#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008442.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_2008442 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1999 _journal_volume 55 _journal_page_first 808 _journal_page_last 811 _publ_section_title ; Imide and tribenzyl ester derivatives of Kemp's triacid ; loop_ _publ_author_name "Thu\'ery, Pierre" 'Nierlich, Martine' 'Wang, Zhen-He' 'Hirose, Takuji' _chemical_formula_moiety 'C22 H29 N O4, C H4 O' _chemical_formula_sum 'C23 H33 N O5' _chemical_formula_weight 403.50 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1757(4) _cell_length_b 13.1247(6) _cell_length_c 18.6567(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.412(3) _cell_angle_gamma 90.00 _cell_volume 2228(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _exptl_crystal_density_diffrn 1.203 _diffrn_ambient_temperature 123(2) _refine_ls_R_factor_obs .059 _refine_ls_wR_factor_obs .125 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 O1 .1434(2) .49383(13) .28538(9) .0430(4) Uani d . 1 . O O2 -.0790(2) .31733(13) .09361(10) .0410(4) Uani d . 1 . O O3 .3751(2) .46995(13) .15908(9) .0388(4) Uani d . 1 . O O4 .2651(2) .38138(13) .06483(9) .0368(4) Uani d . 1 . O N1 .0303(2) .40389(14) .19098(10) .0285(4) Uani d . 1 . N C1 .0825(3) .2191(2) .17867(13) .0341(5) Uani d . 1 . C C2 .1130(3) .2246(2) .26075(13) .0356(6) Uani d . 1 . C H2A .0209 .2296 .28077 .043 Uiso calc R 1 . H H2B .1623 .1628 .27919 .043 Uiso calc R 1 . H C3 .2084(2) .3160(2) .28423(12) .0317(5) Uani d . 1 . C C4 .3571(2) .3052(2) .25448(13) .0326(5) Uani d . 1 . C H4A .4142 .3663 .26679 .039 Uiso calc R 1 . H H4B .4102 .2485 .27896 .039 Uiso calc R 1 . H C5 .3483(2) .2881(2) .17288(12) .0311(5) Uani d . 1 . C C6 .2292(3) .2088(2) .14686(14) .0357(6) Uani d . 1 . C H6A .2688 .1415 .15851 .043 Uiso calc R 1 . H H6B .2085 .2133 .09464 .043 Uiso calc R 1 . H C7 -.0147(3) .1275(2) .1551(2) .0493(7) Uani d . 1 . C H7A .0315 .0664 .1751 .074 Uiso calc R 1 . H H7B -.0282 .1230 .1033 .074 Uiso calc R 1 . H H7C -.1084 .1356 .1720 .074 Uiso calc R 1 . H C8 .2386(3) .3243(2) .36683(13) .0415(6) Uani d . 1 . C H8A .3013 .3818 .37976 .062 Uiso calc R 1 . H H8B .2859 .2633 .38623 .062 Uiso calc R 1 . H H8C .1474 .3332 .38617 .062 Uiso calc R 1 . H C9 .3297(2) .3902(2) .13297(13) .0306(5) Uani d . 1 . C C10 .4979(3) .2459(2) .1559(2) .0435(6) Uani d . 1 . C H10A .4924 .2324 .1051 .065 Uiso calc R 1 . H H10B .5203 .1840 .1824 .065 Uiso calc R 1 . H H10C .5735 .2953 .1697 .065 Uiso calc R 1 . H C11 .1288(2) .4123(2) .25552(12) .0301(5) Uani d . 1 . C C12 .0046(2) .3153(2) .15014(13) .0325(5) Uani d . 1 . C C13 -.0513(2) .4946(2) .16521(12) .0287(5) Uani d . 1 . C C14 -.1912(2) .5094(2) .18343(13) .0339(5) Uani d . 1 . C H14 -.2313 .4629 .21303 .041 Uiso calc R 1 . H C15 -.2711(3) .5942(2) .15714(13) .0342(5) Uani d . 1 . C H15 -.3650 .6040 .16960 .041 Uiso calc R 1 . H C16 -.2142(2) .6647(2) .11263(12) .0308(5) Uani d . 1 . C C17 -.0734(2) .6471(2) .09458(13) .0322(5) Uani d . 1 . C H17 -.0337 .6926 .06412 .039 Uiso calc R 1 . H C18 .0086(2) .5634(2) .12105(13) .0313(5) Uani d . 1 . C H18 .1030 .5536 .10925 .038 Uiso calc R 1 . H C19 -.2974(3) .7589(2) .08579(13) .0336(5) Uani d . 1 . C H19A -.4014 .7479 .08764 .040 Uiso calc R 1 . H H19B -.2839 .7703 .03570 .040 Uiso calc R 1 . H C20 -.2485(3) .8535(2) .12957(14) .0363(6) Uani d . 1 . C H20A -.1439 .8632 .12854 .044 Uiso calc R 1 . H H20B -.2635 .8420 .17945 .044 Uiso calc R 1 . H C21 -.3283(3) .9509(2) .10309(14) .0376(6) Uani d . 1 . C H21A -.4332 .9406 .10214 .045 Uiso calc R 1 . H H21B -.2992 1.0052 .13727 .045 Uiso calc R 1 . H C22 -.2980(3) .9845(2) .0284(2) .0504(7) Uani d . 1 . C H22A -.3414 1.0502 .0175 .076 Uiso calc R 1 . H H22B -.3397 .9360 -.0070 .076 Uiso calc R 1 . H H22C -.1938 .9886 .0274 .076 Uiso calc R 1 . H O5 .2493(2) .56019(13) .00235(9) .0398(4) Uani d . 1 . O C23 .3806(3) .6143(2) .0010(2) .0510(7) Uani d . 1 . C H23A .4246 .5948 -.0409 .076 Uiso calc R 1 . H H23B .4469 .5991 .0437 .076 Uiso calc R 1 . H H23C .3602 .6860 -.0009 .076 Uiso calc R 1 . H H1 .2647 .4609 .0415 .044 Uiso calc R 1 . H H2 .1818 .5991 -.0350 .048 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 O1 .0490(10) .0339(10) .0427(10) .0038(8) -.0068(8) -.0058(8) O2 .0397(9) .0319(9) .0471(10) -.0012(7) -.0107(8) -.0033(8) O3 .0417(9) .0338(10) .0399(10) -.0055(8) .0014(8) .0031(8) O4 .0426(9) .0359(9) .0311(9) .0008(8) .0016(7) .0024(8) N1 .0264(9) .0238(10) .0343(10) .0011(7) .0003(8) -.0004(8) C1 .0344(12) .0233(11) .0433(14) .0000(10) .0000(10) .0012(11) C2 .0329(12) .0312(13) .0436(14) .0013(10) .0079(10) .0089(11) C3 .0294(11) .0332(13) .0321(12) .0015(10) .0027(9) .0041(10) C4 .0263(11) .0330(12) .0375(13) .0027(10) .0007(9) .0038(11) C5 .0305(12) .0306(12) .0322(12) .0044(10) .0033(9) .0029(10) C6 .0414(13) .0258(12) .0390(13) .0046(10) .0021(11) .0004(10) C7 .047(2) .0290(13) .069(2) -.0066(12) -.0047(14) .0034(13) C8 .0400(14) .051(2) .0335(13) .0088(12) .0049(10) .0065(12) C9 .0248(11) .0328(13) .0347(13) .0022(10) .0058(9) .0000(11) C10 .0381(14) .0442(15) .050(2) .0127(12) .0115(12) .0089(13) C11 .0287(11) .0305(12) .0311(12) -.0012(9) .0035(9) -.0003(10) C12 .0286(11) .0274(12) .0410(13) -.0037(9) .0022(10) .0020(11) C13 .0291(11) .0255(11) .0308(12) .0026(9) .0013(9) -.0008(10) C14 .0330(12) .0357(13) .0341(12) .0014(10) .0089(10) .0039(11) C15 .0289(11) .0371(13) .0369(13) .0055(10) .0059(10) -.0030(11) C16 .0302(11) .0277(12) .0334(12) .0027(9) -.0006(9) -.0038(10) C17 .0309(12) .0270(12) .0380(13) -.0012(9) .0019(10) .0015(10) C18 .0252(11) .0292(12) .0398(13) -.0005(9) .0051(9) -.0028(11) C19 .0320(12) .0311(12) .0359(13) .0036(10) -.0022(10) -.0029(11) C20 .0384(13) .0309(13) .0381(13) .0014(10) -.0003(10) -.0021(11) C21 .0367(13) .0277(12) .0472(15) .0003(10) .0013(11) -.0026(11) C22 .055(2) .040(2) .054(2) .0008(13) .0003(13) .0069(14) O5 .0333(9) .0401(10) .0449(10) -.0071(8) .0013(7) .0104(8) C23 .0367(14) .049(2) .065(2) -.0099(13) -.0027(13) .0140(15) 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 O1 C11 . 1.206(3) no O2 C12 . 1.222(3) no O3 C9 . 1.206(3) no O4 C9 . 1.336(3) no N1 C12 . 1.394(3) no N1 C11 . 1.414(3) no N1 C13 . 1.454(3) no C1 C12 . 1.513(3) no C1 C2 . 1.523(3) no C1 C7 . 1.528(3) no C1 C6 . 1.545(3) no C2 C3 . 1.516(3) no C3 C11 . 1.522(3) no C3 C8 . 1.534(3) no C3 C4 . 1.544(3) no C4 C5 . 1.531(3) no C5 C9 . 1.532(3) no C5 C6 . 1.541(3) no C5 C10 . 1.550(3) no C13 C18 . 1.383(3) no C13 C14 . 1.384(3) no C14 C15 . 1.387(3) no C15 C16 . 1.390(3) no C16 C17 . 1.396(3) no C16 C19 . 1.505(3) no C17 C18 . 1.386(3) no C19 C20 . 1.522(3) no C20 C21 . 1.524(3) no C21 C22 . 1.521(4) no O5 C23 . 1.401(3) no