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Chinese Journal of Chemistry 1986年第3期4卷 209-216页

作者： KANG Bei-Sheng CAI Jing-Hua CHENG Chang-Neng lu jia-xi fujian institute of research on the structure of matter, academia sinica, fuzhou fujian institute of research on the structure of matter Academia Sinica Fuzhou

Through the reactions of ferrous thiolates with tetrathiomolybdate, we discussed thereaction pathways and possible intermediates during the formation of double-cubane type Mo-Fe-Scluster compounds. We also reported the synthesis, crystal structure, IR and magnetic susceptibi-lity measurements of the title compound 2. The crystal of 2 belongs to triclinic system, Mr=2670.3;P1; a=12.755（4）A, b=13.076（3）A, c=20.576（4） A; α=80.00 （2）°, β=81.39（2）°, γ=61.51（2）°;V=2966.3（14）A3; Z=1; Dc=1.495 g/cm2. Final R factor is 0.077 for 4031 observed *** compound was obtained through the reaction of （Et4N）2[Fe4（SPh）10] （1） with （Et4N）2MoS4inacetonitrile solution. The structure of anion 2 is two cubane clusters bridged by a Fe（SPh）*** Mo…Mo′ distance of 7.188A is the longest among all double-cubane cluster compounds ofknown structures.

关键词： Fe Syntheses and structural studies of molybdenum-iron-sulfur compounds SPh Et4N The synthesis and crystal structure of Mo2Fe7S8

research on in part "loosely" coordinated trinuclear molybdenum cluster compounds—— the synthesis and crystal structure of {Mo3（μ3-S）(μ-S)3[S2P（OEt）2]4·P（C6H5）3} （0.86CH2Cl2）

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Chinese Journal of Chemistry 1986年第4期4卷 301-310页

作者： HUANG jian-Quan lu Shao-Fang LIN Yu-Hui HUANG Jin-Ling lu jia-xi fujian institute of research on the structure of matter, academia sinica, fuzhou fujian institute of research on the structure of matter Academia Sinica Fuzhou

The synthesis and crystal structure of novel trinuclear molybdenum cluster compoundwith somewha "loose" coordination site {Mo3（μ3-S）(μ-S)3[S2P（OEt）2]4· P（C6H5）3}'·（0.86 CH2Cl2）have been reported. The cluster crystallizes in the spece group Pl with two molecules in a unit cellwhose parameters are a=10.472（4）, b=14.375（2）, c=21.695（3）; a=74.O4（1）°, β=76.50（2）°, γ=72.22（2）°, v=2950 and D_o=1.693 ***-x. On the basis of 4840 independent reflections with I≥2σ（1）.the structure was solved by heavy atom method and Fourier method and refined by full-matrixleast-squares techniques to a final R=0.058. The distances between Mo atoms in this cluster are 2.731（1）, 2.748（1） and 2.753（1） *** mean value of Mo--Mo bond lengths is slighly shorter than those in other trinuclear Mo clusterswith "looscly coordinated" site. In addition, the PPh3ligand is loosely coordinated to one Mo atomin direction opposite to the μ3-S with Mo--P bond length of 2.647（3）. This is different from theother strocturally analogous clusters, in which the loosely coordinated ligand is trans to μ2--S. Asummary of Mo--Mo and Mo-L bonding for such clusters is given.

关键词： Mo3 the synthesis and crystal structure of OEt research on in part S2P coordinated trinuclear molybdenum cluster compounds loosely CH Cl

Investigation of single MoFe3S4 cubane cluster——I. First successful synthesis by spontaneous self-assembly reaction and structure of （Et4N） [MoFe3S4（Et2NCSS）5]CH3CN

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Chinese Journal of Chemistry 1986年第2期4卷 107-115页

作者： LIU Qiu-Tian* HUANG Liang-Ren KANG Bei-Sheng LIU Chun-Wan WANG Ling-Ling lu jia-xi, fujian institute of research on the structure of matter, academia sinica, fuzhou fujian institute of research on the structure of matter Academia Sinica Fuzhou

A single MoFe3S4cubane-like cluster compound has been synthesized through spon-taneous self-assembly of simple inorganic salts with organosulfur ligand for the first time. （Et4N）-[MoFe3S4（Et2NCSS）5]CH3CN（1） is quite stable in air. The crystal of 1 is monoclinic with spacegroup P21/c, a=22.897（3）,b=12.399（2）,c=20.928（4）,β=97.15（1）°, and Z=4. A fullmatrix least-squares refinement with 6725 unique reflections for all nonhydrogen atoms givesR=0.068. The anion of 1 is the first isolated single MoFe3S4cubane cluster with core oxidation state [Mo-Fe3S4]4+. The distance between the two 6-coordinate metal atoms （Mo,Fe） is 2.624 , which isthe shortest M-M'bond observed for Mo-Fe-S clusters so far and the only one shorter than sim-ilar distances in FeMo-cofactor. The bond orders of this anion were calculated by EHMO method and the results coincide withthe general rule. The structural feature and the unusual stability of 1 can be attributed to the bidentatechelating effect of Et2NCSS-, which leads to high coordination of metal atoms and the various ligatedtypes.

关键词： First successful synthesis by spontaneous self-assembly reaction and structure of Et4N Investigation of single MoFe3S4 cubane cluster Et2NCSS CN

Studies on the synthesis, structure, IR spectra and reactivity of a new dinuclear Mo（0） complex, [Et4N]2[Mo2（CO）8（SCH2CO2Et）2]

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Chinese Journal of Chemistry 1986年第4期4卷 294-300页

作者： ZHUANG Bo-Tao HUANG Liang-Ren HE Ling-Jie CHEN Wen-Zhang YANG Yu lu jia-xi fujian institute of research on the structure of matter, academia sinica. fuzhou fujian institute of research on the structure of matter Academia Sinica Fuzhou

Reaction of Et4NI, NaSCH2CO2Et and Mo（CO）6in CH3CN affords a new dinuclearmolybdenum （O） complex, [Et4N]2[Mo2（CO）B（SCH2CO2Et）2] （1）. Electrochemistry and reactivityinvestigation indicate that 1 undergoes an interesting two-electron oxidation in a single step （-0.43 V）and a substitution of its carbonyls by coordinating solvents resulting in two kinds of Mo（I）-complexes, Mo2（CO）8（SCH2CO2Et）2and (Mo2（CO）6SCH2CO2Et)2（CH3CN）2. vc=o and vmo-co havebeen assigned. The crystal and molecular structure has been determined from three-dimensionalX-ray data. 1 crystallized in the triclinic, space group Pl with a=10.362（1）, b=10.391（1）, c=10.815（2）; a=91.64（2）°, β=100.07（2）°, γ=114.46（1）°, Z=1; R=4.8% for 2975 reflectionswith I>3σ（I）. Nonbonding of Mo…Mo [3.939（1）] and the configuration of MoS2Mo unit in1 are very different from those in related Mo（I）-product. These results confirm our previous speculationthat the two-electron character derives from creation or cleavage of a metal-metal single bondcoupled with structural rearrangement in a bridged bimetallic center.

关键词： Mo2 SCH2CO2Et Et4N CO

Investigation of single MoFe3S4 cubane-like clusters Ⅳ.Synthesis and structure of a novel doublybridged single cubane-like cluster compound MoF3S4（μ-Me2dtc）2（Me2dtc）4·2CH3CN

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Acta Chimica sinica(English Edition) 1988年第4期 286-293页

作者： LIU Qiu-Tian~* HUANG Liang-Ren YANG Yu lu jia-xi fujian institute of research on the structure of matter,academia sinica,fuzhou

By reacting（NH4）2 MoS4,FeCl2 and Me2dtc Na at room temperature,we have synthesizedin one pot two single cubane-like cluster compounds,MoFe3S4（Me2dtc）5·CH2Cl2（1）and MoFe3S4-（Me2dtc）6·2CH3CN（3）,which were separated by stepwise *** structure of 3 wassolved and refined for 5183 reflections to final R value of *** 3 is a novel cluster posses-sing the highest core oxidation state[MoFe3S4]? and contains two Me2dtc *** structuralfeature of 3 is reported and the observation that several single cubane-like clusters containing variousoxidation states can coexist in an assembly system is discussed.

关键词： Mo Synthesis and structure of a novel doublybridged single cubane-like cluster compound MoF3S4 Me2dtc CN CH

FT-IR spectra and normal coordinate analysis of the [Cl2FeS2MoS2FeCl2]2-dianion

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Chinese Journal of Chemistry 1988年第1期 1-6页

作者： LIN Zheng-Yan HE Ling-Jie ZHANG Lin-Na lu jia-xi fujian institute of research on the structure of matter,academia sinica,fuzhou

The FT-IR spectra of the[ClFeSMoSFeCl]dianion were measured in the range500 to 100 cm.A simplified general valence force field was used in a normal coordinate *** calculated frequencies agree well with the observed values,with a mean deviation of less than1.0%,thus confirming the assignments of the vibrational *** 16 force constants,including stretching,bending,torsion and stretching-stretching interactions were *** and the reliability of the results were discussed.

关键词： Cl2FeS2MoS2FeCl2 In dianion FeS FT-IR spectra and normal coordinate analysis of the IR

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固氮酶底物配位活化的量子化学模拟

化学学报 1988年第4期46卷 315-320页

作者：刘春万华建民卢嘉锡中国科学院福建物质结构研究所福州南京大学配合物研究所

用EHMO法就Roussin红盐,MoFeS_(4)(NO)_(2)^(2-),Roussin黑盐及网兜状模型对C_(2)H_(2),N_(2),NNH^(+)和NCH等固氮酶底物的配位活化进行了量子化学模拟.

关键词：配位方式固氮酶还原酶配位活化键级炔烃乙炔黑盐底物红盐量子化学模拟

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若干线型Mo—Fe—S簇合物红外光谱及其与结构关系的研究

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化学学报 1987年第7期45卷 676-681页

作者：何玲洁张琳娜卢嘉锡中国科学院福建物质结构研究所中国科学院福建物质结构研究所福州

本文对若干线型Mo—Fe—S簇合物[Cl2FeS2MoS2FeCl2]2-（1）、[S2MoS2FeCl2]2-（2）、[S2MoS2Fe（SPh）2]2-（3）、[S2MoS2FeS2Fe（SPh）2]3-（4）、[S2MoS2FeS2MoS2]3-（5）、[Cl2FeS2FeCl2]2-（6）、[（PhS）2FeS2Fe（SPh）2]2-（7）的红外光谱进行了研究.通过比较它们的特征频率、结构参数和金属原子的氧化态,对νMo-St、νMo-Sb、νFe-Sb、νFe-SPh、νFe-Cl进行了归属.并对δS-Mo-s的归属作了初步探讨.文中讨论了MoS2Fe单元中Mo原子对νFe-Sb的影响.通过振动频率与结构关系的研究揭示其内在联系及规律性.对两条途径的亲电诱导效应进行了讨论.并提出一个能定性标志Fe→Mo电荷迁移大小的有用参数△ν值.

关键词： Fe 簇合物 Mo 红外光谱 IR 光谱

铁钼硫原子簇化合物的合成与结构研究 Ⅰ.（Et4N）4[Mo2Fe7S8（SPh）12]的合成与晶体结构

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化学学报 1986年第8期44卷 781-786页

作者：康北笙蔡进华陈昌能卢嘉锡中国科学院福建物质结构研究所中国科学院福建物质结构研究所福州

本文通过对巯基铁与MoSi42-反应的研究,对双立方烷型铁-钼-硫原子簇化合物的形成途径及中间物作了讨论.同时报道了[Fe4（SPh）10]（Et4N）2与[MoS4][Et4N]2反应的产物（Et4N）4-[Mo2Fe7S8（SPh）12]（2）的合成、晶体结构、红外光谱和... 详细信息

本文通过对巯基铁与MoSi42-反应的研究,对双立方烷型铁-钼-硫原子簇化合物的形成途径及中间物作了讨论.同时报道了[Fe4（SPh）10]（Et4N）2与[MoS4][Et4N]2反应的产物（Et4N）4-[Mo2Fe7S8（SPh）12]（2）的合成、晶体结构、红外光谱和磁化率.晶体2属三斜晶系,Mr=2670.3;空间群PI;α=12.775（4）,b=13.076（3）,c=20.576（4）A;α=80.00（2）°,β=81.39（2）°,γ=61.51（2）°;V=2966.3（14）A3;Z=1;Dc=1.495g·cm-3;F（000）=1378;偏离因子R=0.077.特别指出了分子中Mo—Mo’的距离[7.188（6）A]是当今同类化合物中最长的,它对研究固氮酶活性中心模型物的合成和结构规律,有重要意义.

关键词： Fe 化合物原子簇立方烷 Mo2Fe7S8 SPh Et4N 晶体结构结晶构造固体结构

六氯三(烯丙基硫脲)一水合二钨(Ⅲ)的晶体与分子结构

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化学学报 1984年第1期42卷 8-13页

作者：卢绍芳商茂虞黄金陵卢嘉锡中国科学院福建物质结构研究所中国科学院福建物质结构研究所福州

六氯三（烯丙基硫脉）一水合二钨（III）晶体属单斜晶系,空间群为P21;晶胞参数:a=8.496（1）A,b=18.760（2）A,c=8.591（1）A,β=91.36（1）°;Z=2;DC=2.297g·cm3。在CAD-4四圆衍射仪上录得独立衍射3069个。晶体结构用重原子法和差值Fo... 详细信息

六氯三（烯丙基硫脉）一水合二钨（III）晶体属单斜晶系,空间群为P21;晶胞参数:a=8.496（1）A,b=18.760（2）A,c=8.591（1）A,β=91.36（1）°;Z=2;DC=2.297g·cm3。在CAD-4四圆衍射仪上录得独立衍射3069个。晶体结构用重原子法和差值Fourier法解出,经全矩阵最小二乘方修正,R=0.038。研究结果表明,这是由三个烯丙基硫脲的硫原子桥联的双核钨原子簇化合物,W—W间距2.443（1）A,显示出较强的金属—金属相互作用。

关键词：烯丙基晶体结构单斜晶系链烯烃基结晶构造固体结构重原子法晶体分子结构