Lewis-Base Adducts of Group-1B Metal(I) Compounds. XXIII. Synthesis and Structures of the 'Tris(3,5-Dimethylpyridine)Copper(I) Halides, [(C7H9N)3CuX], X = Cl, Br, I

1986 ◽  
Vol 39 (7) ◽  
pp. 1043 ◽  
Author(s):  
JM Dyason ◽  
LM Engelhardt ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Total Loss ◽  
Lewis Base ◽  
Molecular Symmetry ◽  
X Ray ◽  
Ray Methods

The crystal structures of the title compounds, (C7H9N)3CuX, X = Cl , Br, I [(1), (2), (3)], have been determined by single-crystal X-ray methods at 295 K, being refined to residuals of 0.022, 0.053, 0.047 for 151, 312, 720 independent 'observed' reflections respectively. The three structures containing 3,5-dimethylpyridine have an interesting relationship in symmetry: (1) is rhombohedral , R3m, a 9.050(3)Ǻ, α 110.89(3)°, Z 1; (2) is rhombohedral, R3c, a 10.328(5)Ǻ, α 95.60(4), Z 2; and (3), derived from (2), is monoclinic, Cc, a 13.233(6), b 15.083(7), c 11.491(6)Ǻ, β 98.27(4)°, Z 4. The distances Cu- Cl , Br, I are 2.412(9), 2.51(1), 2.683(3)Ǻ, with Cu-N 2.08(1), 2.02(1), 1.98(2)- 2.15(4)Ǻ respectively. In (1), the symmetry of the molecule, containing pseudo- tetrahedrally coordinated copper, N3CuX, is a full 3 m, with the ligands lying in mirror planes containing the 3 axis; in (2), the ligands rotate about the Cu-N bonds so that the molecular symmetry is 3; and in (3) further distortion of this kind causes total loss of crystallographically imposed symmetry. This descent in symmetry is the converse of that observed in the rhombohedral series [(C6H7N)3CuX] (C6H7N = 3-methylpyridine), and the possible underlying reasons are explored in terms of intra- and inter-molecular X...H interactions.

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.

Influence of aromatic sulfonation on the geometry of [2.2]paracyclophane: crystal structures of one sulfonate, one disulfonic anhydride and five disulfonimides

2001 ◽  
Vol 57 (6) ◽  
pp. 780-790 ◽  
Author(s):  
Dirk J. A. De Ridder ◽  
Kees Goubitz ◽  
Margot Fontijn ◽  
Pavla Čapková ◽  
Eva Dova ◽  
...  
Keyword(s):  
Organic Chemistry ◽  
New York ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structural Changes ◽  
Symmetry Plane ◽  
Academic Press ◽  
Molecular Symmetry ◽  
X Ray Diffraction ◽  
X Ray

The crystal structures of potassium [2.2]paracyclophane-4-sulfonate (1), [2.2]paracyclophane-4,15-disulfonic anhydride (2), [2.2]paracyclophane-4,15-disulfonimide (3), N-n-propyl-[2.2]paracyclophane-4,15-disulfonimide (4), N-isopropyl-[2.2]paracyclophane-4,15-disulfonimide (5), N-cyclopropyl-[2.2]paracyclophane-4,15-disulfonimide (6) and N-phenyl-[2.2]paracyclophane-4,15-disulfonimide (7) were established by single-crystal X-ray diffraction. The structural changes caused by sulfonation are discussed with respect to the parent [2.2]paracyclophane (tricyclo[8.2.2.24,7]hexadeca-4,6,10,12,13,15-hexaene). The main features are a change in the non-bonding distances between the para-phenylene rings and a rotation of these rings with respect to the molecular symmetry plane. The rings are rotated away from each other in the case of monosulfonation (1), but are rotated in the opposite way in the case of the disulfonic anhydride (2) or the disulfonimide compounds (3)–(7). The results are also discussed in terms of the parameters proposed by Keehn [(1983), Organic Chemistry, A Series of Monographs 45, edited by P. H. Keehn & S. M. Rosenfeld, Vol. 1, pp. 69–238. New York: Academic Press] showing that (bonded and non-bonded) angles involving the para-phenylene rings are mainly affected.

Crystal structure refinements of magnesite, calcite, rhodochrosite, siderite, smithonite, and dolomite, with discussion of some aspects of the stereochemistry of calcite type carbonates

1981 ◽  
Vol 156 (3-4) ◽  
Author(s):  
H. Effenberger ◽  
K. Mereiter ◽  
J. Zemann
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
X Ray ◽  
Ray Methods

AbstractThe crystal structures of magnesite, calcite, rhodochrosite, siderite, smithonite and dolomite were refined by standard single crystal X-ray methods using diffraction data up to sin[unk]/

Darstellung und Kristallstrukturen von LiGaCl4 und LiGaI4/ Preparation and Crystal Structure of LiGaCL4 and LiGaI4

1987 ◽  
Vol 42 (2) ◽  
pp. 248-250 ◽  
Author(s):  
Wolfgang Hönle ◽  
Bernhard Hettich ◽  
Arndt Simon
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray ◽  
Common Features ◽  
Bond Lengths ◽  
Ray Methods

Abstract The crystal structures of LiGaCl4 and LiGaI4 have been determined by single crystal X-ray methods. Both compounds are isotypic with LiAlCl4 and characterized by LiX6 octahedra and GaX4 tetrahedra. Mean bond lengths are: d̄(Ga-X) = 217.4 pm (Cl) and 255.9 pm (I); d̄(Li-X) = 263.9 pm (Cl) and 305.3 pm (I), respectively. Common features of the isotypic compounds LiGaX4 (X = Cl, Br. I) are discussed.

Die Kristallstrukturen der Eisen- und Cobalt-Hexacyanokomplexe Rb2LiM(CN)6 und Rb2NaM(CN)6 / The Crystal Structures of the Iron- and Cobalt-Hexacyanocomplexes Rb2LiM(CN)6 and Rb2NaM(CN)6

1996 ◽  
Vol 51 (6) ◽  
pp. 826-831 ◽  
Author(s):  
Stefan Peschel ◽  
Werner Paulus ◽  
Dietrich Babel
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Crystal Structures ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Cyano Complexes ◽  
Related Compounds ◽  
Ray Methods

Abstract The crystal structures of four isotypic cyano complexes, belonging to the monoclinic type of cryolite (P21/n, Z = 2), were determined by single crystal X-ray methods and in one case also by neutron diffraction: Rb2LiFe(CN)6 (a = 717.3, b = 748.0, c = 1030.2 pm, β = 90.24°; Fe - C = 193.6, C - N = 114.5, Li - N = 227.0 pm), Rb,NaFe(CN)6 (a = 724.5, b = 772.5, c = 1055.2 pm, β = 90.39°; Fe - C = 193.9, C - N = 114.2, Na - N = 250.4 pm), Rb,LiCo(CN)6 (a = 715.5, b = 741.2, c = 1025.0 pm, β = 90.14°; Co - C = 189.6, C - N = 114.3, Li - N = 226.9 pm), Rb2NaCo(CN)6 (a = 722.5, b = 766.3, c = 1049.2 pm, β = 90.33°; Co - C = 189.9 (188.8), C - N = 113.4 (7/5.5), Na - N = 250.6 (249.6 pm). The irregular [RbN8l coordination polyhedra exhibit average distances close to Rb - N = 336 pm. Details are discussed and the results compared with those of related compounds

Lewis-Base Adducts of Groups 11 Metal(I) Compounds. LXII. The Crystal Structures of the 1 : 1 Adducts of Copper(I) Chloride, Bromide and Thiocyanate With Quinoline

1991 ◽  
Vol 44 (8) ◽  
pp. 1049 ◽  
Author(s):  
PC Healy ◽  
BW Skelton ◽  
AF Waters ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray ◽  
Structure Determinations ◽  
The Subject ◽  
The Common

Adducts (1 : 1) of copper(I) chloride, bromide and thiocyanate with quinoline have been synthesized and have been the subject of single-crystal X-ray structure determinations at 295 K. Crystals of the chloride are orthorhombic, P 212121, a 15.358(7), b 14.309(6), c 3.801(2)Ǻ, Z 4; R was 0.055 for 541 'observed' reflections. Crystals of the bromide are monoclinic, C2/c, a 19.417(5), b 14.048(4), c 15.753(6) Ǻ, β 125.31(2)°, Z 4 tetramers; R was 0.049 for 1138 'observed' reflections. Crystals of the thiocyanate are monoclinic, P 21/c, a 5.682(1), b 10.412(2), c 16.838(5)Ǻ, β 97.48(2)°, Z 4 f.u .; R was 0.045 for 914 'observed' reflections. The chloride takes the form of the common 'stair' polymer, unexpectedly, while the thiocyanate is an expanded version of the same. The bromide provides a second example of a novel tetrameric 'basket' structure exemplified previously by the iodide analogue.

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 1B Metal(I) Compounds. XXII. Crystal Structure of 'Bis(pyridine)silver(I) Perchlorate

1985 ◽  
Vol 38 (9) ◽  
pp. 1325 ◽  
Author(s):  
JC Dyason ◽  
PC Healy ◽  
LM Engelhardt ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Complex Cation ◽  
Lewis Base ◽  
X Ray ◽  
Ray Methods

Determination of the crystal structure of 'bis (pyridine)silver(I) perchlorate' by single-crystal X-ray methods shows it to be of 2.4:1 pyridine:silver (I) perchlorate stoichiometry , the structure being refined by least squares to a residual of 0.054 for 1142 'observed' reflections. Crystals are tetragonal, I4, a 21.95(1), c 7.684(3) Ǻ. The structure comprises perchlorate anions of two types of I and 4 symmetry, together with two types of complex cation: [Ag( py )2]+, with 1 symmetry, and [Ag( py )4]+ with 4 symmetry. For the two types of cation Ag-N are 2.15(1), 2.16(1) and 2.30(1) 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.

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