research papers
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 [Pmm, 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, 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
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768102001970/sn0020sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768102001970/sn0020Isup2.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768102001970/sn0020Isup3.hkl |
CCDC reference: 188248
(I) top
Crystal data top
Triclinic, P1 | β = 116.776 (2)° |
a = 13.6414 (8) Å | γ = 119.3326 (19)° |
b = 13.8338 (7) Å | Synchrotron radiation |
c = 13.8548 (7) Å | T = 235 K |
α = 91.830 (3)° |
Refinement top
Rp = 0.077 | 15 parameters |
Rwp = 0.105 | 0 restraints |
Rexp = 0.122 | (Δ/σ)max = 0.06 |
7665 data points |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
C1 | −0.030 (2) | 0.0227 (14) | −0.1262 (17) | 0.0284 (19)* | |
C2 | 0.045 (2) | 0.4640 (14) | −0.3896 (17) | 0.0284 (19)* | |
C3 | 0.1120 (19) | 0.1109 (17) | −0.0549 (16) | 0.0284 (19)* | |
C4 | −0.0972 (19) | 0.3757 (17) | −0.4609 (15) | 0.0284 (19)* | |
C5 | 0.1922 (18) | 0.1324 (18) | −0.0986 (18) | 0.0284 (19)* | |
C6 | −0.1774 (18) | 0.3543 (18) | −0.4172 (18) | 0.0284 (19)* | |
C7 | −0.087 (2) | −0.0403 (10) | −0.2381 (19) | 0.0284 (19)* | |
C8 | 0.102 (2) | 0.5270 (10) | −0.2777 (19) | 0.0284 (19)* | |
C9 | −0.003 (2) | −0.0179 (11) | −0.284 (2) | 0.0284 (19)* | |
C10 | 0.018 (2) | 0.5046 (11) | −0.232 (2) | 0.0284 (19)* | |
C11 | −0.0970 (19) | 0.0654 (16) | −0.1002 (15) | 0.0284 (19)* | |
C12 | 0.1119 (19) | 0.4213 (16) | −0.4156 (16) | 0.0284 (19)* | |
C13 | −0.2121 (17) | −0.0634 (7) | −0.3289 (18) | 0.0284 (19)* | |
C14 | 0.2269 (17) | 0.5501 (7) | −0.1869 (18) | 0.0284 (19)* | |
C15 | 0.133 (2) | 0.0666 (16) | −0.215 (2) | 0.0284 (19)* | |
C16 | −0.119 (2) | 0.4200 (16) | −0.301 (2) | 0.0284 (19)* | |
C17 | −0.2172 (16) | 0.0433 (15) | −0.1873 (17) | 0.0284 (19)* | |
C18 | 0.2320 (16) | 0.4434 (15) | −0.3285 (17) | 0.0284 (19)* | |
C19 | −0.2760 (14) | −0.0225 (11) | −0.3040 (17) | 0.0284 (19)* | |
C20 | 0.2908 (14) | 0.5092 (11) | −0.2118 (18) | 0.0284 (19)* | |
C21 | 0.3034 (14) | 0.2602 (19) | −0.176 (2) | 0.0284 (19)* | |
C22 | −0.2886 (14) | 0.2265 (19) | −0.3401 (19) | 0.0284 (19)* | |
C23 | 0.2972 (13) | 0.2520 (19) | −0.0741 (17) | 0.0284 (19)* | |
C24 | −0.2824 (13) | 0.2346 (19) | −0.4417 (17) | 0.0284 (19)* | |
C25 | 0.3177 (12) | 0.3452 (18) | −0.0070 (13) | 0.0284 (19)* | |
C26 | −0.3029 (12) | 0.1415 (18) | −0.5088 (12) | 0.0284 (19)* | |
C27 | 0.3298 (11) | 0.3612 (17) | −0.2061 (19) | 0.0284 (19)* | |
C28 | −0.3150 (11) | 0.1255 (17) | −0.3097 (18) | 0.0284 (19)* | |
C29 | 0.3512 (9) | 0.4584 (14) | −0.1361 (17) | 0.0284 (19)* | |
C30 | −0.3364 (9) | 0.0283 (14) | −0.3797 (16) | 0.0284 (19)* | |
C31 | 0.2022 (19) | 0.1456 (18) | −0.263 (2) | 0.0284 (19)* | |
C32 | −0.1874 (19) | 0.3411 (18) | −0.253 (2) | 0.0284 (19)* | |
C33 | 0.2562 (16) | 0.3519 (17) | −0.3250 (18) | 0.0284 (19)* | |
C34 | −0.2413 (16) | 0.1347 (17) | −0.1908 (18) | 0.0284 (19)* | |
C35 | 0.3453 (10) | 0.4506 (15) | −0.0387 (13) | 0.0284 (19)* | |
C36 | −0.3305 (10) | 0.0361 (15) | −0.4771 (13) | 0.0284 (19)* | |
C37 | 0.132 (2) | 0.1368 (18) | −0.3770 (19) | 0.0284 (19)* | |
C38 | −0.117 (2) | 0.3499 (17) | −0.1388 (19) | 0.0284 (19)* | |
C39 | 0.159 (2) | 0.2421 (19) | −0.4087 (17) | 0.0284 (19)* | |
C40 | −0.144 (2) | 0.2446 (18) | −0.1071 (17) | 0.0284 (19)* | |
C41 | 0.2100 (18) | 0.4143 (16) | 0.0350 (8) | 0.0284 (19)* | |
C42 | −0.1951 (19) | 0.0724 (16) | −0.5508 (8) | 0.0284 (19)* | |
C43 | 0.2341 (17) | 0.3228 (18) | 0.0385 (8) | 0.0284 (19)* | |
C44 | −0.2193 (17) | 0.1639 (18) | −0.5543 (8) | 0.0284 (19)* | |
C45 | 0.1334 (19) | 0.2081 (19) | 0.0150 (10) | 0.0284 (19)* | |
C46 | −0.1186 (19) | 0.2786 (19) | −0.5308 (10) | 0.0284 (19)* | |
C47 | 0.086 (2) | 0.3873 (17) | 0.0081 (11) | 0.0284 (19)* | |
C48 | −0.071 (2) | 0.0994 (17) | −0.5239 (12) | 0.0284 (19)* | |
C49 | −0.019 (2) | 0.2677 (19) | −0.0163 (12) | 0.0284 (19)* | |
C50 | 0.034 (2) | 0.2190 (19) | −0.4995 (13) | 0.0284 (19)* | |
C51 | 0.2787 (16) | 0.4932 (12) | −0.0127 (12) | 0.0284 (19)* | |
C52 | −0.2639 (16) | −0.0066 (12) | −0.5031 (12) | 0.0284 (19)* | |
C53 | 0.026 (2) | 0.4381 (15) | −0.0676 (17) | 0.0284 (19)* | |
C54 | −0.012 (2) | 0.0321 (16) | −0.4643 (18) | 0.0284 (19)* | |
C55 | 0.004 (2) | 0.1800 (18) | −0.0130 (12) | 0.0284 (19)* | |
C56 | 0.011 (2) | 0.3067 (18) | −0.5028 (12) | 0.0284 (19)* | |
C57 | 0.2208 (18) | 0.5420 (8) | −0.0853 (16) | 0.0284 (19)* | |
C58 | −0.2059 (18) | −0.0553 (8) | −0.4305 (16) | 0.0284 (19)* | |
C59 | 0.092 (2) | 0.5138 (11) | −0.1133 (18) | 0.0284 (19)* | |
C60 | −0.077 (2) | −0.0271 (11) | −0.4025 (18) | 0.0284 (19)* | |
CR61 | 0.5 | 0.0 | 0.0 | 0.156 (4)* | |
C62 | 0.371 (2) | −0.1448 (16) | 0.022 (3) | 0.156 (4)* | |
C63 | 0.495 (3) | −0.074 (3) | 0.127 (2) | 0.156 (4)* | |
C64 | 0.555 (3) | 0.049 (3) | 0.1681 (8) | 0.156 (4)* | |
C65 | 0.489 (3) | 0.100 (2) | 0.104 (3) | 0.156 (4)* | |
C66 | 0.364 (2) | 0.0283 (18) | −0.001 (3) | 0.156 (4)* | |
C67 | 0.3050 (9) | −0.0939 (16) | −0.042 (2) | 0.156 (4)* | |
H68 | 0.326 (3) | −0.2374 (15) | −0.010 (5) | 0.156 (4)* | |
H69 | 0.545 (4) | −0.112 (5) | 0.175 (4) | 0.156 (4)* | |
H70 | 0.649 (3) | 0.103 (5) | 0.2477 (6) | 0.156 (4)* | |
H71 | 0.534 (4) | 0.192 (2) | 0.136 (5) | 0.156 (4)* | |
H72 | 0.315 (3) | 0.067 (3) | −0.049 (5) | 0.156 (4)* | |
C73 | 0.17349 (12) | −0.169 (3) | −0.153 (3) | 0.156 (4)* | |
CR74 | 0.5 | 0.5 | 0.5 | 0.156 (4)* | |
C75 | 0.3042 (6) | 0.4371 (19) | 0.3806 (18) | 0.156 (4)* | |
C76 | 0.3221 (18) | 0.437 (3) | 0.490 (3) | 0.156 (4)* | |
C77 | 0.427 (3) | 0.539 (4) | 0.5865 (19) | 0.156 (4)* | |
C78 | 0.514 (3) | 0.642 (2) | 0.5740 (15) | 0.156 (4)* | |
C79 | 0.497 (2) | 0.6428 (11) | 0.4647 (18) | 0.156 (4)* | |
C80 | 0.3915 (16) | 0.5402 (16) | 0.3681 (11) | 0.156 (4)* | |
H81 | 0.2246 (14) | 0.359 (2) | 0.307 (2) | 0.156 (4)* | |
H82 | 0.256 (2) | 0.358 (4) | 0.499 (4) | 0.156 (4)* | |
H83 | 0.441 (5) | 0.539 (5) | 0.669 (2) | 0.156 (4)* | |
H84 | 0.594 (5) | 0.720 (3) | 0.647 (2) | 0.156 (4)* | |
H85 | 0.563 (3) | 0.7210 (13) | 0.455 (3) | 0.156 (4)* | |
C86 | 0.373 (3) | 0.541 (3) | 0.2530 (14) | 0.156 (4)* |