SYNTHESIS AND CRYSTAL STRUCTURE OF A TRITUNGSTEN CLU-STER COMPOUND H[W_3O_2(O_2CCH_3)_9]·5H_2O

In this paper we report the structure of another new W3 cluster compound H[W3O2(O2CCH3)9]·5H2O prepared by the method reported previously. The title compound crystal lizes in monoctinic system, space group P21 with cell dimensions: a = 8. 237(3),6=13. 273(2),c=14.508(4)A,β=92.97°(3),V=1584A3.Z=2,and Dc=2. 529g/cm3.The average W - W, W -U_3-O,W -Oac and W -Ot distances are 2. 775, 2. 01,2. 09 and 2. 04 A, respectively.     

SYNTHESIS AND CRYSTAL STRUCTURE OF TRINUCLEAR CLUSTER [M_3O_2(O_2CCH_3)_6(H_2O)_3]ZnBr_4·8H_2O(M=0. 33Mo+0. 67W)

<正> C12H40O25Br4MoW2Zn, Mr=1432. 75,Monoclinic,Space group C2/c,a= 13. 239(2),b= 16. 215(3),c= 17. 670(3) A ,β= 105. 53(2) ,V=3654 A3,Z= 4,μ= 64. 0cm-1,λ(MoKa) = 0. 71073 A , F (000) = 2688, Dc = 2. 605g/cm3. Final R = 0. 042,Rw = 0. 057 for 2688 observed independent reflections.     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [CrMo_3 (μ_3-O)_3(μ-O)(μ-O_2CCH_3)_5(O_2CCH_3)_3]Na2 · H_2O

<正> The title complex C CrMo3 (μ3-O )3 (μ-O) (μ-O2CCH3 )5 (O2CCH3)3]2Na2 · H2O (Mr=1814. 32) crystallizes in monoclinic, space group P21/ n with a=11.209(5), b=18. 05(1), c=14. 44(1) A , β= 98. 30(5)°. V=2890 (3) A3, Z=2, A = 2. 08 g/cm3, F(000) -1780, Final R = 0. 049, Rw = 0. 058 for 2622 independent reflectons with I>3σ(I). The complex anion contains two Mo3O4 cores which connect two chromium atoms through four μ3-O atoms and eight bridging CH3COO- groups. Each of the Cr atoms and the Mo atoms is coordinated by six oxygen atoms. The anions are linked by Na cations to form one-dimensional infinite chain structure.     

CRYSTAL STRUCTURE OF HETEROPOLY TUNGSTOANTIMONATE (NH4)_12[Cu3(H_2O)_3Sb_2W_18O_56]·9H_2O

<正> (NH4)12[Cu3(H2O)3Sb2W18O66].9H2O,Mr = 5232.06, orthorhombic, space group Pmcn, a=15.423(4), b = 19.307(6), c = 30.275(6) A,V= 9015.0 A3, Z=4,Dc=3.866 g/cm3,u= 247.569 cm-1,R = 0.064 for 2652 observed reflections [I> 3σ(I)]. X-ray analysis shows that the heteropoly anion of the title compound consists of two α-β-SbW9O33 subunits, which are derived from the a-Keggin structure by loss of one W3O13 group constituted by three edge-sharing WO6 octahedra, merged together through the connection with three CuO4(H2O) units with the O atoms shared with the W atoms.     

SYNTHESIS AND STRUCTURE OF A MIXED-VALENCE HEXAMOLYBDENUM COMPLEX [Et_4N]_2[Mo_6O_(19)H_4]

A hexamolybdenum complex, [Et_4N]_2[Mo_6O_(19)H_4] crystal, withpentavalent and hexavalent molybdenum has been obtained in the solution ofDMF and CH_3OH as organic solvents using MoCl_5 as a starting material. Thecrystallographic parameters obtained by X-ray diffraction analysis are:crthorhombic, a=10. 757(3), b=10. 763(2), c=14. 238(4)A, =1648. 9A~3; Z=2; spacegroup Pnnm; final R=0. 047; final Rw=0. 051~(**)     

CRYSTAL STRUCTURE OF [Sm(CCl_3COO)_3(H_2O)_2]·2H_2O

<正> Biaqua-trichloroacetate-samarium dihydrate, [Sm(CCl3COO)3(H2O)2]-2H2O, Mr=707.54, orthorhombic, space group Pnne, with a = 19.158(5), b = 22.176(4), c= 9.798(4)A, Z= 8, V= 4162.7A3.F{000)= 2696,λ(MoKα)=0.71069A, Dx = 2.258 g/cm3, final R=0.061. The title compound has non-molecular structural character, and its structural units Sm(μ-CCl3COO)s/2-(H2O>2 constitute 2-dinensional infinite chains of Sm(μ-CCl3COO)4Sm(μ-CCl3-COO)2Sm.The Sa(Ⅲ) atom in each unit is bound to two O atoms from aqua-molecules and six 0 atoms from six bridging CCl3COO groups (four of which are shared with the SB atom of another unit, two shared with the Sm atom of a third unit) forming a square antiprism.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Mo_2OS(μ-S)_2[S_2CNC_4H_8]_2

Mo_2OS(μ-S)_2[S_2CNC_4H_8]_2, Mr=612.61, triclinic, PI, a=8.666(2)(?), b=17.366(6)(?), c=6.708(1)(?), α=98.29(2)°, β=97.27(2)°, γ=79.36(2)°, V=976.5(5)(?)~3, Z=2, Dc=2.03g/cm~3, MoKα(λ=0.71069(?)), μ=19.75cm~(-1), F(000)=588, Final R=0.064, Rw=0.073 for 1517 unique intensity data (I>3σ(I)). The binuclear unit of [Mo_2OS_3] has a new asymmetrically terminal coordinated configuration with Mo-Mo distance of 2.807(3)(?).     

SYNTHESIS, STRUCTURE AND PROPERTIES OF Na_3[V_2O_3(nta)_2]·5H_2O

<正> Compound Na3 [V2O3 (nta )2 ]·5H2O (1) (ntaH3 = N (CH2CO2H)3) has been prepared by reduction of a mixture of (NH4)2[VO(O2)2Cl] and H3(nta) in H2O with Na2S2O4. The compound crystallizes in the triclinic system, space group P1 with Mr = 685. 2, a = 11. 050(6), b=12. 179(4), c=9. 792 (3)A,α=111.71(2),β= 98. 23(3), γ= 89. 36(2)°, Z=2, V = 1210. 5A3,λ(MoKa) = 0. 71069 A, F(000) = 694 and DC = 1. 880g/cm3. The structure was solved by direct methods and refined by full-matrix least squares to final R and Rw values of 0. 055 and 0. 065, respectively.The structure of the anion can be considered as two [VO(nta)] fragments connected by one μ2-O atom. Each vanadium atom in the fragment is coordinated by one vanadyl oxygen atom, one bridging-oxygen atom, three oxygen atoms and one nitrogen atom from (nta) ligand in a distorted octahedral geometry. In this paper, we have studied the conversion of compound 1 to mononuclear compound Na2[VO(O2) (nta)]·5H2O (2) by oxidation with hydrogen peroxide, as well as thei     

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.     

CRYSTAL STRUCTURE OF COMPLEX OF ERBIUM(Ⅲ) AND QLYCINE,[Er(GLy)_2(H_2O)_4]_2(ClO_4)_6·4(C_4H_8O_2)

<正> The crystal structure of [Er(Gly)2 (HaO)4]2(ClO4)6.4(Dio) (Gly= NH2CH2COOH; Dio=dioxane) has been determined belonging to triclinic system with space group P1.The final R was 0.055. The carboxyl groups of Gly are associated to Er(Ⅲ) atoms to act as the bidentate bridging ligands.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A TUNGSTEN-COPPER-SULFUR CLUSTER [Et_4N]_2[WCU_3S_4(S_2CNEt_2)_3]

<正> [Et4N]2 [WCu3S4 (S2CNEt2)3], Mr = 1172. 01, orthorhombic, space group P212121 with a=12. 858(9),b=13. 204(5) ,c=29. 501(9) A ,V=5008. 7 A3, Z = 4, Dc = 1. 55gcm-3, μ(MoKa) = 40. 3cm-1. The final R and Rw are 0. 069 and 0. 075, respectively, for 3072 observed unique reflections. The anion contains a slightly distorted WS42~ tetrahedron coordinated by three CuS2 CNEt2 units,with four metal atoms lying in a plane.     

TRINUCLEAR BASIC CARBOXYLATE COMPOUNDS OF TRANSITION METALS PART 2. SYNTHESIS AND CRYSTAL STRUCTURE OF [Fe_3O (EtCO_2)_3(MeCO_2)_3(H_2O)_3]NO3·H_2O

<正> The title complex crystallizes in monoclinic system,space group C 2/m with α=19. 870(5),b=13. 070(2),c=18. 246(4)A ,β=134. 32(1)°,Mr = 707. 88, V=3390. 0A3.Z = 4,DC=1. 387g/cm3,F(000) = 1468,final R=0. 066 for 2244 independent reflections with Ⅰ >3σ(Ⅰ). The cation was shown to contain three Fe (Ⅲ) atoms at the apices of an equilateral triangle with a 3-O bridge.The Fe (1)-(μ3-O)and Fe(2)-(μ3-O) distances are 1. 907(6) and 1. 87(1) A , respectively. And mixed ligands of acetato and propionyloxy lato are bridged to each pair of the Fe(Ⅲ) atoms.     

SYNTHESIS AND CRYSTAL STRUCTURE OF HETEROPOLY MOLYBDOSILICIC LANTHANIDE K_(10)H_3[Pr(SiMo_(11)O_(39))_2]·18H_2O

The intensity data of the title complex were collected at a low temperature of -90℃. Thecompound crystallizes in the monoclinic space group P2_1/n, a = 17.504(2), b = 27.323 (5),c = 21 .616(4)A, β= 104.49 (2)°, Z=4. The structure was solved by Patterson and Fouriertechniques and refined by least- squares to an R = 0.088 for 8320 independent reflections.The central Pr ion is bonded to eight oxygen atoms from two molybdosilicic heteropolyligands to form a square antiprism. The Pr- O average distance is 2.44 (2)A. Both molyb-dosilicic heteropoly ligands are of a defective α- Keggin structure.     

CRYSTAL STRUCTURE OF [PdCl_2 (DMAF)_2]·C_7H_8

<正> C33H42 Fe2PdCl2N2 (dichloro-bis (dimethylaminomethylferrocene) pal-ladium(Ⅰ) toluene solvate) ,Mr = 755. 72,monoclinic,P21/c,a=7. 521(1),b= 11. 128 (2),c=19. 260(7) A ,β=91. 77(2)°,V=1611. 1A3,Z=2,Dc = 1. 56g·cm-3,D0 = 1. 58g·cm-3,μ=76. 3cm-1, The least-squares refinement gave a final R value of 0. 062 for 2192 observed reflections. The Pd atom is of squareplanar coordination. The ferrocene ligand of in DMAF has an approximately eclipsed conformation.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2

All attempts to prepare light lanthanide dicyclopeutadienyt chloride failed,due to the disproportionation reaction. The crystal complex of [(η~5-C_5H_5)_2NdCl.OC_4H_8]_2 was successfully prepared by the reaction of NdCl_3·2C_4H_8O with cyclopentadienyl sodium (molar ratio 1:1.8)in tetrahydrofuran at room temperatureThe composition of the title compound was determined by the methods of elemental analysis, infrared spectroscopy and photoelectron spectroscopy. The crystal structure of [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2 was determined from single crystal X-ray diffraction. Data were collected at-60℃ under dry nitrogen atmosphere.The complex crystallizes in the monoclinic space group P2_1/c,with Z=2. Lattice parameters are: a=8.201(3), b=21.589(6),c=8.596(3),β=109.10(3)°.The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R=0.0636 for 1680 reflections. There are two Nd atoms in the dimeric unit which are bridged asymmetrically by the two chlori     

CRYSTAL AND MOLECULAR STRUCTURE OF TETRAAQUA TRIM TRATO SAMARIUM(Ⅲ) DIHYDRATE [Sm(H_2O)_4(NO3)_3] ·2H_2O

<正> [Sm(H2O)4(NO3)3]·2H2O,Mr=444. 46,triclinic,space group P1 ,a = 6.747(1),b=9. 156(1),c=11.673(l) A ,α= 69. 90(1),β=88. 88(1),γ=69. 29 (1)°,V = 629.0A3,Z=2,λ(MoKa) = 0. 7107A,F(000) = 430,Dx=2. 346/cm3,final R=0. 032. The Sm atom in the title complex has bicapped square antiprismtic coordination of oxygen atoms from four water molecules and three NO3 groups. The Sm -O(nitrato) and Sm-O(aqua) distances are in the ranges of 2. 517-2. 716 and 2. 407-2. 432A , respectively. The N-O bond lengths vary between 1. 209 and 1. 265 A with the shortest distances being those involving noncoordinated oxygen atoms. The two lattice water molecules are outside the coordination sphere of the Sm atom but participate in the network of intermolecular hydrogen bonds.     

CRYSTAL STRUCTURE OF A HETERONUCLEAR LANTHANIDE COMPLEX OF ERBIUM-YTTRIUM AND GLYCINE[ErY(GlY)_6(H_2O)_4](ClO_4)_65H_2O

The title complex [ErY(Gly)_6(H_2O)_4](ClO_4)_6 5H_2O has been synthesized.Its crystalstructure has been determined by X-ray diffraction method.The crystal is triclinic with space groupP1.The unit cell parameters are as follows:a=11.518(4),b=14.105(7),c=15.530(6) ,α=96.61(3),β=102.74(3),γ=105.70(3)°,V=2327.7(17) ~3,Z=2,Dc=2.091g/cm~3.The structure has been refinedto a final R of 0.0785.The crystal is an infinite chain complex,in which four carboxyl groups fromglycine molecules bridge the Er(Ⅲ)and Y(Ⅲ)ion,other two carboxyl groups bridge two adjacentEr(Ⅲ)or two Y(Ⅲ)ions.     

FORMATION AND CRYSTAL STRUCTURE OF (Et_4N)_2[Fe(SC_6H_4CH_3-P)_4]

<正> INTRODUCTION. In the study of synthetic methods and chemical reactions of Mo-Fe-S cluster compounds for simulation of the catalytic active center of nitrogenase, the reaction.systems of MoS_4~(2-) and varios ferric or ferrous salts have caused the interests of many chemists. We have been studying the system of ferrous thiolates and thiomolybdates and found interesting results. In a previous paper, we reported the syn-     

SYNTHESIS AND STRUCTURE OF TETRANUCLEAR MOLYBDENUM CLUSTER COMPOUND[Mo_4S_4(μ-O_2CC_6H_5)_2(dtp)_4]

The cluster compound[Mo_4S_4(μ-O_2CC_5H_5)_2(dtp)_4](dtp=S_2P(OEt)_2)wasobtained by the ligand substitution reaction of tetranuclear molybdenum cluster[Mo_4S_4(μ-dtp)_2(dtp)_4]in the mixed solvent of acetone,ethanol and water in thepresence of C_6H_5CO_2Na.It is monoclinic and crystallizes in space group C2/c,Mr=1495.09,a=12.175(5),b=22.01(1),c=20.875(9),β=99.04(4)°;V=5575(5);Z=4;Dc=1.78g/cm~3.Final R factor is 0.066.The result reveals that the[Mo_4S_4]clustercore and t-(dtp)~(-1)ligands are retained and only μ-bridged(dtp)~(-1)ligands aresubstituted by(C_6H_5CO_2)~(-1)in the substitution reaction,thus producing the newtitle cluster compound,the structure of which contains two species of bidentateligand.     

SYNTHESIS AND STRUCTURE OF AN ASYMMETRIC TRICOBALT COMPOUND Co_3(o-HOC_6H_4S)_2(o-OC_6H_4S)_2(PEt_3)_3

Compound Co_3(o-HOC_6H_4S)_2(o-OC_6H_4S)_2(PEt_3)_3 was obtained by reaction of CoCl_2,o-HOC_6H_4SH(H_2mD)and PEt_3 in ethanol in the presence of NaOCH_3.The three Co atoms aretriangularly arranged and asymmetrically bridged by four S and one O atoms from the fourH_2mp ligands and terminally ligated by one O and three P atoms.Two free hydroxyl groupsform two internal hydrogen bonds with adjacent oxo donor atoms.