. 2022 Jul 20;22(8):4696–4707. doi: 10.1021/acs.cgd.1c01093

Table 2. Disorder Occupancy of the Minor Site C16A Observed in Single Crystals and Powdered Samples of Salbutamol Oxalate Crystallized under Different Conditions, as Determined by X-ray Crystallography and ¹³C Solid-State NMR.

			X-ray disorder occupancy at 150 K
	conditions		individual single crystal trials^a
sample	time (days)	temp (°C)	#1	#2	#3	average (%)	distribution (%)^b	NMR occupancy at 300 K (%)^c
1a	<1	50	0.161 (6)	0.121 (5)	0.132 (6)	13.8	(−) 1.7	12 ± 3
							(+) 2.3
1b	≈3	20	0.150 (4)	0.140 (5)	0.129 (5)	13.9	(−) 1.0	9 ± 3
							(+) 1.1
1c	≈3	30	0.153 (5)	0.148 (4)	0.165 (6)	15.5	(−) 0.7	11 ± 2
							(+) 1.0

Standard uncertainties were noted down before site occupancies were fixed.

Distribution from the average value.

Occupancies determined by ¹³C CPMAS solid-state NMR by measuring the relative intensity of the resonance, C16, corresponding to the minor phase at 11.7 T at room temperature (see Figure 4).

Table 2. Disorder Occupancy of the Minor Site C16A Observed in Single Crystals and Powdered Samples of Salbutamol Oxalate Crystallized under Different Conditions, as Determined by X-ray Crystallography and 13C Solid-State NMR.

Table 2. Disorder Occupancy of the Minor Site C16A Observed in Single Crystals and Powdered Samples of Salbutamol Oxalate Crystallized under Different Conditions, as Determined by X-ray Crystallography and ¹³C Solid-State NMR.