A mercury(Ⅱ) iodide complex with organosulfide [Hg(pymt)(pymtH)I] 1 (pymt = the anion of pyrimidine-2-thiolate) has been synthesized by slow evaporation of the solution at room temperature and structurally characterized by single-crystal X-ray diffraction. Basic ideas and data collected are given. X-ray diffraction analysis reveals that complex 1 is mononuclear. Crystallographic data: C8H7HgIN4S2, Mr = 550.79, monoclinic system, space group P21/c, a = 11.218(4), b = 9.551(3), c = 15.877(4) A^°, β = 129.697(15)°, V = 1308.9(7) A^°^3, Z = 4, Mr = 550.79, Dc = 2.795 g/cm^3, F(000) = 995, μ(MoKa) = 14.415 mm^-1, 2(MoKa) = 0.71073 A^°, T= 293(2) K, 2θmax = 54.9°, GOOF= 1.053, the final R = 0.0310 and wR = 0.0742 for 2547 observed reflections with I 〉 2σ(I) (refinement on F^2). Complex 1 is connected through hydrogen bonds to give a one-dimensional supramolecular chain structure. Furthermore, π-π interactions are also found between the pyrimidine rings with the center-to-center distances of 3.439(4) and 3.603(4) A^°, so complex 1 expands the chains into a two-dimensional network.
The title complex cis-bis(tetrahydrothiophene)-bis(nitrate) platinum(H), (tht)2Pt(NO3)2, was the reducing product from potassium hexachloroplatinate(IV) K2PtC16 where the platinum is tetra-valenced. Crystal data for CsH16N206PtS2: monoclinic, space group P21/c, a = 9.8833(5), b = 8.6744(4), c = 18.6407(9)A,β = 114.401(3)°, V = 1455.35(12)A3 Z = 4, Mr = 495.44, Dc = 2.261 g/cm3, F(000) = 944,μ = 9.950 mm-1, 2(MoKa) = 0.71073 A, T= 293(2) K, 2θmax = 54.96°, GOOF = 1.033, R = 0.0350 and wR = 0.0785 for 2572 observed reflections with I 〉 2σ(I). X-ray diffraction studies reveal that the title complex has interesting weak metal-metal interactions and two molecules linked by metal-metal interaction exist as a group. Luminescent spectrum illuminates red emission of the complex at room temperature.
The title compound [In(H2ip)(pdc)(H2O)] (H3ip = 5-hydroxyisophthalic acid, H2Pdc = pyridine-2,6-dicarboxylic acid) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 13.830(8), b = 6.488(4), c = 17.632(10)A^°, β = 92.510(10)°, C15H10InNO10, Mr= 479.06, V = 1580.6(15)A^°3, Z = 4, De= 2.013 g/cm^3, F(000) = 944,μ = 1.557 mm^-1, the final R = 0.0413 and wR = 0.0793 for 2950 observed reflections with I 〉 2σ(I). The In(Ⅲ) ion is seven-coordinated in a slightly distorted penta-bipyramidal geometry. The mixed ligands connect the In(Ⅲ) ions into 21 helical chains along the [010] direction, and the hydrogen bonds assemble the chains into a three-dimensional supramolecular network.
The reaction of 2,4,6-tris(2-pyridyl)-1,3,5-triazine (tptz) and K2PdCl4 in THF/H2O (10:1) results in the hydrolysis of tptz to bis(2-pyridylcarbonyl)amide anion (bpca), and affords complex Pd(bpca)Cl 1, which is the first example of Pd(Ⅱ)-promoted hydrolysis of ligands. Crystal data for 1: orthorhombic, space group Pbcn, a = 12.0136(17), b = 14.180(2), c = 6.9747(11)A, V= 1188.2(3) A3, Z = 4, Mr = 368.06, Dc = 2.058 g/cm3, F(000) = 720,μ = 1.786 mm^-1, λ(MoKα) = 0.71073 A, T= 293(2) K, 2θmax = 54.9°, GOOF = 1.085, the final R= 0.0647 and wR = 0.1051 for 1234 observed reflections with I 〉 2σ(I) (refinement on F2). Complex 1 is connected through hydrogen bonding to give a 2D network. And weak Pd...Pd interactions are also found between adjacent molecules with the distance of 3.6074(5) A, so the complex is further extended into a 3D supramolecular structure. Thermal gravity analysis (TGA) shows that 1 exhibits high thermal stability below 310℃. X-ray powder diffraction (XRD) and UV/Vis spectrum of 1 are also discussed.
The title complex,[Zn(ip)2(H2O)2][ZnCl4]·H2O·2DMF 1(ip=imidazo[4,5-f][1,10] phenanthroline),has been synthesized via the slow evaporation of concentrated reaction solution at room temperature.It was characterized by single-crystal X-ray diffraction.Crystal data for C32H36Cl4N10O5Zn2:white prism,0.17mm×0.15mm×0.10mm,monoclinic,space group P2/c,a=11.928(8),b=9.868(6),c=16.520(11),β=104.879(12)°,V=1879(2)3,Z=2,Mr=913.25,Dc=1.614 g/cm3,F(000)=932,μ=1.616 mm-1,λ(MoKα)=0.71073,GOOF=1.045,R=0.0710 and wR=0.1755 for 3055 observed reflections with I 〉 2σ(I). X-ray diffraction study reveals that the title complex has an interesting 3D architecture via hydrogen bonding interactions and π-π interactions. The IR, TGA, XRD and luminescent properties of complex 1 were also studied.
A new coordination polymer {[In(bdc)(OH)]·4H2O}n(H2bdc=1,4-benzenedi-carboxylic acid) has been synthesized through hydrothermal conditions,and was characterized by X-ray single-crystal diffraction and other measurements.The complex crystallizes in the orthorhombic system,space group Imma with a=18.3621(13),b=7.1932(5),c=11.8278(8),V=1562.24(19)3,Z=4.Dc=1.565g/cm3,Mr=368.00,F(000)=728,μ(MoKα)=1.542 mm–1,S=1.019,R=0.0468 and wR=0.1326 for 884 observed reflections(>2σ(Ⅰ)).The title compound represents a 3-Dframework containing four kinds of tunnels in different shapes and sizes.
The title compound {[Cu4(OH)4(2,2'-bpy)4(bqdc)]·2ClO4}n 1 (bqdc = 2,2'-biquinoline-4,4'-dicarboxylic acid) has been synthesized by hydrothermal method. Its crystal structure is of triclinic, space group P1^- with a = 7.6561(5), b = 12.4652(8), c = 15.7501(10) A, α= 80.0480(10), β= 87.7900(10), γ = 74.0800(1)°, V = 1423.65(16) A^3, Z = 2, C30H23ClN5O8Cu2, Mr = 744.06, Dc = 1.736 g/cm^3, μ = 1.651 mm^-1, F(000) = 754, the final R = 0.0421 and wR = 0.1163 for 4973 observed reflections with Ⅰ〉 2σ(Ⅰ). In 1, tetra-copper chair-like clusters of [Cu4(OH)4(2,2'-bpy)4]^4+ are connected by bqdc ligands to form one-dimensional chains, which are further connected by hydrogen bonds to generate a two-dimensional supramolecular network .
The title compound, [Pd(2,2′-bipy)2](Haadip)2·4H2O, was synthesized via the hydrothermal reaction of PdCl2 with 5-aminodiacetic isophthalic acid (H4adip) in an acetic acid water solution. It was characterized by elemental analysis and infrared spectrum. Crystal data for C44H44N6O20Pd: monoclinic, space group P21/n, a = 11.0674(2), b = 9.9716(2), c= 20.5770(3)A, β = 92.7300(3)°, V = 2268.29(7)A^3, Z = 2, Mr = 1083.25, Dc = 1.586 g/cm^3, F(000) = 1112,μ = 0.499 mm^-1, 2(MoKa) = 0.71073 A, T = 293(2) K, 2θmax = 51.38°, GOOF = 1.067, R = 0.0268 and wR = 0.0710 for 3770 reflections with 1 〉 2σ(I). X-ray diffraction studies reveal that the title compound has an interesting 3D microporous architecture via hydrogen bonds with the cations located inside the channel.