research papers
The average structure of the composite urea/octanedioic acid has been refined using the superspace formalism [superspace group H′3121(00γ)00]. Modulation effects seem to be almost negligible. The guest substructure appears to be largely disordered and has been modelled using rigid units occupying 12 equiprobable different orientations inside the urea tunnels. Guest molecules are slightly tilted with respect to the tunnel axis favouring a stronger guest–guest intratunnel interaction.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101002166/na0117sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768101002166/na0117Isup2.hkl |
Computing details top
Data collection: STOE IPDS; cell refinement: STOE IPDS; data reduction: STOE IPDS; program(s) used to solve structure: JANA2000 (Petricek et al., 2000); program(s) used to refine structure: JANA2000 (Petricel et al., 2000); software used to prepare material for publication: JANA2000 (Petricek et al., 2000).
(I) top
Crystal data top
C6O6N12H24+0.893(C8O4H14) | Z = 18 |
Mr = 515.4 | Dx = 1.34 Mg m−3 Dm = 1.33 (2) Mg m−3 Dm measured by ? |
Trigonal, ? | Mo Kα radiation, λ = 0.71073 Å |
q = 0.89300c* | θ = 3.3–52.1° |
a = 14.185 (6) Å | µ = 0.10 mm−1 |
c = 10.978 (1) Å | T = 293 K |
V = 1913 (1) Å3 | × × mm |
Data collection top
Unknown diffractometer | θmax = 26.2°, θmin = 2.9° |
20973 measured reflections | h = −17→17 |
2146 independent reflections | k = −17→17 |
1017 reflections with 3 | l = −13→13 |
Rint = 0.587 |
Refinement top
Refinement on F | 62 parameters |
R[F2 > 2σ(F2)] = 0.059 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000004F2) |
wR(F2) = 0.060 | (Δ/σ)max = 0.176 |
S = 8.84 | Δρmax = 0.53 e Å−3 |
2146 reflections | Δρmin = −1.10 e Å−3 |
Crystal data top
C6O6N12H24+0.893(C8O4H14) | V = 1913 (1) Å3 |
Mr = 515.4 | Z = 18 |
Trigonal, ? | Mo Kα radiation |
q = 0.89300c* | µ = 0.10 mm−1 |
a = 14.185 (6) Å | T = 293 K |
c = 10.978 (1) Å | × × mm |
Data collection top
Unknown diffractometer | 1017 reflections with 3 |
20973 measured reflections | Rint = 0.587 |
2146 independent reflections |
Refinement top
R[F2 > 2σ(F2)] = 0.059 | 62 parameters |
wR(F2) = 0.060 | (Δ/σ)max = 0.176 |
S = 8.84 | Δρmax = 0.53 e Å−3 |
2146 reflections | Δρmin = −1.10 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
O(a) | 0.3237 (1) | 0 | 0 | 0.0342 (8) | |
O(b) | 0.3132 (1) | 0.3132 (1) | 0.166667 | 0.0352 (9) | |
C(a) | 0.4121 (2) | 0 | 0 | 0.037 (1) | |
C(b) | 0.4025 (2) | 0.4025 (2) | 0.166667 | 0.032 (1) | |
N(a) | 0.4510 (2) | −0.0166 (2) | 0.0989 (2) | 0.046 (1) | |
N(b) | 0.4608 (1) | 0.4449 (2) | 0.2740 (1) | 0.0436 (8) | |
H(1a) | 0.4229 (9) | −0.0384 (9) | 0.1831 (5) | 0.040 (2) | |
H(1b) | 0.4231 (9) | 0.3922 (7) | 0.3408 (8) | 0.040 (2) | |
H(2a) | 0.5283 (5) | −0.003 (1) | 0.099 (1) | 0.040 (2) | |
H(2b) | 0.5390 (4) | 0.5032 (6) | 0.275 (1) | 0.040 (2) | |
C(4a) | 0.050 (1) | 0.0171 (7) | −0.18 (1) | 0.056 (4) | 0.083333 |
C(3a) | 0.002 (1) | −0.0410 (7) | −0.28 (1) | 0.056 (4) | 0.083333 |
C(2a) | 0.078 (1) | 0.0166 (7) | −0.38 (1) | 0.056 (4) | 0.083333 |
C(1a) | 0.030 (1) | −0.0277 (7) | −0.49 (1) | 0.056 (4) | 0.083333 |
O(11a) | −0.062 (1) | −0.1052 (7) | −0.50 (1) | 0.056 (4) | 0.083333 |
O(21a) | 0.098 (1) | 0.0256 (7) | −0.57 (1) | 0.056 (4) | 0.083333 |
H(14a) | 0.065 (1) | 0.1007 (7) | −0.18 (1) | 0.056 (4) | 0.083333 |
H(24a) | 0.130 (1) | 0.0231 (7) | −0.16 (1) | 0.056 (4) | 0.083333 |
H(13a) | −0.016 (1) | −0.1261 (7) | −0.28 (1) | 0.056 (4) | 0.083333 |
H(23a) | −0.076 (1) | −0.0441 (7) | −0.30 (1) | 0.056 (4) | 0.083333 |
H(12a) | 0.103 (1) | 0.1033 (7) | −0.38 (1) | 0.056 (4) | 0.083333 |
H(22a) | 0.154 (1) | 0.0137 (7) | −0.37 (1) | 0.056 (4) | 0.083333 |
H(11a) | 0.063 (1) | −0.0041 (7) | −0.64 (1) | 0.056 (4) | 0.083333 |
C(5a) | −0.023 (1) | −0.0390 (7) | −0.08 (1) | 0.056 (4) | 0.083333 |
C(6a) | 0.026 (1) | 0.0191 (7) | 0.03 (1) | 0.056 (4) | 0.083333 |
C(7a) | −0.050 (1) | −0.0384 (7) | 0.12 (1) | 0.056 (4) | 0.083333 |
C(8a) | −0.002 (1) | 0.0058 (7) | 0.23 (1) | 0.056 (4) | 0.083333 |
O(18a) | 0.090 (1) | 0.0833 (7) | 0.25 (1) | 0.056 (4) | 0.083333 |
O(28a) | −0.070 (1) | −0.0475 (7) | 0.31 (1) | 0.056 (4) | 0.083333 |
H(15a) | −0.037 (1) | −0.1226 (7) | −0.07 (1) | 0.056 (4) | 0.083333 |
H(25a) | −0.102 (1) | −0.0450 (7) | −0.09 (1) | 0.056 (4) | 0.083333 |
H(16a) | 0.044 (1) | 0.1042 (7) | 0.02 (1) | 0.056 (4) | 0.083333 |
H(26a) | 0.104 (1) | 0.0222 (7) | 0.04 (1) | 0.056 (4) | 0.083333 |
H(17a) | −0.075 (1) | −0.1252 (7) | 0.12 (1) | 0.056 (4) | 0.083333 |
H(27a) | −0.126 (1) | −0.0356 (7) | 0.12 (1) | 0.056 (4) | 0.083333 |
H(18a) | −0.035 (1) | −0.0178 (7) | 0.39 (1) | 0.056 (4) | 0.083333 |
C(4b) | 0.059 (2) | 0.020 (2) | 0.121607 | 0.056 (4) | 0.083333 |
C(3b) | −0.002 (2) | −0.019 (2) | 0.01418 | 0.056 (4) | 0.083333 |
C(2b) | 0.075 (2) | 0.003 (2) | −0.080953 | 0.056 (4) | 0.083333 |
C(1b) | 0.022 (2) | −0.020 (2) | −0.191048 | 0.056 (4) | 0.083333 |
O(11b) | −0.076 (2) | −0.057 (2) | −0.205053 | 0.056 (4) | 0.083333 |
O(21b) | 0.092 (2) | 0.002 (2) | −0.271661 | 0.056 (4) | 0.083333 |
H(14b) | 0.116 (2) | 0.108 (2) | 0.116084 | 0.056 (4) | 0.083333 |
H(24b) | 0.109 (2) | −0.019 (2) | 0.134431 | 0.056 (4) | 0.083333 |
H(13b) | −0.062 (2) | −0.107 (2) | 0.01832 | 0.056 (4) | 0.083333 |
H(23b) | −0.049 (2) | 0.022 (2) | −0.000215 | 0.056 (4) | 0.083333 |
H(12b) | 0.140 (2) | 0.089 (2) | −0.082401 | 0.056 (4) | 0.083333 |
H(22b) | 0.117 (2) | −0.044 (2) | −0.074565 | 0.056 (4) | 0.083333 |
H(11b) | 0.054 (2) | −0.012 (2) | −0.344498 | 0.056 (4) | 0.083333 |
C(5b) | −0.015 (2) | −0.003 (2) | 0.21931 | 0.056 (4) | 0.083333 |
C(6b) | 0.046 (2) | 0.036 (2) | 0.326737 | 0.056 (4) | 0.083333 |
C(7b) | −0.031 (2) | 0.014 (2) | 0.42187 | 0.056 (4) | 0.083333 |
C(8b) | 0.022 (2) | 0.037 (2) | 0.531964 | 0.056 (4) | 0.083333 |
O(18b) | 0.120 (2) | 0.073 (2) | 0.54597 | 0.056 (4) | 0.083333 |
O(28b) | −0.047 (2) | 0.015 (2) | 0.612578 | 0.056 (4) | 0.083333 |
H(15b) | −0.072 (2) | −0.091 (2) | 0.224833 | 0.056 (4) | 0.083333 |
H(25b) | −0.065 (2) | 0.036 (2) | 0.206486 | 0.056 (4) | 0.083333 |
H(16b) | 0.106 (2) | 0.124 (2) | 0.322597 | 0.056 (4) | 0.083333 |
H(26b) | 0.093 (2) | −0.005 (2) | 0.341132 | 0.056 (4) | 0.083333 |
H(17b) | −0.095 (2) | −0.072 (2) | 0.423318 | 0.056 (4) | 0.083333 |
H(27b) | −0.073 (2) | 0.061 (2) | 0.415482 | 0.056 (4) | 0.083333 |
H(18b) | −0.010 (2) | 0.028 (2) | 0.685415 | 0.056 (4) | 0.083333 |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
O(a) | 0.0282 (7) | 0.068 (1) | 0.020 (1) | 0.0340 (6) | −0.0018 (4) | −0.0036 (9) |
O(b) | 0.046 (1) | 0.046 (1) | 0.021 (1) | 0.028 (1) | 0.0009 (5) | −0.0009 (5) |
C(a) | 0.039 (1) | 0.041 (2) | 0.033 (2) | 0.0206 (8) | 0.0015 (7) | 0.003 (1) |
C(b) | 0.041 (1) | 0.041 (1) | 0.021 (2) | 0.025 (2) | 0.0053 (7) | −0.0053 (7) |
N(a) | 0.060 (1) | 0.064 (1) | 0.0174 (9) | 0.034 (1) | 0.0090 (9) | 0.0110 (8) |
N(b) | 0.0348 (9) | 0.045 (1) | 0.020 (1) | −0.0033 (8) | −0.0035 (8) | −0.0136 (9) |
Experimental details
Crystal data | |
Chemical formula | C6O6N12H24+0.893(C8O4H14) |
Mr | 515.4 |
Crystal system, space group | Trigonal, ? |
Temperature (K) | 293 |
Wave vectors | q = 0.89300c* |
a, c (Å) | 14.185 (6), 10.978 (1) |
V (Å3) | 1913 (1) |
Z | 18 |
Radiation type | Mo Kα |
µ (mm−1) | 0.10 |
Crystal size (mm) | × × |
Data collection | |
Diffractometer | Unknown diffractometer |
Absorption correction | – |
No. of measured, independent and observed (3) reflections | 20973, 2146, 1017 |
Rint | 0.587 |
(sin θ/λ)max (Å−1) | 0.621 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.060, 8.84 |
No. of reflections | 2146 |
No. of parameters | 62 |
No. of restraints | ? |
(Δ/σ)max | 0.176 |
Δρmax, Δρmin (e Å−3) | 0.53, −1.10 |
Computer programs: STOE IPDS, JANA2000 (Petricek et al., 2000), JANA2000 (Petricel et al., 2000).