#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007297.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_2007297 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 832 _journal_page_last 834 _publ_section_title ; (4S,6S,11R)-(+)-2-N-Benzylmethylamino-4,6-dimethyl-1,3,2-dioxa- phosphorinane ; loop_ _publ_author_name 'Hommer, Herbert' "Dom\'inguez, Zaira" "Gordillo, B\'arbara" _chemical_name_common ; (2R,4S,6S)-(+)-2-N-benzylmethyl-amino-2-thio-4,6- dimethyl-1,3,2-dioxaphosphorinane ; _chemical_formula_moiety 'C13 H20 N O2 P S' _chemical_formula_sum 'C13 H20 N O2 P S' _chemical_formula_weight 285.33 _chemical_melting_point 87-89\%C _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_space_group_name_Hall 'P 31 2" ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.9210(10) _cell_length_b 9.9210(10) _cell_length_c 26.880(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2291.2(5) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.24 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .037 _refine_ls_wR_factor_obs .106 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol P2 -.00522(12) .71065(12) .01895(3) .0465(3) Uani d . 1 . P S9 -.18699(14) .61719(14) .06111(4) .0639(3) Uani d . 1 . S N10 -.0355(4) .7715(4) -.03305(11) .0522(8) Uani d . 1 . N H10 -.115(6) .769(6) -.0367(16) .078 Uiso d . 1 . H O1 .0592(3) .5995(3) .00250(9) .0535(7) Uani d . 1 . O O3 .1430(3) .8568(3) .04171(9) .0547(7) Uani d . 1 . O C4 .2561(5) .8417(5) .07329(13) .0615(11) Uani d . 1 . C H4A .3498 .9447 .07540 .092 Uiso calc R 1 . H C5 .3012(5) .7346(5) .0483(2) .0587(11) Uani d . 1 . C H5A .3705 .7197 .0701 .088 Uiso calc R 1 . H H5B .3585 .7842 .0182 .088 Uiso calc R 1 . H C6 .1646(5) .5766(5) .03493(13) .0529(10) Uani d . 1 . C H6A .1095 .5222 .06528 .079 Uiso calc R 1 . H C7 .1915(6) .7942(6) .12595(13) .080(2) Uani d . 1 . C H7A .1586 .8642 .1381 .121 Uiso calc R 1 . H H7B .2709 .7983 .1474 .121 Uiso calc R 1 . H H7C .1043 .6901 .1255 .121 Uiso calc R 1 . H C8 .2123(6) .4762(6) .0061(2) .0732(13) Uani d . 1 . C H8A .1223 .3764 -.0002 .110 Uiso calc R 1 . H H8B .2866 .4627 .0251 .110 Uiso calc R 1 . H H8C .2581 .5257 -.0250 .110 Uiso calc R 1 . H C11 .0852(5) .8530(5) -.07163(13) .0531(10) Uani d . 1 . C H11 .179(6) .867(6) -.0579(16) .080 Uiso d . 1 . H C12 .1017(6) 1.0093(6) -.0836(2) .0755(14) Uani d . 1 . C H12A .1844 1.0628 -.1072 .113 Uiso calc R 1 . H H12B .1252 1.0700 -.0538 .113 Uiso calc R 1 . H H12C .0061 .9944 -.0976 .113 Uiso calc R 1 . H C13 .0517(5) .7544(5) -.11794(12) .0507(9) Uani d . 1 . C C14 -.0877(5) .6966(6) -.14306(15) .0676(13) Uani d . 1 . C H14A -.1650 .7138 -.13040 .081 Uiso calc R 1 . H C15 -.1140(7) .6143(7) -.1863(2) .089(2) Uani d . 1 . C H15A -.2082 .5777 -.2029 .106 Uiso calc R 1 . H C16 -.0054(10) .5856(7) -.2052(2) .100(2) Uani d . 1 . C H16A -.0246 .5292 -.2345 .120 Uiso calc R 1 . H C17 .1326(9) .6393(8) -.1811(2) .103(2) Uani d . 1 . C H17A .2078 .6193 -.1941 .124 Uiso calc R 1 . H C18 .1623(7) .7241(7) -.1371(2) .082(2) Uani d . 1 . C H18A .2567 .7600 -.1207 .099 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 P2 .0483(6) .0464(6) .0388(4) .0192(5) .0013(4) -.0027(4) S9 .0601(7) .0644(7) .0533(5) .0208(6) .0162(5) .0049(5) N10 .046(2) .068(2) .042(2) .027(2) .0062(15) .005(2) O1 .055(2) .053(2) .0524(13) .0262(15) -.0067(12) -.0067(12) O3 .059(2) .048(2) .0485(13) .0202(14) -.0045(13) -.0045(13) C4 .061(3) .058(3) .048(2) .017(2) -.013(2) -.006(2) C5 .044(2) .063(3) .060(2) .020(2) -.006(2) .004(2) C6 .052(2) .052(2) .050(2) .022(2) -.002(2) .006(2) C7 .095(4) .098(4) .042(2) .044(3) -.014(2) -.008(2) C8 .069(3) .068(3) .089(3) .039(3) -.005(3) -.005(3) C11 .049(2) .066(3) .045(2) .030(2) .001(2) .006(2) C12 .093(4) .062(3) .064(3) .033(3) .012(3) .004(2) C13 .057(2) .053(2) .047(2) .031(2) .012(2) .014(2) C14 .064(3) .077(3) .053(2) .029(2) .004(2) .002(2) C15 .089(4) .079(4) .059(3) .012(3) .004(3) -.004(3) C16 .158(7) .065(3) .064(3) .045(4) .027(4) -.001(3) C17 .159(7) .120(6) .077(3) .104(6) .049(4) .018(4) C18 .092(4) .113(5) .071(3) .074(4) .019(3) .012(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 P2 O3 . 1.583(3) yes P2 O1 . 1.589(3) yes P2 N10 . 1.609(3) yes P2 S9 . 1.9300(10) yes N10 H10 . .78(5) yes N10 C11 . 1.481(5) yes O1 C6 . 1.464(5) yes O3 C4 . 1.474(5) yes C4 C5 . 1.502(6) yes C4 C7 . 1.528(5) yes C5 C6 . 1.516(6) yes C6 C8 . 1.513(6) yes C11 H11 . .95(5) yes C11 C12 . 1.510(6) yes C11 C13 . 1.514(5) yes C13 C18 . 1.374(6) yes C13 C14 . 1.380(6) yes C14 C15 . 1.370(7) yes C15 C16 . 1.343(8) yes C16 C17 . 1.359(9) yes C17 C18 . 1.396(8) yes