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Bis(toluene)chromium fulleride, [Cr(C7H8)2]C60, has been synthesized as a black microcrystalline powder from C60 and [Cr(C7H8)2] in toluene. [Cr(C7H8)2]C60 is an ionic compound in which the fullerene is negatively charged and the bis(toluene)chromium molecule positively charged. At T = 250 K a reversible first-order phase transition from a primitive cubic high-temperature phase to a triclinic low-temperature phase occurs. The high-temperature phase [Pm\overline 3m, a = 9.9840 (1) Å, T = 295 K] is composed of dynamically disordered fulleride anions and bis(toluene)chromium(I) cations in a CsCl-type arrangement. The triclinic low-temperature modification [P\overline 1, a = 13.6414 (8), b = 13.8338 (7), c = 13.8548 (7) Å, α = 91.830 (3), β = 116.776 (2), γ = 119.333 (2)°, T = 235 K] consists of ordered C60 dimers and two crystallographically distinct bis(toluene)chromium entities.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768102001970/sn0020sup1.cif
Contains datablock I

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768102001970/sn0020Isup2.rtv
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768102001970/sn0020Isup3.hkl
Contains datablock I

CCDC reference: 188248

Computing details top

Program(s) used to refine structure: GSAS.

(I) top
Crystal data top
Triclinic, P1β = 116.776 (2)°
a = 13.6414 (8) Åγ = 119.3326 (19)°
b = 13.8338 (7) ÅSynchrotron radiation
c = 13.8548 (7) ÅT = 235 K
α = 91.830 (3)°
Data collection top
2θmin = 3.003°, 2θmax = 25.995°, 2θstep = 0.003°
Refinement top
Rp = 0.07715 parameters
Rwp = 0.1050 restraints
Rexp = 0.122(Δ/σ)max = 0.06
7665 data points
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.030 (2)0.0227 (14)0.1262 (17)0.0284 (19)*
C20.045 (2)0.4640 (14)0.3896 (17)0.0284 (19)*
C30.1120 (19)0.1109 (17)0.0549 (16)0.0284 (19)*
C40.0972 (19)0.3757 (17)0.4609 (15)0.0284 (19)*
C50.1922 (18)0.1324 (18)0.0986 (18)0.0284 (19)*
C60.1774 (18)0.3543 (18)0.4172 (18)0.0284 (19)*
C70.087 (2)0.0403 (10)0.2381 (19)0.0284 (19)*
C80.102 (2)0.5270 (10)0.2777 (19)0.0284 (19)*
C90.003 (2)0.0179 (11)0.284 (2)0.0284 (19)*
C100.018 (2)0.5046 (11)0.232 (2)0.0284 (19)*
C110.0970 (19)0.0654 (16)0.1002 (15)0.0284 (19)*
C120.1119 (19)0.4213 (16)0.4156 (16)0.0284 (19)*
C130.2121 (17)0.0634 (7)0.3289 (18)0.0284 (19)*
C140.2269 (17)0.5501 (7)0.1869 (18)0.0284 (19)*
C150.133 (2)0.0666 (16)0.215 (2)0.0284 (19)*
C160.119 (2)0.4200 (16)0.301 (2)0.0284 (19)*
C170.2172 (16)0.0433 (15)0.1873 (17)0.0284 (19)*
C180.2320 (16)0.4434 (15)0.3285 (17)0.0284 (19)*
C190.2760 (14)0.0225 (11)0.3040 (17)0.0284 (19)*
C200.2908 (14)0.5092 (11)0.2118 (18)0.0284 (19)*
C210.3034 (14)0.2602 (19)0.176 (2)0.0284 (19)*
C220.2886 (14)0.2265 (19)0.3401 (19)0.0284 (19)*
C230.2972 (13)0.2520 (19)0.0741 (17)0.0284 (19)*
C240.2824 (13)0.2346 (19)0.4417 (17)0.0284 (19)*
C250.3177 (12)0.3452 (18)0.0070 (13)0.0284 (19)*
C260.3029 (12)0.1415 (18)0.5088 (12)0.0284 (19)*
C270.3298 (11)0.3612 (17)0.2061 (19)0.0284 (19)*
C280.3150 (11)0.1255 (17)0.3097 (18)0.0284 (19)*
C290.3512 (9)0.4584 (14)0.1361 (17)0.0284 (19)*
C300.3364 (9)0.0283 (14)0.3797 (16)0.0284 (19)*
C310.2022 (19)0.1456 (18)0.263 (2)0.0284 (19)*
C320.1874 (19)0.3411 (18)0.253 (2)0.0284 (19)*
C330.2562 (16)0.3519 (17)0.3250 (18)0.0284 (19)*
C340.2413 (16)0.1347 (17)0.1908 (18)0.0284 (19)*
C350.3453 (10)0.4506 (15)0.0387 (13)0.0284 (19)*
C360.3305 (10)0.0361 (15)0.4771 (13)0.0284 (19)*
C370.132 (2)0.1368 (18)0.3770 (19)0.0284 (19)*
C380.117 (2)0.3499 (17)0.1388 (19)0.0284 (19)*
C390.159 (2)0.2421 (19)0.4087 (17)0.0284 (19)*
C400.144 (2)0.2446 (18)0.1071 (17)0.0284 (19)*
C410.2100 (18)0.4143 (16)0.0350 (8)0.0284 (19)*
C420.1951 (19)0.0724 (16)0.5508 (8)0.0284 (19)*
C430.2341 (17)0.3228 (18)0.0385 (8)0.0284 (19)*
C440.2193 (17)0.1639 (18)0.5543 (8)0.0284 (19)*
C450.1334 (19)0.2081 (19)0.0150 (10)0.0284 (19)*
C460.1186 (19)0.2786 (19)0.5308 (10)0.0284 (19)*
C470.086 (2)0.3873 (17)0.0081 (11)0.0284 (19)*
C480.071 (2)0.0994 (17)0.5239 (12)0.0284 (19)*
C490.019 (2)0.2677 (19)0.0163 (12)0.0284 (19)*
C500.034 (2)0.2190 (19)0.4995 (13)0.0284 (19)*
C510.2787 (16)0.4932 (12)0.0127 (12)0.0284 (19)*
C520.2639 (16)0.0066 (12)0.5031 (12)0.0284 (19)*
C530.026 (2)0.4381 (15)0.0676 (17)0.0284 (19)*
C540.012 (2)0.0321 (16)0.4643 (18)0.0284 (19)*
C550.004 (2)0.1800 (18)0.0130 (12)0.0284 (19)*
C560.011 (2)0.3067 (18)0.5028 (12)0.0284 (19)*
C570.2208 (18)0.5420 (8)0.0853 (16)0.0284 (19)*
C580.2059 (18)0.0553 (8)0.4305 (16)0.0284 (19)*
C590.092 (2)0.5138 (11)0.1133 (18)0.0284 (19)*
C600.077 (2)0.0271 (11)0.4025 (18)0.0284 (19)*
CR610.50.00.00.156 (4)*
C620.371 (2)0.1448 (16)0.022 (3)0.156 (4)*
C630.495 (3)0.074 (3)0.127 (2)0.156 (4)*
C640.555 (3)0.049 (3)0.1681 (8)0.156 (4)*
C650.489 (3)0.100 (2)0.104 (3)0.156 (4)*
C660.364 (2)0.0283 (18)0.001 (3)0.156 (4)*
C670.3050 (9)0.0939 (16)0.042 (2)0.156 (4)*
H680.326 (3)0.2374 (15)0.010 (5)0.156 (4)*
H690.545 (4)0.112 (5)0.175 (4)0.156 (4)*
H700.649 (3)0.103 (5)0.2477 (6)0.156 (4)*
H710.534 (4)0.192 (2)0.136 (5)0.156 (4)*
H720.315 (3)0.067 (3)0.049 (5)0.156 (4)*
C730.17349 (12)0.169 (3)0.153 (3)0.156 (4)*
CR740.50.50.50.156 (4)*
C750.3042 (6)0.4371 (19)0.3806 (18)0.156 (4)*
C760.3221 (18)0.437 (3)0.490 (3)0.156 (4)*
C770.427 (3)0.539 (4)0.5865 (19)0.156 (4)*
C780.514 (3)0.642 (2)0.5740 (15)0.156 (4)*
C790.497 (2)0.6428 (11)0.4647 (18)0.156 (4)*
C800.3915 (16)0.5402 (16)0.3681 (11)0.156 (4)*
H810.2246 (14)0.359 (2)0.307 (2)0.156 (4)*
H820.256 (2)0.358 (4)0.499 (4)0.156 (4)*
H830.441 (5)0.539 (5)0.669 (2)0.156 (4)*
H840.594 (5)0.720 (3)0.647 (2)0.156 (4)*
H850.563 (3)0.7210 (13)0.455 (3)0.156 (4)*
C860.373 (3)0.541 (3)0.2530 (14)0.156 (4)*
 

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