Home Physical Sciences Crystal structure of bis[(μ2-4⋯O,O′:O′)-(4-hydroxybenzoato-κ2O,O′)-(1,10-phenanthroline-κ2N,N′)]-di-lead(II)μ-4-hydroxybenzoato-κ3O,O′:O′;κ3O,O′:O′-bis-[(4-hydroxybenzoato-κ2O,O′)bis(1,10-phenanthroline-κ2N,N′)di-lead(II)] monohydrate, C52H36N4O12Pb2 ⋅ H2O
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Crystal structure of bis[(μ2-4⋯O,O′:O′)-(4-hydroxybenzoato-κ2O,O′)-(1,10-phenanthroline-κ2N,N′)]-di-lead(II)μ-4-hydroxybenzoato-κ3O,O′:O′3O,O′:O′-bis-[(4-hydroxybenzoato-κ2O,O′)bis(1,10-phenanthroline-κ2N,N′)di-lead(II)] monohydrate, C52H36N4O12Pb2 ⋅ H2O

  • Ben-Cai Dai , Chang-Chun Liu , Yang Zhou , Jin Chen , Yang Fu and Pei-Zheng Zhao ORCID logo EMAIL logo
Published/Copyright: February 12, 2020

Abstract

C52H36N4O12Pb2 ⋅ H2O, monoclinic, P21/n (no. 19), a = 13.7767(1) Å, b = 7.9925(1) Å, c = 21.2490(2) Å, β = 93.1490(10)°, V = 2336.20(4) Å3, Z = 4, Rgt(F) = 0.0220, wRref(F2) = 0.0582, T = 170 K.

CCDC no.: 1948114

The symmetric unit of the title compound 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:Colourless block
Size:0.18 × 0.15 × 0.12 mm
Wavelength:Cu Kα radiation (1.54184 Å)
μ:14.5 mm−1
Diffractometer, scan mode:SuperNova, ω
θmax, completeness:71.4°, >99%
N(hkl)measured, N(hkl)unique, Rint:13530, 4473, 0.025
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4280
N(param)refined:327
Programs:CrysAlisPRO [1], SHELX [2], [3], Olex2 [4]
Table 2:

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

AtomxyzUiso*/Ueq
Pb010.48621(2)0.02888(2)0.59982(2)0.01486(6)
O10.54684(16)0.1199(3)0.71761(10)0.0241(5)
O20.48805(15)0.2951(3)0.64403(10)0.0220(5)
O30.69817(16)0.8023(3)0.83811(11)0.0242(5)
H30.73960.76920.86440.036*
O40.66988(15)0.1705(3)0.58260(10)0.0233(5)
O50.54817(15)0.1857(3)0.51039(9)0.0202(5)
O60.86619(19)0.5518(4)0.35781(12)0.0304(6)
H60.92280.51970.36110.046*
N10.33194(18)0.1403(4)0.54478(12)0.0189(5)
N20.3284(2)−0.0268(3)0.65712(14)0.0209(6)
C10.3328(2)0.2258(4)0.49147(15)0.0228(7)
H10.39260.25570.47650.027*
C20.2483(3)0.2736(5)0.45643(16)0.0274(8)
H20.25210.33350.41910.033*
C30.1606(2)0.2311(5)0.47796(17)0.0307(8)
H3A0.10370.26000.45490.037*
C40.1558(2)0.1431(5)0.53518(16)0.0250(7)
C50.0659(2)0.0966(5)0.56160(19)0.0344(9)
H50.00760.12830.54090.041*
C60.0636(3)0.0089(5)0.6151(2)0.0352(10)
H6A0.0041−0.02080.63050.042*
C70.1528(3)−0.0400(5)0.64927(19)0.0275(8)
C80.1556(3)−0.1351(5)0.70479(17)0.0339(9)
H80.0980−0.17230.72100.041*
C90.2425(3)−0.1729(5)0.73504(16)0.0301(8)
H90.2450−0.23630.77180.036*
C100.3282(2)−0.1144(5)0.70980(15)0.0247(7)
H100.3873−0.13830.73110.030*
C110.2424(2)0.0091(4)0.62605(17)0.0207(7)
C120.2443(2)0.0998(4)0.56734(14)0.0192(7)
C130.5828(2)0.4093(4)0.73081(14)0.0183(6)
C140.6524(2)0.3789(4)0.77954(15)0.0209(7)
H140.67180.26950.78830.025*
C150.6928(2)0.5075(4)0.81484(17)0.0209(7)
H150.73960.48530.84690.025*
C160.6637(2)0.6698(4)0.80253(14)0.0199(7)
C170.5971(2)0.7046(5)0.75229(15)0.0248(7)
H170.57970.81440.74260.030*
C180.5573(2)0.5716(5)0.71683(16)0.0239(7)
H180.51280.59340.68330.029*
C190.5368(2)0.2653(4)0.69578(14)0.0183(6)
C200.6977(2)0.3088(4)0.48567(14)0.0167(6)
C210.7989(2)0.3018(4)0.49339(14)0.0195(7)
H210.82780.24290.52720.023*
C220.8564(2)0.3808(5)0.45167(15)0.0220(7)
H220.92370.37560.45730.026*
C230.8131(3)0.4693(4)0.40059(17)0.0223(7)
C240.7128(3)0.4799(4)0.39316(16)0.0217(7)
H240.68390.54100.35990.026*
C250.6557(2)0.3996(4)0.43521(14)0.0201(7)
H250.58830.40620.42980.024*
C260.6356(2)0.2176(4)0.52926(14)0.0180(6)
O71.05036(18)0.4552(3)0.34915(12)0.0293(6)
H7A1.10140.50580.36310.044*
H7B1.05800.42150.31180.044*

Source of materials

A solution of Pb(CH3COOH)2 ⋅ 3H2O (0.1902 g, 0.5 mmol) in distilled water (5 mL) was added to a solution of 1,10-phenanthroline (C12H8N2, 0.0906 g, 0.5 mmol) and 4-hydroxybenzoate acid (0.1392 g, 1 mmol) in ethanol/water (v:v = 1:1, 20 mL). The mixture was stirred at 323 K and refluxed for 6 h and then a white precipitate was filtered. Bright colorless single crystals were obtained by slow evaporation of the filtrate after 3 d at room temperature, one of which was selected for an X-ray experiment.

Experimental details

Hydrogen atoms bound to C were positioned geometrically and refined as riding atoms, with C—H = 0.93 Å. Hydroxy H atoms were refined in a similar manner, with O—H = 0.82 Å. Water H atoms were found according to the residual electron-density peaks around each water O atom and the directions of hydrogen bonds, and were then locked in position with O—H = 0.85 Å and included in the refinement with the SHELXL AFIX 3 command. Uiso(H) were set to Uiso(H) = 1.2Ueq(C or N) and Uiso(H) = 1.5Ueq(O), respectively.

Comment

The coordination chemistry of lead(II) with N and O donor ligands has been investigated in past decades as [5]. Because of its electronic configuration and size, Pb(II) exhibits various coordination numbers and geometries. A number of lead(II) complexes with different donor ligands has been synthesized and studied by X-ray crystallography [6], [7], [8], [9], [10].

The crystal structure of the title compound consists of dimeric units of Pb(C7H5O3)2(C12H6N2), related by a crystallographic inversion centre (the figure), and complemented by an uncoordinated water molecule. Each PbII cation is chelated by two N atoms of 1,10-phenanthroline with Pb—N distances of 2.531(2) Å and 2.589(3) Å, and five carbonyl O atoms from three 4-hydroxybenzoate anions. The 4-hydroxybenzoate groups coordinate to each PbII ion in two different ways. Two 4-hydroxybenzoate ions behave as chelating ligands to a Pb atom, two form bridges between the two Pb atoms. The five Pb—O distances are significantly different, as are the two Pb—N distances. The shortest Pb—O distance is 2.326(2) Å and the longest is 2.920(2) Å. The weak Pb—O bridging interactions form a centrosymmetric four-membered Pb2O2 quadrilateral with a Pb⋯Pb distance of 4.305(6) Å. Molecules are linked into a two-dimensional frameword by O—H⋯O hydrogen bonds. The packing is further stabilized by π–π interactions in the sequence of benzoate-phenanthroline-benzoate-phenanthroline of neighbouring molecules. The centroid-centroid distances between Cg1(C20-C25) and Cg2(N1/C1-C4/C12) [symmetry code: 1 − x, 1 − y, 1 − z] and between Cg3(N2/C10-C7/C11) [symmetry code: 1 − x, 1 − y, 1 − z] and Cg4(C20-C25) [symmetry code: x, 1 + y, z] are 3.521 Å and 3.613 Å, respectively. This combination of hydrogen bonds and π-π stacking interactions builds a three-dimensional network architecture.

Acknowledgements

Special Scientific Research Projects of Henan Academy of Science (18JB03006) is gratefully acknowledged.

References

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Received: 2019-11-14
Accepted: 2020-01-15
Published Online: 2020-02-12
Published in Print: 2020-04-28

©2020 Ben-Cai Dai et al., published by De Gruyter.

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

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  67. Crystal structure of (2-p-tolylpyrimidine-κ2C,N)(triphenylphosphane-κP) palladium(II), C29H24ClN2PPd
  68. Halogen bonding in crystal structure of bis(1,4,7,10-tetraoxacyclododecane-κ4O,O′,O′′,O′′′)cesium triiodide, C16H32CsI3O8
  69. The synthesis and crystal structure of N-(3-cyano-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-4-(trifluoromethylsulfinyl)-1H-pyrazol-5-yl)-2-phenylacetamide, C20H10N4Cl2F6O2S
  70. The crystal structure of 4-(trifluoromethyl)nicotinic acid, C7H4F3NO2
  71. Crystal structure of 3-(2-methylbenzyl)thiazolidin-2-one, C11H13ONS
  72. The crystal structure of 2,2,2-trifluoro-1-(isoquinolin-1-yl)ethane-1,1-diol, C11H8F3NO2
  73. The crystal structure of 3-bromoisonicotinic acid, C6H4BrNO2
  74. The crystal structure of 5-nitropicolinic acid monohydrate, C6H6N2O5
  75. The crystal structure of 3-(4-hydroxybenzyl)-1,5-dioxaspiro[5.5]undecane-2,4-dione, C16H18O5
  76. Crystal structure of [[Mo3Se7(S2CNEt2)3]2(μ-Se)] ⋅ 2(C6H4Cl2), C42H68Cl4Mo6N6S12Se15
  77. Crystal structure of (E)-4-hydroxy-3-((5-phenyl-1,3,4-oxadiazol-2-yl)thio)pent-3-en-2-one, C13H12N2O3S
  78. The crystal structure of (2,3-dioxo-5,6:13,14-dibenzo-9,10-benzo-1,4,8,11-7, 11-diene-κ4N,N′,N′′,N′′′)-nickel(II), Ni(C22H14N4O2)
  79. Crystal structure of 3-(1-benzyl-2-ethyl-4-nitro-1H-imidazol-5-ylthio)-propanoic acid, C15H17N3O4S
  80. The crystal structure of dichlorobis(2-(dicyclohexylphosphino)-2′,4′,6′-tri-i-propyl-1,1′-biphenyl) palladium(II)-dichloroform, C68H100Cl8P2Pd
  81. Crystal structure and antimicrobial properties of (1,4,7,10-tetraoxacyclododecane-κ4O,O′,O′′,O′′′)cesium(I) pentaiodide, C16H32CsI5O8
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