [Pb（ANS）2（phen）]n

A new one-dimensional coordination polymer, [Pb(phen)(ANS)2]n (ANS = 2-ami- nonaphthalene-1-sulfonate, phen = 1,10-phenanthroline), has been prepared by hydrothermal synthesis and structurally characterized by elemental analysis, IR and single-crystal X-ray diffrac- tion. The results determined by XRD reveal that the complex crystallizes in monoclinic, space group P21/c with a = 16.8374(14), b = 16.9825(14), c = 9.9392 (8) , β = 95.9830(10)o, V = 2826.5(4) 3, Mr = 831.86, Dc = 1.955 g/cm3, μ(MoKα) = 6.173 mm-1, F(000) = 1624, Z = 4, the final R = 0.0272 and wR = 0.0694 for 4305 observed reflections (I > 2σ(I)). In the complex, the adjacent lead(II) ions are bridged through the oxygen atoms of sulfonate groups in a syn-syn conformation, yielding an infinite zigzag chain. And the intermolecular N–H···O hydrogen bonds link the chains into two-dimensional layered networks, which are further assembled into a separate two-layer-film-like packing structure.     

Synthesis, Crystal Structure and Luminescent Properties of [Zn（bipy）_2（H_2O）_4]·L·3H_2O

A novel coordination complex [Zn(bipy)2(H2O)4]·L·3H2O (1, bipy = 4,4'-bipyridine, LHNa = aniline-2,5-disulfonic acid monosodium salt) has been synthesized from LHNa by using hydrothermal method and structurally characterized. The result indicates that complex 1 belongs to the monoclinic system, space group P21/c with a = 20.392(3), b = 7.4052(12), c = 23.843(3) , β = 116.253(10)°, V = 3.2291(8) 3, Z = 4, Dc = 1.553 g·cm-3, μ = 0.962 mm-1, F(000) = 1568, and the final R = 0.0497 and wR = 0.1290. The complex 1 has a 0-D discrete structure, and generates an infinite 3-D network with the aid of O–H…O hydrogen bonds and π-π interactions.     

Synthesis,Structure and Catalytic Activity of a Manganese(Ⅲ) Complex Based on 2-(2-Hydroxyphenyl)-5,6-dichlorobenzimidazole Ligands

A new ligand, 2-(2-hydroxyphenyl)-5,6-dichlorobenzimidazole, H2pbmCl2(1), and a novel MnIII complex, [MnIII(HpbmCl2)(pbmCl2)(DMF)2](2),(DMF = N,N-dimethylformamide), have been synthesized and characterized. The crystal of compound 1(C13H8Cl2N2O, Mr = 279.12) belongs to the monoclinic system, space group P21 with a = 3.770(5), b = 25.20(3), c = 5.865(7) , = 92.727(17)o, V = 556.6(12) 3, Z = 2, Dc = 1.665 g/cm3, S = 1.137, μ= 0.568 mm-1, F(000) = 284, the final R = 0.0876 and wR = 0.2334 for 1848 independent reflections. The molecule is planar due to the presence of a strong intramolecular hydrogen bond between O–H group of phenol and N atom of imidazole. H2pbmCl2(1) molecules are arranged into a one-dimensional linear chain through intermolecular hydrogen bonds(N–H···O and C–H···Cl). The crystal of complex 2(C32H27Cl4MnN6O4, Mr = 756.34) belongs to the monoclinic system, space group P21/c with a = 19.043(10), b = 10.808(5), c = 18.704(11), = 115.540(6)o, V = 3473(3) 3, Z = 4, Dc = 1.446 g/cm3, S = 1.3, μ = 0.733 mm-1, F(000) = 1544, the final R = 0.1219 and wR = 0.2681 for 7811 independent reflections. The Mn ion adopts a distorted octahedral geometry coordinated by two deprotonated H2pbmCl2 ligands and two DMF molecules. The [MnIII(HpbmCl2)(pbmCl2)(DMF)2] molecules are arranged into a three-dimensional structure through hydrogen bonds(N–H···N, C–H···N and C–H···Cl) and weak π···πinteractions. The activity measurements suggest that complex 2 is able to serve as a catalyst for H2O2 disproportionation reaction to form O2 in neutral water solution.     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of [Ni（phen）3]-（C8H12O4）-（H2O）14

One novel complex [Ni（phen）3],（C8H12O4）·（H2O）14 with hexane dicarboxylic acid and 1,10-phenanthroline has been hydrothermally synthesized and characterized. Crystal data： monoclinic, space group C2/c, a = 2.3475（5）, b = 1.2208（2）, c = 1.9499（4） nm, β= 114.682（3）°, V = 5.0778（16） nm^3, Dc = 1.339 g/cm^3, Z = 4,μ（MoKa） = 0.458 mm^-1, F（000） = 2168, GOOF = 1.014, R = 0.0401 and wR = 0.0961. The nickel（H） center in the title complex is coordinated with six nitrogen atoms of three 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. However, the nickel（Ⅱ） ion does not coordinate to the hexane dicarboxylic acid. The complex molecules form a 3D structure through hydrogen bonds. TG analysis shows that the title complex is stable below 240.0 ℃.     

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…     

Crystal Structure and Interaction with DNA of [Ni(phen)(mal)(H2O)2]·3H2O

A new complex [Ni(phen)(mal)(H2O)2]·3H2O (phen = 1,10-phenanthroline,mal2-= malonic acid) has been synthesized by the reaction of nickel nitrate,phen and malonic acid.EA,IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the title complex.Crystal data:monoclinic system,space group P2/c,a =8.937(3),b = 12.163(5),c = 9.725(3)(A),β = 119.36°,C15H19N2O9Ni,Mr= 430.03,Z = 2,F(000) =446,V = 921.3 (A)3,Dc = 1.550 g/cm3,μ = 1.104 mm-1,-10≤h≤ 10,-12≤k≤ 14,-11 ≤l≤7,R =0.0261 and wR = 0.0609 for 4376 (Rint = 0.0203) independent reflections and 1631 observed ones (I＞ 2σ(I)).Ni(Ⅱ) exhibits an octahedral coordination geometry,with hydrogen bonds and π-π interactions stabilizing the whole structure.UV spectrum of the complex interacting with protamine DNA indicates that the title compound interacts with DNA via insertion mode with bonding constant Kb of 1.11 × 104.     

Fe(Phen)(CN)4]-: a versatile building block for the design of heterometallic systems. Crystal structures and magnetic properties of PPh4[Fe(Phen)(CN)4]*2H2O and [[Fe(Phen)(CN)4]2M(H2O)2]*4H2O [Phen = 1,10-phenanthroline; M = Mn(II) and Zn(II)

The mononuclear PPh4[Fe(phen)(CN)4]*2H2O (1) complex and the cyanide-bridged bimetallic [[Fe(phen)(CN)4]2M(H2O)2]*4H2O compounds [M = Mn(II) (2) and Zn(II) (3); phen = 1,10-phenanthroline; PPh4 = tetraphenylphosphonium cation] have been synthesized and structurally and magnetically characterized. Complex 1 crystallizes in the monoclinic system, space group P2(1)/c, with a = 9.364(4) A, b = 27.472(5) A, c = 14.301(3) A, beta = 97.68(2) degrees, and Z = 4. Complexes 2 and 3 are isostructural and they crystallize in the monoclinic system, space group P2(1)/n, with a = 7.5292(4) A, b = 15.6000(10) A, c = 15.4081(9) A, beta = 93.552(2) degrees, and Z = 2 for 2 and a = 7.440(1) A, b = 15.569(3) A, c = 15.344(6) A, beta = 93.63(2) degrees, and Z = 2 for 3. The structure of complex 1 is made up of mononuclear [Fe(phen)(CN)4]- anions, tetraphenyphosphonium cations, and water molecules of crystallization. The iron(III) is hexacoordinate with two nitrogen atoms of a chelating phen (2.018(6) and 2.021(6) A for Fe-N) and four carbon atoms of four terminal cyanide groups (Fe-C bond lengths varying in the range 1.906(8)-1.95(1) A) building a distorted octahedron around the metal atom. The structure of complexes 2 and 3 consists of neutral double zigzag chains of formula [[Fe(phen)(CN)4]2M(H2O)2] and crystallization water molecules. The [Fe(phen)(CN)4]- entity of 1 is present in 2 and 3 acting as a bridging ligand toward M(H2O)2 units [M = Mn(II) (2) and Zn(II) (3)] through two cyanide groups in cis positions, the other two cyanide remaining terminal. Two water molecules in trans positions and four cyanide-nitrogen atoms from four [Fe(phen)(CN)4]- units build a distorted octahedral surrounding Mn(II) (2) and Zn(II) (3). The M-O bond lengths are 2.185(3) (2) and 2.105(3) A (3), whereas the M-N bond distances vary in the ranges 2.210(3)-2.258(3) A (2) and 2.112(3)-2.186(3) A (3). The structure of the [Fe(phen)(CN)4]- complex ligand in 2 and 3 is as in 1. The shorter intrachain Fe-M distances through bridging cyano are 5.245(5) and 5.208(5) A in 2 and 5.187(1) and 5.132(1) A in 3. The magnetic properties of 1-3 have been investigated in the temperature range 2.0-300 K. Complex 1 is a low-spin iron(III) complex with an appreciable orbital contribution. The magnetic properties of 3 correspond to the sum of two magnetically isolated spin triplets, the magnetic coupling between the low-spin iron(III) centers through the -CN-Zn-NC- bridging skeleton (iron-iron separation larger than 10.2 A) being negligible. More interestingly, 2 exhibits one-dimensional ferrimagnetic behavior due to the noncompensation of the local interacting spins (S(Mn) = 5/2 and S(Fe) = 1/2) which interact antiferromagnetically through bridging cyano groups. A comparison between the magnetic properties of the isostructural compounds 2 and 3 allow us to check the antiferromagnetic coupling in 2.     

Synthesis and Structural Characterization of {[Mn(phen)_2(OAc)(H_2O)]ClO_4}_2H_2O

1 INTRODUCTION Chemistry of manganese cluster has become an attractive research field because of the involvement of manganese in several biological redox-active sys- tems[1,2], especially in the oxygen-evolving complex (OEC) of photosystem Ⅱ (PSⅡ) in green plants[3]. It was thought that the coordination environment of Mn in OEC contains O and N donors, and the bind- ing of aqua to the Mn site may be important to the oxidation of aqua for the evolution of dioxygen[4, 5]. In recent …     

Crystal Structure and Interaction with DNA of [Ni(phen)(mal)(H_2O)_2]·3H_2O

1 INTRODUCTION In the last few years, much attention has been paid to the molecular structure and biological activity of coordinated complexes in inorganic chemistry field. Ni(Ⅱ) is one of the commonest transition metals with two coordination numbers (4 and 6)[1～3]. Ge- nerally speaking, Ni(Ⅱ) coordination mode depends on the structure of ligand, solvent and reaction con- ditions, among which ligand plays a decisive role and determines not only the molecular structure of the complex bu…     

Crystal Structure of Dimeric Units Cd2（ncpo）2（phen）2（H2O）2 Constructed by Flexible Dicarboxylic Acid with Fluorescent Emission

A dimeric coordination complex Cd2（ncpo）2（phen）2（H2O）2 was constructed by a flexible dicarboxylic acid, 2-nitro-4-carboxylphenoxyacetic acid. Its crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal is of monoclinic system, space group P21/n with a = 17.2616（3）, b = 12.7460（2）, c = 18.4041（3） A^°, β= 94.432（1）°, C42H30Cd2N6O16, Mr = 1099.52, V = 4037.09（12）A^°^3 Dc = 1.809 g/cm^3, F（000） = 2192, μ = 1.139 cm^-1 and Z = 4. The final R = 0.0218 and wR = 0.0703 for 8288 observed reflections with I 〉 2σ（I）. There are two crystallographically independent but structurally very similar molecules in the unit cell of the title complex. It is noticeable that the ligand ncpo^2- displays a good flexibility, demonstrating different modes from the rigid ligands. The luminescence property has been investigated, which shows photoluminescence at 465, 490 and 574 nm upon excitation at 320 nm in the solid state at room temperature.     

Synthesis and Crystal Structure of the Binuclear Complex: [Cu2(phen)2(ip)(Hip)2]·4H2O

A binuclear complex [Cu2(phen)2(ip)(Hip)2]·4H2O has been synthesized by the reaction of Cu(CH3COO)2·H2O, phen(1,10-phenanthroline) and isophthalic acid (H2ip) under hydrothermal condition. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex: monoclinic, space group C2/c, a = 19.214(3), b = 10.6973(14), c = 22.567(3) (A), β = 105.081(2)°,C24H19N2O8Cu, Mr= 526.95, Z = 8, F(000) = 2160, V= 4478.6(10)(A)3, Dc = 1.563 g/cm3, μ = 1.030mm-1, -24≤h≤16, -13 ≤k≤ 13, -28≤l≤28, R = 0.0369 and wR = 0.0819 for 4615 (Rint = 1.0357)independent reflections and 3290 observed ones (I＞ 2σ(Ⅰ)). Structural analysis shows that coordination geometry of Cu(Ⅱ) is a planar square, and the title complex exhibits a 2-D framework supramolecular structure by hydrogen bonds and π-π stacking interactions.     

Hydrothermal Synthesis and Crystal Structure of a Cobalt(Ⅱ) Polymer with One-dimensional Chain Structure: [ Co(phen) (BDC)(H2O)]n·0.5nH2BDC

A metal-organic coordination polymer [Co(phen)(BDC)(H2O)]n·0.5nH2BDC(H2BDC = terephthalic acid, phen = 1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in triclinic, space group P1- with a = 9.771(3), b =10.739(3), c= 11.249(4) (A), α = 75.946(3), β = 65.306(3), γ = 86.073(4)°, V = 1039.6(6)(A)3, C24H17CoN2O7, Mr=504.33, Dc = 1.611 g/cm3, μ(MoKa) = 0.878 mm-1, F(000) = 516, Z = 2, the final R = 0.0547 and wR = 0.1138 for 2916 observed reflections (I＞ 2σ(Ⅰ)). It exhibits a one-dimensional zigzag chain-like structure.     

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…