Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105037766/av5043sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768105037766/av5043tmcs1sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768105037766/av5043tmcs2sup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768105037766/av5043tmcs3sup4.hkl |
CCDC references: 298302; 298303; 298304
For all compounds, data collection: CrysAlis (Oxford Diffraction, 2004); cell refinement: CrysAlis (Oxford Diffraction, 2004); data reduction: CrysAlis (Oxford Diffraction, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
C_{3}H_{9}ClSi | D_{x} = 1.153 Mg m^{−}^{3} |
M_{r} = 108.64 | Melting point: 215 K |
Orthorhombic, Pmn2_{1} | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac -2 | Cell parameters from 839 reflections |
a = 7.785 (2) Å | θ = 4.2–27.4° |
b = 6.43 (3) Å | µ = 0.66 mm^{−}^{1} |
c = 6.254 (3) Å | T = 293 K |
V = 313.0 (15) Å^{3} | Disc, colourless |
Z = 2 | 0.46 × 0.46 × 0.18 × 0.23 (radius) mm |
F(000) = 116 |
Kuma KM4CCD κ geometry diffractometer | 194 independent reflections |
Radiation source: fine-focus sealed tube | 170 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.075 |
ω scans | θ_{max} = 27.4°, θ_{min} = 4.2° |
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 = −10→10 |
T_{min} = 0.41, T_{max} = 0.94 | k = −1→1 |
1793 measured reflections | l = −8→8 |
Refinement on F^{2} | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F^{2} > 2σ(F^{2})] = 0.032 | w = 1/[σ^{2}(F_{o}^{2}) + (0.0568P)^{2}] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
wR(F^{2}) = 0.083 | (Δ/σ)_{max} < 0.001 |
S = 1.01 | Δρ_{max} = 0.08 e Å^{−}^{3} |
194 reflections | Δρ_{min} = −0.11 e Å^{−}^{3} |
29 parameters | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
1 restraint | Extinction coefficient: 0.19 (3) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.6 (3) |
C_{3}H_{9}ClSi | V = 313.0 (15) Å^{3} |
M_{r} = 108.64 | Z = 2 |
Orthorhombic, Pmn2_{1} | Mo Kα radiation |
a = 7.785 (2) Å | µ = 0.66 mm^{−}^{1} |
b = 6.43 (3) Å | T = 293 K |
c = 6.254 (3) Å | 0.46 × 0.46 × 0.18 × 0.23 (radius) mm |
Kuma KM4CCD κ geometry diffractometer | 194 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 | 170 reflections with I > 2σ(I) |
T_{min} = 0.41, T_{max} = 0.94 | R_{int} = 0.075 |
1793 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F^{2}) = 0.083 | Δρ_{max} = 0.08 e Å^{−}^{3} |
S = 1.01 | Δρ_{min} = −0.11 e Å^{−}^{3} |
194 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
29 parameters | Absolute structure parameter: 0.6 (3) |
1 restraint |
Experimental. High-pressure measurement at 0.23 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 F^{2} against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^{2}, conventional R-factors R are based on F, with F set to zero for negative F^{2}. The threshold expression of F^{2} > σ(F^{2}) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^{2} 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 | U_{iso}*/U_{eq} | Occ. (<1) | |
Cl1 | 0.0000 | 0.361 (2) | 0.4727 (5) | 0.153 (13) | |
Si1 | 0.0000 | 0.6592 (17) | 0.3753 (2) | 0.0402 (7)* | |
C1 | 0.0000 | 0.699 (4) | 0.0771 (13) | 0.06 (2) | |
H11 | 0.0000 | 0.8453 | 0.0461 | 0.068* | |
H12 | −0.1007 | 0.6360 | 0.0166 | 0.068* | 0.50 |
H12A | 0.1007 | 0.6360 | 0.0166 | 0.068* | 0.50 |
C2 | 0.1922 (9) | 0.826 (6) | 0.4857 (11) | 0.07 (2) | |
H21 | 0.2703 | 0.7133 | 0.4556 | 0.089* | |
H22 | 0.1765 | 0.8379 | 0.6377 | 0.089* | |
H23 | 0.2385 | 0.9517 | 0.4311 | 0.089* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
Cl1 | 0.086 (2) | 0.28 (4) | 0.088 (2) | 0.000 | 0.000 | −0.011 (5) |
C1 | 0.061 (4) | 0.05 (7) | 0.059 (4) | 0.000 | 0.000 | 0.046 (13) |
C2 | 0.068 (4) | 0.08 (6) | 0.077 (4) | −0.026 (8) | −0.011 (3) | −0.045 (10) |
Cl1—Si1 | 2.010 (15) | Si1—C2 | 1.964 (19) |
Si1—C1 | 1.882 (9) | Si1—C2^{i} | 1.964 (19) |
C1—Si1—C2 | 105.9 (7) | C1—Si1—Cl1 | 115.4 (10) |
C1—Si1—C2^{i} | 105.9 (7) | C2—Si1—Cl1 | 114.3 (10) |
C2—Si1—C2^{i} | 99.3 (16) | C2^{i}—Si1—Cl1 | 114.3 (10) |
Symmetry code: (i) −x, y, z. |
C_{3}H_{9}ClSi | D_{x} = 1.160 Mg m^{−}^{3} |
M_{r} = 108.64 | Melting point: 215 K |
Orthorhombic, Pmn2_{1} | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac -2 | Cell parameters from 989 reflections |
a = 7.768 (2) Å | θ = 4.2–22.5° |
b = 6.42 (2) Å | µ = 0.66 mm^{−}^{1} |
c = 6.233 (2) Å | T = 293 K |
V = 311.0 (11) Å^{3} | Disc, colourless |
Z = 2 | 0.44 × 0.44 × 0.18 × 0.22 (radius) mm |
F(000) = 116 |
Kuma KM4CCD κ geometry diffractometer | 164 independent reflections |
Radiation source: fine-focus sealed tube | 158 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.057 |
ω scans | θ_{max} = 22.5°, θ_{min} = 4.2° |
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 = −8→8 |
T_{min} = 0.40, T_{max} = 0.94 | k = −2→2 |
1473 measured reflections | l = −6→6 |
Refinement on F^{2} | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F^{2} > 2σ(F^{2})] = 0.032 | w = 1/[σ^{2}(F_{o}^{2}) + (0.0448P)^{2} + 0.0802P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
wR(F^{2}) = 0.082 | (Δ/σ)_{max} = 0.223 |
S = 1.22 | Δρ_{max} = 0.11 e Å^{−}^{3} |
164 reflections | Δρ_{min} = −0.09 e Å^{−}^{3} |
32 parameters | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
1 restraint | Extinction coefficient: 0.018 (17) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.2 (4) |
C_{3}H_{9}ClSi | V = 311.0 (11) Å^{3} |
M_{r} = 108.64 | Z = 2 |
Orthorhombic, Pmn2_{1} | Mo Kα radiation |
a = 7.768 (2) Å | µ = 0.66 mm^{−}^{1} |
b = 6.42 (2) Å | T = 293 K |
c = 6.233 (2) Å | 0.44 × 0.44 × 0.18 × 0.22 (radius) mm |
Kuma KM4CCD κ geometry diffractometer | 164 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 | 158 reflections with I > 2σ(I) |
T_{min} = 0.40, T_{max} = 0.94 | R_{int} = 0.057 |
1473 measured reflections | θ_{max} = 22.5° |
R[F^{2} > 2σ(F^{2})] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F^{2}) = 0.082 | (Δ/σ)_{max} = 0.223 |
S = 1.22 | Δρ_{max} = 0.11 e Å^{−}^{3} |
164 reflections | Δρ_{min} = −0.09 e Å^{−}^{3} |
32 parameters | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
1 restraint | Absolute structure parameter: 0.2 (4) |
Experimental. High-pressure measurement at 0.3 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 F^{2} against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^{2}, conventional R-factors R are based on F, with F set to zero for negative F^{2}. The threshold expression of F^{2} > σ(F^{2}) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^{2} 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 | U_{iso}*/U_{eq} | Occ. (<1) | |
Cl1 | 0.0000 | 0.393 (2) | 0.4611 (5) | 0.087 (10) | |
Si1 | 0.0000 | 0.693 (2) | 0.3624 (4) | 0.072 (7) | |
C1 | 0.0000 | 0.700 (4) | 0.0724 (15) | 0.034 (16) | |
H11 | 0.0000 | 0.8417 | 0.0247 | 0.041* | |
H12 | −0.1009 | 0.6304 | 0.0193 | 0.041* | 0.50 |
H12A | 0.1009 | 0.6304 | 0.0193 | 0.041* | 0.50 |
C2 | 0.1988 (13) | 0.815 (4) | 0.4743 (18) | 0.095 (15) | |
H21 | 0.2972 | 0.7648 | 0.3974 | 0.114* | |
H22 | 0.2115 | 0.7849 | 0.6241 | 0.114* | |
H23 | 0.1898 | 0.9618 | 0.4551 | 0.114* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
Cl1 | 0.0707 (19) | 0.11 (3) | 0.081 (2) | 0.000 | 0.000 | −0.004 (8) |
Si1 | 0.0462 (16) | 0.13 (2) | 0.0433 (17) | 0.000 | 0.000 | 0.016 (5) |
C1 | 0.049 (5) | 0.00 (5) | 0.053 (5) | 0.000 | 0.000 | 0.002 (12) |
C2 | 0.072 (5) | 0.16 (5) | 0.054 (4) | −0.014 (10) | −0.013 (4) | 0.016 (11) |
Cl1—Si1 | 2.02 (2) | Si1—C2 | 1.869 (15) |
Si1—C1 | 1.808 (10) | Si1—C2^{i} | 1.869 (15) |
C1—Si1—C2 | 111.3 (5) | C1—Si1—Cl1 | 109.2 (10) |
C1—Si1—C2^{i} | 111.3 (5) | C2—Si1—Cl1 | 106.8 (7) |
C2—Si1—C2^{i} | 111.4 (14) | C2^{i}—Si1—Cl1 | 106.8 (7) |
Symmetry code: (i) −x, y, z. |
C_{3}H_{9}ClSi | D_{x} = 1.205 Mg m^{−}^{3} |
M_{r} = 108.64 | Melting point: 215 K |
Orthorhombic, Pmn2_{1} | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac -2 | Cell parameters from 798 reflections |
a = 7.668 (2) Å | θ = 4.2–24.9° |
b = 6.34 (2) Å | µ = 0.69 mm^{−}^{1} |
c = 6.159 (2) Å | T = 293 K |
V = 299.4 (11) Å^{3} | Disc, colourless |
Z = 2 | 0.42 × 0.42 × 0.18 × 0.21 (radius) mm |
F(000) = 116 |
Kuma KM4CCD κ geometry diffractometer | 199 independent reflections |
Radiation source: fine-focus sealed tube | 193 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.060 |
ω scans | θ_{max} = 24.9°, θ_{min} = 4.2° |
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 = −9→9 |
T_{min} = 0.41, T_{max} = 0.92 | k = −2→2 |
1697 measured reflections | l = −7→7 |
Refinement on F^{2} | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F^{2} > 2σ(F^{2})] = 0.039 | w = 1/[σ^{2}(F_{o}^{2}) + (0.0395P)^{2} + 0.1814P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
wR(F^{2}) = 0.092 | (Δ/σ)_{max} < 0.001 |
S = 1.27 | Δρ_{max} = 0.17 e Å^{−}^{3} |
199 reflections | Δρ_{min} = −0.19 e Å^{−}^{3} |
29 parameters | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
1 restraint | Extinction coefficient: 0.031 (17) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.0 (4) |
C_{3}H_{9}ClSi | V = 299.4 (11) Å^{3} |
M_{r} = 108.64 | Z = 2 |
Orthorhombic, Pmn2_{1} | Mo Kα radiation |
a = 7.668 (2) Å | µ = 0.69 mm^{−}^{1} |
b = 6.34 (2) Å | T = 293 K |
c = 6.159 (2) Å | 0.42 × 0.42 × 0.18 × 0.21 (radius) mm |
Kuma KM4CCD κ geometry diffractometer | 199 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 | 193 reflections with I > 2σ(I) |
T_{min} = 0.41, T_{max} = 0.92 | R_{int} = 0.060 |
1697 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.039 | H atoms treated by a mixture of independent and constrained refinement |
wR(F^{2}) = 0.092 | Δρ_{max} = 0.17 e Å^{−}^{3} |
S = 1.27 | Δρ_{min} = −0.19 e Å^{−}^{3} |
199 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
29 parameters | Absolute structure parameter: 0.0 (4) |
1 restraint |
Experimental. High-pressure measurement at 0.58 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 F^{2} against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^{2}, conventional R-factors R are based on F, with F set to zero for negative F^{2}. The threshold expression of F^{2} > σ(F^{2}) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^{2} 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 | U_{iso}*/U_{eq} | Occ. (<1) | |
Cl1 | 0.0000 | 0.3912 (19) | 0.4721 (5) | 0.084 (6) | |
Si1 | 0.0000 | 0.6887 (15) | 0.3702 (4) | 0.046 (5) | |
C1 | 0.0000 | 0.694 (4) | 0.0740 (14) | 0.045 (2)* | |
H11 | 0.0000 | 0.8375 | 0.0247 | 0.054* | |
H12 | −0.1022 | 0.6234 | 0.0207 | 0.054* | 0.50 |
H12A | 0.1022 | 0.6234 | 0.0207 | 0.054* | 0.50 |
C2 | 0.2020 (11) | 0.815 (3) | 0.4833 (16) | 0.068 (14) | |
H21 | 0.2983 | 0.7629 | 0.4031 | 0.081* | |
H22 | 0.2149 | 0.7785 | 0.6316 | 0.081* | |
H23 | 0.1974 | 0.9622 | 0.4700 | 0.081* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
Cl1 | 0.0595 (18) | 0.125 (18) | 0.0667 (15) | 0.000 | 0.000 | 0.000 (7) |
Si1 | 0.0391 (13) | 0.064 (15) | 0.0360 (11) | 0.000 | 0.000 | 0.011 (5) |
C2 | 0.064 (4) | 0.09 (4) | 0.045 (3) | −0.013 (9) | −0.012 (3) | −0.002 (11) |
Cl1—Si1 | 1.988 (14) | Si1—C2 | 1.878 (12) |
Si1—C1 | 1.825 (9) | Si1—C2^{i} | 1.878 (12) |
C1—Si1—C2 | 111.3 (5) | C1—Si1—Cl1 | 109.4 (10) |
C1—Si1—C2^{i} | 111.3 (5) | C2—Si1—Cl1 | 106.7 (7) |
C2—Si1—C2^{i} | 111.2 (12) | C2^{i}—Si1—Cl1 | 106.7 (7) |
Symmetry code: (i) −x, y, z. |
Experimental details
(tmcs1) | (tmcs2) | (tmcs3) | |
Crystal data | |||
Chemical formula | C_{3}H_{9}ClSi | C_{3}H_{9}ClSi | C_{3}H_{9}ClSi |
M_{r} | 108.64 | 108.64 | 108.64 |
Crystal system, space group | Orthorhombic, Pmn2_{1} | Orthorhombic, Pmn2_{1} | Orthorhombic, Pmn2_{1} |
Temperature (K) | 293 | 293 | 293 |
a, b, c (Å) | 7.785 (2), 6.43 (3), 6.254 (3) | 7.768 (2), 6.42 (2), 6.233 (2) | 7.668 (2), 6.34 (2), 6.159 (2) |
V (Å^{3}) | 313.0 (15) | 311.0 (11) | 299.4 (11) |
Z | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm^{−}^{1}) | 0.66 | 0.66 | 0.69 |
Crystal size (mm) | 0.46 × 0.46 × 0.18 × 0.23 (radius) | 0.44 × 0.44 × 0.18 × 0.22 (radius) | 0.42 × 0.42 × 0.18 × 0.21 (radius) |
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 |
T_{min}, T_{max} | 0.41, 0.94 | 0.40, 0.94 | 0.41, 0.92 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1793, 194, 170 | 1473, 164, 158 | 1697, 199, 193 |
R_{int} | 0.075 | 0.057 | 0.060 |
θ_{max} (°) | 27.4 | 22.5 | 24.9 |
(sin θ/λ)_{max} (Å^{−}^{1}) | 0.647 | 0.537 | 0.592 |
Refinement | |||
R[F^{2} > 2σ(F^{2})], wR(F^{2}), S | 0.032, 0.083, 1.01 | 0.032, 0.082, 1.22 | 0.039, 0.092, 1.27 |
No. of reflections | 194 | 164 | 199 |
No. of parameters | 29 | 32 | 29 |
No. of restraints | 1 | 1 | 1 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
(Δ/σ)_{max} | < 0.001 | 0.223 | < 0.001 |
Δρ_{max}, Δρ_{min} (e Å^{−}^{3}) | 0.08, −0.11 | 0.11, −0.09 | 0.17, −0.19 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.6 (3) | 0.2 (4) | 0.0 (4) |
Computer programs: CrysAlis (Oxford Diffraction, 2004), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1990).