CEYSTAL STRUCTURE OF EXTRACTED COMPLEX OF URANYL CHLORIDE WITH DICYCLOHEXYL-18-CROWN-6(MIXED ISOMERS),UO_2Cl_4]_3 [C_(20)H_(36)O_6- (ISOMER A)-H_3O]_4 [C_(20)H_(36)O_6(ISOMER B)-H_3O]_2

<正> Mr= 3584.7, monoclinic, P21/c, a = 14.647(2), b = 20.333(2), c = 25.759(3) A, β= 91.05(1)°, Z = 2, V = 7670.1 A3, Dc = 1.544 g/cm3,μ=32.629 cm-1, R=0.056 for 4207 observed reflections. Each asymmetric unit consists of two UO2Cl42- complex anions and three C20B36O6-H3O+ complex cations. In two of the complex cations (isosaer A), HaO+ cation is anchored in each crown ether ring by three stronger hydrogen bonds. In another complex cation (isomer B) only two stronger hydronger bonds are formed between the H3O+ cation and crown ether. The third hydrogen bond is very weak.     

CRYSTAL STRUCTURE OF Fe4S4[SC（CH3）3]4[（C4H9）4N]2

<正> Fe_4S_4[SC(CH_3)_3]_4[(C1H_9)_2,Mr=1193. 23,tetragonal,142d,a = 23. 272(2), c= 13. 080(5) A ,V=7084(3) A3,Z=4,DC=1. 12g·cm-3,UUUU(MoKa) = 10. 8cm-1,F(000) = 2568,R=0. 058 for 1005 observed reflections. The cluster anion contains a cubane-type Fe4S4 core compressed along the 4 axis which is crystallographically imposed. Compared to other salts with different cations ,the core is subject to slight structural distortions in different crystalline environments and crystallographic symmetry of the anion is related to that of the cation.     

CRYSTAL STRUCTURE OF BENZO-15-CROWN-5-POTASSIUM TETRAIODOINDATE(Ⅲ)

<正> K(C14H2oO5)2InI4, Mr =1198.16, triclinic,P1,a=ll.839(3), b=12.993(4), c= 14.774(6)A,α=107.87(3),β=109.25(3),γ=95.08(2)°,V=1996.1A3, Z=2, Dc=1.993g.cm-3, MoKa radiation, =0.71073A, F(000)=1136e, R=0.049 for 4381 observable reflections. The structure consists of complex cation K(B15C5)2+ and complex anion InI4-. In the cation, potassium ion lies between two ether oxygen planes of two benzo-15-crown-5 molecules. In the an-ion, indium atom is tetrahedrally coordinated by four iodine atoms.     

CRYSTAL AND MOLECULAR STRUCTURE OF N-CYANOMETHYL PH-THALIMIDE AND N-CYANOMETHYL SUCCIMIDE

<正> Diethylaminoacetonitrile (1) reacts with phthalimide (2) or succirnide (3) to produce N-cyanomethyl phthalimide (4) C10H6O2N2 (Mr = 186. 168) or N-cyanomethyl succirnide (5) C6H6O2N2(Mr= 138. 128),respectively. Their molecular and crystal structures were determined by IR, 1H NMR, MS and X-ray diffraction analysis, compound (4) crystallizes in monoclinic space group P21/a(P21/c) ,with cell dimensions 0=8. 225(4) ,6= 10. 956(4),c= 10. 041(5) A .β=102. 43(4)°,V=883. 1A3, μ= 0. 90cm-1, F (000) = 384, Z = 4; compound (5) crystallizes in monoclinic space group P1,with a=8. 404(2),b = 9. 710(2),c= 10. 093(2) A ,α= 104. 73(2)°,β = 108. 55(2)°, γ= 112. 03(2)°,V= 655. 2 A3,μ= 1.0cm-1 ,F(000) = 288,Z= 4. The average inner angles of the five-membered ring of (4) and (5) are about 108°. The imide and the carbon atom of the methylene radical of N-cyanomethyl and phenyl ring are all in one plane . so the bonds are delocalized and the α-hydrogen atoms of N-cyanomethyl are activated. The syntheses and crysta     

STRUCTURE OF NOVEL DICOPPER(Ⅱ) COMPLEX Cu_2 (oxpn) (NCS)_2 (H_2O)(oxpn=N,N''''-bis(3-aminopropyl) oxamido)

<正> C10H10Cu2N6O4S2,Mr = 475. 41,monoclinic,space group P2/c,a = 8. 531 (2),b= 6. 870(1) ,c= 14. 463(2) A ,β=93. 84 (2), V= 845. 7 A3,Z=2,D = 1. 866 g·cm-3,μ=27. 799cm-1,F(000) = 484,R=0. 071. The molecules possesse basically a planar structure ,with the two aquamolecules displaced 2. 75 A to opposite sides of this plane and being at the apexpositions of the square pyramidal coordination of the two Cu atoms, respectively, the two carbonyls of the oxamide show the "trans-form".     

STRUCTURE OF A NOVEL METHYLENE-BRIDGED TETRAPYRIMIDINIUM MACROCYCLIC COMPOUND (C_(24)H_(22)N_(12))·4C1·5H_2O

<正> Attempt to prepaie thiamine-metal complex resulted in a cyclic te-trapyrimidinlum tetrachloride. The retracationic macrocycle consists of four substituted pyrimidinium rings connected by methylene bridges. The cation interacts with two chloride anions at two sides of the macrocycle respectively, through the C-H....Cl hydrogen bonds and pyrimidinium ring-chloride electrostatic forces. Crystallographic data: (C24H32N12)4+·4Cl-·5H2O, Mr = 720. 49, monoclinic, C2/c, a = 10. 746 (5), b = 16.612(5), c=19. 263(4)A, β=100. 43(3)°,V = 3382(2)A3, Z = 4, Dv = 1. 41gcm-3, μ(MoKa) = 4. 1cm-1, F (000) = 1512, R = 0.057 for 1505 observed reflections (I>2σ(I)).     

CRYSTAL AND MOLECULAR STRUCTURE OF BENZO-15-CROWN-5 POTASSIUM TETRACHLOROAURATE K(C_(14)H_(20)O_5)_2-AuCl_4

<正> The crystal and molecular structure of the title compound K(C14 H20O5)2AuCl4 has been determined by X-ray diffraction method.The crystallographic data are as follows;Mr=914.51,triclinic,space group P1,a=10.988(2),b=13.472(4),c=13.696(2)A,α=77.72(1),β=79.02(2),γ=64.92(2)°,V=1782.6(4)A3,Z=2,Dc=1.704 g.cm-3,μ=45.858 cm-1,F(000)=454,R=0.019,Rw=0.018 for 5697 observed reflections with I≥3σ(I).X-ray structure determination shows that benzo-15-crown-5(B15C5)forms a 2:1 complex with KAu-C14 in which K+is sandwiched between two crown rings.The dihedral angle between these two ether oxygen planes is 11.9°.The anion AuCl4-has a planar square configuration which is bound with the complex cation K(B15C5)2+by electrostatic force to form an ion-pair.     

SYNTHESIS AND MOLECULAR STRUCTURE OF METHYL 1—BENZYL—6—PHENYLPIPERIDIN—2—ONE—5—CARBOXYLATE

<正> C20H21NO3,Mr=323.39,monoclinic, space group P21, a= 7. 338(2), b=15. 419(3),c=7. 515(1)A,β=95.98(1)°,V= 845. 7(2)A3,Dm(flotation in aq. KL)=1.267,Dx(Z=2)=1.270gcm-3,λ(MoKα)=0.71069A,μ=0.08cm-1,F(000)=344,T=295°K,final RF=0. 042 for 1651 observed reflections. The title compound was synthesized and established as the trans isomer, with the phenyl and carbomethoxy substituents occupying pseudo-axial and axial positions, respectively, of the piperidin-2-one ring in a half-chair conformation.     

CRYSTAL AND MOLECULAR STRUCTURE OF [K(C_(14)H_(20)O_5)_2]_2[Co(NCS)_4]

<正> The title complex (Mr= 1442.6) crystallizes in the monoclinic, space group PC, with a =14.515(7),b =15.773(5), c =16.287(11)51,β=95.13(5)°,Z=2,V=3713.8A3,Dc=1.29 g·cm-3. The structure was solved by Patterson method and the final R=0.068. The potassium atom in the cation lies between the two planes of the oxygen atoms from two benzo-15-crown-5 molecules.     

Synthesis,Crystal Structures and Antioxidant Activities of 1,5-Diketone Derivatives

A new transition-metal-free protocol for the synthesis of polysubstituted 1,5-diketone derivatives from readily available starting materials has been developed. All the compounds were confirmed by HRMS, ~1H NMR and ~(13)C NMR, and the single crystal structure of compound 4 f was determined to be of triclinic system, space group P1 with a = 8.6515(8), b = 8.6694(10), c = 12.4985(8) ?, b = 102.152(6)°, V = 895.43(15) ?~3, D_c = 1.625 g/cm~3, Z = 2, F(000) = 436, m(MoKα) = 1.807 mm~(-1), R = 0.0342 and w R = 0.0691. Furthermore, the result of antioxidation test demonstrated that compound 4 a exhibited better antioxidant activity than butylated hydroxytoluene and vitamin C by the ABTS+ radical cation decolorization assay. In addition, we further studied the mechanism of the transition-metal-free catalytic multicomponent domino reaction.     

Crystal Structure of Binuclear Oxomolybdenum(V), [Fe(H_2O)_6][Mo_2O_4(EDTA)]·5H_2O

1　ＩＮＴＲＯＤＵＣＴＩＯＮＡｌｔｈｏｕｇｈｔｈｅｂｉｎｕｃｌｅａｒｏｘｏｍｏｌｙｂｄｅｎｕｍ (Ｖ )ｃｏｍｐｏｕｎｄｓｏｆｅｔｈｙｌｅｎｅｄｉ ａｍｉｎｅｔｅｔｒａａｃｅｔａｔｅ (ＥＤＴＡ)ｃｈｅｌａｔｅｌｉｇａｎｄｗｅｒｅｗｉｄｅｌｙｓｔｕｄｉｅｄｄｕｒｉｎｇｌａｔｅｒ 50ｓ[1～ 4],ｔｈｅｆｉｒｓｔｓｕｃｈｃｒｙｓｔａｌｓｔｒｕｃｔｕｒｅｏｆｐｏｔａｓｓｉｕｍｓａｌｔｄｉｄｎｏｔａｐｐｅａｒｕｎｔｉｌ1 967[5 ],ａｎｄａｎ ｏｔｈｅｒｓｔｒｕｃｔｕｒｅｏｆｓｏｄｉｕｍｓａｌｔｗａｓｒｅｐｏｒｔｅｄｉ…     

CRYSTAL AND MOLECULAR STRUCTURE OF AuCSC(NH_2)_2]_2CiO_4 CONTAINING TWO-COORDINATE COMPLEX CATION

<正> Au [SC(NH2)2]2C1O4, Mr,= 448. 66, orthorhombic, Pcca, α= 17. 873 (2),b = 8. 2933(7), c = 7. 196(2) A V=1066. 6A3,Z=4,DC = 2. 794g·cm-3,R= 0. 049,Rw=0. 068 for 807 observed reflections. The structure consists of complex cation Au[SC(NH2)2]2+ and perchlorate ion ClO4-. The gold atom( I ) in the cation has a slightly bent linear coordination geometry.     

CRYSTAL STRUCTURES OF 1,2-BENZO[2.2]PARACYCLOPHANE AND 1,2-BENZO[2.2]PARACYCLOPHANE-1,7-DIENE

<正> C20H16 (1) Mr = 256.34 and C20H14 (2), Mr = 254.32 are isomorphous, orthorhombic, P212121, Z = 4. For (?), ?a= 7.116(1), b =7.874(2), c = 24.564(4) A, V = 1376.4(3) A3, Dx = 1.237 g cm-3, μ(Mo-K α) =0.65 cm-1 , final R = 0.047 for 1152 observed reflections; for 2, a=6.963(2), b = 7.985(4), c = 24.315(8) A, V = 1351.9(8) A3, Dx = 1.250 g cm-3,μ(Mo-Kα) = 0.66 cm-1 , final R = 0.076 for 886 observed data. Structuralfeatures are similar to those of the parent [2.2]paracyclophane and related derivatives.     

CRYSTAL STRUCTURE OF {Ni[(C_4H_9O)_2PS_2](C_(12)H_8N_2)_2} -[(C_4H_9O)_2PS_2]

<正> {Ni C(C4H9O)2PS2] (C12H8N2)2} [C(C4H9O)2PS2], Mr= 795. 60, Monocinic,P2,/n,a=16. 806(2), b=12. 720(2), c=21. 248(2) A. β=98. 454(7)°, V = 4493A3,Z=4,Dc= 1. 18g·cm-3,Mo Ka radiation,A=0. 71069A ,F(000) = 1664, R=0. 102 for 4154 reflections with I≥3σ(I).The crystal structure consists of complex cation {NiC(C4H9O)2PS2](C12H8N2)2}+ and complex anion C(C4H9O)2PS2]-. In the cation, nickel (Ⅱ) atom is coordinated by four nitrogen atoms and two sulfur atoms to form a distorted octahedron.     

CRYSTAL STRUCTURE OF [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.