联苯甲酰双缩氨基脲硝酸钕水合物晶体结构的测定

联苯甲酰双缩氨基脲硝酸钕水合物分子式为[Nd（C16H16N6O2）（NO3）3（H2O）]·H2O，Mr＝690．2，正交晶系，空间群为Fdd2，晶胞参数，利用2312个可观测衍射进行结构修正，最后R＝0.048。晶体中含有2个水分子，其中1个参加配位。3个硝酸根呈双齿配应；有机配体中有2个N原子和两个O原子参与配位，Nd的总配位数为11。     

Crystal and Molecular Structure of Hexahydro-2-(Nitro-Benzoylmethylene)Pyrimidine

1INTRODUCTIONHeterocyclicketeneaminalsareversatilestartingmaterialsforthesynthesisofawidevarietyofnewheterocyclesandfusedheterocycles.Thus,thesynthesisandre-actionofheterocyclicketeneaminalshavegivenrisetomuchattention[18i.Recentlynitrationofheterocyclicketeneaminalswasstudied[9i.Wehavepreparedhexahydro-2-(nitro-benzoylmethylene)pyrimidi(1).ItscrystalstructurehasbeendeterminedbyX-raydiffractionmethodandthemolecularstructureisdiscussed.2EXPERIMENTALThesinglecrystalofhexahydro-2-(nitr…     

Synthesis and Crystal Structure of a Zinc(II) Complex Salt with the Schiff Base of Picolinaldehyde N-oxide and Semicarbazone

1 INTRODUCTION The donor properties of pyridine N-oxide and its substituted derivatives to form metal complexes have been widely investigated[1～3]. The resulting comple- xes were used as drugs[4] and catalysts[5]. So far, there have been a few reports on the synthesis of Schiff base derived from picolinaldehyde N-oxide with se- micarbazone (PNOS Scheme 1) and its metal com- plexes. And crystal structures of the complexes of PNOS with Au(III)[6], Pd(II)[7] and Cu(II)[8] were re- …     

Synthesis and Crystal Structure of a Zinc(Ⅱ) Complex Salt with the Schiff Base of Picolinaldehyde N-oxide and Semicarbazone

The title zinc(Ⅱ) complex salt [Zn(H2O)6](ClO4)2·(PNOS)4, where PNOS is derived from picolinaldehyde N-oxide with semicarbazone, has been prepared and structurally characterized by X-ray single-crystal analysis. It crystallizes in triclinic, space group P1 with a = 7.529(3),b = 10.206(4), c = 14.678(6) A, α = 86.293(6), β = 87.686(7), γ= 81.382(6)°, C28H44Cl2N16O22Zn,Mr = 1093.06, V= 1112.3(8) A3, Z = 1, Dc = 1.632 g/cm3, S = 1.089,μ(MoKα) = 0.773 mm-1 ,F(000) = 564, the final R = 0.0438 and wR = 0.1076 for 3888 independent reflections with Rint =0.0224. The crystal structure possesses a [Zn(H2O)6]2+ cation, two ClO4- anions and four PNOSs.In the crystal structure, Zn2+ cation is located at the symcenter and coordinated by six water molecules. In [Zn(H2O)6]2+, an elongate octahedral complex cation, the average Zn-O bond length is 2.087(2) A. There exist a lot of H bonds in the structure, linking the cation [Zn(H2O)6]2+, anion ClO4-and PNOS to form a 3D network.     

Molecular and Crystal Structure of 4-Amino-4'-Nitrodiphenyl Ether

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｏｒｇａｎｉｃｓｅｃｏｎｄｏｒｄｅｒｎｏｎｌｉｎｅａｒｏｐｔｉｃａｌ(ＮＬＯ)ｍａｔｅｒｉａｌｓｈａｖｅｂｅｅｎｐａｉｄｍｏｒｅａｎｄｍｏｒｅａｔｔｅｎｔｉｏｎｓｂｅｃａｕｓｅｏｆｔｈｅｉｒｉｍｐｏｒｔａｎｔａｐｐｌｉｃａｔｉｏｎｓｉｎｏｐｔｏｅｌｅｃｔｒｏｎｉｃｓｔｅｃｈｎｏｌｏｇｙｆｉｅｌｄｓ.[1～3]Ｔｈｅｉｒｓｅｃｏｎｄｈａｒｍｏｎｉｃｇｅｎｅｒａｔｉｏｎ(ＳＨＧ)ｅｆｆｉｃｉｅｎｃｉｅｓｕｓｕａｌｌｙｅｘｃｅｅｄｔｈｏｓｅｏｆｃｏｍｍｏｎｌｙｕｓｅｄｉｎｏｒｇ…     

Crystal Structure of iso-propylcyclopentadienylchloro-(bistriphenylphosphine) ruthenium

１　ＩＮＴＲＯＤＵＣＴＩＯＮＣｙｃｌｏｐｅｎｔａｄｉｅｎｙｌｃｏｍｐｌｅｘｅｓｈａｖｅｂｅｅｎｉｎｔｅｎｓｉｖｅｌｙｓｔｕｄｉｅｄｆｏｒｔｈｅｉｒｒｉｃｈｃｈｅｍｉｃａｌａｎｄｃａｔａｌｙｔｉｃｐｒｏｐｅｒｔｉｅｓ〔１〕．Ｉｔｈａｓｂｅｅｎｗｅｌｌｅｓｔａｂｌｉｓｈｅｄｔｈａｔｔｈｅｒｅｐｌａｃｅｍｅｎｔｏｆａｎη５－ｃｙｃｌｏｐｅｎｔａｄｉｅｎｙｌｌｉｇａｎｄｂｙａｎη５－ｐｅｎｔａｍｅｔｈｙｌｃｙｃｌｏｐｅｎｔａｄｉｅｎｙｌｌｉｇａｎｄｉｎｔｒａｎｓｉｔｉｏｎｍｅｔａｌｃｏｍｐｌｅｘｅｓｒｅ…     

2－（1，3－亚丙二硫基）亚甲基环己酮的晶体结构

报导了标题化合物Ｃ_（１０）Ｈ_（１４）ＯＳ_２（Ｍ_ｒ＝２１４．３５）的晶体结构，该晶体属正交晶系，空间群为Ｐ２_１２_１２_１，晶胞参数为ａ＝６．４４３（３），ｂ＝８．９８０（４），ｃ＝１８．２１３（７）；Ｖ＝１０５３．８（６）３；Ｚ＝４，Ｄ_ｘ＝１．３５ｇ／ｃｍ~３，Ｆ（０００）＝４５５，μ＝４．５ｃｍ~（－１）（ＭｏＫａ）。最终偏离因子Ｒ＝０．０３３，Ｒ_ｗ＝０．０３４。分子中的两支Ｃ_（ｓｐ）２－Ｓ键键长近于相等，分别为１．７６１（３）和１．７６９（３），Ｃ（１）－Ｃ（５）键长为１．３６１（４）。     

2－（1，3－亚丙二硫基）亚甲基环己酮的晶体结构

报导了标题化合物Ｃ_（１０）Ｈ_（１４）ＯＳ_２（Ｍ_ｒ＝２１４．３５）的晶体结构，该晶体属正交晶系，空间群为Ｐ２_１２_１２_１，晶胞参数为ａ＝６．４４３（３），ｂ＝８．９８０（４），ｃ＝１８．２１３（７）；Ｖ＝１０５３．８（６）３；Ｚ＝４，Ｄ_ｘ＝１．３５ｇ／ｃｍ~３，Ｆ（０００）＝４５５，μ＝４．５ｃｍ~（－１）（ＭｏＫａ）。最终偏离因子Ｒ＝０．０３３，Ｒ_ｗ＝０．０３４。分子中的两支Ｃ_（ｓｐ）２－Ｓ键键长近于相等，分别为１．７６１（３）和１．７６９（３），Ｃ（１）－Ｃ（５）键长为１．３６１（４）。     

Crystal and Molecular Structure of Quinide

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆＱｕｉｎｉｄｅＷＡＮＧＧａｎｇ－Ｌｉ；ＺＨＡＯＳｈｕ－Ｊｉｅ；ＣＨＥＮＤｅ－Ｃｈａｎｇ（ＮａｔｉｏｎａｌＩｎｓｔｉｔｕｔｅｆｏｒｔｈｅＣｏｎｔｒｏｌｏｆＰｈａｒｍａｃｅｕｔｉｃａｌａｎｄＢｉ...     

Crystal and Molecular Structure of Cyanuric Acid

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆＣｙａｎｕｒｉｃＡｃｉｄＣｈｅｎＣｈａｎｇ－Ｚｈａｎｇ；ＳｈｉＪｉａｎ－ＱｉｕＬｉｎＺｈｏｕ－Ｂｉｎ；ＧａｏＤｏｎｇ－Ｓｈｏｕ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ；ＬｉＤｉｎｇ（ＦｕｊｉａｎＩｎｓ...     

Photocycloaddition of （4－methyl－7－coumarinyl） Oxyacetic Acid Propanediol Diester and X－ray Crystal Structure of Product

Ｐｈｏｔｏｃｙｃｌｏａｄｄｉｔｉｏｎｏｆ（４－ｍｅｔｈｙｌ－７－ｃｏｕｍａｒｉｎｙｌ）ＯｘｙａｃｅｔｉｃＡｃｉｄＰｒｏｐａｎｅｄｉｏｌＤｉｅｓｔｅｒａｎｄＸ－ｒａｙＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＰｒｏｄｕｃｔＤｕＤａ－Ｍｉｎｇ；ＷａｎｇＹｏｎｇ...     

Crystal and Molecular Structure of OMPCTF

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆＯＭＰＣＴＦＷａｎｇＲｕｉ－Ｙａｏ；ＪｉｎＺｈｏｎｇ－Ｓｈｅｎｇ（ＬａｂｏｒａｔｏｒｙｏｆＲａｒｅＥａｒｔｈＣｈｅｍｉｓｔｒｙａｎｄＰｈｙｓｉｃｓ，ＣｈａｎｇｃｈｕｎＩｎｓｔｉｔｕｔｅｏｆＡ...     

Molecular and Crystal Structure of Cinnam ylidene Acetophenone

１　ＩＮＴＲＯＤＵＣＴＩＯＮＣｕｒｒｅｎｔｌｙ，ｃｏｎｓｉｓｔｅｎｔｅｆｆｏｒｔｓｈａｖｅｂｅｅｎｍａｄｅｔｏｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｆｏｒｇａｎｉｃｎｏｎｌｉｎｅａｒｏｐｔｉｃａｌ（ＮＬＯ）ｍａｔｅｒｉａｌｓ〔１〕．Ｓｏｍｅｏｆｃｉｎｎａｍｙｌｉｄｅｎｅａｃｅｔｏｐｈｅｎｏｎｅｄｅｒｉｖａｔｉｖｅｓｈａｖｅｆａｉｒｌｙｓｔｒｏｎｇｓｅｃｏｎｄｈａｒｍｏｎｉｃｇｅｎｅｒａｔｉｏｎ（ＳＨＧ）ａｎｄｔｈｅｒｅｆｏｒｅａｒｅｐｏｔｅｎｔｉａｌｕｓｅｆｕｌｉｎＮＬＯｆｉｅｌｄｓ．Ｄｕｒｉｎ…     

铌取代型杂多钨酸盐的合成、表征、生物活性及晶体结构

合成了铌、过氧化铌取代的钨硅、钨锗杂多配合物M     

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。     

Crystal Structure of Derivative of H_4′-NOBIN and the Applications in Hetero-Diels-Alder Reaction

Novel Schiff bases of H4′-NOBIN 5a and 5b were synthesized by condensation of 3 with aldehydes. Compound 5b was structurally characterized by single-crystal X-ray diffraction. The asymmetric hetero-Diels-Alder reactions were carried out with high yields and good enan-tioselectivities in the presence of Ti-(S)-5a complex as catalyst. Crystallographic data for 5b: C27H22BrNO, Mr = 456.37, triclinic, space group P1 with a = 9.1618(2), b = 10.3836(2), c = 12.7718(2), α = 105.4860(10),β = 94.6360(10), γ = 108.4610(10)o, V = 1092.32(4)3, Z = 2, Dc = 1.388 g/cm3, μ = 1.900 mm-1, F(000) = 468, R = 0.0476 and wR = 0.1248 for 3092 observed reflections (Ⅰ > 2σ(Ⅰ)).     

含吡唑啉酮氨基脲类化合物的合成及结构

以1-苯基-3-甲基-吡唑啉酮-5 (PMP)和1,3-二苯基-吡唑啉酮-5 (DPP)为原料合成了六种4-酰基吡唑啉酮,并分别与氨基脲缩合,得到六个新的含吡唑啉酮环的缩氨基脲类化合物.用IR, ¹H NMR和¹³C NMR对各化合物进行了表征及结构确证,并用X射线单晶衍射法测定了化合物1c [1-苯基-3-甲基-4-丙酰基-吡唑啉酮-5缩氨基脲(PMPP-SC)]的晶体结构.     

反,反-2-氨基-1,3,3-三氰基-5-硝基-4,6-二对甲苯基环己烯的合成和晶体结构

标题化合物C23H19O2N5 (Mr=397.44)是由对甲苯基亚甲基丙二腈与硝基甲烷在N,N-二甲基甲酰胺(DMF)中反应而得。结构通过单晶X-射线衍射分析确定,其晶体属于单斜晶系,空间群P21/a,a=12.712(2),b=13.071(4),c=13.368(2),b=106.37(1), V=2131.2(8)?,Dc=1.239g/cm3, Z=4, m (MoKa)=0.82cm-1, F(000)=832。R=0.056。结构显示六员环上的对甲苯基与硝基处于反式,说明该加成反应具有立体选择性。     

Synthesis, Crystal Structure and Electrochemical Properties of a Novel Phenothiazine Derivative

A new compound 1,1‘-bis(3-pyridyl)-propylene(3,7-diformyl-N-ethylphenothiazinyl)ketone (C30H23N3O2S, Mr = 489.4) has been synthesized, and its crystal structure was determined by single-crystal X-ray diffraction method. The crystal is of orthorhombic, space group Ima2 with a = 27.491 (5), b = 11.942(2), c = 7.389(2) A, V = 2425.8(7) A^3, Z = 8, Dc =1.340 g/cm^3,μ = 0,167 mm ^1, F(000) = 1024, the final R = 0.0363 and wR = 0.0869 for 2054 unique reflections with Rint = 0.0254. The structural determination shows that the molecule assumes a butterfly configuration with nearly planar wings. In addition, the electrochemical study indicates that there is a high electronic delocalization in the molecule.     

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）。