SYNTHESIS AND CRYSTAL STRUCTURE OF Pr(NO_3)_3(Me_2-16-C-5)

<正> The complex Pr (NO3)3 (Me2-16-C-5) (Me2-16-C-5 = 3, 3-dimethyl-1,5,8,11,14-pentaoxacyclohexadecane) crystallizes in the hexagonal space group P65with a = b = 13. 145(2), c=25. 611(5) A ; Z = 6; V = 3832(1)A3; Dc = 1. 53gcm-3; F (000) = 1776;μ= 19. 7cm-1 (MoKa). The final refinement converged with R = 0. 049 and Rw = 0. 051 for 2005 observed reflections. The Pr(Ⅲ) ion is 11-coordinated to three bidentate nitrate groups and five oxygen atoms of a crown ether. The average Pr -O(crown) and Pr -O(NO3-) bond lengths are 2. 68 and 2. 57A , respectively.     

Synthesis and Crystal Structure of［Lu（NO_3）_3（H_2O）_2（CH_3CN）］（Benzo－15－C－5）·CH_3CN

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｌｕ（ＮＯ_３）_３（Ｈ_２Ｏ）_２（ＣＨ_３ＣＮ）］（Ｂｅｎｚｏ－１５－Ｃ－５）·ＣＨ_３ＣＮＷａｎｇＲｕｉ－Ｙａｏ；ＪｉｎＺｈｏｎｇ－Ｓｈｅｎｇ；ＮｉＪｉａ－Ｚｕａｎ（Ｌａｂｏｒａｔｏｒｙｏ...     

SYNTHESIS AND CRYSTAL STRUCTURE OF La（NO3）3（16—C—5）

<正> The title complex LaC11H22O14N3 (Mr = 559. 27) crystallizes in the monoclinic space group P21/c with a=14. 452(7) ,b=8. 260(2),c= 16. 641(8) A ,β= 90. 85(4)°, Z = 4, V=1986. 2(1) A3,Dc=1. 87g·cm-3, F(000) = 1112,μ(MoKa) = 22. 7cm-1. The final refinement converged with R=0. 036 and Rw = 0. 038 for 2996 observed independent reflectios. The average La-O(crown) bond length of 2. 683 A (2. 660-2. 701A)is shorter than that in La(NO3)3(15-C-5)(2. 694A).The distances between opposite O atoms (3. 47~4. 68A) indicate that the cavity of 16-C-5 in the complex is elliptic.     

CRYSTAL STRUCTURE OF Ce(ClO_4)_3 COMPLEX WITH 3,3-R,R''''-16-C-5(R=CH_3;R''''=CH_3O(CH_2)_2OCH~-_2)

<正> The title compound C18H37O20NCeCl3, Mr = 834. 25, orthorhom-bic, P212121, a = 11.836(4), b = 13.899(6), c= 19. 401(6) A ; V=3192(2)A3; Z = 4; Dc=1. 74gcm-3, F (000) = 1684,μ= 17. 8cm-1 (MoKa). The final R = 0. 080, Rw = 0. 081. The Ce(Ⅲ) ion is coordinated to one O atom of one C1O4- ion, a CH3CN molecule, a water molecule and seven O atoms from a crown ether molecule. The other two C1O4- ions are not coordinated to the metal. The bond lengths of Ce-N(CH3CN), Ce -O(ClO4-), Ce -O(H2O) and Ce-O(crown) are 2. 61,2. 82,2. 53, and 2. 56A, respectively.     

Crystal Structure of[La(NO_3)_3(12-crown-4)-(H_2O)](12-crown-4)

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｌａ（ＮＯ_３）_３（１２－ｃｒｏｗｎ－４）－（Ｈ_２Ｏ）］（１２－ｃｒｏｗｎ－４）ＭａｏＪｉａｎｇ－Ｇａｏ；ＪｉｎＺｈｏｎｇ－Ｓｈｅｎｇ；ＹｕＦｅｎｇ－Ｌａｎ（ＬａｂｏｒａｔｏｒｙｏｆＲａｒｅＥａｒｔｈＣｈｅｍｉ?..     

硝酸镧联吡啶冠醚混配配合物La(NO_3)_3(bipy)(H_2O)_2(B-15-C-5)的合成及晶体结构

本文报道了La(NO_3)_3(bipy)(2H_2O)(B-15-C-5)(Mr=785.46)的合成和晶体结构。晶体属单斜晶系,空间群为P2_1/n。晶胞参数:a=11.951(6),b=18.181(7),c=14.754(5),β=96.19(3)°,V=3187.0,Z=4,D=1.637g/cm~3。晶体结构由直接法和Fourier合成解出,使用对角块矩阵和全矩阵最小二乘法对原子参数进行修正,最后偏离因子R=0.035(5261个,I>3σ(I)的衍射)。单晶结构分析表明,在该配合物中,直接参与配位的是联吡啶上的两个氮原子,三个NO_3中的六个氧原子以及两个水分子中的氧原子,La~(3+)的配位数为10。B-15-C-5是通过氢键与H_2O分子相连的。     

SYNTHESIS AND CRYSTAL STRUCTURE OF A TUNGSTEN-COPPER-SULFUR CLUSTER [Et_4N]_2[WCU_3S_4(S_2CNEt_2)_3]

<正> [Et4N]2 [WCu3S4 (S2CNEt2)3], Mr = 1172. 01, orthorhombic, space group P212121 with a=12. 858(9),b=13. 204(5) ,c=29. 501(9) A ,V=5008. 7 A3, Z = 4, Dc = 1. 55gcm-3, μ(MoKa) = 40. 3cm-1. The final R and Rw are 0. 069 and 0. 075, respectively, for 3072 observed unique reflections. The anion contains a slightly distorted WS42~ tetrahedron coordinated by three CuS2 CNEt2 units,with four metal atoms lying in a plane.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS [4,4,4-TRIFLUOR-1-(2-THIENYL) Butandion-1,3] COPPER (Ⅱ) WITH DIMETHYLFORMAMIDE, [Cu(TTA)_2(DMF)]

<正> [Cu(C8H4F3O2S)2(C3H7NO)], Mr = 579. 0, monoclinic, P21/c, a = 9. 4851(6), b = 26. 6574(6), c=9.2619(6) A ,β=96.08(3)°, V = 2328.7A3, Z=4, Dc=1. 65gcm-3, μ(MoKa) = 7. 2cm-1, F (000) = 1172, MoKa radiation, final R = 0. 074 and Rw = 0. 068 for 1841 reflections with I≥3σ(Ⅰ). The Cu(Ⅱ) atom is coordinated by five oxygen atoms, one of which from DMF is in the axial position, to form a square pyramidal geometry. That the thenoyl groups in the ligands take the cis-form around the Cu(Ⅱ) atom is explained by the hydrogen bonding effect.     

Synthesis and Crystal Structure of[Fe_2V (μ_3-O) (μ-O_2CCH_3)_6 (THF)_3]Cl· 3H_2O

lmTR0DUCTI0NTrivanadium(III)ox0-carb0xylat0complexeshaveattractedmuchinterestre-cently"~".Manyc0mp0unds0fthiskindhavebeensynthesizedandtheirstructural,physicalandspectr0sc0picpr0pertieshavebeenstudied.Butnone0fthiskindofcom-plexeswithmixedmeta1shavebeensynthesized.Hereinwereportthecrystalstruc-tureofthefirstmixedmeta1carboxylatocomp0undofvanadium.2EXPERIMENTAL2.1Synthesis0.l6g(lmmol)VCl3,0.32g(2mmol)FeCl3and0.48g(6mm0l)NaCO,CH,wasdisso1vedinaso1uti0n0ft0luerie(20ml),THF(lOml),ac…     

MOLECULAR AND CRYSTAL STRUCTURE OF TETRAHYDROFURAN COORDINATED YTTERBIUM TRICHLORIDES YbCl_3(C_4H_8O)_3

<正> YbCl3(C4H8O)3, Mr = 495. 73, monoclinic, space group P21/c, a = 9.024(2), b=12.863(2), c=15. 762(7) A ,β=92. 21(2)°. V = 1828. 7(9) A3, Z = 4, DC=1. 801gcm-3, A(MoKa) = 0. 71073A, μ= 64. 44cm-1, F (000) = 964, R = 0. 075 for 2259 unique observed reflections. The Yb3+ ion is in a distorted octahedral coordination with three Cl ions and three O atoms from three tetrahydrofuran (THF) molecules. The average Yb -Cl distance is 2. 525A and Yb -O is 2. 303A.     

SYNTHESIS AND CRYSTAL STRUCTURE OF （C5H5）2Ti（o—NHPhC6H4CO2）2

<正> Cp2Ti(o-NHPhC6H4CO2)2, Mr = 602. 54, space group C2/c, a = 33. 77(2), b = 12. 611(6), c=14. 486(9) A ,β=103. 28(4)°,V = 6004(5) (?)3,Z = 8, Dc= 1. 33gcm-1, MoKa(λ=0. 71069(?)) radiation, μ = 3. 21cm-1, F(000) = 2512e, R = 0. 066, Rw= 0. 085 for 2511 radiations. The Ti atom in the molecule is coordinated by two C5H5 groups and two monodentate carboxyl ligands in a distorted tetrahedral geometry with the bonds in the range of Ti-C = 2. 334 - 2. 41(?) ; Ti-O = 1. 914(5) and 1. 919(5)(?);and the bond angles O-Ti-O = 91. 7(2)°; (cent-C5H5)-Ti-(cent-C5H5) = 135. 9(6)°.     

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.     

CRYSTAL STRUCTURE OF LANTHANUM (Ⅲ) COMPLEX WITH CRYPTAND [2,2,1]:H_2[2,2,1]·[La(NO)_3)_2·[2,2,1]]·La-(NO_3)_6·CH_3CN

<正> C34H69La2N13O34(Mr= 1418. 9) belongs to orthorhombic system, space group Pcab with a = 15. 513(3), b = 19. 463(5), c=38. 014(5)(?); Z = 8; V = 11477(4)(?)3; F(000) = 6000; μ=16.1cm-1(MoKa). The final R and Rw are 0. 045 and 0. 045, respectively. The molecule is Composed of one H2[2,2,1]2+, one [La(NO3)2[2,2, 1]]+, one La(NO3)63- and one solvent molecule CH3CN. The La3+ in [La-(NO3)2· [2,2,1]]+ is 11-coordinated by four oxygen atoms from two bidentate NO3- and seven heteroatoms from a [2,2,1] molecule; the La3+ ion in La (NO3)63- is coordinated to six bidentate NO3-. The La - O distances fall in the range of 2. 60-2. 70(?) and the La-N(cryp) mean distance is 2. 88(?).     

The Novel Benzo-15-Crown-5 with Palladium(II) Complex:[Na(B15C5)]2[Pd(SCN)4]

A novel Pd(II) Benzo-15-crown-5 complex [Na(B15C5)]2[Pd(SCN)4] has been isolated and characterized by IR and X-ray diffraction analysis.The crystal structure belongs to monoclinic,space group P21/n with cell dimensions,a=1.0164(6),b=1.3743(3),c=1.4987(7) nm,b=95.248(6)o ,V=2.0847nm3,Z=2,F(000)=944,R=0.053,Rw=0.072.The compound consists of two [Na(B15C5)]+ complex cations and a [Pd(SCN)4]2- complex anion.Each sodium ion is coordinated by five crown ether oxygen atoms and one N atom from the SCN group of [Pd(SCN)4]2- to form stable neutral complex.     

Crystal Structure of Quaternary Mixed Anion Complex of Labthanide [Ce(CH_3COO)_2(NO)_3(phen)]_2

11NTRODUrmNSomequaternarymixedanioncomplesesoflanthanidesweresynthesized.karasavetalsynthesized">Eu(acac)(NO3)(bipy)2.3H2OandJin[2ietal.Synthe-sizedEu(m-MBA)(NO3)(phen)andEu(o-MBA)(NO,)(phen).Onlyacrystalstructureofceriumcontainingphenwasstudied,Ce(CH,COCHCOCH,)3(phen),fromCambridgeStructureDatabase.SowesynthesizedthecomplexoftCe(CH,Coo)z(Noa)(phen)J,andthecrystalstructure.2EXPERmENTAL2.1Cry8talpreparationThecrystalwasseparatedfromtheethanol/waterso-lutionofceriumnitrate…     

STUDIES OF RARE EARTH METAL COMPLEXES OF AMINO ACIDS AND PEPTIDES. SYNTHESES AND CRYSTAL STRUCTURES OF TRIAQUO TRIS (N-ACETYLGLYCINE) LANTHANIDE Ln(CH_3CONHCH_2COO)_3(H_2O)_3(Ln = Nd~(3+),Eu~(3+) and Er~(3+))

<正> The title complexes were synthesized and their crystal structures were determined. These complexes crystallize in trigonal space group R3 with 3 molecules in a unit cell and are isostructural to each other. Crystallographic data: complex 1, Nd(CH3CONHCH2COO)3(H2O)3, Mr = 546. 6, a= 16. 582(4), c = 5. 982(2)(?), V= 1424. 5(8)(?)3, Dc=1. 91gcm-3, F (000) = 819, μ = 28.06cm-1, R(Rw) = 0. 048(0. 061); complex 2, Eu (CH3CONHCH2COO)3 (H2O)3, Mr = 554.3, a = 16.564(10), c=5.974(3)(?), V = 1418(2)(?)3,Dc= 1. 95gcm-3, R (Rw) = 0. 018 (0. 025), F (000) = 828, μ= 33. 83cm-1; complex 3, Er-(CH3CONHCH2COO)3(H2O)3, Mr = 569. 6, a = 16. 476(7), c=5. 946(6)(?), V = 1398(2) (?)3, D, = 2. 03gcm-3, R (Rw ) = 0. 020 (0. 027) , F (000) = 843, μ= 46. 25cm-1. These complexes adopt mononuclear structure, in which Ln(Ⅲ) ion is coordinated to six oxygen atoms from three ligands and three oxygen atoms from water molecules with the polyhedron of 4,4,4-tricapped triangular prism. The carboxy-lato group of the ligand bonds to Ln     

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.     

Syntheses,Crystal Structures and IR Spectra of Two Mixed Metal Complexes:〔Cr_nFe_(3-n)(μ_3-O)-(μ-O_2CC_2H_5)_6 Py_3〕Cl(n=1,2)

1INTR0DUCTI0NTrinuclearoxo-carboxylatocomplexescontainingmixedmetalionshavebeenofintenseinterestsincethefirststructuredeterminedbyX-raydiffractioninl965t1i,Theimportanceofthesecompoundsshowsinservingasmodelstotesttheoriesforthepotentialmagneticcoupllngbetweenmetalionsinmultinuclearsystem,asempha-sizedbyCANNONDetal.t2i.However,inrecentyears,wehavefoundthatthiskindofcompoundsmayactasaprecursorofthecatalystfortheadditi0nreactionofacetylenewitheitherH,O0rH,,andf0rtheketonizationofacidbydec…     

Crystal Structure of Lanthanum（Ⅲ） Nitrate Complex with 4－Tert－butyl－benzo－15－crown－5 （L）

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＬａｎｔｈａｎｕｍ（Ⅲ）ＮｉｔｒａｔｅＣｏｍｐｌｅｘｗｉｔｈ４－Ｔｅｒｔ－ｂｕｔｙｌ－ｂｅｎｚｏ－１５－ｃｒｏｗｎ－５（Ｌ）￥ＭａｏＪｉａｎｇ－Ｇａｏ；ＷａｎｇＲｕｉ－Ｙａｏ；ＪｉｎＺｈｏｎｇ－Ｓｈｅｎｇ（Ｌａｂｏ...     

Crystal Structure of 3-methyl-1, 2, 3, 4, 4a, 4b, 9a, 15, 15a,15b-decahydro-(4,5);(4a,15)-dimethano-tricyclo(4, 3, 1, 0~(2,7)) deca 〔8, 9, 1, 10-a,b, c〕pyrido〔4,3-a〕-acridin-6-en-9-ol-8-one

1INTRODUCTIONIntheO-demethyIationof7a-o-amino-phenyl-6,14-endo-ethenotetrahydrothe-baine,catalyzedbyhydrobromicacid,ifinhightemperatureandprolongedtime,anewcomPoundwithyie1dof17.9%wasfound,whosestructurecannotbedeferredfromthepreviousacid-catalyzedrearrangementof6,14-endo-ethnotetrahydrothe-baines(1-33.ItwascrystallizedfromanhydrousethanolsolutionanditsstructurewasdeterminedbyX-raycrystallography.2EXPERmENTALAcrystalwithdimensionsofO.3mmXO.4mmXO.5mmwasmountedonanEnraf-NoniusCAD4d…