Crystal growth and structural analysis of PrMnO3 and TbMnO3

Single crystals of PrMnO3 and TbMnO3 were grown by floating zone method and the crystal structure was determined by single crystal X-ray diffractometry. The structure of these compounds belongs to the orthorhombic system (space group is Pnma, No. 62) with the lattice parameters alpha approximate to root (.) - a(p), b approximate to 2 (.) a(p) , c approximate to root 2.a(p) and Z = 4, where a(p) is ideal cubic perovskite cell parameter.

X-ray crystal structure and molecular mechanics calculations of (2,6-iso-dipropyl-phenylamide) dimethyl (tetra-methylcyclopenta-dienyl) silane titanium dichloride

Crystal and molecular structure of (2.6-dipropylphenylamide) dimethyl (tetra-methyl cyclopentadienyl) silane titanium dichloride (I) was fully characterized by X-ray diffraction. The crystal is obtained from a mixture of ether/hexane as orthorhombic. with a = 12.658 (3) Angstrom. b = 16.62 (3) Angstrom. c = 11.760 (2) Angstrom. V = 2474.2 (9) Angstrom(3). Z = 4, space group Pnma. R = 0.0399; Componud I compose of the pi-bounded ring with its dimethylsilyl-dipropyl phenyl amido group and the two terminal chloride atoms coordinated to central metal to form a so-called constrained geometry catalyst (CGC) structure. The result of molecular mechanics (MM) calculations on compound I shows that bond lengths and bond angles from the MM calculation are comparable to the data obtained from the X-ray diffraction study. The relation of the structure of CGCs and their catalytic activity by MM calculations is also discussed.

Synthesis and characterization of a novel hybrid single crystal [Ga-3(PO4)(3)F-2]H3O center dot (H3NCH2CH2)(2)NH2

A novel three-dimensional fluorinated gallium phosphate has been hydrothermally,synthesized by using diethylenetriamine as an organic structure-directing agent. X-ray single crystal structure analysis indicates this compound crystallizes in the orthorhombic space group P-bca, a = 1. 605 6 (7) nm, b = 1.011 4 (4) nm, c=1. 854 6(5) nm, V=3. 011 6(19) nm(3), Z=4. The three-dimensional framework based on linkage of corner-sharing polyhedron PO4, GaO4F and GaO4F2 delimit ten-ring channels along b axis in which the triply protonated amines are located serving as charge compensating guests and supporters.

Hydrothermal synthesis and crystal structure of [{Cu(2,2 '-bpy)(2)}(2)Mo8O26]: a beta-octamolybdate cluster covalently bonded to two {Cu(2,2 '-bpy)(2)}(2+) coordination complexes via bridging oxo groups

An organic-inorganic hybrid solid, (Cu(2,2'-bpy)(2))(2)Mo8O26, has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Dark green crystals crystallize in the orthorhombic system, space group Pna21, a = 24.164(5), b = 18.281(4), c = 11.877(2) Angstrom, alpha = 90 degrees, beta = 90 degrees, gamma = 90 degrees, V= 5247(2) Angstrom (3), Z = 4, lambda (MoK alpha) = 0.71073 Angstrom (R(F) = 0.0331 for 5353 reflections). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range 1.69 degrees < theta < 25.04 degrees using the omega -scan technique. The structure was solved by the direct method and refined by full-matrix least squares on F-2 using SHELXL-93. The structure of this compound consists of discrete (Cu(2,2'-bpy)(2))(2)Mo8O26 clusters, constructed from beta -octamolybdate subunits ((Mo8O26)(4-)) covalently bonded to two (Cu(2,2'-bpy)(2))(2+) coordination complexes via bridging oxo groups that connect two adjacent molybdenum sites. (C) 2001 Academic Press.

Hydrothermal synthesis and crystal structure of a novel layered compound [Ni(C10H8N2)(2)V3O8.5]

A novel layered compound, [Ni(C10H8N2)(2)V3O8.5], was hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 1.551 8(3) nm, b = 1.476 1(3) nm, c = 1.048 3(2) nm, beta = 92.02(3), V = 2.399 8(8) nm(3), Z = 4, R = 0. 046 7, wR(2) = 0. 085 9.

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 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.

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.

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

夹心杂多化合物的合成及晶体结构

PW_9O_(34)~(9-)(简写PW_9)阴离子可以与Sn~(4+)反应生成[Sn_3~Ⅳ(PW_9O_(34))_2]~(6-)杂多化合物.标题化合物经元素分析、红外、极借、~(31)P和~(183)W核磁共振谱、X射线光电子能谱及X射线单晶测定了结构.K_5O_4Na_4H_5[Sn_3(PW_9O_(34))_2]·16H_2O的单晶是单斜晶系,空间群P2_1/n,晶胞参数a=1.3625(3)nm,b=2.3625(5)nm,c=2.9306(6)nm,α=90°,β= 99.67(3)°,γ=90°,V=9.299nm~3,Z=4.它是一种三个Sn~(4+)在两个PW_9单元间的夹心结构.

β-烷氧羰乙基三氯化锡与Schiff碱配合物的合成、表征与结构

合成表征了32个标题化合物ROCOCHR~1CH_2SnCl_3·(2-HOC_6H_4CH=NC_6H_4-X)(R=Me,Et,n-Bu;R~1=H,Me;X=H,4’-Cl,3’-Br,3’-OH,3’,4’-Cl_2,4’-OMe),通过元素分析,UV-vis,IR和~1H NMR进行了表征n-BuOCOCH_2CH_2SnCl_3·(2-HOC_6H_4CH=NC_6H_4OMe-4’)的晶体结构分析表明,该晶体属单斜晶系,a=1.4661(3)nm,b=0.9307(2)nm,c=1.7888(4)nm,β=94.04(3)°;v=2.4348nm~3,Z=4;空间群P2_1/c.该化合物为含有分子内碳基氧配位,Schiff碱以酚羟基上的氧原子配位,中心锡原子为六配位,空间构型为畸变八面体构型的单分子有机锡化合物.

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.

Synthesis, structure characterization and transesterification of the complexes of beta-alkoxycarbonylethyltin trichlorides

Thirteen title complexes ROCOCH2CH2SnCl3 . L(R = C(1 similar to 5)alkyl;L = DBSO,HMPA) were synthesized and characterized by elemental analysis, IR,H-1 NMR. The crystal structure of n -PrOCOCH2CH2SnCl3 . DBSO was determined by the X-ray diffraction analysis. The crystal belongs to orthorhombic system,space group P2(1)2(1)2(1) with a = 1.062, b = 1.427, c = 1.635nm; Z = 4. The complex exists as a discrete molecule, and the tin atom attains a distorted octahedral geometry via the coordination of intramolecular carbonyl oxygen and the Lewis base donor atom. The transesterification of CH3OCOCH2CH2SnCl3 . L with alcohol was studied, and the intramolecular Lewis acid catalytic mechanism was suggested.