Dichlorido(η4-cyclo­octa-1,5-diene)bis­(propane­nitrile-κN)ruthenium(II)

Chiririwa, H.; Meijboom, R.

doi:10.1107/S1600536811035379

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 10| October 2011| Page m1336

https://doi.org/10.1107/S1600536811035379

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Dichlorido(η⁴-cycloocta-1,5-diene)bis(propanenitrile-κN)ruthenium(II)

Haleden Chiririwa ^a ^* and Reinout Meijboom ^a

^aResearch Centre for Synthesis and Catalysis, Department of Chemistry, University of Johannesburg, PO Box 524, Auckland Park, 2006 Johannesburg, South Africa
^*Correspondence e-mail: harrychiririwa@yahoo.com

(Received 16 August 2011; accepted 30 August 2011; online 14 September 2011)

In the title complex, [RuCl₂(C₈H₁₂)(C₃H₅N)₂], the metal ion is coordinated to both double bonds of the cycloocta-1,5-diene ligand, two chloride ions (in cis positions) and two N-atom donors from two propanenitrile molecules that complete the coordination sphere for the neutral complex. The coordination around the Ru^II atom can thus be considered as octahedral with slight trigonal distortion.

Related literature

For the structure of the acetonitrile derivative, see: Ashworth et al. (1987 ); Chiririwa et al. (2011 ). For the synthesis of starting materials, see: Ashworth et al. (1987).

Experimental

Crystal data

[RuCl₂(C₈H₁₂)(C₃H₅N)₂]
M_r = 390.31
Triclinic, $[P \overline 1]$
a = 7.593 (5) Å
b = 8.800 (5) Å
c = 12.658 (5) Å
α = 108.156 (5)°
β = 96.281 (5)°
γ = 90.536 (5)°
V = 798.0 (8) Å³
Z = 2
Mo Kα radiation
μ = 1.31 mm⁻¹
T = 100 K
0.29 × 0.28 × 0.21 mm

Data collection

Bruker APEXII CCD diffractometer
15438 measured reflections
3949 independent reflections
3911 reflections with I > 2σ(I)
R_int = 0.029

Refinement

R[F² > 2σ(F²)] = 0.017
wR(F²) = 0.043
S = 1.07
3949 reflections
174 parameters
H-atom parameters constrained
Δρ_max = 0.55 e Å⁻³
Δρ_min = −0.62 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus and XPREP (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ) and ORTEP-3 (Farrugia, 1997 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536811035379/im2311sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811035379/im2311Isup2.hkl

checkCIF report

Comment top

The present ruthenium complex, Fig.1, has been synthesized in a similar way as done earlier for the acetonitrile derivative (Chiririwa et al. 2011). Organonitrile solvate complexes are widely useful for synthesis of organometallic compounds because of facile substitution at the solvate coordination sites. Similarly, 1,5-cyclooctadiene complexes have found considerable use in organometallic chemistry as well.

The two propanenitrile ligands are trans to each other, although the N(2)—Ru(1)—N(1) angle is widened to 164.95 (5)° due to repulsion by the alkene bonds of the COD ligand. The corresponding angle is 163.15 (6)° in the acetonitrile derivative. One of the propanenitrile ligands is slightly bent as we observed earlier in the acetonitrile derivative. The N(2)—C(21)—C(22) bond angle is 176.8 (2)°. The C(21)—C(22)—C(23) and C(11)—C(12)—C(13) bond angles are slightly bigger than the ideal tetrahedral angle and are almost similar with values of 111.3 (1)° and 111.8 (1)° respectively.

Related literature top

For the structure of the acetonitrile derivative, see: Ashworth et al. (1987); Chiririwa et al. (2011). For the synthesis of starting materials, see: Ashworth et al. (1987).

Experimental top

A suspension of [{RuCl₂(COD)}_x] (0.5 g) in propanenitrile (30 ml) was refluxed for 8 h. The orange solution was filtered hot and concentrated on a steam bath to ca. half volume. Cooling to 0 °C overnight afforded orange crystals suitable for X-ray diffraction studies in 50% yield.

Structure description top

For the structure of the acetonitrile derivative, see: Ashworth et al. (1987); Chiririwa et al. (2011). For the synthesis of starting materials, see: Ashworth et al. (1987).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus and XPREP (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. Molecular structure of the title compound, showing 50% probability displacement ellipsoids.

Dichlorido(η⁴-cycloocta-1,5-diene)bis(propanenitrile-κN)ruthenium(II) top

Crystal data top

[RuCl₂(C₈H₁₂)(C₃H₅N)₂]	Z = 2
M_r = 390.31	F(000) = 396
Triclinic, P1	D_x = 1.624 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71069 Å
a = 7.593 (5) Å	Cell parameters from 9962 reflections
b = 8.800 (5) Å	θ = 3.0–28.3°
c = 12.658 (5) Å	µ = 1.31 mm⁻¹
α = 108.156 (5)°	T = 100 K
β = 96.281 (5)°	Block, orange
γ = 90.536 (5)°	0.29 × 0.28 × 0.21 mm
V = 798.0 (8) Å³

Data collection top

Bruker APEXII CCD diffractometer	3911 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.029
Graphite monochromator	θ_max = 28.3°, θ_min = 1.7°
φ and ω scans	h = −10→10
15438 measured reflections	k = −11→10
3949 independent reflections	l = −15→16

Refinement top

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)] = 0.017	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.043	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0132P)² + 0.6531P] where P = (F_o² + 2F_c²)/3
3949 reflections	(Δ/σ)_max = 0.002
174 parameters	Δρ_max = 0.55 e Å⁻³
0 restraints	Δρ_min = −0.62 e Å⁻³

Crystal data top

[RuCl₂(C₈H₁₂)(C₃H₅N)₂]	γ = 90.536 (5)°
M_r = 390.31	V = 798.0 (8) Å³
Triclinic, P1	Z = 2
a = 7.593 (5) Å	Mo Kα radiation
b = 8.800 (5) Å	µ = 1.31 mm⁻¹
c = 12.658 (5) Å	T = 100 K
α = 108.156 (5)°	0.29 × 0.28 × 0.21 mm
β = 96.281 (5)°

Data collection top

Bruker APEXII CCD diffractometer	3911 reflections with I > 2σ(I)
15438 measured reflections	R_int = 0.029
3949 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.017	0 restraints
wR(F²) = 0.043	H-atom parameters constrained
S = 1.07	Δρ_max = 0.55 e Å⁻³
3949 reflections	Δρ_min = −0.62 e Å⁻³
174 parameters

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
C1	−0.11889 (18)	0.24062 (16)	0.86381 (11)	0.0132 (2)
H1	−0.0776	0.3394	0.9141	0.016*
C2	−0.21829 (18)	0.23779 (16)	0.76462 (12)	0.0134 (2)
H2	−0.2427	0.3352	0.7532	0.016*
C3	−0.28956 (19)	0.08642 (17)	0.67378 (12)	0.0159 (3)
H3A	−0.3375	0.114	0.6083	0.019*
H3B	−0.3862	0.04	0.6995	0.019*
C4	−0.14983 (19)	−0.04040 (16)	0.63958 (12)	0.0147 (3)
H4A	−0.1537	−0.1125	0.6838	0.018*
H4B	−0.1805	−0.103	0.5616	0.018*
C5	0.03841 (18)	0.03064 (15)	0.65508 (11)	0.0121 (2)
H5	0.0783	0.0616	0.5976	0.015*
C6	0.15194 (18)	0.05054 (15)	0.75234 (11)	0.0125 (2)
H6	0.2672	0.0906	0.7565	0.015*
C7	0.09657 (19)	0.00994 (16)	0.85206 (12)	0.0151 (3)
H7A	0.1929	0.0421	0.9126	0.018*
H7B	0.0776	−0.1052	0.8317	0.018*
C8	−0.0737 (2)	0.09040 (17)	0.89491 (12)	0.0161 (3)
H8A	−0.1728	0.0129	0.8656	0.019*
H8B	−0.0608	0.1179	0.9758	0.019*
C11	0.30431 (19)	0.35812 (17)	0.98608 (12)	0.0154 (3)
C12	0.4147 (2)	0.37569 (18)	1.09193 (12)	0.0177 (3)
H12A	0.339	0.3788	1.1494	0.021*
H12B	0.4839	0.4762	1.1147	0.021*
C13	0.5395 (2)	0.2387 (2)	1.08180 (15)	0.0295 (4)
H13A	0.4716	0.1407	1.0687	0.044*
H13B	0.6184	0.2599	1.1499	0.044*
H13C	0.6072	0.2291	1.0205	0.044*
C21	−0.12818 (18)	0.32906 (16)	0.52863 (11)	0.0132 (2)
C22	−0.2237 (2)	0.37027 (19)	0.43512 (12)	0.0181 (3)
H22A	−0.1637	0.3277	0.3689	0.022*
H22B	−0.2228	0.4858	0.453	0.022*
C23	−0.4155 (2)	0.3029 (2)	0.41046 (14)	0.0225 (3)
H23A	−0.4167	0.1881	0.384	0.034*
H23B	−0.4781	0.341	0.3543	0.034*
H23C	−0.472	0.3374	0.4777	0.034*
N1	0.22016 (16)	0.33593 (14)	0.90225 (10)	0.0129 (2)
N2	−0.05984 (15)	0.30029 (13)	0.60433 (10)	0.0119 (2)
Cl1	0.33515 (4)	0.32622 (4)	0.67591 (3)	0.01333 (7)
Cl2	0.01618 (5)	0.57453 (4)	0.81456 (3)	0.01527 (7)
Ru1	0.065082 (13)	0.290208 (11)	0.752556 (8)	0.00846 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0144 (6)	0.0121 (6)	0.0140 (6)	−0.0003 (5)	0.0058 (5)	0.0043 (5)
C2	0.0118 (6)	0.0124 (6)	0.0170 (6)	0.0000 (5)	0.0043 (5)	0.0051 (5)
C3	0.0133 (6)	0.0147 (6)	0.0187 (6)	−0.0016 (5)	0.0014 (5)	0.0041 (5)
C4	0.0167 (6)	0.0120 (6)	0.0144 (6)	−0.0016 (5)	0.0013 (5)	0.0026 (5)
C5	0.0153 (6)	0.0089 (6)	0.0128 (6)	0.0013 (5)	0.0028 (5)	0.0036 (5)
C6	0.0158 (6)	0.0088 (6)	0.0139 (6)	0.0016 (5)	0.0025 (5)	0.0047 (5)
C7	0.0200 (7)	0.0128 (6)	0.0144 (6)	0.0010 (5)	0.0016 (5)	0.0073 (5)
C8	0.0226 (7)	0.0146 (6)	0.0142 (6)	0.0005 (5)	0.0056 (5)	0.0077 (5)
C11	0.0175 (7)	0.0137 (6)	0.0153 (6)	−0.0010 (5)	0.0027 (5)	0.0047 (5)
C12	0.0179 (7)	0.0207 (7)	0.0129 (6)	−0.0012 (5)	−0.0017 (5)	0.0041 (5)
C13	0.0230 (8)	0.0353 (9)	0.0248 (8)	0.0108 (7)	−0.0039 (6)	0.0039 (7)
C21	0.0141 (6)	0.0112 (6)	0.0147 (6)	−0.0006 (5)	0.0019 (5)	0.0044 (5)
C22	0.0171 (7)	0.0238 (7)	0.0169 (6)	0.0001 (5)	−0.0019 (5)	0.0129 (6)
C23	0.0172 (7)	0.0272 (8)	0.0218 (7)	−0.0018 (6)	−0.0044 (6)	0.0084 (6)
N1	0.0158 (5)	0.0117 (5)	0.0119 (5)	−0.0009 (4)	0.0018 (4)	0.0045 (4)
N2	0.0128 (5)	0.0101 (5)	0.0130 (5)	0.0004 (4)	0.0019 (4)	0.0039 (4)
Cl1	0.01152 (14)	0.01657 (15)	0.01382 (14)	0.00017 (11)	0.00207 (11)	0.00737 (12)
Cl2	0.02060 (16)	0.00875 (14)	0.01670 (15)	0.00064 (11)	0.00411 (12)	0.00369 (11)
Ru1	0.01012 (6)	0.00786 (6)	0.00801 (6)	0.00031 (4)	0.00092 (4)	0.00342 (4)

Geometric parameters (Å, º) top

C1—C2	1.386 (2)	C8—H8A	0.97
C1—C8	1.524 (2)	C8—H8B	0.97
C1—Ru1	2.2197 (15)	C11—N1	1.1368 (19)
C1—H1	0.93	C11—C12	1.465 (2)
C2—C3	1.512 (2)	C12—C13	1.523 (2)
C2—Ru1	2.2278 (19)	C12—H12A	0.97
C2—H2	0.93	C12—H12B	0.97
C3—C4	1.543 (2)	C13—H13A	0.96
C3—H3A	0.97	C13—H13B	0.96
C3—H3B	0.97	C13—H13C	0.96
C4—C5	1.522 (2)	C21—N2	1.1387 (19)
C4—H4A	0.97	C21—C22	1.4639 (19)
C4—H4B	0.97	C22—C23	1.529 (2)
C5—C6	1.386 (2)	C22—H22A	0.97
C5—Ru1	2.2274 (17)	C22—H22B	0.97
C5—H5	0.93	C23—H23A	0.96
C6—C7	1.5140 (19)	C23—H23B	0.96
C6—Ru1	2.2150 (17)	C23—H23C	0.96
C6—H6	0.93	N1—Ru1	2.0413 (14)
C7—C8	1.549 (2)	N2—Ru1	2.0356 (14)
C7—H7A	0.97	Cl1—Ru1	2.4211 (13)
C7—H7B	0.97	Cl2—Ru1	2.4231 (14)

C2—C1—C8	123.45 (12)	C11—C12—H12B	109.3
C2—C1—Ru1	72.16 (9)	C13—C12—H12B	109.3
C8—C1—Ru1	112.17 (9)	H12A—C12—H12B	107.9
C2—C1—H1	118.3	C12—C13—H13A	109.5
C8—C1—H1	118.3	C12—C13—H13B	109.5
Ru1—C1—H1	85.7	H13A—C13—H13B	109.5
C1—C2—C3	124.17 (13)	C12—C13—H13C	109.5
C1—C2—Ru1	71.53 (8)	H13A—C13—H13C	109.5
C3—C2—Ru1	111.07 (9)	H13B—C13—H13C	109.5
C1—C2—H2	117.9	N2—C21—C22	176.82 (15)
C3—C2—H2	117.9	C21—C22—C23	111.33 (13)
Ru1—C2—H2	87.4	C21—C22—H22A	109.4
C2—C3—C4	113.93 (12)	C23—C22—H22A	109.4
C2—C3—H3A	108.8	C21—C22—H22B	109.4
C4—C3—H3A	108.8	C23—C22—H22B	109.4
C2—C3—H3B	108.8	H22A—C22—H22B	108
C4—C3—H3B	108.8	C22—C23—H23A	109.5
H3A—C3—H3B	107.7	C22—C23—H23B	109.5
C5—C4—C3	113.59 (12)	H23A—C23—H23B	109.5
C5—C4—H4A	108.8	C22—C23—H23C	109.5
C3—C4—H4A	108.8	H23A—C23—H23C	109.5
C5—C4—H4B	108.8	H23B—C23—H23C	109.5
C3—C4—H4B	108.8	C11—N1—Ru1	178.21 (12)
H4A—C4—H4B	107.7	C21—N2—Ru1	170.17 (11)
C6—C5—C4	121.89 (12)	N2—Ru1—N1	164.95 (5)
C6—C5—Ru1	71.34 (8)	N2—Ru1—C6	115.27 (5)
C4—C5—Ru1	113.47 (9)	N1—Ru1—C6	76.54 (5)
C6—C5—H5	119.1	N2—Ru1—C1	113.39 (6)
C4—C5—H5	119.1	N1—Ru1—C1	76.63 (6)
Ru1—C5—H5	85.4	C6—Ru1—C1	80.71 (6)
C5—C6—C7	122.86 (13)	N2—Ru1—C5	79.67 (5)
C5—C6—Ru1	72.32 (8)	N1—Ru1—C5	112.85 (5)
C7—C6—Ru1	111.05 (9)	C6—Ru1—C5	36.35 (5)
C5—C6—H6	118.6	C1—Ru1—C5	87.81 (5)
C7—C6—H6	118.6	N2—Ru1—C2	77.11 (5)
Ru1—C6—H6	86.7	N1—Ru1—C2	112.46 (6)
C6—C7—C8	114.14 (11)	C6—Ru1—C2	94.63 (6)
C6—C7—H7A	108.7	C1—Ru1—C2	36.30 (5)
C8—C7—H7A	108.7	C5—Ru1—C2	79.57 (5)
C6—C7—H7B	108.7	N2—Ru1—Cl1	84.91 (5)
C8—C7—H7B	108.7	N1—Ru1—Cl1	86.21 (5)
H7A—C7—H7B	107.6	C6—Ru1—Cl1	88.31 (4)
C1—C8—C7	115.40 (11)	C1—Ru1—Cl1	161.35 (4)
C1—C8—H8A	108.4	C5—Ru1—Cl1	92.24 (4)
C7—C8—H8A	108.4	C2—Ru1—Cl1	161.29 (4)
C1—C8—H8B	108.4	N2—Ru1—Cl2	83.36 (4)
C7—C8—H8B	108.4	N1—Ru1—Cl2	85.00 (4)
H8A—C8—H8B	107.5	C6—Ru1—Cl2	161.36 (4)
N1—C11—C12	176.32 (15)	C1—Ru1—Cl2	92.67 (4)
C11—C12—C13	111.76 (13)	C5—Ru1—Cl2	161.68 (4)
C11—C12—H12A	109.3	C2—Ru1—Cl2	90.02 (4)
C13—C12—H12A	109.3	Cl1—Ru1—Cl2	93.06 (2)

C8—C1—C2—C3	−1.8 (2)	C8—C1—Ru1—C6	8.48 (10)
Ru1—C1—C2—C3	103.38 (13)	C2—C1—Ru1—C5	−75.28 (9)
C8—C1—C2—Ru1	−105.22 (13)	C8—C1—Ru1—C5	44.33 (10)
C1—C2—C3—C4	−49.30 (18)	C8—C1—Ru1—C2	119.61 (13)
Ru1—C2—C3—C4	32.14 (15)	C2—C1—Ru1—Cl1	−165.82 (9)
C2—C3—C4—C5	−28.89 (17)	C8—C1—Ru1—Cl1	−46.21 (17)
C3—C4—C5—C6	93.14 (16)	C2—C1—Ru1—Cl2	86.39 (8)
C3—C4—C5—Ru1	11.23 (15)	C8—C1—Ru1—Cl2	−154.00 (9)
C4—C5—C6—C7	−2.5 (2)	C6—C5—Ru1—N2	168.49 (9)
Ru1—C5—C6—C7	104.06 (12)	C4—C5—Ru1—N2	−74.04 (10)
C4—C5—C6—Ru1	−106.56 (12)	C6—C5—Ru1—N1	−2.75 (9)
C5—C6—C7—C8	−53.39 (18)	C4—C5—Ru1—N1	114.72 (10)
Ru1—C6—C7—C8	28.63 (14)	C4—C5—Ru1—C6	117.46 (13)
C2—C1—C8—C7	87.27 (17)	C6—C5—Ru1—C1	−77.26 (9)
Ru1—C1—C8—C7	4.58 (15)	C4—C5—Ru1—C1	40.21 (10)
C6—C7—C8—C1	−22.28 (17)	C6—C5—Ru1—C2	−112.87 (9)
C5—C6—Ru1—N2	−12.53 (9)	C4—C5—Ru1—C2	4.60 (10)
C7—C6—Ru1—N2	−131.71 (10)	C6—C5—Ru1—Cl1	84.08 (9)
C5—C6—Ru1—N1	177.40 (9)	C4—C5—Ru1—Cl1	−158.46 (9)
C7—C6—Ru1—N1	58.22 (10)	C6—C5—Ru1—Cl2	−169.16 (9)
C5—C6—Ru1—C1	99.03 (9)	C4—C5—Ru1—Cl2	−51.69 (17)
C7—C6—Ru1—C1	−20.15 (10)	C1—C2—Ru1—N2	−177.67 (9)
C7—C6—Ru1—C5	−119.18 (14)	C3—C2—Ru1—N2	61.93 (10)
C5—C6—Ru1—C2	65.39 (9)	C1—C2—Ru1—N1	−9.89 (9)
C7—C6—Ru1—C2	−53.79 (10)	C3—C2—Ru1—N1	−130.28 (10)
C5—C6—Ru1—Cl1	−96.10 (8)	C1—C2—Ru1—C6	67.44 (8)
C7—C6—Ru1—Cl1	144.72 (9)	C3—C2—Ru1—C6	−52.95 (11)
C5—C6—Ru1—Cl2	169.34 (9)	C3—C2—Ru1—C1	−120.39 (14)
C7—C6—Ru1—Cl2	50.16 (18)	C1—C2—Ru1—C5	100.66 (9)
C2—C1—Ru1—N2	2.47 (9)	C3—C2—Ru1—C5	−19.73 (10)
C8—C1—Ru1—N2	122.09 (10)	C1—C2—Ru1—Cl1	165.87 (9)
C2—C1—Ru1—N1	170.61 (9)	C3—C2—Ru1—Cl1	45.47 (18)
C8—C1—Ru1—N1	−69.77 (10)	C1—C2—Ru1—Cl2	−94.49 (8)
C2—C1—Ru1—C6	−111.14 (9)	C3—C2—Ru1—Cl2	145.12 (10)

Experimental details

Crystal data
Chemical formula	[RuCl₂(C₈H₁₂)(C₃H₅N)₂]
M_r	390.31
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	7.593 (5), 8.800 (5), 12.658 (5)
α, β, γ (°)	108.156 (5), 96.281 (5), 90.536 (5)
V (Å³)	798.0 (8)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.31
Crystal size (mm)	0.29 × 0.28 × 0.21

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	–
No. of measured, independent and observed [I > 2σ(I)] reflections	15438, 3949, 3911
R_int	0.029

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.017, 0.043, 1.07
No. of reflections	3949
No. of parameters	174
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.55, −0.62

Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SAINT-Plus and XPREP (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005) and ORTEP-3 (Farrugia, 1997), WinGX (Farrugia, 1999).

Acknowledgements

Financial assistance from the South African National Research Foundation (SA NRF), the Research Fund of the University of Johannesburg and SASOL is gratefully acknowledged.

References

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