Synthesis, Spectroscopic Properties and Crystal Structure of (C_4N_2H_(12))_2Zr(C_2O_4)_4·H_2O

1 INTRODUCTION The researches on transition metal coordination complexes have been rapidly expanded because of their fascinating structural diversity and potential applications[1～4]. As we know, zirconium oxalates can be used as precursors in the synth…     

Synthesis and Crystal Structure of (C6N3H18)2Ti4O4(C2O4)7·4H2O

The title compound (C6N3H18)2Ti4O4(C2O4)7(4H2O 1 (C13H22N3O18Ti2, Mr = 604.14) was synthesized by the reaction of Ti(SO4)2, H2C2O4(2H2O and N-(2-ammonioethyl)- piperazinium (AEPP) in aqueous solution. The single-crystal X-ray analysis has revealed that 1 crystallizes in the triclinic system, space group Pī with a = 9.1437(6), b = 11.4991(10), c = 11.6975(8)A, α = 96.2915(18), β = 107.998(3), γ = 104.276(4)°, V = 1110.35(14)A3, Z = 2, Dc = 1.807 g/cm3, F(000) = 618, μ = 0.815 mm－1, the final R = 0.0463 and wR = 0.1264 for 3718 observed reflections with I > 2σ(I). X-ray crystal-structure analysis suggests that compound 1 consists of [Ti4O4(C2O4)7]6－ anion and two protonated N-(2-ammonioethyl)piperazinium cations. The anions are linked into an infinite chain through Ti4O4(C2O4)8 by sharing the oxalates as bridging ligands.     

Synthesis, Crystal Structure and Properties of Complex VO（C12H12N2O2） （C13H10NO2）

IntroductionAsthevanadate dependentenzyme ,ahaloperox idase,andvanadiumnitrogenasehavebeenfoundinsuccession ,somescientistsareinterestedinthecoor dinationchemistryandthebiochemistryofvanadi um[1] .Thereactivecenterofvanadiumbromoperoxi dasecontainstheoxovanadiumVO3+ coordinatedbyoxygenandnitrogenatoms[2 ] .However,thestudiesaboutoxovanadiumVO3+ coordinationcompoundscontainingbioactiveligandsarerarelyfound[3— 8] .Hydroximicacidthatcanbeconsideredtobethederivativeofthecarboxylicacid ,theamide…     

Crystal Structure and Properties of Rb4H2I2O10 · 4H2O

Single crystals of the Rb₄H₂I₂O₁₀· 4H₂O were synthesized for the first time and studied by X-ray diffraction analysis. The crystals are monoclinic, a = 7.321(6) Å, b = 12.599(8) Å, c = 8.198(8) Å, = 96.30(7)°, Z = 2, space group P2₁/c. The H₂I₂O₁₀ ^4– anion is formed by the edge-sharing IO₆ octahedra. The anions are united by hydrogen bonds into a chain running along the x axis. The chains are combined by water molecules into a three-dimensional structure through hydrogen bonds. The compound is a proton conductor. The conductivity values measured at 20–60°C vary within 10^–6 to 10^–4 ohm^–1 cm^–1.     

Synthesis and Crystal Structure of [Ni(H2O)6][Ni(H2O)2(C4H2O4)]·4H2O

Reaction of a freshly prepared Ni(OH)_{2?2 x} (CO₃) _x ·yH₂O with maleic acid in H₂O at room temperature afforded [Ni(H₂O)₆][Ni(H₂O)₂(C₄H₂O₄)]·4H₂O, which consists of [Ni(H₂O)₆]²⁺ cations, [Ni(H₂O)₂(C₄H₂O₄)]^2? anions and lattice H₂O molecules. Ni atoms in cations are octahedrally coordinated and Ni atoms in anions are each octahedrally coordinated by bidentate chelating maleato ligands and two water molecules at trans positions. Cations and anions are interlinked by hydrogen bonds to form 1D chains, which are hexagonally arranged and connected by the lattice water molecules. When heated in a flowing argon stream, the compound decomposes, with complete dehydration being followed by dissociation of nickel maleate into NiO and maleic anhydride.     

Synthesis,Crystal Structure,and Properties of [Dy(p-ABA)3Phen · H2O] · 1.5H2O1

(1.10-Phenanthroline)-tris(4-amidobenzoate)dysprosium, [Dy(p-ABA)₃Phen · H₂O] · 1.5H₂O (where p-ABA = p-amidobenzoate and Phen = 1.10-phenanthroline) has been synthesized. The complex was characterized by elemental analysis, UV, IR spectroscopy, and molar conductance. The crystal structure was determined by X-ray crystallography. The coordination number of the mononuclear complex is nine. The crystals are triclinic, space group P1 with a = 10.4484(13) Å, b = 12.2015(15) Å, c = 14.0170(17) Å; α = 92.800(2)°, β = 102.7220(10)°, γ = 108.880(2)°. Z = 2, d _c = 1.617 mg m^?3, F(000) = 786. R1 = 0.0327, and wR2 = 0.0911.     

Synthesis and Crystal Structure of [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O

The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nanthroline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10)(A), α = 80.6830(10), β = 66.6480(10), γ = 64.0480(10)o, V = 1554.63(4) (A)3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm3, μ = 0.845 mm-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (I > 2σ(I)). The compound contains a six-coordinated copper(II) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)～2.225(2)(A)), one sulfate O atom (Cu-O = 2.0037(17) (A)) and one water O atom (Cu-O(5w) = 2.719(2) (A)) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.     

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.     

Synthesis, Crystal Structure and Luminescent Property of [Zn(C12H9O3)2(C10H8N2)]n·nH2O

Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4'-bipyridine (4,4'-bipy)has afforded a new Zn(Ⅱ) compound,[Zn(C12H9O3)2(C10H8N2)]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335(2), b = 19.3834(4), c = 20.1707(4) (A), β =104.9830(10)°, V = 2920.82(11) A3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm3, μ = 0.895 mm-1, F(000) = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections (Ⅰ>2σ(Ⅰ)). Complex 1 consists of one-dimensional zigzag chains deriving from Zn(C12H9O3)2 units linked by 4,4'-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis (TGA) and luminescent property for 1 have also been studied in this paper.     

Hydrothermal Synthesis, Crystal Structure and Thermal Stability of [Ni(phen)3]·(C8H12O4)·(H2O)14

One novel complex [Ni(phen)3]·(C8H12O4)·(H2O)14 with hexane dicarboxylic acid and 1,10-phenanthroline has been hydrothermally synthesized and characterized. Crystal data: monoclinic, space group C2/c, a = 2.3475(5), b = 1.2208(2), c = 1.9499(4) nm, β = 114.682(3)o, V = 5.0778(16) nm3, Dc = 1.339 g/cm3, Z = 4, μ(MoKα) = 0.458 mm-1, F(000) = 2168, GOOF = 1.014, R = 0.0401 and wR = 0.0961. The nickel(Ⅱ) center in the title complex is coordinated with six nitrogen atoms of three 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. However, the nickel(Ⅱ) ion does not coordinate to the hexane dicarboxylic acid. The complex molecules form a 3D structure through hydrogen bonds. TG analysis shows that the title complex is stable below 240.0 ℃.     

Synthesis, Crystal Structure and Luminescence Property of [Co(hmz)2(H2O)4]·2H2O

A new mononuclear Co(Ⅱ) complex, [Co(hmz)2(H2O)4]·2H2O, has been synthesized by the reaction of Co(CH3COO)2·4H2O with 1-(4-hydroxyphenyl)-5-mercaptotetrazole (Hhmz). It crystallizes in the monoclinic system, space group P21/n with a = 13.502(5), b = 6.718(3), c = 13.972(6) (A), β = 117.532(4)°, V = 1123.9(8) (A)3, Z = 2, M r = 553.45, F(000) = 570, Dc = 1.635 g/cm3, μ = 1.008 mm-1, the final R = 0.0272 and wR = 0.0684 for 2194 observed reflections (Ⅰ＞ 2σ(Ⅰ)). The Co(Ⅱ) is six-coordinated by two nitrogen atoms from two hmz-1 ligands and four water molecules, forming an octahedral geometry. The intermolecular hydrogen bonding and offset-panel π-π stacking interactions between the adjacent molecules extend the compound into a three- dimensional supramolecular framework. The title compound emits strong blue fluorescent light (λem(max) = 427 nm) at room temperature and is red-shifted compared with free ligand Hhmz (λem(max) = 342 nm).     

Synthesis, Crystal Structure and Properties of [Co(1,3- bdoaH)2·4H2O] ·4H2O with Benzene-1,3-dioxyacetate Ligand

The cobalt(II) complex C20H34O20Co has been synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P with a = 5.1374(10), b = 10.519(2), c = 12.913(3) (A), α = 86.89(3), β = 79.94(3), γ = 86.74(3)o, V = 685.3(3) (A)3, Z = 1, Mr = 653.40, Dc = 1.583 g/cm3, μ = 0.717 mm-1, F(000) = 341, the final R = 0.0657 and wR = 0.1141 for 1900 observed reflections with I > 2σ(I). The cobalt ion is six-coordinated by two O atoms of different 1,3-bdoaH- ligands and four water molecules, residing in an octahedral environment. The intermolecular hydrogen bonds form a 3-D supramolecular network structure.     

Synthesis, Properties and Crystal Structure of a New Bismuth Oxalate:Na(C5NH6)[Bi(H2O)(C2O4)2]2·4H2O

A new bismuth oxalate Na(C5NH6)[Bi(H2O)(C2O4)2]2.4H2O has been obtained under hydrothermal conditions and characterized by X-ray diffraction.It crystallizes in mono-clinic, space group C2/m with a = 12.020(5), b = 11.190(8), c = 11.067(10)(A), β= 121.78(2)°,NaBi2CI3NH18O22, Mr= 981.24, V = 1265.4(16)(A)3, Z = 2, Dc = 2.575 g/cm3, μ(MoKα) = 14.005 mm-1, F(000) = 912, R = 0.0179 and wR = 0.0394.In the structure, the Bi(Ⅲ) centers are interconnected by oxalate ligands to produce honeycomb-like layers, which are further pillared by bridging ligand oxalate molecules to form a 3-D open-framework structure.Furthermore, the title compound exhibits blue luminescence with the emission peaks located at 394nm in the solid state at room temperature, and thus it could be useful in the field of photoactive materials.     

Synthesis,Crystal Structure and Spectral Properties of [Ce(NO3)5(H2O)2]·2(Hphen)·(H2O)

A novel complex [Ce(NO3)5(H2O)2]·2(Hphen)·(H2O) (phen =1,10-phenanthroline) with formula C24H24CeN9O18 and Mr = 866.64 has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group Pī with a = 7.5534(2), b = 8.083(2), c = 25.8377(6) A, α = 86.847(1), β = 89.937(1), γ = 86.981(1)o, V = 1572.94(6) A3, Dc = 1.830 g/cm3, F(000) = 866, β = 1.545 cm-1 and Z = 2. The final refinement gave R = 0.0486 and wR = 0.1278 for 4852 observed reflections with I > 2σ(I). It consists of discrete [Ce(NO3)5(H2O)2]2- anion, two Hphen+ cations and a lattice water molecule. In the compound, all of the five nitrates are bidentate, and the coordination of Ce(III) is 12. The photo-luminescence of this compound was also investigated.     

Synthesis and structure of nalidixium tetrachloroantimonate monohydrate, (C12H13N2O3)SbCl4 · H2O

Nalidixium tetrachloroantimonate monohydrate, (C₁₂H₁₃N₂O₃)SbCl₄ · H₂O, has been synthesized and its crystal structure has been determined. The structure is built of the [Sb₂Cl₈]^2? anions, C₁₂H₁₃N₂O ₃ ⁺ nalidixium cations, and H₂O molecules joint by hydrogen bonds and π-π-and Cl?Cl interactions. The [Sb₂Cl₈]^2? anion is a dimer of the SbCl₅ E distorted octahedra sharing common Cl?Cl edge (E is the lone electron pair). The Sb polyhedra contain two short Sb-Cl bonds (2.387 and 2.395 Å), one bond of a medium length (2.508 Å), and two long bridging bonds (2.745 and 3.054 Å).     

Synthesis and Crystal Structure of Triacetyltribenzyl-Hexaazaisowurtzitane (TATBIW·0.5 H)_2O)

The hexanitro hexaaza isowurtzitane (HNIW) (2, 4, 6, 8, 10, 12-hexanitro-2, 4, 6, 8, 10,12-hexaazatetracyclo-[5.5.0.05,9.03,11]-dodecane), more commonly called CL-20, be-longs to the family of high energetic dense caged nitramines. It was first synthesized byA.T.Nielsen in 19871. HNIW is superior to HMX with respect to density, velocity,detonation pressure and enthalpy of formation. Based on cylinder expansion andtantalume plate acceleration experiments, the HNIW was found to be appr…     

Synthesis, Properties and Crystal Structure of a Novel Coordinated Polymer: {(H2en)(H3O)[(BiPb(C2O4)4(H2O)2)]·2(H2O)}n

A novel oxalate compound {(H2en)(H3O)[BiPb(C2O4)4(H2O)2]·2(H2O)}n 1 (en = ethylenediamine) containing lead and bismuth has been synthesized by hydrothermal methods, and structurally characterized by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/c with a = 11.6160(1), b = 12.7426(1), c = 15.5683(5) (A), β = 108.442(4)°, BiPbC10N2O21H21, Mr = 921.46, V = 2186.0(4) (A)3, Z = 4, Dc = 2.800 g/cm3, F(000) = 1712 and μ(MoKα) = 15.837 mm-1. The final R = 0.0502 and wR = 0.1261 for 3391 observed reflections with I > 2(σI). The title com- pound consists of 2-D polyanions and protonized organic amine cations, and they are combined to each other by static attractive force and H-bonds to form the so-called organic-inorganic hybrid material.     

Synthesis and Crystal Structure of a One-dimensional Azido-bridged Manganese (II) Compound [Mn(N3)2(H2O)3·C6H12N4]n

A new one-dimensional azido-bridged manganese compound has been prepared and structurally characterized by X-ray diffraction. The complex [Mn(N3)2(H2O)3·C6H12N4]n crystallizes in space group Pnma with a = 6.5252 (5), b = 9.3226(7), c = 22.2070(15)(A), V = 1350.89(17)(A)3, Z = 4, Mr = 333.24, Dc = 1.639 g/cm3, μ= 1.005 mm-1 and F(000) = 692. The final refinement gave R = 0.0328 and wR = 0.0777 for 1085 observed reflections with I > 2σ(I). The structure contains [Mn- (N3)2(H2O)3]n polymeric chains and uncoordinated hexamethylenetetramine (HMTA) molecules with Mn/HMTA molar ratio of 1:1. The Mn atoms are bridged by end-to-end azido ligands to construct one-dimensional zig-zag infinite chains. Each Mn atom is six-coordinated by three N atoms of three azido ligands and three water O atoms, resulting in an octahedral geometry. Extending hydrogen- bonding interactions involving water O atoms, azido and HMTA N atoms link the chains and HMTA molecules into a three-dimensional network.     

Synthesis,Crystal Structure and Properties of Novel Composite Complex: [La(Nmp)4(H2o)4][HsiMo12O40]·2nmp·H2o

A new composite complex of [La(NMP)₄(H₂O)₄][HSiMo₁₂O₄₀]·2NMP·H₂O (NMP = N-methyl-2- pyrrolidone) was synthesized and characterized by IR, UV, ESR, TG-DTA and single crystal structural analysis. The water and organic ligands (NMP) coordinate directly with La(III) to form a dodecahedral complex and the SiMo₁₂O^4? ₄₀ anion is the counter ion. IR and X-ray analysis show that there is strong interaction between the polyoxometalate and organic donors. The complex is strongly photosensitive under irradiation with sunlight, resulting in a charge-transfer complex by oxidation of the N-methyl-2-pyrrolidone and reduction of the polyoxometalate. Low temperature ESR spectra indicate thermal electron delocalization among the Mo atoms in the title compound.