An algorithm for determining the element-selective charge density has been developed using the maximum entropy method (MEM), Rietveld analysis and synchrotron X-ray multi-wavelength anomalous powder diffraction data. This article describes in detail both experimental and analytical aspects of the developed method. A structural study of yttrium mono-metallofullerene, Y@C82, 1:1 co-crystallized with toluene using the present technique is reported in order to demonstrate the applicability of the method even when only medium resolution data are available (d > 1.32 Å). Element-selective MEM charge density maps, computed from synchrotron X-ray powder diffraction data collected at three distinct wavelengths around the yttrium K-absorption edge (∼0.727 A), are employed for determining three crystallographic sites of the disordered yttrium.
Supporting information
Cell refinement: SP (Nishibori et al., 2007); program(s) used to solve structure: GAIA (Nishibori et al., 2007); program(s) used to refine structure: SP (Nishibori et al., 2007); molecular graphics: pyMOL (DeLano, 2002).
Endohedral metallofullerene
top
Crystal data top
YC82·C7H8 | Z = 1 |
Mr = 4663.79 | F(000) = 2324 |
Orthorhombic, Cmc21 | Dx = 1.063 Mg m−3 |
Hall symbol: C 2c -2 | Synchrotron radiation, λ = 0.73330 Å |
a = 11.22205 (6) Å | µ = 0.33 mm−1 |
b = 34.8174 (2) Å | T = 300 K |
c = 11.22569 (7) Å | black |
V = 4386.13 (7) Å3 | cylinder, 3 × 0.4 mm |
Data collection top
Large Debye-Scherrer camera diffractometer | Data collection mode: transmission |
Radiation source: synchrotron, SPring-8 BL02B2 | Scan method: step |
Si(111) monochromator | 2θmin = 3.00°, 2θmax = 32.50°, 2θstep = 0.010° |
Specimen mounting: capillary | |
Refinement top
Refinement on Inet | Profile function: pseudo-Voigt |
Least-squares matrix: full | 272 parameters |
Rp = 0.044 | 348 restraints |
Rwp = 0.015 | 0 constraints |
Rexp = ? | H atoms treated by a mixture of independent and constrained refinement |
χ2 = ? | Weighting scheme based on measured s.u.'s |
7508 data points | |
Excluded region(s): none | Background function: split Pearson VII |
Crystal data top
YC82·C7H8 | V = 4386.13 (7) Å3 |
Mr = 4663.79 | Z = 1 |
Orthorhombic, Cmc21 | Synchrotron radiation, λ = 0.73330 Å |
a = 11.22205 (6) Å | µ = 0.33 mm−1 |
b = 34.8174 (2) Å | T = 300 K |
c = 11.22569 (7) Å | cylinder, 3 × 0.4 mm |
Data collection top
Large Debye-Scherrer camera diffractometer | Scan method: step |
Specimen mounting: capillary | 2θmin = 3.00°, 2θmax = 32.50°, 2θstep = 0.010° |
Data collection mode: transmission | |
Refinement top
Rp = 0.044 | 7508 data points |
Rwp = 0.015 | 272 parameters |
Rexp = ? | 348 restraints |
χ2 = ? | H atoms treated by a mixture of independent and constrained refinement |
Special details top
Refinement. Rigid-body refinement. The carbon atoms on fullerene molecules and encapsulated
Y have rotational displacement,they are approximated by mixuture of a
spherical shell model and atoms for reduction of parameters·A center of
spherical shell are listed as YSP, CSP. The maximum deviations of carbon bond
distances and bond angles from theoretically predicted hollow C82 are less
than 0.03 A and 0.2 degree in the restraint Rietveld refinement. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
CSP | 0.00000 | 0.13787 (3) | 0.2545 (12) | 0.0189* | |
YSP | 0.00000 | 0.1118 (8) | 0.43053 (3) | 0.0669* | 0.82092 |
Y1 | 0.11559 | 0.104 (4) | 0.3698 (7) | 0.3134 | 0.04477 |
Y2 | 0.11559 | 0.1316 (8) | 0.4088 (7) | 0.3134 | 0.04477 |
C1 | 0.2211 (3) | 0.16117 (8) | −0.0436 (2) | 0.2377 | 0.50000 |
C2 | 0.2182 (3) | 0.19620 (8) | 0.0059 (2) | 0.2364 | 0.50000 |
C3 | 0.2171 (2) | 0.04280 (6) | 0.2450 (2) | 0.2263 | 0.50000 |
C4 | 0.2155 (3) | 0.20464 (6) | 0.4739 (3) | 0.2300 | 0.50000 |
C5 | 0.2124 (1) | 0.04996 (6) | 0.3675 (2) | 0.2235 | 0.50000 |
C6 | 0.2132 (3) | 0.17079 (8) | 0.5373 (3) | 0.2274 | 0.50000 |
C7 | 0.2822 (2) | 0.08112 (8) | 0.4112 (2) | 0.2266 | 0.50000 |
C8 | 0.2825 (2) | 0.14064 (13) | 0.4936 (2) | 0.2291 | 0.50000 |
C9 | 0.2225 (3) | 0.09648 (9) | −0.0195 (3) | 0.2353 | 0.50000 |
C10 | 0.2180 (2) | 0.23356 (8) | 0.1731 (2) | 0.2360 | 0.50000 |
C11 | 0.2214 (3) | 0.06558 (6) | 0.0547 (3) | 0.2333 | 0.50000 |
C12 | 0.2173 (2) | 0.23644 (8) | 0.2907 (2) | 0.2359 | 0.50000 |
C13 | 0.2806 (2) | 0.06710 (7) | 0.1665 (2) | 0.2269 | 0.50000 |
C14 | 0.2797 (2) | 0.20790 (7) | 0.3637 (2) | 0.2300 | 0.50000 |
C15 | 0.3358 (2) | 0.10248 (11) | 0.2081 (3) | 0.2168 | 0.50000 |
C16 | 0.3339 (2) | 0.17619 (12) | 0.3117 (3) | 0.2192 | 0.50000 |
C17 | 0.3424 (2) | 0.10709 (11) | 0.3294 (3) | 0.2228 | 0.50000 |
C18 | 0.3417 (2) | 0.14372 (14) | 0.3811 (3) | 0.2242 | 0.50000 |
C19 | 0.2444 (1) | 0.10157 (7) | 0.5102 (2) | 0.2299 | 0.50000 |
C20 | 0.2823 (2) | 0.13090 (11) | 0.0158 (3) | 0.2302 | 0.50000 |
C21 | 0.2799 (2) | 0.20274 (10) | 0.1177 (2) | 0.2305 | 0.50000 |
C22 | 0.3322 (2) | 0.13531 (12) | 0.1330 (3) | 0.2148 | 0.50000 |
C23 | 0.3310 (2) | 0.17248 (12) | 0.1847 (4) | 0.2156 | 0.50000 |
C24 | 0.1108 (3) | 0.02784 (6) | 0.1819 (2) | 0.2353 | 0.50000 |
C25 | 0.0000 | 0.02131 (5) | 0.24493 (7) | 0.2313 | 0.25000 |
C26 | 0.0000 | 0.02592 (4) | 0.37120 (8) | 0.2358 | 0.25000 |
C27 | 0.1034 (1) | 0.03971 (6) | 0.4313 (1) | 0.2363 | 0.50000 |
C28 | 0.1311 (1) | 0.09271 (5) | 0.5686 (2) | 0.2360 | 0.50000 |
C29 | 0.0650 (1) | 0.06056 (2) | 0.5285 (1) | 0.2385 | 0.50000 |
C30 | 0.0654 (1) | 0.12277 (2) | 0.6181 (1) | 0.2400 | 0.50000 |
C31 | 0.1074 (3) | 0.22903 (7) | 0.4669 (2) | 0.1717 | 0.50000 |
C32 | 0.0000 | 0.21867 (12) | 0.5224 (2) | 0.1693 | 0.25000 |
C33 | 0.0000 | 0.18512 (6) | 0.5968 (13) | 0.1722 | 0.25000 |
C34 | 0.1106 (3) | 0.04255 (7) | 0.0681 (2) | 0.1705 | 0.50000 |
C35 | 0.1070 (2) | 0.24795 (8) | 0.3527 (2) | 0.1723 | 0.50000 |
C36 | 0.0000 | 0.05260 (4) | 0.0086 (1) | 0.1669 | 0.25000 |
C37 | 0.0000 | 0.25428 (13) | 0.2902 (2) | 0.1677 | 0.25000 |
C38 | 0.1048 (1) | 0.16142 (7) | 0.6050 (3) | 0.1725 | 0.50000 |
C39 | 0.1129 (3) | 0.10678 (7) | −0.0880 (2) | 0.1737 | 0.50000 |
C40 | 0.1075 (2) | 0.24190 (8) | 0.1044 (2) | 0.1721 | 0.50000 |
C41 | 0.0000 | 0.08540 (3) | −0.0711 (1) | 0.1681 | 0.25000 |
C42 | 0.0000 | 0.25148 (5) | 0.1621 (1) | 0.1676 | 0.25000 |
C43 | 0.1127 (3) | 0.14593 (7) | −0.1036 (2) | 0.1756 | 0.50000 |
C44 | 0.1079 (2) | 0.21831 (12) | 0.0030 (2) | 0.1713 | 0.50000 |
C45 | 0.0000 | 0.16767 (2) | −0.1034 (3) | 0.1695 | 0.25000 |
C46 | 0.0000 | 0.2068 (3) | −0.0513 (6) | 0.1679 | 0.25000 |
C52 | 0.50000 | 0.071 (5) | 0.862 (9) | 0.1512* | 0.60000 |
C53 | 0.50000 | 0.033 (4) | 0.868 (9) | 0.1512* | 0.60000 |
C54 | 0.50000 | 0.0106 (4) | 0.762 (10) | 0.1512* | |
C55 | 0.50000 | 0.028 (4) | 0.653 (10) | 0.1512* | 0.60000 |
C56 | 0.50000 | 0.066 (5) | 0.647 (9) | 0.1512* | 0.60000 |
C57 | 0.50000 | 0.0885 (5) | 0.754 (15) | 0.1512* | |
C58 | 0.50000 | 0.1281 (4) | 0.747 (6) | 0.1512* | |
H9 | 0.50000 | 0.088 (5) | 0.945 (9) | 0.1512* | 0.60000 |
H10 | 0.50000 | 0.019 (4) | 0.957 (9) | 0.1512* | 0.60000 |
H11 | 0.50000 | −0.0214 (4) | 0.768 (10) | 0.1512* | |
H12 | 0.50000 | 0.011 (4) | 0.570 (10) | 0.1512* | 0.60000 |
H13 | 0.50000 | 0.081 (5) | 0.558 (9) | 0.1512* | 0.60000 |
H14 | 0.42 (1) | 0.1394 (4) | 0.791 (6) | 0.1512* | 0.30000 |
H15 | 0.50000 | 0.1369 (4) | 0.654 (6) | 0.1512* | 0.60000 |
H16 | 0.58 (1) | 0.1394 (4) | 0.791 (6) | 0.1512* | 0.30000 |
C67 | 0.392 (4) | 0.0685 (12) | 0.76 (2) | 0.1512* | 0.40000 |
C68 | 0.392 (4) | 0.0306 (12) | 0.758 (14) | 0.1512* | 0.40000 |
H24 | 0.306 (4) | 0.0845 (12) | 0.75 (2) | 0.1512* | 0.40000 |
H25 | 0.306 (4) | 0.0146 (12) | 0.761 (14) | 0.1512* | 0.40000 |
H29 | 0.45 (1) | 0.1371 (4) | 0.666 (6) | 0.1512* | 0.20000 |
H30 | 0.59 (1) | 0.1385 (4) | 0.745 (6) | 0.1512* | 0.20000 |
H31 | 0.45 (1) | 0.1400 (4) | 0.825 (6) | 0.1512* | 0.20000 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.3083 | 0.3233 | 0.3086 | 0.0735 | −0.0812 | 0.0734 |
Y2 | 0.3083 | 0.3874 | 0.2446 | 0.0137 | −0.1087 | 0.0183 |
C1 | 0.2341 | 0.3220 | 0.1571 | −0.0320 | 0.1313 | 0.0428 |
C2 | 0.2345 | 0.2668 | 0.2079 | −0.0782 | 0.1085 | 0.0883 |
C3 | 0.2212 | 0.1426 | 0.3152 | 0.1276 | 0.0039 | −0.0053 |
C4 | 0.2268 | 0.2370 | 0.2261 | −0.0888 | −0.0944 | −0.0891 |
C5 | 0.2205 | 0.1630 | 0.2870 | 0.1158 | −0.0467 | 0.0597 |
C6 | 0.2254 | 0.2970 | 0.1599 | −0.0428 | −0.1199 | −0.0561 |
C7 | 0.1566 | 0.2542 | 0.2692 | 0.0991 | −0.0862 | 0.0536 |
C8 | 0.1617 | 0.3193 | 0.2063 | −0.0055 | −0.1337 | −0.0046 |
C9 | 0.2310 | 0.2956 | 0.1792 | 0.0570 | 0.1209 | −0.0705 |
C10 | 0.2352 | 0.1562 | 0.3167 | −0.1283 | 0.0353 | 0.0479 |
C11 | 0.2284 | 0.2259 | 0.2455 | 0.0986 | 0.0884 | −0.0895 |
C12 | 0.2352 | 0.1454 | 0.3272 | −0.1320 | −0.0155 | −0.0216 |
C13 | 0.1592 | 0.2208 | 0.3007 | 0.1224 | 0.0493 | −0.0384 |
C14 | 0.1640 | 0.2287 | 0.2973 | −0.1202 | −0.0608 | −0.0466 |
C15 | 0.0762 | 0.2774 | 0.2967 | 0.0729 | 0.0312 | −0.0101 |
C16 | 0.0817 | 0.2775 | 0.2983 | −0.0777 | −0.0375 | −0.0131 |
C17 | 0.0762 | 0.2921 | 0.3002 | 0.0649 | −0.0482 | 0.0134 |
C18 | 0.0791 | 0.3114 | 0.2821 | −0.0134 | −0.0838 | −0.0048 |
C19 | 0.2022 | 0.2964 | 0.1911 | 0.0536 | −0.1239 | 0.0561 |
C20 | 0.1621 | 0.3204 | 0.2082 | 0.0114 | 0.1341 | −0.0096 |
C21 | 0.1647 | 0.2429 | 0.2837 | −0.1110 | 0.0770 | 0.0545 |
C22 | 0.0780 | 0.2979 | 0.2684 | 0.0044 | 0.0807 | −0.0016 |
C23 | 0.0806 | 0.2771 | 0.2891 | −0.0695 | 0.0472 | 0.0150 |
C24 | 0.3015 | 0.0890 | 0.3154 | 0.0762 | 0.0161 | −0.0501 |
C25 | 0.3200 | 0.0540 | 0.3198 | 0.0000 | 0.0000 | −0.0072 |
C26 | 0.3268 | 0.0814 | 0.2993 | 0.0000 | 0.0000 | 0.0822 |
C27 | 0.3062 | 0.1381 | 0.2646 | 0.0635 | −0.0366 | 0.1092 |
C28 | 0.2925 | 0.2884 | 0.1270 | 0.0365 | −0.0831 | 0.0879 |
C29 | 0.3225 | 0.2143 | 0.1786 | 0.0309 | −0.0354 | 0.1331 |
C30 | 0.3241 | 0.3286 | 0.0672 | 0.0063 | −0.0486 | 0.0343 |
C31 | 0.2166 | 0.1258 | 0.1727 | −0.0408 | −0.0305 | −0.0796 |
C32 | 0.2286 | 0.1458 | 0.1335 | 0.0000 | 0.0000 | −0.0888 |
C33 | 0.2330 | 0.2050 | 0.0787 | 0.0000 | 0.0000 | −0.0657 |
C34 | 0.2145 | 0.1131 | 0.1840 | 0.0433 | 0.0272 | −0.0738 |
C35 | 0.2177 | 0.0790 | 0.2202 | −0.0487 | −0.0141 | −0.0445 |
C36 | 0.2250 | 0.1310 | 0.1447 | 0.0000 | 0.0000 | −0.0869 |
C37 | 0.2262 | 0.0525 | 0.2245 | 0.0000 | 0.0000 | −0.0176 |
C38 | 0.2187 | 0.2266 | 0.0721 | −0.0099 | −0.0486 | −0.0330 |
C39 | 0.2185 | 0.2225 | 0.0800 | 0.0145 | 0.0508 | −0.0443 |
C40 | 0.2175 | 0.0958 | 0.2030 | −0.0458 | 0.0213 | 0.0639 |
C41 | 0.2267 | 0.1913 | 0.0862 | 0.0000 | 0.0000 | −0.0706 |
C42 | 0.2261 | 0.0621 | 0.2147 | 0.0000 | 0.0000 | 0.0432 |
C43 | 0.2214 | 0.2372 | 0.0681 | −0.0036 | 0.0531 | 0.0115 |
C44 | 0.2163 | 0.1497 | 0.1480 | −0.0355 | 0.0358 | 0.0828 |
C45 | 0.2289 | 0.2180 | 0.0617 | 0.0000 | 0.0000 | 0.0429 |
C46 | 0.2265 | 0.1703 | 0.1069 | 0.0000 | 0.0000 | 0.0820 |
Geometric parameters (Å, º) top
C1—C20 | 1.4237 | C29—C29i | 1.4589 |
C1—C43 | 1.4883 | C30—C30i | 1.4678 |
C1—C2 | 1.3407 | C30—C38 | 1.4241 |
C2—C44 | 1.4580 | C31—C32 | 1.4039 |
C2—C21 | 1.4513 | C31—C35 | 1.4413 |
C3—C24 | 1.4819 | C32—C33 | 1.4360 |
C3—C13 | 1.4143 | C33—C38 | 1.4396 |
C3—C5 | 1.3986 | C33—C38i | 1.4396 |
C4—C31 | 1.4829 | C34—C36 | 1.4523 |
C4—C6 | 1.3770 | C35—C37 | 1.4081 |
C4—C14 | 1.4361 | C36—C41 | 1.4507 |
C5—C7 | 1.4252 | C37—C42 | 1.4413 |
C5—C27 | 1.4617 | C39—C41 | 1.4817 |
C6—C38 | 1.4710 | C39—C43 | 1.3743 |
C6—C8 | 1.3955 | C40—C44 | 1.4037 |
C7—C19 | 1.3864 | C40—C42 | 1.4093 |
C7—C17 | 1.4551 | C43—C45 | 1.4739 |
C8—C18 | 1.4310 | C44—C46 | 1.4136 |
C8—C19 | 1.4381 | C45—C46 | 1.4826 |
C9—C39 | 1.4942 | C52—C53 | 1.3248 |
C9—C20 | 1.4295 | C52—C57 | 1.3569 |
C9—C11 | 1.3607 | C53—C54 | 1.4227 |
C10—C21 | 1.4215 | C54—C55 | 1.3654 |
C10—C12 | 1.3240 | C54—C68 | 1.3985 |
C10—C40 | 1.4889 | C54—C68ii | 1.3985 |
C11—C13 | 1.4210 | C55—C56 | 1.3248 |
C11—C34 | 1.4872 | C56—C57 | 1.4340 |
C12—C14 | 1.4661 | C57—C58 | 1.3810 |
C12—C35 | 1.4755 | C57—C67 | 1.3994 |
C13—C15 | 1.4558 | C57—C67ii | 1.3994 |
C14—C16 | 1.3891 | C67—C68 | 1.3198 |
C15—C22 | 1.4209 | C52—H9 | 1.1000 |
C15—C17 | 1.3731 | C53—H10 | 1.1100 |
C16—C18 | 1.3757 | C54—H11 | 1.1200 |
C16—C23 | 1.4319 | C55—H12 | 1.1100 |
C17—C18 | 1.4012 | C56—H13 | 1.1300 |
C19—C28 | 1.4634 | C58—H15 | 1.0900 |
C20—C22 | 1.4381 | C58—H14 | 1.1000 |
C21—C23 | 1.4158 | C58—H16 | 1.1000 |
C22—C23 | 1.4184 | C58—H29 | 1.1100 |
C24—C34 | 1.3763 | C58—H30 | 1.0700 |
C24—C25 | 1.4486 | C58—H31 | 1.1200 |
C25—C26 | 1.4265 | C58—H29ii | 1.1100 |
C26—C27 | 1.4255 | C58—H30ii | 1.0700 |
C26—C27i | 1.4255 | C58—H31ii | 1.1200 |
C27—C29 | 1.3796 | C67—H24 | 1.1200 |
C28—C29 | 1.4163 | C68—H25 | 1.1100 |
C28—C30 | 1.3956 | | |
| | | |
C2—C1—C20 | 119.41 | C19—C28—C30 | 118.64 |
C2—C1—C43 | 119.48 | C29—C28—C30 | 116.27 |
C20—C1—C43 | 110.02 | C27—C29—C28 | 120.24 |
C1—C2—C21 | 119.31 | C27—C29—C29i | 108.20 |
C1—C2—C44 | 119.45 | C28—C29—C29i | 121.58 |
C21—C2—C44 | 109.97 | C28—C30—C38 | 120.23 |
C5—C3—C13 | 121.67 | C28—C30—C30i | 121.89 |
C5—C3—C24 | 120.15 | C30i—C30—C38 | 108.09 |
C13—C3—C24 | 108.54 | C4—C31—C35 | 108.14 |
C6—C4—C14 | 121.48 | C11—C34—C24 | 107.05 |
C6—C4—C31 | 120.14 | C12—C35—C31 | 107.03 |
C14—C4—C31 | 108.63 | C6—C38—C30 | 121.31 |
C3—C5—C7 | 116.96 | C9—C39—C43 | 107.76 |
C3—C5—C27 | 118.02 | C10—C40—C44 | 107.65 |
C7—C5—C27 | 118.50 | C1—C43—C39 | 107.13 |
C4—C6—C8 | 116.85 | C2—C44—C40 | 107.07 |
C4—C6—C38 | 118.19 | C53—C52—C57 | 119.60 |
C8—C6—C38 | 118.40 | C52—C53—C54 | 120.33 |
C5—C7—C17 | 120.73 | C53—C54—C55 | 120.42 |
C5—C7—C19 | 119.91 | C68—C54—C68ii | 120.14 |
C17—C7—C19 | 109.20 | C54—C55—C56 | 119.25 |
C6—C8—C18 | 120.84 | C55—C56—C57 | 120.20 |
C6—C8—C19 | 120.02 | C52—C57—C56 | 120.20 |
C18—C8—C19 | 108.86 | C52—C57—C58 | 119.94 |
C11—C9—C20 | 119.83 | C56—C57—C58 | 119.85 |
C11—C9—C39 | 119.82 | C58—C57—C67 | 119.97 |
C20—C9—C39 | 109.14 | C58—C57—C67ii | 119.97 |
C12—C10—C21 | 119.75 | C67—C57—C67ii | 120.01 |
C12—C10—C40 | 119.79 | C57—C67—C68 | 119.78 |
C21—C10—C40 | 109.12 | C54—C68—C67 | 119.82 |
C9—C11—C13 | 120.46 | C53—C52—H9 | 120.00 |
C9—C11—C34 | 119.72 | C57—C52—H9 | 121.00 |
C13—C11—C34 | 108.76 | C52—C53—H10 | 119.00 |
C10—C12—C14 | 120.21 | C54—C53—H10 | 121.00 |
C10—C12—C35 | 119.73 | C53—C54—H11 | 120.00 |
C14—C12—C35 | 108.73 | C55—C54—H11 | 120.00 |
C3—C13—C11 | 107.01 | C68—C54—H11 | 120.00 |
C3—C13—C15 | 121.38 | C68ii—C54—H11 | 120.00 |
C11—C13—C15 | 120.92 | C54—C55—H12 | 121.00 |
C4—C14—C12 | 107.18 | C56—C55—H12 | 120.00 |
C4—C14—C16 | 121.25 | C55—C56—H13 | 121.00 |
C12—C14—C16 | 120.86 | C57—C56—H13 | 119.00 |
C13—C15—C17 | 116.10 | C57—C58—H15 | 110.00 |
C13—C15—C22 | 118.57 | C57—C58—H14 | 109.00 |
C17—C15—C22 | 119.73 | C57—C58—H16 | 109.00 |
C14—C16—C18 | 116.30 | C57—C58—H29 | 109.00 |
C14—C16—C23 | 118.69 | C57—C58—H30 | 110.00 |
C18—C16—C23 | 119.42 | C57—C58—H31 | 109.00 |
C7—C17—C15 | 121.88 | C57—C58—H29ii | 109.00 |
C7—C17—C18 | 107.55 | C57—C58—H30ii | 110.00 |
C15—C17—C18 | 121.12 | C57—C58—H31ii | 109.00 |
C8—C18—C16 | 122.13 | H14—C58—H16 | 110.00 |
C8—C18—C17 | 107.45 | H29—C58—H30 | 111.00 |
C16—C18—C17 | 120.91 | H29—C58—H31 | 106.00 |
C7—C19—C8 | 106.92 | H29—C58—H29ii | 61.00 |
C7—C19—C28 | 121.11 | H29—C58—H30ii | 54.00 |
C8—C19—C28 | 121.05 | H29—C58—H31ii | 142.00 |
C1—C20—C9 | 105.32 | H30—C58—H31 | 111.00 |
C1—C20—C22 | 122.50 | H29ii—C58—H30 | 54.00 |
C9—C20—C22 | 121.73 | H30—C58—H30ii | 140.00 |
C2—C21—C10 | 105.28 | H30—C58—H31ii | 55.00 |
C2—C21—C23 | 122.40 | H29ii—C58—H31 | 142.00 |
C10—C21—C23 | 121.82 | H30ii—C58—H31 | 55.00 |
C15—C22—C20 | 117.90 | H31—C58—H31ii | 60.00 |
C15—C22—C23 | 119.44 | H29ii—C58—H30ii | 111.00 |
C20—C22—C23 | 117.91 | H29ii—C58—H31ii | 106.00 |
C16—C23—C21 | 118.10 | H30ii—C58—H31ii | 111.00 |
C16—C23—C22 | 119.31 | C57—C67—H24 | 120.00 |
C21—C23—C22 | 117.74 | C68—C67—H24 | 120.00 |
C3—C24—C34 | 108.31 | C54—C68—H25 | 120.00 |
C5—C27—C29 | 121.36 | C67—C68—H25 | 120.00 |
C19—C28—C29 | 118.64 | | |
Symmetry codes: (i) −x, y, z; (ii) −x+1, y, z. |
Experimental details
Crystal data |
Chemical formula | YC82·C7H8 |
Mr | 4663.79 |
Crystal system, space group | Orthorhombic, Cmc21 |
Temperature (K) | 300 |
a, b, c (Å) | 11.22205 (6), 34.8174 (2), 11.22569 (7) |
V (Å3) | 4386.13 (7) |
Z | 1 |
Radiation type | Synchrotron, λ = 0.73330 Å |
µ (mm−1) | 0.33 |
Specimen shape, size (mm) | Cylinder, 3 × 0.4 |
|
Data collection |
Diffractometer | Large Debye-Scherrer camera diffractometer |
Specimen mounting | Capillary |
Data collection mode | Transmission |
Scan method | Step |
2θ values (°) | 2θmin = 3.00 2θmax = 32.50 2θstep = 0.010 |
|
Refinement |
R factors and goodness of fit | Rp = 0.044, Rwp = 0.015, Rexp = ?, χ2 = ? |
No. of data points | 7508 |
No. of parameters | 272 |
No. of restraints | 348 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |