Synthesis and Crystal Structure of a Binuclear Cobalt(Ⅱ)Carboxylate Complex Co2(O2CCMe3)4(C9H7N)2

Reaction of cobalt carbonate, pivalic acid and quinoline in a refluxing ethanol solvent yielded the dicobalt(Ⅱ) compound, Co2(O2CCMe3)4(C9H7N)2 (1) (C9H7N is quinoline), which has been characterised by elemental analysis, IR and X-ray diffraction method. Crystallographic data: monoclinic, P21/a, a=9.341(2), b=18.591(4), c=11.822(2)(), β=97.71(2), V=2034(1)()3, Z=2, Mr=918.19, Dc=1.27 g/cm-3, F(000)=820, μ(MoKα)=8.60 cm-1, T=293K, final R=0.049, Rw=0.060 for 2715 observed reflections with I>3.0 σ(I). The centrosymmetric molecule comprises a pair of cobalt(Ⅱ) atoms connected by four pivalate ligands in syn-syn bridging modes. Square pyramidal five-coordination of cobalt(Ⅱ) is further completed by a quimoline molecule. The CoⅡ-CoⅡ distance is 2.784(1)().     

cis-Diaquabis（di-2-pyrimidinyl sulfide- K2N,N） Cobalt（II） Ditetrafluoridoborate： Lone Pair-aromatic and Anion-П Interactions in the Self-assembly of Coordination Complex

The title complex, [Co(DprS)2 (H2O)2]2(BF4)4 (DprS is di-2-pyrimidinyl sulfide), was obtained and characterized by elemental analysis, FT-IR and X-ray crystallography. The complex crystallizes in space group P21/c with a=11.742(1), b=22.439(2), c=20.538(2) , β=109.713(5)°, Z=4, V=5094.3(3)3 , Dc=1.692 g·cm-3 , μ=0.929 mm-1 , F(000)=2600, R=0.0756 and wR=0.1929. The asymmetric unit of the title complex is comprised of two isomeric cobalt(Ⅱ) centers (Co(1) and Co(2)) with a cis-[Co(DprS)2(H2O)2]2+ moiety. Each Co(Ⅱ) center exhibits a similar distorted N4O2-octahedral coordination geometry surrounded by a pair of DprS in a N,N’-chelate mode and two aqua ligands in a cis-relationship. Unconventional S···π(pyrimidinyl), N···π(pyrimidinyl), and anion(BF4-)···π(pyrimidinyl) are found to combine with the C H···F and O H···F interactions to stabilize a whole three-dimensional framework with the mononuclear units (Co(1) and Co(2)). The ligand conformation will be also discussed.     

Synthesis and Structure of a Novel Cobalt(Ⅱ)Complex with the Tertiary Carbinol Derivative of Di-4-pyridinylmethanone

The title complex [Co[(4-C5H4N)2C(OH)(NHC3H7)]2(NO3)2]∞ was obtained and characterized through elemental analysis, FT-IR and X-ray crystallography. The complex crystallizes in space group P3(2)21 with a=10.2480(11), b=10.2480(11), c=26.943(6), β=120.00°, [Co[(4-C5H4N)2C(OH)(NHC3H7)]2(NO3)2]∞, C28H34CoN8O8 , Mr=669.56, Z=3, V=2450.5(7)3 , Dc=1.361 g·cm-3 , μ=0.584 mm-1 , F(000)=1047, R=0.0498 and wR=0.1301. The Co(Ⅱ) center exhibits a N4O2-octahedral coordination geometry surrounded by a pair of nitrates at the axial positions and four pyridyl N atoms at the equatorial sites. An infinite double-bridged chain structure with μ2-bridging (4-C5H4N)2C(OH)(NHC3H7) ligands is formed, which is the in situ product of metal-promoted nucleophilic addition reaction of propan-1-amine with di-4-pyridinylmethanone ((4-C5H4N)2CO) in the presence of Co(NO3)2·6H2O. It is the first tertiary carbinol metal complex derived from di-4-pyridinylmethanone so far, and also the rare example of tertiary carbinol derivative of dipyridylmethanone family. The nucleophilic reaction at the carbonyl of dipyridylmethanone in the presence of metal salt will be discussed.     

Synthesis, Crystal Structure and Properties of a Dinuclear Cobalt（II） Complex [Co2（a-furacrylato）4（Phen）2（H2O）]·C2H5OH

A dinuclear cobalt(Ⅱ) complex [Co2(α-furacrylato)4(Phen)2(H2O)]·C2H5OH has been synthesized with α-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crystal is of monoclinic system, space group C2/c with a=1.07388(8), b=2.4300(2), c=1.86708(14)nm, β=104.3830(10)o, V=4.719.4(7) nm3 , Dc=1.503 g/cm3 , Z=2, F(000)=2196, GOOF=1.053, the final R=0.0343 and wR=0.0883. The crystal structure shows that two neighboring cobalt(Ⅱ) ions are linked by the bridging coordination of two α-furacrylic acid anions and one water molecule, and their end positions are respectively coordinated with two 1,10-phenanthroline molecules and two α-furacrylic acid anions, forming a dinuclear structure. Both cobalt(Ⅱ) ions adopt hexa-coordinated distorted octahedral geometry. The electrochemical and fluorescence properties of the title complex are also discussed.     

Synthesis and Crystal Structure of a 1-D Chain Zinc（Ⅱ） Coordinated Polymer with N-p-Tolysulfonyl-glutamine

A novel coordination polymer {[Zn(ts-gln)(bipy)]3H2O}n (ts-glnH2=N-p-toly-sulfonyl-glutamine,bipy=2,2-bipyridine) has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic,space group P212121 with a=8.2622(5),b=16.6244(10),c=18.2807(10) ,V=2510.9(3) 3,C22H28N4O8SZn,Mr=573.91,Z=4,Dc= 1.518 g/cm3,μ(MoKa)=1.115 mm-1,F(000)=1192,the final R=0.0262 and wR=0.0662 for 5691 independent reflections with Rint=0.0240. The zinc(Ⅱ) atom is coordinated by N(3) and N(4) atoms of a bipy molecule,two carboxylate O(1) and O(2A) and amino N(1) atoms of ts-gln ligands,resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc(Ⅱ) ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.     

Synthesis and Crystal Structure of a 1-D Chain Zinc(Ⅱ) Coordinated Polymer with N-p-Tolysulfonyl-glutamine

A novel coordination polymer {[Zn(ts-gln)(bipy)]3H2O}n (ts-glnH2=N-p-toly-sulfonyl-glutamine,bipy=2,2-bipyridine) has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic,space group P212121 with a=8.2622(5),b=16.6244(10),c=18.2807(10) ,V=2510.9(3) 3,C22H28N4O8SZn,Mr=573.91,Z=4,Dc= 1.518 g/cm3,μ(MoKa)=1.115 mm-1,F(000)=1192,the final R=0.0262 and wR=0.0662 for 5691 independent reflections with Rint=0.0240. The zinc(Ⅱ) atom is coordinated by N(3) and N(4) atoms of a bipy molecule,two carboxylate O(1) and O(2A) and amino N(1) atoms of ts-gln ligands,resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc(Ⅱ) ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.     

THE SYNTHESIS AND STRUCTURE OF THE IMIDAZOLATE-BRIDGED HETEROTRINUCLEAR COMPLEX (en)_2Ni[(Im)Co-(NH_3)_5]_2(CIO_4)_6·5H_2O

<正> (H2NC2H4NH2)2Ni [(C3H3N2) Co (NH3)5]2 (CIO4)6 · 5H2O,NiCo2Cl6O29N18C10H62, Mr = 1288. 00, monoclinic, C2/c, a = 31. 832(4), b = 9. 691 (1), c=15. 425(4)(?),β=90. 71(2)°, Z = 4, V = 4758. 0(?)3, Dc=1. 798g/cm3, μ (MoKa) = 15. 22cm-1, F(000)=2656. The three metal nuclei, one Ni( Ⅱ ) and two Co( Ⅲ ), bridged by two imidazolyl anions (Im = C3H3N2), form an isosceles triangle. The Ni( Ⅱ ) atom is situated on the two-fold axis and coordinated by six nitrogen atoms to form a distorted octahedron with two nitrogen atoms from two Im in cis-positions. The two Co( Ⅲ ) atoms are related by C2 symmetry and each Co( Ⅲ ) is coordinated by six nitrogen atoms to form an octahedral configuration.     

Synthesis and Structural Characterization of Co( Ⅱ ) Coordination Polymer [Co(μ-phth)(imi)2]n

A new cobalt( Ⅱ ) complex [Co(μ-phth)(imi)2]n (phth = o-phthalato, imi = imidazole)has been synthesized by the reaction of CoCl2 with disodium o-phthalate and imidazole. The crystal structure of the compound has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group Pn with a = 8.405(1), b = 9.995(1), c = 9.996(2) (A),β= 104.479(2),V= 813.0(2) (A)3, Dc= 1.467 g/cm3, C14H12N4O4Co, Mr= 359.21, F(000) = 366,μ = 1.079 mm-1, Z = 2, R = 0.0483 and wR = 0.1209 for 1583 observed reflections (Ⅰ＞ 2σ(Ⅰ)). In the title complex, the Co(Ⅱ) ions are bridged by o-phthalate ligands in a bidentate mode, producing a zigzag infinite chain structure. Each four-coordinated cobalt( Ⅱ ) center was coordinated by two oxygen atoms and two nitrogen atoms to give a distorted tetrahedral geometry. The chains are linked by hydrogen bonds between oxygen atoms belonging to carboxylate groups and hydrogen atoms of imidazole molecules, forming an unusual two-dimensional coordination polymer.     

SYNTHESIS AND CRYSTAL STRUCTURE OFμ-TEREPHTHALATO BINUCLEAR COBALT(Ⅱ) COMPLEX [Co_2(tpha)(bpy)_4](ClO_4)_2

<正> The structure of μ-terephthalato binuclear cobalt (Ⅱ) complex CCo2(tpha)(bpy)4](ClO4)2(tpha=μ-terephthalato, bpy=2,2' -bipyridine) has been determined by X-ray method. Crystals of title complex are monoelinic, space group P21/c, with a = 13. 086(2), b = 9. 428(2), c=20. 237(4) A. β= 108. 83(1)°, Mr = 1105.61, Z = 2, Dx = 1. 55g/cm3, μ= 8. 09cm-1 and F(000)= 1128. The structure has been solved by direct methods and refined to R=0. 053, The title cation has Ct symmetry in which the terephthalato group acts as bridging ligand between the two metal atoms. Each cobalt(Ⅱ)ion is in a distorted octahedral environment. The Co.....Co distance is 10. 35A.     

Synthesis,Crystal Structure and Properties of the Cobalt(Ⅱ) Complex of Methyl-5-norbornene-2,3-dicarboxylic Acid

A new cobalt complex Co(C10H8N2)(H2O)3[C9H11O2(COO)] with methy-5-norbornene-2,3-dicarboxylic anhydride acid(MNA) and 2,2'-bipyridine as ligands has been synthesized in the mixed solvents of ethanol and water. It crystallizes in monoclinic, space group P21/c with a = 13.0430(13), b = 21.014(2), c = 7.5151(7) ?, β = 102.319(2)o, V = 2012.4(3) ?3, Dc = 1.529 g/cm3, Z = 4, F(000) = 964, GOOF = 1.051, the final R = 0.0457 and wR = 0.0974. The crystal structure shows that the cobalt ion is coordinated with four oxygen atoms from one MNA molecule and three water molecules together with two nitrogen atoms from the 2,2'-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stability and electrochemical properties have studied in this paper.     

From Dinuclear to Mononuclear：Co（Ⅱ） Complexes with Pyridine-2,6-Dicarboxylic Acid（H_2PDA）

Reactions of pyridine-2,6-dicarboxylic acid(H2PDA) with cobalt(Ⅱ) acetate resul-ted in two cobalt(Ⅱ) complexes,[Co(HPDA)2].2H2O.0.5CH3OH(1) and [Co2(PDA)2(H2O)5].2H2O(2),which were characterized by single-crystal X-ray diffraction,IR and electronic absorption spectra.For both complexes,every cobalt atom lies in peudo-octahedral coordination geometry,and the whole structures present 3D frameworks linked by π-π stacking interactions and extensive hydrogen bonds.Magnetic studies showed λ =-83.38 cm-1 for(1) and g = 2.50 and J =-1.38 cm-1 for(2).     

Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Synthesis and crystal structure of dinuclear nickel (Ⅱ) complex

The crystal structure of Ni(Ⅱ) complex with 3-hydroxyl-1, 5-diazacycloheptane-N, N'-diacetate was determined by X-ray diffraction method. Crystal data for Ni2 (C9H14N2O5)2·2H2O: monoclinic, space group P21/n, a = 1.1717(5), b = 0.9794(3), c = 1.2971(2) nm, β= 96.62(3), V= 1.4786(7) nm3, Dc = 1.377 g/cm3, Z = 2,μ=13.321 cm-1 (Mo-Kα), F(000)=640. The final R and Rw are 0.075 and 0.089 respectively. The Ni(Ⅱ) ion forms 2:2 complex with ligand. Two ligands are bridged by two Ni(Ⅱ) atoms which are bridged by two O atoms. Every Ni(Ⅱ) is coordinated by two N atoms and four 0 atoms. The coordination polyhedron of the Ni(Ⅱ) ion is a distorted octahedron.     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Synthesis,Structure,and Magnetic Property of One Novel Entangled Cobalt~Ⅱ-organic Compound

One novel entangled cobalt compound,{[Co 3 (nbta) 2 (4,4-bpy) 2 (H 2 O) 2 ](H 2 O) 2 } n (1,H 3 nbta=5-nitro-1,2,3-benzenetricarboxylic acid,4,4-bpy=4,4-bipyridyl),was prepared and characterized by X-ray diffraction,magnetism,elemental analysis,XPS,TGA and IR spectroscopy.The crystal of 1 crystallizes in monoclinic,space group Pc with a=13.0717(16),b=11.4167(14),c=15.9342(19),β=90.5190(10)o,V=2377.9(5)3,Z=2,C 48 H 36 Co 3 N 8 O 20,M r=1221.64,D c=1.706 g/cm 3,F(000)=1242 and μ(MoKα)=1.128 mm-1.The final R=0.0497 and wR=0.1461 for 4185 observed reflections with I > 2σ(I) and R=0.0721 and wR=0.1619 for all data.X-ray diffraction analyses revealed that Co(1) is linked by the nbta 3-ligands to form the ladder shape along the c axis,which is further extended into two-dimensional networks via the joint of Co(2) along the a axis.Moreover,these two dimensional motifs are interconnected by the 4,4-bpy bridges to form a complicated 3-D polymeric framework.Magnetic measurements revealed that compound 1 shows strong antiferromagnetic property.     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2''-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Crystal Structure of 5—（l—Menthyloxy）—3—chloro—4— Pyrrolidinyl—2（5H0—f

The molecular structure of the title compound 5-(l-menthyloxy)-3-chloro-4-pyrrolidinyl-2(5H)-furanone, C18H28ClNO3(Ⅰ), has been determined by X-ray diffraction at 296(1)K. The crystal is monoclinic with space group P21, a=9.457(3), b=10.413(3), c=9.525(2), β=95.19(2)°, V=934(1) 3, Z=2, Mr=341.88, Dx=1.22 g/cm3, μ=2.15 cm-1, F(000)=368. The final R factor is 0.059, and Rw is 0.065 for 1020 observed reflections with I≥3σ(I). The absolute configuration at C(14) of the acetal carbon was proved to be S, taking into account the known configuration of 1R, 2S, 5R-menthyl moiety. There are three rings in the molecule of this compound: the furanone ring, the pyrrolidine ring and the mentholoxy group ring. The franone ring is connected with the pyrrolidine ring and the mentholoxy ring by N atom and μ2-O bridge atom respectively.     

Synthesis and Crystal Structure of 8-(2,3-Dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo [f] cyclohepta [c] quinoline

The title compound 8-(2,3-dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo[f]-cyclohepta[c]quinoline(C26H25NO2,Mr=383.47) was synthesized and characterized by IR,1H NMR,13C NMR and elemental analysis.The crystal belongs to triclinic,space group P1 with a= 8.1490(16),b=9.2550(19),c=14.373(3) ,α=86.96(3),β=89.66(3),γ=70.32(3)°,Z=2,V=1019.2(4) 3,Dc=1.250 g·cm-3,μ(MoKα)=0.078 mm-1,F(000)=408,the final R=0.0555 and wR=0.1240 for 2228 observed reflections(Ⅰ > 2σ(Ⅰ)).X-ray analysis reveals that the seven-numbered ring is slightly similar to a six-numbered ring,forming the chair-like conformation.The four rings(Ⅰ,Ⅱ,Ⅲ and Ⅳ) in the benzo[f]cyclohepta[c]quinoline moiety form a screw structure.     

Synthesis and Crystal Structure of a Co(Ⅱ) Complex with Taurine-5-methyl-2-hydroxyisophthalaldehyde Schiff Bases [Co(C_(13)H_(16)N_2O_7S_2)(H_2O)_3]_2·H_2O

The title complex CoL(H2O)32·H2O(C26H46N4O21S4Co2),where L = taurine-5-methyl-2-hydroxyisophthalaldehydes,has been synthesized and characterized by IR and X-ray diffraction analysis.The crystal of the complex belongs to the triclinic system,space group P1,with a = 11.197(4),b = 13.309(5),c = 14.486(5),α = 78.827(13),β = 70.547(11),γ = 81.058(13)°,Mr = 996.77,S = 1.08,V = 1987.2(13)3,Z = 2,Dc = 1.666 g/cm3,F(000)= 1032,μ = 1.131 mm?1,R = 0.0633 and wR = 0.1293.According to the structural analysis,the Co(Ⅱ)ion adopts a slightly distorted six-coordinated octahedral geometry.One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom.Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds,thus generating an infinite chain constructed by hydrogen bonds.     

Synthesis and Crystal Structure of Bis{2-bromo- 4-chloro-6-[（2-isopropylammonioethylimino）- methyl]phenolato}bisthiocyanatozinc（Ⅱ）

A Schiff base zinc(Ⅱ) complex [Zn(C12H16BrClN2O)2(NCS)2] was prepared and characterized by elemental analysis,IR and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a=8.414(1),b=9.124(1),c=22.212(3),α=79.177(2),β=86.296(2),γ=89.899(2)o,V=1671.3(4)3,Z=2,Dc=1.631 g/cm3,Mr=820.79,λ(MoKα)= 0.71073,μ=3.444 mm-1,F(000)=824,R=0.0646 and wR=0.1179. A total of 7371 unique reflections were collected,of which 3904 with I > 2σ(I) were observed. The complex crystallizes with two half-molecules per asymmetric unit and each mononuclear molecule is centrosymmetric. The Zn atom lying at the inversion centre is six-coordinated in a slightly distorted octahedral geometry by two phenolate O atoms and two imine N atoms from two Schiff base ligands,as well as two N atoms from two thiocyanate anions. In the crystal structure,the combination of π-π stacking interactions and intermolecular hydrogen bonds (N–H…Br,N–H…O,N–H…N,C–H…O,C–H…S and C–H…Cl) leads to a three-dimensional network.