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 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.

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.

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.

Synthesis, properties and crystal structure of charge-transfer salt (DBTTF)(6)HSiMo12O40H2O

Charge-transfer salt (DBTTF)(6)HSiMo(12)O(40)4H(2)O was synthesized by electrocrystallization and characterized by IR spectrum and electronic spectrum. Its magnetic property, conductivity and crystal structure were determined. The title compound consists of heteropoly anions, water molecules and DBTTF columns which are formed by repeated arrangement of tetramer (DBTTF), in the direction of 15 degrees to the a axis in the tunnel constituted by the anions and other type of DBTTF. The title compound is paramagnetic and semiconducting. (C) 1998 Elsevier Science Ltd. All rights reserved.

Synthesis, electrical properties and crystal structure of a new radical-ion salt based on pi-extended bis(TTF) and a Keggin heteropolymolybdate

By electrocrystallization of 2,6-[4,5-bis(n-butylsulfanyl)-1,3-dithiol-2-ylidene]-4,8-bis(6-iodo-n-hexyloxy)-1,3,5,7-tetrathia-s-indacene (BHBDTI) and [NBu4](4)[SiMo12O40] in the mixed solvent CHCl2CH2Cl and CH3CN, the new radical-ion salt [C42H60Cl2O2S12](2)[SiMo12O40] was prepared. It was characterized by means of IR and ESR spectroscopy and X-ray diffraction. In the crystal structure, organic radical dications and silicomolybdate anions are alternatively arranged along the a axis to form a 1-D conducting layer. The organic layer consists of two isolated groups of BHBDTI divided by the (011) plane without short interatomic contacts. However, in each group, BHBDTI molecules associate with each other in a head to tail manner running along the [011] direction and face-to-face overlapping with a relative shift by approximately one TTF subunit along the long axis of the molecule and a slight shift along the short axis of the molecule with significantly short S ... S contacts. The room-temperature d.c. conductivity determined by the two-probe method is 10(-4) S cm(-1), suggesting that the compound is a semiconductor.

Synthesis and crystal structure of a polymeric erbium(III)-sodium(I) coordination complex of picolinic acid N-oxide

A new Er(III)-Na(I) coordination polymer of stoichiometry [NaEr2L5(H2O)(6)(NO3)](NO3). 3.5H(2)O (HL = picolinic acid N-oxide) has been synthesized and characterized by single-crystal X-ray analysis. Crystals are triclinic, P (1) over bar with a = 9.823(2), b = 12.453(2), c = 20.643(4) Angstrom; alpha = 98.49(3), beta = 101.40(3), gamma = 108.69(3)degrees; V = 2284(1) Angstrom(3); Z = 2. Of the two independent eight-coordinate erbium(III) ions in this complex, one is surrounded by four bidentate chelating L ligands, and the other by one bidentate chelating L ligand, four aqua ligands and two anti-carboxylate oxygen atoms from two neighboring [ErL4] units. The sodium(I) ion is in a distorted octahedral environment, being coordinated by a unidentate nitrate anion, three aqua ligands and two anti-carboxylate oxygen atoms from two adjacent [ErL4] units. The complex is built from zigzag chains of syn-anti carboxylate-bridged erbium(III) moieties directed in the a direction, which are cross-linked pairwise by aqua-bridged dimeric sodium(I) units. The resulting composite polymeric chains are further connected by hydrogen bonds to form a three-dimensional network.

Synthesis, properties and crystal structure of organic-inorganic radical salt (DBTTF)(6)HPMo12O40 center dot 2H(2)O

Organic-inorganic radical salt (DBTTF)(6)PMo12O40 . 2H(2)O was synthesized by electrocrystallization and characterized by IR spectrum, electronic spectrum and ESR technology, Its magnetic property, conductivity and crystal structure were determined. The title compound crystallized in a triclinic system with P1 space group, a = 1.378 7(7), b = 1.420 4 (2), c = 1.570 2(2) nm, alpha = 104.57(1)degrees, beta = 103.41(2)degrees, gamma = 95.80(2)degrees, V = 2.853(2) nm(3) Z = 1 and a final R = 0.072 7.

Synthesis and crystal structure of chiral bis(cyclopentadienyl) samarium Schiff base complexes bearing intramolecular C-C bond formation and hydrogen transfer

SmCl3, reacted with CpNa (Cp = Cyclopentadienyl) in the ratio of 1:3 in THF, which then was reacted with (S)-(+)-N-1-(phenylethyl) salicylideneamine/toluene to yield the title complex, [GRAPHICS] The X-ray crystal structure determination of the title complex reveals that 1 is a dimer with intramolecular C-C bond formation and hydrogen transfer, which leads to the configuration turnover of the carbon atom at the benzyl position of the ligand, while those of the newly formed asymmetric centers may have either Ii or S type configurations. (C) 1998 Elsevier Science Ltd. All rights reserved.

Synthesis and crystal structure of aluminium complex with 3-hydroxyflavone

[Al(C15H9O3)(3)](2) . 2CHCl(3) . 8H(2)O was synthesized, and its crystal structure was determined. It belongs to trigonal system, R3, a=b=1. 655 8(3) nm, c=3. 646 5(20) nm, alpha = beta = 90 degrees, gamma = 120 degrees, V = 8. 656 08(0. 005 86) nm(3). D-c = 1.45 g/cm(3), mu(Mo K alpha) = 3. 20 cm(-1), F (000) = 3 924. The crystal structure was solved by Patterson and Fourier techniques, and refined by a block-diagonal least-squares method. A total of 3 737 independent intensity data were collected, of which 1 033 with I greater than or equal to 3 sigma(I-0) were observed, R = 0. 091 8, Rw=0. 091 8. Al3+ ion was 6-coordinated, bound to six oxygen atoms from three 3-hydroxyflavones to form a distortional coordination octahedron.

Synthesis, extraction and electronic structure of Ce@C-2n

In view of the growing interest in endohedral lanthanide fullerenes, Ce, as a typical +4 oxidation state lanthanide element, has been systematically studied. The synthesis, extraction and electronic structure of Ce@C-2n are investigated. Soot containing Ce@C-2n was synthesized in high yield by carbonizing CeO2-containing graphite rods and are back-burning the CeC2-enriched cathode deposit in a DC are plasma apparatus. Ce@C-2n, dominated by Ce@C-82, can be efficiently extracted from the insoluble part of the soot after toluene Soxhlet extraction by pyridine at high temperature and high pressure in a closed vessel. About 60% Ce@C-2n (2n = 82,80,78,76) and 35% Ce@C-82 can be enriched in the pyridine extract. This fact is identified by desorption electron impact mass spectrometry (DEI MS). The electronic structure of Ce@C-2n is analyzed by using X-ray photoemission spectroscopy (XPS) of pyridine-free film. It is suggested that the encapsulated Ce atom is in a charge state close to +3 and was effectively protected from reaction with water and oxygen by the enclosing fullerene cage. Unlike theoretical expectation, the electronic state of Ce@C-82 is formally described as Ce+3@C-82(3-). (C) 1997 Elsevier Science Ltd.

Synthesis, properties and crystal structure of a heteropoly compound containing titanium

K4H2CoW12O40. 2Ti02 . 9H(2)O crystallizes from an aqueous solution of Na2WO4, Co(OAc)(2) and Ti(SO4)(2). The compound has very similar i.r. and u.v. spectra to those of [CoW12O40](6-) and [CoW11TiO40](8-) but its polarographic behaviour is different from that of [CoW11TiO40](8-) and exhibits only reduction of tungsten(VI). A single crystal structural analysis indicates that this compound consists of the heteropolyanion [CoW12O40](6-), titanium-oxygen chain, potassium ions and water molecules.