Synthesis,Crystal Structure and Gas Adsorption of a Two-fold Interpenetrated Three-dimensional Framework {[Cd(2-NO_2-BDC)(4,4?-DPA)]·(DMF)}_n

The reaction of Cd(NO_3)_2·4H_2O with 4,4?-dipyridylacetylene(4,4?-DPA) and 2-nitroterephthalic acid(2-NO_2-H_2BDC) in DMF/H_2O mixed solvent has afforded a compound {[Cd(2-NO_2-BDC)(4,4?-DPA)]·(DMF)}_n(1). Compound 1 has been characterized by single-crystal X-ray diffraction, powder X-ray diffraction, thermogravimetry analysis, and IR spectrum. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 12.1488(3), b = 14.6689(3), c = 13.1615(3) ?, β = 111.809(3)o, V = 2177.63(9) ?~3, Z = 4, C_(23)H_(18)N_4O_7 Cd, M_r = 574.81, D_c = 1.753 g/cm~3, μ = 8.523 mm~(-1), F(000) = 1152, the final R = 0.0411 and wR = 0.1064 for 3589 observed reflections with I 2s(I). In compound 1, the Cd(Ⅱ) ions are linked by the carboxylate groups of 2-NO_2-BDC ligands to give a two-dimensional layered structure based on the centrosymmetric dinuclear Cd_2(COO)_2 units, which are further connected by the 4,4?-DPA ligands to produce a three-dimensional framework with pcu topology. Careful examination revealed that compound 1 is a 2-fold interpenetrating framework. Furthermore, the gas adsorption properties of 1 for N_2 and CO_2 have also been investigated.     

A 1D Double Stranded Chain Complex Based on Barium Ion and 1,3,5-Triazine

A new coordination compound [Ba(OBPT)2(H2O)2]·H2O was obtained at room temperature by the reaction of 4,6-bis(2-pyridyl)-1,3,5-triazin-2-ol(HOBPT) with BaCl2.It was characterized by elemental analysis,FTIR,TG analysis,powder X-ray diffraction analysis and single-crystal X-ray diffraction analysis.The complex crystallizes in the monoclinic P21/n space group,with a = 16.325(1),b = 6.7977(5),c = 24.164(2) ,β = 104.009(1),V = 2601.8(3) 3,Z =4,C26H22BaN10O5,Mr = 691.88,Dc = 1.766 g/cm3,F(000) = 1376 and μ(MoKα) = 1.587 mm-1.The final R = 0.0282 and wR = 0.0724 for 5095 observed reflections with I > 2σ(I) and R = 0.0312 and wR = 0.0744 for all data.In the complex,the barium ion is ten-coordinated with six nitrogen atoms from two ligands,two deprotonated hydroxyl oxygen atoms from another two ligands and two coordinated water molecules to form a double stranded chain.The extensive supramolecular interac-tions lead to the formation of an infinite 2D framework.     

Syntheses, Crystal Structures and Characterization of Layered and Layer-pillared Zinc Arsonates

Two zinc arsonate coordination polymers, Zn(4-apa)·H2O (1, 4-apaH2 = 4-amino- phenylarsonatic acid) and Zn(4-apa) (2), have been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal and powder X-ray diffraction. Crystal data for 1: monoclinic, space group C2/c with a = 23.056(5), b = 5.4224(11), c = 15.027(3) , β = 121.22(3)°, V = 1606.6(6) ?3, Dc = 2.468 g·cm-3, F(000) = 1168, μ = 7.122 mm-1, Z = 8, the final R = 0.0309 and wR = 0.0752 for 1763 observed reflections with I > 2σ(I). For 2: monoclinic, space group P21/c with a = 8.7852(18), b = 9.2744(19), c = 9.752(2) , β = 103.45(3)°, V = 772.7(3)3, Dc = 2.410 g·cm-3, F(000) = 544, μ = 7.387 mm-1, Z = 4, the final R = 0.0321 and wR = 0.0741 for 1696 observed reflections with I > 2σ(I). The structure of 1 shows a two-dimensional (4,4)-network composed of an inorganic ladder chain bridged by the phenyl-linkers of 4-apa ligands. Compound 2 exhibits a 3D layer-pillared framework with crb net, in which inorganic (4-82)-networks are joined by the phenyl-linkers.     

Syntheses, Crystal Structures and Magnetic Properties of a New Nitronyl Nitroxide Radical and Its Cu(Ⅱ) Complex

A new compound (NIT-mNO2 = 4,4,5,5-tetramethylimidazoline-2-yl-(2'-chlor-5'- nitrophenyl)-3-oxide-1-oxyl) 1 and its complex (Cu(NIT-mNO2)(hfac)2) 2 have been synthesized and structurally and magnetically characterized. Complex 1 crystallizes in monoclinic, space group P21/n with a = 10.6798(9), b = 11.2705(9), c = 12.9559(10) , β = 107.3770(10)o, V = 1488.3(2) 3, C13H15ClN3O4, Mr = 312.73, Z = 4, Dc = 1.396 g/cm3, μ(MoKa) = 0.276 mm-1, F(000) = 652, the final R = 0.0606 and wR = 0.1773 for 3405 independent reflections with Rint = 0.0203. The nitronyl nitroxide unit (imidazoline ring) is not coplanar with the phenyl ring with the dihedral angle between them of 55.75o. The compound results in a 1-D zig-zag chain structure by intermolecular H-bond interaction. Compound 2 crystallizes in triclinic, space group P1 with a = 10.3699(10), b = 10.6286(11), c = 15.1683(15), α = 77.5330(10), β = 773080(10), γ = 87.3420(10)o, V = 1592.5(3) 3, C23H17ClF12N3O8Cu, Mr = 790.39, Z = 2, Dc = 1.648 g/cm3, μ(MoKa) = 0.888 mm-1, F(000) = 788, the final R = 0.0793 and wR = 0.2153 for 5794 independent reflections with Rint = 0.0196. The Cu(II) ion is located at a center of symmetry, and each Cu(II) is surrounded by six oxygen atoms at the vertices of a distorted tetragonal octahedron. Four of the six oxygen atoms belong to two hfac ligands and occupy the equatorial coordination sites, while the other two of NIT-mNO2 act as μ-1,5 bridge between the Cu(II) ion, thus forming a 1-D chain structure. The magnetic susceptibility data indicate intermolecular antiferromagnetic interactions between compound 1 and intrachain ferromagnetic behaviors.     

Synthesis,Crystal Structure and DNA Interaction Study of 3-(2-(3,5-Diphenyl-4,5-dihydropyrazol1-yl)thiazol-4-yl)-2H-chromen-2-one

A new compound 3-(2-(3,5-diphenyl-4,5-dihydropyrazol-1-yl)thiazol-4-yl)-2Hchromen-2-one was synthesized by cyclocondensation of 3,5-diphenyl-4,5-dihydropyrazole-1-carbothioamide with 3-(2-bromoacetyl)-2H-chromen-2-one in ethanol at reflux for 2hrs. The compound was characterized by IR, 1H-NMR, 13C-NMR and single-crystal X-ray diffraction analysis. The newly synthesized compound(C27H19N3O2S) crystallizes in the triclinic system, space group P1 with a = 5.2476(6), b = 18.289(2), c = 23.115(3) , α = 93.546(7), β = 94.715(6), γ = 92.347(7)°, V = 2204.3(4)3, Z = 4, Mr = 449.51, crystal size = 0.38 mm × 0.22 mm × 0.16 mm,(I 2σ(I)) = 35317, 9736, 3785, Rint = 0.081,(Δρ)max = 0.19 and(Δρ)min = –0.24 e·-3. DNA interaction studies revealed that the target compound strongly interacts with DNA through an intercalation binding mode and the binding constant of the compound is 7.45 × 104 M-1.     

Synthesis,Crystal and Electronic Structure of Ba_3ZnSb_2O_9 with the 6H-perovskite-type Structure

Crystals of Ba3ZnSb2O9 have been grown by a high-temperature solid-state reaction and characterized by single-crystal X-ray diffraction.Ba3ZnSb2O9 crystallizes in the hexagonal P63/mmc space group with a = 5.8663(4),c = 14.478(2) ,V = 431.49(8) 3,Z = 2 and R(all data) = 0.0167.The structure of Ba3ZnSb2O9 consists of pairs of face-sharing Sb2O9 bi-octahedra connected via corners with two single layers of mutually isolated ZnO6 octahedra.Each Ba2+ ion is bonded to 12 oxygen atoms.The UV-vis absorption spectrum of the compound has been investigated.Additionally,the calculations of band structure and density of states have also been performed with density functional theory method.The obtained results tend to support the experimental data of the absorption spectrum.     

Syntheses, Crystal Structures and Magnetic Properties of a New Nitronyl Nitroxide Radical and Its Cu(Ⅱ) Complex

A new compound (NIT-mNO2 = 4,4,5,5-tetramethylimidazoline-2-yl-(2'-chlor-5'- nitrophenyl)-3-oxide-1-oxyl) 1 and its complex (Cu(NIT-mNO2)(hfac)2) 2 have been synthesized and structurally and magnetically characterized. Complex 1 crystallizes in monoclinic, space group P21/n with a = 10.6798(9), b = 11.2705(9), c = 12.9559(10) , β = 107.3770(10)o, V = 1488.3(2) 3, C13H15ClN3O4, Mr = 312.73, Z = 4, Dc = 1.396 g/cm3, μ(MoKa) = 0.276 mm-1, F(000) = 652, the final R = 0.0606 and wR = 0.1773 for 3405 independent reflections with Rint = 0.0203. The nitronyl nitroxide unit (imidazoline ring) is not coplanar with the phenyl ring with the dihedral angle between them of 55.75o. The compound results in a 1-D zig-zag chain structure by intermolecular H-bond interaction. Compound 2 crystallizes in triclinic, space group P1 with a = 10.3699(10), b = 10.6286(11), c = 15.1683(15), α = 77.5330(10), β = 773080(10), γ = 87.3420(10)o, V = 1592.5(3) 3, C23H17ClF12N3O8Cu, Mr = 790.39, Z = 2, Dc = 1.648 g/cm3, μ(MoKa) = 0.888 mm-1, F(000) = 788, the final R = 0.0793 and wR = 0.2153 for 5794 independent reflections with Rint = 0.0196. The Cu(II) ion is located at a center of symmetry, and each Cu(II) is surrounded by six oxygen atoms at the vertices of a distorted tetragonal octahedron. Four of the six oxygen atoms belong to two hfac ligands and occupy the equatorial coordination sites, while the other two of NIT-mNO2 act as μ-1,5 bridge between the Cu(II) ion, thus forming a 1-D chain structure. The magnetic susceptibility data indicate intermolecular antiferromagnetic interactions between compound 1 and intrachain ferromagnetic behaviors.     

Synthesis,Structure and Luminescent Properties of a Two-dimensional Cobalt(Ⅱ) Coordination Polymer Based on 2-Thiobarbituric Acid

A two-dimensional coordination polymer [Co(H_2tba)_2(DMF)_2]_n 1(H_2tba = 2-thiobarbituric acid anion, DMF = N,N-dimethylformamide) has been synthesized by Co Cl2·6H2O with the 2-thiobarbituric acid ligands under solvothermal conditions. Compound 1 was further characterized by FTIR, elemental analysis, TGA and powder XRD techniques. Single-crystal X-ray diffraction studies revealed that the title compound crystallizes in the monoclinic space group Pbca with a = 12.5948(12), b = 11.4269(11), c = 14.8939(15) ?, V = 2143.5(4) ?~3, Z = 4, Dc = 1.523 g·cm-3, F(000) = 1012, μ = 1.038 mm~(-1), R = 0.0358 and w R2 = 0.0888(I 2σ(I)). Single-crystal X-ray diffraction analysis reveals that 1 is the first two-dimensional noninterpenetrating(4, 4) net coordination polymer based on the 2-thiobarbituric acid. Coordination polymer 1 exhibits two luminescent emission spectra at 477 and 489 nm with the excitation peak at 273 nm.     

Hydrothermal Synthesis, Crystal Structure and Photoluminescence of [Sm（PCA）_3（H_2O）_2]_n·6nH_2O

A new one-dimensional (1-D) compound [Sm(PCA)3(H2O)2]n·6nH2O (1, HPCA=pyrazinecarboxylic acid) has been synthesized via hydrothermal reaction and structurally characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the Pbca space group of orthorhombic system with a=19.465(3), b=12.034(4), c=19.842(4) , V=4648(2)3, C15H25N6O14Sm, Mr=663.76, Dc=1.897 g/cm3, S=1.023, μ(MoKα)=2.610 mm-1, F(000)=2648, R=0.0239 and wR=0.0616. Compound 1 is characteristic of an infinite 1-D chain-like structure with the samarium atoms locating at an environment of a monocapped square antiprism. The [Sm(PCA)3(H2O)2]n chains and the lattice water molecules interconnect together through π-π interactions and hydrogen bonding interactions to yield a 3-D supramolecular framework. Photoluminescent investigation reveals that the title compound displays an emission in the greenish blue region.     

Synthesis,Crystal Structure and DNA Binding Studies of α,α'-Bis(3,5-bismethyl-1-pyrozolyl)-carbene-acetyl-isopropenyl Hydrazine

The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro- penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) , α = 75.311(4), β = 82.695(4), γ = 77.143(4)o, Z = 2, V = 847.9(3) 3, Dc = 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 ). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders. Keywords: α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopropenyl, preparation, crystal structure, DNA binding     

Synthesis, Structure and Comparison of Luminescent Property between Two Hexanuclear Silver（I） Thiosemicarbazone Clusters

A new silver(Ⅰ) compound 4 containing thiosemicarbazone with group 2-quinoline was synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analysis and fluorescence spectrum. Compound 4 crystallizes in triclinic, space group P1 with a = 12.2710(9), b = 16.9281(13), c = 17.2984(13), α = 112.8500(10), β = 103.4890(10), γ = 102.6860(10)°, V = 3020.9(4) 3, C80H94Ag6N28O6S6, Mr = 2383.41, Dc = 1.310 g/cm3, μ(MoKα) = 1.108 mm-1, F(000) = 1196, Z = 1, the final R = 0.0567 and wR = 0.1368 for 5112 observed reflections (I > 2σ(I)). Similar to the structure of compound 2 we have reported, compound 4 also exhibits a hexanuclear silver(Ⅰ) cluster. In the cluster, the S atom of ligand L4 (L4 = 2-quinolinecarboxaldehyde thiosemicarbazone) serves as a triply bridged chelator to connect the six silver atoms into a Ag6L46 cluster. The luminescence property of 4 is investigated at room temperature and compared with that of 2.     

Synthesis,Structure and Comparison of Luminescent Property between Two Hexanuclear Silver(Ⅰ) Thiosemicarbazone Clusters

A new silver(Ⅰ) compound 4 containing thiosemicarbazone with group 2-quinoline was synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analysis and fluorescence spectrum. Compound 4 crystallizes in triclinic, space group P1 with a = 12.2710(9), b = 16.9281(13), c = 17.2984(13), α = 112.8500(10), β = 103.4890(10), γ = 102.6860(10)°, V = 3020.9(4) 3, C80H94Ag6N28O6S6, Mr = 2383.41, Dc = 1.310 g/cm3, μ(MoKα) = 1.108 mm-1, F(000) = 1196, Z = 1, the final R = 0.0567 and wR = 0.1368 for 5112 observed reflections (I 2σ(I)). Similar to the structure of compound 2 we have reported, compound 4 also exhibits a hexanuclear silver(Ⅰ) cluster. In the cluster, the S atom of ligand L4 (L4 = 2-quinolinecarboxaldehyde thiosemicarbazone) serves as a triply bridged chelator to connect the six silver atoms into a Ag6L46 cluster. The luminescence property of 4 is investigated at room temperature and compared with that of 2.     

Hydrothermal Synthesis and Crystal Structure of a Manganese Complex

The title compound [Mn(Phen)(p-MBA)2]n(1) was synthesized via the hydro-thermal reaction of KMnO4 and NaOH with phen and p-methybenzoic acid(p-MBA) in water.The title compound was characterized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in orthorhombic,space group Pbcn with a = 24.132(1),b = 10.404(0),c = 9.386(0) ,V = 2356.65(13) 3,Z = 4,C28H22MnN2O4,Mr = 505.42,Dc = 1.424 g/cm3,F(000) = 1044 and μ(MoKα) = 0.598 mm-1.The final R = 0.0781 and wR = 0.1363 for 1972 observed reflections with Ⅰ 2σ(Ⅰ) and R = 0.0897 and wR = 0.1420 for all data.X-ray diffraction reveals that the Phen and p-methy benzoic acid ligand link the Mn atoms into a single one-dimensional coordination polymer,and extensive intermolecular π-π interactions lead these 1D chains to form a two-dimensional supramolecular architecture.     

Three New Zn(Ⅱ)/Cd(Ⅱ) Coordination Polymers Constructed with 2-Mercaptonicotinic Acid and 1,2-Di(4-pyridyl)ethylene: Syntheses and Structure Analysis

Three new Zn(Ⅱ)/Cd(Ⅱ) coordination polymers based on 2-mercaptonicotinic acid (H2mna) with 1,2-di(4-pyridyl)ethylene (dpe) introduced as a bridging ligand have been synthesized via hydrothermal method and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis and IR. As reported in this paper, [Zn2(dpe)0.5(mna)2] (1) can be classified as a two-dimensional layer structure in which the 1D chain composed of Zn(Ⅱ) and mna ligands is bridged by dpe ligands, while the complex named [Zn4(dpe)4(mna)4] (2) is a tetra-nuclear cluster compound. These two compounds are further extended to three-dimensional structures by hydrogen bonds along with C-H…π and π…π interactions. Compound 3 with general formular [Cd2(dpe)0.5(mna)2]·H2O belongs to a three-dimensional porous structure in which the 2D metal layers formed by the coordination of Cd(Ⅱ) and mna ligands are connected with the bridging of dpe ligands.     

An Unusual Organometallic Supramolecule Composed of Chiral Dirhodium Units and Sulfato Bridging Ligands

A chiral supramolecular compound (H3O){[cis-Rh2((C6H5)2P(C6H4))2(SO4)- (DMF)]2(μ- OC2H5)}·6C2H5OH (1) has been synthesized and characterized by X-ray single-crystal analysis. Compound 1 crystallizes in monoclinic, space group C2/c with a = 26.752(3), b = 13.5868(16), c = 26.611(3) , β = 103.891(2)°, V = 9389.5(19) 3, Z = 4, C92H114N2O18P4Rh4, Mr = 2135.49, Dc = 1.511 g/cm3, F(000) = 4384 and μ(MoKα) = 0.870 mm-1. The final R = 0.0441 and wR = 0.1186 for 8283 observed reflections with I > 2σ(I) and R = 0.0567 and wR = 0.1290 for all data. The structure of the compound is unique. It contains two inherent chiral {cis-Rh2[(C6H5)2P(C6H4)]2}2+ units which are connected not only in the equatorial positions by two sulfato ligands, but also in two of their axial positions by a μ2 ethoxide anion. The remaining axial positions of Rh24+ units in 1 are occupied by the DMF molecules. The sulfato ligands act as μ4 tridentate bridges to connect the Rh24+ units. The Rh-Rh metal-metal bond distances are comparable to those in analogous dirhodium compounds.     

Synthesis,Crystal and Band Structures,and Optical Properties of Mercury Pnictide Halide Hg19As10Br18

A mercury pnictide halide semiconductor Hg19As10Br18(1) has been prepared by the solid-state reaction and structurally characterized by single-crystal X-ray diffraction analysis.Compound 1 crystallizes in triclinic,space group P with a = 11.262(4),b = 11.352(4),c = 12.309(5) ,α = 105.724(2),β = 105.788(4),γ = 109.0780(10)° and V = 1314.3(8) 3.The structure of 1 is composed of parallel perovskite-like layers bridged by the linearly coordinated Br atoms to form a three-dimensional framework.The optical properties were investigated in terms of the diffuse reflectance spectrum.The electronic band structure along with density of states(DOS) calculated by DFT method indicates that compound 1 is a semiconductor with an indirect band gap,and that the optical absorption is mainly originated from the charge transitions from Br-4p and As-4p to the Hg-6s states.     

Solvothermal Synthesis,Crystal Structure and Luminescent Property of a Two-dimensional Lead(Ⅱ) Compound:[Pb(bmzbc)_2]_n

A two-dimensional coordination polymer, [Pb(bmzbc)_2]_n(1)(Hbmzbc =4-benzimidazole-1-yl-benzoic acid), has been synthesized by the solvothermal reaction of Pb(NO_3)_2 with Hbmzbc at 120 ℃ in ethanol solvent. Compound 1 has been characterized by single-crystal X-ray diffraction, powder X-ray diffraction, thermogravimetry analysis, and IR spectrum. Compound 1 crystallizes in the orthorhombic system, space group Pccn, with a = 12.5801(7), b = 20.0795(11), c = 9.1830(6) ?, V = 2319.6(2) ?~3, Z = 4, C_(28)H_(18)N_4O_4Pb, M_r = 681.65, D_c = 1.952 g/cm~3, μ = 7.319 mm~(-1), F(000) = 1312, the final R = 0.0336 and wR = 0.0965 for 1699 observed reflection with I 2σ(I). In 1, the bmzbc~– ligands bridge the Pb(Ⅱ) ions to generate a 2-D sheet with(4, 4) topology. The complex exhibits turquoise photoluminescent emission with a maximum at 480 nm upon excitation at 300 nm.     

Syntheses and Crystal Structures of 3-Carboxylsalicylidenefurfurylimine And Its Trinuclear Nickle(Ⅱ) Complex

A Schiff base ligand(H2CSF,C13H11NO4,1) derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3(CSF)2(CH3COO)2(DMF)2(H2O)2](2) were synthesized.Compound 1 was characterized by elemental analysis,1H NMR,IR,MS and X-ray diffraction analysis.The crystal of 1 belongs to the monoclinic system,space group P21/c with a = 8.472(2),b = 19.743(5),c = 7.2300(18) ,β = 110.278(4)°,V = 1134.4(5) 3,Z = 4,Mr = 245.23,Dc = 1.436 g·cm-3,μ = 0.108 mm-1,F(000) = 512,λ = 0.71073 ,the final R = 0.0440 and wR = 0.1199 for 1426 observed reflections(I 2σ(I)).In the crystal of 1,there exist intramolecular hydrogen bonds and weak intermolecular C-H···O hydrogen bonds.Compound 2 was characterized by elemental analysis,IR,TG and X-ray diffraction analysis.The crystal of 2 is of triclinic system,space group P1 with a = 10.1237(17),b = 10.4086(18),c = 10.4884(18) ,α = 82.528(2),β = 67.339(2),γ = 83.010(2)°,V = 1008.1(3) 3,Z = 1,Mr = 962.87,Dc = 1.586 g·cm-3,μ = 1.463 mm-1,F(000) = 498,λ = 0.71073 ,the final R = 0.0517 and wR = 0.0805 for 2065 observed reflections(I 2σ(I)).The geometry of the trinuclear molecule is centrosymmetric,in which every Ni(Ⅱ) ion is coordinated in a slightly distorted octahedron.The three Ni(Ⅱ) ions are arranged in a straight line.The two CSF2-ions act as NOO tridentate ligands with the phenolate and carboxylate oxygen as bridging atoms.The coordination atoms of CSF2-anions and water molecules are coordinated on the equatorial plane,while the two bridging acetate ions and two DMF are trans-coordinated on the apical sites.     

Synthesis and Crystal Structure of 9-（4-Dimethylaminophenyl）-l,8-dioxo- 9H-dibenzo [c,h ]-2,7,10-trioxanthene

The title compound 9-(4-dimethylaminophenyl)-1,8-dioxo-9H-dibenzo[c,h]- 2,7,10-trioxanthene (3) was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethyla- minobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in triclinic, space group P with a = 7.8753(16), b = 11.029(2), c = 12.913(3) , α = 69.79(3), β = 89.01(3), γ = 81.90(3)°, V = 1041.5(4) 3, Z = 2 , F(000) = 456, Dc = 1.395 Mg/m3, Mr = 437.43, μ = 0.097 mm-1, λ = 0.71073 , the final R = 0.0491 and wR = 0.1314 for 2662 observed reflections with I > 2σ(I).     

Layer Zirconogermanate——(H_2DETA)[ZrGe_3O_8F_2] Showing Odd 3MR and 7MR

A layered zirconogermanate,(H2DETA)[ZrGe3O8F2](1),was hydro(solvo)thermally synthesized with diethylenetriamine(DETA) as template,and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallized in the monoclinic space group P21/c with data of unit cell:a=0.7644(2) nm,b=1.1235(2) nm,c=1.6860(3) nm,V=1.4479(5) nm3,μ(Mo Kα)=6.931 mm-1,Z=4,R1=0.0402 for 3236 reflections with Fo>2σ(Fo). The structure of compound 1 was formed by alternatively packing the inorganic layer of ZrGe3O8F2 and H...