Synthesis and Crystal Structure of Cluster 〔C_6H_4-1,2-(CO_2CH_2C_2H-μ)_2〕〔Co_2(CO)_6〕_2

１ＩＮＴＲＯＤＵＣＴＩＯＮＯｃｔａｃａｒｂｏｎｙｌｄｉｃｏｂａｌｔｉｓａｖｅｒｙｃｏｎｖｅｎｉｅｎｔｓｔａｒｔｉｎｇｍａｔｅｒｉａｌｆｏｒｔｈｅｐｒｅｐａｒａｔｉｏｎｏｆａｌｍｏｓｔａｎｙｃｏｂａｌｔｃｏｍｐｏｕｎｄ〔１〕．Ｔｈｅｒｅａｃｔｉｏｎｓｏ...     

Synthesis and Characterization of Tetrametal Cluster〔Co_2(CO)_6〕〔μ-HC_2CH_2OCH_2C_2H-μ〕〔Co_2(CO)_6〕

１ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｔｅｎｓｅｉｎｔｅｒｅｓｔｉｎｔｒａｎｓｉｔｉｏｎ ｍｅｔａｌｃｌｕｓｔｅｒｓｃｏｎｔｉｎｕｅｓｂｅｃａｕｓｅｔｈｅｙｒｅｐｒｅｓｅｎｔｐｏｓ ｓｉｂｌｅｃｏｎｃｅｐｔｕａｌｂｒｉｄｇｅｓｂｅｔｗｅｅｎｈｏｍｏｇｅｎｅｏ...     

Synthesis and Crystal Structure of 〔EDA〕〔Ni(dmit)_2〕_3

１ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅＮｉ（ｄｍｉｔ）２ｍｏｌｅｃｕｌｅｓｇｉｖｅｒｉｓｅｔｏａｎｕｍｂｅｒｏｆｍｏｌｅｃｕｌａｒｃｏｎｄｕｃｔｏｒｓ〔１，２〕ｉｎａｄｄｉｔｉｏｎｔｏｓｕｐｅｒｃｏｎｄｕｃｔｏｒｓ〔３，４〕．Ｔｈｅｍｕｌｔｙｓｕｌｆｕｒｆ...     

Crystal Structure of 〔PrAl(CF_3COO)_2(CF_3CHOO)(C_2H_5)_2(C_4H_8O)_2〕_2

１ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｒｅｃｅｎｔｙｅａｒｓ,ａｓｅｒｉｅｓｏｆｌａｎｔｈａｎｉｄｅ ａｌｕｍｉｎｉｕｍｃｏｍｐｌｅｘｅｓｗｈｉｃｈａｒｅａｃｔｉｖｅｆｏｒｐｏｌｙ ｍｅｒｉｚａｔｉｏｎｏｆｏｌｆｉｎｓ〔１〕ｈａｖｅｂｅｅｎｒｅｐｏｒｔｅｄ．...     

The Molybdenum(0) Complex 〔Et_4N〕_2〔Mo_2(CO)_6(pys)_2〕(pys=Pyridine-2-thiolato)

１ＩＮＴＲＯＤＵＣＴＩＯＮＲｅｃｅｎｔｒｅｓｅａｒｃｈｏｎａｓｅｒｉｅｓｏｆｄｉｎｕｃｌｅａｒｍｏｌｙｂｄｅｎｕｍ（０）ｃａｒｂｏｎｙｌｃｏｍｐｌｅｘｅｓｃｏｎｔａｉｎ ｉｎｇｔｈｉｏｌａｔｏ ｂｒｉｄｇｅｓｈａｓｌｅｄｔｏｔｈｅｃｏｎｃｌｕｓｉｏｎ...     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound 〔Et_4N〕_2〔Mo_2(CO)_8(SC_6H_4-OCH_3-p)_2〕

１　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｏｕｒｅｆｆｏｒｔｓｔｏｄｅｖｅｌｏｐｔｈｅｌｏｗ－ｖａｌｅｎｃｅＭｏ－ＳＲｃｏｍｐｏｕｎｄｓ,ｗｅｈａｖｅｆｏｕｎｄａｎＭｏ（０）－ｃｏｍｐｏｕｎｄ,〔Ｍｏ２（ＳＲ）２（ＣＯ）８〕２－,ｗｈｉｃｈｉｓｏｂｔａｉｎｅｄｆｒｏｍｔｈｅｒｅａｃｔｉｏｎｏｆＭｏ（ＣＯ）６ｗｉｔｈＲＳ－ｉｎｈｉｇｈｙｉｅｌｄ,ｐｏｓｓｅｓｓｅｓａｎｉｎｔｅｒｅｓｔｉｎｇｔｗｏ－ｅｌｅｃｔｒｏｎｔｒａｎｓｆｅｒｐｒｏｐｅｒｔｙ．Ｎｕｍｅｒｏｕｓｋｉｎｄｓｏｆｄｉｎｕｃｌｅａｒｍｏｌｙｂｄｅ…     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound〔Et_4N〕_2〔Mo_2(CO)_8(SC_6H_4-NH_2-p)_2〕

１ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｅｘｉｓｔｅｎｃｅａｎｄｓｉｇｎｉｆｉｃａｎｃｅｏｆｔｈｅｍｏｌｙｂｄｅｎｕｍ ｓｕｌｆｕｒｂｏｎｄｉｎｇｉｎｍｏｌｙｂｄｅｎｕｍｅｎｚｙｍｅｓ〔１〕ｈａｖｅｓｔｉｍｕｌａｔｅｄｔｈｅｓｔｕｄｉｅｓｏｎｔｈｅｃｈｅｍｉ...     

Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato Bridges 〔Et_4N〕_2〔Mo_2(CO)_8(SC_6H_4-Cl-p)_2〕

１　ＩＮＴＲＯＤＵＣＴＩＯＮＳｔｕｄｉｅｓｏｎＭｏ－Ｓ（ＳＲ）ｃｏｍｐｏｕｎｄｓｈａｖｅａｌｗａｙｓｂｅｅｎａｎａｃｔｉｖｅｒｅｓｅａｒｃｈａｒｅａｂｅ－ｃａｕｓｅｏｆｔｈｅｅｘｉｓｔｅｎｃｅａｎｄｉｍｐｏｒｔａｎｃｅｏｆＭｏ－Ｓ（ＳＲ）ｂｏｎｄｉｎｇｉｎｍｏｌｙｂｄｅｎｕｍｅｎ－ｚｙｍｅｓ〔１〕ｉｎｂｉｏｌｏｇｉｃａｌｓｙｓｔｅｍａｎｄｔｈｅｐｏｔｅｎｔｉａｌａｐｐｌｉｃａｔｉｏｎｔｏｍａｔｅｒｉａｌｓａｎｄｃａｔａｌｙｓｔ〔２〕．Ｉｎｒｅｃｅｎｔｙｅａｒｓ,ｗｅａｒｅｉｎｔｅｒｅｓｔｅｄｉｎ…     

Syntheses of Clusters Containing C_2M_2(M=Co,Mo)Cores and Crystal Structure of 〔dpp〕 〔Mo_2Cp_2(CO)_4〕·CH_2Cl_2

１ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｅｘｔｅｎｓｉｖｅａｎｄｒａｐｉｄｄｅｖｅｌｏｐｍｅｎｔｏｆｔｈｅｃｈｅｍｉｓｔｒｙｏｆｄｉｎｕｃｌｅａｒｔｒａｎｓｉｔｉｏｎｍｅｔａｌｃｏｍｐｌｅｘｅｓｂｒｉｄｇｅｄｂｙｕｎｓａｔｕｒａｔｅｄｈｙｄｒｏｃａｒｂｏｎｓ...     

Synthesis and Structural Investigation of ｛CpEu〔CH(COOC_2H_5)_2〕〔μ-CH(COOC_2H_5)_2〕｝_2

１ＩＮＴＲＯＤＵＣＴＩＯＮＯｒｇａｎｏｌａｎｔｈａｎｉｄｅｃｏｍｐｌｅｘｅｓｉｎｖｏｌｖｉｎｇｂｏｔｈｃｙｃｌｏｐｅｎｔａｄｉｅｎｙｌａｎｄβ ｄｉｋｅｔｏｎａｔｏｃｈｅｌａｔｅｌｉｇａｎｄｓｈａｖｅｂｅｅｎｓｙｎｔｈｅｓｉｚｅｄ〔１ ４〕,ａｎｄｏ...     

A convenient route to synthesize the fully conjugated bimetallic complex (Bu4N)2[tto[Ni(dmit)2]] (tto = tetrathiooxalate,C2S4(2-), and dmit = 1,3-dithiole-2-thione-4,5-dithiolate,C3S5(2-) and the crystal structure of a new crystal form

A novel route for the conversion of (Bu4N)2[Ni(dmit)2] to (Bu4N)2[tto[Ni(dmit)2]] is reported here. This provides a much more efficient way of synthesizing (Bu4N)2[tto[Ni(dmit)2]] than the literature method. During the process, the conversion of dmit2- to tto2- was realized for the first time. This new synthesis should facilitate further research on the conducting bimetallic complexes [C]x[tto[Ni(dmit)2]]. In addition, a new crystal form of (Bu4N)2[tto[Ni(dmit)2]]. In addition, a new crystal form of (Bu4N)2[tto[Ni(dmit)2]] was determined by X-ray crystallographic analysis.     

[Et_4N]_2[Zn_2(OPh)_2Cl_4]的合成和晶体结构

ZnCl2, PhONa和Et4NCl稨2O在乙腈溶剂中反应合成了一种二核锌配合物[Et4N]2[Zn2(OPh)2Cl4]。X射线衍射结果表明,晶体属单斜晶系,C2/m空间群,晶胞参数 a = 14.1366(2), b=13.6985(5), c=9.3308(3)牛?107.851(2)o, V=1719.92(9)?,C28H50O2N2Zn2Cl4,Mr=721.24,Z=2,Dx=1.393g/cm3,μ(MoKα)=1.732mm—1,F(000)=756, R=0.0552, wR=0.1534, S=1.027。 配合物是由2个阳离子Et4N+和1个阴离子[Zn2(OPh)2Cl4]2—组成。阴离子[Zn2(OPh)2Cl4]2—包含着1个中心Zn2O2菱形平面。配合物中的2个锌原子通过2个苯酚中的氧原子桥连,每个锌原子还与2个氯原子配位形成变形四面体结构。     

[Hg(C5H4S5)I2]2的合成与晶体结构(C5H4S5 = 4,5-亚乙基二硫杂-1,3-二硫杂-2-硫酮)

用 HgI2 和 4,5-亚乙基二硫杂-1,3-二硫杂-2-硫酮 (C5H4S5)反应,合成一种二核汞配合物[Hg(C5H4S5)I2]2 1。X 射线衍射结果表明,晶体属于单斜晶系,C2/c 空间群,晶胞参数 a =21.6847(1),b = 8.5125(4),c = 15.6699(8),a=112.7850(1)°,V=2666.8(2) ?3。Mr = 1357.54,Z = 4,Dx = 3.381 g/cm3,ì = 16.913 cm–1,F(000) = 2400,R=0.0639,wR=0.1711,S=1.052。配合物 1 具有二聚体结构,2 个汞原子通过 2 个碘原子桥联,形成 1 个 Hg2I2菱形平面,汞原子周围的配位是四面体结构,通过分子间的硫…硫作用和碘…硫作用,形成准二维超分子网络。 S S S H g I I S S S S I I H g S     

STRUCTURE STUDIES OF [Et_4N]_4[Cu_8(i-mnt)_6] (i-mnt=S_2C=C(CN)_2) AND [Me_4N]_4[Cu_5Ag_3(i-mnt)_6]·H_2O

<正> [Me4N]6[Ag6(i-mnt)6].H2O(1),[Et4N]4[Cu8(i-mnt)6](2) and [Me4N]4-[Cu5Ag3(i-mnt)6].H2O(3)(i-mnt=S2C=C(CN)2) were synthesized. The crystal and molecular structure of the complex 1 was reported by us.The structure of the complex 2 was determined from single crystal X-ray diffraction data. [Et4N]4[Cu8(i-mnt)s] 2, Mr=1870.46, monoclinic, P21/n, a=14.724(6), b = 17.228(3), c=15.59(1)A,β= 100.75(7)°,V=3886.3A3;Z = 2,Dc= 1.598 g/cm3. Complex 3 has been characterized by ICP elemental analyses and IR spectrum.     

配合物{[Cu(hmtade)][Ni(dmit)2]}2·4DMSO的合成、表征及晶体结构

合成了配合物{[Cu(hmtade)][Ni(dmit)2]}2·4DMSO(1)(hmtade为5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂环十四-4,11-二烯; dmit为1,3-二硫杂环戊二烯-2-硫酮-4,5-二硫醇; DMSO为二甲亚砜), 采用元素分析、红外光谱和紫外-可见光谱进行了表征, 并用X射线衍射法测定了晶体结构. 该晶体属于单斜晶系, P21/n空间群; 晶胞参数: a=1.49952(6) nm, b=1.77229(7) nm, c=3.1275(1) nm, β=102.442(1)°, V=8.1163(5) nm3, Dc=1.558 Mg/m3, Z=8, F(000)=3944, μ(Mo Kα)=1.637 mm-1, S=1.016, (Δ/σ)max=0.001, R1=0.0673, wR2 =0.1672[I>2σ(I)]. 晶体结构研究表明, 配合物{[Cu(hmtade)]·[Ni(dmit)2]}2·4DMSO包含2个[Cu(hmtade)][Ni(dmit)2]子单元. 每个子单元中, 1个dmit中的1个S原子与Cu及Ni配位, 形成异双核Cu—Ni配合物. 其中Cu(Ⅱ)为五配位的四方锥构形, Cu—N键长在0.1949(5)~0.2007(4) nm范围内, Cu—S键长分别为0.28913(18)和0.28952(18) nm; 配阴离子[Ni(dmit)2]2-为畸变四方形, Ni—S键长在0.21729(16)~0.21905(17) nm范围内. 溶剂分子DMSO与配体hmtade形成了N—H…O氢键. 通过分子内S…S和S…H短接触形成了二聚体, 二聚体之间通过S…S短接触形成一维链状结构, 并通过S…S, S…H和C…H短接触进一步形成二维和三维结构.     

Synthesis and characterisation of cyanodithioimidocarbonate [C2N2S2]2- complexes

[PPh4]2[M(C2N2S2)2](M = Pt, Pd) and [Pt(C2N2S2)(PR3)2](PR3= PMe2Ph, PPh3) and [Pt(C2N2S2)(PP)](PP = dppe, dppm, dppf) were all obtained by the reaction of the appropriate metal halide containing complex with potassium cyanodithioimidocarbonate. The dimeric cyanodithioimidocarbonate complexes [[Pt(C2N2S2)(PR3)]2](PR3 = PMe2Ph), [M[(C2N2S2)(eta5-C5Me5)]2](M = Rh, Ir)and [[Ru(C2N2S2)(eta6-p-MeC6H4iPr)]2] have been synthesised from the appropriate transition metal dimer starting material. The cyanodithioimidocarbonate ligand is S,S and bidentate in the monomeric complexes with the terminal CN group being approximately coplanar with the CS2 group and trigonal at nitrogen thus reducing the planar symmetry of the ligand. In the dimeric compound one of the sulfur atoms bridges two metal atoms with the core exhibiting a cubane-like geometry.     

Synthesis and Crystal Structure of [2-dapp]2[Zn（dmit）2] （2-dapp = 2-（4-Dimethylaminophenyl）ethyl-l-methylpyridinium, dmit = 1,3-Dithiole-2-thione-4,5-dithiolato）

1 INTRODUCTION The transition metal complexes with dmit ligand together with their derivatives have received signi- ficant attention due to their metallic-like electronic properties[1～8]. More recently, our researches show that they may be the new kind…     

(Bu_4N)[Ni(dmit)_2]的一步合成及一种新晶相

用中心离子替代和空气自动氧化的方法由(Bu_4N)_2[Zn(dmit)_2]一步合成了 (Bu_4N)[Ni(dmit)_2]，这种方法可推广到其它Z[M(dmit)_2]配合物和Z[M(dmit) _2]_2导电配合物的合成(Bu_4N)[Ni(dmit)_2]结晶过程中出现两个晶相，其中空间 群为C2/c的侧心单斜相为新晶相，X射线结构测定结果为：a=2.0191(2)nm, b=1. 3404(1) nm,β=105.55(1)~°,V=3165.5(6)nm~3, R=0.055,　晶体中的Ni(dmit) _2]－呈D_(2h)点群对称性，平面性接近完美，共轭性相当显著，相邻Ni(dmit)_2] －平面间的夹角为75.56（3）~°。     

Die Kristallstrukturen von trans‐[NiBr2(Pyridin)4] und [Ni(HNPEt3)4]I2

Crystal Structures of trans ‐[NiBr₂(pyridine)₄] and [Ni(HNPEt₃)₄]I₂ Turquoise single crystals of trans‐[NiBr₂(pyridine)₄] have been obtained by the reaction of excess pyridine with nickel(II) bromide/diacetonealcohol. According to the crystal structure determination the nickel atom is octahedrally coordinated by the two bromine atoms in trans‐position and by the nitrogen atoms of the pyridine molecules. Space group Pna2₁, Z = 4, lattice dimensions at 20 °C: a = 1592.9(2), b = 943.8(1), c = 1413.0(2) pm, R₁ = 0.0492. Dark blue single crystals of the phosphoraneimine complex [Ni(HNPEt₃)₄]I₂ have been obtained from NiI₂/H₂O with excess Me₃SiNPEt₃ and subsequent recrystallization from acetonitrile. According to the crystal structure determination the nickel atom is tetrahedrally coordinated by the nitrogen atoms of the HNPEt₃ molecules. The iodide ions are connected via N–H…I contacts with the cation to form an ion triple. Space group P2₁/c, Z = 4, lattice dimensions at –80 °C: a = 1934.9(2), b = 1078.3(1), c = 1966.3(2) pm, β = 111.040(8)°; R₁ = 0.043.     

[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征

通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺.