MOLECULAR STRUCTURE AND SPECTRAL STUDIES OF Ni(ENAC)

<正> C12H20N2O2Ni,Mr = 283. 02, orthorhombic, Pbn21 ,a = 10. 269 (2), b = 12. 182(2),c= 10. 348(1) A,V=1294.5 A3,Z = 4,DC = 1. 452 g/cm3,MoKa radia-tion(λ= 0.71073 A ) ,μ= 14. 96 cm-1, F (000) = 600, R = 0. 058 for 1131 reflections. The Ni (Ⅱ ) ion in This molecule has a square planar configuration. The three chelate rings formed by Ni atom and ENAC2- are coplanar with the plane of NiO2N2. Ultra violet-visible and IR spectra are in agreement with the crystal structure data.     

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 AND MOLECULAR STRUCTURE OF 1,10-PHENANTHROLINE TETRACARBONYL CHROMIUM AND -MOLYBDENUM COMPLEXES, (C_(12)H_8N_2)M(GO)_4 (M=Cr and Mo)

<正> The crystal and molecular structures of (C12H8N2)Mo(CO)4 and (C12H8N2)Cr(CO)4 are reported. They crystallize in the space group C2/m and are isomorphous with each other. The unit cell dimensions for (C12H8N2 Cr(CO)4 are a=15.404(2), b=12.091(2), c=8.223(2) A, 3=108.70(2)0, and V=1450.6(9) A3, while for (C12H8N2)Mo(CO)4 are a=15.546(6), b=12.086(4), c=8.269(1.) A, β= 107.37(2)0 and V=1482.9(l.5) A3, and both Z=4. Final R=0.040 Rw=0.050 for (C12H8N2)Cr(CO)4 and R=0.034 Rw=0.053 for (C12H8N2)Mo(CO)4.     

CRYSTAL STRUCTURE OF THE METHYL 4—（N—（1—OXYPROPYL）—N—PHENYLAMINO]—1—[2—（2—THIENYL）ETHYL]—4—PIPERIDINECARBOXYLATE（R31826）HYDROCHLORIDE

<正> C22H28N2O3S.HCl, Mr = 436.9, triclinic,P1;a=8.557(3),b= 10.299(2),c= 13.894(2)A;α= 99.25(1),β=86.64(2),γ= 107.68(2)°;V= 1151.2(3)A3,Z= 2, DC = 1.27g/cm3,R=0.064. The torsion angle C(14)-C(1)-N(2)-0(19) in the title compound is 137.5 being much larger than that (106°) in R30730. The dihedral angle between mean planes of the thiophene ring and piperidine ring is about 83 .     

CRYSTAL STRUCTURE OF 2—（BENZOYLMETHYLENE）IMIDAZO—LIDINE

<正> The title compound C11H12NzO,Mr= 188. 25. Crystalizes in monoclinic space group P21/n with the following cell parameters;a= 7. 108(4),b= 6. 371(3),c = 21.588(11)A,β=97. 32(2)°. V = 969. 7(8)A3,Z=4,Dc=1. 29g/cm,μ(MoKa) = 0. 9cm-1,F(000) = 400. The final R=0. 068 for 1046 independent reflections with F≥2. 5σ(F). The molecule exists in ketene aminal form rather than in its imine or enol form.     

STRUCTURE OF CHLORO [2-2''''-PYRIDYL)-6-MSTHYLBEHZOTHIAZOLE] PYROCATECHOLATOANTIMONY(Ⅲ)

<正> C19H14N2O2ClSSb,Mr = 491.6, space group P1, a = 5.977(1), b= 8.708(1), c = 8.962(1) X, a=93.91(1),B= 103.25(1),r=94.80(1), V = 450.6 A3, Z = 1, Do = 1.79, DC = 1.812 g.cm-3,F(000) = 242,u(MoKa)= 18.1 cm-1,R=0.024 for 2903 reflections. The Sb atom is situated in a distorted square- pyramidal ( octahedral) environment, with Sb-Cl 2.546(2), Sb-0 2.004(2)/2.038(3), and Sb-N 2.442(3)/2.526(3)A.     

SYNTHESIS AND STRUCTURE OF PERCHLORATOBIS-(2,2''''-BIPYRIDYL) COPPER (Ⅱ) PERCHLORATE

<正> C20H16Cl2CuN4O8,JMr = 574. 82,triclinic,space group PI,a =7. 397 (1),b=11. 172(3),c=15. 185(5)A,α=66. 28(2),β=76. 91(1),γ= 80. 74(2)°,V = 1115. 6A3,Z = 2,D=1. 71g·cm-3,μ=12. 76cm-1,F(000) = 582,R=0. 045,Rw = 0. 048. The Cu atom is coordinated by four N atoms from the two 2,2'-bipyridyls and two O atoms from two ClO4- groups,forming a distorted octahedron. A chain structure is developed through the coordinated ClO4-.     

STUDY ON THE STRUCTURES OF COMPLEXES OF LANTHANIDE WITH BIDENTATE HETEROCYCLIC AMINE——THE STRUCTURE OF BIS[TRI(TRICHLOROACETATO)-1,10-PHENANTHROLINE-BTHANOL-GADOLINIUM]

<正> (GdC12H8N2(CCl3CO2)3C2H5OH)2,Mr=870.60,monoclinic,space group P21/n, a= 12.489(1), b= 18.5194(1),c=13.399(1)A,β=92.9(1)°,V=3095.2A3,Dc=1.868g/cm3 and Z=2. The structure was solved by Patterson and Fourier methods,and refined by full matrix least squares method to R=0.078 for 1619 observed reflections with I>3σ(I).The molecule of the complex is a dimer located at the crystallographic center and each Gd(Ⅲ) atom is eight-coordinated with the coordination polyhedron being a distorted square antiprism.     

CRYSTAL STRUCTURE OF ORGANOMETALLIC COMPLEX [Zn（pom）2Br2]

<正> Organometallic complex [Zn (pom)2Br2] (pom = 3-M ethyl-4-Ni-tropyridine-1-Oxide), C12H12Br2N4O6Zn, MT = 533. 44, triclinic, P1, a = 11. 450 (3), b = 13. 027(2), c=6. 605(1)A, α=101. 25(1),β=96. 96(2), γ=108. 06 (2)°,V = 901.2(4)A3, Z = 2, Dc=1. 97 gcm-3,λ(MoKa) = 0. 71069A , F(OOO) = 520, μ= 58. 21cm-1, final R = 0. 040 for 2192 observed reflections, T = 296K. The compound is a mononuclear complex, containing a tetrahedrally coordinated zinc atom.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE HEXANUCLE-AR DIAZENIDO-OXOMOLYBDATE [(n-C_4H_9)_4N]_3[Mo_6O_(18)-(N_2C_6H_3-2,4-(NO_2)_2]

<正> Crystal of the title complex [(n-C4H9)4N]3[Mo6O18(N2C6H3-2,4-(NO2)2](Mr= 1710. 5) is orthorhombic with space group P21cn (Pna21), a = 17. 304(3), b = 17.580(2), c=24. 355(4) (?), V = 7409(2)(?)3, Z = 4, Dc=1. 60g/ cm3, μ=10. 29cm-1, F (000) = 3647. The structural solutions and refinements based on 3900 reflections (I≥3σ(I)) converged at R = 0. 0575, Rw =0. 0498. The atoms of Mo(3), Mo(4), O(1), O(5), O(9), O(11) and the [N2C6H3-2,4-(NO2)2] unit in the complex anion locate approximately in a plane about which the complex anion is nearly symmetrical.     

THE SYNTHESIS AND X-RAY CRYSTAL STRUCTURE STUDIES OF (DI-3-INDOL YL )M ETH YLFERROCENE

<正> A novel anhydrous zinc chloride catalyzed condensation reaction of ferrocenealdehyde with indole in solid state gave the title compound (Di-3-indolyl) methylferrocene ((C8H6N)2CHC5H4FeC5H5) selectively, and its crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1, with cell parameters a = 9. 624(2), b = 9. 957(2), c=11. 295 (4)A,α=92. 17(2), β=92. 23(2), γ=111. 30(1)°, V=985. 4A3, Mr = 430. 33, Z = 2, Dx = 1. 44g/cm3,μ= 7. 8cm-1, F(000) = 444. The final R = 0. 056 for 3027 observed reflections.     

X-RAY STRUCTURE AND MOLECULAR MECHANICS CALCULA-TIONS OF N-(2-CHLOROPHENYL)-2-PYRIDINECAR-BOTHIOAMIDE

<正> C12H9N2SCl, Mr= 248. 74, monoclinic, P21/n, a = 3. 902(2), b = 11.547(1), c = 25. 132(4)(?), β =93. 71(2)°, V = 1131. 1(?)3, Z = 4, Dc = 1.461, Do= 1. 45gcm-3, λ(MoKα) = 0, 71073A, μ = 4.84cm-1, F(000) = 512, R = 0. 041 for 1755 unique observed reflections. In comparison of the title molecular structure with that of N-(2-methylphenyl)-2-Pyridinecarbothipamide, the difference is insignificant. Intramolecular hydrogen bonds and short contacts are formed to the utmost extent, and the intermolecular hydrogen bonds such as C - H… S and C-H…Cl play an important role in the molecular packing. Molecular mechanics calculations (MMPM) is informative on the feature of the molecular conformation observed.     

CRYSTAL AND MOLECULAR STRUCTURE OF 1-ETHOXYCAR-BONYLMETHYL-2 N-(DIMETHYLAMINO)THIOCARBONYL 3-PR-OPYL 2,4-DIOXO 1,3,2-BENZODIAZAPHOSPHORIN (1)

<正> The title compound,C17H24N3O4PS(Mr = 405. 42) ,is a new compound of six-membered benzoheterocycle in which the five atoms N(1),C(1),C(11),C(16) andN(2) are coplanar with the and groups in trans-cross conformations. The crystal belongs to triclinic system,space group P1,with cell parameters a = 8. 580(2),b = 10.015 (4),c= 11. 896 (4) A ,α= 90. 65(3) ,β= 105. 70(3). γ= 89. 52(3)% V = 983. 9 A3,Z=2,Dx = 1. 37g/cm3. The final refinement converged with R=0. 074,Rw = 0. 090.     

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.     

CRYSTAL STRUCTURE OF 3-NITRO-2, 6-BIS(4''''-BENZO-15-CROWN-5)-AMINOPYRIDINE POTASSIUM PICRATE HYDRATE METHANOL, (C_(33)H_(42)N_4o_(12)K)C_6H_2N_3o_7·H_2O ·CH_3OH

<正> The title compound, (C33H42N4O12K)C6H2N3O7·H2O·CH3OH,Mr = 1003. 98,space group P1,a=11. 458(2) ,b= 14. 565(6) ,c=15. 828(3) A ;α=63. 34 (2),β=74. 06(1),γ=81. 03(2)°,V=2268. 1 A3;Z = 2,Dx = l. 47g/cm3,λ=0. 71069 A (MoKa).The final R = 0. 041 for 1700 observed reflections (I≥3σ(I)). The molecule is sandwich-like, and the cation K+ is sandwiched between the two crown rings.     

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.     

SOLID STATE PHOTOCHEMICAL SYNTHESIS OF A NOVEL HOST COMPOUND METHYL 4-(DI-3-INDOLYL) METHYLBENZOATE AND X-RAY CRYSTAL STRUCTURE OF ITS 1:1 INCLUSION COM-PLEX WITH ACETONE

<正> A novel host compound methyl 4-(di-3-indolyl) methylbenzoate p-CH3OCOC6H4CH (C8H6N)2(3) was prepared by irradiation of the mixed crystals of methyl p-formylbenzoate (1) and indole (2.). The crystal structure of 1:1 inclusion complex (3' ) formed by compound (3) and acetone has been examined by X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1, with cell parameters: a = 9.902(3), b = 10. 626(2), c=12. 945(2) A , α=70. 69(2),β = 72.56(2), γ = 69. 53(2)°, V = 1177. 82(?)3, Mr = 438. 53, Z = 2, Dx = 1. 236g/ cm3, μ = 0. 75cm-1, F (000) = 464. The final R is 0. 041 for 2006 observed unique reflections. There are three main planes in one molecule of this compound, the dihedral angles between them are 62. 37°, 89. 12° and 83. 308, respectively.     

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.     

STRUCTURE OF N-(p-CHLORO )-PHENYL ZMINODIACETIC ACID

<正> N-(para-chloro)-phenyl iminodiacetic acid hydrate ethanol solvate ClC6H4N(CH2COOH)2· H2O·C2H5OH, Mr = 307.73, monoclinic, P21/n, Cu-Ka (λ=1. 5410(?)), a = 16. 732(1), b = 5. 337(1), c=16. 300(1)(?) ,β=108. 52(1)°, V = 1380. 1(?)3, Z = 4, Dc=1.481g.cm-3, * = 27. 172cm-1, F(000) = 648, final R = 0. 072 for 1610 observed reflections. The crystal structure consists of discrete molecule of N-(para-chloro)-phenyl iminodiacetic acid, hydrate as well as ethanol solvate. A big ring consisting of atoms O(3), C(3), C(4), N(1), C(2), C(1), O(2) and H(2) is nearly planar with the maximum deviation of the atom N(1) of 0. 54 (?). Owing to the intramolecular hydrogen bond O(2)-H(2)…O(3) , the bond C(3) -O(3) in the COOH group is longer than the bond C(3)-O(4).     

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.