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.

Synthesis, structure characterization of the complexes of beta-alkoxycarbonylethyltin trichlorides with Schiff base ligands

Thirty - two title complexes (ROCOCHRCH2SnCl3)-C-1 . (2 - HOC6H4CH = NC6H4 - X) (R = Me, Et, n - Bu; R-1 = H, Me; X = H,4' - Cl, 3' - Pr, 3' - OH, 3', 4' - Cl-2, 4' - OMe) were synthesized and characterized by elemental analysis,UV - vis, IR, H-1 NMR. The crystal structure of n - BuOCOCH2CH2SnCl3 . (2 - HOC6H4CH - NC6H4OMe - 4') were determined by the X - ray diffraction analysis, The crystal belongs to monoclinic system, with a = 1.4661 (3)nm, b = 0.9307 (2)nm, c = 1.7888 (4)nm, beta = 94.04 (3)degrees, V = 2.4348nm(3), D-c = 1.581mg/m(3), Z = 4, F(000) = 1160, mu = 1.405mm(-1), R = 0.0354, R-w = 0,0486, space group: P2(1)/c. The complexes exist as a discrete monomer. The tin atom has a distorted octahedral geometry due to intramolecular coordination of the carbonyl oxygen and the phenolic oxygen of the Schiff base ligands, The coordination number of tin atom is 6.

Synthesis and characterization of sandwiched heteropolycompound

New complex K5O4Na4H5 [Sn-3(PW9O34)(2)]. 16N(2)O was prepared and its structure was determined by elemental analysis, IR, P-31, W-183 NMR, polarography, XPS and X-ray crystallography. The anion has A-alpha-Keggin structure. The new complex crystallize is the monoclinic, P2(1)/n with a = 1.3625 (3) nm, b = 2.3625 (5) nm, c = 2.9306 (6) nm, alpha = 90 degrees, beta = 99.67 (3)degrees, gamma = 90 degrees, V = 9.299 nm(3), Z = 4.

Crystal Structure of [PrAl(CF3COO)(2)(CF3CHOO)(C2H5)(2)(C4H8O)(2)](2)

[PrAl (CF3COO)(2) (CF3CHOO) (C2H5)(2) (C4H8O)(2)](2) M-r = 1420. 56, monoclinic, P2(1)/n, a = 10. 651 (6) , b = 24. 276(9), c = 11. 110(5) Angstrom, beta = 107. 650 (4)degrees , V = 2737. 4(1) Angstrom (3) , Z = 2, D-c = 3. 45 g/cm(3) , F(000) = 2816 , T = 233K, MoK alpha radiation (lambda= 0. 71069 Angstrom), mu(MoK alpha) = 38. 017 cm(-1) , R = 0. 048 for 2847 observed reflections (I greater than or equal to 3 sigma(I)). It is isostructural with [LnAl (CF3COO)(2) (CF3CHOO) -R-2 (C4H8O)(2)](2) (Ln = Ho, R = Et; Ln = Ndt Y, R = Bu-1). Pr3+ is coordinated by eight oxygen atoms from five bridging ligands and two THF forming a distorted bicap-prism.

Co_3(CO)_7(μ_3-S)(μ,η~2-SCNR_2)的合成和晶体结构

Co2 (CO) 8 与 4个二硫代双 (烷基硫代甲酰胺 )类前配体 [R2 NC(S) S]2 反应 ,得 4个含烷基硫代甲酰胺基的三核钴羰基硫簇合物 .通过元素分析、IR、 1H NMR和 MS等方法表征了它们的结构 ,用 X射线衍射法测定了其中一个簇合物 Co3 (CO) 7(μ3 - S) [μ,η2 - SCN(i- Pr) 2 ]( )的晶体结构 .晶体属单斜晶系 ,P2 1/n空间群 ,晶胞参数 a=1.1452 (2 ) nm,b=1.50 2 8(3) nm,c=1.2 144 (2 ) nm,α=90°,β =92 .15(3)°,γ =90°,V =2 .0 885(7) nm3 ,Z=4 ,F (0 0 0 ) =10 96 ,Dc=1.74 7mg· m-3 ,GOF(F2 ) =0 .835,μ=2 .588nm-1.最终因子 R[I>2 σ(I) ]=0 . 0 4 0 7,Rw=0 .0 6 2 4

Synthesis, crystal structure and properties of (Z)-3-triphenylstannyl-1,1-diphenyl propenol

Five new organotin compounds were synthesized and characterized, X-ray crystal structure analysis of (Z)-3-triphenylstannyl-1,1-diphenyl propenol was performed, The crystal belongs to space group P2(1)/n. The cell parameters are: a = 1.235 7(2) nm, b = 0.987 4(2) nm, c = 2.208 1(4) nm, beta = 95.23(3)degrees, V = 2.683 0(9) nm(3), Z = 4, R = 0.027 9, R-w = 0.064 5. The tin atom of the molecule exists in a distorted tetrahedron, Z isomer of double bond is obtained.

Synthesis and structure of alpha-B-Keggin type heteropoly complex K5H[Co-4(VW9O33)(2)]center dot 5H(2)O

A new complex K5H[Co-4(VW9O33)(2)]. 5H(2)O was prepared and its structure was determined by X - ray diffraction analysis. The anion has alpha - beta - Keggin structure. Two (VW9O33)(7-) moieties (alpha - B isomers) are linked via four Co(11)O-6 groups. The single crystal of the title complex is monoclinic P2(1/n) with a = 1.2307(3) nm, b = 2.1250(4) nm, c = 1.5817(3) nm, beta = 91.86(3)degrees, V = 4.1343 (14) nm(3), R = 0.0895, R-w = 0.2180.

Synthesis and structural characterization of a novel polymeric praseodymium(III) complex with a new flexible double betaine

A novel polymeric Pr(III) complex with a new double betaine, namely [{Pr(L-1)(1.5)(H2O)(2)}(n)] [ClOli4]3(n). nH(2)O (1) (L-1= 1,4-diazoniobicyclo[2,2,2]octane- 1,4-dipropionate), has been synthesized and characterized by X-ray analysis. In the title complex, the Pr(III) atom is nine-coordinated by seven oxygen atoms from five L-1 ligands and two aqua ligands. Each pair of adjacent praseodymium(III) atoms is linked by a pair of mu(3) chelating and bridging carboxylate groups, thus forming an infinite metal metal chain running parallel to the a direction, and such chains are cross-linked by flexible backbones of L-1 ligands into a three-dimensional network with the perchlorate anions and lattice water molecules accommodated in the interstitial space. The title complex crystallizes in the monoclinic space group P2(1)/n with a = 8.085(2), b = 14.316(3), c = 29.775(6) Angstrom, beta = 103.04(3)degrees and Z = 4.

Syntheses of indenyl lanthanide derivatives and the molecular structures of [(C9H7)(2)PrCl(THF)](2) and [(C9H7)(3)La(THF)]

The reaction of anhydrous PrCl3 with Na(C9H7) in 1.2 mole ratio in THF gives [(C9H7)(2)PrCl(THF)](2)1. 1 crystallized in monoclinic system, space group P2(1)/c with a = 7.808(2), b = 17.796(6), c = 14.070(4) Angstrom, beta = 93.97(2)degrees, V= 1950.3(9) Angstrom(3), Dcalcd = 1.63 g/cm(3) and Z = 2. Each Pr ion is surrounded by two indenyl, two Cl and one THF in a roughly trigonal bipyramid arrangement with average Pr-C(ring) and Pr-Cl distances of 2.81 and 2.84 Angstrom. The reaction of LaCl3 with Na(C9H7) in 1:3 mole ratio gives (C9H7)(3)LaTHF 2, which crystallizes in the monoclinic space group P2(1)/a with unit cell constants a = 21.871(8), b = 10.585(3), c = 23.652(7) Angstrom,beta = 114.62(2)degrees, V = 4977.9 Angstrom(3) and Z = 8. (C) 1997 Elsevier Science S.A.