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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 66| Part 3| March 2010| Page m338
doi:10.1107/S1600536810006732

Bis(tetra­phenyl­phospho­nium) tetra­iodidomanganate(II) acetone monosolvate

Ehsan Jaliliana* and Sven Lidinb

aDepartment of Enviromental and Material Chemistry, Arrhenius Laboratory, Stockholm University, 106 91 Stockholm, Sweden, and bPolymer and Materials Chemistry, Lund University, 221 00 Lund, Sweden
*Correspondence e-mail: ehsan.jalilian@mmk.su.se

(Received 29 January 2010; accepted 22 February 2010; online 27 February 2010)

The title compound, (C24H20P)2[MnI4]·(CH3)2CO, prepared from the reaction of manganese powder, iodine and tetra­phenyl­phospho­nium iodide in acetone shows a tetra­hedral complex anion [Mn—I = 2.6868 (5)–2.7281 (4) Å and I—Mn—I = 104.011 (13)–116.164 (15)°], two tetra­phenyl­phospho­nium cations and one mol­ecule of acetone.

Related literature

For a general text on the luminescence of tetra­hedral MnX4 (X = Cl, Br, I) complexes, see: Greenwood & Earnshaw (1984[Greenwood, N. N. & Earnshaw, A. (1984). Chemistry of the Elements, pp. 1231-1235. Oxford: Pergamon.]); Lee (1998[Lee, J. D. (1998). Concise Inorganic Chemistry, 5th ed., p. 742. Malden, USA: Blackwell.]). For structurally characterized MnX4 complexes, see: Barber et al. (1980[Barber, M., Bordoli, R. S., Hosseiny, A., Minten, K., Perkin, C. R., Sedgwick, R. D. & McAuliffe, C. A. (1980). Inorg. Chim. Acta Lett. 45, L89-L90.]); Beagley et al. (1984[Beagley, B., Briggs, J. C., Hosseiny, A., Hill, W. E., King, T. J., McAuliffe, C. A. & Minten, K. (1984). J. Chem. Soc. Chem. Commun. 5, 305-306.], 1992[Beagley, B., Mackie, A. G., Matear, P. P., McAuliffe, C. A., Ndifon, P. T. & Pritchard, R. G. (1992). J. Chem. Soc. Dalton Trans. pp. 1301-1304.]); Davies et al. (1982[Davies, J. I., Howard, C. G., Skapski, A. C. & Wilkinson, G. (1982). J. Chem. Soc. Chem. Commun. 18, 1077-1078.]); Godfrey et al. (1991[Godfrey, S. M., Kelly, D. G., Mackie, A. G., Rory, P. P. M., McAuliffe, C. A., Pritchard, R. G. & Watson, S. M. (1991). J. Chem. Soc. Chem. Commun. 20, 1447-1449.]); Howard et al. (1983[Howard, C. G., Wilkinson, G., Thorntonpett, M. & Hursthouse, M. B. (1983). J. Chem. Soc. Dalton Trans. pp. 2025-2030.]); Hosseiny et al. (1980[Hosseiny, A., McAuliffe, C. A., Minten, K., Parrott, M. J., Pritchard, R. & Tames, J. (1980). Inorg. Chim. Acta, 39, 227-231.], 1981[Hosseiny, A., Mackie, A. G., McAuliffe, C. A. & Minten, K. (1981). Inorg. Chim. Acta, 49, 99-105.]); McAuliffe et al. (1979[McAuliffe, C. A., Alkhateeb, H., Jones, M. H., Levason, W., Minten, K. & McCullough, F. P. (1979). J. Chem. Soc. Chem. Commun. 17, 736-738.], 1992[McAuliffe, C. A., Godfrey, S. M., Mackie, A. G. & Pritchard, R. G. (1992). J. Chem. Soc. Chem. Commun. 6, pp. 483-485.]); McAuliffe & Alkhateeb (1980[McAuliffe, C. A. & Alkhateeb, H. (1980). Inorg. Chim. Acta Lett. 45, L195-L196.]). For the extinction correction, see: Becker & Coppens (1974[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129-147.]).

[Scheme 1]

Experimental

Crystal data

  • (C24H20P)2[MnI4]·C3H6O

  • Mr = 1299.4

  • Monoclinic, P 21 /c

  • a = 19.5230 (4) Å

  • b = 14.9733 (3) Å

  • c = 17.6152 (4) Å

  • β = 105.161 (2)°

  • V = 4970.12 (19) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 2.85 mm−1

  • T = 100 K

  • 0.47 × 0.40 × 0.38 mm
Data collection

  • Oxford Diffraction Xcalibur3 with Sapphire-3 CCD detector diffractometer

  • Absorption correction: Gaussian (CrysAlis RED; Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]) Tmin = 0.388, Tmax = 0.480

  • 181649 measured reflections

  • 20267 independent reflections

  • 12474 reflections with I > 3σ(I)

  • Rint = 0.055
Refinement

  • R[F2 > 2σ(F2)] = 0.034

  • wR(F2) = 0.062

  • S = 1.17

  • 20267 reflections

  • 533 parameters

  • H-atom parameters constrained

  • Δρmax = 2.03 e Å−3

  • Δρmin = −1.59 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); data reduction: CrysAlis RED; program(s) used to solve structure: Superflip (Oszlányi & Sütő, 2004[Oszlányi, G. & Sütő, A. (2004). Acta Cryst. A60, 134-141.]); program(s) used to refine structure: JANA2000 (Petříček & Dušek, 2000[Petříček, V. & Dušek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic.]); molecular graphics: DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: JANA2000.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810006732/zs2027sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810006732/zs2027Isup2.hkl

checkCIF report


Comment top

Halide complexes with the composition [MnL4]2- (L = Cl,Br,I) are well known for their luminescence properties (Greenwood & Earnshaw, 1984; Lee, 1998) but there are structural data for the tetrahalo complexes in the Cambridge Structural Database (Barber et al. (1980); Beagley et al., 1984, 1992); Davies et al., 1982; Godfrey et al. (1991); Howard et al., 1983; Hosseiny et al., 1980, 1981); McAuliffe et al., 1979, 1992; McAuliffe & Alkhateeb, 1980), there is a surprising paucity of [MnI4]2- structures. The compound presented here, the acetone solvate 2[(C6H5)4P+] [Mn I4]2- . (CH3)2C═O (I), prepared from the reaction of manganese powder, iodine and tetraphenylphosphonium iodide in acetone under nitrogen, shows strong yellow luminescence. The strong absorbance of (I) in the visible spectrum is evident from the luminescence behaviour. Only very small crystals emit light homogeneously, while larger crystals emit primarily from the edges. The complex anion has tetrahedral stereochemistry with only small variations in Mn—I distances [range, 2.6868 (5)–2.7281 (4) Å] but has a somewhat larger variation in the I—Mn—I angles [104.011 (13)– 116.164 (15)°]. The counter cations are unexceptional with a narrow distribution of P—C and C—C distances [1.793 (3)–1.801 (3)Å and 1.369 (4)–1.409 (3)Å respectively], and C—P—C and (P/C)—C—C angles in the ranges 105.69 (12)–112.69 (12)° and 119.1 (2)–122.85 (19)° respectively.

Related literature top

For a general text on the luminescence of tetrahedral MnX4 (X = Cl,Br,I) complexes, see: Greenwood & Earnshaw (1984); Lee (1998). For structurally characterized MnX4 complexes, see: Barber et al. (1980); Beagley et al. (1984, 1992); Davies et al. (1982); Godfrey et al. (1991); Howard et al. (1983); Hosseiny et al. (1980, 1981); McAuliffe et al. (1979, 1992); McAuliffe & Alkhateeb (1980). For the extinction correction, see: Becker & Coppens (1974).

Experimental top

Tetraphenylphosphonium iodide (3.34 mmol), iodine (6.86 mmol) and manganese powder (28.26 mmol) were mixed and heated under reflux in acetone (50 ml) under a nitrogen atmosphere. After 4 hours the solution became pale yellow. The mixture was filtered while hot and the solution was kept at -10°C. Centimeter-sized yellow crystals formed over the course of several months.

Refinement top

The structure wase solved by charge-flipping (Oszlanyi & Suto, 2004), giving the I, Mn, P and O positions, and a major number of the C positions. Subsequently the remaining C positions were found using difference Fourier analysis. All non-hydrogen positions were refined using full matrix least squares. The hydrogen atoms were located by geometrical methods and were allowed to ride, with C–H = 1.00 Å and Ueq = 1.2Uiso(C).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2008); cell refinement: CrysAlis RED (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: Superflip (Oszlányi & Sütő, 2004); program(s) used to refine structure: JANA2000 (Petříček & Dušek, 2000); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: JANA2000 (Petříček & Dušek, 2000).

Figures top
[Figure 1] Fig. 1. Molecular structure and atom-labelling scheme for the two cations, the complex anion and the acetone molecule of solvation in (I). Non-H atoms are shown as 50% probability displacement ellipsoids.
Bis(tetraphenylphosphonium) tetraiodidomanganate(II) acetone solvate top
Crystal data top
(C24H20P)2[MnI4]·C3H6OF(000) = 2508
Mr = 1299.4Dx = 1.736 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 57375 reflections
a = 19.5230 (4) Åθ = 3.6–34.5°
b = 14.9733 (3) ŵ = 2.85 mm−1
c = 17.6152 (4) ÅT = 100 K
β = 105.161 (2)°Block, yellow
V = 4970.12 (19) Å30.47 × 0.40 × 0.38 mm
Z = 4
Data collection top
Oxford Diffraction Xcalibur3 with Sapphire-3 CCD detector
diffractometer		20267 independent reflections
Radiation source: Enhance (Mo) X-ray source12474 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.055
Detector resolution: 16.5467 pixels mm-1θmax = 34.6°, θmin = 3.6°
ω scansh = −30→30
Absorption correction: gaussian
(CrysAlis RED; Oxford Diffraction, 2008)		k = −23→23
Tmin = 0.388, Tmax = 0.480l = −28→27
181649 measured reflections
Refinement top
Refinement on F2Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2]
R[F2 > 2σ(F2)] = 0.034(Δ/σ)max = 0.027
wR(F2) = 0.062Δρmax = 2.03 e Å−3
S = 1.17Δρmin = −1.59 e Å−3
20267 reflectionsExtinction correction: B–C type 1 Gaussian isotropic (Becker & Coppens, 1974)
533 parametersExtinction coefficient: 3216
H-atom parameters constrained
Crystal data top
(C24H20P)2[MnI4]·C3H6OV = 4970.12 (19) Å3
Mr = 1299.4Z = 4
Monoclinic, P21/cMo Kα radiation
a = 19.5230 (4) ŵ = 2.85 mm−1
b = 14.9733 (3) ÅT = 100 K
c = 17.6152 (4) Å0.47 × 0.40 × 0.38 mm
β = 105.161 (2)°
Data collection top
Oxford Diffraction Xcalibur3 with Sapphire-3 CCD detector
diffractometer		20267 independent reflections
Absorption correction: gaussian
(CrysAlis RED; Oxford Diffraction, 2008)		12474 reflections with I > 3σ(I)
Tmin = 0.388, Tmax = 0.480Rint = 0.055
181649 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.034533 parameters
wR(F2) = 0.062H-atom parameters constrained
S = 1.17Δρmax = 2.03 e Å−3
20267 reflectionsΔρmin = −1.59 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
I10.363127 (8)0.413343 (12)0.250596 (9)0.01811 (5)
I20.267877 (9)0.620469 (12)0.356895 (10)0.01822 (5)
I30.141259 (9)0.494648 (12)0.139458 (10)0.02192 (5)
I40.195916 (9)0.328035 (14)0.355201 (13)0.03074 (7)
Mn0.237671 (18)0.46300 (3)0.27725 (2)0.01406 (11)
P10.47887 (3)0.30247 (5)0.01743 (4)0.01217 (18)
C1110.53341 (11)0.34965 (17)0.10643 (13)0.0123 (7)
C1120.60335 (12)0.31820 (18)0.13592 (14)0.0163 (8)
C1130.64455 (12)0.35154 (18)0.20608 (15)0.0175 (8)
C1140.61761 (12)0.41635 (19)0.24673 (14)0.0192 (8)
C1150.54947 (12)0.44842 (18)0.21707 (14)0.0169 (8)
C1160.50700 (12)0.41493 (17)0.14693 (13)0.0134 (7)
C1210.45766 (12)0.18827 (17)0.03195 (14)0.0138 (7)
C1220.39281 (13)0.15420 (18)−0.01153 (15)0.0194 (8)
C1230.37516 (15)0.06537 (19)−0.00242 (16)0.0245 (9)
C1240.42276 (15)0.0112 (2)0.04915 (16)0.0245 (9)
C1250.48694 (14)0.04433 (19)0.09243 (16)0.0231 (9)
C1260.50544 (13)0.13267 (18)0.08403 (15)0.0190 (8)
C1310.52539 (12)0.31146 (17)−0.05770 (13)0.0126 (7)
C1320.50406 (12)0.25842 (17)−0.12442 (14)0.0163 (8)
C1330.53392 (13)0.27192 (18)−0.18677 (15)0.0190 (8)
C1340.58487 (13)0.33707 (18)−0.18244 (15)0.0198 (8)
C1350.60681 (12)0.38938 (17)−0.11562 (15)0.0174 (8)
C1360.57672 (12)0.37746 (18)−0.05310 (14)0.0157 (7)
C1410.39641 (12)0.36202 (17)−0.01352 (14)0.0132 (7)
C1420.34925 (12)0.36048 (17)0.03393 (14)0.0162 (8)
C1430.28478 (12)0.40427 (18)0.01055 (15)0.0197 (8)
C1440.26611 (13)0.44760 (18)−0.06160 (16)0.0215 (8)
C1450.31231 (13)0.44827 (18)−0.10941 (16)0.0210 (8)
C1460.37791 (12)0.40604 (17)−0.08547 (14)0.0160 (7)
P20.06885 (3)0.86274 (4)0.17163 (4)0.01173 (18)
C2110.08918 (12)0.86045 (16)0.27704 (13)0.0130 (7)
C2120.15444 (12)0.83129 (18)0.32274 (14)0.0175 (8)
C2130.16835 (13)0.83290 (18)0.40413 (15)0.0208 (8)
C2140.11744 (14)0.86422 (17)0.43938 (15)0.0190 (8)
C2150.05190 (14)0.89340 (18)0.39351 (15)0.0198 (8)
C2160.03718 (13)0.89155 (17)0.31238 (14)0.0173 (8)
C2210.00816 (11)0.77516 (17)0.13074 (14)0.0132 (7)
C222−0.00761 (14)0.70859 (18)0.17697 (15)0.0210 (8)
C223−0.04934 (15)0.6372 (2)0.14317 (16)0.0258 (9)
C224−0.07579 (13)0.63309 (19)0.06201 (16)0.0231 (9)
C225−0.06029 (13)0.70026 (19)0.01553 (15)0.0210 (8)
C226−0.01808 (13)0.77095 (19)0.04895 (14)0.0194 (8)
C2310.03084 (12)0.97044 (17)0.14318 (14)0.0145 (7)
C2320.07276 (14)1.04643 (18)0.16375 (15)0.0198 (8)
C2330.04151 (16)1.13010 (19)0.15066 (16)0.0248 (10)
C234−0.03094 (17)1.1383 (2)0.11864 (16)0.0276 (10)
C235−0.07273 (15)1.0636 (2)0.09981 (16)0.0278 (10)
C236−0.04223 (13)0.97791 (19)0.11118 (15)0.0200 (8)
C2410.14687 (12)0.84220 (17)0.13787 (14)0.0146 (7)
C2420.17576 (12)0.90571 (19)0.09763 (14)0.0172 (8)
C2430.23399 (13)0.8829 (2)0.06978 (15)0.0217 (8)
C2440.26273 (12)0.7991 (2)0.08253 (15)0.0214 (8)
C2450.23370 (12)0.73475 (19)0.12204 (15)0.0202 (8)
C2460.17550 (12)0.75620 (18)0.14940 (14)0.0168 (8)
O0.24790 (10)0.42937 (14)0.69284 (13)0.0327 (7)
C1a0.27226 (14)0.36418 (19)0.66823 (16)0.0236 (9)
C2a0.34963 (14)0.3428 (2)0.69304 (18)0.0278 (10)
C3a0.22555 (17)0.3008 (2)0.6115 (2)0.0435 (13)
H1120.6229480.2721140.1062650.0195*
H1130.6940220.328940.2277370.021*
H1140.6476650.4399350.2977140.023*
H1150.5306960.4958550.2461710.0203*
H1160.4575590.437820.1257250.0161*
H1220.358870.193589−0.049360.0233*
H1230.3283520.041076−0.0330020.0294*
H1240.410536−0.052860.0551550.0294*
H1250.5204960.0044740.1302050.0277*
H1260.5523920.1562640.1148870.0228*
H1320.4674660.210873−0.1274460.0196*
H1330.5184770.23429−0.2351430.0228*
H1340.6060150.346525−0.2277540.0238*
H1350.6443390.435736−0.1123960.0208*
H1360.5917360.415883−0.0051760.0189*
H1420.3621530.3275460.0850930.0194*
H1430.2517820.4047180.0454390.0237*
H1440.2191770.478425−0.0791270.0258*
H1450.2984020.479311−0.1614510.0252*
H1460.411450.407354−0.1197180.0192*
H2120.1912880.8092080.2971390.021*
H2130.2151440.8114510.4372990.025*
H2140.1277540.8658940.4980380.0228*
H2150.0153360.9157960.4193810.0237*
H216−0.0099360.9121340.2793380.0208*
H2220.0112090.7118010.235440.0252*
H223−0.0604630.5885810.1770310.0309*
H224−0.1060360.5815190.0372830.0278*
H225−0.0798810.697556−0.0428560.0253*
H226−0.0062340.8189750.0150190.0233*
H2320.1249711.0406690.1877680.0237*
H2330.0714871.1848840.1644350.0298*
H234−0.0529521.1989840.1091790.0331*
H2420.1549640.9670660.0887840.0206*
H2430.2548680.9279880.0403730.026*
H2440.3051230.783880.0632110.0257*
H2450.254780.6735180.1305570.0242*
H2460.1539670.7102930.1773510.0202*
H235−0.125171.0701130.077870.0333*
H236−0.0723660.923370.09660.024*
H21a0.3689440.341550.6457730.0334*
H22a0.3750650.3895350.7305380.0334*
H23a0.3567010.2831690.7194250.0334*
H31a0.2401160.3000660.5611030.0522*
H32a0.2303950.239390.6346120.0522*
H33a0.1750290.3206720.6008840.0522*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.01517 (7)0.02419 (10)0.01640 (8)0.00176 (6)0.00667 (6)−0.00113 (7)
I20.02231 (7)0.01323 (9)0.01828 (8)−0.00060 (6)0.00380 (6)−0.00199 (7)
I30.02058 (7)0.02372 (11)0.01732 (8)−0.00178 (7)−0.00243 (6)−0.00117 (7)
I40.02084 (8)0.02760 (12)0.04608 (12)−0.00157 (7)0.01286 (8)0.01617 (9)
Mn0.01352 (15)0.0144 (2)0.01427 (17)−0.00100 (14)0.00358 (13)−0.00023 (15)
P10.0119 (2)0.0138 (3)0.0108 (3)0.0004 (2)0.0029 (2)−0.0005 (2)
C1110.0120 (9)0.0161 (14)0.0088 (10)−0.0011 (9)0.0026 (8)0.0011 (9)
C1120.0125 (10)0.0191 (15)0.0172 (12)0.0021 (9)0.0037 (9)0.0010 (10)
C1130.0126 (10)0.0189 (15)0.0190 (12)0.0008 (9)0.0007 (9)0.0048 (10)
C1140.0161 (10)0.0266 (16)0.0129 (11)−0.0072 (10)0.0004 (9)0.0012 (11)
C1150.0194 (11)0.0167 (14)0.0157 (12)−0.0010 (10)0.0063 (9)−0.0029 (10)
C1160.0132 (9)0.0137 (13)0.0127 (11)−0.0006 (9)0.0022 (8)0.0013 (10)
C1210.0166 (10)0.0136 (14)0.0118 (11)0.0005 (9)0.0048 (8)0.0000 (9)
C1220.0214 (12)0.0195 (15)0.0153 (12)−0.0028 (10)0.0012 (9)−0.0002 (10)
C1230.0287 (14)0.0222 (17)0.0210 (13)−0.0076 (11)0.0038 (11)−0.0017 (12)
C1240.0389 (15)0.0151 (16)0.0226 (13)−0.0028 (12)0.0135 (12)−0.0002 (11)
C1250.0277 (13)0.0193 (16)0.0234 (14)0.0053 (11)0.0087 (11)0.0062 (12)
C1260.0192 (11)0.0202 (16)0.0177 (12)0.0021 (10)0.0050 (9)0.0008 (11)
C1310.0136 (9)0.0122 (13)0.0128 (11)0.0029 (9)0.0050 (8)−0.0002 (9)
C1320.0172 (11)0.0144 (14)0.0167 (12)−0.0006 (9)0.0033 (9)−0.0041 (10)
C1330.0204 (11)0.0211 (16)0.0160 (12)0.0035 (10)0.0059 (10)−0.0043 (11)
C1340.0213 (11)0.0241 (16)0.0168 (12)0.0089 (11)0.0098 (10)0.0034 (11)
C1350.0167 (10)0.0137 (14)0.0234 (13)0.0022 (9)0.0085 (9)0.0014 (11)
C1360.0175 (11)0.0135 (14)0.0161 (11)0.0037 (10)0.0044 (9)0.0009 (10)
C1410.0136 (10)0.0126 (14)0.0131 (11)−0.0004 (9)0.0030 (8)−0.0012 (9)
C1420.0160 (10)0.0172 (15)0.0150 (12)−0.0003 (9)0.0035 (9)0.0008 (10)
C1430.0143 (10)0.0227 (16)0.0226 (13)0.0015 (10)0.0057 (9)−0.0030 (11)
C1440.0175 (11)0.0181 (15)0.0273 (14)0.0047 (10)0.0029 (10)0.0023 (12)
C1450.0218 (12)0.0179 (15)0.0215 (13)0.0025 (10)0.0022 (10)0.0079 (11)
C1460.0171 (10)0.0148 (14)0.0156 (11)−0.0008 (9)0.0035 (9)0.0012 (10)
P20.0110 (2)0.0128 (4)0.0119 (3)0.0011 (2)0.0038 (2)0.0008 (2)
C2110.0156 (10)0.0106 (13)0.0128 (11)−0.0011 (9)0.0036 (8)0.0003 (9)
C2120.0174 (11)0.0181 (15)0.0173 (12)0.0030 (10)0.0052 (9)0.0012 (10)
C2130.0204 (11)0.0220 (16)0.0167 (12)0.0005 (11)−0.0012 (9)−0.0010 (11)
C2140.0306 (13)0.0125 (14)0.0129 (11)−0.0051 (10)0.0037 (10)−0.0019 (10)
C2150.0265 (12)0.0180 (16)0.0181 (12)0.0038 (10)0.0117 (10)−0.0004 (11)
C2160.0180 (11)0.0173 (15)0.0174 (12)0.0049 (10)0.0059 (9)0.0013 (10)
C2210.0105 (9)0.0142 (14)0.0147 (11)0.0006 (9)0.0029 (8)0.0008 (10)
C2220.0282 (13)0.0188 (16)0.0152 (12)−0.0034 (11)0.0042 (10)0.0003 (11)
C2230.0355 (15)0.0211 (17)0.0208 (14)−0.0101 (12)0.0076 (11)−0.0005 (12)
C2240.0195 (12)0.0223 (17)0.0265 (14)−0.0033 (11)0.0039 (10)−0.0079 (12)
C2250.0209 (12)0.0252 (16)0.0144 (12)−0.0006 (11)0.0000 (9)−0.0038 (11)
C2260.0217 (12)0.0227 (16)0.0133 (12)−0.0031 (10)0.0038 (9)0.0027 (11)
C2310.0184 (11)0.0130 (14)0.0135 (11)0.0048 (9)0.0065 (9)0.0036 (10)
C2320.0232 (12)0.0182 (15)0.0214 (13)0.0019 (11)0.0119 (10)0.0015 (11)
C2330.0435 (16)0.0137 (16)0.0239 (14)0.0003 (12)0.0204 (12)0.0016 (12)
C2340.0486 (18)0.0181 (17)0.0209 (14)0.0179 (13)0.0176 (13)0.0087 (12)
C2350.0279 (14)0.038 (2)0.0185 (13)0.0178 (13)0.0083 (11)0.0089 (13)
C2360.0182 (11)0.0233 (16)0.0192 (12)0.0049 (10)0.0063 (9)0.0024 (11)
C2410.0115 (9)0.0174 (14)0.0140 (11)0.0002 (9)0.0017 (8)−0.0028 (10)
C2420.0169 (10)0.0201 (15)0.0144 (11)−0.0008 (10)0.0040 (9)−0.0010 (10)
C2430.0204 (11)0.0294 (17)0.0169 (12)−0.0068 (11)0.0076 (10)−0.0012 (12)
C2440.0126 (10)0.0330 (18)0.0194 (12)0.0002 (10)0.0056 (9)−0.0088 (12)
C2450.0161 (11)0.0234 (16)0.0195 (12)0.0055 (10)0.0020 (9)−0.0068 (11)
C2460.0144 (10)0.0193 (15)0.0163 (12)−0.0003 (10)0.0033 (9)−0.0016 (10)
O0.0273 (10)0.0255 (13)0.0414 (13)0.0058 (9)0.0019 (9)−0.0016 (10)
C1a0.0255 (13)0.0204 (17)0.0228 (14)−0.0001 (11)0.0027 (11)0.0040 (12)
C2a0.0274 (14)0.0204 (17)0.0352 (16)0.0002 (12)0.0072 (12)−0.0012 (13)
C3a0.0322 (17)0.043 (2)0.049 (2)−0.0037 (15)0.0009 (15)−0.0165 (18)
Geometric parameters (Å, º) top
I1—Mn2.7155 (4)P2—C2411.801 (3)
I2—Mn2.7281 (4)C211—C2121.388 (3)
I3—Mn2.6962 (4)C211—C2161.402 (4)
I4—Mn2.6868 (5)C212—C2131.388 (4)
P1—C1111.794 (2)C212—H2121.000
P1—C1211.793 (3)C213—C2141.384 (4)
P1—C1311.795 (3)C213—H2131.000
P1—C1411.796 (2)C214—C2151.393 (3)
C111—C1121.409 (3)C214—H2141.000
C111—C1161.387 (4)C215—C2161.382 (4)
C112—C1131.380 (3)C215—H2151.000
C112—H1121.000C216—H2161.000
C113—C1141.389 (4)C221—C2221.372 (4)
C113—H1131.000C221—C2261.399 (3)
C114—C1151.382 (3)C222—C2231.381 (4)
C114—H1141.000C222—H2221.000
C115—C1161.389 (3)C223—C2241.389 (4)
C115—H1151.000C223—H2231.000
C116—H1161.000C224—C2251.380 (4)
C121—C1221.394 (3)C224—H2241.000
C121—C1261.399 (3)C225—C2261.376 (4)
C122—C1231.394 (4)C225—H2251.000
C122—H1221.000C226—H2261.000
C123—C1241.381 (4)C231—C2321.393 (4)
C123—H1231.000C231—C2361.395 (3)
C124—C1251.378 (4)C232—C2331.386 (4)
C124—H1241.000C232—H2321.000
C125—C1261.389 (4)C233—C2341.384 (4)
C125—H1251.000C233—H2331.000
C126—H1261.000C234—C2351.374 (4)
C131—C1321.389 (3)C234—H2341.000
C131—C1361.395 (4)C235—C2361.406 (4)
C132—C1331.386 (4)C235—H2351.000
C132—H1321.000C236—H2361.000
C133—C1341.381 (4)C241—C2421.391 (4)
C133—H1331.000C241—C2461.397 (4)
C134—C1351.385 (4)C242—C2431.393 (4)
C134—H1341.000C242—H2421.000
C135—C1361.389 (4)C243—C2441.369 (4)
C135—H1351.000C243—H2431.000
C136—H1361.000C244—C2451.393 (4)
C141—C1421.396 (4)C244—H2441.000
C141—C1461.390 (3)C245—C2461.383 (4)
C142—C1431.383 (3)C245—H2451.000
C142—H1421.000C246—H2461.000
C143—C1441.388 (4)O—C1a1.214 (4)
C143—H1431.000C1a—C2a1.493 (4)
C144—C1451.386 (4)C1a—C3a1.502 (4)
C144—H1441.000C2a—H21a1.000
C145—C1461.391 (3)C2a—H22a1.000
C145—H1451.000C2a—H23a1.000
C146—H1461.000C3a—H31a1.000
P2—C2111.795 (2)C3a—H32a1.000
P2—C2211.788 (2)C3a—H33a1.000
P2—C2311.791 (3)
I1—Mn—I2104.011 (13)C211—P2—C241111.17 (11)
I1—Mn—I3109.957 (15)C221—P2—C231111.43 (10)
I1—Mn—I4106.881 (14)C221—P2—C241105.69 (12)
I2—Mn—I3108.490 (14)C231—P2—C241112.69 (12)
I2—Mn—I4116.164 (15)P2—C211—C212121.8 (2)
I3—Mn—I4111.014 (13)P2—C211—C216117.60 (16)
C111—P1—C121110.94 (11)C212—C211—C216120.6 (2)
C111—P1—C131108.40 (11)C211—C212—C213119.7 (2)
C111—P1—C141110.48 (11)C211—C212—H212120.1
C121—P1—C131110.90 (12)C213—C212—H212120.1
C121—P1—C141107.14 (11)C212—C213—C214120.0 (2)
C131—P1—C141108.97 (11)C212—C213—H213120.0
P1—C111—C112119.15 (19)C214—C213—H213120.0
P1—C111—C116120.78 (16)C213—C214—C215120.3 (2)
C112—C111—C116120.1 (2)C213—C214—H214119.9
C111—C112—C113119.4 (2)C215—C214—H214119.9
C111—C112—H112120.3C214—C215—C216120.3 (3)
C113—C112—H112120.3C214—C215—H215119.9
C112—C113—C114120.3 (2)C216—C215—H215119.8
C112—C113—H113119.9C211—C216—C215119.1 (2)
C114—C113—H113119.9C211—C216—H216120.4
C113—C114—C115120.3 (2)C215—C216—H216120.4
C113—C114—H114119.8P2—C221—C222121.44 (17)
C115—C114—H114119.8P2—C221—C226118.3 (2)
C114—C115—C116120.2 (2)C222—C221—C226120.0 (2)
C114—C115—H115119.9C221—C222—C223120.3 (2)
C116—C115—H115119.9C221—C222—H222119.8
C111—C116—C115119.8 (2)C223—C222—H222119.8
C111—C116—H116120.1C222—C223—C224119.8 (3)
C115—C116—H116120.1C222—C223—H223120.1
P1—C121—C122118.75 (18)C224—C223—H223120.1
P1—C121—C126121.44 (18)C223—C224—C225119.9 (2)
C122—C121—C126119.8 (2)C223—C224—H224120.0
C121—C122—C123120.2 (2)C225—C224—H224120.0
C121—C122—H122119.9C224—C225—C226120.5 (2)
C123—C122—H122119.9C224—C225—H225119.8
C122—C123—C124119.5 (2)C226—C225—H225119.8
C122—C123—H123120.2C221—C226—C225119.5 (2)
C124—C123—H123120.2C221—C226—H226120.2
C123—C124—C125120.7 (3)C225—C226—H226120.2
C123—C124—H124119.7P2—C231—C232119.37 (17)
C125—C124—H124119.7P2—C231—C236119.4 (2)
C124—C125—C126120.6 (2)C232—C231—C236120.6 (2)
C124—C125—H125119.7C231—C232—C233119.5 (2)
C126—C125—H125119.7C231—C232—H232120.3
C121—C126—C125119.3 (2)C233—C232—H232120.3
C121—C126—H126120.4C232—C233—C234120.4 (3)
C125—C126—H126120.4C232—C233—H233119.8
P1—C131—C132118.90 (19)C234—C233—H233119.8
P1—C131—C136120.31 (19)C233—C234—C235120.3 (3)
C132—C131—C136120.4 (2)C233—C234—H234119.8
C131—C132—C133119.5 (2)C235—C234—H234119.8
C131—C132—H132120.3C234—C235—C236120.4 (3)
C133—C132—H132120.3C234—C235—H235119.8
C132—C133—C134120.4 (2)C236—C235—H235119.8
C132—C133—H133119.8C231—C236—C235118.8 (2)
C134—C133—H133119.8C231—C236—H236120.6
C133—C134—C135120.3 (3)C235—C236—H236120.6
C133—C134—H134119.8P2—C241—C242122.85 (19)
C135—C134—H134119.8P2—C241—C246116.8 (2)
C134—C135—C136120.0 (2)C242—C241—C246120.3 (2)
C134—C135—H135120.0C241—C242—C243119.3 (2)
C136—C135—H135120.0C241—C242—H242120.4
C131—C136—C135119.4 (2)C243—C242—H242120.4
C131—C136—H136120.3C242—C243—C244120.2 (3)
C135—C136—H136120.3C242—C243—H243119.9
P1—C141—C142119.28 (18)C244—C243—H243119.9
P1—C141—C146120.7 (2)C243—C244—C245120.9 (3)
C142—C141—C146119.9 (2)C243—C244—H244119.6
C141—C142—C143120.3 (2)C245—C244—H244119.6
C141—C142—H142119.8C244—C245—C246119.5 (3)
C143—C142—H142119.8C244—C245—H245120.3
C142—C143—C144119.7 (3)C246—C245—H245120.3
C142—C143—H143120.2C241—C246—C245119.8 (3)
C144—C143—H143120.2C241—C246—H246120.1
C143—C144—C145120.2 (2)C245—C246—H246120.1
C143—C144—H144119.9O—C1a—C2a121.9 (2)
C145—C144—H144119.9O—C1a—C3a121.3 (3)
C144—C145—C146120.4 (2)C2a—C1a—C3a116.8 (3)
C144—C145—H145119.8H21a—C2a—H22a109.5
C146—C145—H145119.8H21a—C2a—H23a109.5
C141—C146—C145119.4 (2)H22a—C2a—H23a109.5
C141—C146—H146120.3H31a—C3a—H32a109.5
C145—C146—H146120.3H31a—C3a—H33a109.5
C211—P2—C221110.29 (12)H32a—C3a—H33a109.5
C211—P2—C231105.66 (12)

Experimental details

Crystal data
Chemical formula(C24H20P)2[MnI4]·C3H6O
Mr1299.4
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)19.5230 (4), 14.9733 (3), 17.6152 (4)
β (°) 105.161 (2)
V (Å3)4970.12 (19)
Z4
Radiation typeMo Kα
µ (mm−1)2.85
Crystal size (mm)0.47 × 0.40 × 0.38
Data collection
DiffractometerOxford Diffraction Xcalibur3 with Sapphire-3 CCD detector
diffractometer
Absorption correctionGaussian
(CrysAlis RED; Oxford Diffraction, 2008)
Tmin, Tmax0.388, 0.480
No. of measured, independent and
observed [I > 3σ(I)] reflections		181649, 20267, 12474
Rint0.055
(sin θ/λ)max (Å−1)0.799
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.062, 1.17
No. of reflections20267
No. of parameters533
No. of restraints?
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)2.03, −1.59

Computer programs: CrysAlis CCD (Oxford Diffraction, 2008), CrysAlis RED (Oxford Diffraction, 2008), Superflip (Oszlányi & Sütő, 2004), JANA2000 (Petříček & Dušek, 2000), DIAMOND (Brandenburg, 1999).

 

Acknowledgements

Financial support from the Swedish Research Council is gratefully acknowledged.

References

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ISSN: 2056-9890
Volume 66| Part 3| March 2010| Page m338
doi:10.1107/S1600536810006732
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