Di­chloro­oxo(N,N′,N′′-tri­methyl-1,4,7-tri­aza­cyclo­nonane-κ3N)­vanadium(IV)

Fiedler, D.; Miljanić, O.S.; Welch, E.J.

doi:10.1107/S160053680201053X

Dichlorooxo(N,N′,N′′-trimethyl-1,4,7-triazacyclononane-κ³N)vanadium(IV)

D. Fiedler, O. S. Miljanić and E. J. Welch

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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201053X/ob6133sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680201053X/ob6133Isup2.hkl Contains datablock I

CCDC reference: 189870

checkCIF report

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

Computing details top

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).

(I) top

Crystal data top

[VCl₂O(C₉H₂₁N₃)]	F(000) = 644
M_r = 309.13	D_x = 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	R_int = 0.046
ω scans	θ_max = 25.4°, θ_min = 1.6°
Absorption correction: empirical (using intensity measurements) (Blessing, 1995)	h = −15→16
T_min = 0.48, T_max = 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(F_o²) + (0.XXXXP)² + 0.XXXXP] where P = (F_o² + 2F_c²)/3
2167 reflections	(Δ/σ)_max = −0.002
146 parameters	Δρ_max = 0.30 e Å⁻³
0 restraints	Δρ_min = −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	U_iso*/U_eq
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)

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Di­chloro­oxo(N,N′,N′′-tri­methyl-1,4,7-tri­aza­cyclo­nonane-κ3N)­vanadium(IV)

Supporting information

Key indicators

checkCIF results

Dichlorooxo(N,N′,N′′-trimethyl-1,4,7-triazacyclononane-κ³N)vanadium(IV)