Home The crystal structure of tetra(1-ethylimidazole-κ 1 N)-[μ 4-imidazole-4,5-dicarboxylato-κ 4 O, N, O′, N′]-trioxido-divanadium, C25H33N10O7V2
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The crystal structure of tetra(1-ethylimidazole-κ 1 N)-[μ 4-imidazole-4,5-dicarboxylato-κ 4 O, N, O′, N′]-trioxido-divanadium, C25H33N10O7V2

  • Na Li , Xiao-Jie Wang ORCID logo EMAIL logo , Yu-Cai Qin and Jing-Yun Wang
Published/Copyright: April 14, 2023

Abstract

C25H33N10O7V2, triclinic, P 1 (no. 2), a = 10.3933(4) Å, b = 12.5655(5) Å, c = 14.1841(5) Å, α = 65.373(1)°, β =  70.351 ( 1 ) , γ =  88.052 ( 2 ) , V = 1573.62(11) Å3, Z = 2, R gt (F) = 0.0362, wR ref (F 2) = 0.0885, T = 173 K.

CCDC no.: 2251358

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: Purple block
Size: 0.26 × 0.18 × 0.12 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.65 mm−1
Diffractometer, scan mode: φ and ω
θ max, completeness: 25.4°, 99%
N(hkl)measured, N(hkl)unique, R int: 13,171, 5733, 0.038
Criterion for I obs, N(hkl)gt: I obs > 2σ(I obs), 4326
N(param)refined: 441
Programs: Bruker [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
C1 0.2837 (3) 0.8382 (2) 0.56417 (19) 0.0217 (6)
H1 0.304385 0.921621 0.526685 0.026*
C2 0.2237 (3) 0.6562 (2) 0.60165 (19) 0.0182 (5)
C3 0.2558 (3) 0.6569 (2) 0.68855 (19) 0.0191 (5)
C4 0.1891 (2) 0.5672 (2) 0.56758 (19) 0.0179 (5)
C5 0.2755 (3) 0.5708 (2) 0.79107 (19) 0.0200 (6)
C6 0.6149 (3) 0.8189 (3) 0.8402 (2) 0.0347 (7)
H6 0.646550 0.895157 0.780268 0.042*
C7 0.5999 (3) 0.6589 (3) 0.9882 (2) 0.0344 (7)
H7 0.617384 0.601812 1.050696 0.041*
C8 0.4974 (3) 0.6493 (2) 0.9532 (2) 0.0278 (6)
H8 0.429060 0.583195 0.987680 0.033*
C11 0.5331 (3) 0.8559 (2) 0.3084 (2) 0.0233 (6)
H11 0.522576 0.921362 0.326391 0.028*
C12 0.6280 (3) 0.7207 (2) 0.2579 (2) 0.0312 (7)
H12 0.693193 0.673448 0.235017 0.037*
C13 0.4910 (3) 0.7083 (3) 0.2788 (2) 0.0304 (7)
H13 0.443460 0.650278 0.271836 0.036*
C14 0.7885 (3) 0.8590 (3) 0.2671 (2) 0.0357 (7)
H14A 0.826470 0.793323 0.314290 0.043*
H14B 0.776768 0.920251 0.295134 0.043*
C15 0.8896 (3) 0.9106 (3) 0.1490 (3) 0.0454 (8)
H15A 0.900830 0.850571 0.120654 0.068*
H15B 0.978668 0.936338 0.147234 0.068*
H15C 0.854659 0.978313 0.102740 0.068*
C16 0.1187 (3) 0.7002 (3) 0.2434 (2) 0.0286 (6)
H16 0.051046 0.642482 0.307502 0.034*
C17 0.2464 (3) 0.8057 (3) 0.0699 (2) 0.0304 (7)
H17 0.285718 0.835845 −0.008517 0.036*
C18 0.2815 (3) 0.8445 (3) 0.1346 (2) 0.0296 (7)
H18 0.350260 0.908074 0.108818 0.035*
C21 −0.0872 (3) 0.6773 (2) 0.5116 (2) 0.0243 (6)
H21 −0.064010 0.603493 0.511737 0.029*
C22 −0.2066 (3) 0.8131 (3) 0.5446 (3) 0.0386 (8)
H22 −0.280223 0.851901 0.571493 0.046*
C23 −0.0753 (3) 0.8617 (3) 0.4795 (2) 0.0312 (7)
H23 −0.040789 0.941996 0.452220 0.037*
C24 −0.3350 (3) 0.6078 (3) 0.6257 (2) 0.0380 (8)
H24A −0.391693 0.618163 0.692279 0.046*
H24B −0.305735 0.527927 0.650840 0.046*
C25 −0.4202 (3) 0.6173 (3) 0.5567 (3) 0.0462 (9)
H25A −0.453423 0.694739 0.534922 0.069*
H25B −0.498874 0.555272 0.599840 0.069*
H25C −0.364034 0.608123 0.490169 0.069*
N1 0.2938 (2) 0.77216 (18) 0.66340 (16) 0.0205 (5)
N2 0.2412 (2) 0.77246 (18) 0.52482 (16) 0.0199 (5)
N3 0.5071 (2) 0.75076 (18) 0.85937 (17) 0.0232 (5)
N4 0.6742 (3) 0.7673 (2) 0.9157 (2) 0.0371 (6)
N5 0.4308 (2) 0.79277 (19) 0.31190 (17) 0.0225 (5)
N6 0.6537 (2) 0.8153 (2) 0.27624 (18) 0.0256 (5)
N7 0.2010 (2) 0.77671 (19) 0.24488 (16) 0.0231 (5)
N8 0.1429 (2) 0.7144 (2) 0.13961 (18) 0.0304 (6)
N9 0.0011 (2) 0.77588 (18) 0.45882 (16) 0.0214 (5)
N10 −0.2126 (2) 0.6962 (2) 0.56419 (19) 0.0307 (6)
O1 0.19169 (17) 0.61322 (15) 0.46655 (13) 0.0194 (4)
O2 0.16089 (19) 0.46137 (15) 0.63101 (14) 0.0258 (4)
O3 0.2392 (2) 0.46473 (16) 0.83405 (15) 0.0293 (5)
O4 0.33995 (19) 0.62254 (15) 0.82895 (14) 0.0253 (4)
O5 0.27083 (19) 0.86327 (17) 0.82264 (14) 0.0274 (4)
O6 0.50398 (19) 0.89838 (15) 0.65755 (13) 0.0243 (4)
O7 0.22472 (19) 0.94104 (16) 0.33137 (14) 0.0260 (4)
V1 0.38325 (4) 0.79850 (4) 0.76216 (3) 0.01819 (12)
V2 0.21698 (4) 0.80033 (4) 0.37792 (3) 0.01870 (12)
C9a 0.7945 (14) 0.828 (2) 0.915 (2) 0.054 (5)
H9Aa 0.782259 0.814432 0.992014 0.064*
H9Ba 0.803103 0.913690 0.869643 0.064*
C10a 0.9231 (11) 0.7787 (17) 0.869 (2) 0.067 (4)
H10Aa 0.913741 0.693559 0.914111 0.100*
H10Ba 1.003205 0.817352 0.868860 0.100*
H10Ca 0.935582 0.793521 0.792310 0.100*
C9′b 0.8064 (12) 0.8059 (19) 0.9178 (17) 0.057 (4)
H9′Ab 0.821092 0.748200 0.985421 0.068*
H9′Bb 0.801139 0.883130 0.921248 0.068*
C10′b 0.9264 (8) 0.8169 (13) 0.8177 (14) 0.070 (3)
H10Db 0.936384 0.739270 0.817106 0.106*
H10Eb 1.010527 0.846865 0.819975 0.106*
H10Fb 0.910566 0.871599 0.750421 0.106*
C19c 0.049 (2) 0.6577 (19) 0.110 (2) 0.030 (4)
H19Ac 0.045447 0.712126 0.036463 0.036*
H19Bc −0.044885 0.638786 0.165483 0.036*
C20c 0.1041 (19) 0.5449 (18) 0.105 (2) 0.048 (4)
H20Ac 0.199977 0.563442 0.054481 0.071*
H20Bc 0.048262 0.510366 0.079031 0.071*
H20Cc 0.099066 0.488426 0.179660 0.071*
C19′d 0.0823 (16) 0.6386 (13) 0.1056 (14) 0.046 (3)
H19Cd 0.117168 0.672550 0.023611 0.055*
H19Dd −0.018800 0.638803 0.131127 0.055*
C20′d 0.1133 (14) 0.5134 (9) 0.1501 (12) 0.058 (3)
H20Dd 0.213124 0.512054 0.123949 0.087*
H20Ed 0.070160 0.468308 0.124163 0.087*
H20Fd 0.076723 0.478170 0.231400 0.087*
  1. aOccupancy: 0.44 (3), bOccupancy: 0.56 (3), cOccupancy: 0.35 (3), dOccupancy: 0.65 (3).

1 Source of materials

NH4VO3 (0.34 g, 2 mmol), VO(acac)2 (0.265 g, 1 mmol), 4,5-imidazoledicarboxylic acid (0.16 g, 1 mmol) in 7 mL N-ethylimidazole was sealed in a 25 mL Teflon-lined stainless steel autoclave and was heated under autogenous pressure at 120 °C for 4320 min and then cooled to room temperature. Purple block crystals were collected.

2 Experimental details

The structure was solved by Direct Methods with the SHELXS-2018 program. All H-atoms from C and N atoms were positioned with idealized geometry and refined isotropically (U iso(H) = 1.2U eq(C)) using a riding model with C–H = 0.930Å. The C9, C10 and C19, C20 atoms of ethyl group are processed with PART [3] instruction.

3 Comment

The coordination chemistry of vanadium has developed rapidly, especially in the organic catalysis and biological activity [5], [6], [7], [8], [9]. In fact, the vanadium can display a variety of coordination numbers (such as 4, tetrahedron; 5, square-pyramid or trigonal bipyramid; 6, octahedron) and a wide range of the accessible oxidation states from +5 to +2, which greatly enriched the structural types of vanadium complexes [10], [11], [12]. On the other hand, the complex coordination number and oxidation states pose an extremely challenge for precise synthesis of target products [13], [14], [15]. So it is highly desirable to develop a controllable synthesis of vanadium complexes. In this text, we provide a simple one-pot method for preparing a dinuclear vanadium coordination compound. Single crystal X-ray diffraction shows that the title compound has two independent vanadium atoms V1 and V2, which adopted entirely different coordination modes. The coordination of V1 can be seen as tetragonal pyramid, which is completed by two N atoms and one O atom from one N-ethylimidazole and 4,5-imidazoledicarboxylic acid, respectively, and two V=O double bonds. The V2 has a distorted octahedron and the equatorial plane contains four N atoms from three N-ethylimidazole and 4,5-imidazoledicarboxylic acid, respectively, and the two vertexes are two O atoms. 4,5-imidazoledicarboxylate anion is a tetradentate-bridge for two vanadium atoms.


Corresponding author: Xiao-Jie Wang, School of Petrochemical Engineering, Liaoning Petrochemical University, Fushun, Liaoning Province 113001, P.R. China, E-mail:

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

  2. Research funding: Liaoning Revitalization Talents Program (XLYC2007130), and Talent Scientific Research Fund of Liaoning Petrochemical University (2016XJJL-019).

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

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Received: 2023-03-10
Accepted: 2023-03-24
Published Online: 2023-04-14
Published in Print: 2023-06-27

© 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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  49. Synthesis and crystal structure of 1-((3R,10S,13S,17S)-10,13-dimethyl-3-(m-tolylamino)hexadecahydro-1H-cyclopenta[α]phenanthren-17-yl)ethan-1-one, C28H41NO
  50. The crystal structure of diaqua-bis(4-bromo-2-formylphenoxy)zinc(II), C14H12Br2O6Zn
  51. The crystal structure of tetra(1-ethylimidazole-κ 1 N)-[μ 4-imidazole-4,5-dicarboxylato-κ 4 O, N, O′, N′]-trioxido-divanadium, C25H33N10O7V2
  52. The crystal structure of (E)-N′-(1-(4-fluorophenyl)propylidene)-2-hydroxybenzohydrazide, C16H15FN2O2
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