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The title complex, [VCl2(dtbeda)(thf)2] (dtbeda is N,N'-di-tert-butyl­ethane-1,2-di­amine), was prepared from the reaction of [V2Cl3(thf)6]2[Zn2Cl6] with dtbeda in refluxing thf. The crystal structure of [VCl2(dtbeda)(thf)2] exhibits chlorides in trans positions in a distorted octahedral geometry around the vanadium site. The asymmetric unit consists of one-half of the complex, which is located on a twofold rotation axis in space group C2/c.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803019743/ac6058sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803019743/ac6058Isup2.hkl
Contains datablock I

CCDC reference: 225685

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.053
  • wR factor = 0.137
  • Data-to-parameter ratio = 22.8

checkCIF/PLATON results

No syntax errors found


No errors found in this datablock

Computing details top

Cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL DENZO (Otwinowski & Minor,1997) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia,1999).

Dichlorobis(tetrahydrofuran)N,N'-di-tert-buthylethane-1,2-diaminevanadium(II) top
Crystal data top
[V(C4H8O)2(C8H22N2)Cl2]F(000) = 932
Mr = 436.34Dx = 1.275 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 16335 reflections
a = 20.915 (2) Åθ = 3.7–27.5°
b = 10.3733 (9) ŵ = 0.69 mm1
c = 11.4042 (13) ÅT = 173 K
β = 113.236 (5)°Prism, green
V = 2273.6 (4) Å30.2 × 0.2 × 0.15 mm
Z = 4
Data collection top
KappaCCD
diffractometer
2003 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.056
CCD scansθmax = 27.5°, θmin = 3.7°
Absorption correction: multi-scan
Blessing, 1995
h = 2427
Tmin = 0.813, Tmax = 0.903k = 1312
8029 measured reflectionsl = 1414
2597 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.137H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0475P)2 + 4.9995P]
where P = (Fo2 + 2Fc2)/3
2597 reflections(Δ/σ)max < 0.001
114 parametersΔρmax = 0.70 e Å3
0 restraintsΔρmin = 0.45 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell e.s.d.'s are taken

into account individually in the estimation of e.s.d.'s in distances, angles

and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V0.50.72388 (6)0.250.02631 (19)
Cl0.51710 (4)0.71992 (7)0.47867 (6)0.0351 (2)
O0.57366 (10)0.88754 (18)0.28900 (17)0.0328 (4)
N0.42839 (12)0.5557 (2)0.2406 (2)0.0314 (5)
C10.46139 (16)0.4410 (3)0.2102 (3)0.0372 (7)
H1A0.45310.44180.11850.045*
H1B0.44030.36160.22750.045*
C20.34990 (15)0.5559 (3)0.1762 (3)0.0355 (6)
C30.32379 (17)0.6618 (3)0.2383 (3)0.0445 (7)
H3A0.33880.64360.32960.067*
H3B0.27290.66510.19840.067*
H3C0.34290.74490.2270.067*
C40.32744 (17)0.5829 (3)0.0346 (3)0.0457 (8)
H4A0.34460.51420.00440.069*
H4B0.34670.66580.0230.069*
H4C0.27650.5860.00620.069*
C50.31879 (17)0.4263 (3)0.1948 (3)0.0441 (8)
H5A0.33460.35720.15410.066*
H5B0.26790.43130.15590.066*
H5C0.33420.40830.28620.066*
C60.61246 (17)0.9463 (3)0.4123 (3)0.0385 (7)
H6A0.65660.89960.45780.046*
H6B0.58490.94510.46560.046*
C70.6266 (2)1.0829 (3)0.3844 (3)0.0479 (8)
H7A0.671.11640.45120.057*
H7B0.58751.14080.37690.057*
C80.63345 (19)1.0683 (3)0.2581 (3)0.0465 (8)
H8A0.62441.15090.21080.056*
H8B0.68031.03680.27010.056*
C90.57848 (18)0.9702 (3)0.1900 (3)0.0414 (7)
H9A0.53331.01290.14180.05*
H9B0.59180.91940.12960.05*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V0.0372 (4)0.0225 (3)0.0222 (3)00.0149 (3)0
Cl0.0511 (5)0.0332 (4)0.0242 (3)0.0050 (3)0.0183 (3)0.0012 (3)
O0.0443 (12)0.0289 (10)0.0274 (10)0.0060 (8)0.0166 (9)0.0004 (8)
N0.0361 (13)0.0264 (11)0.0334 (12)0.0020 (9)0.0157 (10)0.0024 (9)
C10.0465 (17)0.0240 (13)0.0445 (17)0.0021 (12)0.0215 (14)0.0052 (12)
C20.0404 (16)0.0325 (15)0.0364 (15)0.0041 (12)0.0180 (13)0.0028 (12)
C30.0481 (19)0.0374 (17)0.057 (2)0.0007 (13)0.0299 (16)0.0042 (15)
C40.0437 (18)0.053 (2)0.0365 (17)0.0067 (14)0.0115 (14)0.0027 (14)
C50.0485 (19)0.0357 (16)0.0512 (19)0.0084 (13)0.0230 (16)0.0042 (14)
C60.0468 (18)0.0369 (16)0.0283 (14)0.0059 (13)0.0111 (13)0.0025 (12)
C70.064 (2)0.0353 (16)0.0398 (17)0.0114 (15)0.0161 (16)0.0028 (14)
C80.057 (2)0.0393 (17)0.0434 (18)0.0110 (14)0.0197 (16)0.0076 (14)
C90.059 (2)0.0339 (15)0.0341 (16)0.0096 (13)0.0213 (14)0.0058 (13)
Geometric parameters (Å, º) top
V—O2.2165 (19)C1—H1B0.990
V—Oi2.2165 (19)C3—H3A0.980
V—N2.274 (2)C3—H3B0.979
V—Ni2.274 (2)C3—H3C0.980
V—Cli2.4888 (7)C4—H4A0.980
V—Cl2.4888 (7)C4—H4B0.980
O—C91.453 (3)C4—H4C0.981
O—C61.451 (3)C5—H5A0.980
N—C11.483 (4)C5—H5B0.980
N—C21.511 (4)C5—H5C0.980
C1—C1i1.508 (6)C6—H6A0.989
C2—C31.520 (4)C6—H6B0.989
C2—C41.519 (4)C7—H7A0.990
C2—C51.544 (4)C7—H7B0.991
C6—C71.506 (4)C8—H8A0.990
C7—C81.511 (5)C8—H8A0.990
C8—C91.502 (4)C9—H9A0.991
C1—H1A0.990C9—H9B0.991
O—V—Oi80.02 (10)C3—C2—C4110.2 (3)
O—V—N171.80 (7)N—C2—C5111.6 (2)
O—V—Ni100.69 (8)C3—C2—C5108.4 (2)
O—V—Ni100.69 (8)C4—C2—C5109.6 (3)
Oi—V—Ni171.80 (7)O—C6—C7105.8 (2)
N—V—Ni79.80 (12)C6—C7—C8102.0 (3)
O—V—Cli91.38 (5)C9—C8—C7102.7 (3)
Oi—V—Cli90.07 (5)O—C9—C8105.8 (2)
N—V—Cli96.78 (6)N—C1—H1A109.65
Ni—V—Cli81.76 (6)N—C1—H1B109.61
O—V—Cl90.07 (5)C2—C3—H3A109.41
Oi—V—Cl91.38 (5)C2—C4—H4A109.47
N—V—Cl81.76 (6)C2—C5—H5A109.43
Ni—V—Cl96.78 (6)C2—C3—H3A109.41
Cli—V—Cl178.11 (4)C6—C7—H7A111.37
C9—O—C6108.7 (2)C7—C6—H6A110.65
C9—O—V123.51 (16)C7—C6—H6B110.61
C6—O—V126.51 (16)C9—C8—H8A111.21
C1—N—C2113.8 (2)C9—C8—H8B111.22
C1—N—V105.55 (16)C8—C9—H9A110.61
C2—N—V126.21 (17)C8—C9—H9B110.62
N—C1—C1i110.2 (2)O—C9—H9A110.59
N—C2—C3107.2 (2)O—C9—H9B110.56
N—C2—C4109.8 (2)O—C6—H6A110.61
Symmetry code: (i) x+1, y, z+1/2.
 

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