Home Physical Sciences Crystal structure of catena-poly[diaqua-bis(μ2-1H-benzo[d]imidazole-5-carboxylato-κ2N:O)nickel(II)] dihydrate, C16H18N4NiO8
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Crystal structure of catena-poly[diaqua-bis(μ2-1H-benzo[d]imidazole-5-carboxylato-κ2N:O)nickel(II)] dihydrate, C16H18N4NiO8

  • Wang Xin , Liu Qingyun , Yang Liguo EMAIL logo , Liu Nana and Dai Yuqiang
Published/Copyright: February 6, 2018

Abstract

C16H18N4NiO8, monoclinic, C2/c (no. 15), a = 16.1598(8) Å, b = 8.7803(5) Å, c = 14.1809(11) Å, β = 118.197(1)°, V = 1773.32(19) Å3, Z = 4, Rgt(F) = 0.0220, wRref(F2) = 0.0598, T = 273(2) K.

CCDC no.: 1818183

A part of the title crystal structure is shown in the figure. 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:Green block
Size:0.38 × 0.26 × 0.20 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.15 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
θmax, completeness:25°, >99%
N(hkl)measured, N(hkl)unique, Rint:4327, 1568, 0.016
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1474
N(param)refined:133
Programs:Bruker programs [1], SHELX [2, 3]
Table 2:

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

AtomxyzUiso*/Ueq
Ni10.00001.00000.00000.02092(11)
O10.09367(8)0.93388(12)0.16166(8)0.0272(2)
O20.16481(8)0.72938(13)0.14089(9)0.0324(3)
O3−0.07765(8)1.13558(13)0.05024(9)0.0340(3)
H9−0.11231.1915−0.00280.051*
H10−0.09991.14140.09380.051*
C10.13350(10)0.80590(17)0.19249(12)0.0243(3)
C30.10419(10)0.81796(17)0.34983(12)0.0240(3)
H30.07680.91320.32690.029*
C20.14242(10)0.74053(17)0.29469(12)0.0244(3)
C40.10743(10)0.75090(17)0.43998(12)0.0233(3)
C60.14652(11)0.60571(18)0.47196(12)0.0269(3)
C70.18671(13)0.52743(19)0.41909(14)0.0337(4)
H70.21400.43220.44220.040*
C50.08998(11)0.68848(18)0.57616(12)0.0291(3)
H50.07340.69070.63060.035*
C80.18462(12)0.59641(19)0.33101(13)0.0308(4)
H80.21170.54700.29430.037*
N10.07270(9)0.80092(15)0.50807(10)0.0261(3)
N20.13392(10)0.57039(16)0.55931(11)0.0313(3)
H20.15110.48770.59610.038*
O40.85326(10)0.16957(16)0.19135(11)0.0485(4)
H110.86660.09730.23610.073*
H120.79990.20180.18060.073*

Source of material

A solution of 1H-benzo[d]imidazole-5-carboxylic acid (HL, 0.10 mmol) in MeOH (5 mL) was neutralized by NaOH and carefully layered on a solution of NiBr2 (0.10 mmol) in H2O (5 mL). Diffusion between the two phases over a period of 2 weeks produced lighted yellow block crystals (Yield 46% based on HL).

Experimental details

All H atoms were placed geometrically and treated as riding on their parent atoms, with C—H 0.96, with Uiso(H) = 1.5Ueq(C).

Discussion

The understanding of various molecular interactions plays a major role in supramolecular chemistry and crystal engineering. The knowledge of structural motifs generated by such interactions can be utilized in the design of novel materials with desirable physical and chemical properties. Hydrogen bonding and π–π stacking interactions are by far the most well-studied interactions. These interactions are employed to control the conformational and topological features of the molecular assembly in the solid state [e.g. 4, 5]. In the last decade, benzimidazole-5-carboxylic acid (HL) was widely used in the design of therapeutic agents, such as diuretic and natriureitc, antiparasitic, serotonin antagonist, antineoplastic and antiflarial, herbicidal, and antihypertensive compounds. The analysis of various interactions in drugs has attracted considerable interest for their wide-ranging antiviral activity and the possibiligy of forming supramolecular aggregates with transition-metal ions. However, to the best of our knowledge, up to now few of attention has been attached on the coordination behavior of benzimidazole-5-carboxylic acid(HL) [6], [7], [8].

As shown in the figure, the Ni ion lies in a slightly distorted environment, consisting of two oxygen donors from two carboxylate groups, two oxygen atoms from two water ligands, and two benzimidazole nitrogen atoms from two ligands. The adjacent Ni ions are linked by the 1H-benzo[d]imidazole-5-carboxylato ligands to form a 1D chain through. The adjacent 1D chains are linked to a network through hydrogen bonds.

Acknowledgements

This work was supported by Henan science and technology project (nos. 172102210161, 172102210160, 172102310166) and the Research Fund of Anyang Institute of Technology (nos. YJJ2016014).

References

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Received: 2017-9-21
Accepted: 2018-1-19
Published Online: 2018-2-6
Published in Print: 2018-3-28

©2018 Wang Xin et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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