Synthesis and Molecular Structure of 4′,9′,4^″,9^″-Tetra-tert-butyl-1′,6′,1^″,6^″-tetramethoxy-2,5-dioxa[3.3]metabiphenylophane

Table 1

Crystallographic data for 4′,9′,4′′,9′′-tetra-tert-butyl-1′,6′,1′′,6′′-tetramethoxy-2,5-dioxa[3.3]metabiphenylophane 3.

Empirical f	C48H64O6
Formula weight	736.99
Temperature	90 K
Wavelength	0.71073 Å
Crystal system	Monoclinic
Space group	(no. 14)
Unit cell dimensions	= 19.908(2) Å
	= 9.7193(11) Å	= 109.594(1)°
	= 23.350(3) Å
Volume	4256.5(8) Å^−3
	4
Density (calculated)	1.150 g/cm^3
Absorption coefficient	0.074 mm^−1
(000)	1600
Crystal size	0.400 0.350 0.250 mm
Theta range for data collection	1.17° to 28.65°
Index ranges	−26 ≤ ≤ 26, −13 ≤ ≤ 13, −29 ≤ ≤ 30
Reflections collected	48529
Independent reflections	10321 [(int) = 0.0234]
Reflections [> 2sigma()]	9126
Completeness to theta = 28.65°	94.4%
Absorption correction	Empirical
Refinement method	Full-matrix least-squares on
Data/restraints/parameters	10321/0/503
Goodness-of-fit on	1.072
Final R1 indices [ > 2sigma()]	= 0.0408, = 0.1157
indices (all data)	= 0.0476, = 0.1279
Largest diff. peak and hole; (RMS deviation of 0.11 e/Å^3)	0.476 and −0.331 eÅ^−3