Home Crystal structure of poly[aqua-(2,2′-bipyridine-κN,N′)-(μ4-5,5′-(hexane-1,6-diyl)-bis(oxy)diisophthalato κ8O1,O2:O3,O4:O5,O6:O7,O8)manganese(II)], C21H21MnN2O7
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Crystal structure of poly[aqua-(2,2′-bipyridine-κN,N′)-(μ4-5,5′-(hexane-1,6-diyl)-bis(oxy)diisophthalato κ8O1,O2:O3,O4:O5,O6:O7,O8)manganese(II)], C21H21MnN2O7

  • Lu Liu EMAIL logo , Jin Zhang , Huiling Gao and Shaoxin Deng
Published/Copyright: March 13, 2017

Abstract

C21H21MnN2O7, triclinic, P1̅, a = 8.6230(17) Å, b = 9.967(2) Å, c = 13.257(3) Å, α = 80.92(3)°, β = 78.53(3)°, γ = 84.75(3)°, V = 1100.5(4) Å3, Z = 2, Rgt(F) = 0.0555, wRref(F2) = 0.1474, T = 293(2) K.

CCDC no.:: 1532295

A part of the title crystal structure is shown in the figure. The asymmetric unit is labeled. 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:Colourless irregular-shaped
Size:0.22 × 0.19 × 0.17 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:6.4 cm−1
Diffractometer, scan mode:Rigaku Saturn 724, φ and ω
2θmax, completeness:50°, >99%
N(hkl)measured, N(hkl)unique, Rint:11218, 3866, 0.043
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3284
N(param)refined:280
Programs:SHELX [13], CrystalClear [14]
Table 2

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

AtomxyzUiso*/Ueq
Mn1−0.03641(6)−0.14986(6)0.81828(4)0.0296(2)
O10.1150(4)0.0067(3)0.7292(2)0.0441(8)
O2−0.0345(3)0.0890(3)0.8626(2)0.0421(7)
O30.1570(4)0.7127(3)0.7393(3)0.0546(9)
O4−0.0561(4)0.6128(3)0.8193(2)0.0472(8)
O50.0545(3)−0.2088(3)0.9609(2)0.0441(7)
H50.0199−0.15381.00100.066*
H5A0.0932−0.28500.98500.066*
O60.5510(3)0.3257(3)0.6254(3)0.0485(8)
O70.1953(5)0.5369(4)0.0013(3)0.0864(13)
H7B0.15780.48430.06370.130*
H7A0.26070.5122−0.02240.130*
N1−0.2868(4)−0.1574(4)0.9094(3)0.0371(8)
N2−0.2038(4)−0.1227(3)0.7037(3)0.0362(8)
C1−0.1537(6)−0.1055(5)0.6004(3)0.0493(12)
H1−0.0481−0.08810.57410.059*
C2−0.2519(7)−0.1125(5)0.5317(4)0.0581(13)
H2−0.2139−0.09830.46040.070*
C3−0.4074(6)−0.1409(5)0.5704(4)0.0556(13)
H3−0.4756−0.14800.52550.067*
C4−0.4608(6)−0.1587(5)0.6760(3)0.0473(11)
H4−0.5656−0.17790.70340.057*
C5−0.3569(5)−0.1477(4)0.7416(3)0.0345(9)
C6−0.4030(5)−0.1623(4)0.8565(3)0.0391(10)
C7−0.5582(6)−0.1750(7)0.9064(4)0.0712(17)
H7−0.6376−0.17690.86850.085*
C8−0.5945(6)−0.1849(8)1.0138(4)0.081(2)
H8−0.6985−0.19411.04880.098*
C9−0.4753(6)−0.1809(7)1.0678(4)0.0661(16)
H9−0.4966−0.18701.13990.079*
C10−0.3246(5)−0.1676(5)1.0129(3)0.0510(12)
H10−0.2437−0.16561.04970.061*
C110.0734(4)0.1011(4)0.7832(3)0.0303(8)
C120.1582(4)0.2307(4)0.7514(3)0.0276(8)
C130.0819(5)0.3546(4)0.7751(3)0.0303(8)
H13−0.02290.35810.80990.036*
C140.1632(5)0.4721(4)0.7466(3)0.0311(9)
C150.3209(5)0.4670(4)0.6958(3)0.0333(9)
H150.37510.54630.67690.040*
C160.3967(4)0.3439(4)0.6736(3)0.0324(9)
C170.3136(4)0.2256(4)0.6997(3)0.0297(8)
H170.36310.14330.68230.036*
C180.0830(5)0.6078(4)0.7692(3)0.0370(9)
C190.6468(5)0.4419(5)0.6046(4)0.0453(11)
H19A0.64830.47610.66900.054*
H19B0.60270.51400.55830.054*
C200.8120(5)0.3985(5)0.5552(4)0.0453(11)
H20A0.80870.35840.49360.054*
H20B0.85740.33000.60340.054*
C210.9155(5)0.5191(5)0.5253(4)0.0436(11)
H21A0.91750.55910.58710.052*
H21B0.86890.58740.47750.052*

Source of material

The title compound was prepared under hydrothermal conditions. A mixture of 5,5′-(hexane-1,6-diyl)-bis(oxy)diisophthalic acid (22.1 mg, 0.05 mmol), 2,2′-bipyridine (15.6 mg, 0.1 mmol), manganese(II) actetate tetrahydrate (24.5 mg, 0.1 mmol), sodium hydroxide solution (0.2 mol/L, 0.5 mL) and H2O (10 mL) were placed in a Teflon-lined stainless steel vessel, heated to 130 °C for 3 day, and then cooled to room temperature. Colorless irregular-shaped crystals of the title compound were obtained.

Experimental details

The structure was solved by direct methods and refined with the SHELX crystallographic software package [13]. The hydrogen atoms were placed at calculated positions and refined as riding atoms with isotropic displacement parameters.

Discussion

Metal-organic frameworks (MOFs) with boundless network structures have been a vibrant research field and aroused considerable attention from both academia and industry [1], [2], [3], [4], [5], [6], [7]. Theoretical predictions and network-based methods to regulate the network topology and geometries have been done to generate serviceable functional frameworks [8]. Of the many advisable means to the design of these frameworks, the route of selecting choreographed organic ligands as building blocks with metal ions as nodes has been certified to be an effective strategy. In this paper, we have chosen the tetracarboxylic acids 5,5′-(hexane-1,6-diyl)-bis(oxy)diisophthalic acid (H4L) as an educt. H4L and the corresponding deprotonated anions are expected to be vigoroso precursors for the construction of outstanding structures as they may admit various coordination modes [9]. The flexibility of the (−CH2−)6 spacers and the existence of two methoxy groups will enable the carboxylic/carboxylate groups to coordinate metal ions in different directions [10], [11], [12]. On the other hand, the “mix-ligand” synthetic strategies also has become a research hotspot. By introducing 2,2′-bipy into the Mn(II)/L4− synthesis system, a new Mn(II) coordination polymer has been obtained.

As shown in the figure, the asymmetric unit contains one crystallographically independent Mn atom, one half of a L4− ligand, one 2,2′-bipy ligand and one coordinated water molecule. Mn1 is six-coordinated (MnO4N2), in which Mn1 is equatorially bonded to carboxylic oxygen atoms (O1, O3A, O4A and N1) from two different L4− ligands (Mn1—O1 = 2.171(3), Mn1—O3A = 2.257(3), Mn1—O4A = 2.385(3), Mn1—N1 = 2.256(3) Å) and one 2,2′-bipy ligand. The two axial sites are occupied by one N atom from one 2,2′-bipy ligand (Mn1—N2 = 2.265(3) Å) and one carboxyl O from one coordinated water molecule (Mn1—O5 = 2.165(3) Å). The bond angles around Mn range from 55.72(11) to 160.43(12)°. In this structure, the L4− anions connects four manganese(II) metal nodes in a κ8O1,O2:O3,O4:O5,O6:O7,O8-mode. The Mn1 ion and symmetry-related Mn1 metal centers show intermetallic distance of about 9.97 and 18.48 Å. The connection constructs a 1D stair-like structure (cf. the figure). Noticeably, the 2,2′-bipy ligand do not play an indispensable role in the construction of final 1D architecture.

Acknowledgement

This work was financially supported by the research start-up fund of Henan Institute of Science and Technology, the key scientific research project funding scheme of colleges and universities of henan province (16A150007).

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Received: 2016-8-4
Accepted: 2017-2-14
Published Online: 2017-3-13
Published in Print: 2017-5-24

©2017 Lu Liu 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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