Acetonitrile­trichloridobis(cyclo­hexyl­diphenyl­phosphane)rhodium(III) acetonitrile disolvate

Theunis J Muller; Hendrik G Visser; Andreas Roodt

doi:10.1107/S1600536811047477

. 2011 Nov 19;67(Pt 12):m1785–m1786. doi: 10.1107/S1600536811047477

Acetonitriletrichloridobis(cyclohexyldiphenylphosphane)rhodium(III) acetonitrile disolvate

Theunis J Muller ^a,^*, Hendrik G Visser ^a, Andreas Roodt ^a

PMCID: PMC3238697 PMID: 22199574

Abstract

In the title compound, [RhCl₃(CH₃CN)(C₁₈H₂₁P)₂]·2CH₃CN, the complex molecule lies on a twofold rotation axis that passes through the Rh^III atom, one Cl atom, and the C and N atoms of the coordinated acetonitrile molecule. The Rh^III atom is coordinated by two P atoms in trans positions, three Cl atoms and an acetonitrile molecule in a distorted octahedral geometry. Intramolecular C—H⋯Cl interactions are observed. The uncoordinated acetonitrile molecule is disordered over two sites with occupancies of 0.588 (4) and 0.412 (4).

Related literature

For background to the catalytic activity of rhodium–phosphane adducts, see: Brink et al. (2010 ▶); Marko & Heil (1974 ▶); Nagy-Magos et al. (1978 ▶); Oro et al. (1978 ▶); Roodt et al. (2003 ▶). For related structures, see: Archer et al. (1993 ▶); Aslanov et al. (1970 ▶); Clegg et al. (2002 ▶); Drew et al. (1970 ▶).

Experimental

Crystal data

[RhCl₃(C₂H₃N)(C₁₈H₂₁P)₂]·2C₂H₃N
M _r = 869.06
Monoclinic,
a = 24.995 (1) Å
b = 10.041 (1) Å
c = 16.258 (1) Å
β = 96.763 (1)°
V = 4052.0 (5) Å³
Z = 4
Mo Kα radiation
μ = 0.73 mm⁻¹
T = 100 K
0.32 × 0.25 × 0.16 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T _min = 0.797, T _max = 0.889
33882 measured reflections
5038 independent reflections
4615 reflections with I > 2σ(I)
R _int = 0.027

Refinement

R[F ² > 2σ(F ²)] = 0.022
wR(F ²) = 0.055
S = 1.04
5038 reflections
264 parameters
2 restraints
H-atom parameters constrained
Δρ_max = 0.37 e Å⁻³
Δρ_min = −0.63 e Å⁻³

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT-Plus (Bruker, 2008 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); 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 ▶).

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811047477/is2783sup1.cif

e-67-m1785-sup1.cif^{(28.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811047477/is2783Isup2.hkl

e-67-m1785-Isup2.hkl^{(241.8KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Rh1—N1	1.9978 (17)
Rh1—Cl2	2.3297 (5)
Rh1—Cl1	2.3486 (3)
Rh1—P1	2.4013 (3)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C10—H10⋯Cl2	0.95	2.59	3.4452 (14)	150
C20—H20B⋯Cl2	0.99	2.72	3.4797 (14)	134

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Acknowledgments

The University of the Free State and Inkaba are gratefully acknowledged for financial support.

supplementary crystallographic information

Comment

Rhodium catalysts formed in situ from RhCl₃xH₂O and phosphanes have been used for the hydrogenation (Marko & Heil, 1974; Nagy-Magos et al., 1978) and hydroformylation (Oro et al., 1978) of olefins. The catalytic activity is determined by the electronic and steric effects of the phosphane ligand (Roodt et al., 2003; Brink et al., 2010).

The title compound (Fig. 1) crystallizes in the monoclinic space group C2/c. The Rh^III atom is situated on a twofold rotation axis, which passes atoms Cl2, N1 and C2. Two cyclohexyldiphenylphosphane ligands are positioned trans to each other, with the other four coordination sites occupied by three mer-chloroligands and one molecule of the acetonitrile solvent. In contrast to the structure reported by Clegg et al. (2002) the solvent molecule lies opposite the shortest Rh—Cl2 bond [2.3297 (5) Å] in the complex. Deviations from ideal octahedral geometry are minor (Table 1). The Rh—P1 bond length is 2.4013 (5) Å, while the Rh—Cl1 bond length is 2.3486 (6) Å. The P1—Rh—P1ⁱ angle is 176.462 (17)° which is close to the Cl1—Rh—Cl1ⁱ at 176.185 (18)° [symmetry code: (i) -x, y, -z + 1/2]. This complex is therefore structurally related to trans-ReCl₃(PMe₂Ph)₃ (Aslanov et al., 1970) and ReCl₃(PPh₃)₂MeCN (Drew et al., 1970), and other metal halide derivatives of this type (Archer et al., 1993). The uncoordinated acetonitrile molecule is disordered over two positions with occupancies of 0.588 (4) and 0.412 (4). The molecular structure of the complex is stabilized by intramolecular C—H···Cl interactions (Table 2).

Experimental

RhCl₃.H₂O (20 mg, 9.557×10 ^-5 mol) was added to acetonitrile (5 ml) and heated to reflux. Cyclohexyldiphenylphosphane (2 eq, 1.911×10 ^-4 mol, 51,2 mg) was added to the solution. The solution was refluxed for 15 min before it was cooled to room temperature. Crystals suitable for X-ray analysis was grown overnight by the slow evaporation of acetonitrile at room temperature (yield 0.0750 g, 89%)

Figures

Fig. 1. — Diamond representation of the title compound, showing the numbering scheme and displacement ellipsoids (50% probability).

Crystal data

[RhCl₃(C₂H₃N)(C₁₈H₂₁P)₂]·2C₂H₃N	F(000) = 1800
M_r = 869.06	D_x = 1.425 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 24.995 (1) Å	Cell parameters from 9837 reflections
b = 10.041 (1) Å	θ = 2.5–28.3°
c = 16.258 (1) Å	µ = 0.73 mm⁻¹
β = 96.763 (1)°	T = 100 K
V = 4052.0 (5) Å³	Cuboid, red
Z = 4	0.32 × 0.25 × 0.16 mm

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Data collection

Bruker APEXII CCD diffractometer	4615 reflections with I > 2σ(I)
graphite	R_int = 0.027
φ and ω scans	θ_max = 28.4°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −33→33
T_min = 0.797, T_max = 0.889	k = −13→13
33882 measured reflections	l = −21→19
5038 independent reflections

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Refinement

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.055	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0236P)² + 4.9122P] where P = (F_o² + 2F_c²)/3
5038 reflections	(Δ/σ)_max = 0.001
264 parameters	Δρ_max = 0.37 e Å⁻³
2 restraints	Δρ_min = −0.63 e Å⁻³

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Special details

Experimental. The intensity data was collected on a Bruker X8 ApexII 4 K Kappa CCD diffractometer using an exposure time of 20 s/frame. A total of 1963 frames were collected with a frame width of 0.5° covering up to θ = 28.35° with 99.6% completeness accomplished

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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.

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Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

	x	y	z	U_iso*/U_eq	Occ. (<1)
Rh1	0	0.145288 (14)	0.25	0.01099 (5)
Cl1	−0.053994 (13)	0.13750 (3)	0.35876 (2)	0.01819 (7)
Cl2	0	0.37731 (4)	0.25	0.01635 (9)
P1	0.079330 (13)	0.13791 (3)	0.34878 (2)	0.01236 (7)
N1	0	−0.05368 (17)	0.25	0.0166 (3)
C15	0.07347 (5)	0.20332 (14)	0.45392 (8)	0.0160 (3)
H15	0.0418	0.1572	0.4734	0.019*
C11	0.18508 (6)	0.40163 (15)	0.26099 (10)	0.0230 (3)
H11	0.1831	0.479	0.2271	0.028*
C2	0	−0.3095 (2)	0.25	0.0238 (4)
H2A	0.019	−0.3421	0.2046	0.036*	0.5
H2B	−0.0372	−0.3421	0.2426	0.036*	0.5
H2C	0.0182	−0.3421	0.3029	0.036*	0.5
C5	0.14501 (6)	−0.23233 (15)	0.32610 (10)	0.0228 (3)
H5	0.1671	−0.2744	0.29	0.027*
C4	0.13087 (6)	−0.09925 (15)	0.31407 (9)	0.0186 (3)
H4	0.1431	−0.0512	0.2696	0.022*
C18	0.10192 (7)	0.36857 (16)	0.60247 (9)	0.0242 (3)
H18A	0.1342	0.4175	0.5893	0.029*
H18B	0.0942	0.3966	0.6582	0.029*
C3	0.09890 (5)	−0.03580 (13)	0.36674 (8)	0.0151 (3)
C8	0.07948 (6)	−0.10963 (15)	0.42960 (9)	0.0197 (3)
H8	0.0562	−0.069	0.4644	0.024*
C16	0.12161 (6)	0.17108 (15)	0.51730 (9)	0.0217 (3)
H16A	0.1273	0.0735	0.5193	0.026*
H16B	0.1544	0.2129	0.5	0.026*
C10	0.13773 (6)	0.33469 (15)	0.27481 (9)	0.0205 (3)
H10	0.1037	0.369	0.2525	0.025*
C7	0.09408 (7)	−0.24283 (15)	0.44145 (10)	0.0250 (3)
H7	0.0812	−0.2921	0.485	0.03*
C19	0.05461 (6)	0.40325 (16)	0.53948 (9)	0.0220 (3)
H19A	0.0505	0.5013	0.537	0.026*
H19B	0.0214	0.3657	0.5579	0.026*
C14	0.19135 (6)	0.17214 (15)	0.35757 (10)	0.0209 (3)
H14	0.1936	0.0956	0.3922	0.025*
C9	0.14076 (5)	0.21728 (14)	0.32148 (9)	0.0166 (3)
C13	0.23812 (6)	0.23857 (16)	0.34300 (10)	0.0243 (3)
H13	0.2723	0.2043	0.3647	0.029*
C20	0.06056 (6)	0.35127 (14)	0.45333 (9)	0.0201 (3)
H20A	0.0897	0.4009	0.4305	0.024*
H20B	0.0267	0.3673	0.4167	0.024*
C17	0.11302 (6)	0.22091 (16)	0.60265 (9)	0.0214 (3)
H17A	0.0823	0.1728	0.6221	0.026*
H17B	0.1455	0.2016	0.6418	0.026*
C6	0.12719 (6)	−0.30370 (15)	0.39021 (10)	0.0253 (3)
H6	0.1376	−0.394	0.3991	0.03*
C12	0.23475 (6)	0.35541 (17)	0.29659 (11)	0.0281 (4)
H12	0.2666	0.4036	0.2893	0.034*
C1	0	−0.1644 (2)	0.25	0.0199 (4)
N2A	0.22420 (12)	0.4183 (3)	0.0550 (2)	0.0384 (8)	0.588 (4)
C21A	0.2017 (4)	0.1790 (4)	0.1017 (6)	0.0345 (17)	0.588 (4)
H21A	0.1631	0.173	0.1067	0.052*	0.588 (4)
H21B	0.2223	0.1594	0.1554	0.052*	0.588 (4)
H21C	0.211	0.1144	0.0605	0.052*	0.588 (4)
C22A	0.21444 (12)	0.3123 (3)	0.07576 (19)	0.0331 (8)	0.588 (4)
N2B	0.2558 (2)	0.0458 (6)	−0.0078 (4)	0.0611 (16)	0.412 (4)
C21B	0.2042 (7)	0.1588 (10)	0.1007 (9)	0.060 (4)	0.412 (4)
H21D	0.2034	0.2552	0.0914	0.09*	0.412 (4)
H21E	0.2224	0.1399	0.1563	0.09*	0.412 (4)
H21F	0.1673	0.1243	0.096	0.09*	0.412 (4)
C22B	0.2333 (2)	0.0950 (6)	0.0394 (4)	0.0523 (17)	0.412 (4)

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Atomic displacement parameters (Å²)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rh1	0.01107 (7)	0.00977 (7)	0.01209 (7)	0	0.00121 (5)	0
Cl1	0.01540 (15)	0.02406 (18)	0.01562 (16)	−0.00089 (12)	0.00398 (12)	0.00129 (12)
Cl2	0.0172 (2)	0.0117 (2)	0.0195 (2)	0	−0.00028 (17)	0
P1	0.01149 (15)	0.01268 (16)	0.01287 (16)	−0.00007 (12)	0.00121 (12)	0.00040 (12)
N1	0.0136 (7)	0.0180 (9)	0.0173 (8)	0	−0.0018 (6)	0
C15	0.0154 (6)	0.0181 (7)	0.0141 (6)	0.0006 (5)	0.0003 (5)	−0.0021 (5)
C11	0.0214 (7)	0.0184 (7)	0.0299 (8)	−0.0017 (6)	0.0054 (6)	0.0036 (6)
C2	0.0263 (11)	0.0165 (10)	0.0285 (11)	0	0.0033 (9)	0
C5	0.0222 (7)	0.0179 (7)	0.0278 (8)	0.0047 (6)	0.0007 (6)	−0.0026 (6)
C4	0.0168 (6)	0.0190 (7)	0.0199 (7)	0.0011 (5)	0.0018 (5)	0.0012 (6)
C18	0.0279 (8)	0.0275 (8)	0.0170 (7)	−0.0023 (6)	0.0019 (6)	−0.0044 (6)
C3	0.0144 (6)	0.0146 (6)	0.0154 (6)	−0.0001 (5)	−0.0016 (5)	0.0009 (5)
C8	0.0219 (7)	0.0187 (7)	0.0185 (7)	−0.0024 (5)	0.0022 (5)	0.0010 (5)
C16	0.0238 (7)	0.0224 (7)	0.0178 (7)	0.0031 (6)	−0.0026 (6)	−0.0019 (6)
C10	0.0154 (6)	0.0212 (7)	0.0250 (7)	0.0004 (5)	0.0022 (5)	0.0044 (6)
C7	0.0322 (8)	0.0196 (7)	0.0222 (8)	−0.0048 (6)	−0.0006 (6)	0.0060 (6)
C19	0.0246 (7)	0.0207 (7)	0.0201 (7)	0.0025 (6)	0.0004 (6)	−0.0046 (6)
C14	0.0161 (6)	0.0217 (7)	0.0247 (7)	0.0002 (5)	0.0014 (5)	0.0038 (6)
C9	0.0138 (6)	0.0177 (7)	0.0185 (7)	−0.0020 (5)	0.0025 (5)	−0.0004 (5)
C13	0.0147 (6)	0.0283 (8)	0.0295 (8)	−0.0003 (6)	0.0007 (6)	0.0013 (6)
C20	0.0251 (7)	0.0184 (7)	0.0165 (7)	0.0033 (6)	0.0014 (5)	−0.0010 (5)
C17	0.0191 (7)	0.0275 (8)	0.0168 (7)	−0.0026 (6)	−0.0020 (5)	−0.0011 (6)
C6	0.0302 (8)	0.0152 (7)	0.0285 (8)	0.0014 (6)	−0.0051 (6)	0.0020 (6)
C12	0.0166 (7)	0.0297 (9)	0.0390 (9)	−0.0052 (6)	0.0073 (6)	0.0039 (7)
C1	0.0174 (9)	0.0200 (11)	0.0217 (10)	0	−0.0004 (7)	0
N2A	0.0365 (16)	0.0417 (17)	0.0367 (17)	−0.0067 (12)	0.0033 (12)	−0.0085 (13)
C21A	0.027 (3)	0.040 (3)	0.037 (4)	−0.005 (2)	0.007 (2)	−0.007 (2)
C22A	0.0247 (14)	0.0420 (19)	0.0323 (16)	−0.0032 (13)	0.0020 (11)	−0.0101 (14)
N2B	0.063 (3)	0.066 (4)	0.052 (3)	−0.027 (3)	−0.002 (3)	−0.014 (3)
C21B	0.073 (8)	0.047 (4)	0.055 (8)	−0.014 (5)	−0.021 (5)	0.009 (5)
C22B	0.056 (4)	0.049 (3)	0.046 (3)	−0.023 (3)	−0.017 (3)	0.000 (3)

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Geometric parameters (Å, °)

Rh1—N1	1.9978 (17)	C16—C17	1.514 (2)
Rh1—Cl2	2.3297 (5)	C16—H16A	0.99
Rh1—Cl1	2.3486 (3)	C16—H16B	0.99
Rh1—Cl1ⁱ	2.3486 (3)	C10—C9	1.399 (2)
Rh1—P1	2.4013 (3)	C10—H10	0.95
Rh1—P1ⁱ	2.4013 (3)	C7—C6	1.384 (2)
P1—C3	1.8257 (14)	C7—H7	0.95
P1—C9	1.8304 (14)	C19—C20	1.518 (2)
P1—C15	1.8529 (14)	C19—H19A	0.99
N1—C1	1.112 (3)	C19—H19B	0.99
C15—C20	1.520 (2)	C14—C13	1.390 (2)
C15—C16	1.5240 (18)	C14—C9	1.4049 (19)
C15—H15	1	C14—H14	0.95
C11—C12	1.387 (2)	C13—C12	1.392 (2)
C11—C10	1.402 (2)	C13—H13	0.95
C11—H11	0.95	C20—H20A	0.99
C2—C1	1.457 (3)	C20—H20B	0.99
C2—H2A	0.98	C17—H17A	0.99
C2—H2B	0.98	C17—H17B	0.99
C2—H2C	0.98	C6—H6	0.95
C5—C6	1.381 (2)	C12—H12	0.95
C5—C4	1.390 (2)	N2A—C22A	1.151 (5)
C5—H5	0.95	C21A—C22A	1.4501 (10)
C4—C3	1.392 (2)	C21A—H21A	0.98
C4—H4	0.95	C21A—H21B	0.98
C18—C17	1.508 (2)	C21A—H21C	0.98
C18—C19	1.511 (2)	N2B—C22B	1.119 (9)
C18—H18A	0.99	C21B—C22B	1.4498 (10)
C18—H18B	0.99	C21B—H21D	0.98
C3—C8	1.395 (2)	C21B—H21E	0.98
C8—C7	1.394 (2)	C21B—H21F	0.98
C8—H8	0.95

N1—Rh1—Cl2	180	C17—C16—C15	111.33 (12)
N1—Rh1—Cl1	88.093 (9)	C17—C16—H16A	109.4
Cl2—Rh1—Cl1	91.907 (9)	C15—C16—H16A	109.4
N1—Rh1—Cl1ⁱ	88.093 (9)	C17—C16—H16B	109.4
Cl2—Rh1—Cl1ⁱ	91.907 (9)	C15—C16—H16B	109.4
Cl1—Rh1—Cl1ⁱ	176.185 (18)	H16A—C16—H16B	108
N1—Rh1—P1	88.231 (9)	C9—C10—C11	119.86 (13)
Cl2—Rh1—P1	91.769 (9)	C9—C10—H10	120.1
Cl1—Rh1—P1	89.879 (12)	C11—C10—H10	120.1
Cl1ⁱ—Rh1—P1	90.003 (12)	C6—C7—C8	120.40 (15)
N1—Rh1—P1ⁱ	88.231 (9)	C6—C7—H7	119.8
Cl2—Rh1—P1ⁱ	91.769 (9)	C8—C7—H7	119.8
Cl1—Rh1—P1ⁱ	90.003 (12)	C18—C19—C20	113.09 (13)
Cl1ⁱ—Rh1—P1ⁱ	89.879 (12)	C18—C19—H19A	109
P1—Rh1—P1ⁱ	176.463 (17)	C20—C19—H19A	109
C3—P1—C9	103.78 (6)	C18—C19—H19B	109
C3—P1—C15	103.88 (6)	C20—C19—H19B	109
C9—P1—C15	103.24 (6)	H19A—C19—H19B	107.8
C3—P1—Rh1	108.72 (4)	C13—C14—C9	120.50 (14)
C9—P1—Rh1	118.33 (5)	C13—C14—H14	119.8
C15—P1—Rh1	117.21 (4)	C9—C14—H14	119.8
C1—N1—Rh1	180	C10—C9—C14	119.15 (13)
C20—C15—C16	111.22 (12)	C10—C9—P1	120.32 (10)
C20—C15—P1	112.36 (10)	C14—C9—P1	119.84 (11)
C16—C15—P1	113.99 (10)	C14—C13—C12	119.89 (14)
C20—C15—H15	106.2	C14—C13—H13	120.1
C16—C15—H15	106.2	C12—C13—H13	120.1
P1—C15—H15	106.2	C19—C20—C15	111.96 (12)
C12—C11—C10	120.26 (14)	C19—C20—H20A	109.2
C12—C11—H11	119.9	C15—C20—H20A	109.2
C10—C11—H11	119.9	C19—C20—H20B	109.2
C1—C2—H2A	109.5	C15—C20—H20B	109.2
C1—C2—H2B	109.5	H20A—C20—H20B	107.9
H2A—C2—H2B	109.5	C18—C17—C16	111.65 (13)
C1—C2—H2C	109.5	C18—C17—H17A	109.3
H2A—C2—H2C	109.5	C16—C17—H17A	109.3
H2B—C2—H2C	109.5	C18—C17—H17B	109.3
C6—C5—C4	120.38 (15)	C16—C17—H17B	109.3
C6—C5—H5	119.8	H17A—C17—H17B	108
C4—C5—H5	119.8	C5—C6—C7	119.61 (14)
C5—C4—C3	120.53 (14)	C5—C6—H6	120.2
C5—C4—H4	119.7	C7—C6—H6	120.2
C3—C4—H4	119.7	C11—C12—C13	120.15 (14)
C17—C18—C19	110.91 (12)	C11—C12—H12	119.9
C17—C18—H18A	109.5	C13—C12—H12	119.9
C19—C18—H18A	109.5	N1—C1—C2	180
C17—C18—H18B	109.5	N2A—C22A—C21A	179.5 (5)
C19—C18—H18B	109.5	C22B—C21B—H21D	109.5
H18A—C18—H18B	108	C22B—C21B—H21E	109.5
C4—C3—C8	118.80 (13)	H21D—C21B—H21E	109.5
C4—C3—P1	120.07 (11)	C22B—C21B—H21F	109.5
C8—C3—P1	121.00 (11)	H21D—C21B—H21F	109.5
C7—C8—C3	120.21 (14)	H21E—C21B—H21F	109.5
C7—C8—H8	119.9	N2B—C22B—C21B	179.9 (11)
C3—C8—H8	119.9

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Symmetry codes: (i) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, °)

D—H···A	D—H	H···A	D···A	D—H···A
C10—H10···Cl2	0.95	2.59	3.4452 (14)	150.
C20—H20B···Cl2	0.99	2.72	3.4797 (14)	134.

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Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS2783).

References

Archer, C. M., Dilworth, J. R., Thompson, R. M., McPartlin, M., Povey, D. C. & Kelly, J. D. (1993). J. Chem. Soc. Dalton Trans. pp. 461–466.
Aslanov, L., Mason, R., Wheeler, A. G. & Whimp, P. O. (1970). J. Chem. Soc. Chem. Commun. pp. 30–31.
Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Brink, A., Roodt, A., Steyl, G. & Visser, H. G. (2010). J. Chem. Soc. Dalton Trans. 39, 5572—5578. [DOI] [PubMed]
Bruker (2008). APEX2, SAINT-Plus and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
Clegg, W., Scott, A. J., Norman, N. C., Robins, E. G. & Whittell, G. R. (2002). Acta Cryst. E58, m410–m411.
Drew, M. G. B., Tisley, D. G. & Walton, R. A. (1970). J. Chem. Soc. Chem. Commun. pp. 600–601.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.
Marko, L. & Heil, B. (1974). Catal. Rev. 8, 269–293.
Nagy-Magos, Z., Vastag, S., Heil, B. & Marko, L. (1978). Transition Met. Chem. 3, 123–126.
Oro, L. A., Manrique, A. & Royo, M. (1978). Transition Met. Chem. 3, 383–384.
Roodt, A., Otto, S. & Steyl, G. (2003). Coord. Chem. Rev. 245, 121–137.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811047477/is2783sup1.cif

e-67-m1785-sup1.cif^{(28.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811047477/is2783Isup2.hkl

e-67-m1785-Isup2.hkl^{(241.8KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[bb1] Archer, C. M., Dilworth, J. R., Thompson, R. M., McPartlin, M., Povey, D. C. & Kelly, J. D. (1993). J. Chem. Soc. Dalton Trans. pp. 461–466.

[bb2] Aslanov, L., Mason, R., Wheeler, A. G. & Whimp, P. O. (1970). J. Chem. Soc. Chem. Commun. pp. 30–31.

[bb3] Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.

[bb4] Brink, A., Roodt, A., Steyl, G. & Visser, H. G. (2010). J. Chem. Soc. Dalton Trans. 39, 5572—5578. [DOI] [PubMed]

[bb5] Bruker (2008). APEX2, SAINT-Plus and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.

[bb6] Clegg, W., Scott, A. J., Norman, N. C., Robins, E. G. & Whittell, G. R. (2002). Acta Cryst. E58, m410–m411.

[bb7] Drew, M. G. B., Tisley, D. G. & Walton, R. A. (1970). J. Chem. Soc. Chem. Commun. pp. 600–601.

[bb8] Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.

[bb9] Marko, L. & Heil, B. (1974). Catal. Rev. 8, 269–293.

[bb10] Nagy-Magos, Z., Vastag, S., Heil, B. & Marko, L. (1978). Transition Met. Chem. 3, 123–126.

[bb11] Oro, L. A., Manrique, A. & Royo, M. (1978). Transition Met. Chem. 3, 383–384.

[bb12] Roodt, A., Otto, S. & Steyl, G. (2003). Coord. Chem. Rev. 245, 121–137.

[bb13] Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]

PERMALINK

Acetonitriletrichloridobis(cyclohexyldiphenylphosphane)rhodium(III) acetonitrile disolvate

Theunis J Muller

Hendrik G Visser

Andreas Roodt

Abstract

Related literature

Experimental

Crystal data

Data collection

Refinement

Supplementary Material

Table 1. Selected bond lengths (Å).

Table 2. Hydrogen-bond geometry (Å, °).

Acknowledgments

supplementary crystallographic information

Comment

Experimental

Refinement

Figures

Fig. 1.

Crystal data

Data collection

Refinement

Special details

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

Atomic displacement parameters (Å²)

Geometric parameters (Å, °)

Hydrogen-bond geometry (Å, °)

Footnotes

References

Associated Data

Supplementary Materials

ACTIONS

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PERMALINK

Acetonitrile­trichloridobis(cyclo­hexyl­diphenyl­phosphane)rhodium(III) acetonitrile disolvate

Theunis J Muller

Hendrik G Visser

Andreas Roodt

Abstract

Related literature

Experimental

Crystal data

Data collection

Refinement

Supplementary Material

Table 1. Selected bond lengths (Å).

Table 2. Hydrogen-bond geometry (Å, °).

Acknowledgments

supplementary crystallographic information

Comment

Experimental

Refinement

Figures

Fig. 1.

Crystal data

Data collection

Refinement

Special details

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

Atomic displacement parameters (Å2)

Geometric parameters (Å, °)

Hydrogen-bond geometry (Å, °)

Footnotes

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

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Acetonitriletrichloridobis(cyclohexyldiphenylphosphane)rhodium(III) acetonitrile disolvate

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

Atomic displacement parameters (Å²)