Home Physical Sciences Crystal structure of poly[octakis(μ-oxido)-tris(μ-1,1′-[[1,1′-biphenyl]-4,4′-diylbis(methylene)]bis(1H-imidazole))-tetrakis(oxido)-tetra-vanadium-dimanganese(II)dihydrate], C30H29MnN6O7V2
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Crystal structure of poly[octakis(μ-oxido)-tris(μ-1,1′-[[1,1′-biphenyl]-4,4′-diylbis(methylene)]bis(1H-imidazole))-tetrakis(oxido)-tetra-vanadium-dimanganese(II)dihydrate], C30H29MnN6O7V2

  • Ling-Ling Dai , Xiao-Jie Wang ORCID logo EMAIL logo and Yu-Cai Qin
Published/Copyright: May 9, 2024

Abstract

C30H29MnN6 O7V2, triclinic, P 1 (no. 2), a = 9.0806(3) Å, b = 11.1937(3) Å, c = 16.3585(5) Å, α = 102.2430(10)°, β = 100.090(1)°, γ = 97.7410(10)°, V = 1574.09(8) Å3, Z = 2, Rgt (F) = 0.0335, wRref (F 2) = 0.0886, T = 100 K.

CCDC no.: 2351581

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: Red block
Size: 0.22 × 0.21 × 0.20 mm
Wavelength:

μ:
Mo Kα radiation (0.71073 Å)

1.03 mm−1
Diffractometer, scan mode:

θ max, completeness:
Bruker APEX-II, φ and ω

29.6°, 99 %
N(hkl)measured, N(hkl)unique, R int: 20461, 8754, 0.040
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 7493
N(param)refined: 418
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
Mn1 0.08351 (2) 0.43771 (2) 0.07793 (2) 0.00901 (6)
V1 0.41899 (3) 0.31707 (2) 0.04087 (2) 0.01094 (6)
V2 0.73956 (3) 0.54233 (2) 0.10127 (2) 0.00932 (6)
O1 0.29237 (13) 0.36147 (11) 0.09690 (8) 0.0154 (2)
O2 0.41738 (14) 0.16744 (11) 0.02952 (9) 0.0213 (3)
O3 0.60607 (13) 0.40293 (11) 0.08941 (9) 0.0204 (3)
O4 0.81290 (14) 0.59937 (12) 0.20145 (8) 0.0208 (3)
O5 0.64009 (13) 0.65512 (11) 0.06354 (8) 0.0177 (2)
O6 0.87633 (12) 0.51279 (10) 0.04525 (7) 0.0110 (2)
N1 0.21646 (15) 0.61824 (12) 0.15768 (8) 0.0121 (2)
N2 0.41141 (15) 0.77252 (12) 0.21469 (8) 0.0116 (2)
N3 0.92245 (15) 1.05943 (12) 0.91941 (8) 0.0129 (3)
N4 0.96379 (15) 1.25359 (12) 0.99559 (8) 0.0116 (2)
N5 0.02485 (15) 0.39073 (13) 0.19559 (9) 0.0140 (3)
N6 −0.08807 (16) 0.31673 (13) 0.28808 (9) 0.0159 (3)
C1 0.36340 (17) 0.65715 (14) 0.16324 (10) 0.0128 (3)
H1 0.426803 0.609820 0.134634 0.015*
C2 0.28751 (18) 0.80997 (15) 0.24399 (11) 0.0156 (3)
H2 0.285649 0.887051 0.281380 0.019*
C3 0.16845 (18) 0.71454 (15) 0.20868 (10) 0.0151 (3)
H3 0.067798 0.714018 0.217628 0.018*
C4 0.56659 (18) 0.84452 (15) 0.23587 (10) 0.0151 (3)
H4A 0.564222 0.926067 0.221738 0.018*
H4B 0.630226 0.799788 0.201123 0.018*
C5 0.63577 (17) 0.86426 (15) 0.32979 (10) 0.0144 (3)
C6 0.6971 (2) 0.76987 (18) 0.35942 (12) 0.0256 (4)
H6 0.700655 0.695135 0.319997 0.031*
C7 0.7531 (2) 0.78448 (19) 0.44643 (12) 0.0288 (4)
H7 0.792763 0.718825 0.465979 0.035*
C8 0.7518 (2) 0.89435 (16) 0.50530 (11) 0.0188 (3)
C9 0.6942 (2) 0.98926 (17) 0.47547 (11) 0.0227 (4)
H9 0.694665 1.065377 0.514610 0.027*
C10 0.6353 (2) 0.97389 (16) 0.38825 (11) 0.0211 (3)
H10 0.594572 1.039185 0.368801 0.025*
C11 0.8066 (2) 0.90785 (16) 0.59862 (11) 0.0191 (3)
C12 0.7295 (2) 0.83149 (18) 0.64066 (12) 0.0264 (4)
H12 0.643439 0.770985 0.609327 0.032*
C13 0.7776 (2) 0.84310 (17) 0.72790 (12) 0.0244 (4)
H13 0.723396 0.791203 0.755812 0.029*
C14 0.9040 (2) 0.92978 (15) 0.77443 (10) 0.0173 (3)
C15 0.98291 (19) 1.00514 (17) 0.73286 (11) 0.0197 (3)
H15 1.070567 1.063956 0.764207 0.024*
C16 0.9342 (2) 0.99486 (17) 0.64556 (11) 0.0202 (3)
H16 0.988128 1.047322 0.617883 0.024*
C17 0.9525 (2) 0.94305 (15) 0.86946 (11) 0.0193 (3)
H17A 0.897255 0.871849 0.885326 0.023*
H17B 1.062586 0.941062 0.883761 0.023*
C18 1.02595 (18) 1.16323 (14) 0.95613 (10) 0.0135 (3)
H18 1.130644 1.170999 0.954099 0.016*
C19 0.81080 (18) 1.20369 (15) 0.98190 (10) 0.0134 (3)
H19 0.735864 1.246565 1.002139 0.016*
C20 0.78400 (18) 1.08347 (15) 0.93489 (10) 0.0150 (3)
H20 0.689258 1.027969 0.916670 0.018*
C21 −0.08954 (18) 0.31159 (15) 0.20501 (11) 0.0144 (3)
H21 −0.163420 0.257891 0.158880 0.017*
C22 0.1027 (2) 0.44954 (17) 0.27777 (11) 0.0197 (3)
H22 0.190973 0.512198 0.291844 0.024*
C23 0.0348 (2) 0.40481 (17) 0.33563 (11) 0.0210 (3)
H23 0.065715 0.429224 0.396212 0.025*
C24 −0.1961 (2) 0.24075 (16) 0.32138 (12) 0.0208 (4)
H24A −0.140246 0.193135 0.356930 0.025*
H24B −0.267847 0.180564 0.272993 0.025*
C25 −0.2845 (2) 0.31965 (16) 0.37462 (12) 0.0188 (3)
C26 −0.2784 (2) 0.31846 (18) 0.45943 (12) 0.0251 (4)
H26 −0.215352 0.269417 0.485018 0.030*
C27 −0.3631 (2) 0.38800 (18) 0.50815 (12) 0.0255 (4)
H27 −0.358404 0.383916 0.565953 0.031*
C28 −0.45434 (19) 0.46311 (15) 0.47394 (12) 0.0184 (3)
C29 −0.4576 (3) 0.4645 (3) 0.38850 (16) 0.0439 (7)
H29 −0.518269 0.515261 0.363173 0.053*
C30 −0.3754 (3) 0.3942 (2) 0.33934 (15) 0.0415 (6)
H30 −0.381254 0.397052 0.281242 0.050*
O1W 0.63013 (15) 1.04705 (12) 0.11624 (8) 0.0230 (3)
H1WA 0.570121 1.090666 0.093043 0.034*
H1WB 0.617167 0.977710 0.077574 0.034*

1 Source of materials

A mixture comprising NaVO3 (0.5 mmol, 61.0 mg) and N2H4·H2O (0.1 mmol, 6.2 μL) in H2O (9.5 mL) was stirred for a duration of 30 min at ambient temperature. The mixture was stirred for an additional hour after being enriched with a solution containing 4,4′-bis(imidazol-1-ylmethyl)biphenyl (bibp; 0.15 mmol, 47.1 mg) in DMF (0.5 mL) and Mn(OAc)2·4H2O (0.1 mmol, 24.5 mg). The pH of this mixture was then adjusted by adding HCl (aq 1.0 M) to 3.42, and the resulting mixture was poured into a 23 mL Teflon-lined autoclave reactor and kept at 393 K for 3 days. The product was obtained as a green crystalline solid after the autoclave was cooled to room temperature.

2 Experimental details

The structure was solved by Direct Methods with the SHELXS-2018 program. All the non–H atoms were refined anisotropically. All H-atoms from C atoms were positioned with idealized geometry and refined isotropic (U iso(H) = 1.2U eq(C)) and (U iso(H) = 1.5U eq(C)) using a riding model with C–H = 0.950 Å (imidazole and phenyl groups) and C–H = 0.990 Å (methylene), respectively. The water H-atom positions were fixed with O–H = 0.870 Å (U iso(H) = 1.5U eq(O)).

3 Comment

Vanadium-based functional complexes have attracted widespread research interest due to their rich topological structural types. 5 16 The bibp is a linear bridging ligand containing rigid biphenyls and flexible alkyl groups, and if applied to the synthesis of polyvanadates-based coordination complexes, it may yield very interesting crystal structures. However, to our knowledge, only two polyvanadate based compounds containing bibp ligands have been reported up to now. 9 Here, we prepared a new polyvanadate manganese complex based on bibp ligand using a simple one pot method. Single-crystal X-ray diffraction study shows the title compound crystallizes in the space group P 1 and exhibits a very complicated 3D framework. The asymmetric unit consists of 2 V atoms, 1 Mn atom, 1.5 bridging ligands bibp, and one water molecule. The V1 and V2 are coordinated by four O atoms (O1, O2, O3, O5) and (O3, O4, O5A, O6), respectively. All the V–O bond lengths are in the range of 1.611–1.803 Å, which are comparable with other vanadium cluster structures. 9 17 Four VO4 units are joined together with each sharing two of its O atoms, resulting in the ring-like {V4O12} motif. The Mn(II) ion is hexacoordinated in a distorted octahedral coordination sphere formed by three N atoms of different bibp ligands [Mn–N: 2.217–2.231 Å] and three O atoms from two of the above-mentioned {V4O12} units [Mn–O: 2.183–2.190 Å]. The two Mn(II) atoms are bridged into a dinuclear unit {Mn2} by two crystallographically equivalent μ3-O (O6) atoms of the {V4} rings. The bibp ligands show two distinct conformations in the crystal structure. In one of the ligands, the two benzene rings on the biphenyl are in the same plane, while in the other biphenyl, the two benzene rings appear perpendicular to each other.


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: Talent Scientific Research Fund of Liaoning Petrochemical University (2016XJJL-019).

  3. Competing interests: The authors declare no conflicts of interest regarding this article.

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Received: 2024-03-21
Accepted: 2024-04-27
Published Online: 2024-05-09
Published in Print: 2024-08-27

© 2024 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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  43. The crystal structure of fac-tricarbonyl(bis(3,5-dimethyl-4H-pyrazole)-κ1 N)-((nitrato)-κ1 O)-rhenium(I)— 3,5-dimethyl-4H-pyrazole(1/1), C18H23N7O6Re
  44. The crystal structure of 4′-chloro-griseofulvin: (2S,6′R)-4′,7-dichloro-4,6-dimethoxy-6′-methyl-3H-spiro[benzofuran-2,1′-cyclohexan]-3′-ene-2′,3-dione, C16H14Cl2O5
  45. Crystal structure of tetraethylammonium bicarbonate–1-(diaminomethylene)thiourea(1/1)
  46. Crystal structure of 1-cyclohexyl-4-p-tolyl-1,4-dihydropyridine-3,5-dicarboxylic acid dimethyl ester, C22H27NO4
  47. The crystal structure of catena-poly(μ2-1,4-bis-(1H-imidazol-1-yl)benzene-copper(I)) dichloridocopper(I), {[CuC12H10N4]+[CuCl2]} n
  48. The crystal structure of propane-1-aminium-2-carbamate, C4H10N2O2
  49. Crystal structure of 5,6,3′,4′,5′-pentamethoxy-flavone dihydrate, C20H24O9
  50. Crystal structure of (E)-N-(2-bromophenyl)-4-(4-(3,5-dimethoxystyryl)phenoxy)pyrimidin-2-amine, C26H22BrN3O3
  51. Crystal structure of methyl (3R)-1-(2-bromo-4-fluorophenyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate hydrochloride hydrate, C19H19BrClFN2O3
  52. The crystal structure of 1-(2-chlorophenyl)-3-(p-tolyl)urea, C14H13ClN2O
  53. The crystal structure of 1-cyclohexyl-3-(p-tolyl)urea, C14H20N2O
  54. Crystal structure of ((benzyl(hydroxy)-amino)(4-chlorophenyl)methyl)-diphenylphosphine oxide, C26H23ClNO2P
  55. The crystal structure of ethyl 3-(1-methyl-1H-indole-2-carbonyl)-2-phenylquinoline-4-carboxylate, C28H22N2O3
  56. The crystal structure of 1,4-bis(1H-imidazol-3-ium-1-yl)benzene dinitrate, C12H12N4 2+·2(NO3 )
  57. Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
  58. Crystal structure of 1-(4-(dimethylamino)phenyl)-2,3-bis(diphenylphosphoryl)propan-1-one, C35H33NO3P2
  59. Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
  60. Crystal structure of (R)-N, N -dimethyl-[1, 1′-binaphthalene]-2, 2′-diamine, C22H20N2
  61. Crystal structure of 1-phenyl-4-(2-furoyl)-3-furyl-1H-pyrazol-5-ol, C18H12N2O4
  62. Crystal structure of bis(14,34-dimethyl[11,21:23,31-terphenyl]-22-yl)diselane, C40H34Se2
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