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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889808024643/hx5073sup1.cif
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0021889808024643/hx5073sup2.pdf
Supplementary material

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(I) top
Crystal data top
?β = 100.568 (2)°
Mr = ?γ = 98.884°
?, ?V = 440.26 (10) Å3
a = 6.217 (1) ÅZ = ?
b = 6.985 (1) Å? radiation, λ = ? Å
c = 10.506 (1) Å × × mm
α = 94.686°
Data collection top
h = ??l = ??
k = ??
Refinement top
Refinement on F2348 parameters
Least-squares matrix: full0 restraints
R[F2 > 2σ(F2)] = 0.026 w2 = 1/[s2(Fo2)]
wR(F2) = 0.033(Δ/σ)max < 0.001
S = 1.29Δρmax = 0.41 e Å3
8807 reflectionsΔρmin = 0.51 e Å3
Crystal data top
?β = 100.568 (2)°
Mr = ?γ = 98.884°
?, ?V = 440.26 (10) Å3
a = 6.217 (1) ÅZ = ?
b = 6.985 (1) Å? radiation, λ = ? Å
c = 10.506 (1) Å × × mm
α = 94.686°
Data collection top
Refinement top
R[F2 > 2σ(F2)] = 0.026348 parameters
wR(F2) = 0.0330 restraints
S = 1.29Δρmax = 0.41 e Å3
8807 reflectionsΔρmin = 0.51 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/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)0.370510.0609570.2439250.014
H(3)0.6433040.4435080.2474730.016
H(5)0.1378890.3574910.229230.015
H(9A)0.2147910.1797270.3893570.017
H(9B)0.2528280.0330910.4249140.017
H(10A)0.1423820.2023570.0646080.018
H(10B)0.0944660.2902440.0811780.019
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
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)0.0168560.0154650.0108330.0013050.0028780.002567
H(3)0.0179160.0146550.0129890.0004090.0022670.001235
H(5)0.0218780.013460.0093570.0022140.0023410.002375
H(9A)0.027690.0112470.0144670.0054240.0033930.005786
H(9B)0.025260.0160440.0118320.0059150.0056090.001987
H(10A)0.0218660.0201960.014260.0008560.0102760.005935
H(10B)0.0124740.0216650.0189890.0022790.0022420.000645
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)ii1.5521 (6)
O(5)—H(5)1.0582 (3)C(2)—C(2)iii1.5425 (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)i1.3754 (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)iii121.18 (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)i114.80 (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)i176.05 (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)ii120.25 (4)O(9)—H(9B)—H(9A)37.152 (19)
O(3)—C(1)—C(1)ii113.33 (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)iii112.39 (3)
Symmetry codes: (i) x+1, y, z+1; (ii) x+1, y+1, z; (iii) x1, 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
V3)440.26 (10)
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 0.026, 0.033, 1.29
No. of reflections8807
No. of parameters348
Δρmax, Δρmin (e Å3)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)ii1.5521 (6)
O(5)—H(5)1.0582 (3)C(2)—C(2)iii1.5425 (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)i1.3754 (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)iii121.18 (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)i114.80 (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)i176.05 (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)ii120.25 (4)O(9)—H(9B)—H(9A)37.152 (19)
O(3)—C(1)—C(1)ii113.33 (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)iii112.39 (3)
Symmetry codes: (i) x+1, y, z+1; (ii) x+1, y+1, z; (iii) x1, y, z.
 

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