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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804013686/na6335sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804013686/na6335Isup2.hkl
Contains datablock I

CCDC reference: 223750

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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.

(I) top
Crystal data top
C6H18ClN3O3RuS3F(000) = 832
Mr = 412.93Dx = 1.908 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.141 (2) ÅCell parameters from 1005 reflections
b = 11.822 (3) Åθ = 3.0–26.2°
c = 14.934 (4) ŵ = 1.71 mm1
β = 90.217 (5)°T = 293 K
V = 1437.2 (7) Å3Block, red
Z = 40.26 × 0.14 × 0.10 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2915 independent reflections
Radiation source: fine-focus sealed tube2276 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
φ and ω scansθmax = 26.4°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 810
Tmin = 0.652, Tmax = 0.843k = 1412
8004 measured reflectionsl = 1818
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)] = 0.030H-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 reflectionsΔρmax = 0.49 e Å3
161 parametersΔρmin = 0.46 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction 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
xyzUiso*/Ueq
Ru10.42731 (3)0.67009 (2)0.597285 (17)0.02198 (10)
S10.31715 (12)0.66660 (8)0.73720 (6)0.0352 (2)
S20.55279 (10)0.84024 (7)0.61254 (6)0.0280 (2)
S30.20576 (10)0.75063 (7)0.53057 (6)0.0281 (2)
O10.3548 (5)0.7567 (3)0.8009 (2)0.0765 (11)
O20.0984 (3)0.8260 (2)0.58216 (19)0.0452 (7)
O30.4547 (3)0.9437 (2)0.60392 (19)0.0406 (7)
C10.3673 (6)0.5370 (4)0.7898 (3)0.0540 (13)
H1A0.48450.52980.79390.081*
H1B0.32360.47550.75520.081*
H1C0.32090.53550.84880.081*
C20.0998 (5)0.6506 (5)0.7366 (3)0.0721 (16)
H2A0.06320.63130.79570.108*
H2B0.06950.59150.69570.108*
H2C0.04950.72020.71820.108*
C30.0779 (5)0.6474 (3)0.4792 (3)0.0422 (10)
H3A0.02430.60360.52470.063*
H3B0.14350.59850.44260.063*
H3C0.00320.68440.44270.063*
C40.2652 (5)0.8257 (4)0.4325 (3)0.0474 (10)
H4A0.16920.85460.40290.071*
H4B0.32250.77550.39290.071*
H4C0.33590.88730.44890.071*
C50.7135 (5)0.8499 (3)0.5336 (3)0.0459 (11)
H5A0.66790.85240.47430.069*
H5B0.78380.78510.53920.069*
H5C0.77590.91740.54450.069*
C60.6698 (6)0.8540 (4)0.7124 (3)0.0577 (13)
H6A0.72990.92380.71110.086*
H6B0.74530.79190.71710.086*
H6C0.59750.85370.76310.086*
Cl10.67715 (12)0.58134 (9)0.65165 (7)0.0445 (3)
N10.5266 (4)0.6509 (2)0.46627 (19)0.0311 (7)
N20.6004 (4)0.5703 (3)0.44499 (19)0.0296 (7)
N30.6792 (4)0.4933 (2)0.42110 (19)0.0308 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.02541 (15)0.01892 (15)0.02162 (15)0.00301 (12)0.00049 (10)0.00092 (12)
S10.0429 (5)0.0374 (5)0.0253 (5)0.0014 (5)0.0042 (4)0.0014 (4)
S20.0276 (4)0.0240 (5)0.0324 (5)0.0004 (4)0.0017 (4)0.0037 (4)
S30.0285 (5)0.0241 (4)0.0317 (5)0.0030 (4)0.0050 (4)0.0030 (4)
O10.126 (3)0.067 (2)0.0367 (18)0.029 (2)0.019 (2)0.0195 (17)
O20.0386 (15)0.0422 (16)0.0549 (18)0.0141 (13)0.0032 (13)0.0140 (14)
O30.0394 (16)0.0228 (13)0.0595 (19)0.0051 (11)0.0035 (14)0.0032 (12)
C10.059 (3)0.062 (3)0.041 (3)0.010 (2)0.011 (2)0.024 (2)
C20.045 (3)0.118 (5)0.053 (3)0.016 (3)0.020 (2)0.021 (3)
C30.041 (2)0.040 (2)0.046 (2)0.0049 (18)0.0151 (19)0.0048 (19)
C40.054 (3)0.045 (2)0.043 (2)0.003 (2)0.011 (2)0.015 (2)
C50.036 (2)0.039 (2)0.063 (3)0.0066 (18)0.015 (2)0.006 (2)
C60.069 (3)0.054 (3)0.050 (3)0.012 (2)0.026 (2)0.008 (2)
Cl10.0435 (6)0.0411 (6)0.0489 (6)0.0091 (5)0.0046 (5)0.0074 (5)
N10.0410 (18)0.0224 (17)0.0300 (17)0.0021 (13)0.0106 (14)0.0040 (12)
N20.0357 (18)0.0281 (18)0.0250 (16)0.0065 (15)0.0015 (13)0.0028 (14)
N30.0369 (17)0.0205 (15)0.0350 (17)0.0012 (14)0.0057 (14)0.0036 (13)
Geometric parameters (Å, º) top
Ru1—N12.132 (3)C2—H2A0.9600
Ru1—N3i2.135 (3)C2—H2B0.9600
Ru1—S32.2669 (10)C2—H2C0.9600
Ru1—S22.2671 (10)C3—H3A0.9600
Ru1—S12.2772 (11)C3—H3B0.9600
Ru1—Cl12.4258 (11)C3—H3C0.9600
S1—O11.460 (3)C4—H4A0.9600
S1—C11.768 (4)C4—H4B0.9600
S1—C21.780 (5)C4—H4C0.9600
S2—O31.467 (3)C5—H5A0.9600
S2—C51.768 (4)C5—H5B0.9600
S2—C61.774 (4)C5—H5C0.9600
S3—O21.468 (3)C6—H6A0.9600
S3—C31.776 (4)C6—H6B0.9600
S3—C41.781 (4)C6—H6C0.9600
C1—H1A0.9600N1—N21.171 (4)
C1—H1B0.9600N2—N31.171 (4)
C1—H1C0.9600N3—Ru1i2.135 (3)
N1—Ru1—N3i86.60 (11)S1—C1—H1C109.5
N1—Ru1—S386.86 (9)H1A—C1—H1C109.5
N3i—Ru1—S390.07 (9)H1B—C1—H1C109.5
N1—Ru1—S290.84 (8)S1—C2—H2A109.5
N3i—Ru1—S2176.83 (8)S1—C2—H2B109.5
S3—Ru1—S291.66 (4)H2A—C2—H2B109.5
N1—Ru1—S1172.80 (8)S1—C2—H2C109.5
N3i—Ru1—S186.58 (8)H2A—C2—H2C109.5
S3—Ru1—S195.47 (4)H2B—C2—H2C109.5
S2—Ru1—S195.90 (4)S3—C3—H3A109.5
N1—Ru1—Cl186.60 (9)S3—C3—H3B109.5
N3i—Ru1—Cl189.52 (9)H3A—C3—H3B109.5
S3—Ru1—Cl1173.46 (4)S3—C3—H3C109.5
S2—Ru1—Cl188.46 (4)H3A—C3—H3C109.5
S1—Ru1—Cl191.02 (4)H3B—C3—H3C109.5
O1—S1—C1107.1 (2)S3—C4—H4A109.5
O1—S1—C2106.7 (2)S3—C4—H4B109.5
C1—S1—C297.9 (2)H4A—C4—H4B109.5
O1—S1—Ru1120.15 (14)S3—C4—H4C109.5
C1—S1—Ru1109.40 (15)H4A—C4—H4C109.5
C2—S1—Ru1113.12 (17)H4B—C4—H4C109.5
O3—S2—C5106.98 (18)S2—C5—H5A109.5
O3—S2—C6106.7 (2)S2—C5—H5B109.5
C5—S2—C699.1 (2)H5A—C5—H5B109.5
O3—S2—Ru1119.10 (11)S2—C5—H5C109.5
C5—S2—Ru1108.93 (14)H5A—C5—H5C109.5
C6—S2—Ru1113.95 (16)H5B—C5—H5C109.5
O2—S3—C3107.09 (18)S2—C6—H6A109.5
O2—S3—C4107.08 (19)S2—C6—H6B109.5
C3—S3—C498.5 (2)H6A—C6—H6B109.5
O2—S3—Ru1119.90 (12)S2—C6—H6C109.5
C3—S3—Ru1111.42 (14)H6A—C6—H6C109.5
C4—S3—Ru1110.64 (14)H6B—C6—H6C109.5
S1—C1—H1A109.5N2—N1—Ru1122.2 (2)
S1—C1—H1B109.5N3—N2—N1176.6 (3)
H1A—C1—H1B109.5N2—N3—Ru1i121.3 (2)
N1—Ru1—S1—O1154.9 (7)N3i—Ru1—S2—C692.6 (16)
N3i—Ru1—S1—O1173.8 (2)S3—Ru1—S2—C6144.43 (19)
S3—Ru1—S1—O196.5 (2)S1—Ru1—S2—C648.76 (19)
S2—Ru1—S1—O14.2 (2)Cl1—Ru1—S2—C642.11 (19)
Cl1—Ru1—S1—O184.3 (2)N1—Ru1—S3—O2157.92 (16)
N1—Ru1—S1—C130.5 (7)N3i—Ru1—S3—O2115.49 (16)
N3i—Ru1—S1—C149.3 (2)S2—Ru1—S3—O267.17 (15)
S3—Ru1—S1—C1139.06 (18)S1—Ru1—S3—O228.92 (15)
S2—Ru1—S1—C1128.70 (18)Cl1—Ru1—S3—O2158.2 (3)
Cl1—Ru1—S1—C140.14 (18)N1—Ru1—S3—C375.94 (17)
N1—Ru1—S1—C277.5 (7)N3i—Ru1—S3—C310.66 (17)
N3i—Ru1—S1—C258.7 (2)S2—Ru1—S3—C3166.68 (15)
S3—Ru1—S1—C231.1 (2)S1—Ru1—S3—C397.23 (15)
S2—Ru1—S1—C2123.3 (2)Cl1—Ru1—S3—C375.7 (4)
Cl1—Ru1—S1—C2148.1 (2)N1—Ru1—S3—C432.57 (18)
N1—Ru1—S2—O3103.88 (16)N3i—Ru1—S3—C4119.16 (18)
N3i—Ru1—S2—O3140.0 (15)S2—Ru1—S3—C458.18 (16)
S3—Ru1—S2—O317.00 (14)S1—Ru1—S3—C4154.27 (16)
S1—Ru1—S2—O378.68 (14)Cl1—Ru1—S3—C432.8 (4)
Cl1—Ru1—S2—O3169.54 (14)N3i—Ru1—N1—N251.1 (3)
N1—Ru1—S2—C519.09 (19)S3—Ru1—N1—N2141.4 (3)
N3i—Ru1—S2—C517.0 (16)S2—Ru1—N1—N2127.0 (3)
S3—Ru1—S2—C5105.96 (17)S1—Ru1—N1—N232.3 (9)
S1—Ru1—S2—C5158.36 (17)Cl1—Ru1—N1—N238.6 (3)
Cl1—Ru1—S2—C567.49 (17)Ru1—N1—N2—N3144 (6)
N1—Ru1—S2—C6128.7 (2)N1—N2—N3—Ru1i147 (6)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···Cl10.962.723.307 (4)120
C2—H2C···O20.962.423.102 (6)128
C4—H4B···N10.962.473.007 (5)115
C6—H6B···Cl10.962.733.349 (5)123
C6—H6C···O10.962.353.110 (6)135
C3—H3B···Cl1i0.962.943.891 (4)171
C1—H1B···N3i0.962.663.191 (5)115
C1—H1C···O3ii0.962.593.261 (5)127
C3—H3C···O1iii0.962.513.411 (5)157
C6—H6A···Cl1iv0.962.873.589 (4)133
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1/2, y1/2, z+3/2; (iii) x1/2, y+3/2, z1/2; (iv) x+3/2, y+1/2, z+3/2.
 

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