CRYSTAL STRUCTURE OF (Br(μ-Met)(μ-Gly)(H_2O)_4]_2[Er(μ-Net)_2(H_2O)_4]_2(ClO_4)_(12)

<正> [Er(u-Met)(u-Gly)(H2O)4]2[Er(u-Met)2(HaO)4]2(ClO4)12(NMet=CH3S-(CH2)2CH(NH2)COOH,Gly=NH2CH2COOH), Mr=3194, trilinic, space group P1, a = 12.375(6),b= 14.041(13), c=19.074(13)A,α=80.85(6),β=80.72(6).γ=62.82(6)° ,Z=1,V= 2896A3,Dc=1.83 g/cm3,R=0.091. The carboxyl groups of Met and Gly in the title complex are bonded to Er atoms as bidentate bridging ligands.There are two different cations located at crystallographic symmetry centers in one unit cell.     

CRYSTAL STRUCTURE OF [Et_4N]_2[Mo_2O_2(μ-S)_2(S_2)_2]

<正> [(C2H5)4N]2[Mo2o2S2(S2)2], Mr = 676. 74, monoclinic, P21/c, a = 13.510(2), b = 14.373(2), c=14. 777(3)(?), β = 97.53(2)°, V = 2844.7(9) (?)3, Z = 4, Dc= 1. 58g/cm3, μ(MoKα) = 13.0cm-1, F(000) = 1384, R =0. 033 for 1803 observed reflections. The structure contains discrete [Mo2O2S2(S2)2]2- anions and Et4N+ cations. The two oxygen atoms bonded to the Mo atoms are in cis-form with respect to the Mo2S2 bridging unit, with an average Mo- O distance of 1. 678 (?), The Mo…Mo distance is 2. 832(1)(?).     

Synthesis and structure of [(μ4-succinato)hexadecaphenyltetraantimony] triiodide solvate with benzene [(Ph4Sb)2O2CCH2CH2CO2(Ph4Sb)2][I3]2 · 4PhH

Russian Journal of Coordination Chemistry - The reaction of bis(tetraphenylantimony) succinate with iodine in benzene affords [(μ4-succinato) hexadecaphenyltetraantimony] triiodide solvate...     

STRUCTURE OF {Mo4S4（μ—OAc）2[S2P（OC2H5）2]4H}

<正> {Mo4S4(μ-OAc)2(dtp)4H}3,(dtp=S2P(OEt)2),Mr=1371.60,Or-thorhombic, space group Pcab, a = 18. 90 (2) ,b = 21. 678 (4 ) , c = 24. 491 (4 ) A , V = 10031(7)A3,Z=8,Dc=1.818g/cm-3,F(000)=5464,λ(MoKa)=0.71073A,finalR= 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4]5+ from[3+1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a tetranuclear cubane-type core [Mo4S4]5+ with six Mo - Mo distances in the range 2. 685~2. 969A and is very similar to that of the previously characterized compound {Mo4S4(μ-OAc)2(dtp)4}2, [Mo4S4]6+, which was obtained directly by the reaction of MoCl3·3H2O with dtp. Some notable differences, however, can be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds , That can be attributed to the difference in the oxidation state of these two clusters .     

The insertion of acetylene into the formal ruthenium-phosphorus bonds of closo-[Ru4(μ4-PPh)2(μ2-CO)(CO)10. Crystal structure of [Ru4(μ4-PPh){μ4-η3-P(Ph)CHCH}(μ2-CO)(CO)10]

Treatment of closo-[Ru₄(μ₄-PPh)₂(μ₂-CO)(CO)₁₀] with acetylene under ambient conditions leads to the insertion of the acetylene into the skeletal framework of the cluster and the formation of [Ru₄(μ₄-PPh){μ₄-η³-P(Ph)CHCH}(μ₂-CO)(CO)₁₀], the structure of which has been determined X-ray crystallographically.     

[Cu3(μ10-bta)(μ2-C2O4)(H2O)2]n的水热合成与结构表征

有机-无机杂化材料因其在催化、化学吸附、磁性和电子导体等方面具有广泛的应用而成为人们的研究热点[1,2]. 通过过渡金属离子和特殊的有机配体之间的反应, 一系列具有独特结构的配位聚合物已被合成出来. 多齿有机配体可螯合两个或多个金属离子, 这些金属离子之间存在良好的电子交换[3], 可形成一维、二维或三维的配位聚合物. 均苯三甲酸和均苯四甲酸都是良好的桥连多齿配体, Chui等采用均苯三甲酸合成了具有吸附作用的大孔道的[Cu3(tma)2(H2O)]n[4] (tma=benzene-1,3,5-tricarb-oxylate)三维配位聚合物, 并且[Ni(C12H3ON6O2)]3(tma)*H2O[5], [M(tma)2]*12H2O(M=Co,Ni,Zn)[6], Na2[Co(H2O)6(bta)]*4H2O[7] (bta=benzene-1,2,4,5-tetracarboxylate)和[Co(phen)(md)][8] (phen=1,10-phenanthroline, md=benzene-1,3-dicarboxylate)等配位聚合物也先后被合成出来.     

CRYSTAL STRUCTURE OF ORGANOLANTHANIDE COMPLEX [Li~+(DME)_3]_2[(CpNd)_4(μ_2-CH_3)_2(μ_4-O)(μ_2-Cl)_6]~(2-)

<正> The crystal and molecular structure of [Li+(DME)3]2[(CpNd)4 (μ2-CH3)2(μ4-O) (μ2-Cl)6]2~was determined from single crystal X-ray diffraction. The complex crystallizes in the monoclinic space group P21/n with lattice parameters a= 14. 614(5), b= 18. 683 (5),c= 24. 595 (6) A, β = ,91-85(2)°, V = 6712(3) A3,2 = 4,DC = 1. 63g/cm3,F(000) = 3256,Mr=1650. 85. The structure was solved by direct methods and Fourier techniques and refined by least-squares to a final R=0. 047,RW = 0. 049 for 3761 with I>3σ(I). The result revealed that the anion [(CpNd)4(μ4-O) (μ2-Cl)6(μ2-CH3)2]2- is composed of four neodymium (Ⅲ) atoms bridged by six Cl atoms, two methyl groups and one oxygen atom, and every Nd is bonded to a cyclopentadienyl group. The four Nd atoms form a distorted tetrahedron. The cations are composed of two Li+(DME)3 with average Li-O distance of 2. 120(40) A.     

[Bu4N]2[Fe2(μ-S2O3)2(NO)4]: Synthesis,Structure, Redox Properties,and EPR Study

The [n-Bu₄N]₂[Fe₂(-S₂O₃)₂(NO)₄] complex was studied using X-ray diffraction analysis, cyclic voltammetry, and EPR spectroscopy, and its crystal structure was determined. The redox properties of the [Fe₂(-S₂O₃)₂(NO)₄]^2–anion in CH₃CN and CH₂Cl₂solutions were studied. An addition of excess reducer (sodium thiosulfate) to the thiosulfate complex was shown to produce an EPR signal with g= 2.03 typical of the mononuclear iron dinitrosyl complexes. The mechanism for [Fe₂(-S₂O₃)₂(NO)₄]^2–reduction was suggested.     

[（phen）2Mn2（μ—O）（μ—Ac）2（H2O2）]（ClO4）2·4H2O双核锰？…

MnAc3.2H2O在pH=4.0的HAc-NaAc缓冲溶液中和邻菲罗啉(phen)反应, 制得了双核锰(Ⅲ)合物[(phen)2Mn2(μ-O)(μ-Ac)2 (H2O)2](ClO4)2.H2O, 并进行了红外光谱表征. X射线单晶衍射表明, 该晶体属单斜晶系, 空间群P21/n, 晶胞参数: a=1.025 28(5) nm, b=1.792 75(9) nm, c=1.984 14(10) nm, β=94.843 0(10)°, V=3.634 0(3) nm3, Z=4, Dc=1.669 g.cm-3. 紫外可见光谱在480 nm处有一个吸收峰. 循环伏安实验说明, 此配合物在乙腈溶液中经历了一个半可逆的一电子氧化还原过程.     

Silver(I) ion induced formation of 2-D ternary lead(II)-silver(I)-4-tolythiolate [PbAg2(μ-Stol)2(μ4-Stol)2]n from 1-D binary lead(II)-4-tolythiolate [(μ-Cl)Pb2(Stol)(μ-Stol)2]n (tol = 4-tolyl)

Treatment of [Pb(Stol)₂]_n with an equiv of [Et₄N]Cl in DMF afforded a new 1-D polymeric complex, [(μ-Cl)Pb₂(Stol)(μ-Stol)₂]_n (1), with Pb–Cl–Pb links. Interaction of 1 with a suspension of [Ag(Stol)] in DMF resulted in formation of a 2-D polymeric complex, [PbAg₂(μ-Stol)₂(μ₄-Stol)₂]_n (2), with the planar four-membered Ag₂S₂ and PbAgS₂ rings bridged by μ-Stol and μ₄-Stol ligands. Both polymeric complexes were structurally characterized by single-crystal X-ray diffraction analysis.     

含低价钼的双核化合物(Et_4N)_2[(CO)_4Mo(μ-S)_2MOS_2]和(Et_4N)_2[(CO)_4Mo(μ-S)_2WS_2]的合成及晶体结构

用新方法合成并测定了含Mo(0)的双核化合物(Et_4N)_2[(CO)_4Mo(μ-S)_2MOS_2](Ⅰ)和(Et_4N)_2[(CO)_4Mo(μ-S)_2WS_2](Ⅱ)的晶体结构.Ⅰ和Ⅱ空间群均为Pbcm,Ⅰ的a=1.8403(2)nm,b=1.1963(1)nm,c=1.3482(1)nm,Z=4,R=0.042;Ⅱ的a=1.8453(2)nm,b=1.2004(2)nm,c=1.3494(3)nm,Z=4,R=0.032,Ⅰ和Ⅱ的阴离子均为以Mo(0)为中心的八面体和以Mo(Ⅵ)(或W)为中心的四面体共边且以μ-S连接,Mo(μ-S)2M(M=Mo,W)共平面.其中Mo—Mo键距为0.2992(2)nm,Mo—W为0.30330(8)nm,并发现其Fourier IR中Mo(0)-Sb键的v=424.3 cm~-1。     

New iron(II) spin crossover coordination polymers [Fe(μ-atrz)3]X2·2H2O (X = ClO4¯, BF4¯) and [Fe(μ-atrz)(μ-pyz)(NCS)2]·4H2O with an interesting solvent effect

A potential bridging triazole-based ligand, atrz (trans-4,4'-azo-1,2,4-triazole), is chosen to serve as building sticks and incorporated with a spin crossover metal center to form a metal organic framework. Coordination polymers of iron(II) with the formula [Fe(μ-atrz)(3)]X(2)·2H(2)O (where X = ClO(4)(-) (1·2H(2)O) and BF(4)(-) (2·2H(2)O)) in a 3D framework and [Fe(μ-atrz)(μ-pyz)(NCS)(2)]·4H(2)O (3·4H(2)O) in a 2D layer structure were synthesized and structurally characterized. The magnetic measurements of 1·2H(2)O and 2·2H(2)O reveal spin transitions near room temperature; that of 3 exhibits an abrupt spin transition at ~200 K with a wide thermal hysteresis, and the spin transition behavior of these polymers are apparently correlated with the water content of the sample. Crystal structures have been determined both at high spin and at low spin states for 1·2H(2)O, 2·2H(2)O, and 3·4H(2)O. Each iron(II) center in 1·2H(2)O and 2·2H(2)O is octahedrally coordinated with six μ-atrz ligands, which in turn links the other Fe center forming a strong three-dimensional (3D) network; counteranion and water molecules are located in the voids of the lattice. The FeN(6) octahedron of 3·4H(2)O is formed with two atrz, two pyrazine (pyz) ligands, and two NCS(-) ligands, where the ligands atrz and pyz are bridged between iron centers forming a 2D layer polymer. A zigzag chain of water molecules is found between the layers, and there is a distinct correlation between the thermal hysteresis with the amount of water molecules the exist in the crystal.     

Synthesis, Characterization and Crystal Structure of [Co2Mo2(μ4-C2HPh)(μ-CO)4(CO)4(η5-C5H4C(O)Me)2]

The reaction of μ-alkyne-bridged dimolybdenum compound [Mo2(μ-C2HPh)(CO)4(η5-C5H4C(O)Me)2] 1 with Co2(CO)8 in refluxing toluene gave a new butterfly compound [Co2Mo2(μ4-C2HPh)(μ-CO)4(CO)4(η5-C5H4C(O)Me)2] 2 which was fully characterized by elemental analysis, IR, 1H NMR and X-ray single crystal diffraction techniques. 2 crystallized in monoclinic system, C30H20Co2Mo2O10, Mr=850.23, space group P21/a(#14), a=14.165(5), b=12.498(2), c=16.204(2)(A), β = 96.50(2)°, V = 2850(1)(A)3, Z = 4, Dc = 1.981 g cm-3, F(000)=1672, μ(MoKα)=20.41 cm-1, final R=0.030, Rw=0.039 for 4831 observable reflections with I>2σ(I). The structure contains a Co2Mo2 butterfly core, and each Mo-Co bond is spanned by an asymmetric semi-bridging carbonyl ligand.     

Alkylation of [Pt2(μ-S)2(PPh3)4] with boronic acid derivatives

The reactivity of the metalloligand [Pt₂(μ-S)₂(PPh₃)₄] with the boron-functionalized alkylating agents BrCH₂(C₆H₄)B(OR)₂ (R = H or C(CH₃)₂) was investigated by electrospray ionization mass spectrometry (ESI-MS) in real time using pressurized sample infusion (PSI). The macroscopic reaction of [Pt₂(μ-S)₂(PPh₃)₄] with one mole equivalent of alkylating agents BrCH₂(C₆H₄)B{OC(CH₃)₂}₂ and BrCH₂(C₆H₄)B(OH)₂ gave the dinuclear monocationic μ-sulfide thiolate complexes [Pt₂(μ-S){μ-SCH₂(C₆H₄)B{OC(CH₃)₂}₂}(PPh₃)₄]⁺ and [Pt₂(μ-S){μ-S⁺CH₂(C₆H₄)B(OH)(O^?)}(PPh₃)₄]. The products were isolated as the [PF₆]^? salt and zwitterion, respectively, and fully characterized by ESI-MS, IR, ¹H and ³¹P NMR spectroscopy, and single-crystal X-ray structure determinations.     

Synthesis and Structure of a New Dimanganese Complex [Mn2（μ-OAc）2（phen）4]（ClO4）2

1INTRODUCTION Manganese complexes have drawn considerable interests in recent years because they can serve as models for active sites of manganese-containing me-talloenzymes,such as photosystem II(PSII),man-ganese superoxide dismutase(MnSOD),manganese ribonucleotide reductase(MnRR)et al[1].The binu-clear manganese enzymes,including catalase,MnRR and arginase,were indicated to have carboxylato-,oxo-,hydroxo-or aquo-bridged cores[2~4].Structures with Mn substituted into the iron ribon…     

The unusual stability of [NpO2Cl4]2−: Synthesis and characterisation of [NpO2(DPPMO2)2Cl]2[NpO2Cl4] and [Ph3PNH2]2[NpO2Cl4]

The [NpO₂(DPPMO₂)₂Cl][NpO₂Cl₄] complex (where DPPMO₂ = bis(diphenylphosphino)methanedioxide) contains the linear neptunyl group, {NpO₂}²⁺, with two bidentate P=O donor ligands. Coordinating anion Cl^? fills the fifth equatorial coordination site yielding a complex of general formula [NpO₂(DPPMO₂)₂X]₂[Y] (1) (where X = Cl^? and Y = [NpO₂Cl₄]^2?. Reaction between our newly prepared neptunium starting material [NpO₂Cl₂(thf)]_n and phosphinimine ligand produced crystals of [Ph₃PNH₂]₂[NpO₂Cl₄] (2). Compounds 1 and 2 have been structurally characterised.     

Synthesis and structure of tetra-p-tolylantimony complexes [(4-MeC6H4)4Sb] 2 + [Hg2I6]2−, [(4-MeC6H4)4Sb] 2 + [HgI4]2−, [(4-MeC6H4)4Sb] 3 + [Sb3I12]2−, and [(4-MeC6H4)4Sb]+[ReO4]−

Complexes [(4-MeC₆H₄)₄Sb] ₂ ⁺ [Hg₂I₆]^2? (I), [(4-MeC₆H₄)₄Sb] ₂ ⁺ [HgI₄]^2? (II), [(4-MeC₆H₄)₄Sb] ₃ ⁺ [Sb₃I₁₂]^2? (III), were synthesized by reactions of tetra-p-tolylantimony iodide with mercury iodide and antimony iodide, respectively. Tetra-p-tolylantimony perrhenate [(4-MeC₆H₄)₄Sb]⁺[ReO₄]^? (IV) was prepared from tetra-p-tolylantimony chloride and sodium perrhenate in acetone. Crystal structures of complexes I, II, and IV were determined by X-ray crystallography. Mercury and rhenium atoms have tetrahedral coordinations in these complexes. The Hg-I and Re-O distances in the structures of I, II, and IV vary within 2.7719(13)–2.7908(12)Å, 2.7028(3)–2.9163(3) Å, and 1.693(3)–1.744(3) Å, respectively. Antimony atoms in two crystallographically independent trinuclear centrosymmetric [Sb₃I₁₂]^2? anions of complex III have an octahedral environment. Each terminal SbI₃ fragment (Sb-I_t, 2.8265(9)–2.8333(10)Å) is bound to the central atom through tree bridging iodine atoms (Sb(2)-I_br, 3.2275(9)–3.3620(10)Å). The distances between the central Sb atom and bridging iodine atoms are much shorter (Sb(1)-I_br, 3.0153(6)–3.0316(6) Å; Sb(3)-I_br, 2.9926(6)–3.0074(6) Å).