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In the monocationic octahedral complex, [RuCl(C
6H
18N
4)(CO)]Cl, the ruthenium(II) centre is coordinated by a chloride and a carbonyl ligand and by the tetradentate tris(2-aminoethyl)amine (tren) chelator. The complex has approximate non-crystallographic
Cs symmetry. In the crystal structure, N—H
Cl hydrogen bonds are found, mainly with the chloride counter-ion as the acceptor.
Supporting information
CCDC reference: 672691
Key indicators
- Single-crystal X-ray study
- T = 200 K
- Mean (C-C) = 0.003 Å
- R factor = 0.020
- wR factor = 0.048
- Data-to-parameter ratio = 20.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru - C1 .. 8.55 su
| Author Response: situation checked, assignment of scattering sites correct
|
PLAT420_ALERT_2_C D-H Without Acceptor N4 - H42 ... ?
| Author Response: situation checked, no suitable acceptor present
|
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
The title compound was obtained accidentally on the attempted preparation of
[RuCl2(tren)] by refluxing RuCl3 * 3 H2O with an equimolar amount of
tris(2-aminoethyl)amine (tren) and 7 equivalents of LiCl in DMF in analogy to
a published procedure (Sullivan et al., 1978).
All H atoms were constructed and refined as riding on their parent atoms with
one common isotropic displacement parameter.
Data collection: COLLECT (Hooft, 1997–2004); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003).
Carbonylchlorido[tris(2-aminoethyl)amine]ruthenium(II) chloride
top
Crystal data top
[RuCl(C6H18N4)(CO)]Cl | F(000) = 696 |
Mr = 346.22 | Dx = 1.840 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3049 reflections |
a = 10.1514 (2) Å | θ = 3.1–27.5° |
b = 8.5268 (1) Å | µ = 1.66 mm−1 |
c = 14.7413 (3) Å | T = 200 K |
β = 101.6790 (7)° | Block, yellow |
V = 1249.58 (4) Å3 | 0.17 × 0.12 × 0.07 mm |
Z = 4 | |
Data collection top
KappaCCD diffractometer | 2863 independent reflections |
Radiation source: rotating anode | 2562 reflections with I > 2σ(I) |
MONTEL, graded multilayered X-ray optics monochromator | Rint = 0.031 |
ϕ and ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −13→13 |
Tmin = 0.800, Tmax = 0.890 | k = −11→10 |
23413 measured reflections | l = −19→19 |
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)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.048 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0181P)2 + 1.1292P] where P = (Fo2 + 2Fc2)/3 |
2863 reflections | (Δ/σ)max = 0.001 |
137 parameters | Δρmax = 0.56 e Å−3 |
0 restraints | Δρmin = −0.53 e Å−3 |
Crystal data top
[RuCl(C6H18N4)(CO)]Cl | V = 1249.58 (4) Å3 |
Mr = 346.22 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1514 (2) Å | µ = 1.66 mm−1 |
b = 8.5268 (1) Å | T = 200 K |
c = 14.7413 (3) Å | 0.17 × 0.12 × 0.07 mm |
β = 101.6790 (7)° | |
Data collection top
KappaCCD diffractometer | 2863 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | 2562 reflections with I > 2σ(I) |
Tmin = 0.800, Tmax = 0.890 | Rint = 0.031 |
23413 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.020 | 0 restraints |
wR(F2) = 0.048 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.56 e Å−3 |
2863 reflections | Δρmin = −0.53 e Å−3 |
137 parameters | |
Special details top
Experimental. µ × r = 0.116, Tmin/Tmax = 0.899 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ru | 0.263803 (15) | 0.685462 (18) | 0.091163 (10) | 0.01895 (6) | |
Cl1 | 0.09940 (5) | 0.70362 (7) | −0.05312 (3) | 0.03170 (13) | |
O1 | 0.3830 (2) | 0.3964 (2) | 0.02630 (15) | 0.0593 (5) | |
N1 | 0.18612 (16) | 0.8875 (2) | 0.14884 (11) | 0.0220 (3) | |
N4 | 0.37625 (18) | 0.8578 (2) | 0.03603 (12) | 0.0285 (4) | |
H41 | 0.4667 | 0.8410 | 0.0577 | 0.0381 (16)* | |
H42 | 0.3593 | 0.8499 | −0.0275 | 0.0381 (16)* | |
N7 | 0.39797 (17) | 0.6894 (2) | 0.21966 (12) | 0.0247 (4) | |
H71 | 0.4162 | 0.5884 | 0.2403 | 0.0381 (16)* | |
H72 | 0.4775 | 0.7352 | 0.2130 | 0.0381 (16)* | |
N10 | 0.11750 (16) | 0.5702 (2) | 0.15115 (11) | 0.0240 (4) | |
H101 | 0.0625 | 0.5110 | 0.1068 | 0.0381 (16)* | |
H102 | 0.1595 | 0.5038 | 0.1972 | 0.0381 (16)* | |
C1 | 0.3369 (2) | 0.5085 (3) | 0.04993 (16) | 0.0343 (5) | |
C2 | 0.1995 (2) | 1.0192 (3) | 0.08523 (16) | 0.0310 (5) | |
H21 | 0.1845 | 1.1202 | 0.1147 | 0.0381 (16)* | |
H22 | 0.1310 | 1.0088 | 0.0273 | 0.0381 (16)* | |
C3 | 0.3396 (2) | 1.0170 (3) | 0.06317 (16) | 0.0329 (5) | |
H31 | 0.3428 | 1.0913 | 0.0120 | 0.0381 (16)* | |
H32 | 0.4060 | 1.0521 | 0.1182 | 0.0381 (16)* | |
C5 | 0.2655 (2) | 0.9209 (3) | 0.24410 (14) | 0.0300 (5) | |
H51 | 0.2038 | 0.9582 | 0.2836 | 0.0381 (16)* | |
H52 | 0.3308 | 1.0057 | 0.2405 | 0.0381 (16)* | |
C6 | 0.3403 (2) | 0.7782 (3) | 0.28834 (14) | 0.0307 (5) | |
H61 | 0.4133 | 0.8114 | 0.3400 | 0.0381 (16)* | |
H62 | 0.2779 | 0.7100 | 0.3141 | 0.0381 (16)* | |
C8 | 0.0435 (2) | 0.8471 (3) | 0.14896 (16) | 0.0299 (5) | |
H81 | −0.0093 | 0.8482 | 0.0847 | 0.0381 (16)* | |
H82 | 0.0047 | 0.9264 | 0.1851 | 0.0381 (16)* | |
C9 | 0.0346 (2) | 0.6870 (3) | 0.19081 (15) | 0.0292 (5) | |
H91 | 0.0668 | 0.6930 | 0.2588 | 0.0381 (16)* | |
H92 | −0.0604 | 0.6522 | 0.1785 | 0.0381 (16)* | |
Cl2 | 0.32744 (5) | 0.36408 (7) | 0.31352 (4) | 0.03583 (13) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ru | 0.01829 (9) | 0.02010 (9) | 0.01801 (9) | −0.00241 (6) | 0.00263 (6) | −0.00132 (6) |
Cl1 | 0.0317 (3) | 0.0424 (3) | 0.0181 (2) | −0.0134 (2) | −0.0020 (2) | 0.0007 (2) |
O1 | 0.0670 (13) | 0.0386 (11) | 0.0765 (14) | 0.0085 (10) | 0.0243 (11) | −0.0213 (10) |
N1 | 0.0230 (8) | 0.0200 (8) | 0.0226 (8) | 0.0004 (7) | 0.0039 (7) | 0.0014 (7) |
N4 | 0.0253 (9) | 0.0384 (11) | 0.0225 (8) | −0.0102 (8) | 0.0060 (7) | 0.0013 (8) |
N7 | 0.0212 (8) | 0.0261 (9) | 0.0247 (9) | −0.0008 (7) | 0.0001 (7) | 0.0038 (7) |
N10 | 0.0228 (8) | 0.0243 (9) | 0.0233 (8) | −0.0079 (7) | 0.0007 (7) | 0.0025 (7) |
C1 | 0.0345 (12) | 0.0319 (12) | 0.0371 (12) | −0.0037 (10) | 0.0082 (10) | −0.0065 (10) |
C2 | 0.0319 (11) | 0.0236 (11) | 0.0352 (12) | 0.0013 (9) | 0.0017 (9) | 0.0087 (9) |
C3 | 0.0351 (12) | 0.0275 (12) | 0.0348 (12) | −0.0104 (9) | 0.0045 (9) | 0.0082 (10) |
C5 | 0.0385 (12) | 0.0267 (11) | 0.0239 (10) | −0.0036 (9) | 0.0041 (9) | −0.0065 (9) |
C6 | 0.0337 (12) | 0.0374 (13) | 0.0180 (10) | −0.0053 (10) | −0.0020 (9) | −0.0018 (9) |
C8 | 0.0207 (10) | 0.0337 (12) | 0.0364 (12) | 0.0040 (9) | 0.0089 (9) | 0.0010 (10) |
C9 | 0.0234 (10) | 0.0375 (12) | 0.0282 (11) | −0.0055 (9) | 0.0087 (8) | 0.0010 (9) |
Cl2 | 0.0257 (3) | 0.0361 (3) | 0.0443 (3) | 0.0040 (2) | 0.0038 (2) | 0.0146 (3) |
Geometric parameters (Å, º) top
Ru—C1 | 1.838 (2) | N10—H101 | 0.9200 |
Ru—N7 | 2.0975 (17) | N10—H102 | 0.9200 |
Ru—N10 | 2.1176 (16) | C2—C3 | 1.522 (3) |
Ru—N4 | 2.1208 (17) | C2—H21 | 0.9900 |
Ru—N1 | 2.1409 (17) | C2—H22 | 0.9900 |
Ru—Cl1 | 2.4281 (5) | C3—H31 | 0.9900 |
O1—C1 | 1.149 (3) | C3—H32 | 0.9900 |
N1—C2 | 1.487 (3) | C5—C6 | 1.510 (3) |
N1—C8 | 1.489 (3) | C5—H51 | 0.9900 |
N1—C5 | 1.498 (3) | C5—H52 | 0.9900 |
N4—C3 | 1.484 (3) | C6—H61 | 0.9900 |
N4—H41 | 0.9200 | C6—H62 | 0.9900 |
N4—H42 | 0.9200 | C8—C9 | 1.508 (3) |
N7—C6 | 1.477 (3) | C8—H81 | 0.9900 |
N7—H71 | 0.9200 | C8—H82 | 0.9900 |
N7—H72 | 0.9200 | C9—H91 | 0.9900 |
N10—C9 | 1.497 (3) | C9—H92 | 0.9900 |
| | | |
C1—Ru—N7 | 94.58 (9) | H101—N10—H102 | 108.1 |
C1—Ru—N10 | 96.99 (8) | O1—C1—Ru | 178.3 (2) |
N7—Ru—N10 | 90.72 (6) | N1—C2—C3 | 109.53 (17) |
C1—Ru—N4 | 99.04 (9) | N1—C2—H21 | 109.8 |
N7—Ru—N4 | 91.91 (7) | C3—C2—H21 | 109.8 |
N10—Ru—N4 | 163.50 (7) | N1—C2—H22 | 109.8 |
C1—Ru—N1 | 175.95 (9) | C3—C2—H22 | 109.8 |
N7—Ru—N1 | 81.51 (6) | H21—C2—H22 | 108.2 |
N10—Ru—N1 | 82.04 (6) | N4—C3—C2 | 111.40 (17) |
N4—Ru—N1 | 82.24 (7) | N4—C3—H31 | 109.3 |
C1—Ru—Cl1 | 90.85 (7) | C2—C3—H31 | 109.3 |
N7—Ru—Cl1 | 174.57 (5) | N4—C3—H32 | 109.3 |
N10—Ru—Cl1 | 88.83 (5) | C2—C3—H32 | 109.3 |
N4—Ru—Cl1 | 87.02 (5) | H31—C3—H32 | 108.0 |
N1—Ru—Cl1 | 93.06 (5) | N1—C5—C6 | 112.32 (17) |
C2—N1—C8 | 112.88 (16) | N1—C5—H51 | 109.1 |
C2—N1—C5 | 110.32 (16) | C6—C5—H51 | 109.1 |
C8—N1—C5 | 112.42 (16) | N1—C5—H52 | 109.1 |
C2—N1—Ru | 105.61 (12) | C6—C5—H52 | 109.1 |
C8—N1—Ru | 104.53 (12) | H51—C5—H52 | 107.9 |
C5—N1—Ru | 110.72 (12) | N7—C6—C5 | 110.56 (17) |
C3—N4—Ru | 110.29 (12) | N7—C6—H61 | 109.5 |
C3—N4—H41 | 109.6 | C5—C6—H61 | 109.5 |
Ru—N4—H41 | 109.6 | N7—C6—H62 | 109.5 |
C3—N4—H42 | 109.6 | C5—C6—H62 | 109.5 |
Ru—N4—H42 | 109.6 | H61—C6—H62 | 108.1 |
H41—N4—H42 | 108.1 | N1—C8—C9 | 110.39 (17) |
C6—N7—Ru | 110.62 (12) | N1—C8—H81 | 109.6 |
C6—N7—H71 | 109.5 | C9—C8—H81 | 109.6 |
Ru—N7—H71 | 109.5 | N1—C8—H82 | 109.6 |
C6—N7—H72 | 109.5 | C9—C8—H82 | 109.6 |
Ru—N7—H72 | 109.5 | H81—C8—H82 | 108.1 |
H71—N7—H72 | 108.1 | N10—C9—C8 | 110.95 (16) |
C9—N10—Ru | 110.59 (12) | N10—C9—H91 | 109.4 |
C9—N10—H101 | 109.5 | C8—C9—H91 | 109.4 |
Ru—N10—H101 | 109.5 | N10—C9—H92 | 109.4 |
C9—N10—H102 | 109.5 | C8—C9—H92 | 109.4 |
Ru—N10—H102 | 109.5 | H91—C9—H92 | 108.0 |
| | | |
N7—Ru—N1—C2 | 119.66 (13) | C1—Ru—N10—C9 | −178.62 (14) |
N10—Ru—N1—C2 | −148.41 (13) | N7—Ru—N10—C9 | 86.67 (13) |
N4—Ru—N1—C2 | 26.54 (12) | N4—Ru—N10—C9 | −12.5 (3) |
Cl1—Ru—N1—C2 | −60.03 (12) | N1—Ru—N10—C9 | 5.35 (13) |
N7—Ru—N1—C8 | −121.04 (13) | Cl1—Ru—N10—C9 | −87.91 (12) |
N10—Ru—N1—C8 | −29.11 (12) | C8—N1—C2—C3 | −160.53 (18) |
N4—Ru—N1—C8 | 145.84 (13) | C5—N1—C2—C3 | 72.8 (2) |
Cl1—Ru—N1—C8 | 59.28 (12) | Ru—N1—C2—C3 | −46.91 (19) |
N7—Ru—N1—C5 | 0.25 (13) | Ru—N4—C3—C2 | −23.8 (2) |
N10—Ru—N1—C5 | 92.17 (13) | N1—C2—C3—N4 | 48.3 (2) |
N4—Ru—N1—C5 | −92.87 (13) | C2—N1—C5—C6 | −138.18 (19) |
Cl1—Ru—N1—C5 | −179.44 (12) | C8—N1—C5—C6 | 94.9 (2) |
C1—Ru—N4—C3 | −177.75 (15) | Ru—N1—C5—C6 | −21.6 (2) |
N7—Ru—N4—C3 | −82.80 (14) | Ru—N7—C6—C5 | −39.3 (2) |
N10—Ru—N4—C3 | 16.2 (3) | N1—C5—C6—N7 | 40.3 (2) |
N1—Ru—N4—C3 | −1.64 (13) | C2—N1—C8—C9 | 163.23 (18) |
Cl1—Ru—N4—C3 | 91.87 (13) | C5—N1—C8—C9 | −71.2 (2) |
C1—Ru—N7—C6 | −157.49 (15) | Ru—N1—C8—C9 | 48.95 (19) |
N10—Ru—N7—C6 | −60.42 (14) | Ru—N10—C9—C8 | 20.0 (2) |
N4—Ru—N7—C6 | 103.28 (14) | N1—C8—C9—N10 | −47.2 (2) |
N1—Ru—N7—C6 | 21.42 (13) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H41···Cl2i | 0.92 | 2.53 | 3.3569 (19) | 150 |
N7—H71···Cl2 | 0.92 | 2.46 | 3.2442 (18) | 144 |
N7—H72···Cl2i | 0.92 | 2.36 | 3.2830 (18) | 176 |
N10—H101···Cl1ii | 0.92 | 2.48 | 3.3319 (17) | 154 |
N10—H102···Cl2 | 0.92 | 2.47 | 3.3609 (18) | 164 |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x, −y+1, −z. |
Experimental details
Crystal data |
Chemical formula | [RuCl(C6H18N4)(CO)]Cl |
Mr | 346.22 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 200 |
a, b, c (Å) | 10.1514 (2), 8.5268 (1), 14.7413 (3) |
β (°) | 101.6790 (7) |
V (Å3) | 1249.58 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.66 |
Crystal size (mm) | 0.17 × 0.12 × 0.07 |
|
Data collection |
Diffractometer | KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2001) |
Tmin, Tmax | 0.800, 0.890 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 23413, 2863, 2562 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.650 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.020, 0.048, 1.06 |
No. of reflections | 2863 |
No. of parameters | 137 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.56, −0.53 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H41···Cl2i | 0.92 | 2.53 | 3.3569 (19) | 149.7 |
N7—H71···Cl2 | 0.92 | 2.46 | 3.2442 (18) | 143.9 |
N7—H72···Cl2i | 0.92 | 2.36 | 3.2830 (18) | 175.6 |
N10—H101···Cl1ii | 0.92 | 2.48 | 3.3319 (17) | 154.1 |
N10—H102···Cl2 | 0.92 | 2.47 | 3.3609 (18) | 164.2 |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x, −y+1, −z. |
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The title compound, C7H18Cl2N4ORu, was obtained on the attempted preparation of [RuCl2(tren)] by refluxing RuCl3 with an equimolar amount of tris(2-aminoethyl)amine (tren) in DMF.
The molecular structure is shown in Fig. 1. The complex features three 5-membered rings: Ru–N1–C2–C3–N4 adopts a twist conformation on N1–C2 (Q2 = 0.444 (2) Å, ϕ2 = 241.5 (2)°), whereas Ru–N1–C5–C6–N7 (Q2 = 0.359 (2) Å, ϕ2 = 294.6 (3)°) shows an envelope conformation on C6. Ru–N1–C8–C9–N10 is twisted on N1–C8 (Q2 = 0.459 (2) Å, ϕ2 = 55.6 (2)°). Ring puckering parameters (Cremer & Pople, 1975) were calculated with PLATON (Spek, 2007).
Bond lengths and angles are normal.
The molecular packing including the hydrogen bond system is shown in Fig. 2. The search for hydrogen bonded molecular aggregates provided an infinite two-dimensional network (base vectors = [0 1 0], [2 0 1]) along the (1 0 - 2)-plane.