Syntheses and Crystal Structures of Two New Iron-sulfur Carbonyl Complexes: [Fe2(SC6H4Cl)2(CO)6]·0.5(Et2O) and [Fe3(SC6H4NH2)6(CO)6]·2(MeOH)

Two new iron-sulfur carbonyl complexes, [Fe2(SC6H4Cl)2(CO)6]·0.5(Et2O) 1 and [Fe3(SC6H4NH2)6(CO)6]·2(MeOH) 2, have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Crystal data for 1: monoclinic, C2/c, a = 18.4439(8), b = 11.0999(5), c = 25.1830(10)(A), β = 97.0370(10)o, V = 5116.8(4)(A)3, Z = 8, C20H13Cl2Fe2O6.50S2, Mr = 604.02, Dc = 1.568 g/cm3, μ = 1.540 mm-1, F(000) = 2424, the final R = 0.0545 and wR = 0.1454 for 3443 observed reflections with I > 2σ(I); 2: monoclinic, P21/n, a = 12.350, b = 26.3050(11), c = 16.057(A),β = 97.891(3)°, V = 5166.9(2)(A)3, Z = 4, C44H44Fe3N6O8S6, Mr = 1144.76, Dc = 1.472 g/cm3, μ = 1.128 mm-1, F(000) = 2352, the final R = 0.0442 and wR = 0.1197 for 7978 observed reflections with I > 2σ(I). Complex 1 contains one iron dimer, in which two tricarbonyliron(I) fragments are bridged together by two 4-chlorophenylthiolate ligands, whereas complex 2 contains a linear tri-iron cluster, in which two terminal tricarbonyliron(II) fragments and the central Fe(II) atom are linked together by six 4-aminophenylthiolate bridging ligands.     

Syntheses and Crystal Structures of Two 3D Zinc(II) Compounds Involving Coordination and Hydrogen Bonds

1 INTRODUCTION Self-assembly through coordination and hydrogen bonds has been proved to be a powerful tool for con- structing functional organic crystalline materials[1~4]. Except for the important role of H-bonds in the sta- bilization of structures, hydrogen bonding groups namely hydroxyl, amide groups in adjacent coor- dination polymeric chains or discrete lamellas can form hydrogen bonds, which allow for the assembly of well-formed crystalline solid[5, 6]. Our recent inte- rest is foc…     

Syntheses, Crystal Structures and Magnetism of Two New Coordination Polymers [Ni（bix）2Cl2]n and [Co（bix）Cl2]n

The self-assembly reactions of MIICl2 (M = Ni, Co) with the flexible bix ligand [bix = 1,4-bis(imidazole-1-ylmethyl)benzene] yielded a 2D network [NiII(bix)2Cl2]n 1 and a 1D chain [CoII(bix)Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231(7), b = 12.7787(9), c = 13.9374(13) , β = 105.419(4)o, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0(2) 3, Dc = 1.518 g/cm3, μ = 0.969 mm-1, F(000) = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections (I > 2σ(I)). Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696(6), b = 10.2128(6), c = 14.4943(9) , C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01(17) 3, Dc = 1.453 g/cm3, μ = 1.334 mm-1, F(000) = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections (I > 2σ(I)). Magnetic properties of the title complexes were also investigated.     

Supramolecular Formation via Hydrogen Bonding in Copper and Nickel Complexes with 2-Hydroxynicotinic Acid

Two complexes,Cu(HnicO)2 1 and Ni(HnicO)2(H2O)2 2 (H2nicO=2-hydroxy-nicolinic acid),were synthesized by hydrothermal reactions and structurally characterized. Complex 1 crystallizes in monoclinic,space group P21/n,with a=8.314(7),b=6.275(4),c=11.283(7),β =98.32(3)°,V=582.5(7)3,Z=2,Mr=339.74,Dc=1.937 g/cm3,F(000)=342,μ=1.908 mm-1,S =1.097,the final R=0.0284 and wR=0.0781 for 1177 observed reflections with I > 2σ(I). Complex 2 crystallizes in monoclinic,space group P21/c,with a=7.438(5),b=12.22(1),c=7.537(5),β=100.07(3)°,V=674.3(8)3,Z=2,Mr=370.95,Dc=1.827 g/cm3,F(000)=380,μ =1.487 mm-1,S=1.041,the final R=0.0335 and wR=0.0779 for 1202 observed reflections with I > 2σ(I). There are extended 3D framework structures in complexes 1 and 2 due to the N–H…O and C–H…O hydrogen bonds. The copper atom in 1 has square planar coordination,while the nickel atom in 2 adopts octahedral coordination geometry. The TG curve shows that complex 2 is stable in solid state to 150 ℃.     

Synthesis,Crystal Structure and Density Functional Theory Studies of 9-Hexyl-3-（（pyridin-4-yl）vinyl）-9H-carbazol

A novel pyridine derivate, 9-hexyl-3-（（pyridin-4-yl）vinyl）-9H-carbazole, was synthesized and characterized by 1H NMR spectra and X-ray diffraction analysis. The complex crystallizes in monoclinic, space group P21/n with a = 9.111（5）, b = 8.239（5）, c = 26.835（5） A, β = 95.340（5）°, Mr = 354.48, V = 2005.6（17） A3, Z = 4, Dc = 1.174 g/cm3,μ = 0.068 mm^-1, F（000） = 760, R = 0.0565 and wR = 0.1550 for 12635 observed reflections （I 〉 2σ（I））. Density functional theory （DFT） calculations were carried out to interpret its UV-Vis spectra, and the results are in agreement with the available experiments.     

Synthesis and Crystal Structure of a One-dimensional Ladder-like Complex [Cu2(L)(dca)2]n (dca = [N(CN)2]-,L = 1,4-Bis(3-furanyl)-2,3-diaza-1,3-butadiene)

A new Cu(I)-dicyanamide with formula [Cu2(L)(dca)2]n (dca = dicyanamide anion, L = 1,4-bis(3-furanyl)-2,3-diaza-1,3-butadiene) has been synthesized and structurally characterized.The complex crystallizes in the monoclinic system, space group P21/n with a = 9.271(2), b = 7.7355(16), c = 11.967(3) -, β = 102.693(3)°, V = 837.3(3) -3, Z = 4, Mr = 223.68, Dc = 1.775 g/cm3, μ(MoKα) = 2.567 mm-1, F(000) = 444, R = 0.0782 and wR = 0.2582 for 951 observed reflections (I > 2σ(I)).Single-crystal X-ray analysis reveals that the copper atom is three-coordinated by two nitrogen atoms from two dicyanamide anions and another one from the ligand, and each copper atom is connected by two [N(CN)2]- anions to form an infinite double-stranded bridge fashion leading to 1D ladder-like motifs.     

Synthesis and Crystal Structure of a 1D Alternate Chain Polymer [Zn2(NBA)2(4,4--bipy)]n

A one-dimensional zinc-containing coordination polymer,[Zn2(NBA)2(4,4'-bipy)]n(NBA = 3-nitrobenzoic acid,4,4'-bipy = 4,4'-bipyrindine),has been solvothermally synthesized and characterized by single-crystal X-ray diffraction,IR and elemental analysis.The crystal structure is of monoclinic,space group C2/c with a = 24.6478(2),b = 14.0964(3),c = 11.4275(2),β =108.7870(10)°,V = 3758.89(11)3,C38H20N6O16Zn2,Mr = 947.34,Z = 4,Dc = 1.674 g/cm3,μ = 1.363 mm-1,F(000) = 1912,R = 0.0720 and wR = 0.2277 for 2841 observed reflections(I > 2σ(I)).In this compound,NBA in syn-syn coordination mode bridges zinc centers into dimeric-zinctetracarboxylate [Zn2(COO)4] secondary building units(SBUs) which are linked through μ-4,4'-bpy affording 1D alternating chains.These adjacent chains are further stacked through intermolecular π···π interactions to form a 3D framework.     

Syntheses and(Crystal Structures of Two New One-dimensional Double Hydrogen-bonding-chain Complexes [Ni(bipy)2Cl]·ClO4 and [Zn(bipy)2Cl]·BF4

Two new transition metal complexes, [Ni(bipy)2Cl]·ClO4 (bipy = 2,2'-bipyridine) 1 and [Zn(bipy)2Cl]·BF4 2, have been synthesized and characterized by single-crystal X-ray diffraction analysis. Both 1 and 2 crystallize in monoclinic space group P21/n with Z = 4. For 1, a = 10.776(1), b = 12.067(1), c = 16.146(2)(A), β= 93.021(2)o, V = 2031.9(4)(A)3, Mr = 505.98, Dc = 1.654 g/cm3, μ = 1.255 mm-1, F(000) = 1032, the final R = 0.0406 and wR = 0.1002 for 3983 observed reflections with Ⅰ ＞ 2σ(I). For 2, a = 10.758(4), b = 12.058(4), c = 16.135(5) (A), β = 104.57(1)o, V = 2025.7(12) (A)3, Mr = 500.00, Dc = 1.639 g/cm3, μ = 1.396 mm-1, F(000) = 1008, the final R = 0.0470 and wR = 0.1237 for 3759 observed reflections with Ⅰ ＞ 2σ(I). The crystal structures of 1 and 2 are isostructural with very similar supramolecular structures. A one-dimen- sional zigzag double hydrogen-bonding-chain is generated by the intermolecular M-bipy …anion…bipy--M hydrogen bonding interactions between the chelating ligands of bipy and anion.     

One-dimensional Inclusion Polymers of Calix[4]arene Monomethoxycarboxylic Acid

X-ray crystal structures of the inclusion complexes of calix[4]arene monomethoxycarboxylic acid 1 （C30H2606） with acetontrile and acetone are reported. The crystal of C30H26O6·CH3CN is of monoclinic, space group P2 1/c with a = 11.691（5）, b = 13.753（5）, c = 17.072（7）A, β = 100.104（7）°, C32H29NO6, Mr = 523.56, V = 2702.4（18）A^3, Z = 4, De= 1.287 g/cm^3, μ（MoKα） = 0.089 mm^-1, T = 293（2） K, 5570 independent reflections with 3220 observed ones （1 〉 2σ（I））, R = 0.0521 and wR = 0.1132 with GOF = 1.042 （R = 0.1055 and wR = 0.1350 for all data）. The data for C30H26O6·CH3COCH3： monoclinic, space group P2 1/c, α = 12.366（4）, b = 12.119（4）, c = 18.796（6） A, β = 90.871（6）°, C33H32O7, Mr = 540.59, V = 2816.6（16）A^3, Z = 4, Dc = 1.275 g/cm^3, μ（MoKα） = 0.089 mm^-1, T = 293（2） K, 5783 independent reflections including 2580 observed ones （I 〉 2σ（I））, R = 0.0555 and wR = 0.1424 with GOF= 0.975 （R = 0.1601 and wR = 0.1884 for all data）. Their architectures exhibit one-dimensional inclusion polymers which are mediated head-to-tail by the guests.     

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…     

Hydrothermal Synthesis, Crystal Structure and Fluorescent Property of a Keggin Polyoxometalate [CuI(2,2''-bipy)2]3[PWⅥ12O40]

A Keggin-type tungstohosphate compound [CuI(2,2'-bipy)2]3[PWVI12O40] 1 (bipy = bipyridine) was prepared by the hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 (C60H48Cu3N12O40PW12) crystallizes in the monoclinic system, space group P21/c with a = 16.9837(10), b = 17.9732(13) c = 27.8701(13)(A), β = 96.1039(10)°, V = 8459.2(9)(A)3, Mr = 4004.89, Z = 4, Dc = 3.145 g/cm3, μ = 17.089 mm-1, F(000) = 7208, S = 1.005, the final R = 0.0469 and wR = 0.0827 for 10807 observed reflections (I > 2σ(I)). Compound 1 consists of one discrete normal Keggin polyanion [PWVI12O40]3- and three isolated coordinated cat- ions [CuI(2,2'-bipy)2]+. Significantly, there exist three crystallographically independent asymmetric reduced copper (I) centers in 1. Furthermore, the compound shows strong photoluminescence property in solid state at room temperature.     

Syntheses and Crystal Structures of Methyl 2-（4,5-Dibromo- 1-methylpyrrole-2-carbonylamino）-3-phenyl propanoate and 4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used as the materials to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great deal of pyrrole derivatives present bioactivities, such as antitumor and antiviral activities[2~5]. Thus, due to the interest in exploring the syntheses of potential bioactive materials which contain pyrrole ring andna…     

Synthesis and Crystal Structure of 1-[4-(Pyrimidin-2-yl)piperazin-1-ylmethyl]-1H-benzotriazole

1 INTRODUCTION Based on the reported 1.65 ? high resolution crystal structure of spinach KARI (ketol-acid reduc- toisomerase) complex[1], we obtained 279 molecules with low binding energy toward KARI from MDL/ ACD 3D database searching, using program DOCK 4.0[2]. These potential structures provide further information for the design of new KARI inhibitors, one of novel derivatives of which as the title com- pound has been synthesized. Its crystal structure will provide us more inf…     

Synthesis and Crystal Structure of a New Dinuclear Copper(Ⅱ) Polymer: [Cu2(bipy)2(Hbtc)2(H2O)2]·(H2O)1/2

A new dinuclear copper(Ⅱ) polymer [Cu2(bipy)2(Hbtc)2(H2O)2]·(H2O)1/2 1 (bipy=2,2'-bipyridine, H3btc = benzene-1,3,5-tricarboxylic acid) was obtained by the hydrothermal single-crystal X-ray diffraction analysis and identified using elemental analysis and IR spectrum.The title complex crystallizes in monoclinic system, space group P21/c with a = 7.2880(5), b =18.4778(13), c = 13.5465(10)(A), β = 95.9580(10)°, C19H14.50CuN2O7.25, Mr = 450.37, V= 1814.4(2)(A)3, Z=4, Dc = 1.649 g/cm3, μ = 1.253 mm-1, F(000) = 918, Rint = 0.0185, the final R = 0.0271and wR = 0.0710 for 2773 observed reflections (I＞2σ(I)). The study results reveal that a pair of distorted square-pyramidal Cu2+ ions are interlinked by bis-monodentate bridging Hbtc2- ligands to constitute a 16-membered ring.     

Synthesis and Structure of a Zinc(Ⅱ)Complex:[Zn(Pybta)·Cl2]n

The title compound, [Zn(Pybta)Cl2]n (Pybta = 1-(2-pyridylmethyl)benzontriazole), has a zigzag chain structure. It crystallizes in the monoclinic system, space group P21/c with a = 9.0103(11), b = 17.0276(18), c = 9.2288(11) A, β = 101.309(6)°, Mr= 346.51, V= 1388.4(3) (A)3, Z= 4, Dc= 1.658 g/cm3, F(000) = 696, μ = 2.143 mm-1, the final R = 0.0492 and wR = 0.1236 for 2545 observed reflections with Ⅰ 2σ(Ⅰ). The Zn atom is four-coordinated by two N and two Cl atoms, forming a slightly distorted tetrahedral geometry. Each zigzag chain links its adjacent symmetry-related equivalents via multiple π-π interactions, which are not frequently observed in the previously reported architectures.     

Synthesis and Crystal Structure of a Novel Zinc Complex[Zn(OH2)(HDPA)2]·3H2O

A new complex [Zn(OH2)(HDPA)2]·3H2O 1 (H2DPA = 2,6-pyridine-dicarboxylic acid) has been prepared at room temperature from the reaction of zinc(II) chloride and 2,6-pyri- dine-dicarboxylic acid in mixed solvent of H2O and EtOH with pyridine, and characterized by X-ray analysis and thermal analysis, exhibiting that the coordination geometry of Zn(II) ion is an octa- hedron. Crystal data: ZnC14H16N2O12, Mr = 469.66, monoclinic, P21/n, a = 7.0067(3), b = 23.8215 (12), c = 10.7404(3)(A), β = 99.823(2)°,V = 1766.40(13)(A)3, Z = 4, Dc = 1.766 g/cm3, F(000) = 960, μ = 1.463 mm-1, R1 = 0.0462 and wR2 = 0.0884 (I > 2σ(I)).     

Synthesis and Crystal Structure of μ1,1,3 Formic Bridging 3D Microporous Ni(Ⅱ) Complex

A μ1,1,3 formic bridging Ni2 complex [Ni3(HCOO)6·H2O]]n 1 has been synthesi-zed under hydrothermal conditions. The single-crystal X-ray diffraction analysis shows that 1 exhibits a 3D open microporous tube formed by covalent and coordination bonds. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 11.1487(13), b = 9.7763(11), c =17.9685(17) A, β= 126.948(6)°, C6H6Ni3O13, Mr = 462.02, V = 1565.2(3) A3 Z = 4, Dc= 1.961 g/cm3, μ = 3.630 mm-1, F(000) = 917.7, Rint = 0.0234, the final R = 0.0234 and wR = 0.0734 for 3469 observed reflections (Ⅰ>2σ(Ⅰ)).     

Synthesis and Crystal Structure of a Dinuclear Cobalt(II) Complex [Co2(1H-benzimidazole)4(1,4-bdoa)2]

1 INTRODUCTION In the last decades, metal carboxylate complexes have become a particularly important subject in mo- dern coordination chemistry owing to their fascina- ting structural diversity and potential applications as functional materials[1～3]. The generation of supramo- lecular architectures relies on the combination of se- veral factors, such as the coordination geometry of metals, bonding of the ligands and reaction condi- tions[4, 5]. In relation to the ligands, the judicious c…     

Synthesis and Crystal Structure of [Zn(HPDB)2(H2O)2]n·2nDMSO·2nH2O (H2-PDB = Pyridine-3,4-dicarboxylic Acid)

The title complex [Zn(HPDB)2(H2O)2]n·(2nDMSO(2nH2O(H2-PDB is pyridine-3, 4-dicarboxylic acid and DMSO the dimethyl sulphoxide) was synthesized under traditional solution condition. Its crystal (C18H28N2O14S2Zn) belongs to monoclinic system, space group P21/c with a = 8.2791(6), b = 12.5495(10), c = 13.6519(11)(A), β = 105.294(2)°, V = 1368.18(18)(A)3, Z = 2, Mr = 625.91, Dx = 1.514 g/cm3, μ = 1.117 mm-1, F(000) = 648, R = 0.0654 and wR = 0.1654 for 2414 observed reflections (I > 2σ(I)). It has a 2-D planar network, in which the Zn atom is six-coor- dinated and hydrogen bonds between carboxylate groups, DMSO and water molecules result in the final 3D structure.     

Synthesis and Crystal Structure of （4S）-5-（2-Methoxy-2-oxoethylamino）-5-oxo-4-（3,4,5-trimethoxybenzamido） Pentanoic Acid

1 INTRODUCTION Aminopeptidase N (APN), a member of mem- brane-bound zinc-dependent exopeptidase, is known to be high expression on the brush border membran- es of the small intestine and renal proximal tubules[1]. The over-expression of APN has been involved in several pathological conditions including cancer[2], leukemia, diabetic nephropathy[3], rheumatoid arth- ritis[4], angiogenesis[5] and central nervous system di- seases, such as Alzheimer’s disease[6]. This has led to the sear…