CRYSTAL STRUCTURE OF Pt（dppe）（SPh）2

<正> Anaerobic reaction of Pt (dppe)Cl2 (dppe = Ph2PCH2CH2PPh2) with NaSPh and elemental selenium affords complex Pt(dppe)(SPh)2,which crystallizes in the monoclinic system space group C2/c with a=14. 392(7) ,b=16. 380(7) ,c=14. 266(5) A ,β=86. 44(4)°,V=3342(5) A3,Z = 4,Dc=1. 613g/cm3,and μ(MoKa) = 44. 813 cm-1. The final structural refinement converged with unweighted and weighted R factors of 0. 041 and 0. 057 for 2206 observed reflections (I>3σ(I)). X-ray analysis shows that the Pt atom in Pt(dppe)(SPh)2 is at the center of the approximately planar tetragon of two P atoms and two S atoms.     

CRYSTAL AND MOLECULAR STRUCTURE OF cis—（μ—PhS—（CH2）3SPh）PdCl2

<正> The title complex, C15S2Cl2H16Pd, Mr = 437. 73, crystallizes in monoclinic space group P21/c with a = 10. 177(2), b=10. 788(1), c= 15. 305(1) (?),β=102. 73(1)°, V = 1638. 1(?)3, Z = 4, Dx =1.77g/cm3, μ = 16.8cm-1, F (000) = 872. The final structure refinement converged with unweighted and weighted R factors of 0. 025 and 0. 033 for 2490 observed unique reflections. The complex has mononuclear structure with the ligand cis-chelated to the Pd(Ⅱ) atom.     

RESEARCH ON CRYSTAL STRUCTURE OF 4—AMINOBENZOPHENONE（ABP）

<正> 4-aminobenzophenone(ABP), (C6H5)CO(C6H4NH2),Mr= 197. 23, monoelinic, space group P21,a= 12. 036 (3), b = 5. 450 (7), c= 8. 299(2) A,β = 97. 86°,V = 539. 32(3) A3,Z = 2,DC = 2. 215,Dm = 1. 209g/cm3,λ(MoKa) = 0. 71073 A,F(000)= 208,μ=0. 722cm-1,R=0. 083,Rw = 0. 084 for 721 observed reflections. There exists a cleavage plane (100) in the crystal ABP.     

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 .     

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.     

STRUCTURE OF DIAQUO（N—p—METHYLPHENYL）IMINODIAC—ETATO COPPER（Ⅱ）

<正> Diaquo (N - p-methylphenyl) iminodiacetato Copper (Ⅱ) Cu-CH3C6H4N(CH2COO)2](H2O)2, Mr = 320. 79, orthorhombic,Pcab (No. 62 non-stamdard setting, symmetry code: x,y,z; 1/2 + x ,y , 1/2 + z; x; , 1/2 -y , 1/2 -z; y,z),a = 7. 612(2), b = 12.938(1), c=26.574(3)(?) , V = 2616. 9(2) A3, Z = 8, Dc=1. 628 Mg.m-3, Do = 1.63 Mg.m-3, μ(CuKα) = 2. 62mm-1, F(000) = 1320, T =298K, final R = 0. 049 for 1136 observed reflections. In the molecule, the Cu (1) atom is bonded to two carboxyl oxygen atoms O(1), O(2), and two oxygen atoms O(10), O(20) from two water molecules and an imino N(1) atom to form a distorted square pyramid, in which the O(20) atom occupies an axial position and bond length of Cu(1)- O(20) 2.315(?) shows Jahn-Teller effect.     

SYNTHESIS AND STRUCTURE OF （Me4N）[Mo（OC6H4S—o）3]

<正> (Me_4N)[Mo(OC_6H_4S-o)_3] ,Mr=542. 57,orthorhombic,space group Pnb21 with a = 22. 708(1),b = 9. 737(4),c=10. 486(2) A;V=2318. 6A3;Z=4,Dc = 1. 55g/cm3,final R=0. 064 and Rw=0. 074.μ=8. 3cm-1, F(000) = 1108,The atom Mo( V ) of the anion issix-coordinated to three oxygen and three sulfur atoms in a distorted octahedral geometry.     

CRYSTAL STRUCTURES OF [Bu4N]2[M2Ag3（ μ3—S）2（μ—S）4S2Et2dtc]（M=W,Mo）

<正> The title compounds were prepared from the reation of (NH4)2MS4 (M=W,Mo),AgNO3,NadtcEt2 and Et4NBr in CH3CN-H2O solution. The isomorphous compounds [Bu4N]2[W2Ag3S8Et2du] ( I ) and [Bu4N]2[Mo2Ag3S8Et2dtc] (Ⅱ) crystallize in triclinic space qroup Pi with the following crystal parameters:α=13. 043(4),b = 21. 640(6),c=10. 757(6)A ,α=95. 09(5),β = 91. 90(4),γ = 98. 57(3)°,Z = 2,V = 2987A3,Dc=1. 76g/cm3 for I 5;a= 12. 989(2) ,b=21. 574 (9) ,c= 10. 7/1(1) A .α= 95. 06(7), β=91. 61(4), γ=98. 52(2)°, Z = 2,V = 2961 A3.Dc= 1. 58g/cm3 for Ⅱ . The final R and Rw values are 0. 061 and 0. 072 for Ⅰ ,and 0. 062 and 0. 076 for Ⅱ The M2Ag3 (M = W, Mo) unit in anion M2Ag3S8Et2dtc forms a five-membered ring.     

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.     

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.     

MOLECULAR AND CRYSTAL STRUCTURE OF （（C6H5）3P）2Ag（CO2H）

<正> C_37 H_31 O_2P_2Ag, Mr = 677. 47. The crystal structure belongs to mon-oclicnic system with space group Cc. Cell constants a =24. 952(2), b = 9. 179(1), c = 15. 262(1) A ,β= 116. 34 (2)°, V= 3132. 9 (3) A3, Z = 4, Dc = 1. 436g/cm3, D0 = 1. 43g/cm3.The final R achieved is 0. 052 for 5677 observed reflections, F (000) = 673. Like other silver complexes, Ag ( I ) in the center of the complex is 4-coordinat-ed. Formic acid anion also acts as a bidentate ligand in this complex beside two triph-enylphosphine groups.     

STRUCTURE OF（C6H5COCHCOC6H5）SmI2（THF）3

<正> (C6H5COCHCOC6H5)SmI2(THF)3,Mr= 843. 75,triclinic space group P1,a=13. 274(3),b=9. 886(3),c= 12. 526(4)A,a= 110. 89(3),B=93. 98(2),y=85. 16(2) ,V=1528. 9(8)A3,Z=2,Dc=1. 83g/cm3, (MoKa) = 0. 71069A,u= 40. 3cm-1,F(000) - 810. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0.082(Rw= 0. 083). The central Sm(III) ion is coordinated by two iodine ions, two oxygen atoms from C6H5COCHCOC6H5 and three oxygen atoms from three THF molecules to form a distorted pentagonal bipyramid. The Sm-I distances are 3. 103 and 3. 092 A ,The Sm-O (O atom from C6H5COCHCOC6H5) distances are 2. 273 and 2. 307 A and the average Sm -O(THF) distance is 2. 500A.     

Synthesis and Crystal Structure of Tri—（2—mercaptopyridine N—oxide）bis（dimethyl sulfoxide） Dysprosium（Ⅲ）

A range of rare earth metal complexes of 2-mercaptopyridine N-oxide (Hmpo) have been synthesized, and studied by elemental analysis and IR spectroscopic technique. Crystal structure of Dy(mpo)3(DMSO)2 (DMSO = dimethyl sulfoxide) has been determined. The complex crystallizes in the triclinic system, space group Pī with lattice parameters: a = 9.602(3), b = 9.803(3), c = 15.498(5)A, α= 89.51(1), β= 85.73(1), γ= 62.99(1)°, Dc = 1.787 g/cm3, C19H24N3O5S5Dy, Mr = 697.21, Z = 2, F(000) = 690, μ = 3.321mm-1, the final R = 0.0237 and wR = 0.0587 for 4116 reflections with I>σ2(I). The coordination number of dysprosium Ⅲ is eight, and its coordination geometry is a somewhat distorted square antiprism with O(3), O(4), O(5), S(3) and O(1), O(2), S(1), S(2) at the tetragonal bases (dihedral angle between their mean planes is 2.9(1)0). Around the Dy atom, three five-membered ring planes (Dy, O, N, C, S) make the dihedral angles of 74.42, 11.31 and 83.72, respectively.     

CRYSTAL STRUCTURE OF A SILVER COMPLEX Ag（PPh3）2（S2P—（OCH3）2）

<正> The crystal structure of the title silver complex has been determined by the single crystal X-ray diffraction method.The white plate crystal is tri-clinic.space group P1 with a=12.289(1),b=13.330(2),c=14.846(1)A.α=59.78(1),β=70.33(1),γ=64.01(1)°,V=1867.9A3,Z=2,Dc=1.404 g/ cm3,Mr=789.6,F(000)=808,MoKa radiation,μ(MoKa)=7.891 cm-1,final R=0.049 and Rw=0.051 for 5753 observed reflections.The silver(I)is surrounded by two P and two S atoms in a distorted tetrahedral coordination.     

2—（2‘吡啶基）—5—甲苯并噻唑及其二氯二乙基锡（Ⅳ）络合物的结构以及抗

X－射线单晶衍射法测定了2－（2'-吡啶基）－5－甲苯并噻唑（I）及其二氯二乙基锡（IV）络合物（2）的结构，晶体（I）属单斜晶系，《空间群为P21／n，晶胞参数a=5.808(2),b=10.283(3),C=18.373(3)A,β=91.48(2)°，Z=4,Dc=1.370g.cm^-3，偏离因子R＝0．047。晶体（2）属单斜晶系，空间群p21/c,晶胞参数a=17.271(2),b=9.411(1),c=14.015(2)A,β122．98（1）°，Z＝4，D＝1．648g.cm^-3，偏因子R－0．047，络合物中Sn-N平均键长已达2．5－A，参考顺铂类药物研究经验，展望了抗肿瘤有机锡络合物发展的前景。     

CRYSTAL STRUCTURE OF ERBIUM（Ⅲ）COMPLEX WITH 1，3，5—BENZENETRICARBOXYLIC ACID

<正> The crystal structure of erbium (Ⅲ) complex of 1,3,5-benzenetricar-boxylic acid is reported. The title compound crystallizes in triclinic space group of P1 and cell parameters a = 7. 649(3) ,b= 9. 859(2) ,c= 11. 171 (3) A ;α= 106. 90(2),β= 104. 40(3),γ=107. 20(3)°;Z = 2;V = 716. 5A3.The final R and Rw are 0. 0328 and 0. 0338 respectively. The rare earth ion is nine-coordinated by four oxygen atoms from two carboxylato groups in two 1, 3, 5- benzenetricarboxylato groups and five aqua molecules, forming a distorted monocapped square antiprism. The Er-O distances fall in the range of 2. 327-2. 627A.     

SYNTHESIS AND CRYSTAL STRUCTURE OF V ^（v）O[N（CH2Ch2O）3]

<正> Reaction of ammonium metavanadate with triethanolamine in ethanol yields the title compound (2,2' , 2"-nitrilotriethoxy)oxo-vanadium (Ⅴ ). The crystal and molecular structure has been determined crystallographically. The complex V(v) O[N(CH2CH2O)3] crystallzes in the monoclinic system, space group P21, a = 7.140(1), 6 = 7.474(2), c=8.040(2) A ,β=92. 48(2)°, V=428. 7(1) A3, Mr= 213.1, Z = 2, F(000) = 220,μ= 10. 95cm-1, Dc= 1. 65gcm-3, final R= 0. 032 and Rw = 0. 034 based on 758 independant reflections with I>2σ(I). The vanadium center is in a distorted trigonal bipyramidal environment of a quadridentate chelating ligand and a terminal oxygen atom.     

Synthesis, Structure and Conductivity of （PyH）[Ni（dmit）2]2

A new molecular conductor (PyH)[Ni(dmit)2]2 (dmit = 4, 5-dimercapto-1, 3-dithiole-2-thione) has been prepared and its crystal structure has been determined. Crystallographic parameters for (PyH)[Ni(dmit)2]2: C17H6NNi2S20; triclinic system; P-1 space group; a = 5.9227 (4) , b =8.2279 (6), c = 16.7535 (9) A, a = 90.233 (5) , 0 = 92.107 (6) , y= 104.654 (6) ; V= 789.25 (9) A3; Z = 1; Dc = 2.068 g/cm3; F (000) = 491. The conductivity at one direction on (001) plane at room temperature was measured to be 0.13 ii^-cmf1. The resistivity-temperature curve in the temperature range of 90-290 K shows that this compound behaves as a semiconductor.     

CRYSTAL STRUCTURE OF 2，4—DINITROPHENYL—t—BUTYL NITRONE（DNPBN）

<正> C11H13 N3 O5·t-Bu- N = CHC6H3(NO2)2,Mr = 267. 27, Monoclinic space group C2/c,a= 18. 546(3),b = 5. 729(1),c= 27. 479(5) A,β= 118. 42(1)°/,F = 2567. 6(9)A3,F(000) = 1120,Z=8,Dx=1. 38g/cm3. The structure of DNPBN is akin to that of PBN reported by us except for shorter N - O and C = N bonds.     

Synthesis and Crystal Structure of Bis（nitrate）bis（N—n—octyl—α—pyrrolidone）uranyl（Ⅱ）

The crystal structure of the title compound UO2(NO3)2[CH2(CH2)2CONC8H17] was determined by single-crystal X-ray diffraction. Crystal data: triclinic, space group P ī, a = 7.456(2), b = 8.371(2), c = 13.470(3)A, α = 95.66(1), β = 94.64(2), γ = 102.67(2)°, C24H46N4O10U, Mr = 788.68, V = 811.73A3, Dc = 1.613 g/cm3, Z = 1, F(000) = 390, μ = 5.052 mm-1, the final R = 0.0256 and wR = 0.0568 for 2826 observed reflections I>2σ(I). The central uranyl ions are coordinated by six oxygen atoms. Two of them are from the carbonyl groups of N-octyl--pyrrolidone molecules, and the other four from two nitrate groups.