Lewis-Base Adducts of Main Group 1 Metal-Compounds. XII. Synthesis and Crystal Structure of (2,2′-Bipyridine)(bromo)(propan-2-ol)lithium(I)

1990 ◽  
Vol 43 (4) ◽  
pp. 755 ◽  
Author(s):  
BW Skelton ◽  
CR Whitaker ◽  
AH White

The title compound is readily crystallized from a 1 : 1 mixture of 2,2′-bipyridine and lithium(I) bromide in propan-2-ol; its structure has been established by single-crystal X-ray methods at c. 295 K. Crystals are monoclinic, P21/c, a 10.942(3), b 15.060(4), c 9.359(3)Ǻ, β 108.57(2)°, Z = 4; R was 0.050 for 1820 'observed' reflections. In the four-coordinate LiBrN2O environment, Li- Br,O are 2.47(1), 1.94(1)Ǻ, and Li-N are 2.05(1), 2.07(1)Ǻ.

1988 ◽  
Vol 41 (3) ◽  
pp. 409 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White

The title compound, an artefact of recrystallization of lithium bromide from improperly dried quinoline, has been characterized by a single- crystal X-ray structure determination. Crystals are triclinic, Pī , a 16.608(9), b 12.27(1), c 7.962(8)Ǻ, α 101.98(8),β 91.79(7),γ 92.27(6), Z 2; R was 0.058 for 2404 'observed' reflections. The cation is the first to be structurally defined for a [Li(OH2)2 (N-base)2]+ system; Li-O are 1.92(2), 1.93(2)Ǻ and Li-N 2.12(2), 2.14(2)Ǻ.


1991 ◽  
Vol 44 (2) ◽  
pp. 309 ◽  
Author(s):  
S Harvey ◽  
BW Skelton ◽  
AH White

Crystallization of anhydrous lithium(I) chloride from dry sulfolane yields a colourless crystalline 1 : 1 adduct, characterized by analysis and a single-crystal X-ray structure determination. Crystals are orthorhombic, Pna21, a 10.940(3), b 9.611(4), c 6.576(3)Ǻ, Z= 4 formula units; R was 0.033 for 869 independent 'observed' reflections. The structure is an infinite polymer containing four-coordinate (LiCl2O2) lithium, bridged by Li-Cl interactions and O,O′ sulfolanes. Li- Cl, Cl′ are 2.375(8), 2.309(7), and Li-O, O′ 2.016(7), 1.991(6)Ǻ.


1989 ◽  
Vol 42 (1) ◽  
pp. 201 ◽  
Author(s):  
CL Raston ◽  
CR Whitaker ◽  
AH White

Although only sparingly soluble in acetonitrile, lithium(1) bromide and iodide crystallize as acetonitrile adducts, structurally characterized as LiX/MeCN 1 : 2 and 1 : 4 respectively by single-crystal structure determinations. The bromide is a �,�′-dibromo-bridged dimer , ( MeCN )2LiBr2Li( NCMe )2)] (monoclinic, P21/n, a 7.624(2), b 12.61 2(2), c 8.047(3) � , β 98.94(3)°p; Z 2 dimers; R 0.038 for No 1081 'observed' reflections); Li-Br, N 2.534(7), 2.492(8); 2.031(9), 2.047(8) � respectively, with Li…Li, 3.17(1); Br…Br, 3.8989(9) � respectively. The iodide is ionic, [Li( NCMe )4]+1- (orthorhombic, P21221, a 20.66(1), b 12.208(6), c 8.4296) �, Z 6; R 0.062 for No 866).


1988 ◽  
Vol 41 (3) ◽  
pp. 341 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White

Complexes [XLiL3], X = Cl , Br, I; L = 4-t-butylpyridine, (1)-(3) have been synthesized by recrystallization of the anhydrous lithium halide from the parent base, and characterized structurally by single-crystal X-ray structure determination. (1) and (2) are isomorphous (monoclinic, P21), a ≈ 11.8, b ≈ 12.1, c ≈ 11.8 Ǻ, β 120°, Z 2 (R 0.051, 0.040 for No 1491, 1499 'observed' reflections); (3) is orthorhombic, Pbca, a 22.119(10), b 21.108(10), c 12.845(10) Ǻ, Z 8, R 0.067 for No 967. (1)- (3) are all pseudo- trigonal and contain four-coordinate XLiN3 arrays [Li-X, 2.33(1); 2.53(1); 2.76(4) Ǻ; Li-N, 2.03(1)-2.11(1); 2.04(1)-2.09(2); 2.03(4)-2.07(4)Ǻ]. Similar data are also recorded for X = I, L = quinoline (4)[monoclinic, P21/c, a 15.684(6), b 7.693(4), c 26.758(12) Ǻ,β 107.71(3)°, Z 4; R 0.072, No 3096; Li-I, 2.78(2); Li-N, 2.08(2)- 2.13(2)Ǻ]. While a close parallel may be drawn between the similarity of the chemistry of lithium(I) and copper(I) in respect of (1)-(3), (4) is unusual being the first XML3 derivative for a quinoline -type ligand; it is a monoquinoline solvate.


1990 ◽  
Vol 43 (7) ◽  
pp. 1163 ◽  
Author(s):  
CL Raston ◽  
WT Robinson ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White

The syntheses and single-crystal X-ray structure determinations of adducts of the lithium(I) halides with the following stoichiometries are reported: 1 : 3 lithium(I) bromide, iodide/ pyridine, monomers; 1 : 2 lithium(I) bromide/ quinoline and lithium(I) iodide/ quinaldine , both as [L2LiX2LiL2] dimers ; and 1 : 1� lithium(I) iodide/2,4,6-trimethylpyridine, 'step' tetramer.


1998 ◽  
Vol 53 (2) ◽  
pp. 239-241 ◽  
Author(s):  
Regina Bettenhausen ◽  
Wolfgang Milius ◽  
Wolfgang Schnick

Abstract The title compound has been synthesized as a green solid by the reaction of MeCl2 SiNHSiMe3 and Ti(NMe2)4 in CH2Cl2. The crystal structure was determined by single crystal X-ray methods at room temperature (C2/c, a = 1825,7(4), b = 909,9(2), c = 1116,1(2) pm, β = 125,09(3)°, Z = 4,R1= 0,047, wR2 = 0,147) to be an ionic salt [H2NMe2]+[(Me2NH)2TiCl4]- . The central titanium(III) atom of the anion is bound to four Cl atoms and weakly coordinated by two Me2NH ligands.


1994 ◽  
Vol 49 (12) ◽  
pp. 1654-1658 ◽  
Author(s):  
Markus Wieber ◽  
Stefan Lang ◽  
Stefan Rohse ◽  
Ralph Habersack ◽  
Christian Burschka

The synthesis of triphenyltelluroniumsulfide (Ph3TeS)4 is described together with a NMR-spectroscopic characterization. The structure of the title compound was determined by single crystal X-ray diffraction. Crystals of triphenyltelluroniumsulfide are triclinic (space group P1) with the cell parameters a = 1178.0(3) pm. b = 1295.8(6) pm. c = 1298.7(4) pm, α = 77.67(3)°, β = 82.18(2)°, γ = 66.00(2)° (V = 1766(1) × 106 pm3) and Z = 2. The compound appears to form a step-like structure of two [Ph3TeS]2 units and crystallizes with two molecules of CH2Cl2 per unit cell.


2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides


2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Shuang Gao ◽  
Hai-Tao Qu ◽  
Fei Ye ◽  
Ying Fu

A new compound,N-dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine, was synthesized and characterized. The crystal structure of the title compound (C11H10Cl3NO2,Mr=294.55) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space groupP21/c, witha=6.7619(14),b=24.866(5),c=9.737(3) Å,α=90.00,β=130.982(18),γ=90.00°,V=1235.9(5) Å3,Z=4,Dx=1.583 Mg/cm3,λ(Mo  Ka)=0.71073 Å,F(000)=600,μ=0.729 mm−1,R=0.0476, andwR=0.1274for 2217 reflections withI>2σ(I).


1997 ◽  
Vol 52 (7) ◽  
pp. 819-822 ◽  
Author(s):  
Bernd Schwarze ◽  
Wolfgang Milius ◽  
Wolfgang Schnick

Abstract The chlorinated titanium amides [(Cl3Si)2N]2TiCl2 (1) and (Cl3Si)2NTiCl3 have been syn­thesized selectively from hexachlorodisilazane lithium and TiCl4. The crystal structure of 1 was determined by single crystal X-ray methods at room temperature (P212121, a = 1232.4(2), b = 1265.5(2), c -1469.1(2) pm, Z = 4). The central titanium atom of 1 is bound to two nitrogen atoms and two Cl atoms and is weakly coordinated further by two Cl atoms of the trichlorosilyl groups.


Sign in / Sign up

Export Citation Format

Share Document