# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/220 data_global _audit_creation_date ? _audit_creation_method 'PARSTCIF' _audit_update_record ? # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _iucr_compatibility_tag ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _publ_requested_journal 'Acta Cryst. C' _publ_requested_category ? _publ_requested_coeditor_name ? # AUTHOR LIST loop_ _publ_author_name ; S.Canestrari, A.Nar'in, P.Sgarabotto, L.Righi, L.Greci ; # TITLE _publ_section_title ;New Insights on the Reaction of Trialkylphosphites with 2-Phenyl-3-phenylimino- 3H-indol-N-oxide: An Indolic Nitrone. Crystal structures of 1-Diethylphosphonyl -2-Phenyl-3-Phenylamino Indole and N-2-Phenyl-3,1-Benzoxazine-4-Phenylimino ; # TEXT data_(I) # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source # # symbol number description f' f'' source # 'P ' 4 'Phosphorus ' 0.2955 0.4335 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'O ' 12 'Oxygen ' 0.0492 0.0322 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'N ' 8 'Nitrogen ' 0.0311 0.0180 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'C ' 96 'Carbon ' 0.0181 0.0091 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'H ' 100 'Hydrogen ' 0.0000 0.0000 'Int. Tab. C, 4.2.6.8, 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_group # # Table of coordinates # -------------------- # #label x/a y/b z/c Ueq tmf typ calc sof dis P1 0.7333(1) 0.1633(1) 0.2098(1) 0.0563(4) Uani P . . . O1 0.7872(2) 0.0997(3) 0.2788(1) 0.0652(11) Uani O . . . O3 0.6528(2) 0.0682(3) 0.1528(1) 0.0645(10) Uani O . . . O4 0.6494(3) 0.2856(4) 0.2070(2) 0.1012(16) Uani O . . . N1 0.8248(3) 0.2264(4) 0.1703(2) 0.0531(11) Uani N . . . N2 1.1000(3) 0.3252(4) 0.1557(2) 0.0636(14) Uani N . . . C1 0.9440(3) 0.2447(4) 0.1993(2) 0.0514(13) Uani C . . . C2 0.9868(3) 0.2893(4) 0.1468(2) 0.0534(14) Uani C . . . C3 0.8969(3) 0.3029(4) 0.0818(2) 0.0547(16) Uani C . . . C4 0.8940(4) 0.3487(4) 0.0131(2) 0.0661(19) Uani C . . . C5 0.7917(5) 0.3544(5) -0.0383(2) 0.0761(20) Uani C . . . C6 0.6935(5) 0.3215(5) -0.0221(2) 0.0794(22) Uani C . . . C7 0.6939(4) 0.2734(5) 0.0459(2) 0.0690(17) Uani C . . . C8 0.7978(3) 0.2657(4) 0.0969(2) 0.0542(14) Uani C . . . C11 1.0066(3) 0.2246(4) 0.2755(2) 0.0514(13) Uani C . . . C12 1.0967(4) 0.1331(4) 0.2933(3) 0.0669(17) Uani C . . . C13 1.1606(4) 0.1191(5) 0.3651(3) 0.0753(20) Uani C . . . C14 1.1347(4) 0.1948(5) 0.4175(3) 0.0772(20) Uani C . . . C15 1.0444(4) 0.2867(6) 0.3997(2) 0.0714(18) Uani C . . . C16 0.9822(4) 0.3007(5) 0.3296(2) 0.0618(16) Uani C . . . C21 1.1698(3) 0.2455(4) 0.1273(2) 0.0543(13) Uani C . . . C22 1.1355(4) 0.1163(4) 0.0956(2) 0.0626(17) Uani C . . . C23 1.2066(5) 0.0386(6) 0.0686(3) 0.0779(21) Uani C . . . C24 1.3134(6) 0.0854(7) 0.0728(3) 0.0915(26) Uani C . . . C25 1.3474(5) 0.2134(7) 0.1043(3) 0.0861(22) Uani C . . . C26 1.2760(4) 0.2937(6) 0.1311(2) 0.0679(18) Uani C . . . C31 0.6919(5) -0.0681(6) 0.1359(4) 0.0910(26) Uani C . . . C32 0.5941(8) -0.1553(11) 0.0999(7) 0.1390(52) Uani C . . . C41 0.6463(11) 0.3779(11) 0.2564(5) 0.1699(56) Uani C . . . C42 0.5611(9) 0.4856(9) 0.2355(6) 0.1320(44) Uani C . . . H2 1.1257(39) 0.4032(54) 0.1775(25) 0.089(16) Uiso H . . . H4 0.9671(30) 0.3764(39) 0.0042(19) 0.056(11) Uiso H . . . H5 0.7908(33) 0.3900(45) -0.0855(23) 0.079(12) Uiso H . . . H6 0.6209(36) 0.3293(47) -0.0602(24) 0.078(14) Uiso H . . . H7 0.6187(38) 0.2481(50) 0.0581(23) 0.075(14) Uiso H . . . H12 1.1227(36) 0.0829(49) 0.2541(23) 0.087(14) Uiso H . . . H13 1.2162(33) 0.0519(45) 0.3704(21) 0.069(13) Uiso H . . . H14 1.1866(33) 0.1813(41) 0.4693(22) 0.067(11) Uiso H . . . H15 1.0161(35) 0.3502(48) 0.4376(23) 0.084(13) Uiso H . . . H16 0.9248(29) 0.3652(38) 0.3165(18) 0.061(11) Uiso H . . . H22 1.0514(34) 0.0839(43) 0.0907(19) 0.074(12) Uiso H . . . H23 1.1778(35) -0.0476(52) 0.0450(23) 0.084(14) Uiso H . . . H24 1.3674(43) 0.0256(63) 0.0532(28) 0.133(19) Uiso H . . . H25 1.4201(38) 0.2445(48) 0.1065(23) 0.082(14) Uiso H . . . H26 1.3102(41) 0.3783(58) 0.1554(26) 0.102(18) Uiso H . . . H311 0.7479(54) -0.1158(70) 0.1779(35) 0.132(25) Uiso H . . . H312 0.7610(64) -0.0490(83) 0.1104(40) 0.205(32) Uiso H . . . H321 0.5371(45) -0.1562(57) 0.1336(32) 0.098(19) Uiso H . . . H322 0.618(10) -0.259(14) 0.0924(67) 0.121(66) Uiso H . . . H323 0.5503(72) -0.107(10) 0.0495(45) 0.180(39) Uiso H . . . H411 0.6088(34) 0.3128(47) 0.2946(24) 0.037(13) Uiso H . . . H412 0.7192(58) 0.4166(79) 0.2828(41) 0.177(29) Uiso H . . . H421 0.5878(67) 0.5522(80) 0.1959(42) 0.134(33) Uiso H . . . H422 0.4778(92) 0.448(13) 0.2084(66) 0.219(58) Uiso H . . . H423 0.5591(90) 0.551(12) 0.2789(58) 0.210(52) Uiso H . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 #label U11 U22 U33 U23 U13 U12 P1 0.0596(6) 0.0565(6) 0.0551(6) 0.0029(5) 0.0204(4) 0.0074(5) O1 0.0674(17) 0.0672(18) 0.0613(16) 0.0127(14) 0.0193(13) -0.0018(14) O3 0.0522(15) 0.0660(19) 0.0736(18) -0.0030(14) 0.0154(14) -0.0010(13) O4 0.1306(29) 0.1033(28) 0.0774(21) 0.0052(19) 0.0423(22) 0.0624(23) N1 0.0548(18) 0.0586(20) 0.0434(15) 0.0035(14) 0.0103(13) -0.0033(15) N2 0.0707(23) 0.0559(23) 0.0711(22) -0.0154(18) 0.0314(18) -0.0100(18) C1 0.0611(22) 0.0465(22) 0.0460(19) -0.0015(16) 0.0144(17) 0.0017(18) C2 0.0621(23) 0.0471(21) 0.0527(21) -0.0105(17) 0.0192(18) -0.0067(18) C3 0.0772(26) 0.0429(22) 0.0451(20) -0.0059(16) 0.0194(19) -0.0035(18) C4 0.0990(34) 0.0503(24) 0.0542(23) -0.0039(19) 0.0304(24) -0.0086(24) C5 0.1100(39) 0.0652(30) 0.0505(25) 0.0022(21) 0.0191(26) -0.0074(27) C6 0.0995(38) 0.0713(33) 0.0521(25) 0.0075(23) -0.0022(26) 0.0031(28) C7 0.0727(28) 0.0659(28) 0.0608(25) 0.0012(21) 0.0073(22) -0.0047(23) C8 0.0617(23) 0.0510(23) 0.0454(19) -0.0007(17) 0.0086(18) -0.0015(18) C11 0.0524(20) 0.0513(22) 0.0469(19) 0.0009(17) 0.0087(16) -0.0047(18) C12 0.0678(26) 0.0560(27) 0.0723(27) 0.0004(21) 0.0129(22) 0.0026(20) C13 0.0613(27) 0.0554(28) 0.0949(38) 0.0182(26) 0.0004(26) 0.0005(23) C14 0.0838(33) 0.0772(36) 0.0589(27) 0.0142(25) 0.0021(25) -0.0232(27) C15 0.0787(30) 0.0816(33) 0.0507(24) 0.0017(23) 0.0140(22) -0.0059(26) C16 0.0633(25) 0.0679(29) 0.0509(21) -0.0012(20) 0.0115(18) 0.0029(22) C21 0.0572(22) 0.0565(26) 0.0467(19) 0.0051(17) 0.0110(17) 0.0058(18) C22 0.0780(29) 0.0491(24) 0.0607(24) -0.0003(19) 0.0202(22) 0.0069(21) C23 0.0942(38) 0.0626(32) 0.0710(29) -0.0026(23) 0.0149(26) 0.0210(27) C24 0.0996(42) 0.0973(45) 0.0802(33) 0.0010(31) 0.0302(31) 0.0377(38) C25 0.0602(28) 0.1124(45) 0.0857(34) 0.0083(32) 0.0214(26) 0.0153(30) C26 0.0628(26) 0.0766(31) 0.0619(25) 0.0016(23) 0.0144(21) 0.0007(23) C31 0.0654(30) 0.0751(36) 0.1216(47) -0.0293(33) 0.0098(34) -0.0006(29) C32 0.093(5) 0.109(6) 0.206(11) -0.065(7) 0.031(6) -0.023(5) C41 0.224(12) 0.139(8) 0.113(6) -0.062(6) -0.004(7) 0.086(8) C42 0.1374(70) 0.0964(54) 0.1499(78) -0.0391(56) 0.0222(64) 0.0465(49) # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.454(3) . . no P1 O3 1.557(3) . . no P1 O4 1.558(4) . . no P1 N1 1.663(5) . . no O3 C31 1.463(7) . . no O4 C41 1.32(1) . . no N1 C1 1.436(5) . . no N1 C8 1.425(5) . . no N2 C2 1.410(5) . . no N2 C21 1.387(6) . . no N2 H2 0.87(4) . . no C1 C2 1.355(6) . . no C1 C11 1.479(5) . . no C2 C3 1.434(5) . . no C3 C4 1.403(6) . . no C3 C8 1.394(6) . . no C4 C5 1.374(6) . . no C4 H4 1.01(4) . . no C5 C6 1.384(9) . . no C5 H5 0.98(4) . . no C6 C7 1.405(6) . . no C6 H6 0.99(3) . . no C7 C8 1.386(5) . . no C7 H7 1.06(5) . . no C11 C12 1.384(6) . . no C11 C16 1.388(6) . . no C12 C13 1.404(7) . . no C12 H12 1.03(5) . . no C13 C14 1.367(8) . . no C13 H13 0.93(4) . . no C14 C15 1.389(7) . . no C14 H14 1.04(3) . . no C15 C16 1.370(5) . . no C15 H15 1.09(4) . . no C16 H16 0.92(3) . . no C21 C22 1.393(5) . . no C21 C26 1.380(6) . . no C22 C23 1.373(8) . . no C22 H22 1.07(4) . . no C23 C24 1.38(1) . . no C23 H23 0.96(4) . . no C24 C25 1.381(9) . . no C24 H24 1.04(6) . . no C25 C26 1.387(9) . . no C25 H25 0.94(4) . . no C26 H26 0.97(5) . . no C31 C32 1.47(1) . . no C31 H311 1.02(6) . . no C31 H312 1.13(8) . . no C32 H321 1.10(6) . . no C32 H322 1.06(*) . . no C32 H323 1.08(8) . . no C41 C42 1.45(1) . . no C41 H411 1.17(5) . . no C41 H412 0.98(6) . . no C42 H421 1.12(8) . . no C42 H422 1.08(*) . . no C42 H423 1.06(*) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 O3 116.5(2) . . . no O1 P1 O4 118.1(2) . . . no O1 P1 N1 112.9(2) . . . no O3 P1 O4 97.4(2) . . . no O3 P1 N1 105.3(2) . . . no O4 P1 N1 104.6(2) . . . no P1 O3 C31 119.7(3) . . . no P1 O4 C41 129.8(6) . . . no P1 N1 C1 128.9(3) . . . no P1 N1 C8 124.8(3) . . . no C1 N1 C8 106.2(3) . . . no C2 N2 C21 122.4(4) . . . no C2 N2 H2 119(3) . . . no C21 N2 H2 119(3) . . . no N1 C1 C2 109.1(4) . . . no N1 C1 C11 124.2(3) . . . no C2 C1 C11 126.6(4) . . . no N2 C2 C1 125.6(4) . . . no N2 C2 C3 125.5(4) . . . no C1 C2 C3 108.8(3) . . . no C2 C3 C4 132.3(4) . . . no C2 C3 C8 107.4(4) . . . no C4 C3 C8 120.3(4) . . . no C3 C4 C5 118.2(4) . . . no C3 C4 H4 118(2) . . . no C5 C4 H4 124(2) . . . no C4 C5 C6 121.0(5) . . . no C4 C5 H5 117(3) . . . no C6 C5 H5 122(3) . . . no C5 C6 C7 122.0(4) . . . no C5 C6 H6 119(3) . . . no C7 C6 H6 119(3) . . . no C6 C7 C8 116.4(4) . . . no C6 C7 H7 122(2) . . . no C8 C7 H7 122(3) . . . no N1 C8 C3 108.4(3) . . . no N1 C8 C7 129.5(4) . . . no C3 C8 C7 122.1(4) . . . no C1 C11 C12 119.1(4) . . . no C1 C11 C16 122.1(3) . . . no C12 C11 C16 118.7(4) . . . no C11 C12 C13 119.6(5) . . . no C11 C12 H12 121(3) . . . no C13 C12 H12 119(2) . . . no C12 C13 C14 120.7(5) . . . no C12 C13 H13 111(3) . . . no C14 C13 H13 128(3) . . . no C13 C14 C15 119.8(5) . . . no C13 C14 H14 117(2) . . . no C15 C14 H14 123(2) . . . no C14 C15 C16 119.5(4) . . . no C14 C15 H15 125(2) . . . no C16 C15 H15 115(2) . . . no C11 C16 C15 121.7(4) . . . no C11 C16 H16 118(2) . . . no C15 C16 H16 121(2) . . . no N2 C21 C22 121.3(4) . . . no N2 C21 C26 119.7(4) . . . no C22 C21 C26 119.0(4) . . . no C21 C22 C23 120.2(4) . . . no C21 C22 H22 118(2) . . . no C23 C22 H22 122(2) . . . no C22 C23 C24 121.2(6) . . . no C22 C23 H23 117(3) . . . no C24 C23 H23 122(3) . . . no C23 C24 C25 118.6(6) . . . no C23 C24 H24 121(3) . . . no C25 C24 H24 120(3) . . . no C24 C25 C26 120.9(6) . . . no C24 C25 H25 118(3) . . . no C26 C25 H25 121(3) . . . no C21 C26 C25 120.1(5) . . . no C21 C26 H26 125(3) . . . no C25 C26 H26 114(3) . . . no O3 C31 C32 109.3(6) . . . no O3 C31 H311 114(4) . . . no O3 C31 H312 108(4) . . . no C32 C31 H311 114(4) . . . no C32 C31 H312 121(4) . . . no H311 C31 H312 90(6) . . . no C31 C32 H321 108(3) . . . no C31 C32 H322 111(7) . . . no C31 C32 H323 109(5) . . . no H321 C32 H322 110(8) . . . no H321 C32 H323 108(6) . . . no H322 C32 H323 111(9) . . . no O4 C41 C42 116.4(9) . . . no O4 C41 H411 102(2) . . . no O4 C41 H412 115(5) . . . no C42 C41 H411 99(2) . . . no C42 C41 H412 112(5) . . . no H411 C41 H412 110(5) . . . no C41 C42 H421 105(4) . . . no C41 C42 H422 115(7) . . . no C41 C42 H423 112(6) . . . no H421 C42 H422 106(8) . . . no H421 C42 H423 107(7) . . . no H422 C42 H423 110(9) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 O3 C31 -51.9(4) . . . . no O4 P1 O3 C31 -178.5(4) . . . . no N1 P1 O3 C31 74.1(4) . . . . no O1 P1 O4 C41 28.4(8) . . . . no O3 P1 O4 C41 153.9(7) . . . . no N1 P1 O4 C41 -98.1(8) . . . . no O1 P1 N1 C1 -10.4(5) . . . . no O1 P1 N1 C8 165.4(3) . . . . no O3 P1 N1 C1 -138.6(4) . . . . no O3 P1 N1 C8 37.2(4) . . . . no O4 P1 N1 C1 119.2(4) . . . . no O4 P1 N1 C8 -64.9(4) . . . . no P1 O3 C31 C32 161.8(6) . . . . no P1 O3 C31 H311 33(4) . . . . no P1 O3 C31 H312 -65(4) . . . . no P1 O4 C41 C42 176.0(6) . . . . no P1 O4 C41 H411 -76(2) . . . . no P1 O4 C41 H412 43(5) . . . . no P1 N1 C1 C2 175.3(3) . . . . no P1 N1 C1 C11 -7.8(6) . . . . no C8 N1 C1 C2 -1.2(5) . . . . no C8 N1 C1 C11 175.8(4) . . . . no P1 N1 C8 C3 -175.3(3) . . . . no P1 N1 C8 C7 6.7(7) . . . . no C1 N1 C8 C3 1.4(4) . . . . no C1 N1 C8 C7 -176.6(4) . . . . no C21 N2 C2 C1 111.2(5) . . . . no C21 N2 C2 C3 -73.3(6) . . . . no H2 N2 C2 C1 -72(4) . . . . no H2 N2 C2 C3 103(4) . . . . no C2 N2 C21 C22 -7.8(6) . . . . no C2 N2 C21 C26 173.0(4) . . . . no H2 N2 C21 C22 176(4) . . . . no H2 N2 C21 C26 -2(4) . . . . no N1 C1 C2 N2 176.7(4) . . . . no N1 C1 C2 C3 0.5(5) . . . . no C11 C1 C2 N2 -0.2(7) . . . . no C11 C1 C2 C3 -176.4(4) . . . . no N1 C1 C11 C12 125.2(5) . . . . no N1 C1 C11 C16 -58.7(6) . . . . no C2 C1 C11 C12 -58.4(6) . . . . no C2 C1 C11 C16 117.7(5) . . . . no N2 C2 C3 C4 1.5(7) . . . . no N2 C2 C3 C8 -175.9(4) . . . . no C1 C2 C3 C4 177.7(4) . . . . no C1 C2 C3 C8 0.3(5) . . . . no C2 C3 C4 C5 -177.6(4) . . . . no C2 C3 C4 H4 2(3) . . . . no C8 C3 C4 C5 -0.6(6) . . . . no C8 C3 C4 H4 179(2) . . . . no C2 C3 C8 N1 -1.1(4) . . . . no C2 C3 C8 C7 177.1(4) . . . . no C4 C3 C8 N1 -178.8(4) . . . . no C4 C3 C8 C7 -0.6(6) . . . . no C3 C4 C5 C6 2.7(7) . . . . no C3 C4 C5 H5 178(3) . . . . no H4 C4 C5 C6 -176(3) . . . . no H4 C4 C5 H5 -1(4) . . . . no C4 C5 C6 C7 -3.7(8) . . . . no C4 C5 C6 H6 178(3) . . . . no H5 C5 C6 C7 -178(3) . . . . no H5 C5 C6 H6 3(4) . . . . no C5 C6 C7 C8 2.4(7) . . . . no C5 C6 C7 H7 -179(3) . . . . no H6 C6 C7 C8 -179(3) . . . . no H6 C6 C7 H7 -1(4) . . . . no C6 C7 C8 N1 177.5(4) . . . . no C6 C7 C8 C3 -0.3(6) . . . . no H7 C7 C8 N1 0(3) . . . . no H7 C7 C8 C3 -177(3) . . . . no C1 C11 C12 C13 176.4(4) . . . . no C1 C11 C12 H12 3(3) . . . . no C16 C11 C12 C13 0.2(7) . . . . no C16 C11 C12 H12 -172(3) . . . . no C1 C11 C16 C15 -176.5(4) . . . . no C1 C11 C16 H16 0(3) . . . . no C12 C11 C16 C15 -0.4(7) . . . . no C12 C11 C16 H16 176(3) . . . . no C11 C12 C13 C14 0.0(8) . . . . no C11 C12 C13 H13 177(3) . . . . no H12 C12 C13 C14 174(3) . . . . no H12 C12 C13 H13 -8(4) . . . . no C12 C13 C14 C15 -0.1(8) . . . . no C12 C13 C14 H14 -178(3) . . . . no H13 C13 C14 C15 -176(3) . . . . no H13 C13 C14 H14 5(4) . . . . no C13 C14 C15 C16 -0.1(8) . . . . no C13 C14 C15 H15 179(3) . . . . no H14 C14 C15 C16 178(3) . . . . no H14 C14 C15 H15 -2(4) . . . . no C14 C15 C16 C11 0.4(7) . . . . no C14 C15 C16 H16 -175(3) . . . . no H15 C15 C16 C11 -178(3) . . . . no H15 C15 C16 H16 5(4) . . . . no N2 C21 C22 C23 -179.2(4) . . . . no N2 C21 C22 H22 4(3) . . . . no C26 C21 C22 C23 0.0(7) . . . . no C26 C21 C22 H22 -176(2) . . . . no N2 C21 C26 C25 178.6(5) . . . . no N2 C21 C26 H26 4(4) . . . . no C22 C21 C26 C25 -0.7(7) . . . . no C22 C21 C26 H26 -174(4) . . . . no C21 C22 C23 C24 0.7(8) . . . . no C21 C22 C23 H23 -176(3) . . . . no H22 C22 C23 C24 177(3) . . . . no H22 C22 C23 H23 0(4) . . . . no C22 C23 C24 C25 -0.6(9) . . . . no C22 C23 C24 H24 179(4) . . . . no H23 C23 C24 C25 177(3) . . . . no H23 C23 C24 H24 -3(5) . . . . no C23 C24 C25 C26 0(1) . . . . no C23 C24 C25 H25 -178(3) . . . . no H24 C24 C25 C26 -179(4) . . . . no H24 C24 C25 H25 1(5) . . . . no C24 C25 C26 C21 0.8(9) . . . . no C24 C25 C26 H26 175(3) . . . . no H25 C25 C26 C21 -179(3) . . . . no H25 C25 C26 H26 -4(5) . . . . no O3 C31 C32 H321 -52(3) . . . . no O3 C31 C32 H322 -172(8) . . . . no O3 C31 C32 H323 64(5) . . . . no H311 C31 C32 H321 77(5) . . . . no H311 C31 C32 H322 -43(9) . . . . no H311 C31 C32 H323 -166(7) . . . . no H312 C31 C32 H321 -177(6) . . . . no H312 C31 C32 H322 61(9) . . . . no H312 C31 C32 H323 -60(7) . . . . no O4 C41 C42 H421 -68(4) . . . . no O4 C41 C42 H422 48(7) . . . . no O4 C41 C42 H423 175(7) . . . . no H411 C41 C42 H421 -176(5) . . . . no H411 C41 C42 H422 -60(8) . . . . no H411 C41 C42 H423 66(7) . . . . no H412 C41 C42 H421 66(7) . . . . no H412 C41 C42 H422 -176(9) . . . . no H412 C41 C42 H423 -49(8) . . . . no # CHEMICAL DATA _chemical_name_systematic ; 1-Diethylphosphnyl-2-Phenyl-3-Phenylamino Indole ; _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'P1 O3 N2 C24 H25 ' _chemical_formula_weight 420.45 _chemical_melting_point ? _chemical_compound_source ; ...... ; # CRYSTAL DATA _cell_length_a 12.437(3) _cell_length_b 9.569(2) _cell_length_c 19.543(4) _cell_angle_alpha 90.00(0) _cell_angle_beta 106.9(1) _cell_angle_gamma 90.0(0) _cell_volume 2225.(1) _cell_formula_units_Z 4.00 _cell_measurement_temperature 295 _cell_measurement_radiation X _cell_measurement_wavelength 1.54178 _cell_measurement_reflns_used 35 _cell_measurement_theta_min 24 _cell_measurement_theta_max 41 _symmetry_space_group_name_H-M ' P 21/C ' _symmetry_Int_Tables_number 14 _exptl_crystal_description ; ...... ; _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.2549 _exptl_crystal_F_000 888.0 _exptl_absorpt_coefficient_mu 1.3143 # EXPERIMENTAL DATA _diffrn_special_details ; ....... ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type X _diffrn_radiation_source Cu _diffrn_radiation_monochromator Graphite _reflns_number_total 4647 # REFINEMENT DATA _refine_special_details ; ...... ; _refine_ls_extinction_coef ? _refine_ls_number_reflns 2070 _refine_ls_number_parameters 371 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.049 _refine_ls_restrained_S_all 0.339 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag #D H A D-H H..A D..A D-H..A A site sym Flg N2 H2 O1 0.87(5) 2.21(5) 3.076(5) 170(5) 4_755 ? # -x+2,+y+1/2,-z+1/2 #-------------------------- data section of block --------------------------- data_(II) # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source # # symbol number description f' f'' source # 'O ' 4 'Oxygen ' 0.0492 0.0322 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'N ' 8 'Nitrogen ' 0.0311 0.0180 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'C ' 80 'Carbon ' 0.0181 0.0091 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'H ' 56 'Hydrogen ' 0.0000 0.0000 'Int. Tab. C, 4.2.6.8, 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_group # # Table of coordinates # -------------------- # #label x/a y/b z/c Ueq tmf typ calc sof dis O3 0.3162(3) 0.0491(8) 0.8626(1) 0.0742(16) Uani O . . . N1 0.1394(4) 0.0408(10) 0.8134(2) 0.0682(19) Uani N . . . N4 0.4945(4) 0.3104(11) 0.8510(1) 0.0804(20) Uani N . . . C2 0.1969(5) -0.0380(13) 0.8481(2) 0.0676(22) Uani C . . . C4 0.3826(5) 0.2411(13) 0.8379(2) 0.0683(23) Uani C . . . C5 0.3200(5) 0.3455(12) 0.7988(2) 0.0608(21) Uani C . . . C6 0.3753(6) 0.5487(14) 0.7726(2) 0.0727(25) Uani C . . . C7 0.3144(6) 0.6420(14) 0.7355(2) 0.0796(27) Uani C . . . C8 0.1937(7) 0.5387(15) 0.7242(2) 0.0805(30) Uani C . . . C9 0.1378(6) 0.3388(15) 0.7499(2) 0.0733(28) Uani C . . . C10 0.1996(5) 0.2410(13) 0.7875(2) 0.0642(21) Uani C . . . C21 0.1425(5) -0.2394(14) 0.8787(2) 0.0658(23) Uani C . . . C22 0.1985(7) -0.2887(16) 0.9190(2) 0.0847(29) Uani C . . . C23 0.1422(8) -0.4726(19) 0.9473(3) 0.1023(34) Uani C . . . C24 0.0299(8) -0.6077(17) 0.9353(3) 0.0971(35) Uani C . . . C25 -0.0236(7) -0.5591(17) 0.8955(3) 0.0897(32) Uani C . . . C26 0.0300(7) -0.3783(15) 0.8666(2) 0.0838(28) Uani C . . . C41 0.5526(5) 0.2030(16) 0.8902(2) 0.0754(26) Uani C . . . C42 0.6481(8) 0.0088(19) 0.8890(3) 0.1109(37) Uani C . . . C43 0.7121(8) -0.0768(21) 0.9267(3) 0.1261(45) Uani C . . . C44 0.6855(8) 0.0325(20) 0.9648(3) 0.0999(31) Uani C . . . C45 0.5907(10) 0.2222(22) 0.9662(3) 0.1414(49) Uani C . . . C46 0.5257(9) 0.3050(24) 0.9289(3) 0.1369(45) Uani C . . . H6 0.4533(49) 0.631(10) 0.7833(14) 0.084(18) Uiso H . . . H7 0.3501(45) 0.805(12) 0.7140(16) 0.082(18) Uiso H . . . H8 0.1532(42) 0.606(10) 0.6974(15) 0.072(17) Uiso H . . . H9 0.0550(39) 0.2592(96) 0.7420(12) 0.061(15) Uiso H . . . H22 0.2876(51) -0.193(13) 0.9275(17) 0.124(21) Uiso H . . . H23 0.1823(52) -0.522(13) 0.9746(18) 0.109(21) Uiso H . . . H24 -0.0044(44) -0.742(13) 0.9562(17) 0.085(21) Uiso H . . . H25 -0.0971(49) -0.639(11) 0.8849(16) 0.083(21) Uiso H . . . H26 -0.0105(39) -0.3235(98) 0.8371(14) 0.061(14) Uiso H . . . H42 0.6612(59) -0.052(14) 0.8607(22) 0.138(29) Uiso H . . . H43 0.7811(82) -0.201(21) 0.9259(28) 0.229(45) Uiso H . . . H44 0.7275(44) -0.032(10) 0.9911(17) 0.085(18) Uiso H . . . H45 0.5772(66) 0.299(18) 0.9951(23) 0.187(35) Uiso H . . . H46 0.4748(86) 0.440(21) 0.9280(30) 0.220(44) Uiso H . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 #label U11 U22 U33 U23 U13 U12 O3 0.0596(25) 0.0843(31) 0.0780(27) 0.0044(23) -0.0023(19) -0.0019(22) N1 0.0627(29) 0.0730(38) 0.0685(30) -0.0007(30) -0.0014(24) -0.0007(29) N4 0.0630(30) 0.1013(42) 0.0761(35) -0.0027(32) -0.0048(26) 0.0010(31) C2 0.0519(33) 0.0721(43) 0.0788(41) -0.0092(39) 0.0027(29) 0.0064(33) C4 0.0591(38) 0.0779(43) 0.0685(36) -0.0054(39) 0.0083(32) 0.0087(40) C5 0.0600(35) 0.0599(39) 0.0627(33) -0.0001(33) 0.0049(30) 0.0022(32) C6 0.0633(41) 0.0747(48) 0.0801(42) -0.0045(41) 0.0033(34) -0.0018(39) C7 0.0691(43) 0.0871(52) 0.0829(45) 0.0110(42) 0.0058(36) -0.0032(38) C8 0.0857(50) 0.0860(51) 0.0693(42) 0.0058(41) -0.0016(37) 0.0073(44) C9 0.0587(37) 0.0785(50) 0.0823(45) 0.0048(38) -0.0002(36) 0.0000(37) C10 0.0617(37) 0.0664(43) 0.0645(34) -0.0025(37) 0.0042(31) 0.0008(37) C21 0.0670(36) 0.0646(43) 0.0662(35) -0.0022(38) 0.0087(31) 0.0073(36) C22 0.0836(47) 0.0923(57) 0.0777(43) 0.0158(45) 0.0002(38) 0.0044(44) C23 0.1112(60) 0.1075(65) 0.0870(51) 0.0194(51) -0.0052(49) 0.0139(53) C24 0.1041(61) 0.0892(61) 0.0998(61) 0.0114(52) 0.0232(52) 0.0039(46) C25 0.0832(52) 0.0919(57) 0.0945(58) -0.0013(50) 0.0089(44) -0.0058(47) C26 0.0804(45) 0.0878(54) 0.0833(46) 0.0034(42) 0.0055(38) -0.0005(40) C41 0.0543(34) 0.0979(56) 0.0740(40) -0.0043(43) 0.0022(33) -0.0069(40) C42 0.1163(60) 0.1339(74) 0.0836(56) -0.0030(56) 0.0155(49) 0.0424(57) C43 0.1172(66) 0.1617(96) 0.0993(63) 0.0164(66) 0.0039(52) 0.0573(61) C44 0.0941(54) 0.1113(68) 0.0915(55) 0.0165(55) -0.0225(49) -0.0018(52) C45 0.1545(84) 0.1688(96) 0.0965(65) -0.0289(71) -0.0348(64) 0.0640(76) C46 0.1409(73) 0.1747(96) 0.0920(58) -0.0312(60) -0.0225(55) 0.0838(70) # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3 C2 1.384(6) . . no O3 C4 1.394(7) . . no N1 C2 1.263(8) . . no N1 C10 1.407(8) . . no N4 C4 1.278(7) . . no N4 C41 1.424(7) . . no C2 C21 1.474(9) . . no C4 C5 1.436(8) . . no C5 C6 1.398(9) . . no C5 C10 1.397(8) . . no C6 C7 1.360(9) . . no C6 H6 0.96(5) . . no C7 C8 1.40(1) . . no C7 H7 1.09(5) . . no C8 C9 1.38(1) . . no C8 H8 0.97(4) . . no C9 C10 1.384(9) . . no C9 H9 0.97(4) . . no C21 C22 1.374(9) . . no C21 C26 1.394(9) . . no C22 C23 1.38(1) . . no C22 H22 1.07(5) . . no C23 C24 1.38(1) . . no C23 H23 0.95(5) . . no C24 C25 1.35(1) . . no C24 H24 0.98(5) . . no C25 C26 1.38(1) . . no C25 H25 0.91(5) . . no C26 H26 1.02(4) . . no C41 C42 1.36(1) . . no C41 C46 1.33(1) . . no C42 C43 1.38(1) . . no C42 H42 0.94(6) . . no C43 C44 1.33(1) . . no C43 H43 0.94(9) . . no C44 C45 1.34(1) . . no C44 H44 0.96(5) . . no C45 C46 1.37(1) . . no C45 H45 0.98(7) . . no C46 H46 0.83(9) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O3 C4 119.5(4) . . . no C2 N1 C10 117.7(6) . . . no C4 N4 C41 122.4(4) . . . no O3 C2 N1 125.8(5) . . . no O3 C2 C21 111.2(5) . . . no N1 C2 C21 123.0(6) . . . no O3 C4 N4 118.6(5) . . . no O3 C4 C5 117.1(5) . . . no N4 C4 C5 124.3(5) . . . no C4 C5 C6 122.0(6) . . . no C4 C5 C10 118.1(5) . . . no C6 C5 C10 119.9(5) . . . no C5 C6 C7 120.8(6) . . . no C5 C6 H6 117(3) . . . no C7 C6 H6 122(3) . . . no C6 C7 C8 119.4(6) . . . no C6 C7 H7 125(3) . . . no C8 C7 H7 116(3) . . . no C7 C8 C9 120.4(7) . . . no C7 C8 H8 118(3) . . . no C9 C8 H8 122(3) . . . no C8 C9 C10 120.6(6) . . . no C8 C9 H9 122(3) . . . no C10 C9 H9 118(2) . . . no N1 C10 C5 121.8(5) . . . no N1 C10 C9 119.3(6) . . . no C5 C10 C9 118.9(5) . . . no C2 C21 C22 121.7(6) . . . no C2 C21 C26 118.9(5) . . . no C22 C21 C26 119.4(6) . . . no C21 C22 C23 119.9(7) . . . no C21 C22 H22 119(3) . . . no C23 C22 H22 121(3) . . . no C22 C23 C24 120.5(8) . . . no C22 C23 H23 121(4) . . . no C24 C23 H23 118(3) . . . no C23 C24 C25 119.0(8) . . . no C23 C24 H24 117(3) . . . no C25 C24 H24 124(3) . . . no C24 C25 C26 121.9(8) . . . no C24 C25 H25 125(3) . . . no C26 C25 H25 113(3) . . . no C21 C26 C25 119.3(7) . . . no C21 C26 H26 116(2) . . . no C25 C26 H26 124(3) . . . no N4 C41 C42 120.1(6) . . . no N4 C41 C46 122.4(6) . . . no C42 C41 C46 117.2(7) . . . no C41 C42 C43 120.3(8) . . . no C41 C42 H42 112(4) . . . no C43 C42 H42 128(4) . . . no C42 C43 C44 121.5(9) . . . no C42 C43 H43 121(6) . . . no C44 C43 H43 118(6) . . . no C43 C44 C45 118.4(9) . . . no C43 C44 H44 122(3) . . . no C45 C44 H44 120(3) . . . no C44 C45 C46 120.3(9) . . . no C44 C45 H45 115(5) . . . no C46 C45 H45 125(4) . . . no C41 C46 C45 122.3(8) . . . no C41 C46 H46 114(7) . . . no C45 C46 H46 123(7) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 O3 C2 N1 0.1(8) . . . . no C4 O3 C2 C21 -179.8(5) . . . . no C2 O3 C4 N4 -177.3(5) . . . . no C2 O3 C4 C5 2.0(7) . . . . no C10 N1 C2 O3 -1.9(9) . . . . no C10 N1 C2 C21 178.0(5) . . . . no C2 N1 C10 C5 1.6(9) . . . . no C2 N1 C10 C9 -178.1(6) . . . . no C41 N4 C4 O3 -1.2(8) . . . . no C41 N4 C4 C5 179.6(6) . . . . no C4 N4 C41 C42 108.9(8) . . . . no C4 N4 C41 C46 -77.7(9) . . . . no O3 C2 C21 C22 9.8(8) . . . . no O3 C2 C21 C26 -171.6(5) . . . . no N1 C2 C21 C22 -170.2(6) . . . . no N1 C2 C21 C26 8.5(9) . . . . no O3 C4 C5 C6 177.0(5) . . . . no O3 C4 C5 C10 -2.2(8) . . . . no N4 C4 C5 C6 -3.8(9) . . . . no N4 C4 C5 C10 177.1(6) . . . . no C4 C5 C6 C7 179.4(6) . . . . no C4 C5 C6 H6 -5(3) . . . . no C10 C5 C6 C7 -1.5(9) . . . . no C10 C5 C6 H6 173(3) . . . . no C4 C5 C10 N1 0.5(9) . . . . no C4 C5 C10 C9 -179.9(6) . . . . no C6 C5 C10 N1 -178.7(6) . . . . no C6 C5 C10 C9 0.9(9) . . . . no C5 C6 C7 C8 2(1) . . . . no C5 C6 C7 H7 178(3) . . . . no H6 C6 C7 C8 -171(3) . . . . no H6 C6 C7 H7 4(5) . . . . no C6 C7 C8 C9 0(1) . . . . no C6 C7 C8 H8 -178(3) . . . . no H7 C7 C8 C9 -177(3) . . . . no H7 C7 C8 H8 5(4) . . . . no C7 C8 C9 C10 1(1) . . . . no C7 C8 C9 H9 -177(3) . . . . no H8 C8 C9 C10 178(3) . . . . no H8 C8 C9 H9 0(4) . . . . no C8 C9 C10 N1 179.0(6) . . . . no C8 C9 C10 C5 -0.7(9) . . . . no H9 C9 C10 N1 -1(3) . . . . no H9 C9 C10 C5 178(3) . . . . no C2 C21 C22 C23 177.9(7) . . . . no C2 C21 C22 H22 -4(4) . . . . no C26 C21 C22 C23 0(1) . . . . no C26 C21 C22 H22 176(3) . . . . no C2 C21 C26 C25 -177.8(6) . . . . no C2 C21 C26 H26 -2(3) . . . . no C22 C21 C26 C25 1(1) . . . . no C22 C21 C26 H26 176(3) . . . . no C21 C22 C23 C24 0(1) . . . . no C21 C22 C23 H23 175(4) . . . . no H22 C22 C23 C24 -176(4) . . . . no H22 C22 C23 H23 -1(5) . . . . no C22 C23 C24 C25 0(1) . . . . no C22 C23 C24 H24 178(4) . . . . no H23 C23 C24 C25 -174(4) . . . . no H23 C23 C24 H24 3(5) . . . . no C23 C24 C25 C26 0(1) . . . . no C23 C24 C25 H25 180(4) . . . . no H24 C24 C25 C26 -176(4) . . . . no H24 C24 C25 H25 3(6) . . . . no C24 C25 C26 C21 0(1) . . . . no C24 C25 C26 H26 -174(3) . . . . no H25 C25 C26 C21 179(4) . . . . no H25 C25 C26 H26 5(5) . . . . no N4 C41 C42 C43 174.3(7) . . . . no N4 C41 C42 H42 -5(4) . . . . no C46 C41 C42 C43 0(1) . . . . no C46 C41 C42 H42 -179(4) . . . . no N4 C41 C46 C45 -173.2(8) . . . . no N4 C41 C46 H46 -2(7) . . . . no C42 C41 C46 C45 0(1) . . . . no C42 C41 C46 H46 171(7) . . . . no C41 C42 C43 C44 -1(1) . . . . no C41 C42 C43 H43 -175(7) . . . . no H42 C42 C43 C44 179(5) . . . . no H42 C42 C43 H43 5(8) . . . . no C42 C43 C44 C45 3(1) . . . . no C42 C43 C44 H44 178(4) . . . . no H43 C43 C44 C45 177(6) . . . . no H43 C43 C44 H44 -7(7) . . . . no C43 C44 C45 C46 -1(1) . . . . no C43 C44 C45 H45 -177(5) . . . . no H44 C44 C45 C46 -176(4) . . . . no H44 C44 C45 H45 6(6) . . . . no C44 C45 C46 C41 0(2) . . . . no C44 C45 C46 H46 -169(8) . . . . no H45 C45 C46 C41 177(5) . . . . no H45 C45 C46 H46 7(*) . . . . no # CHEMICAL DATA _chemical_name_systematic ; N-2-Phenyl-3,1-Benzoxazine-4-Phenylimino ; _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'O1 N2 C20 H14 ' _chemical_formula_weight 298.34 _chemical_melting_point ? _chemical_compound_source ; ...... ; # CRYSTAL DATA _cell_length_a 10.627(2) _cell_length_b 4.667(2) _cell_length_c 30.968(3) _cell_angle_alpha 90.00(0) _cell_angle_beta 93.0(1) _cell_angle_gamma 90.0(0) _cell_volume 1533.8(8) _cell_formula_units_Z 4.00 _cell_measurement_temperature 295 _cell_measurement_radiation X _cell_measurement_wavelength 1.54178 _cell_measurement_reflns_used ? _cell_measurement_theta_min 21 _cell_measurement_theta_max 32 _symmetry_cell_setting ? _symmetry_space_group_name_H-M ' P 21/c ' _symmetry_Int_Tables_number 14 _exptl_crystal_description ; ...... ; _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.2920 _exptl_crystal_F_000 624.0 _exptl_absorpt_coefficient_mu 0.6408 # EXPERIMENTAL DATA _diffrn_special_details ; ....... ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type X _diffrn_radiation_source Cu _diffrn_radiation_monochromator Graphite _diffrn_radiation_detector ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _reflns_number_total 3340 _reflns_number_gt 850 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 70 # REFINEMENT DATA _refine_special_details ; ...... ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_structure_factor_coef ? _refine_ls_matrix_type ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_extinction_method ? _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 850 _refine_ls_number_parameters 264 _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_ref 0.047 _refine_ls_goodness_of_fit_ref 1.415 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? _refine_diff_density_max ? _refine_diff_density_min ? _refine_diff_density_rms ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2'