Home The crystal structure of catena-poly[5-aminonicotinic acid-k1 N-m2-bromido-copper(I)], Cu(C6N2H6O2)Br
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The crystal structure of catena-poly[5-aminonicotinic acid-k1 N-m2-bromido-copper(I)], Cu(C6N2H6O2)Br

  • Nuo Chen , Qing-Hua Zheng , Wang Zhao and Wei-Wei Zhou ORCID logo EMAIL logo
Published/Copyright: June 1, 2023

Abstract

[Cu(C6N2H6O2)Br] n , monoclinic, P21/c (no. 14), a = 16.536(6) Å, b = 3.8463(14) Å, c = 14.403(6) Å, β =  115.009 ( 5 ) , V = 830.2(6) Å3, Z = 4, Rgt (F) = 0.0441, wRref (F 2) = 0.1054, T = 296 K.

CCDC no.: 2254951

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: Yellow chip
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 7.40 mm−1
Diffractometer, scan mode: Bruker D8 Venture, φ and ω-scans
θ max, completeness: 27.6°, >99 %
N (hkl)measuredN(hkl)uniqueR int: 4571, 1868, 0.037
Criterion for I obs, N(hkl)gt: I obs > 2σ(I obs), 1358
N(param)refined: 110
Programs: Bruker programs [1], DIAMOND [2], OLEX2 [3], SHELX [4, 5]
Table 2:

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

x y z U iso*/U eq
Br1 0.04937 (3) 0.60713 (12) 0.89026 (4) 0.03316 (18)
Cu1 0.04263 (5) 0.6119 (2) 0.71430 (6) 0.0449 (2)
N2 0.2571 (3) 0.2995 (14) 0.5384 (3) 0.0462 (13)
H2A 0.209158 0.221538 0.489664 0.055*
H2B 0.306793 0.292385 0.532741 0.055*
O2 0.3932 (3) 0.9469 (14) 0.9578 (3) 0.0588 (13)
O3 0.4754 (3) 0.7980 (16) 0.8761 (4) 0.0720 (16)
H3 0.514998 0.889406 0.926127 0.108*
N1 0.1651 (3) 0.5711 (11) 0.7167 (3) 0.0296 (9)
C1 0.1738 (3) 0.4479 (13) 0.6347 (4) 0.0313 (12)
H1 0.122907 0.364999 0.580441 0.038*
C2 0.2542 (4) 0.4356 (14) 0.6251 (4) 0.0331 (12)
C3 0.3302 (4) 0.5608 (15) 0.7076 (4) 0.0356 (12)
H3A 0.385498 0.558828 0.705148 0.043*
C4 0.3216 (3) 0.6870 (14) 0.7926 (4) 0.0329 (12)
C5 0.3996 (4) 0.8228 (16) 0.8836 (5) 0.0410 (14)
C6 0.2385 (3) 0.6903 (14) 0.7947 (4) 0.0334 (12)
H6 0.233596 0.778236 0.852295 0.040*

1 Source of materials

A mixture of CuBr (2 mmol, 0.286 g), 5-aminonicotinic acid (2 mmol, 0.276 mg), 0.4 mol L−1 NaOH solution (1 mL), H2O (7 mL) was sealed in a 25 mL Teflon-lined steel autoclave, and heated at 443 K for 6 days, then slowly cooled down to room temperature. Yellow block crystals could be seen in the product.

2 Experimental details

Coordinates of hydrogen atoms were added geometrically. Their U iso values were set to 1.2 U eq or 1.5 U eq of the parent atoms.

3 Comment

The 5-aminonicotinic acid and its derivatives are widely used in preparation of coordination compounds, because their complexes exhibit a wide range of applications [6], [7], [8], [9], [10], [11], [12], [13]. But there are few reports on its copper complexes [9], [10], [11], [12], [13].

Single-crystal X-ray diffraction analysis reveals that the title compound is a new ladder chain structure. The Cu(I) ion has a distorted tetrahedron geometry coordinated by one N atom from the 5-aminonicotinic acid ligand and three symmetry-related Br ligands. The bond angles of Br⋯Cu⋯N are from 107.3 to 114.8 , while the Br⋯Cu⋯Br angles range from 99.554 ( 31 ) to 111.847 ( 35 ) . The Cu–N distance is 2.0169(54) Å [11, 12], and the Cu–Br distances are in the range 2.4894(15)–2.5327(10) Å [13].

All Cu(I) ions are linked by μ 3-bridged Br atoms, constructing a one-dimensional ladder-[Cu12Br12]-chain. Each 5-aminonicotinic acid ligand is arranged on both sides of the ladder chain in the transtrans conformation, adopting monodentate coordination mode.


Corresponding author: Wei-Wei Zhou, School of Chemistry & Materials Engineering, Huainan Normal University, Huainan, Anhui 232038, P.R. China, E-mail:

Acknowledgments

We gratefully acknowledge the financial support NSF (Natural Science Foundation) of Anhui Province (2108085MB53), Project of Huainan City, University NSF of Anhui Province (KJ2020A0647) and the NSF for Distinguished Young Scholars of Anhui University (2022AH020087) and Program for Innovation Research Team in Huainan Normal University (XJTD202006).

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

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

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Received: 2023-04-23
Accepted: 2023-05-11
Published Online: 2023-06-01
Published in Print: 2023-08-28

© 2023 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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