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The octahedral title compound, [Ru(C2H5O)(NO)(NO2)2(C6H16N2)], crystallizes in the rhombohedral space group P31 with an ethoxy ligand axially coordinated trans to the nitrosyl ligand. The RuII ion is equatorially coordinated by a tetramethylethylenediamine group acting as a bidentate ligand, and to two nitro moieties whose planes are tilted with respect to the mean equatorial plane. Each nitrogen ligand bonded to the metallic centre has a different hybridization state.
Supporting information
CCDC reference: 184468
Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms, 1995); 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 (Farrugia, 1999).
ethoxydinitronitrosyl(
N,
N,
N',
N'-tetramethylethylendiamine-
κ2N,
N')ruthenium(II)
top
Crystal data top
[Ru(C6H16N2)(C2H5O)NO(NO2)2] | Dx = 1.740 Mg m−3 |
Mr = 384.37 | Cu Kα radiation, λ = 1.5418 Å |
Trigonal, P31 | Cell parameters from 25 reflections |
a = 7.930 (2) Å | θ = 10.1–21.6° |
c = 20.210 (9) Å | µ = 8.97 mm−1 |
V = 1100.6 (6) Å3 | T = 293 K |
Z = 3 | Prism, dark orange |
F(000) = 588 | 0.08 × 0.06 × 0.06 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 1431 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.045 |
Graphite monochromator | θmax = 69.8°, θmin = 6.5° |
non–profiled ω/2θ scans | h = 0→9 |
Absorption correction: ψ-scan (North et al., 1968) | k = −9→0 |
Tmin = 0.439, Tmax = 0.566 | l = 0→24 |
1593 measured reflections | 1 standard reflections every 30 min |
1439 independent reflections | intensity decay: 1% |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.035 | H-atom parameters constrained |
wR(F2) = 0.094 | w = 1/[σ2(Fo2) + (0.0392P)2 + 4.2825P] where P = (Fo2 + 2Fc2)/3 |
S = 1.15 | (Δ/σ)max < 0.001 |
1439 reflections | Δρmax = 0.87 e Å−3 |
207 parameters | Δρmin = −1.72 e Å−3 |
1 restraint | Absolute structure: Flack (1983) |
Primary atom site location: Patterson | Absolute structure parameter: 0.04 (2) |
Special details top
Experimental. Spectroscopic analysis: IR (KBr disc, νN—O, cm-1): 1832; 1H NMR
(CDCl3, δ, p.p.m.): 4.72 (q, 2H, CH2 in OEt), 3.02 (t, 3H, CH3 in OEt),
2.89 (s, 6H, CH3 in TMED), 2.79 (m, 4H, CH2 in TMED), 2.71 (s, 6H, CH3
in TMED). IR spectra were recorded on a Nicolet FTIR 510P. 1H NMR spectra
were run on a 200 MHz Bruker AC200 instrument in a CDCl3 solution, using the
solvent peak as the internal reference (δ 7.26 p.p.m.). |
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 | |
Ru | 0.43700 (8) | 0.20021 (8) | 0.00000 (5) | 0.02372 (18) | |
N1 | 0.4983 (13) | 0.0822 (14) | −0.0608 (4) | 0.038 (2) | |
O1 | 0.5637 (17) | 0.0251 (18) | −0.1000 (5) | 0.071 (3) | |
N2 | 0.2107 (12) | −0.0682 (13) | 0.0478 (4) | 0.0286 (18) | |
C21 | 0.239 (2) | −0.0613 (17) | 0.1218 (5) | 0.048 (3) | |
H21A | 0.2213 | 0.0407 | 0.1402 | 0.03 (3)* | |
H21B | 0.3676 | −0.0363 | 0.1316 | 0.03 (3)* | |
H21C | 0.1448 | −0.1838 | 0.1408 | 0.05 (3)* | |
C22 | 0.2091 (18) | −0.2452 (15) | 0.0225 (6) | 0.044 (3) | |
H22A | 0.1139 | −0.3573 | 0.0464 | 0.3 (2)* | |
H22B | 0.3354 | −0.2315 | 0.0286 | 0.05 (4)* | |
H22C | 0.1769 | −0.2611 | −0.0237 | 0.02 (2)* | |
C3 | 0.0201 (13) | −0.0222 (15) | −0.0373 (5) | 0.036 (2) | |
H3A | 0.0240 | −0.1188 | −0.0657 | 0.03 (3)* | |
H3B | −0.1016 | −0.0244 | −0.0455 | 0.02 (2)* | |
N3 | 0.1868 (12) | 0.1751 (13) | −0.0540 (4) | 0.0307 (19) | |
C31 | 0.1358 (17) | 0.3233 (17) | −0.0339 (6) | 0.040 (3) | |
H31A | 0.2507 | 0.4497 | −0.0343 | 0.05 (3)* | |
H31B | 0.0817 | 0.2947 | 0.0099 | 0.06 (4)* | |
H31C | 0.0418 | 0.3218 | −0.0642 | 0.05 (4)* | |
C32 | 0.2190 (18) | 0.1934 (19) | −0.1263 (5) | 0.044 (3) | |
H32A | 0.1044 | 0.1780 | −0.1480 | 0.10 (6)* | |
H32B | 0.2460 | 0.0946 | −0.1415 | 0.03 (3)* | |
H32C | 0.3274 | 0.3195 | −0.1364 | 0.03 (3)* | |
C4 | 0.0276 (15) | −0.0732 (17) | 0.0336 (6) | 0.039 (2) | |
H4A | 0.0153 | 0.0185 | 0.0621 | 0.03 (3)* | |
H4B | −0.0806 | −0.2023 | 0.0427 | 0.02 (2)* | |
N4 | 0.6666 (16) | 0.2117 (15) | 0.0561 (5) | 0.041 (2) | |
O3 | 0.6836 (14) | 0.0656 (16) | 0.0570 (5) | 0.063 (3) | |
O4 | 0.7794 (14) | 0.3582 (17) | 0.0852 (6) | 0.067 (3) | |
N5 | 0.6303 (14) | 0.4645 (14) | −0.0460 (5) | 0.039 (2) | |
O5 | 0.7857 (15) | 0.4861 (16) | −0.0653 (7) | 0.073 (3) | |
O6 | 0.5938 (13) | 0.5947 (12) | −0.0521 (5) | 0.062 (2) | |
O2 | 0.3778 (10) | 0.3238 (10) | 0.0693 (3) | 0.0348 (15) | |
C5 | 0.4808 (17) | 0.5047 (16) | 0.1020 (6) | 0.046 (3) | |
H5A | 0.5187 | 0.6104 | 0.0706 | 0.01 (2)* | |
H5B | 0.5975 | 0.5179 | 0.1224 | 0.04 (3)* | |
C6 | 0.349 (2) | 0.5116 (18) | 0.1536 (6) | 0.050 (3) | |
H6A | 0.3143 | 0.4077 | 0.1847 | 0.08 (5)* | |
H6B | 0.2338 | 0.4972 | 0.1329 | 0.27 (19)* | |
H6C | 0.4154 | 0.6342 | 0.1763 | 0.07 (4)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ru | 0.0176 (3) | 0.0227 (3) | 0.0271 (3) | 0.0073 (2) | 0.0013 (2) | −0.0003 (3) |
N1 | 0.031 (4) | 0.043 (5) | 0.040 (5) | 0.017 (4) | 0.002 (4) | −0.006 (4) |
O1 | 0.086 (7) | 0.101 (8) | 0.050 (6) | 0.066 (7) | 0.009 (5) | −0.022 (5) |
N2 | 0.020 (4) | 0.032 (4) | 0.036 (5) | 0.014 (4) | 0.002 (3) | 0.007 (4) |
C21 | 0.059 (7) | 0.041 (6) | 0.031 (6) | 0.014 (5) | 0.013 (5) | 0.011 (5) |
C22 | 0.057 (7) | 0.029 (5) | 0.047 (6) | 0.021 (5) | −0.002 (5) | −0.003 (5) |
C3 | 0.020 (4) | 0.032 (5) | 0.045 (6) | 0.005 (4) | −0.003 (4) | 0.003 (4) |
N3 | 0.022 (4) | 0.033 (4) | 0.030 (4) | 0.008 (3) | 0.003 (3) | 0.001 (3) |
C31 | 0.040 (6) | 0.039 (6) | 0.041 (6) | 0.020 (5) | −0.006 (5) | 0.000 (5) |
C32 | 0.049 (6) | 0.053 (7) | 0.033 (6) | 0.028 (6) | −0.006 (5) | 0.002 (5) |
C4 | 0.028 (5) | 0.033 (5) | 0.055 (7) | 0.013 (4) | 0.003 (5) | 0.006 (5) |
N4 | 0.042 (5) | 0.039 (5) | 0.045 (5) | 0.024 (5) | −0.008 (4) | −0.005 (4) |
O3 | 0.059 (6) | 0.080 (7) | 0.069 (6) | 0.047 (6) | −0.009 (5) | 0.003 (5) |
O4 | 0.040 (5) | 0.076 (7) | 0.084 (8) | 0.027 (5) | −0.022 (5) | −0.016 (6) |
N5 | 0.031 (5) | 0.038 (5) | 0.033 (5) | 0.007 (4) | −0.004 (4) | −0.001 (4) |
O5 | 0.036 (5) | 0.060 (6) | 0.109 (9) | 0.014 (4) | 0.026 (6) | 0.020 (6) |
O6 | 0.060 (5) | 0.035 (4) | 0.080 (6) | 0.015 (4) | 0.018 (5) | 0.022 (4) |
O2 | 0.036 (4) | 0.034 (4) | 0.032 (4) | 0.015 (3) | 0.003 (3) | −0.004 (3) |
C5 | 0.045 (6) | 0.035 (6) | 0.051 (7) | 0.013 (5) | −0.001 (5) | −0.019 (5) |
C6 | 0.070 (8) | 0.047 (6) | 0.041 (6) | 0.036 (6) | −0.002 (5) | −0.008 (5) |
Geometric parameters (Å, º) top
Ru—N1 | 1.754 (9) | C21—H21B | 0.96 |
Ru—O2 | 1.898 (7) | C21—H21C | 0.96 |
Ru—N5 | 2.10 (1) | C22—H22A | 0.96 |
Ru—N4 | 2.11 (1) | C22—H22B | 0.96 |
Ru—N3 | 2.185 (9) | C22—H22C | 0.96 |
Ru—N2 | 2.205 (9) | C3—H3A | 0.97 |
N1—O1 | 1.16 (1) | C3—H3B | 0.97 |
N2—C4 | 1.46 (1) | C31—H31A | 0.96 |
N2—C22 | 1.49 (1) | C31—H31B | 0.96 |
N2—C21 | 1.51 (1) | C31—H31C | 0.96 |
C3—N3 | 1.50 (1) | C32—H32A | 0.96 |
C3—C4 | 1.50 (2) | C32—H32B | 0.96 |
N3—C32 | 1.48 (1) | C32—H32C | 0.96 |
N3—C31 | 1.48 (2) | C4—H4A | 0.97 |
N4—O4 | 1.21 (1) | C4—H4B | 0.97 |
N4—O3 | 1.23 (1) | C5—H5A | 0.97 |
N5—O6 | 1.21 (1) | C5—H5B | 0.97 |
N5—O5 | 1.22 (1) | C6—H6A | 0.96 |
O2—C5 | 1.41 (1) | C6—H6B | 0.96 |
C5—C6 | 1.50 (2) | C6—H6C | 0.96 |
C21—H21A | 0.96 | | |
| | | |
N1—Ru—O2 | 176.8 (4) | C5—O2—Ru | 134.7 (7) |
N1—Ru—N5 | 87.9 (4) | O2—C5—C6 | 107.7 (9) |
O2—Ru—N5 | 93.3 (4) | H21A—C21—H21B | 109.5 (12) |
N1—Ru—N4 | 86.3 (4) | H21A—C21—H21C | 109.5 (13) |
O2—Ru—N4 | 90.7 (4) | H21B—C21—H21C | 109.5 (12) |
N5—Ru—N4 | 90.6 (4) | H22A—C22—H22B | 109.5 (12) |
N1—Ru—N3 | 94.7 (4) | H22A—C22—H22C | 109.5 (12) |
O2—Ru—N3 | 88.2 (3) | H22B—C22—H22C | 109.5 (13) |
N5—Ru—N3 | 92.7 (3) | H3A—C3—H3B | 108.0 (10) |
N4—Ru—N3 | 176.6 (4) | H3A—C3—C4 | 109.4 (10) |
N1—Ru—N2 | 95.8 (4) | H3B—C3—C4 | 109.4 (10) |
O2—Ru—N2 | 83.3 (3) | N3—C3—H3A | 109.4 (10) |
N5—Ru—N2 | 174.0 (4) | N3—C3—H3B | 109.3 (10) |
N4—Ru—N2 | 94.3 (4) | H31A—C31—H31B | 109.5 (12) |
N3—Ru—N2 | 82.4 (3) | H31A—C31—H31C | 109.5 (12) |
O1—N1—Ru | 171 (1) | H31B—C31—H31C | 109.5 (12) |
C4—N2—C22 | 111.6 (9) | H32A—C32—H32B | 109.5 (12) |
C4—N2—C21 | 108.8 (9) | H32A—C32—H32C | 109.5 (12) |
C22—N2—C21 | 107.8 (9) | H32B—C32—H32C | 109.5 (12) |
C4—N2—Ru | 105.0 (6) | N2—C4—H4A | 109.5 (10) |
C22—N2—Ru | 112.3 (7) | N2—C4—H4B | 109.5 (10) |
C21—N2—Ru | 111.4 (7) | C3—C4—H4A | 109.5 (10) |
N3—C3—C4 | 111.4 (8) | C3—C4—H4B | 109.5 (11) |
C32—N3—C31 | 107.3 (9) | H4A—C4—H4B | 108.1 (11) |
C32—N3—C3 | 110.2 (9) | O2—C5—H5A | 110.2 (11) |
C31—N3—C3 | 108.6 (8) | O2—C5—H5B | 110.2 (10) |
C32—N3—Ru | 112.4 (7) | H5A—C5—H5B | 108.5 (12) |
C31—N3—Ru | 112.8 (7) | H5A—C5—C6 | 110.2 (11) |
C3—N3—Ru | 105.7 (6) | H5B—C5—C6 | 110.2 (12) |
N2—C4—C3 | 110.7 (9) | C5—C6—H6A | 109.5 (12) |
O4—N4—O3 | 121 (1) | C5—C6—H6B | 109.5 (11) |
O4—N4—Ru | 120.8 (8) | C5—C6—H6C | 109.5 (12) |
O3—N4—Ru | 117.7 (8) | H6A—C6—H6B | 109.5 (13) |
O6—N5—O5 | 120 (1) | H6A—C6—H6C | 109.5 (12) |
O6—N5—Ru | 122.0 (8) | H6B—C6—H6C | 109.5 (13) |
O5—N5—Ru | 117.7 (9) | | |
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