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The low-temperature structure of hexamethylbenzene has been determined from neutron powder diffraction data and found to differ from the room-temperature phase predominantly by a translation of molecular planes to a form a cubic close-packed type structure. By performing measurements as a function of temperature, the role of thermally induced agitation of the molecular units in the first-order phase transition is clearly demonstrated.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104034007/lc5016sup1.cif
Contains datablocks HMB_5_publ, HMB_80_REDO_publ, HMB_100_REDO_publ, HMB_125_REDO_publ, HMB_129_REDO_publ, HMB_132_REDO_publ, HMB_publ

CCDC references: 205339; 268162; 268163; 268164; 268165; 268166; 268167

Computing details top

For all compounds, program(s) used to refine structure: GSAS.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(HMB_5_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6γ = 90.239 (7)°
Mr = 180.38V = 237.15 (1) Å3
Triclinic, P1Z = 1
a = 6.1803 (5) ÅMonchromatic beam radiation, λ = 1.594 Å
b = 6.1898 (6) ÅT = 5K K
c = 6.1993 (5) Åwhite
α = 90.041 (9)°?, ? × ? × ? mm
β = 90.129 (9)°
Data collection top
Radiation source: nuclear reactor2θmin = 0.437°, 2θmax = 162.837°, 2θstep = 0.05°
Refinement top
Least-squares matrix: fullExcluded region(s): 150.5° < 2θ < 154°
Rp = 0.066Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 200.080 #2(GV) = -0.100 #3(GW) = 136.977 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 9.1738 #8(shft) = -26.2722 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.09010 parameters
Rexp = 0.0230 restraints
R(F2) = 0.09220(Δ/σ)max = 5.80
χ2 = 15.210Background function: GSAS Background function number 1 with 6 terms. Shifted Chebyshev function of 1st kind 1: 211.141 2: 5.50416 3: 2.18815 4: 2.60253 5: 0.389629 6: 1.62396
3249 data points
Crystal data top
C6(CD3)6β = 90.129 (9)°
Mr = 180.38γ = 90.239 (7)°
Triclinic, P1V = 237.15 (1) Å3
a = 6.1803 (5) ÅZ = 1
b = 6.1898 (6) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.1993 (5) ÅT = 5K K
α = 90.041 (9)°?, ? × ? × ? mm
Data collection top
2θmin = 0.437°, 2θmax = 162.837°, 2θstep = 0.05°
Refinement top
Rp = 0.0663249 data points
Rwp = 0.09010 parameters
Rexp = 0.0230 restraints
R(F2) = 0.09220(Δ/σ)max = 5.80
χ2 = 15.210
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.433260.382780.681510.00871*
C20.616820.320330.563590.0062*
C30.682920.438160.380740.00682*
C40.356370.250710.873030.00516*
C50.751840.131060.640310.00804*
C60.876070.355840.248910.00502*
D70.1860.260930.895570.02554*
D80.424720.304811.022280.0321*
D90.3980.08860.850710.01524*
D100.742290.100250.80930.02213*
D110.91960.156690.608150.0188*
D120.7110.007790.549840.02646*
D131.02640.42440.30590.02564*
D140.856210.402710.080780.02341*
D150.884950.178020.250390.01691*
Geometric parameters (Å, º) top
C1—C21.4063 (1)D8—C41.0693 (1)
C1—C3i1.3781 (1)D8—D71.6908 (2)
C1—C41.5180 (2)D8—D91.7161 (2)
C2—C11.4063 (1)D9—C41.0461 (1)
C2—C31.4088 (1)D9—D71.7160 (2)
C2—C51.5173 (2)D9—D81.7161 (2)
C3—C1i1.3781 (1)D10—C51.0667 (1)
C3—C21.4088 (1)D10—D111.6975 (2)
C3—C61.5367 (2)D10—D121.7515 (2)
C4—C11.5180 (2)D11—C51.0675 (1)
C4—D71.0646 (1)D11—D101.6975 (2)
C4—D81.0693 (1)D11—D121.6780 (2)
C4—D91.0461 (1)D12—C51.0554 (1)
C5—C21.5173 (2)D12—D101.7515 (2)
C5—D101.0667 (1)D12—D111.6780 (2)
C5—D111.0675 (1)D13—C61.0785 (1)
C5—D121.0554 (1)D13—D141.7504 (2)
C6—C31.5367 (2)D13—D151.7875 (2)
C6—D131.0785 (1)D14—C61.0889 (1)
C6—D141.0889 (1)D14—D131.7504 (2)
C6—D151.1023 (1)D14—D151.7535 (2)
D7—C41.0646 (1)D15—C61.1023 (1)
D7—D81.6908 (2)D15—D131.7875 (2)
D7—D91.7160 (2)D15—D141.7535 (2)
C2—C1—C3i119.937 (6)D8—C4—D9108.429 (8)
C2—C1—C4120.760 (7)C2—C5—D10114.523 (8)
C3i—C1—C4119.271 (7)C2—C5—D11111.290 (7)
C1—C2—C3120.684 (7)C2—C5—D12109.422 (8)
C1—C2—C5119.739 (6)D10—C5—D11105.380 (9)
C3—C2—C5119.504 (7)D10—C5—D12111.257 (8)
C1i—C3—C2119.378 (7)D11—C5—D12104.455 (8)
C1i—C3—C6121.720 (6)C3—C6—D13111.416 (7)
C2—C3—C6118.819 (7)C3—C6—D14109.484 (8)
C1—C4—D7112.335 (8)C3—C6—D15111.610 (7)
C1—C4—D8112.697 (6)D13—C6—D14107.728 (9)
C1—C4—D9109.593 (8)D13—C6—D15110.093 (7)
D7—C4—D8104.810 (8)D14—C6—D15106.304 (9)
D7—C4—D9108.776 (7)
Symmetry code: (i) x+1, y+1, z+1.
(HMB_80_REDO_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6β = 90.116 (19)°
Mr = 180.38γ = 90.266 (13)°
Triclinic, P1V = 238.50 (2) Å3
a = 6.1934 (10) ÅZ = 1
b = 6.2008 (13) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2102 (9) ÅT = 80 K
α = 90.012 (15)°?, ? × ? × ? mm
Data collection top
Radiation source: nuclear reactor2θmin = 0.283°, 2θmax = 162.683°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3249 data points
Rp = 0.068Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 234.279 #2(GV) = -1.672 #3(GW) = 159.777 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = -1.0807 #8(shft) = -2.7387 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.0887 parameters
Rexp = 0.0320 restraints
R(F2) = 0.11334(Δ/σ)max = 0.03
χ2 = 19.714Background function: GSAS Background function number 1 with 6 terms. Shifted Chebyshev function of 1st kind 1: 115.290 2: 12.0802 3: -0.106168 4: 0.676159 5: 0.774878 6: 1.72880
Crystal data top
C6(CD3)6β = 90.116 (19)°
Mr = 180.38γ = 90.266 (13)°
Triclinic, P1V = 238.50 (2) Å3
a = 6.1934 (10) ÅZ = 1
b = 6.2008 (13) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2102 (9) ÅT = 80 K
α = 90.012 (15)°?, ? × ? × ? mm
Data collection top
2θmin = 0.283°, 2θmax = 162.683°, 2θstep = 0.05°
Refinement top
Rp = 0.068χ2 = 19.714
Rwp = 0.0883249 data points
Rexp = 0.0327 parameters
R(F2) = 0.113340 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.433260.382780.681510.00816*
C20.616820.320330.563590.01719*
C30.682920.438160.380740.00902*
C40.356370.250710.873030.01082*
C50.751840.131060.640030.01285*
C60.876070.355840.248910.02152*
D70.1860.260930.895570.02856*
D80.424720.304811.022280.03618*
D90.3980.08860.850710.0311*
D100.742290.100250.80930.03583*
D110.91960.156690.608150.04149*
D120.7110.007790.549840.03607*
D131.02640.42440.30590.05361*
D140.856210.402710.080780.02963*
D150.884950.178020.250390.03271*
Geometric parameters (Å, º) top
C1—C21.4092 (3)D8—C41.0714 (2)
C1—C3i1.3808 (3)D8—D71.6943 (3)
C1—C41.5202 (3)D8—D91.7196 (3)
C2—C11.4092 (3)D9—C41.0482 (2)
C2—C31.4108 (3)D9—D71.7198 (3)
C2—C51.5198 (3)D9—D81.7196 (3)
C3—C1i1.3808 (3)D10—C51.0702 (2)
C3—C21.4108 (3)D10—D111.7003 (3)
C3—C61.5399 (3)D10—D121.7550 (3)
C4—C11.5202 (3)D11—C51.0692 (2)
C4—D71.0668 (2)D11—D101.7003 (3)
C4—D81.0714 (2)D11—D121.6811 (3)
C4—D91.0482 (2)D12—C51.0565 (2)
C5—C21.5198 (3)D12—D101.7550 (3)
C5—D101.0702 (2)D12—D111.6811 (3)
C5—D111.0692 (2)D13—C61.0806 (2)
C5—D121.0565 (2)D13—D141.7539 (3)
C6—C31.5399 (3)D13—D151.7907 (3)
C6—D131.0806 (2)D14—C61.0907 (2)
C6—D141.0907 (2)D14—D131.7539 (3)
C6—D151.1043 (2)D14—D151.7563 (3)
D7—C41.0668 (2)D15—C61.1043 (2)
D7—D81.6943 (3)D15—D131.7907 (3)
D7—D91.7198 (3)D15—D141.7563 (3)
C2—C1—C3i119.974 (12)D8—C4—D9108.434 (15)
C2—C1—C4120.746 (14)C2—C5—D10114.432 (15)
C3i—C1—C4119.247 (14)C2—C5—D11111.389 (13)
C1—C2—C3120.669 (14)C2—C5—D12109.508 (15)
C1—C2—C5119.826 (12)D10—C5—D11105.262 (18)
C3—C2—C5119.433 (14)D10—C5—D12111.220 (14)
C1i—C3—C2119.355 (14)D11—C5—D12104.526 (14)
C1i—C3—C6121.756 (11)C3—C6—D13111.417 (13)
C2—C3—C6118.807 (14)C3—C6—D14109.465 (15)
C1—C4—D7112.321 (16)C3—C6—D15111.643 (13)
C1—C4—D8112.697 (12)D13—C6—D14107.755 (17)
C1—C4—D9109.570 (15)D13—C6—D15110.072 (13)
D7—C4—D8104.818 (16)D14—C6—D15106.280 (15)
D7—C4—D9108.805 (13)
Symmetry code: (i) x+1, y+1, z+1.
(HMB_100_REDO_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6β = 90.06 (3)°
Mr = 180.38γ = 90.195 (18)°
Triclinic, P1V = 239.81 (2) Å3
a = 6.2055 (15) ÅZ = 1
b = 6.212 (2) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2214 (11) ÅT = 110 K
α = 90.00 (2)°?, ? × ? × ? mm
Data collection top
Radiation source: nuclear reactor2θmin = 0.283°, 2θmax = 162.683°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3249 data points
Rp = 0.065Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 234.300 #2(GV) = -1.672 #3(GW) = 159.800 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = -1.0810 #8(shft) = -2.7390 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.0858 parameters
Rexp = 0.0320 restraints
R(F2) = 0.11121(Δ/σ)max = 0.06
χ2 = 19.360Background function: GSAS Background function number 1 with 6 terms. Shifted Chebyshev function of 1st kind 1: 120.506 2: 14.5214 3: -2.24029 4: 0.249249 5: 0.910463 6: 1.29052
Crystal data top
C6(CD3)6β = 90.06 (3)°
Mr = 180.38γ = 90.195 (18)°
Triclinic, P1V = 239.81 (2) Å3
a = 6.2055 (15) ÅZ = 1
b = 6.212 (2) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2214 (11) ÅT = 110 K
α = 90.00 (2)°?, ? × ? × ? mm
Data collection top
2θmin = 0.283°, 2θmax = 162.683°, 2θstep = 0.05°
Refinement top
Rp = 0.065χ2 = 19.360
Rwp = 0.0853249 data points
Rexp = 0.0328 parameters
R(F2) = 0.111210 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.433260.382780.681510.01853*
C20.616820.320330.563590.01905*
C30.682920.438160.380740.0093*
C40.356370.250710.873030.0123*
C50.751840.131060.640030.01516*
C60.876070.355840.248890.021 (4)*
D70.1860.260930.895570.06924*
D80.424720.304811.022280.04921*
D90.3980.08860.850710.03311*
D100.742290.100250.80930.0455*
D110.91960.156690.608150.05384*
D120.7110.007790.549840.04543*
D131.02640.42440.30590.08483*
D140.856210.402710.080780.04048*
D150.884950.178020.250390.02789*
Geometric parameters (Å, º) top
C1—C21.4110 (4)D8—C41.0740 (3)
C1—C3i1.3827 (4)D8—D71.6986 (5)
C1—C41.5228 (4)D8—D91.7230 (5)
C2—C11.4110 (4)D9—C41.0497 (3)
C2—C31.4132 (4)D9—D71.7218 (4)
C2—C51.5219 (4)D9—D81.7230 (5)
C3—C1i1.3827 (4)D10—C51.0720 (2)
C3—C21.4132 (4)D10—D111.7029 (5)
C3—C61.5418 (4)D10—D121.7585 (4)
C4—C11.5228 (4)D11—C51.0713 (3)
C4—D71.0687 (3)D11—D101.7029 (5)
C4—D81.0740 (3)D11—D121.6856 (4)
C4—D91.0497 (3)D12—C51.0589 (3)
C5—C21.5219 (4)D12—D101.7585 (4)
C5—D101.0720 (2)D12—D111.6856 (4)
C5—D111.0713 (3)D13—C61.0835 (3)
C5—D121.0589 (3)D13—D141.7581 (5)
C6—C31.5418 (4)D13—D151.7950 (5)
C6—D131.0835 (3)D14—C61.0926 (2)
C6—D141.0926 (2)D14—D131.7581 (5)
C6—D151.1062 (4)D14—D151.7591 (5)
D7—C41.0687 (3)D15—C61.1062 (4)
D7—D81.6986 (5)D15—D131.7950 (5)
D7—D91.7218 (4)D15—D141.7591 (5)
C2—C1—C3i119.951 (17)D8—C4—D9108.45 (2)
C2—C1—C4120.75 (2)C2—C5—D10114.46 (2)
C3i—C1—C4119.27 (2)C2—C5—D11111.37 (2)
C1—C2—C3120.67 (2)C2—C5—D12109.46 (2)
C1—C2—C5119.804 (17)D10—C5—D11105.22 (3)
C3—C2—C5119.45 (2)D10—C5—D12111.23 (2)
C1i—C3—C2119.37 (2)D11—C5—D12104.61 (2)
C1i—C3—C6121.731 (16)C3—C6—D13111.41 (2)
C2—C3—C6118.81 (2)C3—C6—D14109.46 (2)
C1—C4—D7112.32 (2)C3—C6—D15111.600 (19)
C1—C4—D8112.660 (17)D13—C6—D14107.79 (3)
C1—C4—D9109.59 (2)D13—C6—D15110.118 (19)
D7—C4—D8104.88 (3)D14—C6—D15106.27 (2)
D7—C4—D9108.736 (17)
Symmetry code: (i) x+1, y+1, z+1.
(HMB_125_REDO_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6β = 90.02 (5)°
Mr = 180.38γ = 90.17 (2)°
Triclinic, P1V = 240.47 (2) Å3
a = 6.211 (2) ÅZ = 1
b = 6.219 (3) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2257 (19) ÅT = 125 K
α = 90.00 (4)°?, ? × ? × ? mm
Data collection top
Radiation source: nuclear reactor2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3249 data points
Rp = 0.072Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 553.987 #2(GV) = -265.073 #3(GW) = 196.280 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = -4.7283 #8(shft) = 1.4254 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.09613 parameters
Rexp = 0.0320 restraints
R(F2) = 0.12846(Δ/σ)max = 4.58
χ2 = 21.252Background function: GSAS Background function number 1 with 6 terms. Shifted Chebyshev function of 1st kind 1: 122.396 2: 14.6668 3: -4.67912 4: -6.742070E-02 5: 0.392455 6: 1.28008
Crystal data top
C6(CD3)6β = 90.02 (5)°
Mr = 180.38γ = 90.17 (2)°
Triclinic, P1V = 240.47 (2) Å3
a = 6.211 (2) ÅZ = 1
b = 6.219 (3) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2257 (19) ÅT = 125 K
α = 90.00 (4)°?, ? × ? × ? mm
Data collection top
2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05°
Refinement top
Rp = 0.0723249 data points
Rwp = 0.09613 parameters
Rexp = 0.0320 restraints
R(F2) = 0.12846(Δ/σ)max = 4.58
χ2 = 21.252
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.433260.382780.681510.01133*
C20.616820.320330.563590.02823*
C30.682920.438160.380740.00399*
C40.356370.250710.873030.0152*
C50.751840.131060.640310.02162*
C60.876070.355840.248910.03908*
D70.1860.260930.895570.0698*
D80.424720.304811.022280.05633*
D90.3980.08860.850710.04026*
D100.742290.100250.80930.03802*
D110.91960.156690.608150.06314*
D120.7110.007790.549840.05312*
D131.02640.42440.30590.07668*
D140.856210.402710.080780.03899*
D150.884950.178020.250390.03555*
Geometric parameters (Å, º) top
C1—C21.4115 (6)D8—C41.0751 (4)
C1—C3i1.3841 (6)D8—D71.7005 (7)
C1—C41.5239 (7)D8—D91.7249 (8)
C2—C11.4115 (6)D9—C41.0508 (5)
C2—C31.4142 (6)D9—D71.7230 (6)
C2—C51.5239 (7)D9—D81.7249 (8)
C3—C1i1.3841 (6)D10—C51.0710 (4)
C3—C21.4142 (6)D10—D111.7037 (8)
C3—C61.5424 (7)D10—D121.7600 (7)
C4—C11.5239 (7)D11—C51.0724 (4)
C4—D71.0695 (4)D11—D101.7037 (8)
C4—D81.0751 (4)D11—D121.6877 (6)
C4—D91.0508 (5)D12—C51.0611 (5)
C5—C21.5239 (7)D12—D101.7600 (7)
C5—D101.0710 (4)D12—D111.6877 (6)
C5—D111.0724 (4)D13—C61.0848 (4)
C5—D121.0611 (5)D13—D141.7601 (8)
C6—C31.5424 (7)D13—D151.7975 (8)
C6—D131.0848 (4)D14—C61.0935 (4)
C6—D141.0935 (4)D14—D131.7601 (8)
C6—D151.1075 (6)D14—D151.7609 (9)
D7—C41.0695 (4)D15—C61.1075 (6)
D7—D81.7005 (7)D15—D131.7975 (8)
D7—D91.7230 (6)D15—D141.7609 (9)
C2—C1—C3i119.95 (3)D8—C4—D9108.46 (4)
C2—C1—C4120.72 (3)C2—C5—D10114.55 (4)
C3i—C1—C4119.30 (3)C2—C5—D11111.30 (3)
C1—C2—C3120.65 (3)C2—C5—D12109.37 (4)
C1—C2—C5119.75 (3)D10—C5—D11105.28 (4)
C3—C2—C5119.53 (3)D10—C5—D12111.28 (4)
C1i—C3—C2119.40 (3)D11—C5—D12104.57 (3)
C1i—C3—C6121.73 (3)C3—C6—D13111.40 (3)
C2—C3—C6118.78 (3)C3—C6—D14109.43 (3)
C1—C4—D7112.30 (4)C3—C6—D15111.60 (3)
C1—C4—D8112.63 (3)D13—C6—D14107.80 (4)
C1—C4—D9109.63 (4)D13—C6—D15110.15 (3)
D7—C4—D8104.92 (4)D14—C6—D15106.27 (4)
D7—C4—D9108.70 (2)
Symmetry code: (i) x+1, y+1, z+1.
(HMB_129_REDO_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6β = 90.02 (2)°
Mr = 180.38γ = 90.139 (16)°
Triclinic, P1V = 240.88 (3) Å3
a = 6.2157 (12) ÅZ = 1
b = 6.2221 (18) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2284 (12) ÅT = 129 K
α = 90.00 (2)°?, ? × ? × ? mm
Data collection top
Radiation source: nuclear reactor2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3249 data points
Rp = 0.068Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 364.770 #2(GV) = -95.448 #3(GW) = 181.708 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = -0.0050 #8(shft) = -2.2890 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.0909 parameters
Rexp = 0.0320 restraints
R(F2) = 0.11030(Δ/σ)max = 0.07
χ2 = 7.784Background function: GSAS Background function number 1 with 6 terms. Shifted Chebyshev function of 1st kind 1: 122.133 2: 13.8067 3: -4.87116 4: -0.341430 5: 0.122913 6: 1.03957
Crystal data top
C6(CD3)6β = 90.02 (2)°
Mr = 180.38γ = 90.139 (16)°
Triclinic, P1V = 240.88 (3) Å3
a = 6.2157 (12) ÅZ = 1
b = 6.2221 (18) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2284 (12) ÅT = 129 K
α = 90.00 (2)°?, ? × ? × ? mm
Data collection top
2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05°
Refinement top
Rp = 0.068χ2 = 7.784
Rwp = 0.0903249 data points
Rexp = 0.0329 parameters
R(F2) = 0.110300 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.433260.382780.681510.02513*
C20.616820.320330.563590.02259*
C30.682920.438160.380740.0169*
C40.356370.250710.873030.01106*
C50.751840.131060.640310.02248*
C60.876070.355840.248910.0286*
D70.1860.260930.895570.01953*
D80.424720.304811.022280.02566*
D90.3980.08860.850710.05281*
D100.742290.100250.80930.07166*
D110.91960.156690.608150.02249*
D120.7110.007790.549840.14009*
D131.02640.42440.30590.07702*
D140.856210.402710.080780.05327*
D150.884950.178020.250390.06147*
Geometric parameters (Å, º) top
C1—C21.4124 (3)D8—C41.0757 (2)
C1—C3i1.3845 (3)D8—D71.7019 (4)
C1—C41.5248 (4)D8—D91.7257 (5)
C2—C11.4124 (3)D9—C41.0512 (3)
C2—C31.4151 (3)D9—D71.7237 (4)
C2—C51.5245 (4)D9—D81.7257 (5)
C3—C1i1.3845 (3)D10—C51.0715 (2)
C3—C21.4151 (3)D10—D111.7049 (4)
C3—C61.5432 (3)D10—D121.7608 (4)
C4—C11.5248 (4)D11—C51.0734 (2)
C4—D71.0703 (2)D11—D101.7049 (4)
C4—D81.0757 (2)D11—D121.6892 (4)
C4—D91.0512 (3)D12—C51.0617 (3)
C5—C21.5245 (4)D12—D101.7608 (4)
C5—D101.0715 (2)D12—D111.6892 (4)
C5—D111.0734 (2)D13—C61.0858 (2)
C5—D121.0617 (3)D13—D141.7611 (4)
C6—C31.5432 (3)D13—D151.7988 (4)
C6—D131.0858 (2)D14—C61.0940 (2)
C6—D141.0940 (2)D14—D131.7611 (4)
C6—D151.1080 (3)D14—D151.7617 (5)
D7—C41.0703 (2)D15—C61.1080 (3)
D7—D81.7019 (4)D15—D131.7988 (4)
D7—D91.7237 (4)D15—D141.7617 (5)
C2—C1—C3i119.939 (15)D8—C4—D9108.46 (2)
C2—C1—C4120.741 (17)C2—C5—D10114.554 (19)
C3i—C1—C4119.288 (18)C2—C5—D11111.289 (16)
C1—C2—C3120.662 (17)C2—C5—D12109.355 (19)
C1—C2—C5119.745 (15)D10—C5—D11105.28 (2)
C3—C2—C5119.519 (18)D10—C5—D12111.265 (19)
C1i—C3—C2119.397 (18)D11—C5—D12104.594 (17)
C1i—C3—C6121.723 (15)C3—C6—D13111.420 (17)
C2—C3—C6118.797 (17)C3—C6—D14109.431 (18)
C1—C4—D7112.321 (18)C3—C6—D15111.571 (17)
C1—C4—D8112.607 (16)D13—C6—D14107.79 (2)
C1—C4—D9109.63 (2)D13—C6—D15110.160 (16)
D7—C4—D8104.943 (19)D14—C6—D15106.27 (2)
D7—C4—D9108.679 (15)
Symmetry code: (i) x+1, y+1, z+1.
(HMB_132_REDO_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6β = 90.03 (3)°
Mr = 180.38γ = 90.12 (3)°
Triclinic, P1V = 240.98 (2) Å3
a = 6.2183 (19) ÅZ = 1
b = 6.222 (3) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2281 (18) ÅT = 132 K
α = 90.01 (4)°?, ? × ? × ? mm
Data collection top
Radiation source: nuclear reactor2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3249 data points
Rp = 0.068Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 364.800 #2(GV) = -95.450 #3(GW) = 181.700 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = -0.0020 #8(shft) = -2.3020 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.0917 parameters
Rexp = 0.0320 restraints
R(F2) = 0.12625(Δ/σ)max < 0.001
χ2 = 19.184Background function: GSAS Background function number 1 with 6 terms. Shifted Chebyshev function of 1st kind 1: 124.877 2: 15.2913 3: -5.50637 4: 0.289517 5: 0.563200 6: 1.96920
Crystal data top
C6(CD3)6β = 90.03 (3)°
Mr = 180.38γ = 90.12 (3)°
Triclinic, P1V = 240.98 (2) Å3
a = 6.2183 (19) ÅZ = 1
b = 6.222 (3) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 6.2281 (18) ÅT = 132 K
α = 90.01 (4)°?, ? × ? × ? mm
Data collection top
2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05°
Refinement top
Rp = 0.068χ2 = 19.184
Rwp = 0.0913249 data points
Rexp = 0.0327 parameters
R(F2) = 0.126250 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.433260.382780.681510.03057*
C20.616820.320330.563590.02376*
C30.682920.438160.380740.01994*
C40.356370.250710.873030.01642*
C50.751840.131060.640310.02296*
C60.876070.355840.248910.03332*
D70.1860.260930.895570.02279*
D80.424720.304811.022280.02466*
D90.3980.08860.850710.05788*
D100.742290.100250.80930.08336*
D110.91960.156690.608150.02077*
D120.7110.007790.549840.11643*
D131.02640.42440.30590.09469*
D140.856210.402710.080780.05923*
D150.884950.178020.250390.0581*
Geometric parameters (Å, º) top
C1—C21.4127 (5)D8—C41.0757 (4)
C1—C3i1.3845 (5)D8—D71.7024 (6)
C1—C41.5251 (6)D8—D91.7257 (7)
C2—C11.4127 (5)D9—C41.0511 (4)
C2—C31.4152 (5)D9—D71.7239 (6)
C2—C51.5244 (6)D9—D81.7257 (7)
C3—C1i1.3845 (5)D10—C51.0715 (3)
C3—C21.4152 (5)D10—D111.7054 (6)
C3—C61.5436 (5)D10—D121.7607 (6)
C4—C11.5251 (6)D11—C51.0739 (3)
C4—D71.0708 (3)D11—D101.7054 (6)
C4—D81.0757 (4)D11—D121.6899 (6)
C4—D91.0511 (4)D12—C51.0617 (4)
C5—C21.5244 (6)D12—D101.7607 (6)
C5—D101.0715 (3)D12—D111.6899 (6)
C5—D111.0739 (3)D13—C61.0862 (4)
C5—D121.0617 (4)D13—D141.7612 (6)
C6—C31.5436 (5)D13—D151.7993 (7)
C6—D131.0862 (4)D14—C61.0940 (4)
C6—D141.0940 (4)D14—D131.7612 (6)
C6—D151.1080 (5)D14—D151.7617 (7)
D7—C41.0708 (3)D15—C61.1080 (5)
D7—D81.7024 (6)D15—D131.7993 (7)
D7—D91.7239 (6)D15—D141.7617 (7)
C2—C1—C3i119.94 (2)D8—C4—D9108.46 (3)
C2—C1—C4120.76 (3)C2—C5—D10114.55 (3)
C3i—C1—C4119.27 (3)C2—C5—D11111.29 (3)
C1—C2—C3120.68 (3)C2—C5—D12109.35 (3)
C1—C2—C5119.75 (2)D10—C5—D11105.29 (3)
C3—C2—C5119.50 (3)D10—C5—D12111.25 (3)
C1i—C3—C2119.38 (3)D11—C5—D12104.61 (3)
C1i—C3—C6121.72 (2)C3—C6—D13111.45 (3)
C2—C3—C6118.81 (3)C3—C6—D14109.43 (3)
C1—C4—D7112.35 (3)C3—C6—D15111.55 (3)
C1—C4—D8112.59 (2)D13—C6—D14107.77 (3)
C1—C4—D9109.63 (3)D13—C6—D15110.17 (3)
D7—C4—D8104.95 (3)D14—C6—D15106.27 (3)
D7—C4—D9108.67 (2)
Symmetry code: (i) x+1, y+1, z+1.
(HMB_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6β = 98.460 (12)°
Mr = 180.38γ = 100.057 (11)°
Triclinic, P1V = 241.36 (6) Å3
a = 5.2360 (8) ÅZ = 1
b = 6.1845 (8) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 7.952 (1) ÅT = 140 K
α = 103.816 (12)°?, ? × ? × ? mm
Data collection top
Radiation source: nuclear reactor2θmin = 0.758°, 2θmax = 163.158°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3249 data points
Rp = 0.060Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 767.683 #2(GV) = -142.247 #3(GW) = 126.504 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 11.3563 #8(shft) = -60.3156 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.0819 parameters
Rexp = 0.0320 restraints
R(F2) = 0.15460(Δ/σ)max = 0.07
χ2 = 7.398Background function: GSAS Background function number 2 with 6 terms. Cosine Fourier series 1: 126.649 2: -16.6175 3: -5.83631 4: -2.49663 5: 1.67274 6: -4.72451
Crystal data top
C6(CD3)6β = 98.460 (12)°
Mr = 180.38γ = 100.057 (11)°
Triclinic, P1V = 241.36 (6) Å3
a = 5.2360 (8) ÅZ = 1
b = 6.1845 (8) ÅMonchromatic beam radiation, λ = 1.594 Å
c = 7.952 (1) ÅT = 140 K
α = 103.816 (12)°?, ? × ? × ? mm
Data collection top
2θmin = 0.758°, 2θmax = 163.158°, 2θstep = 0.05°
Refinement top
Rp = 0.060χ2 = 7.398
Rwp = 0.0813249 data points
Rexp = 0.0329 parameters
R(F2) = 0.154600 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.564640.616220.319290.00703*
C20.678160.433110.386920.02147*
C30.614620.315430.567510.0305*
C40.647050.748110.123580.01857*
C50.873580.354540.263330.01904*
C60.752820.12490.637850.03363*
D70.507430.687520.057560.03729*
D80.824790.703090.069740.11386*
D90.681620.922960.112840.07042*
D100.869590.178770.319780.11099*
D110.063060.44070.252430.06375*
D120.816480.37890.14120.06264*
D130.952710.177610.579530.07353*
D140.649220.027530.620180.04368*
D150.711060.078690.779740.04463*
Geometric parameters (Å, º) top
C1—C21.4012 (2)D8—C41.0757 (2)
C1—C3i1.3935 (2)D8—D71.6661 (2)
C1—C41.5319 (3)D8—D91.7411 (2)
C1—D72.0993 (3)D8—D121.9398 (3)
C2—C11.4012 (2)D9—C41.0452 (2)
C2—C31.4065 (2)D9—D71.7621 (2)
C2—C51.5346 (2)D9—D81.7411 (2)
C3—C1i1.3935 (2)D10—C51.0677 (2)
C3—C21.4065 (2)D10—D11ii1.6703 (3)
C3—C61.5255 (2)D10—D121.7386 (3)
C3—D132.0994 (3)D11—C5iii1.0217 (2)
C4—C11.5319 (3)D11—D10iii1.6703 (3)
C4—D71.0304 (1)D11—D12iii1.7090 (2)
C4—D81.0757 (2)D12—C51.0424 (1)
C4—D91.0452 (2)D12—D81.9398 (3)
C5—C21.5346 (2)D12—D101.7386 (3)
C5—D101.0677 (2)D12—D11ii1.7090 (2)
C5—D11ii1.0217 (2)D13—C32.0994 (3)
C5—D121.0424 (1)D13—C61.0405 (2)
C6—C31.5255 (2)D13—D141.7855 (3)
C6—D131.0405 (2)D13—D151.7837 (3)
C6—D141.0535 (2)D14—C61.0535 (2)
C6—D151.0743 (2)D14—D131.7855 (3)
D7—C12.0993 (3)D14—D151.6097 (2)
D7—C41.0304 (1)D15—C61.0743 (2)
D7—D81.6661 (2)D15—D131.7837 (3)
D7—D91.7621 (2)D15—D141.6097 (2)
C2—C1—C3i119.673 (11)D8—C4—D9110.352 (12)
C2—C1—C4120.205 (10)C2—C5—D10108.938 (13)
C3i—C1—C4120.056 (10)C2—C5—D11ii110.885 (11)
C1—C2—C3121.372 (10)C2—C5—D12108.120 (10)
C1—C2—C5120.182 (11)D10—C5—D11ii106.135 (13)
C3—C2—C5118.441 (10)D10—C5—D12110.962 (11)
C1i—C3—C2118.954 (10)D11ii—C5—D12111.782 (13)
C1i—C3—C6121.115 (10)C3—C6—D13108.318 (13)
C2—C3—C6119.847 (10)C3—C6—D14108.172 (11)
C1—C4—D7108.440 (13)C3—C6—D15109.511 (11)
C1—C4—D8107.995 (12)D13—C6—D14117.010 (11)
C1—C4—D9108.967 (13)D13—C6—D15115.003 (12)
D7—C4—D8104.555 (11)D14—C6—D1598.309 (14)
D7—C4—D9116.201 (10)
Symmetry codes: (i) x1, y1, z+1; (ii) x1, y, z; (iii) x+1, y, z.

Experimental details

(HMB_5_publ)(HMB_80_REDO_publ)(HMB_100_REDO_publ)(HMB_125_REDO_publ)
Crystal data
Chemical formulaC6(CD3)6C6(CD3)6C6(CD3)6C6(CD3)6
Mr180.38180.38180.38180.38
Crystal system, space groupTriclinic, P1Triclinic, P1Triclinic, P1Triclinic, P1
Temperature (K)5K80110125
a, b, c (Å)6.1803 (5), 6.1898 (6), 6.1993 (5)6.1934 (10), 6.2008 (13), 6.2102 (9)6.2055 (15), 6.212 (2), 6.2214 (11)6.211 (2), 6.219 (3), 6.2257 (19)
α, β, γ (°)90.041 (9), 90.129 (9), 90.239 (7)90.012 (15), 90.116 (19), 90.266 (13)90.00 (2), 90.06 (3), 90.195 (18)90.00 (4), 90.02 (5), 90.17 (2)
V3)237.15 (1)238.50 (2)239.81 (2)240.47 (2)
Z1111
Radiation typeMonchromatic beam, λ = 1.594 ÅMonchromatic beam, λ = 1.594 ÅMonchromatic beam, λ = 1.594 ÅMonchromatic beam, λ = 1.594 Å
Specimen shape, size (mm)?, ? × ? × ??, ? × ? × ??, ? × ? × ??, ? × ? × ?
Data collection
Diffractometer????
Specimen mounting????
Data collection mode????
Scan method????
2θ values (°)2θmin = 0.437 2θmax = 162.837 2θstep = 0.052θmin = 0.283 2θmax = 162.683 2θstep = 0.052θmin = 0.283 2θmax = 162.683 2θstep = 0.052θmin = 0.263 2θmax = 162.663 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.066, Rwp = 0.090, Rexp = 0.023, R(F2) = 0.09220, χ2 = 15.210Rp = 0.068, Rwp = 0.088, Rexp = 0.032, R(F2) = 0.11334, χ2 = 19.714Rp = 0.065, Rwp = 0.085, Rexp = 0.032, R(F2) = 0.11121, χ2 = 19.360Rp = 0.072, Rwp = 0.096, Rexp = 0.032, R(F2) = 0.12846, χ2 = 21.252
No. of data points3249324932493249
No. of parameters107813
(Δ/σ)max5.800.030.064.58


(HMB_129_REDO_publ)(HMB_132_REDO_publ)(HMB_publ)
Crystal data
Chemical formulaC6(CD3)6C6(CD3)6C6(CD3)6
Mr180.38180.38180.38
Crystal system, space groupTriclinic, P1Triclinic, P1Triclinic, P1
Temperature (K)129132140
a, b, c (Å)6.2157 (12), 6.2221 (18), 6.2284 (12)6.2183 (19), 6.222 (3), 6.2281 (18)5.2360 (8), 6.1845 (8), 7.952 (1)
α, β, γ (°)90.00 (2), 90.02 (2), 90.139 (16)90.01 (4), 90.03 (3), 90.12 (3)103.816 (12), 98.460 (12), 100.057 (11)
V3)240.88 (3)240.98 (2)241.36 (6)
Z111
Radiation typeMonchromatic beam, λ = 1.594 ÅMonchromatic beam, λ = 1.594 ÅMonchromatic beam, λ = 1.594 Å
Specimen shape, size (mm)?, ? × ? × ??, ? × ? × ??, ? × ? × ?
Data collection
Diffractometer???
Specimen mounting???
Data collection mode???
Scan method???
2θ values (°)2θmin = 0.263 2θmax = 162.663 2θstep = 0.052θmin = 0.263 2θmax = 162.663 2θstep = 0.052θmin = 0.758 2θmax = 163.158 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.068, Rwp = 0.090, Rexp = 0.032, R(F2) = 0.11030, χ2 = 7.784Rp = 0.068, Rwp = 0.091, Rexp = 0.032, R(F2) = 0.12625, χ2 = 19.184Rp = 0.060, Rwp = 0.081, Rexp = 0.032, R(F2) = 0.15460, χ2 = 7.398
No. of data points324932493249
No. of parameters979
(Δ/σ)max0.07< 0.0010.07

Computer programs: GSAS.

 

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