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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 12| December 2011| Page m1666
https://doi.org/10.1107/S1600536811045715

trans-Carbonyl­chloridobis(tri-o-tolyl­phosphane-κP)rhodium(I)

Stefan Warsink,a* Renier Koena and Andreas Roodta

aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
*Correspondence e-mail: 2011009426@ufs4life.ac.za

(Received 19 October 2011; accepted 31 October 2011; online 5 November 2011)

In the title compound, [RhCl(C21H21P)2(CO)], the coordination geometry around the RhI atom is slightly distorted square-planar with the phosphane ligands in trans positions with respect to each other. The chloride and carbonyl ligands show positional disorder, and the RhI atom lies on a center of inversion. The effective cone angle ΘE for the title compound is 169.0 (3)°. There are no significant inter­molecular inter­actions.

Related literature

For background information, see: Angoletta (1959[Angoletta, M. (1959). Gazz. Chim. Ital. 89, 2359-2361.]); Vaska & Di Luzio (1961[Vaska, L. & Di Luzio, J. W. (1961). J. Am. Chem. Soc. 83, 2784-2785.]); For a review of related compounds, see: Roodt et al. (2003[Roodt, A., Otto, S. & Steyl, G. (2003). Coord. Chem. Rev. 245, 121-137.]). For related structures, see: Meijboom et al. (2005[Meijboom, R., Muller, A. & Roodt, A. (2005). Acta Cryst. E61, m699-m701.]); Otto et al. (1999[Otto, S., Mzamane, S. N. & Roodt, A. (1999). Acta Cryst. C55, 67-69.]).

[Scheme 1]

Experimental

Crystal data

  • [RhCl(C21H21P)2(CO)]

  • Mr = 775.07

  • Monoclinic, P 21 /n

  • a = 10.6440 (14) Å

  • b = 10.9464 (15) Å

  • c = 15.605 (2) Å

  • β = 93.102 (5)°

  • V = 1815.5 (4) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.67 mm−1

  • T = 100 K

  • 0.30 × 0.17 × 0.12 mm
Data collection

  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.872, Tmax = 0.921

  • 21616 measured reflections

  • 4481 independent reflections

  • 3344 reflections with I > 2σ(I)

  • Rint = 0.078
Refinement

  • R[F2 > 2σ(F2)] = 0.049

  • wR(F2) = 0.143

  • S = 1.03

  • 4481 reflections

  • 235 parameters

  • H-atom parameters constrained

  • Δρmax = 2.35 e Å−3

  • Δρmin = −1.13 e Å−3

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus and XPREP (Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: Mercury (Macrae et al., 2008[Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811045715/pv2465sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811045715/pv2465Isup2.hkl

checkCIF report


Comment top

The complex first synthesized by Angoletta (1959) and later correctly formulated by Vaska (Vaska & Di Luzio, 1961), trans-[IrCl(CO)(PPh3)2] has become known under the name of the latter. This complex and its analogues have been extensively used as catalysts and model compounds (Roodt et al., 2003).

Here we report a rhodium analogue bearing o-tolyl substituents on the phosphane ligands (I). As with many of these 'Vaska complexes', compound (I) crystallized with the metal on a crystallographric centre of symmetry, leading to a 50/50 disorder for the chloride and carbonyl ligands. With this report, Vaska complexes bearing all isomers of tritolylphosphane have been described. Compound (I) crystallizes in a slightly distorted square planar geometry with the phosphane ligands in trans-position to each other (Fig. 1).

The Rh—C and Rh—Cl bonds do not show large deviations from similar complexes, showing that the steric influence of the o-methyl substituents is not so significant as to distort the coordination geometry to a large degree. However, the Rh—P bond is longer than in similar complexes, indicating that the bulky ortho-aryl substituents force the phosphane ligands away from the rhodium. A useful indicator for the steric influence of phosphane ligands is the effective cone angle ΘE. For compound (I) this angle was found to be 169.0 (3) °, significantly larger than differently substituted triarylphosphanes like tri(m-tolyl)-phosphane, for which values of 155° and 160° were reported (Meijboom et al., 2005).

Related literature top

For background information, see: Angoletta (1959); Vaska & Di Luzio (1961); For a review of medle compounds, See: Roodt et al. (2003). For related structures, see: Meijboom et al. (2005); Otto et al. (1999).

Experimental top

Compound (I) was synthesized by slow addition of 4 equivalents of tri(o-tolyl)phosphane to a dimethyl formamide solution of [RhCl(CO)2]2. After precipitation with ice water and separation of the product, it was recrystallized by slow evaporation from a 1:5 dichloromethane/hexane mixture. Analysis of the compound showed a CO stretching signal in IR at 1972 cm-1, and a signal for the phosphane ligands in 31P NMR at 25.7 p.p.m. with a JRh-P of 125.9 Hz. These signals are in good agreement with various other rhodium Vaska's complexes.

Refinement top

The aromatic and methyl H atoms were placed in geometrically idealized positions (C—H = 0.93 and 0.96 Å, respectively) and constrained to ride on their parent atoms with Uiso(H) = 1.2Ueq(C) for aromatic, and Uiso(H) = 1.5Ueq(C) for methyl H-atoms. The highest residual electron density was located 0.87 Å from Rh1 and was essentially meaningless.

Structure description top

The complex first synthesized by Angoletta (1959) and later correctly formulated by Vaska (Vaska & Di Luzio, 1961), trans-[IrCl(CO)(PPh3)2] has become known under the name of the latter. This complex and its analogues have been extensively used as catalysts and model compounds (Roodt et al., 2003).

Here we report a rhodium analogue bearing o-tolyl substituents on the phosphane ligands (I). As with many of these 'Vaska complexes', compound (I) crystallized with the metal on a crystallographric centre of symmetry, leading to a 50/50 disorder for the chloride and carbonyl ligands. With this report, Vaska complexes bearing all isomers of tritolylphosphane have been described. Compound (I) crystallizes in a slightly distorted square planar geometry with the phosphane ligands in trans-position to each other (Fig. 1).

The Rh—C and Rh—Cl bonds do not show large deviations from similar complexes, showing that the steric influence of the o-methyl substituents is not so significant as to distort the coordination geometry to a large degree. However, the Rh—P bond is longer than in similar complexes, indicating that the bulky ortho-aryl substituents force the phosphane ligands away from the rhodium. A useful indicator for the steric influence of phosphane ligands is the effective cone angle ΘE. For compound (I) this angle was found to be 169.0 (3) °, significantly larger than differently substituted triarylphosphanes like tri(m-tolyl)-phosphane, for which values of 155° and 160° were reported (Meijboom et al., 2005).

For background information, see: Angoletta (1959); Vaska & Di Luzio (1961); For a review of medle compounds, See: Roodt et al. (2003). For related structures, see: Meijboom et al. (2005); Otto et al. (1999).

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: Mercury (Macrae et al., 2008); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. Molecular Structure of (I). Displacement ellipsoids are drawn at the 50% probability level [symmetry code: (i) -x, -y, 1 - z]. H atoms and disordered Chlorido and carbonyl ligands have been omitted for clarity.
trans-Carbonylchloridobis(tri-o-tolylphosphane- κP)rhodium(I) top
Crystal data top
[RhCl(C21H21P)2(CO)]F(000) = 800
Mr = 775.07Dx = 1.418 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ynCell parameters from 6713 reflections
a = 10.6440 (14) Åθ = 2.3–28.1°
b = 10.9464 (15) ŵ = 0.67 mm−1
c = 15.605 (2) ÅT = 100 K
β = 93.102 (5)°Cuboid, yellow
V = 1815.5 (4) Å30.30 × 0.17 × 0.12 mm
Z = 2
Data collection top
Bruker X8 APEXII 4K KappaCCD
diffractometer		4481 independent reflections
Radiation source: sealed tube3344 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.078
Detector resolution: 512 pixels mm-1θmax = 28.3°, θmin = 2.3°
φ and ω scansh = −12→14
Absorption correction: multi-scan
(SADABS; Bruker, 2007)		k = −13→14
Tmin = 0.872, Tmax = 0.921l = −20→19
21616 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.143H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0845P)2 + 0.2003P]
where P = (Fo2 + 2Fc2)/3
4481 reflections(Δ/σ)max = 0.001
235 parametersΔρmax = 2.35 e Å−3
0 restraintsΔρmin = −1.13 e Å−3
Crystal data top
[RhCl(C21H21P)2(CO)]V = 1815.5 (4) Å3
Mr = 775.07Z = 2
Monoclinic, P21/nMo Kα radiation
a = 10.6440 (14) ŵ = 0.67 mm−1
b = 10.9464 (15) ÅT = 100 K
c = 15.605 (2) Å0.30 × 0.17 × 0.12 mm
β = 93.102 (5)°
Data collection top
Bruker X8 APEXII 4K KappaCCD
diffractometer		4481 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2007)		3344 reflections with I > 2σ(I)
Tmin = 0.872, Tmax = 0.921Rint = 0.078
21616 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0490 restraints
wR(F2) = 0.143H-atom parameters constrained
S = 1.03Δρmax = 2.35 e Å−3
4481 reflectionsΔρmin = −1.13 e Å−3
235 parameters
Special details top

Experimental. The intensity data was collected on a Bruker X8 Apex II 4 K Kappa CCD diffractometer using an exposure time of 60 s/frame. A total of 1376 frames was collected with a frame width of 0.5° covering up to θ=28.27° with 99.5% 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.1009 (10)−0.1237 (10)0.4794 (7)0.025 (2)0.50
C20.2646 (3)0.1270 (3)0.4195 (2)0.0193 (7)
C30.3138 (3)0.1696 (3)0.4992 (2)0.0249 (8)
C40.4438 (4)0.1739 (3)0.5146 (3)0.0294 (8)
H100.47650.20610.56630.035*
C50.5256 (4)0.1321 (3)0.4558 (3)0.0312 (9)
H60.61210.13590.46760.037*
C60.4771 (3)0.0841 (3)0.3786 (2)0.0279 (8)
H150.53110.05370.33890.033*
C70.3484 (3)0.0814 (3)0.3608 (2)0.0230 (7)
H90.31680.04880.30900.028*
C80.2326 (4)0.2095 (4)0.5707 (2)0.0345 (9)
H24A0.15270.23740.54670.052*
H24B0.27360.27470.60240.052*
H24C0.21980.14180.60830.052*
C90.0342 (3)0.2733 (3)0.3794 (2)0.0211 (7)
C100.1102 (4)0.3733 (3)0.4027 (2)0.0263 (8)
H220.19100.36030.42660.032*
C110.0664 (4)0.4919 (3)0.3905 (3)0.0327 (9)
H180.11740.55810.40620.039*
C12−0.0537 (4)0.5105 (3)0.3547 (3)0.0362 (10)
H4−0.08360.58970.34620.043*
C13−0.1299 (4)0.4121 (4)0.3314 (3)0.0319 (9)
H19−0.21020.42640.30700.038*
C14−0.0886 (3)0.2918 (3)0.3437 (2)0.0238 (7)
C15−0.1760 (3)0.1889 (4)0.3142 (2)0.0285 (8)
H14A−0.15280.16000.25920.043*
H14B−0.26110.21840.30970.043*
H14C−0.16950.12330.35500.043*
C160.0791 (3)0.0561 (3)0.2837 (2)0.0188 (7)
C170.1169 (3)0.1212 (3)0.2114 (2)0.0222 (7)
C180.0976 (3)0.0660 (4)0.1308 (2)0.0271 (8)
H230.12150.10740.08220.033*
C190.0436 (4)−0.0488 (4)0.1218 (2)0.0305 (8)
H170.0326−0.08380.06760.037*
C200.0061 (3)−0.1115 (3)0.1923 (2)0.0286 (8)
H13−0.0311−0.18800.18580.034*
C210.0239 (3)−0.0601 (3)0.2729 (2)0.0235 (7)
H5−0.0008−0.10290.32060.028*
C220.1748 (4)0.2474 (3)0.2150 (2)0.0273 (8)
H16A0.21790.26190.16350.041*
H16B0.23340.25290.26380.041*
H16C0.10980.30730.22000.041*
O10.1652 (12)−0.2035 (10)0.4677 (9)0.030 (3)0.50
P10.09397 (8)0.11591 (8)0.39409 (6)0.0182 (2)
Cl10.1376 (3)−0.1671 (3)0.4666 (2)0.0226 (7)0.50
Rh10.00000.00000.50000.01825 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.029 (6)0.018 (6)0.027 (5)−0.004 (4)0.001 (4)−0.004 (4)
C20.0171 (15)0.0122 (15)0.0287 (17)−0.0030 (12)0.0015 (13)0.0071 (13)
C30.0302 (19)0.0125 (16)0.0319 (19)−0.0026 (14)0.0020 (15)0.0026 (14)
C40.0285 (19)0.0198 (19)0.039 (2)−0.0063 (15)−0.0085 (16)0.0042 (16)
C50.0226 (18)0.023 (2)0.048 (2)−0.0048 (15)−0.0030 (16)0.0143 (17)
C60.0220 (17)0.0217 (19)0.040 (2)0.0005 (14)0.0065 (15)0.0088 (16)
C70.0245 (17)0.0132 (16)0.0314 (19)−0.0003 (13)0.0024 (14)0.0032 (14)
C80.037 (2)0.037 (2)0.029 (2)−0.0065 (18)0.0011 (16)−0.0055 (17)
C90.0238 (17)0.0160 (16)0.0244 (17)−0.0018 (13)0.0089 (13)0.0005 (14)
C100.0303 (19)0.0183 (18)0.0309 (19)−0.0033 (15)0.0083 (15)−0.0002 (15)
C110.041 (2)0.0162 (18)0.042 (2)−0.0027 (16)0.0131 (18)−0.0035 (16)
C120.045 (2)0.020 (2)0.046 (2)0.0091 (17)0.016 (2)0.0019 (17)
C130.032 (2)0.025 (2)0.040 (2)0.0087 (16)0.0080 (16)0.0019 (17)
C140.0231 (17)0.0233 (18)0.0259 (18)0.0018 (14)0.0097 (14)0.0017 (14)
C150.0215 (17)0.031 (2)0.033 (2)0.0027 (15)0.0019 (14)0.0020 (16)
C160.0165 (15)0.0171 (17)0.0228 (16)0.0001 (13)0.0013 (12)−0.0004 (14)
C170.0179 (16)0.0210 (18)0.0279 (18)0.0032 (13)0.0036 (13)0.0002 (14)
C180.0267 (18)0.029 (2)0.0256 (18)0.0086 (16)0.0012 (14)0.0007 (15)
C190.030 (2)0.031 (2)0.030 (2)0.0074 (17)−0.0033 (15)−0.0135 (17)
C200.0250 (18)0.0208 (18)0.040 (2)0.0014 (15)−0.0034 (15)−0.0072 (16)
C210.0197 (16)0.0218 (19)0.0292 (18)0.0033 (14)0.0028 (13)0.0007 (15)
C220.0302 (19)0.0255 (19)0.0268 (19)−0.0044 (15)0.0079 (15)0.0041 (15)
O10.028 (5)0.020 (6)0.041 (4)0.007 (4)0.011 (4)0.006 (4)
P10.0184 (4)0.0132 (4)0.0233 (4)−0.0029 (3)0.0037 (3)−0.0007 (3)
Cl10.025 (2)0.016 (2)0.0269 (13)0.0042 (13)0.0070 (13)0.0036 (16)
Rh10.01767 (19)0.0145 (2)0.0230 (2)−0.00172 (14)0.00487 (14)0.00057 (14)
Geometric parameters (Å, º) top
C1—Cl10.654 (9)C13—C141.399 (5)
C1—O11.131 (11)C13—H190.9300
C1—Rh11.769 (11)C14—C151.516 (5)
C2—C31.402 (5)C15—H14A0.9600
C2—C71.405 (5)C15—H14B0.9600
C2—P11.842 (3)C15—H14C0.9600
C3—C41.393 (5)C16—C211.408 (5)
C3—C81.513 (5)C16—C171.411 (5)
C4—C51.377 (6)C16—P11.841 (3)
C4—H100.9300C17—C181.401 (5)
C5—C61.387 (5)C17—C221.513 (5)
C5—H60.9300C18—C191.386 (6)
C6—C71.383 (5)C18—H230.9300
C6—H150.9300C19—C201.373 (6)
C7—H90.9300C19—H170.9300
C8—H24A0.9600C20—C211.382 (5)
C8—H24B0.9600C20—H130.9300
C8—H24C0.9600C21—H50.9300
C9—C101.398 (5)C22—H16A0.9600
C9—C141.407 (5)C22—H16B0.9600
C9—P11.846 (4)C22—H16C0.9600
C10—C111.389 (5)P1—Rh12.3496 (10)
C10—H220.9300Cl1—Rh12.418 (3)
C11—C121.383 (7)Rh1—C1i1.769 (11)
C11—H180.9300Rh1—P1i2.3496 (10)
C12—C131.385 (6)Rh1—Cl1i2.418 (3)
C12—H40.9300
Cl1—C1—Rh1172.6 (14)H14A—C15—H14C109.5
O1—C1—Rh1178.8 (14)H14B—C15—H14C109.5
C3—C2—C7118.4 (3)C21—C16—C17119.7 (3)
C3—C2—P1122.0 (3)C21—C16—P1116.6 (2)
C7—C2—P1119.3 (3)C17—C16—P1123.7 (3)
C4—C3—C2119.0 (3)C18—C17—C16117.8 (3)
C4—C3—C8117.7 (3)C18—C17—C22117.8 (3)
C2—C3—C8123.3 (3)C16—C17—C22124.4 (3)
C5—C4—C3122.1 (4)C19—C18—C17121.4 (3)
C5—C4—H10119.0C19—C18—H23119.3
C3—C4—H10119.0C17—C18—H23119.3
C4—C5—C6119.0 (3)C20—C19—C18120.6 (3)
C4—C5—H6120.5C20—C19—H17119.7
C6—C5—H6120.5C18—C19—H17119.7
C7—C6—C5120.0 (4)C19—C20—C21119.6 (4)
C7—C6—H15120.0C19—C20—H13120.2
C5—C6—H15120.0C21—C20—H13120.2
C6—C7—C2121.2 (3)C20—C21—C16120.9 (3)
C6—C7—H9119.4C20—C21—H5119.6
C2—C7—H9119.4C16—C21—H5119.6
C3—C8—H24A109.5C17—C22—H16A109.5
C3—C8—H24B109.5C17—C22—H16B109.5
H24A—C8—H24B109.5H16A—C22—H16B109.5
C3—C8—H24C109.5C17—C22—H16C109.5
H24A—C8—H24C109.5H16A—C22—H16C109.5
H24B—C8—H24C109.5H16B—C22—H16C109.5
C10—C9—C14120.2 (3)C16—P1—C2105.01 (15)
C10—C9—P1120.5 (3)C16—P1—C9101.78 (16)
C14—C9—P1119.3 (3)C2—P1—C9107.12 (15)
C11—C10—C9120.7 (4)C16—P1—Rh1116.59 (11)
C11—C10—H22119.6C2—P1—Rh1109.66 (11)
C9—C10—H22119.6C9—P1—Rh1115.72 (11)
C12—C11—C10119.3 (4)C1—Rh1—C1i180.000 (2)
C12—C11—H18120.4C1—Rh1—P1i90.0 (4)
C10—C11—H18120.4C1i—Rh1—P1i90.0 (4)
C11—C12—C13120.5 (4)C1—Rh1—P190.0 (4)
C11—C12—H4119.8C1i—Rh1—P190.0 (4)
C13—C12—H4119.8P1i—Rh1—P1180.0
C12—C13—C14121.4 (4)C1—Rh1—Cl12.0 (4)
C12—C13—H19119.3C1i—Rh1—Cl1178.0 (4)
C14—C13—H19119.3P1i—Rh1—Cl191.66 (10)
C13—C14—C9117.9 (3)P1—Rh1—Cl188.34 (10)
C13—C14—C15118.3 (3)C1—Rh1—Cl1i178.0 (4)
C9—C14—C15123.7 (3)C1i—Rh1—Cl1i2.0 (4)
C14—C15—H14A109.5P1i—Rh1—Cl1i88.34 (10)
C14—C15—H14B109.5P1—Rh1—Cl1i91.66 (10)
H14A—C15—H14B109.5Cl1—Rh1—Cl1i180.00 (18)
C14—C15—H14C109.5
Symmetry code: (i) −x, −y, −z+1.

Experimental details

Crystal data
Chemical formula[RhCl(C21H21P)2(CO)]
Mr775.07
Crystal system, space groupMonoclinic, P21/n
Temperature (K)100
a, b, c (Å)10.6440 (14), 10.9464 (15), 15.605 (2)
β (°) 93.102 (5)
V (Å3)1815.5 (4)
Z2
Radiation typeMo Kα
µ (mm−1)0.67
Crystal size (mm)0.30 × 0.17 × 0.12
Data collection
DiffractometerBruker X8 APEXII 4K KappaCCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2007)
Tmin, Tmax0.872, 0.921
No. of measured, independent and
observed [I > 2σ(I)] reflections		21616, 4481, 3344
Rint0.078
(sin θ/λ)max (Å−1)0.666
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.143, 1.03
No. of reflections4481
No. of parameters235
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)2.35, −1.13

Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SAINT-Plus and XPREP (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), Mercury (Macrae et al., 2008), WinGX (Farrugia, 1999).

 

Acknowledgements

The authors thank SASOL, the South African NRF and THRIP and the University of the Free State Research Fund for financial support. The views expressed do not necessarily represent that of the NRF.

References

First citationAngoletta, M. (1959). Gazz. Chim. Ital. 89, 2359–2361.  CAS Google Scholar
 First citationBruker (2007). APEX2, SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationFarrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.  CrossRef CAS IUCr Journals Google Scholar
 First citationMacrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466–470.  Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
 First citationMeijboom, R., Muller, A. & Roodt, A. (2005). Acta Cryst. E61, m699–m701.  CSD CrossRef IUCr Journals Google Scholar
 First citationOtto, S., Mzamane, S. N. & Roodt, A. (1999). Acta Cryst. C55, 67–69.  CSD CrossRef CAS IUCr Journals Google Scholar
 First citationRoodt, A., Otto, S. & Steyl, G. (2003). Coord. Chem. Rev. 245, 121–137.  Web of Science CSD CrossRef CAS Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

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ISSN: 2056-9890
Volume 67| Part 12| December 2011| Page m1666
https://doi.org/10.1107/S1600536811045715
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