A glass capillary cell for in situ powder X-ray diffraction of condensed volatile compounds. Solid HCFC-123a and HCFC-124

A rotating glass capillary cell with a gas handling system has been built to allow in situ studies by powder X-ray diffraction. The cell can be used to condense volatile compounds, or to follow solid-state chemical reactions under vacuum or at gas pressures up to around 7 × 10⁵ Pa. Using the cell, cooled by a stream of helium gas, the solid phases of 1,2-dichlorotrifluoroethane (HCFC-123a) and 2-chloro-1,1,1,2-tetrafluoroethane (HCFC-124) have been investigated using powder synchrotron X-ray radiation. These were found to have disordered hexagonal structures, with a = 4.018 (5), c = 6.553 (1) Å and a = 4.048 (1), c = 6.625 (1) Å, respectively, at 64 K.

Computing details

(I)

Crystal data

C2HCl2F3	Z = ?
Mr = 152.93	Melting point: 78 K
Hexagonal, P63/mmc	Synchrotron radiation, λ = 0.401340 Å
a = 4.000 Å	T = 60 K
c = 6.523 Å	× × mm
V = 90.37 Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

S = 2.90

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Biso*/Beq
C	−0.14036	0.39482	0.04282	3.00*
C	0.29145	0.69269	0.04592	3.00*
Cl	−0.34393	0.41134	−0.19441	3.00*
Cl	0.49659	0.68285	0.28375	3.00*
F	−0.31455	0.47429	0.19040	3.00*
F	−0.19820	0.04516	0.07190	3.00*
F	0.46472	0.60928	−0.10377	3.00*
H	0.33420	0.97862	0.02355	6.00*