Structure determination of di-μ-hydroxo-bis[(2-(2-pyridyl)phenyl-κ²N,C¹)palladium(II)] by X-ray powder diffractometry

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.

Computing details

Program(s) used to solve structure: FOX; program(s) used to refine structure: FULLPROF.

Figures

bis(mu2-hydroxo)-(2-pyridininphenyl)-C,N)palladium

Crystal data

C22H18N2O2Pd2	β = 92.115 (3)°
Mr = 555.2	V = 2833.2 (3) Å^3
Monoclinic, P121/N1	Z = 6
Hall symbol: -P 2yn	Dx = 1.953 Mg m^−3
a = 15.9574 (10) Å	Cu Kα radiation, λ = 1.54183 Å
b = 16.1807 (10) Å	T = 298 K
c = 10.9808 (7) Å	?, ? × ? × ? mm

Data collection

Diffractometer	Scan method: step
Radiation source: sealed X-ray tube	2θmin = 4.975°, 2θmax = 99.975°, 2θstep = 0.020°
C 111 monochromator

Refinement

Rp = 9.545	Profile function: pseudo-Voigt
Rwp = 12.461	76 parameters
Rexp = 6.098	13 restraints
RBragg = 9.837	H-atom parameters constrained
χ^2 = 4.176
4751 data points	Background function: Linear Interpolation

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0.8460 (4)	−0.0628 (5)	0.7950 (5)	0.00000*
O1	0.855 (2)	−0.151 (2)	0.929 (3)	0.00000*
N1	0.7255 (6)	−0.0368 (8)	0.8518 (12)	0.00000*
C1	0.7976 (6)	0.0142 (8)	0.6576 (12)	0.00000*
C7	0.6779 (6)	0.0189 (8)	0.7865 (12)	0.00000*
C11	0.6977 (6)	−0.0663 (8)	0.9581 (12)	0.00000*
H10	0.7311 (6)	−0.1051 (8)	1.0028 (12)	0.00000*
C8	0.6007 (6)	0.0441 (8)	0.8280 (12)	0.00000*
H7	0.5673 (6)	0.0821 (8)	0.7815 (12)	0.00000*
C2	0.8395 (6)	0.0380 (8)	0.5545 (12)	0.00000*
H3	0.8931 (6)	0.0156 (8)	0.5400 (12)	0.00000*
C5	0.6816 (6)	0.1040 (8)	0.5937 (12)	0.00000*
H6	0.6277 (6)	0.1262 (8)	0.6071 (12)	0.00000*
C9	0.5726 (6)	0.0140 (8)	0.9368 (12)	0.00000*
H8	0.5199 (6)	0.0310 (8)	0.9657 (12)	0.00000*
C4	0.7246 (6)	0.1279 (8)	0.4924 (12)	0.00000*
H5	0.7004 (6)	0.1668 (8)	0.4367 (12)	0.00000*
C10	0.6221 (6)	−0.0418 (8)	1.0036 (12)	0.00000*
H9	0.6043 (6)	−0.0627 (8)	1.0793 (12)	0.00000*
C3	0.8032 (6)	0.0946 (8)	0.4724 (12)	0.00000*
H4	0.8325 (6)	0.1105 (8)	0.4024 (12)	0.00000*
C6	0.7175 (6)	0.0474 (8)	0.6760 (12)	0.00000*
Pd2	0.4657 (5)	0.7121 (4)	0.3995 (7)	0.00000*
O2	0.4550 (19)	0.633 (2)	0.253 (3)	0.00000*
N2	0.5588 (8)	0.7887 (7)	0.3325 (13)	0.00000*
C12	0.4760 (8)	0.8039 (7)	0.5303 (13)	0.00000*
C18	0.5771 (8)	0.8602 (7)	0.3937 (13)	0.00000*
C22	0.5945 (8)	0.7737 (7)	0.2251 (13)	0.00000*
H18	0.5815 (8)	0.7238 (7)	0.1832 (13)	0.00000*
C19	0.6331 (8)	0.9167 (7)	0.3469 (13)	0.00000*
H15	0.6465 (8)	0.9659 (7)	0.3905 (13)	0.00000*
C13	0.4304 (8)	0.8076 (7)	0.6355 (13)	0.00000*
H11	0.3934 (8)	0.7638 (7)	0.6539 (13)	0.00000*
C16	0.5394 (8)	0.9363 (7)	0.5851 (13)	0.00000*
H14	0.5769 (8)	0.9800 (7)	0.5679 (13)	0.00000*
C20	0.6693 (8)	0.9012 (7)	0.2369 (13)	0.00000*
H16	0.7076 (8)	0.9396 (7)	0.2043 (13)	0.00000*
C15	0.4927 (8)	0.9395 (7)	0.6887 (13)	0.00000*
H13	0.4977 (8)	0.9855 (7)	0.7421 (13)	0.00000*
C21	0.6493 (8)	0.8287 (7)	0.1743 (13)	0.00000*
H17	0.6730 (8)	0.8173 (7)	0.0979 (13)	0.00000*
C14	0.4386 (8)	0.8750 (7)	0.7143 (13)	0.00000*
H12	0.4070 (8)	0.8768 (7)	0.7858 (13)	0.00000*
C17	0.5315 (8)	0.8691 (7)	0.5062 (13)	0.00000*
Pd3	0.0427 (5)	0.9257 (5)	0.0879 (6)	0.00000*
O3	0.049 (2)	0.981 (2)	−0.090 (3)	0.00000*
N3	0.1379 (9)	0.8409 (7)	0.0635 (12)	0.00000*
C23	0.0291 (9)	0.8451 (7)	0.2331 (12)	0.00000*
C29	0.1523 (9)	0.7820 (7)	0.1507 (12)	0.00000*
C33	0.1916 (9)	0.8486 (7)	−0.0283 (12)	0.00000*
H27	0.1811 (9)	0.8897 (7)	−0.0886 (12)	0.00000*
C30	0.2209 (9)	0.7294 (7)	0.1443 (12)	0.00000*
H24	0.2301 (9)	0.6878 (7)	0.2043 (12)	0.00000*
C24	−0.0319 (9)	0.8502 (7)	0.3199 (12)	0.00000*
H20	−0.0745 (9)	0.8909 (7)	0.3119 (12)	0.00000*
C27	0.0914 (9)	0.7291 (7)	0.3451 (12)	0.00000*
H23	0.1334 (9)	0.6877 (7)	0.3532 (12)	0.00000*
C31	0.2757 (9)	0.7377 (7)	0.0506 (12)	0.00000*
H25	0.3227 (9)	0.7019 (7)	0.0458 (12)	0.00000*
C26	0.0309 (9)	0.7357 (7)	0.4316 (12)	0.00000*
H22	0.0316 (9)	0.6993 (7)	0.4994 (12)	0.00000*
C32	0.2612 (9)	0.7986 (7)	−0.0369 (12)	0.00000*
H26	0.2986 (9)	0.8058 (7)	−0.1015 (12)	0.00000*
C25	−0.0310 (9)	0.7959 (7)	0.4187 (12)	0.00000*
H21	−0.0729 (9)	0.8001 (7)	0.4775 (12)	0.00000*
C28	0.0908 (9)	0.7831 (7)	0.2462 (12)	0.00000*