Home Crystal structure of catena-poly[hexakis(μ2-2-acetylphenolato-κ3O:O,O′)trimanganese(II)], C48H42Mn3O12
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Crystal structure of catena-poly[hexakis(μ2-2-acetylphenolato-κ3O:O,O′)trimanganese(II)], C48H42Mn3O12

  • Qian-jun Deng EMAIL logo and Dong-chu Chen
Published/Copyright: May 26, 2017

Abstract

C48H42Mn3O12, triclinic, P1̅ (no. 2), a = 9.1889(6) Å, b = 9.3226(9) Å, c = 12.8605(11) Å, α = 79.231(8)°, β = 73.223(7)°, γ = 89.228(7)°, V = 1035.26(15) Å3, Z = 1, Rgt(F) = 0.0593, wRref(F2) = 0.1664, T = 293 K.

CCDC no.:: 1546445

The asymmetric unit of the title coordination structure is shown in the figure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Yellow column
Size:0.41 × 0.23 × 0.12 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:9.7 cm−1
Diffractometer, scan mode:Bruker SMART, ω scans
2θmax, completeness:52.8°, >99%
N(hkl)measured, N(hkl)unique, Rint:8590, 4230, 0.047
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3375
N(param)refined:289
Programs:SHELX [1], Bruker programs [2]
Table 2

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

AtomxyzUiso*/Ueq
Mn10.16339(5)0.41059(5)0.46707(4)0.02551(19)
Mn20.50000.50000.50000.0261(2)
O1−0.0725(2)0.3715(3)0.56667(19)0.0275(5)
O20.1564(3)0.1725(3)0.5124(2)0.0361(6)
O30.1510(2)0.3796(3)0.30474(19)0.0332(6)
O40.4056(2)0.4236(3)0.37559(18)0.0290(5)
O50.2737(2)0.4290(3)0.59211(18)0.0272(5)
O60.5397(3)0.2704(3)0.5534(2)0.0341(6)
C10.7178(4)0.3024(4)0.1710(3)0.0384(9)
H10.82050.28560.16080.046*
C20.6507(4)0.2813(5)0.0906(3)0.0430(10)
H20.70710.25020.02680.052*
C30.4998(4)0.3074(4)0.1078(3)0.0396(9)
H30.45520.29520.05350.048*
C40.4085(3)0.3519(4)0.2035(3)0.0281(7)
C50.4778(3)0.3762(3)0.2859(3)0.0257(7)
C60.6343(4)0.3476(4)0.2650(3)0.0323(8)
H60.68250.36010.31730.039*
C70.2456(4)0.3693(4)0.2167(3)0.0286(7)
C80.1874(4)0.3748(5)0.1165(3)0.0420(9)
H8A0.07890.38160.13840.063*
H8B0.21380.28760.08690.063*
H8C0.23300.45860.06110.063*
C90.1220(4)−0.0711(4)0.6071(4)0.0458(10)
H9A0.1894−0.08870.53870.069*
H9B0.0332−0.13530.62860.069*
H9C0.1730−0.08880.66340.069*
C100.0753(4)0.0859(4)0.5921(3)0.0290(7)
C11−0.0613(4)0.1262(4)0.6700(3)0.0289(8)
C12−0.1297(3)0.2648(4)0.6527(3)0.0262(7)
C13−0.2665(4)0.2852(4)0.7314(3)0.0297(8)
H13−0.31640.37160.71980.036*
C14−0.3297(4)0.1817(4)0.8255(3)0.0373(9)
H14−0.42020.19980.87570.045*
C15−0.2601(4)0.0513(4)0.8460(3)0.0430(10)
H15−0.3000−0.01660.91100.052*
C16−0.1302(4)0.0250(4)0.7677(3)0.0419(9)
H16−0.0855−0.06430.77990.050*
C170.5174(4)0.0262(4)0.6464(3)0.0429(10)
H17A0.56950.01020.70220.064*
H17B0.58560.01200.57720.064*
H17C0.4315−0.04160.66770.064*
C180.4635(4)0.1805(4)0.6341(3)0.0311(8)
C190.2397(3)0.3397(4)0.6907(3)0.0259(7)
C200.1101(4)0.3653(4)0.7728(3)0.0344(8)
H200.05170.44430.75740.041*
C210.0666(4)0.2767(5)0.8759(3)0.0438(10)
H21−0.01910.29790.92930.053*
C220.1489(4)0.1559(5)0.9011(3)0.0465(10)
H220.11930.09570.97070.056*
C230.2754(4)0.1274(4)0.8207(3)0.0399(9)
H230.32980.04570.83690.048*
C240.3261(4)0.2168(4)0.7148(3)0.0296(8)

Source of material

A mixture of MnCl2⋅6H2O (0.083 g, 0.5 mmol), 2-acetylphenol (Hayp) (0.13 g, 1 mmol), triethylamine (0.5 mL), and distilled water (18 mL) was poured into a Teflon-lined autoclave (25 mL) and heated at 165 °C for 96 h. The title complex was collected as pale-yellow columnar crystals from the reaction mixture.

Experimental details

All H atoms attached to C atoms were positioned with idealized geometry and were refined with Uiso(H) = 1.2Ueq(C) using a riding model with C—H = 0.93 Å for aromatic H atoms and C—H = 0.96 Å for methylic H atoms.

Comment

The rational design and construction of coordination polymers have attracted widespread attention in recent years owing to their fascinating structures and potential functional applications [3], [4], [5], [6]. In the field of coordination frameworks, salicylic acid derivatives have been widely used due to their excellent bridging ability [7], [8], [9]. However, only few examples of 2-acetylphenolato (ayp) ligands have been reported [10], [11], [12]. In this paper, we select ayp to react with Mn2+ ions to construct a new coordination polymer.

The asymmetric unit of the title complex consists of one and a half Mn2+ ion and three ayp ligands. The coordination environment of both Mn(II) is similar. Each Mn center adopts a distorted octahedral coordination geometry involving six oxygen atoms from the four ayp ligands. Around the Mn1 center, the Mn—O bond length is 2.166(2)–2.252(2) Å, and the bond angles O—Mn—O are in the range of 76.83(8)°–173.19(8)°. Accordingly, the bond lengths and angles of the Mn2 center are in the ranges of 2.118(2)–2.252(2) Å and 76.52(8)°–180°, respectively. All bond lengths and angles lie in a normal range. Each ayp ligand connects two Mn2+ ions via the μ23O:O,O′ coordination. The Mn2+ ions are linked into an one-dimensional chain propagated in direction of the crystallographic c axis with a Mn—Mn distance of 3.376(2) Å. Meanwhile, the adjacent 1D chains are connected through weak intermolecular π-π stacking interactions.

Acknowledgement

We are grateful for the financial support from the Science and Technique Innovation Foundation of Foshan City [grant No. 2014HK100204], the Major Scientific Research Programs of Foshan University. Thanks are also sent to the special funding project of the technical innovation of Foshan city (2014AG10009) and the self-innovation promotion project of the universities in Guangdong province (2015KQNCX178).

References

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Received: 2016-12-14
Accepted: 2017-5-4
Published Online: 2017-5-26
Published in Print: 2017-7-26

©2017 Qian-jun Deng et al., published by De Gruyter, Berlin/Boston.

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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  61. Corrigendum
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