Synthesis,Structure,Characterization and Electrochemistry of a New Din

Reaction of Et4NCl, NaSCH2COOMe and W(CO)6 in MeCN affords a new dinuclear tungsten(0) complex [Et4N]2[W2(CO)8(SCH2COOMe)2] (1). The crystal and molecular structure has been determined by X-ray single crystal diffraction. 1 Crystallized in the triclinic, space group P with a=11.141(7), b=10.267(4), c=10.798(3)(); α=93.96(3), β=96.88(4), γ=114.97(5)°; V=1003()3, Z=1, Dc=1.76 g/cm3, μ=60.1 cm-1, R=0.042 and Rw=0.050 for 2967 independent reflections with I>3.0 σ(I). 1 contains a WS2W planar core with nonbonding W...W distance of 3.9611(5)(), and its IR, 13C NMR, and cyclic voltammetry were measured and discussed.     

Synthesis, Structure, Characterization and Electrochemistry of a New Dinuclear W(0)-complex [Et4N]2[W2(CO)8(SCH2COOMe)2]

Reaction of Et4NCl, NaSCH2COOMe and W(CO)6 in MeCN affords a new dinuclear tungsten(0) complex [Et4N]2[W2(CO)8(SCH2COOMe)2] (1). The crystal and molecular structure has been determined by X-ray single crystal diffraction. 1 Crystallized in the triclinic, space group P with a=11.141(7), b=10.267(4), c=10.798(3)(); α=93.96(3), β=96.88(4), γ=114.97(5)°; V=1003()3, Z=1, Dc=1.76 g/cm3, μ=60.1 cm-1, R=0.042 and Rw=0.050 for 2967 independent reflections with I>3.0 σ(I). 1 contains a WS2W planar core with nonbonding W...W distance of 3.9611(5)(), and its IR, 13C NMR, and cyclic voltammetry were measured and discussed.     

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.     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound [Et4N ] 2 [Mo2 (CO) 8 (SC6H4-OCH3-p) 2]

Reaction of Mo(CO)6 with p-H3CO-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2 (CO)8 (SC6H4-OCH3-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C38H54Mo2N2O10S2, Mr = 954.87, triclinic, P-1, a = 11.348 (7), b =11.616(5), c=10.065(7) A, a=113.86(4), β=111.39(5), γ=91.92(5)°, V=1104.0(1) A3, Z=1, Dc=1.44 g/cm3, F(000)=492, μ=7.0cm-1, Final R=0. 046 and Rw=0. 049 for 2657 reflections with I＞3. Oσ(I). The X-ray structure analysis revealed that the Mo2S2 core of 1 is planar. The geometry around each Mo atom is a distorted octahedron, the two octahedrons form an edge-sharing bioctahedron. The bond. In addition, the 95Mo NMR chemical shift of 1 is discussed.     

The Molybdenum（0）Complex [Et4N]2[Mo2（CO）6（pys）2]（pys=Pyrindine—2—thiol

The title compound tetraethylammonium hexacarbonylbis(μ-pyridine-2-thiolato-S∶S) dimolybdenum [Et4N]2[Mo2(CO)6(pys)2] crystallizes in the monoclinic, space group, P21/c with a=13.217(2), b=21.648(2), c=27.193(6)(), β=82.52(2)°, V=7714.6()3, Z=8, Mr=840.77, Dc=1.45 g/cm3, μ=7.8 cm-1, R=0.038 and Rw=0.040 for 6082 reflections with I≥3σ(I). X-ray crystal structure study reveals that the asymmetric unit of the title compound is comprised of two independent formulations of the molecular formula. Each dianion has approximate C2 symmetry and the dimetallic Mo2S2 core adopts a "butterfly" conformation with a dihedral angle between the halves of 139.3(1)° for the first independent anion and 142.8(1)° for the second one. The two pyridine rings lie on the same side of the molecule in a cis arrangement and the Mo...Mo separations are 3.76(1) and 3.838(1)().     

Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato-Bridges [Et4N] 2 [Mo2 (CO) 8 (SC6H4-Cl -p) 2]

Reaction of Mo (CO)6 with p-Cl-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum (0) compound [Et4N]2 [Mo2 (CO)8 (SC6H4-Cl-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C36H48Cl2Mo2N2O8S2, Mr= 963.71, monoclinie, P21/c, a=9. 269(4),b=13.750(3), c=17.466(6) A ;β=104.84(3)°; V=2151.8(3) A3; Z=2; Dc=1.49 g/cm3; F(000)=984; μ=8.3 cm-1; MoKα radiation (λ=0. 71073A ); Final R = 0. 055 and Rw=0. 065 for 3287 reflections with I＞3. 0σ(I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distance is 4. 014(2) A , and this obviously indicates the absence of Mo-Mo bond.     

Synthesis and Structure Characterization of Aqua-（μ2-carbonato-O,O′）-（2,2′-bipyridyl）-copper（Ⅱ） Dihydrate

Under hydrothermal conditions the reaction of cis-aconitic acid with Cu2(OH)2CO3 and bipy (bipy = 2,2'-bipy) in H2O/DMF (3:2) afforded a neutral mononuclear compound [Cu- (bipy)((2-CO3)(H2O)](2H2O, which has been structurally characterized by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic, space group Pī with a = 8.3950(5), b = 8.7974(5), c = 9.4496(3)（A。）, α = 98.270(3), β = 93.014(3), γ = 100.068(3)°, V = 677.83(6) （A。）3, Dc = 1.635 g/cm3, Z = 2, C11H14CuN2O6, Mr = 333.78, μ = 1.637 mm－1, λ(MoKα) = 0.71073 （A。）, F(000) = 342, the final R = 0.0616 and wR = 0.1273 for 1621 observed reflections with I > 2σ(I). The structure of the complex contains a distorted square pyramidal core with a bipy, a carbonate anion and a water molecule coordinating to a CuⅡ atom. The dihedral angle between the two planes composed of N(1)N(2)Cu(1) and O(1)O(3)Cu(1) is 21.73(8)°. The intermolecular hydrogen bonds (O…O) are observed in the crystal structure.     

Synthesis,Crystal Structure and Antiproliferative Activity of 2-（（（5-（（（5,7-Dimethyl-[1,2,4]triazolo-[1,5-a]pyrimidin-2-yl）thio）methyl）-4-phenyl-4H-1,2,4-triazol-3-yl）thio）methyl）-4Hchromen-4-one Methanol Solvate

The novel crystal of the title compound 2-(((5-(((5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl)thio)methyl)-4-phenyl-4H-1,2,4-triazol-3-yl)thio)methyl)-4H-chromen-4-one methanol solvate(C27H25N7O3S2, Mr = 559.66) has been prepared and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monocline system, space group P21/c with a = 11.9879(9), b = 14.0743(10), c = 15.9706(11), β = 98.509(2)°, V = 2664.9(3)3, Z = 4, Dc = 1.395 g/cm3, F(000) = 1168, μ = 0.116 mm-1, MoKa radiation(λ = 0.71073), R = 0.0652, and wR = 0.1425 for 5220 observed reflections with I 2σ(I). X-ray diffraction analyses reveal that the molecule adopts a C-shape. The planes of the benzopyrone and triazolopyrimidine were nearly parallel to each other, with a dihedral angle of 1.21(3)°. Intramolecular and intermolecular hydrogen bonds together with π-π interations are found to exist in the structure. The results of MTT assay indicate that the title compound displays excellent antiproliferative activity against two human cancer cell lines.     

Synthesis,Crystal Structure,and Antitumor Activity of 1-（4-Methoxybenzylidene）-2-（1-phenyl-6-trifluoromethyl- 1H-pyrazolo [3,4-d] pyrimidin-4-yl）hydrazine Monohydrate

The novel title compound 1-(4-methoxybenzylidene)-2-(1-phenyl-6-trifluoromethyl-1H-pyrazolo[3,4-d]pyrimidin-4-yl)hydrazine monohydrate(C20H15F3N6O·H2O, Mr = 430.40) has been synthesized by a four-step procedure including the cyclization, chlorination, hydrazinolysis and condensation reaction, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pbca with a = 8.3779(13), b = 17.607(3), c = 26.774(4) , V = 3949.2(11) 3, Z = 8, Dc = 1.448 g/cm3, μ = 0.117 mm–1, F(000) = 1776, the final R = 0.0553 and wR = 0.1516 for 2354 observed reflections with I 2■(I). X-ray diffraction analysis reveals that the title compound is almost coplanar except for the trifluoromethyl and phenyl moieties. In the crystal packing, the molecules are linked by intermolecular O(1W)–H(1WA)···N(2), O(1W)–H(1WA)···N(4) and N(5)–H(5A)···O(1W) hydrogen bonds via water molecules and stacked through π-π stacking interactions. The preliminary bioassay suggested that the title compound exhibits relatively good antitumor activity against HepG2 and BCG-823.     

CRYSTAL STRUCTURE AND POWDER DIFFRACTION OF Na5Y（WO4）4

<正> Title compound Na5Y (WO4)4 (Mr = 1195. 24) crystallizes in the space group I41/a with the cell parameters a= 11. 447(7), c= 11. 336(1) A , Z = 4, V = 1485(2) A3, A = 5. 34 g/cm3. A(MoKα) = 0. 71069 A. F(000) = 2702, final R = 0. 045,Rw = 0. 054 for 936 observed reflections with I≥3σ(I). The title compound has a scheelite structure.In this paper, we also give the X-ray powder diffraction data of Na5Y(WO4)4 obtained by using a D/max-ra type diffractometer.     

Synthesis and Structure of Tungsten Carbonyl Compound with 2-Mercapto Pyrimidine [Et_4N] [W (CO)_4(SC_4H_3,N_2) ]

1INTR0DUCTI0NLowva1encemolybdenum/tungstencomp1exeswiththiolatoligandsareusefulforthestudiesonsyntheticandstructuralchemistry.Inrecentyearswehavesynthe-sizedandcharacterizedaseriesofdinuclearMo-SRc0mpoundscontainingaplanarMoSzMocorewithamon0dentatethiolatoligand"-"anda"butterfly"M0S2Mocorewithabidentatethi0latoligand"=."H0wdoesmultidentateliganddo"hasnaturallyattracted0urinterest-2-mercaptoPyrimidine(PymS)wasusedasamultidentateligandtocarry0utsynthesisexperiment.unexpectedly,whichgavea…     

Synthesis and Structure of a New Dinuclear Tungsten(Ⅰ) Compound with Phenylselenol Ligand, [W2(SePh)2(CO)6(MeCN)2]

The reaction of Et4NCl, C6H5SeNa and W(CO)6 in MeCN afforded a new dinuclear tungsten(Ⅰ) complex W2(SePh)2(CO)6(MeCN)2 1 (Mr = 929.98). The crystal structure has been determined by X-ray single-crystal diffraction. 1 Crystallizes in monoclinic, space group P21/n with a = 7.501(1), b = 18.387(2), c = 9.491(1) (A), β = 103.897(2)°, V = 1270.6(3) (A)3, Z = 2, Dc = 2.431g/cm3, μ = 119.50 cm-1, F(000) = 852, R = 0.0695 and wR = 0.1724 for 2220 independent reflections with I ＞ 2σ(Ⅰ). The X-ray structure analysis reveals that the W2Se2 core of 1 is planar with W-W bond length of 3.0433(13) (A) and W-Se of 2.5922(17) (A).     

Synthesis and Structure of a New Dinuclear Tungsten(I) Compound with Phenylselenol Ligand,[W_2(SePh)_2(CO)_6(MeCN)_2]

1 INTRODUCTION The chemistry of complexes containing lowvalence molybdenum and tungsten metal atoms has increa- singly attracted the attention of chemists and bioinor- ganic chemists due to their significance for studies on metal enzymes[1～5]. Since the dinuclear molybde- num and tungsten (0, I) oxygen family carbonyl complexes, [M2(μ-XR)a(CO)bLc]2-, 0 (M = Mo, W; X = O, S, Se, Te; b = 8, 6; L = MeCN; c = 0, 2), were synthesized and their interesting twoelectron- transfer charact…     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound[Et4N]2[Mo2(CO)8(SC6H4-CH3-p)2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅｔｈｉｏｌａｔｅｌｉｇａｎｄｗａｓｉｎｔｒｏｄｕｃｅｄｉｎｔｏｍｏｌｙｂｄｅｎｕｍｃａｒｂｏｎｙｌｃｏｍｐｏｕｎｄｉｎ1 984 [1],ｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｎｌｏｗ ｖａｌｅｎｃｅＭｏ -ＳＲｃｏｍｐｏｕｎｄｓｈａｓｒｅｃｅｉｖｅｄａｔｔｅｎｔｉｏｎｆｏｒｔｈｉｓｋｉｎｄｏｆｌｏｗ ｖａｌｅｎｃｅｃｏｍｐｏｕｎｄｓｐｏｓｓｅｓｓｃｅｒｔａｉｎａｄｖａｎｔａｇｅｏｎｃｏｍｐｏｕｎｄｓｙｎ ｔｈｅｓｉｓ,ｍｏｌｅｃｕｌｅｓｔｒｕｃｔｕｒｅａｎｄｐｈｙｓｉｃａｌａ…     

Synthesis and Structure of Dimolybdenum Carbonyl Thiolate Compound [Et4N]2[Mo2（CO）8（SC6H4—CH3—m）2]

1 INTRODUCTION In 1984, thiolate ligand was successfully introduced into molybdenum carbonyl compound by the reaction of Mo(CO)6 with [Et4N]SR( R = C6H5, But) in a moderate condition[1]. From then on, a series of dinuclear molybdenum(0) carbonyl thiolate compounds have been synthesized and characterized by using a variety of thiolate ligands in our research group. It was found that a planar Mo2S2 unit is in the compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-p)2][2] (2) and a "butterfly" t…     

Synthesis and Structure of 4，5－bis（2，4－Dinitrophenylthio）－1，3－Dithiole－2－Thione

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ４，５－ｂｉｓ（２，４－Ｄｉｎｉｔｒｏｐｈｅｎｙｌｔｈｉｏ）－１，３－Ｄｉｔｈｉｏｌｅ－２－ＴｈｉｏｎｅＱｕＺｈｅｎｇ；ＣａｉＪｉｎｇ－Ｈｕａ；ＦａｎｇＱｉ；ＹｏｕＸｉａｏ－Ｚｅｎｇ（Ｃｏｏｒｄｉｎａｔｉ...     

金属-金属键形成反应的研究: [η^5-RO~2CC~5H~4(CO)~3M]~2Hg(R=Me,Et;M=Cr,Mo,W)的合成及鉴定

η^5-RO~2CC~5H~4(CO)~3MNa与R^1HgCl,R^1=Me, Et, Ph)可发生一种非预期的金属键形成反应, 生成[η^5-RO~2CC~5H~4(CO)~3M]~2Hg(R=Me,Et;M=Cr,Mo,W)。对反应中间物η^5-EtO~2CC~5H~4(CO)~3MoHgPh的研究表明: 反应是按缩合及对称化两步机理进行的。(R=Et,M=Mo)属三斜晶系, 空间群P-1。a=0.6333(1), b=0.7712(1), c=1.4204(4)nm; a=77.31(1),β=74.51(2), γ=68.72(1)^°; V=0.61714nm^3;Z=1;D~x=2.246g/cm^3;R=0.044。