Home The crystal structure of hexakis(3-thiophenecarboxylato-κ2O,O″)-bis(1,10-phenanthroline-κ2N,N′) trimanganese(II), C54H34N4O12S6Mn3
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The crystal structure of hexakis(3-thiophenecarboxylato-κ2O,O″)-bis(1,10-phenanthroline-κ2N,N′) trimanganese(II), C54H34N4O12S6Mn3

  • Lili Zhou , Zhongyu Zhang ORCID logo EMAIL logo , Xiaoxia Men and Yaxuan Zhang
Published/Copyright: November 1, 2023

Abstract

C54H34N4O12S6Mn3, monoclinic, P21/c (no. 14), a = 11.0140(4) Å, b = 22.3222(9) Å, c = 11.2886(5) Å, β = 105.436(1)°, Z = 2, V = 2675.27(19) Å3, R gt (F) = 0.0361, wR ref (F2) = 0.0846, T = 273 K.

CCDC no.: 2248088

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, yellow
Size: 0.3 × 0.2 × 0.2 mm
Wavelength: Mo Ka radiation, l = 0.71073 Å
μ: 0.999 mm−1
Diffractometer, scan mode: Bruker APEX-II, φ and ω
θmax, completeness: 27.130°, >99.9 %
N(hkl)measured, N(hkl)unique, Rint: 18,414, 5917, 0.0212
Criterion for Iobs, N(hkl)gt: Iobs > 2σ(Iobs), 4961
N(param)refined: 415
Programs: Bruker [1], Olex2 [2]
Table 2:

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

x y z Uiso*/Ueq
Mn1 0.73967 (3) 0.40694 (2) 0.14482 (3) 0.02828 (9)
Mn2 0.5000 0.5000 0.0000 0.02615 (10)
S1 0.95691 (19) 0.67057 (8) 0.0273 (3) 0.0514 (4)
S1A 0.8134 (7) 0.6943 (3) 0.0527 (4) 0.0555 (12)
S2 0.6314 (4) 0.3550 (2) −0.4534 (3) 0.0647 (7)
S2A 0.5203 (9) 0.4195 (4) −0.4609 (7) 0.0774 (14)
S3 0.2754 (5) 0.2953 (2) 0.3461 (6) 0.0670 (10)
S3A 0.1959 (2) 0.35109 (12) 0.3206 (3) 0.0621 (6)
O1 0.87238 (17) 0.47788 (7) 0.10875 (17) 0.0467 (4)
O2 0.68980 (14) 0.51176 (6) 0.12348 (15) 0.0371 (3)
O3 0.75166 (17) 0.36587 (8) −0.03845 (14) 0.0466 (4)
O4 0.5896 (2) 0.42410 (8) −0.05724 (17) 0.0572 (5)
O5 0.57984 (15) 0.36671 (8) 0.18492 (16) 0.0451 (4)
O6 0.45650 (16) 0.44745 (7) 0.13974 (15) 0.0418 (4)
N1 0.85287 (16) 0.32868 (8) 0.23992 (16) 0.0313 (4)
N2 0.81628 (18) 0.43196 (8) 0.35117 (17) 0.0362 (4)
C1 0.8661 (2) 0.27730 (10) 0.1860 (2) 0.0415 (5)
H1 0.8329 0.2741 0.1014 0.050*
C2 0.9275 (3) 0.22775 (11) 0.2505 (3) 0.0528 (7)
H2 0.9338 0.1922 0.2096 0.063*
C3 0.9780 (3) 0.23213 (12) 0.3739 (3) 0.0538 (7)
H3 1.0200 0.1996 0.4179 0.065*
C4 0.9670 (2) 0.28546 (11) 0.4347 (2) 0.0419 (6)
C5 0.90194 (19) 0.33307 (10) 0.3635 (2) 0.0320 (5)
C6 0.8849 (2) 0.38844 (10) 0.4220 (2) 0.0342 (5)
C7 0.9374 (2) 0.39500 (13) 0.5496 (2) 0.0469 (6)
C8 0.9154 (3) 0.44940 (14) 0.6029 (3) 0.0616 (8)
H8 0.9488 0.4559 0.6867 0.074*
C9 0.8454 (3) 0.49234 (14) 0.5317 (3) 0.0630 (8)
H9 0.8295 0.5283 0.5662 0.076*
C10 0.7971 (3) 0.48216 (12) 0.4059 (2) 0.0506 (6)
H10 0.7491 0.5121 0.3583 0.061*
C11 1.0188 (3) 0.29402 (15) 0.5642 (3) 0.0576 (8)
H11 1.0623 0.2628 0.6116 0.069*
C12 1.0058 (3) 0.34603 (16) 0.6181 (3) 0.0615 (8)
H12 1.0421 0.3505 0.7020 0.074*
C13 0.7980 (2) 0.52018 (10) 0.10373 (19) 0.0336 (5)
C14 0.8332 (2) 0.58191 (9) 0.07821 (17) 0.0321 (4)
C15 0.9443 (2) 0.59671 (10) 0.05037 (19) 0.0405 (5)
H15 1.0054 0.5688 0.0450 0.049*
H15A 1.0084 0.5707 0.0444 0.049*
C16 0.8193 (11) 0.6841 (5) 0.0531 (5) 0.059 (2)
H16 0.7850 0.7223 0.0499 0.070*
C16A 0.9406 (17) 0.6615 (9) 0.032 (3) 0.056 (3)
H16A 1.0045 0.6826 0.0109 0.067*
C17 0.7578 (2) 0.63207 (11) 0.0807 (2) 0.0423 (5)
H17 0.6797 0.6315 0.0977 0.051*
H17A 0.6799 0.6291 0.0977 0.051*
C18 0.6616 (2) 0.39456 (9) −0.1044 (2) 0.0343 (5)
C19 0.6340 (2) 0.39290 (10) −0.2403 (2) 0.0348 (5)
C20 0.6901 (3) 0.35426 (13) −0.3045 (2) 0.0518 (6)
H20 0.7567 0.3295 −0.2659 0.062*
H20A 0.7506 0.3253 −0.2727 0.062*
C21 0.5322 (18) 0.4089 (8) −0.4434 (15) 0.097 (8)
H21 0.4757 0.4258 −0.5114 0.116*
C21A 0.632 (2) 0.3691 (11) −0.438 (2) 0.096 (15)
H21A 0.6570 0.3512 −0.5021 0.116*
C22 0.5417 (3) 0.42729 (14) −0.3181 (3) 0.0619 (8)
H22 0.4941 0.4570 −0.2942 0.074*
H22A 0.4936 0.4542 −0.2869 0.074*
C23 0.4818 (2) 0.39585 (10) 0.18369 (19) 0.0315 (4)
C24 0.3880 (2) 0.36767 (10) 0.24012 (18) 0.0320 (4)
C25 0.3990 (3) 0.31041 (11) 0.2909 (2) 0.0457 (6)
H25 0.4655 0.2843 0.2937 0.055*
H25A 0.4654 0.2847 0.2910 0.055*
C26 0.2792 (2) 0.39597 (11) 0.2484 (2) 0.0439 (6)
H26 0.2577 0.4347 0.2202 0.053*
H26A 0.2547 0.4342 0.2188 0.053*
C27 0.2091 (12) 0.3628 (5) 0.3000 (14) 0.058 (2)
H27 0.1317 0.3750 0.3102 0.069*
C27A 0.3030 (12) 0.2960 (6) 0.3401 (16) 0.061 (2)
H27A 0.2973 0.2600 0.3797 0.074*

1 Source of materials

3–Thiophenecarboxylic acid (6.0 mmol) was dissolved in 20 mL of anhydrous methanol. Mn(CH3COO)2·4H2O (3.0 mmol) dissolved in 15 mL of anhydrous methanol was added dropwise to the above 3-thiophenecarboxylic acid solution and stirred for 4 h at 55 °C. Then 1,10-phenanthroline (2.0 mmol) was dissolved in 10 mL of anhydrous methanol was added dropwise to the above solution and stirred for 3 h at 55 °C cooled and filtered. The filtrate was left for slow evaporation at room temperature. The yellow block crystals were formed 16 days later. Yield: 39.7 %. Anal. Calcd. for C54H34N4O12S6Mn3: C, 50.35; H, 2.66; N, 4.35; S, 14.94; found: C, 50.31; H, 2.70; N, 4.39; S, 14.90.

2 Experimental details

A suitable crystal was selected and mounted on a Bruker Smart APEX—II CCD. Hydrogen atoms were placed in their geometrically idealized positions and constrained to ride on their parent atoms.

3 Comment

Metal complexes are considered as promising anticancer drugs [3]. Thiophene carboxylates and its metal complexes have attracted extensive attention. Some of these metal complexes have excellent biological activities [4, 5]. We report herein a new trinuclear manganese metal complex constructed by 3-thiophenecarboxylate and 1,10-phenanthroline ligands. The title complex has a trinuclear structure, in which three Mn(II) ions are connected by O atoms of 3-thiophenecarboxylates. In the complex, each Mn(II) ion is six-coordinated in a distorted octahedral environment, in which one Mn(II) ion is coordinated by six O atoms of the 3-thiophenecarboxylato ligand, whereas the other two Mn(II) ions are coordinated by four O atoms and two N atoms from the 3-thiophenecarboxylato ligand and 1,10-phenanthroline ligand, respectively. The bond distances of Mn–N are 2.2464 (17) and 2.3245(18) Å, bond lengths of Mn–O are 2.1204 (14)–2.465(2) Å, respectively, which are similar with the references [6, 7]. The complex is has a centrosymmetric structure, and the symmetry center is the Mn2(II) ion.


Corresponding author: Zhongyu Zhang, College of Medicine and Nursing, Dezhou University, Dezhou, 253000, Shandong, China, E-mail:

Funding source: Transverse Research Project of Dezhou University

Award Identifier / Grant number: HXKT2022144 and HXKT2022212

Funding source: Bidding Subject of Dezhou University

Award Identifier / Grant number: 3010040205

Funding source: Shandong Province College Students Innovation and Entrepreneurship Training Program Project

Award Identifier / Grant number: 901569

  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 the Transverse Research Project of Dezhou University (No. HXKT2022144 and No. HXKT2022212), the Bidding Subject of Dezhou University (No. 3010040205) and the Shandong Province College Students Innovation and Entrepreneurship Training Program Project (No. 901569).

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

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Received: 2023-05-11
Accepted: 2023-10-20
Published Online: 2023-11-01
Published in Print: 2023-12-15

© 2023 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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