(μ-Benzene­thiol­ato)­bis­[(bi­pyridine)­tri­carbonyl­rhodium(I)] perchlorate di­chloro­methane hemisolvate

The title binuclear Re^I–thiol­ate complex, [Re₂(C₆H₅S)(C₁₀H₈N₂)₂(CO)₆]ClO₄·0.5CH₂Cl₂, was isolated from the reaction between [Re(bpy)(CO)₃](SC₆H₅) and [Cu₂(μ₂-dppm)₂(MeCN)₄](ClO₄)₂ (bpy is bi­pyridine and dppm is di­phenyl­phosphino­methane). The two rhenium–di­imine moieties are bridged by one S-donor and each Re atom adopts a distorted octahedral geometry.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.015 Å
• Disorder in solvent or counterion
• R factor = 0.038
• wR factor = 0.109
• Data-to-parameter ratio = 13.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_302  Alert C Anion/Solvent Disorder .......................      11.00 Perc.


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 1 Alert Level C = Please check

---

S1. Comment

There has been increasing interest in designing polymetallic complexes with mixed diimine and thiolate ligands owing to the unique optical and optoelectronic properties (Yam et al., 2000; Tang et al., 2002). It is well known that thiolates as versatile bridging ligands could exhibit various bonding modes to produce metal cluster complexes with diverse structural topologies (Su et al., 1998). We describe here a dinuclear rhenium(I) complex, [{Re(bpy)(CO)₃}₂(µ-SC₆H₅)]ClO₄·0.5CH₂Cl₂, (II), which resulted from the self-assembly between the metal components {Re(bpy)(CO)₃}(SC₆H₅), (I), and [Cu₂(µ₂-dppm)₂(MeCN)₄](ClO₄)₂.

A perspective drawing of the complex cation of (II) with the atomic numbering scheme is shown in Fig. 1, and selected bonding parameters are given in Table 1. The two rehnium–diimne moieties are bridged by the S-donor from the benzenethiolate ligand, with an Re2—S1—Re1 bite angle of 124.35 (8)°. The three carbonyl ligands at each Re atom are arranged in a facial configuration. Each Re atom adopts a slightly distorted octahedral geormetry, with the S1—Re1—C43 and S1—Re2—C46 bond angles being 174.8 (2) and 175.8 (3)°, respectively. The planes of the two bipyridyl ligands and the phenyl ring of the bridging thiolate ligand show a stacked conformation, with dihedral angles between the idealized planes of the two bipyridyl units and the phenyl ring of 14.1 (2) and 16.1 (3)°. Because of the steric effects of each chelating bipyridyl ligand, the N2—Re1—N1 [75.3 (2)°] and N4—Re2—N3 [74.2 (3)°] angles are far from 90° (Yam et al., 1995, 1996). The average bond distances of Re—S [2.526 (2) Å] and Re—C [1.918 (9) Å] are found to be comparable to those observed in [Re(CO)₃SCH₃]₄ (Abel et al., 1970; Yam et al., 1997).

S2. Experimental

The starting material {Re(bpy)(CO)₃}(µ-SC₆H₅), (I), was synthesized by modification of literature procedures (Yam et al., 1997) using a large excess of benzenethiolate to give (I) as a red–orange solid in good yield. Reaction between (I) and [Cu₂(µ₂-dppm)₂(MeCN)₄](ClO₄)₂ (Diez et al., 1987) with an equimolar ratio in dichloromethane was carried out under anaerobic conditions for 12 h, where a color change from red into yellow–orange was observed. Well shaped yellow crystals of (II) suitable for X-ray diffraction analysis were grown by layering of diethyl ether onto the concentrated solution.

S3. Refinement

The positions of the H atoms were genetared geometrically (C—H bond length fixed at 0.96 Å), assigned isotropic displacement parameters and allowed to ride on their respective parent C atoms before the final cycle of least-squares refinement. The dichloromethane molecule exists near the center of symmetry and atom C01 has two possible positions with occupancies of 50%.

Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures

Fig. 1. A view of the complex cation of (II) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level.

(µ-benzenethiolato){Bis((bipyridine)(tricarbonyl))} dirhenium(I)perchloratedichloromethanesolvate

Crystal data

[Re2(C6H5S)(C10H8N2)2(CO)6]ClO4·0.5CH2Cl2	Z = 2
Mr = 1103.90	F(000) = 1050
Triclinic, P1	Dx = 2.068 Mg m^−3
a = 9.7014 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.3257 (3) Å	Cell parameters from 6144 reflections
c = 17.8823 (5) Å	θ = 1.1–25.1°
α = 85.994 (1)°	µ = 7.10 mm^−1
β = 86.487 (1)°	T = 293 K
γ = 83.405 (1)°	Prism, yellow
V = 1772.57 (9) Å^3	0.78 × 0.36 × 0.34 mm

Data collection

Siemens SMART CCD diffractometer	6185 independent reflections
Radiation source: fine-focus sealed tube	5245 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.027
ϕ and ω scans	θmax = 25.1°, θmin = 1.1°
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996)	h = −11→11
Tmin = 0.040, Tmax = 0.090	k = −12→12
9243 measured reflections	l = −16→21

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.038	H-atom parameters constrained
wR(F^2) = 0.109	w = 1/[σ^2(Fo^2) + (0.0571P)^2 + 6.9595P] where P = (Fo^2 + 2Fc^2)/3
S = 1.13	(Δ/σ)max = 0.001
6185 reflections	Δρmax = 1.35 e Å^−3
470 parameters	Δρmin = −2.22 e Å^−3
2 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0061 (3)

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Re1	0.23301 (3)	0.35079 (3)	0.118705 (16)	0.03192 (13)
Re2	0.15717 (3)	0.76402 (3)	0.183675 (17)	0.03283 (13)
Cl1	0.7755 (2)	0.9347 (3)	0.41867 (13)	0.0577 (6)
Cl01	0.9287 (7)	0.5067 (7)	0.4318 (3)	0.165 (2)
S1	0.3060 (2)	0.54781 (19)	0.17589 (12)	0.0395 (5)
O1	0.9039 (8)	0.9347 (13)	0.4489 (5)	0.103 (3)
O2	0.7146 (19)	1.0619 (16)	0.4113 (7)	0.185 (8)
O3	0.6930 (14)	0.8636 (16)	0.4680 (6)	0.153 (6)
O4	0.7887 (10)	0.8881 (11)	0.3464 (5)	0.101 (3)
O41	0.3514 (8)	0.4635 (8)	−0.0321 (4)	0.067 (2)
O42	−0.0584 (7)	0.4842 (8)	0.0873 (4)	0.066 (2)
O43	0.1710 (7)	0.1101 (7)	0.0409 (4)	0.0607 (18)
O44	−0.1020 (8)	0.6347 (8)	0.2383 (5)	0.076 (2)
O45	0.0975 (9)	0.7444 (8)	0.0182 (4)	0.075 (2)
O46	−0.0191 (8)	1.0292 (7)	0.1803 (5)	0.069 (2)
N1	0.1775 (7)	0.2675 (6)	0.2301 (4)	0.0349 (14)
N2	0.4270 (7)	0.2563 (6)	0.1601 (4)	0.0333 (14)
N3	0.2380 (7)	0.7876 (6)	0.2920 (4)	0.0375 (15)
N4	0.3602 (7)	0.8304 (6)	0.1593 (4)	0.0392 (16)
C1	0.0491 (10)	0.2718 (10)	0.2612 (5)	0.049 (2)
H1B	−0.0229	0.3167	0.2346	0.059*
C01	1.048 (3)	0.4087 (18)	0.4885 (11)	0.129 (13)	0.50
H01A	1.0124	0.3262	0.5037	0.155*	0.50
H01B	1.1360	0.3906	0.4605	0.155*	0.50
C2	0.0169 (11)	0.2133 (11)	0.3305 (6)	0.060 (3)
H2B	−0.0743	0.2199	0.3503	0.072*
C3	0.1206 (12)	0.1458 (11)	0.3695 (6)	0.061 (3)
H3A	0.1013	0.1039	0.4161	0.074*
C4	0.2552 (11)	0.1402 (9)	0.3390 (5)	0.052 (2)
H4A	0.3274	0.0955	0.3655	0.062*
C5	0.2834 (9)	0.2011 (8)	0.2687 (5)	0.0406 (19)
C6	0.4218 (9)	0.2005 (7)	0.2310 (5)	0.0386 (18)
C7	0.5433 (10)	0.1496 (8)	0.2667 (6)	0.049 (2)
H7A	0.5391	0.1134	0.3158	0.059*
C8	0.6690 (10)	0.1549 (10)	0.2265 (6)	0.057 (3)
H8A	0.7506	0.1186	0.2481	0.068*
C9	0.6750 (9)	0.2126 (10)	0.1556 (6)	0.053 (2)
H9A	0.7601	0.2183	0.1293	0.064*
C10	0.5522 (9)	0.2626 (8)	0.1234 (5)	0.043 (2)
H10A	0.5561	0.3017	0.0750	0.052*
C11	0.1649 (11)	0.7839 (10)	0.3581 (5)	0.055 (2)
H11A	0.0708	0.7737	0.3588	0.066*
C12	0.2240 (12)	0.7948 (11)	0.4246 (5)	0.060 (3)
H12A	0.1697	0.7933	0.4693	0.072*
C13	0.3629 (11)	0.8079 (10)	0.4255 (6)	0.058 (3)
H13A	0.4045	0.8132	0.4706	0.070*
C14	0.4390 (12)	0.8129 (10)	0.3583 (6)	0.057 (3)
H14A	0.5335	0.8217	0.3573	0.068*
C15	0.3748 (9)	0.8049 (8)	0.2923 (5)	0.0404 (19)
C16	0.4443 (8)	0.8242 (7)	0.2171 (5)	0.0368 (18)
C17	0.5850 (10)	0.8386 (10)	0.2051 (6)	0.056 (2)
H17A	0.6420	0.8329	0.2454	0.067*
C18	0.6391 (11)	0.8614 (11)	0.1329 (7)	0.068 (3)
H18A	0.7333	0.8692	0.1240	0.082*
C19	0.5522 (10)	0.8725 (10)	0.0741 (6)	0.056 (3)
H19A	0.5865	0.8907	0.0252	0.068*
C20	0.4139 (10)	0.8564 (9)	0.0886 (6)	0.050 (2)
H20A	0.3556	0.8636	0.0488	0.060*
C31	0.3972 (9)	0.5039 (8)	0.2596 (5)	0.042 (2)
C32	0.5397 (10)	0.5029 (8)	0.2540 (6)	0.048 (2)
H32A	0.5846	0.5238	0.2081	0.057*
C33	0.6151 (12)	0.4711 (12)	0.3166 (7)	0.071 (3)
H33A	0.7109	0.4730	0.3135	0.085*
C34	0.5480 (15)	0.4364 (13)	0.3838 (7)	0.080 (4)
H34A	0.5999	0.4115	0.4255	0.096*
C35	0.4066 (15)	0.4378 (12)	0.3906 (6)	0.073 (3)
H35A	0.3621	0.4161	0.4366	0.088*
C36	0.3311 (11)	0.4722 (9)	0.3276 (6)	0.054 (2)
H36A	0.2349	0.4739	0.3312	0.064*
C41	0.3039 (9)	0.4233 (9)	0.0241 (5)	0.043 (2)
C42	0.0515 (9)	0.4352 (8)	0.0971 (4)	0.0389 (18)
C43	0.1935 (8)	0.2010 (9)	0.0702 (5)	0.0421 (19)
C44	−0.0066 (9)	0.6835 (9)	0.2178 (5)	0.047 (2)
C45	0.1166 (10)	0.7502 (9)	0.0816 (5)	0.047 (2)
C46	0.0491 (9)	0.9316 (8)	0.1822 (5)	0.0427 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re1	0.0340 (2)	0.0352 (2)	0.02719 (19)	−0.00303 (13)	−0.00627 (13)	−0.00376 (13)
Re2	0.03205 (19)	0.0353 (2)	0.0314 (2)	0.00023 (13)	−0.00579 (13)	−0.00696 (13)
Cl1	0.0447 (12)	0.0912 (19)	0.0398 (12)	−0.0113 (12)	−0.0107 (10)	−0.0097 (12)
Cl01	0.169 (5)	0.201 (6)	0.135 (5)	−0.036 (5)	−0.056 (4)	−0.022 (4)
S1	0.0456 (11)	0.0343 (10)	0.0392 (11)	0.0019 (9)	−0.0140 (9)	−0.0086 (8)
O1	0.055 (5)	0.206 (11)	0.056 (5)	−0.043 (6)	−0.012 (4)	−0.012 (6)
O2	0.259 (18)	0.184 (13)	0.089 (8)	0.119 (13)	−0.054 (10)	−0.047 (9)
O3	0.133 (10)	0.256 (17)	0.092 (8)	−0.126 (11)	−0.006 (7)	0.010 (9)
O4	0.099 (7)	0.144 (8)	0.065 (6)	0.000 (6)	−0.023 (5)	−0.047 (6)
O41	0.061 (4)	0.091 (5)	0.048 (4)	−0.022 (4)	−0.005 (3)	0.016 (4)
O42	0.048 (4)	0.081 (5)	0.069 (5)	0.013 (4)	−0.026 (4)	−0.014 (4)
O43	0.067 (4)	0.051 (4)	0.070 (5)	−0.017 (3)	−0.001 (4)	−0.029 (4)
O44	0.065 (5)	0.096 (6)	0.072 (5)	−0.038 (4)	0.012 (4)	−0.015 (4)
O45	0.093 (6)	0.097 (6)	0.038 (4)	−0.003 (5)	−0.032 (4)	−0.005 (4)
O46	0.062 (4)	0.052 (4)	0.087 (6)	0.021 (4)	0.006 (4)	−0.011 (4)
N1	0.039 (4)	0.037 (3)	0.029 (3)	−0.005 (3)	0.000 (3)	−0.006 (3)
N2	0.038 (4)	0.028 (3)	0.034 (4)	−0.001 (3)	−0.005 (3)	−0.001 (3)
N3	0.043 (4)	0.037 (4)	0.032 (4)	0.001 (3)	−0.004 (3)	−0.011 (3)
N4	0.036 (4)	0.034 (3)	0.048 (4)	−0.001 (3)	−0.007 (3)	−0.009 (3)
C1	0.047 (5)	0.066 (6)	0.037 (5)	−0.017 (4)	−0.003 (4)	−0.005 (4)
C01	0.13 (3)	0.17 (4)	0.09 (2)	−0.02 (3)	0.01 (2)	−0.02 (2)
C2	0.060 (6)	0.074 (7)	0.049 (6)	−0.024 (5)	0.004 (5)	−0.009 (5)
C3	0.080 (7)	0.069 (7)	0.037 (5)	−0.024 (6)	0.012 (5)	−0.003 (5)
C4	0.071 (6)	0.046 (5)	0.037 (5)	−0.009 (5)	−0.007 (5)	0.006 (4)
C5	0.055 (5)	0.038 (4)	0.031 (4)	−0.011 (4)	−0.011 (4)	0.002 (3)
C6	0.044 (5)	0.030 (4)	0.041 (5)	0.000 (3)	−0.006 (4)	−0.005 (3)
C7	0.053 (5)	0.039 (5)	0.053 (6)	0.004 (4)	−0.023 (4)	0.006 (4)
C8	0.047 (5)	0.054 (6)	0.069 (7)	0.005 (4)	−0.020 (5)	−0.001 (5)
C9	0.036 (5)	0.064 (6)	0.059 (6)	0.001 (4)	0.001 (4)	−0.015 (5)
C10	0.044 (5)	0.046 (5)	0.039 (5)	−0.002 (4)	0.002 (4)	−0.011 (4)
C11	0.059 (6)	0.070 (6)	0.036 (5)	−0.001 (5)	0.005 (4)	−0.011 (4)
C12	0.077 (7)	0.071 (7)	0.032 (5)	−0.008 (6)	0.005 (5)	−0.017 (5)
C13	0.068 (7)	0.070 (7)	0.038 (5)	−0.010 (5)	−0.013 (5)	−0.007 (5)
C14	0.065 (6)	0.053 (6)	0.057 (6)	−0.010 (5)	−0.019 (5)	−0.011 (5)
C15	0.046 (5)	0.035 (4)	0.043 (5)	−0.002 (4)	−0.013 (4)	−0.016 (4)
C16	0.040 (4)	0.031 (4)	0.041 (5)	−0.008 (3)	−0.005 (4)	−0.007 (3)
C17	0.044 (5)	0.057 (6)	0.071 (7)	−0.010 (4)	−0.009 (5)	−0.014 (5)
C18	0.046 (6)	0.072 (7)	0.087 (9)	−0.013 (5)	0.008 (6)	−0.013 (6)
C19	0.054 (6)	0.066 (6)	0.046 (6)	−0.009 (5)	0.022 (5)	0.000 (5)
C20	0.052 (5)	0.046 (5)	0.051 (6)	0.002 (4)	−0.004 (4)	−0.006 (4)
C31	0.049 (5)	0.034 (4)	0.043 (5)	−0.003 (4)	−0.020 (4)	−0.004 (4)
C32	0.049 (5)	0.038 (5)	0.056 (6)	−0.002 (4)	−0.012 (4)	−0.005 (4)
C33	0.059 (7)	0.075 (8)	0.083 (9)	−0.006 (6)	−0.033 (6)	−0.011 (6)
C34	0.092 (9)	0.086 (8)	0.068 (8)	−0.006 (7)	−0.056 (7)	−0.007 (6)
C35	0.102 (10)	0.076 (8)	0.043 (6)	−0.015 (7)	−0.019 (6)	−0.002 (5)
C36	0.064 (6)	0.052 (5)	0.050 (6)	−0.015 (5)	−0.017 (5)	−0.005 (4)
C41	0.037 (4)	0.051 (5)	0.044 (5)	−0.005 (4)	−0.006 (4)	−0.003 (4)
C42	0.046 (5)	0.043 (5)	0.031 (4)	−0.005 (4)	−0.014 (4)	−0.007 (3)
C43	0.033 (4)	0.049 (5)	0.044 (5)	−0.005 (4)	0.006 (4)	−0.012 (4)
C44	0.044 (5)	0.052 (5)	0.046 (5)	−0.009 (4)	−0.003 (4)	−0.010 (4)
C45	0.050 (5)	0.041 (5)	0.050 (6)	−0.002 (4)	−0.015 (4)	−0.002 (4)
C46	0.039 (4)	0.040 (5)	0.050 (5)	0.002 (4)	−0.007 (4)	−0.009 (4)

Geometric parameters (Å, º)

Re1—C43	1.912 (9)	C3—H3A	0.9300
Re1—C41	1.921 (9)	C4—C5	1.392 (12)
Re1—C42	1.922 (9)	C4—H4A	0.9300
Re1—N2	2.165 (6)	C5—C6	1.464 (12)
Re1—N1	2.175 (6)	C6—C7	1.406 (12)
Re1—S1	2.529 (2)	C7—C8	1.382 (14)
Re2—C45	1.909 (9)	C7—H7A	0.9300
Re2—C46	1.917 (8)	C8—C9	1.364 (14)
Re2—C44	1.924 (9)	C8—H8A	0.9300
Re2—N4	2.169 (7)	C9—C10	1.385 (13)
Re2—N3	2.173 (7)	C9—H9A	0.9300
Re2—S1	2.523 (2)	C10—H10A	0.9300
Cl1—O2	1.378 (13)	C11—C12	1.368 (14)
Cl1—O3	1.385 (11)	C11—H11A	0.9300
Cl1—O1	1.387 (8)	C12—C13	1.372 (15)
Cl1—O4	1.403 (8)	C12—H12A	0.9300
Cl01—C01^i	1.763 (5)	C13—C14	1.372 (14)
Cl01—C01	1.766 (5)	C13—H13A	0.9300
S1—C31	1.791 (8)	C14—C15	1.380 (12)
O41—C41	1.151 (11)	C14—H14A	0.9300
O42—C42	1.144 (10)	C15—C16	1.479 (12)
O43—C43	1.154 (10)	C16—C17	1.392 (12)
O44—C44	1.133 (11)	C17—C18	1.378 (16)
O45—C45	1.167 (11)	C17—H17A	0.9300
O46—C46	1.140 (10)	C18—C19	1.379 (16)
N1—C1	1.331 (11)	C18—H18A	0.9300
N1—C5	1.364 (11)	C19—C20	1.377 (13)
N2—C10	1.351 (11)	C19—H19A	0.9300
N2—C6	1.357 (10)	C20—H20A	0.9300
N3—C11	1.341 (11)	C31—C36	1.376 (14)
N3—C15	1.359 (11)	C31—C32	1.379 (13)
N4—C16	1.349 (11)	C32—C33	1.373 (14)
N4—C20	1.359 (12)	C32—H32A	0.9300
C1—C2	1.374 (13)	C33—C34	1.377 (18)
C1—H1B	0.9300	C33—H33A	0.9300
C01—Cl01^i	1.763 (5)	C34—C35	1.368 (18)
C01—H01A	0.9700	C34—H34A	0.9300
C01—H01B	0.9700	C35—C36	1.385 (14)
C2—C3	1.357 (16)	C35—H35A	0.9300
C2—H2B	0.9300	C36—H36A	0.9300
C3—C4	1.380 (15)
C43—Re1—C41	89.5 (4)	N1—C5—C6	115.4 (7)
C43—Re1—C42	89.6 (3)	C4—C5—C6	124.8 (8)
C41—Re1—C42	89.2 (4)	N2—C6—C7	121.5 (8)
C43—Re1—N2	93.9 (3)	N2—C6—C5	116.1 (7)
C41—Re1—N2	98.5 (3)	C7—C6—C5	122.4 (8)
C42—Re1—N2	171.6 (3)	C8—C7—C6	117.9 (9)
C43—Re1—N1	93.3 (3)	C8—C7—H7A	121.0
C41—Re1—N1	173.3 (3)	C6—C7—H7A	121.0
C42—Re1—N1	97.0 (3)	C9—C8—C7	120.8 (9)
N2—Re1—N1	75.3 (2)	C9—C8—H8A	119.6
C43—Re1—S1	174.8 (2)	C7—C8—H8A	119.6
C41—Re1—S1	86.6 (3)	C8—C9—C10	118.8 (9)
C42—Re1—S1	93.9 (2)	C8—C9—H9A	120.6
N2—Re1—S1	83.18 (17)	C10—C9—H9A	120.6
N1—Re1—S1	90.15 (17)	N2—C10—C9	122.1 (8)
C45—Re2—C46	89.2 (4)	N2—C10—H10A	118.9
C45—Re2—C44	90.7 (4)	C9—C10—H10A	118.9
C46—Re2—C44	89.5 (4)	N3—C11—C12	122.2 (10)
C45—Re2—N4	96.0 (3)	N3—C11—H11A	118.9
C46—Re2—N4	98.1 (3)	C12—C11—H11A	118.9
C44—Re2—N4	169.9 (3)	C11—C12—C13	120.3 (9)
C45—Re2—N3	170.2 (3)	C11—C12—H12A	119.9
C46—Re2—N3	93.0 (3)	C13—C12—H12A	119.9
C44—Re2—N3	98.9 (3)	C12—C13—C14	118.3 (9)
N4—Re2—N3	74.2 (3)	C12—C13—H13A	120.9
C45—Re2—S1	87.5 (3)	C14—C13—H13A	120.9
C46—Re2—S1	175.8 (3)	C13—C14—C15	119.7 (10)
C44—Re2—S1	93.2 (3)	C13—C14—H14A	120.2
N4—Re2—S1	79.59 (18)	C15—C14—H14A	120.2
N3—Re2—S1	89.80 (18)	N3—C15—C14	121.7 (9)
O2—Cl1—O3	108.8 (11)	N3—C15—C16	114.7 (7)
O2—Cl1—O1	108.3 (10)	C14—C15—C16	123.4 (8)
O3—Cl1—O1	108.6 (7)	N4—C16—C17	121.2 (8)
O2—Cl1—O4	106.7 (7)	N4—C16—C15	115.0 (7)
O3—Cl1—O4	112.6 (8)	C17—C16—C15	123.7 (8)
O1—Cl1—O4	111.7 (6)	C18—C17—C16	119.4 (10)
C01^i—Cl01—C01	71.5 (7)	C18—C17—H17A	120.3
C31—S1—Re2	111.8 (3)	C16—C17—H17A	120.3
C31—S1—Re1	112.1 (3)	C17—C18—C19	119.4 (9)
Re2—S1—Re1	124.35 (8)	C17—C18—H18A	120.3
C1—N1—C5	118.5 (7)	C19—C18—H18A	120.3
C1—N1—Re1	125.1 (6)	C20—C19—C18	119.2 (9)
C5—N1—Re1	116.4 (5)	C20—C19—H19A	120.4
C10—N2—C6	118.8 (7)	C18—C19—H19A	120.4
C10—N2—Re1	124.2 (5)	N4—C20—C19	122.0 (9)
C6—N2—Re1	116.6 (5)	N4—C20—H20A	119.0
C11—N3—C15	117.8 (8)	C19—C20—H20A	119.0
C11—N3—Re2	125.4 (6)	C36—C31—C32	120.0 (8)
C15—N3—Re2	116.8 (5)	C36—C31—S1	122.8 (7)
C16—N4—C20	118.8 (7)	C32—C31—S1	117.2 (7)
C16—N4—Re2	116.7 (6)	C33—C32—C31	119.8 (10)
C20—N4—Re2	123.5 (6)	C33—C32—H32A	120.1
N1—C1—C2	123.6 (9)	C31—C32—H32A	120.1
N1—C1—H1B	118.2	C32—C33—C34	119.6 (11)
C2—C1—H1B	118.2	C32—C33—H33A	120.2
Cl01^i—C01—Cl01	108.5 (7)	C34—C33—H33A	120.2
Cl01^i—C01—H01A	110.0	C35—C34—C33	121.4 (10)
Cl01—C01—H01A	110.0	C35—C34—H34A	119.3
Cl01^i—C01—H01B	110.0	C33—C34—H34A	119.3
Cl01—C01—H01B	110.0	C34—C35—C36	118.6 (11)
H01A—C01—H01B	108.4	C34—C35—H35A	120.7
C3—C2—C1	118.8 (10)	C36—C35—H35A	120.7
C3—C2—H2B	120.6	C31—C36—C35	120.5 (10)
C1—C2—H2B	120.6	C31—C36—H36A	119.7
C2—C3—C4	119.0 (9)	C35—C36—H36A	119.7
C2—C3—H3A	120.5	O41—C41—Re1	177.2 (8)
C4—C3—H3A	120.5	O42—C42—Re1	177.1 (8)
C3—C4—C5	120.4 (10)	O43—C43—Re1	179.3 (8)
C3—C4—H4A	119.8	O44—C44—Re2	179.2 (10)
C5—C4—H4A	119.8	O45—C45—Re2	176.8 (9)
N1—C5—C4	119.7 (8)	O46—C46—Re2	177.5 (8)

Symmetry code: (i) −x+2, −y+1, −z+1.