Home Crystal structure of poly[tetra(μ2-cyanido-κ2N:O)-bis(N,N-dimethylformamide-κO)-manganese(II)-platinum(II)], C10H14MnN6O2Pt
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Crystal structure of poly[tetra(μ2-cyanido-κ2N:O)-bis(N,N-dimethylformamide-κO)-manganese(II)-platinum(II)], C10H14MnN6O2Pt

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Published/Copyright: February 11, 2021

Abstract

C10H14MnN6O2Pt, monoclinic, C2/m (no. 12), a = 15.8030(7) Å, b = 7.6794(3) Å, c = 7.0970(3) Å, β = 110.8462(17)°, V = 804.89(6) Å3, Z = 2, Rgt(F) = 0.0108, wRref(F2) = 0.0266, T = 223 K.

CCDC no.: 2060116

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:0.19 × 0.18 × 0.10 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:9.47 mm−1
Diffractometer, scan mode:PHOTON 100 CMOS, φ and ω
θmax, completeness:26.1°, >99%
N(hkl)measured, N(hkl)unique, Rint:13,288, 857, 0.054
Criterion for Iobs, N(hkl)gt:Iobs > 2σ(Iobs), 857
N(param)refined:74
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
Pt10.00000.50001.00000.01293 (6)
Mn10.00000.00000.50000.01480 (13)
O10.13526 (15)0.00000.4826 (4)0.0309 (5)
N10.03721 (13)0.2056 (2)0.7346 (3)0.0240 (4)
N20.23249 (18)0.00000.3127 (5)0.0307 (7)
C10.02585 (14)0.3157 (3)0.8325 (3)0.0183 (4)
C20.1513 (2)0.00000.3241 (5)0.0272 (7)
H20.100 (2)0.00000.190 (6)0.029 (10)*
C30.2450 (3)0.00000.1186 (7)0.0529 (13)
H3A0.300 (4)0.00000.599 (9)0.074 (19)*
H3B0.284 (3)0.100 (5)0.122 (6)0.075 (12)*
C40.3134 (3)0.00000.4932 (9)0.0592 (15)
H4A0.185 (4)0.00000.011 (9)0.069 (17)*
H4B0.354 (3)0.089 (6)0.484 (7)0.108 (17)*

Source of material

To a yellow suspension of [Mn(NCS)2(bipy)2] (bipy = 2,2′-bipyridine; 0.2345 g; 0.485 mmol) in MeOH (30 mL) was added K2Pt(CN)4 (0.1830 g, 0.485 mmol) and stirred for 5 h at room temperature. The formed precipitate was separated by filtration, washed with MeOH, H2O and acetone, and dried at 50 °C, to give a white powder (0.2274 g). Crystals suitable for X-ray diffraction analysis were obtained by slow evaporation from an H2O/N,N-dimethylformamide (DMF) solution at 60 °C.

Experimental details

All H atoms were located from Fourier difference maps and refined isotropically; C–H = 0.85(6)–1.01(4) Å. The highest peak (0.48 e Å−3) and the deepest hole (−0.63 e Å−3) in the difference Fourier map are located 0.88 and 0.87 Å from the atom Pt1, respectively.

Comment

The crystal structures of the related heterometallic cyanido-bridged Mn–Pt-complexes [{Mn(salen)}2Pt(CN)4]n (salen = N,N′-bis(salicylidene)ethylenediiminato) [5], [, 6], [Mn(L)Pt(CN)4]n (L = 2,13-dimethyl-3,12-diaza-6,9-dioxa-1(2,6)-pyridinacyclotridecaphane-2,12-diene) [7] and [Mn(phen)Pt(CN)4]n (phen = 1,10-phenanthroline) [8] have been determined previously.

The title complex has a heterometallic polymeric structure, in which the cationic [Mn(DMF)]2+ (DMF = N,N-dimethylformamide) units are connected by the anionic [Pt(CN)4]2− bridges, forming a two-dimensional square-grid network. The linking of two Pt units and two Mn units forms a slightly puckered 12-membered square structure. In the complex, the Pt(II) ion is four-coordinated in a slightly distorted square-planar environment by four C atoms of four CN ligands, whereas the Mn(II) ion is six-coordinated in a slightly distorted octahedral environment by four N atoms from four bridging [Pt(CN)4]2− units [9] and two axial O atoms from the two DMF solvent molecules, and the two metal cations are located on an inversion center, respectively. The complex is disposed about a twofold rotation axis running in the [010] direction passing through the Pt1 and Mn1 atoms, and has a crystallographic mirror plane parallel to the ac plane passing through the Pt1, Mn1, O1, N2, C2, C3 and C4 atoms, which are located at the special positions (x, 0, z), and thus the asymmetric unit contains one quarter of the compound [4]. The Mn–O axial bonds [Mn1–O1 = 2.185(2) Å] are slightly shorter than the Mn–N(cyanido) equatorial bonds [Mn1–N1 = 2.2170(18) Å].


Corresponding author: Kwang Ha, Research Institute of Catalysis, School of Chemical Engineering, Chonnam National University, Gwangju61186, Republic of Korea, E-mail:

Acknowledgements

The author thanks the KBSI, Seoul Center, for the X-ray data collection.

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: This research was supported by Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education (grant number: 2018R1D1A1B07050550)

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

References

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Received: 2021-01-17
Accepted: 2021-02-01
Published Online: 2021-02-11
Published in Print: 2021-05-26

© 2021 Kwang Ha, published by De Gruyter, Berlin/Boston

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

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