fac-Trichloro(quinolin-8-ylimido-N,N′)(triphenylphosphine-P)rhenium(V)

The Re atom in [Re(C₉H₆N₂)Cl₃(C₁₈H₁₅P)] is octahedrally coordinated by three Cl atoms in facial positions, two N atoms from 8-imido­quinoline (imq) and one P atom from tri­phenyl­phosphine. The Re—N(imido) distance [1.760 (9) and 1.772 (8) Å] for imq is very short and implies double-bond character. The trans influence of the P atom is indicated. Intra- and intermolecular π–π interactions between the π-rings in the complex are also observed.

S1. Comment

Since the first arylimido Re complex, [ReCl₃(NPh)(PEt₂Ph)₂] (Ph = phenyl, Et = ethyl), was synthesized using aniline as the source of the imido-type ligand (Chatt & Rowe, 1962), many analogous complexes have been reported (Refosco et al., 1998). In complexes with such monodentate arylimido ligands, the coordinated nitrogen atom is fully deprotonated and the very short Re—N(imido) distances are observed. On the other hand, the Re complexes with the polydentate arylimido ligand are still rare. For example, the complexes with 8-imidoquinoline (imq) have not been obtained, but the complex with 8-amidoquinoline, [ReO(Himq)₂(PPh₃)]BPh₄, was formed by the reaction of [ReOCl₃(PPh₃)₂] with 8-aminoquinoline (H₂imq) (Ahmet et al., 1995). In this work, we report the structure of the Re complex with imq, [ReCl₃(imq)(PPh₃)], (I). There are two crystallographically independent complex molecules in an asymmetric unit that are related by an approximate c glide. A perspective drawing of one of the molecules is shown in Fig. 1, and the selected bond distances and angles are listed in Table 1. The crystal structures consist of neutral molecules, in which each central Re atom is octahedrally surrounded by an imq, a PPh₃ and three Cl^- ligands. The Cl^- ligands coordinate facially to the Re atom, and imq ligand acts as a bidentate ligand. \sch

The bond distances and angles in the crystallographically independent molecules 1 and 2 are similar to each other (Table 1). One of the Re—N distances [Re(m)—N(m2)] for imq is significantly shorter than the other. This is inconsistent with the fact that the M—N(amine) and M—N(quinoline ring) distances for H₂imq are similar to each other (M = Zn; Kerr et al., 1981 or M = Sn; Hazell et al., 1997), in which both M—N distances exhibit the single bonding behavior. The Re—N(amido) distances for the Re complex with the partially deprotonated H_imq, [ReO(Himq)₂(PPh₃)]BPh₄, are 1.958 (6) and 2.028 (6) Å (Ahmet et al., 1995). Similar distances were observed for the Re complexes containing the partially deprotonated amido N atoms of aminophenyl derivatives [1.988 (4) Å; Ahmet et al., 1995, or 1.973 (7) Å; Refosco et al., 1995], and of the 3- or 4-nitro-1,2-diaminobenzene [1.96 (2)–1.98 (3) Å; Bandoli et al., 2000]. On the other hand, the short Re—N(imido) distances were observed for the Re complexes containing the fully deprotonated imido nitrogen atoms of aminophenyl derivatives [1.757 (4) Å; Ahmet et al., 1995, or 1.780 (7) Å; Refosco et al., 1995]. Further, the Re(m)—N(m2)-C(m26) angles are some larger than the corresponding angles [117.4 (5) and 120.3 (5)°] of the complex with the amido-type Himq (Ahmet et al., 1995). Accordingly, the Re—N(imido) bond for imq seems to have a double-bond character and the Re—N(quinoline ring) bond has a normal single-bond, that is, this suggests that two protons of the amino group in H₂imq are fully deprotonated, indicating that the Re atom in this complex is pentavalent. In addition, the Re(m)—Cl(m1) distance occupying the trans position of the P atom is longer than those occupying the other two cis positions. This indicates obviously the trans influence for the P atom in PPh₃.

In the bond angles around the Re atom concerning imq, the Cl(m3)-Re(m)—N(m2) angle is significantly deviated from 180° (Table 1) for the ideal octahedral geometry. This seems to depend on not only the acute bite angle and the Re—N(imido) double bonding of imq, but also the interaction between the aromatic rings of PPh₃ and imq. The torsion angle for N(m1)-Re(m)—P(m)—C(m13) torsion angle is 16.8 (4)° in 1 and 16.4 (4)° in 2, and the closest Nm1—Cm14 distance is 3.15 (1) Å in 1 and 3.11 (1) Å in 2. These facts suggest that the two aromatic π-rings, which are almost parallel, overlap each other, and the intramolecular π-π interactions exist between their π-rings. Furthermore, imq ligands in the two molecules are almost parallel and their distances are about 3.5 Å. Similar distances were observed for the tetranuclear Pd^II complexes with 2,2'-bipyridine, indicating the π-π stacking contacts (Yamada & Okamato, 1999; Yamada et al., 2000). Accordingly, these facts seem to indicate that the intermolecular π-π interactions also exist between imq ligands for two complex molecules in the unit cell.

Related literature

For related literature, see: Ahmet et al. (1995); Bandoli et al. (2000); Chatt & Rowe (1962); Hazell et al. (1997); Johnson et al. (1967); Kerr et al. (1981); Refosco et al. (1995, 1998); Yamada et al. (2000).

S2. Experimental

To a solution containing [ReOCl₃(PPh₃)₂] (2.08 g, 2.50 mmol) (Johnson et al., 1967) in toluene (100 cm³) was added a solution containing 8-aminoquinoline (0.518 g, 3.59 mmol) in toluene (38 cm³). This mixture was stirred at 298 K for 1 d and the unreacted materials were filtered off. When the dark red solution was stood at 298 K for 2 weeks, the dark red microcrystals appeared (yield 0.10 g). Found: C 47.04, H 3.30, N 4.00%. Calculated for [Re(C₉H₆N₂)Cl₃(C₁₈H₁₅P)]: C 46.53, H 3.04, N 4.02%. The crystals suitable for X-ray analysis were obtained by the recrystallization from acetonitrile at 298 K.

S3. Refinement

After checking their presence in the difference map, all H atoms were fixed geometrically and allowed to ride on their attached atoms [C—H = N—H = 0.95 Å; U = 1.3U(C,N)]. The major features in the final difference map area associated with the Re atoms.

Computing details

Data collection: WinAFC; cell refinement: WinAFC; data reduction: TEXSAN (Molecular Structure Corporation, Rigaku Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.

Figures

Fig. 1. A view of molecule 1 with the atomic numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. Molecule 2 has the corresponding numbering scheme, in which the number after each atom is `2' or `2n' as shown in molecule 1.

(I)

Crystal data

[Re(C9H6N2)Cl3(C18H15P)]	Dx = 1.827 Mg m^−3
Mr = 697.02	Mo Kα radiation, λ = 0.7107 Å
Monoclinic, P21/a	Cell parameters from 25 reflections
a = 17.624 (5) Å	θ = 11.1–14.4°
b = 27.665 (5) Å	µ = 5.20 mm^−1
c = 10.428 (3) Å	T = 296 K
β = 94.52 (2)°	Prismatic, brown
V = 5068 (2) Å^3	0.38 × 0.15 × 0.15 mm
Z = 8

Data collection

Rigaku AFC7S diffractometer	Rint = 0.035
ω scans	θmax = 27.5°
Absorption correction: ψ scan (North et al., 1968)	h = 0→22
Tmin = 0.37, Tmax = 0.46	k = 0→35
12687 measured reflections	l = −13→13
12409 independent reflections	3 standard reflections every 150 reflections
7306 reflections with F^2 > 2.0σ(F^2)	intensity decay: 2.1%

Refinement

Refinement on F^2	w = 1/[σ^2(Fo^2) + 0.04P^2] where P = Max(Fo^2) + 2Fc^2)/3)
R[F^2 > 2σ(F^2)] = 0.048	(Δ/σ)max = 0.001
wR(F^2) = 0.127	Δρmax = 1.81 e Å^−3
S = 0.97	Δρmin = −1.94 e Å^−3
11631 reflections	Extinction correction: Zachariasen (1967) type 2 Gaussian isotropic
614 parameters	Extinction coefficient: 0.00014 (4)
H-atom parameters not refined

Special details

Refinement. Refinement using reflections with F² > -10.0 σ(F²). The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 σ(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Re1	0.20931 (2)	−0.12103 (1)	0.88507 (4)	0.03209 (9)
Re2	0.31012 (2)	0.04994 (1)	0.61427 (4)	0.03001 (9)
Cl11	0.1181 (1)	−0.05571 (9)	0.8886 (3)	0.0500 (7)
Cl12	0.1729 (2)	−0.1307 (1)	0.6652 (2)	0.0499 (8)
Cl13	0.1171 (1)	−0.17143 (9)	0.9680 (3)	0.0467 (7)
Cl21	0.4025 (2)	−0.01421 (10)	0.6184 (3)	0.0520 (8)
Cl22	0.3412 (2)	0.06117 (10)	0.8358 (2)	0.0474 (7)
Cl23	0.4028 (1)	0.10187 (9)	0.5395 (3)	0.0460 (7)
P1	0.2862 (1)	−0.19401 (9)	0.8777 (2)	0.0305 (6)
P2	0.2272 (1)	0.12094 (8)	0.6158 (2)	0.0298 (6)
N11	0.2411 (4)	−0.1080 (3)	1.0908 (8)	0.037 (2)
N12	0.2942 (5)	−0.0873 (3)	0.8896 (9)	0.047 (3)
N21	0.2833 (4)	0.0365 (3)	0.4072 (8)	0.035 (2)
N22	0.2258 (5)	0.0148 (3)	0.6052 (8)	0.040 (2)
C101	0.3488 (5)	−0.1980 (4)	0.7454 (9)	0.037 (3)
C102	0.3693 (5)	−0.1576 (4)	0.6782 (10)	0.046 (3)
C103	0.4263 (7)	−0.1624 (5)	0.592 (1)	0.065 (4)
C104	0.4595 (7)	−0.2063 (6)	0.574 (1)	0.074 (5)
C105	0.4395 (6)	−0.2455 (5)	0.638 (1)	0.059 (4)
C106	0.3828 (6)	−0.2418 (4)	0.725 (1)	0.047 (3)
C107	0.2349 (5)	−0.2509 (3)	0.8736 (9)	0.037 (3)
C108	0.1740 (7)	−0.2574 (4)	0.786 (1)	0.059 (4)
C109	0.1328 (6)	−0.2995 (4)	0.779 (1)	0.069 (4)
C110	0.1529 (7)	−0.3368 (4)	0.864 (1)	0.060 (4)
C111	0.2141 (7)	−0.3323 (4)	0.950 (1)	0.052 (3)
C112	0.2563 (6)	−0.2888 (4)	0.955 (1)	0.052 (3)
C113	0.3544 (5)	−0.1958 (3)	1.0176 (9)	0.036 (2)
C114	0.3318 (5)	−0.2051 (3)	1.1383 (9)	0.036 (3)
C115	0.3797 (6)	−0.2000 (4)	1.2473 (10)	0.042 (3)
C116	0.4544 (6)	−0.1839 (4)	1.236 (1)	0.053 (3)
C117	0.4778 (6)	−0.1734 (4)	1.116 (1)	0.054 (3)
C118	0.4287 (6)	−0.1794 (4)	1.007 (1)	0.045 (3)
C119	0.2080 (6)	−0.1190 (4)	1.198 (1)	0.049 (3)
C120	0.2397 (8)	−0.1087 (4)	1.322 (1)	0.062 (4)
C121	0.3080 (8)	−0.0880 (4)	1.340 (1)	0.059 (4)
C122	0.3491 (6)	−0.0754 (4)	1.230 (1)	0.061 (4)
C123	0.4213 (8)	−0.0539 (4)	1.228 (1)	0.070 (4)
C124	0.4525 (7)	−0.0431 (4)	1.117 (2)	0.077 (5)
C125	0.4120 (6)	−0.0514 (4)	0.997 (1)	0.059 (4)
C126	0.3427 (5)	−0.0735 (3)	0.994 (1)	0.046 (3)
C127	0.3115 (6)	−0.0860 (3)	1.109 (1)	0.042 (3)
C201	0.1622 (5)	0.1207 (3)	0.7453 (8)	0.034 (2)
C202	0.1439 (5)	0.0779 (4)	0.8058 (10)	0.039 (3)
C203	0.0832 (6)	0.0781 (4)	0.886 (1)	0.050 (3)
C204	0.0450 (6)	0.1206 (5)	0.906 (1)	0.058 (4)
C205	0.0632 (7)	0.1625 (5)	0.846 (1)	0.062 (4)
C206	0.1227 (6)	0.1627 (4)	0.765 (1)	0.052 (3)
C207	0.2733 (5)	0.1810 (3)	0.6268 (9)	0.033 (2)
C208	0.3272 (6)	0.1885 (4)	0.728 (1)	0.048 (3)
C209	0.3598 (6)	0.2339 (4)	0.742 (1)	0.056 (4)
C210	0.3421 (7)	0.2695 (4)	0.652 (1)	0.061 (4)
C211	0.2891 (8)	0.2619 (4)	0.554 (1)	0.067 (4)
C212	0.2530 (7)	0.2168 (4)	0.542 (1)	0.056 (3)
C213	0.1603 (5)	0.1235 (3)	0.4731 (9)	0.032 (2)
C214	0.1878 (6)	0.1298 (3)	0.3523 (10)	0.040 (3)
C215	0.1380 (6)	0.1279 (4)	0.2424 (10)	0.047 (3)
C216	0.0615 (7)	0.1179 (4)	0.252 (1)	0.054 (3)
C217	0.0345 (5)	0.1112 (4)	0.371 (1)	0.055 (3)
C218	0.0834 (5)	0.1131 (4)	0.4824 (10)	0.042 (3)
C219	0.3190 (6)	0.0465 (4)	0.3039 (9)	0.040 (3)
C220	0.2877 (7)	0.0373 (4)	0.1788 (10)	0.048 (3)
C221	0.2161 (7)	0.0168 (4)	0.159 (1)	0.057 (4)
C222	0.1763 (6)	0.0041 (3)	0.2640 (10)	0.040 (3)
C223	0.1043 (7)	−0.0177 (4)	0.263 (1)	0.057 (4)
C224	0.0737 (6)	−0.0307 (4)	0.373 (1)	0.065 (4)
C225	0.1098 (6)	−0.0211 (4)	0.493 (1)	0.054 (3)
C226	0.1790 (5)	0.0016 (3)	0.4977 (10)	0.037 (3)
C227	0.2134 (5)	0.0144 (3)	0.3859 (10)	0.038 (3)
H1	0.3454	−0.1273	0.6902	0.0552*
H2	0.4417	−0.1350	0.5453	0.0775*
H3	0.4979	−0.2090	0.5156	0.0884*
H4	0.4633	−0.2757	0.6242	0.0706*
H5	0.3678	−0.2697	0.7697	0.0564*
H6	0.1599	−0.2320	0.7271	0.0709*
H7	0.0907	−0.3030	0.7173	0.0833*
H8	0.1235	−0.3656	0.8622	0.0722*
H9	0.2286	−0.3581	1.0071	0.0628*
H10	0.2998	−0.2856	1.0139	0.0619*
H11	0.2810	−0.2155	1.1464	0.0435*
H12	0.3626	−0.2071	1.3293	0.0501*
H13	0.4887	−0.1804	1.3102	0.0636*
H14	0.5280	−0.1618	1.1086	0.0646*
H15	0.4455	−0.1724	0.9245	0.0545*
H16	0.1601	−0.1349	1.1892	0.0585*
H17	0.2123	−0.1164	1.3937	0.0740*
H18	0.3295	−0.0816	1.4245	0.0705*
H19	0.4492	−0.0466	1.3075	0.0845*
H20	0.5023	−0.0297	1.1207	0.0919*
H21	0.4327	−0.0418	0.9190	0.0710*
H22	0.1718	0.0492	0.7933	0.0469*
H23	0.0687	0.0491	0.9262	0.0603*
H24	0.0053	0.1208	0.9620	0.0701*
H25	0.0354	0.1913	0.8586	0.0749*
H26	0.1360	0.1918	0.7240	0.0623*
H27	0.3415	0.1632	0.7867	0.0572*
H28	0.3947	0.2406	0.8143	0.0668*
H29	0.3674	0.2998	0.6601	0.0730*
H30	0.2765	0.2867	0.4926	0.0806*
H31	0.2143	0.2113	0.4753	0.0668*
H32	0.2405	0.1355	0.3453	0.0482*
H33	0.1564	0.1334	0.1605	0.0560*
H34	0.0278	0.1156	0.1765	0.0644*
H35	−0.0182	0.1052	0.3767	0.0658*
H36	0.0646	0.1075	0.5640	0.0506*
H37	0.3682	0.0606	0.3149	0.0475*
H38	0.3157	0.0451	0.1073	0.0571*
H39	0.1942	0.0114	0.0741	0.0686*
H40	0.0763	−0.0235	0.1826	0.0680*
H41	0.0261	−0.0470	0.3678	0.0780*
H42	0.0873	−0.0299	0.5691	0.0649*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re1	0.0295 (2)	0.0312 (2)	0.0348 (2)	0.0019 (1)	−0.0030 (1)	−0.0002 (2)
Re2	0.0284 (2)	0.0304 (2)	0.0310 (2)	0.0018 (1)	0.0009 (1)	−0.0008 (2)
Cl11	0.048 (1)	0.040 (1)	0.060 (2)	0.014 (1)	−0.010 (1)	−0.008 (1)
Cl12	0.054 (2)	0.057 (2)	0.037 (1)	0.015 (1)	−0.007 (1)	−0.001 (1)
Cl13	0.035 (1)	0.041 (1)	0.065 (2)	−0.0028 (10)	0.010 (1)	−0.006 (1)
Cl21	0.048 (1)	0.050 (2)	0.058 (2)	0.017 (1)	−0.002 (1)	−0.010 (1)
Cl22	0.051 (1)	0.055 (2)	0.035 (1)	0.013 (1)	−0.005 (1)	−0.003 (1)
Cl23	0.037 (1)	0.045 (1)	0.057 (2)	−0.011 (1)	0.010 (1)	−0.006 (1)
P1	0.027 (1)	0.032 (1)	0.032 (1)	−0.0007 (9)	−0.0007 (9)	0.0007 (10)
P2	0.027 (1)	0.029 (1)	0.033 (1)	0.0012 (9)	−0.0004 (9)	0.0002 (10)
N11	0.040 (4)	0.027 (4)	0.046 (5)	0.007 (3)	0.003 (4)	−0.002 (4)
N12	0.045 (5)	0.033 (5)	0.060 (6)	0.003 (4)	−0.003 (4)	0.005 (4)
N21	0.040 (4)	0.024 (4)	0.039 (5)	−0.001 (3)	0.001 (3)	0.001 (3)
N22	0.043 (5)	0.030 (4)	0.047 (5)	−0.001 (3)	0.012 (4)	0.002 (4)
C101	0.036 (5)	0.044 (6)	0.032 (5)	0.002 (4)	0.005 (4)	−0.005 (4)
C102	0.034 (5)	0.065 (7)	0.039 (6)	0.009 (5)	0.003 (4)	0.009 (5)
C103	0.046 (7)	0.10 (1)	0.044 (7)	0.001 (7)	0.005 (5)	0.030 (7)
C104	0.046 (7)	0.15 (1)	0.028 (6)	0.025 (8)	0.003 (5)	−0.003 (7)
C105	0.041 (6)	0.080 (9)	0.058 (8)	0.001 (6)	0.018 (5)	−0.022 (7)
C106	0.047 (6)	0.045 (6)	0.049 (6)	−0.006 (5)	0.007 (5)	−0.017 (5)
C107	0.040 (5)	0.037 (5)	0.032 (5)	0.002 (4)	−0.004 (4)	−0.007 (4)
C108	0.057 (7)	0.046 (7)	0.069 (8)	0.001 (5)	−0.026 (6)	−0.006 (6)
C109	0.047 (7)	0.045 (7)	0.11 (1)	−0.006 (5)	−0.027 (7)	−0.019 (7)
C110	0.050 (7)	0.045 (7)	0.086 (10)	−0.003 (5)	0.009 (6)	−0.011 (7)
C111	0.061 (7)	0.039 (6)	0.058 (7)	−0.007 (5)	0.006 (6)	0.000 (5)
C112	0.054 (7)	0.042 (6)	0.057 (7)	−0.005 (5)	−0.002 (5)	−0.005 (5)
C113	0.042 (5)	0.030 (5)	0.035 (5)	0.002 (4)	0.001 (4)	0.003 (4)
C114	0.034 (5)	0.035 (5)	0.039 (5)	0.000 (4)	−0.002 (4)	0.004 (4)
C115	0.047 (6)	0.040 (6)	0.038 (5)	0.000 (4)	0.001 (4)	0.000 (4)
C116	0.043 (6)	0.058 (7)	0.054 (7)	0.000 (5)	−0.021 (5)	−0.002 (6)
C117	0.038 (6)	0.068 (8)	0.054 (7)	0.007 (5)	−0.002 (5)	0.011 (6)
C118	0.039 (5)	0.049 (6)	0.047 (6)	0.006 (4)	0.002 (5)	0.010 (5)
C119	0.057 (7)	0.043 (6)	0.046 (6)	−0.001 (5)	0.002 (5)	−0.007 (5)
C120	0.10 (1)	0.039 (6)	0.049 (7)	0.003 (6)	−0.005 (7)	−0.014 (5)
C121	0.094 (10)	0.041 (7)	0.038 (6)	0.026 (6)	−0.013 (6)	0.001 (5)
C122	0.045 (6)	0.026 (5)	0.10 (1)	0.011 (4)	−0.039 (7)	−0.004 (6)
C123	0.070 (9)	0.041 (7)	0.09 (1)	−0.001 (6)	−0.041 (8)	−0.001 (7)
C124	0.045 (7)	0.039 (7)	0.14 (1)	−0.019 (5)	−0.024 (8)	0.010 (8)
C125	0.043 (6)	0.042 (6)	0.091 (10)	−0.008 (5)	−0.008 (6)	0.015 (7)
C126	0.030 (5)	0.027 (5)	0.078 (8)	−0.003 (4)	−0.017 (5)	0.006 (5)
C127	0.041 (5)	0.025 (4)	0.057 (6)	−0.002 (4)	−0.012 (5)	0.008 (5)
C201	0.031 (4)	0.038 (5)	0.031 (5)	0.003 (4)	−0.004 (3)	−0.006 (4)
C202	0.032 (5)	0.043 (6)	0.042 (6)	0.009 (4)	0.000 (4)	−0.001 (5)
C203	0.043 (6)	0.072 (8)	0.037 (6)	0.005 (5)	0.008 (5)	0.006 (5)
C204	0.035 (5)	0.092 (10)	0.050 (7)	0.011 (6)	0.011 (5)	0.001 (7)
C205	0.053 (7)	0.068 (8)	0.066 (8)	0.021 (6)	0.008 (6)	−0.019 (7)
C206	0.045 (6)	0.051 (7)	0.062 (8)	0.011 (5)	0.020 (5)	0.005 (6)
C207	0.033 (5)	0.029 (5)	0.037 (5)	0.010 (4)	0.007 (4)	−0.004 (4)
C208	0.042 (6)	0.033 (5)	0.065 (7)	0.004 (4)	−0.015 (5)	0.000 (5)
C209	0.045 (6)	0.049 (7)	0.072 (8)	0.000 (5)	−0.006 (6)	−0.019 (6)
C210	0.059 (7)	0.031 (6)	0.09 (1)	−0.010 (5)	0.014 (7)	−0.016 (6)
C211	0.10 (1)	0.037 (6)	0.059 (8)	−0.011 (6)	−0.005 (7)	0.009 (6)
C212	0.070 (8)	0.035 (6)	0.058 (7)	0.000 (5)	−0.023 (6)	0.002 (5)
C213	0.034 (4)	0.029 (4)	0.034 (5)	0.003 (4)	0.002 (4)	−0.001 (4)
C214	0.050 (6)	0.030 (5)	0.040 (6)	−0.002 (4)	0.006 (4)	0.001 (4)
C215	0.058 (7)	0.043 (6)	0.038 (6)	0.005 (5)	−0.004 (5)	−0.003 (5)
C216	0.064 (7)	0.052 (7)	0.041 (6)	−0.007 (6)	−0.021 (5)	0.012 (5)
C217	0.024 (5)	0.072 (8)	0.067 (8)	−0.015 (5)	−0.009 (5)	0.006 (6)
C218	0.030 (5)	0.057 (7)	0.039 (5)	−0.008 (4)	−0.003 (4)	0.006 (5)
C219	0.049 (6)	0.036 (5)	0.036 (5)	−0.002 (4)	0.013 (4)	−0.002 (4)
C220	0.073 (8)	0.039 (6)	0.031 (5)	0.010 (5)	0.004 (5)	−0.001 (4)
C221	0.082 (9)	0.045 (7)	0.043 (7)	0.009 (6)	−0.005 (6)	−0.012 (5)
C222	0.048 (6)	0.035 (5)	0.035 (5)	0.003 (4)	−0.007 (4)	−0.011 (4)
C223	0.056 (7)	0.044 (6)	0.064 (8)	−0.005 (5)	−0.030 (6)	−0.003 (6)
C224	0.042 (6)	0.049 (7)	0.10 (1)	−0.007 (5)	−0.015 (7)	−0.012 (7)
C225	0.048 (6)	0.032 (5)	0.082 (9)	−0.010 (5)	−0.002 (6)	0.002 (6)
C226	0.041 (5)	0.030 (5)	0.040 (6)	0.001 (4)	0.000 (4)	0.003 (4)
C227	0.045 (5)	0.027 (4)	0.040 (5)	−0.011 (4)	−0.010 (4)	0.002 (4)

Geometric parameters (Å, º)

Re1—Cl11	2.421 (2)	Re2—Cl21	2.406 (3)
Re1—Cl12	2.347 (3)	Re2—Cl22	2.352 (3)
Re1—Cl13	2.356 (3)	Re2—Cl23	2.353 (2)
Re1—P1	2.436 (2)	Re2—P2	2.449 (2)
Re1—N11	2.204 (8)	Re2—N21	2.205 (8)
Re1—N12	1.760 (9)	Re2—N22	1.772 (8)
P1—C101	1.837 (9)	P2—C201	1.838 (9)
P1—C107	1.813 (10)	P2—C207	1.849 (9)
P1—C113	1.817 (9)	P2—C213	1.826 (9)
N11—C119	1.33 (1)	N21—C219	1.32 (1)
N11—C127	1.38 (1)	N21—C227	1.38 (1)
N12—C126	1.39 (1)	N22—C226	1.39 (1)
C101—C102	1.38 (1)	C201—C202	1.39 (1)
C101—C106	1.37 (1)	C201—C206	1.38 (1)
C102—C103	1.41 (1)	C202—C203	1.41 (1)
C103—C104	1.37 (2)	C203—C204	1.38 (2)
C104—C105	1.33 (2)	C204—C205	1.37 (2)
C105—C106	1.41 (1)	C205—C206	1.39 (1)
C107—C108	1.37 (1)	C207—C208	1.38 (1)
C107—C112	1.38 (1)	C207—C212	1.35 (1)
C108—C109	1.37 (1)	C208—C209	1.38 (1)
C109—C110	1.39 (2)	C209—C210	1.38 (2)
C110—C111	1.35 (2)	C210—C211	1.35 (2)
C111—C112	1.41 (1)	C211—C212	1.40 (1)
C113—C114	1.37 (1)	C213—C214	1.40 (1)
C113—C118	1.40 (1)	C213—C218	1.40 (1)
C114—C115	1.37 (1)	C214—C215	1.39 (1)
C115—C116	1.40 (1)	C215—C216	1.39 (1)
C116—C117	1.37 (2)	C216—C217	1.37 (2)
C117—C118	1.39 (1)	C217—C218	1.40 (1)
C119—C120	1.40 (1)	C219—C220	1.40 (1)
C120—C121	1.33 (2)	C220—C221	1.38 (2)
C121—C122	1.44 (2)	C221—C222	1.39 (2)
C122—C123	1.41 (2)	C222—C223	1.40 (1)
C122—C127	1.41 (1)	C222—C227	1.41 (1)
C123—C124	1.35 (2)	C223—C224	1.36 (2)
C124—C125	1.42 (2)	C224—C225	1.38 (2)
C125—C126	1.36 (1)	C225—C226	1.37 (1)
C126—C127	1.40 (2)	C226—C227	1.40 (1)
Cl11—Re1—Cl12	88.23 (9)	Cl21—Re2—Cl22	88.58 (9)
Cl11—Re1—Cl13	87.60 (9)	Cl21—Re2—Cl23	88.29 (10)
Cl11—Re1—P1	172.21 (8)	Cl21—Re2—P2	174.04 (9)
Cl11—Re1—N11	88.9 (2)	Cl21—Re2—N21	89.2 (2)
Cl11—Re1—N12	99.7 (3)	Cl21—Re2—N22	99.2 (3)
Cl12—Re1—Cl13	98.5 (1)	Cl22—Re2—Cl23	97.52 (10)
Cl12—Re1—P1	89.12 (9)	Cl22—Re2—P2	88.88 (8)
Cl12—Re1—N11	176.9 (2)	Cl22—Re2—N21	177.7 (2)
Cl12—Re1—N12	104.7 (3)	Cl22—Re2—N22	104.7 (3)
Cl13—Re1—P1	85.55 (8)	Cl23—Re2—P2	86.70 (9)
Cl13—Re1—N11	82.5 (2)	Cl23—Re2—N21	83.1 (2)
Cl13—Re1—N12	155.9 (3)	Cl23—Re2—N22	156.7 (3)
P1—Re1—N11	93.9 (2)	P2—Re2—N21	93.4 (2)
P1—Re1—N12	88.1 (3)	P2—Re2—N22	86.7 (3)
N11—Re1—N12	74.7 (4)	N21—Re2—N22	75.0 (3)
Re1—P1—C101	116.3 (3)	Re2—P2—C201	114.1 (3)
Re1—P1—C107	116.3 (3)	Re2—P2—C207	117.5 (3)
Re1—P1—C113	109.4 (3)	Re2—P2—C213	111.9 (3)
C101—P1—C107	104.9 (4)	C201—P2—C207	104.7 (4)
C101—P1—C113	101.7 (4)	C201—P2—C213	101.5 (4)
C107—P1—C113	107.0 (4)	C207—P2—C213	105.6 (4)
Re1—N11—C119	133.0 (7)	Re2—N21—C219	133.3 (7)
Re1—N11—C127	111.4 (7)	Re2—N21—C227	110.7 (6)
C119—N11—C127	115.5 (9)	C219—N21—C227	116.0 (8)
Re1—N12—C126	129.6 (8)	Re2—N22—C226	129.0 (7)
P1—C101—C102	121.9 (8)	P2—C201—C202	121.1 (7)
P1—C101—C106	117.7 (8)	P2—C201—C206	117.3 (8)
C102—C101—C106	120.0 (9)	C202—C201—C206	120.7 (9)
C101—C102—C103	118 (1)	C201—C202—C203	118.7 (9)
C102—C103—C104	120 (1)	C202—C203—C204	119 (1)
C103—C104—C105	121 (1)	C203—C204—C205	121 (1)
C104—C105—C106	119 (1)	C204—C205—C206	119 (1)
C101—C106—C105	120 (1)	C201—C206—C205	119 (1)
P1—C107—C108	119.5 (8)	P2—C207—C208	117.2 (7)
P1—C107—C112	122.2 (8)	P2—C207—C212	121.6 (8)
C108—C107—C112	118.3 (10)	C208—C207—C212	121.2 (9)
C107—C108—C109	122.2 (10)	C207—C208—C209	118.3 (10)
C108—C109—C110	119 (1)	C208—C209—C210	120 (1)
C109—C110—C111	120 (1)	C209—C210—C211	120 (1)
C110—C111—C112	119 (1)	C210—C211—C212	119.3 (10)
C107—C112—C111	120 (1)	C207—C212—C211	120 (1)
P1—C113—C114	121.3 (7)	P2—C213—C214	119.5 (7)
P1—C113—C118	119.4 (7)	P2—C213—C218	120.2 (7)
C114—C113—C118	118.4 (9)	C214—C213—C218	119.8 (9)
C113—C114—C115	122.5 (9)	C213—C214—C215	119.8 (9)
C114—C115—C116	118.9 (9)	C214—C215—C216	120.2 (10)
C115—C116—C117	119.6 (9)	C215—C216—C217	120.0 (9)
C116—C117—C118	120 (1)	C216—C217—C218	120.8 (9)
C113—C118—C117	120.0 (10)	C213—C218—C217	119.3 (9)
N11—C119—C120	123 (1)	N21—C219—C220	123.1 (9)
C119—C120—C121	120 (1)	C219—C220—C221	120.0 (10)
C120—C121—C122	119 (1)	C220—C221—C222	119.8 (10)
C121—C122—C123	128 (1)	C221—C222—C223	127 (1)
C121—C122—C127	115 (1)	C221—C222—C227	115.5 (9)
C123—C122—C127	115 (1)	C223—C222—C227	116.7 (10)
C122—C123—C124	122 (1)	C222—C223—C224	121 (1)
C123—C124—C125	120 (1)	C223—C224—C225	121 (1)
C124—C125—C126	118 (1)	C224—C225—C226	117 (1)
N12—C126—C125	129 (1)	N22—C226—C225	128 (1)
N12—C126—C127	110.3 (9)	N22—C226—C227	109.7 (8)
C125—C126—C127	120 (1)	C225—C226—C227	121.8 (10)
N11—C127—C122	124 (1)	N21—C227—C222	125.4 (9)
N11—C127—C126	113.4 (9)	N21—C227—C226	114.7 (8)
C122—C127—C126	121.8 (10)	C222—C227—C226	119.8 (9)
Re1—P1—C101—C102	19.0 (9)	N21—C227—C222—C223	−178.6 (9)
Re1—P1—C101—C106	−168.9 (7)	N21—C227—C226—N22	0 (1)
Re1—P1—C107—C108	50 (1)	N21—C227—C226—C225	−179.3 (9)
Re1—P1—C107—C112	−131.2 (8)	N22—Re2—P2—C201	56.2 (4)
Re1—P1—C113—C114	72.0 (8)	N22—Re2—P2—C207	179.3 (4)
Re1—P1—C113—C118	−96.8 (8)	N22—Re2—P2—C213	−58.4 (4)
Re1—N11—C119—C120	177.6 (8)	N22—Re2—N21—C219	−174.8 (9)
Re1—N11—C127—C122	−176.4 (8)	N22—Re2—N21—C227	7.4 (6)
Re1—N11—C127—C126	5.2 (10)	N22—C226—C225—C224	−179 (1)
Re1—N12—C126—C125	173.0 (9)	N22—C226—C227—C222	179.5 (9)
Re1—N12—C126—C127	−6 (1)	C101—P1—C107—C108	−79.5 (10)
Re2—P2—C201—C202	−20.8 (8)	C101—P1—C107—C112	98.9 (9)
Re2—P2—C201—C206	169.8 (7)	C101—P1—C113—C114	−164.5 (8)
Re2—P2—C207—C208	−54.5 (8)	C101—P1—C113—C118	26.7 (9)
Re2—P2—C207—C212	128.2 (8)	C101—C102—C103—C104	0 (1)
Re2—P2—C213—C214	−65.2 (8)	C101—C106—C105—C104	0 (1)
Re2—P2—C213—C218	106.7 (8)	C102—C101—P1—C107	149.0 (8)
Re2—N21—C219—C220	−175.2 (7)	C102—C101—P1—C113	−99.7 (9)
Re2—N21—C227—C222	174.8 (8)	C102—C101—C106—C105	1 (1)
Re2—N21—C227—C226	−5.6 (10)	C102—C103—C104—C105	0 (1)
Re2—N22—C226—C225	−172.2 (8)	C103—C102—C101—C106	−1 (1)
Re2—N22—C226—C227	8 (1)	C103—C104—C105—C106	0 (1)
Cl11—Re1—P1—C101	118.1 (7)	C106—C101—P1—C107	−38.9 (9)
Cl11—Re1—P1—C107	−6.2 (8)	C106—C101—P1—C113	72.4 (9)
Cl11—Re1—P1—C113	−127.4 (7)	C107—P1—C113—C114	−54.7 (9)
Cl11—Re1—N11—C119	77.2 (9)	C107—P1—C113—C118	136.5 (8)
Cl11—Re1—N11—C127	−106.7 (6)	C107—C108—C109—C110	0 (2)
Cl11—Re1—N12—C126	93.3 (9)	C107—C112—C111—C110	0 (1)
Cl12—Re1—P1—C101	48.0 (3)	C108—C107—P1—C113	173.0 (9)
Cl12—Re1—P1—C107	−76.3 (4)	C108—C107—C112—C111	−2 (1)
Cl12—Re1—P1—C113	162.4 (3)	C108—C109—C110—C111	−1 (2)
Cl12—Re1—N11—C119	98 (4)	C109—C108—C107—C112	2 (1)
Cl12—Re1—N11—C127	−85 (4)	C109—C110—C111—C112	1 (1)
Cl12—Re1—N12—C126	−175.9 (8)	C112—C107—P1—C113	−8 (1)
Cl13—Re1—P1—C101	146.6 (3)	C113—C114—C115—C116	0 (1)
Cl13—Re1—P1—C107	22.3 (4)	C113—C118—C117—C116	0 (1)
Cl13—Re1—P1—C113	−99.0 (3)	C114—C113—C118—C117	0 (1)
Cl13—Re1—N11—C119	−10.6 (9)	C114—C115—C116—C117	0 (1)
Cl13—Re1—N11—C127	165.6 (6)	C115—C114—C113—C118	−1 (1)
Cl13—Re1—N12—C126	−12 (1)	C115—C116—C117—C118	−1 (1)
Cl21—Re2—P2—C201	−113.4 (9)	C119—N11—C127—C122	0 (1)
Cl21—Re2—P2—C207	9 (1)	C119—N11—C127—C126	−177.9 (9)
Cl21—Re2—P2—C213	132.1 (9)	C119—C120—C121—C122	1 (1)
Cl21—Re2—N21—C219	−75.1 (9)	C120—C119—N11—C127	1 (1)
Cl21—Re2—N21—C227	107.1 (6)	C120—C121—C122—C123	−179 (1)
Cl21—Re2—N22—C226	−95.9 (8)	C120—C121—C122—C127	0 (1)
Cl22—Re2—P2—C201	−48.6 (3)	C121—C122—C123—C124	−178 (1)
Cl22—Re2—P2—C207	74.4 (4)	C121—C122—C127—C126	176.6 (9)
Cl22—Re2—P2—C213	−163.2 (3)	C122—C123—C124—C125	2 (2)
Cl22—Re2—N21—C219	−91 (5)	C122—C127—C126—C125	1 (1)
Cl22—Re2—N21—C227	90 (5)	C123—C122—C127—C126	−3 (1)
Cl22—Re2—N22—C226	173.2 (8)	C123—C124—C125—C126	−4 (1)
Cl23—Re2—P2—C201	−146.2 (3)	C124—C123—C122—C127	1 (1)
Cl23—Re2—P2—C207	−23.2 (3)	C124—C125—C126—C127	2 (1)
Cl23—Re2—P2—C213	99.2 (3)	C201—P2—C207—C208	73.3 (8)
Cl23—Re2—N21—C219	13.3 (9)	C201—P2—C207—C212	−104.0 (9)
Cl23—Re2—N21—C227	−164.5 (6)	C201—P2—C213—C214	172.7 (8)
Cl23—Re2—N22—C226	11 (1)	C201—P2—C213—C218	−15.4 (9)
P1—Re1—N11—C119	−95.6 (9)	C201—C202—C203—C204	−1 (1)
P1—Re1—N11—C127	80.6 (6)	C201—C206—C205—C204	0 (1)
P1—Re1—N12—C126	−87.4 (9)	C202—C201—P2—C207	−150.6 (7)
P1—C101—C102—C103	170.5 (8)	C202—C201—P2—C213	99.8 (8)
P1—C101—C106—C105	−170.9 (8)	C202—C201—C206—C205	0 (1)
P1—C107—C108—C109	−179 (1)	C202—C203—C204—C205	2 (1)
P1—C107—C112—C111	178.8 (9)	C203—C202—C201—C206	1 (1)
P1—C113—C114—C115	−170.5 (8)	C203—C204—C205—C206	−1 (1)
P1—C113—C118—C117	169.8 (8)	C206—C201—P2—C207	40.0 (9)
P2—Re2—N21—C219	99.5 (9)	C206—C201—P2—C213	−69.6 (9)
P2—Re2—N21—C227	−78.2 (6)	C207—P2—C213—C214	63.8 (8)
P2—Re2—N22—C226	85.2 (8)	C207—P2—C213—C218	−124.4 (8)
P2—C201—C202—C203	−167.8 (8)	C207—C208—C209—C210	−3 (1)
P2—C201—C206—C205	168.7 (9)	C207—C212—C211—C210	−2 (2)
P2—C207—C208—C209	−176.9 (8)	C208—C207—P2—C213	180.0 (8)
P2—C207—C212—C211	179.9 (10)	C208—C207—C212—C211	2 (1)
P2—C213—C214—C215	174.7 (7)	C208—C209—C210—C211	4 (2)
P2—C213—C218—C217	−174.4 (8)	C209—C208—C207—C212	0 (1)
N11—Re1—P1—C101	−131.2 (4)	C209—C210—C211—C212	0 (2)
N11—Re1—P1—C107	104.5 (4)	C212—C207—P2—C213	2.6 (10)
N11—Re1—P1—C113	−16.8 (4)	C213—C214—C215—C216	−2 (1)
N11—Re1—N12—C126	7.2 (8)	C213—C218—C217—C216	2 (1)
N11—C119—C120—C121	−2 (1)	C214—C213—C218—C217	−2 (1)
N11—C127—C122—C121	−1 (1)	C214—C215—C216—C217	1 (1)
N11—C127—C122—C123	178.6 (9)	C215—C214—C213—C218	2 (1)
N11—C127—C126—N12	0 (1)	C215—C216—C217—C218	−1 (1)
N11—C127—C126—C125	179.9 (9)	C219—N21—C227—C222	−3 (1)
N12—Re1—P1—C101	−56.7 (5)	C219—N21—C227—C226	176.2 (9)
N12—Re1—P1—C107	179.0 (5)	C219—C220—C221—C222	−1 (1)
N12—Re1—P1—C113	57.7 (5)	C220—C219—N21—C227	2 (1)
N12—Re1—N11—C119	177.5 (10)	C220—C221—C222—C223	−178 (1)
N12—Re1—N11—C127	−6.3 (6)	C220—C221—C222—C227	1 (1)
N12—C126—C125—C124	−176 (1)	C221—C222—C223—C224	176 (1)
N12—C126—C127—C122	−179.2 (9)	C221—C222—C227—C226	−178.0 (10)
N21—Re2—P2—C201	130.9 (4)	C222—C223—C224—C225	3 (1)
N21—Re2—P2—C207	−106.0 (4)	C222—C227—C226—C225	0 (1)
N21—Re2—P2—C213	16.4 (4)	C223—C222—C227—C226	1 (1)
N21—Re2—N22—C226	−9.2 (8)	C223—C224—C225—C226	−1 (1)
N21—C219—C220—C221	0 (1)	C224—C223—C222—C227	−3 (1)
N21—C227—C222—C221	1 (1)	C224—C225—C226—C227	0 (1)