Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810602982X/av5066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae015gsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae02gsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae03g1sup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae03g2sup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae05gsup6.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae11gsup7.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae15gsup8.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae224ksup9.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae243ksup10.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae274ksup11.hkl |
CCDC references: 629848; 629849; 629850; 629851; 629852; 629853; 629854; 629855; 629856; 629857
For all compounds, data collection: CrysAlis (Oxford Diffraction, 2002); cell refinement: CrysAlis (Oxford Diffraction, 2002); data reduction: CrysAlis (Oxford Diffraction, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001)
and POV-RAY (Persistence of Vision, 2004); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
C_{2}H_{8}N_{2} | F(000) = 68 |
M_{r} = 60.10 | D_{x} = 1.100 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 5.065 (1) Å | Cell parameters from 457 reflections |
b = 7.181 (1) Å | θ = 4.4–29.1° |
c = 5.508 (1) Å | µ = 0.07 mm^{−}^{1} |
β = 115.07 (3)° | T = 224 K |
V = 181.46 (7) Å^{3} | Plate, colourless |
Z = 2 | 0.6 × 0.4 × 0.1 mm |
Kuma KM4CCD κ geometry diffractometer | 369 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | R_{int} = 0.061 |
Graphite monochromator | θ_{max} = 29.1°, θ_{min} = 4.4° |
ω scans | h = −6→6 |
1070 measured reflections | k = −8→9 |
457 independent reflections | l = −7→7 |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.045 | H-atom parameters constrained |
wR(F^{2}) = 0.132 | w = 1/[σ^{2}(F_{o}^{2}) + (0.0726P)^{2} + 0.0014P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.11 | (Δ/σ)_{max} < 0.001 |
457 reflections | Δρ_{max} = 0.31 e Å^{−}^{3} |
25 parameters | Δρ_{min} = −0.16 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.33 (14) |
C_{2}H_{8}N_{2} | V = 181.46 (7) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 5.065 (1) Å | µ = 0.07 mm^{−}^{1} |
b = 7.181 (1) Å | T = 224 K |
c = 5.508 (1) Å | 0.6 × 0.4 × 0.1 mm |
β = 115.07 (3)° |
Kuma KM4CCD κ geometry diffractometer | 369 reflections with I > 2σ(I) |
1070 measured reflections | R_{int} = 0.061 |
457 independent reflections |
R[F^{2} > 2σ(F^{2})] = 0.045 | 0 restraints |
wR(F^{2}) = 0.132 | H-atom parameters constrained |
S = 1.11 | Δρ_{max} = 0.31 e Å^{−}^{3} |
457 reflections | Δρ_{min} = −0.16 e Å^{−}^{3} |
25 parameters |
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} | ||
N1 | 0.8524 (2) | 0.36693 (15) | 0.21202 (19) | 0.0300 (4) | |
H1 | 0.9814 | 0.4725 | 0.2722 | 0.036* | |
H2 | 0.8806 | 0.3101 | 0.0775 | 0.036* | |
C1 | 0.5496 (2) | 0.43086 (17) | 0.1161 (2) | 0.0257 (4) | |
H4 | 0.5252 | 0.4882 | 0.2647 | 0.038 (4)* | |
H3 | 0.4225 | 0.3230 | 0.0606 | 0.033 (4)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.0290 (7) | 0.0326 (7) | 0.0281 (6) | 0.0037 (4) | 0.0117 (5) | 0.0029 (4) |
C1 | 0.0283 (7) | 0.0252 (7) | 0.0259 (6) | −0.0004 (4) | 0.0137 (5) | 0.0025 (4) |
N1—C1 | 1.4682 (15) | C1—C1^{i} | 1.526 (2) |
N1—H1 | 0.9634 | C1—H4 | 0.9700 |
N1—H2 | 0.9084 | C1—H3 | 0.9700 |
C1—N1—H1 | 109.3 | C1^{i}—C1—H4 | 108.4 |
C1—N1—H2 | 110.4 | N1—C1—H3 | 108.4 |
H1—N1—H2 | 108.4 | C1^{i}—C1—H3 | 108.4 |
N1—C1—C1^{i} | 115.33 (12) | H4—C1—H3 | 107.5 |
N1—C1—H4 | 108.4 |
Symmetry code: (i) −x+1, −y+1, −z. |
C_{2}H_{8}N_{2} | D_{x} = 1.100 Mg m^{−}^{3} |
M_{r} = 60.10 | Melting point: 284.29 K |
Monoclinic, P2_{1}/c | Mo Kα radiation, λ = 0.71073 Å |
a = 5.070 (1) Å | Cell parameters from 866 reflections |
b = 7.185 (1) Å | θ = 4.4–29.1° |
c = 5.501 (1) Å | µ = 0.07 mm^{−}^{1} |
β = 115.11 (3)° | T = 243 K |
V = 181.45 (7) Å^{3} | Plate, colourless |
Z = 2 | 0.6 × 0.4 × 0.1 mm |
F(000) = 68 |
Kuma KM4CCD κ geometry diffractometer | 406 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | R_{int} = 0.048 |
Graphite monochromator | θ_{max} = 29.1°, θ_{min} = 4.4° |
ω scans | h = −6→6 |
1241 measured reflections | k = −8→9 |
458 independent reflections | l = −7→6 |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.040 | H-atom parameters constrained |
wR(F^{2}) = 0.112 | w = 1/[σ^{2}(F_{o}^{2}) + (0.059P)^{2} + 0.0216P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.11 | (Δ/σ)_{max} < 0.001 |
458 reflections | Δρ_{max} = 0.34 e Å^{−}^{3} |
25 parameters | Δρ_{min} = −0.15 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.38 (11) |
C_{2}H_{8}N_{2} | V = 181.45 (7) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 5.070 (1) Å | µ = 0.07 mm^{−}^{1} |
b = 7.185 (1) Å | T = 243 K |
c = 5.501 (1) Å | 0.6 × 0.4 × 0.1 mm |
β = 115.11 (3)° |
Kuma KM4CCD κ geometry diffractometer | 406 reflections with I > 2σ(I) |
1241 measured reflections | R_{int} = 0.048 |
458 independent reflections |
R[F^{2} > 2σ(F^{2})] = 0.040 | 0 restraints |
wR(F^{2}) = 0.112 | H-atom parameters constrained |
S = 1.11 | Δρ_{max} = 0.34 e Å^{−}^{3} |
458 reflections | Δρ_{min} = −0.15 e Å^{−}^{3} |
25 parameters |
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} | ||
N1 | 0.85189 (18) | 0.36691 (12) | 0.21189 (17) | 0.0296 (4) | |
H1 | 0.8814 | 0.3078 | 0.0682 | 0.036* | |
H2 | 0.9720 | 0.4671 | 0.2683 | 0.036* | |
C1 | 0.5496 (2) | 0.43080 (13) | 0.11635 (18) | 0.0252 (4) | |
H4 | 0.5256 | 0.4882 | 0.2653 | 0.035 (3)* | |
H3 | 0.4224 | 0.3231 | 0.0607 | 0.034 (3)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.0281 (5) | 0.0328 (6) | 0.0269 (5) | 0.0032 (3) | 0.0107 (4) | 0.0034 (3) |
C1 | 0.0282 (6) | 0.0250 (5) | 0.0242 (5) | 0.0001 (3) | 0.0128 (4) | 0.0024 (3) |
N1—C1 | 1.4672 (13) | C1—C1^{i} | 1.5277 (18) |
N1—H1 | 0.9631 | C1—H4 | 0.9700 |
N1—H2 | 0.9084 | C1—H3 | 0.9700 |
C1—N1—H1 | 110.3 | C1^{i}—C1—H4 | 108.5 |
C1—N1—H2 | 108.7 | N1—C1—H3 | 108.5 |
H1—N1—H2 | 108.4 | C1^{i}—C1—H3 | 108.5 |
N1—C1—C1^{i} | 115.22 (9) | H4—C1—H3 | 107.5 |
N1—C1—H4 | 108.5 |
Symmetry code: (i) −x+1, −y+1, −z. |
C_{2}H_{8}N_{2} | F(000) = 68 |
M_{r} = 60.10 | D_{x} = 1.085 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 5.102 (1) Å | Cell parameters from 240 reflections |
b = 7.197 (1) Å | θ = 4.4–28.6° |
c = 5.535 (1) Å | µ = 0.07 mm^{−}^{1} |
β = 115.18 (3)° | T = 274 K |
V = 183.93 (7) Å^{3} | Plate, colourless |
Z = 2 | 0.6 × 0.4 × 0.1 mm |
Kuma KM4CCD κ geometry diffractometer | 330 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | R_{int} = 0.129 |
Graphite monochromator | θ_{max} = 28.6°, θ_{min} = 4.4° |
ω scans | h = −6→6 |
940 measured reflections | k = −8→9 |
452 independent reflections | l = −7→6 |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.085 | H-atom parameters constrained |
wR(F^{2}) = 0.210 | w = 1/[σ^{2}(F_{o}^{2}) + (0.1384P)^{2}] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.04 | (Δ/σ)_{max} < 0.001 |
452 reflections | Δρ_{max} = 0.35 e Å^{−}^{3} |
25 parameters | Δρ_{min} = −0.29 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.6 (3) |
C_{2}H_{8}N_{2} | V = 183.93 (7) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 5.102 (1) Å | µ = 0.07 mm^{−}^{1} |
b = 7.197 (1) Å | T = 274 K |
c = 5.535 (1) Å | 0.6 × 0.4 × 0.1 mm |
β = 115.18 (3)° |
Kuma KM4CCD κ geometry diffractometer | 330 reflections with I > 2σ(I) |
940 measured reflections | R_{int} = 0.129 |
452 independent reflections |
R[F^{2} > 2σ(F^{2})] = 0.085 | 0 restraints |
wR(F^{2}) = 0.210 | H-atom parameters constrained |
S = 1.04 | Δρ_{max} = 0.35 e Å^{−}^{3} |
452 reflections | Δρ_{min} = −0.29 e Å^{−}^{3} |
25 parameters |
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} | ||
N1 | 0.8483 (3) | 0.3676 (2) | 0.2102 (3) | 0.0444 (7) | |
H1 | 0.9857 | 0.4683 | 0.2801 | 0.053* | |
H2 | 0.8744 | 0.3138 | 0.0727 | 0.053* | |
C1 | 0.5494 (3) | 0.4318 (2) | 0.1156 (3) | 0.0380 (7) | |
H4 | 0.5265 | 0.4899 | 0.2636 | 0.039 (4)* | |
H3 | 0.4226 | 0.3244 | 0.0615 | 0.052 (6)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.0385 (11) | 0.0432 (11) | 0.0442 (10) | 0.0051 (6) | 0.0106 (7) | 0.0048 (6) |
C1 | 0.0388 (11) | 0.0318 (10) | 0.0404 (10) | −0.0011 (6) | 0.0140 (7) | 0.0030 (6) |
N1—C1 | 1.461 (2) | C1—C1^{i} | 1.519 (3) |
N1—H1 | 0.9670 | C1—H4 | 0.9700 |
N1—H2 | 0.9127 | C1—H3 | 0.9700 |
C1—N1—H1 | 112.0 | C1^{i}—C1—H4 | 108.4 |
C1—N1—H2 | 109.6 | N1—C1—H3 | 108.4 |
H1—N1—H2 | 108.2 | C1^{i}—C1—H3 | 108.4 |
N1—C1—C1^{i} | 115.35 (18) | H4—C1—H3 | 107.5 |
N1—C1—H4 | 108.4 |
Symmetry code: (i) −x+1, −y+1, −z. |
C_{2}H_{8}N_{2} | The unit-cell dimensions corrected for the effect of the gasket-shadowing: Katrusiak Andrzej - being prepared for publication |
M_{r} = 60.10 | D_{x} = 1.091 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 5.078 (5) Å | Cell parameters from 355 reflections |
b = 7.204 (8) Å | θ = 4.4–29.6° |
c = 5.528 (12) Å | µ = 0.07 mm^{−}^{1} |
β = 115.24 (18)° | T = 296 K |
V = 182.9 (6) Å^{3} | , colourless |
Z = 2 | 0.30 × 0.30 × 0.08 mm |
F(000) = 68 |
Kuma KM4CCD κ geometry diffractometer | 224 independent reflections |
Radiation source: fine-focus sealed tube | 188 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.075 |
Detector resolution: 16.4 pixels mm^{-1} | θ_{max} = 29.6°, θ_{min} = 4.4° |
HP ω scans – for more details see: A. Budzianowski, A. Katrusiak in High–Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157–168 | h = −6→6 |
Absorption correction: integration 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 | k = −8→8 |
T_{min} = 0.44, T_{max} = 0.84 | l = −5→5 |
1259 measured reflections |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.084 | H-atom parameters constrained |
wR(F^{2}) = 0.130 | w = 1/[σ^{2}(F_{o}^{2}) + (0.P)^{2} + 0.1653P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.25 | (Δ/σ)_{max} < 0.001 |
224 reflections | Δρ_{max} = 0.10 e Å^{−}^{3} |
25 parameters | Δρ_{min} = −0.11 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 1.00 (13) |
C_{2}H_{8}N_{2} | V = 182.9 (6) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 5.078 (5) Å | µ = 0.07 mm^{−}^{1} |
b = 7.204 (8) Å | T = 296 K |
c = 5.528 (12) Å | 0.30 × 0.30 × 0.08 mm |
β = 115.24 (18)° |
Kuma KM4CCD κ geometry diffractometer | 224 independent reflections |
Absorption correction: integration 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 | 188 reflections with I > 2σ(I) |
T_{min} = 0.44, T_{max} = 0.84 | R_{int} = 0.075 |
1259 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.084 | 0 restraints |
wR(F^{2}) = 0.130 | H-atom parameters constrained |
S = 1.25 | Δρ_{max} = 0.10 e Å^{−}^{3} |
224 reflections | Δρ_{min} = −0.11 e Å^{−}^{3} |
25 parameters |
Experimental. high-pressure measurement at 0.15 (5) GPa - the high pressure of ethylenodiamine |
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} | ||
N1 | 0.8491 (8) | 0.3686 (5) | 0.2117 (10) | 0.0493 (14) | |
H1 | 0.9739 | 0.4767 | 0.2550 | 0.059* | |
H2 | 0.8699 | 0.3049 | 0.0787 | 0.059* | |
C1 | 0.5489 (7) | 0.4333 (6) | 0.1154 (11) | 0.0423 (14) | |
H4 | 0.5257 | 0.4926 | 0.2627 | 0.057 (13)* | |
H3 | 0.4211 | 0.3261 | 0.0623 | 0.032 (9)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.0464 (19) | 0.060 (3) | 0.039 (4) | 0.0037 (15) | 0.0158 (19) | 0.0043 (15) |
C1 | 0.047 (2) | 0.048 (4) | 0.034 (5) | −0.0048 (17) | 0.019 (2) | 0.0019 (15) |
N1—C1 | 1.461 (5) | C1—C1^{i} | 1.503 (9) |
N1—H1 | 0.9673 | C1—H4 | 0.9700 |
N1—H2 | 0.9100 | C1—H3 | 0.9700 |
C1—N1—H1 | 107.8 | C1^{i}—C1—H4 | 108.4 |
C1—N1—H2 | 109.2 | N1—C1—H3 | 108.4 |
H1—N1—H2 | 108.5 | C1^{i}—C1—H3 | 108.4 |
N1—C1—C1^{i} | 115.4 (5) | H4—C1—H3 | 107.5 |
N1—C1—H4 | 108.4 |
Symmetry code: (i) −x+1, −y+1, −z. |
C_{2}H_{8}N_{2} | The unit-cell dimensions corrected for the effect of the gasket-shadowing: Katrusiak Andrzej - being prepared for publication |
M_{r} = 60.10 | D_{x} = 1.182 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 4.949 (6) Å | Cell parameters from 343 reflections |
b = 7.704 (8) Å | θ = 5.3–28.9° |
c = 4.96 (3) Å | µ = 0.08 mm^{−}^{1} |
β = 116.7 (11)° | T = 296 K |
V = 169.0 (19) Å^{3} | , colourless |
Z = 2 | 0.42 × 0.42 × 0.10 mm |
F(000) = 68 |
Kuma KM4CCD κ geometry diffractometer | 117 independent reflections |
Radiation source: fine-focus sealed tube | 113 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.062 |
Detector resolution: 16.4 pixels mm^{-1} | θ_{max} = 28.9°, θ_{min} = 5.3° |
HP ω scans – for more details see: A. Budzianowski, A. Katrusiak in High–Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157–168 | h = −3→3 |
Absorption correction: integration 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 | k = −10→10 |
T_{min} = 0.48, T_{max} = 0.94 | l = −6→6 |
1260 measured reflections |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.142 | H-atom parameters constrained |
wR(F^{2}) = 0.266 | w = 1/[σ^{2}(F_{o}^{2}) + (0.050P)^{2} + 0.3P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.76 | (Δ/σ)_{max} < 0.001 |
117 reflections | Δρ_{max} = 0.12 e Å^{−}^{3} |
20 parameters | Δρ_{min} = −0.13 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.3 (2) |
C_{2}H_{8}N_{2} | V = 169.0 (19) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 4.949 (6) Å | µ = 0.08 mm^{−}^{1} |
b = 7.704 (8) Å | T = 296 K |
c = 4.96 (3) Å | 0.42 × 0.42 × 0.10 mm |
β = 116.7 (11)° |
Kuma KM4CCD κ geometry diffractometer | 117 independent reflections |
Absorption correction: integration 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 | 113 reflections with I > 2σ(I) |
T_{min} = 0.48, T_{max} = 0.94 | R_{int} = 0.062 |
1260 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.142 | 0 restraints |
wR(F^{2}) = 0.266 | H-atom parameters constrained |
S = 1.76 | Δρ_{max} = 0.12 e Å^{−}^{3} |
117 reflections | Δρ_{min} = −0.13 e Å^{−}^{3} |
20 parameters |
Experimental. high-pressure measurement at 0.30 (5) GPa - the high pressure of ethylenodiamine |
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} | ||
N1 | 0.777 (5) | 0.3540 (11) | 0.276 (3) | 0.045 (3)* | |
H1 | 0.8596 | 0.3022 | 0.1628 | 0.054* | |
H2 | 0.9307 | 0.3962 | 0.4451 | 0.054* | |
C1 | 0.501 (7) | 0.4352 (12) | 0.112 (3) | 0.05 (2) | |
H4 | 0.4423 | 0.4927 | 0.2512 | 0.05 (2)* | |
H3 | 0.3500 | 0.3472 | 0.0054 | 0.11 (6)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
C1 | 0.07 (7) | 0.042 (5) | 0.050 (15) | 0.005 (11) | 0.03 (3) | −0.002 (6) |
N1—C1 | 1.39 (4) | C1—C1^{i} | 1.487 (18) |
N1—H1 | 0.9174 | C1—H4 | 0.9700 |
N1—H2 | 0.9023 | C1—H3 | 0.9700 |
C1—N1—H1 | 115.4 | C1^{i}—C1—H4 | 108.7 |
C1—N1—H2 | 125.4 | N1—C1—H3 | 108.7 |
H1—N1—H2 | 107.9 | C1^{i}—C1—H3 | 108.7 |
N1—C1—C1^{i} | 114 (3) | H4—C1—H3 | 107.6 |
N1—C1—H4 | 108.7 |
Symmetry code: (i) −x+1, −y+1, −z. |
C_{2}H_{8}N_{2} | The unit-cell dimensions corrected for the effect of the gasket-shadowing: Katrusiak Andrzej - being prepared for publication |
M_{r} = 60.10 | D_{x} = 1.236 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 4.82 (5) Å | Cell parameters from 510 reflections |
b = 7.563 (5) Å | θ = 5.3–29.4° |
c = 4.873 (18) Å | µ = 0.08 mm^{−}^{1} |
β = 114.5 (8)° | T = 296 K |
V = 162 (2) Å^{3} | , colourless |
Z = 2 | 0.41 × 0.41 × 0.09 mm |
F(000) = 68 |
Kuma KM4CCD κ geometry diffractometer | 124 independent reflections |
Radiation source: fine-focus sealed tube | 103 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.064 |
Detector resolution: 16.4 pixels mm^{-1} | θ_{max} = 29.4°, θ_{min} = 5.3° |
HP ω scans – for more details see: A. Budzianowski, A. Katrusiak in High–Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157–168 | h = −3→3 |
Absorption correction: integration 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 | k = −10→10 |
T_{min} = 0.45, T_{max} = 0.93 | l = −6→6 |
1159 measured reflections |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.064 | H-atom parameters constrained |
wR(F^{2}) = 0.212 | w = 1/[σ^{2}(F_{o}^{2}) + (0.1176P)^{2} + 0.1743P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 0.96 | (Δ/σ)_{max} < 0.001 |
124 reflections | Δρ_{max} = 0.10 e Å^{−}^{3} |
25 parameters | Δρ_{min} = −0.10 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 1.0 (6) |
C_{2}H_{8}N_{2} | V = 162 (2) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 4.82 (5) Å | µ = 0.08 mm^{−}^{1} |
b = 7.563 (5) Å | T = 296 K |
c = 4.873 (18) Å | 0.41 × 0.41 × 0.09 mm |
β = 114.5 (8)° |
Kuma KM4CCD κ geometry diffractometer | 124 independent reflections |
Absorption correction: integration 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 | 103 reflections with I > 2σ(I) |
T_{min} = 0.45, T_{max} = 0.93 | R_{int} = 0.064 |
1159 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.064 | 0 restraints |
wR(F^{2}) = 0.212 | H-atom parameters constrained |
S = 0.96 | Δρ_{max} = 0.10 e Å^{−}^{3} |
124 reflections | Δρ_{min} = −0.10 e Å^{−}^{3} |
25 parameters |
Experimental. high-pressure measurement at 1.10 (5) GPa - the high pressure of ethylenodiamine |
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} | ||
N1 | 0.794 (3) | 0.3522 (6) | 0.2867 (16) | 0.071 (10) | |
H1 | 0.8436 | 0.2967 | 0.1520 | 0.085* | |
H2 | 0.9550 | 0.4152 | 0.4101 | 0.085* | |
C1 | 0.495 (4) | 0.4306 (7) | 0.1128 (19) | 0.055 (13) | |
H4 | 0.4213 | 0.4857 | 0.2498 | 0.059 (15)* | |
H3 | 0.3521 | 0.3380 | 0.0041 | 0.10 (3)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.11 (3) | 0.047 (2) | 0.070 (7) | 0.014 (5) | 0.052 (13) | 0.014 (2) |
C1 | 0.08 (4) | 0.045 (3) | 0.053 (7) | −0.005 (5) | 0.039 (16) | −0.007 (3) |
N1—C1 | 1.46 (3) | C1—C1^{i} | 1.536 (11) |
N1—H1 | 0.8923 | C1—H4 | 0.9700 |
N1—H2 | 0.8967 | C1—H3 | 0.9700 |
C1—N1—H1 | 105.4 | C1^{i}—C1—H4 | 109.2 |
C1—N1—H2 | 123.0 | N1—C1—H3 | 109.2 |
H1—N1—H2 | 108.6 | C1^{i}—C1—H3 | 109.2 |
N1—C1—C1^{i} | 112.1 (18) | H4—C1—H3 | 107.9 |
N1—C1—H4 | 109.2 |
Symmetry code: (i) −x+1, −y+1, −z. |
C_{2}H_{8}N_{2} | The unit-cell dimensions corrected for the effect of the gasket-shadowing: Katrusiak Andrzej - being prepared for publication |
M_{r} = 60.10 | D_{x} = 1.243 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 9.69 (10) Å | Cell parameters from 516 reflections |
b = 7.488 (5) Å | θ = 5.0–29.8° |
c = 4.849 (14) Å | µ = 0.08 mm^{−}^{1} |
β = 114.0 (7)° | T = 296 K |
V = 321 (4) Å^{3} | , colourless |
Z = 4 | 0.41 × 0.41 × 0.08 mm |
F(000) = 136 |
Kuma KM4CCD κ geometry diffractometer | 235 independent reflections |
Radiation source: fine-focus sealed tube | 225 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.108 |
Detector resolution: 16.4 pixels mm^{-1} | θ_{max} = 29.8°, θ_{min} = 5.0° |
HP ω scans – for more details see: A. Budzianowski, A. Katrusiak in High–Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157–168 | h = −5→5 |
Absorption correction: integration 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 | k = −10→10 |
T_{min} = 0.45, T_{max} = 0.93 | l = −6→6 |
2437 measured reflections |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.237 | H-atom parameters constrained |
wR(F^{2}) = 0.433 | w = 1/[σ^{2}(F_{o}^{2}) + (0.050P)^{2} + 5.P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.39 | (Δ/σ)_{max} < 0.001 |
235 reflections | Δρ_{max} = 0.33 e Å^{−}^{3} |
26 parameters | Δρ_{min} = −0.27 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.8 (3) |
C_{2}H_{8}N_{2} | V = 321 (4) Å^{3} |
M_{r} = 60.10 | Z = 4 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 9.69 (10) Å | µ = 0.08 mm^{−}^{1} |
b = 7.488 (5) Å | T = 296 K |
c = 4.849 (14) Å | 0.41 × 0.41 × 0.08 mm |
β = 114.0 (7)° |
Kuma KM4CCD κ geometry diffractometer | 235 independent reflections |
Absorption correction: integration 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 | 225 reflections with I > 2σ(I) |
T_{min} = 0.45, T_{max} = 0.93 | R_{int} = 0.108 |
2437 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.237 | 0 restraints |
wR(F^{2}) = 0.433 | H-atom parameters constrained |
S = 1.39 | Δρ_{max} = 0.33 e Å^{−}^{3} |
235 reflections | Δρ_{min} = −0.27 e Å^{−}^{3} |
26 parameters |
Experimental. high-pressure measurement at 1.50 (5) GPa - the high pressure of ethylenodiamine |
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} | ||
N1 | 0.144 (4) | 0.3449 (13) | 0.275 (3) | 0.012 (3)* | |
H1 | 0.1350 | 0.2312 | 0.3093 | 0.014* | |
H2 | 0.2069 | 0.3559 | 0.1780 | 0.014* | |
C1 | −0.004 (7) | 0.436 (2) | 0.105 (5) | 0.037 (5)* | |
H3 | −0.0352 | 0.4949 | 0.2479 | 0.045* | |
H4 | −0.0791 | 0.3469 | −0.0018 | 0.045* | |
N2 | 0.651 (5) | 0.3723 (17) | 0.317 (4) | 0.036 (5)* | |
H7 | 0.6942 | 0.3060 | 0.2219 | 0.043* | |
H8 | 0.6699 | 0.3212 | 0.4965 | 0.043* | |
C2 | 0.503 (6) | 0.4301 (18) | 0.118 (5) | 0.029 (5)* | |
H5 | 0.4531 | 0.4790 | 0.2386 | 0.035* | |
H6 | 0.4456 | 0.3264 | 0.0127 | 0.035* |
N1—C1 | 1.49 (6) | N2—C2 | 1.43 (6) |
N1—H1 | 0.8791 | N2—H7 | 0.8906 |
N1—H2 | 0.9119 | N2—H8 | 0.8984 |
C1—C1^{i} | 1.42 (3) | C2—C2^{ii} | 1.53 (3) |
C1—H3 | 0.9700 | C2—H5 | 0.9700 |
C1—H4 | 0.9700 | C2—H6 | 0.9700 |
C1—N1—H1 | 113.6 | C2—N2—H7 | 111.9 |
C1—N1—H2 | 111.5 | C2—N2—H8 | 122.4 |
H1—N1—H2 | 108.9 | H7—N2—H8 | 108.1 |
N1—C1—C1^{i} | 113 (6) | N2—C2—C2^{ii} | 116 (6) |
N1—C1—H3 | 109.0 | N2—C2—H5 | 108.4 |
C1^{i}—C1—H3 | 109.0 | C2^{ii}—C2—H5 | 108.4 |
N1—C1—H4 | 109.0 | N2—C2—H6 | 108.4 |
C1^{i}—C1—H4 | 109.0 | C2^{ii}—C2—H6 | 108.4 |
H3—C1—H4 | 107.8 | H5—C2—H6 | 107.4 |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z. |
C_{2}H_{8}N_{2} | The unit-cell dimensions corrected for the effect of the gasket-shadowing: Katrusiak Andrzej - being prepared for publication |
M_{r} = 60.10 | D_{x} = 1.113 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 5.10 (3) Å | Cell parameters from 794 reflections |
b = 5.212 (2) Å | θ = 4.9–29.3° |
c = 7.262 (12) Å | µ = 0.08 mm^{−}^{1} |
β = 111.6 (4)° | T = 296 K |
V = 179.5 (12) Å^{3} | , colourless |
Z = 2 | 0.42 × 0.42 × 0.11 mm |
F(000) = 68 |
Kuma KM4CCD κ geometry diffractometer | 141 independent reflections |
Radiation source: fine-focus sealed tube | 125 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.097 |
Detector resolution: 16.4 pixels mm^{-1} | θ_{max} = 29.3°, θ_{min} = 4.9° |
HP ω scans – for more details see: A. Budzianowski, A. Katrusiak in High–Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157–168 | h = −3→3 |
Absorption correction: integration 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 | k = −7→7 |
T_{min} = 0.47, T_{max} = 0.89 | l = −9→9 |
1272 measured reflections |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.055 | H-atom parameters constrained |
wR(F^{2}) = 0.104 | w = 1/[σ^{2}(F_{o}^{2}) + (0.0185P)^{2} + 0.1484P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.10 | (Δ/σ)_{max} < 0.001 |
141 reflections | Δρ_{max} = 0.10 e Å^{−}^{3} |
25 parameters | Δρ_{min} = −0.09 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 10.4 (13) |
C_{2}H_{8}N_{2} | V = 179.5 (12) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 5.10 (3) Å | µ = 0.08 mm^{−}^{1} |
b = 5.212 (2) Å | T = 296 K |
c = 7.262 (12) Å | 0.42 × 0.42 × 0.11 mm |
β = 111.6 (4)° |
Kuma KM4CCD κ geometry diffractometer | 141 independent reflections |
Absorption correction: integration 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 | 125 reflections with I > 2σ(I) |
T_{min} = 0.47, T_{max} = 0.89 | R_{int} = 0.097 |
1272 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.055 | 0 restraints |
wR(F^{2}) = 0.104 | H-atom parameters constrained |
S = 1.10 | Δρ_{max} = 0.10 e Å^{−}^{3} |
141 reflections | Δρ_{min} = −0.09 e Å^{−}^{3} |
25 parameters |
Experimental. high-pressure measurement at 0.20 (5) GPa - the high pressure of ethylenodiamine |
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} | ||
N1 | 0.824 (3) | 0.7076 (8) | 0.6248 (9) | 0.060 (9) | |
H1 | 0.9058 | 0.7499 | 0.5280 | 0.072* | |
H2 | 0.9338 | 0.5602 | 0.6780 | 0.072* | |
C1 | 0.536 (3) | 0.6165 (8) | 0.5673 (10) | 0.067 (10) | |
H3 | 0.4094 | 0.7550 | 0.5009 | 0.046 (16)* | |
H4 | 0.5008 | 0.5752 | 0.6864 | 0.030 (9)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.09 (3) | 0.038 (2) | 0.049 (5) | −0.004 (5) | 0.026 (11) | −0.006 (2) |
C1 | 0.14 (3) | 0.026 (2) | 0.049 (5) | 0.004 (5) | 0.053 (12) | 0.000 (2) |
N1—C1 | 1.45 (2) | C1—C1^{i} | 1.517 (10) |
N1—H1 | 0.9644 | C1—H3 | 0.9700 |
N1—H2 | 0.9443 | C1—H4 | 0.9700 |
C1—N1—H1 | 121.9 | C1^{i}—C1—H3 | 108.5 |
C1—N1—H2 | 103.6 | N1—C1—H4 | 108.5 |
H1—N1—H2 | 97.8 | C1^{i}—C1—H4 | 108.5 |
N1—C1—C1^{i} | 115.2 (14) | H3—C1—H4 | 107.5 |
N1—C1—H3 | 108.5 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
C_{2}H_{8}N_{2} | The unit-cell dimensions corrected for the effect of the gasket-shadowing: Katrusiak Andrzej - being prepared for publication |
M_{r} = 60.10 | D_{x} = 1.152 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 5.031 (10) Å | Cell parameters from 697 reflections |
b = 5.132 (3) Å | θ = 5.0–29.4° |
c = 7.167 (5) Å | µ = 0.08 mm^{−}^{1} |
β = 110.60 (12)° | T = 296 K |
V = 173.2 (4) Å^{3} | , colourless |
Z = 2 | 0.40 × 0.40 × 0.09 mm |
F(000) = 68 |
Kuma KM4CCD κ geometry diffractometer | 96 independent reflections |
Radiation source: fine-focus sealed tube | 72 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.091 |
Detector resolution: 16.4 pixels mm^{-1} | θ_{max} = 29.4°, θ_{min} = 5.0° |
HP ω scans – for more details see: A. Budzianowski, A. Katrusiak in High–Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157–168 | h = −3→3 |
Absorption correction: integration 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 | k = −6→6 |
T_{min} = 0.55, T_{max} = 0.91 | l = −9→9 |
897 measured reflections |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.074 | H-atom parameters constrained |
wR(F^{2}) = 0.253 | w = 1/[σ^{2}(F_{o}^{2}) + (0.1848P)^{2}] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.22 | (Δ/σ)_{max} < 0.001 |
96 reflections | Δρ_{max} = 0.15 e Å^{−}^{3} |
20 parameters | Δρ_{min} = −0.14 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.3 (4) |
C_{2}H_{8}N_{2} | V = 173.2 (4) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 5.031 (10) Å | µ = 0.08 mm^{−}^{1} |
b = 5.132 (3) Å | T = 296 K |
c = 7.167 (5) Å | 0.40 × 0.40 × 0.09 mm |
β = 110.60 (12)° |
Kuma KM4CCD κ geometry diffractometer | 96 independent reflections |
Absorption correction: integration 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 | 72 reflections with I > 2σ(I) |
T_{min} = 0.55, T_{max} = 0.91 | R_{int} = 0.091 |
897 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.074 | 0 restraints |
wR(F^{2}) = 0.253 | H-atom parameters constrained |
S = 1.22 | Δρ_{max} = 0.15 e Å^{−}^{3} |
96 reflections | Δρ_{min} = −0.14 e Å^{−}^{3} |
20 parameters |
Experimental. high-pressure measurement at 0.30 (5) GPa - the high pressure of ethylenodiamine |
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} | ||
N1 | 0.820 (6) | 0.7126 (10) | 0.6209 (18) | 0.11 (2) | |
H1 | 0.8483 | 0.7223 | 0.4970 | 0.138* | |
H2 | 0.9604 | 0.5891 | 0.6817 | 0.138* | |
C1 | 0.542 (5) | 0.6209 (14) | 0.5720 (15) | 0.043 (3)* | |
H3 | 0.4128 | 0.7625 | 0.5109 | 0.18 (11)* | |
H4 | 0.5124 | 0.5753 | 0.6946 | 0.027 (12)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.25 (6) | 0.036 (3) | 0.097 (12) | −0.008 (10) | 0.11 (3) | −0.002 (4) |
N1—C1 | 1.40 (4) | C1—C1^{i} | 1.574 (19) |
N1—H1 | 0.9479 | C1—H3 | 0.9700 |
N1—H2 | 0.9334 | C1—H4 | 0.9700 |
C1—N1—H1 | 104.4 | C1^{i}—C1—H3 | 108.2 |
C1—N1—H2 | 114.4 | N1—C1—H4 | 108.2 |
H1—N1—H2 | 97.9 | C1^{i}—C1—H4 | 108.2 |
N1—C1—C1^{i} | 116 (2) | H3—C1—H4 | 107.4 |
N1—C1—H3 | 108.2 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
C_{2}H_{8}N_{2} | The unit-cell dimensions corrected for the effect of the gasket-shadowing: Katrusiak Andrzej - being prepared for publication |
M_{r} = 60.10 | D_{x} = 1.157 Mg m^{−}^{3} |
Monoclinic, P2_{1}/c | Melting point: 284.29 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 4.9921 (18) Å | Cell parameters from 761 reflections |
b = 5.137 (4) Å | θ = 4.4–29.9° |
c = 7.200 (4) Å | µ = 0.08 mm^{−}^{1} |
β = 110.87 (5)° | T = 296 K |
V = 172.53 (19) Å^{3} | , colourless |
Z = 2 | 0.35 × 0.35 × 0.08 mm |
F(000) = 68 |
Kuma KM4CCD κ geometry diffractometer | 206 independent reflections |
Radiation source: fine-focus sealed tube | 193 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.063 |
Detector resolution: 16.4 pixels mm^{-1} | θ_{max} = 29.9°, θ_{min} = 4.4° |
HP ω scans – for more details see: A. Budzianowski, A. Katrusiak in High–Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157–168 | h = −6→6 |
Absorption correction: integration 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 | k = −4→4 |
T_{min} = 0.49, T_{max} = 0.82 | l = −8→8 |
1110 measured reflections |
Refinement on F^{2} | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F^{2} > 2σ(F^{2})] = 0.059 | H-atom parameters constrained |
wR(F^{2}) = 0.149 | w = 1/[σ^{2}(F_{o}^{2}) + (0.0578P)^{2} + 0.1608P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.07 | (Δ/σ)_{max} < 0.001 |
206 reflections | Δρ_{max} = 0.13 e Å^{−}^{3} |
25 parameters | Δρ_{min} = −0.15 e Å^{−}^{3} |
0 restraints | Extinction correction: SHELXL, Fc^{*}=kFc[1+0.001xFc^{2}λ^{3}/sin(2θ)]^{-1/4} |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.3 (2) |
C_{2}H_{8}N_{2} | V = 172.53 (19) Å^{3} |
M_{r} = 60.10 | Z = 2 |
Monoclinic, P2_{1}/c | Mo Kα radiation |
a = 4.9921 (18) Å | µ = 0.08 mm^{−}^{1} |
b = 5.137 (4) Å | T = 296 K |
c = 7.200 (4) Å | 0.35 × 0.35 × 0.08 mm |
β = 110.87 (5)° |
Kuma KM4CCD κ geometry diffractometer | 206 independent reflections |
Absorption correction: integration 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} = 0.49, T_{max} = 0.82 | R_{int} = 0.063 |
1110 measured reflections |
R[F^{2} > 2σ(F^{2})] = 0.059 | 0 restraints |
wR(F^{2}) = 0.149 | H-atom parameters constrained |
S = 1.07 | Δρ_{max} = 0.13 e Å^{−}^{3} |
206 reflections | Δρ_{min} = −0.15 e Å^{−}^{3} |
25 parameters |
Experimental. high-pressure measurement at 0.50 (5) GPa - the high pressure of ethylenodiamine |
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} | ||
N1 | 0.8294 (5) | 0.7134 (7) | 0.6240 (4) | 0.0389 (11) | |
H1 | 0.8702 | 0.7232 | 0.5052 | 0.047* | |
H2 | 0.9595 | 0.5829 | 0.6877 | 0.047* | |
C1 | 0.5352 (6) | 0.6194 (9) | 0.5681 (5) | 0.0305 (11) | |
H3 | 0.4060 | 0.7593 | 0.5019 | 0.049 (10)* | |
H4 | 0.4988 | 0.5771 | 0.6882 | 0.034 (8)* |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
N1 | 0.0366 (14) | 0.028 (3) | 0.049 (2) | −0.0029 (13) | 0.0115 (11) | −0.0056 (10) |
C1 | 0.0351 (14) | 0.021 (4) | 0.035 (3) | 0.0021 (12) | 0.0114 (12) | −0.0012 (9) |
N1—C1 | 1.460 (4) | C1—C1^{i} | 1.531 (6) |
N1—H1 | 0.9483 | C1—H3 | 0.9700 |
N1—H2 | 0.9324 | C1—H4 | 0.9700 |
C1—N1—H1 | 106.7 | C1^{i}—C1—H3 | 108.5 |
C1—N1—H2 | 110.7 | N1—C1—H4 | 108.5 |
H1—N1—H2 | 98.4 | C1^{i}—C1—H4 | 108.5 |
N1—C1—C1^{i} | 114.9 (3) | H3—C1—H4 | 107.5 |
N1—C1—H3 | 108.5 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
(DAE224K) | (DAE243K) | (DAE274K) | (DAE015G) | |
Crystal data | ||||
Chemical formula | C_{2}H_{8}N_{2} | C_{2}H_{8}N_{2} | C_{2}H_{8}N_{2} | C_{2}H_{8}N_{2} |
M_{r} | 60.10 | 60.10 | 60.10 | 60.10 |
Crystal system, space group | Monoclinic, P2_{1}/c | Monoclinic, P2_{1}/c | Monoclinic, P2_{1}/c | Monoclinic, P2_{1}/c |
Temperature (K) | 224 | 243 | 274 | 296 |
a, b, c (Å) | 5.065 (1), 7.181 (1), 5.508 (1) | 5.070 (1), 7.185 (1), 5.501 (1) | 5.102 (1), 7.197 (1), 5.535 (1) | 5.078 (5), 7.204 (8), 5.528 (12) |
β (°) | 115.07 (3) | 115.11 (3) | 115.18 (3) | 115.24 (18) |
V (Å^{3}) | 181.46 (7) | 181.45 (7) | 183.93 (7) | 182.9 (6) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm^{−}^{1}) | 0.07 | 0.07 | 0.07 | 0.07 |
Crystal size (mm) | 0.6 × 0.4 × 0.1 | 0.6 × 0.4 × 0.1 | 0.6 × 0.4 × 0.1 | 0.30 × 0.30 × 0.08 |
Data collection | ||||
Diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer |
Absorption correction | – | – | – | Integration 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} | – | – | – | 0.44, 0.84 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1070, 457, 369 | 1241, 458, 406 | 940, 452, 330 | 1259, 224, 188 |
R_{int} | 0.061 | 0.048 | 0.129 | 0.075 |
(sin θ/λ)_{max} (Å^{−}^{1}) | 0.683 | 0.683 | 0.673 | 0.696 |
Refinement | ||||
R[F^{2} > 2σ(F^{2})], wR(F^{2}), S | 0.045, 0.132, 1.11 | 0.040, 0.112, 1.11 | 0.085, 0.210, 1.04 | 0.084, 0.130, 1.25 |
No. of reflections | 457 | 458 | 452 | 224 |
No. of parameters | 25 | 25 | 25 | 25 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρ_{max}, Δρ_{min} (e Å^{−}^{3}) | 0.31, −0.16 | 0.34, −0.15 | 0.35, −0.29 | 0.10, −0.11 |
(DAE03G1) | (DAE11G) | (DAE15G) | (DAE02G) | |
Crystal data | ||||
Chemical formula | C_{2}H_{8}N_{2} | C_{2}H_{8}N_{2} | C_{2}H_{8}N_{2} | C_{2}H_{8}N_{2} |
M_{r} | 60.10 | 60.10 | 60.10 | 60.10 |
Crystal system, space group | Monoclinic, P2_{1}/c | Monoclinic, P2_{1}/c | Monoclinic, P2_{1}/c | Monoclinic, P2_{1}/c |
Temperature (K) | 296 | 296 | 296 | 296 |
a, b, c (Å) | 4.949 (6), 7.704 (8), 4.96 (3) | 4.82 (5), 7.563 (5), 4.873 (18) | 9.69 (10), 7.488 (5), 4.849 (14) | 5.10 (3), 5.212 (2), 7.262 (12) |
β (°) | 116.7 (11) | 114.5 (8) | 114.0 (7) | 111.6 (4) |
V (Å^{3}) | 169.0 (19) | 162 (2) | 321 (4) | 179.5 (12) |
Z | 2 | 2 | 4 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm^{−}^{1}) | 0.08 | 0.08 | 0.08 | 0.08 |
Crystal size (mm) | 0.42 × 0.42 × 0.10 | 0.41 × 0.41 × 0.09 | 0.41 × 0.41 × 0.08 | 0.42 × 0.42 × 0.11 |
Data collection | ||||
Diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer |
Absorption correction | Integration 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 | Integration 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 | Integration 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 | Integration 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} | 0.48, 0.94 | 0.45, 0.93 | 0.45, 0.93 | 0.47, 0.89 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1260, 117, 113 | 1159, 124, 103 | 2437, 235, 225 | 1272, 141, 125 |
R_{int} | 0.062 | 0.064 | 0.108 | 0.097 |
(sin θ/λ)_{max} (Å^{−}^{1}) | 0.680 | 0.691 | 0.700 | 0.688 |
Refinement | ||||
R[F^{2} > 2σ(F^{2})], wR(F^{2}), S | 0.142, 0.266, 1.76 | 0.064, 0.212, 0.96 | 0.237, 0.433, 1.39 | 0.055, 0.104, 1.10 |
No. of reflections | 117 | 124 | 235 | 141 |
No. of parameters | 20 | 25 | 26 | 25 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρ_{max}, Δρ_{min} (e Å^{−}^{3}) | 0.12, −0.13 | 0.10, −0.10 | 0.33, −0.27 | 0.10, −0.09 |
(DAE03G2) | (DAE05G) | |
Crystal data | ||
Chemical formula | C_{2}H_{8}N_{2} | C_{2}H_{8}N_{2} |
M_{r} | 60.10 | 60.10 |
Crystal system, space group | Monoclinic, P2_{1}/c | Monoclinic, P2_{1}/c |
Temperature (K) | 296 | 296 |
a, b, c (Å) | 5.031 (10), 5.132 (3), 7.167 (5) | 4.9921 (18), 5.137 (4), 7.200 (4) |
β (°) | 110.60 (12) | 110.87 (5) |
V (Å^{3}) | 173.2 (4) | 172.53 (19) |
Z | 2 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm^{−}^{1}) | 0.08 | 0.08 |
Crystal size (mm) | 0.40 × 0.40 × 0.09 | 0.35 × 0.35 × 0.08 |
Data collection | ||
Diffractometer | Kuma KM4CCD κ geometry diffractometer | Kuma KM4CCD κ geometry diffractometer |
Absorption correction | Integration 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 | Integration 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} | 0.55, 0.91 | 0.49, 0.82 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 897, 96, 72 | 1110, 206, 193 |
R_{int} | 0.091 | 0.063 |
(sin θ/λ)_{max} (Å^{−}^{1}) | 0.690 | 0.701 |
Refinement | ||
R[F^{2} > 2σ(F^{2})], wR(F^{2}), S | 0.074, 0.253, 1.22 | 0.059, 0.149, 1.07 |
No. of reflections | 96 | 206 |
No. of parameters | 20 | 25 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
Δρ_{max}, Δρ_{min} (e Å^{−}^{3}) | 0.15, −0.14 | 0.13, −0.15 |
Computer programs: CrysAlis (Oxford Diffraction, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001)
and POV-RAY (Persistence of Vision, 2004).