Helium cryostat synchrotron charge densities determined using a large CCD detector - the upgraded beamline D3 at DESY

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.

Computing details

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

(I)

Crystal data

?	β = 100.568 (2)°
Mr = ?	γ = 98.884°
?, ?	V = 440.26 (10) Å^3
a = 6.217 (1) Å	Z = ?
b = 6.985 (1) Å	? radiation, λ = ? Å
c = 10.506 (1) Å	× × mm
α = 94.686°

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

Refinement on F^2	348 parameters
Least-squares matrix: full	0 restraints
R[F^2 > 2σ(F^2)] = 0.026	w2 = 1/[s^2(Fo^2)]
wR(F^2) = 0.033	(Δ/σ)max < 0.001
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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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.