Di-μ-iodido-bis­[acet­yl(4-methyl-2,6,7-trioxa-1-phosphabicyclo­[2.2.2]octa­ne)(N-nitroso-N-oxidoaniline-κ2O,O′)rhodium(III)]

Venter, J.A.; Purcell, W.; Visser, H.G.

doi:10.1107/S1600536809043050

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 65| Part 12| December 2009| Pages m1528-m1529

doi:10.1107/S1600536809043050

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Di-μ-iodido-bis[acetyl(4-methyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane)(N-nitroso-N-oxidoaniline-κ²O,O′)rhodium(III)]

Johan A. Venter,^a ^* W. Purcell ^a and H. G. Visser ^a

^aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
^*Correspondence e-mail: venterja.sci@ufs.ac.za

(Received 12 October 2009; accepted 19 October 2009; online 7 November 2009)

The title compound, [Rh₂(C₆H₅N₂O₂)₂(C₂H₃O)₂I₂(C₅H₉O₃P)₂], contains a binuclear centrosymmetric Rh^III dimer bridged by iodide anions, with respective Rh⋯Rh and I⋯I distances of 4.1437 (5) and 3.9144 (5) Å. The Rh^III atom is in a distorted octahedral RhCI₂O₂P coordination with considerably different Rh—I distances to the bridging iodide anions. There are no classical hydrogen-bonding interactions observed for this complex.

Related literature

For the synthesis of similar Rh complexes and information on oxidative addition products, see: Basson et al. (1984 ; 1986a ,b ; 1987 , 1992 ); Roodt & Steyn (2000 ); Smit et al. (1994 ); Steyn et al. (1992 ); Van Leewen & Roobeeck (1981 ).

Experimental

Crystal data

[Rh₂(C₆H₅N₂O₂)₂(C₂H₃O)₂I₂(C₅H₉O₃P)₂]
M_r = 1116.14
Monoclinic, P 2₁ /c
a = 10.055 (2) Å
b = 16.944 (3) Å
c = 11.149 (2) Å
β = 112.75 (3)°
V = 1751.7 (7) Å³
Z = 2
Mo Kα radiation
μ = 2.86 mm⁻¹
T = 293 K
0.10 × 0.08 × 0.06 mm

Data collection

Bruker SMART CCD 1K diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004 ) T_min = 0.763, T_max = 0.847
12035 measured reflections
4344 independent reflections
3129 reflections with I > 2σ(I)
R_int = 0.051

Refinement

R[F² > 2σ(F²)] = 0.033
wR(F²) = 0.075
S = 0.95
4344 reflections
220 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 0.93 e Å⁻³
Δρ_min = −0.50 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

C1—Rh	2.040 (8)
I—Rh	2.6351 (8)
Rh—O3	2.044 (5)
Rh—O2	2.052 (5)
Rh—P	2.186 (2)
Rh—Iⁱ	3.0511 (9)

Rh—I—Rhⁱ	93.30 (2)
C1—Rh—O3	92.9 (3)
C1—Rh—O2	92.2 (3)
O3—Rh—O2	78.74 (19)
O2—Rh—P	172.54 (15)
C1—Rh—I	93.9 (2)
O3—Rh—I	168.12 (14)
C1—Rh—Iⁱ	172.7 (2)
Symmetry code: (i) -x+1, -y, -z+1.

Data collection: SMART (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809043050/wm2267sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809043050/wm2267Isup2.hkl

checkCIF report

Comment top

The title compound (Fig. 1) is the product of the oxidative addition of CH₃I to [Rh(cupf)(CO){P(OCH₂)₃CCH₃}] (cupf = cupferrate, (C₆H₅N₂O₂) (Basson et al., 1992) which forms part of a series of rhodium complexes used in the kinetic studies of these reactions (Basson et al., 1984; 1986b; Steyn et al., 1992; Smit et al., 1994; Roodt & Steyn, 2000).

In the structure, the Rh^III metal centre is coordinated to two bridging iodide ligands, an acyl ligand, a cyclic phosphite ligand (P(OCH₂)₃CCH₃) and an O,O'-bidentate cupferrate ligand. The coordination sphere around the metal is somewhat distorted from the octahedral geometry and a number of angles deviate significantly from the ideal (see Table 1). This is probably due to the small bite angle of 78.74 (19) ° formed by the cupferrate ligand and the metal centre. The angles, P—Rh—O2 of 172.54 (15) °, P—Rh—I of 96.21 (6)° and P—Rh—C1 of 87.2 (2) ° clearly support the visual impression of Fig. 1 showing the phosphite ligand bent outward to minimise steric interaction. The respective Rh—Rh and I—I distances were calculated as 4.1437 (5) and 3.9144 (5) Å. At 2.186 (2) Å the Rh—P bond lenght is short, compared to the 2.327 (4) Å of [Rh(cupf)(CO)(CH₃)(I)(PPh₃)] (Basson et al., 1987). This stems from the nature of phosphites to be excellent π-acceptors, causing stronger back donation from rhodium resulting in a shorter Rh—P bond. Also, the sterically small cyclic phosphite ligand allows for a closer fit in the coordination sphere. The Rh-I' distance (symmetry operator -x+1, -y, -z+1), the one trans to the acyl ligand, is significantly longer than the other Rh—I distance, demonstrating the large trans-influence of the acyl ligand. The formation of [Rh(cupf)(COCH₃)(µ-I){P(OCH₂)₃CCH₃}]₂ can most probably be attributed to the minor steric requirements of both the cupferrate ligand with its narrow bite angle and even more importantly the small cone angle of the phosphite. No classical hydrogen-bonding interactions are observed in the title compound.

Related literature top

For the synthesis of similar Rh complexes and information on oxidative addition products, see: Basson et al. (1984; 1986a,b; 1987, 1992); Roodt & Steyn (2000); Smit et al. (1994); Steyn et al. (1992); Van Leewen & Roobeeck (1981).

Experimental top

The bicyclic phosphite ester, P(OCH₂)₃CCH₃, and [Rh(C₆H₅N₂O₂)(CO)₂] was prepared according to the respective methods reported previously (Van Leewen & Roobeeck, 1981; Basson et al., 1986a). Equimolar amounts of the cyclic phosphite was mixed with [Rh(C₆H₅N₂O₂)(CO)₂] in acetone to form [Rh(C₆H₅N₂O₂)(CO)(P(OCH₂)₃CCH₃)]. The reaction mixture was concentrated by evaporation after which a tenfold excess of CH₃I was added. The container was covered with a perforated plastic film and left to stand for two days at 271 K after which brown-red single crystals of the title compound were isolated.

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus (Bruker, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. View of the dimeric compex present in the title compound. Probability level for displacement ellipsoids is 50%. Symmetry-related atoms are generated by the symmetry operator i) -x+1, -y, -z+1.

Di-µ-iodido-bis[acetyl(4-methyl-2,6,7-trioxa-1- phosphabicyclo[2.2.2]octane)(N-nitroso-N-oxidoaniline- κ²O,O')rhodium(III)] top

Crystal data top

[Rh₂(C₆H₅N₂O₂)₂(C₂H₃O)₂I₂(C₅H₉O₃P)₂]	F(000) = 1080
M_r = 1116.14	D_x = 2.116 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 859 reflections
a = 10.055 (2) Å	θ = 2.3–28.1°
b = 16.944 (3) Å	µ = 2.86 mm⁻¹
c = 11.149 (2) Å	T = 293 K
β = 112.75 (3)°	Cuboid, brown-red
V = 1751.7 (7) Å³	0.10 × 0.08 × 0.06 mm
Z = 2

Data collection top

Bruker SMART CCD 1K diffractometer	4344 independent reflections
Radiation source: fine-focus sealed tube	3129 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.051
ω scans	θ_max = 28.3°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −13→11
T_min = 0.763, T_max = 0.847	k = −22→14
12035 measured reflections	l = −12→14

Refinement top

Refinement on F²	1 restraint
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.033	w = 1/[σ²(F_o²) + (0.0354P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.075	(Δ/σ)_max < 0.001
S = 0.95	Δρ_max = 0.93 e Å⁻³
4344 reflections	Δρ_min = −0.50 e Å⁻³
220 parameters

Crystal data top

[Rh₂(C₆H₅N₂O₂)₂(C₂H₃O)₂I₂(C₅H₉O₃P)₂]	V = 1751.7 (7) Å³
M_r = 1116.14	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.055 (2) Å	µ = 2.86 mm⁻¹
b = 16.944 (3) Å	T = 293 K
c = 11.149 (2) Å	0.10 × 0.08 × 0.06 mm
β = 112.75 (3)°

Data collection top

Bruker SMART CCD 1K diffractometer	4344 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	3129 reflections with I > 2σ(I)
T_min = 0.763, T_max = 0.847	R_int = 0.051
12035 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.033	1 restraint
wR(F²) = 0.075	H-atom parameters constrained
S = 0.95	Δρ_max = 0.93 e Å⁻³
4344 reflections	Δρ_min = −0.50 e Å⁻³
220 parameters

Special details top

Experimental. The intensity data were collected on a Bruker SMART CCD 1 K diffractometer using an exposure time of 20 s/frame. A total of 1315 frames were collected with a frame width of 0.3° covering up to θ = 28.29° with 99.8% completeness accomplished. The first 50 frames were recollected at the end of the data collection to check for decay; none was found.

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

	x	y	z	U_iso*/U_eq
C6	0.3530 (9)	0.3279 (4)	0.4556 (7)	0.0389 (18)
C5	0.3479 (11)	0.2939 (5)	0.5784 (8)	0.053 (2)
H1A	0.4329	0.3102	0.6522	0.064*
H1B	0.2637	0.314	0.5908	0.064*
C4	0.4801 (10)	0.2932 (5)	0.4347 (9)	0.050 (2)
H2A	0.4849	0.3154	0.3563	0.06*
H2B	0.568	0.3073	0.5072	0.06*
C7	0.3688 (11)	0.4178 (5)	0.4674 (9)	0.060 (3)
H5A	0.4549	0.431	0.5408	0.091*
H5B	0.2867	0.4399	0.479	0.091*
H5C	0.3747	0.4389	0.3897	0.091*
O1	0.1009 (7)	0.0872 (4)	0.5202 (7)	0.0698 (19)
C1	0.1039 (9)	0.0605 (5)	0.4219 (9)	0.045 (2)
C2	−0.0248 (11)	0.0383 (7)	0.3093 (10)	0.074 (3)
H9A	−0.0107	−0.0129	0.279	0.111*
H9B	−0.0418	0.0763	0.2412	0.111*
H9C	−0.1064	0.0366	0.3338	0.111*
I	0.43362 (5)	−0.00049 (3)	0.64352 (4)	0.03779 (16)
Rh	0.29476 (7)	0.04485 (4)	0.40073 (6)	0.03779 (16)
P	0.3320 (2)	0.17126 (11)	0.43763 (19)	0.0342 (4)
O2	0.2452 (6)	−0.0699 (3)	0.3412 (5)	0.0382 (12)
N1	0.1775 (7)	−0.0076 (4)	0.1406 (6)	0.0433 (16)
O3	0.2017 (6)	0.0583 (3)	0.2034 (5)	0.0413 (13)
N2	0.1995 (7)	−0.0702 (3)	0.2114 (6)	0.0366 (14)
C11	0.1793 (8)	−0.1465 (4)	0.1476 (7)	0.0355 (17)
O6	0.4702 (6)	0.2079 (3)	0.4228 (6)	0.0495 (14)
O4	0.2045 (6)	0.2201 (3)	0.3337 (5)	0.0511 (15)
O5	0.3416 (7)	0.2073 (3)	0.5719 (5)	0.0535 (16)
C15	0.2426 (11)	−0.2819 (5)	0.1644 (10)	0.061 (3)
H010	0.292	−0.3249	0.2131	0.073*
C16	0.2521 (10)	−0.2091 (5)	0.2224 (8)	0.050 (2)
H011	0.3069	−0.2026	0.3107	0.061*
C13	0.0867 (11)	−0.2264 (6)	−0.0368 (10)	0.068 (3)
H012	0.0298	−0.2321	−0.1248	0.082*
C12	0.0962 (10)	−0.1545 (5)	0.0197 (8)	0.058 (2)
H013	0.0463	−0.1114	−0.0288	0.07*
C14	0.1587 (11)	−0.2907 (6)	0.0322 (10)	0.065 (3)
H014	0.1518	−0.3393	−0.0083	0.078*
C3	0.2178 (10)	0.3068 (4)	0.3415 (9)	0.051 (2)
H01A	0.1346	0.3297	0.3522	0.061*
H01B	0.2222	0.3275	0.262	0.061*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C6	0.059 (5)	0.025 (4)	0.037 (4)	0.005 (4)	0.022 (4)	0.005 (3)
C5	0.086 (7)	0.039 (5)	0.042 (5)	0.001 (4)	0.033 (5)	−0.008 (4)
C4	0.064 (6)	0.030 (4)	0.064 (6)	−0.013 (4)	0.034 (5)	−0.010 (4)
C7	0.097 (8)	0.035 (5)	0.056 (6)	0.003 (5)	0.036 (5)	0.007 (4)
O1	0.070 (5)	0.070 (5)	0.085 (5)	0.003 (4)	0.047 (4)	−0.006 (4)
C1	0.050 (5)	0.040 (5)	0.053 (5)	0.010 (4)	0.027 (4)	0.004 (4)
C2	0.060 (7)	0.091 (8)	0.076 (7)	0.000 (6)	0.032 (6)	0.008 (6)
I	0.0466 (3)	0.0360 (2)	0.0325 (2)	0.00276 (18)	0.01725 (17)	0.00362 (16)
Rh	0.0466 (3)	0.0360 (2)	0.0325 (2)	0.00276 (18)	0.01725 (17)	0.00362 (16)
P	0.0421 (11)	0.0291 (10)	0.0324 (10)	0.0012 (8)	0.0155 (8)	0.0015 (8)
O2	0.058 (3)	0.024 (2)	0.035 (3)	−0.008 (2)	0.021 (3)	−0.002 (2)
N1	0.043 (4)	0.051 (4)	0.029 (3)	0.001 (3)	0.007 (3)	0.005 (3)
O3	0.054 (3)	0.024 (3)	0.044 (3)	0.001 (2)	0.017 (3)	0.007 (2)
N2	0.046 (4)	0.028 (3)	0.035 (3)	−0.003 (3)	0.015 (3)	0.001 (3)
C11	0.040 (4)	0.030 (4)	0.038 (4)	−0.004 (3)	0.017 (3)	−0.006 (3)
O6	0.051 (3)	0.032 (3)	0.076 (4)	−0.004 (3)	0.036 (3)	−0.007 (3)
O4	0.056 (4)	0.030 (3)	0.052 (3)	0.009 (3)	0.004 (3)	0.002 (3)
O5	0.100 (5)	0.032 (3)	0.038 (3)	−0.001 (3)	0.038 (3)	0.000 (2)
C15	0.078 (7)	0.039 (5)	0.064 (6)	0.004 (5)	0.025 (5)	−0.002 (4)
C16	0.067 (6)	0.038 (4)	0.041 (5)	0.002 (4)	0.016 (4)	−0.006 (4)
C13	0.071 (7)	0.066 (7)	0.053 (6)	−0.016 (5)	0.008 (5)	−0.022 (5)
C12	0.062 (6)	0.055 (6)	0.041 (5)	0.002 (5)	0.001 (4)	−0.005 (4)
C14	0.067 (7)	0.053 (6)	0.079 (7)	−0.021 (5)	0.033 (6)	−0.030 (5)
C3	0.072 (6)	0.026 (4)	0.054 (5)	0.010 (4)	0.022 (5)	0.003 (4)

Geometric parameters (Å, º) top

C6—C5	1.504 (10)	Rh—P	2.186 (2)
C6—C4	1.504 (11)	Rh—Iⁱ	3.0511 (9)
C6—C3	1.502 (12)	P—O6	1.588 (6)
C6—C7	1.533 (10)	P—O5	1.585 (5)
C5—O5	1.468 (9)	P—O4	1.589 (5)
C5—H1A	0.97	O2—N2	1.339 (7)
C5—H1B	0.97	N1—O3	1.290 (8)
C4—O6	1.451 (8)	N1—N2	1.289 (8)
C4—H2A	0.97	N2—C11	1.451 (9)
C4—H2B	0.97	C11—C12	1.352 (10)
C7—H5A	0.96	C11—C16	1.374 (11)
C7—H5B	0.96	O4—C3	1.474 (9)
C7—H5C	0.96	C15—C16	1.379 (11)
O1—C1	1.196 (10)	C15—C14	1.394 (13)
C1—C2	1.461 (13)	C15—H010	0.93
C1—Rh	2.040 (8)	C16—H011	0.93
C2—H9A	0.96	C13—C14	1.368 (14)
C2—H9B	0.96	C13—C12	1.358 (12)
C2—H9C	0.96	C13—H012	0.93
I—Rh	2.6351 (8)	C12—H013	0.93
I—Rhⁱ	3.0511 (9)	C14—H014	0.93
Rh—O3	2.044 (5)	C3—H01A	0.97
Rh—O2	2.052 (5)	C3—H01B	0.97

C5—C6—C4	108.7 (7)	C1—Rh—Iⁱ	172.7 (2)
C5—C6—C3	110.0 (7)	O3—Rh—Iⁱ	85.36 (16)
C4—C6—C3	108.7 (7)	O2—Rh—Iⁱ	80.51 (15)
C5—C6—C7	110.0 (6)	P—Rh—Iⁱ	99.96 (6)
C4—C6—C7	109.6 (7)	I—Rh—Iⁱ	86.70 (2)
C3—C6—C7	109.8 (6)	O6—P—O5	102.2 (3)
O5—C5—C6	110.7 (6)	O6—P—O4	102.2 (3)
O5—C5—H1A	109.5	O5—P—O4	103.0 (3)
C6—C5—H1A	109.5	O6—P—Rh	117.2 (2)
O5—C5—H1B	109.5	O5—P—Rh	120.0 (2)
C6—C5—H1B	109.5	O4—P—Rh	110.0 (2)
H1A—C5—H1B	108.1	N2—O2—Rh	107.0 (4)
O6—C4—C6	111.8 (6)	O3—N1—N2	115.4 (6)
O6—C4—H2A	109.3	N1—O3—Rh	113.5 (4)
C6—C4—H2A	109.3	N1—N2—O2	124.3 (6)
O6—C4—H2B	109.3	N1—N2—C11	118.3 (6)
C6—C4—H2B	109.3	O2—N2—C11	117.3 (6)
H2A—C4—H2B	107.9	C12—C11—C16	122.0 (7)
C6—C7—H5A	109.5	C12—C11—N2	121.2 (7)
C6—C7—H5B	109.5	C16—C11—N2	116.7 (7)
H5A—C7—H5B	109.5	C4—O6—P	114.3 (5)
C6—C7—H5C	109.5	C3—O4—P	116.6 (5)
H5A—C7—H5C	109.5	C5—O5—P	114.7 (4)
H5B—C7—H5C	109.5	C16—C15—C14	119.7 (9)
O1—C1—C2	123.8 (9)	C16—C15—H010	120.2
O1—C1—Rh	120.9 (7)	C14—C15—H010	120.2
C2—C1—Rh	115.3 (7)	C11—C16—C15	118.8 (8)
C1—C2—H9A	109.5	C11—C16—H011	120.6
C1—C2—H9B	109.5	C15—C16—H011	120.6
H9A—C2—H9B	109.5	C14—C13—C12	121.8 (9)
C1—C2—H9C	109.5	C14—C13—H012	119.1
H9A—C2—H9C	109.5	C12—C13—H012	119.1
H9B—C2—H9C	109.5	C11—C12—C13	118.9 (9)
Rh—I—Rhⁱ	93.30 (2)	C11—C12—H013	120.6
C1—Rh—O3	92.9 (3)	C13—C12—H013	120.6
C1—Rh—O2	92.2 (3)	C13—C14—C15	118.8 (8)
O3—Rh—O2	78.74 (19)	C13—C14—H014	120.6
C1—Rh—P	87.2 (2)	C15—C14—H014	120.6
O3—Rh—P	93.85 (14)	O4—C3—C6	108.6 (6)
O2—Rh—P	172.54 (15)	O4—C3—H01A	110
C1—Rh—I	93.9 (2)	C6—C3—H01A	110
O3—Rh—I	168.12 (14)	O4—C3—H01B	110
O2—Rh—I	91.25 (14)	C6—C3—H01B	110
P—Rh—I	96.21 (6)	H01A—C3—H01B	108.4

Symmetry code: (i) −x+1, −y, −z+1.

Experimental details

Crystal data
Chemical formula	[Rh₂(C₆H₅N₂O₂)₂(C₂H₃O)₂I₂(C₅H₉O₃P)₂]
M_r	1116.14
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	10.055 (2), 16.944 (3), 11.149 (2)
β (°)	112.75 (3)
V (Å³)	1751.7 (7)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.86
Crystal size (mm)	0.10 × 0.08 × 0.06

Data collection
Diffractometer	Bruker SMART CCD 1K diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2004)
T_min, T_max	0.763, 0.847
No. of measured, independent and observed [I > 2σ(I)] reflections	12035, 4344, 3129
R_int	0.051
(sin θ/λ)_max (Å⁻¹)	0.667

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.033, 0.075, 0.95
No. of reflections	4344
No. of parameters	220
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.93, −0.50

Computer programs: SMART (Bruker, 2004), SAINT-Plus (Bruker, 2004), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top

C1—Rh	2.040 (8)	Rh—P	2.186 (2)
I—Rh	2.6351 (8)	Rh—Iⁱ	3.0511 (9)
Rh—O3	2.044 (5)	P—O6	1.588 (6)
Rh—O2	2.052 (5)	P—O5	1.585 (5)

Rh—I—Rhⁱ	93.30 (2)	O2—Rh—P	172.54 (15)
C1—Rh—O3	92.9 (3)	C1—Rh—I	93.9 (2)
C1—Rh—O2	92.2 (3)	O3—Rh—I	168.12 (14)
O3—Rh—O2	78.74 (19)	C1—Rh—Iⁱ	172.7 (2)

Symmetry code: (i) −x+1, −y, −z+1.

Acknowledgements

The University of the Witwatersrand (Professor D. Levendis and Dr D. G. Billing) is thanked for the use of its diffractometer. Financial assistance by the South African National Research Foundation (grant No. 2038915), the Central Research Fund of the University of the Free State, THRIP and Sasol is gratefully acknowledged. Opinions, findings, conclusions or recommendations expressed in this material are those of the authors and do not necessarily reflect the views of the National Research Foundation.

References

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