Reaction of [RuCl2(Me2SO)4] with sodium azide in water affords the title complex di-μ-1,3-azido-bis[chlorotris(dimethyl sulfoxide-κS)ruthenium(II)], [Ru2Cl2(N3)2(C2H6OS)6]. X-Ray crystal structure determination has been performed on the title compound. The result reveals that two [Ru(Me2SO)3]2+ units are linked by two bridging azide ligands to form a centrosymmetric complex. The geometry about each Ru atom is essentially octahedral, with three S atoms of Me2SO arranged in a facial configuration, two coordinated N atoms of bridging N3− ligands and a chloride anion.
Supporting information
CCDC reference: 223750
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-N) = 0.004 Å
- R factor = 0.030
- wR factor = 0.065
- Data-to-parameter ratio = 18.1
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ru1 - Cl1 .. 17.01 su
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT048_ALERT_1_C MoietyFormula Not Given ........................ ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.84
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT230_ALERT_2_C Hirshfeld Test Diff for N1 - N2 .. 5.91 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for N2 - N3 .. 5.98 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru1 - S1 .. 6.32 su
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... S1
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1
N1 -RU1 -S1 -O1 154.90 0.70 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6
N1 -RU1 -S1 -C1 30.50 0.70 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 11
N1 -RU1 -S1 -C2 -77.50 0.70 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 17
N3 -RU1 -S2 -O3 140.00 1.50 3.666 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 22
N3 -RU1 -S2 -C5 17.00 1.60 3.666 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 27
N3 -RU1 -S2 -C6 -92.60 1.60 3.666 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 35
CL1 -RU1 -S3 -O2 -158.20 0.30 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 40
CL1 -RU1 -S3 -C3 75.70 0.40 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 45
CL1 -RU1 -S3 -C4 -32.80 0.40 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 49
S1 -RU1 -N1 -N2 -32.30 0.90 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 51
RU1 -N1 -N2 -N3 -144.00 6.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 52
N1 -N2 -N3 -RU1 -147.00 6.00 1.555 1.555 1.555 3.666
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.843
Tmax scaled 0.843 Tmin scaled 0.652
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
22 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
14 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
Crystal data top
C6H18ClN3O3RuS3 | F(000) = 832 |
Mr = 412.93 | Dx = 1.908 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.141 (2) Å | Cell parameters from 1005 reflections |
b = 11.822 (3) Å | θ = 3.0–26.2° |
c = 14.934 (4) Å | µ = 1.71 mm−1 |
β = 90.217 (5)° | T = 293 K |
V = 1437.2 (7) Å3 | Block, red |
Z = 4 | 0.26 × 0.14 × 0.10 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2915 independent reflections |
Radiation source: fine-focus sealed tube | 2276 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
φ and ω scans | θmax = 26.4°, θmin = 2.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→10 |
Tmin = 0.652, Tmax = 0.843 | k = −14→12 |
8004 measured reflections | l = −18→18 |
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)] = 0.030 | H-atom parameters constrained |
wR(F2) = 0.065 | w = 1/[σ2(Fo2) + (0.0251P)2 + 0.6144P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.001 |
2915 reflections | Δρmax = 0.49 e Å−3 |
161 parameters | Δρmin = −0.46 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0011 (2) |
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 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 | |
Ru1 | 0.42731 (3) | 0.67009 (2) | 0.597285 (17) | 0.02198 (10) | |
S1 | 0.31715 (12) | 0.66660 (8) | 0.73720 (6) | 0.0352 (2) | |
S2 | 0.55279 (10) | 0.84024 (7) | 0.61254 (6) | 0.0280 (2) | |
S3 | 0.20576 (10) | 0.75063 (7) | 0.53057 (6) | 0.0281 (2) | |
O1 | 0.3548 (5) | 0.7567 (3) | 0.8009 (2) | 0.0765 (11) | |
O2 | 0.0984 (3) | 0.8260 (2) | 0.58216 (19) | 0.0452 (7) | |
O3 | 0.4547 (3) | 0.9437 (2) | 0.60392 (19) | 0.0406 (7) | |
C1 | 0.3673 (6) | 0.5370 (4) | 0.7898 (3) | 0.0540 (13) | |
H1A | 0.4845 | 0.5298 | 0.7939 | 0.081* | |
H1B | 0.3236 | 0.4755 | 0.7552 | 0.081* | |
H1C | 0.3209 | 0.5355 | 0.8488 | 0.081* | |
C2 | 0.0998 (5) | 0.6506 (5) | 0.7366 (3) | 0.0721 (16) | |
H2A | 0.0632 | 0.6313 | 0.7957 | 0.108* | |
H2B | 0.0695 | 0.5915 | 0.6957 | 0.108* | |
H2C | 0.0495 | 0.7202 | 0.7182 | 0.108* | |
C3 | 0.0779 (5) | 0.6474 (3) | 0.4792 (3) | 0.0422 (10) | |
H3A | 0.0243 | 0.6036 | 0.5247 | 0.063* | |
H3B | 0.1435 | 0.5985 | 0.4426 | 0.063* | |
H3C | −0.0032 | 0.6844 | 0.4427 | 0.063* | |
C4 | 0.2652 (5) | 0.8257 (4) | 0.4325 (3) | 0.0474 (10) | |
H4A | 0.1692 | 0.8546 | 0.4029 | 0.071* | |
H4B | 0.3225 | 0.7755 | 0.3929 | 0.071* | |
H4C | 0.3359 | 0.8873 | 0.4489 | 0.071* | |
C5 | 0.7135 (5) | 0.8499 (3) | 0.5336 (3) | 0.0459 (11) | |
H5A | 0.6679 | 0.8524 | 0.4743 | 0.069* | |
H5B | 0.7838 | 0.7851 | 0.5392 | 0.069* | |
H5C | 0.7759 | 0.9174 | 0.5445 | 0.069* | |
C6 | 0.6698 (6) | 0.8540 (4) | 0.7124 (3) | 0.0577 (13) | |
H6A | 0.7299 | 0.9238 | 0.7111 | 0.086* | |
H6B | 0.7453 | 0.7919 | 0.7171 | 0.086* | |
H6C | 0.5975 | 0.8537 | 0.7631 | 0.086* | |
Cl1 | 0.67715 (12) | 0.58134 (9) | 0.65165 (7) | 0.0445 (3) | |
N1 | 0.5266 (4) | 0.6509 (2) | 0.46627 (19) | 0.0311 (7) | |
N2 | 0.6004 (4) | 0.5703 (3) | 0.44499 (19) | 0.0296 (7) | |
N3 | 0.6792 (4) | 0.4933 (2) | 0.42110 (19) | 0.0308 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ru1 | 0.02541 (15) | 0.01892 (15) | 0.02162 (15) | 0.00301 (12) | 0.00049 (10) | −0.00092 (12) |
S1 | 0.0429 (5) | 0.0374 (5) | 0.0253 (5) | 0.0014 (5) | 0.0042 (4) | −0.0014 (4) |
S2 | 0.0276 (4) | 0.0240 (5) | 0.0324 (5) | 0.0004 (4) | −0.0017 (4) | −0.0037 (4) |
S3 | 0.0285 (5) | 0.0241 (4) | 0.0317 (5) | 0.0030 (4) | −0.0050 (4) | −0.0030 (4) |
O1 | 0.126 (3) | 0.067 (2) | 0.0367 (18) | −0.029 (2) | 0.019 (2) | −0.0195 (17) |
O2 | 0.0386 (15) | 0.0422 (16) | 0.0549 (18) | 0.0141 (13) | −0.0032 (13) | −0.0140 (14) |
O3 | 0.0394 (16) | 0.0228 (13) | 0.0595 (19) | 0.0051 (11) | 0.0035 (14) | −0.0032 (12) |
C1 | 0.059 (3) | 0.062 (3) | 0.041 (3) | 0.010 (2) | 0.011 (2) | 0.024 (2) |
C2 | 0.045 (3) | 0.118 (5) | 0.053 (3) | 0.016 (3) | 0.020 (2) | 0.021 (3) |
C3 | 0.041 (2) | 0.040 (2) | 0.046 (2) | −0.0049 (18) | −0.0151 (19) | −0.0048 (19) |
C4 | 0.054 (3) | 0.045 (2) | 0.043 (2) | 0.003 (2) | −0.011 (2) | 0.015 (2) |
C5 | 0.036 (2) | 0.039 (2) | 0.063 (3) | −0.0066 (18) | 0.015 (2) | −0.006 (2) |
C6 | 0.069 (3) | 0.054 (3) | 0.050 (3) | −0.012 (2) | −0.026 (2) | −0.008 (2) |
Cl1 | 0.0435 (6) | 0.0411 (6) | 0.0489 (6) | 0.0091 (5) | −0.0046 (5) | 0.0074 (5) |
N1 | 0.0410 (18) | 0.0224 (17) | 0.0300 (17) | 0.0021 (13) | 0.0106 (14) | −0.0040 (12) |
N2 | 0.0357 (18) | 0.0281 (18) | 0.0250 (16) | −0.0065 (15) | 0.0015 (13) | 0.0028 (14) |
N3 | 0.0369 (17) | 0.0205 (15) | 0.0350 (17) | 0.0012 (14) | 0.0057 (14) | −0.0036 (13) |
Geometric parameters (Å, º) top
Ru1—N1 | 2.132 (3) | C2—H2A | 0.9600 |
Ru1—N3i | 2.135 (3) | C2—H2B | 0.9600 |
Ru1—S3 | 2.2669 (10) | C2—H2C | 0.9600 |
Ru1—S2 | 2.2671 (10) | C3—H3A | 0.9600 |
Ru1—S1 | 2.2772 (11) | C3—H3B | 0.9600 |
Ru1—Cl1 | 2.4258 (11) | C3—H3C | 0.9600 |
S1—O1 | 1.460 (3) | C4—H4A | 0.9600 |
S1—C1 | 1.768 (4) | C4—H4B | 0.9600 |
S1—C2 | 1.780 (5) | C4—H4C | 0.9600 |
S2—O3 | 1.467 (3) | C5—H5A | 0.9600 |
S2—C5 | 1.768 (4) | C5—H5B | 0.9600 |
S2—C6 | 1.774 (4) | C5—H5C | 0.9600 |
S3—O2 | 1.468 (3) | C6—H6A | 0.9600 |
S3—C3 | 1.776 (4) | C6—H6B | 0.9600 |
S3—C4 | 1.781 (4) | C6—H6C | 0.9600 |
C1—H1A | 0.9600 | N1—N2 | 1.171 (4) |
C1—H1B | 0.9600 | N2—N3 | 1.171 (4) |
C1—H1C | 0.9600 | N3—Ru1i | 2.135 (3) |
| | | |
N1—Ru1—N3i | 86.60 (11) | S1—C1—H1C | 109.5 |
N1—Ru1—S3 | 86.86 (9) | H1A—C1—H1C | 109.5 |
N3i—Ru1—S3 | 90.07 (9) | H1B—C1—H1C | 109.5 |
N1—Ru1—S2 | 90.84 (8) | S1—C2—H2A | 109.5 |
N3i—Ru1—S2 | 176.83 (8) | S1—C2—H2B | 109.5 |
S3—Ru1—S2 | 91.66 (4) | H2A—C2—H2B | 109.5 |
N1—Ru1—S1 | 172.80 (8) | S1—C2—H2C | 109.5 |
N3i—Ru1—S1 | 86.58 (8) | H2A—C2—H2C | 109.5 |
S3—Ru1—S1 | 95.47 (4) | H2B—C2—H2C | 109.5 |
S2—Ru1—S1 | 95.90 (4) | S3—C3—H3A | 109.5 |
N1—Ru1—Cl1 | 86.60 (9) | S3—C3—H3B | 109.5 |
N3i—Ru1—Cl1 | 89.52 (9) | H3A—C3—H3B | 109.5 |
S3—Ru1—Cl1 | 173.46 (4) | S3—C3—H3C | 109.5 |
S2—Ru1—Cl1 | 88.46 (4) | H3A—C3—H3C | 109.5 |
S1—Ru1—Cl1 | 91.02 (4) | H3B—C3—H3C | 109.5 |
O1—S1—C1 | 107.1 (2) | S3—C4—H4A | 109.5 |
O1—S1—C2 | 106.7 (2) | S3—C4—H4B | 109.5 |
C1—S1—C2 | 97.9 (2) | H4A—C4—H4B | 109.5 |
O1—S1—Ru1 | 120.15 (14) | S3—C4—H4C | 109.5 |
C1—S1—Ru1 | 109.40 (15) | H4A—C4—H4C | 109.5 |
C2—S1—Ru1 | 113.12 (17) | H4B—C4—H4C | 109.5 |
O3—S2—C5 | 106.98 (18) | S2—C5—H5A | 109.5 |
O3—S2—C6 | 106.7 (2) | S2—C5—H5B | 109.5 |
C5—S2—C6 | 99.1 (2) | H5A—C5—H5B | 109.5 |
O3—S2—Ru1 | 119.10 (11) | S2—C5—H5C | 109.5 |
C5—S2—Ru1 | 108.93 (14) | H5A—C5—H5C | 109.5 |
C6—S2—Ru1 | 113.95 (16) | H5B—C5—H5C | 109.5 |
O2—S3—C3 | 107.09 (18) | S2—C6—H6A | 109.5 |
O2—S3—C4 | 107.08 (19) | S2—C6—H6B | 109.5 |
C3—S3—C4 | 98.5 (2) | H6A—C6—H6B | 109.5 |
O2—S3—Ru1 | 119.90 (12) | S2—C6—H6C | 109.5 |
C3—S3—Ru1 | 111.42 (14) | H6A—C6—H6C | 109.5 |
C4—S3—Ru1 | 110.64 (14) | H6B—C6—H6C | 109.5 |
S1—C1—H1A | 109.5 | N2—N1—Ru1 | 122.2 (2) |
S1—C1—H1B | 109.5 | N3—N2—N1 | 176.6 (3) |
H1A—C1—H1B | 109.5 | N2—N3—Ru1i | 121.3 (2) |
| | | |
N1—Ru1—S1—O1 | 154.9 (7) | N3i—Ru1—S2—C6 | −92.6 (16) |
N3i—Ru1—S1—O1 | 173.8 (2) | S3—Ru1—S2—C6 | 144.43 (19) |
S3—Ru1—S1—O1 | −96.5 (2) | S1—Ru1—S2—C6 | 48.76 (19) |
S2—Ru1—S1—O1 | −4.2 (2) | Cl1—Ru1—S2—C6 | −42.11 (19) |
Cl1—Ru1—S1—O1 | 84.3 (2) | N1—Ru1—S3—O2 | −157.92 (16) |
N1—Ru1—S1—C1 | 30.5 (7) | N3i—Ru1—S3—O2 | 115.49 (16) |
N3i—Ru1—S1—C1 | 49.3 (2) | S2—Ru1—S3—O2 | −67.17 (15) |
S3—Ru1—S1—C1 | 139.06 (18) | S1—Ru1—S3—O2 | 28.92 (15) |
S2—Ru1—S1—C1 | −128.70 (18) | Cl1—Ru1—S3—O2 | −158.2 (3) |
Cl1—Ru1—S1—C1 | −40.14 (18) | N1—Ru1—S3—C3 | 75.94 (17) |
N1—Ru1—S1—C2 | −77.5 (7) | N3i—Ru1—S3—C3 | −10.66 (17) |
N3i—Ru1—S1—C2 | −58.7 (2) | S2—Ru1—S3—C3 | 166.68 (15) |
S3—Ru1—S1—C2 | 31.1 (2) | S1—Ru1—S3—C3 | −97.23 (15) |
S2—Ru1—S1—C2 | 123.3 (2) | Cl1—Ru1—S3—C3 | 75.7 (4) |
Cl1—Ru1—S1—C2 | −148.1 (2) | N1—Ru1—S3—C4 | −32.57 (18) |
N1—Ru1—S2—O3 | 103.88 (16) | N3i—Ru1—S3—C4 | −119.16 (18) |
N3i—Ru1—S2—O3 | 140.0 (15) | S2—Ru1—S3—C4 | 58.18 (16) |
S3—Ru1—S2—O3 | 17.00 (14) | S1—Ru1—S3—C4 | 154.27 (16) |
S1—Ru1—S2—O3 | −78.68 (14) | Cl1—Ru1—S3—C4 | −32.8 (4) |
Cl1—Ru1—S2—O3 | −169.54 (14) | N3i—Ru1—N1—N2 | −51.1 (3) |
N1—Ru1—S2—C5 | −19.09 (19) | S3—Ru1—N1—N2 | −141.4 (3) |
N3i—Ru1—S2—C5 | 17.0 (16) | S2—Ru1—N1—N2 | 127.0 (3) |
S3—Ru1—S2—C5 | −105.96 (17) | S1—Ru1—N1—N2 | −32.3 (9) |
S1—Ru1—S2—C5 | 158.36 (17) | Cl1—Ru1—N1—N2 | 38.6 (3) |
Cl1—Ru1—S2—C5 | 67.49 (17) | Ru1—N1—N2—N3 | −144 (6) |
N1—Ru1—S2—C6 | −128.7 (2) | N1—N2—N3—Ru1i | −147 (6) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1A···Cl1 | 0.96 | 2.72 | 3.307 (4) | 120 |
C2—H2C···O2 | 0.96 | 2.42 | 3.102 (6) | 128 |
C4—H4B···N1 | 0.96 | 2.47 | 3.007 (5) | 115 |
C6—H6B···Cl1 | 0.96 | 2.73 | 3.349 (5) | 123 |
C6—H6C···O1 | 0.96 | 2.35 | 3.110 (6) | 135 |
C3—H3B···Cl1i | 0.96 | 2.94 | 3.891 (4) | 171 |
C1—H1B···N3i | 0.96 | 2.66 | 3.191 (5) | 115 |
C1—H1C···O3ii | 0.96 | 2.59 | 3.261 (5) | 127 |
C3—H3C···O1iii | 0.96 | 2.51 | 3.411 (5) | 157 |
C6—H6A···Cl1iv | 0.96 | 2.87 | 3.589 (4) | 133 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1/2, y−1/2, −z+3/2; (iii) x−1/2, −y+3/2, z−1/2; (iv) −x+3/2, y+1/2, −z+3/2. |