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The title compound, [Ru(C12H7Br2N2)2(CO)2], possesses a distorted octa­hedral environment about the Ru atom, with two cyclo­metallated 4,4'-dibromo­azobenzene ligands and two mutually cis carbonyl ligands. The donor atoms are arranged such that the N atoms are mutually trans and the aryl C atoms are trans to carbonyl ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805041358/cf6479sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805041358/cf6479Isup2.hkl
Contains datablock I

CCDC reference: 296734

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.024
  • wR factor = 0.028
  • Data-to-parameter ratio = 12.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT431_ALERT_2_B Short Inter HL..A Contact Br12 .. N12 .. 3.09 Ang.
Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru1 - C1 .. 6.37 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru1 - C2 .. 5.88 su PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 14
Alert level G
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

The title compound (I) has been prepared as a minor product from the reaction of Ru3(CO)12 and 4,4'-dibromoazobenzene in refluxing n-octane; the major product is the cluster complex Ru33-NC6H4Br)2(CO)9 (Willis et al., 2005). Two strong ν(CO) absorptions at 2047 and 1984 cm−1 in the IR spectrum of (I) are consistent with the presence of two mutually cis carbonyl groups. The crystal structure was investigated to ascertain the relative dispositions of the remaining C and N donor atoms of the two cyclometallated 4,4'-dibromoazobenzene ligands.

The complex possesses a distorted octahedral coordination at the Ru atom and the X-ray study confirms the cis-disposed carbonyl ligands (Fig. 1). The N atoms of the cyclometallated azobenzene ligands are mutually trans, and the aryl C atoms are trans to the carbonyl ligands.

For ruthenium complexes of this type, i.e. with cis monodentate ligands and two N,C-cyclometallated ligands, three different arrangements of the cyclometallated donor atoms are possible. An analogue containing azobenzene residues Ru(C6H4N=NPh)2(CO)2 (Bruce et al., 1987) and a further minor product from the present reaction (Willis et al., 2006) possesses one configuration, in which one N atom is trans to an aryl C, while the other N atom is trans to a carbonyl ligand, with the other aryl C trans to the remaining carbonyl ligand. The second possibility, in which each of the N atoms is trans to a carbonyl ligand, is seen in Ru(C13H8N)2(CO)2 (Patrick et al., 1983). Compound (I) has the third configuration, not previously observed for ruthenium complexes with ligands of this type.

Experimental top

Ru3(CO)12 (200 mg, 0.31 mmol) was added to a solution of 4,4'-dibromoazobenzene (210 mg, 0.62 mmol) in n-octane (30 ml), and the mixture heated at reflux for 4 h. The resulting brown solution was taken to dryness on a rotary evaporator, and the residue dissolved in a minimum of CH2Cl2 (ca 3 ml) and applied to preparative thin-layer chromatography plates. Elution with CH2Cl2/petrol ether (1/9) gave four bands and a heavy baseline: band 1 was yellow (RF =)/4; band 2 was orange (RF = 0.52); band 3 was yellow (RF = 0.21); band 4 (RF = 0.10) was yellow. The contents of band 4 were identified as Ru(CO)2(C12H7Br2N2)2, compound (I), (50 mg, 19%). MS (secondary ion, Cs+): 837 − 28n ([MnCO]+, n = 0–2. IR (CH2Cl2): ν(CO) 2047 s, 1984 s cm−1. Crystals were obtained by liquid diffusion of methanol into a dichloromethane solution.

Refinement top

H atoms were included at idealized positions and made to ride on their parent atoms, with C—H = 1.00 Å and Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: COLLECT (Nonius, 1997); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ORTEPII (Johnson, 1976) in TEXSAN (Molecular Structure Corporation, 1997); software used to prepare material for publication: CRYSTALS.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing 30% probability displacement ellipsoids. H atoms have been omitted for clarity.
(OC-6–32)-Bis[5-bromo-2-(4-bromophenyldiazenyl)phenyl]dicarbonylruthenium(II) top
Crystal data top
[Ru(C12H7Br2N2)2(CO)2]F(000) = 1592
Mr = 835.11Dx = 2.115 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 32959 reflections
a = 13.5277 (2) Åθ = 3–27°
b = 12.4006 (3) ŵ = 6.73 mm1
c = 15.6585 (2) ÅT = 200 K
β = 93.176 (1)°Block, orange
V = 2622.70 (8) Å30.38 × 0.21 × 0.14 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
4200 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.05
ϕ and ω scansθmax = 27.5°, θmin = 3.3°
Absorption correction: integration
(Coppens, 1970)
h = 1717
Tmin = 0.192, Tmax = 0.497k = 1616
49588 measured reflectionsl = 2020
5998 independent reflections
Refinement top
Refinement on F0 restraints
R[F2 > 2σ(F2)] = 0.025 w = [1-(Fo-Fc)2/36σ2(F)]2/[1.39T0(x)-0.108T1(x) + 0.987T2(x)]
where Ti are Chebychev polynomials and x = Fc/Fmax (Prince, 1982; Watkin, 1994)
wR(F2) = 0.028(Δ/σ)max = 0.002
S = 1.09Δρmax = 0.95 e Å3
4200 reflectionsΔρmin = 0.75 e Å3
334 parameters
Crystal data top
[Ru(C12H7Br2N2)2(CO)2]V = 2622.70 (8) Å3
Mr = 835.11Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.5277 (2) ŵ = 6.73 mm1
b = 12.4006 (3) ÅT = 200 K
c = 15.6585 (2) Å0.38 × 0.21 × 0.14 mm
β = 93.176 (1)°
Data collection top
Nonius KappaCCD
diffractometer
5998 independent reflections
Absorption correction: integration
(Coppens, 1970)
4200 reflections with I > 3σ(I)
Tmin = 0.192, Tmax = 0.497Rint = 0.05
49588 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.025334 parameters
wR(F2) = 0.0280 restraints
S = 1.09Δρmax = 0.95 e Å3
4200 reflectionsΔρmin = 0.75 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.754629 (17)0.578893 (19)0.607309 (15)0.0213
Br111.01812 (3)0.95706 (4)0.70555 (3)0.0492
Br120.67482 (3)0.21752 (3)0.22049 (2)0.0444
Br210.50973 (3)0.84548 (3)0.35052 (2)0.0367
Br220.76775 (3)0.52785 (3)1.09337 (2)0.0402
O10.5920 (2)0.4045 (3)0.5985 (2)0.0552
O20.9309 (2)0.4522 (3)0.68953 (19)0.0492
N110.80505 (18)0.5535 (2)0.48647 (15)0.0227
N120.87088 (19)0.6155 (2)0.45750 (16)0.0261
N210.70005 (18)0.6453 (2)0.71766 (16)0.0227
N220.63669 (19)0.7219 (2)0.71081 (16)0.0255
C10.6526 (3)0.4669 (3)0.6022 (2)0.0305
C20.8628 (2)0.4942 (3)0.6614 (2)0.0287
C1110.9015 (2)0.6964 (3)0.5152 (2)0.0268
C1120.8612 (2)0.6994 (2)0.59614 (19)0.0243
C1130.8980 (2)0.7774 (3)0.6528 (2)0.0273
C1140.9683 (2)0.8511 (3)0.6269 (2)0.0316
C1151.0043 (3)0.8503 (3)0.5457 (2)0.0347
C1160.9710 (2)0.7713 (3)0.4890 (2)0.0329
C1210.7747 (2)0.4695 (2)0.42717 (18)0.0239
C1220.6744 (2)0.4515 (3)0.4089 (2)0.0287
C1230.6446 (3)0.3752 (3)0.3480 (2)0.0309
C1240.7156 (3)0.3172 (3)0.30732 (19)0.0321
C1250.8153 (3)0.3324 (3)0.3269 (2)0.0374
C1260.8453 (3)0.4102 (3)0.3865 (2)0.0334
C2110.6092 (2)0.7485 (2)0.62670 (19)0.0241
C2120.6529 (2)0.6940 (2)0.5592 (2)0.0238
C2130.6234 (2)0.7251 (3)0.4763 (2)0.0269
C2140.5516 (2)0.8055 (3)0.4632 (2)0.0272
C2150.5081 (2)0.8577 (3)0.5299 (2)0.0293
C2160.5378 (2)0.8290 (3)0.6132 (2)0.0297
C2210.7250 (2)0.6190 (3)0.80583 (19)0.0245
C2220.7422 (2)0.5121 (3)0.8293 (2)0.0267
C2230.7555 (2)0.4849 (3)0.9152 (2)0.0292
C2240.7540 (2)0.5655 (3)0.97620 (19)0.0294
C2250.7416 (3)0.6736 (3)0.9538 (2)0.0335
C2260.7258 (3)0.6992 (3)0.8680 (2)0.0303
H11310.87430.78090.71210.0327*
H11511.05310.90570.52850.0417*
H11610.99610.76770.43020.0395*
H12210.62400.49330.43940.0344*
H12310.57270.36220.33370.0370*
H12510.86550.28780.29840.0452*
H12610.91740.42340.40010.0401*
H21310.65330.69010.42630.0322*
H21510.45660.91460.51840.0350*
H21610.50840.86540.66290.0357*
H22210.74500.45500.78440.0321*
H22310.76600.40800.93280.0351*
H22510.74400.73120.99850.0402*
H22610.71490.77610.85060.0363*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.02339 (11)0.01940 (11)0.02132 (11)0.00000 (9)0.00195 (8)0.00054 (9)
Br110.0421 (2)0.0513 (2)0.0549 (2)0.01992 (18)0.00908 (17)0.02564 (19)
Br120.0650 (3)0.0387 (2)0.02878 (17)0.00613 (18)0.00311 (16)0.01149 (14)
Br210.04012 (19)0.03902 (19)0.02996 (17)0.00306 (15)0.00832 (14)0.00638 (14)
Br220.0427 (2)0.0545 (2)0.02356 (16)0.00860 (17)0.00230 (13)0.00586 (14)
O10.0595 (18)0.0520 (18)0.0551 (18)0.0338 (15)0.0127 (14)0.0075 (14)
O20.0369 (14)0.0555 (17)0.0547 (16)0.0144 (13)0.0012 (12)0.0209 (14)
N110.0221 (12)0.0232 (12)0.0227 (12)0.0014 (10)0.0003 (9)0.0003 (10)
N120.0282 (13)0.0270 (13)0.0231 (12)0.0048 (11)0.0009 (10)0.0012 (10)
N210.0237 (12)0.0210 (12)0.0234 (12)0.0000 (10)0.0019 (9)0.0014 (10)
N220.0275 (13)0.0219 (12)0.0272 (13)0.0012 (10)0.0021 (10)0.0007 (10)
C10.0355 (17)0.0271 (16)0.0294 (16)0.0003 (14)0.0064 (13)0.0020 (13)
C20.0345 (17)0.0275 (16)0.0244 (14)0.0019 (13)0.0030 (13)0.0037 (12)
C1110.0271 (15)0.0273 (15)0.0258 (14)0.0029 (12)0.0006 (12)0.0015 (12)
C1120.0234 (14)0.0224 (15)0.0268 (14)0.0020 (11)0.0019 (11)0.0031 (12)
C1130.0267 (15)0.0290 (16)0.0261 (15)0.0003 (13)0.0001 (12)0.0019 (12)
C1140.0267 (15)0.0294 (17)0.0386 (18)0.0034 (13)0.0008 (13)0.0080 (14)
C1150.0304 (17)0.0359 (18)0.0380 (18)0.0104 (14)0.0028 (14)0.0007 (14)
C1160.0317 (17)0.0382 (19)0.0290 (16)0.0079 (14)0.0029 (13)0.0006 (14)
C1210.0304 (15)0.0205 (14)0.0209 (13)0.0005 (12)0.0004 (11)0.0003 (11)
C1220.0308 (16)0.0264 (15)0.0288 (15)0.0001 (13)0.0006 (12)0.0028 (13)
C1230.0320 (16)0.0282 (16)0.0322 (16)0.0045 (14)0.0012 (13)0.0003 (13)
C1240.049 (2)0.0268 (16)0.0199 (14)0.0038 (14)0.0004 (13)0.0033 (12)
C1250.044 (2)0.0368 (19)0.0324 (17)0.0027 (16)0.0086 (15)0.0104 (15)
C1260.0310 (16)0.0361 (19)0.0333 (16)0.0006 (14)0.0029 (13)0.0037 (14)
C2110.0239 (14)0.0228 (14)0.0256 (14)0.0009 (11)0.0018 (11)0.0003 (11)
C2120.0231 (14)0.0206 (14)0.0273 (14)0.0002 (11)0.0002 (11)0.0032 (12)
C2130.0285 (15)0.0245 (15)0.0275 (15)0.0009 (12)0.0010 (12)0.0016 (12)
C2140.0251 (14)0.0254 (15)0.0305 (16)0.0035 (12)0.0036 (12)0.0034 (13)
C2150.0254 (15)0.0283 (16)0.0337 (16)0.0042 (12)0.0026 (12)0.0012 (13)
C2160.0293 (16)0.0273 (16)0.0326 (16)0.0014 (13)0.0033 (13)0.0002 (13)
C2210.0244 (14)0.0271 (15)0.0218 (14)0.0001 (12)0.0007 (11)0.0019 (12)
C2220.0314 (16)0.0240 (15)0.0248 (14)0.0021 (12)0.0017 (12)0.0007 (12)
C2230.0304 (16)0.0281 (16)0.0292 (16)0.0025 (13)0.0022 (13)0.0033 (13)
C2240.0264 (14)0.0403 (19)0.0216 (14)0.0037 (13)0.0022 (11)0.0004 (13)
C2250.0416 (19)0.0324 (18)0.0264 (16)0.0033 (15)0.0009 (13)0.0030 (13)
C2260.0395 (18)0.0234 (15)0.0280 (15)0.0034 (13)0.0001 (13)0.0025 (12)
Geometric parameters (Å, º) top
Ru1—N112.071 (2)C121—C1261.388 (4)
Ru1—N212.086 (2)C122—C1231.387 (5)
Ru1—C11.957 (3)C122—H12211.000
Ru1—C21.956 (3)C123—C1241.383 (5)
Ru1—C1122.090 (3)C123—H12311.000
Ru1—C2122.093 (3)C124—C1251.380 (5)
Br11—C1141.898 (3)C125—C1261.387 (5)
Br12—C1241.897 (3)C125—H12511.000
Br21—C2141.889 (3)C126—H12611.000
Br22—C2241.892 (3)C211—C2121.412 (4)
O1—C11.127 (4)C211—C2161.396 (4)
O2—C21.127 (4)C212—C2131.392 (4)
N11—N121.279 (4)C213—C2141.399 (4)
N11—C1211.439 (4)C213—H21311.000
N12—C1111.397 (4)C214—C2151.388 (5)
N21—N221.280 (4)C215—C2161.390 (5)
N21—C2211.440 (4)C215—H21511.000
N22—C2111.388 (4)C216—H21611.000
C111—C1121.407 (4)C221—C2221.392 (4)
C111—C1161.399 (4)C221—C2261.391 (4)
C112—C1131.387 (4)C222—C2231.390 (4)
C113—C1141.395 (5)C222—H22211.000
C113—H11311.000C223—C2241.382 (5)
C114—C1151.387 (5)C223—H22311.000
C115—C1161.380 (5)C224—C2251.394 (5)
C115—H11511.000C225—C2261.385 (5)
C116—H11611.000C225—H22511.000
C121—C1221.390 (4)C226—H22611.000
Br11···C123i3.436 (4)O2···N22v3.404 (4)
Br11···O1ii3.545 (3)O2···C216v3.451 (4)
Br11···C222ii3.599 (3)C113···C223ii3.438 (5)
Br12···N12iii3.092 (2)C113···C222ii3.494 (5)
Br21···O1iv3.502 (4)C114···C223ii3.483 (4)
O1···C214iv3.359 (5)C114···C222ii3.575 (4)
O1···C213iv3.474 (4)C211···C223ii3.537 (4)
O1···C226v3.562 (5)C216···C223ii3.448 (4)
N11—Ru1—N21165.18 (10)C122—C123—C124119.2 (3)
N11—Ru1—C197.02 (12)C122—C123—H1231120.377
N21—Ru1—C191.87 (12)C124—C123—H1231120.380
N11—Ru1—C292.13 (11)Br12—C124—C123119.1 (3)
N21—Ru1—C298.29 (12)Br12—C124—C125119.3 (3)
C1—Ru1—C298.38 (14)C123—C124—C125121.5 (3)
N11—Ru1—C11276.62 (11)C124—C125—C126119.3 (3)
N21—Ru1—C11293.71 (11)C124—C125—H1251120.331
C1—Ru1—C112172.86 (12)C126—C125—H1251120.330
C2—Ru1—C11285.23 (12)C121—C126—C125119.6 (3)
N11—Ru1—C21291.05 (11)C121—C126—H1261120.177
N21—Ru1—C21276.88 (11)C125—C126—H1261120.177
C1—Ru1—C21291.21 (13)N22—C211—C212119.6 (3)
C2—Ru1—C212169.44 (13)N22—C211—C216117.4 (3)
C112—Ru1—C21285.72 (11)C212—C211—C216123.0 (3)
Ru1—N11—N12120.3 (2)C211—C212—Ru1110.6 (2)
Ru1—N11—C121127.09 (19)C211—C212—C213117.1 (3)
N12—N11—C121112.7 (2)Ru1—C212—C213132.3 (2)
N11—N12—C111112.9 (3)C212—C213—C214119.7 (3)
Ru1—N21—N22119.32 (19)C212—C213—H2131120.165
Ru1—N21—C221129.05 (19)C214—C213—H2131120.168
N22—N21—C221111.6 (2)Br21—C214—C213119.6 (2)
N21—N22—C211113.5 (2)Br21—C214—C215117.6 (2)
Ru1—C1—O1178.1 (3)C213—C214—C215122.9 (3)
Ru1—C2—O2173.6 (3)C214—C215—C216118.3 (3)
N12—C111—C112119.0 (3)C214—C215—H2151120.849
N12—C111—C116117.8 (3)C216—C215—H2151120.847
C112—C111—C116123.1 (3)C211—C216—C215119.1 (3)
C111—C112—Ru1111.1 (2)C211—C216—H2161120.446
C111—C112—C113116.8 (3)C215—C216—H2161120.448
Ru1—C112—C113132.1 (2)N21—C221—C222119.7 (3)
C112—C113—C114119.9 (3)N21—C221—C226120.1 (3)
C112—C113—H1131120.071C222—C221—C226120.1 (3)
C114—C113—H1131120.069C221—C222—C223119.8 (3)
Br11—C114—C113119.2 (3)C221—C222—H2221120.090
Br11—C114—C115118.0 (3)C223—C222—H2221120.091
C113—C114—C115122.8 (3)C222—C223—C224119.2 (3)
C114—C115—C116118.4 (3)C222—C223—H2231120.417
C114—C115—H1151120.790C224—C223—H2231120.418
C116—C115—H1151120.790Br22—C224—C223119.1 (3)
C111—C116—C115118.9 (3)Br22—C224—C225119.0 (2)
C111—C116—H1161120.544C223—C224—C225121.8 (3)
C115—C116—H1161120.538C224—C225—C226118.4 (3)
N11—C121—C122119.3 (3)C224—C225—H2251120.812
N11—C121—C126120.1 (3)C226—C225—H2251120.813
C122—C121—C126120.6 (3)C221—C226—C225120.6 (3)
C121—C122—C123119.7 (3)C221—C226—H2261119.706
C121—C122—H1221120.171C225—C226—H2261119.707
C123—C122—H1221120.170
Ru1—N11—N12—C1110.2 (3)N22—N21—Ru1—C2121.8 (2)
Ru1—N11—C121—C12249.7 (3)N22—N21—C221—C222143.3 (3)
Ru1—N11—C121—C126132.7 (3)N22—N21—C221—C22632.6 (4)
Ru1—N21—N22—C2112.4 (3)N22—C211—C212—C213179.2 (3)
Ru1—N21—C221—C22238.1 (4)N22—C211—C216—C215179.8 (3)
Ru1—N21—C221—C226145.9 (3)C1—Ru1—N11—C1215.3 (2)
Ru1—C112—C111—N122.8 (3)C1—Ru1—N21—C22188.9 (3)
Ru1—C112—C111—C116176.8 (2)C1—Ru1—C212—C21192.4 (2)
Ru1—C112—C113—C114178.0 (2)C1—Ru1—C212—C21388.4 (3)
Ru1—C212—C211—N220.2 (3)C2—Ru1—N11—C12193.4 (2)
Ru1—C212—C211—C216179.4 (2)C2—Ru1—N21—C2219.8 (3)
Ru1—C212—C213—C214179.4 (2)C2—Ru1—C112—C11195.4 (2)
Br11—C114—C113—C112179.8 (2)C2—Ru1—C112—C11383.7 (3)
Br11—C114—C115—C116177.9 (3)C111—N12—N11—C121179.3 (2)
Br12—C124—C123—C122177.2 (3)C111—C112—Ru1—C21290.0 (2)
Br12—C124—C125—C126175.9 (3)C111—C112—C113—C1142.9 (4)
Br21—C214—C213—C212178.7 (2)C111—C116—C115—C1140.9 (5)
Br21—C214—C215—C216179.8 (2)C112—Ru1—N11—C121178.0 (2)
Br22—C224—C223—C222177.9 (2)C112—Ru1—N21—C22195.6 (3)
Br22—C224—C225—C226176.3 (3)C112—Ru1—C212—C21194.1 (2)
N11—Ru1—C112—C1112.1 (2)C112—Ru1—C212—C21385.2 (3)
N11—Ru1—C112—C113177.1 (3)C112—C111—C116—C1152.0 (5)
N11—Ru1—C212—C211170.6 (2)C112—C113—C114—C1150.2 (5)
N11—Ru1—C212—C2138.6 (3)C113—C112—Ru1—C21290.8 (3)
N11—N12—C111—C1121.8 (4)C113—C112—C111—C1163.9 (4)
N11—N12—C111—C116177.8 (3)C113—C114—C115—C1161.8 (5)
N11—C121—C122—C123176.1 (3)C121—N11—Ru1—C21296.6 (2)
N11—C121—C126—C125177.4 (3)C121—C122—C123—C1240.9 (5)
N12—N11—Ru1—C1175.4 (2)C121—C126—C125—C1241.7 (5)
N12—N11—Ru1—C285.9 (2)C122—C121—C126—C1250.1 (5)
N12—N11—Ru1—C1121.3 (2)C122—C123—C124—C1251.0 (5)
N12—N11—Ru1—C21284.0 (2)C123—C122—C121—C1261.5 (5)
N12—N11—C121—C122130.9 (3)C123—C124—C125—C1262.3 (5)
N12—N11—C121—C12646.7 (4)C211—N22—N21—C221178.9 (2)
N12—C111—C112—C113176.5 (3)C211—C212—C213—C2141.4 (4)
N12—C111—C116—C115178.3 (3)C211—C216—C215—C2140.6 (5)
N21—Ru1—C112—C111166.6 (2)C212—Ru1—N21—C221179.7 (3)
N21—Ru1—C112—C11314.3 (3)C212—C211—C216—C2150.2 (4)
N21—Ru1—C212—C2110.8 (2)C212—C213—C214—C2150.7 (5)
N21—Ru1—C212—C213180.0 (3)C213—C212—C211—C2161.3 (4)
N21—N22—C211—C2121.6 (4)C213—C214—C215—C2160.4 (5)
N21—N22—C211—C216178.0 (3)C221—C222—C223—C2241.7 (4)
N21—C221—C222—C223172.9 (3)C221—C226—C225—C2241.7 (6)
N21—C221—C226—C225174.6 (3)C222—C221—C226—C2251.3 (5)
N22—N21—Ru1—C192.6 (2)C222—C223—C224—C2251.4 (4)
N22—N21—Ru1—C2168.6 (2)C223—C222—C221—C2263.1 (4)
N22—N21—Ru1—C11282.9 (2)C223—C224—C225—C2263.1 (5)
Symmetry codes: (i) x+1/2, y+3/2, z+1/2; (ii) x+3/2, y+1/2, z+3/2; (iii) x+3/2, y1/2, z+1/2; (iv) x+1, y+1, z+1; (v) x+3/2, y1/2, z+3/2.

Experimental details

Crystal data
Chemical formula[Ru(C12H7Br2N2)2(CO)2]
Mr835.11
Crystal system, space groupMonoclinic, P21/n
Temperature (K)200
a, b, c (Å)13.5277 (2), 12.4006 (3), 15.6585 (2)
β (°) 93.176 (1)
V3)2622.70 (8)
Z4
Radiation typeMo Kα
µ (mm1)6.73
Crystal size (mm)0.38 × 0.21 × 0.14
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionIntegration
(Coppens, 1970)
Tmin, Tmax0.192, 0.497
No. of measured, independent and
observed [I > 3σ(I)] reflections
49588, 5998, 4200
Rint0.05
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.028, 1.09
No. of reflections4200
No. of parameters334
Δρmax, Δρmin (e Å3)0.95, 0.75

Computer programs: COLLECT (Nonius, 1997), DENZO/SCALEPACK (Otwinowski & Minor, 1997), DENZO/SCALEPACK, SIR92 (Altomare et al., 1994), CRYSTALS (Betteridge et al., 2003), ORTEPII (Johnson, 1976) in TEXSAN (Molecular Structure Corporation, 1997), CRYSTALS.

Selected geometric parameters (Å, º) top
Ru1—N112.071 (2)Ru1—C21.956 (3)
Ru1—N212.086 (2)Ru1—C1122.090 (3)
Ru1—C11.957 (3)Ru1—C2122.093 (3)
N11—Ru1—N21165.18 (10)C1—Ru1—C112172.86 (12)
N11—Ru1—C197.02 (12)C2—Ru1—C11285.23 (12)
N21—Ru1—C191.87 (12)N11—Ru1—C21291.05 (11)
N11—Ru1—C292.13 (11)N21—Ru1—C21276.88 (11)
N21—Ru1—C298.29 (12)C1—Ru1—C21291.21 (13)
C1—Ru1—C298.38 (14)C2—Ru1—C212169.44 (13)
N11—Ru1—C11276.62 (11)C112—Ru1—C21285.72 (11)
N21—Ru1—C11293.71 (11)
 

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