CRYSTAL AND MOLECULAR STRUCTURE OF 3a-(4-CHLORO-PHENYL)-1, 5-DIPHENYL-3a, 4,5,11-TETRAHYDRO-1, 2, 4-OXA-DIAZOLINO [5,4-d][1, 5]BENZOTHIAZEPINE, (C_(28)H_(21)N_2OClS)

<正> The structure of 3a-(4-chlorophenyl)-1, 5-diphenyl-3a, 4,5,11-te-trahydrq-1, 2, 4-oxadiazolino [5, 4-d][1, 5] benzothiazepine (C28H21N2OClS) has been determined. The compound crystallizes in triclinic space group P1 with two formula units in a cell of dimensions: a =11. 114(2), b = 11. 673(1), c=10. 435(1) (?), α=98. 42(1), β=118. 69(1),γ = 98. 64(1)° and V = 1136. 2(3)(?)3. The structure was solved by using direct methods and refined by full matrix least-squares. The final crystallographic discrepancy factor is 0. 058 for 2384 observed reflections. The molecular backbone is a tricyclic system : The seven-membered hetero ring in the center is in twisted-boat conformation, and is cis-fused to 1, 2, 4-oxadiazolino ring which is in an envelope form, together with the equilaterally adjoined benzene ring . The compound has a non-planar conjugation system.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A MOLYBDENUM-COPPER-SULFUR CLUSTER COMPLEX WITH DITHIOBENZOATE LIGAND [Bu_4N]_2[MoCu_2S_4(C_6H_5CS_2)_2]

<正> The title compound has been synthesized by the reaction of (Bu4N)2MoS4, CuCl and (C6H5CS2)(Bu4N) in DMF and recrystallized from DMF/ Et2O. The red black crystal belongs to the triclinic space group P1 with a = 12. 021 (6), b = 17.045(8), c=17. 136(7)(?) , α=110.05(3), β=108.64(4), γ=103.87 (4)°, V = 2873(3)(?)3, Dc=1. 321gcm-3, Z = 2. The structure was refined to R = 0. 065 for .4783 reflections. The anion of the title compound can be described as a MoS42- tetrahedron coordinated by two [Cu(C6H5CS2)] units with the three metal atoms lying on a line. The coordination number of each Cu atom is three.     

CRYSTAL STRUCTURE OF (C_5H_9C_5H_4)_3Er_4(μ_2-Cl)_6(μ_3-Cl)(μ_4-O)-(THF)_3

<正> The crystal of (C5H9C5H4)Er4(μ2-Cl)6(μ3-Cl)(μ4-O)(THF)3 belongs to triclinic space group P1, with a = 11. 909(4), b = 15.343(5), c=15. 619 (4)(?), α=104. 18(2), β=98. 81(3), γ= 111. 06(2)°, V = 2486(1)(?)3, Z = 2, Dc = 2. 07g/cm3, λ(MoKα) = 0.71073(?), μ= 73. 4cm-1, F(000) = 1476, Mr=1549. 25. The structure was solved by Patterson and Fourier techniques and refined by block diagonel least-squares method to final R = 0. 078 and Rw = 0. 084 for 5594 reflections with I≥1. 5σ(I). The results revealed that the complex is composed of four Er atoms bridged by seven Cl and one oxygen atoms with three of the Er atoms bonded each to a cyclopentylcyclopentadienyl group, and one Er atom, bonded to three THF. The Er atoms constitute a pseudo-tetrahedron.     

CRYSTAL STRUCTURE OF ERBIUM (Ⅲ) COMPLEX WITH 1,2,4-BENZENETRICARBOXYLIC ACID

<正> [ErC6H3(COO)3(H2O)3] ·H2O, Mr = 446. 5, orthorhombic, space group P212121, a = 6. 072(1), b = 9.530(2), c=19. 844(4)(?) , 7 = 1148.3 (4)(?)3, Z=4, Dc = 2.58g/cm3, F(000) = 852, μ(Mo Kα) = 76. 4/cm. The final R = 0. 044 and Rw = 0. 046 for 1570 observed unique reflections with I> 3σ(I). The erbium ion is nine-coordinated by six oxygen atoms from four 1, 2, 4-benzenetri-carboxylates and three from three aqua molecules, forming a mpnocapped square an-tiprism. The Er -O distances fall in the range of 2. 31 - 2. 66 A with an average of 2. 42(?). The structures of title complex and [13] show a similar three dimensional polymeric network.     

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 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.     

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.     

STRUCTURE AND BONDING OF Sm_(0.27)Nb_(2.73)Se_4 BY SOLID STATE REACTION

<正> The title compound was prepared from the corresponding elements (Sm, Nb and Se) using transport reaction with iodine at a temperature gradient of 1100/1040℃. The crystal structure was established by the single crystal X-ray diffraction technique with the following crystal data: Sm0.27Nb2.73Se4, Mr = 609. 8, hexagonal, P63/m, a = 9.997(1), c=3.470(2) A , V = 300. 4(2)A3, Z = 2, Dc= 6. 75 g/cm3, F (000) = 529. 34,μ= 292. 6cm-1, R = 0. 018, Rw = 0. 019. The ternary compound was confirmed to be isostructural with the compound Nb3Se4, and was found to be a conductor.     

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.     

REACTIVITY OF METAL(O) DITHIOCARBAMATO CARBONYL COMPLEXES [Mo(CO)_4(S_2CNEt_2)]~- (M=Mo, W): SYNTHESIS AND STRUCTURE OF A NEW MIXED-VALENCE DINUCLEAR MOLYBDENUM-SULFUR COMPLEX, [Et_4N]_2[(CO)_4MoS_2MoS_2]

<正> The reaction of [Et4N][Mo(CO)4(S2CNEt2)] with tetraethylam-monium tetrathiomolybdate affords a new mixed-valence dinuclear molybdenum complex [Et4N]2[(CO)4MoS2MoS2] (1). 1 crystallizes in the orthorhombic space group Pbom with a = 18.403(2), b = 11.963(1), c= 13. 482(1)(?) , Z = 4, V = 2986(?)3, Dc=1. 55g/cm3, Mr = 6S2. 69. R =0. 042 and Rw =0. 057 for 1975 independent reflections with I≥3σ(I), F(000) = 1416, μ =11. 2cm-1. The structure of the anion of 1 consists of an octahedron for the lowvalent Mo atom and a tetrahedron for the high-valent Mo atom sharing an S - S edge. The Mo - Mo bond distance is 2. 992 (2) (?) and the bimetallic center MoS2Mo is planar with Mo-S of 2. 517 and 2. 231 A and MoSMo angles of 78. 04° and 77. 67°. The electron delocalization between the two Mo atoms with wide separated oxidation states is also discussed.     

THE FORMATION AND CRYSTAL STRUCTURE OF 3β, 5α, 6β, 25-TETROL-24ζ/-METHYLCHOLESTAN TRIHYDRATE: C_(28)O_4H_(50)·3H_2O

<正> Compound C28O4H50·3H2O(Mr = 504. 74) is the orthorhombic space group P212121,wilh a=8. 244(3),b=9. 957(2),c=36. 442(3) A ,V=2991. 4 A3,Z = 4,Dc=1. 123g/cm3,and F(000) = 1120. The structure was solved by direct methods and refined by full-matrix least-squares to R=0. 064 for 2029 independent reflections with I≥1σ(I). The results showed that the basic structure of C28C4H50 is a 4-carboatomic ring -3 - terpene. There are three water molecules in an asymmetric unit.     

CRYSTAL AND MOLECULAR STRUCTURE OF TRIS (HYDROX-YMETHYL) AMINOM ETHANE ARSENATE (THAMAS)

<正> (CH2OH)3CNH3H2AsO4, M, = 263. 08, monoclinic, space group P21, with a = 8. 232(2), b = 6. 180(2), c=9. 856(3)(?) , β=104. 77(2)°, Z = 2, V = 484. 81(?)3, Dc= 1. 80 g/cm3, MoKα radiation, μ = 35. 02cm-1, F(000) = 268. The final R and Rw are 0. 040 and 0. 037, respectively. The molecule of THAMAS is composed of TAMH+ and H2AsO4- which are held together by a hydrogen bond. Adjacent molecules in THAMAS crystals are connected by intermolecular hydrogen bonds.     

CRYSTAL AND MOLECULAR STRUCTURE OF 1-(4-DIMETHY-LAMINOPHENYL)-2- (3, 4-METHYLENE-DIOXYPHENYL ) ACRY-LONITRILE, C_(18)H_(16)N_2O_2

<正> C18H16N2O2, Mr = 292. 34, monoclinic space .group P21/c, a= 7.972(6), b = 6. 446(3), c=28.906(4)(?); β=95.59(8)°, V = 1478. 3(7)(?)3, Z = 4, Dx =1. 313 g/cm3, R = 0. 049. The non-hydrogen atoms of the title molecule are nearly co-planar forming a conjugation system.     

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     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF Mo_3(μ_3-O)-(μ-S)_3(μ-OOCCH_3)(dtp)_3(Py)

<正> The title compound was obtained by the reaction of Mo3(μ3-O) (μ-S)3(dtp)4(H2O) with CH3COONa and pyridine. Mo3C19H38N1O9P3S9,Mr= 1093. 79, triclinic, space group P1, a = 12. 921(3) , b = 14. 260(3) , c= 12. 800(3)(?),α = 97. 54(2), β=116. 66(1), γ=100. 10(2) °, V = 2015, 2(8)(?)3, Z=2, Dc = 1. 80gcm-3, F(000) = 1092, final R = 0. 066 for 3444 observations, room temp. In the structure the three Mo atoms form an isosceles triangle capped by a μ3-O atom with three sides of 2. 589(2) , 2. 642(2), and 2. 627(2) (?) respectively, and the car-boxyl bridged Mo-Mo bond is the shortest one.     

CRYSTAL STRUCTURE OF CYCLOOCTADIENYL POTASSIUM TE- TRAHYDROFURANATE ,C_8H_(11)K(OC_4H_8)_2

<正> The title compound, cyclooctadienyl potassium tetrahydrofuranate was prepared by the reaction of cycloocta-1,5-diene with metallic potassium in tetrahydrof u-ran(THF) in the presence of triethylamine. Its crystal structure was determined by a low temperature X-ray diffraction analysis method. The crystal is monoclinic with space group Pc,a=6. 192(3),b=9. 444(8),c=14. 543(1) A ,β=94. 92(5)°,V = 847. 24 A3,Z = 2,DC= 1. 14 g/cm3 and μ(MoKa) = 5. 58cm-1. The structure was solved by heavy-atom methods and refined by least-squares to a final R value of 0. 049. The potassium cations, each with two complex THF molecules attached,are linked by bridging cyclooctadienyl an-ions,while the anions are connected to the bridging cations to form a puckered chain.     

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.     

STUDIES ON RARE EARTH METAL COMPLEXES OF AMINO ACIDS. THE SYNTHESIS AND CRYSTAL STRUCTURE OF TE-TRAKIS ( ALANINE ) OCTAAQUODILANTHANIDE HEXAPER-CHLORATE [Ln_2(Ala)_4(H_2O)_8]*(ClO_4)_6(Ln = Er~(3+)and Eu~(3+),Ala=CH_3CH(~+NH_3)COO~-)

<正> Complex [Er2(Ala)4(H2O)8]·(ClO4)6, 1, Mr = 1431. 8, mono-clinic, space group C2/c with cell parameters a= 18. 21(1), 6 = 14. 67(2), c=17. 19(3)(?), β=101. 60(8)°, V = 4495(4)(?)3, Dc=2.11g/cm3, Do = 2. 09g/cm3, Z = 4, F (000) = 2808, μ= 42. 30cm-1; Complex [Eu2(Ala)4(H2O)8]·(ClO4)6, 2, Mr = 1401.4, monoclinic, space group C2/c, a = 18. 16(4) , b = 14.52(2), c=17. 35(1)(?), β=102. 3(1)°, Z = 4, V= 4468(11)(?)3. The structure of complex 1 is refined by full-matrix least - squares method with 3348 observed reflections (I≥3σ (I)) to R = 0. 048 and Rw= 0.060. The two erbium ions in the dimeric complex cation [Er2(Ala)4(H2O)8]]6+ are connected by four bridging carboxylato groups, each pair of the carboxylato groups is coplanar with the two Er(III) ions and the dihedral angle between the two planes is 91. 42*. Each Er3+ion is coordinated by four carboxylato oxygen atoms and four water oxygen atoms, assuming a square antiprism arrangment. The alanine exists in the form of CH3CH (+NH3) COO- , and the mo     

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.     

Preparation and Crystal Structure of 12β,15α-dihydroxyprogesterone

Progesterone(1) was biotransformed into the title compound 12β,15α-dihydroxy-progesterone(2) with Colletotrichum lini AS3.4486.The biotransformation process was monitored with HPLC.The structure of 2 was determined by 1H NMR,13C NMR,ESI-MS and single-crystal X-ray diffraction.The crystal of the compound belongs to orthorhombic,space group P212121 with a = 8.0671(9),b = 12.3970(15),c = 18.532(3) ,Z = 4,V = 1853.3(4)3,Dc = 1.242 mg/m3,μ = 0.084 mm-1,F(000) = 752,R = 0.0373 and wR = 0.0850.Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 2 has been constructed by multiply intermolecular O(2)-H(2)…O(4) and O(3)-H(3)…O(2) H-bonding interactions.