Structure determination of di-μ-hydroxo-bis[(2-(2-pyridyl)phenyl-κ² N,C ¹)palladium(II)] by X-ray powder diffractometry

Abstract

The title compound was synthesized in the form of a powder, and was studied by elemental analysis, IR spectroscopy, thermogravimetry and mass spectroscopy. Its crystal structure was then determined by X-ray powder diffractometry, using X-ray diffraction data collected in the reflection Bragg-Brentano geometry. The methodology followed in the present study to resolve the crystal structure consisted of peak indexing, then the use of the Monte-Carlo/parallel tempering search algorithm, and finally Rietveld refinement coupled with difference-Fourier synthesis. We found that the crystals are composed of monoclinic unit cells, with 1.5 molecules in the asymmetric unit and therefore six molecules per unit cell. In addition, we concluded that the complexes adopt a planar conformation, forming trimers created by groups of parallel molecules.

N-Heterocyclic-Carbene Complexes Readily Prepared from Di-μ-hydroxopalladacycles Catalyze the Suzuki Arylation of 9-Bromophenanthrene

“…The formation of I is evident through its IR spectra, characterized by the appearance of a typical −OH stretching absorption at 3433 cm –1 and considerable changes in the carbonyl region due to the absence of the bridging acetate groups. The 1 H NMR spectrum displayed a high-field resonance (−1.60 ppm) characteristic of palladium hydroxo complexes. , Mass spectrometry (HPLC/MS TOF) also contributed to the characterization of the new complex, displaying a fragment assigned to M + .…”

Crystal Packing in Di‐(μ‐OH)‐ortho‐palladated Complexes – A DFT Insight into the Molecular Structure and Solid‐State Interactions

“…The plot output from the Rietveld analysis is shown in Figure 1. The crystal structure of complex 1 has been elucidated previously by some of us by using Cu-K α1,2 radiation; [24] the use of strictly monochromatic radiation improves the structural elucidation and yields more reliable information about the relative positions of molecules in the packing. Molecular structures of complexes 1 and 2 are shown in Figure 2.…”

Pd(II), Pd(III) and Pd(IV) Cyclometallated Compounds with 2-Arylpyridines and Their Derivatives or Analogues: 44 Years (1980–2023) of NMR and Single Crystal X-ray Studies

“…All of these dimers are listed in Table 2, including 27 X-ray structures (for 18 species). SOHDUO 01 [96] SOHDUO 02 [19] SOHDUO 03 [97] all (1A) LUM1 [19] OH KEXXIV [98] KEXXIV 01 [99] both (1B) acetate-O,O CDCl 3 [33,44,45,47,95,[100][101][102][103][104][105][106] XEMQIQ [107] XEMQIQ 01 [108] XEMQIQ 02 [109] XEMQIQ 03 [67] XEMQIQ 04 [19] XEMQIQ 05 [110] all (2) COJBEJ (2) (a) [109] BIO [110] LUM1 [19] 1 /2 3,3-dimethylglutarate CD 2 Cl 2 [58] trifluoroacetate-O,O CDCl 3 , CD 2 Cl 2 [19,24] MAHNUG (2) [19] LUM1 [19] benzoate CDCl 3 , CD 2 Cl 2 [103] 4-nitrobenzoate CDCl 3 , CD 2 Cl 2 [103] succinimidate-N,O CDCl 3 , CD 3 COCD 3 [45,66] XOTVIL (2) [66] trans(N,N) CAT [45] 2,2,3,3tetramethylsuccin imidate…”

“…In some Pd(II) dimers, both 2-arylpyridine* ligands are nearly in the same plane, the wellknown examples being the chloride-and hydroxide-bridged species [Pd(2ppy*)(µ-Cl)] 2 (X-ray structures SOHDUO, SOHDUO 01, SOHDUO 02, SOHDUO 03 [19,[95][96][97]) and [Pd(2ppy*)(µ-OH)] 2 (X-ray structures KEXXIV, KEXXIV 01 [98,99]). In many others, both 2-arylpyridine* ligands lie in two distinct planes which are, however, nearly parallel, as exemplified by the acetate-bridged species [Pd(2ppy*)(µ-acetate-O,O)] 2 (X-ray structures XEMQIQ, XEMQIQ 01, XEMQIQ 02, XEMQIQ 03, XEMQIQ 04, XEMQIQ 305 [19,67,[107][108][109][110]) and [Pd(7,8benzoquinoline*)(µ-acetate-O,O)] 2 (X-ray structure YULCUE [45,102,103,148,169]).…”