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The crystal structure of a dinuclear oxidovanadium(IV/V) complex [V2O2(μ-O)(μ-H(SO4)2)(4,4′-tBubpy)2] aceto­nitrile monosolvate has been determined.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989023009040/nx2001sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989023009040/nx2001Isup2.hkl
Contains datablock I

CCDC reference: 2301351

Computing details top

Data collection: CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011); cell refinement: CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011); data reduction: CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011); program(s) used to solve structure: olex2.solve 1.5 (Bourhis et al., 2015); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015); molecular graphics: Olex2 1.5 (Dolomanov et al., 2009); software used to prepare material for publication: Olex2 1.5 (Dolomanov et al., 2009).

(µ-Hydrogen disulfato)-µ-oxido-bis[(4,4'-di-tert-butyl-2,2'-bipyridine)oxidovanadium(IV/V)] acetonitrile monosolvate top
Crystal data top
[V2(HS2O8)O3(C18H24N2)2]·C2H3NDx = 1.362 Mg m3
Mr = 920.84Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, FdddCell parameters from 30626 reflections
a = 13.0134 (2) Åθ = 1.9–30.6°
b = 34.9495 (5) ŵ = 0.57 mm1
c = 39.4864 (6) ÅT = 110 K
V = 17958.9 (5) Å3Block, clear dark brown
Z = 160.16 × 0.11 × 0.06 mm
F(000) = 7696
Data collection top
Rigaku Saturn724+ (2x2 bin mode)
diffractometer
6582 independent reflections
Radiation source: Rotating Anode5675 reflections with I > 2σ(I)
Detector resolution: 28.5714 pixels mm-1Rint = 0.049
profile data from ω–scansθmax = 30.5°, θmin = 2.1°
Absorption correction: multi-scan
(CrysAlisPro; Rigaku OD, 2020)
h = 1818
Tmin = 0.815, Tmax = 1.000k = 4950
51528 measured reflectionsl = 5554
Refinement top
Refinement on F2Primary atom site location: iterative
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.043H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.110 w = 1/[σ2(Fo2) + (0.0469P)2 + 46.648P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max = 0.003
6582 reflectionsΔρmax = 0.50 e Å3
287 parametersΔρmin = 0.33 e Å3
27 restraints
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
V10.70713 (2)0.54069 (2)0.59096 (2)0.02335 (8)
S10.75306 (3)0.47690 (2)0.64590 (2)0.02120 (10)
O50.66572 (10)0.49435 (3)0.66352 (3)0.0235 (2)
O30.78535 (10)0.50242 (4)0.61695 (3)0.0255 (3)
O60.71873 (10)0.43950 (3)0.63066 (3)0.0258 (3)
O40.84010 (10)0.46966 (4)0.66746 (3)0.0299 (3)
O10.79258 (12)0.57322 (4)0.58859 (3)0.0369 (3)
O20.6250000.55852 (5)0.6250000.0394 (5)
N20.75091 (11)0.51363 (4)0.54454 (3)0.0216 (3)
N10.60817 (12)0.56465 (4)0.55441 (3)0.0224 (3)
C30.48418 (13)0.59696 (5)0.50377 (4)0.0225 (3)
C60.69971 (13)0.52426 (5)0.51604 (4)0.0202 (3)
C70.72724 (13)0.51037 (5)0.48439 (4)0.0223 (3)
H70.6887350.5175930.4649720.027*
C80.81169 (13)0.48568 (5)0.48092 (4)0.0252 (3)
C110.41640 (14)0.61383 (5)0.47598 (5)0.0260 (3)
C40.55602 (13)0.56814 (4)0.49641 (4)0.0210 (3)
H40.5625350.5589530.4738720.025*
C50.61741 (13)0.55301 (4)0.52172 (4)0.0200 (3)
C20.47668 (14)0.60821 (5)0.53749 (5)0.0265 (3)
H20.4288970.6274750.5438210.032*
C100.83025 (13)0.48947 (5)0.54148 (4)0.0259 (3)
H100.8652300.4815140.5613930.031*
C90.86340 (14)0.47561 (5)0.51049 (5)0.0283 (4)
H90.9215000.4591940.5093970.034*
C10.53844 (15)0.59148 (5)0.56180 (4)0.0266 (3)
H10.5310670.5993650.5846950.032*
C150.84388 (15)0.47210 (6)0.44572 (5)0.0329 (4)
C120.48286 (15)0.62876 (5)0.44658 (5)0.0310 (4)
H12A0.5246270.6077830.4375280.047*
H12B0.5279930.6491800.4548150.047*
H12C0.4382680.6388070.4286640.047*
C130.34999 (16)0.64692 (6)0.48896 (6)0.0375 (5)
H13A0.3943110.6668150.4985830.056*
H13B0.3029880.6374650.5064510.056*
H13C0.3102030.6576490.4701500.056*
C140.34585 (16)0.58193 (6)0.46305 (5)0.0346 (4)
H14A0.2997900.5737630.4813030.052*
H14B0.3875620.5601540.4555980.052*
H14C0.3050670.5914660.4439670.052*
C180.93513 (18)0.44437 (7)0.44714 (6)0.0434 (5)
H18A0.9155260.4214720.4599280.065*
H18B0.9933530.4568790.4583290.065*
H18C0.9548060.4370440.4240810.065*
C170.87660 (19)0.50771 (7)0.42503 (5)0.0437 (5)
H17A0.9291380.5219480.4375720.065*
H17B0.8167240.5241710.4212580.065*
H17C0.9046610.4995450.4031580.065*
C160.75339 (19)0.45218 (7)0.42815 (6)0.0467 (6)
H16A0.6951860.4698930.4266860.070*
H16B0.7332000.4295680.4412370.070*
H16C0.7739660.4443430.4053060.070*
N30.6842 (6)0.5900 (2)0.3294 (2)0.102 (2)0.5
C190.5721 (5)0.64049 (17)0.36076 (15)0.0605 (14)0.5
H19A0.5496900.6603080.3448250.091*0.5
H19B0.6119880.6522770.3790370.091*0.5
H19C0.5117400.6276480.3703300.091*0.5
C200.6367 (5)0.61212 (17)0.34275 (17)0.0616 (15)0.5
H60.659 (3)0.4376 (11)0.6263 (12)0.022 (11)*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.03845 (17)0.01764 (13)0.01395 (13)0.00275 (11)0.00195 (11)0.00237 (10)
S10.0276 (2)0.01950 (18)0.01648 (18)0.00117 (15)0.00710 (15)0.00280 (14)
O50.0351 (6)0.0179 (5)0.0175 (5)0.0015 (5)0.0031 (5)0.0012 (4)
O30.0312 (6)0.0263 (6)0.0188 (6)0.0014 (5)0.0056 (5)0.0055 (5)
O60.0299 (7)0.0197 (5)0.0278 (6)0.0026 (5)0.0082 (5)0.0035 (5)
O40.0337 (7)0.0335 (7)0.0225 (6)0.0012 (5)0.0126 (5)0.0061 (5)
O10.0574 (9)0.0273 (6)0.0260 (7)0.0137 (6)0.0164 (6)0.0075 (5)
O20.0866 (16)0.0163 (8)0.0154 (8)0.0000.0162 (9)0.000
N20.0258 (7)0.0224 (6)0.0165 (6)0.0021 (5)0.0045 (5)0.0027 (5)
N10.0361 (8)0.0169 (6)0.0142 (6)0.0020 (5)0.0000 (5)0.0007 (5)
C30.0267 (8)0.0173 (7)0.0236 (8)0.0009 (6)0.0029 (6)0.0032 (6)
C60.0248 (7)0.0199 (7)0.0160 (7)0.0009 (6)0.0030 (6)0.0017 (6)
C70.0259 (8)0.0238 (7)0.0171 (7)0.0025 (6)0.0047 (6)0.0001 (6)
C80.0259 (8)0.0288 (8)0.0207 (8)0.0024 (7)0.0022 (6)0.0010 (6)
C110.0290 (8)0.0202 (7)0.0289 (8)0.0042 (6)0.0069 (7)0.0053 (6)
C40.0267 (8)0.0196 (7)0.0167 (7)0.0002 (6)0.0016 (6)0.0022 (6)
C50.0280 (8)0.0163 (6)0.0157 (7)0.0014 (6)0.0010 (6)0.0007 (5)
C20.0331 (9)0.0202 (7)0.0260 (8)0.0017 (6)0.0018 (7)0.0064 (6)
C100.0255 (8)0.0306 (8)0.0216 (8)0.0004 (7)0.0069 (6)0.0034 (7)
C90.0252 (8)0.0342 (9)0.0257 (8)0.0061 (7)0.0041 (7)0.0014 (7)
C10.0418 (10)0.0195 (7)0.0185 (7)0.0011 (7)0.0019 (7)0.0046 (6)
C150.0333 (9)0.0419 (10)0.0234 (8)0.0141 (8)0.0034 (7)0.0064 (8)
C120.0378 (10)0.0261 (8)0.0292 (9)0.0026 (7)0.0079 (7)0.0021 (7)
C130.0373 (10)0.0317 (10)0.0436 (11)0.0128 (8)0.0062 (9)0.0083 (8)
C140.0348 (10)0.0284 (9)0.0407 (11)0.0005 (7)0.0120 (8)0.0066 (8)
C180.0416 (11)0.0547 (13)0.0337 (11)0.0206 (10)0.0025 (9)0.0081 (10)
C170.0523 (13)0.0544 (13)0.0243 (9)0.0141 (11)0.0077 (9)0.0033 (9)
C160.0444 (12)0.0551 (14)0.0404 (12)0.0158 (10)0.0109 (10)0.0243 (11)
N30.088 (4)0.100 (4)0.117 (5)0.037 (3)0.042 (4)0.029 (4)
C190.073 (3)0.063 (3)0.045 (3)0.037 (3)0.003 (3)0.007 (2)
C200.053 (3)0.065 (3)0.067 (3)0.022 (3)0.008 (3)0.001 (2)
Geometric parameters (Å, º) top
V1—O5i2.2827 (12)C10—H100.9500
V1—O31.9692 (12)C10—C91.385 (3)
V1—O11.5932 (14)C9—H90.9500
V1—O21.8268 (7)C1—H10.9500
V1—N22.1399 (14)C15—C181.534 (3)
V1—N12.1077 (14)C15—C171.549 (3)
S1—O51.4654 (13)C15—C161.534 (3)
S1—O31.5098 (12)C12—H12A0.9800
S1—O61.5066 (13)C12—H12B0.9800
S1—O41.4391 (13)C12—H12C0.9800
O6—H60.80 (4)C13—H13A0.9800
N2—C61.360 (2)C13—H13B0.9800
N2—C101.339 (2)C13—H13C0.9800
N1—C51.359 (2)C14—H14A0.9800
N1—C11.337 (2)C14—H14B0.9800
C3—C111.526 (2)C14—H14C0.9800
C3—C41.405 (2)C18—H18A0.9800
C3—C21.392 (2)C18—H18B0.9800
C6—C71.388 (2)C18—H18C0.9800
C6—C51.486 (2)C17—H17A0.9800
C7—H70.9500C17—H17B0.9800
C7—C81.404 (2)C17—H17C0.9800
C8—C91.393 (2)C16—H16A0.9800
C8—C151.527 (2)C16—H16B0.9800
C11—C121.539 (3)C16—H16C0.9800
C11—C131.532 (2)N3—C201.120 (9)
C11—C141.532 (2)C19—H19A0.9800
C4—H40.9500C19—H19B0.9800
C4—C51.384 (2)C19—H19C0.9800
C2—H20.9500C19—C201.482 (8)
C2—C11.382 (3)
O3—V1—O5i85.44 (5)N2—C10—H10118.7
O3—V1—N290.49 (5)N2—C10—C9122.69 (15)
O3—V1—N1160.47 (5)C9—C10—H10118.7
O1—V1—O5i172.18 (6)C8—C9—H9119.9
O1—V1—O398.89 (7)C10—C9—C8120.11 (16)
O1—V1—O2102.02 (7)C10—C9—H9119.9
O1—V1—N294.54 (7)N1—C1—C2122.68 (16)
O1—V1—N195.89 (6)N1—C1—H1118.7
O2—V1—O5i83.64 (5)C2—C1—H1118.7
O2—V1—O398.66 (5)C8—C15—C18112.05 (16)
O2—V1—N2159.52 (5)C8—C15—C17107.79 (16)
O2—V1—N190.62 (5)C8—C15—C16110.01 (17)
N2—V1—O5i78.84 (5)C18—C15—C17108.31 (18)
N1—V1—O5i78.52 (5)C18—C15—C16108.92 (18)
N1—V1—N275.63 (5)C16—C15—C17109.72 (18)
O5—S1—O3109.23 (7)C11—C12—H12A109.5
O5—S1—O6108.70 (8)C11—C12—H12B109.5
O6—S1—O3107.02 (7)C11—C12—H12C109.5
O4—S1—O5113.76 (8)H12A—C12—H12B109.5
O4—S1—O3109.43 (8)H12A—C12—H12C109.5
O4—S1—O6108.49 (8)H12B—C12—H12C109.5
S1—O5—V1i143.30 (7)C11—C13—H13A109.5
S1—O3—V1130.69 (8)C11—C13—H13B109.5
S1—O6—H6117 (3)C11—C13—H13C109.5
V1—O2—V1i140.11 (10)H13A—C13—H13B109.5
C6—N2—V1117.24 (11)H13A—C13—H13C109.5
C10—N2—V1124.13 (11)H13B—C13—H13C109.5
C10—N2—C6118.41 (14)C11—C14—H14A109.5
C5—N1—V1118.52 (11)C11—C14—H14B109.5
C1—N1—V1122.95 (11)C11—C14—H14C109.5
C1—N1—C5118.51 (15)H14A—C14—H14B109.5
C4—C3—C11120.86 (15)H14A—C14—H14C109.5
C2—C3—C11122.56 (15)H14B—C14—H14C109.5
C2—C3—C4116.56 (15)C15—C18—H18A109.5
N2—C6—C7121.55 (15)C15—C18—H18B109.5
N2—C6—C5114.41 (14)C15—C18—H18C109.5
C7—C6—C5123.97 (14)H18A—C18—H18B109.5
C6—C7—H7119.8H18A—C18—H18C109.5
C6—C7—C8120.33 (15)H18B—C18—H18C109.5
C8—C7—H7119.8C15—C17—H17A109.5
C7—C8—C15119.64 (15)C15—C17—H17B109.5
C9—C8—C7116.86 (16)C15—C17—H17C109.5
C9—C8—C15123.49 (16)H17A—C17—H17B109.5
C3—C11—C12110.40 (15)H17A—C17—H17C109.5
C3—C11—C13112.15 (15)H17B—C17—H17C109.5
C3—C11—C14107.75 (14)C15—C16—H16A109.5
C13—C11—C12108.28 (16)C15—C16—H16B109.5
C14—C11—C12109.39 (15)C15—C16—H16C109.5
C14—C11—C13108.84 (16)H16A—C16—H16B109.5
C3—C4—H4119.7H16A—C16—H16C109.5
C5—C4—C3120.58 (15)H16B—C16—H16C109.5
C5—C4—H4119.7H19A—C19—H19B109.5
N1—C5—C6114.19 (14)H19A—C19—H19C109.5
N1—C5—C4121.35 (15)H19B—C19—H19C109.5
C4—C5—C6124.43 (14)C20—C19—H19A109.5
C3—C2—H2119.9C20—C19—H19B109.5
C1—C2—C3120.28 (16)C20—C19—H19C109.5
C1—C2—H2119.9N3—C20—C19178.4 (7)
V1—N2—C6—C7175.43 (12)C7—C6—C5—N1175.49 (16)
V1—N2—C6—C51.51 (18)C7—C6—C5—C42.7 (3)
V1—N2—C10—C9172.91 (14)C7—C8—C9—C100.7 (3)
V1—N1—C5—C60.61 (18)C7—C8—C15—C18178.11 (18)
V1—N1—C5—C4178.82 (12)C7—C8—C15—C1762.8 (2)
V1—N1—C1—C2177.27 (13)C7—C8—C15—C1656.8 (2)
O5i—V1—O2—V1i36.88 (3)C11—C3—C4—C5179.87 (15)
O5—S1—O3—V124.59 (12)C11—C3—C2—C1178.68 (16)
O3—V1—O2—V1i47.50 (4)C4—C3—C11—C1254.6 (2)
O3—S1—O5—V1i14.21 (15)C4—C3—C11—C13175.46 (16)
O6—S1—O5—V1i102.23 (13)C4—C3—C11—C1464.8 (2)
O6—S1—O3—V192.92 (11)C4—C3—C2—C10.4 (3)
O4—S1—O5—V1i136.79 (12)C5—N1—C1—C21.0 (3)
O4—S1—O3—V1149.72 (10)C5—C6—C7—C8174.54 (16)
O1—V1—O2—V1i148.59 (5)C2—C3—C11—C12127.22 (18)
N2—V1—O2—V1i68.14 (17)C2—C3—C11—C136.4 (2)
N2—C6—C7—C82.1 (3)C2—C3—C11—C14113.38 (19)
N2—C6—C5—N11.4 (2)C2—C3—C4—C51.9 (2)
N2—C6—C5—C4179.52 (15)C10—N2—C6—C70.7 (2)
N2—C10—C9—C82.1 (3)C10—N2—C6—C5176.23 (15)
N1—V1—O2—V1i115.25 (4)C9—C8—C15—C183.4 (3)
C3—C4—C5—N11.9 (2)C9—C8—C15—C17115.7 (2)
C3—C4—C5—C6176.08 (15)C9—C8—C15—C16124.7 (2)
C3—C2—C1—N11.0 (3)C1—N1—C5—C6177.74 (15)
C6—N2—C10—C91.4 (3)C1—N1—C5—C40.5 (2)
C6—C7—C8—C91.3 (3)C15—C8—C9—C10179.22 (18)
C6—C7—C8—C15177.25 (17)
Symmetry code: (i) x+5/4, y, z+5/4.
Hydrogen-bond geometry (Å, º) top
Cg2 is the centroid of the N2/C6–C10 ring.
D—H···AD—HH···AD···AD—H···A
C14—H14A···Cg2ii0.982.783.431 (2)124
Symmetry code: (ii) x+1, y+1, z+1.
BVS calculations for vanadium atoms of [V2O2(µ-O)(µ-H(SO4)2)(4,4'-tBubpy)2] (V2) top
BVS calculations were conducted using X-ray data of [V2O2(µ-O)(µ-H(SO4)2)(4,4'-tBubpy)2]. Bond-valence parameters: VIV—O (1.784 Å), VV—O (1.803 Å), and V—N (1.86 Å) (Brese et al., 1991).
[V2O2(µ-O)(µ-H(SO4)2)(4,4'-tBubpy)2]V1
V(IV)4.41
V(V)4.59
 

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