#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2011699.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_2011699 _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 H24 O3 S' _chemical_formula_sum 'C19 H24 O3 S' _chemical_formula_weight 332.44 _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 10.369(2) _cell_length_b 20.791(3) _cell_length_c 8.071(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1740.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _exptl_crystal_density_diffrn 1.269 _diffrn_ambient_temperature 170(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 .93535(13) .19996(7) .76797(19) .0381(3) Uani d . 1 . . S O1 .9410(3) .09980(18) .9678(4) .0359(9) Uani d . 1 . . O O2 1.4073(3) .1698(2) .4511(5) .0416(10) Uani d . 1 . . O O3 1.2621(4) .2080(2) .2721(7) .0625(13) Uani d . 1 . . O C1 .8669(12) .2086(6) .9739(14) .048(4) Uani d P .58(2) A 1 C H1A .8865 .2514 1.0210 .058 Uiso calc PR .58(2) A 1 H H1B .7723 .2023 .9720 .058 Uiso calc PR .58(2) A 1 H C1* .9642(19) .2133(7) .9860(18) .043(5) Uani d P .42(2) A 2 C H1*1 1.0561 .2240 1.0050 .051 Uiso calc PR .42(2) A 2 H H1*2 .9107 .2494 1.0265 .051 Uiso calc PR .42(2) A 2 H C2 .9318(6) .1565(3) 1.0699(7) .0497(16) Uani d . 1 A . C H2A 1.0191 .1707 1.1037 .060 Uiso calc R 1 B 1 H H2B .8816 .1468 1.1712 .060 Uiso calc R 1 B 1 H C3 .9849(5) .1142(2) .8052(6) .0253(12) Uani d . 1 A . C C4 1.1324(4) .1093(2) .7915(6) .0242(11) Uani d . 1 . . C C5 1.1871(5) .1132(3) .6168(6) .0270(12) Uani d . 1 A . C H5 1.2770 .0958 .6216 .032 Uiso calc R 1 . . H C6 1.1108(5) .0698(3) .4980(7) .0320(12) Uani d . 1 . . C H6A 1.1405 .0778 .3832 .038 Uiso calc R 1 A . H H6B 1.1292 .0243 .5248 .038 Uiso calc R 1 . . H C7 .9653(5) .0810(3) .5070(7) .0382(14) Uani d . 1 A . C H7A .9206 .0509 .4312 .046 Uiso calc R 1 . . H H7B .9451 .1255 .4716 .046 Uiso calc R 1 . . H C8 .9177(5) .0703(3) .6857(7) .0351(13) Uani d . 1 . . C H8A .8236 .0781 .6908 .042 Uiso calc R 1 A . H H8B .9335 .0251 .7181 .042 Uiso calc R 1 . . H C9 1.2005(5) .0950(2) .9241(7) .0301(13) Uani d . 1 A . C H9 1.1525 .0905 1.0237 .036 Uiso calc R 1 . . H C10 1.3436(5) .0846(2) .9401(7) .0297(11) Uani d . 1 . . C C11 1.3869(5) .0379(3) 1.0489(8) .0412(14) Uani d . 1 A . C H11 1.3265 .0130 1.1100 .049 Uiso calc R 1 . . H C12 1.5183(5) .0271(3) 1.0690(8) .0450(16) Uani d . 1 . . C H12 1.5468 -.0054 1.1432 .054 Uiso calc R 1 A . H C13 1.6062(5) .0623(3) .9845(8) .0434(15) Uani d . 1 A . C H13 1.6958 .0544 .9987 .052 Uiso calc R 1 . . H C14 1.5649(5) .1092(3) .8785(7) .0363(13) Uani d . 1 . . C H14 1.6264 .1342 .8197 .044 Uiso calc R 1 A . H C15 1.4332(5) .1210(2) .8552(6) .0301(11) Uani d . 1 A . C H15 1.4057 .1539 .7815 .036 Uiso calc R 1 . . H C16 1.1965(5) .1821(3) .5509(6) .0324(12) Uani d . 1 . . C H16A 1.1098 .1964 .5149 .039 Uiso calc R 1 A . H H16B 1.2246 .2108 .6419 .039 Uiso calc R 1 . . H C17 1.2895(5) .1891(3) .4068(7) .0341(13) Uani d . 1 A . C C18 1.5085(5) .1752(3) .3257(7) .0379(13) Uani d . 1 . . C H18A 1.5249 .2208 .2983 .045 Uiso calc R 1 . . H H18B 1.4832 .1522 .2233 .045 Uiso calc R 1 . . H C19 1.6257(6) .1451(3) .4004(9) .0540(18) Uani d . 1 . . C H19A 1.6477 .1675 .5034 .081 Uiso calc R 1 . . H H19B 1.6979 .1484 .3225 .081 Uiso calc R 1 . . H H19C 1.6084 .0997 .4244 .081 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 .0411(7) .0432(7) .0301(6) .0125(7) .0059(9) .0007(7) O1 .0305(19) .053(2) .0245(19) -.0032(18) .0058(18) .0061(18) O2 .032(2) .068(3) .025(2) .0022(19) .0057(17) .010(2) O3 .045(2) .110(4) .032(2) .016(2) .011(3) .031(3) C1 .032(7) .071(8) .042(6) .002(5) .007(5) -.020(6) C1* .060(13) .036(9) .032(8) -.002(7) -.005(8) -.005(6) C2 .049(4) .073(4) .027(3) .001(4) .006(3) -.008(3) C3 .024(2) .026(3) .026(3) .002(2) .002(2) .006(2) C4 .029(2) .018(2) .026(3) .0025(19) .002(2) .002(2) C5 .025(3) .040(3) .016(2) .002(2) .003(2) .001(2) C6 .036(3) .034(3) .026(3) -.001(2) .003(2) -.005(2) C7 .036(3) .050(4) .029(3) -.007(3) -.006(3) -.008(3) C8 .026(3) .045(3) .035(3) -.003(3) .006(2) -.005(3) C9 .025(3) .036(3) .029(3) -.002(2) .007(2) .000(2) C10 .030(3) .034(3) .026(3) .003(2) -.003(2) .001(2) C11 .037(3) .047(3) .040(3) -.004(3) -.005(3) .005(3) C12 .042(3) .050(4) .043(4) .007(3) -.012(3) .016(3) C13 .023(2) .059(4) .048(4) .010(3) -.004(3) -.008(3) C14 .029(3) .046(3) .034(3) -.002(3) .003(3) -.005(3) C15 .030(3) .035(3) .026(3) -.003(2) -.008(2) -.001(2) C16 .029(3) .046(3) .023(3) .000(2) .004(2) .004(2) C17 .029(3) .046(4) .027(3) .000(2) .005(2) .003(3) C18 .037(3) .053(3) .024(3) -.006(3) .010(2) .007(3) C19 .038(3) .081(5) .043(4) .005(3) .007(3) .006(4) 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 C1* . 1.806(14) y S1 C1 . 1.816(11) y S1 C3 . 1.880(5) y O1 C3 . 1.421(6) y O1 C2 . 1.442(7) y O2 C17 . 1.335(6) y O2 C18 . 1.462(6) y O3 C17 . 1.191(7) y C1 C2 . 1.491(13) n C1 H1A . .9900 n C1 H1B . .9900 n C1* C2 . 1.401(15) n C1* H1*1 . .9900 n C1* H1*2 . .9900 n C2 H2A . .9900 n C2 H2B . .9900 n C3 C8 . 1.499(7) n C3 C4 . 1.537(6) n C4 C9 . 1.317(7) n C4 C5 . 1.522(7) n C5 C16 . 1.532(7) n C5 C6 . 1.536(7) n C5 H5 . 1.0000 n C6 C7 . 1.528(7) n C6 H6A . .9900 n C6 H6B . .9900 n C7 C8 . 1.541(8) n C7 H7A . .9900 n C7 H7B . .9900 n C8 H8A . .9900 n C8 H8B . .9900 n C9 C10 . 1.506(7) n C9 H9 . .9500 n C10 C15 . 1.381(7) n C10 C11 . 1.385(8) n C11 C12 . 1.390(8) n C11 H11 . .9500 n C12 C13 . 1.352(8) n C12 H12 . .9500 n C13 C14 . 1.366(8) n C13 H13 . .9500 n C14 C15 . 1.400(7) n C14 H14 . .9500 n C15 H15 . .9500 n C16 C17 . 1.517(7) n C16 H16A . .9900 n C16 H16B . .9900 n C18 C19 . 1.493(8) n C18 H18A . .9900 n C18 H18B . .9900 n C19 H19A . .9800 n C19 H19B . .9800 n C19 H19C . .9800 n