#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200226.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_2200226 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o258 _journal_page_last o260 _publ_section_title ; meso-Octacyclopropylcalix[4]pyrrole ethanol solvate ; loop_ _publ_author_name 'Camiolo, Salvatore' 'Coles, Simon J.' 'Gale, Philip A.' 'Hursthouse, Michael B.' 'Paver, Michael A.' _chemical_formula_moiety 'C46 H58 N4 O' _chemical_formula_sum 'C46 H58 N4 O' _chemical_formula_iupac 'C44 H52 N4, C2 H6 O' _chemical_formula_weight 682.96 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.908(5) _cell_length_b 7.6861(15) _cell_length_c 22.947(5) _cell_angle_alpha 90 _cell_angle_beta 114.31(3) _cell_angle_gamma 90 _cell_volume 3843.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.180 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 N1 -.1041(5) .0915(15) .2239(5) .056(3) Uani d . 1 . . N H1 -.0821 -.0046 .2328 .067 Uiso calc R 1 . . H N2 .0200(5) .1262(16) .3564(5) .058(4) Uani d . 1 C . N H2 .0196 .2207 .3346 .07 Uiso calc R 1 . . H C1 -.1348(6) .082(2) .1034(7) .071(5) Uani d . 1 . . C C2 -.1628(8) .217(3) .0479(7) .094(7) Uani d . 1 . . C H2A -.2059 .2497 .0392 .113 Uiso calc R 1 . . H C3 -.1274(9) .363(4) .0347(9) .119(9) Uani d . 1 . . C H3A -.1482 .4771 .0215 .142 Uiso calc R 1 . . H H3B -.0826 .3695 .0609 .142 Uiso calc R 1 . . H C4 -.1511(10) .215(4) -.0096(9) .140(11) Uani d . 1 . . C H4A -.1863 .2374 -.051 .168 Uiso calc R 1 . . H H4B -.121 .13 -.0117 .168 Uiso calc R 1 . . H C5 -.1773(9) -.069(3) .0794(11) .106(7) Uani d . 1 . . C H5 -.1837 -.1074 .0355 .127 Uiso calc R 1 . . H C6 -.2334(9) -.095(3) .0945(11) .116(8) Uani d . 1 . . C H6A -.24 -.0127 .1241 .139 Uiso calc R 1 . . H H6B -.2712 -.1435 .0605 .139 Uiso calc R 1 . . H C7 -.1791(10) -.204(3) .1193(11) .114(8) Uani d . 1 . . C H7A -.1521 -.1941 .1654 .137 Uiso calc R 1 . . H H7B -.183 -.3241 .1022 .137 Uiso calc R 1 . . H C8 -.1336(6) .162(2) .1630(6) .057(4) Uani d . 1 . . C C9 -.1622(7) .308(2) .1705(7) .074(5) Uani d . 1 . . C H9 -.1862 .3847 .1373 .089 Uiso calc R 1 . . H C10 -.1505(7) .325(2) .2346(7) .071(5) Uani d . 1 . . C H10 -.1657 .416 .2522 .085 Uiso calc R 1 . . H C11 -.1139(6) .1923(19) .2682(6) .054(4) Uani d . 1 . . C C12 -.0917(7) .148(2) .3378(6) .060(4) Uani d . 1 C . C C13 -.1372(7) .032(2) .3503(7) .073(5) Uani d . 1 . . C H13 -.1246 .0041 .3966 .088 Uiso calc R 1 . . H C14 -.2048(8) .050(3) .3138(10) .107(7) Uani d . 1 . . C H14A -.2309 .0401 .3378 .129 Uiso calc R 1 . . H H14B -.2198 .1331 .2777 .129 Uiso calc R 1 . . H C15 -.1729(8) -.108(3) .3070(10) .099(7) Uani d . 1 . . C H15A -.1793 -.2171 .3266 .119 Uiso calc R 1 . . H H15B -.1682 -.1243 .2665 .119 Uiso calc R 1 . . H C16 -.0855(13) .321(3) .3753(8) .113(9) Uani d . 1 . . C H16 -.1287 .3613 .3628 .135 Uiso calc R 1 A 1 H C17 -.0571(11) .339(3) .4431(8) .123(9) Uani d . 1 C . C H17A -.0216 .264 .4678 .148 Uiso calc R 1 B 1 H H17B -.0827 .3761 .4656 .148 Uiso calc R 1 B 1 H C18 -.0528(16) .463(5) .3901(15) .077(11) Uani d P .5 C 1 C H18A -.0747 .5755 .3822 .093 Uiso calc PR .5 C 1 H H18B -.0139 .4639 .3844 .093 Uiso calc PR .5 C 1 H C18' -.116(2) .407(8) .400(2) .148(18) Uani d P .5 C 2 C C19 -.0307(6) .059(2) .3623(7) .064(5) Uani d . 1 . . C C20 -.0104(8) -.086(3) .3990(10) .113(7) Uani d . 1 C . C H20 -.0349 -.1612 .4116 .136 Uiso calc R 1 . . H C21 .0520(9) -.105(3) .4151(10) .120(7) Uani d . 1 . . C H21 .0772 -.1964 .4404 .144 Uiso calc R 1 C . H C22 .0710(7) .028(2) .3887(7) .076(5) Uani d . 1 . . C O01 0 .386(3) .25 .066(4) Uani d SPU .5 . 1 O H01 .0363 .3492 .2647 .099 Uiso calc PR .25 . 1 H C01 0 .539(14) .25 .225(5) Uani d SPU .5 . 1 C H01A -.0252 .5543 .2037 .271 Uiso calc PR .25 . 1 H H01B .0426 .5544 .2541 .271 Uiso calc PR .25 . 1 H C02 -.007(7) -.318(14) .266(7) .177(5) Uani d PU .25 . 1 C H02A -.0331 -.3229 .2894 .265 Uiso calc PR .25 . 1 H H02B -.0258 -.244 .2284 .265 Uiso calc PR .25 . 1 H H02C .0334 -.2698 .2942 .265 Uiso calc PR .25 . 1 H O02 0 -.174(6) .25 .129(5) Uani d SPU .5 . 2 O H02 -.0027 -.1732 .2123 .194 Uiso calc PR .25 . 2 H C01' 0 .535(17) .25 .220(5) Uani d SPU .5 . 2 C H01C .0088 .4536 .2221 .329 Uiso calc PR .25 . 2 H H01D -.0417 .5155 .2466 .329 Uiso calc PR .25 . 2 H H01E .0294 .5173 .2944 .329 Uiso calc PR .25 . 2 H C02' -.004(11) -.320(18) .266(9) .192(5) Uani d PU .25 . 2 C H02D .0246 -.3201 .3114 .23 Uiso calc PR .25 . 2 H H02E -.0456 -.3201 .266 .23 Uiso calc PR .25 . 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 N1 .041(6) .062(7) .058(6) .003(5) .014(5) -.001(5) N2 .041(6) .080(8) .048(6) -.006(6) .014(5) .018(5) C1 .035(8) .109(11) .063(8) -.006(8) .015(6) -.028(8) C2 .046(9) .184(18) .040(8) .018(11) .005(7) -.010(10) C3 .071(12) .22(2) .065(10) .010(14) .026(9) .042(13) C4 .084(13) .28(3) .050(10) .038(18) .019(9) -.016(15) C5 .076(12) .128(16) .112(14) -.017(12) .036(10) -.024(12) C6 .047(11) .159(19) .133(17) -.017(12) .028(11) -.028(14) C7 .105(15) .117(15) .114(15) -.003(13) .039(12) -.017(13) C8 .034(7) .091(10) .043(7) .006(7) .011(5) -.001(7) C9 .066(9) .104(11) .051(8) .034(9) .024(7) .018(8) C10 .072(9) .094(10) .052(7) .037(8) .031(6) .008(7) C11 .042(7) .073(9) .049(7) .000(7) .021(6) .000(7) C12 .048(8) .083(10) .048(7) -.007(7) .020(6) .006(7) C13 .044(8) .119(13) .059(8) -.011(8) .024(6) .011(9) C14 .049(9) .18(2) .100(12) -.002(12) .039(8) .027(13) C15 .083(11) .127(15) .097(11) -.041(11) .048(9) -.001(11) C16 .16(2) .111(15) .053(10) .001(14) .025(11) -.007(10) C17 .116(15) .20(2) .057(10) -.001(16) .043(10) -.029(12) C18 .07(2) .08(2) .08(2) -.004(17) .022(16) -.019(17) C18' .12(3) .24(5) .13(2) -.02(3) .09(2) -.09(3) C19 .040(8) .090(10) .059(8) -.008(7) .017(6) .027(7) C20 .056(10) .145(14) .136(13) .005(11) .038(9) .089(11) C21 .056(10) .158(14) .140(13) .015(11) .035(9) .107(11) C22 .042(8) .113(12) .065(8) .006(9) .015(7) .037(9) O01 .081(6) .053(6) .065(6) 0 .031(4) 0 C01 .327(6) .123(7) .300(7) 0 .204(4) 0 C02 .294(6) .093(7) .193(7) -.003(5) .149(4) .000(5) O02 .122(6) .104(6) .147(7) 0 .041(4) 0 C01' .319(6) .136(7) .296(7) 0 .219(4) 0 C02' .319(6) .106(7) .190(7) -.002(5) .146(4) .000(5) 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 N1 C11 . 1.374(19) ? N1 C8 . 1.391(17) ? N2 C22 . 1.365(19) ? N2 C19 . 1.374(19) ? C1 C5 . 1.49(3) ? C1 C8 . 1.49(2) ? C1 C22 2 1.52(2) ? C1 C2 . 1.56(2) ? C2 C4 . 1.46(3) ? C2 C3 . 1.51(3) ? C3 C4 . 1.48(3) ? C5 C7 . 1.40(3) ? C5 C6 . 1.53(3) ? C6 C7 . 1.45(3) ? C8 C9 . 1.36(2) ? C9 C10 . 1.39(2) ? C10 C11 . 1.36(2) ? C11 C12 . 1.501(19) ? C12 C19 . 1.49(2) ? C12 C13 . 1.52(2) ? C12 C16 . 1.56(3) ? C13 C15 . 1.47(2) ? C13 C14 . 1.49(2) ? C14 C15 . 1.48(3) ? C16 C18' . 1.28(5) ? C16 C18 . 1.30(4) ? C16 C17 . 1.42(3) ? C17 C18' . 1.44(5) ? C17 C18 . 1.58(4) ? C19 C20 . 1.36(2) ? C20 C21 . 1.39(3) ? C21 C22 . 1.36(3) ? C22 C1 2 1.52(2) ? O01 C01 . 1.18(11) ? C01 C02 1_565 1.19(15) ? C02 C01 1_545 1.19(15) ? O02 C02' . 1.20(15) ? C01' C02' 2_565 1.19(18) ? C02' C01' 1_545 1.19(18) ?