#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006622.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_2006622 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1471 _journal_page_last 1472 _publ_section_title ; 9a-Trimethylsilyloctahydroquinolizinium Picrate ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'White, Jonathan M.' 'Tham, Wai-Ying' _chemical_formula_sum 'C18 H28 N4 O7 Si1' _chemical_formula_iupac 'C12 H26 N1 Si1 1+, C6 H2 N3 O7 1-' _chemical_formula_weight 440.52 _chemical_melting_point 422 _symmetry_cell_setting 'Monoclinic' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8710(10) _cell_length_b 21.586(2) _cell_length_c 8.4840(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 102.580(10) _cell_angle_gamma 90.000(10) _cell_volume 2121.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.379 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .0500 _refine_ls_wR_factor_obs .1331 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 Si .30577(5) .11822(3) .05271(7) .0434(2) Uani d . 1 . Si N1 .1806(2) .08988(9) .3024(2) .0442(4) Uani d . 1 . N H1 .120(2) .1034(12) .227(3) .056(7) Uiso d . 1 . H C2 .1257(2) .04243(13) .3933(4) .0610(7) Uani d . 1 . C H2A .187(2) .0295(13) .487(4) .069(8) Uiso d . 1 . H H2B .067(3) .0657(13) .434(3) .068(8) Uiso d . 1 . H C3 .0778(3) -.01117(15) .2869(4) .0737(8) Uani d . 1 . C H3A .013(3) .0048(15) .196(4) .085(9) Uiso d . 1 . H H3B .042(3) -.0379(18) .340(4) .099(11) Uiso d . 1 . H C4 .1709(3) -.04264(13) .2211(4) .0708(8) Uani d . 1 . C H4A .227(3) -.0611(15) .307(4) .081(9) Uiso d . 1 . H H4B .139(3) -.0731(16) .156(4) .086(10) Uiso d . 1 . H C5 .2255(3) .00381(12) .1274(3) .0608(6) Uani d . 1 . C H5A .296(3) -.0175(14) .097(4) .076(8) Uiso d . 1 . H H5B .169(3) .0148(13) .036(4) .069(8) Uiso d . 1 . H C6 .2738(2) .06331(9) .2197(3) .0418(5) Uani d . 1 . C C7 .3804(2) .04791(11) .3518(3) .0525(6) Uani d . 1 . C H7A .438(2) .0327(13) .288(3) .063(7) Uiso d . 1 . H H7B .363(2) .0125(12) .417(3) .053(6) Uiso d . 1 . H C8 .4246(2) .10089(14) .4641(4) .0645(7) Uani d . 1 . C H8A .489(3) .0874(15) .550(4) .086(9) Uiso d . 1 . H H8B .453(3) .1339(15) .409(4) .077(9) Uiso d . 1 . H C9 .3296(3) .12640(15) .5384(3) .0656(7) Uani d . 1 . C H9A .307(2) .0943(15) .608(4) .074(8) Uiso d . 1 . H H9B .355(3) .1594(16) .599(4) .083(10) Uiso d . 1 . H C10 .2243(2) .14369(11) .4117(3) .0541(6) Uani d . 1 . C H10A .244(2) .1753(11) .343(3) .049(6) Uiso d . 1 . H H10B .163(2) .1575(12) .461(3) .057(7) Uiso d . 1 . H C11 .1713(3) .1252(2) -.1068(4) .0666(7) Uani d . 1 . C H11A .182(3) .1570(16) -.181(4) .082(9) Uiso d . 1 . H H11B .110(3) .1367(16) -.061(4) .094(11) Uiso d . 1 . H H11C .154(3) .0877(19) -.177(4) .102(12) Uiso d . 1 . H C12 .4220(3) .0794(2) -.0254(4) .0652(7) Uani d . 1 . C H12A .447(3) .1031(16) -.102(4) .084(10) Uiso d . 1 . H H12B .399(3) .0436(19) -.073(5) .102(13) Uiso d . 1 . H H12C .488(3) .0714(16) .061(4) .089(10) Uiso d . 1 . H C13 .3535(3) .19878(13) .1109(4) .0658(7) Uani d . 1 . C H13A .414(4) .2013(18) .202(5) .106(13) Uiso d . 1 . H H13B .291(3) .2242(16) .137(4) .084(9) Uiso d . 1 . H H13C .368(3) .2157(18) .008(5) .111(12) Uiso d . 1 . H C14 -.1141(2) .16736(11) .1943(3) .0459(5) Uani d . 1 . C C15 -.1086(2) .23458(11) .1845(3) .0445(5) Uani d . 1 . C C16 -.1874(2) .27412(12) .2256(3) .0495(5) Uani d . 1 . C H16 -.180(3) .3136(15) .216(4) .075(9) Uiso d . 1 . H C17 -.2778(2) .25049(11) .2846(3) .0515(6) Uani d . 1 . C C18 -.2906(2) .18747(12) .3010(3) .0513(6) Uani d . 1 . C H18 -.347(2) .1721(11) .346(3) .051(6) Uiso d . 1 . H C19 -.2134(2) .14791(10) .2572(3) .0467(5) Uani d . 1 . C O1 -.04567(15) .13134(8) .1506(2) .0625(5) Uani d . 1 . O O2 .0752(2) .23551(11) .1374(4) .0980(8) Uani d . 1 . O O3 -.0279(2) .31645(10) .0742(2) .0725(5) Uani d . 1 . O O4 -.3513(2) .34723(12) .3078(5) .1236(11) Uani d . 1 . O O5 -.4332(2) .27024(12) .3970(3) .0923(7) Uani d . 1 . O O6 -.3225(2) .06574(11) .3130(4) .1210(11) Uani d . 1 . O O7 -.1590(2) .04502(11) .2780(4) .1160(10) Uani d . 1 . O N2 -.0148(2) .26372(10) .1268(2) .0545(5) Uani d . 1 . N N3 -.3598(2) .29223(12) .3319(3) .0721(7) Uani d . 1 . N N4 -.2331(2) .08248(10) .2818(3) .0611(5) Uani d . 1 . N 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 Si .0397(3) .0416(3) .0522(4) .0026(2) .0168(3) .0063(3) N1 .0373(9) .0453(10) .0520(10) .0016(7) .0144(8) .0067(8) C2 .0573(15) .061(2) .072(2) -.0043(12) .0310(14) .0135(13) C3 .066(2) .065(2) .093(2) -.0213(14) .024(2) .013(2) C4 .085(2) .0432(14) .084(2) -.0161(14) .018(2) .0004(14) C5 .075(2) .0454(13) .064(2) -.0084(12) .0189(14) -.0035(12) C6 .0421(11) .0360(10) .0506(12) .0012(8) .0173(9) .0012(9) C7 .0474(12) .0501(13) .0615(14) .0121(10) .0153(11) .0127(11) C8 .0499(14) .067(2) .070(2) .0005(12) -.0014(13) .0106(14) C9 .081(2) .057(2) .0553(15) -.0009(14) .0058(13) -.0059(13) C10 .0621(15) .0450(12) .0609(14) .0056(11) .0260(12) -.0033(11) C11 .057(2) .078(2) .064(2) .0074(14) .0120(13) .017(2) C12 .061(2) .070(2) .074(2) .0124(14) .035(2) .009(2) C13 .072(2) .0475(14) .084(2) -.0084(13) .031(2) .0062(14) C14 .0380(11) .0527(13) .0460(12) .0027(9) .0068(9) -.0022(9) C15 .0355(10) .0543(13) .0441(11) -.0001(9) .0093(9) .0000(9) C16 .0411(12) .0502(14) .0549(13) .0040(10) .0053(10) .0003(11) C17 .0345(11) .0605(14) .0597(14) .0065(9) .0104(10) -.0054(11) C18 .0350(11) .066(2) .0534(13) -.0043(10) .0104(10) -.0026(11) C19 .0391(11) .0508(12) .0485(12) -.0011(9) .0058(9) .0011(10) O1 .0515(10) .0590(10) .0817(12) .0099(8) .0245(9) -.0064(9) O2 .0565(12) .0823(14) .171(2) .0052(10) .0586(14) .0061(15) O3 .0619(11) .0778(13) .0776(13) -.0093(9) .0149(9) .0222(10) O4 .096(2) .071(2) .227(4) .0243(13) .085(2) .001(2) O5 .0612(12) .104(2) .126(2) .0012(11) .0512(13) -.0251(14) O6 .0746(15) .076(2) .224(3) -.0067(12) .057(2) .033(2) O7 .113(2) .0593(13) .199(3) .0094(13) .085(2) .020(2) N2 .0437(11) .0646(13) .0569(12) -.0037(9) .0149(9) -.0005(10) N3 .0451(12) .077(2) .097(2) .0086(11) .0229(12) -.0144(13) N4 .0494(12) .0570(12) .0771(14) -.0044(10) .0140(10) .0059(10) 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 Si C12 . 1.856(3) y Si C11 . 1.860(3) y Si C13 . 1.862(3) y Si C6 . 1.947(2) y N1 C10 . 1.506(3) y N1 C2 . 1.512(3) y N1 C6 . 1.544(3) y N1 H1 . .90(3) y C2 C3 . 1.501(4) y C2 H2A . 1.00(3) ? C2 H2B . .98(3) ? C3 C4 . 1.505(5) y C3 H3A . 1.02(3) ? C3 H3B . .90(4) ? C4 C5 . 1.511(4) y C4 H4A . .96(3) ? C4 H4B . .89(3) ? C5 C6 . 1.548(3) y C5 H5A . 1.03(3) ? C5 H5B . .94(3) ? C6 C7 . 1.534(3) y C7 C8 . 1.508(4) y C7 H7A . 1.01(3) ? C7 H7B . .99(3) ? C8 C9 . 1.511(4) y C8 H8A . .98(4) ? C8 H8B . .95(3) ? C9 C10 . 1.507(4) y C9 H9A . .99(3) ? C9 H9B . .89(4) ? C10 H10A . .96(3) ? C10 H10B . .96(3) ? C11 H11A . .96(4) ? C11 H11B . .92(4) ? C11 H11C . 1.00(4) ? C12 H12A . .92(4) ? C12 H12B . .89(4) ? C12 H12C . .97(4) ? C13 H13A . .94(4) ? C13 H13B . .99(3) ? C13 H13C . 1.00(4) ? C14 O1 . 1.238(3) ? C14 C15 . 1.455(3) ? C14 C19 . 1.458(3) ? C15 C16 . 1.366(3) ? C15 N2 . 1.454(3) ? C16 C17 . 1.377(3) ? C16 H16 . .86(3) ? C17 C18 . 1.379(4) ? C17 N3 . 1.446(3) ? C18 C19 . 1.363(3) ? C18 H18 . .90(3) ? C19 N4 . 1.454(3) ? O2 N2 . 1.216(3) ? O3 N2 . 1.220(3) ? O4 N3 . 1.213(3) ? O5 N3 . 1.224(3) ? O6 N4 . 1.204(3) ? O7 N4 . 1.200(3) ? O1 H1 . 2.025(3) n