Orientational disorder as a function of temperature in the clathrate structure of hydroquinone and C60

Blanc, E.; Restori, R.; Schwarzenbach, D.; Bürgi, H.-B.; Förtsch, M.; Venugopalan, P.; Ermer, O.

doi:10.1107/S0108768100007564

Orientational disorder as a function of temperature in the clathrate structure of hydroquinone and C₆₀

E. Blanc, R. Restori, D. Schwarzenbach, H.-B. Bürgi, M. Förtsch, P. Venugopalan and O. Ermer

In the compound [C₆H₆O₂]₃C₆₀, hydroquinone (C₆H₆O₂) forms a three-dimensional hydrogen-bonded network enclosing roughly spherical cages with point symmetry $\overline 3$ m and a diameter of 13.2 Å at 100 K. Although C₆₀ 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, C₆₀ was restrained to the icosahedral molecular symmetry m $\overline {35}$ 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 C₆₀ 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 C₆₀ are relatively small (5.5° at 373 K) and the probability function of orientations of C₆₀ 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 C₆₀ appear to be uncorrelated.

Keywords: Orientational disorder; Clathrates; Temperature; Hydroquinone.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100007564/bk0080sup1.cif Contains datablocks global, 373K, 293K, 200K, 100K
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100007564/bk0080373Ksup2.hkl Contains datablock 373K
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100007564/bk0080293Ksup3.hkl Contains datablock 293K
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100007564/bk0080200Ksup4.hkl Contains datablock 200K
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100007564/bk0080100Ksup5.hkl Contains datablock 100K

CCDC references: 156654; 156655; 156656; 156657

Computing details top

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.

(373K) top

Crystal data top

(C₆H₆O₂)₃·C₆₀	D_x = 1.658 Mg m⁻³
M_r = 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	R_int = 0.017
Radiation source: fine-focus sealed tube	θ_max = 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	Δρ_max = 0.4 e Å⁻³
1136 reflections	Δρ_min = −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
M_r = 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	R_int = 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	Δρ_max = 0.4 e Å⁻³
85 parameters	Δρ_min = −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	U_iso*/U_eq
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)

(293K) top

Crystal data top

(C₆H₆O₂)₃·C₆₀	D_x = 1.672 Mg m⁻³
M_r = 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	R_int = 0.011
Radiation source: fine-focus sealed tube	θ_max = 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	Δρ_max = 0.4 e Å⁻³
1124 reflections	Δρ_min = −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
M_r = 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	R_int = 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	Δρ_max = 0.4 e Å⁻³
85 parameters	Δρ_min = −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	U_iso*/U_eq
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)

(200K) top

Crystal data top

(C₆H₆O₂)₃·C₆₀	D_x = 1.685 Mg m⁻³
M_r = 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	R_int = 0.022
Radiation source: fine-focus sealed tube	θ_max = 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	Δρ_max = 0.4 e Å⁻³
1115 reflections	Δρ_min = −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
M_r = 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	R_int = 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	Δρ_max = 0.4 e Å⁻³
85 parameters	Δρ_min = −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	U_iso*/U_eq
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)

(100K) top

Crystal data top

(C₆H₆O₂)₃·C₆₀	D_x = 1.700 Mg m⁻³
M_r = 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	R_int = 0.015
Radiation source: fine-focus sealed tube	θ_max = 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	Δρ_max = 0.4 e Å⁻³
1106 reflections	Δρ_min = −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
M_r = 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	R_int = 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	Δρ_max = 0.4 e Å⁻³
85 parameters	Δρ_min = −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	U_iso*/U_eq
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
M_r	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
R_int	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
Δρ_max, Δρ_min (e Å⁻³)	0.4, −0.4	0.4, −0.4	0.4, −0.4	0.4, −0.4

Computer programs: CAD-4 Software, trial and error, local software, adaptation of LSLS, ATOMS, Dowty (1993), Shape Software. 521 Hidden Valley Road, Kingsport TN 37663, USA..

	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)

	T11	T22	T33	T13
C103	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C104	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C105	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C106	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C109	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C110	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C111	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C112	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C113	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C114	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C115	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C116	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C117	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C118	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C119	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)
C120	.00807 (12)	.00663 (12)	.00795 (11)	.00031 (10)

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

	L11	L22	L33	L13
C103	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C104	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C105	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C106	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C109	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C110	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C111	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C112	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C113	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C114	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C115	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C116	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C117	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C118	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C119	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)
C120	.001842 (15)	.001135 (13)	.000912 (17)	-.000112 (11)

Search IUCr Journals		doi		Advanced search
Author		volume	page