THE REACTION OF（μ_3－CPh）Co_3（CO）_9 WITH TRANSITION METAL CARBONYL ANION M（CO）_3（RCOCp）AND CHARACTERIZATION OF CLUSTERS（μ_3－CPh）CO_2M（CO）_8（RCOCPp）（M＝Mo，W；R＝H，CH_3．C_2H_5O）

ＴＨＥＲＥＡＣＴＩＯＮＯＦ（μ_３－ＣＰｈ）Ｃｏ_３（ＣＯ）_９ＷＩＴＨ　ＴＲＡＮＳＩＴＩＯＮＭＥＴＡＬＣＡＲＢＯＮＹＬＡＮＩＯＮＭ（ＣＯ）_３（ＲＣＯＣｐ）ＡＮＤＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＯＦＣＬＵＳＴＥＲＳ（μ_３－ＣＰｈ）ＣＯ_２Ｍ（ＣＯ）_８（ＲＣＯＣＰｐ）（Ｍ＝Ｍｏ，Ｗ；Ｒ＝Ｈ，ＣＨ_３．Ｃ_２Ｈ_５Ｏ）Ａｕｔｈｏｒｔｏｗｈｏｍｃｏｒｍｓｐｏｎｄｅｎｃｅｓｈｏｕｌｄａｄｄｒｅｓｓｅｄ．ＥｘｐｅｒｉｍｅｎｔａｌｓｅｃｔｉｏｎＧｅｎｅｒａｌｐｒｏｃｅｄｕｒｅａｎｄｍａｔｅｒｉａｌＡｌｌｏｐｅｒａｔｉｏｎｗａｓｃａｒｒｉｅｄｏｕｔｕｎｄｅｒｈｉｇｈｌｙｐｕｒｅｎｉｔｒｏｇｅｎａｔｍｏｓｐｈｅｒｅｕｓｉｎｇｓｈａｄａｒｄＳｃｈｌｅｎｌｃａｎｄｖａｃｕｕｍｔｅｃｈｎｉｑｕｅｓ．Ｈｅ－ｃａｎｅ，ｂｅｎｚｅｎｅａｎｄｔｅｔｒａｈｙｄｒｏｆｕｒａｎｗｅｒｅｐｒｅｄｒｉｅｄｏｖｅｒｓｏｄｉｕｍｗｉｒｅａｎｄｄｉｓｔｉｌｌｅｄｆｒｏｍｓｏｄｉｕｍ－ｂｅｎｚｏｐｈｅｎｏｎｅｕｎｄｅｒｎｉｔｒｏｇｅｎ．ＮａＭ（ＣＯ）３（ＲＣＯＣＰ）ａｎｄＰｈＣＣｏ３（ＣＯ），ｗｅｒｅｐｒｅｐａｒｅｄａｃｃｏｒｄｉｎｇｔｏｌｉｔｅｒａｔＵｒｅ     

Synthesis and Crystal Structure of （1,3—^tBu2C5H3）2Sm（μ—Cl）2Li（THF）2

1　ＩＮＴＲＯＤＵＣＴＩＯＮＡｓａｔｙｐｅｏｆｉｍｐｏｒｔａｎｃｅｐｒｅｃｕｒｓｏｒ,ａｌｏｔｏｆｏｒｇａｎｏｌａｎｔｈａｎｉｄｅｃｈｌｏｒｉｄｅｃｏｍｐｌｅｘｅｓｈａｖｅｂｅｅｎｓｙｎｔｈｅｓｉｚｅｄａｎｄｓｔｒｕｃｔｕｒａｌｌｙｃｈａｒａｃｔｅｒｉｚｅｄ[1].Ｔｈｅｂｉｍｅｔａｌｌｉｃｃｏｍｐｌｅｘｅｓｃｏｎｔａｉｎｉｎｇａｌｋａｌｉｍｅｔａｌ,Ｃｐ2Ｌｎ(μＣｌ)2Ｍ(Ｌ)(Ｃｐ=η5Ｃ5Ｈ5ｏｒＣ5Ｍｅ5;Ｍ=Ｌｉ,Ｎａ;Ｌ=ＴＨＦ,ＴＭＥＤＡ),ｉｓａｍａｉｎｓｔｒｕｃｔｕｒｅｔｙｐｅ.Ｉｎｔｈｅｃｏｕｒｓｅｏ…     

STUDY ON SYNTHESIS，CHARACTERIZATION AND CATALYSIS OF PILLARED ANION CLAY（Ⅲ）──SYNTHESIS OF ZnAl－BW_（11）O_（39）Z（H_2）~（n－）

ＳＴＵＤＹＯＮＳＹＮＴＨＥＳＩＳ，ＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＡＮＤＣＡＴＡＬＹＳＩＳＯＦＰＩＬＬＡＲＥＤＡＮＩＯＮＣＬＡＹ（Ⅲ）──ＳＹＮＴＨＥＳＩＳＯＦＺｎＡｌ－ＢＷ_（１１）Ｏ_（３９）Ｚ（Ｈ_２）~（ｎ－）ＴｈａｎｋｓｆｏｒｔｈｅｓｕｐｐｏｒｔｏｆＦｏｕｎｄａｔｉｏｎｏｆＣＥＣａｎｄｔｈｅｏｐｅｎｌａｂｏｆＨｙｄｒｏｔｈｅｒｍａｌＳｙｎｔｈｅｓｉｓｉｎＪｉｎｎＵｎｉｖｅｒｓｉｔｙｅｄｄｉｆｆｅｒｅｎｔｋｉｎｄｓｏｆｔｒｉｈｅｔｅｒｏｐｏｌｙｏｘｏｍｅｔａｌａｔｅ（ＴＨ＇ＰＯＭｓ）ｔｏｔｈｅＺｎＡＩｌａｙｅｒｅｄｃｌａｙｓ，ｕｓｉｎｇｔｈｅｅｓｔｅｒｉｆｉｃａｔｉｏｎｏｆｎ－ｂｕｔｙｌａｌｃｏｈｏｌａｎｄａｃｅｔｉｃａｃｉｄａｓｐｒｏｂｅｒｅａｃｔｉｏｎ．ａｎｄｆｏｕｎｄｔｈａｔｔｈｅｐｉｌｌａｒｅｄｃｏｍｐｏｕｎｄｓｗｅｒｅｍｏｒｅａｃｔｉｖｅａｎｄｓｅｌｅｃｔｉｖｅｔｈａｎｔｈｅｓｏｌｉｄａｃｉｄｃａｔａｌｙｓｔｓｓｕｃｈａｓａｃｉｄｉｃｉｏｎ－ｅｘｃｈａｎｇｅｒｅｓｉｎｓｌ４］．Ｏｎｔｈｅｂａｓｉｓｏｆｐｒｅｖｉｏｕｓｗｏｒｋ．ｗｅｎｏｗｅｎｃａｐｓｕｌａｔｅｔｒｉｈｅｔｅｒｏｐｏｌｙｏｘｏｍｅ     

Synthesis and Structure of a Novel Cluster with Trigonal-bipyramidal Ge_2Ru_3 Core

ＩｎｔｒｏｄｕｃｔｉｏｎＷｅｒｅｃｅｎｔｌｙｒｅｐｏｒｔｅｄａｎｉｎｔｒａｍｏｌｅｃｕｌａｒｔｈｅｒｍａｌｒｅａｒ ｒａｎｇｅｍｅｎｔｂｅｔｗｅｅｎＳｉ—ＳｉａｎｄＦｅ—Ｆｅｂｏｎｄｓｉｎｔｈｅｄｉｎｕ ｃｌｅａｒｉｒｏｎｃｏｍｐｌｅｘ { (Ｍｅ2 ＳｉＳｉＭｅ2 ) [(η5 Ｃ5Ｈ4 )Ｆｅ(ＣＯ) ]2 (μ ＣＯ) 2 } (Ｓｃｈｅｍｅ 1) .1 5Ｔｈｅｔｈｅｒｍａｌｒｅａｒｒａｎｇｅｍｅｎｔｗａｓｌａｔｅｒｅｘｔｅｎｄｅｄｔｏｇｅｒｍａｎｉｕｍ ｉｒｏｎａｎｄｓｉｌｉｃｏｎ ｒｕｔｈｅｎｉ ｕｍａｎａｌｏｇｕｅｓ .6 8Ｔｈ…     

Skeleton Vibrations and Force Constants of ［Fe_2Cr（μ_3－O）（glycine）_6（H_2O）_3］（NO_3）_7．3H_2O

ＳｋｅｌｅｔｏｎＶｉｂｒａｔｉｏｎｓａｎｄＦｏｒｃｅＣｏｎｓｔａｎｔｓｏｆ［Ｆｅ_２Ｃｒ（μ_３－Ｏ）（ｇｌｙｃｉｎｅ）_６（Ｈ_２Ｏ）_３］（ＮＯ_３）_７．３Ｈ_２ＯＺｈａｎｇＬｉｎ－Ｎａ，ＬｉｎＺｈｅｎｇ－Ｙａｎ（ＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｏ...     

Preparation and Crystal Structures of LaCl_3（12－crown－4）（MeOH）and［LaCl_3（phen）_2（H_2O）］·MeOH

Ｐｒｅｐａｒａｔｉｏｎ　ａｎｄ　Ｃｒｙｓｔａｌ　Ｓｔｒｕｃｔｕｒｅｓ　ｏｆ　ＬａＣｌ_３（１２－ｃｒｏｗｎ－４）（ＭｅＯＨ）ａｎｄ［ＬａＣｌ_３（ｐｈｅｎ）_２（Ｈ_２Ｏ）］·ＭｅＯＨＭａｏＪｉａｎｇ－Ｇａｏ（ＦｕｊｉａｎＩｎｓｔｉｔｕｔｅｏｆＲｅｓｅａ...     

STUDY ON REACTION OF （μ_3－CCO_2Et）CO_2M（CO）_8（CpMe）（M＝Mo，W） WITH Na_2［Fe（CO）_4］．SYNTHESIS OF TWO KINDS OF THE NOVEL CLUSTERS EtO_2CCFeCoM（CO）_8（CpMe）H AND （OCC）FeCoM（CO）_8（CpMe）

ＳＴＵＤＹＯＮＲＥＡＣＴＩＯＮＯＦ（μ_３－ＣＣＯ_２Ｅｔ）ＣＯ_２Ｍ（ＣＯ）_８（ＣｐＭｅ）（Ｍ＝Ｍｏ，Ｗ）ＷＩＴＨＮａ_２［Ｆｅ（ＣＯ）_４］．ＳＹＮＴＨＥＳＩＳＯＦＴＷＯＫＩＮＤＳＯＦＴＨＥＮＯＶＥＬＣＬＵＳＴＥＲＳＥｔＯ_２ＣＣＦｅＣｏＭ（ＣＯ）_８...     

THE REVISED STRUCTURE OF GNETIFOLIN A

ＴＨＥＲＥＶＩＳＥＤＳＴＲＵＣＴＵＲＥＯＦＧＮＥＴＩＦＯＬＩＮＡ￥ＺｈｉＭｉｎＷＡＮＧ；ＸｉａｏＴｉａｎＬＩＡＮＧａｎｄＳｈｕＦｅｎｇＣＨＥＮ（ＩｎｓｔｉｔｕｔｅｏｆＭａｔｅｒｉａＮｅｄｉｃａ，Ｃｈｉｎｅｓｅ．ＡｃａｄｅｍｙｏｆＭｅｄｉｃａｌＳｃｉｅ...     

A NOVEL APPROACH FOR THE PREPARATION OF MEDIUM-SIZE LACTAMS

ＡＮＯＶＥＬＡＰＰＲＯＡＣＨＦＯＲＴＨＥＰＲＥＰＡＲＡＴＩＯＮＯＦＭＥＤＩＵＭ－ＳＩＺＥＬＡＣＴＡＭＳ￥ＹｕｎＸｉｎＢｏ；ＤｏｎｇＬｕＢＡＩ（ＳｈａｎｇｈａｉＩｎｓｔｉｔｕｔｅｏｆＭａｔｅｒｉａＭｅｄｉｃａ，ＣｈｉｎｅｓｅＡｃａｄｅｍｙｏｆＳｃｉｅｎ...     

AN ESR STUDY OF MgO TREATED WITH SHOCK WAVE

ＡＮＥＳＲＳＴＵＤＹＯＦＭｇＯＴＲＥＡＴＥＤＷＩＴＨＳＨＯＣＫＷＡＶＥ￥ＴｉｎｇＬｕＹＡＮＧ；ＫａｎｇＸＵ；ＬｉａｎｇＢｏＦＥＮＧ；ａｎｄＳｈｉＫｏｎｇＳＨＥＮ（ＬａｎｚｈｏｕＩｎｓｔｉｔｕｔｅｏｆＣｈｅｍｉｃａｌＰｈｙｓｉｃｓ，ＣｈｉｎｅｓｅＡｃａ...     

Single- and double-cubane clusters in the multiple oxidation states [VFe(3)S(4)](3+,2+,1+)

A new series of cubane-type [VFe(3)S(4)](z)() clusters (z = 1+, 2+, 3+) has been prepared as possible precursor species for clusters related to those present in vanadium-containing nitrogenase. Treatment of [(HBpz(3))VFe(3)S(4)Cl(3)](2)(-) (2, z = 2+), protected from further reaction at the vanadium site by the tris(pyrazolyl)hydroborate ligand, with ferrocenium ion affords the oxidized cluster [(HBpz(3))VFe(3)S(4)Cl(3)](1)(-) (3, z = 3+). Reaction of 2 with Et(3)P results in chloride substitution to give [(HBpz(3))VFe(3)S(4)(PEt(3))(3)](1+) (4, z = 2+). Reaction of 4 with cobaltocene reduced the cluster with formation of the edge-bridged double-cubane [(HBpz(3))(2)V(2)Fe(6)S(8)(PEt(3))(4)] (5, z = 1+, 1+), which with excess chloride underwent ligand substitution to afford [(HBpz(3))(2)V(2)Fe(6)S(8)Cl(4)](4)(-) (6, z = 1+, 1+). X-ray structures of (Me(4)N)[3], [4](PF(6)), 5, and (Et(4)N)(4)[6] x 2MeCN are described. Cluster 5 is isostructural with previously reported [(Cl(4)cat)(2)(Et(3)P)(2)Mo(2)Fe(6)S(8)(PEt(3))(4)] and contains two VFe(3)S(4) cubanes connected across edges by a Fe(2)S(2) rhomb in which the bridging Fe-S distances are shorter than intracubane Fe-S distances. M?ssbauer (2-5), magnetic (2-5), and EPR (2, 4) data are reported and demonstrate an S = 3/2 ground state for 2 and 4 and a diamagnetic ground state for 3. Analysis of (57)Fe isomer shifts based on an empirical correlation between shift and oxidation state and appropriate reference shifts results in two conclusions. (i) The oxidation 2 --> 3 + e(-) results in a change in electron density localized largely or completely on the Fe(3) subcluster and associated sulfur atoms. (ii) The most appropriate charge distributions are [V(3+)Fe(3+)Fe(2+)(2)S(4)](2+) (Fe(2.33+)) for 1, 2, and 4 and [V(3+)Fe(3+)(2)Fe(2+)S(4)](3+) (Fe(2.67+)) for 3 and [V(2)Fe(6)S(8)(SEt)(9)](3+). Conclusion i applies to every MFe(3)S(4) cubane-type cluster thus far examined in different redox states at parity of cluster ligation. The formalistic charge distributions are regarded as the best current approximations to electron distributions in these delocalized species. The isomer shifts require that iron atoms are mixed-valence in each cluster.     

The Synthesis and Crystallographic Characterization of Heterotrimetallic Linear Complex of [Et_4N][ (Ph_3P)_2{CuS_2WS_2Fe} Br_2]

1INTRoDUCTIONMolybdenum(Tungsten)-copper-sulfurandmolydenum(tungsten)-iron-sulfurcompoundshavebeenstudiedextensivelybecauseoftheirconnectionwithbiologicalprocesses[l,2j.Someheterotrimetalliccomplexeshavebeensynthesized,suchas[NEt'jtPh,p)sAgSzMoSzCu(CN))and[NEt'jtPh,P),AgS,MooCu(CN)jt3i,[l(CH,CH,)'j(PPh,)2{AgS2WS2Cu}(CN)jt4i,[(CH,CH2)4j(PPh,)2{AgS,WOCu}(CN)j('3,butheterotrimetal1iccomplexescontainingtungsten,copper,andironatomshaveseldombeenreported.Onecomplexofthiskindha…     

Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato-Bridges [Et4N] 2 [Mo2 (CO) 8 (SC6H4-Cl -p) 2]

Reaction of Mo (CO)6 with p-Cl-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum (0) compound [Et4N]2 [Mo2 (CO)8 (SC6H4-Cl-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C36H48Cl2Mo2N2O8S2, Mr= 963.71, monoclinie, P21/c, a=9. 269(4),b=13.750(3), c=17.466(6) A ;β=104.84(3)°; V=2151.8(3) A3; Z=2; Dc=1.49 g/cm3; F(000)=984; μ=8.3 cm-1; MoKα radiation (λ=0. 71073A ); Final R = 0. 055 and Rw=0. 065 for 3287 reflections with I＞3. 0σ(I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distance is 4. 014(2) A , and this obviously indicates the absence of Mo-Mo bond.     

Structural Studies of [V_2S_6O_2(CuPPh_3)_4(CuMeCN)_2]·2CH_2Cl_2·2PrOH

ＳｔｒｕｃｔｕｒａｌＳｔｕｄｉｅｓｏｆ［Ｖ_２Ｓ_６Ｏ_２（ＣｕＰＰｈ_３）_４（ＣｕＭｅＣＮ）_２］·２ＣＨ_２Ｃｌ_２·２ＰｒＯＨＺＨＡＮＧＨａｎ－Ｈｕｉ；ＹＵＸｉｕ－Ｆｅｎ；ＹＡＮＧＲｏｎｇ－Ｓｈｅｎｇ；ＺＨＥＮＧＦａ－Ｋｕｎ；ＨＵＡＮＧＬｉａｏ－Ｙｕ...     

含有环己巯基配体的钨簇合物的合成及晶体结构研究

C6H11Na, Et4NBF4, FeCl2, (NH4)2WS4在20mL CH3OH溶剂的反应中, 标题簇合物(Et4N)3[W2Fe6S8(SC6H11)6(OCH3)3]被分离得到, 对其进行X-ray 单晶衍射和结构解析。 该化合物属正交晶系,空间群 Pmmn, 晶胞参数 a = 17.370(5), b = 15.986(4), c = 17.858(3), V = 4958.6(6)3, Z = 2,C63H135N3O3S14Fe6W2, Mr = 2134.47, Dc = 1.43g/cm3, F(000) = 2172.0, m(MoKa) = 3.49 mm-1, T = 293(2)K。 采用2966个I > 2.0s (I) 的衍射点对所有非氢原子参数进行结构修正。 得到最后的偏离因子为R = 0.072, Rw = 0.091。 这是一个双类立方烷的结构, 2个单类立方烷的端基金属钨原子通过3个甲氧基桥联。 [WFe3S4] 与 [MoFe3S4]簇核结构比较说明, 两者存在一定的相似性。     

Reactions of [Et(4)N](3)[Sb{Fe(CO)(4)}(4)] with Alkyl Halides and Dihalides: Formation of the Alkyl- and the Dialkylantimony-Iron Carbonyl Complexes

The reactions of [Et(4)N](3)[Sb{Fe(CO)(4)}(4)] (1) with RX (R = Me, Et, n-Pr; X = I) in MeCN form the monoalkylated antimony complexes [Et(4)N](2)[RSb{Fe(CO)(4)}(3)] (R = Me, 2; R = Et, 4; R = n-Pr, 6) and the dialkylated antimony clusters [Et(4)N][R(2)Sb{Fe(CO)(4)}(2)] (R = Me, 3; R = Et, 5; R = n-Pr, 7), respectively. When [Et(4)N](3)[Sb{Fe(CO)(4)}(4)] reacts with i-PrI, only the monoalkylated antimony complex [Et(4)N](2)[i-PrSb{Fe(CO)(4)}(3)] (8) is obtained. The mixed dialkylantimony complex [Et(4)N][MeEtSb{Fe(CO)(4)}(2)] (9) also can be synthesized from the reaction of 2 with EtI. While the reaction with Br(CH(2))(2)Br produces [Et(4)N](2)[BrSb{Fe(CO)(4)}(3)] (10), treatment with Cl(CH(2))(3)Br forms the monoalkylated product [Et(4)N](2)[Cl(CH(2))(3)Sb{Fe(CO)(4)}(3)] (11) and a dialkylated novel antimony-iron complex [Et(4)N][{&mgr;-(CH(2))(3)}Sb{Fe(CO)(4)}(3)] (12). On the other hand, the reaction with Br(CH(2))(4)Br forms the monoalkylated antimony product and the dialkylated antimony complex [Et(4)N][{&mgr;-(CH(2))(4)}Sb{Fe(CO)(4)}(2)] (13). Complexes 2-13 are characterized by spectroscopic methods or/and X-ray analyses. On the basis of these analyses, the core of the monoalkyl clusters consists of a central antimony atom tetrahedrally bonded to one alkyl group and three Fe(CO)(4) fragments and the dialkyl products are structurally similar to the monoalkyl clusters, with the central antimony bonded to two alkyl groups and two Fe(CO)(4) moieties in each case. The dialkyl complex 3 crystallizes in the monoclinic space group P2(1)/c with a = 13.014(8) ?, b = 11.527(8) ?, c = 17.085(5) ?, beta = 105.04(3) degrees, V = 2475(2) ?(3), and Z = 4. Crystals of 12 are orthorhombic, of space group Pbca, with a = 14.791(4) ?, b = 15.555(4) ?, c = 27.118(8) ?, V = 6239(3) ?(3), and Z = 8. The anion of cluster 12 exhibits a central antimony atom bonded to three Fe(CO)(4) fragments with a -(CH(2))(3)- group bridging between the Sb atom and one Fe(CO)(4) fragment. This paper discusses the details of the reactions of [Et(4)N](3)[Sb{Fe(CO)(4)}(4)] with a series of alkyl halides and dihalides. These reactions basically proceed via a novel double-alkylation pathway, and this facile methodology can as well provide a convenient route to a series of alkylated antimony-iron carbonyl clusters.     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound [Et4N ] 2 [Mo2 (CO) 8 (SC6H4-OCH3-p) 2]

Reaction of Mo(CO)6 with p-H3CO-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2 (CO)8 (SC6H4-OCH3-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C38H54Mo2N2O10S2, Mr = 954.87, triclinic, P-1, a = 11.348 (7), b =11.616(5), c=10.065(7) A, a=113.86(4), β=111.39(5), γ=91.92(5)°, V=1104.0(1) A3, Z=1, Dc=1.44 g/cm3, F(000)=492, μ=7.0cm-1, Final R=0. 046 and Rw=0. 049 for 2657 reflections with I＞3. Oσ(I). The X-ray structure analysis revealed that the Mo2S2 core of 1 is planar. The geometry around each Mo atom is a distorted octahedron, the two octahedrons form an edge-sharing bioctahedron. The bond. In addition, the 95Mo NMR chemical shift of 1 is discussed.     

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.     

[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。