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A 165 mm Mar CCD detector has been fitted on a large Huber four-circle diffractometer together with a helium cryostat at beamline D3 at Hasylab, DESY in Hamburg. This setup allows fast collection of accurate, short-wavelength, very low temperature X-ray diffraction data for charge-density analysis. As a test example, diffraction data have been collected in 10 h on a hydrogen-bonded network system with 15 unique atoms, and the electron density was modelled with the multipole formalism in an X-N procedure using matching-temperature neutron diffraction data collected at Institut Laue Langevin, Grenoble in France.
Keywords: experimental electron density distribution; He cooling; synchrotron radiation; X-N refinement; atomic displacement parameters.
Supporting information
 | Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889808024643/hx5073sup1.cif |
 | Portable Document Format (PDF) file https://doi.org/10.1107/S0021889808024643/hx5073sup2.pdf |
Computing details top
Program(s) used to refine structure: Volkov et al., (2006); molecular graphics: Volkov et al., (2006); software used to prepare material for publication: Volkov et al., (2006).
![[Figure 1]](http://journals.iucr.org/j/issues/2008/05/00/hx5073/hx5073fig1thm.gif)
![[Figure 2]](http://journals.iucr.org/j/issues/2008/05/00/hx5073/hx5073fig2thm.gif)
![[Figure 3]](http://journals.iucr.org/j/issues/2008/05/00/hx5073/hx5073fig3thm.gif)
![[Figure 4]](http://journals.iucr.org/j/issues/2008/05/00/hx5073/hx5073fig4thm.gif)
![[Figure 5]](http://journals.iucr.org/j/issues/2008/05/00/hx5073/hx5073fig5thm.gif)
![[Figure 6]](http://journals.iucr.org/j/issues/2008/05/00/hx5073/hx5073fig6thm.gif)
![[Figure 7]](http://journals.iucr.org/j/issues/2008/05/00/hx5073/hx5073fig7thm.gif)
(I) top
Crystal data top
| ? | β = 100.568 (2)° |
| Mr = ? | γ = 98.884° |
| ?, ? | V = 440.26 (10) Å3 |
| a = 6.217 (1) Å | Z = ? |
| b = 6.985 (1) Å | ? radiation, λ = ? Å |
| c = 10.506 (1) Å | × × mm |
| α = 94.686° |
Refinement top
| Refinement on F2 | 348 parameters |
| Least-squares matrix: full | 0 restraints |
| R[F2 > 2σ(F2)] = 0.026 | w2 = 1/[s2(Fo2)] |
| wR(F2) = 0.033 | (Δ/σ)max < 0.001 |
| S = 1.29 | Δρmax = 0.41 e Å−3 |
| 8807 reflections | Δρmin = −0.51 e Å−3 |
Crystal data top
| ? | β = 100.568 (2)° |
| Mr = ? | γ = 98.884° |
| ?, ? | V = 440.26 (10) Å3 |
| a = 6.217 (1) Å | Z = ? |
| b = 6.985 (1) Å | ? radiation, λ = ? Å |
| c = 10.506 (1) Å | × × mm |
| α = 94.686° |
Refinement top
| R[F2 > 2σ(F2)] = 0.026 | 348 parameters |
| wR(F2) = 0.033 | 0 restraints |
| S = 1.29 | Δρmax = 0.41 e Å−3 |
| 8807 reflections | Δρmin = −0.51 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
| x | y | z | Uiso*/Ueq | ||
| K(1) | 0.166902 (10) | 0.146531 (9) | 0.272299 (6) | 0.005 | |
| O(1) | 0.32768 (6) | 0.32887 (5) | 0.06605 (3) | 0.005 | |
| O(2) | −0.49600 (6) | −0.07104 (5) | 0.15539 (3) | 0.005 | |
| O(3) | 0.65294 (6) | 0.51936 (5) | 0.15900 (3) | 0.005 | |
| O(4) | −0.23141 (6) | 0.11365 (5) | 0.07737 (3) | 0.005 | |
| O(5) | 0.18091 (6) | −0.44219 (5) | 0.30600 (3) | 0.006 | |
| O(6) | 0.28126 (6) | −0.15314 (5) | 0.42892 (3) | 0.006 | |
| O(7) | 0.35630 (6) | −0.34409 (5) | 0.64478 (3) | 0.006 | |
| O(8) | 0.21781 (6) | −0.62730 (5) | 0.51715 (3) | 0.006 | |
| O(9) | −0.21285 (6) | −0.05175 (5) | 0.35666 (3) | 0.006 | |
| O(10) | 0.05496 (6) | −0.23947 (5) | 0.12958 (3) | 0.006 | |
| C(1) | 0.48896 (5) | 0.45360 (5) | 0.06365 (3) | 0.004 | |
| C(2) | −0.41627 (5) | 0.01568 (5) | 0.06547 (3) | 0.004 | |
| C(3) | 0.24662 (5) | −0.33147 (5) | 0.41668 (3) | 0.004 | |
| C(4) | 0.27615 (5) | −0.44739 (5) | 0.53688 (3) | 0.004 | |
| H(2) | −0.37051 | −0.060957 | 0.243925 | 0.014 | |
| H(3) | 0.643304 | 0.443508 | 0.247473 | 0.016 | |
| H(5) | 0.137889 | −0.357491 | 0.22923 | 0.015 | |
| H(9A) | −0.214791 | −0.179727 | 0.389357 | 0.017 | |
| H(9B) | −0.252828 | 0.033091 | 0.424914 | 0.017 | |
| H(10A) | 0.142382 | −0.202357 | 0.064608 | 0.018 | |
| H(10B) | −0.094466 | −0.290244 | 0.081178 | 0.019 |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| K(1) | 0.00580 (6) | 0.00486 (6) | 0.00548 (6) | −0.00018 (4) | 0.00117 (4) | 0.00075 (4) |
| O(1) | 0.00492 (10) | 0.00590 (10) | 0.00412 (10) | −0.00124 (9) | 0.00006 (8) | 0.00131 (8) |
| O(2) | 0.00534 (10) | 0.00783 (11) | 0.00281 (10) | 0.00008 (9) | −0.00020 (8) | 0.00221 (8) |
| O(3) | 0.00589 (11) | 0.00639 (10) | 0.00255 (9) | −0.00078 (9) | −0.00129 (8) | 0.00151 (8) |
| O(4) | 0.00407 (10) | 0.00692 (10) | 0.00415 (10) | −0.00080 (9) | −0.00043 (8) | 0.00110 (8) |
| O(5) | 0.01056 (12) | 0.00447 (10) | 0.00202 (9) | 0.00162 (9) | −0.00066 (8) | 0.00014 (8) |
| O(6) | 0.00916 (11) | 0.00319 (9) | 0.00390 (10) | 0.00083 (9) | 0.00042 (8) | 0.00057 (8) |
| O(7) | 0.00869 (11) | 0.00503 (10) | 0.00201 (9) | 0.00022 (9) | −0.00072 (8) | 0.00039 (8) |
| O(8) | 0.01088 (12) | 0.00320 (10) | 0.00404 (10) | 0.00093 (9) | 0.00033 (9) | 0.00082 (8) |
| O(9) | 0.00744 (11) | 0.00578 (10) | 0.00342 (10) | 0.00201 (9) | 0.00017 (8) | 0.00092 (8) |
| O(10) | 0.00519 (10) | 0.00768 (11) | 0.00403 (10) | 0.00022 (9) | −0.00021 (8) | 0.00195 (8) |
| C(1) | 0.00434 (10) | 0.00406 (9) | 0.00242 (9) | 0.00007 (9) | −0.00017 (8) | 0.00071 (7) |
| C(2) | 0.00385 (10) | 0.00468 (9) | 0.00258 (9) | 0.00031 (9) | −0.00020 (7) | 0.00070 (8) |
| C(3) | 0.00560 (10) | 0.00338 (10) | 0.00237 (9) | 0.00080 (8) | 0.00018 (8) | 0.00060 (8) |
| C(4) | 0.00558 (10) | 0.00341 (10) | 0.00235 (9) | 0.00098 (8) | 0.00012 (8) | 0.00067 (8) |
| H(2) | 0.016856 | 0.015465 | 0.010833 | 0.001305 | 0.002878 | 0.002567 |
| H(3) | 0.017916 | 0.014655 | 0.012989 | 0.000409 | 0.002267 | 0.001235 |
| H(5) | 0.021878 | 0.01346 | 0.009357 | 0.002214 | 0.002341 | 0.002375 |
| H(9A) | 0.02769 | 0.011247 | 0.014467 | 0.005424 | 0.003393 | 0.005786 |
| H(9B) | 0.02526 | 0.016044 | 0.011832 | 0.005915 | 0.005609 | −0.001987 |
| H(10A) | 0.021866 | 0.020196 | 0.01426 | 0.000856 | 0.010276 | 0.005935 |
| H(10B) | 0.012474 | 0.021665 | 0.018989 | −0.002279 | −0.002242 | 0.000645 |
Geometric parameters (Å, º) top
| O(1)—C(1) | 1.2281 (4) | O(9)—H(2) | 1.3820 (3) |
| O(2)—C(2) | 1.2952 (4) | O(9)—H(9A) | 0.9827 (3) |
| O(2)—H(2) | 1.0885 (3) | O(9)—H(9B) | 0.9842 (3) |
| O(3)—C(1) | 1.2882 (4) | O(10)—H(5) | 1.4546 (3) |
| O(3)—H(3) | 1.1133 (3) | O(10)—H(10A) | 0.9747 (3) |
| O(4)—C(2) | 1.2228 (4) | O(10)—H(10B) | 0.9710 (3) |
| O(5)—C(3) | 1.3033 (4) | C(1)—C(1)ii | 1.5521 (6) |
| O(5)—H(5) | 1.0582 (3) | C(2)—C(2)iii | 1.5425 (6) |
| O(6)—C(3) | 1.2229 (4) | C(3)—C(4) | 1.5530 (4) |
| O(7)—C(4) | 1.2657 (4) | H(9A)—H(9B) | 1.5670 |
| O(7)—H(3)i | 1.3754 (3) | H(10A)—H(10B) | 1.5517 |
| O(8)—C(4) | 1.2421 (4) | ||
| C(2)—O(2)—H(2) | 111.54 (3) | O(4)—C(2)—C(2)iii | 121.18 (4) |
| C(1)—O(3)—H(3) | 112.99 (3) | O(5)—C(3)—O(6) | 125.02 (3) |
| C(3)—O(5)—H(5) | 110.49 (3) | O(5)—C(3)—C(4) | 113.58 (3) |
| C(4)—O(7)—H(3)i | 114.80 (3) | O(6)—C(3)—C(4) | 121.40 (3) |
| H(2)—O(9)—H(9A) | 111.54 (3) | O(7)—C(4)—O(8) | 127.74 (3) |
| H(2)—O(9)—H(9B) | 108.01 (3) | O(7)—C(4)—C(3) | 114.90 (3) |
| H(9A)—O(9)—H(9B) | 105.63 (3) | O(8)—C(4)—C(3) | 117.36 (3) |
| H(5)—O(10)—H(10A) | 119.94 (3) | O(2)—H(2)—O(9) | 178.91 (2) |
| H(5)—O(10)—H(10B) | 114.53 (3) | O(3)—H(3)—O(7)i | 176.05 (2) |
| H(10A)—O(10)—H(10B) | 105.78 (3) | O(5)—H(5)—O(10) | 173.22 (2) |
| O(1)—C(1)—O(3) | 126.41 (3) | O(9)—H(9A)—H(9B) | 37.22 (2) |
| O(1)—C(1)—C(1)ii | 120.25 (4) | O(9)—H(9B)—H(9A) | 37.152 (19) |
| O(3)—C(1)—C(1)ii | 113.33 (3) | O(10)—H(10A)—H(10B) | 37.03 (2) |
| O(2)—C(2)—O(4) | 126.43 (3) | O(10)—H(10B)—H(10A) | 37.19 (2) |
| O(2)—C(2)—C(2)iii | 112.39 (3) |
| Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z; (iii) −x−1, −y, −z. |
Experimental details
| Crystal data | |
| Chemical formula | ? |
| Mr | ? |
| Crystal system, space group | ?, ? |
| Temperature (K) | ? |
| a, b, c (Å) | 6.217 (1), 6.985 (1), 10.506 (1) |
| α, β, γ (°) | 94.686, 100.568 (2), 98.884 |
| V (Å3) | 440.26 (10) |
| 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 | 0.026, 0.033, 1.29 |
| No. of reflections | 8807 |
| No. of parameters | 348 |
| Δρmax, Δρmin (e Å−3) | 0.41, −0.51 |
Computer programs: Volkov et al., (2006).
Selected geometric parameters (Å, º) top
| O(1)—C(1) | 1.2281 (4) | O(9)—H(2) | 1.3820 (3) |
| O(2)—C(2) | 1.2952 (4) | O(9)—H(9A) | 0.9827 (3) |
| O(2)—H(2) | 1.0885 (3) | O(9)—H(9B) | 0.9842 (3) |
| O(3)—C(1) | 1.2882 (4) | O(10)—H(5) | 1.4546 (3) |
| O(3)—H(3) | 1.1133 (3) | O(10)—H(10A) | 0.9747 (3) |
| O(4)—C(2) | 1.2228 (4) | O(10)—H(10B) | 0.9710 (3) |
| O(5)—C(3) | 1.3033 (4) | C(1)—C(1)ii | 1.5521 (6) |
| O(5)—H(5) | 1.0582 (3) | C(2)—C(2)iii | 1.5425 (6) |
| O(6)—C(3) | 1.2229 (4) | C(3)—C(4) | 1.5530 (4) |
| O(7)—C(4) | 1.2657 (4) | H(9A)—H(9B) | 1.5670 |
| O(7)—H(3)i | 1.3754 (3) | H(10A)—H(10B) | 1.5517 |
| O(8)—C(4) | 1.2421 (4) | ||
| C(2)—O(2)—H(2) | 111.54 (3) | O(4)—C(2)—C(2)iii | 121.18 (4) |
| C(1)—O(3)—H(3) | 112.99 (3) | O(5)—C(3)—O(6) | 125.02 (3) |
| C(3)—O(5)—H(5) | 110.49 (3) | O(5)—C(3)—C(4) | 113.58 (3) |
| C(4)—O(7)—H(3)i | 114.80 (3) | O(6)—C(3)—C(4) | 121.40 (3) |
| H(2)—O(9)—H(9A) | 111.54 (3) | O(7)—C(4)—O(8) | 127.74 (3) |
| H(2)—O(9)—H(9B) | 108.01 (3) | O(7)—C(4)—C(3) | 114.90 (3) |
| H(9A)—O(9)—H(9B) | 105.63 (3) | O(8)—C(4)—C(3) | 117.36 (3) |
| H(5)—O(10)—H(10A) | 119.94 (3) | O(2)—H(2)—O(9) | 178.91 (2) |
| H(5)—O(10)—H(10B) | 114.53 (3) | O(3)—H(3)—O(7)i | 176.05 (2) |
| H(10A)—O(10)—H(10B) | 105.78 (3) | O(5)—H(5)—O(10) | 173.22 (2) |
| O(1)—C(1)—O(3) | 126.41 (3) | O(9)—H(9A)—H(9B) | 37.22 (2) |
| O(1)—C(1)—C(1)ii | 120.25 (4) | O(9)—H(9B)—H(9A) | 37.152 (19) |
| O(3)—C(1)—C(1)ii | 113.33 (3) | O(10)—H(10A)—H(10B) | 37.03 (2) |
| O(2)—C(2)—O(4) | 126.43 (3) | O(10)—H(10B)—H(10A) | 37.19 (2) |
| O(2)—C(2)—C(2)iii | 112.39 (3) |
| Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z; (iii) −x−1, −y, −z. |
