PDF《data reports》

Crystal structure of [N,N0

0 0 -bis(4-methyl- phenyl)-1,2-diphenylethane-1,2-diimine- j2 N,N0

0 0 ]dichloridopalladium(II) methanol monosolvate Alfredo Pen ?aloza,a Frank R.

Fronczekb and Ralph Isovitscha * a

13406 Philadelphia Street, Whittier College, Department of Chemistry, Whittier College, Whittier, CA 90601, USA, and b Department of Chemistry, Louisiana State University, Baton Rouge, LA 70803, USA. *Correspondence e-mail: risovitsch@whittier.edu Received

28 July 2015;

accepted

7 August

2015 Edited by M. Weil, Vienna University of Technology, Austria The title compound, [PdCl2(C28H24N2)]?CH3OH, was pre- pared from the reaction of PdCl2(DMSO)2 (DMSO is dimethyl sulfoxide) and N,N0 -bis(4-methylphenyl)-1,2-diphenylethane- 1,2-diimine in methanol. The chelating diimine core of the title compound deviates slightly from planarity, with an N―C― C―N torsion angle of 5.3 (3) . Delocalization in the diimine core is indicated by N―C and C―C bonds that are, respectively, longer and shorter than those found in related nonchelating diimines. The distorted square-planar coordina- tion environment around the PdII atom is manifested as bond angles that are smaller and larger than

90 , and palladacycle torsion angles of ?173.22 (16) and 167.06 (16) . These deviations are attributed to the small bite angle of 79.13 (8) of the diimine chelate. The crystal packing exhibits weak intermolecular hydrogen-bonding interactions involving aromatic H atoms, Cl atoms and intercalated methanol solvent molecules, de?ning layers parallel to (010). Keywords: crystal structure;

palladium(II) dichlorido diimine complex;

polymerization catalyst. CCDC reference:

1417572 1. Related literature Palladium(II) diimiine complexes have been widely used as polymerization catalysts for -ole?ns (Johnson et al., 1995;

Popeney &

Guan, 2005) and are prepared easily by the reac- tion of PdCl2(DMSO)2 with the diimine of choice (Kubota et al., 2013;

Ettedgui &

Neumann, 2009;

Price et al., 1972). For structural information about related palladium(II) diimine complexes, see: Kubota et al. (2013);

Comerlato et al. (2001);

Dyakonenko et al. (2015). For structures of other diimines, see: Wang et al. (2012);

Zhao et al. (2015). 2. Experimental 2.1. Crystal data [PdCl2(C28H24N2)]?CH4O Mr = 597.83 Triclinic, P1 a = 8.8213 (3) A ? b = 12.3364 (3) A ? c = 12.7697 (4) A ? = 108.992 (2) = 93.900 (3) = 92.457 (3) V = 1307.83 (7) A ?

3 Z =

2 Mo K radiation = 0.94 mm?1 T =

90 K 0.18 ? 0.10 ? 0.06 mm 2.2. Data collection Bruker Kappa APEXII DUO CCD diffractometer Absorption correction: multi-scan (SADABS;

Bruker, 2014) Tmin = 0.831, Tmax = 0.946

12258 measured re?ections

5965 independent re?ections

5026 re?ections with I >

2(I) Rint = 0.032 2.3. Refinement R[F2 >

2(F2 )] = 0.031 wR(F2 ) = 0.066 S = 1.02

5965 re?ections

322 parameters

1 restraint H atoms treated by a mixture of independent and constrained re?nement ?max = 0.57 e A ? ?3 ?min = ?0.64 e A ? ?3 Table

1 Hydrogen-bond geometry (A ? , ). D―H? ? ?A D―H H? ? ?A D? ? ?A D―H? ? ?A O1―H10H? ? ?Cl2 0.83 (2) 2.36 (2) 3.161 (2)

163 (3) C17―H17? ? ?Cl2i 0.95 2.80 3.708 (3)

161 C21―H21? ? ?O1ii 0.95 2.48 3.275 (3)

141 Symmetry codes: (i) ?x ? 1;

?y ? 1;

?z ? 1;

(ii) ?x ? 2;

?y ? 1;

?z ? 1. Data collection: APEX2 (Bruker, 2014);

cell re?nement: SAINT (Bruker, 2014);

data reduction: SAINT;

program(s) used to solve structure: SHELXS97 (Sheldrick, 2008);

program(s) used to re?ne structure: SHELXL97 (Sheldrick, 2008);