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Syntheses, Crystal Structures and Magnetic Properties of a New nitronyl nitroxide radical and Its Cu(Ⅱ) Complex

Chinese Journal of Structural Chemistry 2007年第7期26卷 860-866页

作者：蒋凯赵保利王利亚王玉芳 College of Chemistry and Environmental Science Henan Normal University Department of Chemistry Luoyang Normal University

A new compound （NIT-mNO2 = 4,4,5,5-tetramethylimidazoline-2-yl-（2＇-chlor-5＇- nitrophenyl）-3-oxide-l-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 P211n with a = 10.6798（9）, b = 11.2705（9）, c = 12.9559（10）A, β = 107.3770（10）°, V = 1488.3（2） A^3, C13H15ClN3O4, Mr = 312.73, Z = 4, Dc = 1.396 g/cm^3, g（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 55.75°. The compound results in a 1-D zig-zag chain structure by intermolecular H-bond interaction. Compound 2 crystallizes in triclinic, space group Pi with a = 10.3699（10）, b = 10.6286（11）, c = 15.1683（15）A, a = 77.5330（10）, ,β = 773080（10）, y = 87.3420（10）＊, V = 1592.5（3） A^3, C23HITCIFI2N3O8Cu, Mr = 790.39, Z = 2, Dc = 1.648 g/cm^3, 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.

关键词： crystal structure magnetic properties nitronyl nitroxide radical Cu(Ⅱ) complex

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One-dimensional lanthanide complexes bridged by nitronyl nitroxide radical ligands with non-chelating nitrogen donors: Structure and magnetic characterization

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Science China Chemistry 2012年第6期55卷 997-1003页

作者： LIU RuiNa HU Peng LI LiCun LIAO DaiZheng SUTTER Jean-Pascal Key Laboratory of Advanced Energy Materials Chemistry Department of Chemistry Nankai University Tianjin 300071 China Tianjin Key Laboratory of Metal and Molecule-based Material Chemistry Nankai University Tianjin 300071 China Universite de Toulouse UPS INPT LCC F-31077 Toulouse France

A series of new lanthanide-radical complexes [{Ln（hfac）3}2（NITPhlM）2] （Ln = Nd （1）, Eu （2）, Tb （3）, Er （4）; hfac = hexafluoroacetylacetonate; NITPhlM = 2-[4-（1-imidazole）phenyl]-4,4,5,5-tetramethylimidazoline-l-oxyl-3-oxide） have been prepared and characterized. Single crystal X-ray diffraction analyses reveal that these complexes are isostructural with one-dimensional chain structures. These consist in Ln（hfac）3 units bridged by the paramagnetic ligands by the means of coor- dination of their nitronyl nitroxide groups and imidazole rings. Interestingly, each Ln ion is either bound to two nitronyl ni- troxide groups or to two imidazole units, and the different Ln centers alternate along the chain. Magnetic studies show that complex 3 exhibits a single-chain magnet behavior.

关键词： nitronyl nitroxide radical lanthanide crystal structure single-chain magnets

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Crystal Structure and Magnetic Characteristics of Novel Neutral Lanthanide(Ⅲ)- nitronyl nitroxide radical Complexes

Crystal Structure and Magnetic Characteristics of Novel Neut...

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第二届海峡两岸功能材料科技与产业峰会（2015）

作者： Yi-Fang Hou Shu-Tao Yang Shu-Ping Wang College of Chemistry & Material Science Hebei Normal University

Three novel rare-earth complexes based on a new nitronyl nitroxide radical have been synthesized and characterized by single-crystal X-ray diffraction,with formula{[Ln(hfac)(NITPh Br F)2]·CHCl}(Ln=Gd(1),Tb(2),Dy(3);hfac=hexafiuoroacetylacetonate;NITPhB rF=2-(5-bromo-2-fluorophenyl)-tetramethylimidazoline-1-oxyl-3-oxide).These compounds are isostructural,which crystallize in the monoclinic

关键词： nitronyl nitroxide radical lanthanide complex crystal structure magnetic property

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Two new hetero-binuclear compounds based on the nitronyl nitroxide radical

Two new hetero-binuclear compounds based on the nitronyl nit...

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中国化学会第30届学术年会-第十六分会：晶体工程

作者： Meng Yang Jian-ni Guo Li-cun Li Department of Chemistry Nankai University

Synthesis of 3d-4f heterometallic compounds has become an outstanding area of molecular magnetic materials because they are excellent candidates for SMMs[1-3].Although lots of Cu-Ln compounds have been synthesized,to our best knowledge,Cu-Ln polynuclear compounds based on nitronyl nitroxide radical are rare[4].Here we synthesized two new 3d-4f binuclear complexes of[Ln(hfac)Cu(hfac)(NIT-5Br-3Py)](Ln = Tb(1),Gd(2);hfac = hexafluoroacetylacetonate,NIT-5Br-3Py = 2-(4,4,5,5-tetramethyl-imidazoline-3-oxyl-1-oxide)-5-bromo-3-pyridine).The structure of complex 1 is shown in Figure *** Tb atom is eight-coordinated by six O atoms from three bidentate hfac ligands,one O atom from the nitroxide radicals and the last one from the coordinated *** Cu is five coordinated with four O atoms from two hfac ligands and one N atom from pyridine ring of the nitroxide radicals forming a distorted tetragonal pyramid *** Tb and Cu atoms are bridged by NO group and N atom of one nitronyl nitroxide radical forming a binuclear *** complex 2,[Gd(hfac)Cu(hfac)NIT-5Br-3Py]is isomorphic to complex 1 except for the substitution of Gd with the Tb *** studies show that there exist ferromagnetic exchange couplings between the coordinated NO groups of radical ligands and Ln *** relaxation of the magnetization was observed in compound 1in a zero field(Fig.2).

关键词： hetero-binuclear nitronyl nitroxide radical magnetization

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Two new tetranuclear lanthanide complexes based on the nitronyl nitroxide radical

Two new tetranuclear lanthanide complexes based on the nitro...

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中国化学会第十届全国无机化学学术会议

作者： Jiao Lu Jianni Guo Licun Li Department of Chemistry Nankai University

As spin carriers,nitronyl nitroxide radicals are appealing building blocks to construct molecular magnetic materials owing to the advantages of their effective exchange interaction and *** lanthanide ions can provide large magnetic moments and significant magnetic anisotropy,making them ideal candidates for the construction of molecular *** we have successfully obtained two new isomorphic tetranuclear lanthanide–nitronyl nitroxide radical complexes[(Ln(hfac))(NIT-PhPyO)]by employing the pyridinone-substituted nitronyl nitroxide radical NIT-PhPyO (Ln=Dy(1),Ho(2);hfac=hexafluoroacetylacetonate;NIT-PhPyO=2-[4-(4-pyridinone)phenyl]-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide).Single crystal X-ray crystallographic analysis reveals that in complexes 1 and 2,two NIT-PhPyO radical bridges three Ln ions inμ-η:η mode and other two radial ligands are coordinated to Ln ions as terminal *** magnetic studies show that there exist antiferromagnetic exchange couplings between the coordinated NO groups of radical ligands and Ln *** 1 exhibit frequency dependent magnetic susceptibilities,indicating slow magnetic relaxation phenomenon.

关键词： molecular magnetism nitronyl nitroxide radical lanthanide tetranuclear complexes

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Two new hetero-tri-spin chain compounds based on the nitronyl nitroxide radical

Two new hetero-tri-spin chain compounds based on the nitrony...

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中国化学会第八届全国配位化学会议

作者： Jing Xie Cun Li Guifang Sun Meng Yang Li-cun Li Department of Chemistry Nankai University

When compared with pure transition metal or lanthanide complexes,3 d-4 f heterometallic compounds combine the advantages of favorable magnetic coupling between the metal centres and the high magnetic anisotropy carried by 4 f ions,thus providing more possibilities to improve the blocking *** addition,molecular magnetic systems introducing nitronyl nitroxide radicals could enhance magnetic coupling owing to their two NO *** we report two new nitronyl nitroxide bridged 3 d-4 f magnetic chain compounds of[Ln(hfac) Zn(hfac)(NIT-Pyrim)](Ln=Gd(1),Dy(2);hfac=hexafluoroacetylacetonate,NIT-Pyrim =(2-pyrimidine-4,4,5,5-tetramethyl-imidazoline-1-oxyl-3-oxide).Single crystal X-ray crystallographic analysis reveals that complexes 1 and 2 consist of 1 D chains built up by Ln(hfac) and Zn(hfac) units bridged by the radical ligands through their NO moieties and the nitrogen *** structure of complex 1 is shown in Figure *** Gd atom is eight-coordinated by six O atoms from three bidentate hfac ligands,two O atoms from the nitroxide *** Zn is six coordinated with four O atoms from two hfac ligands and two N atoms from pyrimidine ring of the nitroxide *** studies show that there exist ferromagnetic exchange couplings between the coordinated NO groups of radical ligands and Ln ions.

关键词： hetero-tri-spin nitronyl nitroxide radical magnetization

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Two new one-dimensional compounds based on pyridinone-substituted nitronyl nitroxide radical

Two new one-dimensional compounds based on pyridinone-substi...

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中国化学会第十届全国无机化学学术会议

作者： Lu Xi Li-cun Li Department of Chemistry College of Chemistry Nankai University

The lanthanide-based complexes have attracted much attention in the field of molecular magnetism for they are excellent candidates of SMMs[1-2].The nitronyl nitroxide radical,an excellent organic ligand,has been corroborated to be a quite effective choice to construct Ln-radical compounds[3-4].Along this line,we synthesized two new4f-based complexes,namely[{Ln(hfac)}(NITPy-PyO)] (Ln=Gd (1),Tb (2);hfac=hexafluoroacetylacetonate;NITPy-PyO=2-[4-(4-pyridinone)pyridyl]-4,4,5,*** presented in Figure 1,complexes 1 and 2 have an isomorphic geometry,containing three crystallographically independent Ln(hfac) units and two NITPy-PyO *** the Gd ions adopt an O coordination mode with six O atoms from three bidentate hfac *** Gd1 and Gd2 ions are bridged by a couple of O atoms from two radicals to yield a GdO unit,while the coordination sphere of Gd3 is completed by the O atoms from two NO groups of two radicals,resulting in a one dimensional chain *** studies indicate that weak antiferromagnetic interaction is observed between Gd1 and Gd2 ions while there is ferromagnetic coupling between the coordinated NO groups and Gd3 ion(Figure 2).Further dynamic magnetic studies indicate that complex 2 exhibits slow magnetic relaxation behavior at low temperature.

关键词： one-dimensional chain nitronyl nitroxide radical magnetization

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Synthesis,Crystal Structure and Magnetic Property of a New Cd(Ⅱ) Complex with Four nitronyl nitroxide radicals

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Chinese Journal of Structural Chemistry 2011年第6期30卷 853-857页

作者：崔志华魏海霞高东昭孙亚秋张国英许艳艳 Tianjin Key Laboratory of Structure and Performance for Functional Molecule College of ChemistryTianjin Normal University

A new Cd（Ⅱ） complex with four nitronyl nitroxide radicals [Cd（NIT4Py）4Cl2]（NIT4Py = 2-（4＇-pyridinyl）-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide） has been synthesized and structurally characterized by X-ray diffraction *** crystallizes in triclinic,space group P1 with a = 7.2441（4）,b = 13.6964（8）,c = 13.7354（8） ,α = 89.8610（10）,β = 77.9180（10）,γ = 87.2250（10）°,V = 1331.01（13） 3,C48H64CdCl2N12O8,Mr = 1120.41,Z = 1,Dc = 1.398 g/cm3,μ（MoKα） = 0.573 mm-1,F（000） = 582,S = 1.043,the final R = 0.0257 and wR = 0.0641 for 4333 observed reflections（I 〉2σ（I））.The title complex exists in the mononuclear-metal structures,in which each Cd（Ⅱ） ion adopts a distorted octahedral geometry and is coordinated by two Cl-anions and four pyridyl-N atoms from four NIT4Py *** magnetic measurements show weak antiferromagnetic interactions between the nitroxide radicals.

关键词： Cd(Ⅱ) complex nitronyl nitroxide radical crystal structure antiferromagnetic interaction

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A New One-dimensional Dicyanamide Bridged Zinc(II) Complex Containing nitronyl nitroxide radicals:Synthesis,Crystal Structure and Magnetic Properties

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Chinese Journal of Structural Chemistry 2009年第6期28卷 713-717页

作者：王利亚程江涛蒋凯王玉芳 College of Chemistry and Chemical Engineering Luoyang Normal University College of Chemistry and Environmental Science Henan Normal University

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′-methyl）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 P^-1, with a = 7.428（3）, b = 9.839（3）, c = 16.708（6） A^°, α = 93.270（4）, β = 101.642（4）,γ= 100.632（4）°, C17.5H21N8O5.5Zn, Mr = 496.79, V = 1169.7（7） A^°^3, Dc = 1.411 g/cm^3, 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 zine（ID 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∑ijJijSiS within the complex.

关键词： crystal structure nitronyl nitroxide radical Zn(Ⅱ) complex dicyanamide anion antiferromagnetic interactions

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Synthesis,Crystal Structure and Magnetic Properties of an Oxalato-bridged Dinickel(Ⅱ) Complex with nitronyl nitroxide radicals

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Chinese Journal of Structural Chemistry 2010年第1期29卷 51-56页

作者：王玉芳鞠丰阳王利亚 Department of Chemistry College of Chemistry and Chemical EngineeringLuoyang Normal university

A new oxalato-bridged dinickel（Ⅱ） complex [Ni2（NIT-MeImz）4（C2O4）]（Ac）2·8H2O has been synthesized and characterized structurally as well as *** crystallizes in monoclinic,space group C2/c with a=24.608（4）,b=21.399（3）,c=17.992（3）,β=131.680（2）°,V=7076（2）3,C50H86N16Ni2O24,Mr=1412.77,Z=4,Dc=1.326 g/cm3,μ（MoKα）=0.614 mm-1,F（000）=2984,R=0.0751 and wR=0.1791 for 2956 observed reflections with Ⅰ＆gt;2σ（Ⅰ）.X-ray analysis reveals that the crystal structure consists of [Ni2（NIT-MeImz）4（C2O4）]2＋ moiety and two Ac^- anions. Each nickel（H） ion is six-coordinated with a distorted octahedral geometry： two nitrogen atoms and two oxygen atoms from NIT-Melmz together with two other oxygen atoms from the oxalato ion. The 2-D net structure is formed and arranged through intermolecular H-bonding interactions. Magnetic measurements show antiferromagnetic interactions for this complex.

关键词： nickel(Ⅱ) complex nitronyl nitroxide radical antiferromagnetic interactions

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