Home The crystal structure of tetrakis(6-phenylpyridine-2-carboxylate-κ 2 N,O)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 2 O:O′)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 3N,O:O)tetralead(II) C48H32N4O8Pb2
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The crystal structure of tetrakis(6-phenylpyridine-2-carboxylate-κ 2 N,O)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 2 O:O′)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 3N,O:O)tetralead(II) C48H32N4O8Pb2

  • Wang Li-Hua , Tai Hao-Wen , Li Qiu-Shi , Xia Yu-Pei ORCID logo EMAIL logo and Tai Xi-Shi ORCID logo
Published/Copyright: September 19, 2022

Abstract

C48H32N4O8Pb2, triclinic, P 1 (no. 2), a = 9.2712(8) Å, b = 14.5959(13) Å, c = 16.6178(13) Å, α = 76.089(7)°, β = 77.068(7)°, γ = 74.717(7)°, V = 2074.5(3) Å3, Z = 2, R gt (F) = 0.0563, wR ref (F 2) = 0.1783, T = 250 K.

CCDC no.: 2205534

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 needle
Size: 0.14 × 0.11 × 0.09 mm
Wavelength: Mo radiation (0.71073 Å)
μ: 8.17 mm−1
Diffractometer, scan mode: SuperNova, ω
θ max, completeness: 25.0°, >99%
N(hkl)measured, N(hkl)unique, R int: 13595, 7291, 0.048
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 5570
N(param)refined: 559
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 0.58527 (3) 0.73130 (2) 0.19173 (2) 0.02710 (7)
Pb2 0.64948 (3) 0.94295 (2) −0.09748 (2) 0.02269 (7)
O1 0.3359 (7) 0.5273 (5) 0.3657 (5) 0.0720 (16)
O2 0.4072 (6) 0.6410 (4) 0.2625 (3) 0.0376 (10)
O3 0.1470 (6) 0.9375 (4) 0.2349 (3) 0.0511 (13)
O4 0.3688 (5) 0.8562 (4) 0.1799 (3) 0.0305 (10)
O5 0.5303 (6) 0.6746 (4) 0.0755 (3) 0.0409 (11)
O6 0.6073 (6) 0.8055 (3) 0.0099 (3) 0.0324 (9)
O7 0.6180 (5) 0.9964 (3) 0.0323 (3) 0.0267 (9)
O8 0.6667 (6) 0.9584 (5) 0.1632 (3) 0.0487 (17)
N1 0.4558 (6) 0.7991 (4) 0.3315 (4) 0.0291 (9)
N2 0.7003 (7) 0.5544 (5) 0.2680 (3) 0.0347 (11)
N3 0.8865 (6) 0.8869 (4) −0.0210 (4) 0.0311 (9)
N4 0.5872 (6) 0.7682 (4) −0.1425 (3) 0.0258 (10)
C1 0.4998 (8) 0.7694 (5) 0.4078 (4) 0.0271 (7)
C2 0.3978 (8) 0.7783 (5) 0.4820 (5) 0.0339 (7)
H2 0.429946 0.756813 0.534460 0.041*
C3 0.2483 (9) 0.8195 (6) 0.4761 (5) 0.0431 (18)
H3 0.176669 0.824166 0.525735 0.052*
C4 0.2004 (10) 0.8543 (6) 0.3993 (5) 0.0429 (17)
H4 0.099482 0.886397 0.394981 0.051*
C5 0.3086 (8) 0.8393 (5) 0.3298 (4) 0.0327 (13)
C6 0.2692 (7) 0.8811 (5) 0.2411 (4) 0.0240 (9)
C7 0.6648 (8) 0.7342 (5) 0.4050 (4) 0.0262 (9)
C8 0.7219 (8) 0.6583 (5) 0.4682 (4) 0.0348 (11)
H8 0.656012 0.628376 0.512045 0.042*
C9 0.8774 (9) 0.6291 (6) 0.4639 (5) 0.0419 (13)
H9 0.916894 0.578519 0.505540 0.050*
C10 0.9758 (10) 0.6718 (6) 0.4005 (5) 0.0489 (12)
H10 1.080869 0.650547 0.400045 0.059*
C11 0.9235 (9) 0.7449 (6) 0.3380 (5) 0.0445 (13)
H11 0.991736 0.772674 0.294066 0.053*
C12 0.7681 (8) 0.7772 (5) 0.3405 (5) 0.0356 (13)
H12 0.731045 0.828538 0.298619 0.043*
C13 0.7056 (8) 0.9596 (5) 0.0861 (4) 0.0286 (12)
C14 0.8651 (7) 0.9089 (4) 0.0540 (4) 0.0236 (8)
C15 0.9783 (8) 0.8968 (5) 0.0981 (4) 0.0299 (12)
H15 0.956555 0.911100 0.152307 0.036*
C16 1.1274 (8) 0.8627 (5) 0.0606 (4) 0.0310 (11)
H16 1.208447 0.852855 0.089268 0.037*
C17 1.1535 (8) 0.8436 (6) −0.0201 (4) 0.0354 (11)
H17 1.253110 0.823518 −0.047883 0.042*
C18 1.0308 (7) 0.8545 (5) −0.0592 (4) 0.0274 (8)
C19 1.0542 (8) 0.8247 (5) −0.1417 (4) 0.0304 (6)
C20 1.1956 (12) 0.8190 (8) −0.2813 (6) 0.0745 (9)
H20 1.271840 0.836838 −0.325755 0.089*
C21 1.1692 (10) 0.8517 (7) −0.2070 (5) 0.0558 (11)
H21 1.227984 0.891936 −0.200099 0.067*
C22 1.1058 (11) 0.7581 (7) −0.2892 (6) 0.0674 (10)
H22 1.124241 0.734397 −0.339255 0.081*
C23 0.9962 (10) 0.7338 (6) −0.2277 (5) 0.0478 (10)
H23 0.937364 0.693820 −0.234942 0.057*
C24 0.9675 (8) 0.7665 (5) −0.1535 (4) 0.0306 (7)
H24 0.888775 0.749173 −0.110556 0.037*
C25 0.5657 (7) 0.7299 (5) 0.0094 (4) 0.0242 (7)
C26 0.5594 (8) 0.7032 (5) −0.0710 (4) 0.0264 (8)
C27 0.5299 (9) 0.6182 (5) −0.0714 (5) 0.0382 (9)
H27 0.509966 0.575563 −0.020055 0.046*
C28 0.5282 (11) 0.5927 (6) −0.1442 (5) 0.0538 (15)
H28 0.505782 0.533388 −0.143829 0.065*
C29 0.5590 (10) 0.6534 (6) −0.2162 (5) 0.0450 (11)
H29 0.561521 0.636160 −0.267569 0.054*
C30 0.5879 (9) 0.7438 (5) −0.2159 (4) 0.0332 (9)
C31 0.6177 (9) 0.8145 (5) −0.2951 (4) 0.0353 (12)
C32 0.7132 (10) 0.7835 (6) −0.3661 (5) 0.0443 (16)
H32 0.761202 0.717588 −0.362019 0.053*
C33 0.7393 (11) 0.8451 (6) −0.4410 (5) 0.0557 (19)
H33 0.804175 0.821904 −0.487515 0.067*
C34 0.6714 (11) 0.9388 (6) −0.4474 (5) 0.0562 (16)
H34 0.688965 0.982502 −0.498383 0.067*
C35 0.5736 (11) 0.9714 (6) −0.3772 (5) 0.0539 (18)
H35 0.520835 1.036450 −0.382682 0.065*
C36 0.5539 (9) 0.9113 (5) −0.3025 (5) 0.0404 (16)
H36 0.496043 0.935879 −0.255065 0.049*
C37 0.8497 (8) 0.5222 (5) 0.2733 (4) 0.0329 (12)
C38 0.8934 (9) 0.4644 (5) 0.3472 (5) 0.0375 (12)
H38 0.996600 0.446049 0.352142 0.045*
C39 0.7858 (9) 0.4332 (6) 0.4139 (5) 0.0424 (14)
H39 0.815169 0.391972 0.463219 0.051*
C40 0.6347 (9) 0.4646 (6) 0.4058 (5) 0.0427 (14)
H40 0.559119 0.445246 0.450003 0.051*
C41 0.5960 (8) 0.5237 (5) 0.3337 (4) 0.0316 (11)
C42 0.4342 (8) 0.5662 (5) 0.3217 (5) 0.0350 (9)
C43 0.9561 (9) 0.5539 (6) 0.1980 (5) 0.0396 (10)
C44 0.9183 (10) 0.5616 (6) 0.1208 (5) 0.0455 (14)
H44 0.826789 0.547093 0.118136 0.055*
C45 1.0149 (10) 0.5910 (6) 0.0457 (6) 0.0513 (11)
H45 0.991925 0.595307 −0.007612 0.062*
C46 1.1495 (11) 0.6136 (7) 0.0556 (7) 0.0614 (11)
H46 1.215949 0.634266 0.006890 0.074*
C47 1.1856 (11) 0.6071 (7) 0.1285 (7) 0.0665 (16)
H47 1.273283 0.626164 0.131376 0.080*
C48 1.0921 (9) 0.5713 (6) 0.2036 (6) 0.0531 (12)
H48 1.122621 0.559751 0.256104 0.064*

Source of materials

The Pb(II) complex was synthesized by the following method: 0.0996 g (0.50 mmol) 6-phenylpyridine-2-carboxylic acid, 0.1897 g (0.50 mmol) Pb(CH3COO)2.3H2O, and 0.040 g (0.50 mmol) NaOH were added to a solution containing 15 mL 95% ethanol and 15 mL water with stirring. The mixture was heated to 80 °C and the reaction was continued for 6 h. After the reaction was stopped and cooled to room temperature, the above mixture was filtered. The filtrate was transferred to a small beaker. The colorless needle crystals of the title compound were obtained in 22 days.

Experimental details

The hydrogen atoms were positioned geometrically (C–H = 0.94 Å). Their U iso values were set to 1.2U eq of the parent atoms. RIGU options were used to stabilize the refinement [3].

Comment

Lead(II) complexes have shown excellent potential applications in many aspects such as hydrogen storage capacity [5], fluorescence properties [6], antibacterial activities [7], silico analysis and physicochemical properties [8], and photochromism and metallomesogenic properties [9]. Our research group has been working on the synthesis, structure and properties of related metal complexes using the ligand used in the title compound [10], [11], [12], [13], [14], [15], [16].

The title structure of 1 was determined by X-ray single-crystal diffraction. The molecular structure is given in the figure. The title complex contains four lead(II) ions and eight 6-phenylpyridine-2-carboxylate (PPC) ligands. As shown in the figure, both Pb1 and Pb1a atoms are six-coordinated with four carboxylate oxygen atoms (O2, O4, O5, O6,or O2a, O4a, O5a, O6a) and two nitrogen atoms (N1, N2, or N1a, N2a) from six different PPC ligands, respectively. And both Pb2 and Pb2a atoms also are six-coordinated with four carboxylate oxygen atoms (O4a, O6, O7, O7a, or O4, O6a, O7, O7a) and two nitrogen atoms (N3, N4, or N3a, N4a) from four different PPC ligands, respectively. All Pb atoms adopt a distorted octahedral coordination polyhedron. The Pb–O and Pb–N distances are in the range of 2.319(5)–2.491(4) Å and 2.629(6)–2.655(6) Å, which are comparable to other lead(II) complexes. Thus the title complex is a tetranuclear species, The lead (II) complex forms the 3D supramolecular framework by weak interaction of phenyl rings and pyridine rings.


Corresponding author: Xia Yu-Pei, College of Chemistry and Chemical Engineering, Weifang University, Weifang, Shandong 261061, P. R. China, E-mail:

Funding source: National Natural Science Foundation of China https://doi.org/10.13039/501100001809

Award Identifier / Grant number: 21171132

Funding source: Natural Science Foundation of Shandong https://doi.org/10.13039/501100007129

Award Identifier / Grant number: ZR2014BL003

Funding source: Project of Shandong Province Higher Educational Science and Technology Program https://doi.org/10.13039/501100015642

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, https://doi.org/10.13039/501100001809), the Natural Science Foundation of Shandong (ZR2014BL003, https://doi.org/10.13039/501100007129), the Project of Shandong Province Higher Educational Science and Technology Program (J14LC01, https://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: 2022-07-25
Accepted: 2022-09-06
Published Online: 2022-09-19
Published in Print: 2022-12-16

© 2022 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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  32. The crystal structure of nitroxyl-κ N-{hydridotris(3-trifluoromethyl-5-methylpyrazolyl-1-yl-κN 3)borato}nickel(II), C15H13BF9N7NiO
  33. The crystal structure of [(2,2′-bipyridine-κ2 N,N)-bis(6-phenylpyridine-2-carboxylato- κ2 N,O)nickel(II)] monohydrate, C34H26N4O5Ni
  34. The crystal structure of 5-(2-fluoro-3-methoxyphenyl)-1-(2-fluoro-6-(trifluoromethyl)benzyl)-6-methylpyrimidine-2,4(1H,3H)-dione, C20H15F5N2O3
  35. The crystal structure of ethyl 2,3,5-trifluoro-4-(4-oxo-3,4-dihydropyridin-1(2H)-yl)benzoate, C14H12F3NO3
  36. [2,2′-{Ethane-1,2-diylbis[(azanylylidene)methanylylidene]}bis(3-bromo-2-hydroxyphenyl)]iron(III) nitrate, C20H12Br2CuN2O2
  37. The crystal structure of 1-(2-iodophenyl)-4-phenyl-1H-1,2,3-triazole, C14H10IN3
  38. Synthesis and crystal structure of 2-(2-oxo-2-(thiophen-2-yl)ethyl)-4H-chromen-4-one, C15H10O3S
  39. {6,6′-((1E,1′E)-((2,2-dimethylpropane-1,3-diyl)bis(azaneylylidene))bis(methaneylylidene))bis(2-bromo-4-chlorophenolate)-κ4N,N′,O,O′}copper(II), C19H16Br2Cl2CuN2O2
  40. The crystal structure of N′-[bis(2-hydroxyphenyl)methylidene]pyridine-4-carbohydrazide, C19H15N3O3
  41. Crystal structure of 2-chloro-6-formylphenolato-κ2O,O′-(6,6′-(((2,2-dimethylpropane-1,3-diyl)bis(azaneylylidene))bis(methaneylylidene))bis(2-chlorophenolato)κ4 N,N,O,O′)cobalt(III), C26H22Cl3CoN2O4
  42. The crystal structure of tetrakis(6-phenylpyridine-2-carboxylate-κ 2 N,O)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 2 O:O′)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 3N,O:O)tetralead(II) C48H32N4O8Pb2
  43. The crystal structure of 3,7-dihydroxy-9-methoxy-4a-methyl-4aH-benzo[c] chromene-2,6-dione —dichloromethane (1/1), C16H14Cl2O6
  44. The crystal structure of (Z)-6-(((5-chloro-2-hydroxyphenyl)amino)methylene)- 4-nitrocyclohexa, C13H9ClN2O4
  45. Crystal structure of dichlorido-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ1 N)zinc(II), C60H68O4N12Cl10Zn
  46. The crystal structure of 4-(2-bromoethoxy)-2-hydroxybenzaldehyde, C9H9BrO3
  47. The crystal structure of 5-azido-1-methyl-4-nitroimidazole, C4H4O2N6
  48. Crystal structure of dibromido-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)zinc(II), C60H68O4N12Br2Cl8Zn
  49. Crystal structure of tetrasodium-bis(μ 2-oxido)-hexafluoro-didioxo-molybdenum(V), Na2(Mo2O4F6)
  50. Crystal structure of (E)-N′-(2-chloro-6-hydroxybenzylidene)-4- hydroxybenzohydrazide-water (1/1), C14H13Cl1N2O4
  51. Crystal structure of (E)-N-(4-morpholinophenyl)-1-(quinolin-2-yl)methanimine, C20H19N3O
  52. The crystal structure of catena-poly[(1,10-phenanthroline-κ2 N,N′)-(μ3-2-hydroxybenzene-1,3-dicarboxylato-κ5 O,O′:O″,O‴:O‴)cadmium(II)], C20H12CdN2O5
  53. The crystal structure of 2,6-di-tert-butyl-4-(4-(methylthio)benzylidene)cyclohexa-2,5-dien-1-one, C22H28OS
  54. La3.65Mg30Sb1.07 as a disordered derivative of Th2Ni17-type structure
  55. Crystal structure of (E)-N-(4-morpholinophenyl)-1-(quinoxalin-2-yl)methanimine, C19H18N4O
  56. The crystal structure of 2,2′-(1,2-phenylenebis(methylene))bis(1,3-dimethylisothiouronium) bromide, C14H24Br2N4S2
  57. Crystal structure of tetraaqua-bis[4-(1H-1,2,4-triazol-1-yl)benzoato-κ1 N]zinc(II), C18H20ZnN6O8
  58. Crystal structure of bis(tricarbonyl)-{(S)-(tert-butoxycarbonyl)(1-methoxy-1-oxo-3-sulfido-k2 S:S′-propan-2-yl)amido-k2N:N′}diiron(I) (Fe—Fe), C15H15Fe2NO10S
  59. Crystal structure of (E)-3-((4-chlorophenyl)thio)-4-hydroxypent-3-en-2-one, C11H11ClO2S
  60. The crystal structure of (E)-3′,6′-bis(diethylamino)-2-((5-(diethylamino)-2-hydroxybenzylidene)amino)spiro[isoindoline-1,9′-xanthen]-3-one, C39H45N5O3
  61. The crystal structure of 2-(4-methoxynaphthalen-1-yl)-4H-chromen-4-one, C20H14O3
  62. The crystal structure of trans-dichlorido-(ethylenediamine-κ 2 N,N′)-bis(triphenylphosphine-κ 1 P)ruthenium(II), C38H38Cl2N2P2Ru
  63. The double polymeric chain of catena-poly[(μ2-6-bromopyridine-3-carboxylato-κ2 O,O′) (6-bromopyridine-3-carboxylato-κ2 O,O′) (μ2-1,2-bis(4-pyridyl)ethylene-κ2 N:N′)cobalt(II)], C24H16CoBr2N4O4
  64. The crystal structure of tert-butyl 2-(4-(12-bromo [2.2]paracyclophanyl)carbamoyl)pyrrolidine-1-carboxylate, C26H31BrN2O3
  65. The crystal structure of (Z)-2-(2,3-dimethoxybenzylidene)naphtho[1,2-b]furan-3(2H)-one, C21H16O4
  66. Crystal structure of 2-hydroxy-1-tosylindolin-3-yl- 2-naphthoate, C26H21N1S1O5
  67. The crystal structure of 1-methyl-N-(1-methyl-1H-imidazole-2-carbonyl)-1H-imidazole-2-carboxamide, C10H11N5O2
  68. The crystal structure of (E)-2-((5-bromo-2-hydroxybenzylidene)amino)-3′,6′-bis(ethylamino)-2′, 7′-dimethylspiro[isoindoline-1,9′-xanthen]-3-one, C33H31BrN4O3
  69. The crystal structure of dimethanol-5,15-diphenylporphyrin-21,23-diido-κ4 N,Nʹ,Nʺ,Nʹʺ-manganese(III) trans-dicyanido-bis(acetylacetonato-κ2O,Oʹ)ruthenium(III), C46H42N6O6RuMn
  70. Crystal structure of 1,4,8,11-tetraazacyclotetradecane-1,8-diium bis(3,5-dicarboxybenzoate), C28H36N4O12
  71. Bifurcated halogen bonds in the crystal structure of 2,2′-bi(1,8-naphthyridine)—1,4-diiodotetrafluorobenzene (1/1), C22H10F4I2N4
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