Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_prabcd _audit_creation_method SHELXL-97 _chemical_name_systematic ; 6-deoxy-6-(1-propylamino)cyclomaltoheptaose ; _chemical_name_common ; 6-deoxy-6-(1-propylamino)-beta-cyclodextrin ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H97 N O44' _chemical_formula_weight 1356.2 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 14.414(1) _cell_length_b 19.377(2) _cell_length_c 26.997(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7540 _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2788 _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6695 _exptl_absorpt_correction_T_max 0.7798 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5611 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 74.20 _reflns_number_total 5611 _reflns_number_gt 3878 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.6(5) _refine_ls_number_reflns 5611 _refine_ls_number_parameters 894 _refine_ls_number_restraints 119 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.2593 _refine_ls_wR_factor_gt 0.2387 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.054 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.1487(7) 0.2202(4) 0.2408(3) 0.093(2) Uani 1 1 d . . . H11 H 0.1712 0.1813 0.2606 0.112 Uiso 1 1 calc R . . C21 C 0.0412(7) 0.2370(4) 0.2566(3) 0.090(2) Uani 1 1 d . . . H21 H 0.0404 0.2459 0.2923 0.108 Uiso 1 1 calc R . . C31 C 0.0024(7) 0.2989(4) 0.2314(3) 0.090(2) Uani 1 1 d . . . H31 H -0.0041 0.2875 0.1962 0.108 Uiso 1 1 calc R . . C41 C 0.0758(6) 0.3590(4) 0.2355(3) 0.086(2) Uani 1 1 d . . . H41 H 0.0758 0.3758 0.2697 0.103 Uiso 1 1 calc R . . C51 C 0.1789(6) 0.3385(4) 0.2213(3) 0.093(2) Uani 1 1 d D . . H51 H 0.1810 0.3284 0.1858 0.112 Uiso 1 1 calc R . . C61 C 0.2565(9) 0.3940(5) 0.2334(5) 0.135(4) Uani 1 1 d D . . H61A H 0.2378 0.4376 0.2189 0.162 Uiso 1 1 calc R . . H61B H 0.2585 0.4003 0.2690 0.162 Uiso 1 1 calc R . . O21 O -0.0142(5) 0.1758(3) 0.2476(2) 0.1080(19) Uani 1 1 d . . . O31 O -0.0919(5) 0.3160(3) 0.2505(2) 0.1088(18) Uani 1 1 d . . . O41 O 0.0401(4) 0.4129(2) 0.20427(18) 0.0882(15) Uani 1 1 d . . . O51 O 0.2106(5) 0.2786(3) 0.2479(2) 0.0980(16) Uani 1 1 d . . . O61 O 0.3537(5) 0.3779(4) 0.2159(5) 0.163(4) Uani 1 1 d . . . C12 C 0.2652(6) 0.0533(4) 0.0976(3) 0.094(2) Uani 1 1 d . . . H12 H 0.2954 0.0117 0.0847 0.113 Uiso 1 1 calc R . . C22 C 0.1737(7) 0.0310(4) 0.1298(3) 0.093(2) Uani 1 1 d . . . H22 H 0.1930 0.0022 0.1578 0.111 Uiso 1 1 calc R . . C32 C 0.1232(6) 0.0932(3) 0.1488(3) 0.082(2) Uani 1 1 d . . . H32 H 0.0986 0.1194 0.1206 0.098 Uiso 1 1 calc R . . C42 C 0.1992(6) 0.1387(3) 0.1768(3) 0.082(2) Uani 1 1 d . . . H42 H 0.2187 0.1145 0.2069 0.098 Uiso 1 1 calc R . . C52 C 0.2863(6) 0.1562(4) 0.1452(3) 0.093(2) Uani 1 1 d D . . H52 H 0.2657 0.1825 0.1162 0.112 Uiso 1 1 calc R . . C62 C 0.3681(9) 0.1965(7) 0.1697(6) 0.141(4) Uani 1 1 d D . . H62A H 0.4156 0.2043 0.1449 0.169 Uiso 1 1 calc R . . H62B H 0.3455 0.2413 0.1803 0.169 Uiso 1 1 calc R . . O22 O 0.1087(5) -0.0084(3) 0.0981(2) 0.1076(19) Uani 1 1 d . . . O32 O 0.0459(5) 0.0717(3) 0.1808(2) 0.1018(17) Uani 1 1 d . . . O42 O 0.1464(4) 0.2004(2) 0.19078(18) 0.0844(14) Uani 1 1 d . . . O52 O 0.3323(4) 0.0928(3) 0.1273(2) 0.1044(17) Uani 1 1 d . . . O62 O 0.4066(9) 0.1647(7) 0.2087(6) 0.206(5) Uani 1 1 d . . . C13 C 0.2689(8) 0.1185(4) -0.0928(3) 0.102(3) Uani 1 1 d . . . H13 H 0.2821 0.1065 -0.1273 0.123 Uiso 1 1 calc R . . C23 C 0.1816(8) 0.0763(5) -0.0751(4) 0.116(3) Uani 1 1 d . . . H23 H 0.1943 0.0276 -0.0822 0.139 Uiso 1 1 calc R . . C33 C 0.1645(8) 0.0815(5) -0.0216(3) 0.105(3) Uani 1 1 d . . . H33 H 0.1424 0.1286 -0.0156 0.126 Uiso 1 1 calc R . . C43 C 0.2556(7) 0.0740(4) 0.0078(3) 0.094(2) Uani 1 1 d . . . H43 H 0.2745 0.0254 0.0071 0.113 Uiso 1 1 calc R . . C53 C 0.3380(6) 0.1190(4) -0.0115(3) 0.092(2) Uani 1 1 d D . . H53 H 0.3211 0.1677 -0.0077 0.111 Uiso 1 1 calc R . . C63 C 0.4386(7) 0.1075(5) 0.0131(4) 0.112(3) Uani 1 1 d D . . H63A H 0.4336 0.1137 0.0486 0.134 Uiso 1 1 calc R . . H63B H 0.4582 0.0604 0.0070 0.134 Uiso 1 1 calc R . . O23 O 0.0966(8) 0.0957(6) -0.1044(3) 0.179(4) Uani 1 1 d . . . O33 O 0.0879(6) 0.0342(4) -0.0049(3) 0.137(3) Uani 1 1 d . . . O43 O 0.2314(4) 0.0922(3) 0.05822(19) 0.0927(15) Uani 1 1 d . . . O53 O 0.3520(5) 0.1054(3) -0.0631(2) 0.1028(17) Uani 1 1 d . . . N63 N 0.5116(5) 0.1561(5) -0.0067(3) 0.114(2) Uani 1 1 d D . . C73 C 0.6113(9) 0.1373(9) 0.0080(5) 0.163(6) Uani 1 1 d D . . H73A H 0.6182 0.1423 0.0435 0.196 Uiso 1 1 calc R . . H73B H 0.6229 0.0895 -0.0004 0.196 Uiso 1 1 calc R . . C83 C 0.6825(9) 0.1828(11) -0.0180(6) 0.194(7) Uani 1 1 d D . . H83A H 0.6604 0.2301 -0.0174 0.233 Uiso 1 1 calc R . . H83B H 0.7399 0.1812 0.0007 0.233 Uiso 1 1 calc R . . C93 C 0.7029(15) 0.1637(14) -0.0702(6) 0.250(12) Uani 1 1 d D . . H93A H 0.6461 0.1527 -0.0869 0.375 Uiso 1 1 calc R . . H93B H 0.7433 0.1243 -0.0707 0.375 Uiso 1 1 calc R . . H93C H 0.7326 0.2017 -0.0865 0.375 Uiso 1 1 calc R . . C14 C 0.2610(10) 0.3590(6) -0.1808(4) 0.135(5) Uani 1 1 d . A . H14 H 0.2803 0.3892 -0.2080 0.162 Uiso 1 1 calc R . . C24 C 0.2137(9) 0.2980(5) -0.2026(4) 0.113(3) Uani 1 1 d . . . H24 H 0.2565 0.2746 -0.2253 0.135 Uiso 1 1 calc R . . C34 C 0.1833(8) 0.2476(4) -0.1630(3) 0.100(3) Uani 1 1 d . . . H34 H 0.1377 0.2699 -0.1413 0.119 Uiso 1 1 calc R . . C44 C 0.2737(7) 0.2302(4) -0.1322(3) 0.100(3) Uani 1 1 d . . . H44 H 0.3172 0.2036 -0.1526 0.120 Uiso 1 1 calc R . . C54 C 0.3221(8) 0.2968(4) -0.1121(3) 0.103(3) Uani 1 1 d D A . H54 H 0.2795 0.3210 -0.0897 0.124 Uiso 1 1 calc R . . C64 C 0.4154(10) 0.2850(6) -0.0853(5) 0.139(4) Uani 1 1 d D . . O24 O 0.1257(7) 0.3188(4) -0.2312(3) 0.140(3) Uani 1 1 d . . . O34 O 0.1431(6) 0.1863(4) -0.1844(3) 0.124(2) Uani 1 1 d . . . O44 O 0.2417(5) 0.1885(3) -0.0906(2) 0.1013(17) Uani 1 1 d . . . O54 O 0.3438(6) 0.3403(3) -0.1526(3) 0.116(2) Uani 1 1 d . . . O6A4 O 0.4883(18) 0.2511(9) -0.1072(7) 0.164(7) Uani 0.48 1 d P A 1 O6B4 O 0.4438(18) 0.3452(8) -0.0602(8) 0.189(8) Uani 0.52 1 d P A 2 C15 C 0.1100(7) 0.5948(4) -0.1121(3) 0.094(2) Uani 1 1 d . . . H15 H 0.1022 0.6449 -0.1142 0.113 Uiso 1 1 calc R . . C25 C 0.0484(7) 0.5614(5) -0.1504(4) 0.104(3) Uani 1 1 d . . . H25 H 0.0649 0.5808 -0.1828 0.125 Uiso 1 1 calc R . . C35 C 0.0654(8) 0.4828(5) -0.1526(3) 0.106(3) Uani 1 1 d . . . H35 H 0.0413 0.4622 -0.1221 0.127 Uiso 1 1 calc R . . C45 C 0.1791(7) 0.4689(5) -0.1549(4) 0.106(3) Uani 1 1 d . A . H45 H 0.2024 0.4833 -0.1874 0.127 Uiso 1 1 calc R . . C55 C 0.2351(8) 0.5064(5) -0.1139(4) 0.111(3) Uani 1 1 d D . . H55 H 0.2097 0.4907 -0.0822 0.134 Uiso 1 1 calc R . . C65 C 0.3471(9) 0.4997(6) -0.1097(5) 0.133(4) Uani 1 1 d D . . H65A H 0.3691 0.5289 -0.0830 0.160 Uiso 1 1 calc R . . H65B H 0.3633 0.4524 -0.1017 0.160 Uiso 1 1 calc R . . O25 O -0.0558(5) 0.5742(4) -0.1421(3) 0.126(2) Uani 1 1 d . . . O35 O 0.0186(7) 0.4525(4) -0.1933(3) 0.141(3) Uani 1 1 d . . . O45 O 0.1869(6) 0.3969(3) -0.1509(3) 0.119(2) Uani 1 1 d . . . O55 O 0.2115(5) 0.5781(3) -0.1182(2) 0.1102(19) Uani 1 1 d . . . O65 O 0.3893(7) 0.5181(4) -0.1525(3) 0.140(3) Uani 1 1 d . . . C16 C 0.0114(12) 0.6481(5) 0.0733(4) 0.140(5) Uani 1 1 d . . . H16 H -0.0017 0.6799 0.1007 0.168 Uiso 1 1 calc R . . C26 C -0.0710(10) 0.6541(6) 0.0343(4) 0.130(4) Uani 1 1 d . . . H26 H -0.0733 0.7019 0.0226 0.156 Uiso 1 1 calc R . . C36 C -0.0448(9) 0.6086(6) -0.0090(4) 0.119(3) Uani 1 1 d . . . H36 H -0.0467 0.5608 0.0027 0.143 Uiso 1 1 calc R . . C46 C 0.0560(8) 0.6227(5) -0.0275(3) 0.109(3) Uani 1 1 d D . . H46 H 0.0577 0.6687 -0.0425 0.131 Uiso 1 1 calc R . . C56 C 0.1323(9) 0.6193(6) 0.0137(4) 0.127(4) Uani 1 1 d D . . H56 H 0.1379 0.5718 0.0258 0.152 Uiso 1 1 calc R . . C66 C 0.2271(9) 0.6445(13) -0.0047(5) 0.227(12) Uani 1 1 d D . . O26 O -0.1671(7) 0.6355(5) 0.0554(3) 0.158(3) Uani 1 1 d . . . O36 O -0.1193(7) 0.6162(5) -0.0471(3) 0.152(3) Uani 1 1 d . . . O46 O 0.0775(5) 0.5724(3) -0.0653(2) 0.1035(18) Uani 1 1 d . . . O56 O 0.1033(7) 0.6640(4) 0.0541(3) 0.145(3) Uani 1 1 d D . . O66A O 0.228(2) 0.7107(13) -0.0208(10) 0.28(2) Uani 0.48 1 d PD . . O66B O 0.2985(13) 0.6369(16) 0.0299(10) 0.260(15) Uani 0.52 1 d PD . . C17 C 0.0131(7) 0.4765(4) 0.2265(3) 0.092(2) Uani 1 1 d . . . H17 H 0.0086 0.4693 0.2624 0.110 Uiso 1 1 calc R . . C27 C -0.0851(7) 0.4989(4) 0.2069(3) 0.096(2) Uani 1 1 d . . . H27 H -0.1041 0.5402 0.2252 0.115 Uiso 1 1 calc R . . C37 C -0.0834(7) 0.5172(4) 0.1518(3) 0.097(2) Uani 1 1 d . . . H37 H -0.0710 0.4752 0.1327 0.117 Uiso 1 1 calc R . . C47 C -0.0010(8) 0.5691(4) 0.1438(3) 0.101(3) Uani 1 1 d . . . H47 H -0.0167 0.6132 0.1595 0.121 Uiso 1 1 calc R . . C57 C 0.1003(7) 0.5429(4) 0.1648(3) 0.095(2) Uani 1 1 d D . . H57 H 0.1181 0.5005 0.1475 0.114 Uiso 1 1 calc R . . C67 C 0.1816(8) 0.5955(5) 0.1618(4) 0.118(3) Uani 1 1 d D . . H67A H 0.2354 0.5771 0.1788 0.142 Uiso 1 1 calc R . . H67B H 0.1982 0.6030 0.1274 0.142 Uiso 1 1 calc R . . O27 O -0.1570(5) 0.4445(3) 0.2153(2) 0.1101(18) Uani 1 1 d . . . O37 O -0.1737(5) 0.5445(3) 0.1371(3) 0.1129(19) Uani 1 1 d . . . O47 O 0.0085(6) 0.5795(3) 0.0924(2) 0.1083(19) Uani 1 1 d . . . O57 O 0.0863(5) 0.5275(3) 0.2173(2) 0.0973(16) Uani 1 1 d . . . O67 O 0.1554(6) 0.6580(3) 0.1834(3) 0.129(2) Uani 1 1 d . . . O1W O 0.4204(17) 0.6659(8) -0.1241(6) 0.296(11) Uani 1 1 d U . . O2W O 0.4612(15) 0.2776(8) 0.0472(7) 0.242(7) Uani 0.88 1 d PU . . O3AW O -0.232(3) 0.7462(9) 0.1206(10) 0.296(15) Uani 0.68 1 d PU . . O3BW O -0.384(4) 0.721(3) 0.162(2) 0.25(2) Uani 0.32 1 d PU . . O4W O -0.3254(16) 0.6096(19) 0.1871(9) 0.320(14) Uani 0.81 1 d PU . . O5W O -0.142(2) 0.6522(15) -0.2107(7) 0.388(17) Uani 1 1 d U . . O6W O 0.4075(14) 0.4033(16) 0.0183(13) 0.372(15) Uani 1 1 d U . . O7AW O 0.197(3) 0.7907(14) 0.1710(17) 0.28(2) Uani 0.45 1 d PU . . O7BW O 0.317(5) 0.738(4) 0.1689(13) 0.37(4) Uani 0.37 1 d PU . . O8AW O -0.161(6) 0.747(2) -0.0771(13) 0.34(4) Uani 0.25 1 d PU . . O8BW O -0.342(3) 0.630(3) 0.0064(17) 0.35(3) Uani 0.51 1 d PU . . O9AW O 0.605(3) 0.6505(15) -0.093(2) 0.225(16) Uani 0.36 1 d PU . . O9BW O 0.593(4) 0.6441(13) -0.1448(10) 0.154(16) Uani 0.23 1 d PU . . O10W O -0.3384(14) 0.4907(12) 0.2470(12) 0.294(12) Uani 0.79 1 d PU . . O11W O 0.4554(15) 0.2885(10) 0.2693(8) 0.317(14) Uani 0.94 1 d PU . . O12W O 0.055(4) 0.495(2) -0.2887(12) 0.33(2) Uani 0.63 1 d PU . . O13W O -0.061(3) 0.0262(17) -0.1470(18) 0.27(2) Uani 0.40 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.134(7) 0.076(4) 0.070(4) -0.001(4) -0.027(4) 0.004(5) C21 0.130(7) 0.079(4) 0.060(4) -0.002(3) 0.005(4) 0.007(5) C31 0.125(7) 0.068(4) 0.076(4) -0.008(3) 0.002(5) 0.005(4) C41 0.119(6) 0.065(4) 0.073(4) -0.008(3) -0.012(4) 0.015(4) C51 0.110(6) 0.072(4) 0.097(5) -0.012(4) -0.018(5) -0.005(4) C61 0.159(11) 0.078(5) 0.168(10) -0.013(6) -0.036(9) -0.009(6) O21 0.165(6) 0.067(3) 0.092(3) -0.007(2) 0.013(4) -0.011(4) O31 0.120(5) 0.090(3) 0.116(4) -0.003(3) 0.020(4) 0.007(3) O41 0.125(4) 0.063(2) 0.076(3) -0.007(2) -0.002(3) 0.009(3) O51 0.120(4) 0.073(3) 0.100(3) -0.004(3) -0.028(3) 0.008(3) O61 0.097(5) 0.119(5) 0.274(12) -0.032(7) -0.003(6) -0.008(4) C12 0.109(6) 0.069(4) 0.104(5) -0.005(4) 0.006(5) 0.008(4) C22 0.133(7) 0.064(4) 0.082(5) 0.001(4) 0.005(5) 0.002(4) C32 0.117(6) 0.060(3) 0.068(4) -0.001(3) 0.010(4) 0.003(4) C42 0.101(5) 0.063(4) 0.081(4) 0.001(3) -0.014(4) 0.011(4) C52 0.089(5) 0.090(5) 0.102(5) -0.007(4) 0.005(4) 0.005(4) C62 0.130(9) 0.117(8) 0.175(12) -0.052(9) -0.003(9) -0.011(7) O22 0.137(5) 0.078(3) 0.107(4) -0.018(3) 0.012(4) -0.021(3) O32 0.131(5) 0.083(3) 0.091(3) -0.005(3) 0.020(3) -0.021(3) O42 0.113(4) 0.063(2) 0.077(3) -0.006(2) -0.005(3) 0.013(3) O52 0.106(4) 0.082(3) 0.125(4) -0.012(3) 0.003(4) 0.010(3) O62 0.200(11) 0.185(10) 0.233(13) -0.060(10) -0.076(10) 0.027(9) C13 0.140(8) 0.084(5) 0.083(5) -0.010(4) 0.010(5) -0.016(5) C23 0.139(8) 0.101(6) 0.108(6) -0.001(5) -0.013(6) -0.032(6) C33 0.129(7) 0.095(5) 0.090(5) 0.004(4) 0.006(5) -0.009(5) C43 0.121(7) 0.069(4) 0.092(5) -0.003(4) 0.017(5) 0.003(4) C53 0.125(7) 0.068(4) 0.084(5) -0.009(4) 0.016(5) -0.007(4) C63 0.112(7) 0.087(5) 0.135(7) 0.009(6) 0.009(6) 0.005(5) O23 0.199(9) 0.221(10) 0.116(5) 0.013(6) -0.016(6) -0.097(8) O33 0.152(6) 0.137(5) 0.123(5) 0.015(4) -0.002(5) -0.060(5) O43 0.120(4) 0.072(3) 0.086(3) 0.006(3) 0.018(3) 0.019(3) O53 0.123(5) 0.089(3) 0.096(4) -0.008(3) 0.020(4) -0.007(3) N63 0.092(5) 0.125(6) 0.125(6) 0.014(5) 0.003(4) -0.024(5) C73 0.134(10) 0.222(16) 0.134(9) 0.051(10) -0.012(8) -0.046(11) C83 0.133(10) 0.27(2) 0.184(15) -0.003(15) -0.037(11) -0.028(13) C93 0.201(17) 0.39(4) 0.160(14) 0.07(2) 0.021(14) -0.04(2) C14 0.194(12) 0.105(7) 0.105(7) 0.004(6) 0.081(8) 0.012(8) C24 0.143(8) 0.108(7) 0.086(5) -0.004(5) 0.001(6) 0.020(6) C34 0.126(7) 0.090(5) 0.083(5) -0.012(4) 0.023(5) -0.009(5) C44 0.127(7) 0.085(5) 0.087(5) 0.003(4) 0.015(5) 0.007(5) C54 0.138(8) 0.085(5) 0.086(5) 0.003(4) 0.018(5) -0.014(5) C64 0.177(12) 0.092(6) 0.147(9) -0.006(6) -0.008(10) -0.006(8) O24 0.175(7) 0.137(6) 0.108(5) 0.006(4) 0.016(5) 0.018(6) O34 0.154(6) 0.112(4) 0.106(4) -0.007(4) -0.006(4) 0.002(4) O44 0.134(5) 0.085(3) 0.086(3) 0.002(3) 0.020(3) -0.007(3) O54 0.134(5) 0.103(4) 0.110(4) 0.012(4) 0.025(4) -0.001(4) O6A4 0.21(2) 0.129(12) 0.149(14) -0.016(11) 0.037(14) 0.008(14) O6B4 0.25(2) 0.106(10) 0.211(17) -0.015(11) -0.030(18) -0.061(13) C15 0.126(7) 0.071(4) 0.085(5) 0.015(4) 0.015(5) 0.007(4) C25 0.112(7) 0.106(6) 0.095(5) 0.010(5) 0.007(5) 0.009(5) C35 0.139(8) 0.098(6) 0.082(5) 0.008(5) 0.019(5) -0.013(6) C45 0.131(8) 0.091(5) 0.095(5) 0.010(5) 0.042(6) 0.005(5) C55 0.140(9) 0.077(5) 0.117(7) 0.001(5) 0.020(6) -0.002(5) C65 0.172(12) 0.113(7) 0.115(8) 0.009(6) 0.010(8) 0.029(7) O25 0.132(5) 0.121(5) 0.125(5) 0.010(4) 0.011(4) 0.014(4) O35 0.167(7) 0.129(5) 0.129(5) -0.024(4) 0.006(5) -0.031(5) O45 0.160(6) 0.078(3) 0.119(4) 0.012(3) 0.052(4) 0.013(4) O55 0.119(5) 0.083(3) 0.129(5) 0.011(3) 0.011(4) -0.006(3) O65 0.179(7) 0.132(5) 0.110(5) 0.008(4) 0.016(5) 0.019(6) C16 0.238(15) 0.071(5) 0.110(7) -0.003(5) 0.038(9) 0.006(8) C26 0.205(12) 0.102(6) 0.084(5) 0.014(5) -0.006(7) 0.032(8) C36 0.158(9) 0.099(6) 0.102(6) 0.009(5) 0.025(7) 0.032(6) C46 0.157(9) 0.075(4) 0.096(6) 0.000(4) 0.017(6) -0.015(5) C56 0.168(10) 0.118(7) 0.096(6) -0.009(6) 0.009(7) -0.032(8) C66 0.169(15) 0.39(4) 0.123(11) -0.025(17) -0.021(11) -0.08(2) O26 0.181(8) 0.185(8) 0.109(5) 0.029(5) 0.043(5) 0.074(7) O36 0.168(7) 0.185(8) 0.102(4) 0.009(5) 0.000(5) 0.063(6) O46 0.147(5) 0.076(3) 0.087(3) 0.003(3) 0.018(3) 0.002(3) O56 0.229(9) 0.094(4) 0.111(5) -0.008(4) 0.035(6) -0.037(5) O66A 0.42(5) 0.26(3) 0.18(2) -0.006(19) 0.05(2) -0.26(4) O66B 0.28(3) 0.22(3) 0.28(3) 0.00(3) 0.13(3) -0.04(3) C17 0.134(7) 0.064(4) 0.078(4) -0.011(3) 0.011(5) 0.010(5) C27 0.121(7) 0.084(5) 0.082(5) -0.012(4) 0.012(5) 0.015(5) C37 0.138(8) 0.071(4) 0.084(5) -0.005(4) -0.004(5) 0.013(5) C47 0.153(8) 0.068(4) 0.081(5) -0.006(4) 0.017(5) 0.012(5) C57 0.123(7) 0.071(4) 0.091(5) -0.016(4) 0.011(5) 0.007(5) C67 0.130(8) 0.098(6) 0.127(7) 0.006(6) 0.028(6) 0.004(6) O27 0.128(5) 0.088(3) 0.113(4) 0.006(3) 0.008(4) 0.009(4) O37 0.114(4) 0.105(4) 0.120(4) 0.009(3) -0.004(4) 0.011(4) O47 0.174(6) 0.070(3) 0.081(3) -0.005(2) 0.006(4) 0.014(4) O57 0.137(5) 0.071(3) 0.084(3) -0.006(2) -0.005(3) 0.001(3) O67 0.155(6) 0.087(4) 0.146(5) -0.012(4) 0.039(5) -0.014(4) O1W 0.45(3) 0.210(13) 0.226(13) 0.050(11) -0.065(16) -0.168(17) O2W 0.301(19) 0.171(10) 0.253(15) -0.032(11) -0.001(16) 0.015(13) O3AW 0.47(4) 0.122(10) 0.29(2) -0.049(13) -0.09(3) 0.080(18) O3BW 0.22(4) 0.22(4) 0.30(5) -0.02(4) 0.08(4) 0.03(4) O4W 0.222(17) 0.48(4) 0.26(2) -0.12(3) 0.014(16) 0.05(2) O5W 0.51(4) 0.47(3) 0.179(12) 0.059(17) -0.036(17) 0.24(3) O6W 0.216(17) 0.41(3) 0.49(4) -0.12(3) -0.02(2) -0.03(2) O7AW 0.32(4) 0.146(17) 0.38(5) 0.09(2) -0.18(4) -0.10(2) O7BW 0.52(7) 0.46(7) 0.13(2) 0.02(3) 0.02(3) -0.35(6) O8AW 0.67(9) 0.24(4) 0.11(2) -0.04(2) -0.10(4) 0.33(5) O8BW 0.27(3) 0.43(5) 0.36(4) -0.23(4) -0.17(3) 0.14(4) O9AW 0.24(3) 0.126(19) 0.31(4) 0.03(3) -0.04(3) -0.05(2) O9BW 0.31(5) 0.077(14) 0.076(14) 0.025(12) 0.02(2) -0.02(2) O10W 0.189(15) 0.25(2) 0.44(3) -0.05(2) 0.08(2) 0.058(15) O11W 0.35(2) 0.260(16) 0.34(2) -0.150(17) -0.22(2) 0.158(17) O12W 0.47(5) 0.32(4) 0.21(2) 0.07(2) -0.06(3) -0.08(4) O13W 0.26(3) 0.18(2) 0.37(5) 0.03(3) -0.18(4) -0.07(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 O42 1.403(9) . ? C11 O51 1.454(11) . ? C11 C21 1.639(14) . ? C21 O21 1.449(10) . ? C21 C31 1.488(11) . ? C31 O31 1.492(12) . ? C31 C41 1.578(12) . ? C41 O41 1.437(9) . ? C41 C51 1.584(13) . ? C51 O51 1.439(10) . ? C51 C61 1.585(12) . ? C61 O61 1.510(16) . ? O41 C17 1.425(9) . ? C12 O43 1.390(10) . ? C12 O52 1.472(11) . ? C12 C22 1.637(13) . ? C22 O22 1.479(11) . ? C22 C32 1.498(11) . ? C32 O32 1.470(10) . ? C32 C42 1.597(12) . ? C42 O42 1.466(9) . ? C42 C52 1.554(12) . ? C52 O52 1.478(10) . ? C52 C62 1.561(13) . ? C62 O62 1.339(18) . ? C13 O44 1.413(11) . ? C13 O53 1.462(12) . ? C13 C23 1.575(14) . ? C23 C33 1.468(14) . ? C23 O23 1.506(15) . ? C33 O33 1.504(12) . ? C33 C43 1.542(14) . ? C43 O43 1.448(10) . ? C43 C53 1.563(12) . ? C53 O53 1.433(10) . ? C53 C63 1.610(12) . ? C63 N63 1.509(12) . ? N63 C73 1.534(16) . ? C73 C83 1.524(15) . ? C83 C93 1.486(16) . ? C14 O54 1.460(16) . ? C14 C24 1.487(17) . ? C14 O45 1.526(12) . ? C24 C34 1.513(14) . ? C24 O24 1.538(14) . ? C34 O34 1.443(11) . ? C34 C44 1.582(15) . ? C44 O44 1.458(10) . ? C44 C54 1.565(13) . ? C54 O54 1.417(11) . ? C54 C64 1.544(14) . ? C64 O6A4 1.37(2) . ? C64 O6B4 1.409(19) . ? C15 O46 1.415(10) . ? C15 C25 1.509(14) . ? C15 O55 1.508(12) . ? C25 O25 1.540(13) . ? C25 C35 1.543(14) . ? C35 O35 1.416(13) . ? C35 C45 1.662(15) . ? C45 O45 1.404(11) . ? C45 C55 1.551(15) . ? C55 O55 1.434(11) . ? C55 C65 1.623(14) . ? C65 O65 1.354(14) . ? C16 O47 1.425(11) . ? C16 O56 1.456(17) . ? C16 C26 1.591(19) . ? C26 C36 1.512(15) . ? C26 O26 1.540(17) . ? C36 O36 1.496(15) . ? C36 C46 1.560(16) . ? C46 O46 1.445(10) . ? C46 C56 1.566(16) . ? C56 O56 1.455(13) . ? C56 C66 1.535(14) . ? C66 O66A 1.354(19) . ? C66 O66B 1.398(18) . ? C17 O57 1.466(11) . ? C17 C27 1.573(14) . ? C27 O27 1.495(12) . ? C27 C37 1.530(12) . ? C37 O37 1.459(11) . ? C37 C47 1.571(14) . ? C47 O47 1.409(10) . ? C47 C57 1.647(14) . ? C57 O57 1.461(10) . ? C57 C67 1.555(12) . ? C67 O67 1.396(12) . ? O9AW O9BW 1.40(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O42 C11 O51 110.7(7) . . ? O42 C11 C21 106.4(7) . . ? O51 C11 C21 113.1(6) . . ? O21 C21 C31 112.1(7) . . ? O21 C21 C11 108.4(6) . . ? C31 C21 C11 113.3(7) . . ? C21 C31 O31 111.3(7) . . ? C21 C31 C41 108.1(7) . . ? O31 C31 C41 115.0(6) . . ? O41 C41 C31 104.8(6) . . ? O41 C41 C51 112.1(7) . . ? C31 C41 C51 115.2(6) . . ? O51 C51 C41 112.4(7) . . ? O51 C51 C61 102.7(7) . . ? C41 C51 C61 116.3(7) . . ? O61 C61 C51 116.8(8) . . ? C17 O41 C41 118.6(5) . . ? C51 O51 C11 111.5(6) . . ? O43 C12 O52 111.5(6) . . ? O43 C12 C22 105.5(7) . . ? O52 C12 C22 112.2(7) . . ? O22 C22 C32 107.7(7) . . ? O22 C22 C12 109.9(6) . . ? C32 C22 C12 111.2(6) . . ? O32 C32 C22 110.0(6) . . ? O32 C32 C42 113.4(6) . . ? C22 C32 C42 105.9(7) . . ? O42 C42 C52 112.5(6) . . ? O42 C42 C32 102.6(6) . . ? C52 C42 C32 114.5(6) . . ? O52 C52 C42 111.1(6) . . ? O52 C52 C62 102.4(7) . . ? C42 C52 C62 119.2(8) . . ? O62 C62 C52 114.5(11) . . ? C11 O42 C42 117.3(6) . . ? C12 O52 C52 108.4(6) . . ? O44 C13 O53 111.7(7) . . ? O44 C13 C23 105.3(8) . . ? O53 C13 C23 113.5(7) . . ? C33 C23 O23 111.3(10) . . ? C33 C23 C13 113.4(8) . . ? O23 C23 C13 111.1(8) . . ? C23 C33 O33 112.1(8) . . ? C23 C33 C43 110.9(9) . . ? O33 C33 C43 114.4(7) . . ? O43 C43 C33 104.8(7) . . ? O43 C43 C53 111.1(7) . . ? C33 C43 C53 115.0(7) . . ? O53 C53 C43 109.2(7) . . ? O53 C53 C63 104.4(7) . . ? C43 C53 C63 118.0(7) . . ? N63 C63 C53 113.3(7) . . ? C12 O43 C43 120.1(6) . . ? C53 O53 C13 112.7(7) . . ? C63 N63 C73 114.4(8) . . ? C83 C73 N63 112.1(11) . . ? C93 C83 C73 115.2(14) . . ? O54 C14 C24 112.6(9) . . ? O54 C14 O45 114.6(9) . . ? C24 C14 O45 105.7(10) . . ? C14 C24 C34 111.4(8) . . ? C14 C24 O24 111.6(9) . . ? C34 C24 O24 106.5(9) . . ? O34 C34 C24 111.4(7) . . ? O34 C34 C44 111.4(7) . . ? C24 C34 C44 105.7(8) . . ? O44 C44 C54 109.3(7) . . ? O44 C44 C34 105.2(8) . . ? C54 C44 C34 111.9(7) . . ? O54 C54 C64 104.9(9) . . ? O54 C54 C44 108.7(7) . . ? C64 C54 C44 115.4(8) . . ? O6A4 C64 O6B4 112.4(17) . . ? O6A4 C64 C54 122.4(14) . . ? O6B4 C64 C54 110.8(14) . . ? C13 O44 C44 114.4(6) . . ? C54 O54 C14 111.7(8) . . ? O46 C15 C25 106.7(7) . . ? O46 C15 O55 110.7(7) . . ? C25 C15 O55 113.7(7) . . ? C15 C25 O25 113.8(8) . . ? C15 C25 C35 110.9(8) . . ? O25 C25 C35 108.6(8) . . ? O35 C35 C25 111.3(9) . . ? O35 C35 C45 111.9(8) . . ? C25 C35 C45 108.6(8) . . ? O45 C45 C55 111.7(9) . . ? O45 C45 C35 103.8(8) . . ? C55 C45 C35 114.3(8) . . ? O55 C55 C45 105.8(8) . . ? O55 C55 C65 108.6(8) . . ? C45 C55 C65 122.1(9) . . ? O65 C65 C55 111.4(10) . . ? C45 O45 C14 119.5(7) . . ? C55 O55 C15 115.4(7) . . ? O47 C16 O56 110.6(10) . . ? O47 C16 C26 106.6(10) . . ? O56 C16 C26 115.3(9) . . ? C36 C26 O26 111.9(11) . . ? C36 C26 C16 106.4(10) . . ? O26 C26 C16 114.2(8) . . ? O36 C36 C26 107.2(9) . . ? O36 C36 C46 115.5(8) . . ? C26 C36 C46 112.2(11) . . ? O46 C46 C36 107.9(8) . . ? O46 C46 C56 108.8(8) . . ? C36 C46 C56 114.8(8) . . ? O56 C56 C66 108.0(10) . . ? O56 C56 C46 107.8(10) . . ? C66 C56 C46 112.5(9) . . ? O66A C66 O66B 108(3) . . ? O66A C66 C56 114.7(16) . . ? O66B C66 C56 113.9(14) . . ? C15 O46 C46 119.6(6) . . ? C16 O56 C56 113.7(8) . . ? O41 C17 O57 108.3(7) . . ? O41 C17 C27 110.0(7) . . ? O57 C17 C27 113.9(6) . . ? O27 C27 C37 108.8(7) . . ? O27 C27 C17 112.2(7) . . ? C37 C27 C17 112.1(8) . . ? O37 C37 C27 109.5(8) . . ? O37 C37 C47 113.9(6) . . ? C27 C37 C47 107.1(7) . . ? O47 C47 C37 107.5(7) . . ? O47 C47 C57 107.4(8) . . ? C37 C47 C57 115.2(6) . . ? O57 C57 C67 106.9(7) . . ? O57 C57 C47 106.0(7) . . ? C67 C57 C47 116.6(7) . . ? O67 C67 C57 110.0(8) . . ? C47 O47 C16 119.5(7) . . ? C57 O57 C17 113.7(6) . . ? _diffrn_measured_fraction_theta_max 0.670 _diffrn_reflns_theta_full 74.20 _diffrn_measured_fraction_theta_full 0.670 _refine_diff_density_max 0.434 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.093 data_chabcd _audit_creation_method SHELXL-97 _chemical_name_systematic ; 6-deoxy-6-[(R)-1-cyclohexylethyl]aminocyclomaltoheptaose ; _chemical_name_common ; 6-deoxy-6-[(R)-1-cyclohexylethyl]amino-beta-cyclodextrin ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H101 N O42' _chemical_formula_weight 1388.3 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.215(1) _cell_length_b 15.862(1) _cell_length_c 15.417(1) _cell_angle_alpha 90.00 _cell_angle_beta 116.79(1) _cell_angle_gamma 90.00 _cell_volume 3321 _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1454 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6050 _diffrn_reflns_av_R_equivalents 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 74.53 _reflns_number_total 5850 _reflns_number_gt 4495 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(3) _refine_ls_number_reflns 5850 _refine_ls_number_parameters 878 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.2066 _refine_ls_wR_factor_gt 0.1892 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.6853(6) 0.1471(6) 0.4159(5) 0.079(2) Uani 1 1 d . . . H11 H 0.6897 0.1342 0.4799 0.095 Uiso 1 1 calc R . . C21 C 0.7790(6) 0.1927(8) 0.4291(6) 0.091(3) Uani 1 1 d . . . H21 H 0.8351 0.1569 0.4693 0.109 Uiso 1 1 calc R . . C31 C 0.7783(5) 0.2033(6) 0.3305(6) 0.079(2) Uani 1 1 d . . . H31 H 0.7263 0.2435 0.2923 0.095 Uiso 1 1 calc R . . C41 C 0.7563(5) 0.1206(5) 0.2755(5) 0.0647(17) Uani 1 1 d . . . H41 H 0.8109 0.0812 0.3091 0.078 Uiso 1 1 calc R . . C51 C 0.6626(5) 0.0824(5) 0.2668(5) 0.0605(16) Uani 1 1 d . . . H51 H 0.6081 0.1211 0.2303 0.073 Uiso 1 1 calc R . . C61 C 0.6384(6) -0.0043(6) 0.2168(6) 0.077(2) Uani 1 1 d . . . H61A H 0.6928 -0.0226 0.2048 0.092 Uiso 1 1 calc R . . H61B H 0.6305 -0.0451 0.2596 0.092 Uiso 1 1 calc R . . O21 O 0.7905(5) 0.2699(6) 0.4777(5) 0.116(3) Uani 1 1 d . . . O31 O 0.8710(5) 0.2379(6) 0.3442(6) 0.119(3) Uani 1 1 d . . . O41 O 0.7478(3) 0.1390(3) 0.1806(3) 0.0607(11) Uani 1 1 d . . . O51 O 0.6707(4) 0.0718(4) 0.3629(4) 0.0802(16) Uani 1 1 d . . . O61 O 0.5508(5) -0.0016(5) 0.1273(5) 0.0979(19) Uani 1 1 d . . . C12 C 0.3618(5) 0.2982(4) 0.3833(4) 0.0516(13) Uani 1 1 d . . . C22 C 0.4544(5) 0.3514(4) 0.4253(5) 0.0567(15) Uani 1 1 d . . . H22 H 0.4835 0.3493 0.4964 0.068 Uiso 1 1 calc R . . C32 C 0.5271(4) 0.3207(4) 0.3942(4) 0.0541(14) Uani 1 1 d . . . H32 H 0.5020 0.3319 0.3246 0.065 Uiso 1 1 calc R . . C42 C 0.5460(4) 0.2280(4) 0.4111(4) 0.0505(13) Uani 1 1 d . . . H42 H 0.5818 0.2171 0.4811 0.061 Uiso 1 1 calc R . . C52 C 0.4492(5) 0.1793(4) 0.3688(4) 0.0526(13) Uani 1 1 d . . . H52 H 0.4171 0.1866 0.2981 0.063 Uiso 1 1 calc R . . C62 C 0.4594(6) 0.0854(5) 0.3912(5) 0.0682(18) Uani 1 1 d . . . H62A H 0.3949 0.0592 0.3612 0.082 Uiso 1 1 calc R . . H62B H 0.4994 0.0597 0.3641 0.082 Uiso 1 1 calc R . . O22 O 0.4261(4) 0.4365(3) 0.3942(4) 0.0755(14) Uani 1 1 d . . . O32 O 0.6194(4) 0.3638(3) 0.4454(4) 0.0754(14) Uani 1 1 d . . . O42 O 0.6049(3) 0.2031(3) 0.3658(3) 0.0605(11) Uani 1 1 d . . . O52 O 0.3855(3) 0.2128(3) 0.4065(3) 0.0571(10) Uani 1 1 d . . . O62 O 0.5039(6) 0.0714(4) 0.4937(5) 0.0968(18) Uani 1 1 d . . . C13 C 0.0410(4) 0.3612(4) 0.0569(4) 0.0504(13) Uani 1 1 d . . . H13 H -0.0289 0.3760 0.0212 0.060 Uiso 1 1 calc R . . C23 C 0.0968(5) 0.4360(4) 0.1177(5) 0.0541(14) Uani 1 1 d . . . H23 H 0.0679 0.4522 0.1607 0.065 Uiso 1 1 calc R . . C33 C 0.2032(4) 0.4129(4) 0.1786(4) 0.0498(13) Uani 1 1 d . . . H33 H 0.2324 0.4015 0.1346 0.060 Uiso 1 1 calc R . . C43 C 0.2133(4) 0.3343(4) 0.2377(4) 0.0490(12) Uani 1 1 d . . . H43 H 0.1924 0.3463 0.2881 0.059 Uiso 1 1 calc R . . C53 C 0.1505(4) 0.2632(4) 0.1725(5) 0.0553(14) Uani 1 1 d . . . H53 H 0.1773 0.2457 0.1282 0.066 Uiso 1 1 calc R . . C63 C 0.1472(6) 0.1879(5) 0.2319(8) 0.095(3) Uani 1 1 d . . . H63A H 0.1020 0.1462 0.1889 0.114 Uiso 1 1 calc R . . H63B H 0.2120 0.1625 0.2638 0.114 Uiso 1 1 calc R . . O23 O 0.0866(4) 0.5041(3) 0.0536(4) 0.0646(12) Uani 1 1 d . . . O33 O 0.2526(4) 0.4835(3) 0.2371(4) 0.0703(13) Uani 1 1 d . . . O43 O 0.3138(3) 0.3104(3) 0.2819(3) 0.0475(9) Uani 1 1 d . . . O53 O 0.0509(3) 0.2910(3) 0.1172(3) 0.0605(11) Uani 1 1 d . . . O63 O 0.1161(5) 0.2120(6) 0.3042(6) 0.125(3) Uani 1 1 d . . . C14 C -0.0163(5) 0.3018(5) -0.3032(5) 0.0620(16) Uani 1 1 d . . . H14 H -0.0614 0.2919 -0.3718 0.074 Uiso 1 1 calc R . . C24 C -0.0362(5) 0.3886(5) -0.2744(5) 0.0659(18) Uani 1 1 d . . . H24 H -0.1061 0.3919 -0.2904 0.079 Uiso 1 1 calc R . . C34 C 0.0233(5) 0.4040(4) -0.1667(5) 0.0589(15) Uani 1 1 d . . . H34 H 0.0931 0.4083 -0.1511 0.071 Uiso 1 1 calc R . . C44 C 0.0095(4) 0.3312(4) -0.1101(4) 0.0532(14) Uani 1 1 d . . . H44 H -0.0583 0.3312 -0.1184 0.064 Uiso 1 1 calc R . . C54 C 0.0315(5) 0.2473(4) -0.1436(4) 0.0535(14) Uani 1 1 d . . . H54 H 0.1004 0.2469 -0.1319 0.064 Uiso 1 1 calc R . . C64 C 0.0131(6) 0.1709(4) -0.0957(6) 0.0628(16) Uani 1 1 d . . . H64A H 0.0336 0.1208 -0.1177 0.075 Uiso 1 1 calc R . . H64B H 0.0530 0.1752 -0.0259 0.075 Uiso 1 1 calc R . . O24 O -0.0170(5) 0.4489(4) -0.3300(4) 0.0887(18) Uani 1 1 d . . . O34 O -0.0081(5) 0.4818(3) -0.1428(4) 0.0813(15) Uani 1 1 d . . . O44 O 0.0766(3) 0.3424(3) -0.0093(3) 0.0491(9) Uani 1 1 d . . . O54 O -0.0309(3) 0.2381(3) -0.2463(3) 0.0637(12) Uani 1 1 d . . . O64 O -0.0872(4) 0.1623(3) -0.1161(4) 0.0711(13) Uani 1 1 d . . . C15 C 0.2427(7) 0.2310(5) -0.4352(5) 0.071(2) Uani 1 1 d . . . H15 H 0.2597 0.2127 -0.4865 0.085 Uiso 1 1 calc R . . C25 C 0.1922(8) 0.3164(6) -0.4620(7) 0.084(2) Uani 1 1 d . . . H25 H 0.1346 0.3122 -0.5256 0.101 Uiso 1 1 calc R . . C35 C 0.1581(7) 0.3431(5) -0.3855(6) 0.0721(19) Uani 1 1 d . . . H35 H 0.2168 0.3527 -0.3238 0.087 Uiso 1 1 calc R . . C45 C 0.0987(6) 0.2738(4) -0.3702(5) 0.0620(17) Uani 1 1 d . . . H45 H 0.0356 0.2680 -0.4286 0.074 Uiso 1 1 calc R . . C55 C 0.1526(6) 0.1904(4) -0.3480(5) 0.0658(17) Uani 1 1 d . . . H55 H 0.2122 0.1953 -0.2861 0.079 Uiso 1 1 calc R . . C65 C 0.0911(7) 0.1169(5) -0.3410(8) 0.087(3) Uani 1 1 d . . . O25 O 0.2596(6) 0.3745(4) -0.4684(6) 0.104(2) Uani 1 1 d . . . O35 O 0.1052(6) 0.4195(4) -0.4139(6) 0.101(2) Uani 1 1 d . . . O45 O 0.0811(3) 0.2992(3) -0.2906(3) 0.0552(10) Uani 1 1 d . . . O55 O 0.1812(4) 0.1707(3) -0.4240(4) 0.0752(14) Uani 1 1 d . . . O65 O 0.0174(10) 0.1060(9) -0.4321(10) 0.073(6) Uani 0.44(2) 1 d P . . O6'5 O 0.1475(9) 0.0442(6) -0.3043(9) 0.080(5) Uani 0.56(2) 1 d P . . C16 C 0.6176(7) 0.1597(6) -0.2314(6) 0.080(2) Uani 1 1 d . . . H16 H 0.6796 0.1386 -0.2282 0.096 Uiso 1 1 calc R . . C26 C 0.5948(7) 0.2452(6) -0.2795(7) 0.085(2) Uani 1 1 d . . . H26 H 0.5924 0.2395 -0.3438 0.102 Uiso 1 1 calc R . . C36 C 0.4970(7) 0.2751(5) -0.2931(6) 0.073(2) Uani 1 1 d . . . H36 H 0.5005 0.2855 -0.2289 0.088 Uiso 1 1 calc R . . C46 C 0.4197(6) 0.2096(5) -0.3438(6) 0.0676(19) Uani 1 1 d . . . H46 H 0.4115 0.2023 -0.4102 0.081 Uiso 1 1 calc R . . C56 C 0.4492(7) 0.1261(5) -0.2906(6) 0.0700(19) Uani 1 1 d . . . H56 H 0.4543 0.1334 -0.2254 0.084 Uiso 1 1 calc R . . C66 C 0.3796(8) 0.0538(5) -0.3400(6) 0.082(2) Uani 1 1 d . . . H66A H 0.4057 0.0028 -0.3023 0.098 Uiso 1 1 calc R . . H66B H 0.3165 0.0655 -0.3412 0.098 Uiso 1 1 calc R . . O26 O 0.6731(5) 0.3029(5) -0.2235(6) 0.104(2) Uani 1 1 d . . . O36 O 0.4720(6) 0.3532(4) -0.3467(5) 0.0923(18) Uani 1 1 d . . . O46 O 0.3290(4) 0.2392(3) -0.3478(4) 0.0707(13) Uani 1 1 d . . . O56 O 0.5420(5) 0.1013(4) -0.2815(4) 0.0789(15) Uani 1 1 d . . . O66 O 0.3654(5) 0.0400(4) -0.4349(4) 0.0803(15) Uani 1 1 d . . . C17 C 0.8080(5) 0.0953(5) 0.1490(6) 0.0676(18) Uani 1 1 d . . . H17 H 0.8617 0.0678 0.2046 0.081 Uiso 1 1 calc R . . C27 C 0.8513(6) 0.1620(6) 0.1051(7) 0.077(2) Uani 1 1 d . . . H27 H 0.8988 0.1341 0.0879 0.092 Uiso 1 1 calc R . . C37 C 0.7708(6) 0.1997(5) 0.0144(7) 0.073(2) Uani 1 1 d . . . H37 H 0.7284 0.2343 0.0327 0.087 Uiso 1 1 calc R . . C47 C 0.7079(5) 0.1317(5) -0.0561(6) 0.0648(17) Uani 1 1 d . . . H47 H 0.7478 0.1014 -0.0812 0.078 Uiso 1 1 calc R . . C57 C 0.6721(5) 0.0698(4) -0.0036(5) 0.0592(15) Uani 1 1 d . . . H57 H 0.6294 0.0994 0.0186 0.071 Uiso 1 1 calc R . . C67 C 0.6155(6) -0.0027(5) -0.0688(6) 0.0714(19) Uani 1 1 d . . . H67A H 0.5552 0.0188 -0.1211 0.086 Uiso 1 1 calc R . . H67B H 0.6546 -0.0273 -0.0976 0.086 Uiso 1 1 calc R . . O27 O 0.9013(4) 0.2241(4) 0.1762(5) 0.0906(18) Uani 1 1 d . . . O37 O 0.8119(4) 0.2523(4) -0.0337(5) 0.0836(16) Uani 1 1 d . . . O47 O 0.6286(4) 0.1713(3) -0.1338(4) 0.0706(13) Uani 1 1 d . . . O57 O 0.7547(3) 0.0348(3) 0.0790(4) 0.0657(12) Uani 1 1 d . . . C1 C 0.5567(6) -0.2230(5) -0.0529(6) 0.0683(18) Uani 1 1 d . . . H1 H 0.5040 -0.2596 -0.0979 0.082 Uiso 1 1 calc R . . C2 C 0.5752(8) -0.2483(7) 0.0460(7) 0.088(3) Uani 1 1 d . . . H2A H 0.5156 -0.2403 0.0531 0.105 Uiso 1 1 calc R . . H2B H 0.6259 -0.2123 0.0929 0.105 Uiso 1 1 calc R . . C3 C 0.6074(10) -0.3388(7) 0.0672(8) 0.108(3) Uani 1 1 d . . . H3A H 0.6253 -0.3504 0.1349 0.130 Uiso 1 1 calc R . . H3B H 0.5521 -0.3748 0.0281 0.130 Uiso 1 1 calc R . . C4 C 0.6907(8) -0.3611(7) 0.0482(9) 0.100(3) Uani 1 1 d . . . H4A H 0.7008 -0.4216 0.0549 0.120 Uiso 1 1 calc R . . H4B H 0.7498 -0.3342 0.0965 0.120 Uiso 1 1 calc R . . C5 C 0.6756(10) -0.3351(7) -0.0504(10) 0.108(3) Uani 1 1 d . . . H5A H 0.6238 -0.3691 -0.0990 0.130 Uiso 1 1 calc R . . H5B H 0.7356 -0.3448 -0.0563 0.130 Uiso 1 1 calc R . . C6 C 0.6471(8) -0.2409(6) -0.0692(7) 0.089(3) Uani 1 1 d . . . H6A H 0.7019 -0.2064 -0.0256 0.106 Uiso 1 1 calc R . . H6B H 0.6328 -0.2265 -0.1354 0.106 Uiso 1 1 calc R . . C7 C 0.5202(6) -0.1309(6) -0.0813(7) 0.086(2) Uani 1 1 d . . . H7 H 0.5144 -0.1211 -0.1465 0.103 Uiso 1 1 calc R . . C8 C 0.4180(8) -0.1158(8) -0.0870(11) 0.134(5) Uani 1 1 d . . . H8A H 0.4217 -0.1216 -0.0235 0.201 Uiso 1 1 calc R . . H8B H 0.3723 -0.1564 -0.1301 0.201 Uiso 1 1 calc R . . H8C H 0.3960 -0.0600 -0.1111 0.201 Uiso 1 1 calc R . . N1 N 0.5910(5) -0.0686(4) -0.0161(5) 0.0728(16) Uani 1 1 d . . . O1W O 0.2001(7) 0.6161(7) 0.3321(6) 0.135(3) Uani 1 1 d . . . O2AW O 0.1135(14) -0.0365(18) -0.1609(16) 0.186(9) Uani 0.60 1 d P . . O2BW O -0.0112(11) -0.1204(10) -0.3056(11) 0.081(4) Uani 0.40 1 d P . . O3W O -0.1311(11) -0.0012(8) -0.4131(10) 0.177(4) Uani 1 1 d . . . O4W O 0.6005(10) 0.4604(9) -0.1727(12) 0.198(6) Uani 1 1 d . . . O5W O -0.0947(10) 0.4050(7) -0.5773(8) 0.165(4) Uani 1 1 d . . . O6AW O -0.1759(10) 0.5519(8) -0.4041(9) 0.171(7) Uani 0.77 1 d P . . O6BW O -0.024(2) 0.6226(17) -0.3834(17) 0.088(8) Uani 0.23 1 d P . . O7W O 0.7087(8) 0.4009(10) -0.3501(10) 0.182(5) Uani 1 1 d . . . O8AW O 0.2043(18) -0.0759(11) -0.008(3) 0.187(14) Uani 0.45 1 d P . . O8BW O 0.1911(16) 0.0019(15) 0.141(3) 0.27(2) Uani 0.55 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.084(5) 0.100(6) 0.039(3) 0.002(4) 0.016(3) 0.033(5) C21 0.054(4) 0.141(9) 0.062(4) -0.015(5) 0.011(3) 0.025(5) C31 0.043(3) 0.106(6) 0.081(5) -0.031(5) 0.022(3) -0.010(4) C41 0.049(3) 0.077(5) 0.058(4) -0.001(3) 0.015(3) 0.007(3) C51 0.060(4) 0.062(4) 0.055(3) 0.012(3) 0.023(3) 0.012(3) C61 0.087(5) 0.067(5) 0.081(5) 0.011(4) 0.041(4) 0.007(4) O21 0.071(4) 0.168(7) 0.082(4) -0.065(5) 0.012(3) -0.010(4) O31 0.068(3) 0.147(7) 0.136(6) -0.072(5) 0.042(4) -0.043(4) O41 0.057(2) 0.061(3) 0.067(3) -0.009(2) 0.031(2) 0.000(2) O51 0.096(4) 0.086(4) 0.063(3) 0.024(3) 0.039(3) 0.034(3) O61 0.090(4) 0.102(5) 0.096(4) -0.013(4) 0.037(4) -0.004(4) C12 0.063(3) 0.050(3) 0.038(3) 0.004(2) 0.019(2) 0.001(3) C22 0.070(4) 0.045(3) 0.047(3) -0.004(3) 0.018(3) 0.001(3) C32 0.054(3) 0.051(3) 0.047(3) 0.003(3) 0.014(3) -0.007(3) C42 0.054(3) 0.056(3) 0.034(2) 0.004(2) 0.014(2) -0.003(3) C52 0.061(3) 0.051(3) 0.046(3) 0.002(2) 0.024(3) 0.001(3) C62 0.082(5) 0.049(4) 0.068(4) -0.001(3) 0.029(4) -0.005(3) O22 0.094(4) 0.042(2) 0.068(3) -0.009(2) 0.016(3) -0.001(2) O32 0.068(3) 0.063(3) 0.082(3) 0.004(3) 0.022(3) -0.013(2) O42 0.055(2) 0.079(3) 0.045(2) 0.011(2) 0.0197(19) 0.015(2) O52 0.068(3) 0.052(2) 0.055(2) 0.0107(19) 0.030(2) 0.000(2) O62 0.120(4) 0.071(4) 0.093(4) 0.029(3) 0.043(3) 0.020(3) C13 0.047(3) 0.049(3) 0.054(3) 0.006(3) 0.022(3) 0.001(2) C23 0.061(4) 0.043(3) 0.062(3) 0.005(3) 0.031(3) 0.007(3) C33 0.050(3) 0.042(3) 0.054(3) -0.006(2) 0.020(3) -0.003(2) C43 0.049(3) 0.043(3) 0.058(3) -0.002(3) 0.027(3) -0.001(2) C53 0.046(3) 0.052(3) 0.061(3) 0.003(3) 0.018(3) -0.003(3) C63 0.059(4) 0.059(4) 0.119(7) 0.039(5) -0.003(5) -0.009(3) O23 0.079(3) 0.040(2) 0.068(3) 0.010(2) 0.027(2) 0.013(2) O33 0.076(3) 0.042(2) 0.078(3) -0.009(2) 0.022(2) -0.003(2) O43 0.053(2) 0.049(2) 0.0403(18) -0.0018(16) 0.0208(16) 0.0000(17) O53 0.053(2) 0.057(3) 0.070(3) 0.014(2) 0.026(2) -0.0062(19) O63 0.082(4) 0.165(8) 0.137(6) 0.087(6) 0.056(4) 0.011(4) C14 0.056(4) 0.066(4) 0.052(3) -0.002(3) 0.013(3) -0.005(3) C24 0.058(4) 0.077(5) 0.059(4) 0.023(3) 0.023(3) 0.012(3) C34 0.064(4) 0.045(3) 0.062(4) 0.010(3) 0.023(3) 0.010(3) C44 0.044(3) 0.047(3) 0.055(3) 0.008(3) 0.011(2) 0.002(2) C54 0.053(3) 0.049(3) 0.053(3) -0.002(3) 0.018(3) -0.006(3) C64 0.077(4) 0.043(3) 0.072(4) 0.000(3) 0.036(3) -0.006(3) O24 0.117(5) 0.072(3) 0.081(3) 0.032(3) 0.049(3) 0.028(3) O34 0.101(4) 0.046(3) 0.087(3) 0.010(2) 0.034(3) 0.024(3) O44 0.0426(19) 0.049(2) 0.051(2) 0.0002(18) 0.0175(16) 0.0017(17) O54 0.066(3) 0.066(3) 0.052(2) -0.008(2) 0.020(2) -0.023(2) O64 0.077(3) 0.054(3) 0.087(3) -0.004(2) 0.042(3) -0.013(2) C15 0.110(6) 0.054(4) 0.062(4) -0.002(3) 0.051(4) 0.007(4) C25 0.119(7) 0.067(5) 0.083(5) 0.016(4) 0.061(5) 0.007(5) C35 0.106(6) 0.047(3) 0.083(5) 0.010(3) 0.060(4) 0.005(4) C45 0.078(4) 0.053(4) 0.048(3) -0.004(3) 0.022(3) -0.001(3) C55 0.090(5) 0.047(3) 0.062(4) -0.002(3) 0.036(4) -0.008(3) C65 0.090(6) 0.051(4) 0.116(7) -0.002(4) 0.043(5) -0.016(4) O25 0.157(6) 0.076(4) 0.132(6) 0.022(4) 0.112(5) 0.015(4) O35 0.146(6) 0.056(3) 0.141(6) 0.028(3) 0.101(5) 0.023(3) O45 0.055(2) 0.056(2) 0.049(2) -0.0004(19) 0.0180(18) -0.0057(19) O55 0.101(4) 0.053(3) 0.075(3) -0.010(2) 0.042(3) -0.005(3) O65 0.079(10) 0.055(8) 0.072(9) -0.008(6) 0.021(7) -0.013(6) O6'5 0.101(9) 0.044(6) 0.096(9) 0.000(5) 0.046(7) 0.000(5) C16 0.111(6) 0.077(5) 0.081(5) -0.001(4) 0.069(5) 0.003(5) C26 0.119(7) 0.079(5) 0.086(5) -0.001(4) 0.071(5) -0.009(5) C36 0.110(6) 0.057(4) 0.073(4) -0.003(3) 0.059(5) 0.001(4) C46 0.109(6) 0.049(3) 0.067(4) -0.003(3) 0.060(4) 0.006(4) C56 0.104(6) 0.057(4) 0.068(4) -0.002(3) 0.056(4) 0.003(4) C66 0.122(7) 0.056(4) 0.081(5) 0.005(4) 0.056(5) 0.006(4) O26 0.115(5) 0.088(4) 0.136(6) 0.000(4) 0.082(5) -0.022(4) O36 0.145(5) 0.058(3) 0.106(4) 0.003(3) 0.085(4) -0.003(3) O46 0.103(4) 0.058(3) 0.068(3) -0.005(2) 0.054(3) 0.000(3) O56 0.110(4) 0.062(3) 0.076(3) 0.000(3) 0.052(3) 0.009(3) O66 0.107(4) 0.066(3) 0.068(3) -0.003(3) 0.039(3) 0.006(3) C17 0.054(4) 0.078(5) 0.076(4) -0.019(4) 0.033(3) -0.002(3) C27 0.070(4) 0.073(5) 0.105(6) -0.020(4) 0.055(4) -0.009(4) C37 0.069(4) 0.065(4) 0.106(6) -0.007(4) 0.059(4) -0.007(4) C47 0.071(4) 0.059(4) 0.086(5) -0.011(4) 0.054(4) -0.006(3) C57 0.062(4) 0.054(4) 0.066(4) -0.009(3) 0.032(3) -0.003(3) C67 0.076(5) 0.069(4) 0.073(4) -0.014(4) 0.038(4) -0.011(4) O27 0.073(3) 0.087(4) 0.125(5) -0.038(4) 0.056(3) -0.033(3) O37 0.090(4) 0.068(3) 0.118(4) -0.005(3) 0.069(3) -0.018(3) O47 0.083(3) 0.072(3) 0.074(3) 0.001(3) 0.051(3) 0.010(3) O57 0.063(3) 0.056(3) 0.080(3) -0.011(2) 0.034(2) 0.000(2) C1 0.074(4) 0.059(4) 0.076(4) -0.010(3) 0.038(4) -0.012(3) C2 0.104(6) 0.091(6) 0.095(6) -0.002(5) 0.069(5) -0.015(5) C3 0.148(9) 0.089(7) 0.099(7) 0.023(6) 0.064(7) -0.019(7) C4 0.103(7) 0.085(6) 0.127(8) 0.019(6) 0.065(6) -0.002(5) C5 0.128(9) 0.073(6) 0.150(10) 0.003(6) 0.086(8) 0.001(6) C6 0.125(7) 0.075(5) 0.092(6) -0.003(4) 0.072(6) -0.013(5) C7 0.078(5) 0.077(5) 0.081(5) -0.011(4) 0.017(4) -0.014(4) C8 0.089(7) 0.086(8) 0.183(13) -0.035(8) 0.023(7) -0.003(6) N1 0.091(4) 0.058(3) 0.073(4) -0.010(3) 0.040(3) -0.018(3) O1W 0.154(7) 0.153(8) 0.087(4) 0.017(5) 0.043(5) 0.061(7) O2AW 0.167(16) 0.24(3) 0.188(18) 0.039(18) 0.116(15) -0.008(16) O2BW 0.089(9) 0.077(9) 0.097(10) 0.030(8) 0.059(8) 0.018(7) O3W 0.231(12) 0.120(8) 0.195(11) -0.010(8) 0.109(10) -0.008(9) O4W 0.208(12) 0.155(10) 0.276(17) -0.070(11) 0.150(12) -0.018(9) O5W 0.215(11) 0.111(7) 0.138(7) 0.033(6) 0.053(7) -0.012(7) O6AW 0.154(9) 0.113(8) 0.137(9) -0.053(7) -0.031(7) 0.058(8) O6BW 0.104(17) 0.075(15) 0.066(13) -0.001(12) 0.023(12) 0.048(14) O7W 0.158(9) 0.199(13) 0.195(11) 0.019(10) 0.085(8) -0.006(9) O8AW 0.176(19) 0.067(10) 0.41(4) 0.000(17) 0.21(3) -0.009(12) O8BW 0.122(13) 0.111(14) 0.59(6) 0.00(3) 0.16(3) -0.004(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 O51 1.408(11) . ? C11 O42 1.424(9) . ? C11 C21 1.528(14) . ? C21 O21 1.404(13) . ? C21 C31 1.525(13) . ? C31 O31 1.438(10) . ? C31 C41 1.515(12) . ? C41 O41 1.439(9) . ? C41 C51 1.499(10) . ? C51 O51 1.440(8) . ? C51 C61 1.538(11) . ? C61 O61 1.423(11) . ? O41 C17 1.400(8) . ? C12 O52 1.407(8) . ? C12 O43 1.409(7) . ? C12 C22 1.514(9) . ? C22 O22 1.432(8) . ? C22 C32 1.474(10) . ? C32 O32 1.436(8) . ? C32 C42 1.499(9) . ? C42 O42 1.417(8) . ? C42 C52 1.525(9) . ? C52 O52 1.439(8) . ? C52 C62 1.520(10) . ? C62 O62 1.429(10) . ? C13 O44 1.387(7) . ? C13 O53 1.416(7) . ? C13 C23 1.513(9) . ? C23 O23 1.425(8) . ? C23 C33 1.505(9) . ? C33 O33 1.421(7) . ? C33 C43 1.512(9) . ? C43 O43 1.416(7) . ? C43 C53 1.527(9) . ? C53 O53 1.432(7) . ? C53 C63 1.519(10) . ? C63 O63 1.445(15) . ? C14 O45 1.407(8) . ? C14 O54 1.419(9) . ? C14 C24 1.518(11) . ? C24 O24 1.400(9) . ? C24 C34 1.510(10) . ? C34 O34 1.430(8) . ? C34 C44 1.518(9) . ? C44 O44 1.435(7) . ? C44 C54 1.519(9) . ? C54 O54 1.440(7) . ? C54 C64 1.509(9) . ? C64 O64 1.418(9) . ? C15 O46 1.401(10) . ? C15 O55 1.402(10) . ? C15 C25 1.520(12) . ? C25 O25 1.415(12) . ? C25 C35 1.546(12) . ? C35 O35 1.412(10) . ? C35 C45 1.508(11) . ? C45 O45 1.427(8) . ? C45 C55 1.512(10) . ? C55 O55 1.456(9) . ? C55 C65 1.529(11) . ? C65 O65 1.355(17) . ? C65 O6'5 1.395(15) . ? C16 O56 1.407(11) . ? C16 O47 1.448(9) . ? C16 C26 1.510(13) . ? C26 O26 1.440(12) . ? C26 C36 1.484(13) . ? C36 O36 1.442(10) . ? C36 C46 1.499(12) . ? C46 O46 1.433(10) . ? C46 C56 1.515(10) . ? C56 O56 1.410(10) . ? C56 C66 1.514(12) . ? C66 O66 1.396(10) . ? C17 O57 1.398(9) . ? C17 C27 1.554(12) . ? C27 O27 1.413(10) . ? C27 C37 1.506(13) . ? C37 O37 1.433(9) . ? C37 C47 1.524(11) . ? C47 O47 1.408(10) . ? C47 C57 1.521(10) . ? C57 O57 1.437(9) . ? C57 C67 1.514(10) . ? C67 N1 1.472(11) . ? C1 C2 1.476(12) . ? C1 C6 1.532(12) . ? C1 C7 1.554(13) . ? C2 C3 1.505(16) . ? C3 C4 1.467(16) . ? C4 C5 1.490(17) . ? C5 C6 1.546(15) . ? C7 N1 1.473(10) . ? C7 C8 1.537(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O51 C11 O42 110.1(6) . . ? O51 C11 C21 111.9(7) . . ? O42 C11 C21 107.4(8) . . ? O21 C21 C31 112.2(10) . . ? O21 C21 C11 111.7(7) . . ? C31 C21 C11 109.4(6) . . ? O31 C31 C41 111.5(6) . . ? O31 C31 C21 109.4(7) . . ? C41 C31 C21 111.3(9) . . ? O41 C41 C51 110.1(5) . . ? O41 C41 C31 106.9(7) . . ? C51 C41 C31 111.1(6) . . ? O51 C51 C41 108.6(6) . . ? O51 C51 C61 107.5(6) . . ? C41 C51 C61 114.1(6) . . ? O61 C61 C51 111.5(7) . . ? C17 O41 C41 118.7(6) . . ? C11 O51 C51 114.6(6) . . ? O52 C12 O43 111.1(5) . . ? O52 C12 C22 110.2(5) . . ? O43 C12 C22 108.4(5) . . ? O22 C22 C32 111.0(6) . . ? O22 C22 C12 107.5(5) . . ? C32 C22 C12 111.5(5) . . ? O32 C32 C22 110.9(6) . . ? O32 C32 C42 107.9(5) . . ? C22 C32 C42 112.4(5) . . ? O42 C42 C32 107.6(5) . . ? O42 C42 C52 110.6(5) . . ? C32 C42 C52 110.5(5) . . ? O52 C52 C62 106.7(6) . . ? O52 C52 C42 109.7(5) . . ? C62 C52 C42 114.8(6) . . ? O62 C62 C52 110.7(6) . . ? C42 O42 C11 119.1(5) . . ? C12 O52 C52 113.3(5) . . ? O44 C13 O53 110.7(5) . . ? O44 C13 C23 109.2(5) . . ? O53 C13 C23 110.2(5) . . ? O23 C23 C33 111.5(5) . . ? O23 C23 C13 108.0(5) . . ? C33 C23 C13 110.0(5) . . ? O33 C33 C23 108.5(5) . . ? O33 C33 C43 112.7(5) . . ? C23 C33 C43 111.4(5) . . ? O43 C43 C33 107.7(5) . . ? O43 C43 C53 109.8(5) . . ? C33 C43 C53 110.4(5) . . ? O53 C53 C63 106.7(5) . . ? O53 C53 C43 110.2(5) . . ? C63 C53 C43 111.3(6) . . ? O63 C63 C53 111.7(8) . . ? C12 O43 C43 118.5(5) . . ? C13 O53 C53 113.8(5) . . ? O45 C14 O54 110.1(5) . . ? O45 C14 C24 108.8(5) . . ? O54 C14 C24 111.0(6) . . ? O24 C24 C34 112.0(7) . . ? O24 C24 C14 108.5(6) . . ? C34 C24 C14 111.7(5) . . ? O34 C34 C24 108.7(5) . . ? O34 C34 C44 111.1(6) . . ? C24 C34 C44 109.8(6) . . ? O44 C44 C34 108.3(5) . . ? O44 C44 C54 108.6(5) . . ? C34 C44 C54 111.3(5) . . ? O54 C54 C64 106.4(5) . . ? O54 C54 C44 109.0(5) . . ? C64 C54 C44 114.8(5) . . ? O64 C64 C54 112.8(6) . . ? C13 O44 C44 120.0(4) . . ? C14 O54 C54 113.5(5) . . ? O46 C15 O55 109.5(6) . . ? O46 C15 C25 108.5(7) . . ? O55 C15 C25 111.0(7) . . ? O25 C25 C15 107.8(8) . . ? O25 C25 C35 112.2(8) . . ? C15 C25 C35 109.8(6) . . ? O35 C35 C45 112.1(7) . . ? O35 C35 C25 109.8(6) . . ? C45 C35 C25 110.5(7) . . ? O45 C45 C35 106.7(6) . . ? O45 C45 C55 110.2(6) . . ? C35 C45 C55 111.8(6) . . ? O55 C55 C45 109.5(6) . . ? O55 C55 C65 107.9(6) . . ? C45 C55 C65 113.4(7) . . ? O65 C65 O6'5 112.7(10) . . ? O65 C65 C55 105.7(9) . . ? O6'5 C65 C55 112.0(8) . . ? C14 O45 C45 118.9(5) . . ? C15 O55 C55 114.3(5) . . ? O56 C16 O47 109.8(6) . . ? O56 C16 C26 111.8(8) . . ? O47 C16 C26 106.8(7) . . ? O26 C26 C36 112.8(8) . . ? O26 C26 C16 109.4(8) . . ? C36 C26 C16 110.6(7) . . ? O36 C36 C26 110.1(7) . . ? O36 C36 C46 110.7(7) . . ? C26 C36 C46 110.6(7) . . ? O46 C46 C36 108.0(6) . . ? O46 C46 C56 110.8(6) . . ? C36 C46 C56 110.6(7) . . ? O56 C56 C66 106.3(6) . . ? O56 C56 C46 109.8(6) . . ? C66 C56 C46 114.8(7) . . ? O66 C66 C56 112.9(7) . . ? C15 O46 C46 118.5(5) . . ? C16 O56 C56 113.9(6) . . ? O57 C17 O41 111.4(5) . . ? O57 C17 C27 110.1(6) . . ? O41 C17 C27 106.7(6) . . ? O27 C27 C37 111.8(7) . . ? O27 C27 C17 108.8(7) . . ? C37 C27 C17 110.4(6) . . ? O37 C37 C27 110.4(6) . . ? O37 C37 C47 108.9(7) . . ? C27 C37 C47 111.6(7) . . ? O47 C47 C57 111.5(6) . . ? O47 C47 C37 108.2(6) . . ? C57 C47 C37 109.8(6) . . ? O57 C57 C67 107.7(6) . . ? O57 C57 C47 109.9(6) . . ? C67 C57 C47 111.7(6) . . ? N1 C67 C57 112.5(6) . . ? C47 O47 C16 118.8(6) . . ? C17 O57 C57 113.1(6) . . ? C2 C1 C6 110.6(8) . . ? C2 C1 C7 115.1(8) . . ? C6 C1 C7 111.2(7) . . ? C1 C2 C3 112.1(8) . . ? C4 C3 C2 114.3(8) . . ? C3 C4 C5 112.8(10) . . ? C4 C5 C6 111.1(10) . . ? C1 C6 C5 110.2(8) . . ? N1 C7 C8 110.1(8) . . ? N1 C7 C1 112.4(7) . . ? C8 C7 C1 112.8(9) . . ? C67 N1 C7 112.9(7) . . ? _diffrn_measured_fraction_theta_max 0.829 _diffrn_reflns_theta_full 74.53 _diffrn_measured_fraction_theta_full 0.829 _refine_diff_density_max 0.592 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.064 data_rphabcd _audit_creation_method SHELXL-97 _chemical_name_systematic ; 6-deoxy-6-[(R)-1-phenylethyl]aminocyclomaltoheptaose ; _chemical_name_common ; 6-deoxy-6-[(R)-1-phenylrthyl]amino-beta-cyclodextrin ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H105 N O43' _chemical_formula_weight 1456.4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.019(2) _cell_length_b 9.115(1) _cell_length_c 25.988(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.96(1) _cell_angle_gamma 90.00 _cell_volume 3480 _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1438 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5727 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 74.21 _reflns_number_total 5721 _reflns_number_gt 5111 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1601P)^2^+0.6574P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 5727 _refine_ls_number_parameters 993 _refine_ls_number_restraints 214 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2061 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.393 _refine_ls_shift/su_mean 0.015 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.4553(5) 0.5605(10) 0.6106(3) 0.0566(19) Uani 1 1 d . . . H11 H 0.4551 0.5646 0.5729 0.068 Uiso 1 1 calc R . . C21 C 0.5494(5) 0.5143(11) 0.6399(3) 0.061(2) Uani 1 1 d . . . H21 H 0.5950 0.5822 0.6315 0.073 Uiso 1 1 calc R . . C31 C 0.5518(4) 0.5185(11) 0.6990(2) 0.0543(19) Uani 1 1 d . . . H31 H 0.5104 0.4432 0.7074 0.065 Uiso 1 1 calc R . . C41 C 0.5225(4) 0.6644(9) 0.7156(2) 0.0479(16) Uani 1 1 d . . . H41 H 0.5683 0.7391 0.7131 0.058 Uiso 1 1 calc R . . C51 C 0.4292(5) 0.7095(9) 0.6823(2) 0.0474(15) Uani 1 1 d . . . H51 H 0.3832 0.6398 0.6890 0.057 Uiso 1 1 calc R . . C61 C 0.3983(7) 0.8634(12) 0.6920(4) 0.077(3) Uani 1 1 d . . . H61A H 0.3387 0.8804 0.6699 0.092 Uiso 1 1 calc R . . H61B H 0.3925 0.8716 0.7284 0.092 Uiso 1 1 calc R . . O21 O 0.5681(4) 0.3680(10) 0.6240(2) 0.085(2) Uani 1 1 d . . . O31 O 0.6419(4) 0.4860(10) 0.7267(2) 0.084(2) Uani 1 1 d . . . O41 O 0.5134(3) 0.6480(6) 0.76925(15) 0.0418(10) Uani 1 1 d . . . O51 O 0.4332(4) 0.7018(7) 0.62734(17) 0.0603(14) Uani 1 1 d . . . O61 O 0.4578(10) 0.9710(12) 0.6817(4) 0.146(4) Uani 1 1 d . . . C12 O 0.1815(6) 0.2154(12) 0.5340(3) 0.108(3) Uani 1 1 d . . . H12 H 0.1423 0.1615 0.5053 0.129 Uiso 1 1 calc R . . C22 C 0.2735(6) 0.1418(12) 0.5468(4) 0.071(2) Uani 1 1 d . . . H22 H 0.2997 0.1429 0.5153 0.085 Uiso 1 1 calc R . . C32 C 0.3358(5) 0.2276(10) 0.5898(3) 0.0595(19) Uani 1 1 d . . . H32 H 0.3127 0.2216 0.6224 0.071 Uiso 1 1 calc R . . C42 C 0.3394(5) 0.3843(9) 0.5740(2) 0.0490(16) Uani 1 1 d . . . H42 H 0.3712 0.3920 0.5447 0.059 Uiso 1 1 calc R . . C52 C 0.2452(5) 0.4513(10) 0.5580(3) 0.0525(17) Uani 1 1 d . . . H52 H 0.2173 0.4567 0.5888 0.063 Uiso 1 1 calc R . . C62 C 0.2456(6) 0.6031(11) 0.5341(4) 0.069(2) Uani 1 1 d . . . H62A H 0.1836 0.6371 0.5220 0.083 Uiso 1 1 calc R . . H62B H 0.2768 0.6714 0.5604 0.083 Uiso 1 1 calc R . . O22 O 0.2630(6) -0.0076(8) 0.5615(4) 0.095(2) Uani 1 1 d . . . O32 O 0.4250(4) 0.1623(8) 0.5981(3) 0.088(2) Uani 1 1 d . . . O42 O 0.3902(3) 0.4582(7) 0.61871(17) 0.0539(12) Uani 1 1 d . . . O52 O 0.1889(4) 0.3611(7) 0.51803(19) 0.0621(14) Uani 1 1 d . . . O62 O 0.2910(5) 0.5981(9) 0.4906(3) 0.089(2) Uani 1 1 d . . . C13A C -0.1010(11) 0.133(2) 0.6256(6) 0.080(7) Uani 0.50 1 d PDU A 1 C23A C -0.0596(12) 0.0023(19) 0.6019(7) 0.079(8) Uani 0.50 1 d PDU A 1 C33A C 0.0411(12) 0.0371(18) 0.6017(9) 0.066(7) Uani 0.50 1 d PDU A 1 C43A C 0.0455(11) 0.1813(19) 0.5718(10) 0.087(9) Uani 0.50 1 d PDU A 1 C53A C 0.0020(11) 0.3044(18) 0.5977(10) 0.071(7) Uani 0.50 1 d PDU A 1 C63A C -0.0093(17) 0.442(2) 0.5642(7) 0.079(8) Uani 0.50 1 d PDU A 1 O23A O -0.062(2) -0.125(2) 0.6353(10) 0.091(7) Uani 0.50 1 d PDU A 1 O33A O 0.0764(16) -0.082(3) 0.5760(11) 0.094(9) Uani 0.50 1 d PDU A 1 O53A O -0.0914(9) 0.263(2) 0.5975(6) 0.069(5) Uani 0.50 1 d PDU A 1 O63A O -0.0512(13) 0.558(2) 0.5869(7) 0.074(5) Uani 0.50 1 d PDU A 1 C13B C -0.0929(13) 0.087(2) 0.6275(6) 0.095(9) Uani 0.50 1 d PDU A 2 C23B C -0.0375(13) -0.0366(19) 0.6113(7) 0.089(9) Uani 0.50 1 d PDU A 2 C33B C 0.0603(13) 0.015(2) 0.6097(11) 0.083(9) Uani 0.50 1 d PDU A 2 C43B C 0.0535(9) 0.1496(19) 0.5742(5) 0.067(6) Uani 0.50 1 d PDU A 2 C53B C -0.0073(11) 0.265(2) 0.5897(8) 0.088(9) Uani 0.50 1 d PDU A 2 C63B C -0.021(3) 0.390(3) 0.5493(11) 0.119(13) Uani 0.50 1 d PDU A 2 O23B O -0.035(2) -0.163(3) 0.6435(14) 0.122(12) Uani 0.50 1 d PDU A 2 O33B O 0.1035(15) -0.104(2) 0.5877(11) 0.089(8) Uani 0.50 1 d PDU A 2 O53B O -0.0959(11) 0.204(2) 0.5900(6) 0.098(9) Uani 0.50 1 d PDU A 2 O63B O -0.065(2) 0.508(3) 0.5700(10) 0.132(12) Uani 0.50 1 d PDU A 2 O43 O 0.1426(3) 0.2089(8) 0.57909(18) 0.0662(16) Uani 1 1 d D . . C14 C -0.1395(4) 0.2188(10) 0.8186(2) 0.0512(17) Uani 1 1 d . . . H14 H -0.1808 0.2306 0.8429 0.061 Uiso 1 1 calc R . . C24 C -0.1426(5) 0.0621(11) 0.8002(3) 0.059(2) Uani 1 1 d . . . H24 H -0.2060 0.0395 0.7838 0.071 Uiso 1 1 calc R . . C34 C -0.0857(6) 0.0420(11) 0.7581(3) 0.062(2) Uani 1 1 d . . . H34 H -0.0214 0.0573 0.7741 0.074 Uiso 1 1 calc R . . C44 C -0.1150(5) 0.1542(14) 0.7148(3) 0.074(3) Uani 1 1 d . A . H44 H -0.1781 0.1354 0.6970 0.088 Uiso 1 1 calc R . . C54 C -0.1070(5) 0.3087(13) 0.7377(3) 0.066(2) Uani 1 1 d . . . H54 H -0.0439 0.3253 0.7558 0.079 Uiso 1 1 calc R . . C64 C -0.1370(7) 0.4340(18) 0.7010(4) 0.099(4) Uani 1 1 d . . . H64A H -0.1349 0.5238 0.7213 0.118 Uiso 1 1 calc R . . H64B H -0.0950 0.4444 0.6775 0.118 Uiso 1 1 calc R . . O24 O -0.1161(4) -0.0347(7) 0.8442(2) 0.0644(14) Uani 1 1 d . . . O34 O -0.0980(6) -0.1045(10) 0.7381(3) 0.101(3) Uani 1 1 d . . . O44 O -0.0566(3) 0.1353(9) 0.67880(17) 0.074(2) Uani 1 1 d D . . O54 O -0.1653(3) 0.3173(8) 0.77606(19) 0.0626(15) Uani 1 1 d . . . O64 O -0.2252(5) 0.4143(15) 0.6713(3) 0.129(4) Uani 1 1 d . . . C15 C 0.0904(4) 0.4514(7) 0.9796(2) 0.0366(12) Uani 1 1 d . . . H15 H 0.1045 0.4939 1.0150 0.044 Uiso 1 1 calc R . . C25 C 0.0728(4) 0.2882(8) 0.9837(2) 0.0398(13) Uani 1 1 d . . . H25 H 0.0227 0.2757 1.0022 0.048 Uiso 1 1 calc R . . C35 C 0.0443(4) 0.2219(7) 0.9299(2) 0.0372(12) Uani 1 1 d . . . H35 H 0.0959 0.2266 0.9123 0.045 Uiso 1 1 calc R . . C45 C -0.0347(4) 0.3076(7) 0.8972(2) 0.0360(12) Uani 1 1 d . . . H45 H -0.0894 0.2933 0.9117 0.043 Uiso 1 1 calc R . . C55 C -0.0125(4) 0.4697(8) 0.8968(2) 0.0417(13) Uani 1 1 d . . . H55 H 0.0380 0.4842 0.8787 0.050 Uiso 1 1 calc R . . C65 C -0.0917(5) 0.5641(10) 0.8711(3) 0.0568(18) Uani 1 1 d . . . H65A H -0.0724 0.6659 0.8727 0.068 Uiso 1 1 calc R . . H65B H -0.1099 0.5371 0.8343 0.068 Uiso 1 1 calc R . . O25 O 0.1515(3) 0.2152(6) 1.01351(17) 0.0501(11) Uani 1 1 d . . . O35 O 0.0153(3) 0.0717(5) 0.93053(19) 0.0471(11) Uani 1 1 d . . . O45 O -0.0493(3) 0.2486(5) 0.84559(16) 0.0435(10) Uani 1 1 d . . . O55 O 0.0142(3) 0.5214(5) 0.95008(17) 0.0431(10) Uani 1 1 d . . . O65 O -0.1683(3) 0.5502(7) 0.8956(2) 0.0632(15) Uani 1 1 d . . . C16 C 0.3990(3) 0.7152(7) 0.9677(2) 0.0354(12) Uani 1 1 d . . . H16 H 0.4469 0.7873 0.9805 0.043 Uiso 1 1 calc R . . C26 C 0.4028(4) 0.5969(7) 1.0091(2) 0.0346(12) Uani 1 1 d . . . H26 H 0.3960 0.6419 1.0423 0.041 Uiso 1 1 calc R . . C36 C 0.3262(4) 0.4888(7) 0.9912(2) 0.0349(12) Uani 1 1 d . . . H36 H 0.3358 0.4423 0.9588 0.042 Uiso 1 1 calc R . . C46 C 0.2347(3) 0.5723(7) 0.9782(2) 0.0341(12) Uani 1 1 d . . . H46 H 0.2208 0.6135 1.0105 0.041 Uiso 1 1 calc R . . C56 C 0.2384(4) 0.6940(7) 0.9390(2) 0.0379(13) Uani 1 1 d . . . H56 H 0.2453 0.6505 0.9056 0.046 Uiso 1 1 calc R . . C66 C 0.1545(4) 0.7917(9) 0.9292(3) 0.0541(18) Uani 1 1 d . . . H66A H 0.1603 0.8648 0.9030 0.065 Uiso 1 1 calc R . . H66B H 0.1012 0.7326 0.9153 0.065 Uiso 1 1 calc R . . O26 O 0.4893(2) 0.5263(5) 1.01639(15) 0.0415(10) Uani 1 1 d . . . O36 O 0.3231(3) 0.3769(5) 1.02843(17) 0.0447(10) Uani 1 1 d . . . O46 O 0.1672(2) 0.4658(5) 0.95636(16) 0.0381(9) Uani 1 1 d . . . O56 O 0.3139(3) 0.7876(5) 0.95795(18) 0.0419(10) Uani 1 1 d . . . O66 O 0.1422(4) 0.8623(7) 0.9749(3) 0.0770(18) Uani 1 1 d . . . C17 C 0.5640(4) 0.7421(9) 0.8071(2) 0.0450(16) Uani 1 1 d . . . H17 H 0.6113 0.7889 0.7919 0.054 Uiso 1 1 calc R . . C27 C 0.6103(4) 0.6487(9) 0.8543(2) 0.0445(15) Uani 1 1 d . . . H27 H 0.6531 0.7113 0.8782 0.053 Uiso 1 1 calc R . . C37 C 0.5405(4) 0.5895(9) 0.8840(2) 0.0453(15) Uani 1 1 d . . . H37 H 0.5013 0.5188 0.8615 0.054 Uiso 1 1 calc R . . C47 C 0.4822(3) 0.7155(8) 0.8968(2) 0.0393(13) Uani 1 1 d . . . H47 H 0.5197 0.7841 0.9211 0.047 Uiso 1 1 calc R . . C57 C 0.4384(4) 0.7943(8) 0.8466(2) 0.0403(13) Uani 1 1 d . . . H57 H 0.4033 0.7222 0.8226 0.048 Uiso 1 1 calc R . . C67 C 0.3766(4) 0.9221(8) 0.8512(2) 0.0433(14) Uani 1 1 d . . . H67A H 0.3461 0.9527 0.8162 0.052 Uiso 1 1 calc R . . H67B H 0.3302 0.8903 0.8698 0.052 Uiso 1 1 calc R . . O27 O 0.6607(3) 0.5328(7) 0.83638(18) 0.0543(13) Uani 1 1 d . . . O37 O 0.5880(3) 0.5158(7) 0.93001(19) 0.0619(14) Uani 1 1 d . . . O47 O 0.4155(3) 0.6508(5) 0.92116(14) 0.0382(9) Uani 1 1 d . . . O57 O 0.5093(3) 0.8518(5) 0.82208(17) 0.0446(10) Uani 1 1 d . . . N67 N 0.4260(3) 1.0493(7) 0.8792(2) 0.0431(12) Uani 1 1 d . . . C1 C 0.3650(4) 1.1778(8) 0.8797(3) 0.0467(15) Uani 1 1 d . . . H1 H 0.4044 1.2604 0.8937 0.056 Uiso 1 1 calc R . . C2 C 0.3010(5) 1.1549(10) 0.9169(3) 0.0553(17) Uani 1 1 d . . . H2A H 0.2620 1.0728 0.9053 0.083 Uiso 1 1 calc R . . H2B H 0.2647 1.2414 0.9174 0.083 Uiso 1 1 calc R . . H2C H 0.3357 1.1361 0.9516 0.083 Uiso 1 1 calc R . . C1P C 0.3156(5) 1.2228(10) 0.8241(3) 0.0598(19) Uani 1 1 d . . . C2P C 0.3634(6) 1.2816(13) 0.7898(4) 0.078(3) Uani 1 1 d . . . H2P H 0.4255 1.2983 0.8011 0.094 Uiso 1 1 calc R . . C3P C 0.3213(8) 1.3177(17) 0.7378(4) 0.099(4) Uani 1 1 d . . . H3P H 0.3558 1.3565 0.7152 0.119 Uiso 1 1 calc R . . C4P C 0.2311(9) 1.296(2) 0.7207(5) 0.135(7) Uani 1 1 d . . . H4P H 0.2024 1.3303 0.6877 0.162 Uiso 1 1 calc R . . C5P C 0.1807(8) 1.223(3) 0.7522(5) 0.132(7) Uani 1 1 d . . . H5P H 0.1211 1.1947 0.7386 0.158 Uiso 1 1 calc R . . C6P C 0.2208(7) 1.1945(19) 0.8036(4) 0.103(4) Uani 1 1 d . . . H6P H 0.1856 1.1555 0.8258 0.124 Uiso 1 1 calc R . . C1M C 0.289(3) 0.358(7) 0.3098(17) 0.24(3) Uani 0.52 1 d PDU . . O1M O 0.233(3) 0.288(8) 0.266(3) 0.34(3) Uani 0.52 1 d PDU . . C2M C 0.5467(17) 0.378(5) 0.4928(11) 0.232(14) Uani 1 1 d DU . . O2M O 0.6440(15) 0.3656(19) 0.5286(9) 0.230(8) Uani 1 1 d DU . . C3M C -0.195(3) 0.688(3) 0.6042(10) 0.265(18) Uani 1 1 d DU . . O3M O -0.2435(8) 0.5617(17) 0.5808(4) 0.144(4) Uani 1 1 d DU . . C4M C 0.343(2) 0.444(5) 0.3843(15) 0.230(19) Uani 0.66 1 d PDU . . O4M O 0.3063(12) 0.370(2) 0.4230(5) 0.127(5) Uani 0.66 1 d PDU . . C5M C 0.097(6) -0.296(10) 0.7420(18) 0.38(5) Uani 0.44 1 d PDU . . O5M O 0.094(4) -0.277(7) 0.7958(15) 0.34(4) Uani 0.44 1 d PDU . . O1W O 0.2763(5) 0.4904(12) 1.1156(3) 0.108(3) Uani 1 1 d . . . O2W O 0.6089(11) 1.138(2) 0.7411(8) 0.215(8) Uani 1 1 d . . . O3W O 0.137(3) -0.326(4) 0.6521(19) 0.46(3) Uani 1 1 d . . . O4W O 0.2628(14) 0.854(3) 1.0647(8) 0.254(10) Uani 1 1 d . . . O5W O 0.3925(6) 0.7073(13) 1.1561(5) 0.138(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.060(4) 0.077(6) 0.031(3) -0.007(3) 0.005(3) -0.018(4) C21 0.053(4) 0.085(6) 0.044(3) -0.017(4) 0.009(3) -0.007(4) C31 0.041(3) 0.087(6) 0.034(3) -0.011(3) 0.006(2) 0.007(4) C41 0.046(3) 0.070(5) 0.028(3) -0.008(3) 0.010(2) -0.006(3) C51 0.050(3) 0.057(4) 0.031(3) 0.004(3) -0.002(2) 0.002(3) C61 0.092(6) 0.078(7) 0.055(4) 0.009(5) 0.000(4) 0.020(5) O21 0.065(3) 0.121(6) 0.067(3) -0.045(4) 0.008(3) 0.011(4) O31 0.043(3) 0.147(7) 0.058(3) -0.032(4) 0.002(2) 0.027(3) O41 0.039(2) 0.057(3) 0.0293(17) -0.0038(19) 0.0062(15) 0.000(2) O51 0.075(3) 0.066(4) 0.035(2) 0.005(2) -0.001(2) -0.004(3) O61 0.224(12) 0.079(6) 0.121(7) 0.003(6) 0.002(7) -0.023(8) C12 0.110(6) 0.122(7) 0.090(5) 0.002(5) 0.020(4) -0.031(6) C22 0.069(5) 0.070(6) 0.078(5) -0.006(5) 0.028(4) -0.009(5) C32 0.050(4) 0.074(5) 0.055(4) 0.008(4) 0.011(3) 0.001(4) C42 0.051(3) 0.066(5) 0.030(3) -0.003(3) 0.009(2) 0.000(3) C52 0.043(3) 0.072(5) 0.040(3) 0.003(3) 0.003(3) 0.000(3) C62 0.057(4) 0.073(6) 0.071(5) 0.009(5) -0.002(4) 0.004(4) O22 0.095(5) 0.063(4) 0.131(6) -0.003(4) 0.030(4) -0.014(4) O32 0.068(4) 0.069(4) 0.122(6) 0.009(4) 0.008(4) 0.018(3) O42 0.056(3) 0.072(3) 0.0320(19) 0.000(2) 0.0033(18) -0.010(2) O52 0.059(3) 0.080(4) 0.042(2) 0.003(3) 0.000(2) -0.019(3) O62 0.100(5) 0.090(5) 0.075(4) 0.026(4) 0.017(3) -0.009(4) C13A 0.046(10) 0.17(2) 0.025(9) 0.020(11) 0.010(7) -0.031(11) C23A 0.060(10) 0.142(19) 0.030(9) 0.011(11) -0.003(8) -0.060(12) C33A 0.050(9) 0.121(17) 0.024(8) -0.020(10) 0.002(7) -0.037(11) C43A 0.039(10) 0.139(19) 0.085(16) 0.045(14) 0.020(10) -0.011(12) C53A 0.042(9) 0.120(15) 0.056(13) -0.003(11) 0.019(9) -0.010(10) C63A 0.060(11) 0.13(2) 0.040(9) 0.044(13) 0.004(8) 0.018(13) O23A 0.110(16) 0.128(16) 0.049(9) -0.018(10) 0.050(11) -0.065(13) O33A 0.080(14) 0.142(18) 0.063(14) -0.008(11) 0.018(12) -0.025(12) O53A 0.036(6) 0.138(14) 0.030(6) 0.007(8) 0.001(5) -0.027(7) O63A 0.067(9) 0.100(12) 0.056(9) 0.004(8) 0.012(7) -0.011(8) C13B 0.079(16) 0.16(2) 0.040(13) -0.034(13) 0.005(11) -0.033(15) C23B 0.093(16) 0.15(2) 0.017(7) -0.018(12) -0.001(9) -0.052(16) C33B 0.078(15) 0.124(19) 0.048(14) 0.000(13) 0.012(12) -0.036(14) C43B 0.068(13) 0.125(16) 0.004(5) -0.002(8) -0.001(6) -0.021(12) C53B 0.061(13) 0.18(2) 0.018(7) 0.035(12) -0.012(7) -0.022(13) C63B 0.11(2) 0.17(3) 0.08(2) 0.01(2) 0.011(17) 0.02(2) O23B 0.13(2) 0.14(2) 0.096(18) -0.030(16) 0.029(14) -0.078(18) O33B 0.083(14) 0.128(17) 0.056(12) -0.016(11) 0.017(11) -0.055(11) O53B 0.070(10) 0.18(2) 0.033(7) 0.001(11) -0.007(6) -0.050(11) O63B 0.131(19) 0.17(3) 0.088(18) 0.051(18) -0.006(14) 0.03(2) O43 0.058(3) 0.103(5) 0.036(2) 0.001(3) 0.008(2) -0.023(3) C14 0.037(3) 0.075(5) 0.039(3) 0.009(3) 0.004(2) -0.008(3) C24 0.056(4) 0.083(6) 0.037(3) -0.005(4) 0.009(3) -0.026(4) C34 0.063(4) 0.082(6) 0.042(3) -0.014(4) 0.013(3) -0.023(4) C44 0.048(4) 0.132(9) 0.038(3) 0.008(5) 0.002(3) -0.031(5) C54 0.046(4) 0.097(7) 0.053(4) 0.021(5) 0.006(3) -0.003(4) C64 0.076(6) 0.153(13) 0.068(5) 0.047(7) 0.015(4) 0.030(7) O24 0.079(3) 0.068(4) 0.047(3) 0.001(3) 0.017(2) -0.020(3) O34 0.148(7) 0.093(5) 0.074(4) -0.038(4) 0.048(4) -0.052(5) O44 0.051(3) 0.137(6) 0.035(2) -0.002(3) 0.0097(19) -0.024(3) O54 0.045(2) 0.093(4) 0.047(3) 0.013(3) 0.002(2) 0.002(3) O64 0.077(4) 0.236(13) 0.074(4) 0.063(6) 0.014(3) 0.044(6) C15 0.029(2) 0.045(3) 0.037(3) 0.000(3) 0.008(2) 0.004(2) C25 0.030(3) 0.047(4) 0.043(3) 0.006(3) 0.008(2) 0.001(3) C35 0.029(2) 0.042(3) 0.040(3) 0.009(3) 0.007(2) 0.002(2) C45 0.029(2) 0.046(3) 0.034(3) 0.006(3) 0.008(2) 0.002(2) C55 0.030(3) 0.045(3) 0.049(3) 0.011(3) 0.006(2) 0.005(2) C65 0.051(4) 0.057(5) 0.056(4) 0.003(4) -0.004(3) 0.011(3) O25 0.040(2) 0.059(3) 0.046(2) 0.019(2) -0.0043(17) 0.003(2) O35 0.045(2) 0.038(2) 0.055(3) 0.007(2) 0.0032(19) 0.0012(19) O45 0.0340(19) 0.058(3) 0.039(2) 0.000(2) 0.0074(16) -0.0029(19) O55 0.0303(18) 0.046(3) 0.051(2) -0.004(2) 0.0039(16) 0.0043(18) O65 0.036(2) 0.080(4) 0.068(3) -0.021(3) -0.004(2) 0.017(3) C16 0.030(2) 0.041(3) 0.036(3) -0.005(3) 0.009(2) -0.004(2) C26 0.028(2) 0.043(3) 0.032(2) -0.006(2) 0.0059(19) 0.002(2) C36 0.029(2) 0.036(3) 0.038(3) 0.009(2) 0.005(2) 0.001(2) C46 0.029(2) 0.037(3) 0.037(3) 0.000(2) 0.007(2) 0.002(2) C56 0.030(2) 0.042(3) 0.043(3) 0.001(3) 0.009(2) -0.002(2) C66 0.034(3) 0.051(4) 0.075(5) 0.016(4) 0.006(3) 0.007(3) O26 0.0287(18) 0.053(3) 0.042(2) 0.000(2) 0.0048(15) 0.0063(19) O36 0.041(2) 0.045(3) 0.048(2) 0.014(2) 0.0088(18) 0.0044(19) O46 0.0282(18) 0.045(2) 0.042(2) -0.0044(19) 0.0093(15) 0.0001(17) O56 0.0319(19) 0.042(2) 0.054(2) -0.002(2) 0.0127(17) 0.0005(18) O66 0.067(3) 0.065(4) 0.107(5) 0.004(4) 0.037(3) 0.019(3) C17 0.033(3) 0.068(5) 0.036(3) -0.017(3) 0.012(2) -0.007(3) C27 0.032(3) 0.063(4) 0.039(3) -0.017(3) 0.010(2) 0.003(3) C37 0.036(3) 0.061(4) 0.039(3) -0.001(3) 0.008(2) 0.008(3) C47 0.024(2) 0.055(4) 0.037(3) -0.007(3) 0.004(2) -0.001(3) C57 0.034(3) 0.057(4) 0.031(3) -0.003(3) 0.010(2) 0.000(3) C67 0.038(3) 0.050(4) 0.040(3) -0.001(3) 0.003(2) 0.000(3) O27 0.033(2) 0.083(4) 0.046(2) -0.016(3) 0.0057(17) 0.012(2) O37 0.054(3) 0.082(4) 0.051(3) 0.012(3) 0.014(2) 0.026(3) O47 0.0359(19) 0.047(2) 0.0323(18) -0.0070(18) 0.0085(15) -0.0051(18) O57 0.043(2) 0.052(3) 0.042(2) -0.003(2) 0.0156(17) -0.002(2) N67 0.042(2) 0.049(3) 0.037(2) 0.001(2) 0.005(2) 0.002(2) C1 0.042(3) 0.043(4) 0.055(4) -0.001(3) 0.009(3) 0.004(3) C2 0.057(4) 0.057(5) 0.052(4) -0.004(4) 0.012(3) 0.008(4) C1P 0.054(4) 0.066(5) 0.060(4) 0.018(4) 0.014(3) 0.010(4) C2P 0.058(4) 0.092(7) 0.079(6) 0.013(6) 0.003(4) -0.011(5) C3P 0.099(7) 0.126(11) 0.070(6) 0.036(7) 0.010(5) -0.025(7) C4P 0.092(8) 0.211(19) 0.094(8) 0.070(11) 0.002(7) 0.032(11) C5P 0.066(6) 0.22(2) 0.095(8) 0.052(11) -0.008(6) 0.012(9) C6P 0.062(5) 0.155(13) 0.087(7) 0.026(8) 0.004(5) -0.018(7) C1M 0.18(3) 0.40(7) 0.18(4) 0.12(4) 0.09(3) 0.19(4) O1M 0.21(4) 0.34(7) 0.46(7) 0.05(7) 0.02(4) -0.03(5) C2M 0.20(2) 0.28(4) 0.25(3) 0.02(3) 0.13(2) 0.06(3) O2M 0.251(19) 0.122(11) 0.32(2) -0.025(15) 0.076(18) 0.015(13) C3M 0.36(4) 0.25(3) 0.17(2) 0.02(2) 0.02(2) -0.19(3) O3M 0.136(8) 0.191(13) 0.108(7) 0.035(8) 0.034(6) 0.007(9) C4M 0.21(3) 0.29(5) 0.18(3) 0.03(4) 0.03(3) 0.10(4) O4M 0.158(12) 0.152(14) 0.085(8) -0.005(9) 0.059(8) 0.003(11) C5M 0.53(10) 0.20(6) 0.26(6) -0.05(5) -0.24(6) 0.11(6) O5M 0.54(8) 0.23(5) 0.15(3) -0.02(3) -0.17(4) 0.02(5) O1W 0.099(5) 0.131(7) 0.104(5) -0.021(6) 0.050(4) 0.005(5) O2W 0.170(13) 0.175(15) 0.268(19) 0.024(15) -0.028(12) -0.009(12) O3W 0.67(7) 0.24(3) 0.58(6) 0.09(4) 0.40(6) 0.19(4) O4W 0.279(19) 0.24(2) 0.27(2) -0.108(19) 0.110(16) -0.107(19) O5W 0.095(6) 0.108(7) 0.205(11) -0.026(8) 0.018(6) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 O42 1.399(9) . ? C11 O51 1.421(11) . ? C11 C21 1.520(11) . ? C21 O21 1.440(13) . ? C21 C31 1.532(9) . ? C31 O31 1.427(8) . ? C31 C41 1.493(12) . ? C41 O41 1.436(7) . ? C41 C51 1.542(9) . ? C51 O51 1.443(8) . ? C51 C61 1.515(13) . ? C61 O61 1.389(16) . ? O41 C17 1.403(7) . ? C12 O52 1.402(12) . ? C12 O43 1.415(9) . ? C12 C22 1.510(14) . ? C22 O22 1.432(13) . ? C22 C32 1.518(13) . ? C32 O32 1.441(10) . ? C32 C42 1.490(13) . ? C42 O42 1.421(8) . ? C42 C52 1.519(10) . ? C52 O52 1.451(9) . ? C52 C62 1.518(13) . ? C62 O62 1.435(12) . ? C13A O44 1.405(15) . ? C13A O53A 1.411(15) . ? C13A C23A 1.533(16) . ? C23A O23A 1.452(16) . ? C23A C33A 1.547(15) . ? C33A O33A 1.432(16) . ? C33A C43A 1.535(16) . ? C43A O43 1.454(15) . ? C43A C53A 1.524(17) . ? C53A O53A 1.452(15) . ? C53A C63A 1.517(16) . ? C63A O63A 1.419(14) . ? C13B O44 1.404(17) . ? C13B O53B 1.441(16) . ? C13B C23B 1.510(16) . ? C23B O23B 1.422(17) . ? C23B C33B 1.552(16) . ? C33B O33B 1.443(17) . ? C33B C43B 1.523(16) . ? C43B O43 1.424(14) . ? C43B C53B 1.501(15) . ? C53B O53B 1.442(16) . ? C53B C63B 1.533(19) . ? C63B O63B 1.423(14) . ? C14 O54 1.414(9) . ? C14 O45 1.417(7) . ? C14 C24 1.504(13) . ? C24 O24 1.434(10) . ? C24 C34 1.532(10) . ? C34 O34 1.431(12) . ? C34 C44 1.517(14) . ? C44 O44 1.419(10) . ? C44 C54 1.523(17) . ? C54 O54 1.459(10) . ? C54 C64 1.495(15) . ? C64 O64 1.400(13) . ? C15 O55 1.394(7) . ? C15 O46 1.415(7) . ? C15 C25 1.519(10) . ? C25 O25 1.436(7) . ? C25 C35 1.501(9) . ? C35 O35 1.438(8) . ? C35 C45 1.523(8) . ? C45 O45 1.420(7) . ? C45 C55 1.516(10) . ? C55 O55 1.439(8) . ? C55 C65 1.508(9) . ? C65 O65 1.431(10) . ? C16 O47 1.413(7) . ? C16 O56 1.414(7) . ? C16 C26 1.516(9) . ? C26 O26 1.426(7) . ? C26 C36 1.513(8) . ? C36 O36 1.413(7) . ? C36 C46 1.545(7) . ? C46 O46 1.433(7) . ? C46 C56 1.516(8) . ? C56 O56 1.424(7) . ? C56 C66 1.520(9) . ? C66 O66 1.395(11) . ? C17 O57 1.400(8) . ? C17 C27 1.536(10) . ? C27 O27 1.433(8) . ? C27 C37 1.523(9) . ? C37 O37 1.428(8) . ? C37 C47 1.522(9) . ? C47 O47 1.420(7) . ? C47 C57 1.515(8) . ? C57 O57 1.448(7) . ? C57 C67 1.509(10) . ? C67 N67 1.484(9) . ? N67 C1 1.489(9) . ? C1 C2 1.513(10) . ? C1 C1P 1.537(10) . ? C1P C2P 1.364(12) . ? C1P C6P 1.436(12) . ? C2P C3P 1.407(13) . ? C3P C4P 1.351(17) . ? C4P C5P 1.39(2) . ? C5P C6P 1.373(15) . ? C1M O1M 1.42(2) . ? C2M O2M 1.566(18) . ? C3M O3M 1.433(18) . ? C4M O4M 1.41(2) . ? C5M O5M 1.42(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O42 C11 O51 110.1(6) . . ? O42 C11 C21 110.3(7) . . ? O51 C11 C21 110.5(6) . . ? O21 C21 C11 109.3(6) . . ? O21 C21 C31 110.1(8) . . ? C11 C21 C31 108.7(6) . . ? O31 C31 C41 110.2(6) . . ? O31 C31 C21 108.8(6) . . ? C41 C31 C21 111.4(7) . . ? O41 C41 C31 106.2(6) . . ? O41 C41 C51 108.4(5) . . ? C31 C41 C51 111.3(6) . . ? O51 C51 C61 106.7(6) . . ? O51 C51 C41 108.9(5) . . ? C61 C51 C41 115.3(7) . . ? O61 C61 C51 112.9(9) . . ? C17 O41 C41 118.0(5) . . ? C11 O51 C51 114.0(6) . . ? O52 C12 O43 110.9(8) . . ? O52 C12 C22 111.1(7) . . ? O43 C12 C22 108.3(7) . . ? O22 C22 C12 109.6(8) . . ? O22 C22 C32 112.2(9) . . ? C12 C22 C32 109.3(8) . . ? O32 C32 C42 110.5(7) . . ? O32 C32 C22 108.0(8) . . ? C42 C32 C22 110.0(7) . . ? O42 C42 C32 105.8(6) . . ? O42 C42 C52 110.1(6) . . ? C32 C42 C52 112.1(7) . . ? O52 C52 C42 109.8(7) . . ? O52 C52 C62 106.0(6) . . ? C42 C52 C62 113.3(7) . . ? O62 C62 C52 109.7(8) . . ? C11 O42 C42 117.7(5) . . ? C12 O52 C52 113.3(6) . . ? O44 C13A O53A 114.8(13) . . ? O44 C13A C23A 104.8(12) . . ? O53A C13A C23A 110.6(11) . . ? O23A C23A C13A 108.5(12) . . ? O23A C23A C33A 108.3(14) . . ? C13A C23A C33A 108.6(11) . . ? O33A C33A C43A 110.8(14) . . ? O33A C33A C23A 107.6(13) . . ? C43A C33A C23A 108.8(12) . . ? O43 C43A C53A 109.0(14) . . ? O43 C43A C33A 103.2(13) . . ? C53A C43A C33A 109.8(13) . . ? O53A C53A C63A 102.7(16) . . ? O53A C53A C43A 108.0(13) . . ? C63A C53A C43A 111.2(14) . . ? O63A C63A C53A 112.4(14) . . ? C13A O53A C53A 114.7(11) . . ? O44 C13B O53B 111.1(14) . . ? O44 C13B C23B 111.7(13) . . ? O53B C13B C23B 107.9(12) . . ? O23B C23B C13B 113.1(14) . . ? O23B C23B C33B 110.7(15) . . ? C13B C23B C33B 111.0(12) . . ? O33B C33B C43B 110.0(16) . . ? O33B C33B C23B 106.6(14) . . ? C43B C33B C23B 108.5(13) . . ? O43 C43B C53B 108.8(12) . . ? O43 C43B C33B 107.9(11) . . ? C53B C43B C33B 111.4(11) . . ? O53B C53B C43B 110.4(14) . . ? O53B C53B C63B 107(2) . . ? C43B C53B C63B 109.8(13) . . ? O63B C63B C53B 108.1(17) . . ? C13B O53B C53B 112.8(12) . . ? C12 O43 C43B 118.8(7) . . ? C12 O43 C43A 118.3(11) . . ? C43B O43 C43A 12.5(11) . . ? O54 C14 O45 110.2(6) . . ? O54 C14 C24 111.7(6) . . ? O45 C14 C24 107.6(6) . . ? O24 C24 C14 110.3(5) . . ? O24 C24 C34 113.1(8) . . ? C14 C24 C34 110.8(7) . . ? O34 C34 C44 111.4(7) . . ? O34 C34 C24 108.8(7) . . ? C44 C34 C24 109.3(8) . . ? O44 C44 C34 106.4(8) . . ? O44 C44 C54 111.1(8) . . ? C34 C44 C54 110.3(6) . . ? O54 C54 C64 104.5(8) . . ? O54 C54 C44 107.9(7) . . ? C64 C54 C44 117.9(8) . . ? O64 C64 C54 112.3(11) . . ? C13B O44 C13A 18.0(14) . . ? C13B O44 C44 119.6(9) . . ? C13A O44 C44 114.7(8) . . ? C14 O54 C54 113.2(6) . . ? O55 C15 O46 111.8(5) . . ? O55 C15 C25 110.6(5) . . ? O46 C15 C25 106.9(5) . . ? O25 C25 C35 111.1(5) . . ? O25 C25 C15 110.8(5) . . ? C35 C25 C15 110.5(5) . . ? O35 C35 C25 113.6(5) . . ? O35 C35 C45 107.0(5) . . ? C25 C35 C45 110.6(5) . . ? O45 C45 C55 110.7(5) . . ? O45 C45 C35 106.4(5) . . ? C55 C45 C35 110.9(5) . . ? O55 C55 C65 106.0(6) . . ? O55 C55 C45 109.3(5) . . ? C65 C55 C45 113.9(5) . . ? O65 C65 C55 112.7(6) . . ? C14 O45 C45 119.0(5) . . ? C15 O55 C55 114.4(5) . . ? O47 C16 O56 110.6(4) . . ? O47 C16 C26 108.9(5) . . ? O56 C16 C26 111.1(4) . . ? O26 C26 C36 111.2(5) . . ? O26 C26 C16 108.3(4) . . ? C36 C26 C16 109.3(4) . . ? O36 C36 C26 113.0(4) . . ? O36 C36 C46 110.5(4) . . ? C26 C36 C46 109.4(5) . . ? O46 C46 C56 110.5(4) . . ? O46 C46 C36 106.1(5) . . ? C56 C46 C36 110.6(4) . . ? O56 C56 C46 110.1(5) . . ? O56 C56 C66 106.3(5) . . ? C46 C56 C66 113.4(5) . . ? O66 C66 C56 112.3(6) . . ? C15 O46 C46 117.7(4) . . ? C16 O56 C56 114.1(5) . . ? O57 C17 O41 111.6(5) . . ? O57 C17 C27 111.6(5) . . ? O41 C17 C27 108.1(6) . . ? O27 C27 C37 111.7(6) . . ? O27 C27 C17 109.4(5) . . ? C37 C27 C17 110.9(5) . . ? O37 C37 C47 112.5(5) . . ? O37 C37 C27 108.4(5) . . ? C47 C37 C27 109.4(6) . . ? O47 C47 C57 111.1(4) . . ? O47 C47 C37 106.0(6) . . ? C57 C47 C37 109.7(5) . . ? O57 C57 C67 106.0(6) . . ? O57 C57 C47 108.8(4) . . ? C67 C57 C47 117.5(5) . . ? N67 C67 C57 112.9(5) . . ? C16 O47 C47 118.3(5) . . ? C17 O57 C57 113.0(5) . . ? C67 N67 C1 111.9(5) . . ? N67 C1 C2 111.7(6) . . ? N67 C1 C1P 112.4(6) . . ? C2 C1 C1P 113.0(6) . . ? C2P C1P C6P 116.4(8) . . ? C2P C1P C1 120.1(7) . . ? C6P C1P C1 123.3(7) . . ? C1P C2P C3P 121.8(9) . . ? C4P C3P C2P 120.2(10) . . ? C3P C4P C5P 120.4(10) . . ? C6P C5P C4P 118.8(12) . . ? C5P C6P C1P 121.8(11) . . ? _diffrn_measured_fraction_theta_max 0.758 _diffrn_reflns_theta_full 74.21 _diffrn_measured_fraction_theta_full 0.758 _refine_diff_density_max 0.630 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.084 data_indbcd _audit_creation_method SHELXL-97 _chemical_name_systematic ; 6-deoxy-6-[(1R,2S)-1-(2-hydroxy)indamyl]aminocyclomaltoheptaose ; _chemical_name_common ; 6-deoxy-6-[(1R,2S)-1-(2-hydroxy)indanyl]amino-beta-cyclodextrin ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H108 N O50' _chemical_formula_weight 1535.4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.519(1) _cell_length_b 10.124(2) _cell_length_c 23.519(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.67(1) _cell_angle_gamma 90.00 _cell_volume 3605 _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1569 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5644 _exptl_absorpt_correction_T_max 0.7383 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7674 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 74.25 _reflns_number_total 7499 _reflns_number_gt 7146 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1554P)^2^+0.5985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(18) _refine_ls_number_reflns 7499 _refine_ls_number_parameters 1005 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1875 _refine_ls_wR_factor_gt 0.1824 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.610 _refine_ls_shift/su_mean 0.025 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.0062(3) 0.0717(5) 0.2774(2) 0.0513(9) Uani 1 1 d . A . H11 H -0.0570 0.0620 0.2604 0.062 Uiso 1 1 calc R . . C21 C 0.0188(3) 0.0930(6) 0.3427(2) 0.0549(10) Uani 1 1 d . . . H21 H -0.0097 0.0203 0.3591 0.066 Uiso 1 1 calc R . . C31 C 0.1176(3) 0.0938(5) 0.37154(16) 0.0506(9) Uani 1 1 d . . . H31 H 0.1448 0.1728 0.3590 0.061 Uiso 1 1 calc R . . C41 C 0.1633(3) -0.0272(5) 0.35471(17) 0.0496(9) Uani 1 1 d . . . H41 H 0.1434 -0.1065 0.3720 0.060 Uiso 1 1 calc R . . C51 C 0.1449(3) -0.0399(5) 0.28886(19) 0.0546(10) Uani 1 1 d D A . H51 H 0.1693 0.0369 0.2724 0.066 Uiso 1 1 calc R . . C61 C 0.1814(5) -0.1656(8) 0.2677(3) 0.0794(17) Uani 1 1 d D . . O21 O -0.0219(2) 0.2142(5) 0.35328(15) 0.0662(9) Uani 1 1 d . . . H21A H -0.0340 0.2116 0.3855 0.099 Uiso 1 1 calc R . . O31 O 0.1240(2) 0.1006(6) 0.43259(14) 0.0757(12) Uani 1 1 d . . . H31A H 0.1761 0.1034 0.4495 0.114 Uiso 1 1 calc R . . O41 O 0.25664(17) -0.0085(3) 0.37598(11) 0.0448(6) Uani 1 1 d . . . O51 O 0.0503(2) -0.0446(4) 0.26675(15) 0.0603(8) Uani 1 1 d . . . O6A1 O 0.1938(4) -0.1440(8) 0.2086(2) 0.0773(16) Uani 0.72 1 d PD A 1 O6B1 O 0.1372(12) -0.2750(16) 0.2943(10) 0.163(16) Uani 0.28 1 d PD A 2 C12 C -0.0377(3) 0.4459(5) 0.1171(2) 0.0527(10) Uani 1 1 d . . . H12 H -0.0734 0.5011 0.0865 0.063 Uiso 1 1 calc R . . C22 C -0.0518(3) 0.4897(5) 0.1757(2) 0.0573(10) Uani 1 1 d . . . H22 H -0.1146 0.4816 0.1761 0.069 Uiso 1 1 calc R . . C32 C 0.0022(3) 0.4020(5) 0.22355(19) 0.0487(9) Uani 1 1 d . . . H32 H 0.0653 0.4145 0.2252 0.058 Uiso 1 1 calc R . . C42 C -0.0225(2) 0.2574(4) 0.20994(17) 0.0444(8) Uani 1 1 d . A . H42 H -0.0831 0.2413 0.2140 0.053 Uiso 1 1 calc R . . C52 C -0.0135(3) 0.2209(5) 0.14906(17) 0.0478(8) Uani 1 1 d . . . H52 H 0.0490 0.2243 0.1472 0.057 Uiso 1 1 calc R . . C62 C -0.0497(3) 0.0859(5) 0.1306(2) 0.0564(10) Uani 1 1 d . . . H62A H -0.0462 0.0696 0.0906 0.068 Uiso 1 1 calc R . . H62B H -0.0148 0.0192 0.1550 0.068 Uiso 1 1 calc R . . O22 O -0.0252(3) 0.6249(4) 0.1858(2) 0.0721(10) Uani 1 1 d . . . H22A H -0.0643 0.6662 0.1965 0.108 Uiso 1 1 calc R . . O32 O -0.0167(3) 0.4353(4) 0.27849(15) 0.0630(8) Uani 1 1 d . . . H32A H -0.0399 0.5085 0.2764 0.094 Uiso 1 1 calc R . . O42 O 0.03834(18) 0.1808(3) 0.25220(13) 0.0509(7) Uani 1 1 d . . . O52 O -0.06310(19) 0.3127(4) 0.10705(13) 0.0537(7) Uani 1 1 d . . . O62 O -0.1385(2) 0.0778(4) 0.13584(19) 0.0687(9) Uani 1 1 d . . . H62 H -0.1599 0.0078 0.1218 0.103 Uiso 1 1 calc R . . C13 C 0.2271(2) 0.6052(4) 0.02338(16) 0.0456(8) Uani 1 1 d . . . H13 H 0.2529 0.6432 -0.0074 0.055 Uiso 1 1 calc R . . C23 C 0.1695(3) 0.7080(4) 0.04404(19) 0.0485(9) Uani 1 1 d . . . H23 H 0.1214 0.7315 0.0111 0.058 Uiso 1 1 calc R . . C33 C 0.1295(2) 0.6489(4) 0.09158(17) 0.0452(8) Uani 1 1 d . . . H33 H 0.1776 0.6239 0.1243 0.054 Uiso 1 1 calc R . . C43 C 0.0779(2) 0.5256(4) 0.06868(17) 0.0453(8) Uani 1 1 d . . . H43 H 0.0253 0.5498 0.0392 0.054 Uiso 1 1 calc R . . C53 C 0.1351(3) 0.4292(5) 0.04252(18) 0.0481(8) Uani 1 1 d . . . H53 H 0.1806 0.3918 0.0740 0.058 Uiso 1 1 calc R . . C63 C 0.0815(3) 0.3186(5) 0.0095(2) 0.0619(11) Uani 1 1 d . . . H63A H 0.0495 0.2740 0.0350 0.074 Uiso 1 1 calc R . . H63B H 0.0385 0.3553 -0.0229 0.074 Uiso 1 1 calc R . . O23 O 0.2185(2) 0.8241(3) 0.06350(17) 0.0587(8) Uani 1 1 d . . . H23A H 0.2714 0.8080 0.0691 0.088 Uiso 1 1 calc R . . O33 O 0.0752(2) 0.7427(4) 0.11154(16) 0.0588(8) Uani 1 1 d . . . H33A H 0.0373 0.7041 0.1246 0.088 Uiso 1 1 calc R . . O43 O 0.05237(17) 0.4632(4) 0.11710(12) 0.0500(7) Uani 1 1 d . . . O53 O 0.17686(19) 0.4945(3) 0.00181(12) 0.0503(7) Uani 1 1 d . . . O63 O 0.1342(4) 0.2254(5) -0.0120(2) 0.0931(14) Uani 1 1 d . . . H63 H 0.1658 0.1863 0.0154 0.140 Uiso 1 1 calc R . . C14 C 0.5721(2) 0.5564(4) 0.11320(17) 0.0444(8) Uani 1 1 d . . . H14 H 0.6312 0.5737 0.1065 0.053 Uiso 1 1 calc R . . C24 C 0.5271(3) 0.6887(4) 0.11820(19) 0.0475(8) Uani 1 1 d . . . H24 H 0.5289 0.7409 0.0834 0.057 Uiso 1 1 calc R . . C34 C 0.4316(2) 0.6682(4) 0.12048(16) 0.0414(7) Uani 1 1 d . . . H34 H 0.4287 0.6194 0.1560 0.050 Uiso 1 1 calc R . . C44 C 0.3851(2) 0.5890(4) 0.06778(15) 0.0385(7) Uani 1 1 d . . . H44 H 0.3867 0.6377 0.0320 0.046 Uiso 1 1 calc R . . C54 C 0.4336(3) 0.4578(4) 0.06814(18) 0.0449(8) Uani 1 1 d . . . H54 H 0.4325 0.4107 0.1044 0.054 Uiso 1 1 calc R . . C64 C 0.3949(4) 0.3701(5) 0.0170(2) 0.0622(11) Uani 1 1 d . . . H64A H 0.4326 0.2935 0.0175 0.075 Uiso 1 1 calc R . . H64B H 0.3373 0.3392 0.0209 0.075 Uiso 1 1 calc R . . O24 O 0.5741(2) 0.7591(3) 0.16796(18) 0.0659(9) Uani 1 1 d . . . H24A H 0.5457 0.7576 0.1936 0.099 Uiso 1 1 calc R . . O34 O 0.3896(2) 0.7935(3) 0.12157(13) 0.0500(6) Uani 1 1 d . . . H34A H 0.3927 0.8160 0.1555 0.075 Uiso 1 1 calc R . . O44 O 0.29604(16) 0.5690(3) 0.07166(11) 0.0437(6) Uani 1 1 d . . . O54 O 0.52417(18) 0.4837(3) 0.06563(12) 0.0497(7) Uani 1 1 d . . . O64 O 0.3860(3) 0.4369(5) -0.03739(15) 0.0715(10) Uani 1 1 d . . . H64 H 0.4351 0.4564 -0.0424 0.107 Uiso 1 1 calc R . . C15 C 0.7690(2) 0.2833(4) 0.28586(16) 0.0406(7) Uani 1 1 d . . . H15 H 0.8259 0.2468 0.3062 0.049 Uiso 1 1 calc R . . C25 C 0.7730(2) 0.4341(4) 0.28904(17) 0.0426(8) Uani 1 1 d . . . H25 H 0.8213 0.4643 0.2716 0.051 Uiso 1 1 calc R . . C35 C 0.6875(2) 0.4922(4) 0.25477(16) 0.0407(7) Uani 1 1 d . . . H35 H 0.6398 0.4667 0.2738 0.049 Uiso 1 1 calc R . . C45 C 0.6665(2) 0.4379(4) 0.19286(16) 0.0396(7) Uani 1 1 d . . . H45 H 0.7099 0.4707 0.1717 0.047 Uiso 1 1 calc R . . C55 C 0.6672(2) 0.2868(4) 0.19318(17) 0.0424(8) Uani 1 1 d . . . H55 H 0.6189 0.2539 0.2100 0.051 Uiso 1 1 calc R . . C65 C 0.6605(3) 0.2274(5) 0.13364(18) 0.0576(11) Uani 1 1 d . . . H65A H 0.6625 0.1319 0.1372 0.069 Uiso 1 1 calc R . . H65B H 0.6037 0.2508 0.1091 0.069 Uiso 1 1 calc R . . O25 O 0.7911(2) 0.4746(3) 0.34844(13) 0.0526(7) Uani 1 1 d . . . H25A H 0.7576 0.4362 0.3655 0.079 Uiso 1 1 calc R . . O35 O 0.6933(2) 0.6325(3) 0.25483(16) 0.0574(8) Uani 1 1 d . . . H35A H 0.7283 0.6555 0.2352 0.086 Uiso 1 1 calc R . . O45 O 0.58107(16) 0.4857(3) 0.16589(11) 0.0417(5) Uani 1 1 d . . . O55 O 0.75040(18) 0.2408(3) 0.22735(11) 0.0441(6) Uani 1 1 d . . . O65 O 0.7269(3) 0.2683(5) 0.10654(16) 0.0706(10) Uani 1 1 d . . . H65 H 0.7711 0.2228 0.1179 0.106 Uiso 1 1 calc R . . C16 C 0.6437(2) -0.0276(4) 0.42902(16) 0.0419(7) Uani 1 1 d . . . H16 H 0.6458 -0.0979 0.4579 0.050 Uiso 1 1 calc R . . C26 C 0.7005(2) 0.0886(4) 0.45685(15) 0.0431(7) Uani 1 1 d . . . H26 H 0.7615 0.0588 0.4711 0.052 Uiso 1 1 calc R . . C36 C 0.6984(2) 0.1971(4) 0.41230(16) 0.0410(7) Uani 1 1 d . . . H36 H 0.6382 0.2322 0.4013 0.049 Uiso 1 1 calc R . . C46 C 0.7242(2) 0.1418(4) 0.35811(15) 0.0390(7) Uani 1 1 d . . . H46 H 0.7877 0.1233 0.3664 0.047 Uiso 1 1 calc R . . C56 C 0.6726(2) 0.0184(4) 0.33486(16) 0.0408(7) Uani 1 1 d . . . H56 H 0.6109 0.0424 0.3189 0.049 Uiso 1 1 calc R . . C66 C 0.7094(3) -0.0501(4) 0.2881(2) 0.0550(10) Uani 1 1 d . . . H66A H 0.6796 -0.1341 0.2789 0.066 Uiso 1 1 calc R . . H66B H 0.6970 0.0035 0.2530 0.066 Uiso 1 1 calc R . . O26 O 0.6671(2) 0.1380(4) 0.50408(13) 0.0576(8) Uani 1 1 d . . . H26A H 0.6141 0.1532 0.4931 0.086 Uiso 1 1 calc R . . O36 O 0.7567(2) 0.3015(3) 0.43668(14) 0.0571(7) Uani 1 1 d . . . H36A H 0.7677 0.3473 0.4104 0.086 Uiso 1 1 calc R . . O46 O 0.70305(16) 0.2430(3) 0.31462(11) 0.0408(5) Uani 1 1 d . . . O56 O 0.6763(2) -0.0763(3) 0.38140(13) 0.0465(6) Uani 1 1 d . . . O66 O 0.8017(3) -0.0725(4) 0.30484(19) 0.0719(10) Uani 1 1 d . . . H66 H 0.8202 -0.0963 0.2764 0.108 Uiso 1 1 calc R . . C17 C 0.3003(2) -0.0898(4) 0.42251(15) 0.0412(7) Uani 1 1 d . . . H17 H 0.2557 -0.1379 0.4380 0.049 Uiso 1 1 calc R . . C27 C 0.3546(3) -0.0046(4) 0.47128(15) 0.0452(8) Uani 1 1 d . . . H27 H 0.3751 -0.0602 0.5057 0.054 Uiso 1 1 calc R . . C37 C 0.4342(2) 0.0560(4) 0.45385(15) 0.0420(7) Uani 1 1 d . . . H37 H 0.4140 0.1217 0.4232 0.050 Uiso 1 1 calc R . . C47 C 0.4873(2) -0.0500(4) 0.43077(15) 0.0383(7) Uani 1 1 d . . . H47 H 0.5133 -0.1108 0.4623 0.046 Uiso 1 1 calc R . . C57 C 0.4273(2) -0.1263(4) 0.38139(15) 0.0392(7) Uani 1 1 d . . . H57 H 0.4039 -0.0666 0.3489 0.047 Uiso 1 1 calc R . . C67 C 0.4756(2) -0.2413(4) 0.36028(17) 0.0419(7) Uani 1 1 d . . . H67A H 0.5187 -0.2078 0.3396 0.050 Uiso 1 1 calc R . . H67B H 0.5067 -0.2923 0.3934 0.050 Uiso 1 1 calc R . . O27 O 0.2988(2) 0.0960(4) 0.48557(13) 0.0560(7) Uani 1 1 d . . . H27A H 0.2599 0.0622 0.4993 0.084 Uiso 1 1 calc R . . O37 O 0.4868(2) 0.1203(4) 0.50369(13) 0.0529(7) Uani 1 1 d . . . H37A H 0.5342 0.1423 0.4966 0.079 Uiso 1 1 calc R . . O47 O 0.55591(17) 0.0165(3) 0.41000(11) 0.0415(5) Uani 1 1 d . . . O57 O 0.35577(17) -0.1822(3) 0.40350(12) 0.0439(6) Uani 1 1 d . . . N67 N 0.4114(2) -0.3261(3) 0.32133(14) 0.0427(6) Uani 1 1 d D . . H67 H 0.368(3) -0.342(6) 0.341(2) 0.051 Uiso 1 1 d D . . C77 C 0.4491(2) -0.4488(4) 0.30507(16) 0.0406(7) Uani 1 1 d . . . H77 H 0.4911 -0.4269 0.2809 0.049 Uiso 1 1 calc R . . C87 C 0.4956(3) -0.5412(4) 0.35481(19) 0.0486(9) Uani 1 1 d . . . H87 H 0.5576 -0.5163 0.3692 0.058 Uiso 1 1 calc R . . C97 C 0.4875(3) -0.6783(4) 0.3272(2) 0.0535(10) Uani 1 1 d . . . H97A H 0.5357 -0.6957 0.3081 0.064 Uiso 1 1 calc R . . H97B H 0.4862 -0.7465 0.3559 0.064 Uiso 1 1 calc R . . CA7 C 0.4003(3) -0.6694(4) 0.28357(19) 0.0481(9) Uani 1 1 d . . . CB7 C 0.3438(4) -0.7711(5) 0.2591(3) 0.0677(13) Uani 1 1 d . . . HB7 H 0.3584 -0.8590 0.2676 0.081 Uiso 1 1 calc R . . CC7 C 0.2653(4) -0.7370(6) 0.2217(3) 0.0701(14) Uani 1 1 d . . . HC7 H 0.2258 -0.8032 0.2056 0.084 Uiso 1 1 calc R . . CD7 C 0.2442(3) -0.6079(6) 0.2076(2) 0.0619(12) Uani 1 1 d . . . HD7 H 0.1916 -0.5879 0.1815 0.074 Uiso 1 1 calc R . . CE7 C 0.3008(3) -0.5065(5) 0.23202(18) 0.0516(9) Uani 1 1 d . . . HE7 H 0.2863 -0.4188 0.2227 0.062 Uiso 1 1 calc R . . CF7 C 0.3790(2) -0.5384(4) 0.27050(16) 0.0419(7) Uani 1 1 d . . . OG7 O 0.4487(3) -0.5437(4) 0.40098(15) 0.0651(8) Uani 1 1 d . . . O1AW O 0.1815(17) 1.0883(17) 0.0911(7) 0.175(8) Uani 0.59 1 d PU . . O1BW O 0.176(3) 0.975(6) 0.153(3) 0.33(3) Uani 0.41 1 d PU . . O2AW O 0.3890(18) 1.1726(14) 0.1307(8) 0.212(10) Uani 0.65 1 d PU . . O2BW O 0.256(3) 1.116(3) 0.0846(17) 0.194(17) Uani 0.35 1 d PU . . O3W O 0.3715(3) 0.8591(5) 0.22908(17) 0.0756(10) Uani 1 1 d U . . O4AW O 0.8864(11) -0.168(2) 0.4103(7) 0.167(7) Uani 0.61 1 d PU . . O4BW O 0.884(2) -0.290(3) 0.3747(10) 0.164(11) Uani 0.39 1 d PU . . O5AW O 1.0926(18) -0.180(7) 0.4822(16) 0.26(3) Uani 0.35 1 d PU . . O5BW O 1.006(3) 0.001(4) 0.4916(15) 0.276(14) Uani 0.65 1 d PU . . O6W O 0.7190(5) 0.4699(8) 0.0281(3) 0.1138(19) Uani 1 1 d U . . O7W O 0.9359(6) 0.2347(18) 0.4598(4) 0.122(5) Uani 0.58 1 d PU . . O8W O 0.2924(7) -0.6543(11) 0.4133(7) 0.172(5) Uani 0.89 1 d PU . . O9AW O 0.0237(12) 0.6828(17) 0.3293(7) 0.162(6) Uani 0.62 1 d PU . . O9BW O -0.0478(16) 0.591(3) 0.3862(14) 0.169(10) Uani 0.38 1 d PU . . O10W O 0.8001(8) 0.0777(16) 0.5979(5) 0.180(6) Uani 0.80 1 d PU . . O11W O -0.1681(3) 0.7513(5) 0.2166(2) 0.0813(11) Uani 1 1 d U . . O12W O 0.3121(3) 0.1448(4) 0.60003(16) 0.0668(9) Uani 1 1 d U . . O13W O 0.5145(5) 1.0105(9) 0.2061(4) 0.130(3) Uani 0.86 1 d PU . . O14W O 0.4485(4) 0.9994(7) 0.0575(2) 0.1012(16) Uani 1 1 d U . . O15W O -0.2241(4) -0.1634(7) 0.1008(2) 0.1010(16) Uani 1 1 d U . . O16W O 0.126(2) 0.376(3) 0.4690(13) 0.236(14) Uani 0.53 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0396(17) 0.057(2) 0.054(2) 0.0008(19) 0.0025(15) -0.0018(17) C21 0.0450(19) 0.063(3) 0.054(2) 0.004(2) 0.0060(16) 0.0079(19) C31 0.0470(19) 0.064(2) 0.0384(17) -0.0026(17) 0.0038(14) 0.0068(19) C41 0.0449(18) 0.056(2) 0.0451(18) 0.0039(17) 0.0029(14) 0.0019(18) C51 0.054(2) 0.056(2) 0.049(2) -0.0066(18) 0.0007(17) 0.0055(19) C61 0.084(4) 0.077(4) 0.070(3) -0.022(3) 0.000(3) 0.022(3) O21 0.0513(16) 0.088(3) 0.0586(17) -0.0026(18) 0.0101(13) 0.0214(18) O31 0.0635(19) 0.118(4) 0.0426(15) -0.0110(19) 0.0051(13) 0.025(2) O41 0.0421(12) 0.0473(14) 0.0420(12) 0.0078(11) 0.0032(10) 0.0057(11) O51 0.0577(17) 0.0527(18) 0.0592(17) -0.0066(14) -0.0114(13) 0.0009(15) O6A1 0.077(3) 0.100(4) 0.051(2) -0.019(3) 0.007(2) 0.015(3) O6B1 0.103(15) 0.19(3) 0.15(2) -0.07(2) -0.074(15) 0.07(2) C12 0.0356(17) 0.058(2) 0.061(2) 0.012(2) 0.0034(15) 0.0052(17) C22 0.0415(18) 0.058(3) 0.074(3) 0.009(2) 0.0161(18) 0.0096(19) C32 0.0391(17) 0.054(2) 0.053(2) -0.0003(18) 0.0095(15) 0.0044(16) C42 0.0310(15) 0.054(2) 0.0459(18) 0.0001(16) 0.0030(13) 0.0036(15) C52 0.0426(18) 0.054(2) 0.0434(18) 0.0022(17) 0.0022(14) 0.0046(17) C62 0.061(2) 0.054(2) 0.050(2) -0.0033(19) 0.0044(18) 0.002(2) O22 0.080(2) 0.0511(19) 0.094(3) -0.0009(18) 0.038(2) 0.0137(17) O32 0.073(2) 0.059(2) 0.0599(18) -0.0092(15) 0.0206(15) 0.0027(17) O42 0.0376(12) 0.0600(18) 0.0491(14) 0.0061(13) -0.0033(10) 0.0023(13) O52 0.0421(13) 0.0612(19) 0.0513(15) 0.0108(14) -0.0038(11) -0.0020(13) O62 0.0609(18) 0.0559(19) 0.086(2) -0.0044(18) 0.0085(17) -0.0127(16) C13 0.0386(16) 0.053(2) 0.0412(17) 0.0052(16) 0.0002(13) -0.0032(16) C23 0.0435(18) 0.042(2) 0.056(2) 0.0074(17) 0.0018(16) 0.0025(16) C33 0.0385(16) 0.0443(19) 0.0501(19) -0.0022(16) 0.0037(14) 0.0059(15) C43 0.0375(16) 0.051(2) 0.0447(17) 0.0029(16) 0.0026(13) -0.0018(16) C53 0.0446(18) 0.048(2) 0.0481(19) -0.0046(16) 0.0022(15) -0.0051(17) C63 0.064(3) 0.054(3) 0.063(3) -0.013(2) 0.004(2) -0.014(2) O23 0.0493(15) 0.0409(15) 0.082(2) 0.0055(15) 0.0062(15) 0.0017(13) O33 0.0510(15) 0.0507(17) 0.075(2) -0.0055(15) 0.0137(14) 0.0066(14) O43 0.0349(12) 0.0619(18) 0.0506(14) 0.0097(13) 0.0036(10) 0.0034(12) O53 0.0499(14) 0.0563(17) 0.0426(13) -0.0046(12) 0.0059(11) -0.0052(13) O63 0.105(3) 0.060(2) 0.106(3) -0.028(2) 0.004(3) 0.002(2) C14 0.0393(16) 0.048(2) 0.0454(18) 0.0055(16) 0.0078(14) 0.0008(15) C24 0.0417(18) 0.0403(18) 0.056(2) 0.0047(16) 0.0007(15) -0.0064(16) C34 0.0416(17) 0.0360(18) 0.0436(17) -0.0025(14) 0.0029(13) 0.0039(14) C44 0.0369(15) 0.0377(17) 0.0408(15) -0.0008(14) 0.0084(12) 0.0017(14) C54 0.0433(18) 0.0413(19) 0.0489(18) -0.0012(16) 0.0072(14) 0.0053(15) C64 0.073(3) 0.051(2) 0.057(2) -0.012(2) 0.001(2) 0.007(2) O24 0.0545(17) 0.0425(16) 0.086(2) -0.0083(16) -0.0150(15) -0.0003(14) O34 0.0523(15) 0.0416(14) 0.0523(15) -0.0057(12) 0.0031(12) 0.0110(12) O44 0.0377(12) 0.0496(14) 0.0417(12) 0.0064(11) 0.0044(9) -0.0005(11) O54 0.0433(13) 0.0612(18) 0.0436(13) -0.0044(13) 0.0072(10) 0.0100(13) O64 0.082(2) 0.077(2) 0.0489(16) -0.0099(16) 0.0006(15) 0.014(2) C15 0.0371(16) 0.0387(17) 0.0453(18) -0.0003(14) 0.0073(13) 0.0047(14) C25 0.0422(17) 0.0369(17) 0.0470(18) -0.0015(14) 0.0061(14) -0.0008(14) C35 0.0412(17) 0.0317(16) 0.0483(18) -0.0014(14) 0.0078(14) 0.0022(14) C45 0.0357(15) 0.0362(17) 0.0461(18) -0.0012(14) 0.0073(13) 0.0033(13) C55 0.0425(18) 0.0353(17) 0.0478(19) -0.0024(14) 0.0067(14) 0.0047(14) C65 0.073(3) 0.048(2) 0.047(2) -0.0112(18) 0.0021(18) 0.010(2) O25 0.0595(17) 0.0440(15) 0.0486(14) -0.0034(12) -0.0006(12) -0.0031(13) O35 0.0682(19) 0.0313(13) 0.0663(19) -0.0026(12) 0.0007(14) -0.0025(13) O45 0.0344(11) 0.0427(13) 0.0466(12) 0.0064(11) 0.0060(9) 0.0035(10) O55 0.0466(13) 0.0417(13) 0.0432(12) -0.0019(11) 0.0085(10) 0.0132(11) O65 0.080(2) 0.079(3) 0.0543(17) 0.0022(17) 0.0191(16) 0.024(2) C16 0.0429(17) 0.0354(16) 0.0460(17) 0.0037(14) 0.0070(13) 0.0016(14) C26 0.0442(17) 0.0422(19) 0.0405(16) -0.0004(15) 0.0044(13) 0.0009(15) C36 0.0432(17) 0.0339(16) 0.0434(17) -0.0037(14) 0.0041(14) -0.0021(14) C46 0.0406(16) 0.0309(15) 0.0436(17) 0.0024(13) 0.0051(13) 0.0043(13) C56 0.0446(17) 0.0316(16) 0.0461(17) -0.0021(14) 0.0099(14) 0.0049(14) C66 0.072(3) 0.0375(19) 0.058(2) -0.0092(17) 0.019(2) 0.0004(19) O26 0.0696(19) 0.0612(19) 0.0412(13) -0.0079(13) 0.0103(13) -0.0061(16) O36 0.0703(19) 0.0466(17) 0.0528(15) -0.0117(13) 0.0101(14) -0.0183(15) O46 0.0386(11) 0.0353(12) 0.0471(13) 0.0043(11) 0.0064(10) 0.0060(10) O56 0.0567(15) 0.0308(12) 0.0529(14) 0.0018(11) 0.0140(12) 0.0043(11) O66 0.071(2) 0.060(2) 0.091(3) -0.013(2) 0.0312(19) 0.0113(18) C17 0.0429(17) 0.0421(18) 0.0372(16) 0.0070(14) 0.0056(13) 0.0039(15) C27 0.0462(18) 0.051(2) 0.0370(16) 0.0019(15) 0.0052(13) 0.0057(17) C37 0.0484(18) 0.0399(18) 0.0352(15) -0.0023(14) 0.0036(13) 0.0025(15) C47 0.0426(16) 0.0339(16) 0.0360(15) 0.0010(13) 0.0038(12) 0.0000(14) C57 0.0442(17) 0.0331(15) 0.0382(16) -0.0008(13) 0.0046(13) -0.0008(14) C67 0.0439(17) 0.0327(17) 0.0474(18) -0.0041(14) 0.0063(14) -0.0004(14) O27 0.0577(17) 0.0639(19) 0.0463(14) -0.0037(14) 0.0112(12) 0.0126(15) O37 0.0573(17) 0.0567(17) 0.0435(13) -0.0147(13) 0.0085(12) -0.0047(14) O47 0.0439(12) 0.0342(12) 0.0446(12) 0.0027(10) 0.0059(10) 0.0003(10) O57 0.0440(13) 0.0375(13) 0.0496(13) 0.0020(11) 0.0092(10) -0.0004(11) N67 0.0437(15) 0.0352(15) 0.0472(16) -0.0054(13) 0.0056(12) 0.0000(13) C77 0.0376(16) 0.0375(18) 0.0449(17) -0.0007(14) 0.0051(13) -0.0003(14) C87 0.0436(18) 0.0399(19) 0.056(2) 0.0016(17) -0.0029(15) 0.0002(16) C97 0.0458(19) 0.0356(18) 0.072(3) 0.0006(18) -0.0031(18) 0.0031(16) CA7 0.049(2) 0.0353(18) 0.056(2) -0.0005(16) 0.0033(17) 0.0012(16) CB7 0.073(3) 0.039(2) 0.081(3) -0.002(2) -0.004(2) -0.010(2) CC7 0.061(3) 0.062(3) 0.074(3) -0.004(2) -0.013(2) -0.017(2) CD7 0.051(2) 0.066(3) 0.058(2) 0.002(2) -0.0104(18) -0.004(2) CE7 0.049(2) 0.049(2) 0.0498(19) 0.0008(17) -0.0025(16) 0.0060(18) CF7 0.0438(17) 0.0373(18) 0.0415(16) -0.0018(14) 0.0026(14) 0.0009(15) OG7 0.079(2) 0.062(2) 0.0522(16) 0.0040(15) 0.0100(15) -0.0058(18) O1AW 0.28(2) 0.121(11) 0.121(9) 0.003(8) 0.042(12) 0.124(14) O1BW 0.29(4) 0.31(6) 0.43(7) -0.21(5) 0.16(5) 0.01(4) O2AW 0.41(3) 0.101(9) 0.176(13) 0.043(9) 0.184(17) 0.059(14) O2BW 0.29(4) 0.12(2) 0.21(3) 0.00(2) 0.14(3) 0.08(3) O3W 0.099(3) 0.067(2) 0.0609(19) 0.0036(18) 0.0158(18) 0.011(2) O4AW 0.137(10) 0.203(19) 0.143(11) 0.042(13) -0.005(8) 0.036(12) O4BW 0.20(2) 0.139(19) 0.120(14) 0.016(14) -0.032(14) -0.076(19) O5AW 0.102(14) 0.44(7) 0.20(3) 0.06(4) -0.021(15) -0.01(3) O5BW 0.32(3) 0.27(3) 0.28(2) 0.11(3) 0.17(2) 0.01(3) O6W 0.140(5) 0.105(4) 0.107(4) 0.014(4) 0.048(4) 0.016(4) O7W 0.078(5) 0.202(14) 0.087(5) -0.003(8) 0.020(4) 0.025(7) O8W 0.136(7) 0.109(6) 0.286(15) -0.001(9) 0.077(8) -0.016(6) O9AW 0.209(15) 0.128(11) 0.147(10) -0.050(9) 0.034(10) -0.060(11) O9BW 0.124(14) 0.14(2) 0.22(3) -0.06(2) -0.003(15) -0.037(16) O10W 0.180(10) 0.159(10) 0.150(8) 0.008(8) -0.075(7) 0.017(9) O11W 0.098(3) 0.064(2) 0.087(3) -0.006(2) 0.030(2) 0.008(2) O12W 0.092(3) 0.0486(17) 0.0635(19) -0.0079(15) 0.0240(18) -0.0107(17) O13W 0.094(4) 0.086(4) 0.185(8) -0.022(5) -0.027(4) -0.001(4) O14W 0.124(4) 0.098(4) 0.082(3) 0.012(3) 0.025(3) 0.013(3) O15W 0.104(3) 0.104(4) 0.084(3) 0.012(3) -0.004(2) -0.012(3) O16W 0.35(4) 0.148(18) 0.23(2) -0.057(18) 0.10(2) -0.12(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 O42 1.397(6) . ? C11 O51 1.412(6) . ? C11 C21 1.520(6) . ? C21 O21 1.426(7) . ? C21 C31 1.536(6) . ? C31 O31 1.419(5) . ? C31 C41 1.510(7) . ? C41 O41 1.438(5) . ? C41 C51 1.518(6) . ? C51 O51 1.448(5) . ? C51 C61 1.520(7) . ? C61 O6A1 1.461(8) . ? C61 O6B1 1.508(17) . ? O41 C17 1.417(4) . ? C12 O52 1.410(6) . ? C12 O43 1.408(5) . ? C12 C22 1.509(7) . ? C22 O22 1.434(7) . ? C22 C32 1.531(6) . ? C32 O32 1.427(5) . ? C32 C42 1.529(6) . ? C42 O42 1.439(5) . ? C42 C52 1.515(6) . ? C52 O52 1.449(5) . ? C52 C62 1.504(7) . ? C62 O62 1.412(6) . ? C13 O53 1.395(5) . ? C13 O44 1.427(4) . ? C13 C23 1.518(6) . ? C23 O23 1.420(5) . ? C23 C33 1.516(6) . ? C33 O33 1.416(5) . ? C33 C43 1.516(6) . ? C43 O43 1.433(5) . ? C43 C53 1.535(6) . ? C53 O53 1.430(5) . ? C53 C63 1.506(6) . ? C63 O63 1.413(7) . ? C14 O54 1.408(5) . ? C14 O45 1.411(5) . ? C14 C24 1.527(6) . ? C24 O24 1.427(5) . ? C24 C34 1.509(5) . ? C34 O34 1.429(5) . ? C34 C44 1.520(5) . ? C44 O44 1.419(4) . ? C44 C54 1.525(5) . ? C54 O54 1.444(5) . ? C54 C64 1.509(6) . ? C64 O64 1.428(7) . ? C15 O46 1.405(5) . ? C15 O55 1.410(5) . ? C15 C25 1.529(5) . ? C25 O25 1.424(5) . ? C25 C35 1.513(5) . ? C35 O35 1.423(5) . ? C35 C45 1.523(5) . ? C45 O45 1.423(4) . ? C45 C55 1.529(5) . ? C55 O55 1.441(4) . ? C55 C65 1.507(5) . ? C65 O65 1.390(7) . ? C16 O47 1.410(4) . ? C16 O56 1.415(5) . ? C16 C26 1.529(5) . ? C26 O26 1.417(5) . ? C26 C36 1.513(5) . ? C36 O36 1.427(5) . ? C36 C46 1.523(5) . ? C46 O46 1.434(4) . ? C46 C56 1.519(5) . ? C56 O56 1.447(5) . ? C56 C66 1.515(5) . ? C66 O66 1.418(6) . ? C17 O57 1.409(5) . ? C17 C27 1.532(5) . ? C27 O27 1.424(5) . ? C27 C37 1.514(6) . ? C37 O37 1.430(4) . ? C37 C47 1.524(5) . ? C47 O47 1.433(4) . ? C47 C57 1.529(5) . ? C57 O57 1.441(5) . ? C57 C67 1.526(5) . ? C67 N67 1.472(5) . ? N67 C77 1.459(5) . ? C77 CF7 1.510(5) . ? C77 C87 1.547(5) . ? C87 OG7 1.433(6) . ? C87 C97 1.525(6) . ? C97 CA7 1.510(6) . ? CA7 CF7 1.385(6) . ? CA7 CB7 1.393(6) . ? CB7 CC7 1.381(8) . ? CC7 CD7 1.370(9) . ? CD7 CE7 1.390(7) . ? CE7 CF7 1.384(5) . ? O1AW O1BW 1.88(8) . ? O1AW O2BW 1.23(4) . ? O4AW O4BW 1.49(3) . ? O4BW O9BW 1.59(4) 1_645 ? O9BW O4BW 1.59(4) 1_465 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O42 C11 O51 110.6(3) . . ? O42 C11 C21 109.8(4) . . ? O51 C11 C21 109.8(4) . . ? O21 C21 C11 109.6(4) . . ? O21 C21 C31 110.9(4) . . ? C11 C21 C31 109.9(3) . . ? O31 C31 C41 111.8(4) . . ? O31 C31 C21 106.7(3) . . ? C41 C31 C21 111.1(4) . . ? O41 C41 C31 107.3(4) . . ? O41 C41 C51 108.4(3) . . ? C31 C41 C51 110.1(4) . . ? O51 C51 C61 106.0(4) . . ? O51 C51 C41 108.5(4) . . ? C61 C51 C41 113.9(4) . . ? O6A1 C61 O6B1 132.2(11) . . ? O6A1 C61 C51 108.7(6) . . ? O6B1 C61 C51 104.1(9) . . ? C17 O41 C41 117.8(3) . . ? C11 O51 C51 113.7(3) . . ? O52 C12 O43 111.1(4) . . ? O52 C12 C22 110.0(4) . . ? O43 C12 C22 107.8(4) . . ? O22 C22 C12 109.8(4) . . ? O22 C22 C32 109.9(4) . . ? C12 C22 C32 109.6(4) . . ? O32 C32 C42 108.9(4) . . ? O32 C32 C22 109.9(4) . . ? C42 C32 C22 109.3(4) . . ? O42 C42 C52 109.8(3) . . ? O42 C42 C32 106.0(3) . . ? C52 C42 C32 111.1(4) . . ? O52 C52 C62 106.1(3) . . ? O52 C52 C42 110.0(3) . . ? C62 C52 C42 112.8(4) . . ? O62 C62 C52 109.8(4) . . ? C11 O42 C42 118.6(3) . . ? C12 O52 C52 114.4(3) . . ? O53 C13 O44 110.1(3) . . ? O53 C13 C23 110.3(3) . . ? O44 C13 C23 108.2(3) . . ? O23 C23 C13 111.1(3) . . ? O23 C23 C33 111.4(4) . . ? C13 C23 C33 109.3(3) . . ? O33 C33 C43 111.3(3) . . ? O33 C33 C23 110.5(4) . . ? C43 C33 C23 109.4(3) . . ? O43 C43 C33 107.3(3) . . ? O43 C43 C53 108.8(3) . . ? C33 C43 C53 111.0(3) . . ? O53 C53 C63 106.2(4) . . ? O53 C53 C43 111.2(4) . . ? C63 C53 C43 112.2(4) . . ? O63 C63 C53 112.6(4) . . ? C12 O43 C43 120.2(3) . . ? C13 O53 C53 115.2(3) . . ? O54 C14 O45 111.5(3) . . ? O54 C14 C24 110.4(3) . . ? O45 C14 C24 109.6(3) . . ? O24 C24 C34 111.6(4) . . ? O24 C24 C14 109.9(3) . . ? C34 C24 C14 110.6(3) . . ? O34 C34 C24 109.5(3) . . ? O34 C34 C44 110.3(3) . . ? C24 C34 C44 109.7(3) . . ? O44 C44 C34 108.5(3) . . ? O44 C44 C54 111.2(3) . . ? C34 C44 C54 108.0(3) . . ? O54 C54 C64 107.1(4) . . ? O54 C54 C44 109.0(3) . . ? C64 C54 C44 113.5(3) . . ? O64 C64 C54 112.2(4) . . ? C44 O44 C13 118.9(3) . . ? C14 O54 C54 114.3(3) . . ? O46 C15 O55 111.5(3) . . ? O46 C15 C25 107.0(3) . . ? O55 C15 C25 110.5(3) . . ? O25 C25 C35 111.8(3) . . ? O25 C25 C15 109.4(3) . . ? C35 C25 C15 109.9(3) . . ? O35 C35 C25 109.8(3) . . ? O35 C35 C45 111.2(3) . . ? C25 C35 C45 110.3(3) . . ? O45 C45 C35 106.6(3) . . ? O45 C45 C55 110.3(3) . . ? C35 C45 C55 110.9(3) . . ? O55 C55 C65 105.1(3) . . ? O55 C55 C45 109.3(3) . . ? C65 C55 C45 113.3(4) . . ? O65 C65 C55 113.6(4) . . ? C14 O45 C45 117.9(3) . . ? C15 O55 C55 114.3(3) . . ? O47 C16 O56 110.3(3) . . ? O47 C16 C26 108.6(3) . . ? O56 C16 C26 109.5(3) . . ? O26 C26 C36 109.3(3) . . ? O26 C26 C16 109.4(3) . . ? C36 C26 C16 109.8(3) . . ? O36 C36 C26 110.1(3) . . ? O36 C36 C46 110.4(3) . . ? C26 C36 C46 110.1(3) . . ? O46 C46 C56 108.1(3) . . ? O46 C46 C36 105.9(3) . . ? C56 C46 C36 112.9(3) . . ? O56 C56 C66 106.7(3) . . ? O56 C56 C46 110.0(3) . . ? C66 C56 C46 112.7(3) . . ? O66 C66 C56 112.9(4) . . ? C15 O46 C46 118.3(3) . . ? C16 O56 C56 114.0(3) . . ? O57 C17 O41 111.2(3) . . ? O57 C17 C27 109.7(3) . . ? O41 C17 C27 110.0(3) . . ? O27 C27 C37 110.4(4) . . ? O27 C27 C17 108.4(3) . . ? C37 C27 C17 111.9(3) . . ? O37 C37 C27 108.4(3) . . ? O37 C37 C47 110.8(3) . . ? C27 C37 C47 110.4(3) . . ? O47 C47 C37 106.9(3) . . ? O47 C47 C57 110.6(3) . . ? C37 C47 C57 109.8(3) . . ? O57 C57 C67 106.8(3) . . ? O57 C57 C47 108.3(3) . . ? C67 C57 C47 111.8(3) . . ? N67 C67 C57 109.5(3) . . ? C16 O47 C47 118.8(3) . . ? C17 O57 C57 115.2(3) . . ? C77 N67 C67 113.8(3) . . ? N67 C77 CF7 111.7(3) . . ? N67 C77 C87 117.7(3) . . ? CF7 C77 C87 101.8(3) . . ? OG7 C87 C97 107.4(4) . . ? OG7 C87 C77 110.7(3) . . ? C97 C87 C77 104.3(3) . . ? CA7 C97 C87 102.3(3) . . ? CF7 CA7 CB7 121.2(4) . . ? CF7 CA7 C97 110.0(3) . . ? CB7 CA7 C97 128.8(4) . . ? CC7 CB7 CA7 117.8(5) . . ? CD7 CC7 CB7 121.5(5) . . ? CC7 CD7 CE7 120.7(4) . . ? CF7 CE7 CD7 118.8(4) . . ? CE7 CF7 CA7 120.1(4) . . ? CE7 CF7 C77 129.6(4) . . ? CA7 CF7 C77 110.3(3) . . ? O1BW O1AW O2BW 116(3) . . ? O4AW O4BW O9BW 127.0(17) . 1_645 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 74.25 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.611 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.079