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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
CCDC reference: 225685
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (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
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 = 436.34 | Dx = 1.275 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 16335 reflections |
a = 20.915 (2) Å | θ = 3.7–27.5° |
b = 10.3733 (9) Å | µ = 0.69 mm−1 |
c = 11.4042 (13) Å | T = 173 K |
β = 113.236 (5)° | Prism, green |
V = 2273.6 (4) Å3 | 0.2 × 0.2 × 0.15 mm |
Z = 4 | |
Data collection top
KappaCCD diffractometer | 2003 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
CCD scans | θmax = 27.5°, θmin = 3.7° |
Absorption correction: multi-scan Blessing, 1995 | h = −24→27 |
Tmin = 0.813, Tmax = 0.903 | k = −13→12 |
8029 measured reflections | l = −14→14 |
2597 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.137 | H-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 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −0.45 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
V | 0.5 | 0.72388 (6) | 0.25 | 0.02631 (19) | |
Cl | 0.51710 (4) | 0.71992 (7) | 0.47867 (6) | 0.0351 (2) | |
O | 0.57366 (10) | 0.88754 (18) | 0.28900 (17) | 0.0328 (4) | |
N | 0.42839 (12) | 0.5557 (2) | 0.2406 (2) | 0.0314 (5) | |
C1 | 0.46139 (16) | 0.4410 (3) | 0.2102 (3) | 0.0372 (7) | |
H1A | 0.4531 | 0.4418 | 0.1185 | 0.045* | |
H1B | 0.4403 | 0.3616 | 0.2275 | 0.045* | |
C2 | 0.34990 (15) | 0.5559 (3) | 0.1762 (3) | 0.0355 (6) | |
C3 | 0.32379 (17) | 0.6618 (3) | 0.2383 (3) | 0.0445 (7) | |
H3A | 0.3388 | 0.6436 | 0.3296 | 0.067* | |
H3B | 0.2729 | 0.6651 | 0.1984 | 0.067* | |
H3C | 0.3429 | 0.7449 | 0.227 | 0.067* | |
C4 | 0.32744 (17) | 0.5829 (3) | 0.0346 (3) | 0.0457 (8) | |
H4A | 0.3446 | 0.5142 | −0.0044 | 0.069* | |
H4B | 0.3467 | 0.6658 | 0.023 | 0.069* | |
H4C | 0.2765 | 0.586 | −0.0062 | 0.069* | |
C5 | 0.31879 (17) | 0.4263 (3) | 0.1948 (3) | 0.0441 (8) | |
H5A | 0.3346 | 0.3572 | 0.1541 | 0.066* | |
H5B | 0.2679 | 0.4313 | 0.1559 | 0.066* | |
H5C | 0.3342 | 0.4083 | 0.2862 | 0.066* | |
C6 | 0.61246 (17) | 0.9463 (3) | 0.4123 (3) | 0.0385 (7) | |
H6A | 0.6566 | 0.8996 | 0.4578 | 0.046* | |
H6B | 0.5849 | 0.9451 | 0.4656 | 0.046* | |
C7 | 0.6266 (2) | 1.0829 (3) | 0.3844 (3) | 0.0479 (8) | |
H7A | 0.67 | 1.1164 | 0.4512 | 0.057* | |
H7B | 0.5875 | 1.1408 | 0.3769 | 0.057* | |
C8 | 0.63345 (19) | 1.0683 (3) | 0.2581 (3) | 0.0465 (8) | |
H8A | 0.6244 | 1.1509 | 0.2108 | 0.056* | |
H8B | 0.6803 | 1.0368 | 0.2701 | 0.056* | |
C9 | 0.57848 (18) | 0.9702 (3) | 0.1900 (3) | 0.0414 (7) | |
H9A | 0.5333 | 1.0129 | 0.1418 | 0.05* | |
H9B | 0.5918 | 0.9194 | 0.1296 | 0.05* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V | 0.0372 (4) | 0.0225 (3) | 0.0222 (3) | 0 | 0.0149 (3) | 0 |
Cl | 0.0511 (5) | 0.0332 (4) | 0.0242 (3) | −0.0050 (3) | 0.0183 (3) | −0.0012 (3) |
O | 0.0443 (12) | 0.0289 (10) | 0.0274 (10) | −0.0060 (8) | 0.0166 (9) | 0.0004 (8) |
N | 0.0361 (13) | 0.0264 (11) | 0.0334 (12) | −0.0020 (9) | 0.0157 (10) | −0.0024 (9) |
C1 | 0.0465 (17) | 0.0240 (13) | 0.0445 (17) | −0.0021 (12) | 0.0215 (14) | −0.0052 (12) |
C2 | 0.0404 (16) | 0.0325 (15) | 0.0364 (15) | −0.0041 (12) | 0.0180 (13) | −0.0028 (12) |
C3 | 0.0481 (19) | 0.0374 (17) | 0.057 (2) | −0.0007 (13) | 0.0299 (16) | −0.0042 (15) |
C4 | 0.0437 (18) | 0.053 (2) | 0.0365 (17) | −0.0067 (14) | 0.0115 (14) | −0.0027 (14) |
C5 | 0.0485 (19) | 0.0357 (16) | 0.0512 (19) | −0.0084 (13) | 0.0230 (16) | −0.0042 (14) |
C6 | 0.0468 (18) | 0.0369 (16) | 0.0283 (14) | −0.0059 (13) | 0.0111 (13) | −0.0025 (12) |
C7 | 0.064 (2) | 0.0353 (16) | 0.0398 (17) | −0.0114 (15) | 0.0161 (16) | −0.0028 (14) |
C8 | 0.057 (2) | 0.0393 (17) | 0.0434 (18) | −0.0110 (14) | 0.0197 (16) | 0.0076 (14) |
C9 | 0.059 (2) | 0.0339 (15) | 0.0341 (16) | −0.0096 (13) | 0.0213 (14) | 0.0058 (13) |
Geometric parameters (Å, º) top
V—O | 2.2165 (19) | C1—H1B | 0.990 |
V—Oi | 2.2165 (19) | C3—H3A | 0.980 |
V—N | 2.274 (2) | C3—H3B | 0.979 |
V—Ni | 2.274 (2) | C3—H3C | 0.980 |
V—Cli | 2.4888 (7) | C4—H4A | 0.980 |
V—Cl | 2.4888 (7) | C4—H4B | 0.980 |
O—C9 | 1.453 (3) | C4—H4C | 0.981 |
O—C6 | 1.451 (3) | C5—H5A | 0.980 |
N—C1 | 1.483 (4) | C5—H5B | 0.980 |
N—C2 | 1.511 (4) | C5—H5C | 0.980 |
C1—C1i | 1.508 (6) | C6—H6A | 0.989 |
C2—C3 | 1.520 (4) | C6—H6B | 0.989 |
C2—C4 | 1.519 (4) | C7—H7A | 0.990 |
C2—C5 | 1.544 (4) | C7—H7B | 0.991 |
C6—C7 | 1.506 (4) | C8—H8A | 0.990 |
C7—C8 | 1.511 (5) | C8—H8A | 0.990 |
C8—C9 | 1.502 (4) | C9—H9A | 0.991 |
C1—H1A | 0.990 | C9—H9B | 0.991 |
| | | |
O—V—Oi | 80.02 (10) | C3—C2—C4 | 110.2 (3) |
O—V—N | 171.80 (7) | N—C2—C5 | 111.6 (2) |
O—V—Ni | 100.69 (8) | C3—C2—C5 | 108.4 (2) |
O—V—Ni | 100.69 (8) | C4—C2—C5 | 109.6 (3) |
Oi—V—Ni | 171.80 (7) | O—C6—C7 | 105.8 (2) |
N—V—Ni | 79.80 (12) | C6—C7—C8 | 102.0 (3) |
O—V—Cli | 91.38 (5) | C9—C8—C7 | 102.7 (3) |
Oi—V—Cli | 90.07 (5) | O—C9—C8 | 105.8 (2) |
N—V—Cli | 96.78 (6) | N—C1—H1A | 109.65 |
Ni—V—Cli | 81.76 (6) | N—C1—H1B | 109.61 |
O—V—Cl | 90.07 (5) | C2—C3—H3A | 109.41 |
Oi—V—Cl | 91.38 (5) | C2—C4—H4A | 109.47 |
N—V—Cl | 81.76 (6) | C2—C5—H5A | 109.43 |
Ni—V—Cl | 96.78 (6) | C2—C3—H3A | 109.41 |
Cli—V—Cl | 178.11 (4) | C6—C7—H7A | 111.37 |
C9—O—C6 | 108.7 (2) | C7—C6—H6A | 110.65 |
C9—O—V | 123.51 (16) | C7—C6—H6B | 110.61 |
C6—O—V | 126.51 (16) | C9—C8—H8A | 111.21 |
C1—N—C2 | 113.8 (2) | C9—C8—H8B | 111.22 |
C1—N—V | 105.55 (16) | C8—C9—H9A | 110.61 |
C2—N—V | 126.21 (17) | C8—C9—H9B | 110.62 |
N—C1—C1i | 110.2 (2) | O—C9—H9A | 110.59 |
N—C2—C3 | 107.2 (2) | O—C9—H9B | 110.56 |
N—C2—C4 | 109.8 (2) | O—C6—H6A | 110.61 |
Symmetry code: (i) −x+1, y, −z+1/2. |
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