Literature DB >> 21578647

μ-Bis(diphenyl-arsino)methane-1:2κAs:As-nona-carbonyl-1κC,2κC,3κC-[(2-methoxy-phen-yl)diphenyl-phosphino-3κP]-triangulo-triruthenium(0).

Omar Bin Shawkataly, Imthyaz Ahmed Khan, Chin Sing Yeap, Hoong-Kun Fun.   

Abstract

In the title triangulo-triruthenium compound, [Ru(3)(C(25)H(22)As(2))(C(19)H(17)OP)(CO)(9)], the bis-(diphenyl-arsino)methane ligand bridges a Ru-Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru(3) triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phosphine substituted phenyl rings make dihedral angles of 74.34 (12), 68.34 (12) and 85.45 (11)° with each other. The dihedral angles between the two phenyl rings are 87.56 (11) and 60.56 (11)° for the two diphenyl-arsino groups. In the crystal packing, the mol-ecules are linked together into chains via inter-molecular C-H⋯O hydrogen bonds down the a axis. Weak inter-molecular C-H⋯π inter-actions further stabilize the crystal structure.

Entities:  

Year:  2009        PMID: 21578647      PMCID: PMC2972135          DOI: 10.1107/S1600536809047783

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


Related literature

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985 ▶, 1988a ▶,b ▶); Shawkataly et al. (1998 ▶, 2004 ▶, 2009a ▶,b ▶). For related structures, see: Shawkataly et al. (2009a ▶,b ▶). For the synthesis of bis­(diphenylarsino)methane, see: Bruce et al. (1983 ▶). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986 ▶).

Experimental

Crystal data

[Ru3(C25H22As2)(C19H17OP)(CO)9] M = 1319.86 Triclinic, a = 10.4414 (1) Å b = 11.6541 (1) Å c = 21.7581 (3) Å α = 84.220 (1)° β = 84.910 (1)° γ = 69.324 (1)° V = 2460.49 (5) Å3 Z = 2 Mo Kα radiation μ = 2.34 mm−1 T = 100 K 0.22 × 0.15 × 0.08 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer Absorption correction: multi-scan (; Bruker, 2005 ▶) T min = 0.624, T max = 0.830 66801 measured reflections 14256 independent reflections 11583 reflections with I > 2σ(I) R int = 0.042

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 0.059 S = 1.02 14256 reflections 623 parameters H-atom parameters constrained Δρmax = 0.67 e Å−3 Δρmin = −0.80 e Å−3 Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); 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 datablocks global, I. DOI: 10.1107/S1600536809047783/sj2676sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809047783/sj2676Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ru3(C25H22As2)(C19H17OP)(CO)9]Z = 2
Mr = 1319.86F(000) = 1300
Triclinic, P1Dx = 1.782 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.4414 (1) ÅCell parameters from 9969 reflections
b = 11.6541 (1) Åθ = 2.3–32.5°
c = 21.7581 (3) ŵ = 2.34 mm1
α = 84.220 (1)°T = 100 K
β = 84.910 (1)°Block, purple
γ = 69.324 (1)°0.22 × 0.15 × 0.08 mm
V = 2460.49 (5) Å3
Bruker SMART APEXII CCD area-detector diffractometer14256 independent reflections
Radiation source: fine-focus sealed tube11583 reflections with I > 2σ(I)
graphiteRint = 0.042
φ and ω scansθmax = 30.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −14→14
Tmin = 0.624, Tmax = 0.830k = −16→16
66801 measured reflectionsl = −30→30
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.0249P)2 + 1.1204P] where P = (Fo2 + 2Fc2)/3
14256 reflections(Δ/σ)max = 0.001
623 parametersΔρmax = 0.67 e Å3
0 restraintsΔρmin = −0.80 e Å3
Experimental. The crystal was placed in the cold stream of an Oxford Cyrosystems Cobra open-flow nitrogen cryostat (Cosier & Glazer, 1986) operating at 100.0 (1) K.
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.
xyzUiso*/Ueq
Ru10.304381 (17)0.169488 (15)0.205414 (8)0.01208 (4)
Ru20.134145 (17)0.409411 (15)0.239146 (8)0.01210 (4)
Ru30.366826 (17)0.266015 (15)0.309439 (8)0.01236 (4)
As10.14602 (2)0.160785 (19)0.131363 (10)0.01190 (5)
As20.03462 (2)0.457750 (19)0.139265 (10)0.01170 (5)
P10.42521 (6)0.35723 (5)0.38908 (3)0.01382 (11)
O10.17427 (18)0.03586 (15)0.30752 (7)0.0228 (4)
O20.55893 (18)−0.06037 (15)0.20185 (8)0.0273 (4)
O30.45546 (17)0.30219 (15)0.11329 (8)0.0234 (4)
O40.33593 (17)0.53968 (15)0.19120 (8)0.0236 (4)
O5−0.0492 (2)0.64365 (15)0.29555 (8)0.0298 (4)
O6−0.07509 (17)0.28542 (16)0.28668 (8)0.0242 (4)
O70.11632 (17)0.25538 (16)0.39212 (7)0.0223 (4)
O80.53996 (19)0.00676 (15)0.35308 (8)0.0291 (4)
O90.59248 (17)0.33052 (15)0.22840 (8)0.0228 (4)
O100.35430 (18)0.17638 (16)0.47263 (8)0.0246 (4)
C10.2071 (2)0.07700 (19)0.05505 (10)0.0134 (4)
C20.3397 (2)−0.0067 (2)0.04739 (10)0.0164 (4)
H2A0.4021−0.01860.07750.020*
C30.3793 (2)−0.0725 (2)−0.00503 (10)0.0182 (4)
H3A0.4676−0.1293−0.00970.022*
C40.2873 (2)−0.0534 (2)−0.05045 (10)0.0182 (5)
H4A0.3145−0.0966−0.08580.022*
C50.1552 (2)0.0296 (2)−0.04332 (10)0.0180 (4)
H5A0.09380.0426−0.07390.022*
C60.1146 (2)0.0933 (2)0.00947 (10)0.0167 (4)
H6A0.02500.14730.01470.020*
C70.0285 (2)0.0696 (2)0.16641 (10)0.0149 (4)
C80.0956 (2)−0.0566 (2)0.18016 (10)0.0175 (4)
H8A0.1891−0.09180.17030.021*
C90.0238 (2)−0.1294 (2)0.20841 (10)0.0201 (5)
H9A0.0692−0.21300.21750.024*
C10−0.1162 (3)−0.0774 (2)0.22309 (11)0.0224 (5)
H10A−0.1649−0.12610.24170.027*
C11−0.1828 (3)0.0478 (2)0.20972 (11)0.0225 (5)
H11A−0.27630.08280.21950.027*
C12−0.1106 (2)0.1215 (2)0.18172 (10)0.0183 (4)
H12A−0.15580.20530.17330.022*
C130.0169 (2)0.32006 (19)0.09980 (10)0.0145 (4)
H13A0.03410.33100.05540.017*
H13B−0.07610.32020.10740.017*
C14−0.1539 (2)0.56912 (19)0.13745 (10)0.0142 (4)
C15−0.2506 (2)0.5387 (2)0.17774 (11)0.0192 (5)
H15A−0.22220.46970.20550.023*
C16−0.3882 (2)0.6101 (2)0.17687 (11)0.0212 (5)
H16A−0.45210.58890.20370.025*
C17−0.4304 (2)0.7133 (2)0.13582 (12)0.0223 (5)
H17A−0.52310.76040.13430.027*
C18−0.3347 (2)0.7466 (2)0.09695 (11)0.0222 (5)
H18A−0.36320.81740.07030.027*
C19−0.1965 (2)0.6748 (2)0.09750 (10)0.0172 (4)
H19A−0.13270.69740.07130.021*
C200.1329 (2)0.5313 (2)0.07702 (10)0.0144 (4)
C210.1333 (2)0.6484 (2)0.08547 (10)0.0165 (4)
H21A0.07940.69220.11760.020*
C220.2144 (2)0.6995 (2)0.04593 (11)0.0205 (5)
H22A0.21380.77780.05140.025*
C230.2957 (2)0.6342 (2)−0.00136 (11)0.0230 (5)
H23A0.35020.6685−0.02760.028*
C240.2965 (2)0.5178 (2)−0.00993 (11)0.0226 (5)
H24A0.35130.4740−0.04190.027*
C250.2148 (2)0.4663 (2)0.02946 (10)0.0180 (4)
H25A0.21540.38800.02370.022*
C260.3085 (2)0.3882 (2)0.45772 (10)0.0171 (4)
C270.2424 (2)0.5067 (2)0.47683 (11)0.0225 (5)
H27A0.26190.57220.45530.027*
C280.1483 (3)0.5289 (3)0.52739 (12)0.0303 (6)
H28A0.10520.60840.53960.036*
C290.1194 (3)0.4319 (3)0.55912 (12)0.0336 (7)
H29A0.05490.44670.59240.040*
C300.1848 (3)0.3124 (3)0.54234 (11)0.0307 (6)
H30A0.16490.24760.56450.037*
C310.2803 (3)0.2903 (2)0.49224 (11)0.0225 (5)
C320.5915 (2)0.2698 (2)0.42165 (10)0.0165 (4)
C330.6086 (3)0.2668 (2)0.48475 (11)0.0215 (5)
H33A0.53450.30670.51110.026*
C340.7365 (3)0.2039 (2)0.50829 (12)0.0262 (5)
H34A0.74700.20060.55050.031*
C350.8479 (3)0.1465 (2)0.46937 (12)0.0263 (5)
H35A0.93350.10620.48530.032*
C360.8325 (2)0.1487 (2)0.40697 (12)0.0251 (5)
H36A0.90740.10970.38080.030*
C370.7044 (2)0.2096 (2)0.38307 (11)0.0205 (5)
H37A0.69400.21010.34100.025*
C380.4412 (2)0.5069 (2)0.36453 (10)0.0156 (4)
C390.5592 (2)0.5330 (2)0.37148 (11)0.0206 (5)
H39A0.63410.47310.38940.025*
C400.5655 (3)0.6487 (2)0.35168 (11)0.0261 (5)
H40A0.64500.66510.35600.031*
C410.4541 (3)0.7389 (2)0.32574 (11)0.0277 (6)
H41A0.45840.81620.31310.033*
C420.3359 (3)0.7140 (2)0.31854 (11)0.0256 (5)
H42A0.26060.77460.30130.031*
C430.3305 (3)0.5985 (2)0.33716 (11)0.0204 (5)
H43A0.25190.58170.33140.024*
C440.2190 (2)0.0905 (2)0.27097 (10)0.0168 (4)
C450.4604 (2)0.0246 (2)0.20180 (10)0.0182 (5)
C460.3947 (2)0.2583 (2)0.14876 (10)0.0167 (4)
C470.2710 (2)0.4822 (2)0.21067 (10)0.0173 (4)
C480.0229 (2)0.5545 (2)0.27574 (10)0.0182 (5)
C490.0088 (2)0.3253 (2)0.26981 (10)0.0170 (4)
C500.2029 (2)0.2631 (2)0.35747 (10)0.0175 (4)
C510.4774 (2)0.1058 (2)0.33704 (10)0.0178 (4)
C520.5059 (2)0.3065 (2)0.25589 (10)0.0173 (4)
C530.3141 (3)0.0748 (3)0.49814 (14)0.0371 (7)
H53A0.36830.00210.47800.056*
H53B0.21890.09290.49180.056*
H53C0.32830.06140.54170.056*
U11U22U33U12U13U23
Ru10.01299 (8)0.01047 (8)0.01293 (8)−0.00370 (6)−0.00310 (6)−0.00082 (6)
Ru20.01320 (8)0.01058 (8)0.01226 (8)−0.00360 (6)−0.00261 (6)−0.00003 (6)
Ru30.01372 (8)0.01118 (8)0.01253 (8)−0.00423 (6)−0.00349 (6)−0.00038 (6)
As10.01311 (10)0.01034 (10)0.01269 (10)−0.00425 (8)−0.00292 (8)−0.00022 (8)
As20.01245 (10)0.01009 (10)0.01241 (10)−0.00383 (8)−0.00205 (8)0.00073 (8)
P10.0157 (3)0.0133 (3)0.0136 (3)−0.0060 (2)−0.0029 (2)−0.0005 (2)
O10.0313 (10)0.0192 (8)0.0195 (8)−0.0113 (7)−0.0010 (7)0.0004 (7)
O20.0214 (9)0.0183 (9)0.0372 (10)0.0009 (7)−0.0057 (8)−0.0051 (8)
O30.0232 (9)0.0246 (9)0.0219 (9)−0.0087 (7)0.0018 (7)−0.0004 (7)
O40.0202 (9)0.0234 (9)0.0297 (9)−0.0109 (7)−0.0069 (7)0.0044 (7)
O50.0387 (11)0.0162 (9)0.0269 (10)−0.0024 (8)0.0089 (8)−0.0027 (7)
O60.0216 (9)0.0260 (9)0.0261 (9)−0.0115 (7)−0.0050 (7)0.0080 (7)
O70.0203 (9)0.0317 (9)0.0161 (8)−0.0104 (7)−0.0009 (7)−0.0025 (7)
O80.0355 (11)0.0154 (8)0.0341 (10)−0.0043 (8)−0.0139 (8)0.0024 (8)
O90.0191 (8)0.0248 (9)0.0234 (9)−0.0079 (7)−0.0009 (7)0.0033 (7)
O100.0321 (10)0.0238 (9)0.0223 (9)−0.0165 (8)−0.0063 (7)0.0067 (7)
C10.0175 (10)0.0102 (9)0.0135 (10)−0.0064 (8)0.0001 (8)0.0000 (8)
C20.0170 (11)0.0157 (10)0.0170 (11)−0.0062 (9)−0.0036 (8)0.0009 (9)
C30.0165 (11)0.0152 (10)0.0212 (11)−0.0036 (9)0.0000 (9)−0.0024 (9)
C40.0246 (12)0.0168 (11)0.0158 (11)−0.0103 (9)0.0003 (9)−0.0024 (9)
C50.0209 (11)0.0181 (11)0.0159 (11)−0.0074 (9)−0.0067 (9)0.0016 (9)
C60.0157 (11)0.0137 (10)0.0202 (11)−0.0044 (8)−0.0038 (9)0.0002 (9)
C70.0201 (11)0.0152 (10)0.0121 (10)−0.0090 (9)−0.0014 (8)−0.0016 (8)
C80.0181 (11)0.0162 (11)0.0193 (11)−0.0069 (9)−0.0039 (9)−0.0005 (9)
C90.0282 (13)0.0149 (11)0.0190 (11)−0.0096 (10)−0.0054 (9)0.0020 (9)
C100.0267 (13)0.0216 (12)0.0232 (12)−0.0146 (10)0.0000 (10)0.0010 (10)
C110.0195 (12)0.0229 (12)0.0256 (12)−0.0090 (10)0.0031 (10)−0.0020 (10)
C120.0181 (11)0.0147 (10)0.0211 (11)−0.0045 (9)−0.0020 (9)−0.0008 (9)
C130.0153 (10)0.0115 (10)0.0163 (10)−0.0036 (8)−0.0047 (8)0.0001 (8)
C140.0141 (10)0.0132 (10)0.0150 (10)−0.0036 (8)−0.0034 (8)−0.0011 (8)
C150.0172 (11)0.0186 (11)0.0207 (11)−0.0059 (9)−0.0034 (9)0.0037 (9)
C160.0191 (11)0.0235 (12)0.0234 (12)−0.0103 (10)0.0009 (9)−0.0035 (10)
C170.0133 (11)0.0198 (11)0.0317 (13)−0.0020 (9)−0.0035 (10)−0.0049 (10)
C180.0234 (12)0.0156 (11)0.0255 (12)−0.0034 (9)−0.0065 (10)0.0004 (10)
C190.0182 (11)0.0134 (10)0.0203 (11)−0.0060 (9)−0.0024 (9)0.0012 (9)
C200.0139 (10)0.0157 (10)0.0146 (10)−0.0068 (8)−0.0032 (8)0.0034 (8)
C210.0170 (11)0.0167 (10)0.0162 (10)−0.0064 (9)−0.0020 (8)0.0002 (9)
C220.0222 (12)0.0167 (11)0.0243 (12)−0.0094 (9)−0.0043 (10)0.0031 (9)
C230.0200 (12)0.0275 (13)0.0219 (12)−0.0110 (10)−0.0015 (9)0.0070 (10)
C240.0201 (12)0.0288 (13)0.0164 (11)−0.0065 (10)0.0022 (9)−0.0010 (10)
C250.0196 (11)0.0173 (11)0.0179 (11)−0.0073 (9)−0.0013 (9)−0.0017 (9)
C260.0173 (11)0.0231 (11)0.0135 (10)−0.0096 (9)−0.0032 (8)−0.0018 (9)
C270.0192 (12)0.0291 (13)0.0200 (12)−0.0080 (10)−0.0036 (9)−0.0050 (10)
C280.0237 (13)0.0435 (16)0.0221 (13)−0.0072 (12)−0.0014 (10)−0.0108 (12)
C290.0232 (14)0.062 (2)0.0147 (12)−0.0135 (14)0.0026 (10)−0.0069 (13)
C300.0311 (14)0.0494 (17)0.0165 (12)−0.0219 (13)−0.0034 (10)0.0071 (12)
C310.0243 (12)0.0323 (13)0.0163 (11)−0.0162 (11)−0.0074 (9)0.0024 (10)
C320.0185 (11)0.0134 (10)0.0200 (11)−0.0082 (9)−0.0072 (9)0.0033 (9)
C330.0269 (13)0.0172 (11)0.0208 (12)−0.0069 (10)−0.0077 (10)−0.0007 (9)
C340.0332 (14)0.0222 (12)0.0253 (13)−0.0102 (11)−0.0140 (11)0.0022 (10)
C350.0241 (13)0.0208 (12)0.0338 (14)−0.0077 (10)−0.0142 (11)0.0090 (11)
C360.0176 (12)0.0218 (12)0.0341 (14)−0.0061 (10)−0.0024 (10)0.0043 (11)
C370.0201 (12)0.0241 (12)0.0189 (11)−0.0102 (10)−0.0035 (9)0.0035 (10)
C380.0222 (11)0.0146 (10)0.0121 (10)−0.0083 (9)−0.0019 (8)−0.0028 (8)
C390.0228 (12)0.0210 (12)0.0206 (11)−0.0106 (10)−0.0049 (9)0.0015 (9)
C400.0311 (14)0.0282 (13)0.0261 (13)−0.0191 (11)−0.0056 (11)0.0014 (11)
C410.0477 (17)0.0179 (12)0.0223 (12)−0.0176 (12)−0.0048 (11)0.0022 (10)
C420.0351 (15)0.0170 (11)0.0233 (12)−0.0059 (11)−0.0108 (11)0.0012 (10)
C430.0249 (12)0.0164 (11)0.0209 (12)−0.0073 (9)−0.0064 (9)−0.0015 (9)
C440.0199 (11)0.0132 (10)0.0165 (11)−0.0039 (9)−0.0042 (9)−0.0022 (9)
C450.0213 (12)0.0183 (11)0.0182 (11)−0.0098 (9)−0.0027 (9)−0.0037 (9)
C460.0175 (11)0.0140 (10)0.0171 (11)−0.0028 (9)−0.0029 (9)−0.0033 (9)
C470.0161 (11)0.0170 (11)0.0182 (11)−0.0038 (9)−0.0043 (9)−0.0031 (9)
C480.0221 (12)0.0171 (11)0.0161 (11)−0.0088 (9)0.0003 (9)0.0021 (9)
C490.0193 (11)0.0155 (10)0.0138 (10)−0.0026 (9)−0.0064 (9)0.0022 (9)
C500.0188 (11)0.0169 (11)0.0169 (11)−0.0044 (9)−0.0060 (9)−0.0044 (9)
C510.0221 (12)0.0178 (11)0.0158 (11)−0.0089 (9)−0.0049 (9)−0.0011 (9)
C520.0209 (11)0.0141 (10)0.0159 (11)−0.0041 (9)−0.0058 (9)0.0002 (9)
C530.0394 (16)0.0335 (15)0.0441 (17)−0.0230 (14)−0.0149 (13)0.0211 (13)
Ru1—C451.890 (2)C13—H13B0.9700
Ru1—C461.925 (2)C14—C191.392 (3)
Ru1—C441.941 (2)C14—C151.395 (3)
Ru1—As12.4423 (3)C15—C161.384 (3)
Ru1—Ru32.8471 (2)C15—H15A0.9300
Ru1—Ru22.8616 (2)C16—C171.385 (3)
Ru2—C481.887 (2)C16—H16A0.9300
Ru2—C471.933 (2)C17—C181.386 (3)
Ru2—C491.934 (2)C17—H17A0.9300
Ru2—As22.4209 (3)C18—C191.389 (3)
Ru2—Ru32.8830 (2)C18—H18A0.9300
Ru3—C511.885 (2)C19—H19A0.9300
Ru3—C501.933 (2)C20—C251.386 (3)
Ru3—C521.939 (2)C20—C211.397 (3)
Ru3—P12.3495 (6)C21—C221.391 (3)
As1—C71.952 (2)C21—H21A0.9300
As1—C11.953 (2)C22—C231.380 (3)
As1—C131.968 (2)C22—H22A0.9300
As2—C141.939 (2)C23—C241.385 (3)
As2—C201.940 (2)C23—H23A0.9300
As2—C131.965 (2)C24—C251.396 (3)
P1—C261.822 (2)C24—H24A0.9300
P1—C381.833 (2)C25—H25A0.9300
P1—C321.838 (2)C26—C271.396 (3)
O1—C441.139 (3)C26—C311.407 (3)
O2—C451.148 (3)C27—C281.389 (3)
O3—C461.150 (3)C27—H27A0.9300
O4—C471.141 (3)C28—C291.375 (4)
O5—C481.145 (3)C28—H28A0.9300
O6—C491.146 (3)C29—C301.388 (4)
O7—C501.148 (3)C29—H29A0.9300
O8—C511.144 (3)C30—C311.389 (4)
O9—C521.142 (3)C30—H30A0.9300
O10—C311.368 (3)C32—C371.395 (3)
O10—C531.436 (3)C32—C331.395 (3)
C1—C21.391 (3)C33—C341.392 (3)
C1—C61.399 (3)C33—H33A0.9300
C2—C31.389 (3)C34—C351.381 (4)
C2—H2A0.9300C34—H34A0.9300
C3—C41.387 (3)C35—C361.378 (4)
C3—H3A0.9300C35—H35A0.9300
C4—C51.383 (3)C36—C371.394 (3)
C4—H4A0.9300C36—H36A0.9300
C5—C61.383 (3)C37—H37A0.9300
C5—H5A0.9300C38—C391.393 (3)
C6—H6A0.9300C38—C431.398 (3)
C7—C121.386 (3)C39—C401.395 (3)
C7—C81.401 (3)C39—H39A0.9300
C8—C91.387 (3)C40—C411.382 (4)
C8—H8A0.9300C40—H40A0.9300
C9—C101.391 (3)C41—C421.389 (4)
C9—H9A0.9300C41—H41A0.9300
C10—C111.389 (3)C42—C431.385 (3)
C10—H10A0.9300C42—H42A0.9300
C11—C121.395 (3)C43—H43A0.9300
C11—H11A0.9300C53—H53A0.9600
C12—H12A0.9300C53—H53B0.9600
C13—H13A0.9700C53—H53C0.9600
C45—Ru1—C4691.04 (9)C19—C14—C15119.3 (2)
C45—Ru1—C4490.46 (9)C19—C14—As2123.36 (16)
C46—Ru1—C44172.53 (9)C15—C14—As2117.35 (16)
C45—Ru1—As1107.84 (7)C16—C15—C14120.7 (2)
C46—Ru1—As195.19 (6)C16—C15—H15A119.6
C44—Ru1—As191.31 (6)C14—C15—H15A119.6
C45—Ru1—Ru398.86 (7)C15—C16—C17119.7 (2)
C46—Ru1—Ru391.92 (6)C15—C16—H16A120.2
C44—Ru1—Ru380.62 (6)C17—C16—H16A120.2
As1—Ru1—Ru3152.186 (9)C16—C17—C18120.1 (2)
C45—Ru1—Ru2158.58 (6)C16—C17—H17A120.0
C46—Ru1—Ru283.95 (7)C18—C17—H17A120.0
C44—Ru1—Ru292.01 (7)C17—C18—C19120.4 (2)
As1—Ru1—Ru293.368 (8)C17—C18—H18A119.8
Ru3—Ru1—Ru260.666 (6)C19—C18—H18A119.8
C48—Ru2—C4791.34 (9)C18—C19—C14119.8 (2)
C48—Ru2—C4991.77 (9)C18—C19—H19A120.1
C47—Ru2—C49175.54 (9)C14—C19—H19A120.1
C48—Ru2—As297.50 (7)C25—C20—C21119.46 (19)
C47—Ru2—As291.55 (6)C25—C20—As2122.17 (16)
C49—Ru2—As291.22 (6)C21—C20—As2117.89 (16)
C48—Ru2—Ru1169.88 (7)C22—C21—C20120.1 (2)
C47—Ru2—Ru193.48 (7)C22—C21—H21A120.0
C49—Ru2—Ru182.96 (7)C20—C21—H21A120.0
As2—Ru2—Ru191.262 (8)C23—C22—C21120.2 (2)
C48—Ru2—Ru3113.31 (7)C23—C22—H22A119.9
C47—Ru2—Ru376.67 (6)C21—C22—H22A119.9
C49—Ru2—Ru399.15 (6)C22—C23—C24120.2 (2)
As2—Ru2—Ru3146.953 (10)C22—C23—H23A119.9
Ru1—Ru2—Ru359.420 (6)C24—C23—H23A119.9
C51—Ru3—C5095.57 (10)C23—C24—C25119.9 (2)
C51—Ru3—C5297.26 (10)C23—C24—H24A120.1
C50—Ru3—C52167.15 (9)C25—C24—H24A120.1
C51—Ru3—P193.36 (7)C20—C25—C24120.2 (2)
C50—Ru3—P190.24 (6)C20—C25—H25A119.9
C52—Ru3—P188.34 (7)C24—C25—H25A119.9
C51—Ru3—Ru189.47 (7)C27—C26—C31118.2 (2)
C50—Ru3—Ru193.66 (6)C27—C26—P1122.46 (17)
C52—Ru3—Ru187.15 (6)C31—C26—P1119.37 (18)
P1—Ru3—Ru1174.946 (15)C28—C27—C26121.4 (2)
C51—Ru3—Ru2145.12 (6)C28—C27—H27A119.3
C50—Ru3—Ru272.13 (6)C26—C27—H27A119.3
C52—Ru3—Ru297.40 (6)C29—C28—C27119.2 (3)
P1—Ru3—Ru2118.530 (16)C29—C28—H28A120.4
Ru1—Ru3—Ru259.915 (6)C27—C28—H28A120.4
C7—As1—C197.55 (9)C28—C29—C30121.2 (2)
C7—As1—C13104.20 (9)C28—C29—H29A119.4
C1—As1—C13100.98 (9)C30—C29—H29A119.4
C7—As1—Ru1112.20 (6)C29—C30—C31119.5 (2)
C1—As1—Ru1122.94 (6)C29—C30—H30A120.3
C13—As1—Ru1116.04 (6)C31—C30—H30A120.3
C14—As2—C20104.26 (9)O10—C31—C30124.8 (2)
C14—As2—C1399.21 (9)O10—C31—C26114.7 (2)
C20—As2—C13104.44 (9)C30—C31—C26120.5 (2)
C14—As2—Ru2116.46 (6)C37—C32—C33118.9 (2)
C20—As2—Ru2114.03 (6)C37—C32—P1120.28 (17)
C13—As2—Ru2116.51 (6)C33—C32—P1120.79 (18)
C26—P1—C38103.46 (10)C34—C33—C32120.1 (2)
C26—P1—C32102.75 (10)C34—C33—H33A120.0
C38—P1—C32102.83 (10)C32—C33—H33A120.0
C26—P1—Ru3117.33 (7)C35—C34—C33120.4 (2)
C38—P1—Ru3113.44 (7)C35—C34—H34A119.8
C32—P1—Ru3115.22 (7)C33—C34—H34A119.8
C31—O10—C53117.7 (2)C36—C35—C34120.1 (2)
C2—C1—C6119.1 (2)C36—C35—H35A119.9
C2—C1—As1120.56 (16)C34—C35—H35A119.9
C6—C1—As1120.17 (16)C35—C36—C37119.9 (2)
C3—C2—C1120.2 (2)C35—C36—H36A120.0
C3—C2—H2A119.9C37—C36—H36A120.0
C1—C2—H2A119.9C36—C37—C32120.6 (2)
C4—C3—C2120.0 (2)C36—C37—H37A119.7
C4—C3—H3A120.0C32—C37—H37A119.7
C2—C3—H3A120.0C39—C38—C43118.6 (2)
C5—C4—C3120.2 (2)C39—C38—P1122.91 (18)
C5—C4—H4A119.9C43—C38—P1118.50 (16)
C3—C4—H4A119.9C38—C39—C40120.3 (2)
C6—C5—C4119.8 (2)C38—C39—H39A119.9
C6—C5—H5A120.1C40—C39—H39A119.9
C4—C5—H5A120.1C41—C40—C39120.4 (2)
C5—C6—C1120.6 (2)C41—C40—H40A119.8
C5—C6—H6A119.7C39—C40—H40A119.8
C1—C6—H6A119.7C40—C41—C42119.9 (2)
C12—C7—C8119.4 (2)C40—C41—H41A120.0
C12—C7—As1125.02 (16)C42—C41—H41A120.0
C8—C7—As1115.46 (16)C43—C42—C41119.8 (2)
C9—C8—C7120.5 (2)C43—C42—H42A120.1
C9—C8—H8A119.7C41—C42—H42A120.1
C7—C8—H8A119.7C42—C43—C38121.1 (2)
C8—C9—C10120.0 (2)C42—C43—H43A119.5
C8—C9—H9A120.0C38—C43—H43A119.5
C10—C9—H9A120.0O1—C44—Ru1174.8 (2)
C11—C10—C9119.5 (2)O2—C45—Ru1175.9 (2)
C11—C10—H10A120.2O3—C46—Ru1174.4 (2)
C9—C10—H10A120.2O4—C47—Ru2170.1 (2)
C10—C11—C12120.6 (2)O5—C48—Ru2176.4 (2)
C10—C11—H11A119.7O6—C49—Ru2173.66 (19)
C12—C11—H11A119.7O7—C50—Ru3171.28 (19)
C7—C12—C11119.9 (2)O8—C51—Ru3176.9 (2)
C7—C12—H12A120.0O9—C52—Ru3174.72 (19)
C11—C12—H12A120.0O10—C53—H53A109.5
As2—C13—As1111.74 (10)O10—C53—H53B109.5
As2—C13—H13A109.3H53A—C53—H53B109.5
As1—C13—H13A109.3O10—C53—H53C109.5
As2—C13—H13B109.3H53A—C53—H53C109.5
As1—C13—H13B109.3H53B—C53—H53C109.5
H13A—C13—H13B107.9
C45—Ru1—Ru2—C48−64.4 (4)C7—As1—C1—C2−106.30 (17)
C46—Ru1—Ru2—C48−141.6 (4)C13—As1—C1—C2147.58 (16)
C44—Ru1—Ru2—C4832.1 (4)Ru1—As1—C1—C216.38 (19)
As1—Ru1—Ru2—C48123.5 (4)C7—As1—C1—C668.64 (18)
Ru3—Ru1—Ru2—C48−46.0 (4)C13—As1—C1—C6−37.49 (18)
C45—Ru1—Ru2—C4753.9 (2)Ru1—As1—C1—C6−168.68 (13)
C46—Ru1—Ru2—C47−23.35 (9)C6—C1—C2—C30.3 (3)
C44—Ru1—Ru2—C47150.35 (9)As1—C1—C2—C3175.31 (16)
As1—Ru1—Ru2—C47−118.22 (6)C1—C2—C3—C41.1 (3)
Ru3—Ru1—Ru2—C4772.29 (6)C2—C3—C4—C5−1.0 (3)
C45—Ru1—Ru2—C49−123.4 (2)C3—C4—C5—C6−0.4 (3)
C46—Ru1—Ru2—C49159.35 (9)C4—C5—C6—C11.8 (3)
C44—Ru1—Ru2—C49−26.95 (9)C2—C1—C6—C5−1.8 (3)
As1—Ru1—Ru2—C4964.48 (6)As1—C1—C6—C5−176.76 (16)
Ru3—Ru1—Ru2—C49−105.01 (6)C1—As1—C7—C12−120.94 (19)
C45—Ru1—Ru2—As2145.56 (19)C13—As1—C7—C12−17.5 (2)
C46—Ru1—Ru2—As268.28 (6)Ru1—As1—C7—C12108.78 (18)
C44—Ru1—Ru2—As2−118.02 (6)C1—As1—C7—C863.38 (18)
As1—Ru1—Ru2—As2−26.588 (9)C13—As1—C7—C8166.78 (16)
Ru3—Ru1—Ru2—As2163.916 (9)Ru1—As1—C7—C8−66.90 (17)
C45—Ru1—Ru2—Ru3−18.36 (19)C12—C7—C8—C90.5 (3)
C46—Ru1—Ru2—Ru3−95.63 (6)As1—C7—C8—C9176.41 (17)
C44—Ru1—Ru2—Ru378.06 (6)C7—C8—C9—C100.3 (3)
As1—Ru1—Ru2—Ru3169.496 (9)C8—C9—C10—C11−0.6 (4)
C45—Ru1—Ru3—C51−24.23 (10)C9—C10—C11—C120.1 (4)
C46—Ru1—Ru3—C51−115.58 (10)C8—C7—C12—C11−0.9 (3)
C44—Ru1—Ru3—C5164.77 (10)As1—C7—C12—C11−176.44 (17)
As1—Ru1—Ru3—C51139.50 (7)C10—C11—C12—C70.6 (4)
Ru2—Ru1—Ru3—C51162.45 (7)C14—As2—C13—As1−148.46 (11)
C45—Ru1—Ru3—C50−119.78 (9)C20—As2—C13—As1104.11 (11)
C46—Ru1—Ru3—C50148.86 (9)Ru2—As2—C13—As1−22.64 (13)
C44—Ru1—Ru3—C50−30.78 (9)C7—As1—C13—As2120.32 (11)
As1—Ru1—Ru3—C5043.95 (7)C1—As1—C13—As2−138.89 (10)
Ru2—Ru1—Ru3—C5066.90 (7)Ru1—As1—C13—As2−3.55 (13)
C45—Ru1—Ru3—C5273.07 (9)C20—As2—C14—C190.7 (2)
C46—Ru1—Ru3—C52−18.29 (9)C13—As2—C14—C19−106.86 (19)
C44—Ru1—Ru3—C52162.07 (9)Ru2—As2—C14—C19127.29 (17)
As1—Ru1—Ru3—C52−123.20 (7)C20—As2—C14—C15179.39 (17)
Ru2—Ru1—Ru3—C52−100.25 (7)C13—As2—C14—C1571.82 (18)
C45—Ru1—Ru3—Ru2173.32 (7)Ru2—As2—C14—C15−54.04 (18)
C46—Ru1—Ru3—Ru281.96 (7)C19—C14—C15—C162.2 (3)
C44—Ru1—Ru3—Ru2−97.68 (7)As2—C14—C15—C16−176.57 (18)
As1—Ru1—Ru3—Ru2−22.956 (18)C14—C15—C16—C17−0.4 (3)
C48—Ru2—Ru3—C51140.28 (14)C15—C16—C17—C18−1.7 (4)
C47—Ru2—Ru3—C51−134.08 (14)C16—C17—C18—C192.0 (4)
C49—Ru2—Ru3—C5144.34 (14)C17—C18—C19—C14−0.2 (3)
As2—Ru2—Ru3—C51−62.34 (12)C15—C14—C19—C18−1.8 (3)
Ru1—Ru2—Ru3—C51−31.81 (12)As2—C14—C19—C18176.81 (17)
C48—Ru2—Ru3—C5066.77 (10)C14—As2—C20—C25−126.47 (18)
C47—Ru2—Ru3—C50152.42 (10)C13—As2—C20—C25−22.8 (2)
C49—Ru2—Ru3—C50−29.16 (10)Ru2—As2—C20—C25105.46 (17)
As2—Ru2—Ru3—C50−135.84 (7)C14—As2—C20—C2161.52 (18)
Ru1—Ru2—Ru3—C50−105.32 (7)C13—As2—C20—C21165.16 (16)
C48—Ru2—Ru3—C52−105.57 (10)Ru2—As2—C20—C21−66.56 (18)
C47—Ru2—Ru3—C52−19.92 (10)C25—C20—C21—C220.7 (3)
C49—Ru2—Ru3—C52158.50 (9)As2—C20—C21—C22172.95 (16)
As2—Ru2—Ru3—C5251.82 (7)C20—C21—C22—C23−0.7 (3)
Ru1—Ru2—Ru3—C5282.34 (7)C21—C22—C23—C240.4 (3)
C48—Ru2—Ru3—P1−13.43 (7)C22—C23—C24—C25−0.1 (4)
C47—Ru2—Ru3—P172.22 (7)C21—C20—C25—C24−0.4 (3)
C49—Ru2—Ru3—P1−109.36 (7)As2—C20—C25—C24−172.32 (17)
As2—Ru2—Ru3—P1143.96 (2)C23—C24—C25—C200.1 (3)
Ru1—Ru2—Ru3—P1174.484 (18)C38—P1—C26—C276.5 (2)
C48—Ru2—Ru3—Ru1172.09 (7)C32—P1—C26—C27113.28 (19)
C47—Ru2—Ru3—Ru1−102.26 (7)Ru3—P1—C26—C27−119.22 (17)
C49—Ru2—Ru3—Ru176.15 (7)C38—P1—C26—C31−175.21 (17)
As2—Ru2—Ru3—Ru1−30.525 (15)C32—P1—C26—C31−68.45 (19)
C45—Ru1—As1—C785.03 (10)Ru3—P1—C26—C3159.04 (19)
C46—Ru1—As1—C7177.80 (10)C31—C26—C27—C28−1.8 (3)
C44—Ru1—As1—C7−5.88 (10)P1—C26—C27—C28176.48 (18)
Ru3—Ru1—As1—C7−78.06 (7)C26—C27—C28—C29−0.2 (4)
Ru2—Ru1—As1—C7−97.98 (7)C27—C28—C29—C301.4 (4)
C45—Ru1—As1—C1−30.66 (10)C28—C29—C30—C31−0.6 (4)
C46—Ru1—As1—C162.12 (10)C53—O10—C31—C3011.7 (3)
C44—Ru1—As1—C1−121.57 (10)C53—O10—C31—C26−169.1 (2)
Ru3—Ru1—As1—C1166.25 (7)C29—C30—C31—O10177.8 (2)
Ru2—Ru1—As1—C1146.34 (7)C29—C30—C31—C26−1.4 (4)
C45—Ru1—As1—C13−155.35 (10)C27—C26—C31—O10−176.68 (19)
C46—Ru1—As1—C13−62.58 (10)P1—C26—C31—O105.0 (3)
C44—Ru1—As1—C13113.73 (10)C27—C26—C31—C302.6 (3)
Ru3—Ru1—As1—C1341.55 (8)P1—C26—C31—C30−175.73 (18)
Ru2—Ru1—As1—C1321.64 (7)C26—P1—C32—C37168.47 (18)
C48—Ru2—As2—C14−26.10 (10)C38—P1—C32—C37−84.30 (19)
C47—Ru2—As2—C14−117.66 (10)Ru3—P1—C32—C3739.64 (19)
C49—Ru2—As2—C1465.84 (10)C26—P1—C32—C33−14.2 (2)
Ru1—Ru2—As2—C14148.83 (7)C38—P1—C32—C3393.00 (19)
Ru3—Ru2—As2—C14174.76 (7)Ru3—P1—C32—C33−143.06 (16)
C48—Ru2—As2—C2095.45 (10)C37—C32—C33—C34−0.3 (3)
C47—Ru2—As2—C203.89 (10)P1—C32—C33—C34−177.61 (17)
C49—Ru2—As2—C20−172.61 (10)C32—C33—C34—C351.4 (4)
Ru1—Ru2—As2—C20−89.62 (7)C33—C34—C35—C36−1.4 (4)
Ru3—Ru2—As2—C20−63.69 (8)C34—C35—C36—C370.3 (4)
C48—Ru2—As2—C13−142.72 (10)C35—C36—C37—C320.8 (3)
C47—Ru2—As2—C13125.73 (10)C33—C32—C37—C36−0.8 (3)
C49—Ru2—As2—C13−50.77 (10)P1—C32—C37—C36176.54 (17)
Ru1—Ru2—As2—C1332.21 (7)C26—P1—C38—C39107.4 (2)
Ru3—Ru2—As2—C1358.15 (7)C32—P1—C38—C390.7 (2)
C51—Ru3—P1—C26−95.89 (11)Ru3—P1—C38—C39−124.40 (18)
C50—Ru3—P1—C26−0.29 (11)C26—P1—C38—C43−73.14 (19)
C52—Ru3—P1—C26166.93 (11)C32—P1—C38—C43−179.84 (18)
Ru2—Ru3—P1—C2669.41 (9)Ru3—P1—C38—C4355.06 (19)
C51—Ru3—P1—C38143.46 (11)C43—C38—C39—C400.3 (3)
C50—Ru3—P1—C38−120.94 (11)P1—C38—C39—C40179.77 (19)
C52—Ru3—P1—C3846.28 (10)C38—C39—C40—C410.9 (4)
Ru2—Ru3—P1—C38−51.24 (8)C39—C40—C41—C42−0.9 (4)
C51—Ru3—P1—C3225.31 (11)C40—C41—C42—C43−0.3 (4)
C50—Ru3—P1—C32120.91 (10)C41—C42—C43—C381.5 (4)
C52—Ru3—P1—C32−71.87 (10)C39—C38—C43—C42−1.5 (3)
Ru2—Ru3—P1—C32−169.39 (8)P1—C38—C43—C42179.03 (19)
D—H···AD—HH···AD···AD—H···A
C16—H16A···O4i0.932.523.244 (3)135
C29—H29A···O5ii0.932.563.286 (3)135
C5—H5A···Cg1iii0.932.843.668 (2)149
C18—H18A···Cg2iv0.932.953.701 (2)139
C22—H22A···Cg2v0.932.953.787 (2)151
C24—H24A···Cg3iv0.932.813.499 (2)132
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A DA D—H⋯A
C16—H16A⋯O4i 0.932.523.244 (3)135
C29—H29A⋯O5ii 0.932.563.286 (3)135
C5—H5ACg1iii 0.932.843.668 (2)149
C18—H18ACg2iv 0.932.953.701 (2)139
C22—H22ACg2v 0.932.953.787 (2)151
C24—H24ACg3iv 0.932.813.499 (2)132

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) . Cg1, Cg2 and Cg3 are the centroids of the C7–C12, C1–C6 and C14–C19 rings, respectively.

  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.  Undeca-carbonyl-1κC,2κC,3κC-[tris-(4-methyl-phen-yl)arsine-1κAs]-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:  2009-11-21

3.  [μ-Bis-(diphenyl-phosphino)methane-1:2κP:P']nonacarbonyl-1κC,2κC,3κC-[tris-(4-methyl-phen-yl)arsine-3κAs]-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:  2009-11-21

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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