Synthesis and Crystal Structure of a Novel 1D Mercury（II） Iodide Coordination Polymer Containing 40-Membered Macrocycle

A mercury coordination polymer [Hg3(TizT)2I6]n (Mr = 1921.72, TizT = 2,4,6- tri(imidazole-1-yl)-1,3,5-triazine) containing a 40-membered macrocycle which was constructed by four TizT ligands and four mercury(II) iodide molecules had been synthesized by the reaction of HgI2 with TizT. The complex was characterized by elemental analysis, FT-IR, 1H NMR spectra and X-ray crystallography. The crystal of the complex belongs to the monoclinic system and C2/c space group with a = 35.840(5), b = 8.169(5), c = 14.980(5) , β = 104.466(5)°, Z = 4, V = 4247(3) 3, Dc = 3.006 g·cm-3, μ = 15.223 mm-1, F(000) = 3384, Rint = 0.0504, wR = 0.0833 and constructs a chair-like conformation of cyclohexane one by one, which forms a 1-D polymer through the fashion of fused ring aromatic hydrocarbon. The hydrogen bonds and π-π interactions shape the 2-D network structure. The two compounds excited weak fluorescence.     

Synthesis,Crystal Structure and Band Structure of Tb3Co4Sn（13）

A new intermetallic compound,Tb3Co4Sn13,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.Tb3Co4Sn13 crystallizes in cubic,space group Pm3n(No.223) with a = 9.5072(2) ,V = 859.33(3) 3,Z = 2,Mr = 2255.45,Dc = 8.717 g/cm3,μ = 34.369 mm-1,F(000) = 1906,and the final R = 0.0140 and wR = 0.0312 for 199 observed reflections with I > 2σ(I).The structure of Tb3Co4Sn13 belongs to the Yb3Rh4Sn13 type.It is isostructural with RE3Co4Sn13(RE = La,Ce),featuring a 3D [Co4Sn12] framework based on [CoSn6] trigonal prisms.The [CoSn6] trigonal prisms are interconnected via corner-sharing and Sn-Sn bonds to form a 3D [Co4Sn12] framework.The other Sn and Tb atoms are located in the spacers of the 3D framework.Band structure calculations indicate that Tb3Co4Sn13 is metallic.     

A Two-dimensional Metallic Oxide Constructed from Molybdenum Clusters and Ag（Ⅰ）-[3-（2-pyridyl）-pyrazole] Cationic Coordination Components

A new polyoxomolybdate compound [Ag 3 (HL) 4 ](PMo 12 O 40)] 1 (HL=3-(2-pyridyl)pyrazole) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.375(3),b=12.076(3),c=13.196(4),α=84.170(4),β=71.961(3),γ=86.326(4)°,V=1563.1(7)3,C 32 H 28 Ag 3 Mo 12 N 12 O 40 P,M r=2726.52,D c=2.897 g/cm 3,μ(MoKα)=3.366 mm 1,F(000)=1284,Z=1,the final R=0.0587 and wR=0.1312 for 4139 observed reflections (I > 2σ(Ⅰ)).X-ray diffraction analyses reveal that the PMo 12 O 40 3clusters in compound 1 are linked by four Ag 3 (HL) 4 3+ units via the terminal oxygen atoms to form a two-dimensional architecture.The symmetrical unit of Ag 3 (HL) 4 3+ exhibits two distinct Ag(Ⅰ) environments:a two-coordinate {AgN 2 } site and a five-coordinate {AgN 3 O 2 } site which links to two molybdate clusters.     

Synthesis and Crystal Structure of 3-（4-Chlorophenyl）-8-cyano-2-（di-isopropylamino）-5-methyl-7-（methylthio）-pyrido[4,3-d]pyrimidine-4（3H）-one

The crystal structure of the new title compound 3-(4-chlorophenyl)-8-cyano-2-(di-iso-propylamino)-5-methyl-7-(methylthio)-pyrido[4,3-d]pyrimidine-4(3H)-one(C22H24ClN5OS,Mr = 441.97)has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic,space group Pna21 with a = 7.6721(5),b = 18.9370(11),c = 15.6260(9),V = 2270.2(2)3,Z = 4,Dc = 1.293 g/cm3,F(000)= 928,μ = 0.283 mm-1,MoKa radiation(λ = 0.71073 ),R = 0.0494 and wR = 0.1062 for 3278 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the py-ridopyrimidinone moiety are almost coplanar. Intramolecular C(20)-H(20)···N(4),C(19)-H(19A)···N(3),C(18)-H(18C)···N(3)and C(16)-H(16B)···O(5)hydrogen bonds together with weak C···π interactions are found in the structure.     

Syntheses and Characterization of Two Diiron Dithiolate Complexes Containing 4-Dimethylaminopyridine

Two diiron dithiolate complexes, (μ-pdt)Fe2(CO)5(C7H10N2) 3 and (μ-edt)-Fe2(CO)5(C7H10N2) 4 (pdt = -S(CH2)3S-, edt = -S(CH2)2S-), have been synthesized and characterized by single-crystal X-ray diffraction. Complex 3 crystallizes in the monoclinic system, space group P21/c with a = 10.168(4), b = 11.816(4), c = 16.595(7)  and β = 95.195(6)o; and complex 4 crystallizes in the orthorhombic system, space group P212121 with a = 9.317(3), b = 11.898(4), c = 34.006(10)  .The distances of Fe(1)–Fe(2) are 2.5058(9)  in 3 and 2.4942(10)  in 4, falling in the normal range of Fe–Fe bond length (2.49～2.57 ). The cyclic voltammograms show that 3 and 4 display irreversible reduction peaks (FeIFeI/ FeIFe0) at –1.717 V and –1.673 V vs. Ag/AgCl, respectively. With different acids, complex 3 has distinguishable behavior, two protonations in addition of HBF4-Et2O and single protonation besides HOAc-CH3CN, and complex 4 has a similar action to 3 with HOAc-CH3CN for a semblable structure.     

Synthesis and Crystal Structure of the Diiron Azadithiolate Complex [（μ-SCH_2）_2NPh]Fe_2（CO）5（Ph_2PCH_2PPh_2）

Reaction of [(μ-SCH2)2NPh]Fe2(CO)6 with Ph2PCH2PPh2 in the presence of Me3NO·2H2O gave the title complex [(μ-SCH2)2NPh]Fe2(CO)5(Ph2PCH2PPh2)(1)in 78% yield.The new complex 1 was characterized by elemental analysis,spectroscopy and X-ray crys-tallography.It crystallizes in triclinic,space group P1 with a = 10.832(2),b = 12.003(2),c = 15.579(3),V = 1785.6(6)3,Z = 2,C32H26Fe2NO5PS2,Mr = 819.40,Dc = 1.524 g/cm3,μ(MoKα)= 1.064 mm-1,F(000)= 840,T = 113(2)K,the final R = 0.0543 and wR = 0.1218 for 6203 observed reflections(I > 2σ(I)).The Ph2PCH2PPh2 ligand resides in an axial position of the square-pyramidal coordination sphere of the Fe atom and trans to the benzene ring in order to reduce the steric repulsion between Ph2PCH2PPh2 and the benzene ring.     

Hydrothermal Synthesis and Crystal Structure of a 2D Zinc（Ⅱ） Coordination Polymer with 5-Hydroxynicotinic Acid

The title compound,[Zn(5-hydroxynicotinate) 2 2H 2 O] n,has been synthesized by reacting zinc sulfate vitriol with 5-hydroxynicotinic acid under hydrothermal conditions,and its structure was determined by X-ray crystallography with the following data:monoclinic,space group C2/c,C 12 H 12 N 2 O 8 Zn,M r=377.61,a=10.223(3),b=10.319(3),c=13.613(4),β=105.922(6)°,Z=4,V=1380.9(8)3,F(000)=768,D c=1.816 g/cm 3,μ(MoKα)=1.826 mm-1,the final R=0.0401 and wR=0.1380 for 1157 observed reflections (I > 2σ(I)).In the structure of the title compound,the Zn II ion located in an inversion center lies in a distorted tetrahedral environment at a N 2 O 2 coordination mode,and the 5-hydroxynicotinic acid ligand links symmetry-related Zn II ions at a μ 2-N,O bridging way forming a two-dimensional covalent structure.In the crystal,solvent water molecules form intermolecular O-H O hydrogen bonds and pyridine rings of adjacent layers form π-π stacking (3.346),which connect adjacent two-dimensional sheets into a three-dimensional supramolecular network.     

Synthesis and Crystal Structure of N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Synthesis,Crystal Structure and Photoluminescence Property of a Ni（Ⅱ） Coordination Polymer with One-dimensional Double-sinusoidal Structure

A new coordination polymer [Ni(3-bpo)(m-bdc)(C2H5OH) 2]n(1,3-bpo = 2,5-bis(3-pyridyl) -1,3,4-oxadiazole,m-H2bdc = 1,3-benzenedicarboxylic acid) was solvothermally synthesi-zed and characterized by IR,TGA and single-crystal X-ray diffraction. The title complex crystalli-zes in the orthorhombic system,space group Pnma with a = 7.786(3) ,b = 17.253(6) ,c = 18.478(6) ,V = 2481.9(14) 3,Mr = 539.18,Dc = 1.443 g/cm3,Z = 4,R = 0.0353 and wR = 0.0589. The m-bdc and 3-bpo bridge two Ni(Ⅱ) ions through two carboxylate groups and two pyridyl groups forming a 1D infinite double-sinusoidal chain along the c axis. The photoluminescence of 1 shows a large red shift compared to that of free ligands in the solid state.     

Synthesis and Crystal Structure of a Dinuclear Complex of Cu（II） with Tetra（3,5-diphenyl pyrazole）

A Cu(II) complex of tetra(3,5-diphenyl pyrazole) [Cu(C15H12N2)2Cl2]2 (1) was synthesized, and its structure was determined by single-crystal X-ray diffraction and further characterized by elemental analysis, NMR and IR. 1 belongs to the monoclinic system, space group P21/c with a = 13.3780(5), b = 15.1392(6), c = 15.5923(6) , β = 124.522(2)°, Z = 2 and V = 2601.86(17) 3. In 1, each Cu2+ ion is coordinated with two N atoms from two tetra(3,5-diphenyl pyrazole) ligands and three Cl- anions to give a distorted square-pyramidal geometry, which is further linked through edge-sharing bridging by Cl- anions to form a centrosymmetric dinuclear structure.