Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Nickle （II） Achieved from 5-Iodo-isophthalic Acid Ligand

A new coordination polymer [Ni（L）（m-bix）（H2O）]n （1, H2L = 5-iodo-isophthalic acid, m-bix=1,3-bis（imidazol-1-ylmethyl）-benzene） has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, powder XRD and single-crystal X-ray analysis. The crystal is of triclinic, space group Pī with a = 9.1638（3）, b = 10.2319（3）, c = 13.2463（4） ？, α = 80.1710（10）, β = 83.671（2）, γ = 70.3790（10）o,C22H19NiIN4O5, Mr = 605.02, V = 1150.85（6） ？3, Dc = 1.746 g/cm3, F（000） = 600, μ = 2.225 mm-1, S = 1.045 and Z = 2. The final R = 0.0388 and wR = 0.1257 for 5089 observed reflections with I 〉 2σ（I）. In the title complex, the M and P layers are arranged alternately to give a double-layer structure by the symmetry related hydrogen bonds, and these double-layers are further joined together to achieve a 2D supramolecular architecture through I···π interaction involving iodine atoms and imidazole rings. The thermal stability of the title complex was studied by thermal gravimetric （TG） and differential thermal analysis （DTA）.     

Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Cobalt(II) Achieved from 1,1′-Biphenyl-2,2′,6,6′-tetracarboxylic Acid Ligand

<正>A new three-dimensional coordination polymer {[Co(BPTC)_(0.5)(bix)]·(H_2O)}_n (1, H4BPTC = 1,1′-biphenyl-2,2′,6,6′-tetracarboxylic acid, bix = 1,3-bis(imidazol-1-ylmethyl)-benzene) has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, and single-crystal X-ray analysis. The crystal is of orthorhombic, space group Pbcn with a = 13.2975(10), b = 13.8424(12), c = 22.6367(17), CoC_(22)H_(19)N_4O_5, M_r = 478.34, V = 4166.7(6) ~3, D_c = 1.525 g/cm~3, F(000) = 1968, μ = 0.867 mm~(-1), S = 1.023 and Z = 8. The final R = 0.0683 and wR = 0.1529 for 3655 observed reflections with I > 2σ(I). In the title complex, the 2D Co-BPTC layer is formed through self-assembly of Co(II) ions and bridging BPTC~(4-) ligands in a molar ratio of 2:1. The metal-organic lattice layers are further united together through the second bridging ligand bix to form a 3D metal-organic framework. The thermal stability of the title complex was studied by thermal gravimetric (TG) and differential thermal analysis (DTA).     

A High Dimensional Coordination Polymer Based on [β-Mo8O26]4- Inorganic Building Block： Synthesis, Structure and Topology

A high dimensional copper coordination polymer {[Cu2(btb)2(H2O)4( -Mo8O26)] H2O}n(1, btb = 1,4-bis(1,2,4-triazol-1-yl)butane) based on [ -Mo8O26]4 anions and flexible bis(triazole) ligands has been synthesized and characterized by elemental analysis, IR spectra, single-crystal X-ray diffraction and thermal analysis. The crystallographic data show that complex 1 crystallizes in triclinic space group P with a = 9.7550(10), b = 10.3996(11), c = 10.9516(11), = 77.622(2), = 89.602(2), = 87.610(2), V = 1084.25(19)3, C16H34Cu2Mo8 N12O31, Mr = 1785.15, Dc = 2.734 g cm 3, μ(MoKα) = 3.303 mm 1, F(000) = 856, GOF = 1.060, Z = 1, the final R = 0.0376 and wR = 0.0982 for I > 2 (I). In 1, the inorganic building block [ -Mo8O26]4 anions are connected with each other to generate one-dimensional chains. Then the chains are further connected by Cu2+ ions to form a three-dimensional (3D) inorganic framework [Cu2( -Mo8O26)]n containing quadrangular channels, with the pcu alpha-Po primitive cubic topology. The btb ligands are encapsulated into the void of the 3D inorganic framework forming a new three-dimensional architecture. The thermal analysis illustrates that complex 1 retains a comparatively good thermal stability.     

Synthesis,Characterization and Molecular Structure of a Diiron Complex(μ-SCH_2CH_2CH_2S-μ)Fe_2(CO)_5(Ph_2PCH_3)

The title complex,(μ-pdt)Fe_2(CO)_5(Ph_2PCH_3)(pdt = SCH_2CH_2CH_2S),was obtained by the reaction of the parent complex(μ-pdt)Fe_2(CO)_6 with Ph_2PCH_3 and Me_3NO·2H_2O in good yield(90%). The title complex was characterized by IR,~1H NMR,~(31)P{~1H} NMR and ~(13)C{~1H} NMR spectroscopy as well as by single-crystal X-ray diffraction analysis. The molecular structure shows that the title complex contains a butterfly diiron propanedithiolate cluster with five terminal carbonyls and a monophosphine ligand Ph_2PCH_3. The crystal packing diagram reveals that intermolecular C H···O hydrogen bonds between CH_2 and carbonyls,π-π stacking interactions and van der Waals' interactions stabilize the solid state to form a three-dimensional network.     

Synthesis, Crystal Structure and Photoluminescent Property of a Novel Silver(Ⅰ) Compound {[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n

Self-assembly of Ag(Ⅰ) nitrate, 1,3-bis(4-pyridyl)propane (bpp) and phthalic acid monopotassium salt (KHphth) in CH3OH-H2O solution produced the title complex,{[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n, which was characterized by single-crystal X-ray diffraction,elemental analysis, IR spectrum, and photoluminescent spectrum. Single-crystal X-ray analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, with α =15.4174(5), b = 8.6398(2), c = 25.2466(8) (A), β = 91.072(1)°, V = 3362.34(17) (A)3, Z = 4,C34H37N5O9Ag2, Mr = 875.43, Dc = 1.729 g/cm3, μ = 1.228 mm-1, F(000) = 1768, the final R =0.0749 and wR = 0.1580 for 5754 reflections with I ＞ 2σ(I). The Ag atom is coordinated by two N atoms from two bpp molecules in an approximately linear geometry. The Ag(Ⅰ) ions are linked by the bpp molecules to form one-dimensional zigzag chains propagating along the c axis. The Hphth-and nitrate counter-ions are bridged by solvent water molecules through hydrogen bonds to generate a one-dimensional chain extending along the b axis. Electrostatic interactions between cations and anions, extensive hydrogen bonds and π-π interactions are responsible for the three-dimensional supramolecular structure. In the solid state, the compound exhibits blue photoluminescence with the maximum at 436 nm upon excitation at 344 nm.     

Solvothermal Synthesis and Crystal Structure of a Zn（II） Microporous Metal-organic Framework

A novel three-dimensional Zn(Ⅱ) coordination polymer, Zn3(C2H2N3)4(SiF6), has been synthesized under solvothermal conditions using 1H-1,2,4-triazole-3-carboxylic acid and zinc fluoride as the starting materials. The complex has been characterized by elemental analysis, IR, TG analysis and single-crystal X-ray diffraction analysis. The complex crystallizes in the tetragonal I4/mmm space group with a=11.592(0), c=7.526(1), V=1011.3(2)3 , Z=2, Mr=610.46, Dc=2.005 g/cm3 and F(000)=596. The final R=0.0312 and wR=0.067 for 319 observed reflections with I>2σ(I). In the title complex, the Zn centers are interconnected by μ 3 -bridging triazole ligands to form a microporous three-dimensional metal-organic framework.     

A Three-dimensional Zn~(Ⅱ) Based Coordination Polymer with 2-Fold Interpenetrated Topology Displaying Luminescent Property

A new coordination polymer, [Zn2(m-bix)(p-bdc)2](1), was synthesized under hydrothermal conditions by a reaction of 1,3-bis(imidazol-1-ylmethyl)benzene(m-bix), 1,3-benzenedicarboxylic acid(H2p-bdc) and Zn(NO3)2. The colorless block crystals of complex 1(C30H22N4O8Zn2) belong to the triclinic system, space group P1 with a = 10.213(2), b = 12.052(2), c= 12.392(3) A, α = 82.97(3), β = 76.04(3), γ = 78.02(3)o, V = 1443.8(5) A3, Z = 2, Dc = 1.604 g/cm-3,Mr = 697.26, F(000) = 708, R = 0.0403 and w R = 0.0907 for 4886 observed reflections(I 2σ(I)). In1, the tetrahedral ZnI I cations are linked by [p-bdc]2– anions into 2D sq1 networks, which are further connected by bix ligands forming an interesting 2-fold 4,4-connected mog-type 3D network with a point symbol of {4·64·8}2{42·62·82}. Complex 1 was characterized by elemental, IR spectroscopy,powder X-ray diffractions and thermalgravimetric analysis. In addition, complex 1 exhibits coordination induced photoluminescent property.     

Synthesis,Crystal Structure and Characterization of a Ni(Ⅱ) Complex of Constructed 2,6-Bis(benzimidazol-2-yl) pyridine

A fluorescent Ni(II) complex 1, [Ni(OH-H2Bdc)(Bibimp)]n·nH2O, constructed with 5-hydroxyisophthalic acid(OH-H2Bdc) and 2,6-bis(2-benzimidazolyl)pyridine)(Bibimp) has been synthesized by hydrothermal methods and structurally characterized by elemental analysis, IR spectroscopy, TG/DTG, fluorescence spectrum and single-crystal X-ray diffraction. The title complex crystallizes in triclinic system, space group P1 with a = 10.187(2), b = 10.273(2), c = 13.401(3), α = 69.65(3), β = 69.66(3), γ = 70.61(3)o, V = 1196.8(4) 3, and Z = 2. The adjacent chains of complex 1 are stacked offset with respect to each other in an ABAB fashion by van der Waals interactions, and only a weak interlayer nonclassical C–H···O hydrogen bond has been observed. Complex 1 displays strong blue fluorescent emissions at 483 nm in the solid state upon photo-excitation at 365 nm at room temperature.     

Hydrothermal Synthesis and Crystal Structure of a Manganese(II) Coordination Polymer with 1,1′-Biphenyl-2,2′,6,6′-tetracarboxyl Acid and 2,2′:6,2′′-Terpyridine Ligands

The title compound {[Mn(H2BPTC)(tpy)(H2O)]·(H2O)3}n (1, H4BPTC = 1,1′- biphenyl-2,2′,6,6′-tetracarboxylic acid, tby = 2,2′:6,2′′-terpyridine) has been synthesized by the hydrothermal reaction, and its structure was determined by X-ray diffraction and characterized by elemental analysis, IR spectrum and thermogravimetric analysis. The crystal is of monoclinic, space group P21/c with a = 10.971(2), b = 20.776(4), c = 14.332(3) , β = 109.25(3)o, MnC31H27N3O12, Mr = 688.50, V = 3084.1(10) 3, Dc = 1.483 g/cm3, F(000) = 1420, μ = 0.498 mm-1, S = 1.066 and Z = 4. The final refinement gave R = 0.0447 and wR = 0.1103 for 5107 observed reflections with I > 2σ(I). The title complex has a {[Mn(H2BPTC)(tpy)(H2O)]}n chain structure, and the hydrogen bonding interactions make it more stable. Each chain is further connected to the adjacent ones through π···π, C-H···π and rich hydrogen bonds to form a metal-organic coordination polymer.     

Synthesis,Structure and Properties of a New Lead(Ⅱ) Complex of 1,3-Benzenedicarboxylic Acid, 1,10-Phenanthroline and Its Thermal Decomposition to PbO Micro-crystal Particles

The self-assembly of 1,10-phenanthroline(phen) and 1,3-benzenedicarboxylic acid(H2bdc) with Pb(NO3)2 under solvothermal conditions in N,N-dimethylacetamide(DMA) gives rise to a one-dimensional chain coordination polymer, [Pb(phen)(bdc)](1), which was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. This complex crystallizes in triclinic, space group P1 with a = 7.5595(6), b = 9.8199(8), c = 13.1663(11) , α = 69.7590(10), β = 80.6000(10), γ = 71.3180(10)o, Z = 2, C20H12N2O4Pb, Mr = 551.51, Dc = 2.112 g/cm3, F(000) = 520 and μ = 9.757 mm-1. The final R = 0.0304 and wR = 0.0763 for 3427 observed reflections with I 2σ(I) and R = 0.0365 and wR = 0.0894 for all data. The structure contains one crystallographic unique Pb(Ⅱ) atom, one phen molecule chelating with a Pb(Ⅱ) atom, and one bdc2- anion, acting as a bidentate bridging ligand linking the Pb(Ⅱ) atoms to form a one-dimensional structure. The two-dimensional layer and three-dimensional stacking structures are formed by C–H···O hydrogen bonding interactions. The thermal stable and fluorescent properties of 1 were investigated. PbO micro-crystal particles are produced by calcination of powder sample of complex 1. The obtained PbO is characterized and observed by XRD and SEM analyses.     

Synthesis, Crystal Structure and Thermal Stability of a Saturated Dimeric Ce(Ⅲ)-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline),was prepared by the reaction of Ce(NO3)3·6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P(1) with a =10.912(2), b = 11.962(3), c = 12.474(3)(A), a = 104.889(3), β = 93.523(3), γ = 113.332(3)°,C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2(6) (A)3, Z = 1, Dc = 1.598 g/cm3,μ = 1.652 mm-1, S =1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I ＞ 2σ(1). The structure of the title complex consists of two Ce(C6H5COO)3(C12H8N2) units,forming a binuclear molecule. Each Ce(Ⅲ) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.     

cis-Diaquabis（di-2-pyrimidinyl sulfide- K2N,N） Cobalt（II） Ditetrafluoridoborate： Lone Pair-aromatic and Anion-П Interactions in the Self-assembly of Coordination Complex

The title complex, [Co(DprS)2 (H2O)2]2(BF4)4 (DprS is di-2-pyrimidinyl sulfide), was obtained and characterized by elemental analysis, FT-IR and X-ray crystallography. The complex crystallizes in space group P21/c with a=11.742(1), b=22.439(2), c=20.538(2) , β=109.713(5)°, Z=4, V=5094.3(3)3 , Dc=1.692 g·cm-3 , μ=0.929 mm-1 , F(000)=2600, R=0.0756 and wR=0.1929. The asymmetric unit of the title complex is comprised of two isomeric cobalt(Ⅱ) centers (Co(1) and Co(2)) with a cis-[Co(DprS)2(H2O)2]2+ moiety. Each Co(Ⅱ) center exhibits a similar distorted N4O2-octahedral coordination geometry surrounded by a pair of DprS in a N,N’-chelate mode and two aqua ligands in a cis-relationship. Unconventional S···π(pyrimidinyl), N···π(pyrimidinyl), and anion(BF4-)···π(pyrimidinyl) are found to combine with the C H···F and O H···F interactions to stabilize a whole three-dimensional framework with the mononuclear units (Co(1) and Co(2)). The ligand conformation will be also discussed.     

Synthesis and Crystal Structure of the Copper(Ⅱ) Complex with Tris- (1,10-phenanthroline-5,6-dione)

The title complex [ CuL3 ] (C1O4)2 · 2H2O· 2CH3CN (L = 1, 10-phenanthroline-5, 6-dione) has been synthesized and characterized by elemental analysis, conductivity, infrared and UV-Vis spectra. X-ray diffraction analysis at room temperature indicates that the complex (C40H28Cl2 CuNsO16, Mr = 1011.14) crystallizes in orthorhombic system, space group P21 21 21 with a = 13. 983(1), b = 14. 310 (1), c =20.890(2) (A。), V = 4179.7(6) (A。)3, Z = 4, Dc= 1.607g/cm3, F(000) = 2026,μ(MoKa) = 0.736 mm-1. The final R and w,R factors are 0.0446 and 0. 1212 respectively with 8545 independent reflections. The title complex is composed of a discrete [CuL3 ]2+ cation, uncoordinated ClO4- anions, H2O and CH3CN molecules. The central Cu(Ⅱ) atom is six-coordinated by six nitrogen donors of three ligands. The coordination geometry of Cu(Ⅱ) could be considered as an approximately ideal octahedral configuration with little static Jahn-Teller distortion (the longest and shortest Cu- N bonds are 2. 102 vs 2. 139 (A。) with the mean length of 2. 122 (A。) ), which is very rare for a six-coordinated Cu(Ⅱ) complex.     

Hydrothermal Synthesis,Crystal Structure and Properties of a Lanthanum(Ⅲ) Complex Based on a N,O-Donor Ligand

A novel metal-organic complex [La(o-NCP)3]n(o-HNCP = 2-(2-carboxyphenyl)imidazo(4,5- f)(1,10)-phenanthroline) has been hydrothermally synthesized and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The complex crystallizes in triclinic, space group P1 with a = 9.898(2), b = 16.193(3), c = 16.909(3) , α = 67.68(3), β = 80.85(3), γ = 78.78(3)o, V = 2448.2(8) A3, Z = 2, Mr = 1156.9, Dc = 1.569 g/cm3, μ = 0.71073 A, F(000) = 1164, GOOF = 1.065, the final R = 0.051 and wR = 0.123 for 8539 observed reflections with I 2A(I). The complex exhibits a one-dimensional double chain structure. The adjacent chains are further connected by N–H...N hydrogen bonds which help to form a two-dimensional supramolecular architecture. Furthermore, the complex exhibits excellent thermal stability and luminescent property.     

Synthesis, Characterization and Properties of Tri-substitute Potassium Salt of Trinitrophloroglucinol

The title complex [K3（TNPG）·（H2O）2]n was synthesized by the reaction of the aqueous solutions of trinitrophlomglucinol （TNPG） with KHCO3. The complex was characterized by elemental analysis and FTIR spectroscopy, and its single crystal structure was determined by X-ray diffraction analysis. The structural analysis demonstrates that two different coordination modes of K cations [K（1） and K（2）] are around TNPG^3- anions in complex [Ka（TNPG）·（H2O）2]n, where the coordination numbers are eight. All K atoms coordinate with O atoms of phenolic hydroxyl group and nitro-group simultaneously. The thermolysis of the [Ka（TNPG） · （H2O）2]n has been investigated by using differential scanning calorimetry （DSC） and thermogravimetry-derivative thermogravimetry （TG-DTG） at a heating rate of 10 ℃/min. The thermal decomposition processes of the title complex were comprised of one endothermic dehydration stage and one exothermic decomposition stage in 270-320℃, and the final decomposition residue contained KNC. Impact and friction sensitivity results of the complex revealed its sensitive nature towards mechanical stimuli. The experiments verified that the complex has some characteristics of explosive.     

An Extended Cu(Ⅱ) Complex Structure Sustained by Hydrogen Bonding and C-H…π Interactions

The title complex [Cu(L1)(L2)(H2O)]·H2O(1,HL1 = N-(imino(pyridin-2-yl)me-thyl)picolinamidine),HL2 = salicylic acid) has been obtained by volatilization method with L1 prepared from 2,4,6-tripyridyl-1,3,5-triazine in situ.1 was fully characterized by single-crystal X-ray diffraction,elemental analysis and FT-IR.This complex exhibits a three-dimensional frame-work constructed through hydrogen bonding and C-H···π stacking interactions.The cyclic voltametric behavior of complex 1 was also investigated.1 belongs to the monoclinic system,space group P21/c with a = 15.112(5),b = 7.115(2),c = 19.899(6) ,β = 112.32°,V = 1979.4(11) 3,Mr = 460.94,Dc = 1.540 g/cm3,F(000) = 948,μ = 1.146 mm-1,Z = 4,the final R = 0.0612 and wR = 0.1813 for 2510 observed reflections with I 2σ(I).     

Synthesis and Characterization of a Two-dimensional Cadmium(Ⅱ) Metal Organic Framework with Fes Topology

A new Cd(Ⅱ) coordination polymer, {[Cd(Hnbta)(L)]·H2O}n(L = 1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane), H3nbta= 5-nitrobenzene-1,2,3-tricarboxylic acid), has been hydro-thermally synthesized and characterized by elemental analyses, IR, XRPD, and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 17.3056(13), b = 11.0114(9), c = 17.7484(14) A, β = 117.3640(10)o, V = 3003.7(4) A3, Z = 4, C31H31CdN5O9, Mr = 730.01, Dc = 1.614 g/cm3, μ = 0.792 mm-1 and F(000) = 1488. The cadmium(Ⅱ) ions are bridged by Hnbta2- to generate a two-dimensional metal organic framework with fes topology. In addition, the thermal stability and fluorescence properties of the complex were also studied.     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

Crystal Structure and Properties of a Copper(Ⅱ) Complex Containing p-Toluenesulfonate and Imidazole Ligands

A novel supramolecular mixed ligand complex of formula [Cu(PTS)2(Him)2(H2O)2] (C20H26CuN4O8S2,PTS=p-toluenesulfonate,Him=imidazole) has been synthesized in aqueous solution and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The compound crystallizes in the monoclinic system,space group P21/n,Z=2,a=5.650(2),b=14.671(3),c=14.638(3),β=100.10(3)°,V=1194.60(4)3,Dc=1.607 g/cm3,μ(MoKα)=1.143 mm-1,F(000)=598,R=0.0615 and wR=0.1503 for 1752 observed reflections with I 2σ(I).The copper(II) ion in the complex adopts a slightly distorted octahedral coordination geometry and is six-coordinated with N2O4 donor set consisting of two nitrogen atoms and four oxygen atoms provided by the ligands of two imidazole molecules,two water molecules and two p-toluenesulfonate ions.The sulfonate group of the PTS ligand remains weak-coordinated and forms a number of hydrogen bonds with water molecules and imidazole ligands.X-ray structural analysis reveals that the coordination molecules are connected to form a 3-D supramolecular framework by electrostatic interaction,weak van der Waals forces,hydrogen bonding and π-π interaction.The thermal behaviour of the title complex was investigated by using DSC and TG-DTG techniques.     

Synthesis and Crystal Structure of a Nitronyl Nitroxide Complex {[Zn(NIT4Py)(fum)(H2O)2]·H2}n

The title compound {[Zn(NIT4Py)(fum)(H2O)2]·H2O}n, where N1T4Py=2-(4'-pyridinyl)-4,4,5,5-tetra-methylimidazoline-l-oxyl-3-oxide and rum=fumarate, has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P1 with a =6.9533(9), b=9.805(1), c=15.248(2)A, a=94.608(2), β=92.328(2),γ=105.840(2)°,C16H24N3O9Zn, Mr=467.75, V=994.8(2) A3, Z=2, Dc=1.562 g/cm3,μ(MoKa)=1.289 mm-1,F(000)=486, the final R=0.0243 and wR=0.0622 for 3505 independent reflections with Rint=0.0125. The Zn(Ⅱ) adopts a distorted five-coordinate triangle bipyramidal geometry. The basic framework structure of the complex is a 1-D chain. The intrachain hydrogen bonds are helpful to stabilize the 1-D chain structure. Furthermore, the chains are connected by O-H…O hydrogen bonds to give a 2-D double-layer network.