Home Crystal structure of tetraqua-bis(4-(hydroxymethyl)benzoato-κO)cobalt(II), C16H22O10Co
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Crystal structure of tetraqua-bis(4-(hydroxymethyl)benzoato-κO)cobalt(II), C16H22O10Co

  • Haixia Pang ORCID logo EMAIL logo , Zhucan Xie , Hong Zhang , Baoming Xu and Hongyu Gan
Published/Copyright: November 14, 2019

Abstract

C16H22O10Co, monoclinic, P21/c (no. 14), a = 9.811(2) Å, b = 15.530(3) Å, c = 13.639(3) Å, β = 122.122(3)°, V = 1760.0(6) Å3, Z = 4, Rgt(F) = 0.0243, wRref(F2) = 0.0821, T = 297(2) K.

CCDC no.: 1870917

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:Red block
Size:0.12 × 0.10 × 0.10 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.03 mm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω
θmax, completeness:26.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:13698, 3630, 0.024
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3147
N(param)refined:275
Programs:Bruker [1], SHELX [2], [3]
Table 2:

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

AtomxyzUiso*/Ueq
Co10.50001.00000.00000.01816(11)
O10.64030(14)0.81942(7)0.15867(9)0.0337(3)
O20.49999(12)0.93834(7)0.13528(8)0.0263(2)
O30.87911(15)0.80479(7)0.74794(9)0.0369(3)
H3A0.826(2)0.7601(9)0.7288(17)0.055*
O40.56340(12)0.88314(6)−0.04615(8)0.0241(2)
H4A0.585(2)0.8522(10)0.0100(10)0.036*
H4B0.5001(19)0.8584(11)−0.1071(10)0.036*
O50.25526(12)0.97162(8)−0.10987(9)0.0257(2)
H5A0.221(2)0.9309(9)−0.0903(17)0.039*
H5B0.196(2)1.0121(9)−0.1184(19)0.039*
C90.62874(16)0.87075(9)0.31850(11)0.0217(3)
C100.70424(18)0.79877(9)0.38683(12)0.0263(3)
H100.72040.75030.35420.032*
C110.75581(17)0.79852(10)0.50356(11)0.0273(3)
H110.80670.75010.54850.033*
C120.73178(18)0.87002(9)0.55331(12)0.0261(3)
C130.65422(18)0.94148(9)0.48438(12)0.0291(3)
H130.63650.98960.51680.035*
C140.60319(17)0.94206(9)0.36874(12)0.0268(3)
H140.55130.99040.32390.032*
C150.58610(16)0.87520(9)0.19539(11)0.0215(3)
C160.7845(2)0.87454(11)0.67937(13)0.0396(4)
H16A0.84520.92730.71200.048*
H16B0.68930.87800.68390.048*
Co20.00001.00000.00000.01894(11)
O60.20139(14)0.84480(7)0.18122(9)0.0340(3)
O70.00257(12)0.93662(7)0.13624(8)0.0254(2)
O80.35407(14)0.80992(7)0.74756(9)0.0344(3)
H8A0.33800.75120.74080.052*
O90.07394(13)0.88217(7)−0.04228(9)0.0261(2)
H9A0.116(2)0.8560(11)0.0198(10)0.040*
H9B0.017(2)0.8502(10)−0.0971(11)0.039*
O10−0.24270(12)0.96813(7)−0.10997(9)0.0253(2)
H10A−0.282(2)0.9312(10)−0.0888(17)0.038*
H10B−0.300(2)1.0108(9)−0.1268(19)0.038*
C10.13634(17)0.87290(9)0.32336(11)0.0225(3)
C20.27268(18)0.83125(9)0.41126(12)0.0292(3)
H20.34650.80780.39570.035*
C30.2997(2)0.82429(10)0.52167(13)0.0313(3)
H30.39170.79660.57950.038*
C40.19044(18)0.85846(9)0.54631(12)0.0262(3)
C50.05240(18)0.89816(10)0.45795(12)0.0288(3)
H5−0.02330.91970.47280.035*
C60.02630(17)0.90594(10)0.34837(12)0.0276(3)
H6−0.06590.93360.29060.033*
C70.11252(16)0.88439(9)0.20573(11)0.0218(3)
C80.2183(2)0.85791(11)0.66624(12)0.0344(4)
H8C0.23120.91680.69340.041*
H8B0.12370.83440.66200.041*

Source of materials

The title compound was synthesized by mixing 0.761 g (0.5 mmol) 4-hydroxymethylbenzoic acid, 0.146 g (0.5 mmol) Co(NO3)2⋅6 H2O, 12 mL ethyl alcohol absolute and 6 mL H2O in a 50 mL beaker. After all the raw materials were dissolved, triethylamine was added dropwise to adjust the pH to 6. Then waiting for the solvent evaporate, red rod crystals were separated out with 79% yield after about 20 days. Elemental analysis calculated for C16H22O10Co: C 44.35, H 5.08, O 36.93%;

found C 44.42, H 5.10, O 36.91%. IR spectrum (cm−1, KBr pellet): 3284(s), 1611(m), 1529(s), 1446(w), 1383(s), 1203(w), 1047(s), 987(w), 765(s), 501(m).

Experimental details

H-atoms attached to carbon were refined using a riding model implemented in the SHELXL program [2]. H-atoms attached to oxygen were freely refined subject to distance restraints and Uiso constraints, with the exception of hydroxy H8A, whose coordinates were constrained to ride on the parent atom.

The structure was refined in space group P21/c rather than in P21/n, even though the latter leads to a beta angle closer to 90°, to enable a comparison with the isomorphous structure of the Ni(II) analogue [4]. Strong pseudo-translational symmetry is observed in the structure for 92% of non-H atoms.

Comment

Cobalt complexes play an important role in the development of functional materials because of their catalytic properties and their excellent optical and magnetic properties. Studies have shown that cobalt complexes have active performance in the fields of catalytic chemistry, biochemistry, and analytical chemistry [4], [5], [6]. As a rigid ligand, aromatic carboxylic acids facilitate the construction of specific morphological and functional coordination compounds [7]. The study of aromatic carboxylic acid cobalt complexes is of great significance in the field of material chemistry.

In the crystal structure of the title compound there are two halves of the titled molecules existing in the asymmetric unit with the metal cations sitting on inversion centres. Each cation adopts a distorted octahedral coordination configuration, and is coordinated to four water molecules and to two carboxylate oxygen atoms, with O4(water) and its symmetry equivalent [O10(water) and its symmetry equivalent for the second molecule in the asymmetric unit] occupying the axial positions. In the complex, the Co1—O2 bond length is 2.0789(10) Å, the Co1—O5 bond length is 2.1926(11) Å, the Co1—O4 bond length is 2.1196(10) Å, and the Co2—O10 bond length is 2.0896(10) Å, the bond length of Co2—O7 is 2.0911(10) Å, and the length of the Co2—O9 bond is 2.1596(11) Å, which is longer than that reported in [8], [9], [10] and in the isomorphous Ni(II) analogue [11]. The O2—Co1—O2 bond angle is 180.0° as defined by symmetry, the O2—Co1—O5 bond angle is 89.83(4)°, the O2—Co1—O4 bond angle is 90.44(4)°, and the O5—Co1—O4 bond angle is 90.76(4)°, O10—Co2—O7 bond angle is 89.83(4)°, O10—Co2—O9 bond angle is 91.38(4)°, O7—Co2—O9 bond angle is 89.50(4)°, the remaining bond lengths and angles are all within the normal range. The hydroxy groups and the four coordinated water molecules act as the hydrogen-bonding donors and acceptors giving rise to a complex three-dimensional hydrogen-bonded network is formed.

Acknowledgements

This work is supported by the Hubei Provincial Key Laboratory of Green Materials for Light Industry and Collaborative Innovation Center of Green Light-weight Materials and Processing (No. 201907A02), Hubei University of Technology, the Students Platform for Innovation and Entrepreneurship Training Program of Hubei University of Technology (no. 201910500106).

References

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Received: 2019-09-03
Accepted: 2019-10-24
Published Online: 2019-11-14
Published in Print: 2020-02-25

©2019 Haixia Pang et al., published by De Gruyter, Berlin/Boston

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

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  71. The crystal structure of [(tetra-μ2-2,6-difluorobenzoato-κ2O:O′)-bis-(2,6-difluorobenzoato-κ2O:O′)-bis-(1,10-phenanthroline-κ2N:N′)]dierbium(III) C66H34N4O12F12Er2
  72. Crystal structure of bis(3-chloro-N-(1-(pyrazin-2-yl)ethylidene)benzohydrazonato-k3N,N′,O)nickel(II), C26H20N8O2Cl2Ni
  73. Crystal structure of (E)-3-(3-(5-methyl-1-phenyl-1H-1,2,3-triazol-4-yl)-1-phenyl-1H-pyrazol-4-yl)-1-phenylprop-2-en-1-one, C27H21N5O
  74. Crystal structure of (E)-N′-((4-aminophenyl)sulfonyl)-N,N-dimethylformimidamide, C9H13N3O2S
  75. Crystal structure of η6-p-cymene-iodido-(N-isopropyl-1-(pyridin-2-yl)methanimine-κ2N,N′)ruthenium(II) hexafluorophosphate(V), C19H26IN2F6Ru
  76. Crystal structure of 6-iodo-3-phenyl-2-propylquinazolin-4(3H)-one, C17H15IN2O
  77. Low temperature redetermination of the crystal structure of catena-poly[[tri-4-fluorobenzyltin(IV)]μ2-pyridine-4-carboxylato-κ2N:O], {C27H22F3NO2Sn}n
  78. Crystal structure of bis(2-propyl-1H-benzo[d]imidazol-3-ium) tetrachloridozincate(II), C10H13Cl4N2Zn
  79. The crystal structure of (Z)-3-hydrazono-5-nitroindolin-2-one – dimethyl sulfoxide (1/1), C8H6N4O3
  80. Crystal structure of bis-[N-(1-pyrazin-2-yl-ethylidene)-cyanoacetic acid-hydrazonato-κ3O,N,N′)]-zinc(II), C18H16N10O2Zn
  81. Crystal structure and photochromism of 1-(2,5-dimethyl-3-thienyl)-2-[2-methyl-5-(benzaldoxime)-3-thienyl] perfluorocyclopentene, C23H17F6NOS2
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