
Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768102018797/bm0050sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S0108768102018797/bm0050sup2.hkl |
![]() | Portable Document Format (PDF) file https://doi.org/10.1107/S0108768102018797/bm0050sup3.pdf |
CCDC reference: 201623
Data collection: Bruker SMART; cell refinement: Bruker SMART; data reduction: Bruker SHELXTL; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.
PhOH | F(000) = 300 |
Mr = 94.11 | Dx = 1.240 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.610 (4) Å | Cell parameters from 331 reflections |
b = 5.4416 (11) Å | θ = 2.5–25.5° |
c = 12.217 (5) Å | µ = 0.08 mm−1 |
β = 101.47 (3)° | T = 293 K |
V = 756.4 (4) Å3 | × × mm |
Z = 6 |
CCD area detector diffractometer | 455 independent reflections |
Radiation source: fine-focus sealed tube | 269 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
phi and ω scans | θmax = 24.9°, θmin = 2.7° |
Absorption correction: SADABS ? | h = −12→12 |
Tmin = 0.213, Tmax = 1.000 | k = −6→6 |
1129 measured reflections | l = −7→7 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.086 | w = 1/[σ2(Fo2) + (0.1876P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.278 | (Δ/σ)max = 0.002 |
S = 0.98 | Δρmax = 0.32 e Å−3 |
455 reflections | Δρmin = −0.20 e Å−3 |
29 parameters | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
14 restraints | Absolute structure parameter: 0 (10) |
PhOH | V = 756.4 (4) Å3 |
Mr = 94.11 | Z = 6 |
Monoclinic, P21 | Mo Kα radiation |
a = 11.610 (4) Å | µ = 0.08 mm−1 |
b = 5.4416 (11) Å | T = 293 K |
c = 12.217 (5) Å | × × mm |
β = 101.47 (3)° |
CCD area detector diffractometer | 455 independent reflections |
Absorption correction: SADABS ? | 269 reflections with I > 2σ(I) |
Tmin = 0.213, Tmax = 1.000 | Rint = 0.057 |
1129 measured reflections |
R[F2 > 2σ(F2)] = 0.086 | 14 restraints |
wR(F2) = 0.278 | Δρmax = 0.32 e Å−3 |
S = 0.98 | Δρmin = −0.20 e Å−3 |
455 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
29 parameters | Absolute structure parameter: 0 (10) |
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. |
x | y | z | Uiso*/Ueq | ||
O1A | 0.7050 (10) | 0.4386 (19) | 0.3000 (15) | 0.0583 (15)* | |
H1A | 0.6716 | 0.3230 | 0.3235 | 0.087* | |
C2A | 0.6911 (8) | 0.4219 (16) | 0.1876 (15) | 0.0583 (15)* | |
C3A | 0.6275 (9) | 0.2301 (18) | 0.1293 (17) | 0.0583 (15)* | |
H3A | 0.5935 | 0.1113 | 0.1675 | 0.070* | |
C4A | 0.6146 (10) | 0.216 (2) | 0.0139 (17) | 0.0583 (15)* | |
H4A | 0.5721 | 0.0877 | −0.0251 | 0.070* | |
C5A | 0.6654 (11) | 0.394 (3) | −0.0432 (15) | 0.0583 (15)* | |
H5A | 0.6568 | 0.3842 | −0.1204 | 0.070* | |
C6A | 0.7290 (11) | 0.585 (3) | 0.0150 (15) | 0.0583 (15)* | |
H6A | 0.7629 | 0.7043 | −0.0232 | 0.070* | |
C7A | 0.7418 (9) | 0.5996 (18) | 0.1304 (15) | 0.0583 (15)* | |
H7A | 0.7844 | 0.7279 | 0.1694 | 0.070* | |
O1B | 0.6823 (10) | 0.937 (2) | 0.3864 (14) | 0.0583 (15)* | |
H1B | 0.7209 | 0.8193 | 0.3720 | 0.087* | |
C2B | 0.6694 (11) | 0.923 (2) | 0.4937 (14) | 0.0583 (15)* | |
C3B | 0.7169 (10) | 0.726 (2) | 0.5603 (15) | 0.0583 (15)* | |
H3B | 0.7597 | 0.6059 | 0.5317 | 0.070* | |
C4B | 0.7005 (9) | 0.709 (3) | 0.6697 (15) | 0.0583 (15)* | |
H4B | 0.7322 | 0.5776 | 0.7143 | 0.070* | |
C5B | 0.6366 (10) | 0.889 (3) | 0.7124 (14) | 0.0583 (15)* | |
H5B | 0.6256 | 0.8773 | 0.7856 | 0.070* | |
C6B | 0.5891 (9) | 1.085 (3) | 0.6458 (14) | 0.0583 (15)* | |
H6B | 0.5463 | 1.2053 | 0.6744 | 0.070* | |
C7B | 0.6055 (10) | 1.102 (2) | 0.5364 (14) | 0.0583 (15)* | |
H7B | 0.5737 | 1.2337 | 0.4918 | 0.070* | |
O1C | 1.0164 (12) | 0.860 (2) | 0.4541 (16) | 0.0583 (15)* | |
H1C | 0.9818 | 0.9714 | 0.4791 | 0.087* | |
C2C | 1.0088 (13) | 0.893 (2) | 0.3444 (13) | 0.0583 (15)* | |
C3C | 0.9567 (10) | 1.0874 (15) | 0.2791 (17) | 0.0583 (15)* | |
H3C | 0.9167 | 1.2084 | 0.3103 | 0.070* | |
C4C | 0.9644 (10) | 1.101 (2) | 0.1671 (16) | 0.0583 (15)* | |
H4C | 0.9295 | 1.2314 | 0.1235 | 0.070* | |
C5C | 1.0241 (12) | 0.920 (4) | 0.1205 (13) | 0.0583 (15)* | |
H5C | 1.0293 | 0.9295 | 0.0456 | 0.070* | |
C6C | 1.0762 (10) | 0.726 (3) | 0.1858 (17) | 0.0583 (15)* | |
H6C | 1.1162 | 0.6046 | 0.1546 | 0.070* | |
C7C | 1.0686 (11) | 0.7119 (15) | 0.2977 (16) | 0.0583 (15)* | |
H7C | 1.1034 | 0.5817 | 0.3414 | 0.070* |
O1A—C2A | 1.354 (15) | C4B—C5B | 1.3900 |
C2A—C3A | 1.3900 | C5B—C6B | 1.3900 |
C2A—C7A | 1.3900 | C6B—C7B | 1.3900 |
C3A—C4A | 1.3900 | O1C—C2C | 1.338 (17) |
C4A—C5A | 1.3900 | C2C—C3C | 1.3900 |
C5A—C6A | 1.3900 | C2C—C7C | 1.3900 |
C6A—C7A | 1.3900 | C3C—C4C | 1.3900 |
O1B—C2B | 1.351 (16) | C4C—C5C | 1.3900 |
C2B—C3B | 1.3900 | C5C—C6C | 1.3900 |
C2B—C7B | 1.3900 | C6C—C7C | 1.3900 |
C3B—C4B | 1.3900 | ||
O1A—C2A—C3A | 120.9 (7) | C5B—C4B—C3B | 120.0 |
O1A—C2A—C7A | 119.1 (7) | C4B—C5B—C6B | 120.0 |
C3A—C2A—C7A | 120.0 | C7B—C6B—C5B | 120.0 |
C4A—C3A—C2A | 120.0 | C6B—C7B—C2B | 120.0 |
C3A—C4A—C5A | 120.0 | O1C—C2C—C3C | 127.7 (14) |
C6A—C5A—C4A | 120.0 | O1C—C2C—C7C | 112.1 (14) |
C7A—C6A—C5A | 120.0 | C3C—C2C—C7C | 120.0 |
C6A—C7A—C2A | 120.0 | C2C—C3C—C4C | 120.0 |
O1B—C2B—C3B | 120.3 (7) | C5C—C4C—C3C | 120.0 |
O1B—C2B—C7B | 119.6 (7) | C6C—C5C—C4C | 120.0 |
C3B—C2B—C7B | 120.0 | C5C—C6C—C7C | 120.0 |
C2B—C3B—C4B | 120.0 | C6C—C7C—C2C | 120.0 |
Experimental details
Crystal data | |
Chemical formula | PhOH |
Mr | 94.11 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 293 |
a, b, c (Å) | 11.610 (4), 5.4416 (11), 12.217 (5) |
β (°) | 101.47 (3) |
V (Å3) | 756.4 (4) |
Z | 6 |
Radiation type | Mo Kα |
µ (mm−1) | 0.08 |
Crystal size (mm) | × × |
Data collection | |
Diffractometer | CCD area detector diffractometer |
Absorption correction | SADABS |
Tmin, Tmax | 0.213, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1129, 455, 269 |
Rint | 0.057 |
(sin θ/λ)max (Å−1) | 0.592 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.086, 0.278, 0.98 |
No. of reflections | 455 |
No. of parameters | 29 |
No. of restraints | 14 |
Δρmax, Δρmin (e Å−3) | 0.32, −0.20 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0 (10) |
Computer programs: Bruker SMART, Bruker SHELXTL, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997).