Decacarbonyl-1κ3C,2κ3C,3κ4C-[μ-1-diphenyl­arsino-2-(diphenyl­phosphino)ethane-1:2κ2As:P]-triangulo-tri­ruthenium(0)

Shawkataly, O. bin; Chong, M.-L.; Fun, H.-K.; Didierjean, C.; Aubry, A.

doi:10.1107/S1600536805042327

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Decacarbonyl-1κ³C,2κ³C,3κ⁴C-[μ-1-diphenylarsino-2-(diphenylphosphino)ethane-1:2κ²As:P]-triangulo-triruthenium(0)

O. bin Shawkataly, M.-L. Chong, H.-K. Fun, C. Didierjean and A. Aubry

The title compound, [Ru₃(C₂₆H₂₄AsP)(CO)₁₀], contains a triangle of bonded Ru atoms. The Ph₂P(CH₂)₂AsPh₂ ligand bridges an Ru—Ru bond, occupying equatorial positions on adjacent Ru atoms. There is disorder of the As and P atoms.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805042327/lh6571sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805042327/lh6571Isup2.hkl Contains datablock I

CCDC reference: 296615

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.008 Å
Disorder in main residue
R factor = 0.038
wR factor = 0.075
Data-to-parameter ratio = 18.0

checkCIF/PLATON results

No syntax errors found



Alert level C
GOODF01_ALERT_2_C  The least squares goodness of fit parameter lies
            outside the range 0.80 <> 2.00
            Goodness of fit given =      0.797
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct...          4
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.59 Ratio
PLAT301_ALERT_3_C Main Residue  Disorder .........................       4.00 Perc.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C11    -   C12    ...       1.36 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C17    -   C18    ...       1.39 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C17    -   C22    ...       1.37 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C25    -   C26    ...       1.36 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C25    -   C30    ...       1.37 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C31    -   C32    ...       1.38 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C31    -   C36    ...       1.38 Ang.
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     AS1/P1
                    RU1    AS1/P1
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     P2/AS2
                    RU2    P2/AS2
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     AS1/P1
                    AS1/P1 C17
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     AS1/P1
                    AS1/P1 C11
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     AS1/P1
                    AS1/P1 C23
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     P2/AS2
                    P2/AS2 C31
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     P2/AS2
                    P2/AS2 C25
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........     P2/AS2
                    P2/AS2 C24
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........     AS1/P1
                    AS1/P1 RU1    RU2
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........     P2/AS2
                    P2/AS2 RU2    RU1
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........     AS1/P1
                    C23    AS1/P1 RU1
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........     P2/AS2
                    C24    P2/AS2 RU2

Alert level G
ABSTY01_ALERT_1_G  Extra text has been found in the _exptl_absorpt_correction_type
            field, which should be only a single keyword. A literature
            citation should be included in the _exptl_absorpt_process_details
            field.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  24 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

  14 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   9 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

There have been extensive synthetic studies on mixed-ligand triruthenium cluster carbonyls (Bruce et al., 1983, 1989). In particular, mixed-ligand cluster carbonyls with group 15 donor atom ligands are of special interest because of their catalytic activity. However, structure determinations of triruthenium clusters containing mixed group 15 ligands are rare. As part of our study of substitution of transition metal carbonyl clusters with mixed ligand complexes, we have published several structures of triruthenium carbonyl clusters containing mixed P and As (Shawkataly et al., 1998) and P and Sb ligands (Shawkataly et al., 2004).

The structure of the title compound is similar to that of Ru₃(CO)₁₀[Ph₂P(CH₂)₂PPh₂ (Bruce et al., 1982). The crystal structure of the discrete cluster (Fig. 1) reveals the presence of the triangulo Ru₃ framework found in similar species. The Ph₂P(CH₂)₂AsPh₂ ligand bridges an Ru—Ru bond [2.8532 (6) Å], occupying equatorial sites on adjacent Ru atoms. The non-bridged Ru—Ru bonds are 2.8512 (6) and 2.8331 (6) Å. Positional disorder of the As and P atoms causes their positions to overlap. Similar disorder involving P and As atoms is also present in the crystal structures of Ph₂P(CH₂)₂AsPh₂ (Shawkataly et al., 2005) and Ru₃(CO)₈[Ph₂As(CH₂)₂AsPh₂][Ph₂P(CH₂) ₂PPh₂] (Shawkataly et al., 1998). The P—C, As—C, Ru—C, C—O and C—C bond lengths are typical of these type of organometallic compounds (Cambridge Structural Database; Allen, 2002).

Experimental top

The title compound was synthesized from a mixture of Ru₃(CO)₁₂ and Ph₂P(CH₂)₂AsPh₂ (1:1 ratio) in dry tetrahydrofuran under N₂ with a catalytic amount of diphenylketyl radical (Bruce et al., 1983). The product was purified by thin layer chromatography. Single crystals of the title compound were obtained by solvent diffusion from dichloromethene and methanol.

Computing details top

Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: OTREP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. The molecular structure of (I), showing displacement ellipsoids at the 25% probability level. H atoms have been omitted.

Decacarbonyl-1κ³C,2κ³C,3κ⁴C-[µ-1-diphenylarsino-2- (diphenylphosphino)ethane-1:2κ²As:P]-triangulo-triruthenium(0) top

Crystal data top

[Ru₃(C₂₆H₂₄AsP)(CO)₁₀]	F(000) = 2000
M_r = 1025.65	D_x = 1.832 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 49 reflections
a = 12.7117 (11) Å	θ = 6.7–24.9°
b = 14.3888 (11) Å	µ = 2.19 mm⁻¹
c = 20.4384 (11) Å	T = 293 K
β = 96.026 (5)°	Prism, dark red
V = 3717.7 (5) Å³	0.44 × 0.14 × 0.1 mm
Z = 4

Data collection top

Siemens P4 diffractometer	R_int = 0.042
ω/2θ scans	θ_max = 27.5°, θ_min = 1.6°
Absorption correction: empirical (using intensity measurements) via ψ scans (XSCANS; Siemens, 1994)	h = −1→16
T_min = 0.701, T_max = 0.807	k = −1→18
10420 measured reflections	l = −26→26
8514 independent reflections	3 standard reflections every 60 min
4541 reflections with I > 2σ(I)	intensity decay: 0.3%

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.039	w = 1/[σ²(F_o²) + (0.0098P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.075	(Δ/σ)_max = 0.002
S = 0.80	Δρ_max = 0.40 e Å⁻³
8514 reflections	Δρ_min = −0.43 e Å⁻³
472 parameters

Crystal data top

[Ru₃(C₂₆H₂₄AsP)(CO)₁₀]	V = 3717.7 (5) Å³
M_r = 1025.65	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 12.7117 (11) Å	µ = 2.19 mm⁻¹
b = 14.3888 (11) Å	T = 293 K
c = 20.4384 (11) Å	0.44 × 0.14 × 0.1 mm
β = 96.026 (5)°

Data collection top

Siemens P4 diffractometer	4541 reflections with I > 2σ(I)
Absorption correction: empirical (using intensity measurements) via ψ scans (XSCANS; Siemens, 1994)	R_int = 0.042
T_min = 0.701, T_max = 0.807	3 standard reflections every 60 min
10420 measured reflections	intensity decay: 0.3%
8514 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	0 restraints
wR(F²) = 0.075	H atoms treated by a mixture of independent and constrained refinement
S = 0.80	Δρ_max = 0.40 e Å⁻³
8514 reflections	Δρ_min = −0.43 e Å⁻³
472 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ru3	0.77656 (4)	0.27904 (3)	−0.06363 (2)	0.05082 (13)
Ru1	0.64258 (3)	0.28985 (3)	0.038476 (18)	0.03548 (10)
Ru2	0.81618 (3)	0.16313 (3)	0.049417 (19)	0.03925 (11)
As1	0.59113 (6)	0.28870 (5)	0.14687 (3)	0.03477 (17)	0.5
P1	0.59113 (6)	0.28870 (5)	0.14687 (3)	0.03477 (17)	0.5
P2	0.77651 (6)	0.06985 (5)	0.13978 (3)	0.03303 (17)	0.5
As2	0.77651 (6)	0.06985 (5)	0.13978 (3)	0.03303 (17)	0.5
O1	0.9703 (4)	0.3788 (4)	0.0052 (2)	0.0942 (16)
O2	0.9090 (4)	0.1996 (4)	−0.1657 (2)	0.1026 (18)
O3	0.5880 (3)	0.1666 (4)	−0.12786 (19)	0.0877 (15)
O4	0.6865 (4)	0.4565 (4)	−0.1271 (3)	0.120 (2)
O5	0.7613 (3)	0.4738 (3)	0.0658 (2)	0.0718 (12)
O6	0.4573 (3)	0.3989 (3)	−0.0274 (2)	0.0730 (13)
O7	0.5335 (3)	0.1011 (3)	0.01342 (18)	0.0587 (11)
O8	0.8971 (3)	0.3182 (3)	0.14382 (19)	0.0703 (12)
O9	1.0402 (4)	0.0997 (4)	0.0392 (2)	0.0982 (17)
O10	0.7307 (4)	0.0078 (3)	−0.04530 (19)	0.0769 (13)
C1	0.8958 (5)	0.3419 (5)	−0.0164 (3)	0.0652 (17)
C2	0.8636 (5)	0.2283 (5)	−0.1259 (3)	0.0677 (19)
C3	0.6573 (5)	0.2073 (5)	−0.0988 (3)	0.0632 (17)
C4	0.7183 (5)	0.3885 (5)	−0.1054 (3)	0.074 (2)
C5	0.7221 (4)	0.4036 (4)	0.0550 (2)	0.0478 (13)
C6	0.5282 (4)	0.3584 (3)	−0.0025 (2)	0.0436 (13)
C7	0.5801 (4)	0.1686 (4)	0.0218 (2)	0.0416 (12)
C8	0.8622 (4)	0.2639 (4)	0.1065 (3)	0.0505 (14)
C9	0.9545 (5)	0.1218 (4)	0.0427 (3)	0.0588 (16)
C10	0.7586 (4)	0.0674 (4)	−0.0112 (2)	0.0513 (14)
C11	0.4441 (4)	0.2793 (3)	0.1534 (2)	0.0403 (12)
C12	0.3747 (4)	0.2534 (4)	0.1012 (3)	0.0517 (14)
H12	0.4	0.236	0.0619	0.062*
C13	0.2657 (5)	0.2528 (4)	0.1062 (3)	0.0677 (18)
H13	0.2193	0.2352	0.0701	0.081*
C14	0.2266 (5)	0.2778 (4)	0.1635 (3)	0.0629 (16)
H14	0.1541	0.2779	0.1664	0.075*
C15	0.2957 (5)	0.3026 (4)	0.2163 (3)	0.0614 (16)
H15	0.2697	0.3191	0.2556	0.074*
C16	0.4040 (4)	0.3036 (3)	0.2125 (2)	0.0458 (13)
H16	0.45	0.3203	0.249	0.055*
C17	0.6227 (4)	0.3981 (3)	0.1938 (2)	0.0409 (12)
C18	0.5615 (5)	0.4767 (4)	0.1777 (3)	0.0704 (18)
H18	0.5067	0.4739	0.1438	0.084*
C19	0.5818 (6)	0.5583 (4)	0.2116 (4)	0.095 (3)
H19	0.5417	0.6109	0.1998	0.114*
C20	0.6591 (7)	0.5626 (5)	0.2617 (4)	0.097 (3)
H20	0.6688	0.6171	0.286	0.116*
C21	0.7245 (7)	0.4873 (5)	0.2776 (3)	0.091 (2)
H21	0.7795	0.4912	0.3113	0.109*
C22	0.7059 (5)	0.4055 (4)	0.2417 (3)	0.0618 (17)
H22	0.7509	0.3551	0.2505	0.074*
C23	0.6509 (5)	0.1974 (4)	0.2063 (2)	0.0409 (13)
C24	0.6497 (4)	0.0978 (3)	0.1792 (2)	0.0377 (12)
C25	0.7606 (4)	−0.0584 (3)	0.1210 (2)	0.0376 (12)
C26	0.6646 (4)	−0.1005 (4)	0.1106 (3)	0.0546 (15)
H26	0.6032	−0.0663	0.1131	0.065*
C27	0.6585 (5)	−0.1947 (4)	0.0960 (3)	0.0653 (18)
H27	0.5925	−0.2231	0.0899	0.078*
C28	0.7460 (5)	−0.2461 (4)	0.0905 (3)	0.0616 (17)
H28	0.7406	−0.309	0.0802	0.074*
C29	0.8413 (5)	−0.2046 (4)	0.1003 (3)	0.079 (2)
H29	0.9023	−0.239	0.0964	0.095*
C30	0.8493 (5)	−0.1106 (4)	0.1162 (3)	0.073 (2)
H30	0.9157	−0.0831	0.1236	0.088*
C31	0.8781 (4)	0.0669 (3)	0.2143 (2)	0.0407 (12)
C32	0.9734 (4)	0.1132 (4)	0.2159 (3)	0.0539 (15)
H32	0.9875	0.1483	0.1797	0.065*
C33	1.0480 (5)	0.1088 (5)	0.2697 (3)	0.0753 (19)
H33	1.1115	0.1409	0.2697	0.09*
C34	1.0282 (5)	0.0570 (4)	0.3232 (3)	0.0711 (19)
H34	1.0784	0.0533	0.3596	0.085*
C35	0.9335 (5)	0.0102 (4)	0.3230 (3)	0.0640 (17)
H35	0.9194	−0.0247	0.3593	0.077*
C36	0.8602 (4)	0.0154 (4)	0.2687 (2)	0.0517 (14)
H36	0.7967	−0.0167	0.2688	0.062*
H24A	0.590 (4)	0.089 (3)	0.144 (2)	0.062*
H23A	0.610 (4)	0.204 (4)	0.239 (2)	0.062*
H24B	0.650 (4)	0.050 (3)	0.211 (2)	0.062*
H23B	0.723 (4)	0.212 (4)	0.222 (2)	0.062*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru3	0.0407 (3)	0.0674 (3)	0.0449 (2)	0.0011 (3)	0.00710 (19)	0.0147 (2)
Ru1	0.0361 (2)	0.0300 (2)	0.0400 (2)	0.0011 (2)	0.00198 (17)	0.00036 (19)
Ru2	0.0362 (2)	0.0377 (2)	0.0440 (2)	0.0039 (2)	0.00499 (18)	0.0019 (2)
As1	0.0367 (4)	0.0282 (4)	0.0391 (4)	0.0032 (4)	0.0022 (3)	−0.0027 (3)
P1	0.0367 (4)	0.0282 (4)	0.0391 (4)	0.0032 (4)	0.0022 (3)	−0.0027 (3)
P2	0.0305 (4)	0.0263 (4)	0.0418 (4)	0.0014 (3)	0.0019 (3)	0.0000 (3)
As2	0.0305 (4)	0.0263 (4)	0.0418 (4)	0.0014 (3)	0.0019 (3)	0.0000 (3)
O1	0.075 (4)	0.113 (4)	0.094 (3)	−0.042 (3)	0.003 (3)	0.002 (3)
O2	0.057 (3)	0.164 (5)	0.090 (3)	−0.014 (3)	0.022 (3)	−0.045 (4)
O3	0.052 (3)	0.143 (5)	0.068 (3)	−0.012 (3)	0.010 (2)	−0.003 (3)
O4	0.098 (4)	0.124 (5)	0.139 (4)	0.039 (4)	0.026 (3)	0.076 (4)
O5	0.071 (3)	0.043 (2)	0.098 (3)	−0.015 (2)	−0.006 (2)	−0.004 (2)
O6	0.065 (3)	0.049 (2)	0.098 (3)	0.009 (2)	−0.028 (2)	0.008 (2)
O7	0.063 (3)	0.038 (2)	0.075 (3)	−0.010 (2)	0.006 (2)	−0.012 (2)
O8	0.080 (3)	0.050 (2)	0.076 (3)	−0.009 (2)	−0.015 (2)	−0.004 (2)
O9	0.046 (3)	0.119 (4)	0.131 (4)	0.020 (3)	0.020 (3)	−0.011 (3)
O10	0.091 (3)	0.065 (3)	0.071 (3)	0.005 (3)	−0.007 (2)	−0.026 (2)
C1	0.062 (4)	0.080 (5)	0.056 (4)	−0.004 (4)	0.020 (3)	0.015 (4)
C2	0.039 (3)	0.109 (6)	0.054 (4)	−0.011 (4)	−0.002 (3)	−0.004 (4)
C3	0.041 (3)	0.091 (5)	0.057 (3)	0.005 (4)	0.008 (3)	0.015 (4)
C4	0.059 (4)	0.094 (5)	0.069 (4)	0.013 (4)	0.012 (3)	0.029 (4)
C5	0.043 (3)	0.048 (3)	0.051 (3)	−0.001 (3)	−0.002 (3)	0.005 (3)
C6	0.043 (3)	0.033 (3)	0.053 (3)	−0.006 (3)	−0.001 (3)	0.005 (2)
C7	0.038 (3)	0.049 (3)	0.038 (3)	0.007 (3)	0.003 (2)	−0.004 (3)
C8	0.051 (4)	0.045 (3)	0.054 (3)	0.001 (3)	0.002 (3)	0.009 (3)
C9	0.046 (4)	0.054 (4)	0.077 (4)	0.000 (3)	0.008 (3)	−0.005 (3)
C10	0.050 (3)	0.055 (4)	0.048 (3)	0.015 (3)	0.000 (3)	0.001 (3)
C11	0.035 (3)	0.032 (3)	0.053 (3)	0.002 (3)	0.001 (2)	0.010 (3)
C12	0.043 (3)	0.059 (4)	0.053 (3)	−0.003 (3)	0.004 (3)	0.002 (3)
C13	0.045 (4)	0.086 (5)	0.070 (4)	−0.011 (4)	−0.005 (3)	0.008 (4)
C14	0.046 (4)	0.051 (4)	0.095 (5)	0.002 (3)	0.020 (4)	0.013 (4)
C15	0.068 (4)	0.042 (4)	0.078 (4)	0.006 (3)	0.022 (3)	−0.002 (3)
C16	0.046 (3)	0.038 (3)	0.054 (3)	0.008 (3)	0.006 (3)	−0.004 (3)
C17	0.045 (3)	0.036 (3)	0.041 (3)	0.003 (3)	0.007 (2)	−0.002 (2)
C18	0.062 (4)	0.045 (4)	0.101 (5)	0.007 (3)	−0.004 (4)	−0.012 (4)
C19	0.091 (6)	0.038 (4)	0.157 (8)	0.006 (4)	0.024 (6)	−0.026 (5)
C20	0.126 (8)	0.052 (4)	0.117 (6)	−0.019 (5)	0.034 (6)	−0.041 (5)
C21	0.120 (7)	0.070 (5)	0.078 (5)	−0.029 (5)	−0.015 (5)	−0.020 (4)
C22	0.082 (5)	0.035 (3)	0.063 (4)	−0.004 (3)	−0.015 (3)	−0.002 (3)
C23	0.049 (3)	0.035 (3)	0.038 (3)	0.010 (3)	0.003 (2)	−0.004 (2)
C24	0.042 (3)	0.028 (3)	0.043 (3)	0.005 (2)	0.006 (2)	0.002 (2)
C25	0.037 (3)	0.031 (3)	0.042 (3)	0.008 (2)	−0.006 (2)	−0.002 (2)
C26	0.040 (3)	0.042 (3)	0.082 (4)	0.003 (3)	0.003 (3)	−0.013 (3)
C27	0.049 (4)	0.042 (4)	0.102 (5)	−0.009 (3)	−0.008 (3)	−0.021 (3)
C28	0.064 (4)	0.032 (3)	0.085 (4)	0.003 (3)	−0.012 (3)	−0.015 (3)
C29	0.052 (4)	0.043 (4)	0.142 (6)	0.005 (3)	0.006 (4)	−0.024 (4)
C30	0.038 (3)	0.043 (4)	0.139 (6)	−0.002 (3)	0.009 (4)	−0.025 (4)
C31	0.037 (3)	0.031 (3)	0.053 (3)	0.001 (2)	0.003 (2)	−0.004 (2)
C32	0.046 (4)	0.053 (4)	0.060 (3)	−0.005 (3)	−0.004 (3)	0.004 (3)
C33	0.048 (4)	0.083 (5)	0.089 (5)	−0.003 (4)	−0.017 (4)	0.010 (4)
C34	0.070 (5)	0.074 (5)	0.063 (4)	0.014 (4)	−0.024 (4)	−0.003 (4)
C35	0.072 (5)	0.057 (4)	0.061 (4)	0.009 (4)	−0.006 (4)	0.014 (3)
C36	0.051 (4)	0.050 (3)	0.052 (3)	0.000 (3)	−0.004 (3)	0.006 (3)

Geometric parameters (Å, º) top

Ru3—C4	1.904 (7)	C15—H15	0.93
Ru3—C3	1.911 (7)	C16—H16	0.93
Ru3—C2	1.916 (7)	C17—C22	1.368 (7)
Ru3—C1	1.935 (7)	C17—C18	1.392 (7)
Ru3—Ru1	2.8331 (6)	C18—C19	1.375 (8)
Ru3—Ru2	2.8512 (6)	C18—H18	0.93
Ru1—Ru2	2.8532 (6)	C19—C20	1.344 (9)
Ru1—C6	1.879 (5)	C19—H19	0.93
Ru1—C7	1.932 (6)	C20—C21	1.384 (10)
Ru1—C5	1.934 (6)	C20—H20	0.93
Ru1—As1/P1	2.3748 (8)	C21—C22	1.394 (8)
Ru2—C9	1.875 (6)	C21—H21	0.93
Ru2—C8	1.914 (6)	C22—H22	0.93
Ru2—C10	1.943 (6)	C23—C24	1.536 (7)
Ru2—P2/As2	2.3796 (8)	C23—H23A	0.89 (5)
As1/P1—C17	1.865 (5)	C23—H23B	0.96 (5)
As1/P1—C11	1.893 (5)	C24—H24A	0.99 (5)
As1/P1—C23	1.894 (5)	C24—H24B	0.95 (5)
P2/As2—C31	1.891 (5)	C25—C26	1.359 (7)
P2/As2—C25	1.892 (5)	C25—C30	1.367 (7)
P2/As2—C24	1.919 (5)	C26—C27	1.388 (7)
O1—C1	1.133 (7)	C26—H26	0.93
O2—C2	1.126 (6)	C27—C28	1.350 (8)
O3—C3	1.167 (7)	C27—H27	0.93
O4—C4	1.131 (7)	C28—C29	1.346 (8)
O5—C5	1.139 (6)	C28—H28	0.93
O6—C6	1.147 (5)	C29—C30	1.393 (7)
O7—C7	1.142 (6)	C29—H29	0.93
O8—C8	1.148 (6)	C30—H30	0.93
O9—C9	1.144 (6)	C31—C36	1.376 (6)
O10—C10	1.139 (6)	C31—C32	1.379 (7)
C11—C12	1.363 (6)	C32—C33	1.376 (7)
C11—C16	1.403 (7)	C32—H32	0.93
C12—C13	1.400 (7)	C33—C34	1.370 (8)
C12—H12	0.93	C33—H33	0.93
C13—C14	1.368 (8)	C34—C35	1.378 (8)
C13—H13	0.93	C34—H34	0.93
C14—C15	1.367 (7)	C35—C36	1.373 (6)
C14—H14	0.93	C35—H35	0.93
C15—C16	1.387 (7)	C36—H36	0.93

C4—Ru3—C3	91.3 (3)	C15—C14—C13	119.0 (6)
C4—Ru3—C2	104.0 (3)	C15—C14—H14	120.5
C3—Ru3—C2	92.0 (2)	C13—C14—H14	120.5
C4—Ru3—C1	94.8 (3)	C14—C15—C16	121.2 (6)
C3—Ru3—C1	171.8 (2)	C14—C15—H15	119.4
C2—Ru3—C1	91.9 (2)	C16—C15—H15	119.4
C4—Ru3—Ru1	92.80 (19)	C15—C16—C11	119.9 (5)
C3—Ru3—Ru1	78.04 (17)	C15—C16—H16	120.1
C2—Ru3—Ru1	160.7 (2)	C11—C16—H16	120.1
C1—Ru3—Ru1	96.12 (17)	C22—C17—C18	118.5 (5)
C4—Ru3—Ru2	150.96 (19)	C22—C17—As1	122.8 (4)
C3—Ru3—Ru2	93.14 (17)	C18—C17—As1	118.6 (4)
C2—Ru3—Ru2	104.47 (19)	C19—C18—C17	120.2 (6)
C1—Ru3—Ru2	78.84 (17)	C19—C18—H18	119.9
Ru1—Ru3—Ru2	60.258 (14)	C17—C18—H18	119.9
C6—Ru1—C7	96.4 (2)	C20—C19—C18	120.5 (7)
C6—Ru1—C5	90.0 (2)	C20—C19—H19	119.7
C7—Ru1—C5	172.8 (2)	C18—C19—H19	119.7
C6—Ru1—As1	98.23 (16)	C19—C20—C21	121.0 (7)
C7—Ru1—As1	90.60 (14)	C19—C20—H20	119.5
C5—Ru1—As1	91.93 (16)	C21—C20—H20	119.5
C6—Ru1—Ru3	101.39 (15)	C20—C21—C22	118.2 (6)
C7—Ru1—Ru3	95.03 (14)	C20—C21—H21	120.9
C5—Ru1—Ru3	80.27 (16)	C22—C21—H21	120.9
As1—Ru1—Ru3	158.83 (3)	C17—C22—C21	121.2 (6)
C6—Ru1—Ru2	157.83 (15)	C17—C22—H22	119.4
C7—Ru1—Ru2	74.75 (15)	C21—C22—H22	119.4
C5—Ru1—Ru2	98.10 (16)	C24—C23—As1	115.3 (3)
As1/P1—Ru1—Ru2	102.06 (2)	C24—C23—H23A	113 (3)
Ru3—Ru1—Ru2	60.186 (15)	As1—C23—H23A	100 (3)
C9—Ru2—C8	93.2 (2)	C24—C23—H23B	108 (3)
C9—Ru2—C10	91.3 (2)	As1—C23—H23B	111 (3)
C8—Ru2—C10	175.0 (2)	H23A—C23—H23B	110 (4)
C9—Ru2—P2	98.87 (18)	C23—C24—P2	111.7 (4)
C8—Ru2—P2	91.71 (15)	C23—C24—H24A	111 (3)
C10—Ru2—P2	89.91 (16)	P2—C24—H24A	106 (3)
C9—Ru2—Ru3	102.36 (18)	C23—C24—H24B	115 (3)
C8—Ru2—Ru3	93.90 (15)	P2—C24—H24B	101 (3)
C10—Ru2—Ru3	82.85 (15)	H24A—C24—H24B	110 (4)
P2—Ru2—Ru3	157.68 (3)	C26—C25—C30	118.5 (5)
C9—Ru2—Ru1	157.03 (18)	C26—C25—P2	122.8 (4)
C8—Ru2—Ru1	75.43 (16)	C30—C25—P2	118.6 (4)
C10—Ru2—Ru1	99.59 (16)	C25—C26—C27	119.9 (5)
P2/As2—Ru2—Ru1	101.31 (2)	C25—C26—H26	120.1
Ru3—Ru2—Ru1	59.556 (15)	C27—C26—H26	120.1
C17—As1—C11	100.6 (2)	C28—C27—C26	121.6 (6)
C17—As1—C23	101.9 (2)	C28—C27—H27	119.2
C11—As1—C23	103.8 (2)	C26—C27—H27	119.2
C17—As1—Ru1	114.11 (15)	C29—C28—C27	118.8 (5)
C11—As1—Ru1	115.92 (15)	C29—C28—H28	120.6
C23—As1/P1—Ru1	118.17 (16)	C27—C28—H28	120.6
C31—P2—C25	101.0 (2)	C28—C29—C30	120.5 (6)
C31—P2—C24	101.5 (2)	C28—C29—H29	119.7
C25—P2—C24	102.3 (2)	C30—C29—H29	119.7
C31—P2—Ru2	117.08 (16)	C25—C30—C29	120.6 (6)
C25—P2—Ru2	114.82 (14)	C25—C30—H30	119.7
C24—P2/As2—Ru2	117.59 (15)	C29—C30—H30	119.7
O1—C1—Ru3	172.8 (5)	C36—C31—C32	117.4 (5)
O2—C2—Ru3	175.1 (5)	C36—C31—P2	120.4 (4)
O3—C3—Ru3	171.6 (5)	C32—C31—P2	122.1 (4)
O4—C4—Ru3	175.9 (7)	C33—C32—C31	121.8 (5)
O5—C5—Ru1	174.3 (5)	C33—C32—H32	119.1
O6—C6—Ru1	178.8 (5)	C31—C32—H32	119.1
O7—C7—Ru1	172.8 (5)	C34—C33—C32	119.6 (6)
O8—C8—Ru2	173.2 (5)	C34—C33—H33	120.2
O9—C9—Ru2	177.5 (6)	C32—C33—H33	120.2
O10—C10—Ru2	175.4 (5)	C33—C34—C35	119.8 (6)
C12—C11—C16	118.6 (5)	C33—C34—H34	120.1
C12—C11—As1	121.8 (4)	C35—C34—H34	120.1
C16—C11—As1	119.6 (4)	C36—C35—C34	119.7 (6)
C11—C12—C13	120.6 (5)	C36—C35—H35	120.2
C11—C12—H12	119.7	C34—C35—H35	120.2
C13—C12—H12	119.7	C35—C36—C31	121.7 (5)
C14—C13—C12	120.8 (6)	C35—C36—H36	119.1
C14—C13—H13	119.6	C31—C36—H36	119.1
C12—C13—H13	119.6

C4—Ru3—Ru1—C6	24.7 (3)	C7—Ru1—As1—C23	63.9 (2)
C3—Ru3—Ru1—C6	−66.1 (2)	C5—Ru1—As1—C23	−109.4 (3)
C2—Ru3—Ru1—C6	−126.2 (5)	Ru3—Ru1—As1—C23	−41.8 (2)
C1—Ru3—Ru1—C6	119.8 (2)	Ru2—Ru1—As1—C23	−10.7 (2)
Ru2—Ru3—Ru1—C6	−166.75 (15)	C9—Ru2—P2—C31	48.3 (2)
C4—Ru3—Ru1—C7	122.2 (3)	C8—Ru2—P2—C31	−45.2 (2)
C3—Ru3—Ru1—C7	31.5 (2)	C10—Ru2—P2—C31	139.6 (2)
C2—Ru3—Ru1—C7	−28.7 (5)	Ru3—Ru2—P2—C31	−149.80 (17)
C1—Ru3—Ru1—C7	−142.6 (2)	Ru1—Ru2—P2—C31	−120.68 (16)
Ru2—Ru3—Ru1—C7	−69.21 (14)	C9—Ru2—P2—C25	−69.9 (2)
C4—Ru3—Ru1—C5	−63.3 (3)	C8—Ru2—P2—C25	−163.4 (2)
C3—Ru3—Ru1—C5	−154.1 (2)	C10—Ru2—P2—C25	21.4 (2)
C2—Ru3—Ru1—C5	145.8 (5)	Ru3—Ru2—P2—C25	92.00 (18)
C1—Ru3—Ru1—C5	31.8 (2)	Ru1—Ru2—P2—C25	121.13 (16)
Ru2—Ru3—Ru1—C5	105.26 (15)	C9—Ru2—P2—C24	169.7 (2)
C4—Ru3—Ru1—As1	−132.9 (2)	C8—Ru2—P2—C24	76.2 (2)
C3—Ru3—Ru1—As1	136.3 (2)	C10—Ru2—P2—C24	−99.1 (2)
C2—Ru3—Ru1—As1	76.2 (5)	Ru3—Ru2—P2—C24	−28.44 (19)
C1—Ru3—Ru1—As1	−37.8 (2)	Ru1—Ru2—P2—C24	0.68 (17)
Ru2—Ru3—Ru1—As1	35.64 (7)	C17—As1—C11—C12	138.2 (4)
C4—Ru3—Ru1—Ru2	−168.6 (2)	C23—As1—C11—C12	−116.6 (4)
C3—Ru3—Ru1—Ru2	100.68 (19)	Ru1—As1—C11—C12	14.6 (5)
C2—Ru3—Ru1—Ru2	40.5 (5)	C17—As1—C11—C16	−38.9 (4)
C1—Ru3—Ru1—Ru2	−73.41 (19)	C23—As1—C11—C16	66.3 (4)
C4—Ru3—Ru2—C9	−140.7 (5)	Ru1—As1—C11—C16	−162.5 (3)
C3—Ru3—Ru2—C9	121.0 (3)	C16—C11—C12—C13	1.2 (8)
C2—Ru3—Ru2—C9	28.1 (3)	As1—C11—C12—C13	−175.9 (5)
C1—Ru3—Ru2—C9	−60.9 (3)	C11—C12—C13—C14	−0.3 (10)
Ru1—Ru3—Ru2—C9	−164.70 (18)	C12—C13—C14—C15	−0.7 (9)
C4—Ru3—Ru2—C8	−46.5 (5)	C13—C14—C15—C16	0.6 (9)
C3—Ru3—Ru2—C8	−144.9 (2)	C14—C15—C16—C11	0.4 (9)
C2—Ru3—Ru2—C8	122.2 (3)	C12—C11—C16—C15	−1.3 (8)
C1—Ru3—Ru2—C8	33.2 (3)	As1—C11—C16—C15	175.9 (4)
Ru1—Ru3—Ru2—C8	−70.57 (17)	C11—As1—C17—C22	131.8 (5)
C4—Ru3—Ru2—C10	129.6 (5)	C23—As1—C17—C22	25.1 (5)
C3—Ru3—Ru2—C10	31.3 (2)	Ru1—As1—C17—C22	−103.4 (4)
C2—Ru3—Ru2—C10	−61.6 (2)	C11—As1—C17—C18	−50.8 (5)
C1—Ru3—Ru2—C10	−150.7 (3)	C23—As1—C17—C18	−157.5 (5)
Ru1—Ru3—Ru2—C10	105.57 (17)	Ru1—As1—C17—C18	74.0 (5)
C4—Ru3—Ru2—P2	57.6 (4)	C22—C17—C18—C19	−3.1 (9)
C3—Ru3—Ru2—P2	−40.71 (19)	As1—C17—C18—C19	179.4 (5)
C2—Ru3—Ru2—P2	−133.57 (19)	C17—C18—C19—C20	−1.6 (12)
C1—Ru3—Ru2—P2	137.4 (2)	C18—C19—C20—C21	4.2 (13)
Ru1—Ru3—Ru2—P2	33.61 (7)	C19—C20—C21—C22	−2.1 (12)
C4—Ru3—Ru2—Ru1	24.0 (4)	C18—C17—C22—C21	5.2 (9)
C3—Ru3—Ru2—Ru1	−74.32 (18)	As1—C17—C22—C21	−177.4 (5)
C2—Ru3—Ru2—Ru1	−167.18 (18)	C20—C21—C22—C17	−2.7 (11)
C1—Ru3—Ru2—Ru1	103.76 (19)	C17—As1—C23—C24	−173.3 (4)
C6—Ru1—Ru2—C9	77.9 (6)	C11—As1—C23—C24	82.5 (4)
C7—Ru1—Ru2—C9	146.5 (5)	Ru1—As1—C23—C24	−47.4 (5)
C5—Ru1—Ru2—C9	−32.5 (5)	As1—C23—C24—P2	91.1 (4)
As1—Ru1—Ru2—C9	−126.2 (4)	C31—P2—C24—C23	69.1 (4)
Ru3—Ru1—Ru2—C9	41.3 (4)	C25—P2—C24—C23	173.2 (3)
C6—Ru1—Ru2—C8	140.1 (4)	Ru2—P2—C24—C23	−60.0 (4)
C7—Ru1—Ru2—C8	−151.3 (2)	C31—P2—C25—C26	130.8 (4)
C5—Ru1—Ru2—C8	29.7 (2)	C24—P2—C25—C26	26.3 (5)
As1—Ru1—Ru2—C8	−64.02 (16)	Ru2—P2—C25—C26	−102.3 (4)
Ru3—Ru1—Ru2—C8	103.55 (16)	C31—P2—C25—C30	−50.8 (5)
C6—Ru1—Ru2—C10	−39.2 (4)	C24—P2—C25—C30	−155.3 (5)
C7—Ru1—Ru2—C10	29.4 (2)	Ru2—P2—C25—C30	76.1 (5)
C5—Ru1—Ru2—C10	−149.6 (2)	C30—C25—C26—C27	0.6 (8)
As1—Ru1—Ru2—C10	116.65 (16)	P2—C25—C26—C27	179.0 (4)
Ru3—Ru1—Ru2—C10	−75.77 (16)	C25—C26—C27—C28	−1.4 (9)
C6—Ru1—Ru2—P2	−131.1 (4)	C26—C27—C28—C29	0.9 (10)
C7—Ru1—Ru2—P2	−62.49 (14)	C27—C28—C29—C30	0.4 (10)
C5—Ru1—Ru2—P2	118.54 (15)	C26—C25—C30—C29	0.6 (9)
As1—Ru1—Ru2—P2	24.81 (3)	P2—C25—C30—C29	−177.8 (5)
Ru3—Ru1—Ru2—P2	−167.62 (3)	C28—C29—C30—C25	−1.2 (11)
C6—Ru1—Ru2—Ru3	36.6 (4)	C25—P2—C31—C36	−55.4 (4)
C7—Ru1—Ru2—Ru3	105.13 (14)	C24—P2—C31—C36	49.8 (4)
C5—Ru1—Ru2—Ru3	−73.84 (15)	Ru2—P2—C31—C36	179.2 (3)
As1—Ru1—Ru2—Ru3	−167.57 (3)	C25—P2—C31—C32	122.7 (4)
C6—Ru1—As1—C17	−79.9 (2)	C24—P2—C31—C32	−132.1 (4)
C7—Ru1—As1—C17	−176.5 (2)	Ru2—P2—C31—C32	−2.7 (5)
C5—Ru1—As1—C17	10.3 (2)	C36—C31—C32—C33	−0.2 (8)
Ru3—Ru1—As1—C17	77.89 (19)	P2—C31—C32—C33	−178.3 (5)
Ru2—Ru1—As1—C17	109.02 (18)	C31—C32—C33—C34	0.3 (9)
C6—Ru1—As1—C11	36.3 (2)	C32—C33—C34—C35	−0.4 (10)
C7—Ru1—As1—C11	−60.2 (2)	C33—C34—C35—C36	0.5 (9)
C5—Ru1—As1—C11	126.6 (2)	C34—C35—C36—C31	−0.5 (9)
Ru3—Ru1—As1—C11	−165.87 (16)	C32—C31—C36—C35	0.3 (8)
Ru2—Ru1—As1—C11	−134.74 (17)	P2—C31—C36—C35	178.5 (4)
C6—Ru1—As1—C23	160.4 (2)

Experimental details

Crystal data
Chemical formula	[Ru₃(C₂₆H₂₄AsP)(CO)₁₀]
M_r	1025.65
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	12.7117 (11), 14.3888 (11), 20.4384 (11)
β (°)	96.026 (5)
V (Å³)	3717.7 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.19
Crystal size (mm)	0.44 × 0.14 × 0.1

Data collection
Diffractometer	Siemens P4 diffractometer
Absorption correction	Empirical (using intensity measurements) via ψ scans (XSCANS; Siemens, 1994)
T_min, T_max	0.701, 0.807
No. of measured, independent and observed [I > 2σ(I)] reflections	10420, 8514, 4541
R_int	0.042
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.075, 0.80
No. of reflections	8514
No. of parameters	472
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.40, −0.43

Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXS86 (Sheldrick, 1985), SHELXL97 (Sheldrick, 1997), OTREP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top

Ru3—Ru1	2.8331 (6)	As1/P1—C11	1.893 (5)
Ru3—Ru2	2.8512 (6)	As1/P1—C23	1.894 (5)
Ru1—Ru2	2.8532 (6)	P2/As2—C31	1.891 (5)
Ru1—As1/P1	2.3748 (8)	P2/As2—C25	1.892 (5)
Ru2—P2/As2	2.3796 (8)	P2/As2—C24	1.919 (5)
As1/P1—C17	1.865 (5)	C23—C24	1.536 (7)

As1/P1—Ru1—Ru2	102.06 (2)	C23—As1/P1—Ru1	118.17 (16)
P2/As2—Ru2—Ru1	101.31 (2)	C24—P2/As2—Ru2	117.59 (15)

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