Single crystal structure of form I syndiotactic poly(butene-1)

The structures of single crystals of syndiotactic poly(butene-1) in form I, produced by thin-film growth, are studied by transmission electron microscopy and electron diffraction. Bright-field electron microscopy observation shows that the single crystal exhibits a regular rectangular shape with the long axis along its crystallographic b-axis. Electron diffraction results indicate an isochiral C-centered packing of a-fold helical chains in an orthorhombic unit cell corresponding to the C222(1) space group, according to the model proposed in the literature. The differences with the polymorphic behavior of syndiotactic polypropylene concerning the formation and the stability of the isochiral mode of packing are outlined.

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.

Photochemical synthesis and crystal structure of a charge transfer salt [HMDH2][(H2PMoMo11O40)-Mo-v]center dot 2AA center dot 3H(2)O center dot DMF

The title supramolecular compound, [HMDH2][(H2PMoMo11O40)-Mo-V] . 2AA . 3H(2)O . DMF (HMD = hexamethylene diamine; AA=acetaldehyde; DMF=N,N-dimethyl formamide), has been photochemically synthesized by using elemental analysis, IR, solid diffusion reflectance, electronic spectra, ESR spectra and X-ray single-crystal analysis. The crystallographic data: triclinic, P (1) over bar, a=14.092(2), b=14.347(3), c=14.358(3)Angstrom, alpha = 75.10(3), beta = 80.70(3), gamma = 80.73(3)degrees, V = 2746.6(10)Angstrom (3), Z = 2, M-r = 2081.68, D-c=2.517g/cm(3), F(000) =1970, mu (MoK alpha) =2.766mm(-1). The structure has been refined to R =0.0832 and wR=0.2638, by full-matrix least-squares method. The title compound is composed of hexamethylene diamine, two acetaldehyde molecules, three water molecules, one N,N-dimethylformamide and [(H2PMoMo11O40)-Mo-V](2-) heteropoly anion.

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 a novel amino-acid-containing polyoxometalate: K-6[Cu (Ala)(2) (H2O)(2)](2)[ CU4 (H2O)(2) (AsW9O34)(2)] center dot 16H(2)O

The novel amino-acid-containing polyoxometalate Ka(6) [Cu(Ala)(2) (H2O)(2)](2) [Cu-4 (H2O)(2) . (AsW9O34)(2)] . 16H(2)O was synthesized from the reaction of K-10[Cu-4(H2O)(2)(AsW9O34)(2)] . 20H(2)O with beta -alanine, Its structure has been determined by single crystal X-ray diffraction. It crystallizes in the triclinic space group P (1) over bar, with a=1. 196 3(2) nm, b=1. 536 5(3) nm, c=1. 591 4(3) nm, alpha =93. 97(3)degrees, beta= 110. 88(3)degrees, gamma =101. 07(3)degrees, V=2. 651 8(9) nm(3) and Z=1. Least-squares refinement of the structure leads to R and R-w factors of 0. 067 3 and 0. 162 8, respectively. An unusual structural feature of the compound is that the polyanion [Cu-4(H2O)(2) (AsW9O34)](10-) is linked with the amino-acid complex of Cu2+ by a mu -oxygen atom.

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.

Synthesis, crystal structure and properties of H-8[P4W14O58Na4 (H2O)(20)] center dot 16H(2)O

A novel heteropoly tungstophosphates, H-8[P4W14O58Na4(H2O)(20)] . 16H(2)O, was synthesized by hydrothermal method and characterized by elemental analysis, IR spectrum and single-crystal X-ray structure analysis. The thermal stability of the compound was investigated by using TG-DTA. The crystal is triclinic system with space group P (1) over bar, a = 1. 137 9(2) nm, b=1. 363 2(3) nm, c=1. 627 1(3) nm; alpha=78. 20(3)degrees, beta=71, 20(3)degrees, gamma= 71. 62(3)degrees; V = 2. 252 5(8) nm(3), Z=1, M-r= 4 374. 38, D-c = 3. 225 mg/cm(3), mu = 18. 007 mm(-1), F(000)=1 972, R=0. 074 2, R-w=0. 200 4. The result of structure analysis shows that the anion of the compound consists of two PW7O29Na2(H2O)(10) subunits and two linked phosphorous atoms. A kind of microporous with size of 0. 661 4 nm X 0. 318 9 nm was formed in the crystal structure.

Effect of electron radiation on crystal structure transition of trans-1, 4-polybutadiene

trans-1,4-Polybutadiene (PTBD) was synthesized by rare earth catalyst system, The effect of electron radiation on phase transition from monoclinic phase to hexagonal phase was observed by TEM, Electron diffraction patterns of monoclinic phase, hexagonal phase and two coexistent phases were recorded, The mechanism of phase transition was also discussed in this paper.

Hydrothermal synthesis and crystal structure of Co(En)(3)MoO4

Co(En)(3)MoO4 was synthesized by using the method of hydrothermal synthesis and characterized by elemental analysis, IR, ESR and single-crystal X-ray methods. It crystallizes in hexagonal space group P (3) over bar C1 with a=1.596 4(2) nm, b=1.596 4(2) nm, c = 0.993 5(2) nm, alpha=beta=90 degrees gamma=120 degrees, M-c=399.18, V=2.192 6(6) nm(3), D-c=1.814 g/nm(3), Z=6, F(000)=1 2181 R-1=0.070 3, R-w=0.220 7. According to separation of anion which acted on electrostatic potential, the anion and cation ions formed a type of organic and inorganic material.

Crystal structure of mixed sodium-potassium paradodecatungstate 6-hydrate

The crystal structure of K7Na3[H2W12O42]3 . 6H(2)O was determined by X-ray crystallography,and refined to R=0.0864 based on 7024 observed reflections (I>2 sigma(I)). The crystallographic parameters are a=11.755(2), b=13.0493(3), c=16.289(3) Angstrom; alpha=77.13(3)degrees, beta=82.92(3)degrees, gamma=89.65(3)degrees, triclinic, space group, P (1) over bar, V=2416.7(8) Angstrom(3), Z=2, M-r=3330.98, D-cal=4.578Mg/m(3), F(000)=2904; mu (MoK alpha)=29.170mm(-1), T=293K. Two independent polyanions are centered respectively at 1,1,1/2 and 1/2, 1/2, 0, approximately perpendicular to each other with dihedral angle between the equatorial planes of the molecules at 96 degrees. K+ and Na+ respectively occupy the clefts of the two discrete polyanions.

Hydrothermal synthesis and crystal structure of sandwich-like heteropolymolybdophosphates

Sandwich-like heteropoly molybdochromophosphates of supermolecular compound [NH3(CH2)(6)NH3](2)H-3{Cr[Mo6O15(HPO4)(H2PO4)(3)](2)}. 4H(2)O has been hydrothermally synthesized and the single crystal structure has been determined by X-ray diffraction. The crystal data are has follows: triclinic, space group P (1) over bar a=12.156(2), b=12.809(3), c=13.530(3) Angstrom, alpha=102.46(3)degrees, beta=93.67(3)degrees, gamma=93.46(3)degrees, V=2046.9(7) Angstrom(3), Z=1, M-r=2768.69, D-c=2.246 g/cm(-3), F(000)=1337, mu=2.162 mm(-1). The structure has been refined to R=0.0666 and wR=0.1745 by full-matrix least-squares method. The title compound is composed of 1, 6-diaminohexane, water molecules, and {Cr[Mo6O15(HPO4)(H2PO4)(3)](2)}(7-) anion which consists of six oxygen atoms from two [Mo6P4] units with a sandwich-like transition metal atom Cr located at the center of symmetry.

Synthesis and crystal structure of a novel butterfly-like complex, [WOS3Cu2(PPh3)(2)(Py)(2)] (Py = pyridine)

A new butterfly-like cluster [WOS3Cu2(PPh3)(2)(Py)(2)] was obtained by reacting [WOS3Cu2(PPb3)(3)] with pyridine. The crystal structure of the cluster has been determined by X-ray diffraction. The compound shows an unusual folded structure, in which two 4-coordinate Cu atoms are bound to the WOS3 moiety via two S-S edges.

Crystal structure and drawing-induced polymorphism in poly(aryl ether ether ketone). IV

A new crystal modification induced by strain and denoted as form II exists alongside the dominant form I structure in the uniaxially oriented poly(ether ether ketone) (PEEK) and the related polymers. The crystal structure of form II for PEEK is also found to possess a two-chain orthorhombic packing with unit cell parameters of a equal to 0.475 nm, b equal to 1.060 nm, and c equal to 1.086 nm. More extended and flattened chain conformation of form II relative to that of form I is expected to account for an 8% increase in c-axis dimension, which is attributed to the extensional deformation fixed in situ through strain-induced crystallization during uniaxial drawing. Annealing experiments suggest that form II is thermodynamically metastable and can be transformed into more stable form I by chain relaxation and reorganization at elevated temperature without external tension. This strain-induced polymorphism exists universally in the poly(aryl ether ketone) family. (C) 1999 John Wiley & Sons, Inc.

Synthesis, crystal structure and luminescence studies of a lanthanide coordination polymer with a new double betaine ligand

A novel europium(III) coordination polymer with a new double betaine derivative, {[Eu(L')(NO3)(H2O)(3)](NO3)(2). 3.5H(2)O}(n) (L-1 = 1,3-bis(pyridinio-4-carboxylato)-propane) has been synthesized and its structure determined. Its luminescence properties have also been studied. The title metal carboxylate coordination polymer contains centrosymmetric dimeric units in which each pair of metal ions is linked by a pair of syn-anti carboxylato-O,O' groups, and each pair of such dimeric units is bridged by the backbones of L-1 ligands to form infinite double chains in the b direction. These metal carboxylate chains are further cross-linked by hydrogen bonds among both coordinated and discrete nitrate anions, aqua ligands and lattice water molecules to form a three-dimensional network. Luminescent data show that the L-1 ligand is a good energy donor and the complex has a relatively long luminescent lifetime.

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.