Home The crystal structure of trans-tetraaqua-bis(p-tolylsulfinato-κO)calcium(II)), C14H22O8S2Ca
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The crystal structure of trans-tetraaqua-bis(p-tolylsulfinato-κO)calcium(II)), C14H22O8S2Ca

  • Tai Xi-Shi EMAIL logo and Li Peng-Fei
Published/Copyright: October 27, 2017

Abstract

C14H22O8S2Ca, monoclinic, P21/c (no. 14), a = 16.349(3) Å, b = 5.0828(10) Å, c = 12.183(2) Å, β = 109.29(3)°, V = 955.5(3) Å3, Z = 2, Rgt(F) = 0.0376, wRref(F2) = 0.1129, T = 293(2)K.

CCDC no.: 1578699

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:Yellow block
Size:0.18 × 0.17 × 0.17 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.58 mm−1
Diffractometer, scan mode:Bruker SMART, ω-scans
2θmax, completeness:25°, >99%
N(hkl)measured, N(hkl)unique, Rint:6900, 1672, 0.029
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1603
N(param)refined:116
Programs:Bruker programs [1], SHELX [2, 3] , DIAMOND [4]
Table 2

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

AtomxyzUiso*/Ueq
S10.177639(19)0.91649(7)1.40501(3)0.0260(2)
Ca0.00001.00001.50000.0289(2)
O1W0.11949(7)1.1131(2)1.66464(9)0.0423(3)
H1WB0.13821.25871.69770.063*
H1WA0.14200.98531.71030.063*
O10.16399(7)0.8873(2)1.27650(8)0.0361(3)
O2W−0.00887(8)0.6519(2)1.62043(10)0.0513(4)
H2WB0.03650.61311.67730.077*
H2WA−0.04240.51961.61010.077*
O20.10055(6)0.7977(2)1.43021(9)0.0352(3)
C10.25877(8)0.6708(3)1.46800(11)0.0274(3)
C20.26579(10)0.5712(3)1.57614(13)0.0374(4)
H20.22790.62741.61390.045*
C30.32924(11)0.3877(3)1.62834(15)0.0432(4)
H30.33350.32181.70120.052*
C40.38666(10)0.3000(3)1.57432(13)0.0396(4)
C50.37915(10)0.4050(4)1.46657(14)0.0433(4)
H50.41730.35041.42890.052*
C60.31589(10)0.5904(3)1.41331(13)0.0368(4)
H60.31220.65961.34120.044*
C70.45396(14)0.0953(3)1.63094(17)0.0578(5)
H7A0.4396−0.06651.58830.087*
H7B0.45540.06721.70950.087*
H7C0.50970.15491.63120.087*

Source of materials

1.0 mmol sodium p-tolylsulfinate (0.178 g) and 0.5 mmol calcium perchlorate tetrahydrate (0.311 g) were dissolved in an aqueous-ethanol (v:v = 1:2) solution. The above mixture was stirred for 5 h at 65 °C. The reactant was filtered. The yellow crystals of the title complex were obtained after 20 days.

Experimental details

Coordinates of hydrogen atoms were refined without any constraints or restraints. Their Uiso values were set to 1.2Ueq of the parent atoms.

Comment

Calcium is an important biological element. Relatively few studies have been done on synthesis, structure and property of Ca(II) complexes comparing to transition metal complexes [5], [6], [7], [8]. In order to investigate the synthesis, structure and properties of a further Ca(II) complex, the title compound has been synthesized and structurally characterized. The title complex contains one Ca(II) ion, two p-tolylsulfinate ligands and four coordinated water molecules. The Ca(II) ion is six-coordinated with two O atoms from two p-tolylsulfinate ligands and four O atoms from four coordinated water molecules (cf. the figure). The Ca(II) ion adopts a distorted octahedral geometry with two O atoms (O2 and O2A) at the axial positions, and four O atoms(O1W, O1WA, O2W, O2WA) in the equatorial plane. Adjacent complexes are connected by intermolecular hydrogen bonds. Bond lengths and angles are in the expected ranges and fit with a structurally related compound [9] hydrogen bonds.

Acknowledgement

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 Foundation of Weifang.

References

Bruker: SAINT and SADABS. Bruker AXS Inc., Madison, WI, USA (2000).Search in Google Scholar

Sheldrick, G. M.: A short history of SHELX. Acta. Crystallogr. A64 (2008) 112–122.10.1107/S0108767307043930Search in Google Scholar PubMed

Sheldrick, G. M.: Crystal structure refinement with SHELXTL. Acta. Crystallogr. C71 (2015) 3–8.10.1107/S2053229614024218Search in Google Scholar PubMed PubMed Central

Brandenburg K.: DIAMOND. Visual Crystal Structure Information System. Ver. 3.2. Crystal Impact, Bonn, Germany, (2012).Search in Google Scholar

Yang, Z.-Y.; Yang, R.-D.; Yu, K.-B.: The crystal structures and thermal stability of the complexes of 2- oxo-propionic acid (4-pyridinecarbonyl) hydrazone with alkaline earth metals. Acta. Chim. Sinica. 57 (1999) 236–243.Search in Google Scholar

Wu, G.; Zhang, S.-Q.; Wang, X.-F.; Liu, G.-X.: Synthesis, structure, luminescence properties of alkaline earth metal calcium complex with maleic anhydride ligand and a new precursor to produce pure phase micro-sized calcite particles. Synth. React. Inorg. M. 44 (2014) 1429–1434.10.1080/15533174.2013.809745Search in Google Scholar

Tai, X.-S.; Zhang, Y.-P.; Zhao, W.-H.: Synthesis, crystal structure and antitumor activity of a dinuclear calcium complex based on 1,5-naphthalenedisulfonate and 2,2′-bipyridine ligands. Res. Chem. Intermed. 41 (2015) 4339–4347.10.1007/s11164-014-1533-9Search in Google Scholar

Tai, X.-S.; Wang, X.: Synthesis and crystal structure of a 1D chained coordination polymer constructed from Ca2+ and 2-[(E)-(2-furoylhydrazono)methyl]benzenesulfonate. Crystals 5 (2015) 458–465.10.3390/cryst5040458Search in Google Scholar

Langs, D. A.; Hare, C. R.: The structure of bis(toluene-p-sulphinato)copper(II) tetrahydrate. Chem. Commun. (1967) 853–854.10.1039/c19670000853Search in Google Scholar

Received: 2017-7-16
Accepted: 2017-10-8
Published Online: 2017-10-27
Published in Print: 2018-1-26

©2018 Tai Xi-Shi 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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