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The polymorphic phase transition of 1,2,4,5-tetrachlorobenzene (TCB) has been investigated using neutron powder diffraction and single-crystal X-ray diffraction. The diffraction experiments show a reversible phase change that occurs as a function of temperature with no apparent loss of sample quality on transition between the two phases. Neutron powder diffraction gives detailed information on the molecular structural changes and lattice parameters from 2 K to room temperature. The structure of the low-temperature form has been elucidated for the first time using single-crystal X-ray diffraction. Comparison of the α and β structures show that they are both based on the same sheet motif, with the differences between the two being very subtle, except in terms of crystal symmetry. Detailed analysis of the structures revealed the changes required for inter-conversion. A computational polymorph search showed that these two sheet structures are more thermodynamically stable than alternative herringbone-type structures.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105042102/so5001sup1.cif
Contains datablocks tcb_alpha_150K_X-ray, global, tcb_alpha_2K_neutron_powder, tcb_alpha_150K_neutron, tcb_beta_150K_neutron, tcb_beta_200K_neutron, tcb_beta_295K_neutron

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768105042102/so5001tcb_alpha_150K_X-raysup2.hkl
Contains datablock both

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768105042102/so5001sup3.pdf
Supplementary material

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768105042102/so5001sup4.pdf
Supplementary material

CCDC references: 605627; 605628; 605629; 605630; 605631; 605632

Computing details top

Data collection: Bruker SMART for tcb_alpha_150K_X-ray; custom ISIS software for tcb_alpha_2K_neutron_powder, tcb_alpha_150K_neutron, tcb_beta_150K_neutron, tcb_beta_200K_neutron, tcb_beta_295K_neutron. Cell refinement: Bruker SAINT for tcb_alpha_150K_X-ray. Data reduction: Bruker SAINT for tcb_alpha_150K_X-ray; custom ISIS software for tcb_alpha_2K_neutron_powder, tcb_alpha_150K_neutron, tcb_beta_150K_neutron, tcb_beta_200K_neutron, tcb_beta_295K_neutron. Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990) for tcb_alpha_150K_X-ray. Program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) for tcb_alpha_150K_X-ray; Topas v3.1 (Coehlo, 2003) for tcb_alpha_2K_neutron_powder, tcb_alpha_150K_neutron, tcb_beta_150K_neutron, tcb_beta_200K_neutron, tcb_beta_295K_neutron. Molecular graphics: Bruker SHELXTL for tcb_alpha_150K_X-ray. Software used to prepare material for publication: Bruker SHELXTL and local programs for tcb_alpha_150K_X-ray.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(tcb_alpha_150K_X-ray) Tetrachlorobenzene - alpha polymorph top
Crystal data top
C6H2Cl4Z = 2
Mr = 215.88F(000) = 212
Triclinic, P1Dx = 1.907 Mg m3
a = 3.8016 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.6369 (15) ÅCell parameters from 2248 reflections
c = 9.4866 (13) Åθ = 2.2–28.2°
α = 92.072 (2)°µ = 1.48 mm1
β = 98.966 (2)°T = 150 K
γ = 96.520 (2)°Block, colourless
V = 375.91 (9) Å30.11 × 0.08 × 0.04 mm
Data collection top
Bruker SMART APEX
diffractometer
5184 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 28.3°, θmin = 1.9°
ω rotation with narrow frames scansh = 55
6306 measured reflectionsk = 1413
5690 independent reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier synthesis
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: geometrically placed
wR(F2) = 0.099Riding model
S = 1.03 w = 1/[σ2(Fo2) + (0.0685P)2]
where P = (Fo2 + 2Fc2)/3
5690 reflections(Δ/σ)max = 0.001
97 parametersΔρmax = 0.43 e Å3
0 restraintsΔρmin = 0.28 e Å3
Crystal data top
C6H2Cl4γ = 96.520 (2)°
Mr = 215.88V = 375.91 (9) Å3
Triclinic, P1Z = 2
a = 3.8016 (5) ÅMo Kα radiation
b = 10.6369 (15) ŵ = 1.48 mm1
c = 9.4866 (13) ÅT = 150 K
α = 92.072 (2)°0.11 × 0.08 × 0.04 mm
β = 98.966 (2)°
Data collection top
Bruker SMART APEX
diffractometer
5184 reflections with I > 2σ(I)
6306 measured reflectionsRint = 0.000
5690 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0350 restraints
wR(F2) = 0.099Riding model
S = 1.03Δρmax = 0.43 e Å3
5690 reflectionsΔρmin = 0.28 e Å3
97 parameters
Special details top

Experimental. It was evident, through the use of RLATT, that the crystal was twinned (non-merohedral). GEMINI was used to index the data and showed that there were two, approximately equal components. The output p4p files for each component were read back into SMART and run through the BRAVAIS and L·S. routines. The data were integrated twice (SAINT) using each orientation matrix and TWINHKL, within the GEMINI suite of programs was used to write HKLF 4 and HKLF 5 SHELX data files. The single-crystal structure was solved using direct methods using SHELXS97 on just a single component and all non-hydrogen atoms were located using subsequent difference-Fourier methods. However, the data completeness was only 80.4% so the HKLF 5 file was used (98.7). SADABS can not be performed in this situation since both programmes require the use of the raw files.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.0779 (3)0.46699 (11)0.36615 (13)0.0191 (3)
Cl10.17010 (9)0.42699 (3)0.19905 (3)0.02629 (10)
C20.0160 (3)0.37396 (11)0.46285 (13)0.0187 (3)
Cl20.04035 (9)0.21651 (3)0.41860 (3)0.02707 (10)
C30.0624 (3)0.59324 (11)0.40440 (13)0.0202 (3)
H3A0.10560.65690.33940.024*
C40.4342 (3)0.02926 (11)0.13591 (13)0.0193 (3)
Cl40.34762 (9)0.06363 (3)0.30447 (3)0.02507 (10)
C50.5161 (3)0.12245 (11)0.04347 (13)0.0187 (3)
Cl50.53680 (9)0.27600 (3)0.09527 (3)0.02577 (10)
C60.4184 (3)0.09367 (11)0.09192 (13)0.0203 (3)
H6A0.36290.15760.15460.024*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0169 (6)0.0250 (7)0.0158 (6)0.0025 (5)0.0042 (5)0.0019 (5)
Cl10.0337 (2)0.02838 (19)0.01834 (17)0.00325 (13)0.01025 (14)0.00256 (12)
C20.0172 (6)0.0181 (6)0.0209 (6)0.0038 (4)0.0023 (5)0.0016 (5)
Cl20.0366 (2)0.01932 (18)0.02724 (19)0.00532 (13)0.01054 (15)0.00138 (12)
C30.0203 (7)0.0209 (7)0.0195 (7)0.0014 (5)0.0034 (5)0.0031 (5)
C40.0171 (6)0.0255 (7)0.0154 (6)0.0008 (5)0.0043 (5)0.0016 (5)
Cl40.0328 (2)0.02663 (19)0.01774 (17)0.00383 (13)0.00967 (14)0.00261 (12)
C50.0172 (6)0.0192 (6)0.0195 (6)0.0019 (4)0.0022 (5)0.0021 (5)
Cl50.0341 (2)0.02090 (18)0.02395 (18)0.00593 (13)0.00723 (14)0.00349 (12)
C60.0178 (7)0.0237 (7)0.0194 (6)0.0038 (5)0.0032 (5)0.0028 (5)
Geometric parameters (Å, º) top
C1—C31.3885 (16)C4—C61.3918 (16)
C1—C21.3986 (17)C4—C51.3930 (17)
C1—Cl11.7249 (12)C4—Cl41.7257 (12)
C2—C3i1.3803 (17)C5—C6ii1.3843 (17)
C2—Cl21.7280 (12)C5—Cl51.7293 (12)
C3—C2i1.3803 (17)C6—C5ii1.3843 (17)
C3—H3A0.9500C6—H6A0.9500
C3—C1—C2119.72 (11)C6—C4—C5119.79 (11)
C3—C1—Cl1119.39 (9)C6—C4—Cl4119.06 (9)
C2—C1—Cl1120.89 (9)C5—C4—Cl4121.15 (9)
C3i—C2—C1120.44 (11)C6ii—C5—C4120.46 (11)
C3i—C2—Cl2119.02 (9)C6ii—C5—Cl5118.78 (9)
C1—C2—Cl2120.53 (10)C4—C5—Cl5120.75 (9)
C2i—C3—C1119.84 (11)C5ii—C6—C4119.74 (11)
C2i—C3—H3A120.1C5ii—C6—H6A120.1
C1—C3—H3A120.1C4—C6—H6A120.1
C3—C1—C2—C3i0.4 (2)C6—C4—C5—C6ii0.0 (2)
Cl1—C1—C2—C3i179.12 (10)Cl4—C4—C5—C6ii179.39 (10)
C3—C1—C2—Cl2179.04 (9)C6—C4—C5—Cl5179.90 (9)
Cl1—C1—C2—Cl21.45 (15)Cl4—C4—C5—Cl50.47 (15)
C2—C1—C3—C2i0.4 (2)C5—C4—C6—C5ii0.0 (2)
Cl1—C1—C3—C2i179.13 (10)Cl4—C4—C6—C5ii179.40 (10)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y, z.
(tcb_alpha_2K_neutron_powder) 1,2,4,5-tetrachlorobenzene top
Crystal data top
C6Cl4D2V = 367.78 (1) Å3
Mr = 217.88Z = 2
Triclinic, P1Cell parameters included in refinement
Hall symbol: P-1Neutron radiation, λ = ? Å
a = 3.76062 (4) ŵ = 0.05 mm1
b = 10.58794 (5) ÅT = 2 K
c = 9.44562 (3) ÅParticle morphology: Needle
α = 92.4066 (4)°Colourless
β = 98.6978 (6)°flat sheet, 20 × 5 mm
γ = 97.5893 (6)°
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Radiation source: Pulsed neutron sourceAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Specimen mounting: 5mm thick vanadium slab canTmin = ?, Tmax = ?
Data collection mode: transmission
Refinement top
Least-squares matrix: selected elements only58 parameters
Rp = 5.73422 restraints
Rwp = 6.7062 constraints
Rexp = 5.093Weighting scheme based on measured s.u.'s
χ2 = 1.734(Δ/σ)max = 0.001
13190 data pointsBackground function: Chebyshev polynomial
Excluded region(s): excluded short and long TOF regions <35000.0/ms and >118500.0/ms excluded detector bank1 <38000.0/ms and >112000.0/ms excluded detector bank2Preferred orientation correction: A Spherical harmonics correction of intensities for preferred orientation was applied according to Jarvinen (1993). The values for detector banks 1 and 2 are given below: sh_bank1_c00 1 sh_bank1_c20 0.93511 sh_bank1_c21p -0.02035 sh_bank1_c21m -0.05750 sh_bank1_c22p -0.96023 sh_bank1_c22m -0.05035 sh_bank1_c40 -0.01777 sh_bank1_c41p 0.00565 sh_bank1_c41m 0.06480 sh_bank1_c42p -0.58460 sh_bank1_c42m -0.01883 sh_bank1_c43p 0.02527 sh_bank1_c43m 0.05883 sh_bank1_c44p 0.34685 sh_bank1_c44m 0.03998
sh_bank2_c00 1 sh_bank2_c20 0.16065 sh_bank2_c21p -0.08458 sh_bank2_c21m 0.01061 sh_bank2_c22p -0.18564 sh_bank2_c22m -0.04873 sh_bank2_c40 0.06927 sh_bank2_c41p -0.02472 sh_bank2_c41m -0.05697 sh_bank2_c42p 0.32069 sh_bank2_c42m -0.01468 sh_bank2_c43p 0.02034 sh_bank2_c43m -0.01361 sh_bank2_c44p -0.14892 sh_bank2_c44m -0.03418
Profile function: Full Voigt with double exponetial
Crystal data top
C6Cl4D2γ = 97.5893 (6)°
Mr = 217.88V = 367.78 (1) Å3
Triclinic, P1Z = 2
a = 3.76062 (4) ÅNeutron radiation, λ = ? Å
b = 10.58794 (5) ŵ = 0.05 mm1
c = 9.44562 (3) ÅT = 2 K
α = 92.4066 (4)°flat sheet, 20 × 5 mm
β = 98.6978 (6)°
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Specimen mounting: 5mm thick vanadium slab canAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Data collection mode: transmissionTmin = ?, Tmax = ?
Refinement top
Rp = 5.73413190 data points
Rwp = 6.70658 parameters
Rexp = 5.09322 restraints
χ2 = 1.734
Special details top

Experimental. The data were collected on 2 detector banks and refined simultanously:

For simplicity the values given as cif data items all correspond to detector bank1 data. Where these values differ from those for bank2, the values for detector bank2 are given in _special_details text blocks.

Geometry. Bond distances, bond angles, torsion angles were calculated using PLATON (Spek, 2003; program version 280604)

Refinement. For detector bank2: _refine_ls_goodness_of_fit_all 1.150

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.0819 (6)0.46665 (11)0.36555 (11)0.49 (4)*
C20.0149 (6)0.37293 (17)0.46264 (13)0.49 (4)*
C30.0658 (8)0.59351 (18)0.40366 (12)0.49 (4)*
Cl10.1732 (6)0.42510 (12)0.19717 (13)0.64 (4)*
Cl20.0503 (6)0.21436 (13)0.42054 (14)0.64 (4)*
H30.1049 (9)0.66473 (18)0.32719 (16)1.30 (5)*
C40.4355 (6)0.02858 (11)0.13704 (11)0.49 (4)*
C50.5085 (7)0.12310 (17)0.04347 (13)0.49 (4)*
C60.4161 (8)0.09291 (18)0.09251 (12)0.49 (4)*
Cl40.3446 (6)0.06415 (12)0.30578 (13)0.64 (4)*
Cl50.5353 (6)0.27670 (13)0.09664 (14)0.64 (4)*
H60.3596 (9)0.16730 (17)0.16542 (19)1.30 (5)*
Geometric parameters (Å, º) top
Cl1—C11.728 (2)Cl4—C41.726 (2)
Cl2—C21.736 (2)Cl5—C51.733 (2)
C1—C21.403 (2)C4—C51.389 (2)
C1—C31.387 (2)C4—C61.378 (2)
C2—C3i1.386 (2)C5—C6ii1.398 (2)
C3—H31.077 (2)C6—H61.088 (3)
Cl1—C1—C2120.63 (11)Cl4—C4—C5120.47 (11)
Cl1—C1—C3119.63 (11)Cl4—C4—C6119.54 (12)
C2—C1—C3119.72 (13)C5—C4—C6119.91 (12)
Cl2—C2—C1120.70 (12)Cl5—C5—C4120.92 (11)
Cl2—C2—C3i118.87 (14)Cl5—C5—C6ii119.05 (15)
C1—C2—C3i120.37 (16)C4—C5—C6ii119.91 (16)
C1—C3—C2i119.90 (15)C4—C6—C5ii120.07 (17)
C1—C3—H3119.62 (17)C4—C6—H6120.19 (16)
H3—C3—C2i120.4 (2)H6—C6—C5ii119.62 (19)
Cl1—C1—C2—Cl24.1 (3)Cl4—C4—C5—Cl53.6 (3)
Cl1—C1—C2—C3i178.6 (2)Cl4—C4—C5—C6ii179.6 (2)
C3—C1—C2—Cl2177.5 (2)C6—C4—C5—Cl5179.9 (2)
C3—C1—C2—C3i0.2 (3)C6—C4—C5—C6ii3.9 (3)
Cl1—C1—C3—C2i178.6 (2)Cl4—C4—C6—C5ii179.6 (2)
C2—C1—C3—C2i0.2 (4)C5—C4—C6—C5ii3.9 (4)
Cl2—C2—C3i—C1i177.6 (2)Cl5—C5—C6ii—C4ii180.0 (2)
C1—C2—C3i—C1i0.2 (4)C4—C5—C6ii—C4ii3.9 (4)
Cl1—C1—C3—H31.3 (4)Cl4—C4—C6—H63.6 (4)
C2—C1—C3—H3177.1 (3)C5—C4—C6—H6179.9 (3)
Cl2—C2—C3i—H3i0.2 (4)Cl5—C5—C6ii—H6ii4.0 (4)
C1—C2—C3i—H3i177.1 (3)C4—C5—C6ii—H6ii179.9 (3)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y, z.
(tcb_alpha_150K_neutron) 1,2,4,5-tetrachlorobenzene top
Crystal data top
C6Cl4D2V = 375.13 (1) Å3
Mr = 217.88Z = 2
Triclinic, P1Cell parameters included in refinement
a = 3.7990 (1) ÅNeutron radiation, λ = ? Å
b = 10.6258 (1) ŵ = 0.51 mm1
c = 9.47938 (7) ÅT = 150 K
α = 91.9780 (9)°Particle morphology: Needle
β = 99.058 (2)°Colourless
γ = 96.234 (2)°flat sheet, 20 × 5 mm
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Radiation source: Pulsed neutron sourceAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Specimen mounting: 5mm thick vanadium slab canTmin = ?, Tmax = ?
Data collection mode: transmission
Refinement top
Least-squares matrix: selected elements only27 parameters
Rp = 3.90211 restraints
Rwp = 4.59974 constraints
Rexp = 3.473Weighting scheme based on measured s.u.'s
χ2 = 1.753(Δ/σ)max = 0.001
13321 data pointsBackground function: Chebyshev polynomial
Excluded region(s): excluded short and long TOF regions <35000.0/ms and >118500.0/ms excluded detector bank1 <38000.0/ms and >112000.0/ms excluded detector bank2Preferred orientation correction: A Spherical harmonics correction of intensities for preferred orientation was applied according to Jarvinen (1993). The values for detector banks 1 and 2 are given below: sh_bank1A_c00 1 sh_bank1A_c20 0.99392 sh_bank1A_c21p -0.15008 sh_bank1A_c21m 0.01363 sh_bank1A_c22p -0.98430 sh_bank1A_c22m -0.04091 sh_bank1A_c40 0.12805 sh_bank1A_c41p -0.00510 sh_bank1A_c41m 0.09046 sh_bank1A_c42p -0.71077 sh_bank1A_c42m -0.00005 sh_bank1A_c43p 0.02703 sh_bank1A_c43m 0.08732 sh_bank1A_c44p 0.42495 sh_bank1A_c44m 0.01521
sh_bank2A_c00 1 sh_bank2A_c20 0.13922 sh_bank2A_c21p -0.27165 sh_bank2A_c21m 0.06322 sh_bank2A_c22p -0.15558 sh_bank2A_c22m -0.04354 sh_bank2A_c40 0.04018 sh_bank2A_c41p -0.04492 sh_bank2A_c41m -0.06239 sh_bank2A_c42p 0.23357 sh_bank2A_c42m -0.03792 sh_bank2A_c43p 0.02061 sh_bank2A_c43m 0.02549 sh_bank2A_c44p -0.14546 sh_bank2A_c44m 0.15963
Profile function: Full Voigt with double exponetial
Crystal data top
C6Cl4D2γ = 96.234 (2)°
Mr = 217.88V = 375.13 (1) Å3
Triclinic, P1Z = 2
a = 3.7990 (1) ÅNeutron radiation, λ = ? Å
b = 10.6258 (1) ŵ = 0.51 mm1
c = 9.47938 (7) ÅT = 150 K
α = 91.9780 (9)°flat sheet, 20 × 5 mm
β = 99.058 (2)°
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Specimen mounting: 5mm thick vanadium slab canAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Data collection mode: transmissionTmin = ?, Tmax = ?
Refinement top
Rp = 3.90213321 data points
Rwp = 4.59927 parameters
Rexp = 3.47311 restraints
χ2 = 1.753
Special details top

Experimental. The data were collected on 2 detector banks and refined simultanously:

For simplicity, the values given as cif data items all correspond to detector bank1 data. Where these values differ from those for bank2, the values for detector bank2 are given in _special_details text blocks.

Geometry. Bond distances, bond angles, torsion angles and H-bond geometries were calculated using PLATON (Spek, 2003; program version 280604). A freely rotating z-matrix model has been used to constrain the atomic parameters to geometrically idealized positions.

Refinement. This is a mixed phase data set with contributions from both alpha and beta tetrachlorobenzene. Both phases were refined simultaneously, the information in this data block relates to the alpha phase.

The refined ratio of alpha to beta = 31.0 (2):69.0 (2)

A freely rotating z-matrix model was used to constrain the atomic parameters to geometrically idealized positions.

For detector bank2: _refine_ls_goodness_of_fit_all 1.193

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.0761950.4661580.3660551.88 (5)*0.5
C20.0128270.3733220.4617071.88 (5)*0.5
C30.0633680.5928360.4043481.88 (5)*0.5
Cl10.1708640.4241110.1996352.29 (6)*0.5
Cl20.0287640.2159300.4141302.29 (6)*0.5
H30.1131050.6657030.3292722.73 (12)*0.5
C1i0.0761950.5338420.6339451.88 (5)*0.5
C2i0.0128270.6266780.5382931.88 (5)*0.5
C3i0.0633680.4071640.5956521.88 (5)*0.5
Cl1i0.1708640.5758890.8003652.29 (6)*0.5
Cl2i0.0287640.7840700.5858712.29 (6)*0.5
H3i0.1131050.3342970.6707282.73 (12)*0.5
C40.4292000.0303740.1349951.88 (5)*0.5
C50.5157840.1231220.0435481.88 (5)*0.5
C60.4134170.0927480.0914471.88 (5)*0.5
Cl40.3412360.0681130.3027192.29 (6)*0.5
Cl50.5353940.2760950.0976542.29 (6)*0.5
H60.3454580.1655450.1632232.73 (12)*0.5
C4j0.5708000.0303740.1349951.88 (5)*0.5
C5j0.4842160.1231220.0435481.88 (5)*0.5
C6j0.5865830.0927480.0914471.88 (5)*0.5
Cl4j0.6587640.0681130.3027192.29 (6)*0.5
Cl5j0.4646060.2760950.0976542.29 (6)*0.5
H6j0.6545420.1655450.1632232.73 (12)*0.5
Geometric parameters (Å, º) top
Cl1—C11.7270C3i—H3i1.09
Cl1i—C1i1.7270Cl4—C41.7270
Cl2—C21.7270Cl4j—C4j1.7270
Cl2i—C2i1.7270Cl5—C51.7270
C1—C21.3900Cl5j—C5j1.7270
C1—C31.3900C4—C51.3900
C1i—C2i1.3900C4—C61.3900
C1i—C3i1.3900C4j—C5j1.3900
C2—C3i1.3900C4j—C6j1.3900
C2i—C31.3900C5—C6j1.3900
C3—H31.09C5j—C61.3900
Cl1—C1—C2120.00Cl4—C4—C5120.00
Cl1—C1—C3120.00Cl4—C4—C6120.00
C2—C1—C3120.00C5—C4—C6120.00
Cl1i—C1i—C2i120.00Cl4j—C4j—C5j120.00
Cl1i—C1i—C3i120.00Cl4j—C4j—C6j120.00
C2i—C1i—C3i120.00C5j—C4j—C6j120.00
Cl2—C2—C1120.00Cl5—C5—C4120.00
Cl2—C2—C3i120.00Cl5—C5—C6j120.00
C1—C2—C3i120.00C4—C5—C6j120.00
Cl2i—C2i—C1i120.00Cl5j—C5j—C4j120.00
Cl2i—C2i—C3120.00Cl5j—C5j—C6120.00
C1i—C2i—C3120.00C4j—C5j—C6120.00
C1—C3—C2i120.00C4—C6—C5j120.00
C1i—C3i—C2120.00C4j—C6j—C5120.00
C1—C3—H3120.00C4—C6—H6120.00
C2i—C3—H3120.00C5j—C6—H6120.00
C1i—C3i—H3i120.00C4j—C6j—H6j120.00
C2—C3i—H3i120.00C5—C6j—H6j120.00
Cl1—C1—C2—Cl20.00Cl4—C4—C5—Cl50.02
Cl1—C1—C2—C3i179.98Cl4—C4—C5—C6j179.98
C3—C1—C2—Cl2180.00C6—C4—C5—Cl5180.00
C3—C1—C2—C3i0.00C6—C4—C5—C6j0.00
Cl1—C1—C3—C2i179.98Cl4—C4—C6—C5j180.00
C2—C1—C3—C2i0.00C5—C4—C6—C5j0.00
Cl1i—C1i—C2i—Cl2i0.02Cl4j—C4j—C5j—Cl5j0.00
Cl1i—C1i—C2i—C3180.00Cl4j—C4j—C5j—C6180.00
C3i—C1i—C2i—Cl2i180.00C6j—C4j—C5j—Cl5j180.00
C3i—C1i—C2i—C30.00C6j—C4j—C5j—C60.00
Cl1i—C1i—C3i—C2179.98Cl4j—C4j—C6j—C5180.00
C2i—C1i—C3i—C20.00C5j—C4j—C6j—C50.00
Cl2—C2—C3i—C1i180.00Cl5—C5—C6j—C4j180.00
C1—C2—C3i—C1i0.00C4—C5—C6j—C4j0.00
Cl2i—C2i—C3—C1180.00Cl5j—C5j—C6—C4180.00
C1i—C2i—C3—C10.02C4j—C5j—C6—C40.00
Cl1—C1—C3—H30.00Cl4—C4—C6—H60.00
C2—C1—C3—H3180.00C5—C4—C6—H6180.00
Cl1i—C1i—C3i—H3i0.00Cl4j—C4j—C6j—H6j0.00
C2i—C1i—C3i—H3i180.00C5j—C4j—C6j—H6j180.00
Cl2—C2—C3i—H3i0.00Cl5—C5—C6j—H6j0.00
C1—C2—C3i—H3i180.00C4—C5—C6j—H6j180.00
Cl2i—C2i—C3—H30.00Cl5j—C5j—C6—H60.00
C1i—C2i—C3—H3180.00C4j—C5j—C6—H6180.00
(tcb_beta_150K_neutron) 1,2,4,5-tetrachlorobenzene top
Crystal data top
C6Cl4D2Z = 2
Mr = 217.88Cell parameters included in refinement
Monoclinic, P21/nNeutron radiation, λ = ? Å
a = 3.78988 (4) ŵ = 0.51 mm1
b = 10.50328 (5) ÅT = 150 K
c = 9.56244 (3) ÅParticle morphology: Needle
β = 99.7184 (6)°Colourless
V = 375.18 (1) Å3flat sheet, 20 × 5 mm
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Radiation source: Pulsed neutron sourceAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Specimen mounting: 5mm thick vanadium slab canTmin = ?, Tmax = ?
Data collection mode: transmission
Refinement top
Least-squares matrix: selected elements only37 parameters
Rp = 3.90211 restraints
Rwp = 4.5992 constraints
Rexp = 3.473Weighting scheme based on measured s.u.'s
χ2 = 1.753(Δ/σ)max = 0.001
13321 data pointsBackground function: Chebyshev polynomial
Excluded region(s): excluded short and long TOF regions <35000.0/ms and >118500.0/ms excluded detector bank1 <38000.0/ms and >112000.0/ms excluded detector bank2Preferred orientation correction: A Spherical harmonics correction of intensities for preferred orientation was applied according to Jarvinen (1993). The values for detector banks 1 and 2 are given below: sh_bank1B_c00 1.0 sh_bank1B_c20 -1.73091 sh_bank1B_c22p 0.03352 sh_bank1B_c22m -0.03672 sh_bank1B_c40 1.11655 sh_bank1B_c42p -0.03514 sh_bank1B_c42m 0.31755 sh_bank1B_c44p -0.50088 sh_bank1B_c44m -0.37093 sh_bank1B_c60 -0.04523 sh_bank1B_c62p -0.00397 sh_bank1B_c62m -0.07907 sh_bank1B_c64p 0.33570 sh_bank1B_c64m 0.03907 sh_bank1B_c66p -0.09855 sh_bank1B_c66m -0.09855
sh_bank2B_c00 1.0 sh_bank2B_c20 -0.46561 sh_bank2B_c22p 0.06283 sh_bank2B_c22m 0.08408 sh_bank2B_c40 -0.22025 sh_bank2B_c42p 0.01598 sh_bank2B_c42m 0.30682 sh_bank2B_c44p 0.28186 sh_bank2B_c44m -0.20096 sh_bank2B_c60 -0.00143 sh_bank2B_c62p 0.12395 sh_bank2B_c62m 0.08929 sh_bank2B_c64p 0.09454 sh_bank2B_c64m -0.04423 sh_bank2B_c66p -0.02742 sh_bank2B_c66m -0.02742
Profile function: Full Voigt with double exponetial
Crystal data top
C6Cl4D2V = 375.18 (1) Å3
Mr = 217.88Z = 2
Monoclinic, P21/nNeutron radiation, λ = ? Å
a = 3.78988 (4) ŵ = 0.51 mm1
b = 10.50328 (5) ÅT = 150 K
c = 9.56244 (3) Åflat sheet, 20 × 5 mm
β = 99.7184 (6)°
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Specimen mounting: 5mm thick vanadium slab canAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Data collection mode: transmissionTmin = ?, Tmax = ?
Refinement top
Rp = 3.90213321 data points
Rwp = 4.59937 parameters
Rexp = 3.47311 restraints
χ2 = 1.753
Special details top

Experimental. The data were collected on 2 detector banks and refined simultanously:

For simplicity, the values given as cif data items all correspond to detector bank1 data. Where these values differ from those for bank2, the values for detector bank2 are given in _special_details text blocks.

Geometry. Bond distances, bond angles, torsion angles and H-bond geometries were calculated using PLATON (Spek, 2003; program version 280604)

Refinement. This is a mixed phase data set with contributions from both alpha and beta tetrachlorobenzene. Both phases were refined simultaneously, the information in this data block relates to the alpha phase.

The refined ratio of alpha to beta = 31.0 (2):69.0 (2)

For detector bank2: _refine_ls_goodness_of_fit_all 1.193

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C1b0.0694 (4)0.46706 (9)0.36565 (8)1.73 (2)*
C2b0.0187 (5)0.37303 (12)0.45853 (8)1.73 (2)*
C3b0.0952 (5)0.59312 (13)0.40974 (8)1.73 (2)*
Cl1b0.1517 (5)0.42866 (10)0.19978 (10)2.33 (2)*
Cl2b0.0446 (5)0.21599 (11)0.40673 (10)2.33 (2)*
H1b0.1536 (6)0.66714 (12)0.33803 (13)2.83 (5)*
Geometric parameters (Å, º) top
Cl1b—C1b1.7154 (14)C1b—C3b1.3880 (16)
Cl2b—C2b1.7202 (17)C2b—C3bi1.3858 (14)
C1b—C2b1.4056 (15)C3b—H1b1.0839 (19)
Cl1b—C1b—C2b121.24 (8)C1b—C2b—C3bi120.17 (11)
Cl1b—C1b—C3b119.38 (9)C1b—C3b—C2bi120.40 (11)
C2b—C1b—C3b119.37 (9)C1b—C3b—H1b120.23 (11)
Cl2b—C2b—C1b119.99 (8)H1b—C3b—C2bi119.17 (14)
Cl2b—C2b—C3bi119.82 (11)
Cl1b—C1b—C2b—Cl2b0.2 (2)Cl2b—C2b—C3bi—C1bi178.90 (14)
Cl1b—C1b—C2b—C3bi177.94 (15)C1b—C2b—C3bi—C1bi3.0 (3)
C3b—C1b—C2b—Cl2b178.93 (15)Cl1b—C1b—C3b—H1b3.1 (3)
C3b—C1b—C2b—C3bi3.0 (2)C2b—C1b—C3b—H1b177.8 (2)
Cl1b—C1b—C3b—C2bi177.91 (15)Cl2b—C2b—C3bi—H1bi4.0 (3)
C2b—C1b—C3b—C2bi3.0 (2)C1b—C2b—C3bi—H1bi177.9 (2)
Symmetry code: (i) x, y+1, z+1.
(tcb_beta_200K_neutron) 1,2,4,5-tetrachlorobenzene top
Crystal data top
C6Cl4D2Z = 2
Mr = 217.88Cell parameters included in refinement
Monoclinic, P21/nNeutron radiation, λ = ? Å
a = 3.81117 (4) ŵ = 0.51 mm1
b = 10.53867 (4) ÅT = 200 K
c = 9.57198 (3) ÅParticle morphology: Needle
β = 99.7088 (5)°Colourless
V = 378.95 (1) Å3flat sheet, 20 × 5 mm
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Radiation source: Pulsed neutron sourceAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Specimen mounting: 5mm thick vanadium slab canTmin = ?, Tmax = ?
Data collection mode: transmission
Refinement top
Least-squares matrix: selected elements only38 parameters
Rp = 4.52411 restraints
Rwp = 5.2532 constraints
Rexp = 4.166Weighting scheme based on measured s.u.'s
χ2 = 1.590(Δ/σ)max = 0.001
13154 data pointsBackground function: Chebyshev polynomial
Excluded region(s): excluded short and long TOF regions <34000.0/ms and >118500.0/ms excluded detector bank1 <38000.0/ms and >112000.0/ms excluded detector bank2Preferred orientation correction: A Spherical harmonics correction of intensities for preferred orientation was applied according to Jarvinen (1993). Since the preferred orientation should not change with temperture or time Spherical_Harmonics correction was refined against the 295 and 200K data simultaniously. The values for detector banks 1 and 2 are given below: sh_bank2_c00 1.0 sh_bank2_c20 -0.43133 sh_bank2_c22p 0.10625 sh_bank2_c22m 0.10944 sh_bank2_c40 -0.38252 sh_bank2_c42p 0.01095 sh_bank2_c42m 0.20350 sh_bank2_c44p 0.32761 sh_bank2_c44m -0.27992 sh_bank2_c60 0.00414 sh_bank2_c62p 0.12097 sh_bank2_c62m 0.13430 sh_bank2_c64p 0.04673 sh_bank2_c64m -0.05007 sh_bank2_c66p -0.06163 sh_bank2_c66m -0.06163
sh_bank1_c00 1.0 sh_bank1_c20 -1.90462 sh_bank1_c22p 0.18262 sh_bank1_c22m -0.11960 sh_bank1_c40 1.49040 sh_bank1_c42p -0.07359 sh_bank1_c42m 0.50678 sh_bank1_c44p -0.56228 sh_bank1_c44m -0.63237 sh_bank1_c60 -0.05871 sh_bank1_c62p 0.04756 sh_bank1_c62m -0.19668 sh_bank1_c64p 0.42608 sh_bank1_c64m 0.08896 sh_bank1_c66p -0.13523 sh_bank1_c66m -0.13523
Profile function: Full Voigt with double exponetial
Crystal data top
C6Cl4D2V = 378.95 (1) Å3
Mr = 217.88Z = 2
Monoclinic, P21/nNeutron radiation, λ = ? Å
a = 3.81117 (4) ŵ = 0.51 mm1
b = 10.53867 (4) ÅT = 200 K
c = 9.57198 (3) Åflat sheet, 20 × 5 mm
β = 99.7088 (5)°
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Specimen mounting: 5mm thick vanadium slab canAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Data collection mode: transmissionTmin = ?, Tmax = ?
Refinement top
Rp = 4.52413154 data points
Rwp = 5.25338 parameters
Rexp = 4.16611 restraints
χ2 = 1.590
Special details top

Experimental. The data were collected on 2 detector banks and refined simultanously:

For simplicity, the values given as cif data items all correspond to detector bank1 data. Where these values differ from those for bank2, the values for detector bank2 are given in _special_details text blocks.

Geometry. Bond distances, bond angles, torsion angles and H-bond geometries were calculated using PLATON (Spek, 2003; program version 280604)

Refinement. For detector bank2: _refine_ls_goodness_of_fit_all 1.208

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.0651 (4)0.46742 (9)0.36540 (7)2.36 (4)*
C20.0139 (5)0.37337 (11)0.45843 (9)2.36 (4)*
C30.0861 (5)0.59328 (13)0.40957 (9)2.36 (4)*
Cl10.1523 (4)0.42918 (9)0.20027 (10)3.11 (4)*
Cl20.0422 (4)0.21672 (10)0.40643 (9)3.11 (4)*
H10.1512 (6)0.66550 (13)0.33866 (14)3.48 (5)*
Geometric parameters (Å, º) top
Cl1—C11.7171 (13)C1—C31.3904 (16)
Cl2—C21.7224 (15)C2—C3i1.3831 (15)
C1—C21.3987 (15)C3—H11.076 (2)
Cl1—C1—C2121.04 (8)C1—C2—C3i119.93 (11)
Cl1—C1—C3119.58 (8)C1—C3—C2i120.67 (11)
C2—C1—C3119.34 (8)C1—C3—H1119.37 (12)
Cl2—C2—C1120.33 (8)H1—C3—C2i119.93 (14)
Cl2—C2—C3i119.68 (10)
Cl1—C1—C2—Cl22.5 (2)Cl2—C2—C3i—C1i179.97 (14)
Cl1—C1—C2—C3i179.46 (14)C1—C2—C3i—C1i3.0 (3)
C3—C1—C2—Cl2179.91 (13)Cl1—C1—C3—H11.4 (3)
C3—C1—C2—C3i2.9 (2)C2—C1—C3—H1179.0 (2)
Cl1—C1—C3—C2i179.40 (15)Cl2—C2—C3i—H1i2.0 (3)
C2—C1—C3—C2i3.0 (2)C1—C2—C3i—H1i179.0 (2)
Symmetry code: (i) x, y+1, z+1.
(tcb_beta_295K_neutron) 1,2,4,5-tetrachlorobenzene top
Crystal data top
C6Cl4D2Z = 2
Mr = 217.88Cell parameters included in refinement
Monoclinic, P21/nNeutron radiation, λ = ? Å
a = 3.85595 (5) ŵ = 0.51 mm1
b = 10.61473 (6) ÅT = 295 K
c = 9.59283 (4) ÅParticle morphology: Needle
β = 99.6884 (7)°Colourless
V = 387.03 (1) Å3flat sheet, 20 × 5 mm
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Radiation source: Pulsed neutron sourceAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Specimen mounting: 5mm thick vanadium slab canTmin = ?, Tmax = ?
Data collection mode: transmission
Refinement top
Least-squares matrix: selected elements only38 parameters
Rp = 4.31511 restraints
Rwp = 5.0502 constraints
Rexp = 4.138Weighting scheme based on measured s.u.'s
χ2 = 1.488(Δ/σ)max = 0.001
13194 data pointsBackground function: Chebyshev polynomial
Excluded region(s): excluded short and long TOF regions <35000.0/ms and >118500.0/ms excluded detector bank1 <38000.0/ms and >112000.0/ms excluded detector bank2Preferred orientation correction: A Spherical harmonics correction of intensities for preferred orientation was applied according to Jarvinen (1993). Since the preferred orientation should not change with temperture or time Spherical_Harmonics correction was refined against the 295 and 200K data simultaniously. The values for detector banks 1 and 2 are given below: sh_bank1_c00 1.0 sh_bank1_c20 -1.90462 sh_bank1_c22p 0.18262 sh_bank1_c22m -0.11960 sh_bank1_c40 1.49040 sh_bank1_c42p -0.07359 sh_bank1_c42m 0.50678 sh_bank1_c44p -0.56228 sh_bank1_c44m -0.63237 sh_bank1_c60 -0.05871 sh_bank1_c62p 0.04756 sh_bank1_c62m -0.19668 sh_bank1_c64p 0.42608 sh_bank1_c64m 0.08896 sh_bank1_c66p -0.13523 sh_bank1_c66m -0.13523
sh_bank2_c00 1.0 sh_bank2_c20 -0.43133 sh_bank2_c22p 0.10625 sh_bank2_c22m 0.10944 sh_bank2_c40 -0.38252 sh_bank2_c42p 0.01095 sh_bank2_c42m 0.20350 sh_bank2_c44p 0.32761 sh_bank2_c44m -0.27992 sh_bank2_c60 0.00414 sh_bank2_c62p 0.12097 sh_bank2_c62m 0.13430 sh_bank2_c64p 0.04673 sh_bank2_c64m -0.05007 sh_bank2_c66p -0.06163 sh_bank2_c66m -0.06163
Profile function: Full Voigt with double exponetial
Crystal data top
C6Cl4D2V = 387.03 (1) Å3
Mr = 217.88Z = 2
Monoclinic, P21/nNeutron radiation, λ = ? Å
a = 3.85595 (5) ŵ = 0.51 mm1
b = 10.61473 (6) ÅT = 295 K
c = 9.59283 (4) Åflat sheet, 20 × 5 mm
β = 99.6884 (7)°
Data collection top
HRPD, ISIS
diffractometer
Scan method: Time-of-flight
Specimen mounting: 5mm thick vanadium slab canAbsorption correction: empirical (using intensity measurements)
Mu = 0.51cm-1 at 1.8A calculated using custom ISIS software program Arial Mucalc
Data collection mode: transmissionTmin = ?, Tmax = ?
Refinement top
Rp = 4.31513194 data points
Rwp = 5.05038 parameters
Rexp = 4.13811 restraints
χ2 = 1.488
Special details top

Experimental. The data were collected on 2 detector banks and refined simultanously:

For simplicity the values given as cif data items all correspond to detector bank1 data. Where these values differ from those for bank2, the values for detector bank2 are given in _special_details text blocks.

Geometry. Bond distances, bond angles, torsion angles and H-bond geometries were calculated using PLATON (Spek, 2003; program version 280604)

Refinement. For detector bank2: _refine_ls_goodness_of_fit_all 1.138

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.0636 (4)0.46829 (10)0.36605 (9)3.78 (5)*
C20.0104 (6)0.37410 (14)0.45951 (10)3.78 (5)*
C30.0843 (6)0.59205 (17)0.41025 (10)3.78 (5)*
Cl10.1550 (6)0.43026 (11)0.20164 (13)5.03 (5)*
Cl20.0356 (6)0.21879 (13)0.40684 (12)5.03 (5)*
H30.1429 (7)0.66426 (18)0.3400 (2)5.56 (7)*
Geometric parameters (Å, º) top
Cl1—C11.721 (2)C1—C31.379 (2)
Cl2—C21.722 (2)C2—C3i1.375 (2)
C1—C21.404 (2)C3—H31.070 (3)
Cl1—C1—C2120.88 (10)C1—C2—C3i119.31 (13)
Cl1—C1—C3119.68 (10)C1—C3—C2i121.22 (14)
C2—C1—C3119.32 (10)C1—C3—H3119.77 (15)
Cl2—C2—C1120.12 (10)H3—C3—C2i118.90 (19)
Cl2—C2—C3i120.44 (13)
Cl1—C1—C2—Cl23.7 (3)Cl2—C2—C3i—C1i179.64 (16)
Cl1—C1—C2—C3i179.63 (17)C1—C2—C3i—C1i4.5 (3)
C3—C1—C2—Cl2179.72 (16)Cl1—C1—C3—H33.4 (3)
C3—C1—C2—C3i4.4 (3)C2—C1—C3—H3179.4 (2)
Cl1—C1—C3—C2i179.49 (17)Cl2—C2—C3i—H3i3.5 (3)
C2—C1—C3—C2i4.5 (3)C1—C2—C3i—H3i179.4 (2)
Symmetry code: (i) x, y+1, z+1.

Experimental details

(tcb_alpha_150K_X-ray)(tcb_alpha_2K_neutron_powder)(tcb_alpha_150K_neutron)(tcb_beta_150K_neutron)
Crystal data
Chemical formulaC6H2Cl4C6Cl4D2C6Cl4D2C6Cl4D2
Mr215.88217.88217.88217.88
Crystal system, space groupTriclinic, P1Triclinic, P1Triclinic, P1Monoclinic, P21/n
Temperature (K)1502150150
a, b, c (Å)3.8016 (5), 10.6369 (15), 9.4866 (13)3.76062 (4), 10.58794 (5), 9.44562 (3)3.7990 (1), 10.6258 (1), 9.47938 (7)3.78988 (4), 10.50328 (5), 9.56244 (3)
α, β, γ (°)92.072 (2), 98.966 (2), 96.520 (2)92.4066 (4), 98.6978 (6), 97.5893 (6)91.9780 (9), 99.058 (2), 96.234 (2)90, 99.7184 (6), 90
V3)375.91 (9)367.78 (1)375.13 (1)375.18 (1)
Z2222
Radiation typeMo KαNeutron, λ = ? ÅNeutron, λ = ? ÅNeutron, λ = ? Å
µ (mm1)1.480.050.510.51
Specimen shape, size (mm)0.11 × 0.08 × 0.04Flat sheet, 20 × 5Flat sheet, 20 × 5Flat sheet, 20 × 5
Data collection
DiffractometerBruker SMART APEX
diffractometer
HRPD, ISIS
diffractometer
HRPD, ISIS
diffractometer
HRPD, ISIS
diffractometer
Specimen mounting5mm thick vanadium slab can5mm thick vanadium slab can5mm thick vanadium slab can
Data collection modeTransmissionTransmissionTransmission
Data collection methodω rotation with narrow frames scansTime-of-flightTime-of-flightTime-of-flight
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
6306, 5690, 5184
Rint0.000
θ values (°)θmax = 28.3, θmin = 1.92θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?
(sin θ/λ)max1)0.666
Refinement
R factors and goodness of fitR[F2 > 2σ(F2)] = 0.035, wR(F2) = 0.099, S = 1.03Rp = 5.734, Rwp = 6.706, Rexp = 5.093, χ2 = 1.734Rp = 3.902, Rwp = 4.599, Rexp = 3.473, χ2 = 1.753Rp = 3.902, Rwp = 4.599, Rexp = 3.473, χ2 = 1.753
No. of reflections/data points5690131901332113321
No. of parameters97582737
No. of restraints0221111
H-atom treatmentRiding model
Δρmax, Δρmin (e Å3)0.43, 0.28


(tcb_beta_200K_neutron)(tcb_beta_295K_neutron)
Crystal data
Chemical formulaC6Cl4D2C6Cl4D2
Mr217.88217.88
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)200295
a, b, c (Å)3.81117 (4), 10.53867 (4), 9.57198 (3)3.85595 (5), 10.61473 (6), 9.59283 (4)
α, β, γ (°)90, 99.7088 (5), 9090, 99.6884 (7), 90
V3)378.95 (1)387.03 (1)
Z22
Radiation typeNeutron, λ = ? ÅNeutron, λ = ? Å
µ (mm1)0.510.51
Specimen shape, size (mm)Flat sheet, 20 × 5Flat sheet, 20 × 5
Data collection
DiffractometerHRPD, ISIS
diffractometer
HRPD, ISIS
diffractometer
Specimen mounting5mm thick vanadium slab can5mm thick vanadium slab can
Data collection modeTransmissionTransmission
Data collection methodTime-of-flightTime-of-flight
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
Rint
θ values (°)2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?
(sin θ/λ)max1)
Refinement
R factors and goodness of fitRp = 4.524, Rwp = 5.253, Rexp = 4.166, χ2 = 1.590Rp = 4.315, Rwp = 5.050, Rexp = 4.138, χ2 = 1.488
No. of reflections/data points1315413194
No. of parameters3838
No. of restraints1111
H-atom treatment
Δρmax, Δρmin (e Å3)

Computer programs: Bruker SMART, custom ISIS software, Bruker SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), Topas v3.1 (Coehlo, 2003), Bruker SHELXTL and local programs.

 

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