# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 1999 # CCDC Number: 440/129 #======================================================================= data_global #======================================================================= _audit_creation_date 17-03-99 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; Prof. Jean Fischer ; _publ_contact_author_address # Address of author for correspondance ; Universite Louis Pasteur Institut Le Bel Laboaratoire de Cristallochimie et de Chimie Structurale UMR 7513 4, rue Blaise Pascal 67070 Strasbourg cedex France ; _publ_contact_author_phone '+33 (0)3 88 41 60 58' _publ_contact_author_fax '+33 (0)3 88 41 53 63' _publ_contact_author_email fischer@chimie.u-strasbg.fr _publ_requested_journal 'New Journal of Chemistry' _publ_contact_letter ; ; _publ_requested_category FM #======================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ;A trefoil knot coordinated to two lithium ions : synthesis and structure ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Dietrich-Buchecker Christiane' ;Laboratoire de Chimie Organo-Minerale Umr 7513 CNRS Universite Louis Pasteur Institut Le Bel 4, rue Blaise pascal 67070 Strasbourg France ; 'Sauvage Jean-Pierre' ;Laboratoire de Chimie Organo-Minerale Umr 7513 CNRS Universite Louis Pasteur Institut Le Bel 4, rue Blaise pascal 67070 Strasbourg France ; 'Hwang Neri Geum' ;Department of Chemistry Dankook University Chenoan 330-714 Korea ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; Backgrounds were obtained from analysis of the scan profile (Blessing, Coppens & Becker, 1974) ; _publ_section_references ; Blessing, R.H., Coppens, P. & Becker, P. (1974). J. Appl. Cryst., 7, 488-492. Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. Philips PW1100, Operation Manual, Eindhoven, 1974. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158-166. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #======================================================================= # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st805 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C114 H102 Cu2 F12 N8 O14 P2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C114 H102 Cu2 F12 N8 O14 P2' _chemical_formula_weight 2225.14 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.017 0.009 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cu ? -2.019 0.589 International_Tables_Vol_IV_Table_2.3.1 F ? 0.069 0.053 International_Tables_Vol_IV_Table_2.3.1 N ? 0.029 0.018 International_Tables_Vol_IV_Table_2.3.1 O ? 0.047 0.032 International_Tables_Vol_IV_Table_2.3.1 P ? 0.283 0.434 International_Tables_Vol_IV_Table_2.3.1 #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall ' P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,+z 1/2-x,1/2+y,-z 1/2+x,1/2-y,-z _cell_length_a 29.084(9) _cell_length_b 14.692(4) _cell_length_c 11.795(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5040(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 19.5 _cell_measurement_theta_max 21.0 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2300 _exptl_absorpt_coefficient_mu 1.612 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.7474 _exptl_absorpt_correction_T_max 1.0000 #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; Maximum theta limited to 54 degrees by cooling device ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type Cu-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Philips_PW1100 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 1 5 6 -6 1 0 3 -5 _diffrn_reflns_number 3424 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 54.08 _reflns_number_total 3424 _reflns_number_gt 2776 _reflns_threshold_expression >3.0\s(I) _computing_data_collection 'Philips/PW1100/16 software 1976' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'pwredu, local program' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^)+0.0016 Fo^4^)+4.0' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack -0.09(7) _refine_ls_number_reflns 2776 _refine_ls_number_parameters 646 _refine_ls_number_restraints 16 _refine_ls_number_constraints 16 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39,876-881' _refine_ls_R_factor_all 0.080 _refine_ls_R_factor_gt 0.064 _refine_ls_wR_factor_all 0.093 _refine_ls_wR_factor_ref 0.088 _refine_ls_goodness_of_fit_all 1.526 _refine_ls_goodness_of_fit_ref 1.469 _refine_ls_shift/su_max 0.009 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.797 _refine_diff_density_min -0.695 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CU1 1.0000 1.0000 0.7392(2) 0.042(1) 0.500 Uani ? ? Cu CU2 1.0000 1.0000 0.3294(2) 0.042(1) 0.500 Uani ? ? Cu N1 0.9697(2) 0.8805(6) 0.6791(7) 0.042(4) 1.000 Uani ? ? N C1 0.9247(3) 0.8747(8) 0.7128(9) 0.050(6) 1.000 Uani ? ? C C2 0.9058(3) 0.9504(7) 0.7691(9) 0.042(5) 1.000 Uani ? ? C N2 0.9333(3) 1.0201(6) 0.7995(7) 0.047(5) 1.000 Uani ? ? N C3 0.9155(3) 1.0950(8) 0.8514(9) 0.050(6) 1.000 Uani ? ? C C4 0.8685(4) 1.0999(8) 0.872(1) 0.065(7) 1.000 Uani ? ? C C5 0.8396(4) 1.028(1) 0.844(1) 0.074(8) 1.000 Uani ? ? C C6 0.8573(4) 0.9492(8) 0.796(1) 0.059(6) 1.000 Uani ? ? C C7 0.8308(3) 0.8735(9) 0.774(1) 0.062(7) 1.000 Uani ? ? C C8 0.8517(4) 0.7968(9) 0.729(1) 0.066(7) 1.000 Uani ? ? C C9 0.8987(4) 0.7950(8) 0.695(1) 0.055(6) 1.000 Uani ? ? C C10 0.9209(4) 0.7210(8) 0.647(1) 0.063(7) 1.000 Uani ? ? C C11 0.9650(4) 0.7260(7) 0.6142(9) 0.052(6) 1.000 Uani ? ? C C12 0.9880(3) 0.8091(6) 0.6256(8) 0.039(5) 1.000 Uani ? ? C C13 0.9469(4) 1.1673(7) 0.8817(9) 0.053(6) 1.000 Uani ? ? C C14 0.9924(4) 1.1492(7) 0.9239(9) 0.054(6) 1.000 Uani ? ? C C15 1.0225(4) 1.2165(8) 0.9485(9) 0.054(6) 1.000 Uani ? ? C C16 1.0093(4) 1.3056(8) 0.9345(9) 0.064(7) 1.000 Uani ? ? C C17 0.9659(5) 1.3257(8) 0.897(1) 0.067(7) 1.000 Uani ? ? C C18 0.9345(4) 1.2584(7) 0.871(1) 0.060(7) 1.000 Uani ? ? C O1 1.0375(3) 1.3797(6) 0.9515(8) 0.083(6) 1.000 Uani ? ? O C19 1.0836(5) 1.358(1) 0.976(1) 0.09(1) 1.000 Uani ? ? C C20 1.0345(3) 0.8208(6) 0.5781(9) 0.040(5) 1.000 Uani ? ? C C21 1.0661(4) 0.7517(7) 0.5700(9) 0.053(6) 1.000 Uani ? ? C C22 1.1084(4) 0.7667(8) 0.519(1) 0.067(7) 1.000 Uani ? ? C C23 1.1203(3) 0.8544(8) 0.477(1) 0.055(6) 1.000 Uani ? ? C C24 1.0884(3) 0.9228(7) 0.4847(8) 0.039(5) 1.000 Uani ? ? C C25 1.0462(3) 0.9044(6) 0.5349(9) 0.039(5) 1.000 Uani ? ? C C26 1.0960(3) 1.0134(7) 0.4365(7) 0.039(5) 1.000 Uani ? ? C C27 1.1401(3) 1.0582(8) 0.449(1) 0.052(6) 1.000 Uani ? ? C C28 1.1435(3) 1.1461(8) 0.414(1) 0.062(6) 1.000 Uani ? ? C C29 1.1064(4) 1.1921(7) 0.3656(9) 0.050(6) 1.000 Uani ? ? C C30 1.1071(4) 1.2858(8) 0.335(1) 0.065(7) 1.000 Uani ? ? C C31 1.0711(4) 1.3268(7) 0.291(1) 0.055(6) 1.000 Uani ? ? C C32 1.0286(4) 1.2774(7) 0.2658(9) 0.051(6) 1.000 Uani ? ? C C33 0.9892(4) 1.3163(7) 0.220(1) 0.059(7) 1.000 Uani ? ? C C34 0.9524(4) 1.2623(8) 0.194(1) 0.061(7) 1.000 Uani ? ? C C35 0.9536(3) 1.1676(7) 0.216(1) 0.048(6) 1.000 Uani ? ? C N3 1.0607(2) 1.0561(5) 0.3871(7) 0.031(4) 1.000 Uani ? ? N N4 0.9911(2) 1.1302(5) 0.2651(6) 0.042(4) 1.000 Uani ? ? N C36 1.0273(3) 1.1846(7) 0.2911(9) 0.046(6) 1.000 Uani ? ? C C37 1.0660(3) 1.1411(7) 0.3526(8) 0.043(5) 1.000 Uani ? ? C C38 0.9172(4) 1.1074(7) 0.1814(9) 0.048(6) 1.000 Uani ? ? C C39 0.8707(4) 1.1332(8) 0.1898(9) 0.054(6) 1.000 Uani ? ? C C40 0.8357(4) 1.0753(9) 0.165(1) 0.063(7) 1.000 Uani ? ? C C41 0.8448(4) 0.9888(9) 0.1303(9) 0.062(6) 1.000 Uani ? ? C C42 0.8900(4) 0.9609(8) 0.114(1) 0.059(7) 1.000 Uani ? ? C C43 0.9255(3) 1.0187(8) 0.1407(9) 0.053(6) 1.000 Uani ? ? C O2 0.8080(3) 0.9329(7) 0.1078(8) 0.084(6) 1.000 Uani ? ? O C44 0.8150(5) 0.844(1) 0.076(1) 0.082(9) 1.000 Uani ? ? C C45 0.7693(5) 0.798(1) 0.058(2) 0.10(1) 1.000 Uani ? ? C O3 0.7453(3) 0.7787(7) 0.157(1) 0.101(7) 1.000 Uani ? ? O C46 0.7598(5) 0.6926(9) 0.204(1) 0.086(9) 1.000 Uani ? ? C C47 0.7389(5) 0.683(1) 0.320(1) 0.10(1) 1.000 Uani ? ? C O4 0.7599(3) 0.7400(6) 0.401(1) 0.091(6) 1.000 Uani ? ? O C48 0.7439(4) 0.733(1) 0.516(1) 0.10(1) 1.000 Uani ? ? C C49 0.7666(9) 0.654(1) 0.575(1) 0.14(1) 1.000 Uani ? ? C O5 0.7415(4) 0.5783(8) 0.5438(9) 0.195(4) 1.000 Uiso ? ? O C50 0.7629 0.4980 0.6031 0.2022 1.000 Uiso ? ? C C51 0.8070 0.4988 0.5885 0.2022 1.000 Uiso ? ? C O6 0.8306 0.5051 0.6849 0.2022 1.000 Uiso ? ? O C52 0.8381 0.4401 0.7517 0.2022 1.000 Uiso ? ? C C53 0.8462(6) 0.459(1) 0.867(1) 0.10(1) 1.000 Uani ? ? C O7 0.8852(4) 0.5179(8) 0.8734(8) 0.113(7) 1.000 Uani ? ? O C54 0.8896(6) 0.552(1) 0.986(1) 0.10(1) 1.000 Uani ? ? C P1 0.6835(1) 0.9156(3) 0.7645(3) 0.081(2) 1.000 Uani ? ? P F1 0.7105(4) 0.9605(6) 0.8682(8) 0.126(7) 1.000 Uani ? ? F F2 0.7251(3) 0.9436(6) 0.6871(8) 0.113(6) 1.000 Uani ? ? F F3 0.6467(3) 0.8837(7) 0.8526(9) 0.134(7) 1.000 Uani ? ? F F4 0.7115(4) 0.8229(6) 0.791(1) 0.132(7) 1.000 Uani ? ? F F5 0.6591(3) 0.8654(9) 0.666(1) 0.153(8) 1.000 Uani ? ? F F6 0.6618(3) 1.0091(7) 0.741(1) 0.150(8) 1.000 Uani ? ? F C55 1.0000 0.5000 0.453(2) 0.09(1) 0.500 Uani ? ? C C56 0.9604(6) 0.493(1) 0.513(2) 0.11(1) 1.000 Uani ? ? C C57 0.9605(7) 0.493(1) 0.634(2) 0.12(1) 1.000 Uani ? ? C C58 1.0000 0.5000 0.674(2) 0.15(2) 0.500 Uani ? ? C H1 0.8559 1.1532 0.9054 0.0855 1.000 Uiso calc C4 H H2 0.8075 1.0332 0.8579 0.1024 1.000 Uiso calc C5 H H3 0.7987 0.8740 0.7886 0.0866 1.000 Uiso calc C7 H H4 0.8340 0.7430 0.7204 0.0884 1.000 Uiso calc C8 H H5 0.9046 0.6656 0.6373 0.0821 1.000 Uiso calc C10 H H6 0.9802 0.6743 0.5838 0.0675 1.000 Uiso calc C11 H H7 1.0016 1.0878 0.9348 0.0700 1.000 Uiso calc C14 H H8 1.0524 1.2023 0.9753 0.0712 1.000 Uiso calc C15 H H9 0.9572 1.3876 0.8891 0.0900 1.000 Uiso calc C17 H H10 0.9045 1.2743 0.8466 0.0798 1.000 Uiso calc C18 H H11 1.0962 1.3214 0.9173 0.1218 1.000 Uiso calc C19 H H12 1.0852 1.3252 1.0460 0.1218 1.000 Uiso calc C19 H H13 1.0590 0.6933 0.5998 0.0699 1.000 Uiso calc C21 H H14 1.1296 0.7179 0.5112 0.0878 1.000 Uiso calc C22 H H15 1.1497 0.8653 0.4444 0.0742 1.000 Uiso calc C23 H H16 1.0243 0.9522 0.5396 0.0504 1.000 Uiso calc C25 H H17 1.1658 1.0270 0.4797 0.0704 1.000 Uiso calc C27 H H18 1.1719 1.1772 0.4234 0.0826 1.000 Uiso calc C28 H H19 1.1345 1.3199 0.3472 0.0847 1.000 Uiso calc C30 H H20 1.0727 1.3900 0.2744 0.0743 1.000 Uiso calc C31 H H21 0.9879 1.3799 0.2057 0.0782 1.000 Uiso calc C33 H H22 0.9256 1.2886 0.1617 0.0792 1.000 Uiso calc C34 H H23 0.8636 1.1932 0.2139 0.0714 1.000 Uiso calc C39 H H24 0.8048 1.0954 0.1710 0.0865 1.000 Uiso calc C40 H H25 0.8963 0.9022 0.0837 0.0773 1.000 Uiso calc C42 H H26 0.9563 0.9985 0.1318 0.0699 1.000 Uiso calc C43 H H27 0.8317 0.8131 0.1331 0.1067 1.000 Uiso calc C44 H H28 0.8320 0.8428 0.0069 0.1067 1.000 Uiso calc C44 H H29 0.7746 0.7425 0.0192 0.1359 1.000 Uiso calc C45 H H30 0.7507 0.8367 0.0127 0.1359 1.000 Uiso calc C45 H H31 0.7924 0.6910 0.2094 0.1141 1.000 Uiso calc C46 H H32 0.7496 0.6444 0.1564 0.1141 1.000 Uiso calc C46 H H33 0.7423 0.6213 0.3442 0.1299 1.000 Uiso calc C47 H H34 0.7071 0.6974 0.3158 0.1299 1.000 Uiso calc C47 H H35 0.7115 0.7247 0.5158 0.1422 1.000 Uiso calc C48 H H36 0.7511 0.7881 0.5549 0.1422 1.000 Uiso calc C48 H H37 0.7656 0.6622 0.6552 0.2598 1.000 Uiso calc C49 H H38 0.7977 0.6483 0.5516 0.2598 1.000 Uiso calc C49 H H39 0.7505 0.4433 0.5727 0.2628 1.000 Uiso calc C50 H H40 0.7562 0.5011 0.6818 0.2628 1.000 Uiso calc C50 H H41 0.8146 0.5494 0.5421 0.2628 1.000 Uiso calc C51 H H42 0.8156 0.4440 0.5513 0.2628 1.000 Uiso calc C51 H H43 0.8644 0.4088 0.7240 0.2628 1.000 Uiso calc C52 H H44 0.8121 0.4011 0.7482 0.2628 1.000 Uiso calc C52 H H45 0.8523 0.4038 0.9066 0.1337 1.000 Uiso calc C53 H H46 0.8201 0.4878 0.8992 0.1337 1.000 Uiso calc C53 H H47 1.1398 1.4382 1.0184 0.1356 1.000 Uiso calc ? H H48 1.0938 1.4905 1.0317 0.1356 1.000 Uiso calc ? H H49 1.0000 0.5000 0.3721 0.1247 0.500 Uiso calc C55 H H50 0.9320 0.4878 0.4737 0.1607 1.000 Uiso calc C56 H H51 0.9335 0.4878 0.6794 0.2089 1.000 Uiso calc C57 H H52 1.0000 0.5000 0.7550 0.2200 0.500 Uiso calc C58 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol CU1 0.0303(8) 0.045(1) 0.056(1) -0.001(1) 0.0000 0.0000 Cu CU2 0.0341(9) 0.043(1) 0.052(1) -0.006(1) 0.0000 0.0000 Cu N1 0.030(4) 0.058(5) 0.042(4) -0.010(4) 0.001(4) -0.000(4) N C1 0.037(5) 0.064(6) 0.052(6) 0.002(5) -0.005(5) 0.010(6) C C2 0.030(5) 0.056(6) 0.043(6) -0.004(5) -0.002(5) 0.005(5) C N2 0.041(4) 0.062(6) 0.040(4) 0.007(4) 0.006(4) 0.009(4) N C3 0.043(5) 0.060(6) 0.048(6) 0.012(5) 0.009(5) 0.010(6) C C4 0.055(6) 0.058(7) 0.084(8) 0.013(6) 0.012(6) 0.010(7) C C5 0.055(6) 0.12(1) 0.064(7) 0.038(6) 0.002(6) 0.027(7) C C6 0.047(6) 0.084(8) 0.051(6) 0.019(6) -0.010(5) 0.019(6) C C7 0.036(5) 0.093(8) 0.071(7) -0.023(6) -0.009(6) 0.018(8) C C8 0.047(5) 0.087(8) 0.070(7) -0.034(6) -0.009(6) 0.012(7) C C9 0.050(6) 0.056(6) 0.060(7) -0.026(5) -0.005(6) 0.007(6) C C10 0.064(7) 0.057(7) 0.069(8) -0.024(6) -0.004(6) -0.002(7) C C11 0.054(6) 0.050(6) 0.052(6) 0.000(5) 0.002(5) 0.004(6) C C12 0.043(6) 0.029(4) 0.046(5) -0.003(4) -0.005(4) -0.002(4) C C13 0.073(7) 0.056(6) 0.036(6) 0.018(6) 0.018(5) -0.002(5) C C14 0.052(6) 0.054(6) 0.056(6) 0.013(5) 0.007(6) -0.008(5) C C15 0.064(6) 0.056(6) 0.044(6) 0.005(6) 0.005(6) -0.009(6) C C16 0.069(7) 0.070(7) 0.054(6) -0.002(7) 0.018(6) -0.015(6) C C17 0.093(9) 0.050(6) 0.065(7) 0.011(7) 0.003(7) -0.002(7) C C18 0.079(7) 0.045(6) 0.061(7) 0.020(6) 0.012(6) 0.002(6) C O1 0.093(6) 0.068(5) 0.092(6) -0.015(5) 0.006(6) -0.000(5) O C19 0.11(1) 0.09(1) 0.082(9) -0.015(9) -0.016(9) -0.013(9) C C20 0.039(5) 0.036(5) 0.046(6) 0.002(5) 0.002(5) -0.010(5) C C21 0.066(6) 0.043(6) 0.053(7) 0.016(5) -0.002(6) 0.005(5) C C22 0.065(6) 0.059(6) 0.079(8) 0.025(6) 0.023(6) 0.000(7) C C23 0.038(5) 0.070(7) 0.063(7) 0.009(5) 0.017(6) -0.001(7) C C24 0.037(5) 0.048(5) 0.032(5) -0.003(5) -0.003(4) -0.001(5) C C25 0.034(4) 0.043(5) 0.040(5) 0.004(4) -0.011(5) 0.002(5) C C26 0.035(4) 0.052(6) 0.033(5) -0.003(5) 0.004(4) -0.002(5) C C27 0.037(5) 0.072(7) 0.054(6) -0.006(5) 0.002(5) 0.011(6) C C28 0.044(5) 0.078(7) 0.068(7) -0.042(5) -0.010(6) 0.002(7) C C29 0.045(5) 0.051(6) 0.053(7) -0.011(5) 0.002(5) -0.001(6) C C30 0.077(7) 0.059(7) 0.060(7) -0.024(6) 0.009(7) -0.001(7) C C31 0.071(7) 0.037(5) 0.064(7) -0.012(5) 0.018(6) 0.005(6) C C32 0.068(7) 0.042(6) 0.046(6) 0.000(5) 0.002(6) -0.002(5) C C33 0.067(7) 0.044(6) 0.070(7) -0.001(6) 0.005(6) 0.003(6) C C34 0.065(7) 0.066(7) 0.051(7) 0.023(6) 0.007(6) -0.000(6) C C35 0.039(5) 0.047(6) 0.060(7) 0.003(5) -0.001(5) 0.004(6) C N3 0.022(3) 0.025(4) 0.055(5) -0.000(3) 0.000(4) 0.001(4) N N4 0.040(4) 0.043(4) 0.041(4) 0.000(4) 0.006(4) 0.000(4) N C36 0.046(5) 0.052(6) 0.041(6) -0.009(5) 0.013(5) -0.005(5) C C37 0.039(5) 0.051(6) 0.039(6) -0.002(5) 0.007(5) 0.001(5) C C38 0.058(6) 0.046(6) 0.042(6) 0.014(5) 0.001(5) 0.007(5) C C39 0.060(6) 0.065(7) 0.039(6) 0.009(6) -0.002(5) -0.002(6) C C40 0.038(5) 0.088(8) 0.074(8) 0.008(6) -0.012(6) 0.001(8) C C41 0.047(5) 0.085(8) 0.059(6) -0.012(6) -0.012(5) 0.015(8) C C42 0.057(6) 0.060(6) 0.061(7) 0.007(6) -0.003(6) -0.006(6) C C43 0.045(5) 0.070(8) 0.046(6) 0.003(6) -0.007(5) -0.001(6) C O2 0.067(5) 0.097(6) 0.089(6) -0.011(5) -0.011(5) 0.002(6) O C44 0.091(9) 0.083(9) 0.072(9) -0.010(8) -0.006(8) -0.005(8) C C45 0.084(9) 0.11(1) 0.11(1) -0.031(9) -0.02(1) -0.00(1) C O3 0.086(6) 0.091(6) 0.130(8) -0.014(6) 0.003(6) -0.001(7) O C46 0.084(9) 0.070(8) 0.11(1) -0.006(8) -0.001(9) 0.010(9) C C47 0.082(9) 0.11(1) 0.11(1) -0.040(8) -0.004(9) 0.01(1) C O4 0.067(5) 0.078(6) 0.147(8) -0.028(5) -0.017(6) -0.009(6) O C48 0.068(7) 0.13(1) 0.13(1) -0.038(8) 0.055(8) -0.05(1) C C49 0.43(3) 0.080(8) 0.09(1) -0.13(1) -0.11(1) 0.021(8) C C53 0.13(1) 0.11(1) 0.072(9) -0.03(1) -0.002(9) -0.004(9) C O7 0.125(7) 0.139(8) 0.084(6) -0.067(6) 0.013(6) -0.031(7) O C54 0.12(1) 0.12(1) 0.08(1) -0.049(9) 0.011(9) 0.01(1) C P1 0.082(2) 0.073(2) 0.090(2) -0.016(2) 0.010(2) -0.023(2) P F1 0.151(7) 0.115(6) 0.116(7) -0.032(6) -0.026(6) -0.019(6) F F2 0.103(5) 0.119(6) 0.118(6) -0.007(5) 0.028(5) 0.010(6) F F3 0.110(6) 0.145(7) 0.151(7) -0.037(6) 0.053(6) -0.050(7) F F4 0.133(7) 0.099(6) 0.176(9) 0.011(6) 0.013(8) -0.009(7) F F5 0.109(6) 0.22(1) 0.149(8) -0.016(7) -0.025(6) -0.087(7) F F6 0.138(7) 0.133(7) 0.18(1) 0.066(6) -0.014(7) 0.012(9) F C55 0.14(2) 0.06(1) 0.09(1) 0.00(1) 0.0000 0.0000 C C56 0.13(1) 0.050(7) 0.19(2) 0.008(9) -0.03(1) -0.01(1) C C57 0.25(2) 0.033(6) 0.20(2) 0.00(1) 0.12(1) 0.01(1) C C58 0.30(3) 0.10(2) 0.10(2) -0.09(2) 0.0000 0.0000 C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CU1 N1 2.089(9) . . ? CU1 N1 2.089(9) . 2_775 ? CU1 N2 2.087(9) . . ? CU1 N2 2.087(9) . 2_775 ? CU2 N3 2.065(8) . . ? CU2 N3 2.065(8) . 2_775 ? CU2 N4 2.074(9) . . ? CU2 N4 2.074(9) . 2_775 ? N1 C1 1.37(1) . . ? N1 C12 1.33(1) . . ? C1 C2 1.41(2) . . ? C1 C9 1.41(2) . . ? C2 N2 1.35(1) . . ? C2 C6 1.45(2) . . ? N2 C3 1.36(2) . . ? C3 C4 1.39(2) . . ? C3 C13 1.44(2) . . ? C4 C5 1.38(2) . . ? C5 C6 1.39(2) . . ? C6 C7 1.38(2) . . ? C7 C8 1.39(2) . . ? C8 C9 1.42(2) . . ? C9 C10 1.39(2) . . ? C10 C11 1.34(2) . . ? C11 C12 1.40(2) . . ? C12 C20 1.48(2) . . ? C13 C14 1.44(2) . . ? C13 C18 1.39(2) . . ? C14 C15 1.35(2) . . ? C15 C16 1.37(2) . . ? C16 C17 1.37(2) . . ? C16 O1 1.38(2) . . ? C17 C18 1.38(2) . . ? O1 C19 1.41(2) . . ? C19 C54 1.55(2) . 2_775 ? C20 C21 1.37(2) . . ? C20 C25 1.37(2) . . ? C21 C22 1.39(2) . . ? C22 C23 1.42(2) . . ? C23 C24 1.37(2) . . ? C24 C25 1.39(1) . . ? C24 C26 1.46(2) . . ? C26 C27 1.45(2) . . ? C26 N3 1.34(1) . . ? C27 C28 1.36(2) . . ? C28 C29 1.40(2) . . ? C29 C30 1.42(2) . . ? C29 C37 1.40(2) . . ? C30 C31 1.32(2) . . ? C31 C32 1.46(2) . . ? C32 C33 1.39(2) . . ? C32 C36 1.40(2) . . ? C33 C34 1.36(2) . . ? C34 C35 1.41(2) . . ? C35 N4 1.35(1) . . ? C35 C38 1.44(2) . . ? N3 C37 1.32(1) . . ? N4 C36 1.36(1) . . ? C36 C37 1.48(2) . . ? C38 C39 1.41(2) . . ? C38 C43 1.41(2) . . ? C39 C40 1.36(2) . . ? C40 C41 1.36(2) . . ? C41 C42 1.39(2) . . ? C41 O2 1.37(2) . . ? C42 C43 1.37(2) . . ? O2 C44 1.37(2) . . ? C44 C45 1.50(2) . . ? C45 O3 1.39(2) . . ? O3 C46 1.44(2) . . ? C46 C47 1.51(3) . . ? C47 O4 1.41(2) . . ? O4 C48 1.44(2) . . ? C48 C49 1.51(3) . . ? C49 O5 1.38(2) . . ? O5 C50 1.51(1) . . ? C50 C51 1.2938 . . ? C50 O6 2.1955 . . ? C51 O6 1.3313 . . ? O6 C52 1.2570 . . ? C52 C53 1.41(2) . . ? C53 O7 1.43(2) . . ? O7 C54 1.42(2) . . ? P1 F1 1.60(1) . . ? P1 F2 1.57(1) . . ? P1 F3 1.56(1) . . ? P1 F4 1.62(1) . . ? P1 F5 1.55(1) . . ? P1 F6 1.54(1) . . ? F1 F2 2.19(2) . . ? F1 F3 2.18(1) . . ? F1 F6 2.19(2) . . ? F2 F4 2.19(2) . . ? F2 F6 2.17(1) . . ? C55 C56 1.36(3) . . ? C55 C56 1.36(3) . 2_765 ? C56 C57 1.43(4) . . ? C57 C58 1.25(4) . . ? C57 C58 1.25(4) . 2_765 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 CU1 N1 140.3(5) . . 2_775 ? N1 CU1 N2 80.9(4) . . . ? N1 CU1 N2 112.9(4) . . 2_775 ? N1 CU1 N2 112.9(4) . 2_775 . ? N1 CU1 N2 80.9(4) . 2_775 2_775 ? N2 CU1 N2 140.1(5) . . 2_775 ? N3 CU2 N3 141.5(5) . . 2_775 ? N3 CU2 N4 81.9(3) . . . ? N3 CU2 N4 112.5(3) . . 2_775 ? N3 CU2 N4 112.5(3) . 2_775 . ? N3 CU2 N4 81.9(3) . 2_775 2_775 ? N4 CU2 N4 137.0(5) . . 2_775 ? CU1 N1 C1 110.9(8) . . . ? CU1 N1 C12 130.7(7) . . . ? C1 N1 C12 117(1) . . . ? N1 C1 C2 117(1) . . . ? N1 C1 C9 121(1) . . . ? C2 C1 C9 120(1) . . . ? C1 C2 N2 119.6(9) . . . ? C1 C2 C6 118(1) . . . ? N2 C2 C6 121(1) . . . ? CU1 N2 C2 110.7(8) . . . ? CU1 N2 C3 128.3(8) . . . ? C2 N2 C3 120(1) . . . ? N2 C3 C4 119(1) . . . ? N2 C3 C13 117(1) . . . ? C4 C3 C13 122(1) . . . ? C3 C4 C5 121(1) . . . ? C4 C5 C6 120(1) . . . ? C2 C6 C5 116(1) . . . ? C2 C6 C7 120(1) . . . ? C5 C6 C7 122(1) . . . ? C6 C7 C8 118(1) . . . ? C7 C8 C9 122(1) . . . ? C1 C9 C8 117(1) . . . ? C1 C9 C10 117(1) . . . ? C8 C9 C10 125(1) . . . ? C9 C10 C11 121(1) . . . ? C10 C11 C12 118(1) . . . ? N1 C12 C11 122(1) . . . ? N1 C12 C20 117.0(9) . . . ? C11 C12 C20 120(1) . . . ? C3 C13 C14 122(1) . . . ? C3 C13 C18 121(1) . . . ? C14 C13 C18 116(1) . . . ? C13 C14 C15 122(1) . . . ? C14 C15 C16 119(1) . . . ? C15 C16 C17 120(1) . . . ? C15 C16 O1 124(1) . . . ? C17 C16 O1 115(1) . . . ? C16 C17 C18 121(1) . . . ? C13 C18 C17 119(1) . . . ? C16 O1 C19 114(1) . . . ? O1 C19 C54 107(1) . . 2_775 ? C12 C20 C21 123(1) . . . ? C12 C20 C25 118(1) . . . ? C21 C20 C25 118(1) . . . ? C20 C21 C22 120(1) . . . ? C21 C22 C23 120(1) . . . ? C22 C23 C24 118(1) . . . ? C23 C24 C25 118(1) . . . ? C23 C24 C26 122(1) . . . ? C25 C24 C26 118.4(9) . . . ? C20 C25 C24 123(1) . . . ? C24 C26 C27 120(1) . . . ? C24 C26 N3 118.7(9) . . . ? C27 C26 N3 120(1) . . . ? C26 C27 C28 117(1) . . . ? C27 C28 C29 121(1) . . . ? C28 C29 C30 124(1) . . . ? C28 C29 C37 115(1) . . . ? C30 C29 C37 120(1) . . . ? C29 C30 C31 122(1) . . . ? C30 C31 C32 121(1) . . . ? C31 C32 C33 124(1) . . . ? C31 C32 C36 117(1) . . . ? C33 C32 C36 117(1) . . . ? C32 C33 C34 119(1) . . . ? C33 C34 C35 120(1) . . . ? C34 C35 N4 119(1) . . . ? C34 C35 C38 122(1) . . . ? N4 C35 C38 117(1) . . . ? CU2 N3 C26 127.8(7) . . . ? CU2 N3 C37 112.0(7) . . . ? C26 N3 C37 119.3(9) . . . ? CU2 N4 C35 129.3(7) . . . ? CU2 N4 C36 111.3(8) . . . ? C35 N4 C36 118(1) . . . ? C32 C36 N4 123(1) . . . ? C32 C36 C37 120(1) . . . ? N4 C36 C37 116(1) . . . ? C29 C37 N3 124(1) . . . ? C29 C37 C36 117(1) . . . ? N3 C37 C36 118(1) . . . ? C35 C38 C39 121(1) . . . ? C35 C38 C43 122(1) . . . ? C39 C38 C43 116(1) . . . ? C38 C39 C40 122(1) . . . ? C39 C40 C41 120(1) . . . ? C40 C41 C42 120(1) . . . ? C40 C41 O2 117(1) . . . ? C42 C41 O2 122(1) . . . ? C41 C42 C43 119(1) . . . ? C38 C43 C42 121(1) . . . ? C41 O2 C44 120(1) . . . ? O2 C44 C45 109(1) . . . ? C44 C45 O3 114(1) . . . ? C45 O3 C46 110(1) . . . ? O3 C46 C47 108(1) . . . ? C46 C47 O4 112(1) . . . ? C47 O4 C48 117(1) . . . ? O4 C48 C49 110(1) . . . ? C48 C49 O5 105(2) . . . ? C49 O5 C50 106(1) . . . ? O5 C50 C51 109.9(4) . . . ? O5 C50 O6 122.5(5) . . . ? C51 C50 O6 33.78 . . . ? C50 C51 O6 113.51 . . . ? C50 O6 C51 32.71 . . . ? C50 O6 C52 113.31 . . . ? C51 O6 C52 124.92 . . . ? O6 C52 C53 119.1(8) . . . ? C52 C53 O7 107(1) . . . ? C53 O7 C54 109(1) . . . ? C19 C54 O7 106(1) . 2_775 . ? F1 P1 F2 87.6(6) . . . ? F1 P1 F3 87.2(6) . . . ? F1 P1 F4 87.4(7) . . . ? F1 P1 F5 175.9(8) . . . ? F1 P1 F6 88.4(7) . . . ? F2 P1 F3 172.9(7) . . . ? F2 P1 F4 86.9(7) . . . ? F2 P1 F5 92.4(7) . . . ? F2 P1 F6 88.7(7) . . . ? F3 P1 F4 88.0(7) . . . ? F3 P1 F5 92.4(7) . . . ? F3 P1 F6 96.1(8) . . . ? F4 P1 F5 88.6(8) . . . ? F4 P1 F6 174.0(7) . . . ? F5 P1 F6 95.7(8) . . . ? P1 F1 F2 45.7(4) . . . ? P1 F1 F3 45.8(4) . . . ? P1 F1 F6 44.7(5) . . . ? F2 F1 F3 91.4(6) . . . ? F2 F1 F6 59.5(5) . . . ? F3 F1 F6 63.8(6) . . . ? P1 F2 F1 46.7(4) . . . ? P1 F2 F4 47.4(4) . . . ? P1 F2 F6 45.1(5) . . . ? F1 F2 F4 60.8(5) . . . ? F1 F2 F6 60.1(5) . . . ? F4 F2 F6 92.4(6) . . . ? P1 F3 F1 47.0(4) . . . ? P1 F4 F2 45.7(4) . . . ? P1 F6 F1 46.9(4) . . . ? P1 F6 F2 46.3(4) . . . ? F1 F6 F2 60.4(5) . . . ? C56 C55 C56 116(2) . . 2_765 ? C55 C56 C57 121(2) . . . ? C56 C57 C58 112(3) . . . ? C57 C58 C57 135(5) . . 2_765 ?