Ten-vertex rhodadithiaborane ­chemistry: [8-{I(CH₂)₅}-3-(η⁵-C₅Me₅)-arachno-3,7,8-RhS₂B₈H₉]

Neutral 8-(5-iodo-n-pentyl)-3-(η⁵-penta­methyl­cyclo­pentadi­enyl)-arachno-3-rhoda-7,8-di­thia­undecaborane, [Rh(C₅H₁₉B₈­IS₂)­(C₁₀H₁₅)], obtained from the [arachno-7,8-S₂B₉H₁₀]⁻ anion by treatment with I(CH₂)₅I followed by [Rh(C₅Me₅)Cl₂]₂ and N,N,N′,N′-tetra­methyl-1,8-di­amino­naphthalene, has the 11-vertex cluster geometry of [arachno-7,8-S₂B₉H₁₀]⁻, but with an {Rh(C₅Me₅)} unit in the 3-position instead of a {BH} unit, and with a –(CH₂)₅I chain attached exo to an S atom.

S1. Comment

A contemporary survey of boron chemistry (Davidson et al., 2000) shows that there is much current interest in the linking together of boron-containing clusters with varying degrees of intimacy to give a remarkable variety of larger macromolecular assemblies (Lamrani et al., 2000; Hawthorne, 2000; Grimes, 2000; Colquhoun et al., 2000; Bould et al., 1999; Barton et al., 2000; Sivaev et al., 2000). Within this variety, there is a classification that may be described as consisting of 'bola' boranes, in which two clusters are linked together by a long flexible chain, for example the {–P—C—C—P–}-linked rhodathiaborane clusters in [(dppe)RhSB₉H₈(PPh₂CH₂CH₂PPh₂)B₉H₈SRh(dppe)] (Barton, 2000) and the {–O—C—C—C—C–}-linked borane and carborane units in the [B₁₂H₁₁O(CH₂)₄C₂B₁₀H₁₁]^2- dianion (Sivaev et al., 2000). In this context, we report the formation and structural characterization of a potential precursor, viz. [8-{I(CH₂)₅}-5-(η⁵-C₅Me₅)-arachno-5,7,8-RhS₂B₈H₉], compound (I), to another type of bola-borane species. \sch

The heteroborane cluster architecture (Figure 1) is seen to be based on the arachno-type eleven-vertex cluster structure of the starting [S₂B₉H₁₀]^- anion, (II), but with the {BH(exo)} vertex at the 3-position replaced by the 'isolobal' cluster contributor {Rh(η⁵-C₅Me₅)}. It is of interest that, during the course of the reaction, there has been an effective replacement of {BH(exo)} by {Rh(η⁵-C₅Me₅)}. Since this is a very intimately bound cluster position (cluster connectivity five), however, it implies that the replacement mechanism will be complex. Interestingly, in the closely related reaction of neutral [MeS₂B₉H₁₀] with [{Rh(η⁵-C₅Me₅)Cl₂}₂] the product [(η⁴-C₅Me₅H)RhSB₉H₉SMe] is quite different (Macías et al., 1997): (a) it retains all boron atoms, (b) there is a hydrogen atom transfer to the hydrocarbon ligand and an associated reduction in intimacy of the rhodium-to-hydrocarbon bonding, and (c) the alkylated sulfur atom is partially extruded from the cluster into a boron-boron bridging position. In [8-{I(CH₂)₅}-3- (η⁵-C₅Me₅)-arachno-3,7,8-RhS₂B₈H₉], the other feature different from the [S₂B₉H₁₀]^- anion is of course the alkylation of one of the sulfur atoms, S8, by the long-chain -(CH₂)₅I moiety. There is some precedent for S-alkylation in the structurally characterized neutral [MeS₂B₉H₁₀] species obtainable from [S₂B₉H₁₀]^- by iodide displacement from MeI (Holub et al., 1994), but here the alkylated sulfur is again extruded to a boron-boron bridging position, in contrast to the present compound. As expected, the bridging hydrogen atom on the open face is at the B10–B11 site distal from the alkylated, formally positive, S8 sulfur site, rather than at the adjacent B9–B10 position. The distance from the Rh atom to the alkylated sulfur atom S8 at 2.6185 (16) Å is significantly longer than that to non-alkylated S7 at 2.3922 (16) Å, and the boron-sulfur distance B4–S8 at 2.064 (8) Å is similarly longer than the otherwise corresponding B2–S7 distance of 1.938 (9) Å. Comparison of dimensions given in the Table shows that there are related differential effects throughout the cluster associated with the S-alkylation and the concomitant siting of the bridging hydrogen atom at B10–B11. The establishment of compound (I) leads to the interesting idea of a potential bolaborane (Barton, 2000) by use of an excess of the starting thiaborane, followed by excess of the organometallic substrate, to give [8,8'-{α,ω-(CH₂)₅}-{3-(η⁵-C₅Me₅)- arachno-3,7,8-RhS₂B₈H₉}₂], (III), and analogous structures when the concept is extended to other related systems. We currently examine for these and related possibilities.

Related literature

For related literature, see: Barton (2000); Bould et al. (1999); Colquhoun et al. (2000); Davidson et al. (2000); Grimes (2000); Hawthorne (2000); Heřmánek (1999); Holub et al. (1994); Lamrani et al. (2000); Reed (1993); Sivaev et al. (2000).

S2. Experimental

A solution of [tmndH]⁺[S₂B₉H₁₀]^- (500 mg, 1.3 mmol, tmnd = N,N,N',N'-tetramethyl-1,8-diaminonaphthalene) and I(CH₂)₅I (200 mg, 0.1 ml, 0.6 mmol) in CH₂Cl₂ (30 ml) was heated at reflux under N₂ for 24 h, the pale yellow solution filtered, and the solvent removed from the filtrate (rotary evaporator). The resulting yellow solid evaporate was extracted with hexane. Evaporation of the hexane extract gave a colourless oily residue, for which integrated ¹H NMR spectroscopy indicated a ca 50% conversion of I(CH₂)₅I. The ¹¹B NMR spectrum showed nine different resonances, at δ(¹¹B) +32.9, +13.0, +9.8, +0.8, -1.8, -9.2, -18.6, -21.7 and -34.2 p.p.m.. These are very similar to those reported for [MeS₂B₉H₁₀] (Holub et al., 1994), supporting mono-S-alkylation and the generation of [I(CH₂)₅S₂B₉H₁₀] (185 mg, mmol, 0.6 mmol, 50%). This crude product was dissolved in CH₂Cl₂ (30 ml) and stirred with tmnd (128 mg, 0.6 mmol), and then [(C₅Me₅)RhCl₂]₂ (185 mg, 0.3 mmol) was added. The brown-black solution was stirred for 1 h, filtered through silica and reduced in volume. Preparative thin-layer chromatography (Silica GF254; 60% CH₂Cl₂/40% hexane) yielded a number of coloured components. The principal species was dark amber [8-{I(CH₂)₅}-3- (η⁵-C₅Me₅)-arachno-3,7,8-RhS₂B₈H₉] [compound (I), R_F ca 0.5; 12 mg, 0.02 mmol, 3%]. Crystallization was from dichloromethane-hexane. Selected NMR data for CD₂Cl₂ solution of [{I(CH₂)₅}(C₅Me₅)RhS₂B₈H₉], (I), at 294–300 K as follows; cluster assignments by [¹¹B–¹¹B], [¹H–¹H] and (¹H)-{¹¹B} correlation experiments [Heřmánek, 1999; Reed, 1993]; ordered as assignment δ(¹¹B)/p.p.m. [δ(¹H)/p.p.m. for directly attached exo-hydrogen]: BH1 - 4.9 [+1.84], BH2 + 4.6 [+2.42], BH4 - 14.1 [+1.06], BH5 + 8.9 [+3.81], BH6 - 16.9 [+1.72], BH9 - 8.4 [+2.11], BH10 - 33.9 [+0.59] and BH11 - 1.6 [+3.11], with δ(¹H)(µ-10,11) -1.75 [stronger coupling to B10 than to B11], and δ(¹H)(C₅Me₅) at +1.89, {S(CH₂)₅I} {CH₂} groups along the chain successively at δ(¹H) +2.40 (α to S), +1.76, +1.51, +1.85 and +3.24 (α to I).

S3. Refinement

Cage H atoms were located from the Fourier difference syntheses and, were although their positional parameters were included in structure factor calculations, they were not refined. Non-cage H atoms were constrained in calculated positions with isotropic displacement parameters of 1.2U_eq of the parent C atom.

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: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEX (McArdle, 1995); software used to prepare material for publication: WC (Thornton-Pett, 2000).

Figures

Fig. 1. Crystallographically determined molecular structure of (I) drawn with 40% probability ellipsoids and with H atoms shown as small circles of artificial radii.

[8-(5-iodo-n-hexyl)-5-(pentahapto-pentamethylcyclopentadienyl)- arachno-3-rhoda-7,8-dithia-arachno-undecaborane]

Crystal data

[Rh(C5H19B8IS2)(C10H15)]	F(000) = 2352
Mr = 594.83	Dx = 1.657 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71069 Å
a = 28.6498 (4) Å	Cell parameters from 31844 reflections
b = 10.6700 (2) Å	θ = 1.7–26.0°
c = 18.2997 (4) Å	µ = 2.19 mm^−1
β = 121.524 (1)°	T = 180 K
V = 4768.53 (15) Å^3	Prism, dark red
Z = 8	0.33 × 0.20 × 0.13 mm

Data collection

Nonius KappaCCD area-detector diffractometer	4616 independent reflections
Radiation source: fine-focus sealed tube	4244 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.100
Detector resolution: 9.091 pixels mm^-1	θmax = 26.0°, θmin = 1.7°
1 degree ϕ exposures scans	h = −35→35
Absorption correction: multi-scan (SORTAV; Blessing, 1995)	k = −13→12
Tmin = 0.532, Tmax = 0.764	l = −22→22
31844 measured reflections

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)] = 0.058	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.162	w = 1/[σ^2(Fo^2) + (0.0723P)^2 + 27.1436P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
4616 reflections	Δρmax = 1.84 e Å^−3
250 parameters	Δρmin = −1.16 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0022 (2)

Special details

Experimental. 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 degree phi 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
Rh3	0.154692 (18)	0.02351 (4)	0.35982 (3)	0.0455 (2)
C1	0.1723 (2)	0.0846 (6)	0.2617 (3)	0.0515 (13)
C2	0.1153 (2)	0.0514 (6)	0.2202 (3)	0.0473 (12)
C3	0.1112 (2)	−0.0767 (6)	0.2375 (3)	0.0505 (13)
C4	0.1662 (3)	−0.1253 (6)	0.2903 (4)	0.0543 (13)
C5	0.2036 (3)	−0.0242 (6)	0.3037 (4)	0.0556 (14)
C6	0.1957 (3)	0.2095 (7)	0.2589 (4)	0.0695 (19)
H6A	0.2304	0.2233	0.3129	0.104*
H6B	0.1698	0.2761	0.2506	0.104*
H6C	0.2020	0.2105	0.2112	0.104*
C7	0.0680 (3)	0.1321 (6)	0.1606 (3)	0.0557 (14)
H7A	0.0792	0.2203	0.1707	0.084*
H7B	0.0380	0.1193	0.1709	0.084*
H7C	0.0556	0.1099	0.1012	0.084*
C8	0.0590 (3)	−0.1509 (7)	0.2001 (4)	0.0644 (16)
H8A	0.0508	−0.1889	0.1459	0.097*
H8B	0.0290	−0.0952	0.1897	0.097*
H8C	0.0633	−0.2170	0.2403	0.097*
C9	0.1812 (3)	−0.2567 (7)	0.3152 (5)	0.0737 (19)
H9A	0.1795	−0.3028	0.2675	0.111*
H9B	0.1556	−0.2941	0.3293	0.111*
H9C	0.2184	−0.2609	0.3654	0.111*
C10	0.2641 (3)	−0.0378 (9)	0.3495 (6)	0.078 (2)
H10A	0.2744	−0.0733	0.3104	0.117*
H10B	0.2765	−0.0937	0.3988	0.117*
H10C	0.2813	0.0445	0.3694	0.117*
C11	0.0798 (3)	0.3467 (7)	0.3238 (4)	0.0679 (17)
H11A	0.0704	0.3221	0.2655	0.081*
H11B	0.0461	0.3417	0.3262	0.081*
C16	0.1011 (4)	0.4796 (7)	0.3416 (5)	0.0686 (18)
H16A	0.0758	0.5324	0.2919	0.082*
H16B	0.1371	0.4810	0.3464	0.082*
C13	0.1075 (3)	0.5387 (7)	0.4241 (5)	0.0690 (18)
H13A	0.1271	0.4789	0.4722	0.083*
H13B	0.1300	0.6154	0.4386	0.083*
C14	0.0541 (3)	0.5713 (8)	0.4148 (5)	0.0700 (18)
H14A	0.0319	0.4940	0.4009	0.084*
H14B	0.0342	0.6294	0.3657	0.084*
C15	0.0584 (3)	0.6309 (7)	0.4928 (5)	0.0725 (18)
H15A	0.0219	0.6621	0.4776	0.087*
H15B	0.0833	0.7039	0.5101	0.087*
B1	0.1105 (4)	−0.0666 (7)	0.4177 (4)	0.0574 (17)
H1	0.0899	−0.1722	0.3908	0.069*
B2	0.1856 (3)	−0.0876 (7)	0.4864 (4)	0.0600 (17)
H2	0.2057	−0.1930	0.4964	0.072*
B4	0.0820 (3)	0.0836 (8)	0.3771 (4)	0.0548 (16)
H4	0.0441	0.0856	0.3295	0.066*
B5	0.0889 (4)	0.0321 (9)	0.4711 (5)	0.0641 (19)
H5	0.0502	0.0013	0.4727	0.077*
B6	0.1477 (4)	−0.0570 (8)	0.5348 (5)	0.0643 (19)
H6	0.1392	−0.1389	0.5639	0.077*
S7	0.23388 (7)	0.04961 (19)	0.50007 (10)	0.0623 (4)
S8	0.13148 (7)	0.23828 (15)	0.40274 (9)	0.0543 (4)
B9	0.0991 (3)	0.1897 (8)	0.4679 (4)	0.0630 (18)
H9	0.0643	0.2754	0.4594	0.076*
B10	0.1460 (4)	0.1040 (8)	0.5633 (4)	0.0635 (19)
H10	0.1402	0.1208	0.6129	0.076*
H101	0.1934	0.1638	0.5686	0.076*
B11	0.2087 (4)	0.0295 (8)	0.5795 (5)	0.0628 (18)
H11	0.2428	0.0078	0.6486	0.075*
I15	0.08834 (2)	0.50440 (5)	0.60066 (4)	0.0747 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh3	0.0514 (3)	0.0528 (3)	0.0379 (3)	0.00072 (18)	0.0272 (2)	0.00154 (16)
C1	0.060 (3)	0.065 (4)	0.042 (3)	−0.007 (3)	0.036 (3)	−0.002 (2)
C2	0.059 (3)	0.058 (3)	0.035 (2)	0.001 (3)	0.031 (2)	0.001 (2)
C3	0.059 (3)	0.057 (3)	0.043 (3)	−0.005 (3)	0.033 (3)	−0.004 (2)
C4	0.062 (3)	0.057 (3)	0.051 (3)	0.003 (3)	0.034 (3)	−0.001 (3)
C5	0.054 (3)	0.071 (4)	0.050 (3)	0.001 (3)	0.033 (3)	−0.008 (3)
C6	0.084 (5)	0.077 (5)	0.061 (4)	−0.025 (4)	0.047 (4)	−0.007 (3)
C7	0.062 (3)	0.066 (4)	0.041 (3)	0.005 (3)	0.029 (3)	0.003 (3)
C8	0.066 (4)	0.069 (4)	0.055 (3)	−0.017 (3)	0.029 (3)	−0.005 (3)
C9	0.092 (5)	0.065 (4)	0.063 (4)	0.015 (4)	0.040 (4)	−0.002 (3)
C10	0.051 (4)	0.113 (7)	0.075 (5)	0.004 (4)	0.037 (4)	−0.017 (4)
C11	0.084 (5)	0.070 (4)	0.047 (3)	0.006 (4)	0.032 (3)	0.002 (3)
C16	0.082 (5)	0.074 (5)	0.056 (4)	0.009 (4)	0.041 (4)	0.013 (3)
C13	0.082 (5)	0.061 (4)	0.063 (4)	−0.004 (3)	0.037 (4)	−0.002 (3)
C14	0.081 (5)	0.071 (5)	0.062 (4)	0.006 (4)	0.041 (4)	−0.005 (3)
C15	0.084 (5)	0.063 (4)	0.075 (4)	0.004 (4)	0.045 (4)	−0.003 (3)
B1	0.097 (5)	0.052 (4)	0.050 (3)	−0.001 (3)	0.058 (4)	0.009 (3)
B2	0.083 (5)	0.055 (4)	0.042 (3)	0.007 (4)	0.033 (3)	0.008 (3)
B4	0.050 (3)	0.076 (5)	0.048 (3)	−0.001 (3)	0.032 (3)	−0.004 (3)
B5	0.076 (5)	0.084 (5)	0.047 (4)	−0.008 (4)	0.042 (4)	0.000 (3)
B6	0.088 (5)	0.066 (5)	0.046 (3)	−0.010 (4)	0.039 (4)	0.002 (3)
S7	0.0573 (9)	0.0770 (11)	0.0471 (8)	−0.0021 (8)	0.0234 (7)	−0.0021 (7)
S8	0.0671 (9)	0.0554 (8)	0.0458 (7)	0.0033 (7)	0.0333 (7)	0.0017 (6)
B9	0.077 (5)	0.074 (5)	0.046 (3)	0.002 (4)	0.037 (3)	−0.004 (3)
B10	0.083 (5)	0.074 (5)	0.039 (3)	−0.003 (4)	0.036 (3)	−0.004 (3)
B11	0.072 (5)	0.069 (5)	0.050 (4)	−0.002 (4)	0.034 (4)	−0.004 (3)
I15	0.0792 (4)	0.0839 (4)	0.0730 (4)	−0.0085 (2)	0.0480 (3)	−0.0124 (2)

Geometric parameters (Å, º)

Rh3—C4	2.165 (6)	C16—H16A	0.99
Rh3—C5	2.187 (6)	C16—H16B	0.99
Rh3—C3	2.189 (6)	C13—C14	1.489 (11)
Rh3—C1	2.203 (5)	C13—H13A	0.99
Rh3—C2	2.209 (5)	C13—H13B	0.99
Rh3—B1	2.249 (6)	C14—C15	1.508 (9)
Rh3—B2	2.326 (7)	C14—H14A	0.99
Rh3—B4	2.354 (6)	C14—H14B	0.99
Rh3—S7	2.3922 (16)	C15—I15	2.163 (8)
Rh3—S8	2.6185 (16)	C15—H15A	0.99
C1—C5	1.422 (9)	C15—H15B	0.99
C1—C2	1.440 (8)	B1—B5	1.753 (11)
C1—C6	1.503 (9)	B1—B4	1.776 (11)
C2—C3	1.422 (9)	B1—B6	1.831 (10)
C2—C7	1.492 (8)	B1—B2	1.854 (12)
C3—C4	1.446 (9)	B1—H1	1.25
C3—C8	1.503 (8)	B2—B6	1.754 (11)
C4—C5	1.449 (9)	B2—B11	1.929 (11)
C4—C9	1.467 (9)	B2—S7	1.938 (9)
C5—C10	1.487 (10)	B2—H2	1.23
C6—H6A	0.98	B4—B5	1.715 (10)
C6—H6B	0.98	B4—B9	1.852 (10)
C6—H6C	0.98	B4—S8	2.064 (8)
C7—H7A	0.98	B4—H4	0.97
C7—H7B	0.98	B5—B9	1.713 (12)
C7—H7C	0.98	B5—B6	1.745 (13)
C8—H8A	0.98	B5—B10	1.796 (12)
C8—H8B	0.98	B5—H5	1.17
C8—H8C	0.98	B6—B11	1.755 (12)
C9—H9A	0.98	B6—B10	1.803 (12)
C9—H9B	0.98	B6—H6	1.11
C9—H9C	0.98	S7—B11	1.943 (8)
C10—H10A	0.98	S8—B9	1.925 (7)
C10—H10B	0.98	B9—B10	1.799 (11)
C10—H10C	0.98	B9—H9	1.30
C11—C16	1.509 (10)	B10—B11	1.840 (12)
C11—S8	1.839 (7)	B10—H10	1.02
C11—H11A	0.99	B10—H101	1.46
C11—H11B	0.99	B11—H101	1.48
C16—C13	1.556 (10)	B11—H11	1.15
C4—Rh3—C5	38.9 (2)	C14—C15—H15A	108.9
C4—Rh3—C3	38.8 (2)	I15—C15—H15A	108.9
C5—Rh3—C3	64.4 (2)	C14—C15—H15B	108.9
C4—Rh3—C1	64.4 (2)	I15—C15—H15B	108.9
C5—Rh3—C1	37.8 (2)	H15A—C15—H15B	107.7
C3—Rh3—C1	64.0 (2)	B5—B1—B4	58.1 (4)
C4—Rh3—C2	64.0 (2)	B5—B1—B6	58.2 (5)
C5—Rh3—C2	63.4 (2)	B4—B1—B6	107.4 (5)
C3—Rh3—C2	37.7 (2)	B5—B1—B2	108.5 (5)
C1—Rh3—C2	38.1 (2)	B4—B1—B2	120.6 (5)
C4—Rh3—B1	105.0 (2)	B6—B1—B2	56.9 (4)
C5—Rh3—B1	141.2 (3)	B5—B1—Rh3	117.0 (5)
C3—Rh3—B1	96.5 (2)	B4—B1—Rh3	70.5 (3)
C1—Rh3—B1	159.5 (3)	B6—B1—Rh3	113.6 (5)
C2—Rh3—B1	122.0 (3)	B2—B1—Rh3	68.3 (3)
C4—Rh3—B2	96.6 (2)	B5—B1—H1	122.1
C5—Rh3—B2	110.2 (3)	B4—B1—H1	129.1
C3—Rh3—B2	119.1 (3)	B6—B1—H1	112.3
C1—Rh3—B2	146.3 (3)	B2—B1—H1	107.5
C2—Rh3—B2	156.8 (3)	Rh3—B1—H1	117.8
B1—Rh3—B2	47.8 (3)	B6—B2—B1	60.9 (4)
C4—Rh3—B4	134.1 (3)	B6—B2—B11	56.7 (4)
C5—Rh3—B4	162.9 (2)	B1—B2—B11	105.1 (5)
C3—Rh3—B4	101.5 (2)	B6—B2—S7	112.5 (5)
C1—Rh3—B4	128.7 (2)	B1—B2—S7	119.6 (4)
C2—Rh3—B4	99.6 (2)	B11—B2—S7	60.3 (4)
B1—Rh3—B4	45.3 (3)	B6—B2—Rh3	113.2 (5)
B2—Rh3—B4	84.7 (3)	B1—B2—Rh3	63.9 (3)
C4—Rh3—S7	111.45 (17)	B11—B2—Rh3	109.0 (4)
C5—Rh3—S7	92.85 (18)	S7—B2—Rh3	67.5 (2)
C3—Rh3—S7	150.16 (17)	B6—B2—H2	117.3
C1—Rh3—S7	110.29 (16)	B1—B2—H2	119.8
C2—Rh3—S7	148.19 (16)	B11—B2—H2	122.9
B1—Rh3—S7	89.8 (2)	S7—B2—H2	115.1
B2—Rh3—S7	48.5 (2)	Rh3—B2—H2	121.2
B4—Rh3—S7	103.53 (17)	B5—B4—B1	60.3 (4)
C4—Rh3—S8	163.48 (16)	B5—B4—B9	57.2 (4)
C5—Rh3—S8	132.08 (18)	B1—B4—B9	109.1 (5)
C3—Rh3—S8	129.52 (17)	B5—B4—S8	108.8 (5)
C1—Rh3—S8	100.82 (17)	B1—B4—S8	121.0 (5)
C2—Rh3—S8	99.98 (16)	B9—B4—S8	58.6 (3)
B1—Rh3—S8	86.50 (19)	B5—B4—Rh3	113.6 (5)
B2—Rh3—S8	99.88 (19)	B1—B4—Rh3	64.2 (3)
B4—Rh3—S8	48.7 (2)	B9—B4—Rh3	116.6 (4)
S7—Rh3—S8	79.83 (6)	S8—B4—Rh3	72.4 (2)
C5—C1—C2	107.7 (5)	B5—B4—H4	113.3
C5—C1—C6	125.2 (6)	B1—B4—H4	116.6
C2—C1—C6	127.0 (6)	B9—B4—H4	116.0
C5—C1—Rh3	70.5 (3)	S8—B4—H4	119.8
C2—C1—Rh3	71.2 (3)	Rh3—B4—H4	122.4
C6—C1—Rh3	125.9 (4)	B9—B5—B4	65.4 (5)
C3—C2—C1	108.9 (5)	B9—B5—B6	115.8 (6)
C3—C2—C7	124.6 (5)	B4—B5—B6	114.2 (6)
C1—C2—C7	126.2 (6)	B9—B5—B1	117.0 (5)
C3—C2—Rh3	70.4 (3)	B4—B5—B1	61.6 (4)
C1—C2—Rh3	70.7 (3)	B6—B5—B1	63.1 (5)
C7—C2—Rh3	129.9 (4)	B9—B5—B10	61.6 (5)
C2—C3—C4	107.8 (5)	B4—B5—B10	112.1 (6)
C2—C3—C8	125.7 (6)	B6—B5—B10	61.2 (5)
C4—C3—C8	126.3 (6)	B1—B5—B10	111.5 (6)
C2—C3—Rh3	71.9 (3)	B9—B5—H5	117.2
C4—C3—Rh3	69.7 (3)	B4—B5—H5	119.9
C8—C3—Rh3	128.4 (4)	B6—B5—H5	115.2
C3—C4—C5	107.3 (5)	B1—B5—H5	117.3
C3—C4—C9	126.2 (6)	B10—B5—H5	120.4
C5—C4—C9	126.0 (6)	B5—B6—B2	113.6 (5)
C3—C4—Rh3	71.5 (3)	B5—B6—B11	113.7 (6)
C5—C4—Rh3	71.4 (3)	B2—B6—B11	66.7 (5)
C9—C4—Rh3	128.9 (4)	B5—B6—B10	60.8 (5)
C1—C5—C4	108.4 (5)	B2—B6—B10	116.1 (6)
C1—C5—C10	127.2 (7)	B11—B6—B10	62.3 (5)
C4—C5—C10	124.4 (7)	B5—B6—B1	58.7 (4)
C1—C5—Rh3	71.7 (3)	B2—B6—B1	62.3 (4)
C4—C5—Rh3	69.7 (3)	B11—B6—B1	113.8 (5)
C10—C5—Rh3	127.1 (5)	B10—B6—B1	107.7 (5)
C1—C6—H6A	109.5	B5—B6—H6	111.7
C1—C6—H6B	109.5	B2—B6—H6	116.3
H6A—C6—H6B	109.5	B11—B6—H6	127.1
C1—C6—H6C	109.5	B10—B6—H6	124.3
H6A—C6—H6C	109.5	B1—B6—H6	112.1
H6B—C6—H6C	109.5	B2—S7—B11	59.6 (3)
C2—C7—H7A	109.5	B2—S7—Rh3	64.0 (2)
C2—C7—H7B	109.5	B11—S7—Rh3	106.0 (3)
H7A—C7—H7B	109.5	C11—S8—B9	101.9 (4)
C2—C7—H7C	109.5	C11—S8—B4	98.6 (3)
H7A—C7—H7C	109.5	B9—S8—B4	55.2 (3)
H7B—C7—H7C	109.5	C11—S8—Rh3	122.8 (2)
C3—C8—H8A	109.5	B9—S8—Rh3	103.3 (3)
C3—C8—H8B	109.5	B4—S8—Rh3	58.95 (19)
H8A—C8—H8B	109.5	B5—B9—B10	61.4 (5)
C3—C8—H8C	109.5	B5—B9—B4	57.4 (4)
H8A—C8—H8C	109.5	B10—B9—B4	105.9 (6)
H8B—C8—H8C	109.5	B5—B9—S8	115.6 (5)
C4—C9—H9A	109.5	B10—B9—S8	112.4 (5)
C4—C9—H9B	109.5	B4—B9—S8	66.2 (3)
H9A—C9—H9B	109.5	B5—B9—H9	124.1
C4—C9—H9C	109.5	B10—B9—H9	127.6
H9A—C9—H9C	109.5	B4—B9—H9	119.7
H9B—C9—H9C	109.5	S8—B9—H9	108.9
C5—C10—H10A	109.5	B5—B10—B9	56.9 (5)
C5—C10—H10B	109.5	B5—B10—B6	58.0 (5)
H10A—C10—H10B	109.5	B9—B10—B6	108.9 (5)
C5—C10—H10C	109.5	B5—B10—B11	107.4 (5)
H10A—C10—H10C	109.5	B9—B10—B11	123.1 (5)
H10B—C10—H10C	109.5	B6—B10—B11	57.6 (5)
C16—C11—S8	110.7 (5)	B5—B10—H10	114.8
C16—C11—H11A	109.5	B9—B10—H10	112.8
S8—C11—H11A	109.5	B6—B10—H10	117.8
C16—C11—H11B	109.5	B11—B10—H10	122.1
S8—C11—H11B	109.5	B5—B10—H101	127.5
H11A—C11—H11B	108.1	B9—B10—H101	92.2
C11—C16—C13	114.8 (6)	B6—B10—H101	105.8
C11—C16—H16A	108.6	B11—B10—H101	51.8
C13—C16—H16A	108.6	H10—B10—H101	116.3
C11—C16—H16B	108.6	B6—B11—B10	60.1 (5)
C13—C16—H16B	108.6	B6—B11—B2	56.6 (4)
H16A—C16—H16B	107.5	B10—B11—B2	106.4 (5)
C14—C13—C16	113.0 (7)	B6—B11—S7	112.2 (5)
C14—C13—H13A	109.0	B10—B11—S7	123.0 (5)
C16—C13—H13A	109.0	B2—B11—S7	60.1 (3)
C14—C13—H13B	109.0	B6—B11—H101	107.1
C16—C13—H13B	109.0	B10—B11—H101	50.6
H13A—C13—H13B	107.8	B2—B11—H101	124.6
C13—C14—C15	114.8 (7)	S7—B11—H101	89.6
C13—C14—H14A	108.6	B6—B11—H11	118.3
C15—C14—H14A	108.6	B10—B11—H11	117.5
C13—C14—H14B	108.6	B2—B11—H11	122.9
C15—C14—H14B	108.6	S7—B11—H11	114.3
H14A—C14—H14B	107.6	H101—B11—H11	111.4
C14—C15—I15	113.5 (5)