Supplementary Material (ESI) for Organic & Biomolecular Chemistry This journal is (c) The Royal Society of Chemistry 2005 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Stephen Loeb' _publ_contact_author_address ; Department of 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_coeditor_name ? _publ_contact_letter ; This structure is one of nine that are part of a study on the formation of [2]psedorotaxanes from 1,2-bis(pyridinium)ethane axles and 24-membered crown ether wheels. ; _publ_section_title ; A Versatile Template for [2]Pseudorotaxanes. 1,2-Bis(pyridinium)ethane Axles and 24-Crown-8 Ether Wheels ; loop_ _publ_author_name 'Stephen Loeb' 'Jorge Tiburcio' 'Sarah J. Vella' 'James A. Wisner' data_[2]pseudorotaxane_[(1,2-bis(4,4'-bipyridinium)ethane)-DB24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H58 B2 F8 N6 O12' _chemical_formula_weight 1084.62 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.5068(3) _cell_length_b 12.0843(3) _cell_length_c 21.5489(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.703(1) _cell_angle_gamma 90.00 _cell_volume 2669.0(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.201819 _exptl_absorpt_correction_T_max 0.492011 _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 'Bruker APEX 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 12655 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4624 _reflns_number_gt 2027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.1378P)^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 4624 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1768 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2529 _refine_ls_wR_factor_gt 0.2100 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _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 O1 O 0.3337(3) 0.5814(3) 0.50435(14) 0.0657(9) Uani 1 1 d . . . O2 O 0.2813(3) 0.4831(3) 0.62266(13) 0.0636(9) Uani 1 1 d . . . O3 O 0.0570(3) 0.5610(3) 0.65681(13) 0.0651(9) Uani 1 1 d . . . O4 O 0.1966(3) 0.5619(3) 0.38908(14) 0.0659(9) Uani 1 1 d . . . O5 O 0.3649(6) 0.2896(7) 0.3047(3) 0.187(3) Uani 1 1 d . . . O6 O 0.1761(4) 0.2515(3) 0.22343(18) 0.0883(12) Uani 1 1 d . . . N1 N 0.1842(5) 1.1930(4) 0.4209(3) 0.0830(13) Uani 1 1 d . . . N2 N -0.0021(3) 0.6539(3) 0.48881(16) 0.0489(9) Uani 1 1 d . . . N3 N 0.2907(6) 0.2695(4) 0.2365(2) 0.0963(15) Uani 1 1 d . . . C1 C 0.1067(7) 1.1313(5) 0.3780(3) 0.0941(18) Uani 1 1 d . . . H1A H 0.0749 1.1619 0.3380 0.113 Uiso 1 1 calc R . . C2 C 0.0695(5) 1.0241(4) 0.3885(2) 0.0752(15) Uani 1 1 d . . . H2A H 0.0135 0.9853 0.3564 0.090 Uiso 1 1 calc R . . C3 C 0.1164(4) 0.9753(4) 0.4469(2) 0.0485(11) Uani 1 1 d . . . C4 C 0.1997(4) 1.0387(4) 0.4912(2) 0.0620(13) Uani 1 1 d . . . H4A H 0.2358 1.0099 0.5312 0.074 Uiso 1 1 calc R . . C5 C 0.2296(5) 1.1457(5) 0.4759(3) 0.0716(14) Uani 1 1 d . . . H5A H 0.2858 1.1866 0.5069 0.086 Uiso 1 1 calc R . . C6 C 0.0782(4) 0.8628(4) 0.4606(2) 0.0470(11) Uani 1 1 d . . . C7 C -0.0037(4) 0.7983(4) 0.4159(2) 0.0568(12) Uani 1 1 d . . . H7A H -0.0331 0.8257 0.3749 0.068 Uiso 1 1 calc R . . C8 C -0.0423(4) 0.6959(4) 0.4302(2) 0.0563(12) Uani 1 1 d . . . H8A H -0.0973 0.6546 0.3990 0.068 Uiso 1 1 calc R . . C9 C 0.0790(4) 0.7125(4) 0.5335(2) 0.0548(12) Uani 1 1 d . . . H9A H 0.1083 0.6826 0.5739 0.066 Uiso 1 1 calc R . . C10 C 0.1186(4) 0.8142(4) 0.5204(2) 0.0566(12) Uani 1 1 d . . . H10A H 0.1747 0.8533 0.5523 0.068 Uiso 1 1 calc R . . C11 C -0.0483(4) 0.5441(3) 0.5034(2) 0.0577(12) Uani 1 1 d . . . H11A H -0.1314 0.5285 0.4748 0.069 Uiso 1 1 calc R . . H11B H -0.0616 0.5437 0.5466 0.069 Uiso 1 1 calc R . . C12 C 0.2710(4) 0.6547(4) 0.4015(2) 0.0565(12) Uani 1 1 d . . . C13 C 0.2771(5) 0.7361(5) 0.3574(2) 0.0696(14) Uani 1 1 d . . . H13A H 0.2300 0.7288 0.3157 0.084 Uiso 1 1 calc R . . C14 C 0.3536(5) 0.8284(5) 0.3755(3) 0.0785(16) Uani 1 1 d . . . H14A H 0.3574 0.8835 0.3459 0.094 Uiso 1 1 calc R . . C15 C 0.4235(5) 0.8396(5) 0.4362(3) 0.0777(15) Uani 1 1 d . . . H15A H 0.4747 0.9022 0.4476 0.093 Uiso 1 1 calc R . . C16 C 0.4193(5) 0.7595(5) 0.4808(3) 0.0700(14) Uani 1 1 d . . . H16A H 0.4664 0.7680 0.5224 0.084 Uiso 1 1 calc R . . C17 C 0.3441(4) 0.6657(4) 0.4632(2) 0.0574(12) Uani 1 1 d . . . C18 C 0.4222(4) 0.5813(4) 0.5642(2) 0.0693(14) Uani 1 1 d . . . H18A H 0.4091 0.6470 0.5879 0.083 Uiso 1 1 calc R . . H18B H 0.5111 0.5821 0.5583 0.083 Uiso 1 1 calc R . . C19 C 0.4004(4) 0.4806(4) 0.6002(2) 0.0686(14) Uani 1 1 d . . . H19A H 0.3990 0.4164 0.5730 0.082 Uiso 1 1 calc R . . H19B H 0.4732 0.4719 0.6364 0.082 Uiso 1 1 calc R . . C20 C 0.2884(4) 0.5459(4) 0.6783(2) 0.0644(13) Uani 1 1 d . . . H20A H 0.2987 0.6236 0.6693 0.077 Uiso 1 1 calc R . . H20B H 0.3636 0.5228 0.7105 0.077 Uiso 1 1 calc R . . C21 C 0.1661(5) 0.5299(5) 0.7028(2) 0.0702(14) Uani 1 1 d . . . H21A H 0.1584 0.4528 0.7140 0.084 Uiso 1 1 calc R . . H21B H 0.1710 0.5740 0.7408 0.084 Uiso 1 1 calc R . . C22 C -0.0607(5) 0.5644(5) 0.6793(2) 0.0768(15) Uani 1 1 d . . . H22A H -0.1183 0.6189 0.6547 0.092 Uiso 1 1 calc R . . H22B H -0.0401 0.5894 0.7232 0.092 Uiso 1 1 calc R . . C23 C 0.1315(5) 0.5418(5) 0.3238(2) 0.0744(15) Uani 1 1 d . . . H23A H 0.1949 0.5386 0.2973 0.089 Uiso 1 1 calc R . . H23B H 0.0708 0.6014 0.3085 0.089 Uiso 1 1 calc R . . C24 C 0.3717(6) 0.2748(5) 0.1875(3) 0.0983(19) Uani 1 1 d . . . H24A H 0.3179 0.2595 0.1463 0.147 Uiso 1 1 calc R . . H24B H 0.4404 0.2210 0.1972 0.147 Uiso 1 1 calc R . . H24C H 0.4088 0.3474 0.1875 0.147 Uiso 1 1 calc R . . B1 B 0.3228(10) 0.9134(7) 0.6818(4) 0.104(3) Uani 1 1 d . . . F1 F 0.4069(5) 0.9345(4) 0.73500(18) 0.1510(17) Uani 1 1 d . . . F2 F 0.2354(4) 0.9878(4) 0.6658(3) 0.178(2) Uani 1 1 d . . . F3 F 0.2661(9) 0.8187(5) 0.6865(3) 0.257(4) Uani 1 1 d . . . F4 F 0.3734(6) 0.8936(9) 0.6335(2) 0.263(5) 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 O1 0.0453(19) 0.087(2) 0.065(2) 0.0032(18) 0.0116(16) -0.0132(17) O2 0.0487(19) 0.080(2) 0.0631(18) -0.0052(17) 0.0152(15) -0.0099(17) O3 0.0485(19) 0.085(2) 0.0613(18) -0.0016(17) 0.0113(17) -0.0002(17) O4 0.0563(19) 0.084(2) 0.0610(19) 0.0020(17) 0.0202(16) -0.0129(19) O5 0.128(5) 0.279(8) 0.143(5) -0.008(5) 0.004(4) -0.010(5) O6 0.043(2) 0.114(3) 0.103(3) -0.006(2) 0.004(2) -0.014(2) N1 0.079(3) 0.071(3) 0.104(3) 0.012(3) 0.032(3) -0.011(3) N2 0.040(2) 0.052(2) 0.059(2) 0.001(2) 0.0196(18) 0.0000(18) N3 0.094(4) 0.090(4) 0.105(4) -0.008(3) 0.020(3) 0.002(3) C1 0.113(5) 0.082(5) 0.083(4) 0.019(4) 0.014(4) -0.012(4) C2 0.085(4) 0.065(4) 0.073(3) 0.006(3) 0.011(3) -0.011(3) C3 0.035(2) 0.050(3) 0.063(3) -0.002(2) 0.018(2) 0.001(2) C4 0.039(3) 0.065(3) 0.082(3) 0.011(3) 0.015(2) -0.002(2) C5 0.050(3) 0.068(4) 0.099(4) -0.006(3) 0.021(3) -0.013(3) C6 0.034(2) 0.054(3) 0.056(3) -0.001(2) 0.016(2) 0.004(2) C7 0.048(3) 0.066(3) 0.052(2) 0.003(2) 0.004(2) -0.007(3) C8 0.049(3) 0.063(3) 0.055(3) -0.004(2) 0.009(2) -0.012(2) C9 0.043(3) 0.065(3) 0.054(3) 0.006(2) 0.006(2) -0.005(2) C10 0.047(3) 0.064(3) 0.056(3) -0.009(2) 0.004(2) -0.007(3) C11 0.050(3) 0.057(3) 0.071(3) 0.003(2) 0.024(2) -0.012(2) C12 0.038(3) 0.068(3) 0.071(3) 0.003(3) 0.029(2) 0.001(2) C13 0.050(3) 0.091(4) 0.073(3) 0.007(3) 0.025(3) 0.002(3) C14 0.055(3) 0.086(4) 0.104(4) 0.021(4) 0.038(3) 0.001(3) C15 0.046(3) 0.080(4) 0.108(4) 0.000(4) 0.019(3) -0.010(3) C16 0.049(3) 0.085(4) 0.080(3) 0.003(3) 0.023(3) -0.008(3) C17 0.033(2) 0.075(4) 0.070(3) 0.000(3) 0.024(2) 0.001(2) C18 0.039(3) 0.098(4) 0.071(3) 0.003(3) 0.012(3) -0.010(3) C19 0.048(3) 0.089(4) 0.070(3) 0.000(3) 0.016(3) 0.002(3) C20 0.047(3) 0.075(3) 0.069(3) -0.010(3) 0.007(2) -0.002(2) C21 0.063(3) 0.094(4) 0.052(3) -0.004(3) 0.011(3) 0.003(3) C22 0.063(3) 0.094(4) 0.079(3) -0.023(3) 0.028(3) 0.003(3) C23 0.063(3) 0.101(4) 0.065(3) -0.006(3) 0.028(3) -0.004(3) C24 0.087(4) 0.113(5) 0.112(4) -0.006(4) 0.059(4) 0.004(4) B1 0.121(7) 0.070(5) 0.103(6) -0.020(4) -0.016(6) 0.016(5) F1 0.159(4) 0.162(4) 0.104(3) -0.020(3) -0.032(3) 0.008(3) F2 0.109(3) 0.113(3) 0.278(6) 0.000(4) -0.030(4) 0.025(3) F3 0.368(10) 0.107(4) 0.228(6) 0.017(4) -0.079(7) -0.062(5) F4 0.162(5) 0.524(14) 0.106(3) -0.041(5) 0.032(3) 0.104(7) _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 O1 C17 1.371(5) . ? O1 C18 1.415(5) . ? O2 C20 1.407(5) . ? O2 C19 1.438(5) . ? O3 C21 1.393(5) . ? O3 C22 1.424(5) . ? O4 C12 1.359(5) . ? O4 C23 1.443(5) . ? O5 N3 1.524(7) . ? O6 N3 1.194(6) . ? N1 C5 1.309(6) . ? N1 C1 1.319(7) . ? N2 C9 1.339(5) . ? N2 C8 1.340(5) . ? N2 C11 1.471(5) . ? N3 C24 1.497(7) . ? C1 C2 1.387(8) . ? C2 C3 1.379(6) . ? C3 C4 1.378(6) . ? C3 C6 1.466(6) . ? C4 C5 1.387(7) . ? C6 C7 1.383(6) . ? C6 C10 1.395(6) . ? C7 C8 1.358(6) . ? C9 C10 1.348(6) . ? C11 C11 1.501(9) 3_566 ? C12 C13 1.380(6) . ? C12 C17 1.388(6) . ? C13 C14 1.380(7) . ? C14 C15 1.358(7) . ? C15 C16 1.372(7) . ? C16 C17 1.386(7) . ? C18 C19 1.488(6) . ? C20 C21 1.504(6) . ? C22 C23 1.478(7) 3_566 ? C23 C22 1.478(7) 3_566 ? B1 F2 1.278(8) . ? B1 F4 1.292(10) . ? B1 F1 1.309(8) . ? B1 F3 1.305(10) . ? 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 C17 O1 C18 117.4(4) . . ? C20 O2 C19 114.3(3) . . ? C21 O3 C22 113.9(3) . . ? C12 O4 C23 117.4(4) . . ? C5 N1 C1 115.7(5) . . ? C9 N2 C8 119.8(4) . . ? C9 N2 C11 120.7(4) . . ? C8 N2 C11 119.5(4) . . ? O6 N3 C24 122.8(5) . . ? O6 N3 O5 122.1(5) . . ? C24 N3 O5 115.1(5) . . ? N1 C1 C2 124.6(5) . . ? C3 C2 C1 119.4(5) . . ? C4 C3 C2 116.1(4) . . ? C4 C3 C6 122.4(4) . . ? C2 C3 C6 121.4(4) . . ? C3 C4 C5 119.8(4) . . ? N1 C5 C4 124.5(5) . . ? C7 C6 C10 115.0(4) . . ? C7 C6 C3 122.6(4) . . ? C10 C6 C3 122.3(4) . . ? C8 C7 C6 121.8(4) . . ? N2 C8 C7 120.7(4) . . ? N2 C9 C10 120.6(4) . . ? C9 C10 C6 122.1(4) . . ? N2 C11 C11 110.9(4) . 3_566 ? O4 C12 C13 124.4(5) . . ? O4 C12 C17 116.2(4) . . ? C13 C12 C17 119.5(5) . . ? C14 C13 C12 119.6(5) . . ? C15 C14 C13 120.8(5) . . ? C14 C15 C16 120.7(5) . . ? C15 C16 C17 119.3(5) . . ? O1 C17 C16 123.6(4) . . ? O1 C17 C12 116.3(4) . . ? C16 C17 C12 120.2(5) . . ? O1 C18 C19 109.3(4) . . ? O2 C19 C18 113.7(4) . . ? O2 C20 C21 109.9(4) . . ? O3 C21 C20 110.4(4) . . ? O3 C22 C23 115.2(4) . 3_566 ? O4 C23 C22 108.5(4) . 3_566 ? F2 B1 F4 108.1(8) . . ? F2 B1 F1 114.0(7) . . ? F4 B1 F1 115.0(9) . . ? F2 B1 F3 109.0(9) . . ? F4 B1 F3 100.1(8) . . ? F1 B1 F3 109.6(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.523 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.065 # Attachment 'New-L2.cif' data_[2]pseudorotaxane_[(1,2-bis(4,4'-bipyridinium)ethane)-DN24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H62 B2 F8 N6 O12' _chemical_formula_weight 1184.74 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2482(7) _cell_length_b 37.030(2) _cell_length_c 13.0751(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.498(2) _cell_angle_gamma 90.00 _cell_volume 5517.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.905246 _exptl_absorpt_correction_T_max 1.000000 _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 'Bruker APEX 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 18652 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 20.81 _reflns_number_total 5635 _reflns_number_gt 4040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.0301P)^2^+45.0171P] 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 5635 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.1121 _refine_ls_wR_factor_ref 0.2335 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 O1 O 0.4911(5) 0.04586(16) 0.2329(5) 0.0385(16) Uani 1 1 d . . . O2 O 0.5144(5) 0.07040(16) 0.0270(5) 0.0407(17) Uani 1 1 d . . . O3 O 0.3787(6) 0.12398(16) -0.1180(5) 0.0426(17) Uani 1 1 d . . . O4 O 0.2355(5) 0.18739(15) -0.1384(4) 0.0316(15) Uani 1 1 d . . . O5 O 0.1253(5) 0.20573(15) -0.0117(5) 0.0341(15) Uani 1 1 d . . . O6 O 0.0683(5) 0.15957(16) 0.1497(5) 0.0405(17) Uani 1 1 d . . . O7 O 0.2408(6) 0.13685(17) 0.3473(5) 0.0490(18) Uani 1 1 d . . . O8 O 0.4122(6) 0.0791(2) 0.3667(5) 0.0541(19) Uani 1 1 d . . . O9 O 0.7324(8) -0.0481(3) 0.3590(7) 0.086(3) Uani 1 1 d . . . O10 O 0.7942(7) -0.0504(2) 0.2283(6) 0.071(2) Uani 1 1 d . . . O11 O 0.7227(13) 0.1671(5) -0.1426(12) 0.190(7) Uani 1 1 d . . . O12 O 0.6081(10) 0.1856(3) -0.0723(9) 0.113(4) Uani 1 1 d . . . N1 N 0.4702(7) 0.3626(2) 0.1372(7) 0.047(2) Uani 1 1 d . . . N2 N 0.4092(6) 0.17376(17) 0.1496(6) 0.0265(18) Uani 1 1 d . . . N3 N 0.2340(6) 0.08830(17) 0.0777(6) 0.0241(17) Uani 1 1 d . . . N4 N 0.0513(6) -0.09168(19) 0.0928(6) 0.0337(19) Uani 1 1 d . . . N5 N 0.8109(8) -0.0477(2) 0.3247(7) 0.048(2) Uani 1 1 d . . . N6 N 0.6482(11) 0.1877(3) -0.1405(10) 0.088(3) Uani 1 1 d . . . C1 C 0.4542(9) 0.3454(3) 0.2207(9) 0.052(3) Uani 1 1 d . . . H1A H 0.4522 0.3592 0.2794 0.063 Uiso 1 1 calc R . . C2 C 0.4406(8) 0.3088(2) 0.2251(8) 0.037(2) Uani 1 1 d . . . H2A H 0.4298 0.2984 0.2854 0.044 Uiso 1 1 calc R . . C3 C 0.4429(7) 0.2875(2) 0.1395(7) 0.022(2) Uani 1 1 d . . . C4 C 0.4578(7) 0.3048(2) 0.0523(7) 0.031(2) Uani 1 1 d . . . H4A H 0.4595 0.2917 -0.0077 0.038 Uiso 1 1 calc R . . C5 C 0.4702(8) 0.3422(3) 0.0548(9) 0.043(3) Uani 1 1 d . . . H5A H 0.4790 0.3534 -0.0054 0.052 Uiso 1 1 calc R . . C6 C 0.4322(7) 0.2477(2) 0.1438(7) 0.025(2) Uani 1 1 d . . . C7 C 0.3818(7) 0.2312(2) 0.2104(7) 0.034(2) Uani 1 1 d . . . H7A H 0.3535 0.2454 0.2538 0.040 Uiso 1 1 calc R . . C8 C 0.3723(7) 0.1947(2) 0.2142(7) 0.033(2) Uani 1 1 d . . . H8A H 0.3402 0.1843 0.2615 0.040 Uiso 1 1 calc R . . C9 C 0.4589(7) 0.1887(2) 0.0842(7) 0.029(2) Uani 1 1 d . . . H9A H 0.4844 0.1739 0.0401 0.035 Uiso 1 1 calc R . . C10 C 0.4730(7) 0.2248(2) 0.0808(7) 0.025(2) Uani 1 1 d . . . H10A H 0.5100 0.2345 0.0363 0.030 Uiso 1 1 calc R . . C11 C 0.3882(8) 0.1343(2) 0.1471(7) 0.033(2) Uani 1 1 d . . . H11A H 0.3992 0.1258 0.2203 0.040 Uiso 1 1 calc R . . H11B H 0.4436 0.1219 0.1222 0.040 Uiso 1 1 calc R . . C12 C 0.2654(7) 0.1266(2) 0.0705(7) 0.033(2) Uani 1 1 d . . . H12A H 0.2112 0.1421 0.0888 0.040 Uiso 1 1 calc R . . H12B H 0.2582 0.1321 -0.0043 0.040 Uiso 1 1 calc R . . C13 C 0.1830(7) 0.0789(2) 0.1483(7) 0.030(2) Uani 1 1 d . . . H13A H 0.1698 0.0964 0.1934 0.037 Uiso 1 1 calc R . . C14 C 0.1501(8) 0.0442(2) 0.1553(7) 0.029(2) Uani 1 1 d . . . H14A H 0.1150 0.0381 0.2051 0.034 Uiso 1 1 calc R . . C15 C 0.1691(7) 0.0179(2) 0.0878(6) 0.023(2) Uani 1 1 d . . . C16 C 0.2213(8) 0.0287(2) 0.0155(8) 0.037(2) Uani 1 1 d . . . H16A H 0.2341 0.0117 -0.0315 0.045 Uiso 1 1 calc R . . C17 C 0.2549(8) 0.0638(2) 0.0115(7) 0.033(2) Uani 1 1 d . . . H17A H 0.2916 0.0705 -0.0365 0.040 Uiso 1 1 calc R . . C18 C 0.1294(7) -0.0203(2) 0.0905(6) 0.022(2) Uani 1 1 d . . . C19 C 0.0811(8) -0.0314(2) 0.1640(8) 0.039(2) Uani 1 1 d . . . H19A H 0.0731 -0.0152 0.2152 0.047 Uiso 1 1 calc R . . C20 C 0.0440(9) -0.0668(3) 0.1623(8) 0.043(3) Uani 1 1 d . . . H20A H 0.0117 -0.0736 0.2137 0.052 Uiso 1 1 calc R . . C21 C 0.1007(9) -0.0808(2) 0.0251(8) 0.044(3) Uani 1 1 d . . . H21A H 0.1107 -0.0978 -0.0231 0.053 Uiso 1 1 calc R . . C22 C 0.1394(8) -0.0461(2) 0.0194(7) 0.037(2) Uani 1 1 d . . . H22A H 0.1721 -0.0403 -0.0324 0.044 Uiso 1 1 calc R . . C23 C 0.4013(8) 0.0420(3) 0.3631(8) 0.040(3) Uani 1 1 d . . . C24 C 0.3509(8) 0.0234(3) 0.4223(8) 0.045(3) Uani 1 1 d . . . H24A H 0.3265 0.0357 0.4723 0.054 Uiso 1 1 calc R . . C25 C 0.3342(8) -0.0141(3) 0.4103(8) 0.049(3) Uani 1 1 d . . . C26 C 0.2774(9) -0.0343(4) 0.4669(9) 0.061(3) Uani 1 1 d . . . H26A H 0.2522 -0.0230 0.5179 0.073 Uiso 1 1 calc R . . C27 C 0.2588(9) -0.0703(4) 0.4477(9) 0.064(4) Uani 1 1 d . . . H27A H 0.2197 -0.0832 0.4850 0.077 Uiso 1 1 calc R . . C28 C 0.2970(10) -0.0884(3) 0.3737(9) 0.060(3) Uani 1 1 d . . . H28A H 0.2827 -0.1130 0.3618 0.072 Uiso 1 1 calc R . . C29 C 0.3551(9) -0.0704(3) 0.3184(9) 0.053(3) Uani 1 1 d . . . H29A H 0.3808 -0.0825 0.2692 0.063 Uiso 1 1 calc R . . C30 C 0.3759(8) -0.0331(3) 0.3367(8) 0.046(3) Uani 1 1 d . . . C31 C 0.4314(8) -0.0119(3) 0.2783(7) 0.041(3) Uani 1 1 d . . . H31A H 0.4611 -0.0234 0.2309 0.049 Uiso 1 1 calc R . . C32 C 0.4424(8) 0.0247(3) 0.2894(8) 0.037(2) Uani 1 1 d . . . C33 C 0.5520(8) 0.0283(3) 0.1731(8) 0.040(3) Uani 1 1 d . . . H33A H 0.4984 0.0129 0.1170 0.048 Uiso 1 1 calc R . . H33B H 0.6139 0.0132 0.2223 0.048 Uiso 1 1 calc R . . C34 C 0.6029(8) 0.0555(3) 0.1214(8) 0.042(3) Uani 1 1 d . . . H34A H 0.6391 0.0745 0.1737 0.050 Uiso 1 1 calc R . . H34B H 0.6632 0.0444 0.1002 0.050 Uiso 1 1 calc R . . C35 C 0.5623(8) 0.0937(3) -0.0319(8) 0.043(3) Uani 1 1 d . . . H35A H 0.6249 0.0815 -0.0469 0.052 Uiso 1 1 calc R . . H35B H 0.5946 0.1151 0.0113 0.052 Uiso 1 1 calc R . . C36 C 0.4670(8) 0.1041(2) -0.1374(8) 0.039(2) Uani 1 1 d . . . H36A H 0.4999 0.1184 -0.1812 0.047 Uiso 1 1 calc R . . H36B H 0.4331 0.0824 -0.1786 0.047 Uiso 1 1 calc R . . C37 C 0.2867(9) 0.1354(2) -0.2165(7) 0.041(3) Uani 1 1 d . . . H37A H 0.2128 0.1252 -0.2188 0.049 Uiso 1 1 calc R . . H37B H 0.3020 0.1265 -0.2797 0.049 Uiso 1 1 calc R . . C38 C 0.2770(8) 0.1757(2) -0.2225(7) 0.037(2) Uani 1 1 d . . . H38A H 0.3530 0.1864 -0.2108 0.044 Uiso 1 1 calc R . . H38B H 0.2226 0.1831 -0.2942 0.044 Uiso 1 1 calc R . . C39 C 0.2154(8) 0.2242(2) -0.1371(7) 0.034(2) Uani 1 1 d . . . C40 C 0.2432(7) 0.2493(2) -0.1957(7) 0.031(2) Uani 1 1 d . . . H40A H 0.2781 0.2425 -0.2450 0.037 Uiso 1 1 calc R . . C41 C 0.2212(8) 0.2859(2) -0.1849(7) 0.033(2) Uani 1 1 d . . . C42 C 0.2511(8) 0.3129(3) -0.2447(8) 0.046(3) Uani 1 1 d . . . H42A H 0.2848 0.3061 -0.2950 0.056 Uiso 1 1 calc R . . C43 C 0.2332(9) 0.3486(3) -0.2325(9) 0.051(3) Uani 1 1 d . . . H43A H 0.2570 0.3659 -0.2715 0.061 Uiso 1 1 calc R . . C44 C 0.1788(9) 0.3589(3) -0.1608(9) 0.052(3) Uani 1 1 d . . . H44A H 0.1644 0.3832 -0.1532 0.062 Uiso 1 1 calc R . . C45 C 0.1459(8) 0.3336(3) -0.1011(8) 0.048(3) Uani 1 1 d . . . H45A H 0.1100 0.3409 -0.0531 0.058 Uiso 1 1 calc R . . C46 C 0.1662(8) 0.2962(2) -0.1120(8) 0.036(2) Uani 1 1 d . . . C47 C 0.1341(8) 0.2693(2) -0.0531(7) 0.033(2) Uani 1 1 d . . . H47A H 0.0961 0.2758 -0.0060 0.039 Uiso 1 1 calc R . . C48 C 0.1575(8) 0.2336(2) -0.0634(7) 0.031(2) Uani 1 1 d . . . C49 C 0.0382(8) 0.2131(2) 0.0333(8) 0.038(2) Uani 1 1 d . . . H49A H -0.0246 0.2272 -0.0183 0.045 Uiso 1 1 calc R . . H49B H 0.0722 0.2269 0.1006 0.045 Uiso 1 1 calc R . . C50 C -0.0098(9) 0.1781(3) 0.0570(9) 0.049(3) Uani 1 1 d . . . H50A H -0.0821 0.1830 0.0690 0.059 Uiso 1 1 calc R . . H50B H -0.0289 0.1626 -0.0069 0.059 Uiso 1 1 calc R . . C51 C 0.0819(8) 0.1757(3) 0.2515(8) 0.045(3) Uani 1 1 d . . . H51A H 0.0071 0.1849 0.2499 0.054 Uiso 1 1 calc R . . H51B H 0.1366 0.1957 0.2661 0.054 Uiso 1 1 calc R . . C52 C 0.1268(10) 0.1481(3) 0.3380(9) 0.055(3) Uani 1 1 d . . . H52A H 0.1296 0.1579 0.4077 0.066 Uiso 1 1 calc R . . H52B H 0.0743 0.1275 0.3203 0.066 Uiso 1 1 calc R . . C53 C 0.2819(13) 0.1100(4) 0.4342(9) 0.082(4) Uani 1 1 d . . . H53A H 0.2773 0.1199 0.5012 0.099 Uiso 1 1 calc R . . H53B H 0.2311 0.0890 0.4138 0.099 Uiso 1 1 calc R . . C54 C 0.3949(10) 0.0996(4) 0.4534(9) 0.070(4) Uani 1 1 d . . . H54A H 0.4225 0.0853 0.5201 0.084 Uiso 1 1 calc R . . H54B H 0.4433 0.1211 0.4666 0.084 Uiso 1 1 calc R . . C55 C 0.9336(10) -0.0446(3) 0.4035(8) 0.063(3) Uani 1 1 d . . . H55A H 0.9340 -0.0422 0.4767 0.095 Uiso 1 1 calc R . . H55B H 0.9697 -0.0238 0.3856 0.095 Uiso 1 1 calc R . . H55C H 0.9766 -0.0659 0.3992 0.095 Uiso 1 1 calc R . . C56 C 0.6081(15) 0.2144(5) -0.2232(14) 0.171(10) Uani 1 1 d . . . H56A H 0.5494 0.2290 -0.2106 0.257 Uiso 1 1 calc R . . H56B H 0.5749 0.2030 -0.2938 0.257 Uiso 1 1 calc R . . H56C H 0.6726 0.2294 -0.2214 0.257 Uiso 1 1 calc R . . B1 B 0.9169(11) 0.0555(4) 0.2962(11) 0.048(3) Uani 1 1 d . . . B2 B 0.8000(13) 0.2755(4) 0.0224(11) 0.059(4) Uani 1 1 d . . . F1 F 0.8921(6) 0.08029(17) 0.2149(5) 0.075(2) Uani 1 1 d . . . F2 F 0.8715(9) 0.0597(4) 0.3644(7) 0.220(8) Uani 1 1 d . . . F3 F 0.8640(9) 0.0244(2) 0.2344(9) 0.162(5) Uani 1 1 d . . . F4 F 1.0301(6) 0.0452(2) 0.3360(5) 0.088(2) Uani 1 1 d . . . F5 F 0.8530(10) 0.3083(3) 0.0616(8) 0.152(4) Uani 1 1 d . . . F6 F 0.6859(7) 0.2787(3) 0.0053(7) 0.119(3) Uani 1 1 d . . . F7 F 0.8115(7) 0.2696(2) -0.0755(5) 0.107(3) Uani 1 1 d . . . F8 F 0.8557(6) 0.2510(2) 0.0999(6) 0.093(2) 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 O1 0.040(4) 0.040(4) 0.042(4) 0.006(3) 0.023(3) 0.006(3) O2 0.036(4) 0.040(4) 0.048(4) 0.013(3) 0.017(4) 0.009(3) O3 0.058(4) 0.039(4) 0.033(4) 0.000(3) 0.019(4) 0.022(4) O4 0.035(4) 0.030(4) 0.031(4) 0.003(3) 0.013(3) 0.007(3) O5 0.046(4) 0.025(3) 0.039(4) 0.003(3) 0.024(3) 0.002(3) O6 0.052(4) 0.039(4) 0.037(4) -0.004(3) 0.024(4) 0.004(3) O7 0.075(5) 0.037(4) 0.035(4) 0.005(3) 0.019(4) 0.015(4) O8 0.058(5) 0.061(5) 0.041(4) -0.012(4) 0.015(4) 0.016(4) O9 0.074(6) 0.130(8) 0.070(6) -0.014(5) 0.045(5) 0.009(6) O10 0.087(6) 0.092(6) 0.035(5) -0.017(4) 0.022(4) -0.016(5) O11 0.140(12) 0.259(18) 0.181(14) -0.019(12) 0.072(11) 0.082(12) O12 0.167(11) 0.095(7) 0.123(9) -0.004(6) 0.108(9) -0.036(7) N1 0.064(6) 0.025(5) 0.058(6) -0.006(5) 0.029(5) -0.002(4) N2 0.033(4) 0.017(4) 0.027(4) -0.003(4) 0.009(4) 0.002(3) N3 0.028(4) 0.014(4) 0.030(4) -0.004(4) 0.011(4) -0.002(3) N4 0.044(5) 0.025(4) 0.032(5) 0.004(4) 0.014(4) 0.002(4) N5 0.070(7) 0.041(5) 0.039(6) -0.004(4) 0.027(6) 0.005(5) N6 0.072(9) 0.108(10) 0.090(9) 0.012(8) 0.037(7) 0.008(7) C1 0.060(8) 0.046(8) 0.057(8) -0.007(6) 0.029(6) 0.011(6) C2 0.040(6) 0.028(6) 0.042(6) -0.003(5) 0.015(5) 0.000(5) C3 0.021(5) 0.014(5) 0.032(6) 0.002(4) 0.012(4) 0.006(4) C4 0.031(6) 0.022(6) 0.040(6) 0.004(5) 0.012(5) -0.002(4) C5 0.043(6) 0.032(7) 0.057(7) 0.014(6) 0.021(5) 0.006(5) C6 0.019(5) 0.028(5) 0.023(5) -0.003(4) 0.004(4) 0.002(4) C7 0.035(6) 0.037(6) 0.037(6) -0.006(5) 0.022(5) -0.003(5) C8 0.028(6) 0.027(6) 0.042(6) 0.001(5) 0.011(5) 0.001(4) C9 0.039(6) 0.030(6) 0.022(5) -0.002(4) 0.016(5) -0.002(5) C10 0.022(5) 0.023(6) 0.031(5) 0.002(4) 0.011(4) -0.006(4) C11 0.039(6) 0.023(5) 0.040(6) 0.002(4) 0.018(5) 0.006(4) C12 0.033(6) 0.023(5) 0.040(6) 0.002(4) 0.008(5) 0.005(4) C13 0.043(6) 0.017(5) 0.039(6) -0.007(4) 0.024(5) 0.001(4) C14 0.045(6) 0.022(6) 0.027(5) 0.000(4) 0.023(5) 0.002(5) C15 0.027(5) 0.019(5) 0.022(5) 0.014(4) 0.008(4) 0.003(4) C16 0.057(7) 0.022(6) 0.043(6) -0.008(5) 0.031(6) -0.004(5) C17 0.042(6) 0.030(6) 0.028(6) -0.008(5) 0.013(5) -0.003(5) C18 0.029(5) 0.021(5) 0.017(5) -0.005(4) 0.010(4) 0.006(4) C19 0.051(7) 0.031(6) 0.039(6) -0.001(5) 0.021(5) -0.005(5) C20 0.060(7) 0.036(6) 0.050(7) 0.006(5) 0.038(6) -0.001(5) C21 0.059(7) 0.026(6) 0.057(7) -0.009(5) 0.032(6) -0.006(5) C22 0.046(6) 0.037(6) 0.032(6) -0.007(5) 0.019(5) -0.009(5) C23 0.031(6) 0.045(7) 0.042(6) 0.004(6) 0.010(5) 0.002(5) C24 0.035(6) 0.058(8) 0.047(7) 0.003(6) 0.019(5) 0.013(6) C25 0.029(6) 0.076(9) 0.037(6) 0.026(6) 0.007(5) 0.012(6) C26 0.043(7) 0.086(10) 0.050(8) 0.009(7) 0.013(6) 0.006(7) C27 0.045(7) 0.099(11) 0.048(8) 0.036(8) 0.015(6) 0.011(7) C28 0.062(8) 0.051(7) 0.063(8) 0.022(6) 0.018(7) -0.004(6) C29 0.044(7) 0.056(8) 0.059(8) 0.018(6) 0.020(6) 0.005(6) C30 0.033(6) 0.071(8) 0.032(6) 0.015(6) 0.009(5) 0.014(6) C31 0.039(6) 0.053(8) 0.031(6) 0.002(5) 0.014(5) 0.012(5) C32 0.037(6) 0.042(7) 0.035(6) 0.001(5) 0.016(5) 0.009(5) C33 0.039(6) 0.045(6) 0.041(6) 0.005(5) 0.019(5) 0.008(5) C34 0.040(6) 0.041(6) 0.052(7) 0.009(5) 0.027(6) 0.008(5) C35 0.039(6) 0.038(6) 0.055(7) 0.001(5) 0.019(6) -0.003(5) C36 0.050(7) 0.032(6) 0.044(6) 0.001(5) 0.027(6) 0.008(5) C37 0.054(7) 0.037(6) 0.024(6) -0.001(5) 0.004(5) 0.010(5) C38 0.049(6) 0.035(6) 0.037(6) 0.003(5) 0.027(5) 0.002(5) C39 0.036(6) 0.031(6) 0.031(6) 0.004(5) 0.009(5) 0.003(5) C40 0.033(6) 0.031(6) 0.035(6) 0.001(5) 0.020(5) 0.002(4) C41 0.033(6) 0.022(6) 0.036(6) 0.002(5) 0.004(5) -0.001(4) C42 0.034(6) 0.043(7) 0.052(7) 0.003(6) 0.003(5) 0.006(5) C43 0.058(7) 0.036(7) 0.053(7) 0.005(6) 0.013(6) -0.021(6) C44 0.059(7) 0.016(6) 0.061(8) 0.014(6) -0.002(6) -0.001(5) C45 0.045(7) 0.039(7) 0.046(7) -0.005(5) 0.000(5) 0.011(5) C46 0.033(6) 0.025(6) 0.042(6) -0.002(5) 0.003(5) 0.002(5) C47 0.039(6) 0.025(6) 0.038(6) -0.007(5) 0.018(5) -0.002(5) C48 0.036(6) 0.024(6) 0.023(5) 0.001(4) 0.001(5) -0.002(5) C49 0.037(6) 0.034(6) 0.050(7) 0.001(5) 0.024(5) 0.003(5) C50 0.046(7) 0.044(6) 0.056(7) 0.000(6) 0.018(6) 0.003(6) C51 0.035(6) 0.047(7) 0.057(7) -0.010(6) 0.021(5) 0.004(5) C52 0.079(9) 0.050(7) 0.054(7) -0.004(6) 0.045(7) 0.001(6) C53 0.128(13) 0.090(10) 0.028(7) -0.005(7) 0.029(8) 0.032(9) C54 0.057(8) 0.110(11) 0.034(7) -0.006(7) 0.007(6) 0.016(8) C55 0.066(9) 0.073(8) 0.043(7) 0.005(6) 0.012(7) 0.011(7) C56 0.145(16) 0.181(19) 0.125(15) 0.111(15) -0.024(12) -0.056(14) B1 0.030(8) 0.060(9) 0.058(9) 0.010(8) 0.021(7) -0.007(7) B2 0.056(10) 0.075(11) 0.049(9) 0.025(8) 0.022(7) 0.021(8) F1 0.117(6) 0.060(4) 0.055(4) 0.003(4) 0.041(4) 0.005(4) F2 0.177(9) 0.44(2) 0.092(7) 0.148(10) 0.111(7) 0.222(12) F3 0.145(9) 0.085(6) 0.190(11) 0.055(7) -0.017(8) -0.017(6) F4 0.060(5) 0.154(7) 0.056(4) 0.005(4) 0.029(4) 0.023(5) F5 0.211(11) 0.107(8) 0.107(7) 0.022(6) 0.022(7) -0.027(8) F6 0.084(6) 0.180(9) 0.118(7) 0.045(6) 0.065(5) 0.058(6) F7 0.109(6) 0.170(8) 0.058(5) 0.038(5) 0.050(4) 0.075(6) F8 0.108(6) 0.114(6) 0.074(5) 0.043(5) 0.053(5) 0.055(5) _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 O1 C32 1.358(10) . ? O1 C33 1.421(10) . ? O2 C35 1.419(10) . ? O2 C34 1.422(10) . ? O3 C36 1.407(10) . ? O3 C37 1.429(10) . ? O4 C39 1.387(10) . ? O4 C38 1.437(10) . ? O5 C48 1.369(10) . ? O5 C49 1.420(10) . ? O6 C51 1.412(10) . ? O6 C50 1.417(11) . ? O7 C52 1.418(11) . ? O7 C53 1.454(13) . ? O8 C23 1.380(11) . ? O8 C54 1.444(12) . ? O9 N5 1.200(10) . ? O10 N5 1.204(10) . ? O11 N6 1.198(14) . ? O12 N6 1.168(13) . ? N1 C5 1.317(12) . ? N1 C1 1.339(12) . ? N2 C9 1.337(10) . ? N2 C8 1.342(10) . ? N2 C11 1.481(10) . ? N3 C13 1.335(10) . ? N3 C17 1.342(10) . ? N3 C12 1.483(10) . ? N4 C21 1.305(11) . ? N4 C20 1.319(11) . ? N5 C55 1.483(13) . ? N6 C56 1.413(17) . ? C1 C2 1.369(13) . ? C2 C3 1.379(12) . ? C3 C4 1.377(11) . ? C3 C6 1.482(11) . ? C4 C5 1.390(12) . ? C6 C7 1.381(11) . ? C6 C10 1.396(11) . ? C7 C8 1.357(12) . ? C9 C10 1.352(11) . ? C11 C12 1.497(12) . ? C13 C14 1.360(11) . ? C14 C15 1.392(11) . ? C15 C16 1.380(11) . ? C15 C18 1.499(11) . ? C16 C17 1.371(12) . ? C18 C19 1.364(11) . ? C18 C22 1.369(11) . ? C19 C20 1.386(12) . ? C21 C22 1.383(12) . ? C23 C24 1.344(13) . ? C23 C32 1.396(13) . ? C24 C25 1.405(14) . ? C25 C26 1.404(14) . ? C25 C30 1.428(14) . ? C26 C27 1.362(16) . ? C27 C28 1.391(15) . ? C28 C29 1.359(14) . ? C29 C30 1.409(14) . ? C30 C31 1.430(13) . ? C31 C32 1.361(13) . ? C33 C34 1.472(12) . ? C35 C36 1.494(12) . ? C37 C38 1.497(12) . ? C39 C40 1.325(12) . ? C39 C48 1.434(12) . ? C40 C41 1.397(12) . ? C41 C42 1.399(13) . ? C41 C46 1.407(12) . ? C42 C43 1.361(13) . ? C43 C44 1.387(14) . ? C44 C45 1.372(14) . ? C45 C46 1.422(13) . ? C46 C47 1.402(12) . ? C47 C48 1.368(12) . ? C49 C50 1.499(12) . ? C51 C52 1.475(13) . ? C53 C54 1.368(15) . ? B1 F2 1.222(14) . ? B1 F4 1.346(13) . ? B1 F1 1.351(13) . ? B1 F3 1.420(15) . ? B2 F6 1.338(15) . ? B2 F8 1.344(14) . ? B2 F7 1.355(14) . ? B2 F5 1.386(17) . ? 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 C32 O1 C33 117.4(7) . . ? C35 O2 C34 111.8(7) . . ? C36 O3 C37 113.5(7) . . ? C39 O4 C38 114.7(6) . . ? C48 O5 C49 117.2(7) . . ? C51 O6 C50 114.2(7) . . ? C52 O7 C53 108.3(8) . . ? C23 O8 C54 120.7(9) . . ? C5 N1 C1 116.0(8) . . ? C9 N2 C8 120.0(7) . . ? C9 N2 C11 120.6(7) . . ? C8 N2 C11 119.3(7) . . ? C13 N3 C17 121.2(7) . . ? C13 N3 C12 119.4(7) . . ? C17 N3 C12 119.4(7) . . ? C21 N4 C20 114.6(8) . . ? O9 N5 O10 122.5(10) . . ? O9 N5 C55 119.2(9) . . ? O10 N5 C55 118.3(9) . . ? O12 N6 O11 120.9(15) . . ? O12 N6 C56 120.3(15) . . ? O11 N6 C56 118.8(16) . . ? N1 C1 C2 124.1(10) . . ? C1 C2 C3 119.6(9) . . ? C4 C3 C2 116.9(8) . . ? C4 C3 C6 122.4(8) . . ? C2 C3 C6 120.7(8) . . ? C3 C4 C5 119.4(9) . . ? N1 C5 C4 123.9(9) . . ? C7 C6 C10 116.3(8) . . ? C7 C6 C3 122.1(8) . . ? C10 C6 C3 121.6(8) . . ? C8 C7 C6 121.9(8) . . ? N2 C8 C7 120.0(8) . . ? N2 C9 C10 121.6(8) . . ? C9 C10 C6 120.1(8) . . ? N2 C11 C12 109.1(7) . . ? N3 C12 C11 111.1(7) . . ? N3 C13 C14 121.2(8) . . ? C13 C14 C15 119.8(8) . . ? C16 C15 C14 117.2(7) . . ? C16 C15 C18 121.7(7) . . ? C14 C15 C18 121.0(7) . . ? C17 C16 C15 121.5(8) . . ? N3 C17 C16 119.1(8) . . ? C19 C18 C22 115.9(8) . . ? C19 C18 C15 122.0(7) . . ? C22 C18 C15 122.0(7) . . ? C18 C19 C20 119.9(9) . . ? N4 C20 C19 124.5(9) . . ? N4 C21 C22 125.2(9) . . ? C18 C22 C21 119.6(8) . . ? C24 C23 O8 123.4(9) . . ? C24 C23 C32 121.3(10) . . ? O8 C23 C32 115.3(9) . . ? C23 C24 C25 121.4(10) . . ? C26 C25 C24 123.2(11) . . ? C26 C25 C30 117.5(11) . . ? C24 C25 C30 119.3(10) . . ? C27 C26 C25 120.4(12) . . ? C26 C27 C28 121.5(11) . . ? C29 C28 C27 120.6(11) . . ? C28 C29 C30 119.2(11) . . ? C29 C30 C25 120.6(10) . . ? C29 C30 C31 122.7(10) . . ? C25 C30 C31 116.6(10) . . ? C32 C31 C30 122.4(9) . . ? O1 C32 C31 124.2(8) . . ? O1 C32 C23 116.8(9) . . ? C31 C32 C23 119.0(9) . . ? O1 C33 C34 109.6(8) . . ? O2 C34 C33 110.4(8) . . ? O2 C35 C36 108.6(7) . . ? O3 C36 C35 111.2(7) . . ? O3 C37 C38 111.4(8) . . ? O4 C38 C37 107.6(7) . . ? C40 C39 O4 126.8(8) . . ? C40 C39 C48 120.9(8) . . ? O4 C39 C48 112.3(8) . . ? C39 C40 C41 121.4(8) . . ? C40 C41 C42 122.5(9) . . ? C40 C41 C46 119.3(8) . . ? C42 C41 C46 118.2(8) . . ? C43 C42 C41 122.9(10) . . ? C42 C43 C44 119.0(10) . . ? C45 C44 C43 120.7(10) . . ? C44 C45 C46 120.7(10) . . ? C47 C46 C41 118.6(8) . . ? C47 C46 C45 122.9(9) . . ? C41 C46 C45 118.5(9) . . ? C48 C47 C46 121.5(8) . . ? C47 C48 O5 124.8(8) . . ? C47 C48 C39 118.2(8) . . ? O5 C48 C39 116.9(7) . . ? O5 C49 C50 109.4(7) . . ? O6 C50 C49 113.7(8) . . ? O6 C51 C52 108.1(8) . . ? O7 C52 C51 110.3(8) . . ? C54 C53 O7 111.8(11) . . ? C53 C54 O8 115.7(9) . . ? F2 B1 F4 115.7(11) . . ? F2 B1 F1 117.1(12) . . ? F4 B1 F1 113.5(9) . . ? F2 B1 F3 106.5(12) . . ? F4 B1 F3 100.4(11) . . ? F1 B1 F3 100.4(10) . . ? F6 B2 F8 113.3(11) . . ? F6 B2 F7 108.7(11) . . ? F8 B2 F7 113.8(11) . . ? F6 B2 F5 107.7(12) . . ? F8 B2 F5 105.8(12) . . ? F7 B2 F5 107.2(12) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.124 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.075 # Attachment 'New-L3.cif' data_[2]pseudorotaxane_[(1,2-bis(4-phenylpyridinium)ethane)-DB24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286502' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H60 B2 F8 N4 O12' _chemical_formula_weight 1082.64 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' B B 0.0013 0.0007 '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' _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 11.6700(9) _cell_length_b 13.1966(10) _cell_length_c 17.1182(13) _cell_angle_alpha 91.475(2) _cell_angle_beta 96.658(2) _cell_angle_gamma 91.858(2) _cell_volume 2616.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.920885 _exptl_absorpt_correction_T_max 1.000000 _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 'Bruker APEX 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 21185 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9196 _reflns_number_gt 6716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.1136P)^2^+2.5368P] 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 9196 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2168 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _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 O1 O 0.75974(18) -0.47604(16) 0.37730(12) 0.0376(5) Uani 1 1 d . . . O2 O 0.77406(18) -0.63852(16) 0.49469(12) 0.0373(5) Uani 1 1 d . . . O3 O 0.58952(19) -0.71289(16) 0.57334(14) 0.0445(6) Uani 1 1 d . . . O4 O 0.60822(19) -0.33696(16) 0.34607(13) 0.0410(5) Uani 1 1 d . . . O5 O 0.0800(4) -0.4376(4) 0.0888(2) 0.1133(14) Uani 1 1 d . . . O6 O 0.2618(3) -0.4525(3) 0.1118(2) 0.0862(10) Uani 1 1 d . . . O101 O -0.12525(18) 0.17017(16) 0.14064(12) 0.0372(5) Uani 1 1 d . . . O102 O 0.05985(19) 0.23719(16) 0.05627(13) 0.0411(5) Uani 1 1 d . . . O103 O 0.25072(19) 0.17454(17) -0.00979(13) 0.0414(5) Uani 1 1 d . . . O104 O -0.25039(19) 0.00329(16) 0.11936(13) 0.0395(5) Uani 1 1 d . . . O105 O 0.3249(4) 0.0469(4) 0.4367(3) 0.1355(18) Uani 1 1 d . . . O106 O 0.4884(3) 0.1135(3) 0.4217(2) 0.1009(12) Uani 1 1 d . . . N1 N 0.4715(2) -0.56249(18) 0.40002(14) 0.0302(5) Uani 1 1 d . . . N2 N 0.1705(4) -0.4260(3) 0.1307(2) 0.0639(9) Uani 1 1 d . . . N101 N 0.0356(2) -0.04236(18) 0.10350(14) 0.0306(5) Uani 1 1 d . . . N102 N 0.3930(4) 0.0803(3) 0.3959(3) 0.0784(12) Uani 1 1 d . . . C1 C 0.5542(3) -0.5773(3) 0.1152(2) 0.0507(9) Uani 1 1 d . . . H1A H 0.5331 -0.5115 0.1259 0.061 Uiso 1 1 calc R . . C2 C 0.5886(4) -0.6017(3) 0.0429(2) 0.0603(11) Uani 1 1 d . . . H2A H 0.5920 -0.5518 0.0057 0.072 Uiso 1 1 calc R . . C3 C 0.6178(3) -0.6991(3) 0.0252(2) 0.0493(9) Uani 1 1 d . . . H3A H 0.6406 -0.7154 -0.0238 0.059 Uiso 1 1 calc R . . C4 C 0.6131(3) -0.7719(3) 0.0807(2) 0.0471(9) Uani 1 1 d . . . H4A H 0.6319 -0.8381 0.0690 0.057 Uiso 1 1 calc R . . C5 C 0.5805(3) -0.7476(3) 0.15379(19) 0.0411(8) Uani 1 1 d . . . H5A H 0.5785 -0.7976 0.1910 0.049 Uiso 1 1 calc R . . C6 C 0.5507(2) -0.6498(2) 0.17238(17) 0.0345(7) Uani 1 1 d . . . C7 C 0.5204(2) -0.6209(2) 0.25110(17) 0.0315(6) Uani 1 1 d . . . C8 C 0.4554(3) -0.5364(2) 0.26362(18) 0.0356(7) Uani 1 1 d . . . H8A H 0.4267 -0.4987 0.2210 0.043 Uiso 1 1 calc R . . C9 C 0.4334(3) -0.5082(2) 0.33712(18) 0.0351(7) Uani 1 1 d . . . H9A H 0.3914 -0.4507 0.3442 0.042 Uiso 1 1 calc R . . C10 C 0.5323(3) -0.6453(2) 0.39059(18) 0.0351(7) Uani 1 1 d . . . H10A H 0.5573 -0.6830 0.4340 0.042 Uiso 1 1 calc R . . C11 C 0.5579(3) -0.6750(2) 0.31741(18) 0.0371(7) Uani 1 1 d . . . H11A H 0.6011 -0.7322 0.3120 0.045 Uiso 1 1 calc R . . C12 C 0.4476(2) -0.5299(2) 0.47947(16) 0.0316(6) Uani 1 1 d . . . H12A H 0.4312 -0.5887 0.5097 0.038 Uiso 1 1 calc R . . H12B H 0.3807 -0.4878 0.4756 0.038 Uiso 1 1 calc R . . C13 C 0.6683(3) -0.3658(2) 0.28519(19) 0.0383(7) Uani 1 1 d . . . C14 C 0.6531(3) -0.3269(3) 0.2109(2) 0.0457(8) Uani 1 1 d . . . H14A H 0.5963 -0.2800 0.1989 0.055 Uiso 1 1 calc R . . C15 C 0.7209(3) -0.3564(3) 0.1538(2) 0.0509(9) Uani 1 1 d . . . H15A H 0.7108 -0.3285 0.1042 0.061 Uiso 1 1 calc R . . C16 C 0.8030(3) -0.4269(3) 0.1707(2) 0.0503(9) Uani 1 1 d . . . H16A H 0.8489 -0.4467 0.1325 0.060 Uiso 1 1 calc R . . C17 C 0.8184(3) -0.4695(3) 0.2448(2) 0.0429(8) Uani 1 1 d . . . H17A H 0.8738 -0.5179 0.2555 0.052 Uiso 1 1 calc R . . C18 C 0.7513(3) -0.4396(2) 0.30263(18) 0.0368(7) Uani 1 1 d . . . C19 C 0.8535(3) -0.5411(3) 0.39694(19) 0.0401(7) Uani 1 1 d . . . H19A H 0.9250 -0.5080 0.3858 0.048 Uiso 1 1 calc R . . H19B H 0.8418 -0.6032 0.3651 0.048 Uiso 1 1 calc R . . C20 C 0.8619(3) -0.5656(3) 0.4821(2) 0.0419(8) Uani 1 1 d . . . H20A H 0.9371 -0.5921 0.4987 0.050 Uiso 1 1 calc R . . H20B H 0.8535 -0.5044 0.5132 0.050 Uiso 1 1 calc R . . C21 C 0.7899(3) -0.6749(3) 0.57266(18) 0.0406(8) Uani 1 1 d . . . H21D H 0.7834 -0.6195 0.6101 0.049 Uiso 1 1 calc R . . H21E H 0.8663 -0.7017 0.5833 0.049 Uiso 1 1 calc R . . C22 C 0.7007(3) -0.7559(3) 0.58155(19) 0.0420(8) Uani 1 1 d . . . H22A H 0.7036 -0.8091 0.5417 0.050 Uiso 1 1 calc R . . H22B H 0.7157 -0.7855 0.6329 0.050 Uiso 1 1 calc R . . C23 C 0.4982(3) -0.7814(3) 0.5891(3) 0.0565(10) Uani 1 1 d . . . H23A H 0.5261 -0.8498 0.5912 0.068 Uiso 1 1 calc R . . H23B H 0.4356 -0.7799 0.5467 0.068 Uiso 1 1 calc R . . C24 C 0.5456(3) -0.2454(3) 0.3356(2) 0.0555(10) Uani 1 1 d . . . H24A H 0.4818 -0.2557 0.2942 0.067 Uiso 1 1 calc R . . H24B H 0.5960 -0.1911 0.3208 0.067 Uiso 1 1 calc R . . C25 C 0.1675(5) -0.3832(4) 0.2092(3) 0.0830(14) Uani 1 1 d . . . H25A H 0.0899 -0.3658 0.2159 0.124 Uiso 1 1 calc R . . H25B H 0.2172 -0.3235 0.2165 0.124 Uiso 1 1 calc R . . H25C H 0.1934 -0.4322 0.2473 0.124 Uiso 1 1 calc R . . C101 C -0.1007(3) -0.1954(3) 0.3497(2) 0.0439(8) Uani 1 1 d . . . H10B H -0.1489 -0.2249 0.3076 0.053 Uiso 1 1 calc R . . C102 C -0.1148(3) -0.2224(3) 0.4256(2) 0.0542(10) Uani 1 1 d . . . H10C H -0.1726 -0.2696 0.4343 0.065 Uiso 1 1 calc R . . C103 C -0.0432(4) -0.1794(3) 0.4886(2) 0.0540(10) Uani 1 1 d . . . H10D H -0.0524 -0.1976 0.5397 0.065 Uiso 1 1 calc R . . C104 C 0.0420(3) -0.1094(3) 0.4752(2) 0.0500(9) Uani 1 1 d . . . H10E H 0.0903 -0.0804 0.5175 0.060 Uiso 1 1 calc R . . C105 C 0.0564(3) -0.0817(2) 0.39961(18) 0.0390(7) Uani 1 1 d . . . H10F H 0.1141 -0.0342 0.3914 0.047 Uiso 1 1 calc R . . C106 C -0.0151(3) -0.1246(2) 0.33561(17) 0.0331(7) Uani 1 1 d . . . C107 C 0.0004(2) -0.0950(2) 0.25471(17) 0.0305(6) Uani 1 1 d . . . C108 C -0.0313(3) -0.1603(2) 0.19012(18) 0.0351(7) Uani 1 1 d . . . H10G H -0.0655 -0.2234 0.1977 0.042 Uiso 1 1 calc R . . C109 C -0.0133(3) -0.1335(2) 0.11601(18) 0.0342(7) Uani 1 1 d . . . H10H H -0.0348 -0.1785 0.0738 0.041 Uiso 1 1 calc R . . C110 C 0.0646(2) 0.0242(2) 0.16409(17) 0.0329(7) Uani 1 1 d . . . H11B H 0.0963 0.0876 0.1547 0.039 Uiso 1 1 calc R . . C111 C 0.0479(2) -0.0003(2) 0.23890(18) 0.0333(7) Uani 1 1 d . . . H11C H 0.0685 0.0467 0.2800 0.040 Uiso 1 1 calc R . . C112 C 0.0563(3) -0.0161(2) 0.02272(17) 0.0338(7) Uani 1 1 d . . . H11D H 0.0849 -0.0744 -0.0037 0.041 Uiso 1 1 calc R . . H11E H 0.1140 0.0387 0.0247 0.041 Uiso 1 1 calc R . . C113 C -0.2412(3) 0.0479(2) 0.19339(19) 0.0389(7) Uani 1 1 d . . . C114 C -0.2940(3) 0.0105(3) 0.2554(2) 0.0523(9) Uani 1 1 d . . . H11F H -0.3393 -0.0491 0.2484 0.063 Uiso 1 1 calc R . . C116 C -0.2129(3) 0.1485(3) 0.3395(2) 0.0528(10) Uani 1 1 d . . . H11G H -0.2033 0.1822 0.3883 0.063 Uiso 1 1 calc R . . C115 C -0.2797(4) 0.0614(3) 0.3285(2) 0.0598(11) Uani 1 1 d . . . H11H H -0.3159 0.0359 0.3699 0.072 Uiso 1 1 calc R . . C117 C -0.1594(3) 0.1867(3) 0.2778(2) 0.0467(8) Uani 1 1 d . . . H11I H -0.1134 0.2458 0.2856 0.056 Uiso 1 1 calc R . . C118 C -0.1738(3) 0.1376(2) 0.20480(18) 0.0368(7) Uani 1 1 d . . . C119 C -0.0819(3) 0.2739(2) 0.1440(2) 0.0434(8) Uani 1 1 d . . . H11J H -0.0191 0.2840 0.1861 0.052 Uiso 1 1 calc R . . H11K H -0.1426 0.3196 0.1535 0.052 Uiso 1 1 calc R . . C120 C -0.0404(3) 0.2935(3) 0.0664(2) 0.0461(8) Uani 1 1 d . . . H12C H -0.1013 0.2747 0.0245 0.055 Uiso 1 1 calc R . . H12D H -0.0222 0.3654 0.0628 0.055 Uiso 1 1 calc R . . C121 C 0.1653(3) 0.2952(3) 0.0686(2) 0.0453(8) Uani 1 1 d . . . H12E H 0.1721 0.3303 0.1195 0.054 Uiso 1 1 calc R . . H12F H 0.1671 0.3456 0.0284 0.054 Uiso 1 1 calc R . . C122 C 0.2630(3) 0.2259(3) 0.0651(2) 0.0471(9) Uani 1 1 d . . . H12G H 0.3357 0.2645 0.0729 0.057 Uiso 1 1 calc R . . H12H H 0.2627 0.1770 0.1064 0.057 Uiso 1 1 calc R . . C123 C 0.3445(3) 0.1110(3) -0.0196(2) 0.0495(9) Uani 1 1 d . . . H12I H 0.3414 0.0531 0.0140 0.059 Uiso 1 1 calc R . . H12J H 0.4170 0.1483 -0.0044 0.059 Uiso 1 1 calc R . . C124 C -0.3384(3) -0.0751(3) 0.1035(2) 0.0491(9) Uani 1 1 d . . . H12K H -0.4123 -0.0493 0.1137 0.059 Uiso 1 1 calc R . . H12L H -0.3211 -0.1313 0.1379 0.059 Uiso 1 1 calc R . . C125 C 0.3606(5) 0.0866(5) 0.3121(4) 0.0972(18) Uani 1 1 d . . . H12M H 0.2842 0.0574 0.2985 0.146 Uiso 1 1 calc R . . H12N H 0.4141 0.0502 0.2844 0.146 Uiso 1 1 calc R . . H12O H 0.3620 0.1564 0.2976 0.146 Uiso 1 1 calc R . . B1 B 0.1628(4) 0.3374(4) 0.3296(3) 0.0560(12) Uani 1 1 d . . . B101 B 0.3214(3) -0.1329(3) 0.1605(2) 0.0436(9) Uani 1 1 d . . . F1 F 0.1890(6) 0.3911(6) 0.2780(4) 0.274(5) Uani 1 1 d . . . F2 F 0.0625(3) 0.3435(5) 0.3531(3) 0.167(2) Uani 1 1 d . . . F3 F 0.1462(5) 0.2433(4) 0.2950(3) 0.194(3) Uani 1 1 d . . . F4 F 0.2464(3) 0.3321(4) 0.3911(2) 0.1351(16) Uani 1 1 d . . . F101 F 0.3195(3) -0.0302(2) 0.14412(17) 0.0935(9) Uani 1 1 d . . . F102 F 0.2386(2) -0.1827(2) 0.10695(15) 0.0786(8) Uani 1 1 d . . . F103 F 0.42632(19) -0.1714(2) 0.15488(15) 0.0747(7) Uani 1 1 d . . . F104 F 0.2889(2) -0.14356(18) 0.23500(13) 0.0692(7) 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 O1 0.0397(12) 0.0362(12) 0.0393(12) 0.0062(9) 0.0128(9) 0.0051(9) O2 0.0365(12) 0.0441(12) 0.0317(11) 0.0071(9) 0.0046(9) 0.0005(9) O3 0.0454(13) 0.0368(12) 0.0568(15) 0.0112(10) 0.0240(11) 0.0096(10) O4 0.0411(12) 0.0388(12) 0.0463(13) 0.0100(10) 0.0162(10) 0.0057(10) O5 0.097(3) 0.139(4) 0.093(3) 0.027(2) -0.031(2) -0.019(3) O6 0.096(3) 0.087(2) 0.083(2) 0.0160(18) 0.037(2) 0.009(2) O101 0.0398(12) 0.0365(12) 0.0358(12) -0.0020(9) 0.0089(9) -0.0022(9) O102 0.0453(13) 0.0337(12) 0.0446(13) -0.0012(9) 0.0097(10) -0.0087(10) O103 0.0404(12) 0.0448(13) 0.0382(12) -0.0001(10) 0.0036(9) -0.0082(10) O104 0.0423(12) 0.0353(12) 0.0429(13) 0.0029(9) 0.0141(10) -0.0035(9) O105 0.117(4) 0.134(4) 0.160(5) -0.001(3) 0.050(3) -0.050(3) O106 0.076(2) 0.125(3) 0.100(3) -0.022(2) 0.013(2) -0.013(2) N1 0.0294(12) 0.0339(13) 0.0272(13) -0.0020(10) 0.0045(10) 0.0001(10) N2 0.070(2) 0.061(2) 0.060(2) 0.0198(17) 0.0023(19) -0.0016(18) N101 0.0269(12) 0.0360(14) 0.0289(13) 0.0069(10) 0.0018(10) -0.0008(10) N102 0.062(2) 0.060(2) 0.113(4) -0.028(2) 0.020(2) -0.0117(19) C1 0.068(2) 0.046(2) 0.041(2) -0.0059(16) 0.0180(17) -0.0006(17) C2 0.084(3) 0.059(2) 0.042(2) 0.0006(17) 0.026(2) -0.001(2) C3 0.047(2) 0.067(2) 0.0343(19) -0.0133(17) 0.0099(15) 0.0025(17) C4 0.0403(18) 0.058(2) 0.0413(19) -0.0168(16) -0.0031(15) 0.0129(16) C5 0.0379(17) 0.050(2) 0.0345(17) -0.0054(14) -0.0002(13) 0.0119(15) C6 0.0276(15) 0.0441(18) 0.0308(16) -0.0057(13) 0.0015(12) -0.0003(13) C7 0.0252(14) 0.0366(16) 0.0318(16) -0.0031(12) 0.0012(12) -0.0032(12) C8 0.0383(17) 0.0389(17) 0.0303(16) 0.0037(13) 0.0051(13) 0.0068(13) C9 0.0356(16) 0.0355(17) 0.0350(17) 0.0029(13) 0.0061(13) 0.0058(13) C10 0.0380(17) 0.0357(17) 0.0310(16) 0.0004(13) 0.0004(13) 0.0064(13) C11 0.0379(17) 0.0372(17) 0.0357(17) -0.0046(13) 0.0010(13) 0.0093(13) C12 0.0324(15) 0.0368(16) 0.0268(15) -0.0003(12) 0.0090(12) 0.0000(12) C13 0.0360(17) 0.0352(17) 0.0457(19) 0.0064(14) 0.0138(14) -0.0033(13) C14 0.0442(19) 0.046(2) 0.048(2) 0.0171(16) 0.0102(16) 0.0000(15) C15 0.058(2) 0.056(2) 0.041(2) 0.0141(16) 0.0146(17) -0.0043(18) C16 0.056(2) 0.054(2) 0.044(2) 0.0030(16) 0.0209(17) -0.0044(18) C17 0.0440(19) 0.0392(18) 0.048(2) 0.0030(15) 0.0158(15) -0.0010(14) C18 0.0379(17) 0.0362(17) 0.0373(17) 0.0053(13) 0.0105(13) -0.0071(13) C19 0.0339(16) 0.0441(19) 0.0442(19) 0.0056(14) 0.0118(14) 0.0024(14) C20 0.0351(17) 0.0459(19) 0.0448(19) 0.0066(15) 0.0042(14) 0.0011(14) C21 0.0425(18) 0.0491(19) 0.0312(17) 0.0067(14) 0.0040(13) 0.0134(15) C22 0.051(2) 0.0433(19) 0.0354(18) 0.0112(14) 0.0130(15) 0.0183(15) C23 0.061(2) 0.0343(19) 0.081(3) 0.0061(18) 0.035(2) 0.0047(16) C24 0.059(2) 0.044(2) 0.070(3) 0.0231(18) 0.030(2) 0.0108(17) C25 0.105(4) 0.077(3) 0.068(3) -0.005(2) 0.009(3) 0.021(3) C101 0.0441(19) 0.048(2) 0.0401(19) 0.0085(15) 0.0078(15) 0.0008(15) C102 0.060(2) 0.056(2) 0.051(2) 0.0186(18) 0.0215(18) 0.0051(18) C103 0.078(3) 0.056(2) 0.0337(19) 0.0133(16) 0.0212(18) 0.024(2) C104 0.071(2) 0.047(2) 0.0317(18) 0.0009(15) -0.0005(16) 0.0184(18) C105 0.0453(18) 0.0378(17) 0.0336(17) 0.0049(13) 0.0008(14) 0.0077(14) C106 0.0349(16) 0.0344(16) 0.0307(16) 0.0071(12) 0.0037(12) 0.0082(12) C107 0.0250(14) 0.0363(16) 0.0297(15) 0.0049(12) -0.0002(11) 0.0038(12) C108 0.0351(16) 0.0339(16) 0.0355(17) 0.0059(13) 0.0012(13) -0.0065(13) C109 0.0351(16) 0.0359(17) 0.0302(16) 0.0011(12) 0.0004(12) -0.0056(13) C110 0.0312(15) 0.0324(16) 0.0347(17) 0.0056(13) 0.0024(12) -0.0012(12) C111 0.0321(15) 0.0353(16) 0.0314(16) 0.0003(12) -0.0002(12) 0.0012(12) C112 0.0334(16) 0.0407(17) 0.0274(15) 0.0083(13) 0.0038(12) -0.0038(13) C113 0.0387(17) 0.0420(18) 0.0389(18) 0.0098(14) 0.0122(14) 0.0125(14) C114 0.059(2) 0.048(2) 0.056(2) 0.0156(17) 0.0234(18) 0.0131(17) C116 0.058(2) 0.068(3) 0.0339(19) 0.0043(17) 0.0054(16) 0.024(2) C115 0.068(3) 0.075(3) 0.043(2) 0.0192(19) 0.0240(19) 0.032(2) C117 0.0393(18) 0.061(2) 0.0394(19) -0.0014(16) 0.0006(14) 0.0157(16) C118 0.0325(16) 0.0436(18) 0.0351(17) 0.0033(14) 0.0042(13) 0.0098(13) C119 0.0449(19) 0.0371(18) 0.048(2) -0.0070(15) 0.0050(15) 0.0004(14) C120 0.052(2) 0.0365(18) 0.050(2) 0.0018(15) 0.0053(16) -0.0020(15) C121 0.056(2) 0.0426(19) 0.0367(18) -0.0060(14) 0.0083(15) -0.0187(16) C122 0.0445(19) 0.056(2) 0.0385(19) -0.0043(15) 0.0011(15) -0.0194(16) C123 0.0351(18) 0.049(2) 0.063(2) -0.0007(17) 0.0028(16) -0.0094(15) C124 0.0412(19) 0.045(2) 0.063(2) 0.0012(17) 0.0198(17) -0.0105(15) C125 0.074(3) 0.097(4) 0.115(5) -0.039(3) -0.004(3) -0.011(3) B1 0.039(2) 0.077(3) 0.052(3) 0.000(2) 0.0161(19) -0.029(2) B101 0.045(2) 0.052(2) 0.035(2) 0.0021(17) 0.0087(16) 0.0072(18) F1 0.253(7) 0.362(10) 0.180(5) 0.134(6) -0.055(5) -0.197(7) F2 0.072(2) 0.248(6) 0.179(4) -0.051(4) 0.013(2) 0.019(3) F3 0.183(5) 0.126(4) 0.244(6) -0.071(4) -0.101(4) 0.059(3) F4 0.079(2) 0.226(5) 0.089(2) -0.006(2) -0.0159(17) -0.065(3) F101 0.143(3) 0.0646(17) 0.0786(19) 0.0238(14) 0.0293(18) 0.0102(17) F102 0.0550(14) 0.109(2) 0.0689(16) -0.0212(14) -0.0037(12) 0.0178(13) F103 0.0456(13) 0.106(2) 0.0723(16) 0.0022(14) 0.0044(11) 0.0154(13) F104 0.0927(18) 0.0719(15) 0.0475(13) 0.0085(11) 0.0249(12) 0.0051(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 O1 C18 1.372(4) . ? O1 C19 1.428(4) . ? O2 C20 1.422(4) . ? O2 C21 1.424(4) . ? O3 C22 1.427(4) . ? O3 C23 1.429(4) . ? O4 C13 1.374(4) . ? O4 C24 1.436(4) . ? O5 N2 1.209(5) . ? O6 N2 1.208(5) . ? O101 C118 1.365(4) . ? O101 C119 1.441(4) . ? O102 C121 1.420(4) . ? O102 C120 1.431(4) . ? O103 C123 1.423(4) . ? O103 C122 1.425(4) . ? O104 C113 1.375(4) . ? O104 C124 1.432(4) . ? O105 N102 1.198(5) . ? O106 N102 1.213(5) . ? N1 C10 1.338(4) . ? N1 C9 1.349(4) . ? N1 C12 1.476(4) . ? N2 C25 1.449(6) . ? N101 C110 1.347(4) . ? N101 C109 1.347(4) . ? N101 C112 1.479(4) . ? N102 C125 1.447(7) . ? C1 C2 1.379(5) . ? C1 C6 1.389(5) . ? C2 C3 1.376(6) . ? C3 C4 1.373(5) . ? C4 C5 1.383(5) . ? C5 C6 1.387(5) . ? C6 C7 1.476(4) . ? C7 C11 1.392(4) . ? C7 C8 1.395(4) . ? C8 C9 1.358(4) . ? C10 C11 1.372(4) . ? C12 C12 1.523(6) 2_646 ? C13 C14 1.379(5) . ? C13 C18 1.408(5) . ? C14 C15 1.382(5) . ? C15 C16 1.370(5) . ? C16 C17 1.395(5) . ? C17 C18 1.389(4) . ? C19 C20 1.494(4) . ? C21 C22 1.491(5) . ? C23 C24 1.480(5) 2_646 ? C24 C23 1.480(5) 2_646 ? C101 C102 1.384(5) . ? C101 C106 1.391(5) . ? C102 C103 1.383(6) . ? C103 C104 1.378(6) . ? C104 C105 1.381(5) . ? C105 C106 1.394(4) . ? C106 C107 1.478(4) . ? C107 C108 1.392(4) . ? C107 C111 1.397(4) . ? C108 C109 1.364(4) . ? C110 C111 1.363(4) . ? C112 C112 1.525(6) 2 ? C113 C114 1.382(5) . ? C113 C118 1.397(5) . ? C114 C115 1.395(6) . ? C116 C115 1.364(6) . ? C116 C117 1.385(5) . ? C117 C118 1.383(5) . ? C119 C120 1.492(5) . ? C121 C122 1.490(5) . ? C123 C124 1.493(5) 2 ? C124 C123 1.493(5) 2 ? B1 F1 1.206(6) . ? B1 F2 1.285(5) . ? B1 F4 1.355(6) . ? B1 F3 1.360(6) . ? B101 F103 1.354(4) . ? B101 F104 1.381(4) . ? B101 F102 1.389(5) . ? B101 F101 1.391(5) . ? 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 C18 O1 C19 115.3(2) . . ? C20 O2 C21 111.4(2) . . ? C22 O3 C23 114.0(3) . . ? C13 O4 C24 116.0(2) . . ? C118 O101 C119 116.5(2) . . ? C121 O102 C120 114.4(3) . . ? C123 O103 C122 112.5(3) . . ? C113 O104 C124 115.5(2) . . ? C10 N1 C9 120.0(2) . . ? C10 N1 C12 119.9(2) . . ? C9 N1 C12 120.1(2) . . ? O6 N2 O5 123.5(5) . . ? O6 N2 C25 118.6(4) . . ? O5 N2 C25 117.7(5) . . ? C110 N101 C109 120.1(2) . . ? C110 N101 C112 120.6(2) . . ? C109 N101 C112 119.3(2) . . ? O105 N102 O106 123.2(5) . . ? O105 N102 C125 119.8(5) . . ? O106 N102 C125 116.9(5) . . ? C2 C1 C6 120.9(3) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 119.2(3) . . ? C3 C4 C5 120.5(3) . . ? C4 C5 C6 120.9(3) . . ? C5 C6 C1 117.9(3) . . ? C5 C6 C7 121.9(3) . . ? C1 C6 C7 120.1(3) . . ? C11 C7 C8 116.3(3) . . ? C11 C7 C6 121.7(3) . . ? C8 C7 C6 122.0(3) . . ? C9 C8 C7 121.0(3) . . ? N1 C9 C8 121.0(3) . . ? N1 C10 C11 120.6(3) . . ? C10 C11 C7 121.1(3) . . ? N1 C12 C12 109.2(3) . 2_646 ? O4 C13 C14 124.6(3) . . ? O4 C13 C18 115.8(3) . . ? C14 C13 C18 119.6(3) . . ? C13 C14 C15 121.1(3) . . ? C16 C15 C14 119.6(3) . . ? C15 C16 C17 120.6(3) . . ? C18 C17 C16 120.1(3) . . ? O1 C18 C17 124.8(3) . . ? O1 C18 C13 116.2(3) . . ? C17 C18 C13 119.0(3) . . ? O1 C19 C20 110.1(3) . . ? O2 C20 C19 110.0(3) . . ? O2 C21 C22 109.5(3) . . ? O3 C22 C21 109.1(3) . . ? O3 C23 C24 111.4(3) . 2_646 ? O4 C24 C23 108.1(3) . 2_646 ? C102 C101 C106 120.7(3) . . ? C103 C102 C101 120.1(4) . . ? C104 C103 C102 119.6(3) . . ? C103 C104 C105 120.7(3) . . ? C104 C105 C106 120.3(3) . . ? C101 C106 C105 118.6(3) . . ? C101 C106 C107 121.1(3) . . ? C105 C106 C107 120.3(3) . . ? C108 C107 C111 116.4(3) . . ? C108 C107 C106 121.7(3) . . ? C111 C107 C106 121.9(3) . . ? C109 C108 C107 121.2(3) . . ? N101 C109 C108 120.5(3) . . ? N101 C110 C111 120.9(3) . . ? C110 C111 C107 120.8(3) . . ? N101 C112 C112 109.5(3) . 2 ? O104 C113 C114 124.7(3) . . ? O104 C113 C118 116.2(3) . . ? C114 C113 C118 119.1(3) . . ? C113 C114 C115 120.5(4) . . ? C115 C116 C117 120.0(4) . . ? C116 C115 C114 120.1(4) . . ? C118 C117 C116 120.5(4) . . ? O101 C118 C117 124.5(3) . . ? O101 C118 C113 115.7(3) . . ? C117 C118 C113 119.8(3) . . ? O101 C119 C120 106.7(3) . . ? O102 C120 C119 111.2(3) . . ? O102 C121 C122 108.9(3) . . ? O103 C122 C121 109.0(3) . . ? O103 C123 C124 109.9(3) . 2 ? O104 C124 C123 109.7(3) . 2 ? F1 B1 F2 119.7(7) . . ? F1 B1 F4 113.8(4) . . ? F2 B1 F4 111.4(4) . . ? F1 B1 F3 104.7(6) . . ? F2 B1 F3 97.1(4) . . ? F4 B1 F3 107.8(5) . . ? F103 B101 F104 111.5(3) . . ? F103 B101 F102 110.1(3) . . ? F104 B101 F102 108.3(3) . . ? F103 B101 F101 112.0(3) . . ? F104 B101 F101 107.5(3) . . ? F102 B101 F101 107.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.084 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.061 # Attachment 'New-L4.cif' data_[2]pseudorotaxane_[(1,2-bis(4-phenylpyridinium)ethane)-DN24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H64 B2 F8 N4 O12' _chemical_formula_weight 1182.75 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 12.3959(8) _cell_length_b 19.1294(12) _cell_length_c 12.9148(8) _cell_angle_alpha 90.00 _cell_angle_beta 112.8550(10) _cell_angle_gamma 90.00 _cell_volume 2822.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.740488 _exptl_absorpt_correction_T_max 1.000000 _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 'Bruker APEX 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 22117 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9879 _reflns_number_gt 6669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.0893P)^2^+1.4800P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.7(14) _refine_ls_number_reflns 9879 _refine_ls_number_parameters 740 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1284 _refine_ls_R_factor_gt 0.0950 _refine_ls_wR_factor_ref 0.2236 _refine_ls_wR_factor_gt 0.2081 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.003 _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 O1 O 0.1416(4) 0.6622(3) -0.3478(4) 0.0552(13) Uani 1 1 d . . . O2 O 0.2999(5) 0.7815(3) -0.3120(4) 0.0721(18) Uani 1 1 d . . . O3 O 0.4866(5) 0.8241(3) -0.1178(5) 0.0660(16) Uani 1 1 d . . . O4 O 0.4281(4) 0.9139(2) 0.0429(4) 0.0373(10) Uani 1 1 d . . . O5 O 0.3202(4) 0.8793(2) 0.1697(3) 0.0352(10) Uani 1 1 d . . . O6 O 0.1662(4) 0.7586(2) 0.1455(4) 0.0435(11) Uani 1 1 d . . . O7 O 0.0297(3) 0.6542(2) -0.0071(3) 0.0350(10) Uani 1 1 d . . . O8 O 0.0470(4) 0.6052(2) -0.2194(3) 0.0353(10) Uani 1 1 d . A . O9 O 0.5269(9) 0.6121(4) -0.2816(7) 0.117(3) Uani 1 1 d . . . O10 O 0.6798(8) 0.6076(5) -0.3150(8) 0.142(4) Uani 1 1 d . . . O11 O 0.3314(10) 1.1673(8) -0.3238(10) 0.192(6) Uani 1 1 d . . . O12 O 0.4350(8) 1.1273(4) -0.4092(7) 0.115(3) Uani 1 1 d . . . N1 N 0.3121(4) 0.6844(2) -0.0401(4) 0.0270(11) Uani 1 1 d . . . N2 N 0.1473(4) 0.8530(2) -0.1189(4) 0.0322(12) Uani 1 1 d . . . N3 N 0.5935(9) 0.5824(6) -0.3117(7) 0.096(3) Uani 1 1 d . . . N4 N 0.4015(9) 1.1292(6) -0.3344(8) 0.108(3) Uani 1 1 d . . . C1 C 0.3106(7) 0.4171(4) -0.0213(7) 0.060(2) Uani 1 1 d . . . H1A H 0.2763 0.4319 0.0274 0.072 Uiso 1 1 calc R . . C2 C 0.3183(8) 0.3474(4) -0.0412(8) 0.076(3) Uani 1 1 d . . . H2A H 0.2895 0.3156 -0.0038 0.092 Uiso 1 1 calc R . . C3 C 0.3643(9) 0.3225(5) -0.1105(10) 0.087(4) Uani 1 1 d . . . H3A H 0.3662 0.2749 -0.1240 0.104 Uiso 1 1 calc R . . C4 C 0.4076(9) 0.3695(6) -0.1600(10) 0.093(4) Uani 1 1 d . . . H4A H 0.4448 0.3531 -0.2054 0.112 Uiso 1 1 calc R . . C5 C 0.4011(7) 0.4408(4) -0.1482(7) 0.066(2) Uani 1 1 d . . . H5A H 0.4274 0.4716 -0.1889 0.080 Uiso 1 1 calc R . . C6 C 0.3541(5) 0.4649(3) -0.0739(6) 0.0437(18) Uani 1 1 d . . . C7 C 0.3405(5) 0.5425(3) -0.0598(5) 0.0335(15) Uani 1 1 d . . . C8 C 0.3676(5) 0.5912(3) -0.1260(5) 0.0368(16) Uani 1 1 d . . . H8A H 0.3973 0.5759 -0.1780 0.044 Uiso 1 1 calc R . . C9 C 0.3514(5) 0.6607(4) -0.1161(5) 0.0404(17) Uani 1 1 d . . . H9A H 0.3679 0.6922 -0.1628 0.048 Uiso 1 1 calc R . . C10 C 0.2903(5) 0.6396(3) 0.0276(5) 0.0324(14) Uani 1 1 d . . . H10A H 0.2642 0.6565 0.0814 0.039 Uiso 1 1 calc R . . C11 C 0.3052(5) 0.5695(3) 0.0203(5) 0.0372(15) Uani 1 1 d . . . H11A H 0.2913 0.5395 0.0705 0.045 Uiso 1 1 calc R . . C12 C 0.2899(5) 0.7602(3) -0.0358(6) 0.0380(15) Uani 1 1 d . . . H12A H 0.3453 0.7866 -0.0566 0.046 Uiso 1 1 calc R . . H12B H 0.3005 0.7734 0.0401 0.046 Uiso 1 1 calc R . . C13 C 0.1667(5) 0.7771(3) -0.1154(5) 0.0347(15) Uani 1 1 d . . . H13A H 0.1541 0.7603 -0.1901 0.042 Uiso 1 1 calc R . . H13B H 0.1113 0.7538 -0.0909 0.042 Uiso 1 1 calc R . . C14 C 0.1868(5) 0.8936(3) -0.1802(5) 0.0358(15) Uani 1 1 d . . . H14A H 0.2225 0.8734 -0.2243 0.043 Uiso 1 1 calc R . . C15 C 0.1756(5) 0.9652(3) -0.1790(5) 0.0337(15) Uani 1 1 d . . . H15A H 0.2045 0.9926 -0.2218 0.040 Uiso 1 1 calc R . . C16 C 0.1218(5) 0.9971(4) -0.1150(5) 0.0341(15) Uani 1 1 d . . . C17 C 0.0793(5) 0.9531(3) -0.0544(5) 0.0295(14) Uani 1 1 d . . . H17A H 0.0410 0.9721 -0.0118 0.035 Uiso 1 1 calc R . . C18 C 0.0928(5) 0.8825(3) -0.0563(5) 0.0324(14) Uani 1 1 d . . . H18A H 0.0644 0.8541 -0.0142 0.039 Uiso 1 1 calc R . . C19 C 0.1118(5) 1.0751(3) -0.1124(5) 0.0320(15) Uani 1 1 d . . . C20 C 0.1328(7) 1.1171(3) -0.1893(6) 0.0527(19) Uani 1 1 d . . . H20A H 0.1547 1.0971 -0.2438 0.063 Uiso 1 1 calc R . . C21 C 0.1215(8) 1.1882(4) -0.1859(7) 0.063(2) Uani 1 1 d . . . H21A H 0.1378 1.2161 -0.2371 0.076 Uiso 1 1 calc R . . C22 C 0.0877(6) 1.2179(4) -0.1108(8) 0.059(2) Uani 1 1 d . . . H22A H 0.0760 1.2660 -0.1126 0.071 Uiso 1 1 calc R . . C23 C 0.0701(6) 1.1788(4) -0.0312(8) 0.058(2) Uani 1 1 d . . . H23A H 0.0510 1.2004 0.0240 0.069 Uiso 1 1 calc R . . C24 C 0.0806(6) 1.1051(3) -0.0321(7) 0.052(2) Uani 1 1 d . . . H24A H 0.0666 1.0777 0.0209 0.063 Uiso 1 1 calc R . . C25 C 0.0829(5) 0.5599(3) -0.2807(5) 0.0372(15) Uani 1 1 d . . . C26 C 0.0719(5) 0.4902(3) -0.2801(5) 0.0361(15) Uani 1 1 d . A . H26A H 0.0401 0.4704 -0.2325 0.043 Uiso 1 1 calc R . . C27 C 0.1070(5) 0.4449(4) -0.3500(6) 0.0437(18) Uani 1 1 d . . . C28 C 0.0943(6) 0.3722(4) -0.3477(6) 0.0504(19) Uani 1 1 d . A . H28A H 0.0646 0.3514 -0.2992 0.061 Uiso 1 1 calc R . . C29 C 0.1268(7) 0.3327(5) -0.4189(8) 0.067(2) Uani 1 1 d . . . H29A H 0.1172 0.2845 -0.4190 0.080 Uiso 1 1 calc R A . C30 C 0.1729(7) 0.3608(5) -0.4898(8) 0.071(3) Uani 1 1 d . A . H30A H 0.1926 0.3323 -0.5381 0.086 Uiso 1 1 calc R . . C31 C 0.1894(6) 0.4299(5) -0.4889(7) 0.066(2) Uani 1 1 d . . . H31A H 0.2233 0.4486 -0.5356 0.079 Uiso 1 1 calc R A . C32 C 0.1572(6) 0.4756(5) -0.4195(7) 0.060(2) Uani 1 1 d . A . C33 C 0.1709(6) 0.5499(4) -0.4187(6) 0.052(2) Uani 1 1 d . . . H33A H 0.2055 0.5706 -0.4633 0.062 Uiso 1 1 calc R A . C34 C 0.1331(6) 0.5904(4) -0.3523(6) 0.0472(18) Uani 1 1 d . A . C37 C 0.4112(8) 0.7926(5) -0.3116(8) 0.073(2) Uiso 1 1 d . . . H37A H 0.4050 0.8114 -0.3835 0.088 Uiso 1 1 calc R . . H37B H 0.4538 0.7488 -0.2991 0.088 Uiso 1 1 calc R . . C38 C 0.4751(8) 0.8435(5) -0.2191(8) 0.082(3) Uani 1 1 d . . . H38A H 0.5525 0.8512 -0.2189 0.098 Uiso 1 1 calc R A . H38B H 0.4339 0.8878 -0.2362 0.098 Uiso 1 1 calc R . . C39 C 0.5608(7) 0.8654(4) -0.0299(7) 0.058(2) Uani 1 1 d . . . H39A H 0.6283 0.8777 -0.0465 0.070 Uiso 1 1 calc R A . H39B H 0.5888 0.8371 0.0378 0.070 Uiso 1 1 calc R . . C40 C 0.5105(6) 0.9312(3) -0.0050(6) 0.0423(16) Uani 1 1 d . . . H40A H 0.5725 0.9599 0.0470 0.051 Uiso 1 1 calc R . . H40B H 0.4722 0.9577 -0.0737 0.051 Uiso 1 1 calc R . . C41 C 0.3961(5) 0.9679(3) 0.0923(5) 0.0369(16) Uani 1 1 d . . . C42 C 0.4178(5) 1.0372(3) 0.0810(5) 0.0316(14) Uani 1 1 d . . . H42A H 0.4550 1.0499 0.0337 0.038 Uiso 1 1 calc R . . C43 C 0.3845(6) 1.0901(3) 0.1401(5) 0.0398(16) Uani 1 1 d . . . C44 C 0.4017(6) 1.1622(4) 0.1274(6) 0.0496(19) Uani 1 1 d . . . H44A H 0.4349 1.1769 0.0777 0.059 Uiso 1 1 calc R . . C45 C 0.3692(6) 1.2106(3) 0.1884(6) 0.053(2) Uani 1 1 d . . . H45A H 0.3842 1.2577 0.1816 0.063 Uiso 1 1 calc R . . C46 C 0.3158(7) 1.1920(4) 0.2587(6) 0.0512(19) Uani 1 1 d . . . H46A H 0.2921 1.2261 0.2966 0.061 Uiso 1 1 calc R . . C47 C 0.2973(6) 1.1233(3) 0.2732(6) 0.0460(18) Uani 1 1 d . . . H47A H 0.2631 1.1111 0.3233 0.055 Uiso 1 1 calc R . . C48 C 0.3286(5) 1.0696(3) 0.2143(5) 0.0303(14) Uani 1 1 d . . . C49 C 0.3074(5) 0.9988(3) 0.2231(5) 0.0344(15) Uani 1 1 d . . . H49A H 0.2707 0.9854 0.2706 0.041 Uiso 1 1 calc R . . C50 C 0.3377(5) 0.9491(3) 0.1661(5) 0.0363(16) Uani 1 1 d . . . C51 C 0.2734(6) 0.8579(3) 0.2504(5) 0.0407(16) Uani 1 1 d . . . H51A H 0.1976 0.8795 0.2329 0.049 Uiso 1 1 calc R . . H51B H 0.3252 0.8730 0.3248 0.049 Uiso 1 1 calc R . . C52 C 0.2610(6) 0.7799(3) 0.2487(6) 0.0470(18) Uani 1 1 d . . . H52A H 0.3335 0.7581 0.2534 0.056 Uiso 1 1 calc R . . H52B H 0.2448 0.7647 0.3129 0.056 Uiso 1 1 calc R . . C53 C 0.0851(6) 0.7160(3) 0.1656(5) 0.0409(16) Uani 1 1 d . . . H53A H 0.0532 0.7404 0.2131 0.049 Uiso 1 1 calc R . . H53B H 0.1236 0.6739 0.2045 0.049 Uiso 1 1 calc R . . C54 C -0.0126(5) 0.6967(3) 0.0556(6) 0.0404(16) Uani 1 1 d . . . H54B H -0.0738 0.6723 0.0703 0.048 Uiso 1 1 calc R . . H54A H -0.0461 0.7388 0.0136 0.048 Uiso 1 1 calc R . . C55 C -0.0605(5) 0.6298(3) -0.1065(5) 0.0333(15) Uani 1 1 d . A . H55A H -0.0911 0.6685 -0.1582 0.040 Uiso 1 1 calc R . . H55B H -0.1239 0.6112 -0.0884 0.040 Uiso 1 1 calc R . . C56 C -0.0171(5) 0.5747(3) -0.1612(5) 0.0361(15) Uani 1 1 d . . . H56A H 0.0326 0.5425 -0.1048 0.043 Uiso 1 1 calc R A . H56B H -0.0828 0.5485 -0.2134 0.043 Uiso 1 1 calc R . . C57 C 0.5705(11) 0.5084(7) -0.3417(11) 0.121(4) Uiso 1 1 d . . . H57A H 0.6316 0.4900 -0.3621 0.182 Uiso 1 1 calc R . . H57B H 0.4967 0.5039 -0.4040 0.182 Uiso 1 1 calc R . . H57C H 0.5683 0.4829 -0.2785 0.182 Uiso 1 1 calc R . . C58 C 0.4513(16) 1.0744(9) -0.2539(15) 0.181(7) Uiso 1 1 d . . . H58A H 0.5010 1.0457 -0.2778 0.271 Uiso 1 1 calc R . . H58B H 0.3897 1.0463 -0.2482 0.271 Uiso 1 1 calc R . . H58C H 0.4965 1.0945 -0.1820 0.271 Uiso 1 1 calc R . . B1 B -0.1451(9) 0.4004(4) -0.1248(8) 0.050(2) Uani 1 1 d . . . F1 F -0.0259(10) 0.3937(6) -0.0814(10) 0.214(5) Uani 1 1 d . . . F2 F -0.1484(7) 0.4632(3) -0.0830(7) 0.138(3) Uani 1 1 d . . . F3 F -0.1966(10) 0.3552(3) -0.0910(6) 0.196(5) Uani 1 1 d . . . F4 F -0.1669(7) 0.3971(4) -0.2298(5) 0.144(3) Uani 1 1 d . . . B2 B 0.7522(10) 1.0462(7) 0.0136(11) 0.080(3) Uani 1 1 d . . . F5 F 0.6873(10) 1.1035(6) -0.0239(10) 0.237(7) Uani 1 1 d . . . F6 F 0.8586(6) 1.0644(5) 0.0255(6) 0.162(4) Uani 1 1 d . . . F7 F 0.7022(6) 0.9997(3) -0.0687(5) 0.109(2) Uani 1 1 d . . . F8 F 0.7454(6) 1.0329(5) 0.1091(5) 0.165(4) Uani 1 1 d . . . C35A C 0.1570(14) 0.7108(9) -0.4287(13) 0.031(4) Uiso 0.40 1 d P A -1 H35A H 0.1226 0.6910 -0.5036 0.037 Uiso 0.40 1 calc PR A -1 H35B H 0.1172 0.7544 -0.4285 0.037 Uiso 0.40 1 calc PR A -1 C36A C 0.2794(13) 0.7240(8) -0.4001(12) 0.033(3) Uiso 0.40 1 d P A -1 H36A H 0.2944 0.7404 -0.4643 0.040 Uiso 0.40 1 calc PR A -1 H36B H 0.3267 0.6829 -0.3686 0.040 Uiso 0.40 1 calc PR A -1 C36B C 0.1976(8) 0.7617(5) -0.4133(7) 0.024(2) Uiso 0.60 1 d P A -2 H36C H 0.2023 0.7837 -0.4791 0.029 Uiso 0.60 1 calc PR A -2 H36D H 0.1261 0.7771 -0.4065 0.029 Uiso 0.60 1 calc PR A -2 C35B C 0.1968(12) 0.6830(6) -0.4253(10) 0.041(3) Uiso 0.60 1 d P A -2 H35C H 0.1507 0.6684 -0.5017 0.049 Uiso 0.60 1 calc PR A -2 H35D H 0.2755 0.6643 -0.4022 0.049 Uiso 0.60 1 calc PR A -2 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 O1 0.049(3) 0.072(4) 0.045(3) 0.000(3) 0.019(2) -0.029(3) O2 0.100(5) 0.069(4) 0.047(3) -0.006(3) 0.029(3) -0.064(3) O3 0.059(3) 0.075(4) 0.085(4) -0.038(3) 0.051(3) -0.027(3) O4 0.042(3) 0.034(2) 0.038(2) -0.0040(19) 0.017(2) -0.0106(19) O5 0.038(2) 0.023(2) 0.045(3) -0.0039(18) 0.016(2) -0.0048(18) O6 0.044(3) 0.041(3) 0.036(3) 0.005(2) 0.005(2) -0.019(2) O7 0.029(2) 0.031(2) 0.047(3) -0.0088(19) 0.017(2) -0.0096(18) O8 0.034(2) 0.033(2) 0.041(3) 0.0027(19) 0.016(2) -0.0069(18) O9 0.157(8) 0.131(7) 0.097(6) -0.001(5) 0.085(6) 0.018(6) O10 0.084(6) 0.203(10) 0.120(7) 0.028(6) 0.018(5) -0.021(6) O11 0.110(8) 0.279(15) 0.199(12) -0.055(10) 0.074(8) 0.028(9) O12 0.164(8) 0.100(6) 0.124(7) -0.006(4) 0.104(7) -0.035(5) N1 0.017(2) 0.029(3) 0.036(3) 0.009(2) 0.011(2) 0.000(2) N2 0.027(3) 0.026(3) 0.035(3) -0.001(2) 0.003(2) -0.001(2) N3 0.056(5) 0.173(10) 0.055(5) 0.016(6) 0.016(4) -0.005(6) N4 0.068(6) 0.169(10) 0.085(7) 0.038(7) 0.028(6) -0.010(6) C1 0.059(5) 0.053(5) 0.056(5) 0.003(4) 0.009(4) -0.011(4) C2 0.088(7) 0.024(4) 0.069(6) 0.012(4) -0.022(5) -0.017(4) C3 0.087(7) 0.037(5) 0.087(8) -0.019(5) -0.019(6) 0.006(5) C4 0.075(7) 0.071(7) 0.123(9) -0.022(6) 0.027(7) 0.037(6) C5 0.066(5) 0.052(5) 0.085(6) 0.007(4) 0.034(5) 0.034(4) C6 0.024(3) 0.040(4) 0.047(4) -0.002(3) -0.009(3) -0.003(3) C7 0.012(3) 0.035(4) 0.038(4) 0.002(3) -0.008(3) -0.003(2) C8 0.039(4) 0.039(4) 0.038(4) 0.000(3) 0.021(3) 0.015(3) C9 0.022(3) 0.055(5) 0.032(4) 0.011(3) -0.002(3) -0.007(3) C10 0.022(3) 0.047(4) 0.033(3) 0.006(3) 0.016(3) 0.004(3) C11 0.028(3) 0.039(4) 0.041(4) 0.008(3) 0.009(3) 0.009(3) C12 0.040(4) 0.025(3) 0.046(4) -0.006(3) 0.014(3) -0.003(3) C13 0.041(4) 0.030(4) 0.035(4) -0.006(3) 0.016(3) -0.010(3) C14 0.027(4) 0.045(4) 0.035(4) 0.011(3) 0.012(3) 0.000(3) C15 0.033(3) 0.034(4) 0.033(3) 0.026(3) 0.012(3) -0.010(3) C16 0.010(3) 0.060(4) 0.024(3) 0.000(3) -0.003(3) 0.010(3) C17 0.034(3) 0.022(3) 0.032(3) 0.009(2) 0.013(3) -0.002(2) C18 0.031(3) 0.035(4) 0.031(3) 0.005(3) 0.012(3) -0.012(3) C19 0.015(3) 0.030(3) 0.042(4) -0.005(3) 0.002(3) -0.005(2) C20 0.073(5) 0.032(4) 0.045(4) 0.007(3) 0.014(4) -0.006(3) C21 0.096(7) 0.039(4) 0.052(5) -0.003(4) 0.026(5) -0.016(4) C22 0.039(4) 0.023(4) 0.092(6) 0.008(4) 0.000(4) 0.000(3) C23 0.044(4) 0.036(4) 0.095(6) -0.011(4) 0.028(4) -0.012(3) C24 0.033(4) 0.037(4) 0.088(6) -0.002(4) 0.025(4) -0.007(3) C25 0.031(3) 0.040(4) 0.036(4) 0.013(3) 0.007(3) 0.002(3) C26 0.033(4) 0.053(4) 0.023(3) 0.015(3) 0.012(3) 0.003(3) C27 0.013(3) 0.053(4) 0.049(4) -0.007(3) -0.005(3) 0.006(3) C28 0.036(4) 0.065(5) 0.042(4) 0.010(4) 0.006(3) 0.029(4) C29 0.041(5) 0.071(6) 0.073(6) -0.012(5) 0.007(4) 0.021(4) C30 0.037(5) 0.090(7) 0.075(6) -0.035(5) 0.009(4) 0.009(4) C31 0.032(4) 0.108(8) 0.057(5) -0.031(5) 0.016(4) -0.005(4) C32 0.022(4) 0.098(7) 0.051(5) -0.014(4) 0.004(3) -0.011(4) C33 0.035(4) 0.086(6) 0.037(4) 0.002(4) 0.017(3) -0.024(4) C34 0.030(4) 0.069(5) 0.039(4) 0.000(4) 0.010(3) -0.013(3) C38 0.071(6) 0.118(8) 0.083(7) -0.016(6) 0.057(5) -0.043(6) C39 0.047(4) 0.060(5) 0.076(6) -0.023(4) 0.033(4) -0.007(4) C40 0.037(4) 0.044(4) 0.046(4) -0.004(3) 0.016(3) -0.004(3) C41 0.026(3) 0.048(4) 0.025(3) -0.017(3) -0.003(3) -0.005(3) C42 0.029(3) 0.028(3) 0.036(4) -0.003(3) 0.010(3) -0.016(3) C43 0.034(4) 0.037(4) 0.033(4) 0.006(3) -0.003(3) -0.002(3) C44 0.041(4) 0.041(4) 0.061(5) 0.006(3) 0.013(4) 0.001(3) C45 0.062(5) 0.013(3) 0.064(5) 0.010(3) 0.004(4) -0.001(3) C46 0.056(5) 0.041(4) 0.051(5) -0.007(3) 0.014(4) -0.011(3) C47 0.031(4) 0.044(4) 0.054(5) 0.004(3) 0.006(3) 0.004(3) C48 0.023(3) 0.021(3) 0.038(4) -0.017(3) 0.002(3) -0.012(2) C49 0.032(3) 0.038(4) 0.035(4) 0.004(3) 0.015(3) -0.003(3) C50 0.022(3) 0.039(4) 0.035(4) -0.004(3) -0.004(3) -0.002(3) C51 0.053(4) 0.033(4) 0.033(4) -0.001(3) 0.013(3) -0.008(3) C52 0.050(4) 0.045(4) 0.038(4) 0.001(3) 0.008(3) -0.007(3) C53 0.054(4) 0.041(4) 0.041(4) -0.012(3) 0.034(3) -0.006(3) C54 0.030(3) 0.041(4) 0.057(4) 0.003(3) 0.024(3) 0.000(3) C55 0.027(3) 0.026(3) 0.046(4) 0.013(3) 0.013(3) -0.011(2) C56 0.030(3) 0.026(3) 0.041(4) -0.002(3) 0.002(3) -0.003(3) B1 0.077(7) 0.034(5) 0.054(6) -0.008(4) 0.042(5) -0.009(4) F1 0.173(9) 0.243(11) 0.228(11) 0.048(9) 0.080(9) 0.084(8) F2 0.223(8) 0.078(4) 0.173(7) -0.032(4) 0.143(7) -0.038(5) F3 0.436(14) 0.115(5) 0.138(6) -0.082(5) 0.221(9) -0.167(7) F4 0.207(8) 0.178(7) 0.067(4) -0.028(4) 0.076(5) -0.102(6) B2 0.054(6) 0.096(9) 0.101(9) -0.023(7) 0.041(6) -0.040(6) F5 0.201(11) 0.187(10) 0.239(14) -0.084(9) -0.008(10) 0.044(8) F6 0.122(6) 0.284(10) 0.103(5) -0.036(6) 0.067(5) -0.108(7) F7 0.127(5) 0.138(5) 0.093(4) -0.034(4) 0.075(4) -0.055(4) F8 0.122(6) 0.326(11) 0.075(4) -0.050(6) 0.068(4) -0.128(7) _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 O1 C34 1.377(9) . ? O1 C35A 1.465(16) . ? O1 C35B 1.469(12) . ? O2 C37 1.395(10) . ? O2 C36B 1.475(10) . ? O2 C36A 1.532(15) . ? O3 C38 1.313(10) . ? O3 C39 1.395(8) . ? O4 C41 1.353(7) . ? O4 C40 1.424(7) . ? O5 C50 1.356(7) . ? O5 C51 1.436(8) . ? O6 C53 1.394(7) . ? O6 C52 1.452(8) . ? O7 C54 1.386(7) . ? O7 C55 1.414(7) . ? O8 C25 1.361(8) . ? O8 C56 1.415(7) . ? O9 N3 1.185(11) . ? O10 N3 1.189(10) . ? O11 N4 1.182(13) . ? O12 N4 1.192(11) . ? N1 C10 1.324(7) . ? N1 C9 1.333(8) . ? N1 C12 1.481(7) . ? N2 C14 1.331(8) . ? N2 C18 1.361(8) . ? N2 C13 1.468(8) . ? N3 C57 1.466(15) . ? N4 C58 1.435(17) . ? C1 C6 1.369(10) . ? C1 C2 1.369(11) . ? C2 C3 1.322(15) . ? C3 C4 1.330(15) . ? C4 C5 1.378(12) . ? C5 C6 1.380(11) . ? C6 C7 1.512(9) . ? C7 C11 1.371(9) . ? C7 C8 1.391(9) . ? C8 C9 1.358(9) . ? C10 C11 1.363(8) . ? C12 C13 1.508(8) . ? C14 C15 1.377(9) . ? C15 C16 1.388(9) . ? C16 C17 1.384(8) . ? C16 C19 1.500(9) . ? C17 C18 1.362(8) . ? C19 C24 1.365(10) . ? C19 C20 1.378(9) . ? C20 C21 1.370(10) . ? C21 C22 1.324(11) . ? C22 C23 1.356(11) . ? C23 C24 1.417(10) . ? C25 C26 1.340(9) . ? C25 C34 1.424(9) . ? C26 C27 1.435(9) . ? C27 C32 1.405(11) . ? C27 C28 1.402(10) . ? C28 C29 1.366(11) . ? C29 C30 1.364(12) . ? C30 C31 1.336(12) . ? C31 C32 1.417(11) . ? C32 C33 1.430(11) . ? C33 C34 1.367(10) . ? C37 C38 1.505(12) . ? C39 C40 1.494(9) . ? C41 C42 1.372(8) . ? C41 C50 1.447(9) . ? C42 C43 1.420(9) . ? C43 C44 1.417(9) . ? C43 C48 1.437(9) . ? C44 C45 1.373(10) . ? C45 C46 1.363(10) . ? C46 C47 1.359(9) . ? C47 C48 1.419(9) . ? C48 C49 1.392(8) . ? C49 C50 1.343(9) . ? C51 C52 1.500(8) . ? C53 C54 1.512(9) . ? C55 C56 1.482(9) . ? B1 F3 1.250(10) . ? B1 F4 1.278(10) . ? B1 F2 1.324(9) . ? B1 F1 1.369(13) . ? B2 F8 1.292(13) . ? B2 F6 1.314(11) . ? B2 F5 1.334(15) . ? B2 F7 1.339(12) . ? C35A C36A 1.44(2) . ? C36B C35B 1.512(14) . ? 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 C34 O1 C35A 129.2(8) . . ? C34 O1 C35B 106.9(7) . . ? C35A O1 C35B 28.2(6) . . ? C37 O2 C36B 123.4(7) . . ? C37 O2 C36A 89.4(8) . . ? C36B O2 C36A 47.0(6) . . ? C38 O3 C39 115.7(6) . . ? C41 O4 C40 114.7(5) . . ? C50 O5 C51 114.9(5) . . ? C53 O6 C52 112.2(5) . . ? C54 O7 C55 112.2(5) . . ? C25 O8 C56 115.1(5) . . ? C10 N1 C9 119.5(5) . . ? C10 N1 C12 121.4(5) . . ? C9 N1 C12 119.1(5) . . ? C14 N2 C18 119.6(5) . . ? C14 N2 C13 120.1(5) . . ? C18 N2 C13 120.3(5) . . ? O9 N3 O10 124.6(13) . . ? O9 N3 C57 117.4(11) . . ? O10 N3 C57 117.8(12) . . ? O11 N4 O12 128.0(12) . . ? O11 N4 C58 119.7(13) . . ? O12 N4 C58 112.2(13) . . ? C6 C1 C2 119.3(9) . . ? C3 C2 C1 123.8(10) . . ? C2 C3 C4 116.3(9) . . ? C3 C4 C5 124.3(11) . . ? C4 C5 C6 117.8(9) . . ? C1 C6 C5 118.3(7) . . ? C1 C6 C7 120.8(7) . . ? C5 C6 C7 120.6(7) . . ? C11 C7 C8 115.8(6) . . ? C11 C7 C6 122.9(6) . . ? C8 C7 C6 121.2(6) . . ? C9 C8 C7 121.2(6) . . ? N1 C9 C8 120.8(6) . . ? N1 C10 C11 121.6(6) . . ? C10 C11 C7 121.0(6) . . ? N1 C12 C13 109.8(4) . . ? N2 C13 C12 110.1(4) . . ? N2 C14 C15 120.8(6) . . ? C14 C15 C16 121.2(5) . . ? C17 C16 C15 116.5(6) . . ? C17 C16 C19 122.6(6) . . ? C15 C16 C19 120.9(6) . . ? C18 C17 C16 121.1(6) . . ? N2 C18 C17 120.9(5) . . ? C24 C19 C20 119.4(6) . . ? C24 C19 C16 119.0(6) . . ? C20 C19 C16 121.6(6) . . ? C21 C20 C19 120.4(8) . . ? C22 C21 C20 120.9(8) . . ? C21 C22 C23 120.6(7) . . ? C22 C23 C24 120.0(8) . . ? C19 C24 C23 118.5(7) . . ? C26 C25 O8 125.0(6) . . ? C26 C25 C34 118.9(7) . . ? O8 C25 C34 116.1(6) . . ? C25 C26 C27 122.7(6) . . ? C32 C27 C28 120.6(7) . . ? C32 C27 C26 117.8(7) . . ? C28 C27 C26 121.5(7) . . ? C29 C28 C27 118.0(8) . . ? C30 C29 C28 122.9(9) . . ? C31 C30 C29 119.2(8) . . ? C30 C31 C32 122.4(9) . . ? C27 C32 C31 116.7(8) . . ? C27 C32 C33 119.5(7) . . ? C31 C32 C33 123.8(8) . . ? C34 C33 C32 120.0(7) . . ? C33 C34 O1 123.6(6) . . ? C33 C34 C25 121.1(7) . . ? O1 C34 C25 115.3(6) . . ? O2 C37 C38 108.4(7) . . ? O3 C38 C37 115.4(7) . . ? O3 C39 C40 116.9(6) . . ? O4 C40 C39 109.0(5) . . ? O4 C41 C42 125.6(6) . . ? O4 C41 C50 115.7(6) . . ? C42 C41 C50 118.6(6) . . ? C41 C42 C43 121.4(6) . . ? C44 C43 C42 122.9(6) . . ? C44 C43 C48 118.4(6) . . ? C42 C43 C48 118.7(5) . . ? C45 C44 C43 120.0(7) . . ? C46 C45 C44 122.2(6) . . ? C47 C46 C45 119.8(7) . . ? C46 C47 C48 122.0(7) . . ? C49 C48 C47 124.0(6) . . ? C49 C48 C43 118.4(6) . . ? C47 C48 C43 117.6(5) . . ? C50 C49 C48 122.8(6) . . ? C49 C50 O5 126.6(6) . . ? C49 C50 C41 120.2(6) . . ? O5 C50 C41 113.2(6) . . ? O5 C51 C52 110.0(5) . . ? O6 C52 C51 109.5(5) . . ? O6 C53 C54 109.9(5) . . ? O7 C54 C53 110.2(5) . . ? O7 C55 C56 111.2(5) . . ? O8 C56 C55 110.0(5) . . ? F3 B1 F4 114.2(8) . . ? F3 B1 F2 112.7(8) . . ? F4 B1 F2 116.8(8) . . ? F3 B1 F1 114.1(11) . . ? F4 B1 F1 100.3(9) . . ? F2 B1 F1 96.8(9) . . ? F8 B2 F6 112.0(10) . . ? F8 B2 F5 104.7(12) . . ? F6 B2 F5 105.1(11) . . ? F8 B2 F7 116.5(9) . . ? F6 B2 F7 113.7(10) . . ? F5 B2 F7 103.2(11) . . ? C36A C35A O1 110.2(12) . . ? C35A C36A O2 99.8(11) . . ? O2 C36B C35B 108.5(8) . . ? O1 C35B C36B 100.7(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.437 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.066 # Attachment 'New-L5.cif' data_[2]pseudorotaxane_[(1,2-bis(4-ethylacetylpyridinium)ethane)-DB24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H60 B2 F8 N4 O12' _chemical_formula_weight 1034.60 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.2421(4) _cell_length_b 15.7037(5) _cell_length_c 12.1739(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.9090(10) _cell_angle_gamma 90.00 _cell_volume 2522.28(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.220748 _exptl_absorpt_correction_T_max 0.492089 _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 'Bruker APEX 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 12358 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4399 _reflns_number_gt 2253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.1676P)^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 0.022(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4399 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1625 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.3025 _refine_ls_wR_factor_gt 0.2672 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _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 O1 O 0.9177(3) -0.1237(3) -0.2153(4) 0.0837(12) Uani 1 1 d . . . O2 O 0.9872(3) -0.1011(4) -0.0460(4) 0.133(2) Uani 1 1 d . . . O3 O 0.2878(2) -0.1361(2) 0.0947(2) 0.0563(9) Uani 1 1 d . . . O4 O 0.3091(3) -0.1442(2) -0.1437(3) 0.0667(10) Uani 1 1 d . . . O5 O 0.5859(2) 0.0261(2) 0.2590(2) 0.0641(10) Uani 1 1 d . . . O6 O 0.4027(3) -0.0752(2) 0.2588(3) 0.0692(10) Uani 1 1 d . . . N1 N 0.6184(3) -0.0598(2) -0.0242(3) 0.0444(9) Uani 1 1 d . . . N2 N 0.8410(8) -0.0299(7) 0.3346(11) 0.208(5) Uani 1 1 d . . . C1 C 0.9970(7) -0.1601(7) -0.3732(7) 0.152(4) Uani 1 1 d . . . H1A H 1.0595 -0.1735 -0.4038 0.229 Uiso 1 1 calc R . . H1B H 0.9672 -0.1107 -0.4094 0.229 Uiso 1 1 calc R . . H1C H 0.9512 -0.2074 -0.3838 0.229 Uiso 1 1 calc R . . C2 C 1.0169(5) -0.1427(6) -0.2542(7) 0.115(3) Uani 1 1 d . . . H2A H 1.0472 -0.1919 -0.2162 0.138 Uiso 1 1 calc R . . H2B H 1.0624 -0.0945 -0.2418 0.138 Uiso 1 1 calc R . . C3 C 0.9156(4) -0.1040(4) -0.1115(5) 0.0746(16) Uani 1 1 d . . . C4 C 0.8079(3) -0.0874(3) -0.0834(4) 0.0540(12) Uani 1 1 d . . . C5 C 0.7942(3) -0.0571(3) 0.0196(4) 0.0599(13) Uani 1 1 d . . . H5A H 0.8497 -0.0457 0.0695 0.072 Uiso 1 1 calc R . . C6 C 0.6970(3) -0.0437(3) 0.0486(4) 0.0548(12) Uani 1 1 d . . . H6A H 0.6864 -0.0235 0.1185 0.066 Uiso 1 1 calc R . . C7 C 0.6326(3) -0.0875(3) -0.1252(4) 0.0529(12) Uani 1 1 d . . . H7A H 0.5768 -0.0971 -0.1754 0.063 Uiso 1 1 calc R . . C8 C 0.7278(3) -0.1018(3) -0.1560(4) 0.0525(12) Uani 1 1 d . . . H8A H 0.7371 -0.1214 -0.2265 0.063 Uiso 1 1 calc R . . C9 C 0.5133(3) -0.0466(3) 0.0073(4) 0.0498(11) Uani 1 1 d . . . H9A H 0.5088 -0.0634 0.0834 0.060 Uiso 1 1 calc R . . H9B H 0.4661 -0.0812 -0.0390 0.060 Uiso 1 1 calc R . . C10 C 0.3035(4) -0.0818(3) 0.2735(4) 0.0580(13) Uani 1 1 d . . . C11 C 0.2588(6) -0.0564(4) 0.3704(5) 0.0826(18) Uani 1 1 d . . . H11A H 0.2993 -0.0333 0.4291 0.099 Uiso 1 1 calc R . . C12 C 0.1570(6) -0.0655(5) 0.3785(6) 0.098(2) Uani 1 1 d . . . H12A H 0.1289 -0.0493 0.4427 0.118 Uiso 1 1 calc R . . C13 C 0.0982(5) -0.0976(5) 0.2945(6) 0.096(2) Uani 1 1 d . . . H13A H 0.0293 -0.1048 0.3011 0.115 Uiso 1 1 calc R . . C14 C 0.1381(4) -0.1202(4) 0.1985(5) 0.0765(16) Uani 1 1 d . . . H14A H 0.0954 -0.1402 0.1395 0.092 Uiso 1 1 calc R . . C15 C 0.2425(4) -0.1134(3) 0.1881(4) 0.0587(13) Uani 1 1 d . . . C16 C 0.2283(4) -0.1839(4) 0.0154(4) 0.0688(14) Uani 1 1 d . . . H16A H 0.1729 -0.1492 -0.0169 0.083 Uiso 1 1 calc R . . H16B H 0.1997 -0.2329 0.0502 0.083 Uiso 1 1 calc R . . C17 C 0.2933(4) -0.2128(3) -0.0727(4) 0.0657(14) Uani 1 1 d . . . H17A H 0.3580 -0.2332 -0.0393 0.079 Uiso 1 1 calc R . . H17B H 0.2603 -0.2592 -0.1143 0.079 Uiso 1 1 calc R . . C18 C 0.3625(5) -0.1700(4) -0.2339(4) 0.0761(17) Uani 1 1 d . . . H18A H 0.3285 -0.2180 -0.2711 0.091 Uiso 1 1 calc R . . H18B H 0.4307 -0.1875 -0.2079 0.091 Uiso 1 1 calc R . . C19 C 0.6333(4) 0.0968(4) 0.3120(4) 0.0796(18) Uani 1 1 d . . . H19A H 0.7015 0.0814 0.3404 0.096 Uiso 1 1 calc R . . H19B H 0.5961 0.1135 0.3738 0.096 Uiso 1 1 calc R . . C20 C 0.5681(5) -0.0456(5) 0.3265(5) 0.088(2) Uani 1 1 d . . . H20A H 0.5859 -0.0967 0.2877 0.106 Uiso 1 1 calc R . . H20B H 0.6134 -0.0419 0.3933 0.106 Uiso 1 1 calc R . . C21 C 0.4692(5) -0.0549(5) 0.3565(4) 0.0881(19) Uani 1 1 d . . . H21A H 0.4472 -0.0026 0.3893 0.106 Uiso 1 1 calc R . . H21B H 0.4667 -0.1002 0.4104 0.106 Uiso 1 1 calc R . . C22 C 0.8220(7) -0.1053(9) 0.3391(9) 0.140(3) Uani 1 1 d . . . C23 C 0.8024(8) -0.1858(7) 0.3413(10) 0.159(4) Uani 1 1 d . . . H23A H 0.7755 -0.2040 0.2695 0.191 Uiso 1 1 calc R . . H23B H 0.7535 -0.1964 0.3936 0.191 Uiso 1 1 calc R . . H23C H 0.8635 -0.2167 0.3627 0.191 Uiso 1 1 calc R . . B1 B 0.6204(6) -0.2214(5) -0.4193(6) 0.0702(18) Uani 1 1 d . . . F1 F 0.5689(4) -0.2475(3) -0.5125(5) 0.168(2) Uani 1 1 d . . . F2 F 0.6224(14) -0.1409(6) -0.4105(13) 0.162(7) Uani 0.67 1 d P . . F2A F 0.583(2) -0.168(2) -0.366(3) 0.178(16) Uani 0.33 1 d P . . F3 F 0.7144(11) -0.2569(11) -0.4067(15) 0.177(5) Uani 0.67 1 d P . . F3A F 0.7072(17) -0.192(3) -0.465(3) 0.247(15) Uani 0.33 1 d P . . F4 F 0.5820(13) -0.2561(17) -0.3320(15) 0.244(8) Uani 0.67 1 d P . . F4A F 0.650(3) -0.2849(11) -0.3599(15) 0.125(7) Uani 0.33 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 O1 0.059(2) 0.103(3) 0.092(3) 0.001(2) 0.030(2) 0.019(2) O2 0.049(2) 0.214(6) 0.135(4) -0.030(4) -0.001(3) 0.034(3) O3 0.0549(19) 0.063(2) 0.0518(18) -0.0029(16) 0.0066(15) -0.0111(16) O4 0.083(2) 0.061(2) 0.0578(19) -0.0070(17) 0.0176(17) -0.0153(19) O5 0.069(2) 0.077(2) 0.0454(17) 0.0012(17) -0.0006(15) -0.0160(19) O6 0.076(2) 0.070(2) 0.060(2) 0.0056(17) -0.0060(18) -0.0136(19) N1 0.045(2) 0.043(2) 0.045(2) 0.0010(16) 0.0058(16) 0.0041(17) N2 0.188(9) 0.117(7) 0.323(13) 0.019(9) 0.040(9) 0.004(7) C1 0.143(7) 0.189(10) 0.136(7) 0.023(6) 0.080(6) 0.070(7) C2 0.073(4) 0.131(7) 0.149(7) 0.004(5) 0.053(4) 0.018(4) C3 0.050(3) 0.086(4) 0.089(4) 0.001(3) 0.014(3) 0.011(3) C4 0.046(3) 0.048(3) 0.068(3) 0.010(2) 0.007(2) 0.007(2) C5 0.048(3) 0.069(3) 0.062(3) -0.006(3) -0.003(2) 0.004(2) C6 0.056(3) 0.058(3) 0.049(3) -0.009(2) -0.001(2) 0.006(2) C7 0.052(3) 0.057(3) 0.049(3) 0.003(2) 0.001(2) 0.000(2) C8 0.056(3) 0.056(3) 0.046(2) 0.003(2) 0.012(2) 0.007(2) C9 0.051(3) 0.052(3) 0.049(2) 0.004(2) 0.015(2) 0.006(2) C10 0.070(3) 0.045(3) 0.058(3) 0.008(2) 0.002(3) -0.008(3) C11 0.119(5) 0.062(4) 0.066(4) 0.004(3) 0.002(3) -0.005(4) C12 0.113(6) 0.088(5) 0.099(5) -0.009(4) 0.043(4) 0.004(4) C13 0.085(4) 0.101(5) 0.105(5) 0.005(4) 0.035(4) 0.017(4) C14 0.062(3) 0.083(4) 0.085(4) 0.006(3) 0.007(3) 0.004(3) C15 0.064(3) 0.051(3) 0.062(3) 0.011(2) 0.013(3) -0.004(3) C16 0.077(3) 0.062(3) 0.067(3) -0.002(3) 0.005(3) -0.016(3) C17 0.076(3) 0.053(3) 0.070(3) -0.009(3) 0.016(3) -0.010(3) C18 0.098(4) 0.070(4) 0.062(3) -0.025(3) 0.020(3) -0.020(3) C19 0.089(4) 0.106(5) 0.044(3) -0.022(3) 0.007(3) -0.035(4) C20 0.075(4) 0.117(5) 0.069(3) 0.032(3) -0.011(3) -0.020(4) C21 0.091(5) 0.103(5) 0.067(4) 0.018(3) -0.008(3) -0.015(4) C22 0.110(7) 0.136(9) 0.177(9) 0.014(8) 0.028(6) 0.034(7) C23 0.147(8) 0.097(7) 0.230(11) -0.011(7) -0.001(7) 0.004(6) B1 0.075(5) 0.061(5) 0.074(4) -0.013(4) -0.001(4) 0.004(4) F1 0.205(5) 0.125(4) 0.162(4) -0.051(3) -0.051(4) 0.018(4) F2 0.232(19) 0.053(4) 0.182(11) -0.014(6) -0.081(11) 0.006(7) F2A 0.174(19) 0.18(3) 0.19(3) -0.14(3) 0.038(17) 0.04(2) F3 0.138(9) 0.189(13) 0.201(12) 0.025(9) -0.011(8) 0.057(8) F3A 0.106(13) 0.31(4) 0.33(3) 0.16(3) 0.042(17) -0.010(18) F4 0.244(15) 0.26(2) 0.238(14) 0.123(13) 0.097(12) 0.052(14) F4A 0.19(2) 0.090(10) 0.093(10) 0.023(8) -0.002(12) 0.054(14) _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 O1 C3 1.304(7) . ? O1 C2 1.464(7) . ? O2 C3 1.187(6) . ? O3 C15 1.378(5) . ? O3 C16 1.409(5) . ? O4 C17 1.408(6) . ? O4 C18 1.416(6) . ? O5 C19 1.404(6) . ? O5 C20 1.426(7) . ? O6 C10 1.344(6) . ? O6 C21 1.454(6) . ? N1 C7 1.333(5) . ? N1 C6 1.332(5) . ? N1 C9 1.490(5) . ? N2 C22 1.211(14) . ? C1 C2 1.475(11) . ? C3 C4 1.517(7) . ? C4 C8 1.340(6) . ? C4 C5 1.367(6) . ? C5 C6 1.379(6) . ? C7 C8 1.365(6) . ? C9 C9 1.513(9) 3_655 ? C10 C15 1.355(7) . ? C10 C11 1.421(8) . ? C11 C12 1.367(9) . ? C12 C13 1.330(9) . ? C13 C14 1.369(8) . ? C14 C15 1.403(7) . ? C16 C17 1.503(7) . ? C18 C19 1.496(8) 3_655 ? C19 C18 1.496(8) 3_655 ? C20 C21 1.396(8) . ? C22 C23 1.291(15) . ? B1 F2A 1.194(19) . ? B1 F2 1.268(12) . ? B1 F4A 1.273(17) . ? B1 F4 1.333(15) . ? B1 F1 1.337(7) . ? B1 F3 1.361(12) . ? B1 F3A 1.40(2) . ? F2 F2A 0.89(3) . ? F2 F3A 1.57(4) . ? F2A F4 1.44(3) . ? F3 F4A 1.15(3) . ? F3 F3A 1.24(3) . ? F4 F4A 1.08(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 C3 O1 C2 117.1(5) . . ? C15 O3 C16 116.4(4) . . ? C17 O4 C18 111.5(4) . . ? C19 O5 C20 116.7(4) . . ? C10 O6 C21 116.0(4) . . ? C7 N1 C6 120.8(4) . . ? C7 N1 C9 119.4(3) . . ? C6 N1 C9 119.8(4) . . ? O1 C2 C1 105.3(6) . . ? O2 C3 O1 125.3(5) . . ? O2 C3 C4 123.6(6) . . ? O1 C3 C4 111.0(5) . . ? C8 C4 C5 120.2(4) . . ? C8 C4 C3 121.9(5) . . ? C5 C4 C3 117.9(4) . . ? C4 C5 C6 119.2(4) . . ? N1 C6 C5 119.6(4) . . ? N1 C7 C8 120.9(4) . . ? C4 C8 C7 119.2(4) . . ? N1 C9 C9 108.5(4) . 3_655 ? O6 C10 C15 116.8(4) . . ? O6 C10 C11 124.8(5) . . ? C15 C10 C11 118.4(5) . . ? C12 C11 C10 120.9(6) . . ? C13 C12 C11 120.0(6) . . ? C12 C13 C14 120.7(6) . . ? C13 C14 C15 120.8(6) . . ? C10 C15 O3 117.0(4) . . ? C10 C15 C14 119.1(5) . . ? O3 C15 C14 123.9(5) . . ? O3 C16 C17 109.1(4) . . ? O4 C17 C16 109.3(4) . . ? O4 C18 C19 108.7(5) . 3_655 ? O5 C19 C18 110.8(4) . 3_655 ? C21 C20 O5 116.0(5) . . ? C20 C21 O6 109.0(5) . . ? N2 C22 C23 178.5(14) . . ? F2A B1 F2 42.4(17) . . ? F2A B1 F4A 111(2) . . ? F2 B1 F4A 136.8(12) . . ? F2A B1 F4 69.3(19) . . ? F2 B1 F4 110.2(13) . . ? F4A B1 F4 49.1(12) . . ? F2A B1 F1 118.3(17) . . ? F2 B1 F1 112.5(8) . . ? F4A B1 F1 110.6(11) . . ? F4 B1 F1 110.5(11) . . ? F2A B1 F3 130.0(17) . . ? F2 B1 F3 112.8(11) . . ? F4A B1 F3 51.9(13) . . ? F4 B1 F3 98.7(11) . . ? F1 B1 F3 111.4(8) . . ? F2A B1 F3A 112(2) . . ? F2 B1 F3A 72.2(19) . . ? F4A B1 F3A 105.2(19) . . ? F4 B1 F3A 146.5(15) . . ? F1 B1 F3A 98.1(15) . . ? F3 B1 F3A 53.4(14) . . ? F2A F2 B1 64.3(16) . . ? F2A F2 F3A 119(2) . . ? B1 F2 F3A 57.7(13) . . ? F2 F2A B1 73.2(18) . . ? F2 F2A F4 131(3) . . ? B1 F2A F4 59.9(14) . . ? F4A F3 F3A 124.8(19) . . ? F4A F3 B1 60.1(11) . . ? F3A F3 B1 64.8(12) . . ? F3 F3A B1 61.9(12) . . ? F3 F3A F2 101.7(18) . . ? B1 F3A F2 50.1(11) . . ? F4A F4 B1 62.5(12) . . ? F4A F4 F2A 106(2) . . ? B1 F4 F2A 50.8(10) . . ? F4 F4A F3 132(2) . . ? F4 F4A B1 68.3(13) . . ? F3 F4A B1 68.0(14) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.560 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.071 # Attachment 'New-L6.cif' data_[2]pseudorotaxane_[(1,2-bis(3-ethylacetylpyridinium)ethane)-DB24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H60 B2 F8 N4 O16' _chemical_formula_weight 1074.58 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.33570(10) _cell_length_b 22.4319(3) _cell_length_c 25.0932(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5254.96(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.153867 _exptl_absorpt_correction_T_max 0.492068 _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 'Bruker APEX 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 16397 _diffrn_reflns_av_R_equivalents 0.1401 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 20.81 _reflns_number_total 2752 _reflns_number_gt 2174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.0819P)^2^+20.0743P] 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 0.0033(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2752 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1786 _refine_ls_R_factor_gt 0.1437 _refine_ls_wR_factor_ref 0.3084 _refine_ls_wR_factor_gt 0.2894 _refine_ls_goodness_of_fit_ref 1.293 _refine_ls_restrained_S_all 1.293 _refine_ls_shift/su_max 0.005 _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 O1 O 0.2855(8) 0.1350(4) 0.3477(3) 0.078(2) Uani 1 1 d . . . O2 O 0.0827(10) 0.1771(4) 0.3754(3) 0.099(3) Uani 1 1 d . . . O3 O 0.4659(7) 0.1617(3) 0.5303(3) 0.0568(19) Uani 1 1 d . . . O4 O 0.5832(7) -0.0820(3) 0.3757(3) 0.0579(19) Uani 1 1 d . . . O5 O 0.6437(7) 0.0412(3) 0.3833(3) 0.066(2) Uani 1 1 d . . . O6 O 0.6000(7) 0.1508(3) 0.4393(3) 0.064(2) Uani 1 1 d . . . O7 O 0.054(2) 0.2103(7) 0.7411(7) 0.230(8) Uani 1 1 d . . . O8 O 0.2363(18) 0.2272(7) 0.6940(6) 0.189(6) Uani 1 1 d . . . N1 N 0.3228(7) 0.0350(3) 0.4829(3) 0.0401(19) Uani 1 1 d . . . N2 N 0.1664(17) 0.1931(9) 0.7227(5) 0.128(5) Uani 1 1 d . . . C1 C 0.3687(19) 0.1433(9) 0.2603(6) 0.146(7) Uani 1 1 d . . . H1A H 0.3544 0.1631 0.2267 0.220 Uiso 1 1 calc R . . H1B H 0.3547 0.1012 0.2558 0.220 Uiso 1 1 calc R . . H1C H 0.4644 0.1507 0.2726 0.220 Uiso 1 1 calc R . . C2 C 0.2736(18) 0.1645(8) 0.2964(5) 0.125(6) Uani 1 1 d . . . H2A H 0.1773 0.1591 0.2827 0.150 Uiso 1 1 calc R . . H2B H 0.2893 0.2069 0.3011 0.150 Uiso 1 1 calc R . . C3 C 0.1850(13) 0.1447(5) 0.3828(5) 0.068(3) Uani 1 1 d . . . C4 C 0.2045(10) 0.1101(4) 0.4334(4) 0.048(3) Uani 1 1 d . . . C5 C 0.1187(11) 0.1216(5) 0.4763(5) 0.065(3) Uani 1 1 d . . . H5A H 0.0515 0.1521 0.4746 0.078 Uiso 1 1 calc R . . C6 C 0.1315(11) 0.0884(5) 0.5216(5) 0.068(3) Uani 1 1 d . . . H6A H 0.0703 0.0948 0.5503 0.082 Uiso 1 1 calc R . . C7 C 0.2362(11) 0.0453(4) 0.5243(4) 0.053(3) Uani 1 1 d . . . H7A H 0.2469 0.0231 0.5554 0.063 Uiso 1 1 calc R . . C8 C 0.3088(10) 0.0679(4) 0.4376(4) 0.049(3) Uani 1 1 d . . . H8A H 0.3712 0.0616 0.4093 0.058 Uiso 1 1 calc R . . C9 C 0.4330(8) -0.0124(4) 0.4864(4) 0.047(3) Uani 1 1 d . . . H9A H 0.4570 -0.0265 0.4510 0.056 Uiso 1 1 calc R . . H9B H 0.3961 -0.0458 0.5068 0.056 Uiso 1 1 calc R . . C10 C 0.5096(11) 0.1991(5) 0.4450(4) 0.056(3) Uani 1 1 d . . . C11 C 0.4895(12) 0.2439(6) 0.4055(4) 0.071(3) Uani 1 1 d . . . H11A H 0.5384 0.2420 0.3733 0.085 Uiso 1 1 calc R . . C12 C 0.3952(13) 0.2910(5) 0.4159(7) 0.083(4) Uani 1 1 d . . . H12A H 0.3801 0.3201 0.3902 0.099 Uiso 1 1 calc R . . C13 C 0.3252(13) 0.2945(6) 0.4635(6) 0.077(4) Uani 1 1 d . . . H13A H 0.2628 0.3260 0.4702 0.092 Uiso 1 1 calc R . . C14 C 0.3464(11) 0.2523(5) 0.5010(5) 0.064(3) Uani 1 1 d . . . H14A H 0.2973 0.2549 0.5332 0.076 Uiso 1 1 calc R . . C15 C 0.4395(10) 0.2053(5) 0.4927(4) 0.051(3) Uani 1 1 d . . . C16 C 0.4333(12) 0.1784(5) 0.5850(4) 0.068(3) Uani 1 1 d . . . H16A H 0.3305 0.1785 0.5905 0.081 Uiso 1 1 calc R . . H16B H 0.4693 0.2181 0.5923 0.081 Uiso 1 1 calc R . . C17 C 0.4957(12) -0.1332(5) 0.3770(4) 0.065(3) Uani 1 1 d . . . H17A H 0.4872 -0.1501 0.3416 0.078 Uiso 1 1 calc R . . H17B H 0.4007 -0.1230 0.3897 0.078 Uiso 1 1 calc R . . C18 C 0.5366(11) -0.0400(5) 0.3362(4) 0.068(3) Uani 1 1 d . . . H18A H 0.4419 -0.0253 0.3452 0.082 Uiso 1 1 calc R . . H18B H 0.5316 -0.0593 0.3017 0.082 Uiso 1 1 calc R . . C19 C 0.6408(11) 0.0110(5) 0.3341(4) 0.065(3) Uani 1 1 d . . . H19A H 0.7357 -0.0040 0.3259 0.078 Uiso 1 1 calc R . . H19B H 0.6129 0.0384 0.3061 0.078 Uiso 1 1 calc R . . C20 C 0.7433(12) 0.0901(5) 0.3866(5) 0.085(4) Uani 1 1 d . . . H20A H 0.8044 0.0843 0.4174 0.102 Uiso 1 1 calc R . . H20B H 0.8039 0.0896 0.3552 0.102 Uiso 1 1 calc R . . C21 C 0.6774(12) 0.1457(5) 0.3905(5) 0.085(4) Uani 1 1 d . . . H21A H 0.6123 0.1510 0.3607 0.102 Uiso 1 1 calc R . . H21B H 0.7495 0.1767 0.3887 0.102 Uiso 1 1 calc R . . C22 C 0.214(2) 0.1351(7) 0.7354(8) 0.159(8) Uani 1 1 d . . . H22A H 0.1449 0.1160 0.7581 0.239 Uiso 1 1 calc R . . H22B H 0.3044 0.1374 0.7535 0.239 Uiso 1 1 calc R . . H22C H 0.2247 0.1123 0.7032 0.239 Uiso 1 1 calc R . . B1 B 0.9107(19) 0.0315(9) 0.6483(8) 0.085(5) Uani 1 1 d . . . F1 F 0.8210(10) 0.0452(4) 0.6061(4) 0.154(4) Uani 1 1 d . . . F2 F 0.975(4) 0.0770(11) 0.6684(14) 0.167(11) Uani 0.50 1 d P . . F2A F 0.855(4) 0.063(3) 0.6870(14) 0.27(2) Uani 0.50 1 d P . . F3 F 0.822(3) 0.004(2) 0.679(2) 0.201(19) Uani 0.50 1 d P . . F3A F 0.918(6) -0.018(2) 0.673(2) 0.24(2) Uani 0.50 1 d P . . F4 F 0.992(3) -0.0048(13) 0.6212(11) 0.155(12) Uani 0.50 1 d P . . F4A F 1.041(2) 0.051(3) 0.6386(13) 0.21(2) Uani 0.50 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 O1 0.070(5) 0.098(6) 0.066(5) 0.014(5) -0.001(4) 0.012(5) O2 0.096(6) 0.092(6) 0.108(7) 0.023(5) -0.012(5) 0.042(6) O3 0.059(4) 0.055(4) 0.057(4) -0.007(4) 0.012(3) 0.000(4) O4 0.056(4) 0.064(5) 0.054(4) 0.006(4) -0.004(3) -0.014(4) O5 0.068(5) 0.065(5) 0.065(5) -0.023(4) 0.031(4) -0.012(4) O6 0.057(4) 0.063(5) 0.071(5) -0.014(4) 0.023(4) -0.002(4) O7 0.241(19) 0.202(15) 0.246(17) -0.008(13) 0.093(15) 0.070(14) O8 0.213(14) 0.200(14) 0.154(12) 0.068(11) 0.041(11) -0.011(11) N1 0.031(4) 0.047(5) 0.042(5) -0.007(4) -0.006(4) 0.003(4) N2 0.116(12) 0.184(18) 0.085(9) -0.024(10) 0.026(8) 0.003(12) C1 0.131(14) 0.24(2) 0.070(11) 0.025(12) -0.010(10) 0.024(14) C2 0.145(14) 0.168(15) 0.061(9) 0.057(10) -0.015(10) 0.020(12) C3 0.067(8) 0.057(7) 0.080(9) -0.010(7) -0.019(7) 0.028(7) C4 0.033(6) 0.061(7) 0.050(7) 0.005(6) -0.010(5) 0.000(6) C5 0.050(7) 0.051(7) 0.093(9) -0.003(7) 0.001(7) 0.023(5) C6 0.052(7) 0.072(8) 0.080(9) 0.003(7) 0.020(6) 0.014(6) C7 0.051(6) 0.051(6) 0.056(7) -0.002(5) 0.009(6) 0.001(6) C8 0.034(6) 0.060(7) 0.051(7) -0.006(6) -0.010(5) -0.007(5) C9 0.037(5) 0.039(5) 0.065(7) -0.007(5) 0.001(5) 0.014(5) C10 0.046(6) 0.062(7) 0.060(8) -0.018(7) 0.009(6) -0.015(6) C11 0.070(8) 0.092(10) 0.050(7) 0.011(7) -0.006(6) -0.025(8) C12 0.062(8) 0.046(8) 0.140(14) 0.002(8) -0.054(9) -0.008(7) C13 0.061(8) 0.080(10) 0.090(10) 0.000(9) -0.012(8) 0.004(7) C14 0.050(7) 0.064(7) 0.077(8) 0.000(7) -0.012(6) 0.003(6) C15 0.037(6) 0.055(7) 0.062(7) 0.010(6) -0.005(5) -0.007(6) C16 0.083(8) 0.056(7) 0.064(8) -0.008(6) 0.013(6) -0.009(6) C17 0.085(8) 0.058(7) 0.053(7) -0.008(6) 0.003(6) -0.037(7) C18 0.060(7) 0.078(8) 0.066(8) -0.012(7) 0.006(6) 0.000(7) C19 0.061(7) 0.073(8) 0.061(8) 0.023(7) 0.008(6) -0.004(6) C20 0.055(7) 0.071(8) 0.130(11) -0.007(8) 0.044(7) -0.014(7) C21 0.068(8) 0.082(9) 0.105(10) -0.029(8) 0.043(7) -0.009(7) C22 0.163(17) 0.083(12) 0.23(2) 0.012(13) 0.057(15) 0.042(12) B1 0.064(12) 0.082(13) 0.109(15) 0.009(13) 0.016(12) -0.009(12) F1 0.113(7) 0.159(8) 0.191(10) 0.014(7) -0.045(7) -0.010(6) F2 0.16(3) 0.142(18) 0.20(3) -0.055(18) -0.02(2) -0.09(2) F2A 0.13(2) 0.45(6) 0.23(3) -0.22(4) 0.07(2) -0.04(4) F3 0.111(19) 0.22(4) 0.27(4) 0.10(3) -0.01(2) -0.09(2) F3A 0.27(5) 0.23(4) 0.23(4) 0.13(3) 0.05(4) 0.03(4) F4 0.101(15) 0.16(2) 0.21(3) -0.11(2) -0.041(16) 0.072(15) F4A 0.055(13) 0.45(7) 0.13(2) 0.10(3) -0.007(12) -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 O1 C3 1.306(12) . ? O1 C2 1.452(13) . ? O2 C3 1.214(12) . ? O3 C15 1.381(11) . ? O3 C16 1.456(11) . ? O4 C17 1.410(11) . ? O4 C18 1.435(12) . ? O5 C19 1.410(11) . ? O5 C20 1.440(12) . ? O6 C10 1.382(11) . ? O6 C21 1.426(12) . ? O7 N2 1.212(16) . ? O8 N2 1.236(16) . ? N1 C7 1.338(11) . ? N1 C8 1.361(11) . ? N1 C9 1.483(10) . ? N2 C22 1.41(2) . ? C1 C2 1.355(18) . ? C3 C4 1.500(14) . ? C4 C8 1.362(12) . ? C4 C5 1.366(13) . ? C5 C6 1.365(14) . ? C6 C7 1.375(13) . ? C9 C9 1.529(16) 5_656 ? C10 C15 1.370(13) . ? C10 C11 1.424(14) . ? C11 C12 1.399(15) . ? C12 C13 1.364(16) . ? C13 C14 1.349(15) . ? C14 C15 1.383(14) . ? C16 C17 1.540(14) 5_656 ? C17 C16 1.540(14) 5_656 ? C18 C19 1.501(13) . ? C20 C21 1.394(14) . ? B1 F3A 1.27(4) . ? B1 F2 1.29(3) . ? B1 F3 1.29(4) . ? B1 F4 1.30(2) . ? B1 F2A 1.30(3) . ? B1 F4A 1.31(3) . ? B1 F1 1.38(2) . ? F2 F4A 1.14(4) . ? F2 F2A 1.25(4) . ? F2A F3 1.37(6) . ? F3 F3A 1.03(5) . ? F3A F4 1.50(5) . ? F4 F4A 1.40(5) . ? 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 C3 O1 C2 117.9(10) . . ? C15 O3 C16 115.2(8) . . ? C17 O4 C18 112.0(8) . . ? C19 O5 C20 115.4(8) . . ? C10 O6 C21 117.5(9) . . ? C7 N1 C8 119.8(8) . . ? C7 N1 C9 119.8(8) . . ? C8 N1 C9 120.4(8) . . ? O7 N2 O8 119(2) . . ? O7 N2 C22 118.6(18) . . ? O8 N2 C22 122.3(16) . . ? C1 C2 O1 112.5(13) . . ? O2 C3 O1 124.1(11) . . ? O2 C3 C4 122.4(12) . . ? O1 C3 C4 113.4(9) . . ? C8 C4 C5 119.3(9) . . ? C8 C4 C3 120.8(10) . . ? C5 C4 C3 119.8(10) . . ? C6 C5 C4 120.2(9) . . ? C5 C6 C7 119.0(10) . . ? N1 C7 C6 120.9(10) . . ? N1 C8 C4 120.7(9) . . ? N1 C9 C9 109.4(8) . 5_656 ? C15 C10 O6 117.5(10) . . ? C15 C10 C11 118.2(10) . . ? O6 C10 C11 124.2(10) . . ? C12 C11 C10 119.0(11) . . ? C13 C12 C11 120.6(12) . . ? C14 C13 C12 120.0(12) . . ? C13 C14 C15 121.4(11) . . ? C10 C15 O3 116.1(9) . . ? C10 C15 C14 120.7(10) . . ? O3 C15 C14 123.3(10) . . ? O3 C16 C17 108.9(8) . 5_656 ? O4 C17 C16 107.5(8) . 5_656 ? O4 C18 C19 109.2(8) . . ? O5 C19 C18 110.3(8) . . ? C21 C20 O5 113.6(9) . . ? C20 C21 O6 110.8(11) . . ? F3A B1 F2 118(4) . . ? F3A B1 F3 48(2) . . ? F2 B1 F3 117(4) . . ? F3A B1 F4 71(3) . . ? F2 B1 F4 116(2) . . ? F3 B1 F4 112(3) . . ? F3A B1 F2A 97(4) . . ? F2 B1 F2A 58(2) . . ? F3 B1 F2A 64(3) . . ? F4 B1 F2A 163(3) . . ? F3A B1 F4A 109(3) . . ? F2 B1 F4A 52(2) . . ? F3 B1 F4A 150(3) . . ? F4 B1 F4A 64(2) . . ? F2A B1 F4A 110(3) . . ? F3A B1 F1 127(3) . . ? F2 B1 F1 114(2) . . ? F3 B1 F1 100(2) . . ? F4 B1 F1 95.3(18) . . ? F2A B1 F1 102(2) . . ? F4A B1 F1 110.5(18) . . ? F4A F2 F2A 127(4) . . ? F4A F2 B1 65(2) . . ? F2A F2 B1 61.7(19) . . ? F2 F2A B1 60.3(18) . . ? F2 F2A F3 113(4) . . ? B1 F2A F3 58(3) . . ? F3A F3 B1 65(4) . . ? F3A F3 F2A 106(5) . . ? B1 F3 F2A 58.7(19) . . ? F3 F3A B1 67(4) . . ? F3 F3A F4 116(6) . . ? B1 F3A F4 55(2) . . ? B1 F4 F4A 58.2(15) . . ? B1 F4 F3A 53.3(19) . . ? F4A F4 F3A 93(3) . . ? F2 F4A B1 62.7(17) . . ? F2 F4A F4 119(3) . . ? B1 F4A F4 57.3(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.257 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.062 # Attachment 'New-L7.cif' data_[2]pseudorotaxane_[(1,2-bis(3-methoxypyridinium)ethane)-24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H50 B2 F8 N2 O10' _chemical_formula_weight 772.34 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.4924(6) _cell_length_b 16.5364(10) _cell_length_c 10.7738(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.5840(10) _cell_angle_gamma 90.00 _cell_volume 1857.00(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.871299 _exptl_absorpt_correction_T_max 1.000000 _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 'Bruker APEX 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 14875 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6537 _reflns_number_gt 5684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.1379P)^2^+1.4729P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.8(14) _refine_ls_number_reflns 6537 _refine_ls_number_parameters 477 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2357 _refine_ls_wR_factor_gt 0.2265 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.011 _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 O1 O 0.8322(3) 0.0569(2) 1.1068(3) 0.0519(8) Uani 1 1 d . . . O2 O 0.6974(3) 0.4793(2) 0.4043(3) 0.0499(8) Uani 1 1 d . . . O3 O 1.0880(3) 0.2229(2) 0.8867(4) 0.0595(9) Uani 1 1 d . A . O4 O 1.0822(4) 0.2047(2) 0.6248(4) 0.0650(10) Uani 1 1 d . . . O5 O 0.8496(5) 0.2151(4) 0.4370(4) 0.0880(16) Uani 1 1 d . . . O6 O 0.5812(4) 0.2646(3) 0.4482(4) 0.0732(11) Uani 1 1 d . . . O7 O 0.4439(3) 0.3155(2) 0.6411(4) 0.0555(9) Uani 1 1 d . . . O8 O 0.4401(4) 0.3399(3) 0.8963(4) 0.0682(11) Uani 1 1 d . . . O9 O 0.6811(4) 0.3529(3) 1.0697(3) 0.0807(14) Uani 1 1 d . . . O10 O 0.9560(3) 0.3254(3) 1.0491(3) 0.0618(10) Uani 1 1 d . . . N1 N 0.7175(3) 0.1857(2) 0.8478(3) 0.0369(8) Uani 1 1 d . . . N2 N 0.8232(3) 0.36330(19) 0.6741(3) 0.0358(8) Uani 1 1 d . . . C1 C 0.9620(5) 0.0415(4) 1.0799(6) 0.0697(16) Uani 1 1 d . . . H1A H 1.0058 0.0092 1.1455 0.104 Uiso 1 1 calc R . . H1B H 1.0064 0.0919 1.0746 0.104 Uiso 1 1 calc R . . H1C H 0.9599 0.0132 1.0019 0.104 Uiso 1 1 calc R . . C2 C 0.7574(4) 0.1026(3) 1.0226(4) 0.0385(9) Uani 1 1 d . . . C3 C 0.6279(4) 0.1084(3) 1.0404(4) 0.0410(10) Uani 1 1 d . . . H3A H 0.5976 0.0824 1.1078 0.049 Uiso 1 1 calc R . . C4 C 0.5465(5) 0.1518(3) 0.9593(5) 0.0485(11) Uani 1 1 d . . . H4A H 0.4601 0.1558 0.9702 0.058 Uiso 1 1 calc R . . C5 C 0.5938(4) 0.1903(3) 0.8600(5) 0.0467(10) Uani 1 1 d . . . H5A H 0.5389 0.2192 0.8023 0.056 Uiso 1 1 calc R . . C6 C 0.8003(4) 0.1443(2) 0.9266(4) 0.0342(8) Uani 1 1 d . . . H6A H 0.8870 0.1439 0.9161 0.041 Uiso 1 1 calc R . . C7 C 0.7656(4) 0.2306(3) 0.7420(4) 0.0388(9) Uani 1 1 d . . . H7A H 0.7059 0.2246 0.6669 0.047 Uiso 1 1 calc R . . H7B H 0.8481 0.2091 0.7257 0.047 Uiso 1 1 calc R . . C8 C 0.7788(4) 0.3184(3) 0.7776(4) 0.0401(9) Uani 1 1 d . . . H8A H 0.6967 0.3395 0.7958 0.048 Uiso 1 1 calc R . . H8B H 0.8398 0.3243 0.8518 0.048 Uiso 1 1 calc R . . C9 C 0.9505(4) 0.3654(3) 0.6627(4) 0.0428(10) Uani 1 1 d . . . H9A H 1.0087 0.3408 0.7226 0.051 Uiso 1 1 calc R . . C10 C 0.9920(4) 0.4031(3) 0.5650(5) 0.0463(11) Uani 1 1 d . . . H10A H 1.0792 0.4031 0.5562 0.056 Uiso 1 1 calc R . . C11 C 0.9071(4) 0.4422(3) 0.4766(4) 0.0422(10) Uani 1 1 d . . . H11A H 0.9369 0.4691 0.4098 0.051 Uiso 1 1 calc R . . C12 C 0.7783(4) 0.4405(2) 0.4890(4) 0.0370(9) Uani 1 1 d . . . C13 C 0.7371(4) 0.3996(3) 0.5909(4) 0.0364(9) Uani 1 1 d . . . H13A H 0.6503 0.3976 0.6009 0.044 Uiso 1 1 calc R . . C14 C 0.5641(5) 0.4843(4) 0.4211(5) 0.0607(14) Uani 1 1 d . . . H14A H 0.5191 0.5136 0.3527 0.091 Uiso 1 1 calc R . . H14B H 0.5548 0.5118 0.4980 0.091 Uiso 1 1 calc R . . H14C H 0.5292 0.4307 0.4240 0.091 Uiso 1 1 calc R . . C15 C 1.0714(6) 0.2855(4) 1.0870(6) 0.0757(17) Uani 1 1 d . . . H15A H 1.0527 0.2337 1.1230 0.091 Uiso 1 1 calc R . . H15B H 1.1205 0.3172 1.1515 0.091 Uiso 1 1 calc R . . C16 C 1.1502(5) 0.2722(4) 0.9825(5) 0.0624(14) Uani 1 1 d . . . H16A H 1.1699 0.3241 0.9473 0.075 Uiso 1 1 calc R . . H16B H 1.2307 0.2470 1.0150 0.075 Uiso 1 1 calc R . . C17 C 1.1789(5) 0.1783(4) 0.8280(6) 0.0651(15) Uani 1 1 d . . . H17A H 1.2140 0.1356 0.8835 0.078 Uiso 1 1 calc R A . H17B H 1.2488 0.2137 0.8116 0.078 Uiso 1 1 calc R . . C18 C 1.1202(6) 0.1425(4) 0.7092(7) 0.0761(19) Uani 1 1 d . A . H18A H 1.1817 0.1076 0.6748 0.091 Uiso 1 1 calc R . . H18B H 1.0464 0.1100 0.7240 0.091 Uiso 1 1 calc R . . C21 C 0.7358(8) 0.1752(5) 0.3764(6) 0.088(2) Uani 1 1 d . . . H21A H 0.7558 0.1480 0.3012 0.105 Uiso 1 1 calc R . . H21B H 0.7060 0.1350 0.4320 0.105 Uiso 1 1 calc R . . C22 C 0.6368(7) 0.2349(5) 0.3449(5) 0.083(2) Uani 1 1 d . . . H22A H 0.6733 0.2799 0.3032 0.099 Uiso 1 1 calc R A . H22B H 0.5701 0.2112 0.2864 0.099 Uiso 1 1 calc R . . C23 C 0.4762(7) 0.2221(5) 0.4875(7) 0.083(2) Uani 1 1 d . . . H23A H 0.5077 0.1838 0.5521 0.100 Uiso 1 1 calc R A . H23B H 0.4341 0.1916 0.4175 0.100 Uiso 1 1 calc R . . C24 C 0.3851(5) 0.2739(5) 0.5346(5) 0.0691(16) Uani 1 1 d . . . H24A H 0.3529 0.3125 0.4708 0.083 Uiso 1 1 calc R . . H24B H 0.3133 0.2423 0.5570 0.083 Uiso 1 1 calc R . . C25 C 0.3535(5) 0.3689(4) 0.6920(7) 0.0740(19) Uani 1 1 d . . . H25A H 0.3296 0.4124 0.6337 0.089 Uiso 1 1 calc R . . H25B H 0.2765 0.3391 0.7051 0.089 Uiso 1 1 calc R . . C26 C 0.4119(6) 0.4019(4) 0.8098(8) 0.079(2) Uani 1 1 d . . . H26A H 0.4900 0.4305 0.7968 0.094 Uiso 1 1 calc R . . H26B H 0.3536 0.4401 0.8418 0.094 Uiso 1 1 calc R . . C27 C 0.4619(7) 0.3665(7) 1.0256(8) 0.119(4) Uani 1 1 d . . . H27A H 0.3932 0.4038 1.0381 0.142 Uiso 1 1 calc R . . H27B H 0.4502 0.3195 1.0769 0.142 Uiso 1 1 calc R . . C28 C 0.5682(8) 0.4008(9) 1.0723(7) 0.148(5) Uani 1 1 d . . . H28A H 0.5605 0.4154 1.1583 0.178 Uiso 1 1 calc R . . H28B H 0.5788 0.4505 1.0267 0.178 Uiso 1 1 calc R . . C29 C 0.7903(8) 0.3993(5) 1.1180(6) 0.088(2) Uani 1 1 d . . . H29A H 0.8113 0.4374 1.0550 0.105 Uiso 1 1 calc R . . H29B H 0.7700 0.4299 1.1901 0.105 Uiso 1 1 calc R . . C30 C 0.8968(6) 0.3495(5) 1.1530(5) 0.0786(19) Uani 1 1 d . . . H30A H 0.9581 0.3784 1.2109 0.094 Uiso 1 1 calc R . . H30B H 0.8692 0.3019 1.1955 0.094 Uiso 1 1 calc R . . C19A C 1.0647(13) 0.1927(10) 0.4834(14) 0.036(3) Uani 0.40 1 d P A -1 H19A H 1.1447 0.2103 0.4551 0.043 Uiso 0.40 1 calc PR A -1 H19B H 1.0611 0.1346 0.4710 0.043 Uiso 0.40 1 calc PR A -1 C20A C 1.0055(19) 0.2121(8) 0.4304(12) 0.055(4) Uani 0.40 1 d P A -1 H20A H 1.0157 0.1848 0.3525 0.066 Uiso 0.40 1 calc PR A -1 H20B H 1.0303 0.2679 0.4187 0.066 Uiso 0.40 1 calc PR A -1 C19B C 1.0511(16) 0.1557(9) 0.5229(13) 0.083(4) Uani 0.60 1 d P A -2 H19C H 1.0750 0.1017 0.5523 0.100 Uiso 0.60 1 calc PR A -2 H19D H 1.1119 0.1701 0.4652 0.100 Uiso 0.60 1 calc PR A -2 C20B C 0.9383(8) 0.1457(6) 0.4500(9) 0.058(2) Uani 0.60 1 d P A -2 H20C H 0.8937 0.1006 0.4830 0.069 Uiso 0.60 1 calc PR A -2 H20D H 0.9573 0.1305 0.3671 0.069 Uiso 0.60 1 calc PR A -2 B1 B 0.2207(5) 0.4875(4) 0.2999(6) 0.0499(13) Uani 1 1 d . . . F1 F 0.2143(5) 0.4307(4) 0.3870(6) 0.162(3) Uani 1 1 d . . . F2 F 0.2810(6) 0.5581(3) 0.3418(5) 0.1235(18) Uani 1 1 d . . . F3 F 0.2895(5) 0.4637(4) 0.2120(5) 0.1259(19) Uani 1 1 d . . . F4 F 0.1008(4) 0.5076(3) 0.2518(5) 0.1042(15) Uani 1 1 d . . . B2 B 0.6918(5) 0.5730(3) 0.7876(4) 0.0384(10) Uani 1 1 d . . . F5 F 0.7710(5) 0.6001(4) 0.7081(5) 0.130(2) Uani 1 1 d . . . F6 F 0.7394(5) 0.5010(3) 0.8336(5) 0.1054(15) Uani 1 1 d . . . F7 F 0.5716(4) 0.5602(3) 0.7281(4) 0.0927(11) Uiso 1 1 d . . . F8 F 0.6804(7) 0.6257(5) 0.8732(7) 0.156(2) 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 O1 0.0516(19) 0.0572(19) 0.0469(17) 0.0194(16) 0.0051(15) 0.0108(16) O2 0.0475(18) 0.0563(19) 0.0458(17) 0.0142(15) 0.0043(14) 0.0007(15) O3 0.0335(17) 0.070(2) 0.073(2) -0.0105(19) 0.0001(16) 0.0051(16) O4 0.052(2) 0.073(3) 0.071(2) -0.027(2) 0.0095(17) 0.0118(18) O5 0.078(3) 0.135(4) 0.051(2) -0.017(2) 0.007(2) 0.053(3) O6 0.055(2) 0.097(3) 0.068(2) -0.006(2) 0.0081(18) -0.019(2) O7 0.0337(16) 0.055(2) 0.075(2) -0.0036(17) -0.0050(15) 0.0046(14) O8 0.047(2) 0.066(2) 0.090(3) -0.030(2) 0.0016(18) 0.0026(18) O9 0.058(2) 0.141(4) 0.0443(18) 0.002(2) 0.0081(16) 0.030(3) O10 0.053(2) 0.085(3) 0.0461(17) -0.0124(18) -0.0006(15) 0.0016(19) N1 0.0378(19) 0.0323(17) 0.0411(18) 0.0035(15) 0.0074(14) 0.0016(15) N2 0.0403(18) 0.0333(18) 0.0343(16) 0.0006(14) 0.0068(14) 0.0016(15) C1 0.046(3) 0.087(4) 0.074(4) 0.028(3) 0.000(3) 0.016(3) C2 0.043(2) 0.033(2) 0.039(2) -0.0005(17) 0.0027(18) 0.0040(18) C3 0.049(2) 0.033(2) 0.044(2) 0.0086(18) 0.019(2) 0.0009(19) C4 0.039(2) 0.050(3) 0.060(3) 0.008(2) 0.017(2) 0.007(2) C5 0.040(2) 0.042(2) 0.058(3) 0.010(2) 0.006(2) 0.008(2) C6 0.032(2) 0.0307(18) 0.041(2) -0.0008(16) 0.0056(16) 0.0023(16) C7 0.045(2) 0.040(2) 0.0332(19) 0.0102(17) 0.0114(17) 0.0042(19) C8 0.044(2) 0.038(2) 0.038(2) 0.0025(17) 0.0068(18) 0.0032(18) C9 0.038(2) 0.042(2) 0.047(2) 0.0029(19) 0.0016(18) 0.0038(19) C10 0.033(2) 0.047(2) 0.060(3) 0.009(2) 0.013(2) -0.0006(19) C11 0.047(2) 0.032(2) 0.050(2) -0.0004(19) 0.016(2) -0.0046(19) C12 0.041(2) 0.033(2) 0.037(2) 0.0027(17) 0.0064(17) -0.0023(17) C13 0.034(2) 0.037(2) 0.039(2) 0.0006(18) 0.0067(17) -0.0006(17) C14 0.049(3) 0.070(3) 0.061(3) 0.013(3) 0.000(2) 0.008(2) C15 0.076(4) 0.077(4) 0.068(4) -0.007(3) -0.016(3) 0.001(3) C16 0.041(3) 0.077(4) 0.066(3) -0.005(3) -0.007(2) 0.002(3) C17 0.041(3) 0.063(3) 0.092(4) 0.007(3) 0.011(3) 0.019(2) C18 0.057(3) 0.050(3) 0.128(6) -0.018(4) 0.040(4) -0.002(3) C21 0.125(6) 0.087(5) 0.051(3) -0.024(3) 0.009(4) 0.014(5) C22 0.078(4) 0.118(6) 0.049(3) -0.002(3) -0.005(3) -0.020(4) C23 0.083(5) 0.083(4) 0.081(4) -0.010(4) -0.002(3) -0.034(4) C24 0.041(3) 0.105(5) 0.060(3) 0.015(3) -0.002(2) -0.013(3) C25 0.036(3) 0.056(3) 0.131(6) 0.042(4) 0.014(3) 0.009(2) C26 0.047(3) 0.050(3) 0.144(6) -0.032(4) 0.032(4) -0.008(3) C27 0.053(4) 0.191(10) 0.115(6) -0.093(7) 0.025(4) -0.009(5) C28 0.086(6) 0.283(15) 0.070(4) -0.076(7) -0.009(4) 0.084(8) C29 0.099(5) 0.101(5) 0.066(4) -0.030(4) 0.025(4) -0.010(4) C30 0.068(4) 0.123(6) 0.044(3) -0.012(3) 0.002(3) -0.012(4) C19A 0.028(6) 0.043(8) 0.037(7) 0.008(6) 0.007(5) -0.001(6) C20A 0.098(11) 0.040(7) 0.029(6) -0.003(5) 0.016(7) 0.021(8) C19B 0.111(11) 0.070(9) 0.067(8) -0.018(7) 0.007(7) 0.036(8) C20B 0.038(4) 0.066(5) 0.069(5) -0.026(4) 0.007(4) -0.003(4) B1 0.038(3) 0.055(3) 0.058(3) 0.008(3) 0.011(2) 0.013(2) F1 0.124(4) 0.198(6) 0.173(5) 0.158(5) 0.057(4) 0.041(4) F2 0.147(5) 0.077(3) 0.137(4) -0.008(3) -0.024(3) -0.006(3) F3 0.095(3) 0.176(5) 0.116(4) -0.026(4) 0.054(3) 0.033(3) F4 0.060(2) 0.115(3) 0.135(4) 0.039(3) -0.001(2) 0.027(2) B2 0.043(3) 0.035(2) 0.037(2) -0.0137(19) 0.0051(19) -0.005(2) F5 0.090(3) 0.165(5) 0.148(4) 0.075(4) 0.071(3) 0.016(3) F6 0.094(3) 0.080(3) 0.137(4) 0.033(3) -0.010(3) 0.009(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 O1 C2 1.359(5) . ? O1 C1 1.447(7) . ? O2 C12 1.337(5) . ? O2 C14 1.433(6) . ? O3 C16 1.415(7) . ? O3 C17 1.411(6) . ? O4 C19B 1.373(13) . ? O4 C18 1.401(8) . ? O4 C19A 1.526(14) . ? O5 C20B 1.474(10) . ? O5 C21 1.452(10) . ? O5 C20A 1.646(19) . ? O6 C22 1.403(8) . ? O6 C23 1.412(8) . ? O7 C24 1.417(7) . ? O7 C25 1.448(7) . ? O8 C26 1.395(9) . ? O8 C27 1.454(8) . ? O9 C29 1.427(9) . ? O9 C28 1.428(9) . ? O10 C15 1.397(7) . ? O10 C30 1.400(7) . ? N1 C5 1.321(6) . ? N1 C6 1.332(5) . ? N1 C7 1.496(5) . ? N2 C13 1.339(5) . ? N2 C9 1.355(6) . ? N2 C8 1.460(5) . ? C2 C6 1.362(6) . ? C2 C3 1.397(6) . ? C3 C4 1.356(7) . ? C4 C5 1.384(7) . ? C7 C8 1.504(6) . ? C9 C10 1.339(7) . ? C10 C11 1.388(7) . ? C11 C12 1.374(6) . ? C12 C13 1.400(6) . ? C15 C16 1.489(9) . ? C17 C18 1.480(9) . ? C21 C22 1.445(11) . ? C23 C24 1.419(10) . ? C25 C26 1.451(10) . ? C27 C28 1.300(13) . ? C29 C30 1.405(10) . ? C19A C20A 0.857(17) . ? C19B C20B 1.353(16) . ? B1 F3 1.314(7) . ? B1 F1 1.335(7) . ? B1 F4 1.346(7) . ? B1 F2 1.378(8) . ? B2 F8 1.283(9) . ? B2 F5 1.337(7) . ? B2 F7 1.364(7) . ? B2 F6 1.363(7) . ? 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 C2 O1 C1 116.7(4) . . ? C12 O2 C14 119.6(4) . . ? C16 O3 C17 110.4(4) . . ? C19B O4 C18 96.2(8) . . ? C19B O4 C19A 30.1(7) . . ? C18 O4 C19A 123.0(8) . . ? C20B O5 C21 99.6(6) . . ? C20B O5 C20A 50.3(6) . . ? C21 O5 C20A 137.5(6) . . ? C22 O6 C23 118.3(5) . . ? C24 O7 C25 111.1(4) . . ? C26 O8 C27 114.6(6) . . ? C29 O9 C28 109.1(7) . . ? C15 O10 C30 110.5(5) . . ? C5 N1 C6 122.8(4) . . ? C5 N1 C7 118.0(4) . . ? C6 N1 C7 119.2(4) . . ? C13 N2 C9 121.6(4) . . ? C13 N2 C8 119.3(3) . . ? C9 N2 C8 119.1(3) . . ? O1 C2 C6 124.9(4) . . ? O1 C2 C3 116.3(4) . . ? C6 C2 C3 118.8(4) . . ? C4 C3 C2 119.9(4) . . ? C3 C4 C5 119.1(4) . . ? N1 C5 C4 119.6(4) . . ? N1 C6 C2 119.7(4) . . ? N1 C7 C8 108.3(3) . . ? N2 C8 C7 108.9(3) . . ? C10 C9 N2 119.7(4) . . ? C9 C10 C11 121.0(4) . . ? C12 C11 C10 119.1(4) . . ? O2 C12 C11 118.6(4) . . ? O2 C12 C13 122.6(4) . . ? C11 C12 C13 118.8(4) . . ? N2 C13 C12 119.8(4) . . ? O10 C15 C16 112.8(5) . . ? O3 C16 C15 112.8(5) . . ? O3 C17 C18 111.2(4) . . ? O4 C18 C17 109.0(5) . . ? C22 C21 O5 109.1(6) . . ? O6 C22 C21 113.9(5) . . ? O6 C23 C24 112.8(6) . . ? O7 C24 C23 109.6(5) . . ? C26 C25 O7 109.4(4) . . ? O8 C26 C25 110.1(5) . . ? C28 C27 O8 122.4(7) . . ? C27 C28 O9 115.3(10) . . ? C30 C29 O9 111.3(7) . . ? O10 C30 C29 111.4(5) . . ? C20A C19A O4 127.7(15) . . ? C19A C20A O5 129.1(15) . . ? O4 C19B C20B 130.4(10) . . ? C19B C20B O5 117.4(8) . . ? F3 B1 F1 111.8(6) . . ? F3 B1 F4 111.3(5) . . ? F1 B1 F4 108.9(5) . . ? F3 B1 F2 102.8(6) . . ? F1 B1 F2 115.1(6) . . ? F4 B1 F2 106.9(5) . . ? F8 B2 F5 110.4(6) . . ? F8 B2 F7 106.6(5) . . ? F5 B2 F7 111.1(5) . . ? F8 B2 F6 113.1(5) . . ? F5 B2 F6 107.2(5) . . ? F7 B2 F6 108.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.663 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.068 # Attachment 'New-L8.cif' data_[2]pseudorotaxane[(1,2-bis(pyridinium)ethane)-24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 B2 F8 N2 O8' _chemical_formula_weight 712.29 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.433(5) _cell_length_b 20.012(5) _cell_length_c 19.631(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.572(4) _cell_angle_gamma 90.00 _cell_volume 6836(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description white _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.791230 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX 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 42093 _diffrn_reflns_av_R_equivalents 0.1631 _diffrn_reflns_av_sigmaI/netI 0.1574 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 20.82 _reflns_number_total 7150 _reflns_number_gt 4120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.0031P)^2^+9.1044P] 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 7150 _refine_ls_number_parameters 901 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1374 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1851 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.051 _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 N1 N 0.1866(3) 0.1967(2) 0.7718(3) 0.0217(13) Uani 1 1 d . . . N2 N 0.2877(3) 0.0504(2) 0.6993(3) 0.0222(14) Uani 1 1 d . . . C1 C 0.1730(4) 0.1908(3) 0.8375(4) 0.0335(19) Uani 1 1 d . . . H1A H 0.2043 0.1622 0.8661 0.040 Uiso 1 1 calc R . . C2 C 0.1144(5) 0.2255(4) 0.8640(4) 0.040(2) Uani 1 1 d . . . H2A H 0.1034 0.2198 0.9105 0.048 Uiso 1 1 calc R . . C3 C 0.0715(4) 0.2688(3) 0.8225(5) 0.046(2) Uani 1 1 d . . . H3A H 0.0324 0.2952 0.8407 0.056 Uiso 1 1 calc R . . C4 C 0.0855(4) 0.2735(3) 0.7557(5) 0.037(2) Uani 1 1 d . . . H4A H 0.0550 0.3024 0.7268 0.045 Uiso 1 1 calc R . . C5 C 0.1430(4) 0.2371(3) 0.7294(4) 0.0319(19) Uani 1 1 d . . . H5A H 0.1523 0.2400 0.6823 0.038 Uiso 1 1 calc R . . C6 C 0.2494(4) 0.1578(3) 0.7443(3) 0.0287(18) Uani 1 1 d . . . H6A H 0.2940 0.1570 0.7781 0.034 Uiso 1 1 calc R . . H6B H 0.2658 0.1796 0.7023 0.034 Uiso 1 1 calc R . . C7 C 0.2239(4) 0.0865(3) 0.7280(3) 0.0254(17) Uani 1 1 d . . . H7A H 0.2089 0.0640 0.7700 0.030 Uiso 1 1 calc R . . H7B H 0.1789 0.0869 0.6947 0.030 Uiso 1 1 calc R . . C8 C 0.2924(4) 0.0485(3) 0.6320(4) 0.0344(19) Uani 1 1 d . . . H8A H 0.2534 0.0687 0.6029 0.041 Uiso 1 1 calc R . . C9 C 0.3527(5) 0.0180(4) 0.6047(4) 0.053(2) Uani 1 1 d . . . H9A H 0.3566 0.0178 0.5566 0.063 Uiso 1 1 calc R . . C10 C 0.4081(4) -0.0126(4) 0.6463(6) 0.052(2) Uani 1 1 d . . . H10A H 0.4495 -0.0355 0.6274 0.062 Uiso 1 1 calc R . . C11 C 0.4031(5) -0.0096(4) 0.7156(5) 0.047(2) Uani 1 1 d . . . H11A H 0.4415 -0.0296 0.7454 0.057 Uiso 1 1 calc R . . C12 C 0.3422(4) 0.0222(3) 0.7411(4) 0.0338(19) Uani 1 1 d . . . H12A H 0.3383 0.0246 0.7891 0.041 Uiso 1 1 calc R . . O1 O 0.2943(3) 0.2410(3) 0.6106(3) 0.0650(18) Uani 1 1 d . . . O2 O 0.4205(3) 0.1750(2) 0.6930(2) 0.0384(13) Uani 1 1 d . . . O3 O 0.4184(3) 0.1438(2) 0.8440(2) 0.0335(12) Uani 1 1 d . . . O4 O 0.2935(2) 0.1113(2) 0.9318(2) 0.0338(12) Uani 1 1 d . . . O5 O 0.1852(2) 0.0105(2) 0.8675(2) 0.0314(12) Uani 1 1 d . . . O6 O 0.0557(2) 0.0838(2) 0.7982(2) 0.0269(11) Uani 1 1 d . . . O7 O 0.0512(2) 0.1190(2) 0.6474(2) 0.0235(11) Uani 1 1 d . . . O8 O 0.1764(3) 0.1472(2) 0.5586(2) 0.0379(13) Uani 1 1 d . . . C13 C 0.2242(6) 0.1883(5) 0.5197(4) 0.079(3) Uani 1 1 d . . . H13A H 0.2689 0.1612 0.5078 0.095 Uiso 1 1 calc R . . H13B H 0.1949 0.1997 0.4765 0.095 Uiso 1 1 calc R . . C14 C 0.2505(6) 0.2445(6) 0.5474(5) 0.124(5) Uani 1 1 d . . . H14A H 0.2060 0.2741 0.5537 0.149 Uiso 1 1 calc R . . H14B H 0.2826 0.2666 0.5141 0.149 Uiso 1 1 calc R . . C15 C 0.3735(4) 0.2520(4) 0.6064(4) 0.055(2) Uani 1 1 d . . . H15A H 0.3823 0.2976 0.5891 0.066 Uiso 1 1 calc R . . H15B H 0.3945 0.2196 0.5743 0.066 Uiso 1 1 calc R . . C16 C 0.4134(4) 0.2439(4) 0.6752(4) 0.049(2) Uani 1 1 d . . . H16A H 0.4651 0.2644 0.6755 0.059 Uiso 1 1 calc R . . H16B H 0.3840 0.2674 0.7095 0.059 Uiso 1 1 calc R . . C17 C 0.4830(4) 0.1629(4) 0.7421(4) 0.045(2) Uani 1 1 d . . . H17A H 0.5294 0.1849 0.7260 0.054 Uiso 1 1 calc R . . H17B H 0.4932 0.1142 0.7435 0.054 Uiso 1 1 calc R . . C18 C 0.4725(4) 0.1858(4) 0.8127(4) 0.039(2) Uani 1 1 d . . . H18A H 0.5224 0.1845 0.8397 0.047 Uiso 1 1 calc R . . H18B H 0.4538 0.2325 0.8119 0.047 Uiso 1 1 calc R . . C19 C 0.4161(4) 0.1581(3) 0.9144(3) 0.0352(19) Uani 1 1 d . . . H19A H 0.3907 0.2018 0.9204 0.042 Uiso 1 1 calc R . . H19B H 0.4692 0.1611 0.9353 0.042 Uiso 1 1 calc R . . C20 C 0.3735(4) 0.1052(3) 0.9489(3) 0.0282(18) Uani 1 1 d . . . H20A H 0.3916 0.0608 0.9346 0.034 Uiso 1 1 calc R . . H20B H 0.3834 0.1091 0.9989 0.034 Uiso 1 1 calc R . . C21 C 0.2479(4) 0.0655(3) 0.9672(3) 0.0317(19) Uani 1 1 d . . . H21A H 0.1974 0.0861 0.9746 0.038 Uiso 1 1 calc R . . H21B H 0.2736 0.0556 1.0125 0.038 Uiso 1 1 calc R . . C22 C 0.2356(4) 0.0012(3) 0.9280(3) 0.0325(19) Uani 1 1 d . . . H22A H 0.2858 -0.0159 0.9147 0.039 Uiso 1 1 calc R . . H22B H 0.2131 -0.0325 0.9577 0.039 Uiso 1 1 calc R . . C23 C 0.1063(4) 0.0051(3) 0.8815(3) 0.0338(19) Uani 1 1 d . . . H23A H 0.0935 0.0393 0.9154 0.041 Uiso 1 1 calc R . . H23B H 0.0963 -0.0395 0.9008 0.041 Uiso 1 1 calc R . . C24 C 0.0568(4) 0.0150(3) 0.8165(3) 0.0335(19) Uani 1 1 d . . . H24A H 0.0774 -0.0117 0.7793 0.040 Uiso 1 1 calc R . . H24B H 0.0038 -0.0004 0.8231 0.040 Uiso 1 1 calc R . . C25 C -0.0075(4) 0.1009(3) 0.7527(3) 0.0280(18) Uani 1 1 d . . . H25A H -0.0130 0.1501 0.7526 0.034 Uiso 1 1 calc R . . H25B H -0.0546 0.0819 0.7706 0.034 Uiso 1 1 calc R . . C26 C -0.0026(3) 0.0780(3) 0.6805(3) 0.0213(16) Uani 1 1 d . . . H26A H 0.0143 0.0308 0.6798 0.026 Uiso 1 1 calc R . . H26B H -0.0538 0.0811 0.6559 0.026 Uiso 1 1 calc R . . C27 C 0.0533(4) 0.1015(3) 0.5765(3) 0.0281(18) Uani 1 1 d . . . H27A H 0.0002 0.0982 0.5557 0.034 Uiso 1 1 calc R . . H27B H 0.0783 0.0573 0.5724 0.034 Uiso 1 1 calc R . . C28 C 0.0964(4) 0.1524(3) 0.5400(3) 0.0320(19) Uani 1 1 d . . . H28A H 0.0874 0.1459 0.4901 0.038 Uiso 1 1 calc R . . H28B H 0.0779 0.1975 0.5515 0.038 Uiso 1 1 calc R . . N101 N -0.3091(3) 0.1321(3) 0.6603(2) 0.0217(13) Uani 1 1 d . . . N102 N -0.2026(3) 0.1289(3) 0.8320(2) 0.0178(13) Uani 1 1 d . . . C101 C -0.3359(4) 0.1915(3) 0.6370(3) 0.0264(17) Uani 1 1 d . . . H10B H -0.3107 0.2318 0.6509 0.032 Uiso 1 1 calc R . . C102 C -0.3999(4) 0.1931(4) 0.5930(3) 0.037(2) Uani 1 1 d . . . H10C H -0.4195 0.2346 0.5762 0.044 Uiso 1 1 calc R . . C103 C -0.4358(4) 0.1349(4) 0.5733(3) 0.041(2) Uani 1 1 d . . . H10D H -0.4804 0.1359 0.5429 0.050 Uiso 1 1 calc R . . C104 C -0.4069(4) 0.0746(4) 0.5976(4) 0.037(2) Uani 1 1 d . . . H10E H -0.4307 0.0337 0.5837 0.045 Uiso 1 1 calc R . . C105 C -0.3439(4) 0.0748(3) 0.6416(3) 0.0280(18) Uani 1 1 d . . . H10F H -0.3242 0.0337 0.6595 0.034 Uiso 1 1 calc R . . C106 C -0.2407(3) 0.1305(3) 0.7092(3) 0.0232(17) Uani 1 1 d . . . H10G H -0.2081 0.1702 0.7028 0.028 Uiso 1 1 calc R . . H10H H -0.2098 0.0899 0.7017 0.028 Uiso 1 1 calc R . . C107 C -0.2689(3) 0.1300(3) 0.7809(3) 0.0210(16) Uani 1 1 d . . . H10I H -0.3005 0.1703 0.7877 0.025 Uiso 1 1 calc R . . H10J H -0.3015 0.0902 0.7869 0.025 Uiso 1 1 calc R . . C108 C -0.1822(4) 0.0716(3) 0.8642(3) 0.0223(17) Uani 1 1 d . . . H10K H -0.2108 0.0321 0.8542 0.027 Uiso 1 1 calc R . . C109 C -0.1209(4) 0.0696(3) 0.9109(3) 0.0291(18) Uani 1 1 d . . . H10L H -0.1063 0.0289 0.9330 0.035 Uiso 1 1 calc R . . C110 C -0.0807(4) 0.1273(3) 0.9254(3) 0.0307(18) Uani 1 1 d . . . H11B H -0.0380 0.1267 0.9579 0.037 Uiso 1 1 calc R . . C111 C -0.1020(4) 0.1856(3) 0.8931(3) 0.0270(18) Uani 1 1 d . . . H11C H -0.0744 0.2257 0.9032 0.032 Uiso 1 1 calc R . . C112 C -0.1637(4) 0.1856(3) 0.8458(3) 0.0205(16) Uani 1 1 d . . . H11D H -0.1788 0.2258 0.8229 0.025 Uiso 1 1 calc R . . O101 O -0.2439(3) 0.2998(2) 0.7461(2) 0.0337(12) Uani 1 1 d . . . O102 O -0.1669(3) 0.2577(2) 0.6284(2) 0.0341(12) Uani 1 1 d . . . O103 O -0.1581(3) 0.1232(2) 0.5690(2) 0.0350(12) Uani 1 1 d . . . O104 O -0.1894(3) 0.0002(2) 0.6233(2) 0.0352(12) Uani 1 1 d . . . O105 O -0.2474(3) -0.0327(2) 0.7504(2) 0.0317(12) Uani 1 1 d . . . O106 O -0.3446(3) -0.0062(2) 0.8543(2) 0.0317(12) Uani 1 1 d . . . O107 O -0.3625(3) 0.1304(2) 0.9081(2) 0.0354(13) Uani 1 1 d . . . O108 O -0.3129(3) 0.2576(2) 0.8668(2) 0.0433(14) Uani 1 1 d . . . C113 C -0.3385(6) 0.3103(4) 0.8243(6) 0.102(4) Uani 1 1 d . . . H11E H -0.3842 0.2938 0.7970 0.122 Uiso 1 1 calc R . . H11F H -0.3568 0.3458 0.8545 0.122 Uiso 1 1 calc R . . C114 C -0.2940(6) 0.3399(5) 0.7811(5) 0.090(4) Uani 1 1 d . . . H11Q H -0.2629 0.3740 0.8068 0.108 Uiso 1 1 calc R . . H11R H -0.3277 0.3639 0.7468 0.108 Uiso 1 1 calc R . . C115 C -0.1971(4) 0.3422(3) 0.7080(4) 0.039(2) Uani 1 1 d . . . H11G H -0.1742 0.3777 0.7380 0.046 Uiso 1 1 calc R . . H11H H -0.2288 0.3638 0.6706 0.046 Uiso 1 1 calc R . . C116 C -0.1347(4) 0.3021(3) 0.6788(4) 0.039(2) Uani 1 1 d . . . H11I H -0.0976 0.3323 0.6582 0.047 Uiso 1 1 calc R . . H11J H -0.1068 0.2763 0.7156 0.047 Uiso 1 1 calc R . . C117 C -0.1125(4) 0.2342(4) 0.5831(4) 0.041(2) Uani 1 1 d . . . H11K H -0.0686 0.2131 0.6094 0.050 Uiso 1 1 calc R . . H11L H -0.0926 0.2721 0.5569 0.050 Uiso 1 1 calc R . . C118 C -0.1497(5) 0.1847(4) 0.5355(4) 0.046(2) Uani 1 1 d . . . H11M H -0.2008 0.2015 0.5185 0.055 Uiso 1 1 calc R . . H11N H -0.1181 0.1785 0.4958 0.055 Uiso 1 1 calc R . . C119 C -0.1926(4) 0.0722(4) 0.5266(3) 0.039(2) Uani 1 1 d . . . H11O H -0.1758 0.0768 0.4796 0.047 Uiso 1 1 calc R . . H11P H -0.2493 0.0766 0.5249 0.047 Uiso 1 1 calc R . . C120 C -0.1694(4) 0.0054(4) 0.5547(3) 0.040(2) Uani 1 1 d . . . H12B H -0.1956 -0.0302 0.5270 0.048 Uiso 1 1 calc R . . H12C H -0.1133 -0.0006 0.5524 0.048 Uiso 1 1 calc R . . C121 C -0.1765(4) -0.0641(3) 0.6528(4) 0.038(2) Uani 1 1 d . . . H12D H -0.1269 -0.0823 0.6393 0.046 Uiso 1 1 calc R . . H12E H -0.2180 -0.0951 0.6368 0.046 Uiso 1 1 calc R . . C122 C -0.1751(4) -0.0569(3) 0.7290(3) 0.0338(19) Uani 1 1 d . . . H12F H -0.1636 -0.1008 0.7506 0.041 Uiso 1 1 calc R . . H12G H -0.1338 -0.0255 0.7445 0.041 Uiso 1 1 calc R . . C123 C -0.2945(4) -0.0836(3) 0.7767(4) 0.0355(19) Uani 1 1 d . . . H12H H -0.2663 -0.1069 0.8150 0.043 Uiso 1 1 calc R . . H12I H -0.3085 -0.1168 0.7406 0.043 Uiso 1 1 calc R . . C124 C -0.3658(4) -0.0516(3) 0.8009(4) 0.039(2) Uani 1 1 d . . . H12J H -0.3934 -0.0275 0.7627 0.047 Uiso 1 1 calc R . . H12K H -0.4005 -0.0863 0.8177 0.047 Uiso 1 1 calc R . . C125 C -0.4083(4) 0.0194(4) 0.8869(4) 0.038(2) Uani 1 1 d . . . H12L H -0.4355 -0.0175 0.9088 0.046 Uiso 1 1 calc R . . H12M H -0.4447 0.0406 0.8527 0.046 Uiso 1 1 calc R . . C126 C -0.3823(4) 0.0699(3) 0.9397(3) 0.0351(19) Uani 1 1 d . . . H12N H -0.4239 0.0782 0.9708 0.042 Uiso 1 1 calc R . . H12O H -0.3371 0.0524 0.9672 0.042 Uiso 1 1 calc R . . C127 C -0.3312(4) 0.1796(4) 0.9550(3) 0.043(2) Uani 1 1 d . . . H12P H -0.2748 0.1738 0.9614 0.052 Uiso 1 1 calc R . . H12Q H -0.3534 0.1739 0.9998 0.052 Uiso 1 1 calc R . . C128 C -0.3491(4) 0.2474(4) 0.9280(4) 0.045(2) Uani 1 1 d . . . H12R H -0.4054 0.2523 0.9196 0.054 Uiso 1 1 calc R . . H12S H -0.3312 0.2813 0.9620 0.054 Uiso 1 1 calc R . . B1 B 0.9261(5) 0.0987(4) 0.3619(4) 0.033(2) Uani 1 1 d . . . F1 F 0.8949(3) 0.16194(19) 0.3677(2) 0.0635(14) Uani 1 1 d . . . F2 F 0.9693(3) 0.0831(2) 0.4209(2) 0.0700(14) Uani 1 1 d . . . F3 F 0.9727(3) 0.09798(19) 0.3070(2) 0.0548(12) Uani 1 1 d . . . F4 F 0.8679(2) 0.05200(18) 0.35172(19) 0.0447(11) Uani 1 1 d . . . B2 B 0.5679(5) 0.1195(4) 0.1248(4) 0.025(2) Uani 1 1 d . . . F5 F 0.5158(2) 0.1370(2) 0.0726(2) 0.0546(12) Uani 1 1 d . . . F6 F 0.5842(2) 0.0517(2) 0.1212(2) 0.0581(13) Uani 1 1 d . . . F7 F 0.5378(2) 0.13118(19) 0.1872(2) 0.0494(12) Uani 1 1 d . . . F8 F 0.6356(2) 0.1542(2) 0.1201(2) 0.0559(13) Uani 1 1 d . . . B102 B 0.0766(5) 0.1268(4) 0.0726(5) 0.030(2) Uani 1 1 d . . . F105 F 0.0373(5) 0.1556(5) 0.1161(3) 0.231(6) Uani 1 1 d . . . F106 F 0.0358(4) 0.0729(3) 0.0502(4) 0.155(3) Uani 1 1 d . . . F107 F 0.1418(3) 0.1050(3) 0.1007(3) 0.112(2) Uani 1 1 d . . . F108 F 0.0814(3) 0.1634(3) 0.0148(3) 0.0901(19) Uani 1 1 d . . . B101 B -0.4120(5) -0.1223(4) 0.5887(5) 0.057(3) Uani 1 1 d D . . F101 F -0.3866(7) -0.0908(6) 0.5370(6) 0.135(7) Uani 0.60 1 d PD A -1 F102 F -0.3552(4) -0.1696(3) 0.6135(4) 0.054(2) Uani 0.60 1 d PD A -1 F103 F -0.4181(6) -0.0789(5) 0.6435(5) 0.058(3) Uani 0.60 1 d PD A -1 F104 F -0.4789(5) -0.1564(5) 0.5797(6) 0.088(4) Uani 0.60 1 d PD A -1 F501 F -0.4423(14) -0.0740(7) 0.5418(7) 0.151(11) Uani 0.40 1 d PD A -2 F502 F -0.4318(13) -0.1751(8) 0.5543(10) 0.177(13) Uani 0.40 1 d PD A -2 F503 F -0.3403(9) -0.1120(17) 0.5913(13) 0.55(5) Uani 0.40 1 d PD A -2 F504 F -0.4445(12) -0.1123(12) 0.6424(10) 0.139(11) Uani 0.40 1 d PD A -2 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 N1 0.016(3) 0.020(3) 0.029(4) 0.002(3) 0.006(3) 0.001(3) N2 0.017(3) 0.023(3) 0.027(4) 0.004(3) 0.004(3) 0.003(3) C1 0.046(5) 0.031(5) 0.024(5) 0.002(4) 0.006(4) 0.009(4) C2 0.056(6) 0.029(5) 0.037(5) -0.005(4) 0.019(5) -0.003(4) C3 0.034(5) 0.022(5) 0.086(8) -0.014(5) 0.024(5) 0.002(4) C4 0.025(5) 0.031(5) 0.055(6) 0.011(4) -0.006(5) -0.001(4) C5 0.034(5) 0.031(4) 0.031(5) 0.009(4) -0.004(4) -0.004(4) C6 0.024(4) 0.032(4) 0.030(4) 0.005(4) 0.007(4) 0.003(4) C7 0.019(4) 0.039(5) 0.019(4) 0.001(3) 0.005(3) 0.006(4) C8 0.032(5) 0.048(5) 0.024(5) 0.002(4) 0.008(4) 0.015(4) C9 0.049(6) 0.064(6) 0.048(6) -0.013(5) 0.032(5) 0.009(5) C10 0.026(6) 0.028(5) 0.104(9) -0.001(5) 0.023(6) 0.012(4) C11 0.021(5) 0.039(5) 0.081(8) 0.021(5) -0.005(5) -0.010(4) C12 0.025(5) 0.031(4) 0.046(5) 0.012(4) 0.006(5) -0.005(4) O1 0.042(4) 0.104(5) 0.047(4) 0.047(3) -0.014(3) -0.036(3) O2 0.036(3) 0.046(3) 0.033(3) 0.004(3) -0.003(3) -0.013(2) O3 0.037(3) 0.035(3) 0.028(3) -0.001(2) -0.001(2) -0.012(2) O4 0.024(3) 0.042(3) 0.036(3) 0.013(2) 0.000(3) 0.003(2) O5 0.022(3) 0.051(3) 0.021(3) 0.005(2) 0.003(2) 0.005(2) O6 0.027(3) 0.029(3) 0.024(3) -0.002(2) -0.003(2) -0.005(2) O7 0.020(3) 0.034(3) 0.016(3) -0.002(2) 0.003(2) -0.004(2) O8 0.034(3) 0.045(3) 0.034(3) 0.010(2) 0.000(3) -0.007(3) C13 0.114(9) 0.099(8) 0.025(5) 0.007(5) 0.012(6) -0.064(7) C14 0.127(10) 0.165(12) 0.073(8) 0.082(8) -0.049(8) -0.100(9) C15 0.040(6) 0.073(6) 0.052(6) 0.032(5) 0.006(5) -0.022(5) C16 0.040(5) 0.045(6) 0.061(6) 0.020(4) -0.015(5) -0.023(4) C17 0.027(5) 0.065(6) 0.041(5) 0.005(4) -0.002(4) -0.012(4) C18 0.031(5) 0.048(5) 0.038(5) -0.002(4) -0.001(4) -0.005(4) C19 0.046(5) 0.039(5) 0.020(5) -0.009(4) -0.002(4) 0.001(4) C20 0.024(5) 0.037(5) 0.023(4) -0.004(3) 0.001(4) -0.002(4) C21 0.029(5) 0.047(5) 0.019(4) 0.007(4) -0.001(4) 0.012(4) C22 0.032(5) 0.042(5) 0.023(4) 0.011(4) -0.001(4) 0.003(4) C23 0.026(5) 0.042(5) 0.032(5) 0.006(4) -0.004(4) -0.002(4) C24 0.035(5) 0.037(5) 0.028(4) 0.001(4) -0.007(4) -0.007(4) C25 0.019(4) 0.031(4) 0.033(5) 0.003(4) -0.001(4) 0.002(3) C26 0.015(4) 0.027(4) 0.022(4) 0.006(3) 0.001(3) -0.003(3) C27 0.021(4) 0.040(5) 0.023(5) -0.002(4) -0.002(4) -0.002(4) C28 0.037(5) 0.032(4) 0.026(4) 0.003(4) -0.001(4) 0.005(4) N101 0.015(3) 0.033(4) 0.017(3) -0.003(3) -0.001(3) 0.003(3) N102 0.017(3) 0.022(3) 0.014(3) 0.002(3) 0.003(3) 0.000(3) C101 0.028(5) 0.027(4) 0.024(4) 0.003(3) 0.004(4) 0.008(4) C102 0.024(5) 0.056(6) 0.029(5) 0.016(4) -0.006(4) 0.004(4) C103 0.024(5) 0.079(7) 0.020(4) 0.000(5) -0.008(4) -0.003(5) C104 0.033(5) 0.045(5) 0.034(5) -0.017(4) -0.002(4) -0.001(4) C105 0.028(5) 0.032(5) 0.023(4) -0.004(4) -0.003(4) -0.003(4) C106 0.016(4) 0.033(4) 0.020(4) -0.002(3) 0.000(4) 0.003(3) C107 0.015(4) 0.035(4) 0.014(4) -0.001(3) 0.002(3) 0.003(3) C108 0.030(4) 0.018(4) 0.019(4) 0.007(3) 0.002(4) 0.001(3) C109 0.030(5) 0.032(5) 0.024(4) 0.007(4) 0.000(4) 0.007(4) C110 0.027(4) 0.040(5) 0.024(4) -0.003(4) -0.008(4) 0.006(4) C111 0.026(5) 0.034(5) 0.021(4) -0.002(4) 0.001(4) -0.004(3) C112 0.020(4) 0.022(4) 0.020(4) 0.004(3) 0.005(4) 0.002(3) O101 0.043(3) 0.028(3) 0.031(3) 0.002(2) 0.007(3) 0.014(3) O102 0.030(3) 0.037(3) 0.037(3) -0.008(2) 0.008(3) -0.002(2) O103 0.042(3) 0.040(3) 0.024(3) 0.000(3) 0.000(2) -0.002(2) O104 0.037(3) 0.035(3) 0.035(3) -0.005(2) 0.011(3) 0.004(2) O105 0.030(3) 0.027(3) 0.039(3) 0.004(2) 0.004(3) 0.004(2) O106 0.022(3) 0.039(3) 0.035(3) -0.005(2) 0.006(3) -0.008(2) O107 0.046(3) 0.042(3) 0.019(3) 0.006(3) 0.004(2) -0.007(3) O108 0.049(3) 0.051(4) 0.032(3) 0.005(3) 0.017(3) 0.016(3) C113 0.087(8) 0.050(6) 0.177(12) 0.057(7) 0.082(8) 0.044(6) C114 0.124(10) 0.088(8) 0.064(7) 0.036(6) 0.049(7) 0.074(8) C115 0.060(6) 0.019(4) 0.035(5) 0.000(4) -0.005(5) -0.002(4) C116 0.046(5) 0.035(5) 0.037(5) 0.007(4) 0.003(4) -0.017(4) C117 0.048(5) 0.041(5) 0.038(5) 0.005(4) 0.020(5) 0.002(4) C118 0.060(6) 0.053(6) 0.026(5) 0.010(4) 0.020(4) 0.013(5) C119 0.034(5) 0.059(6) 0.025(4) -0.010(4) 0.002(4) -0.003(4) C120 0.037(5) 0.062(6) 0.023(5) -0.017(4) 0.010(4) -0.001(4) C121 0.034(5) 0.030(5) 0.050(6) -0.011(4) 0.002(4) 0.009(4) C122 0.028(5) 0.028(4) 0.045(5) -0.002(4) -0.001(4) 0.005(4) C123 0.044(5) 0.026(4) 0.036(5) -0.002(4) -0.001(4) -0.005(4) C124 0.037(5) 0.039(5) 0.041(5) -0.007(4) 0.002(4) -0.014(4) C125 0.033(5) 0.048(5) 0.035(5) 0.011(4) 0.007(4) -0.004(4) C126 0.030(5) 0.045(5) 0.031(5) 0.012(4) 0.009(4) 0.003(4) C127 0.040(5) 0.071(6) 0.019(4) -0.008(4) 0.003(4) -0.015(4) C128 0.043(5) 0.054(6) 0.038(5) -0.021(4) 0.006(5) -0.005(4) B1 0.052(6) 0.026(6) 0.021(6) -0.008(4) 0.000(5) -0.004(5) F1 0.090(4) 0.030(3) 0.072(3) -0.014(2) 0.017(3) 0.007(2) F2 0.073(3) 0.089(4) 0.045(3) -0.004(3) -0.022(3) 0.003(3) F3 0.070(3) 0.052(3) 0.045(3) -0.015(2) 0.024(3) -0.018(2) F4 0.046(3) 0.039(2) 0.049(3) 0.003(2) 0.002(2) -0.009(2) B2 0.031(6) 0.025(5) 0.020(5) -0.012(4) 0.009(5) 0.004(4) F5 0.041(3) 0.075(3) 0.047(3) 0.000(2) -0.007(2) 0.015(2) F6 0.055(3) 0.039(3) 0.080(3) -0.012(2) 0.009(3) 0.014(2) F7 0.056(3) 0.052(3) 0.042(3) 0.002(2) 0.020(2) 0.017(2) F8 0.046(3) 0.078(3) 0.044(3) 0.004(2) 0.006(2) -0.037(3) B102 0.016(5) 0.041(6) 0.031(6) -0.008(5) 0.000(5) -0.003(5) F105 0.270(11) 0.341(12) 0.083(5) -0.053(6) 0.015(6) 0.225(10) F106 0.189(7) 0.097(5) 0.166(6) 0.076(5) -0.101(6) -0.062(5) F107 0.043(3) 0.221(7) 0.069(4) 0.059(4) -0.009(3) 0.019(4) F108 0.080(4) 0.107(4) 0.077(4) 0.059(3) -0.035(3) -0.055(3) B101 0.037(8) 0.072(9) 0.062(9) -0.007(9) 0.008(7) -0.021(7) F101 0.185(14) 0.094(9) 0.140(13) 0.065(8) 0.126(11) 0.072(9) F102 0.047(6) 0.031(4) 0.084(6) -0.003(4) -0.003(5) 0.012(4) F103 0.069(8) 0.066(7) 0.035(6) -0.024(5) -0.022(5) 0.027(6) F104 0.065(7) 0.075(8) 0.117(10) 0.017(7) -0.046(7) -0.022(6) F501 0.36(3) 0.063(12) 0.032(9) -0.021(8) 0.017(15) -0.102(16) F502 0.26(3) 0.077(13) 0.17(2) -0.061(13) -0.13(2) 0.094(16) F503 0.052(16) 1.15(13) 0.43(6) -0.54(7) -0.02(3) -0.10(4) F504 0.106(19) 0.20(3) 0.114(19) -0.009(19) 0.015(15) 0.011(18) _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 N1 C1 1.331(8) . ? N1 C5 1.359(8) . ? N1 C6 1.473(7) . ? N2 C8 1.330(8) . ? N2 C12 1.340(8) . ? N2 C7 1.468(7) . ? C1 C2 1.365(9) . ? C2 C3 1.379(10) . ? C3 C4 1.352(10) . ? C4 C5 1.367(9) . ? C6 C7 1.522(8) . ? C8 C9 1.355(9) . ? C9 C10 1.370(10) . ? C10 C11 1.370(10) . ? C11 C12 1.359(10) . ? O1 C15 1.406(8) . ? O1 C14 1.416(10) . ? O2 C16 1.426(7) . ? O2 C17 1.430(7) . ? O3 C19 1.415(7) . ? O3 C18 1.430(8) . ? O4 C20 1.419(7) . ? O4 C21 1.423(7) . ? O5 C23 1.424(7) . ? O5 C22 1.443(7) . ? O6 C25 1.416(7) . ? O6 C24 1.421(7) . ? O7 C26 1.432(7) . ? O7 C27 1.438(7) . ? O8 C28 1.424(7) . ? O8 C13 1.426(9) . ? C13 C14 1.319(12) . ? C15 C16 1.489(9) . ? C17 C18 1.482(9) . ? C19 C20 1.481(8) . ? C21 C22 1.507(8) . ? C23 C24 1.509(8) . ? C25 C26 1.498(8) . ? C27 C28 1.478(8) . ? N101 C105 1.338(7) . ? N101 C101 1.347(7) . ? N101 C106 1.485(7) . ? N102 C112 1.340(7) . ? N102 C108 1.347(7) . ? N102 C107 1.483(7) . ? C101 C102 1.368(8) . ? C102 C103 1.367(9) . ? C103 C104 1.381(9) . ? C104 C105 1.353(8) . ? C106 C107 1.519(8) . ? C108 C109 1.364(8) . ? C109 C110 1.370(8) . ? C110 C111 1.369(8) . ? C111 C112 1.378(8) . ? O101 C114 1.398(9) . ? O101 C115 1.423(8) . ? O102 C116 1.419(7) . ? O102 C117 1.422(8) . ? O103 C118 1.408(8) . ? O103 C119 1.427(7) . ? O104 C120 1.415(7) . ? O104 C121 1.423(7) . ? O105 C123 1.424(7) . ? O105 C122 1.436(7) . ? O106 C125 1.413(8) . ? O106 C124 1.419(7) . ? O107 C126 1.413(7) . ? O107 C127 1.431(7) . ? O108 C113 1.399(9) . ? O108 C128 1.407(8) . ? C113 C114 1.323(11) . ? C115 C116 1.493(9) . ? C117 C118 1.482(9) . ? C119 C120 1.493(9) . ? C121 C122 1.501(9) . ? C123 C124 1.501(9) . ? C125 C126 1.498(9) . ? C127 C128 1.482(9) . ? B1 F2 1.378(9) . ? B1 F3 1.390(9) . ? B1 F1 1.385(9) . ? B1 F4 1.386(9) . ? B2 F5 1.372(8) . ? B2 F8 1.376(9) . ? B2 F7 1.382(8) . ? B2 F6 1.390(8) . ? B102 F105 1.267(9) . ? B102 F107 1.306(9) . ? B102 F106 1.350(9) . ? B102 F108 1.357(9) . ? B101 F101 1.296(11) . ? B101 F104 1.353(11) . ? B101 F103 1.393(12) . ? B101 F502 1.288(15) . ? B101 F102 1.432(10) . ? B101 F504 1.244(16) . ? B101 F503 1.263(15) . ? B101 F501 1.415(16) . ? 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 C1 N1 C5 121.3(6) . . ? C1 N1 C6 119.3(6) . . ? C5 N1 C6 119.4(6) . . ? C8 N2 C12 120.7(6) . . ? C8 N2 C7 119.3(5) . . ? C12 N2 C7 119.9(6) . . ? N1 C1 C2 120.5(7) . . ? C1 C2 C3 119.0(7) . . ? C4 C3 C2 119.6(7) . . ? C3 C4 C5 120.7(7) . . ? N1 C5 C4 118.7(7) . . ? N1 C6 C7 111.0(5) . . ? N2 C7 C6 108.9(5) . . ? N2 C8 C9 120.2(7) . . ? C8 C9 C10 120.0(8) . . ? C11 C10 C9 119.1(8) . . ? C12 C11 C10 119.0(7) . . ? C11 C12 N2 120.8(7) . . ? C15 O1 C14 114.8(7) . . ? C16 O2 C17 112.4(5) . . ? C19 O3 C18 111.0(5) . . ? C20 O4 C21 113.6(5) . . ? C23 O5 C22 112.2(5) . . ? C25 O6 C24 113.0(4) . . ? C26 O7 C27 110.8(4) . . ? C28 O8 C13 114.6(6) . . ? C14 C13 O8 118.1(8) . . ? C13 C14 O1 118.3(9) . . ? O1 C15 C16 109.6(6) . . ? O2 C16 C15 110.8(6) . . ? O2 C17 C18 116.4(6) . . ? O3 C18 C17 110.0(6) . . ? O3 C19 C20 110.3(5) . . ? O4 C20 C19 110.1(5) . . ? O4 C21 C22 111.5(5) . . ? O5 C22 C21 111.8(5) . . ? O5 C23 C24 109.7(5) . . ? O6 C24 C23 109.8(5) . . ? O6 C25 C26 115.8(5) . . ? O7 C26 C25 109.3(5) . . ? O7 C27 C28 110.2(5) . . ? O8 C28 C27 110.1(5) . . ? C105 N101 C101 121.5(5) . . ? C105 N101 C106 119.4(5) . . ? C101 N101 C106 119.1(5) . . ? C112 N102 C108 120.7(5) . . ? C112 N102 C107 119.2(5) . . ? C108 N102 C107 120.1(5) . . ? N101 C101 C102 119.1(6) . . ? C103 C102 C101 120.0(7) . . ? C102 C103 C104 119.7(6) . . ? C105 C104 C103 118.8(7) . . ? N101 C105 C104 120.9(6) . . ? N101 C106 C107 107.8(5) . . ? N102 C107 C106 110.1(5) . . ? N102 C108 C109 120.9(6) . . ? C108 C109 C110 119.0(6) . . ? C111 C110 C109 120.1(6) . . ? C110 C111 C112 119.3(6) . . ? N102 C112 C111 120.1(6) . . ? C114 O101 C115 108.3(6) . . ? C116 O102 C117 113.2(5) . . ? C118 O103 C119 113.9(5) . . ? C120 O104 C121 114.3(5) . . ? C123 O105 C122 113.7(5) . . ? C125 O106 C124 113.0(5) . . ? C126 O107 C127 113.6(5) . . ? C113 O108 C128 118.4(6) . . ? C114 C113 O108 122.7(8) . . ? C113 C114 O101 117.9(8) . . ? O101 C115 C116 109.7(5) . . ? O102 C116 C115 109.7(6) . . ? O102 C117 C118 109.4(6) . . ? O103 C118 C117 110.1(6) . . ? O103 C119 C120 109.3(5) . . ? O104 C120 C119 109.9(6) . . ? O104 C121 C122 108.2(5) . . ? O105 C122 C121 111.3(5) . . ? O105 C123 C124 108.5(5) . . ? O106 C124 C123 108.9(5) . . ? O106 C125 C126 110.2(6) . . ? O107 C126 C125 110.3(5) . . ? O107 C127 C128 109.6(6) . . ? O108 C128 C127 110.1(6) . . ? F2 B1 F3 109.5(7) . . ? F2 B1 F1 109.6(6) . . ? F3 B1 F1 109.0(6) . . ? F2 B1 F4 109.0(6) . . ? F3 B1 F4 109.9(6) . . ? F1 B1 F4 109.9(7) . . ? F5 B2 F8 110.6(6) . . ? F5 B2 F7 110.4(6) . . ? F8 B2 F7 110.4(6) . . ? F5 B2 F6 109.8(6) . . ? F8 B2 F6 108.1(6) . . ? F7 B2 F6 107.5(6) . . ? F105 B102 F107 111.2(8) . . ? F105 B102 F106 106.7(9) . . ? F107 B102 F106 107.4(8) . . ? F105 B102 F108 112.4(8) . . ? F107 B102 F108 115.8(7) . . ? F106 B102 F108 102.5(6) . . ? F101 B101 F104 118.5(10) . . ? F101 B101 F103 110.3(9) . . ? F104 B101 F103 108.0(9) . . ? F101 B101 F502 94.7(13) . . ? F104 B101 F502 46.9(10) . . ? F103 B101 F502 152.2(12) . . ? F101 B101 F102 109.0(8) . . ? F104 B101 F102 106.4(7) . . ? F103 B101 F102 103.5(7) . . ? F502 B101 F102 78.1(10) . . ? F101 B101 F504 141.4(13) . . ? F104 B101 F504 75.9(12) . . ? F103 B101 F504 35.3(11) . . ? F502 B101 F504 117.0(13) . . ? F102 B101 F504 99.2(13) . . ? F101 B101 F503 64.4(14) . . ? F104 B101 F503 158.3(14) . . ? F103 B101 F503 89.4(12) . . ? F502 B101 F503 112.8(12) . . ? F102 B101 F503 55.5(16) . . ? F504 B101 F503 116.1(12) . . ? F101 B101 F501 44.8(10) . . ? F104 B101 F501 88.6(10) . . ? F103 B101 F501 91.9(9) . . ? F502 B101 F501 98.1(9) . . ? F102 B101 F501 153.5(12) . . ? F504 B101 F501 105.6(11) . . ? F503 B101 F501 104.1(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.529 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.061 # Attachment 'New-L9.cif' data_[2]pseudorotaxane_[(1,2-bis(4-benzyl-4'-bipyridinium)ethane)-DN24C8][BF4]2 _database_code_depnum_ccdc_archive 'CCDC 286508' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H82 B4 F16 N8 O9' _chemical_formula_weight 1598.74 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' B B 0.0013 0.0007 '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' _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 13.598(2) _cell_length_b 16.807(3) _cell_length_c 17.859(3) _cell_angle_alpha 87.625(3) _cell_angle_beta 87.329(3) _cell_angle_gamma 70.059(2) _cell_volume 3831.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description orange-yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.823898 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX 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 36817 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.1067 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13433 _reflns_number_gt 6557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker 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^)+(0.1832P)^2^+4.8142P] 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 13433 _refine_ls_number_parameters 1022 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1889 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.3487 _refine_ls_wR_factor_gt 0.2836 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _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 N1 N 0.3759(4) 0.2959(3) 0.0773(3) 0.0345(11) Uani 1 1 d . . . N2 N 0.5090(4) 0.0681(3) 0.4162(2) 0.0349(11) Uani 1 1 d . . . C1 C 0.1753(6) 0.4293(4) -0.0362(4) 0.059(2) Uani 1 1 d . . . H1A H 0.1915 0.4785 -0.0261 0.071 Uiso 1 1 calc R . . C2 C 0.0790(7) 0.4381(6) -0.0631(5) 0.078(3) Uani 1 1 d . . . H2A H 0.0297 0.4930 -0.0722 0.094 Uiso 1 1 calc R . . C3 C 0.0539(6) 0.3681(6) -0.0768(4) 0.068(2) Uani 1 1 d . . . H3A H -0.0129 0.3739 -0.0948 0.082 Uiso 1 1 calc R . . C4 C 0.1253(6) 0.2905(5) -0.0643(5) 0.065(2) Uani 1 1 d . . . H4A H 0.1078 0.2419 -0.0742 0.078 Uiso 1 1 calc R . . C5 C 0.2214(5) 0.2798(4) -0.0382(4) 0.0559(19) Uani 1 1 d . . . H5A H 0.2700 0.2245 -0.0297 0.067 Uiso 1 1 calc R . . C6 C 0.2483(5) 0.3512(4) -0.0236(3) 0.0394(15) Uani 1 1 d . . . C7 C 0.3531(5) 0.3430(4) 0.0040(3) 0.0421(15) Uani 1 1 d . . . H7A H 0.3569 0.4003 0.0093 0.051 Uiso 1 1 calc R . . H7B H 0.4075 0.3133 -0.0338 0.051 Uiso 1 1 calc R . . C8 C 0.4269(5) 0.2120(4) 0.0776(3) 0.0389(15) Uani 1 1 d . . . H8A H 0.4479 0.1841 0.0314 0.047 Uiso 1 1 calc R . . C9 C 0.4492(5) 0.1663(3) 0.1436(3) 0.0352(14) Uani 1 1 d . . . H9A H 0.4838 0.1067 0.1430 0.042 Uiso 1 1 calc R . . C10 C 0.4213(4) 0.2070(3) 0.2120(3) 0.0295(13) Uani 1 1 d . . . C11 C 0.3685(4) 0.2936(3) 0.2090(3) 0.0323(13) Uani 1 1 d . . . H11A H 0.3479 0.3234 0.2543 0.039 Uiso 1 1 calc R . . C12 C 0.3456(5) 0.3369(4) 0.1419(3) 0.0371(14) Uani 1 1 d . . . H12A H 0.3082 0.3961 0.1410 0.045 Uiso 1 1 calc R . . C13 C 0.4504(4) 0.1588(3) 0.2831(3) 0.0312(13) Uani 1 1 d . . . C14 C 0.4833(5) 0.0707(3) 0.2864(3) 0.0368(14) Uani 1 1 d . . . H14A H 0.4855 0.0406 0.2421 0.044 Uiso 1 1 calc R . . C15 C 0.5122(5) 0.0273(4) 0.3522(3) 0.0364(14) Uani 1 1 d . . . H15A H 0.5350 -0.0328 0.3531 0.044 Uiso 1 1 calc R . . C16 C 0.4754(5) 0.1535(4) 0.4145(4) 0.0435(16) Uani 1 1 d . . . H16A H 0.4720 0.1824 0.4597 0.052 Uiso 1 1 calc R . . C17 C 0.4465(5) 0.1992(4) 0.3501(3) 0.0407(15) Uani 1 1 d . . . H17A H 0.4235 0.2593 0.3507 0.049 Uiso 1 1 calc R . . C18 C 0.5419(5) 0.0189(4) 0.4861(3) 0.0387(14) Uani 1 1 d . . . H18A H 0.5517 0.0560 0.5246 0.046 Uiso 1 1 calc R . . H18B H 0.6095 -0.0272 0.4772 0.046 Uiso 1 1 calc R . . O1 O 0.2649(3) 0.0462(3) 0.3769(2) 0.0456(11) Uani 1 1 d . . . O2 O 0.4186(5) -0.1237(3) 0.3699(4) 0.099(2) Uani 1 1 d . . . O3 O 0.3768(4) 0.1629(3) 0.5964(3) 0.0599(14) Uani 1 1 d . . . O4 O 0.2455(4) 0.1637(3) 0.4712(2) 0.0499(12) Uani 1 1 d . . . C19 C 0.2128(5) 0.1918(4) 0.4010(3) 0.0418(15) Uani 1 1 d . . . C20 C 0.1705(5) 0.2747(4) 0.3788(4) 0.0469(16) Uani 1 1 d . . . H20A H 0.1587 0.3174 0.4147 0.056 Uiso 1 1 calc R . . C21 C 0.1439(5) 0.2983(4) 0.3037(4) 0.0422(15) Uani 1 1 d . . . C22 C 0.1036(5) 0.3849(4) 0.2789(4) 0.0556(18) Uani 1 1 d . . . H22A H 0.0907 0.4285 0.3140 0.067 Uiso 1 1 calc R . . C23 C 0.0834(5) 0.4051(4) 0.2049(4) 0.0538(18) Uani 1 1 d . . . H23A H 0.0597 0.4628 0.1885 0.065 Uiso 1 1 calc R . . C24 C 0.0975(5) 0.3414(5) 0.1533(4) 0.0521(18) Uani 1 1 d . . . H24A H 0.0817 0.3562 0.1022 0.063 Uiso 1 1 calc R . . C25 C 0.1338(5) 0.2582(4) 0.1757(4) 0.0484(17) Uani 1 1 d . . . H25A H 0.1431 0.2157 0.1399 0.058 Uiso 1 1 calc R . . C26 C 0.1578(5) 0.2344(4) 0.2511(4) 0.0425(15) Uani 1 1 d . . . C27 C 0.1978(5) 0.1482(4) 0.2763(4) 0.0415(15) Uani 1 1 d . . . H27A H 0.2067 0.1046 0.2417 0.050 Uiso 1 1 calc R . . C28 C 0.2233(5) 0.1272(4) 0.3486(4) 0.0398(15) Uani 1 1 d . . . C29 C 0.2634(6) -0.0209(4) 0.3300(4) 0.0519(18) Uani 1 1 d . . . H29A H 0.3042 -0.0200 0.2828 0.062 Uiso 1 1 calc R . . H29B H 0.1905 -0.0129 0.3173 0.062 Uiso 1 1 calc R . . C30 C 0.3097(7) -0.1034(4) 0.3707(5) 0.068(2) Uani 1 1 d . . . H30A H 0.2815 -0.0994 0.4230 0.082 Uiso 1 1 calc R . . H30B H 0.2917 -0.1481 0.3461 0.082 Uiso 1 1 calc R . . C31 C 0.4773(9) -0.2027(6) 0.3775(7) 0.110(4) Uani 1 1 d . . . H31A H 0.4561 -0.2352 0.3403 0.132 Uiso 1 1 calc R . . H31B H 0.4612 -0.2232 0.4278 0.132 Uiso 1 1 calc R . . C32 C 0.4109(8) 0.2237(4) 0.6303(4) 0.076(3) Uani 1 1 d . . . H32A H 0.3899 0.2267 0.6842 0.091 Uiso 1 1 calc R . . H32B H 0.3762 0.2802 0.6067 0.091 Uiso 1 1 calc R . . C33 C 0.2649(6) 0.1828(5) 0.5992(4) 0.062(2) Uani 1 1 d . . . H33A H 0.2337 0.2199 0.6420 0.075 Uiso 1 1 calc R . . H33B H 0.2484 0.1300 0.6072 0.075 Uiso 1 1 calc R . . C34 C 0.2191(6) 0.2259(4) 0.5287(4) 0.061(2) Uani 1 1 d . . . H34A H 0.1421 0.2513 0.5352 0.073 Uiso 1 1 calc R . . H34B H 0.2475 0.2715 0.5145 0.073 Uiso 1 1 calc R . . N3 N 0.2126(4) 0.5480(3) -0.2771(3) 0.0451(13) Uani 1 1 d . . . N4 N 0.0096(4) 0.9048(3) -0.0552(3) 0.0333(11) Uani 1 1 d . . . C35 C 0.1144(7) 0.4473(5) -0.4000(5) 0.074(2) Uani 1 1 d . . . H35A H 0.1340 0.4778 -0.4405 0.088 Uiso 1 1 calc R . . C36 C 0.0331(8) 0.4138(7) -0.4081(7) 0.098(4) Uani 1 1 d . . . H36A H -0.0018 0.4217 -0.4541 0.117 Uiso 1 1 calc R . . C37 C 0.0054(8) 0.3705(8) -0.3500(9) 0.110(4) Uani 1 1 d . . . H37A H -0.0495 0.3483 -0.3553 0.132 Uiso 1 1 calc R . . C38 C 0.0552(9) 0.3585(6) -0.2845(7) 0.101(4) Uani 1 1 d . . . H38A H 0.0363 0.3267 -0.2446 0.121 Uiso 1 1 calc R . . C39 C 0.1335(7) 0.3923(5) -0.2750(5) 0.073(2) Uani 1 1 d . . . H39A H 0.1660 0.3857 -0.2281 0.087 Uiso 1 1 calc R . . C40 C 0.1643(6) 0.4358(4) -0.3340(4) 0.0538(19) Uani 1 1 d . . . C41 C 0.2507(6) 0.4700(4) -0.3242(4) 0.058(2) Uani 1 1 d . . . H41A H 0.2763 0.4845 -0.3739 0.070 Uiso 1 1 calc R . . H41B H 0.3097 0.4263 -0.2996 0.070 Uiso 1 1 calc R . . C42 C 0.1515(5) 0.6214(4) -0.3080(4) 0.0488(17) Uani 1 1 d . . . H42A H 0.1341 0.6235 -0.3591 0.059 Uiso 1 1 calc R . . C43 C 0.1137(5) 0.6933(4) -0.2668(3) 0.0409(15) Uani 1 1 d . . . H43A H 0.0716 0.7450 -0.2896 0.049 Uiso 1 1 calc R . . C44 C 0.1376(4) 0.6900(3) -0.1912(3) 0.0327(13) Uani 1 1 d . . . C45 C 0.2010(4) 0.6121(4) -0.1612(3) 0.0365(14) Uani 1 1 d . . . H45A H 0.2184 0.6073 -0.1099 0.044 Uiso 1 1 calc R . . C46 C 0.2379(5) 0.5430(4) -0.2055(4) 0.0413(15) Uani 1 1 d . . . H46A H 0.2821 0.4907 -0.1849 0.050 Uiso 1 1 calc R . . C47 C 0.0955(4) 0.7655(3) -0.1439(3) 0.0304(13) Uani 1 1 d . . . C48 C 0.0580(4) 0.8475(3) -0.1756(3) 0.0333(13) Uani 1 1 d . . . H48A H 0.0620 0.8561 -0.2284 0.040 Uiso 1 1 calc R . . C49 C 0.0157(5) 0.9149(3) -0.1300(3) 0.0369(14) Uani 1 1 d . . . H49A H -0.0101 0.9703 -0.1518 0.044 Uiso 1 1 calc R . . C50 C 0.0468(5) 0.8275(4) -0.0231(3) 0.0373(14) Uani 1 1 d . . . H50A H 0.0434 0.8209 0.0299 0.045 Uiso 1 1 calc R . . C51 C 0.0898(5) 0.7575(3) -0.0665(3) 0.0366(14) Uani 1 1 d . . . H51A H 0.1159 0.7029 -0.0431 0.044 Uiso 1 1 calc R . . C52 C -0.0399(5) 0.9797(3) -0.0079(3) 0.0393(15) Uani 1 1 d . . . H52A H -0.0673 0.9620 0.0399 0.047 Uiso 1 1 calc R . . H52B H -0.0993 1.0210 -0.0342 0.047 Uiso 1 1 calc R . . O5 O 0.2327(3) 0.9474(2) -0.1102(2) 0.0363(10) Uani 1 1 d . . . O6 O 0.0689(3) 1.1151(2) -0.1513(2) 0.0397(10) Uani 1 1 d . . . O7 O -0.1316(3) 1.1018(2) -0.1594(2) 0.0403(10) Uani 1 1 d . . . O8 O 0.2651(3) 0.8633(2) 0.0184(2) 0.0361(10) Uani 1 1 d . . . C53 C 0.3029(4) 0.8163(3) -0.0443(3) 0.0322(13) Uani 1 1 d . . . C54 C 0.3571(4) 0.7311(3) -0.0429(3) 0.0327(13) Uani 1 1 d . . . H54A H 0.3721 0.7014 0.0039 0.039 Uiso 1 1 calc R . . C55 C 0.3913(4) 0.6866(4) -0.1103(3) 0.0362(14) Uani 1 1 d . . . C56 C 0.4473(5) 0.5986(4) -0.1101(4) 0.0421(15) Uani 1 1 d . . . H56A H 0.4642 0.5680 -0.0639 0.050 Uiso 1 1 calc R . . C57 C 0.4772(5) 0.5574(4) -0.1764(4) 0.0458(17) Uani 1 1 d . . . H57A H 0.5153 0.4983 -0.1757 0.055 Uiso 1 1 calc R . . C58 C 0.4522(5) 0.6013(4) -0.2449(4) 0.0493(17) Uani 1 1 d . . . H58A H 0.4723 0.5717 -0.2904 0.059 Uiso 1 1 calc R . . C59 C 0.3993(5) 0.6864(4) -0.2469(4) 0.0421(15) Uani 1 1 d . . . H59A H 0.3828 0.7157 -0.2938 0.050 Uiso 1 1 calc R . . C60 C 0.3690(5) 0.7308(4) -0.1801(3) 0.0374(14) Uani 1 1 d . . . C61 C 0.3150(4) 0.8201(3) -0.1802(3) 0.0328(13) Uani 1 1 d . . . H61A H 0.3001 0.8509 -0.2265 0.039 Uiso 1 1 calc R . . C62 C 0.2845(4) 0.8614(3) -0.1143(3) 0.0333(13) Uani 1 1 d . . . C63 C 0.2290(5) 0.9949(4) -0.1798(3) 0.0392(15) Uani 1 1 d . . . H63A H 0.1874 0.9780 -0.2162 0.047 Uiso 1 1 calc R . . H63B H 0.3007 0.9831 -0.2016 0.047 Uiso 1 1 calc R . . C64 C 0.1795(5) 1.0879(4) -0.1645(4) 0.0422(15) Uani 1 1 d . . . H64A H 0.2119 1.1008 -0.1201 0.051 Uiso 1 1 calc R . . H64B H 0.1952 1.1208 -0.2078 0.051 Uiso 1 1 calc R . . C65 C 0.0131(5) 1.1293(4) -0.2189(3) 0.0391(15) Uani 1 1 d . . . H65A H 0.0291 1.0753 -0.2451 0.047 Uiso 1 1 calc R . . H65B H 0.0345 1.1693 -0.2525 0.047 Uiso 1 1 calc R . . C66 C -0.1014(5) 1.1652(4) -0.2003(3) 0.0398(15) Uani 1 1 d . . . H66A H -0.1168 1.2160 -0.1697 0.048 Uiso 1 1 calc R . . H66B H -0.1410 1.1818 -0.2469 0.048 Uiso 1 1 calc R . . C67 C -0.2421(5) 1.1213(4) -0.1519(3) 0.0400(15) Uani 1 1 d . . . H67A H -0.2572 1.0681 -0.1423 0.048 Uiso 1 1 calc R . . H67B H -0.2740 1.1468 -0.1997 0.048 Uiso 1 1 calc R . . C68 C 0.2920(5) 0.8187(4) 0.0895(3) 0.0371(14) Uani 1 1 d . . . H68A H 0.3690 0.7970 0.0940 0.044 Uiso 1 1 calc R . . H68B H 0.2668 0.7700 0.0929 0.044 Uiso 1 1 calc R . . B1 B 0.2512(7) 0.5924(4) 0.0850(5) 0.048(2) Uani 1 1 d . . . F1 F 0.3354(5) 0.6082(3) 0.1130(4) 0.112(2) Uani 1 1 d . . . F2 F 0.2715(5) 0.5692(3) 0.0125(3) 0.108(2) Uani 1 1 d . . . F3 F 0.1685(4) 0.6677(2) 0.0857(3) 0.0774(13) Uani 1 1 d . . . F4 F 0.2240(4) 0.5321(2) 0.1280(3) 0.0779(14) Uani 1 1 d . . . B2 B 0.6332(18) 0.5895(6) -0.4385(7) 0.136(7) Uani 1 1 d . . . F5 F 0.6701(6) 0.5965(4) -0.3743(4) 0.141(3) Uani 1 1 d . . . F6 F 0.6073(13) 0.5263(6) -0.4422(8) 0.305(10) Uani 1 1 d . . . F7 F 0.5926(13) 0.6588(5) -0.4693(6) 0.303(9) Uani 1 1 d . . . F8 F 0.709(2) 0.5620(12) -0.4810(13) 0.55(2) Uani 1 1 d . . . B3 B 0.5286(9) 0.8923(6) 0.1461(5) 0.086(3) Uani 1 1 d DU . . F9 F 0.5898(5) 0.9324(7) 0.1459(8) 0.295(7) Uani 1 1 d DU . . F10 F 0.5538(16) 0.8371(7) 0.1982(5) 0.523(14) Uani 1 1 d DU . . F11 F 0.4383(5) 0.9478(5) 0.1636(4) 0.160(3) Uani 1 1 d DU . . F12 F 0.5361(4) 0.8475(4) 0.0890(3) 0.1101(19) Uani 1 1 d DU . . B4 B 0.7874(10) 0.0854(7) 0.3795(6) 0.075(3) Uani 1 1 d . . . F13 F 0.8611(6) 0.0930(7) 0.3348(3) 0.179(4) Uani 1 1 d . . . F14 F 0.7394(8) 0.0375(8) 0.3545(4) 0.216(6) Uani 1 1 d . . . F15 F 0.8130(5) 0.0704(5) 0.4503(3) 0.128(2) Uani 1 1 d . . . F16 F 0.7084(12) 0.1576(8) 0.3790(9) 0.304(8) Uani 1 1 d . . . N1S N 0.9180(10) 0.1564(12) 0.6145(6) 0.203(7) Uani 1 1 d . . . C1S C 0.9657(10) 0.1380(10) 0.5588(7) 0.123(5) Uani 1 1 d . . . C2S C 1.0201(8) 0.1124(7) 0.4904(6) 0.102(3) Uani 1 1 d . . . H2SA H 0.9910 0.0746 0.4661 0.153 Uiso 1 1 calc R . . H2SB H 1.0943 0.0825 0.4996 0.153 Uiso 1 1 calc R . . H2SC H 1.0130 0.1623 0.4578 0.153 Uiso 1 1 calc R . . N2S N 0.8655(14) 0.3397(9) 0.4852(7) 0.170(6) Uani 1 1 d . . . C3S C 0.7852(18) 0.3299(8) 0.4962(8) 0.141(6) Uani 1 1 d . . . C4S C 0.6834(15) 0.3181(10) 0.5044(9) 0.193(9) Uani 1 1 d . . . H4SA H 0.6275 0.3733 0.5020 0.290 Uiso 1 1 calc R . . H4SB H 0.6783 0.2899 0.5528 0.290 Uiso 1 1 calc R . . H4SC H 0.6762 0.2831 0.4639 0.290 Uiso 1 1 calc R . . N3S N 0.4183(12) 0.6505(9) 0.2695(7) 0.198(8) Uani 1 1 d . . . C5S C 0.3501(11) 0.6265(8) 0.2829(7) 0.116(4) Uani 1 1 d . . . C6S C 0.2684(8) 0.5942(8) 0.2979(6) 0.109(4) Uani 1 1 d . . . H6SA H 0.2420 0.6060 0.3497 0.163 Uiso 1 1 calc R . . H6SB H 0.2945 0.5328 0.2909 0.163 Uiso 1 1 calc R . . H6SC H 0.2117 0.6211 0.2634 0.163 Uiso 1 1 calc R . . N4S N 0.7831(14) 0.9107(9) -0.0580(11) 0.175(7) Uani 1 1 d . . . C7S C 0.7211(11) 0.9436(8) -0.0389(8) 0.085(4) Uani 1 1 d . . . C8S C 0.6170(13) 0.9999(11) -0.0051(10) 0.183(7) Uani 1 1 d . . . H2SA H 0.5894 0.9666 0.0309 0.275 Uiso 1 1 calc R . . H2SB H 0.5672 1.0228 -0.0451 0.275 Uiso 1 1 calc R . . H2SC H 0.6275 1.0467 0.0205 0.275 Uiso 1 1 calc R . . O1W O 0.6007(5) 0.6548(3) 0.1847(3) 0.0858(18) 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 N1 0.038(3) 0.031(3) 0.034(3) 0.003(2) -0.005(2) -0.012(2) N2 0.051(3) 0.028(3) 0.027(3) -0.001(2) 0.000(2) -0.015(2) C1 0.079(5) 0.035(4) 0.057(5) 0.011(3) -0.023(4) -0.010(4) C2 0.072(6) 0.066(6) 0.074(6) 0.006(5) -0.023(5) 0.009(5) C3 0.045(4) 0.091(7) 0.054(5) -0.014(4) -0.011(4) -0.002(4) C4 0.053(5) 0.059(5) 0.093(6) -0.023(4) -0.008(4) -0.028(4) C5 0.048(4) 0.039(4) 0.079(5) -0.007(4) -0.009(4) -0.010(3) C6 0.047(4) 0.028(3) 0.037(3) 0.007(3) -0.007(3) -0.007(3) C7 0.049(4) 0.035(3) 0.043(4) 0.013(3) -0.007(3) -0.015(3) C8 0.046(4) 0.033(3) 0.035(3) -0.001(3) 0.000(3) -0.009(3) C9 0.044(4) 0.022(3) 0.034(3) 0.001(3) -0.004(3) -0.004(3) C10 0.031(3) 0.025(3) 0.034(3) 0.001(2) 0.000(2) -0.012(2) C11 0.038(3) 0.024(3) 0.035(3) 0.000(3) -0.001(3) -0.009(3) C12 0.039(3) 0.026(3) 0.049(4) 0.000(3) -0.006(3) -0.013(3) C13 0.034(3) 0.027(3) 0.033(3) 0.001(3) -0.001(2) -0.012(3) C14 0.052(4) 0.024(3) 0.030(3) -0.006(3) -0.002(3) -0.007(3) C15 0.053(4) 0.022(3) 0.029(3) 0.000(3) -0.004(3) -0.007(3) C16 0.065(4) 0.025(3) 0.044(4) -0.008(3) 0.000(3) -0.019(3) C17 0.060(4) 0.021(3) 0.039(4) 0.001(3) 0.001(3) -0.012(3) C18 0.051(4) 0.031(3) 0.033(3) -0.005(3) -0.005(3) -0.011(3) O1 0.059(3) 0.033(2) 0.045(3) 0.000(2) -0.004(2) -0.016(2) O2 0.098(5) 0.033(3) 0.161(6) -0.027(3) -0.053(4) -0.007(3) O3 0.083(4) 0.029(2) 0.055(3) -0.018(2) -0.012(3) 0.000(2) O4 0.065(3) 0.032(2) 0.041(3) -0.007(2) 0.001(2) -0.001(2) C19 0.043(4) 0.037(4) 0.038(4) -0.001(3) 0.005(3) -0.005(3) C20 0.049(4) 0.037(4) 0.049(4) -0.006(3) 0.005(3) -0.008(3) C21 0.033(3) 0.041(4) 0.047(4) 0.005(3) 0.003(3) -0.007(3) C22 0.052(4) 0.043(4) 0.063(5) 0.003(4) 0.001(4) -0.007(3) C23 0.048(4) 0.043(4) 0.064(5) 0.013(4) 0.002(4) -0.008(3) C24 0.042(4) 0.060(5) 0.050(4) 0.016(4) -0.001(3) -0.014(3) C25 0.042(4) 0.056(4) 0.051(4) 0.004(3) 0.000(3) -0.022(3) C26 0.035(3) 0.048(4) 0.045(4) 0.005(3) -0.002(3) -0.015(3) C27 0.044(4) 0.039(4) 0.042(4) -0.003(3) -0.002(3) -0.014(3) C28 0.037(4) 0.034(4) 0.047(4) -0.002(3) 0.006(3) -0.011(3) C29 0.068(5) 0.042(4) 0.052(4) -0.005(3) -0.005(4) -0.027(4) C30 0.098(7) 0.043(4) 0.071(5) 0.001(4) -0.028(5) -0.031(4) C31 0.124(9) 0.045(6) 0.167(11) -0.036(6) -0.040(8) -0.027(6) C32 0.126(8) 0.026(4) 0.057(5) -0.010(3) -0.035(5) 0.003(4) C33 0.067(5) 0.055(5) 0.049(4) -0.014(4) 0.004(4) 0.001(4) C34 0.076(5) 0.043(4) 0.041(4) -0.009(3) 0.001(4) 0.010(4) N3 0.044(3) 0.035(3) 0.056(4) -0.018(3) 0.011(3) -0.013(3) N4 0.040(3) 0.020(2) 0.036(3) -0.008(2) 0.002(2) -0.005(2) C35 0.075(6) 0.053(5) 0.085(6) -0.039(4) 0.008(5) -0.009(4) C36 0.068(6) 0.080(7) 0.134(10) -0.069(7) -0.015(6) 0.000(5) C37 0.077(7) 0.121(10) 0.150(12) -0.086(9) 0.029(8) -0.051(7) C38 0.118(9) 0.086(7) 0.116(9) -0.056(7) 0.042(7) -0.058(7) C39 0.086(6) 0.051(5) 0.088(6) -0.032(4) 0.015(5) -0.031(5) C40 0.056(4) 0.038(4) 0.067(5) -0.030(4) 0.008(4) -0.013(3) C41 0.060(5) 0.038(4) 0.071(5) -0.033(4) 0.011(4) -0.009(3) C42 0.058(4) 0.046(4) 0.040(4) -0.008(3) 0.000(3) -0.014(3) C43 0.047(4) 0.031(3) 0.041(4) -0.007(3) 0.002(3) -0.008(3) C44 0.034(3) 0.024(3) 0.041(4) -0.004(3) 0.000(3) -0.012(3) C45 0.038(3) 0.030(3) 0.042(4) -0.004(3) -0.001(3) -0.011(3) C46 0.039(4) 0.028(3) 0.056(4) -0.009(3) -0.002(3) -0.009(3) C47 0.032(3) 0.021(3) 0.039(4) -0.003(2) 0.000(3) -0.010(2) C48 0.038(3) 0.023(3) 0.038(3) 0.001(3) -0.003(3) -0.009(3) C49 0.044(4) 0.018(3) 0.045(4) 0.000(3) -0.005(3) -0.006(3) C50 0.052(4) 0.029(3) 0.034(3) -0.003(3) -0.004(3) -0.017(3) C51 0.051(4) 0.021(3) 0.035(4) -0.001(3) -0.003(3) -0.008(3) C52 0.046(4) 0.025(3) 0.042(4) -0.013(3) 0.000(3) -0.004(3) O5 0.042(2) 0.020(2) 0.041(2) -0.0007(17) -0.0003(18) -0.0030(17) O6 0.043(2) 0.026(2) 0.045(3) -0.0022(18) -0.0010(19) -0.0057(18) O7 0.046(3) 0.026(2) 0.045(2) 0.0008(18) 0.0084(19) -0.0090(19) O8 0.044(2) 0.025(2) 0.036(2) -0.0056(18) 0.0004(18) -0.0070(18) C53 0.027(3) 0.027(3) 0.040(4) -0.003(3) 0.002(3) -0.007(2) C54 0.033(3) 0.027(3) 0.039(3) -0.004(3) 0.000(3) -0.011(3) C55 0.036(3) 0.028(3) 0.047(4) -0.008(3) -0.001(3) -0.013(3) C56 0.036(3) 0.026(3) 0.059(4) -0.007(3) -0.004(3) -0.003(3) C57 0.038(4) 0.024(3) 0.071(5) -0.011(3) -0.001(3) -0.005(3) C58 0.046(4) 0.046(4) 0.057(5) -0.022(4) 0.009(3) -0.017(3) C59 0.037(4) 0.041(4) 0.048(4) -0.014(3) 0.006(3) -0.013(3) C60 0.038(3) 0.032(3) 0.044(4) -0.005(3) -0.002(3) -0.014(3) C61 0.033(3) 0.024(3) 0.040(3) -0.003(3) -0.002(3) -0.007(2) C62 0.029(3) 0.025(3) 0.042(4) 0.000(3) -0.001(3) -0.005(2) C63 0.044(4) 0.031(3) 0.038(4) -0.001(3) 0.003(3) -0.009(3) C64 0.040(4) 0.030(3) 0.054(4) 0.007(3) -0.002(3) -0.009(3) C65 0.042(4) 0.031(3) 0.042(4) 0.011(3) -0.002(3) -0.010(3) C66 0.051(4) 0.026(3) 0.038(4) 0.010(3) -0.007(3) -0.008(3) C67 0.041(4) 0.037(3) 0.043(4) -0.002(3) -0.003(3) -0.014(3) C68 0.040(3) 0.030(3) 0.038(4) -0.001(3) 0.001(3) -0.008(3) B1 0.069(6) 0.024(4) 0.050(5) 0.008(3) -0.012(4) -0.015(4) F1 0.114(4) 0.086(4) 0.151(5) 0.059(4) -0.076(4) -0.050(3) F2 0.188(6) 0.074(3) 0.081(4) -0.020(3) 0.027(4) -0.071(4) F3 0.087(3) 0.035(2) 0.100(4) 0.017(2) -0.014(3) -0.009(2) F4 0.105(4) 0.034(2) 0.091(3) 0.018(2) -0.002(3) -0.021(2) B2 0.32(2) 0.020(5) 0.061(7) -0.009(5) -0.034(11) -0.045(9) F5 0.212(8) 0.066(4) 0.143(6) -0.008(4) -0.048(5) -0.039(4) F6 0.50(2) 0.111(6) 0.374(17) 0.075(8) -0.306(17) -0.165(10) F7 0.61(2) 0.065(5) 0.215(10) 0.018(5) -0.262(14) -0.064(8) F8 0.77(5) 0.30(2) 0.49(3) -0.12(2) 0.53(3) -0.13(2) B3 0.147(9) 0.073(7) 0.047(5) -0.022(4) 0.021(6) -0.050(6) F9 0.065(4) 0.280(10) 0.575(19) -0.320(11) 0.054(7) -0.076(5) F10 1.11(4) 0.163(10) 0.083(6) 0.011(6) 0.007(14) 0.051(12) F11 0.096(4) 0.251(8) 0.163(6) -0.155(6) 0.056(4) -0.090(5) F12 0.113(4) 0.129(5) 0.107(4) -0.078(4) 0.034(3) -0.061(4) B4 0.097(8) 0.080(7) 0.050(6) 0.009(5) -0.018(6) -0.033(7) F13 0.182(7) 0.367(13) 0.070(4) 0.047(6) -0.022(4) -0.201(9) F14 0.267(11) 0.395(16) 0.100(5) -0.073(7) 0.050(6) -0.260(12) F15 0.146(5) 0.195(7) 0.057(3) 0.033(4) -0.019(3) -0.080(5) F16 0.276(15) 0.194(11) 0.342(18) 0.048(11) -0.100(13) 0.054(11) N1S 0.146(11) 0.39(2) 0.070(7) 0.022(10) -0.002(7) -0.097(13) C1S 0.099(9) 0.205(14) 0.073(8) 0.032(9) -0.016(7) -0.064(9) C2S 0.084(7) 0.130(9) 0.101(8) 0.009(7) 0.006(6) -0.050(7) N2S 0.269(18) 0.175(12) 0.120(9) 0.044(8) -0.024(10) -0.149(13) C3S 0.26(2) 0.086(8) 0.095(9) -0.001(7) 0.017(12) -0.081(12) C4S 0.29(2) 0.155(14) 0.194(16) -0.058(12) 0.110(15) -0.155(16) N3S 0.248(15) 0.234(14) 0.200(13) -0.168(11) 0.128(11) -0.192(13) C5S 0.142(11) 0.103(9) 0.113(9) -0.058(7) 0.047(8) -0.057(8) C6S 0.086(7) 0.144(10) 0.097(8) 0.016(7) -0.004(6) -0.042(7) N4S 0.210(18) 0.109(12) 0.242(19) 0.023(11) -0.092(15) -0.093(12) C7S 0.092(9) 0.047(6) 0.104(8) 0.016(6) -0.003(7) -0.009(6) C8S 0.163(16) 0.183(16) 0.234(19) 0.025(15) -0.034(14) -0.096(14) O1W 0.101(4) 0.048(3) 0.087(4) 0.002(3) 0.009(3) -0.001(3) _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 N1 C8 1.342(7) . ? N1 C12 1.343(7) . ? N1 C7 1.491(7) . ? N2 C16 1.350(7) . ? N2 C15 1.349(7) . ? N2 C18 1.468(7) . ? C1 C6 1.366(9) . ? C1 C2 1.375(11) . ? C2 C3 1.366(12) . ? C3 C4 1.351(11) . ? C4 C5 1.360(10) . ? C5 C6 1.405(9) . ? C6 C7 1.490(8) . ? C8 C9 1.368(8) . ? C9 C10 1.397(8) . ? C10 C11 1.385(7) . ? C10 C13 1.474(8) . ? C11 C12 1.367(8) . ? C13 C14 1.393(8) . ? C13 C17 1.391(8) . ? C14 C15 1.357(8) . ? C16 C17 1.351(8) . ? C18 C18 1.538(12) 2_656 ? O1 C28 1.368(7) . ? O1 C29 1.438(7) . ? O2 C31 1.301(10) . ? O2 C30 1.400(10) . ? O3 C32 1.423(9) . ? O3 C33 1.441(9) . ? O4 C19 1.362(7) . ? O4 C34 1.439(7) . ? C19 C20 1.363(9) . ? C19 C28 1.428(8) . ? C20 C21 1.411(9) . ? C21 C26 1.413(9) . ? C21 C22 1.428(9) . ? C22 C23 1.367(10) . ? C23 C24 1.401(10) . ? C24 C25 1.363(9) . ? C25 C26 1.410(9) . ? C26 C27 1.426(9) . ? C27 C28 1.353(9) . ? C29 C30 1.487(10) . ? C31 C32 1.440(13) 2_656 ? C32 C31 1.440(13) 2_656 ? C33 C34 1.480(10) . ? N3 C46 1.331(8) . ? N3 C42 1.343(8) . ? N3 C41 1.511(7) . ? N4 C50 1.338(7) . ? N4 C49 1.342(7) . ? N4 C52 1.486(7) . ? C35 C40 1.361(11) . ? C35 C36 1.416(13) . ? C36 C37 1.357(16) . ? C37 C38 1.353(16) . ? C38 C39 1.386(13) . ? C39 C40 1.387(11) . ? C40 C41 1.494(10) . ? C42 C43 1.370(8) . ? C43 C44 1.399(8) . ? C44 C45 1.399(8) . ? C44 C47 1.483(7) . ? C45 C46 1.368(8) . ? C47 C51 1.384(8) . ? C47 C48 1.401(7) . ? C48 C49 1.366(7) . ? C50 C51 1.375(8) . ? C52 C52 1.507(12) 2_575 ? O5 C62 1.377(6) . ? O5 C63 1.443(7) . ? O6 C65 1.423(7) . ? O6 C64 1.427(7) . ? O7 C67 1.425(7) . ? O7 C66 1.430(7) . ? O8 C53 1.373(6) . ? O8 C68 1.445(7) . ? C53 C54 1.368(8) . ? C53 C62 1.422(8) . ? C54 C55 1.418(8) . ? C55 C60 1.414(8) . ? C55 C56 1.413(8) . ? C56 C57 1.370(9) . ? C57 C58 1.397(9) . ? C58 C59 1.364(9) . ? C59 C60 1.404(8) . ? C60 C61 1.428(8) . ? C61 C62 1.366(8) . ? C63 C64 1.507(8) . ? C65 C66 1.492(8) . ? C67 C68 1.508(8) 2_575 ? C68 C67 1.508(8) 2_575 ? B1 F2 1.357(9) . ? B1 F3 1.377(9) . ? B1 F1 1.380(9) . ? B1 F4 1.386(8) . ? B2 F7 1.226(13) . ? B2 F6 1.232(15) . ? B2 F8 1.22(2) . ? B2 F5 1.298(13) . ? B3 F9 1.236(10) . ? B3 F10 1.259(10) . ? B3 F12 1.272(8) . ? B3 F11 1.296(10) . ? B4 F13 1.289(12) . ? B4 F14 1.300(12) . ? B4 F15 1.320(11) . ? B4 F16 1.318(14) . ? N1S C1S 1.155(15) . ? C1S C2S 1.402(16) . ? N2S C3S 1.17(2) . ? C3S C4S 1.46(2) . ? N3S C5S 1.144(14) . ? C5S C6S 1.404(16) . ? N4S C7S 0.896(19) . ? C7S C8S 1.52(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 C8 N1 C12 120.7(5) . . ? C8 N1 C7 118.9(5) . . ? C12 N1 C7 120.4(5) . . ? C16 N2 C15 119.0(5) . . ? C16 N2 C18 121.5(5) . . ? C15 N2 C18 119.5(5) . . ? C6 C1 C2 121.1(7) . . ? C1 C2 C3 120.2(7) . . ? C4 C3 C2 119.1(7) . . ? C3 C4 C5 122.0(7) . . ? C4 C5 C6 119.5(7) . . ? C1 C6 C5 118.0(6) . . ? C1 C6 C7 120.4(6) . . ? C5 C6 C7 121.7(5) . . ? C6 C7 N1 113.0(5) . . ? N1 C8 C9 120.8(5) . . ? C8 C9 C10 120.1(5) . . ? C11 C10 C9 117.0(5) . . ? C11 C10 C13 122.7(5) . . ? C9 C10 C13 120.3(5) . . ? C12 C11 C10 121.2(5) . . ? N1 C12 C11 120.1(5) . . ? C14 C13 C17 116.9(5) . . ? C14 C13 C10 121.6(5) . . ? C17 C13 C10 121.4(5) . . ? C15 C14 C13 120.8(5) . . ? N2 C15 C14 121.1(5) . . ? C17 C16 N2 121.8(5) . . ? C16 C17 C13 120.4(5) . . ? N2 C18 C18 109.5(6) . 2_656 ? C28 O1 C29 117.0(5) . . ? C31 O2 C30 118.8(7) . . ? C32 O3 C33 114.3(6) . . ? C19 O4 C34 116.9(5) . . ? O4 C19 C20 125.1(6) . . ? O4 C19 C28 115.4(5) . . ? C20 C19 C28 119.5(6) . . ? C19 C20 C21 121.3(6) . . ? C26 C21 C20 119.2(6) . . ? C26 C21 C22 118.8(6) . . ? C20 C21 C22 122.0(6) . . ? C23 C22 C21 120.3(7) . . ? C22 C23 C24 120.4(6) . . ? C25 C24 C23 120.6(7) . . ? C24 C25 C26 120.9(7) . . ? C25 C26 C21 119.0(6) . . ? C25 C26 C27 122.5(6) . . ? C21 C26 C27 118.4(6) . . ? C28 C27 C26 121.2(6) . . ? C27 C28 O1 125.0(6) . . ? C27 C28 C19 120.2(6) . . ? O1 C28 C19 114.8(5) . . ? O1 C29 C30 109.0(5) . . ? O2 C30 C29 108.5(7) . . ? O2 C31 C32 118.3(9) . 2_656 ? O3 C32 C31 111.8(6) . 2_656 ? O3 C33 C34 110.6(6) . . ? O4 C34 C33 107.9(5) . . ? C46 N3 C42 120.9(5) . . ? C46 N3 C41 120.0(6) . . ? C42 N3 C41 119.1(6) . . ? C50 N4 C49 120.2(5) . . ? C50 N4 C52 119.9(5) . . ? C49 N4 C52 119.9(5) . . ? C40 C35 C36 120.0(10) . . ? C37 C36 C35 119.7(10) . . ? C36 C37 C38 120.5(10) . . ? C37 C38 C39 120.5(11) . . ? C40 C39 C38 120.0(9) . . ? C35 C40 C39 119.3(8) . . ? C35 C40 C41 120.9(8) . . ? C39 C40 C41 119.8(7) . . ? C40 C41 N3 110.5(5) . . ? N3 C42 C43 121.0(6) . . ? C42 C43 C44 119.6(6) . . ? C43 C44 C45 117.5(5) . . ? C43 C44 C47 121.4(5) . . ? C45 C44 C47 121.0(5) . . ? C46 C45 C44 120.1(6) . . ? N3 C46 C45 120.8(6) . . ? C51 C47 C48 117.4(5) . . ? C51 C47 C44 121.1(5) . . ? C48 C47 C44 121.5(5) . . ? C49 C48 C47 119.4(5) . . ? N4 C49 C48 121.8(5) . . ? N4 C50 C51 120.4(5) . . ? C50 C51 C47 120.9(5) . . ? N4 C52 C52 109.5(6) . 2_575 ? C62 O5 C63 115.3(4) . . ? C65 O6 C64 112.7(5) . . ? C67 O7 C66 113.6(4) . . ? C53 O8 C68 115.9(4) . . ? C54 C53 O8 124.4(5) . . ? C54 C53 C62 119.4(5) . . ? O8 C53 C62 116.1(5) . . ? C53 C54 C55 121.0(6) . . ? C60 C55 C56 118.5(5) . . ? C60 C55 C54 119.6(5) . . ? C56 C55 C54 121.9(6) . . ? C57 C56 C55 120.3(6) . . ? C56 C57 C58 120.6(6) . . ? C59 C58 C57 120.5(6) . . ? C58 C59 C60 120.3(6) . . ? C59 C60 C55 119.8(5) . . ? C59 C60 C61 121.8(6) . . ? C55 C60 C61 118.4(5) . . ? C62 C61 C60 120.6(5) . . ? C61 C62 O5 123.7(5) . . ? C61 C62 C53 120.8(5) . . ? O5 C62 C53 115.5(5) . . ? O5 C63 C64 108.7(5) . . ? O6 C64 C63 114.1(5) . . ? O6 C65 C66 109.0(5) . . ? O7 C66 C65 108.2(4) . . ? O7 C67 C68 113.2(5) . 2_575 ? O8 C68 C67 108.9(5) . 2_575 ? F2 B1 F3 107.2(6) . . ? F2 B1 F1 110.2(7) . . ? F3 B1 F1 106.9(6) . . ? F2 B1 F4 111.0(6) . . ? F3 B1 F4 109.3(7) . . ? F1 B1 F4 112.1(6) . . ? F7 B2 F6 127.2(18) . . ? F7 B2 F8 98.7(17) . . ? F6 B2 F8 93.7(14) . . ? F7 B2 F5 111.4(8) . . ? F6 B2 F5 113.9(11) . . ? F8 B2 F5 106(2) . . ? F9 B3 F10 107.4(11) . . ? F9 B3 F12 115.4(8) . . ? F10 B3 F12 102.2(8) . . ? F9 B3 F11 104.1(7) . . ? F10 B3 F11 108.7(9) . . ? F12 B3 F11 118.5(9) . . ? F13 B4 F14 113.8(10) . . ? F13 B4 F15 114.4(10) . . ? F14 B4 F15 114.6(10) . . ? F13 B4 F16 108.8(12) . . ? F14 B4 F16 98.3(12) . . ? F15 B4 F16 105.1(11) . . ? N1S C1S C2S 176.4(16) . . ? N2S C3S C4S 176.0(17) . . ? N3S C5S C6S 177.8(13) . . ? N4S C7S C8S 179(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.220 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.083