#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006538.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_2006538 _journal_name_full 'Acta Crystallographica' _journal_year 1997 _journal_volume C53 _journal_page_first 1288 _journal_page_last 1290 _publ_section_title ; (11R,11aS-trans)-11-Ethylthio-2,3,5,10,11,11a-hexahydro-1H-pyrrolo[2,1-c][1,4] benzodiazepin-5-one ; loop_ _publ_author_name 'Kubicki, Maciej' "Szkaradzi\'nska, Maria B." 'Codding, Penelope W.' _chemical_formula_moiety 'C14 H18 N2 O S' _chemical_formula_sum 'C14 H18 N2 O S' _chemical_formula_weight 262.36 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 8.9850(8) _cell_length_b 8.9850(8) _cell_length_c 17.1652(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1385.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.258 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .0529 _refine_ls_wR_factor_obs .1443 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 C11a .8622(8) .5068(6) .0558(3) .072(2) Uani d . 1 . C H1A1 .9432(8) .4429(6) .0745(3) .086 Uiso calc PR .554(9) 1 H H1A2 .9347(8) .4253(6) .0554(3) .086 Uiso calc PR .446(9) 2 H C1' .923(2) .6125(15) .1232(7) .071(4) Uani d PD .446(9) 2 C H1C .840(2) .6514(15) .1529(7) .085 Uiso calc PR .446(9) 2 H H1D .985(2) .5549(15) .1582(7) .085 Uiso calc PR .446(9) 2 H C2' 1.010(4) .736(3) .0919(11) .136(8) Uani d PDU .446(9) 2 C H2C 1.115(4) .717(3) .0977(11) .163 Uiso calc PR .446(9) 2 H H2D .985(4) .827(3) .1189(11) .163 Uiso calc PR .446(9) 2 H C3' .969(2) .747(2) .0069(8) .071(5) Uani d PD .446(9) 2 C H3C 1.056(2) .768(2) -.0246(8) .085 Uiso calc PR .446(9) 2 H H3D .896(2) .826(2) -.0014(8) .085 Uiso calc PR .446(9) 2 H N4 .9004(5) .5900(4) -.0146(2) .0596(10) Uani d . 1 . N C1 .8217(19) .6383(13) .1147(7) .083(4) Uani d PD .554(9) 1 C H1A .7154(19) .6573(13) .1153(7) .100 Uiso calc PR .554(9) 1 H H1B .8544(19) .6152(13) .1672(7) .100 Uiso calc PR .554(9) 1 H C2 .9030(15) .7650(10) .0832(7) .072(3) Uani d PD .554(9) 1 C H2A 1.0040(15) .7669(10) .1032(7) .087 Uiso calc PR .554(9) 1 H H2B .8542(15) .8575(10) .0971(7) .087 Uiso calc PR .554(9) 1 H C3 .9033(18) .7444(18) -.0041(9) .082(5) Uani d PD .554(9) 1 C H3A .8166(18) .7907(18) -.0275(9) .098 Uiso calc PR .554(9) 1 H H3B .9922(18) .7872(18) -.0270(9) .098 Uiso calc PR .554(9) 1 H C5 .9054(4) .5374(6) -.0869(3) .0536(10) Uani d . 1 . C O5 .9357(4) .6250(5) -.1410(2) .0715(11) Uani d . 1 . O C5a .8824(5) .3762(6) -.1028(3) .0573(11) Uani d . 1 . C C6 .9484(8) .3293(9) -.1731(4) .089(2) Uani d . 1 . C H6 1.0011(8) .3985(9) -.2025(4) .107 Uiso calc R 1 . H C7 .9381(10) .1857(11) -.1999(5) .113(3) Uani d . 1 . C H7 .9808(10) .1597(11) -.2474(5) .136 Uiso calc R 1 . H C8 .8646(8) .0808(9) -.1566(4) .097(2) Uani d . 1 . C H8 .8609(8) -.0175(9) -.1734(4) .116 Uiso calc R 1 . H C9 .7959(6) .1216(7) -.0878(3) .0705(14) Uani d . 1 . C H9 .7434(6) .0504(7) -.0597(3) .085 Uiso calc R 1 . H C9a .8034(5) .2672(6) -.0594(3) .0539(11) Uani d . 1 . C N10 .7297(5) .2914(5) .0094(2) .0579(10) Uani d . 1 . N H10 .689(5) .215(5) .033(3) .043(11) Uiso d . 1 . H C11 .7132(6) .4247(5) .0479(3) .0625(12) Uani d D 1 . C H11B .6843(6) .3982(5) .1012(3) .075 Uiso calc PR .554(9) 1 H H11A .6757(6) .4037(5) .1004(3) .075 Uiso calc PR .446(9) 2 H S12 .5940(4) .5820(4) .0213(2) .0659(13) Uani d PD .554(9) 1 S C13 .4168(10) .4902(17) .0413(11) .107(5) Uani d PDU .554(9) 1 C H13A .4149(10) .3950(17) .0147(11) .129 Uiso calc PR .554(9) 1 H H13B .4095(10) .4710(17) .0968(11) .129 Uiso calc PR .554(9) 1 H C14 .2918(13) .575(2) .0176(14) .132(6) Uani d PDU .554(9) 1 C H14A .2022(13) .521(2) .0295(14) .171 Uiso calc PR .554(9) 1 H H14B .2970(13) .592(2) -.0376(14) .171 Uiso calc PR .554(9) 1 H H14C .2915(13) .668(2) .0446(14) .171 Uiso calc PR .554(9) 1 H S12' .5589(3) .5194(5) -.0093(2) .0475(12) Uani d PD .446(9) 2 S C13' .4125(11) .3852(17) .0036(9) .074(4) Uani d PD .446(9) 2 C H13C .4478(11) .2881(17) -.0128(9) .089 Uiso calc PR .446(9) 2 H H13D .3875(11) .3790(17) .0585(9) .089 Uiso calc PR .446(9) 2 H C14' .2811(13) .422(2) -.0398(12) .109(7) Uani d PD .446(9) 2 C H14D .2063(13) .348(2) -.0311(12) .141 Uiso calc PR .446(9) 2 H H14E .3048(13) .427(2) -.0943(12) .141 Uiso calc PR .446(9) 2 H H14F .2445(13) .517(2) -.0230(12) .141 Uiso calc PR .446(9) 2 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 C11A .124(5) .050(2) .040(2) -.007(3) -.006(3) -.001(2) C1' .090(10) .074(8) .049(6) -.009(7) -.004(6) -.016(6) C2' .198(19) .119(14) .091(11) -.055(15) -.024(14) -.020(11) C3' .100(14) .050(7) .063(8) -.006(9) -.001(9) -.002(5) N4 .080(3) .047(2) .052(2) .006(2) .006(2) .005(2) C1 .114(10) .070(7) .065(6) -.018(7) .010(7) -.029(5) C2 .083(7) .048(5) .086(7) -.018(5) .023(6) -.022(5) C3 .080(9) .050(6) .114(12) -.003(7) .004(8) .013(7) C5 .037(2) .073(3) .051(2) .004(2) -.002(2) .013(2) O5 .057(2) .104(3) .054(2) -.011(2) .0004(15) .030(2) C5A .040(2) .092(3) .040(2) -.007(2) -.002(2) -.007(2) C6 .080(4) .127(6) .060(3) -.024(4) .021(3) -.023(3) C7 .119(6) .142(7) .079(4) -.032(5) .040(4) -.050(5) C8 .093(5) .106(5) .091(5) -.020(4) .001(4) -.052(4) C9 .058(3) .085(3) .069(3) -.018(2) -.001(2) -.024(3) C9A .041(2) .080(3) .040(2) -.004(2) -.005(2) -.011(2) N10 .067(2) .061(2) .046(2) -.011(2) .012(2) -.001(2) C11 .086(3) .058(3) .043(2) .017(2) .021(2) .012(2) S12 .074(2) .049(2) .075(2) .0104(14) .027(2) .012(2) C13 .095(8) .088(8) .138(12) .009(7) .052(8) .030(9) C14 .081(8) .134(12) .180(15) .019(8) .021(10) .036(12) S12' .0403(12) .049(2) .053(2) .0038(10) .0048(10) .0125(15) C13' .057(6) .085(9) .081(9) -.013(6) .005(6) .018(7) C14' .062(8) .136(16) .128(15) -.023(9) -.001(9) .049(13) 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 C11A N4 . 1.463(6) ? C11A C11 . 1.535(8) ? C11A C1' . 1.595(12) ? C11A C1 . 1.598(12) ? C11A H1A1 . .98 ? C11A H1A2 . .98 ? C1' C2' . 1.46(2) ? C1' H1C . .97 ? C1' H1D . .97 ? C2' C3' . 1.51(2) ? C2' H2C . .97 ? C2' H2D . .97 ? C3' N4 . 1.59(2) ? C3' H3C . .97 ? C3' H3D . .97 ? N4 C5 . 1.328(6) ? N4 C3 . 1.40(2) ? C1 C2 . 1.457(13) ? C1 H1A . .97 ? C1 H1B . .97 ? C2 C3 . 1.51(2) ? C2 H2A . .97 ? C2 H2B . .97 ? C3 H3A . .97 ? C3 H3B . .97 ? C5 O5 . 1.247(5) ? C5 C5A . 1.488(8) ? C5A C6 . 1.408(7) ? C5A C9A . 1.420(7) ? C6 C7 . 1.374(12) ? C6 H6 . .93 ? C7 C8 . 1.371(12) ? C7 H7 . .93 ? C8 C9 . 1.381(9) ? C8 H8 . .93 ? C9 C9A . 1.398(7) ? C9 H9 . .93 ? C9A N10 . 1.372(6) ? N10 C11 . 1.376(6) ? N10 H10 . .87(5) ? C11 S12 . 1.832(5) ? C11 S12' . 1.900(6) ? C11 H11B . .98 ? C11 H11A . .98 ? S12 C13 . 1.826(10) ? C13 C14 . 1.417(15) ? C13 H13A . .97 ? C13 H13B . .97 ? C14 H14A . .96 ? C14 H14B . .96 ? C14 H14C . .96 ? S12' C13' . 1.799(9) ? C13' C14' . 1.435(15) ? C13' H13C . .97 ? C13' H13D . .97 ? C14' H14D . .96 ? C14' H14E . .96 ? C14' H14F . .96 ?