[μ-6,9-Cl-8-(OMe)-6,9-(η⁵-C₅Me₅)₂-arachno-6,9,5-Rh₂SB₇H₇]

The title compound, μ-6,9-chloro-8-methoxy-6,9-bis­(η⁵-penta­methyl­cyclo­penta­dienyl)-6,9-dirhoda-5-thia-arachno-decaborane(7), [Rh₂(CH₁₀B₇OS)(C₁₀H₁₅)₂Cl], has a single Cl atom bridging the two remote rhodium `prow' vertices of an arachno ten-vertex dirhoda­thia­decaborane cluster, with Rh—­Cl distances of 2.3475 (11) and 2.3536 (11) Å, and an Rh—Cl—Rh angle of 106.82 (4)°.

S1. Comment

Since the initial structure elucidation of the arachno and nido ten-vertex skeletons in borane cluster chemistry diagrammatically depicted in (I) (Van der Mass Reddy & Lipscomb, 1959; Kasper et al., 1950), there has been a fascination with bridging the 6,9 positions across the open face, either with a single atom as in (II) or a two-atom unit as in (III), but instances of both have been surprisingly rare. Several examples of structurally characterized one-atom bridges of the arachno skeleton have been reported. These include a phosphorus-bridged unit as in the [B₁₀H₁₂-µ-6,9-(PPh₂)]^- anion (Thornton-Pett et al., 1986), a sulfur-bridged unit as in the [B₁₀H₁₂-µ-6,9-(SMe)]^- anion and related species (Binder & Hein, 1997, and references therein). Bridged nido skeletons have been structurally characterized containing an aluminium-bridged unit, [6,9-C₂B₈H₁₂-µ-6,9-{Al(OEt)Me}] (Schubert et al., 1987), a tin bridge in [6,9-C₂B₈H₁₂-µ-6,9-SnMe₂] and related species (Kennedy et al., 1992; Nestor et al., 1993), as well as a nitrogen-bridged cluster in [5,10-C₂B₈H₁₂-µ-6,9-(NH^terBu)] and related species (Janoušek et al., 1992; Dörfler et al., 2000). In this paper we now report a chlorine bridge for the arachno-6,9,5-dimetallathiadecaborane cluster compound [µ-6,9-Cl-8-(OMe)-6,9-(η⁵-C₅Me₅)₂-arachno-6,9,5-Rh₂SB₇H₇], (IV) (Figure 1). A chlorine-bridged rhodium pair has been noted previously in the eleven-vertex dimetallathiaborane [2,3-(PPh₃)₂-3-Cl-µ-2,3-Cl-µ-2^P,7^C-(Ph₂P-2-C₆H₄) -closo-2,3,1-Rh₂SB₉H₈] (Ferguson et al., 1990), although the bridged rhodium atoms are adjacent in the contiguous {RhS₂B₉} cluster [Rh—Rh distance 2.6307 (9) Å], rather than apart, as in the present compound [Rh—Rh distance 3.7748 (5) Å]. There is a bromine-bridged metals-apart example reported, in [µ-Br(CO)₆(B₃H₈)Mn₂] (Chen et al., 1980). \sch

The asymmetric unit contains approximately 0.1 molecules of disordered CH₂Cl₂ solvent. The cluster structure is seen to be of the basic ten-vertex nido/arachno boat-shaped geometry, with a rhodium centre at each of the two 6,9 `prow' positions. The two Rh atoms are linked by a bridging Cl atom. An S atom occupies one of the open-face `gunwale' positions, and there is a hydrogen bridge at the opposing interboron `gunwale' position, consistent with the general arachno ten-vertex character that is also apparent from the formal Wadian (Wade, 1976) 16-electron {2n+6} arachno electron count. The compound could also be regarded as of 11-vertex `remote arachno' cluster constitution (Porterfield et al., 1990). Using simple electron counting rules, each of the formal octahedral rhodium(III) centres has two two-electron bonding vectors which are contributed to the cluster (Kennedy, 1998; Bould et al., 1999) and three which are directed towards the {η⁵-C₅Me₅} group. The sixth vector constitutes a two-electron bond with the bridging Cl atom, and one such from each rhodium generates the bridge. The two rhodium-chlorine distances of 2.3475 (11) and 2.3536 (11) Å are similar to those in the closo twelve-vertex species mentioned above [2.437 (2) and 2.448 (2) Å], and shorter than those in the doubly bridged rhodium dimer [{RhCl₂(η⁵-C₅Me₅)}₂] from which compound (IV) was prepared [2.401 (4) Å] (Hoard & Sharpe, 1993).

S2. Experimental

The title compound was isolated, along with its 10-methoxy isomer (V) from the reaction between [(RhCl₂{η⁵-C₅Me₅})₂] (100 mg, 162 µmol) and the [tmndaH]⁺ salt of the [SB₈H₁₁]^- anion (Jones et al., 1989) (136 mg; 394 µmol; tmnda = 1,8-bisdimethylaminonaphthalene) in CH₂Cl₂ / MeOH (1:1, 30 ml) for 30 min. Filtration and repeated TLC (silica gel G) on the filtrate mixture, using CH₂Cl₂/hexane mixtures, revealed a mixture of several coloured components, from which it was possible to separate dark red (IV) (4 mg, 6 µmol, 4%) and amber (V) (10 mg, 15 µmol, 9%) in pure form (R_F 0.28 and 0.35 respectively, liquid phase CH₂Cl₂/hexane 8:2). Crystals of compound (IV) were obtained from diffusion of hexane into a solution in CH₂Cl₂. Selected NMR data for CDCl₃ solutions at 300 K {cluster resonances ordered as: assignment (¹¹B)/p.p.m. [(¹H)/p.p.m. for directly attached exo-hydrogen]}. [µ-6,9-Cl-8-(OMe)-6,9-(η⁵-C₅Me₅)₂ -arachno-6,9,5-Rh₂SB₇H₇] (IV): BH(1) +8.9 [+3.64], BH(2) -21.3 [+1.34], BH(3) +5.7 [+3.54], BH(4) -26.7 [+1.44], BH(7) +1.5 [+3.19], B(8) +27.4 [OMe substituted] and BH(10) +14.4 [+3.97], with δ(¹H)(µ-7,8) -0.19, δ(¹H)(C₅Me₅) at +1.69 and +1.56, δ(¹H)(OMe) at +3.61; [µ-6,9-Cl-10-(OMe)-6,9-(η⁵-C₅Me₅)₂ -arachno-6,9,5-Rh₂SB₇H₇] (V) BH(1) +9.5 [+4.08], BH(2) -23.5 [+1.55], BH(3) +6.7 [+3.63], BH(4) -26.0 [+1.45], BH(7) +3.9 [+3.30], BH(8) +26.0 [+1.45] and B(10) +9.5 [OMe substituted], with δ(¹H)(µ-7,8) -1.71, δ(¹H)(C₅Me₅) at +1.71 and +1.62, δ(¹H)(OMe) at +3.42; mass spectrometry (70 eV E·I.): each had a weak m/e(max) isotopomer envelope centred at 657 corresponding to the calculated molecular ion, [C₂₁H₄₀B₇Cl₁0₁S₁Rh₂]⁺, with a principal fragmentation involving loss of Cl.

S3. Refinement

The final difference Fourier map showed two areas of diffuse electron density. Attempts to model these meaningfully as disordered solvent molecules were entirely unsuccessful. The contribution of these solvent `voids' was therefore `subtracted' from the measured data using the SQUEEZE routine of PLATON (van der Sluis & Spek, 1990). This program indicated an approximate total of 23 electrons in the two sites which, assuming both voids contain disordered hexane molecules, corresponds to approximately 0.11C₆H₁₄. However, an accurate determination of the stoichiometric quantity of solvent in the crystal is not possible, so no contribution from the solvent has been included in the calculations of molecular formula, F(000) value, and calculated density. Methyl-associated hydrogen atoms were constrained to calculated positions with isotropic displacement parameters equal to 1.5 × U_eq of the parent carbon atom. Cluster-associated hydrogen atoms were either located via Fourier difference syntheses (open face) or positioned in calculated positions (five-connected vertices) and assigned isotropic displacement parameters equal to 1.2 × U_eq of the parent boron atom. Although parameters associated with these atoms were used in structure factor calculations they were not included in refinement.

Computing details

Data collection: COLLECT (Nonius, 1999); cell refinement: DENZO-SMN (Otwinowski & Minor, 1996); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: PLATON (Spek, 2000) and SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEX (McArdle, 1995); software used to prepare material for publication: WC (Thornton-Pett, 2000).

Figures

Fig. 1. Perspective view of a single molecule of (IV) drawn with 40% probability ellipsoids and with H atoms shown as small circles of artificial radius. Hydrogen atoms on the C5Me5 methyl groups are omitted for clarity.

(IV)

Crystal data

[Rh2(B7H7S)(C10H15)2(CH3O)Cl]	Dx = 1.563 Mg m^−3
Mr = 657.53	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4	Cell parameters from 37770 reflections
Hall symbol: P -4	θ = 1.0–27.5°
a = 18.1926 (2) Å	µ = 1.37 mm^−1
c = 8.4442 (1) Å	T = 150 K
V = 2794.78 (5) Å^3	Prism, dark red
Z = 4	0.60 × 0.19 × 0.15 mm
F(000) = 1328

Data collection

Nonius KappaCCD area detector diffractometer	5488 independent reflections
Radiation source: fine-focus sealed tube	5465 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.079
Detector resolution: 9.091 pixels mm^-1	θmax = 26.0°, θmin = 3.2°
Standard procedure using manufacturer proprietary software (Nonius, 1999) scans	h = −22→22
Absorption correction: multi-scan (Blessing, 1995)	k = −22→22
Tmin = 0.495, Tmax = 0.822	l = −9→10
50782 measured reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.031	w = 1/[σ^2(Fo^2) + (0.0358P)^2 + 4.4768P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.080	(Δ/σ)max = 0.003
S = 1.14	Δρmax = 0.40 e Å^−3
5488 reflections	Δρmin = −0.60 e Å^−3
310 parameters	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0086 (6)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983)
Secondary atom site location: difference Fourier map	Absolute structure parameter: −0.02 (4)

Special details

Experimental. The crystal was mounted under oil in random orientation. Data were collected using a mixture of area-detector ω and ϕ-exposures with the CCD detector positioned 29 mm from the sample. PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15° ϕ range.

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
Rh6	0.988741 (18)	0.308783 (19)	0.33706 (4)	0.02450 (11)
C61	1.1008 (2)	0.3155 (3)	0.2876 (6)	0.0337 (10)
C62	1.0809 (2)	0.3755 (3)	0.3830 (6)	0.0328 (10)
C63	1.0564 (3)	0.3474 (3)	0.5338 (6)	0.0328 (10)
C64	1.0601 (3)	0.2717 (3)	0.5297 (6)	0.0354 (11)
C65	1.0879 (3)	0.2505 (3)	0.3777 (6)	0.0349 (11)
C66	1.1352 (3)	0.3185 (4)	0.1283 (6)	0.0440 (13)
H66A	1.1173	0.3619	0.0714	0.066*
H66B	1.1223	0.2741	0.0688	0.066*
H66C	1.1888	0.3214	0.1395	0.066*
C67	1.0909 (3)	0.4497 (3)	0.3438 (8)	0.0465 (13)
H67A	1.1429	0.4627	0.3558	0.070*
H67B	1.0612	0.4804	0.4144	0.070*
H67C	1.0757	0.4579	0.2339	0.070*
C68	1.0333 (3)	0.3908 (3)	0.6716 (7)	0.0454 (13)
H68A	0.9954	0.3638	0.7303	0.068*
H68B	1.0133	0.4380	0.6359	0.068*
H68C	1.0757	0.3995	0.7407	0.068*
C69	1.0384 (3)	0.2214 (3)	0.6603 (7)	0.0451 (13)
H69A	1.0812	0.2114	0.7275	0.068*
H69B	1.0201	0.1752	0.6157	0.068*
H69C	0.9997	0.2445	0.7239	0.068*
C70	1.1035 (3)	0.1778 (3)	0.3257 (8)	0.0482 (13)
H70A	1.1004	0.1756	0.2100	0.072*
H70B	1.0678	0.1437	0.3720	0.072*
H70C	1.1532	0.1639	0.3595	0.072*
Rh9	0.785635 (17)	0.344798 (18)	0.28884 (4)	0.02386 (11)
C91	0.7176 (3)	0.4090 (3)	0.4566 (7)	0.0363 (11)
C92	0.6971 (3)	0.3361 (3)	0.4660 (6)	0.0359 (11)
C93	0.6731 (3)	0.3157 (3)	0.3151 (7)	0.0413 (12)
C94	0.6806 (3)	0.3760 (3)	0.2111 (7)	0.0427 (12)
C95	0.7052 (3)	0.4348 (3)	0.3021 (8)	0.0435 (13)
C96	0.7443 (3)	0.4500 (4)	0.5952 (10)	0.068 (2)
H96A	0.7023	0.4675	0.6573	0.101*
H96B	0.7736	0.4921	0.5598	0.101*
H96C	0.7748	0.4178	0.6610	0.101*
C97	0.7013 (4)	0.2899 (4)	0.6122 (8)	0.066 (2)
H97A	0.6901	0.2387	0.5855	0.099*
H97B	0.6655	0.3079	0.6900	0.099*
H97C	0.7509	0.2930	0.6570	0.099*
C98	0.6414 (3)	0.2468 (4)	0.2653 (11)	0.077 (3)
H98A	0.6578	0.2075	0.3363	0.115*
H98B	0.6571	0.2358	0.1569	0.115*
H98C	0.5877	0.2504	0.2689	0.115*
C99	0.6553 (4)	0.3819 (7)	0.0430 (8)	0.095 (4)
H99A	0.6949	0.4025	−0.0220	0.143*
H99B	0.6122	0.4141	0.0376	0.143*
H99C	0.6422	0.3330	0.0034	0.143*
C100	0.7135 (4)	0.5096 (4)	0.2467 (13)	0.086 (3)
H10A	0.7389	0.5095	0.1442	0.129*
H10B	0.7424	0.5377	0.3236	0.129*
H10C	0.6650	0.5322	0.2346	0.129*
B1	0.8735 (4)	0.2217 (4)	0.0659 (7)	0.0405 (14)
H1	0.8666	0.1717	−0.0101	0.049*
B2	0.9609 (3)	0.2638 (4)	0.0977 (7)	0.0373 (12)
H2	1.0112	0.2402	0.0408	0.045*
B3	0.8963 (3)	0.3048 (4)	−0.0186 (6)	0.0379 (13)
H3	0.9042	0.3089	−0.1498	0.045*
B4	0.8104 (3)	0.2900 (4)	0.0689 (7)	0.0359 (13)
H4	0.7604	0.2836	−0.0072	0.043*
S5	0.91537 (7)	0.21050 (6)	0.27978 (17)	0.0352 (3)
B7	0.9507 (3)	0.3580 (3)	0.1056 (6)	0.0298 (11)
H7	0.9839	0.3973	0.0588	0.036*
H78	0.9077	0.3872	0.1794	0.036*
B8	0.8529 (3)	0.3768 (3)	0.0843 (6)	0.0279 (10)
B10	0.8186 (3)	0.2385 (3)	0.2407 (7)	0.0368 (12)
H10	0.7743	0.1987	0.2705	0.044*
Cl69	0.88523 (6)	0.35823 (6)	0.46435 (13)	0.0277 (2)
O81	0.82880 (19)	0.4375 (2)	0.0078 (4)	0.0381 (8)
C81	0.8741 (3)	0.4740 (3)	−0.0995 (7)	0.0412 (12)
H81A	0.9116	0.5018	−0.0415	0.062*
H81B	0.8445	0.5079	−0.1634	0.062*
H81C	0.8980	0.4381	−0.1689	0.062*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh6	0.02247 (17)	0.02950 (19)	0.02152 (16)	0.00049 (13)	0.00129 (12)	−0.00361 (13)
C61	0.025 (2)	0.049 (3)	0.027 (2)	−0.0015 (19)	−0.0004 (19)	−0.005 (2)
C62	0.0153 (19)	0.046 (3)	0.038 (3)	0.0017 (18)	−0.0023 (17)	−0.005 (2)
C63	0.024 (2)	0.049 (3)	0.025 (2)	−0.002 (2)	−0.0031 (18)	−0.007 (2)
C64	0.025 (2)	0.055 (3)	0.027 (2)	0.007 (2)	0.0005 (18)	0.002 (2)
C65	0.027 (2)	0.049 (3)	0.029 (2)	0.011 (2)	−0.0020 (18)	−0.005 (2)
C66	0.028 (2)	0.072 (4)	0.031 (3)	0.004 (2)	0.010 (2)	0.004 (2)
C67	0.037 (3)	0.042 (3)	0.060 (3)	−0.010 (2)	0.002 (3)	−0.004 (3)
C68	0.030 (2)	0.069 (4)	0.037 (3)	−0.005 (2)	0.000 (2)	−0.024 (3)
C69	0.037 (3)	0.062 (3)	0.036 (3)	0.010 (2)	0.002 (2)	0.015 (3)
C70	0.046 (3)	0.045 (3)	0.053 (3)	0.020 (2)	0.005 (3)	−0.004 (3)
Rh9	0.02126 (17)	0.02690 (18)	0.02341 (16)	−0.00525 (12)	0.00095 (12)	−0.00162 (13)
C91	0.022 (2)	0.038 (3)	0.048 (3)	0.0045 (19)	0.005 (2)	−0.014 (2)
C92	0.030 (2)	0.042 (3)	0.035 (2)	−0.001 (2)	0.011 (2)	0.000 (2)
C93	0.023 (2)	0.047 (3)	0.054 (3)	−0.008 (2)	0.005 (2)	−0.016 (3)
C94	0.020 (2)	0.074 (4)	0.034 (3)	0.001 (2)	0.002 (2)	0.000 (3)
C95	0.026 (2)	0.042 (3)	0.062 (4)	0.004 (2)	0.010 (2)	0.010 (3)
C96	0.039 (3)	0.080 (5)	0.084 (5)	0.000 (3)	−0.004 (3)	−0.053 (4)
C97	0.066 (4)	0.074 (5)	0.058 (4)	0.014 (4)	0.033 (3)	0.028 (3)
C98	0.031 (3)	0.075 (5)	0.123 (7)	−0.025 (3)	0.024 (4)	−0.053 (5)
C99	0.036 (3)	0.217 (12)	0.033 (3)	0.032 (5)	−0.008 (3)	−0.007 (5)
C100	0.045 (3)	0.052 (4)	0.160 (9)	0.021 (3)	0.026 (5)	0.050 (5)
B1	0.040 (3)	0.042 (3)	0.039 (3)	−0.001 (3)	−0.003 (3)	−0.018 (3)
B2	0.033 (3)	0.054 (4)	0.025 (2)	0.000 (2)	−0.002 (2)	−0.011 (2)
B3	0.029 (3)	0.065 (4)	0.020 (2)	0.004 (3)	0.002 (2)	−0.011 (2)
B4	0.030 (3)	0.048 (3)	0.029 (3)	−0.005 (2)	−0.002 (2)	−0.019 (2)
S5	0.0370 (6)	0.0256 (5)	0.0430 (6)	−0.0017 (4)	−0.0017 (5)	−0.0044 (5)
B7	0.029 (2)	0.040 (3)	0.021 (2)	−0.002 (2)	0.0028 (19)	0.001 (2)
B8	0.026 (2)	0.035 (3)	0.023 (2)	−0.001 (2)	0.0005 (19)	0.003 (2)
B10	0.042 (3)	0.030 (3)	0.039 (3)	−0.006 (2)	−0.003 (2)	−0.008 (2)
Cl69	0.0216 (5)	0.0358 (6)	0.0256 (5)	−0.0003 (4)	0.0007 (4)	−0.0063 (4)
O81	0.0296 (17)	0.048 (2)	0.0371 (19)	0.0013 (15)	0.0040 (14)	0.0162 (16)
C81	0.037 (3)	0.053 (3)	0.034 (2)	−0.010 (2)	−0.001 (2)	0.014 (2)

Geometric parameters (Å, º)

Rh6—C61	2.085 (4)	C93—C94	1.412 (8)
Rh6—C62	2.105 (5)	C93—C98	1.441 (8)
Rh6—C65	2.120 (5)	C94—C95	1.391 (9)
Rh6—C63	2.184 (5)	C94—C99	1.495 (8)
Rh6—C64	2.188 (5)	C95—C100	1.447 (8)
Rh6—B2	2.238 (5)	C96—H96A	0.9800
Rh6—B7	2.259 (5)	C96—H96B	0.9800
Rh6—S5	2.2831 (12)	C96—H96C	0.9800
Rh6—Cl69	2.3475 (11)	C97—H97A	0.9800
C61—C62	1.405 (7)	C97—H97B	0.9800
C61—C65	1.425 (8)	C97—H97C	0.9800
C61—C66	1.485 (7)	C98—H98A	0.9800
C62—C67	1.402 (7)	C98—H98B	0.9800
C62—C63	1.443 (7)	C98—H98C	0.9800
C63—C64	1.380 (7)	C99—H99A	0.9800
C63—C68	1.467 (7)	C99—H99B	0.9800
C64—C65	1.433 (7)	C99—H99C	0.9800
C64—C69	1.486 (7)	C100—H10A	0.9800
C65—C70	1.423 (7)	C100—H10B	0.9800
C66—H66A	0.9800	C100—H10C	0.9800
C66—H66B	0.9800	B1—B4	1.691 (9)
C66—H66C	0.9800	B1—B3	1.723 (10)
C67—H67A	0.9800	B1—B2	1.786 (9)
C67—H67B	0.9800	B1—B10	1.808 (9)
C67—H67C	0.9800	B1—S5	1.971 (6)
C68—H68A	0.9800	B1—H1	1.12
C68—H68B	0.9800	B2—B3	1.702 (8)
C68—H68C	0.9800	B2—B7	1.725 (8)
C69—H69A	0.9800	B2—S5	1.998 (7)
C69—H69B	0.9800	B2—H2	1.12
C69—H69C	0.9800	B3—B7	1.736 (8)
C70—H70A	0.9800	B3—B4	1.750 (8)
C70—H70B	0.9800	B3—B8	1.760 (8)
C70—H70C	0.9800	B3—H3	1.12
Rh9—B10	2.066 (6)	B4—B10	1.733 (9)
Rh9—C94	2.099 (5)	B4—B8	1.764 (8)
Rh9—C93	2.126 (5)	B4—H4	1.12
Rh9—B4	2.156 (5)	S5—B10	1.863 (6)
Rh9—B8	2.195 (5)	B7—B8	1.820 (7)
Rh9—C95	2.199 (5)	B7—H7	1.02
Rh9—C92	2.203 (5)	B7—H78	1.13
Rh9—C91	2.214 (5)	B8—O81	1.351 (6)
Rh9—Cl69	2.3536 (11)	B8—H78	1.29
C91—C92	1.379 (7)	B10—H10	1.11
C91—C95	1.405 (9)	O81—C81	1.394 (6)
C91—C96	1.471 (8)	C81—H81A	0.98
C92—C93	1.398 (8)	C81—H81B	0.98
C92—C97	1.495 (8)	C81—H81C	0.98
C61—Rh6—C62	39.16 (19)	C95—C94—Rh9	75.1 (3)
C61—Rh6—C65	39.6 (2)	C93—C94—Rh9	71.5 (3)
C62—Rh6—C65	65.2 (2)	C99—C94—Rh9	126.6 (4)
C61—Rh6—C63	65.32 (18)	C94—C95—C91	108.0 (5)
C62—Rh6—C63	39.25 (19)	C94—C95—C100	125.3 (7)
C65—Rh6—C63	63.79 (19)	C91—C95—C100	126.7 (7)
C61—Rh6—C64	65.60 (18)	C94—C95—Rh9	67.3 (3)
C62—Rh6—C64	64.4 (2)	C91—C95—Rh9	72.0 (3)
C65—Rh6—C64	38.82 (18)	C100—C95—Rh9	127.8 (4)
C63—Rh6—C64	36.8 (2)	C91—C96—H96A	109.5
C61—Rh6—B2	93.6 (2)	C91—C96—H96B	109.5
C62—Rh6—B2	123.9 (2)	H96A—C96—H96B	109.5
C65—Rh6—B2	99.0 (2)	C91—C96—H96C	109.5
C63—Rh6—B2	158.8 (2)	H96A—C96—H96C	109.5
C64—Rh6—B2	133.9 (2)	H96B—C96—H96C	109.5
C61—Rh6—B7	95.93 (19)	C92—C97—H97A	109.5
C62—Rh6—B7	100.1 (2)	C92—C97—H97B	109.5
C65—Rh6—B7	126.82 (19)	H97A—C97—H97B	109.5
C63—Rh6—B7	134.7 (2)	C92—C97—H97C	109.5
C64—Rh6—B7	161.39 (19)	H97A—C97—H97C	109.5
B2—Rh6—B7	45.1 (2)	H97B—C97—H97C	109.5
C61—Rh6—S5	125.12 (15)	C93—C98—H98A	109.5
C62—Rh6—S5	162.93 (14)	C93—C98—H98B	109.5
C65—Rh6—S5	98.06 (15)	H98A—C98—H98B	109.5
C63—Rh6—S5	137.97 (15)	C93—C98—H98C	109.5
C64—Rh6—S5	105.25 (15)	H98A—C98—H98C	109.5
B2—Rh6—S5	52.43 (17)	H98B—C98—H98C	109.5
B7—Rh6—S5	87.02 (15)	C94—C99—H99A	109.5
C61—Rh6—Cl69	148.62 (14)	C94—C99—H99B	109.5
C62—Rh6—Cl69	109.46 (14)	H99A—C99—H99B	109.5
C65—Rh6—Cl69	143.13 (13)	C94—C99—H99C	109.5
C63—Rh6—Cl69	88.87 (13)	H99A—C99—H99C	109.5
C64—Rh6—Cl69	104.68 (13)	H99B—C99—H99C	109.5
B2—Rh6—Cl69	111.83 (15)	C95—C100—H10A	109.5
B7—Rh6—Cl69	89.89 (14)	C95—C100—H10B	109.5
S5—Rh6—Cl69	85.88 (4)	H10A—C100—H10B	109.5
C62—C61—C65	107.2 (4)	C95—C100—H10C	109.5
C62—C61—C66	126.9 (5)	H10A—C100—H10C	109.5
C65—C61—C66	125.7 (5)	H10B—C100—H10C	109.5
C62—C61—Rh6	71.2 (3)	B4—B1—B3	61.7 (4)
C65—C61—Rh6	71.5 (3)	B4—B1—B2	106.6 (4)
C66—C61—Rh6	126.6 (3)	B3—B1—B2	58.0 (3)
C67—C62—C61	125.4 (5)	B4—B1—B10	59.3 (3)
C67—C62—C63	126.1 (5)	B3—B1—B10	108.8 (4)
C61—C62—C63	108.1 (5)	B2—B1—B10	107.2 (4)
C67—C62—Rh6	128.0 (4)	B4—B1—S5	108.9 (4)
C61—C62—Rh6	69.6 (3)	B3—B1—S5	112.1 (4)
C63—C62—Rh6	73.3 (3)	B2—B1—S5	64.0 (3)
C64—C63—C62	108.4 (4)	B10—B1—S5	58.9 (3)
C64—C63—C68	124.8 (5)	B4—B1—H1	122
C62—C63—C68	126.8 (5)	B3—B1—H1	120
C64—C63—Rh6	71.7 (3)	B2—B1—H1	122
C62—C63—Rh6	67.4 (3)	B10—B1—H1	123
C68—C63—Rh6	127.9 (3)	S5—B1—H1	119
C63—C64—C65	108.0 (5)	B3—B2—B7	60.9 (4)
C63—C64—C69	125.7 (5)	B3—B2—B1	59.1 (4)
C65—C64—C69	126.4 (5)	B7—B2—B1	109.7 (4)
C63—C64—Rh6	71.5 (3)	B3—B2—S5	111.8 (4)
C65—C64—Rh6	68.0 (3)	B7—B2—S5	114.1 (3)
C69—C64—Rh6	125.8 (4)	B1—B2—S5	62.5 (3)
C70—C65—C61	125.0 (5)	B3—B2—Rh6	121.1 (4)
C70—C65—C64	126.6 (5)	B7—B2—Rh6	68.1 (3)
C61—C65—C64	108.3 (5)	B1—B2—Rh6	119.6 (4)
C70—C65—Rh6	125.8 (4)	S5—B2—Rh6	64.94 (17)
C61—C65—Rh6	68.9 (3)	B3—B2—H2	119
C64—C65—Rh6	73.1 (3)	B7—B2—H2	119
C61—C66—H66A	109.5	B1—B2—H2	120
C61—C66—H66B	109.5	S5—B2—H2	119
H66A—C66—H66B	109.5	Rh6—B2—H2	110
C61—C66—H66C	109.5	B2—B3—B1	62.9 (4)
H66A—C66—H66C	109.5	B2—B3—B7	60.2 (3)
H66B—C66—H66C	109.5	B1—B3—B7	112.2 (4)
C62—C67—H67A	109.5	B2—B3—B4	107.8 (4)
C62—C67—H67B	109.5	B1—B3—B4	58.3 (4)
H67A—C67—H67B	109.5	B7—B3—B4	109.8 (4)
C62—C67—H67C	109.5	B2—B3—B8	110.6 (4)
H67A—C67—H67C	109.5	B1—B3—B8	109.9 (4)
H67B—C67—H67C	109.5	B7—B3—B8	62.8 (3)
C63—C68—H68A	109.5	B4—B3—B8	60.3 (3)
C63—C68—H68B	109.5	B2—B3—H3	121
H68A—C68—H68B	109.5	B1—B3—H3	120
C63—C68—H68C	109.5	B7—B3—H3	119
H68A—C68—H68C	109.5	B4—B3—H3	123
H68B—C68—H68C	109.5	B8—B3—H3	120
C64—C69—H69A	109.5	B1—B4—B10	63.7 (4)
C64—C69—H69B	109.5	B1—B4—B3	60.1 (4)
H69A—C69—H69B	109.5	B10—B4—B3	111.1 (4)
C64—C69—H69C	109.5	B1—B4—B8	111.2 (4)
H69A—C69—H69C	109.5	B10—B4—B8	112.7 (4)
H69B—C69—H69C	109.5	B3—B4—B8	60.1 (3)
C65—C70—H70A	109.5	B1—B4—Rh9	119.7 (4)
C65—C70—H70B	109.5	B10—B4—Rh9	63.1 (3)
H70A—C70—H70B	109.5	B3—B4—Rh9	118.6 (3)
C65—C70—H70C	109.5	B8—B4—Rh9	67.3 (3)
H70A—C70—H70C	109.5	B1—B4—H4	118
H70B—C70—H70C	109.5	B10—B4—H4	120
B10—Rh9—C94	117.1 (2)	B3—B4—H4	120
B10—Rh9—C93	93.8 (2)	B8—B4—H4	119
C94—Rh9—C93	39.0 (2)	Rh9—B4—H4	112
B10—Rh9—B4	48.4 (2)	B10—S5—B1	56.2 (3)
C94—Rh9—B4	92.6 (2)	B10—S5—B2	97.1 (3)
C93—Rh9—B4	100.1 (2)	B1—S5—B2	53.5 (3)
B10—Rh9—B8	86.1 (2)	B10—S5—Rh6	112.12 (18)
C94—Rh9—B8	100.9 (2)	B1—S5—Rh6	109.8 (2)
C93—Rh9—B8	133.2 (2)	B2—S5—Rh6	62.63 (17)
B4—Rh9—B8	47.8 (2)	B2—B7—B3	58.9 (3)
B10—Rh9—C95	154.2 (2)	B2—B7—B8	106.8 (4)
C94—Rh9—C95	37.7 (2)	B3—B7—B8	59.3 (3)
C93—Rh9—C95	62.6 (2)	B2—B7—Rh6	66.8 (3)
B4—Rh9—C95	121.8 (2)	B3—B7—Rh6	118.4 (4)
B8—Rh9—C95	102.3 (2)	B8—B7—Rh6	117.4 (3)
B10—Rh9—C92	106.2 (2)	B2—B7—H7	128
C94—Rh9—C92	64.3 (2)	B3—B7—H7	120
C93—Rh9—C92	37.6 (2)	B8—B7—H7	114
B4—Rh9—C92	134.8 (2)	Rh6—B7—H7	116
B8—Rh9—C92	163.8 (2)	B2—B7—H78	124
C95—Rh9—C92	62.1 (2)	B3—B7—H78	102
B10—Rh9—C91	141.4 (2)	B8—B7—H78	45
C94—Rh9—C91	63.2 (2)	Rh6—B7—H78	86
C93—Rh9—C91	61.75 (19)	H7—B7—H78	107
B4—Rh9—C91	155.8 (2)	O81—B8—B3	121.2 (4)
B8—Rh9—C91	132.5 (2)	O81—B8—B4	123.6 (4)
C95—Rh9—C91	37.1 (2)	B3—B8—B4	59.6 (3)
C92—Rh9—C91	36.4 (2)	O81—B8—B7	121.2 (4)
B10—Rh9—Cl69	89.88 (17)	B3—B8—B7	58.0 (3)
C94—Rh9—Cl69	150.44 (17)	B4—B8—B7	105.5 (4)
C93—Rh9—Cl69	134.55 (17)	O81—B8—Rh9	114.3 (3)
B4—Rh9—Cl69	115.44 (15)	B3—B8—Rh9	116.2 (3)
B8—Rh9—Cl69	92.22 (14)	B4—B8—Rh9	64.9 (3)
C95—Rh9—Cl69	113.78 (17)	B7—B8—Rh9	114.6 (3)
C92—Rh9—Cl69	98.19 (14)	O81—B8—H78	115
C91—Rh9—Cl69	88.43 (14)	B3—B8—H78	93
C92—C91—C95	109.3 (5)	B4—B8—H78	121
C92—C91—C96	122.1 (6)	B7—B8—H78	38
C95—C91—C96	128.5 (6)	Rh9—B8—H78	89
C92—C91—Rh9	71.4 (3)	B4—B10—B1	57.0 (3)
C95—C91—Rh9	70.9 (3)	B4—B10—S5	112.1 (4)
C96—C91—Rh9	126.3 (4)	B1—B10—S5	64.9 (3)
C91—C92—C93	106.7 (5)	B4—B10—Rh9	68.5 (3)
C91—C92—C97	125.0 (6)	B1—B10—Rh9	118.6 (4)
C93—C92—C97	128.3 (6)	S5—B10—Rh9	119.7 (3)
C91—C92—Rh9	72.2 (3)	B4—B10—H10	119
C93—C92—Rh9	68.2 (3)	B1—B10—H10	118
C97—C92—Rh9	124.4 (4)	S5—B10—H10	118
C92—C93—C94	109.3 (5)	Rh9—B10—H10	111
C92—C93—C98	128.5 (6)	Rh6—Cl69—Rh9	106.82 (4)
C94—C93—C98	122.2 (6)	B8—O81—C81	120.6 (4)
C92—C93—Rh9	74.2 (3)	O81—C81—H81A	109.5
C94—C93—Rh9	69.4 (3)	O81—C81—H81B	109.5
C98—C93—Rh9	124.9 (4)	H81A—C81—H81B	109.5
C95—C94—C93	106.5 (5)	O81—C81—H81C	109.5
C95—C94—C99	124.6 (7)	H81A—C81—H81C	109.5
C93—C94—C99	128.0 (7)	H81B—C81—H81C	109.5