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).     

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     

CRYSTAL AND MOLECULAR STRUCTURE OF DIPOTASSIUM TRIS(HYDROXYACETATO)VANADYL (IV) MONOHYDRATE

<正> Preliminary information. The vanadyl complexes are found to be increasingly used in the areas of catalysis, new materials research as well as in bio chemistry. Therefore, more attentions have been paid to such compounds. The title complex K_2[VO(C_2H_3O-3)_2(C_2H_2O_3)] H_2O has been prepared by reaction of VOSO_4 with hydroxyacetic acid in aqueous solution, with KOH added to a suitable PH value.     

V(HSO_4)_3 promoted oxidation of alcohols and trimethylsilyl,tetrahyropyranyl and methoxymethyl ethers with Cu(NO_3)_2·3H_2O in the absence of solvent

V(HSO_4)_3 has been found to be an efficient reagent for the promotion of the oxidation of alcohols and trimethylsilyl, tetrahydropyranyl and methoxymethyl ethers to their corresponding carbonyl compounds with Cu(NO_3)_2·3H_2O in the absence of solvent.     

Structural comparison to the molybdenumsite of nitrogenase Synthesis and crystal structure of binuclear oxomolybdenum(V)complex with both omercaptophenolate and alkoxide ligands

Complex(n-Bu_4N)[Mo_2O_2(OMe)(mp)_3][1,mp=(o-OC_H_4S)~(2-)]was synthesized by thereaction of MoOCl_3(THF)_2 and Na_2mp in EtOH and crystallized in monoclinic space group P2_/nwith crystal data:a=13.910(3),b=23.554(3),c=12.558(2),β=105.20(2)°,Z=4,D_o=1.455g/cm~3,final R=0.077 for 5325 reflections[I>3σ(I)].The two[Mo(O)mp]~+ moicties are bridgedby one 1,2-bidentate ligand mp~(2-) with exceedingly small bite angle(69.0°)and bite distance(2.70)and by a methoxy group.The structure can be interpreted as two distorted octahedraaround the Mo atoms sharing a face.Attempts have been made to provide structural informa-tions for the syntheses of modelling compounds of FeMoco by comparing the Mo—O and Mo—Sbond distances of o-mercaptophenolate ligated compounds to those of the molybdenum site ofnitrogenase.     

THE STRUCTURE AND SYNTHESIS OF [MoFe_3S_4(Etadtc)·_5]MeCN

<正> INTRODUCTION. More and more models of active center were suggested with wide study on the MoFe-protain and FeMo-cofactor of nitrogenase. Most of them contain MFe_3S_(3+4) (M=Mo,Fe) cubane-type core, so a great interest has been focused on the Studies of MoFe_4, cubane-type compounds. The type species have been reported by holm et al. We have also made researches on the single cubane-like compounds. Here we describe the synthesis and structure of [MoFe_3S_4(Et_2dtc)_5MeCN (1).     

CONDENSATION REACTION OF INACTIVATED BENZENE

A new dimolybdenum(V)complex[(C_6H_4Cl)_2C(Ph)]_2[Mo_2(μ-Cl)_3Cl_4O_2][Mo_2(μ-Cl)_2Cl_4O_2(μ-OCOPh)]has been obtained in the reaction of PhCl with benzoyl peroxide(PhCO_2)_2 and MoCl_5.Its crystal structure has been determined by X-ray diffraction meth-ods.Spectroscopic characterization of the compound and ASED-MO calculation of thetrityl cation are reported.     

THE SYNTHESIS AND STRUCTURE OF THE CLUSTER COMPOUND {(Mo_3(μ_3-O)(S_2)_3[S_2P(OEt)a]3)2Cl}FeCl_4

<正> INTRODUCTION. Resently a series of M2-type trinuclear Mo clusters with the formula {Mo_3(μ-Y)(S_2)_3[S_2P(OEt)_2]_2]_3}X, (Y=O or S; X=Cl or I) have been synthesized by our research group through either the reduction of the higher valence Mo(V) compounds or the oxidation of the middle valence Mo(Ⅲ) species. In this paper we report a novel type of cluster cation     

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…     

CRYSTAL AND MOLECULAR STRUCTURE OF {Fe_6Mo_2S_8(S-t-Bu)_6(OMe)_3}(Et_4N)_3

<正> Introduction. The title compound has been synthesized by reaction of {(SR)_2FeMoS_4}2-with {Fe_4(SR) 10}~2- (R=t-Bu) in methanol. It is interesting to note that the complex, which involves two {Fe_3MoS_4}cubane-like clusters, is generally regarded as the best model compound for molybdenum center of nitrogenase. The synthesis and property of {Fe_6Mo_2S_8(S-tBu)_6(OMe)_3}~3- have been discribed. Although it has previously been noted that the structure of this complex is similar to its tungsten analog, the detail structural report of the title compound has not yet been given.     

STUDY ON THE nd~a METAL REPLACED YBa_2Cu_(3-X)M_XO_(7-Y)

A systematic study of the structural and superconducting behavior of the high Tc compounds YBa_1Cu_(1.9)M_(0.1)O_(7-y) has been performed where M=Ti, V, Mn, Fe, Co, Ni, Zn, Zr, Nb, Mo, In and Sn. Structural analysis shows that most replacements somewhat modify the YBa_2Cu_3O_(7-y) lattice parameters in the orthorhombic structure, with the exception of Fe and Co which transit into tetragonal phase. Although the 1D Cu-O chains are destroyed, the depressed Tc remain within 73 to 76K in the case of Fe and Co. However. the substitution of Ni and Zn on the Cu_2 sites appears to strongly decrease Tc whereas their structure remains orthorhombic. This indicates that the 2D Cu-O planes play a very important role in the transportation of superconducting electrons but the 1D Cu-O chains play a role not only in supplying carrier number but also in coupling the Cu-O planes.     

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.     

CRYSTAL AND MOLECULAR STRUCTURE OF K(C_3H_(12)N_2)_2(HV_(10)O_(28_).8.5H_2O

<正> Preliminary information. Vanadium compounds plays an important role in catalysis since they have a property of easily changeable oxidation states. As a part of our study on vanadium compounds, the crystal structure of the title compound is reported, which is prepared by the reaction of (C_3H_(12)N_2)_2-V_2O_7, NaVO_3 with KOH in an aqueous solution.     

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 PYRIDINUM μ-OXO-μ-SULFATO-BIS(OXO(TRITHIOCYNATO)-MOLYBDAIE(V))

<正> Introduction. The structural characterization of the compounds of Mo with inorganicacid radical may be belpful to the elucidation of the role of Mo enzymes in the catalysis of oxyanions(NO_3~-/N02~-,S04~2-/SO_3~2-)~1 Their spectral properties have therefore been investigated. Trzebiatowska et al. believe that there are two complexing models with the bridging SO_4~2-. One is that two Oxygen atoms in sulfate are bonded to two Mo atoms respectively whereas the Other is that theY are bonded to two Mo atoms simultaneously, forming a     

A SERIES OF TRINUCLEAR MOLYBDENUM CLUSTERS WITH LOOSE COORDINATION SITES

<正> The cluster compound Mo3S4[S2P(OEt)2]4(H2O) with a comparatively stable cluster core [Mo3(μ3-S)(μ-S)3]4+ and some labile ligands or loosely coordination sites has been already prepared successfully by a self-assembly reaction. Its surprising chemical reactivity in the reactions of substitution, addition, and oxidation has been noted and used widely for the syntheses of a series of new, trinuclear Mo cluster compounds, of which the structures of the 12 selected compounds characterized by X-ray diffraction analysis are exhibited in diagrams. Meanwhile, those compounds with the same cluster core [Mo3(μ3-S)(μ-S)2]4+ show two groups of characteristic IR bands at ~480 cm-1 for the Mo-(μ-S) vibration and -450cm-1. for the Mo- (μ3-S), and their selected bond distances are tabulated as well.In a cluster-catalyzed homogeneous process, it is important that clusters have loose coordination sites or are coordination unsaturated. In our further research on the medium-valence molybdenum clusters[1], we have foun     

CRYSTAL STRUCTURE OF 2-METHYL-4-(ρ-)PLUOROPHENYL-2,3,4,5 TETRAHYDRO-BENZO-(l,5)-THIAZEPINE(C16H16SNF)

<正> INTRODUCTION. In our systematic investigation on the 2, 4-substituted derivatives of dihydro- and tetrahydro-benzo-(1,5)-thiazepines, it has been discovered that there are large differences between dihydro- and tetrahydro- compounds in their conformation and in their spectral splits of proton     

STUDY ON SOME BIOLOGICALLY ACTIVE CO-ORDINATION COMPOUNDS OF METAL IONS (Ⅰ)——SYNTHESIS,CHARACTERIZATION,STRUCTURE AND ANTITUMOR ACTIVITY OF COMPLEX OF 3,6-DI-(DIMETHYLAMINO)-DIBENZOPY-RIODONIUM LANTHANUM EDTA

The title coordination compound has been synthesized by the reaction of HLaEDTA·7H_2Owith (CH_3)_2N-?-N(CH_3)_2·HCOO~- in ethanol aqueous solution. Thesingle crystal has grown from aqueous solution and has been characterized by IR, TG-DTA,X-ray powder diffraction, molar conductance, UV and ~1H-NMR. The determination of itscrystal and molecular structure shows that it crystallizes in space group P2_(1/n) with latticeparameters: a = 14.735A, b = 29.335A, c = 16.409A, β = 99.24°, v = 7009.30A~3, z = 4,F(000) = 3488, molecular weight M = 1756.90, D_C = 1.665g/cm~3. It has been refined by thefull matrix least squares method to final discrepancy factor R = 0.096. The anion [La2(EDTA)_2(H_2O)_4]~(2-) turns out to be a dimer, in which each of the twoEDTA~(4-) ions is coordinated to a La~(3+) ion with five of its six coordinating sites and the re-maining sixth one-the oxygen atom of carboxylis bridged to two La~(3+) ions, thus forming aparallelogrammic four-membered ring La_2O_2. The nine coordinations about     

SYNTHESIS AND STRUCTURE OF A NEW DINUCLEAR MOLYBDENUM(O) COMPLEX [Et_4N]_2 [Mo_2 (CO)_8 (SCH_2COOEt)_2]

<正> t Reaction of Et^NI, NaSCH2COOEt with Mo(CO)6 in MeCN affords a new dinuclear molybdenum(O) complex, [Eti,N]2 [Mo2(CO) 8(SCH2COOEt)2] (I) . The crystal and molecular structure has been determined from three-dimensional X-ray data. 1_ crystallizes in the triclinic, space group PI with a=10.362(1), b= 10.391(1), c=10.815(2) X, a=91.64(2), 6=100.07(2), Y=H4.46(1)? Z=l, R= 0.048 for 2975 reflections with I?o(I). Noribonding of Mo...Mo distance (3.939(11)A) in _! supports the previous speculation for the two-electron redox properity,of complex anion, [Mo2(CO)g(SR)2J2~.     

STUDIES ON O-ALKYL O-ARYLPHOSPHORO- (THIOUREIDO)-THIOATES AND O-ALKYL PHOSPHORO-BIS-(THIOUREIDO)THIOATES

Two series of new organic phosphorus compounds with the general formula Ⅰ and Ⅱ have been prepared by the reaction of thc phosphoro-(isothioeyanatido) thioates and phosphoro-bis-(isothiocyanatido) thioates separately with amines.where R=Et; Ar=2-NO_2-4-Meph, 2, 4-Cl_2ph; NR~1R~2=NMeMe, NHC_3H_7-iso, NEtEt, Result from the preliminary bioassay showed that some of these compounds have fairly good herbieidal activities, especisllyThe structure of these compounds has been confirmed by IR and NMR.