Crystal Structure and Spectroscopic and Coordination Properties of Bis（4-fluorobenzohydroxamato）dimethyltin（Ⅳ）

An organotin（Ⅳ） complex [（CH3）2Sn（4-FC6H4CONHO）2] has been synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction techni- ques. The crystal belongs to the orthorhombic system, space group Pbca with a = 9.7565（13）, b = 17.664（2）, c = 20.784（3）A, Z = 8, V = 3581.9（8）A^3 Dc = 1.695 g/cm^3,μ（MoKa） = 1.469 mm^-1, F（000） = 1808, R = 0.0321 and wR = 0.0838. In the molecular structure of the title complex, the tin atoms are five-coordinated in a trigonal bipyramidal geometry, and the special coordination properties of dimethyltin（Ⅳ） with hydroxamate-type ligands are also discussed.     

Synthesis,Crystal Structure and Spectroscopic Properties of Zn(Ⅱ) with N-carbamylglutamate Ligand

Zn C6H8N2O5.H2O(NCGZn) has been synthesized, and its functional groups present in the title compound were confirmed by elemental analysis, TG and IR spectral studies. Meanwhile, the crystal of NCGZn was obtained by slow evaporation of a saturated aqueous solution at room temperature and confirmed by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P21 with a = 5.03220(1), b = 13.3747(4), c = 12.9944(4) , β = 92.987(2)o, V = 873.39(4) 3, Z = 2, C12H20N4O12Zn2, Mr = 543.10, Dc = 2.065 g/cm3, F(000) = 552, μ(Mo Ka) = 2.826 mm-1, R = 0.0422 and w R = 0.1142. In NCGZn, Zn(1) and the symmetry formed Zn(1) ions are connected by five atoms from four NCG-2H anions and a water molecule. A NCG ligand has two carboxylate groups, one connecting a Zn ion, and the other bridgiong two Zn ions. The NCG ligand bridges four Zn ions through the amino group and two carboxylate groups with a water molecule to yield a 3D coordination polymer structure with hydrogen bonds.     

Supramolecular Ribbons. Crystal Structure and Spectroscopic Properties of 2,2′-Bipyrroyl

 A crystal structure determination of 2,2′-bipyrroyl (1; 2,2′-dipyrryl-diketone, bis (2-pyrrolyl)ethanedione) and its spectroscopic properties in solution are reported. In the crystal, 1 self-assembles via hydrogen bonding into supramolecular ribbons that extend indefinitely through the crystal lattice. The observed molecular conformation is one where each pyrrole ring and adjacent carbonyl group are co-planar (torsion angle ∼ 0.9°), with the N-H pointing in the same direction as the C=O. The two carbonyls have a transoid but not co-planar geometry with a torsion angle of ∼128°. Adjacent molecules in the crystal are linked by pairs of intermolecular hydrogen bonds, pyrrole NH to carbonyl oxygen, to form a matrix of polymeric chains that lie like neatly stacked, parallel streams of ribbons. Molecular mechanics calculations on the monomer indicate an intra-molecularly hydrogen bonded planar conformation (sp, ap, sp) at the global energy minimum. In CHCl₃, 1 is monomeric according to vapor pressure osmometry (MW _obs=179±10 vsċMW _calc=188). In THF, the measured molecular weight is 340±15, which corresponds best to one molecule of 1 solvated by two THF molecules (MW=322 for C₁₀H₈N₂O₄ċ2 C₄H₈O) rather than to a dimer.     

Supramolecular Ribbons. Crystal Structure and Spectroscopic Properties of 2,2′-Bipyrroyl

Summary.  A crystal structure determination of 2,2′-bipyrroyl (1; 2,2′-dipyrryl-diketone, bis (2-pyrrolyl)ethanedione) and its spectroscopic properties in solution are reported. In the crystal, 1 self-assembles via hydrogen bonding into supramolecular ribbons that extend indefinitely through the crystal lattice. The observed molecular conformation is one where each pyrrole ring and adjacent carbonyl group are co-planar (torsion angle ∼ 0.9°), with the N-H pointing in the same direction as the C=O. The two carbonyls have a transoid but not co-planar geometry with a torsion angle of ∼128°. Adjacent molecules in the crystal are linked by pairs of intermolecular hydrogen bonds, pyrrole NH to carbonyl oxygen, to form a matrix of polymeric chains that lie like neatly stacked, parallel streams of ribbons. Molecular mechanics calculations on the monomer indicate an intra-molecularly hydrogen bonded planar conformation (sp, ap, sp) at the global energy minimum. In CHCl₃, 1 is monomeric according to vapor pressure osmometry (MW _obs=179±10 vsċMW _calc=188). In THF, the measured molecular weight is 340±15, which corresponds best to one molecule of 1 solvated by two THF molecules (MW=322 for C₁₀H₈N₂O₄ċ2 C₄H₈O) rather than to a dimer. Received October 21, 1999. Accepted November 2, 1999     

Crystal Structure and Luminescent Properties of a Zn(Ⅱ) Coordination Polymer Assembled by Mixed-ligand

A Zn(Ⅱ) coordination polymer [Zn(NIP)(3,3'-bpt)]·H2O(1, NIP = 5-nitroisophthalate, 3,3'-bpt = 1H-3,5-bis(3-pyridyl)-1,2,4-triazolate) has been synthesized by the hydrothermal reaction at 140 ℃ and structurally characterized by IR spectroscopy, X-ray diffraction, thermal analysis, single-crystal X-ray diffraction and luminescent properties. In complex 1, the zinc atom is five-coordinated with three carboxylate oxygen atoms from three H2 NIP and two nitrogen atoms from two 3,3'-bpt, respectively, forming a distorted trigonal bipyramidal geometry and showing a 1D chain structure, which is further bridged by NIP to form a 3D supramolecular network via self-assembly of hydrogen bonds.     

Synthesis and Crystal Structure of a New Zinc(Ⅱ) Coordination Polymer Assembled by 4-Nitrophthalic Acid and Bis(imidazol) Ligands

A new complex [Zn(4-nph)(bib)]_(2n)·nH_2O(1) has been obtained by the reaction of metal(Zn(Ⅱ)),1,4-bis(imidazol-1-yl)-butane(bib) with 4-nitrophthalic acid(4-H_(2nph)).The crystal structure of 1 has been determined by single-crystal X-ray diffraction analysis.Compound 1 is of triclinic system,space group P1 with a = 10.3251,b = 12.4503,c = 16.6497 ?,α = 88.487(3),β = 72.529(3),γ = 79.991(3)°,V = 2009.8(5) ?~3 and Mr = 945.47.Complex 1 shows a three-dimensional(3 D) framework.Moreover,through intermolecular hydrogen bonds,compound 1 is assembled into a supramolecular structure.The thermal stability and luminescent properties of 1 are also investigated.     

Synthesis,Structure and Luminescent Properties of Cd(Ⅱ) Coordination Polymers Based on 4-Nitrobenzoic Acid and Bis(imidazol) Ligand

A new Cd(Ⅱ) coordination polymer, [Cd_(0.5)(nba)(bib)_(0.5)]_(2n)(1, Hnba = 4-nitrobenzoic acid, bib = 1,4-bis(imidazol-1-yl)-butane), was synthesized at room temperature condition and characterized by IR spectra, elemental analyses, single-crystal and powder X-ray diffractions. Complex 1 belongs to the monoclinic system, C2/c space group, with a = 26.0600(14), b = 6.7889(4), c = 16.5825(9) ?, β = 118.8120(10)°, V = 2570.6(2) ?3, Z = 4. It shows one-dimensional chains and is further linked by π-π stacking interactions to yield a three-dimensional supramolecular structure. Thermal stability and luminescence of 1 were investigated.     

Crystal Structure and Spectroscopic Analysis of Polyphenyl Quinoxaline with Hg(Ⅱ)

The interaction of Hg~(2+) with polyphenyl quinoxaline ligand 2,3,6,7,10,11-hexaphenyldipyrazino[2,3-f:2?,3?-h]quinoxaline(HPQ) was investigated, and a new complex(C_(49)H_(32)N_6Br_2Cl_2Hg) has been synthesized and characterized. It exhibits a 0D single-core structure,and adopts triclinic P 1 space group with a = 11.139(2), b = 13.429(3), c = 14.488(3) ?, α =76.10(3), β = 83.16(3), γ = 87.36(3)o, V = 2088.4(7) ?3, Z = 2, S = 1.056, F(000) = 1104, R = 0.0417 and w R = 0.0931(I 2σ(I)). Furthermore, the behavior of HPQ with Hg~(2+) in the solution was also investigated, and the result shows that HPQ was found to have excellent fluorescent selectivity for Hg~(2+) over many other metal ions(Li~+, K~+, Na~+, Sr~+, Ca~(2+), Mg~(2+), Mn~(2+), Fe~(3+), Ni~(2+), Co~(2+), Cu~(2+), Zn~(2+),Cd~(2+), Pb~(2+), Al~(3+) and Cr~(3+)) based on the intermolecular charge-transfer mechanism, which makes HPQ a potential fluorescence sensor or probe for Hg~(2+).     

Synthesis and Crystal Structure of Bis(S-methyl-β-N- (4-dimethylaminophenyl)methlenedithiocarbazate) Nickel (Ⅱ)

11NTRoDUCT1ONRecently,transitionmetalorganometallicandcoordinationcomplexeshavee-mergedaspotentialbuildingblocksfornonlinearoptical(NLO)materials(l-5i.Com-paredwlthorganlcmolecu1es,metalcomplexesofferalargervarietyofstructures,comparabIeor,insomecases,higherenvironmenta1stabilityandamuchgreaterdi-versityoftunableelectronicpropertiesbythevirtueofthecoordinatedmetalcen-tert6i.Thethio-Schiffbaseligandderivedfromdithiocarbazatesandthiosemicar-bazidescancoordinatereadilywithtransitionmetalstog…     

Crystal Structure,Spectroscopic Characterization,and Electrochemical and Thermal Stability Properties of a Dinuclear Nickel(Ⅱ) Complex

A new nickel(Ⅱ) complex Ni_2(L)_2(2,2?-bipy)2·5.5H_2 O with methy-bicycle[2.2.1]hept-5-ene-2,3-dicarboxylic acid(H2L) and 2,2?-bipyridine(2,2?-bipy) as ligands has been synthesized in the mixed solvent DMF and water(v:v = 5:2). It crystallizes in the triclinic space group P1 with a = 10.414(2), b = 12.884(3), c = 16.176(4) ?, α = 70.715(5), β = 80.599(5), γ = 77.383(6)o, V = 1989.4(8) ?3, Dc = 1.531 g/cm3, Z = 2, F(000) = 958, GOOF = 1.028, the final R = 0.0808 and w R = 0.2036. The crystal structure shows that the whole molecule consists of two independent dinuclear units, in which two nickel ions are bridged by two μ2-η1:η0 3-carboxylate groups of L2- anions. The coordination environment of Ni(Ⅱ) ion is Ni N_2O_3, giving a distorted square pyramidal geometry. The thermal stability and electrochemical properties of the complex were investigated.     

Crystal Structure and Photoluminescence Properties of Two Barium(Ⅱ) MOFs

In this article, two Ba(Ⅱ) metal-organic frameworks(MOFs), {[Ba(BPS)(H₂O)₂]·H₂O}_n(1) and[Ba(BPS)(H₂O)₂]_n(2)(H₂BPS=4,4'-bibenzoic acid-2,2'-sulfone), were synthesized and characterized. X-Ray crystal structural analyses reveal that compounds 1 and 2 have different structures, which is probably related to different coordination modes of ligand in compounds 1 and 2. It is remarkable that compounds 1 and 2 both show excellent thermal stability. The solid-state emission spectra reveal that compounds 1 and 2 both present strong luminescence emission bands at room temperature.     

Crystal Structure and Fluorescent Study of a Terbium(Ⅲ) Coordination Polymer

A novel Tb(Ⅲ) coordination polymer [Tb(bpapO2)2(NO3)3]n [bpapO2 = N2,N6- bi(pyridin-2-yl)pyridine-2,6-diamine-N,N'-dioxide-dioxide] has been synthesized and it exhibits terbium's characteristic fluorescent emission under UV radiation of 326 nm at room temperature. X-ray structural determination indicates that each terbium(Ⅲ) ion, centered in TbO8 core, connects to three adjacent coordinate centers via a bi-dentate ligand bpapO2, forming a one-dimensional coordination polymer. The compound crystallizes in the triclinic system, space group P1, with a = 11.2271(5), b = 11.7997(5), c = 14.8016(6) Ⅲ, α = 72.7060(10), β = 89.9630(10), γ = 66.7680(10)o, Z = 2, Dc = 1.822 g/cm3, V = 1705.14(13) Ⅲ3, F(000) = 932, the final R = 0.0340 and wR = 0.0669 for 4812 observed reflections with I 2σ(I).     

Hydrothermal Synthesis,Crystal Structure and Magnetic Properties of a Cobalt(II) Coordination Polymer Assembled by 4-Sulfophthalate and 4,4'-Bipyridine

1 INTRUDUCTION The rational design and synthesis of metal-direc- ted supramolecular framework have received much attention in coordination chemistry because of their potential applications in catalysis, molecular selec- tion, non-linear optics, ion exchange and microelec- tronics[1～4]. During the lastdecade, many high-di- mensional coordination complexes have been de- signed and prepared through molecular self-as- sembly process[5～10]. The construction of open metal organic framework, s…     

Crystal Structure of Bis(3-hydroxy-2-pyridyl)disulfide

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＢｉｓ（３－ｈｙｄｒｏｘｙ－２－ｐｙｒｉｄｙｌ）ｄｉｓｕｌｆｉｄｅＣｈｅｎＸｕｅ－Ｔａｉ；ＫａｎｇＢｅｉ－Ｓｈｅｎｇ；ＸｕＹｏｎｇ－Ｊｉｎ；ＨｕＹｏｎｇ－Ｈａｎ（ＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆＳｔｒｕｃｔ...     

Synthesis, Crystal Structure and Optical Properties of a Cerium(Ⅳ) Complex with Chelidamic Acid

A new cerium complex,(C7H8)[Ce(C7H3NO5)2(H2O)3]·2H2O or (C7H8)[Ce(HChel)2-(H2O)3]·2H2O (1,H3Chel = 4-hydroxypyridine-2,6-dicarboxylic (chelidamic) acid),has been prepared by the hydrothermal reaction,and its crystal structure was determined based on single-crystal diffraction data. Compound 1 crystallizes in monoclinic,space group P21/c with a = 12.4267(9),b = 10.8195(7),c = 19.5650(13),β = 92.898(3)o,V = 2627.2(3) 3,Dc = 1.733 g/cm3,Z = 4,Mr = 685.55,μ = 1.809 mm-1,λ(MoKα) = 0.71073  and F(000) = 1372. The final R = 0.0455 and wR = 0.1984 for 5983 observed reflections with Ⅰ > 2σ(Ⅰ),and R = 0.0490 and wR = 0.2053 for all data. Complex 1 contains one cerium ion,two chelidamic acid ligands,three coordinated water molecules,one discrete toluene molecule,and two discrete water molecules. The Ce(IV) ion is nine-coordinate with the coordination polyhedron made up of four oxygen atoms and two nitrogen atoms from two tridentate chelating chelidamic acid ligands,and three coordinated water molecules. A three-dimensional network is formed by the H-bonds. Moreover,optical properties are investigated and the results show that this complex has sharp optical absorption at 221,396 and 571 nm but no marked fluorescent emission.     

Synthesis, Characterization and Properties of Organotin Complexes Dibutyltin（Ⅳ） Bis（heteroaromatic carboxylate） and Crystal Structure of Dibutyltin（Ⅳ） Bis（2-thiazolylcarboxylate）

The six organotin complexes dibutyltin(IV) bis(heteroaromatic carboxylate) were synthesized by the reaction of (n‐Bu)2SnO with heteroaromatic carboxylic acid in 1:2 molar ratio. These complexes have been characterized by elemental analysis, IR, ¹H, ¹³C and ¹¹⁹Sn NMR. The crystal structure of dibutyltin(IV) bis(2‐thiazolylcarboxylate) was determined by X‐ray single crystal diffraction. This compound is a weakly bridged dimer through weak interaction Sn···O between molecules. The tin atoms took six‐coordinate skew‐trapezoidal bipyramidal geometry. The crystal of complex 3 belongs to monoclinic symmetry with space group P2₁/c, a=1.863(2) nm, b=2.220(3) nm, c=1.0395(10) nm, β=90.275(16)°, Z=8, V=4.292(8) nm³, D_c=1.514 Mg/m³, μ=1.406 mm^‐1, F(000)=1968, S=0.999, R=0.0549, wR=0.1011.     

Synthesis, Spectroscopic Properties and Crystal Structural Characterization of a Triphenyltin(Ⅳ) Complex with 5-Bromonicotinic Acid

A novel organotin complex [Ph3Sn(C2H5OH)(OCOC5H3NBr)SnPh3(OCOC5H3NBr)]has been synthesized by the reaction of 5-bromonicotinic acid with triphenyltin hydroxide in ethanol and characterized by elemental analysis, IR and 1H NMR. The crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 15.564(2), b = 24.975(4), c = 12.2973(19) (A), β = 92.224(2)°, Z = 4, V = 4776.5(13) (A)3, Dc = 1.596g/cm3, μ(MoKα) = 2.765 mm-1, F(000) = 2264, R = 0.0385 and wR = 0.0667. In the molecular structure of the title complex, the tin atoms are five-coordinated in a trigonal bipyramidal geometry.