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In the compound [C
6H
6O
2]
3C
60, hydroquinone (C
6H
6O
2) forms a three-dimensional hydrogen-bonded network enclosing roughly spherical cages with point symmetry
m and a diameter of 13.2 Å at 100 K. Although C
60 fits tightly into these cages, it shows threefold orientational disorder, the molecular site symmetry being 2/
m. The disorder has been studied with single-crystal Mo
Kα X-ray data at four temperatures, 100, 200, 293 and 373 K. In the refinement, C
60 was restrained to the icosahedral molecular symmetry
m and to rigid-body translational and librational displacements including third- and fourth-order cumulants to account for curvilinear atomic movements,
R(|
F|) = 3.2–4.7%. At 100 K, bond lengths in C
60 refine to the expected values 1.450 (1) and 1.388 (1) Å. The ratio of these values increases with increasing temperature, but the radius of the molecule remains constant at 3.537 (2) Å. The r.m.s. libration amplitudes of C
60 are relatively small (5.5° at 373 K) and the probability function of orientations of C
60 inside the cage shows large values only at the refined positions, indicating that the energy barrier of reorientation is large. Refinement of an ordered twinned structure was unsuccessful; the orientations of neighboring C
60 appear to be uncorrelated.
Supporting information
CCDC references: 156654; 156655; 156656; 156657
For all compounds, data collection: CAD-4 Software; cell refinement: CAD-4 Software; data reduction: local software; program(s) used to solve structure: trial and error; program(s) used to refine structure: local software, adaptation of LSLS; molecular graphics: ATOMS, Dowty (1993), Shape Software. 521 Hidden Valley Road, Kingsport TN 37663, USA.
Crystal data top
(C6H6O2)3·C60 | Dx = 1.658 Mg m−3 |
Mr = 1051.00 | Mo Kα radiation, λ = 0.710769 Å |
Trigonal, R3m | Cell parameters from 25 reflections |
Hall symbol: -R 3 2" | θ = 8.7–26.3° |
a = 16.212 (2) Å | µ = 0.11 mm−1 |
c = 13.873 (2) Å | T = 373 K |
V = 3157.7 (9) Å3 | , dark brown-red |
Z = 3 | 0.41 × 0.36 × 0.33 mm |
F(000) = 1602 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.017 |
Radiation source: fine-focus sealed tube | θmax = 30.0° |
Graphite monochromator | h = −11→22 |
ω scans | k = 0→22 |
3607 measured reflections | l = −19→19 |
1136 independent reflections | 3 standard reflections every 120 min |
702 reflections with I > 3σ(I) | intensity decay: 10.0% |
Refinement top
Refinement on F2 | All H-atom parameters refined |
Least-squares matrix: full | Weighting scheme based on measured s.u.'s |
R[F2 > 2σ(F2)] = 0.047 | (Δ/σ)max = 0.01 |
wR(F2) = 0.073 | Δρmax = 0.4 e Å−3 |
1136 reflections | Δρmin = −0.4 e Å−3 |
85 parameters | Extinction correction: Becker & Coppens (1974), Becker & Coppens (1974) |
68 restraints | |
Crystal data top
(C6H6O2)3·C60 | Z = 3 |
Mr = 1051.00 | Mo Kα radiation |
Trigonal, R3m | µ = 0.11 mm−1 |
a = 16.212 (2) Å | T = 373 K |
c = 13.873 (2) Å | 0.41 × 0.36 × 0.33 mm |
V = 3157.7 (9) Å3 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.017 |
3607 measured reflections | 3 standard reflections every 120 min |
1136 independent reflections | intensity decay: 10.0% |
702 reflections with I > 3σ(I) | |
Refinement top
R[F2 > 2σ(F2)] = 0.047 | 68 restraints |
wR(F2) = 0.073 | All H-atom parameters refined |
1136 reflections | Δρmax = 0.4 e Å−3 |
85 parameters | Δρmin = −0.4 e Å−3 |
Special details top
Refinement. The C60 molecule had thermal parameters refined via the T and L tensors of the rigid body model. The angles were restrained. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C4 | 0.26248 (2) | 0.13124 (1) | 0.59748 (2) | 0.04114 (15) | |
O4 | 0.19225 (3) | 0.09612 (2) | 0.52840 (2) | 0.06608 (15) | |
C5 | 0.29812 (2) | 0.07592 (2) | 0.63244 (2) | 0.04538 (13) | |
H4 | 0.1686 (5) | 0.1220 (4) | 0.5112 (5) | 0.114 (3)* | |
H5 | 0.27274 (16) | 0.01282 (16) | 0.60774 (14) | 0.0449 (6)* | |
C103 | 0.01414 (5) | −0.03855 (5) | 0.24888 (3) | 0.0978 (2) | |
C104 | −0.08235 (5) | −0.11472 (5) | 0.22536 (3) | 0.0905 (2) | |
C105 | −0.14221 (6) | −0.07111 (3) | 0.21049 (5) | 0.0863 (2) | |
C106 | −0.20948 (5) | −0.10474 (3) | 0.14114 (5) | 0.0807 (2) | |
C109 | −0.24600 (5) | −0.16852 (4) | −0.01830 (6) | 0.0843 (2) | |
C110 | −0.22335 (4) | −0.18530 (4) | 0.08024 (5) | 0.0805 (2) | |
C111 | −0.16889 (4) | −0.22533 (4) | 0.09359 (4) | 0.0819 (2) | |
C112 | −0.09530 (4) | −0.18896 (5) | 0.16907 (4) | 0.0864 (2) | |
C113 | −0.01255 (4) | −0.19277 (6) | 0.13192 (5) | 0.0873 (2) | |
C114 | −0.03475 (4) | −0.23097 (7) | 0.03213 (5) | 0.0835 (3) | |
C115 | −0.13117 (4) | −0.25207 (5) | 0.00890 (5) | 0.0837 (2) | |
C116 | −0.15122 (5) | −0.23640 (5) | −0.08021 (5) | 0.0879 (2) | |
C117 | −0.21120 (5) | −0.19238 (7) | −0.09503 (5) | 0.0898 (2) | |
C118 | −0.17437 (7) | −0.12934 (8) | −0.17762 (6) | 0.0973 (2) | |
C119 | −0.09076 (5) | −0.13255 (7) | −0.21394 (4) | 0.0975 (2) | |
C120 | −0.07678 (5) | −0.19835 (5) | −0.15308 (5) | 0.0909 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C4 | 0.0425 (2) | 0.03971 (16) | 0.0421 (2) | 0.02123 (11) | 0.00834 (18) | 0.00417 (9) |
O4 | 0.0648 (2) | 0.06576 (17) | 0.0673 (2) | 0.03242 (11) | −0.01330 (17) | −0.00665 (9) |
C5 | 0.05424 (19) | 0.02983 (15) | 0.05376 (17) | 0.02230 (14) | 0.00855 (12) | 0.00087 (12) |
Crystal data top
(C6H6O2)3·C60 | Dx = 1.672 Mg m−3 |
Mr = 1051.00 | Mo Kα radiation, λ = 0.710769 Å |
Trigonal, R3m | Cell parameters from 25 reflections |
Hall symbol: -R 3 2" | θ = 8.7–26.3° |
a = 16.177 (2) Å | µ = 0.11 mm−1 |
c = 13.813 (2) Å | T = 293 K |
V = 3130.5 (9) Å3 | , dark brown-red |
Z = 3 | 0.41 × 0.36 × 0.33 mm |
F(000) = 1602 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.011 |
Radiation source: fine-focus sealed tube | θmax = 30.0° |
Graphite monochromator | h = −11→22 |
ω scans | k = 0→22 |
3365 measured reflections | l = −19→19 |
1124 independent reflections | 3 standard reflections every 120 min |
751 reflections with I > 3σ(I) | intensity decay: none |
Refinement top
Refinement on F2 | All H-atom parameters refined |
Least-squares matrix: full | Weighting scheme based on measured s.u.'s |
R[F2 > 2σ(F2)] = 0.042 | (Δ/σ)max = 0.01 |
wR(F2) = 0.057 | Δρmax = 0.4 e Å−3 |
1124 reflections | Δρmin = −0.4 e Å−3 |
85 parameters | Extinction correction: Becker & Coppens (1974), Becker & Coppens (1974) |
68 restraints | |
Crystal data top
(C6H6O2)3·C60 | Z = 3 |
Mr = 1051.00 | Mo Kα radiation |
Trigonal, R3m | µ = 0.11 mm−1 |
a = 16.177 (2) Å | T = 293 K |
c = 13.813 (2) Å | 0.41 × 0.36 × 0.33 mm |
V = 3130.5 (9) Å3 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.011 |
3365 measured reflections | 3 standard reflections every 120 min |
1124 independent reflections | intensity decay: none |
751 reflections with I > 3σ(I) | |
Refinement top
R[F2 > 2σ(F2)] = 0.042 | 68 restraints |
wR(F2) = 0.057 | All H-atom parameters refined |
1124 reflections | Δρmax = 0.4 e Å−3 |
85 parameters | Δρmin = −0.4 e Å−3 |
Special details top
Refinement. The C60 molecule had thermal parameters refined via the T and L tensors of the rigid body model. The angles were restrained. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C4 | 0.26227 (2) | 0.13114 (1) | 0.59711 (2) | 0.03277 (14) | |
O4 | 0.19189 (2) | 0.09594 (1) | 0.52763 (2) | 0.05426 (14) | |
C5 | 0.29797 (2) | 0.07550 (2) | 0.63209 (2) | 0.03554 (12) | |
H4 | 0.1651 (4) | 0.1201 (4) | 0.5140 (5) | 0.095 (3)* | |
H5 | 0.27097 (14) | 0.01065 (19) | 0.60757 (13) | 0.0389 (6)* | |
C103 | 0.01332 (5) | −0.03893 (4) | 0.24998 (3) | 0.06795 (18) | |
C104 | −0.08291 (4) | −0.11488 (4) | 0.22624 (3) | 0.06291 (17) | |
C105 | −0.14263 (5) | −0.07131 (2) | 0.21130 (4) | 0.05982 (17) | |
C106 | −0.21049 (5) | −0.10524 (2) | 0.14108 (5) | 0.05576 (17) | |
C109 | −0.24626 (4) | −0.16847 (4) | −0.01840 (5) | 0.05790 (18) | |
C110 | −0.22414 (3) | −0.18546 (4) | 0.08018 (4) | 0.05557 (17) | |
C111 | −0.16913 (3) | −0.22596 (4) | 0.09389 (4) | 0.05698 (17) | |
C112 | −0.09587 (4) | −0.18971 (4) | 0.16939 (3) | 0.06023 (17) | |
C113 | −0.01313 (4) | −0.19330 (5) | 0.13225 (4) | 0.06108 (18) | |
C114 | −0.03533 (4) | −0.23195 (6) | 0.03297 (4) | 0.0588 (2) | |
C115 | −0.13145 (4) | −0.25269 (5) | 0.00948 (4) | 0.05849 (18) | |
C116 | −0.15115 (4) | −0.23638 (5) | −0.08097 (4) | 0.06107 (17) | |
C117 | −0.21114 (5) | −0.19282 (6) | −0.09600 (4) | 0.06199 (17) | |
C118 | −0.17441 (6) | −0.12986 (6) | −0.17879 (5) | 0.06731 (17) | |
C119 | −0.09048 (4) | −0.13263 (6) | −0.21489 (4) | 0.06768 (17) | |
C120 | −0.07674 (4) | −0.19881 (5) | −0.15422 (5) | 0.06362 (17) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C4 | 0.0322 (2) | 0.03231 (14) | 0.03377 (18) | 0.01610 (11) | 0.00587 (17) | 0.00293 (8) |
O4 | 0.05011 (19) | 0.05688 (17) | 0.05353 (19) | 0.02506 (10) | −0.01262 (15) | −0.00631 (8) |
C5 | 0.04283 (17) | 0.02449 (13) | 0.04080 (15) | 0.01795 (13) | 0.00704 (12) | 0.00086 (11) |
Crystal data top
(C6H6O2)3·C60 | Dx = 1.685 Mg m−3 |
Mr = 1051.00 | Mo Kα radiation, λ = 0.710769 Å |
Trigonal, R3m | Cell parameters from 25 reflections |
Hall symbol: -R 3 2" | θ = 8.7–26.3° |
a = 16.152 (2) Å | µ = 0.11 mm−1 |
c = 13.750 (2) Å | T = 200 K |
V = 3106.4 (9) Å3 | , dark brown-red |
Z = 3 | 0.41 × 0.36 × 0.33 mm |
F(000) = 1602 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.022 |
Radiation source: fine-focus sealed tube | θmax = 30.0° |
Graphite monochromator | h = −11→22 |
ω scans | k = 0→22 |
2676 measured reflections | l = −19→19 |
1115 independent reflections | 3 standard reflections every 120 min |
739 reflections with I > 3σ(I) | intensity decay: 10.0% |
Refinement top
Refinement on F2 | All H-atom parameters refined |
Least-squares matrix: full | Weighting scheme based on measured s.u.'s |
R[F2 > 2σ(F2)] = 0.032 | (Δ/σ)max = 0.01 |
wR(F2) = 0.057 | Δρmax = 0.4 e Å−3 |
1115 reflections | Δρmin = −0.4 e Å−3 |
85 parameters | Extinction correction: Becker & Coppens (1974), Becker & Coppens (1974) |
68 restraints | |
Crystal data top
(C6H6O2)3·C60 | Z = 3 |
Mr = 1051.00 | Mo Kα radiation |
Trigonal, R3m | µ = 0.11 mm−1 |
a = 16.152 (2) Å | T = 200 K |
c = 13.750 (2) Å | 0.41 × 0.36 × 0.33 mm |
V = 3106.4 (9) Å3 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.022 |
2676 measured reflections | 3 standard reflections every 120 min |
1115 independent reflections | intensity decay: 10.0% |
739 reflections with I > 3σ(I) | |
Refinement top
R[F2 > 2σ(F2)] = 0.032 | 68 restraints |
wR(F2) = 0.057 | All H-atom parameters refined |
1115 reflections | Δρmax = 0.4 e Å−3 |
85 parameters | Δρmin = −0.4 e Å−3 |
Special details top
Refinement. The C60 molecule had thermal parameters refined via the T and L tensors of the rigid body model. The angles were restrained. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C4 | 0.26213 (3) | 0.13106 (2) | 0.59684 (3) | 0.02369 (17) | |
O4 | 0.19155 (3) | 0.09578 (2) | 0.52661 (3) | 0.04079 (18) | |
C5 | 0.29767 (2) | 0.07486 (3) | 0.63180 (2) | 0.02606 (15) | |
H4 | 0.1631 (6) | 0.1196 (6) | 0.5187 (7) | 0.069 (4)* | |
H5 | 0.2710 (2) | 0.0101 (3) | 0.6083 (2) | 0.0339 (10)* | |
C103 | 0.01199 (5) | −0.03911 (4) | 0.25161 (4) | 0.04051 (16) | |
C104 | −0.08393 (4) | −0.11486 (5) | 0.22746 (4) | 0.03813 (16) | |
C105 | −0.14322 (5) | −0.07161 (3) | 0.21232 (5) | 0.03611 (17) | |
C106 | −0.21195 (5) | −0.10598 (2) | 0.14049 (5) | 0.03331 (18) | |
C109 | −0.24667 (5) | −0.16836 (5) | −0.01855 (5) | 0.03358 (18) | |
C110 | −0.22527 (4) | −0.18550 (4) | 0.07979 (4) | 0.03313 (18) | |
C111 | −0.16941 (4) | −0.22675 (5) | 0.09419 (4) | 0.03507 (17) | |
C112 | −0.09670 (4) | −0.19049 (5) | 0.16990 (4) | 0.03726 (16) | |
C113 | −0.01408 (4) | −0.19412 (6) | 0.13335 (5) | 0.03841 (16) | |
C114 | −0.03564 (5) | −0.23240 (8) | 0.03471 (5) | 0.03764 (18) | |
C115 | −0.13181 (5) | −0.25333 (6) | 0.01085 (5) | 0.03659 (18) | |
C116 | −0.15124 (5) | −0.23626 (6) | −0.08205 (5) | 0.03713 (17) | |
C117 | −0.21124 (5) | −0.19364 (8) | −0.09729 (5) | 0.03628 (17) | |
C118 | −0.17363 (6) | −0.12953 (8) | −0.18020 (6) | 0.03890 (17) | |
C119 | −0.09029 (5) | −0.13260 (7) | −0.21644 (5) | 0.04020 (16) | |
C120 | −0.07688 (4) | −0.19886 (5) | −0.15591 (6) | 0.03902 (16) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C4 | 0.0223 (3) | 0.0247 (2) | 0.0233 (2) | 0.01117 (13) | 0.0050 (2) | 0.00250 (10) |
O4 | 0.0345 (3) | 0.0460 (2) | 0.0380 (2) | 0.01724 (13) | −0.00891 (19) | −0.00445 (9) |
C5 | 0.03045 (19) | 0.01829 (17) | 0.02925 (16) | 0.01205 (16) | 0.00530 (15) | 0.00083 (14) |
Crystal data top
(C6H6O2)3·C60 | Dx = 1.700 Mg m−3 |
Mr = 1051.00 | Mo Kα radiation, λ = 0.710769 Å |
Trigonal, R3m | Cell parameters from 25 reflections |
Hall symbol: -R 3 2" | θ = 8.7–26.3° |
a = 16.119 (2) Å | µ = 0.11 mm−1 |
c = 13.687 (2) Å | T = 100 K |
V = 3079.5 (9) Å3 | , dark brown-red |
Z = 3 | 0.41 × 0.36 × 0.33 mm |
F(000) = 1602 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.015 |
Radiation source: fine-focus sealed tube | θmax = 30.0° |
Graphite monochromator | h = −11→22 |
ω scans | k = 0→22 |
3481 measured reflections | l = −19→19 |
1106 independent reflections | 3 standard reflections every 120 min |
823 reflections with I > 3σ(I) | intensity decay: 10.0% |
Refinement top
Refinement on F2 | All H-atom parameters refined |
Least-squares matrix: full | Weighting scheme based on measured s.u.'s |
R[F2 > 2σ(F2)] = 0.036 | (Δ/σ)max = 0.01 |
wR(F2) = 0.057 | Δρmax = 0.4 e Å−3 |
1106 reflections | Δρmin = −0.4 e Å−3 |
85 parameters | Extinction correction: Becker & Coppens (1974), Becker & Coppens (1974) |
68 restraints | |
Crystal data top
(C6H6O2)3·C60 | Z = 3 |
Mr = 1051.00 | Mo Kα radiation |
Trigonal, R3m | µ = 0.11 mm−1 |
a = 16.119 (2) Å | T = 100 K |
c = 13.687 (2) Å | 0.41 × 0.36 × 0.33 mm |
V = 3079.5 (9) Å3 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | Rint = 0.015 |
3481 measured reflections | 3 standard reflections every 120 min |
1106 independent reflections | intensity decay: 10.0% |
823 reflections with I > 3σ(I) | |
Refinement top
R[F2 > 2σ(F2)] = 0.036 | 68 restraints |
wR(F2) = 0.057 | All H-atom parameters refined |
1106 reflections | Δρmax = 0.4 e Å−3 |
85 parameters | Δρmin = −0.4 e Å−3 |
Special details top
Refinement. The C60 molecule had thermal parameters refined via the T and L tensors of the rigid body model. The angles were restrained. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C4 | 0.26185 (2) | 0.13093 (1) | 0.59647 (2) | 0.01469 (12) | |
O4 | 0.19128 (2) | 0.09564 (1) | 0.52590 (2) | 0.02748 (9) | |
C5 | 0.29761 (2) | 0.07461 (2) | 0.63151 (2) | 0.01634 (10) | |
H4 | 0.1641 (4) | 0.1213 (5) | 0.5139 (5) | 0.057 (2)* | |
H5 | 0.27155 (16) | 0.00903 (17) | 0.60727 (16) | 0.0171 (6)* | |
C103 | 0.01121 (3) | −0.03939 (3) | 0.25305 (3) | 0.01999 (11) | |
C104 | −0.08454 (3) | −0.11505 (3) | 0.22847 (3) | 0.01919 (11) | |
C105 | −0.14371 (4) | −0.07185 (2) | 0.21317 (4) | 0.01831 (11) | |
C106 | −0.21277 (4) | −0.10639 (2) | 0.14028 (4) | 0.01680 (11) | |
C109 | −0.24707 (4) | −0.16842 (4) | −0.01893 (4) | 0.01628 (11) | |
C110 | −0.22594 (3) | −0.18566 (3) | 0.07958 (3) | 0.01651 (11) | |
C111 | −0.16967 (3) | −0.22742 (4) | 0.09436 (3) | 0.01765 (11) | |
C112 | −0.09723 (3) | −0.19122 (3) | 0.17031 (2) | 0.01881 (10) | |
C113 | −0.01454 (3) | −0.19459 (4) | 0.13371 (4) | 0.01924 (11) | |
C114 | −0.03595 (4) | −0.23305 (5) | 0.03548 (4) | 0.01897 (12) | |
C115 | −0.13185 (3) | −0.25368 (4) | 0.01121 (3) | 0.01827 (11) | |
C116 | −0.15143 (4) | −0.23647 (4) | −0.08310 (3) | 0.01823 (11) | |
C117 | −0.21135 (4) | −0.19410 (5) | −0.09847 (3) | 0.01745 (11) | |
C118 | −0.17352 (4) | −0.12978 (5) | −0.18151 (4) | 0.01857 (11) | |
C119 | −0.09032 (3) | −0.13267 (5) | −0.21750 (3) | 0.01954 (10) | |
C120 | −0.07712 (3) | −0.19902 (4) | −0.15680 (4) | 0.01923 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C4 | 0.01174 (17) | 0.01716 (13) | 0.01337 (16) | 0.00587 (9) | 0.00208 (14) | 0.00104 (7) |
O4 | 0.01988 (15) | 0.03597 (15) | 0.02123 (14) | 0.00994 (8) | −0.00633 (12) | −0.00316 (6) |
C5 | 0.01829 (14) | 0.01201 (13) | 0.01784 (12) | 0.00692 (11) | 0.00339 (10) | 0.00014 (10) |
Experimental details
| (373K) | (293K) | (200K) | (100K) |
Crystal data |
Chemical formula | (C6H6O2)3·C60 | (C6H6O2)3·C60 | (C6H6O2)3·C60 | (C6H6O2)3·C60 |
Mr | 1051.00 | 1051.00 | 1051.00 | 1051.00 |
Crystal system, space group | Trigonal, R3m | Trigonal, R3m | Trigonal, R3m | Trigonal, R3m |
Temperature (K) | 373 | 293 | 200 | 100 |
a, c (Å) | 16.212 (2), 13.873 (2) | 16.177 (2), 13.813 (2) | 16.152 (2), 13.750 (2) | 16.119 (2), 13.687 (2) |
V (Å3) | 3157.7 (9) | 3130.5 (9) | 3106.4 (9) | 3079.5 (9) |
Z | 3 | 3 | 3 | 3 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.11 | 0.11 | 0.11 | 0.11 |
Crystal size (mm) | 0.41 × 0.36 × 0.33 | 0.41 × 0.36 × 0.33 | 0.41 × 0.36 × 0.33 | 0.41 × 0.36 × 0.33 |
|
Data collection |
Diffractometer | Enraf-Nonius CAD-4 diffractometer | Enraf-Nonius CAD-4 diffractometer | Enraf-Nonius CAD-4 diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | – | – | – | – |
No. of measured, independent and observed [I > 3σ(I)] reflections | 3607, 1136, 702 | 3365, 1124, 751 | 2676, 1115, 739 | 3481, 1106, 823 |
Rint | 0.017 | 0.011 | 0.022 | 0.015 |
(sin θ/λ)max (Å−1) | 0.703 | 0.703 | 0.703 | 0.703 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.073, ? | 0.042, 0.057, ? | 0.032, 0.057, ? | 0.036, 0.057, ? |
No. of reflections | 1136 | 1124 | 1115 | 1106 |
No. of parameters | 85 | 85 | 85 | 85 |
No. of restraints | 68 | 68 | 68 | 68 |
H-atom treatment | All H-atom parameters refined | All H-atom parameters refined | All H-atom parameters refined | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 0.4, −0.4 | 0.4, −0.4 | 0.4, −0.4 | 0.4, −0.4 |
| T11 | T22 | T33 | T13 |
C103 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C104 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C105 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C106 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C109 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C110 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C111 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C112 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C113 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C114 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C115 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C116 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C117 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C118 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C119 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
C120 | .0216 (2) | .0227 (2) | .02433 (15) | .0033 (3) |
| L11 | L22 | L33 | L13 |
C103 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C104 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C105 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C106 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C109 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C110 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C111 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C112 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C113 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C114 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C115 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C116 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C117 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C118 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C119 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
C120 | .00908 (4) | .00886 (3) | .00557 (4) | -.00174 (2) |
| T11 | T22 | T33 | T13 |
C103 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C104 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C105 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C106 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C109 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C110 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C111 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C112 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C113 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C114 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C115 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C116 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C117 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C118 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C119 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
C120 | .01699 (17) | .01709 (18) | .01832 (13) | .00161 (19) |
| L11 | L22 | L33 | L13 |
C103 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C104 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C105 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C106 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C109 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C110 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C111 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C112 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C113 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C114 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C115 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C116 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C117 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C118 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C119 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
C120 | .00628 (3) | .00581 (2) | .00369 (3) | -.001188 (18) |
| T11 | T22 | T33 | T13 |
C103 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C104 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C105 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C106 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C109 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C110 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C111 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C112 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C113 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C114 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C115 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C116 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C117 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C118 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C119 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
C120 | .01333 (18) | .01157 (19) | .01348 (16) | .00031 (17) |
| L11 | L22 | L33 | L13 |
C103 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C104 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C105 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C106 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C109 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C110 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C111 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C112 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C113 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C114 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C115 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C116 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C117 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C118 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C119 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |
C120 | .00388 (2) | .00274 (2) | .00212 (3) | -.000512 (18) |