CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.     

Synthesis,Structure Characterization and Biological Activity of a Novel Amino Acid Salt(HAla)_8(H_3O)_(10)[PMo_(12)O_(40)]_6·22H_2O

A novel compound was synthesized and characterized by means of elemental analysis, IR and UV spectra, TG, CV and single crystal X-ray diffraction. The compound crystallized in an orthorhombic space group C222 with a = 1. 622 4(3) nm, b=3. 498 4(7) nm, c=l. 301 5(3) nm,V=7. 387(3) nm3, Z = 6, R1 = 0. 037 3, wR2 = 0. 114 0. The Ala (Ala = alanine) molecules were protonated at the amino nitrogen N (1) and the C (2) of Ala group with the terminal oxygen atom O(15), O(14), O(26) and O(27) of the polyoxometalates participating in the hydrogen bond network. The anti-tumor activity of the title compound was estimated against Hela and Pc-3m cancer cells.     

The Syntheses and crystal structures of trans-dichlorobis (10-thiabenzo-15-crown-5)-palladium(Ⅱ)and trans-dichlorobis-(10-selenabenzo-15-crown-5)palladium(Ⅱ)

The preparation and X-ray crystal structures of the adducts of 10-thiabenzo-15-crown-5 and 10-selenabenzo-15-crown-5 with PdCl2 are reported. [PdCl2(C14H20O4S)2] (1): or-thorhombic, space group Pbca with cell dimensions of a=17.285(5), 6=8.354(3), c=21.689(4) A, K=3131.9 A3, Z=4;R=0.0330 for 2301 reflections with I > 3o(I), [PdCl2(C14H2oO4Se)2] (2): monoclinic, space group P21/n with cell dimensions of a=18.928(4), b=8.912(3), c=9.813(2) A, β=96.90(2)0, V=1643.4 A3, Z=2; R=0.0289 for 2617 reflections with I> 3σ(I), Both complexes are monomeric, square-planar palladiurn(Ⅱ) compounds with the Pd(Ⅱ) ion situating on a crystal-lographic inversion centre, and the crown ligands all adopt the axial coordination with the Pd-S bond of 2.3233(7) A and the Pd-Se bond of 2.4357(3) A. Their complexing characteristics are discussed in brief.     

Synthesis and Crystal Structure of Sodium Monosulfuron (N-(4-Methylpyrimidin-2-yl)-N'-2-(nitrophenylsulfonyl) Urea Sodium)

Monosulfuron is a novel sulfonylurea herbicide with ultra-low dosage invented and patented by Nankai University.Herein its sodium salt was firstly synthesized and crystal structure was determined by X-ray diffraction method.The title compound belongs to the triclinic system, space group P1- with a = 7.306(6), b = 9.446(8), c = 11.872(10)(A), α= 76.578(14), β= 78.049(13), γ= 77.620(14)°, V = 767.7(11)(A)3, Mr = 377.32, Z = 2, Dc = 1.632 g/cm3,μ= 0.283 mm-1, F(000) = 388, R = 0.0444 and wR = 0.1186.In the title compound, Na(1) coordinates with O(4) and O(5) from one monosulfuron molecule, N(4A) and O(5A) from the other monosulfuron molecule and the oxygen atom from H2O to give five coordination bonds.The title complex is further linked into a three-dimensional structure through π…π interactions and intermolecular hydrogen bonds between the oxygen and nitrogen atoms.     

Synthesis and Crystal Structure of Metronidazole-derived Compound

A MET-OH derivative,MET-OTs 1,was designed,prepared and structurally charac-terized by single-crystal X-ray diffraction. X-ray structure analysis reveals that 1 crystallizes in the monoclinic system,space group P21/c,with a=16.1178(14),b=7.5473(6),c=13.4161(11),V= 1520.3(2)3,β=111.3210(10)o,Z=4,Dc=1.421 g/cm3 and F(000)=680.     

SYNTHESIS AND STRUCTURE OF EUROPIUM (Ⅲ) WITH N,N'''' BISSALICYLIDENE ETHYLENEDIAMINE (H_2salen)

<正> A europium (Ⅲ) complex with N, N' - bissalicylidene-ethylenediamine (H2salen) has the formula Eu(Hsalen)(salen)4H2O,where water molecules are in the outer sphere and do not coordinate with Eu (Ⅲ), was synthesized and structurally studied. The central atom Eu is coordinated by four nitrogen atoms and four oxygen atoms in a deltadodecahedron arrangement. The crystal is monoclinic,space group P21/a with cell constants a=16. 441(2),b=20. 599(3),c=10. 719(2) A ,β=84. 16(1)°,Z=4 and V = 3611. 5(8) A3,Dc=1. 392g/cm3.The final standard deviation R is 0. 093.     

THE CTYSTAL STRUCTURE OF m—FERROCENYLACETOOHENONE

<正> The title compound C18H16FeO (Mr=304. 17) crystallizes in the mono-clinic system,space group P21/c with cell constants a= 14. 428(3),b=9. 939(8),c = 10. 027(5) A .B=93. 73(1),Z=4,Dc=1.41 gcm-3 and V= 1435. 0A 3.The structure is solved by direct methods and refined by least-squares technique to final R=0. 038 and Rw=0.051 based on 2413 independent reflections with I>3o(I). Result shows that both the Cp rings are approximately parallel with dihedral angle of 1. 2 ,The phenyl ring is somewhat tilted from the Cp ring linked to it with a dihedral angle of 8. 36 . The oxygen and carbon atoms of the aceto group are almost co-planar with the phenyl ring.     

CRYSTAL STRUCTURE OF p—PROPIONYLCALIX [4]ARENE

<正> The title compound was synthesized by Friedel-Crafts reaction of tetrahydroxycalix [4] arene and propionyl choride, and its crystal structure was determined by X-ray diffraction technique. C10O8H40,Mr = 648. 75, triclinic, space group P1 with cell parameters, a = 9. 930(5), b = 11. 838(3), c=14. 522(7) A,α= 94. 92(3),β=102. 96(4),γ= 98. 32(3)°, V = 1635A3, Z = 2, Dc = 1. 399g/ cm3, μ(CuKa) = 3. 27cm-1, F (000) = 344. The final R = 0. 075, Rw = 0.092 for 5716 independent reflections with I>3σ(I). The crystal structure analysis shows that the molecule exists in fine cone conformation.     

Synthesis, Crystal Structure and Fluorescene of a One-dimensional Compound {CdI2（2,2＇-bipy）}n

The title compound, {CdI2(2,2'-bipy)}n, was prepared by the hydrothermal reaction of CdI2 and 2,2'-bipy in an aqueous solution, and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: C10H8N2CdI2, monoclinic system, space group C2/c, a = 16.927(1), b = 10.0925(7), c = 7.7422(3) (A), β = 106.0629(4)°, V = 1271.00(14)(A)3, Z = 4, F(000) = 944, μ = 6.546 mm-1, Dc= 2.730 g/cm3, Mr = 522.38, the final R = 0.0309 and wR = 0.0805 for 1310 observed reflections (I＞2σ(Ⅰ)). X-ray crystal structure analysis shows that the Cd atom is coordinated by four iodines and two N atoms from one 2,2'-bipy to form an 1-D chain-like structure through bridging iodines. The fluorescene of the title compound was also discussed.     

SYNTHESIS AND CRYSTAL STRUCTURE OF (β-PHENYL) CAR-BOXYLETHYLTRICHLOROGERMANIUM

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1,a=8. 450(4),b=11. 730(3),c=14. 718(6)A ,α=104. 50(3),β=103. 71 (4),γ=69. 20(3)°,Z=4,V=1302. 4(9) A3,Dc,= 1.67g/cm3, λ(MoKa) = 0. 71069 A ,μ=30. 7/cm,F(000) = 646,Mr = 327. 6,final R=0. 037 for 2198 reflections with I<3σ(I). There are two molecules of different conformation in an asymmetric unit. Atom Ge is coordinated by three chlorine atoms and one carbon atom to form an irregular tetrahedron.     

Decomposition of benzenediazonium fluoborate in esters of α,β-unsaturated acids

Summary It was shown that In contrast to the Meerwein-Koelsch reaction, the decomposition of benzenediazonlum fluoborate In esters of ,-unsaturated acids proceeds by a heterolytlc mechanism with the phenyl attacking the -carbon and the carbalkoxyl group of these esters. The reaction with ethyl crotonate gave -methylatropic acid (after hydrolysis) and a small amount of a dibasic acid, C₁₄H₁₆O₄ (or C₁₄H₁₄O₄). With methyl acrylate it gave atropic acid, phenyl acrylate, and a smaller amount of -methyl--phenylglutaric acid. With methyl methacrylate It formed benzylacrylic acid and the product of further conversions of phenyl methacrylate, namely the keto phenol 2-methyl-5-hydroxyindan-1-one.     

High-sensitivity spectrophotometric determination of trace amounts of Levodopa, Carbidopa and α-Methyldopa

Summary A simple, sensitive and accurate spectrophotometric method for the determination of Levodopa (LVDA)(I), Carbidopa (CBDA)(II) and -Methyldopa (-MDA)(III) at the ppb level has been developed. This method is based on the oxidation of (I), (II) and (III) by Fe(III), using a Fe(III)-o-Phenanthroline mixture and is followed by the formation of a highly stable orange-red coloured tris-complex [Fe(II)-(o-Phenanthroline)₃]²⁺ in a moderate acidic medium (pH=5.0±0.2) which exhibits an absorption maximum at =510 nm. The apparent molar absorptivities were 1.26×10⁵, 1.02×10⁵ and 1.29×10⁵ l mol^–1 cm^–1 and the Sandell's sensitivities were 1.57, 2.20 and 1.60 ng cm^–2 for (I), (II) and (III), respectively. Beer's law is obeyed in a concentration range from 50 to 2500 ppb for (I) and (III) and from 100 to 4000 ppb for (II). The slope and the intercept of the regression lines for each of these drugs were calculated with correlation coefficients of 0.9999 for (I) and (III) and 0.9998 for (II). The results obtained from the determination of the drugs studied, using both the described procedure and the corresponding official method, were statistically compared by means of the Student's t-test and by the variance ratio F-test, and no significant difference was observed.     

Studies on Selena-Macrocyclic Amides Synthesis and Structural Characterization of 7-Phenyl-5, 9-dioxo-1-selena-4, 7, 10-triazacyclododecane and 6-(4-Nitrobenzyl )-5, 9-dioxo-1, 4, 7, 10-selenatriazacyclododecane

lmTR0DUCTI0NSincetheseleniumcoronandswereachivevedin1989tli,thesynthesisandcoor-dinationchemistrystudyofthismacrocycliccomPOundshavereceivedwideattentionowingtotheirstrongcomplexingabilitiestowardssoft.transiti0nandheavymetals.InourprevibuspaPer,wereP0rtedthecrystalstructureoftw0selenacrownethers(2'3)andaPd(1)complexwith10'selenabenzo-15-crown-5t4i.Duetothedifficultyofthepreparationsofselenium-nitr0genmixeddonorc0n-..tainingmacrocycles,thestudyontheseligandsisconsiderablyscarce.Thesynthes…     

SYNTHESIS AND CRYSTAL STRUCTURE OF A TRITUNGSTEN CLUS-TER COMPOUND [W_3O_2(O_2CCH_3)_6(H_2O)_3]ZnBr_4·8H_2O

<正> C12H40O25Br4W3Zn, Mr = 1520. 71, monoclinic, space group P1, a = 10. 470(4) b=17. 669(6),c=14. 477(2) A ,α=99. 80(2),αB=101. 51(2),γ=99. 78 (4)°,V=1829A3,Z = 2,DX = 2. 66g/cm3,λ(MoKa) = 0. 71073A,μU= 146. 9cm-1,F (000) = 1408. Final R=0. 038,Rw = 0. 049 for 4088 independent observable reflections.     

X-ray Structure of 1- (3' -Phenyl-4' -morpholinyl-2' 5' - dithiole-1' - ylidene)-3, 4-biscarboethoxy-2-thionaphthalene

1INTR0DUCTIONa-Thiocarbonylthioformamideshavebeensynthesizedsince1980[l-23,however,thereisn0reP0rtofthesecomP0undsrelatedtheirpropertiesandreactivities(3).Ac-cordingtothepublishedpapers('-",adithioketone,adithioesterandadithioth-ioesteraresnitablefort4 2JcycloadditionwithalkenicandacetylenicdienophileS.Wewanttoknowwhethera-thiocarbonylthioformamideshavethesamecharacters,thereforethereactionofathiobenzoylthioformmorpholine(1)withdiethylacetylenedicarboxylate(2)wasexplored.Theredultsshowth…     

Synthesis and Structure of 〔Cu(Hcdta)〕(H_2O)

1mTRODUCTION.Theimportantprogressinmagnetostructuralchemistryinthepastfewyearsisthesystematicdevel0pmentofstructurallyorderedbimetalliccompound"'.Thefami-liesofcrystallineandam0rphouscomplexes[MM'(cdta)j.xH,O(M,M'maybethefirsttransitionmetalorthesecondmaingroupelements)haveprovidedniceex-amplesofstructuralversatilityinmagneticstudiest2-6i,wherequiteafewstructuresmentionedabove,includingbimetallicandhomometalliccompoundscomprisingcop-per0rothermetalatoms,havebeeninvestigated"-".Ontheother…     

Crystal Structure of {(PPh_3)_2RuB_(10)H_8[(CH_3)_2CHO]_2}

1INTRODUCTIONFromreactionsof[RuCl,(PPh,),jwithcloso-[B,,H,,j'-respectivelyinEtOH/CH,Cl,t'i,CH,COOH/THF"'andC,H,COOH/CH,Cl,">solution,itcanbefoundthatbothalcoholandorganicacidcanreplacehydrogenatomsinborane.Further-more,accordingtotheirdifferentreactiontime(3h,1OOhand113hrespectively),wecanknowthatalcoholismoreactivetoreplacehydrogenatomsinborane.NowinordertoconfirmthisrulefurtherweusePhCH(OH)COOH/(CH3)2CHOHsolutioninsteadofabove-mentionedsolutions.Newcompounds(I)and(II…     

SYNTHESIS AND STRUCTURE OF BIS (TETRAETHYLAMMONIUM)-DIPHENYLTHIO LATODITHIOFERRATO-S, S'''' )-DIOXOMOLYBDATE,(Et_4N)_2 [O_2MoS_2Fe (SC_6H_5)_2]

<正> (Et_4N)_2[O_2MoS_2Fe(SPh)_2],M= 726. 77,orthorhombic, space group P212121,with a=12. 434(2),b=10. 162(3),c=28. 285(2) A,V=3573. 8(14) A3,Z = 4,Dc=1. 351gcnr-3,D0=1. 36gcm-3(flotation)λ(MoKa) = 0. 71069A ,μ=10. 0cm-1, F(000) = 1520,T=298K. The structure was solved by heavy-atom method and refined by full-matrix least squares techniques to final R=0. 071 and Rw = 0. 074 for 1992 reflections (I≥3σ(I)). The title complex is a hetero dimetallic cluster containing a planar Mo(μ-S)2Fe rhomboidal core with the Mo-Fe distance of 2. 765(2) A.     

Nickel Group Complexes With Thiolate or/and Phosphine Ligands.Synthesis and X-ray CrystalStructure of 〔Ni_2(pdt)_2 (PEt_3)_2〕

IINTRODUCTIONTransitionmetalcomplexesblendingbothphosphineandthiolateligandshavereceivedattentioninrecentyears,notonlyduetotheirvariationingeometricandelectronicstructuresandproperties,butalsobecauseoftheirapplicationforhomogeneousorheterogeneouscatalyticfunctionsll--33.TheearlierstudiesonthisprojeclweremainlyinthesynthesesofsimplecomplexesandsurveyoftheirpropertiesandEfewhavebeenstructurallyanalyzed"--".Althoughsomeresearchgroupscarriedculpreliminaryworkonnickelgroupcomplexeswithphosphin…     

Synthesis and Structure of Barium Complex Containing 2,2,6,6-Tetramethyl-3,5-heptanedionate and 1,10-Phenanthroline Ligands

1　ＩＮＴＲＯＤＵＣＴＩＯＮＭｅｔａｌ ｏｒｇａｎｉｃｃｈｅｍｉｃａｌｄｅｐｏｓｉｔｉｏｎ(ＭＯＣＶＤ)ｉｓａｎａｐｐｅａｌｉｎｇｔｅｃｈｎｉｑｕｅｆｏｒｅｌｅｃ ｔｒｏｎｉｃａｐｐｌｉｃａｔｉｏｎｓ.ＡｓｏｎｅｏｆｔｈｅＭＯＣＶＤｓｏｕｒｃｅｍａｔｅｒｉａｌｓｆｏｒＹＢＣＯｓｕｐｅｒｃｏｎｄｕｃｔｏｒｆｉｌｍｓ,ｂｉｓ( 2 ,2 ,6,6 ｔｅｔｒａｍｅｔｈｙｌ 3,5 ｈｅｐｔａｎｅｄｉｏｎａｔｅ)ｂａｒｉｕｍｈａｓｂｅｅｎｅｘｔｅｎｓｉｖｅｌｙｕｓｅｄｉｎｔｈｅｐａｓｔ[1～ 3].Ｔｈｅｌａｒｇｅｓｉｚｅｏｆｔｈｅ…