Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201053X/ob6133sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680201053X/ob6133Isup2.hkl |
CCDC reference: 189870
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).
[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 |
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 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 |
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. |
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* |
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) |
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) |