Synthesis and Crystal Structure of Pyridine－2－thiolato－Molybdenum Complex［Et_4N］［Mo（CO_4）（pyS）］

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＰｙｒｉｄｉｎｅ－２－ｔｈｉｏｌａｔｏ－ＭｏｌｙｂｄｅｎｕｍＣｏｍｐｌｅｘ［Ｅｔ_４Ｎ］［Ｍｏ（ＣＯ_４）（ｐｙＳ）］ＹｕＰｅｉ－Ｈｕａ；ＨｕａｎｇＬｉａｎｇ－Ｒｅｎ；ＺｈｕａｎｇＢｏ－Ｔａｏ...     

Synthesis and Structure of Ion-pairComplex［Mo （dtc）_4］［Sm （dtc）_4］

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆＩｏｎ－ｐａｉｒＣｏｍｐｌｅｘ［Ｍｏ（ｄｔｃ）＿４］［Ｓｍ（ｄｔｃ）＿４］ＳＵＮＣｈｕｎ－ｔｉｎｇ，ＺＨＵＹａ－ｂｉｎ，ＬＩＵＸｉａｏ－ｘｕｎａｎｄＹＩＳｈｕｚｈｅｎ（ＣｈｅｍｉｓｔｒｙＤｅｐａｒｔｍｅｎ...     

Synthesis and Crystal Structure of［（n－Bu）_4N］_2［Mo_4O_（10）（OC_（10）H_6O）_2（OCH_3）_2］

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［（ｎ－Ｂｕ）_４Ｎ］_２［Ｍｏ_４Ｏ_（１０）（ＯＣ_（１０）Ｈ_６Ｏ）_２（ＯＣＨ_３）_２］￥ＬｕＸｉａｏ－Ｍｉｎｇ；ＺｈｕＨｕｉ－Ｊｕ；ＹａｎｇＮｉｎｇ；ＬｉｕＳｈｕｎ－Ｃｈｅｎｇ；ＪｉｎＸ?..     

Synthesis and Crystal Structure of an Inclusion Compound Mn（SCN）2（H2O）4 2C6H12N4

1 INTRODUCTION Pronounced interest has recently been focused on the supramolecular chemistry and crystal enginee- ring of coordination compounds organized by coor- dinate covalent or molecular contacts like hydro- gen-bonding, π-π interactions, et al. because of their fascinating structure diversity and potential applica- tions as functional materials in catalysis and separa- tion[1]. A lot of infinite one-, two- and three-dimen- sional coordination frameworks have been synthe- sized, s…     

Synthesis and Crystal Structure of［Tris（2－benzimidazylmethyl）amine］［Imidazole］Copper（Ⅱ）Perchlorate

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｔｒｉｓ（２－ｂｅｎｚｉｍｉｄａｚｙｌｍｅｔｈｙｌ）ａｍｉｎｅ］［Ｉｍｉｄａｚｏｌｅ］Ｃｏｐｐｅｒ（Ⅱ）ＰｅｒｃｈｌｏｒａｔｅＺｈｏｕＷｅｉ－Ｈｏｎｇ；ＬｉｕＸｉａｏ－Ｌａｎ；ＭｉａｏＦａ...     

Synthesis and Crystal Structure of a New Dimolybdenum（V） Complex Na4[Mo2O4（HNTA）2]2·19H2O

The new binuclear molybdenum（V） complex Na4[Mo2O4（HNTA）2]2·19H2O （NTA = nitrilotriacetate） has been prepared and characterized by single-crystal X-ray diffraction analysis and IR. The crystal has space group Pnma with a = 10.2239（2）,b = 23.8174（3）,c = 23.1845（4） A,V = 5645.58（16）A^3,Z = 4,C24H66Mo4N4Na4O51,Mr = 1702.50,Dc = 1.958 g/cm^3,μ = 1.027 mm^-1,F（000） = 3280,T = 293（2） K,the final R = 0.0609 and wR = 0.1449 for 5512 observed reflections （I 〉 2σ（I））. Each MoV atom has a distorted octahedral coordination geometry,and the two coordination octahedra share a common edge to form a dioxo-bridged Mo2O4 unit which is coordinated by NTA ligands. The dianionic binuclear units [Mo2O4（HNTA）2]^2- are interconnected by Na^＋ into a layered structure.     

Synthesis and Crystal Structure of Squarate Complex ［CuLaSm（C_4O_4）_4（H_2O）_（16）］·2H_2O

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＳｑｕａｒａｔｅＣｏｍｐｌｅｘ［ＣｕＬａＳｍ（Ｃ_４Ｏ_４）_４（Ｈ_２Ｏ）_（１６）］·２Ｈ_２Ｏ￥ＳｈｉＪｉｎｇ－Ｍｉｎ；ＹａｎＳｈｉ－Ｐｉｎｇ；ＬｉａｏＤａｉ－Ｚｈｅｎｇ；ＪｉａｎｇＺｏｎｇ...     

Synthesis and Crystal Structural Characterization of （NH＿4）＿5H＿3Mn＿3V＿（12）O＿（40）·15H＿2O

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒａｌＣｈａｒａｃｔｅｒｉｚａｔｉｏｎｏｆ（ＮＨ＿４）＿５Ｈ＿３Ｍｎ＿３Ｖ＿（１２）Ｏ＿（４０）·１５Ｈ＿２ＯＷＡＮＧＺｕｏ－Ｐｉｎｇ;ＬＩＵＪｉｎｇ－ｆｕａｎｄＷＡＮＧＥｎ－ｂｏ（Ｄｅｐａｔｍｅｎ...     

Synthesis and Crystal Structure of （Et4N）2[Pd2（mp）2（mpH）2]

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ（Ｅｔ_４Ｎ）_２［Ｐｄ_２（ｍｐ）_２（ｍｐＨ）_２］ＳｈｉＪｉ－Ｃｈｅｎｇ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ；ＷｅｎＴｉｎｇ－Ｂｉｎ；ＤｅｎｇＹｕ－Ｈｅｎｇ；ＣｈｅｎｇＣｈａｎｇ－Ｎｅｎｇ；Ｌｉ?..     

Synthesis,Structure, and Decomposition of (NH4)2[Mo6Cl14] · H2O

(NH₄)₂[Mo₆Cl₁₄] · H₂O ( 1 ) was prepared from reactions of MoCl₂ in ethanol with aqueous NH₄Cl solution. It crystallizes in the monoclinic space group I2/a (no. 15), Z = 4 with a = 912.3(1), b = 1491.2(2), c = 1724.8(2) pm, β = 92.25(1)°; R1 = 0.023 (based on F values) and wR2 = 0.059 (based on F² values), for all measured X‐ray reflections. The structure of the cluster anion can be given as [(Mo₆Cl)Cl]^2– (i = inner, a = outer ligands). Thermal stability studies show that 1 loses crystal water followed by the loss of NH₄Cl above 350 °C to yield MoCl₂. The water‐free compound (NH₄)₂[Mo₆Cl₁₄] ( 2 ) was synthesized by solid state reaction of MoCl₂ and NH₄Cl in a sealed quartz ampoule at 270 °C. No single‐crystals could be obtained. Decompositions of 1 and 2 under nitrogen and argon exhibited the loss of NH₄Cl at about 350 °C. Decomposition under NH₃ resulted in the formation of MoN and Mo₂N at 540 °C and 720 °C, respectively.     

Investigation of the Crystal Structure,Characterization, Hirshfeld Surface,and Theoretical Study of (C6H14N)5[HP2Mo5O23]·4H2O

The synthesis of an organoammonium diphosphopentamolybdates(VI), (C₆H₁₄N)₅[HP₂Mo₅O₂₃] · 4H₂O ( 1 ), is reportet. The molecular structure and spectroscopic analysis were performed using experimental techniques like X‐ray diffraction, FT‐IR, and UV/Vis. The single crystal analysis of the title compound shows that the compound crystallizes in the monoclinic crystal system with space group P2₁/c and cell constants of a = 12.7934(2) Å, b = 14.8145(2) Å, c = 27.2637(5) Å, and β = 92.9298(14)°. The Hirshfeld surfaces and the associated 2D fingerprint plots were investigated to study the intermolecular interactions in the crystal packing and this study has confirmed that the hydrogen bonding interactions play a dominating role in the stability of crystal structure. The theoretical calculations were done using PM3 semi‐empirical model and several properties were studied.     

Synthesis and Structure of K_8[P_2W_18Mo_2Co_2O_68(H_2O)_2][MoO_6]·15H_2O

Recently, Many tri-component heteropoly compounds have been synthesized, but tetra-component heteropoly compounds have not been reported. It is known that mixtures of Mo and Co oxides are a promoted hydrodesulphurization catalyst. The title compound is a polyoxophosphate containing Mo, Co and W, the divalent anion possesses two-fused Keggin structure, whereas MoO_6 has been confirmed to be an elementary structure unit of isopoly and heteropoly molybdates, but it, as an idependent anion, has not been reported either.     

[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征

通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺.     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound〔Et_4N〕_2〔Mo_2(CO)_8(SC_6H_4-NH_2-p)_2〕

１ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｅｘｉｓｔｅｎｃｅａｎｄｓｉｇｎｉｆｉｃａｎｃｅｏｆｔｈｅｍｏｌｙｂｄｅｎｕｍ ｓｕｌｆｕｒｂｏｎｄｉｎｇｉｎｍｏｌｙｂｄｅｎｕｍｅｎｚｙｍｅｓ〔１〕ｈａｖｅｓｔｉｍｕｌａｔｅｄｔｈｅｓｔｕｄｉｅｓｏｎｔｈｅｃｈｅｍｉ...     

The First Molybdenum Oxo‐iodide Cluster – [Mo4OI12]2–

Reaction of Mo(CO)₆ with Bu₄NI and I₂ in diglyme yielded a new butterfly Mo^III cluster [Mo₄OI₁₂]^2–. The structure of tetraphenylphosphonium salt was determined by X‐ray single crystal diffraction. Ph₄P⁺ and Bu₄N⁺ salts were further characterized by elemental analysis, mass spectrometry, energy‐dispersive X‐ray (EDX), IR, Raman, and UV/Vis spectroscopy and CVA studies. The cluster anion has a butterfly array of molybdenum atoms and can be represented as [Mo₄(μ₄‐O)(μ₃‐I)₂(μ₂‐I₄)I₆]^2–.     

[Mo(NPPh3)4]2+ [MoNCl3(NPPh3)]2− · C7H8, ein Phosphaniminato-Komplex mit einem Dikation von Molybdän(VI)

[Mo(NPPh₃)₄]²⁺ [MoNCl₃(NPPh₃)]₂^? · C₇H₈, a Phosphoraneiminato Complex with a Dication of Molybdenum(VI). The title compound was prepared by the reaction of MoNCl₃ with Me₃SiNPPh₃ in acetonitrile solution. Red single crystals separated upon addition of toluene. They were characterized by IR spectroscopy and by an X-ray structure determination. (Space group P1 , Z = 2, 6918 observed unique reflections, R = 0.059. Lattice dimensions at 20°C: a = 1 181.4, b = 2 021.4, c =2 409.7pm; α = 65.87°, β = 101.09°, γ= 78.97°). In the dication [Mo(NPPh₃)₄]²⁺ the molybdenum atom is surrounded in a tetrahedral fashion by the four nitrogen atoms of the phosphorane iminato ligands. The MoN and PN bond lengths correspond well with double bonds. In the two anions [MoNCl₃(NPPh₃)]^?, which occur in different conformations, the molybdenum atoms are fivefold coordinated by the terminal nitride ligand Mo?N: in axial positions and by the three chlorine atoms and the nitrogen atom of the (NPPh₃)^? ligand in the equatorial positions.     

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.     

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…     

Molybdänhalogenidcluster mit sechs terminalen Alkoholatliganden: (C18H36N2O6Na)2[Mo6Cl8(OCH3)6] · 6CH3OH und (C18H36N2O6Na2)2[Mo6Cl8(OC6H5)6]

Molybdenum(II) Halide Clusters with six Alcoholate Ligands: (C₁₈H₃₆N₂O₆Na)₂[Mo₆Cl₈(OCH₃)₆] · 6CH₃OH and (C₁₈H₃₆N₂O₆Na)₂[Mo₆Cl₈(OC₆H₅)₆] . The reaction of Na₂[Mo₆Cl₈(OCH₃)₆] and 2,2,2-crypt yields (C₁₈H₃₆N₂O₆Na)₂[Mo₆Cl₈(OCH₃)₆] · 6 CH₃OH ( 1 ), which is converted to (C₁₈H₃₆N₂O₆Na)₂[Mo₆Cl₈(OC₆H₅)₆] ( 2 ) by metathesis with phenol. According to single crystal structure determinations ( 1 : P3 1c, a=14.613(3) Å, c=21.036(8) Å; 2 : P3 1c, a=15.624(1) Å, c=19.671(2) Å) the compounds contain anionic clusters [Mo₆Cl₈ⁱ(OR^a)₆]^2? ( 1 : d(Mo—Mo) 2.608(1) Å to 2.611(1) Å, d(Mo—Cl) 2.489(1) Å to 2.503(1) Å, d(Mo—O) 2.046(4) Å; 2 : d(Mo—Mo) 2.602(3) Å to 2.608(3) Å, d(Mo—Cl) 2.471(5) Å to 2.4992(5) Å, d(Mo—O) 2.091(14) Å). Electronic interactions of the halide cluster and the phenolate ligands in [Mo₆Cl₈(OC₆H₅)₆]^2? is investigated by means of UV/VIS spectroscopy and EHMO calculations.