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At least 109 records · Page 6

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DOE OSTI2018

Synthesis and crystal structure of the coordination polymer [{Li(H_2O)_3}{sub 2}(C{sub 36}H{sub 36}N{sub 24}O{sub 12})]Cl{sub 2}•6H{sub 2}O

The coordination polymer of the composition [{Li(H_2O)_3}{sub 2}(C{sub 36}H{sub 36}N{sub 24}O{sub 12})]Cl{sub 2}•6H{sub 2}O (1) was synthesized by heating an aqueous solution of lithium chloride and cucurbit[6]uril (CB[6]). According to single-crystal X-ray diffraction data, solvated lithium cations in compound 1 form coordination bonds with oxygen atoms of CB[6] molecules. Compound 1 was characterized by X-ray diffraction, IR spectroscopy, thermogravimetric and elemental analysis. Luminescence spectra of the new compound were measured.

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DOE OSTI2018

Coordination polymers based on zinc(II) and manganese(II) with 1,4-cyclohexanedicarboxylic acid

Three new metal-organic coordination polymers were obtained namely, [Mn{sub 3}(chdc){sub 3}-(NMP){sub 2}(DMF){sub 2}] (1, chdc{sup 2–} is trans-1,4-cyclohexanedicarboxylate, NMP is N-methylpyrrolidone, DMF is N,N-dimethylformamide), [Zn{sub 3}(chdc){sub 3}(NMP){sub 2}]•2NMP (2), and [Zn{sub 3}(chdc){sub 3}(ur)-(DMF){sub 0.5}]•DMF (3, ur is the urotropine). The crystal structures of polymers 1, 2, and 3 were determined by single-crystal X-ray crystallography. All three compounds were found to contain a trinuclear secondary building unit {M_3(OOC)_6}. Coordination polymers 1 and 2 have a layered structure, while polymer 3 has a three-dimensional coordination framework with isolated pores formed due to the presence of urotropine bridging molecules. Compounds 1 and 3 were characterized by IR spectroscopy, thermogravimetric and elemental analysis data, powder X-ray diffraction. Compound 3 was also characterized by UV-Vis diffuse reflectance spectrum.

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DOE OSTI2018

Synthesis and structural features of new pentacoordinated monofluorosilanes containing C,O-chelate ligands based on 2-amino acid N-methylamides

Pentacoordinated monofluorosilanes R{sup 1}SO{sub 2}NHCHR{sub 2}C(O)N(Me)CH{sub 2}SiMe{sub 2}F containing moieties of N′-methyl-N-(organosulfonyl)-2-amino acid amides of glycine, alanine, and leucine as C,O-chelating ligands were synthesized via the reaction of corresponding disiloxanes with BF{sub 3}•Et{sub 2}O. The structures of obtained compounds were investigated by single-crystal X-ray diffraction analysis.

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DOE OSTI2018

New benzo[f]quinolino[3,4-b][1,7]naphthyridine-6,8(5H,9H)-diones: synthesis, electronic, molecular, and crystal structures. Protonation and complexation with lanthanum and europium salts

A series of novel benzo[f]quinolino[3,4-b][1,7]naphthyridine-6,8(5H,9H)-diones, which are promising ligands for the extractive separation of actinides and lanthanides, and also their complexes with lanthanum and europium were synthesized. The molecular and crystal structures of one among the ligands were determined by single crystal X-ray diffraction. The protonation of compounds was investigated by IR and NMR spectroscopy. The electronic structure of starting substances and protonated forms was estimated by DFT calculations.

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DOE OSTI2019

Sterically hindered tetrylenes based on new 1,10-phenanthroline-containing diols: initiators for ε-caprolactone polymerization

Previously unknown tetradentate ONNO-type ligands 1–5 (4,7-di(4-R´-phenoxy)-2,9- di(HOCR{sub 2}CH)-1,10-phenanthrolines (R´ = Me, R–R = –(CH{sub 2}){sub 5}– (1), R = Me (2), R–R = 2,2-adamantylene (3); R´ = But, R–R = –(CH{sub 2}){sub 5}– (4), R = Me (5)) were synthesized by sequential treatment of 2,9-dimethyl-4,7-di(4-R´-phenoxy)-1,10-phenanthrolines 6 (R´ = Me) and 7 (R´ = Bu{sup t}) with excess LDA and appropriate dialkyl ketone. The structure of compound 4 was determined by single-crystal X-ray diffraction. Previously uncharacterized phenanthroline 6 was synthesized by the treatment of 4,7-dichloro-2,9-dimethyl-1,10-phenanthroline with excess p-cresol in the presence of KOH. The reaction of compounds 1–5 with one equivalent of Lappert´s germylene or stannylene, M[N(SiMe{sub 3}){sub 2}]{sub 2} (M = Ge, Sn), gave the corresponding germylenes 8–12 (M = Ge, R´ = Me, R–R = –(CH{sub 2}){sub 5}– (8), R = Me (9), R–R = 2,2-adamantylene (10), R´ = Bu{sup t}, R{sub 2} = –(CH{sub 2}){sub 5}– (11), R = Me (12)) and stannylenes 13–17 (M = Sn, R´ = Me, R–R = –(CH{sub 2}){sub 5}– (13), R = Me (14), R–R = 2,2-adamantylene (15), R´ = Bu{sup t}, R–R = –(CH{sub 2}){sub 5}– (16), R{sub 2} = Me (17)) in satisfactory yields. According to {sup 1}H, {sup 13}C, and {sup 119}Sn NMR data, the synthesized stannylenes are monomeric in solution, and the tin atom has a coordination number of 4. In the series of the compounds under consideration, stannylene 16 proved to be the most active initiator for e-caprolactone polymerization, whereas the germylenes were shown to be inactive in this process.

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DOE OSTI2019

Binding of gold(III) with silver(I) dipropyldithiocarbamate: supramolecular self-assembly (role of secondary Au…S and Ag…S bonds) and thermal behavior of the ionic-polymer complex ([Au(S{sub 2}CNPr{sub 2}){sub 2}][AgCl{sub 2}]){sub n}

The double ionic-polymer complex ([Au(S{sub 2}CNPr{sub 2}){sub 2}][AgCl{sub 2}]){sub n} (1) was prepared as an individual fixation form of gold(III) from NaCl solutions with silver(I) dipropyldithiocarbamate and was characterized by single-crystal X-ray diffraction and {sup 13}C magic-angle spinning (MAS) NMR spectroscopy. The structure of 1 comprises two nonequivalent centrosymmetric complex cations [Au(S{sub 2}CNPr{sub 2}){sub 2}]{sup +} (A and B) and the discrete linear anion [AgCl{sub 2}]{sup –}. Gold(III) cations are linked by pairs of unsymmetrical secondary Au…S bonds to form linear supramolecular chains (…A…B…)n. Neighboring cations are additionally linked by [AgCl{sub 2}]{sup –} anions via secondary Ag…S and Cl…S bonds, the anions being involved in the overall stabilization of the supramolecular structure. The cation–anion interactions lead to a distortion of the linear configuration of the [AgCl{sub 2}]{sup –} anion. The character of thermolysis of 1 accompanied by quantitative regeneration of bound Au and Ag was established by simultaneous thermal analysis.

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DOE OSTI2019

Metal-organic frameworks based on magnesium(II): adsorption and luminescence properties

Two new metal-organic frameworks based on magnesium(II) ions, [Mg{sub 4}(bdc){sub 3}(dma){sub 6}(NO{sub 3}){sub 2}]•DMA (1; bdc is 1,4-benzenedicarboxylate; dma, DMA is N,N-dimethylacetamide) and [Mg{sub 3}(bpdc){sub 3}(nmp){sub 4}] (2; bpdc is 4,4´-biphenyldicarboxylate; nmp is N-methylpyrrolidone), were synthesized in DMA or NMP, respectively. According to the single-crystal X-ray diffraction data, compound 1 is built of binuclear carboxylate units {Mg_2(O_2CR)_3}, which were previously not observed in metal-organic frameworks. Compound 2 is based on trinuclear carb oxylate units {Mg_3(O_2CR)_6}. Compound 1 has a layered structure (hcb topology), whereas compound 2 has a distorted three-dimensional cubic structure (pcu topology). The phase purity and chemical identity of the compounds were confirmed by IR spectroscopy, thermogravimetry, elemental analysis, and powder X-ray diffraction. Photoluminescence properties of both compounds are indicative of intraligand charge-transfer transitions of one (for 1) or two (for 2) types. Textural characteristics of an activated sample of 1 were measured by nitrogen and hydrogen adsorption at 77 K and by carbon dioxide adsorption at 195 K.

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DOE OSTI2019

Decarboxylation and electrophilic substitution in 3-tert-butyl-4-oxopyrazolo[5,1-c][1,2,4]triazines

Reactivity of 7-R-3-tert-butyl-4-oxo-4,6-dihydropyrazolo[5,1-c][1,2,4]triazine-8-carboxylic acids (R = NH{sub 2}, N{sub 3}, H) and products of their decarboxylation towards different electrophilic agents (chloroacetone, Boc{sub 2}O/NaN{sub 3}, DMF/POCl{sub 3}, TMSBr, N-halosuccinimides, and HNO{sub 2}) was studied. A selective synthesis of new C(7),C(8)-functionalized and N(1)-tert-butyloxycarbonyl-substituted 4-oxopyrazolo[5,1-c][1,2,4]triazines was performed. The structures of the synthesized compounds were confirmed by IR and NMR spectroscopy, high resolution mass spectrometry and single crystal X-ray diffraction analysis.

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DOE OSTI2018

Electrical and Thermal Conductivity of Solid Solution Sn{sub 1–x}Mn{sub x}Te (0 ≥ x ≥ 0.04)

Electrical and thermal properties of the Sn{sub 1–x}Mn{sub x}Te single crystals (0 ≥ x ≥ 0.04) with contacts of eutectic alloy 57Bi + 43Sn (in mass%) are investigated at temperatures from 77 to 300 K. Experimental results show that this alloy with specified single crystals forms ohmic contact with a sufficiently low contact resistance. The electronic thermal conductivity in some samples reaches about 50% of the total thermal conductivity, and structural defects contribute significantly to the thermal resistance of the crystals.