# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Peter Nockemann' _publ_contact_author_email P.NOCKEMANN@QUB.AC.UK _publ_section_title ; Hydrophobic Ionic Liquids with Strongly Coordinating Anions ; loop_ _publ_author_name 'Peter Nockemann' 'Koen Binnemans' 'Hasan Mehdi' 'Kristof Van Hecke' 'Luc Van Meervelt' # Attachment 'wg201_fin.cif' data_wg201 _database_code_depnum_ccdc_archive 'CCDC 742062' #TrackingRef 'wg201_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H3 Co F18 O6, C8 H15 N2' _chemical_formula_sum 'C23 H18 Co F18 N2 O6' _chemical_formula_weight 819.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0040(6) _cell_length_b 17.7374(11) _cell_length_c 20.1614(11) _cell_angle_alpha 74.172(3) _cell_angle_beta 87.160(4) _cell_angle_gamma 89.240(4) _cell_volume 3094.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2649 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 69.10 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 5.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.128 _exptl_absorpt_correction_T_max 0.421 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29476 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.1030 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 70.07 _reflns_number_total 11258 _reflns_number_gt 8050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0611P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11258 _refine_ls_number_parameters 990 _refine_ls_number_restraints 286 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1407 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.099 _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 C1 C 0.2118(5) 0.0545(2) 0.6418(2) 0.0284(9) Uani 1 1 d . . . C2 C 0.2593(4) 0.1109(2) 0.6830(2) 0.0236(8) Uani 1 1 d . . . C3 C 0.2337(5) 0.0861(2) 0.7536(2) 0.0286(9) Uani 1 1 d . . . H3 H 0.2001 0.0340 0.7739 0.034 Uiso 1 1 calc R . . C4 C 0.2551(5) 0.1342(2) 0.7961(2) 0.0257(9) Uani 1 1 d . . . C5 C 0.2029(7) 0.1035(3) 0.8731(3) 0.0439(13) Uani 1 1 d . . . C6 C 0.0509(5) 0.4422(2) 0.6455(2) 0.0309(10) Uani 1 1 d . . . C7 C 0.2010(5) 0.4035(2) 0.6663(2) 0.0236(8) Uani 1 1 d . . . C8 C 0.3110(5) 0.4501(2) 0.6827(2) 0.0302(9) Uani 1 1 d . . . H8 H 0.2940 0.5047 0.6755 0.036 Uiso 1 1 calc R . . C9 C 0.4445(5) 0.4177(2) 0.7092(2) 0.0277(9) Uani 1 1 d . . . C10 C 0.5584(7) 0.4736(3) 0.7248(3) 0.0497(14) Uani 1 1 d . . . C11 C 0.8581(5) 0.2001(2) 0.7080(2) 0.0257(9) Uani 1 1 d . . . C12 C 0.7167(5) 0.2330(2) 0.6725(2) 0.0225(8) Uani 1 1 d . . . C13 C 0.7342(5) 0.2901(2) 0.6091(2) 0.0247(9) Uani 1 1 d . . . H13 H 0.8321 0.3034 0.5900 0.030 Uiso 1 1 calc R . . C14 C 0.6158(5) 0.3280(2) 0.5729(2) 0.0236(9) Uani 1 1 d . . . C15 C 0.6518(5) 0.3916(2) 0.5045(2) 0.0280(9) Uani 1 1 d . . . C16 C 0.3979(6) 0.0232(3) 0.1026(3) 0.0397(12) Uani 1 1 d . . . C17 C 0.4326(5) 0.0615(2) 0.1600(2) 0.0251(9) Uani 1 1 d . . . C18 C 0.3992(5) 0.0194(2) 0.2280(2) 0.0260(9) Uani 1 1 d . . . H18 H 0.3690 -0.0338 0.2379 0.031 Uiso 1 1 calc R . . C19 C 0.4093(5) 0.0539(2) 0.2815(2) 0.0219(8) Uani 1 1 d . C . C20 C 0.3466(5) 0.0072(2) 0.3537(2) 0.0292(8) Uani 1 1 d DU . . C21 C 0.8183(5) 0.3371(2) 0.2938(2) 0.0264(9) Uani 1 1 d . . . C22 C 0.7814(5) 0.2688(2) 0.26453(19) 0.0214(8) Uani 1 1 d . C . C23 C 0.9004(5) 0.2264(2) 0.2464(2) 0.0279(9) Uani 1 1 d . . . H23 H 0.9978 0.2382 0.2566 0.033 Uiso 1 1 calc R . . C24 C 0.8822(5) 0.1672(2) 0.2138(2) 0.0249(9) Uani 1 1 d . C . C25 C 1.0248(5) 0.1291(2) 0.1939(2) 0.0363(9) Uani 1 1 d DU . . C26 C 0.2353(5) 0.3852(2) 0.1641(2) 0.0270(9) Uani 1 1 d . . . C27 C 0.3791(5) 0.3422(2) 0.15346(19) 0.0219(8) Uani 1 1 d . C . C28 C 0.4896(5) 0.3842(2) 0.1069(2) 0.0234(8) Uani 1 1 d . . . H28 H 0.4782 0.4391 0.0881 0.028 Uiso 1 1 calc R . . C29 C 0.6142(5) 0.3477(2) 0.08784(19) 0.0226(8) Uani 1 1 d . C . C30 C 0.7250(5) 0.3974(2) 0.0330(2) 0.0282(9) Uani 1 1 d . . . C31 C 0.3482(5) 0.2388(2) 0.4822(2) 0.0295(9) Uani 1 1 d . . . H31 H 0.3619 0.2157 0.5299 0.035 Uiso 1 1 calc R . . C32 C 0.3665(6) 0.2629(3) 0.3696(2) 0.0330(10) Uani 1 1 d . . . H32 H 0.3957 0.2601 0.3244 0.040 Uiso 1 1 calc R . . C33 C 0.2675(5) 0.3137(3) 0.3862(2) 0.0325(10) Uani 1 1 d . . . H33 H 0.2138 0.3530 0.3547 0.039 Uiso 1 1 calc R . . C34 C 0.1697(6) 0.3408(3) 0.4969(3) 0.0389(11) Uani 1 1 d . . . H34A H 0.1652 0.3109 0.5457 0.058 Uiso 1 1 calc R . . H34B H 0.0688 0.3483 0.4801 0.058 Uiso 1 1 calc R . . H34C H 0.2153 0.3920 0.4921 0.058 Uiso 1 1 calc R . . C35 C 0.5323(6) 0.1555(2) 0.4371(2) 0.0314(10) Uani 1 1 d . . . H35A H 0.5536 0.1454 0.3916 0.038 Uiso 1 1 calc R . . H35B H 0.4942 0.1063 0.4694 0.038 Uiso 1 1 calc R . . C36 C 0.6741(6) 0.1782(2) 0.4629(2) 0.0302(9) Uani 1 1 d . . . H36A H 0.6579 0.1776 0.5120 0.036 Uiso 1 1 calc R . . H36B H 0.7014 0.2323 0.4364 0.036 Uiso 1 1 calc R . . C37 C 0.8014(6) 0.1231(3) 0.4562(2) 0.0347(10) Uani 1 1 d . . . H37A H 0.8148 0.1221 0.4074 0.042 Uiso 1 1 calc R . . H37B H 0.7755 0.0694 0.4842 0.042 Uiso 1 1 calc R . . C38 C 0.9483(7) 0.1477(4) 0.4798(3) 0.0530(14) Uani 1 1 d . . . H38A H 0.9761 0.2002 0.4512 0.080 Uiso 1 1 calc R . . H38B H 1.0266 0.1104 0.4751 0.080 Uiso 1 1 calc R . . H38C H 0.9360 0.1484 0.5282 0.080 Uiso 1 1 calc R . . C39 C 0.4301(6) 0.7855(3) 0.0188(2) 0.0348(11) Uani 1 1 d . . . H39 H 0.4796 0.7973 -0.0255 0.042 Uiso 1 1 calc R . . C40 C 0.2586(7) 0.7760(3) 0.1015(2) 0.0432(13) Uani 1 1 d . . . H40 H 0.1660 0.7805 0.1248 0.052 Uiso 1 1 calc R . . C41 C 0.3813(7) 0.7419(3) 0.1305(2) 0.0435(13) Uani 1 1 d . . . H41 H 0.3927 0.7176 0.1781 0.052 Uiso 1 1 calc R . . C42 C 0.1872(8) 0.8421(4) -0.0196(3) 0.0587(16) Uani 1 1 d . . . H42A H 0.2391 0.8580 -0.0651 0.088 Uiso 1 1 calc R . . H42B H 0.1463 0.8886 -0.0078 0.088 Uiso 1 1 calc R . . H42C H 0.1062 0.8061 -0.0203 0.088 Uiso 1 1 calc R . . C43 C 0.6433(8) 0.7192(4) 0.0844(3) 0.0614(16) Uani 1 1 d DU . . H43A H 0.7091 0.7605 0.0549 0.074 Uiso 1 1 calc R A 1 H43B H 0.6688 0.7133 0.1328 0.074 Uiso 1 1 calc R A 1 C44A C 0.6828(10) 0.6453(6) 0.0681(6) 0.067(2) Uani 0.673(10) 1 d PDU B 1 H44A H 0.6496 0.6481 0.0214 0.080 Uiso 0.673(10) 1 calc PR B 1 H44B H 0.6275 0.6020 0.1012 0.080 Uiso 0.673(10) 1 calc PR B 1 C45A C 0.8445(11) 0.6261(8) 0.0702(6) 0.069(3) Uani 0.673(10) 1 d PDU B 1 H45A H 0.8987 0.6685 0.0356 0.083 Uiso 0.673(10) 1 calc PR B 1 H45B H 0.8597 0.5773 0.0559 0.083 Uiso 0.673(10) 1 calc PR B 1 C46A C 0.9137(11) 0.6153(7) 0.1383(5) 0.072(3) Uani 0.673(10) 1 d PDU B 1 H46A H 0.9112 0.6651 0.1506 0.108 Uiso 0.673(10) 1 calc PR B 1 H46B H 1.0171 0.5982 0.1349 0.108 Uiso 0.673(10) 1 calc PR B 1 H46C H 0.8580 0.5756 0.1739 0.108 Uiso 0.673(10) 1 calc PR B 1 C44B C 0.6255(18) 0.6304(7) 0.0946(11) 0.063(3) Uani 0.327(10) 1 d PDU B 2 H44C H 0.5381 0.6122 0.1265 0.076 Uiso 0.327(10) 1 calc PR B 2 H44D H 0.6036 0.6217 0.0497 0.076 Uiso 0.327(10) 1 calc PR B 2 C45B C 0.7562(19) 0.5806(9) 0.1224(10) 0.068(3) Uani 0.327(10) 1 d PDU B 2 H45C H 0.7749 0.5857 0.1689 0.082 Uiso 0.327(10) 1 calc PR B 2 H45D H 0.7328 0.5250 0.1269 0.082 Uiso 0.327(10) 1 calc PR B 2 C46B C 0.893(2) 0.6033(15) 0.0768(14) 0.067(5) Uani 0.327(10) 1 d PDU B 2 H46D H 0.8726 0.6033 0.0296 0.101 Uiso 0.327(10) 1 calc PR B 2 H46E H 0.9729 0.5656 0.0937 0.101 Uiso 0.327(10) 1 calc PR B 2 H46F H 0.9249 0.6558 0.0773 0.101 Uiso 0.327(10) 1 calc PR B 2 N1 N 0.2586(4) 0.2980(2) 0.45666(18) 0.0285(8) Uani 1 1 d . . . N2 N 0.4166(4) 0.2166(2) 0.43009(17) 0.0275(8) Uani 1 1 d . . . N3 N 0.2911(5) 0.8033(2) 0.0317(2) 0.0373(10) Uani 1 1 d . . . N4 N 0.4895(5) 0.7489(2) 0.0772(2) 0.0392(10) Uani 1 1 d . B . O1 O 0.3106(3) 0.17558(14) 0.64705(14) 0.0230(6) Uani 1 1 d . . . O2 O 0.3092(3) 0.20178(15) 0.78161(14) 0.0262(6) Uani 1 1 d . . . O3 O 0.2070(3) 0.33330(15) 0.66593(14) 0.0232(6) Uani 1 1 d . . . O4 O 0.4877(4) 0.34807(15) 0.72252(15) 0.0277(6) Uani 1 1 d . . . O5 O 0.5978(3) 0.20637(15) 0.70547(14) 0.0239(6) Uani 1 1 d . . . O6 O 0.4787(3) 0.31938(15) 0.58815(14) 0.0246(6) Uani 1 1 d . . . O7 O 0.4841(3) 0.12988(16) 0.13734(14) 0.0250(6) Uani 1 1 d . . . O8 O 0.4617(3) 0.11939(15) 0.28098(13) 0.0223(6) Uani 1 1 d . . . O9 O 0.6454(3) 0.26076(15) 0.25684(14) 0.0235(6) Uani 1 1 d . . . O10 O 0.7664(3) 0.14107(14) 0.19790(14) 0.0226(6) Uani 1 1 d . . . O11 O 0.3787(3) 0.27185(15) 0.18728(14) 0.0253(6) Uani 1 1 d . . . O12 O 0.6524(3) 0.27706(15) 0.10809(14) 0.0257(6) Uani 1 1 d . . . F1 F 0.2601(4) 0.07703(14) 0.57607(14) 0.0427(7) Uani 1 1 d . . . F2 F 0.2644(3) -0.01779(13) 0.66876(13) 0.0360(6) Uani 1 1 d . . . F3 F 0.0640(4) 0.04856(18) 0.64270(19) 0.0515(8) Uani 1 1 d . . . F4 F 0.1593(6) 0.0301(2) 0.89081(18) 0.0838(15) Uani 1 1 d U . . F5 F 0.0930(4) 0.1486(2) 0.88769(16) 0.0652(10) Uani 1 1 d . . . F6 F 0.3114(4) 0.1090(2) 0.91414(15) 0.0577(9) Uani 1 1 d . . . F7 F 0.0183(4) 0.4383(2) 0.58228(18) 0.0584(9) Uani 1 1 d . . . F8 F -0.0578(4) 0.40604(17) 0.6875(2) 0.0621(11) Uani 1 1 d . . . F9 F 0.0437(3) 0.51757(14) 0.64348(16) 0.0391(6) Uani 1 1 d . . . F10 F 0.5005(4) 0.5367(2) 0.7385(3) 0.0756(13) Uani 1 1 d . . . F11 F 0.6502(5) 0.5013(3) 0.6677(3) 0.0871(15) Uani 1 1 d . . . F12 F 0.6475(5) 0.4390(2) 0.7724(3) 0.0824(14) Uani 1 1 d . . . F13 F 0.8436(3) 0.12655(14) 0.74613(17) 0.0439(7) Uani 1 1 d . . . F14 F 0.8975(3) 0.24209(15) 0.75028(14) 0.0372(6) Uani 1 1 d . . . F15 F 0.9749(3) 0.20265(16) 0.66322(14) 0.0386(6) Uani 1 1 d . . . F16 F 0.6523(4) 0.46198(15) 0.51562(16) 0.0491(8) Uani 1 1 d . . . F17 F 0.7846(3) 0.38136(17) 0.47605(14) 0.0434(7) Uani 1 1 d . . . F18 F 0.5523(3) 0.39229(16) 0.45842(13) 0.0388(6) Uani 1 1 d . . . F19 F 0.5072(4) 0.03715(17) 0.05389(16) 0.0539(9) Uani 1 1 d . . . F20 F 0.2777(5) 0.0561(3) 0.0711(2) 0.0810(13) Uani 1 1 d . . . F21 F 0.3804(6) -0.0534(2) 0.12450(18) 0.0775(15) Uani 1 1 d . . . F22A F 0.2687(5) -0.0546(2) 0.35388(18) 0.0536(12) Uani 0.858(6) 1 d PDU C 1 F23A F 0.2543(5) 0.0533(2) 0.37995(18) 0.0537(12) Uani 0.858(6) 1 d PDU C 1 F24A F 0.4513(4) -0.0126(3) 0.39842(19) 0.0557(11) Uani 0.858(6) 1 d PDU C 1 F22B F 0.382(2) -0.0686(6) 0.3609(9) 0.043(3) Uani 0.142(6) 1 d PDU C 2 F23B F 0.2021(10) 0.0077(13) 0.3586(10) 0.050(4) Uani 0.142(6) 1 d PDU C 2 F24B F 0.402(2) 0.0243(13) 0.4057(8) 0.046(3) Uani 0.142(6) 1 d PDU C 2 F25 F 0.7064(3) 0.35164(14) 0.33434(13) 0.0319(6) Uani 1 1 d . . . F26 F 0.9387(3) 0.32302(16) 0.33160(15) 0.0398(6) Uani 1 1 d . . . F27 F 0.8453(3) 0.40204(13) 0.24329(14) 0.0388(7) Uani 1 1 d . . . F28A F 1.1361(7) 0.1343(5) 0.2328(4) 0.0786(19) Uani 0.737(8) 1 d PDU D 1 F29A F 1.0777(6) 0.1730(3) 0.1321(3) 0.0743(18) Uani 0.737(8) 1 d PDU D 1 F30A F 1.0093(6) 0.0599(3) 0.1891(4) 0.0704(19) Uani 0.737(8) 1 d PDU D 1 F28B F 1.0268(16) 0.0555(6) 0.2347(8) 0.059(3) Uani 0.263(8) 1 d PDU D 2 F29B F 1.1501(12) 0.1596(8) 0.1954(9) 0.052(3) Uani 0.263(8) 1 d PDU D 2 F30B F 1.0221(15) 0.1183(10) 0.1309(6) 0.064(3) Uani 0.263(8) 1 d PDU D 2 F31 F 0.1239(3) 0.36156(19) 0.13321(18) 0.0514(8) Uani 1 1 d . . . F32 F 0.1942(3) 0.37015(17) 0.23061(14) 0.0454(8) Uani 1 1 d . . . F33 F 0.2447(3) 0.46286(14) 0.13958(15) 0.0421(7) Uani 1 1 d . . . F34 F 0.8596(4) 0.3942(2) 0.05659(18) 0.0610(10) Uani 1 1 d . . . F35 F 0.6889(3) 0.47304(14) 0.01288(15) 0.0435(7) Uani 1 1 d . . . F36 F 0.7316(5) 0.37229(18) -0.02292(16) 0.0602(11) Uani 1 1 d . . . Co1 Co 0.39372(8) 0.26259(3) 0.68581(3) 0.02192(16) Uani 1 1 d . . . Co2 Co 0.56142(7) 0.19778(3) 0.19562(3) 0.02045(16) Uani 1 1 d . C . 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 C1 0.032(3) 0.0214(18) 0.032(2) -0.0049(16) -0.0103(17) 0.0022(16) C2 0.017(2) 0.0215(18) 0.029(2) -0.0010(15) -0.0070(15) 0.0054(15) C3 0.033(2) 0.0254(19) 0.024(2) 0.0012(16) -0.0066(17) -0.0018(17) C4 0.027(2) 0.0245(19) 0.021(2) 0.0011(15) -0.0013(16) -0.0003(16) C5 0.056(4) 0.043(3) 0.026(2) 0.003(2) 0.001(2) -0.013(2) C6 0.026(2) 0.0237(19) 0.042(3) -0.0077(18) -0.0004(19) -0.0004(17) C7 0.022(2) 0.0276(19) 0.0183(18) -0.0022(15) 0.0032(15) 0.0003(16) C8 0.029(2) 0.0261(19) 0.036(2) -0.0096(17) -0.0032(18) -0.0007(17) C9 0.029(2) 0.030(2) 0.025(2) -0.0088(17) -0.0012(16) 0.0002(17) C10 0.047(3) 0.027(2) 0.074(4) -0.010(2) -0.028(3) 0.004(2) C11 0.026(2) 0.0222(18) 0.025(2) 0.0012(15) 0.0000(16) -0.0017(16) C12 0.023(2) 0.0218(17) 0.023(2) -0.0061(15) 0.0016(16) 0.0000(15) C13 0.023(2) 0.0244(18) 0.025(2) -0.0057(16) 0.0045(16) -0.0029(15) C14 0.029(2) 0.0207(17) 0.0194(19) -0.0041(15) 0.0037(16) -0.0041(15) C15 0.030(3) 0.031(2) 0.020(2) -0.0011(16) 0.0012(16) -0.0046(17) C16 0.047(3) 0.046(3) 0.029(2) -0.017(2) 0.007(2) -0.014(2) C17 0.026(2) 0.0252(19) 0.025(2) -0.0090(16) 0.0029(16) -0.0016(16) C18 0.026(2) 0.0242(18) 0.026(2) -0.0055(16) 0.0028(16) -0.0002(16) C19 0.021(2) 0.0199(17) 0.0207(19) 0.0009(14) 0.0024(15) 0.0009(14) C20 0.034(2) 0.0301(17) 0.0196(18) -0.0010(15) 0.0030(14) -0.0068(15) C21 0.028(2) 0.0268(19) 0.024(2) -0.0067(16) -0.0011(16) -0.0020(16) C22 0.022(2) 0.0231(17) 0.0161(18) -0.0010(14) 0.0021(14) -0.0035(15) C23 0.025(2) 0.0242(18) 0.035(2) -0.0084(17) -0.0041(17) -0.0003(16) C24 0.025(2) 0.0200(17) 0.025(2) 0.0019(15) 0.0014(16) -0.0028(16) C25 0.022(2) 0.0331(17) 0.059(2) -0.0212(17) -0.0002(17) 0.0013(16) C26 0.024(2) 0.031(2) 0.021(2) 0.0026(16) -0.0045(16) 0.0054(17) C27 0.026(2) 0.0229(18) 0.0166(18) -0.0046(14) -0.0078(15) 0.0024(15) C28 0.027(2) 0.0192(17) 0.0192(19) 0.0028(14) -0.0019(15) 0.0045(15) C29 0.023(2) 0.0264(19) 0.0144(17) 0.0012(15) -0.0032(14) -0.0019(16) C30 0.029(2) 0.0265(19) 0.023(2) 0.0025(16) 0.0004(17) -0.0005(17) C31 0.037(3) 0.034(2) 0.0162(19) -0.0058(16) 0.0009(16) -0.0073(18) C32 0.037(3) 0.042(2) 0.017(2) -0.0033(17) 0.0013(17) 0.001(2) C33 0.027(2) 0.047(2) 0.020(2) -0.0029(18) -0.0010(16) -0.0026(19) C34 0.035(3) 0.052(3) 0.031(2) -0.014(2) -0.0027(19) 0.007(2) C35 0.043(3) 0.0267(19) 0.025(2) -0.0065(16) -0.0016(18) -0.0012(18) C36 0.043(3) 0.0266(19) 0.021(2) -0.0053(16) -0.0056(17) 0.0043(18) C37 0.044(3) 0.035(2) 0.022(2) -0.0014(17) -0.0038(18) 0.009(2) C38 0.049(4) 0.064(3) 0.043(3) -0.009(3) -0.014(2) 0.017(3) C39 0.050(3) 0.033(2) 0.021(2) -0.0066(17) -0.0017(19) -0.003(2) C40 0.064(4) 0.044(3) 0.020(2) -0.0067(19) 0.008(2) -0.005(2) C41 0.070(4) 0.040(2) 0.019(2) -0.0056(19) 0.001(2) -0.005(2) C42 0.057(4) 0.080(4) 0.030(3) -0.001(3) 0.001(2) 0.016(3) C43 0.060(4) 0.082(4) 0.055(3) -0.038(3) -0.023(3) 0.030(3) C44A 0.056(5) 0.088(5) 0.078(5) -0.057(4) -0.003(4) 0.015(4) C45A 0.047(6) 0.090(6) 0.085(6) -0.050(5) 0.009(5) 0.007(5) C46A 0.049(6) 0.079(6) 0.087(7) -0.024(5) 0.009(5) 0.007(5) C44B 0.054(7) 0.088(6) 0.064(6) -0.049(5) -0.004(6) 0.024(6) C45B 0.051(6) 0.086(6) 0.079(6) -0.044(6) -0.003(5) 0.012(5) C46B 0.043(10) 0.077(10) 0.088(10) -0.035(9) 0.003(9) 0.010(8) N1 0.025(2) 0.0379(18) 0.0212(17) -0.0048(14) -0.0017(14) -0.0050(15) N2 0.029(2) 0.0347(17) 0.0174(16) -0.0050(14) 0.0005(13) -0.0044(15) N3 0.053(3) 0.0358(19) 0.0195(19) -0.0025(15) 0.0044(17) 0.0002(18) N4 0.059(3) 0.0363(19) 0.026(2) -0.0138(16) -0.0083(18) 0.0040(18) O1 0.0239(16) 0.0217(12) 0.0225(14) -0.0053(11) 0.0025(11) -0.0003(11) O2 0.0286(17) 0.0266(14) 0.0207(14) -0.0021(11) 0.0012(11) 0.0001(12) O3 0.0213(15) 0.0214(12) 0.0257(14) -0.0048(10) 0.0014(11) -0.0017(10) O4 0.0346(18) 0.0233(13) 0.0250(15) -0.0057(11) -0.0062(12) 0.0030(12) O5 0.0222(15) 0.0228(12) 0.0246(14) -0.0029(11) -0.0015(11) 0.0003(11) O6 0.0242(16) 0.0269(13) 0.0191(13) -0.0004(11) -0.0012(11) 0.0011(11) O7 0.0274(16) 0.0296(14) 0.0169(13) -0.0051(11) 0.0010(11) -0.0014(12) O8 0.0244(15) 0.0227(12) 0.0168(13) -0.0005(10) -0.0007(10) -0.0013(11) O9 0.0234(16) 0.0262(13) 0.0204(14) -0.0058(11) 0.0019(11) -0.0019(11) O10 0.0240(16) 0.0205(12) 0.0212(13) -0.0023(10) -0.0013(11) 0.0019(11) O11 0.0244(16) 0.0242(13) 0.0221(14) 0.0023(11) 0.0005(11) -0.0005(11) O12 0.0264(16) 0.0262(13) 0.0201(14) 0.0002(11) 0.0030(11) 0.0029(11) F1 0.072(2) 0.0302(12) 0.0256(13) -0.0060(10) -0.0115(13) -0.0018(13) F2 0.0533(18) 0.0210(11) 0.0323(14) -0.0043(10) -0.0078(12) 0.0054(11) F3 0.0343(18) 0.0528(16) 0.078(2) -0.0335(16) -0.0178(15) 0.0023(13) F4 0.149(4) 0.059(2) 0.0329(18) 0.0058(15) 0.008(2) -0.054(2) F5 0.049(2) 0.105(3) 0.0311(16) -0.0050(17) 0.0194(15) 0.0049(19) F6 0.073(2) 0.068(2) 0.0240(15) 0.0037(14) -0.0142(14) 0.0004(17) F7 0.051(2) 0.079(2) 0.060(2) -0.0402(18) -0.0294(16) 0.0309(17) F8 0.0277(17) 0.0444(16) 0.095(3) 0.0101(16) 0.0188(17) 0.0042(13) F9 0.0342(16) 0.0249(12) 0.0582(18) -0.0103(12) -0.0092(12) 0.0053(10) F10 0.056(2) 0.0525(19) 0.142(4) -0.062(2) -0.042(2) 0.0161(16) F11 0.061(3) 0.080(3) 0.121(4) -0.027(3) 0.004(3) -0.038(2) F12 0.087(3) 0.0489(18) 0.121(4) -0.028(2) -0.071(3) 0.0101(18) F13 0.0322(16) 0.0250(12) 0.0630(19) 0.0094(12) -0.0119(13) -0.0019(11) F14 0.0380(16) 0.0412(14) 0.0334(14) -0.0106(11) -0.0090(11) -0.0013(11) F15 0.0259(15) 0.0507(15) 0.0358(14) -0.0070(12) 0.0011(11) 0.0141(11) F16 0.075(2) 0.0249(12) 0.0395(16) 0.0035(11) 0.0019(15) -0.0075(13) F17 0.0276(15) 0.0587(17) 0.0300(14) 0.0097(12) 0.0083(11) 0.0021(12) F18 0.0342(16) 0.0520(15) 0.0210(12) 0.0063(11) -0.0026(10) -0.0060(12) F19 0.077(2) 0.0496(16) 0.0411(17) -0.0264(14) 0.0253(17) -0.0143(15) F20 0.064(3) 0.143(4) 0.063(2) -0.069(3) -0.0224(19) 0.007(3) F21 0.142(4) 0.0523(19) 0.0453(19) -0.0289(16) 0.029(2) -0.049(2) F22A 0.075(3) 0.0511(19) 0.0327(18) -0.0101(15) 0.0213(17) -0.041(2) F23A 0.071(3) 0.0484(18) 0.0344(19) -0.0037(14) 0.0276(18) 0.0067(17) F24A 0.046(2) 0.074(3) 0.0267(17) 0.0205(18) -0.0051(14) -0.0106(17) F22B 0.065(8) 0.029(4) 0.024(7) 0.008(5) 0.011(7) -0.004(5) F23B 0.036(3) 0.063(8) 0.040(7) 0.006(7) 0.009(5) -0.007(5) F24B 0.062(8) 0.054(7) 0.018(6) -0.006(6) 0.000(6) -0.009(7) F25 0.0329(15) 0.0335(12) 0.0324(13) -0.0146(10) 0.0024(10) -0.0011(10) F26 0.0358(16) 0.0446(14) 0.0454(16) -0.0214(13) -0.0137(12) 0.0005(12) F27 0.0520(18) 0.0223(11) 0.0384(15) -0.0032(10) 0.0088(13) -0.0104(11) F28A 0.039(3) 0.102(5) 0.120(4) -0.071(4) -0.037(3) 0.041(3) F29A 0.053(3) 0.073(3) 0.084(3) -0.007(2) 0.038(2) 0.016(3) F30A 0.040(3) 0.040(2) 0.146(5) -0.055(3) 0.024(3) -0.0021(19) F28B 0.034(6) 0.039(4) 0.093(6) -0.003(4) 0.022(6) 0.009(4) F29B 0.032(4) 0.037(4) 0.098(7) -0.037(5) 0.007(5) -0.005(4) F30B 0.037(6) 0.100(8) 0.069(4) -0.046(4) -0.010(5) 0.027(6) F31 0.0283(17) 0.0676(19) 0.062(2) -0.0216(16) -0.0174(14) 0.0116(14) F32 0.0406(18) 0.0603(16) 0.0258(14) 0.0015(12) 0.0085(12) 0.0228(13) F33 0.0425(17) 0.0294(12) 0.0461(16) 0.0012(11) 0.0098(13) 0.0129(11) F34 0.0288(17) 0.070(2) 0.059(2) 0.0251(16) -0.0001(14) -0.0092(15) F35 0.0449(18) 0.0268(12) 0.0457(17) 0.0098(11) 0.0127(13) -0.0020(11) F36 0.094(3) 0.0539(17) 0.0307(16) -0.0127(14) 0.0312(17) -0.0293(18) Co1 0.0237(4) 0.0216(3) 0.0183(3) -0.0023(2) 0.0020(2) -0.0004(2) Co2 0.0223(4) 0.0209(3) 0.0154(3) -0.0004(2) -0.0005(2) 0.0001(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 C1 F1 1.327(5) . ? C1 F3 1.335(6) . ? C1 F2 1.340(5) . ? C1 C2 1.541(6) . ? C2 O1 1.258(5) . ? C2 C3 1.378(6) . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 O2 1.253(5) . ? C4 C5 1.548(6) . ? C5 F4 1.313(6) . ? C5 F6 1.333(7) . ? C5 F5 1.336(7) . ? C6 F8 1.312(5) . ? C6 F9 1.327(5) . ? C6 F7 1.343(6) . ? C6 C7 1.532(7) . ? C7 O3 1.249(5) . ? C7 C8 1.405(6) . ? C8 C9 1.393(7) . ? C8 H8 0.9500 . ? C9 O4 1.251(5) . ? C9 C10 1.538(7) . ? C10 F12 1.298(7) . ? C10 F10 1.319(6) . ? C10 F11 1.363(8) . ? C11 F13 1.326(5) . ? C11 F14 1.339(5) . ? C11 F15 1.344(5) . ? C11 C12 1.521(6) . ? C12 O5 1.258(5) . ? C12 C13 1.401(6) . ? C13 C14 1.382(7) . ? C13 H13 0.9500 . ? C14 O6 1.259(5) . ? C14 C15 1.547(5) . ? C15 F18 1.319(6) . ? C15 F16 1.328(5) . ? C15 F17 1.333(5) . ? C16 F21 1.317(6) . ? C16 F20 1.328(8) . ? C16 F19 1.332(5) . ? C16 C17 1.538(6) . ? C17 O7 1.260(5) . ? C17 C18 1.392(6) . ? C18 C19 1.385(6) . ? C18 H18 0.9500 . ? C19 O8 1.257(5) . ? C19 C20 1.547(5) . ? C20 F24B 1.292(9) . ? C20 F23B 1.300(9) . ? C20 F22A 1.309(5) . ? C20 F24A 1.314(5) . ? C20 F23A 1.347(5) . ? C20 F22B 1.348(9) . ? C21 F27 1.329(5) . ? C21 F25 1.333(5) . ? C21 F26 1.338(6) . ? C21 C22 1.532(6) . ? C22 O9 1.256(5) . ? C22 C23 1.391(6) . ? C23 C24 1.398(6) . ? C23 H23 0.9500 . ? C24 O10 1.238(5) . ? C24 C25 1.529(6) . ? C25 F29B 1.262(8) . ? C25 F30A 1.267(5) . ? C25 F28A 1.323(6) . ? C25 F30B 1.335(8) . ? C25 F28B 1.341(8) . ? C25 F29A 1.344(6) . ? C26 F32 1.329(5) . ? C26 F33 1.333(5) . ? C26 F31 1.335(6) . ? C26 C27 1.530(6) . ? C27 O11 1.248(5) . ? C27 C28 1.404(5) . ? C28 C29 1.378(6) . ? C28 H28 0.9500 . ? C29 O12 1.256(5) . ? C29 C30 1.542(5) . ? C30 F34 1.318(6) . ? C30 F36 1.319(6) . ? C30 F35 1.333(5) . ? C31 N1 1.321(6) . ? C31 N2 1.339(5) . ? C31 H31 0.9500 . ? C32 C33 1.352(7) . ? C32 N2 1.365(6) . ? C32 H32 0.9500 . ? C33 N1 1.370(6) . ? C33 H33 0.9500 . ? C34 N1 1.461(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N2 1.477(6) . ? C35 C36 1.502(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.522(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.536(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 N4 1.316(7) . ? C39 N3 1.318(7) . ? C39 H39 0.9500 . ? C40 C41 1.334(9) . ? C40 N3 1.375(6) . ? C40 H40 0.9500 . ? C41 N4 1.394(6) . ? C41 H41 0.9500 . ? C42 N3 1.452(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44A 1.471(8) . ? C43 N4 1.475(8) . ? C43 C44B 1.540(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44A C45A 1.491(9) . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C45A C46A 1.499(9) . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A H46A 0.9800 . ? C46A H46B 0.9800 . ? C46A H46C 0.9800 . ? C44B C45B 1.500(10) . ? C44B H44C 0.9900 . ? C44B H44D 0.9900 . ? C45B C46B 1.494(10) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? C46B H46D 0.9800 . ? C46B H46E 0.9800 . ? C46B H46F 0.9800 . ? O1 Co1 2.073(3) . ? O2 Co1 2.053(3) . ? O3 Co1 2.073(3) . ? O4 Co1 2.067(3) . ? O5 Co1 2.082(3) . ? O6 Co1 2.065(3) . ? O7 Co2 2.047(3) . ? O8 Co2 2.068(2) . ? O9 Co2 2.052(3) . ? O10 Co2 2.087(3) . ? O11 Co2 2.076(3) . ? O12 Co2 2.073(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 F1 C1 F3 107.2(4) . . ? F1 C1 F2 107.3(3) . . ? F3 C1 F2 106.9(3) . . ? F1 C1 C2 112.7(3) . . ? F3 C1 C2 111.4(3) . . ? F2 C1 C2 111.0(4) . . ? O1 C2 C3 128.4(4) . . ? O1 C2 C1 115.0(4) . . ? C3 C2 C1 116.5(3) . . ? C2 C3 C4 122.6(4) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? O2 C4 C3 129.5(4) . . ? O2 C4 C5 112.8(4) . . ? C3 C4 C5 117.7(4) . . ? F4 C5 F6 107.1(5) . . ? F4 C5 F5 109.5(5) . . ? F6 C5 F5 105.4(4) . . ? F4 C5 C4 113.7(4) . . ? F6 C5 C4 111.0(4) . . ? F5 C5 C4 109.8(4) . . ? F8 C6 F9 107.8(4) . . ? F8 C6 F7 106.1(4) . . ? F9 C6 F7 105.8(4) . . ? F8 C6 C7 111.2(4) . . ? F9 C6 C7 114.4(4) . . ? F7 C6 C7 111.1(3) . . ? O3 C7 C8 129.2(4) . . ? O3 C7 C6 113.4(4) . . ? C8 C7 C6 117.4(4) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? O4 C9 C8 129.3(4) . . ? O4 C9 C10 113.5(4) . . ? C8 C9 C10 117.2(4) . . ? F12 C10 F10 110.2(6) . . ? F12 C10 F11 104.1(6) . . ? F10 C10 F11 105.0(4) . . ? F12 C10 C9 113.2(4) . . ? F10 C10 C9 114.7(5) . . ? F11 C10 C9 108.7(5) . . ? F13 C11 F14 106.6(4) . . ? F13 C11 F15 107.3(3) . . ? F14 C11 F15 106.0(3) . . ? F13 C11 C12 113.1(3) . . ? F14 C11 C12 110.6(3) . . ? F15 C11 C12 112.8(3) . . ? O5 C12 C13 128.2(4) . . ? O5 C12 C11 114.9(3) . . ? C13 C12 C11 116.9(3) . . ? C14 C13 C12 123.2(4) . . ? C14 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? O6 C14 C13 129.0(3) . . ? O6 C14 C15 113.4(4) . . ? C13 C14 C15 117.6(4) . . ? F18 C15 F16 107.9(4) . . ? F18 C15 F17 107.4(3) . . ? F16 C15 F17 107.2(3) . . ? F18 C15 C14 111.5(3) . . ? F16 C15 C14 110.2(3) . . ? F17 C15 C14 112.6(4) . . ? F21 C16 F20 110.0(5) . . ? F21 C16 F19 107.3(4) . . ? F20 C16 F19 105.4(5) . . ? F21 C16 C17 113.8(4) . . ? F20 C16 C17 109.7(4) . . ? F19 C16 C17 110.4(4) . . ? O7 C17 C18 128.7(4) . . ? O7 C17 C16 113.4(4) . . ? C18 C17 C16 117.9(4) . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? O8 C19 C18 129.7(3) . . ? O8 C19 C20 113.0(3) . . ? C18 C19 C20 117.2(3) . . ? F24B C20 F23B 110.9(12) . . ? F24B C20 F22A 127.8(10) . . ? F23B C20 F22A 58.5(10) . . ? F23B C20 F24A 134.3(9) . . ? F22A C20 F24A 109.9(4) . . ? F24B C20 F23A 68.4(11) . . ? F23B C20 F23A 50.6(10) . . ? F22A C20 F23A 105.9(4) . . ? F24A C20 F23A 104.4(4) . . ? F24B C20 F22B 105.1(11) . . ? F23B C20 F22B 104.4(11) . . ? F22A C20 F22B 46.8(10) . . ? F24A C20 F22B 71.4(10) . . ? F23A C20 F22B 141.9(8) . . ? F24B C20 C19 116.0(10) . . ? F23B C20 C19 112.6(9) . . ? F22A C20 C19 114.5(3) . . ? F24A C20 C19 112.0(3) . . ? F23A C20 C19 109.5(3) . . ? F22B C20 C19 106.8(8) . . ? F27 C21 F25 108.0(3) . . ? F27 C21 F26 107.0(3) . . ? F25 C21 F26 107.0(3) . . ? F27 C21 C22 110.9(3) . . ? F25 C21 C22 111.3(3) . . ? F26 C21 C22 112.4(3) . . ? O9 C22 C23 128.1(4) . . ? O9 C22 C21 114.7(3) . . ? C23 C22 C21 117.2(4) . . ? C22 C23 C24 122.6(4) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? O10 C24 C23 129.2(4) . . ? O10 C24 C25 114.5(4) . . ? C23 C24 C25 116.2(4) . . ? F29B C25 F30A 123.1(8) . . ? F30A C25 F28A 111.8(6) . . ? F29B C25 F30B 104.9(9) . . ? F30A C25 F30B 61.7(8) . . ? F28A C25 F30B 131.9(7) . . ? F29B C25 F28B 108.0(9) . . ? F28A C25 F28B 79.9(8) . . ? F30B C25 F28B 102.5(9) . . ? F29B C25 F29A 66.1(8) . . ? F30A C25 F29A 107.4(5) . . ? F28A C25 F29A 100.6(5) . . ? F30B C25 F29A 48.7(7) . . ? F28B C25 F29A 141.3(7) . . ? F29B C25 C24 120.6(7) . . ? F30A C25 C24 114.9(4) . . ? F28A C25 C24 112.5(4) . . ? F30B C25 C24 112.4(6) . . ? F28B C25 C24 106.8(6) . . ? F29A C25 C24 108.4(4) . . ? F32 C26 F33 106.8(4) . . ? F32 C26 F31 106.7(4) . . ? F33 C26 F31 107.3(4) . . ? F32 C26 C27 111.2(3) . . ? F33 C26 C27 113.8(3) . . ? F31 C26 C27 110.6(4) . . ? O11 C27 C28 128.8(4) . . ? O11 C27 C26 113.3(3) . . ? C28 C27 C26 117.9(3) . . ? C29 C28 C27 121.6(3) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? O12 C29 C28 129.2(3) . . ? O12 C29 C30 112.7(3) . . ? C28 C29 C30 118.1(3) . . ? F34 C30 F36 108.5(4) . . ? F34 C30 F35 106.3(4) . . ? F36 C30 F35 106.6(4) . . ? F34 C30 C29 111.3(4) . . ? F36 C30 C29 110.5(4) . . ? F35 C30 C29 113.5(3) . . ? N1 C31 N2 109.0(4) . . ? N1 C31 H31 125.5 . . ? N2 C31 H31 125.5 . . ? C33 C32 N2 107.1(4) . . ? C33 C32 H32 126.5 . . ? N2 C32 H32 126.5 . . ? C32 C33 N1 107.5(4) . . ? C32 C33 H33 126.2 . . ? N1 C33 H33 126.2 . . ? N1 C34 H34A 109.5 . . ? N1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 C36 112.6(3) . . ? N2 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? N2 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C35 C36 C37 111.9(4) . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C38 112.3(4) . . ? C36 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? C36 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.9 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 C39 N3 109.1(4) . . ? N4 C39 H39 125.5 . . ? N3 C39 H39 125.5 . . ? C41 C40 N3 107.3(5) . . ? C41 C40 H40 126.3 . . ? N3 C40 H40 126.3 . . ? C40 C41 N4 106.7(4) . . ? C40 C41 H41 126.6 . . ? N4 C41 H41 126.6 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44A C43 N4 119.9(6) . . ? N4 C43 C44B 103.5(7) . . ? C44A C43 H43A 107.3 . . ? N4 C43 H43A 107.3 . . ? C44B C43 H43A 135.0 . . ? C44A C43 H43B 107.3 . . ? N4 C43 H43B 107.3 . . ? C44B C43 H43B 94.0 . . ? H43A C43 H43B 106.9 . . ? C43 C44A C45A 114.7(8) . . ? C43 C44A H44A 108.6 . . ? C45A C44A H44A 108.6 . . ? C43 C44A H44B 108.6 . . ? C45A C44A H44B 108.6 . . ? H44A C44A H44B 107.6 . . ? C44A C45A C46A 116.4(9) . . ? C44A C45A H45A 108.2 . . ? C46A C45A H45A 108.2 . . ? C44A C45A H45B 108.2 . . ? C46A C45A H45B 108.2 . . ? H45A C45A H45B 107.3 . . ? C45B C44B C43 116.0(11) . . ? C45B C44B H44C 108.3 . . ? C43 C44B H44C 108.3 . . ? C45B C44B H44D 108.3 . . ? C43 C44B H44D 108.3 . . ? H44C C44B H44D 107.4 . . ? C46B C45B C44B 112.0(13) . . ? C46B C45B H45C 109.2 . . ? C44B C45B H45C 109.2 . . ? C46B C45B H45D 109.2 . . ? C44B C45B H45D 109.2 . . ? H45C C45B H45D 107.9 . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C31 N1 C33 108.2(4) . . ? C31 N1 C34 125.5(4) . . ? C33 N1 C34 126.3(4) . . ? C31 N2 C32 108.2(4) . . ? C31 N2 C35 125.6(4) . . ? C32 N2 C35 126.1(3) . . ? C39 N3 C40 108.7(5) . . ? C39 N3 C42 125.7(4) . . ? C40 N3 C42 125.6(5) . . ? C39 N4 C41 108.2(5) . . ? C39 N4 C43 125.6(5) . . ? C41 N4 C43 126.2(5) . . ? C2 O1 Co1 125.1(3) . . ? C4 O2 Co1 124.9(3) . . ? C7 O3 Co1 125.1(3) . . ? C9 O4 Co1 124.4(3) . . ? C12 O5 Co1 122.9(3) . . ? C14 O6 Co1 123.2(3) . . ? C17 O7 Co2 126.0(3) . . ? C19 O8 Co2 125.0(2) . . ? C22 O9 Co2 124.8(2) . . ? C24 O10 Co2 123.4(3) . . ? C27 O11 Co2 124.7(3) . . ? C29 O12 Co2 124.2(2) . . ? O2 Co1 O6 177.55(11) . . ? O2 Co1 O4 93.29(11) . . ? O6 Co1 O4 88.94(11) . . ? O2 Co1 O3 92.73(11) . . ? O6 Co1 O3 88.37(11) . . ? O4 Co1 O3 87.70(12) . . ? O2 Co1 O1 88.31(11) . . ? O6 Co1 O1 89.42(11) . . ? O4 Co1 O1 176.95(11) . . ? O3 Co1 O1 94.82(12) . . ? O2 Co1 O5 90.74(11) . . ? O6 Co1 O5 88.46(11) . . ? O4 Co1 O5 84.55(12) . . ? O3 Co1 O5 171.68(11) . . ? O1 Co1 O5 92.83(11) . . ? O7 Co2 O9 176.93(12) . . ? O7 Co2 O8 87.59(11) . . ? O9 Co2 O8 90.94(11) . . ? O7 Co2 O12 91.00(11) . . ? O9 Co2 O12 90.57(11) . . ? O8 Co2 O12 177.48(13) . . ? O7 Co2 O11 96.60(12) . . ? O9 Co2 O11 86.12(12) . . ? O8 Co2 O11 91.03(11) . . ? O12 Co2 O11 87.06(11) . . ? O7 Co2 O10 89.33(12) . . ? O9 Co2 O10 88.18(12) . . ? O8 Co2 O10 97.12(11) . . ? O12 Co2 O10 84.94(11) . . ? O11 Co2 O10 170.12(10) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 70.07 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.028 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.093 # Attachment 'wg202_fin.cif' data_wg202 _database_code_depnum_ccdc_archive 'CCDC 742063' #TrackingRef 'wg202_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H3 Cu F18 O6, C8 H15 N2 ' _chemical_formula_sum 'C23 H18 Cu F18 N2 O6' _chemical_formula_weight 823.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0624(2) _cell_length_b 17.4690(3) _cell_length_c 20.1946(4) _cell_angle_alpha 73.5270(10) _cell_angle_beta 86.2880(10) _cell_angle_gamma 89.1060(10) _cell_volume 3059.36(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9691 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 70.95 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_absorpt_coefficient_mu 2.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.693 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43008 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 70.98 _reflns_number_total 11449 _reflns_number_gt 9555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0545P)^2^+2.1446P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11449 _refine_ls_number_parameters 999 _refine_ls_number_restraints 288 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.071 _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 C1 C -0.1634(3) 0.00658(15) 0.35199(13) 0.0259(5) Uani 1 1 d DU . . C2 C -0.0959(2) 0.05347(13) 0.28027(12) 0.0179(4) Uani 1 1 d . B . C3 C -0.1004(3) 0.01840(14) 0.22676(14) 0.0225(5) Uani 1 1 d . . . H3 H -0.1269 -0.0363 0.2366 0.027 Uiso 1 1 calc R B . C4 C -0.0662(3) 0.06290(15) 0.15899(14) 0.0217(5) Uani 1 1 d . B . C5 C -0.0937(4) 0.02623(19) 0.10016(16) 0.0356(7) Uani 1 1 d . . . C6 C -0.2637(3) 0.40519(16) 0.16323(14) 0.0270(5) Uani 1 1 d . . . C7 C -0.1290(3) 0.35264(14) 0.15505(13) 0.0215(5) Uani 1 1 d . B . C8 C -0.0101(3) 0.39032(14) 0.10867(13) 0.0242(5) Uani 1 1 d . . . H8 H -0.0124 0.4466 0.0891 0.029 Uiso 1 1 calc R . . C9 C 0.1078(3) 0.34860(14) 0.09103(12) 0.0206(5) Uani 1 1 d . B . C10 C 0.2266(3) 0.39467(16) 0.03738(14) 0.0272(5) Uani 1 1 d . . . C11 C 0.5345(3) 0.13679(17) 0.18197(17) 0.0365(6) Uani 1 1 d DU . . C12 C 0.3851(3) 0.16670(14) 0.20567(13) 0.0215(5) Uani 1 1 d . B . C13 C 0.3945(3) 0.22975(14) 0.23589(14) 0.0250(5) Uani 1 1 d . . . H13 H 0.4897 0.2481 0.2416 0.030 Uiso 1 1 calc R C . C14 C 0.2715(3) 0.26623(13) 0.25757(12) 0.0201(5) Uani 1 1 d . B . C15 C 0.3020(3) 0.33600(15) 0.28716(14) 0.0253(5) Uani 1 1 d . . . C16 C 0.4560(3) 0.54942(16) 0.35854(16) 0.0277(5) Uani 1 1 d . . . C17 C 0.3105(3) 0.59423(14) 0.33859(13) 0.0214(5) Uani 1 1 d . . . C18 C 0.1940(3) 0.55124(14) 0.32220(14) 0.0240(5) Uani 1 1 d . . . H18 H 0.2044 0.4953 0.3298 0.029 Uiso 1 1 calc R . . C19 C 0.0665(3) 0.58737(15) 0.29574(13) 0.0234(5) Uani 1 1 d . . . C20 C -0.0523(3) 0.53325(17) 0.28105(18) 0.0345(6) Uani 1 1 d . . . C21 C -0.1468(3) 0.61270(15) 0.49059(14) 0.0267(5) Uani 1 1 d . . . C22 C -0.1142(3) 0.67906(14) 0.42242(13) 0.0207(5) Uani 1 1 d . . . C23 C -0.2336(3) 0.71397(14) 0.38668(14) 0.0229(5) Uani 1 1 d . . . H23 H -0.3299 0.6960 0.4054 0.027 Uiso 1 1 calc R . . C24 C -0.2200(3) 0.77515(14) 0.32357(13) 0.0200(5) Uani 1 1 d . . . C25 C -0.3666(3) 0.80372(15) 0.29005(14) 0.0234(5) Uani 1 1 d . . . C26 C 0.3039(4) 0.89772(19) 0.12787(16) 0.0381(7) Uani 1 1 d . . . C27 C 0.2513(3) 0.86925(15) 0.20455(14) 0.0238(5) Uani 1 1 d . . . C28 C 0.2694(3) 0.91968(15) 0.24533(15) 0.0281(6) Uani 1 1 d . . . H28 H 0.3021 0.9729 0.2241 0.034 Uiso 1 1 calc R . . C29 C 0.2410(3) 0.89441(14) 0.31639(14) 0.0211(5) Uani 1 1 d . . . C30 C 0.2846(3) 0.95223(15) 0.35730(15) 0.0264(5) Uani 1 1 d . . . C31 C -0.0681(3) 0.78176(16) 0.02082(15) 0.0304(6) Uani 1 1 d . A . H31 H -0.0217 0.7915 -0.0243 0.037 Uiso 1 1 calc R . . C32 C -0.2327(4) 0.77634(18) 0.10580(16) 0.0379(7) Uani 1 1 d . . . H32 H -0.3232 0.7817 0.1305 0.045 Uiso 1 1 calc R . . C33 C -0.1078(4) 0.74525(19) 0.13332(15) 0.0411(7) Uani 1 1 d . A . H33 H -0.0930 0.7246 0.1812 0.049 Uiso 1 1 calc R . . C34 C -0.3132(4) 0.8347(2) -0.01573(17) 0.0442(8) Uani 1 1 d . . . H34A H -0.2633 0.8494 -0.0621 0.066 Uiso 1 1 calc R . . H34B H -0.3557 0.8826 -0.0059 0.066 Uiso 1 1 calc R . . H34C H -0.3921 0.7962 -0.0134 0.066 Uiso 1 1 calc R . . C35A C 0.1552(7) 0.7251(4) 0.0823(6) 0.0401(16) Uani 0.690(8) 1 d PDU A 1 H35A H 0.1902 0.7277 0.1271 0.048 Uiso 0.690(8) 1 calc PR A 1 H35B H 0.2132 0.7644 0.0451 0.048 Uiso 0.690(8) 1 calc PR A 1 C36A C 0.1860(7) 0.6424(4) 0.0748(4) 0.0547(14) Uani 0.690(8) 1 d PDU A 1 H36A H 0.1330 0.6026 0.1137 0.066 Uiso 0.690(8) 1 calc PR A 1 H36B H 0.1464 0.6386 0.0313 0.066 Uiso 0.690(8) 1 calc PR A 1 C37A C 0.3485(8) 0.6220(6) 0.0741(5) 0.0600(19) Uani 0.690(8) 1 d PDU A 1 H37A H 0.3612 0.5703 0.0635 0.072 Uiso 0.690(8) 1 calc PR A 1 H37B H 0.4014 0.6631 0.0363 0.072 Uiso 0.690(8) 1 calc PR A 1 C38A C 0.4195(6) 0.6166(4) 0.1409(4) 0.0588(16) Uani 0.690(8) 1 d PDU A 1 H38A H 0.4171 0.6691 0.1495 0.088 Uiso 0.690(8) 1 calc PR A 1 H38B H 0.5224 0.5992 0.1374 0.088 Uiso 0.690(8) 1 calc PR A 1 H38C H 0.3652 0.5779 0.1791 0.088 Uiso 0.690(8) 1 calc PR A 1 C35B C 0.1370(15) 0.7077(8) 0.0914(17) 0.049(3) Uani 0.310(8) 1 d PDU A 2 H35C H 0.1742 0.7141 0.1345 0.059 Uiso 0.310(8) 1 calc PR A 2 H35D H 0.2095 0.7329 0.0528 0.059 Uiso 0.310(8) 1 calc PR A 2 C36B C 0.1262(13) 0.6206(7) 0.0973(7) 0.042(2) Uani 0.310(8) 1 d PDU A 2 H36C H 0.1065 0.6134 0.0518 0.050 Uiso 0.310(8) 1 calc PR A 2 H36D H 0.0432 0.5965 0.1306 0.050 Uiso 0.310(8) 1 calc PR A 2 C37B C 0.2685(12) 0.5796(7) 0.1214(7) 0.056(2) Uani 0.310(8) 1 d PDU A 2 H37C H 0.2844 0.5844 0.1681 0.067 Uiso 0.310(8) 1 calc PR A 2 H37D H 0.2601 0.5221 0.1250 0.067 Uiso 0.310(8) 1 calc PR A 2 C38B C 0.3988(15) 0.6139(14) 0.0738(12) 0.065(5) Uani 0.310(8) 1 d PDU A 2 H38D H 0.3721 0.6248 0.0257 0.098 Uiso 0.310(8) 1 calc PR A 2 H38E H 0.4807 0.5757 0.0820 0.098 Uiso 0.310(8) 1 calc PR A 2 H38F H 0.4292 0.6637 0.0823 0.098 Uiso 0.310(8) 1 calc PR A 2 C39 C 0.8463(3) 0.24022(16) 0.48010(14) 0.0264(5) Uani 1 1 d . . . H39 H 0.8649 0.2187 0.5276 0.032 Uiso 1 1 calc R . . C40 C 0.7549(3) 0.31265(17) 0.38413(14) 0.0301(6) Uani 1 1 d . . . H40 H 0.6978 0.3510 0.3531 0.036 Uiso 1 1 calc R . . C41 C 0.8542(3) 0.26184(17) 0.36729(14) 0.0298(6) Uani 1 1 d . . . H41 H 0.8805 0.2578 0.3221 0.036 Uiso 1 1 calc R . . C42 C 0.6657(3) 0.3431(2) 0.49532(17) 0.0369(6) Uani 1 1 d . . . H42A H 0.6671 0.3147 0.5447 0.055 Uiso 1 1 calc R . . H42B H 0.5634 0.3482 0.4816 0.055 Uiso 1 1 calc R . . H42C H 0.7088 0.3964 0.4867 0.055 Uiso 1 1 calc R . . C43 C 1.0284(3) 0.15647(15) 0.43378(14) 0.0266(5) Uani 1 1 d . . . H43A H 1.0546 0.1496 0.3875 0.032 Uiso 1 1 calc R . . H43B H 0.9909 0.1047 0.4643 0.032 Uiso 1 1 calc R . . C44 C 1.1659(3) 0.17976(15) 0.46266(14) 0.0266(5) Uani 1 1 d . . . H44A H 1.1449 0.1760 0.5122 0.032 Uiso 1 1 calc R . . H44B H 1.1918 0.2359 0.4380 0.032 Uiso 1 1 calc R . . C45 C 1.2970(3) 0.12620(17) 0.45507(15) 0.0329(6) Uani 1 1 d . . . H45A H 1.2721 0.0703 0.4810 0.039 Uiso 1 1 calc R . . H45B H 1.3154 0.1285 0.4057 0.039 Uiso 1 1 calc R . . C46 C 1.4365(4) 0.1505(2) 0.48144(19) 0.0459(8) Uani 1 1 d . . . H46A H 1.4643 0.2050 0.4545 0.069 Uiso 1 1 calc R . . H46B H 1.5167 0.1138 0.4766 0.069 Uiso 1 1 calc R . . H46C H 1.4188 0.1486 0.5303 0.069 Uiso 1 1 calc R . . Cu1 Cu 0.05020(4) 0.195883(19) 0.195355(17) 0.01811(10) Uani 1 1 d . B . Cu2 Cu 0.11453(4) 0.744504(19) 0.315164(18) 0.01976(10) Uani 1 1 d . . . F1A F -0.2438(4) 0.05454(13) 0.38086(13) 0.0527(7) Uani 0.892(5) 1 d PDU B 1 F2A F -0.0597(3) -0.0210(2) 0.39595(14) 0.0647(10) Uani 0.892(5) 1 d PDU B 1 F3A F -0.2485(3) -0.05291(15) 0.35128(13) 0.0438(6) Uani 0.892(5) 1 d PDU B 1 F1B F -0.150(2) 0.0355(10) 0.4024(7) 0.042(2) Uani 0.108(5) 1 d PDU B 2 F2B F -0.0792(18) -0.0603(8) 0.3709(9) 0.040(3) Uani 0.108(5) 1 d PDU B 2 F3B F -0.2925(15) -0.0217(13) 0.3485(11) 0.044(3) Uani 0.108(5) 1 d PDU B 2 F4 F -0.2084(3) 0.06198(19) 0.06578(13) 0.0655(7) Uani 1 1 d . B . F5 F -0.1191(3) -0.05158(13) 0.12182(12) 0.0671(8) Uani 1 1 d U B . F6 F 0.0208(2) 0.03845(12) 0.05431(11) 0.0464(5) Uani 1 1 d . B . F7 F -0.3726(2) 0.39100(14) 0.12719(14) 0.0562(6) Uani 1 1 d . . . F8 F -0.2363(2) 0.48278(10) 0.14157(10) 0.0382(4) Uani 1 1 d . . . F9 F -0.3146(3) 0.38835(13) 0.22880(11) 0.0556(6) Uani 1 1 d . . . F10 F 0.2009(2) 0.47299(10) 0.01525(10) 0.0401(4) Uani 1 1 d . . . F11 F 0.3581(2) 0.38606(15) 0.06328(12) 0.0557(6) Uani 1 1 d . . . F12 F 0.2359(3) 0.36812(11) -0.01824(10) 0.0484(5) Uani 1 1 d . . . F13A F 0.5851(3) 0.1884(2) 0.12168(18) 0.0609(10) Uani 0.803(7) 1 d PDU C 1 F14A F 0.6376(4) 0.1375(3) 0.2254(3) 0.0591(11) Uani 0.803(7) 1 d PDU C 1 F15A F 0.5286(4) 0.0662(2) 0.1727(3) 0.0594(10) Uani 0.803(7) 1 d PDU C 1 F13B F 0.5450(14) 0.1446(10) 0.1147(4) 0.059(2) Uani 0.197(7) 1 d PDU C 2 F14B F 0.6566(12) 0.1590(9) 0.1991(8) 0.045(2) Uani 0.197(7) 1 d PDU C 2 F15B F 0.5310(15) 0.0559(5) 0.2084(8) 0.043(2) Uani 0.197(7) 1 d PDU C 2 F16 F 0.18893(19) 0.34780(9) 0.32900(9) 0.0321(3) Uani 1 1 d . C . F17 F 0.3229(2) 0.40347(9) 0.23679(10) 0.0401(4) Uani 1 1 d . C . F18 F 0.4214(2) 0.32353(11) 0.32453(11) 0.0426(4) Uani 1 1 d . C . F19 F 0.4887(3) 0.54984(15) 0.42223(14) 0.0636(7) Uani 1 1 d . . . F20 F 0.5670(2) 0.58501(12) 0.31638(17) 0.0666(8) Uani 1 1 d . . . F21 F 0.45546(18) 0.47376(9) 0.35883(10) 0.0338(4) Uani 1 1 d . . . F22 F 0.0019(3) 0.47445(16) 0.2588(2) 0.0818(10) Uani 1 1 d . . . F23 F -0.1493(2) 0.57248(12) 0.23909(13) 0.0518(5) Uani 1 1 d . . . F24 F -0.1337(3) 0.49833(18) 0.34040(15) 0.0793(9) Uani 1 1 d . . . F25 F -0.1426(3) 0.54145(10) 0.47881(11) 0.0485(5) Uani 1 1 d . . . F26 F -0.2798(2) 0.61978(13) 0.52019(10) 0.0481(5) Uani 1 1 d . . . F27 F -0.0498(2) 0.61213(11) 0.53683(9) 0.0378(4) Uani 1 1 d . . . F28 F -0.47690(18) 0.80500(10) 0.33691(9) 0.0335(4) Uani 1 1 d . . . F29 F -0.35489(19) 0.87681(9) 0.24604(10) 0.0376(4) Uani 1 1 d . . . F30 F -0.40787(18) 0.75524(10) 0.25397(9) 0.0321(3) Uani 1 1 d . . . F31 F 0.1959(3) 0.89245(13) 0.08793(10) 0.0494(5) Uani 1 1 d . . . F32 F 0.3503(4) 0.97284(15) 0.10809(12) 0.0755(9) Uani 1 1 d . . . F33 F 0.4128(2) 0.85114(16) 0.11421(11) 0.0566(6) Uani 1 1 d . . . F34 F 0.2459(3) 0.92503(10) 0.42460(9) 0.0466(5) Uani 1 1 d . . . F35 F 0.2203(2) 1.02282(9) 0.33430(9) 0.0337(4) Uani 1 1 d . . . F36 F 0.4292(2) 0.96488(15) 0.35107(15) 0.0606(7) Uani 1 1 d . . . N1 N -0.2067(3) 0.79915(14) 0.03521(12) 0.0311(5) Uani 1 1 d . . . N2 N -0.0038(3) 0.74861(14) 0.07933(13) 0.0341(5) Uani 1 1 d D . . N3 N 0.7520(2) 0.29845(14) 0.45488(12) 0.0256(4) Uani 1 1 d . . . N4 N 0.9105(2) 0.21689(13) 0.42806(11) 0.0242(4) Uani 1 1 d . . . O1 O -0.04529(18) 0.12043(9) 0.27835(9) 0.0190(3) Uani 1 1 d . . . O2 O -0.0199(2) 0.13384(10) 0.13673(9) 0.0221(3) Uani 1 1 d . . . O3 O -0.1418(2) 0.28162(10) 0.18846(10) 0.0251(4) Uani 1 1 d . . . O4 O 0.1365(2) 0.27442(10) 0.11103(9) 0.0224(3) Uani 1 1 d . . . O5 O 0.27422(19) 0.13337(10) 0.19467(9) 0.0214(3) Uani 1 1 d . . . O6 O 0.13550(19) 0.25324(10) 0.25494(9) 0.0213(3) Uani 1 1 d . . . O7 O 0.3123(2) 0.66518(10) 0.33842(10) 0.0236(4) Uani 1 1 d . . . O8 O 0.0295(2) 0.66012(10) 0.28073(9) 0.0245(4) Uani 1 1 d . . . O9 O 0.02322(19) 0.69179(10) 0.40796(9) 0.0221(3) Uani 1 1 d . . . O10 O -0.10623(19) 0.80779(10) 0.29109(9) 0.0234(4) Uani 1 1 d . . . O11 O 0.1985(2) 0.79957(10) 0.22184(9) 0.0234(4) Uani 1 1 d . . . O12 O 0.18758(19) 0.82895(10) 0.35288(9) 0.0215(3) 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 C1 0.0278(12) 0.0247(11) 0.0236(12) -0.0046(9) 0.0006(9) -0.0075(9) C2 0.0145(10) 0.0170(10) 0.0204(11) -0.0022(8) -0.0033(8) 0.0020(8) C3 0.0215(12) 0.0172(10) 0.0300(13) -0.0088(9) 0.0000(10) -0.0025(9) C4 0.0171(11) 0.0248(12) 0.0273(13) -0.0141(10) -0.0006(9) -0.0014(9) C5 0.0398(16) 0.0418(16) 0.0323(15) -0.0232(13) 0.0069(12) -0.0131(13) C6 0.0258(13) 0.0291(13) 0.0239(13) -0.0039(10) -0.0019(10) 0.0041(10) C7 0.0256(12) 0.0204(11) 0.0184(11) -0.0043(9) -0.0071(9) 0.0020(9) C8 0.0277(13) 0.0184(11) 0.0240(12) -0.0016(9) -0.0045(10) -0.0009(9) C9 0.0246(12) 0.0204(11) 0.0163(11) -0.0032(9) -0.0048(9) -0.0032(9) C10 0.0296(13) 0.0258(12) 0.0231(13) -0.0019(10) 0.0002(10) -0.0039(10) C11 0.0224(12) 0.0343(12) 0.0598(16) -0.0244(12) -0.0030(11) 0.0025(10) C12 0.0204(12) 0.0200(11) 0.0225(12) -0.0034(9) -0.0017(9) 0.0018(9) C13 0.0236(12) 0.0196(11) 0.0336(14) -0.0102(10) -0.0035(10) -0.0021(9) C14 0.0250(12) 0.0179(10) 0.0168(11) -0.0038(8) -0.0011(9) -0.0026(9) C15 0.0268(13) 0.0229(12) 0.0278(13) -0.0100(10) -0.0002(10) -0.0022(10) C16 0.0215(12) 0.0254(12) 0.0397(15) -0.0154(11) 0.0005(11) -0.0031(10) C17 0.0233(12) 0.0195(11) 0.0211(12) -0.0063(9) 0.0043(9) -0.0009(9) C18 0.0244(12) 0.0190(11) 0.0299(13) -0.0093(9) -0.0007(10) -0.0003(9) C19 0.0259(12) 0.0220(11) 0.0237(12) -0.0094(9) 0.0018(10) -0.0003(9) C20 0.0316(14) 0.0244(13) 0.0516(18) -0.0150(12) -0.0166(13) 0.0076(11) C21 0.0264(13) 0.0246(12) 0.0255(13) -0.0013(10) -0.0014(10) -0.0022(10) C22 0.0238(12) 0.0181(10) 0.0205(12) -0.0062(9) 0.0005(9) -0.0016(9) C23 0.0216(12) 0.0217(11) 0.0243(12) -0.0053(9) 0.0014(9) -0.0026(9) C24 0.0200(11) 0.0175(10) 0.0248(12) -0.0095(9) -0.0024(9) 0.0015(9) C25 0.0227(12) 0.0212(11) 0.0253(13) -0.0049(9) -0.0022(10) -0.0024(9) C26 0.0497(18) 0.0375(15) 0.0235(14) -0.0021(11) -0.0022(13) -0.0111(14) C27 0.0235(12) 0.0213(11) 0.0232(13) 0.0000(9) -0.0039(10) 0.0006(9) C28 0.0320(14) 0.0197(11) 0.0298(14) -0.0002(10) -0.0106(11) -0.0049(10) C29 0.0158(11) 0.0179(11) 0.0311(13) -0.0087(9) -0.0068(9) 0.0038(8) C30 0.0261(13) 0.0209(11) 0.0349(15) -0.0105(10) -0.0113(11) 0.0046(9) C31 0.0412(16) 0.0298(13) 0.0228(13) -0.0117(10) -0.0003(11) -0.0043(11) C32 0.0544(19) 0.0377(15) 0.0210(14) -0.0090(11) 0.0052(13) -0.0024(13) C33 0.069(2) 0.0359(15) 0.0183(13) -0.0073(11) -0.0040(14) 0.0026(14) C34 0.0449(18) 0.059(2) 0.0257(15) -0.0079(14) -0.0029(13) 0.0088(15) C35A 0.051(3) 0.038(3) 0.040(4) -0.022(3) -0.015(3) 0.003(2) C36A 0.046(3) 0.056(3) 0.077(4) -0.043(3) -0.002(3) 0.004(2) C37A 0.040(4) 0.071(4) 0.088(4) -0.054(3) 0.006(3) 0.005(3) C38A 0.042(3) 0.052(3) 0.083(4) -0.022(3) 0.002(3) 0.010(2) C35B 0.055(5) 0.051(6) 0.049(6) -0.023(5) -0.017(5) 0.018(5) C36B 0.049(5) 0.039(5) 0.045(5) -0.024(4) -0.004(4) 0.012(4) C37B 0.045(5) 0.059(5) 0.070(5) -0.029(4) -0.004(4) 0.013(4) C38B 0.036(8) 0.074(8) 0.088(8) -0.027(7) 0.002(7) 0.017(7) C39 0.0280(13) 0.0309(13) 0.0220(12) -0.0098(10) -0.0023(10) -0.0038(10) C40 0.0285(13) 0.0378(14) 0.0232(13) -0.0074(11) -0.0015(10) 0.0003(11) C41 0.0337(14) 0.0363(14) 0.0185(12) -0.0066(10) -0.0014(10) 0.0000(11) C42 0.0308(15) 0.0513(17) 0.0354(16) -0.0234(13) -0.0021(12) 0.0065(13) C43 0.0355(14) 0.0247(12) 0.0212(12) -0.0090(9) -0.0015(10) 0.0007(10) C44 0.0351(14) 0.0223(11) 0.0228(12) -0.0067(9) -0.0035(10) -0.0002(10) C45 0.0377(15) 0.0329(14) 0.0270(14) -0.0068(11) -0.0026(11) 0.0047(11) C46 0.0372(17) 0.057(2) 0.0419(18) -0.0107(15) -0.0093(14) 0.0061(14) Cu1 0.02151(18) 0.01673(17) 0.01623(18) -0.00478(12) -0.00121(13) -0.00171(12) Cu2 0.02261(19) 0.01738(17) 0.01996(19) -0.00684(13) 0.00116(13) -0.00094(13) F1A 0.0853(19) 0.0340(10) 0.0345(12) -0.0098(9) 0.0309(12) -0.0042(10) F2A 0.0391(12) 0.091(2) 0.0368(13) 0.0291(14) -0.0106(9) -0.0169(11) F3A 0.0580(14) 0.0385(12) 0.0363(11) -0.0160(10) 0.0179(10) -0.0285(11) F1B 0.060(6) 0.042(5) 0.024(4) -0.009(3) 0.009(4) -0.019(4) F2B 0.045(5) 0.037(4) 0.024(5) 0.009(4) 0.009(5) 0.006(4) F3B 0.032(4) 0.051(7) 0.041(6) -0.002(6) 0.002(5) -0.020(4) F4 0.0531(13) 0.114(2) 0.0500(13) -0.0540(14) -0.0171(10) 0.0008(13) F5 0.114(2) 0.0479(12) 0.0485(12) -0.0338(10) 0.0272(13) -0.0454(13) F6 0.0598(12) 0.0450(10) 0.0429(11) -0.0310(8) 0.0219(9) -0.0147(9) F7 0.0315(10) 0.0632(13) 0.0837(16) -0.0320(12) -0.0287(10) 0.0145(9) F8 0.0442(10) 0.0260(8) 0.0417(10) -0.0073(7) 0.0038(8) 0.0099(7) F9 0.0579(13) 0.0611(12) 0.0329(10) 0.0054(9) 0.0160(9) 0.0293(10) F10 0.0485(10) 0.0234(8) 0.0415(10) -0.0005(7) 0.0100(8) -0.0077(7) F11 0.0255(9) 0.0742(14) 0.0493(12) 0.0123(10) -0.0027(8) -0.0121(9) F12 0.0745(14) 0.0400(9) 0.0292(9) -0.0117(7) 0.0207(9) -0.0186(9) F13A 0.0440(15) 0.0616(17) 0.0718(17) -0.0168(14) 0.0264(13) 0.0022(13) F14A 0.0307(16) 0.066(2) 0.095(3) -0.0431(19) -0.0244(18) 0.0183(14) F15A 0.0355(14) 0.0481(14) 0.114(3) -0.0591(18) 0.017(2) -0.0051(12) F13B 0.044(4) 0.076(5) 0.062(3) -0.033(3) 0.004(3) 0.020(4) F14B 0.016(3) 0.042(4) 0.089(5) -0.040(4) 0.011(4) -0.006(3) F15B 0.027(4) 0.029(2) 0.083(5) -0.035(3) 0.015(5) 0.001(3) F16 0.0389(9) 0.0306(8) 0.0314(8) -0.0178(6) 0.0052(7) -0.0046(7) F17 0.0603(12) 0.0200(7) 0.0391(10) -0.0096(7) 0.0111(8) -0.0103(7) F18 0.0385(10) 0.0452(10) 0.0564(12) -0.0316(9) -0.0168(8) 0.0013(8) F19 0.0618(14) 0.0792(15) 0.0734(16) -0.0531(13) -0.0431(12) 0.0391(12) F20 0.0279(10) 0.0378(10) 0.115(2) 0.0030(11) 0.0240(11) 0.0033(8) F21 0.0304(8) 0.0229(7) 0.0512(10) -0.0138(7) -0.0097(7) 0.0045(6) F22 0.0454(12) 0.0714(15) 0.169(3) -0.0914(19) -0.0476(16) 0.0241(11) F23 0.0467(11) 0.0402(10) 0.0735(14) -0.0180(9) -0.0321(10) 0.0036(8) F24 0.0775(18) 0.0874(18) 0.0638(16) -0.0017(13) -0.0135(13) -0.0543(16) F25 0.0780(14) 0.0209(8) 0.0425(11) -0.0016(7) -0.0061(10) -0.0064(8) F26 0.0300(9) 0.0610(12) 0.0348(10) 0.0136(9) 0.0100(7) 0.0032(8) F27 0.0379(9) 0.0445(9) 0.0238(8) 0.0034(7) -0.0062(7) -0.0085(7) F28 0.0232(8) 0.0416(9) 0.0345(9) -0.0096(7) -0.0004(6) 0.0087(6) F29 0.0288(8) 0.0242(7) 0.0502(10) 0.0075(7) -0.0127(7) -0.0027(6) F30 0.0322(8) 0.0368(8) 0.0296(8) -0.0118(7) -0.0051(6) -0.0080(7) F31 0.0646(13) 0.0536(11) 0.0260(9) -0.0018(8) -0.0157(9) -0.0014(10) F32 0.132(2) 0.0529(13) 0.0319(11) 0.0046(9) 0.0044(13) -0.0515(15) F33 0.0429(11) 0.0894(16) 0.0311(10) -0.0101(10) 0.0130(8) 0.0000(11) F34 0.0859(15) 0.0285(8) 0.0285(9) -0.0090(7) -0.0216(9) -0.0063(9) F35 0.0499(10) 0.0214(7) 0.0325(8) -0.0112(6) -0.0089(7) 0.0091(7) F36 0.0257(9) 0.0711(14) 0.111(2) -0.0660(14) -0.0121(10) -0.0016(9) N1 0.0446(14) 0.0299(11) 0.0189(11) -0.0077(9) 0.0015(10) -0.0036(10) N2 0.0524(16) 0.0292(11) 0.0258(12) -0.0147(9) -0.0095(11) 0.0020(10) N3 0.0211(10) 0.0334(11) 0.0246(11) -0.0120(9) -0.0008(8) -0.0038(9) N4 0.0275(11) 0.0269(10) 0.0191(10) -0.0077(8) -0.0018(8) -0.0047(8) O1 0.0206(8) 0.0185(8) 0.0180(8) -0.0050(6) -0.0027(6) -0.0009(6) O2 0.0260(9) 0.0232(8) 0.0193(8) -0.0090(6) -0.0030(7) -0.0020(7) O3 0.0238(9) 0.0216(8) 0.0272(9) -0.0025(7) -0.0011(7) -0.0021(7) O4 0.0270(9) 0.0199(8) 0.0186(8) -0.0031(6) 0.0004(7) 0.0009(7) O5 0.0222(8) 0.0193(8) 0.0234(9) -0.0069(6) -0.0030(7) -0.0003(6) O6 0.0228(9) 0.0212(8) 0.0217(8) -0.0092(6) -0.0003(7) -0.0026(6) O7 0.0239(9) 0.0199(8) 0.0287(9) -0.0104(7) 0.0021(7) -0.0010(7) O8 0.0295(9) 0.0197(8) 0.0264(9) -0.0094(7) -0.0058(7) 0.0023(7) O9 0.0206(8) 0.0241(8) 0.0206(8) -0.0051(6) -0.0004(6) -0.0008(6) O10 0.0222(9) 0.0198(8) 0.0268(9) -0.0045(7) 0.0003(7) 0.0008(6) O11 0.0280(9) 0.0199(8) 0.0220(9) -0.0062(6) 0.0021(7) -0.0011(7) O12 0.0222(8) 0.0186(8) 0.0249(9) -0.0088(6) 0.0008(7) -0.0002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F1B 1.272(9) . ? C1 F3B 1.290(9) . ? C1 F3A 1.308(3) . ? C1 F2A 1.325(4) . ? C1 F1A 1.332(3) . ? C1 F2B 1.361(9) . ? C1 C2 1.540(3) . ? C2 O1 1.252(3) . ? C2 C3 1.388(4) . ? C3 C4 1.386(4) . ? C3 H3 0.9500 . ? C4 O2 1.261(3) . ? C4 C5 1.536(4) . ? C5 F6 1.323(4) . ? C5 F5 1.323(4) . ? C5 F4 1.334(5) . ? C6 F8 1.323(3) . ? C6 F9 1.325(4) . ? C6 F7 1.330(4) . ? C6 C7 1.544(4) . ? C7 O3 1.236(3) . ? C7 C8 1.419(4) . ? C8 C9 1.369(4) . ? C8 H8 0.9500 . ? C9 O4 1.271(3) . ? C9 C10 1.536(3) . ? C10 F11 1.322(4) . ? C10 F12 1.329(4) . ? C10 F10 1.335(3) . ? C11 F14B 1.278(8) . ? C11 F15A 1.301(4) . ? C11 F13B 1.323(8) . ? C11 F14A 1.325(4) . ? C11 F13A 1.350(4) . ? C11 F15B 1.361(8) . ? C11 C12 1.540(4) . ? C12 O5 1.233(3) . ? C12 C13 1.408(4) . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C14 O6 1.264(3) . ? C14 C15 1.537(3) . ? C15 F17 1.327(3) . ? C15 F16 1.336(3) . ? C15 F18 1.339(3) . ? C16 F20 1.316(4) . ? C16 F21 1.320(3) . ? C16 F19 1.340(4) . ? C16 C17 1.540(4) . ? C17 O7 1.239(3) . ? C17 C18 1.414(4) . ? C18 C19 1.373(4) . ? C18 H18 0.9500 . ? C19 O8 1.265(3) . ? C19 C20 1.540(4) . ? C20 F23 1.308(4) . ? C20 F22 1.310(4) . ? C20 F24 1.356(5) . ? C21 F27 1.321(3) . ? C21 F26 1.331(4) . ? C21 F25 1.331(4) . ? C21 C22 1.543(3) . ? C22 O9 1.269(3) . ? C22 C23 1.376(4) . ? C23 C24 1.412(4) . ? C23 H23 0.9500 . ? C24 O10 1.239(3) . ? C24 C25 1.542(3) . ? C25 F29 1.334(3) . ? C25 F30 1.335(3) . ? C25 F28 1.336(3) . ? C26 F32 1.325(4) . ? C26 F31 1.329(4) . ? C26 F33 1.334(5) . ? C26 C27 1.532(4) . ? C27 O11 1.260(3) . ? C27 C28 1.384(4) . ? C28 C29 1.385(4) . ? C28 H28 0.9500 . ? C29 O12 1.256(3) . ? C29 C30 1.545(3) . ? C30 F36 1.324(3) . ? C30 F35 1.328(3) . ? C30 F34 1.331(4) . ? C31 N1 1.321(4) . ? C31 N2 1.327(4) . ? C31 H31 0.9500 . ? C32 C33 1.332(5) . ? C32 N1 1.373(4) . ? C32 H32 0.9500 . ? C33 N2 1.383(5) . ? C33 H33 0.9500 . ? C34 N1 1.457(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35A N2 1.493(6) . ? C35A C36A 1.515(7) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C36A C37A 1.510(7) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A C38A 1.510(8) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C35B N2 1.453(9) . ? C35B C36B 1.496(10) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36B C37B 1.506(9) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B C38B 1.492(10) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39 N3 1.326(4) . ? C39 N4 1.329(4) . ? C39 H39 0.9500 . ? C40 C41 1.349(4) . ? C40 N3 1.378(4) . ? C40 H40 0.9500 . ? C41 N4 1.380(4) . ? C41 H41 0.9500 . ? C42 N3 1.466(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 N4 1.477(4) . ? C43 C44 1.518(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.528(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.515(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? Cu1 O2 1.9560(17) . ? Cu1 O6 1.9692(17) . ? Cu1 O1 1.9724(16) . ? Cu1 O4 1.9824(17) . ? Cu1 O3 2.2631(19) . ? Cu1 O5 2.2913(18) . ? Cu2 O11 1.9660(18) . ? Cu2 O9 1.9721(17) . ? Cu2 O12 1.9819(17) . ? Cu2 O8 1.9841(17) . ? Cu2 O7 2.2394(19) . ? Cu2 O10 2.2833(18) . ? 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 F1B C1 F3B 115.5(12) . . ? F1B C1 F3A 126.9(7) . . ? F1B C1 F2A 60.1(10) . . ? F3B C1 F2A 130.4(10) . . ? F3A C1 F2A 108.5(3) . . ? F3B C1 F1A 81.7(11) . . ? F3A C1 F1A 107.4(2) . . ? F2A C1 F1A 104.0(3) . . ? F1B C1 F2B 101.1(10) . . ? F3B C1 F2B 102.8(11) . . ? F3A C1 F2B 73.9(9) . . ? F1A C1 F2B 139.6(8) . . ? F1B C1 C2 118.0(7) . . ? F3B C1 C2 112.0(10) . . ? F3A C1 C2 114.3(2) . . ? F2A C1 C2 111.5(2) . . ? F1A C1 C2 110.6(2) . . ? F2B C1 C2 104.7(7) . . ? O1 C2 C3 128.5(2) . . ? O1 C2 C1 113.8(2) . . ? C3 C2 C1 117.7(2) . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? O2 C4 C3 128.7(2) . . ? O2 C4 C5 112.3(2) . . ? C3 C4 C5 118.9(2) . . ? F6 C5 F5 107.6(3) . . ? F6 C5 F4 106.0(3) . . ? F5 C5 F4 108.8(3) . . ? F6 C5 C4 110.9(2) . . ? F5 C5 C4 113.3(3) . . ? F4 C5 C4 109.9(3) . . ? F8 C6 F9 107.4(2) . . ? F8 C6 F7 107.1(2) . . ? F9 C6 F7 107.3(3) . . ? F8 C6 C7 114.1(2) . . ? F9 C6 C7 111.0(2) . . ? F7 C6 C7 109.7(2) . . ? O3 C7 C8 128.2(2) . . ? O3 C7 C6 114.8(2) . . ? C8 C7 C6 116.9(2) . . ? C9 C8 C7 122.4(2) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? O4 C9 C8 130.2(2) . . ? O4 C9 C10 111.6(2) . . ? C8 C9 C10 118.2(2) . . ? F11 C10 F12 107.6(3) . . ? F11 C10 F10 106.8(2) . . ? F12 C10 F10 106.7(2) . . ? F11 C10 C9 110.9(2) . . ? F12 C10 C9 110.9(2) . . ? F10 C10 C9 113.5(2) . . ? F14B C11 F15A 118.0(8) . . ? F14B C11 F13B 108.6(8) . . ? F15A C11 F13B 71.3(7) . . ? F15A C11 F14A 109.3(3) . . ? F13B C11 F14A 130.9(6) . . ? F14B C11 F13A 78.9(7) . . ? F15A C11 F13A 107.9(4) . . ? F14A C11 F13A 104.4(3) . . ? F14B C11 F15B 105.6(9) . . ? F13B C11 F15B 101.3(8) . . ? F14A C11 F15B 87.4(7) . . ? F13A C11 F15B 135.3(7) . . ? F14B C11 C12 121.2(7) . . ? F15A C11 C12 114.0(3) . . ? F13B C11 C12 112.2(5) . . ? F14A C11 C12 111.5(3) . . ? F13A C11 C12 109.2(2) . . ? F15B C11 C12 105.8(6) . . ? O5 C12 C13 128.9(2) . . ? O5 C12 C11 116.0(2) . . ? C13 C12 C11 115.1(2) . . ? C14 C13 C12 123.0(2) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? O6 C14 C13 130.2(2) . . ? O6 C14 C15 113.6(2) . . ? C13 C14 C15 116.1(2) . . ? F17 C15 F16 107.3(2) . . ? F17 C15 F18 107.9(2) . . ? F16 C15 F18 106.5(2) . . ? F17 C15 C14 110.9(2) . . ? F16 C15 C14 111.6(2) . . ? F18 C15 C14 112.4(2) . . ? F20 C16 F21 107.8(2) . . ? F20 C16 F19 106.4(3) . . ? F21 C16 F19 106.1(2) . . ? F20 C16 C17 110.5(2) . . ? F21 C16 C17 114.8(2) . . ? F19 C16 C17 110.8(2) . . ? O7 C17 C18 128.2(2) . . ? O7 C17 C16 114.2(2) . . ? C18 C17 C16 117.6(2) . . ? C19 C18 C17 122.4(2) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? O8 C19 C18 129.8(2) . . ? O8 C19 C20 113.1(2) . . ? C18 C19 C20 117.0(2) . . ? F23 C20 F22 109.7(3) . . ? F23 C20 F24 104.1(3) . . ? F22 C20 F24 105.6(3) . . ? F23 C20 C19 113.3(2) . . ? F22 C20 C19 113.8(3) . . ? F24 C20 C19 109.5(3) . . ? F27 C21 F26 106.8(2) . . ? F27 C21 F25 107.7(2) . . ? F26 C21 F25 107.0(2) . . ? F27 C21 C22 112.3(2) . . ? F26 C21 C22 112.6(2) . . ? F25 C21 C22 110.2(2) . . ? O9 C22 C23 130.2(2) . . ? O9 C22 C21 112.6(2) . . ? C23 C22 C21 117.3(2) . . ? C22 C23 C24 123.3(2) . . ? C22 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? O10 C24 C23 128.8(2) . . ? O10 C24 C25 115.9(2) . . ? C23 C24 C25 115.3(2) . . ? F29 C25 F30 106.9(2) . . ? F29 C25 F28 107.6(2) . . ? F30 C25 F28 107.3(2) . . ? F29 C25 C24 112.1(2) . . ? F30 C25 C24 110.5(2) . . ? F28 C25 C24 112.3(2) . . ? F32 C26 F31 107.1(3) . . ? F32 C26 F33 108.9(3) . . ? F31 C26 F33 106.3(3) . . ? F32 C26 C27 113.1(3) . . ? F31 C26 C27 110.9(3) . . ? F33 C26 C27 110.2(3) . . ? O11 C27 C28 128.8(2) . . ? O11 C27 C26 112.7(2) . . ? C28 C27 C26 118.5(2) . . ? C27 C28 C29 121.6(2) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? O12 C29 C28 128.4(2) . . ? O12 C29 C30 114.9(2) . . ? C28 C29 C30 116.7(2) . . ? F36 C30 F35 107.1(2) . . ? F36 C30 F34 107.3(2) . . ? F35 C30 F34 107.1(2) . . ? F36 C30 C29 111.2(2) . . ? F35 C30 C29 111.2(2) . . ? F34 C30 C29 112.6(2) . . ? N1 C31 N2 109.4(3) . . ? N1 C31 H31 125.3 . . ? N2 C31 H31 125.3 . . ? C33 C32 N1 107.5(3) . . ? C33 C32 H32 126.2 . . ? N1 C32 H32 126.2 . . ? C32 C33 N2 107.5(3) . . ? C32 C33 H33 126.3 . . ? N2 C33 H33 126.3 . . ? N1 C34 H34A 109.5 . . ? N1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35A C36A 114.3(5) . . ? N2 C35A H35A 108.7 . . ? C36A C35A H35A 108.7 . . ? N2 C35A H35B 108.7 . . ? C36A C35A H35B 108.7 . . ? H35A C35A H35B 107.6 . . ? C37A C36A C35A 113.1(6) . . ? C37A C36A H36A 109.0 . . ? C35A C36A H36A 109.0 . . ? C37A C36A H36B 109.0 . . ? C35A C36A H36B 109.0 . . ? H36A C36A H36B 107.8 . . ? C38A C37A C36A 114.6(6) . . ? C38A C37A H37A 108.6 . . ? C36A C37A H37A 108.6 . . ? C38A C37A H37B 108.6 . . ? C36A C37A H37B 108.6 . . ? H37A C37A H37B 107.6 . . ? N2 C35B C36B 112.8(10) . . ? N2 C35B H35C 109.0 . . ? C36B C35B H35C 109.0 . . ? N2 C35B H35D 109.0 . . ? C36B C35B H35D 109.0 . . ? H35C C35B H35D 107.8 . . ? C35B C36B C37B 109.9(9) . . ? C35B C36B H36C 109.7 . . ? C37B C36B H36C 109.7 . . ? C35B C36B H36D 109.7 . . ? C37B C36B H36D 109.7 . . ? H36C C36B H36D 108.2 . . ? C38B C37B C36B 112.4(10) . . ? C38B C37B H37C 109.1 . . ? C36B C37B H37C 109.1 . . ? C38B C37B H37D 109.1 . . ? C36B C37B H37D 109.1 . . ? H37C C37B H37D 107.8 . . ? C37B C38B H38D 109.5 . . ? C37B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? N3 C39 N4 108.8(2) . . ? N3 C39 H39 125.6 . . ? N4 C39 H39 125.6 . . ? C41 C40 N3 107.0(2) . . ? C41 C40 H40 126.5 . . ? N3 C40 H40 126.5 . . ? C40 C41 N4 107.1(2) . . ? C40 C41 H41 126.4 . . ? N4 C41 H41 126.4 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 C43 C44 112.1(2) . . ? N4 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? N4 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C43 C44 C45 111.8(2) . . ? C43 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 107.9 . . ? C46 C45 C44 112.4(3) . . ? C46 C45 H45A 109.1 . . ? C44 C45 H45A 109.1 . . ? C46 C45 H45B 109.1 . . ? C44 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O2 Cu1 O6 175.38(8) . . ? O2 Cu1 O1 90.80(7) . . ? O6 Cu1 O1 89.40(7) . . ? O2 Cu1 O4 88.84(7) . . ? O6 Cu1 O4 91.19(7) . . ? O1 Cu1 O4 177.13(7) . . ? O2 Cu1 O3 98.57(7) . . ? O6 Cu1 O3 86.04(7) . . ? O1 Cu1 O3 91.33(7) . . ? O4 Cu1 O3 85.91(7) . . ? O2 Cu1 O5 88.68(7) . . ? O6 Cu1 O5 86.72(7) . . ? O1 Cu1 O5 98.40(7) . . ? O4 Cu1 O5 84.43(7) . . ? O3 Cu1 O5 167.80(6) . . ? O11 Cu2 O9 177.75(8) . . ? O11 Cu2 O12 91.61(7) . . ? O9 Cu2 O12 88.28(7) . . ? O11 Cu2 O8 90.95(8) . . ? O9 Cu2 O8 89.06(8) . . ? O12 Cu2 O8 176.43(8) . . ? O11 Cu2 O7 92.23(7) . . ? O9 Cu2 O7 90.02(7) . . ? O12 Cu2 O7 96.05(7) . . ? O8 Cu2 O7 86.34(7) . . ? O11 Cu2 O10 90.80(7) . . ? O9 Cu2 O10 86.96(7) . . ? O12 Cu2 O10 92.31(7) . . ? O8 Cu2 O10 85.17(7) . . ? O7 Cu2 O10 171.02(6) . . ? C31 N1 C32 108.2(3) . . ? C31 N1 C34 125.3(3) . . ? C32 N1 C34 126.5(3) . . ? C31 N2 C33 107.5(3) . . ? C31 N2 C35B 130.6(14) . . ? C33 N2 C35B 121.0(13) . . ? C31 N2 C35A 123.6(5) . . ? C33 N2 C35A 128.8(5) . . ? C39 N3 C40 108.7(2) . . ? C39 N3 C42 125.4(2) . . ? C40 N3 C42 125.8(2) . . ? C39 N4 C41 108.4(2) . . ? C39 N4 C43 125.8(2) . . ? C41 N4 C43 125.7(2) . . ? C2 O1 Cu1 124.71(16) . . ? C4 O2 Cu1 124.25(16) . . ? C7 O3 Cu1 121.45(17) . . ? C9 O4 Cu1 126.48(17) . . ? C12 O5 Cu1 118.79(16) . . ? C14 O6 Cu1 125.83(16) . . ? C17 O7 Cu2 122.46(17) . . ? C19 O8 Cu2 126.85(17) . . ? C22 O9 Cu2 125.18(16) . . ? C24 O10 Cu2 118.36(15) . . ? C27 O11 Cu2 124.22(17) . . ? C29 O12 Cu2 124.21(17) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 70.98 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.724 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.092 # Attachment 'wg197_fin.cif' data_wg197 _database_code_depnum_ccdc_archive 'CCDC 742064' #TrackingRef 'wg197_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H43 N2, C5 H F6 O2' _chemical_formula_sum 'C27 H44 F6 N2 O2' _chemical_formula_weight 542.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0727 .0534 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7419(2) _cell_length_b 9.9974(2) _cell_length_c 37.1893(7) _cell_angle_alpha 93.9900(10) _cell_angle_beta 91.6070(10) _cell_angle_gamma 91.1070(10) _cell_volume 2869.65(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7264 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 71.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43326 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 71.61 _reflns_number_total 11016 _reflns_number_gt 8955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0709P)^2^+0.4450P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11016 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1 C -0.2896(2) 0.7270(2) 0.03282(4) 0.0319(4) Uani 1 1 d . . . H1A H -0.4145 0.7203 0.0362 0.048 Uiso 1 1 calc R . . H1B H -0.2492 0.6420 0.0217 0.048 Uiso 1 1 calc R . . H1C H -0.2648 0.7993 0.0171 0.048 Uiso 1 1 calc R . . C2 C -0.27287(18) 0.79784(14) 0.09847(4) 0.0175(3) Uani 1 1 d . . . H2 H -0.3932 0.8085 0.1018 0.021 Uiso 1 1 calc R . . C3 C 0.00886(18) 0.79477(14) 0.10864(4) 0.0195(3) Uani 1 1 d . . . H3 H 0.1191 0.8031 0.1205 0.023 Uiso 1 1 calc R . . C4 C -0.02420(18) 0.75339(15) 0.07354(4) 0.0215(3) Uani 1 1 d . . . H4 H 0.0587 0.7275 0.0562 0.026 Uiso 1 1 calc R . . C5 C -0.17814(18) 0.87930(14) 0.16084(4) 0.0181(3) Uani 1 1 d . . . H5A H -0.3001 0.8625 0.1668 0.022 Uiso 1 1 calc R . . H5B H -0.1578 0.9776 0.1620 0.022 Uiso 1 1 calc R . . C6 C -0.06027(19) 0.81893(15) 0.18864(4) 0.0202(3) Uani 1 1 d . . . H6A H 0.0615 0.8429 0.1841 0.024 Uiso 1 1 calc R . . H6B H -0.0729 0.7200 0.1861 0.024 Uiso 1 1 calc R . . C7 C -0.10380(19) 0.86962(15) 0.22708(4) 0.0208(3) Uani 1 1 d . . . H7A H -0.0810 0.9676 0.2303 0.025 Uiso 1 1 calc R . . H7B H -0.2282 0.8529 0.2309 0.025 Uiso 1 1 calc R . . C8 C 0.0037(2) 0.79948(16) 0.25500(4) 0.0228(3) Uani 1 1 d . . . H8A H -0.0043 0.7016 0.2489 0.027 Uiso 1 1 calc R . . H8B H 0.1263 0.8276 0.2531 0.027 Uiso 1 1 calc R . . C9 C -0.04853(19) 0.82676(15) 0.29400(4) 0.0225(3) Uani 1 1 d . . . H9A H -0.1703 0.7975 0.2964 0.027 Uiso 1 1 calc R . . H9B H -0.0401 0.9244 0.3006 0.027 Uiso 1 1 calc R . . C10 C 0.06629(19) 0.75336(16) 0.31989(4) 0.0229(3) Uani 1 1 d . . . H10A H 0.0613 0.6563 0.3124 0.028 Uiso 1 1 calc R . . H10B H 0.1873 0.7851 0.3178 0.028 Uiso 1 1 calc R . . C11 C 0.0168(2) 0.77247(16) 0.35926(4) 0.0241(3) Uani 1 1 d . . . H11A H -0.1038 0.7399 0.3615 0.029 Uiso 1 1 calc R . . H11B H 0.0213 0.8694 0.3668 0.029 Uiso 1 1 calc R . . C12 C 0.1346(2) 0.69870(16) 0.38450(4) 0.0238(3) Uani 1 1 d . . . H12A H 0.1301 0.6018 0.3768 0.029 Uiso 1 1 calc R . . H12B H 0.2550 0.7313 0.3822 0.029 Uiso 1 1 calc R . . C13 C 0.0864(2) 0.71700(16) 0.42392(4) 0.0248(3) Uani 1 1 d . . . H13A H -0.0337 0.6836 0.4263 0.030 Uiso 1 1 calc R . . H13B H 0.0898 0.8140 0.4315 0.030 Uiso 1 1 calc R . . C14 C 0.2050(2) 0.64450(16) 0.44922(4) 0.0242(3) Uani 1 1 d . . . H14A H 0.2013 0.5475 0.4418 0.029 Uiso 1 1 calc R . . H14B H 0.3252 0.6777 0.4468 0.029 Uiso 1 1 calc R . . C15 C 0.1565(2) 0.66377(16) 0.48859(4) 0.0249(3) Uani 1 1 d . . . H15A H 0.0364 0.6303 0.4909 0.030 Uiso 1 1 calc R . . H15B H 0.1595 0.7609 0.4960 0.030 Uiso 1 1 calc R . . C16 C 0.2751(2) 0.59202(16) 0.51423(4) 0.0245(3) Uani 1 1 d . . . H16A H 0.2719 0.4948 0.5070 0.029 Uiso 1 1 calc R . . H16B H 0.3953 0.6253 0.5119 0.029 Uiso 1 1 calc R . . C17 C 0.2250(2) 0.61266(16) 0.55353(4) 0.0248(3) Uani 1 1 d . . . H17A H 0.1048 0.5792 0.5558 0.030 Uiso 1 1 calc R . . H17B H 0.2277 0.7100 0.5607 0.030 Uiso 1 1 calc R . . C18 C 0.3428(2) 0.54192(16) 0.57948(4) 0.0244(3) Uani 1 1 d . . . H18A H 0.3404 0.4446 0.5724 0.029 Uiso 1 1 calc R . . H18B H 0.4629 0.5757 0.5774 0.029 Uiso 1 1 calc R . . C19 C 0.2903(2) 0.56315(16) 0.61865(4) 0.0259(3) Uani 1 1 d . . . H19A H 0.1702 0.5291 0.6206 0.031 Uiso 1 1 calc R . . H19B H 0.2917 0.6606 0.6256 0.031 Uiso 1 1 calc R . . C20 C 0.4066(2) 0.49408(17) 0.64514(4) 0.0273(3) Uani 1 1 d . . . H20A H 0.4057 0.3966 0.6382 0.033 Uiso 1 1 calc R . . H20B H 0.5266 0.5285 0.6434 0.033 Uiso 1 1 calc R . . C21 C 0.3511(3) 0.51593(19) 0.68392(4) 0.0351(4) Uani 1 1 d . . . H21A H 0.2316 0.4804 0.6856 0.042 Uiso 1 1 calc R . . H21B H 0.3501 0.6135 0.6906 0.042 Uiso 1 1 calc R . . C22 C 0.4677(3) 0.4492(2) 0.71077(5) 0.0483(5) Uani 1 1 d . . . H22A H 0.4691 0.3524 0.7044 0.072 Uiso 1 1 calc R . . H22B H 0.4238 0.4654 0.7351 0.072 Uiso 1 1 calc R . . H22C H 0.5853 0.4867 0.7101 0.072 Uiso 1 1 calc R . . C23 C 0.33664(19) 1.01517(15) 0.06575(4) 0.0222(3) Uani 1 1 d . . . H23A H 0.4549 1.0343 0.0586 0.033 Uiso 1 1 calc R . . H23B H 0.2548 1.0598 0.0502 0.033 Uiso 1 1 calc R . . H23C H 0.3139 0.9181 0.0633 0.033 Uiso 1 1 calc R . . C24 C 0.44289(18) 1.08680(14) 0.12824(4) 0.0169(3) Uani 1 1 d . . . H24 H 0.5625 1.0748 0.1244 0.020 Uiso 1 1 calc R . . C25 C 0.19676(18) 1.13279(15) 0.15423(4) 0.0206(3) Uani 1 1 d . . . H25 H 0.1156 1.1587 0.1720 0.025 Uiso 1 1 calc R . . C26 C 0.16071(18) 1.09337(14) 0.11917(4) 0.0201(3) Uani 1 1 d . . . H26 H 0.0496 1.0865 0.1076 0.024 Uiso 1 1 calc R . . C27 C 0.46728(18) 1.16044(15) 0.19398(4) 0.0202(3) Uani 1 1 d . . . H27A H 0.4371 1.2517 0.2035 0.024 Uiso 1 1 calc R . . H27B H 0.5932 1.1601 0.1900 0.024 Uiso 1 1 calc R . . C28 C 0.42410(18) 1.06087(15) 0.22176(4) 0.0197(3) Uani 1 1 d . . . H28A H 0.4625 0.9705 0.2133 0.024 Uiso 1 1 calc R . . H28B H 0.2974 1.0563 0.2246 0.024 Uiso 1 1 calc R . . C29 C 0.51333(19) 1.10347(15) 0.25804(4) 0.0211(3) Uani 1 1 d . . . H29A H 0.6396 1.1097 0.2547 0.025 Uiso 1 1 calc R . . H29B H 0.4741 1.1939 0.2662 0.025 Uiso 1 1 calc R . . C30 C 0.4781(2) 1.00782(15) 0.28732(4) 0.0225(3) Uani 1 1 d . . . H30A H 0.5203 0.9178 0.2795 0.027 Uiso 1 1 calc R . . H30B H 0.3518 0.9998 0.2904 0.027 Uiso 1 1 calc R . . C31 C 0.5650(2) 1.05439(15) 0.32356(4) 0.0226(3) Uani 1 1 d . . . H31A H 0.5198 1.1431 0.3316 0.027 Uiso 1 1 calc R . . H31B H 0.6907 1.0657 0.3202 0.027 Uiso 1 1 calc R . . C32 C 0.5369(2) 0.95800(16) 0.35312(4) 0.0235(3) Uani 1 1 d . . . H32A H 0.4113 0.9474 0.3568 0.028 Uiso 1 1 calc R . . H32B H 0.5813 0.8690 0.3451 0.028 Uiso 1 1 calc R . . C33 C 0.6263(2) 1.00591(16) 0.38898(4) 0.0238(3) Uani 1 1 d . . . H33A H 0.7514 1.0189 0.3851 0.029 Uiso 1 1 calc R . . H33B H 0.5797 1.0939 0.3973 0.029 Uiso 1 1 calc R . . C34 C 0.6029(2) 0.90868(16) 0.41843(4) 0.0241(3) Uani 1 1 d . . . H34A H 0.6482 0.8204 0.4100 0.029 Uiso 1 1 calc R . . H34B H 0.4779 0.8966 0.4225 0.029 Uiso 1 1 calc R . . C35 C 0.6941(2) 0.95568(16) 0.45418(4) 0.0245(3) Uani 1 1 d . . . H35A H 0.6482 1.0437 0.4627 0.029 Uiso 1 1 calc R . . H35B H 0.8190 0.9684 0.4501 0.029 Uiso 1 1 calc R . . C36 C 0.6717(2) 0.85784(16) 0.48360(4) 0.0241(3) Uani 1 1 d . . . H36A H 0.5468 0.8450 0.4876 0.029 Uiso 1 1 calc R . . H36B H 0.7176 0.7698 0.4751 0.029 Uiso 1 1 calc R . . C37 C 0.7624(2) 0.90459(16) 0.51932(4) 0.0242(3) Uani 1 1 d . . . H37A H 0.7169 0.9928 0.5278 0.029 Uiso 1 1 calc R . . H37B H 0.8874 0.9169 0.5153 0.029 Uiso 1 1 calc R . . C38 C 0.7392(2) 0.80719(16) 0.54872(4) 0.0241(3) Uani 1 1 d . . . H38A H 0.7854 0.7192 0.5403 0.029 Uiso 1 1 calc R . . H38B H 0.6142 0.7944 0.5526 0.029 Uiso 1 1 calc R . . C39 C 0.8292(2) 0.85434(16) 0.58462(4) 0.0239(3) Uani 1 1 d . . . H39A H 0.9543 0.8665 0.5807 0.029 Uiso 1 1 calc R . . H39B H 0.7837 0.9427 0.5929 0.029 Uiso 1 1 calc R . . C40 C 0.8051(2) 0.75769(16) 0.61422(4) 0.0238(3) Uani 1 1 d . . . H40A H 0.8517 0.6695 0.6061 0.029 Uiso 1 1 calc R . . H40B H 0.6800 0.7449 0.6180 0.029 Uiso 1 1 calc R . . C41 C 0.8942(2) 0.80664(16) 0.65005(4) 0.0239(3) Uani 1 1 d . . . H41A H 1.0193 0.8193 0.6462 0.029 Uiso 1 1 calc R . . H41B H 0.8479 0.8951 0.6580 0.029 Uiso 1 1 calc R . . C42 C 0.8713(2) 0.71183(16) 0.68002(4) 0.0248(3) Uani 1 1 d . . . H42A H 0.9175 0.6232 0.6721 0.030 Uiso 1 1 calc R . . H42B H 0.7464 0.6995 0.6841 0.030 Uiso 1 1 calc R . . C43 C 0.9617(2) 0.76204(17) 0.71551(4) 0.0287(3) Uani 1 1 d . . . H43A H 1.0862 0.7762 0.7112 0.034 Uiso 1 1 calc R . . H43B H 0.9141 0.8500 0.7235 0.034 Uiso 1 1 calc R . . C44 C 0.9433(3) 0.6679(2) 0.74556(5) 0.0381(4) Uani 1 1 d . . . H44A H 0.8206 0.6548 0.7504 0.057 Uiso 1 1 calc R . . H44B H 1.0040 0.7068 0.7674 0.057 Uiso 1 1 calc R . . H44C H 0.9934 0.5813 0.7382 0.057 Uiso 1 1 calc R . . C45 C 0.7921(2) 0.20955(18) 0.02694(4) 0.0295(3) Uani 1 1 d . . . C46 C 0.78992(18) 0.18938(15) 0.06776(4) 0.0210(3) Uani 1 1 d . . . C47 C 0.81373(19) 0.30430(15) 0.09144(4) 0.0231(3) Uani 1 1 d . . . H47 H 0.8227 0.3895 0.0817 0.028 Uiso 1 1 calc R . . C48 C 0.82472(17) 0.29729(14) 0.12897(4) 0.0198(3) Uani 1 1 d . . . C49 C 0.8636(2) 0.42968(16) 0.15167(4) 0.0270(3) Uani 1 1 d . . . C50 C 0.3219(2) 0.45474(16) 0.06196(4) 0.0272(3) Uani 1 1 d . . . C51 C 0.35266(18) 0.58003(15) 0.08827(4) 0.0214(3) Uani 1 1 d . . . C52 C 0.37274(19) 0.55798(15) 0.12496(4) 0.0231(3) Uani 1 1 d . . . H52 H 0.3724 0.4684 0.1320 0.028 Uiso 1 1 calc R . . C53 C 0.39332(17) 0.66338(15) 0.15168(4) 0.0195(3) Uani 1 1 d . . . C54 C 0.41536(19) 0.62264(16) 0.19091(4) 0.0227(3) Uani 1 1 d . . . N1 N -0.20042(15) 0.75600(13) 0.06791(3) 0.0198(2) Uani 1 1 d . . . N2 N -0.14861(15) 0.82248(11) 0.12375(3) 0.0166(2) Uani 1 1 d . . . N3 N 0.31609(15) 1.06511(12) 0.10349(3) 0.0179(2) Uani 1 1 d . . . N4 N 0.37357(15) 1.12813(12) 0.15926(3) 0.0176(2) Uani 1 1 d . . . O1 O 0.76958(14) 0.07093(11) 0.07482(3) 0.0262(2) Uani 1 1 d . . . O2 O 0.81210(13) 0.19824(10) 0.14712(3) 0.0212(2) Uani 1 1 d . . . O3 O 0.35453(13) 0.68692(10) 0.07326(3) 0.0212(2) Uani 1 1 d . . . O4 O 0.39691(13) 0.78651(10) 0.14893(3) 0.0220(2) Uani 1 1 d . . . F1 F 0.80608(16) 0.33684(12) 0.01855(3) 0.0445(3) Uani 1 1 d . . . F2 F 0.64763(15) 0.15845(13) 0.01037(3) 0.0451(3) Uani 1 1 d . . . F3 F 0.92420(17) 0.14520(15) 0.01180(3) 0.0539(3) Uani 1 1 d . . . F4 F 1.02683(15) 0.43605(13) 0.16352(4) 0.0512(3) Uani 1 1 d . . . F5 F 0.77183(18) 0.43775(13) 0.18134(4) 0.0535(3) Uani 1 1 d . . . F6 F 0.8292(3) 0.53826(12) 0.13478(4) 0.0738(5) Uani 1 1 d . . . F7 F 0.17084(14) 0.46104(12) 0.04394(3) 0.0421(3) Uani 1 1 d . . . F8 F 0.44409(15) 0.44621(12) 0.03728(3) 0.0419(3) Uani 1 1 d . . . F9 F 0.3211(2) 0.33841(11) 0.07747(3) 0.0561(4) Uani 1 1 d . . . F10 F 0.40909(15) 0.49094(11) 0.19462(3) 0.0379(2) Uani 1 1 d . . . F11 F 0.56808(14) 0.66715(11) 0.20499(3) 0.0372(2) Uani 1 1 d . . . F12 F 0.29514(17) 0.67612(16) 0.21157(3) 0.0581(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0260(7) 0.0551(11) 0.0138(7) -0.0008(7) -0.0019(6) -0.0040(7) C2 0.0191(6) 0.0175(7) 0.0164(6) 0.0048(5) -0.0006(5) 0.0006(5) C3 0.0193(6) 0.0213(7) 0.0183(7) 0.0043(5) -0.0008(5) 0.0002(5) C4 0.0204(7) 0.0260(8) 0.0184(7) 0.0031(5) 0.0020(5) 0.0003(5) C5 0.0214(6) 0.0187(7) 0.0141(6) 0.0008(5) -0.0013(5) 0.0023(5) C6 0.0240(7) 0.0218(7) 0.0146(6) 0.0001(5) -0.0023(5) 0.0034(5) C7 0.0248(7) 0.0218(7) 0.0154(7) -0.0004(5) -0.0018(5) 0.0024(5) C8 0.0274(7) 0.0275(8) 0.0137(7) 0.0015(5) -0.0008(6) 0.0032(6) C9 0.0267(7) 0.0254(7) 0.0151(7) 0.0010(5) -0.0013(6) 0.0016(6) C10 0.0252(7) 0.0285(8) 0.0151(7) 0.0021(5) -0.0009(5) -0.0004(6) C11 0.0291(7) 0.0273(8) 0.0160(7) 0.0030(6) -0.0014(6) -0.0006(6) C12 0.0260(7) 0.0286(8) 0.0170(7) 0.0047(6) -0.0024(6) -0.0027(6) C13 0.0313(8) 0.0259(8) 0.0173(7) 0.0036(6) -0.0018(6) -0.0014(6) C14 0.0273(7) 0.0282(8) 0.0171(7) 0.0053(6) -0.0021(6) -0.0043(6) C15 0.0317(8) 0.0264(8) 0.0169(7) 0.0043(6) -0.0020(6) -0.0015(6) C16 0.0277(7) 0.0282(8) 0.0178(7) 0.0056(6) -0.0022(6) -0.0045(6) C17 0.0304(8) 0.0266(8) 0.0175(7) 0.0040(6) -0.0029(6) -0.0011(6) C18 0.0267(7) 0.0279(8) 0.0187(7) 0.0057(6) -0.0041(6) -0.0039(6) C19 0.0329(8) 0.0267(8) 0.0182(7) 0.0038(6) -0.0030(6) -0.0018(6) C20 0.0311(8) 0.0299(8) 0.0211(7) 0.0072(6) -0.0053(6) -0.0064(6) C21 0.0497(10) 0.0362(9) 0.0193(8) 0.0065(6) -0.0049(7) -0.0062(7) C22 0.0645(13) 0.0538(13) 0.0272(9) 0.0186(8) -0.0164(9) -0.0145(10) C23 0.0276(7) 0.0249(7) 0.0137(6) 0.0004(5) -0.0004(5) -0.0009(5) C24 0.0197(6) 0.0158(6) 0.0157(6) 0.0047(5) -0.0003(5) 0.0003(5) C25 0.0206(7) 0.0224(7) 0.0195(7) 0.0052(5) 0.0017(5) 0.0039(5) C26 0.0199(6) 0.0215(7) 0.0196(7) 0.0051(5) -0.0018(5) 0.0028(5) C27 0.0236(7) 0.0230(7) 0.0140(6) 0.0031(5) -0.0026(5) -0.0022(5) C28 0.0232(7) 0.0223(7) 0.0138(6) 0.0026(5) -0.0007(5) 0.0008(5) C29 0.0249(7) 0.0244(7) 0.0141(6) 0.0036(5) -0.0017(5) -0.0004(5) C30 0.0286(7) 0.0249(7) 0.0144(7) 0.0044(5) -0.0018(6) -0.0004(6) C31 0.0282(7) 0.0257(8) 0.0144(7) 0.0055(5) -0.0019(6) -0.0016(6) C32 0.0302(7) 0.0267(8) 0.0139(7) 0.0048(6) -0.0020(6) -0.0011(6) C33 0.0302(8) 0.0273(8) 0.0141(7) 0.0055(5) -0.0026(6) -0.0019(6) C34 0.0319(8) 0.0262(8) 0.0145(7) 0.0060(6) -0.0029(6) -0.0022(6) C35 0.0314(8) 0.0274(8) 0.0148(7) 0.0055(6) -0.0029(6) -0.0027(6) C36 0.0321(8) 0.0257(8) 0.0147(7) 0.0042(6) -0.0021(6) -0.0025(6) C37 0.0309(8) 0.0279(8) 0.0140(7) 0.0054(6) -0.0028(6) -0.0025(6) C38 0.0325(8) 0.0255(8) 0.0145(7) 0.0052(6) -0.0034(6) -0.0018(6) C39 0.0300(8) 0.0274(8) 0.0144(7) 0.0050(5) -0.0036(6) -0.0031(6) C40 0.0316(8) 0.0247(8) 0.0153(7) 0.0044(5) -0.0031(6) -0.0016(6) C41 0.0290(7) 0.0278(8) 0.0152(7) 0.0046(6) -0.0031(6) -0.0024(6) C42 0.0313(8) 0.0281(8) 0.0152(7) 0.0052(6) -0.0018(6) -0.0008(6) C43 0.0342(8) 0.0344(9) 0.0176(7) 0.0055(6) -0.0050(6) -0.0012(6) C44 0.0511(11) 0.0455(11) 0.0187(8) 0.0105(7) -0.0037(7) 0.0052(8) C45 0.0275(8) 0.0383(9) 0.0232(8) 0.0053(6) 0.0007(6) 0.0008(6) C46 0.0167(6) 0.0270(8) 0.0197(7) 0.0055(5) 0.0002(5) 0.0018(5) C47 0.0245(7) 0.0209(7) 0.0245(7) 0.0080(6) -0.0017(6) -0.0006(5) C48 0.0148(6) 0.0212(7) 0.0239(7) 0.0046(5) 0.0007(5) 0.0004(5) C49 0.0327(8) 0.0218(8) 0.0267(8) 0.0038(6) -0.0035(6) 0.0009(6) C50 0.0335(8) 0.0256(8) 0.0225(7) 0.0011(6) 0.0012(6) -0.0014(6) C51 0.0197(6) 0.0222(7) 0.0222(7) 0.0006(6) 0.0015(5) 0.0001(5) C52 0.0273(7) 0.0206(7) 0.0219(7) 0.0048(5) 0.0016(6) 0.0004(5) C53 0.0164(6) 0.0232(7) 0.0195(7) 0.0053(5) 0.0006(5) 0.0022(5) C54 0.0238(7) 0.0277(8) 0.0172(7) 0.0046(6) 0.0016(6) 0.0042(6) N1 0.0208(6) 0.0246(6) 0.0142(6) 0.0034(4) -0.0014(4) -0.0008(4) N2 0.0193(5) 0.0157(6) 0.0151(5) 0.0044(4) -0.0013(4) 0.0003(4) N3 0.0211(6) 0.0174(6) 0.0154(6) 0.0035(4) -0.0011(4) 0.0006(4) N4 0.0206(6) 0.0197(6) 0.0131(5) 0.0058(4) -0.0006(4) -0.0001(4) O1 0.0304(6) 0.0230(6) 0.0252(5) 0.0024(4) -0.0011(4) -0.0001(4) O2 0.0212(5) 0.0211(5) 0.0220(5) 0.0069(4) 0.0021(4) -0.0005(4) O3 0.0216(5) 0.0221(5) 0.0205(5) 0.0051(4) 0.0013(4) -0.0004(4) O4 0.0237(5) 0.0211(5) 0.0214(5) 0.0032(4) -0.0010(4) 0.0012(4) F1 0.0627(7) 0.0459(7) 0.0265(5) 0.0182(4) -0.0027(5) -0.0064(5) F2 0.0452(6) 0.0664(8) 0.0229(5) 0.0066(5) -0.0098(4) -0.0139(5) F3 0.0510(7) 0.0795(9) 0.0335(6) 0.0093(6) 0.0196(5) 0.0211(6) F4 0.0333(6) 0.0537(7) 0.0621(8) -0.0224(6) -0.0068(5) -0.0086(5) F5 0.0640(8) 0.0429(7) 0.0519(7) -0.0172(5) 0.0232(6) 0.0034(5) F6 0.1529(16) 0.0172(6) 0.0492(7) 0.0067(5) -0.0397(9) -0.0045(7) F7 0.0366(5) 0.0460(6) 0.0405(6) -0.0137(5) -0.0071(5) -0.0066(4) F8 0.0439(6) 0.0451(6) 0.0347(6) -0.0149(5) 0.0117(5) 0.0005(5) F9 0.1122(11) 0.0209(5) 0.0344(6) 0.0005(4) -0.0036(6) -0.0078(6) F10 0.0549(6) 0.0311(5) 0.0287(5) 0.0143(4) -0.0075(4) -0.0068(4) F11 0.0430(6) 0.0404(6) 0.0282(5) 0.0104(4) -0.0136(4) -0.0091(4) F12 0.0595(7) 0.0919(10) 0.0284(6) 0.0226(6) 0.0221(5) 0.0469(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 C1 N1 1.4673(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.327(2) . ? C2 N2 1.3335(18) . ? C2 H2 0.9500 . ? C3 C4 1.357(2) . ? C3 N2 1.3816(19) . ? C3 H3 0.9500 . ? C4 N1 1.3755(19) . ? C4 H4 0.9500 . ? C5 N2 1.4804(18) . ? C5 C6 1.5234(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.5319(19) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5289(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.525(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.5268(19) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.524(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.527(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.522(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.525(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.522(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.530(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.524(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.528(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.525(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.526(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.519(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.524(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N3 1.4705(18) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N4 1.3289(19) . ? C24 N3 1.3309(18) . ? C24 H24 0.9500 . ? C25 C26 1.356(2) . ? C25 N4 1.3785(18) . ? C25 H25 0.9500 . ? C26 N3 1.3770(19) . ? C26 H26 0.9500 . ? C27 N4 1.4758(17) . ? C27 C28 1.5229(19) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.5283(18) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.5252(19) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.5285(19) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.5286(19) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.5278(19) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.5263(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.5279(19) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.529(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.5249(19) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.526(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.5288(19) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.527(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.5282(19) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.525(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.525(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.518(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 F1 1.334(2) . ? C45 F3 1.336(2) . ? C45 F2 1.337(2) . ? C45 C46 1.546(2) . ? C46 O1 1.2386(19) . ? C46 C47 1.404(2) . ? C47 C48 1.403(2) . ? C47 H47 0.9500 . ? C48 O2 1.2405(18) . ? C48 C49 1.540(2) . ? C49 F6 1.319(2) . ? C49 F4 1.325(2) . ? C49 F5 1.328(2) . ? C50 F9 1.334(2) . ? C50 F8 1.336(2) . ? C50 F7 1.336(2) . ? C50 C51 1.545(2) . ? C51 O3 1.2396(19) . ? C51 C52 1.402(2) . ? C52 C53 1.401(2) . ? C52 H52 0.9500 . ? C53 O4 1.2421(19) . ? C53 C54 1.5477(19) . ? C54 F12 1.3208(19) . ? C54 F10 1.3335(19) . ? C54 F11 1.3352(19) . ? 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 N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 108.60(12) . . ? N1 C2 H2 125.7 . . ? N2 C2 H2 125.7 . . ? C4 C3 N2 106.86(12) . . ? C4 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? C3 C4 N1 107.00(13) . . ? C3 C4 H4 126.5 . . ? N1 C4 H4 126.5 . . ? N2 C5 C6 112.15(11) . . ? N2 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C7 111.32(12) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 111.15(12) . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C7 115.32(12) . . ? C9 C8 H8A 108.4 . . ? C7 C8 H8A 108.4 . . ? C9 C8 H8B 108.4 . . ? C7 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? C8 C9 C10 111.60(12) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 114.25(13) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C12 113.02(13) . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 113.53(13) . . ? C13 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 113.61(13) . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 113.28(13) . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 C16 113.72(13) . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 113.02(13) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C18 113.60(13) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C19 C18 C17 112.89(13) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 113.91(14) . . ? C18 C19 H19A 108.8 . . ? C20 C19 H19A 108.8 . . ? C18 C19 H19B 108.8 . . ? C20 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C19 112.95(15) . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20B 109.0 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C20 C21 C22 113.53(18) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 N3 108.36(12) . . ? N4 C24 H24 125.8 . . ? N3 C24 H24 125.8 . . ? C26 C25 N4 106.95(13) . . ? C26 C25 H25 126.5 . . ? N4 C25 H25 126.5 . . ? C25 C26 N3 106.86(12) . . ? C25 C26 H26 126.6 . . ? N3 C26 H26 126.6 . . ? N4 C27 C28 112.03(11) . . ? N4 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? N4 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 110.38(12) . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C30 C29 C28 113.65(12) . . ? C30 C29 H29A 108.8 . . ? C28 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C28 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 C31 112.65(12) . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C30 C31 C32 113.80(12) . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C33 C32 C31 112.88(12) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 113.34(13) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 113.39(13) . . ? C33 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? C33 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C34 C35 C36 113.38(13) . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C35 113.48(13) . . ? C37 C36 H36A 108.9 . . ? C35 C36 H36A 108.9 . . ? C37 C36 H36B 108.9 . . ? C35 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C36 C37 C38 113.45(13) . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 113.52(13) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C40 C39 C38 113.70(13) . . ? C40 C39 H39A 108.8 . . ? C38 C39 H39A 108.8 . . ? C40 C39 H39B 108.8 . . ? C38 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C39 C40 C41 113.15(13) . . ? C39 C40 H40A 108.9 . . ? C41 C40 H40A 108.9 . . ? C39 C40 H40B 108.9 . . ? C41 C40 H40B 108.9 . . ? H40A C40 H40B 107.8 . . ? C42 C41 C40 114.02(13) . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? C40 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C41 C42 C43 113.27(13) . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42B 108.9 . . ? C43 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C42 114.14(14) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? F1 C45 F3 106.59(14) . . ? F1 C45 F2 106.78(13) . . ? F3 C45 F2 106.91(15) . . ? F1 C45 C46 115.10(14) . . ? F3 C45 C46 110.47(13) . . ? F2 C45 C46 110.57(13) . . ? O1 C46 C47 129.10(14) . . ? O1 C46 C45 113.86(14) . . ? C47 C46 C45 117.04(13) . . ? C48 C47 C46 122.08(13) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? O2 C48 C47 129.48(14) . . ? O2 C48 C49 113.75(13) . . ? C47 C48 C49 116.74(13) . . ? F6 C49 F4 109.20(15) . . ? F6 C49 F5 106.08(16) . . ? F4 C49 F5 104.66(14) . . ? F6 C49 C48 114.19(13) . . ? F4 C49 C48 110.85(13) . . ? F5 C49 C48 111.33(13) . . ? F9 C50 F8 106.34(14) . . ? F9 C50 F7 106.85(14) . . ? F8 C50 F7 106.66(13) . . ? F9 C50 C51 114.76(13) . . ? F8 C50 C51 110.90(13) . . ? F7 C50 C51 110.89(13) . . ? O3 C51 C52 129.53(14) . . ? O3 C51 C50 113.69(13) . . ? C52 C51 C50 116.77(13) . . ? C53 C52 C51 122.33(14) . . ? C53 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? O4 C53 C52 129.98(13) . . ? O4 C53 C54 113.88(13) . . ? C52 C53 C54 116.15(13) . . ? F12 C54 F10 106.69(13) . . ? F12 C54 F11 107.13(14) . . ? F10 C54 F11 106.33(12) . . ? F12 C54 C53 111.14(12) . . ? F10 C54 C53 115.00(13) . . ? F11 C54 C53 110.13(12) . . ? C2 N1 C4 108.99(12) . . ? C2 N1 C1 126.29(13) . . ? C4 N1 C1 124.56(13) . . ? C2 N2 C3 108.55(12) . . ? C2 N2 C5 124.42(12) . . ? C3 N2 C5 126.90(11) . . ? C24 N3 C26 108.95(12) . . ? C24 N3 C23 125.90(12) . . ? C26 N3 C23 125.13(12) . . ? C24 N4 C25 108.88(12) . . ? C24 N4 C27 126.40(12) . . ? C25 N4 C27 124.70(12) . . ? _diffrn_measured_fraction_theta_max .980 _diffrn_reflns_theta_full 71.61 _diffrn_measured_fraction_theta_full .980 _refine_diff_density_max .546 _refine_diff_density_min -.387 _refine_diff_density_rms .113 # Attachment 'wg195_fin.cif' data_wg195 _database_code_depnum_ccdc_archive 'CCDC 742065' #TrackingRef 'wg195_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H3 F18 Na O6, 2(C8 H15 N2)' _chemical_formula_sum 'C31 H33 F18 N4 Na O6' _chemical_formula_weight 922.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.6351(5) _cell_length_b 16.6309(7) _cell_length_c 20.5944(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.070(2) _cell_angle_gamma 90.00 _cell_volume 3881.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6956 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 71.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872.1 _exptl_absorpt_coefficient_mu 1.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 0.728 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32095 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 70.07 _reflns_number_total 7162 _reflns_number_gt 6124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0593P)^2^+1.4212P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7162 _refine_ls_number_parameters 697 _refine_ls_number_restraints 506 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.048 _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 C1 C 0.75726(19) 0.46534(12) -0.01105(10) 0.0312(4) Uani 1 1 d . . . C2 C 0.80973(17) 0.41721(10) 0.05280(9) 0.0236(4) Uani 1 1 d . . . C3 C 0.91575(17) 0.44566(11) 0.09230(10) 0.0258(4) Uani 1 1 d . . . H3 H 0.9550 0.4889 0.0762 0.031 Uiso 1 1 calc R . . C4 C 0.96597(16) 0.41260(10) 0.15466(9) 0.0229(4) Uani 1 1 d . . . C5 C 1.07421(18) 0.45577(12) 0.19686(10) 0.0307(4) Uani 1 1 d . . . C6 C 1.0671(2) 0.25261(14) -0.00471(11) 0.0366(5) Uani 1 1 d . . . C7 C 1.01921(17) 0.22568(11) 0.05572(10) 0.0265(4) Uani 1 1 d . . . C8 C 1.10403(16) 0.20854(11) 0.11381(10) 0.0267(4) Uani 1 1 d . . . H8 H 1.1846 0.2187 0.1145 0.032 Uiso 1 1 calc R . . C9 C 1.07500(16) 0.17696(10) 0.17107(10) 0.0231(4) Uani 1 1 d . . . C10 C 1.18267(17) 0.15623(12) 0.22782(10) 0.0291(4) Uani 1 1 d . . . C11 C 0.45702(15) 0.11607(10) 0.06460(9) 0.0318(4) Uani 1 1 d DU . . C12 C 0.56029(16) 0.15739(10) 0.11434(10) 0.0235(4) Uani 1 1 d . B . C13 C 0.54882(16) 0.16117(11) 0.18025(10) 0.0250(4) Uani 1 1 d . . . H13 H 0.4794 0.1403 0.1909 0.030 Uiso 1 1 calc R B . C14 C 0.63599(16) 0.19468(10) 0.23123(10) 0.0233(4) Uani 1 1 d . B . C15 C 0.60599(14) 0.20030(10) 0.30054(9) 0.0314(4) Uani 1 1 d DU . . C16 C 0.5423(2) 0.66736(14) 0.03662(13) 0.0437(5) Uani 1 1 d . . . H16A H 0.5600 0.6140 0.0566 0.066 Uiso 1 1 calc R . . H16B H 0.6157 0.6933 0.0321 0.066 Uiso 1 1 calc R . . H16C H 0.4892 0.6618 -0.0075 0.066 Uiso 1 1 calc R . . C17 C 0.37680(18) 0.74581(11) 0.06164(10) 0.0288(4) Uani 1 1 d . . . H17 H 0.3245 0.7389 0.0193 0.035 Uiso 1 1 calc R . . C18 C 0.45077(17) 0.78312(11) 0.16499(10) 0.0257(4) Uani 1 1 d . . . H18 H 0.4582 0.8071 0.2076 0.031 Uiso 1 1 calc R . . C19 C 0.53367(17) 0.73955(11) 0.14431(10) 0.0272(4) Uani 1 1 d . . . H19 H 0.6105 0.7271 0.1695 0.033 Uiso 1 1 calc R . . C20 C 0.24219(16) 0.82915(11) 0.11095(10) 0.0288(4) Uani 1 1 d . . . H20A H 0.2175 0.8198 0.1533 0.035 Uiso 1 1 calc R . . H20B H 0.1798 0.8078 0.0741 0.035 Uiso 1 1 calc R . . C21 C 0.25605(18) 0.91849(12) 0.10122(11) 0.0305(4) Uani 1 1 d . . . H21A H 0.2887 0.9273 0.0614 0.037 Uiso 1 1 calc R . . H21B H 0.3130 0.9405 0.1403 0.037 Uiso 1 1 calc R . . C22 C 0.13953(19) 0.96371(13) 0.09251(12) 0.0381(5) Uani 1 1 d . . . H22A H 0.1534 1.0215 0.0856 0.046 Uiso 1 1 calc R . . H22B H 0.0839 0.9435 0.0521 0.046 Uiso 1 1 calc R . . C23 C 0.0835(2) 0.95459(15) 0.15219(13) 0.0441(6) Uani 1 1 d . . . H23A H 0.0518 0.9001 0.1528 0.066 Uiso 1 1 calc R . . H23B H 0.0195 0.9937 0.1488 0.066 Uiso 1 1 calc R . . H23C H 0.1432 0.9641 0.1934 0.066 Uiso 1 1 calc R . . C24 C 0.78242(19) 1.02018(13) 0.07129(11) 0.0345(5) Uani 1 1 d . . . H24A H 0.8286 1.0700 0.0772 0.052 Uiso 1 1 calc R . . H24B H 0.7052 1.0302 0.0416 0.052 Uiso 1 1 calc R . . H24C H 0.8243 0.9789 0.0517 0.052 Uiso 1 1 calc R . . C25 C 0.81292(17) 1.02560(11) 0.19465(10) 0.0276(4) Uani 1 1 d . A . H25 H 0.8607 1.0725 0.2016 0.033 Uiso 1 1 calc R . . C26 C 0.7129(2) 0.91946(13) 0.21227(12) 0.0374(5) Uani 1 1 d . A . H26 H 0.6787 0.8789 0.2344 0.045 Uiso 1 1 calc R . . C27 C 0.7027(2) 0.92598(13) 0.14665(12) 0.0383(5) Uani 1 1 d . . . H27 H 0.6595 0.8911 0.1134 0.046 Uiso 1 1 calc R . . C29A C 0.9444(4) 0.9739(3) 0.3386(2) 0.0330(10) Uani 0.540(6) 1 d PDU A 1 H29A H 0.9920 1.0097 0.3167 0.040 Uiso 0.540(6) 1 calc PR A 1 H29B H 0.9678 0.9842 0.3872 0.040 Uiso 0.540(6) 1 calc PR A 1 C28A C 0.8151(8) 0.9957(8) 0.3141(4) 0.0338(17) Uani 0.540(6) 1 d PDU A 1 H28A H 0.7659 0.9619 0.3367 0.041 Uiso 0.540(6) 1 calc PR A 1 H28B H 0.8024 1.0527 0.3243 0.041 Uiso 0.540(6) 1 calc PR A 1 C30A C 0.9735(3) 0.8875(2) 0.3257(2) 0.0321(10) Uani 0.540(6) 1 d PDU A 1 H30A H 0.9526 0.8774 0.2771 0.039 Uiso 0.540(6) 1 calc PR A 1 H30B H 0.9247 0.8515 0.3467 0.039 Uiso 0.540(6) 1 calc PR A 1 C31A C 1.1031(9) 0.8670(8) 0.3525(8) 0.042(2) Uani 0.540(6) 1 d PDU A 1 H31A H 1.1522 0.9049 0.3344 0.063 Uiso 0.540(6) 1 calc PR A 1 H31B H 1.1182 0.8122 0.3390 0.063 Uiso 0.540(6) 1 calc PR A 1 H31C H 1.1221 0.8705 0.4012 0.063 Uiso 0.540(6) 1 calc PR A 1 C29B C 0.9221(4) 0.9309(4) 0.3474(2) 0.0343(11) Uani 0.460(6) 1 d PDU A 2 H29C H 0.9444 0.9420 0.3959 0.041 Uiso 0.460(6) 1 calc PR A 2 H29D H 0.8834 0.8776 0.3413 0.041 Uiso 0.460(6) 1 calc PR A 2 C28B C 0.8336(10) 0.9945(9) 0.3140(4) 0.0356(18) Uani 0.460(6) 1 d PDU A 2 H28C H 0.7684 0.9965 0.3376 0.043 Uiso 0.460(6) 1 calc PR A 2 H28D H 0.8732 1.0475 0.3197 0.043 Uiso 0.460(6) 1 calc PR A 2 C30B C 1.0324(4) 0.9276(3) 0.3210(2) 0.0334(11) Uani 0.460(6) 1 d PDU A 2 H30C H 1.0726 0.9804 0.3277 0.040 Uiso 0.460(6) 1 calc PR A 2 H30D H 1.0109 0.9166 0.2725 0.040 Uiso 0.460(6) 1 calc PR A 2 C31B C 1.1169(10) 0.8623(9) 0.3557(10) 0.041(3) Uani 0.460(6) 1 d PDU A 2 H31D H 1.1423 0.8749 0.4033 0.062 Uiso 0.460(6) 1 calc PR A 2 H31E H 1.1859 0.8601 0.3360 0.062 Uiso 0.460(6) 1 calc PR A 2 H31F H 1.0766 0.8102 0.3502 0.062 Uiso 0.460(6) 1 calc PR A 2 N1 N 0.48528(15) 0.71662(9) 0.07948(9) 0.0287(4) Uani 1 1 d . . . N2 N 0.35320(14) 0.78628(9) 0.11258(8) 0.0244(3) Uani 1 1 d . . . N3 N 0.76618(14) 0.99252(9) 0.13599(9) 0.0271(3) Uani 1 1 d . . . N4 N 0.78181(15) 0.98223(9) 0.24184(9) 0.0290(4) Uani 1 1 d D . . O1 O 0.74701(12) 0.36017(7) 0.06311(7) 0.0259(3) Uani 1 1 d . . . O2 O 0.93272(11) 0.35438(7) 0.18357(6) 0.0247(3) Uani 1 1 d . . . O3 O 0.91016(12) 0.21898(9) 0.04491(7) 0.0300(3) Uani 1 1 d . . . O4 O 0.97650(11) 0.16373(7) 0.18224(7) 0.0252(3) Uani 1 1 d . . . O5 O 0.64174(12) 0.18046(8) 0.08909(7) 0.0285(3) Uani 1 1 d . . . O6 O 0.73478(11) 0.22190(8) 0.22880(7) 0.0267(3) Uani 1 1 d . . . F1 F 0.72809(15) 0.41803(8) -0.06384(7) 0.0531(4) Uani 1 1 d . . . F2 F 0.65716(14) 0.50150(10) -0.00482(9) 0.0621(5) Uani 1 1 d . . . F3 F 0.82683(13) 0.52220(8) -0.02598(7) 0.0453(3) Uani 1 1 d . . . F4 F 1.04325(12) 0.49345(7) 0.24829(6) 0.0402(3) Uani 1 1 d . . . F5 F 1.12316(12) 0.51023(8) 0.16453(7) 0.0453(3) Uani 1 1 d . . . F6 F 1.15832(11) 0.40308(9) 0.22402(7) 0.0443(3) Uani 1 1 d . . . F7 F 0.99624(15) 0.30524(12) -0.04241(9) 0.0671(5) Uani 1 1 d . . . F8 F 1.17386(12) 0.28569(10) 0.01083(7) 0.0503(4) Uani 1 1 d . . . F9 F 1.07351(18) 0.18978(11) -0.04423(9) 0.0688(5) Uani 1 1 d . . . F10 F 1.24114(12) 0.22302(8) 0.25275(7) 0.0427(3) Uani 1 1 d . . . F11 F 1.26060(10) 0.10924(7) 0.20708(7) 0.0371(3) Uani 1 1 d . . . F12 F 1.15200(12) 0.11833(9) 0.27813(7) 0.0459(3) Uani 1 1 d . . . F13A F 0.4338(6) 0.1503(4) 0.00544(18) 0.0733(17) Uani 0.651(12) 1 d PDU B 1 F14A F 0.4843(4) 0.03913(16) 0.0564(4) 0.0540(13) Uani 0.651(12) 1 d PDU B 1 F15A F 0.3562(3) 0.1127(3) 0.0846(2) 0.0408(10) Uani 0.651(12) 1 d PDU B 1 F13B F 0.3519(6) 0.1418(10) 0.0689(6) 0.066(3) Uani 0.247(12) 1 d PDU B 2 F14B F 0.4682(11) 0.1276(7) 0.0027(3) 0.037(2) Uani 0.247(12) 1 d PDU B 2 F15B F 0.4600(14) 0.0372(2) 0.0741(6) 0.046(2) Uani 0.247(12) 1 d PDU B 2 F13C F 0.3840(11) 0.1758(6) 0.0399(8) 0.052(3) Uani 0.104(4) 1 d PDU B 3 F14C F 0.4914(11) 0.0827(10) 0.0140(6) 0.046(3) Uani 0.104(4) 1 d PDU B 3 F15C F 0.3951(13) 0.0626(8) 0.0894(6) 0.052(3) Uani 0.104(4) 1 d PDU B 3 F16A F 0.5423(12) 0.1379(6) 0.3122(5) 0.058(3) Uani 0.242(10) 1 d PDU B 1 F17A F 0.5403(12) 0.2652(6) 0.3024(4) 0.059(3) Uani 0.242(10) 1 d PDU B 1 F18A F 0.6980(6) 0.2050(8) 0.3515(4) 0.044(2) Uani 0.242(10) 1 d PDU B 1 F16B F 0.6902(4) 0.1681(6) 0.3474(3) 0.0591(19) Uani 0.487(13) 1 d PDU B 2 F17B F 0.5055(4) 0.1668(5) 0.3048(3) 0.0426(15) Uani 0.487(13) 1 d PDU B 2 F18B F 0.5995(10) 0.27764(16) 0.3168(4) 0.065(2) Uani 0.487(13) 1 d PDU B 2 F17C F 0.4934(3) 0.2039(8) 0.3017(5) 0.050(2) Uani 0.270(9) 1 d PDU B 3 F16C F 0.6490(12) 0.1337(5) 0.3334(4) 0.060(3) Uani 0.270(9) 1 d PDU B 3 F18C F 0.6598(9) 0.2615(5) 0.3357(4) 0.052(2) Uani 0.270(9) 1 d PDU B 3 Na1 Na 0.81552(6) 0.24854(4) 0.13412(3) 0.02084(17) Uani 1 1 d . B . 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 C1 0.0338(11) 0.0312(9) 0.0253(11) 0.0052(8) 0.0001(8) -0.0001(8) C2 0.0273(9) 0.0224(8) 0.0202(10) -0.0004(7) 0.0039(7) 0.0033(7) C3 0.0298(10) 0.0232(8) 0.0242(10) 0.0011(7) 0.0057(8) -0.0034(7) C4 0.0229(9) 0.0230(8) 0.0224(10) -0.0052(7) 0.0043(7) -0.0026(7) C5 0.0302(10) 0.0362(10) 0.0241(11) -0.0013(8) 0.0027(8) -0.0085(8) C6 0.0329(11) 0.0520(12) 0.0243(11) -0.0039(9) 0.0052(8) -0.0138(9) C7 0.0255(9) 0.0278(9) 0.0263(11) -0.0054(7) 0.0064(8) -0.0048(7) C8 0.0187(8) 0.0332(9) 0.0281(11) -0.0021(7) 0.0053(7) -0.0029(7) C9 0.0213(9) 0.0200(8) 0.0276(10) -0.0027(7) 0.0045(7) 0.0009(6) C10 0.0249(9) 0.0315(9) 0.0302(11) -0.0011(8) 0.0048(8) 0.0054(7) C11 0.0254(9) 0.0412(10) 0.0282(10) -0.0049(8) 0.0050(8) -0.0089(8) C12 0.0201(9) 0.0223(8) 0.0257(10) -0.0015(7) -0.0002(7) -0.0012(6) C13 0.0196(8) 0.0274(9) 0.0280(11) -0.0018(7) 0.0054(7) -0.0036(7) C14 0.0216(9) 0.0232(8) 0.0253(10) 0.0000(7) 0.0061(7) 0.0013(7) C15 0.0247(9) 0.0423(10) 0.0272(11) -0.0049(8) 0.0059(7) -0.0042(7) C16 0.0487(14) 0.0428(12) 0.0413(14) -0.0119(10) 0.0138(11) 0.0040(10) C17 0.0341(10) 0.0281(9) 0.0211(10) -0.0011(7) -0.0006(8) -0.0043(7) C18 0.0229(9) 0.0309(9) 0.0209(10) -0.0009(7) -0.0001(7) -0.0044(7) C19 0.0251(9) 0.0287(9) 0.0254(11) 0.0007(7) 0.0006(7) -0.0032(7) C20 0.0210(9) 0.0317(9) 0.0305(11) 0.0013(8) -0.0008(7) -0.0015(7) C21 0.0302(10) 0.0331(10) 0.0258(11) 0.0049(8) 0.0012(8) 0.0002(8) C22 0.0330(11) 0.0343(10) 0.0407(13) 0.0002(9) -0.0051(9) 0.0042(8) C23 0.0300(11) 0.0478(13) 0.0509(15) -0.0107(11) 0.0017(10) 0.0062(9) C24 0.0351(11) 0.0423(11) 0.0265(11) 0.0066(8) 0.0080(9) 0.0032(9) C25 0.0285(10) 0.0232(8) 0.0323(11) 0.0016(7) 0.0094(8) -0.0021(7) C26 0.0370(11) 0.0351(11) 0.0390(13) 0.0068(9) 0.0060(9) -0.0117(9) C27 0.0395(12) 0.0336(10) 0.0360(13) 0.0053(9) -0.0039(9) -0.0135(9) C29A 0.0360(19) 0.034(2) 0.027(2) -0.0038(16) 0.0032(15) -0.0057(15) C28A 0.039(3) 0.037(3) 0.027(3) -0.002(2) 0.010(2) 0.003(2) C30A 0.0284(18) 0.037(2) 0.028(2) -0.0048(15) 0.0016(15) -0.0034(15) C31A 0.034(3) 0.049(4) 0.036(4) -0.010(3) -0.004(3) 0.001(3) C29B 0.039(2) 0.041(3) 0.022(2) -0.0004(19) 0.0064(17) -0.0066(19) C28B 0.044(3) 0.037(3) 0.031(4) -0.005(3) 0.019(3) -0.001(3) C30B 0.036(2) 0.038(2) 0.026(2) 0.0020(17) 0.0061(17) -0.0073(19) C31B 0.034(4) 0.043(5) 0.045(6) 0.010(4) 0.004(4) -0.007(3) N1 0.0335(9) 0.0267(8) 0.0256(9) -0.0024(6) 0.0060(7) -0.0013(6) N2 0.0238(8) 0.0254(7) 0.0211(8) -0.0009(6) -0.0008(6) -0.0033(6) N3 0.0258(8) 0.0283(8) 0.0271(9) 0.0033(6) 0.0057(7) 0.0000(6) N4 0.0328(9) 0.0272(8) 0.0287(9) 0.0025(6) 0.0107(7) -0.0016(6) O1 0.0259(7) 0.0260(6) 0.0228(7) 0.0013(5) -0.0008(5) -0.0027(5) O2 0.0276(7) 0.0237(6) 0.0203(7) 0.0004(5) 0.0005(5) -0.0026(5) O3 0.0224(7) 0.0415(7) 0.0249(8) -0.0034(6) 0.0030(5) -0.0035(5) O4 0.0202(6) 0.0257(6) 0.0300(7) 0.0036(5) 0.0061(5) -0.0001(5) O5 0.0241(7) 0.0368(7) 0.0243(7) -0.0037(5) 0.0050(5) -0.0084(5) O6 0.0208(6) 0.0338(7) 0.0250(7) -0.0043(5) 0.0041(5) -0.0056(5) F1 0.0829(11) 0.0457(7) 0.0218(7) 0.0036(5) -0.0070(7) -0.0143(7) F2 0.0528(9) 0.0772(11) 0.0584(10) 0.0340(8) 0.0172(8) 0.0355(8) F3 0.0529(8) 0.0424(7) 0.0351(7) 0.0167(5) -0.0018(6) -0.0120(6) F4 0.0459(7) 0.0440(7) 0.0296(7) -0.0141(5) 0.0059(5) -0.0158(6) F5 0.0452(8) 0.0567(8) 0.0320(7) 0.0019(6) 0.0045(6) -0.0294(6) F6 0.0246(6) 0.0557(8) 0.0460(8) 0.0004(6) -0.0056(5) -0.0027(5) F7 0.0525(9) 0.1022(13) 0.0455(10) 0.0363(9) 0.0090(7) -0.0035(9) F8 0.0381(7) 0.0784(10) 0.0353(8) 0.0035(7) 0.0102(6) -0.0266(7) F9 0.0893(13) 0.0839(12) 0.0460(10) -0.0316(8) 0.0423(9) -0.0362(10) F10 0.0372(7) 0.0428(7) 0.0400(8) -0.0110(5) -0.0081(5) 0.0008(5) F11 0.0263(6) 0.0434(6) 0.0402(7) -0.0023(5) 0.0044(5) 0.0136(5) F12 0.0357(7) 0.0651(9) 0.0373(8) 0.0222(6) 0.0088(6) 0.0146(6) F13A 0.061(3) 0.112(4) 0.0332(16) 0.0226(19) -0.0176(13) -0.052(2) F14A 0.0327(15) 0.0486(13) 0.080(4) -0.0374(15) 0.0104(16) -0.0105(12) F15A 0.0186(11) 0.062(2) 0.0410(18) -0.0158(14) 0.0043(10) -0.0090(10) F13B 0.021(3) 0.112(7) 0.058(6) -0.036(6) -0.005(3) 0.002(4) F14B 0.036(5) 0.048(4) 0.018(2) 0.002(2) -0.010(2) -0.022(3) F15B 0.053(6) 0.044(2) 0.039(5) 0.007(3) 0.008(4) -0.030(3) F13C 0.029(6) 0.065(5) 0.052(8) -0.002(5) -0.013(5) 0.001(4) F14C 0.036(6) 0.069(7) 0.030(6) -0.024(5) 0.003(4) -0.018(5) F15C 0.036(7) 0.069(6) 0.051(6) -0.002(5) 0.009(5) -0.027(5) F16A 0.062(5) 0.080(4) 0.043(5) -0.023(4) 0.038(5) -0.040(4) F17A 0.061(6) 0.079(4) 0.037(4) -0.021(4) 0.010(4) 0.032(4) F18A 0.028(3) 0.086(6) 0.018(3) -0.002(4) 0.0078(17) -0.009(3) F16B 0.0323(19) 0.123(5) 0.019(2) 0.007(3) -0.0006(13) 0.000(3) F17B 0.0229(16) 0.073(4) 0.038(2) -0.019(3) 0.0193(17) -0.0093(19) F18B 0.096(6) 0.0565(16) 0.053(4) -0.0322(18) 0.038(4) -0.021(2) F17C 0.0244(19) 0.090(6) 0.036(3) -0.026(5) 0.011(2) 0.000(2) F16C 0.086(6) 0.068(3) 0.024(4) 0.014(3) 0.009(4) 0.028(4) F18C 0.050(4) 0.076(4) 0.034(4) -0.027(3) 0.020(3) -0.031(3) Na1 0.0188(3) 0.0216(3) 0.0208(4) -0.0006(2) 0.0016(3) -0.0017(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 C1 F1 1.323(3) . ? C1 F3 1.325(2) . ? C1 F2 1.342(3) . ? C1 C2 1.543(3) . ? C2 O1 1.244(2) . ? C2 C3 1.398(3) . ? C3 C4 1.398(3) . ? C3 H3 0.9500 . ? C4 O2 1.243(2) . ? C4 C5 1.537(3) . ? C5 F5 1.326(2) . ? C5 F6 1.338(3) . ? C5 F4 1.348(3) . ? C6 F7 1.326(3) . ? C6 F8 1.329(2) . ? C6 F9 1.337(3) . ? C6 C7 1.541(3) . ? C7 O3 1.243(2) . ? C7 C8 1.397(3) . ? C8 C9 1.400(3) . ? C8 H8 0.9500 . ? C9 O4 1.239(2) . ? C9 C10 1.547(3) . ? C10 F12 1.329(2) . ? C10 F11 1.338(2) . ? C10 F10 1.342(2) . ? C11 F13A 1.317(2) . ? C11 F13B 1.317(3) . ? C11 F15C 1.318(3) . ? C11 F14C 1.321(3) . ? C11 F14B 1.324(3) . ? C11 F15B 1.326(3) . ? C11 F15A 1.329(2) . ? C11 F13C 1.332(3) . ? C11 F14A 1.338(2) . ? C11 C12 1.552(2) . ? C12 O5 1.240(2) . ? C12 C13 1.395(3) . ? C13 C14 1.400(3) . ? C13 H13 0.9500 . ? C14 O6 1.247(2) . ? C14 C15 1.547(3) . ? C15 F17B 1.316(3) . ? C15 F17C 1.317(3) . ? C15 F18A 1.321(3) . ? C15 F18C 1.322(3) . ? C15 F16B 1.323(3) . ? C15 F17A 1.328(3) . ? C15 F16A 1.329(3) . ? C15 F18B 1.335(3) . ? C15 F16C 1.336(3) . ? C16 N1 1.468(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N1 1.324(3) . ? C17 N2 1.326(3) . ? C17 H17 0.9500 . ? C18 C19 1.350(3) . ? C18 N2 1.379(2) . ? C18 H18 0.9500 . ? C19 N1 1.380(3) . ? C19 H19 0.9500 . ? C20 N2 1.469(2) . ? C20 C21 1.513(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.525(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.523(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N3 1.462(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N4 1.325(3) . ? C25 N3 1.327(3) . ? C25 H25 0.9500 . ? C26 C27 1.334(3) . ? C26 N4 1.372(3) . ? C26 H26 0.9500 . ? C27 N3 1.375(3) . ? C27 H27 0.9500 . ? C29A C30A 1.513(5) . ? C29A C28A 1.518(7) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C28A N4 1.468(7) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C30A C31A 1.522(8) . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C29B C30B 1.504(6) . ? C29B C28B 1.528(8) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C28B N4 1.485(8) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C30B C31B 1.529(8) . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? O1 Na1 2.3861(14) . ? O2 Na1 2.3166(14) . ? O3 Na1 2.3968(16) . ? O4 Na1 2.3749(14) . ? O5 Na1 2.3200(14) . ? O6 Na1 2.3895(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 C1 F3 106.88(18) . . ? F1 C1 F2 106.16(19) . . ? F3 C1 F2 106.93(17) . . ? F1 C1 C2 111.74(16) . . ? F3 C1 C2 115.04(17) . . ? F2 C1 C2 109.61(17) . . ? O1 C2 C3 129.30(17) . . ? O1 C2 C1 114.01(16) . . ? C3 C2 C1 116.58(16) . . ? C2 C3 C4 122.15(17) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? O2 C4 C3 129.47(17) . . ? O2 C4 C5 113.39(17) . . ? C3 C4 C5 117.04(16) . . ? F5 C5 F6 107.48(17) . . ? F5 C5 F4 107.36(16) . . ? F6 C5 F4 106.03(17) . . ? F5 C5 C4 115.16(17) . . ? F6 C5 C4 111.02(16) . . ? F4 C5 C4 109.34(16) . . ? F7 C6 F8 106.93(19) . . ? F7 C6 F9 105.8(2) . . ? F8 C6 F9 107.01(19) . . ? F7 C6 C7 111.96(19) . . ? F8 C6 C7 114.50(18) . . ? F9 C6 C7 110.15(18) . . ? O3 C7 C8 129.05(19) . . ? O3 C7 C6 115.00(18) . . ? C8 C7 C6 115.87(17) . . ? C7 C8 C9 122.64(17) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? O4 C9 C8 129.24(18) . . ? O4 C9 C10 116.46(17) . . ? C8 C9 C10 114.30(16) . . ? F12 C10 F11 107.02(16) . . ? F12 C10 F10 107.25(17) . . ? F11 C10 F10 106.49(16) . . ? F12 C10 C9 112.36(16) . . ? F11 C10 C9 112.37(16) . . ? F10 C10 C9 111.01(15) . . ? F13A C11 F13B 85.6(5) . . ? F13A C11 F15C 129.4(6) . . ? F13B C11 F15C 66.2(9) . . ? F13A C11 F14C 59.1(8) . . ? F13B C11 F14C 129.9(7) . . ? F15C C11 F14C 108.1(4) . . ? F13B C11 F14B 108.2(4) . . ? F15C C11 F14B 130.7(7) . . ? F13A C11 F15B 123.9(6) . . ? F13B C11 F15B 107.8(4) . . ? F14C C11 F15B 72.4(8) . . ? F14B C11 F15B 106.3(4) . . ? F13A C11 F15A 107.1(3) . . ? F14C C11 F15A 132.2(6) . . ? F14B C11 F15A 126.2(5) . . ? F15B C11 F15A 84.7(6) . . ? F13A C11 F13C 49.0(8) . . ? F15C C11 F13C 107.1(4) . . ? F14C C11 F13C 107.0(4) . . ? F14B C11 F13C 73.6(8) . . ? F15B C11 F13C 142.0(9) . . ? F15A C11 F13C 67.6(8) . . ? F13A C11 F14A 107.5(3) . . ? F13B C11 F14A 124.8(7) . . ? F15C C11 F14A 64.5(8) . . ? F14C C11 F14A 51.3(8) . . ? F14B C11 F14A 86.5(5) . . ? F15A C11 F14A 104.5(2) . . ? F13C C11 F14A 144.5(7) . . ? F13A C11 C12 112.7(3) . . ? F13B C11 C12 113.8(5) . . ? F15C C11 C12 116.9(6) . . ? F14C C11 C12 112.3(5) . . ? F14B C11 C12 109.9(5) . . ? F15B C11 C12 110.5(6) . . ? F15A C11 C12 114.8(2) . . ? F13C C11 C12 104.7(6) . . ? F14A C11 C12 109.6(2) . . ? O5 C12 C13 130.11(17) . . ? O5 C12 C11 114.28(16) . . ? C13 C12 C11 115.59(15) . . ? C12 C13 C14 122.36(17) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? O6 C14 C13 129.23(18) . . ? O6 C14 C15 114.68(16) . . ? C13 C14 C15 116.08(16) . . ? F17B C15 F18A 123.0(6) . . ? F17C C15 F18A 127.9(7) . . ? F17B C15 F18C 127.4(4) . . ? F17C C15 F18C 107.8(3) . . ? F18A C15 F18C 47.3(7) . . ? F17B C15 F16B 107.6(3) . . ? F17C C15 F16B 125.5(5) . . ? F18C C15 F16B 74.4(5) . . ? F17B C15 F17A 79.4(6) . . ? F17C C15 F17A 51.8(8) . . ? F18A C15 F17A 107.3(4) . . ? F18C C15 F17A 64.0(8) . . ? F16B C15 F17A 130.0(5) . . ? F17C C15 F16A 55.5(9) . . ? F18A C15 F16A 106.7(4) . . ? F18C C15 F16A 135.8(6) . . ? F16B C15 F16A 84.5(6) . . ? F17A C15 F16A 106.3(4) . . ? F17B C15 F18B 106.8(3) . . ? F17C C15 F18B 80.7(4) . . ? F18A C15 F18B 80.0(5) . . ? F16B C15 F18B 106.4(3) . . ? F16A C15 F18B 129.9(6) . . ? F17B C15 F16C 81.5(5) . . ? F17C C15 F16C 106.8(4) . . ? F18A C15 F16C 60.2(8) . . ? F18C C15 F16C 106.5(3) . . ? F17A C15 F16C 144.2(6) . . ? F16A C15 F16C 54.6(9) . . ? F18B C15 F16C 135.1(4) . . ? F17B C15 C14 115.2(3) . . ? F17C C15 C14 116.9(4) . . ? F18A C15 C14 115.1(5) . . ? F18C C15 C14 112.0(4) . . ? F16B C15 C14 111.4(3) . . ? F17A C15 C14 109.1(4) . . ? F16A C15 C14 111.8(5) . . ? F18B C15 C14 109.0(3) . . ? F16C C15 C14 106.3(4) . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 N2 108.74(17) . . ? N1 C17 H17 125.6 . . ? N2 C17 H17 125.6 . . ? C19 C18 N2 107.09(17) . . ? C19 C18 H18 126.5 . . ? N2 C18 H18 126.5 . . ? C18 C19 N1 106.81(17) . . ? C18 C19 H19 126.6 . . ? N1 C19 H19 126.6 . . ? N2 C20 C21 111.12(16) . . ? N2 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N2 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 C22 112.43(17) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C21 112.77(18) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 N3 108.58(17) . . ? N4 C25 H25 125.7 . . ? N3 C25 H25 125.7 . . ? C27 C26 N4 107.26(18) . . ? C27 C26 H26 126.4 . . ? N4 C26 H26 126.4 . . ? C26 C27 N3 107.41(19) . . ? C26 C27 H27 126.3 . . ? N3 C27 H27 126.3 . . ? C30A C29A C28A 114.4(6) . . ? C30A C29A H29A 108.7 . . ? C28A C29A H29A 108.7 . . ? C30A C29A H29B 108.7 . . ? C28A C29A H29B 108.7 . . ? H29A C29A H29B 107.6 . . ? N4 C28A C29A 108.3(5) . . ? N4 C28A H28A 110.0 . . ? C29A C28A H28A 110.0 . . ? N4 C28A H28B 110.0 . . ? C29A C28A H28B 110.0 . . ? H28A C28A H28B 108.4 . . ? C29A C30A C31A 113.1(6) . . ? C29A C30A H30A 109.0 . . ? C31A C30A H30A 109.0 . . ? C29A C30A H30B 109.0 . . ? C31A C30A H30B 109.0 . . ? H30A C30A H30B 107.8 . . ? C30B C29B C28B 114.0(7) . . ? C30B C29B H29C 108.8 . . ? C28B C29B H29C 108.8 . . ? C30B C29B H29D 108.8 . . ? C28B C29B H29D 108.8 . . ? H29C C29B H29D 107.7 . . ? N4 C28B C29B 115.8(7) . . ? N4 C28B H28C 108.3 . . ? C29B C28B H28C 108.3 . . ? N4 C28B H28D 108.3 . . ? C29B C28B H28D 108.3 . . ? H28C C28B H28D 107.4 . . ? C29B C30B C31B 111.6(7) . . ? C29B C30B H30C 109.3 . . ? C31B C30B H30C 109.3 . . ? C29B C30B H30D 109.3 . . ? C31B C30B H30D 109.3 . . ? H30C C30B H30D 108.0 . . ? C30B C31B H31D 109.5 . . ? C30B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C30B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C17 N1 C19 108.77(17) . . ? C17 N1 C16 124.72(19) . . ? C19 N1 C16 126.50(19) . . ? C17 N2 C18 108.59(17) . . ? C17 N2 C20 124.49(17) . . ? C18 N2 C20 126.88(17) . . ? C25 N3 C27 108.21(17) . . ? C25 N3 C24 126.06(17) . . ? C27 N3 C24 125.70(18) . . ? C25 N4 C26 108.54(18) . . ? C25 N4 C28A 127.4(6) . . ? C26 N4 C28A 124.0(6) . . ? C25 N4 C28B 122.9(7) . . ? C26 N4 C28B 127.8(7) . . ? C2 O1 Na1 124.77(12) . . ? C4 O2 Na1 126.67(12) . . ? C7 O3 Na1 118.15(12) . . ? C9 O4 Na1 119.51(12) . . ? C12 O5 Na1 131.51(12) . . ? C14 O6 Na1 129.51(13) . . ? O2 Na1 O5 156.88(6) . . ? O2 Na1 O4 86.42(5) . . ? O5 Na1 O4 114.25(5) . . ? O2 Na1 O1 76.12(5) . . ? O5 Na1 O1 89.68(5) . . ? O4 Na1 O1 147.19(5) . . ? O2 Na1 O6 94.77(5) . . ? O5 Na1 O6 76.57(5) . . ? O4 Na1 O6 88.16(5) . . ? O1 Na1 O6 120.39(5) . . ? O2 Na1 O3 99.56(5) . . ? O5 Na1 O3 95.93(5) . . ? O4 Na1 O3 75.07(5) . . ? O1 Na1 O3 80.65(5) . . ? O6 Na1 O3 157.08(6) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 70.07 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.368 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.059 # Attachment 'wg209_fin.cif' data_wg209 _database_code_depnum_ccdc_archive 'CCDC 742066' #TrackingRef 'wg209_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H4 F24 Nd O8, C8 H15 N2' _chemical_formula_sum 'C28 H19 F24 N2 Nd O8' _chemical_formula_weight 1111.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' 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 16.4109(3) _cell_length_b 21.9547(5) _cell_length_c 43.1651(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15552.2(5) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6903 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 71.31 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8656 _exptl_absorpt_coefficient_mu 11.734 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.018 _exptl_absorpt_correction_T_max 0.096 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 134988 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 71.47 _reflns_number_total 15060 _reflns_number_gt 12984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0883P)^2^+73.9228P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15060 _refine_ls_number_parameters 1251 _refine_ls_number_restraints 979 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.069 _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 C1 C 0.9552(5) 0.1872(3) 0.12198(16) 0.0317(10) Uani 1 1 d U . . C2 C 0.9171(3) 0.2504(3) 0.11590(12) 0.0172(9) Uani 1 1 d U . . C3 C 0.9423(4) 0.2986(3) 0.13424(13) 0.0205(10) Uani 1 1 d U . . H3 H 0.9842 0.2919 0.1490 0.025 Uiso 1 1 calc R . . C4 C 0.9082(3) 0.3562(2) 0.13171(11) 0.0127(8) Uani 1 1 d U . . C5 C 0.9364(3) 0.4056(3) 0.15484(13) 0.0183(8) Uani 1 1 d U . . C6 C 0.5990(3) 0.3724(2) -0.00999(11) 0.0237(8) Uani 1 1 d DU . . C7 C 0.6279(3) 0.3319(3) 0.01730(11) 0.0141(7) Uani 1 1 d U A . C8 C 0.6027(3) 0.2718(3) 0.01738(11) 0.0145(8) Uani 1 1 d U . . H8 H 0.5668 0.2579 0.0017 0.017 Uiso 1 1 calc R A . C9 C 0.6293(3) 0.2309(3) 0.04028(11) 0.0112(7) Uani 1 1 d U A . C10 C 0.6005(3) 0.1650(3) 0.03782(13) 0.0178(7) Uani 1 1 d U . . C11 C 0.8705(4) 0.4696(3) 0.00740(13) 0.0226(8) Uani 1 1 d U . . C12 C 0.8513(3) 0.4041(3) 0.01810(12) 0.0161(8) Uani 1 1 d U A . C13 C 0.8531(3) 0.3584(3) -0.00371(12) 0.0192(9) Uani 1 1 d U . . H13 H 0.8646 0.3683 -0.0247 0.023 Uiso 1 1 calc R . . C14 C 0.8383(3) 0.2979(3) 0.00429(12) 0.0193(8) Uani 1 1 d U A . C15 C 0.8456(3) 0.2495(3) -0.02152(12) 0.0308(9) Uani 1 1 d DU . . C16 C 0.6872(3) 0.2758(3) 0.18036(12) 0.0306(10) Uani 1 1 d DU . . C17 C 0.6845(4) 0.3124(3) 0.14980(12) 0.0170(11) Uani 1 1 d . A . C18 C 0.6449(4) 0.3678(3) 0.15096(13) 0.0235(13) Uani 1 1 d . . . H18 H 0.6204 0.3803 0.1698 0.028 Uiso 1 1 calc R C . C19 C 0.6400(3) 0.4055(3) 0.12546(12) 0.0163(11) Uani 1 1 d . A . C20 C 0.5922(4) 0.4649(3) 0.12909(16) 0.0253(13) Uani 1 1 d . . . C21 C 0.4087(4) 0.3359(3) 0.23576(13) 0.0221(10) Uani 1 1 d U . . C22 C 0.3773(3) 0.3790(3) 0.21037(11) 0.0114(10) Uani 1 1 d . . . C23 C 0.4036(3) 0.4395(3) 0.21101(12) 0.0176(11) Uani 1 1 d . . . H23 H 0.4368 0.4530 0.2277 0.021 Uiso 1 1 calc R . . C24 C 0.3824(3) 0.4799(3) 0.18790(12) 0.0131(10) Uani 1 1 d . . . C25 C 0.4139(4) 0.5457(3) 0.19141(14) 0.0270(11) Uani 1 1 d U . . C26 C 0.0745(4) 0.5332(3) 0.09945(12) 0.0186(12) Uani 1 1 d . . . C27 C 0.1090(3) 0.4691(3) 0.10520(11) 0.0129(10) Uani 1 1 d . . . C28 C 0.0826(3) 0.4223(3) 0.08614(12) 0.0184(12) Uani 1 1 d . . . H28 H 0.0423 0.4302 0.0709 0.022 Uiso 1 1 calc R . . C29 C 0.1143(3) 0.3638(3) 0.08910(12) 0.0147(11) Uani 1 1 d . . . C30 C 0.0862(4) 0.3161(3) 0.06520(14) 0.0280(15) Uani 1 1 d . . . C31 C 0.3949(6) 0.4555(4) 0.05750(16) 0.0477(14) Uani 1 1 d U . . C32 C 0.3769(4) 0.4125(3) 0.08479(13) 0.0269(14) Uani 1 1 d . . . C33 C 0.4271(4) 0.3619(3) 0.08888(13) 0.0259(14) Uani 1 1 d . . . H33 H 0.4744 0.3573 0.0764 0.031 Uiso 1 1 calc R . . C34 C 0.4086(3) 0.3186(3) 0.11089(12) 0.0183(12) Uani 1 1 d . . . C35 C 0.4644(4) 0.2634(4) 0.11404(15) 0.0310(15) Uani 1 1 d . . . C36 C 0.1147(3) 0.2450(3) 0.21060(11) 0.0233(10) Uani 1 1 d DU . . C37 C 0.1479(3) 0.3081(3) 0.20167(12) 0.0136(11) Uani 1 1 d . D . C38 C 0.1434(3) 0.3525(3) 0.22427(12) 0.0172(11) Uani 1 1 d . . . H38 H 0.1296 0.3412 0.2449 0.021 Uiso 1 1 calc R D . C39 C 0.1588(3) 0.4139(3) 0.21746(12) 0.0150(11) Uani 1 1 d . D . C40 C 0.1390(4) 0.4610(3) 0.24231(14) 0.0275(14) Uani 1 1 d . . . C41 C 0.6379(5) 0.6008(4) 0.04507(16) 0.0388(18) Uani 1 1 d . . . H41A H 0.6309 0.6449 0.0473 0.058 Uiso 1 1 calc R . . H41B H 0.5859 0.5803 0.0490 0.058 Uiso 1 1 calc R . . H41C H 0.6563 0.5915 0.0240 0.058 Uiso 1 1 calc R . . C42 C 0.7358(4) 0.6150(3) 0.08825(15) 0.0235(14) Uani 1 1 d . . . H42 H 0.7250 0.6570 0.0916 0.028 Uiso 1 1 calc R . . C43 C 0.7877(4) 0.5233(3) 0.09143(13) 0.0213(12) Uani 1 1 d . . . H43 H 0.8204 0.4899 0.0978 0.026 Uiso 1 1 calc R . . C44 C 0.7304(4) 0.5226(3) 0.06914(14) 0.0222(12) Uani 1 1 d . . . H44 H 0.7149 0.4886 0.0569 0.027 Uiso 1 1 calc R . . C45 C 0.8455(4) 0.6019(3) 0.12773(13) 0.0235(13) Uani 1 1 d . . . H45A H 0.8453 0.6470 0.1285 0.028 Uiso 1 1 calc R . . H45B H 0.9015 0.5886 0.1226 0.028 Uiso 1 1 calc R . . C46 C 0.8225(3) 0.5770(3) 0.15955(13) 0.0214(12) Uani 1 1 d . . . H46A H 0.8121 0.5327 0.1580 0.026 Uiso 1 1 calc R . . H46B H 0.7718 0.5969 0.1668 0.026 Uiso 1 1 calc R . . C47 C 0.8908(4) 0.5885(4) 0.18299(15) 0.0309(15) Uani 1 1 d . . . H47A H 0.9404 0.5664 0.1763 0.037 Uiso 1 1 calc R . . H47B H 0.9038 0.6326 0.1833 0.037 Uiso 1 1 calc R . . C48 C 0.8680(5) 0.5682(5) 0.21547(16) 0.051(2) Uani 1 1 d . . . H48A H 0.8233 0.5936 0.2232 0.077 Uiso 1 1 calc R . . H48B H 0.9153 0.5725 0.2292 0.077 Uiso 1 1 calc R . . H48C H 0.8507 0.5255 0.2150 0.077 Uiso 1 1 calc R . . C49 C 0.3145(6) 0.5941(5) 0.1073(2) 0.055(2) Uani 1 1 d U . . H49A H 0.2899 0.5995 0.0867 0.083 Uiso 1 1 calc R . . H49B H 0.3159 0.5507 0.1124 0.083 Uiso 1 1 calc R . . H49C H 0.3701 0.6104 0.1071 0.083 Uiso 1 1 calc R . . C50 C 0.2194(5) 0.5979(4) 0.1527(2) 0.0406(15) Uani 1 1 d U . . H50 H 0.2168 0.5551 0.1556 0.049 Uiso 1 1 calc R . . C51 C 0.2039(4) 0.6932(3) 0.15608(16) 0.0305(13) Uani 1 1 d U . . H51 H 0.1848 0.7322 0.1623 0.037 Uiso 1 1 calc R . . C52 C 0.2577(5) 0.6847(5) 0.1336(2) 0.0471(17) Uani 1 1 d U . . H52 H 0.2854 0.7150 0.1219 0.057 Uiso 1 1 calc R . . C53 C 0.1207(4) 0.6352(4) 0.19437(15) 0.0311(14) Uani 1 1 d U . . H53A H 0.0992 0.5931 0.1946 0.037 Uiso 1 1 calc R . . H53B H 0.0744 0.6630 0.1904 0.037 Uiso 1 1 calc R . . C54 C 0.1558(3) 0.6494(3) 0.22561(14) 0.0195(11) Uani 1 1 d U . . H54A H 0.1795 0.6909 0.2253 0.023 Uiso 1 1 calc R . . H54B H 0.2002 0.6203 0.2302 0.023 Uiso 1 1 calc R . . C55 C 0.0916(4) 0.6457(3) 0.25107(16) 0.0268(13) Uani 1 1 d U . . H55A H 0.0497 0.6773 0.2473 0.032 Uiso 1 1 calc R . . H55B H 0.0645 0.6055 0.2500 0.032 Uiso 1 1 calc R . . C56 C 0.1259(5) 0.6543(4) 0.28295(17) 0.0426(18) Uani 1 1 d U . . H56A H 0.1615 0.6199 0.2881 0.064 Uiso 1 1 calc R . . H56B H 0.0812 0.6564 0.2980 0.064 Uiso 1 1 calc R . . H56C H 0.1573 0.6922 0.2837 0.064 Uiso 1 1 calc R . . N1 N 0.6991(3) 0.5793(3) 0.06744(10) 0.0201(10) Uani 1 1 d . . . N2 N 0.7898(3) 0.5816(2) 0.10327(10) 0.0140(9) Uani 1 1 d . . . N3 N 0.2640(4) 0.6279(4) 0.13122(14) 0.0419(14) Uani 1 1 d U . . N4 N 0.1793(3) 0.6410(2) 0.16913(11) 0.0186(9) Uani 1 1 d U . . O1 O 0.8641(2) 0.24987(18) 0.09503(8) 0.0142(7) Uani 1 1 d U . . O2 O 0.8547(2) 0.37444(18) 0.11322(8) 0.0127(7) Uani 1 1 d U . . O3 O 0.6734(2) 0.35886(18) 0.03592(8) 0.0149(7) Uani 1 1 d U . . O4 O 0.6765(2) 0.24089(18) 0.06248(8) 0.0125(7) Uani 1 1 d U . . O5 O 0.8350(2) 0.40032(19) 0.04671(8) 0.0152(7) Uani 1 1 d U . . O6 O 0.8208(2) 0.27671(19) 0.03029(8) 0.0176(7) Uani 1 1 d U . . O7 O 0.7187(2) 0.28751(18) 0.12723(8) 0.0155(8) Uani 1 1 d . . . O8 O 0.6725(2) 0.39787(18) 0.09927(8) 0.0152(8) Uani 1 1 d . . . O9 O 0.3311(2) 0.35430(17) 0.19131(8) 0.0136(8) Uani 1 1 d . . . O10 O 0.3380(2) 0.47168(17) 0.16471(8) 0.0120(7) Uani 1 1 d . . . O11 O 0.1599(2) 0.46697(18) 0.12691(8) 0.0154(8) Uani 1 1 d . . . O12 O 0.1652(2) 0.34426(18) 0.10787(8) 0.0133(7) Uani 1 1 d . . . O13 O 0.3174(3) 0.4286(2) 0.10058(9) 0.0219(9) Uani 1 1 d . . . O14 O 0.3488(2) 0.31817(19) 0.12910(9) 0.0169(8) Uani 1 1 d . . . O15 O 0.1713(2) 0.31278(17) 0.17395(8) 0.0131(7) Uani 1 1 d . . . O16 O 0.1838(2) 0.43608(17) 0.19244(8) 0.0144(7) Uani 1 1 d . . . F1 F 0.9755(3) 0.1601(2) 0.09547(10) 0.0486(11) Uani 1 1 d U . . F2 F 1.0218(3) 0.1897(2) 0.13922(11) 0.0480(11) Uani 1 1 d U . . F3 F 0.9015(4) 0.1512(2) 0.13637(12) 0.0539(11) Uani 1 1 d U . . F4 F 1.0069(3) 0.39327(19) 0.16829(10) 0.0398(9) Uani 1 1 d U . . F5 F 0.9437(2) 0.45971(16) 0.14118(8) 0.0238(7) Uani 1 1 d U . . F6 F 0.8804(3) 0.4123(2) 0.17711(8) 0.0362(9) Uani 1 1 d U . . F7A F 0.6038(7) 0.4312(3) -0.0030(2) 0.0280(15) Uani 0.54(2) 1 d PDU A 1 F8A F 0.5219(5) 0.3605(5) -0.0174(3) 0.0382(18) Uani 0.54(2) 1 d PDU A 1 F9A F 0.6452(7) 0.3607(6) -0.03440(18) 0.0348(18) Uani 0.54(2) 1 d PDU A 1 F7B F 0.6621(6) 0.3821(7) -0.0297(3) 0.0350(19) Uani 0.46(2) 1 d PDU A 2 F8B F 0.5411(8) 0.3466(5) -0.0274(3) 0.037(2) Uani 0.46(2) 1 d PDU A 2 F9B F 0.5758(9) 0.4269(4) -0.0014(3) 0.0337(18) Uani 0.46(2) 1 d PDU A 2 F10 F 0.5406(2) 0.15659(18) 0.01749(9) 0.0313(8) Uani 1 1 d U A . F11 F 0.6618(2) 0.12918(18) 0.02943(9) 0.0303(8) Uani 1 1 d U A . F12 F 0.5740(2) 0.14522(18) 0.06533(8) 0.0303(8) Uani 1 1 d U A . F13 F 0.9140(2) 0.4995(2) 0.02817(9) 0.0361(9) Uani 1 1 d U . . F14 F 0.8013(2) 0.5005(2) 0.00335(9) 0.0354(8) Uani 1 1 d U . . F15 F 0.9109(3) 0.4710(2) -0.01944(9) 0.0422(10) Uani 1 1 d U . . F16A F 0.8017(5) 0.2663(4) -0.04712(14) 0.0451(17) Uani 0.577(7) 1 d PDU B 1 F17A F 0.9178(4) 0.2396(4) -0.0309(2) 0.0540(18) Uani 0.577(7) 1 d PDU B 1 F18A F 0.8051(5) 0.1975(3) -0.01481(17) 0.0455(16) Uani 0.577(7) 1 d PDU B 1 F16B F 0.8852(7) 0.2719(5) -0.0460(2) 0.049(2) Uani 0.423(7) 1 d PDU B 2 F17B F 0.9013(6) 0.2072(4) -0.0121(2) 0.0407(19) Uani 0.423(7) 1 d PDU B 2 F18B F 0.7785(5) 0.2249(6) -0.0276(3) 0.055(2) Uani 0.423(7) 1 d PDU B 2 F19A F 0.7229(7) 0.2211(4) 0.1769(2) 0.0358(19) Uani 0.535(17) 1 d PDU C 1 F20A F 0.7236(8) 0.3047(5) 0.2028(2) 0.046(2) Uani 0.535(17) 1 d PDU C 1 F21A F 0.6119(4) 0.2613(6) 0.1911(2) 0.046(2) Uani 0.535(17) 1 d PDU C 1 F19B F 0.7547(7) 0.2946(6) 0.1953(3) 0.047(2) Uani 0.465(17) 1 d PDU C 2 F20B F 0.6258(7) 0.2905(7) 0.1988(2) 0.047(2) Uani 0.465(17) 1 d PDU C 2 F21B F 0.6913(9) 0.2176(4) 0.1761(3) 0.039(2) Uani 0.465(17) 1 d PDU C 2 F22 F 0.6394(3) 0.5088(2) 0.14076(12) 0.0457(11) Uani 1 1 d . C . F23 F 0.5281(3) 0.4585(2) 0.14766(12) 0.0501(12) Uani 1 1 d U C . F24 F 0.5637(3) 0.4858(2) 0.10219(10) 0.0409(10) Uani 1 1 d . C . F25 F 0.4576(3) 0.2946(2) 0.22379(10) 0.0505(12) Uani 1 1 d U . . F26 F 0.4481(3) 0.3638(2) 0.25832(10) 0.0542(13) Uani 1 1 d U . . F27 F 0.3483(3) 0.3055(2) 0.24861(10) 0.0453(11) Uani 1 1 d U . . F28 F 0.4798(3) 0.5498(2) 0.20845(11) 0.0568(12) Uani 1 1 d U . . F29 F 0.3558(4) 0.5792(2) 0.20539(12) 0.0572(12) Uani 1 1 d U . . F30 F 0.4296(2) 0.57103(17) 0.16420(8) 0.0308(8) Uani 1 1 d U . . F31 F 0.0554(2) 0.56112(16) 0.12607(8) 0.0224(7) Uani 1 1 d . . . F32 F 0.0073(2) 0.53300(17) 0.08190(8) 0.0272(8) Uani 1 1 d U . . F33 F 0.1294(2) 0.56841(17) 0.08516(8) 0.0290(8) Uani 1 1 d . . . F34 F 0.0108(2) 0.3253(2) 0.05505(10) 0.0392(10) Uani 1 1 d . . . F35 F 0.0873(4) 0.2600(2) 0.07664(12) 0.0621(16) Uani 1 1 d . . . F36 F 0.1351(3) 0.3174(3) 0.04097(10) 0.0535(13) Uani 1 1 d U . . F37 F 0.4100(3) 0.5108(2) 0.06683(11) 0.0543(11) Uani 1 1 d U . . F38 F 0.3345(4) 0.4569(3) 0.03813(12) 0.0770(15) Uani 1 1 d U . . F39 F 0.4621(4) 0.4393(3) 0.04140(14) 0.0850(17) Uani 1 1 d U . . F40 F 0.5348(3) 0.2690(2) 0.09887(11) 0.0487(12) Uani 1 1 d . . . F41 F 0.4852(3) 0.2548(2) 0.14395(10) 0.0435(11) Uani 1 1 d . . . F42 F 0.4290(3) 0.2128(2) 0.10456(12) 0.0453(11) Uani 1 1 d . . . F43A F 0.1443(3) 0.2007(2) 0.19265(12) 0.0411(12) Uani 0.837(6) 1 d PDU D 1 F44A F 0.1264(4) 0.2303(3) 0.23956(10) 0.0486(14) Uani 0.837(6) 1 d PDU D 1 F45A F 0.0342(3) 0.2435(2) 0.20515(13) 0.0418(12) Uani 0.837(6) 1 d PDU D 1 F43B F 0.1811(9) 0.2120(10) 0.2179(5) 0.037(3) Uani 0.163(6) 1 d PDU D 2 F44B F 0.0741(13) 0.2450(11) 0.2374(3) 0.033(3) Uani 0.163(6) 1 d PDU D 2 F45B F 0.0746(13) 0.2137(10) 0.1900(4) 0.036(3) Uani 0.163(6) 1 d PDU D 2 F46 F 0.1241(4) 0.4377(2) 0.26988(9) 0.0559(14) Uani 1 1 d . D . F47 F 0.0714(3) 0.4910(2) 0.23432(11) 0.0509(13) Uani 1 1 d . D . F48 F 0.1972(3) 0.5018(2) 0.24450(12) 0.0584(15) Uani 1 1 d . D . Nd1 Nd 0.764618(15) 0.324036(12) 0.076590(5) 0.00681(9) Uani 1 1 d . A . Nd2 Nd 0.250096(15) 0.390379(12) 0.147660(6) 0.00629(9) 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 C1 0.038(3) 0.025(2) 0.032(2) -0.0047(18) -0.0185(19) 0.0145(18) C2 0.017(2) 0.0205(16) 0.014(2) 0.0000(14) -0.0054(16) 0.0063(16) C3 0.017(2) 0.0247(19) 0.020(2) -0.0026(18) -0.0140(19) 0.0091(19) C4 0.009(2) 0.0189(16) 0.0099(18) 0.0011(14) -0.0039(14) 0.0007(15) C5 0.015(2) 0.0255(18) 0.015(2) -0.0035(15) -0.0083(13) 0.000(2) C6 0.0233(18) 0.0362(15) 0.0115(16) 0.0055(13) -0.0053(12) 0.0089(17) C7 0.0090(19) 0.0261(14) 0.0073(14) 0.0000(13) 0.0000(12) 0.0052(14) C8 0.009(2) 0.0282(16) 0.0065(17) -0.0014(14) -0.0035(14) 0.0018(16) C9 0.0036(16) 0.0234(12) 0.0066(14) -0.0013(11) 0.0004(12) 0.0006(12) C10 0.0109(19) 0.0268(15) 0.0155(17) -0.0006(15) -0.0071(13) -0.0035(14) C11 0.018(2) 0.037(2) 0.0120(19) 0.0033(16) 0.0035(16) -0.0072(18) C12 0.005(2) 0.0342(16) 0.0089(16) 0.0003(14) 0.0029(16) -0.0042(16) C13 0.012(2) 0.0367(18) 0.0086(18) -0.0020(14) 0.0039(18) 0.004(2) C14 0.010(2) 0.0343(17) 0.0131(16) -0.0037(14) 0.0011(16) 0.0050(18) C15 0.031(2) 0.043(2) 0.0190(18) -0.0135(16) 0.0047(16) 0.0040(17) C16 0.040(2) 0.044(2) 0.008(2) 0.004(2) -0.0005(17) 0.002(2) C17 0.020(3) 0.025(3) 0.007(2) -0.002(2) 0.000(2) -0.003(2) C18 0.024(3) 0.037(4) 0.010(2) -0.010(2) 0.008(2) 0.002(3) C19 0.008(2) 0.024(3) 0.017(3) -0.007(2) 0.006(2) -0.002(2) C20 0.014(3) 0.024(3) 0.038(3) -0.003(3) 0.013(2) 0.006(2) C21 0.018(3) 0.032(3) 0.017(2) 0.0082(19) -0.0068(17) -0.0006(17) C22 0.003(2) 0.022(3) 0.009(2) 0.000(2) 0.0018(18) 0.000(2) C23 0.015(3) 0.030(3) 0.008(2) -0.002(2) -0.0061(19) -0.008(2) C24 0.011(2) 0.016(3) 0.012(2) -0.003(2) 0.0023(19) -0.005(2) C25 0.044(3) 0.020(3) 0.017(2) -0.0043(19) -0.0068(19) -0.016(2) C26 0.017(3) 0.028(3) 0.010(2) 0.002(2) -0.005(2) 0.012(2) C27 0.005(2) 0.027(3) 0.006(2) 0.002(2) -0.0002(18) 0.007(2) C28 0.016(3) 0.030(3) 0.009(2) -0.003(2) -0.009(2) 0.007(2) C29 0.011(3) 0.022(3) 0.011(2) -0.004(2) 0.002(2) -0.003(2) C30 0.024(3) 0.039(4) 0.021(3) -0.019(3) -0.007(2) 0.006(3) C31 0.057(3) 0.071(3) 0.015(3) 0.016(3) 0.0065(18) -0.017(4) C32 0.030(3) 0.043(4) 0.007(2) 0.001(2) -0.002(2) -0.016(3) C33 0.018(3) 0.047(4) 0.012(3) -0.001(2) 0.011(2) -0.006(3) C34 0.011(3) 0.034(3) 0.010(2) -0.011(2) 0.002(2) -0.003(2) C35 0.015(3) 0.050(5) 0.028(3) -0.010(3) 0.006(2) 0.010(3) C36 0.027(2) 0.023(3) 0.0196(19) 0.0088(17) -0.0009(18) -0.009(2) C37 0.008(2) 0.022(3) 0.011(2) 0.009(2) -0.0031(18) -0.003(2) C38 0.016(3) 0.023(3) 0.013(2) 0.005(2) 0.000(2) -0.001(2) C39 0.008(2) 0.021(3) 0.016(2) 0.000(2) 0.0007(19) 0.001(2) C40 0.043(4) 0.018(3) 0.021(3) -0.001(2) 0.013(3) -0.004(3) C41 0.030(4) 0.061(5) 0.026(3) 0.009(3) -0.010(3) 0.018(3) C42 0.018(3) 0.029(4) 0.024(3) 0.013(3) 0.008(2) 0.007(2) C43 0.025(3) 0.020(3) 0.019(3) -0.001(2) 0.001(2) 0.004(2) C44 0.028(3) 0.022(3) 0.017(3) 0.000(2) 0.001(2) 0.002(2) C45 0.013(3) 0.038(4) 0.019(3) -0.003(3) -0.001(2) -0.006(2) C46 0.013(3) 0.036(4) 0.015(3) -0.002(2) 0.001(2) 0.000(2) C47 0.022(3) 0.047(4) 0.024(3) -0.008(3) -0.006(2) 0.003(3) C48 0.035(4) 0.099(8) 0.020(3) -0.009(4) -0.011(3) 0.004(4) C49 0.053(5) 0.072(6) 0.040(4) -0.009(4) -0.001(3) 0.003(4) C50 0.028(4) 0.035(3) 0.058(4) -0.021(3) -0.013(3) -0.003(3) C51 0.024(3) 0.037(3) 0.031(3) 0.017(3) 0.003(2) 0.002(3) C52 0.034(4) 0.075(4) 0.032(4) 0.005(4) 0.010(3) 0.005(4) C53 0.019(3) 0.044(4) 0.031(3) 0.016(3) -0.003(2) -0.012(3) C54 0.012(3) 0.018(3) 0.029(2) -0.004(2) 0.007(2) -0.001(2) C55 0.023(3) 0.022(3) 0.036(3) 0.010(3) 0.010(2) -0.001(2) C56 0.037(4) 0.056(5) 0.035(3) -0.012(4) 0.013(3) -0.004(4) N1 0.011(2) 0.038(3) 0.012(2) 0.008(2) 0.0017(17) 0.006(2) N2 0.010(2) 0.018(2) 0.014(2) 0.0008(17) 0.0031(17) 0.0004(18) N3 0.021(3) 0.081(4) 0.024(3) -0.015(3) -0.007(2) -0.015(3) N4 0.014(2) 0.019(2) 0.023(2) -0.0008(17) -0.0091(16) 0.0004(17) O1 0.0132(17) 0.0178(19) 0.0116(15) -0.0021(13) -0.0028(12) 0.0027(14) O2 0.0079(16) 0.0183(18) 0.0120(16) -0.0039(14) -0.0063(12) 0.0043(13) O3 0.0115(17) 0.0219(18) 0.0113(15) 0.0029(13) -0.0043(12) 0.0029(13) O4 0.0052(15) 0.0250(19) 0.0071(14) -0.0002(13) -0.0024(11) -0.0001(13) O5 0.0113(17) 0.028(2) 0.0066(13) -0.0022(13) 0.0004(13) -0.0035(15) O6 0.0112(18) 0.028(2) 0.0141(14) -0.0064(13) 0.0046(14) 0.0026(15) O7 0.0153(19) 0.025(2) 0.0061(16) -0.0026(15) -0.0010(14) 0.0017(16) O8 0.0104(18) 0.023(2) 0.0123(17) -0.0022(15) 0.0023(14) 0.0033(15) O9 0.0080(17) 0.0156(19) 0.0172(18) 0.0060(14) -0.0078(14) -0.0021(14) O10 0.0109(17) 0.0151(19) 0.0100(16) 0.0011(14) 0.0004(13) -0.0021(14) O11 0.0137(18) 0.017(2) 0.0158(17) -0.0033(15) -0.0087(14) 0.0018(15) O12 0.0104(18) 0.018(2) 0.0114(16) -0.0046(14) -0.0051(14) -0.0017(15) O13 0.025(2) 0.030(2) 0.0104(17) 0.0087(16) -0.0033(16) -0.0053(18) O14 0.0094(18) 0.024(2) 0.0174(18) 0.0052(16) 0.0070(15) 0.0036(15) O15 0.0095(17) 0.017(2) 0.0125(17) 0.0013(14) -0.0024(14) -0.0037(14) O16 0.0133(18) 0.0144(19) 0.0156(17) 0.0032(14) 0.0051(14) 0.0010(15) F1 0.060(3) 0.040(2) 0.045(2) -0.0198(18) -0.0234(17) 0.036(2) F2 0.055(2) 0.035(2) 0.054(2) -0.0073(18) -0.0381(19) 0.0255(17) F3 0.075(3) 0.028(2) 0.058(3) 0.020(2) -0.019(2) 0.001(2) F4 0.0339(16) 0.0402(19) 0.0454(19) -0.0099(15) -0.0316(15) 0.0066(15) F5 0.0227(18) 0.0216(15) 0.0271(16) -0.0053(12) -0.0067(13) -0.0013(13) F6 0.0440(19) 0.049(2) 0.0161(16) -0.0131(15) 0.0066(14) -0.0079(18) F7A 0.030(4) 0.0337(16) 0.021(3) 0.0109(17) -0.002(3) 0.010(2) F8A 0.028(2) 0.047(4) 0.040(4) 0.012(3) -0.019(2) 0.009(2) F9A 0.049(3) 0.043(4) 0.012(2) 0.006(2) 0.007(2) 0.003(3) F7B 0.040(3) 0.044(4) 0.021(3) 0.015(3) 0.007(2) 0.005(3) F8B 0.035(3) 0.050(4) 0.028(3) 0.005(3) -0.021(3) 0.007(3) F9B 0.036(4) 0.035(2) 0.030(3) 0.008(2) -0.006(3) 0.014(3) F10 0.0225(16) 0.037(2) 0.0342(16) 0.0010(16) -0.0204(15) -0.0103(14) F11 0.0238(15) 0.0270(16) 0.0401(19) -0.0127(16) -0.0086(13) 0.0032(13) F12 0.032(2) 0.033(2) 0.0258(14) 0.0076(14) -0.0025(12) -0.0167(15) F13 0.036(2) 0.043(2) 0.0289(16) 0.0056(16) -0.0070(15) -0.0230(18) F14 0.0302(17) 0.040(2) 0.036(2) 0.0119(17) -0.0025(14) 0.0014(15) F15 0.049(2) 0.054(3) 0.0234(15) 0.0094(16) 0.0221(16) -0.0119(19) F16A 0.060(3) 0.052(3) 0.023(2) -0.016(2) -0.013(2) 0.001(3) F17A 0.035(2) 0.066(4) 0.061(4) -0.042(3) 0.009(2) 0.008(2) F18A 0.065(4) 0.043(2) 0.029(3) -0.016(2) 0.001(3) -0.009(3) F16B 0.075(4) 0.048(4) 0.024(3) -0.011(2) 0.021(3) 0.005(3) F17B 0.048(3) 0.039(3) 0.035(4) -0.015(2) 0.004(3) 0.013(3) F18B 0.044(3) 0.061(4) 0.059(4) -0.029(3) -0.008(3) -0.007(3) F19A 0.044(4) 0.040(3) 0.024(3) 0.012(2) 0.003(3) 0.000(3) F20A 0.064(4) 0.055(3) 0.018(3) 0.000(3) -0.016(3) 0.003(3) F21A 0.043(3) 0.056(5) 0.040(4) 0.020(3) 0.009(3) 0.002(3) F19B 0.054(3) 0.052(4) 0.035(4) 0.005(3) -0.020(3) -0.002(3) F20B 0.058(3) 0.055(4) 0.027(4) 0.011(3) 0.018(3) 0.006(3) F21B 0.050(5) 0.042(2) 0.025(4) 0.007(3) 0.007(4) -0.007(3) F22 0.040(2) 0.031(2) 0.066(3) -0.024(2) 0.005(2) 0.0031(19) F23 0.035(2) 0.048(3) 0.067(3) 0.005(2) 0.036(2) 0.0148(19) F24 0.031(2) 0.043(3) 0.048(2) 0.005(2) 0.0003(18) 0.0215(19) F25 0.051(3) 0.063(3) 0.037(2) 0.0189(18) 0.0031(18) 0.037(2) F26 0.080(3) 0.052(3) 0.031(2) 0.0163(16) -0.041(2) -0.017(2) F27 0.0299(19) 0.063(3) 0.043(2) 0.038(2) -0.0015(15) -0.0074(17) F28 0.073(2) 0.050(3) 0.048(2) 0.0126(19) -0.038(2) -0.041(2) F29 0.092(3) 0.024(2) 0.056(3) -0.017(2) 0.026(2) -0.005(2) F30 0.040(2) 0.025(2) 0.0280(15) 0.0086(14) -0.0072(13) -0.0206(16) F31 0.0213(17) 0.0242(18) 0.0217(16) -0.0062(14) -0.0037(13) 0.0134(14) F32 0.0248(18) 0.0321(19) 0.0246(16) 0.0013(14) -0.0156(14) 0.0151(15) F33 0.034(2) 0.027(2) 0.0263(18) 0.0130(15) 0.0021(15) 0.0051(16) F34 0.024(2) 0.056(3) 0.037(2) -0.024(2) -0.0158(17) -0.0049(18) F35 0.088(4) 0.033(3) 0.065(3) -0.024(2) -0.043(3) 0.000(3) F36 0.042(2) 0.086(3) 0.033(2) -0.038(2) 0.0066(18) -0.002(2) F37 0.065(3) 0.058(2) 0.040(2) 0.0276(17) -0.0012(19) -0.011(2) F38 0.092(3) 0.103(4) 0.036(2) 0.035(2) -0.024(2) -0.028(3) F39 0.096(3) 0.098(3) 0.061(3) 0.027(3) 0.048(3) 0.004(3) F40 0.019(2) 0.075(3) 0.053(3) -0.013(2) 0.0193(19) 0.012(2) F41 0.029(2) 0.066(3) 0.036(2) 0.000(2) -0.0049(17) 0.026(2) F42 0.034(2) 0.038(3) 0.064(3) -0.023(2) 0.005(2) 0.0113(19) F43A 0.058(3) 0.020(2) 0.045(2) 0.0048(17) 0.015(2) -0.0094(18) F44A 0.081(3) 0.040(3) 0.0249(16) 0.0190(17) -0.014(2) -0.022(2) F45A 0.0272(17) 0.046(3) 0.052(3) 0.009(2) -0.0005(17) -0.0221(18) F43B 0.035(4) 0.034(5) 0.042(5) 0.008(4) 0.001(3) 0.004(4) F44B 0.038(5) 0.033(5) 0.028(3) 0.004(4) 0.009(4) -0.007(4) F45B 0.043(5) 0.032(5) 0.033(4) -0.003(4) -0.003(4) -0.011(4) F46 0.108(4) 0.044(3) 0.0159(18) -0.0049(18) 0.017(2) 0.002(3) F47 0.053(3) 0.047(3) 0.053(3) 0.000(2) 0.026(2) 0.027(2) F48 0.057(3) 0.055(3) 0.063(3) -0.042(3) 0.024(3) -0.025(2) Nd1 0.00380(14) 0.01241(16) 0.00421(14) -0.00119(9) -0.00158(8) 0.00174(9) Nd2 0.00260(14) 0.00815(16) 0.00812(14) 0.00224(9) -0.00215(9) -0.00057(9) _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 C1 F2 1.323(8) . ? C1 F1 1.332(8) . ? C1 F3 1.336(10) . ? C1 C2 1.546(8) . ? C2 O1 1.252(7) . ? C2 C3 1.384(8) . ? C3 C4 1.388(8) . ? C3 H3 0.9500 . ? C4 O2 1.253(6) . ? C4 C5 1.544(7) . ? C5 F4 1.322(7) . ? C5 F5 1.332(7) . ? C5 F6 1.338(7) . ? C6 F9B 1.309(8) . ? C6 F9A 1.324(7) . ? C6 F7A 1.328(8) . ? C6 F8A 1.331(7) . ? C6 F8B 1.339(8) . ? C6 F7B 1.356(8) . ? C6 C7 1.550(7) . ? C7 O3 1.247(7) . ? C7 C8 1.383(8) . ? C8 C9 1.404(7) . ? C8 H8 0.9500 . ? C9 O4 1.252(6) . ? C9 C10 1.525(8) . ? C10 F11 1.327(7) . ? C10 F10 1.330(6) . ? C10 F12 1.337(7) . ? C11 F13 1.322(7) . ? C11 F14 1.335(8) . ? C11 F15 1.336(7) . ? C11 C12 1.542(9) . ? C12 O5 1.267(6) . ? C12 C13 1.377(8) . ? C13 C14 1.394(9) . ? C13 H13 0.9500 . ? C14 O6 1.248(7) . ? C14 C15 1.543(8) . ? C15 F18B 1.255(8) . ? C15 F17A 1.270(7) . ? C15 F16B 1.335(8) . ? C15 F18A 1.351(7) . ? C15 F17B 1.366(8) . ? C15 F16A 1.369(7) . ? C16 F21B 1.294(8) . ? C16 F20A 1.303(8) . ? C16 F20B 1.325(8) . ? C16 F19A 1.346(8) . ? C16 F19B 1.347(8) . ? C16 F21A 1.358(8) . ? C16 C17 1.544(7) . ? C17 O7 1.250(7) . ? C17 C18 1.380(9) . ? C18 C19 1.379(9) . ? C18 H18 0.9500 . ? C19 O8 1.261(7) . ? C19 C20 1.530(8) . ? C20 F23 1.330(7) . ? C20 F24 1.334(8) . ? C20 F22 1.335(8) . ? C21 F25 1.316(8) . ? C21 F27 1.318(7) . ? C21 F26 1.319(7) . ? C21 C22 1.537(7) . ? C22 O9 1.243(6) . ? C22 C23 1.397(8) . ? C23 C24 1.380(8) . ? C23 H23 0.9500 . ? C24 O10 1.251(6) . ? C24 C25 1.542(8) . ? C25 F28 1.311(8) . ? C25 F30 1.325(7) . ? C25 F29 1.346(9) . ? C26 F33 1.338(7) . ? C26 F32 1.338(6) . ? C26 F31 1.340(6) . ? C26 C27 1.537(8) . ? C27 O11 1.256(6) . ? C27 C28 1.385(8) . ? C28 C29 1.391(8) . ? C28 H28 0.9500 . ? C29 O12 1.240(7) . ? C29 C30 1.542(8) . ? C30 F36 1.319(8) . ? C30 F34 1.327(8) . ? C30 F35 1.327(9) . ? C31 F38 1.297(10) . ? C31 F37 1.302(11) . ? C31 F39 1.351(11) . ? C31 C32 1.538(9) . ? C32 O13 1.243(8) . ? C32 C33 1.393(10) . ? C33 C34 1.379(9) . ? C33 H33 0.9500 . ? C34 O14 1.258(7) . ? C34 C35 1.525(9) . ? C35 F42 1.319(9) . ? C35 F40 1.333(7) . ? C35 F41 1.349(8) . ? C36 F45B 1.300(10) . ? C36 F44A 1.305(6) . ? C36 F43A 1.335(6) . ? C36 F44B 1.336(9) . ? C36 F45A 1.342(6) . ? C36 F43B 1.346(10) . ? C36 C37 1.538(7) . ? C37 O15 1.261(6) . ? C37 C38 1.381(8) . ? C38 C39 1.402(8) . ? C38 H38 0.9500 . ? C39 O16 1.253(7) . ? C39 C40 1.526(8) . ? C40 F48 1.314(8) . ? C40 F46 1.319(7) . ? C40 F47 1.335(9) . ? C41 N1 1.471(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 N2 1.320(8) . ? C42 N1 1.336(9) . ? C42 H42 0.9500 . ? C43 C44 1.345(9) . ? C43 N2 1.378(8) . ? C43 H43 0.9500 . ? C44 N1 1.348(8) . ? C44 H44 0.9500 . ? C45 N2 1.466(7) . ? C45 C46 1.526(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.532(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.518(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N3 1.518(11) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N3 1.351(12) . ? C50 N4 1.354(9) . ? C50 H50 0.9500 . ? C51 C52 1.323(11) . ? C51 N4 1.340(8) . ? C51 H51 0.9500 . ? C52 N3 1.256(13) . ? C52 H52 0.9500 . ? C53 N4 1.458(8) . ? C53 C54 1.499(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.524(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.499(10) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? O1 Nd1 2.439(4) . ? O2 Nd1 2.431(3) . ? O3 Nd1 2.430(3) . ? O4 Nd1 2.407(4) . ? O5 Nd1 2.408(4) . ? O6 Nd1 2.434(4) . ? O7 Nd1 2.447(4) . ? O8 Nd1 2.423(4) . ? O9 Nd2 2.438(3) . ? O10 Nd2 2.410(4) . ? O11 Nd2 2.413(4) . ? O12 Nd2 2.432(3) . ? O13 Nd2 2.461(4) . ? O14 Nd2 2.404(4) . ? O15 Nd2 2.421(4) . ? O16 Nd2 2.435(4) . ? 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 F2 C1 F1 107.2(6) . . ? F2 C1 F3 108.0(6) . . ? F1 C1 F3 107.5(6) . . ? F2 C1 C2 113.1(6) . . ? F1 C1 C2 110.9(5) . . ? F3 C1 C2 110.0(6) . . ? O1 C2 C3 128.8(5) . . ? O1 C2 C1 113.3(5) . . ? C3 C2 C1 117.9(5) . . ? C2 C3 C4 122.1(5) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? O2 C4 C3 128.6(5) . . ? O2 C4 C5 113.4(5) . . ? C3 C4 C5 118.0(5) . . ? F4 C5 F5 107.3(5) . . ? F4 C5 F6 107.9(5) . . ? F5 C5 F6 106.3(5) . . ? F4 C5 C4 113.7(5) . . ? F5 C5 C4 111.5(4) . . ? F6 C5 C4 109.7(5) . . ? F9B C6 F9A 124.7(8) . . ? F9A C6 F7A 109.6(7) . . ? F9B C6 F8A 88.4(7) . . ? F9A C6 F8A 108.3(7) . . ? F7A C6 F8A 107.6(6) . . ? F9B C6 F8B 109.8(7) . . ? F9A C6 F8B 82.9(7) . . ? F7A C6 F8B 125.5(7) . . ? F9B C6 F7B 104.8(8) . . ? F7A C6 F7B 86.8(7) . . ? F8A C6 F7B 127.3(7) . . ? F8B C6 F7B 104.9(7) . . ? F9B C6 C7 113.4(7) . . ? F9A C6 C7 108.5(6) . . ? F7A C6 C7 111.5(6) . . ? F8A C6 C7 111.2(6) . . ? F8B C6 C7 113.7(6) . . ? F7B C6 C7 109.4(6) . . ? O3 C7 C8 129.1(5) . . ? O3 C7 C6 113.6(5) . . ? C8 C7 C6 117.3(4) . . ? C7 C8 C9 121.3(5) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? O4 C9 C8 128.2(5) . . ? O4 C9 C10 114.3(5) . . ? C8 C9 C10 117.4(4) . . ? F11 C10 F10 107.3(5) . . ? F11 C10 F12 107.2(5) . . ? F10 C10 F12 107.5(5) . . ? F11 C10 C9 110.3(4) . . ? F10 C10 C9 114.0(5) . . ? F12 C10 C9 110.3(4) . . ? F13 C11 F14 107.2(6) . . ? F13 C11 F15 108.0(5) . . ? F14 C11 F15 107.3(5) . . ? F13 C11 C12 111.8(5) . . ? F14 C11 C12 109.8(5) . . ? F15 C11 C12 112.5(5) . . ? O5 C12 C13 128.6(6) . . ? O5 C12 C11 113.4(5) . . ? C13 C12 C11 118.1(5) . . ? C12 C13 C14 121.5(5) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? O6 C14 C13 128.1(5) . . ? O6 C14 C15 114.3(5) . . ? C13 C14 C15 117.6(5) . . ? F18B C15 F17A 132.7(8) . . ? F18B C15 F16B 114.8(9) . . ? F17A C15 F16B 50.0(6) . . ? F17A C15 F18A 112.4(7) . . ? F16B C15 F18A 136.0(7) . . ? F18B C15 F17B 110.9(9) . . ? F17A C15 F17B 49.8(6) . . ? F16B C15 F17B 99.2(7) . . ? F18A C15 F17B 72.0(7) . . ? F18B C15 F16A 59.0(8) . . ? F17A C15 F16A 106.3(7) . . ? F16B C15 F16A 61.2(7) . . ? F18A C15 F16A 98.2(6) . . ? F17B C15 F16A 140.9(7) . . ? F18B C15 C14 112.4(7) . . ? F17A C15 C14 114.7(6) . . ? F16B C15 C14 110.9(6) . . ? F18A C15 C14 112.8(5) . . ? F17B C15 C14 107.7(6) . . ? F16A C15 C14 110.9(5) . . ? F21B C16 F20A 124.2(9) . . ? F21B C16 F20B 111.5(8) . . ? F20A C16 F20B 77.5(7) . . ? F20A C16 F19A 108.4(7) . . ? F20B C16 F19A 128.0(8) . . ? F21B C16 F19B 109.1(8) . . ? F20B C16 F19B 105.3(8) . . ? F19A C16 F19B 88.1(7) . . ? F21B C16 F21A 82.2(7) . . ? F20A C16 F21A 106.1(7) . . ? F19A C16 F21A 102.9(7) . . ? F19B C16 F21A 131.1(8) . . ? F21B C16 C17 113.1(7) . . ? F20A C16 C17 113.4(6) . . ? F20B C16 C17 111.4(6) . . ? F19A C16 C17 112.5(6) . . ? F19B C16 C17 105.9(7) . . ? F21A C16 C17 112.8(6) . . ? O7 C17 C18 128.7(5) . . ? O7 C17 C16 115.2(5) . . ? C18 C17 C16 116.1(5) . . ? C19 C18 C17 121.8(5) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? O8 C19 C18 127.7(6) . . ? O8 C19 C20 114.9(5) . . ? C18 C19 C20 117.4(5) . . ? F23 C20 F24 106.5(5) . . ? F23 C20 F22 107.9(5) . . ? F24 C20 F22 106.4(6) . . ? F23 C20 C19 112.1(5) . . ? F24 C20 C19 112.6(5) . . ? F22 C20 C19 110.9(5) . . ? F25 C21 F27 106.0(6) . . ? F25 C21 F26 108.1(6) . . ? F27 C21 F26 107.0(5) . . ? F25 C21 C22 110.4(5) . . ? F27 C21 C22 111.1(5) . . ? F26 C21 C22 113.9(5) . . ? O9 C22 C23 128.1(5) . . ? O9 C22 C21 114.1(5) . . ? C23 C22 C21 117.8(5) . . ? C24 C23 C22 121.3(5) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? O10 C24 C23 129.2(5) . . ? O10 C24 C25 114.1(5) . . ? C23 C24 C25 116.6(5) . . ? F28 C25 F30 107.9(5) . . ? F28 C25 F29 107.2(5) . . ? F30 C25 F29 107.9(6) . . ? F28 C25 C24 113.3(6) . . ? F30 C25 C24 111.8(5) . . ? F29 C25 C24 108.6(5) . . ? F33 C26 F32 107.2(4) . . ? F33 C26 F31 106.7(5) . . ? F32 C26 F31 107.1(4) . . ? F33 C26 C27 110.9(5) . . ? F32 C26 C27 113.1(5) . . ? F31 C26 C27 111.5(4) . . ? O11 C27 C28 128.6(5) . . ? O11 C27 C26 113.5(5) . . ? C28 C27 C26 117.9(4) . . ? C27 C28 C29 120.8(5) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? O12 C29 C28 129.2(5) . . ? O12 C29 C30 113.8(5) . . ? C28 C29 C30 117.0(5) . . ? F36 C30 F34 107.6(5) . . ? F36 C30 F35 107.9(6) . . ? F34 C30 F35 106.1(6) . . ? F36 C30 C29 109.5(6) . . ? F34 C30 C29 113.4(5) . . ? F35 C30 C29 112.2(5) . . ? F38 C31 F37 108.9(8) . . ? F38 C31 F39 107.4(7) . . ? F37 C31 F39 104.4(7) . . ? F38 C31 C32 111.2(7) . . ? F37 C31 C32 111.8(6) . . ? F39 C31 C32 112.9(8) . . ? O13 C32 C33 128.4(6) . . ? O13 C32 C31 113.3(7) . . ? C33 C32 C31 118.2(6) . . ? C34 C33 C32 120.5(5) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? O14 C34 C33 127.5(6) . . ? O14 C34 C35 114.0(5) . . ? C33 C34 C35 118.5(5) . . ? F42 C35 F40 107.9(5) . . ? F42 C35 F41 106.9(6) . . ? F40 C35 F41 105.3(5) . . ? F42 C35 C34 112.2(5) . . ? F40 C35 C34 113.8(6) . . ? F41 C35 C34 110.4(5) . . ? F45B C36 F44A 126.7(11) . . ? F45B C36 F43A 53.4(11) . . ? F44A C36 F43A 108.8(5) . . ? F45B C36 F44B 109.9(12) . . ? F43A C36 F44B 133.2(11) . . ? F45B C36 F45A 50.9(11) . . ? F44A C36 F45A 107.8(5) . . ? F43A C36 F45A 103.8(5) . . ? F44B C36 F45A 70.2(11) . . ? F45B C36 F43B 106.5(12) . . ? F44A C36 F43B 61.7(10) . . ? F43A C36 F43B 56.5(10) . . ? F44B C36 F43B 101.6(12) . . ? F45A C36 F43B 145.6(12) . . ? F45B C36 C37 118.9(11) . . ? F44A C36 C37 114.2(5) . . ? F43A C36 C37 112.4(4) . . ? F44B C36 C37 113.2(11) . . ? F45A C36 C37 109.1(5) . . ? F43B C36 C37 104.9(11) . . ? O15 C37 C38 129.0(5) . . ? O15 C37 C36 114.8(5) . . ? C38 C37 C36 116.1(5) . . ? C37 C38 C39 121.4(5) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? O16 C39 C38 127.8(5) . . ? O16 C39 C40 114.3(5) . . ? C38 C39 C40 117.8(5) . . ? F48 C40 F46 109.6(6) . . ? F48 C40 F47 106.7(6) . . ? F46 C40 F47 105.7(6) . . ? F48 C40 C39 111.0(5) . . ? F46 C40 C39 114.2(5) . . ? F47 C40 C39 109.3(5) . . ? N1 C41 H41A 109.5 . . ? N1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N2 C42 N1 107.9(6) . . ? N2 C42 H42 126.0 . . ? N1 C42 H42 126.0 . . ? C44 C43 N2 107.1(5) . . ? C44 C43 H43 126.5 . . ? N2 C43 H43 126.5 . . ? C43 C44 N1 107.1(6) . . ? C43 C44 H44 126.4 . . ? N1 C44 H44 126.4 . . ? N2 C45 C46 112.6(5) . . ? N2 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? N2 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? C45 C46 C47 110.7(5) . . ? C45 C46 H46A 109.5 . . ? C47 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C48 C47 C46 112.4(6) . . ? C48 C47 H47A 109.1 . . ? C46 C47 H47A 109.1 . . ? C48 C47 H47B 109.1 . . ? C46 C47 H47B 109.1 . . ? H47A C47 H47B 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N3 C49 H49A 109.5 . . ? N3 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N3 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N3 C50 N4 106.5(7) . . ? N3 C50 H50 126.8 . . ? N4 C50 H50 126.8 . . ? C52 C51 N4 112.9(8) . . ? C52 C51 H51 123.6 . . ? N4 C51 H51 123.6 . . ? N3 C52 C51 104.8(8) . . ? N3 C52 H52 127.6 . . ? C51 C52 H52 127.6 . . ? N4 C53 C54 113.6(5) . . ? N4 C53 H53A 108.8 . . ? C54 C53 H53A 108.8 . . ? N4 C53 H53B 108.8 . . ? C54 C53 H53B 108.8 . . ? H53A C53 H53B 107.7 . . ? C53 C54 C55 111.8(5) . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C56 C55 C54 113.3(6) . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55B 108.9 . . ? C54 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C42 N1 C44 109.4(5) . . ? C42 N1 C41 124.2(6) . . ? C44 N1 C41 126.3(6) . . ? C42 N2 C43 108.4(5) . . ? C42 N2 C45 127.1(6) . . ? C43 N2 C45 124.5(5) . . ? C52 N3 C50 112.4(7) . . ? C52 N3 C49 126.0(8) . . ? C50 N3 C49 121.6(8) . . ? C51 N4 C50 103.3(6) . . ? C51 N4 C53 125.9(6) . . ? C50 N4 C53 130.8(6) . . ? C2 O1 Nd1 133.9(4) . . ? C4 O2 Nd1 134.1(4) . . ? C7 O3 Nd1 133.2(4) . . ? C9 O4 Nd1 134.3(4) . . ? C12 O5 Nd1 132.0(4) . . ? C14 O6 Nd1 131.8(4) . . ? C17 O7 Nd1 133.8(4) . . ? C19 O8 Nd1 135.6(4) . . ? C22 O9 Nd2 134.6(3) . . ? C24 O10 Nd2 134.4(3) . . ? C27 O11 Nd2 135.3(4) . . ? C29 O12 Nd2 134.6(4) . . ? C32 O13 Nd2 135.2(4) . . ? C34 O14 Nd2 136.8(4) . . ? C37 O15 Nd2 131.7(4) . . ? C39 O16 Nd2 132.1(4) . . ? O4 Nd1 O5 132.83(12) . . ? O4 Nd1 O8 103.59(13) . . ? O5 Nd1 O8 92.87(13) . . ? O4 Nd1 O3 71.70(13) . . ? O5 Nd1 O3 71.92(13) . . ? O8 Nd1 O3 72.38(13) . . ? O4 Nd1 O2 151.04(12) . . ? O5 Nd1 O2 74.95(12) . . ? O8 Nd1 O2 79.17(12) . . ? O3 Nd1 O2 134.52(13) . . ? O4 Nd1 O6 72.31(13) . . ? O5 Nd1 O6 71.07(13) . . ? O8 Nd1 O6 148.62(13) . . ? O3 Nd1 O6 76.97(13) . . ? O2 Nd1 O6 119.87(12) . . ? O4 Nd1 O1 88.74(12) . . ? O5 Nd1 O1 108.56(13) . . ? O8 Nd1 O1 137.08(12) . . ? O3 Nd1 O1 149.07(12) . . ? O2 Nd1 O1 71.63(12) . . ? O6 Nd1 O1 74.30(13) . . ? O4 Nd1 O7 78.03(12) . . ? O5 Nd1 O7 148.61(12) . . ? O8 Nd1 O7 70.51(13) . . ? O3 Nd1 O7 123.97(12) . . ? O2 Nd1 O7 75.84(13) . . ? O6 Nd1 O7 135.25(14) . . ? O1 Nd1 O7 72.29(13) . . ? O14 Nd2 O10 100.77(13) . . ? O14 Nd2 O11 138.54(13) . . ? O10 Nd2 O11 87.96(13) . . ? O14 Nd2 O15 92.98(13) . . ? O10 Nd2 O15 134.24(12) . . ? O11 Nd2 O15 109.68(13) . . ? O14 Nd2 O12 82.88(13) . . ? O10 Nd2 O12 150.09(12) . . ? O11 Nd2 O12 71.13(13) . . ? O15 Nd2 O12 74.46(12) . . ? O14 Nd2 O16 146.88(13) . . ? O10 Nd2 O16 73.73(12) . . ? O11 Nd2 O16 74.53(13) . . ? O15 Nd2 O16 71.28(13) . . ? O12 Nd2 O16 118.43(12) . . ? O14 Nd2 O9 71.10(13) . . ? O10 Nd2 O9 71.24(12) . . ? O11 Nd2 O9 147.97(13) . . ? O15 Nd2 O9 72.55(12) . . ? O12 Nd2 O9 136.28(13) . . ? O16 Nd2 O9 76.34(13) . . ? O14 Nd2 O13 69.34(14) . . ? O10 Nd2 O13 74.39(13) . . ? O11 Nd2 O13 74.41(14) . . ? O15 Nd2 O13 150.09(13) . . ? O12 Nd2 O13 79.40(13) . . ? O16 Nd2 O13 135.72(14) . . ? O9 Nd2 O13 120.29(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 71.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.371 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.169