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.

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 Group 11 Metal(I) Compounds. LI. Synthesis and Structural Characterization of Mononuclear Chloro-, Bromo- and Iodo-pyridinebis(triphenylphosphine)copper(I) Complexes

1989 ◽  
Vol 42 (6) ◽  
pp. 895 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Copper Atom ◽  
Lewis Base ◽  
X Ray

Complexes [ XCu ( py )(PPh3)2], X = Cl, Br, I, py = pyridine, have been synthesized and characterized by single-crystal X-ray structure determination. Chloride and iodide derivatives have similar cells [ isomorphous (?) but not isostructural ], triclinic, pi, a = 19.5 A, b = 10.5, c = 9.6 � , α ≈ 66, β ≈ 86, γ ≈ 83�, Z = 2; the bromide is monoclinic, Cc, a 13.568(9), b 15.760(12), c 16.545(8) � , β 95.65(5)�, Z = 4. Cl, Br, I structures were refined to residuals of 0.042, 0.055, 0.039 for 4288, 2241, 4808 'observed' reflections. In all cases, the copper atom is four-coordinate; for such an array, Cu-X lengths are unusually short [2.318(2), 2.459(2), 2.636(1) � (Cl, Br, I) and Cu-N unusually long (2.14(1) � ], while (Cu-P) increase from 2.264 to 2.288 � across the series. The dominant aspect of the complexes is thus that of XCu (PPh3)2 solvated by pyridine.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXXIV Synthesis and Structure of the 1 : 1 Adduct of Silver(I) Nitrate with Triphenylstibine

1997 ◽  
Vol 50 (6) ◽  
pp. 671 ◽  
Author(s):  
Effendy ◽  
John D. Kildea ◽  
Allan H. White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Related Species ◽  
Room Temperature ◽  
Structural Data ◽  
Lewis Base ◽  
One Dimensional ◽  
X Ray ◽  
The One

The synthesis and room-temperature single-crystal X-ray structure determination of the 1 : 1 adduct of silver(I) nitrate with triphenylstibine, AgNO3/SbPh3 (1 : 1), is recorded, being monoclinic, Cc,a 12·824(2), b 15·794(4),c 9·796(2) Å, β 117·50(1)°, Z= 4; conventional R on F was 0·030 for 2881 independent ‘observed’ (I > 3σ(I)) reflections. The complex is a one-dimensional polymer with bridging nitrate groups, resembling in this respect its phosphine and arsine analogues. The completion of this study, along with related species recorded in accompanying papers, means that full structural data are now available for the complete array AgNO3/EPh3 (1 : n), E = P, As, Sb, n = 1–4, with the one exception of E = Sb, n = 2.

Lewis-Base Adducts of Lead(II) Compounds. III. Synthesis and Structural Characterization of Mononuclear (Nitrato-O,O′)bis(1,10-phenanthroline)-(thiocyanato-N)lead(II)

1989 ◽  
Vol 42 (2) ◽  
pp. 335 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
Lone Pair ◽  
Lewis Base ◽  
Lead Atom ◽  
X Ray

The isolation and single-crystal X-ray structure determination of the title compound, [(phen)2Pb(NCS)(O2NO)] is described; crystals are triclinic, P1, a 15.554(7), b 9-670(4), c 8.429(3) α 72.53(3), β 81.90(3), γ 72.88(3)� Z = 2, yielding R 0.052 for 3405 independent 'observed' reflections. The lead atom is seven-coordinate [Pb-N 2.49(1)-2.60(1) (phen), 2.89(1) (NCS); Pb-O 2.75(1), 2.89(1) �] with a large vacancy in the coordination sphere, possibly indicative of a stereochemically active lone pair.

Lewis Base Adducts of Lead(II) Compounds. I. Polymer Isomerism in Some 1-2 Adducts of Lead(II) Halides With Pyridine Bases

1987 ◽  
Vol 40 (12) ◽  
pp. 2107 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Coordination Sphere ◽  
Structure Determination ◽  
Lone Pair ◽  
Lewis Base ◽  
The Other ◽  
X Ray ◽  
Coordination Sites ◽  
Pyridine Bases ◽  
Orthogonal Geometry

Recrystallization of lead(II) halides, PbX2 (X = C1, Br, I), from n- methylpyridine, n = 3, 4, yields crystalline 1 : 2 adducts; these have all been shown by single-crystal X-ray structure determination to contain the lead in an essentially octahedral six-coordinate environment, two of the coordination sites being occupied by monodentate pyridine base moieties and four by bridging halogen, yielding infinite polymeric arrays. For X = Cl, Br, n = 3, the nitrogen atoms lie cis in the coordination sphere; for the other complexes, they are trans. In the two cis complexes, distortion from ideal orthogonal geometry is more substantial than in the trans, possibly indicative of the presence of a sterically active 'lone pair'.

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 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 Group 11 Metal(I) Compounds. LXI. The 1 : 1 Adducts of the Copper(I) Halides (Cl, Br, I) With Bis(2-diphenylphosphinoethyl)phenylphosphine, 'triphos'

1991 ◽  
Vol 44 (7) ◽  
pp. 919 ◽  
Author(s):  
RD Hart ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Copper Atom ◽  
Phosphorus Atom ◽  
Lewis Base ◽  
The Other ◽  
Asymmetric Unit ◽  
X Ray

The 1 : 1 adducts between the copper(I) halides, CuX , X = Cl , Br, I, and the title ligand, 'triphos', Ph2P(CH2)2P(Ph)(CH2)2PPh2, have been synthesized and characterized by single-crystal X-ray structure determination. The three complexes are isomorphous : monoclinic P21/c, a ≈ 14.5, b ≈ 20.5, c ≈ 24.5 Ǻ, β ≈ 118.5°; the asymmetric unit of each structure is the binuclear [Cu2X2( triphos )2] unit (with one acetonitrile solvate). Residuals were 0.047, 0.049 and 0.065 for 6006, 4832 and 5108 'observed', independent reflections respectively. About each copper atom, the four-coordinate environment comprises a terminal halogen [Cu- Cl,Br,I , 2.305(3), 2.311(2); 2.441(2), 2.443(2); 2.614(2), 2.614(2)Ǻ], two phosphorus atoms (central and distal) from the same ligand , and one distal phosphorus atom from the other ligand.

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 Lead(II) Compounds. XX. Synthesis and Structure of the 1:1 Adduct of Pyridine With Lead(II) Thiocyanate

1996 ◽  
Vol 49 (10) ◽  
pp. 1165 ◽  
Author(s):  
JM Harrowfield ◽  
H Miyamae ◽  
BW Skelton ◽  
AA Soudi ◽  
AH White
Keyword(s):  
Nitrogen Atom ◽  
Single Crystal ◽  
Structure Determination ◽  
Room Temperature ◽  
Lewis Base ◽  
Two Dimensional ◽  
X Ray

The synthesis and room-temperature single-crystal X-ray structure determination are recorded for a 1:1 adduct of lead(II) thiocyanate with pyridine (' py '). [( py ) Pb (SCN)2](∞|∞) is triclinic, Pī , a 10.544(1), b 7.3729(7), c 6.705(2) Ǻ, α 103.91(2), β 95.99(2), γ 100.51(1)°, Z = 2 f.u .; R was 0.041 for 3226 'observed' (I > 3σ(I)) reflections. The structure is a two-dimensional polymer in the be plane with eight-coordinate ( py -N)PbN3S4 linked by the familiar four- membered Pb2S2 and eight-membered Pb2(NCS)2 motifs by way of bridging thiocyanate groups; one of the latter, unusually, has a bifurcating bridging nitrogen atom leading to the introduction of Pb2N2 motifs. The structure of the parent lead(II) thiocyanate is also discussed.

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