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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102001701/da1216sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102001701/da1216Isup2.hkl
Contains datablock I

CCDC reference: 184468

Computing details top

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 m3
Mr = 384.37Cu Kα radiation, λ = 1.5418 Å
Trigonal, P31Cell parameters from 25 reflections
a = 7.930 (2) Åθ = 10.1–21.6°
c = 20.210 (9) ŵ = 8.97 mm1
V = 1100.6 (6) Å3T = 293 K
Z = 3Prism, dark orange
F(000) = 5880.08 × 0.06 × 0.06 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
1431 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.045
Graphite monochromatorθmax = 69.8°, θmin = 6.5°
non–profiled ω/2θ scansh = 09
Absorption correction: ψ-scan
(North et al., 1968)
k = 90
Tmin = 0.439, Tmax = 0.566l = 024
1593 measured reflections1 standard reflections every 30 min
1439 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-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 reflectionsΔρmax = 0.87 e Å3
207 parametersΔρmin = 1.72 e Å3
1 restraintAbsolute structure: Flack (1983)
Primary atom site location: PattersonAbsolute 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
xyzUiso*/Ueq
Ru0.43700 (8)0.20021 (8)0.00000 (5)0.02372 (18)
N10.4983 (13)0.0822 (14)0.0608 (4)0.038 (2)
O10.5637 (17)0.0251 (18)0.1000 (5)0.071 (3)
N20.2107 (12)0.0682 (13)0.0478 (4)0.0286 (18)
C210.239 (2)0.0613 (17)0.1218 (5)0.048 (3)
H21A0.22130.04070.14020.03 (3)*
H21B0.36760.03630.13160.03 (3)*
H21C0.14480.18380.14080.05 (3)*
C220.2091 (18)0.2452 (15)0.0225 (6)0.044 (3)
H22A0.11390.35730.04640.3 (2)*
H22B0.33540.23150.02860.05 (4)*
H22C0.17690.26110.02370.02 (2)*
C30.0201 (13)0.0222 (15)0.0373 (5)0.036 (2)
H3A0.02400.11880.06570.03 (3)*
H3B0.10160.02440.04550.02 (2)*
N30.1868 (12)0.1751 (13)0.0540 (4)0.0307 (19)
C310.1358 (17)0.3233 (17)0.0339 (6)0.040 (3)
H31A0.25070.44970.03430.05 (3)*
H31B0.08170.29470.00990.06 (4)*
H31C0.04180.32180.06420.05 (4)*
C320.2190 (18)0.1934 (19)0.1263 (5)0.044 (3)
H32A0.10440.17800.14800.10 (6)*
H32B0.24600.09460.14150.03 (3)*
H32C0.32740.31950.13640.03 (3)*
C40.0276 (15)0.0732 (17)0.0336 (6)0.039 (2)
H4A0.01530.01850.06210.03 (3)*
H4B0.08060.20230.04270.02 (2)*
N40.6666 (16)0.2117 (15)0.0561 (5)0.041 (2)
O30.6836 (14)0.0656 (16)0.0570 (5)0.063 (3)
O40.7794 (14)0.3582 (17)0.0852 (6)0.067 (3)
N50.6303 (14)0.4645 (14)0.0460 (5)0.039 (2)
O50.7857 (15)0.4861 (16)0.0653 (7)0.073 (3)
O60.5938 (13)0.5947 (12)0.0521 (5)0.062 (2)
O20.3778 (10)0.3238 (10)0.0693 (3)0.0348 (15)
C50.4808 (17)0.5047 (16)0.1020 (6)0.046 (3)
H5A0.51870.61040.07060.01 (2)*
H5B0.59750.51790.12240.04 (3)*
C60.349 (2)0.5116 (18)0.1536 (6)0.050 (3)
H6A0.31430.40770.18470.08 (5)*
H6B0.23380.49720.13290.27 (19)*
H6C0.41540.63420.17630.07 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru0.0176 (3)0.0227 (3)0.0271 (3)0.0073 (2)0.0013 (2)0.0003 (3)
N10.031 (4)0.043 (5)0.040 (5)0.017 (4)0.002 (4)0.006 (4)
O10.086 (7)0.101 (8)0.050 (6)0.066 (7)0.009 (5)0.022 (5)
N20.020 (4)0.032 (4)0.036 (5)0.014 (4)0.002 (3)0.007 (4)
C210.059 (7)0.041 (6)0.031 (6)0.014 (5)0.013 (5)0.011 (5)
C220.057 (7)0.029 (5)0.047 (6)0.021 (5)0.002 (5)0.003 (5)
C30.020 (4)0.032 (5)0.045 (6)0.005 (4)0.003 (4)0.003 (4)
N30.022 (4)0.033 (4)0.030 (4)0.008 (3)0.003 (3)0.001 (3)
C310.040 (6)0.039 (6)0.041 (6)0.020 (5)0.006 (5)0.000 (5)
C320.049 (6)0.053 (7)0.033 (6)0.028 (6)0.006 (5)0.002 (5)
C40.028 (5)0.033 (5)0.055 (7)0.013 (4)0.003 (5)0.006 (5)
N40.042 (5)0.039 (5)0.045 (5)0.024 (5)0.008 (4)0.005 (4)
O30.059 (6)0.080 (7)0.069 (6)0.047 (6)0.009 (5)0.003 (5)
O40.040 (5)0.076 (7)0.084 (8)0.027 (5)0.022 (5)0.016 (6)
N50.031 (5)0.038 (5)0.033 (5)0.007 (4)0.004 (4)0.001 (4)
O50.036 (5)0.060 (6)0.109 (9)0.014 (4)0.026 (6)0.020 (6)
O60.060 (5)0.035 (4)0.080 (6)0.015 (4)0.018 (5)0.022 (4)
O20.036 (4)0.034 (4)0.032 (4)0.015 (3)0.003 (3)0.004 (3)
C50.045 (6)0.035 (6)0.051 (7)0.013 (5)0.001 (5)0.019 (5)
C60.070 (8)0.047 (6)0.041 (6)0.036 (6)0.002 (5)0.008 (5)
Geometric parameters (Å, º) top
Ru—N11.754 (9)C21—H21B0.96
Ru—O21.898 (7)C21—H21C0.96
Ru—N52.10 (1)C22—H22A0.96
Ru—N42.11 (1)C22—H22B0.96
Ru—N32.185 (9)C22—H22C0.96
Ru—N22.205 (9)C3—H3A0.97
N1—O11.16 (1)C3—H3B0.97
N2—C41.46 (1)C31—H31A0.96
N2—C221.49 (1)C31—H31B0.96
N2—C211.51 (1)C31—H31C0.96
C3—N31.50 (1)C32—H32A0.96
C3—C41.50 (2)C32—H32B0.96
N3—C321.48 (1)C32—H32C0.96
N3—C311.48 (2)C4—H4A0.97
N4—O41.21 (1)C4—H4B0.97
N4—O31.23 (1)C5—H5A0.97
N5—O61.21 (1)C5—H5B0.97
N5—O51.22 (1)C6—H6A0.96
O2—C51.41 (1)C6—H6B0.96
C5—C61.50 (2)C6—H6C0.96
C21—H21A0.96
N1—Ru—O2176.8 (4)C5—O2—Ru134.7 (7)
N1—Ru—N587.9 (4)O2—C5—C6107.7 (9)
O2—Ru—N593.3 (4)H21A—C21—H21B109.5 (12)
N1—Ru—N486.3 (4)H21A—C21—H21C109.5 (13)
O2—Ru—N490.7 (4)H21B—C21—H21C109.5 (12)
N5—Ru—N490.6 (4)H22A—C22—H22B109.5 (12)
N1—Ru—N394.7 (4)H22A—C22—H22C109.5 (12)
O2—Ru—N388.2 (3)H22B—C22—H22C109.5 (13)
N5—Ru—N392.7 (3)H3A—C3—H3B108.0 (10)
N4—Ru—N3176.6 (4)H3A—C3—C4109.4 (10)
N1—Ru—N295.8 (4)H3B—C3—C4109.4 (10)
O2—Ru—N283.3 (3)N3—C3—H3A109.4 (10)
N5—Ru—N2174.0 (4)N3—C3—H3B109.3 (10)
N4—Ru—N294.3 (4)H31A—C31—H31B109.5 (12)
N3—Ru—N282.4 (3)H31A—C31—H31C109.5 (12)
O1—N1—Ru171 (1)H31B—C31—H31C109.5 (12)
C4—N2—C22111.6 (9)H32A—C32—H32B109.5 (12)
C4—N2—C21108.8 (9)H32A—C32—H32C109.5 (12)
C22—N2—C21107.8 (9)H32B—C32—H32C109.5 (12)
C4—N2—Ru105.0 (6)N2—C4—H4A109.5 (10)
C22—N2—Ru112.3 (7)N2—C4—H4B109.5 (10)
C21—N2—Ru111.4 (7)C3—C4—H4A109.5 (10)
N3—C3—C4111.4 (8)C3—C4—H4B109.5 (11)
C32—N3—C31107.3 (9)H4A—C4—H4B108.1 (11)
C32—N3—C3110.2 (9)O2—C5—H5A110.2 (11)
C31—N3—C3108.6 (8)O2—C5—H5B110.2 (10)
C32—N3—Ru112.4 (7)H5A—C5—H5B108.5 (12)
C31—N3—Ru112.8 (7)H5A—C5—C6110.2 (11)
C3—N3—Ru105.7 (6)H5B—C5—C6110.2 (12)
N2—C4—C3110.7 (9)C5—C6—H6A109.5 (12)
O4—N4—O3121 (1)C5—C6—H6B109.5 (11)
O4—N4—Ru120.8 (8)C5—C6—H6C109.5 (12)
O3—N4—Ru117.7 (8)H6A—C6—H6B109.5 (13)
O6—N5—O5120 (1)H6A—C6—H6C109.5 (12)
O6—N5—Ru122.0 (8)H6B—C6—H6C109.5 (13)
O5—N5—Ru117.7 (9)
 

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