. 2019 May 15;24(10):1875. doi: 10.3390/molecules24101875

Table 6.

Experimental details of the crystallographic analysis for lactones 5a, 7a, 13a, 12b and 12c.

	5a	7a	13a	12b	12c
Empirical formula	C $_{16}$ H $_{15}$ O $_{2}$ Cl	C $_{16}$ H $_{15}$ O $_{2}$ Br	C $_{16}$ H $_{16}$ O $_{3}$	C $_{12}$ H $_{14}$ O $_{3}$	C $_{12}$ H $_{13}$ FO $_{3}$
Formula weight	274.73	319.19	256.29	206.24	224.22
Temperature (K)	293.15	293.15	100	100	293.15
Wavelength (Å)	0.71073	0.71073	1.54184	1.54184	0.71073
Crystal system, space group	monoclinic, $P 2_{1 / c}$	monoclinic, $P 2_{1 / c}$	monoclinic, $P 2_{1 / c}$	orthorhombic P b c a ( $P 2_{1} / b 2_{1} / c 2_{1} / a$ )	orthorhombic P b c a
a (Å)	13.670(3)	13.9026(9)	11.4137(2)	10.1332(2)	10.042(3)
b(Å)	8.9220(2)	8.9784(4)	11.46100(10)	7.62820(10)	7.591(2)
c(Å)	11.890(3)	11.8318(9)	10.7848(2)	27.2405(2)	28.174(3)
$β$ ( $^{\circ}$ )	111.73(3)	111.418(8)	117.359(2)	90	90
Volume (Å $^{3}$ )	1347.1(5)	1374.89(17)	1252.982 (4)	2105.64(5)	2147.8(9)
Z, Calculated density (Mg/m $^{3}$ )	4, 1.355	4, 1.542	4, 0.154	8, 0.1831	8, 1.387
Absorption coefficient (mm $^{- 1}$ )	0.278	2.984	0.126	0.150	0.110
F(000)	576	648	544	880	944
Theta range for data collection ( $^{\circ}$ )	2.935 −28.804	2.927 −26.999	3.86 −76.29	3.24 −75.38	3.441 −28.867
Index ranges	−17 ≤ h ≤ 18, −11 ≤ k ≤ 12, −16 ≤ l ≤ 9	−17≤ h≤ 17, −11 ≤ k ≤ 11, −12 ≤ l ≤ 15	−14 ≤ h ≤ 14, −14 ≤ k ≤ 14, −12 ≤ l ≤ 13	−142 ≤ h≤ 10, −9 ≤ k ≤ 9, −32 ≤ l ≤ 33	−13 ≤ h≤ 13, −8≤ k ≤ 10, −36 ≤ l ≤ 37
Reflections Collected unique observed [I > 2sigma(I)]	9623	9471	17416	13106	14345
	3259	2957	2623	2170	2677
	1811	1923	2483	2017	1951
$R_{i n t}$	0.0713	0.0959	0.0281	0.0401	0.0501
Completeness to $Θ$ (%)	25.242 $^{\circ}$ , 99.1	25.242 $^{\circ}$ , 99.2	76.29 $^{\circ}$ , 99.0	75.38 $^{\circ}$ , 99.0	25.242 $^{\circ}$ , 99.8
Refinement method	Full-matrix least-squares on $F^{2}$	Full-matrix least-squares on $F^{2}$	Full-matrix least-squares on $F^{2}$	Full-matrix least-squares on $F^{2}$	Full-matrix least-squares on $F^{2}$
Data/restraints/parameters	3259/0/172	2957/0/172	2623/0/259	2170/0/140	2677/0/149
Goodness-of-fit on $F^{2}$	0.883	1.436	4.030	3.16	1.052
Final R indices [I > 2sigma(I)]	$R_{1}$ = 0.0569	$R_{1}$ = 0.0703	$R_{1}$ = 0.0408	$R_{1}$ = 0.0408	$R_{1}$ = 0.0485
Final R indices [I > 2sigma(I)]	$w R_{2}$ = 0.1289	$w R_{2}$ = 0.1686	$w R_{2}$ = 0.1184	$w R_{2}$ = 0.0534	$w R_{2}$ = 0.1315
R indices (all data)	$R_{1}$ = 0.1079	$R_{1}$ = 0.1149	$R_{1}$ = 0.0422	$R_{1}$ = 0.0429	$R_{1}$ = 0.0669
R indices (all data)	$w R_{2}$ = 0.1433	$w R_{2}$ = 0.2216	$w R_{2}$ = 0.1192	$w R_{2}$ = 0.0540	$w R_{2}$ = 0.1384