#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2011700.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_2011700 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 79 _journal_page_last 81 _publ_section_title ; Johnson orthoester Claisen rearrangement products of some (1-oxa-4-thiaspiro[4.5]dec-6-en-6-yl)alkanols ; loop_ _publ_author_name 'Parvez, Masood' 'Yadav, Veejendra K.' 'Senthil, Govindaraji' _chemical_name_common ; 1-Oxa-4-thiaspiro[4.5]decane ; _chemical_formula_moiety 'C19 H23 Br O3 S' _chemical_formula_sum 'C19 H23 Br O3 S' _chemical_formula_weight 411.34 _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.243(2) _cell_length_b 11.5410(10) _cell_length_c 22.180(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.09(2) _cell_angle_gamma 90.00 _cell_volume 1849.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.477 _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 Br1 1.21939(9) -.37684(6) -.32880(3) .0713(3) Uani d . 1 . . Br S1 -.2539(2) -.36685(12) -.04414(6) .0555(4) Uani d . 1 . . S O1 -.1207(5) -.2545(3) .05246(16) .0561(10) Uani d . 1 . . O O2 .4492(5) -.3296(3) -.17692(14) .0468(9) Uani d . 1 . . O O3 .4897(6) -.5198(3) -.16423(19) .0669(11) Uani d . 1 . . O C1 -.2675(10) -.4330(6) .0288(3) .0734(19) Uani d . 1 . . C H1A -.3885 -.4208 .0439 .088 Uiso calc R 1 . . H H1B -.2439 -.5156 .0269 .088 Uiso calc R 1 . . H C2 -.1219(11) -.3739(6) .0675(3) .0740(19) Uani d . 1 . . C H2A -.1458 -.3833 .1097 .089 Uiso calc R 1 . . H H2B -.0023 -.4079 .0613 .089 Uiso calc R 1 . . H C3 -.1267(7) -.2373(4) -.0112(2) .0428(11) Uani d . 1 . . C C4 .0595(6) -.2278(4) -.0373(2) .0383(11) Uani d . 1 . . C C5 .0341(7) -.2095(4) -.1055(2) .0425(11) Uani d . 1 . . C H5 -.0458 -.2723 -.1217 .051 Uiso calc R 1 . . H C6 -.0726(7) -.0961(5) -.1178(3) .0529(13) Uani d . 1 . . C H6A -.0007 -.0319 -.1004 .063 Uiso calc R 1 . . H H6B -.0903 -.0836 -.1611 .063 Uiso calc R 1 . . H C7 -.2558(7) -.0993(5) -.0916(3) .0585(15) Uani d . 1 . . C H7A -.3328 -.1577 -.1123 .070 Uiso calc R 1 . . H H7B -.3165 -.0249 -.0979 .070 Uiso calc R 1 . . H C8 -.2376(7) -.1266(5) -.0239(3) .0533(13) Uani d . 1 . . C H8A -.1766 -.0625 -.0023 .064 Uiso calc R 1 . . H H8B -.3599 -.1354 -.0093 .064 Uiso calc R 1 . . H C9 .2215(7) -.2251(5) -.0066(2) .0486(12) Uani d . 1 . . C H9 .3210 -.2182 -.0306 .058 Uiso calc R 1 . . H C10 .2766(9) -.2311(6) .0602(2) .0687(18) Uani d . 1 . . C H10A .4088 -.2256 .0666 .103 Uiso calc R 1 . . H H10B .2358 -.3034 .0760 .103 Uiso calc R 1 . . H H10C .2202 -.1682 .0804 .103 Uiso calc R 1 . . H C11 .2104(7) -.2135(5) -.1396(2) .0460(12) Uani d . 1 . . C H11A .1821 -.1871 -.1807 .055 Uiso calc R 1 . . H H11B .3012 -.1610 -.1204 .055 Uiso calc R 1 . . H C12 .2925(7) -.3342(5) -.1409(2) .0497(13) Uani d . 1 . . C H12A .3307 -.3595 -.1002 .060 Uiso calc R 1 . . H H12B .2014 -.3885 -.1583 .060 Uiso calc R 1 . . H C13 .5375(7) -.4287(5) -.1841(2) .0467(12) Uani d . 1 . . C C14 .7036(7) -.4138(4) -.2188(2) .0421(11) Uani d . 1 . . C C15 .8280(8) -.5035(5) -.2202(2) .0549(14) Uani d . 1 . . C H15 .8072 -.5710 -.1988 .066 Uiso calc R 1 . . H C16 .9834(8) -.4955(5) -.2526(3) .0600(15) Uani d . 1 . . C H16 1.0662 -.5569 -.2541 .072 Uiso calc R 1 . . H C17 1.0120(8) -.3923(5) -.2832(2) .0500(13) Uani d . 1 . . C C18 .8921(8) -.3003(5) -.2806(2) .0565(14) Uani d . 1 . . C H18 .9149 -.2311 -.3003 .068 Uiso calc R 1 . . H C19 .7390(7) -.3127(5) -.2487(2) .0531(14) Uani d . 1 . . C H19 .6565 -.2512 -.2472 .064 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 Br1 .0631(4) .0805(5) .0740(5) .0032(4) .0311(3) -.0040(4) S1 .0572(8) .0511(8) .0589(8) -.0150(7) .0081(6) .0042(7) O1 .066(2) .062(2) .044(2) .001(2) .0207(18) -.0003(17) O2 .054(2) .046(2) .0434(18) -.0013(17) .0222(16) .0017(15) O3 .081(3) .043(2) .082(3) -.009(2) .035(2) -.002(2) C1 .092(5) .061(4) .071(4) -.008(4) .027(4) .015(3) C2 .100(5) .073(4) .051(3) .011(4) .014(3) .017(3) C3 .043(3) .048(3) .038(3) -.003(2) .009(2) -.002(2) C4 .040(3) .038(3) .037(2) .000(2) .006(2) .001(2) C5 .040(3) .048(3) .039(3) -.008(2) .002(2) .003(2) C6 .053(3) .052(3) .054(3) .000(3) .004(3) .013(3) C7 .045(3) .052(3) .077(4) .005(3) .002(3) .014(3) C8 .047(3) .048(3) .067(3) .003(3) .013(3) .000(3) C9 .046(3) .056(3) .043(3) -.005(2) .000(2) -.005(2) C10 .063(4) .094(5) .047(3) .004(4) -.009(3) -.005(3) C11 .048(3) .051(3) .040(3) -.002(2) .011(2) .004(2) C12 .051(3) .056(3) .044(3) -.010(3) .018(2) -.001(2) C13 .058(3) .043(3) .041(3) -.009(2) .011(2) -.003(2) C14 .050(3) .042(3) .035(2) -.001(2) .008(2) -.007(2) C15 .067(4) .038(3) .061(3) -.001(3) .016(3) -.003(3) C16 .062(4) .050(3) .070(4) .007(3) .018(3) -.009(3) C17 .062(3) .053(3) .035(3) .003(3) .005(2) -.008(2) C18 .072(4) .050(3) .050(3) .011(3) .017(3) .013(3) C19 .055(3) .055(3) .053(3) .014(3) .026(3) .010(3) 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 Br1 C17 . 1.878(5) y S1 C1 . 1.798(6) y S1 C3 . 1.876(5) y O1 C2 . 1.418(7) y O1 C3 . 1.423(6) y O2 C13 . 1.325(6) y O2 C12 . 1.434(5) y O3 C13 . 1.201(6) y C1 C2 . 1.478(9) n C1 H1A . .9700 n C1 H1B . .9700 n C2 H2A . .9700 n C2 H2B . .9700 n C3 C4 . 1.509(6) n C3 C8 . 1.525(7) n C4 C9 . 1.314(7) n C4 C5 . 1.525(6) n C5 C11 . 1.530(6) n C5 C6 . 1.534(7) n C5 H5 . .9800 n C6 C7 . 1.487(7) n C6 H6A . .9700 n C6 H6B . .9700 n C7 C8 . 1.531(8) n C7 H7A . .9700 n C7 H7B . .9700 n C8 H8A . .9700 n C8 H8B . .9700 n C9 C10 . 1.507(7) n C9 H9 . .9300 n C10 H10A . .9600 n C10 H10B . .9600 n C10 H10C . .9600 n C11 C12 . 1.516(7) n C11 H11A . .9700 n C11 H11B . .9700 n C12 H12A . .9700 n C12 H12B . .9700 n C13 C14 . 1.484(7) n C14 C15 . 1.374(7) n C14 C19 . 1.376(7) n C15 C16 . 1.382(7) n C15 H15 . .9300 n C16 C17 . 1.393(8) n C16 H16 . .9300 n C17 C18 . 1.375(7) n C18 C19 . 1.365(7) n C18 H18 . .9300 n C19 H19 . .9300 n