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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
CCDC reference: 879424
Crystal data top
? | β = 101.0000° |
Mr = ? | V = ? Å3 |
Monoclinic, C2/C | Z = ? |
a = 51.0843 Å | ? radiation, λ = ? Å |
b = 5.1938 Å | × × mm |
c = 17.4771 Å | |
Crystal data top
? | β = 101.0000° |
Mr = ? | V = ? Å3 |
Monoclinic, C2/C | Z = ? |
a = 51.0843 Å | ? radiation, λ = ? Å |
b = 5.1938 Å | × × mm |
c = 17.4771 Å | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1 | 0.08490 | 0.58820 | 0.78180 | 0.00000* | |
C2 | 0.09300 | 0.76920 | 0.73200 | 0.00000* | |
C3 | 0.11820 | 0.75570 | 0.71430 | 0.00000* | |
C4 | 0.13560 | 0.55430 | 0.74420 | 0.00000* | |
C5 | 0.12760 | 0.37000 | 0.79340 | 0.00000* | |
C6 | 0.10250 | 0.39050 | 0.81290 | 0.00000* | |
C7 | 0.19990 | 0.38660 | 0.68070 | 0.00000* | |
C8 | 0.20730 | 0.19960 | 0.63160 | 0.00000* | |
C9 | 0.23090 | 0.22250 | 0.60480 | 0.00000* | |
C10 | 0.24800 | 0.43220 | 0.62780 | 0.00000* | |
C11 | 0.24060 | 0.62230 | 0.67620 | 0.00000* | |
C12 | 0.21660 | 0.59960 | 0.70180 | 0.00000* | |
C13 | 0.31180 | 0.59740 | 0.56020 | 0.00000* | |
C14 | 0.31960 | 0.78380 | 0.51140 | 0.00000* | |
C15 | 0.34350 | 0.76030 | 0.48630 | 0.00000* | |
C16 | 0.36050 | 0.55060 | 0.51080 | 0.00000* | |
C17 | 0.35270 | 0.36090 | 0.55860 | 0.00000* | |
C18 | 0.32840 | 0.38450 | 0.58260 | 0.00000* | |
C19 | 0.42660 | 0.40750 | 0.45570 | 0.00000* | |
C20 | 0.43680 | 0.24650 | 0.40430 | 0.00000* | |
C21 | 0.46070 | 0.30590 | 0.38200 | 0.00000* | |
C22 | 0.47410 | 0.52920 | 0.41220 | 0.00000* | |
C23 | 0.46490 | 0.68810 | 0.46520 | 0.00000* | |
C24 | 0.44100 | 0.62570 | 0.48710 | 0.00000* | |
C25 | 0.05740 | 0.61530 | 0.79620 | 0.00000* | |
C26 | 0.17480 | 0.33920 | 0.70930 | 0.00000* | |
C27 | 0.28660 | 0.64640 | 0.58790 | 0.00000* | |
C28 | 0.40020 | 0.34130 | 0.47520 | 0.00000* | |
N29 | 0.16100 | 0.55280 | 0.72420 | 0.00000* | |
N30 | 0.27260 | 0.43390 | 0.60310 | 0.00000* | |
N31 | 0.38560 | 0.55060 | 0.48950 | 0.00000* | |
N32 | 0.49890 | 0.59890 | 0.38770 | 0.00000* | |
O33 | 0.03880 | 0.70140 | 0.74690 | 0.00000* | |
O34 | 0.05480 | 0.54180 | 0.86810 | 0.00000* | |
O35 | 0.16680 | 0.11560 | 0.71680 | 0.00000* | |
O36 | 0.27870 | 0.87060 | 0.59490 | 0.00000* | |
O37 | 0.39230 | 0.11550 | 0.47580 | 0.00000* | |
O38 | 0.50830 | 0.81900 | 0.40740 | 0.00000* | |
O39 | 0.50950 | 0.44210 | 0.35110 | 0.00000* | |
H40 | 0.07880 | 0.92910 | 0.70573 | 0.00000* | |
H41 | 0.12496 | 0.90810 | 0.67533 | 0.00000* | |
H42 | 0.14158 | 0.20534 | 0.81706 | 0.00000* | |
H43 | 0.09630 | 0.24416 | 0.85469 | 0.00000* | |
H44 | 0.19381 | 0.02660 | 0.61340 | 0.00000* | |
H45 | 0.23663 | 0.07093 | 0.56378 | 0.00000* | |
H46 | 0.25424 | 0.79427 | 0.69434 | 0.00000* | |
H47 | 0.21024 | 0.75523 | 0.74048 | 0.00000* | |
H48 | 0.30618 | 0.95648 | 0.49212 | 0.00000* | |
H49 | 0.34955 | 0.91103 | 0.44556 | 0.00000* | |
H50 | 0.36624 | 0.18877 | 0.57754 | 0.00000* | |
H51 | 0.32173 | 0.22972 | 0.62098 | 0.00000* | |
H52 | 0.42544 | 0.06560 | 0.38059 | 0.00000* | |
H53 | 0.46893 | 0.17409 | 0.34009 | 0.00000* | |
H54 | 0.47693 | 0.86463 | 0.48953 | 0.00000* | |
H55 | 0.43304 | 0.75232 | 0.53079 | 0.00000* | |
H56 | 0.17159 | 0.73698 | 0.71937 | 0.00000* | |
H57 | 0.28257 | 0.24952 | 0.59409 | 0.00000* | |
H58 | 0.39350 | 0.74776 | 0.48459 | 0.00000* | |
H59 | 0.03473 | 0.55275 | 0.89274 | 0.00000* | |
Bond lengths (Å) top
C1—C2 | 1.396 | C16—C17 | 1.398 |
C1—C6 | 1.404 | C16—N31 | 1.402 |
C1—C25 | 1.480 | C17—C18 | 1.389 |
C2—C3 | 1.382 | C17—H50 | 1.140 |
C2—H40 | 1.140 | C18—H51 | 1.140 |
C3—C4 | 1.407 | C19—C20 | 1.399 |
C3—H41 | 1.140 | C19—C24 | 1.404 |
C4—C5 | 1.399 | C19—C28 | 1.493 |
C4—N29 | 1.407 | C20—C21 | 1.385 |
C5—C6 | 1.392 | C20—H52 | 1.140 |
C5—H42 | 1.140 | C21—C22 | 1.398 |
C6—H43 | 1.140 | C21—H53 | 1.140 |
C7—C8 | 1.395 | C22—C23 | 1.388 |
C7—C12 | 1.403 | C22—N32 | 1.458 |
C7—C26 | 1.483 | C23—C24 | 1.386 |
C8—C9 | 1.379 | C23—H54 | 1.140 |
C8—H44 | 1.140 | C24—H55 | 1.140 |
C9—C10 | 1.406 | C25—O33 | 1.238 |
C9—H45 | 1.140 | C25—O34 | 1.344 |
C10—C11 | 1.398 | C26—N29 | 1.366 |
C10—N30 | 1.405 | C26—O35 | 1.246 |
C11—C12 | 1.388 | C27—N30 | 1.368 |
C11—H46 | 1.140 | C27—O36 | 1.246 |
C12—H47 | 1.140 | C28—N31 | 1.368 |
C13—C14 | 1.398 | C28—O37 | 1.241 |
C13—C18 | 1.403 | N29—H56 | 1.110 |
C13—C27 | 1.481 | N30—H57 | 1.110 |
C14—C15 | 1.379 | N31—H58 | 1.110 |
C14—H48 | 1.140 | N32—O38 | 1.262 |
C15—C16 | 1.408 | N32—O39 | 1.224 |
C15—H49 | 1.140 | O34—H59 | 1.187 |
Experimental details
Crystal data |
Chemical formula | ? |
Mr | ? |
Crystal system, space group | Monoclinic, C2/C |
Temperature (K) | ? |
a, b, c (Å) | 51.0843, 5.1938, 17.4771 |
β (°) | 101.0000 |
V (Å3) | ? |
Z | ? |
Radiation type | ?, λ = ? Å |
µ (mm−1) | ? |
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 Å−3) | ?, ? |
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