Synthesis and Crystal Structure of Diaqua(2,2"-Dipyridyl)isothiocyanatoneptunoyl Monohydrate [NpO2(C10H8N2)(NCS)(H2O)2] · H2O

The crystal structure of the complex [NpO₂(C₁₀H₈N₂)(NCS)(H₂O)₂] · H₂O is determined. The unit cell parameters are a= 7.406, b= 9.517, c= 11.518 Å, = 103.65°, = 92.68°, = 96.53°, V= 781.6 ų, space group , Z= 2, (calcd) = 2.257 g/cm³, R= 0.046, R _w= 0.122. The coordination polyhedron of the Np atom is a pentagonal bipyramid with two nitrogen atoms of dipyridyl, a nitrogen atom of isothiocyanate ion, two oxygen atoms of water molecules lying in the equatorial plane, and oxygen atoms of the neptunoyl group lying in the axial positions.     

Synthesis and Crystal Structure of a Macrocycle [Cu(dadm)(mal)(H2O)]2·2H2O

The reaction of 4,4′-diaminodiphenylmethane (dadm), malonic acid (H2mal) and Cu(NO3)2 in aqueous solution results in a discrete binuclear Cu(II) macrocycle: [Cu(dadm)(mal)- (H2O)]2(2H2O. It crystallizes in monoclinic, space group P21/c with a = 15.231(3), b = 11.847(2), c = 9.801(2)A,Z= 106.75(3)o, V = 1693.5(6)A3, Z = 2, C32H40Cu2N4O12, Mr = 799.76, Dc = 1.568 g/cm3, λ(MoK() = 0.71073A, μ = 1.325 mm-1, F(000) = 828, the final R = 0.0531 and Wr = 0.1244 for 3421 observed reflections with I > 2σ(I). Each Cu(II) is coordinated by two oxygen atoms from a mal ligand, two nitrogen atoms from two dadm ligands and a water oxygen atom to form a triangle bipyramidal motif. The title compound possesses a distorted macrocycle enclosed by dadm with approximate dimensions of 8.3A× 5.9A.     

Synthesis, Characterization and Crystal Structure of (2,2′-Bipyridine)(μ-maleato)copper(II) Dihydrate

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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.     

Synthesis and Structure of a Novel Compound [Cu2(EDTA)(Py)2(H2O)2]·2H2O

A novel compound [Cu2(EDTA)(Py)2(H2O)2]·2H2O was synthesized by the reaction of CuSO4(5H2O with H4EDTA in pyridine/water (V/V = 1/4) solvent, and characterized by elemental analysis, IR spectrum and X-ray single-crystal diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 1.26974(6), b = 0.67949(3), c = 1.48548(3) nm, β = 91.454(2)o, V = 1.28122(9) nm3, Z = 2, Dc = 1.673 g/cm3, Mr = 645.56, F(000) = 664, μ(MoKα) = 1.729 mm-1, the final R = 0.0353 and wR = 0.0832 for 1920 observed reflections (I > 2((I)). The compound is a centrosymmetric binuclear molecule with bridged EDTA group. Each Cu(II) atom is linked to two oxygen atoms and one nitrogen atom of EDTA, one oxygen atom of water and one nitrogen atom of pyridine to form a distorted square pyramidal environment. There exist face-to-face π-π stacking interactions between pyridine rings from neighboring molecule with the interplanar distance of 0.3670 nm and hydrogen bonding between EDTA and water molecules.     

Synthesis, Crystal Structure and Luminescence Property of [Co(hmz)2(H2O)4]·2H2O

A new mononuclear Co(Ⅱ) complex, [Co(hmz)2(H2O)4]·2H2O, has been synthesized by the reaction of Co(CH3COO)2·4H2O with 1-(4-hydroxyphenyl)-5-mercaptotetrazole (Hhmz). It crystallizes in the monoclinic system, space group P21/n with a = 13.502(5), b = 6.718(3), c = 13.972(6) (A), β = 117.532(4)°, V = 1123.9(8) (A)3, Z = 2, M r = 553.45, F(000) = 570, Dc = 1.635 g/cm3, μ = 1.008 mm-1, the final R = 0.0272 and wR = 0.0684 for 2194 observed reflections (Ⅰ＞ 2σ(Ⅰ)). The Co(Ⅱ) is six-coordinated by two nitrogen atoms from two hmz-1 ligands and four water molecules, forming an octahedral geometry. The intermolecular hydrogen bonding and offset-panel π-π stacking interactions between the adjacent molecules extend the compound into a three- dimensional supramolecular framework. The title compound emits strong blue fluorescent light (λem(max) = 427 nm) at room temperature and is red-shifted compared with free ligand Hhmz (λem(max) = 342 nm).     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H2O)3}·2H2O]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) (A), β= 108.198(4)°, V=1288.6(6) (A)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.     

Synthesis,structure, and DNA-binding of a new binuclear copper(II) complex: [Cu2(heap)(H2O)2](pic)2 · 2H2O

In this study, a new μ-oxamido-bridged binuclear copper(II) complex [Cu₂(heap)(H₂O)₂](pic)₂ ? 2H₂O, where heap and pic stand for the anion of N,N′-bis(N-hydroxyethylaminopropyl)oxamide and 2,4,6-trinitrophenol, respectively, has been synthesized and characterized by elemental analyses, IR, UV, molar conductance, and single-crystal X-ray diffraction. The complex has an embedded inversion center at the middle of the C–C bond of the oxamido group. Each copper(II) is in a square-pyramidal coordination geometry. The bridging ligand (heap) adopts a bis-tetradentate trans conformation and the oxamido group is in an imidic acid configuration. Hydrogen bonds contribute to a 3-D supramolecular structure in the crystal. The interaction of the binuclear complex with herring sperm deoxyribonucleic acid (HS-DNA) has been investigated by using absorption and emission spectra, electrochemical techniques, and viscometry. The results suggest that the binuclear copper(II) complex interacts with HS-DNA by electrostatic interaction with intrinsic binding constant of 2.67 × 10⁴ (mol L^?1)^?1. The influence of anions on the structure and the interaction of the binuclear complex with HS-DNA were preliminarily discussed.     

Synthesis,Crystal Structure,and Properties of [Dy(p-ABA)3Phen · H2O] · 1.5H2O1

(1.10-Phenanthroline)-tris(4-amidobenzoate)dysprosium, [Dy(p-ABA)₃Phen · H₂O] · 1.5H₂O (where p-ABA = p-amidobenzoate and Phen = 1.10-phenanthroline) has been synthesized. The complex was characterized by elemental analysis, UV, IR spectroscopy, and molar conductance. The crystal structure was determined by X-ray crystallography. The coordination number of the mononuclear complex is nine. The crystals are triclinic, space group P1 with a = 10.4484(13) Å, b = 12.2015(15) Å, c = 14.0170(17) Å; α = 92.800(2)°, β = 102.7220(10)°, γ = 108.880(2)°. Z = 2, d _c = 1.617 mg m^?3, F(000) = 786. R1 = 0.0327, and wR2 = 0.0911.     

Synthesis and Crystal Structure of [Ni(II)(L)(py)_3]·(py)

1 INTRODUCTION Schiff bases and their metal complexes are useful reagents in organic synthesis[1], and they have exhi- bited some biological activities as anticancer and antitumor drugs[2]. The crystal structures and physi- cal and chemical properties of many Schiff bases and their transition metals complexes have been re- ported[3~5]. Further interest in the coordination che- mistry of nickel(II) arises from the role of these complexes in several catalytic reactions, such as electrocat…     

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 [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O

The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nanthroline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10)(A), α = 80.6830(10), β = 66.6480(10), γ = 64.0480(10)o, V = 1554.63(4) (A)3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm3, μ = 0.845 mm-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (I > 2σ(I)). The compound contains a six-coordinated copper(II) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)～2.225(2)(A)), one sulfate O atom (Cu-O = 2.0037(17) (A)) and one water O atom (Cu-O(5w) = 2.719(2) (A)) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.     

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.     

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.     

Synthesis and Structure of anti-Configuration Complex [Cu(tssb)2]·2[(H3O)Cl]·4H2O

The title complex [Cu(tssb)2]·2[(H3O)Cl]·4H2O (C18H34Cl2CuN2O14S2) (tssb = taurine salicylaldehyde Schiff base) has been synthesized by the reaction of taurine salicylaldehyde Schiff base (tssb) and copper acetate in water-ethanol. Its single-crystal structure was determined by X-ray diffraction method. The crystal structure belongs to triclinic, space group P with a = 0.7407(1), b = 1.3329(3), c = 1.5736(3)nm, α = 103.800(4), β = 95.030(4), γ = 104.416(4)°, Mr = 701.06, V = 1.4433(5) nm3, Z = 2, Dc = 1.613 g/cm3, μ = 1.153 mm-1 and F(000) = 726. The compound is an infinitely expanding three-dimensional network connected with hydrogen bonds. The Cu(Ⅱ) atom is coordinated by two nitrogen and two oxygen atoms to form a distorted planar coordination compound which adopts anti-configuration because two sulfonic acid groups are positioned diagonally on a plane.     

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)).     

A Cu(II) Complex with IM-MeImz-κ~2 N,O Mode in [Cu(IM-MeImz)_2]·(SCN)_2: Synthesis, Crystal Structure and Magnetic Properties

A new copper(II) compound with imino nitroxide radicals [Cu(IM-MeImz)2]?(SCN)2 (IM-meImz =2-(5-methylimidazol-4-yl)-4,4,5,5-tetramethyl-2-imidazoline-1-oxyl) has been synthesized and characterized structurally and magnetically. It crystallizes in monoclinic, space group P21/c with a = 9.3604(7), b = 10.3012(7), c = 16.6684(12) , β = 105.0290(10)o, V = 1552.25(19) 3, C24H34CuN10O2S2, Mr = 622.27, Z = 2, Dc = 1.331 g/cm3, μ(MoKα) = 0.876 mm-1, F(000) = 650, the final R = 0.0374 and wR = 0.1079. X-ray analysis demonstrates that the IM-MeImz ligand is coordinated to the copper(II) ion as an unusual didentate chelate with a κ2 N(MeImz),O(IM) mode in the complex. The square-planar coordination sites at Cu(II) are occupied by two O and two N atoms from the imino nitroxide radicals. The complex molecules are connected as a onedimensional polymer structure by intermolecular interactions. Magnetic measurements show that there are intramolecular antiferromagnetic interactions between the Cu(II) ion and radicals.     

A Cu(Ⅱ) Complex with IM-MeImz-к2 N,O Mode in [Cu(IM-MeImz)2]·(SCN)2: Synthesis, Crystal Structure and Magnetic Properties

A new copper(Ⅱ) compound with imino nitroxide radicals [Cu(IM-MeImz)2]·(SCN)2 (IM-meImz =2-(5-methylimidazol-4-yl)-4,4,5,5-tetramethyl-2-imidazoline-1-oxyl) has been synthesized and characterized structurally and magnetically. It crystallizes in monoclinic, space group P21/c with a = 9.3604(7), b = 10.3012(7), c = 16.6684(12) (A), β = 105.0290(10)°, V = 1552.25(19)(A)3, C24H34CuN10O2S2, Mr = 622.27, Z = 2, Dc = 1.331 g/cm3, μ(MoKα) = 0.876 mm-1, F(000) =650, the final R = 0.0374 and wR = 0.1079. X-ray analysis demonstrates that the IM-MeImz ligand is coordinated to the copper(Ⅱ) ion as an unusual didentate chelate with a κ2 N(MeImz),O(IM) mode in the complex. The square-planar coordination sites at Cu(Ⅱ) are occupied by two O and two N atoms from the imino nitroxide radicals. The complex molecules are connected as a onedimensional polymer structure by intermolecular interactions. Magnetic measurements show that there are intramolecular antiferromagnetic interactions between the Cu(Ⅱ) ion and radicals.     

Synthesis,spectroscopic, and biological activities of two binuclear complexes [Cu(II)(1-phenylamidino-O-methylurea)2(H2O)]2(Cl2)2 and [Cu(II)(1-phenylamidino-O-i-butylurea)tmen]2(Cl2)2·2H2O

EPR spectra of two copper(II) binuclear complexes, [Cu(II)(1-phenylamidino-O-methylurea)₂(H₂O)]₂(Cl₂)₂ (1) and [Cu(II)(1-phenylamidino-O-i-butylurea)tmen]₂(Cl₂)₂?·?2H₂O (2), at room temperature showed fine structure transitions (ΔM _s?=?±1) and a very weak half-field signal corresponding to forbidden transitions (ΔM _s?=?±2). The spectrum of 1 showed disappearance of normal and half-field transitions when cooled to 77?K, suggesting antiferromagnetical coupling dicopper complex which is also supported by the low magnetic moments (µ _eff?=?1.64?B.M.). The isotropic exchange interaction constant J (41?cm^?1) for 2 indicated that interaction between the two spins of the binuclear complex is ferromagnetic, confirmed from the high magnetic moment value (µ _eff?=?2.25?B.M.). The binding of these complexes with calf thymus DNA suggested that these complexes interact with DNA by electrostatic or groove binding, not by intercalation. The two complexes have good antibacterial activity against tested bacteria responsible for urinary tract infection.     

Synthesis,Crystal Structure and Spectral Properties of [Ce(NO3)5(H2O)2]·2(Hphen)·(H2O)

A novel complex [Ce(NO3)5(H2O)2]·2(Hphen)·(H2O) (phen =1,10-phenanthroline) with formula C24H24CeN9O18 and Mr = 866.64 has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group Pī with a = 7.5534(2), b = 8.083(2), c = 25.8377(6) A, α = 86.847(1), β = 89.937(1), γ = 86.981(1)o, V = 1572.94(6) A3, Dc = 1.830 g/cm3, F(000) = 866, β = 1.545 cm-1 and Z = 2. The final refinement gave R = 0.0486 and wR = 0.1278 for 4852 observed reflections with I > 2σ(I). It consists of discrete [Ce(NO3)5(H2O)2]2- anion, two Hphen+ cations and a lattice water molecule. In the compound, all of the five nitrates are bidentate, and the coordination of Ce(III) is 12. The photo-luminescence of this compound was also investigated.