Cu_2I_2(PPh_3)_3·DMF的合成和晶体结构

Ｃｕ２Ｉ２（ＰＰｈ３）３·ＤＭＦ（Ｐｈ＝Ｃ６Ｈ５,ＤＭＦ＝ＨＣＯＮ（ＣＨ３）２）是通过Ｗ２Ｓ４〔Ｓ２ＣＮ－（ＣＨ２ＣＨ２ＯＨ）２〕２,ＰＰｈ３和ＣｕＩ在ＣＨ２Ｃｌ２和ＤＭＦ为溶剂,在室温条件下合成的晶体产物。其空间群为Ｐ２１／ｃ,晶胞参数：Ｃ５７Ｈ５２Ｃｕ２Ｉ２ＮＯＰ３,ａ＝１５．８６３（５）,ｂ＝１９．６１９（７）,ｃ＝１８．２３２（４）,β＝１０９．５３（２）°,Ｖ＝５３４８（３）３,Ｚ＝４,Ｍｒ＝１２４０．８７,Ｄｃ＝１．５４ｇ／ｃｍ３,μ（Ｍｏ－Ｋα）＝２０．６６ｃｍ－１,Ｆ（０００）＝２４７２,对于Ｉ＞３σ（Ｉ）的５９５４个衍射点,最终的Ｒ＝０．０４６,Ｒｗ＝０．０６９。晶体结构由二核铜化合物和溶剂ＤＭＦ组成,两个Ｃｕ原子呈现不对称配位结构,ＤＭＦ在三配位Ｃｕ原子的近邻,它的氧原子和配位ＰＰｈ３的碳原子最近距离在３．３２（２）－３．４４（２）,ＤＭＦ参与晶体中对二核铜分子的结构和分子的堆积有明显的影响     

新颍Mo-Cu-Se簇合物｛MoCu_3Se_3I｝(PPh_3)_3O·0.5CH_2Cl_2的合成及晶体结构

新颍ＭｏＣｕＳｅ簇合物｛ＭｏＣｕ３Ｓｅ３Ｉ｝（ＰＰｈ３）３Ｏ·０．５ＣＨ２Ｃｌ２是由［Ｅｔ４Ｎ］２ＭｏＳｅ４、Ｃｕ（ＰＰｈ３）２ＮＯ３和ＫＩ在乙腈和二氯甲烷１∶１的混合溶剂中反应所得。晶体属单斜晶系，空间群Ｐ２１／ｃ；晶胞参数：ａ＝１１．９９４（２），ｂ＝２８．３５８（８），ｃ＝１９．５００（３）；β＝１０２．０４（１）°；Ｖ＝６４８６．７（４）３；Ｚ＝４；Ｄｃ＝１５８ｇ／ｃｍ３；Ｆ（０００）＝２９９２。晶体结构用直接法解出，经全矩阵最小二乘法修正，用４０５７个Ｉ＞３．０σ（Ｉ）的独立衍射点，最终偏离因子Ｒ＝０．０７３，ＲＷ＝０．０７９。标题化合物的核心｛ＭｏＣｕ３Ｓｅ３Ｉ｝是一个崎变的立方烷构型。ＭｏＣｕ和ＭｏＳｅ的平均间距分别是２７８２和２３８５；三个ＣｕＩ的间距为２８０３（４），２９０５（３），３０１５（４）。     

SOLID STATE SYNTHESIS AND CRYSTAL STRUCTURE OF THE CLUSTER COMPOUND［MwS_4Cu_3（PPh_3）_3Cl］（Mw＝0，56W＋0．44M0）

ＳＯＬＩＤ　ＳＴＡＴＥ　ＳＹＮＴＨＥＳＩＳ　ＡＮＤ　ＣＲＹＳＴＡＬ　ＳＴＲＵＣＴＵＲＥ　ＯＦ　ＴＨＥ　ＣＬＵＳＴＥＲ　ＣＯＭＰＯＵＮＤ［ＭｗＳ_４Ｃｕ_３（ＰＰｈ_３）_３Ｃｌ］（Ｍｗ＝０，５６Ｗ＋０．４４Ｍ０）ＳＯＬＩＤＳＴＡＴＥＳＹＮＴＨＥＳＩＳＡＮ...     

SYNTHESIS AND CRYSTAL STRUCTURE OF THE CLUSTER COMPOUND MoS_4Cu_2Ag（Ph_3P）_3Br．H_2O

ＳＹＮＴＨＥＳＩＳ ＡＮＤ ＣＲＹＳＴＡＬ ＳＴＲＵＣＴＵＲＥ ＯＦ ＴＨＥ ＣＬＵＳＴＥＲ ＣＯＭＰＯＵＮＤ ＭｏＳ_４Ｃｕ_２Ａｇ（Ｐｈ_３Ｐ）_３Ｂｒ．Ｈ_２Ｏ￥ＤｅＬｉａｎｇＬＯＮＧ；ＸｉｎＱｕａｎＸＩＮ（ＳｔａｌｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆ?..     

THE SYNTHESIS AND CRYSTAL STRUCTURE COMPLEX OF SCHIFF BASE CONTAINING S·N－Cd_3｜CH_3O（O）C_6H_3CH＝NNHC（S）NH_2｜4·（CH_3COO_2·1／2［CH_3S（O）CH_3］·2H_2O

ＴＨＥＳＹＮＴＨＥＳＩＳＡＮＤＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＣＯＭＰＬＥＸＯＦＳＣＨＩＦＦＢＡＳＥＣＯＮＴＡＩＮＩＮＧＳ·Ｎ－Ｃｄ_３｜ＣＨ_３Ｏ（Ｏ）Ｃ_６Ｈ_３ＣＨ＝ＮＮＨＣ（Ｓ）ＮＨ_２｜４·（ＣＨ_３ＣＯＯ_２·１／２［ＣＨ_３Ｓ（Ｏ）ＣＨ_３］·?..     

THE APPLICATION OF Cu（facam）2 TO THE ASYMMETRIC CYCLOPROPANATION OF 2，5－DIMETHYL－2，4－HEXADIENE

ＴＨＥ　ＡＰＰＬＩＣＡＴＩＯＮ　ＯＦ　Ｃｕ（ｆａｃａｍ）２　ＴＯ　ＴＨＥ　ＡＳＹＭＭＥＴＲＩＣ　ＣＹＣＬＯＰＲＯＰＡＮＡＴＩＯＮ　ＯＦ　２，５－ＤＩＭＥＴＨＹＬ－２，４－ＨＥＸＡＤＩＥＮＥＴＨＥＡＰＰＬＩＣＡＴＩＯＮＯＦＣｕ（ｆａｃａｍ）２ＴＯＴＨＥ...     

SYNTHESIS AND CHARACTERIZATION OF (PPh_3)_3Co(μ-CO)_2 V(CO)_2Cp AND (PPh_3)

ＳＹＮＴＨＥＳＩＳＡＮＤＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＯＦ（ＰＰｈ_３）_３Ｃｏ（μ－ＣＯ）_２Ｖ（ＣＯ）_２ＣｐＡＮＤ（ＰＰｈ_３）ＨＰｔ（μ－ＣＯ）（μ－ＰＰｈ_２）Ｖ（ＣＯ）_２ＣｐＣｈａｎｇＰｉｎｇＳＨＡＯ（ＤａｌｉａｎＩｎｓｔｉｔｕｔｅｏｆＣｈ?..     

标题固相合成V—Cu—S簇合物;VS4（CuPPh3）5X2（X=Br,I）的晶体结构

标题两个化合物是在反应体系（ＮＨ４）３ＶＳ４／ＣｕＸ／ＰＰｈ３／ＮＥｔ４Ｘ中采用低温固相反应方法得到的，单晶Ｘ射线结构分析表明：ＶＳ４（ＣｕＰＰｈ３）５Ｂｒ２（Ｉ）和ＶＳ４－（ＣｕＰＰｈ３）５Ｉ２是同构的，其中晶体属于单斜晶系，空间群Ｐ２１ｃ，Ｍｒ＝１９６８．２，ａ＝２０．２１５（７），ｂ＝１５．６９１（４），ｃ＝２７．３４５（９）Ａ，β＝９５．２９（３）°，Ｖ＝８６３７．０Ａ＾３，Ｚ＝４，Ｄｃ＝     

SYNTHESIS OF TETRAMETHYLDISILANDIYL DICYCLOPENTADIENYL LANTHANIDE COMPLEXES AND STRUCTURE OF 〔Me_4Si_2（C_5H_4）_2Sm（μ－Cl）（THF）〕_2

ＳＹＮＴＨＥＳＩＳＯＦＴＥＴＲＡＭＥＴＨＹＬＤＩＳＩＬＡＮＤＩＹＬＤＩＣＹＣＬＯＰＥＮＴＡＤＩＥＮＹＬＬＡＮＴＨＡＮＩＤＥＣＯＭＰＬＥＸＥＳＡＮＤＳＴＲＵＣＴＵＲＥＯＦ〔Ｍｅ_４Ｓｉ_２（Ｃ_５Ｈ_４）_２Ｓｍ（μ－Ｃｌ）（ＴＨＦ）〕_２￥ＦｕＱｕａｎＳＯ...     

SYNTHEIS， SITUCTURE AND CHARACTERIZATION OF BINUCLEAR Cu（II） COMPLEX ［Cu（C_6H_5COO）_2（C_5H_6N_2）］_2．（C_4H_8O）_2

ＳＹＮＴＨＥＩＳ，ＳＩＴＵＣＴＵＲＥＡＮＤＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＯＦＢＩＮＵＣＬＥＡＲＣｕ（ＩＩ）ＣＯＭＰＬＥＸ［Ｃｕ（Ｃ_６Ｈ_５ＣＯＯ）_２（Ｃ_５Ｈ_６Ｎ_２）］_２．（Ｃ_４Ｈ_８Ｏ）_２￥ＲｕｉＮａＹＡＮＧａｎｄＤｏｕＭａｎＪＩＮ（Ｈｅｎａ...     

C(6)H(5)NH(CH(3))(2)](2)Te(2)I(10): secondary I...I bonds build up a 3D network

The crystal structure of [C(6)H(5)NH(CH(3))(2)](2)Te(2)I(10) consists of the N,N-dimethylanilinium cation and a hitherto unreported tellurium iodide anion Te(2)I(10)(2)(-) [crystal data: C(8)H(12)NTeI(5), monoclinic, P2(1)/c, a = 9.4787(2) A, b = 14.2874(3) A, c = 13.6869(3) A, beta = 95.1918(8) degrees, V = 1845.96(7) A(3), Z = 4]. The Te(2)I(10)(2)(-) dianion is based on two edge-sharing TeI(6)(2)(-) octahedra, and interestingly, it builds up a three-dimensional Te(IV)-I open framework through extensive interconnecting I.I contacts. These I.I contacts (3.66-3.80 A) are significantly shorter than the corresponding sum of van der Waals radii (4.0 A) and may potentially promote charge carrier migration throughout the Te-I network. This material can also be drop-cast into thin films from a heated DMF solution.     

Formation and Crystal Structure of the Salt (IC(PPh3)2)2I[I3]·(I2)2 with a new Polyiodide Chain

The reaction of the carbodiphosphorane Ph₃P=C=PPh₃ ( 1 ) with MeI in the presence of iodine gives the oxidation product (IC(PPh₃)₂)₂I[I₃]·(I₂)₂ ( 2 ). In the solid state dimeric units linked by indefinite ···I^?···I₂···I₃^?···I₂···I^?··· chains are found. An additional I···I contact between the cation and the I₂ molecule is formed, amounting to 359.23(5) pm. 2 crystallizes in the monoclinic space group P2/c, with the unit cell dimensions a = 2053.9(1), b = 1011.4(1), c = 1889.8(1) pm; β = 105.21(1)° and Z = 4.     

Reaktion von Chlornitrat mit CF3I: Isolierung von Trifluormethylchloriodnitrat CF3I(Cl)ONO2 und Kristallstruktur von Trifluormethylioddinitrat CF3I(ONO2)2

Reaction of Chlorine Nitrate with CF₃I: Isolation of Trifluormethylchloroiodinenitrate CF₃I(Cl)ONO₂ and the Crystal Structure of Trifluormethyliodinedinitrate CF₃I(ONO₂)₂ CF₃I reacts with ClONO₂ to Iodine(III)-compounds. After an addition CF₃I(Cl)ONO₂ is isolated and characterized by vibrational spectra. With surplus ClONO₂ it is formed CF₃I(ONO₂)₂. CF₃I(ONO₂)₂ crystallizes monoclinic in the space group P2₁/c with the cell parameters a = 1 024.3(6) pm, b = 873.5(6) pm, c = 873.4(6) pm and Z = 4. We measered following bonding distances: I? O: 207.3(3) and 220.8(2) pm, I? C: 221.1(4) pm and N? O: from 119.1(4) to 141.5(3) pm. Through an intermolecular I ··· O-contact the central iodine becomes a distorted plane geometry.     

Untersuchungen an Polyhalogeniden III. Tetrammin-kupfer(II)-tetraiodid, [Cu(NH3)4I2 · I2], und Tetrammin-kupfer(II)-hexaiodid, [Cu(NH3)4I3]I3

Studies on Polyhalides. III. Crystal Structures of [Cu(NH₃)₄I₂ · I₂] and [Cu(NH₃)₄I₃]I₃ Tetramminecopper(II)tetraiodide [Cu(NH₃)₄I₂ · I₂] (I) crystallizes monoclinically in the space group C2/m with a = 1 185.9 pm, b = 892.8 pm, c = 656.8 pm, β = 111.10° and Z = 2 formula units. Tetramminecopper(II)hexaiodide [Cu(NH₃)₄I₃]I₃ (II) crystallizes orthorhombically in the space group Pnnm with a = 874.9 pm, b = 1 089.8 pm, c = 885.3 pm, and Z = 2 formula units. A special feature of these structures are coordinated polyiodide ions I₄^2? (I) or I₃^? (II). In both compounds four coplanar nitrogen atoms and two axial iodine atoms form a quasi-octahedral coordination around copper with the usual (4+2)-tetragonal distortion. The copper ions are connected by linear, centrosymmetric polyiodide ions I₄^2? (I) or I₃^? (II). Therefore infinite planar zigzag chains of units [Cu(NH₃)₄I₄] (I) or [Cu(NH₃)₄I₃]⁺(II) are resulting. The counterion I₃^? (II) is intercalated between these chains.     

Copper(I)alkyl bonding in the dinuclear copper(I) compound [(CH3)2P(CH2)2]2Cu2

The complex of empirical formula Cu^I[(CH₃)₂(CH₂)₂P] has been found to be dimeric with two digonal copper(I) atoms bridged by two ligand molecules through coppercarbon σ-bonds, resulting in a centrosymmetric eight-membered heterocycle.     

Zur Struktur der basischen Diquecksilber(I)-nitrate. I kristallstruktur des Hg2OH(NO3) · Hg2(NO3)2

The Crystal Structure of the Basic Dimercury (I) Nitrates. I. The Crystal Structure of Hg₂OH(NO₃) · Hg₂(NO₃)₂ The unit cell of Hg₂OH(NO₃) · Hg₂(NO₃)₂ is orthorhombic, space group Cc2a - standard setting Aba2 (C) — with a = 2017.1(5) pm, b = 935.8(3) pm, c = 1121.7(3) pm and contains 8 formula units. Characteristic are chains [Hg₂OH(Hg₂)_2/2]³⁺ parallel [001]. These are interconnected to a three-dimensional network by nitrate ions coordinated to mercury. The structure achieves additional stabilization through weak hydrogen bonds between oxygen atoms of the hydroxy groups and neighbouring nitrate ions. The bonding relationship of one hydrogen atom to four tetrahedrally correlated oxygen atoms is discussed.     

Crystal structure and heat capacity of the mixed-valence trinuclear iron monoiodoacetate complex, [Fe(III)2Fe(II)O(O2CCH2I)6(H2O)3][Fe(III)3O(O2CCH2I)6(H2O)3]I

The crystal structure of a trinuclear iron monoiodoacetate complex was determined. Although it has been incorrectly characterized as [Fe₃O(O₂CCH₂I)₆(H₂O)₃], the correct chemical formula turned out to be [Fe(III)₂Fe(II)O(O₂CCH₂I)₆(H₂O)₃]-[Fe(III)₃O(O₂CCH₂I)₆(H₂O)₃]I (1). The two kinds of Fe₃O molecules (Fe(III)₂Fe(II)O and Fe(III)₃O) are crystallographically indistinguishable. All the Fe atoms are crystallographically equivalent because of a crystallographic threefold symmetry. Heat capacities of 1 seem to exhibit no thermal anomaly in the temperature range 5.5–309 K, although the valence detrapping phenomenon has been observed in this temperature range. This fact indicates that the valence-detrapping phenomenon in 1 occurs without any phase transition, leading 1 to a glassy state, probably because the crystal of 1 is just like a solid solution of distorted mixed-valence Fe(III)₂Fe(II)O molecules and permanently undistorted Fe(III)₃O molecules which may act as an inhibitor for a cooperative valence-trapping.