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 AND CRYSTAL STRUCTURE OF Mo_20_2S_2(Py)_4(Mo0_4)

<正> Introduction. A series of trinuclear molybdenum clusters has been synthesized and identified. Most of them have almost the sameMo-Mo distance. We have synthesized another kind of trinuclear molybdenum complex which has different Mo-Mo distances and can be comsidered as composed of the complex (Mo_2O_2S_2(py)_4)~2+ and the molbdenic ion (MoO_4)~2-. This paper reports the synthesis and structure of the title compound.     

STRUCTURAL CHEMISTRY OF EIGHT-COORDINATE COMPLEXES OP MNTHANOID WITH BIDBNTATE LIGANDS IV.CRYSTAL STRUCTURES OF [C_4H_8OH] [Eu(S_2CNC_4H_8)_4]·xC_4H_8O(x=2,0)

<正> Compound [C4H3OH][Eu(S2CNC4H3)4].2C4H8O(I), Mr=953,80,monoclinic, P21/n,a = 11,332(3), b= 22,837(5), c= 15.671(2)A,β= 94.93(1)°, V= 4040.2 A3,Z= 4,Dc = 1.567 g/cm3. [C4H8OH][Bu(S2CNC4H8)4] (2),Mr=809.72, monoclinic,P 21/c,a= 12.184(2), b= 15.181(3), c= 18.334(3)A,β=98.57(1)°,V=3353,3 A3,Z = 4, Dc= 1.605 g/cm3. The Eu atom in the anions of 1 and 2 is coordinated by eight S atoms frow four S2CNC4H8 chelate groups in the form of a dodecahedron with approximate D2d symmetry.     

CRYSTAL STRUCTURE OF [Et_4N]_2[Mo_2O_2(μ-S)_2(S_2)_2]

<正> [(C2H5)4N]2[Mo2o2S2(S2)2], Mr = 676. 74, monoclinic, P21/c, a = 13.510(2), b = 14.373(2), c=14. 777(3)(?), β = 97.53(2)°, V = 2844.7(9) (?)3, Z = 4, Dc= 1. 58g/cm3, μ(MoKα) = 13.0cm-1, F(000) = 1384, R =0. 033 for 1803 observed reflections. The structure contains discrete [Mo2O2S2(S2)2]2- anions and Et4N+ cations. The two oxygen atoms bonded to the Mo atoms are in cis-form with respect to the Mo2S2 bridging unit, with an average Mo- O distance of 1. 678 (?), The Mo…Mo distance is 2. 832(1)(?).     

THE CRYSTAL STRUCTURE OF Mo_203[S_2P(OC_2H_5)_2]_4

<正> Introduction. In an attempt to synthesize Mo cluster compounds from the high-valenced Mo compounds in P_2S_5/EtOH-HC1 system we have obtained a brownblack rhombohedral crystal. The composition of it Mo_2O_3[S_2P(OC_2H_5)_2]_4 has been confirmed by X-ray single crystal structure determination, which reveals that the crystal structure is different from that by Knox, J. R. & Prout, C. K. (1969).     

CRYSTAL AND MOLECULAR STRUCTURE OF [K(C_(14)H_(20)O_5)_2]_2[Co(NCS)_4]

<正> The title complex (Mr= 1442.6) crystallizes in the monoclinic, space group PC, with a =14.515(7),b =15.773(5), c =16.287(11)51,β=95.13(5)°,Z=2,V=3713.8A3,Dc=1.29 g·cm-3. The structure was solved by Patterson method and the final R=0.068. The potassium atom in the cation lies between the two planes of the oxygen atoms from two benzo-15-crown-5 molecules.     

MOLECULAR AND CRYSTAL STRUCTURES OF TETRANUCLEAR MOLYBDENUM CLUSTER[Mo_4(μ_3-O)_2O_4Cl_2(o-CH_3C_6H_4COO)~6]■

The new cluster[Mo_4(μ_3-O)_2O_4Cl_2(o-CH_3C_6H_4COO)_6]has been prepared by thereaction of molybdenum pentachloride and o-methylbenzoic acid.The crystal andmolecular structures were determined by the X-ray diffraction method.It crystallizesin the orthorhombic space group Pnna with cell parameters:Mr=1361.6,a=13.792(4),b=17.957(3),c=20.974(9) ,V=5194(2) ~3,Z=4,Dc=1.74/cm~3,F(OOO)=2704,μ(MoK )=11.0/cm,R=0.074.     

THE CRYSTAL AND MOLECULAR STRUCTURE OF (QH)_3[Mo_2O_4(■-COO)(NCS)_4]·H_20 AND (QH)_3[Mo_2O_4(CH_30H)(NCS)_5]

<正> INTRODUCTION. In the reported crystal structures of di(μ-X)(X=O,S)-bridged oxodimolybdates (Ⅴ), the local, symmetric array of donor atoms linked to the Mo atoms is well known. The title compounds (QH)_3[Mo_2O_4(COO)-(NCS)_4]-H_2O(Ⅰ) and (QH)_3[Mo_2O_4(CH_3OH)(NCS)_5](Ⅱ), in which the environments     

SYNTHESIS AND CRYSTAL STRUCTURE OF Mo_3(μ_3-O)(μ-S)_3[S_2P(OEt)_2]_4(C_3H_3N_2)

<正> Mr=1164, space group C2/c, a=14.954(13)A,b=22.323(6)A,c=27.003(18)A,β=98.23(7)°,V=8920 A3, Z=8. Final R=0.069 for 2818 unique diffraction data with I≥30(I). The title cluster compound is of Ml configuration with a triple bridging atom O and with a 'loosely coordinated site' occupied by an imidazole ligand. Three Mo-Mo bond lengths are 2.657 (2), 2.649(2),and 2.646(2)A,respectively. The average bond length of Mo-(μ3-O) bonds is 2.052 A.     

CRYSTAL STRUCTDBE OF H_2(Et_4N)_2[Mo_8O_(26)]

<正> Mr= 1446.02, Monoclinic, P21/n, a = 11.841(2),b= 20.008(6), c= 12.053(8)A,β=105.15(3)°,V= 2756(3)A3,Z= 2, DC = 1.738 g·cm-3. Final R=0.035 for 4326 reflections. The title compound is the decomposition product of the trinuclear Mo cluster anion [Mo3(μ3-O)(μ-Cl)3(μ-OAc)3Cl3]-. The [No8O26]4- anion reported here has the a -type configuration, which consists of a ring made up of six edge-sharing [MoO5] octahedra linked loosely to two [MoO4] units.     

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.     

CRYSTAL AND MOLECULAR STRUCTURE OF GUANIDINIUM BIS (o-AMINOPHENYLARSENIC) HEXAMOLYBDATE (CN_3H_6)_4[(o NH_2C_6H_4 As)_2Mo_6O_(24)]

<正> Guanidinium bis (o - aminophenylarsenic) hexamolybdate belongs to monoclinic space group P21/c,with a=10. 217(2),b= 18. 870(2),c= 10. 939(2)A,β = 102. 82(3)°,Z = 2,V=2056. 4A3,and Dc=2. 477 g·cm-3. Each molecule contains one [(o-NH2C6H4As)2Mo6O24]4- anion and four CN3H6+ cations. In the anion,six distorted MoO6 octahedra are connected with edges-sharing to form a six-membered Mo ring which is capped above and below by two o - aminophenylarsenic groups. There is half a molecule in an asymmetric unit. It is interesting that both phenyl planes are almost perpendicular to the plane of the Mo atoms. The structure of the anion is similar to that of [ (CH3 As)2Mo6O24]4-,[(n-C3H7As)2Mo6O24]4- or [(C6H5CH2As)2Mo6O24]4-. This is the first example of this type of compounds in which the As atom is directly connected to a substituted phenyl group.     

CRYSTAL STRUCTURE OF (Et_4N)_4[Mo_2Fe_7S_8(SPh)_(12)]

<正> (Et4N)4[Mo2Fe7S8(SPh)12] : Mw=2670.3, triclinic, p1, a=12.775(4), b=13.076(3), c=20.576(4)A, α=80.00(2), β=81.39(2), γ=61.51(2)°, V=2966.3(14) A3, Z=1, D=1.494 gcm-3, R=0.077 for 4031 observed reflections. The complex was prepared by reactions of (Et4N)2[Fe4(SPh) 10] with (Et4N)2MoS4 in an ace-tonitrile solution. The structure of [Mo2Fe7S8(SPh)12]4- anion is a double-cubane-like configuration bridged by a Fe(SPh)6 group.     

EPR AND ELECTRONIC STRUCTURE OF Mo(V) COMPLEX Mo_2O_3(S_2CNEt_2)_4

<正> INTRODUCTION. Particular interest of some chemists has directed to the chemistry of molybdenum, as the oxidation states of molybdenum (-2～+6) are interesting and Mo atom in various forms usually is contained in the active site of enzymes or catalysts.     

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 [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.     

CRYSTAL STRUCTURE OF [(C_4H_9)_4N][O_2Mo~(VI)S_2Cu~Itu](tu=(NH_2)_2CS)

<正> Crystal and molecular structure of [(C4H9)4N][O2MoS2Cutu] (tu-thiourea) has been determined by X-ray diffraction technique. The crystal is monoclinic, space group P21/n, with a = 11.871(4), b=13.920(2), c= 15.814(11)A;β= 90.22(4)°,V=2613.2A3,Z = 4, DC= 1.459, Do = 1.46g/cm3. The final R and Rw are 0.049 and 0.056, respectively. The title complex has a rhombic planar MoCu(μ-S)2 core with Mo-Cu distance of 2.647A.The Ho atom is tetrahedrally coordinated by two 0 atoms and two u-S atoms. The Cu-S(tu) bond length of 2.191 A is significantly shorter than the Cu-S(bridge) in analogues.     

CRYSTAL STRUCTURE OF (Et_4N)_3[Mo_2Fe_6S_8(SPH)_9]

<正> Introduction. A series Of Mo-Fe-S complexes with doublecubane structure has been synthesized and identified. Because of the similarity of its extended X-ray absorption fine structure (EXAFS) to that of FeMo cofactor and nitrogenase, suggestion has been made that the doublecubane complexes may serve as models for the Mo site of nitrogenase. Therefore, the investigation of this type of complexes has attracted much attention. By using the similar method of spontaeous self-assembly reaction, and starting from certain kinds of Mo-Fe-S compounds, we have been able to obtain several kinds of compounds, one of which     

CRYSTAL STRUCTURE OF Mo_2(u-S)_2(S_2P(OEt)_2)_4

<正> Mr=996.91, triclinic, P1, a=8.773(2), b=9.712(3), c=13.652(1) A; α=69.24(0), β=70.43(3), γ=66.87(l)°; Z=l, Dx=1.699 g/cm 3. Final R=0.053 for 3186 reflections with I≥3a(I). There is an interesting trans influence of μ-s bridge in this binuclear cluster. Mo-Mo distance is 2.752(1) A.