cis-Tetra­kis(μ-N-phenyl­acetamidato)-κ4N:O;κ4O:N-bis­[(benzo­nitrile-κN)rhodium(II)](Rh—Rh)

Eagle, C.T.; Quarshie, F.; Ketron, M.E.; Atem-Tambe, N.

doi:10.1107/S1600536813012828

metal-organic compounds

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Volume 69| Part 6| June 2013| Page m329

doi:10.1107/S1600536813012828

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cis-Tetrakis(μ-N-phenylacetamidato)-κ⁴N:O;κ⁴O:N-bis[(benzonitrile-κN)rhodium(II)](Rh—Rh)

Cassandra T. Eagle,^a ^* Fredricka Quarshie,^a Megan E. Ketron ^a and Nkongho Atem-Tambe ^a

^aDepartment of Chemistry, East Tennessee State University, PO Box 70695, Johnson City, TN 37614, USA
^*Correspondence e-mail: eaglec@etsu.edu

(Received 23 January 2013; accepted 9 May 2013; online 18 May 2013)

The complex molecule of the title compound, [Rh₂{N(C₆H₅)COCH₃}₄(C₆H₅CN)₂], exhibits crystallographically imposed centrosymmetry. The four acetamide ligands bridging the dirhodium core are arranged in a 2,2-cis manner, with two N atoms and two O atoms coordinating to the unique Rh^II atom cis to one another. The N_eq—Rh—Rh—O_eq torsion angles on the acetamide bridges vary between 1.62 (4) and 1.78 (4)°. The Rh—Rh bond length is 2.4319 (3) Å. The axial nitrile ligand completes the distorted octahedral coordination sphere and shows a non-linear coordination with an Rh—N—C bond angle of 167.14 (15)°, while the N—C bond length is 1.135 (3) Å.

Related literature

For related structures, see: Bear & Kadish (1987 ); Eagle et al. (2000 , 2012 ).

Experimental

Crystal data

[Rh₂(C₈H₈NO)₄(C₇H₅N)₂]
M_r = 948.69
Monoclinic, P 2₁ /n
a = 10.2115 (7) Å
b = 9.9667 (7) Å
c = 21.3672 (16) Å
β = 100.971 (7)°
V = 2134.9 (3) Å³
Z = 2
Mo Kα radiation
μ = 0.82 mm⁻¹
T = 223 K
0.49 × 0.35 × 0.16 mm

Data collection

Rigaku XtaLAB mini diffractometer
Absorption correction: multi-scan (REQAB; Rigaku, 1998 ) T_min = 0.689, T_max = 0.880
21686 measured reflections
4872 independent reflections
4413 reflections with I > 2σ(I)
R_int = 0.023

Refinement

R[F² > 2σ(F²)] = 0.021
wR(F²) = 0.054
S = 1.03
4872 reflections
264 parameters
H-atom parameters constrained
Δρ_max = 0.39 e Å⁻³
Δρ_min = −0.34 e Å⁻³

Data collection: CrystalClear-SM Auto (Rigaku, 2011 ); cell refinement: CrystalClear-SM Auto; data reduction: CrystalClear-SM Auto; program(s) used to solve structure: SIR2004 (Burla et al., 2005 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: CrystalStructure (Rigaku, 2010 ); software used to prepare material for publication: CrystalStructure (Rigaku, 2010).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536813012828/mw2103sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813012828/mw2103Isup2.hkl

checkCIF report

Comment top

Previous papers report the structures of the related complexes 2,2-cis-Rh₂[N(C₆H₅)COCH₃]₄^.2DMSO (Bear et al. 1987), 2,2-trans-Rh₂[N(C₆H₅)COCH₃]₄^.2NCC₆H₅ (2) (Eagle et al., 2000) and 2,2-trans-Rh₂[N(C₉H₁₁)COCH₃]₄^.2NCC₆H₅ (3) (Eagle et al., 2012). The numbering scheme of the title compound was adapted from that of compound 2.

The axial rhodium-nitrogen-carbon bond angle for 1, 167.14 (15)°, (Fig. 1) is distinctly non-linear which is different from those found in 2 (178.5 (5)° and 169.3 (5)°) and 3 (180°; imposed by space group symmetry). The axial carbon-nitrogen bond length in 1 is 1.135 (3) Å which is comparable to the corresponding distances found in 2 (1.135 (8) and 1.145 (8) Å) and slightly longer than that in 3 (1.106 (6) Å). Compound 1 has pseudo four-fold symmetry with torsion angles on each acetamide bridge varying between 1.62 (4)° and 1.78 (4)°. These can be compared to the range of 9.03° and 11.89° in 2 and 1.12 (9)° in 3. A packing diagram of the structure is shown in Fig. 2 and indicates that van der Waals forces hold the molecules of 1 together.

The infrared absorption spectrum of 1 showed bands at 2359 and 2320 cm^-1 attributable to carbon-nitrogen bond stretching modes. The corresponding band for uncomplexed benzonitrile appears at 2228 cm^-1. This indicates that there is a shortening of the carbon-nitrogen bond and a stronger σ-interaction to the rhodium metal compared to the π-back-bonding which occurs upon complexation with cis-tetrakis[µ-N-(phenyl)acetamidato]-κ⁴N:O;κ⁴O:N rhodium(II)].

Related literature top

For related structures, see: Bear et al. (1987) and Eagle et al. (2000, 2012).

Experimental top

Approximately 10 mg of 2,2-cis-[Rh₂(N(C₆H₅)COCH₃)₄] was dissolved in 18 mL of dichloromethane. 10 µL of benzonitrile was then added to this solution, via a gas tight syringe, turning the solution from a green to a light blue color. Crystals grew over a one week period via vapor diffusion with acetone. From the structure determination compound 1 is an adduct of cis-tetrakis[µ-N-(phenyl)acetamidato]-κ⁴N:O;κ⁴O:N rhodium(II)] with benzonitrile in each axial site.

Computing details top

Data collection: CrystalClear-SM Auto (Rigaku, 2011); cell refinement: CrystalClear-SM Auto (Rigaku, 2011); data reduction: CrystalClear-SM Auto (Rigaku, 2011); program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalStructure (Rigaku, 2010); software used to prepare material for publication: CrystalStructure (Rigaku, 2010).

Figures top

	Fig. 1. ORTEP of the title compound showing 30% probability ellipsoids. Hydrogen atoms are drawn as small spheres.
	Fig. 2. Packing diagram for the title compound as seen along the b axis.

cis-Tetrakis(µ-N-phenylacetamidato)-κ⁴N:O;κ⁴O:N-bis[(benzonitrile-κN)rhodium(II)](Rh—Rh) top

Crystal data top

[Rh₂(C₈H₈NO)₄(C₇H₅N)₂]	F(000) = 964.00
M_r = 948.69	D_x = 1.476 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2yn	Cell parameters from 20104 reflections
a = 10.2115 (7) Å	θ = 3.2–27.5°
b = 9.9667 (7) Å	µ = 0.82 mm⁻¹
c = 21.3672 (16) Å	T = 223 K
β = 100.971 (7)°	Prism, red
V = 2134.9 (3) Å³	0.49 × 0.35 × 0.16 mm
Z = 2

Data collection top

Rigaku XtaLAB mini diffractometer	4413 reflections with F² > 2σ(F²)
Detector resolution: 6.827 pixels mm^-1	R_int = 0.023
ω scans	θ_max = 27.5°
Absorption correction: multi-scan (REQAB; Rigaku, 1998)	h = −13→13
T_min = 0.689, T_max = 0.880	k = −12→12
21686 measured reflections	l = −27→27
4872 independent reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.054	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0268P)² + 0.9991P] where P = (F_o² + 2F_c²)/3
4872 reflections	(Δ/σ)_max = 0.005
264 parameters	Δρ_max = 0.39 e Å⁻³
0 restraints	Δρ_min = −0.34 e Å⁻³
Primary atom site location: structure-invariant direct methods

Crystal data top

[Rh₂(C₈H₈NO)₄(C₇H₅N)₂]	V = 2134.9 (3) Å³
M_r = 948.69	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 10.2115 (7) Å	µ = 0.82 mm⁻¹
b = 9.9667 (7) Å	T = 223 K
c = 21.3672 (16) Å	0.49 × 0.35 × 0.16 mm
β = 100.971 (7)°

Data collection top

Rigaku XtaLAB mini diffractometer	4872 independent reflections
Absorption correction: multi-scan (REQAB; Rigaku, 1998)	4413 reflections with F² > 2σ(F²)
T_min = 0.689, T_max = 0.880	R_int = 0.023
21686 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	0 restraints
wR(F²) = 0.054	H-atom parameters constrained
S = 1.03	Δρ_max = 0.39 e Å⁻³
4872 reflections	Δρ_min = −0.34 e Å⁻³
264 parameters

Special details top

Refinement. Refinement was performed using all reflections. 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 (Å²) top

	x	y	z	U_iso*/U_eq
Rh1	0.987101 (12)	0.041420 (12)	0.552011 (5)	0.02306 (5)
O1	1.07504 (13)	−0.13034 (12)	0.59283 (5)	0.0343 (3)
O2	0.80499 (13)	−0.05051 (13)	0.53865 (6)	0.0347 (3)
N1	0.89591 (14)	0.20483 (14)	0.50448 (7)	0.0279 (3)
N2	1.17358 (13)	0.12274 (14)	0.55998 (6)	0.0267 (3)
N3	0.95315 (16)	0.11158 (17)	0.64638 (7)	0.0365 (4)
C1	1.12289 (18)	−0.21431 (17)	0.55768 (8)	0.0311 (4)
C3	0.75803 (17)	−0.10896 (17)	0.48590 (8)	0.0299 (4)
C5	0.83771 (17)	0.30448 (18)	0.53903 (8)	0.0321 (4)
C11	1.23573 (16)	0.18266 (18)	0.61898 (8)	0.0292 (4)
C18	0.89020 (19)	0.24259 (19)	0.74055 (8)	0.0358 (4)
C17	0.92479 (19)	0.16727 (19)	0.68819 (8)	0.0356 (4)
C16	1.2654 (2)	0.1039 (2)	0.67331 (9)	0.0400 (5)
C2	1.2038 (3)	−0.3258 (2)	0.59377 (10)	0.0456 (5)
C13	1.3258 (3)	0.3739 (3)	0.68191 (11)	0.0509 (6)
C4	0.61698 (19)	−0.1591 (3)	0.48041 (10)	0.0445 (5)
C19	0.7609 (3)	0.2429 (3)	0.75172 (11)	0.0524 (6)
C14	1.3553 (2)	0.2951 (3)	0.73554 (10)	0.0512 (6)
C10	0.9057 (3)	0.4201 (3)	0.55934 (13)	0.0560 (7)
C6	0.7144 (2)	0.2840 (3)	0.55464 (12)	0.0545 (6)
C8	0.7233 (3)	0.4990 (3)	0.60496 (15)	0.0680 (8)
C12	1.2654 (2)	0.31854 (19)	0.62366 (10)	0.0409 (5)
C7	0.6577 (3)	0.3819 (3)	0.58741 (15)	0.0697 (8)
C20	0.7314 (3)	0.3185 (3)	0.80154 (11)	0.0544 (6)
C9	0.8477 (3)	0.5177 (3)	0.59178 (17)	0.0758 (9)
C21	0.8268 (3)	0.3914 (3)	0.83920 (11)	0.0561 (6)
C23	0.9875 (3)	0.3163 (3)	0.77885 (11)	0.0611 (7)
C15	1.3258 (3)	0.1600 (3)	0.73092 (10)	0.0504 (6)
C22	0.9550 (3)	0.3898 (4)	0.82871 (13)	0.0771 (9)
H9	1.2446	0.0119	0.6710	0.0480*
H10A	1.2502	−0.2924	0.6346	0.0548*
H10B	1.2682	−0.3583	0.5694	0.0548*
H10C	1.1450	−0.3986	0.6006	0.0548*
H11	1.3466	0.4658	0.6845	0.0611*
H12A	0.5704	−0.1511	0.4366	0.0534*
H12B	0.5714	−0.1059	0.5077	0.0534*
H12C	0.6184	−0.2524	0.4934	0.0534*
H13	0.6941	0.1923	0.7258	0.0629*
H14	1.3950	0.3329	0.7749	0.0614*
H15	0.9920	0.4335	0.5512	0.0672*
H16	0.6684	0.2034	0.5431	0.0653*
H17	0.6834	0.5662	0.6259	0.0816*
H18	1.2446	0.3735	0.5874	0.0491*
H19	0.5733	0.3671	0.5976	0.0836*
H20	0.6439	0.3191	0.8093	0.0653*
H21	0.8946	0.5972	0.6048	0.0910*
H22	0.8052	0.4431	0.8726	0.0674*
H23	1.0753	0.3168	0.7713	0.0733*
H24	1.3468	0.1053	0.7673	0.0604*
H25	1.0215	0.4391	0.8556	0.0926*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rh1	0.03062 (7)	0.02261 (7)	0.01845 (7)	−0.00433 (5)	0.01099 (5)	−0.00399 (5)
O1	0.0538 (8)	0.0259 (6)	0.0250 (6)	−0.0002 (6)	0.0122 (6)	0.0003 (5)
O2	0.0396 (7)	0.0403 (7)	0.0290 (6)	−0.0155 (6)	0.0184 (6)	−0.0093 (6)
N1	0.0307 (7)	0.0264 (7)	0.0280 (7)	−0.0011 (6)	0.0087 (6)	−0.0042 (6)
N2	0.0292 (7)	0.0268 (7)	0.0249 (7)	−0.0039 (6)	0.0076 (6)	−0.0035 (6)
N3	0.0406 (9)	0.0419 (9)	0.0298 (8)	−0.0058 (7)	0.0140 (7)	−0.0090 (7)
C1	0.0376 (9)	0.0251 (8)	0.0308 (9)	−0.0041 (7)	0.0066 (7)	−0.0008 (7)
C3	0.0331 (9)	0.0286 (9)	0.0299 (9)	−0.0061 (7)	0.0110 (7)	−0.0026 (7)
C5	0.0323 (9)	0.0307 (9)	0.0332 (9)	0.0018 (7)	0.0058 (7)	−0.0056 (7)
C11	0.0264 (8)	0.0335 (9)	0.0275 (8)	0.0006 (7)	0.0048 (7)	−0.0063 (7)
C18	0.0435 (10)	0.0405 (10)	0.0264 (9)	0.0037 (9)	0.0148 (8)	−0.0042 (8)
C17	0.0404 (10)	0.0399 (10)	0.0288 (9)	−0.0032 (8)	0.0122 (8)	−0.0030 (8)
C16	0.0450 (11)	0.0423 (11)	0.0320 (10)	−0.0012 (9)	0.0056 (8)	−0.0006 (8)
C2	0.0604 (13)	0.0352 (10)	0.0380 (11)	0.0072 (10)	0.0009 (10)	0.0021 (9)
C13	0.0508 (12)	0.0414 (11)	0.0555 (13)	0.0017 (10)	−0.0027 (10)	−0.0205 (11)
C4	0.0353 (10)	0.0559 (13)	0.0456 (11)	−0.0143 (9)	0.0161 (9)	−0.0126 (10)
C19	0.0440 (12)	0.0684 (15)	0.0484 (12)	−0.0031 (11)	0.0178 (10)	−0.0126 (11)
C14	0.0416 (11)	0.0692 (15)	0.0384 (11)	0.0033 (11)	−0.0034 (9)	−0.0232 (11)
C10	0.0430 (12)	0.0450 (12)	0.0852 (18)	−0.0103 (10)	0.0256 (12)	−0.0277 (12)
C6	0.0380 (11)	0.0518 (13)	0.0778 (16)	−0.0093 (10)	0.0219 (11)	−0.0282 (12)
C8	0.0578 (15)	0.0585 (15)	0.091 (2)	0.0060 (13)	0.0224 (14)	−0.0397 (15)
C12	0.0458 (11)	0.0316 (10)	0.0411 (11)	0.0026 (8)	−0.0025 (9)	−0.0056 (8)
C7	0.0437 (13)	0.0741 (18)	0.098 (2)	−0.0029 (13)	0.0304 (13)	−0.0401 (17)
C20	0.0491 (13)	0.0688 (16)	0.0534 (13)	0.0122 (12)	0.0301 (11)	−0.0022 (12)
C9	0.0659 (17)	0.0508 (15)	0.116 (3)	−0.0130 (13)	0.0304 (17)	−0.0484 (16)
C21	0.0731 (16)	0.0614 (15)	0.0411 (12)	0.0123 (13)	0.0293 (11)	−0.0113 (11)
C23	0.0485 (13)	0.0875 (19)	0.0526 (14)	−0.0088 (13)	0.0233 (11)	−0.0350 (14)
C15	0.0527 (13)	0.0667 (15)	0.0285 (10)	0.0033 (11)	−0.0003 (9)	−0.0007 (10)
C22	0.0711 (17)	0.103 (3)	0.0626 (16)	−0.0158 (17)	0.0259 (14)	−0.0519 (17)

Geometric parameters (Å, º) top

Rh1—Rh1ⁱ	2.4319 (3)	C6—C7	1.390 (4)
Rh1—O1	2.0493 (12)	C8—C7	1.362 (4)
Rh1—O2	2.0438 (14)	C8—C9	1.365 (5)
Rh1—N1	2.0472 (14)	C20—C21	1.351 (4)
Rh1—N2	2.0466 (14)	C21—C22	1.369 (5)
Rh1—N3	2.2229 (16)	C23—C22	1.385 (4)
O1—C1	1.282 (3)	C16—H9	0.940
O2—C3	1.278 (2)	C2—H10A	0.970
N1—C1ⁱ	1.309 (3)	C2—H10B	0.970
N1—C5	1.432 (3)	C2—H10C	0.970
N2—C3ⁱ	1.315 (3)	C13—H11	0.940
N2—C11	1.430 (2)	C4—H12A	0.970
N3—C17	1.135 (3)	C4—H12B	0.970
C1—C2	1.507 (3)	C4—H12C	0.970
C3—C4	1.508 (3)	C19—H13	0.940
C5—C10	1.373 (3)	C14—H14	0.940
C5—C6	1.378 (3)	C10—H15	0.940
C11—C16	1.386 (3)	C6—H16	0.940
C11—C12	1.387 (3)	C8—H17	0.940
C18—C17	1.446 (3)	C12—H18	0.940
C18—C19	1.386 (3)	C7—H19	0.940
C18—C23	1.374 (3)	C20—H20	0.940
C16—C15	1.385 (3)	C9—H21	0.940
C13—C14	1.374 (4)	C21—H22	0.940
C13—C12	1.393 (3)	C23—H23	0.940
C19—C20	1.383 (4)	C15—H24	0.940
C14—C15	1.380 (4)	C22—H25	0.940
C10—C9	1.390 (5)

Rh1ⁱ—Rh1—O1	89.45 (4)	C19—C20—C21	120.9 (3)
Rh1ⁱ—Rh1—O2	88.51 (4)	C10—C9—C8	120.6 (3)
Rh1ⁱ—Rh1—N1	86.26 (5)	C20—C21—C22	120.0 (3)
Rh1ⁱ—Rh1—N2	87.11 (4)	C18—C23—C22	119.3 (3)
Rh1ⁱ—Rh1—N3	176.96 (5)	C16—C15—C14	120.8 (2)
O1—Rh1—O2	89.90 (5)	C21—C22—C23	120.6 (3)
O1—Rh1—N1	175.42 (5)	C11—C16—H9	119.8
O1—Rh1—N2	88.28 (6)	C15—C16—H9	119.8
O1—Rh1—N3	90.46 (6)	C1—C2—H10A	109.5
O2—Rh1—N1	88.37 (6)	C1—C2—H10B	109.5
O2—Rh1—N2	175.28 (6)	C1—C2—H10C	109.5
O2—Rh1—N3	88.45 (6)	H10A—C2—H10B	109.5
N1—Rh1—N2	93.12 (6)	H10A—C2—H10C	109.5
N1—Rh1—N3	93.73 (6)	H10B—C2—H10C	109.5
N2—Rh1—N3	95.92 (6)	C14—C13—H11	119.7
Rh1—O1—C1	118.76 (10)	C12—C13—H11	119.7
Rh1—O2—C3	120.41 (13)	C3—C4—H12A	109.5
Rh1—N1—C1ⁱ	121.73 (12)	C3—C4—H12B	109.5
Rh1—N1—C5	119.35 (11)	C3—C4—H12C	109.5
C1ⁱ—N1—C5	118.55 (14)	H12A—C4—H12B	109.5
Rh1—N2—C3ⁱ	120.96 (11)	H12A—C4—H12C	109.5
Rh1—N2—C11	119.25 (11)	H12B—C4—H12C	109.5
C3ⁱ—N2—C11	119.44 (14)	C18—C19—H13	120.4
Rh1—N3—C17	167.14 (15)	C20—C19—H13	120.4
O1—C1—N1ⁱ	123.29 (16)	C13—C14—H14	120.4
O1—C1—C2	114.51 (16)	C15—C14—H14	120.4
N1ⁱ—C1—C2	122.20 (17)	C5—C10—H15	119.7
O2—C3—N2ⁱ	122.80 (16)	C9—C10—H15	119.8
O2—C3—C4	114.33 (17)	C5—C6—H16	119.8
N2ⁱ—C3—C4	122.86 (16)	C7—C6—H16	119.8
N1—C5—C10	120.72 (18)	C7—C8—H17	120.4
N1—C5—C6	120.67 (17)	C9—C8—H17	120.4
C10—C5—C6	118.6 (2)	C11—C12—H18	119.9
N2—C11—C16	119.43 (16)	C13—C12—H18	119.9
N2—C11—C12	121.70 (16)	C6—C7—H19	119.7
C16—C11—C12	118.85 (17)	C8—C7—H19	119.7
C17—C18—C19	121.03 (18)	C19—C20—H20	119.6
C17—C18—C23	118.9 (2)	C21—C20—H20	119.6
C19—C18—C23	120.1 (2)	C10—C9—H21	119.7
N3—C17—C18	178.0 (2)	C8—C9—H21	119.7
C11—C16—C15	120.3 (2)	C20—C21—H22	120.0
C14—C13—C12	120.6 (2)	C22—C21—H22	120.0
C18—C19—C20	119.2 (2)	C18—C23—H23	120.4
C13—C14—C15	119.2 (2)	C22—C23—H23	120.4
C5—C10—C9	120.5 (3)	C16—C15—H24	119.6
C5—C6—C7	120.4 (2)	C14—C15—H24	119.6
C7—C8—C9	119.2 (3)	C21—C22—H25	119.7
C11—C12—C13	120.28 (19)	C23—C22—H25	119.7
C6—C7—C8	120.7 (3)

O1—Rh1—Rh1ⁱ—O2ⁱ	−90.08 (4)	N1—Rh1—Rh1ⁱ—O1ⁱ	1.62 (4)
O1—Rh1—Rh1ⁱ—N1ⁱ	−1.62 (4)	N1—Rh1—Rh1ⁱ—O2ⁱ	91.54 (4)
O1—Rh1—Rh1ⁱ—N2ⁱ	91.69 (4)	N1—Rh1—Rh1ⁱ—N2ⁱ	−86.68 (4)
O2—Rh1—Rh1ⁱ—O1ⁱ	90.08 (4)	N2—Rh1—Rh1ⁱ—O1ⁱ	−91.69 (4)
O2—Rh1—Rh1ⁱ—N1ⁱ	−91.54 (4)	N2—Rh1—Rh1ⁱ—O2ⁱ	−1.78 (4)
O2—Rh1—Rh1ⁱ—N2ⁱ	1.78 (4)	N2—Rh1—Rh1ⁱ—N1ⁱ	86.68 (4)

Symmetry code: (i) −x+2, −y, −z+1.

Experimental details

Crystal data
Chemical formula	[Rh₂(C₈H₈NO)₄(C₇H₅N)₂]
M_r	948.69
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	223
a, b, c (Å)	10.2115 (7), 9.9667 (7), 21.3672 (16)
β (°)	100.971 (7)
V (Å³)	2134.9 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.82
Crystal size (mm)	0.49 × 0.35 × 0.16

Data collection
Diffractometer	Rigaku XtaLAB mini diffractometer
Absorption correction	Multi-scan (REQAB; Rigaku, 1998)
T_min, T_max	0.689, 0.880
No. of measured, independent and observed [F² > 2σ(F²)] reflections	21686, 4872, 4413
R_int	0.023
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.054, 1.03
No. of reflections	4872
No. of parameters	264
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.39, −0.34

Computer programs: CrystalClear-SM Auto (Rigaku, 2011), SIR2004 (Burla et al., 2005), SHELXL97 (Sheldrick, 2008), CrystalStructure (Rigaku, 2010).

Acknowledgements

We thank Dr Lee Daniels of Rigaku Americas for his training on the Rigaku XtaLAB diffractometer and his extended help in the completion of the structure determination. Support was provided by a Start Up Grant from ETSU. We thank Johnson Matthey for their generous loan of rhodium trichloride.

References

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