#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2200073.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_2200073 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o28 _journal_page_last o29 _publ_section_title ; endo-(1'R, 2'R, 5'S, 7'R, 9'S)-2-(9'-Benzyloxy-2'-phenyl-3', 6'-dioxabicyclo[3.2.2]nonan-7'-yl)-7-bromo-5,8-dimethoxynaphthalen-1-yl acetate ; loop_ _publ_author_name 'Timothy J. Brenstrum' 'Margaret A. Brimble' 'Peter Turner' _chemical_formula_moiety 'C34 H33 Br O7' _chemical_formula_sum 'C34 H33 Br O7' _chemical_formula_weight 633.51 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 19.5150(10) _cell_length_b 23.667(2) _cell_length_c 6.541(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3021.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _exptl_crystal_density_diffrn 1.393 _diffrn_ambient_temperature 294(2) 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 Br1 .96750(3) .09686(3) -.05259(13) .0935(3) Uani d . 1 . . Br O1 .56407(16) .20795(14) .4274(6) .0644(9) Uani d . 1 . . O O2 .56036(17) .34224(14) .5699(7) .0745(11) Uani d . 1 . . O O3 .54484(19) .18553(15) .8661(7) .0843(12) Uani d . 1 . . O O4 .74688(16) .23284(14) .1453(5) .0595(8) Uani d . 1 . . O O5 .8305(2) .26370(16) .3496(7) .0776(11) Uani d . 1 . . O O6 .85879(17) .18547(15) -.0133(6) .0659(9) Uani d . 1 . . O O7 .8080(2) .00178(14) .4892(8) .0842(13) Uani d . 1 . . O C1 .6316(2) .2297(2) .3920(8) .0556(11) Uani d . 1 . . C H1 .6318 .2493 .2600 .067 Uiso calc R 1 . . H C2 .6533(2) .27178(17) .5577(8) .0519(11) Uani d . 1 . . C H2 .7035 .2722 .5597 .062 Uiso calc R 1 . . H C3 .6298(2) .25151(19) .7669(8) .0572(12) Uani d . 1 . . C H3A .6540 .2170 .8015 .069 Uiso calc R 1 . . H H3B .6414 .2798 .8685 .069 Uiso calc R 1 . . H C4 .5532(3) .2405(2) .7740(9) .0620(13) Uani d . 1 . . C H4 .5311 .2690 .8600 .074 Uiso calc R 1 . . H C5 .5235(2) .2429(2) .5625(9) .0629(13) Uani d . 1 . . C H5 .4779 .2256 .5699 .075 Uiso calc R 1 . . H C6 .5133(3) .3027(2) .4865(11) .0785(17) Uani d . 1 . . C H6A .5176 .3030 .3388 .094 Uiso calc R 1 . . H H6B .4671 .3147 .5199 .094 Uiso calc R 1 . . H C7 .6295(2) .33348(18) .5157(10) .0654(14) Uani d . 1 . . C H7 .6347 .3412 .3693 .078 Uiso calc R 1 . . H C8 .6720(3) .37487(19) .6311(11) .0693(15) Uani d . 1 . . C C9 .6497(3) .3983(2) .8139(12) .0847(19) Uani d . 1 . . C H9 .6066 .3891 .8641 .102 Uiso calc R 1 . . H C10 .6916(4) .4357(2) .9235(15) .102(2) Uani d . 1 . . C H10 .6758 .4519 1.0442 .123 Uiso calc R 1 . . H C11 .7563(4) .4484(3) .8520(17) .108(3) Uani d . 1 . . C H11 .7848 .4725 .9256 .130 Uiso calc R 1 . . H C12 .7783(4) .4252(3) .6719(17) .101(2) Uani d . 1 . . C H12 .8218 .4337 .6229 .122 Uiso calc R 1 . . H C13 .7367(3) .3898(2) .5638(13) .0831(18) Uani d . 1 . . C H13 .7524 .3751 .4405 .100 Uiso calc R 1 . . H C14 .6804(2) .17996(18) .3789(8) .0535(11) Uani d . 1 . . C C15 .6690(3) .13042(19) .4902(9) .0621(13) Uani d . 1 . . C H15 .6289 .1266 .5658 .075 Uiso calc R 1 . . H C16 .7157(3) .08766(19) .4899(10) .0668(14) Uani d . 1 . . C H16 .7082 .0560 .5709 .080 Uiso calc R 1 . . H C17 .7755(2) .09084(19) .3677(8) .0583(12) Uani d . 1 . . C C18 .8241(3) .04559(19) .3654(10) .0656(13) Uani d . 1 . . C C19 .8813(3) .0487(2) .2487(11) .0741(15) Uani d . 1 . . C H19 .9139 .0200 .2524 .089 Uiso calc R 1 . . H C20 .8904(2) .0960(2) .1220(8) .0632(12) Uani d . 1 . . C C21 .8461(2) .1404(2) .1148(8) .0555(11) Uani d . 1 . . C C22 .7869(2) .13918(18) .2459(8) .0502(11) Uani d . 1 . . C C23 .7386(2) .18412(19) .2630(8) .0532(11) Uani d . 1 . . C C24 .7972(3) .2688(2) .1991(10) .0674(14) Uani d . 1 . . C C25 .8021(3) .3149(3) .0407(14) .104(3) Uani d . 1 . . C H25A .8277 .3461 .0953 .156 Uiso calc R 1 . . H H25B .7569 .3275 .0047 .156 Uiso calc R 1 . . H H25C .8248 .3006 -.0788 .156 Uiso calc R 1 . . H C26 .8297(3) .1785(4) -.2147(9) .103(2) Uani d . 1 . . C H26A .8441 .1430 -.2708 .154 Uiso calc R 1 . . H H26B .8450 .2086 -.3017 .154 Uiso calc R 1 . . H H26C .7806 .1793 -.2054 .154 Uiso calc R 1 . . H C27 .8576(3) -.0429(2) .5058(13) .096(2) Uani d . 1 . . C H27A .8668 -.0581 .3725 .144 Uiso calc R 1 . . H H27B .8399 -.0722 .5925 .144 Uiso calc R 1 . . H H27C .8992 -.0283 .5633 .144 Uiso calc R 1 . . H C28 .4846(3) .1790(2) .9722(12) .0849(18) Uani d . 1 . . C H28A .4470 .1951 .8947 .102 Uiso calc R 1 . . H H28B .4875 .1986 1.1022 .102 Uiso calc R 1 . . H C29 .4722(3) .1169(2) 1.0074(9) .0675(14) Uani d . 1 . . C C30 .4775(3) .0943(3) 1.2008(10) .0789(16) Uani d . 1 . . C H30 .4909 .1173 1.3092 .095 Uiso calc R 1 . . H C31 .4632(4) .0379(3) 1.2355(12) .0911(19) Uani d . 1 . . C H31 .4657 .0231 1.3670 .109 Uiso calc R 1 . . H C32 .4453(3) .0042(3) 1.0755(15) .094(2) Uani d . 1 . . C H32 .4352 -.0336 1.0984 .113 Uiso calc R 1 . . H C33 .4421(4) .0251(3) .8851(14) .097(2) Uani d . 1 . . C H33 .4302 .0014 .7772 .116 Uiso calc R 1 . . H C34 .4565(4) .0818(3) .8475(11) .0880(19) Uani d . 1 . . C H34 .4553 .0958 .7147 .106 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 Br1 .0722(4) .0954(4) .1128(5) .0176(3) .0302(4) .0167(4) O1 .0494(17) .069(2) .075(2) -.0040(15) .0021(18) -.0120(19) O2 .0603(19) .0546(18) .109(3) .0108(15) -.015(2) .007(2) O3 .075(2) .062(2) .116(3) .0093(18) .031(2) .020(2) O4 .0522(17) .0634(18) .063(2) .0027(15) -.0038(17) .0188(18) O5 .074(2) .067(2) .092(3) -.0155(19) -.013(2) .007(2) O6 .0595(19) .078(2) .060(2) .0061(16) .0033(17) .0157(19) O7 .082(2) .0570(19) .114(4) .0130(17) .022(3) .023(2) C1 .055(2) .057(3) .055(3) .001(2) -.001(2) .006(2) C2 .048(2) .046(2) .061(3) .0033(18) -.003(2) .005(2) C3 .064(3) .044(2) .063(3) .003(2) -.005(3) .003(2) C4 .068(3) .049(2) .069(3) .005(2) .014(3) .007(3) C5 .044(2) .067(3) .078(3) -.001(2) -.002(3) .000(3) C6 .063(3) .072(3) .101(5) .006(2) -.017(3) .009(4) C7 .065(3) .047(2) .084(4) -.002(2) -.006(3) .012(3) C8 .073(3) .040(2) .096(4) .005(2) -.010(3) .012(3) C9 .080(4) .053(3) .121(6) .009(3) -.007(4) -.010(4) C10 .113(5) .057(3) .137(7) .015(3) -.012(5) -.022(4) C11 .098(5) .050(3) .175(9) -.006(3) -.033(6) .007(5) C12 .089(4) .058(3) .157(8) -.009(3) .000(5) .013(5) C13 .087(4) .050(3) .112(5) -.014(3) .008(4) .012(4) C14 .054(2) .049(2) .057(3) -.004(2) -.001(2) -.002(2) C15 .063(3) .056(3) .068(3) -.004(2) .009(3) .003(3) C16 .071(3) .049(2) .081(4) -.004(2) .010(3) .006(3) C17 .059(2) .048(2) .068(3) -.003(2) -.003(2) -.002(3) C18 .066(3) .049(3) .082(4) -.001(2) .001(3) .006(3) C19 .064(3) .069(3) .090(4) .013(3) .002(3) .010(3) C20 .066(3) .058(3) .066(3) .003(2) .003(2) -.002(3) C21 .053(2) .061(3) .053(3) .002(2) -.007(2) .001(2) C22 .048(2) .047(2) .055(3) -.0031(18) -.004(2) .000(2) C23 .054(2) .056(2) .050(3) -.003(2) -.011(2) .005(2) C24 .056(3) .062(3) .084(4) .002(2) .005(3) .021(3) C25 .082(4) .087(4) .143(7) -.001(3) .016(5) .061(5) C26 .092(5) .165(7) .052(3) .030(5) -.005(3) .013(4) C27 .099(4) .073(4) .117(6) .019(3) .014(4) .033(4) C28 .095(4) .069(3) .091(4) -.013(3) .024(4) .002(3) C29 .069(3) .062(3) .072(4) -.011(2) .015(3) -.005(3) C30 .090(4) .071(3) .076(4) .001(3) .013(3) -.005(3) C31 .107(5) .071(4) .095(5) -.002(4) .016(5) .010(4) C32 .084(4) .062(3) .135(7) -.012(3) .013(5) .013(5) C33 .100(5) .074(4) .117(6) -.020(3) -.004(4) -.019(4) C34 .109(5) .080(4) .075(4) -.016(4) -.004(4) -.002(3) 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 Br1 C20 . 1.889(5) ? O1 C1 . 1.434(5) ? O1 C5 . 1.447(6) ? O2 C7 . 1.411(6) ? O2 C6 . 1.421(6) ? O3 C28 . 1.373(7) ? O3 C4 . 1.442(6) ? O4 C24 . 1.346(7) ? O4 C23 . 1.396(5) ? O5 C24 . 1.187(7) ? O6 C21 . 1.380(6) ? O6 C26 . 1.444(7) ? O7 C18 . 1.352(6) ? O7 C27 . 1.437(6) ? C1 C14 . 1.516(6) ? C1 C2 . 1.531(7) ? C1 H1 . .9800 ? C2 C3 . 1.521(7) ? C2 C7 . 1.557(6) ? C2 H2 . .9800 ? C3 C4 . 1.519(7) ? C3 H3A . .9700 ? C3 H3B . .9700 ? C4 C5 . 1.501(8) ? C4 H4 . .9800 ? C5 C6 . 1.512(7) ? C5 H5 . .9800 ? C6 H6A . .9700 ? C6 H6B . .9700 ? C7 C8 . 1.489(8) ? C7 H7 . .9800 ? C8 C13 . 1.383(8) ? C8 C9 . 1.388(9) ? C9 C10 . 1.401(9) ? C9 H9 . .9300 ? C10 C11 . 1.381(10) ? C10 H10 . .9300 ? C11 C12 . 1.369(12) ? C11 H11 . .9300 ? C12 C13 . 1.365(10) ? C12 H12 . .9300 ? C13 H13 . .9300 ? C14 C23 . 1.370(6) ? C14 C15 . 1.398(6) ? C15 C16 . 1.362(7) ? C15 H15 . .9300 ? C16 C17 . 1.416(7) ? C16 H16 . .9300 ? C17 C22 . 1.412(7) ? C17 C18 . 1.430(6) ? C18 C19 . 1.355(8) ? C19 C20 . 1.404(7) ? C19 H19 . .9300 ? C20 C21 . 1.361(7) ? C21 C22 . 1.438(7) ? C22 C23 . 1.426(6) ? C24 C25 . 1.508(8) ? C25 H25A . .9600 ? C25 H25B . .9600 ? C25 H25C . .9600 ? C26 H26A . .9600 ? C26 H26B . .9600 ? C26 H26C . .9600 ? C27 H27A . .9600 ? C27 H27B . .9600 ? C27 H27C . .9600 ? C28 C29 . 1.508(7) ? C28 H28A . .9700 ? C28 H28B . .9700 ? C29 C34 . 1.370(8) ? C29 C30 . 1.377(9) ? C30 C31 . 1.383(8) ? C30 H30 . .9300 ? C31 C32 . 1.361(11) ? C31 H31 . .9300 ? C32 C33 . 1.341(11) ? C32 H32 . .9300 ? C33 C34 . 1.393(9) ? C33 H33 . .9300 ? C34 H34 . .9300 ? _cod_database_code 2200073