Home Crystal structure of bis(2,5,5,7-tetramethyl-1,4-diazepane-1,4-diium) diaqua-bis(1,2-diaminopropane)copper(II) bis(μ6-oxido)tetrakis(μ3-oxido)-tetradecakis(μ2-oxido)-octaoxido-decavanadium(V) – water (1/4), C24H76CuN8V10O34
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Crystal structure of bis(2,5,5,7-tetramethyl-1,4-diazepane-1,4-diium) diaqua-bis(1,2-diaminopropane)copper(II) bis(μ6-oxido)tetrakis(μ3-oxido)-tetradecakis(μ2-oxido)-octaoxido-decavanadium(V) – water (1/4), C24H76CuN8V10O34

  • Yuan-Huan Deng and Qiong Wang ORCID logo EMAIL logo
Published/Copyright: February 13, 2023

Abstract

C24H76CuN8V10O34, monoclinic, P21/n (no. 14), a = 22.416(4) Å, b = 11.7003(18) Å, c = 20.079(3) Å, β = 95.594(7)°, V = 5241.2(14) Å3, Z = 4, Rgt(F) = 0.0243, wRref(F2) = 0.1110, T = 296(2) K.

CCDC no.: 2238091

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 block
Size: 0.32 × 0.28 × 0.16 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 2.20 mm−1
Diffractometer, scan mode: Bruker APEX-II, φ and ω
θmax, completeness: 27.7°, >99%
N(hkl)measured, N(hkl)unique, Rint: 23,078, 6030, 0.017
Criterion for Iobs, N(hkl)gt: Iobs > 2σ(Iobs), 5457
N(param)refined: 372
Programs: BRUKER [1], SHELX [2, 3], Diamond [4]
Table 2:

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

Atom x y z Uiso*/Ueq
C1 0.03679 (12) 0.3798 (3) −0.11290 (15) 0.0439 (7)
H1C 0.041899 0.302830 −0.095249 0.053*
H1D 0.057839 0.385277 −0.152761 0.053*
C2 0.02858 (13) 0.5957 (3) 0.13012 (15) 0.0442 (7)
H2 0.032544 0.520744 0.151916 0.053*
C3 0.05883 (17) 0.6850 (4) 0.17758 (17) 0.0671 (12)
H3C 0.099336 0.662042 0.191001 0.101*
H3D 0.037217 0.691690 0.216390 0.101*
H3E 0.058947 0.757501 0.155177 0.101*
C4 0.22262 (10) 0.1238 (2) 0.34069 (10) 0.0212 (4)
H4C 0.220476 0.107438 0.293150 0.025*
H4D 0.257242 0.083975 0.362235 0.025*
C5 0.23111 (10) 0.2504 (2) 0.35119 (10) 0.0203 (4)
H5 0.223193 0.268815 0.397133 0.024*
C6 0.29457 (11) 0.2863 (2) 0.34177 (11) 0.0259 (5)
H6A 0.302866 0.269932 0.296739 0.039*
H6B 0.322106 0.244917 0.372494 0.039*
H6C 0.299028 0.366784 0.350102 0.039*
C7 0.12320 (10) 0.2923 (2) 0.30476 (11) 0.0235 (5)
H7 0.113162 0.291251 0.351175 0.028*
C8 0.08911 (13) 0.3890 (3) 0.26745 (16) 0.0402 (7)
H8A 0.104640 0.461052 0.284166 0.060*
H8B 0.047362 0.383714 0.274081 0.060*
H8C 0.093811 0.383303 0.220551 0.060*
C9 0.10787 (11) 0.1762 (2) 0.27272 (11) 0.0252 (5)
H9A 0.134116 0.164361 0.237686 0.030*
H9B 0.067247 0.180431 0.251241 0.030*
C10 0.11213 (10) 0.0694 (2) 0.31806 (11) 0.0238 (5)
C11 0.05876 (13) 0.0598 (3) 0.35984 (14) 0.0400 (7)
H11A 0.065786 −0.001124 0.391673 0.060*
H11B 0.023032 0.044054 0.330931 0.060*
H11C 0.053996 0.130370 0.383109 0.060*
C12 0.11831 (14) −0.0374 (2) 0.27630 (13) 0.0366 (6)
H12A 0.154152 −0.032351 0.253914 0.055*
H12B 0.084188 −0.044028 0.243714 0.055*
H12C 0.120487 −0.103342 0.304887 0.055*
Cu1 0.000000 0.500000 0.000000 0.03230 (13)
N1 0.06171 (10) 0.4632 (2) −0.06247 (11) 0.0343 (5)
H1A 0.072299 0.526699 −0.082731 0.041*
H1B 0.094203 0.434248 −0.039550 0.041*
N2 0.05650 (10) 0.5898 (2) 0.06584 (11) 0.0344 (5)
H2A 0.091951 0.555133 0.071983 0.041*
H2B 0.061952 0.659872 0.050263 0.041*
N3 0.16745 (9) 0.07901 (17) 0.36767 (9) 0.0210 (4)
H3A 0.158773 0.124355 0.400988 0.025*
H3B 0.175620 0.010084 0.384969 0.025*
N4 0.18909 (8) 0.31918 (16) 0.30407 (10) 0.0222 (4)
H4A 0.199067 0.308583 0.262685 0.027*
H4B 0.194595 0.392849 0.313865 0.027*
O1 0.32906 (6) 0.13368 (13) −0.00322 (7) 0.0158 (3)
O1W 0.36185 (9) 0.71604 (17) 0.01840 (9) 0.0330 (4)
H1WA 0.3423 (14) 0.7737 (17) 0.0027 (14) 0.050*
H1WB 0.3576 (15) 0.6611 (17) −0.0093 (13) 0.050*
O2 0.33601 (7) 0.22691 (13) 0.12096 (7) 0.0189 (3)
O2W 0.01306 (11) 0.3186 (2) 0.07593 (14) 0.0528 (6)
H2WA 0.0502 (6) 0.302 (3) 0.086 (2) 0.079*
H2WB −0.0020 (15) 0.264 (3) 0.0503 (19) 0.079*
O3 0.29706 (7) 0.01488 (13) 0.10366 (7) 0.0198 (3)
O3W 0.00836 (13) 0.8519 (3) 0.02340 (17) 0.0667 (7)
H3WA 0.0338 (16) 0.900 (3) 0.043 (2) 0.100*
H3WB −0.0194 (15) 0.893 (3) 0.003 (2) 0.100*
O4 0.30296 (8) 0.09609 (16) 0.22751 (7) 0.0284 (4)
O5 0.19626 (7) 0.06776 (14) 0.15541 (7) 0.0213 (3)
O6 0.23562 (7) 0.27741 (13) 0.17502 (7) 0.0189 (3)
O7 0.13061 (7) 0.23931 (14) 0.10264 (7) 0.0197 (3)
O8 0.16435 (7) 0.45362 (14) 0.13021 (8) 0.0228 (3)
O9 0.26817 (7) 0.40191 (12) 0.06890 (7) 0.0154 (3)
O10 0.20803 (8) 0.59375 (14) 0.01466 (8) 0.0269 (4)
O11 0.30921 (7) 0.52044 (13) −0.03272 (7) 0.0209 (3)
O12 0.41239 (8) 0.47772 (17) −0.08858 (10) 0.0340 (4)
O13 0.37349 (7) 0.34949 (14) 0.01809 (8) 0.0210 (3)
O14 0.23194 (6) 0.18940 (12) 0.05115 (6) 0.0145 (3)
V1 0.31511 (2) 0.27377 (3) 0.04238 (2) 0.01411 (10)
V2 0.27020 (2) 0.13518 (3) 0.15649 (2) 0.01905 (11)
V3 0.19248 (2) 0.33928 (3) 0.10149 (2) 0.01578 (10)
V4 0.23405 (2) 0.47874 (3) −0.01697 (2) 0.01670 (10)
V5 0.35161 (2) 0.41005 (3) −0.07815 (2) 0.02052 (11)

Source of material

An aqueous solution (10 mL) of NH4VO3 (117 mg, 1 mmol) was layered with an acetonitrile solution (10 mL) of [Cu(1,2-pn)2](ClO4)2 (42.3 mg, 0.1 mmol) (pn = diaminopropane) and 2,5,5,7-tetramethyl-1,4-diazepane (tmda, 15.6 mg, 0.1 mmol). The resultant solution was slowly and naturally diffused at room temperature. Crystals of the title compound were obtained within one week.

Experimental details

The structure was solved using Direct Methods, which yielded the positions of all non-hydrogen atoms. All the hydrogen atoms were placed in calculated positions with fixed isotropic thermal parameters. The Uiso values of the hydrogen atoms of methyl groups were set to 1.5Ueq(C) and the Uiso values of all other hydrogen atoms were set to 1.2Ueq(C, N).

Comment

Similar substances to the title compound have been synthesized [56], which exhibited three-dimensional structures formed by connections of polyoxovanadium clusters with [Cu(1,2-pn)2]2+ groups.

X-ray crystal structural analysis reveals that the asymmetric unit of the title structure contains one half of a[Cu(1,2-pn)2(H2O)2]2+, one half of a [V10O26]6−, one 2,5,5,7-tetramethyl-1,4-diazepane-1,4-diium, [tmda]2+ and two water molecules (see the figure; water molecules were omitted). The central Cu(II) atom displays a six-coordinate octahedral coordination geometry by coordination with four nitrogen atoms of 1,2-pn, and two oxygen atoms of water.

The monomers of [Cu(1,2-pn)2(H2O)2]2+, [V10O26]6−, [tmda]2+ and water molecules are connected through intermolecular hydrogen bonds to form a three-dimensional structure.


Corresponding author: Qiong Wang, College of Chemistry and Bioengineering, Hunan University of Science and Engineering, Yongzhou, Hunan 425199, P. R. China, E-mail:

Funding source: The Scientific Research Fund of Hunan Provincial Education Department http://dx.doi.org/10.13039/100014472

Award Identifier / Grant number: 22C0529

Acknowledgments

This work was financially supported by the construct program of applied characteristic discipline in Hunan University of Science and Engineering.

  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 financially supported by the construct program of applied characteristic discipline in The Scientific Research Fund of Hunan Provincial Education Department (22C0529).

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

References

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2. Sheldrick, G. M. SHELXTL – integrated space-group and crystal-structure determination. Acta Crystallogr. 2015, A71, 3–8; https://doi.org/10.1107/s2053273314026370.Search in Google Scholar PubMed PubMed Central

3. Sheldrick, G. M. Crystal structure refinement with Shelxl. Acta Crystallogr. 2015, C71, 3–8; https://doi.org/10.1107/s2053229614024218.Search in Google Scholar

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Received: 2022-11-24
Accepted: 2023-01-26
Published Online: 2023-02-13
Published in Print: 2023-04-25

© 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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  72. The crystal structure of 1-(2-fluorobenzoyl)-5-methoxy-2-methyl-1H-indole-3-carbonitrile, C18H13FN2O2
  73. Crystal structure of bis(trimethylphenylammonium) aqua-oxido-octathiotritungstate, (Me3PhN)2[W3OS8(H2O)]
  74. The crystal structure of trichlorido[N-[(2-oxyphenyl)methylidene]phenylglycinemethylester-κ3O,N,O′]-tin(IV) – methylene chloride (1/1), C16H14Cl3NO3Sn·CH2Cl2
  75. The crystal structure of furan-2,5-diylbis((4-chlorophenyl)methanol), C18H14Cl2O3
  76. The crystal structure of hexalithium decavanadate hexadecahydrate, H32Li6O44V10
  77. Crystal structure of ethyl 4-{[5-(adamantan-1-yl)-2-sulfanylidene-2,3-dihydro-1,3,4-oxadiazol-3-yl]methyl}piperazine-1-carboxylate, C20H30N4O3S
  78. Crystal structure of aqua(μ2-2,2′,2″-((nitrilo)tris(ethane-2,1-diyl(nitrilo)methylylidene))tris (6-ethoxyphenolato))(pentane-2,4-dionato-κ2O,O′)-dinickel(II), C38H48N4Ni2O9
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