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.     

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.     

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 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 AND OPTICAL PROPERTIES OF TRIHYDROXYL METHYL-AMINOMETHANE(TAM),H_2NC(CH_2OH)_3

<正> H2NC(CH2OH)3,Mr=121.14, orthorhombic, space group P21cn a= 7.786(2), b=8.785(1), c=8.835(1)A,V=604.4(3)A3, Do=1.326g.cm-3, Z=4. Dc= 1.331g.cm-3, F(000)=264e,λ(MoKα)=0.71073A, graphite monochromator, R= 0.049, Rw=0.057 for 651 observed reflections.     

Crystal Structure of Copper（ Ⅱ）Complex with 3—Hydroxyl—1,5—diazaylo

Crystal structure of copper (II) complex with a new aminocarboxylate ligand, 3-hydroxyl-1, 5-diazacycloheptane-N,N-diacetate, C9H14CuN2O5.H2O, Mr=311.78 is reported. It crystallizes in orthorhombic Pna21 with a=13.340(4), b=8.127(1), c=10.583(4) , V=1147.2(7)3 , Z=4, Dc=1.805g/cm3, μ=19.287cm-1 (MoKα), F(000)=644. The final R and Rw are 0.049 and 0.065 for 888 observed reflections with I≥3σ(I). The result of X-ray structure determination shows that the Cu(Ⅱ) forms a planar complex with two oxygen atoms and two nitrogen atoms of the ligand.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Ta_3(Te_2)_6

<正> Ta3(Te2)6, Mr = 2074. 04, tetragonal, P4/ncc, a = 9. 204(1) A , c=20,401(8) A, V=1728. 3 A 3, Z = 4, Dc = 7. 97g/cm3, λ(MoKa) = 0. 71073 A . μ= 386, 3cm-1,F(000) = 3372, T= 296K , R= 0. 027, Rw = 0, 029 for 493 observed unique reflections. The structure is composed of infinite [TaTe4] chains along the e axis. In these chains, the Ta sequences distort in such a way that linear Ta, clusters are formed.     

STRUCTURE OF 1，2，4—TRIPHENYLCYCLOPENTA—1，3—DIENE

<正> C23H18, Mr = 294. 40, orthorhombic, Pbca, a = 20. 927(9), b = 20. 695(9), c = 7. 570(2)(?), V = 3278(2)(?)3, Z = 8, Dc=1.19gcm-3, μ(MoKα) = 0. 63cm-1, F(000) = 1248, R = 0. 057 for 1109 observed reflections with I>2. 5* (I). The dihedral angles between a given phenyl ring and the cyclopentadienyl plane are 28. 2, 50. 2 and 21. 8°, respectively. The structure is stabilized through weak stacking of the cyclopentadiene moieties in crystals.     

CRYSTAL STRUCTURE OF RhCl(dppm)_2·H_2O

<正> C50H46OP4ClRh, RhCl(dppm)2 · H2O, Mr = 922. 2, monoclinic, P21/2, a=10. 532(3), b=22.574(8), c=18. 641(8) A, β=93. 41(3)°, V = 4424 (3) A3, Z = 4, Dc=1. 386 g. cm-3, λ(MoKα) = 0. 71073A , F(000) = 1904. The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares to final R = 0. 037 and Rw = 0. 036 for 3432 (F> 6. 0σ(F) ) observed reflections. The structure of the title compound contains RhCl-(dppm)2 and non-coordinated H2O molecules. The rhodium atom is coordinated by one chlorine atom and four phosphorus atoms of two DPPM ligands forming a tetragonal pyramidal configuration.     

STRUCTURE OF BIS(TETRAETHYLAMMONIUM)BIS[BIS(PHENYLTHIOLATO) (μ-SULFIDO)-IRON(Ⅲ)],(Et4N)2[Fe2S2(SC6H5)4]

<正> Mr= 873.02, orthorhombic P21212, a= 16.153(3), b= 15.718(2), c= 8.847(3) A, V= 2246.2(14)A3, Z=2, Dx? 1.291gcm-3, MoK(?), radiation, λ= 0.71069A, μ= 9.417mm-1, F(000)= 924, R(Rw)= 0.073(0.069) for 1936 observed reflections. The structure of the anion contains a FesSz core, in which each iron atom is coordinated by two μ2-S atoms and two thiolate sulfur atoms to form a distorted tetrahedron.     

Molecular and Crystal Structure of Cinnam ylidene Acetophenone

１　ＩＮＴＲＯＤＵＣＴＩＯＮＣｕｒｒｅｎｔｌｙ，ｃｏｎｓｉｓｔｅｎｔｅｆｆｏｒｔｓｈａｖｅｂｅｅｎｍａｄｅｔｏｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｆｏｒｇａｎｉｃｎｏｎｌｉｎｅａｒｏｐｔｉｃａｌ（ＮＬＯ）ｍａｔｅｒｉａｌｓ〔１〕．Ｓｏｍｅｏｆｃｉｎｎａｍｙｌｉｄｅｎｅａｃｅｔｏｐｈｅｎｏｎｅｄｅｒｉｖａｔｉｖｅｓｈａｖｅｆａｉｒｌｙｓｔｒｏｎｇｓｅｃｏｎｄｈａｒｍｏｎｉｃｇｅｎｅｒａｔｉｏｎ（ＳＨＧ）ａｎｄｔｈｅｒｅｆｏｒｅａｒｅｐｏｔｅｎｔｉａｌｕｓｅｆｕｌｉｎＮＬＯｆｉｅｌｄｓ．Ｄｕｒｉｎ…     

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.     

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 DINUCLEAR IRON CARBONYL DERIVATIVE (μ-SC_6H_5) (μ-P (SC_6H_5)_2) Fe_2 (CO)_5 (P-(SC_6H_5)_3)

<正> The reaction of Fe3(CO)12 with P(SPh)3 yields the tile compound. C41H30Fe2O5P2S6, Mr = 968. 65, monoclinic, space group, P21/n, a = 14. 449(9), b = 18. 046(11), c=16.871(10)(?), β=98. 76°, V = 4348(?)3, Z = 4, Dc=1. 480g/ cm3, λ(MoKα) = 0. 71073(?) The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares procedure to R = 0.084, Rw = 0.144 for 4059 reflections. Fe(1)-Fe(2) = 2. 576(6), Fe(2)-P(2) = 2.194(9)(?). The dihedral angle between the Fe(l)SFe(2) and Fe(1)PFe(2) planes is 81. 9°. The other one (dihedral angle between SFe(1)P and SFe(2)P planes) is 75. 2°.     

SYNTHESES OF TUNGSTEN COMPLEXES WITH o-MERCAP-TOPHENOL.CRYSTAL STRUCTURE OF (Ph_4P)[WO(OMe)(mp)_2]

<正> Reaction of WCl6, mpH2 o-mercaptophenol) and MeONa in the presence of Ph4PBr gave complexes (Ph4P)[W(mp)3] (1) and (Ph4P) CWO(OMe) (mp)2] (2). Crystal data complex (2), C37H31O4PS2W, Mr = 818. 61, monoclinic, space group P2/a, a=26. 555(3), b=9. 634(1), c=13. 523(7) A. β=94. 68 (2)°, V=3448. 1 A3. A=1. 58 g/cm3, Z = 4. λ(MoKα)=0. 71073 A , μ= 36. 2 cm-1, F(000) = 1624, T=296K, final R(Rw) = 0. 068(0. 070) for 3929 observed reflections. The WO4S2 core is arranged in a distorted octahedral geometry.