Home Physical Sciences Crystal structure of poly[dimethanol-κ1O-(µ2-(E)-2-((2-oxidobenzylidene)amino)acetato)-(µ3-(E)-2-((2-oxidobenzylidene)amino)acetato)dicadmium(II)], C20H22Cd2N2O8
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Crystal structure of poly[dimethanol-κ1O-(µ2-(E)-2-((2-oxidobenzylidene)amino)acetato)-(µ3-(E)-2-((2-oxidobenzylidene)amino)acetato)dicadmium(II)], C20H22Cd2N2O8

  • Xiao-Yu Guo ORCID logo , Yun-Chao Liu and Peng-Hui Yin ORCID logo EMAIL logo
Published/Copyright: August 26, 2022

Abstract

C20H22Cd2N2O8, monoclinic, P21/c (no. 14), a = 13.131(3) Å, b = 8.2018(16) Å, c = 20.973(4) Å, β = 103.59(3)°, V = 2195.5(8) Å3, Z = 4, R gt (F) = 0.0260, wR ref (F 2) = 0.0609, T = 293(2) K.

CCDC no.: 2183711

A part of the title 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: Yellow prism
Size: 0.23 × 0.21 × 0.21 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 1.99 mm−1
Diffractometer, scan mode: Rigaku Saturn, ω
θ max, completeness: 26.0°, >99%
N(hkl)measured, N(hkl)unique, R int: 22832, 4300, 0.027
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 4115
N(param)refined: 296
Programs: SHELX [1, 2], CrystalClear [3]
Table 2:

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

Atom x y z U iso*/U eq
Cd1 0.38743 (2) 0.59031 (2) 0.43339 (2) 0.02857 (7)
Cd2 0.16756 (2) 0.43739 (3) 0.32271 (2) 0.03002 (7)
N1 0.49929 (18) 0.7484 (3) 0.39478 (12) 0.0330 (5)
N2 −0.04881 (19) 0.7942 (3) 0.13776 (12) 0.0396 (6)
O1 0.31999 (15) 0.5571 (3) 0.32522 (10) 0.0363 (5)
O2 0.52666 (15) 0.6562 (2) 0.52312 (10) 0.0340 (5)
O3 0.62212 (17) 0.8746 (3) 0.55960 (10) 0.0460 (6)
O4 0.30615 (18) 0.8295 (3) 0.46241 (13) 0.0490 (6)
H4 0.3300 (17) 0.9249 (14) 0.4559 (19) 0.073*
O5 −0.23809 (15) 0.9677 (2) 0.06770 (9) 0.0312 (4)
O6 0.08170 (19) 0.6789 (3) 0.30385 (11) 0.0543 (7)
O7 −0.05741 (17) 0.8317 (3) 0.26685 (10) 0.0433 (5)
O8 0.2723 (2) 0.2003 (3) 0.31689 (12) 0.0571 (7)
H8 0.323 (2) 0.185 (3) 0.3503 (12) 0.086*
C1 0.5737 (2) 0.7865 (3) 0.51453 (15) 0.0332 (6)
C2 0.5721 (2) 0.8410 (4) 0.44522 (15) 0.0372 (7)
H2A 0.553056 0.955407 0.440740 0.045*
H2B 0.642100 0.830372 0.437985 0.045*
C3 0.5086 (2) 0.7631 (4) 0.33604 (15) 0.0370 (7)
H3 0.565983 0.823353 0.330660 0.044*
C4 0.4421 (2) 0.6990 (4) 0.27669 (14) 0.0338 (6)
C5 0.4701 (3) 0.7433 (4) 0.21797 (16) 0.0453 (8)
H5 0.531445 0.802034 0.220449 0.054*
C6 0.4097 (3) 0.7024 (4) 0.15751 (16) 0.0503 (9)
H6 0.429079 0.734437 0.119491 0.060*
C7 0.3196 (3) 0.6130 (4) 0.15405 (15) 0.0433 (8)
H7 0.277405 0.586051 0.113261 0.052*
C8 0.2913 (2) 0.5630 (4) 0.21016 (14) 0.0359 (7)
H8A 0.231257 0.500033 0.206444 0.043*
C9 0.3506 (2) 0.6048 (3) 0.27284 (14) 0.0302 (6)
C10 0.0164 (2) 0.7458 (4) 0.25817 (15) 0.0384 (7)
C11 0.0324 (3) 0.7200 (5) 0.18993 (17) 0.0530 (9)
H11A 0.099886 0.764928 0.187881 0.064*
H11B 0.034393 0.603764 0.181760 0.064*
C12 −0.0426 (3) 0.7739 (5) 0.07951 (16) 0.0487 (9)
H12 0.013751 0.711370 0.073912 0.058*
C13 −0.1117 (2) 0.8352 (4) 0.01933 (15) 0.0431 (8)
C14 −0.0835 (3) 0.7953 (6) −0.03923 (19) 0.0695 (13)
H14 −0.024489 0.730957 −0.036936 0.083*
C15 −0.1388 (4) 0.8465 (6) −0.09967 (18) 0.0750 (14)
H15 −0.117695 0.818192 −0.137561 0.090*
C16 −0.2267 (3) 0.9413 (5) −0.10260 (17) 0.0573 (10)
H16 −0.265132 0.978521 −0.143013 0.069*
C17 −0.2580 (3) 0.9813 (4) −0.04664 (15) 0.0426 (7)
H17 −0.317649 1.045049 −0.050170 0.051*
C18 −0.2032 (2) 0.9295 (3) 0.01570 (14) 0.0301 (6)
C19 0.1956 (3) 0.8534 (5) 0.4556 (2) 0.0612 (10)
H19A 0.158636 0.823275 0.412040 0.092*
H19B 0.182318 0.966020 0.463099 0.092*
H19C 0.172148 0.786904 0.486948 0.092*
C20 0.2450 (4) 0.0473 (5) 0.2900 (2) 0.0841 (16)
H20A 0.306548 −0.019632 0.296140 0.126*
H20B 0.195682 −0.002453 0.311291 0.126*
H20C 0.213940 0.058096 0.243955 0.126*

Source of material

All reagents used in this paper were purchased from commercial sources and used without further purification. A methanol solution (3 mL) of {[1-(2-hydroxyphenyl) methylidene]amino}acetic acid (H2L, 0.05 mmol) was added dropwise to an aqueous solution (3 mL) of CdCl2·2.5H2O (0.05 mmol). The resulting solution was placed in a 25 mL Teflon-lined stainless steel reactor, which was sealed and heated to 353 K for 72 h. After the mixture was cooled to room temperature at a rate of 5 K h−1, yellow crystals of the title compound were obtained (yield 26%, based on Cd).

Experimental details

Hydrogen atoms bound to C atoms were positioned geometrically and refined as riding atoms, with C–H = 0.93 Å (CH, aromatic) or 0.96 Å (CH3) or 0.97 Å (CH2). Hydrogen atoms on CH3OH were found according to the residual electron-density peaks with O–H = 0.866(9) Å(O4–H4) or 0.858(9) Å(O8–H8). H atoms were refined with U iso(H) = 1.2 U eq(C) and 1.5 U eq(C, O) for methyl H atoms and OH.

Comment

Schiff-bases are considered as good ligands and have been widely used in the synthesis of new coordination compounds (CPs) [4, 5]. Among the reported literatures, amino acid Schiff bases and their corresponding CPs have received much attention for their medicinal and pharmaceutical applications, especially for their antibacterial and anticancer activity [6], [7], [8]. The above results stimulated our research interest on the N-salicylideneglycinato-metal CPs. Up to now, a series of N-salicylideneglycinato-metal CPs have been synthesized and characterized, such as Cr(III), Ni(II), Cu(II) and zinc(II) CPs [8], [9], [10]. In order to further enrich the categories and numbers of CPs based on this ligand, we continue to use {[1-(2-hydroxyphenyl) methylidene]amino}acetic acid (H2L) as ligand to react with CdCl2·2.5H2O and obtained the new CP [Cd2L2(CH3OH)2].

The asymmetric unit of the title structure consists of two Cd(II) cations, two 2-((2-oxidobenzylidene)amino)acetate anions (L2−) and two methanol molecules. Each Cd1 cation is six-coordinated and located in a distorted octahedral CdNO5 coordination environment formed by one N atom (N1) and four O atoms (O1, O2, O2#2 and O5#1) from two L2− anions and by one methanol molecule (O4). Each Cd2 cation is also six-coordinated by N2#1, O1, O5#1, O6 and O7#1 from two L2− anions together with one methanol molecule (O8), exhibiting a deformed CdNO5 octahedral geometry. The bond lengths of Cd–O are in the range of 2.1990(19)–2.402(2) Å and the bond lengths of Cd–N are 2.248(2) and 2.260(3) Å, respectively. It is known from the literature that these bond lengths are similar to those reported in other Cd(II) complexes [11], [12], [13]. There are two kinds of crystallographically independent L2− anion ligands. One L2− anion ligand coordinates to Cd(II) cations in tridentate mode, while the other L2- anion ligand coordinates to Cd(II) cations in tetradentate mode. Cd1 and Cd2 cations are furthermore connected by L2- anion ligands (see the figure) to form a two-dimensional layered structure with Cd1–Cd1 distance of 3.8547(12) Å, Cd2–Cd2 distance of 6.2591(13) Å and Cd1–Cd2 distance of 3.4854(11) Å. In addition, there are O–H⃛O hydrogen bonds between hydroxyl and carboxylate groups. Adjacent layers are further packed through van der Waals forces, resulting in a three-dimensional architecture.


Corresponding author: Peng-Hui Yin, Pharmacy College, Henan University of Chinese Medicine, Zhengzhou 450046, Henan, P. R. China, E-mail:

Funding source: Science and Technology Innovation Talents of Henan University of Chinese Medicine 10.13039/100017634

Award Identifier / Grant number: 2014XCXRC04

Funding source: Science and Technology Department of Henan Province 10.13039/501100011447

Award Identifier / Grant number: 2014KYYWF–QN03

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

  2. Research funding: This study was supported by Science and Technology Innovation Talents of Henan University of Chinese Medicine (2014XCXRC04) and Science and Technology Department of Henan Province (2014KYYWF–QN03).

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

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Received: 2022-04-04
Accepted: 2022-07-04
Published Online: 2022-08-26
Published in Print: 2022-12-16

© 2022 the author(s), 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 bis(tricarbonyl)-{(S)-(tert-butoxycarbonyl)(1-methoxy-1-oxo-3-sulfido-k2 S:S′-propan-2-yl)amido-k2N:N′}diiron(I) (Fe—Fe), C15H15Fe2NO10S
  59. Crystal structure of (E)-3-((4-chlorophenyl)thio)-4-hydroxypent-3-en-2-one, C11H11ClO2S
  60. The crystal structure of (E)-3′,6′-bis(diethylamino)-2-((5-(diethylamino)-2-hydroxybenzylidene)amino)spiro[isoindoline-1,9′-xanthen]-3-one, C39H45N5O3
  61. The crystal structure of 2-(4-methoxynaphthalen-1-yl)-4H-chromen-4-one, C20H14O3
  62. The crystal structure of trans-dichlorido-(ethylenediamine-κ 2 N,N′)-bis(triphenylphosphine-κ 1 P)ruthenium(II), C38H38Cl2N2P2Ru
  63. The double polymeric chain of catena-poly[(μ2-6-bromopyridine-3-carboxylato-κ2 O,O′) (6-bromopyridine-3-carboxylato-κ2 O,O′) (μ2-1,2-bis(4-pyridyl)ethylene-κ2 N:N′)cobalt(II)], C24H16CoBr2N4O4
  64. The crystal structure of tert-butyl 2-(4-(12-bromo [2.2]paracyclophanyl)carbamoyl)pyrrolidine-1-carboxylate, C26H31BrN2O3
  65. The crystal structure of (Z)-2-(2,3-dimethoxybenzylidene)naphtho[1,2-b]furan-3(2H)-one, C21H16O4
  66. Crystal structure of 2-hydroxy-1-tosylindolin-3-yl- 2-naphthoate, C26H21N1S1O5
  67. The crystal structure of 1-methyl-N-(1-methyl-1H-imidazole-2-carbonyl)-1H-imidazole-2-carboxamide, C10H11N5O2
  68. The crystal structure of (E)-2-((5-bromo-2-hydroxybenzylidene)amino)-3′,6′-bis(ethylamino)-2′, 7′-dimethylspiro[isoindoline-1,9′-xanthen]-3-one, C33H31BrN4O3
  69. The crystal structure of dimethanol-5,15-diphenylporphyrin-21,23-diido-κ4 N,Nʹ,Nʺ,Nʹʺ-manganese(III) trans-dicyanido-bis(acetylacetonato-κ2O,Oʹ)ruthenium(III), C46H42N6O6RuMn
  70. Crystal structure of 1,4,8,11-tetraazacyclotetradecane-1,8-diium bis(3,5-dicarboxybenzoate), C28H36N4O12
  71. Bifurcated halogen bonds in the crystal structure of 2,2′-bi(1,8-naphthyridine)—1,4-diiodotetrafluorobenzene (1/1), C22H10F4I2N4
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