Home Physical Sciences Crystal structure of 4,4′-(1,4-phenylene)bis(pyridin-1-ium) catena-poly[diaqua-bis(μ2-3′,5′-dicarboxy-[1,1′-biphenyl]-2,5-dicarboxylato-κ2O:O′] dihydrate, C48H42O22N2Ca
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Crystal structure of 4,4′-(1,4-phenylene)bis(pyridin-1-ium) catena-poly[diaqua-bis(μ2-3′,5′-dicarboxy-[1,1′-biphenyl]-2,5-dicarboxylato-κ2O:O′] dihydrate, C48H42O22N2Ca

  • Dong-Mi Li and Shi-Hui Li EMAIL logo
Published/Copyright: October 20, 2017

Abstract

C48H42O22N2Ca, triclinic, P1̅ (no. 2), a = 7.2548(2) Å, b = 11.7056(4) Å, c = 14.6024(4) Å, α = 72.687(3)°, β = 82.667(2)°, γ = 73.303(3)°, V = 1132.76(6) Å3, Z = 1, Rgt(F) = 0.0403, wRref(F2) = 0.0993, T = 293(2) K.

CCDC no.:: 1577843

The crystal structure 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:Block, colourless
Size:0.41 × 0.32 × 0.28 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.23 mm−1
Diffractometer, scan mode:Bruker FRAMBO, φ and ω-scans
2θmax, completeness:25.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:13169, 4209, 0.030
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3588
N(param)refined:333
Programs:Bruker programs [1], SHELX [2]
Table 2

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

AtomxyzUiso*/Ueq
Ca11.00000.00000.00000.02588(15)
N10.2888(3)1.01816(15)0.45096(12)0.0345(4)
H10.25321.09720.44240.041*
O10.4591(3)0.18976(17)0.83379(12)0.0547(5)
H1W0.41190.27400.83050.082*
H2W0.59780.15850.83990.082*
O20.2174(3)0.11264(16)0.17397(13)0.0566(5)
H3W0.16830.04450.19370.085*
H4W0.14530.15910.21460.085*
O30.8053(3)−0.13190(19)0.01694(13)0.0672(6)
H5W0.6933−0.14360.05460.101*
H6W0.7656−0.1347−0.04150.101*
O40.6941(2)0.12995(13)0.22316(9)0.0355(4)
H40.77100.06130.23320.053*
O50.7544(2)0.12476(14)0.07079(10)0.0426(4)
O60.3233(2)0.44671(14)−0.17993(10)0.0420(4)
O70.1378(2)0.61116(13)−0.13538(10)0.0333(3)
H70.09940.6317−0.18990.050*
O80.0341(2)0.27860(12)0.29264(9)0.0309(3)
O90.1961(2)0.26086(13)0.41699(10)0.0406(4)
O10−0.0899(2)0.91697(13)0.28802(10)0.0425(4)
O110.1001(2)0.90262(12)0.15765(9)0.0322(3)
C10.6625(3)0.17342(17)0.13190(14)0.0265(4)
C20.5037(2)0.28865(16)0.10597(13)0.0216(4)
C30.4078(2)0.34745(16)0.17488(13)0.0216(4)
H30.44180.31340.23850.026*
C40.2618(2)0.45656(16)0.14985(12)0.0206(4)
C50.2147(2)0.50630(17)0.05356(13)0.0224(4)
H50.11870.58000.03550.027*
C60.3090(2)0.44742(17)−0.01549(13)0.0227(4)
C70.4535(3)0.33835(17)0.01096(13)0.0242(4)
H7A0.51680.2984−0.03500.029*
C80.1599(2)0.52225(16)0.22214(12)0.0212(4)
C90.0900(3)0.46126(16)0.31216(12)0.0218(4)
C10−0.0050(3)0.52967(17)0.37542(13)0.0273(4)
H10−0.05230.48920.43470.033*
C11−0.0309(3)0.65637(17)0.35245(13)0.0278(4)
H11−0.09530.70050.39570.033*
C120.0403(3)0.71765(17)0.26370(13)0.0243(4)
C130.1340(3)0.64953(16)0.20039(13)0.0233(4)
H130.18110.69050.14130.028*
C140.1083(3)0.32310(17)0.34219(13)0.0236(4)
C150.0143(3)0.85504(17)0.23481(13)0.0274(4)
C160.2583(3)0.50040(18)−0.11864(13)0.0265(4)
C170.3978(3)0.76490(18)0.47631(14)0.0291(4)
C180.2905(3)0.81753(19)0.54730(15)0.0344(5)
H180.25480.76650.60490.041*
C190.2377(3)0.94354(19)0.53270(15)0.0353(5)
H190.16550.97740.58030.042*
C200.3946(3)0.9715(2)0.38244(15)0.0388(5)
H200.43061.02500.32630.047*
C210.4512(3)0.84654(19)0.39320(15)0.0364(5)
H210.52580.81590.34470.044*
C220.4509(3)0.62914(18)0.48863(14)0.0292(4)
C230.4801(3)0.58160(19)0.40948(15)0.0357(5)
H230.46650.63600.34810.043*
C240.4716(3)0.54417(19)0.57991(15)0.0355(5)
H240.45230.57320.63410.043*

Source of material

A mixture of Ca(OAc)2)⋅H2O (0.1 mmol, 0.0176 g), biphenyl-2,5,3′,5′-tetracarboxylic acid (0.1 mmol, 0.033 g), 1,4-di(pyridin-4-yl)benzene (0.2 mmol, 0.015 g) and distilled water (10 mL) was heated in a 25 mL stainless steel reactor with a Teflon liner at 413 K for 45 h, and then slowly cooled down to room temperature. Colourless block crystals of the title compound were obtained.

Experimental details

C-bound hydrogen atoms were placed in calculated positions and were included in the refinement in the riding model approximation, with Uiso(H) set to 1.2 Ueq(C). The hydrogen atom of the hydroxyl group was allowed to rotate with a fixed angle around the C–O bond to best fit the experimental electron density, with Uiso(H) set to 1.5 Ueq(O).

Discussion

The synthetic development of coordination polymers (CPs) continues to attract much attention because of their intriguing structural topologies and potential applications in gas storage, separation, sensing and heterogeneous catalysis [3], [4], [5], [6]. In the construction of CPs, multidentate organic ligands play a vital role since the structural integrity of these ligands in most cases remains unaltered throughout the mixed-ligands strategy incorporating N-donor colinkers with different lengths and rigidness/exibility has been proved successful to create various CPs. In particular, different conformations of the ligand often play an important role in the self-assembly processes to form metal-organic coordination polymers. The organic carboxylate ligands have been proven to be good candidates for the construction of CPs [7], [8], [9], [10]. Thus, polycarboxylates have been widely utilized to construct coordination polymers [11, 12] . We chose 2,3′,5,5′-biphenyltetracarboxylic acid and 1,4-di(pyridin-4-yl)benzene to construct a new compound. In the course of this study the pure organic title compound was surprisingly obtained.

The asymmetric unit of the title structure contains one half of a Ca(II) ion, one 5,5′-dicarboxy-(1,10-biphenyl)-2,3′-dicarboxylate, one 4,4′-(1,4-phenylene)bis(pyridin-1-ium) cation and one water molecule. The calcium atom is six-coordinated by four oxygen atoms from two biphenyl-2,5,3′,5′-tetracarboxylate ligands, the Ca—O bond lengths range from 2.3040(13) to 2.3486(13) Å, and by two oxygen atoms from coordinated water molecules. The Ca—O3 bond length is 2.3186(18) Å. The O—Ca—O angles are in the range of 84.37(5)° to 180°. In addition, there are intermolecular hydrogen bonds between uncoordinated water molecules with adjacent biphenyl-2,5,3′,5′-tetracarboxylate anions: d(O(1)—H(1W)…O(6)B) = 2.837(2) Å, d(O(1)—H(2W)…O(11)A) = 3.073(2) Å, d(O(2)—H(4W)…O(8)) = 2.912(2) Å, d(O(2)—H(3W)…O(11)C) = 2.903(2) Å. Symmetry codes: A −x + 1, −y + 1, −z + 1; B x, y, z + 1 ; C x, y − 1, z. These interactions result in an infinite three dimensional architecture. The bond lengths and angles are generally in the expected ranges [13, 14] .

Acknowledgements

This work was supported by the Institutions of higher learning key scientific research project of Henan Province (18B150015).

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Received: 2017-6-22
Accepted: 2017-10-3
Published Online: 2017-10-20
Published in Print: 2017-11-27

©2017 Dong-Mi Li et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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  58. The crystal structure of the Matrine derivative: 12-(1H-indol-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one hydrate, C23H29N3O
  59. The crystal structure of tris(μ2-1,3-bis(4,4,4-trifluoro-3-oxido-1-(oxo)but-2-en-1-yl)phenyl-κ4O,O′:O′′,O′′′)-bis(1,2-dimethoxyethane-κ2O,O′)dilutetium(III), C50H38F18Lu2O16
  60. The crystal structure of (Z)-2-(3-(2-(4-chlorobenzoyl)hydrazono)-2-oxoindolin-1-yl) acetic acid, C17H12ClN3O4
  61. Synthesis and crystal structure of trans-tetraqua-bis(2-(((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)ammonio)acetato-κO)cobalt(II) hexahydrate, C36H48CoN2O28S2
  62. The crystal structure of N,N-dimethyl-2,6-di-p-tolylpyrimidin-4-amine, C20H21N3
  63. The crystal structure (E)-4-methyl-N′-(2-nitrobenzylidene)benzenesulfonohydrazide, C14H13N3O4S
  64. Crystal structure of catena-poly[(μ2-1,3-bis(benzimidazol-1-yl)propane κ2N:N′)-(μ2-5-methoxyisophthalato-κ2O:O′)zinc(II)] hydrate, C26H24ZnN4O6
  65. The crystal structure of (E)-N′-(quinolin-2-ylmethylene)furan-2-carbohydrazide monohydrate, C15H13N3O3
  66. Crystal structure of 2,8-diphenyl-3,7,9-trioxa-1-azaspiro[4.5]dec-1-ene, C18H17N1O3
  67. Crystal structure of diethyl 2-(4-chlorophenyl)-1,3-dioxane-5,5-dicarboxylate, C16H19ClO6
  68. Crystal structure of 1-(carboxymethyl)-1H-benzo[d][1,2,3]triazole 3-oxide, C8H7N3O3
  69. Crystal structure of (acetylacetonato-κ2O,O′)-(2-amino-6-chlorobenzoato-κO)-oxido(1,10-phenanthroline-κ2N,N′)vanadium(IV) – trichloromethane (1/1)
  70. Crystal structure of (1E,4E)-1,5-bis(4-chlorophenyl)penta-1,4-dien-3-one, C17H12Cl2O
  71. The crystal structure of trans-dibromido-bis(pyridine-κN)platinum(II), C10H10Br2N2Pt
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