Lewis-Base Adducts of Main Group 1 Metal Compounds. IV. Synthesis and Structure of the XLiL3 System (X = Cl, Br, I, L = 4-t-Butylpyridine, and X = I, L = Quinoline)

1988 ◽  
Vol 41 (3) ◽  
pp. 341 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Main Group ◽  
Lewis Base ◽  
Similar Data ◽  
Metal Compounds ◽  
X Ray ◽  
Close Parallel ◽  
Group 1

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.

Lewis-Base Adducts of Main Group 1 Metal Compounds. V. Diaquabis(quinoline)lithium(I) Bromide Bis(quinoline)

1988 ◽  
Vol 41 (3) ◽  
pp. 409 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Lithium Bromide ◽  
Main Group ◽  
Lewis Base ◽  
Metal Compounds ◽  
X Ray ◽  
Group 1

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.

Lewis-Base Adducts of Main Group 1 Metal-Compounds. XIII. Synthesis and Structures of Some Pyridine Base Lithium Bromide and Iodide Adducts

1990 ◽  
Vol 43 (7) ◽  
pp. 1163 ◽  
Author(s):  
CL Raston ◽  
WT Robinson ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Lithium Bromide ◽  
Main Group ◽  
Lewis Base ◽  
Metal Compounds ◽  
X Ray ◽  
Pyridine Base ◽  
Structure Determinations ◽  
Group 1

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.

Lewis-Base Adducts of Main Group 1 Metal(I) Compounds. XIV. Synthesis and Crystal Structure of a 1 : 1 Lithium(I) Chloride Sulfolane Adduct

1991 ◽  
Vol 44 (2) ◽  
pp. 309 ◽  
Author(s):  
S Harvey ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Main Group ◽  
Lewis Base ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Group 1

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.

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
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Main Group ◽  
Lewis Base ◽  
Metal Compounds ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ray Methods ◽  
Group 1

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.

Lewis-Base Adducts of Main Group 1 Metal Compounds. X. Lithium Bromide and Iodide Complexes With Acetonitrile (1 : 2, 1 : 4 Respectively)

1989 ◽  
Vol 42 (1) ◽  
pp. 201 ◽  
Author(s):  
CL Raston ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Lithium Bromide ◽  
Main Group ◽  
Lewis Base ◽  
Single Crystal Structure ◽  
Metal Compounds ◽  
Structure Determinations ◽  
Group 1

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).

Lewis-Base Adducts of Main Group Metal(I) Compounds. XI. Di-μ-iodo-bis(N,N,N′,N″,N″-pentamethyldiethylenetriamine-N,N′,N″-sodium)

1989 ◽  
Vol 42 (8) ◽  
pp. 1393 ◽  
Author(s):  
CL Raston ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Main Group ◽  
Lewis Base ◽  
Coordination Complex ◽  
X Ray ◽  
Group Metal ◽  
Main Group Metal

The synthesis and structural characterization of the 1:1 adduct of sodium(I) iodide and N,N,N′,N″,N″- pentamethyldiethylenetriamine (pmdeta), a novel coordination complex of sodium(I), is recorded. Single-crystal X-ray structure determination shows the compound to be a �,�′- diiodo-bridged dimer, with the tridentate base making up the five-coordinate environment of sodium: [( pmdeta )NaI2Na( pmdeta )]. Crystals are triclinic, P1, a 10.113(2),b 9.470(2), c 8.793(4) � , α 114.48(2), β 92.09(2), γ 96-65(1)°, Z= 1 dimer ; R was 0.037 for 1837 'observed' reflections.

Lewis-Base Adducts of Main Group-1 Metal-Compounds. IX. Synthesis and Structural Characterization of Adducts of the Lithium(1) Halides With N,N,N',N'-Tetramethylethylenediamine

1988 ◽  
Vol 41 (12) ◽  
pp. 1925 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Chloride Complex ◽  
Lewis Base ◽  
Metal Compounds ◽  
X Ray ◽  
Binuclear Species ◽  
Iodide Form ◽  
Group 1

Crystalline adducts of the lithium(I) halides, LiX (X = Cl , Br, I) with N,N,N′,N′- tetramethylethyl-enediamine (tmeda) have been synthesized and characterized by single-crystal X-ray studies. Both bromide and iodide form 1 : 1 adducts which are μ,μ-dihalo-bridged binuclear species, [( tmeda )LiX2Li( tmeda )], with four-coordinate N2LiX2 lithium environments; in addition, the iodide yields an ionic 1 : 2 adduct, [Li( tmeda )2]+I-. The chloride complex is a novel 3 : 2 polymer based an a double cubane Li6Cl6 unit solvated by chelating and bridging tmeda units.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. XXXVII. A Novel Isomerism in the Heterobimetallic 1:1 Adducts of Copper(I) Halides With Tris(dithiocarbamato)cobalt(III)

1988 ◽  
Vol 41 (6) ◽  
pp. 839 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Lewis Base ◽  
X Ray

Reaction of copper(I) iodide with tris (N,N- dipropyl -and N, N- diisopropyl-dithiocarbamato )cobalt(III), [Co(S2CNR2)3 ≡ Co( dtc )3](R = Pr or Pri ), yields 1:1 adducts which have been characterized by single-crystal X-ray structure determination. Crystals of the propyl species are monoclinic, P21/c, a 13.722(7), b 16.854(7), c 16.787(8)Ǻ, β 121.66(3)°, R was 0.056 for No 2834 'observed' reflections. The isopropyl derivative is orthorhombic, Ccca , a 33.93 (1), b 13.616(8), c 14.574(5)Ǻ; R was 0.075 for No 726. Each adduct is dimeric [Co( dtc )3](CuI2Cu)[Co( dtc )3]; the propyl derivative has crystallographically imposed i symmetry, whereas the isopropyl adduct has quasi-222 symmetry. Thus, the chiralities of the pair of Co( dtc )3 moieties in the dipropyl adduct are opposite, whereas in the isopropyl adduct they are the same.

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