Single crystals of C -1H and D -1H were obtained
from cooling crystallization experiments from water,C Cl-I° by crystallization from acetonitrile, C Cl-2H from an EtOH/water (1:1) mixture,
andD Cl-2H by solvent evaporation from
2-propanol. Essential crystal data are collected in Table2 and Table S14 of the Supporting
Information . The data for C -1H and D Cl-2H (Cu radiation; λ = 1.5418 Å) and D -1H and C Cl-I° (Mo radiation;
λ = 0.7107 Å) were collected on an Oxford Diffraction Gemini-R
Ultra diffractometer operated by CrysAlis software.48 Data forC Cl-2H were recorded
on a Rigaku AFC12 goniometer driven by the CrystalClear-SM Expert
3.1 b27 software (Rigaku, 2012) and equipped with an enhanced sensitivity
(HG) Saturn724+ detector mounted at the window of
an FR-E+ Super Bright Mo rotating anode generator with HFVarimax optics.49 The structures were solved by direct methods
(SIR201150 or SHELXL201351 ) and refined by full-matrix least-squares on F2 using SHELXL2013 and the program package WinGX.52 The treatment of the H atoms is reported in
section 4.2 of theSupporting Information .
from cooling crystallization experiments from water,
and
2-propanol. Essential crystal data are collected in Table
Information
λ = 0.7107 Å) were collected on an Oxford Diffraction Gemini-R
Ultra diffractometer operated by CrysAlis software.48 Data for
on a Rigaku AFC12 goniometer driven by the CrystalClear-SM Expert
3.1 b27 software (Rigaku, 2012) and equipped with an enhanced sensitivity
(HG) Saturn724+ detector mounted at the window of
an FR-E+ Super Bright Mo rotating anode generator with HFVarimax optics.49 The structures were solved by direct methods
(SIR201150 or SHELXL201351 ) and refined by full-matrix least-squares on F2 using SHELXL2013 and the program package WinGX.52 The treatment of the H atoms is reported in
section 4.2 of the