#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012104.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_2012104 _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-methylphenyl)methylidene]-1,4-di-p-tosyl-1,2,3,4-tetrahydroquinoxaline' _chemical_formula_moiety 'C30 H28 N2 O4 S2' _chemical_formula_sum 'C30 H28 N2 O4 S2' _chemical_formula_weight 544.66 _chemical_melting_point '428(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 10.559(4) _cell_length_b 11.658(4) _cell_length_c 23.169(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.54(3) _cell_angle_gamma 90.00 _cell_volume 2803.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.290 _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 S1 .30086(6) .25747(5) .15874(4) .0788(2) Uani d . 1 . . S N1 .14136(17) .23239(15) .15816(9) .0638(5) Uani d . 1 . . N O1 .30516(18) .33353(16) .11065(12) .1101(8) Uani d . 1 . . O O2 .35635(19) .2907(2) .21676(11) .1189(9) Uani d . 1 . . O S2 -.18201(5) .01590(5) .11171(3) .06174(19) Uani d . 1 . . S N2 -.02264(16) .03468(14) .13007(8) .0548(4) Uani d . 1 . . N O3 -.21918(16) -.05499(16) .15587(9) .0875(6) Uani d . 1 . . O O4 -.20392(16) -.02169(14) .05199(8) .0783(5) Uani d . 1 . . O C1 .1090(2) .1597(2) .20364(10) .0628(6) Uani d . 1 . . C C2 .1501(3) .1889(3) .26257(13) .0868(9) Uani d . 1 . . C H2 .1956 .2566 .2722 .104 Uiso calc R 1 . . H C3 .1239(3) .1186(4) .30619(14) .1105(12) Uani d . 1 . . C H3 .1504 .1396 .3453 .133 Uiso calc R 1 . . H C4 .0584(3) .0169(4) .29266(14) .1076(11) Uani d . 1 . . C H4 .0454 -.0325 .3225 .129 Uiso calc R 1 . . H C5 .0122(3) -.0115(3) .23484(12) .0822(8) Uani d . 1 . . C H5 -.0328 -.0797 .2259 .099 Uiso calc R 1 . . H C6 .0326(2) .0615(2) .18956(10) .0593(5) Uani d . 1 . . C C7 .0387(2) .09056(17) .08535(10) .0561(5) Uani d . 1 . . C H7A -.0179 .0853 .0474 .067 Uiso calc R 1 . . H H7B .1183 .0510 .0827 .067 Uiso calc R 1 . . H C8 .06717(19) .21462(17) .10031(10) .0557(5) Uani d . 1 . . C C9 .0305(2) .30615(18) .06680(11) .0638(6) Uani d . 1 . . C H9 .0497 .3769 .0848 .077 Uiso calc R 1 . . H C10 -.0360(2) .31014(18) .00546(11) .0622(6) Uani d . 1 . . C C11 -.0157(3) .2325(2) -.03727(12) .0813(8) Uani d . 1 . . C H11 .0436 .1735 -.0274 .098 Uiso calc R 1 . . H C12 -.0820(4) .2414(3) -.09396(13) .0945(9) Uani d . 1 . . C H12 -.0670 .1878 -.1217 .113 Uiso calc R 1 . . H C13 -.1707(3) .3282(3) -.11085(12) .0834(8) Uani d . 1 . . C C14 -.1890(3) .4070(2) -.06887(13) .0768(7) Uani d . 1 . . C H14 -.2474 .4666 -.0791 .092 Uiso calc R 1 . . H C15 -.1227(2) .39927(19) -.01235(12) .0686(6) Uani d . 1 . . C H15 -.1357 .4547 .0148 .082 Uiso calc R 1 . . H C16 -.2420(4) .3373(4) -.17354(13) .1192(12) Uani d . 1 . . C H16A -.1909 .3037 -.1994 .179 Uiso calc R 1 . . H H16B -.2577 .4165 -.1836 .179 Uiso calc R 1 . . H H16C -.3226 .2973 -.1774 .179 Uiso calc R 1 . . H C17 .36745(19) .12593(19) .14356(10) .0576(5) Uani d . 1 . . C C18 .4110(2) .0497(2) .18827(11) .0711(6) Uani d . 1 . . C H18 .4082 .0689 .2270 .085 Uiso calc R 1 . . H C19 .4583(3) -.0543(2) .17511(13) .0787(7) Uani d . 1 . . C H19 .4873 -.1056 .2054 .094 Uiso calc R 1 . . H C20 .4644(2) -.0855(2) .11845(13) .0708(7) Uani d . 1 . . C C21 .4215(2) -.0086(2) .07457(12) .0749(7) Uani d . 1 . . C H21 .4251 -.0280 .0360 .090 Uiso calc R 1 . . H C22 .3731(2) .0970(2) .08624(11) .0686(6) Uani d . 1 . . C H22 .3446 .1483 .0559 .082 Uiso calc R 1 . . H C23 .5167(3) -.2009(3) .10473(18) .1132(12) Uani d . 1 . . C H23A .5571 -.2373 .1406 .170 Uiso calc R 1 . . H H23B .5789 -.1906 .0797 .170 Uiso calc R 1 . . H H23C .4475 -.2481 .0852 .170 Uiso calc R 1 . . H C24 -.25481(19) .15097(19) .11401(10) .0572(5) Uani d . 1 . . C C25 -.2946(2) .2117(2) .06328(11) .0696(6) Uani d . 1 . . C H25 -.2838 .1819 .0273 .084 Uiso calc R 1 . . H C26 -.3511(2) .3180(2) .06639(14) .0798(7) Uani d . 1 . . C H26 -.3788 .3589 .0319 .096 Uiso calc R 1 . . H C27 -.3675(2) .3649(2) .11888(16) .0812(8) Uani d . 1 . . C C28 -.3270(3) .3020(3) .16894(15) .0987(10) Uani d . 1 . . C H28 -.3367 .3323 .2050 .118 Uiso calc R 1 . . H C29 -.2722(3) .1950(3) .16707(12) .0840(8) Uani d . 1 . . C H29 -.2473 .1530 .2014 .101 Uiso calc R 1 . . H C30 -.4278(3) .4826(2) .1217(2) .1225(14) Uani d . 1 . . C H30A -.4716 .5044 .0832 .184 Uiso calc R 1 . . H H30B -.3617 .5376 .1357 .184 Uiso calc R 1 . . H H30C -.4883 .4802 .1480 .184 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 S1 .0496(3) .0506(3) .1297(6) -.0030(3) -.0005(3) -.0133(4) N1 .0488(10) .0500(10) .0879(13) .0041(8) .0004(9) -.0115(10) O1 .0652(11) .0557(10) .208(2) -.0022(8) .0202(13) .0383(13) O2 .0637(11) .1138(16) .167(2) -.0072(11) -.0120(12) -.0788(16) S2 .0455(3) .0496(3) .0859(4) -.0014(2) .0009(3) .0042(3) N2 .0453(9) .0484(9) .0682(11) .0009(7) .0037(8) .0032(8) O3 .0571(10) .0759(11) .1266(15) -.0089(8) .0090(10) .0376(11) O4 .0651(10) .0660(10) .0942(12) .0022(8) -.0107(9) -.0255(9) C1 .0485(12) .0615(13) .0738(15) .0158(10) -.0007(10) -.0098(12) C2 .0697(16) .097(2) .0852(19) .0249(15) -.0079(14) -.0256(17) C3 .094(2) .161(4) .0707(19) .041(2) -.0014(17) -.011(2) C4 .087(2) .158(4) .077(2) .022(2) .0107(16) .024(2) C5 .0634(15) .099(2) .0811(18) .0086(14) .0062(13) .0202(16) C6 .0448(11) .0621(13) .0689(14) .0130(10) .0053(10) .0018(11) C7 .0511(11) .0451(11) .0709(13) .0002(9) .0081(10) -.0016(10) C8 .0457(11) .0456(11) .0746(14) .0012(9) .0082(10) -.0034(10) C9 .0569(13) .0430(11) .0928(17) .0030(10) .0173(12) .0004(11) C10 .0630(13) .0457(11) .0811(15) .0022(10) .0216(12) .0091(11) C11 .103(2) .0639(15) .0847(18) .0247(14) .0369(16) .0159(14) C12 .136(3) .0761(18) .0794(19) .0126(18) .0405(18) .0097(15) C13 .096(2) .0749(17) .0808(17) -.0080(15) .0207(15) .0211(15) C14 .0700(15) .0600(15) .100(2) .0043(12) .0138(14) .0225(14) C15 .0670(14) .0452(12) .0950(18) .0015(11) .0187(13) .0066(12) C16 .135(3) .134(3) .084(2) -.016(2) .008(2) .026(2) C17 .0415(11) .0552(12) .0718(14) -.0002(9) -.0013(10) .0017(11) C18 .0680(15) .0767(16) .0631(14) .0133(13) -.0022(11) .0047(12) C19 .0709(16) .0693(16) .0904(19) .0158(13) .0003(13) .0224(14) C20 .0464(12) .0608(14) .104(2) -.0007(11) .0095(12) -.0074(14) C21 .0590(14) .0906(19) .0753(16) .0020(13) .0126(12) -.0143(15) C22 .0563(13) .0786(16) .0684(15) .0013(12) .0046(11) .0167(13) C23 .0759(18) .0706(18) .192(4) .0041(15) .022(2) -.032(2) C24 .0405(11) .0578(12) .0713(14) .0021(9) .0053(10) .0020(11) C25 .0626(14) .0661(14) .0788(16) .0094(12) .0092(12) .0049(13) C26 .0631(15) .0665(16) .108(2) .0090(12) .0105(14) .0177(15) C27 .0462(13) .0610(15) .136(3) .0024(11) .0147(14) -.0119(17) C28 .088(2) .103(2) .105(2) .0233(18) .0190(17) -.0307(19) C29 .0805(18) .098(2) .0742(17) .0228(16) .0149(13) -.0001(15) C30 .0707(18) .0667(17) .227(4) .0082(15) .018(2) -.027(2) 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 S1 O2 . 1.419(2) yes S1 O1 . 1.431(2) yes S1 N1 . 1.707(2) yes S1 C17 . 1.749(2) yes N1 C8 . 1.439(3) yes N1 C1 . 1.441(3) no S2 O3 . 1.4250(18) yes S2 O4 . 1.4293(18) yes S2 N2 . 1.6729(18) yes S2 C24 . 1.757(2) yes N2 C6 . 1.430(3) no N2 C7 . 1.471(3) yes C1 C2 . 1.397(4) no C1 C6 . 1.405(3) no C2 C3 . 1.368(5) no C2 H2 . .9300 no C3 C4 . 1.379(5) no C3 H3 . .9300 no C4 C5 . 1.380(4) no C4 H4 . .9300 no C5 C6 . 1.398(3) no C5 H5 . .9300 no C7 C8 . 1.505(3) yes C7 H7A . .9700 no C7 H7B . .9700 no C8 C9 . 1.335(3) yes C9 C10 . 1.466(3) no C9 H9 . .9300 no C10 C11 . 1.387(3) no C10 C15 . 1.396(3) no C11 C12 . 1.374(4) no C11 H11 . .9300 no C12 C13 . 1.386(4) no C12 H12 . .9300 no C13 C14 . 1.378(4) no C13 C16 . 1.512(4) no C14 C15 . 1.370(4) no C14 H14 . .9300 no C15 H15 . .9300 no C16 H16A . .9600 no C16 H16B . .9600 no C16 H16C . .9600 no C17 C18 . 1.378(3) no C17 C22 . 1.382(3) no C18 C19 . 1.368(4) no C18 H18 . .9300 no C19 C20 . 1.375(4) no C19 H19 . .9300 no C20 C21 . 1.370(4) no C20 C23 . 1.510(4) no C21 C22 . 1.378(4) no C21 H21 . .9300 no C22 H22 . .9300 no C23 H23A . .9600 no C23 H23B . .9600 no C23 H23C . .9600 no C24 C25 . 1.371(3) no C24 C29 . 1.375(3) no C25 C26 . 1.383(4) no C25 H25 . .9300 no C26 C27 . 1.373(4) no C26 H26 . .9300 no C27 C28 . 1.373(4) no C27 C30 . 1.519(4) no C28 C29 . 1.378(4) no C28 H28 . .9300 no C29 H29 . .9300 no C30 H30A . .9600 no C30 H30B . .9600 no C30 H30C . .9600 no