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The crystal structure of the heterobimetallic title compound, [ReRuCl(C10H16As2)2(C10H8N2)2(CO)3](PF6)2·2C3H6O, is described. Both metal centres have pseudo-octahedral coordination geometries, with a facial arrangement of the carbonyl ligands at ReI and a trans disposition of the diarsine ligands at RuII. The dihedral angle between the pyridyl rings of the 4,4′-bi­pyridine bridging ligand is 13.9 (6)°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100008076/gg1004sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100008076/gg1004Isup2.hkl
Contains datablock I

CCDC reference: 150324

Comment top

There is currently great interest in ligand-bridged, di- and polynuclear transition metal complexes. Such compounds are of fundamental importance for the study of intermetallic electronic interactions (Creutz, 1983; Nelsen, 2000), and may also find practical applications in the emerging field of molecular electronics, as components of molecular-scale wires or switches (Crutchley, 1994; Ward, 1995).

We have previously reported a series of symmetrical, dinuclear complexes containing trans-[RuIICl(pdma)2]+ [pdma = 1,2-phenylenebis(dimethylarsine)] centres (Coe et al., 1997), and here describe the synthesis and structure of a related hetero-dinuclear complex salt, (I), containing a fac-[ReI(2,2'-bpy)(CO)3]+ (2,2'-bpy = 2,2'-bipyridine) moiety. Such rhenium(I) α-diimine centres are of interest for their photoexcitation properties (Schanze et al., 1993). A recent report of particular relevance to the present study described photoinduced electron-transfer in the trinuclear complex fac, trans-[ReI(dmb)(CO)3] (µ-4,4'-bpy)RuIII(en)2(µ-NC)FeIII(CN)5]+ (dmb = 4,4'-dimethyl-2,2'-bipyridine, 4,4'-bpy = 4,4'-bipyridine, en = 1,2-diaminoethane) (Pfennig et al., 1998). To our knowledge, (I) contains the first hetero-dinuclear transition metal complex featuring a 4,4'-bpy bridging ligand to be structurally characterized. The only other related complex, [CdII(4,4'-bpy)2{AgI(CN)2}2], has an interpenetrating double framework structure containing 4,4'-bpy bridges between cadmium(II) and silver(I) ions (Soma et al., 1994). \sch

Complex (I) was synthesized by the reaction of trans-[RuIICl(pdma)2(4,4'-bpy)]PF6 (Coe et al., 1997) with fac-ReI(CF3SO3)(2,2'-bpy)(CO)3 (Sullivan & Meyer, 1984). The intense dπ(RuII) π*(4,4'-bpy) metal-to-ligand charge-transfer absorption band of trans-[RuIICl(pdma)2(4,4'-bpy)]PF6 (λmax = 418 nm in acetonitrile; Coe et al., 1997) undergoes a red-shift of ca 0.2 eV upon coordination of the fac-ReI(2,2'-bpy)(CO)3 group to afford (I). However, the RuIII/II E1/2 potentials obtained from cyclic voltammetry for (I) and for trans-[RuIICl(pdma)2(4,4'-bpy)]PF6 are identical (1.09 V versus the saturated calomel electrode in acetonitrile). There is thus minimal electronic communication between the two metal centres in (I).

The molecular structure of the complex in (I) is as indicated by 1NMR spectroscopy, with both metal centres having pseudo-octahedral coordination geometries, a facial arrangement of the carbonyl ligands at rhenium(I) and a trans disposition of the diarsine ligands at ruthenium(II). The metal centres are almost perfectly eclipsed with respect to each other, and their geometrical parameters are similar to those found previously in fac-[{ReI(2,2'-bpy)(CO)3}2(µ-bpa)] (BPh4)2·2C4H10O [bpa = 1,2-bis(4-pyridyl)ethane] (Lin et al., 1992) and in other trans-{RuIICl(pdma)2}+ complexes (Coe et al., 1997). Also as observed in related structures (Coe et al., 1997), the Ru-coordinated ring of the 4,4'-bpy ligand approximately bisects the As–Ru–As chelate angles. The dihedral angle between the rings of the 4,4'-bpy bridging ligand in (I) is 13.9 (6)° (ring planes defined by N1/C21/C22/C23/C24/C25 and N2/C26/C27/C28/C29/C30), a little larger than the corresponding angle in the mononuclear precursor trans-[RuIICl(pdma)2(4,4'-bpy)]PF6 (10.27 (5)°) (Coe et al., 2000). The close similarity of these dihedral angles is consistent with the lack of intermetallic (π) electronic coupling in (I) shown by cyclic voltammetry (see above). The structure of (I) contains no classical hydrogen bonds, but the following close contacts are worthy of note: C25—H25···O5, C···O 3.080 (17) Å and C38—H38···O1, C···O 3.22 (2) Å (symmetry code: 1 − x, 1 − y, −0.5 + z).

Experimental top

A solution of fac-[Re(CO)3(2,2'-bpy)(CF3SO3)] (13 mg, 0.023 mmol) and trans-[RuCl(pdma)2(4,4'-bpy)]PF6 (20 mg, 0.020 mmol) in 2-butanone (10 cm3) was heated at reflux in the dark under Ar for 5 h. Addition of aqueous NH4PF6 produced an orange precipitate, which was filtered off, washed with water and dried. Reprecipitation from acetone/diethyl ether, followed by several recrystallizations from acetonitrile/diethyl ether afforded a red crystalline solid [yield 7 mg (22%)]. Found: C 32.54, H 3.07, N 3.29. Calculated for C43H48As4ClF12N4O3P2ReRu: C 32.66, H 3.06, N 3.54%. 1H NMR data (200 MHz, CD3COCD3): δ 9.43 (2H, d, J = 4.8 Hz, H6,6'), 8.67 (2H, d, J = 8.2 Hz, H3,3'), 8.58 (2H, d, J = 6.8 Hz, C5H4N), 8.42 (2H, t, H4,4'), 8.29 (4H, m, 2C6H2), 7.95 (2H, t, H5,5'), 7.83 (4H, m, 2C6H2), 7.76 (2H, d, J = 6.9 Hz, C5H4N), 7.68 (2H, d, J = 6.8 Hz, C5H4N), 7.41 (2H, d, J = 6.9 Hz, C5H4N), 1.88 (12H, s, 4 x AsMe), 1.74 (12H, s, 4 x AsMe). i.r. υ(CO) (KBr disc) 2033, 1926 cm−1. Crystals suitable for single-crystal X-ray diffraction measurements were obtained by slow diffusion of diethyl ether vapour into a solution of (I) in acetone at 277 K.

Refinement top

Geometrical and thermal restraints were applied to the two PF6 anions in order to accurately model the disorder present, whilst the absolute structure configuration was tested using the Flack parameter (Flack, 1983).

Computing details top

Data collection: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998); cell refinement: DENZO and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1990).

Figures top
[Figure 1] Fig. 1. View of the complex cation in (I), with H atoms omitted (50% probability displacement ellipsoids).
(I) top
Crystal data top
[ReRuCl(C10H16As2)2(C10H8N2)2(CO)3](PF6)2·2C3H6OF(000) = 3312
Mr = 1697.35Dx = 1.838 Mg m3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2nCell parameters from 15874 reflections
a = 22.736 (5) Åθ = 1.1–25°
b = 30.654 (6) ŵ = 4.54 mm1
c = 8.799 (2) ÅT = 150 K
V = 6132 (2) Å3Plate, orange
Z = 40.45 × 0.08 × 0.02 mm
Data collection top
Nonius KappaCCD
diffractometer
6157 reflections with I > 2σ(I)
Radiation source: Nonius FR591 rotating anodeRint = 0.109
ϕ and ω scansθmax = 25°, θmin = 1.1°
Absorption correction: multi-scans
(SORTAV; Blessing, 1995)
h = 1427
Tmin = 0.235, Tmax = 0.915k = 3636
15874 measured reflectionsl = 89
7883 independent reflections
Refinement top
Refinement on F2H-atom parameters constrained
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0546P)2], P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.051(Δ/σ)max = 0.006
wR(F2) = 0.115Δρmax = 1.55 e Å3
S = 0.99Δρmin = 1.16 e Å3
7883 reflectionsAbsolute structure: Flack (1983)
852 parametersAbsolute structure parameter: 0.066 (10)
308 restraints
Crystal data top
[ReRuCl(C10H16As2)2(C10H8N2)2(CO)3](PF6)2·2C3H6OV = 6132 (2) Å3
Mr = 1697.35Z = 4
Orthorhombic, Pna21Mo Kα radiation
a = 22.736 (5) ŵ = 4.54 mm1
b = 30.654 (6) ÅT = 150 K
c = 8.799 (2) Å0.45 × 0.08 × 0.02 mm
Data collection top
Nonius KappaCCD
diffractometer
7883 independent reflections
Absorption correction: multi-scans
(SORTAV; Blessing, 1995)
6157 reflections with I > 2σ(I)
Tmin = 0.235, Tmax = 0.915Rint = 0.109
15874 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.051H-atom parameters constrained
wR(F2) = 0.115Δρmax = 1.55 e Å3
S = 0.99Δρmin = 1.16 e Å3
7883 reflectionsAbsolute structure: Flack (1983)
852 parametersAbsolute structure parameter: 0.066 (10)
308 restraints
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
xyzUiso*/UeqOcc. (<1)
Re10.54544 (2)0.632662 (16)0.88929 (7)0.03053 (15)
Ru10.88113 (5)0.61175 (3)0.06056 (10)0.0226 (2)
As10.94020 (6)0.55697 (4)0.06469 (13)0.0247 (3)
As20.83271 (6)0.55013 (4)0.17887 (13)0.0250 (3)
As30.82761 (6)0.66561 (4)0.20670 (14)0.0312 (4)
As40.93459 (6)0.67408 (5)0.03777 (15)0.0301 (3)
Cl10.95169 (15)0.60767 (12)0.2666 (4)0.0389 (9)
O10.6277 (5)0.5739 (4)1.0782 (11)0.053 (3)
O20.6183 (5)0.7085 (4)1.0091 (13)0.068 (4)
O30.4801 (5)0.6455 (4)1.1954 (11)0.061 (3)
N10.8183 (4)0.6139 (3)0.1169 (10)0.020 (2)
N20.5956 (5)0.6245 (3)0.6793 (12)0.032 (3)
N30.4874 (5)0.6693 (3)0.7399 (11)0.030 (3)
N40.4896 (4)0.5831 (4)0.7884 (11)0.026 (3)
C10.9362 (6)0.5481 (5)0.2845 (14)0.043 (4)
H1A0.89580.54070.31340.065*
H1B0.94810.5750.33660.065*
H1C0.96260.52430.31360.065*
C21.0248 (5)0.5573 (5)0.0334 (17)0.045 (4)
H2A1.04230.53180.0830.067*
H2B1.04160.5840.07720.067*
H2C1.03330.55640.07580.067*
C30.9165 (5)0.4987 (4)0.0058 (14)0.025 (3)
C40.9412 (6)0.4612 (5)0.0497 (15)0.036 (4)
H40.97160.4630.12330.043*
C50.9227 (6)0.4213 (5)0.0010 (17)0.043 (4)
H50.94080.39550.03850.051*
C60.8775 (6)0.4186 (4)0.1033 (18)0.040 (3)
H60.86510.39090.13880.047*
C70.8504 (6)0.4553 (4)0.1563 (12)0.033 (3)
H70.81840.45330.22520.04*
C80.8710 (5)0.4963 (3)0.1063 (14)0.020 (2)
C90.8359 (6)0.5443 (5)0.3934 (14)0.044 (4)
H9A0.8770.54270.42610.066*
H9B0.8170.56960.44090.066*
H9C0.81530.51760.42390.066*
C100.7497 (5)0.5370 (4)0.1427 (16)0.043 (4)
H10A0.72720.56420.140.064*
H10B0.74560.52180.04530.064*
H10C0.73490.51830.22460.064*
C110.7423 (6)0.6679 (5)0.1990 (17)0.048 (4)
H11A0.72850.69460.24940.071*
H11B0.72930.6680.09280.071*
H11C0.72590.64240.2510.071*
C120.8410 (7)0.6709 (5)0.4217 (15)0.049 (4)
H12A0.82170.64670.47470.074*
H12B0.88340.670.44210.074*
H12C0.82480.69860.4580.074*
C130.8479 (6)0.7238 (4)0.1328 (16)0.037 (4)
C140.8197 (7)0.7605 (4)0.1893 (16)0.041 (4)
H140.79110.75830.26780.049*
C150.8349 (7)0.8012 (4)0.126 (2)0.059 (5)
H150.81430.82660.15730.071*
C160.8781 (7)0.8049 (6)0.0220 (19)0.058 (5)
H160.88830.83280.01720.07*
C170.9081 (6)0.7673 (5)0.0287 (16)0.036 (4)
H170.93880.76980.10140.044*
C180.8924 (6)0.7265 (4)0.0288 (15)0.031 (3)
C190.9418 (7)0.6844 (5)0.2574 (14)0.053 (5)
H19A0.96950.66330.3010.079*
H19B0.90320.68080.30560.079*
H19C0.95620.7140.27510.079*
C201.0157 (6)0.6847 (5)0.0250 (19)0.057 (5)
H20A1.0270.71450.00210.085*
H20B1.0190.68080.13520.085*
H20C1.04180.6640.02660.085*
C210.7938 (5)0.6517 (4)0.1631 (14)0.027 (3)
H210.80930.67820.12410.032*
C220.7476 (5)0.6539 (4)0.2634 (13)0.029 (3)
H220.73160.68140.29170.035*
C230.7247 (6)0.6160 (4)0.3226 (13)0.025 (3)
C240.7502 (5)0.5773 (4)0.2798 (13)0.026 (3)
H240.73670.55060.3220.031*
C250.7953 (5)0.5773 (4)0.1759 (13)0.028 (3)
H250.81090.550.14410.034*
C260.6758 (5)0.6183 (4)0.4379 (14)0.029 (3)
C270.6471 (6)0.6566 (4)0.4688 (14)0.035 (4)
H270.65280.68150.40620.042*
C280.6088 (6)0.6586 (4)0.5953 (14)0.035 (3)
H280.59170.68590.62070.042*
C290.6208 (6)0.5855 (5)0.6448 (15)0.035 (4)
H290.61130.56030.70290.042*
C300.6611 (5)0.5822 (4)0.5226 (14)0.029 (3)
H300.67830.55470.4990.035*
C310.4870 (6)0.7114 (5)0.7220 (16)0.041 (4)
H310.51020.72820.79010.049*
C320.4559 (7)0.7336 (5)0.6129 (16)0.046 (4)
H320.45790.76450.60380.055*
C330.4211 (7)0.7084 (6)0.5161 (19)0.056 (5)
H330.39850.72180.43830.067*
C340.4199 (7)0.6651 (6)0.5341 (17)0.053 (4)
H340.39630.64790.46810.064*
C350.4522 (6)0.6449 (5)0.6469 (15)0.032 (4)
C360.4529 (6)0.5974 (5)0.6752 (14)0.034 (3)
C370.4184 (6)0.5676 (6)0.5982 (17)0.047 (4)
H370.39240.57740.52090.056*
C380.4214 (7)0.5233 (6)0.633 (2)0.060 (5)
H380.39850.50240.57910.073*
C390.4581 (6)0.5111 (5)0.7461 (17)0.046 (4)
H390.4610.48120.77360.056*
C400.4906 (6)0.5412 (5)0.8202 (15)0.039 (4)
H400.51560.53160.89990.047*
C410.5974 (6)0.5951 (5)1.0044 (15)0.037 (4)
C420.5916 (6)0.6808 (5)0.9645 (17)0.041 (4)
C430.5020 (6)0.6399 (4)1.0784 (17)0.039 (4)
O40.8001 (5)0.7517 (4)0.2878 (14)0.069 (4)
C440.7224 (8)0.7774 (6)0.139 (2)0.081 (6)
H44A0.72630.74920.08740.122*
H44B0.72660.80090.06430.122*
H44C0.68360.77920.18710.122*
C450.7683 (8)0.7815 (5)0.255 (2)0.055 (5)
C460.7727 (8)0.8253 (5)0.328 (2)0.086 (7)
H46A0.78730.8220.43220.13*
H46B0.73380.8390.33030.13*
H46C0.79990.84370.270.13*
O50.7994 (5)0.4797 (4)0.2586 (16)0.087 (4)
C470.7442 (9)0.4184 (7)0.171 (2)0.088 (6)
H47A0.73620.4360.08010.132*
H47B0.70770.41410.22780.132*
H47C0.76010.390.13990.132*
C480.7882 (7)0.4415 (5)0.269 (2)0.060 (5)
C490.8203 (8)0.4128 (5)0.376 (3)0.084 (6)
H49A0.79220.39920.44630.126*
H49B0.84870.43010.43430.126*
H49C0.84110.390.31940.126*
P110.3619 (4)0.5536 (3)1.1346 (10)0.063 (3)0.837 (18)
F110.3632 (9)0.5157 (4)1.0192 (15)0.142 (8)0.837 (18)
F120.3610 (6)0.5917 (5)1.2557 (16)0.086 (5)0.837 (18)
F130.3620 (7)0.5874 (4)1.0032 (12)0.091 (6)0.837 (18)
F140.3639 (6)0.5185 (4)1.2724 (15)0.076 (5)0.837 (18)
F150.4316 (5)0.5543 (5)1.1386 (19)0.107 (6)0.837 (18)
F160.2928 (5)0.5512 (6)1.1405 (18)0.120 (7)0.837 (18)
P210.3462 (15)0.5592 (12)1.146 (4)0.047 (12)0.163 (18)
F210.381 (2)0.5951 (18)1.239 (6)0.066 (16)0.163 (18)
F220.311 (2)0.5234 (11)1.056 (5)0.045 (13)0.163 (18)
F230.376 (2)0.5224 (18)1.248 (6)0.064 (16)0.163 (18)
F240.317 (2)0.5961 (12)1.046 (5)0.067 (15)0.163 (18)
F250.399 (2)0.5560 (18)1.033 (6)0.073 (15)0.163 (18)
F260.2949 (19)0.5627 (15)1.267 (5)0.062 (15)0.163 (18)
P310.6126 (7)0.7867 (3)0.5322 (17)0.067 (5)0.60 (3)
F310.6071 (10)0.7593 (5)0.688 (2)0.068 (7)0.60 (3)
F320.6168 (9)0.8126 (5)0.380 (2)0.073 (7)0.60 (3)
F330.5767 (9)0.7495 (4)0.448 (2)0.060 (7)0.60 (3)
F340.6493 (9)0.8229 (5)0.617 (2)0.074 (7)0.60 (3)
F350.6710 (9)0.7606 (5)0.495 (2)0.073 (8)0.60 (3)
F360.5535 (8)0.8109 (5)0.575 (2)0.079 (7)0.60 (3)
P410.6440 (11)0.7871 (5)0.603 (3)0.075 (7)0.40 (3)
F410.6514 (16)0.8173 (8)0.460 (3)0.099 (12)0.40 (3)
F420.6372 (14)0.7552 (8)0.744 (3)0.081 (11)0.40 (3)
F430.5929 (17)0.8165 (10)0.661 (4)0.117 (14)0.40 (3)
F440.6956 (12)0.7558 (9)0.542 (4)0.083 (13)0.40 (3)
F450.5980 (13)0.7583 (11)0.511 (4)0.101 (15)0.40 (3)
F460.6917 (17)0.8142 (9)0.690 (4)0.127 (14)0.40 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.0269 (3)0.0322 (3)0.0325 (3)0.0027 (3)0.0100 (3)0.0011 (3)
Ru10.0228 (5)0.0233 (5)0.0217 (5)0.0031 (5)0.0064 (4)0.0015 (4)
As10.0212 (7)0.0295 (8)0.0233 (7)0.0040 (6)0.0006 (6)0.0002 (6)
As20.0266 (8)0.0252 (7)0.0231 (7)0.0049 (7)0.0022 (6)0.0005 (6)
As30.0343 (9)0.0299 (8)0.0294 (8)0.0075 (7)0.0055 (6)0.0061 (6)
As40.0314 (8)0.0278 (8)0.0312 (7)0.0044 (7)0.0088 (6)0.0010 (6)
Cl10.037 (2)0.046 (2)0.034 (2)0.0072 (19)0.0161 (16)0.0032 (16)
O10.060 (8)0.055 (7)0.043 (6)0.002 (6)0.007 (6)0.007 (6)
O20.055 (8)0.063 (8)0.085 (9)0.018 (7)0.006 (6)0.029 (7)
O30.067 (8)0.088 (9)0.028 (6)0.011 (7)0.034 (6)0.007 (6)
N10.022 (6)0.028 (6)0.009 (5)0.002 (5)0.005 (4)0.005 (4)
N20.035 (7)0.026 (6)0.033 (6)0.010 (6)0.010 (5)0.003 (5)
N30.028 (7)0.030 (7)0.032 (7)0.010 (6)0.019 (5)0.003 (5)
N40.012 (6)0.039 (7)0.027 (6)0.008 (5)0.006 (5)0.006 (5)
C10.033 (9)0.072 (11)0.025 (8)0.010 (8)0.012 (6)0.003 (7)
C20.022 (8)0.055 (10)0.057 (10)0.000 (8)0.003 (7)0.003 (8)
C30.019 (6)0.022 (7)0.035 (7)0.008 (6)0.013 (5)0.009 (6)
C40.039 (9)0.035 (8)0.035 (8)0.000 (8)0.011 (7)0.014 (7)
C50.030 (9)0.035 (9)0.063 (10)0.025 (8)0.009 (8)0.015 (8)
C60.045 (9)0.019 (6)0.055 (9)0.002 (7)0.026 (9)0.013 (8)
C70.036 (8)0.049 (9)0.014 (7)0.004 (8)0.001 (6)0.005 (6)
C80.026 (6)0.014 (5)0.018 (5)0.011 (5)0.008 (6)0.003 (6)
C90.050 (10)0.053 (10)0.030 (8)0.005 (9)0.006 (7)0.001 (7)
C100.038 (8)0.039 (8)0.052 (10)0.002 (7)0.001 (7)0.003 (7)
C110.038 (9)0.054 (10)0.051 (9)0.009 (8)0.000 (8)0.008 (8)
C120.065 (11)0.040 (9)0.043 (9)0.002 (8)0.000 (8)0.028 (7)
C130.046 (9)0.022 (7)0.044 (9)0.002 (7)0.028 (8)0.007 (6)
C140.046 (10)0.027 (8)0.049 (9)0.012 (8)0.018 (7)0.022 (7)
C150.076 (12)0.023 (8)0.078 (12)0.004 (9)0.030 (12)0.016 (9)
C160.048 (11)0.065 (12)0.062 (11)0.027 (10)0.027 (9)0.009 (9)
C170.015 (7)0.042 (9)0.053 (9)0.004 (7)0.012 (7)0.012 (7)
C180.031 (8)0.022 (7)0.042 (8)0.010 (7)0.025 (7)0.005 (6)
C190.076 (12)0.062 (11)0.021 (7)0.026 (10)0.008 (7)0.019 (7)
C200.031 (9)0.048 (10)0.090 (12)0.018 (8)0.017 (9)0.005 (9)
C210.032 (8)0.013 (6)0.035 (7)0.008 (6)0.001 (6)0.007 (6)
C220.027 (8)0.039 (8)0.021 (7)0.005 (7)0.007 (6)0.004 (7)
C230.032 (8)0.022 (7)0.022 (7)0.003 (7)0.003 (6)0.003 (6)
C240.023 (7)0.040 (8)0.015 (6)0.004 (7)0.003 (6)0.011 (6)
C250.024 (8)0.036 (8)0.025 (7)0.005 (7)0.001 (6)0.002 (6)
C260.026 (7)0.032 (7)0.029 (8)0.003 (6)0.005 (6)0.003 (6)
C270.051 (9)0.009 (6)0.046 (8)0.006 (7)0.029 (7)0.008 (6)
C280.034 (8)0.034 (8)0.037 (8)0.019 (7)0.022 (7)0.008 (7)
C290.030 (9)0.030 (8)0.044 (9)0.005 (7)0.013 (7)0.000 (7)
C300.023 (7)0.027 (7)0.038 (8)0.005 (6)0.002 (6)0.003 (6)
C310.041 (10)0.034 (9)0.048 (10)0.006 (8)0.029 (8)0.005 (7)
C320.057 (11)0.043 (9)0.037 (9)0.016 (9)0.036 (8)0.011 (8)
C330.057 (12)0.056 (12)0.055 (11)0.015 (10)0.014 (9)0.015 (9)
C340.042 (10)0.079 (14)0.038 (9)0.009 (10)0.003 (8)0.001 (9)
C350.032 (9)0.041 (9)0.022 (7)0.016 (8)0.020 (7)0.001 (6)
C360.019 (7)0.054 (9)0.029 (8)0.002 (8)0.015 (7)0.018 (7)
C370.029 (9)0.060 (11)0.051 (10)0.002 (9)0.005 (7)0.009 (8)
C380.034 (10)0.046 (11)0.102 (15)0.003 (9)0.001 (10)0.033 (10)
C390.042 (10)0.042 (9)0.056 (10)0.009 (9)0.017 (8)0.002 (8)
C400.041 (9)0.032 (9)0.043 (8)0.006 (8)0.018 (7)0.011 (7)
C410.033 (9)0.049 (10)0.028 (8)0.021 (8)0.000 (7)0.013 (7)
C420.016 (7)0.045 (9)0.063 (10)0.011 (7)0.009 (7)0.007 (8)
C430.046 (10)0.019 (8)0.053 (10)0.013 (7)0.025 (8)0.002 (7)
O40.069 (9)0.040 (7)0.100 (9)0.000 (7)0.018 (7)0.000 (7)
C440.094 (17)0.073 (14)0.076 (14)0.014 (13)0.031 (13)0.006 (11)
C450.040 (10)0.030 (9)0.094 (13)0.023 (9)0.032 (10)0.017 (9)
C460.065 (13)0.036 (10)0.16 (2)0.009 (10)0.014 (13)0.017 (11)
O50.082 (10)0.033 (7)0.144 (12)0.000 (7)0.045 (9)0.008 (8)
C470.109 (18)0.079 (15)0.077 (13)0.014 (14)0.002 (13)0.004 (12)
C480.045 (11)0.040 (10)0.095 (14)0.001 (9)0.028 (10)0.006 (10)
C490.077 (13)0.060 (11)0.114 (15)0.025 (11)0.036 (14)0.000 (13)
P110.077 (6)0.052 (5)0.059 (5)0.023 (4)0.033 (4)0.008 (4)
F110.24 (2)0.052 (8)0.135 (12)0.068 (11)0.080 (12)0.029 (8)
F120.090 (12)0.078 (9)0.091 (10)0.031 (9)0.004 (9)0.024 (8)
F130.152 (15)0.059 (8)0.060 (8)0.042 (9)0.002 (8)0.018 (6)
F140.061 (9)0.066 (9)0.100 (10)0.020 (7)0.008 (7)0.019 (7)
F150.070 (9)0.109 (12)0.141 (14)0.006 (9)0.040 (10)0.035 (10)
F160.086 (10)0.173 (17)0.101 (13)0.036 (10)0.033 (9)0.050 (12)
P210.060 (19)0.029 (16)0.051 (18)0.017 (12)0.018 (11)0.007 (12)
F210.07 (2)0.06 (2)0.07 (2)0.019 (16)0.006 (15)0.006 (16)
F220.05 (2)0.044 (17)0.042 (19)0.009 (15)0.001 (14)0.001 (14)
F230.06 (2)0.06 (2)0.07 (2)0.007 (16)0.007 (15)0.001 (16)
F240.07 (2)0.047 (18)0.08 (2)0.005 (15)0.004 (15)0.004 (15)
F250.064 (19)0.09 (2)0.07 (2)0.001 (15)0.021 (16)0.003 (15)
F260.061 (19)0.05 (2)0.07 (2)0.003 (14)0.022 (16)0.016 (15)
P310.086 (10)0.028 (5)0.086 (9)0.006 (6)0.053 (8)0.002 (6)
F310.091 (16)0.038 (10)0.075 (13)0.019 (11)0.028 (12)0.014 (9)
F320.092 (14)0.031 (8)0.096 (13)0.008 (9)0.034 (13)0.004 (10)
F330.086 (15)0.014 (7)0.081 (14)0.002 (9)0.036 (11)0.003 (8)
F340.087 (16)0.022 (10)0.113 (17)0.020 (10)0.026 (14)0.019 (9)
F350.082 (17)0.026 (10)0.111 (15)0.002 (10)0.047 (14)0.011 (10)
F360.083 (14)0.051 (11)0.102 (15)0.006 (10)0.044 (12)0.009 (10)
P410.103 (16)0.030 (8)0.092 (13)0.020 (10)0.031 (11)0.010 (8)
F410.12 (3)0.051 (17)0.13 (3)0.005 (18)0.03 (2)0.036 (19)
F420.09 (2)0.058 (17)0.09 (2)0.018 (18)0.013 (18)0.019 (15)
F430.16 (3)0.10 (2)0.09 (2)0.07 (2)0.04 (2)0.021 (18)
F440.041 (18)0.07 (2)0.14 (3)0.014 (15)0.026 (18)0.006 (19)
F450.07 (2)0.11 (3)0.13 (3)0.03 (2)0.00 (2)0.05 (2)
F460.14 (3)0.10 (2)0.14 (3)0.03 (2)0.03 (2)0.01 (2)
Geometric parameters (Å, º) top
Re1—C421.928 (15)C20—H20C0.98
Re1—C411.937 (16)C21—C221.375 (16)
Re1—C431.947 (14)C21—H210.95
Re1—N42.169 (11)C22—C231.376 (16)
Re1—N32.176 (11)C22—H220.95
Re1—N22.185 (10)C23—C241.372 (16)
Ru1—N12.117 (9)C23—C261.507 (17)
Ru1—As12.4162 (16)C24—C251.374 (16)
Ru1—As32.4206 (17)C24—H240.95
Ru1—As22.4215 (17)C25—H250.95
Ru1—As42.4243 (17)C26—C271.371 (16)
Ru1—Cl12.424 (3)C26—C301.375 (17)
As1—C21.944 (12)C27—C281.414 (16)
As1—C11.955 (12)C27—H270.95
As1—C31.967 (12)C28—H280.95
As2—C91.897 (12)C29—C301.417 (17)
As2—C101.955 (12)C29—H290.95
As2—C81.973 (10)C30—H300.95
As3—C121.923 (13)C31—C321.374 (19)
As3—C111.943 (13)C31—H310.95
As3—C131.955 (13)C32—C331.40 (2)
As4—C201.952 (12)C32—H320.95
As4—C181.962 (13)C33—C341.33 (2)
As4—C191.965 (12)C33—H330.95
O1—C411.149 (16)C34—C351.38 (2)
O2—C421.116 (15)C34—H340.95
O3—C431.156 (15)C35—C361.48 (2)
N1—C251.343 (15)C36—C371.380 (19)
N1—C211.348 (15)C37—C381.39 (2)
N2—C281.315 (16)C37—H370.95
N2—C291.362 (16)C38—C391.35 (2)
N3—C311.299 (16)C38—H380.95
N3—C351.367 (17)C39—C401.350 (19)
N4—C401.315 (16)C39—H390.95
N4—C361.372 (16)C40—H400.95
C1—H1A0.98O4—C451.202 (19)
C1—H1B0.98C44—C451.46 (2)
C1—H1C0.98C44—H44A0.98
C2—H2A0.98C44—H44B0.98
C2—H2B0.98C44—H44C0.98
C2—H2C0.98C45—C461.49 (2)
C3—C81.362 (16)C46—H46A0.98
C3—C41.370 (17)C46—H46B0.98
C4—C51.36 (2)C46—H46C0.98
C4—H40.95O5—C481.202 (17)
C5—C61.379 (19)C47—C481.50 (2)
C5—H50.95C47—H47A0.98
C6—C71.365 (17)C47—H47B0.98
C6—H60.95C47—H47C0.98
C7—C81.410 (16)C48—C491.48 (2)
C7—H70.95C49—H49A0.98
C9—H9A0.98C49—H49B0.98
C9—H9B0.98C49—H49C0.98
C9—H9C0.98P11—F111.543 (13)
C10—H10A0.98P11—F131.553 (12)
C10—H10B0.98P11—F161.573 (13)
C10—H10C0.98P11—F121.580 (12)
C11—H11A0.98P11—F151.586 (13)
C11—H11B0.98P11—F141.622 (12)
C11—H11C0.98P21—F251.56 (2)
C12—H12A0.98P21—F221.57 (2)
C12—H12B0.98P21—F241.58 (2)
C12—H12C0.98P21—F261.58 (2)
C13—C181.367 (18)P21—F211.59 (2)
C13—C141.386 (17)P21—F231.59 (2)
C14—C151.41 (2)P31—F321.560 (15)
C14—H140.95P31—F341.578 (15)
C15—C161.35 (2)P31—F361.579 (15)
C15—H150.95P31—F351.585 (16)
C16—C171.41 (2)P31—F331.586 (16)
C16—H160.95P31—F311.612 (16)
C17—C181.395 (17)P41—F431.553 (19)
C17—H170.95P41—F461.56 (2)
C19—H19A0.98P41—F411.577 (19)
C19—H19B0.98P41—F421.582 (19)
C19—H19C0.98P41—F451.59 (2)
C20—H20A0.98P41—F441.610 (19)
C20—H20B0.98
C42—Re1—C4186.8 (6)C22—C21—H21118.2
C42—Re1—C4384.0 (6)C21—C22—C23119.4 (12)
C41—Re1—C4386.0 (6)C21—C22—H22120.3
C42—Re1—N4174.2 (5)C23—C22—H22120.3
C41—Re1—N498.9 (5)C24—C23—C22117.8 (12)
C43—Re1—N497.6 (5)C24—C23—C26122.5 (11)
C42—Re1—N398.2 (5)C22—C23—C26119.7 (11)
C41—Re1—N3173.5 (5)C23—C24—C25120.0 (12)
C43—Re1—N398.6 (5)C23—C24—H24120
N4—Re1—N376.1 (4)C25—C24—H24120
C42—Re1—N295.4 (5)N1—C25—C24123.2 (12)
C41—Re1—N293.2 (5)N1—C25—H25118.4
C43—Re1—N2179.0 (6)C24—C25—H25118.4
N4—Re1—N283.1 (4)C27—C26—C30117.8 (11)
N3—Re1—N282.2 (4)C27—C26—C23121.6 (11)
N1—Ru1—As193.4 (3)C30—C26—C23120.4 (11)
N1—Ru1—As391.8 (3)C26—C27—C28119.1 (11)
As1—Ru1—As3174.67 (6)C26—C27—H27120.4
N1—Ru1—As292.0 (3)C28—C27—H27120.4
As1—Ru1—As284.65 (5)N2—C28—C27123.3 (12)
As3—Ru1—As294.31 (6)N2—C28—H28118.4
N1—Ru1—As492.9 (3)C27—C28—H28118.4
As1—Ru1—As496.10 (6)N2—C29—C30120.3 (12)
As3—Ru1—As484.49 (6)N2—C29—H29119.8
As2—Ru1—As4175.01 (6)C30—C29—H29119.8
N1—Ru1—Cl1178.5 (3)C26—C30—C29120.7 (12)
As1—Ru1—Cl186.41 (9)C26—C30—H30119.6
As3—Ru1—Cl188.31 (9)C29—C30—H30119.6
As2—Ru1—Cl186.51 (10)N3—C31—C32125.5 (15)
As4—Ru1—Cl188.61 (10)N3—C31—H31117.3
C2—As1—C1100.8 (6)C32—C31—H31117.3
C2—As1—C3103.4 (5)C31—C32—C33116.3 (15)
C1—As1—C3100.0 (6)C31—C32—H32121.8
C2—As1—Ru1118.8 (5)C33—C32—H32121.8
C1—As1—Ru1121.4 (4)C34—C33—C32119.3 (16)
C3—As1—Ru1109.6 (4)C34—C33—H33120.3
C9—As2—C10100.3 (6)C32—C33—H33120.3
C9—As2—C8103.1 (6)C33—C34—C35121.3 (17)
C10—As2—C8101.6 (5)C33—C34—H34119.4
C9—As2—Ru1118.9 (5)C35—C34—H34119.4
C10—As2—Ru1122.0 (4)N3—C35—C34119.7 (14)
C8—As2—Ru1108.2 (3)N3—C35—C36115.7 (12)
C12—As3—C11100.9 (7)C34—C35—C36124.6 (15)
C12—As3—C13102.3 (6)N4—C36—C37119.5 (14)
C11—As3—C13101.0 (6)N4—C36—C35116.2 (12)
C12—As3—Ru1120.0 (4)C37—C36—C35124.3 (14)
C11—As3—Ru1120.6 (4)C36—C37—C38120.6 (15)
C13—As3—Ru1109.1 (4)C36—C37—H37119.7
C20—As4—C18104.0 (6)C38—C37—H37119.7
C20—As4—C19100.0 (7)C39—C38—C37117.4 (15)
C18—As4—C19101.7 (6)C39—C38—H38121.3
C20—As4—Ru1120.2 (5)C37—C38—H38121.3
C18—As4—Ru1107.1 (4)C40—C39—C38120.3 (15)
C19—As4—Ru1121.3 (4)C40—C39—H39119.8
C25—N1—C21116.1 (10)C38—C39—H39119.8
C25—N1—Ru1121.5 (8)N4—C40—C39123.8 (14)
C21—N1—Ru1121.8 (8)N4—C40—H40118.1
C28—N2—C29118.5 (11)C39—C40—H40118.1
C28—N2—Re1120.2 (9)O1—C41—Re1177.0 (13)
C29—N2—Re1120.6 (9)O2—C42—Re1179.5 (15)
C31—N3—C35117.8 (13)O3—C43—Re1174.8 (13)
C31—N3—Re1126.2 (11)C45—C44—H44A109.5
C35—N3—Re1115.7 (9)C45—C44—H44B109.5
C40—N4—C36118.4 (12)H44A—C44—H44B109.5
C40—N4—Re1125.9 (9)C45—C44—H44C109.5
C36—N4—Re1115.5 (9)H44A—C44—H44C109.5
As1—C1—H1A109.5H44B—C44—H44C109.5
As1—C1—H1B109.5O4—C45—C44122.1 (16)
H1A—C1—H1B109.5O4—C45—C46122.6 (18)
As1—C1—H1C109.5C44—C45—C46115.3 (17)
H1A—C1—H1C109.5C45—C46—H46A109.5
H1B—C1—H1C109.5C45—C46—H46B109.5
As1—C2—H2A109.5H46A—C46—H46B109.5
As1—C2—H2B109.5C45—C46—H46C109.5
H2A—C2—H2B109.5H46A—C46—H46C109.5
As1—C2—H2C109.5H46B—C46—H46C109.5
H2A—C2—H2C109.5C48—C47—H47A109.5
H2B—C2—H2C109.5C48—C47—H47B109.5
C8—C3—C4119.8 (12)H47A—C47—H47B109.5
C8—C3—As1117.5 (9)C48—C47—H47C109.5
C4—C3—As1122.6 (10)H47A—C47—H47C109.5
C5—C4—C3121.0 (13)H47B—C47—H47C109.5
C5—C4—H4119.5O5—C48—C49121.4 (19)
C3—C4—H4119.5O5—C48—C47123.9 (19)
C4—C5—C6119.4 (13)C49—C48—C47114.6 (15)
C4—C5—H5120.3C48—C49—H49A109.5
C6—C5—H5120.3C48—C49—H49B109.5
C7—C6—C5121.0 (12)H49A—C49—H49B109.5
C7—C6—H6119.5C48—C49—H49C109.5
C5—C6—H6119.5H49A—C49—H49C109.5
C6—C7—C8118.5 (12)H49B—C49—H49C109.5
C6—C7—H7120.8F11—P11—F1390.7 (8)
C8—C7—H7120.8F11—P11—F1690.3 (9)
C3—C8—C7120.2 (11)F13—P11—F1693.3 (9)
C3—C8—As2120.0 (9)F11—P11—F12178.7 (10)
C7—C8—As2119.8 (9)F13—P11—F1290.5 (8)
As2—C9—H9A109.5F16—P11—F1290.0 (9)
As2—C9—H9B109.5F11—P11—F1590.3 (9)
H9A—C9—H9B109.5F13—P11—F1590.3 (8)
As2—C9—H9C109.5F16—P11—F15176.3 (10)
H9A—C9—H9C109.5F12—P11—F1589.3 (8)
H9B—C9—H9C109.5F11—P11—F1489.5 (8)
As2—C10—H10A109.5F13—P11—F14178.2 (10)
As2—C10—H10B109.5F16—P11—F1488.5 (8)
H10A—C10—H10B109.5F12—P11—F1489.2 (7)
As2—C10—H10C109.5F15—P11—F1487.9 (8)
H10A—C10—H10C109.5F25—P21—F2291.1 (17)
H10B—C10—H10C109.5F25—P21—F2490.7 (17)
As3—C11—H11A109.5F22—P21—F2490.4 (17)
As3—C11—H11B109.5F25—P21—F26178 (2)
H11A—C11—H11B109.5F22—P21—F2690.8 (17)
As3—C11—H11C109.5F24—P21—F2690.7 (17)
H11A—C11—H11C109.5F25—P21—F2189.3 (17)
H11B—C11—H11C109.5F22—P21—F21179 (2)
As3—C12—H12A109.5F24—P21—F2190.1 (17)
As3—C12—H12B109.5F26—P21—F2188.8 (17)
H12A—C12—H12B109.5F25—P21—F2389.7 (17)
As3—C12—H12C109.5F22—P21—F2390.1 (17)
H12A—C12—H12C109.5F24—P21—F23179 (2)
H12B—C12—H12C109.5F26—P21—F2388.8 (17)
C18—C13—C14122.2 (13)F21—P21—F2389.4 (17)
C18—C13—As3116.9 (10)F32—P31—F3490.8 (9)
C14—C13—As3120.8 (12)F32—P31—F3691.0 (10)
C13—C14—C15117.5 (15)F34—P31—F3690.3 (9)
C13—C14—H14121.2F32—P31—F3591.5 (9)
C15—C14—H14121.2F34—P31—F3590.6 (11)
C16—C15—C14121.5 (15)F36—P31—F35177.3 (11)
C16—C15—H15119.2F32—P31—F3389.7 (10)
C14—C15—H15119.2F34—P31—F33178.8 (12)
C15—C16—C17119.8 (15)F36—P31—F3390.7 (10)
C15—C16—H16120.1F35—P31—F3388.3 (10)
C17—C16—H16120.1F32—P31—F31178.9 (13)
C18—C17—C16119.6 (14)F34—P31—F3190.2 (10)
C18—C17—H17120.2F36—P31—F3188.6 (9)
C16—C17—H17120.2F35—P31—F3188.9 (10)
C13—C18—C17119.1 (13)F33—P31—F3189.2 (9)
C13—C18—As4120.8 (10)F43—P41—F4693.0 (14)
C17—C18—As4120.0 (11)F43—P41—F4189.9 (13)
As4—C19—H19A109.5F46—P41—F4190.2 (14)
As4—C19—H19B109.5F43—P41—F4291.9 (13)
H19A—C19—H19B109.5F46—P41—F4290.9 (14)
As4—C19—H19C109.5F41—P41—F42177.8 (17)
H19A—C19—H19C109.5F43—P41—F4589.8 (15)
H19B—C19—H19C109.5F46—P41—F45177.1 (17)
As4—C20—H20A109.5F41—P41—F4589.1 (14)
As4—C20—H20B109.5F42—P41—F4589.7 (14)
H20A—C20—H20B109.5F43—P41—F44178.6 (18)
As4—C20—H20C109.5F46—P41—F4488.4 (14)
H20A—C20—H20C109.5F41—P41—F4490.3 (14)
H20B—C20—H20C109.5F42—P41—F4487.9 (13)
N1—C21—C22123.5 (12)F45—P41—F4488.7 (14)
N1—C21—H21118.2
N1—Ru1—As1—C2148.2 (6)Ru1—As1—C3—C82.2 (10)
As3—Ru1—As1—C241.2 (9)C2—As1—C3—C454.6 (11)
As2—Ru1—As1—C2120.2 (5)C1—As1—C3—C449.1 (11)
As4—Ru1—As1—C254.9 (5)Ru1—As1—C3—C4177.8 (9)
Cl1—Ru1—As1—C233.3 (5)C8—C3—C4—C52.9 (19)
N1—Ru1—As1—C122.2 (6)As1—C3—C4—C5178.4 (10)
As3—Ru1—As1—C1167.1 (8)C3—C4—C5—C61 (2)
As2—Ru1—As1—C1113.9 (5)C4—C5—C6—C71 (2)
As4—Ru1—As1—C171.0 (5)C5—C6—C7—C82.3 (19)
Cl1—Ru1—As1—C1159.3 (5)C4—C3—C8—C71.7 (17)
N1—Ru1—As1—C393.4 (4)As1—C3—C8—C7177.4 (8)
As3—Ru1—As1—C377.2 (8)C4—C3—C8—As2177.0 (9)
As2—Ru1—As1—C31.7 (4)As1—C3—C8—As21.3 (12)
As4—Ru1—As1—C3173.3 (3)C6—C7—C8—C30.9 (17)
Cl1—Ru1—As1—C385.1 (4)C6—C7—C8—As2179.6 (9)
N1—Ru1—As2—C9148.5 (6)C9—As2—C8—C3127.1 (10)
As1—Ru1—As2—C9118.2 (5)C10—As2—C8—C3129.3 (10)
As3—Ru1—As2—C956.5 (5)Ru1—As2—C8—C30.2 (10)
As4—Ru1—As2—C919.4 (10)C9—As2—C8—C754.2 (10)
Cl1—Ru1—As2—C931.5 (5)C10—As2—C8—C749.4 (10)
N1—Ru1—As2—C1022.6 (5)Ru1—As2—C8—C7178.9 (8)
As1—Ru1—As2—C10115.8 (5)C12—As3—C13—C18120.3 (10)
As3—Ru1—As2—C1069.4 (5)C11—As3—C13—C18135.8 (10)
As4—Ru1—As2—C10145.4 (9)Ru1—As3—C13—C187.8 (10)
Cl1—Ru1—As2—C10157.4 (5)C12—As3—C13—C1457.0 (11)
N1—Ru1—As2—C894.5 (4)C11—As3—C13—C1446.8 (11)
As1—Ru1—As2—C81.2 (3)Ru1—As3—C13—C14174.8 (9)
As3—Ru1—As2—C8173.6 (3)C18—C13—C14—C155.4 (19)
As4—Ru1—As2—C897.6 (8)As3—C13—C14—C15177.4 (10)
Cl1—Ru1—As2—C885.5 (4)C13—C14—C15—C165 (2)
N1—Ru1—As3—C12160.2 (6)C14—C15—C16—C172 (2)
As1—Ru1—As3—C1210.5 (9)C15—C16—C17—C181 (2)
As2—Ru1—As3—C1268.0 (5)C14—C13—C18—C173.4 (19)
As4—Ru1—As3—C12107.1 (5)As3—C13—C18—C17179.3 (9)
Cl1—Ru1—As3—C1218.3 (5)C14—C13—C18—As4175.9 (9)
N1—Ru1—As3—C1133.6 (6)As3—C13—C18—As41.4 (14)
As1—Ru1—As3—C11137.0 (9)C16—C17—C18—C130.3 (19)
As2—Ru1—As3—C1158.5 (5)C16—C17—C18—As4178.9 (10)
As4—Ru1—As3—C11126.4 (5)C20—As4—C18—C13118.4 (11)
Cl1—Ru1—As3—C11144.9 (5)C19—As4—C18—C13138.1 (11)
N1—Ru1—As3—C1382.4 (5)Ru1—As4—C18—C139.9 (11)
As1—Ru1—As3—C13107.0 (8)C20—As4—C18—C1760.8 (11)
As2—Ru1—As3—C13174.5 (4)C19—As4—C18—C1742.7 (11)
As4—Ru1—As3—C1310.3 (4)Ru1—As4—C18—C17170.9 (9)
Cl1—Ru1—As3—C1399.1 (4)C25—N1—C21—C220.5 (17)
N1—Ru1—As4—C20160.9 (6)Ru1—N1—C21—C22171.2 (9)
As1—Ru1—As4—C2067.1 (6)N1—C21—C22—C230.6 (19)
As3—Ru1—As4—C20107.6 (6)C21—C22—C23—C241.1 (18)
As2—Ru1—As4—C2031.2 (10)C21—C22—C23—C26177.3 (11)
Cl1—Ru1—As4—C2019.1 (6)C22—C23—C24—C252.9 (18)
N1—Ru1—As4—C1881.0 (4)C26—C23—C24—C25179.0 (11)
As1—Ru1—As4—C18174.7 (4)C21—N1—C25—C241.4 (17)
As3—Ru1—As4—C1810.6 (4)Ru1—N1—C25—C24173.1 (9)
As2—Ru1—As4—C1887.0 (9)C23—C24—C25—N13.2 (19)
Cl1—Ru1—As4—C1899.0 (4)C24—C23—C26—C27173.7 (12)
N1—Ru1—As4—C1934.8 (6)C22—C23—C26—C2710.2 (19)
As1—Ru1—As4—C1958.9 (6)C24—C23—C26—C3010.4 (19)
As3—Ru1—As4—C19126.4 (6)C22—C23—C26—C30165.7 (12)
As2—Ru1—As4—C19157.3 (9)C30—C26—C27—C286.6 (19)
Cl1—Ru1—As4—C19145.2 (6)C23—C26—C27—C28169.3 (12)
As1—Ru1—N1—C2547.9 (9)C29—N2—C28—C271 (2)
As3—Ru1—N1—C25131.2 (9)Re1—N2—C28—C27171.8 (10)
As2—Ru1—N1—C2536.9 (9)C26—C27—C28—N25 (2)
As4—Ru1—N1—C25144.2 (9)C28—N2—C29—C301 (2)
As1—Ru1—N1—C21140.9 (9)Re1—N2—C29—C30169.4 (9)
As3—Ru1—N1—C2140.0 (9)C27—C26—C30—C294.5 (19)
As2—Ru1—N1—C21134.3 (9)C23—C26—C30—C29171.6 (12)
As4—Ru1—N1—C2144.6 (9)N2—C29—C30—C260.5 (19)
C42—Re1—N2—C2847.1 (11)C35—N3—C31—C322.7 (19)
C41—Re1—N2—C28134.1 (11)Re1—N3—C31—C32170.6 (9)
N4—Re1—N2—C28127.4 (11)N3—C31—C32—C331 (2)
N3—Re1—N2—C2850.5 (11)C31—C32—C33—C340 (2)
C42—Re1—N2—C29123.4 (11)C32—C33—C34—C350 (2)
C41—Re1—N2—C2936.4 (11)C31—N3—C35—C342.8 (18)
N4—Re1—N2—C2962.2 (10)Re1—N3—C35—C34171.2 (10)
N3—Re1—N2—C29139.0 (11)C31—N3—C35—C36178.2 (11)
C42—Re1—N3—C312.4 (11)Re1—N3—C35—C367.8 (13)
C43—Re1—N3—C3182.7 (11)C33—C34—C35—N32 (2)
N4—Re1—N3—C31178.5 (11)C33—C34—C35—C36179.4 (13)
N2—Re1—N3—C3196.7 (11)C40—N4—C36—C370.2 (17)
C42—Re1—N3—C35171.0 (9)Re1—N4—C36—C37176.0 (9)
C43—Re1—N3—C35103.8 (9)C40—N4—C36—C35178.3 (11)
N4—Re1—N3—C358.0 (8)Re1—N4—C36—C355.4 (13)
N2—Re1—N3—C3576.7 (8)N3—C35—C36—N41.6 (15)
C41—Re1—N4—C407.2 (11)C34—C35—C36—N4177.4 (12)
C43—Re1—N4—C4079.9 (11)N3—C35—C36—C37176.9 (11)
N3—Re1—N4—C40177.0 (11)C34—C35—C36—C374 (2)
N2—Re1—N4—C4099.3 (10)N4—C36—C37—C381 (2)
C41—Re1—N4—C36168.7 (8)C35—C36—C37—C38179.4 (13)
C43—Re1—N4—C36104.2 (9)C36—C37—C38—C391 (2)
N3—Re1—N4—C367.1 (8)C37—C38—C39—C401 (2)
N2—Re1—N4—C3676.6 (8)C36—N4—C40—C391.1 (19)
C2—As1—C3—C8129.8 (9)Re1—N4—C40—C39174.7 (10)
C1—As1—C3—C8126.4 (9)C38—C39—C40—N41 (2)

Experimental details

Crystal data
Chemical formula[ReRuCl(C10H16As2)2(C10H8N2)2(CO)3](PF6)2·2C3H6O
Mr1697.35
Crystal system, space groupOrthorhombic, Pna21
Temperature (K)150
a, b, c (Å)22.736 (5), 30.654 (6), 8.799 (2)
V3)6132 (2)
Z4
Radiation typeMo Kα
µ (mm1)4.54
Crystal size (mm)0.45 × 0.08 × 0.02
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionMulti-scans
(SORTAV; Blessing, 1995)
Tmin, Tmax0.235, 0.915
No. of measured, independent and
observed [I > 2σ(I)] reflections
15874, 7883, 6157
Rint0.109
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.115, 0.99
No. of reflections7883
No. of parameters852
No. of restraints308
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.55, 1.16
Absolute structureFlack (1983)
Absolute structure parameter0.066 (10)

Computer programs: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998), DENZO and COLLECT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1990).

Selected geometric parameters (Å, º) top
Re1—C421.928 (15)Ru1—N12.117 (9)
Re1—C411.937 (16)Ru1—As12.4162 (16)
Re1—C431.947 (14)Ru1—As32.4206 (17)
Re1—N42.169 (11)Ru1—As22.4215 (17)
Re1—N32.176 (11)Ru1—As42.4243 (17)
Re1—N22.185 (10)Ru1—Cl12.424 (3)
C42—Re1—C4186.8 (6)N1—Ru1—As193.4 (3)
C42—Re1—C4384.0 (6)N1—Ru1—As391.8 (3)
C41—Re1—C4386.0 (6)As1—Ru1—As3174.67 (6)
C42—Re1—N4174.2 (5)N1—Ru1—As292.0 (3)
C41—Re1—N498.9 (5)As1—Ru1—As284.65 (5)
C43—Re1—N497.6 (5)As3—Ru1—As294.31 (6)
C42—Re1—N398.2 (5)N1—Ru1—As492.9 (3)
C41—Re1—N3173.5 (5)As1—Ru1—As496.10 (6)
C43—Re1—N398.6 (5)As3—Ru1—As484.49 (6)
N4—Re1—N376.1 (4)As2—Ru1—As4175.01 (6)
C42—Re1—N295.4 (5)N1—Ru1—Cl1178.5 (3)
C41—Re1—N293.2 (5)As1—Ru1—Cl186.41 (9)
C43—Re1—N2179.0 (6)As3—Ru1—Cl188.31 (9)
N4—Re1—N283.1 (4)As2—Ru1—Cl186.51 (10)
N3—Re1—N282.2 (4)As4—Ru1—Cl188.61 (10)
 

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