通讯作者地址: Tao, J (通讯作者), Xiamen Univ, Coll Chem & Chem Engn, State Key Lab Phys Chem Solid Surfaces, Xiamen 361005, Peoples R China  
地址: 
1. Xiamen Univ, Coll Chem & Chem Engn, State Key Lab Phys Chem Solid Surfaces, Xiamen 361005, Peoples R China 
2. Xiamen Univ, Coll Chem & Chem Engn, Dept Chem, Xiamen 361005, Peoples R China  
电子邮件地址: taojun@xmu.edu.cnA novel cobalt compound [Co9(HL)4(L)4Cl2]·(EtOH)2(H2O)2 (H3L = (E)-2-2((1,3-dihydroxy-
2-methylpropan-2-ylimino)methyl) phenol) has been solvothermally synthesized and structurally
characterized. The compound crystallised in the space group C2/c with a = 32.624(2)A˚ ,
b = 9.4814(4)A˚,c=33.395(2)A˚,b=109.339(5)◦ and V = 9746.8(9)A˚ 3. The crystal structure is a
mixed-valence nonanuclear Co(II/III) oligomer, which contains a square-pyramidal CoII
5 core formed
through m4-Cl and m3-alkoxo bridges and the pentanuclear CoII
5 core is surrounded by four peripheral
Co(III) ions at the square-pyramidal base plane through m2-alkoxo bridges. Magnetic properties of the
compound can be considered as the magnetism of the CoII
5 core, and the superexchange interactions
between Co(II) ions within the core were calculated with three Co(II)–Co(II) superexchange
parameters by using MAGPACK software package to give J1 = + 11.1 cm-1,
J2 = -6.50 cm-1, J3 = -3.25 cm-1, D = + 6.0 cm-1 and g = 2.30.NNSF  20671079 
20721001  
MOE  107068  
MSTC  NCET-08 -0470 
2007CB81530

Jun Tao

Lan-Sun Zheng

Li-Li Hu

Rong-Bin Huang

Xiao-Jun Sun

Zhong-Quan Jia

孙小军

胡利俐

贾忠全

郑兰荪

陶军

黄荣彬

Dalton Transactions

Xiamen University Institutional Repository

PAPER www.rsc.org/dalton | Dalton TransactionsStructure and magnetic property of a mixed-valence nonanuclear cobaltcompound with a square-pyramidal CoII5 core†Zhong-Quan Jia, Xiao-Jun Sun, Li-Li Hu, Jun Tao,* Rong-Bin Huang and Lan-Sun ZhengReceived 23rd February 2009, Accepted 20th May 2009First published as an Advance Article on the web 24th June 2009DOI: 10.1039/b903733kA novel cobalt compound [Co9(HL)4(L)4Cl2]·(EtOH)2(H2O)2 (H3L = (E)-2-2((1,3-dihydroxy-2-methylpropan-2-ylimino)methyl) phenol) has been solvothermally synthesized and structurallycharacterized. The compound crystallised in the space group C2/c with a = 32.624(2) Å,b = 9.4814(4) Å, c = 33.395(2) Å, b = 109.339(5)◦ and V = 9746.8(9) Å3. The crystal structure is amixed-valence nonanuclear Co(II/III) oligomer, which contains a square-pyramidal CoII5 core formedthrough m4-Cl and m3-alkoxo bridges and the pentanuclear CoII5 core is surrounded by four peripheralCo(III) ions at the square-pyramidal base plane through m2-alkoxo bridges. Magnetic properties of thecompound can be considered as the magnetism of the CoII5 core, and the superexchange interactionsbetween Co(II) ions within the core were calculated with three Co(II)–Co(II) superexchangeparameters by using MAGPACK software package to give J1 = + 11.1 cm-1,J2 = -6.50 cm-1, J3 = -3.25 cm-1, D = + 6.0 cm-1 and g = 2.30.IntroductionHigh-nuclearity paramagnetic clusters (PMCs) attract a greatdeal of interest, due to their fascinating physical properties andthe architectural beauty of their structures.1 In the process ofsynthesis of PMCs, partial oxidation of divalent transition metalions (Mn(II), Fe(II) and Co(II)) usually produced mixed-valencePMCs, as exemplified by the first example of single-moleculemagnet Mn12.2 Since then, a great number of mixed-valencemanganese clusters have been synthesized and their magneticproperties have been widely studied, and a new field in magnetism,the so-called SMMs, has thus been springing up.3 In comparisonwith manganese and iron ions, cobalt ion is also easily and partiallyoxidized and leads to mixed-valence PMCs, whose magneticproperties are more complex due to the effect of the strong orbitalcontribution of Co(II) center to the magnetic moment and thusto a strong magnetic anisotropy. Especially at low temperature,this effect splits the ground state and thus makes the magneticproperties of cobalt clusters much more interesting.4Recently, some interesting mixed-valence Co(II,III) clus-ters, for examples, {CoII2CoIII6},5a {CoII3CoIII3},5b {CoII3CoIII4},5c{CoII4CoIII3},5d {CoII4CoIII4}5e and {CoII6CoIII6},5f have beenreported. For the synthesis of mixed-valence cobalt PMCs,the potentially polynucleating ligands possessing polyalco-hol/alkoxide groups are very suitable.6,5d For example, we recentlyadopted a Schiff-base ligand 2-((2-hydroxybenzylidene)-amino)-2-hydroxymethylpropane-1,3-diol, which contains a {NO} chelat-ing moiety and a tripodal alcohol unit that successfully gaverise to a mixed-valence pentanuclear CoII3CoIII2 compound.7In this compound, the tripodal alcohol unit is partially de-State Key Laboratory of Physical Chemistry of Solid Surfaces & Departmentof Chemistry, College of Chemistry and Chemical Engineering, XiamenUniversity, Xiamen, 361005, People’s Republic of China. E-mail: taojun@xmu.edu.cn† CCDC reference number 720927. For crystallographic data in CIF orother electronic format see DOI: 10.1039/b903733kprotonated, which gives us an impetus to investigate a simi-lar ligand with less alcohol groups. Aiming at extending oursearch of new mixed-valence PMCs that contain polyalco-hol/alkoxide ligands, we report here a new mixed-valence nonanu-clear cluster of formula [CoII5CoIII4(HL)4(L)4Cl2]·(EtOH)2(H2O)2(1·(EtOH)2(H2O)2) with a new ligand (E)-2-2((1,3-dihydroxy-2-methylpropan-2-ylimino)methyl) phenol (H3L, Scheme 1). To ourknowledge, though two nonanuclear Co(II) clusters have beenreported,8 compound 1 is the first example of a nonanuclear mixed-valence Co(II,III) cluster.Scheme 1 H3L and the coordination modes in 1.ExperimentalAll reagents and solvents were commercially available and wereused without further purification. The ligand H3L was synthesizedby condensation of salicylaldehyde and 2-amino-2-methyl-1,3-propanediol (1:1) in hot methanol solution.A single crystal of [CoII5CoIII4(HL)4(L)4Cl2]·(EtOH)2(H2O)2(dark pink block, 0.50 mm ¥ 0.40 mm ¥ 0.32 mm) was mountedon an Oxford Gemini S Ultra diffractometer equipped with aCCD camera and an enhanced graphic monochromated MoKa radiation source (l = 0.71073 Å). Data were collected at223 K. Data reduction was performed with CrysAlis RED and thespace group was assigned by analysis of symmetry and systematicabsences determined by XPREP. The structure of the compound6364 | Dalton Trans., 2009, 6364–6367 This journal is © The Royal Society of Chemistry 2009Downloaded by Xiamen University on 12 January 2011Published on 24 June 2009 on http://pubs.rsc.org | doi:10.1039/B903733KView Onlinewas solved by direct methods using SHELXS-97 and refinedagainst all data in the 2q range by full-matrix least-squares onF 2 using SHELXL-97 software.9 All non-hydrogen atoms wererefined anisotropically. Hydrogen atoms were constrained in theiridealized positions and not refined, the hydrogen atoms on watermolecules were not localized. There is only half a molecule thatconstitutes an asymmetric unit and it contains two water andtwo ethanol molecules per Co9 cluster. The structure containsaccessible voids as calculated by PLATON, it may be due tothe existence of unidentified solvate which could not be modeledsatisfactorily. PLATON/SQUEEZE routines were not used torefine the data.Crystallographic data for 1·(EtOH)2(H2O)2: C92H116N8O28-Cl2Co9, M = 2383.20, monoclinic, space group C2/c (no. 8), a =32.624(2) Å, b = 9.4814(4) Å, c = 33.395(2) Å, b = 109.339(5)◦,V = 9746.8(9) Å3, Z = 4, T = 223 K, 20 988 reflections measured,9324 unique reflections (Rint = 0.0411), refinement with 628parameters converged with agreement factors R1 (I > 2s) =0.0672, wR2 (all data) = 0.1289, GOF = 1.200, 2q ≤ 52◦.Magnetic measurements were perfomed using a QuantumDesign MPMS-XL SQUID magnetometer operating in the tem-perature range 2–300 K with a dc magnetic field up to 7 T.Synthesis of 1·(EtOH)2(H2O)2A mixture of NaOEt (0.068 g, 1 mmol) and H3L (0.042 g,0.2 mmol) was dissolved in absolute ethanol solution (10 mL),followed by addition of Co(OAc)2·4H2O (0.025 g, 0.1 mmol) andSmCl3·6H2O (0.036 g, 0.1 mmol). The resulting solution wasstirred for 30 min and sealed in a 23 mL Teflon-lined stainlesssteel autoclave, heated at 140 ◦C for 1 day. The reaction systemwas then cooled to room temperature at a rate of 4 ◦C h-1 and darkpink crystals were collected by filtration. Yield was about 30%.Elemental percentage for C92H116N8O28Cl2Co9: C 46.37, H 4.91,N 4.70. Found: C 45.92, H 4.93, N 5.21. IR data (cm-1): 3430 (s),1640 (s), 1598 (s), 1540 (w), 1440 (m), 1378 (w), 1342 (m),3111 (m), 1149 (w), 1102 (m), 1050 (w), 935 (w), 758 (m), 606 (m),491 (w).Results and discussionCrystal structureCompound 1·(EtOH)2(H2O)2 crystallized in the monoclinic spacegroup C2/c and the structure of 1 is shown in Fig. 1. Theasymmetric unit comprises five independent cobalt ions with twochloride ions, two independent HL2- and two independent L3-ligands (Scheme 1). Symmetry operation of the space group (C2/c)affords a neutral and centrosymmetric nonanuclear cluster withformula of [Co9(HL)4(L)4Cl2]. Following from the charge balanceof the neutral cluster, there should be four CoIII and five CoII ions.From a structural point of view, the average Co–O bond lengths ofCo1, Co2 and Co4 are 2.108, 2.064 and 2.057 Å, respectively, whichare longer than those of Co3 and Co5 (which average 1.901 and1.896 Å, respectively), thus Co1, Co2 and Co4 can be attributedto the +2 valence state and Co3 and Co5 to the +3 one. Onthe other hand, the values of Co–O and Co–N bond lengths ofCo3 and Co5 are similar to those of typical CoIII–O and CoIII–Nbonds,5d,6,7 confirming the +3 valence state for them. Therefore,Fig. 1 ORTEP drawing at 50% probability of 1 with atom labels. Selectedbond distances (Å) and angles (◦): Co1–O6 2.118(4), Co1–O12 2.098(4),Co1–Cl1 2.292(2), Co2–O2 2.065(4), Co2–O3 2.049(4), Co2–O5 2.018(4),Co2–O6 2.089(4), Co2–O12A 2.099(4), Co2–Cl2 2.667(1), Co3–O11.877(4), Co3–O2 1.922(4), Co3–O4 1.884(4), Co3–O5 1.920(4), Co3–N11.902(5), Co3–N2 1.908(5), Co4–O8 2.059(4), Co4–O9 2.045(4), Co4–O6A2.078(4), Co4–O11A 2.024(4), Co4–O12A 2.091(4), Co4–Cl2 2.708(1),Co5–O7 1.867(4), Co5–O8 1.923(4), Co5–O10A 1.882(4), Co5–O11A1.914(4), Co5–N3 1.897(5), Co5–N4 1.896(5)Co1–O6–Co2 90.00(14),Co1–O12A–Co2 90.28(14), Co1–O6–Co4A 90.88(14), Co1–O12–Co4A91.08(14), Co2–O6–Co4A 110.34(16), Co2–O12A–Co4 110.88(16). Sym-metry code: (A) -x + 1, y, -z + 1/2.the nonanuclear can be viewed as an inner pentanuclear CoII5 coresurrounded by four outer CoIII atoms.The five inner CoII ions form a square-pyramidal structuralfeature, in which Co1 locates at the apical postion with a five-coordinate stereochemistry [CoO4Cl]. The geometry about Co1ion may be square-pyramidal or trigonal-bipyramidal, dependingon the t value (t = (b - a)/60, where b is defined as the largerof the basal angles and a is the remaining angle).10 t is 0 for thecoordination of square-pyramidal and 1 for trigonal-pyramidal.The t value for Co1 is 0.46%, which strongly indicates square-pyramidal geometry. Each cobalt ion (Co2 and Co4) in the basalplane of the square-pyramidal CoII5 cluster possesses an [O5Cl]ligand donor set, giving an distorted octahedral coordinationgeometry, here the chloride ion (Cl2) serves as a m4-bridge thatis connected to four CoII ions (Co2, Co2A, Co4 and Co4A) andlocates above the basal plane for ca 1.15 Å. To our knowledge,this is the first example of a m4-Cl bridge in a CoII compound.The m4-Cl–Co bond lengths (2.667 and 2.708 Å for Co2 and Co4,respectively) are longer than those for mono-coordinate Cl–Co11,m2-Cl–Co12 and m3-Cl–Co bonds.13In the square-pyramidal CoII5 cluster, the apical cobalt ion (Co1)is bridged to the basal ones (Co2, Co2A, Co4 and Co4A) throughfour m3-alkoxo groups from the L3- ligands. The Co1 ◊ ◊ ◊ Co2 andCo1 ◊ ◊ ◊ Co4 distances are 2.975 and 2.990 Å, respectively, whichare much shorter than those of Co2 ◊ ◊ ◊ Co4 and Co2 ◊ ◊ ◊ Co4A(3.451 and 3.420, respectively). The values of Coapical–O–CobasalThis journal is © The Royal Society of Chemistry 2009 Dalton Trans., 2009, 6364–6367 | 6365Downloaded by Xiamen University on 12 January 2011Published on 24 June 2009 on http://pubs.rsc.org | doi:10.1039/B903733KView Onlinebond angles cover the range 90.00–91.08◦ and those of Cobasal–O–Cobasal 110.34–110.88◦. The ligand H3L (Scheme 1, left) is boundto CoII/CoIII ions in two ways: partially deprotonated HL2- inh1,h1,h1,h2-m2 coordination mode (Scheme 1, middle) and fullydeprotonated L3- in h1,h1,h2,h3-m4 coordination mode (Scheme 1,right). Each HL2- ligand is coordinated to one outer CoIII ion andan inner CoII one, for example, the HL2- ligand associated withN1 atom is chelated to the Co3 ion by the phenolate oxygen (O1)and imide nitrogen (N1) atoms, its deprotonated alcohol hydroxylO2 atom is m2-bridged to Co2 and Co3 ions and another one(O3) is coordinated to Co2 ion, and adjacent HL2- ligands formstrong inter-ligand hydrogen bonds (O3–H ◊ ◊ ◊ O8 2.527 andO9–H ◊ ◊ ◊ O2A 2.536 Å, respectively). Each L3- ligand is coordi-nated to one outer CoIII ion and three inner CoII ones, for example,the L3- ligand associated with N2 atom is chelated to the Co3 ionwith its phenolate oxygen (O4) and imide nitrogen (N2) atoms,its alcohol hydroxyl O5 atom is m2-bridged to Co2 and Co3 ions,while its alcohol hydroxyl O6 atom is m3-bridged to Co1, Co2 andCo4A ions.Magnetic propertiesThe dc magnetic susceptibility of 1·(EtOH)2(H2O)2 was measuredin the temperature range of 2–300 K and shown in Fig. 2. Sincethe CoIII ions are low-spin (t2g6, S = 0), the magnetic propertiesare thus attributed to the square-pyramidal CoII5 cluster. At roomtemperature, the cMT value of 13.53 cm3 K mol-1 differs from thespin-only value for five isolated CoII ions (5 ¥ 1.875 cm3 K mol-1),indicating an orbital contribution to the g-value. The four CoIIions in the basal plane in the octahedral environments representhigh-spin centers and exhibit significant spin–orbital coupling,however, the CoII ion in the apical position (Co1) with square-pyramidal coordination may be high-spin or low-spin. Regardinga CoII ion with five-coordination, an increase of the out-of-planedisplacement of the CoII ion from 0 to 0.45–0.74 Å will stablizethe high-spin (S = 3/2) state,14 thus the out-of-plane displacementof the Co1 ion of 0.58 Å indicates a high-spin configuration. Inthe same way, the d-block orbitals of an ML5 compound with asquare-pyramidal geometry where the angle between the apicaland the basal bonds varies from 90 to about 110◦ could lead toa rapid decrease in the quartet-state energy,15a especially whenFig. 2 Temperature-dependent susceptibility of 1·(EtOH)2(H2O)2 underan applied field of 1000 Oe, inset: Magnetization at 2 K.q > 102◦ (q = Lapical–Co–Lbasal).15b The q values for Co1 are 105.94(Cl1–Co1–O6) and 106.09◦ (Cl1–Co1–O12), respectively, whichalso indicate a high-spin state of Co1 ion.On lowering the temperature, cMT slowly decreases until 100 Kand then it falls drastically reaching a value of 6.09 cm3 K mol-1 at2 K. This value is far below the expected one for five magneticallyisolated CoII ions (cMT = 5 ¥ 1.73 cm3 K mol-1), indicating theoccurrence of antiferromagnetic interactions.6 Meanwhile, owingto spin–orbital coupling, the S = 3/2 state is split into twoKramer’s doublets, so the depopulation of the higher energyKramer’s doublets also causes the decrease of cMT. In order toevaluate the magnetic coupling in 1, we apply the Hamiltonianof eqn (1), where J1 represents the coupling parameter of apical–basal interactions, J2 the nearest-neighbor basal–basal ones andJ3 the next-nearest-neighbor basal–basal ones (Scheme 2).H = - 2J1(S1S2 + S1S3 + S1S4 + S1S5) - 2J2(S2S3 + S3S4 +S4S5 + S5S2) - 2J3(S2S4 +S3S5) + mBgHRSiz +DR [(Siz)2–5/4] (1)Scheme 2The experimental data were fitted by using MAGPACK soft-ware package16 to give J1 = +11.1 cm-1, J2 = -6.5 cm-1, J3 =-3.25 cm-1, D = +6.0 cm-1 and g = 2.3. The fitting resultsrevealed ferromagnetic interaction between the apical CoII ionand the basal ones, which is in agreement with the values ofthe Coapical–O–Cobasal bond angles (90.00–91.08◦) that give riseto orthogonal magnetic orbitals.17 While the antiferromagneticinteractions between the basal nearest-neighbor CoII ions and thenext-nearest-neighbor ones may be ascribed to the large Cobasal–O–Cobasal (110.34–110.88◦) and Co–Cl–Co (129.26 and 129.52◦)bond angles, respectively. However, the field dependence of themagnetization at 2 K (Fig. 2, inset) cannot be easily reconciledwith the susceptibility in Fig. 2. The magnetization of 6.42Nb at7 T could be reproduced for g ~ 4.2–4.8 and a total spin S = 3/2,which may imply an intermediate ground state. This is consistentwith the presence of competing interactions and spin-frustrationeffects because of ferromagnetic (J1) and antiferromagnetic(J2 and J3) for Coapical–Cobasal and Cobasal–Cobasal, respectively. Onthe other hand, the magnetic anisotropy on the cobalt centers mayalso play an important role.ConclusionsA new mixed-valence nonanuclear cobalt(II,III) compound con-taining a square-pyramidal arranged {CoII5} inner core and fourperipheral Co(III) ions has been synthesized by using a Schiff-base ligand. Magnetic studies reveal the existence of competingferro- and antiferromagnetic interactions and consequently anintermediate ground state.6366 | Dalton Trans., 2009, 6364–6367 This journal is © The Royal Society of Chemistry 2009Downloaded by Xiamen University on 12 January 2011Published on 24 June 2009 on http://pubs.rsc.org | doi:10.1039/B903733KView OnlineAcknowledgementsThis work was financially supported by the NNSF of China(Grant 20671079, 20721001), the Key Project of MOE (Grant107068), NCET-08–0470 and the 973 project of MSTC (Grant2007CB815301).Notes and references1 (a) Y.-L. Bai, V. Tangoulis, R.-B. Huang, L.-S. Zheng and J. Tao, Chem.-Eur. J., 2009, 15, 2377; (b) X.-J. 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Chem.Soc., Dalton Trans., 1992, 47.This journal is © The Royal Society of Chemistry 2009 Dalton Trans., 2009, 6364–6367 | 6367Downloaded by Xiamen University on 12 January 2011Published on 24 June 2009 on http://pubs.rsc.org | doi:10.1039/B903733KView Online

Structure and magnetic property of a mixed-valence nonanuclear cobalt compound with a square-pyramidal Co-5(II) core

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Structure and magnetic property of a mixed-valence nonanuclear cobalt compound with a square-pyramidal Co-5(II) core

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