# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Loeb, Stephen J.' ; School of Physical Sciences Chemistry and Biochemistry University of Windsor Ontario N9B 3P4 Canada ; 'Davidson, Gregory J. E.' ; School of Physical Sciences Chemistry and Biochemistry University of Windsor Ontario N9B 3P4 Canada ; 'Tiburcio Baez, Jorge' ; School of Physical Sciences Chemistry and Biochemistry University of Windsor Ontario N9B 3P4 Canada ; _publ_contact_author_name 'Prof Stephen Loeb' _publ_contact_author_address ; Chemistry & Biochemistry University of Windsor Windsor Ontario N9B 3P4 CANADA ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_contact_author_email 'loeb@uwindsor.ca' _publ_requested_journal 'ChemComm' _publ_requested_coeditor_name ? _publ_contact_letter ; These two structures are part of a study on the formation of pseudo-polyrotaxanes comprising a protonated 1,2-bis(4,4'-bipyridinium)ethane axle and a dibenzo-24-crown-8 ether wheel ; _publ_section_title ; Pseudo-polyrotaxanes based on a protonated version of the 1,2-bis(4,4’-bipyridinium)ethane/24-crown-8 ether motif ; data_hydrogen-bonded_pseudo-polyrotaxane _database_code_CSD 181512 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H98 F12 N4 O34 S4' _chemical_formula_weight 1943.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.332(3) _cell_length_b 20.385(3) _cell_length_c 12.300(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.332(3) _cell_angle_gamma 90.00 _cell_volume 4341.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'reflections from 120 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description prism _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0305 _exptl_absorpt_correction_T_max 0.0584 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 15289 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 21.00 _reflns_number_total 4649 _reflns_number_gt 2497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL XP' _computing_publication_material 'Siemens SHELXTL XCIF' _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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4649 _refine_ls_number_parameters 574 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1815 _refine_ls_R_factor_gt 0.1163 _refine_ls_wR_factor_ref 0.3337 _refine_ls_wR_factor_gt 0.2865 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 S1 S -0.2613(2) -0.76476(18) 0.7937(4) 0.1023(13) Uani 1 1 d . . . S2 S -0.2424(2) -0.2477(2) 1.0936(4) 0.1208(15) Uani 1 1 d . . . F1 F -0.2569(6) -0.8180(6) 0.9856(9) 0.183(4) Uani 1 1 d . . . F2 F -0.2005(6) -0.7250(7) 0.9764(9) 0.216(6) Uani 1 1 d . . . F3 F -0.3171(6) -0.7303(5) 0.9786(11) 0.192(5) Uani 1 1 d . . . F4 F -0.2382(6) -0.3279(5) 0.9308(9) 0.168(4) Uani 1 1 d . . . F5 F -0.3153(7) -0.2487(6) 0.9065(10) 0.214(5) Uani 1 1 d . . . F6 F -0.1945(8) -0.2294(7) 0.9031(12) 0.235(7) Uani 1 1 d . . . O1 O 0.0020(4) -0.4357(3) 0.7215(5) 0.0669(18) Uani 1 1 d . . . O2 O -0.0336(4) -0.3458(3) 0.9015(6) 0.079(2) Uani 1 1 d . . . O3 O 0.0507(4) -0.3509(3) 1.0950(6) 0.082(2) Uani 1 1 d . . . O4 O -0.0040(4) -0.5631(3) 0.7245(5) 0.0709(19) Uani 1 1 d . . . O5 O -0.4870(4) -0.5625(3) 1.2159(5) 0.0601(17) Uani 1 1 d . . . O6 O -0.5286(4) -0.6329(3) 1.4152(5) 0.0693(19) Uani 1 1 d . . . O7 O -0.5074(4) -0.6587(3) 1.6406(6) 0.073(2) Uani 1 1 d . . . O8 O -0.4725(4) -0.4374(3) 1.1933(5) 0.0639(18) Uani 1 1 d . . . O9 O -0.2656(5) -0.6974(4) 0.7645(10) 0.152(4) Uani 1 1 d . . . O10 O -0.3306(5) -0.8013(5) 0.7765(10) 0.154(4) Uani 1 1 d . . . O11 O -0.1921(4) -0.7976(4) 0.7775(8) 0.114(3) Uani 1 1 d . . . O12 O -0.2550(6) -0.1789(4) 1.1012(10) 0.147(4) Uani 1 1 d . . . O13 O -0.3031(6) -0.2893(5) 1.1355(10) 0.155(4) Uani 1 1 d . . . O14 O -0.1688(5) -0.2721(5) 1.1298(9) 0.129(4) Uani 1 1 d . . . N1 N -0.3737(5) -0.4741(7) 1.4445(7) 0.088(3) Uani 1 1 d . . . H1A H -0.4046 -0.4716 1.4973 0.105 Uiso 1 1 calc R . . N2 N -0.1030(4) -0.4952(4) 1.0454(6) 0.0485(19) Uani 1 1 d . . . C1 C -0.3592(7) -0.5323(8) 1.4013(10) 0.095(4) Uani 1 1 d . . . H1B H -0.3835 -0.5697 1.4268 0.115 Uiso 1 1 calc R . . C2 C -0.3086(5) -0.5372(6) 1.3192(9) 0.067(3) Uani 1 1 d . . . H2A H -0.2987 -0.5781 1.2890 0.081 Uiso 1 1 calc R . . C3 C -0.2725(5) -0.4829(5) 1.2812(8) 0.054(2) Uani 1 1 d . . . C4 C -0.2924(5) -0.4237(5) 1.3272(8) 0.069(3) Uani 1 1 d . . . H4A H -0.2711 -0.3851 1.3015 0.083 Uiso 1 1 calc R . . C5 C -0.3423(6) -0.4211(7) 1.4089(9) 0.085(4) Uani 1 1 d . . . H5A H -0.3541 -0.3809 1.4398 0.102 Uiso 1 1 calc R . . C6 C -0.2143(4) -0.4876(4) 1.1951(7) 0.045(2) Uani 1 1 d . . . C7 C -0.1870(5) -0.5474(4) 1.1605(8) 0.056(3) Uani 1 1 d . . . H7A H -0.2062 -0.5861 1.1889 0.068 Uiso 1 1 calc R . . C8 C -0.1323(5) -0.5495(5) 1.0851(9) 0.063(3) Uani 1 1 d . . . H8A H -0.1150 -0.5900 1.0609 0.075 Uiso 1 1 calc R . . C9 C -0.1296(5) -0.4373(4) 1.0745(8) 0.056(2) Uani 1 1 d . . . H9A H -0.1099 -0.3993 1.0444 0.067 Uiso 1 1 calc R . . C10 C -0.1844(5) -0.4332(4) 1.1461(8) 0.054(2) Uani 1 1 d . . . H10A H -0.2032 -0.3920 1.1639 0.064 Uiso 1 1 calc R . . C11 C -0.0372(5) -0.5004(5) 0.9681(8) 0.060(3) Uani 1 1 d . . . H11A H -0.0419 -0.5408 0.9267 0.072 Uiso 1 1 calc R . . H11B H -0.0392 -0.4639 0.9175 0.072 Uiso 1 1 calc R . . C12 C 0.0433(5) -0.5349(6) 0.6504(8) 0.059(3) Uani 1 1 d . . . C13 C 0.0875(6) -0.5714(6) 0.5794(10) 0.078(3) Uani 1 1 d . . . H13A H 0.0856 -0.6170 0.5802 0.094 Uiso 1 1 calc R . . C14 C 0.1346(7) -0.5385(8) 0.5072(10) 0.090(4) Uani 1 1 d . . . H14A H 0.1641 -0.5621 0.4594 0.108 Uiso 1 1 calc R . . C15 C 0.1367(7) -0.4740(9) 0.5073(10) 0.091(4) Uani 1 1 d . . . H15A H 0.1679 -0.4527 0.4586 0.109 Uiso 1 1 calc R . . C16 C 0.0935(6) -0.4361(6) 0.5784(10) 0.084(3) Uani 1 1 d . . . H16A H 0.0966 -0.3905 0.5778 0.101 Uiso 1 1 calc R . . C17 C 0.0468(5) -0.4676(6) 0.6486(8) 0.058(3) Uani 1 1 d . . . C18 C -0.0057(6) -0.3647(5) 0.7102(9) 0.074(3) Uani 1 1 d . . . H18A H -0.0240 -0.3537 0.6370 0.089 Uiso 1 1 calc R . . H18B H 0.0440 -0.3438 0.7242 0.089 Uiso 1 1 calc R . . C19 C -0.0618(7) -0.3418(5) 0.7903(11) 0.094(4) Uani 1 1 d . . . H19A H -0.0754 -0.2967 0.7739 0.112 Uiso 1 1 calc R . . H19B H -0.1084 -0.3679 0.7818 0.112 Uiso 1 1 calc R . . C20 C 0.0076(7) -0.2923(5) 0.9392(11) 0.089(4) Uani 1 1 d . . . H20A H -0.0186 -0.2524 0.9157 0.107 Uiso 1 1 calc R . . H20B H 0.0583 -0.2925 0.9086 0.107 Uiso 1 1 calc R . . C21 C 0.0160(7) -0.2930(5) 1.0573(10) 0.082(3) Uani 1 1 d . . . H21A H 0.0471 -0.2558 1.0816 0.099 Uiso 1 1 calc R . . H21B H -0.0344 -0.2887 1.0879 0.099 Uiso 1 1 calc R . . C22 C 0.0766(7) -0.3499(6) 1.2107(10) 0.095(4) Uani 1 1 d . . . H22A H 0.1196 -0.3799 1.2215 0.114 Uiso 1 1 calc R . . H22B H 0.0948 -0.3062 1.2294 0.114 Uiso 1 1 calc R . . C23 C -0.0157(7) -0.6318(5) 0.7162(9) 0.084(3) Uani 1 1 d . . . H23A H 0.0317 -0.6548 0.7365 0.101 Uiso 1 1 calc R . . H23B H -0.0308 -0.6435 0.6419 0.101 Uiso 1 1 calc R . . C24 C -0.4348(5) -0.4753(5) 1.1216(7) 0.052(2) Uani 1 1 d . . . C25 C -0.3885(6) -0.4508(5) 1.0411(9) 0.069(3) Uani 1 1 d . . . H25A H -0.3820 -0.4058 1.0335 0.082 Uiso 1 1 calc R . . C26 C -0.3523(6) -0.4935(7) 0.9726(9) 0.079(3) Uani 1 1 d . . . H26A H -0.3236 -0.4770 0.9165 0.094 Uiso 1 1 calc R . . C27 C -0.3581(6) -0.5581(7) 0.9859(9) 0.078(3) Uani 1 1 d . . . H27A H -0.3314 -0.5861 0.9411 0.093 Uiso 1 1 calc R . . C28 C -0.4036(5) -0.5845(5) 1.0661(8) 0.064(3) Uani 1 1 d . . . H28A H -0.4081 -0.6297 1.0736 0.077 Uiso 1 1 calc R . . C29 C -0.4423(5) -0.5424(5) 1.1351(7) 0.049(2) Uani 1 1 d . . . C30 C -0.5068(5) -0.6300(5) 1.2213(8) 0.068(3) Uani 1 1 d . . . H30A H -0.4609 -0.6561 1.2370 0.082 Uiso 1 1 calc R . . H30B H -0.5299 -0.6443 1.1521 0.082 Uiso 1 1 calc R . . C31 C -0.5639(6) -0.6390(5) 1.3108(9) 0.078(3) Uani 1 1 d . . . H31A H -0.6046 -0.6064 1.3020 0.093 Uiso 1 1 calc R . . H31B H -0.5875 -0.6820 1.3037 0.093 Uiso 1 1 calc R . . C32 C -0.5019(6) -0.6942(5) 1.4587(9) 0.072(3) Uani 1 1 d . . . H32A H -0.4679 -0.7148 1.4080 0.086 Uiso 1 1 calc R . . H32B H -0.5455 -0.7232 1.4681 0.086 Uiso 1 1 calc R . . C33 C -0.4603(7) -0.6846(5) 1.5637(10) 0.083(3) Uani 1 1 d . . . H33A H -0.4399 -0.7264 1.5895 0.099 Uiso 1 1 calc R . . H33B H -0.4170 -0.6553 1.5541 0.099 Uiso 1 1 calc R . . C34 C -0.4742(6) -0.6613(5) 1.7483(9) 0.071(3) Uani 1 1 d . . . H34A H -0.4254 -0.6379 1.7514 0.086 Uiso 1 1 calc R . . H34B H -0.4642 -0.7066 1.7687 0.086 Uiso 1 1 calc R . . C35 C -0.4726(6) -0.3686(5) 1.1748(8) 0.071(3) Uani 1 1 d . . . H35A H -0.4898 -0.3592 1.1004 0.085 Uiso 1 1 calc R . . H35B H -0.4209 -0.3511 1.1869 0.085 Uiso 1 1 calc R . . C36 C -0.2583(6) -0.7568(8) 0.9289(19) 0.131(7) Uani 1 1 d . . . C37 C -0.2485(11) -0.2659(9) 0.9566(15) 0.130(6) Uani 1 1 d . . . O1W O -0.4376 -0.5192 1.6236 0.158(5) Uani 1 1 d . . . O2W O -0.1771(9) -0.4909(8) 0.7876(12) 0.229(6) Uani 1 1 d . . . O3W O -0.2854(6) -0.5670(6) 1.6878(11) 0.174(5) Uani 1 1 d . . . H1WA H -0.4694 -0.5009 1.6648 0.200 Uiso 1 1 d . . . H1WB H -0.4483 -0.5597 1.6305 0.200 Uiso 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 S1 0.085(3) 0.080(2) 0.142(4) -0.001(2) 0.002(2) -0.005(2) S2 0.100(3) 0.120(3) 0.143(4) -0.008(3) 0.004(3) 0.025(2) F1 0.206(11) 0.180(10) 0.164(10) 0.018(8) 0.026(8) 0.026(8) F2 0.163(9) 0.341(16) 0.147(9) -0.092(9) 0.039(7) -0.103(10) F3 0.168(8) 0.144(8) 0.274(14) -0.042(8) 0.111(9) -0.028(7) F4 0.189(9) 0.134(8) 0.183(10) 0.003(7) 0.032(8) 0.045(7) F5 0.197(11) 0.277(14) 0.164(10) -0.015(9) -0.049(9) 0.089(10) F6 0.256(14) 0.225(12) 0.233(14) 0.091(10) 0.118(12) 0.042(10) O1 0.081(5) 0.061(4) 0.058(4) 0.009(4) 0.001(4) -0.005(4) O2 0.110(6) 0.058(5) 0.068(5) 0.009(4) -0.007(4) -0.002(4) O3 0.106(5) 0.058(5) 0.082(6) 0.001(4) 0.013(5) -0.001(4) O4 0.107(5) 0.054(4) 0.052(4) -0.009(3) 0.004(4) -0.016(4) O5 0.077(4) 0.052(4) 0.052(4) 0.003(3) 0.011(4) 0.001(3) O6 0.086(5) 0.074(5) 0.048(4) -0.008(4) 0.004(4) -0.001(4) O7 0.078(5) 0.087(5) 0.052(5) 0.001(4) 0.000(4) 0.016(4) O8 0.078(4) 0.060(4) 0.053(4) 0.006(4) 0.003(4) 0.000(3) O9 0.137(8) 0.077(7) 0.243(14) 0.051(7) 0.029(8) 0.004(6) O10 0.093(6) 0.134(8) 0.233(13) 0.011(8) -0.029(7) -0.043(6) O11 0.089(6) 0.096(6) 0.157(9) -0.012(6) 0.012(6) 0.023(5) O12 0.177(9) 0.069(6) 0.197(11) 0.002(6) 0.044(8) 0.036(6) O13 0.135(8) 0.164(10) 0.171(11) 0.029(8) 0.055(8) -0.048(7) O14 0.083(6) 0.142(8) 0.161(10) -0.023(7) -0.024(6) 0.024(6) N1 0.063(6) 0.156(10) 0.045(6) -0.016(7) 0.018(5) -0.001(7) N2 0.051(4) 0.047(5) 0.048(5) 0.005(4) 0.010(4) 0.000(4) C1 0.091(9) 0.140(13) 0.056(8) -0.006(8) 0.011(7) -0.040(9) C2 0.047(6) 0.096(9) 0.059(7) -0.012(6) 0.001(6) 0.003(6) C3 0.043(5) 0.067(7) 0.051(6) 0.006(5) -0.006(5) 0.006(5) C4 0.062(6) 0.086(8) 0.059(7) -0.001(6) 0.007(6) 0.016(6) C5 0.071(7) 0.123(11) 0.064(8) -0.003(7) 0.025(7) 0.015(7) C6 0.025(4) 0.056(6) 0.054(6) -0.001(5) -0.005(4) 0.010(4) C7 0.047(6) 0.056(6) 0.066(7) 0.002(5) 0.005(6) 0.002(5) C8 0.054(6) 0.057(7) 0.080(8) -0.022(6) 0.015(6) 0.004(5) C9 0.066(6) 0.040(6) 0.062(7) 0.006(5) 0.018(6) 0.000(5) C10 0.044(5) 0.050(6) 0.069(7) 0.006(5) 0.014(5) 0.002(5) C11 0.058(6) 0.063(6) 0.061(7) 0.004(5) 0.009(5) 0.001(5) C12 0.053(6) 0.073(8) 0.050(7) -0.008(6) -0.013(5) 0.004(6) C13 0.059(7) 0.099(9) 0.075(8) -0.019(7) -0.027(7) 0.009(7) C14 0.061(8) 0.149(13) 0.061(8) -0.019(9) 0.008(7) 0.010(9) C15 0.062(8) 0.159(14) 0.051(8) 0.026(9) -0.010(6) -0.006(9) C16 0.068(7) 0.117(10) 0.068(8) 0.013(8) 0.000(7) -0.009(7) C17 0.052(6) 0.084(8) 0.037(6) 0.008(6) -0.009(5) -0.004(6) C18 0.082(7) 0.068(8) 0.071(8) 0.023(6) -0.022(7) -0.010(6) C19 0.101(9) 0.063(7) 0.117(12) 0.023(7) 0.005(9) 0.020(7) C20 0.102(9) 0.049(7) 0.118(12) 0.018(7) 0.017(8) -0.001(6) C21 0.101(9) 0.064(8) 0.082(9) -0.018(7) 0.014(7) 0.003(6) C22 0.119(10) 0.079(8) 0.085(10) -0.010(7) -0.028(9) -0.035(7) C23 0.113(9) 0.078(9) 0.062(8) -0.013(6) 0.007(7) -0.022(7) C24 0.043(5) 0.072(7) 0.038(6) -0.005(5) -0.012(5) 0.002(5) C25 0.067(7) 0.074(7) 0.064(7) 0.010(6) -0.004(6) 0.000(6) C26 0.082(8) 0.108(10) 0.046(7) 0.013(7) 0.000(6) -0.004(8) C27 0.073(7) 0.109(10) 0.052(7) -0.003(7) 0.010(6) 0.013(7) C28 0.065(6) 0.068(7) 0.058(7) -0.010(6) -0.008(6) -0.002(5) C29 0.046(5) 0.064(7) 0.036(6) 0.008(5) -0.008(5) -0.001(5) C30 0.067(6) 0.092(9) 0.047(6) -0.001(6) 0.004(6) -0.003(6) C31 0.092(8) 0.071(7) 0.071(8) 0.008(6) 0.004(7) -0.010(6) C32 0.092(8) 0.065(7) 0.059(8) 0.000(6) 0.006(6) 0.015(6) C33 0.093(8) 0.075(8) 0.080(9) 0.029(7) 0.016(8) 0.030(6) C34 0.085(7) 0.062(7) 0.067(8) 0.020(6) -0.003(7) 0.013(6) C35 0.093(8) 0.071(8) 0.048(6) 0.014(5) -0.004(6) 0.004(6) C36 0.025(6) 0.113(12) 0.26(2) -0.073(14) 0.032(10) -0.027(7) C37 0.142(15) 0.123(14) 0.123(15) 0.012(11) -0.007(12) 0.051(12) O1W 0.241(11) 0.081(6) 0.163(10) 0.000(6) 0.136(9) 0.017(6) O2W 0.255(15) 0.249(16) 0.185(14) -0.024(12) 0.036(12) -0.027(12) O3W 0.136(8) 0.194(11) 0.195(12) 0.035(10) 0.034(9) 0.010(8) _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 S1 O11 1.395(8) . ? S1 O9 1.420(9) . ? S1 O10 1.422(8) . ? S1 C36 1.67(2) . ? S2 O12 1.423(9) . ? S2 O14 1.423(8) . ? S2 O13 1.462(9) . ? S2 C37 1.723(19) . ? F1 C36 1.430(19) . ? F2 C36 1.309(14) . ? F3 C36 1.324(14) . ? F4 C37 1.317(17) . ? F5 C37 1.337(16) . ? F6 C37 1.384(19) . ? O1 C17 1.374(11) . ? O1 C18 1.459(11) . ? O2 C20 1.374(12) . ? O2 C19 1.436(14) . ? O3 C21 1.396(12) . ? O3 C22 1.475(13) . ? O4 C12 1.377(11) . ? O4 C23 1.418(11) . ? O5 C29 1.349(10) . ? O5 C30 1.420(11) . ? O6 C31 1.405(12) . ? O6 C32 1.430(11) . ? O7 C33 1.380(12) . ? O7 C34 1.424(12) . ? O8 C24 1.361(10) . ? O8 C35 1.420(11) . ? N1 C5 1.293(14) . ? N1 C1 1.329(15) . ? N2 C8 1.321(11) . ? N2 C9 1.321(10) . ? N2 C11 1.518(11) . ? C1 C2 1.368(15) . ? C2 C3 1.364(13) . ? C3 C4 1.382(13) . ? C3 C6 1.494(13) . ? C4 C5 1.354(14) . ? C6 C10 1.373(11) . ? C6 C7 1.382(11) . ? C7 C8 1.354(12) . ? C9 C10 1.323(11) . ? C11 C11 1.481(16) 3_547 ? C12 C17 1.373(13) . ? C12 C13 1.400(14) . ? C13 C14 1.402(16) . ? C14 C15 1.316(16) . ? C15 C16 1.406(16) . ? C16 C17 1.367(14) . ? C18 C19 1.487(15) . ? C20 C21 1.454(15) . ? C22 C23 1.463(15) 3_547 ? C23 C22 1.463(15) 3_547 ? C24 C29 1.385(12) . ? C24 C25 1.392(13) . ? C25 C26 1.380(14) . ? C26 C27 1.330(14) . ? C27 C28 1.396(14) . ? C28 C29 1.396(12) . ? C30 C31 1.521(13) . ? C32 C33 1.466(14) . ? C34 C35 1.479(13) 3_448 ? C35 C34 1.479(13) 3_448 ? 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 O11 S1 O9 117.7(6) . . ? O11 S1 O10 117.0(6) . . ? O9 S1 O10 115.7(6) . . ? O11 S1 C36 101.3(6) . . ? O9 S1 C36 99.0(8) . . ? O10 S1 C36 101.0(7) . . ? O12 S2 O14 117.5(7) . . ? O12 S2 O13 115.7(7) . . ? O14 S2 O13 109.6(7) . . ? O12 S2 C37 105.8(8) . . ? O14 S2 C37 104.4(8) . . ? O13 S2 C37 101.8(9) . . ? C17 O1 C18 117.3(8) . . ? C20 O2 C19 115.4(9) . . ? C21 O3 C22 114.7(8) . . ? C12 O4 C23 116.9(8) . . ? C29 O5 C30 118.4(7) . . ? C31 O6 C32 112.8(7) . . ? C33 O7 C34 113.2(8) . . ? C24 O8 C35 117.0(8) . . ? C5 N1 C1 121.4(11) . . ? C8 N2 C9 120.3(7) . . ? C8 N2 C11 118.9(8) . . ? C9 N2 C11 120.8(7) . . ? N1 C1 C2 119.9(12) . . ? C3 C2 C1 120.7(11) . . ? C2 C3 C4 116.3(9) . . ? C2 C3 C6 121.6(9) . . ? C4 C3 C6 122.1(9) . . ? C5 C4 C3 121.0(11) . . ? N1 C5 C4 120.6(12) . . ? C10 C6 C7 115.9(8) . . ? C10 C6 C3 122.5(8) . . ? C7 C6 C3 121.6(8) . . ? C8 C7 C6 119.8(9) . . ? N2 C8 C7 121.1(8) . . ? N2 C9 C10 120.3(8) . . ? C9 C10 C6 122.4(8) . . ? C11 C11 N2 109.1(10) 3_547 . ? C17 C12 O4 117.1(9) . . ? C17 C12 C13 119.8(11) . . ? O4 C12 C13 123.1(10) . . ? C12 C13 C14 119.2(11) . . ? C15 C14 C13 119.7(12) . . ? C14 C15 C16 122.3(12) . . ? C17 C16 C15 118.6(12) . . ? C16 C17 C12 120.5(11) . . ? C16 C17 O1 123.7(11) . . ? C12 C17 O1 115.8(9) . . ? O1 C18 C19 107.9(8) . . ? O2 C19 C18 114.1(9) . . ? O2 C20 C21 111.0(9) . . ? O3 C21 C20 111.3(9) . . ? C23 C22 O3 113.1(9) 3_547 . ? O4 C23 C22 108.2(9) . 3_547 ? O8 C24 C29 115.7(9) . . ? O8 C24 C25 124.3(9) . . ? C29 C24 C25 120.0(9) . . ? C26 C25 C24 119.8(10) . . ? C27 C26 C25 120.7(11) . . ? C26 C27 C28 121.1(11) . . ? C27 C28 C29 119.5(10) . . ? O5 C29 C24 116.6(8) . . ? O5 C29 C28 124.5(9) . . ? C24 C29 C28 118.9(9) . . ? O5 C30 C31 108.4(8) . . ? O6 C31 C30 112.3(8) . . ? O6 C32 C33 110.7(8) . . ? O7 C33 C32 111.8(9) . . ? O7 C34 C35 109.9(8) . 3_448 ? O8 C35 C34 107.5(8) . 3_448 ? F2 C36 F3 100.5(13) . . ? F2 C36 F1 102.6(17) . . ? F3 C36 F1 97.3(14) . . ? F2 C36 S1 119.0(12) . . ? F3 C36 S1 120.3(14) . . ? F1 C36 S1 113.6(10) . . ? F4 C37 F5 105.3(16) . . ? F4 C37 F6 107.5(15) . . ? F5 C37 F6 103.2(15) . . ? F4 C37 S2 116.0(13) . . ? F5 C37 S2 114.3(13) . . ? F6 C37 S2 109.5(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.645 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.120 #===END data_pi-stacked_pseudo-polyrotaxane _database_code_CSD 181513 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H126 F12 N4 O40 S4' _chemical_formula_weight 2356.3 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.653(4) _cell_length_b 14.953(5) _cell_length_c 17.266(6) _cell_angle_alpha 98.355(7) _cell_angle_beta 93.107(6) _cell_angle_gamma 110.818(7) _cell_volume 2764.2(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description prism _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1234 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1045 _exptl_absorpt_correction_T_max 0.1452 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 12412 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 23.35 _reflns_number_total 7890 _reflns_number_gt 4361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL XP' _computing_publication_material 'Siemens SHELXTL XCIF' _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^)+(0.1803P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7890 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2867 _refine_ls_wR_factor_gt 0.2482 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.361 _refine_ls_shift/su_mean 0.014 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 S1 S 0.36943(16) 0.09174(13) 0.38147(11) 0.0986(6) Uani 1 1 d . . . S2 S 0.0470(3) 0.3475(3) 0.12871(19) 0.1826(15) Uani 1 1 d . . . F1 F 0.4834(6) 0.2562(4) 0.3379(4) 0.193(3) Uani 1 1 d . . . F2 F 0.2948(7) 0.2288(4) 0.3520(4) 0.210(3) Uani 1 1 d . . . F3 F 0.3416(5) 0.1554(4) 0.2526(3) 0.1538(18) Uani 1 1 d . . . F4 F 0.2033(8) 0.2562(6) 0.1211(5) 0.235(3) Uani 1 1 d . . . F5 F 0.117(3) 0.2797(12) 0.2250(9) 0.53(2) Uani 1 1 d . . . F6 F 0.2706(8) 0.3872(7) 0.1917(8) 0.280(5) Uani 1 1 d . . . O1 O 0.5844(4) -0.1092(3) 0.1548(2) 0.0860(12) Uani 1 1 d . . . O2 O 0.6983(3) 0.1054(3) 0.1645(2) 0.0803(11) Uani 1 1 d . . . O3 O 0.5621(4) 0.2164(3) 0.1354(3) 0.0971(13) Uani 1 1 d . . . O4 O 0.4659(4) -0.2406(3) 0.0315(3) 0.0970(13) Uani 1 1 d . . . O5 O 1.1242(3) 0.1438(3) 0.7073(2) 0.0774(10) Uani 1 1 d . . . O6 O 1.0708(4) 0.1710(4) 0.5504(3) 0.1179(17) Uani 1 1 d . . . O7 O 0.9085(6) 0.1813(5) 0.4083(3) 0.136(2) Uani 1 1 d . . . O8 O 0.8175(3) 0.2870(2) 0.5270(2) 0.0699(10) Uani 1 1 d . . . O9 O 0.9722(3) 0.4536(2) 0.59923(19) 0.0640(9) Uani 1 1 d . . . O10 O 1.2117(3) 0.4878(2) 0.67014(19) 0.0641(9) Uani 1 1 d . . . O11 O 1.3502(3) 0.4630(2) 0.7994(2) 0.0785(11) Uani 1 1 d . . . O12 O 1.2378(4) 0.2714(3) 0.8269(2) 0.0859(12) Uani 1 1 d . . . O13 O 0.4598(5) 0.0599(5) 0.3458(3) 0.142(2) Uani 1 1 d . . . O14 O 0.2478(4) 0.0249(3) 0.3617(3) 0.1199(16) Uani 1 1 d . . . O15 O 0.4024(5) 0.1371(4) 0.4609(3) 0.1293(18) Uani 1 1 d . . . O16 O -0.0408(8) 0.2476(8) 0.1031(5) 0.267(5) Uani 1 1 d . . . O17 O 0.0401(7) 0.4195(6) 0.1849(4) 0.191(3) Uani 1 1 d . . . O18 O 0.0882(10) 0.3861(7) 0.0566(5) 0.230(4) Uani 1 1 d . . . N1 N -0.0273(4) 0.6457(4) 0.2689(3) 0.0720(12) Uani 1 1 d . . . H1A H -0.0762 0.6071 0.2954 0.086 Uiso 1 1 calc R . . N2 N 0.3632(3) 0.9577(3) 0.0549(2) 0.0514(9) Uani 1 1 d . . . C1 C -0.0302(5) 0.6151(4) 0.1927(4) 0.0810(16) Uani 1 1 d . . . H1B H -0.0833 0.5533 0.1685 0.097 Uiso 1 1 calc R . . C2 C 0.0465(5) 0.6765(4) 0.1505(3) 0.0758(15) Uani 1 1 d . . . H2A H 0.0454 0.6566 0.0968 0.091 Uiso 1 1 calc R . . C3 C 0.1261(4) 0.7683(3) 0.1868(3) 0.0495(11) Uani 1 1 d . . . C4 C 0.1247(5) 0.7943(4) 0.2660(3) 0.0633(13) Uani 1 1 d . . . H4A H 0.1779 0.8550 0.2923 0.076 Uiso 1 1 calc R . . C5 C 0.0460(6) 0.7318(5) 0.3062(3) 0.0741(15) Uani 1 1 d . . . H5A H 0.0441 0.7500 0.3598 0.089 Uiso 1 1 calc R . . C6 C 0.2078(4) 0.8361(3) 0.1406(3) 0.0492(11) Uani 1 1 d . . . C7 C 0.1923(4) 0.8176(3) 0.0599(3) 0.0601(12) Uani 1 1 d . . . H7A H 0.1276 0.7626 0.0335 0.072 Uiso 1 1 calc R . . C8 C 0.2698(5) 0.8783(4) 0.0175(3) 0.0619(13) Uani 1 1 d . . . H8A H 0.2578 0.8647 -0.0373 0.074 Uiso 1 1 calc R . . C9 C 0.3804(4) 0.9789(3) 0.1338(3) 0.0561(12) Uani 1 1 d . . . H9A H 0.4446 1.0348 0.1592 0.067 Uiso 1 1 calc R . . C10 C 0.3041(4) 0.9187(3) 0.1766(3) 0.0553(12) Uani 1 1 d . . . H10A H 0.3174 0.9336 0.2313 0.066 Uiso 1 1 calc R . . C11 C 0.4515(4) 1.0205(3) 0.0090(3) 0.0588(12) Uani 1 1 d . . . H11A H 0.4894 1.0858 0.0391 0.071 Uiso 1 1 calc R . . H11B H 0.4084 1.0236 -0.0396 0.071 Uiso 1 1 calc R . . C12 C 0.4340(7) -0.2628(5) 0.1011(6) 0.097(2) Uani 1 1 d . . . C13 C 0.3415(7) -0.3490(6) 0.1146(7) 0.124(3) Uani 1 1 d . . . H13A H 0.2962 -0.3962 0.0718 0.149 Uiso 1 1 calc R . . C14 C 0.3179(11) -0.3641(10) 0.1869(10) 0.155(5) Uani 1 1 d . . . H14A H 0.2556 -0.4215 0.1929 0.186 Uiso 1 1 calc R . . C15 C 0.3791(12) -0.3009(10) 0.2511(8) 0.142(4) Uani 1 1 d . . . H15A H 0.3610 -0.3149 0.3008 0.171 Uiso 1 1 calc R . . C16 C 0.4731(8) -0.2114(7) 0.2433(6) 0.126(3) Uani 1 1 d . . . H16A H 0.5172 -0.1657 0.2873 0.151 Uiso 1 1 calc R . . C17 C 0.4959(7) -0.1954(6) 0.1689(5) 0.093(2) Uani 1 1 d . . . C18 C 0.6578(6) -0.0414(6) 0.2218(4) 0.096(2) Uani 1 1 d . . . H18A H 0.6996 -0.0725 0.2526 0.116 Uiso 1 1 calc R . . H18B H 0.6056 -0.0187 0.2549 0.116 Uiso 1 1 calc R . . C19 C 0.7501(6) 0.0418(5) 0.1943(4) 0.095(2) Uani 1 1 d . . . H19A H 0.8131 0.0790 0.2378 0.114 Uiso 1 1 calc R . . H19B H 0.7901 0.0169 0.1533 0.114 Uiso 1 1 calc R . . C20 C 0.7032(6) 0.1853(5) 0.2193(4) 0.104(2) Uani 1 1 d . . . H20A H 0.7847 0.2144 0.2489 0.125 Uiso 1 1 calc R . . H20B H 0.6434 0.1639 0.2560 0.125 Uiso 1 1 calc R . . C21 C 0.6775(6) 0.2574(4) 0.1810(4) 0.096(2) Uani 1 1 d . . . H21A H 0.6783 0.3109 0.2206 0.115 Uiso 1 1 calc R . . H21B H 0.7413 0.2830 0.1476 0.115 Uiso 1 1 calc R . . C22 C 0.5206(8) 0.2832(6) 0.1038(6) 0.127(3) Uani 1 1 d . . . H22A H 0.5344 0.3387 0.1449 0.153 Uiso 1 1 calc R . . H22B H 0.4322 0.2525 0.0885 0.153 Uiso 1 1 calc R . . C23 C 0.4193(8) -0.3187(5) -0.0346(6) 0.119(3) Uani 1 1 d . . . H23A H 0.3303 -0.3386 -0.0450 0.142 Uiso 1 1 calc R . . H23B H 0.4382 -0.3741 -0.0237 0.142 Uiso 1 1 calc R . . C24 C 1.1511(5) 0.1893(4) 0.8429(3) 0.0726(15) Uani 1 1 d . . . C25 C 1.1201(7) 0.1719(5) 0.9169(4) 0.097(2) Uani 1 1 d . . . H25A H 1.1600 0.2191 0.9609 0.116 Uiso 1 1 calc R . . C26 C 1.0314(8) 0.0862(6) 0.9263(5) 0.105(2) Uani 1 1 d . . . H26A H 1.0121 0.0755 0.9766 0.126 Uiso 1 1 calc R . . C27 C 0.9727(7) 0.0181(6) 0.8640(6) 0.101(2) Uani 1 1 d . . . H27A H 0.9129 -0.0400 0.8711 0.122 Uiso 1 1 calc R . . C28 C 0.9993(6) 0.0326(5) 0.7890(5) 0.0872(18) Uani 1 1 d . . . H28A H 0.9572 -0.0155 0.7459 0.105 Uiso 1 1 calc R . . C29 C 1.0885(5) 0.1186(4) 0.7772(4) 0.0711(15) Uani 1 1 d . . . C30 C 1.0788(6) 0.0709(5) 0.6398(4) 0.0912(19) Uani 1 1 d . . . H30A H 0.9894 0.0486 0.6312 0.109 Uiso 1 1 calc R . . H30B H 1.1017 0.0159 0.6464 0.109 Uiso 1 1 calc R . . C31 C 1.1320(6) 0.1120(6) 0.5733(4) 0.108(2) Uani 1 1 d . . . H31A H 1.2193 0.1502 0.5877 0.129 Uiso 1 1 calc R . . H31B H 1.1237 0.0603 0.5298 0.129 Uiso 1 1 calc R . . C32 C 1.1071(8) 0.2013(8) 0.4803(5) 0.142(3) Uani 1 1 d . . . H32A H 1.1202 0.1488 0.4466 0.171 Uiso 1 1 calc R . . H32B H 1.1855 0.2557 0.4918 0.171 Uiso 1 1 calc R . . C33 C 1.0219(10) 0.2296(6) 0.4388(6) 0.140(3) Uani 1 1 d . . . H33A H 1.0182 0.2853 0.4738 0.168 Uiso 1 1 calc R . . H33B H 1.0639 0.2554 0.3953 0.168 Uiso 1 1 calc R . . C34 C 0.8192(7) 0.1400(5) 0.4561(5) 0.107(2) Uani 1 1 d . . . H34A H 0.8595 0.1335 0.5045 0.128 Uiso 1 1 calc R . . H34B H 0.7664 0.0755 0.4295 0.128 Uiso 1 1 calc R . . C35 C 0.7410(5) 0.1994(4) 0.4760(4) 0.0816(17) Uani 1 1 d . . . H35A H 0.7090 0.2142 0.4284 0.098 Uiso 1 1 calc R . . H35B H 0.6718 0.1637 0.5020 0.098 Uiso 1 1 calc R . . C36 C 0.7678(5) 0.3558(4) 0.5499(3) 0.0567(12) Uani 1 1 d . . . C37 C 0.6446(5) 0.3409(4) 0.5348(3) 0.0730(15) Uani 1 1 d . . . H37A H 0.5889 0.2812 0.5084 0.088 Uiso 1 1 calc R . . C38 C 0.6049(6) 0.4159(5) 0.5595(4) 0.0852(17) Uani 1 1 d . . . H38A H 0.5224 0.4073 0.5479 0.102 Uiso 1 1 calc R . . C39 C 0.6850(6) 0.5022(5) 0.6006(4) 0.0898(18) Uani 1 1 d . . . H39A H 0.6569 0.5515 0.6185 0.108 Uiso 1 1 calc R . . C40 C 0.8096(6) 0.5164(4) 0.6159(3) 0.0751(15) Uani 1 1 d . . . H40A H 0.8643 0.5754 0.6441 0.090 Uiso 1 1 calc R . . C41 C 0.8514(5) 0.4448(3) 0.5898(3) 0.0579(12) Uani 1 1 d . . . C42 C 1.0633(5) 0.5487(3) 0.6243(3) 0.0677(14) Uani 1 1 d . . . H42A H 1.0581 0.5725 0.6788 0.081 Uiso 1 1 calc R . . H42B H 1.0500 0.5930 0.5922 0.081 Uiso 1 1 calc R . . C43 C 1.1856(5) 0.5427(4) 0.6158(3) 0.0696(14) Uani 1 1 d . . . H43A H 1.1871 0.5122 0.5625 0.084 Uiso 1 1 calc R . . H43B H 1.2485 0.6077 0.6254 0.084 Uiso 1 1 calc R . . C44 C 1.3298(5) 0.4822(5) 0.6669(4) 0.0827(16) Uani 1 1 d . . . H44A H 1.3927 0.5469 0.6810 0.099 Uiso 1 1 calc R . . H44B H 1.3374 0.4556 0.6136 0.099 Uiso 1 1 calc R . . C45 C 1.3494(6) 0.4201(4) 0.7215(4) 0.0849(17) Uani 1 1 d . . . H45A H 1.2839 0.3564 0.7095 0.102 Uiso 1 1 calc R . . H45B H 1.4275 0.4119 0.7151 0.102 Uiso 1 1 calc R . . C46 C 1.3973(6) 0.4209(4) 0.8559(4) 0.091(2) Uani 1 1 d . . . H46A H 1.4478 0.4723 0.8983 0.109 Uiso 1 1 calc R . . H46B H 1.4505 0.3907 0.8313 0.109 Uiso 1 1 calc R . . C47 C 1.3024(6) 0.3480(4) 0.8899(3) 0.0844(17) Uani 1 1 d . . . H47A H 1.3402 0.3245 0.9298 0.101 Uiso 1 1 calc R . . H47B H 1.2465 0.3759 0.9139 0.101 Uiso 1 1 calc R . . C48 C 0.3701(9) 0.1880(6) 0.3274(6) 0.121(3) Uani 1 1 d . . . C49 C 0.1876(17) 0.3262(14) 0.1602(18) 0.43(2) Uani 1 1 d . . . O1W O 0.5749(15) -0.0652(9) 0.4070(8) 0.308(6) Uani 1 1 d . . . O2W O -0.1022(14) 0.4548(14) 0.0353(11) 0.451(12) 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 S1 0.0757(11) 0.1031(13) 0.0934(13) -0.0107(10) -0.0044(9) 0.0174(10) S2 0.1121(18) 0.253(4) 0.134(2) -0.043(3) 0.0051(16) 0.039(2) F1 0.189(5) 0.148(4) 0.180(6) 0.031(4) 0.061(4) -0.018(4) F2 0.301(8) 0.204(5) 0.233(7) 0.097(5) 0.173(6) 0.177(6) F3 0.185(5) 0.183(5) 0.106(4) 0.024(3) 0.024(3) 0.083(4) F4 0.241(8) 0.238(8) 0.230(8) -0.019(6) 0.008(6) 0.121(7) F5 1.02(6) 0.278(15) 0.223(12) 0.058(11) 0.07(2) 0.14(2) F6 0.164(6) 0.262(9) 0.389(14) -0.035(10) -0.061(8) 0.098(7) O1 0.097(3) 0.106(3) 0.074(3) 0.042(2) 0.018(2) 0.049(3) O2 0.080(2) 0.093(3) 0.062(2) 0.006(2) -0.0013(19) 0.029(2) O3 0.109(3) 0.086(3) 0.094(3) -0.001(2) -0.005(3) 0.041(3) O4 0.102(3) 0.077(3) 0.118(4) 0.036(3) 0.010(3) 0.034(2) O5 0.084(3) 0.081(2) 0.062(2) 0.001(2) -0.004(2) 0.031(2) O6 0.094(3) 0.216(5) 0.074(3) 0.056(3) 0.036(2) 0.077(4) O7 0.123(4) 0.226(6) 0.075(3) 0.001(4) 0.011(3) 0.096(5) O8 0.066(2) 0.060(2) 0.075(2) 0.0017(17) -0.0008(18) 0.0172(18) O9 0.061(2) 0.055(2) 0.069(2) 0.0124(16) -0.0002(17) 0.0133(17) O10 0.059(2) 0.076(2) 0.062(2) 0.0392(17) 0.0206(16) 0.0179(17) O11 0.088(3) 0.073(2) 0.079(3) 0.011(2) -0.002(2) 0.038(2) O12 0.119(3) 0.070(2) 0.058(2) 0.0066(19) 0.000(2) 0.025(2) O13 0.118(4) 0.192(5) 0.133(5) -0.002(4) 0.010(3) 0.091(4) O14 0.088(3) 0.106(3) 0.123(4) 0.003(3) -0.009(3) -0.007(3) O15 0.113(4) 0.136(4) 0.087(3) -0.025(3) 0.000(3) 0.003(3) O16 0.176(7) 0.309(11) 0.148(6) -0.033(7) -0.043(5) -0.076(7) O17 0.197(7) 0.247(8) 0.141(6) -0.055(6) -0.022(5) 0.135(6) O18 0.310(11) 0.302(10) 0.156(7) 0.099(7) 0.114(7) 0.171(9) N1 0.065(3) 0.083(3) 0.080(4) 0.051(3) 0.034(2) 0.023(3) N2 0.050(2) 0.059(2) 0.046(2) 0.0203(19) 0.0185(18) 0.014(2) C1 0.074(4) 0.074(4) 0.086(5) 0.028(3) 0.023(3) 0.010(3) C2 0.079(4) 0.069(4) 0.067(4) 0.023(3) 0.029(3) 0.006(3) C3 0.047(3) 0.057(3) 0.050(3) 0.020(2) 0.018(2) 0.020(2) C4 0.071(3) 0.068(3) 0.051(3) 0.024(2) 0.022(2) 0.019(3) C5 0.092(4) 0.088(4) 0.052(3) 0.032(3) 0.028(3) 0.034(4) C6 0.045(2) 0.056(3) 0.047(3) 0.014(2) 0.014(2) 0.015(2) C7 0.056(3) 0.062(3) 0.048(3) 0.010(2) 0.011(2) 0.003(2) C8 0.061(3) 0.068(3) 0.047(3) 0.015(2) 0.014(2) 0.010(3) C9 0.054(3) 0.059(3) 0.047(3) 0.010(2) 0.011(2) 0.010(2) C10 0.060(3) 0.063(3) 0.040(3) 0.014(2) 0.017(2) 0.016(3) C11 0.063(3) 0.056(3) 0.057(3) 0.027(2) 0.023(2) 0.014(2) C12 0.089(5) 0.083(5) 0.139(7) 0.040(5) 0.019(5) 0.047(4) C13 0.101(6) 0.105(6) 0.193(10) 0.073(6) 0.036(6) 0.049(5) C14 0.130(9) 0.166(11) 0.235(15) 0.132(11) 0.079(10) 0.089(8) C15 0.157(10) 0.190(12) 0.168(10) 0.128(9) 0.093(8) 0.123(9) C16 0.127(6) 0.163(8) 0.155(8) 0.107(7) 0.071(6) 0.096(6) C17 0.097(5) 0.116(6) 0.119(6) 0.085(5) 0.053(5) 0.073(5) C18 0.096(5) 0.153(6) 0.079(5) 0.057(5) 0.024(4) 0.076(5) C19 0.078(4) 0.141(6) 0.074(4) 0.017(4) -0.010(3) 0.051(4) C20 0.090(5) 0.135(6) 0.071(4) -0.013(4) -0.009(3) 0.037(4) C21 0.083(4) 0.079(4) 0.104(5) -0.017(4) -0.006(4) 0.019(4) C22 0.123(6) 0.091(5) 0.164(8) -0.023(5) -0.003(6) 0.055(5) C23 0.133(7) 0.066(4) 0.158(8) 0.018(5) -0.003(6) 0.042(4) C24 0.082(4) 0.067(4) 0.073(4) 0.018(3) 0.001(3) 0.033(3) C25 0.141(6) 0.090(5) 0.071(4) 0.021(3) 0.011(4) 0.056(5) C26 0.128(6) 0.105(6) 0.106(6) 0.047(5) 0.028(5) 0.057(5) C27 0.093(5) 0.091(5) 0.145(7) 0.057(5) 0.039(5) 0.046(4) C28 0.074(4) 0.076(4) 0.112(6) 0.013(4) -0.005(4) 0.032(4) C29 0.076(4) 0.071(4) 0.074(4) 0.008(3) -0.003(3) 0.040(3) C30 0.090(4) 0.104(5) 0.074(4) -0.014(4) -0.007(4) 0.042(4) C31 0.084(4) 0.162(7) 0.076(5) -0.021(4) -0.008(4) 0.062(5) C32 0.115(6) 0.230(10) 0.115(7) 0.067(7) 0.053(5) 0.083(7) C33 0.146(8) 0.133(7) 0.151(8) 0.095(6) 0.026(7) 0.038(6) C34 0.107(5) 0.082(4) 0.116(6) -0.024(4) -0.031(5) 0.039(4) C35 0.079(4) 0.065(3) 0.086(4) -0.007(3) -0.006(3) 0.018(3) C36 0.067(3) 0.063(3) 0.044(3) 0.014(2) 0.015(2) 0.024(3) C37 0.065(4) 0.082(4) 0.064(3) 0.012(3) 0.013(3) 0.017(3) C38 0.065(4) 0.114(5) 0.083(4) 0.012(4) 0.017(3) 0.041(4) C39 0.094(5) 0.095(5) 0.090(4) 0.005(4) 0.015(4) 0.050(4) C40 0.085(4) 0.069(4) 0.067(3) 0.004(3) 0.002(3) 0.026(3) C41 0.069(3) 0.060(3) 0.047(3) 0.017(2) 0.010(2) 0.023(3) C42 0.077(4) 0.058(3) 0.059(3) 0.018(2) -0.004(3) 0.013(3) C43 0.075(4) 0.067(3) 0.058(3) 0.022(3) 0.009(3) 0.011(3) C44 0.068(4) 0.101(4) 0.086(4) 0.033(3) 0.032(3) 0.030(3) C45 0.085(4) 0.092(4) 0.094(5) 0.026(4) 0.018(3) 0.048(4) C46 0.101(5) 0.075(4) 0.096(5) -0.002(3) -0.029(4) 0.043(4) C47 0.107(5) 0.069(4) 0.072(4) 0.004(3) -0.012(4) 0.033(4) C48 0.133(7) 0.103(6) 0.118(7) 0.007(5) 0.060(6) 0.030(5) C49 0.177(13) 0.251(18) 0.73(5) -0.35(3) -0.24(2) 0.149(14) O1W 0.385(17) 0.280(11) 0.284(14) 0.080(10) 0.055(12) 0.140(12) O2W 0.269(14) 0.52(3) 0.39(2) -0.18(2) -0.022(13) 0.045(15) _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 S1 O14 1.402(4) . ? S1 O15 1.405(5) . ? S1 O13 1.434(5) . ? S1 C48 1.824(9) . ? S2 O17 1.368(6) . ? S2 O16 1.465(9) . ? S2 O18 1.479(8) . ? S2 C49 1.846(14) . ? F1 C48 1.334(9) . ? F2 C48 1.292(9) . ? F3 C48 1.293(9) . ? F4 C49 1.236(13) . ? F5 C49 1.52(4) . ? F6 C49 1.112(12) . ? O1 C17 1.399(8) . ? O1 C18 1.426(8) . ? O2 C20 1.393(7) . ? O2 C19 1.432(7) . ? O3 C21 1.401(7) . ? O3 C22 1.415(9) . ? O4 C12 1.331(9) . ? O4 C23 1.432(9) . ? O5 C29 1.359(7) . ? O5 C30 1.408(6) . ? O6 C32 1.388(9) . ? O6 C31 1.400(8) . ? O7 C33 1.296(10) . ? O7 C34 1.389(9) . ? O8 C36 1.372(6) . ? O8 C35 1.426(6) . ? O9 C41 1.364(6) . ? O9 C42 1.426(5) . ? O10 C44 1.412(6) . ? O10 C43 1.420(6) . ? O11 C45 1.402(7) . ? O11 C46 1.421(6) . ? O12 C24 1.360(7) . ? O12 C47 1.414(6) . ? N1 C5 1.311(7) . ? N1 C1 1.323(7) . ? N2 C9 1.339(6) . ? N2 C8 1.340(6) . ? N2 C11 1.478(5) . ? C1 C2 1.361(8) . ? C2 C3 1.384(7) . ? C3 C4 1.369(6) . ? C3 C6 1.483(6) . ? C4 C5 1.359(7) . ? C6 C7 1.371(6) . ? C6 C10 1.374(6) . ? C7 C8 1.363(7) . ? C9 C10 1.358(6) . ? C11 C11 1.491(9) 2_675 ? C12 C17 1.398(10) . ? C12 C13 1.416(10) . ? C13 C14 1.327(14) . ? C14 C15 1.327(14) . ? C15 C16 1.427(13) . ? C16 C17 1.364(10) . ? C18 C19 1.486(9) . ? C20 C21 1.451(9) . ? C22 C23 1.487(12) 2_655 ? C23 C22 1.487(12) 2_655 ? C24 C25 1.382(9) . ? C24 C29 1.397(8) . ? C25 C26 1.370(10) . ? C26 C27 1.330(10) . ? C27 C28 1.378(10) . ? C28 C29 1.387(8) . ? C30 C31 1.446(10) . ? C32 C33 1.411(11) . ? C34 C35 1.502(8) . ? C36 C37 1.376(7) . ? C36 C41 1.391(7) . ? C37 C38 1.380(8) . ? C38 C39 1.358(8) . ? C39 C40 1.394(8) . ? C40 C41 1.357(7) . ? C42 C43 1.473(7) . ? C44 C45 1.478(8) . ? C46 C47 1.467(9) . ? 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 O14 S1 O15 116.1(3) . . ? O14 S1 O13 113.8(3) . . ? O15 S1 O13 115.3(3) . . ? O14 S1 C48 102.2(4) . . ? O15 S1 C48 105.2(4) . . ? O13 S1 C48 101.5(4) . . ? O17 S2 O16 129.5(6) . . ? O17 S2 O18 110.5(6) . . ? O16 S2 O18 106.9(6) . . ? O17 S2 C49 106.3(6) . . ? O16 S2 C49 101.0(8) . . ? O18 S2 C49 97.6(13) . . ? C17 O1 C18 117.1(5) . . ? C20 O2 C19 115.0(5) . . ? C21 O3 C22 115.3(5) . . ? C12 O4 C23 116.1(6) . . ? C29 O5 C30 117.1(5) . . ? C32 O6 C31 111.2(6) . . ? C33 O7 C34 119.9(6) . . ? C36 O8 C35 118.2(4) . . ? C41 O9 C42 117.7(4) . . ? C44 O10 C43 112.9(4) . . ? C45 O11 C46 113.1(4) . . ? C24 O12 C47 118.9(5) . . ? C5 N1 C1 123.6(4) . . ? C9 N2 C8 120.7(4) . . ? C9 N2 C11 119.5(4) . . ? C8 N2 C11 119.8(4) . . ? N1 C1 C2 118.2(5) . . ? C1 C2 C3 120.7(5) . . ? C4 C3 C2 117.6(4) . . ? C4 C3 C6 121.6(4) . . ? C2 C3 C6 120.8(4) . . ? C5 C4 C3 120.2(5) . . ? N1 C5 C4 119.6(5) . . ? C7 C6 C10 117.0(4) . . ? C7 C6 C3 121.3(4) . . ? C10 C6 C3 121.8(4) . . ? C8 C7 C6 121.3(4) . . ? N2 C8 C7 119.8(4) . . ? N2 C9 C10 120.0(4) . . ? C9 C10 C6 121.2(4) . . ? N2 C11 C11 109.1(4) . 2_675 ? O4 C12 C17 118.2(6) . . ? O4 C12 C13 126.5(9) . . ? C17 C12 C13 115.2(9) . . ? C14 C13 C12 121.6(11) . . ? C15 C14 C13 122.9(13) . . ? C14 C15 C16 119.5(11) . . ? C17 C16 C15 117.5(10) . . ? C16 C17 O1 122.0(9) . . ? C16 C17 C12 123.3(8) . . ? O1 C17 C12 114.8(6) . . ? O1 C18 C19 108.8(5) . . ? O2 C19 C18 113.7(5) . . ? O2 C20 C21 111.3(5) . . ? O3 C21 C20 110.6(5) . . ? O3 C22 C23 115.1(7) . 2_655 ? O4 C23 C22 107.7(6) . 2_655 ? O12 C24 C25 125.8(6) . . ? O12 C24 C29 115.3(6) . . ? C25 C24 C29 118.9(6) . . ? C26 C25 C24 121.0(7) . . ? C27 C26 C25 120.3(8) . . ? C26 C27 C28 120.8(7) . . ? C27 C28 C29 120.4(6) . . ? O5 C29 C28 127.3(6) . . ? O5 C29 C24 114.1(5) . . ? C28 C29 C24 118.6(6) . . ? O5 C30 C31 107.9(6) . . ? O6 C31 C30 109.2(5) . . ? O6 C32 C33 114.5(7) . . ? O7 C33 C32 131.2(8) . . ? O7 C34 C35 112.5(6) . . ? O8 C35 C34 107.5(5) . . ? O8 C36 C37 123.9(5) . . ? O8 C36 C41 115.3(4) . . ? C37 C36 C41 120.8(5) . . ? C36 C37 C38 119.0(5) . . ? C39 C38 C37 120.7(5) . . ? C38 C39 C40 119.8(5) . . ? C41 C40 C39 120.5(5) . . ? C40 C41 O9 124.5(5) . . ? C40 C41 C36 119.1(5) . . ? O9 C41 C36 116.3(4) . . ? O9 C42 C43 108.0(4) . . ? O10 C43 C42 110.1(4) . . ? O10 C44 C45 110.6(5) . . ? O11 C45 C44 109.8(5) . . ? O11 C46 C47 114.5(5) . . ? O12 C47 C46 106.4(5) . . ? F2 C48 F3 109.0(9) . . ? F2 C48 F1 107.8(7) . . ? F3 C48 F1 107.6(7) . . ? F2 C48 S1 111.7(6) . . ? F3 C48 S1 111.4(6) . . ? F1 C48 S1 109.2(7) . . ? F6 C49 F4 117.8(16) . . ? F6 C49 F5 105(3) . . ? F4 C49 F5 101(2) . . ? F6 C49 S2 120.6(12) . . ? F4 C49 S2 116.1(11) . . ? F5 C49 S2 86.6(14) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.663 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.066 #===END