A two-dimensional coordination polymer [Zn2(DTB)(DMF)4(H2O)2]n has been synthesized by 1,4-dinitro-2,3,5,6-tetracarboxylatebenzenic acid and hydrate zinc perchlorate in the solutions of DMF and H2O. The crystal belongs to the triclinic system, space group P1 with a = 8.887(6), b = 9.225(6), c = 9.828(7) ?, α = 85.249(11), β = 74.863(11), γ = 86.510(13)°, V = 774.4(9), Z = 1, C22H32N6O18Zn2, Mr = 799.28, Dc = 1.714 g/cm3, F(000) = 410 and μ = 1.639 mm-1. The structure was refined to R = 0.0539 and wR = 0.1161 for 1584 observed reflections (I > 2σ(I)). In the complex there exist two kinds of coordination environments for the zinc(II) ions and a two-dimensional sheet is formed via the coordination of carboxylates and zinc(II) ions.
Two two-dimensional coordination polymers, [Cd(μ1,3-SCN-)2(μ1,6-L)]n 1 and [Co(μ1,3-SCN-)2(μ1,6-L)]n 2, have been synthesized with 2,3-dimethylpyrazine-1,4-dioxide (L) and thiocyanate as mixed bridging ligands, and their crystal structures were determined by X-ray crystallography. Both crystals belong to monoclinic system, space group C2/c. The other crystal parameters are as follows: for complex 1: α = 9.732(3), b =14.658(5), c = 8.811(3) A, β = 102.935(4)°, Z = 4, V= 1225.1(7) A^3, C8H8CdN4O2S2, Mr = 368.71, Dc = 1.999 g/cm^3, F(000) = 720 and μ= 2.117 mm^-1; for complex 2: α = 9.528(7), b = 14.563(11), c = 8.415(6) A, β= 102.195(9)°, V= 1141.3(14) A^3, Z = 4, C8H8CoN4O2S2, Mr = 315.23, Dc = 1.835 g/cm^3, F(000) = 636 and μ = 1.863 mm^-1. The two complexes show similar two-dimensional sheet structures. Along the c axis one-dimensional chains are constructed by the coordination of Cd(Ⅱ) (or Co(Ⅱ)) ions with μ1,6-L bridging ligand, and the μ1,3-SCN- bridging ligands make the chains connect to each other, resulting in the formation of a two-dimensional sheet on the ac plane.
The mono-nuclear complex [Cdq3][Cd(qH)3](ClO4)CH3OH has been synthesized by 8-quinolinol and hydrated cadmium perchlorate in methanol solution. The crystal belongs to triclinic, space group P/ with a = 11.1449(15), b = 13.3334(18), c = 17.654(2)A°,α = 85.555(2), β= 88.497(2), γ= 75.681(2)°, V = 2534.1(6) A°^3, Z = 1, C110H86Cd4Cl2 N12O22, Mr = 2448.41, Dc =1.604 g/cm^3, F(000) = 1232 and μ = 0.961 mm^-1. The structure was refined to R = 0.0387 and wR =0.0973 for 7775 observed reflections (1 〉 2σ(I)). In this crystal there exist two independent mononuclear complexes of [Cdq3]^- and [Cd(qH)3]^2+. Each cell contains two [Cdq3]^- anions, two [Cd(qH)3]^2+ cations, two ClO4^- anions and two methanol molecules.
SHI Jing-MinZHANG XiaLU Jian-JunCHEN Yu-QinMA Jian-PingLIU Lian-Dong
The organic salt, (H2Bpy)(cda)2, was synthesized by the reaction of sodium car- bamyldicyanomethanide, 4,4-bipyridyl and manganese(II) perchlorate in water solution. The crystal belongs to monoclinic, space group C2/c with a = 20.333(7), b = 6.177(2), c = 15.566(5) ? b = 116.860(5), V = 1744(1) ?, Z = 4, C18H14N8O2 (Mr = 374.37), Dc = 1.426 g/cm3, F(000) = 776, m = 0.100 mm-1 and l = 0.71073 ? The structure was refined to R = 0.0560 and wR = 0.1072 for 590 observed reflections (I > 2s(I)). Two nitrogen atoms of the 4,4?bipyridyl molecule bonded to two hydrogen ions, resulting this neutral molecule into a divalent cation. Through the interaction of colorless H2bpy cation and colorless cda anion the red neutral organic salt was formed.
A three-dimensional coordination polymer [Mn2(μ1.3-N3)4(μ-PP)2]n (PP = 3-(pyrazin-2-yloxy)-pyridine) has been synthesized with 3-(pyrazin-2-yloxy)-pyridine and azide anion as mixed bridge ligand, and its crystal structure was determined by X-ray crystallography. The crystal data: triclinic system, space group P1, with a = 6.794(4), b = 9.885(6), c = 9.947(6) A, α = 64.170(6), β= 84.190(8), γ= 85.319(8)°, V = 597.7(6)A^3, Z = 1, C18H14Mn2N18O2, Mr = 624.35, Dc = 1.735 g/cm^3, F(000) = 314 and μ = 1.117 mm^-1. In the crystal, the azide anion acts as a bridge ligand and makes adjacent Mn(Ⅱ) ions connect into a two-dimensional sheet on the ab plane, then 3-(pyrazin-2-yloxy)-pyridine serves as a bidentate bridge ligand to connect neighboring sheets along
Two coordination polymers, namely, two-dimensional complex 1 {[Cu(μ- L)1.5(ClO4)2(H2O)].(H2O)0.5]n (L = pyrazine-1,4-dioxide) and one-dimensional complex 2 [Co(μ-L)Br2(H2O)2]n, have been synthesized with pyrazine-1,4-dioxide as bridging ligands, and their crystal structures were determined by X-ray crystallography. Crystal data for complex 1: monoclinic system, space group C2/c, with a = 23.310(3), b = 12.2338(17), c = 10.6075(15) A, β= 110.487(2)°, V = 2833.6(7) A3, Z = 8, C6H9C12CuN3O12.5, Mr = 457.60, Dc = 2.145 g/cm^3, F(000) = 1832 and μ = 1.998 mm^-1; and those for 2: monoclinic system, space group C2/c, with a = 11.012(3), b = 7.483(2), c = 11.451(3) A, β = 101.654(4)°, V = 924.2(4) A3, Z = 4, C4HsBr2CoN2O4, Mr = 366.87, Dc = 2.637 g/cm^3, F(000) = 700 and μ = 10.487 mm^-1. 1 shows a two-dimensional sheet structure on the ac plane through the coordination of μ-L bridging ligands with Cu(Ⅱ) ions, while 2 displays a zigzag one-dimensional chain along the c axis via the coordination of μ-L bridging ligand with Co(Ⅱ) ions. Hydrogen bonds in 1 and 2 make the sheets (or chains) connect each other to form a three-dimensional structure.
SHI Jing-Min XU Hai-Yan ZHANG Feng-Xia WU Chang-Ju LIU Lian-Dong
A three-dimensional complex [Cd(μ1,3-SCN)2(dmpo)]n has been synthesized with μ1,3-SCN^- and dmpo as mixed bridge ligands. The crystal belongs to monoclinic, space group C2/c with a = 15.648(2), b = 15.126(2), c = 11.9773(15) A, β= 112.416(2)°, V= 2620.7(6) ,A, Z= 8, C9H9CdN3OS2, Mr = 351.71, Dc = 1.783 g/cm^3, F(000) = 1376 and μ = 1.967 mm^-1. The structure was refined to R = 0.0260 and wR = 0.0647 for 2186 observed reflections (I 〉 2σ(I)). In the crystal the Cd(Ⅱ) ions are coordinated by ,μ1,3-SCN^- bridge ligands to form the crossing chains on the adjacent planes, and these chains are further joined by μ-dmpo mono-dentate bridge ligands leading to a three-dimensional structure. The complex exhibits strong fluorescent emission property.