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When calculating derivatives of structure factors, there is one particular term (the derivatives of the atomic form factors) that will always be zero in the case of tabulated spherical atomic form factors. What happens if the form factors are non-spherical? The assumption that this particular term is very close to zero is generally made in non-spherical refinements (for example, implementations of Hirshfeld atom refinement or transferable aspherical atom models), unless the form factors are refinable parameters (for example multipole modelling). To evaluate this general approximation for one specific method, a numerical differentiation was implemented within the NoSpherA2 framework to calculate the derivatives of the structure factors in a Hirshfeld atom refinement directly as accurately as possible, thus bypassing the approximation altogether. Comparing wR2 factors and atomic parameters, along with their uncertainties from the approximate and numerically differentiating refinements, it turns out that the impact of this approximation on the final crystallographic model is indeed negligible.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053273321009086/pl5014sup1.cif
Contains datablocks epoxide_app, epoxide_hyb, epoxide_num, epoxide_spher, L-Ala_23K_tonto_IAM_app, L-Ala_23K_tonto_IAM_hyb, L-Ala_23K_tonto_IAM_num, L-Ala_23K_tonto_IAM_spher, nh30r_app, nh30r_hyb, nh30r_num, nh30r_spher

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Portable Document Format (PDF) file https://doi.org/10.1107/S2053273321009086/pl5014sup2.pdf
Supporting information

zip

Zip compressed file https://doi.org/10.1107/S2053273321009086/pl5014sup3.zip
Code used for calculations

Computing details top

For all structures, program(s) used to refine structure: olex2.refine 1.5-dev (Bourhis et al., 2015); molecular graphics: Olex2 1.5-dev (Dolomanov et al., 2009); software used to prepare material for publication: Olex2 1.5-dev (Dolomanov et al., 2009).

(epoxide_app) top
Crystal data top
C2H4OV = 251.8 (3) Å3
Mr = 44.05Z = 4
Monoclinic, P21/nF(000) = 96.064
a = 4.633 (5) ÅDx = 1.162 Mg m3
b = 8.400 (1) ÅMo Kα radiation, λ = 0.71068 Å
c = 6.577 (3) ŵ = 0.09 mm1
β = 100.37 (6)°T = 100 K
Data collection top
2081 measured reflectionsθmax = 35.0°, θmin = 4.0°
1109 independent reflectionsh = 96
899 reflections with I 2u(I)k = 016
Rint = 0.0000l = 613
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.023All H-atom parameters refined
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.47(Δ/σ)max = 0.0003
1109 reflectionsΔρmax = 0.15 e Å3
64 parametersΔρmin = 0.19 e Å3
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. DOI 10.1039/D0SC05526C - 2020 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fregment can be embedded in an electrostatic crystal field by employing cluster charges. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-07_11-39-49

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.11630 (7)0.83106 (3)0.12462 (5)0.02954 (8)
C20.14861 (9)0.93867 (5)0.29600 (7)0.02822 (9)
H2a0.2818 (18)0.8900 (8)0.4368 (10)0.065 (2)
H2b0.1738 (15)1.0619 (7)0.2565 (12)0.053 (2)
C30.13420 (10)0.86455 (6)0.21817 (7)0.03217 (10)
H3a0.3087 (18)0.9333 (9)0.1202 (12)0.069 (3)
H3b0.2035 (18)0.7647 (10)0.3037 (13)0.069 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.03540 (16)0.02562 (12)0.02939 (14)0.00304 (12)0.01060 (12)0.00355 (11)
C20.03242 (19)0.02498 (16)0.02736 (18)0.00039 (14)0.00569 (15)0.00209 (13)
H2a0.081 (6)0.072 (5)0.031 (4)0.022 (5)0.015 (4)0.009 (4)
H2b0.064 (6)0.026 (4)0.071 (5)0.008 (3)0.018 (4)0.003 (4)
C30.0306 (2)0.0338 (2)0.0343 (2)0.00344 (16)0.01197 (17)0.00000 (16)
H3a0.049 (5)0.104 (7)0.051 (5)0.028 (5)0.001 (4)0.013 (5)
H3b0.072 (6)0.063 (5)0.077 (5)0.034 (5)0.028 (5)0.004 (5)
Geometric parameters (Å, º) top
O1—C21.4316 (7)C2—C31.4577 (14)
O1—C31.4359 (13)C3—H3a1.102 (8)
C2—H2a1.095 (7)C3—H3b1.090 (7)
C2—H2b1.079 (6)
C3—O1—C261.11 (3)C2—C3—O159.30 (3)
H2a—C2—O1113.1 (4)H3a—C3—O1114.6 (4)
H2b—C2—O1114.6 (4)H3a—C3—C2120.0 (4)
H2b—C2—H2a119.5 (6)H3b—C3—O1114.0 (4)
C3—C2—O159.59 (3)H3b—C3—C2118.5 (5)
C3—C2—H2a118.1 (4)H3b—C3—H3a116.8 (7)
C3—C2—H2b117.0 (4)
(epoxide_hyb) top
Crystal data top
C2H4OV = 251.8 (3) Å3
Mr = 44.05Z = 4
Monoclinic, P21/nF(000) = 96.064
a = 4.633 (5) ÅDx = 1.162 Mg m3
b = 8.400 (1) ÅMo Kα radiation, λ = 0.71068 Å
c = 6.577 (3) ŵ = 0.09 mm1
β = 100.37 (6)°T = 100 K
Data collection top
2081 measured reflectionsθmax = 35.0°, θmin = 4.0°
1109 independent reflectionsh = 96
899 reflections with I 2u(I)k = 016
Rint = 0.0000l = 613
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.023All H-atom parameters refined
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.47(Δ/σ)max = 0.0003
1109 reflectionsΔρmax = 0.15 e Å3
64 parametersΔρmin = 0.19 e Å3
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. DOI 10.1039/D0SC05526C - 2020 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fregment can be embedded in an electrostatic crystal field by employing cluster charges. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-07_11-39-49

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
O10.11630 (7)0.83105 (3)0.12462 (5)
C20.14860 (10)0.93867 (5)0.29601 (7)
H2a0.2819 (18)0.8902 (9)0.4368 (10)
H2b0.1742 (15)1.0620 (7)0.2566 (11)
C30.13422 (11)0.86456 (6)0.21816 (7)
H3a0.30970 (17)0.9332 (9)0.1197 (11)
H3b0.2033 (18)0.7645 (10)0.3035 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.03541 (16)0.02562 (12)0.02940 (14)0.00356 (11)0.01061 (12)0.00304 (12)
C20.0324 (2)0.02500 (17)0.02736 (18)0.00209 (14)0.00568 (15)0.00038 (14)
H2a0.082 (6)0.072 (6)0.031 (4)0.009 (5)0.015 (5)0.023 (6)
H2b0.064 (6)0.026 (4)0.070 (5)0.003 (4)0.018 (4)0.008 (3)
C30.0307 (2)0.0338 (2)0.0344 (2)0.00002 (16)0.01197 (17)0.00346 (16)
H3a0.048 (5)0.104 (8)0.051 (5)0.013 (5)0.002 (4)0.028 (6)
H3b0.071 (6)0.063 (5)0.076 (6)0.004 (6)60.027 (5)0.034 (5)
Geometric parameters (Å, º) top
O1—C21.4316 (5)C2—C31.4578 (6)
O1—C31.4359 (5)C3—H3a1.106 (7)
C2—H2a1.095 (6)C3—H3b1.090 (7)
C2—H2b1.080 (5)
C3—O1—C261.11 (3)C2—C3—O159.30 (3)
H2a—C2—O1113.2 (4)H3a—C3—O1114.6 (4)
H2b—C2—O1114.7 (4)H3a—C3—C2120.1 (4)
H2b—C2—H2a119.4 (6)H3b—C3—O1113.8 (4)
C3—C2—O159.59 (3)H3b—C3—C2118.5 (5)
C3—C2—H2a118.2 (4)H3b—C3—H3a116.8 (7)
C3—C2—H2b117.1 (4)
(epoxide_num) top
Crystal data top
C2H4OV = 251.8 (3) Å3
Mr = 44.05Z = 4
Monoclinic, P21/nF(000) = 96.064
a = 4.633 (5) ÅDx = 1.162 Mg m3
b = 8.400 (1) ÅMo Kα radiation, λ = 0.71068 Å
c = 6.577 (3) ŵ = 0.09 mm1
β = 100.37 (6)°T = 100 K
Data collection top
2081 measured reflectionsθmax = 35.0°, θmin = 4.0°
1109 independent reflectionsh = 96
899 reflections with I 2u(I)k = 016
Rint = 0.0000l = 613
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.023All H-atom parameters refined
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.47(Δ/σ)max = 0.0003
1109 reflectionsΔρmax = 0.15 e Å3
64 parametersΔρmin = 0.19 e Å3
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. DOI 10.1039/D0SC05526C - 2020 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fregment can be embedded in an electrostatic crystal field by employing cluster charges. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-07_11-39-49

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
O10.11630 (6)0.83105 (3)0.12462 (5)
C20.14860 (9)0.93867 (5)0.29601 (7)
H2a0.2819 (18)0.8902 (8)0.4368 (10)
H2b0.1742 (15)1.0620 (6)0.2565 (11)
C30.13422 (10)0.86456 (6)0.21816 (7)
H3a0.3097 (17)0.9333 (8)0.1197 (11)
H3b0.2033 (18)0.7645 (10)0.3035 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.03541 (16)0.02562 (12)0.02939 (14)0.00304 (12)0.01061 (12)0.00355 (11)
C20.0324 (2)0.02500 (17)0.02736 (18)0.00038 (14)0.00568 (15)0.00209 (14)
H2a0.082 (6)0.072 (6)0.031 (4)0.023 (5)0.015 (4)0.009 (5)
H2b0.064 (5)0.026 (4)0.070 (5)0.008 (3)0.018 (4)0.003 (3)
C30.0307 (2)0.0338 (2)0.0343 (2)0.00346 (16)0.01197 (17)0.00002 (16)
H3a0.049 (5)0.104 (7)0.051 (5)0.028 (5)0.002 (4)0.013 (5)
H3b0.071 (6)0.063 (5)0.076 (5)0.034 (5)0.027 (5)0.004 (5)
Geometric parameters (Å, º) top
O1—C21.4316 (5)C2—C31.4578 (6)
O1—C31.4359 (5)C3—H3a1.106 (7)
C2—H2a1.095 (6)C3—H3b1.090 (7)
C2—H2b1.080 (5)
C3—O1—C261.11 (3)C2—C3—O159.30 (3)
H2a—C2—O1113.2 (4)H3a—C3—O1114.6 (4)
H2b—C2—O1114.6 (4)H3a—C3—C2120.1 (4)
H2b—C2—H2a119.4 (6)H3b—C3—O1113.8 (4)
C3—C2—O159.59 (3)H3b—C3—C2118.5 (5)
C3—C2—H2a118.2 (4)H3b—C3—H3a116.8 (7)
C3—C2—H2b117.1 (4)
(epoxide_spher) top
Crystal data top
C2H4OV = 251.8 (3) Å3
Mr = 44.05Z = 4
Monoclinic, P21/nF(000) = 96.064
a = 4.633 (5) ÅDx = 1.162 Mg m3
b = 8.400 (1) ÅMo Kα radiation, λ = 0.71068 Å
c = 6.577 (3) ŵ = 0.09 mm1
β = 100.37 (6)°T = 100 K
Data collection top
2081 measured reflectionsθmax = 35.0°, θmin = 4.0°
1109 independent reflectionsh = 96
899 reflections with I 2u(I)k = 016
Rint = 0.0000l = 613
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.032All H-atom parameters refined
wR(F2) = 0.068 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 2.14(Δ/σ)max = 0.0004
1109 reflectionsΔρmax = 0.22 e Å3
64 parametersΔρmin = 0.24 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.11682 (10)0.83081 (5)0.12407 (7)0.03037 (12)
C20.14838 (14)0.93866 (7)0.29621 (10)0.02901 (13)
H2a0.269 (2)0.8926 (10)0.4231 (13)0.044 (2)
H2b0.1726 (18)1.0511 (10)0.2663 (13)0.035 (2)
C30.13434 (15)0.86489 (8)0.21842 (11)0.03283 (14)
H3a0.293 (2)0.9233 (11)0.1330 (16)0.053 (3)
H3b0.194 (2)0.7758 (12)0.2944 (17)0.053 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0352 (2)0.02728 (18)0.0306 (2)0.00259 (17)0.01112 (17)0.00520 (16)
C20.0340 (3)0.0256 (2)0.0276 (3)0.0007 (2)0.0060 (2)0.0027 (2)
H2a0.056 (6)0.049 (6)0.019 (4)0.006 (6)0.016 (4)0.008 (5)
H2b0.041 (6)0.034 (6)0.031 (5)0.012 (4)0.007 (4)0.003 (4)
C30.0314 (3)0.0346 (3)0.0351 (3)0.0028 (2)0.0129 (3)0.0002 (2)
H3a0.038 (6)0.080 (8)0.043 (6)0.000 (7)0.010 (5)0.003 (6)
H3b0.060 (7)0.040 (6)0.063 (7)0.018 (6)0.025 (6)0.009 (6)
Geometric parameters (Å, º) top
O1—C21.4367 (9)C2—C31.4561 (16)
O1—C31.4425 (14)C3—H3a0.975 (11)
C2—H2a0.995 (8)C3—H3b0.968 (10)
C2—H2b0.975 (8)
C3—O1—C260.76 (4)C2—C3—O159.42 (4)
H2a—C2—O1112.2 (5)H3a—C3—O1115.9 (5)
H2b—C2—O1116.8 (5)H3a—C3—C2121.8 (6)
H2b—C2—H2a118.6 (7)H3b—C3—O1113.4 (6)
C3—C2—O159.82 (4)H3b—C3—C2118.1 (7)
C3—C2—H2a117.5 (6)H3b—C3—H3a115.4 (9)
C3—C2—H2b118.0 (5)
(L-Ala_23K_tonto_IAM_app) top
Crystal data top
C3H7NO2Z = 4
Mr = 89.10F(000) = 192.122
Orthorhombic, P212121Dx = 1.405 Mg m3
a = 5.9279 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.2597 (17) ŵ = 0.12 mm1
c = 5.7939 (9) ÅT = 23 K
V = 421.07 (11) Å3
Data collection top
2519 measured reflectionsθmax = 50.1°, θmin = 3.3°
2519 independent reflectionsh = 012
2393 reflections with I 2u(I)k = 026
Rint = 0.0000l = 012
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.019All H-atom parameters refined
wR(F2) = 0.032 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max = 0.0001
2519 reflectionsΔρmax = 0.18 e Å3
118 parametersΔρmin = 0.21 e Å3
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. DOI 10.1039/D0SC05526C - 2020 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fregment can be embedded in an electrostatic crystal field by employing cluster charges. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-02_13-25-25

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.64729 (4)0.13751 (2)0.18294 (5)0.00530 (3)
H1a0.7045 (11)0.0606 (5)0.1982 (14)0.0235 (19)
H1b0.7785 (10)0.1895 (5)0.2114 (14)0.0210 (17)
H1c0.5838 (12)0.1492 (5)0.0164 (13)0.0280 (19)
C10.46630 (4)0.16109 (2)0.35442 (5)0.00448 (4)
H10.4226 (9)0.2473 (4)0.3432 (11)0.0177 (15)
C20.25987 (5)0.09069 (2)0.30332 (6)0.00694 (4)
H2a0.1921 (10)0.1104 (5)0.1315 (12)0.0278 (19)
H2b0.1278 (10)0.1056 (5)0.4315 (13)0.0247 (18)
H2c0.3041 (10)0.0045 (5)0.3082 (14)0.032 (2)
C30.55403 (5)0.14080 (2)0.59985 (5)0.00423 (3)
O10.72675 (4)0.083782 (17)0.62427 (4)0.00655 (3)
O20.44091 (4)0.184042 (17)0.76112 (4)0.00636 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.00555 (7)0.00610 (7)0.00424 (8)0.00012 (6)0.00068 (6)0.00016 (6)
H1a0.025 (4)0.027 (4)0.018 (5)0.005 (3)0.013 (4)0.003 (3)
H1b0.013 (3)0.028 (4)0.022 (5)0.003 (3)0.007 (4)0.000 (4)
H1c0.037 (4)0.022 (4)0.026 (5)0.009 (4)0.027 (4)0.012 (4)
C10.00519 (8)0.00473 (7)0.00352 (9)0.00044 (6)0.00044 (7)0.00009 (6)
H10.023 (3)0.012 (3)0.018 (4)0.008 (3)0.004 (3)0.001 (3)
C20.00582 (9)0.00886 (9)0.00614 (10)0.00132 (8)0.00059 (8)0.00047 (8)
H2a0.020 (4)0.048 (5)0.016 (4)0.010 (3)0.011 (3)0.011 (4)
H2b0.011 (3)0.031 (4)0.033 (5)0.003 (3)0.008 (4)0.004 (4)
H2c0.032 (5)0.016 (3)0.048 (6)0.004 (3)0.001 (4)0.005 (3)
C30.00487 (7)0.00426 (7)0.00355 (9)0.00023 (7)0.00019 (7)0.00003 (6)
O10.00668 (7)0.00705 (7)0.00592 (8)0.00245 (6)0.00064 (6)0.00052 (6)
O20.00755 (7)0.00762 (6)0.00392 (8)0.00210 (6)0.00060 (6)0.00056 (6)
Geometric parameters (Å, º) top
N1—H1a1.006 (6)C1—C31.5344 (5)
N1—H1b1.019 (6)C2—H2a1.100 (7)
N1—H1c1.045 (8)C2—H2b1.094 (7)
N1—C11.4905 (4)C2—H2c1.089 (6)
C1—H11.090 (5)C3—O11.2478 (4)
C1—C21.5264 (4)C3—O21.2664 (4)
H1b—N1—H1a108.4 (5)C3—C1—C2111.09 (2)
H1c—N1—H1a109.3 (6)H2a—C2—C1110.1 (3)
H1c—N1—H1b109.8 (5)H2b—C2—C1110.3 (3)
C1—N1—H1a111.5 (4)H2b—C2—H2a108.4 (4)
C1—N1—H1b108.7 (4)H2c—C2—C1110.5 (3)
C1—N1—H1c109.2 (4)H2c—C2—H2a108.9 (5)
H1—C1—N1108.6 (3)H2c—C2—H2b108.5 (5)
C2—C1—N1109.76 (2)O1—C3—C1118.30 (2)
C2—C1—H1110.2 (3)O2—C3—C1115.88 (2)
C3—C1—N1110.02 (2)O2—C3—O1125.83 (3)
C3—C1—H1107.0 (3)
N1—C1—C3—O118.19 (2)N1—C1—C3—O2162.16 (2)
(L-Ala_23K_tonto_IAM_hyb) top
Crystal data top
C3H7NO2Z = 4
Mr = 89.10F(000) = 192.122
Orthorhombic, P212121Dx = 1.405 Mg m3
a = 5.9279 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.2597 (17) ŵ = 0.12 mm1
c = 5.7939 (9) ÅT = 23 K
V = 421.07 (11) Å3
Data collection top
2519 measured reflectionsθmax = 50.1°, θmin = 3.3°
2519 independent reflectionsh = 012
2393 reflections with I 2u(I)k = 026
Rint = 0.0000l = 012
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.019All H-atom parameters refined
wR(F2) = 0.032 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max = 0.0001
2519 reflectionsΔρmax = 0.18 e Å3
118 parametersΔρmin = 0.21 e Å3
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. DOI 10.1039/D0SC05526C - 2020 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fregment can be embedded in an electrostatic crystal field by employing cluster charges. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-02_13-25-25

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
N10.64729 (5)0.13751 (2)0.18294 (5)
H1a0.7049 (11)0.0606 (5)0.1977 (14)
H1b0.7785 (10)0.1895 (5)0.2112 (14)
H1c0.5832 (12)0.1493 (6)0.0159 (11)
C10.46630 (5)0.16110 (2)0.35442 (5)
H10.4227 (10)0.2474 (4)0.3435 (12)
C20.25987 (5)0.09069 (3)0.30332 (6)
H2a0.1922 (10)0.1105 (5)0.1313 (11)
H2b0.1277 (10)0.1054 (5)0.4317 (12)
H2c0.3041 (10)0.0044 (4)0.3083 (15)
C30.55403 (5)0.14080 (2)0.59985 (5)
O10.72675 (4)0.083782 (17)0.62427 (5)
O20.44091 (4)0.184043 (17)0.76112 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.00555 (8)0.00610 (8)0.00425 (9)0.00016 (7)0.00068 (7)0.00012 (7)
H1a0.026 (5)0.027 (4)0.018 (5)0.003 (4)0.013 (4)0.005 (4)
H1b0.013 (4)0.028 (4)0.022 (5)0.000 (4)0.007 (4)0.003 (4)
H1c0.036 (5)0.021 (4)0.026 (5)0.012 (4)0.027 (4)0.009 (4)
C10.00519 (9)0.00473 (8)0.00352 (10)0.00009 (7)0.00044 (7)0.00044 (7)
H10.023 (4)0.012 (3)0.018 (4)0.001 (3)0.004 (4)0.008 (3)
C20.00582 (9)0.00886 (9)0.00614 (10)0.00047 (8)0.00059 (8)0.00132 (8)
H2a0.019 (4)0.047 (5)0.016 (5)0.010 (4)0.011 (4)0.010 (4)
H2b0.011 (4)0.031 (4)0.033 (5)0.004 (4)0.008 (5)0.003 (4)
H2c0.031 (5)0.016 (3)0.048 (6)0.005 (4)0.001 (5)0.004 (4)
C30.00487 (8)0.00426 (7)0.00355 (9)0.00003 (7)0.00019 (7)0.00023 (7)
O10.00668 (7)0.00706 (7)0.00592 (9)0.00052 (7)0.00064 (7)0.00245 (6)
O20.00755 (7)0.00762 (7)0.00392 (8)0.00056 (6)0.00060 (7)0.00210 (6)
Geometric parameters (Å, º) top
N1—H1a1.007 (6)C1—C31.5344 (5)
N1—H1b1.019 (6)C2—H2a1.101 (6)
N1—H1c1.050 (6)C2—H2b1.095 (6)
N1—C11.4906 (4)C2—H2c1.090 (5)
C1—H11.091 (4)C3—O11.2478 (3)
C1—C21.5264 (4)C3—O21.2664 (3)
H1b—N1—H1a108.3 (5)C3—C1—C2111.09 (2)
H1c—N1—H1a109.3 (6)H2a—C2—C1110.1 (3)
H1c—N1—H1b109.8 (6)H2b—C2—C1110.4 (3)
C1—N1—H1a111.7 (4)H2b—C2—H2a108.5 (5)
C1—N1—H1b108.8 (4)H2c—C2—C1110.5 (3)
C1—N1—H1c109.1 (4)H2c—C2—H2a109.0 (5)
H1—C1—N1108.7 (3)H2c—C2—H2b108.3 (5)
C2—C1—N1109.76 (2)O1—C3—C1118.30 (2)
C2—C1—H1110.3 (3)O2—C3—C1115.87 (2)
C3—C1—N1110.02 (2)O2—C3—O1125.83 (3)
C3—C1—H1106.9 (3)
N1—C1—C3—O118.19 (2)N1—C1—C3—O2162.16 (2)
(L-Ala_23K_tonto_IAM_num) top
Crystal data top
C3H7NO2Z = 4
Mr = 89.10F(000) = 192.122
Orthorhombic, P212121Dx = 1.405 Mg m3
a = 5.9279 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.2597 (17) ŵ = 0.12 mm1
c = 5.7939 (9) ÅT = 23 K
V = 421.07 (11) Å3
Data collection top
2519 measured reflectionsθmax = 50.1°, θmin = 3.3°
2519 independent reflectionsh = 012
2393 reflections with I 2u(I)k = 026
Rint = 0.0000l = 012
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.019All H-atom parameters refined
wR(F2) = 0.032 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max = 0.0001
2519 reflectionsΔρmax = 0.18 e Å3
118 parametersΔρmin = 0.21 e Å3
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. DOI 10.1039/D0SC05526C - 2020 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fregment can be embedded in an electrostatic crystal field by employing cluster charges. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-02_13-25-25

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
N10.64729 (4)0.13751 (2)0.18294 (5)
H1a0.7049 (11)0.0606 (5)0.1977 (14)
H1b0.7785 (10)0.1895 (5)0.2112 (13)
H1c0.5832 (11)0.1493 (5)0.01595 (11)
C10.46630 (4)0.16109 (2)0.35442 (5)
H10.4227 (9)0.2474 (4)0.3435 (11)
C20.25987 (5)0.09069 (2)0.30332 (6)
H2a0.1922 (10)0.1105 (5)0.1313 (11)
H2b0.1277 (10)0.1054 (5)0.4317 (12)
H2c0.3041 (10)0.0044 (4)0.3083 (14)
C30.55403 (5)0.14080 (2)0.59985 (5)
O10.72675 (4)0.083783 (17)0.62427 (4)
O20.44091 (4)0.184043 (17)0.76112 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.00555 (7)0.00610 (7)0.00425 (9)0.00012 (6)0.00068 (6)0.00016 (6)
H1a0.025 (4)0.027 (4)0.018 (5)0.005 (3)0.013 (4)0.003 (4)
H1b0.013 (3)0.028 (4)0.022 (5)0.003 (3)0.007 (4)0.000 (4)
H1c0.036 (4)0.021 (4)0.026 (5)0.009 (4)0.027 (4)0.012 (4)
C10.00519 (8)0.00473 (7)0.00352 (9)0.00044 (6)0.00044 (7)0.00009 (6)
H10.023 (3)0.012 (3)0.018 (4)0.008 (3)0.004 (3)0.001 (3)
C20.00582 (9)0.00886 (9)0.00614 (10)0.00132 (8)0.00059 (8)0.00047 (8)
H2a0.019 (4)0.047 (5)0.016 (4)0.010 (3)0.011 (3)0.010 (4)
H2b0.011 (3)0.031 (4)0.033 (5)0.003 (3)0.008 (4)0.004 (4)
H2c0.031 (5)0.016 (3)0.048 (6)0.004 (3)0.001 (4)0.005 (3)
C30.00487 (7)0.00426 (7)0.00355 (9)0.00023 (7)0.00019 (7)0.00003 (6)
O10.00668 (7)0.00706 (7)0.00592 (8)0.00245 (6)0.00064 (6)0.00052 (6)
O20.00755 (7)0.00762 (6)0.00392 (8)0.00210 (6)0.00060 (6)0.00056 (6)
Geometric parameters (Å, º) top
N1—H1a1.007 (6)C1—C31.5344 (4)
N1—H1b1.019 (6)C2—H2a1.101 (6)
N1—H1c1.050 (6)C2—H2b1.095 (6)
N1—C11.4906 (4)C2—H2c1.090 (5)
C1—H11.091 (4)C3—O11.2478 (3)
C1—C21.5264 (4)C3—O21.2664 (3)
H1b—N1—H1a108.3 (5)C3—C1—C2111.09 (2)
H1c—N1—H1a109.3 (6)H2a—C2—C1110.1 (3)
H1c—N1—H1b109.8 (6)H2b—C2—C1110.4 (3)
C1—N1—H1a111.7 (4)H2b—C2—H2a108.5 (5)
C1—N1—H1b108.8 (4)H2c—C2—C1110.5 (3)
C1—N1—H1c109.1 (4)H2c—C2—H2a109.0 (5)
H1—C1—N1108.7 (3)H2c—C2—H2b108.3 (5)
C2—C1—N1109.76 (2)O1—C3—C1118.29 (2)
C2—C1—H1110.3 (3)O2—C3—C1115.88 (2)
C3—C1—N1110.02 (2)O2—C3—O1125.83 (3)
C3—C1—H1106.9 (3)
N1—C1—C3—O118.19 (2)N1—C1—C3—O2162.16 (2)
(L-Ala_23K_tonto_IAM_spher) top
Crystal data top
C3H7NO2Z = 4
Mr = 89.10F(000) = 192.122
Orthorhombic, P212121Dx = 1.405 Mg m3
a = 5.9279 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.2597 (17) ŵ = 0.12 mm1
c = 5.7939 (9) ÅT = 23 K
V = 421.07 (11) Å3
Data collection top
2519 measured reflectionsθmax = 50.1°, θmin = 3.3°
2519 independent reflectionsh = 012
2393 reflections with I 2u(I)k = 026
Rint = 0.0000l = 012
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.027All H-atom parameters refined
wR(F2) = 0.061 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 2.15(Δ/σ)max = 0.0003
2519 reflectionsΔρmax = 0.46 e Å3
118 parametersΔρmin = 0.28 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.64715 (8)0.13748 (4)0.18297 (9)0.00562 (6)
H1a0.6958 (17)0.0659 (11)0.186 (2)0.025 (3)
H1b0.7692 (17)0.1850 (9)0.202 (2)0.021 (3)
H1c0.571 (2)0.1479 (8)0.014 (3)0.056 (6)
C10.46618 (8)0.16103 (4)0.35484 (9)0.00493 (7)
H10.4249 (15)0.2401 (7)0.3429 (18)0.007 (2)
C20.25985 (9)0.09071 (5)0.30330 (11)0.00738 (8)
H2a0.2027 (17)0.1081 (8)0.146 (2)0.020 (3)
H2b0.1448 (16)0.1075 (8)0.419 (2)0.015 (3)
H2c0.2996 (17)0.0111 (8)0.310 (2)0.018 (3)
C30.55406 (9)0.14076 (4)0.59995 (9)0.00462 (6)
O10.72708 (7)0.08373 (3)0.62429 (8)0.00683 (6)
O20.44093 (7)0.18410 (3)0.76120 (8)0.00666 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.00577 (14)0.00662 (14)0.00447 (16)0.00018 (12)0.00064 (12)0.00018 (12)
H1a0.006 (6)0.068 (9)0.002 (7)0.009 (6)0.007 (5)0.016 (7)
H1b0.009 (5)0.039 (7)0.015 (8)0.027 (6)0.012 (6)0.010 (6)
H1c0.067 (9)0.000 (5)0.102 (15)0.036 (6)0.079 (11)0.028 (7)
C10.00551 (15)0.00538 (14)0.00390 (17)0.00045 (12)0.00002 (13)0.00009 (12)
H10.004 (5)0.015 (5)0.002 (6)0.010 (4)0.011 (5)0.004 (4)
C20.00614 (16)0.00939 (16)0.00661 (19)0.00130 (15)0.00065 (15)0.00042 (15)
H2a0.008 (6)0.024 (7)0.027 (9)0.007 (5)0.004 (6)0.001 (6)
H2b0.002 (5)0.016 (6)0.028 (9)0.005 (5)0.003 (6)0.004 (6)
H2c0.022 (7)0.018 (6)0.014 (7)0.011 (5)0.002 (6)0.002 (5)
C30.00548 (14)0.00431 (13)0.00408 (17)0.00032 (13)0.00040 (13)0.00007 (12)
O10.00674 (13)0.00691 (12)0.00685 (16)0.00218 (11)0.00058 (12)0.00067 (12)
O20.00796 (13)0.00783 (12)0.00417 (14)0.00172 (11)0.00100 (12)0.00070 (11)
Geometric parameters (Å, º) top
N1—H1a0.923 (13)C1—C31.5329 (8)
N1—H1b0.936 (12)C2—H2a0.993 (13)
N1—H1c1.085 (17)C2—H2b0.978 (11)
N1—C11.4919 (7)C2—H2c1.005 (10)
C1—H11.002 (9)C3—O11.2493 (7)
C1—C21.5260 (8)C3—O21.2668 (7)
H1b—N1—H1a110.3 (8)C3—C1—C2111.23 (4)
H1c—N1—H1a105.1 (9)H2a—C2—C1109.3 (6)
H1c—N1—H1b111.1 (9)H2b—C2—C1107.8 (6)
C1—N1—H1a113.2 (7)H2b—C2—H2a110.1 (8)
C1—N1—H1b110.8 (7)H2c—C2—C1110.7 (6)
C1—N1—H1c106.1 (6)H2c—C2—H2a108.8 (9)
H1—C1—N1108.5 (5)H2c—C2—H2b110.1 (8)
C2—C1—N1109.66 (4)O1—C3—C1118.31 (5)
C2—C1—H1109.7 (5)O2—C3—C1115.81 (4)
C3—C1—N1110.04 (4)O2—C3—O1125.88 (5)
C3—C1—H1107.7 (6)
N1—C1—C3—O118.18 (5)N1—C1—C3—O2162.11 (4)
(nh30r_app) top
Crystal data top
H3NF(000) = 40.004
Mr = 17.03Dx = 0.838 Mg m3
Cubic, P213Mo Kα radiation, λ = 0.71069 Å
a = 5.1305 (8) ŵ = 0.06 mm1
V = 135.05 (4) Å3T = 160 K
Z = 4
Data collection top
1762 measured reflectionsθmax = 30.0°, θmin = 5.6°
136 independent reflectionsh = 77
133 reflections with I 2u(I)k = 57
Rint = 0.030l = 77
Refinement top
Refinement on F20 constraints
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.009 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.020(Δ/σ)max = 0.0003
S = 2.24Δρmax = 0.04 e Å3
136 reflectionsΔρmin = 0.02 e Å3
13 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
0 restraintsAbsolute structure parameter: 5 (2)
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fragment can be embedded in an electrostatic crystal field by employing cluster charges or modelled using implicit solvation models, depending on the software used. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-02_22-18-50

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N0.21056 (4)0.21056 (4)0.21056 (4)0.03619 (17)
H0.3639 (10)0.2677 (12)0.1168 (8)0.0678 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N0.03619 (17)0.03619 (17)0.03619 (17)0.00128 (7)0.00128 (7)0.00128 (7)
H0.070 (3)0.068 (3)0.065 (3)0.009 (2)0.008 (2)0.008 (2)
Geometric parameters (Å, º) top
N—H0.967 (5)N—Hii0.967 (5)
N—Hi0.967 (5)
Hii—N—H108.0 (3)Hi—N—H108.0 (3)
Hi—N—Hii108.0 (3)
Symmetry codes: (i) z, x, y; (ii) y, z, x.
(nh30r_hyb) top
Crystal data top
H3NF(000) = 40.004
Mr = 17.03Dx = 0.838 Mg m3
Cubic, P213Mo Kα radiation, λ = 0.71069 Å
a = 5.1305 (8) ŵ = 0.06 mm1
V = 135.05 (4) Å3T = 160 K
Z = 4
Data collection top
1762 measured reflectionsθmax = 30.0°, θmin = 5.6°
136 independent reflectionsh = 77
133 reflections with I 2u(I)k = 57
Rint = 0.030l = 77
Refinement top
Refinement on F20 constraints
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.009 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.020(Δ/σ)max = 0.0003
S = 2.24Δρmax = 0.04 e Å3
136 reflectionsΔρmin = 0.02 e Å3
13 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
0 restraintsAbsolute structure parameter: 5 (2)
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fragment can be embedded in an electrostatic crystal field by employing cluster charges or modelled using implicit solvation models, depending on the software used. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-02_22-18-50

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
N0.21065 (5)0.21065 (5)0.21065 (5)
H0.3656 (9)0.2688 (10)0.1157 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N0.03654 (19)0.03654 (19)0.03654 (19)0.00141 (8)0.00141 (8)0.00141 (8)
H0.066 (3)0.071 (3)0.068 (3)0.008 (3)0.010 (3)0.012 (3)
Geometric parameters (Å, º) top
N—H0.979 (5)N—Hii0.979 (5)
N—Hi0.979 (5)
Hii—N—H108.0 (3)Hi—N—H108.0 (3)
Hi—N—Hii108.0 (3)
Symmetry codes: (i) z, x, y; (ii) y, z, x.
(nh30r_num) top
Crystal data top
H3NF(000) = 40.004
Mr = 17.03Dx = 0.838 Mg m3
Cubic, P213Mo Kα radiation, λ = 0.71069 Å
a = 5.1305 (8) ŵ = 0.06 mm1
V = 135.05 (4) Å3T = 160 K
Z = 4
Data collection top
1762 measured reflectionsθmax = 30.0°, θmin = 5.6°
136 independent reflectionsh = 77
133 reflections with I 2u(I)k = 57
Rint = 0.030l = 77
Refinement top
Refinement on F20 constraints
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.009 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.019(Δ/σ)max = 0.0003
S = 2.24Δρmax = 0.04 e Å3
136 reflectionsΔρmin = 0.02 e Å3
13 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
0 restraintsAbsolute structure parameter: 5 (2)
Special details top

Refinement. Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fragment can be embedded in an electrostatic crystal field by employing cluster charges or modelled using implicit solvation models, depending on the software used. The following options were used: SOFTWARE: ORCA PARTITIONING: NoSpherA2 INT ACCURACY: High METHOD: PBE BASIS SET: def2-TZVPP CHARGE: 0 MULTIPLICITY: 1 DATE: 2021-06-02_22-18-50

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
N0.21064 (5)0.21064 (5)0.21064 (5)
H0.3655 (9)0.2689 (10)0.1158 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N0.03654 (18)0.03654 (18)0.03654 (18)0.00141 (8)0.00141 (8)0.00141 (8)
H0.066 (3)0.071 (3)0.066 (2)0.012 (3)0.010 (2)0.008 (2)
Geometric parameters (Å, º) top
N—H0.969 (5)N—Hii0.969 (5)
N—Hi0.969 (5)
Hii—N—H107.7 (3)Hi—N—H107.7 (3)
Hi—N—Hii107.7 (3)
Symmetry codes: (i) z, x, y; (ii) y, z, x.
(nh30r_spher) top
Crystal data top
H3NF(000) = 40.004
Mr = 17.03Dx = 0.838 Mg m3
Cubic, P213Mo Kα radiation, λ = 0.71069 Å
a = 5.1305 (8) ŵ = 0.06 mm1
V = 135.05 (4) Å3T = 160 K
Z = 4
Data collection top
1762 measured reflectionsθmax = 30.0°, θmin = 5.6°
136 independent reflectionsh = 77
133 reflections with I 2u(I)k = 57
Rint = 0.030l = 77
Refinement top
Refinement on F20 constraints
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.013 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.032(Δ/σ)max = 0.001
S = 3.65Δρmax = 0.04 e Å3
136 reflectionsΔρmin = 0.03 e Å3
13 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
0 restraintsAbsolute structure parameter: 5 (2)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N0.21005 (9)0.21005 (9)0.21005 (9)0.0354 (3)
H0.3383 (17)0.2467 (18)0.1341 (12)0.0568 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N0.0354 (3)0.0354 (3)0.0354 (3)0.00004 (13)0.00004 (13)0.00004 (13)
H0.076 (4)0.051 (4)0.044 (4)0.030 (4)0.006 (4)0.001 (3)
Geometric parameters (Å, º) top
N—H0.787 (9)N—Hii0.787 (9)
N—Hi0.787 (9)
Hii—N—H109.4 (5)Hi—N—H109.4 (5)
Hi—N—Hii109.4 (5)
Symmetry codes: (i) z, x, y; (ii) y, z, x.
 

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