#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/25/2012512.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_2012512 _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 ; _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _publ_author_name "Konya, Den\'es" 'Philouze, Christian' 'Gimbert, Yves' 'Greene, Andrew E.' _chemical_formula_moiety 'C17 H23 F12 N5 O8 P2 S4 , 0.98(C H Cl3)' _chemical_formula_sum 'C17.98 H23.98 Cl2.95 F12 N5 O8 P2 S4' _chemical_formula_structural 'C17 H23 F12 N5 O8 P2 S4 , 0.98(C H Cl3)' _chemical_formula_weight 960.65 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' _cell_length_a 8.812(4) _cell_length_b 13.897(3) _cell_length_c 14.728(6) _cell_angle_alpha 90 _cell_angle_beta 90.21(3) _cell_angle_gamma 90 _cell_volume 1803.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _exptl_crystal_density_diffrn 1.767 _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 Cl50 .2039(3) .2634(3) .16740(10) .1483(8) Uani d ? . .908 Cl51 .3289(8) .3505(5) .3153(4) .161(2) Uani d ? . .387 Cl52 .0720(3) .2825(3) .3473(2) .1880(10) Uani d ? . .844 Cl53 .3574(7) .2083(7) .3307(4) .191(3) Uani d ? . .378 Cl54 .3230(9) .1652(4) .3031(5) .156(2) Uani d ? . .431 S13 .68930(10) .4471 .89379(8) .0458(3) Uani d ? . 1.000 S14 .67840(10) .06162(7) .90237(8) .0472(3) Uani d ? . 1.000 S37 .31340(10) .45383(8) .68345(8) .0470(3) Uani d ? . 1.000 S38 .31200(10) .07042(8) .68187(8) .0447(3) Uani d ? . 1.000 P2 .59560(9) .25370(10) .85283(5) .0365(2) Uani d ? . 1.000 P27 .30204(8) .26140(10) .75138(5) .0351(2) Uani d ? . 1.000 F19 .9742(4) .4147(3) .9363(3) .1160(10) Uani d ? . 1.000 F20 .9415(4) .5221(3) .8400(3) .126(2) Uani d ? . 1.000 F21 .9170(4) .3732(3) .8046(3) .0950(10) Uani d ? . 1.000 F22 .9652(4) .0878(4) .9360(3) .129(2) Uani d ? . 1.000 F23 .8970(4) .1358(3) .8106(3) .147(2) Uani d ? . 1.000 F24 .9197(4) -.0113(3) .8322(3) .1160(10) Uani d ? . 1.000 F43 .0802(4) .5269(3) .6043(3) .1150(10) Uani d ? . 1.000 F44 .0758(4) .3751(3) .6114(3) .1050(10) Uani d ? . 1.000 F45 .2175(5) .4408(3) .5178(2) .1130(10) Uani d ? . 1.000 F46 .0683(4) .1542(3) .6164(3) .1040(10) Uani d ? . 1.000 F47 .2051(4) .0826(3) .5168(2) .1010(10) Uani d ? . 1.000 F48 .0675(4) .0029(3) .6055(3) .1060(10) Uani d ? . 1.000 O15 .6774(4) .5183(2) .9628(2) .0620(10) Uani d ? . 1.000 O16 .6180(4) .4567(2) .8080(2) .0660(10) Uani d ? . 1.000 O17 .6796(4) -.0057(2) .9730(2) .0660(10) Uani d ? . 1.000 O18 .5975(4) .0460(2) .8218(2) .0710(10) Uani d ? . 1.000 O39 .2368(4) .4646(2) .7668(2) .0580(9) Uani d ? . 1.000 O40 .4152(4) .5242(2) .6494(2) .0586(9) Uani d ? . 1.000 O41 .2405(4) .0602(2) .7674(2) .0560(9) Uani d ? . 1.000 O42 .4068(4) -.0002(2) .6451(2) .0620(10) Uani d ? . 1.000 N1 .6486(4) .3429(2) .9305(2) .0470(10) Uani d ? . 1.000 N3 .6352(4) .1692(2) .9385(2) .0355(8) Uani d ? . 1.000 N10 .4050(3) .2558(3) .84900(10) .0348(6) Uani d ? . 1.000 N26 .3882(4) .3479(2) .6824(2) .0393(9) Uani d ? . 1.000 N28 .3887(4) .1749(2) .6810(2) .0399(9) Uani d ? . 1.000 C4 .7007(5) .2083(3) 1.0235(3) .0440(10) Uani d ? . 1.000 C5 .6446(5) .3113(3) 1.0299(3) .0390(10) Uani d ? . 1.000 C6 .7332(6) .3646(3) 1.0995(3) .0630(10) Uani d ? . 1.000 C7 .7094(9) .3166(4) 1.1909(4) .084(2) Uani d ? . 1.000 C8 .7287(8) .2097(4) 1.1904(4) .081(2) Uani d ? . 1.000 C9 .6571(7) .1555(3) 1.1118(3) .0680(10) Uani d ? . 1.000 C11 .8937(6) .4378(4) .8648(4) .074(2) Uani d ? . 1.000 C12 .8778(6) .0704(3) .8673(4) .0590(10) Uani d ? . 1.000 C25 .3078(4) .2537(5) .9312(2) .0491(9) Uani d ? . 1.000 C29 .4747(5) .2130(3) .6014(3) .0440(10) Uani d ? . 1.000 C30 .5200(4) .3134(3) .6302(3) .0400(10) Uani d ? . 1.000 C31 .5769(6) .3702(3) .5492(3) .0570(10) Uani d ? . 1.000 C32 .7148(6) .3170(4) .5147(3) .069(2) Uani d ? . 1.000 C33 .6876(7) .2118(4) .4906(4) .079(2) Uani d ? . 1.000 C34 .6146(6) .1584(4) .5716(3) .0680(10) Uani d ? . 1.000 C35 .1624(6) .4472(4) .6015(4) .067(2) Uani d ? . 1.000 C36 .1522(6) .0782(4) .5997(4) .075(2) Uani d ? . 1.000 C49 .2220(10) .2560(10) .2864(6) .272(5) Uani d ? . .983 H1 .8081 .2089 1.0183 .053 Uiso c ? . 1.000 H2 .5416 .3098 1.0487 .046 Uiso c ? . 1.000 H3 .6995 .4294 1.1021 .075 Uiso c ? . 1.000 H4 .8379 .3632 1.0843 .075 Uiso c ? . 1.000 H5 .7805 .3430 1.2327 .101 Uiso c ? . 1.000 H6 .6094 .3307 1.2106 .101 Uiso c ? . 1.000 H7 .8345 .1965 1.1898 .098 Uiso c ? . 1.000 H8 .6858 .1854 1.2449 .098 Uiso c ? . 1.000 H9 .6941 .0913 1.1103 .082 Uiso c ? . 1.000 H10 .5498 .1547 1.1182 .082 Uiso c ? . 1.000 H11 .3352 .2002 .9679 .059 Uiso c ? . 1.000 H12 .2044 .2480 .9135 .059 Uiso c ? . 1.000 H13 .3216 .3114 .9647 .059 Uiso c ? . 1.000 H14 .4072 .2178 .5512 .053 Uiso c ? . 1.000 H15 .6025 .3072 .6716 .047 Uiso c ? . 1.000 H16 .6038 .4336 .5671 .068 Uiso c ? . 1.000 H17 .5009 .3731 .5033 .068 Uiso c ? . 1.000 H18 .7910 .3195 .5604 .083 Uiso c ? . 1.000 H19 .7499 .3491 .4618 .083 Uiso c ? . 1.000 H20 .6216 .2083 .4396 .095 Uiso c ? . 1.000 H21 .7817 .1823 .4762 .095 Uiso c ? . 1.000 H22 .6850 .1550 .6205 .081 Uiso c ? . 1.000 H23 .5868 .0952 .5536 .081 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 Cl50 .183(2) .175(2) .0870(10) .022(3) .0050(10) .020(2) Cl51 .194(5) .190(5) .098(3) -.116(4) .013(4) -.041(3) Cl52 .138(2) .276(4) .149(2) .095(2) -.003(2) -.076(2) Cl53 .111(4) .350(10) .112(4) .080(5) -.009(3) .057(5) Cl54 .187(5) .116(3) .163(5) .070(3) -.007(4) -.037(3) S13 .0437(6) .0333(5) .0602(7) -.0036(4) -.0035(5) .0059(5) S14 .0489(6) .0333(5) .0593(7) .0048(5) -.0072(5) -.0067(5) S37 .0510(6) .0328(5) .0571(6) .0033(5) -.0080(5) .0019(5) S38 .0555(6) .0330(5) .0456(6) -.0087(5) -.0047(5) -.0014(5) P2 .0358(4) .0361(4) .0375(4) -.0021(6) -.0028(3) .0008(6) P27 .0347(4) .0340(4) .0367(4) -.0024(6) -.0028(3) -.0004(7) F19 .050(2) .163(4) .135(3) .018(2) -.013(2) -.001(3) F20 .079(2) .074(2) .224(5) -.032(2) .048(3) .009(3) F21 .077(2) .088(2) .121(2) -.013(2) .040(2) -.038(2) F22 .048(2) .175(4) .164(4) .011(2) -.019(2) -.026(3) F23 .094(2) .153(3) .196(4) .045(2) .080(2) .089(3) F24 .086(2) .089(2) .174(4) .023(2) .026(2) -.043(2) F43 .098(3) .093(2) .155(3) .036(2) -.042(2) .024(2) F44 .091(2) .098(2) .126(3) -.029(2) -.053(2) .025(2) F45 .118(3) .140(3) .083(2) -.011(3) -.044(2) .017(2) F46 .086(2) .091(2) .135(3) .023(2) -.060(2) -.023(2) F47 .105(2) .148(3) .050(2) -.034(2) -.023(2) .001(2) F48 .095(2) .095(2) .129(3) -.052(2) -.041(2) -.001(2) O15 .065(2) .034(2) .088(2) .0030(10) -.002(2) -.005(2) O16 .077(2) .058(2) .061(2) -.007(2) -.015(2) .021(2) O17 .086(2) .040(2) .071(2) .011(2) .011(2) .006(2) O18 .075(2) .053(2) .084(2) .013(2) -.028(2) -.028(2) O39 .068(2) .045(2) .062(2) .009(2) .000(2) -.011(2) O40 .062(2) .0360(10) .078(2) -.0030(10) -.008(2) .012(2) O41 .061(2) .050(2) .058(2) -.012(2) .008(2) .007(2) O42 .079(2) .038(2) .068(2) .003(2) .002(2) -.008(2) N1 .065(2) .034(2) .041(2) -.009(2) -.017(2) .007(2) N3 .036(2) .032(2) .039(2) .0080(10) -.0030(10) .0010(10) N10 .0370(10) .0330(10) .0340(10) .000(2) .0000(10) .002(2) N26 .045(2) .037(2) .036(2) .0020(10) .002(2) .0070(10) N28 .048(2) .0280(10) .043(2) -.0040(10) .004(2) -.0040(10) C4 .045(2) .040(2) .048(2) -.008(2) -.008(2) .000(2) C5 .048(2) .032(2) .037(2) .000(2) -.002(2) -.001(2) C6 .093(3) .039(2) .056(3) -.003(2) -.028(2) -.008(2) C7 .158(6) .051(3) .043(3) -.015(3) -.025(3) -.009(2) C8 .135(5) .060(3) .049(3) -.019(3) -.028(3) .002(3) C9 .112(4) .049(2) .043(2) -.017(3) -.018(2) .010(2) C11 .044(3) .074(3) .103(4) -.020(3) .009(3) -.011(3) C12 .061(3) .045(2) .072(3) .006(2) .005(3) -.002(2) C25 .043(2) .066(2) .039(2) .000(3) .0020(10) -.009(3) C29 .051(2) .043(2) .037(2) -.009(2) .001(2) -.003(2) C30 .039(2) .038(2) .042(2) -.002(2) .001(2) .003(2) C31 .072(3) .045(2) .053(2) .003(2) .016(2) .012(2) C32 .074(3) .069(3) .066(3) -.010(3) .035(2) .003(3) C33 .102(4) .068(3) .068(3) -.007(3) .048(3) .003(3) C34 .081(3) .052(3) .070(3) -.007(2) .031(3) -.022(2) C35 .062(3) .066(3) .073(3) -.005(3) -.005(3) .022(3) C36 .082(3) .058(3) .085(3) -.025(3) -.049(3) .008(3) C49 .208(8) .46(2) .149(6) .200(10) -.058(6) -.156(9) 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 . . 1.749(4) yes P2 N3 . . 1.758(3) yes P2 N10 . . 1.681(2) yes P27 N10 . . 1.699(2) yes P27 N26 . . 1.749(3) yes P27 N28 . . 1.763(3) yes S13 O15 . . 1.423(3) no S13 O16 . . 1.416(3) no S13 N1 . . 1.588(3) no S13 C11 . . 1.857(5) no Cl50 C49 . . 1.762(9) no Cl51 C49 . . 1.67(2) no Cl52 C49 . . 1.640(10) no Cl53 C49 . . 1.510(10) no Cl54 C49 . . 1.57(2) no S14 O17 . . 1.399(4) no S14 O18 . . 1.399(4) no S14 N3 . . 1.632(3) no S14 C12 . . 1.837(5) no S37 O39 . . 1.411(3) no S37 O40 . . 1.420(3) no S37 N26 . . 1.613(4) no S37 C35 . . 1.796(6) no S38 O41 . . 1.418(3) no S38 O42 . . 1.399(3) no S38 N28 . . 1.601(3) no S38 C36 . . 1.856(5) no F19 C11 . . 1.309(7) no F20 C11 . . 1.298(6) no F21 C11 . . 1.278(6) no F22 C12 . . 1.293(6) no F23 C12 . . 1.247(6) no F24 C12 . . 1.301(6) no F43 C35 . . 1.324(6) no F44 C35 . . 1.267(6) no F45 C35 . . 1.329(6) no F46 C36 . . 1.313(6) no F47 C36 . . 1.310(7) no F48 C36 . . 1.288(6) no N1 C5 . . 1.528(5) no N3 C4 . . 1.480(5) no N10 C25 . . 1.485(4) no N26 C30 . . 1.475(5) no N28 C29 . . 1.495(5) no C4 C5 . . 1.517(5) no C4 C9 . . 1.544(6) no C4 H1 . . .95 no C5 C6 . . 1.484(6) no C5 H2 . . .95 no C6 C7 . . 1.518(7) no C6 H3 . . .95 no C6 H4 . . .95 no C7 C8 . . 1.495(6) no C7 H5 . . .95 no C7 H6 . . .95 no C8 C9 . . 1.518(7) no C8 H7 . . .95 no C8 H8 . . .95 no C9 H9 . . .95 no C9 H10 . . .95 no C25 H11 . . .95 no C25 H12 . . .95 no C25 H13 . . .95 no C29 C30 . . 1.511(5) no C29 C34 . . 1.514(7) no C29 H14 . . .95 no C30 C31 . . 1.518(6) no C30 H15 . . .95 no C31 C32 . . 1.512(7) no C31 H16 . . .95 no C31 H17 . . .95 no C32 C33 . . 1.523(7) no C32 H18 . . .95 no C32 H19 . . .95 no C33 C34 . . 1.548(7) no C33 H20 . . .95 no C33 H21 . . .95 no C34 H22 . . .95 no C34 H23 . . .95 no _cod_database_code 2012512