Syntheses and Crystal Structures of 3,3'-(9,10-Anthrylene)bis-pentane-2,4-dione and 3-(2-Methoxy-1-naphthalenyl)-pentane-2,4-dione

1 INTRODUCTION 3-Substituted pentane-2,4-diones, as a series of chelating ligands to coordinate with many metal ions, have been extensively studied in coordination chemistry. These compounds can also act as valuable intermediates in the synthesis of calamitic derivatives both with or without metal ion[1]. However, compared to the 3-alkylation of 2,4-pentanediones, the direct synthesis of 3-aromatic pentane-2,4-diones from pentane-2,4- diones is much difficult. Previous methods to direc…     

CRYSTAL STRUCTURE OF CHLORO-([(N,N-dimethylamino)methyl]-ferrocene-2 C,N)(pyridine)palladium(Ⅱ)

<正> C18H21ClN2FePd(PdCl(DMAF)(py)),Mr = 463. 08,monoclinic,P21/n, a=10. 498(3),b=12. 082(8) ,c= 14. 487(9) A ,β= 106. 08(4)°, V= 1765. 8A3,Z = 4,Dc=1. 74g·cm-3. The final refinement converged with R=0. 051 and Rw = 0. 075 for 3277 observed reflections with I≥3σ( I ). The complex possesses a cyclo-palladated ferrocene with a a bonded Pd-C.     

CRYSYTAL AND MOLECULAR STRUCTURES OF η~8-CYCLOOC-TATETRAENYLLANTHANIDE COMPLEXES [(η~8-C_8H_8)LnCl-(OC_4H_8)_2]_2(Ln=Pr, Nd)

<正> Complexes [(η8-C8H8)LnCl(OC4H8)2]2, (Ln = Pr(1), Nd(2)) both crystallize in monoclinic space group P21/n with cell dimensions for 1: a = 11. 860(3), b=12. 697(3), c=12. 161(2)(?), β=111. 88(2)°, V= 1699. 50(69) (?)3, Dc=1. 66gcm-3,Z==2 (4 monomers), μc=30. 2cm-1, F (000) = 848, the final R = 0. 031, Rw = 0. 032 for 2303 independent reflections with I≥ 3σ(I) ; and for 2: a=11. 834(4), b = 12. 666(5), c=12. 166(3)(?), β=111. 73(2)°, V= 1694. 03 (99)(?)3, Dc= 1. 68g. cm-3, Z = 2 (4 monomers), μc=32. 3cm-1, F(000) = 852, R=Rw = 0. 035 for 3487 independent reflections with I≥3σ(I). In each complex, there are two Ln atoms in a dimeric unit which are bridged asymmetrically by two chloride ions with Ln - Cl bond lengths of 2. 847(2) and 2. 924(2)(?) for 1, or 2. 836(1) and 2. 919(2)(?) for 2. The cyclooctatetraene COT dianion ring is planar with eightfold molecular symmetry and an average C -C bond length of 1. 392(?). It is symmetrically coordinated to the Ln atom with an average Ln - C distance of     

CRYSTAL AND MOLECULAR STRUCTURE OF A PENTA-COOR-DINATED SILVER COMPLEX, SILVER 8-HYDROXYQUINOLINE-5-SULFONATE AgC_9H_8NO_4S

<正> AgC9H6NO4S, Mr = 332. 1, monoclinic, space group P21/c, a = 8. 292(1), b = 10. 394(2), c=10. 852(2)A, β=102. 73(1)°, V =912. 4(?)3, Z = 4, Dc = 2. 417gcm-3, λ(MoKα) = 0. 71073(?) , μ = 24. 0cm-1, F (000) = 648, final R =0. 041, Rw = 0. 047 for 1369 observed reflections. The coordination polyhedron of Ag(I) is penta-coordinated square pyramid.     

CRYSTAL AND MOLECULAR STRUCTURE OF N_2-[(4-METHYLPHENYL)-SULFONYL]-CLUTAMINE (C_(12)H_(16)N_2O_5S)

<正> C12H16N2O5S, Mr = 300. 34, monbclinic, P21, a = 12. 748(4), b = 5. 240(1), c=21. 356(4)(?); β=93. 28(2)°, V = 1428. 1(7) (?)3. Z = 4, Dc = 1. 397gcm-3, λ=0. 71073(?). Full matrix least-squares refinement, final R = 0. 042, Rw = 0. 045 for 2050 unique reflexions with I≥3σ(I). The two molecules in the asymmetric unit are connected by two hydrogen bonds to form a dimer.     

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.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS [4, 4, 4-TRIFLUORO-1-(2-THIENYL) BUTANEDIONE-1, 3] NICKEL (Ⅱ) WITH DIMETHYLSULFOXIDE, [Ni(TTA)_2(DMSO)]

<正> The title complex [Ni(TTA)2(DMSO)] (TTA = thenoyl trifluo-roacetone, DMSO=dimethyl sufloxide) belongs to triclinic, space group P1, parameters of crystal cell: a = 9.447(l), b = 10.505(1), c=11. 912(1)(?) , α=97. 42(1), β= 84. 00(1), γ = 102. 08(1)°, V = 1143. 3(?)3, Z = 2, Mr = 581. 22 [Ni (C8H4O2F3S)2(CH3)2SO)], Dc=1. 688g. cm-3, F(000) = 588, final R = 0. 065 and Rw = 0. 072 for 2873 reflections with I≥3σ(I). In the title complex the nickel atom has a square pyramidal geometry with four short Ni-O bonds and one long Ni -O (DMSO) bond.     

Crystal Structure of [CH_3CH(OH)COO]_2Fe(H_2O)_2·H_2O

<正> The title compound C6H16O9Fe, Mr = 288. 13, was synthesized and crystallized in monoclinic space group P21/c, a = 9. 409(4), b = 5. 812(4), c= 22. 122(7)(?) , β=90. 80(3)°. V = 1209. 6(?)3, Z = 4, Dc=1. 572g/cm3, F(000) = 592, μ = 12. 73cm-1, R = 0. 063, Rw= 0. 068 for 1191 observed reflections. The iron atom is surrounded by O(1 - 6) in a distorted octahedron.     

Crystal Structure of Nickel (Ⅱ) Complex with 3Hydroxy1-1, 5-diazacycloheptane

1INTRODUCT1ONMesocyclicdiamines(e.g.1,5-diazacyclooctane,1.4-diazacycloheptane)asversatilechelatingagentsoftenprovideastericeffectalongwithastrongligandfieldeffectE'jTheyeasilyformstablecomplexesinunusualgeometrieswiththetransitionmetalion.[2j.Forexample,thecrystalstructureoftheNiCl,complex,Ni(dach),Cl,(dach=1.4-diazacyclohepane),showsthattheNi(I)isplanarwithNi-Nbonddis-tancesof1.917(5)and1.921(6)Aandthetwodachligandsinthetransboat-boatco.fo.mation[3j'Inordertoextendfurtherthecomplexat…     

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.     

STUDIES ON THE CRYSTAL STRUCTURE OF CHALCONE DERIVATIVES Ⅰ. Crystal Structure of 4-Brom-4'''' -Methoxyl-Chalcone(BMC)

<正> BrC6H4C2H2COC6H4OCH3, Mr = 317. 19, is monoclinic, space group PC with unit cell of a = 15. 869(3), b = 7. 146(2), c=5. 991(1) (?); β=82.85 (1)°; Z = 2, Dc=1. 56g/cm3; V = 674. 1(?)3; λ(MoKa) = 0. 71073A, μ= 30. 1 cm-1, F(000) = 320e, final R = 0. 040, Rw = 0. 041 for 993 observed reflections with I>3σ(I). As the two phenyl planes and the C2H2CO group are non-coplanar, the conjugated system was disturbed. This will produce a large hypsochromic shift of cutoff wavelength of transmission.     

Synthesis and Crystal Structure of 1-(o-methylphenyl)-2-(p-methoxyphenyl)-1,3,2-diazaphospholidin-4-thione-2-sulfide

11NTRODUCTIoNThederivativesofdiazaphospholidinoneorthecorrespondingthionesareknowntopossessinterestingbiologicalproperties,suchasherbicidalactivity"'2i.Inrecentyears,itwasreportedthatthel,4,2-diazaphospholindine-5-thione-2havegoodselectiveherbicidalactivity"'41.Tolookformoreeffectiveherbicideswithlowtoxicity,aseriesofnovel1-(o-methylphenyl)-2-(p-methoxyphenyl)-phospholidin-4-thione-sulfideshavebeensynthesizedandtheirmolecularstructuresstudied.PreliminarybioassaysshowthatthesecomPoundshaveg…     

APPLICATION OF DITHIO - MOLYBDATE IN THE SYNTHESES OF Mo-Cu CLUSTERS: SYNTHESES AND CRYSTAL STRUC-TURES OF MoOS_3(CuPPh_3)(Cu(PPh_3)_2 AND (Ph_4P)_2[Mo_2Cu_5S_6O_2-(S_2CNEt_2)_3] ·DMF

<正> The reactions of (NH4)2MoO2S2 with Cu(PPh3)3Cl in CH3CN in the air, or with CuCl, Ph4PBr, and NaS2CNEt2 in DMF under anaerobic condition, afforded the cluster complexes MoS3OCu2 (PPh3)3 (Ⅰ) and (Ph4P)2 CMo2Cu5S6O2-(S2CNEt2)33 · DMF (Ⅱ), respectively. Compound (Ⅰ), MoOS3Cu2P3C54H45(Mr = 1121. 0) , crystallizes in the triclinic, space group P1 with cell parameters a = 14. 103 (3), b = 17.906(3), c=11.503(2)(?), α=107. 76(1), β=111.81(2), γ = 74.93 (2)°, F = 2532. 9(?)3 and Z=2, Dc=1. 471 g/cm3, F (000) = 1140, μ(MoKα) = 13. 215 cm-1, final R = 0. 060 (Rw = 0.064) for 5959 independent reflections with I >3σ(Ⅰ). Complex (IⅡ), Mo2O3S12Cu5P2N4C66H77 (Mr = 1930. 67) , crystallizes in monoclinic, space group P2/c with cell parameters a = 25. 325(19) , 6 = 22. 506(9) , c =14. 066(8)(?) , β =100. 96(6)°, V =7871. 16 (?)3, Z = 4, D,= 1. 629 g/cm3, F(000) = 3904, μ(MoKα) = 20. 216 cm-1, R = 0. 097 (Rw = 0. 095) for 5677 reflections with I>3σ(Ⅰ). The core structure of complex (Ⅰ) is defective cub     

SYNTHESIS AND STRUCTURE OF THE PEROXOVANADIUM (V) COMPLEX CONTAINING NITRILOTRIACETATE Na_2[VO (O_2) N-(CH_2COO)_3]·5H_2O

<正> Na2[VO(O2)N(CH2COO)3] · 5H2O, Mr= 423. 11, monoclinic, space group P21/c, a = 6. 283(3), b = 20. 378(6), c=12. 056(4)(?) , β=102. 96 (3)°, V = 1507. 9(?)3, Z = 4, Dc= 1. 864 g/cm3. λ(MoKα) = 0. 71069A , F(000) = 864. Final R = 0. 037 and Rw = 0. 046 for 1658 observed reflections with I>10σ (I). The structure of the anion of the title complex shows that the vanadium atom is coordinated by one vanadyl oxygen atom, two oxygen atoms of the peroxp-group, three oxygen atoms and one nitrogen atom from the NTA ligand to form a distorted pentagonal bipyramid.     

SYNTHESES AND CRYSTAL STRUCTURE OF [Et_4N]{Mo(CO)_5L}(L=I~-,SPh~-)

<正> Crystal of [Et4N][Mo(CO)5I](1) (Mr = 493. 15) is tetragonal with space group P4/n, a =b==9. 374(2) ,c=10. 545(2)(?), V=926. 5(?)3, Z = 2, F(000) = 480, Dc=1. 77g/cm3and μ = 23. 6cm-1. R = 0. 040, Rw = 0.043 for 374 observed reflections. Crystal of [Et4N][Mb(CO)5(SPh)] (2) is orthorhombic ith space group Pbam, a= 15. 230(3), b = 18. 389(10), c=8. 172(3)(?), V=2288. 6 (?)3, Z = 4, Dc=1. 38gcm3, μ = 6.7cm-1.R = 0. 043, Rw = 0. 042 for 1621 observed reflections. Complexes 1 and 2 possess the same geometry. The Mo atom is octahe-drally coordinated with obvious trans drrdct, all the Mo -C bond lengths are shorter obviously and the C - O bond are longer than those of Mo(CO)6.     

CRYSTAL STRUCTURES OF ISOMERS OF DIHYDROXYDIBENZO—14—CROWN—4

<正> C18H18O6·H2O, Mr = 348. 34, cis-isomer: orthorhombic, Cmc21, a = 16. 421(3), 6 = 11.978(1), c=8. 624(1)(?), V = 1696. 2(?)3, Z = 4, Dc= 1.293 gcm-3, λ(MoKα) = 0. 71073(?), μ = 0. 911cm-1, F (000) = 763, R = 0. 043, Rw = 0. 042 for 769 unique observed reflections. trans-Isomer : orthorhombic, Cmc21, a = 16. 503(2), b = 12. 297(2), c=8. 557(3) (?). V = 1736(?)3, Z = 4, Dc= 1.271 gem-3, λ(MoKα) = 0. 71073(?), μ = 0. 892cm-1, F (000) = 736, R=0.048, Rw = 0. 046 for 551 unique observed reflections. The configurations of the two molecules appear as butterflies. There is a Cm symmetry in the molecule of each isomer.     

CRYSTAL STRUCTURE OF （C8H8）Sm（2,4—C7H11）（THF）

<正> The crystal structure of (C8H8)Sm(2,4-C7H11)(THF)(2,4-C7H11 = 2, 4-dimethylpentadienyl) , Mr=421. 8, has been determined which, belongs to monoclinic space group P21 with a = 8. 682(3), 6 = 10. 968(3), c=9. 744(3) (?) ,β= 104.24(2)°, V = 899. 3(4)(?)3, Z = 2, Dc=1. 66g/cm3, μc=33. 2cm-1, F(000) = 422 and final R = 0. 041 for 2021 observed reflections with I≥ 2σ(I). The 2,4-dimethylpentadienyl group is in "U " conformation. The carbon-carbon bond distances within the pentadienyl ligand fall essentially in two sets. The average distance of external C - C bonds is shorter than that of the internal bonds.     

CRYSTAL STRUCTURE OF K_7H_6[Nd(GeMo_(11)O_(39))_2]·27H_2O

<正> K7H6[Nd(GeMo11O39)2]·27H2O, Mr = 4413.8, crystallizes in monoclinic, space group P21/n with a = 17. 095(4), b = 26. 895(3), c = 21. 214(5) (?); β=103. 11(2)°;V = 9499. 4(3)(?)3; F(000) = 8808; Z = 4; Dc = 3. 05g/cm3; μ(MoKα) = 43. 7cm-1 and λ=0. 71069(?). A total of 8644 reflections with I≥3σ(I) were used in the structure analysis. The final R value is 0. 090, Rw value is 0. 091. The atom Nd is situated between two tetradentate heteropoly (GeMo11O39)8- ligands to form the anion [Nd(GeMo11O39)2]13-. Nd is surrounded by eight oxygen atoms at average distances of 2. 446 (?), forming a square antiprism.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A NEW BINUCLEAR CUPRUM COMPLEX, [(CuCl)_2(η~2-dppe)_2(μ-dppe)]·2CH_2C1_2

<正> C80H76Cl6Cu2P6,Mr=1563.13,monoclinic,P21/n,a=12.608(9),b=21.729(7),c=14.473(8)A.,β=105.34(5)°,V=3823.6A3,Z=2,Dc=1.28 g.cm-3,F(000)=1528,μ=8.6 cm-1,The final R and Rw are 0.076 and 0.083 respectively for 4418 observed reflections with I≥3σ(I).There is a center of inversion in the molecule.     

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…