An unusual organic-inorganic chain-like hybrid complex [(CuCl)(2)(o-phen)](infinity) (o-phen=o-phenanthroline)

A novel organic-inorganic hybrid complex [(CuCl)(2) (o-phen)](infinity) 1 (o-phen = o-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analyses, XPS spectrum, TG analysis, and single-crystal X-ray diffraction. Compound I crystallizes in the monoclinic system, space group P2(1)/n, a = 3.7285(7) Angstrom, b = 19.603(4) Angstrom, c = 16.757(3) Angstrom, beta = 95.83(3)degrees, V = 1218.4(4) Angstrom(3), Z = 4, lambda(MoKalpha) = 0.71073 Angstrom (R(F) = 0.0643 for 2559 reflections). Data were collected on an R-axis RAPID diffractometer at 293 K in the range of 1.60 < θ < 27.48degrees. The title compound exhibits a one-dimensional chain-like scaffolding constructed by the unusual [Cu3Cl3] hexagon motifs by, sharing opposite edges. Only Cu(1) sites of the [Cu3Cl3] hexagon are coordinated with N donors of o-phen groups. Furthermore, the three-dimensional supermolecular architecture is formed by C-H...Cl hydrogen bonds between o-phen groups and CuCl chains.

Synthesis and structure of iron complex with 1,2-dithiolate-1,2-dicarba-closo-dodecaborane [Li(THF)(4)][Fe(S2C2B10H10)(2)(THF)]

The crystal of complex [Li(THF)(4)][Fe(S2C2B10H10)(2)(THF)] 3 belongs to monoclinic, space group P2(1) with a = 11.964(2), b = 16.527(3), c = 12.554(3) Angstrom,beta = 108.70(3)degrees, V= 2351.3(8) Angstrom(3), Z = 2, M-r = 835.95, D-c = 1.181 g/cm(3), mu (MoKalpha) = 5.30 cm(-1), f(000) = '874, R = 0.0622 and Rw 0.1538 for 1641 observed reflections with I > 2sigma(I). The ionic complex,of 3 contains the square pyramidal anion of [Fe(S2C2B10H10)(2)(THF)](-) and the tetrahedral cation of [Li(THF)(4)](+). The iron is 5-coordinated and located in the square pyramidal configuration. The iron atom and the four sulfur atoms are almost coplanar. The Lithium atom is coordinated with four oxygen atoms of four THF molecules and located in a tetrahedral configuration.

Hydrothermal synthesis and characterization of bimetallic cluster complex [{Mn(phen)(2)}(2)V4O12]center dot 1/2 H2O

A new bimetallic cluster complex with the formula [(Mn(phen)(2))(2)V4O12].1/2 H2O has been synthesized through hydrothermal reaction of vanadate staring material with manganese cation in the presence of nitrogen donor chelating ligand and characterized by single-crystal X-ray diffraction, elemental analysis, IR UV-vis, ESR spectrum and thermal analysis. The compound crystallize in the monoclinic space group P2(1)/c with a = 18.475(4) Angstrom, b = 11.473(2) Angstrom, c = 23.667(5) Angstrom, beta = 97.76(3)degrees, V = 4971(2) Angstrom(3) and Z = 4. The structure of [{Mn(phen)(2)}(2)V4O12].1/2 H2O is composed of a discrete V4O124- cluster covalently attached to two [Mn(phen)(2)](2+) fragments.

Synthesis and crystal structure of cyclopentylindene rare earth complex (C5H9C9H6)(3)SMCl-Li+ (THF)(4)

Rare earth complex (C5H9C9H6)(3)SmCl-Li+ (THF)(4)( I ) was synthesized by reacting anhydrous SmCl3 with two equivalents of C5H9C9H6Li. From mix-solvent of THF and hexane, red color single crystals were obtained. The crystal belongs to a cubic system, space group P2(1)3 with unit cell parameters a= b=c= 1. 754 0(2) nm, alpha=beta=gamma=90degrees, V=5. 396 4(11) nm(3), Z = 4. The ten-coordinated samarium atom is bonded to three cyclopentylindenyl rings and a chlorine atom to form the anionic part of the title complex, ring centroids and the chlorine atom form a tortured tetrahedron around samarium. In the cationic part, lithium atom coordinates to four oxygen atoms of THF molecules to form a normal tetrahedron. The Sm-C(within the same ring) distance varies from 0. 268 to 0. 299 nm.

La_(4-x)(P_2O_5)_3:Eu_x的合成及光谱性质

磷酸盐是一类十分稳定的晶体化合物 ,易形成 P— O键的多酸根聚合体[1 ] ,以直键或环状排列 ,它们能与稀土离子形成稳定的化合物。作为稀土发光材料的基质 ,具有吸收能力强、转换效率高、物理化学性质稳定、能承受大功率的电子束和高能射线等优点 ,在光致发光 [2 ] 、电致发光[3] 、阴极射线发光 [4 ] 和X射线发光 [5] 等方面获得了广泛的应用。近年来 ,关于稀土焦磷酸盐的合成已有不少的报道。常用的方法是高温固相法 [6 ] ,用此方法合成的样品虽然亮度高 ,但纯度较低 ,粒度不均匀 ,所以探索合成稀土焦磷酸盐的新方法十分有必要。本文采用液相法合成稀土焦磷酸盐 ,通过对产物的 X射线衍射图的分析来探索合成稀土焦磷酸盐的最佳酸度和最佳锻烧温度 ,并对产物的激发光谱和发射光谱作了分析 ,此方法具有纯度高、粒度小和工艺简单等特点。La4 - x(P2 O5) 3:Eux 的合成 :准确称取 1 0 .0 0 0 0 g La2 O3(99.99% )和 2 .0 0 0 0 g Eu2 O3(99.99% ) ,分别用浓 HNO3(优级纯 )溶解完全 ,加蒸馏水配制成 0 .1 mol/ L 的 La(N...

Single-crystal X-ray structure and properties of K-10[Ni-4(H2O)(2)(AsW9O34)(2)]center dot 4H(2)O

The rational synthesis and the structural and magnetic characterization of a nickel cluster are presented. The compound comprises a rhomblike Ni4O16 group encapsulated between two-heptadentate tungstoarsenate ligands [AsW9O34](9-). The crystal structure of K-10[Ni-4(H2O)(2)(AsW9O34)(2)](.)4H(2)O was solved in monoclinic, P2(1)/n symmetry, with a = 12.258(3) Angstrom, b = 21.232(4) Angstrom, c = 15.837(3) Angstrom, beta = 92.05(3)degrees, V = 4119.1(14) Angstrom(3), Z = 2, and R = 0.0862. The crystal structure of the Ni(II) derivative was compared with that of the Cu(II), Zn(II), Co(II) and Mn(II) derivatives. The Ni4O14(H2O)(2) unit in the compound shows no Jahn-Teller distortion. On the other hand, the Ni(II) derivative shows ferromagnetic exchange interactions within the Ni4O16 group (J = 7.8 cm(-1), J' = 13.7 cm(-1)) and an S = 4 ground state, the highest spin state reported in a heteropoly complex. Its redox electrochemistry has been studied in acid buffer solutions using cyclic voltammetry. It exhibited two steps of one-electron redox waves attributed to redox processes of the tungsten-oxo framework. The new catalyst showed an electrocatalytic effect on the reduction of NO2-.

Synthesis and structure of molybdenum-citrato cluster mu(2)-S bridge

A new molybdenum-citrato cluster containing [Mo2O2(mu-S)(2)(C6H5O7)(C6H4O7)](5-) anion was synthesized and characterized by elemental analysis, IR, UV-Vis spectra, XPS and X-ray diffraction. The parameters of the crystal structure of the compound are monoclinic, space group P2(1)/c, a = 2. 376 6(5) nm, b = 1. 327 4(3) nm, c = 2. 247 1(5) nm, beta = 118. 21 degrees, V = 6. 247(2) nm(3), Z = 8, D-c = 2. 128 g/cm(3), F(000) = 3 984, mu = 1 694 cm(-1), R = 0. 083 1 and R-2,R-w = 0. 154 9. The anion is binuclear molybdenum-citrato complex with mu(2)-S bridge. Each molybdenum atom pocesesses a distorted octahedral struture, which is coordinated with a terminal oxygen, two sulfur atoms, three oxygen atoms of hydroxyl, alpha-carboxylate, beta-carboxylate from citrate.

含柠檬酸配体的钼硫簇合物的合成与晶体结构的测定

合成了含有Mo—S簇阴离子 [Mo2 O2 ( μ S) 2 (C6H5O7) (C6H4 O7) ]5-柠檬酸簇合物 ,并通过元素分析、红外光谱、紫外 可见光谱和X射线光电子能谱对配合物进行了表征 ,用X射线衍射法测定了该化合物的晶体结构 .结果表明 ,该簇合物属于单斜晶系 ,空间群P2 1/c,a =2 3 766( 5)nm ,b =1 3 2 74 ( 3 )nm ,c =2 2 4 71 ( 5)nm ,α=γ =90°,β=1 1 8 2 1°,V =6 2 4 7( 2 )nm3 ,Z =8,一致性因子R =0 0 83 1 ,R2 ,w=0 1 536.该簇合物阴离子中每一个Mo原子都采取扭曲的八面体结构 ,柠檬酸通过羟基、α 羧基、一个 β 羧基与Mo配位 .晶体结构表明在一个结晶学上不对称的结构单元内有两个结晶学上独立的分子.

Hydrothermal synthesis and structure of [{Mo8V4O36(VO4)(VO)(2)}(n)](7n-) bi-capped alpha-Keggin fragments linked to a chain

The title compound, (H(2)en)(3)H3O {MO8V4O36 (VO4) (VO)(2)} . 4H(2)O, was hydrothermally synthesized and structurally characterized by means of IR, ESR spectrum and single crystal X-ray diffraction. It crystallized in a monoclinic system with space group P2(1)/c, a=1. 980 4(4) nm, b=2. 063 4(4) nm, c=1. 192 0(2) nm, (beta =94. 76(3)degrees and deep black colour. The compound contains V-centered bi-capped alpha -Keggin fragments {Mo8V7O42} that are linked together by edge-shared units (VO5)-O-N via V-O-V bonds, forming a chain.

Synthesis and crystal structure of a novel compound constructed from tris-(2, 2 '-bipy)ruthenium(II) and decatungstate

Self-assembly of tris-[2,2 ' -bipyridine]ruthenium(II) chloride with decatunstate produced a novel cation radical salt, [Ru(bpy)(3)](2)[W10O32] . 3DMSO. This is the first product of 2,2 ' -bipyridineruthenium(II)-polyoxometalates species. Crystal data: Monoclinic, P2(1)/c, a = 12.902(3) Angstrom, b = 21.487(3) Angstrom, c = 15.854(5) Angstrom, beta = 93.46(2)degrees, V = 4387(2) Angstrom (3), Z = 2, R-1 = 0.0599, wR2 = 0.1183. X-ray crystallographic study showed that the crystal structure was constructed by electyrostatic attraction and C-H . . .O hydrogen bonds between tris-[2,2 ' -bipyridine]ruthenium(II) and decatungstate polyanion. The tris-[2,2 ' -bipyridine]ruthenium molecules occupy cavities in the polyoxometalate lattice ordered along b-axis. (C) 2001 Elsevier Science B.V. All rights reserved.

Synthesis and crystal structure of [Nd(eta(6)-1,3,5-C6H3Me3)(AlCl4)(3)]( C6H6) and structural comparison of Ln(eta(6)-arene)(AlCl4)(3)

Reaction of NdCl3, with AlCl3 and mesitylene in benzene gives complex [Nd(eta (6)-1,3,5-C6H3Me3) (AlCl4)(3)] (C6H6) (1) which was characterized by elemental analysis, IR spectra, MS and X-lay diffractions. The X-ray determination indicates that 1 has a distorted pentagonal bipyramidal geometry and crystallizes in the monoclinic, space group P2(1)/n with a = 0.9586(2), b = 1.1717(5), c = 2.8966(7) nm, beta = 90.85 (2)degrees, V = 3.2529(6) nm(3), D-c = 1.573 g/cm(3), Z = 4. A comparison of bond parameters for all the reported Ln(eta (6)-Ar) (AlCl4)(3) complexes indicates that the bond distance of Ln-C is shortened with the increasing of methyl group on benzene and with the decreasing of radius of lanthanide ions.

Synthesis, crystal structure and reactivity of (2,4-C7H11)(2)Yb center dot DME

(2,4-C7H11)(2)Yb . DME was synthesized by the reaction of YbCl3 with K(2,4-C7H11)(2,4-dimethylpentadienyl potassium), and the single crystal X-ray diffraction showed that the complex exists in a cis- staggered conformation. Thf crystal of the compound belongs to the monoclinic space group P2(1)/n with a = 0.675 2 (1) nm, b = 1.490 6 (1) nm, c = 1.529 3 (2) nm, beta = 97.55 (2)degrees, V = 1.977 79 (4) nm(3), Z = 4, F(000) = 735.8 e, mu = 49.49 cm(-1), R = 0.033 and R-w = 0.032. The title complex can be used as a catalyst for the polymerization of methyl methacrylate (MMA).

Synthesis and crystal structure of (1,3-(Bu2C5H3)-Bu-t)(2)Sm(mu-Cl)(2)Li(THF)(2)

Anhydrous SmCl3 reacts with two equal of Li(1-3-(Bu2C5H3)-Bu-t) to give a complex (1,3-(Bu2C5H3)-Bu-t)(2) Sm(mu -Cl)(2)Li(THF)(2) (C34H58Cl2LiO2Sm, M-r = 726.99), monoclinic, space group P2(1)/n, a = 10.615(2), b = 21.037(4), c = 17.166(3) Angstrom, beta = 93.60(3)degrees, V = 3825.7 (13) Angstrom (3), Z = 4, D-c = 1.262 Mg/m(3), mu = 1.699 mm(-1) and F(000) = 1508, final R = 0.0387 and wR = 0.0741 for 5320 observed[I greater than or equal to2 sigma (I)] reflections. The average Sm - C distance is 2.73 Angstrom. Sm - Cl1 and Sm - Cl2 distances are 2.719 (2) and 2. 697 (2) Angstrom, respectively. Two 1, 3-(Bu2C5H3)-Bu-t-ring centroids and two mu (2)-bridging chloride atoms around Sm atom form a distorted tetrahedron.

Estimation of individual phases from the four-phase structure invariants in the single isomorphous replacement case

The probability distribution of the four-phase invariants in the case of single isomorphous replacement has been developed to estimate some individual phases. An example of its application to obtain the phases having special values of 0, pi or +/-pi /2 is given for a known protein structure in space group P2(1)2(1)2(1). The phasing procedure includes the determination of starting phases and an iterative calculation. The initial values of starting phases, which are required by the formula, can be obtained from the estimate of one-phase seminvariants and by specifying the origin and enantiomorph. In addition, the calculations lead to two sets of possible phases for each type of reflection by assigning arbitrarily an initial phase value. The present method provides a possibility for the multisolution technique to increase greatly the number of known phases while keeping the number of the trials quite small.

Syntheses and crystalline structures of clusters Co-3(CO)(7)(mu(3)-S)(mu, eta(2)-SCNR2)

Through the reaction of Co-2(CO)(8) with four thiuram [R2NC(S)S](2), four new sulfur-capped trinuclear cobalt carbonyl clusters Co-3 (CO)(7) (mu(3)-S) (mu, eta(2)-S* C* NR2) ( I : R = Me; I : R = Et; II : R = i-Pr; IV : NR= -N [GRAPHICS] were prepared and characterized by elementary analysis, IR,H-1 NMR and MS spectroscopy. The crystal structure of the cluster Co-3(CO)(7)(mu(3)-S)[mu, eta(2)-S*C*N (i-Pr)(2)]( III) was determined by X-ray single crystal diffraction method. The crystal of m is monoclinic, belonging to space group P2(1)/n, and the cell parameters are as follows: a = 1, 145 2(2) nm, b = 1. 502 8(3) nm, c = 1, 214 4(2) nmj alpha = 90 degrees, beta = 92, 15(3)degrees, gamma = 90 degrees; V = 2. 088 5(7) nm(3) , Z = 4, F (000) = 1 096, D-c = 1. 747 mg . m(-3), mu = 2. 588 mm(-1), R=0. 040 7, R-w=0. 062 4, The structural analysis shows that cluster II has a pyrimidal Co3S framework and contains a heterocylic bridging bidentate ligand [mu, eta(2)-S* C* N (i-Pr)(2)] linked to the Co2 and Co3 atoms of the cluster by a cobalt-carbon and a cobalt-sulfur bond respectively.