research papers
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
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104034007/lc5016sup1.cif |
CCDC references: 205339; 268162; 268163; 268164; 268165; 268166; 268167
(HMB_5_publ) 1,2,3,4,5,6-hexadeuteromethylbenzene top
Crystal data top
C6(CD3)6 | γ = 90.239 (7)° |
Mr = 180.38 | V = 237.15 (1) Å3 |
Triclinic, P1 | Z = 1 |
a = 6.1803 (5) Å | Monchromatic beam radiation, λ = 1.594 Å |
b = 6.1898 (6) Å | T = 5K K |
c = 6.1993 (5) Å | white |
α = 90.041 (9)° | ?, ? × ? × ? mm |
β = 90.129 (9)° |
Data collection top
Radiation source: nuclear reactor | 2θmin = 0.437°, 2θmax = 162.837°, 2θstep = 0.05° |
Refinement top
Least-squares matrix: full | Excluded region(s): 150.5° < 2θ < 154° |
Rp = 0.066 | Profile 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 = 0.090 | 10 parameters |
Rexp = 0.023 | 0 restraints |
R(F2) = 0.09220 | (Δ/σ)max = 5.80 |
χ2 = 15.210 | Background 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)6 | β = 90.129 (9)° |
Mr = 180.38 | γ = 90.239 (7)° |
Triclinic, P1 | V = 237.15 (1) Å3 |
a = 6.1803 (5) Å | Z = 1 |
b = 6.1898 (6) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.1993 (5) Å | T = 5K K |
α = 90.041 (9)° | ?, ? × ? × ? mm |
Refinement top
Rp = 0.066 | 3249 data points |
Rwp = 0.090 | 10 parameters |
Rexp = 0.023 | 0 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
x | y | z | Uiso*/Ueq | ||
C1 | 0.43326 | 0.38278 | 0.68151 | 0.00871* | |
C2 | 0.61682 | 0.32033 | 0.56359 | 0.0062* | |
C3 | 0.68292 | 0.43816 | 0.38074 | 0.00682* | |
C4 | 0.35637 | 0.25071 | 0.87303 | 0.00516* | |
C5 | 0.75184 | 0.13106 | 0.64031 | 0.00804* | |
C6 | 0.87607 | 0.35584 | 0.24891 | 0.00502* | |
D7 | 0.186 | 0.26093 | 0.89557 | 0.02554* | |
D8 | 0.42472 | 0.30481 | 1.02228 | 0.0321* | |
D9 | 0.398 | 0.0886 | 0.85071 | 0.01524* | |
D10 | 0.74229 | 0.10025 | 0.8093 | 0.02213* | |
D11 | 0.9196 | 0.15669 | 0.60815 | 0.0188* | |
D12 | 0.711 | −0.00779 | 0.54984 | 0.02646* | |
D13 | 1.0264 | 0.4244 | 0.3059 | 0.02564* | |
D14 | 0.85621 | 0.40271 | 0.08078 | 0.02341* | |
D15 | 0.88495 | 0.17802 | 0.25039 | 0.01691* |
Geometric parameters (Å, º) top
C1—C2 | 1.4063 (1) | D8—C4 | 1.0693 (1) |
C1—C3i | 1.3781 (1) | D8—D7 | 1.6908 (2) |
C1—C4 | 1.5180 (2) | D8—D9 | 1.7161 (2) |
C2—C1 | 1.4063 (1) | D9—C4 | 1.0461 (1) |
C2—C3 | 1.4088 (1) | D9—D7 | 1.7160 (2) |
C2—C5 | 1.5173 (2) | D9—D8 | 1.7161 (2) |
C3—C1i | 1.3781 (1) | D10—C5 | 1.0667 (1) |
C3—C2 | 1.4088 (1) | D10—D11 | 1.6975 (2) |
C3—C6 | 1.5367 (2) | D10—D12 | 1.7515 (2) |
C4—C1 | 1.5180 (2) | D11—C5 | 1.0675 (1) |
C4—D7 | 1.0646 (1) | D11—D10 | 1.6975 (2) |
C4—D8 | 1.0693 (1) | D11—D12 | 1.6780 (2) |
C4—D9 | 1.0461 (1) | D12—C5 | 1.0554 (1) |
C5—C2 | 1.5173 (2) | D12—D10 | 1.7515 (2) |
C5—D10 | 1.0667 (1) | D12—D11 | 1.6780 (2) |
C5—D11 | 1.0675 (1) | D13—C6 | 1.0785 (1) |
C5—D12 | 1.0554 (1) | D13—D14 | 1.7504 (2) |
C6—C3 | 1.5367 (2) | D13—D15 | 1.7875 (2) |
C6—D13 | 1.0785 (1) | D14—C6 | 1.0889 (1) |
C6—D14 | 1.0889 (1) | D14—D13 | 1.7504 (2) |
C6—D15 | 1.1023 (1) | D14—D15 | 1.7535 (2) |
D7—C4 | 1.0646 (1) | D15—C6 | 1.1023 (1) |
D7—D8 | 1.6908 (2) | D15—D13 | 1.7875 (2) |
D7—D9 | 1.7160 (2) | D15—D14 | 1.7535 (2) |
C2—C1—C3i | 119.937 (6) | D8—C4—D9 | 108.429 (8) |
C2—C1—C4 | 120.760 (7) | C2—C5—D10 | 114.523 (8) |
C3i—C1—C4 | 119.271 (7) | C2—C5—D11 | 111.290 (7) |
C1—C2—C3 | 120.684 (7) | C2—C5—D12 | 109.422 (8) |
C1—C2—C5 | 119.739 (6) | D10—C5—D11 | 105.380 (9) |
C3—C2—C5 | 119.504 (7) | D10—C5—D12 | 111.257 (8) |
C1i—C3—C2 | 119.378 (7) | D11—C5—D12 | 104.455 (8) |
C1i—C3—C6 | 121.720 (6) | C3—C6—D13 | 111.416 (7) |
C2—C3—C6 | 118.819 (7) | C3—C6—D14 | 109.484 (8) |
C1—C4—D7 | 112.335 (8) | C3—C6—D15 | 111.610 (7) |
C1—C4—D8 | 112.697 (6) | D13—C6—D14 | 107.728 (9) |
C1—C4—D9 | 109.593 (8) | D13—C6—D15 | 110.093 (7) |
D7—C4—D8 | 104.810 (8) | D14—C6—D15 | 106.304 (9) |
D7—C4—D9 | 108.776 (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)6 | β = 90.116 (19)° |
Mr = 180.38 | γ = 90.266 (13)° |
Triclinic, P1 | V = 238.50 (2) Å3 |
a = 6.1934 (10) Å | Z = 1 |
b = 6.2008 (13) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2102 (9) Å | T = 80 K |
α = 90.012 (15)° | ?, ? × ? × ? mm |
Data collection top
Radiation source: nuclear reactor | 2θmin = 0.283°, 2θmax = 162.683°, 2θstep = 0.05° |
Refinement top
Least-squares matrix: full | 3249 data points |
Rp = 0.068 | Profile 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 = 0.088 | 7 parameters |
Rexp = 0.032 | 0 restraints |
R(F2) = 0.11334 | (Δ/σ)max = 0.03 |
χ2 = 19.714 | Background 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)6 | β = 90.116 (19)° |
Mr = 180.38 | γ = 90.266 (13)° |
Triclinic, P1 | V = 238.50 (2) Å3 |
a = 6.1934 (10) Å | Z = 1 |
b = 6.2008 (13) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2102 (9) Å | T = 80 K |
α = 90.012 (15)° | ?, ? × ? × ? mm |
Refinement top
Rp = 0.068 | χ2 = 19.714 |
Rwp = 0.088 | 3249 data points |
Rexp = 0.032 | 7 parameters |
R(F2) = 0.11334 | 0 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
C1 | 0.43326 | 0.38278 | 0.68151 | 0.00816* | |
C2 | 0.61682 | 0.32033 | 0.56359 | 0.01719* | |
C3 | 0.68292 | 0.43816 | 0.38074 | 0.00902* | |
C4 | 0.35637 | 0.25071 | 0.87303 | 0.01082* | |
C5 | 0.75184 | 0.13106 | 0.64003 | 0.01285* | |
C6 | 0.87607 | 0.35584 | 0.24891 | 0.02152* | |
D7 | 0.186 | 0.26093 | 0.89557 | 0.02856* | |
D8 | 0.42472 | 0.30481 | 1.02228 | 0.03618* | |
D9 | 0.398 | 0.0886 | 0.85071 | 0.0311* | |
D10 | 0.74229 | 0.10025 | 0.8093 | 0.03583* | |
D11 | 0.9196 | 0.15669 | 0.60815 | 0.04149* | |
D12 | 0.711 | −0.00779 | 0.54984 | 0.03607* | |
D13 | 1.0264 | 0.4244 | 0.3059 | 0.05361* | |
D14 | 0.85621 | 0.40271 | 0.08078 | 0.02963* | |
D15 | 0.88495 | 0.17802 | 0.25039 | 0.03271* |
Geometric parameters (Å, º) top
C1—C2 | 1.4092 (3) | D8—C4 | 1.0714 (2) |
C1—C3i | 1.3808 (3) | D8—D7 | 1.6943 (3) |
C1—C4 | 1.5202 (3) | D8—D9 | 1.7196 (3) |
C2—C1 | 1.4092 (3) | D9—C4 | 1.0482 (2) |
C2—C3 | 1.4108 (3) | D9—D7 | 1.7198 (3) |
C2—C5 | 1.5198 (3) | D9—D8 | 1.7196 (3) |
C3—C1i | 1.3808 (3) | D10—C5 | 1.0702 (2) |
C3—C2 | 1.4108 (3) | D10—D11 | 1.7003 (3) |
C3—C6 | 1.5399 (3) | D10—D12 | 1.7550 (3) |
C4—C1 | 1.5202 (3) | D11—C5 | 1.0692 (2) |
C4—D7 | 1.0668 (2) | D11—D10 | 1.7003 (3) |
C4—D8 | 1.0714 (2) | D11—D12 | 1.6811 (3) |
C4—D9 | 1.0482 (2) | D12—C5 | 1.0565 (2) |
C5—C2 | 1.5198 (3) | D12—D10 | 1.7550 (3) |
C5—D10 | 1.0702 (2) | D12—D11 | 1.6811 (3) |
C5—D11 | 1.0692 (2) | D13—C6 | 1.0806 (2) |
C5—D12 | 1.0565 (2) | D13—D14 | 1.7539 (3) |
C6—C3 | 1.5399 (3) | D13—D15 | 1.7907 (3) |
C6—D13 | 1.0806 (2) | D14—C6 | 1.0907 (2) |
C6—D14 | 1.0907 (2) | D14—D13 | 1.7539 (3) |
C6—D15 | 1.1043 (2) | D14—D15 | 1.7563 (3) |
D7—C4 | 1.0668 (2) | D15—C6 | 1.1043 (2) |
D7—D8 | 1.6943 (3) | D15—D13 | 1.7907 (3) |
D7—D9 | 1.7198 (3) | D15—D14 | 1.7563 (3) |
C2—C1—C3i | 119.974 (12) | D8—C4—D9 | 108.434 (15) |
C2—C1—C4 | 120.746 (14) | C2—C5—D10 | 114.432 (15) |
C3i—C1—C4 | 119.247 (14) | C2—C5—D11 | 111.389 (13) |
C1—C2—C3 | 120.669 (14) | C2—C5—D12 | 109.508 (15) |
C1—C2—C5 | 119.826 (12) | D10—C5—D11 | 105.262 (18) |
C3—C2—C5 | 119.433 (14) | D10—C5—D12 | 111.220 (14) |
C1i—C3—C2 | 119.355 (14) | D11—C5—D12 | 104.526 (14) |
C1i—C3—C6 | 121.756 (11) | C3—C6—D13 | 111.417 (13) |
C2—C3—C6 | 118.807 (14) | C3—C6—D14 | 109.465 (15) |
C1—C4—D7 | 112.321 (16) | C3—C6—D15 | 111.643 (13) |
C1—C4—D8 | 112.697 (12) | D13—C6—D14 | 107.755 (17) |
C1—C4—D9 | 109.570 (15) | D13—C6—D15 | 110.072 (13) |
D7—C4—D8 | 104.818 (16) | D14—C6—D15 | 106.280 (15) |
D7—C4—D9 | 108.805 (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)6 | β = 90.06 (3)° |
Mr = 180.38 | γ = 90.195 (18)° |
Triclinic, P1 | V = 239.81 (2) Å3 |
a = 6.2055 (15) Å | Z = 1 |
b = 6.212 (2) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2214 (11) Å | T = 110 K |
α = 90.00 (2)° | ?, ? × ? × ? mm |
Data collection top
Radiation source: nuclear reactor | 2θmin = 0.283°, 2θmax = 162.683°, 2θstep = 0.05° |
Refinement top
Least-squares matrix: full | 3249 data points |
Rp = 0.065 | Profile 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 = 0.085 | 8 parameters |
Rexp = 0.032 | 0 restraints |
R(F2) = 0.11121 | (Δ/σ)max = 0.06 |
χ2 = 19.360 | Background 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)6 | β = 90.06 (3)° |
Mr = 180.38 | γ = 90.195 (18)° |
Triclinic, P1 | V = 239.81 (2) Å3 |
a = 6.2055 (15) Å | Z = 1 |
b = 6.212 (2) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2214 (11) Å | T = 110 K |
α = 90.00 (2)° | ?, ? × ? × ? mm |
Refinement top
Rp = 0.065 | χ2 = 19.360 |
Rwp = 0.085 | 3249 data points |
Rexp = 0.032 | 8 parameters |
R(F2) = 0.11121 | 0 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
C1 | 0.43326 | 0.38278 | 0.68151 | 0.01853* | |
C2 | 0.61682 | 0.32033 | 0.56359 | 0.01905* | |
C3 | 0.68292 | 0.43816 | 0.38074 | 0.0093* | |
C4 | 0.35637 | 0.25071 | 0.87303 | 0.0123* | |
C5 | 0.75184 | 0.13106 | 0.64003 | 0.01516* | |
C6 | 0.87607 | 0.35584 | 0.24889 | 0.021 (4)* | |
D7 | 0.186 | 0.26093 | 0.89557 | 0.06924* | |
D8 | 0.42472 | 0.30481 | 1.02228 | 0.04921* | |
D9 | 0.398 | 0.0886 | 0.85071 | 0.03311* | |
D10 | 0.74229 | 0.10025 | 0.8093 | 0.0455* | |
D11 | 0.9196 | 0.15669 | 0.60815 | 0.05384* | |
D12 | 0.711 | −0.00779 | 0.54984 | 0.04543* | |
D13 | 1.0264 | 0.4244 | 0.3059 | 0.08483* | |
D14 | 0.85621 | 0.40271 | 0.08078 | 0.04048* | |
D15 | 0.88495 | 0.17802 | 0.25039 | 0.02789* |
Geometric parameters (Å, º) top
C1—C2 | 1.4110 (4) | D8—C4 | 1.0740 (3) |
C1—C3i | 1.3827 (4) | D8—D7 | 1.6986 (5) |
C1—C4 | 1.5228 (4) | D8—D9 | 1.7230 (5) |
C2—C1 | 1.4110 (4) | D9—C4 | 1.0497 (3) |
C2—C3 | 1.4132 (4) | D9—D7 | 1.7218 (4) |
C2—C5 | 1.5219 (4) | D9—D8 | 1.7230 (5) |
C3—C1i | 1.3827 (4) | D10—C5 | 1.0720 (2) |
C3—C2 | 1.4132 (4) | D10—D11 | 1.7029 (5) |
C3—C6 | 1.5418 (4) | D10—D12 | 1.7585 (4) |
C4—C1 | 1.5228 (4) | D11—C5 | 1.0713 (3) |
C4—D7 | 1.0687 (3) | D11—D10 | 1.7029 (5) |
C4—D8 | 1.0740 (3) | D11—D12 | 1.6856 (4) |
C4—D9 | 1.0497 (3) | D12—C5 | 1.0589 (3) |
C5—C2 | 1.5219 (4) | D12—D10 | 1.7585 (4) |
C5—D10 | 1.0720 (2) | D12—D11 | 1.6856 (4) |
C5—D11 | 1.0713 (3) | D13—C6 | 1.0835 (3) |
C5—D12 | 1.0589 (3) | D13—D14 | 1.7581 (5) |
C6—C3 | 1.5418 (4) | D13—D15 | 1.7950 (5) |
C6—D13 | 1.0835 (3) | D14—C6 | 1.0926 (2) |
C6—D14 | 1.0926 (2) | D14—D13 | 1.7581 (5) |
C6—D15 | 1.1062 (4) | D14—D15 | 1.7591 (5) |
D7—C4 | 1.0687 (3) | D15—C6 | 1.1062 (4) |
D7—D8 | 1.6986 (5) | D15—D13 | 1.7950 (5) |
D7—D9 | 1.7218 (4) | D15—D14 | 1.7591 (5) |
C2—C1—C3i | 119.951 (17) | D8—C4—D9 | 108.45 (2) |
C2—C1—C4 | 120.75 (2) | C2—C5—D10 | 114.46 (2) |
C3i—C1—C4 | 119.27 (2) | C2—C5—D11 | 111.37 (2) |
C1—C2—C3 | 120.67 (2) | C2—C5—D12 | 109.46 (2) |
C1—C2—C5 | 119.804 (17) | D10—C5—D11 | 105.22 (3) |
C3—C2—C5 | 119.45 (2) | D10—C5—D12 | 111.23 (2) |
C1i—C3—C2 | 119.37 (2) | D11—C5—D12 | 104.61 (2) |
C1i—C3—C6 | 121.731 (16) | C3—C6—D13 | 111.41 (2) |
C2—C3—C6 | 118.81 (2) | C3—C6—D14 | 109.46 (2) |
C1—C4—D7 | 112.32 (2) | C3—C6—D15 | 111.600 (19) |
C1—C4—D8 | 112.660 (17) | D13—C6—D14 | 107.79 (3) |
C1—C4—D9 | 109.59 (2) | D13—C6—D15 | 110.118 (19) |
D7—C4—D8 | 104.88 (3) | D14—C6—D15 | 106.27 (2) |
D7—C4—D9 | 108.736 (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)6 | β = 90.02 (5)° |
Mr = 180.38 | γ = 90.17 (2)° |
Triclinic, P1 | V = 240.47 (2) Å3 |
a = 6.211 (2) Å | Z = 1 |
b = 6.219 (3) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2257 (19) Å | T = 125 K |
α = 90.00 (4)° | ?, ? × ? × ? mm |
Data collection top
Radiation source: nuclear reactor | 2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05° |
Refinement top
Least-squares matrix: full | 3249 data points |
Rp = 0.072 | Profile 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 = 0.096 | 13 parameters |
Rexp = 0.032 | 0 restraints |
R(F2) = 0.12846 | (Δ/σ)max = 4.58 |
χ2 = 21.252 | Background 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)6 | β = 90.02 (5)° |
Mr = 180.38 | γ = 90.17 (2)° |
Triclinic, P1 | V = 240.47 (2) Å3 |
a = 6.211 (2) Å | Z = 1 |
b = 6.219 (3) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2257 (19) Å | T = 125 K |
α = 90.00 (4)° | ?, ? × ? × ? mm |
Refinement top
Rp = 0.072 | 3249 data points |
Rwp = 0.096 | 13 parameters |
Rexp = 0.032 | 0 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
x | y | z | Uiso*/Ueq | ||
C1 | 0.43326 | 0.38278 | 0.68151 | 0.01133* | |
C2 | 0.61682 | 0.32033 | 0.56359 | 0.02823* | |
C3 | 0.68292 | 0.43816 | 0.38074 | 0.00399* | |
C4 | 0.35637 | 0.25071 | 0.87303 | 0.0152* | |
C5 | 0.75184 | 0.13106 | 0.64031 | 0.02162* | |
C6 | 0.87607 | 0.35584 | 0.24891 | 0.03908* | |
D7 | 0.186 | 0.26093 | 0.89557 | 0.0698* | |
D8 | 0.42472 | 0.30481 | 1.02228 | 0.05633* | |
D9 | 0.398 | 0.0886 | 0.85071 | 0.04026* | |
D10 | 0.74229 | 0.10025 | 0.8093 | 0.03802* | |
D11 | 0.9196 | 0.15669 | 0.60815 | 0.06314* | |
D12 | 0.711 | −0.00779 | 0.54984 | 0.05312* | |
D13 | 1.0264 | 0.4244 | 0.3059 | 0.07668* | |
D14 | 0.85621 | 0.40271 | 0.08078 | 0.03899* | |
D15 | 0.88495 | 0.17802 | 0.25039 | 0.03555* |
Geometric parameters (Å, º) top
C1—C2 | 1.4115 (6) | D8—C4 | 1.0751 (4) |
C1—C3i | 1.3841 (6) | D8—D7 | 1.7005 (7) |
C1—C4 | 1.5239 (7) | D8—D9 | 1.7249 (8) |
C2—C1 | 1.4115 (6) | D9—C4 | 1.0508 (5) |
C2—C3 | 1.4142 (6) | D9—D7 | 1.7230 (6) |
C2—C5 | 1.5239 (7) | D9—D8 | 1.7249 (8) |
C3—C1i | 1.3841 (6) | D10—C5 | 1.0710 (4) |
C3—C2 | 1.4142 (6) | D10—D11 | 1.7037 (8) |
C3—C6 | 1.5424 (7) | D10—D12 | 1.7600 (7) |
C4—C1 | 1.5239 (7) | D11—C5 | 1.0724 (4) |
C4—D7 | 1.0695 (4) | D11—D10 | 1.7037 (8) |
C4—D8 | 1.0751 (4) | D11—D12 | 1.6877 (6) |
C4—D9 | 1.0508 (5) | D12—C5 | 1.0611 (5) |
C5—C2 | 1.5239 (7) | D12—D10 | 1.7600 (7) |
C5—D10 | 1.0710 (4) | D12—D11 | 1.6877 (6) |
C5—D11 | 1.0724 (4) | D13—C6 | 1.0848 (4) |
C5—D12 | 1.0611 (5) | D13—D14 | 1.7601 (8) |
C6—C3 | 1.5424 (7) | D13—D15 | 1.7975 (8) |
C6—D13 | 1.0848 (4) | D14—C6 | 1.0935 (4) |
C6—D14 | 1.0935 (4) | D14—D13 | 1.7601 (8) |
C6—D15 | 1.1075 (6) | D14—D15 | 1.7609 (9) |
D7—C4 | 1.0695 (4) | D15—C6 | 1.1075 (6) |
D7—D8 | 1.7005 (7) | D15—D13 | 1.7975 (8) |
D7—D9 | 1.7230 (6) | D15—D14 | 1.7609 (9) |
C2—C1—C3i | 119.95 (3) | D8—C4—D9 | 108.46 (4) |
C2—C1—C4 | 120.72 (3) | C2—C5—D10 | 114.55 (4) |
C3i—C1—C4 | 119.30 (3) | C2—C5—D11 | 111.30 (3) |
C1—C2—C3 | 120.65 (3) | C2—C5—D12 | 109.37 (4) |
C1—C2—C5 | 119.75 (3) | D10—C5—D11 | 105.28 (4) |
C3—C2—C5 | 119.53 (3) | D10—C5—D12 | 111.28 (4) |
C1i—C3—C2 | 119.40 (3) | D11—C5—D12 | 104.57 (3) |
C1i—C3—C6 | 121.73 (3) | C3—C6—D13 | 111.40 (3) |
C2—C3—C6 | 118.78 (3) | C3—C6—D14 | 109.43 (3) |
C1—C4—D7 | 112.30 (4) | C3—C6—D15 | 111.60 (3) |
C1—C4—D8 | 112.63 (3) | D13—C6—D14 | 107.80 (4) |
C1—C4—D9 | 109.63 (4) | D13—C6—D15 | 110.15 (3) |
D7—C4—D8 | 104.92 (4) | D14—C6—D15 | 106.27 (4) |
D7—C4—D9 | 108.70 (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)6 | β = 90.02 (2)° |
Mr = 180.38 | γ = 90.139 (16)° |
Triclinic, P1 | V = 240.88 (3) Å3 |
a = 6.2157 (12) Å | Z = 1 |
b = 6.2221 (18) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2284 (12) Å | T = 129 K |
α = 90.00 (2)° | ?, ? × ? × ? mm |
Data collection top
Radiation source: nuclear reactor | 2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05° |
Refinement top
Least-squares matrix: full | 3249 data points |
Rp = 0.068 | Profile 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 = 0.090 | 9 parameters |
Rexp = 0.032 | 0 restraints |
R(F2) = 0.11030 | (Δ/σ)max = 0.07 |
χ2 = 7.784 | Background 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)6 | β = 90.02 (2)° |
Mr = 180.38 | γ = 90.139 (16)° |
Triclinic, P1 | V = 240.88 (3) Å3 |
a = 6.2157 (12) Å | Z = 1 |
b = 6.2221 (18) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2284 (12) Å | T = 129 K |
α = 90.00 (2)° | ?, ? × ? × ? mm |
Refinement top
Rp = 0.068 | χ2 = 7.784 |
Rwp = 0.090 | 3249 data points |
Rexp = 0.032 | 9 parameters |
R(F2) = 0.11030 | 0 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
C1 | 0.43326 | 0.38278 | 0.68151 | 0.02513* | |
C2 | 0.61682 | 0.32033 | 0.56359 | 0.02259* | |
C3 | 0.68292 | 0.43816 | 0.38074 | 0.0169* | |
C4 | 0.35637 | 0.25071 | 0.87303 | 0.01106* | |
C5 | 0.75184 | 0.13106 | 0.64031 | 0.02248* | |
C6 | 0.87607 | 0.35584 | 0.24891 | 0.0286* | |
D7 | 0.186 | 0.26093 | 0.89557 | 0.01953* | |
D8 | 0.42472 | 0.30481 | 1.02228 | 0.02566* | |
D9 | 0.398 | 0.0886 | 0.85071 | 0.05281* | |
D10 | 0.74229 | 0.10025 | 0.8093 | 0.07166* | |
D11 | 0.9196 | 0.15669 | 0.60815 | 0.02249* | |
D12 | 0.711 | −0.00779 | 0.54984 | 0.14009* | |
D13 | 1.0264 | 0.4244 | 0.3059 | 0.07702* | |
D14 | 0.85621 | 0.40271 | 0.08078 | 0.05327* | |
D15 | 0.88495 | 0.17802 | 0.25039 | 0.06147* |
Geometric parameters (Å, º) top
C1—C2 | 1.4124 (3) | D8—C4 | 1.0757 (2) |
C1—C3i | 1.3845 (3) | D8—D7 | 1.7019 (4) |
C1—C4 | 1.5248 (4) | D8—D9 | 1.7257 (5) |
C2—C1 | 1.4124 (3) | D9—C4 | 1.0512 (3) |
C2—C3 | 1.4151 (3) | D9—D7 | 1.7237 (4) |
C2—C5 | 1.5245 (4) | D9—D8 | 1.7257 (5) |
C3—C1i | 1.3845 (3) | D10—C5 | 1.0715 (2) |
C3—C2 | 1.4151 (3) | D10—D11 | 1.7049 (4) |
C3—C6 | 1.5432 (3) | D10—D12 | 1.7608 (4) |
C4—C1 | 1.5248 (4) | D11—C5 | 1.0734 (2) |
C4—D7 | 1.0703 (2) | D11—D10 | 1.7049 (4) |
C4—D8 | 1.0757 (2) | D11—D12 | 1.6892 (4) |
C4—D9 | 1.0512 (3) | D12—C5 | 1.0617 (3) |
C5—C2 | 1.5245 (4) | D12—D10 | 1.7608 (4) |
C5—D10 | 1.0715 (2) | D12—D11 | 1.6892 (4) |
C5—D11 | 1.0734 (2) | D13—C6 | 1.0858 (2) |
C5—D12 | 1.0617 (3) | D13—D14 | 1.7611 (4) |
C6—C3 | 1.5432 (3) | D13—D15 | 1.7988 (4) |
C6—D13 | 1.0858 (2) | D14—C6 | 1.0940 (2) |
C6—D14 | 1.0940 (2) | D14—D13 | 1.7611 (4) |
C6—D15 | 1.1080 (3) | D14—D15 | 1.7617 (5) |
D7—C4 | 1.0703 (2) | D15—C6 | 1.1080 (3) |
D7—D8 | 1.7019 (4) | D15—D13 | 1.7988 (4) |
D7—D9 | 1.7237 (4) | D15—D14 | 1.7617 (5) |
C2—C1—C3i | 119.939 (15) | D8—C4—D9 | 108.46 (2) |
C2—C1—C4 | 120.741 (17) | C2—C5—D10 | 114.554 (19) |
C3i—C1—C4 | 119.288 (18) | C2—C5—D11 | 111.289 (16) |
C1—C2—C3 | 120.662 (17) | C2—C5—D12 | 109.355 (19) |
C1—C2—C5 | 119.745 (15) | D10—C5—D11 | 105.28 (2) |
C3—C2—C5 | 119.519 (18) | D10—C5—D12 | 111.265 (19) |
C1i—C3—C2 | 119.397 (18) | D11—C5—D12 | 104.594 (17) |
C1i—C3—C6 | 121.723 (15) | C3—C6—D13 | 111.420 (17) |
C2—C3—C6 | 118.797 (17) | C3—C6—D14 | 109.431 (18) |
C1—C4—D7 | 112.321 (18) | C3—C6—D15 | 111.571 (17) |
C1—C4—D8 | 112.607 (16) | D13—C6—D14 | 107.79 (2) |
C1—C4—D9 | 109.63 (2) | D13—C6—D15 | 110.160 (16) |
D7—C4—D8 | 104.943 (19) | D14—C6—D15 | 106.27 (2) |
D7—C4—D9 | 108.679 (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)6 | β = 90.03 (3)° |
Mr = 180.38 | γ = 90.12 (3)° |
Triclinic, P1 | V = 240.98 (2) Å3 |
a = 6.2183 (19) Å | Z = 1 |
b = 6.222 (3) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2281 (18) Å | T = 132 K |
α = 90.01 (4)° | ?, ? × ? × ? mm |
Data collection top
Radiation source: nuclear reactor | 2θmin = 0.263°, 2θmax = 162.663°, 2θstep = 0.05° |
Refinement top
Least-squares matrix: full | 3249 data points |
Rp = 0.068 | Profile 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 = 0.091 | 7 parameters |
Rexp = 0.032 | 0 restraints |
R(F2) = 0.12625 | (Δ/σ)max < 0.001 |
χ2 = 19.184 | Background 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)6 | β = 90.03 (3)° |
Mr = 180.38 | γ = 90.12 (3)° |
Triclinic, P1 | V = 240.98 (2) Å3 |
a = 6.2183 (19) Å | Z = 1 |
b = 6.222 (3) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 6.2281 (18) Å | T = 132 K |
α = 90.01 (4)° | ?, ? × ? × ? mm |
Refinement top
Rp = 0.068 | χ2 = 19.184 |
Rwp = 0.091 | 3249 data points |
Rexp = 0.032 | 7 parameters |
R(F2) = 0.12625 | 0 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
C1 | 0.43326 | 0.38278 | 0.68151 | 0.03057* | |
C2 | 0.61682 | 0.32033 | 0.56359 | 0.02376* | |
C3 | 0.68292 | 0.43816 | 0.38074 | 0.01994* | |
C4 | 0.35637 | 0.25071 | 0.87303 | 0.01642* | |
C5 | 0.75184 | 0.13106 | 0.64031 | 0.02296* | |
C6 | 0.87607 | 0.35584 | 0.24891 | 0.03332* | |
D7 | 0.186 | 0.26093 | 0.89557 | 0.02279* | |
D8 | 0.42472 | 0.30481 | 1.02228 | 0.02466* | |
D9 | 0.398 | 0.0886 | 0.85071 | 0.05788* | |
D10 | 0.74229 | 0.10025 | 0.8093 | 0.08336* | |
D11 | 0.9196 | 0.15669 | 0.60815 | 0.02077* | |
D12 | 0.711 | −0.00779 | 0.54984 | 0.11643* | |
D13 | 1.0264 | 0.4244 | 0.3059 | 0.09469* | |
D14 | 0.85621 | 0.40271 | 0.08078 | 0.05923* | |
D15 | 0.88495 | 0.17802 | 0.25039 | 0.0581* |
Geometric parameters (Å, º) top
C1—C2 | 1.4127 (5) | D8—C4 | 1.0757 (4) |
C1—C3i | 1.3845 (5) | D8—D7 | 1.7024 (6) |
C1—C4 | 1.5251 (6) | D8—D9 | 1.7257 (7) |
C2—C1 | 1.4127 (5) | D9—C4 | 1.0511 (4) |
C2—C3 | 1.4152 (5) | D9—D7 | 1.7239 (6) |
C2—C5 | 1.5244 (6) | D9—D8 | 1.7257 (7) |
C3—C1i | 1.3845 (5) | D10—C5 | 1.0715 (3) |
C3—C2 | 1.4152 (5) | D10—D11 | 1.7054 (6) |
C3—C6 | 1.5436 (5) | D10—D12 | 1.7607 (6) |
C4—C1 | 1.5251 (6) | D11—C5 | 1.0739 (3) |
C4—D7 | 1.0708 (3) | D11—D10 | 1.7054 (6) |
C4—D8 | 1.0757 (4) | D11—D12 | 1.6899 (6) |
C4—D9 | 1.0511 (4) | D12—C5 | 1.0617 (4) |
C5—C2 | 1.5244 (6) | D12—D10 | 1.7607 (6) |
C5—D10 | 1.0715 (3) | D12—D11 | 1.6899 (6) |
C5—D11 | 1.0739 (3) | D13—C6 | 1.0862 (4) |
C5—D12 | 1.0617 (4) | D13—D14 | 1.7612 (6) |
C6—C3 | 1.5436 (5) | D13—D15 | 1.7993 (7) |
C6—D13 | 1.0862 (4) | D14—C6 | 1.0940 (4) |
C6—D14 | 1.0940 (4) | D14—D13 | 1.7612 (6) |
C6—D15 | 1.1080 (5) | D14—D15 | 1.7617 (7) |
D7—C4 | 1.0708 (3) | D15—C6 | 1.1080 (5) |
D7—D8 | 1.7024 (6) | D15—D13 | 1.7993 (7) |
D7—D9 | 1.7239 (6) | D15—D14 | 1.7617 (7) |
C2—C1—C3i | 119.94 (2) | D8—C4—D9 | 108.46 (3) |
C2—C1—C4 | 120.76 (3) | C2—C5—D10 | 114.55 (3) |
C3i—C1—C4 | 119.27 (3) | C2—C5—D11 | 111.29 (3) |
C1—C2—C3 | 120.68 (3) | C2—C5—D12 | 109.35 (3) |
C1—C2—C5 | 119.75 (2) | D10—C5—D11 | 105.29 (3) |
C3—C2—C5 | 119.50 (3) | D10—C5—D12 | 111.25 (3) |
C1i—C3—C2 | 119.38 (3) | D11—C5—D12 | 104.61 (3) |
C1i—C3—C6 | 121.72 (2) | C3—C6—D13 | 111.45 (3) |
C2—C3—C6 | 118.81 (3) | C3—C6—D14 | 109.43 (3) |
C1—C4—D7 | 112.35 (3) | C3—C6—D15 | 111.55 (3) |
C1—C4—D8 | 112.59 (2) | D13—C6—D14 | 107.77 (3) |
C1—C4—D9 | 109.63 (3) | D13—C6—D15 | 110.17 (3) |
D7—C4—D8 | 104.95 (3) | D14—C6—D15 | 106.27 (3) |
D7—C4—D9 | 108.67 (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)6 | β = 98.460 (12)° |
Mr = 180.38 | γ = 100.057 (11)° |
Triclinic, P1 | V = 241.36 (6) Å3 |
a = 5.2360 (8) Å | Z = 1 |
b = 6.1845 (8) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 7.952 (1) Å | T = 140 K |
α = 103.816 (12)° | ?, ? × ? × ? mm |
Data collection top
Radiation source: nuclear reactor | 2θmin = 0.758°, 2θmax = 163.158°, 2θstep = 0.05° |
Refinement top
Least-squares matrix: full | 3249 data points |
Rp = 0.060 | Profile 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 = 0.081 | 9 parameters |
Rexp = 0.032 | 0 restraints |
R(F2) = 0.15460 | (Δ/σ)max = 0.07 |
χ2 = 7.398 | Background 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)6 | β = 98.460 (12)° |
Mr = 180.38 | γ = 100.057 (11)° |
Triclinic, P1 | V = 241.36 (6) Å3 |
a = 5.2360 (8) Å | Z = 1 |
b = 6.1845 (8) Å | Monchromatic beam radiation, λ = 1.594 Å |
c = 7.952 (1) Å | T = 140 K |
α = 103.816 (12)° | ?, ? × ? × ? mm |
Refinement top
Rp = 0.060 | χ2 = 7.398 |
Rwp = 0.081 | 3249 data points |
Rexp = 0.032 | 9 parameters |
R(F2) = 0.15460 | 0 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
C1 | −0.56464 | −0.61622 | 0.31929 | 0.00703* | |
C2 | −0.67816 | −0.43311 | 0.38692 | 0.02147* | |
C3 | −0.61462 | −0.31543 | 0.56751 | 0.0305* | |
C4 | −0.64705 | −0.74811 | 0.12358 | 0.01857* | |
C5 | −0.87358 | −0.35454 | 0.26333 | 0.01904* | |
C6 | −0.75282 | −0.1249 | 0.63785 | 0.03363* | |
D7 | −0.50743 | −0.68752 | 0.05756 | 0.03729* | |
D8 | −0.82479 | −0.70309 | 0.06974 | 0.11386* | |
D9 | −0.68162 | −0.92296 | 0.11284 | 0.07042* | |
D10 | −0.86959 | −0.17877 | 0.31978 | 0.11099* | |
D11 | −0.06306 | −0.4407 | 0.25243 | 0.06375* | |
D12 | −0.81648 | −0.3789 | 0.1412 | 0.06264* | |
D13 | −0.95271 | −0.17761 | 0.57953 | 0.07353* | |
D14 | −0.64922 | 0.02753 | 0.62018 | 0.04368* | |
D15 | −0.71106 | −0.07869 | 0.77974 | 0.04463* |
Geometric parameters (Å, º) top
C1—C2 | 1.4012 (2) | D8—C4 | 1.0757 (2) |
C1—C3i | 1.3935 (2) | D8—D7 | 1.6661 (2) |
C1—C4 | 1.5319 (3) | D8—D9 | 1.7411 (2) |
C1—D7 | 2.0993 (3) | D8—D12 | 1.9398 (3) |
C2—C1 | 1.4012 (2) | D9—C4 | 1.0452 (2) |
C2—C3 | 1.4065 (2) | D9—D7 | 1.7621 (2) |
C2—C5 | 1.5346 (2) | D9—D8 | 1.7411 (2) |
C3—C1i | 1.3935 (2) | D10—C5 | 1.0677 (2) |
C3—C2 | 1.4065 (2) | D10—D11ii | 1.6703 (3) |
C3—C6 | 1.5255 (2) | D10—D12 | 1.7386 (3) |
C3—D13 | 2.0994 (3) | D11—C5iii | 1.0217 (2) |
C4—C1 | 1.5319 (3) | D11—D10iii | 1.6703 (3) |
C4—D7 | 1.0304 (1) | D11—D12iii | 1.7090 (2) |
C4—D8 | 1.0757 (2) | D12—C5 | 1.0424 (1) |
C4—D9 | 1.0452 (2) | D12—D8 | 1.9398 (3) |
C5—C2 | 1.5346 (2) | D12—D10 | 1.7386 (3) |
C5—D10 | 1.0677 (2) | D12—D11ii | 1.7090 (2) |
C5—D11ii | 1.0217 (2) | D13—C3 | 2.0994 (3) |
C5—D12 | 1.0424 (1) | D13—C6 | 1.0405 (2) |
C6—C3 | 1.5255 (2) | D13—D14 | 1.7855 (3) |
C6—D13 | 1.0405 (2) | D13—D15 | 1.7837 (3) |
C6—D14 | 1.0535 (2) | D14—C6 | 1.0535 (2) |
C6—D15 | 1.0743 (2) | D14—D13 | 1.7855 (3) |
D7—C1 | 2.0993 (3) | D14—D15 | 1.6097 (2) |
D7—C4 | 1.0304 (1) | D15—C6 | 1.0743 (2) |
D7—D8 | 1.6661 (2) | D15—D13 | 1.7837 (3) |
D7—D9 | 1.7621 (2) | D15—D14 | 1.6097 (2) |
C2—C1—C3i | 119.673 (11) | D8—C4—D9 | 110.352 (12) |
C2—C1—C4 | 120.205 (10) | C2—C5—D10 | 108.938 (13) |
C3i—C1—C4 | 120.056 (10) | C2—C5—D11ii | 110.885 (11) |
C1—C2—C3 | 121.372 (10) | C2—C5—D12 | 108.120 (10) |
C1—C2—C5 | 120.182 (11) | D10—C5—D11ii | 106.135 (13) |
C3—C2—C5 | 118.441 (10) | D10—C5—D12 | 110.962 (11) |
C1i—C3—C2 | 118.954 (10) | D11ii—C5—D12 | 111.782 (13) |
C1i—C3—C6 | 121.115 (10) | C3—C6—D13 | 108.318 (13) |
C2—C3—C6 | 119.847 (10) | C3—C6—D14 | 108.172 (11) |
C1—C4—D7 | 108.440 (13) | C3—C6—D15 | 109.511 (11) |
C1—C4—D8 | 107.995 (12) | D13—C6—D14 | 117.010 (11) |
C1—C4—D9 | 108.967 (13) | D13—C6—D15 | 115.003 (12) |
D7—C4—D8 | 104.555 (11) | D14—C6—D15 | 98.309 (14) |
D7—C4—D9 | 116.201 (10) |
Symmetry codes: (i) −x−1, −y−1, −z+1; (ii) x−1, 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 formula | C6(CD3)6 | C6(CD3)6 | C6(CD3)6 | C6(CD3)6 |
Mr | 180.38 | 180.38 | 180.38 | 180.38 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 5K | 80 | 110 | 125 |
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) |
V (Å3) | 237.15 (1) | 238.50 (2) | 239.81 (2) | 240.47 (2) |
Z | 1 | 1 | 1 | 1 |
Radiation type | Monchromatic beam, λ = 1.594 Å | Monchromatic beam, λ = 1.594 Å | Monchromatic beam, λ = 1.594 Å | Monchromatic 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 = 0.05 | 2θmin = 0.283 2θmax = 162.683 2θstep = 0.05 | 2θmin = 0.283 2θmax = 162.683 2θstep = 0.05 | 2θmin = 0.263 2θmax = 162.663 2θstep = 0.05 |
Refinement | ||||
R factors and goodness of fit | Rp = 0.066, Rwp = 0.090, Rexp = 0.023, R(F2) = 0.09220, χ2 = 15.210 | Rp = 0.068, Rwp = 0.088, Rexp = 0.032, R(F2) = 0.11334, χ2 = 19.714 | Rp = 0.065, Rwp = 0.085, Rexp = 0.032, R(F2) = 0.11121, χ2 = 19.360 | Rp = 0.072, Rwp = 0.096, Rexp = 0.032, R(F2) = 0.12846, χ2 = 21.252 |
No. of data points | 3249 | 3249 | 3249 | 3249 |
No. of parameters | 10 | 7 | 8 | 13 |
(Δ/σ)max | 5.80 | 0.03 | 0.06 | 4.58 |
(HMB_129_REDO_publ) | (HMB_132_REDO_publ) | (HMB_publ) | |
Crystal data | |||
Chemical formula | C6(CD3)6 | C6(CD3)6 | C6(CD3)6 |
Mr | 180.38 | 180.38 | 180.38 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 129 | 132 | 140 |
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) |
V (Å3) | 240.88 (3) | 240.98 (2) | 241.36 (6) |
Z | 1 | 1 | 1 |
Radiation type | Monchromatic beam, λ = 1.594 Å | Monchromatic beam, λ = 1.594 Å | Monchromatic 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 = 0.05 | 2θmin = 0.263 2θmax = 162.663 2θstep = 0.05 | 2θmin = 0.758 2θmax = 163.158 2θstep = 0.05 |
Refinement | |||
R factors and goodness of fit | Rp = 0.068, Rwp = 0.090, Rexp = 0.032, R(F2) = 0.11030, χ2 = 7.784 | Rp = 0.068, Rwp = 0.091, Rexp = 0.032, R(F2) = 0.12625, χ2 = 19.184 | Rp = 0.060, Rwp = 0.081, Rexp = 0.032, R(F2) = 0.15460, χ2 = 7.398 |
No. of data points | 3249 | 3249 | 3249 |
No. of parameters | 9 | 7 | 9 |
(Δ/σ)max | 0.07 | < 0.001 | 0.07 |
Computer programs: GSAS.