Buy article online - an online subscription or single-article purchase is required to access this article.
In the title compound, [VOCl2(C9H21N3)], the V atom is at the center of a distorted octahedral coordination sphere and is coordinated by the three N atoms of the N,N′,N′′-trimethyl-1,4,7-triazacyclononane (Me3tacn) ligand, and by two chlorides and an oxo ligand.
Supporting information
CCDC reference: 189870
Key indicators
- Single-crystal X-ray study
- T = 141 K
- Mean (C-C) = 0.007 Å
- R factor = 0.038
- wR factor = 0.108
- Data-to-parameter ratio = 14.8
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level B:
ABSTM_02 Alert B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
Tmin and Tmax reported: 0.480 0.920
Tmin' and Tmax expected: 0.832 0.894
RR' = 0.560
Please check that your absorption correction is appropriate.
| Author response: The absorption corrections were applied using SADABS.
|
REFLT_03
From the CIF: _diffrn_reflns_theta_max 25.44
From the CIF: _reflns_number_total 2167
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 2478
Completeness (_total/calc) 87.45%
Alert B: < 90% complete (theta max?)
| Author response: High angle data were lost due to the twinning within the crystal.
Perhaps a resolution cutoff at 0.9 \%A should have been applied.
|
SYMMS_02 Alert B All angles should not be 90 for a monoclinic cell
Cell 13.6069 7.7759 12.6586
Angles 90.0000 90.0000 90.0000
| Author response: We believe that the real \b is somewhere between 89.9 and 90.1\%.
However, due to twinning, the angle is indistinguishable from 90\%.
|
Alert Level C:
GOODF_01 Alert C The least squares goodness of fit parameter lies
outside the range 0.80 <> 2.00
Goodness of fit given = 0.718
0 Alert Level A = Potentially serious problem
3 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1995); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Crystal data top
[VCl2O(C9H21N3)] | F(000) = 644 |
Mr = 309.13 | Dx = 1.533 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 13.6069 (15) Å | Cell parameters from 5166 reflections |
b = 7.7759 (8) Å | θ = 1.7–25.4° |
c = 12.6586 (14) Å | µ = 1.12 mm−1 |
β = 90.000 (2)° | T = 141 K |
V = 1339.4 (3) Å3 | Plate, blue |
Z = 4 | 0.16 × 0.12 × 0.10 mm |
Data collection top
Siemens SMART CCD diffractometer | 2167 independent reflections |
Radiation source: fine-focus sealed tube | 1929 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
ω scans | θmax = 25.4°, θmin = 1.6° |
Absorption correction: empirical (using intensity measurements) (Blessing, 1995) | h = −15→16 |
Tmin = 0.48, Tmax = 0.92 | k = −6→9 |
5156 measured reflections | l = −14→13 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 0.76 | w = 1/[σ2(Fo2) + (0.XXXXP)2 + 0.XXXXP] where P = (Fo2 + 2Fc2)/3 |
2167 reflections | (Δ/σ)max = −0.002 |
146 parameters | Δρmax = 0.30 e Å−3 |
0 restraints | Δρmin = −0.53 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 on F2 for ALL reflections except for 0 with very negative
F2 or flagged by the user for potential systematic errors. Weighted
R-factors wR and all goodnesses of fit S are based on
F2, conventional R-factors R are based on F,
with F set to zero for negative F2. The observed criterion of
F2 > σ(F2) is used only for calculating _R_factor_obs
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 | |
V1 | 0.25222 (5) | 0.00902 (8) | 0.39124 (5) | 0.0157 (2) | |
Cl1 | 0.11854 (8) | 0.19963 (14) | 0.40875 (10) | 0.0260 (3) | |
Cl2 | 0.36795 (7) | 0.23401 (13) | 0.40500 (10) | 0.0226 (3) | |
O1 | 0.2600 (2) | −0.0728 (3) | 0.5101 (2) | 0.0226 (7) | |
N1 | 0.3651 (3) | −0.1634 (4) | 0.3269 (3) | 0.0202 (8) | |
N2 | 0.1595 (3) | −0.2037 (5) | 0.3376 (3) | 0.0248 (9) | |
N3 | 0.2414 (3) | 0.0524 (4) | 0.2080 (3) | 0.0206 (8) | |
C1 | 0.3226 (3) | −0.3362 (6) | 0.3040 (4) | 0.0269 (11) | |
H1A | 0.3687 (3) | −0.4265 (6) | 0.3283 (4) | 0.032* | |
H1B | 0.3137 (3) | −0.3495 (6) | 0.2268 (4) | 0.032* | |
C2 | 0.2251 (4) | −0.3582 (6) | 0.3587 (4) | 0.0311 (11) | |
H2A | 0.2357 (4) | −0.3705 (6) | 0.4357 (4) | 0.037* | |
H2B | 0.1926 (4) | −0.4640 (6) | 0.3328 (4) | 0.037* | |
C3 | 0.1306 (4) | −0.1977 (6) | 0.2241 (4) | 0.0303 (11) | |
H3A | 0.0611 (4) | −0.2334 (6) | 0.2168 (4) | 0.036* | |
H3B | 0.1716 (4) | −0.2791 (6) | 0.1833 (4) | 0.036* | |
C4 | 0.1433 (4) | −0.0183 (6) | 0.1803 (4) | 0.0282 (12) | |
H4A | 0.1360 (4) | −0.0211 (6) | 0.1025 (4) | 0.034* | |
H4B | 0.0914 (4) | 0.0576 (6) | 0.2092 (4) | 0.034* | |
C5 | 0.3221 (3) | −0.0412 (6) | 0.1517 (4) | 0.0242 (11) | |
H5A | 0.3476 (3) | 0.0312 (6) | 0.0935 (4) | 0.029* | |
H5B | 0.2959 (3) | −0.1487 (6) | 0.1207 (4) | 0.029* | |
C6 | 0.4042 (3) | −0.0833 (6) | 0.2271 (4) | 0.0264 (10) | |
H6A | 0.4406 (3) | 0.0231 (6) | 0.2448 (4) | 0.032* | |
H6B | 0.4506 (3) | −0.1639 (6) | 0.1927 (4) | 0.032* | |
C8 | 0.0703 (3) | −0.2201 (7) | 0.4053 (5) | 0.0361 (13) | |
H7A | 0.0899 (3) | −0.2240 (7) | 0.4798 (5) | 0.054* | |
H7B | 0.0351 (3) | −0.3260 (7) | 0.3870 (5) | 0.054* | |
H7C | 0.0271 (3) | −0.1209 (7) | 0.3936 (5) | 0.054* | |
C9 | 0.2433 (4) | 0.2367 (5) | 0.1748 (4) | 0.0304 (11) | |
H8A | 0.3074 (4) | 0.2867 (5) | 0.1922 (4) | 0.046* | |
H8B | 0.1915 (4) | 0.2999 (5) | 0.2119 (4) | 0.046* | |
H8C | 0.2323 (4) | 0.2443 (5) | 0.0984 (4) | 0.046* | |
C7 | 0.4481 (3) | −0.1820 (6) | 0.4022 (5) | 0.0299 (11) | |
H9A | 0.4761 (3) | −0.0685 (6) | 0.4174 (5) | 0.045* | |
H9B | 0.4987 (3) | −0.2559 (6) | 0.3711 (5) | 0.045* | |
H9C | 0.4242 (3) | −0.2338 (6) | 0.4680 (5) | 0.045* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0149 (4) | 0.0153 (4) | 0.0168 (4) | −0.0008 (3) | 0.0010 (6) | −0.0010 (2) |
Cl1 | 0.0190 (5) | 0.0320 (6) | 0.0271 (7) | 0.0077 (4) | 0.0012 (5) | −0.0048 (5) |
Cl2 | 0.0202 (5) | 0.0197 (5) | 0.0279 (7) | −0.0061 (4) | 0.0005 (5) | −0.0021 (4) |
O1 | 0.028 (2) | 0.0153 (13) | 0.025 (2) | −0.0027 (14) | 0.005 (2) | 0.0032 (11) |
N1 | 0.023 (2) | 0.017 (2) | 0.021 (2) | 0.004 (2) | 0.000 (2) | −0.0011 (15) |
N2 | 0.026 (2) | 0.028 (2) | 0.021 (2) | −0.009 (2) | 0.004 (2) | −0.001 (2) |
N3 | 0.022 (2) | 0.019 (2) | 0.021 (2) | 0.006 (2) | 0.004 (2) | 0.0027 (13) |
C1 | 0.036 (3) | 0.014 (2) | 0.031 (3) | 0.007 (2) | −0.004 (2) | −0.002 (2) |
C2 | 0.041 (3) | 0.020 (2) | 0.033 (3) | −0.006 (2) | 0.001 (2) | 0.000 (2) |
C3 | 0.028 (3) | 0.041 (3) | 0.022 (3) | −0.011 (2) | −0.002 (2) | −0.008 (2) |
C4 | 0.029 (3) | 0.036 (3) | 0.020 (3) | 0.006 (2) | −0.011 (2) | −0.004 (2) |
C5 | 0.031 (3) | 0.022 (2) | 0.020 (3) | 0.006 (2) | 0.009 (2) | 0.002 (2) |
C6 | 0.024 (2) | 0.025 (3) | 0.031 (3) | 0.002 (2) | 0.007 (2) | −0.006 (2) |
C8 | 0.030 (3) | 0.050 (3) | 0.028 (3) | −0.017 (2) | 0.005 (3) | −0.007 (3) |
C9 | 0.050 (3) | 0.019 (2) | 0.023 (2) | 0.002 (3) | 0.002 (3) | 0.003 (2) |
C7 | 0.028 (2) | 0.027 (2) | 0.035 (3) | 0.011 (2) | −0.009 (3) | −0.006 (2) |
Geometric parameters (Å, º) top
V1—O1 | 1.637 (3) | C3—C4 | 1.511 (7) |
V1—N2 | 2.189 (4) | C3—H3A | 0.99 |
V1—N1 | 2.195 (4) | C3—H3B | 0.99 |
V1—N3 | 2.349 (4) | C4—H4A | 0.99 |
V1—Cl1 | 2.3569 (12) | C4—H4B | 0.99 |
V1—Cl2 | 2.3603 (12) | C5—C6 | 1.505 (7) |
N1—C7 | 1.486 (6) | C5—H5A | 0.99 |
N1—C1 | 1.491 (5) | C5—H5B | 0.99 |
N1—C6 | 1.505 (6) | C6—H6A | 0.99 |
N2—C3 | 1.491 (6) | C6—H6B | 0.99 |
N2—C8 | 1.491 (6) | C8—H7A | 0.98 |
N2—C2 | 1.520 (6) | C8—H7B | 0.98 |
N3—C4 | 1.486 (6) | C8—H7C | 0.98 |
N3—C9 | 1.493 (5) | C9—H8A | 0.98 |
N3—C5 | 1.498 (5) | C9—H8B | 0.98 |
C1—C2 | 1.507 (7) | C9—H8C | 0.98 |
C1—H1A | 0.99 | C7—H9A | 0.98 |
C1—H1B | 0.99 | C7—H9B | 0.98 |
C2—H2A | 0.99 | C7—H9C | 0.98 |
C2—H2B | 0.99 | | |
| | | |
O1—V1—N2 | 91.63 (15) | H2A—C2—H2B | 108.1 |
O1—V1—N1 | 93.34 (14) | N2—C3—C4 | 110.7 (4) |
N2—V1—N1 | 80.02 (13) | N2—C3—H3A | 109.5 (2) |
O1—V1—N3 | 165.38 (13) | C4—C3—H3A | 109.5 (3) |
N2—V1—N3 | 76.49 (14) | N2—C3—H3B | 109.5 (2) |
N1—V1—N3 | 76.41 (13) | C4—C3—H3B | 109.5 (3) |
O1—V1—Cl1 | 102.02 (11) | H3A—C3—H3B | 108.1 |
N2—V1—Cl1 | 93.41 (11) | N3—C4—C3 | 111.0 (4) |
N1—V1—Cl1 | 163.50 (11) | N3—C4—H4A | 109.4 (3) |
N3—V1—Cl1 | 87.36 (9) | C3—C4—H4A | 109.4 (3) |
O1—V1—Cl2 | 100.19 (11) | N3—C4—H4B | 109.4 (2) |
N2—V1—Cl2 | 165.44 (11) | C3—C4—H4B | 109.4 (3) |
N1—V1—Cl2 | 90.76 (10) | H4A—C4—H4B | 108.0 |
N3—V1—Cl2 | 90.47 (10) | N3—C5—C6 | 110.4 (4) |
Cl1—V1—Cl2 | 92.40 (4) | N3—C5—H5A | 109.6 (2) |
C7—N1—C1 | 109.4 (4) | C6—C5—H5A | 109.6 (3) |
C7—N1—C6 | 108.1 (3) | N3—C5—H5B | 109.6 (2) |
C1—N1—C6 | 110.3 (4) | C6—C5—H5B | 109.6 (2) |
C7—N1—V1 | 110.7 (3) | H5A—C5—H5B | 108.1 |
C1—N1—V1 | 110.6 (3) | C5—C6—N1 | 111.0 (4) |
C6—N1—V1 | 107.8 (3) | C5—C6—H6A | 109.4 (2) |
C3—N2—C8 | 110.0 (4) | N1—C6—H6A | 109.4 (2) |
C3—N2—C2 | 110.5 (4) | C5—C6—H6B | 109.4 (2) |
C8—N2—C2 | 108.1 (4) | N1—C6—H6B | 109.4 (2) |
C3—N2—V1 | 115.3 (3) | H6A—C6—H6B | 108.0 |
C8—N2—V1 | 110.8 (3) | N2—C8—H7A | 109.5 (3) |
C2—N2—V1 | 101.8 (3) | N2—C8—H7B | 109.5 (2) |
C4—N3—C9 | 107.7 (4) | H7A—C8—H7B | 109.5 |
C4—N3—C5 | 111.5 (4) | N2—C8—H7C | 109.5 (3) |
C9—N3—C5 | 108.6 (3) | H7A—C8—H7C | 109.5 |
C4—N3—V1 | 103.7 (3) | H7B—C8—H7C | 109.5 |
C9—N3—V1 | 114.5 (3) | N3—C9—H8A | 109.5 (2) |
C5—N3—V1 | 110.7 (3) | N3—C9—H8B | 109.5 (2) |
N1—C1—C2 | 110.7 (3) | H8A—C9—H8B | 109.5 |
N1—C1—H1A | 109.5 (2) | N3—C9—H8C | 109.5 (2) |
C2—C1—H1A | 109.5 (2) | H8A—C9—H8C | 109.5 |
N1—C1—H1B | 109.5 (2) | H8B—C9—H8C | 109.5 |
C2—C1—H1B | 109.5 (3) | N1—C7—H9A | 109.5 (2) |
H1A—C1—H1B | 108.1 | N1—C7—H9B | 109.5 (2) |
C1—C2—N2 | 110.3 (4) | H9A—C7—H9B | 109.5 |
C1—C2—H2A | 109.6 (3) | N1—C7—H9C | 109.5 (3) |
N2—C2—H2A | 109.6 (3) | H9A—C7—H9C | 109.5 |
C1—C2—H2B | 109.6 (2) | H9B—C7—H9C | 109.5 |
N2—C2—H2B | 109.6 (2) | | |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.