Synthesis, Crystal Structure and Magnetic Properties of a New Zn(Ⅱ)-Nitronyl Nitroxide Complex

A new complex [Zn(NIT-1'-MeBzIm)Cl2(H2O)] (NIT-1'-MeBzIm = 2-{2'-[(1'-methyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-l-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method. Crystal data: monoclinic, space group P21/n, Z = 4, C15H21Cl2N4O3Zn, Mr = 441.63, a = 7.2225(10), b = 30.849(4), c = 8.8758(13) (A), β= 103.904(2)°, V = 1919.6(5) A3, Dc = 1.528 g/cm3, μ(MoKα) = 1.579 mm-1, F(000) = 908, R = 0.0436 and wR = 0.1029 for 2456 observed reflections with Ⅰ> 2σ(Ⅰ). X-ray analysis reveals that the Zn(Ⅱ) ion is four-coordinated with a distorted tetrahedron. There also exist H-bonds, π-π piling interactions and weak intermolecular contacts between the NO groups which form a mutual stagger 3-D network configuration. Magnetic investigation reveals that there exists intermolecular antiferro- and ferromagnetic interactions in the title complex.     

A New One-dimensional Dicyanamide Bridged Zinc(II) Complex Containing Nitronyl Nitroxide Radicals:Synthesis,Crystal Structure and Magnetic Properties

A new one-dimensional dicyanamide bridged zinc(II) complex containing nitronyl nitroxide radicals Zn(NO3)(NIT-1'-MeBzIm)(dca)n·(H2O)n(NIT-1'-MeBzIm = 2-{2'-(l'-me-thyl)benzimidazolyl}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, dca = dicyanamide anion) has been prepared and structurally characterized by single-crystal X-ray diffraction.The complex crystallizes in triclinic, space group P1, with a = 7.428(3), b = 9.839(3), c = 16.708(6), α = 93.270(4), β = 101.642(4), γ = 100.632(4)°, C17.5H21N8O5.5Zn, Mr = 496.79, V = 1169.7(7) 3, Dc = 1.411 g/cm3, μ(MoKα) = 1.096 mm-1, Z = 2, F(000) = 512, R = 0.0583 and wR = 0.1663 for 4295 observed reflections with I > 2σ(I).X-ray analysis reveals that the zinc(II) ion is six-coordinated with a distorted octahedral geometry.These units develop as 1D species where dicyanamide ligands bridge zinc(II) ions.In addition, molecules are linked by π-π piling interactions to form 1-D double-chains.Magnetic investigation indicates that the weak intramolecular interactions are antiferromagnetic with J =-0.27 cm?1, where the spin Hamitonian is defined as H =-2∑i,jJi,jSiS within the complex.     

A New One-dimensional Dicyanamide Bridged Zinc(Ⅱ) Complex Containing Nitronyl Nitroxide Radicals: Synthesis,Crystal Structure and Magnetic Properties

A new one-dimensional dicyanamide bridged zinc(Ⅱ) complex containing nitronyl nitroxide radicals [Zn(NO3)(NIT-1'-MeBzim)(dca)]n·(H2O)n (NIT-1'-MeBzIm = 2-{2'-[(1'-me-thyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoine-1-oxyl-3-oxide, dca = dicyanamide anion) has been prepared and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in trielinic, space group P1, with a = 7,428(3), b = 9.839(3), c = 16.708(6) A, а = 93.270(4), β= 101.642(4),γ= 100.632(4)°, C17.5H21N8O5.5Zn, Mr = 496.79, V= 1169.7(7) A3, Dc = 1.411 g/cm3,μ(MoKa) = 1.096 mm-1, Z = 2, F(000) = 512, R = 0.0583 and wR = 0.1663 for 4295 observed reflections with I > 2σ(I). X-ray analysis reveals that the zinc(Ⅱ) ion is six-coordinated with a distorted oetahedral geometry. These units develop as 1D species where dieyanamide ligands bridge zine(Ⅱ) ions. In addition, molecules are linked by π-π piling interactions to form 1-D double-chains. Magnetic investigation indicates that the weak intramoleeular interactions are antiferromagnetic with J = -0.27 cm-1, where the spin Hamitonian is defined as H = -2 ∑ijJijSiS within the complex.     

A Novel Complex of Na（I）-Nitronyl Nitroxide [Na（NIT- 1＇-MeBzIm）3]ClO4： Synthesis and Crystal Structure

A novel complex [Na（NIT-1＇-MeBzIm）3]ClO4 （NIT-1＇-MeBzIm = 2-{2＇-[（1＇- methyl）benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide） has been prepared and structurally characterized by elemental analysis, IR spectra and X-ray diffraction methods. The title complex crystallizes in trigonal, space group P3 and Z = 2. Crystal data： C45H57ClN12NaO10, Mr = 984.47, a = 13.9411（8）, b = 13.9411（8）, c = 14.8622（16） A, γ= 120°, V= 2501.5（3） A^3, Dc = 1.307 g/cm^3, μ（MoKα） = 0.152 mm^-1, F（000） = 1038, R = 0.0637 and wR = 0.1813 for 1957 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the Na（I） ion is six-coordinated with three NIT-1＇-MeBzlm radicals. As we know, three radicals coordinating to the Na（I） ion in the main group by a chelate way is the first example. The Na（I） ion resides in a distorted octahedron with a facial configuration. Meanwhile, the intermolecular weak interactions result in a 2-D double layer conformation where the uncoordinated perchlorate anions are inserted in the packing space and take part in the H-bond interactions, and each complex is connected with six neighboring complexes and three perchlorate anions.     

Synthesis, Crystal Structure and Magnetic Properties of a Co(Ⅱ) Complex Containing 2'-(1'- Methyl)benzimidazolyl-substituted Nitronyl Nitroxide

A new complex [Co(NIT-1'-MeBzIm)<,2>Cl<,2>] (NIT-1'-MeBzIm = 2-{2'-[(1'-methyl)- benzimidazolyl] }-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method.The complex crystallizes in the monoclinic system, space group C2/c, Z = 4.Crystal data: C<,30>H<38>Cl<,2>CoN<,8>O<,4>, M<,r> = 704.51, a = 17.074(3), b = 21.350(3), c = 11.6962(19) (A), β= 108.879(2)°, V= 4034.3(11) (A)<'3>, D<,c> = 1.160 g/cm<'3>,μ(MoKα) = 0.597 mm<'-1>, F(000) = 1468, R = 0.0422 and wR = 0.1141 for 2577 observed reflections with I > 2σ(I).X-ray analysis reveals that the Co(Ⅱ) ion is six-coordinated with a distorted octahedral geometry.Temperature dependenee of susceptibility measurements shows the existence of antiferromagnetic interactions between the Co(Ⅱ) ion and the radicals (J= -52.88 cm<'-1>).     

Synthesis and Crystal Structure of 3,3＇-Bis（2-benzimidazolyl）-2,2＇-dipyridine with Hydrated Zinc（Ⅱ） Perchlorate

The reaction of Zn(ClO4)2·6H2O with 3,3'-bis(2-benzimidazolyl)-2,2'-dipyridine (L) gave a mononuclear zinc(II) complex: [ZnL2](ClO4)2·2DMF·4H2O, which was structurally characterized by EA, IR, UV, 1H NMR, fluorescence spectrum and single-crystal X-ray diffraction. The crystal (C54H54Cl2N14O14Zn, Mr = 1259.38) belongs to the monoclinic system, space group C2/c with a = 20.874(2), b = 14.9953(16), c = 20.462(3) , β = 101.553(2)°, V = 6274.8(13) 3, Z = 4, Dc = 1.333 g/cm3, F (000) = 2608, μ(MoKα) = 0.548 mm–1, R = 0.0682 and wR = 0.1931 for 4984 observed reflections with I > 2σ(I). The Zn(II) is four-coordinated in a slightly distorted tetrahedral geometry through four N atoms from four benzimidazole units of two ligands. In the crystal lattice, the [ZnL2]2+ cations are linked to each other by extensive intermolecular hydrogen bonds between nitrogen atoms of benzimidazole rings, water and DMF molecules.     

Synthesis,Crystal Structure and Magnetic Properties of a Co(Ⅱ) Complex Containing 2′-(l′-Methyl)benzimidazolyl-substituted Nitronyl Nitroxide

A new complex [Co(NIT-1′-MeBzIm)2Cl2](NIT-1′-MeBzIm = 2-{2′-[(l′-methyl)-benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method.The complex crystallizes in the monoclinic system,space group C2/c,Z = 4.Crystal data:C30H38Cl2CoN8O4,Mr = 704.51,a = 17.074(3),b = 21.350(3),c = 11.6962(19),β = 108.879(2)°,V = 4034.3(11)3,Dc = 1.160 g/cm3,μ(MoKα) = 0.597 mm-1,F(000) = 1468,R = 0.0422 and wR = 0.1141 for 2577 observed reflections with I > 2σ(I).X-ray analysis reveals that the Co(Ⅱ) ion is six-coordinated with a distorted octahedral geometry.Temperature dependence of susceptibility measurements shows the existence of antiferromagnetic interactions between the Co(Ⅱ) ion and the radicals(J =-52.88 cm-1).     

Synthesis and Crystal Structure of Bisaqua-[N,N'-bis(3,5-dichlorosalicylidene)-1,3-diaminopropano]zinc(II)

1 INTRODUCTION N,N?-Bis(salicylidene)-1,3-diaminopropane (BSDP) is a versatile tetradentate ligand, which forms stable complexes with a large number of transition metals[1～3]. However, the complexes related to the BSDP deriva- tive,N,N?-bis(3,5-dichlorosalicylidene)-1,3-diamino- propane (BCDP), have been seldom reported. The prime interest in these complexes is their ability to afford functional solid materials with potentially controllable properties and novel molecular struc- tur…     

Synthesis and Crystal Structure of N-Hydroxy-9-(3’,4’-methylene- dioxyphenyl)-1,8-dioxo-1,2,3,4,5,6,7,8,9, 10-decahydroacridine in Aqueous Media

1 INTRODUCTION Acridine derivatives are described to have many applications, such as biological fluorescent probes[1] as well as anti-tumor[2], anti-bacterial[3], anti-HIV[4] and anti-malarial[5] agents. Because of the importance of acridine derivatives, much work has been done for several decades. Among them the classical synthetic methods involve condensing functionalized anilines and o-halogeno- benzoic acid derivatives as well as several other steps resulting in the desired acridine[…     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Mo(V) Phosphate [Zn(Mo~v_6P_4O_(31)H_(10))_2(C_4H_(14)N_3)_2]·2C_4H_(13)N_3·8H_2O

1 INTRODUCTION Hydrothermal synthesis of Mo(V) phosphates has allowed various structures, all characterized by the presence of identical clusters with the composition Mo12MP8X62 (X = O, OH) to be stabilized[1～6]. Many Mo(V) phosphates with such clusters have been iso- lated to date. The first compound was discovered by Haushalter and Lai[1] for M = Na with the formula (PPh4)2[(H3O)2NaMo6P4O24(OH)7]?5H2O. Recently, a second type of structure has been observed for M = Na (Na8(…     

Dinuclear Copper（Ⅱ） Complex with a New Polycarboxylate Ligand：Syntheses,Characterization and Crystal Structure

A dinuclear copper(Ⅱ) complex,[Cu2(HL)2(H2O)6] 1(H3L = 2,4,6-tri(3-carboxy-phenylthio)-1,3,5-triazine),was synthesized hydrothermally and characterized by single-crystal X-ray diffraction,IR and thermal analysis.Single-crystal X-ray diffraction reveals that complex 1 is a dinuclear copper(Ⅱ) complex,which is further extended to a 3D network by weak interactions such as O…H-O hydrogen bonds and noncovalent S...S interactions.The crystal of compound 1 belongs to monoclinic,space group C2/c,with a = 50.15(2),b = 6.789(3),c =15.667(8) ,β = 90.588(9)o,V = 5334(4) 3,Z = 4,C48H38Cu2N6O18S6,Mr = 1306.28,Dc = 1.627 g/cm3,F(000) = 2664,Rint = 0.0631,T = 293(2) K,μ = 1.112 mm-1,the final R = 0.0661 and wR = 0.1850 for 3782 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of a Coordination Polymer {[Co(phth)(phen)(H_2O)]·(C_2H_5OH)}_n

1 INTRODUCTION Metal-organic coordination polymer has particu- lar and special structure characters with some caves, holes and channels[1], and can be used in selected catalysis, molecular recognition, reversible exchan- ge of host-guest molecules (ions), super purity sepa- ration, biological conductor[2～5], etc. In the past ten years, polymers with bridging ligand have been widely investigated[6, 7]. The development of supra- molecular architectures of inorganic-organic hybrid molecules …     

A Zn(II) 5-Aminoisophthalate Coordination Polymer

The title compound, [Zn(AIP)(4,4-bipy)0.5(H2O)]n·0.75nH2O 1, was synthesized via the hydrothermal reaction of Zn(OAc)2 with 5-aminoisophthalic acid (H2AIP) and characterized by elemental analysis and infrared spectra. The complex crystallizes in monoclinic system, space group P21/c with a = 12.672(1), b = 7.6557(4), c = 16.181(1) , β = 109.187(2)o, V = 1482.6(2) 3, Z = 1, C52H52N8O23Zn4, Mr = 1418.58, Dc = 1.589 g/cm3, F(000) = 724 and μ(MoKα) = 1.685mm-1. The final R = 0.0702 and wR = 0.1524 for 1847 observed reflections with I > 2σ(I), and R = 0.0873 and wR = 0.1664 for all data. X-ray diffraction studies reveal that the title compound has an interesting 2D microporous architecture with guest water molecules inside the channel.     

Two New Coordination Polymers Assembled with a Functionalized Ligand：Syntheses and Crystal Structures

Two new transition-metal organic coordination polymers [M(mna)2](M = Cd(1),Zn(2);mna = 2-mercaptonicotinic anion) have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction along with IR and elemental analyses.Compound 1 is generally a one-dimensional linear structure bridged through the sulfur donor of mna ligand,while 2 is a one-dimensional zigzag chain ligated via the oxygen donor of mna ligand.These compounds further result in three-dimensional structures via intermolecular π...π stacking interactions and/or hydrogen bonding interactions.The two compounds were structurally determined by single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic space group P21/c with a = 3.730(3),b = 13.973(12),c = 12.380(11) ,β = 97.953(18)°,V = 639.0(10) 3,Z = 2,CdC12H8O4N2S2,Mr = 420.72,Dc = 2.187 g/cm3,F(000) = 412,Rint = 0.0252,T = 293(2) K,μ = 2.052 mm?1,the final R = 0.0269 and wR = 0.0586 for 1377 observed reflections with I > 2σ(I).Complex 2 belongs to monoclinic space group P21/c with a = 13.376(2),b = 12.8429(14),c = 7.4856(10) ,β = 96.190(10)°,V = 1278.5(3) 3,Z = 4,ZnC12H8O4N2S2,Mr = 373.69,Dc = 1.941 g/cm3,F(000) = 752,Rint = 0.0414,T = 293(2) K,μ = 2.264 mm?1,the final R = 0.0418 and wR = 0.0966 for 2396 observed reflections with I > 2σ(I).     

Synthesis,Structure, and Luminescent and Dielectric Properties of a Novel 1D Chain Zinc(Ⅱ) Complex {[Zn(DCImPyO)·(H_2O)_2·]·H_3O}_n

Under hydrothermal conditions, 4-(4,5-dicarboxy-1H-imidazol-2-yl)pyridine 1-oxide (H3DCImPyO) reacted with ZnCl2 to give the 1D chain complex {[Zn(DCImPyO)·(H2O)2·]·H3O}n (1). Single-crystal X-ray determination shows that complex 1 crystallizes in the monoclinic system, space group P2 1 /c with a=9.488(2), b=13.247(3), c=12.959(4) , β=126.716(19)°, Z=4, V=1305.6(6) 3 , C10H11N3O8Zn, D c=1.865 g/cm3 , M r=366.61, λ(MoKa)=0.71073 , μ=1.930 mm -1 , F(000)=744, R=0.0472 and wR=0.1487. Fluorescent analysis showed an intense emission band at 422 nm when the exciting radiation was set at 378 nm. Dielectric constant of complex 1 was measured at different frequencies with temperature variation.     

Synthesis,Structure and Photoluminescence of a Binuclear Zinc（Ⅱ） Coordination Polymer Based on 2-Carboxycinnamic Acid and Dipyrido [3,2-a： 2＇,3 ＇-c]-phenazine

A binuclear zinc（Ⅱ） complex with 2-carboxycinnamic acid （2-ccm） and dipyrido- [3,2-a：2＇,3＇-c]phenazine （DPPZ）, {[Zn2（2-ccm）2（DPPZ）2]·2H2O}n, was synthesized and characterized by elemental analysis, IR, single-crystal X-ray diffraction, thermal gravimetry and fluo- rescent emission. It crystallizes in monoclinic, space group P21/c with a = 13.409（4）, b = 25.530（7）, c = 13.952（4） A, β = 99.554（3）°, V= 4710（2） A3, Z= 4, C56H36N8O10Zn2, Mr= 1111.67, Dc = 1.568 g/cm3, μ（MoKα） = 1.093 mm^-1, F（000） = 2272, R = 0.0422 and wR = 0.0895. In the crystal, the basic unit of 1 is a binuclear Zn2 entity which is linked by 2-ccm ligand to form a 1D double chain along the a axis. The O-H...O hydrogen bonding and π-π interactions lead to a 3D supramolecular motif. In addition, thermal and luminescent properties of complex 1 have also been investigated.     

Synthesis and Crystal Structure of 2-(4-Nitrophenyl)-1,2-benzisoselenazol-3(2H)-one DMF (1:1) Solvate

The title compound (C13H8N2O3Se-C3H7NO) has been synthesized by a simple synthetic route and by recrystallization from DMF. The molecular structure of this compound was obtained by single-crystal X-ray diffraction. The compound crystallized in the triclinic space group P with a = 7.450(6), b = 8.150(7), c = 13.859(12) , α = 75.014(14), β = 83.072(18), γ = 84.409(14)°, V = 805.0(12)3, Z = 2 and R = 0.0271 for 2575 observed reflections with I > 2σ(I). X-ray analysis reveals that not only intermolecular Se…O and C-H…O interactions, but also π…π stacking interactions exist in the adjacent molecules. The above three kinds of intermolecular interactions extend the complex into an infinite three-dimensional layered network.     

Urothermal Synthesis and Crystal Structure of a Zn（Ⅱ） Coordination Polymer with a 3-D Supramolecular Structure

A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I >2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).     

Syntheses and Crystal Structures of Two New One-dimensional Double Hydrogen-bonding-chain Complexes [Ni(bipy)_2Cl]·ClO_4 and [Zn(bipy)_2Cl]·BF_4

Two new transition metal complexes, [Ni(bipy)2Cl]·ClO4 (bipy = 2,2'-bipyridine) 1 and [Zn(bipy)2Cl]·BF4 2, have been synthesized and characterized by single-crystal X-ray diffraction analysis. Both 1 and 2 crystallize in monoclinic space group P21/n with Z = 4. For 1, a = 10.776(1), b = 12.067(1), c = 16.146(2) , β = 93.021(2)o, V = 2031.9(4) 3, Mr = 505.98, Dc = 1.654 g/cm3, μ = 1.255 mm–1, F(000) = 1032, the final R = 0.0406 and wR = 0.1002 for 3983 observed reflections with I > 2σ(I). For 2, a = 10.758(4), b = 12.058(4), c = 16.135(5) , β = 104.57(1)o, V = 2025.7(12) 3, Mr = 500.00, Dc = 1.639 g/cm3, μ = 1.396 mm–1, F(000) = 1008, the final R = 0.0470 and wR = 0.1237 for 3759 observed reflections with I > 2σ(I). The crystal structures of 1 and 2 are isostructural with very similar supramolecular structures. A one-dimen-sional zigzag double hydrogen-bonding-chain is generated by the intermolecular M-bipy ···anion···bipy- M hydrogen bonding interactions between the chelating ligands of bipy and anion.     

Synthesis,Structure and Photoluminescent Property of a Cd-organic Complex [Cd（L）_2（pbda）]_n

A new complex,[Cd(L)2(pbda)]n(1,L = 3-(2-pyridyl)-4-(p-methoxyphenyl)-5-(2-thienyl)-1,2,4-triazole,H2pbda = 1,4-benzenedicarboxylic acid),has been hydrothermally prepared and characterized by single-crystal X-ray diffraction,IR spectroscopy,elemental analysis and PXRD.The complex crystallizes in monoclinic,space group P21/c with a = 8.2929(9),b = 21.668(2),c = 10.9940(11) ,β = 90.242(2)o,V = 1975.5(4) 3,Z = 2,C44H32N8O6S2Cd,Mr = 945.30,Dc = 1.589 g/cm3,μ = 0.721 mm-1,S = 1.097,F(000) = 960,the final R = 0.0590 and wR = 0.1045 for 3846 observed reflections(I > 2σ(I)).In the title complex,the rigid bridging pbda2-ligands utilize oxygen atoms of carboxylate groups to coordinate with Cd(II) atoms to form one-dimensional chains which are further interlinked into a three-dimension framework via the intermolecular weak interactions.Photoluminescence study revealed that complex 1 exhibits strong fluorescent emission band in the solid state at room temperature.