#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006547.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_2006547 _journal_name_full 'Acta Crystallographica' _journal_year 1997 _journal_volume C53 _journal_page_first 1495 _journal_page_last 1497 _publ_section_title ; The Cone Conformer of a Tetrakis(methylthio)tetrapropoxycalix[4]arene ; loop_ _publ_author_name 'Schultz, Thomas M.' 'Hazell, Rita G. ' 'Larsen, Mogens' _chemical_formula_sum 'C44 H56 O4 S4' _chemical_formula_weight 777.20 _chemical_melting_point '178-179\%C' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2+x,1/2-y,1/2+z' '-x,-y,-z' '1/2-x,1/2+y,1/2-z' _cell_length_a 12.479(3) _cell_length_b 27.145(8) _cell_length_c 12.591(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.400(10) _cell_angle_gamma 90.00 _cell_volume 4230(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _exptl_crystal_density_diffrn 1.22 _diffrn_ambient_temperature 120 _refine_ls_R_factor_obs .057 _refine_ls_wR_factor_obs .067 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_occupancy S1 1.12876(9) .45076(4) .55145(10) .0405(7) Uij 1.00 S2 .54928(10) .41612(5) .50420(10) .0449(7) Uij 1.00 S3 .18564(9) .39126(5) .05310(12) .0485(8) Uij 1.00 S4 .60981(8) .51658(4) .26562(9) .0323(6) Uij 1.00 O1 .8694(2) .33610(10) .2096(2) .032(2) Uij 1.00 O2 .7209(2) .24870(10) .2740(2) .031(2) Uij 1.00 O3 .6291(2) .31220(10) .0606(2) .034(2) Uij 1.00 O4 .8129(2) .39140(10) -.0388(2) .034(2) Uij 1.00 C1 .8268(3) .43940(10) .1217(3) .027(2) Uij 1.00 C2 .9477(3) .4283(2) .1483(4) .033(2) Uij 1.00 C3 .9737(3) .4083(2) .2597(3) .030(2) Uij 1.00 C4 1.0353(3) .4355(2) .3394(4) .032(2) Uij 1.00 C5 1.0492(3) .4195(2) .4447(4) .031(2) Uij 1.00 C6 .9969(3) .3766(2) .4721(4) .033(2) Uij 1.00 C7 .9348(3) .34860(10) .3940(4) .031(2) Uij 1.00 C8 .8694(3) .3049(2) .4235(4) .034(2) Uij 1.00 C9 .7483(3) .31570(10) .3996(3) .029(2) Uij 1.00 C10 .7052(3) .3548(2) .4521(3) .031(2) Uij 1.00 C11 .5954(3) .3669(2) .4295(3) .030(2) Uij 1.00 C12 .5302(3) .34080(10) .3520(3) .029(2) Uij 1.00 C13 .5718(3) .30150(10) .2987(3) .029(2) Uij 1.00 C14 .4992(3) .27520(10) .2100(3) .031(2) Uij 1.00 C15 .4566(3) .31160(10) .1241(3) .029(2) Uij 1.00 C16 .3532(3) .33170(10) .1202(3) .030(2) Uij 1.00 C17 .3198(3) .3700(2) .0511(3) .029(2) Uij 1.00 C18 .3909(3) .39000(10) -.0140(3) .029(2) Uij 1.00 C19 .4949(3) .37070(10) -.0116(3) .026(2) Uij 1.00 C20 .5785(3) .3980(2) -.0677(3) .028(2) Uij 1.00 C21 .6519(3) .42600(10) .0172(3) .025(2) Uij 1.00 C22 .6052(3) .45630(10) .0882(3) .025(2) Uij 1.00 C23 .6670(3) .47790(10) .1746(3) .028(2) Uij 1.00 C24 .7777(3) .46810(10) .1938(3) .027(2) Uij 1.00 C25 .9297(3) .3635(2) .2868(3) .030(2) Uij 1.00 C26 .6800(3) .28850(10) .3252(3) .028(2) Uij 1.00 C27 .5251(3) .33070(10) .0548(3) .026(2) Uij 1.00 C28 .7641(3) .41970(10) .0336(3) .027(2) Uij 1.00 C29 1.1749(4) .5046(2) .4888(4) .047(3) Uij 1.00 C30 .4053(4) .4108(2) .4778(4) .050(3) Uij 1.00 C31 .1808(4) .4464(2) -.0184(6) .067(4) Uij 1.00 C32 .4744(4) .4922(2) .2593(4) .041(3) Uij 1.00 C33a .9248(10) .3114(6) .1299(14) .042(8) Uij .42(2) C34a 1.0231(12) .2843(6) .1800(16) .055(10) Uij .42 C35 1.0627(5) .2493(2) .0921(5) .066(4) Uij 1.00 C36 .7081(4) .2029(2) .3279(4) .041(3) Uij 1.00 C37 .7305(6) .1612(2) .2557(5) .069(4) Uij 1.00 C38 .8432(8) .1618(2) .2243(5) .091(6) Uij 1.00 C39a .6645(11) .2890(5) -.0323(9) .045(7) Uij .50(2) C40a .6734(10) .2354(4) -.0160(8) .040(7) Uij .50 C39b .6300(11) .2666(5) .0005(17) .080(12) Uij .50 C40b .7118(16) .2577(9) -.0533(19) .16(2) Uij .50 C41 .7281(6) .2115(2) -.1070(6) .081(5) Uij 1.00 C42 .8450(4) .4200(2) -.1249(4) .055(3) Uij 1.00 C43 .9039(7) .3871(3) -.1948(6) .093(6) Uij 1.00 C44 .8332(10) .3499(3) -.2488(7) .134(9) Uij 1.00 C33b .9212(7) .2889(4) .1865(9) .038(6) Uij .58 C34b 1.0060(8) .2962(4) .1136(11) .041(6) Uij .58 H2a .987 .458 .143 .039 Uiso 1.00 H2b .968 .405 .099 .039 Uiso 1.00 H4 1.068 .465 .321 .039 Uiso 1.00 H6 1.004 .366 .545 .040 Uiso 1.00 H8a .887 .298 .498 .041 Uiso 1.00 H8b .886 .277 .383 .041 Uiso 1.00 H10 .751 .373 .503 .037 Uiso 1.00 H12 .457 .350 .335 .035 Uiso 1.00 H14a .440 .261 .239 .038 Uiso 1.00 H14b .539 .250 .180 .038 Uiso 1.00 H16 .305 .319 .166 .036 Uiso 1.00 H18 .369 .417 -.060 .035 Uiso 1.00 H20a .543 .420 -.119 .034 Uiso 1.00 H20b .620 .375 -.103 .034 Uiso 1.00 H22 .529 .462 .077 .031 Uiso 1.00 H24 .820 .481 .256 .033 Uiso 1.00 H29a 1.217 .521 .546 .055 Uiso 1.00 H29b 1.116 .524 .459 .055 Uiso 1.00 H29c 1.217 .496 .434 .055 Uiso 1.00 H30a .380 .437 .518 .059 Uiso 1.00 H30b .381 .380 .502 .059 Uiso 1.00 H30c .381 .415 .403 .059 Uiso 1.00 H31a .109 .458 -.017 .082 Uiso 1.00 H31b .195 .441 -.090 .082 Uiso 1.00 H31c .232 .469 .016 .082 Uiso 1.00 H32a .444 .513 .308 .049 Uiso 1.00 H32b .475 .459 .281 .049 Uiso 1.00 H32c .437 .495 .189 .049 Uiso 1.00 H33aa .949 .337 .083 .051 Uiso .42 H33ab .877 .291 .087 .051 Uiso .42 H34aa 1.003 .264 .238 .084 Uiso .42 H34ab 1.079 .306 .209 .084 Uiso .42 H35aa 1.124 .232 .125 .081 Uiso .42 H35ab 1.084 .269 .036 .081 Uiso .42 H35ac 1.008 .228 .065 .081 Uiso .42 H36a .636 .200 .345 .050 Uiso 1.00 H36b .757 .202 .392 .050 Uiso 1.00 H37a .680 .163 .192 .082 Uiso 1.00 H37b .721 .131 .292 .082 Uiso 1.00 H38a .857 .135 .178 .108 Uiso 1.00 H38b .893 .160 .287 .108 Uiso 1.00 H38c .852 .192 .188 .108 Uiso 1.00 H39aa .732 .302 -.044 .059 Uiso .50 H39ab .612 .295 -.093 .059 Uiso .50 H40aa .604 .222 -.016 .051 Uiso .50 H40ab .716 .229 .051 .051 Uiso .50 H39ba .565 .265 -.047 .094 Uiso .50 H39bb .631 .240 .052 .094 Uiso .50 H40ba .775 .264 -.007 .193 Uiso .50 H40bb .704 .282 -.110 .193 Uiso .50 H41aa .735 .177 -.096 .098 Uiso .50 H41ba .798 .226 -.107 .098 Uiso .50 H41ca .686 .218 -.174 .098 Uiso .50 H41ab .786 .206 -.147 .098 Uiso .50 H41bb .664 .206 -.155 .098 Uiso .50 H41cb .735 .187 -.052 .098 Uiso .50 H42a .892 .446 -.096 .066 Uiso 1.00 H42b .783 .434 -.166 .066 Uiso 1.00 H43a .961 .371 -.152 .110 Uiso 1.00 H43b .932 .407 -.247 .110 Uiso 1.00 H44a .870 .329 -.293 .164 Uiso 1.00 H44b .775 .366 -.292 .164 Uiso 1.00 H44c .805 .330 -.197 .164 Uiso 1.00 H33ba .867 .268 .151 .054 Uiso .58 H33bb .953 .275 .251 .054 Uiso .58 H34ba 1.057 .319 .148 .093 Uiso .58 H34bb .973 .309 .049 .093 Uiso .58 H35ba 1.118 .254 .047 .081 Uiso .58 H35bb 1.012 .227 .059 .081 Uiso .58 H35bc 1.096 .236 .159 .081 Uiso .58 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 S1 .0354(6) .0384(7) .0435(7) -.0032(5) -.0107(5) -.0096(5) S2 .0434(7) .0511(8) .0403(7) .0089(6) .0057(5) -.0153(6) S3 .0230(6) .0447(7) .0800(10) .0057(5) .0150(6) .0150(7) S4 .0293(5) .0336(6) .0338(6) .0045(4) .0030(4) -.0078(5) O1 .0250(10) .034(2) .034(2) -.0020(10) -.0020(10) -.0080(10) O2 .034(2) .0200(10) .038(2) .0030(10) -.0010(10) -.0010(10) O3 .0240(10) .040(2) .037(2) .0100(10) .0030(10) -.0020(10) O4 .0270(10) .045(2) .031(2) .0010(10) .0110(10) -.0080(10) C1 .018(2) .030(2) .033(2) -.001(2) .003(2) .001(2) C2 .018(2) .039(2) .041(3) -.002(2) .004(2) -.005(2) C3 .018(2) .035(2) .035(2) .003(2) .001(2) -.008(2) C4 .020(2) .031(2) .045(3) .004(2) .001(2) -.005(2) C5 .020(2) .030(2) .042(3) .004(2) -.007(2) -.012(2) C6 .026(2) .031(2) .038(2) .009(2) -.004(2) -.007(2) C7 .018(2) .029(2) .043(3) .008(2) -.005(2) -.004(2) C8 .033(2) .027(2) .037(2) .002(2) -.009(2) -.001(2) C9 .028(2) .027(2) .030(2) .002(2) -.004(2) .005(2) C10 .037(2) .029(2) .024(2) -.002(2) -.003(2) -.002(2) C11 .034(2) .033(2) .024(2) .001(2) .002(2) .002(2) C12 .025(2) .030(2) .034(2) .001(2) .005(2) .004(2) C13 .029(2) .026(2) .028(2) -.006(2) -.001(2) .008(2) C14 .030(2) .026(2) .037(2) -.001(2) -.001(2) .003(2) C15 .027(2) .026(2) .031(2) -.003(2) -.001(2) -.002(2) C16 .027(2) .028(2) .034(2) -.006(2) .002(2) .000(2) C17 .019(2) .029(2) .040(2) .000(2) .001(2) .000(2) C18 .027(2) .026(2) .035(2) .000(2) .002(2) -.002(2) C19 .025(2) .027(2) .025(2) -.003(2) -.001(2) -.005(2) C20 .023(2) .035(2) .026(2) .000(2) .003(2) .001(2) C21 .022(2) .028(2) .026(2) -.003(2) .003(2) .003(2) C22 .021(2) .028(2) .028(2) .002(2) .004(2) .002(2) C23 .026(2) .028(2) .031(2) .001(2) .007(2) .003(2) C24 .023(2) .030(2) .028(2) -.002(2) .000(2) -.002(2) C25 .017(2) .032(2) .039(2) .004(2) -.004(2) -.010(2) C26 .029(2) .023(2) .030(2) .002(2) -.001(2) .003(2) C27 .022(2) .028(2) .027(2) .002(2) -.004(2) -.004(2) C28 .022(2) .033(2) .027(2) .003(2) .007(2) .001(2) C29 .038(3) .040(3) .056(3) -.003(2) -.016(2) -.006(2) C30 .046(3) .061(3) .047(3) .008(2) .018(2) -.007(3) C31 .040(3) .054(3) .112(5) .008(3) .027(3) .021(4) C32 .035(2) .045(3) .046(3) .000(2) .012(2) -.010(2) C33a .046(8) .039(8) .041(9) .001(6) .001(6) -.007(7) C34a .061(9) .064(9) .038(10) .024(7) .005(7) -.007(8) C35 .084(4) .062(4) .061(4) .018(3) .037(3) -.008(3) C36 .050(3) .023(2) .048(3) .000(2) -.001(2) .006(2) C37 .128(6) .022(2) .047(3) .005(3) -.022(3) -.001(2) C38 .172(8) .060(4) .043(3) .067(5) .026(4) .006(3) C39a .058(7) .045(8) .037(6) .013(6) .020(5) -.003(5) C40a .055(7) .029(7) .035(6) .006(5) -.002(5) -.001(5) C39b .062(8) .027(8) .166(16) -.009(6) .076(10) -.021(8) C40b .155(17) .143(18) .22(2) -.115(15) .174(19) -.134(17) C41 .082(4) .068(4) .100(6) .020(4) .033(4) -.028(4) C42 .057(3) .060(3) .054(3) -.003(3) .034(3) -.001(3) C43 .126(6) .106(6) .060(4) .017(5) .058(5) -.004(4) C44 .253(13) .099(7) .065(5) .046(8) .072(7) .000(5) C33b .046(5) .036(6) .029(6) -.006(4) .002(4) -.010(5) C34b .044(6) .043(5) .039(7) -.004(4) .014(5) .001(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 C5 1.780(4) yes S1 C29 1.790(5) yes S2 C11 1.772(4) yes S2 C30 1.790(5) yes S3 C17 1.774(4) no S3 C31 1.744(6) no S4 C23 1.771(4) no S4 C32 1.808(5) no O1 C25 1.369(5) yes O1 C33a 1.453(14) yes O1 C33b 1.481(10) yes O2 C26 1.390(5) yes O2 C36 1.434(5) yes O3 C27 1.385(4) no O3 C39a 1.446(11) no O3 C39b 1.452(14) no O4 C28 1.393(5) no O4 C42 1.431(6) no C1 C2 1.532(5) yes C1 C24 1.397(6) no C1 C28 1.380(6) no C2 C3 1.500(6) yes C3 C4 1.396(6) no C3 C25 1.394(6) no C4 C5 1.384(6) no C5 C6 1.400(6) no C6 C7 1.396(6) no C7 C8 1.513(6) yes C7 C25 1.403(6) no C8 C9 1.531(5) yes C9 C10 1.395(6) no C9 C26 1.395(6) no C10 C11 1.401(6) no C11 C12 1.383(6) no C12 C13 1.395(6) no C13 C14 1.522(6) no C13 C26 1.393(5) no C14 C15 1.508(6) no C15 C16 1.397(6) no C15 C27 1.397(6) no C16 C17 1.385(6) no C17 C18 1.393(6) no C18 C19 1.396(6) no C19 C20 1.526(5) no C19 C27 1.393(6) no C20 C21 1.518(5) no C21 C22 1.396(6) no C21 C28 1.399(5) no C22 C23 1.381(6) no C23 C24 1.397(5) no C33a C34a 1.50(3) no C34a C35 1.585(14) no C33b C34b 1.498(17) no C34b C35 1.501(11) no C36 C37 1.499(7) no C37 C38 1.510(10) no C39a C40a 1.47(2) no C40a C41 1.550(13) no C39b C40b 1.32(2) no C40b C41 1.450(19) no C42 C43 1.510(8) no C43 C44 1.450(13) no