#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007216.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_2007216 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 687 _journal_page_last 693 _publ_section_title ; 3D/2D Hydrogen-Bond Network Preferences for Five New Ryanoid Derivatives ; loop_ _publ_author_name ' Drouin, Marc' ' Dodier, Marco' ' Ruest, Luc' _chemical_name_common '2-deoxyryanodol' _chemical_formula_moiety '2C20 H32 O7, 2.5H2 O' _chemical_formula_sum 'C40 H69 O16.5 ' _chemical_formula_weight 813.98 _chemical_melting_point 'decompose at 243\%C' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2 21 21' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,-y,-z -x,1/2-y,1/2+z _cell_length_a 9.0121(10) _cell_length_b 18.080(4) _cell_length_c 25.476(3) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 4150.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _exptl_crystal_density_diffrn 1.302 _diffrn_ambient_temperature 293 _refine_ls_R_factor_obs .0553 _refine_ls_wR_factor_obs .1509 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 C1 .5402(4) .7830(2) .15696(12) .0350(7) Uani d . 1 . C C2 .4760(5) .8196(2) .10681(15) .0504(9) Uani d . 1 . C H2 .4198 .8620 .1203 .060 Uiso calc . 1 . H C3 .3540(4) .7656(3) .08746(14) .0521(9) Uani d . 1 . C H3 .2597 .7926 .0864 .063 Uiso calc . 1 . H C4 .3406(4) .7041(2) .12881(13) .0399(8) Uani d . 1 . C C5 .4405(4) .6344(2) .1204(2) .0474(9) Uani d . 1 . C C6 .4419(4) .6020(2) .1766(2) .0418(8) Uani d . 1 . C C7 .5421(5) .5372(2) .1913(2) .0593(12) Uani d . 1 . C H7A .5102 .4930 .1729 .071 Uiso calc . 1 . H H7B .6435 .5479 .1811 .071 Uiso calc . 1 . H C8 .5341(5) .5245(2) .2500(2) .0695(15) Uani d . 1 . C H8A .6055 .4866 .2593 .083 Uiso calc . 1 . H H8B .4362 .5056 .2585 .083 Uiso calc . 1 . H C9 .5639(4) .5936(2) .2846(2) .0538(10) Uani d . 1 . C H9 .6676 .6083 .2794 .065 Uiso calc . 1 . H C10 .4651(4) .6579(2) .26644(14) .0377(7) Uani d . 1 . C H10 .3621 .6418 .2710 .045 Uiso calc . 1 . H C11 .4877(3) .6704(2) .20875(13) .0320(7) Uani d . 1 . C C12 .4105(3) .7363(2) .17968(12) .0307(6) Uani d . 1 . C C13 .5727(6) .8529(3) .0643(2) .0712(14) Uani d . 1 . C H13 .6159 .8119 .0444 .085 Uiso calc . 1 . H C14 .5989(4) .6625(2) .10793(15) .0462(9) Uani d . 1 . C H14A .6668 .6209 .1069 .055 Uiso calc . 1 . H H14B .5994 .6858 .0736 .055 Uiso calc . 1 . H C15 .6511(4) .7179(2) .14913(12) .0366(7) Uani d . 1 . C O16 .6449(2) .68216(12) .19951(8) .0331(5) Uani d . 1 . O C17 .5973(4) .8385(2) .19671(14) .0416(8) Uani d . 1 . C H17A .6354 .8128 .2268 .062 Uiso calc . 1 . H H17B .5176 .8704 .2074 .062 Uiso calc . 1 . H H17C .6749 .8675 .1812 .062 Uiso calc . 1 . H C18 .7005(7) .9007(3) .0840(2) .083(2) Uani d . 1 . C H18A .7605 .8726 .1079 .124 Uiso calc . 1 . H H18B .6615 .9433 .1018 .124 Uiso calc . 1 . H H18C .7599 .9164 .0548 .124 Uiso calc . 1 . H C19 .4785(9) .8977(4) .0267(3) .116(3) Uani d . 1 . C H19A .5406 .9184 -.0001 .175 Uiso calc . 1 . H H19B .4300 .9368 .0456 .175 Uiso calc . 1 . H H19C .4053 .8662 .0109 .175 Uiso calc . 1 . H C20 .3859(5) .5798(3) .0788(2) .074(2) Uani d . 1 . C H20A .3876 .6031 .0450 .111 Uiso calc . 1 . H H20B .2864 .5647 .0869 .111 Uiso calc . 1 . H H20C .4496 .5372 .0784 .111 Uiso calc . 1 . H C21 .5417(6) .5778(3) .3433(2) .089(2) Uani d . 1 . C H21A .6044 .5375 .3537 .133 Uiso calc . 1 . H H21B .4399 .5650 .3496 .133 Uiso calc . 1 . H H21C .5669 .6211 .3632 .133 Uiso calc . 1 . H O23 .3819(4) .7365(3) .03628(11) .0902(13) Uani d . 1 . O H23 .3036(14) .734(4) .0200(11) .135 Uiso calc R 1 . H O24 .2920(3) .58261(13) .19239(12) .0498(7) Uani d . 1 . O H24 .268(2) .5434(14) .1786(16) .075 Uiso calc R 1 . H O25 .1871(3) .6870(2) .13372(11) .0492(6) Uani d . 1 . O H25 .1768(5) .6520(17) .1539(15) .074 Uiso calc R 1 . H O26 .4828(2) .72385(14) .29667(9) .0399(5) Uani d . 1 . O H26 .5712(4) .7339(13) .2991(15) .060 Uiso calc R 1 . H O27 .3049(2) .77567(13) .20929(9) .0363(5) Uani d . 1 . O H27 .331(2) .777(2) .2401(3) .055 Uiso calc R 1 . H O28 .7974(2) .7360(2) .13821(9) .0439(6) Uani d . 1 . O H28 .8359(15) .754(2) .1644(6) .066 Uiso calc R 1 . H C1' 1.0294(3) .7264(2) .35305(12) .0336(7) Uani d . 1 . C C2' .9581(4) .6888(2) .40225(15) .0476(9) Uani d . 1 . C H2' .8996 .6485 .3870 .057 Uiso calc . 1 . H C3' .8390(4) .7435(2) .42115(13) .0442(8) Uani d . 1 . C H3' .7440 .7176 .4175 .053 Uiso calc . 1 . H C4' .8336(3) .8082(2) .38182(12) .0342(7) Uani d . 1 . C C5' .9389(4) .8751(2) .39356(13) .0370(7) Uani d . 1 . C C6' .9458(3) .9110(2) .33772(13) .0339(7) Uani d . 1 . C C7' 1.0513(4) .9744(2) .3259(2) .0458(9) Uani d . 1 . C H7'1 1.1514 .9611 .3362 .055 Uiso calc . 1 . H H7'2 1.0221 1.0180 .3456 .055 Uiso calc . 1 . H C8' 1.0465(4) .9910(2) .2669(2) .0507(9) Uani d . 1 . C H8'1 1.1205 1.0283 .2591 .061 Uiso calc . 1 . H H8'2 .9501 1.0116 .2584 .061 Uiso calc . 1 . H C9' 1.0744(4) .9231(2) .23135(15) .0439(8) Uani d . 1 . C H9' 1.1769 .9067 .2367 .053 Uiso calc . 1 . H C10' .9702(3) .8593(2) .24675(12) .0331(7) Uani d . 1 . C H10' .8684 .8770 .2419 .040 Uiso calc . 1 . H C11' .9891(3) .8426(2) .30433(12) .0304(6) Uani d . 1 . C C12' .9046(3) .7768(2) .33069(12) .0300(6) Uani d . 1 . C C13' 1.0476(6) .6505(3) .4441(2) .0694(14) Uani d . 1 . C H13' 1.0944 .6889 .4656 .083 Uiso calc . 1 . H C14' 1.0941(4) .8435(2) .40547(13) .0394(8) Uani d . 1 . C H14C 1.1650 .8838 .4075 .047 Uiso calc . 1 . H H14D 1.0924 .8189 .4393 .047 Uiso calc . 1 . H C15' 1.1444(4) .7887(2) .36353(12) .0346(7) Uani d . 1 . C O16' 1.1443(2) .82696(12) .31408(8) .0312(5) Uani d . 1 . O C17' 1.0839(4) .6716(2) .31236(14) .0425(8) Uani d . 1 . C H17D 1.0100 .6341 .3070 .064 Uiso calc . 1 . H H17E 1.1742 .6491 .3244 .064 Uiso calc . 1 . H H17F 1.1021 .6969 .2799 .064 Uiso calc . 1 . H C18' 1.1699(7) .6002(3) .4239(2) .086(2) Uani d . 1 . C H18D 1.2210 .5782 .4531 .128 Uiso calc . 1 . H H18E 1.2387 .6286 .4034 .128 Uiso calc . 1 . H H18F 1.1274 .5620 .4025 .128 Uiso calc . 1 . H C19' .9462(8) .6062(4) .4797(3) .104(2) Uani d . 1 . C H19D 1.0042 .5820 .5062 .156 Uiso calc . 1 . H H19E .8945 .5697 .4593 .156 Uiso calc . 1 . H H19F .8758 .6387 .4960 .156 Uiso calc . 1 . H C20' .8870(5) .9284(2) .4363(2) .0528(10) Uani d . 1 . C H20D .7902 .9469 .4276 .079 Uiso calc . 1 . H H20E .9554 .9689 .4389 .079 Uiso calc . 1 . H H20F .8827 .9029 .4693 .079 Uiso calc . 1 . H C21' 1.0554(6) .9436(3) .1735(2) .0696(13) Uani d . 1 . C H21D 1.1214 .9835 .1649 .104 Uiso calc . 1 . H H21E .9548 .9587 .1673 .104 Uiso calc . 1 . H H21F 1.0782 .9015 .1520 .104 Uiso calc . 1 . H O23' .8456(4) .7677(2) .47407(10) .0694(9) Uani d . 1 . O H23' .930(2) .783(3) .4806(8) .104 Uiso calc R 1 . H O24' .8007(3) .93668(14) .32238(10) .0427(6) Uani d . 1 . O H24' .7372(3) .9097(15) .3353(15) .064 Uiso calc R 1 . H O25' .6842(3) .8300(2) .37331(10) .0442(6) Uani d . 1 . O H25' .6432(15) .837(3) .40166(11) .066 Uiso calc R 1 . H O26' .9870(2) .79442(14) .21479(9) .0389(5) Uani d . 1 . O H26' 1.0755(3) .7857(14) .2106(15) .058 Uiso calc R 1 . H O27' .7977(2) .74077(13) .29976(9) .0359(5) Uani d . 1 . O H27' .8299(18) .735(2) .2699(5) .054 Uiso calc R 1 . H O28' 1.2883(2) .7662(2) .37496(9) .0432(6) Uani d . 1 . O H28' 1.3324(17) .757(3) .34758(13) .065 Uiso calc R 1 . H O40 .4784(4) .8287(3) .45089(14) .0949(14) Uani d . 1 . O O41 .9747(5) .6843(3) .0530(2) .118(2) Uani d . 1 . O O43 .7238(16) .5000 .0000 .174(10) Uani d SP .50 . O H40A .4488 .8062 .4804 .044 Uiso d . 1 . H H40B .3875 .8126 .4302 .044 Uiso d . 1 . H H41A .9966 .7365 .0616 .162 Uiso d . 1 . H H41B .9696 .6498 .0755 .141 Uiso d . 1 . H H43 .7825 .4826 -.0309 .264 Uiso d . 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 C1 .029(2) .038(2) .038(2) -.0059(13) -.0045(13) -.0002(13) C2 .046(2) .058(2) .047(2) -.013(2) -.010(2) .013(2) C3 .040(2) .077(3) .040(2) -.014(2) -.009(2) .005(2) C4 .023(2) .054(2) .042(2) -.0117(15) -.0021(13) -.003(2) C5 .029(2) .054(2) .060(2) -.013(2) .011(2) -.023(2) C6 .0217(15) .034(2) .070(2) -.0041(13) .007(2) -.010(2) C7 .036(2) .031(2) .111(4) .001(2) .010(2) -.006(2) C8 .032(2) .041(2) .136(5) .005(2) .008(3) .023(2) C9 .028(2) .053(2) .081(3) .006(2) .006(2) .025(2) C10 .0227(15) .040(2) .050(2) .0025(13) .0050(13) .0109(14) C11 .0151(13) .0310(14) .050(2) -.0016(11) .0041(12) -.0008(13) C12 .0209(14) .0356(15) .0358(14) .0007(12) .0005(11) -.0009(13) C13 .066(3) .088(3) .059(3) -.019(3) -.004(2) .025(3) C14 .029(2) .061(2) .049(2) -.012(2) .0106(14) -.021(2) C15 .0230(15) .049(2) .038(2) -.0076(14) .0034(13) -.0077(14) O16 .0171(10) .0383(11) .0438(11) -.0001(9) .0050(9) -.0036(9) C17 .036(2) .040(2) .049(2) -.0087(15) -.0058(15) -.0025(15) C18 .090(4) .082(3) .076(3) -.040(3) .003(3) .019(3) C19 .107(5) .149(6) .093(4) -.027(5) -.018(4) .070(4) C20 .047(3) .085(3) .090(3) -.026(2) .007(2) -.048(3) C21 .067(3) .099(4) .101(4) .014(3) .004(3) .063(3) O23 .087(3) .145(4) .0387(14) -.041(3) -.004(2) -.008(2) O24 .0261(12) .0369(12) .086(2) -.0099(10) .0084(13) -.0036(13) O25 .0219(12) .065(2) .061(2) -.0096(11) -.0029(11) .0002(13) O26 .0226(10) .0551(14) .0422(12) .0046(10) .0017(9) .0030(11) O27 .0251(11) .0437(12) .0402(11) .0084(10) -.0010(9) -.0032(10) O28 .0215(11) .066(2) .0441(12) -.0133(11) .0064(9) -.0109(12) C1' .0264(15) .038(2) .0365(15) .0055(13) .0032(12) .0041(13) C2' .043(2) .050(2) .050(2) .011(2) .010(2) .015(2) C3' .035(2) .057(2) .040(2) .007(2) .0085(14) .012(2) C4' .0206(15) .044(2) .038(2) .0066(13) .0029(12) .0036(14) C5' .027(2) .042(2) .041(2) .0070(14) -.0016(13) -.0037(14) C6' .0210(14) .0347(15) .046(2) .0021(13) -.0017(13) -.0009(13) C7' .035(2) .035(2) .068(2) -.0036(15) -.003(2) -.004(2) C8' .036(2) .038(2) .078(3) -.005(2) .004(2) .011(2) C9' .029(2) .048(2) .055(2) -.004(2) .003(2) .013(2) C10' .0192(15) .042(2) .038(2) -.0026(13) -.0003(12) .0075(13) C11' .0151(13) .0345(14) .042(2) .0008(11) -.0015(12) .0047(13) C12' .0219(14) .0339(14) .0343(14) .0002(12) .0017(11) .0041(12) C13' .071(3) .076(3) .061(3) .024(3) .010(2) .027(2) C14' .028(2) .053(2) .038(2) .0091(15) -.0048(13) -.0067(15) C15' .0224(15) .046(2) .0354(15) .0078(14) -.0031(12) -.0017(13) O16' .0152(9) .0409(11) .0375(10) .0006(9) -.0011(8) .0007(9) C17' .037(2) .042(2) .049(2) .0095(15) .005(2) -.002(2) C18' .103(4) .079(3) .074(3) .049(3) .000(3) .015(3) C19' .108(5) .103(4) .101(4) .019(4) .026(4) .061(4) C20' .047(2) .060(2) .052(2) .014(2) -.001(2) -.012(2) C21' .068(3) .079(3) .062(3) -.011(3) .012(2) .030(2) O23' .078(2) .091(2) .0392(13) .026(2) .0092(15) .0069(15) O24' .0250(11) .0433(12) .0599(15) .0086(10) .0003(11) .0078(11) O25' .0204(11) .0579(15) .0544(14) .0082(11) .0051(10) .0065(12) O26' .0240(11) .0548(14) .0378(11) -.0035(10) -.0006(9) -.0010(10) O27' .0243(10) .0436(12) .0398(11) -.0072(10) .0009(9) -.0008(10) O28' .0232(11) .067(2) .0398(11) .0135(12) -.0026(9) -.0028(12) O40 .044(2) .173(4) .068(2) -.007(2) -.002(2) -.024(3) O41 .077(3) .192(5) .085(3) .002(3) .020(2) -.030(3) O43 .078(10) .31(3) .135(14) .000 .000 .026(14) 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 C1 C17 . 1.516(4) no C1 C2 . 1.551(5) no C1 C12 . 1.554(4) no C1 C15 . 1.557(5) no C2 C13 . 1.514(6) no C2 C3 . 1.550(5) no C2 H2 . .980(4) no C3 O23 . 1.429(5) no C3 C4 . 1.537(5) no C3 H3 . .980(4) no C4 O25 . 1.423(4) no C4 C12 . 1.554(4) no C4 C5 . 1.565(5) no C5 C20 . 1.530(5) no C5 C6 . 1.546(6) no C5 C14 . 1.549(5) no C6 O24 . 1.452(4) no C6 C7 . 1.525(5) no C6 C11 . 1.540(4) no C7 C8 . 1.516(7) no C7 H7A . .970(4) no C7 H7B . .970(4) no C8 C9 . 1.551(7) no C8 H8A . .970(4) no C8 H8B . .970(4) no C9 C21 . 1.536(7) no C9 C10 . 1.535(5) no C9 H9 . .980(4) no C10 O26 . 1.428(4) no C10 C11 . 1.501(5) no C10 H10 . .980(3) no C11 O16 . 1.452(3) no C11 C12 . 1.566(4) no C12 O27 . 1.408(4) no C13 C19 . 1.514(8) no C13 C18 . 1.525(7) no C13 H13 . .980(6) no C14 C15 . 1.526(4) no C14 H14A . .970(4) no C14 H14B . .970(4) no C15 O28 . 1.387(4) no C15 O16 . 1.438(4) no C17 H17A . .960(4) no C17 H17B . .960(4) no C17 H17C . .960(4) no C18 H18A . .960(6) no C18 H18B . .960(6) no C18 H18C . .960(5) no C19 H19A . .960(7) no C19 H19B . .960(9) no C19 H19C . .960(8) no C20 H20A . .960(6) no C20 H20B . .960(4) no C20 H20C . .960(6) no C21 H21A . .960(5) no C21 H21B . .960(6) no C21 H21C . .960(7) no O23 H23 . .82 no O24 H24 . .82 no O25 H25 . .82 no O26 H26 . .82 no O27 H27 . .82 no O28 H28 . .82 no C1' C17' . 1.516(4) no C1' C15' . 1.554(5) no C1' C12' . 1.556(4) no C1' C2' . 1.564(5) no C2' C13' . 1.506(6) no C2' C3' . 1.537(5) no C2' H2' . .980(4) no C3' O23' . 1.419(4) no C3' C4' . 1.541(5) no C3' H3' . .980(4) no C4' O25' . 1.420(4) no C4' C12' . 1.558(4) no C4' C5' . 1.565(5) no C5' C20' . 1.528(5) no C5' C14' . 1.541(4) no C5' C6' . 1.565(5) no C6' O24' . 1.442(4) no C6' C7' . 1.520(5) no C6' C11' . 1.551(4) no C7' C8' . 1.532(6) no C7' H7'1 . .970(4) no C7' H7'2 . .970(4) no C8' C9' . 1.546(6) no C8' H8'1 . .970(4) no C8' H8'2 . .970(4) no C9' C21' . 1.529(6) no C9' C10' . 1.539(4) no C9' H9' . .980(4) no C10' O26' . 1.435(4) no C10' C11' . 1.507(4) no C10' H10' . .980(3) no C11' O16' . 1.449(3) no C11' C12' . 1.564(4) no C12' O27' . 1.405(4) no C13' C19' . 1.515(8) no C13' C18' . 1.519(7) no C13' H13' . .980(6) no C14' C15' . 1.526(4) no C14' H14C . .970(4) no C14' H14D . .970(4) no C15' O28' . 1.390(4) no C15' O16' . 1.437(4) no C17' H17D . .960(4) no C17' H17E . .960(4) no C17' H17F . .960(4) no C18' H18D . .960(5) no C18' H18E . .960(6) no C18' H18F . .960(6) no C19' H19D . .960(6) no C19' H19E . .960(8) no C19' H19F . .960(7) no C20' H20D . .960(4) no C20' H20E . .960(5) no C20' H20F . .960(4) no C21' H21D . .960(5) no C21' H21E . .960(6) no C21' H21F . .960(6) no O23' H23' . .82 no O24' H24' . .82 no O25' H25' . .82 no O26' H26' . .82 no O27' H27' . .82 no O28' H28' . .82 no O40 H40A . .896(4) no O40 H40B . 1.017(3) no O41 H41A . .989(6) no O41 H41B . .848(6) no O43 H43 . 1.000(8) no