Crystal structure of bis(μ2-benzoato-k2O:O′)-bis(μ2-benzoato-k3O,O′:O′)dinitrato-k2O,O′-bis(phenanthroline-k2
N,N′)dierbium(III), C52H36Er2N6O14

Zhang Li; Yu Hai-yan; Wang Ying-lei; Li Ru-lin; Cao Ying-han

doi:10.1515/ncrs-2022-0169

Open Access Published by De Gruyter (O) July 6, 2022

Crystal structure of bis(μ2-benzoato-k²O:O′)-bis(μ2-benzoato-k³O,O′:O′)dinitrato-k²O,O′-bis(phenanthroline-k² N,N′)dierbium(III), C₅₂H₃₆Er₂N₆O₁₄

Zhang Li , Yu Hai-yan , Wang Ying-lei , Li Ru-lin and Cao Ying-han

From the journal Zeitschrift für Kristallographie - New Crystal Structures

https://doi.org/10.1515/ncrs-2022-0169

Abstract

C₅₂H₃₆Er₂N₆O₁₄, triclinic, P 1 ‾ (no. 2), a = 10.6499(5) Å, b = 11.0111(5) Å, c = 11.0380(6) Å, α = 85.030(4)°, β = 81.502(4)°, γ = 68.925(4)°, V = 1193.77(11) Å³, Z = 2, R _gt(F) = 0.0263, wR _ref(F ²) = 0.0592, T = 150.0 K.

CCDC no.: 2180392

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:	Pink block
Size:	0.23 × 0.15 × 0.12 mm
Wavelength:	Mo Kα radiation (0.71073 Å)
μ:	3.57 mm⁻¹
Diffractometer, scan mode:	Xcalibur, ω
θ _max, completeness:	26.4°, >99%
N(hkl)_measured, N(hkl)_unique, R _int:	8402, 4875, 0.023
Criterion for I _obs, N(hkl)_gt:	I _obs > 2 σ(I _obs), 4318
N(param)_refined:	334
Programs:	CrysAlis^PRO [1], Olex2 [2], SHELX [3, 4]

Table 2:

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

Atom	x	y	z	U _iso*/U _eq
Er1	0.62749 (2)	0.49462 (2)	0.35076 (2)	0.02363 (6)
O1	0.7367 (2)	0.3681 (2)	0.5096 (2)	0.0306 (6)
O2	0.4977 (3)	0.3730 (2)	0.4412 (2)	0.0308 (6)
O3	0.5891 (2)	0.3603 (2)	0.6743 (2)	0.0285 (6)
O4	0.3486 (3)	0.3222 (2)	0.5738 (2)	0.0328 (6)
O5	0.7569 (3)	0.3118 (3)	0.2250 (3)	0.0362 (6)
O6	0.5561 (3)	0.4124 (3)	0.1753 (3)	0.0373 (6)
N1	0.8757 (3)	0.4901 (3)	0.3003 (3)	0.0278 (7)
N2	0.6678 (4)	0.3224 (3)	0.1541 (3)	0.0344 (8)
N3	0.6804 (3)	0.6131 (3)	0.1519 (3)	0.0265 (7)
C1	0.4309 (3)	0.2986 (3)	0.4786 (3)	0.0246 (8)
O7	0.6936 (3)	0.2469 (3)	0.0713 (3)	0.0552 (9)
C2	0.7051 (4)	0.3212 (3)	0.6129 (3)	0.0252 (8)
C3	0.9061 (4)	0.5616 (3)	0.2027 (3)	0.0277 (8)
C4	0.8035 (4)	0.6271 (3)	0.1241 (3)	0.0273 (8)
C5	0.5896 (4)	0.6686 (4)	0.0755 (4)	0.0354 (9)
H5	0.506615	0.656583	0.092396	0.042*
C6	0.4526 (4)	0.1803 (3)	0.4090 (3)	0.0287 (8)
C7	0.8142 (4)	0.2112 (3)	0.6677 (3)	0.0266 (8)
C8	0.9712 (4)	0.4306 (4)	0.3704 (4)	0.0382 (10)
H8	0.950884	0.381181	0.437978	0.046*
C9	0.8331 (4)	0.7003 (4)	0.0208 (4)	0.0398 (10)
C10	0.7931 (4)	0.1676 (4)	0.7871 (4)	0.0353 (9)
H10	0.709946	0.206551	0.833838	0.042*
C11	1.0361 (4)	0.5720 (4)	0.1733 (4)	0.0353 (9)
C12	0.5699 (4)	0.1235 (4)	0.3314 (4)	0.0406 (10)
H12	0.638831	0.157971	0.321832	0.049*
C13	0.7317 (5)	0.7601 (4)	−0.0551 (4)	0.0501 (12)
H13	0.747657	0.810603	−0.123463	0.060*
C14	1.1016 (4)	0.4370 (4)	0.3494 (4)	0.0450 (11)
H14	1.165146	0.394487	0.402711	0.054*
C15	0.3514 (5)	0.1272 (4)	0.4245 (4)	0.0399 (10)
H15	0.273272	0.163472	0.478704	0.048*
C16	0.6094 (5)	0.7438 (4)	−0.0283 (4)	0.0467 (11)
H16	0.541182	0.781887	−0.078147	0.056*
C17	1.0613 (5)	0.6472 (4)	0.0670 (4)	0.0504 (13)
H17	1.146301	0.654664	0.048146	0.060*
C18	1.1332 (4)	0.5060 (4)	0.2505 (4)	0.0456 (11)
H18	1.219982	0.509601	0.233762	0.055*
C19	0.9373 (4)	0.1497 (4)	0.5999 (4)	0.0497 (11)
H19	0.953409	0.176230	0.518666	0.060*
C20	0.8933 (5)	0.0668 (4)	0.8385 (4)	0.0483 (11)
H20	0.877347	0.038601	0.919271	0.058*
C21	0.9661 (5)	0.7073 (5)	−0.0065 (4)	0.0519 (12)
H21	0.986551	0.754128	−0.075996	0.062*
C22	0.4812 (7)	−0.0336 (4)	0.2814 (5)	0.0676 (17)
H22	0.490113	−0.104517	0.236533	0.081*
C23	1.0148 (5)	0.0091 (4)	0.7713 (5)	0.0576 (13)
H23	1.083009	−0.057440	0.806375	0.069*
C24	1.0369 (5)	0.0491 (5)	0.6516 (5)	0.0679 (16)
H24	1.119620	0.008088	0.604909	0.082*
C25	0.5850 (6)	0.0161 (4)	0.2682 (4)	0.0582 (14)
H25	0.664613	−0.023139	0.216757	0.070*
C26	0.3665 (6)	0.0207 (4)	0.3594 (5)	0.0592 (14)
H26	0.297988	−0.014347	0.368936	0.071*

Source of material

The following compounds 0.0461 g erbium nitrate hexahydrate (0.10 mmol), 0.0180 g 1,10-phenanthroline (0.10 mmol) and 0.0122 g benzoic acid (0.10 mmol) were mixed homogeneously under stirring, then placed in a 25 mL Teflon-lined stainless steel reactor, and finally heated to 120°. Seventy-two hours later, the reactor cooled naturally. Pink crystals were obtained for X-ray single-crystal diffraction test, yield 46% based on Er.

Experimental details

The structure was solved by direct methods with the SHELXS program. All H-atoms were positioned with idealized geometry and refined isotropically (U _iso(H) = 1.2 U _eq(C) and U _iso(H) = 1.2 U _eq(N)) using a riding model with C–H = 0.950 Å.

Comment

The four-component dimers of lanthanide complexes composed of lanthanide(III) cations, nitrate, benzoic acid or its derivatives, and 1,10-phenanthroline have been reported with a chemical formula [Ln₂(L)₄(phen)₂(NO₃)₂] (Ln = lanthanide(III) ions, phen = 1,10-phenanthroline, and L = benzoate or its derivatives) [5], [6], [7], [8], [9], [10], [11]. Also two analogues of erbium complexes (L = 4-acetamidobenzoate [12] and 2-fluorobenzoate [13]) and two isostructures complex (Ln = praseodymium [14] and holmium [15]) have been published elsewhere, respectively. The title complex, with the formula of [Er₂(L)₄(phen)₂(NO₃)₂] (L = benzoate) has not been reported. The title complex crystallizes in P 1 ‾ located around an inversion center (see the Figure). Consequently the asymmetric unit consists of one Er(III) ion, two benzoates, one phen, and one nitrate. The dimer is made of two asymmetric units linked by four benzoates, which adapt two coordination modes: two of them are in a μ²-k²O:O′ mode while the other two briding ligands use a μ²-k³O,O′:O mode. The distance of the two Er(III) ions is 3.929 Å. The dimers are linked together by weak non-classical hydrogen bonds C10–H10⃛O7, C16–H16⃛O7, and C17–H17⃛O7, and weak π⃛π interactions. All bond lengths are similar to the reported results of its analogues [12, 13].

Corresponding author: Zhang Li, School of Biological and Chemical Engineering, Nanyang Institute of Technology, Nanyang, Henan 473004, P. R. China, E-mail: nyistzl@163.com

Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
Research funding: None declared.
Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2022-04-03

Accepted: 2022-06-20

Published Online: 2022-07-06

Published in Print: 2022-10-26

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

Crystal structure of bis(μ2-benzoato-k²O:O′)-bis(μ2-benzoato-k³O,O′:O′)dinitrato-k²O,O′-bis(phenanthroline-k² N,N′)dierbium(III), C₅₂H₃₆Er₂N₆O₁₄

Abstract

Source of material

Experimental details

Comment

References

Journal and Issue

Articles in the same Issue

Crystal structure of bis(μ2-benzoato-k2O:O′)-bis(μ2-benzoato-k3O,O′:O′)dinitrato-k2O,O′-bis(phenanthroline-k2 N,N′)dierbium(III), C52H36Er2N6O14

Abstract

Source of material

Experimental details

Comment

References

Journal and Issue

Articles in the same Issue

Crystal structure of bis(μ2-benzoato-k²O:O′)-bis(μ2-benzoato-k³O,O′:O′)dinitrato-k²O,O′-bis(phenanthroline-k² N,N′)dierbium(III), C₅₂H₃₆Er₂N₆O₁₄