Lewis-base adducts of Group 1B metal(I) compounds. VII. Synthesis and structures of the 1 : 1 adducts of copper(I) halides with N,N,N',N'-tetramethyletlrylenediamine

1984 ◽  
Vol 37 (11) ◽  
pp. 2207 ◽  
Author(s):  
LM Engelhardt ◽  
RI Papasergio ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
X Ray

1 : 1 adducts of N,N,N',N'-tetramethylethylenediamine ('tmeda') with copper(1) chloride, bromide and iodide have been synthesized and the structures of the solid iodide and chloride derivatives established by single-crystal X-ray diffraction methods. The iodide,(1),is monoclinic, P21/c, a 12.370(5), b 12.119(5), c 15.36(1) �, β 109.16(5)�, Z = 4 dimers; the residual R was 0.067 for 1240 'observed' reflections. The complex is a ��'-diiodobridged dimer (tmeda)CuI2Cu(tmeda); thedistance between the pair of four-coordinate copper atoms is very short [2.566(4) A]. The bromide is isomorphous with the iodide. The chloride, (2), is monoclinic, P21/n, a 14.477(3), b 15.063(3),c 9.326(2) �, β 96.99(2)�, Z = 4 formula units; R was 0.055 for No = 1195. The complex is ionic [Cu(tmeda)2]+ [CuCl2]-.

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIX. Crystal Structure Determinations of Tetrakis(trimethylphosphine)copper(I) Halides and Tetrakis(triphenylphosphine)-copper(I) and -silver(I) Hexafluorophosphates

1990 ◽  
Vol 43 (10) ◽  
pp. 1697 ◽  
Author(s):  
GA Bowmaker ◽  
PC Healy ◽  
LM Engelhardt ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths ◽  
Cu Complex ◽  
Structure Determinations

The crystal structures of [Cu(Pme3)4]X (X = Cl , Br, I) and of [M(PPh3)4] [PF6] (M = Cu, Ag) have been determined by single-crystal X-ray diffraction methods at 295 K. The former compounds contain nearly tetrahedral [Cu(PMe3)4]+ ions on sites of m symmetry with mean Cu-P bond lengths of 2.270, 2.271 and 2.278 Ǻ for X = Cl , Br and I respectively. The latter compounds contain [M(PPh3)4]+ ions on sites of 3 symmetry. In the M =Ag complex the coordination environment is close to tetrahedral, but in the M =Cu complex the length of the axial Cu-P bond [2.465(2)Ǻ] is significantly shorter than that of the off-axis bonds [2.566(2)Ǻ]. Possible reasons for this are discussed.

Lewis-base adducts of Group 1B metal(I) compounds. VI. Crystal structure of the 1 : 2 adduct of copper(I) iodide with pyridine

1984 ◽  
Vol 37 (11) ◽  
pp. 2201 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
PC Healy ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
X Ray

Copper(I) iodide on recrystallization from neat pyridine yields a 1 : 2 adduct; it is established by single-crystal X-ray diffraction methods at 295 K that this is a ��'-diiodobridged dimer, with four- coordinate copper(I), [(py)2CuI2Cu(py)2]. Crystals are orthorhombic, C2221, a 14.578(4), b 10.448(3), c 31.559(7) �, Z = 8 dimers. Cu. . .Cu is 2.699(5) �.

Lewis-Base Adducts of Group 11 Metal(I) Compounds .XLV. Conformational Systematics of [(N-base)1(AgX)1]N Complexes

1989 ◽  
Vol 42 (1) ◽  
pp. 149 ◽  
Author(s):  
LM Engelhardt ◽  
S Gotsis ◽  
PC Healy ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Metal Atom ◽  
Lewis Base ◽  
The Novel ◽  
X Ray Diffraction ◽  
Nitrogen Base ◽  
X Ray ◽  
Structural Types ◽  
Solid State Structures

A number of 1 : 1 silver(1) halide/nitrogen base adducts, [ LAgX ], have been synthesized by recrystallization of the parent silver(I) halide from the neat base, and their solid state structures determined by single-crystal X-ray diffraction and rationalized in terms of the hierarchy of structural types described in the preceding papers based on steric profile of the base. In consequence of increased metal atom size (cf. Cu), a more limited array of structural types is observed.[(pyridine) AgBr,I ] ∞, [(2,4,6-trimethylpyridine) AgCI,Br,I ] ∞ and [( quinaldine ) AgCI,Br ] are 'stair' polymers; [( piperidine ) AgBr,I ]4 and [(2,2,6,6-tetramethyIpiperidine) AgI ]4 are 'cube' tetramers, while [( diethylamine ) AgCI,Br,I ] provide the first complete metal halide series of the novel 'tube' polymer.

Lewis-Base Adducts of Group-11 Metal(I) Compounds. XXXI. Reaction of 2,6-Bis[1-phenyl-1-(pyridin-2-Yl)ethyl]pyridine (L), and Copper(I) Halides in Acetonitrile: Structural Characterization of Salts of the [(MeCN)Cu(meso-L)]+ Cation

1987 ◽  
Vol 40 (11) ◽  
pp. 1881 ◽  
Author(s):  
AJ Canty ◽  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
NJ Minchin ◽  
...  
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Lewis Base ◽  
Tridentate Ligand ◽  
Acetonitrile Solution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ligand Conformation

Reaction of 2,6-bis[l-phenyl-1-(pyridin-2-yl)ethyl]pyridine, L, with copper(1) chloride, bromide, and iodide in acetonitrile solution has been shown to yield salts, structurally characterized by single-crystal X-ray diffraction methods as [( MeCN ) CuL ]+ [ ClCuCl ]-, (1), [( MeCN ) CuL ]+2 [XCuX2CuX]2-, X = Br (2), I (3) (both isomorphous ), all as yellow needles, and a form of (3), orange blocks, as the hemiacetonitrile solvate, (4), [( MeCN ) CuL ]+2 [IcuI2Cul]2-. MeCN . The same cation is common to all four species, containing four-coordinate copper(r), with L as meso -tridentate ligand; in (4), the most precisely defined example, Cu-N( MeCN ) is 1.919(5) �, the shortest copper(1) acetonitrile distance known, while Cu-N(L) are 2.065(5)-2.073(5) �. The reason for non-formation of species of the type [ LCuX ] appears to lie in the tridentate ligand conformation which permits coordination of acetonitrile but not larger halide species.

Synthesis and structures of isopropyl-β-diketiminato copper(I) complexes

2010 ◽  
Vol 88 (5) ◽  
pp. 472-477 ◽  
Author(s):  
Paul O. Oguadinma ◽  
Frank Schaper
Keyword(s):  
Single Crystal ◽  
Copper Complexes ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
X Ray ◽  
Deuterated Benzene

The reaction of N,N′-diisopropyl-2-amino-4-iminopent-2-ene (nacnaci-PrH, 1) either with CuOt-Bu or with a mixture of mesityl copper and 10% CuOt-Bu afforded, in the presence of PPh3, CN(C6Me2H3), or MeCN, the Lewis base coordinated complexes nacnaci-PrCuPPh3·0.5 C6H14 (2), nacnaci-PrCuCN(C6Me2H3) (3), and nacnaci-PrCu(NCMe) (4). Compounds 2, 3, and 4 were characterized by single-crystal X-ray diffraction studies. Compound 4 afforded two species in deuterated benzene in a 2:1 ratio, which were assigned to {nacnaci-PrCu}2(μ-NCMe) and nacnaci-PrCuNCMe (4). Upon addition of 5 equiv. of MeCN, the two sets collapsed into that of 4. No copper complexes were formed in the presence of styrene, stilbene, or diphenylacetylene.

Lewis-base adducts of Group 1 metal(I) compounds. III. Synthesis and crystal structures of the 1 : 1 adducts of silver(I) iodide with triethylamine, 2- and 3-methylpyridine and quinoline

1983 ◽  
Vol 36 (9) ◽  
pp. 1851 ◽  
Author(s):  
PC Healy ◽  
NK Mills ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Unit Cell ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
X Ray ◽  
Group 1

The crystal structures of the title compounds have been determined at 295(1) K by single-crystal X-ray diffraction methods. For [AgI(Et3N)] (1), the unit cell is tetragonal, P42/nmc, a 13.202(6),c 11.654(8) �; the structure was refined to a residual of 0.077 for 589 independent 'observed' reflections, and is isostructural with the 'pseudo-cubane' triethylphosphine and triethylarsineanalogues with two tetrameric units in the cell. For [AgI(2-MeC5H4N)] (2), the cell is orthorhombic,P212121, a 16.63(1), b 10.797(9), c 4.570(4) �, Z 4; a residual of 0.030 was obtained for 770 independent 'observed' reflections. For [AgI(3-MeC5H4N)] (3), the cell is monoclinic, P21/n, a 19.57(2), b 4.633(3), c 9.355(7) �, β 90.85(7)�, Z 4, a residual of 0.038 being obtained for 1382 independent 'observed' reflections. For [AgI(C9H7N)](4), the unit cell is monoclinic, P21/n, a 12.964(9), b 16.84(2), c 4.454(4) �, β 97.10(7)�, Z 4, a residual of 0.040 being obtained for 660 'observed' independent reflections. For compounds (2)-(4), the observed structures are all 'stairpolymers'; the structures of (2) and (3) are quite similar, but that of (4) exhibits significant differences.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LII. Synthesis and Structural Characterization of Mononuclear Chloro- and Bromo-pyridinebis-(triphenylphosphine)silver(I) Complexes

1989 ◽  
Vol 42 (6) ◽  
pp. 907 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Silver Atom ◽  
Lewis Base ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Weak Coordination

The mononuclear adducts chloro - and bromo-pyridinebis (triphenylphosphine)silver have been synthesized and structurally characterized by single-crystal X-ray diffraction methods. The two complexes are isomorphous, monoclinic, space group P21 or P21/m, a ≈ 9.8, b ≈ 20.0, c ≈ 9.1 � , β ≈ 97.5�, Z 2; in space group P21/m, they were refined to residuals of 0.038, 0.036 for 2392, 2157 'observed' reflections respectively. No comparable iodide adduct has been isolated. In both structures the silver atom is four-coordinate; Ag-Cl,Br are 2.511(2), 2.629(1) �; Ag-P, 2.472(1), 2.476(1) �, and Ag-N, 2.585(5), 2.570(5) � respectively, the Ag-N distance being longer than Ag-P, indicating very weak coordination of the pyridine.

Lewis-Base Adducts of Group-11 Metal(I) Compounds. XXIX. Crystal Structures of Bis(Pyridine-4-carbonitrile)silver(I) Nitrate and Bis(4-benzoylpyridine)Silver(I) Nitrate Monohydrate

1987 ◽  
Vol 40 (9) ◽  
pp. 1603 ◽  
Author(s):  
S Gotsis ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Silver Atoms ◽  
Close Contacts

The crystal structures of the title compounds, [Ag(C6H4N2),] (NO3), (I), and [Ag(C12H9NO)2] (NO3).H2O, (2), have been determined by single-crystal X-ray diffraction methods at ~295 K, being refined by full-matrix least-squares methods to residuals of 0.042 and 0.044 for 1814 and 3434 independent 'observed' reflections respectively. Crystals of (1) and (2) are triclinic P1; for (1) a, 27.954(7), b 6.354(2), c 3.710(1)�, α 87.55(3), β 86.21(2), γ 89.35(2)�, Z 2; for (2), a 17.036(5), b 8.691(3), c 7.849(3) �, α � 107.74(2), β 97 53(2), γ 91 .11(2)�, Z 2. In both structures the formulation is basically a linearly coordinated complex cation/anion as shown above: in (I), Ag-N are 2.214(4), 2.203(4) � with N-Ag-N, 162.2(2)"; in (2), Ag-N are 2.146(3), 2.147(3) �, N-Ag-N, 175.3(1)�. The shortest Ag-O contact is found in (1) at 2.693(4)�. No close contacts are found between the silver atoms and cyano or ketonic ligand substituents.

Electron Microscopy of Shock Loaded Polycrystalline Beryllium

1974 ◽  
Vol 32 ◽  
pp. 506-507 ◽  
Author(s):  
J. M. Galbraith ◽  
L. E. Murr ◽  
A. L. Stevens
Keyword(s):  
Electron Microscopy ◽  
Wave Propagation ◽  
Structural Change ◽  
Single Crystal ◽  
Diffraction Pattern ◽  
Shock Loading ◽  
Slip Systems ◽  
Compression Tests ◽  
X Ray Diffraction ◽  
X Ray

Uniaxial compression tests and hydrostatic tests at pressures up to 27 kbars have been performed to determine operating slip systems in single crystal and polycrystal1ine beryllium. A recent study has been made of wave propagation in single crystal beryllium by shock loading to selectively activate various slip systems, and this has been followed by a study of wave propagation and spallation in textured, polycrystal1ine beryllium. An alteration in the X-ray diffraction pattern has been noted after shock loading, but this alteration has not yet been correlated with any structural change occurring during shock loading of polycrystal1ine beryllium.This study is being conducted in an effort to characterize the effects of shock loading on textured, polycrystal1ine beryllium. Samples were fabricated from a billet of Kawecki-Berylco hot pressed HP-10 beryllium.

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