PMCCPMCCPMCC

Search tips
Search criteria 

Advanced

 
Logo of actaeInternational Union of Crystallographysearchopen accessarticle submissionjournal home pagethis article
 
Acta Crystallogr Sect E Struct Rep Online. 2008 February 1; 64(Pt 2): m290.
Published online 2008 January 4. doi:  10.1107/S160053680706792X
PMCID: PMC2960167

trans-Carbon­yl[dihydro­bis(1,2,4-triazol-1-yl-κN 2)borato]hydridobis(triphenyl­phosphine-κP)ruthenium(II) acetonitrile solvate

Abstract

In the crystal structure of the title compound, [Ru(C4H6BN6)H(C18H15P)2(CO)]·C2H3N, discrete mononuclear complexes are found in which the Ru atom is coordinated by two triphenyl­phosphine (PPh3) ligands, one dihydro­bis(1,2,4-triazol-1-yl)borate ligand, one carbonyl ligand and one hydride atom within slightly distorted octa­hedra. The two P atoms of the PPh3 ligands are trans positioned and the two N atoms of the chelating dihydro­bis(1,2,4-triazol-1-yl)borate ligand occupy cis positions.

Related literature

For related literature, see: Youm et al. (2006 [triangle]); Huh et al. (1999 [triangle], 2000 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m290-scheme1.jpg

Experimental

Crystal data

  • [Ru(C4H6BN6)H(C18H15P)2(CO)]·C2H3N
  • M r = 844.64
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m290-efi1.jpg
  • a = 9.0733 (1) Å
  • b = 11.8032 (3) Å
  • c = 20.2609 (6) Å
  • α = 74.438 (11)°
  • β = 89.552 (15)°
  • γ = 70.731 (14)°
  • V = 1965.4 (2) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 0.53 mm−1
  • T = 100 (2) K
  • 0.35 × 0.30 × 0.28 mm

Data collection

  • Nonius KappaCCD diffractometer
  • Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997 [triangle]) T min = 0.838, T max = 0.867
  • 31908 measured reflections
  • 8964 independent reflections
  • 6896 reflections with I > 2σ(I)
  • R int = 0.060

Refinement

  • R[F 2 > 2σ(F 2)] = 0.034
  • wR(F 2) = 0.079
  • S = 0.98
  • 8964 reflections
  • 521 parameters
  • 9 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.76 e Å−3
  • Δρmin = −0.79 e Å−3

Data collection: KappaCCD Server Software (Nonius, 1997 [triangle]); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997 [triangle]); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 [triangle]); molecular graphics: SHELXTL/PC (Bruker, 1998 [triangle]); software used to prepare material for publication: SHELXTL/PC.

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680706792X/nc2075sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680706792X/nc2075Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The author thanks Dr Alan J. Lough of the University of Toronto for the structure determination.

supplementary crystallographic information

Comment

In our ongoing investigations on the preparation of one-dimensional coordination polymers containing catalytically active RuII complex moieties, we recently reported the preparation and spectroscopic data of the title compound (I) (Youm et al., 2006). The proposed structure of (I) which based on the spectroscopic data closely resembles those of the previously structurally characterized analogues, [RuH(AsPh3)22-H2Bpz2)(CO)] (II) (pz is pyrazol-1-yl) (Huh et al., 1999) and [RuH{P(p-C6H4CH3)3}22-H2Bpz2)(CO)] (III) (Huh et al., 2000). Here we report the crystal structure of compound (I).

The crystal structure of compound I shows similar structural features as the analogous structures of (II) and (III) and therefore, confirm the proposed structure of (I) from our spectroscopic investigations.

In the crystal structure of the title compound the Ru atom is coordinated by two phosphorous atoms of two crystallographically independent triphenylphosphine ligands, one carbon atom of the CO ligand, one hydride H atom and two nitrogen atoms of the dihydrobis(1,2,4-triazol-1-yl)borate ligand within a slightly distorted octahedra (Fig. 1). The two phosphorous atoms of the PPh3 ligands are trans-positioned and the two nitrogen atoms of the chelating dihydrobis(1,2,4-triazol-1-yl)borate ligand occupy cis-positions. The two Ru—P bond lengths are slightly longer than those in (III) [2.3448 (17) – 2.3699 (17) Å] (Tab. 1). In (I), the Ru1—P1 bond length is slightly longer than the Ru1—P2 bond by about 0.039 Å (Tab. 1). However, the Ru—N bond distances are very similar to those in (III). The H1—Ru—P2 angle of 81.0 (8)° is smaller than the H1—Ru—P1 angle of 91.1 (8)° (Tab. 1).

Experimental

The title compound was prepared according to the literature method (Youm et al., 2006). Single crystals are obtained by slow evaporation of the solvent from a solution of (I) in acetonitrile.

Refinement

H atoms bonded to C atoms were placed in calculated positions [C—H = 0.95 - 0.97 Å] and included in the refinement in a riding-model approximation with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms. The hydride H atom [H1RU], the H atoms connected to B1 and to the nitrogen atom of the acetonitrile molecules were refined with varying coordinates and free isotropic displacement parameters.

Figures

Fig. 1.
The molecular structure of the title compound with labeling and displacement ellipsoids drawn at the 50% probability level. All hydrogen atoms except the hydride and hydrogen atoms attached to the B atom are omitted for clarity.

Crystal data

[Ru(C4H6BN6)H(C18H15P)2(CO)]·C2H3NZ = 2
Mr = 844.64F000 = 868
Triclinic, P1Dx = 1.427 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 9.0733 (1) ÅCell parameters from 31908 reflections
b = 11.8032 (3) Åθ = 4.1–27.5º
c = 20.2609 (6) ŵ = 0.53 mm1
α = 74.438 (11)ºT = 100 (2) K
β = 89.552 (15)ºBlock cut from needle, pale yellow
γ = 70.731 (14)º0.35 × 0.30 × 0.28 mm
V = 1965.4 (2) Å3

Data collection

Nonius KappaCCD diffractometer8964 independent reflections
Radiation source: fine-focus sealed tube6896 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.060
Detector resolution: 9 pixels mm-1θmax = 27.5º
T = 100(2) Kθmin = 4.1º
[var phi] scan and ω scans with κ offsetsh = −11→11
Absorption correction: multi-scan(DENZO-SMN; Otwinowski & Minor, 1997)k = −13→15
Tmin = 0.838, Tmax = 0.867l = −26→26
31908 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.079  w = 1/[σ2(Fo2) + (0.0387P)2] where P = (Fo2 + 2Fc2)/3
S = 0.99(Δ/σ)max = 0.002
8964 reflectionsΔρmax = 0.76 e Å3
521 parametersΔρmin = −0.79 e Å3
9 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

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)

xyzUiso*/Ueq
Ru10.991567 (18)0.597576 (15)0.723224 (10)0.01409 (6)
H1RU0.815 (2)0.668 (2)0.6948 (12)0.022 (6)*
P10.97691 (6)0.40525 (5)0.71054 (3)0.01384 (12)
P20.97123 (6)0.80041 (5)0.72650 (3)0.01507 (12)
O11.09179 (19)0.66608 (15)0.58094 (9)0.0295 (4)
N11.23032 (19)0.49727 (16)0.77038 (10)0.0160 (4)
N21.2776 (2)0.46297 (17)0.83893 (10)0.0194 (4)
N31.4870 (2)0.38206 (18)0.78677 (11)0.0251 (5)
N40.91255 (19)0.54559 (16)0.82298 (10)0.0162 (4)
N51.0082 (2)0.49179 (16)0.88370 (10)0.0195 (4)
N60.7751 (2)0.47449 (18)0.90769 (11)0.0267 (5)
C11.0512 (2)0.63962 (19)0.63591 (13)0.0181 (5)
C21.3590 (2)0.44611 (19)0.74159 (12)0.0195 (5)
H2A1.36040.45400.69370.023*
C31.4305 (2)0.3955 (2)0.84596 (13)0.0266 (6)
H3A1.49230.36070.88890.032*
C40.7767 (2)0.5315 (2)0.84039 (13)0.0212 (5)
H4A0.68790.55920.80810.025*
C50.9212 (3)0.4511 (2)0.93188 (13)0.0258 (5)
H5A0.96000.40980.97860.031*
C111.0065 (2)0.28484 (19)0.79288 (12)0.0161 (4)
C120.8863 (2)0.2443 (2)0.82195 (12)0.0200 (5)
H12A0.78590.27460.79740.024*
C130.9140 (3)0.1595 (2)0.88699 (13)0.0254 (5)
H13A0.83170.13260.90670.031*
C141.0599 (3)0.1136 (2)0.92364 (13)0.0260 (5)
H14A1.07780.05490.96780.031*
C151.1800 (2)0.1544 (2)0.89514 (13)0.0216 (5)
H15A1.28020.12410.92000.026*
C161.1531 (2)0.23893 (19)0.83086 (12)0.0182 (5)
H16A1.23540.26670.81180.022*
C211.1176 (2)0.32556 (19)0.65704 (12)0.0165 (5)
C221.1077 (2)0.3869 (2)0.58734 (12)0.0216 (5)
H22A1.03220.46810.56960.026*
C231.2054 (3)0.3322 (2)0.54338 (13)0.0245 (5)
H23A1.19670.37570.49600.029*
C241.3165 (3)0.2133 (2)0.56868 (13)0.0245 (5)
H24A1.38470.17580.53880.029*
C251.3268 (3)0.1503 (2)0.63731 (14)0.0298 (6)
H25A1.40160.06870.65460.036*
C261.2285 (3)0.2052 (2)0.68153 (13)0.0240 (5)
H26A1.23670.16070.72880.029*
C310.7951 (2)0.4155 (2)0.66621 (11)0.0161 (4)
C320.6824 (2)0.5310 (2)0.63387 (12)0.0189 (5)
H32A0.69430.60550.63860.023*
C330.5524 (2)0.5382 (2)0.59473 (12)0.0221 (5)
H33A0.47750.61740.57210.026*
C340.5322 (2)0.4303 (2)0.58883 (12)0.0226 (5)
H34A0.44290.43530.56260.027*
C350.6424 (3)0.3145 (2)0.62120 (13)0.0235 (5)
H35A0.62810.24030.61730.028*
C360.7736 (2)0.3071 (2)0.65924 (12)0.0208 (5)
H36A0.84950.22770.68070.025*
C410.9074 (2)0.91694 (19)0.64166 (12)0.0177 (5)
C420.7850 (3)0.9175 (2)0.60011 (13)0.0239 (5)
H42A0.73730.85550.61510.029*
C430.7320 (3)1.0073 (2)0.53737 (13)0.0259 (5)
H43A0.64861.00640.50970.031*
C440.8006 (3)1.0989 (2)0.51474 (13)0.0262 (5)
H44A0.76431.16040.47170.031*
C450.9218 (3)1.0994 (2)0.55539 (13)0.0244 (5)
H45A0.96911.16160.54010.029*
C460.9751 (2)1.0099 (2)0.61834 (12)0.0210 (5)
H46A1.05821.01160.64590.025*
C511.1555 (2)0.81957 (19)0.74822 (12)0.0170 (5)
C521.2868 (2)0.7637 (2)0.71679 (12)0.0201 (5)
H52A1.27840.71690.68640.024*
C531.4298 (2)0.7767 (2)0.73004 (13)0.0230 (5)
H53A1.51860.73900.70840.028*
C541.4430 (2)0.8441 (2)0.77453 (13)0.0238 (5)
H54A1.54130.85160.78390.029*
C551.3140 (2)0.9007 (2)0.80537 (13)0.0221 (5)
H55A1.32320.94780.83550.027*
C561.1690 (2)0.8885 (2)0.79220 (12)0.0194 (5)
H56A1.08010.92750.81340.023*
C610.8356 (2)0.8771 (2)0.78193 (12)0.0182 (5)
C620.8375 (2)0.8146 (2)0.85103 (12)0.0213 (5)
H62A0.90690.73110.86900.026*
C630.7396 (3)0.8727 (2)0.89403 (14)0.0259 (5)
H63A0.74180.82900.94100.031*
C640.6377 (3)0.9956 (2)0.86808 (14)0.0280 (6)
H64A0.57041.03570.89740.034*
C650.6349 (3)1.0586 (2)0.80013 (15)0.0283 (6)
H65A0.56631.14250.78270.034*
C660.7322 (2)1.0002 (2)0.75667 (13)0.0223 (5)
H66A0.72831.04410.70960.027*
B11.1701 (3)0.5070 (3)0.89352 (15)0.0241 (6)
H1B1.227 (3)0.447 (2)0.9452 (14)0.031 (7)*
H2B1.147 (3)0.615 (2)0.8855 (13)0.029 (7)*
N1S0.5802 (3)1.1379 (2)1.00400 (13)0.0398 (6)
C1S0.5862 (3)1.3314 (3)1.04008 (15)0.0385 (7)
C2S0.5840 (3)1.2214 (3)1.02053 (13)0.0290 (6)
H1S0.660 (2)1.3039 (18)1.0804 (9)0.044*
H2S0.620 (2)1.3844 (17)1.0025 (10)0.044*
H3S0.483 (2)1.3758 (17)1.0506 (10)0.044*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ru10.01425 (9)0.01286 (9)0.01445 (11)−0.00458 (6)0.00124 (6)−0.00273 (7)
P10.0149 (3)0.0122 (3)0.0137 (3)−0.0046 (2)0.0013 (2)−0.0025 (2)
P20.0144 (3)0.0128 (3)0.0181 (3)−0.0048 (2)0.0018 (2)−0.0045 (2)
O10.0422 (10)0.0280 (9)0.0200 (11)−0.0163 (8)0.0089 (8)−0.0041 (8)
N10.0166 (9)0.0157 (9)0.0158 (11)−0.0067 (7)0.0022 (7)−0.0034 (8)
N20.0185 (9)0.0210 (10)0.0162 (11)−0.0039 (7)−0.0015 (7)−0.0044 (8)
N30.0171 (9)0.0275 (11)0.0251 (13)−0.0010 (8)−0.0002 (8)−0.0066 (9)
N40.0177 (9)0.0141 (9)0.0158 (11)−0.0042 (7)0.0027 (7)−0.0040 (8)
N50.0215 (9)0.0169 (9)0.0164 (11)−0.0024 (7)0.0018 (7)−0.0040 (8)
N60.0318 (11)0.0277 (11)0.0235 (13)−0.0134 (9)0.0118 (9)−0.0078 (9)
C10.0190 (11)0.0122 (11)0.0225 (14)−0.0055 (8)−0.0011 (9)−0.0034 (9)
C20.0178 (11)0.0192 (11)0.0192 (13)−0.0057 (8)0.0037 (9)−0.0025 (10)
C30.0193 (11)0.0276 (13)0.0260 (15)−0.0007 (9)−0.0055 (10)−0.0051 (11)
C40.0198 (11)0.0208 (12)0.0243 (14)−0.0078 (9)0.0054 (9)−0.0076 (10)
C50.0350 (13)0.0227 (12)0.0174 (14)−0.0085 (10)0.0070 (10)−0.0035 (10)
C110.0204 (10)0.0103 (10)0.0165 (13)−0.0038 (8)0.0018 (8)−0.0037 (9)
C120.0172 (11)0.0192 (11)0.0211 (14)−0.0059 (8)0.0013 (9)−0.0023 (10)
C130.0253 (12)0.0268 (13)0.0226 (15)−0.0132 (10)0.0036 (10)0.0009 (11)
C140.0300 (13)0.0230 (12)0.0188 (14)−0.0080 (10)0.0009 (10)0.0031 (10)
C150.0199 (11)0.0177 (11)0.0226 (14)−0.0034 (9)−0.0010 (9)−0.0020 (10)
C160.0178 (10)0.0155 (11)0.0203 (13)−0.0054 (8)0.0014 (9)−0.0041 (9)
C210.0158 (10)0.0174 (11)0.0196 (13)−0.0081 (8)0.0019 (8)−0.0072 (9)
C220.0229 (11)0.0192 (12)0.0195 (14)−0.0038 (9)0.0018 (9)−0.0044 (10)
C230.0263 (12)0.0294 (13)0.0172 (14)−0.0085 (10)0.0052 (9)−0.0068 (10)
C240.0229 (12)0.0295 (13)0.0271 (15)−0.0103 (10)0.0093 (10)−0.0162 (11)
C250.0298 (13)0.0216 (12)0.0321 (16)0.0003 (10)0.0061 (11)−0.0094 (11)
C260.0264 (12)0.0182 (12)0.0225 (14)−0.0032 (9)0.0033 (10)−0.0036 (10)
C310.0160 (10)0.0189 (11)0.0134 (12)−0.0063 (8)0.0024 (8)−0.0043 (9)
C320.0209 (11)0.0204 (11)0.0167 (13)−0.0092 (9)0.0035 (9)−0.0046 (9)
C330.0170 (11)0.0267 (12)0.0183 (13)−0.0045 (9)−0.0016 (9)−0.0033 (10)
C340.0207 (11)0.0343 (14)0.0158 (13)−0.0133 (10)0.0015 (9)−0.0069 (10)
C350.0257 (12)0.0263 (12)0.0244 (14)−0.0142 (10)0.0043 (10)−0.0102 (11)
C360.0211 (11)0.0175 (11)0.0221 (14)−0.0055 (9)0.0006 (9)−0.0044 (10)
C410.0190 (10)0.0128 (10)0.0183 (13)−0.0025 (8)0.0014 (8)−0.0029 (9)
C420.0255 (12)0.0175 (11)0.0263 (15)−0.0063 (9)−0.0031 (10)−0.0034 (10)
C430.0230 (12)0.0221 (12)0.0260 (15)−0.0005 (9)−0.0063 (10)−0.0049 (11)
C440.0309 (13)0.0186 (12)0.0200 (14)0.0007 (9)0.0015 (10)−0.0019 (10)
C450.0288 (12)0.0176 (11)0.0245 (15)−0.0078 (9)0.0080 (10)−0.0024 (10)
C460.0199 (11)0.0189 (11)0.0237 (14)−0.0062 (9)0.0026 (9)−0.0056 (10)
C510.0168 (10)0.0124 (10)0.0189 (13)−0.0044 (8)0.0011 (8)−0.0002 (9)
C520.0209 (11)0.0164 (11)0.0225 (14)−0.0065 (8)0.0013 (9)−0.0044 (10)
C530.0157 (11)0.0214 (12)0.0303 (15)−0.0051 (9)0.0061 (9)−0.0065 (11)
C540.0179 (11)0.0221 (12)0.0297 (15)−0.0094 (9)−0.0018 (9)−0.0013 (10)
C550.0237 (11)0.0199 (12)0.0236 (14)−0.0103 (9)−0.0023 (9)−0.0039 (10)
C560.0208 (11)0.0156 (11)0.0210 (13)−0.0056 (8)0.0013 (9)−0.0045 (9)
C610.0131 (10)0.0183 (11)0.0269 (14)−0.0068 (8)0.0027 (9)−0.0101 (10)
C620.0216 (11)0.0217 (12)0.0219 (14)−0.0075 (9)0.0032 (9)−0.0081 (10)
C630.0236 (12)0.0335 (14)0.0270 (15)−0.0127 (10)0.0072 (10)−0.0153 (11)
C640.0212 (12)0.0300 (13)0.0409 (18)−0.0093 (10)0.0109 (10)−0.0225 (13)
C650.0219 (12)0.0190 (12)0.0458 (18)−0.0062 (9)0.0074 (11)−0.0129 (12)
C660.0180 (11)0.0164 (11)0.0324 (15)−0.0066 (8)0.0059 (9)−0.0059 (10)
B10.0225 (13)0.0284 (15)0.0204 (16)−0.0031 (11)−0.0001 (11)−0.0123 (12)
N1S0.0555 (15)0.0322 (13)0.0298 (15)−0.0145 (11)0.0069 (11)−0.0064 (11)
C1S0.0487 (17)0.0355 (16)0.0321 (18)−0.0222 (13)−0.0020 (13)−0.0006 (13)
C2S0.0287 (13)0.0345 (15)0.0178 (14)−0.0105 (11)0.0033 (10)0.0022 (11)

Geometric parameters (Å, °)

Ru1—H1RU1.57 (2)C31—C321.394 (3)
Ru1—C11.833 (2)C31—C361.398 (3)
Ru1—N42.1396 (19)C32—C331.392 (3)
Ru1—N12.1771 (17)C32—H32A0.9500
Ru1—P22.3588 (6)C33—C341.380 (3)
Ru1—P12.3978 (6)C33—H33A0.9500
P1—C111.833 (2)C34—C351.387 (3)
P1—C311.837 (2)C34—H34A0.9500
P1—C211.850 (2)C35—C361.389 (3)
P2—C511.831 (2)C35—H35A0.9500
P2—C611.839 (2)C36—H36A0.9500
P2—C411.845 (2)C41—C421.396 (3)
O1—C11.165 (3)C41—C461.403 (3)
N1—C21.334 (3)C42—C431.386 (3)
N1—N21.367 (3)C42—H42A0.9500
N2—C31.339 (3)C43—C441.392 (3)
N2—B11.550 (3)C43—H43A0.9500
N3—C31.328 (3)C44—C451.382 (3)
N3—C21.351 (3)C44—H44A0.9500
N4—C41.330 (3)C45—C461.388 (3)
N4—N51.380 (2)C45—H45A0.9500
N5—C51.339 (3)C46—H46A0.9500
N5—B11.558 (3)C51—C561.389 (3)
N6—C51.330 (3)C51—C521.398 (3)
N6—C41.351 (3)C52—C531.392 (3)
C2—H2A0.9500C52—H52A0.9500
C3—H3A0.9500C53—C541.382 (3)
C4—H4A0.9500C53—H53A0.9500
C5—H5A0.9500C54—C551.380 (3)
C11—C121.396 (3)C54—H54A0.9500
C11—C161.404 (3)C55—C561.405 (3)
C12—C131.390 (3)C55—H55A0.9500
C12—H12A0.9500C56—H56A0.9500
C13—C141.387 (3)C61—C621.393 (3)
C13—H13A0.9500C61—C661.401 (3)
C14—C151.393 (3)C62—C631.387 (3)
C14—H14A0.9500C62—H62A0.9500
C15—C161.378 (3)C63—C641.396 (3)
C15—H15A0.9500C63—H63A0.9500
C16—H16A0.9500C64—C651.374 (4)
C21—C221.392 (3)C64—H64A0.9500
C21—C261.401 (3)C65—C661.393 (3)
C22—C231.384 (3)C65—H65A0.9500
C22—H22A0.9500C66—H66A0.9500
C23—C241.391 (3)B1—H1B1.11 (3)
C23—H23A0.9500B1—H2B1.19 (2)
C24—C251.377 (3)N1S—C2S1.133 (3)
C24—H24A0.9500C1S—C2S1.463 (4)
C25—C261.391 (3)C1S—H1S0.969 (16)
C25—H25A0.9500C1S—H2S0.966 (16)
C26—H26A0.9500C1S—H3S0.960 (16)
H1RU—Ru1—C190.0 (9)C25—C26—H26A119.7
H1RU—Ru1—N487.9 (9)C21—C26—H26A119.7
C1—Ru1—N4176.92 (8)C32—C31—C36118.57 (19)
H1RU—Ru1—N1175.7 (9)C32—C31—P1121.10 (16)
C1—Ru1—N194.31 (8)C36—C31—P1120.10 (16)
N4—Ru1—N187.84 (7)C33—C32—C31120.6 (2)
H1RU—Ru1—P281.0 (8)C33—C32—H32A119.7
C1—Ru1—P286.77 (7)C31—C32—H32A119.7
N4—Ru1—P295.09 (5)C34—C33—C32120.1 (2)
N1—Ru1—P298.90 (5)C34—C33—H33A120.0
H1RU—Ru1—P191.1 (8)C32—C33—H33A120.0
C1—Ru1—P191.65 (7)C33—C34—C35120.0 (2)
N4—Ru1—P186.16 (5)C33—C34—H34A120.0
N1—Ru1—P189.15 (5)C35—C34—H34A120.0
P2—Ru1—P1171.884 (18)C34—C35—C36120.0 (2)
C11—P1—C31106.50 (10)C34—C35—H35A120.0
C11—P1—C21103.72 (10)C36—C35—H35A120.0
C31—P1—C2198.22 (10)C35—C36—C31120.6 (2)
C11—P1—Ru1112.79 (7)C35—C36—H36A119.7
C31—P1—Ru1116.25 (7)C31—C36—H36A119.7
C21—P1—Ru1117.57 (7)C42—C41—C46118.2 (2)
C51—P2—C61103.14 (10)C42—C41—P2120.30 (17)
C51—P2—C41101.34 (10)C46—C41—P2121.40 (17)
C61—P2—C41101.84 (10)C43—C42—C41120.9 (2)
C51—P2—Ru1115.45 (7)C43—C42—H42A119.5
C61—P2—Ru1120.09 (7)C41—C42—H42A119.5
C41—P2—Ru1112.53 (7)C42—C43—C44120.2 (2)
C2—N1—N2104.51 (16)C42—C43—H43A119.9
C2—N1—Ru1128.99 (15)C44—C43—H43A119.9
N2—N1—Ru1126.25 (13)C45—C44—C43119.4 (2)
C3—N2—N1106.52 (19)C45—C44—H44A120.3
C3—N2—B1129.5 (2)C43—C44—H44A120.3
N1—N2—B1123.77 (17)C44—C45—C46120.6 (2)
C3—N3—C2102.03 (18)C44—C45—H45A119.7
C4—N4—N5104.00 (18)C46—C45—H45A119.7
C4—N4—Ru1129.70 (16)C45—C46—C41120.6 (2)
N5—N4—Ru1124.89 (13)C45—C46—H46A119.7
C5—N5—N4106.46 (18)C41—C46—H46A119.7
C5—N5—B1128.5 (2)C56—C51—C52119.42 (19)
N4—N5—B1123.62 (19)C56—C51—P2123.44 (16)
C5—N6—C4101.79 (19)C52—C51—P2117.11 (17)
O1—C1—Ru1178.72 (18)C53—C52—C51120.0 (2)
N1—C2—N3113.9 (2)C53—C52—H52A120.0
N1—C2—H2A123.1C51—C52—H52A120.0
N3—C2—H2A123.1C54—C53—C52120.3 (2)
N3—C3—N2113.1 (2)C54—C53—H53A119.8
N3—C3—H3A123.5C52—C53—H53A119.8
N2—C3—H3A123.5C55—C54—C53120.2 (2)
N4—C4—N6114.5 (2)C55—C54—H54A119.9
N4—C4—H4A122.7C53—C54—H54A119.9
N6—C4—H4A122.7C54—C55—C56120.0 (2)
N6—C5—N5113.2 (2)C54—C55—H55A120.0
N6—C5—H5A123.4C56—C55—H55A120.0
N5—C5—H5A123.4C51—C56—C55120.1 (2)
C12—C11—C16118.6 (2)C51—C56—H56A120.0
C12—C11—P1122.82 (16)C55—C56—H56A120.0
C16—C11—P1118.38 (16)C62—C61—C66118.5 (2)
C13—C12—C11119.8 (2)C62—C61—P2120.30 (16)
C13—C12—H12A120.1C66—C61—P2121.20 (19)
C11—C12—H12A120.1C63—C62—C61121.0 (2)
C14—C13—C12121.1 (2)C63—C62—H62A119.5
C14—C13—H13A119.4C61—C62—H62A119.5
C12—C13—H13A119.4C62—C63—C64119.8 (2)
C13—C14—C15119.4 (2)C62—C63—H63A120.1
C13—C14—H14A120.3C64—C63—H63A120.1
C15—C14—H14A120.3C65—C64—C63119.9 (2)
C16—C15—C14119.8 (2)C65—C64—H64A120.0
C16—C15—H15A120.1C63—C64—H64A120.0
C14—C15—H15A120.1C64—C65—C66120.4 (2)
C15—C16—C11121.4 (2)C64—C65—H65A119.8
C15—C16—H16A119.3C66—C65—H65A119.8
C11—C16—H16A119.3C65—C66—C61120.4 (2)
C22—C21—C26118.0 (2)C65—C66—H66A119.8
C22—C21—P1117.78 (16)C61—C66—H66A119.8
C26—C21—P1124.19 (18)H1B—B1—H2B113.8 (17)
C23—C22—C21121.4 (2)H1B—B1—N2108.0 (13)
C23—C22—H22A119.3H2B—B1—N2108.9 (12)
C21—C22—H22A119.3H1B—B1—N5108.5 (12)
C22—C23—C24119.9 (2)H2B—B1—N5107.4 (11)
C22—C23—H23A120.0N2—B1—N5110.19 (19)
C24—C23—H23A120.0C2S—C1S—H1S108.5 (12)
C25—C24—C23119.6 (2)C2S—C1S—H2S108.8 (12)
C25—C24—H24A120.2H1S—C1S—H2S109.6 (13)
C23—C24—H24A120.2C2S—C1S—H3S109.8 (12)
C24—C25—C26120.5 (2)H1S—C1S—H3S109.6 (14)
C24—C25—H25A119.7H2S—C1S—H3S110.6 (13)
C26—C25—H25A119.7N1S—C2S—C1S178.4 (3)
C25—C26—C21120.6 (2)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NC2075).

References

  • Bruker (1998). SHELXTL/PC Version 5.1. Bruker AXS Inc., Madison, Wisconsin, USA.
  • Huh, S., Kim, Y., Park, S., Park, T.-J. & Jun, M.-J. (1999). Acta Cryst. C55, 850–852.
  • Huh, S., Park, Y. J., Lough, A. J. & Jun, M.-J. (2000). Acta Cryst. C56, 416–417. [PubMed]
  • Nonius (1997). KappaCCD Server Software Version 3.11. Nonius BV, Delft, The Netherlands.
  • Otwinowski, Z. & Minor, W. (1997). Methods Enzymol.276, 307–326.
  • Sheldrick, G. M. (1997). SHELXS97 and SHELXL97 University of Göttingen, Germany.
  • Youm, K.-T., Huh, S., Kim, Y., Park, S. & Jun, M.-J. (2006). Bull. Korean Chem. Soc.27, 1521–1522.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography