# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xu, Hai' _publ_contact_author_email hbxu0513@yahoo.com.cn _publ_author_name 'Hai Xu' data_x _database_code_depnum_ccdc_archive 'CCDC 803484' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H40 Eu2 F36 N2 O18' _chemical_formula_weight 2088.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 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 13.951(5) _cell_length_b 18.353(5) _cell_length_c 15.516(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.683(5) _cell_angle_gamma 90.00 _cell_volume 3806(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11613 _cell_measurement_theta_min 1.7322 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.788 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5648 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _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 'RIGAKU MERCURY CCD/AFC' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 8970 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25742 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6560 _reflns_number_gt 5474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1409P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0093(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6560 _refine_ls_number_parameters 650 _refine_ls_number_restraints 255 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.2387 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.004 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 Eu1 Eu 0.93587(3) 1.02908(2) 0.09787(2) 0.0313(3) Uani 1 1 d . . . O1 O 0.7886(5) 0.9488(4) 0.0587(5) 0.0492(16) Uani 1 1 d . . . O2 O 0.9425(5) 0.9430(4) 0.2173(4) 0.0480(16) Uani 1 1 d . . . O3 O 0.8101(5) 1.0730(4) -0.0332(4) 0.0439(15) Uani 1 1 d . . . O4 O 0.8026(5) 1.0772(4) 0.1515(5) 0.0492(16) Uani 1 1 d . . . O5 O 0.9364(4) 1.1634(4) 0.0931(4) 0.0449(17) Uani 1 1 d . . . O6 O 1.0195(5) 1.0830(3) 0.2436(4) 0.0470(16) Uani 1 1 d . . . O7 O 0.9635(4) 0.9310(3) -0.0008(4) 0.0313(12) Uani 1 1 d . . . O8 O 1.1172(5) 0.9907(4) 0.1615(4) 0.0392(14) Uani 1 1 d . . . O9 O 0.1614(7) 0.9475(6) 0.3340(6) 0.082(3) Uani 1 1 d U . . C1 C 0.6886(10) 0.8945(8) -0.2765(9) 0.095(6) Uani 1 1 d . . . H1B H 0.7228 0.9405 -0.2671 0.142 Uiso 1 1 calc R . . H1C H 0.6197 0.9016 -0.2792 0.142 Uiso 1 1 calc R . . H1D H 0.6928 0.8735 -0.3320 0.142 Uiso 1 1 calc R . . C2 C 0.7370(8) 0.8436(6) -0.1995(7) 0.056(3) Uani 1 1 d . . . C3 C 0.7037(9) 0.7721(6) -0.1922(8) 0.069(3) Uani 1 1 d . . . H3A H 0.6499 0.7540 -0.2376 0.082 Uiso 1 1 calc R . . C4 C 0.7476(8) 0.7288(6) -0.1209(7) 0.053(3) Uani 1 1 d . . . H4A H 0.7270 0.6807 -0.1193 0.063 Uiso 1 1 calc R . . C5 C 0.8243(6) 0.7575(5) -0.0496(6) 0.0399(19) Uani 1 1 d . . . C6 C 0.8739(7) 0.7178(5) 0.0322(6) 0.043(2) Uani 1 1 d . . . C7 C 0.8428(7) 0.6380(5) 0.0421(6) 0.045(2) Uani 1 1 d . . . C8 C 0.7434(10) 0.6226(6) 0.0454(7) 0.061(3) Uani 1 1 d . . . H8A H 0.6959 0.6595 0.0371 0.074 Uiso 1 1 calc R . . C9 C 0.7206(11) 0.5552(8) 0.0607(8) 0.075(4) Uani 1 1 d . . . H9A H 0.6582 0.5465 0.0690 0.090 Uiso 1 1 calc R . . C10 C 0.7840(11) 0.4962(7) 0.0649(9) 0.077(4) Uani 1 1 d . . . H10A H 0.7631 0.4488 0.0706 0.093 Uiso 1 1 calc R . . C11 C 0.8769(15) 0.5104(8) 0.0606(12) 0.099(5) Uani 1 1 d . . . H11B H 0.9221 0.4725 0.0643 0.119 Uiso 1 1 calc R . . C12 C 0.9066(10) 0.5839(6) 0.0502(10) 0.071(3) Uani 1 1 d . . . H12A H 0.9718 0.5935 0.0492 0.085 Uiso 1 1 calc R . . C13 C 0.9478(8) 0.7506(6) 0.0935(6) 0.047(2) Uani 1 1 d . . . H13A H 0.9791 0.7249 0.1456 0.056 Uiso 1 1 calc R . . C14 C 0.9809(6) 0.8194(5) 0.0850(5) 0.0376(19) Uani 1 1 d . . . H14A H 1.0345 0.8375 0.1305 0.045 Uiso 1 1 calc R . . C15 C 0.9381(6) 0.8635(5) 0.0113(6) 0.0364(18) Uani 1 1 d . . . C16 C 0.8578(6) 0.8300(5) -0.0563(5) 0.0323(17) Uani 1 1 d . . . N1 N 0.8107(6) 0.8703(4) -0.1308(5) 0.0444(18) Uani 1 1 d . . . C101 C 0.6435(8) 0.8838(6) 0.0525(8) 0.078(4) Uani 1 1 d D . . F1 F 0.6243(16) 0.8911(13) -0.0355(9) 0.115(6) Uani 0.50 1 d PDU A 2 F2 F 0.5748(14) 0.9232(12) 0.0727(16) 0.117(6) Uani 0.50 1 d PDU A 2 F3 F 0.6220(15) 0.8156(7) 0.0656(16) 0.124(7) Uani 0.50 1 d PDU A 2 F1A F 0.6400(15) 0.8458(11) -0.0202(11) 0.114(6) Uani 0.50 1 d PDU A 1 F2A F 0.5838(13) 0.9397(9) 0.0224(15) 0.107(6) Uani 0.50 1 d PDU A 1 F3A F 0.5964(15) 0.8448(11) 0.0992(14) 0.117(6) Uani 0.50 1 d PDU A 1 C102 C 0.7498(8) 0.9071(6) 0.1039(9) 0.061(3) Uani 1 1 d . A . C103 C 0.7870(9) 0.8828(7) 0.1894(8) 0.061(3) Uani 1 1 d . . . H10C H 0.7481 0.8528 0.2141 0.073 Uiso 1 1 calc R A . C104 C 0.8844(9) 0.9023(5) 0.2415(7) 0.051(3) Uani 1 1 d . A . C105 C 0.9230(11) 0.8700(8) 0.3336(9) 0.075(4) Uani 1 1 d . . . F4 F 0.8578(7) 0.8364(6) 0.3646(6) 0.114(3) Uani 1 1 d . A 1 F5 F 0.9683(10) 0.9186(6) 0.3947(5) 0.128(4) Uani 1 1 d . A 1 F6 F 0.9939(7) 0.8212(6) 0.3339(6) 0.115(3) Uani 1 1 d . A 1 C106 C 0.6713(8) 1.1203(8) -0.1371(8) 0.095(5) Uani 1 1 d D . . F7 F 0.6824(18) 1.0799(14) -0.2033(11) 0.135(8) Uani 0.50 1 d PDU B 2 F8 F 0.5737(9) 1.1295(13) -0.1567(17) 0.113(7) Uani 0.50 1 d PDU B 2 F9 F 0.7031(18) 1.1858(11) -0.1545(16) 0.160(9) Uani 0.50 1 d PDU B 2 F7A F 0.6305(17) 1.0596(9) -0.1788(13) 0.133(7) Uani 0.50 1 d PDU B 1 F8A F 0.5965(14) 1.1659(12) -0.153(2) 0.140(9) Uani 0.50 1 d PDU B 1 F9A F 0.7270(14) 1.1423(15) -0.1876(13) 0.126(8) Uani 0.50 1 d PDU B 1 C107 C 0.7248(8) 1.1011(7) -0.0432(8) 0.062(3) Uani 1 1 d . B . C108 C 0.6803(9) 1.1184(7) 0.0227(7) 0.062(3) Uani 1 1 d . . . H10B H 0.6182 1.1412 0.0046 0.074 Uiso 1 1 calc R B . C109 C 0.7196(8) 1.1049(6) 0.1118(7) 0.050(2) Uani 1 1 d . B . C110 C 0.6569(10) 1.1232(8) 0.1764(8) 0.071(4) Uani 1 1 d . . . F10 F 0.5729(6) 1.1623(7) 0.1356(6) 0.120(4) Uani 1 1 d . B 1 F11 F 0.7098(7) 1.1712(8) 0.2383(6) 0.140(5) Uani 1 1 d . B 1 F12 F 0.6363(10) 1.0719(7) 0.2161(8) 0.143(5) Uani 1 1 d . B 1 C111 C 0.9054(7) 1.2863(6) 0.1111(6) 0.065(3) Uani 1 1 d DU . . F13 F 0.8159(13) 1.2859(10) 0.0517(14) 0.152(11) Uani 0.50 1 d PDU C 2 F14 F 0.9651(17) 1.3183(9) 0.0725(17) 0.119(8) Uani 0.50 1 d PDU C 2 F15 F 0.8925(16) 1.3343(7) 0.1712(10) 0.083(6) Uani 0.50 1 d PDU C 2 F13A F 0.8715(19) 1.2882(9) 0.0233(7) 0.124(9) Uani 0.50 1 d PDU C 1 F14A F 0.9843(13) 1.3314(8) 0.1278(14) 0.113(7) Uani 0.50 1 d PDU C 1 F15A F 0.8416(16) 1.3209(10) 0.1429(15) 0.118(9) Uani 0.50 1 d PDU C 1 C112 C 0.9365(7) 1.2131(5) 0.1488(6) 0.049(2) Uani 1 1 d DU C . C113 C 0.9677(9) 1.2052(6) 0.2420(7) 0.059(3) Uani 1 1 d . . . H11A H 0.9600 1.2441 0.2780 0.070 Uiso 1 1 calc R C . C114 C 1.0100(8) 1.1405(6) 0.2825(7) 0.053(3) Uani 1 1 d . C . C115 C 1.0520(8) 1.1409(5) 0.3839(8) 0.078(4) Uani 1 1 d D . . F16 F 0.9949(14) 1.1815(12) 0.4190(15) 0.101(8) Uani 0.50 1 d PDU C 2 F17 F 1.1418(12) 1.1704(14) 0.408(2) 0.161(12) Uani 0.50 1 d PDU C 2 F18 F 1.0595(19) 1.0762(8) 0.4218(18) 0.100(9) Uani 0.50 1 d PDU C 2 F16A F 1.0370(17) 1.1974(13) 0.4305(17) 0.115(10) Uani 0.50 1 d PDU C 1 F17A F 1.1501(10) 1.1298(14) 0.4085(17) 0.115(8) Uani 0.50 1 d PDU C 1 F18A F 1.013(2) 1.0835(12) 0.413(2) 0.117(11) Uani 0.50 1 d PDU C 1 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 Eu1 0.0305(4) 0.0299(4) 0.0329(3) 0.00218(15) 0.0079(2) 0.00005(15) O1 0.043(4) 0.047(4) 0.062(4) -0.005(3) 0.021(3) -0.013(3) O2 0.052(4) 0.049(4) 0.047(4) 0.016(3) 0.021(3) 0.011(3) O3 0.036(3) 0.048(4) 0.049(3) 0.009(3) 0.013(3) 0.016(3) O4 0.042(4) 0.051(4) 0.058(4) 0.002(3) 0.020(3) 0.009(3) O5 0.052(4) 0.037(4) 0.050(4) -0.002(3) 0.023(3) -0.001(3) O6 0.053(4) 0.035(3) 0.046(3) -0.004(3) 0.002(3) 0.009(3) O7 0.028(3) 0.025(3) 0.036(3) 0.002(2) 0.003(2) -0.005(2) O8 0.036(3) 0.046(3) 0.034(3) 0.006(3) 0.007(3) 0.004(3) O9 0.091(7) 0.089(6) 0.062(5) 0.020(5) 0.015(5) 0.028(6) C1 0.083(9) 0.090(10) 0.076(8) 0.028(7) -0.034(7) -0.051(8) C2 0.050(6) 0.050(6) 0.055(6) 0.004(5) -0.007(5) -0.016(5) C3 0.059(7) 0.057(7) 0.070(7) 0.001(6) -0.014(6) -0.018(6) C4 0.061(6) 0.041(5) 0.049(5) -0.003(4) 0.004(5) -0.016(5) C5 0.036(5) 0.035(5) 0.047(5) 0.001(4) 0.010(4) 0.000(4) C6 0.049(5) 0.024(4) 0.056(6) 0.007(4) 0.014(4) 0.008(4) C7 0.046(5) 0.038(5) 0.045(5) 0.002(4) 0.004(4) -0.010(4) C8 0.076(8) 0.050(6) 0.062(7) 0.003(5) 0.027(6) -0.011(6) C9 0.080(9) 0.074(9) 0.075(8) 0.011(7) 0.027(7) -0.041(8) C10 0.075(9) 0.048(7) 0.094(10) 0.023(7) -0.001(7) -0.017(7) C11 0.122(15) 0.054(8) 0.118(13) 0.016(9) 0.027(11) 0.015(9) C12 0.070(8) 0.028(5) 0.117(11) 0.001(6) 0.030(7) -0.004(5) C13 0.066(7) 0.034(5) 0.041(5) 0.002(4) 0.015(5) 0.001(5) C14 0.034(4) 0.041(5) 0.035(4) -0.001(4) 0.003(3) -0.005(4) C15 0.037(4) 0.033(4) 0.041(4) -0.007(4) 0.013(4) -0.011(4) C16 0.030(4) 0.034(4) 0.030(4) -0.001(3) 0.005(3) -0.004(3) N1 0.038(4) 0.037(4) 0.051(4) 0.009(4) 0.000(3) 0.002(3) C101 0.062(8) 0.080(9) 0.101(10) -0.019(8) 0.035(7) -0.036(7) F1 0.061(10) 0.135(15) 0.140(13) -0.003(11) 0.013(9) -0.047(11) F2 0.056(8) 0.132(13) 0.169(16) -0.025(12) 0.042(10) 0.012(10) F3 0.077(11) 0.105(12) 0.178(15) -0.009(11) 0.019(11) -0.047(10) F1A 0.060(9) 0.123(14) 0.151(13) -0.051(11) 0.016(9) -0.026(11) F2A 0.052(8) 0.103(11) 0.162(16) -0.004(11) 0.023(10) -0.001(9) F3A 0.066(9) 0.135(14) 0.164(14) -0.006(12) 0.056(9) -0.038(10) C102 0.043(6) 0.057(7) 0.091(8) -0.016(6) 0.032(6) -0.013(5) C103 0.060(7) 0.068(7) 0.063(7) 0.016(6) 0.030(5) -0.004(6) C104 0.066(7) 0.043(6) 0.056(6) -0.003(4) 0.036(5) -0.013(5) C105 0.084(9) 0.078(9) 0.072(8) 0.028(7) 0.038(7) 0.005(8) F4 0.108(7) 0.148(9) 0.095(6) 0.050(6) 0.042(5) -0.030(6) F5 0.194(12) 0.135(9) 0.055(5) 0.007(5) 0.034(6) -0.038(8) F6 0.113(7) 0.132(8) 0.107(6) 0.064(6) 0.044(5) 0.058(6) C106 0.069(9) 0.143(16) 0.065(9) 0.020(10) 0.009(7) 0.039(10) F7 0.118(16) 0.219(19) 0.061(9) 0.006(13) 0.015(10) 0.097(14) F8 0.062(9) 0.206(19) 0.074(9) 0.052(14) 0.023(8) 0.059(11) F9 0.133(15) 0.25(2) 0.099(13) 0.090(14) 0.039(11) 0.020(15) F7A 0.109(15) 0.209(18) 0.066(10) 0.020(12) 0.000(10) 0.040(14) F8A 0.104(13) 0.22(2) 0.094(11) 0.073(15) 0.023(11) 0.087(13) F9A 0.101(12) 0.22(2) 0.068(11) 0.070(13) 0.046(9) 0.033(14) C107 0.043(6) 0.080(8) 0.065(7) 0.024(6) 0.018(5) 0.025(6) C108 0.057(7) 0.077(8) 0.057(6) 0.009(6) 0.025(5) 0.031(6) C109 0.055(6) 0.042(5) 0.059(6) 0.001(5) 0.028(5) 0.007(5) C110 0.061(7) 0.089(10) 0.068(7) -0.001(7) 0.027(6) 0.032(7) F10 0.071(5) 0.203(11) 0.087(6) -0.012(6) 0.025(4) 0.060(6) F11 0.083(6) 0.241(14) 0.099(6) -0.083(8) 0.033(5) -0.012(7) F12 0.187(12) 0.135(9) 0.163(10) 0.027(8) 0.141(9) 0.022(9) C111 0.065(7) 0.058(7) 0.071(7) -0.004(6) 0.018(6) 0.004(6) F13 0.18(2) 0.105(15) 0.136(18) 0.019(14) -0.020(17) 0.048(16) F14 0.183(19) 0.070(12) 0.154(18) 0.057(13) 0.126(15) 0.041(13) F15 0.126(16) 0.041(8) 0.085(10) 0.007(7) 0.034(11) 0.047(9) F13A 0.18(2) 0.064(11) 0.107(14) 0.022(10) 0.016(15) 0.057(14) F14A 0.165(16) 0.067(11) 0.106(14) 0.015(10) 0.039(14) -0.046(11) F15A 0.137(19) 0.095(15) 0.150(19) 0.042(13) 0.083(16) 0.057(13) C112 0.051(6) 0.040(5) 0.059(6) -0.004(5) 0.020(5) -0.006(4) C113 0.070(7) 0.045(6) 0.056(6) -0.008(5) 0.011(5) 0.012(5) C114 0.053(6) 0.045(6) 0.056(6) -0.012(5) 0.006(5) -0.004(5) C115 0.095(11) 0.077(10) 0.055(7) -0.023(7) 0.009(7) 0.003(8) F16 0.092(15) 0.146(19) 0.043(10) -0.035(10) -0.017(11) 0.041(14) F17 0.135(18) 0.20(3) 0.106(15) -0.04(2) -0.032(15) -0.048(17) F18 0.16(2) 0.073(12) 0.045(9) -0.001(8) -0.003(13) 0.047(12) F16A 0.134(19) 0.115(14) 0.055(9) -0.059(9) -0.040(13) 0.050(14) F17A 0.110(15) 0.133(18) 0.072(11) -0.025(14) -0.023(11) 0.024(13) F18A 0.16(2) 0.122(19) 0.053(11) 0.015(12) 0.014(16) -0.052(17) _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 Eu1 O3 2.411(6) . ? Eu1 O4 2.412(6) . ? Eu1 O2 2.417(6) . ? Eu1 O6 2.436(6) . ? Eu1 O7 2.447(6) 3_775 ? Eu1 O1 2.459(7) . ? Eu1 O7 2.464(6) . ? Eu1 O5 2.467(7) . ? Eu1 O8 2.538(6) . ? Eu1 Eu1 4.0849(12) 3_775 ? O1 C102 1.260(13) . ? O2 C104 1.237(12) . ? O3 C107 1.265(12) . ? O4 C109 1.252(12) . ? O5 C112 1.256(11) . ? O6 C114 1.242(12) . ? O7 C15 1.317(10) . ? O7 Eu1 2.447(6) 3_775 ? C1 C2 1.514(15) . ? C2 N1 1.342(12) . ? C2 C3 1.408(15) . ? C3 C4 1.357(15) . ? C4 C5 1.403(13) . ? C5 C16 1.423(12) . ? C5 C6 1.456(12) . ? C6 C13 1.329(14) . ? C6 C7 1.548(12) . ? C7 C12 1.315(15) . ? C7 C8 1.430(16) . ? C8 C9 1.316(16) . ? C9 C10 1.39(2) . ? C10 C11 1.34(2) . ? C11 C12 1.434(18) . ? C13 C14 1.364(14) . ? C14 C15 1.388(12) . ? C15 C16 1.435(11) . ? C16 N1 1.372(11) . ? C101 F2 1.308(9) . ? C101 F1A 1.316(9) . ? C101 F3 1.317(9) . ? C101 F2A 1.319(9) . ? C101 F3A 1.320(9) . ? C101 F1 1.321(9) . ? C101 C102 1.529(15) . ? C102 C103 1.353(17) . ? C103 C104 1.413(16) . ? C104 C105 1.497(16) . ? C105 F4 1.300(14) . ? C105 F5 1.323(17) . ? C105 F6 1.334(15) . ? C106 F8A 1.305(10) . ? C106 F7 1.311(9) . ? C106 F9A 1.315(9) . ? C106 F8 1.319(10) . ? C106 F7A 1.332(10) . ? C106 F9 1.335(10) . ? C106 C107 1.476(15) . ? C107 C108 1.377(15) . ? C108 C109 1.356(15) . ? C109 C110 1.544(14) . ? C110 F12 1.205(17) . ? C110 F11 1.356(17) . ? C110 F10 1.364(14) . ? C111 F14 1.297(9) . ? C111 F15A 1.301(9) . ? C111 F13A 1.308(9) . ? C111 F13 1.323(9) . ? C111 F15 1.332(9) . ? C111 F14A 1.341(9) . ? C111 C112 1.480(14) . ? C112 C113 1.393(14) . ? C113 C114 1.394(14) . ? C114 C115 1.514(15) . ? C115 F16A 1.314(10) . ? C115 F18 1.316(10) . ? C115 F16 1.316(10) . ? C115 F17 1.316(10) . ? C115 F18A 1.322(10) . ? C115 F17A 1.327(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 O3 Eu1 O4 73.9(2) . . ? O3 Eu1 O2 136.3(2) . . ? O4 Eu1 O2 80.7(2) . . ? O3 Eu1 O6 133.3(2) . . ? O4 Eu1 O6 75.1(2) . . ? O2 Eu1 O6 69.6(2) . . ? O3 Eu1 O7 77.8(2) . 3_775 ? O4 Eu1 O7 137.6(2) . 3_775 ? O2 Eu1 O7 139.9(2) . 3_775 ? O6 Eu1 O7 104.1(2) . 3_775 ? O3 Eu1 O1 68.8(2) . . ? O4 Eu1 O1 68.4(2) . . ? O2 Eu1 O1 69.1(2) . . ? O6 Eu1 O1 128.0(2) . . ? O7 Eu1 O1 127.8(2) 3_775 . ? O3 Eu1 O7 85.8(2) . . ? O4 Eu1 O7 139.1(2) . . ? O2 Eu1 O7 91.2(2) . . ? O6 Eu1 O7 139.0(2) . . ? O7 Eu1 O7 67.4(2) 3_775 . ? O1 Eu1 O7 71.2(2) . . ? O3 Eu1 O5 69.4(2) . . ? O4 Eu1 O5 69.7(2) . . ? O2 Eu1 O5 132.6(2) . . ? O6 Eu1 O5 67.5(2) . . ? O7 Eu1 O5 71.06(19) 3_775 . ? O1 Eu1 O5 127.0(2) . . ? O7 Eu1 O5 135.16(18) . . ? O3 Eu1 O8 145.5(2) . . ? O4 Eu1 O8 138.5(2) . . ? O2 Eu1 O8 72.9(2) . . ? O6 Eu1 O8 66.0(2) . . ? O7 Eu1 O8 68.82(19) 3_775 . ? O1 Eu1 O8 126.8(2) . . ? O7 Eu1 O8 73.87(19) . . ? O5 Eu1 O8 106.2(2) . . ? O3 Eu1 Eu1 80.11(15) . 3_775 ? O4 Eu1 Eu1 153.87(16) . 3_775 ? O2 Eu1 Eu1 118.11(17) . 3_775 ? O6 Eu1 Eu1 126.92(17) . 3_775 ? O7 Eu1 Eu1 33.84(13) 3_775 3_775 ? O1 Eu1 Eu1 99.96(17) . 3_775 ? O7 Eu1 Eu1 33.59(13) . 3_775 ? O5 Eu1 Eu1 103.48(13) . 3_775 ? O8 Eu1 Eu1 67.41(14) . 3_775 ? C102 O1 Eu1 133.5(7) . . ? C104 O2 Eu1 138.0(7) . . ? C107 O3 Eu1 132.2(7) . . ? C109 O4 Eu1 132.4(6) . . ? C112 O5 Eu1 134.7(6) . . ? C114 O6 Eu1 134.9(6) . . ? C15 O7 Eu1 126.5(5) . 3_775 ? C15 O7 Eu1 120.2(5) . . ? Eu1 O7 Eu1 112.6(2) 3_775 . ? N1 C2 C3 118.2(9) . . ? N1 C2 C1 117.9(9) . . ? C3 C2 C1 123.7(9) . . ? C4 C3 C2 122.0(10) . . ? C3 C4 C5 119.1(9) . . ? C4 C5 C16 119.1(8) . . ? C4 C5 C6 124.3(9) . . ? C16 C5 C6 116.6(8) . . ? C13 C6 C5 118.3(8) . . ? C13 C6 C7 122.7(8) . . ? C5 C6 C7 118.9(8) . . ? C12 C7 C8 119.0(10) . . ? C12 C7 C6 121.4(9) . . ? C8 C7 C6 119.5(9) . . ? C9 C8 C7 118.6(12) . . ? C8 C9 C10 124.0(13) . . ? C11 C10 C9 117.2(12) . . ? C10 C11 C12 120.2(15) . . ? C7 C12 C11 120.7(13) . . ? C6 C13 C14 124.4(9) . . ? C13 C14 C15 122.8(8) . . ? O7 C15 C14 126.6(7) . . ? O7 C15 C16 119.0(7) . . ? C14 C15 C16 114.4(7) . . ? N1 C16 C5 118.5(7) . . ? N1 C16 C15 118.0(8) . . ? C5 C16 C15 123.5(7) . . ? C2 N1 C16 123.0(8) . . ? F2 C101 F1A 130.4(18) . . ? F2 C101 F3 105.8(11) . . ? F1A C101 F3 71.0(12) . . ? F2 C101 F2A 39.1(11) . . ? F1A C101 F2A 104.1(12) . . ? F3 C101 F2A 130.2(16) . . ? F2 C101 F3A 69.8(12) . . ? F1A C101 F3A 106.4(11) . . ? F3 C101 F3A 39.5(11) . . ? F2A C101 F3A 104.7(11) . . ? F2 C101 F1 104.3(12) . . ? F1A C101 F1 38.7(11) . . ? F3 C101 F1 105.6(11) . . ? F2A C101 F1 68.6(12) . . ? F3A C101 F1 129.6(17) . . ? F2 C101 C102 112.9(13) . . ? F1A C101 C102 112.8(12) . . ? F3 C101 C102 114.5(13) . . ? F2A C101 C102 112.7(12) . . ? F3A C101 C102 115.2(14) . . ? F1 C101 C102 112.9(12) . . ? O1 C102 C103 129.8(10) . . ? O1 C102 C101 112.8(11) . . ? C103 C102 C101 117.4(10) . . ? C102 C103 C104 120.9(10) . . ? O2 C104 C103 125.8(10) . . ? O2 C104 C105 116.2(10) . . ? C103 C104 C105 118.0(10) . . ? F4 C105 F5 107.2(12) . . ? F4 C105 F6 106.1(11) . . ? F5 C105 F6 104.4(13) . . ? F4 C105 C104 116.3(12) . . ? F5 C105 C104 112.6(11) . . ? F6 C105 C104 109.4(11) . . ? F8A C106 F7 119(2) . . ? F8A C106 F9A 105.6(12) . . ? F7 C106 F9A 59.0(12) . . ? F8A C106 F8 32.5(15) . . ? F7 C106 F8 103.8(12) . . ? F9A C106 F8 124.9(19) . . ? F8A C106 F7A 103.7(13) . . ? F7 C106 F7A 43.6(12) . . ? F9A C106 F7A 102.2(12) . . ? F8 C106 F7A 74.1(13) . . ? F8A C106 F9 71.2(14) . . ? F7 C106 F9 103.4(12) . . ? F9A C106 F9 46.9(12) . . ? F8 C106 F9 102.7(12) . . ? F7A C106 F9 140.9(16) . . ? F8A C106 C107 119.3(16) . . ? F7 C106 C107 119.8(13) . . ? F9A C106 C107 116.3(12) . . ? F8 C106 C107 116.9(15) . . ? F7A C106 C107 107.7(14) . . ? F9 C106 C107 108.2(14) . . ? O3 C107 C108 127.7(10) . . ? O3 C107 C106 114.2(9) . . ? C108 C107 C106 118.1(9) . . ? C109 C108 C107 125.4(10) . . ? O4 C109 C108 128.4(9) . . ? O4 C109 C110 112.6(9) . . ? C108 C109 C110 118.9(10) . . ? F12 C110 F11 107.9(13) . . ? F12 C110 F10 110.4(13) . . ? F11 C110 F10 102.0(11) . . ? F12 C110 C109 115.2(11) . . ? F11 C110 C109 107.8(11) . . ? F10 C110 C109 112.6(10) . . ? F14 C111 F15A 123.6(15) . . ? F14 C111 F13A 66.1(13) . . ? F15A C111 F13A 107.4(11) . . ? F14 C111 F13 106.5(12) . . ? F15A C111 F13 69.8(13) . . ? F13A C111 F13 44.5(13) . . ? F14 C111 F15 104.9(11) . . ? F15A C111 F15 33.5(12) . . ? F13A C111 F15 129.0(14) . . ? F13 C111 F15 101.6(11) . . ? F14 C111 F14A 37.8(11) . . ? F15A C111 F14A 103.8(11) . . ? F13A C111 F14A 102.5(11) . . ? F13 C111 F14A 134.1(15) . . ? F15 C111 F14A 74.0(12) . . ? F14 C111 C112 116.1(10) . . ? F15A C111 C112 116.6(10) . . ? F13A C111 C112 114.4(9) . . ? F13 C111 C112 112.4(10) . . ? F15 C111 C112 114.1(9) . . ? F14A C111 C112 110.7(10) . . ? O5 C112 C113 125.4(10) . . ? O5 C112 C111 116.4(8) . . ? C113 C112 C111 118.2(8) . . ? C112 C113 C114 121.4(10) . . ? O6 C114 C113 126.6(10) . . ? O6 C114 C115 116.5(9) . . ? C113 C114 C115 116.8(9) . . ? F16A C115 F18 118(3) . . ? F16A C115 F16 27.9(15) . . ? F18 C115 F16 107.8(12) . . ? F16A C115 F17 79.2(16) . . ? F18 C115 F17 107.4(13) . . ? F16 C115 F17 107.0(12) . . ? F16A C115 F18A 107.1(13) . . ? F18 C115 F18A 27.9(17) . . ? F16 C115 F18A 87(2) . . ? F17 C115 F18A 133(2) . . ? F16A C115 F17A 106.2(11) . . ? F18 C115 F17A 77.8(16) . . ? F16 C115 F17A 131.7(16) . . ? F17 C115 F17A 33.1(14) . . ? F18A C115 F17A 105.7(12) . . ? F16A C115 C114 120.1(15) . . ? F18 C115 C114 114.6(15) . . ? F16 C115 C114 109.4(13) . . ? F17 C115 C114 110.3(17) . . ? F18A C115 C114 105.9(15) . . ? F17A C115 C114 111.0(14) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.500 _refine_diff_density_min -2.398 _refine_diff_density_rms 0.431 # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 803485' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H50 F36 N4 Nd2 O18' _chemical_formula_weight 2159.58 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' 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.259(7) _cell_length_b 14.464(3) _cell_length_c 23.046(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.126(5) _cell_angle_gamma 90.00 _cell_volume 8771(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10085 _cell_measurement_theta_min 3.2135 _cell_measurement_theta_max 27.4797 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4248 _exptl_absorpt_coefficient_mu 1.309 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5158 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _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 'SATURN70 CCD/AFC' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 9859 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24726 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7207 _reflns_number_gt 6286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1013P)^2^+31.0498P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7207 _refine_ls_number_parameters 734 _refine_ls_number_restraints 450 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.180 _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 Nd1 Nd 0.195518(11) 0.148243(18) 0.483028(11) 0.0470(2) Uani 1 1 d . . . F1 F 0.1653(8) 0.0197(7) 0.2692(7) 0.150(6) Uani 0.50 1 d PDU A 1 F2 F 0.1993(6) 0.1497(13) 0.2601(9) 0.147(6) Uani 0.50 1 d PDU A 1 F3 F 0.1213(6) 0.1256(14) 0.2201(5) 0.158(6) Uani 0.50 1 d PDU A 1 F1' F 0.1370(8) 0.0338(11) 0.2445(8) 0.167(6) Uani 0.50 1 d PDU A 2 F2' F 0.2083(5) 0.0960(14) 0.2748(8) 0.151(6) Uani 0.50 1 d PDU A 2 F3' F 0.1462(9) 0.1747(11) 0.2267(7) 0.159(6) Uani 0.50 1 d PDU A 2 F4 F -0.0034(5) 0.1553(14) 0.3331(8) 0.164(7) Uani 0.50 1 d PDU A 1 F5 F 0.0176(7) 0.2958(15) 0.3362(12) 0.198(9) Uani 0.50 1 d PDU A 1 F6 F 0.0112(6) 0.2242(16) 0.4165(6) 0.139(7) Uani 0.50 1 d PDU A 1 F4' F -0.0021(8) 0.2188(19) 0.3140(6) 0.173(8) Uani 0.50 1 d PDU A 2 F5' F 0.0269(6) 0.3068(11) 0.3894(10) 0.155(6) Uani 0.50 1 d PDU A 2 F6' F 0.0079(9) 0.1711(16) 0.4054(10) 0.172(8) Uani 0.50 1 d PDU A 2 F7 F 0.3297(8) 0.0099(14) 0.3881(7) 0.135(6) Uani 0.50 1 d PDU B 1 F8 F 0.3327(13) -0.1216(15) 0.4215(11) 0.152(8) Uani 0.50 1 d PDU B 1 F9 F 0.3591(6) -0.0135(13) 0.4774(8) 0.139(6) Uani 0.50 1 d PDU B 1 F7' F 0.3213(13) -0.1203(16) 0.4009(8) 0.120(6) Uani 0.50 1 d PDU C 2 F8' F 0.3483(7) -0.0814(15) 0.4938(8) 0.160(7) Uani 0.50 1 d PDU C 2 F9' F 0.3481(7) 0.0156(11) 0.4241(10) 0.128(5) Uani 0.50 1 d PDU C 2 F10 F 0.0977(6) -0.1325(12) 0.4033(11) 0.170(6) Uani 0.50 1 d PDU D 1 F11 F 0.1449(9) -0.1774(16) 0.3481(7) 0.194(7) Uani 0.50 1 d PDU D 1 F12 F 0.1576(8) -0.2250(10) 0.4376(9) 0.174(6) Uani 0.50 1 d PDU D 1 F10' F 0.1049(7) -0.1160(12) 0.3613(9) 0.178(7) Uani 0.50 1 d PDU D 2 F11' F 0.1617(8) -0.2162(12) 0.3721(9) 0.177(6) Uani 0.50 1 d PDU D 2 F12' F 0.1274(9) -0.1931(15) 0.4431(8) 0.189(7) Uani 0.50 1 d PDU D 2 F13 F 0.2520(12) -0.1640(14) 0.5677(8) 0.190(9) Uani 0.50 1 d PDU E 1 F14 F 0.2860(8) -0.0971(16) 0.6512(12) 0.190(11) Uani 0.50 1 d PDU E 1 F15 F 0.2186(8) -0.1754(11) 0.6377(9) 0.168(8) Uani 0.50 1 d PDU E 1 F13' F 0.2875(7) -0.1128(13) 0.5978(10) 0.162(7) Uani 0.50 1 d PDU E 2 F14' F 0.2572(8) -0.0962(15) 0.6708(6) 0.153(7) Uani 0.50 1 d PDU E 2 F15' F 0.2251(9) -0.1961(9) 0.6038(13) 0.187(9) Uani 0.50 1 d PDU E 2 F16 F 0.0780(18) 0.052(3) 0.6407(9) 0.296(15) Uani 0.50 1 d PDU E 1 F17 F 0.0542(13) -0.0504(14) 0.5717(16) 0.293(17) Uani 0.50 1 d PDU E 1 F18 F 0.0434(10) 0.093(2) 0.5508(15) 0.183(12) Uani 0.50 1 d PDU E 1 F16' F 0.081(2) 0.092(2) 0.6292(12) 0.339(19) Uani 0.50 1 d PDU E 2 F17' F 0.0641(15) -0.0488(15) 0.6030(14) 0.281(15) Uani 0.50 1 d PDU E 2 F18' F 0.0365(12) 0.060(3) 0.5400(18) 0.198(14) Uani 0.50 1 d PDU E 2 O1 O 0.1845(2) 0.1398(3) 0.3720(2) 0.0661(12) Uani 1 1 d . . . O2 O 0.10902(18) 0.1954(4) 0.4279(2) 0.0715(12) Uani 1 1 d . . . O3 O 0.26572(17) 0.0612(3) 0.45853(19) 0.0603(10) Uani 1 1 d . . . O4 O 0.1621(2) -0.0019(3) 0.4419(2) 0.0768(13) Uani 1 1 d . . . O5 O 0.2277(2) 0.0249(3) 0.5598(2) 0.0771(13) Uani 1 1 d . . . O6 O 0.1336(2) 0.1049(4) 0.5400(2) 0.0854(15) Uani 1 1 d . . . O7 O 0.22548(14) 0.2937(2) 0.44831(15) 0.0464(8) Uani 1 1 d . . . O8 O 0.17669(16) 0.2806(3) 0.55075(18) 0.0600(10) Uani 1 1 d . . . O9 O 0.0782(3) 0.3046(7) 0.5363(4) 0.133(3) Uani 1 1 d U . . N1 N 0.2545(2) 0.3041(4) 0.3439(2) 0.0582(12) Uani 1 1 d . . . N2 N 0.0073(4) 0.6299(8) 0.1021(4) 0.181(3) Uani 1 1 d DU . . C1 C 0.3221(4) 0.2580(9) 0.2989(4) 0.106(3) Uani 1 1 d . . . H1B H 0.3339 0.2289 0.3375 0.159 Uiso 1 1 calc R . . H1C H 0.3472 0.3011 0.2932 0.159 Uiso 1 1 calc R . . H1D H 0.3164 0.2117 0.2680 0.159 Uiso 1 1 calc R . . C2 C 0.2737(3) 0.3079(6) 0.2959(3) 0.0743(18) Uani 1 1 d . . . C3 C 0.2469(4) 0.3568(7) 0.2465(4) 0.087(3) Uani 1 1 d . . . H3A H 0.2594 0.3605 0.2127 0.105 Uiso 1 1 calc R . . C4 C 0.2018(3) 0.4004(6) 0.2464(3) 0.083(2) Uani 1 1 d . . . H4A H 0.1847 0.4338 0.2127 0.100 Uiso 1 1 calc R . . C5 C 0.1812(3) 0.3954(5) 0.2962(3) 0.0621(15) Uani 1 1 d . . . C6 C 0.1352(3) 0.4381(5) 0.2997(3) 0.0702(17) Uani 1 1 d . . . C7 C 0.1022(3) 0.4870(8) 0.2476(4) 0.126(3) Uani 1 1 d DU . . C8 C 0.0829(4) 0.4450(10) 0.1924(4) 0.144(3) Uani 1 1 d DU . . H8B H 0.0918 0.3839 0.1878 0.173 Uiso 1 1 calc R . . C9 C 0.0508(4) 0.4892(10) 0.1433(5) 0.156(3) Uani 1 1 d DU . . H9A H 0.0377 0.4585 0.1071 0.188 Uiso 1 1 calc R . . C10 C 0.0392(4) 0.5815(8) 0.1508(5) 0.157(3) Uani 1 1 d DU . . C11 C 0.0584(4) 0.6277(10) 0.2054(5) 0.154(3) Uani 1 1 d DU . . H11A H 0.0501 0.6892 0.2096 0.184 Uiso 1 1 calc R . . C12 C 0.0904(4) 0.5798(9) 0.2537(5) 0.139(3) Uani 1 1 d DU . . H12A H 0.1038 0.6100 0.2900 0.167 Uiso 1 1 calc R . . C13 C 0.1221(3) 0.4315(5) 0.3532(3) 0.0703(17) Uani 1 1 d . . . H13A H 0.0922 0.4596 0.3563 0.084 Uiso 1 1 calc R . . C14 C 0.1515(3) 0.3844(5) 0.4032(3) 0.0602(14) Uani 1 1 d . . . H14A H 0.1408 0.3829 0.4383 0.072 Uiso 1 1 calc R . . C15 C 0.1959(2) 0.3403(4) 0.4020(3) 0.0489(12) Uani 1 1 d . . . C16 C 0.2104(2) 0.3454(4) 0.3471(3) 0.0504(13) Uani 1 1 d . . . C17 C -0.0223(6) 0.5756(12) 0.0518(6) 0.238(6) Uani 1 1 d DU . . H17A H -0.0048 0.5188 0.0490 0.357 Uiso 1 1 calc R . . H17B H -0.0266 0.6100 0.0153 0.357 Uiso 1 1 calc R . . H17C H -0.0550 0.5621 0.0581 0.357 Uiso 1 1 calc R . . C18 C -0.0129(7) 0.7181(10) 0.1141(7) 0.228(5) Uani 1 1 d DU . . H18A H 0.0108 0.7476 0.1472 0.342 Uiso 1 1 calc R . . H18B H -0.0446 0.7088 0.1240 0.342 Uiso 1 1 calc R . . H18C H -0.0182 0.7566 0.0791 0.342 Uiso 1 1 calc R . . C101 C 0.1589(4) 0.1102(6) 0.2687(4) 0.113(3) Uani 1 1 d D . . C102 C 0.1469(4) 0.1392(5) 0.3276(3) 0.077(2) Uani 1 1 d . A . C103 C 0.0980(4) 0.1615(7) 0.3248(4) 0.097(3) Uani 1 1 d . . . H10A H 0.0739 0.1585 0.2879 0.117 Uiso 1 1 calc R A . C104 C 0.0827(3) 0.1885(7) 0.3752(4) 0.084(2) Uani 1 1 d . A . C105 C 0.0268(4) 0.2194(9) 0.3680(4) 0.131(4) Uani 1 1 d D . . C106 C 0.3202(9) -0.0374(13) 0.4332(8) 0.091(3) Uani 0.50 1 d PD B 1 C10A C 0.3233(10) -0.0539(14) 0.4403(7) 0.091(3) Uani 0.50 1 d PD C 2 C107 C 0.2694(3) -0.0204(5) 0.4408(3) 0.0743(18) Uani 1 1 d . . . C108 C 0.2322(4) -0.0865(5) 0.4243(4) 0.089(2) Uani 1 1 d . B . H10B H 0.2410 -0.1436 0.4114 0.107 Uiso 1 1 calc R . . C109 C 0.1825(4) -0.0725(6) 0.4258(4) 0.094(3) Uani 1 1 d . . . C110 C 0.1446(5) -0.1507(6) 0.4020(5) 0.133(6) Uani 1 1 d D D . C111 C 0.2434(5) -0.1139(6) 0.6125(4) 0.119(4) Uani 1 1 d D . . C112 C 0.2094(5) -0.0360(6) 0.5846(4) 0.101(3) Uani 1 1 d . E . C113 C 0.1590(5) -0.0367(8) 0.5908(5) 0.128(4) Uani 1 1 d . . . H11B H 0.1482 -0.0857 0.6105 0.154 Uiso 1 1 calc R E . C114 C 0.1254(5) 0.0355(9) 0.5675(5) 0.117(4) Uani 1 1 d . E . C115 C 0.0747(6) 0.0330(10) 0.5835(7) 0.214(12) Uani 1 1 d 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 Nd1 0.0573(3) 0.0433(3) 0.0389(3) 0.00002(9) 0.00978(15) -0.00460(10) F1 0.209(15) 0.133(10) 0.108(10) -0.060(8) 0.039(10) 0.013(9) F2 0.208(13) 0.170(14) 0.085(9) -0.035(9) 0.079(9) -0.066(11) F3 0.217(15) 0.197(14) 0.046(6) -0.032(8) 0.007(8) 0.005(12) F1' 0.226(16) 0.162(11) 0.105(11) -0.078(9) 0.031(10) -0.058(11) F2' 0.199(12) 0.183(14) 0.084(9) -0.048(10) 0.062(8) -0.013(11) F3' 0.243(16) 0.174(13) 0.066(8) 0.005(9) 0.049(9) -0.005(12) F4 0.064(7) 0.25(2) 0.158(14) 0.008(13) -0.017(8) -0.041(10) F5 0.102(11) 0.218(19) 0.26(2) 0.072(19) 0.015(14) 0.052(12) F6 0.080(8) 0.204(18) 0.127(10) -0.041(11) 0.014(7) 0.022(11) F4' 0.121(11) 0.226(16) 0.129(10) -0.003(11) -0.043(9) 0.043(12) F5' 0.093(8) 0.184(13) 0.183(13) -0.009(12) 0.028(10) 0.026(9) F6' 0.109(10) 0.220(17) 0.192(15) 0.008(13) 0.051(11) -0.020(12) F7 0.142(14) 0.151(11) 0.127(12) -0.041(11) 0.061(11) 0.003(10) F8 0.136(16) 0.116(9) 0.20(2) -0.085(12) 0.029(17) 0.040(9) F9 0.094(7) 0.180(13) 0.127(11) -0.080(11) 0.003(8) 0.037(10) F7' 0.136(16) 0.125(9) 0.094(9) -0.070(8) 0.023(10) 0.010(9) F8' 0.108(10) 0.222(18) 0.133(11) 0.000(13) 0.001(8) 0.062(13) F9' 0.105(10) 0.120(8) 0.178(14) -0.036(12) 0.072(11) -0.004(8) F10 0.147(10) 0.112(9) 0.241(15) -0.038(11) 0.032(11) -0.059(8) F11 0.200(13) 0.142(12) 0.200(13) -0.089(11) -0.020(11) -0.050(10) F12 0.189(13) 0.083(8) 0.249(12) -0.005(9) 0.054(12) -0.053(8) F10' 0.157(10) 0.136(10) 0.206(13) -0.052(10) -0.014(10) -0.049(9) F11' 0.194(12) 0.097(9) 0.208(12) -0.061(9) -0.003(10) -0.029(8) F12' 0.173(12) 0.140(10) 0.248(12) -0.005(10) 0.046(10) -0.083(9) F13 0.28(2) 0.108(13) 0.19(2) 0.046(12) 0.080(18) 0.068(14) F14 0.175(18) 0.123(12) 0.21(2) 0.042(17) -0.057(17) -0.022(14) F15 0.30(2) 0.065(9) 0.144(14) 0.045(9) 0.068(14) -0.001(12) F13' 0.192(17) 0.106(12) 0.185(18) 0.070(13) 0.045(15) 0.049(11) F14' 0.180(17) 0.137(13) 0.130(11) 0.044(10) 0.018(11) 0.005(13) F15' 0.260(19) 0.046(7) 0.25(3) 0.002(12) 0.057(19) -0.008(9) F16 0.24(2) 0.49(4) 0.21(2) 0.17(2) 0.163(18) 0.06(3) F17 0.20(2) 0.29(2) 0.38(4) 0.15(2) 0.06(3) -0.141(18) F18 0.101(13) 0.23(3) 0.23(2) 0.04(2) 0.069(14) -0.049(16) F16' 0.32(3) 0.54(5) 0.22(3) 0.16(3) 0.18(3) 0.08(4) F17' 0.23(2) 0.34(3) 0.30(3) 0.16(2) 0.12(2) -0.09(2) F18' 0.107(14) 0.24(3) 0.23(2) 0.07(2) 0.021(13) -0.064(16) O1 0.086(3) 0.062(3) 0.046(2) -0.0054(17) 0.010(2) -0.004(2) O2 0.063(3) 0.086(3) 0.058(3) 0.003(2) 0.004(2) -0.003(2) O3 0.077(3) 0.046(2) 0.057(2) -0.0101(17) 0.017(2) -0.0010(19) O4 0.089(3) 0.057(3) 0.079(3) -0.008(2) 0.011(2) -0.018(2) O5 0.103(4) 0.054(2) 0.068(3) 0.014(2) 0.013(3) -0.013(2) O6 0.093(4) 0.091(4) 0.078(3) 0.017(3) 0.033(3) -0.017(3) O7 0.056(2) 0.0439(18) 0.0369(17) 0.0038(14) 0.0075(15) 0.0013(15) O8 0.063(2) 0.064(2) 0.055(2) -0.0008(19) 0.0195(18) 0.0062(19) O9 0.079(4) 0.167(7) 0.155(6) -0.063(6) 0.036(4) 0.000(4) N1 0.069(3) 0.064(3) 0.041(2) 0.001(2) 0.015(2) 0.004(2) N2 0.082(4) 0.295(8) 0.159(5) 0.154(6) 0.021(4) 0.053(5) C1 0.093(6) 0.165(10) 0.067(4) 0.011(5) 0.036(4) 0.035(6) C2 0.083(4) 0.096(5) 0.049(3) 0.004(3) 0.027(3) 0.004(4) C3 0.091(6) 0.128(8) 0.046(4) 0.016(3) 0.025(4) 0.006(4) C4 0.102(6) 0.103(6) 0.043(3) 0.023(4) 0.016(3) 0.000(5) C5 0.073(4) 0.067(4) 0.042(3) 0.009(3) 0.007(3) 0.000(3) C6 0.074(4) 0.073(4) 0.057(3) 0.022(3) 0.005(3) 0.010(3) C7 0.081(4) 0.199(6) 0.099(4) 0.102(5) 0.026(3) 0.044(4) C8 0.092(4) 0.227(7) 0.105(4) 0.094(5) 0.011(4) 0.031(5) C9 0.093(4) 0.252(7) 0.117(4) 0.108(5) 0.016(4) 0.031(5) C10 0.082(4) 0.255(7) 0.137(4) 0.135(5) 0.033(3) 0.043(4) C11 0.093(4) 0.223(6) 0.150(5) 0.121(5) 0.039(4) 0.054(4) C12 0.089(4) 0.200(6) 0.131(4) 0.108(5) 0.037(4) 0.054(4) C13 0.074(4) 0.070(4) 0.067(4) 0.018(3) 0.019(3) 0.019(3) C14 0.070(4) 0.061(3) 0.051(3) 0.007(3) 0.018(3) 0.012(3) C15 0.063(3) 0.043(3) 0.039(3) 0.002(2) 0.011(2) -0.001(2) C16 0.061(3) 0.049(3) 0.038(3) 0.004(2) 0.008(2) -0.002(2) C17 0.128(9) 0.343(12) 0.203(9) 0.155(8) -0.027(7) -0.003(10) C18 0.154(9) 0.330(11) 0.205(10) 0.175(8) 0.057(8) 0.112(8) C101 0.146(10) 0.127(9) 0.060(5) -0.029(6) 0.017(6) -0.008(8) C102 0.106(6) 0.070(4) 0.048(4) -0.011(3) 0.007(4) -0.012(4) C103 0.090(6) 0.126(8) 0.057(5) -0.010(4) -0.015(4) -0.016(5) C104 0.069(4) 0.099(6) 0.072(5) 0.002(4) -0.006(4) -0.014(4) C105 0.072(6) 0.180(14) 0.119(9) 0.021(9) -0.014(6) -0.011(7) C106 0.102(7) 0.066(8) 0.107(8) -0.023(6) 0.030(6) 0.016(6) C10A 0.102(7) 0.066(8) 0.107(8) -0.023(6) 0.030(6) 0.016(6) C107 0.095(5) 0.057(4) 0.068(4) -0.012(3) 0.016(4) 0.006(3) C108 0.105(6) 0.060(4) 0.097(6) -0.020(4) 0.019(5) -0.002(4) C109 0.123(7) 0.059(4) 0.091(6) -0.013(4) 0.012(5) -0.027(5) C110 0.135(11) 0.068(6) 0.172(15) -0.038(7) -0.003(10) -0.021(6) C111 0.182(13) 0.063(5) 0.102(8) 0.027(5) 0.016(8) -0.002(7) C112 0.154(9) 0.061(4) 0.070(5) 0.013(4) -0.002(5) -0.028(5) C113 0.145(10) 0.113(8) 0.113(8) 0.054(7) 0.011(7) -0.048(7) C114 0.121(8) 0.131(9) 0.103(7) 0.028(6) 0.037(6) -0.054(7) C115 0.128(13) 0.30(3) 0.22(2) 0.15(2) 0.049(14) -0.044(16) _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 Nd1 O4 2.449(5) . ? Nd1 O7 2.464(4) 7_556 ? Nd1 O7 2.464(4) . ? Nd1 O2 2.465(5) . ? Nd1 O6 2.474(5) . ? Nd1 O3 2.476(4) . ? Nd1 O1 2.500(5) . ? Nd1 O5 2.505(5) . ? Nd1 O8 2.604(4) . ? Nd1 Nd1 4.1093(8) 7_556 ? F1 C101 1.321(10) . ? F2 C101 1.301(10) . ? F3 C101 1.323(9) . ? F1' C101 1.309(9) . ? F2' C101 1.333(10) . ? F3' C101 1.323(10) . ? F4 C105 1.357(10) . ? F5 C105 1.313(10) . ? F6 C105 1.299(10) . ? F4' C105 1.287(9) . ? F5' C105 1.357(10) . ? F6' C105 1.315(10) . ? F7 C106 1.325(11) . ? F8 C106 1.312(10) . ? F9 C106 1.312(11) . ? F7' C10A 1.314(10) . ? F8' C10A 1.306(11) . ? F9' C10A 1.319(10) . ? F10 C110 1.314(10) . ? F11 C110 1.302(10) . ? F12 C110 1.342(10) . ? F10' C110 1.331(10) . ? F11' C110 1.326(10) . ? F12' C110 1.311(10) . ? F13 C111 1.332(10) . ? F14 C111 1.291(10) . ? F15 C111 1.336(10) . ? F13' C111 1.333(10) . ? F14' C111 1.322(10) . ? F15' C111 1.285(10) . ? F16 C115 1.324(11) . ? F17 C115 1.327(11) . ? F18 C115 1.314(11) . ? F16' C115 1.329(11) . ? F17' C115 1.323(11) . ? F18' C115 1.305(11) . ? O1 C102 1.244(10) . ? O2 C104 1.244(9) . ? O3 C107 1.262(8) . ? O4 C109 1.263(11) . ? O5 C112 1.224(10) . ? O6 C114 1.240(11) . ? O7 C15 1.341(7) . ? O7 Nd1 2.464(4) 7_556 ? N1 C2 1.343(8) . ? N1 C16 1.361(8) . ? N2 C10 1.414(11) . ? N2 C18 1.445(10) . ? N2 C17 1.457(10) . ? C1 C2 1.490(11) . ? C2 C3 1.378(11) . ? C3 C4 1.382(13) . ? C4 C5 1.404(10) . ? C5 C6 1.419(10) . ? C5 C16 1.430(8) . ? C6 C13 1.374(10) . ? C6 C7 1.480(9) . ? C7 C8 1.383(13) . ? C7 C12 1.396(13) . ? C8 C9 1.391(10) . ? C9 C10 1.392(13) . ? C10 C11 1.400(13) . ? C11 C12 1.405(10) . ? C13 C14 1.397(9) . ? C14 C15 1.373(9) . ? C15 C16 1.423(9) . ? C101 C102 1.535(12) . ? C102 C103 1.358(14) . ? C103 C104 1.388(14) . ? C104 C105 1.553(14) . ? C106 C107 1.46(3) . ? C10A C107 1.55(3) . ? C107 C108 1.373(12) . ? C108 C109 1.380(14) . ? C109 C110 1.534(13) . ? C111 C112 1.493(14) . ? C112 C113 1.419(18) . ? C113 C114 1.400(18) . ? C114 C115 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 O4 Nd1 O7 136.52(15) . 7_556 ? O4 Nd1 O7 138.83(15) . . ? O7 Nd1 O7 67.00(13) 7_556 . ? O4 Nd1 O2 80.61(18) . . ? O7 Nd1 O2 142.65(16) 7_556 . ? O7 Nd1 O2 87.14(14) . . ? O4 Nd1 O6 75.2(2) . . ? O7 Nd1 O6 110.42(16) 7_556 . ? O7 Nd1 O6 135.91(17) . . ? O2 Nd1 O6 69.50(18) . . ? O4 Nd1 O3 72.07(16) . . ? O7 Nd1 O3 73.84(13) 7_556 . ? O7 Nd1 O3 91.06(13) . . ? O2 Nd1 O3 135.70(15) . . ? O6 Nd1 O3 131.85(18) . . ? O4 Nd1 O1 68.09(16) . . ? O7 Nd1 O1 121.73(15) 7_556 . ? O7 Nd1 O1 70.81(13) . . ? O2 Nd1 O1 69.06(17) . . ? O6 Nd1 O1 127.85(18) . . ? O3 Nd1 O1 68.63(16) . . ? O4 Nd1 O5 70.62(16) . . ? O7 Nd1 O5 72.70(14) 7_556 . ? O7 Nd1 O5 138.82(14) . . ? O2 Nd1 O5 132.28(17) . . ? O6 Nd1 O5 66.8(2) . . ? O3 Nd1 O5 69.51(17) . . ? O1 Nd1 O5 127.93(16) . . ? O4 Nd1 O8 140.58(16) . . ? O7 Nd1 O8 68.92(12) 7_556 . ? O7 Nd1 O8 72.61(13) . . ? O2 Nd1 O8 78.10(15) . . ? O6 Nd1 O8 66.41(18) . . ? O3 Nd1 O8 142.69(13) . . ? O1 Nd1 O8 131.26(14) . . ? O5 Nd1 O8 100.80(16) . . ? O4 Nd1 Nd1 152.43(13) . 7_556 ? O7 Nd1 Nd1 33.50(8) 7_556 7_556 ? O7 Nd1 Nd1 33.50(8) . 7_556 ? O2 Nd1 Nd1 116.53(12) . 7_556 ? O6 Nd1 Nd1 129.78(14) . 7_556 ? O3 Nd1 Nd1 81.04(10) . 7_556 ? O1 Nd1 Nd1 96.79(11) . 7_556 ? O5 Nd1 Nd1 105.85(12) . 7_556 ? O8 Nd1 Nd1 66.74(10) . 7_556 ? C102 O1 Nd1 134.1(5) . . ? C104 O2 Nd1 135.4(6) . . ? C107 O3 Nd1 132.9(5) . . ? C109 O4 Nd1 133.1(5) . . ? C112 O5 Nd1 137.1(6) . . ? C114 O6 Nd1 135.7(8) . . ? C15 O7 Nd1 125.7(3) . 7_556 ? C15 O7 Nd1 120.4(3) . . ? Nd1 O7 Nd1 113.00(13) 7_556 . ? C2 N1 C16 124.5(5) . . ? C10 N2 C18 118.2(7) . . ? C10 N2 C17 117.6(8) . . ? C18 N2 C17 118.0(10) . . ? N1 C2 C3 117.7(7) . . ? N1 C2 C1 118.3(6) . . ? C3 C2 C1 124.0(7) . . ? C2 C3 C4 121.1(7) . . ? C3 C4 C5 121.4(7) . . ? C4 C5 C6 124.9(6) . . ? C4 C5 C16 116.1(6) . . ? C6 C5 C16 118.9(6) . . ? C13 C6 C5 117.5(5) . . ? C13 C6 C7 121.1(7) . . ? C5 C6 C7 121.3(7) . . ? C8 C7 C12 118.2(9) . . ? C8 C7 C6 122.8(9) . . ? C12 C7 C6 119.0(9) . . ? C7 C8 C9 123.6(12) . . ? C8 C9 C10 117.1(12) . . ? C9 C10 C11 121.7(9) . . ? C9 C10 N2 119.3(8) . . ? C11 C10 N2 119.1(8) . . ? C10 C11 C12 119.1(12) . . ? C7 C12 C11 120.3(12) . . ? C6 C13 C14 123.1(6) . . ? C15 C14 C13 121.9(6) . . ? O7 C15 C14 124.6(5) . . ? O7 C15 C16 119.0(5) . . ? C14 C15 C16 116.4(5) . . ? N1 C16 C15 118.6(5) . . ? N1 C16 C5 119.2(6) . . ? C15 C16 C5 122.1(6) . . ? F2 C101 F1' 128.0(16) . . ? F2 C101 F1 108.7(11) . . ? F1' C101 F1 38.0(10) . . ? F2 C101 F3' 69.4(11) . . ? F1' C101 F3' 106.3(10) . . ? F1 C101 F3' 135.6(12) . . ? F2 C101 F3 107.3(11) . . ? F1' C101 F3 67.4(10) . . ? F1 C101 F3 104.3(9) . . ? F3' C101 F3 42.9(10) . . ? F2 C101 F2' 38.0(10) . . ? F1' C101 F2' 104.5(11) . . ? F1 C101 F2' 73.6(11) . . ? F3' C101 F2' 104.4(11) . . ? F3 C101 F2' 130.8(14) . . ? F2 C101 C102 113.5(10) . . ? F1' C101 C102 115.4(11) . . ? F1 C101 C102 108.7(10) . . ? F3' C101 C102 112.3(11) . . ? F3 C101 C102 114.0(11) . . ? F2' C101 C102 112.9(10) . . ? O1 C102 C103 128.6(8) . . ? O1 C102 C101 114.3(8) . . ? C103 C102 C101 117.1(7) . . ? C102 C103 C104 122.2(7) . . ? O2 C104 C103 128.1(8) . . ? O2 C104 C105 112.4(8) . . ? C103 C104 C105 119.4(7) . . ? F4' C105 F6 125.2(17) . . ? F4' C105 F5 59.2(11) . . ? F6 C105 F5 112.1(12) . . ? F4' C105 F6' 112.5(13) . . ? F6 C105 F6' 36.0(11) . . ? F5 C105 F6' 139.6(17) . . ? F4' C105 F5' 107.5(11) . . ? F6 C105 F5' 66.8(12) . . ? F5 C105 F5' 53.2(11) . . ? F6' C105 F5' 102.7(12) . . ? F4' C105 F4 45.4(10) . . ? F6 C105 F4 105.2(11) . . ? F5 C105 F4 104.3(10) . . ? F6' C105 F4 75.2(12) . . ? F5' C105 F4 142.7(13) . . ? F4' C105 C104 115.9(13) . . ? F6 C105 C104 117.2(10) . . ? F5 C105 C104 110.0(11) . . ? F6' C105 C104 108.6(13) . . ? F5' C105 C104 108.7(9) . . ? F4 C105 C104 107.1(11) . . ? F8 C106 F9 101.8(17) . . ? F8 C106 F7 101.7(18) . . ? F9 C106 F7 101.0(16) . . ? F8 C106 C107 119(2) . . ? F9 C106 C107 117.5(18) . . ? F7 C106 C107 113.0(18) . . ? F8' C10A F7' 110.3(16) . . ? F8' C10A F9' 108.6(17) . . ? F7' C10A F9' 107.0(17) . . ? F8' C10A C107 110.5(18) . . ? F7' C10A C107 112(2) . . ? F9' C10A C107 108.8(18) . . ? O3 C107 C108 128.8(8) . . ? O3 C107 C106 110.7(9) . . ? C108 C107 C106 120.3(9) . . ? O3 C107 C10A 116.7(9) . . ? C108 C107 C10A 114.4(9) . . ? C106 C107 C10A 10.5(12) . . ? C107 C108 C109 123.4(7) . . ? O4 C109 C108 129.5(7) . . ? O4 C109 C110 113.2(9) . . ? C108 C109 C110 117.2(8) . . ? F11 C110 F12' 129.9(17) . . ? F11 C110 F10 109.3(12) . . ? F12' C110 F10 62.9(12) . . ? F11 C110 F11' 37.0(11) . . ? F12' C110 F11' 106.4(11) . . ? F10 C110 F11' 129.3(16) . . ? F11 C110 F10' 69.3(12) . . ? F12' C110 F10' 107.9(12) . . ? F10 C110 F10' 47.4(12) . . ? F11' C110 F10' 103.6(11) . . ? F11 C110 F12 106.3(11) . . ? F12' C110 F12 43.3(11) . . ? F10 C110 F12 104.5(11) . . ? F11' C110 F12 71.0(11) . . ? F10' C110 F12 140.3(15) . . ? F11 C110 C109 112.8(13) . . ? F12' C110 C109 114.8(12) . . ? F10 C110 C109 114.3(11) . . ? F11' C110 C109 114.6(13) . . ? F10' C110 C109 108.7(11) . . ? F12 C110 C109 109.0(11) . . ? F15' C111 F14 121.8(19) . . ? F15' C111 F14' 109.6(12) . . ? F14 C111 F14' 45.2(13) . . ? F15' C111 F13 61.0(11) . . ? F14 C111 F13 109.1(13) . . ? F14' C111 F13 146.3(17) . . ? F15' C111 F13' 108.1(12) . . ? F14 C111 F13' 57.5(13) . . ? F14' C111 F13' 102.7(12) . . ? F13 C111 F13' 57.0(13) . . ? F15' C111 F15 40.0(11) . . ? F14 C111 F15 106.9(12) . . ? F14' C111 F15 74.3(11) . . ? F13 C111 F15 100.8(11) . . ? F13' C111 F15 135.2(14) . . ? F15' C111 C112 117.4(14) . . ? F14 C111 C112 120.0(13) . . ? F14' C111 C112 105.8(13) . . ? F13 C111 C112 107.0(12) . . ? F13' C111 C112 112.3(10) . . ? F15 C111 C112 111.3(13) . . ? O5 C112 C113 125.1(9) . . ? O5 C112 C111 117.6(11) . . ? C113 C112 C111 117.3(8) . . ? C114 C113 C112 120.7(8) . . ? O6 C114 C113 127.8(10) . . ? O6 C114 C115 116.1(12) . . ? C113 C114 C115 115.8(9) . . ? F18' C115 F18 24(3) . . ? F18' C115 F17' 109.3(15) . . ? F18 C115 F17' 129(3) . . ? F18' C115 F16 122(5) . . ? F18 C115 F16 107.5(15) . . ? F17' C115 F16 79(2) . . ? F18' C115 F17 85(3) . . ? F18 C115 F17 108.1(15) . . ? F17' C115 F17 31(2) . . ? F16 C115 F17 107.8(15) . . ? F18' C115 F16' 109.0(17) . . ? F18 C115 F16' 88(3) . . ? F17' C115 F16' 107.2(15) . . ? F16 C115 F16' 28(2) . . ? F17 C115 F16' 135(2) . . ? F18' C115 C114 114(2) . . ? F18 C115 C114 109.9(19) . . ? F17' C115 C114 113(2) . . ? F16 C115 C114 114(2) . . ? F17 C115 C114 109.4(19) . . ? F16' C115 C114 104(3) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.371 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.136