Crystal and Molecular Structure of a New Mono－substituted Titanocene Complex，｛（η~5－Cp）［η~5－（1－（4－OCH_3）C_6H_4）C_6H_（10）Cp］（TiCl_2）｝·0．3（n－C_6H_（14））

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆａＮｅｗＭｏｎｏ－ｓｕｂｓｔｉｔｕｔｅｄＴｉｔａｎｏｃｅｎｅＣｏｍｐｌｅｘ，｛（η~５－Ｃｐ）［η~５－（１－（４－ＯＣＨ_３）Ｃ_６Ｈ_４）Ｃ_６Ｈ_（１０）Ｃｐ］（ＴｉＣｌ_２）｝·０．３（ｎ－...     

等瓣置换反应的研究──手性簇合物［（η~5－MeO_2CC_5H_4）（CO）_2Mo］·［（η~5－MeO_2CC_5H_4）（CO）_2W］Fe（CO）_3（μ_3－S）的分子结构及晶体结构

用Ｘ射线衍射法测定了由η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_３ＭｏＮａ和［（η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_２Ｗ］Ｆｅ－（ＣＯ）_３Ｃｏ（Ｃｏ）_３（μ_３－Ｓ）的等瓣置换反应所生成的手性簇合物──［（η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_２Ｍｏ］－［（η~５－ＭｅＯ_２ＣＣ_５Ｈ_４）（ＣＯ）_２Ｗ］Ｆｅ（ＣＯ）_３（μ_３－Ｓ）的分子结构及晶体结构。晶体属Ｐ１空间群，晶胞参数α＝０．８７１６２（５）ｎｍ，ｂ＝０．７６２１８（４）ｎｍ，ｃ＝１．８７１１１（８）ｎｍ；α＝９４．１６４（４）°，β＝９７．９７９（２）°，γ＝９９．１０８（２）°，Ｚ＝２，μ＝５．９ｃｍ~（－１）。最终的一致性因子Ｒ＝０．０３６，Ｒｗ＝０．０３７．该簇合物含ＭｏＷＦｅＳ四面体簇核，其中Ｍｏ、Ｗ原子以１：１的比例无序地分占了四面体的２个顶点．     

Synthesis and Structureof［（C_2H_5）_4N］［Mo_3（μ_3－O）（μ－Cl）_3（μ－CH_3CH_2COO）_3Cl_3］

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ［（Ｃ_２Ｈ_５）_４Ｎ］［Ｍｏ_３（μ_３－Ｏ）（μ－Ｃｌ）_３（μ－ＣＨ_３ＣＨ_２ＣＯＯ）_３Ｃｌ_３］ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；ＷｕＤｉｎｇ－Ｍｉｎｇ；ＨｕａｎｇＪｉａｎ－Ｑｕａｎ；ＨｕａｎｇＪｉｎ－Ｌ...     

Crystal Structure of La_4V_5Si_4O_（22）──A Mixed－Valence Lanthanum Vanadium（Ⅲ／Ⅳ） Oxosilicate

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＬａ_４Ｖ_５Ｓｉ_４Ｏ_（２２）──ＡＭｉｘｅｄ－ＶａｌｅｎｃｅＬａｎｔｈａｎｕｍＶａｎａｄｉｕｍ（Ⅲ／Ⅳ）ＯｘｏｓｉｌｉｃａｔｅＣｈｅｎＪｉｕ－Ｔｏｎｇ；ＧｕｏＧｕｏ－Ｃｏｎｇ；ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；Ｈｕａ...     

Synthesis and Structure of Propionate－bridged Mixed－metal Cluster Compound：〔MoW_2O_2（O_2CC_2H_5）_6（H_2O）_3〕ZnBr_4·4H_2O

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆＰｒｏｐｉｏｎａｔｅ－ｂｒｉｄｇｅｄＭｉｘｅｄ－ｍｅｔａｌＣｌｕｓｔｅｒＣｏｍｐｏｕｎｄ：〔ＭｏＷ_２Ｏ_２（Ｏ_２ＣＣ_２Ｈ_５）_６（Ｈ_２Ｏ）_３〕ＺｎＢｒ_４·４Ｈ_２Ｏ￥ＬｉｕＨｕａｎｇ；ＸｕＬｉ；Ｈｕａ...     

Syntheses and Characterizations of （η~5－C_5H_5）MoFeCo（CO）_8（μ_3－S） and （η~5－C_5H_5）_2Mo_2Fe（CO）_7（μ_3－S）：X－ray Crystal Structure of （η~5－C_5H_5）MoFeCo（CO）_8（μ_3－S）

ＳｙｎｔｈｅｓｅｓａｎｄＣｈａｒａｃｔｅｒｉｚａｔｉｏｎｓｏｆ（η~５－Ｃ_５Ｈ_５）ＭｏＦｅＣｏ（ＣＯ）_８（μ_３－Ｓ）ａｎｄ（η~５－Ｃ_５Ｈ_５）_２Ｍｏ_２Ｆｅ（ＣＯ）_７（μ_３－Ｓ）：Ｘ－ｒａｙＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ（η~５－Ｃ_５Ｈ_...     

Structure of Molybdenum Complex of Benzothiazole－2－thiolate（η~5－C_5H_5）Mo（CO）_2（C_7H_4NS_2）

ＳｔｒｕｃｔｕｒｅｏｆＭｏｌｙｂｄｅｎｕｍＣｏｍｐｌｅｘｏｆＢｅｎｚｏｔｈｉａｚｏｌｅ－２－ｔｈｉｏｌａｔｅ（η~５－Ｃ_５Ｈ_５）Ｍｏ（ＣＯ）_２（Ｃ_７Ｈ_４ＮＳ_２）ＣｈｅｎｇＧｕｏ－Ｂａｏ~ａ；ＷｕＱｉａｎｇ－Ｊｉｎ~ｂ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ~...     

Crystal and Molecular Structure of(η~5-C_5H_5)_2Yb(NC_4H_4)(OC_4H_8)

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆ（η~５－Ｃ_５Ｈ_５）_２Ｙｂ（ＮＣ_４Ｈ_４）（ＯＣ_４Ｈ_８）ＷａｎｇＳｈａｏ－Ｗｕ；ＹｕＹｏｎｇ－Ｆｅｉ；ＨｕＪｉ－ｐｉｎｇ；ＹｅＺｈｏｎｇ－Ｗｅｎ（ＩｎｓｔｉｔｕｔｅｏｆＯｒｇａｎｉｃＣｈ...     

Synthesis and Crystal Structure of［（n－Bu）_4N］_2［Mo_4O_（10）（OC_（10）H_6O）_2（OCH_3）_2］

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［（ｎ－Ｂｕ）_４Ｎ］_２［Ｍｏ_４Ｏ_（１０）（ＯＣ_（１０）Ｈ_６Ｏ）_２（ＯＣＨ_３）_２］￥ＬｕＸｉａｏ－Ｍｉｎｇ；ＺｈｕＨｕｉ－Ｊｕ；ＹａｎｇＮｉｎｇ；ＬｉｕＳｈｕｎ－Ｃｈｅｎｇ；ＪｉｎＸ?..     

Quasi－aromaticity in Cluster Chemistry Ⅱ． Localized Molecular Orbital Studies on 〔Co_6（CO）_（14）〕~（4－） and 〔Ni_2Co_4（CO）_（14）〕~（2－） Cluster Anions

Ｑｕａｓｉ－ａｒｏｍａｔｉｃｉｔｙｉｎＣｌｕｓｔｅｒＣｈｅｍｉｓｔｒｙⅡ．ＬｏｃａｌｉｚｅｄＭｏｌｅｃｕｌａｒＯｒｂｉｔａｌＳｔｕｄｉｅｓｏｎ〔Ｃｏ_６（ＣＯ）_（１４）〕~（４－）ａｎｄ〔Ｎｉ_２Ｃｏ_４（ＣＯ）_（１４）〕~（２－）ＣｌｕｓｔｅｒＡｎｉ?..     

CRYSTAL STRUCTURE OF (Et_4N)_2[Mo_6O(μ-O)_(12)O_5]

<正> Mr= 1140.4, tetragonal,P4/mnc,a=10.726(2), c=14.208(3)A, Z=2,Dc=2.316 g.cm-3,V=1634.5(9)A3,final R=0.050 for 1457 independent reflections. The anion [Mo6O19]2- has its No atoas in octahedral configuration with one oxygen atom situated in the center of the octahedron, twelve bridging oxygen atoms,and six terminal oxygen atoms. The average bond lengths of the three types of Mo-O bonds are 1.678 A (Mo=0), 1.919A [Mo-(μ-O)], and 2.310 A [Mo-(μs-O)], respectively.     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [CrMo_3 (μ_3-O)_3(μ-O)(μ-O_2CCH_3)_5(O_2CCH_3)_3]Na2 · H_2O

<正> The title complex C CrMo3 (μ3-O )3 (μ-O) (μ-O2CCH3 )5 (O2CCH3)3]2Na2 · H2O (Mr=1814. 32) crystallizes in monoclinic, space group P21/ n with a=11.209(5), b=18. 05(1), c=14. 44(1) A , β= 98. 30(5)°. V=2890 (3) A3, Z=2, A = 2. 08 g/cm3, F(000) -1780, Final R = 0. 049, Rw = 0. 058 for 2622 independent reflectons with I>3σ(I). The complex anion contains two Mo3O4 cores which connect two chromium atoms through four μ3-O atoms and eight bridging CH3COO- groups. Each of the Cr atoms and the Mo atoms is coordinated by six oxygen atoms. The anions are linked by Na cations to form one-dimensional infinite chain structure.     

Reaction of Mo(CO)6 with Alkoxide: Synthesis and Structure of the Mo(0)-OR Complex [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2C6H5)3]

The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2- C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a=15.359(2), b=18.378(3), c=24.952(2)(A), β=102.268(4)°, V=6882.3(16) (A)3, Mr=1348.34, Z=4, Dc=1.301 g/cm3, F(000)=2832 and μ= 0.424 mm-1. The final R=0.0606 and wR=0.1552 for 9396 observed reflections (Ⅰ ＞ 2σ(Ⅰ)). 1 contains a [Mo2O3]3- core in triangular bi-pyramidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three μ-O atoms from C6H5CH2OC6H4O- bridging ligands. The Mo…Mo distance is 3.30(8) (A), indicating no metalmetal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2- has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.     

SYNTHESIS AND STRUCTURE OF （Me4N）[Mo（OC6H4S—o）3]

<正> (Me_4N)[Mo(OC_6H_4S-o)_3] ,Mr=542. 57,orthorhombic,space group Pnb21 with a = 22. 708(1),b = 9. 737(4),c=10. 486(2) A;V=2318. 6A3;Z=4,Dc = 1. 55g/cm3,final R=0. 064 and Rw=0. 074.μ=8. 3cm-1, F(000) = 1108,The atom Mo( V ) of the anion issix-coordinated to three oxygen and three sulfur atoms in a distorted octahedral geometry.     

CRYSTAL STRUCTURE AND REACTIVITY OF (Et_4N) [Mo_3(μ_6-O)-(μ-Cl)_3(μ-OAc)_3Cl_3]

<正> (Et4N)[Mo3(μ3-O)(μ-Cl)3(μ-OAc)3Cl3], C14H29Cl6Mo3NO7, Mr = 823.92, triclinic, P1, a = 17. 508(4), b = 19. 602(3), c=8. 091(2)A, α=91. 25(2)°, β= 96. 56(2)°,γ= 83. 61(2)°, V = 2741(1)A3, Z = 4, Dc = 2.00g/cm3, MoKa (λ=0. 71069A), μ= 19. 44cm-1, F(000) = 1616, T = 23℃, final R = 0. 055, Rw = 0. 068 for 5728 unique intensity data (I≥3σ(I)).The molecule consists of cluster aniorn [Mo3(μ3-O) (μ-Cl)3(μ-OAc)3Cl3]- and cation (Et4N) + . There are two independent molecules in an asymmetric unit whose cluster anions A and B have the same configuration except for some bonding parameters. The cluster core may be described as an equilateral {Mo3} triangle with a capping O atom and three bridging Cl atoms below and above it respectively. In addition, each pair of Mo atoms is bridged by an acetate group and each Mo atom is further coordinated to a terminal chlorine atom. The three Mo - Mo bonds are 2. 587 (2), 2.587(2), 2. 582(2) A for cluster anion A and 2. 587(2), 2.595(2), 2.577 (2) A for cluster a     

［Vmo_3O_4（O_2CEt）_8］_2Na_2的合成与结构

［ＶＭｏ３Ｏ４（Ｏ２ＣＥｔ）８］２Ｎａ２（１），三斜晶系，Ｐ１空间群，ａ＝１２．９７７（７），ｂ＝１４．０７０（６），ｃ＝１２．３３８（８），α＝１０９．８１（４），β＝１１７．２０（４），γ＝９０．５１（５）°，Ｖ＝１８４８．８３，Ｍｒ＝２０２０．６，Ｄｃ＝１．８１ｇ／ｃｍ３，Ｚ＝１，Ｆ（０００），μ＝１２．９ｃｍ１（ＭｏＫα）对３７４２个可观测反射点（Ｉ＞３σ（Ｉ））最终一致性因子为Ｒ＝０．０１８，Ｒω＝０．０５４。单晶结构分析表明，簇阴离子中两个［Ｍｏ３Ｏ４］４＋单元通过两个＂桥＂金属Ｖ原子连接成一个奇特的环状结构，Ｍｏ－Ｍｏ平均键长为２．５１９（１），Ｍｏ…Ｖ间平均距离为３．６５４。簇阴离子通过Ｎａ＋连成一个一维长链，Ｎａ原子与氧原子形成一个少见的五配位三角双锥结构，Ｎａ－Ｏ距离仅为２．３１２，Ｎａ－Ｏ间较强的相互作用以及无限长链的晶体结构很好地解释了簇合物（１）的稳定性和不溶性。     

含柠檬酸配体的钼硫簇合物的合成与晶体结构的测定

合成了含有Mo—S簇阴离子 [Mo2 O2 ( μ S) 2 (C6H5O7) (C6H4 O7) ]5-柠檬酸簇合物 ,并通过元素分析、红外光谱、紫外 可见光谱和X射线光电子能谱对配合物进行了表征 ,用X射线衍射法测定了该化合物的晶体结构 .结果表明 ,该簇合物属于单斜晶系 ,空间群P2 1/c,a =2 3 766( 5)nm ,b =1 3 2 74 ( 3 )nm ,c =2 2 4 71 ( 5)nm ,α=γ =90°,β=1 1 8 2 1°,V =6 2 4 7( 2 )nm3 ,Z =8,一致性因子R =0 0 83 1 ,R2 ,w=0 1 536.该簇合物阴离子中每一个Mo原子都采取扭曲的八面体结构 ,柠檬酸通过羟基、α 羧基、一个 β 羧基与Mo配位 .晶体结构表明在一个结晶学上不对称的结构单元内有两个结晶学上独立的分子 .     

Reaction of Mo(CO)_6 with Alkoxide: Synthesis and Structure of the Mo(0)-OR Complex [Et_4N]_3[Mo_2(CO)_6(μ-OC_6H_4OCH_2C_6H_5)_3]

The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2- C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a = 15.359(2), b = 18.378(3), c = 24.952(2), β = 102.268(4)°, V = 6882.3(16) 3, Mr = 1348.34, Z = 4, Dc = 1.301 g/cm3, F(000) = 2832 and μ = 0.424 mm-1. The final R = 0.0606 and wR = 0.1552 for 9396 observed reflections (I > 2σ(I)). 1 contains a [Mo2O3]3- core in triangular bi-pyramidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three μ-O atoms from C6H5CH2OC6H4O- bridging ligands. The Mo…Mo distance is 3.30(8) , indicating no metal- metal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2- has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.     

Synthesis and Crystal Structure of （Et4N）3[{V（o—C6H4OS）3}2Na]

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ（Ｅｔ_４Ｎ）_３［｛Ｖ（ｏ－Ｃ_６Ｈ_４ＯＳ）_３｝_２Ｎａ］￥ＷｅｎＴｉｎｇ－Ｂｉｎ；ＸｕＹｏｎｇ－Ｊｉｎ；ＳｈｉＪｉ－Ｃｈｅｎｇ；ＤｅｎｇＹｕ－Ｈｅｎｇ；ＣｈｅｎＣｈａｎｇ－Ｎｅｎｇ；Ｌｉｕ...     

CRYSTAL STRUCTDBE OF H_2(Et_4N)_2[Mo_8O_(26)]

<正> Mr= 1446.02, Monoclinic, P21/n, a = 11.841(2),b= 20.008(6), c= 12.053(8)A,β=105.15(3)°,V= 2756(3)A3,Z= 2, DC = 1.738 g·cm-3. Final R=0.035 for 4326 reflections. The title compound is the decomposition product of the trinuclear Mo cluster anion [Mo3(μ3-O)(μ-Cl)3(μ-OAc)3Cl3]-. The [No8O26]4- anion reported here has the a -type configuration, which consists of a ring made up of six edge-sharing [MoO5] octahedra linked loosely to two [MoO4] units.