螺（异苯并呋喃—1（3H）,9‘—（9H）—2’—N,N—二苄胺基—6‘—二乙胺基占吨）—…

合成了螺（异苯并呋喃－１（３Ｈ），９’－（９Ｈ）－２’－Ｎ，Ｎ－二苄胺基－６’－二乙胺基占吨）－酮－３，Ｃ３８Ｈ３４Ｎ２Ｏ５，单斜晶系，空间群Ｃｃ，晶体学参数为ａ＝１６．８２６（４），ｂ＝１０．６４８（４），ｃ＝１７．６１８（７）Ａ，β＝９２．２５（２）°，Ｖ＝３１５４（２），Ａ＾３，Ｚ＝４，Ｍｒ＝５６６．７，Ｄｘ＝１．１９ｇ／ｃｍ＾３，Ｆ（０００）＝１２００。结构由直接法解出，偏离因子Ｒ＝０．０     

三环己基锡O，O＇－二（4－氯苯基）二硫代磷酸酯和二丁基锡双［O，O＇－二（4－甲基苯基）二硫代磷酸酯］的分子和晶体结构

三环己基锡Ｏ，Ｏ＇－二（４－氯苯基）二硫代磷酸酯（Ⅰ），Ｃ＿（３０）Ｈ＿（４１）Ｃｌ＿２Ｏ＿２ＰＳ＿２Ｓｎ，Ｍ＿ｒ＝７１８．３６，单斜晶系，Ｐ２＿１／ｎ，ａ＝１６．１５１（２），ｂ＝９．４１５（１），ｃ＝２２．９８７（３），β＝１０５．６９（１）°，Ｚ＝４，Ｄｃ＝１．４１８ｇ·ｃｍ￣（－３），Ｒ＝０．０６３；二丁基锡双［Ｏ，Ｏ＇－二（４－甲基苯基）二硫代磷酸酯］（Ⅱ），Ｃ＿（３６）Ｈ＿（４６）Ｏ＿４Ｐ＿２Ｓ＿４Ｓｎ，Ｍ＿ｒ＝８５１．６６，单斜晶系，Ｐ２＿１／ｃ，ａ＝１２．２８４（４），ｂ＝９．８０７（１），ｃ＝３４．４７１（８），β＝９９．０２（２）°，Ｚ＝４，Ｄ＿ｃ＝１．３７９ｇ·ｃｍ（－３），Ｒ＝０．０４２。化合物Ⅰ具有单分子的四配位变形四面体结构。其Ｓｎ－Ｓ（１）键长为２．５０１（２）；而Ｓｎ与Ｓ（２）的原子间距则为３．５９７；化合物Ⅱ具有单分子的六配位变形八面体结构，其Ｓｎ－Ｓ（１），Ｓｎ－Ｓ（２），Ｓｎ－Ｓ（３）和Ｓｎ－Ｓ（４）的键长分别为２．４９５（３），２．４９３（２），３．２４４（４）和３．２２８（３）。     

RE[CH2（CH2）4CONC4H9]3（NO3）3（RE=La,Dy）的合成和晶体结构

采用Ｘ－射线四园衍射仪测定了Ｄｙ「Ｃｈ２（ＣＨ２）４ＣＯＮＣ４Ｈ９」３（ＮＯ３）３和Ｌａ「ＣＨ２（ＣＨ２）４ＣＯＮＣ４Ｈ３」３（ＮＯ３）３的晶体结构。两个配合物具有相似的结构，均属单斜晶系，空间群为Ｐ２１／ｃ。晶体参数：Ｄｙ「Ｌａ」：ａ＝１．８５６４（３）「１．８５６４（２）」ｎｍ，ｂ＝０．９７６９（２）「０．９８３４（１）」ｎｍ，ｃ＝２．１８６３（６）「２．２００３８（７）」ｎｍ，β＝９６．０８     

［Cu_2（Gly－GlyO）_2（4，4＇－bpy）（OH）_2］·9H_2O

将Ｇｌｙ－ＧｌｙＯ、４，４＇－联吡啶与Ｃｕ（ＮＯ_３）_２·Ｈ_２Ｏ在二次水溶液中反应，合成出以４，４＇－ｂｐｙ为中继基、Ｃｌｙ－ＧｌｙＯ为螯环的新型双核铜配合物，经Ｘ射线单晶结构分析确定该配合物晶体的化学结构式为［（Ｈ_２ＮＣＨ_２ＣＯＮＨＣＨ_２ＣＯＯ）Ｃｕ（ＯＨ）（Ｃ_（１０）Ｈ_８Ｎ_２）Ｃｕ（ＯＮ）（Ｈ_２ＮＣＨ_２ＣＯＮＨＣＨ_２ＣＯＯ）］·９Ｈ_２Ｏ．晶体属Ｐ　空间群，晶胞参数ａ＝１．１４１２ｎｍ，ｂ＝１．２２９８ｎｍ，ｃ＝１．４２６９ｎｍ，α＝１１３．８２°，β＝１０１．９１°，γ＝１０３．６４°，Ｚ＝２．最终一致性因子Ｒ值为０．０６８，Ｒ_ｗ值为０．０５７，标准偏差σ＝０．１９５１。     

μ－4，4＇－联吡啶桥联三核Cu（Ⅱ）配合物的合成和磁性

合成了３种以４，４＇－联吡啶为桥联配体的三核环状Ｃｕ（Ⅱ）配合物［Ｃｕ＿３（４，４＇－ｂｐｙ）＿３·（ｐｈｅｎ）＿３］（ＣｌＯ＿４）＿６·２Ｈ＿２Ｏ（１）、［Ｃｕ＿３（４，４＇－ｂｐｙ）＿３］（ｂｐｙ）＿３］（ＣｌＯ＿４）＿６·Ｈ＿２Ｏ（２）和［Ｃｕ＿３（４，４＇－ｂｐｙ）＿３·（ＮＯ＿２－ｐｈｅｎ）＿３］（ＣｌＯ＿４）＿６·６Ｈ＿２Ｏ（３）。经元素分析、电导、ＩＲ、电子光谱、ＥＳＲ、磁化率等方法进行了表征，推定该配合物具有以４，４＇－联吡啶为扩展桥的结构。利用Ｈｅｉｓｅｎｂｅｒｇ模型求得交换参数Ｊ值为－０．２３ｃｍ－１（１）和－０．９０ｃｍ－１（３），表明配合物中金属离子间仅有很弱的反铁磁交换作用．     

4－氨基－3，5－二甲基－1，2，4－三唑水杨亚胺合铜〔Ⅱ〕配合物合成及其单晶结构

４－氨基－３，５－二甲基－１，２，４－三唑（ＴＺ）与水杨醛缩合形成４－（邻羟苯基亚甲基）－亚胺－３，５－二甲基－１，２，４－三唑Ｓｃｈｉｆｆ碱（ＳＡＴＺ），该Ｓｃｈｉｆｆ碱与Ｃｕ（ＣｌＯ＿４）＿２·６Ｈ＿２Ｏ形成配合物Ｃｕ（ｓａｔｚ）＿２·６Ｈ＿２Ｏ，分子式为Ｃ＿（２２）Ｈ＿（２２）ＣｕＮ＿８Ｏ＿２·６Ｈ＿２Ｏ。经Ｘ射线晶体结构分析表明，晶体属于单斜晶系，空间群Ｐ２＿１／ｃ，Ｚ＝２，α＝８．２０２（１），ｂ＝１９．５６９（４），ｃ＝８．９７２（８）Ａ，β＝１０７．７２°（２），Ｖ＝１３７１．８（５）Ａ３，Ｄｃ＝１．４６ｇ／ｃｍ￣３，μ＝０．８５３ｍｍ￣（－１），Ｆ（０００）＝６３０，Ｒ＝０．０５１，Ｒ＿ｗ＝０．０６２。分子中２个偶氮甲碱（－Ｃ＝Ｎ－）中　　　的Ｎ原子及２个酚氧原子与中心Ｃｕ原子形成规则的菱形平面结构。     

meso－5，10，15，20－四（3，4，5－三甲氧基苯基）卟啉的晶体和分子结构

用Ｘ－射线测定了ｍｅｓｏ－５，１０，１５，２０－四（３，４，５－三甲氧基苯基）卟啉的溶剂（正庚烷）合物（ＴＴＯＭＰＰ·２Ｃ＿７Ｈ＿（１６））的晶体结构。实验表明，该化合物（Ｃ＿（７０）Ｈ＿（８６）Ｎ＿４Ｏ＿（１２））的晶体属三斜晶系，空间群Ｐ１，ａ＝８．７４９（６），ｂ＝１５．１２９（６），ｃ＝１６．４４９（３），ａ＝６０．０７（３），β＝７０．６４（４），γ＝８１．７０（５），Ｖ＝１７７９．６，Ｍ＿ｒ＝１１７５．４９，Ｚ＝１，Ｄ＿ｃ＝１．０９７ｇ／ｃｍ￣３，μ＝０．６９７ｃｍ￣（－１），Ｆ（０００）＝６３０。讨论了卟啉环上取代基的电子和立体效应及卟啉与铁（Ⅲ）离子配位后铁（Ⅲ）离于对卟啉结构参数的影响。     

双（取代环戊二烯基）二氯化锆的晶体结构分析

用Ｘ－射线晶体结构衍射法测定了双［１－苄基－１－乙基丙基环戊二烯基］二氯化锆［η５－Ｃ５Ｈ４Ｃ（Ｃ２Ｈ５）２ＣＨ２Ｃ６Ｈ５］２ＺｒＣｌ２（Ｉ）及（１，２－二异丁基－１，２－甲基－乙基桥联）双环戊二烯基二氯化锆［η５－Ｃ５Ｈ４Ｃ（ＣＨ３）（Ｃ４Ｈ９－ｉ）Ｃ（ＣＨ３）（Ｃ４Ｈ９－ｉ）Ｃ５Ｈ４－η５］ＺｒＣｌ２（Ⅱ）的结构。二者皆为单斜晶系，（Ｉ）的空间群为Ｐ２／ｎ，ａ＝１２．５８２（３），ｂ＝７．９９２（２），ｃ＝１４．９７９（３）Ａ，β＝１０１．６８（１）°，Ｖ＝１４７４．９（９）Ａ３，Ｍｒ＝６１２．８４，Ｚ＝２，Ｄｘ＝１．３８ｇ／ｃｍ３，μ＝５．６９ｃｍ（－１），Ｆ（０００）＝６４０，Ｒ＝０．０３３，Ｒω＝０．０３６。（Ⅱ）的空间群为Ｃｃ，ａ＝１３．３０９（３），ｂ＝９．５９１（１），ｃ＝１６．４４９（８）Ａ。β＝４．８３（３）°，Ｖ＝２０９．２（２）Ａ３，Ｍｒ＝４５８．６３，Ｚ＝４，Ｄｘ＝１．４５６ｇ／ｃｍ３，μ＝７．７７ｃｍ（－１），Ｆ（０００）＝９５２，Ｒ＝０．０５１，Ｒω＝０．０６１。化合物（Ｉ）以重叠式存在，两个苄基处于反式。晶体（Ⅱ）以交叉式存在，甲基、异丁基以反式构象存在。     

meso－5，10，15，20－四（3，4，5－三甲氧基苯基）卟啉的晶体和分子结构

用Ｘ－射线测定了ｍｅｓｏ－５，１０，１５，２０－四（３，４，５－三甲氧基苯基）卟啉的溶剂（正庚烷）合物（ＴＴＯＭＰＰ·２Ｃ＿７Ｈ＿（１６））的晶体结构。实验表明，该化合物（Ｃ＿（７０）Ｈ＿（８６）Ｎ＿４Ｏ＿（１２））的晶体属三斜晶系，空间群Ｐ１，ａ＝８．７４９（６），ｂ＝１５．１２９（６），ｃ＝１６．４４９（３），ａ＝６０．０７（３），β＝７０．６４（４），γ＝８１．７０（５），Ｖ＝１７７９．６，Ｍ＿ｒ＝１１７５．４９，Ｚ＝１，Ｄ＿ｃ＝１．０９７ｇ／ｃｍ￣３，μ＝０．６９７ｃｍ￣（－１），Ｆ（０００）＝６３０。讨论了卟啉环上取代基的电子和立体效应及卟啉与铁（Ⅲ）离子配位后铁（Ⅲ）离于对卟啉结构参数的影响。     

稀土（Ⅲ）（4＇－溴－5＇－硝基苯并－15－冠－5）配合物的制备与表征

在乙腈和丙酮介质中合成了６种轻稀土硝酸盐与４＇－溴－５＇－硝基苯并－１５－冠－５（Ｌ）的固体配合物，经元素分析确定其组成为ＲＥ（ＮＯ＿３）＿３·Ｌ（ＲＥ＝－Ｌａ～Ｎｄ），Ｓｍ（ＮＯ＿３）＿３·Ｌ·Ｈ＿２Ｏ和Ｅｕ（ＮＯ＿３）＿３·Ｌ·ＣＨ＿３ＣＮ·４Ｈ＿２Ｏ，并进行了ＩＲ、ＵＶ、ＴＧ－ＤＴＡ、摩尔电导及Ｘ－射线粉末衍射物相分析等表征，探讨了冠醚苯基上引入双取代基（－Ｂｒ，－ＮＯ＿２）后对稀土离子配位作用的影响．     

Synthesis and Structure of 6'-Diethylamino-2'-phenacylami nospiro-[isobenzofuran- 1 (3H), 9'- [9H]xanthen]-3-one

1mTRODUCTIONWehavereportedsomenuorancomPoundswithdifferentsubstitutedgroups"~'>.Thispaperdescribesacontinuationofourinvestigationonthenuoranderivatives.ThecrystalstructureofthecomPOundC,zHzsNzo'(I)(whereRl-NEt2,R2=H,R3=NHCHzCoCeHs,R`=H)wasdeterminedbyX-raydiffractionmethod.Inaddition,wealsocomparethetitlecomPOundwithotherfluorancomPounds.2EXPERIMENTAL2.1SynthesisAmixtureof2'-carboxy-4-diethylamino-2-hydrzophenoneandP-hydroxy-acetanilide(molarratio1:l)insulfuricacidwasheated…     

3,3-二甲基-9-(5,5-二甲基-3-羟基-2-环己烯-1-酮-2-基)-1-氧代-2,3,4,9-四氢化氧杂蒽的合成和晶体结构

标题化合物C23H26O4是由水杨醛与5，5-二甲基-1，3-环己二酮在N，N-二甲基甲酰胺中反应而得．结构通过单晶X-射线行射法确定，其晶体属于单料晶系，空间群P21/c，a=7．056（7），b=20.263（3），c=13．665（2）A，β＝93．32（1）°，V=1950．7（4）A3，Mr=366．46，Dc=1.248g／cm3，Z=4，μ（MoKa）=0．84cm－1，F（000）=784。晶体结构用直接法解出，经全矩阵最小二乘法对原子参数进行修正，最后的偏离因子R=0．068，Rw=0．075。晶体结构分析结果表明，分子中存在一个共轭的烯醇式结构。     

Syntheses and Crystal Structures of （S）-Methyl 2-（4-R-phenylsulfonamido）-3-（1H-indol-3-yl）propanoate （R = H （1） and Cl （2））

The title compounds （S）-methyl-2-（4-R-phenylsulfonamido）-3-（1H-indol-3- yl）propanoate （R = H （1）, Cl （2）） have been synthesized and their crystal structures also have been determined by X-ray single-crystal diffraction. Compound 1 （C18H18N2O4S） belongs to orthorhombic, space group P212121 with a = 9.6348（14）, b = 11.1517（17）, c = 16.412（3） A, V = 1763.4（5） A^3, Mr = 358.40, Z = 4, De = 1.350 g/cm^3,/t = 0.209 mm^-1, F（000） = 752, R = 0.0348 and wR = 0.0714. Compound 2 （CI8H17ClN2O4S） crystallizes in orthorhombic, space group P212121 with a = 9.3128（14）, b = 10.9655（16）, c = 17.783（3） A, V = 1815.9（5） A^3, Mr = 392.85, Z = 4, De = 1.437 g/cm^3, p = 0.352 mm^-1, F（000） = 816, R = 0.0389 and wR = 0.0845. The absolute structure Flack parameters X of compounds 1 and 2 are -0.03（8） and -0.06（7）, respectively. X-ray analysis reveals that the crystal structures of these two compounds both involve two intermolecular N-H…O hydrogen bond＇s.     

Synthesis and Crystal Structure of （Z）-1- （3-Fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4-methoxyphenyl）methyl）pyridin-2（1H）-one

The title compound （Z）-1-（3-fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4- methoxyphenyl）methyl）pyridin-2（1H）-one （C27H22F2N2O3,Mr = 460.47） was synthesized and crystallized. The crystal belongs to the triclinic system,space group P1 with a = 9.951（6）,b = 10.059（6）,c = 12.927（7）A,α = 109.828（7）,β = 102.304（7）,γ = 104.898（7）°,Z = 2,V = 1110.2（11）A^3,Dc =1.377 Mg/m^3,μ（MoKα） = 0.102 mm^-1,F（000） = 480,the final R = 0.0449 and Rw = 0.1250 for 4595 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that both m-fluorobenzyl groups are diorientationally disordered because of the rotation of C–C single bond which was represented as F（1）,F（2） and F（1＇）,F（2＇）. The diorientational disorder was refined and gave the occupancies of 0.665（4） and 0.335（4） for F（1） and F（1＇）,0.631（3） and 0.369（3） for F（2） and F（2＇）. Hydrogen bonds existing in the cell link different components to stabilize the crystal structure. The active data proved that the title compound has good anti-HBV activity.     

Synthesis,Crystal Structure and Prosperities of 10-（4,5-Dibenzylthio- 1,3-dithiol-2-ylidene）anthracen-9（10H）-one

The title compound 10-（4,5-dibenzylthio-1,3-dithiol-2-ylidene）anthracen-9（10H）- one （C31H22OS4） has been synthesized, and its crystal structure was prepared by crystallization from CH2Cl2-MeOH. The crystal belongs to the triclinic system, space group Pi with a = 10.9758（3）, b = 11.4241（4）, c = 11.7460（2）A^°, α = 62.379（2）, β = 81.227（3）, γ = 80.321（2）°, Mr = 538.73, V = 1281.69（7） A^°^3, Z = 2, Dc = 1.396 g/cm^3, F（000） = 560,μ = 0.395 mm^-1, the final R = 0.0291 and wR = 0.0739. The molecular structure is severely distorted from planarity. The central ring of anthraquinone moiety adopts a boat conformation, while the two outer benzene rings are tilted in the opposite direction to form a dihedral angle of 23.65°. The photocurrent generation was measured and an anodic photocurrent response was obtained. The electronic spectrum was studied by using TDDFr method on the basis of optimized geometries with B3LYP method. The obtained results are in good agreement with the experimental values.     

Synthesis and Crystal Structure of Ethyl 2-(6-(1,3-Dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) Butanoate

The title compound ethyl 2-(6-(1,3-dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate 3 was synthesized by the reaction of ethyl 2-(6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate with 4,5,6,7-tetraydrophthalic anhydride,and its structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 9.3469(2),b = 16.7715(5),c = 13.7153(4) ,β = 104.9680(10)°,μ = 0.107 mm-1,Mr = 430.42,V = 2077.08(10) 3,Z = 4,Dc = 1.376 g/cm3,F(000) = 904,T = 296(2) K,R = 0.0508 and wR = 0.1478.     

Synthesis, Crystal Structure and Antibacterial Activities of 3-[3-Methyl-（2-thienyl）methyl-enehydrazinocarbonyl]-（1H）-1,2,4-triazole

1 INTRODUCTION Azole derivatives, such as the derivatives of pyra- zole, imidazole, triazole including benzotriazole, te- trazole and indole, have extensive biological activi- ties. They have become the central focus of studies of agricultural chemicals, medicines, plant growth regulating agents and so on[1, 2]. Schiff bases also constitute a good type of biologically active sub- structures. Studies on pyrazole Schiff base-type fun- gicides have been reported[3, 4]. However, some struc- …     

Synthesis and Crystal Structure of （H3O）2[Cu3Cl3（H2O）3（NC9H12.5O6）2]

1 INTRODUCTION The polydentate ligand nitrilotripropionic acid, H3ntp[N(CH2CH2COOH)3], has attracted conside- rable research interest in constructing coordination polymers, designing organic-inorganic hybrid mate- rials[1], synthesizing supramolecular compounds[2], etc. due to its high degree of flexibility with three carboxylic acid moieties allowing for a variety of coordination through oxygen atoms[3]. It also pro- vides other versatile properties such as the possibili- ty of inter-…     

3-(9-芴甲氧羰基)四氢噻唑-2-硫酮的合成及其晶体结构

在吡啶存在下, 由9-芴甲氧羰酰氯与四氢噻唑-2-硫酮反应得到3-(9-芴甲氧羰基)四氢噻唑-2-硫酮, 产率为78.0%。用X射线衍射法测定晶体结构, 属正交晶系, Pca21空间群, 晶体学参数:a=0.9654(2), b=2.8032(1), c=0.6069(2)nm, Z=4。分子中的C=O与C=S基团处在C(3)-N-C(4)键的同侧, 为顺式结构。用PM3分子轨道方法研究该化合物的电子结构、电荷和键序分布、前线轨道性质。     

Synthesis and Crystal Structures of Two Novel Anionic Aluminophosphates: A One-Dimensional Chain, UT-7 ([Al(3)P(5)O(20)H](5-)[C(7)H(13)NH(3)(+)](5)), and a Layer Containing Two Cyclic Amines, UT-8 ([Al(3)P(4)O(16)](3-)[C(4)H(7)NH(3)(+)](2)[C(5)H(10)NH(2)(+)])

UT-7 and UT-8 (University of Toronto, structure numbers 7 and 8) are two novel aluminophosphate materials prepared under non-aqueous conditions. Their structures, extended in one and two dimensions, respectively, have been solved by single-crystal X-ray diffraction and characterized by a variety of methods including powder X-ray diffraction (PXRD), insitu high-temperature PXRD, thermogravimetric analysis (TGA), energy dispersive X-ray analysis (EDX), and scanning electron microscopy (SEM). UT-7 ([Al(3)P(5)O(20)H](5)(-)[C(7)H(13)NH(3)(+)](5), triclinic space group P&onemacr;, Z = 2, a = 10.118(3) ?, b = 15.691(4) ?, c = 18.117(3) ?, alpha = 72.91(2) degrees, beta = 85.18(2) degrees, gamma = 79.49(2) degrees ) is built of polymeric one-dimensional chain units, hydrogen-bonded into anionic layers that are charge-compensated by interlamellar cycloheptylammonium cations. UT-7 is isostructural to our previously discovered UT-3 chain structure, isolated in the analogous cyclopentylamine system. UT-8 ([Al(3)P(4)O(16)](3-)[C(4)H(7)NH(3)(+)](2)[C(5)H(10)NH(2)(+)], monoclinic space group P2(1), Z = 2, a = 8.993(4) ?, b = 14.884(8) ?, c = 9.799(9) ?, beta = 103.52(3) degrees ) is a two-dimensional net isostructural to several previously reported [Al(3)P(4)O(16)](3)(-) layers. The interlayer region of UT-8 is occupied by two different cyclic organic amine species, namely piperidinium and cyclobutylammonium. To our knowledge, this is the first report of the crystal structure of an aluminophosphate material containing cyclobutylammonium or a mixture of cyclic amines. Interestingly, UT-7 is observed to thermally transform in the solid state to an as yet unknown layered material that can be independently synthesized in a similar synthetic system. In the same way as UT-3 transforms to the UT-4 layered phase, we believe UT-7 transforms to a layered material by means of a chain to layer transformation.