Home Crystal structure of [(1,4,8,11-tetraazacyclotetradecane-κ4N,N′,N′′,N‴)tetracyanidodiplatinum(II)] dimethyl sulfoxide solvate, C18H36N8O2Pt2S2
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Crystal structure of [(1,4,8,11-tetraazacyclotetradecane-κ4N,N′,N′′,N‴)tetracyanidodiplatinum(II)] dimethyl sulfoxide solvate, C18H36N8O2Pt2S2

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Published/Copyright: February 3, 2025

Abstract

C18H36N8O2Pt2S2, monoclinic, P21/c (no. 14), a = 12.0848(16) Å, b = 14.1725(18) Å, c = 8.1065(9) Å, β = 97.603(4)°, V = 1376.2 Å3, Z = 2, Rgt(F) = 0.0279, wRref(F2) = 0.0749, T = 223 K.

CCDC no.: 2418535

The title crystal structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Colorless block
Size: 0.16 × 0.13 × 0.07 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 10.3 mm−1
Diffractometer, scan mode: Bruker APEX-II CCD, φ and ω scans
θmax, completeness: 28.4°, 100 %
N(hkl)measured, N(hkl)unique, Rint: 26775, 3439, 0.053
Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 2,962
N(param)refined: 155
Programs: Bruker, 1 SHELX 2 , PLATON 3
Table 2:

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

Atom x y z Uiso*/Ueq
Pt1 0.19549 (2) 0.52653 (2) 0.64789 (2) 0.02312 (7)
N1 0.1502 (4) 0.6092 (3) 0.4349 (5) 0.0288 (9)
H1 0.180 (6) 0.671 (5) 0.455 (9) 0.06 (2)*
N2 0.2000 (4) 0.4181 (3) 0.4729 (5) 0.0293 (8)
H2 0.281 (7) 0.410 (6) 0.472 (10) 0.09 (3)*
N3 0.2630 (4) 0.3894 (3) 0.9427 (6) 0.0407 (11)
N4 0.2144 (5) 0.6937 (3) 0.8960 (7) 0.0484 (13)
C1 0.1989 (5) 0.5578 (4) 0.2983 (7) 0.0369 (12)
H1A 0.1704 0.5851 0.1898 0.044*
H1B 0.2804 0.5636 0.3146 0.044*
C2 0.1662 (5) 0.4567 (4) 0.3038 (7) 0.0370 (12)
H2A 0.0851 0.4508 0.2746 0.044*
H2B 0.2023 0.4207 0.2225 0.044*
C3 0.1508 (4) 0.3232 (3) 0.4998 (7) 0.0336 (11)
H3A 0.1803 0.3015 0.6118 0.040*
H3B 0.1765 0.2788 0.4203 0.040*
C4 0.0238 (4) 0.3186 (3) 0.4820 (7) 0.0349 (11)
H4A −0.0062 0.3408 0.3705 0.042*
H4B 0.0015 0.2525 0.4907 0.042*
C5 −0.0287 (4) 0.3760 (3) 0.6095 (6) 0.0309 (10)
H5A −0.0154 0.3437 0.7172 0.037*
H5B 0.0083 0.4376 0.6222 0.037*
C6 0.2382 (4) 0.4413 (3) 0.8371 (6) 0.0294 (10)
C7 0.2044 (4) 0.6327 (3) 0.8043 (6) 0.0299 (10)
S1 0.52466 (12) 0.37642 (11) 0.38997 (18) 0.0414 (3)
O1 0.4279 (3) 0.3953 (3) 0.4853 (5) 0.0498 (10)
C8 0.5019 (6) 0.4465 (5) 0.2090 (8) 0.0537 (16)
H8A 0.5609 0.4352 0.1411 0.081*
H8B 0.5018 0.5126 0.2400 0.081*
H8C 0.4305 0.4303 0.1462 0.081*
C9 0.4997 (8) 0.2644 (6) 0.2945 (12) 0.090 (3)
H9A 0.5618 0.2478 0.2356 0.134*
H9B 0.4315 0.2668 0.2165 0.134*
H9C 0.4921 0.2173 0.3791 0.134*

1 Source of materials

To a solution of [Pt(cyclam)]Cl2 (cyclam = 1,4,8,11-tetraazacyclotetradecane; 0.1053 g, 0.226 mmol) in methanol (10 ml) was added K2Pt(CN)4 (0.0852 g, 0.226 mmol) and refluxed for 1 h. After cooling, the formed precipitate was separated by filtration, washed with methanol and acetone, and dried at 50 °C, to give a white powder (0.0902 g). Crystals suitable for X-ray diffraction analysis were obtained by slow evaporation from a dimethyl sulfoxide (DMSO) solution at 90 °C.

2 Experimental details

Hydrogen atoms on C atoms were positioned geometrically and allowed to ride on their parent atoms with d(C–H) = 0.98 or 0.97 Å and Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C) with the help of the SHELXL program (AFIX 23 or 137 options). 2 Hydrogen atoms bonded to N atoms were located from Fourier difference maps and refined isotropically; d(N–H) = 0.95(8) and 0.99(8) Å.

3 Comment

The crystal structures of the related heterometallic complexes [Ag(cyclam)M1(CN)4] n (cyclam = 1,4,8,11-tetraazacyclotetradecane; M1 = Pd, Pt) 5 and [Cu(cyclam)M2(CN)4] n (M2 = Ni, Pd, Pt) 6 have been determined previously. The structures are formed by one-dimensional cyanido-bridged chains. On the contrary, in the reported bimetallic compounds [Pd(cyclam)][M3(CN)4] (M3 = Pd, Pt, Ni), 7 , 8 , 9 the compounds consist of a cationic Pd(II) complex [Pd(cyclam)]2+ and an anionic M3(II) complex [M3(CN)4]2−, respectively.

The title compound consists of a dinuclear Pt(II) complex [Pt2(cyclam)(CN)4] and two solvent DMSO molecules. In the complex, each Pt(II) ion is four-coordinated in a distorted square-planar environment by two N atoms of a tetradentate cyclam ligand and two C atoms derived from two mutually cis-positioned CN ligands, and an inversion center is located at the centroid of the complex; the asymmetric unit contains one half of the compound. The tight N–Pt–N chelating angles of <N1–Pt1–N2 = 83.09(16)° contribute the distortion of the square-plane. The Pt–N(cyclam) bonds [Pt1–N1/2 = 2.099(4) and 2.097(4) Å] are slightly longer than the Pt–C(cyanido) bonds [Pt1–C6/7 = 1.967(5) and 1.961(5) Å]. The C≡N bond lengths are almost equal with d(C≡N) = 1.136(7) and 1.138(7) Å. In the crystal structure, the complex and solvent DMSO molecules are linked by extensive intermolecular N–H⋯O, N–H⋯N and C–H⋯N hydrogen bonds with distances of 2.762(6)–3.464(8) Å between the donor and acceptor atoms, forming a three-dimensional network. 4


Corresponding author: Kwang Ha, School of Chemical Engineering, Chonnam National University, Gwangju 61186, Republic of Korea, E-mail:

Acknowledgments

This study was financially supported by Chonnam National University (Grant number: 2024-1100-01). The author thanks the KBSI, Seoul Center, for the X-ray data collection.

  1. Conflict of interest: The authors declare no conflicts of interest regarding this article.

  2. Research funding: None declared.

References

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Received: 2025-01-06
Accepted: 2025-01-21
Published Online: 2025-02-03
Published in Print: 2025-04-28

© 2025 the author(s), published by De Gruyter, Berlin/Boston

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

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