CRYSTAL AND MOLECULAR STRUCTURE OF 1-PHENYL-3-METHYL-4-( 3' -PHENYL-1', 3' -ACEDION)-PYRAZOLONE-5

<正> A new 4-acetyl pyrazolone chelating agent C_(19)H_(16)N_2O_3 Mr=320. 348 has been synthesized. The molecular composition is different from β-Diketon and "Double β-Diketon". There are conjugated metiple bonds composed of three carbonyl groups in the molecule. A single crystal of approximate dimensions 0.1 × 0.2 × 0.5mm was mounted on an NICOLET R3M/E four-circle diffractomcter with graphite monochromated MoKa     

CRYSTAL AND MOLECULAR STRUCTURE OF 2-DIETHYLAMINO-1- p TOSYL-3-p CHLOROPHENYL 1,3,2-DIAZAPHOSPHOLIDIN-4-ONE

<正> 2-Diethylamino-l-p-tosyl-3-p-chlorophenyl-1, 3,2-diazaphospholidin-4-one was obtained by the reaction of P (NR2)s with p-tosylglycine p-chloropheny-lamide. Its crystal and molecular structure has been determined by X- ray diffraction method. The crystal C19H23ClN3O3PS is monoclinic with space group P21/c,a=8. 120,b= 11. 165(2),c= 23. 61 (6) A,β=96. 28(2) ,V = 2127. 8 A3,Z=4,Dx= 1. 289g/cm3, Mr = 415. 88,μ=3. 656cm-1,F(000) = 872,R = 0. 057,and RW=0. 070,The lone pair of eletrons of the nitrogen atom out of the ring and that of the phosphorus atom are predominantly in perpendicular conformation. The five-membered ring of 1-p-tosyl-3-p-chlorophenyl-l,3,2-diazaphospholidin-4-one is eventually coplanar.     

三(1-苯基-3-甲基-4-苯甲酰基-吡唑酮-5)二水合镱(Ⅲ)的晶体结构

本文合成了Yb(PMBP)₃(H₂O)₂,并用X-射线单晶衍射法测定了晶体和分子的结构.配合物的晶体为单斜晶系,空间群为P2₁/n,a=24.498(3)Å,b=14.735(3)Å,c=14.888(5)Å,β=101.14(2)Å,V=5285.1ų;Z=4.三个PMBP及两个水分子提供八个氧与镱配位形成四方反棱柱配位多面体.     

三(1-苯基-3-甲基-4-苯甲酰基-吡唑酮-5)二水合镱(Ⅲ)的晶体结构

本文合成了Yb(PMBP)_3(H_2O)_2,并用X-射线单晶衍射法测定了晶体和分子的结构.配合物的晶体为单斜晶系,空间群为P2_1/n,a=24.498(3)(?),b=14(?)35(3)(?),c=14.888(5)(?),β=101.14(2)(?),V=5285.1(?)~3;Z=4.三个PMBP及两个水分子提供八个氧与镱配位形成四方反棱柱配位多面体.     

STRUCTURE OF MOLECULAR COMPOUND CRYSTAL A_2B(A =1, 6, 7, 8,-TETRA-PHENYL (3, 4-BENZO)BICYCLO[4, 2, 0]OCTA-7-ENE, B=CIS, CIS-1,2,3,4,-TETRAPHENYLBUTADIENE)

<正> C100H78, (A: C36H28, B: C28H22) Mr = 1279. 74, monoclinic, P21/a, a=17. 282(3), b=10. 669(4), c= 19, 927(3) A , β =102. 99(1)°,V = 3580. 1(2) A3, Z=2, μ(MoKα) = 0. 623cm-1, F(000) = 1356, Dc=1. 187g/cm3, room temperature. The final R=0. 084, Rw = 0. 086 for 1255 independent observed reflections (I≥3σ(I)). Owing to the existence of 1,6,7, 8-Tetraphenyl (3,4-benzo)-bicyclo[4, 2, 0]octa-7-ene(A) , cis, cts-1, 2, 3, 4-Tetraphenylbutadiene (B) in A2B can take the different conformation from the one in the pure B crystal. The reason of the formation of this molecular compound crystal is put forward.     

CRYSTAL STRUCTURE AND POWDER DIFFRACTION OF Na5Y（WO4）4

<正> Title compound Na5Y (WO4)4 (Mr = 1195. 24) crystallizes in the space group I41/a with the cell parameters a= 11. 447(7), c= 11. 336(1) A , Z = 4, V = 1485(2) A3, A = 5. 34 g/cm3. A(MoKα) = 0. 71069 A. F(000) = 2702, final R = 0. 045,Rw = 0. 054 for 936 observed reflections with I≥3σ(I). The title compound has a scheelite structure.In this paper, we also give the X-ray powder diffraction data of Na5Y(WO4)4 obtained by using a D/max-ra type diffractometer.     

2-二乙氨基-3-(4''''-甲氧基苯甲酰基)-2-硫-1,3,2-氧氮磷杂环戊烷晶体结构研究

取代2-硫-1,3,2-氧氮磷杂环戊烷衍生物多为具有生物活性的含磷杂环化合物。其中,某些可作为杀虫剂、杀螨剂、阻化剂、抗病毒及抗肿瘤活性剂等等。文献报导了系列此类化合物的合成方法,为了进一步探讨环状含氧氮磷杂化合物的生物活性与结构的关系,本文报导标题化合物的晶体结构。     

CRYSTAL AND MOLECULAR STRUCTURE OF cis-ISOMER OF 1-N-PROPYL-3-iso-PHOPYL-2-PHENYL-4-ETHOXY-4,5-DIOXO-2-THIO-1,3,2,4-DIAZADIPHOSPHOLANE

<正> PhP(S)N(C3H5-i)-PO(OEt)CON(C3H5) Mr=358.34, monoclinic, space group P21/c, a=8.654(3), b=15.390(2), c=15.235(3)A,β=101.48(2)°;Z=4, Dx=1.20g/cm3, λ(No Kα)=0.71069A,μ=3.24cm-1. The final refinement converged with R=0.047 and Rw=0.051 for 1326 observed independent reflections.     

铕与PMBP配合物晶体结构和电子结构的研究

本文测定了 Eu(PMBP) 3 · 2 H2 O的晶体结构 ,该晶体属于单斜晶系 ,空间群 P2 1 / n,a=14 .982 1(1) ,b=14 .75 18(8) ,c=2 4 .4 979(9) ,β=10 1.5 2°,Z=4 ,V=5 30 2 .2 3 ,M=10 0 1.9,Dc=1.2 5 4 g/ cm3 ,μ=12 .315 cm-1 。 Eu与 PMBP及水中的 8个氧原子形成四方反棱柱配位多面体 ,根据选用的模型计算其电子结构 ,分子能量 ,净电荷分布和 Mulliken键级 ,进而讨论了配合物的结构和化学键的特征。实　验　部　分按 Eu(Cl O4) 3 · 2 H2 O中 Eu( )与 HPMBP摩尔比 1∶ 3反应 ,得到配合物固体。置于水与无水乙醇中 ,数周后…     

CRYSTAL AND MOLECULAR STRUCTURE OF 1.3-DI-ISO-PROPYL-2-PHENYL-4-METHOXY-4,5-DIOXO-2-THIO-1,3,2,4-DIAZADTPHOSPHOLANE

<正> The structure of the title compound has been determined by X-ray analysis. The crystals of this coiapound are monoclinic, space group P21/c with a=8.432(1),b=11.735(3),c=18.254(4)A,β=93.25(2)°,Z=4, and Dx=1.33 g/cm3. The final refinement converged with R=0.031 and Rw=0.031 for 1788 observed independent reflections.     

1-氧代-4(取代)-2,6,7-三氧杂-1-磷杂双环[2,2,2]辛烷晶体结构研究

具有双环笼状结构的磷酸酯类化合物的合成始于60年代。由于其分子呈高度对称的笼状结构及其衍生物具有很强的生物活性而且作用机理独特,引起人们普遍的关注。某些衍生物可用作杀菌剂,杀螨剂,除草剂,灭火剂,树脂稳定剂等等.由于此类化合物的生理作用机理不同于常用的有机磷农药.因此,可能会成为潜在的农药新途径。对此类化合物的晶体结构的测定,至今只有有限文献报导,为了研究其分子结构与化学性质及生物活性的关系,本文分析了四个磷氧杂双环磷酸酯类化合物的晶体结构,其合成方法已有报导。     

1-苯基-3-甲基-4-苯甲酰基吡唑酮-5稀土络合物的合成与表征

本文通过组成和物相分析证明按Roy和Okarfor的方法所合成的不是RE(PMBP)₃而是RE(PMBP)₃·HPMBP络合物。我们提出一种合成RE(PMBP)₃络合物的新方法,井用此法合成了45种稀土与HPMBP的固体络合物,对它们进行了组成分析,红外光谱和核磁共振谱等研究,其中有30种为新化合物。     

CRYSTAL AND MOLECULAR STRUCTURE OF A NOVEL Au Ag SUPRACLUSTER COMPOUND [Au_13Ag_12(μ-Br)_4(μ_3-Br)_2(Ph_3P)_10-

<正> [Au13Ag12(μ-Br)1(μ3-Br)2 (Ph3P)10Br2] Br, monoclinic. space group C2/m, a = 36. 496(17). b=16. 878(7), c-=19. 772(9) A , β=99. 87(5)°, V=11998. 9 A3.Z=2. The final R(Rw) is 0. 097(0. 109) for 3779 reflections with I>3σ(I). The structure can he considered as two icosahedral cluster units (AurAg6) sharing one vertex and linked hy six bromine atoms. The Au - Au, Au - Ag. and Ag-Ag distances fall in the ranges of 2. 69-2. 96. 2. 84-3. 02. and 2. 92-3. 26 A, respectively.     

CRYSTAL AND MOLECULAR STRUCTURE OF 1，2，3—TRIBENZOYLINDOLIZINE

<正> Crystal and molecujar structure of the title compound, C29H19NO3, was determined by single crystal X-ray diffraction analysis. .Mt=429. 48, monoclin-ic, space group P21/n, a = 10. 365 (3), b= 14. 614(4), c= 14. 857 (4) A ,β= 103.55(2)°,V=2186. 1(10) A3, Z=4, Dc= 1. 30g/cm3,μ(MoKa) = 0. 81cm-1, F (000) = 919. 87. Final residual R value was 0. 0704 and Rw = 0. 0704. The indo-hzine ring is conjugated only with the 1-benzonyl group.     

PMBP与中性磷萃取剂对铽(Ⅲ)的协同萃取

本文研究了1-苯基-3-甲基-4-苯甲酰基吡唑啉酮-5(PMBP)与丁基膦酸二丁酯(DBBP)或磷酸三丁酯(TBP)的氯苯溶液在硝酸介质中对铽(Ⅲ)的协同萃取。测得了萃合物的组成及其萃取平衡常数,讨论了萃合物的可能结构式及协同萃取机理。     

CRYSTAL AND MOLECULAR STRUCTURE OF 2-PHBNYLQUINOXALINE

<正> C14H10N2,Mr =206.24, space group P21/n, a =5.861(3), b =10.230 (5), c =17.440(11) A,β=92.07(5)°,V= 1045(1) A3,Z=4, Dx=1.31 g.cm-3, MoKa radiation,u=0.73 cm-1,F(000)=432,R=0.063 for 1054 observed reflections. 2-Phenylquinoxaline molecule is approximately planar. The dihedral angle between the quinoxaline ring and the substituted phenyl ring is 7.0°. The C-C bond distance connecting these two rings is 1.495(4) A. The whole molecule is a conjugation system.     

三(1-苯基-3-甲基-4-三氟乙酰基-吡唑啉酮-5)二(三苯基氧化膦)合钕(Ⅲ)协萃配合物晶体和分子结构

标题化合物单晶由溶液法合成,呈紫红色,用X—射线衍射法测定了晶体及分子结构。晶体属于三斜晶系,空间群P_(?)(No.2),晶胞参数为a=12.880(4),b=13.649(7),c=21.670(5)(?),α=93.14(3),β=91.63(2),γ=115.99(4)°,最终偏离因子R=0.089 R_w=0.091。     

CRYSTAL STRUCTURE OF 2-METHYL-3-PHENYLACRYLOYL-QUINOXALINE 1,4-DIOXIDE

<正> C18H14N2O3,Mr=306. 32,Monoclinic,P21/b,a = 5. 579(1),b = 8. 963 (2),c = 29. 405(7) A,γ= 92. 62(2)°,V= 1468. 8(7) A3.Z=4, Dx= 1.385 gcm-3, CuKa radiation, μ= 7. 45 cm-1,F(000) = 640,final R= 0. 039,Rw= 0. 045 for 1006 observed (I>3σ(I)) reflections. The quinoxaline part of the molecule is virtually planar. The dihedral angle between the benzene ring of the phenylacryloyl and quinoxaline ring is 99. 6°.     

CRYSTAL AND MOLECULAR STRUCTURE OF SUEFATOAQUO-2, 3-DIMETHYL-2, 3-BUTYLDIAMINEPLATINUM

[PtDMBA(SO4)H2O]H2O crystals belong to the orthorhombic system,a=11.073(3),b=9.672(2),c=21.156(7)A,space group C2cb,z=8.The diffraction data (Moka) were collected with Nicolet R3 four-circle di-ffractometer.The structure was determined by heavy atom method and refined by the least square program,R=0.0716.In the systematic study of anticancer action of a series of platinum compounds,our Coordination Chemistry Research Institute has synthesized PtDMBASO4 2H2O(where DMBA=2,3-dimethyl-2,3-butyldiamino) and found it has antitumor activity against L-1210 in mice.In order to study the relationship between the structure and the anticancer effects of the platinum compounds,the crystal structure of the compound has been determined.     

CRYSTAL STRUCTURE OF A TRINUCLEAR COBALT COMPLEX Co_3(bdt)_3(PBu_3~n)_3 · ~2CH_2C1 (bdt = S_2C_6H_4~2- ) WITH MIXED o-BEN-ZENEDITHIOLATE AND TRIBUTYLPHOSPHINE LIGANDS

<正> Co3(S2C6H4)3{P(C4H9)3}3 ·2CH2Cl2, Mr = 1373. 45, mono-clinic, space group P21/c, a = 16. 110(5), b=36.313(10), c=13. 502(5) A , β= 105. 69(4)% V=7604. 4 A3, Z = 4, Dc = 1. 20 g. cm-3, μ=10. 03 cm-1, and F (000) = 2990. R(Rw) is 0. 086(0. 091) for 4559 observed unique reflections. The three cobalt atoms in the complex form an isosceles triangle with an average Co -Co bond distance of 2. 504(5) A. The average values of Co - S and Co - P bond distances are 2. 271(7) A , and 2. 198(8) A , respectively.