Novel　3-(2-naphthoyl)-6,12-diphenyl-3,9-diazatetraasterane　(3,　Tetraethyl　3-(2-naphthoyl)-6,12-diphenyl-3,9-diazapentacyclo　[6.4.0.0(2,7).0(4,11).0(5,10)]dodecane-1,5,7,11-tetracarboxylate)　was　prepared　by.　510　naphthoylation　of　3,9-diazatetraasterane　(2).　The　target　compound　was　isolated　and　unambiguously　confirmed　by　NMR　spectra,　high-resolution　mass　spectrometry,　and　single-crystal　X-ray　diffraction　analysis.　In　order　to　discuss　the　spatial　effects　on　the　NMR　of　3　by　the　naphthoyl　group,　spectra　analysis　(1D-NMR　and　2D-NMR)　of　2　and　3　was　conducted　in　details　by　the　shifts　and　assignments　of　signals.　Single-crystal　X-ray　diffraction　assists　to　explain　the　molecular　asymmetry　of　3　and　elucidates　the　effects　of　naphthoyl　group　on　the　geometry　of　the　central　cage　of　3,9-diazatetraasterane.　(C)　2016　Elsevier　B.V.　All　rights　reserved.