#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012510.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_2012510 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first o108 _journal_page_last o111 _publ_section_title ; New electron-deficient chiral phosphines: synthesis and structure of [(4R,5R)-1,3-bis(trifluoromethanesulfonyl)perhydro-1,3,2-benzodiazaphosphol- 2-yl] substituted amines ; loop_ _publ_author_name "Konya, Den\'es" 'Philouze, Christian' 'Gimbert, Yves' 'Greene, Andrew E.' _chemical_formula_moiety 'C12 H20 F6 N3 O4 P S2' _chemical_formula_sum 'C12 H20 F6 N3 O4 P S2' _chemical_formula_structural 'C12 H20 F6 N3 O4 P S2' _chemical_formula_weight 479.39 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P1' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' _cell_length_a 8.657(2) _cell_length_b 10.352(2) _cell_length_c 12.859(3) _cell_angle_alpha 104.810(10) _cell_angle_beta 93.08(2) _cell_angle_gamma 111.21(2) _cell_volume 1024.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _exptl_crystal_density_diffrn 1.553 _diffrn_ambient_temperature 293 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_calc_attached_atom _atom_site_refinement_flags _atom_site_occupancy S13 1.02144(7) 1.06656(5) .86241(4) .05380(10) Uani d ? . 1.000 S14 .72711(6) .47601(6) .73474(4) .05440(10) Uani d ? . 1.000 P2 .78330(6) .77520(5) .75681(4) .04260(10) Uani d ? . 1.000 F19 1.2412(2) 1.1270(2) .73050(10) .1060(5) Uani d ? . 1.000 F20 1.1711(3) 1.2993(2) .8086(2) .1290(7) Uani d ? . 1.000 F21 1.0036(3) 1.1208(2) .67640(10) .1135(6) Uani d ? . 1.000 F22 .8234(2) .4536(3) .9221(2) .1616(7) Uani d ? . 1.000 F23 .6296(3) .5291(3) .92260(10) .1379(8) Uani d ? . 1.000 F24 .5796(3) .3098(2) .8486(2) .1576(8) Uani d ? . 1.000 O15 1.1439(2) 1.1296(2) .95740(10) .0695(4) Uani d ? . 1.000 O16 .8643(2) 1.0794(2) .86340(10) .0736(4) Uani d ? . 1.000 O17 .7955(2) .3775(2) .6799(2) .0844(5) Uani d ? . 1.000 O18 .5710(2) .4722(2) .69120(10) .0720(5) Uani d ? . 1.000 N1 .9950(2) .90070(10) .80610(10) .0412(3) Uani d ? . 1.000 N3 .8608(2) .6395(2) .76730(10) .0427(3) Uani d ? . 1.000 N10 .7636(2) .7717(2) .62870(10) .0522(4) Uani d ? . 1.000 C4 1.0443(2) .6837(2) .77710(10) .0445(4) Uani d ? . 1.000 C5 1.1137(2) .8403(2) .84370(10) .0443(4) Uani d ? . 1.000 C6 1.2977(2) .9119(2) .8390(2) .0626(6) Uani d ? . 1.000 C7 1.3904(3) .8326(3) .8832(2) .0759(7) Uani d ? . 1.000 C8 1.3157(3) .6715(3) .8295(2) .0724(6) Uani d ? . 1.000 C9 1.1277(3) .6027(2) .8264(2) .0594(5) Uani d ? . 1.000 C11 1.1162(4) 1.1589(3) .7636(2) .0785(7) Uani d ? . 1.000 C12 .6911(3) .4392(3) .8656(2) .0830(7) Uani d ? . 1.000 C25 .8855(3) .7697(3) .5546(2) .0633(6) Uani d ? . 1.000 C26 .8523(4) .6232(3) .4787(2) .0871(8) Uani d ? . 1.000 C27 .5944(3) .7499(3) .5791(2) .0765(7) Uani d ? . 1.000 C28 .5895(4) .8825(4) .5532(3) .1310(10) Uani d ? . 1.000 H1 1.0728 .6794 .7063 .053 Uiso c ? . 1.000 H2 1.1040 .8429 .9173 .053 Uiso c ? . 1.000 H3 1.3130 .9068 .7656 .075 Uiso c ? . 1.000 H4 1.3398 1.0105 .8820 .075 Uiso c ? . 1.000 H5 1.5037 .8697 .8719 .091 Uiso c ? . 1.000 H6 1.3872 .8503 .9592 .091 Uiso c ? . 1.000 H7 1.3682 .6278 .8685 .087 Uiso c ? . 1.000 H8 1.3378 .6532 .7568 .087 Uiso c ? . 1.000 H9 1.1043 .6078 .8984 .071 Uiso c ? . 1.000 H10 1.0859 .5040 .7833 .071 Uiso c ? . 1.000 H11 .8845 .8324 .5122 .076 Uiso c ? . 1.000 H12 .9935 .8049 .5971 .076 Uiso c ? . 1.000 H13 .9328 .6314 .4308 .105 Uiso c ? . 1.000 H14 .8601 .5606 .5195 .105 Uiso c ? . 1.000 H15 .7428 .5845 .4374 .105 Uiso c ? . 1.000 H16 .5598 .6719 .5135 .092 Uiso c ? . 1.000 H17 .5188 .7260 .6286 .092 Uiso c ? . 1.000 H18 .6180 .9599 .6187 .157 Uiso c ? . 1.000 H19 .6676 .9096 .5058 .157 Uiso c ? . 1.000 H20 .4797 .8615 .5187 .157 Uiso c ? . 1.000 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 S13 .0782(3) .0469(2) .0446(2) .0345(2) .0133(2) .0115(2) S14 .0510(3) .0480(2) .0549(3) .0107(2) -.0008(2) .0139(2) P2 .0439(2) .0575(2) .0365(2) .0281(2) .0094(2) .0178(2) F19 .1220(10) .0950(10) .1300(10) .0456(8) .0656(9) .0666(8) F20 .202(2) .0496(7) .135(2) .0399(9) .0360(10) .0369(8) F21 .1440(10) .1240(10) .0819(9) .0390(10) .0170(9) .0656(7) F22 .0890(10) .271(2) .1510(10) .0320(10) .0050(9) .1656(9) F23 .160(2) .185(2) .0920(10) .0680(10) .0610(10) .0700(10) F24 .130(2) .1260(10) .194(2) -.0180(10) .0220(10) .1090(10) O15 .0940(10) .0529(7) .0509(8) .0299(7) -.0007(7) -.0012(6) O16 .0982(9) .0778(7) .0757(9) .0647(6) .0254(7) .0264(7) O17 .0800(10) .0516(8) .1040(10) .0209(7) .0090(10) .0013(9) O18 .0510(8) .0740(10) .0740(10) .0080(7) -.0124(7) .0211(8) N1 .0488(7) .0423(6) .0368(6) .0233(5) .0079(5) .0104(5) N3 .0391(6) .0464(7) .0461(7) .0180(5) .0047(5) .0174(6) N10 .0565(8) .0709(9) .0374(7) .0318(6) .0041(6) .0197(6) C4 .0404(8) .0466(8) .0494(9) .0198(6) .0098(7) .0144(7) C5 .0442(8) .0485(8) .0417(8) .0243(6) .0046(7) .0070(7) C6 .0434(9) .0540(10) .0800(10) .0137(8) .0081(9) .0120(10) C7 .0413(9) .0780(10) .095(2) .0272(9) -.0030(10) -.0010(10) C8 .0540(10) .0780(10) .097(2) .0421(8) .0120(10) .0210(10) C9 .0553(9) .0549(9) .0740(10) .0307(7) .0011(9) .0165(9) C11 .114(2) .0550(10) .0770(10) .0340(10) .0240(10) .0324(9) C12 .0650(10) .093(2) .0910(10) .0100(10) .0090(10) .0580(10) C25 .0760(10) .0860(10) .0378(8) .0370(10) .0162(8) .0272(8) C26 .107(2) .104(2) .0520(10) .0500(10) .0170(10) .0110(10) C27 .0740(10) .107(2) .0590(10) .0450(10) -.0070(10) .0300(10) C28 .128(2) .155(2) .156(3) .0890(10) -.003(2) .077(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P2 N1 . . 1.783(2) yes P2 N3 . . 1.792(2) yes P2 N10 . . 1.637(2) yes S13 O15 . . 1.412(2) no S13 O16 . . 1.414(2) no S13 N1 . . 1.6080(10) no S13 C11 . . 1.834(3) no S14 O17 . . 1.415(2) no S14 O18 . . 1.418(2) no S14 N3 . . 1.5960(10) no S14 C12 . . 1.837(3) no F19 C11 . . 1.303(3) no F20 C11 . . 1.309(3) no F21 C11 . . 1.320(3) no F22 C12 . . 1.262(3) no F23 C12 . . 1.318(4) no F24 C12 . . 1.291(3) no N1 C5 . . 1.499(2) no N3 C4 . . 1.474(2) no N10 C25 . . 1.461(3) no N10 C27 . . 1.480(3) no C4 C5 . . 1.501(2) no C4 C9 . . 1.513(3) no C4 H1 . . .95 no C5 C6 . . 1.506(3) no C5 H2 . . .95 no C6 C7 . . 1.519(4) no C6 H3 . . .95 no C6 H4 . . .95 no C7 C8 . . 1.503(3) no C7 H5 . . .95 no C7 H6 . . .95 no C8 C9 . . 1.516(3) no C8 H7 . . .95 no C8 H8 . . .95 no C9 H9 . . .95 no C9 H10 . . .95 no C25 C26 . . 1.494(4) no C25 H11 . . .95 no C25 H12 . . .95 no C26 H13 . . .95 no C26 H14 . . .95 no C26 H15 . . .95 no C27 C28 . . 1.507(4) no C27 H16 . . .95 no C27 H17 . . .95 no C28 H18 . . .95 no C28 H19 . . .95 no C28 H20 . . .95 no _cod_database_code 2012510