#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2012461.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_2012461 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first o39 _journal_page_last o41 _publ_section_title ; The supramolecular structures of 5-(3-(4-methylphenyl)- and 5-(3-(4-chlorophenyl)-2-propenylidene]-2,2-dimethyl-[1,3] dioxane-4,6-dione ; loop_ _publ_author_name 'Low, John Nicolson' 'Cobo, Justo' 'Nogueras, Manuel' "S\'anchez, Adolfo" 'Insuasty, Braulio' 'Torres, Harlen' _chemical_formula_moiety 'C16 H16 O4' _chemical_formula_sum 'C16 H16 O4' _chemical_formula_weight 272.29 _chemical_melting_point 401 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2891(3) _cell_length_b 11.4128(4) _cell_length_c 13.4504(5) _cell_angle_alpha 91.217(2) _cell_angle_beta 114.640(3) _cell_angle_gamma 113.7590(15) _cell_volume 1403.88(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(10) _exptl_crystal_density_diffrn 1.288 _diffrn_ambient_temperature 120.0(10) 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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O11 .25428(17) .07135(15) .57136(13) .0359(4) Uani d . 1 . . O C12 .3651(2) .0548(2) .55603(18) .0327(6) Uani d . 1 . . C C121 .4221(3) .1634(2) .5019(2) .0412(6) Uani d . 1 . . C C122 .4809(3) .0560(2) .66668(18) .0426(6) Uani d . 1 . . C O13 .30146(16) -.06671(14) .47684(11) .0320(4) Uani d . 1 . . O C14 .2119(2) -.1784(2) .49390(17) .0288(5) Uani d . 1 . . C O14 .19023(17) -.28312(16) .44886(12) .0378(4) Uani d . 1 . . O C15 .1453(2) -.1604(2) .56262(16) .0275(5) Uani d . 1 . . C C16 .1585(2) -.0295(2) .59303(17) .0304(5) Uani d . 1 . . C O16 .08966(18) -.00424(16) .63185(13) .0412(4) Uani d . 1 . . O C17 .0672(2) -.2682(2) .59001(16) .0297(5) Uani d . 1 . . C C18 -.0094(2) -.2771(2) .65323(17) .0302(5) Uani d . 1 . . C C19 -.0818(2) -.3936(2) .67307(16) .0294(5) Uani d . 1 . . C C191 -.1641(2) -.4159(2) .73519(16) .0261(5) Uani d . 1 . . C C192 -.1893(2) -.3190(2) .77604(17) .0289(5) Uani d . 1 . . C C193 -.2664(2) -.3448(2) .83681(16) .0301(5) Uani d . 1 . . C C194 -.3221(2) -.4687(2) .85977(16) .0275(5) Uani d . 1 . . C C91 -.4076(3) -.4976(2) .92450(18) .0358(6) Uani d . 1 . . C C195 -.2986(2) -.5650(2) .81877(17) .0307(5) Uani d . 1 . . C C196 -.2230(2) -.5409(2) .75661(17) .0298(5) Uani d . 1 . . C O21 -.31404(16) -.06950(14) .89824(12) .0312(4) Uani d . 1 . . O C22 -.2865(3) -.0430(2) 1.01284(18) .0325(6) Uani d . 1 . . C C221 -.4148(3) -.1473(2) 1.0201(2) .0500(7) Uani d . 1 . . C C222 -.1419(3) -.0383(2) 1.09044(18) .0384(6) Uani d . 1 . . C O23 -.28717(17) .08017(14) 1.03894(12) .0344(4) Uani d . 1 . . O C24 -.2123(2) .1856(2) 1.00726(17) .0282(5) Uani d . 1 . . C O24 -.19663(17) .29170(15) 1.04345(12) .0363(4) Uani d . 1 . . O C25 -.1633(2) .1603(2) .92736(16) .0262(5) Uani d . 1 . . C C26 -.2246(2) .0246(2) .86595(17) .0282(5) Uani d . 1 . . C O26 -.20926(17) -.00941(15) .78898(12) .0383(4) Uani d . 1 . . O C27 -.0675(2) .2672(2) .91029(16) .0279(5) Uani d . 1 . . C C28 -.0046(2) .2744(2) .83730(17) .0278(5) Uani d . 1 . . C C29 .0899(2) .3936(2) .83520(17) .0289(5) Uani d . 1 . . C C291 .1671(2) .4208(2) .76888(16) .0272(5) Uani d . 1 . . C C292 .1696(2) .3235(2) .70598(17) .0304(5) Uani d . 1 . . C C293 .2447(2) .3554(2) .64403(17) .0326(5) Uani d . 1 . . C C294 .3214(2) .4858(2) .64154(17) .0330(6) Uani d . 1 . . C C92 .4030(3) .5200(3) .57376(19) .0442(7) Uani d . 1 . . C C295 .3203(2) .5827(2) .70421(18) .0349(6) Uani d . 1 . . C C296 .2457(2) .5523(2) .76738(17) .0305(5) Uani d . 1 . . C H12A .4569 .2485 .5492 .062 Uiso calc R 1 . . H H12B .3436 .1520 .4279 .062 Uiso calc R 1 . . H H12C .5031 .1604 .4935 .062 Uiso calc R 1 . . H H12D .4368 -.0182 .6960 .064 Uiso calc R 1 . . H H12E .5230 .1385 .7205 .064 Uiso calc R 1 . . H H12F .5581 .0486 .6552 .064 Uiso calc R 1 . . H H17 .0632 -.3482 .5635 .036 Uiso calc R 1 . . H H18 -.0096 -.2004 .6818 .036 Uiso calc R 1 . . H H19 -.0783 -.4678 .6434 .035 Uiso calc R 1 . . H H192 -.1526 -.2339 .7617 .035 Uiso calc R 1 . . H H193 -.2818 -.2772 .8635 .036 Uiso calc R 1 . . H H91A -.3994 -.5691 .9614 .054 Uiso calc R 1 . . H H91B -.5106 -.5238 .8730 .054 Uiso calc R 1 . . H H91C -.3687 -.4187 .9814 .054 Uiso calc R 1 . . H H195 -.3353 -.6498 .8336 .037 Uiso calc R 1 . . H H196 -.2108 -.6098 .7281 .036 Uiso calc R 1 . . H H22A -.4230 -.2340 .9991 .075 Uiso calc R 1 . . H H22B -.5045 -.1431 .9687 .075 Uiso calc R 1 . . H H22C -.4007 -.1327 1.0971 .075 Uiso calc R 1 . . H H22D -.0633 .0341 1.0835 .058 Uiso calc R 1 . . H H22E -.1423 -.1216 1.0703 .058 Uiso calc R 1 . . H H22F -.1259 -.0244 1.1681 .058 Uiso calc R 1 . . H H27 -.0385 .3495 .9540 .033 Uiso calc R 1 . . H H28 -.0283 .1966 .7904 .033 Uiso calc R 1 . . H H29 .1072 .4677 .8828 .035 Uiso calc R 1 . . H H292 .1186 .2339 .7059 .037 Uiso calc R 1 . . H H293 .2444 .2872 .6021 .039 Uiso calc R 1 . . H H92D .5075 .5509 .6235 .066 Uiso calc R 1 . . H H92E .3882 .5895 .5367 .066 Uiso calc R 1 . . H H92F .3664 .4419 .5169 .066 Uiso calc R 1 . . H H295 .3717 .6721 .7040 .042 Uiso calc R 1 . . H H296 .2477 .6210 .8101 .037 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 O11 .0376(10) .0269(9) .0520(10) .0126(8) .0304(8) .0116(7) C12 .0330(13) .0243(13) .0447(14) .0095(11) .0249(11) .0057(10) C121 .0392(15) .0342(15) .0573(15) .0132(12) .0317(13) .0153(12) C122 .0333(14) .0381(16) .0424(14) .0096(12) .0120(12) .0035(11) O13 .0333(9) .0273(9) .0366(9) .0089(8) .0220(7) .0071(7) C14 .0237(12) .0302(14) .0302(12) .0094(11) .0132(10) .0066(10) O14 .0405(10) .0286(10) .0467(10) .0109(8) .0272(8) .0024(7) C15 .0243(12) .0275(13) .0292(11) .0090(10) .0139(10) .0042(9) C16 .0309(13) .0308(14) .0306(12) .0118(11) .0174(10) .0091(10) O16 .0507(11) .0340(10) .0567(10) .0206(9) .0386(9) .0139(8) C17 .0256(12) .0277(13) .0309(12) .0084(11) .0128(10) .0022(9) C18 .0276(13) .0284(14) .0328(12) .0094(11) .0158(10) .0031(10) C19 .0260(12) .0274(14) .0312(12) .0086(11) .0138(10) .0033(9) C191 .0208(11) .0254(13) .0258(11) .0064(10) .0095(9) .0044(9) C192 .0280(12) .0201(13) .0327(12) .0061(10) .0137(10) .0037(9) C193 .0314(13) .0256(13) .0315(12) .0103(11) .0158(10) .0006(9) C194 .0247(12) .0270(13) .0256(11) .0081(10) .0107(9) .0055(9) C91 .0336(13) .0397(15) .0370(13) .0147(12) .0205(11) .0111(11) C195 .0297(13) .0242(13) .0362(12) .0098(11) .0159(10) .0102(10) C196 .0302(13) .0243(13) .0377(12) .0124(11) .0181(10) .0075(10) O21 .0300(9) .0217(9) .0387(9) .0077(7) .0174(7) .0055(6) C22 .0406(14) .0232(13) .0443(14) .0150(11) .0281(12) .0114(10) C221 .0569(18) .0269(15) .0816(19) .0129(13) .0510(16) .0173(13) C222 .0496(16) .0335(15) .0372(13) .0228(13) .0206(12) .0122(11) O23 .0412(10) .0221(9) .0536(10) .0136(8) .0343(8) .0128(7) C24 .0257(12) .0250(14) .0355(12) .0123(11) .0148(10) .0076(10) O24 .0450(10) .0239(10) .0498(10) .0154(8) .0305(8) .0088(7) C25 .0240(12) .0238(13) .0321(12) .0112(10) .0138(10) .0077(9) C26 .0243(12) .0264(13) .0334(12) .0119(11) .0127(10) .0092(10) O26 .0453(11) .0326(10) .0377(9) .0147(8) .0231(8) .0036(7) C27 .0299(12) .0254(13) .0311(12) .0152(11) .0139(10) .0074(9) C28 .0299(13) .0274(13) .0325(12) .0153(11) .0177(10) .0081(9) C29 .0294(13) .0288(14) .0344(12) .0156(11) .0174(10) .0087(10) C291 .0223(11) .0274(13) .0305(11) .0105(10) .0118(9) .0083(9) C292 .0276(13) .0255(13) .0359(12) .0117(11) .0131(10) .0059(10) C293 .0323(13) .0368(15) .0307(12) .0169(12) .0154(10) .0042(10) C294 .0282(13) .0428(16) .0304(12) .0164(12) .0151(10) .0113(10) C92 .0386(15) .0576(18) .0410(14) .0187(14) .0253(12) .0138(12) C295 .0332(14) .0302(14) .0441(14) .0118(12) .0226(11) .0160(11) C296 .0314(13) .0257(13) .0388(13) .0139(11) .0193(11) .0081(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 O11 C16 . 1.361(3) no O11 C12 . 1.431(3) no C12 O13 . 1.439(3) no C12 C121 . 1.505(3) no C12 C122 . 1.512(3) no C121 H12A . .9800 no C121 H12B . .9800 no C121 H12C . .9800 no C122 H12D . .9800 no C122 H12E . .9800 no C122 H12F . .9800 no O13 C14 . 1.366(3) no C14 O14 . 1.210(3) no C14 C15 . 1.469(3) no C15 C17 . 1.358(3) no C15 C16 . 1.471(3) no C16 O16 . 1.213(2) no C17 C18 . 1.424(3) no C17 H17 . .9500 no C18 C19 . 1.352(3) no C18 H18 . .9500 no C19 C191 . 1.447(3) no C19 H19 . .9500 no C191 C192 . 1.401(3) no C191 C196 . 1.404(3) no C192 C193 . 1.382(3) no C192 H192 . .9500 no C193 C194 . 1.398(3) no C193 H193 . .9500 no C194 C195 . 1.383(3) no C194 C91 . 1.502(3) no C91 H91A . .9800 no C91 H91B . .9800 no C91 H91C . .9800 no C195 C196 . 1.386(3) no C195 H195 . .9500 no C196 H196 . .9500 no O21 C26 . 1.369(3) no O21 C22 . 1.438(2) no C22 O23 . 1.445(3) no C22 C221 . 1.503(3) no C22 C222 . 1.504(3) no C221 H22A . .9800 no C221 H22B . .9800 no C221 H22C . .9800 no C222 H22D . .9800 no C222 H22E . .9800 no C222 H22F . .9800 no O23 C24 . 1.359(3) no C24 O24 . 1.210(2) no C24 C25 . 1.469(3) no C25 C27 . 1.367(3) no C25 C26 . 1.471(3) no C26 O26 . 1.200(2) no C27 C28 . 1.418(3) no C27 H27 . .9500 no C28 C29 . 1.359(3) no C28 H28 . .9500 no C29 C291 . 1.447(3) no C29 H29 . .9500 no C291 C292 . 1.398(3) no C291 C296 . 1.408(3) no C292 C293 . 1.379(3) no C292 H292 . .9500 no C293 C294 . 1.397(3) no C293 H293 . .9500 no C294 C295 . 1.384(3) no C294 C92 . 1.503(3) no C92 H92D . .9800 no C92 H92E . .9800 no C92 H92F . .9800 no C295 C296 . 1.387(3) no C295 H295 . .9500 no C296 H296 . .9500 no _cod_database_code 2012461