Home The crystal structure of tetrakis(6-phenylpyridine-2-carboxylato-κ2N,O)-bis(1H-pyrazol-3-ylamine-κ2 N:N)dicobalt(II) dihydrate, C27H23N5O5Co
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The crystal structure of tetrakis(6-phenylpyridine-2-carboxylato-κ2N,O)-bis(1H-pyrazol-3-ylamine-κ2 N:N)dicobalt(II) dihydrate, C27H23N5O5Co

  • Gao Xiang and Tai Xi-Shi ORCID logo EMAIL logo
Published/Copyright: March 22, 2022

Abstract

C27H23N5O5Co, triclinic, P 1 (no. 2), a = 8.6503(7) Å, b = 11.1188(8) Å, c = 13.2711(11) Å, α = 79.185(7)°, β = 71.970(7)°, γ = 87.951(6)°, V = 1191.85(17) Å3, Z = 2, R gt (F) = 0.0450, wR ref (F 2) = 0.1143, T = 200 K.

CCDC no.: 2157664

The molecular structure is shown in the figure (The hydrate water molecule was omitted for clarity). 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 block
Size: 0.13 × 0.11 × 0.09 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.77 mm−1
Diffractometer, scan mode: SuperNova, ω
θ max, completeness: 25.0°, >99%
N(hkl)measured, N(hkl)unique, R int: 7764, 4188, 0.035
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 3577
N(param)refined: 346
Programs: Bruker [1], Olex2 [2], SHELX [3], Diamond [4]
Table 2:

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

Atom x y z U iso*/U eq
Co1 0.49294 (4) 0.31008 (3) 0.61683 (3) 0.01887 (15)
O1 0.6220 (2) 0.18818 (17) 0.52693 (15) 0.0223 (4)
O2 0.6744 (2) −0.00853 (17) 0.51837 (15) 0.0241 (4)
O3 0.3907 (2) 0.46017 (18) 0.67507 (15) 0.0242 (5)
O4 0.3396 (3) 0.5777 (2) 0.79980 (18) 0.0375 (6)
N1 0.5570 (3) 0.3045 (2) 0.77585 (17) 0.0183 (5)
N2 0.3726 (3) 0.1335 (2) 0.70471 (17) 0.0186 (5)
N3 0.3055 (3) 0.5654 (2) 0.49406 (18) 0.0209 (5)
H3A 0.320700 0.551263 0.558554 0.025*
H3B 0.213862 0.606595 0.500734 0.025*
N4 0.3475 (3) 0.3495 (2) 0.50726 (18) 0.0214 (5)
N5 0.3006 (3) 0.2610 (2) 0.46418 (19) 0.0274 (6)
H5 0.328575 0.185799 0.474301 0.033*
C1 0.4729 (3) 0.3911 (3) 0.8275 (2) 0.0204 (6)
C2 0.4512 (3) 0.3934 (3) 0.9349 (2) 0.0279 (7)
H2 0.392887 0.455407 0.967061 0.034*
C3 0.5174 (4) 0.3025 (3) 0.9932 (2) 0.0336 (8)
H3 0.502869 0.300622 1.065901 0.040*
C4 0.6054 (4) 0.2143 (3) 0.9415 (2) 0.0310 (7)
H4 0.651833 0.152426 0.979466 0.037*
C5 0.6258 (3) 0.2167 (3) 0.8328 (2) 0.0218 (6)
C6 0.7304 (3) 0.1267 (3) 0.7765 (2) 0.0218 (6)
C7 0.7266 (4) 0.0051 (3) 0.8262 (3) 0.0332 (8)
H7 0.651011 −0.021332 0.893530 0.040*
C8 0.8332 (5) −0.0775 (3) 0.7774 (3) 0.0435 (9)
H8 0.828712 −0.159124 0.811258 0.052*
C9 0.9464 (4) −0.0382 (3) 0.6782 (3) 0.0405 (9)
H9 1.020561 −0.093013 0.646028 0.049*
C10 0.9504 (4) 0.0809 (3) 0.6266 (3) 0.0357 (8)
H10 1.025050 0.106474 0.558859 0.043*
C11 0.8431 (3) 0.1628 (3) 0.6757 (2) 0.0262 (7)
H11 0.846407 0.243750 0.640517 0.031*
C12 0.3946 (3) 0.4857 (3) 0.7640 (2) 0.0238 (6)
C13 0.5959 (3) 0.0735 (3) 0.5618 (2) 0.0190 (6)
C14 0.4560 (3) 0.0397 (3) 0.6644 (2) 0.0199 (6)
C15 0.4210 (3) −0.0809 (3) 0.7131 (2) 0.0248 (7)
H15 0.481159 −0.143167 0.682459 0.030*
C16 0.2952 (4) −0.1077 (3) 0.8083 (2) 0.0289 (7)
H16 0.268560 −0.188412 0.842949 0.035*
C17 0.2102 (4) −0.0131 (3) 0.8509 (2) 0.0288 (7)
H17 0.126389 −0.029551 0.915762 0.035*
C18 0.2484 (3) 0.1076 (3) 0.7977 (2) 0.0223 (6)
C19 0.1523 (3) 0.2081 (3) 0.8431 (2) 0.0230 (6)
C20 0.1152 (4) 0.2094 (3) 0.9535 (2) 0.0295 (7)
H20 0.155658 0.148799 0.996501 0.035*
C21 0.0202 (4) 0.2987 (3) 0.9992 (3) 0.0337 (8)
H21 −0.001831 0.298669 1.072336 0.040*
C22 −0.0424 (4) 0.3880 (3) 0.9371 (3) 0.0373 (8)
H22 −0.108748 0.447336 0.968275 0.045*
C23 −0.0059 (4) 0.3890 (3) 0.8280 (3) 0.0379 (8)
H23 −0.046366 0.450235 0.785551 0.045*
C24 0.0904 (3) 0.2995 (3) 0.7811 (2) 0.0293 (7)
H24 0.113525 0.300839 0.707638 0.035*
C25 0.2783 (3) 0.4509 (3) 0.4709 (2) 0.0217 (6)
C26 0.1872 (4) 0.4273 (3) 0.4064 (3) 0.0324 (8)
H26 0.127291 0.482469 0.372547 0.039*
C27 0.2053 (4) 0.3056 (3) 0.4039 (3) 0.0358 (8)
H27 0.159630 0.261291 0.366945 0.043*
O5 0.1389 (3) 0.7012 (2) 0.6789 (2) 0.0395 (6)
H5A 0.194914 0.666534 0.718207 0.059*
H5B 0.201114 0.745526 0.622613 0.059*

Source of material

The title compound has been synthesized by following method: 0.0498 g 6-phenylpyridine-2-carboxylic acid (0.25 mmol), 0.0208 g 1H-pyrazol-3-ylamine (0.25 mmol), 0.020 g NaOH (0.5 mmol), and 0.0623 g Co(CH3COO)2·4H2O (0.25 mmol) were placed in a 100 mL flask containing 20 mL of an ethanol-water solution (v:v = 1:1) under stirring. Then the mixture was gradually heated up to 75 °C and maintained at this temperature for a further 5 h under constant stirring. The reactants were cooled to room temperature and filtered, and the filtrate was placed into a small conical flask to evaporate slowly. The yellow crystals of the title compound were received from the above solution in 20 days.

Experimental details

The hydrogen atoms were positioned geometrically (C–H = 0.93 Å, N–H = 0.86–0.89 Å and O–H = 0.85 Å). Their U iso values were set to 1.2U eq or 1.5U eq of the parent atoms.

Comment

The studying on the structure and properties of metal complexes has been one of the scientific hotspots [5], [6], [7], [8], [9]. 6-Phenylpyridine-2-carboxylate is a bidentate ligand with very strong coordination capacity, some complexes using it as a ligand have been synthesized and structurally characterized in previous studies of our group [10], [11], [12], [13], [14]. In this paper, another new dinuclear Co(II) complex has been synthesized using Co(CH3COO)2·4H2O, 1H-pyrazol-3-ylamine, 6-phenylpyridine-2-carboxylic acid, and NaOH. The results of structural analysis show that the dinuclear Co(II) complex contains two Co(II) ions, four 6-phenylpyridine-2-carboxylate ligands, two 1H-pyrazol-3-ylamine ligands (Figure 1). Two Co(II) ions are bridged by nitrogen atoms of two 1H-pyrazol-3-ylamine ligands. Each Co(II) ion is six-coordinated with two nitrogen atoms and two oxygen atoms of two different 6-phenylpyridine-2-carboxylate ligands, and two nitrogen atoms of two different 1H-pyrazol-3-ylamine ligands, forming a distorted CoN4O2 octahedron with O1 and O3 atoms in the axial position (O1–Co1–O3, 166.67(8)°). The Co–N distances are 2.178(2)–2.332(2) Å (Co1–N1, 2.332(2) Å; Co1–N2, 2.199(2) Å; Co1–N3a, 2.223(2) Å; Co1–N4, 2.178(2) Å) and the Co–O distances are 2.0299(19)–2.0446(19) Å (Co1–O1, 2.0446(19) Å, and Co1–O3, 2.0299(19) Å). The complex molecules are connected to each other through N–H⋯O hydrogen bonds between the 1H-pyrazol-3-ylamine molecules and the 6-phenylpyridine-2-carboxylate ligands to form a 1D chained structure.

Figure 1: 
The molecular structure of the title complex.
Figure 1:

The molecular structure of the title complex.


Corresponding author: Tai Xi-Shi, College of Chemistry and Chemical Engineering, Weifang University, Weifang, Shandong 261061, P. R. China, E-mail:

Funding source: National Natural Science Foundation of China

Award Identifier / Grant number: 21171132

Funding source: Natural Science Foundation of Shandong

Award Identifier / Grant number: ZR2014BL003

Funding source: Project of Shandong Province Higher Educational Science and Technology Program

Award Identifier / Grant number: J14LC01

Funding source: Science Foundation of Weifang

Award Identifier / Grant number: 2020ZJ1054

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

  2. Research funding: This project was supported by the National Natural Science Foundation of China (No. 21171132, http://dx.doi.org/10.13039/501100001809), the Natural Science Foundation of Shandong (ZR2014BL003, http://dx.doi.org/10.13039/501100007129), the Project of Shandong Province Higher Educational Science and Technology Program (J14LC01, http://dx.doi.org/10.13039/501100015642), and Science Foundation of Weifang (2020ZJ1054).

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

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Received: 2022-02-06
Accepted: 2022-03-11
Published Online: 2022-03-22
Published in Print: 2022-06-27

© 2022 Gao Xiang and Tai Xi-Shi, published by De Gruyter, Berlin/Boston

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

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