Startseite Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-[(4-pyridinylmethyl)amino]benzoato-κ2N:O)cobalt(II)]–1,2bi(4-pyridyl)ethene–water (1/1/1), C50H50N8O8Co
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Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-[(4-pyridinylmethyl)amino]benzoato-κ2N:O)cobalt(II)]–1,2bi(4-pyridyl)ethene–water (1/1/1), C50H50N8O8Co

  • Liu Guang-Zhen ORCID logo EMAIL logo und Ya-Di Li
Veröffentlicht/Copyright: 31. Mai 2022

Abstract

C50H50N8O8Co, triclinic, P 1 , a = 9.2920(4) Å, b = 11.3648(5) Å, c = 11.9954(4) Å, α = 96.478(3)°, β = 104.766(3)°, γ = 103.901(4)°, V = 1168.40(8) Å3, Z = 1, R gt (F) = 0.0393, wR ref (F2) = 0.1431, T = 293(2) K.

CCDC no.: 2172873

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: Block, clear pinkish pink
Size: 0.35 × 0.27 × 0.22 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.43 mm−1
Diffractometer, scan mode: SuperNova, ω-scans
θmax, completeness: 25.5°, >99%
N(hkl)measured, N(hkl)uniqueRint: 13006, 4330, 0.025
Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 3900
N(param)refined: 308
Programs: CrysAlisPRO [1], OLEX2 [2], SHELX [3, 4]
Table 2:

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

x y z Uiso*/Ueq
Co1 0.5000 0.5000 0.0000 0.02821 (16)
O1 0.63176 (17) 0.56042 (14) 0.17568 (11) 0.0364 (4)
O1W 0.51531 (17) 0.32115 (14) 0.01855 (12) 0.0368 (4)
H1WA 0.4978 0.3047 0.0832 0.055*
H1WB 0.4479 0.2929 −0.0480 0.055*
O2 0.6761 (2) 0.76450 (15) 0.19879 (13) 0.0470 (4)
N3 1.0511 (2) 0.7185 (2) 0.71006 (15) 0.0422 (5)
H3 1.1003 0.7931 0.7451 0.051*
N4 0.7093 (2) 0.53415 (17) 0.94256 (14) 0.0349 (4)
C1 0.6914 (2) 0.6674 (2) 0.23659 (17) 0.0311 (5)
C2 0.7840 (2) 0.6792 (2) 0.36118 (16) 0.0316 (5)
C3 0.8698 (3) 0.7945 (2) 0.42957 (18) 0.0385 (5)
H3A 0.8691 0.8650 0.3972 0.046*
C4 0.9555 (3) 0.8054 (2) 0.54411 (18) 0.0408 (5)
H4 1.0120 0.8833 0.5877 0.049*
C5 0.9595 (2) 0.7019 (2) 0.59640 (16) 0.0336 (5)
C6 0.8716 (2) 0.5864 (2) 0.52925 (17) 0.0344 (5)
H6 0.8704 0.5160 0.5622 0.041*
C7 0.7860 (2) 0.5761 (2) 0.41336 (17) 0.0336 (5)
H7 0.7288 0.4984 0.3697 0.040*
C8 1.0720 (2) 0.6216 (2) 0.77610 (18) 0.0406 (6)
H8A 1.1733 0.6489 0.8339 0.049*
H8B 1.0692 0.5493 0.7233 0.049*
C9 0.9487 (2) 0.5868 (2) 0.83785 (17) 0.0324 (5)
C10 0.9406 (3) 0.6702 (2) 0.92759 (19) 0.0433 (6)
H10 1.0157 0.7459 0.9548 0.052*
C11 0.8203 (3) 0.6404 (2) 0.97677 (19) 0.0425 (6)
H11 0.8169 0.6978 1.0371 0.051*
C12 0.7209 (3) 0.4524 (2) 0.8594 (2) 0.0449 (6)
H12 0.6465 0.3763 0.8354 0.054*
C13 0.8382 (3) 0.4753 (2) 0.8071 (2) 0.0438 (6)
H13 0.8423 0.4144 0.7503 0.053*
N1 0.4762 (2) 0.2647 (2) 0.22787 (15) 0.0430 (5)
N2 0.7694 (3) 0.0202 (2) 0.95472 (17) 0.0549 (6)
C14 0.5692 (3) 0.1954 (2) 0.26182 (19) 0.0421 (6)
H14 0.6120 0.1638 0.2072 0.050*
C15 0.6071 (3) 0.1669 (2) 0.37156 (19) 0.0436 (6)
H15 0.6739 0.1181 0.3898 0.052*
C16 0.5448 (2) 0.2118 (2) 0.45536 (18) 0.0373 (5)
C17 0.4478 (3) 0.2842 (3) 0.4206 (2) 0.0486 (6)
H17 0.4026 0.3163 0.4733 0.058*
C18 0.4175 (3) 0.3092 (3) 0.3088 (2) 0.0534 (7)
H18 0.3531 0.3595 0.2885 0.064*
C19 0.5745 (3) 0.1825 (2) 0.57362 (18) 0.0422 (6)
H19 0.5145 0.2041 0.6194 0.051*
C20 0.6786 (3) 0.1284 (3) 0.6200 (2) 0.0483 (6)
H20 0.7404 0.1100 0.5744 0.058*
C21 0.7088 (3) 0.0935 (2) 0.73633 (19) 0.0419 (5)
C22 0.6282 (3) 0.1165 (2) 0.81535 (19) 0.0427 (5)
H22 0.5508 0.1559 0.7964 0.051*
C23 0.6643 (3) 0.0802 (2) 0.9215 (2) 0.0500 (6)
H23 0.6114 0.0989 0.9742 0.060*
C24 0.8441 (4) −0.0036 (3) 0.8777 (2) 0.0612 (8)
H24 0.9175 −0.0465 0.8977 0.073*
C25 0.8189 (3) 0.0316 (3) 0.7706 (2) 0.0574 (7)
H25 0.8760 0.0139 0.7209 0.069*
O2W 0.8011 (3) 1.01111 (17) 0.19379 (15) 0.0600 (5)
H2WA 0.7770 0.9391 0.2093 0.090*
H2WB 0.7887 1.0059 0.1205 0.090*

Source of material

All chemicals were of reagent grade and used as received without further purification. The mixture of 4-[(4-pyridinylmethyl)amino]benzoic acid (H2paba, 11.4 mg, 0.05 mmol), 1,2-bi(4-pyridyl)ethene (bpe, 9.1 mg, 0.05 mmol), Co(OAc)2.4H2O (49.8 mg, 0.2 mmol) and H2O (6 mL) was placed in a 23 mL Teflon-lined autoclave at 393 K for four days, then cooled to room temperature. Pink block crystals were obtained in ca. 81.6% yield. Elemental analysis calcd. (%) for C50H50N8O8Co: C, 63.22; H, 5.31; N, 11.80. Found: C, 63.18; H, 5.42; N, 11.69.

Experimental details

Using Olex2 [2], the structure was solved with the ShelXT [3] structure solution program and refined with the ShelXL [4] refinement package. Hydrogen atoms were placed in their geometrically idealized positions and constrained to ride on their parent atoms. The Uiso of the H-atoms were constrained to 1.2 times Ueq of their bonding carbon and nitrogen atoms and 1.5 times Ueq for the hydrogen atoms at water.

Discussion

The metal coordination polymers (CPs) have been put much attention as functional materials because of their applications in a wide variety of fields in general [5], and especially for Co(II) compounds [69]. Among the many factors influencing the synthesis and properties of CPs, the choice of ligands and metal ions plays key role in the fabrications of the desired structures [10]. Usually mixed-ligands based on carboxylate and N-donor Ligands are widely used in the synthesis of CPs [11], [12]. In recent years, lots of CPs with controlled chemical and physical properties by the Schiff-base ligands have been reported, because the type ligand with O,N-bifunctional group has multiple coordination points and various coordination modes. Up to now, to the best of our knowledge, the CPs base on the 4-[(4-pyridinylmethyl)amino]benzoic acid (Hpaba) are still rare [13, 14]. In this paper, we selected the Schiff-base H2paba ligand, 1,2-bi(4-pyridyl)ethene (bpe) and cobalt acetate to obtain the title compound.

Single-crystal X-ray diffraction reveals that title compound belongs to in triclinic crystal system, space group P 1 and features a one-dimensional chain structure. The asymmetry unit contains half a Co(II) ion, one paba anion, one coordinated water molecule, one guest bpe molecule and one free water molecule, as shown in the Figure. (A: 1 − x, 1 − y, −z; B: 1 − x, 1 − y, 1 − z; C: x, y, −1 + z). The Co(II) atom is six-coordinated by two carboxylate oxygen atoms from two symmetry-related paba anions and two oxygen atoms from two symmetry-related coordinated water molecules in the equatorial plane, plus two nitrogen atoms from two paba anions in the axial positions to generate a distorted octahedral [CoN2O4] arrangement. The Co–O1 bond lengths are 2.0894(13) Å, The Co–O1W bond lengths are to 2.1037(15) Å, whilst the Co–N4 bond lengths are 2.1883(16) Å, respectively. The bond angles around the central Co(II) ion are respectively in the range of 88.15(6)–180.0° for O–Co–O, 88.65(6)–91.35(6)° for O–Co–N, and 180.0° for N–Co–N. The carboxyl group of one paba anion adopt monodentate coordination mode. The adjacent Co(II) centers are bridged by paba anions to form a 1D chain structure along the c direction with the Co⋯Co distance of 11.9954(4) Å. As a result of the presence of coordinated water molecule (O1W), free water molecule (O2W) and free bpe molecule in title compound, there are five kinds of hydrogen bonds. Firstly, there is the oxygen atom in coordinated water as donor and the carboxylate oxygen atoms from paba anions as acceptors (O(1W)–H(1WB)⋯O(1): d = 3.013(2) Å; O(1W)–H(1WB)⋯O(2): d = 2.672(2) Å). Secondly, it is between a coordinated water moleclue as donor and the nitrogen atom as an acceptor from free bpe molecule (O(1W)–H(1WA)⋯N(1): d = 2.751(2) Å). Thirdly, it is between the nitrogen atom N3 of paba anion and the free water O2W atom (N3–(H3)⋯O2W: d = 3.004(3) Å). Fourthly, there is the free water O2W as donor and the carboxylate oxygen atoms from paba anions as an acceptor (O(2W)–H(2WA)⋯O(2): d = 2.778(3) Å). Fifthly, it is between the free water O2W and the nitrogen atom N2 from free bpe molecule (O(2W)–H(2WB)⋯N(2): d = 2.823(3) Å). The adjacent one-dimensional chains are linked together by the hydrogen bond interactions to form a three-dimensional supramolecular structure. At the same time, there exists strong interchain face-face π–π interactions between two pyridine rings of free bpe molecules. The centroid-centroid distance and the dihedral angle between two pyridyl rings are 3.6837(2) Å and 10.0° respectively.


Corresponding author: Liu Guang-Zhen, College of Chemistry and Chemical Engineering, LuoYang Normal University, Luoyang, Henan 471934, P. R. China, E-mail:

Award Identifier / Grant number: 21571093

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: This work was supported by the National Natural Science Foundation of China (No. 21571093).

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2022-03-16
Accepted: 2022-05-16
Published Online: 2022-05-31
Published in Print: 2022-08-26

© 2022 Liu Guang-Zhen and Ya-Di Li, published by De Gruyter, Berlin/Boston

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

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  58. Crystal structure of 2-(1H-pyrazol-3-yl-κN)pyridine-κN-bis(2-(2,4-difluorophenyl)pyridinato-κ2C,N)iridium(III) sesquihydrate, C30H18F4IrN5·1.5[H2O]
  59. Crystal structure of 2-(2-hydroxy-5-nitrophenyl)-5-methyl-1,3-dioxane-5-carboxylic acid, C12H13N1O7
  60. The crystal structure of 1,2-bis(pyridinium-4-yl)ethane diperchlorate, C12H14N2·2ClO4 – a second polymorph
  61. The crystal structure of [(1,10-phenantroline-κ2N,N′)-bis(6-phenylpyridine-2-carboxylato-κ2N,O)manganese(II)] monohydrate, C36H26N4O5Mn
  62. Crystal structure of 1,2-bis(2,2,3,3,5,5,5-heptamethyl-1,1,4,4- tetrakis(trimethylsilyl)pentasilan-1-yl)ditellane, C38H114Si18Te2
  63. Crystal structure of 1,2-bis(2,4-dinitro-1H-imidazol-1-yl)ethane – dimethylformamide (1/1), C11H13N9O9
  64. Crystal structure of (Z)-3-((tert-butylamino) methylene)-2-(2-hydroxynaphthalen-1-yl) chroman-4-one, C24H23NO3
  65. Synthesis and crystal structure of (E)-1-(4-(((E)-3-(tert-butyl)-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-ethyl oxime, C21H26N2O2
  66. Crystal structure of the double salt bis(5-amino-1,2,4-triazol-4-ium-3-yl)methane hydrogen oxalate hemioxalate, C8H11N8O6
  67. Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-[(4-pyridinylmethyl)amino]benzoato-κ2N:O)cobalt(II)]–1,2bi(4-pyridyl)ethene–water (1/1/1), C50H50N8O8Co
  68. Crystal structure of 3-(3-bromophenyl)-1′,3′-dimethyl-2′H,3H,4H-spiro[furo[3, 2-c]chromene-2,5′-pyrimidine]-2′,4,4′,6′(1′H,3′H) tetraone, C22H15BrN2O6
  69. The crystal structure of poly[aqua-(μ2-4,4′- bis(imidazolyl)biphenyl-κ2N:N′)-(μ2-3-nitrobenzene-1,2-dicarboxylato-κ2O:O′)]copper (II) hydrate, C26H21N5O8Cu
  70. The crystal structure of bis(4-(6-carboxy-8-ethyl-3-fluoro-5-oxo-5,8-dihydro-1,8-naphthyridin-2- yl)piperazin-1-ium) adipate tetrahydrate, C36H52F2N8O14
  71. Synthesis and crystal structure of poly[aqua(μ4-(1R,2S,4R)-4-hydroxy-1-((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)pyrrolidin-1-ium-2-carboxylate-κ4O:O′:O″:O‴)sodium(I)] monohydrate, C21H22NNaO12S
  72. Crystal structure of chlorido-(η6-toluene)(2,2′-bipyridine-κ2N,N′)ruthenium(II) hexafluorophosphate, C17H16ClN2RuPF6
  73. The crystal structure of (R)-6-hydroxy-8-methoxy-3-methylisochroman-1-one, C11H12O4
  74. Crystal structure of catena-poly[(5,5,7,12,12,14-hexamethyl -1,4,8,11-tetraazacyclotetradecane- κ4N,N′,Nʺ,N‴)nickel(II)-(μ2-perchlorato-κ2O:O′)] 3,5-dicarboxybenzoate – methanol (1/2), C27H49ClN4NiO12
  75. The crystal structure of 4-(chloromethyl)benzonitrile, C8H6ClN
  76. The crystal structure of dimethylammonium 8-[(7,9-dioxo-6,10-dioxaspiro[4.5]decan-8-ylidene)methyl]-9-oxo-6,10-dioxaspiro[4.5]dec-7-en-7-olate, C19H25NO8
  77. Crystal structure of (2R,3S,4S,5R,6S)-2-(acetoxymethyl)-6-((1-acetyl-5-bromo-4-chloro-1H-indol-3-yl)oxy)tetrahydro-2H-pyran-3,4,5-triyl triacetate hemihydrate C24H25BrClNO11
  78. The crystal structure of the co-crystal tetrakis[2-(tris(4-methoxyphenyl)stannyl)ethyl]silane – tetrahydrofuran – toluene – tetrahydrofurane (1/1/1), C103H116O13SiSn4
  79. Crystal structure of methyl 3-(1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)propanoate, C16H13NO4
  80. Crystal structure of ethyl (Z)-3-amino-2-cyano-3-(2-oxo-2H-chromen-3-yl)acrylate, C15H12N2O4
  81. Crystal structure of methyl 2-(1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)acetate, C15H11NO4
  82. Crystal structure of catena-poly[diaqua-bis(μ2-1,3-di(1H-imidazol-1-yl)propane-κ2N:N′)cobalt(II)] tetrafluoroterephthalate, C26H28N8O6F4Co
Heruntergeladen am 7.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2022-0127/html
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