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The average structure of the composite urea/octanedioic acid has been refined using the superspace formalism [superspace group H′3121(00γ)00\bar{1}]. 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101002166/na0117sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101002166/na0117Isup2.hkl
Contains datablock I

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(I) top
Crystal data top
C6O6N12H24+0.893(C8O4H14)Z = 18
Mr = 515.4Dx = 1.34 Mg m3
Dm = 1.33 (2) Mg m3
Dm measured by ?
Trigonal, ?Mo Kα radiation, λ = 0.71073 Å
q = 0.89300c*θ = 3.3–52.1°
a = 14.185 (6) ŵ = 0.10 mm1
c = 10.978 (1) ÅT = 293 K
V = 1913 (1) Å3 × × mm
Data collection top
Unknown
diffractometer
θmax = 26.2°, θmin = 2.9°
20973 measured reflectionsh = 1717
2146 independent reflectionsk = 1717
1017 reflections with 3l = 1313
Rint = 0.587
Refinement top
Refinement on F62 parameters
R[F2 > 2σ(F2)] = 0.059Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000004F2)
wR(F2) = 0.060(Δ/σ)max = 0.176
S = 8.84Δρmax = 0.53 e Å3
2146 reflectionsΔρmin = 1.10 e Å3
Crystal data top
C6O6N12H24+0.893(C8O4H14)V = 1913 (1) Å3
Mr = 515.4Z = 18
Trigonal, ?Mo Kα radiation
q = 0.89300c*µ = 0.10 mm1
a = 14.185 (6) ÅT = 293 K
c = 10.978 (1) Å × × mm
Data collection top
Unknown
diffractometer
1017 reflections with 3
20973 measured reflectionsRint = 0.587
2146 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05962 parameters
wR(F2) = 0.060(Δ/σ)max = 0.176
S = 8.84Δρmax = 0.53 e Å3
2146 reflectionsΔρmin = 1.10 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O(a)0.3237 (1)000.0342 (8)
O(b)0.3132 (1)0.3132 (1)0.1666670.0352 (9)
C(a)0.4121 (2)000.037 (1)
C(b)0.4025 (2)0.4025 (2)0.1666670.032 (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)0.1216070.056 (4)0.083333
C(3b)0.002 (2)0.019 (2)0.014180.056 (4)0.083333
C(2b)0.075 (2)0.003 (2)0.0809530.056 (4)0.083333
C(1b)0.022 (2)0.020 (2)0.1910480.056 (4)0.083333
O(11b)0.076 (2)0.057 (2)0.2050530.056 (4)0.083333
O(21b)0.092 (2)0.002 (2)0.2716610.056 (4)0.083333
H(14b)0.116 (2)0.108 (2)0.1160840.056 (4)0.083333
H(24b)0.109 (2)0.019 (2)0.1344310.056 (4)0.083333
H(13b)0.062 (2)0.107 (2)0.018320.056 (4)0.083333
H(23b)0.049 (2)0.022 (2)0.0002150.056 (4)0.083333
H(12b)0.140 (2)0.089 (2)0.0824010.056 (4)0.083333
H(22b)0.117 (2)0.044 (2)0.0745650.056 (4)0.083333
H(11b)0.054 (2)0.012 (2)0.3444980.056 (4)0.083333
C(5b)0.015 (2)0.003 (2)0.219310.056 (4)0.083333
C(6b)0.046 (2)0.036 (2)0.3267370.056 (4)0.083333
C(7b)0.031 (2)0.014 (2)0.421870.056 (4)0.083333
C(8b)0.022 (2)0.037 (2)0.5319640.056 (4)0.083333
O(18b)0.120 (2)0.073 (2)0.545970.056 (4)0.083333
O(28b)0.047 (2)0.015 (2)0.6125780.056 (4)0.083333
H(15b)0.072 (2)0.091 (2)0.2248330.056 (4)0.083333
H(25b)0.065 (2)0.036 (2)0.2064860.056 (4)0.083333
H(16b)0.106 (2)0.124 (2)0.3225970.056 (4)0.083333
H(26b)0.093 (2)0.005 (2)0.3411320.056 (4)0.083333
H(17b)0.095 (2)0.072 (2)0.4233180.056 (4)0.083333
H(27b)0.073 (2)0.061 (2)0.4154820.056 (4)0.083333
H(18b)0.010 (2)0.028 (2)0.6854150.056 (4)0.083333
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
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 formulaC6O6N12H24+0.893(C8O4H14)
Mr515.4
Crystal system, space groupTrigonal, ?
Temperature (K)293
Wave vectorsq = 0.89300c*
a, c (Å)14.185 (6), 10.978 (1)
V3)1913 (1)
Z18
Radiation typeMo Kα
µ (mm1)0.10
Crystal size (mm) × ×
Data collection
DiffractometerUnknown
diffractometer
Absorption correction
No. of measured, independent and
observed (3) reflections
20973, 2146, 1017
Rint0.587
(sin θ/λ)max1)0.621
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.059, 0.060, 8.84
No. of reflections2146
No. of parameters62
No. of restraints?
(Δ/σ)max0.176
Δρmax, Δρmin (e Å3)0.53, 1.10

Computer programs: STOE IPDS, JANA2000 (Petricek et al., 2000), JANA2000 (Petricel et al., 2000).

 

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