Crystal structure of diaqua-bis(μ2-6-phenylpyridine-2-carboxylate-κ3N,O:O)-bis(6-phenylpyridine-2-carboxylato-κ2N,O)lead(II) – N,N-dimethylformamide – water (1/2/4), C54H58N6O16Pb2

Xi-Shi Tai; Lei Liang; Xiang-Tao Li; Shu-Hua Cao; Li-Hua Wang

doi:10.1515/ncrs-2021-0277

Open Access Published by De Gruyter (O) August 13, 2021

Crystal structure of diaqua-bis(μ₂-6-phenylpyridine-2-carboxylate-κ³N,O:O)-bis(6-phenylpyridine-2-carboxylato-κ²N,O)lead(II) – N,N-dimethylformamide – water (1/2/4), C₅₄H₅₈N₆O₁₆Pb₂

Xi-Shi Tai , Lei Liang , Xiang-Tao Li , Shu-Hua Cao and Li-Hua Wang

From the journal Zeitschrift für Kristallographie - New Crystal Structures

https://doi.org/10.1515/ncrs-2021-0277

Abstract

C₅₄H₅₈N₆O₁₆Pb₂, triclinic, P 1 ‾ (no. 2), a = 9.4690(6) Å, b = 12.9374(6) Å, c = 13.2303(7) Å, V = 1341.90(15) Å³, α = 63.395(5)°, β = 74.291(5)°, γ = 69.113(5)°, Z = 1, R _gt(F) = 0.0284, wR _ref(F ²) = 0.0484, T = 150 K.

CCDC no.: 2100826

The molecular structure is shown in the figure. 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:	Colourless block
Size:	0.12 × 0.10 × 0.07 mm
Wavelength:	Mo Kα radiation (0.71073 Å)
μ:	6.34 mm⁻¹
Diffractometer, scan mode:	SuperNova, ω
θ _max, completeness:	25.0°, >99%
N(hkl)_measured, N(hkl)_unique, R _int:	8804, 4741, 0.035
Criterion for I _obs, N(hkl)_gt:	I _obs > 2 σ(I _obs), 4320
N(param)_refined:	373
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
Pb1	0.99366 (2)	0.60972 (2)	0.57645 (2)	0.01387 (6)
O1	0.7842 (4)	0.3530 (2)	0.8792 (2)	0.0254 (8)
O2	0.9374 (3)	0.4408 (2)	0.7288 (2)	0.0178 (7)
O3	0.6588 (4)	0.6860 (2)	0.5339 (2)	0.0216 (7)
O4	0.8582 (3)	0.5465 (2)	0.4960 (2)	0.0156 (7)
O6	1.0078 (4)	0.7502 (2)	0.3407 (2)	0.0253 (8)
H6A	1.003083	0.819051	0.287017	0.038*
H6B	1.024040	0.703421	0.307319	0.038*
N1	0.7872 (4)	0.6569 (3)	0.7464 (2)	0.0124 (8)
N2	0.7089 (4)	0.5256 (3)	0.3623 (2)	0.0136 (8)
C1	0.7292 (5)	0.7612 (3)	0.7617 (3)	0.0159 (10)
C2	0.6402 (5)	0.7640 (4)	0.8640 (3)	0.0205 (11)
H2	0.601570	0.836180	0.874007	0.025*
C3	0.6089 (5)	0.6617 (4)	0.9498 (3)	0.0217 (11)
H3	0.549660	0.663556	1.018006	0.026*
C4	0.6679 (5)	0.5555 (4)	0.9323 (3)	0.0191 (11)
H4	0.647456	0.484618	0.987993	0.023*
C5	0.7571 (5)	0.5570 (3)	0.8309 (3)	0.0131 (10)
C6	0.8308 (5)	0.4410 (3)	0.8120 (3)	0.0159 (10)
C7	0.7617 (5)	0.8707 (3)	0.6685 (3)	0.0151 (10)
C8	0.8128 (5)	0.9463 (3)	0.6897 (3)	0.0199 (11)
H8	0.831427	0.925136	0.762955	0.024*
C9	0.8367 (5)	1.0528 (4)	0.6036 (4)	0.0248 (12)
H9	0.872561	1.101962	0.618687	0.030*
C10	0.8066 (6)	1.0853 (4)	0.4951 (4)	0.0267 (12)
H10	0.818888	1.157930	0.437681	0.032*
C11	0.7593 (6)	1.0114 (4)	0.4724 (3)	0.0317 (13)
H11	0.742977	1.032760	0.398491	0.038*
C12	0.7346 (5)	0.9039 (3)	0.5580 (3)	0.0228 (11)
H12	0.700369	0.854786	0.541562	0.027*
C13	0.7184 (5)	0.6135 (3)	0.4877 (3)	0.0147 (10)
C14	0.6320 (5)	0.5998 (3)	0.4167 (3)	0.0123 (10)
C15	0.4800 (5)	0.6612 (3)	0.4113 (3)	0.0169 (10)
H15	0.430976	0.711576	0.450411	0.020*
C16	0.4021 (5)	0.6464 (3)	0.3466 (3)	0.0191 (11)
H16	0.299773	0.687505	0.340436	0.023*
C17	0.4788 (5)	0.5693 (3)	0.2911 (3)	0.0178 (10)
H17	0.428015	0.557289	0.247890	0.021*
C18	0.6319 (5)	0.5101 (3)	0.3002 (3)	0.0130 (9)
C19	0.7182 (5)	0.4280 (3)	0.2407 (3)	0.0140 (9)
C20	0.8616 (5)	0.4357 (4)	0.1798 (3)	0.0180 (10)
H20	0.904136	0.491434	0.177534	0.022*
C21	0.9411 (6)	0.3606 (4)	0.1226 (3)	0.0232 (11)
H21	1.036221	0.366967	0.081002	0.028*
C22	0.8805 (6)	0.2767 (4)	0.1270 (3)	0.0270 (12)
H22	0.935414	0.225309	0.089671	0.032*
C23	0.7374 (6)	0.2686 (4)	0.1870 (3)	0.0257 (12)
H23	0.696177	0.212089	0.189420	0.031*
C24	0.6557 (5)	0.3444 (4)	0.2434 (3)	0.0207 (11)
H24	0.559248	0.339380	0.282886	0.025*
O5	0.4868 (4)	0.8623 (2)	0.0557 (2)	0.0252 (8)
N3	0.6264 (5)	0.8713 (3)	0.1661 (3)	0.0207 (9)
C1S	0.6283 (6)	0.9130 (4)	0.2510 (3)	0.0267 (12)
H1SA	0.668858	0.981328	0.214594	0.040*
H1SB	0.690876	0.849818	0.307195	0.040*
H1SC	0.526218	0.935478	0.287238	0.040*
C2S	0.7710 (6)	0.8150 (4)	0.1147 (4)	0.0336 (13)
H2SA	0.833044	0.869989	0.078194	0.050*
H2SB	0.753437	0.793832	0.059137	0.050*
H2SC	0.822263	0.743870	0.172635	0.050*
C3S	0.4973 (6)	0.8891 (3)	0.1309 (3)	0.0212 (11)
H3S	0.406959	0.925022	0.166535	0.025*
O7	0.9995 (5)	0.9739 (3)	0.1557 (3)	0.0307 (9)
O8	0.7822 (5)	0.1192 (3)	0.9951 (3)	0.0295 (8)
H7A	1.066 (5)	0.944 (3)	0.112 (3)	0.032 (16)*
H7B	0.924 (4)	1.029 (3)	0.116 (4)	0.052 (17)*
H8A	0.787 (6)	0.190 (2)	0.955 (4)	0.049 (17)*
H8B	0.698 (4)	0.117 (5)	0.986 (5)	0.08 (3)*

Source of material

About 0.1 g 6-phenylpyridine-2-carboxylic acid (0.5 mmol), 0.020 g NaOH (0.5 mmol) and 0.1626 g lead acetate (0.5 mmol) were dissolved in 23 mL water-ethanol-N,N-dimethylformamide solution (v:v:v = 10:10:3) at room temperature. White precipitation occurs in the solution. The mixture was stirred for 5 h at 80 °C and continued to react for 4 h. The solution was filtered. After 10 days, the colorless crystals of the title compound were obtained from the filtrate.

Experimental details

The hydrogen atoms were positioned geometrically (C–H = 0.93–0.96 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

Many metal complexes containing nitrogen heterocycles may show good properties in fluorescence, biological activity, sensing performance and photocatalytic activity [5, 6]. Many metal complexes containing nitrogen heterocycles similar to that used in the title structure have been synthesized and structural characterized in our group [7], [8], [9]. In order to further study the structures of metal complexes containing nitrogen heterocycles, the title compound has been synthesized by the one-pot synthesis method. The asymmetric unit of the title structure contains one Pb(II) ion, one bidentate 6-phenylpyridine-2-carboxylate ligand, one tridentate 6-phenylpyridine-2-carboxylate ligand, one coordina-ted water molecule, two lattice water molecules and one uncoordinated DMF molecule. The Pb(II) ion is six-coordinated by three O atoms (O2, O4, O4a), two N atoms (N1 and N2a) from different 6-phenylpyridine-2-carboxylate ligands and one O atom (O6) from coordinated water molecule, which forms a distorted octahedral coordination environment. The complex forms a dimeric structure by the bridge effect of two O atoms (O4, O4a) of carboxylates (see the figure). The Pb(II) complex form a one-dimensional chain structure by the intermolecular OH ⃛ O hydrogen bonds. And the one-dimensional chains further form a three-dimensional network structure through the π–π stacking of benzene rings and pyridine rings.

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

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 and Technology Foundation of Weifang

Award Identifier / Grant number: 2020ZJ1054

Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
Research funding: This project was supported by the National Natural Science Foundation of China (No. 21171132), the Natural Science Foundation of Shandong (ZR2014BL003), the Project of Shandong Province Higher Educational Science and Technology Program (J14LC01) and Science and Technology Foundation of Weifang (2020ZJ1054).
Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2021-07-08

Accepted: 2021-08-02

Published Online: 2021-08-13

Published in Print: 2021-12-20

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