Structural studies on polynuclear osmium carbonyl hydrides. Part 35. Coordination and scission of alkynes on a tungsten-triosmium framework. Crystal structures of (.eta.5-C5H5)WOs3(CO)10[.mu.3-.eta.2-C2(C6H4CH3)2]H and (.eta.5-C5H5)WOs3(CO)10[.mu.3-.eta.2-C2(CO2C2H5)2]H - species with an alkyne ligand bound to Os3 and WOs2 faces of tetrahedral WOs3 clusters

1988 ◽  
Vol 7 (11) ◽  
pp. 2307-2316 ◽  
Author(s):  
Joon T. Park ◽  
John R. Shapley ◽  
Clifford. Bueno ◽  
Joseph W. Ziller ◽  
Melvyn Rowen. Churchill

1982 ◽  
Vol 21 (9) ◽  
pp. 3295-3303 ◽  
Author(s):  
John R. Shapley ◽  
George M. St. George ◽  
Melvyn Rowen. Churchill ◽  
Frederick J. Hollander




1992 ◽  
Vol 45 (7) ◽  
pp. 1155 ◽  
Author(s):  
GA Bowmaker ◽  
D Camp ◽  
RD Hart ◽  
PC Healy ◽  
BW Skelton ◽  
...  

The 1 : 1 complexes of the substituted triphenylphosphine ligands mesityldiphenylphosphine and dimesitylphenylphosphine with copper(1) chloride, bromide and iodide have been the subject of single-crystal X-ray structure determinations at 295 K. All six complexes crystallize as air-stable dimeric molecules, [(PPh2Mes)CuX]2 and [ (PPhMes2)CUX]2 with each copper atom in a distorted trigonal PCuX2. coordination environment. Crystals of [(PPh2Mes)CuCl]2 (1) are monoclinic, P21/n, a 9.961(3), b 18.687(6), c 11.009(7) Ǻ, β 114.63(4)°; R was 0.049 for 2450 'observed' reflections. [(PPh2Mes)CuBrI2 (2) is monoclinic, P21/n, a 9.939(2), b 18.832(6), c 11.238(6) Ǻ, β 115.36(3)°; R was 0.046 for 1803 'observed' reflections. [(PPh2Mes)CuI]2.4/3 C6H6 (3) is rhornbohedral, R3, a 36.877(8), c 9.047(5) A; R was 0.039 for 2537 'observed' reflections. Crystals of [(PPhMes2)CuCl]2.2MeCN (4) are triclinic, Pi, a 15.783(7), b 9.570(4), c 8.914(4) Ǻ, α 72.43(3), β 76.37(3), γ 74.03(3)°; R was 0.045 for 3341 'observed' reflections. [(PPhMes2)CuBr]2.3C6H6 (5) is monoclinic, C2/c, a 9.694(6), b 30.15(2), c 20.66(2) Ǻ, β 98.00(7)°; R was 0.047 for 2117 'observed' reflections. [(PPhMes2)CuI]2.2MeCN (6) is orthorhombic, PP1nb, a 11.694(8), b 14.77(1), c 29.76(3) Ǻ; R was 0.049 for 3447 'observed' reflections. Cu-P bond lengths are: 2.196(2) A (1); 2.198(3) Ǻ (2); 2.222(5) and 2.226(5) Ǻ (3); 2.202(1) Ǻ (4); 2.197(3) A (5); 2.201(4) and 2.264(5) Ǻ (6). The geometries of the LCuX2 and CuX2Cu units are compared with data reported for other monomeric and dimeric compounds for both phosphorus- and nitrogen-based ligands L.



2006 ◽  
Vol 61 (10-11) ◽  
pp. 588-594 ◽  
Author(s):  
Basavalinganadoddy Thimme Gowda ◽  
Jozef Kožíšek ◽  
Hartmut Fuess

TMPAThe effect of substitutions in the ring and in the side chain on the crystal structure of N- (2,4,6-trimethylphenyl)-methyl/chloro-acetamides of the configuration 2,4,6-(CH3)3C6H2NH-COCH3− yXy (X = CH3 or Cl and y = 0,1, 2) has been studied by determining the crystal structures of N-(2,4,6-trimethylphenyl)-acetamide, 2,4,6-(CH3)3C6H2NH-CO-CH3 (); N-(2,4,6- trimethylphenyl)-2-methylacetamide, 2,4,6-(CH3)3C6H2NH-CO-CH2-CH3 (TMPMA); N-(2,4,6- trimethylphenyl)-2,2-dimethylacetamide, 2,4,6-(CH3)3C6H2NH-CO-CH(CH3)2 (TMPDMA) and N-(2,4,6-trimethylphenyl)-2,2-dichloroacetamide, 2,4,6-(CH3)3C6H2NH-CO-CHCl2 (TMPDCA). The crystallographic system, space group, formula units and lattice constants in Å are: TMPA: monoclinic, Pn, Z = 2, a = 8.142(3), b = 8.469(3), c = 8.223(3), β = 113.61(2)◦; TMPMA: monoclinic, P21/n, Z = 8, a = 9.103(1), b = 15.812(2), c = 16.4787(19), α = 89.974(10)◦, β = 96.951(10)◦, γ =89.967(10)◦; TMPDMA: monoclinic, P21/c, Z = 4, a =4.757(1), b= 24.644(4), c =10.785(2), β = 99.647(17)◦; TMPDCA: triclinic, P¯1, Z = 2, a = 4.652(1), b = 11.006(1), c = 12.369(1), α = 82.521(7)◦, β = 83.09(1)◦, γ = 79.84(1)◦. The results are analyzed along with the structural data of N-phenylacetamide, C6H5NH-CO-CH3; N-(2,4,6-trimethylphenyl)-2-chloroacetamide, 2,4,6-(CH3)3C6H2NH-CO-CH2Cl; N-(2,4,6-trichlorophenyl)-acetamide, 2,4,6-Cl3C6H2NH-COCH3; N-(2,4,6-trichlorophenyl)-2-chloroacetamide, 2,4,6-Cl3C6H2NH-CO-CH2Cl; N-(2,4,6-trichlorophenyl)- 2,2-dichloroacetamide, 2,4,6-Cl3C6H2NH-CO-CHCl2 and N-(2,4,6-trichlorophenyl)- 2,2,2-trichloroacetamide, 2,4,6-Cl3C6H2NH-CO-CCl3. TMPA, TMPMA and TMPDCA have one molecule each in their asymmetric units, while TMPDMA has two molecules in its asymmetric unit. Changes in the mean ring distances are smaller on substitution as the effect has to be transmitted through the peptide linkage. The comparison of the other bond parameters reveal that there are significant changes in them on substitution.



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