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Ab-initio crystal structure analysis of organic materials from electron diffraction data is presented. The data were collected using the automated electron diffraction tomography (ADT) technique. The structure solution and refinement route is first validated on the basis of the known crystal structure of tri-p-benzamide. The same procedure is then applied to solve the previously unknown crystal structure of tetra-p-benzamide. In the crystal structure of tetra-p-benzamide, an unusual hydrogen-bonding scheme is realised; the hydrogen-bonding scheme is, however, in perfect agreement with solid-state NMR data.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112003138/so5056sup1.cif
Contains datablock I

CCDC reference: 879424

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
(I) top
Crystal data top
?β = 101.0000°
Mr = ?V = ? Å3
Monoclinic, C2/CZ = ?
a = 51.0843 Å? radiation, λ = ? Å
b = 5.1938 Å × × mm
c = 17.4771 Å
Data collection top
h = ??l = ??
k = ??
Refinement top
Crystal data top
?β = 101.0000°
Mr = ?V = ? Å3
Monoclinic, C2/CZ = ?
a = 51.0843 Å? radiation, λ = ? Å
b = 5.1938 Å × × mm
c = 17.4771 Å
Data collection top
Refinement top
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.084900.588200.781800.00000*
C20.093000.769200.732000.00000*
C30.118200.755700.714300.00000*
C40.135600.554300.744200.00000*
C50.127600.370000.793400.00000*
C60.102500.390500.812900.00000*
C70.199900.386600.680700.00000*
C80.207300.199600.631600.00000*
C90.230900.222500.604800.00000*
C100.248000.432200.627800.00000*
C110.240600.622300.676200.00000*
C120.216600.599600.701800.00000*
C130.311800.597400.560200.00000*
C140.319600.783800.511400.00000*
C150.343500.760300.486300.00000*
C160.360500.550600.510800.00000*
C170.352700.360900.558600.00000*
C180.328400.384500.582600.00000*
C190.426600.407500.455700.00000*
C200.436800.246500.404300.00000*
C210.460700.305900.382000.00000*
C220.474100.529200.412200.00000*
C230.464900.688100.465200.00000*
C240.441000.625700.487100.00000*
C250.057400.615300.796200.00000*
C260.174800.339200.709300.00000*
C270.286600.646400.587900.00000*
C280.400200.341300.475200.00000*
N290.161000.552800.724200.00000*
N300.272600.433900.603100.00000*
N310.385600.550600.489500.00000*
N320.498900.598900.387700.00000*
O330.038800.701400.746900.00000*
O340.054800.541800.868100.00000*
O350.166800.115600.716800.00000*
O360.278700.870600.594900.00000*
O370.392300.115500.475800.00000*
O380.508300.819000.407400.00000*
O390.509500.442100.351100.00000*
H400.078800.929100.705730.00000*
H410.124960.908100.675330.00000*
H420.141580.205340.817060.00000*
H430.096300.244160.854690.00000*
H440.193810.026600.613400.00000*
H450.236630.070930.563780.00000*
H460.254240.794270.694340.00000*
H470.210240.755230.740480.00000*
H480.306180.956480.492120.00000*
H490.349550.911030.445560.00000*
H500.366240.188770.577540.00000*
H510.321730.229720.620980.00000*
H520.425440.065600.380590.00000*
H530.468930.174090.340090.00000*
H540.476930.864630.489530.00000*
H550.433040.752320.530790.00000*
H560.171590.736980.719370.00000*
H570.282570.249520.594090.00000*
H580.393500.747760.484590.00000*
H590.034730.552750.892740.00000*
Bond lengths (Å) top
C1—C21.396C16—C171.398
C1—C61.404C16—N311.402
C1—C251.480C17—C181.389
C2—C31.382C17—H501.140
C2—H401.140C18—H511.140
C3—C41.407C19—C201.399
C3—H411.140C19—C241.404
C4—C51.399C19—C281.493
C4—N291.407C20—C211.385
C5—C61.392C20—H521.140
C5—H421.140C21—C221.398
C6—H431.140C21—H531.140
C7—C81.395C22—C231.388
C7—C121.403C22—N321.458
C7—C261.483C23—C241.386
C8—C91.379C23—H541.140
C8—H441.140C24—H551.140
C9—C101.406C25—O331.238
C9—H451.140C25—O341.344
C10—C111.398C26—N291.366
C10—N301.405C26—O351.246
C11—C121.388C27—N301.368
C11—H461.140C27—O361.246
C12—H471.140C28—N311.368
C13—C141.398C28—O371.241
C13—C181.403N29—H561.110
C13—C271.481N30—H571.110
C14—C151.379N31—H581.110
C14—H481.140N32—O381.262
C15—C161.408N32—O391.224
C15—H491.140O34—H591.187

Experimental details

Crystal data
Chemical formula?
Mr?
Crystal system, space groupMonoclinic, C2/C
Temperature (K)?
a, b, c (Å)51.0843, 5.1938, 17.4771
β (°) 101.0000
V3)?
Z?
Radiation type?, λ = ? Å
µ (mm1)?
Crystal size (mm) × ×
Data collection
Diffractometer?
Absorption correction?
No. of measured, independent and
observed (?) reflections
?, ?, ?
Rint?
Refinement
R[F2 > 2σ(F2)], wR(F2), S ?, ?, ?
No. of reflections?
No. of parameters?
No. of restraints?
Δρmax, Δρmin (e Å3)?, ?

 

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