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1,2-Diaminoethane has been in-situ pressure- and temperature-frozen; apart from two known low-temperature phases, Iα and II, three new phases, Iβ, Iγ and III, have been observed and their structures determined by X-ray diffraction. The measurements at 0.1 MPa were carried out at 274, 243 and 224 K, and 296 K measurements were made at 0.15 GPa (phase Iα), at 0.3 and 1.1 GPa (phase Iβ), at 1.5 GPa (phase Iγ), and at 0.2, 0.3 and 0.5 GPa (phase III). All these phases are monoclinic, space group P21/c, but the unit-cell dimension of phases Iα and III are very different at 296 K: a = 5.078 (5), b = 7.204 (8), c = 5.528 (20) Å, β = 115.2 (2)° at 0.15 GPa, and aIII = 5.10 (3), bIII = 5.212 (2), cIII = 7.262 (12) Å, βIII = 111.6 (4)° at 0.2 GPa, respectively; in both phases Z = 2. An ambient-pressure low-temperature phase II has been observed below 189 K. Discontinuities in the unit-cell dimensions and in the N...N distance mark the isostructural transition between phases Iα and Iβ at 0.2 GPa, which can be attributed to a damping process of the NH2 group rotations. In phase Iγ the unit-cell parameter a doubles and Z increases to 4. The molecule has inversion symmetry in all the structures determined. 1,2-Diaminoethane can be considered as a simple structural ice analogue, but with NH...N hydrogen bonds and with the H-atom donors (four in one molecule) in excess over H-atom acceptors (two per molecule). Thus, the transformations of 1,2-diaminoethane phases involving the conformational dynamics affect the hydrogen-bonding geometry and molecular association in the crystal. The 1,2-diaminoethane:1,2-dihydroxyethane mixture has been separated by pressure-freezing, and a solid 1,2-diaminoethane crystal in liquid 1,2-dihyroxyethane has been obtained.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810602982X/av5066sup1.cif
Contains datablocks DAE224K, DAE243K, DAE274K, DAE015G, DAE03G1, DAE11G, DAE15G, DAE02G, DAE03G2, DAE05G

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae015gsup2.hkl
Contains datablock DAE015G

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae02gsup3.hkl
Contains datablock DAE02G

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae03g1sup4.hkl
Contains datablock DAE03G1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae03g2sup5.hkl
Contains datablock DAE03G2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae05gsup6.hkl
Contains datablock DAE05G

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae11gsup7.hkl
Contains datablock DAE11G

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae15gsup8.hkl
Contains datablock DAE15G

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae224ksup9.hkl
Contains datablock DAE224K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae243ksup10.hkl
Contains datablock DAE243K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810602982X/av5066dae274ksup11.hkl
Contains datablock DAE274K

CCDC references: 629848; 629849; 629850; 629851; 629852; 629853; 629854; 629855; 629856; 629857

Computing details top

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
[Figure 11]
[Figure 12]
(DAE224K) 1,2-diaminoethane phase I alpha top
Crystal data top
C2H8N2F(000) = 68
Mr = 60.10Dx = 1.100 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 5.065 (1) ÅCell parameters from 457 reflections
b = 7.181 (1) Åθ = 4.4–29.1°
c = 5.508 (1) ŵ = 0.07 mm1
β = 115.07 (3)°T = 224 K
V = 181.46 (7) Å3Plate, colourless
Z = 20.6 × 0.4 × 0.1 mm
Data collection top
Kuma KM4CCD κ geometry
diffractometer
369 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.061
Graphite monochromatorθmax = 29.1°, θmin = 4.4°
ω scansh = 66
1070 measured reflectionsk = 89
457 independent reflectionsl = 77
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.132 w = 1/[σ2(Fo2) + (0.0726P)2 + 0.0014P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max < 0.001
457 reflectionsΔρmax = 0.31 e Å3
25 parametersΔρmin = 0.16 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.33 (14)
Crystal data top
C2H8N2V = 181.46 (7) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 5.065 (1) ŵ = 0.07 mm1
b = 7.181 (1) ÅT = 224 K
c = 5.508 (1) Å0.6 × 0.4 × 0.1 mm
β = 115.07 (3)°
Data collection top
Kuma KM4CCD κ geometry
diffractometer
369 reflections with I > 2σ(I)
1070 measured reflectionsRint = 0.061
457 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.132H-atom parameters constrained
S = 1.11Δρmax = 0.31 e Å3
457 reflectionsΔρmin = 0.16 e Å3
25 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.8524 (2)0.36693 (15)0.21202 (19)0.0300 (4)
H10.98140.47250.27220.036*
H20.88060.31010.07750.036*
C10.5496 (2)0.43086 (17)0.1161 (2)0.0257 (4)
H40.52520.48820.26470.038 (4)*
H30.42250.32300.06060.033 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0290 (7)0.0326 (7)0.0281 (6)0.0037 (4)0.0117 (5)0.0029 (4)
C10.0283 (7)0.0252 (7)0.0259 (6)0.0004 (4)0.0137 (5)0.0025 (4)
Geometric parameters (Å, º) top
N1—C11.4682 (15)C1—C1i1.526 (2)
N1—H10.9634C1—H40.9700
N1—H20.9084C1—H30.9700
C1—N1—H1109.3C1i—C1—H4108.4
C1—N1—H2110.4N1—C1—H3108.4
H1—N1—H2108.4C1i—C1—H3108.4
N1—C1—C1i115.33 (12)H4—C1—H3107.5
N1—C1—H4108.4
Symmetry code: (i) x+1, y+1, z.
(DAE243K) 1,2-diaminoethane phase I alpha top
Crystal data top
C2H8N2Dx = 1.100 Mg m3
Mr = 60.10Melting point: 284.29 K
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 5.070 (1) ÅCell parameters from 866 reflections
b = 7.185 (1) Åθ = 4.4–29.1°
c = 5.501 (1) ŵ = 0.07 mm1
β = 115.11 (3)°T = 243 K
V = 181.45 (7) Å3Plate, colourless
Z = 20.6 × 0.4 × 0.1 mm
F(000) = 68
Data collection top
Kuma KM4CCD κ geometry
diffractometer
406 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.048
Graphite monochromatorθmax = 29.1°, θmin = 4.4°
ω scansh = 66
1241 measured reflectionsk = 89
458 independent reflectionsl = 76
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.112 w = 1/[σ2(Fo2) + (0.059P)2 + 0.0216P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max < 0.001
458 reflectionsΔρmax = 0.34 e Å3
25 parametersΔρmin = 0.15 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.38 (11)
Crystal data top
C2H8N2V = 181.45 (7) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 5.070 (1) ŵ = 0.07 mm1
b = 7.185 (1) ÅT = 243 K
c = 5.501 (1) Å0.6 × 0.4 × 0.1 mm
β = 115.11 (3)°
Data collection top
Kuma KM4CCD κ geometry
diffractometer
406 reflections with I > 2σ(I)
1241 measured reflectionsRint = 0.048
458 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0400 restraints
wR(F2) = 0.112H-atom parameters constrained
S = 1.11Δρmax = 0.34 e Å3
458 reflectionsΔρmin = 0.15 e Å3
25 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.85189 (18)0.36691 (12)0.21189 (17)0.0296 (4)
H10.88140.30780.06820.036*
H20.97200.46710.26830.036*
C10.5496 (2)0.43080 (13)0.11635 (18)0.0252 (4)
H40.52560.48820.26530.035 (3)*
H30.42240.32310.06070.034 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0281 (5)0.0328 (6)0.0269 (5)0.0032 (3)0.0107 (4)0.0034 (3)
C10.0282 (6)0.0250 (5)0.0242 (5)0.0001 (3)0.0128 (4)0.0024 (3)
Geometric parameters (Å, º) top
N1—C11.4672 (13)C1—C1i1.5277 (18)
N1—H10.9631C1—H40.9700
N1—H20.9084C1—H30.9700
C1—N1—H1110.3C1i—C1—H4108.5
C1—N1—H2108.7N1—C1—H3108.5
H1—N1—H2108.4C1i—C1—H3108.5
N1—C1—C1i115.22 (9)H4—C1—H3107.5
N1—C1—H4108.5
Symmetry code: (i) x+1, y+1, z.
(DAE274K) 1,2-diaminoethane phase I alpha top
Crystal data top
C2H8N2F(000) = 68
Mr = 60.10Dx = 1.085 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 5.102 (1) ÅCell parameters from 240 reflections
b = 7.197 (1) Åθ = 4.4–28.6°
c = 5.535 (1) ŵ = 0.07 mm1
β = 115.18 (3)°T = 274 K
V = 183.93 (7) Å3Plate, colourless
Z = 20.6 × 0.4 × 0.1 mm
Data collection top
Kuma KM4CCD κ geometry
diffractometer
330 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.129
Graphite monochromatorθmax = 28.6°, θmin = 4.4°
ω scansh = 66
940 measured reflectionsk = 89
452 independent reflectionsl = 76
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.085H-atom parameters constrained
wR(F2) = 0.210 w = 1/[σ2(Fo2) + (0.1384P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
452 reflectionsΔρmax = 0.35 e Å3
25 parametersΔρmin = 0.29 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.6 (3)
Crystal data top
C2H8N2V = 183.93 (7) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 5.102 (1) ŵ = 0.07 mm1
b = 7.197 (1) ÅT = 274 K
c = 5.535 (1) Å0.6 × 0.4 × 0.1 mm
β = 115.18 (3)°
Data collection top
Kuma KM4CCD κ geometry
diffractometer
330 reflections with I > 2σ(I)
940 measured reflectionsRint = 0.129
452 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0850 restraints
wR(F2) = 0.210H-atom parameters constrained
S = 1.04Δρmax = 0.35 e Å3
452 reflectionsΔρmin = 0.29 e Å3
25 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.8483 (3)0.3676 (2)0.2102 (3)0.0444 (7)
H10.98570.46830.28010.053*
H20.87440.31380.07270.053*
C10.5494 (3)0.4318 (2)0.1156 (3)0.0380 (7)
H40.52650.48990.26360.039 (4)*
H30.42260.32440.06150.052 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0385 (11)0.0432 (11)0.0442 (10)0.0051 (6)0.0106 (7)0.0048 (6)
C10.0388 (11)0.0318 (10)0.0404 (10)0.0011 (6)0.0140 (7)0.0030 (6)
Geometric parameters (Å, º) top
N1—C11.461 (2)C1—C1i1.519 (3)
N1—H10.9670C1—H40.9700
N1—H20.9127C1—H30.9700
C1—N1—H1112.0C1i—C1—H4108.4
C1—N1—H2109.6N1—C1—H3108.4
H1—N1—H2108.2C1i—C1—H3108.4
N1—C1—C1i115.35 (18)H4—C1—H3107.5
N1—C1—H4108.4
Symmetry code: (i) x+1, y+1, z.
(DAE015G) 1,2-diaminoethane phase I alpha top
Crystal data top
C2H8N2The unit-cell dimensions corrected for the effect of the gasket-shadowing:
Katrusiak Andrzej - being prepared for publication
Mr = 60.10Dx = 1.091 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 5.078 (5) ÅCell parameters from 355 reflections
b = 7.204 (8) Åθ = 4.4–29.6°
c = 5.528 (12) ŵ = 0.07 mm1
β = 115.24 (18)°T = 296 K
V = 182.9 (6) Å3, colourless
Z = 20.30 × 0.30 × 0.08 mm
F(000) = 68
Data collection top
Kuma KM4CCD κ geometry
diffractometer
224 independent reflections
Radiation source: fine-focus sealed tube188 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.075
Detector resolution: 16.4 pixels mm-1θmax = 29.6°, θmin = 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 = 66
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 = 88
Tmin = 0.44, Tmax = 0.84l = 55
1259 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.084H-atom parameters constrained
wR(F2) = 0.130 w = 1/[σ2(Fo2) + (0.P)2 + 0.1653P]
where P = (Fo2 + 2Fc2)/3
S = 1.25(Δ/σ)max < 0.001
224 reflectionsΔρmax = 0.10 e Å3
25 parametersΔρmin = 0.11 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 1.00 (13)
Crystal data top
C2H8N2V = 182.9 (6) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 5.078 (5) ŵ = 0.07 mm1
b = 7.204 (8) ÅT = 296 K
c = 5.528 (12) Å0.30 × 0.30 × 0.08 mm
β = 115.24 (18)°
Data collection top
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)
Tmin = 0.44, Tmax = 0.84Rint = 0.075
1259 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0840 restraints
wR(F2) = 0.130H-atom parameters constrained
S = 1.25Δρmax = 0.10 e Å3
224 reflectionsΔρmin = 0.11 e Å3
25 parameters
Special details top

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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.8491 (8)0.3686 (5)0.2117 (10)0.0493 (14)
H10.97390.47670.25500.059*
H20.86990.30490.07870.059*
C10.5489 (7)0.4333 (6)0.1154 (11)0.0423 (14)
H40.52570.49260.26270.057 (13)*
H30.42110.32610.06230.032 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0464 (19)0.060 (3)0.039 (4)0.0037 (15)0.0158 (19)0.0043 (15)
C10.047 (2)0.048 (4)0.034 (5)0.0048 (17)0.019 (2)0.0019 (15)
Geometric parameters (Å, º) top
N1—C11.461 (5)C1—C1i1.503 (9)
N1—H10.9673C1—H40.9700
N1—H20.9100C1—H30.9700
C1—N1—H1107.8C1i—C1—H4108.4
C1—N1—H2109.2N1—C1—H3108.4
H1—N1—H2108.5C1i—C1—H3108.4
N1—C1—C1i115.4 (5)H4—C1—H3107.5
N1—C1—H4108.4
Symmetry code: (i) x+1, y+1, z.
(DAE03G1) 1,2-diaminoethane phase I beta top
Crystal data top
C2H8N2The unit-cell dimensions corrected for the effect of the gasket-shadowing:
Katrusiak Andrzej - being prepared for publication
Mr = 60.10Dx = 1.182 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 4.949 (6) ÅCell parameters from 343 reflections
b = 7.704 (8) Åθ = 5.3–28.9°
c = 4.96 (3) ŵ = 0.08 mm1
β = 116.7 (11)°T = 296 K
V = 169.0 (19) Å3, colourless
Z = 20.42 × 0.42 × 0.10 mm
F(000) = 68
Data collection top
Kuma KM4CCD κ geometry
diffractometer
117 independent reflections
Radiation source: fine-focus sealed tube113 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.062
Detector resolution: 16.4 pixels mm-1θmax = 28.9°, θmin = 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 = 33
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 = 1010
Tmin = 0.48, Tmax = 0.94l = 66
1260 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.142H-atom parameters constrained
wR(F2) = 0.266 w = 1/[σ2(Fo2) + (0.050P)2 + 0.3P]
where P = (Fo2 + 2Fc2)/3
S = 1.76(Δ/σ)max < 0.001
117 reflectionsΔρmax = 0.12 e Å3
20 parametersΔρmin = 0.13 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.3 (2)
Crystal data top
C2H8N2V = 169.0 (19) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 4.949 (6) ŵ = 0.08 mm1
b = 7.704 (8) ÅT = 296 K
c = 4.96 (3) Å0.42 × 0.42 × 0.10 mm
β = 116.7 (11)°
Data collection top
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)
Tmin = 0.48, Tmax = 0.94Rint = 0.062
1260 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.1420 restraints
wR(F2) = 0.266H-atom parameters constrained
S = 1.76Δρmax = 0.12 e Å3
117 reflectionsΔρmin = 0.13 e Å3
20 parameters
Special details top

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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.777 (5)0.3540 (11)0.276 (3)0.045 (3)*
H10.85960.30220.16280.054*
H20.93070.39620.44510.054*
C10.501 (7)0.4352 (12)0.112 (3)0.05 (2)
H40.44230.49270.25120.05 (2)*
H30.35000.34720.00540.11 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.07 (7)0.042 (5)0.050 (15)0.005 (11)0.03 (3)0.002 (6)
Geometric parameters (Å, º) top
N1—C11.39 (4)C1—C1i1.487 (18)
N1—H10.9174C1—H40.9700
N1—H20.9023C1—H30.9700
C1—N1—H1115.4C1i—C1—H4108.7
C1—N1—H2125.4N1—C1—H3108.7
H1—N1—H2107.9C1i—C1—H3108.7
N1—C1—C1i114 (3)H4—C1—H3107.6
N1—C1—H4108.7
Symmetry code: (i) x+1, y+1, z.
(DAE11G) 1,2-diaminoethane phase I beta top
Crystal data top
C2H8N2The unit-cell dimensions corrected for the effect of the gasket-shadowing:
Katrusiak Andrzej - being prepared for publication
Mr = 60.10Dx = 1.236 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 4.82 (5) ÅCell parameters from 510 reflections
b = 7.563 (5) Åθ = 5.3–29.4°
c = 4.873 (18) ŵ = 0.08 mm1
β = 114.5 (8)°T = 296 K
V = 162 (2) Å3, colourless
Z = 20.41 × 0.41 × 0.09 mm
F(000) = 68
Data collection top
Kuma KM4CCD κ geometry
diffractometer
124 independent reflections
Radiation source: fine-focus sealed tube103 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.064
Detector resolution: 16.4 pixels mm-1θmax = 29.4°, θmin = 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 = 33
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 = 1010
Tmin = 0.45, Tmax = 0.93l = 66
1159 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.064H-atom parameters constrained
wR(F2) = 0.212 w = 1/[σ2(Fo2) + (0.1176P)2 + 0.1743P]
where P = (Fo2 + 2Fc2)/3
S = 0.96(Δ/σ)max < 0.001
124 reflectionsΔρmax = 0.10 e Å3
25 parametersΔρmin = 0.10 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 1.0 (6)
Crystal data top
C2H8N2V = 162 (2) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 4.82 (5) ŵ = 0.08 mm1
b = 7.563 (5) ÅT = 296 K
c = 4.873 (18) Å0.41 × 0.41 × 0.09 mm
β = 114.5 (8)°
Data collection top
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)
Tmin = 0.45, Tmax = 0.93Rint = 0.064
1159 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0640 restraints
wR(F2) = 0.212H-atom parameters constrained
S = 0.96Δρmax = 0.10 e Å3
124 reflectionsΔρmin = 0.10 e Å3
25 parameters
Special details top

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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.794 (3)0.3522 (6)0.2867 (16)0.071 (10)
H10.84360.29670.15200.085*
H20.95500.41520.41010.085*
C10.495 (4)0.4306 (7)0.1128 (19)0.055 (13)
H40.42130.48570.24980.059 (15)*
H30.35210.33800.00410.10 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.11 (3)0.047 (2)0.070 (7)0.014 (5)0.052 (13)0.014 (2)
C10.08 (4)0.045 (3)0.053 (7)0.005 (5)0.039 (16)0.007 (3)
Geometric parameters (Å, º) top
N1—C11.46 (3)C1—C1i1.536 (11)
N1—H10.8923C1—H40.9700
N1—H20.8967C1—H30.9700
C1—N1—H1105.4C1i—C1—H4109.2
C1—N1—H2123.0N1—C1—H3109.2
H1—N1—H2108.6C1i—C1—H3109.2
N1—C1—C1i112.1 (18)H4—C1—H3107.9
N1—C1—H4109.2
Symmetry code: (i) x+1, y+1, z.
(DAE15G) 1,2-diaminoethane phase I gamma top
Crystal data top
C2H8N2The unit-cell dimensions corrected for the effect of the gasket-shadowing:
Katrusiak Andrzej - being prepared for publication
Mr = 60.10Dx = 1.243 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 9.69 (10) ÅCell parameters from 516 reflections
b = 7.488 (5) Åθ = 5.0–29.8°
c = 4.849 (14) ŵ = 0.08 mm1
β = 114.0 (7)°T = 296 K
V = 321 (4) Å3, colourless
Z = 40.41 × 0.41 × 0.08 mm
F(000) = 136
Data collection top
Kuma KM4CCD κ geometry
diffractometer
235 independent reflections
Radiation source: fine-focus sealed tube225 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.108
Detector resolution: 16.4 pixels mm-1θmax = 29.8°, θmin = 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 = 55
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 = 1010
Tmin = 0.45, Tmax = 0.93l = 66
2437 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.237H-atom parameters constrained
wR(F2) = 0.433 w = 1/[σ2(Fo2) + (0.050P)2 + 5.P]
where P = (Fo2 + 2Fc2)/3
S = 1.39(Δ/σ)max < 0.001
235 reflectionsΔρmax = 0.33 e Å3
26 parametersΔρmin = 0.27 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.8 (3)
Crystal data top
C2H8N2V = 321 (4) Å3
Mr = 60.10Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.69 (10) ŵ = 0.08 mm1
b = 7.488 (5) ÅT = 296 K
c = 4.849 (14) Å0.41 × 0.41 × 0.08 mm
β = 114.0 (7)°
Data collection top
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)
Tmin = 0.45, Tmax = 0.93Rint = 0.108
2437 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.2370 restraints
wR(F2) = 0.433H-atom parameters constrained
S = 1.39Δρmax = 0.33 e Å3
235 reflectionsΔρmin = 0.27 e Å3
26 parameters
Special details top

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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.144 (4)0.3449 (13)0.275 (3)0.012 (3)*
H10.13500.23120.30930.014*
H20.20690.35590.17800.014*
C10.004 (7)0.436 (2)0.105 (5)0.037 (5)*
H30.03520.49490.24790.045*
H40.07910.34690.00180.045*
N20.651 (5)0.3723 (17)0.317 (4)0.036 (5)*
H70.69420.30600.22190.043*
H80.66990.32120.49650.043*
C20.503 (6)0.4301 (18)0.118 (5)0.029 (5)*
H50.45310.47900.23860.035*
H60.44560.32640.01270.035*
Geometric parameters (Å, º) top
N1—C11.49 (6)N2—C21.43 (6)
N1—H10.8791N2—H70.8906
N1—H20.9119N2—H80.8984
C1—C1i1.42 (3)C2—C2ii1.53 (3)
C1—H30.9700C2—H50.9700
C1—H40.9700C2—H60.9700
C1—N1—H1113.6C2—N2—H7111.9
C1—N1—H2111.5C2—N2—H8122.4
H1—N1—H2108.9H7—N2—H8108.1
N1—C1—C1i113 (6)N2—C2—C2ii116 (6)
N1—C1—H3109.0N2—C2—H5108.4
C1i—C1—H3109.0C2ii—C2—H5108.4
N1—C1—H4109.0N2—C2—H6108.4
C1i—C1—H4109.0C2ii—C2—H6108.4
H3—C1—H4107.8H5—C2—H6107.4
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+1, z.
(DAE02G) 1,2-diaminoethane phase II top
Crystal data top
C2H8N2The unit-cell dimensions corrected for the effect of the gasket-shadowing:
Katrusiak Andrzej - being prepared for publication
Mr = 60.10Dx = 1.113 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 5.10 (3) ÅCell parameters from 794 reflections
b = 5.212 (2) Åθ = 4.9–29.3°
c = 7.262 (12) ŵ = 0.08 mm1
β = 111.6 (4)°T = 296 K
V = 179.5 (12) Å3, colourless
Z = 20.42 × 0.42 × 0.11 mm
F(000) = 68
Data collection top
Kuma KM4CCD κ geometry
diffractometer
141 independent reflections
Radiation source: fine-focus sealed tube125 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.097
Detector resolution: 16.4 pixels mm-1θmax = 29.3°, θmin = 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 = 33
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 = 77
Tmin = 0.47, Tmax = 0.89l = 99
1272 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.055H-atom parameters constrained
wR(F2) = 0.104 w = 1/[σ2(Fo2) + (0.0185P)2 + 0.1484P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
141 reflectionsΔρmax = 0.10 e Å3
25 parametersΔρmin = 0.09 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 10.4 (13)
Crystal data top
C2H8N2V = 179.5 (12) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 5.10 (3) ŵ = 0.08 mm1
b = 5.212 (2) ÅT = 296 K
c = 7.262 (12) Å0.42 × 0.42 × 0.11 mm
β = 111.6 (4)°
Data collection top
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)
Tmin = 0.47, Tmax = 0.89Rint = 0.097
1272 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0550 restraints
wR(F2) = 0.104H-atom parameters constrained
S = 1.10Δρmax = 0.10 e Å3
141 reflectionsΔρmin = 0.09 e Å3
25 parameters
Special details top

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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.824 (3)0.7076 (8)0.6248 (9)0.060 (9)
H10.90580.74990.52800.072*
H20.93380.56020.67800.072*
C10.536 (3)0.6165 (8)0.5673 (10)0.067 (10)
H30.40940.75500.50090.046 (16)*
H40.50080.57520.68640.030 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.09 (3)0.038 (2)0.049 (5)0.004 (5)0.026 (11)0.006 (2)
C10.14 (3)0.026 (2)0.049 (5)0.004 (5)0.053 (12)0.000 (2)
Geometric parameters (Å, º) top
N1—C11.45 (2)C1—C1i1.517 (10)
N1—H10.9644C1—H30.9700
N1—H20.9443C1—H40.9700
C1—N1—H1121.9C1i—C1—H3108.5
C1—N1—H2103.6N1—C1—H4108.5
H1—N1—H297.8C1i—C1—H4108.5
N1—C1—C1i115.2 (14)H3—C1—H4107.5
N1—C1—H3108.5
Symmetry code: (i) x+1, y+1, z+1.
(DAE03G2) 1,2-diaminoethane phase II top
Crystal data top
C2H8N2The unit-cell dimensions corrected for the effect of the gasket-shadowing:
Katrusiak Andrzej - being prepared for publication
Mr = 60.10Dx = 1.152 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 5.031 (10) ÅCell parameters from 697 reflections
b = 5.132 (3) Åθ = 5.0–29.4°
c = 7.167 (5) ŵ = 0.08 mm1
β = 110.60 (12)°T = 296 K
V = 173.2 (4) Å3, colourless
Z = 20.40 × 0.40 × 0.09 mm
F(000) = 68
Data collection top
Kuma KM4CCD κ geometry
diffractometer
96 independent reflections
Radiation source: fine-focus sealed tube72 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.091
Detector resolution: 16.4 pixels mm-1θmax = 29.4°, θmin = 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 = 33
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 = 66
Tmin = 0.55, Tmax = 0.91l = 99
897 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.074H-atom parameters constrained
wR(F2) = 0.253 w = 1/[σ2(Fo2) + (0.1848P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.22(Δ/σ)max < 0.001
96 reflectionsΔρmax = 0.15 e Å3
20 parametersΔρmin = 0.14 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.3 (4)
Crystal data top
C2H8N2V = 173.2 (4) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 5.031 (10) ŵ = 0.08 mm1
b = 5.132 (3) ÅT = 296 K
c = 7.167 (5) Å0.40 × 0.40 × 0.09 mm
β = 110.60 (12)°
Data collection top
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)
Tmin = 0.55, Tmax = 0.91Rint = 0.091
897 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0740 restraints
wR(F2) = 0.253H-atom parameters constrained
S = 1.22Δρmax = 0.15 e Å3
96 reflectionsΔρmin = 0.14 e Å3
20 parameters
Special details top

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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.820 (6)0.7126 (10)0.6209 (18)0.11 (2)
H10.84830.72230.49700.138*
H20.96040.58910.68170.138*
C10.542 (5)0.6209 (14)0.5720 (15)0.043 (3)*
H30.41280.76250.51090.18 (11)*
H40.51240.57530.69460.027 (12)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.25 (6)0.036 (3)0.097 (12)0.008 (10)0.11 (3)0.002 (4)
Geometric parameters (Å, º) top
N1—C11.40 (4)C1—C1i1.574 (19)
N1—H10.9479C1—H30.9700
N1—H20.9334C1—H40.9700
C1—N1—H1104.4C1i—C1—H3108.2
C1—N1—H2114.4N1—C1—H4108.2
H1—N1—H297.9C1i—C1—H4108.2
N1—C1—C1i116 (2)H3—C1—H4107.4
N1—C1—H3108.2
Symmetry code: (i) x+1, y+1, z+1.
(DAE05G) 1,2-diaminoethane phase II top
Crystal data top
C2H8N2The unit-cell dimensions corrected for the effect of the gasket-shadowing:
Katrusiak Andrzej - being prepared for publication
Mr = 60.10Dx = 1.157 Mg m3
Monoclinic, P21/cMelting point: 284.29 K
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 4.9921 (18) ÅCell parameters from 761 reflections
b = 5.137 (4) Åθ = 4.4–29.9°
c = 7.200 (4) ŵ = 0.08 mm1
β = 110.87 (5)°T = 296 K
V = 172.53 (19) Å3, colourless
Z = 20.35 × 0.35 × 0.08 mm
F(000) = 68
Data collection top
Kuma KM4CCD κ geometry
diffractometer
206 independent reflections
Radiation source: fine-focus sealed tube193 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.063
Detector resolution: 16.4 pixels mm-1θmax = 29.9°, θmin = 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 = 66
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 = 44
Tmin = 0.49, Tmax = 0.82l = 88
1110 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.059H-atom parameters constrained
wR(F2) = 0.149 w = 1/[σ2(Fo2) + (0.0578P)2 + 0.1608P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
206 reflectionsΔρmax = 0.13 e Å3
25 parametersΔρmin = 0.15 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.3 (2)
Crystal data top
C2H8N2V = 172.53 (19) Å3
Mr = 60.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 4.9921 (18) ŵ = 0.08 mm1
b = 5.137 (4) ÅT = 296 K
c = 7.200 (4) Å0.35 × 0.35 × 0.08 mm
β = 110.87 (5)°
Data collection top
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)
Tmin = 0.49, Tmax = 0.82Rint = 0.063
1110 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0590 restraints
wR(F2) = 0.149H-atom parameters constrained
S = 1.07Δρmax = 0.13 e Å3
206 reflectionsΔρmin = 0.15 e Å3
25 parameters
Special details top

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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.8294 (5)0.7134 (7)0.6240 (4)0.0389 (11)
H10.87020.72320.50520.047*
H20.95950.58290.68770.047*
C10.5352 (6)0.6194 (9)0.5681 (5)0.0305 (11)
H30.40600.75930.50190.049 (10)*
H40.49880.57710.68820.034 (8)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0366 (14)0.028 (3)0.049 (2)0.0029 (13)0.0115 (11)0.0056 (10)
C10.0351 (14)0.021 (4)0.035 (3)0.0021 (12)0.0114 (12)0.0012 (9)
Geometric parameters (Å, º) top
N1—C11.460 (4)C1—C1i1.531 (6)
N1—H10.9483C1—H30.9700
N1—H20.9324C1—H40.9700
C1—N1—H1106.7C1i—C1—H3108.5
C1—N1—H2110.7N1—C1—H4108.5
H1—N1—H298.4C1i—C1—H4108.5
N1—C1—C1i114.9 (3)H3—C1—H4107.5
N1—C1—H3108.5
Symmetry code: (i) x+1, y+1, z+1.

Experimental details

(DAE224K)(DAE243K)(DAE274K)(DAE015G)
Crystal data
Chemical formulaC2H8N2C2H8N2C2H8N2C2H8N2
Mr60.1060.1060.1060.10
Crystal system, space groupMonoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)224243274296
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)
V3)181.46 (7)181.45 (7)183.93 (7)182.9 (6)
Z2222
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.070.070.070.07
Crystal size (mm)0.6 × 0.4 × 0.10.6 × 0.4 × 0.10.6 × 0.4 × 0.10.30 × 0.30 × 0.08
Data collection
DiffractometerKuma KM4CCD κ geometry
diffractometer
Kuma KM4CCD κ geometry
diffractometer
Kuma KM4CCD κ geometry
diffractometer
Kuma KM4CCD κ geometry
diffractometer
Absorption correctionIntegration
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, Tmax0.44, 0.84
No. of measured, independent and
observed [I > 2σ(I)] reflections
1070, 457, 369 1241, 458, 406 940, 452, 330 1259, 224, 188
Rint0.0610.0480.1290.075
(sin θ/λ)max1)0.6830.6830.6730.696
Refinement
R[F2 > 2σ(F2)], wR(F2), 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 reflections457458452224
No. of parameters25252525
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.31, 0.160.34, 0.150.35, 0.290.10, 0.11


(DAE03G1)(DAE11G)(DAE15G)(DAE02G)
Crystal data
Chemical formulaC2H8N2C2H8N2C2H8N2C2H8N2
Mr60.1060.1060.1060.10
Crystal system, space groupMonoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)296296296296
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)
V3)169.0 (19)162 (2)321 (4)179.5 (12)
Z2242
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.080.080.080.08
Crystal size (mm)0.42 × 0.42 × 0.100.41 × 0.41 × 0.090.41 × 0.41 × 0.080.42 × 0.42 × 0.11
Data collection
DiffractometerKuma KM4CCD κ geometry
diffractometer
Kuma KM4CCD κ geometry
diffractometer
Kuma KM4CCD κ geometry
diffractometer
Kuma KM4CCD κ geometry
diffractometer
Absorption correctionIntegration
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

Tmin, Tmax0.48, 0.940.45, 0.930.45, 0.930.47, 0.89
No. of measured, independent and
observed [I > 2σ(I)] reflections
1260, 117, 113 1159, 124, 103 2437, 235, 225 1272, 141, 125
Rint0.0620.0640.1080.097
(sin θ/λ)max1)0.6800.6910.7000.688
Refinement
R[F2 > 2σ(F2)], wR(F2), 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 reflections117124235141
No. of parameters20252625
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.12, 0.130.10, 0.100.33, 0.270.10, 0.09


(DAE03G2)(DAE05G)
Crystal data
Chemical formulaC2H8N2C2H8N2
Mr60.1060.10
Crystal system, space groupMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)296296
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)
V3)173.2 (4)172.53 (19)
Z22
Radiation typeMo KαMo Kα
µ (mm1)0.080.08
Crystal size (mm)0.40 × 0.40 × 0.090.35 × 0.35 × 0.08
Data collection
DiffractometerKuma KM4CCD κ geometry
diffractometer
Kuma KM4CCD κ geometry
diffractometer
Absorption correctionIntegration
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

Tmin, Tmax0.55, 0.910.49, 0.82
No. of measured, independent and
observed [I > 2σ(I)] reflections
897, 96, 72 1110, 206, 193
Rint0.0910.063
(sin θ/λ)max1)0.6900.701
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.074, 0.253, 1.22 0.059, 0.149, 1.07
No. of reflections96206
No. of parameters2025
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.15, 0.140.13, 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).

 

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