Home The crystal structure of trans-dichlorido-bis(pyridine-2-carboxylato-κ2N,O)platinum(IV), C12H8Cl2N2O4Pt
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The crystal structure of trans-dichlorido-bis(pyridine-2-carboxylato-κ2N,O)platinum(IV), C12H8Cl2N2O4Pt

  • Kwang Ha EMAIL logo
Published/Copyright: November 9, 2018

Abstract

C12H8Cl2N2O4Pt, triclinic, P1̄ (no. 2), a = 6.6940(3) Å, b = 9.5552(6) Å, c = 10.7954(6) Å, α = 83.8311(19)°, β = 88.1577(16)°, γ = 86.8053(17)°, V = 685.20(7) Å3, Z = 2, Rgt(F) = 0.0244, wRref(F2) = 0.0601, T = 223(2) K.

CCDC no.: 1875408

Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Yellow block
Size:0.18 × 0.14 × 0.08 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:10.6 mm−1
Diffractometer, scan mode:PHOTON 100 CMOS, φ and ω
θmax, completeness:26.1°, >99%
N(hkl)measured, N(hkl)unique, Rint:23783, 2719, 0.077
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2058
N(param)refined:193
Programs:Bruker [1], SHELX [2], ORTEP-3 [3], PLATON [4]
Table 2:

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

AtomxyzUiso*/Ueq
Pt10.00000.00001.00000.01617(9)
Cl10.1692(2)−0.21830(16)1.02341(15)0.0288(3)
O1−0.1672(5)−0.0657(4)0.8690(4)0.0230(9)
O2−0.1734(6)−0.0815(5)0.6653(4)0.0330(11)
N10.1773(6)0.0537(5)0.8518(4)0.0192(10)
C10.3514(8)0.1175(6)0.8537(6)0.0246(13)
H10.39610.14370.92920.029*
C20.4650(9)0.1447(7)0.7453(6)0.0270(13)
H20.58470.19150.74640.032*
C30.4009(8)0.1026(6)0.6359(6)0.0274(14)
H30.47980.11690.56250.033*
C40.2202(8)0.0390(6)0.6340(5)0.0231(13)
H40.17330.01210.55930.028*
C50.1105(8)0.0160(6)0.7440(5)0.0190(12)
C6−0.0886(8)−0.0483(6)0.7549(5)0.0200(12)
Pt20.00000.50000.50000.01607(9)
Cl20.1491(2)0.71383(16)0.47479(14)0.0274(3)
O3−0.1810(5)0.5627(4)0.3587(4)0.0232(9)
O4−0.2068(6)0.5573(5)0.1543(4)0.0304(10)
N20.1775(6)0.4368(5)0.3608(4)0.0191(10)
C70.3650(8)0.3805(6)0.3742(6)0.0236(13)
H70.42200.36670.45330.028*
C80.4731(9)0.3431(6)0.2708(6)0.0272(14)
H80.60350.30230.27970.033*
C90.3901(9)0.3656(7)0.1540(6)0.0322(15)
H90.46340.34100.08310.039*
C100.1973(9)0.4249(6)0.1438(6)0.0265(14)
H100.13750.44080.06560.032*
C110.0950(8)0.4599(6)0.2483(5)0.0203(12)
C12−0.1119(8)0.5309(6)0.2481(6)0.0232(13)

Source of material

A suspension of K2PtCl6 (0.251 g, 0.517 mmol) and pyridine-2-carboxylic acid (0.268 g, 2.179 mmol) in H2O (20 mL) was refluxed for 6 h, and the mixture was stirred for 12 h at room temperature. The formed precipitate was separated by filtration and washed with water and EtOH, and dried at 50 °C, to give a pale yellow powder (0.183 g). Yellow crystals were obtained by slow evaporation from a CH3CN/N,N-dimethylformamide solution at 60 °C.

Experimental details

Hydrogen atoms were positioned geometrically and allowed to ride on their parent atoms with d(C—H) = 0.94 Å and Uiso(H) = 1.2Ueq(C) with the help of the SHELXL program (AFIX 43 option) [2]. The highest peak (1.49 e Å−3) and the deepest hole (−1.01 e Å−3) in the difference Fourier map are located 0.94 Å and 0.90 Å from the atoms Pt2 and Pt1, respectively.

Comment

This contribution is part of my continuing interest in the structural chemistry of platinum complexes containing pyridine-2-carboxylate (pic) ligand [5], [6], [7], [8]. The crystal structure of the related complex cis-[PtCl2(pic)2]⋅CH3CN was previously determined in the monoclinic space group P21/c [5].

The asymmetric unit contains two crystallographically independent half-molecules of the title complex trans-[PtCl2(pic)2]; an inversion center is located at the centroid of each complex. The two complexes are chemically identical, but slightly different in geometry. The Pt4+ ion in each complex is six-coordinated in a distorted octahedral environment by two N atoms and two O atoms from two pic anionic ligands and two Cl anions. The Cl, N and O atoms are disposed in the trans position, respectively. The main contributions to the distortion are the tight O—Pt—N chelate angles (¡N1—Pt1—O1 = 81.81(17)° and ¡N2—Pt2—O3 = 81.78(17)°). The Pt—N and Pt—O bond lengths in two complexes are almost equal (Pt—N: 2.000(5) and 2.009(4) Å; Pt—O 2.004(4) and 1.999(4) Å). Each complex displays weak, non-classical intermolecular C—H⋯O hydrogen bonding with d(C⋯O) = 3.236(7) and 3.203(7) Å, respectively, thereby forming chains running along [001]. The complexes are stacked in columns along [010]. In the columns, weak intermolecular π-π interactions are present [4].

Acknowledgements

This study was financially supported by Chonnam National University (Grant number: 2017−2777). The author thanks the KBSI, Seoul Center, for the X-ray data collection.

References

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Received: 2018-09-27
Accepted: 2018-10-25
Published Online: 2018-11-09
Published in Print: 2019-03-26

©2019 Kwang Ha, published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 Public License.

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