Reaction of Mo(CO)6 with Alkoxide: Synthesis and Structure of the Mo(0)-OR Complex [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2C6H5)3]

The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2- C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a=15.359(2), b=18.378(3), c=24.952(2)(A), β=102.268(4)°, V=6882.3(16) (A)3, Mr=1348.34, Z=4, Dc=1.301 g/cm3, F(000)=2832 and μ= 0.424 mm-1. The final R=0.0606 and wR=0.1552 for 9396 observed reflections (Ⅰ ＞ 2σ(Ⅰ)). 1 contains a [Mo2O3]3- core in triangular bi-pyramidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three μ-O atoms from C6H5CH2OC6H4O- bridging ligands. The Mo…Mo distance is 3.30(8) (A), indicating no metalmetal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2- has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE HEXANUCLE-AR DIAZENIDO-OXOMOLYBDATE [(n-C_4H_9)_4N]_3[Mo_6O_(18)-(N_2C_6H_3-2,4-(NO_2)_2]

<正> Crystal of the title complex [(n-C4H9)4N]3[Mo6O18(N2C6H3-2,4-(NO2)2](Mr= 1710. 5) is orthorhombic with space group P21cn (Pna21), a = 17. 304(3), b = 17.580(2), c=24. 355(4) (?), V = 7409(2)(?)3, Z = 4, Dc=1. 60g/ cm3, μ=10. 29cm-1, F (000) = 3647. The structural solutions and refinements based on 3900 reflections (I≥3σ(I)) converged at R = 0. 0575, Rw =0. 0498. The atoms of Mo(3), Mo(4), O(1), O(5), O(9), O(11) and the [N2C6H3-2,4-(NO2)2] unit in the complex anion locate approximately in a plane about which the complex anion is nearly symmetrical.     

Synthesis and Structure of a New Dinuclear Molybdenum(Ⅰ) Compound with Cyclohexanthiolate Ligand, [Mo2(SC6H11)2(CO)6(CH3CN)2]

The reaction of [Et4N]2[Mo2(SC6H11)2(CO)8] and I2 in MeCN affords a new dinu- clear molybdenum(Ⅰ) complex [Mo2(SC6H11)2(CO)6(CH3CN)2] 1 (Mr = 672.46). The crystal and molecular structures have been determined by X-ray single-crystal diffraction. 1 crystallizes in monoclinic, space group P21/c with a = 9.302(1), b = 15.514(2), c = 9.307(1)(°A), β = 92.979(2)o, V = 1341.4(3)(°A)3, Z = 2, Dc = 1.665 g/cm3, μ = 11.28 cm-1, F(000) = 676, R = 0.0461 and wR = 0.1274 for 1702 observed reflections with I > 2σ(I). 1 possesses a rhombic bimetallic core MoS2Mo with the Mo-Mo bond length of 2.9712(4)(°A) and Mo-S of 2.4821(5)(°A).     

Strandberg型杂多化合物(C_6H_(11)NH_3)_5H(P_2Mo_5O_(23))4H_2O的水热合成及结构

利用水热合成法合成了分子组成为(C6H11NH3)5H(P2Mo5O23)4H2O的杂多化合物, 用单晶X-ray衍射方法测定了它的结构,该晶体属于单斜晶系,空间群P21/c, a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), Mr = 1483.62, V = 4805.1(17) 3, Z = 4, Dc = 2.051 g/cm3, m = 1.431 mm-1, F(000) = 3000, I >2s(I) 的可观察衍射点4426个, 最终结构偏差因子R = 0.0464, wR = 0.0801, S = 0.731。在[P2Mo5O23]6-杂多阴离子中5个MoO6八面体通过共边和共角相连, 形成1个近似的五角平面骨架, 2个PO4四面体加在五角平面的两侧。热性质研究表明杂多阴离子骨架在547.4 ℃左右分解。     

Synthesis and Crystal Structure of LanthanideHetero-polymolybdate Complex:(NH_4)_(12)H_(10)〔Nd_4Mo_(29)O_(104)(H_2O)_(12)〕·22H_2O

11NTRODUCTIoNNowadaysheteropoly-complexesaremorenoticeableespeciallyinthefieldofcat-alystbecauseinsomeorganicsynthesestheycanbeusedasanoxidativetypeoracidictypecatalystorasboth.Ontheotherhandtherearemanytheoreticaltopicsaboutheteropolycomplexinwhichmanyscientistsareinterested.Inthefieldofpolyacidchemistrythesynthesisofanewheteropolycomplexisanimportantaspect.Molybdenumcanformbinaryheteropolymolybdatecomplexcompoundswithmanymetalandnon-metalelements.Indifferentcompoundstheratioofheteroatoms…     

APPLICATION OF DITHIO - MOLYBDATE IN THE SYNTHESES OF Mo-Cu CLUSTERS: SYNTHESES AND CRYSTAL STRUC-TURES OF MoOS_3(CuPPh_3)(Cu(PPh_3)_2 AND (Ph_4P)_2[Mo_2Cu_5S_6O_2-(S_2CNEt_2)_3] ·DMF

<正> The reactions of (NH4)2MoO2S2 with Cu(PPh3)3Cl in CH3CN in the air, or with CuCl, Ph4PBr, and NaS2CNEt2 in DMF under anaerobic condition, afforded the cluster complexes MoS3OCu2 (PPh3)3 (Ⅰ) and (Ph4P)2 CMo2Cu5S6O2-(S2CNEt2)33 · DMF (Ⅱ), respectively. Compound (Ⅰ), MoOS3Cu2P3C54H45(Mr = 1121. 0) , crystallizes in the triclinic, space group P1 with cell parameters a = 14. 103 (3), b = 17.906(3), c=11.503(2)(?), α=107. 76(1), β=111.81(2), γ = 74.93 (2)°, F = 2532. 9(?)3 and Z=2, Dc=1. 471 g/cm3, F (000) = 1140, μ(MoKα) = 13. 215 cm-1, final R = 0. 060 (Rw = 0.064) for 5959 independent reflections with I >3σ(Ⅰ). Complex (IⅡ), Mo2O3S12Cu5P2N4C66H77 (Mr = 1930. 67) , crystallizes in monoclinic, space group P2/c with cell parameters a = 25. 325(19) , 6 = 22. 506(9) , c =14. 066(8)(?) , β =100. 96(6)°, V =7871. 16 (?)3, Z = 4, D,= 1. 629 g/cm3, F(000) = 3904, μ(MoKα) = 20. 216 cm-1, R = 0. 097 (Rw = 0. 095) for 5677 reflections with I>3σ(Ⅰ). The core structure of complex (Ⅰ) is defective cub     

Hydrothermal Assembly and Structural Characterization of an Octamolybdate Supported Copper(Ⅰ) Tetramer:[Cu2(1,10-phen)2(4,4'-bpy)]2[Mo8O26]·4H2O

A hydrothermal reaction of copper acetate with ammonium molybdate, 4,4'-bpy (4,4'-bipyridine) and 1,10-phen (1,10-phenanthroline) led to the formation of brown crystals of [Cu2(1,10-phen)2(4,4'-bpy)]2 [Mo8O26]@4H2O 1. Single-crystal X-ray analysis has revealed that 1 C68H56N12O30Cu4Mo8 crystallizes in the triclinic system, space group P ī with a = 11.270(3), b = 13.113(6), c = 13.906(3)A, α = 103.33(4),α = 98.54(2),β= 101.29(2)°, V = 1920.1(1)A3, Mr = 2542.9(3), Z = 1, Dc = 2.199 g/cm3, μ= 2.435 mm-1, F(000)= 1240, the final R = 0.0445, wR = 0.1082 and S = 1.021 for 5052 observed reflections with I>σ2(I).It consists of copper Ⅰ tetramer units and α-[Mo8O26]4- anions, which are further attached into a three-dimensional framework through hydrogen bonding and π-π stacking interactions.     

A New Diiminopyridyl Cobalt Complex [CoCl2L] (L = 2,6-Bis(N,N'-bis(2,6-diisopropyl-4-(2,3-dimethyoxylbenzoylamide)phenylimino))pyridine)

The reaction of CoCl2·6H2O with 2,6-bis(N,N'-bis(2,6-diisopropyl-4-(2,3-dimethy-oxyl-benzoylamide)phenylimino))pyridine (L) afforded the complex [CoCl2L], which was fully characterized by elemental analysis, UV-vis, IR spectroscopy, fluorescence, and X-ray diffraction analysis. The compound is oftriclinie system, space group P1- with a = 13.058(3), b = 13.798(3), c =16.695(3) (A), α = 98.191(3),β = 102.792(3), γ = 101.820(3)°,V= 2815.0(9) (A)3, Z= 2, F(000) = 1122,μ = 0.45 mm-1, R = 0.061 and wR= 0.1349 for 9842 observed reflections (1 2σ(Ⅰ)). The Co(Ⅱ center adopts a distorted square-pyramidal coordination geometry. The extended structure shows a one-dimensional zigzag double chain linked by hydrogen bonds and π-π stacking interactions.     

Synthesis and Crystal Structure of a Dicopper(Ⅰ) Complex with Bis(diphenylphosphino)methane and Diethyldithiocarbamate

1 INTRODUCTION Dithiocarbamate derivatives and their metal complexes are extremely versatile compounds which have been used, for example, in the treatment of alcoholism, sarcoma cell and as possible pro- tection against the lethal effect of X-rays etc[1]. Owing to the striking structure features and diversified applications of the metal complexes with dithiocarbamate[2～6], it is of theoretical and practical significance to study the coordination chemistry much more adequately. The meta…     

Hydrothermal Assembly and Structural Characterization of an Octamolybdate Supported Copper (Ⅰ) Tetramer: [Cu_2(1,10-phen)_2(4,4′-bpy)]_2[Mo_8O_(26)]·4H_2O

1 INTRODUCTION The recent expansion of the field of heteropolyoxometalate chemistry derives from their vast topological structures and applicable physical properties[1～5]. One of the crucial strategies for the molecular design of solid materials is how to apply hydrothermal synthesis method to introduce some interesting transition metal coordinated fragments into the covalent backbones of solid materials. Studies have been focused on organic-inorganic hybrid materials containing one kin…     

Synthesis and Crystal Structure of K_8H_5［La（SiW_2Mo_9O_（39））_2（H_2O）_（17）］4H_2O

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＫ_８Ｈ_５［Ｌａ（ＳｉＷ_２Ｍｏ_９Ｏ_（３９））_２（Ｈ_２Ｏ）_（１７）］４Ｈ_２ＯＬｕＢｉｎ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，ＨａｒｂｉｎＮｏｒｍａｌＵｎｉｖｅｒｓｉｔｙ，Ｈａｒ?..     

A Two-dimensional Metallic Oxide Constructed from Molybdenum Clusters and Ag(I)-[3-(2-pyridyl)-pyrazole] Cationic Coordination Components

A new polyoxomolybdate compound [Ag3(HL)4](PMol204o)] 1 (HE = 3-(2-pyridyl)pyrazole) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy. The compound crystallizes in trielinie,space group P(1) with a = 10.375(3),b = 12.076(3),c= 13.196(4) (A°),α= 84.170(4),β =71.961(3),γ = 86.326(4)°,V = 1563.1(7) (A°)3,C32H28Ag3Mo12N12O40P,Mr= 2726.52,Dc = 2.897g/cm3,μ(MoKα) = 3.366 mm-1,F(000) = 1284,Z = 1,the final R = 0.0587 and wR = 0.1312 for 4139 observed reflections (Ⅰ ＞ 2σ(I)). X-ray diffraction analyses reveal that the PMo12O403- clusters in compound 1 are linked by four Ag3(HL)43+ units via the terminal oxygen atoms to form a two-dimensional architecture. The symmetrical unit of Ag3(HL)43+ exhibits two distinct Ag(Ⅰ)environments:a two-coordinate {AgN2} site and a five-coordinate {AgN3O2} site which links to two molybdate clusters.     

含一价铜配合物的新型双金属钼氧簇合物[5-(4-Br-Ph)-2,4'-Hbpy]2·[CuⅠ(5-(4-Br-Ph)-2,4'-bpy)2]2[Mo8O26]的水热合成及晶体结构

采用水热法合成出一种含一价铜配合物的新型双金属钼氧簇合物[5-(4-Br-Ph)-2,4'-Hbpy]2[Cu(5-(4-Br-Ph)-2,4'-bpy)2]2[Mo8O26],并通过X射线单晶结构分析、红外光谱分析、元素分析以及X射线粉末衍射分析对该化合物的结构进行了表征.结果表明,该化合物属单斜晶系,P21/c空间群,晶胞参数a=1.4411(3)nm,b=1.3924(3)nm,c=2.5183(5)nm,β=99.06(3)°,V=4.990(17)nm3,Z=2;该化合物是由一价铜配合物{Cu(5-(4-Br-Ph)-2,4'-bpy)2}+与{β-Mo8O26}4-簇通过共价配位键连接形成的新型多金属钼酸盐,其中游离的质子化配体作为抗衡阳离子.     

Synthesis and Structure of a New Dinuclear Molybdenum(Ⅰ)Compound with Cyclohexanthiolate Ligand,[Mo_2(SC_6H_(11)_2(CO)_8]

<正>Molybdenum( I )-compound [Mo2(SC6H11)2(CO)8] 1, crystallizes in monoclinic, space group P21/c with a = 9.5863(9), b = 9.4469(9), c = 13.869(1) A, β = 99.697(2)°, V= 1238.1(2) A3, Z = 2,DC= 1.734 g/cm3, μ = 12.23 cm-1 and F(000) = 644. The finalR = 0.0455 and wR = 0.1159 for 1590 observed reflections with I> 2σ(I). 1 possesses a rhombic bimetallic core MoS2Mo with the Mo-Mo bond length of 2.975(1) and Mo-S of 2.485(2) A.     

H_(3+n)[AsMo_(12-n)V_nO_(40)]·9H_2O(n=2—4)的结构

X光晶体结构分析证实H_(3+n)[AsMo_(12-n)V_+nO_(40)]·9H_2)(n=2—4)的晶体同构,空间群为P,Z=2。n=2时,a=13.951(5),b=14.137(5),c=13.556(4),α=112.44(2),β=109.49(3),γ=60.77(3)°,V=2120.2,M_r=1943.36,D_c=3.044g.cm~(-3),μ=40.90cm~(-1),F(000)=1828。用6216个I>3σ(I)的独立衍射精修结构,R=0.082;n=3时,a=13.891(7),b=14.076(5),c=13.483(5)A,α=112.34(3),α=109.26(3),γ=60.82(3)°,V=2094.5,M_r=1899.37,D_c=3.011g.cm~(-3),μ=40.63cm~(-1),F(000)=1792。用6699个I>3σ(I)的独立衍射精修结构,R=0.054;n=4时,a=13.854(3),b=14.099(2),c=13.501(4),α=112.09(2),β=109.13(2),γ=61.03(2)°,V=2103.0,M_r=1855.38,D_c=2.92(悬浮法),D_c=2.930g.cm~(-3),μ=39.71cm~(-1),F(000)=1756。用7613个I>3σ(I)的独立衍射精修结构,R=0.044。实验采用MoKα辐射,λ=0.71073,T=296K。杂多阴离子均呈准Keggin结构,12个金属原子呈无序分布,可以M(Mo/V)表示。AsO_4四面体中As—O键长1.66—1.68,O—As—O键角均在109.5°左右。畸变的MO_6八面体中,M—O键长分布在1.63—2.36范围。水分子无序处在晶胞中十四个位置上,除O_w(12)和O_w(13)外的水分子均与杂多阴离子形成氢键,且水分子间形成如沸石中那样的复杂?     

Structure and Two-dimensional Correlation Infrared Spectroscopy Study of a New One-dimensional Chain Compound:(4,4''-Hbpy)3[NaMo8O26] (4,4''-bpy)2(H2O)4 (bpy = Bipydine)

A novel compound, (4,4'-Hbpy)3[NaMo8O26](4,4'-bpy)2(H2O)4 1 (bpy = bipydine),was synthesized by the hydrothermal method. Single-crystal X-ray diffraction shows that compound 1 belongs to the monoclinic system, space group C2/m with a = 19.1921(5), b = 18.6931(6), c = 9.3821 (3) (A), β = 104.8020(11)°, V = 3254.22(17) (A)3, C50H51Mo8N10NaO30, Mr = 2062.52, Z = 2,F(000) = 2016,μ = 1.591 mm- 1 and Dc = 2.105 g/cm3. The final R = 0.0283 and wR = 0.0912 for 3118 observed reflections (I ＞ 2σ(Ⅰ)). Compound 1 contains the β-[Mo8O26]4- anion, sodium ion, 4,4'-bpy and lattice crystalline water molecules. The β-[Mo8O26] units link the sodium ion to form a chain structure. The infinitechains of [Na(Mo8O26)]3- blocks are surrounded by protonized 4,4'-bpy cations,4,4'-bpy and lattice crystalline water molecules. The 2D-IR correlation spectroscopy study indicates that the stretching vibrations of Mo=O occur more preferentially due to the thermal effect. The TGA analysis shows that compound 1 has high thermal stability.     

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…     

Synthesis and Characterization of a One- dimensional Molybdenum Oxide （H2enMe）[Mo3O10]

A hybrid organic-inorganic material (H2enMe)[Mo3O10] (C3H12Mo3N2O10, Mr = 523.97) has been synthesized under hydrothermal conditions and its crystal structure was determined by X-ray diffraction. It crystallizes in the orthorhombic system, space group Pnma with a = 12.430(2), b = 7.6089(12), c = 11.9553(19) , V = 1130.7(3) 3, Dc = 3.078 g/cm3, Z = 4, μ(MoKa) = 3.328 mm1, F(000) = 1000, the final R = 0.0256 and wR = 0.0716 for 1314 observed reflections with I > 2σ(I). A total of 11780 reflections were measured and 1325 were unique (Rint = 0.0244). It consists of infinite one-dimensional edge-sharing MoO6 octahedral chains with [Mo3O10]2 moieties. The protonated diaminopropane cations are located between the chains and linked to the oxygen atoms of the inorganic skeletal backbones by hydrogen bonds. It is indicated that the as-synthesized compound displays photochromic property in the solid state.     

Synthesis,Characterization and Crystal Structure of One Ni_2（salen）_2 Complex

A homochiral complex,Ni 2 (salen) 2 (1,salen=(R,R)-(-)-N,N-bis(3-tert-butyl-5-(4ethynylpyridyl)salicyl-idene)-1,2-diaminocyclohexane),has been synthesized and characterized by IR,microanalysis,CD spectra,TGA,powder and single-crystal X-ray crystallography.It crystallizes in triclinic,space group P1 with a=11.896(2),b=12.571(3),c=13.197(3),α=65.61(3),β=73.90(3),γ=75.87(3)o,V=1707.9(6) 3,Z=2,C 42 H 42 N 4 NiO 2,M r=693.51,D c=1.349 g/cm 3,F(000)=732,μ=0.612 mm-1,GOOF=1.015,the final R=0.0290 and wR=0.0796 for 9002 observed reflections with I > 2σ(Ⅰ).The complex architecture is constructed by intermolecular π···π interaction and assembled into a 2D structure via C-H···π interactions between the cyclohexanes and pyridine rings.     

Synthesis and Crystal Structure of [Sm（4-Pyta）3（H2O）2]n （4-Pyta = 4-Pyridylthioacetate）

A novel coordination polymer [Sm（4-Pyta）3（H2O）2]n has been synthesized by the hydrothermal reaction between 4-Pyta （4-Pyta = 4-pyridylthioacetate） and Sm（NO3）3. The structure was characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space groupP1, with a = 9.100（2）, b = 11.842（3）, c = 12.183（3） A, α= 79.781（4）, β= 74.124（4）, γ = 841882（5）^o, V = 1241.6（5） A^3, Z = 2, Mr = 690.95, Dc = 1.84806 g/cm^3, F（000） = 686,μ = 2.669 mm^-1, the final R = 0.0388 and wR = 0.0808 for 4149 observed reflections with I 〉 2σ（I）. The structural analysis shows that the complex exhibits a one-dimensional architecture. Intermolecular hydrogen bonding interactions are found in the complex molecules.