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Acta Crystallogr Sect E Struct Rep Online. 2009 October 1; 65(Pt 10): m1166.
Published online 2009 September 5. doi:  10.1107/S1600536809035272
PMCID: PMC2970311

Dichlorido(4,5-diaza­fluoren-9-one-κ2 N,N′)palladium(II)

Abstract

The structure of the title compound, [PdCl2(C11H6N2O)], shows a nearly square-planar geometry for the PdII atom within a Cl2N2 donor set.

Related literature

For related palladium complexes, see: Klein et al. (1998 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-m1166-scheme1.jpg

Experimental

Crystal data

  • [PdCl2(C11H6N2O)]
  • M r = 359.48
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1166-efi1.jpg
  • a = 5.131 (5) Å
  • b = 17.105 (5) Å
  • c = 12.763 (5) Å
  • β = 99.183 (5)°
  • V = 1105.8 (12) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 2.14 mm−1
  • T = 293 K
  • 0.35 × 0.33 × 0.25 mm

Data collection

  • Bruker SMART APEXII diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2005 [triangle]) T min = 0.477, T max = 0.586
  • 6785 measured reflections
  • 2703 independent reflections
  • 2198 reflections with I > 2σ(I)
  • R int = 0.028

Refinement

  • R[F 2 > 2σ(F 2)] = 0.029
  • wR(F 2) = 0.058
  • S = 1.04
  • 2703 reflections
  • 178 parameters
  • All H-atom parameters refined
  • Δρmax = 0.37 e Å−3
  • Δρmin = −0.54 e Å−3

Data collection: APEX2 (Bruker, 2005 [triangle]); cell refinement: SAINT (Bruker, 2005 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 [triangle]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 [triangle]).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809035272/tk2532sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809035272/tk2532Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Natural Science Foundation of Guangdong Province (No. 8451063101000730). The authors thank Professor Zhong Min Su and Dr Kui Zhan Shao (Northeast Normal University) for their assistance with the X-ray crystallographic analysis.

supplementary crystallographic information

Comment

The title compound, (I), Fig. 1, shows the palladium atom to be coordinated by two chlorides and two nitrogen atoms, the latter derived from a chelating 4,5-diazafluoren-9-one (dafo) ligand. The coordination geometry is based on a square planar arrangement of the four donor atoms. Related palladium structures featuring dafo ligands are known (Klein et al., 1998).

Experimental

Compound (I) was synthesized hydrothermally from an aqueous mixture (10.0 ml) containing PdCl2 (0.1758 g) and 4,5-diazafluoren-9-one (0.301 g) in a 30 ml Teflon-lined stainless steel vessel. In the vessel, the solution was heated to 413 K for 72 h then cooled to room temperature at a rate of 10 K per hour. Brown prisms were obtained after washed thoroughly with deionized water and air-drying.

Refinement

All H atoms were refined: range of C-H = 0.89 (3) to 0.99 (4) Å.

Figures

Fig. 1.
Molecular structure of (I) with displacement ellipsoids drawn at the 50% probability level.

Crystal data

[PdCl2(C11H6N2O)]F(000) = 696
Mr = 359.48Dx = 2.159 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 13853 reflections
a = 5.131 (5) Åθ = 1.8–28.2°
b = 17.105 (5) ŵ = 2.14 mm1
c = 12.763 (5) ÅT = 293 K
β = 99.183 (5)°Block, yellow
V = 1105.8 (12) Å30.35 × 0.33 × 0.25 mm
Z = 4

Data collection

Bruker SMART APEXII CCD area-detector diffractometer2703 independent reflections
Radiation source: fine-focus sealed tube2198 reflections with I > 2σ(I)
graphiteRint = 0.028
Detector resolution: 10 pixels mm-1θmax = 28.4°, θmin = 2.0°
ω scansh = −6→6
Absorption correction: multi-scan (SADABS; Bruker, 2005)k = −22→13
Tmin = 0.477, Tmax = 0.586l = −16→16
6785 measured reflections

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058All H-atom parameters refined
S = 1.04w = 1/[σ2(Fo2) + (0.0199P)2 + 0.6053P] where P = (Fo2 + 2Fc2)/3
2703 reflections(Δ/σ)max < 0.001
178 parametersΔρmax = 0.37 e Å3
0 restraintsΔρmin = −0.54 e Å3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating Rfactors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Pd10.08571 (4)0.152850 (13)0.283179 (18)0.03075 (8)
N20.2819 (5)0.16090 (14)0.15176 (19)0.0336 (6)
N10.2865 (4)0.04745 (13)0.30833 (19)0.0303 (5)
C60.6231 (5)0.08217 (18)0.0892 (2)0.0343 (7)
C40.6221 (6)−0.01682 (17)0.2253 (2)0.0322 (6)
C50.7568 (6)0.00609 (19)0.1320 (2)0.0378 (7)
O10.9357 (5)−0.02803 (14)0.10159 (19)0.0532 (6)
C110.4449 (5)0.04170 (17)0.2364 (2)0.0319 (6)
C100.4439 (5)0.10020 (17)0.1557 (2)0.0317 (6)
C30.6398 (6)−0.0784 (2)0.2962 (3)0.0402 (8)
C80.4677 (7)0.1976 (2)−0.0016 (3)0.0434 (8)
C10.3028 (6)−0.01242 (19)0.3780 (3)0.0367 (7)
C90.2942 (6)0.2103 (2)0.0695 (3)0.0397 (7)
C70.6379 (7)0.1337 (2)0.0064 (3)0.0414 (8)
C20.4742 (6)−0.0747 (2)0.3724 (3)0.0413 (8)
Cl1−0.10542 (16)0.13410 (5)0.42956 (7)0.0445 (2)
Cl2−0.11747 (16)0.26981 (5)0.24949 (7)0.0479 (2)
H10.187 (6)−0.0098 (17)0.429 (2)0.038 (9)*
H30.762 (7)−0.123 (2)0.295 (3)0.052 (10)*
H40.753 (6)0.1289 (19)−0.038 (3)0.048 (10)*
H20.477 (6)−0.115 (2)0.420 (3)0.046 (9)*
H50.465 (6)0.2338 (19)−0.055 (3)0.043 (9)*
H60.181 (6)0.2543 (19)0.064 (2)0.046 (9)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pd10.02879 (12)0.02863 (13)0.03619 (14)−0.00123 (9)0.00940 (9)−0.00117 (10)
N20.0321 (13)0.0332 (14)0.0364 (14)−0.0019 (11)0.0084 (10)0.0016 (11)
N10.0293 (12)0.0303 (13)0.0328 (14)−0.0010 (10)0.0097 (10)0.0015 (10)
C60.0300 (15)0.0392 (18)0.0341 (17)−0.0042 (13)0.0070 (12)−0.0008 (13)
C40.0306 (15)0.0341 (16)0.0330 (17)−0.0017 (12)0.0086 (12)−0.0034 (13)
C50.0351 (16)0.0419 (18)0.0373 (18)−0.0013 (14)0.0093 (14)−0.0042 (14)
O10.0540 (14)0.0596 (16)0.0516 (15)0.0154 (12)0.0258 (12)0.0029 (12)
C110.0281 (15)0.0337 (16)0.0340 (17)−0.0032 (12)0.0056 (12)−0.0019 (12)
C100.0279 (14)0.0343 (17)0.0329 (16)−0.0027 (12)0.0049 (12)0.0010 (13)
C30.0390 (18)0.0366 (18)0.046 (2)0.0071 (14)0.0092 (15)0.0012 (15)
C80.051 (2)0.045 (2)0.0340 (19)−0.0075 (16)0.0075 (15)0.0118 (15)
C10.0366 (17)0.0387 (18)0.0366 (18)−0.0027 (14)0.0112 (14)0.0016 (14)
C90.0401 (18)0.0362 (18)0.043 (2)0.0004 (15)0.0070 (14)0.0079 (14)
C70.0427 (19)0.049 (2)0.0345 (19)−0.0075 (15)0.0114 (15)−0.0019 (15)
C20.0461 (19)0.0348 (18)0.044 (2)0.0026 (15)0.0122 (15)0.0084 (15)
Cl10.0490 (5)0.0435 (5)0.0461 (5)−0.0033 (4)0.0235 (4)−0.0035 (4)
Cl20.0470 (5)0.0334 (4)0.0651 (6)0.0065 (4)0.0147 (4)0.0033 (4)

Geometric parameters (Å, °)

Pd1—N12.076 (2)C4—C51.521 (4)
Pd1—N22.094 (3)C5—O11.203 (4)
Pd1—Cl22.2652 (11)C11—C101.436 (4)
Pd1—Cl12.2672 (12)C3—C21.391 (5)
N2—C101.326 (4)C8—C91.387 (5)
N2—C91.356 (4)C8—C71.392 (5)
N1—C111.323 (4)C1—C21.390 (5)
N1—C11.350 (4)H3—C30.99 (4)
C6—C101.382 (4)H1—C10.95 (3)
C6—C71.387 (4)H2—C20.92 (4)
C6—C51.531 (4)H5—C80.92 (4)
C4—C111.375 (4)H6—C90.95 (3)
C4—C31.382 (4)H4—C70.89 (3)
N1—Pd1—N283.74 (10)C4—C11—C10111.1 (3)
N1—Pd1—Cl2176.78 (7)N2—C10—C6128.8 (3)
N2—Pd1—Cl293.17 (8)N2—C10—C11120.2 (3)
N1—Pd1—Cl191.09 (7)C6—C10—C11111.0 (3)
N2—Pd1—Cl1174.80 (7)C4—C3—C2116.1 (3)
Cl2—Pd1—Cl192.00 (4)C9—C8—C7122.3 (3)
C10—N2—C9114.2 (3)N1—C1—C2121.3 (3)
C10—N2—Pd1107.26 (19)N2—C9—C8121.6 (3)
C9—N2—Pd1138.5 (2)C6—C7—C8116.4 (3)
C11—N1—C1114.8 (3)C1—C2—C3122.2 (3)
C11—N1—Pd1107.58 (19)C7—C8—H5121.(2)
C1—N1—Pd1137.5 (2)C9—C8—H5116.(2)
C10—C6—C7116.7 (3)N1—C1—H1115.8 (18)
C10—C6—C5106.0 (3)C2—C1—H1122.8 (18)
C7—C6—C5137.4 (3)C1—C2—H2119.(2)
C11—C4—C3117.6 (3)C3—C2—H2119.(2)
C11—C4—C5106.5 (3)N2—C9—H6116.7 (17)
C3—C4—C5135.9 (3)C8—C9—H6121.8 (17)
O1—C5—C4126.4 (3)C4—C3—H3124.(2)
O1—C5—C6128.2 (3)C2—C3—H3120.(2)
C4—C5—C6105.3 (2)C6—C7—H4124.(2)
N1—C11—C4128.0 (3)C8—C7—H4120.(2)
N1—C11—C10120.9 (3)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2532).

References

  • Bruker (2005). APEX2, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Farrugia, L. J. (1997). J. Appl. Cryst.30, 565.
  • Klein, R. A., Witte, P., van Belzen, R., Fraanje, J., Goubitz, K., Numan, M., Schenk, H., Ernsting, J. M. & Elsevier, C. J. (1998). Eur. J. Inorg. Chem. pp. 319–330.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography