#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012105.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2012105 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 861 _journal_page_last 864 _publ_section_title ; A series of three (E)-2-alkylidene-1,4-di-p-tosyl-1,2,3,4-tetrahydroquinoxaline compounds ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Banerjee, Surajit' 'Mukherjee, Alok K.' 'Mukhopadhyay, Rupa' 'Kundu, Nitya G.' 'Welch, Alan J.' _chemical_name_common '2-[(4-methoxyphenyl)methylidene]-1,4-di-p-tosyl-1,2,3,4-tetrahydroquinoxaline' _chemical_formula_moiety 'C30 H28 N2 O5 S2' _chemical_formula_sum 'C30 H28 N2 O5 S2' _chemical_formula_weight 560.66 _chemical_melting_point '425(1) K' _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5460(10) _cell_length_b 11.8440(10) _cell_length_c 21.985(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.250(10) _cell_angle_gamma 90.00 _cell_volume 2693.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _exptl_crystal_density_diffrn 1.383 _diffrn_ambient_temperature 293(2) 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol S2 -.17858(6) .02598(5) .10863(3) .02493(16) Uani d . 1 . . S S1 .30568(6) .25535(5) .15383(3) .02862(17) Uani d . 1 . . S O1 .31578(17) .32301(15) .10120(9) .0377(5) Uani d . 1 . . O O2 .36249(18) .29369(16) .21464(9) .0408(5) Uani d . 1 . . O O3 -.21816(17) -.03498(15) .15782(9) .0348(4) Uani d . 1 . . O O4 -.20330(16) -.01990(15) .04704(8) .0326(4) Uani d . 1 . . O O5 -.25420(18) .32024(16) -.19143(8) .0363(4) Uani d . 1 . . O N1 .14431(18) .24013(16) .15224(9) .0249(5) Uani d . 1 . . N N2 -.01757(18) .04089(16) .12811(9) .0231(4) Uani d . 1 . . N C1 .1100(2) .1757(2) .20220(11) .0258(5) Uani d . 1 . . C C2 .1488(2) .2125(2) .26324(12) .0332(6) Uani d . 1 . . C H2 .1927 .2807 .2711 .040 Uiso calc R 1 . . H C3 .1229(3) .1494(3) .31197(13) .0406(7) Uani d . 1 . . C H3 .1478 .1757 .3524 .049 Uiso calc R 1 . . H C4 .0595(3) .0464(3) .30073(13) .0429(7) Uani d . 1 . . C H4 .0459 .0019 .3337 .052 Uiso calc R 1 . . H C5 .0167(2) .0104(2) .24054(12) .0331(6) Uani d . 1 . . C H5 -.0256 -.0586 .2332 .040 Uiso calc R 1 . . H C6 .0362(2) .0763(2) .19036(11) .0245(5) Uani d . 1 . . C C7 .0426(2) .09252(19) .07916(11) .0232(5) Uani d . 1 . . C H7A -.0144 .0829 .0392 .028 Uiso calc R 1 . . H H7B .1233 .0541 .0778 .028 Uiso calc R 1 . . H C8 .0686(2) .2164(2) .09109(11) .0232(5) Uani d . 1 . . C C9 .0289(2) .3039(2) .05437(11) .0255(5) Uani d . 1 . . C H9 .0497 .3744 .0721 .031 Uiso calc R 1 . . H C10 -.0431(2) .3058(2) -.01015(11) .0237(5) Uani d . 1 . . C C11 -.1221(2) .3986(2) -.02959(12) .0263(5) Uani d . 1 . . C H11 -.1265 .4566 -.0016 .032 Uiso calc R 1 . . H C12 -.1946(2) .4071(2) -.08959(12) .0274(5) Uani d . 1 . . C H12 -.2464 .4699 -.1013 .033 Uiso calc R 1 . . H C13 -.1885(2) .3208(2) -.13162(11) .0274(5) Uani d . 1 . . C C14 -.1085(2) .2274(2) -.11357(12) .0295(6) Uani d . 1 . . C H14 -.1041 .1695 -.1417 .035 Uiso calc R 1 . . H C15 -.0363(2) .2211(2) -.05417(11) .0273(6) Uani d . 1 . . C H15 .0180 .1595 -.0430 .033 Uiso calc R 1 . . H C16 -.3261(3) .4203(3) -.21311(13) .0487(8) Uani d . 1 . . C H16A -.3660 .4110 -.2560 .073 Uiso calc R 1 . . H H16B -.2687 .4839 -.2088 .073 Uiso calc R 1 . . H H16C -.3916 .4327 -.1891 .073 Uiso calc R 1 . . H C17 .3652(2) .1192(2) .14378(11) .0248(5) Uani d . 1 . . C C18 .4030(2) .0912(2) .08884(12) .0304(6) Uani d . 1 . . C H18 .3954 .1432 .0567 .036 Uiso calc R 1 . . H C19 .4522(3) -.0156(2) .08263(12) .0324(6) Uani d . 1 . . C H19 .4796 -.0342 .0462 .039 Uiso calc R 1 . . H C20 .4618(2) -.0957(2) .12942(12) .0274(6) Uani d . 1 . . C C21 .4212(2) -.0662(2) .18368(12) .0301(6) Uani d . 1 . . C H21 .4259 -.1192 .2153 .036 Uiso calc R 1 . . H C22 .3740(2) .0406(2) .19149(12) .0298(6) Uani d . 1 . . C H22 .3484 .0598 .2283 .036 Uiso calc R 1 . . H C23 .5168(3) -.2112(2) .12197(13) .0374(7) Uani d . 1 . . C H23A .5635 -.2371 .1614 .056 Uiso calc R 1 . . H H23B .5742 -.2072 .0931 .056 Uiso calc R 1 . . H H23C .4477 -.2627 .1067 .056 Uiso calc R 1 . . H C24 -.2454(2) .1627(2) .10561(11) .0239(5) Uani d . 1 . . C C25 -.2422(2) .2221(2) .16034(12) .0291(6) Uani d . 1 . . C H25 -.2041 .1906 .1983 .035 Uiso calc R 1 . . H C26 -.2962(2) .3287(2) .15776(13) .0332(6) Uani d . 1 . . C H26 -.2943 .3687 .1943 .040 Uiso calc R 1 . . H C27 -.3536(2) .3773(2) .10133(13) .0302(6) Uani d . 1 . . C C28 -.3542(2) .3163(2) .04760(12) .0312(6) Uani d . 1 . . C H28 -.3922 .3478 .0097 .037 Uiso calc R 1 . . H C29 -.3000(2) .2097(2) .04868(12) .0273(5) Uani d . 1 . . C H29 -.3002 .1704 .0120 .033 Uiso calc R 1 . . H C30 -.4141(3) .4933(2) .09864(15) .0453(8) Uani d . 1 . . C H30A -.3846 .5316 .1373 .068 Uiso calc R 1 . . H H30B -.5065 .4861 .0914 .068 Uiso calc R 1 . . H H30C -.3898 .5358 .0656 .068 Uiso calc R 1 . . 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S2 .0197(3) .0190(3) .0336(3) .0001(2) -.0008(2) .0004(3) S1 .0208(3) .0201(3) .0417(4) -.0018(2) -.0019(3) -.0035(3) O1 .0274(9) .0240(9) .0599(13) -.0040(8) .0040(9) .0090(9) O2 .0291(10) .0347(11) .0523(12) -.0033(9) -.0075(9) -.0161(9) O3 .0258(9) .0294(10) .0476(11) -.0024(8) .0033(8) .0127(9) O4 .0268(9) .0260(9) .0408(11) -.0001(8) -.0038(8) -.0109(8) O5 .0394(10) .0382(11) .0283(10) .0095(9) -.0006(8) .0029(8) N1 .0200(10) .0211(10) .0314(11) -.0004(8) -.0010(8) -.0036(9) N2 .0194(10) .0210(10) .0273(11) .0008(8) .0007(8) .0005(8) C1 .0201(12) .0238(12) .0314(14) .0089(10) -.0001(10) -.0042(11) C2 .0275(13) .0336(14) .0347(15) .0119(11) -.0028(11) -.0081(12) C3 .0347(15) .0570(19) .0282(15) .0149(14) .0015(12) -.0062(14) C4 .0360(15) .061(2) .0320(15) .0116(15) .0059(12) .0111(14) C5 .0257(13) .0379(15) .0350(15) .0036(11) .0041(11) .0075(12) C6 .0201(11) .0257(12) .0260(13) .0063(10) .0002(10) -.0012(10) C7 .0228(12) .0190(12) .0262(13) .0003(10) .0007(10) -.0010(10) C8 .0179(11) .0227(12) .0276(13) -.0011(10) .0008(9) -.0029(10) C9 .0220(12) .0183(12) .0352(14) -.0014(10) .0031(10) -.0031(10) C10 .0209(11) .0195(12) .0305(13) -.0017(10) .0045(10) .0040(10) C11 .0272(12) .0191(12) .0329(14) -.0020(10) .0068(11) .0000(10) C12 .0234(12) .0220(12) .0367(14) .0042(10) .0056(11) .0064(11) C13 .0234(12) .0285(13) .0296(14) -.0001(10) .0036(10) .0045(11) C14 .0354(14) .0236(13) .0311(14) .0045(11) .0105(11) -.0003(11) C15 .0280(13) .0222(12) .0321(14) .0065(10) .0070(11) .0050(11) C16 .0510(19) .061(2) .0327(16) .0299(16) .0050(14) .0082(15) C17 .0169(11) .0234(12) .0310(13) .0005(10) -.0026(10) -.0024(10) C18 .0280(13) .0303(14) .0330(14) -.0008(11) .0065(11) .0067(11) C19 .0338(14) .0345(15) .0304(14) .0000(12) .0099(11) -.0018(12) C20 .0181(11) .0264(13) .0355(14) .0003(10) -.0005(10) -.0047(11) C21 .0291(13) .0320(14) .0264(13) .0064(11) -.0014(11) .0048(11) C22 .0270(13) .0348(14) .0260(13) .0082(11) .0014(10) .0012(11) C23 .0336(14) .0317(15) .0452(17) .0048(12) .0029(12) -.0074(13) C24 .0187(11) .0218(12) .0309(13) -.0012(9) .0045(10) -.0006(10) C25 .0263(12) .0334(14) .0278(13) .0012(11) .0051(10) .0027(11) C26 .0311(14) .0322(14) .0376(15) .0005(12) .0098(12) -.0073(12) C27 .0219(12) .0246(13) .0452(16) .0011(10) .0090(11) -.0027(12) C28 .0248(13) .0295(14) .0373(15) .0047(11) .0013(11) .0076(12) C29 .0247(12) .0263(13) .0300(13) .0029(10) .0033(10) -.0001(11) C30 .0379(16) .0303(15) .067(2) .0100(13) .0075(15) -.0043(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S2 O3 . 1.4286(19) yes S2 O4 . 1.4349(18) yes S2 N2 . 1.6776(19) yes S2 C24 . 1.762(2) yes S1 O2 . 1.428(2) yes S1 O1 . 1.428(2) yes S1 N1 . 1.705(2) yes S1 C17 . 1.760(2) yes O5 C13 . 1.361(3) no O5 C16 . 1.437(3) no N1 C1 . 1.440(3) no N1 C8 . 1.451(3) yes N2 C6 . 1.438(3) no N2 C7 . 1.484(3) yes C1 C2 . 1.394(3) no C1 C6 . 1.408(3) no C2 C3 . 1.377(4) no C2 H2 . .9300 no C3 C4 . 1.390(5) no C3 H3 . .9300 no C4 C5 . 1.380(4) no C4 H4 . .9300 no C5 C6 . 1.399(4) no C5 H5 . .9300 no C7 C8 . 1.506(3) yes C7 H7A . .9700 no C7 H7B . .9700 no C8 C9 . 1.330(3) yes C9 C10 . 1.473(3) no C9 H9 . .9300 no C10 C11 . 1.395(3) no C10 C15 . 1.405(3) no C11 C12 . 1.393(4) no C11 H11 . .9300 no C12 C13 . 1.387(4) no C12 H12 . .9300 no C13 C14 . 1.401(3) no C14 C15 . 1.380(3) no C14 H14 . .9300 no C15 H15 . .9300 no C16 H16A . .9600 no C16 H16B . .9600 no C16 H16C . .9600 no C17 C18 . 1.384(4) no C17 C22 . 1.392(3) no C18 C19 . 1.384(4) no C18 H18 . .9300 no C19 C20 . 1.389(4) no C19 H19 . .9300 no C20 C21 . 1.388(4) no C20 C23 . 1.507(3) no C21 C22 . 1.382(4) no C21 H21 . .9300 no C22 H22 . .9300 no C23 H23A . .9600 no C23 H23B . .9600 no C23 H23C . .9600 no C24 C29 . 1.388(3) no C24 C25 . 1.389(3) no C25 C26 . 1.381(4) no C25 H25 . .9300 no C26 C27 . 1.394(4) no C26 H26 . .9300 no C27 C28 . 1.384(4) no C27 C30 . 1.511(4) no C28 C29 . 1.384(4) no C28 H28 . .9300 no C29 H29 . .9300 no C30 H30A . .9600 no C30 H30B . .9600 no C30 H30C . .9600 no