Home Crystal structure of poly-[diaqua-[bis(μ2-hydroxy)-bis(μ4-3,4,5,6-tetrachlorophthalato-κ3O,O′:O′; κ2O′′:O′′′)dilanthanum(III)], C8H3Cl4LaO6
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Crystal structure of poly-[diaqua-[bis(μ2-hydroxy)-bis(μ4-3,4,5,6-tetrachlorophthalato-κ3O,O′:O′; κ2O′′:O′′′)dilanthanum(III)], C8H3Cl4LaO6

  • Fa-Xue Ma , Dan Zhao EMAIL logo and Rui-Juan Zhang
Published/Copyright: December 21, 2016

Abstract

C8H3Cl4LaO6, monoclinic, P21/n (no. 14), a = 6.6874(10) Å, b = 6.0956(9) Å, c = 30.281(4) Å, β = 91.094(3)°, V = 1234.1(3) Å3, Z = 4, Rgt(F) = 0.048, wRref(F2) = 0.143, T = 296(2) K.

CCDC no.:: 1515750

A part of the title 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:Colourless prism
Size:0.20 × 0.05 × 0.05 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:43.4 cm−1
Diffractometer, scan mode:Bruker APEX-II, ω-scans
2θmax, completeness:56.8°, >97%
N(hkl)measured, N(hkl)unique, Rint:7933, 3014, 0.081
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1926
N(param)refined:172
Programs:Bruker programs [5], SHELX [6]
Table 2

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

AtomxyzUiso*/Ueq
La10.23121(8)0.21435(8)0.00479(2)0.01912(17)
Cl11.1296(4)0.5628(4)0.14107(8)0.0337(6)
Cl21.1677(4)0.2442(5)0.22141(9)0.0435(7)
Cl30.8639(4)−0.1394(5)0.23045(8)0.0395(7)
Cl40.5247(4)−0.1971(4)0.16043(8)0.0363(6)
C10.9758(13)0.3391(15)0.1454(3)0.0196(19)
C20.9864(13)0.2002(14)0.1820(3)0.0205(19)
C30.8507(13)0.0333(14)0.1857(3)0.022(2)
C40.6990(13)0.0043(15)0.1541(3)0.023(2)
C50.6955(12)0.1340(14)0.1164(3)0.0151(17)
C60.8345(12)0.2998(14)0.1123(3)0.0164(17)
C70.8333(12)0.4488(14)0.0723(3)0.0174(18)
C80.5308(12)0.1181(14)0.0807(3)0.0163(18)
O10.9517(9)0.4087(10)0.0414(2)0.0251(15)
O20.7135(9)0.6037(10)0.0706(2)0.0260(15)
O30.5820(9)0.0603(10)0.04201(19)0.0234(14)
O40.3586(10)0.1723(12)0.0889(2)0.0334(17)
H5B0.42440.58980.05610.040*
H5A0.27550.69700.03690.040*
H60.0159−0.11280.06270.040*
O50.3535(10)0.5944(11)0.0308(2)0.0310(16)
O60.0674(9)−0.1014(10)0.03728(19)0.0228(14)

Source of material

Colorless prism-shaped single crystals of the title compound were initially obtained using hydrothermal method. A mixture of 2 mmol 3,4,5,6-tetrachlorophthalic acid, 2 mmol of La(Ac)3 and 4.0 mmol KOH was sealed in a 30 mL Teflon-lined bomb at 180 °C for 7 days and then cooled to room temperature. A few crystals suitable for X-ray diffraction analysis were obtained.

Experimental details

Hydrogen atoms were placed in calculated positions and were included in the refinement in the riding model approximation, with Uiso(H) set to 1.2Ueq of the parent atom.

Discussion

The self-assembly of coordination polymers (CPs) is an intriguing area, which is yielding new generations of supramolecular architectures [1, 2] . Coordination by transition or rare-earth metals with multifunctional ligands is one of the main design principles. The 3,4,5,6-tetrachlorophthalate ligand is a remarkably versatile building block for the construction of supramolecular architectures due to its two rigid carboxyl groups and various coordination modes in the self-assembly reactions. By such coordination, a variety of supramolecular scaffolds are generated to control the arrangement of periodic channels and the formation of 1-, 2-, 3-D networks [3, 4].

The title structure contains one La(III) atom, one water molecule, one hydroxy ligand and one 3,4,5,6-tetrachlorophthalate in an asymmetric unit. The 3,4,5,6-tetrachlorophthalate ligand is deprotonated and acts as μ4-bridging. Considering the linking environment of the La(III) atoms, it is surrounded by nine O atoms, six from 3,4,5,6-tetrachlorophthalate ligands, one from coordinated water molecule, and two from hydroxy ligands. In an overview, the title compound features a two-dimensional structure, in which the layers are stacking along the c-axis.

References

1 Xi, Y.; Wei, W.; Xu, Y.; Huang, X.; Zhang, F.; Hu, C.: Coordination polymers based on substituted terpyridine ligands: synthesis, structural diversity, and highly efficient and selective catalytic oxidation of benzylic C—H bonds. Cryst. Growth Des. 15 (2015) 2695–2702.10.1021/acs.cgd.5b00008Search in Google Scholar

2 Lei, X.-W.; Yue, C.-Y.; Zhao, J.-Q.; Han, Y.-F.; Ba, Z.-R.; Wang, C.; Liu, X.-Y.; Gong, Y.-P.; Liu, X.-Y.: Syntheses, crystal structures, and photocatalytic properties of polymeric iodoargentates [TM(2,2-bipy)3] Ag3I5 (TM = Mn, Fe, Co, Ni, Zn). Eur. J. Inorg. Chem. 26 (2015) 4412–4419.10.1002/ejic.201500684Search in Google Scholar

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Received: 2016-6-20
Accepted: 2016-11-9
Published Online: 2016-12-21
Published in Print: 2017-3-1

©2016 Fa-Xue Ma et al., published by De Gruyter.

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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