Literature DB >> 22719377

[μ-Bis(di-o-tolyl-phosphan-yl)methane-1:2κ(2)P:P']nona-carbonyl-1κ(3)C,2κ(3)C,3κ(3)C-[tris-(2-chloro-eth-yl) phosphite-3κP]-triangulo-triruthenium(0).

Omar Bin Shawkataly, Imthyaz Ahmed Khan, Siti Syaida Sirat, Ching Kheng Quah, Hoong-Kun Fun.   

Abstract

In the title compound, [Ru(3)(C(6)H(12)Cl(3)O(3)P)(C(29)H(30)P(2))(CO)(9)], the bis-(di-o-tolyl-phosphan-yl)methane ligand bridges one Ru-Ru bond and the monodentate phosphite ligand bonds to the third Ru atom. Both ligands are equatorial with respect to the Ru(3) triangle. Each Ru atom bears one equatorial and two axial terminal carbonyl ligands. The dihedral angles between the two benzene rings in the diphenyl-phosphanyl groups are 79.52 (10) and 69.88 (10)°. In the crystal, mol-ecules are linked via C-H⋯O hydrogen bonds into chains along [100].

Entities:  

Year:  2012        PMID: 22719377      PMCID: PMC3379179          DOI: 10.1107/S1600536812023707

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For general background to triangulo-triruthenium compounds with general structure Ru3(CO)12- L (L = group 15 ligand) see: Bruce et al. (1985 ▶,1988a ▶,b ▶); Shawkataly et al. (1998 ▶, 2004 ▶, 2010 ▶, 2011 ▶). For the preparation of the di-o-tolyl­phosphan­yl ligand, see: Filby et al. (2006 ▶). For the stability of the temperature controller used in the data collection, see: Cosier & Glazer (1986 ▶).

Experimental

Crystal data

[Ru3(C6H12Cl3O3P)(C29H30P2)(CO)9] M = 1265.25 Monoclinic, a = 10.1705 (6) Å b = 20.7490 (12) Å c = 12.3584 (7) Å β = 109.241 (1)° V = 2462.3 (2) Å3 Z = 2 Mo Kα radiation μ = 1.23 mm−1 T = 100 K 0.63 × 0.30 × 0.09 mm

Data collection

Bruker SMART APEXII DUO CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2009 ▶) T min = 0.513, T max = 0.899 23611 measured reflections 11176 independent reflections 11085 reflections with I > 2σ(I) R int = 0.016

Refinement

R[F 2 > 2σ(F 2)] = 0.016 wR(F 2) = 0.042 S = 1.05 11176 reflections 590 parameters 1 restraint H-atom parameters constrained Δρmax = 0.78 e Å−3 Δρmin = −0.50 e Å−3 Absolute structure: Flack (1983 ▶), 5368 Friedel pairs Flack parameter: 0.016 (10) Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812023707/rz2762sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812023707/rz2762Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ru3(C6H12Cl3O3P)(C29H30P2)(CO)9]F(000) = 1260
Mr = 1265.25Dx = 1.707 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 9989 reflections
a = 10.1705 (6) Åθ = 2.9–30.1°
b = 20.7490 (12) ŵ = 1.23 mm1
c = 12.3584 (7) ÅT = 100 K
β = 109.241 (1)°Plate, brown
V = 2462.3 (2) Å30.63 × 0.30 × 0.09 mm
Z = 2
Bruker SMART APEXII DUO CCD area-detector diffractometer11176 independent reflections
Radiation source: fine-focus sealed tube11085 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.016
φ and ω scansθmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2009)h = −13→13
Tmin = 0.513, Tmax = 0.899k = −26→26
23611 measured reflectionsl = −15→16
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.016H-atom parameters constrained
wR(F2) = 0.042w = 1/[σ2(Fo2) + (0.0205P)2 + 0.6778P] where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
11176 reflectionsΔρmax = 0.78 e Å3
590 parametersΔρmin = −0.50 e Å3
1 restraintAbsolute structure: Flack (1983), 5368 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.016 (10)
Experimental. The crystal was placed in the cold stream of an Oxford Cryosystems Cobra open-flow nitrogen cryostat (Cosier & Glazer, 1986) operating at 100 K.
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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.
xyzUiso*/Ueq
Ru10.944298 (14)0.325120 (7)0.809961 (11)0.00983 (3)
Ru20.765192 (14)0.257429 (7)0.616918 (12)0.01032 (3)
Ru30.788240 (15)0.218119 (7)0.844371 (12)0.01256 (3)
Cl10.27592 (6)0.02481 (3)0.67579 (5)0.02873 (12)
Cl20.70147 (10)−0.02232 (4)0.58668 (6)0.05110 (19)
Cl30.49238 (9)0.17761 (4)1.09900 (7)0.0544 (2)
P10.97101 (5)0.41265 (2)0.69855 (4)0.01024 (9)
P20.84641 (5)0.31652 (2)0.48990 (4)0.01023 (9)
P30.66767 (5)0.12666 (3)0.84199 (4)0.01523 (10)
O10.72264 (15)0.40026 (8)0.87717 (13)0.0205 (3)
O21.14022 (17)0.35167 (9)1.05085 (13)0.0280 (4)
O31.17618 (15)0.24273 (7)0.77020 (13)0.0210 (3)
O40.55800 (15)0.36598 (8)0.61476 (13)0.0214 (3)
O50.55140 (16)0.17020 (8)0.45254 (14)0.0241 (3)
O60.96944 (16)0.14721 (8)0.62476 (13)0.0222 (3)
O70.50273 (18)0.28256 (8)0.79736 (17)0.0318 (4)
O80.8773 (2)0.24850 (11)1.09856 (14)0.0409 (5)
O91.05262 (17)0.13615 (9)0.88318 (15)0.0279 (4)
O100.50288 (16)0.12107 (8)0.77775 (13)0.0226 (3)
O110.73473 (16)0.06597 (7)0.80111 (15)0.0242 (3)
O120.66222 (17)0.10944 (8)0.96670 (14)0.0262 (3)
C10.86732 (19)0.48302 (9)0.71299 (16)0.0127 (4)
C20.9109 (2)0.52284 (10)0.81082 (17)0.0162 (4)
C30.8240 (2)0.57358 (10)0.81935 (18)0.0177 (4)
H3A0.85210.59980.88400.021*
C40.6980 (2)0.58619 (10)0.73529 (19)0.0194 (4)
H4A0.64380.62090.74250.023*
C50.6533 (2)0.54589 (10)0.63914 (18)0.0175 (4)
H5A0.56810.55310.58240.021*
C60.7371 (2)0.49519 (10)0.62942 (17)0.0156 (4)
H6A0.70640.46830.56580.019*
C71.14826 (18)0.44366 (9)0.72276 (16)0.0120 (3)
C81.1781 (2)0.49736 (10)0.66462 (16)0.0143 (4)
C91.3178 (2)0.51406 (10)0.68754 (17)0.0183 (4)
H9A1.33930.54970.65080.022*
C101.4259 (2)0.47910 (10)0.76359 (18)0.0176 (4)
H10A1.51780.49090.77570.021*
C111.3966 (2)0.42688 (10)0.82107 (17)0.0162 (4)
H11A1.46830.40350.87250.019*
C121.25792 (19)0.40972 (9)0.80080 (16)0.0138 (4)
H12A1.23780.37490.84010.017*
C130.9135 (2)0.39790 (9)0.54139 (15)0.0132 (4)
H13A0.84120.42890.50470.016*
H13B0.99160.40680.51510.016*
C140.72006 (19)0.33745 (9)0.34803 (15)0.0133 (4)
C150.7560 (2)0.36585 (10)0.25707 (16)0.0165 (4)
C160.6482 (2)0.37698 (12)0.15341 (17)0.0233 (5)
H16A0.66980.39570.09300.028*
C170.5111 (2)0.36118 (12)0.13777 (18)0.0267 (5)
H17A0.44270.36880.06750.032*
C180.4757 (2)0.33404 (11)0.22648 (17)0.0213 (4)
H18A0.38370.32340.21690.026*
C190.58066 (19)0.32297 (11)0.33074 (16)0.0167 (4)
H19A0.55680.30530.39090.020*
C200.99155 (19)0.27865 (9)0.45717 (15)0.0124 (4)
C210.9691 (2)0.22669 (10)0.37912 (16)0.0146 (4)
C221.0841 (2)0.20189 (10)0.35464 (18)0.0198 (4)
H22A1.07050.16830.30220.024*
C231.2183 (2)0.22580 (12)0.40620 (19)0.0244 (5)
H23A1.29250.20900.38710.029*
C241.2399 (2)0.27481 (11)0.48596 (19)0.0235 (5)
H24A1.32940.29040.52220.028*
C251.1277 (2)0.30073 (10)0.51188 (17)0.0177 (4)
H25A1.14320.33330.56640.021*
C261.0458 (2)0.51396 (11)0.90788 (18)0.0226 (4)
H26A1.03680.53140.97700.034*
H26B1.11930.53600.89020.034*
H26C1.06740.46890.91820.034*
C271.0691 (2)0.53731 (11)0.57765 (19)0.0219 (4)
H27A1.11290.57360.55550.033*
H27B1.00150.55220.61080.033*
H27C1.02370.51150.51140.033*
C280.9023 (2)0.38464 (11)0.26288 (18)0.0202 (4)
H28A0.89870.40740.19430.030*
H28B0.95800.34650.26980.030*
H28C0.94280.41190.32820.030*
C290.8274 (2)0.19827 (10)0.31925 (17)0.0175 (4)
H29A0.83740.15880.28230.026*
H29B0.77290.22820.26300.026*
H29C0.78150.18980.37440.026*
C300.79802 (19)0.36992 (10)0.84677 (15)0.0142 (4)
C311.0657 (2)0.34207 (10)0.95981 (17)0.0170 (4)
C321.0840 (2)0.27162 (9)0.78005 (16)0.0141 (4)
C330.63816 (19)0.32577 (11)0.62185 (15)0.0155 (4)
C340.6298 (2)0.20390 (10)0.51678 (17)0.0168 (4)
C350.8977 (2)0.18882 (10)0.62918 (16)0.0158 (4)
C360.6115 (2)0.26232 (11)0.81124 (18)0.0206 (4)
C370.8431 (2)0.23582 (11)1.00343 (19)0.0243 (5)
C380.9560 (2)0.16876 (11)0.86278 (18)0.0198 (4)
C390.4397 (2)0.12387 (12)0.65567 (19)0.0251 (5)
H39A0.48610.09430.61930.030*
H39B0.44740.16710.62840.030*
C400.2891 (2)0.10560 (11)0.62675 (19)0.0222 (4)
H40A0.24320.10800.54450.027*
H40B0.24320.13540.66310.027*
C410.6882 (2)−0.00005 (10)0.7999 (2)0.0231 (4)
H41A0.5883−0.00270.76220.028*
H41B0.7099−0.01600.87770.028*
C420.7620 (3)−0.03933 (11)0.7364 (2)0.0281 (5)
H42A0.7480−0.08470.74800.034*
H42B0.8611−0.03060.76720.034*
C430.5575 (3)0.07229 (13)0.9934 (2)0.0329 (6)
H43A0.59910.05121.06680.040*
H43B0.52300.03910.93570.040*
C440.4365 (3)0.11351 (15)0.9983 (2)0.0378 (6)
H44A0.37060.08671.01930.045*
H44B0.38910.13130.92290.045*
U11U22U33U12U13U23
Ru10.00896 (6)0.01019 (7)0.00947 (6)−0.00107 (5)0.00188 (5)0.00001 (5)
Ru20.00989 (6)0.01045 (7)0.00997 (6)−0.00169 (5)0.00238 (5)−0.00079 (5)
Ru30.01346 (7)0.01283 (7)0.01105 (7)−0.00329 (6)0.00359 (5)0.00087 (5)
Cl10.0268 (3)0.0272 (3)0.0268 (3)−0.0127 (2)0.0015 (2)0.0012 (2)
Cl20.0782 (6)0.0479 (4)0.0265 (3)0.0071 (4)0.0162 (3)0.0035 (3)
Cl30.0605 (5)0.0611 (5)0.0514 (4)−0.0233 (4)0.0316 (4)−0.0232 (4)
P10.0102 (2)0.0094 (2)0.0102 (2)−0.00029 (17)0.00210 (17)−0.00042 (16)
P20.00951 (19)0.0108 (2)0.00951 (19)0.00008 (17)0.00197 (16)−0.00049 (17)
P30.0132 (2)0.0138 (2)0.0174 (2)−0.00183 (19)0.00349 (19)0.00325 (18)
O10.0175 (7)0.0215 (8)0.0251 (8)0.0008 (6)0.0105 (6)−0.0009 (6)
O20.0252 (8)0.0373 (9)0.0151 (7)−0.0007 (7)−0.0022 (6)−0.0044 (7)
O30.0179 (7)0.0183 (8)0.0275 (8)0.0005 (6)0.0084 (6)−0.0041 (6)
O40.0161 (7)0.0217 (8)0.0252 (7)0.0030 (6)0.0051 (6)−0.0028 (6)
O50.0201 (7)0.0240 (8)0.0247 (8)−0.0077 (6)0.0025 (6)−0.0061 (6)
O60.0220 (7)0.0196 (8)0.0218 (7)0.0047 (6)0.0031 (6)−0.0028 (6)
O70.0283 (8)0.0205 (8)0.0540 (11)0.0045 (7)0.0236 (8)0.0057 (8)
O80.0530 (11)0.0525 (13)0.0161 (8)−0.0167 (10)0.0097 (8)−0.0062 (8)
O90.0220 (8)0.0316 (9)0.0301 (9)0.0071 (7)0.0086 (7)0.0129 (7)
O100.0199 (7)0.0241 (8)0.0213 (7)−0.0052 (6)0.0032 (6)0.0011 (6)
O110.0228 (8)0.0144 (8)0.0388 (9)−0.0035 (6)0.0146 (7)−0.0032 (7)
O120.0275 (8)0.0288 (9)0.0238 (8)−0.0068 (7)0.0105 (7)0.0066 (7)
C10.0142 (8)0.0104 (9)0.0147 (8)0.0001 (7)0.0064 (7)0.0020 (7)
C20.0178 (9)0.0140 (10)0.0171 (9)−0.0012 (7)0.0064 (8)0.0010 (7)
C30.0216 (10)0.0136 (10)0.0211 (10)−0.0017 (8)0.0111 (8)−0.0029 (8)
C40.0213 (10)0.0143 (10)0.0270 (11)0.0056 (8)0.0138 (9)0.0051 (8)
C50.0147 (9)0.0182 (10)0.0201 (9)0.0037 (8)0.0064 (8)0.0078 (8)
C60.0149 (9)0.0154 (10)0.0152 (9)−0.0008 (7)0.0033 (7)0.0011 (7)
C70.0104 (8)0.0135 (9)0.0127 (8)−0.0016 (7)0.0045 (7)−0.0032 (7)
C80.0166 (9)0.0119 (9)0.0139 (8)−0.0007 (7)0.0044 (7)−0.0025 (7)
C90.0211 (10)0.0158 (10)0.0193 (9)−0.0042 (8)0.0086 (8)0.0011 (8)
C100.0119 (8)0.0198 (10)0.0226 (10)−0.0034 (7)0.0077 (8)−0.0022 (8)
C110.0133 (9)0.0181 (10)0.0168 (9)0.0009 (7)0.0045 (7)−0.0014 (7)
C120.0134 (8)0.0128 (9)0.0155 (9)−0.0011 (7)0.0052 (7)−0.0010 (7)
C130.0159 (9)0.0118 (9)0.0105 (8)−0.0024 (7)0.0022 (7)−0.0004 (7)
C140.0146 (8)0.0126 (10)0.0102 (8)0.0014 (7)0.0008 (7)−0.0006 (7)
C150.0178 (9)0.0158 (10)0.0132 (8)0.0011 (8)0.0017 (7)−0.0014 (7)
C160.0285 (11)0.0278 (12)0.0126 (9)0.0037 (9)0.0054 (8)0.0029 (8)
C170.0230 (11)0.0334 (13)0.0162 (9)0.0048 (10)−0.0037 (8)0.0025 (9)
C180.0159 (9)0.0231 (12)0.0205 (9)0.0023 (8)0.0001 (8)−0.0015 (8)
C190.0162 (8)0.0160 (9)0.0161 (8)0.0014 (8)0.0030 (7)−0.0008 (8)
C200.0138 (8)0.0125 (9)0.0117 (8)0.0026 (7)0.0052 (7)0.0025 (7)
C210.0180 (9)0.0133 (10)0.0124 (8)0.0020 (7)0.0048 (7)0.0026 (7)
C220.0221 (10)0.0185 (11)0.0190 (9)0.0036 (8)0.0071 (8)−0.0022 (8)
C230.0161 (9)0.0305 (12)0.0287 (11)0.0081 (9)0.0102 (8)0.0009 (9)
C240.0121 (9)0.0309 (13)0.0269 (11)0.0008 (8)0.0058 (8)−0.0016 (9)
C250.0146 (9)0.0210 (10)0.0157 (9)−0.0009 (8)0.0024 (7)−0.0014 (8)
C260.0204 (10)0.0223 (11)0.0196 (10)0.0031 (9)−0.0007 (8)−0.0090 (8)
C270.0192 (10)0.0190 (10)0.0237 (11)−0.0020 (8)0.0020 (8)0.0089 (8)
C280.0225 (10)0.0224 (11)0.0166 (9)−0.0004 (8)0.0077 (8)0.0035 (8)
C290.0182 (9)0.0163 (10)0.0179 (9)−0.0006 (7)0.0057 (8)−0.0043 (7)
C300.0117 (8)0.0161 (10)0.0126 (8)−0.0036 (7)0.0010 (7)0.0012 (7)
C310.0149 (9)0.0172 (10)0.0186 (9)−0.0007 (7)0.0052 (8)−0.0009 (7)
C320.0155 (9)0.0126 (10)0.0125 (8)−0.0044 (7)0.0023 (7)−0.0001 (7)
C330.0138 (8)0.0194 (10)0.0128 (8)−0.0050 (8)0.0036 (7)−0.0022 (8)
C340.0147 (9)0.0194 (11)0.0160 (9)−0.0003 (7)0.0046 (7)0.0002 (7)
C350.0167 (9)0.0168 (10)0.0117 (8)−0.0041 (8)0.0016 (7)−0.0011 (7)
C360.0258 (10)0.0134 (10)0.0262 (10)−0.0049 (9)0.0137 (8)−0.0003 (8)
C370.0266 (11)0.0261 (12)0.0212 (11)−0.0078 (9)0.0091 (9)0.0011 (8)
C380.0194 (10)0.0228 (11)0.0166 (9)−0.0056 (8)0.0051 (8)0.0047 (8)
C390.0241 (11)0.0271 (12)0.0212 (11)−0.0020 (9)0.0035 (9)0.0032 (9)
C400.0178 (10)0.0223 (11)0.0231 (11)−0.0012 (8)0.0019 (8)0.0008 (8)
C410.0248 (11)0.0125 (10)0.0292 (11)−0.0033 (8)0.0053 (9)0.0018 (8)
C420.0339 (12)0.0194 (11)0.0287 (12)0.0029 (10)0.0071 (10)0.0029 (9)
C430.0349 (13)0.0343 (14)0.0338 (13)−0.0105 (11)0.0170 (11)0.0080 (11)
C440.0358 (14)0.0510 (18)0.0310 (13)−0.0176 (12)0.0169 (11)−0.0111 (12)
Ru1—C311.890 (2)C10—C111.381 (3)
Ru1—C301.931 (2)C10—H10A0.9300
Ru1—C321.933 (2)C11—C121.395 (3)
Ru1—P12.3483 (5)C11—H11A0.9300
Ru1—Ru32.8415 (2)C12—H12A0.9300
Ru1—Ru22.8492 (2)C13—H13A0.9700
Ru2—C341.881 (2)C13—H13B0.9700
Ru2—C351.931 (2)C14—C191.395 (3)
Ru2—C331.933 (2)C14—C151.419 (3)
Ru2—P22.3462 (5)C15—C161.404 (3)
Ru2—Ru32.8614 (2)C15—C281.517 (3)
Ru3—C371.894 (2)C16—C171.382 (3)
Ru3—C381.938 (2)C16—H16A0.9300
Ru3—C361.938 (2)C17—C181.382 (3)
Ru3—P32.2543 (5)C17—H17A0.9300
Cl1—C401.803 (2)C18—C191.395 (3)
Cl2—C421.782 (3)C18—H18A0.9300
Cl3—C441.782 (3)C19—H19A0.9300
P1—C71.8434 (19)C20—C251.402 (3)
P1—C11.844 (2)C20—C211.414 (3)
P1—C131.8600 (19)C21—C221.399 (3)
P2—C201.8313 (19)C21—C291.507 (3)
P2—C141.8518 (19)C22—C231.394 (3)
P2—C131.8534 (19)C22—H22A0.9300
P3—O111.5916 (16)C23—C241.382 (3)
P3—O121.6007 (16)C23—H23A0.9300
P3—O101.6050 (16)C24—C251.392 (3)
O1—C301.147 (2)C24—H24A0.9300
O2—C311.148 (3)C25—H25A0.9300
O3—C321.152 (2)C26—H26A0.9600
O4—C331.150 (3)C26—H26B0.9600
O5—C341.157 (3)C26—H26C0.9600
O6—C351.143 (3)C27—H27A0.9600
O7—C361.142 (3)C27—H27B0.9600
O8—C371.141 (3)C27—H27C0.9600
O9—C381.151 (3)C28—H28A0.9600
O10—C391.433 (3)C28—H28B0.9600
O11—C411.448 (3)C28—H28C0.9600
O12—C431.439 (3)C29—H29A0.9600
C1—C61.408 (3)C29—H29B0.9600
C1—C21.410 (3)C29—H29C0.9600
C2—C31.401 (3)C39—C401.502 (3)
C2—C261.507 (3)C39—H39A0.9700
C3—C41.383 (3)C39—H39B0.9700
C3—H3A0.9300C40—H40A0.9700
C4—C51.401 (3)C40—H40B0.9700
C4—H4A0.9300C41—C421.494 (3)
C5—C61.384 (3)C41—H41A0.9700
C5—H5A0.9300C41—H41B0.9700
C6—H6A0.9300C42—H42A0.9700
C7—C121.400 (3)C42—H42B0.9700
C7—C81.412 (3)C43—C441.516 (4)
C8—C91.399 (3)C43—H43A0.9700
C8—C271.512 (3)C43—H43B0.9700
C9—C101.392 (3)C44—H44A0.9700
C9—H9A0.9300C44—H44B0.9700
C31—Ru1—C3089.14 (8)H13A—C13—H13B107.2
C31—Ru1—C3290.58 (8)C19—C14—C15118.81 (17)
C30—Ru1—C32173.49 (8)C19—C14—P2116.59 (14)
C31—Ru1—P1105.43 (6)C15—C14—P2124.59 (14)
C30—Ru1—P190.73 (6)C16—C15—C14117.61 (19)
C32—Ru1—P195.61 (6)C16—C15—C28117.38 (19)
C31—Ru1—Ru3102.45 (6)C14—C15—C28125.01 (17)
C30—Ru1—Ru380.17 (6)C17—C16—C15122.5 (2)
C32—Ru1—Ru393.55 (6)C17—C16—H16A118.8
P1—Ru1—Ru3150.492 (13)C15—C16—H16A118.8
C31—Ru1—Ru2160.62 (6)C18—C17—C16120.02 (19)
C30—Ru1—Ru296.02 (5)C18—C17—H17A120.0
C32—Ru1—Ru282.20 (5)C16—C17—H17A120.0
P1—Ru1—Ru293.203 (13)C17—C18—C19118.66 (19)
Ru3—Ru1—Ru260.372 (6)C17—C18—H18A120.7
C34—Ru2—C3587.53 (8)C19—C18—H18A120.7
C34—Ru2—C3395.85 (8)C18—C19—C14122.40 (19)
C35—Ru2—C33174.03 (8)C18—C19—H19A118.8
C34—Ru2—P2102.19 (6)C14—C19—H19A118.8
C35—Ru2—P292.71 (6)C25—C20—C21119.32 (17)
C33—Ru2—P291.38 (6)C25—C20—P2119.52 (15)
C34—Ru2—Ru1165.79 (6)C21—C20—P2121.15 (14)
C35—Ru2—Ru193.48 (6)C22—C21—C20118.00 (18)
C33—Ru2—Ru182.04 (5)C22—C21—C29118.86 (18)
P2—Ru2—Ru191.930 (13)C20—C21—C29123.11 (17)
C34—Ru2—Ru3106.46 (6)C23—C22—C21122.2 (2)
C35—Ru2—Ru383.32 (6)C23—C22—H22A118.9
C33—Ru2—Ru391.00 (5)C21—C22—H22A118.9
P2—Ru2—Ru3150.848 (13)C24—C23—C22119.33 (19)
Ru1—Ru2—Ru359.680 (6)C24—C23—H23A120.3
C37—Ru3—C3891.93 (10)C22—C23—H23A120.3
C37—Ru3—C3693.62 (10)C23—C24—C25119.89 (19)
C38—Ru3—C36173.94 (9)C23—C24—H24A120.1
C37—Ru3—P398.61 (7)C25—C24—H24A120.1
C38—Ru3—P390.61 (6)C24—C25—C20121.15 (19)
C36—Ru3—P386.15 (6)C24—C25—H25A119.4
C37—Ru3—Ru190.90 (7)C20—C25—H25A119.4
C38—Ru3—Ru185.24 (6)C2—C26—H26A109.5
C36—Ru3—Ru197.10 (6)C2—C26—H26B109.5
P3—Ru3—Ru1169.752 (15)H26A—C26—H26B109.5
C37—Ru3—Ru2149.88 (7)C2—C26—H26C109.5
C38—Ru3—Ru292.86 (6)H26A—C26—H26C109.5
C36—Ru3—Ru283.55 (6)H26B—C26—H26C109.5
P3—Ru3—Ru2111.042 (14)C8—C27—H27A109.5
Ru1—Ru3—Ru259.948 (5)C8—C27—H27B109.5
C7—P1—C1105.53 (9)H27A—C27—H27B109.5
C7—P1—C13100.44 (8)C8—C27—H27C109.5
C1—P1—C13103.79 (9)H27A—C27—H27C109.5
C7—P1—Ru1118.08 (6)H27B—C27—H27C109.5
C1—P1—Ru1112.05 (6)C15—C28—H28A109.5
C13—P1—Ru1115.32 (6)C15—C28—H28B109.5
C20—P2—C14104.47 (8)H28A—C28—H28B109.5
C20—P2—C13103.56 (9)C15—C28—H28C109.5
C14—P2—C1399.99 (8)H28A—C28—H28C109.5
C20—P2—Ru2114.25 (6)H28B—C28—H28C109.5
C14—P2—Ru2117.94 (6)C21—C29—H29A109.5
C13—P2—Ru2114.67 (6)C21—C29—H29B109.5
O11—P3—O12106.47 (9)H29A—C29—H29B109.5
O11—P3—O10105.82 (9)C21—C29—H29C109.5
O12—P3—O1095.64 (9)H29A—C29—H29C109.5
O11—P3—Ru3112.45 (6)H29B—C29—H29C109.5
O12—P3—Ru3111.51 (7)O1—C30—Ru1172.48 (16)
O10—P3—Ru3122.83 (6)O2—C31—Ru1179.19 (19)
C39—O10—P3123.43 (14)O3—C32—Ru1173.73 (17)
C41—O11—P3125.37 (14)O4—C33—Ru2174.15 (16)
C43—O12—P3127.12 (16)O5—C34—Ru2176.56 (18)
C6—C1—C2118.54 (18)O6—C35—Ru2173.01 (17)
C6—C1—P1120.05 (15)O7—C36—Ru3172.27 (19)
C2—C1—P1121.25 (15)O8—C37—Ru3177.7 (2)
C3—C2—C1118.49 (18)O9—C38—Ru3172.67 (18)
C3—C2—C26117.62 (18)O10—C39—C40107.98 (18)
C1—C2—C26123.88 (18)O10—C39—H39A110.1
C4—C3—C2122.49 (19)C40—C39—H39A110.1
C4—C3—H3A118.8O10—C39—H39B110.1
C2—C3—H3A118.8C40—C39—H39B110.1
C3—C4—C5119.07 (19)H39A—C39—H39B108.4
C3—C4—H4A120.5C39—C40—Cl1109.75 (16)
C5—C4—H4A120.5C39—C40—H40A109.7
C6—C5—C4119.36 (19)Cl1—C40—H40A109.7
C6—C5—H5A120.3C39—C40—H40B109.7
C4—C5—H5A120.3Cl1—C40—H40B109.7
C5—C6—C1122.00 (19)H40A—C40—H40B108.2
C5—C6—H6A119.0O11—C41—C42107.60 (18)
C1—C6—H6A119.0O11—C41—H41A110.2
C12—C7—C8119.44 (17)C42—C41—H41A110.2
C12—C7—P1116.78 (14)O11—C41—H41B110.2
C8—C7—P1123.74 (14)C42—C41—H41B110.2
C9—C8—C7117.83 (18)H41A—C41—H41B108.5
C9—C8—C27117.79 (18)C41—C42—Cl2112.09 (17)
C7—C8—C27124.38 (18)C41—C42—H42A109.2
C10—C9—C8122.10 (19)Cl2—C42—H42A109.2
C10—C9—H9A119.0C41—C42—H42B109.2
C8—C9—H9A119.0Cl2—C42—H42B109.2
C11—C10—C9120.03 (18)H42A—C42—H42B107.9
C11—C10—H10A120.0O12—C43—C44112.3 (2)
C9—C10—H10A120.0O12—C43—H43A109.2
C10—C11—C12118.98 (18)C44—C43—H43A109.2
C10—C11—H11A120.5O12—C43—H43B109.2
C12—C11—H11A120.5C44—C43—H43B109.2
C11—C12—C7121.60 (18)H43A—C43—H43B107.9
C11—C12—H12A119.2C43—C44—Cl3111.89 (19)
C7—C12—H12A119.2C43—C44—H44A109.2
P2—C13—P1117.51 (10)Cl3—C44—H44A109.2
P2—C13—H13A107.9C43—C44—H44B109.2
P1—C13—H13A107.9Cl3—C44—H44B109.2
P2—C13—H13B107.9H44A—C44—H44B107.9
P1—C13—H13B107.9
C31—Ru1—Ru2—C3443.1 (3)C7—P1—C1—C6131.77 (16)
C30—Ru1—Ru2—C34−61.6 (3)C13—P1—C1—C626.60 (18)
C32—Ru1—Ru2—C34112.1 (3)Ru1—P1—C1—C6−98.46 (15)
P1—Ru1—Ru2—C34−152.7 (3)C7—P1—C1—C2−52.89 (18)
Ru3—Ru1—Ru2—C3413.5 (3)C13—P1—C1—C2−158.06 (16)
C31—Ru1—Ru2—C35−50.52 (19)Ru1—P1—C1—C276.88 (16)
C30—Ru1—Ru2—C35−155.25 (8)C6—C1—C2—C3−1.3 (3)
C32—Ru1—Ru2—C3518.44 (8)P1—C1—C2—C3−176.74 (15)
P1—Ru1—Ru2—C35113.67 (6)C6—C1—C2—C26178.31 (19)
Ru3—Ru1—Ru2—C35−80.18 (6)P1—C1—C2—C262.9 (3)
C31—Ru1—Ru2—C33125.52 (19)C1—C2—C3—C4−0.4 (3)
C30—Ru1—Ru2—C3320.79 (8)C26—C2—C3—C4179.9 (2)
C32—Ru1—Ru2—C33−165.52 (8)C2—C3—C4—C51.7 (3)
P1—Ru1—Ru2—C33−70.29 (6)C3—C4—C5—C6−1.2 (3)
Ru3—Ru1—Ru2—C3395.86 (6)C4—C5—C6—C1−0.6 (3)
C31—Ru1—Ru2—P2−143.36 (18)C2—C1—C6—C51.9 (3)
C30—Ru1—Ru2—P2111.91 (6)P1—C1—C6—C5177.35 (15)
C32—Ru1—Ru2—P2−74.39 (6)C1—P1—C7—C12130.80 (15)
P1—Ru1—Ru2—P220.834 (17)C13—P1—C7—C12−121.58 (15)
Ru3—Ru1—Ru2—P2−173.017 (13)Ru1—P1—C7—C124.65 (17)
C31—Ru1—Ru2—Ru329.66 (18)C1—P1—C7—C8−51.49 (18)
C30—Ru1—Ru2—Ru3−75.07 (6)C13—P1—C7—C856.13 (17)
C32—Ru1—Ru2—Ru398.62 (6)Ru1—P1—C7—C8−177.64 (13)
P1—Ru1—Ru2—Ru3−166.149 (13)C12—C7—C8—C90.4 (3)
C31—Ru1—Ru3—C3717.63 (10)P1—C7—C8—C9−177.22 (15)
C30—Ru1—Ru3—C37−69.28 (9)C12—C7—C8—C27179.29 (19)
C32—Ru1—Ru3—C37109.01 (9)P1—C7—C8—C271.6 (3)
P1—Ru1—Ru3—C37−143.02 (8)C7—C8—C9—C100.9 (3)
Ru2—Ru1—Ru3—C37−172.05 (7)C27—C8—C9—C10−178.0 (2)
C31—Ru1—Ru3—C38−74.23 (9)C8—C9—C10—C11−1.4 (3)
C30—Ru1—Ru3—C38−161.14 (8)C9—C10—C11—C120.5 (3)
C32—Ru1—Ru3—C3817.15 (8)C10—C11—C12—C70.8 (3)
P1—Ru1—Ru3—C38125.12 (7)C8—C7—C12—C11−1.3 (3)
Ru2—Ru1—Ru3—C3896.09 (6)P1—C7—C12—C11176.55 (15)
C31—Ru1—Ru3—C36111.39 (9)C20—P2—C13—P1−103.00 (12)
C30—Ru1—Ru3—C3624.48 (8)C14—P2—C13—P1149.33 (11)
C32—Ru1—Ru3—C36−157.23 (8)Ru2—P2—C13—P122.14 (13)
P1—Ru1—Ru3—C36−49.26 (7)C7—P1—C13—P2126.57 (11)
Ru2—Ru1—Ru3—C36−78.29 (6)C1—P1—C13—P2−124.43 (11)
C31—Ru1—Ru3—P3−140.61 (10)Ru1—P1—C13—P2−1.50 (13)
C30—Ru1—Ru3—P3132.49 (10)C20—P2—C14—C19135.20 (16)
C32—Ru1—Ru3—P3−49.23 (10)C13—P2—C14—C19−117.87 (16)
P1—Ru1—Ru3—P358.74 (9)Ru2—P2—C14—C197.10 (18)
Ru2—Ru1—Ru3—P329.71 (8)C20—P2—C14—C15−43.81 (19)
C31—Ru1—Ru3—Ru2−170.32 (6)C13—P2—C14—C1563.13 (18)
C30—Ru1—Ru3—Ru2102.77 (5)Ru2—P2—C14—C15−171.90 (14)
C32—Ru1—Ru3—Ru2−78.94 (5)C19—C14—C15—C16−0.9 (3)
P1—Ru1—Ru3—Ru229.03 (3)P2—C14—C15—C16178.10 (16)
C34—Ru2—Ru3—C37−160.58 (15)C19—C14—C15—C28179.6 (2)
C35—Ru2—Ru3—C37114.00 (15)P2—C14—C15—C28−1.4 (3)
C33—Ru2—Ru3—C37−64.18 (15)C14—C15—C16—C17−0.2 (3)
P2—Ru2—Ru3—C3730.44 (15)C28—C15—C16—C17179.3 (2)
Ru1—Ru2—Ru3—C3716.00 (14)C15—C16—C17—C180.8 (4)
C34—Ru2—Ru3—C38100.60 (9)C16—C17—C18—C19−0.2 (3)
C35—Ru2—Ru3—C3815.18 (9)C17—C18—C19—C14−0.9 (3)
C33—Ru2—Ru3—C38−163.00 (8)C15—C14—C19—C181.5 (3)
P2—Ru2—Ru3—C38−68.38 (7)P2—C14—C19—C18−177.58 (17)
Ru1—Ru2—Ru3—C38−82.82 (7)C14—P2—C20—C25128.42 (16)
C34—Ru2—Ru3—C36−74.50 (9)C13—P2—C20—C2524.15 (17)
C35—Ru2—Ru3—C36−159.92 (8)Ru2—P2—C20—C25−101.27 (15)
C33—Ru2—Ru3—C3621.90 (9)C14—P2—C20—C21−52.72 (17)
P2—Ru2—Ru3—C36116.52 (7)C13—P2—C20—C21−157.00 (15)
Ru1—Ru2—Ru3—C36102.08 (6)Ru2—P2—C20—C2177.59 (16)
C34—Ru2—Ru3—P38.85 (7)C25—C20—C21—C22−3.8 (3)
C35—Ru2—Ru3—P3−76.57 (6)P2—C20—C21—C22177.39 (15)
C33—Ru2—Ru3—P3105.24 (6)C25—C20—C21—C29177.93 (18)
P2—Ru2—Ru3—P3−160.13 (3)P2—C20—C21—C29−0.9 (3)
Ru1—Ru2—Ru3—P3−174.578 (16)C20—C21—C22—C231.4 (3)
C34—Ru2—Ru3—Ru1−176.58 (6)C29—C21—C22—C23179.8 (2)
C35—Ru2—Ru3—Ru198.00 (6)C21—C22—C23—C241.3 (3)
C33—Ru2—Ru3—Ru1−80.18 (6)C22—C23—C24—C25−1.5 (3)
P2—Ru2—Ru3—Ru114.44 (3)C23—C24—C25—C20−0.9 (3)
C31—Ru1—P1—C741.43 (9)C21—C20—C25—C243.6 (3)
C30—Ru1—P1—C7130.74 (9)P2—C20—C25—C24−177.51 (16)
C32—Ru1—P1—C7−50.72 (9)C31—Ru1—C30—O126.9 (13)
Ru3—Ru1—P1—C7−158.18 (7)C32—Ru1—C30—O1114.4 (14)
Ru2—Ru1—P1—C7−133.19 (7)P1—Ru1—C30—O1−78.5 (13)
C31—Ru1—P1—C1−81.49 (9)Ru3—Ru1—C30—O1129.7 (13)
C30—Ru1—P1—C17.82 (9)Ru2—Ru1—C30—O1−171.8 (13)
C32—Ru1—P1—C1−173.65 (9)C30—Ru1—C31—O2144 (15)
Ru3—Ru1—P1—C178.90 (7)C32—Ru1—C31—O2−29 (15)
Ru2—Ru1—P1—C1103.89 (7)P1—Ru1—C31—O2−125 (15)
C31—Ru1—P1—C13160.09 (9)Ru3—Ru1—C31—O265 (15)
C30—Ru1—P1—C13−110.61 (9)Ru2—Ru1—C31—O239 (15)
C32—Ru1—P1—C1367.93 (9)C31—Ru1—C32—O3−22.0 (16)
Ru3—Ru1—P1—C13−39.52 (8)C30—Ru1—C32—O3−109.4 (16)
Ru2—Ru1—P1—C13−14.53 (7)P1—Ru1—C32—O383.6 (16)
C34—Ru2—P2—C20−88.92 (9)Ru3—Ru1—C32—O3−124.5 (16)
C35—Ru2—P2—C20−0.86 (9)Ru2—Ru1—C32—O3176.1 (16)
C33—Ru2—P2—C20174.80 (9)C34—Ru2—C33—O4−46.4 (17)
Ru1—Ru2—P2—C2092.72 (7)C35—Ru2—C33—O4−170.7 (13)
Ru3—Ru2—P2—C2080.27 (7)P2—Ru2—C33—O456.0 (17)
C34—Ru2—P2—C1434.39 (9)Ru1—Ru2—C33—O4147.8 (17)
C35—Ru2—P2—C14122.45 (9)Ru3—Ru2—C33—O4−153.1 (17)
C33—Ru2—P2—C14−61.90 (9)C35—Ru2—C34—O5−44 (3)
Ru1—Ru2—P2—C14−143.98 (7)C33—Ru2—C34—O5141 (3)
Ru3—Ru2—P2—C14−156.42 (7)P2—Ru2—C34—O548 (3)
C34—Ru2—P2—C13151.76 (9)Ru1—Ru2—C34—O5−138 (3)
C35—Ru2—P2—C13−120.18 (9)Ru3—Ru2—C34—O5−126 (3)
C33—Ru2—P2—C1355.47 (9)C34—Ru2—C35—O639.2 (15)
Ru1—Ru2—P2—C13−26.61 (7)C33—Ru2—C35—O6163.9 (12)
Ru3—Ru2—P2—C13−39.05 (8)P2—Ru2—C35—O6−62.9 (15)
C37—Ru3—P3—O11−117.02 (10)Ru1—Ru2—C35—O6−155.0 (15)
C38—Ru3—P3—O11−24.98 (10)Ru3—Ru2—C35—O6146.1 (15)
C36—Ru3—P3—O11149.90 (10)C37—Ru3—C36—O7−73.4 (15)
Ru1—Ru3—P3—O1140.96 (12)C38—Ru3—C36—O782.8 (18)
Ru2—Ru3—P3—O1168.33 (7)P3—Ru3—C36—O725.0 (15)
C37—Ru3—P3—O122.49 (10)Ru1—Ru3—C36—O7−164.8 (15)
C38—Ru3—P3—O1294.54 (9)Ru2—Ru3—C36—O7136.7 (15)
C36—Ru3—P3—O12−90.59 (9)C38—Ru3—C37—O8104 (6)
Ru1—Ru3—P3—O12160.47 (9)C36—Ru3—C37—O8−78 (6)
Ru2—Ru3—P3—O12−172.16 (7)P3—Ru3—C37—O8−165 (6)
C37—Ru3—P3—O10114.83 (10)Ru1—Ru3—C37—O819 (6)
C38—Ru3—P3—O10−153.13 (10)Ru2—Ru3—C37—O85 (6)
C36—Ru3—P3—O1021.74 (10)C37—Ru3—C38—O948.1 (16)
Ru1—Ru3—P3—O10−87.20 (11)C36—Ru3—C38—O9−108.2 (17)
Ru2—Ru3—P3—O10−59.83 (8)P3—Ru3—C38—O9−50.5 (16)
O11—P3—O10—C39−63.21 (19)Ru1—Ru3—C38—O9138.8 (16)
O12—P3—O10—C39−172.12 (18)Ru2—Ru3—C38—O9−161.6 (16)
Ru3—P3—O10—C3967.74 (18)P3—O10—C39—C40170.33 (15)
O12—P3—O11—C4152.09 (19)O10—C39—C40—Cl1−60.7 (2)
O10—P3—O11—C41−48.89 (19)P3—O11—C41—C42169.99 (16)
Ru3—P3—O11—C41174.49 (15)O11—C41—C42—Cl2−70.8 (2)
O11—P3—O12—C43−82.9 (2)P3—O12—C43—C44−87.7 (3)
O10—P3—O12—C4325.5 (2)O12—C43—C44—Cl3−56.7 (3)
Ru3—P3—O12—C43154.15 (18)
D—H···AD—HH···AD···AD—H···A
C11—H11A···O1i0.932.573.204 (3)126
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
C11—H11A⋯O1i0.932.573.204 (3)126

Symmetry code: (i) .

  4 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  [μ-Bis(diphenyl-arsino)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-[triphenyl-stibine-3κSb]-triangulo-triruthenium(0).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-12-24

3.  [μ-Bis(di-o-tolyl-phosphan-yl)methane-1:2κP:P']deca-carbonyl-1κC,2κC,3κC-triangulo-triruthenium(0)-methanol (8/1).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; H A Hafiz Malik; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-15

4.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  4 in total

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