A Chain Structure Based on Homodinuclear Scandium Units： [Sc（μ-OH）（2,5-pydc）（H2O）]n

The reaction of pyridine-2,5-dicarboxylic acid with Sc2O3 under hydrothermal con- dition yields a new complex [Sc（μ-OH）（2,5-pydc）（H2O）]n 1 which has a chain structure based on homodinuclear scandium units. Crystal data for 1： space group P^-1, a = 6.7192（13）, b = 7.6131（13）, c = 8.9313（14） A, α = 95.976（6）, β = 101.663（6）, γ = 108.151（5）^o, V= 418.26（13） A^3, Z = 2, Dc = 1.946 g/cm^3, g = 0.889 mm^-1, F（000） = 248, C7H6NO6Sc, Mr = 245.09, the final R = 0.0429 and wR = 0.1086.     

Hydrothermal Synthesis and Crystal Structure of a Cadmium(Ⅱ) Polymer with One-dimensional Chain Structure: [Cd(MDPPz)(BDC)(H2O)]n

A metal-organic coordination compound formulated as [Cd(MDPPz)(BDC)(H2O)]n 1 (MDPPz = 11-methyldipyrido[3,2-a:2',3'-c]phenazine, BDC = 1,4-benzenedicarboxylate) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group C2/c, with a = 30.673(8), b = 9.623(3), c = 20.784(6) (A), β = 98.646(3)o, V = 6065(3) (A)3, C27H17CdN4O5, Mr = 589.85, Dc = 1.292 g/cm3, μ(MoKα) = 0.757 mm(1, F(000) = 2360, Z = 8, the final R = 0.0381 and wR = 0.0855 for 4191 observed reflections (I＞2σ(I)). 1 exhibits blue fluorescence property at room temperature.     

Synthesis and Crystal Structure of a Macrocycle [Cu(dadm)(mal)(H2O)]2·2H2O

The reaction of 4,4′-diaminodiphenylmethane (dadm), malonic acid (H2mal) and Cu(NO3)2 in aqueous solution results in a discrete binuclear Cu(II) macrocycle: [Cu(dadm)(mal)- (H2O)]2(2H2O. It crystallizes in monoclinic, space group P21/c with a = 15.231(3), b = 11.847(2), c = 9.801(2)A,Z= 106.75(3)o, V = 1693.5(6)A3, Z = 2, C32H40Cu2N4O12, Mr = 799.76, Dc = 1.568 g/cm3, λ(MoK() = 0.71073A, μ = 1.325 mm-1, F(000) = 828, the final R = 0.0531 and Wr = 0.1244 for 3421 observed reflections with I > 2σ(I). Each Cu(II) is coordinated by two oxygen atoms from a mal ligand, two nitrogen atoms from two dadm ligands and a water oxygen atom to form a triangle bipyramidal motif. The title compound possesses a distorted macrocycle enclosed by dadm with approximate dimensions of 8.3A× 5.9A.     

Formation and Structure of [Al_(13)(μ_3-OH)_6(μ_2-OH)_6(μ_2-OH)_(12)(H_2O)_(24)]Cl_(15)·13H_2O

1 INTRODUCTION At present, the polyaluminium compounds are mainly studied by single-crystal X-ray diffraction method to obtain the components, structures and exis- tence forms of aluminium in hydrolysis system, and then hydrolysis courses and mechanisms of each hydrolytic polyaluminium cation could be further dis- closed[1～5]. Generally, the single crystals suitable for X-ray diffraction are obtained from the crystallization of polyaluminium cations into sulfates or selenates. Following …     

Crystal Structure of Calcium [Aqua(Nitrilotriacetatocobaltate(II)] Tetrahydrate,Ca[Co(Nta)(H2O)]2· 4H2O

Crystals of Ca[Co^II(Nta)]₂· 6H₂O (I), where Nta^3–is a nitrilotriacetate ion, were synthesized and studied using X-ray diffraction analysis. They were found to be monoclinic: a= 6.991(1), b= 10.031(1), c= 16.238(3) Å, = 98.50(1)°, V= 1126.2(3) ų, space group P2₁/n, Z= 2, R ₁= 0.0241, wR ₂= 0.0636, GOOF = 1.050 (for 3132 reflections with I> 2(I)). Structure Iis composed of {[Co(Nta)(H₂O)]^–}₁anion chains united by Ca²⁺cations into a three-dimensional framework. The coordination polyhedra of Co and Ca atoms are distorted octahedra. The Co(II) atom environment includes atoms N(1), O(1), O(3), and O(5) of one Nta^3–ligand, a carbonyl O(2)" atom of the neighboring anion fragment, and an O(w1) atom of the water molecule. The shortest bond is formed by the Co atom with the bridging O(2)" atom in trans-position relative to atom N(1). The Co–O(2)" distance (2.029 Å) is noticeably shorter than the other bond lengths, Co–O(Nta) (2.069–2.103 Å), Co–O(w1), and Co–N(1) (2.155 and 2.177 Å, respectively). Cations Ca²⁺are located in the inversion centers and involve in their coordination atoms O(4), O(6), O(w2), and the oxygen atoms symmetrically bond to them and arranged at 2.271(1), 2.420(1), and 2.351(2) Å, respectively. The structural formula of the title compound is {Ca(H₂O)₂[Co(Nta)(H₂O)]₂}₃· 2H₂O.     

Hydrothermal Synthesis and Crystal Structure of a Cobalt(Ⅱ) Polymer with One-dimensional Chain Structure: [ Co(phen) (BDC)(H2O)]n·0.5nH2BDC

A metal-organic coordination polymer [Co(phen)(BDC)(H2O)]n·0.5nH2BDC(H2BDC = terephthalic acid, phen = 1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in triclinic, space group P1- with a = 9.771(3), b =10.739(3), c= 11.249(4) (A), α = 75.946(3), β = 65.306(3), γ = 86.073(4)°, V = 1039.6(6)(A)3, C24H17CoN2O7, Mr=504.33, Dc = 1.611 g/cm3, μ(MoKa) = 0.878 mm-1, F(000) = 516, Z = 2, the final R = 0.0547 and wR = 0.1138 for 2916 observed reflections (I＞ 2σ(Ⅰ)). It exhibits a one-dimensional zigzag chain-like structure.     

A New Chain-like Copper(II) Polymer: [Cu(MOPIP)(BDC)]n·0.5n(H2O)

A metal-organic coordination compound formulated as [Cu(MOPIP)(BDC)]n·0.5n(H2O) 1(MOPIP = 2-(4-methoxyphenyl)-1H-imidazo[4,5-f][1,10] phenanthroline, BDC = 1,4-benze Nedicar- boxylate) has been hydrothermally synthesized and structurally characterized by elemental analysis, thermogravimetric analysis, IR spectrum, and single-crystal X-ray diffraction. The title compound crystallizes in the triclinic system, space group P, with a = 8.872(5), b = 11.163(6), c = 12.589(6) ?, α = 94.687(7), β = 99.930(6), γ = 103.074(7)°, V = 1186.7(12) ?3, C28H19CuN4O5.5, Mr = 563.01, Dc = 1.576 g/cm3, μ(MoKα) = 0.973 mm(1, F(000) = 576, Z = 2, the final R = 0.0607 and wR = 0.1618 for 3419 observed reflections (I > 2((I)).     

Synthesis and Crystal Structure of a Two-dimensional Framework Supramolecular Complex [Mn(phen)(DPZDA)(H2O)]·2H2O

A novel two-dimensional supramolecular complex [Mn(phen)(DPZDA)(H2O)]·2H2Ohas been synthesized by the reaction of Mn(CH3COO)2, 1,10-phenanthroline (phen) and H2DPZDA (3,5-dimethyl-pyrazine-2,6-dicarboxylic acid). Elemental analysis, IR spectra and X-ray singlecrystal diffraction were carried out to determine the composition and crystal structure of the title complex. Crystal data: triclinic system, space group P-1, a = 7.7474(13), b = 9.3381(15), c =15.146(3)(A), α = 93.872(3), β = 102.451(11), γ = 105.261(11)°, C20H20MnN4O7, Mr = 483.34, Z = 2,F(000) = 498, V = 1023.2(3)(A)3, Dc = 1.569 g/cm3, μ = 0.697 mm-1, -9≤h≤9, -11 ≤k≤ 10, -18≤l≤12, R = 0.0365 and wR = 0.0901 for 3585 independent reflections (Rint = 0.0165) and 2923observed reflections (I ＞ 2σ(I)). Structural analysis indicates that Mn(Ⅱ) adopts a distorted octahedral geometry. The 2-D framework supramolecular structure of the title complex is constructed from hydrogen bonds and π…πinteractions.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

{[Eu(2,5-PDA)(OAc)(H2O)]·1.5H2O}n稀土配合物的晶体结构及荧光性质

在水热条件下合成了一个新的2,5-吡啶二羧酸的稀土配合物{[Eu(2,5-PDA)(Oac)(H2O)]·1.5H2O}n.通过元素分析和X射线单晶衍射确定了该化合物的组成和晶体结构, 并对荧光性质进行了表征.该晶体属单斜晶系, P21/n空间群, 晶胞参数a=0.935 01(15) nm, b=0.834 77(13) nm, c=1.677 9(3) nm, β=106.18°;V=1.257 8(3) nm3, Z=4, 最后的一致性因子[I＞2σ(I)]: R1=0.024 3, Wr2=0.060 5.标题化合物中醋酸根的羧基以螯合-桥联三齿的方式将2个不对称单元中的铕离子连接起来形成二核单元, 2,5-PDA配体分别从与醋酸根和铕离子的平面成88°和56°夹角的方向将二核单元连接起来, 从而形成了由配位键构筑的三维结构, 未配位水分子通过氢键存在于晶体中.     

Syntheses and Crystal Structures of Two New Compounds Containing Triarylamineand Benzoic Hydrazide Units [Zn(μ-O2CCH=CHCO2)(C3H4N2)(H2O)]n

Two new compounds containing triarylamine and benzoic hydrazide units, 4-[N,N-di(4-toyl)amino]benzaldehyde-N-(4-ethoxylphenyl)-formyl hydrazone 3a and 4-[N,N-di(4-toyl) amino]benzaldehyde-N-(2-ethoxylphenyl)-formyl hydrazone 3b, have been synthesized and their crystal structures (C30H29N3O2, Mr = 463.56) were interpreted by a combination technique of 1HNMR, IR, elemental analysis, mass spectra, UV-Vis spectra and X-ray crystallography, respec- tively. The crystal of 3a belongs to monoclinic, space group P21/n with a = 9.321(3) A, b = 11.046(4) A, c = 24.335(9) A, β=92.649(7)°, V = 2502.7(16) A3, Z = 4,μ =0.078 mm-1, Dc =1.230 g/cm3, F(000) = 984, the final R = 0.0590 and wR = 0.1316 for 4367observed reflections with I ＞ 2σ(I). The crystal of 3b belongs to monoclinic, space group P21/c with a = 10.637(4) A, b = 24.138(10) A, c = 10.398(4) A, β= 104.913(8)°, V= 2579.8(17) A3, Z = 4,μ = 0.075 mm-1, Dc = 1.194 g/cm3, F(000) = 984, the final R =0.0631 and wR =0.1006 for 4463 observed reflections with I ＞ 2σ(I). X-ray crystallography revealed that the nitrogen atom in the triarylamine moiety is of sp2 hybridization with the three phenyl rings twisted to each other.     

Synthesis and Crystal Structure of [Cd(NBA)(μ_3-OH)(4,4′-bipy)_(1/2)]_n

A new cadmium polymer [Cd(NBA)(μ3-OH)(4,4′-bipy)1/2]n 1 (NBA = m-nitrobenzoic acid and 4,4′-bipy = 4,4-bipyridine) has been synthesized by hydrothermal reaction. Its structure was determined by single-crystal X-ray diffraction method, and characterized by elemental analysis and IR spectrum. The crystal is of monoclinic, space group C2/c, with a = 15.6912(9), b = 25.9394(15), c = 6.7332(4) ′, β = 114.7700(10)°, V = 2488.4(3) 3, C12H9CdN2O5, Mr = 373.61, Z = 8, Dc = 1.995 g/cm3, μ = 1.776 mm-1, F(000) = 1464, R = 0.0411 and wR = 0.1128 for 2130 observed reflections (I > 2σ(I)). X-ray diffraction studies reveal that the compound features a layered structure, in which 4,4′-bipy ligands bridge Z type of double chains [Cd(μ3-OH)]n and NBA ligands locate at the two sides of the layer. The π-π interactions between the benzene rings of NBA ligands of two adjacent layers lead to the 3D framework.     

Preparation and Identification of a New [Cr2(NTA)2(μ-OH2)]·2H2O Complex

[Cr₂(NTA)₂(μ-OH₂)]·2H₂O is prepared by heating nitrilotriacetic acid (H₃NTA) with an aqueous suspension of freshly precipitated Cr₂O₃·nH₂O. Elemental analysis, IR spectra, UV/vis spectra, X-ray diffraction, thermogravimetric analysis, mass spectra and magnetic susceptibility measurements suggest the existence of a Cr-Cr bond. One of the three water molecules acts as a bridging ligand (μ-H₂O) while the other two are waters of crystallization.     

Synthesis, Structure and Antimicrobial Activity of a Cyclic Compound [Cu(Pmal)(Dadm)(H2O)]2·4H2O

A new copper compound constructed from H2 Pmal (phenylmalonic acid), Dadm (4,4-diaminodiphenylmethane) and Cu(Ⅱ) has been synthesized from H2O-EtOH-DMF solution, and is characterized by X-ray single-crystal diffraction and other measurements. The compound crystallizes in the monoclinic system, space group C2/c with a=13.7866(6), b=10.1557(4), c=30.9036(17), β=101.422(5)o, V=4241.2(3)3 , Z=4, Dc=1.547g/cm3 , Mr=987.94, F(000)=2056, μ(MoKα)=1.078 mm-1 , S=1.007, R=0.0453 and wR=0.987 for 2806 observed reflections (I>2σ (I)). The title compound is characteristic of the cyclic dimeric molecules which further aggregate through hydrogen bonds and π-π interactions to form a 3-D supramolecular network. The microbial activities of the title compound and its reagents are investigated with filter paper discs diffusion method. The results show that the activity of the title compound is slightly better than its precursor reagents.     

Synthesis and characterization of diorganotin(IV) derivatives from rhodanine (HRd): crystal structures of [(PhCH2)2Sn(Rd)(μ-OH)]2 and [n-Bu2Sn(Rd)(μ-OH)]2

The diorganotin(IV) complexes, [R₂Sn(Rd)(μ-OH)]₂ (R?=?Me (1), PhCH₂ (2), n-Bu (3), Ph (4); HRd?=?rhodanine), have been synthesized and characterized by IR and multinuclear (¹H, ¹³C, ¹¹⁹Sn) NMR spectroscopy. The structures of complexes 2 and 3 have been determined by single-crystal X-ray diffraction. Both crystal structures of 2 and 3 show the presence of asymmetrically bridging hydroxy groups leading to an Sn₂O₂ unit. Each atom in complex 1 is also coordinated by an N atom of ligand and two C atoms of the alkyl groups, so the Sn environment is based on a trigonal bipyramid. While in complex 2, a weak intermolecular Sn–O interaction has also been found between the two adjacent molecules, so the geometry of the Sn atom can be best described as six-coordinate octahedral. The salient feature of the supramolecular structure of complex 3 is that of a 1D polymer, in which the discrete molecules are connected through weak intermolecular Sn?···?O interactions.     

Di-μ-hydroxo bridge-cleavage reactions between [Co(nta)(μ-OH)]2 2− and different monodentate ligands

The cleavage of the di--hydroxo bridges of [Co(nta)(-OH)]₂ ^2– by dimethylaminopyridine (dmap) and pyridine (py) has been investigated. [Co(nta)(-OH)]₂ ^2– equilibrates rapidly in aqueous basic solutions with a mono--hydroxo bridged Co^III species [pK _OH = 3.26(2)] and both these species react with the incoming ligand to form different ion associated species which react in the subsequent rate-determining steps (k ₁ and k ₂) to form presumably a ligand-substituted, mono-bridged species, [(nta)(OH)Co--OH-Co(nta)(L)]^2–. Values for k ₂, the preferred mono--hydroxo bridged substitution pathway for these reactions, vary between 6.8(2) × 10^–4 s^–1 (py) and 8.5(4) × 10^–2 s^–1 (dmap).     

Kinetic studies on spontaneous ligand substitution in [Cr(S-pdtra)(H2O)]–NCS– and [Cr(edtrp)(H2O)]–NCS– systems

The kinetics of anation of [Cr(S-pdtra)(H2O)] and [Cr(edtrp)(H2O)] complexes (S-pdtra=S-propane-1,2-diamine-N,N,N -triacetate, edtrp=ethylenediamine-N, N,N-tripropionate) by thiocyanates and aquation of the [Cr(NCS)(S-pdtra)]– and [Cr(NCS)(edtrp)]– ions have been studied in aqueous HClO4 solutions. The rate laws and the activation parameters have been determined and discussed. The observed decrease in reactivity for the edtrp complexes corresponds with a changeover of the reaction mechanism from Ia to Id for reactions of the CrIII-S-pdtra and CrIII-edtrp species, respectively.     

Chromium(III) Complexes with Quadridentate Amines. Crystal Structure of [cis-β-Cr(trien)(C2O4)] Cl·2H2O (I) and [Cr2(μ-OH)2(μ-tren)2] Br4·2H2O (II)

[cis-g-Cr(trien) C₂O₄)] Cl·2H₂O (I) (CrC₈H₂₂N₄O₆Cl) crystallizes at 22°C, from deionized water solution as a racemate in space group Pn (No. 7). Lattice constants are: a = 7.193(2), b = 9.1545(12), c = 11.469(2) Å; g = 100.994(13)°; V = 741.3(3) ų and D_calc = 1.603 gcm^-3 (MW = 357.75, Z = 2). A total of 2251 data were collected, using MoK f radiation ( u = 0.71703 Å), over the range 4 h 2 è h 60°; of these, 1441 (independent and with I S 2 σ (I)) were used in the structural analysis. Data were corrected for absorption ( w = 9.81 cm^-1) and the transmission coefficients ranged from 0.8676 to 0.9942. The final R (F) and R_w(F) residuals were 0.0338 and 0.0764, respectively. The cations of (II) exist in the lattice as enantiomeric pairs. [Cr₂( w -OH)₂( w -tren)₂]Br₄ ·2H₂O (II) (Cr₂C₁₂H₄₂N₈O₄Br₄) crystallizes in the monoclinic space group P2₁/n (No. 14) with a = 10.835(2) Å, b= 7.859(3) Å, c = 16.397(2) Å, g = 105.45(2)°, V = 1345.7(5) ų3 and D_calc = 1.940 g cm^-1 (MW = 786.18, Z = 4). A total of 2467 data were collected, using MoK f radiation ( u = 0.71703 Å), over the range 4 h 2 è h 50°; of these, 1450 (independent and with I S 2 σ ( I )) were used in the structural analysis. Data were corrected for absorption ( w =67.79 cm^-1) and the transmission coefficients ranged from 0.5589 to 0.9949. The final R(F) and R_w(F) residuals were 0.0481 and 0.1408, respectively for 2385 observed reflections with ( I S 2 σ ( I )). In the complex cation, the two Cr(III) centers are in a distorted octahedral environment and are bridged by two hydroxide groups and two ethylamine arms, one from each tren ligand, which spans over the binuclear core. Within the bridging moiety, the Cr···Cr separation is 3.005(2) Å, the ° Cr-OH-Cr = 101.3(2)° and ° O-Cr-O = 78.7(2)°, while the average Cr-N bond distance trans to the hydroxo groups (2.085(6) Å) is shorter than the corresponding cis Cr-N distance (2.104(5) Å).