Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810603477X/av5069sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810603477X/av50691_34GPasup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810603477X/av50691_98GPasup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810603477X/av50692_45GPasup4.hkl |
CCDC references: 637747; 637748; 637749
For all compounds, data collection: CrysAlis (Oxford Diffraction, 2003); cell refinement: CrysAlis (Oxford Diffraction, 2003); data reduction: CrysAlis (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
C5H10O2 | Dx = 1.300 Mg m−3 |
Mr = 102.13 | Melting point: 198 K |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 4.9347 (10) Å | Cell parameters from 1085 reflections |
b = 9.4163 (19) Å | θ = 3.6–27.3° |
c = 11.321 (2) Å | µ = 0.10 mm−1 |
β = 97.39 (3)° | T = 293 K |
V = 521.70 (18) Å3 | Cylinder, colourless |
Z = 4 | 0.36 × 0.28 × 0.15 mm |
F(000) = 224 |
Kuma KM4CCD κ geometry diffractometer | 316 independent reflections |
Radiation source: fine-focus sealed tube | 259 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.142 |
ω scans | θmax = 27.3°, θmin = 3.6° |
Absorption correction: analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | h = −6→6 |
Tmin = 0.68, Tmax = 0.96 | k = −5→5 |
1838 measured reflections | l = −13→13 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.099 | H-atom parameters constrained |
wR(F2) = 0.270 | w = 1/[σ2(Fo2) + (0.1734P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.25 | (Δ/σ)max < 0.001 |
316 reflections | Δρmax = 0.15 e Å−3 |
60 parameters | Δρmin = −0.16 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.22 (11) |
C5H10O2 | V = 521.70 (18) Å3 |
Mr = 102.13 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 4.9347 (10) Å | µ = 0.10 mm−1 |
b = 9.4163 (19) Å | T = 293 K |
c = 11.321 (2) Å | 0.36 × 0.28 × 0.15 mm |
β = 97.39 (3)° |
Kuma KM4CCD κ geometry diffractometer | 316 independent reflections |
Absorption correction: analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | 259 reflections with I > 2σ(I) |
Tmin = 0.68, Tmax = 0.96 | Rint = 0.142 |
1838 measured reflections |
R[F2 > 2σ(F2)] = 0.099 | 0 restraints |
wR(F2) = 0.270 | H-atom parameters constrained |
S = 1.25 | Δρmax = 0.15 e Å−3 |
316 reflections | Δρmin = −0.16 e Å−3 |
60 parameters |
Experimental. High-pressure measurement at 1.34 GPa. |
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 | ||
O2 | 0.2180 (7) | 0.6154 (7) | 0.3982 (3) | 0.054 (5) | |
O1 | −0.0305 (8) | 0.7862 (8) | 0.3083 (3) | 0.072 (4) | |
C3 | −0.2673 (14) | 0.8538 (13) | 0.5166 (7) | 0.076 (7) | |
H3A | −0.3068 | 0.8661 | 0.5968 | 0.115* | |
H3B | −0.4294 | 0.8232 | 0.4671 | 0.115* | |
H3C | −0.2062 | 0.9423 | 0.4873 | 0.115* | |
C2 | −0.0525 (11) | 0.7463 (11) | 0.5145 (5) | 0.051 (6) | |
H2A | −0.1181 | 0.6576 | 0.5439 | 0.061* | |
H2B | 0.1048 | 0.7754 | 0.5695 | 0.061* | |
C1 | 0.0386 (11) | 0.7196 (12) | 0.3971 (5) | 0.045 (2)* | |
C4 | 0.3291 (12) | 0.5829 (10) | 0.2907 (5) | 0.059 (5) | |
H4A | 0.4110 | 0.6674 | 0.2614 | 0.070* | |
H4B | 0.1844 | 0.5512 | 0.2303 | 0.070* | |
C5 | 0.5350 (10) | 0.4719 (14) | 0.3134 (5) | 0.055 (6) | |
H5A | 0.6090 | 0.4504 | 0.2411 | 0.082* | |
H5B | 0.4529 | 0.3881 | 0.3416 | 0.082* | |
H5C | 0.6789 | 0.5041 | 0.3725 | 0.082* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O2 | 0.059 (3) | 0.068 (16) | 0.039 (4) | 0.011 (3) | 0.019 (2) | 0.002 (2) |
O1 | 0.077 (3) | 0.090 (13) | 0.054 (3) | 0.029 (4) | 0.025 (2) | 0.022 (3) |
C3 | 0.057 (4) | 0.11 (2) | 0.069 (6) | 0.008 (5) | 0.033 (3) | 0.007 (5) |
C2 | 0.062 (4) | 0.05 (2) | 0.044 (4) | 0.016 (5) | 0.019 (3) | 0.013 (4) |
C4 | 0.063 (4) | 0.08 (2) | 0.034 (4) | −0.005 (5) | 0.025 (3) | −0.011 (3) |
C5 | 0.053 (4) | 0.06 (2) | 0.060 (4) | 0.010 (4) | 0.024 (3) | −0.002 (4) |
O2—C1 | 1.320 (11) | C3—C2 | 1.468 (12) |
O2—C4 | 1.431 (6) | C2—C1 | 1.479 (8) |
O1—C1 | 1.197 (9) | C4—C5 | 1.457 (12) |
C1—O2—C4 | 118.8 (5) | O1—C1—C2 | 125.4 (9) |
C3—C2—C1 | 115.8 (6) | O2—C1—C2 | 113.5 (6) |
O1—C1—O2 | 121.0 (6) | O2—C4—C5 | 109.7 (5) |
C4—O2—C1—O1 | −0.1 (12) | C3—C2—C1—O2 | −175.6 (8) |
C4—O2—C1—C2 | −177.7 (6) | C1—O2—C4—C5 | 176.2 (7) |
C3—C2—C1—O1 | 6.9 (13) |
C5H10O2 | Dx = 1.319 Mg m−3 |
Mr = 102.13 | Melting point: 198 K |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 4.8917 (10) Å | Cell parameters from 1777 reflections |
b = 9.3649 (19) Å | θ = 2.8–24.8° |
c = 11.318 (2) Å | µ = 0.10 mm−1 |
β = 97.24 (3)° | T = 293 K |
V = 514.35 (18) Å3 | Cylinder, colourless |
Z = 4 | 0.36 × 0.28 × 0.14 mm |
F(000) = 224 |
Kuma KM4CCD κ geometry diffractometer | 283 independent reflections |
Radiation source: fine-focus sealed tube | 264 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.059 |
ω scans | θmax = 24.8°, θmin = 2.8° |
Absorption correction: analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | h = −5→5 |
Tmin = 0.67, Tmax = 0.97 | k = −6→6 |
2054 measured reflections | l = −11→11 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.054 | H-atom parameters constrained |
wR(F2) = 0.107 | w = 1/[σ2(Fo2) + (0.048P)2 + 0.3823P] where P = (Fo2 + 2Fc2)/3 |
S = 1.20 | (Δ/σ)max < 0.001 |
283 reflections | Δρmax = 0.12 e Å−3 |
71 parameters | Δρmin = −0.10 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.02 (2) |
C5H10O2 | V = 514.35 (18) Å3 |
Mr = 102.13 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 4.8917 (10) Å | µ = 0.10 mm−1 |
b = 9.3649 (19) Å | T = 293 K |
c = 11.318 (2) Å | 0.36 × 0.28 × 0.14 mm |
β = 97.24 (3)° |
Kuma KM4CCD κ geometry diffractometer | 283 independent reflections |
Absorption correction: analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | 264 reflections with I > 2σ(I) |
Tmin = 0.67, Tmax = 0.97 | Rint = 0.059 |
2054 measured reflections |
R[F2 > 2σ(F2)] = 0.054 | 0 restraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.20 | Δρmax = 0.12 e Å−3 |
283 reflections | Δρmin = −0.10 e Å−3 |
71 parameters |
Experimental. High-pressure measurement at 1.98 GPa. |
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 | ||
O2 | 0.2191 (5) | 0.6138 (4) | 0.3997 (2) | 0.0326 (16) | |
O1 | −0.0346 (6) | 0.7876 (5) | 0.3074 (3) | 0.048 (2) | |
C3 | −0.2739 (8) | 0.8572 (9) | 0.5161 (4) | 0.038 (3) | |
H3A | −0.3184 | 0.8660 | 0.5960 | 0.057* | |
H3B | −0.4306 | 0.8207 | 0.4655 | 0.057* | |
H3C | −0.2250 | 0.9491 | 0.4877 | 0.057* | |
C2 | −0.0575 (8) | 0.7443 (6) | 0.5151 (3) | 0.037 (3) | |
H2A | 0.0998 | 0.7702 | 0.5720 | 0.045* | |
H2B | −0.1300 | 0.6550 | 0.5413 | 0.045* | |
C1 | 0.0381 (8) | 0.7217 (7) | 0.3969 (4) | 0.028 (3) | |
C4 | 0.3324 (7) | 0.5843 (6) | 0.2900 (3) | 0.030 (2) | |
H4A | 0.4151 | 0.6699 | 0.2618 | 0.036* | |
H4B | 0.1880 | 0.5524 | 0.2291 | 0.036* | |
C5 | 0.5431 (7) | 0.4714 (7) | 0.3152 (3) | 0.029 (2) | |
H5A | 0.6354 | 0.4584 | 0.2459 | 0.044* | |
H5B | 0.4614 | 0.3828 | 0.3349 | 0.044* | |
H5C | 0.6738 | 0.5019 | 0.3808 | 0.044* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O2 | 0.0383 (15) | 0.037 (6) | 0.023 (3) | 0.0107 (19) | 0.0080 (11) | 0.0023 (11) |
O1 | 0.0511 (18) | 0.067 (8) | 0.030 (4) | 0.024 (2) | 0.0143 (14) | 0.0162 (18) |
C3 | 0.038 (2) | 0.033 (12) | 0.045 (4) | 0.004 (3) | 0.0144 (18) | −0.0010 (19) |
C2 | 0.041 (2) | 0.049 (13) | 0.023 (5) | 0.008 (3) | 0.0097 (17) | −0.0027 (17) |
C1 | 0.0259 (18) | 0.031 (12) | 0.027 (4) | −0.008 (3) | 0.0015 (15) | 0.000 (2) |
C4 | 0.0325 (19) | 0.031 (10) | 0.027 (4) | 0.008 (3) | 0.0061 (15) | 0.0010 (17) |
C5 | 0.031 (2) | 0.020 (10) | 0.039 (4) | 0.003 (2) | 0.0094 (16) | −0.0028 (17) |
O2—C1 | 1.341 (6) | C3—C2 | 1.497 (7) |
O2—C4 | 1.449 (4) | C2—C1 | 1.486 (6) |
O1—C1 | 1.202 (6) | C4—C5 | 1.479 (7) |
C1—O2—C4 | 116.5 (3) | O1—C1—C2 | 126.3 (6) |
C1—C2—C3 | 114.2 (4) | O2—C1—C2 | 111.6 (4) |
O1—C1—O2 | 122.1 (4) | O2—C4—C5 | 107.7 (3) |
C4—O2—C1—O1 | 2.6 (6) | C3—C2—C1—O2 | −176.2 (4) |
C4—O2—C1—C2 | −178.4 (3) | C1—O2—C4—C5 | 175.1 (4) |
C3—C2—C1—O1 | 2.7 (7) |
C5H10O2 | Dx = 1.346 Mg m−3 |
Mr = 102.13 | Melting point: 198 K |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 4.8455 (10) Å | Cell parameters from 1559 reflections |
b = 9.3249 (19) Å | θ = 2.9–25.0° |
c = 11.251 (2) Å | µ = 0.10 mm−1 |
β = 97.52 (3)° | T = 293 K |
V = 504.00 (18) Å3 | Cylinder, colourless |
Z = 4 | 0.36 × 0.28 × 0.13 mm |
F(000) = 224 |
Kuma KM4CCD κ geometry diffractometer | 299 independent reflections |
Radiation source: fine-focus sealed tube | 268 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
ω scans | θmax = 25.0°, θmin = 2.9° |
Absorption correction: analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | h = −5→5 |
Tmin = 0.68, Tmax = 0.97 | k = −6→6 |
2119 measured reflections | l = −11→11 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.048 | H-atom parameters constrained |
wR(F2) = 0.119 | w = 1/[σ2(Fo2) + (0.0645P)2 + 0.3573P] where P = (Fo2 + 2Fc2)/3 |
S = 1.14 | (Δ/σ)max < 0.001 |
299 reflections | Δρmax = 0.13 e Å−3 |
71 parameters | Δρmin = −0.14 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.04 (3) |
C5H10O2 | V = 504.00 (18) Å3 |
Mr = 102.13 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 4.8455 (10) Å | µ = 0.10 mm−1 |
b = 9.3249 (19) Å | T = 293 K |
c = 11.251 (2) Å | 0.36 × 0.28 × 0.13 mm |
β = 97.52 (3)° |
Kuma KM4CCD κ geometry diffractometer | 299 independent reflections |
Absorption correction: analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | 268 reflections with I > 2σ(I) |
Tmin = 0.68, Tmax = 0.97 | Rint = 0.047 |
2119 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 0 restraints |
wR(F2) = 0.119 | H-atom parameters constrained |
S = 1.14 | Δρmax = 0.13 e Å−3 |
299 reflections | Δρmin = −0.14 e Å−3 |
71 parameters |
Experimental. High-pressure measurement at 2.45 GPa. |
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 | ||
O2 | 0.2203 (5) | 0.6135 (4) | 0.3999 (2) | 0.0334 (14) | |
O1 | −0.0367 (6) | 0.7880 (5) | 0.3066 (3) | 0.0480 (19) | |
C3 | −0.2768 (8) | 0.8585 (8) | 0.5162 (4) | 0.039 (2) | |
H3A | −0.3290 | 0.8666 | 0.5954 | 0.058* | |
H3B | −0.4342 | 0.8271 | 0.4617 | 0.058* | |
H3C | −0.2154 | 0.9501 | 0.4910 | 0.058* | |
C2 | −0.0585 (7) | 0.7448 (6) | 0.5156 (3) | 0.0369 (19) | |
H2A | 0.1008 | 0.7710 | 0.5729 | 0.044* | |
H2B | −0.1318 | 0.6553 | 0.5422 | 0.044* | |
C1 | 0.0373 (8) | 0.7212 (7) | 0.3967 (4) | 0.032 (2) | |
C4 | 0.3332 (7) | 0.5842 (5) | 0.2896 (3) | 0.032 (2) | |
H4A | 0.4162 | 0.6703 | 0.2614 | 0.038* | |
H4B | 0.1866 | 0.5524 | 0.2283 | 0.038* | |
C5 | 0.5464 (7) | 0.4708 (7) | 0.3147 (3) | 0.034 (2) | |
H5A | 0.6387 | 0.4548 | 0.2454 | 0.051* | |
H5B | 0.4622 | 0.3831 | 0.3365 | 0.051* | |
H5C | 0.6794 | 0.5027 | 0.3802 | 0.051* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O2 | 0.0365 (15) | 0.041 (5) | 0.025 (3) | 0.0102 (17) | 0.0101 (11) | 0.0022 (10) |
O1 | 0.0512 (18) | 0.060 (7) | 0.036 (3) | 0.025 (2) | 0.0150 (15) | 0.0168 (16) |
C3 | 0.037 (2) | 0.033 (9) | 0.050 (4) | 0.003 (3) | 0.0155 (18) | −0.0031 (19) |
C2 | 0.041 (2) | 0.044 (8) | 0.027 (4) | 0.006 (3) | 0.0109 (17) | −0.0009 (17) |
C1 | 0.0270 (19) | 0.041 (10) | 0.028 (5) | −0.007 (3) | 0.0043 (16) | 0.001 (2) |
C4 | 0.0333 (18) | 0.036 (9) | 0.027 (4) | 0.004 (2) | 0.0087 (16) | −0.0004 (15) |
C5 | 0.029 (2) | 0.038 (9) | 0.037 (4) | 0.005 (2) | 0.0091 (15) | −0.0014 (17) |
O2—C1 | 1.337 (6) | C3—C2 | 1.498 (7) |
O2—C4 | 1.445 (4) | C2—C1 | 1.489 (6) |
O1—C1 | 1.204 (6) | C4—C5 | 1.479 (7) |
C1—O2—C4 | 116.3 (3) | O1—C1—C2 | 125.9 (5) |
C1—C2—C3 | 114.4 (4) | O2—C1—C2 | 111.8 (4) |
O1—C1—O2 | 122.3 (4) | O2—C4—C5 | 107.7 (3) |
C4—O2—C1—O1 | 2.1 (6) | C3—C2—C1—O2 | −176.6 (4) |
C4—O2—C1—C2 | −178.2 (3) | C1—O2—C4—C5 | 175.3 (4) |
C3—C2—C1—O1 | 3.1 (7) |
Experimental details
(ethylpropionate1) | (ethylpropionate2) | (ethylpropionate3) | |
Crystal data | |||
Chemical formula | C5H10O2 | C5H10O2 | C5H10O2 |
Mr | 102.13 | 102.13 | 102.13 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 293 | 293 | 293 |
a, b, c (Å) | 4.9347 (10), 9.4163 (19), 11.321 (2) | 4.8917 (10), 9.3649 (19), 11.318 (2) | 4.8455 (10), 9.3249 (19), 11.251 (2) |
β (°) | 97.39 (3) | 97.24 (3) | 97.52 (3) |
V (Å3) | 521.70 (18) | 514.35 (18) | 504.00 (18) |
Z | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.10 | 0.10 | 0.10 |
Crystal size (mm) | 0.36 × 0.28 × 0.15 | 0.36 × 0.28 × 0.14 | 0.36 × 0.28 × 0.13 |
Data collection | |||
Diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer |
Absorption correction | Analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | Analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 | Analytical Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Poznań. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 |
Tmin, Tmax | 0.68, 0.96 | 0.67, 0.97 | 0.68, 0.97 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1838, 316, 259 | 2054, 283, 264 | 2119, 299, 268 |
Rint | 0.142 | 0.059 | 0.047 |
(sin θ/λ)max (Å−1) | 0.646 | 0.590 | 0.594 |
Refinement | |||
R[F2 > 2σ(F2)], wR(F2), S | 0.099, 0.270, 1.25 | 0.054, 0.107, 1.20 | 0.048, 0.119, 1.14 |
No. of reflections | 316 | 283 | 299 |
No. of parameters | 60 | 71 | 71 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.15, −0.16 | 0.12, −0.10 | 0.13, −0.14 |
Computer programs: CrysAlis (Oxford Diffraction, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1990).
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