# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Sergey Troyanov' _publ_contact_author_address ; Department of Chemisty Moscow State University Moscow, Leninskie gory Moscow 119992 RUSSIAN FEDERATION ; _publ_contact_author_email STROYANO@THERMO.CHEM.MSU.RU _publ_section_title ; New trifluoromethylated derivatives of [60]fullerene, C60(CF3)n with n = 12 and 14 ; loop_ _publ_author_name 'Sergey Troyanov' 'Stanislav M. Avdoshenko' 'Alexey Goryunkov' 'Iiya N. Ioffe' 'Erhard Kemnitz' ; N.A.Omelyanyuk ; 'Lev N. Sidorov' 'Nadezhda B. Tamm' # Attachment '60-14-I.CIF' data_60p7p1n _database_code_depnum_ccdc_archive 'CCDC 652165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 F42' _chemical_formula_weight 1686.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2190(2) _cell_length_b 13.8820(2) _cell_length_c 35.5411(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.5440(10) _cell_angle_gamma 90.00 _cell_volume 5535.00(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19847 _cell_measurement_theta_min 5 _cell_measurement_theta_max 30 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.91000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.2 beam line, BESSY, Berlin' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR345 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25510 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 33.70 _reflns_number_total 8031 _reflns_number_gt 6826 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Twinning was present due to the value of the beta angle close to 90 deg. In addition, the molecule is disordered relative its pseudo mirror plane, i. e. two enantiomers overlap one another nearly statistically (0.594/0.406). Therefore, some apparent contacts between symmetry related molecules should not be considered. Some C(cage)-CF3 distances associated with the disordered CF3 groups (C69 and C74) seem to be too long (1.83 and 1.77 A). This is caused by the fact that minor components of the C atoms on cage (C41 and C60, respectively) could not be localized. Therefore, these C-C distances should not be considered as realistic ones because two C atoms involved are from different components of the disordered molecule. ; _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^)+(0.0800P)^2^+85.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0111(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8031 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1761 _refine_ls_R_factor_gt 0.1517 _refine_ls_wR_factor_ref 0.3577 _refine_ls_wR_factor_gt 0.3491 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.208 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 F61A F 0.5973(9) 0.0879(8) 0.2451(3) 0.081(3) Uani 1 1 d . . . F61B F 0.4831(9) 0.1939(8) 0.2226(3) 0.068(3) Uani 1 1 d . . . F61C F 0.4149(9) 0.0519(8) 0.2339(3) 0.078(3) Uani 1 1 d . . . F62A F 0.5524(11) -0.1345(7) 0.3438(5) 0.109(5) Uani 1 1 d . . . F62B F 0.5856(10) -0.0681(7) 0.2912(4) 0.103(5) Uani 1 1 d . . . F62C F 0.4116(9) -0.1227(7) 0.3047(5) 0.117(6) Uani 1 1 d . . . F63A F 0.8113(8) 0.2019(6) 0.2921(3) 0.063(3) Uani 1 1 d . . . F63B F 0.7917(8) 0.3546(6) 0.2929(3) 0.063(3) Uani 1 1 d . . . F63C F 0.6929(9) 0.2706(8) 0.2535(2) 0.069(3) Uani 1 1 d . . . F64A F 0.0510(9) 0.1991(9) 0.2493(3) 0.077(3) Uani 1 1 d . . . F64B F 0.0242(9) 0.0622(8) 0.2779(4) 0.092(4) Uani 1 1 d . . . F64C F 0.1659(9) 0.0798(9) 0.2386(4) 0.102(5) Uani 1 1 d . . . F65A F 0.0250(10) -0.0684(7) 0.3402(5) 0.141(7) Uani 1 1 d . . . F65B F 0.1882(12) -0.1474(7) 0.3504(6) 0.141(7) Uani 1 1 d . . . F65C F 0.1561(10) -0.0853(8) 0.2961(5) 0.109(5) Uani 1 1 d . . . F66A F 0.8332(8) 0.0692(7) 0.3424(3) 0.072(3) Uani 1 1 d . . . F66B F 0.7474(10) -0.0504(7) 0.3691(4) 0.104(5) Uani 1 1 d . . . F66C F 0.8357(10) 0.0550(8) 0.4021(4) 0.087(4) Uani 1 1 d . . . F67A F 0.0339(8) 0.3794(7) 0.2626(3) 0.064(3) Uani 1 1 d . . . F67B F 0.1900(10) 0.3596(11) 0.2293(3) 0.097(4) Uani 1 1 d . . . F67C F 0.1717(11) 0.4880(8) 0.2593(4) 0.103(4) Uani 1 1 d . . . F68A F 0.2948(12) -0.1598(10) 0.4247(6) 0.164(9) Uani 1 1 d . . . F68B F 0.1163(14) -0.1063(8) 0.4229(7) 0.182(11) Uani 1 1 d . . . F68C F 0.2244(14) -0.0889(11) 0.4739(5) 0.144(6) Uani 1 1 d U . . F69A F 0.5376(16) 0.6455(10) 0.4381(5) 0.070(5) Uani 0.595(9) 1 d P . . F69B F 0.6610(15) 0.6095(10) 0.3941(5) 0.065(5) Uani 0.595(9) 1 d P . . F69C F 0.6833(11) 0.5730(12) 0.4554(5) 0.128(6) Uani 1 1 d . . . F69D F 0.687(2) 0.2593(14) 0.5123(6) 0.055(6) Uani 0.405(9) 1 d P . . F69E F 0.690(2) 0.4056(15) 0.4974(6) 0.060(6) Uani 0.405(9) 1 d P . . F69F F 0.5560(17) 0.3575(15) 0.5346(5) 0.047(5) Uani 0.405(9) 1 d P . . F70A F 0.3046(11) 0.6591(6) 0.3362(4) 0.101(4) Uani 1 1 d . . . F70B F 0.1629(11) 0.6510(7) 0.3751(5) 0.115(5) Uani 1 1 d . . . F70C F 0.1340(15) 0.6053(8) 0.3190(5) 0.127(6) Uani 1 1 d . . . F71A F -0.0969(11) 0.4295(10) 0.4232(4) 0.110(5) Uani 1 1 d . . . F71B F -0.1012(8) 0.4369(8) 0.3640(3) 0.080(3) Uani 1 1 d . . . F71C F -0.0142(10) 0.5445(7) 0.3965(7) 0.170(9) Uani 1 1 d . . . F72A F -0.0926(12) 0.2810(13) 0.4634(4) 0.130(6) Uani 1 1 d . . . F72B F 0.0240(15) 0.2654(14) 0.5100(4) 0.149(6) Uani 1 1 d U . . F72C F -0.0280(14) 0.1459(15) 0.4825(5) 0.151(7) Uani 1 1 d U . . F73A F 0.242(2) 0.0420(19) 0.5249(6) 0.197(10) Uani 1 1 d U . . F73B F 0.2258(18) 0.2040(15) 0.5437(5) 0.158(7) Uani 1 1 d U . . F73C F 0.3795(16) 0.1258(12) 0.5434(3) 0.126(6) Uani 1 1 d . . . F74A F 0.1265(18) 0.6172(11) 0.4385(5) 0.078(6) Uani 0.595(9) 1 d P . . F74B F 0.3049(17) 0.6489(11) 0.4526(6) 0.086(6) Uani 0.595(9) 1 d P . . F74C F 0.1976(19) 0.5512(10) 0.4871(5) 0.080(6) Uani 0.595(9) 1 d P . . F74D F 0.1488(19) 0.4305(17) 0.5175(7) 0.066(7) Uani 0.405(9) 1 d P . . F74E F 0.181(2) 0.2963(18) 0.5406(7) 0.066(7) Uani 0.405(9) 1 d PU . . C1 C 0.4588(14) 0.1533(10) 0.2879(5) 0.055(5) Uani 1 1 d . . . C2 C 0.3858(13) 0.0767(9) 0.3089(5) 0.051(4) Uani 1 1 d . . . C3 C 0.4727(14) 0.0204(11) 0.3353(5) 0.059(5) Uani 1 1 d . . . C4 C 0.5778(15) 0.0958(10) 0.3401(5) 0.060(5) Uani 1 1 d . . . C5 C 0.5617(11) 0.1685(9) 0.3140(4) 0.037(3) Uani 1 1 d . . . C6 C 0.6298(12) 0.2626(9) 0.3169(4) 0.039(3) Uani 1 1 d . . . C7 C 0.5423(14) 0.3457(10) 0.3108(4) 0.044(4) Uani 1 1 d . . . C8 C 0.4304(12) 0.3370(10) 0.2949(4) 0.046(4) Uani 1 1 d . . . C9 C 0.3781(14) 0.2425(9) 0.2857(4) 0.045(4) Uani 1 1 d . . . C10 C 0.2592(14) 0.2471(11) 0.2882(4) 0.052(4) Uani 1 1 d . . . C11 C 0.1885(14) 0.1560(11) 0.2989(4) 0.054(4) Uani 1 1 d . . . C12 C 0.2690(13) 0.0760(9) 0.3135(5) 0.049(4) Uani 1 1 d . . . C13 C 0.2090(15) 0.0228(11) 0.3471(6) 0.069(6) Uani 1 1 d . . . C14 C 0.2983(16) 0.0021(9) 0.3775(5) 0.058(5) Uani 1 1 d . . . C15 C 0.4107(18) 0.0039(11) 0.3726(6) 0.067(5) Uani 1 1 d . . . C16 C 0.4770(18) 0.0204(13) 0.4054(7) 0.081(7) Uani 1 1 d . . . C17 C 0.5865(14) 0.0762(13) 0.4106(5) 0.060(5) Uani 1 1 d . . . C18 C 0.6529(15) 0.1022(11) 0.3740(5) 0.058(5) Uani 1 1 d . . . C19 C 0.6776(13) 0.2095(12) 0.3829(4) 0.050(4) Uani 1 1 d . . . C20 C 0.6694(15) 0.2794(10) 0.3573(4) 0.049(4) Uani 1 1 d . . . C21 C 0.6345(13) 0.3750(11) 0.3682(4) 0.047(4) Uani 1 1 d . . . C22 C 0.5580(14) 0.4148(10) 0.3417(6) 0.063(5) Uani 1 1 d . . . C23 C 0.4603(13) 0.4738(9) 0.3494(4) 0.042(3) Uani 1 1 d . . . C24 C 0.3527(14) 0.4677(9) 0.3316(5) 0.054(4) Uani 1 1 d . . . C25 C 0.3324(13) 0.3974(10) 0.3035(4) 0.045(4) Uani 1 1 d . . . C26 C 0.2159(15) 0.3482(10) 0.2952(5) 0.055(4) Uani 1 1 d . . . C27 C 0.1468(14) 0.3562(9) 0.3308(4) 0.044(4) Uani 1 1 d . . . C28 C 0.0878(13) 0.2709(9) 0.3462(4) 0.046(4) Uani 1 1 d . . . C29 C 0.1126(13) 0.1795(10) 0.3333(5) 0.051(4) Uani 1 1 d . . . C30 C 0.1267(14) 0.1029(9) 0.3604(5) 0.051(4) Uani 1 1 d . . . C31 C 0.1114(15) 0.1239(10) 0.3986(5) 0.064(5) Uani 1 1 d . . . C32 C 0.1854(16) 0.0880(14) 0.4295(7) 0.081(7) Uani 1 1 d . . . C33 C 0.2685(17) 0.0043(13) 0.4192(6) 0.087(8) Uani 1 1 d . . . C34 C 0.391(2) 0.0315(18) 0.4359(7) 0.089(8) Uani 1 1 d . . . C35 C 0.403(2) 0.096(2) 0.4629(7) 0.095(8) Uani 1 1 d . . . C36 C 0.5097(17) 0.1615(18) 0.4641(5) 0.087(8) Uani 1 1 d . . . C37 C 0.5957(17) 0.1433(19) 0.4374(6) 0.091(8) Uani 1 1 d . . . C38 C 0.6574(14) 0.2277(13) 0.4200(5) 0.065(5) Uani 1 1 d . . . C39 C 0.6289(17) 0.3162(15) 0.4332(5) 0.072(5) Uani 1 1 d . . . C40 C 0.6155(14) 0.3921(12) 0.4054(5) 0.057(4) Uani 1 1 d . . . C41 C 0.5238(17) 0.4644(19) 0.4184(5) 0.090(8) Uani 1 1 d . . . C42 C 0.4408(14) 0.4918(11) 0.3898(5) 0.053(4) Uani 1 1 d . . . C43 C 0.3180(16) 0.5024(12) 0.3949(6) 0.070(6) Uani 1 1 d . . . C44 C 0.2520(13) 0.4999(10) 0.3571(5) 0.050(4) Uani 1 1 d . . . C45 C 0.1583(14) 0.4235(10) 0.3579(5) 0.052(4) Uani 1 1 d . . . C46 C 0.0834(15) 0.3964(11) 0.3921(5) 0.058(4) Uani 1 1 d . . . C47 C 0.0602(14) 0.2902(11) 0.3844(4) 0.051(4) Uani 1 1 d . . . C48 C 0.0744(14) 0.2181(10) 0.4114(5) 0.057(5) Uani 1 1 d . . . C49 C 0.109(2) 0.2346(17) 0.4507(5) 0.095(8) Uani 1 1 d . . . C50 C 0.1935(18) 0.1496(18) 0.4569(6) 0.082(7) Uani 1 1 d . . . C51 C 0.304(2) 0.158(2) 0.4836(7) 0.123(12) Uani 1 1 d . . . C52 C 0.3510(19) 0.260(2) 0.4816(6) 0.090(7) Uani 1 1 d . . . C53 C 0.478(2) 0.255(2) 0.4759(5) 0.107(10) Uani 1 1 d . . . C54 C 0.5416(17) 0.3366(18) 0.4633(7) 0.082(7) Uani 1 1 d . . . C55 C 0.4733(16) 0.4221(16) 0.4502(7) 0.087(7) Uani 1 1 d . . . C56 C 0.357(2) 0.4278(15) 0.4548(5) 0.075(6) Uani 1 1 d . . . C57 C 0.2644(17) 0.4737(19) 0.4290(6) 0.088(7) Uani 1 1 d . . . C58 C 0.1635(16) 0.4042(14) 0.4265(4) 0.059(5) Uani 1 1 d . . . C59 C 0.1756(19) 0.3353(18) 0.4534(6) 0.084(6) Uani 1 1 d . . . C60 C 0.296(2) 0.3477(18) 0.4728(6) 0.100(10) Uani 1 1 d . . . C61 C 0.4888(13) 0.1195(11) 0.2479(5) 0.052(4) Uani 1 1 d . . . C62 C 0.5103(16) -0.0786(13) 0.3200(8) 0.085(7) Uani 1 1 d . . . C63 C 0.7313(13) 0.2709(11) 0.2882(5) 0.052(4) Uani 1 1 d . . . C64 C 0.1075(17) 0.1223(15) 0.2668(6) 0.080(7) Uani 1 1 d . . . C65 C 0.1402(16) -0.0715(13) 0.3337(9) 0.093(8) Uani 1 1 d . . . C66 C 0.7736(19) 0.0428(13) 0.3707(6) 0.068(5) Uani 1 1 d . . . C67 C 0.1538(15) 0.3880(14) 0.2607(5) 0.061(5) Uani 1 1 d . . . C68 C 0.224(2) -0.0909(18) 0.4347(10) 0.136(13) Uani 1 1 d . . . C69 C 0.610(3) 0.5749(17) 0.4248(7) 0.058(9) Uani 0.595(9) 1 d P . . C69A C 0.615(3) 0.3369(17) 0.5034(10) 0.037(8) Uani 0.405(9) 1 d P . . C70 C 0.2105(19) 0.6073(13) 0.3443(10) 0.098(8) Uani 1 1 d . . . C71 C -0.0328(13) 0.4539(11) 0.3946(6) 0.066(6) Uani 1 1 d . . . C72 C 0.000(2) 0.231(3) 0.4749(7) 0.118(10) Uani 1 1 d . . . C73 C 0.279(3) 0.114(3) 0.5230(11) 0.168(18) Uani 1 1 d U . . C74 C 0.225(3) 0.5767(17) 0.4510(7) 0.049(7) Uani 0.595(9) 1 d P . . C74A C 0.241(5) 0.359(4) 0.5191(13) 0.081(15) Uani 0.405(9) 1 d PU . . 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 F61A 0.060(6) 0.108(8) 0.075(7) -0.050(6) 0.020(5) -0.007(6) F61B 0.067(6) 0.088(7) 0.049(6) -0.021(5) 0.015(5) -0.013(5) F61C 0.059(6) 0.100(8) 0.075(7) -0.054(6) 0.013(5) -0.022(5) F62A 0.087(8) 0.034(5) 0.208(15) 0.013(7) 0.048(9) 0.016(5) F62B 0.087(8) 0.064(6) 0.160(12) -0.052(7) 0.069(8) -0.004(6) F62C 0.052(6) 0.049(6) 0.250(17) -0.059(8) 0.020(8) -0.011(5) F63A 0.058(5) 0.057(5) 0.074(6) -0.003(4) 0.029(5) -0.005(4) F63B 0.052(5) 0.055(5) 0.081(7) -0.004(5) 0.016(5) -0.020(4) F63C 0.071(6) 0.110(8) 0.026(5) -0.011(5) 0.009(5) -0.027(6) F64A 0.063(6) 0.093(8) 0.075(7) -0.037(6) -0.006(6) -0.013(6) F64B 0.048(6) 0.074(7) 0.153(11) -0.053(7) 0.022(6) -0.027(5) F64C 0.054(6) 0.118(9) 0.134(11) -0.091(8) 0.012(7) -0.007(6) F65A 0.068(7) 0.047(6) 0.31(2) -0.054(9) 0.092(10) -0.023(5) F65B 0.102(9) 0.021(5) 0.30(2) 0.008(8) 0.071(11) -0.002(5) F65C 0.064(7) 0.059(6) 0.207(15) -0.050(8) 0.039(9) -0.020(5) F66A 0.047(5) 0.083(7) 0.087(7) 0.026(5) 0.029(5) 0.020(5) F66B 0.075(7) 0.042(6) 0.195(14) 0.011(7) 0.039(8) 0.014(5) F66C 0.086(8) 0.093(8) 0.083(9) 0.037(6) 0.034(7) 0.039(6) F67A 0.048(5) 0.091(7) 0.054(6) -0.003(5) -0.002(5) -0.009(5) F67B 0.071(7) 0.182(13) 0.039(6) 0.024(7) 0.005(6) -0.015(8) F67C 0.099(9) 0.081(8) 0.128(11) 0.058(7) -0.033(8) -0.025(7) F68A 0.104(10) 0.098(9) 0.29(2) 0.135(12) 0.102(12) 0.061(8) F68B 0.108(11) 0.056(7) 0.38(3) 0.065(11) 0.150(16) 0.014(7) F68C 0.114(10) 0.137(11) 0.181(13) 0.114(10) 0.070(10) 0.049(8) F69A 0.099(13) 0.042(8) 0.067(11) -0.019(7) -0.012(10) -0.018(8) F69B 0.087(12) 0.043(8) 0.065(11) -0.006(7) -0.017(9) -0.018(8) F69C 0.073(8) 0.160(14) 0.152(14) 0.089(11) -0.020(9) -0.027(9) F69D 0.075(15) 0.044(11) 0.046(13) -0.013(9) 0.010(11) 0.018(10) F69E 0.066(14) 0.054(13) 0.061(15) -0.025(11) 0.005(12) -0.021(11) F69F 0.041(11) 0.067(13) 0.034(12) 0.000(9) -0.009(10) -0.010(9) F70A 0.091(8) 0.030(5) 0.181(13) 0.006(6) 0.001(8) -0.012(5) F70B 0.085(8) 0.039(5) 0.222(16) -0.028(8) 0.029(10) 0.003(5) F70C 0.130(12) 0.055(7) 0.195(16) 0.028(8) -0.068(12) 0.017(7) F71A 0.086(8) 0.125(11) 0.121(10) -0.012(8) 0.043(8) 0.041(8) F71B 0.033(5) 0.108(8) 0.098(9) -0.011(7) -0.009(6) 0.003(5) F71C 0.056(7) 0.037(6) 0.42(3) -0.058(10) 0.029(11) -0.001(5) F72A 0.082(8) 0.223(17) 0.087(9) 0.055(10) 0.044(7) 0.087(10) F72B 0.150(12) 0.232(15) 0.066(8) 0.010(9) 0.052(8) 0.085(11) F72C 0.104(10) 0.199(14) 0.153(12) 0.070(11) 0.087(9) 0.043(10) F73A 0.189(16) 0.264(18) 0.138(13) 0.103(13) -0.021(11) -0.126(14) F73B 0.175(14) 0.195(15) 0.106(10) 0.044(10) 0.053(10) 0.049(12) F73C 0.150(13) 0.170(14) 0.058(8) 0.040(8) 0.024(8) 0.096(12) F74A 0.111(15) 0.053(9) 0.071(12) -0.033(8) 0.002(11) 0.031(10) F74B 0.088(13) 0.054(10) 0.117(16) -0.054(10) 0.011(11) -0.009(9) F74C 0.141(17) 0.040(8) 0.059(11) -0.025(7) 0.006(11) -0.003(9) F74D 0.046(12) 0.074(15) 0.079(17) -0.030(12) 0.008(12) -0.001(11) F74E 0.068(13) 0.070(13) 0.061(13) -0.010(10) 0.005(11) -0.015(11) C1 0.056(9) 0.040(8) 0.072(11) -0.015(7) 0.038(9) -0.009(7) C2 0.043(8) 0.027(6) 0.083(12) -0.018(7) 0.027(8) -0.017(6) C3 0.058(10) 0.043(8) 0.078(12) -0.018(8) 0.040(9) 0.001(7) C4 0.058(10) 0.037(8) 0.084(14) -0.006(8) 0.040(10) -0.002(7) C5 0.025(6) 0.032(6) 0.054(9) -0.011(6) 0.006(6) -0.004(5) C6 0.033(7) 0.042(7) 0.042(9) 0.002(6) 0.012(6) -0.004(6) C7 0.059(10) 0.046(8) 0.028(8) 0.014(6) 0.005(7) 0.003(7) C8 0.037(8) 0.053(8) 0.048(9) 0.004(7) 0.010(7) -0.005(6) C9 0.059(9) 0.030(7) 0.047(9) -0.016(6) 0.006(8) -0.006(6) C10 0.052(9) 0.064(10) 0.041(9) -0.013(7) 0.024(8) -0.011(7) C11 0.054(9) 0.055(9) 0.053(10) -0.005(7) 0.019(8) -0.009(7) C12 0.054(9) 0.025(6) 0.069(11) -0.014(6) 0.020(8) -0.002(6) C13 0.056(10) 0.043(8) 0.108(15) -0.015(9) 0.042(11) -0.004(8) C14 0.065(11) 0.021(6) 0.090(13) 0.028(7) 0.035(10) 0.013(6) C15 0.073(13) 0.044(9) 0.083(14) 0.036(9) 0.013(11) 0.012(8) C16 0.063(12) 0.060(11) 0.120(19) 0.054(11) 0.037(13) 0.015(9) C17 0.040(9) 0.080(12) 0.060(12) 0.036(9) 0.023(8) 0.030(8) C18 0.064(11) 0.043(8) 0.069(12) 0.023(7) 0.034(10) 0.011(7) C19 0.034(8) 0.075(10) 0.040(9) 0.008(7) 0.010(7) 0.015(7) C20 0.073(11) 0.040(7) 0.035(8) -0.002(6) 0.023(8) 0.004(7) C21 0.038(8) 0.058(9) 0.046(10) -0.009(7) -0.011(7) 0.001(7) C22 0.045(9) 0.036(8) 0.108(15) -0.014(9) -0.006(10) -0.014(7) C23 0.046(9) 0.028(6) 0.051(9) -0.011(6) -0.010(7) -0.005(6) C24 0.055(10) 0.026(7) 0.080(12) 0.021(7) 0.011(9) 0.002(6) C25 0.043(8) 0.054(8) 0.036(9) 0.007(6) 0.005(7) -0.011(7) C26 0.071(11) 0.036(7) 0.057(10) 0.008(7) 0.013(9) -0.016(7) C27 0.071(10) 0.028(6) 0.032(8) -0.006(5) -0.010(7) -0.012(6) C28 0.049(8) 0.033(7) 0.056(9) -0.017(6) 0.020(7) -0.014(6) C29 0.043(8) 0.046(8) 0.065(10) -0.024(7) 0.021(8) -0.020(6) C30 0.057(9) 0.022(6) 0.076(11) 0.012(6) 0.021(8) -0.004(6) C31 0.066(11) 0.036(8) 0.091(14) 0.010(8) 0.046(10) -0.001(7) C32 0.054(10) 0.076(12) 0.113(18) 0.070(13) 0.042(12) 0.033(10) C33 0.068(12) 0.062(11) 0.132(18) 0.047(11) 0.069(13) 0.038(9) C34 0.085(16) 0.109(17) 0.072(15) 0.052(13) 0.028(13) 0.047(13) C35 0.076(15) 0.13(2) 0.074(16) 0.066(15) 0.031(13) 0.043(14) C36 0.067(12) 0.16(2) 0.036(10) 0.025(11) 0.028(9) 0.062(13) C37 0.056(11) 0.14(2) 0.081(15) 0.057(15) 0.033(11) 0.048(13) C38 0.046(9) 0.084(12) 0.065(12) 0.024(9) 0.010(9) 0.045(9) C39 0.066(12) 0.100(14) 0.051(11) -0.027(10) 0.012(9) 0.023(10) C40 0.040(9) 0.064(10) 0.069(12) -0.023(9) -0.005(8) 0.016(7) C41 0.063(12) 0.19(2) 0.017(9) -0.037(11) -0.013(9) 0.062(14) C42 0.046(9) 0.051(9) 0.061(11) -0.027(8) -0.004(8) -0.002(7) C43 0.056(10) 0.056(10) 0.100(15) -0.037(10) 0.015(11) 0.010(8) C44 0.046(9) 0.038(7) 0.065(11) -0.007(7) 0.002(8) -0.001(6) C45 0.057(10) 0.041(8) 0.058(10) -0.003(7) 0.002(8) 0.010(7) C46 0.065(10) 0.049(9) 0.060(11) -0.006(7) 0.013(9) 0.021(8) C47 0.053(9) 0.048(8) 0.052(10) 0.007(7) 0.004(8) 0.005(7) C48 0.061(10) 0.044(8) 0.065(11) 0.002(7) 0.041(9) 0.014(7) C49 0.107(17) 0.126(19) 0.053(13) 0.029(12) 0.052(12) 0.064(15) C50 0.075(14) 0.118(17) 0.055(12) 0.046(12) 0.039(11) 0.048(12) C51 0.091(17) 0.19(3) 0.086(17) 0.064(18) 0.060(15) 0.079(19) C52 0.071(14) 0.15(2) 0.049(12) -0.028(13) 0.018(11) 0.013(14) C53 0.104(18) 0.19(3) 0.025(11) 0.002(13) 0.012(11) 0.08(2) C54 0.051(11) 0.115(17) 0.079(15) -0.057(13) -0.026(11) 0.027(11) C55 0.047(10) 0.104(16) 0.108(18) -0.064(14) -0.006(11) 0.019(11) C56 0.110(18) 0.076(13) 0.038(11) -0.014(9) 0.015(11) 0.013(12) C57 0.048(11) 0.15(2) 0.066(14) -0.015(13) -0.005(10) 0.025(12) C58 0.059(11) 0.090(13) 0.029(10) -0.016(8) 0.000(8) 0.026(9) C59 0.079(14) 0.108(17) 0.065(14) -0.020(12) 0.024(12) 0.024(12) C60 0.082(15) 0.13(2) 0.088(17) -0.066(15) -0.058(13) 0.086(15) C61 0.039(8) 0.051(9) 0.065(11) -0.019(8) 0.008(8) -0.007(7) C62 0.054(11) 0.042(10) 0.16(2) -0.026(12) 0.044(13) -0.013(9) C63 0.043(8) 0.052(9) 0.060(12) -0.019(7) 0.020(8) -0.008(7) C64 0.056(11) 0.079(13) 0.107(16) -0.062(12) 0.037(11) -0.032(10) C65 0.051(11) 0.048(11) 0.18(3) -0.024(13) 0.046(14) -0.009(8) C66 0.087(14) 0.071(12) 0.046(11) 0.024(9) 0.026(11) 0.029(10) C67 0.055(10) 0.092(13) 0.037(10) 0.018(8) -0.010(9) -0.010(9) C68 0.088(17) 0.095(17) 0.23(3) 0.076(19) 0.11(2) 0.049(14) C69 0.11(3) 0.037(13) 0.024(14) -0.013(10) 0.026(16) -0.001(14) C69A 0.044(19) 0.004(11) 0.06(2) -0.002(12) 0.013(17) -0.009(12) C70 0.056(12) 0.040(10) 0.20(3) 0.002(13) -0.004(16) -0.002(9) C71 0.026(8) 0.046(9) 0.126(17) -0.024(9) 0.014(10) 0.002(7) C72 0.098(19) 0.18(3) 0.071(17) 0.031(18) 0.047(15) 0.00(2) C73 0.09(2) 0.24(4) 0.17(3) 0.08(3) 0.07(2) 0.11(3) C74 0.09(2) 0.038(13) 0.024(14) -0.017(10) 0.012(13) -0.007(13) C74A 0.09(3) 0.11(4) 0.04(3) 0.03(2) 0.01(3) 0.00(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F61A C61 1.298(18) . ? F61B C61 1.370(19) . ? F61C C61 1.344(17) . ? F62A C62 1.24(3) . ? F62B C62 1.34(2) . ? F62C C62 1.37(2) . ? F63A C63 1.319(18) . ? F63B C63 1.354(16) . ? F63C C63 1.303(19) . ? F64A C64 1.38(3) . ? F64B C64 1.316(19) . ? F64C C64 1.340(18) . ? F65A C65 1.32(2) . ? F65B C65 1.32(3) . ? F65C C65 1.36(3) . ? F66A C66 1.266(18) . ? F66B C66 1.33(2) . ? F66C C66 1.32(2) . ? F67A C67 1.352(19) . ? F67B C67 1.26(2) . ? F67C C67 1.40(2) . ? F68A C68 1.29(2) . ? F68B C68 1.29(4) . ? F68C C68 1.39(4) . ? F69A C69 1.36(3) . ? F69A F69F 1.44(2) 3_666 ? F69B C69 1.33(3) . ? F69C C69 1.36(3) . ? F69C C74A 1.55(6) 3_666 ? F69D C69A 1.38(4) . ? F69E C69A 1.29(3) . ? F69E F74C 1.49(3) 3_666 ? F69F C69A 1.33(4) . ? F69F F69A 1.44(2) 3_666 ? F69F F74B 1.62(3) 3_666 ? F70A C70 1.31(2) . ? F70B C70 1.37(3) . ? F70C C70 1.24(3) . ? F71A C71 1.29(2) . ? F71B C71 1.35(2) . ? F71C C71 1.277(18) . ? F72A C72 1.31(3) . ? F72B C72 1.36(3) . ? F72C C72 1.25(3) . ? F73A C73 1.08(5) . ? F73B F74E 1.38(3) . ? F73B C73 1.57(4) . ? F73C C73 1.34(4) . ? F74A C74 1.31(3) . ? F74B C74 1.35(3) . ? F74B F69F 1.62(3) 3_666 ? F74B C69A 1.81(4) 3_666 ? F74C C74 1.37(3) . ? F74C F69E 1.49(3) 3_666 ? F74D C74A 1.44(6) . ? F74E C74A 1.34(5) . ? C1 C5 1.49(2) . ? C1 C9 1.54(2) . ? C1 C2 1.540(18) . ? C1 C61 1.54(2) . ? C2 C12 1.32(2) . ? C2 C3 1.56(3) . ? C3 C15 1.52(2) . ? C3 C62 1.54(2) . ? C3 C4 1.58(2) . ? C4 C5 1.38(2) . ? C4 C18 1.47(3) . ? C5 C6 1.516(17) . ? C6 C20 1.51(2) . ? C6 C7 1.530(19) . ? C6 C63 1.542(18) . ? C7 C8 1.38(2) . ? C7 C22 1.47(2) . ? C8 C25 1.42(2) . ? C8 C9 1.472(19) . ? C9 C10 1.34(2) . ? C10 C26 1.51(2) . ? C10 C11 1.54(2) . ? C11 C12 1.52(2) . ? C11 C64 1.52(3) . ? C11 C29 1.534(19) . ? C12 C13 1.56(2) . ? C13 C14 1.49(3) . ? C13 C30 1.52(2) . ? C13 C65 1.59(2) . ? C14 C15 1.27(2) . ? C14 C33 1.52(3) . ? C15 C16 1.40(3) . ? C16 C17 1.46(3) . ? C16 C34 1.46(3) . ? C17 C37 1.34(3) . ? C17 C18 1.55(2) . ? C18 C19 1.55(2) . ? C18 C66 1.59(2) . ? C19 C20 1.33(2) . ? C19 C38 1.36(2) . ? C20 C21 1.439(19) . ? C21 C40 1.36(2) . ? C21 C22 1.38(2) . ? C22 C23 1.40(2) . ? C23 C24 1.36(2) . ? C23 C42 1.47(2) . ? C24 C25 1.42(2) . ? C24 C44 1.52(2) . ? C25 C26 1.50(2) . ? C26 C27 1.49(2) . ? C26 C67 1.51(2) . ? C27 C45 1.347(19) . ? C27 C28 1.465(18) . ? C28 C29 1.378(18) . ? C28 C47 1.42(2) . ? C29 C30 1.44(2) . ? C30 C31 1.40(2) . ? C31 C48 1.45(2) . ? C31 C32 1.46(3) . ? C32 C50 1.30(3) . ? C32 C33 1.54(2) . ? C33 C68 1.52(3) . ? C33 C34 1.54(3) . ? C34 C35 1.32(3) . ? C35 C36 1.51(4) . ? C35 C51 1.59(3) . ? C36 C37 1.38(2) . ? C36 C53 1.41(3) . ? C37 C38 1.50(3) . ? C38 C39 1.35(2) . ? C39 C40 1.45(3) . ? C39 C54 1.49(3) . ? C40 C41 1.51(2) . ? C41 C55 1.40(3) . ? C41 C42 1.42(2) . ? C41 C69 1.83(4) . ? C42 C43 1.40(2) . ? C43 C57 1.41(3) . ? C43 C44 1.53(3) . ? C44 C45 1.49(2) . ? C44 C70 1.62(2) . ? C45 C46 1.53(2) . ? C46 C58 1.51(2) . ? C46 C47 1.52(2) . ? C46 C71 1.53(2) . ? C47 C48 1.39(2) . ? C48 C49 1.46(3) . ? C49 C72 1.50(3) . ? C49 C50 1.53(3) . ? C49 C59 1.59(3) . ? C50 C51 1.56(4) . ? C51 C52 1.51(4) . ? C51 C73 1.55(4) . ? C52 C60 1.40(3) . ? C52 C53 1.44(3) . ? C53 C54 1.41(3) . ? C54 C55 1.49(3) . ? C54 C69A 1.64(4) . ? C55 C56 1.32(3) . ? C56 C60 1.46(3) . ? C56 C57 1.52(3) . ? C57 C58 1.49(3) . ? C57 C74 1.69(3) . ? C58 C59 1.36(3) . ? C59 C60 1.52(3) . ? C60 C74A 1.77(5) . ? C69A F74B 1.81(4) 3_666 ? C74A F69C 1.55(6) 3_666 ? 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 C69 F69A F69F 131.1(18) . 3_666 ? C69 F69C C74A 141(2) . 3_666 ? C69A F69E F74C 142(3) . 3_666 ? C69A F69F F69A 159(2) . 3_666 ? C69A F69F F74B 74.7(19) . 3_666 ? F69A F69F F74B 121.1(16) 3_666 3_666 ? F74E F73B C73 147(2) . . ? C74 F74B F69F 127(2) . 3_666 ? C74 F74B C69A 116(2) . 3_666 ? F69F F74B C69A 45.3(13) 3_666 3_666 ? C74 F74C F69E 92.6(19) . 3_666 ? C74A F74E F73B 118(3) . . ? C5 C1 C9 111.7(11) . . ? C5 C1 C2 102.1(13) . . ? C9 C1 C2 105.4(11) . . ? C5 C1 C61 116.4(12) . . ? C9 C1 C61 109.5(14) . . ? C2 C1 C61 111.0(12) . . ? C12 C2 C1 126.7(15) . . ? C12 C2 C3 122.5(14) . . ? C1 C2 C3 107.8(12) . . ? C15 C3 C62 107.7(14) . . ? C15 C3 C2 108.2(13) . . ? C62 C3 C2 114.0(16) . . ? C15 C3 C4 110.6(15) . . ? C62 C3 C4 115.0(12) . . ? C2 C3 C4 101.2(12) . . ? C5 C4 C18 125.3(14) . . ? C5 C4 C3 108.6(16) . . ? C18 C4 C3 123.3(14) . . ? C4 C5 C1 114.2(13) . . ? C4 C5 C6 121.4(14) . . ? C1 C5 C6 123.5(12) . . ? C20 C6 C5 109.9(11) . . ? C20 C6 C7 101.7(11) . . ? C5 C6 C7 108.5(11) . . ? C20 C6 C63 113.8(12) . . ? C5 C6 C63 113.2(11) . . ? C7 C6 C63 109.0(11) . . ? C8 C7 C22 117.8(13) . . ? C8 C7 C6 125.0(13) . . ? C22 C7 C6 108.3(13) . . ? C7 C8 C25 124.5(14) . . ? C7 C8 C9 121.9(13) . . ? C25 C8 C9 105.4(12) . . ? C10 C9 C8 109.7(12) . . ? C10 C9 C1 128.5(13) . . ? C8 C9 C1 118.3(13) . . ? C9 C10 C26 112.2(13) . . ? C9 C10 C11 119.5(15) . . ? C26 C10 C11 123.7(12) . . ? C12 C11 C64 112.3(15) . . ? C12 C11 C29 102.4(13) . . ? C64 C11 C29 109.4(13) . . ? C12 C11 C10 112.2(13) . . ? C64 C11 C10 111.8(15) . . ? C29 C11 C10 108.3(12) . . ? C2 C12 C11 122.6(13) . . ? C2 C12 C13 122.2(16) . . ? C11 C12 C13 110.4(12) . . ? C14 C13 C30 108.8(15) . . ? C14 C13 C12 110.6(13) . . ? C30 C13 C12 99.1(12) . . ? C14 C13 C65 112.2(16) . . ? C30 C13 C65 113.6(14) . . ? C12 C13 C65 111.8(17) . . ? C15 C14 C13 123.8(16) . . ? C15 C14 C33 111(2) . . ? C13 C14 C33 123.2(14) . . ? C14 C15 C16 114.2(19) . . ? C14 C15 C3 126(2) . . ? C16 C15 C3 117.3(17) . . ? C15 C16 C17 129.2(16) . . ? C15 C16 C34 106.6(19) . . ? C17 C16 C34 114(2) . . ? C37 C17 C16 121.2(16) . . ? C37 C17 C18 113.8(17) . . ? C16 C17 C18 115.4(19) . . ? C4 C18 C19 109.1(12) . . ? C4 C18 C17 113.5(15) . . ? C19 C18 C17 98.0(14) . . ? C4 C18 C66 113.1(15) . . ? C19 C18 C66 111.2(15) . . ? C17 C18 C66 110.9(13) . . ? C20 C19 C38 121.0(15) . . ? C20 C19 C18 123.3(15) . . ? C38 C19 C18 110.2(14) . . ? C19 C20 C21 120.3(13) . . ? C19 C20 C6 123.5(14) . . ? C21 C20 C6 108.6(13) . . ? C40 C21 C22 119.3(15) . . ? C40 C21 C20 118.0(14) . . ? C22 C21 C20 110.7(14) . . ? C21 C22 C23 125.6(17) . . ? C21 C22 C7 108.6(13) . . ? C23 C22 C7 116.3(14) . . ? C24 C23 C22 124.4(13) . . ? C24 C23 C42 108.9(13) . . ? C22 C23 C42 114.6(15) . . ? C23 C24 C25 120.6(13) . . ? C23 C24 C44 111.5(15) . . ? C25 C24 C44 120.5(14) . . ? C8 C25 C24 116.1(14) . . ? C8 C25 C26 111.4(13) . . ? C24 C25 C26 125.9(13) . . ? C27 C26 C25 104.9(13) . . ? C27 C26 C10 112.3(11) . . ? C25 C26 C10 100.0(13) . . ? C27 C26 C67 114.9(14) . . ? C25 C26 C67 112.8(12) . . ? C10 C26 C67 110.7(14) . . ? C45 C27 C28 109.5(12) . . ? C45 C27 C26 127.6(13) . . ? C28 C27 C26 119.8(11) . . ? C29 C28 C47 122.5(14) . . ? C29 C28 C27 121.8(12) . . ? C47 C28 C27 107.9(11) . . ? C28 C29 C30 118.7(14) . . ? C28 C29 C11 125.2(13) . . ? C30 C29 C11 108.5(13) . . ? C31 C30 C29 118.6(12) . . ? C31 C30 C13 122.1(15) . . ? C29 C30 C13 113.3(13) . . ? C30 C31 C48 122.0(15) . . ? C30 C31 C32 125.8(15) . . ? C48 C31 C32 103.7(17) . . ? C50 C32 C31 112.0(16) . . ? C50 C32 C33 130(2) . . ? C31 C32 C33 115(2) . . ? C68 C33 C14 114(2) . . ? C68 C33 C32 111.7(13) . . ? C14 C33 C32 112.6(15) . . ? C68 C33 C34 112(2) . . ? C14 C33 C34 100.1(14) . . ? C32 C33 C34 105(2) . . ? C35 C34 C16 123(2) . . ? C35 C34 C33 121.8(19) . . ? C16 C34 C33 106(2) . . ? C34 C35 C36 120.0(19) . . ? C34 C35 C51 130(3) . . ? C36 C35 C51 103(2) . . ? C37 C36 C53 124(2) . . ? C37 C36 C35 116(2) . . ? C53 C36 C35 111.1(19) . . ? C17 C37 C36 125(2) . . ? C17 C37 C38 106.5(16) . . ? C36 C37 C38 118(2) . . ? C39 C38 C19 122.9(16) . . ? C39 C38 C37 117.1(16) . . ? C19 C38 C37 109.6(19) . . ? C38 C39 C40 116.6(15) . . ? C38 C39 C54 126(2) . . ? C40 C39 C54 106.7(17) . . ? C21 C40 C39 121.2(14) . . ? C21 C40 C41 121.7(16) . . ? C39 C40 C41 109.9(15) . . ? C55 C41 C42 115.0(18) . . ? C55 C41 C40 104.5(19) . . ? C42 C41 C40 113.7(13) . . ? C55 C41 C69 118.0(15) . . ? C42 C41 C69 102(2) . . ? C40 C41 C69 103.5(16) . . ? C43 C42 C41 125.0(17) . . ? C43 C42 C23 107.4(15) . . ? C41 C42 C23 123.1(13) . . ? C42 C43 C57 120.6(19) . . ? C42 C43 C44 110.7(15) . . ? C57 C43 C44 122.7(16) . . ? C45 C44 C24 109.3(12) . . ? C45 C44 C43 109.5(14) . . ? C24 C44 C43 99.9(13) . . ? C45 C44 C70 117.2(14) . . ? C24 C44 C70 108.4(14) . . ? C43 C44 C70 111.1(15) . . ? C27 C45 C44 122.7(14) . . ? C27 C45 C46 110.3(14) . . ? C44 C45 C46 125.6(14) . . ? C58 C46 C47 108.2(14) . . ? C58 C46 C71 114.4(14) . . ? C47 C46 C71 111.8(14) . . ? C58 C46 C45 107.3(15) . . ? C47 C46 C45 101.0(12) . . ? C71 C46 C45 113.2(14) . . ? C48 C47 C28 119.8(13) . . ? C48 C47 C46 123.6(15) . . ? C28 C47 C46 108.4(12) . . ? C47 C48 C31 117.7(14) . . ? C47 C48 C49 124.8(16) . . ? C31 C48 C49 111.5(16) . . ? C48 C49 C72 109(2) . . ? C48 C49 C50 100.0(16) . . ? C72 C49 C50 113.3(19) . . ? C48 C49 C59 108.4(15) . . ? C72 C49 C59 113(2) . . ? C50 C49 C59 112(2) . . ? C32 C50 C49 111(2) . . ? C32 C50 C51 123.7(19) . . ? C49 C50 C51 121(2) . . ? C52 C51 C50 108.5(19) . . ? C52 C51 C73 118(3) . . ? C50 C51 C73 112(3) . . ? C52 C51 C35 103.9(19) . . ? C50 C51 C35 103(2) . . ? C73 C51 C35 109.6(19) . . ? C60 C52 C53 116(3) . . ? C60 C52 C51 132(2) . . ? C53 C52 C51 108(2) . . ? C36 C53 C54 120.9(18) . . ? C36 C53 C52 110(3) . . ? C54 C53 C52 121(2) . . ? C53 C54 C39 114.4(18) . . ? C53 C54 C55 118.7(18) . . ? C39 C54 C55 105(2) . . ? C53 C54 C69A 89(2) . . ? C39 C54 C69A 107.2(17) . . ? C55 C54 C69A 121.6(17) . . ? C56 C55 C41 119(2) . . ? C56 C55 C54 121(2) . . ? C41 C55 C54 112.2(17) . . ? C55 C56 C60 119(2) . . ? C55 C56 C57 128(2) . . ? C60 C56 C57 105.5(19) . . ? C43 C57 C58 117.4(18) . . ? C43 C57 C56 110.1(16) . . ? C58 C57 C56 106(2) . . ? C43 C57 C74 105.9(19) . . ? C58 C57 C74 112.0(16) . . ? C56 C57 C74 104.7(18) . . ? C59 C58 C57 110.1(19) . . ? C59 C58 C46 124.9(19) . . ? C57 C58 C46 122.6(17) . . ? C58 C59 C60 109(2) . . ? C58 C59 C49 122(2) . . ? C60 C59 C49 123(2) . . ? C52 C60 C56 124(2) . . ? C52 C60 C59 113(2) . . ? C56 C60 C59 108(2) . . ? C52 C60 C74A 91(2) . . ? C56 C60 C74A 121(2) . . ? C59 C60 C74A 97(2) . . ? F61A C61 F61C 108.2(12) . . ? F61A C61 F61B 104.0(13) . . ? F61C C61 F61B 105.0(14) . . ? F61A C61 C1 112.7(15) . . ? F61C C61 C1 114.6(12) . . ? F61B C61 C1 111.5(12) . . ? F62A C62 F62B 110.5(16) . . ? F62A C62 F62C 107.0(16) . . ? F62B C62 F62C 105.0(19) . . ? F62A C62 C3 115(2) . . ? F62B C62 C3 110.4(15) . . ? F62C C62 C3 108.4(15) . . ? F63C C63 F63A 108.4(12) . . ? F63C C63 F63B 106.3(13) . . ? F63A C63 F63B 105.8(12) . . ? F63C C63 C6 112.8(13) . . ? F63A C63 C6 112.5(13) . . ? F63B C63 C6 110.7(11) . . ? F64B C64 F64C 107.4(13) . . ? F64B C64 F64A 107.4(16) . . ? F64C C64 F64A 103.2(19) . . ? F64B C64 C11 113.0(19) . . ? F64C C64 C11 113.7(15) . . ? F64A C64 C11 111.4(13) . . ? F65A C65 F65B 110.1(18) . . ? F65A C65 F65C 108(2) . . ? F65B C65 F65C 105.7(16) . . ? F65A C65 C13 113.3(15) . . ? F65B C65 C13 109(2) . . ? F65C C65 C13 110.0(16) . . ? F66A C66 F66C 110.8(18) . . ? F66A C66 F66B 111.4(16) . . ? F66C C66 F66B 106.1(15) . . ? F66A C66 C18 111.4(14) . . ? F66C C66 C18 108.3(15) . . ? F66B C66 C18 108.6(16) . . ? F67B C67 F67A 110.3(15) . . ? F67B C67 F67C 103.5(14) . . ? F67A C67 F67C 103.4(14) . . ? F67B C67 C26 117.1(16) . . ? F67A C67 C26 112.3(13) . . ? F67C C67 C26 109.0(14) . . ? F68B C68 F68A 111(3) . . ? F68B C68 F68C 108.8(17) . . ? F68A C68 F68C 107(2) . . ? F68B C68 C33 110(2) . . ? F68A C68 C33 109.9(15) . . ? F68C C68 C33 110(3) . . ? F69B C69 F69C 114(3) . . ? F69B C69 F69A 107(2) . . ? F69C C69 F69A 95.4(17) . . ? F69B C69 C41 115.7(18) . . ? F69C C69 C41 113.6(18) . . ? F69A C69 C41 109(2) . . ? F69E C69A F69F 108(2) . . ? F69E C69A F69D 103(3) . . ? F69F C69A F69D 106(3) . . ? F69E C69A C54 101(2) . . ? F69F C69A C54 118(2) . . ? F69D C69A C54 119(2) . . ? F69E C69A F74B 75(2) . 3_666 ? F69F C69A F74B 60.0(17) . 3_666 ? F69D C69A F74B 66.5(18) . 3_666 ? C54 C69A F74B 173.9(19) . 3_666 ? F70C C70 F70A 114(3) . . ? F70C C70 F70B 108.6(19) . . ? F70A C70 F70B 104.7(18) . . ? F70C C70 C44 112.2(17) . . ? F70A C70 C44 109.6(16) . . ? F70B C70 C44 107(2) . . ? F71C C71 F71A 108.0(17) . . ? F71C C71 F71B 107.8(19) . . ? F71A C71 F71B 105.7(14) . . ? F71C C71 C46 112.2(13) . . ? F71A C71 C46 113.0(17) . . ? F71B C71 C46 109.9(14) . . ? F72C C72 F72A 112(3) . . ? F72C C72 F72B 101(2) . . ? F72A C72 F72B 104(2) . . ? F72C C72 C49 112(3) . . ? F72A C72 C49 116(2) . . ? F72B C72 C49 111(2) . . ? F73A C73 F73C 114(3) . . ? F73A C73 C51 119(5) . . ? F73C C73 C51 107(3) . . ? F73A C73 F73B 124(3) . . ? F73C C73 F73B 88(3) . . ? C51 C73 F73B 100(2) . . ? F74A C74 F74B 105(2) . . ? F74A C74 F74C 103(2) . . ? F74B C74 F74C 108(2) . . ? F74A C74 C57 115.3(19) . . ? F74B C74 C57 118(2) . . ? F74C C74 C57 106.1(18) . . ? F74E C74A F74D 96(4) . . ? F74E C74A F69C 110(3) . 3_666 ? F74D C74A F69C 90(3) . 3_666 ? F74E C74A C60 131(4) . . ? F74D C74A C60 106(3) . . ? F69C C74A C60 114(3) 3_666 . ? _diffrn_measured_fraction_theta_max 0.763 _diffrn_reflns_theta_full 33.70 _diffrn_measured_fraction_theta_full 0.763 _refine_diff_density_max 0.853 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.121 # Attachment '60-14-II.CIF' data_on7p4m _database_code_depnum_ccdc_archive 'CCDC 652166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 F42' _chemical_formula_weight 1686.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.1180(3) _cell_length_b 11.1525(3) _cell_length_c 12.2892(3) _cell_angle_alpha 69.8720(10) _cell_angle_beta 70.1330(10) _cell_angle_gamma 76.8920(10) _cell_volume 1335.12(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13001 _cell_measurement_theta_min 5 _cell_measurement_theta_max 30 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 0.226 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.1 at the PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14005 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 5.30 _diffrn_reflns_theta_max 33.96 _reflns_number_total 8341 _reflns_number_gt 8015 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1800P)^2^+0.1400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 8341 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1806 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.7244(4) 0.2457(5) 0.2180(5) 0.0406(10) Uani 1 1 d . . . C2 C 0.6335(4) 0.3721(5) 0.2033(4) 0.0331(9) Uani 1 1 d . . . C3 C 0.6922(4) 0.4744(4) 0.2175(4) 0.0349(9) Uani 1 1 d . . . C4 C 0.7822(4) 0.3891(4) 0.2930(4) 0.0320(9) Uani 1 1 d . . . C5 C 0.7979(4) 0.2650(4) 0.2930(4) 0.0333(10) Uani 1 1 d . . . C6 C 0.8532(4) 0.1518(4) 0.3834(4) 0.0348(9) Uani 1 1 d . . . C7 C 0.7678(4) 0.0418(4) 0.4402(4) 0.0373(10) Uani 1 1 d . . . C8 C 0.6912(4) 0.0108(5) 0.3745(4) 0.0368(10) Uani 1 1 d . . . C9 C 0.6495(4) 0.1335(4) 0.2849(4) 0.0312(9) Uani 1 1 d . . . C10 C 0.5203(4) 0.1445(4) 0.3025(4) 0.0321(9) Uani 1 1 d . . . C11 C 0.4399(4) 0.2636(5) 0.2498(4) 0.0387(10) Uani 1 1 d . . . C12 C 0.5086(4) 0.3819(4) 0.2127(4) 0.0357(9) Uani 1 1 d . . . C13 C 0.4101(4) 0.4950(4) 0.2443(4) 0.0362(10) Uani 1 1 d . . . C14 C 0.4618(4) 0.5651(4) 0.3002(4) 0.0327(9) Uani 1 1 d . . . C15 C 0.5890(4) 0.5512(4) 0.2914(4) 0.0334(9) Uani 1 1 d . . . C16 C 0.6074(4) 0.5811(5) 0.3911(4) 0.0354(9) Uani 1 1 d . . . C17 C 0.7066(4) 0.5178(4) 0.4404(4) 0.0314(9) Uani 1 1 d . . . C18 C 0.8216(4) 0.4305(4) 0.3815(4) 0.0321(8) Uani 1 1 d . . . C19 C 0.8282(4) 0.3165(5) 0.4930(4) 0.0353(9) Uani 1 1 d . . . C20 C 0.8395(4) 0.1916(4) 0.4936(4) 0.0324(9) Uani 1 1 d . . . C21 C 0.7807(4) 0.0967(4) 0.6016(4) 0.0333(9) Uani 1 1 d . . . C22 C 0.7382(4) 0.0077(4) 0.5612(4) 0.0354(9) Uani 1 1 d . . . C23 C 0.6362(4) -0.0782(4) 0.6521(4) 0.0327(9) Uani 1 1 d . . . C24 C 0.5349(4) -0.0661(4) 0.5877(4) 0.0344(9) Uani 1 1 d . . . C25 C 0.5616(4) -0.0275(4) 0.4649(4) 0.0312(9) Uani 1 1 d . . . C26 C 0.4607(4) 0.0461(4) 0.4130(4) 0.0341(9) Uani 1 1 d . . . C27 C 0.3405(4) 0.0721(5) 0.4849(4) 0.0322(9) Uani 1 1 d . . . C28 C 0.2664(4) 0.2025(5) 0.4500(4) 0.0359(10) Uani 1 1 d . . . C29 C 0.3173(4) 0.2942(5) 0.3449(4) 0.0336(9) Uani 1 1 d . . . C30 C 0.3027(4) 0.4237(4) 0.3432(4) 0.0350(9) Uani 1 1 d . . . C31 C 0.2373(4) 0.4523(4) 0.4521(4) 0.0343(9) Uani 1 1 d . . . C32 C 0.2787(4) 0.5429(4) 0.4902(4) 0.0330(9) Uani 1 1 d . . . C33 C 0.3817(4) 0.6252(4) 0.4031(4) 0.0349(9) Uani 1 1 d . . . C34 C 0.4812(4) 0.6147(4) 0.4667(4) 0.0321(9) Uani 1 1 d . . . C35 C 0.4572(4) 0.5757(4) 0.5904(4) 0.0350(9) Uani 1 1 d . . . C36 C 0.5564(4) 0.5026(4) 0.6425(4) 0.0351(9) Uani 1 1 d . . . C37 C 0.6824(4) 0.4742(4) 0.5683(4) 0.0371(10) Uani 1 1 d . . . C38 C 0.7559(4) 0.3525(4) 0.5998(4) 0.0332(9) Uani 1 1 d . . . C39 C 0.7017(4) 0.2583(5) 0.7049(4) 0.0345(9) Uani 1 1 d . . . C40 C 0.7199(4) 0.1270(4) 0.7059(4) 0.0322(8) Uani 1 1 d . . . C41 C 0.6126(4) 0.0547(4) 0.8072(4) 0.0312(9) Uani 1 1 d . . . C42 C 0.5552(4) -0.0156(4) 0.7523(4) 0.0345(9) Uani 1 1 d . . . C43 C 0.4306(4) -0.0023(4) 0.7612(4) 0.0307(8) Uani 1 1 d . . . C44 C 0.4120(4) -0.0302(4) 0.6609(4) 0.0318(9) Uani 1 1 d . . . C45 C 0.3126(4) 0.0308(4) 0.6115(4) 0.0348(9) Uani 1 1 d . . . C46 C 0.1982(4) 0.1178(4) 0.6699(4) 0.0354(10) Uani 1 1 d . . . C47 C 0.1904(4) 0.2352(4) 0.5571(4) 0.0335(9) Uani 1 1 d . . . C48 C 0.1766(4) 0.3616(4) 0.5564(4) 0.0328(9) Uani 1 1 d . . . C49 C 0.1647(4) 0.3991(4) 0.6688(4) 0.0336(9) Uani 1 1 d . . . C50 C 0.2492(4) 0.5103(4) 0.6115(4) 0.0323(9) Uani 1 1 d . . . C51 C 0.3256(4) 0.5407(4) 0.6795(4) 0.0323(9) Uani 1 1 d . . . C52 C 0.3704(4) 0.4147(5) 0.7664(4) 0.0376(10) Uani 1 1 d . . . C53 C 0.5042(4) 0.4054(5) 0.7496(4) 0.0360(10) Uani 1 1 d . . . C54 C 0.5749(4) 0.2850(5) 0.7838(4) 0.0352(9) Uani 1 1 d . . . C55 C 0.5132(4) 0.1706(4) 0.8328(4) 0.0337(9) Uani 1 1 d . . . C56 C 0.3852(4) 0.1801(4) 0.8457(4) 0.0344(9) Uani 1 1 d . . . C57 C 0.3227(4) 0.0778(4) 0.8327(4) 0.0336(9) Uani 1 1 d . . . C58 C 0.2330(4) 0.1616(4) 0.7578(4) 0.0332(9) Uani 1 1 d . . . C59 C 0.2205(4) 0.2869(4) 0.7529(4) 0.0326(9) Uani 1 1 d . . . C60 C 0.3123(4) 0.3049(5) 0.8089(4) 0.0378(10) Uani 1 1 d . . . C61 C 0.8124(5) 0.2339(5) 0.0877(4) 0.0435(11) Uani 1 1 d . . . C62 C 0.7622(4) 0.5680(5) 0.0955(4) 0.0400(11) Uani 1 1 d . . . C63 C 0.9966(4) 0.1020(5) 0.3287(4) 0.0375(10) Uani 1 1 d . . . C64 C 0.7585(4) -0.0993(5) 0.3148(5) 0.0411(11) Uani 1 1 d . . . C65 C 0.4043(5) 0.2423(5) 0.1451(4) 0.0443(11) Uani 1 1 d . . . C66 C 0.3660(4) 0.5880(5) 0.1310(4) 0.0385(10) Uani 1 1 d . . . C67 C 0.9414(4) 0.4990(5) 0.3247(4) 0.0371(9) Uani 1 1 d . . . C68 C 0.6926(4) -0.2176(4) 0.7020(5) 0.0364(9) Uani 1 1 d . . . C69 C 0.3258(5) 0.7660(5) 0.3540(5) 0.0441(11) Uani 1 1 d . . . C70 C 0.6574(5) -0.0289(5) 0.9186(5) 0.0413(11) Uani 1 1 d . . . C71 C 0.0754(4) 0.0489(5) 0.7224(5) 0.0391(10) Uani 1 1 d . . . C72 C 0.0231(4) 0.4487(4) 0.7239(5) 0.0376(10) Uani 1 1 d . . . C73 C 0.2559(5) 0.6442(5) 0.7455(4) 0.0394(10) Uani 1 1 d . . . C74 C 0.2532(5) -0.0088(5) 0.9578(4) 0.0376(10) Uani 1 1 d . . . F1 F 0.8451(4) 0.1140(4) 0.0856(4) 0.0679(10) Uani 1 1 d . . . F2 F 0.9243(3) 0.2812(4) 0.0553(3) 0.0667(10) Uani 1 1 d . . . F3 F 0.7531(4) 0.2928(6) 0.0055(4) 0.0875(15) Uani 1 1 d . . . F4 F 0.7600(3) 0.6835(3) 0.1094(3) 0.0473(7) Uani 1 1 d . . . F5 F 0.8839(3) 0.5247(3) 0.0536(3) 0.0545(8) Uani 1 1 d . . . F6 F 0.7010(4) 0.5897(4) 0.0126(3) 0.0566(9) Uani 1 1 d . . . F7 F 1.0736(3) 0.1845(3) 0.3136(4) 0.0584(9) Uani 1 1 d . . . F8 F 1.0167(3) 0.0810(4) 0.2244(3) 0.0560(9) Uani 1 1 d . . . F9 F 1.0325(3) -0.0073(3) 0.4058(4) 0.0572(9) Uani 1 1 d . . . F10 F 0.6944(3) -0.1122(4) 0.2496(3) 0.0583(9) Uani 1 1 d . . . F11 F 0.7646(5) -0.2130(3) 0.3999(4) 0.0695(10) Uani 1 1 d . . . F12 F 0.8797(3) -0.0881(4) 0.2536(4) 0.0765(13) Uani 1 1 d . . . F13 F 0.5030(4) 0.2572(4) 0.0440(3) 0.0636(10) Uani 1 1 d . . . F14 F 0.3705(3) 0.1255(3) 0.1787(3) 0.0535(8) Uani 1 1 d . . . F15 F 0.3052(3) 0.3245(4) 0.1178(3) 0.0560(8) Uani 1 1 d . . . F16 F 0.4100(4) 0.5384(4) 0.0396(3) 0.0642(9) Uani 1 1 d . . . F17 F 0.2392(3) 0.6189(4) 0.1568(4) 0.0636(10) Uani 1 1 d . . . F18 F 0.4160(3) 0.6995(3) 0.0922(3) 0.0545(8) Uani 1 1 d . . . F19 F 0.9237(3) 0.6106(3) 0.2397(3) 0.0436(6) Uani 1 1 d . . . F20 F 1.0438(3) 0.4281(3) 0.2742(3) 0.0496(8) Uani 1 1 d . . . F21 F 0.9701(3) 0.5287(3) 0.4092(3) 0.0473(7) Uani 1 1 d . . . F22 F 0.6057(4) -0.2802(3) 0.7932(4) 0.0671(11) Uani 1 1 d . . . F23 F 0.7323(4) -0.2817(3) 0.6215(3) 0.0608(9) Uani 1 1 d . . . F24 F 0.7944(3) -0.2232(4) 0.7381(4) 0.0649(10) Uani 1 1 d . . . F25 F 0.4176(3) 0.8351(3) 0.2705(3) 0.0484(7) Uani 1 1 d . . . F26 F 0.2356(3) 0.7723(3) 0.3020(3) 0.0506(7) Uani 1 1 d . . . F27 F 0.2730(3) 0.8222(3) 0.4410(3) 0.0496(7) Uani 1 1 d . . . F28 F 0.6816(4) 0.0464(4) 0.9712(3) 0.0675(10) Uani 1 1 d . . . F29 F 0.7678(3) -0.0977(4) 0.8870(3) 0.0620(9) Uani 1 1 d . . . F30 F 0.5723(4) -0.1019(4) 1.0006(3) 0.0666(10) Uani 1 1 d . . . F31 F 0.0896(3) -0.0574(3) 0.8094(3) 0.0423(6) Uani 1 1 d . . . F32 F 0.0520(3) 0.0181(3) 0.6368(3) 0.0432(6) Uani 1 1 d . . . F33 F -0.0284(3) 0.1231(3) 0.7676(3) 0.0501(8) Uani 1 1 d . . . F34 F -0.0167(3) 0.5534(4) 0.6478(4) 0.0594(9) Uani 1 1 d . . . F35 F 0.0075(3) 0.4768(4) 0.8234(3) 0.0604(10) Uani 1 1 d . . . F36 F -0.0557(3) 0.3626(3) 0.7521(4) 0.0588(9) Uani 1 1 d . . . F37 F 0.3410(3) 0.6820(4) 0.7783(3) 0.0551(8) Uani 1 1 d . . . F38 F 0.2037(4) 0.7444(4) 0.6783(4) 0.0728(12) Uani 1 1 d . . . F39 F 0.1684(3) 0.5953(3) 0.8492(3) 0.0629(10) Uani 1 1 d . . . F40 F 0.3164(3) -0.0310(3) 1.0374(3) 0.0482(7) Uani 1 1 d . . . F41 F 0.2405(3) -0.1212(3) 0.9518(3) 0.0483(7) Uani 1 1 d . . . F42 F 0.1347(3) 0.0487(4) 0.9984(3) 0.0558(8) 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 0.046(2) 0.036(2) 0.044(2) -0.016(2) -0.018(2) 0.0015(19) C2 0.0406(19) 0.038(2) 0.0218(17) -0.0121(19) -0.0131(17) 0.0039(18) C3 0.042(2) 0.031(2) 0.031(2) -0.011(2) -0.0126(18) 0.0032(18) C4 0.0333(17) 0.034(2) 0.029(2) -0.0174(19) -0.0070(16) 0.0035(16) C5 0.0357(18) 0.032(2) 0.036(2) -0.022(2) -0.0101(17) 0.0067(16) C6 0.0399(19) 0.031(2) 0.031(2) -0.012(2) -0.0115(17) 0.0069(18) C7 0.0363(18) 0.036(2) 0.045(3) -0.027(2) -0.0117(18) 0.0086(17) C8 0.044(2) 0.034(2) 0.037(2) -0.023(2) -0.0086(19) 0.0017(18) C9 0.0387(18) 0.035(2) 0.0233(18) -0.0162(19) -0.0105(16) 0.0035(17) C10 0.0442(19) 0.033(2) 0.0241(18) -0.0149(19) -0.0113(17) -0.0020(17) C11 0.042(2) 0.040(2) 0.036(2) -0.018(2) -0.0119(19) 0.0017(18) C12 0.044(2) 0.034(2) 0.030(2) -0.015(2) -0.0127(18) 0.0045(17) C13 0.0396(19) 0.032(2) 0.038(2) -0.015(2) -0.0121(18) 0.0023(18) C14 0.0391(18) 0.028(2) 0.034(2) -0.011(2) -0.0173(17) 0.0026(16) C15 0.0398(19) 0.032(2) 0.031(2) -0.010(2) -0.0179(18) 0.0031(17) C16 0.046(2) 0.033(2) 0.032(2) -0.015(2) -0.0158(19) -0.0006(18) C17 0.0420(19) 0.0245(19) 0.029(2) -0.0085(19) -0.0139(17) 0.0002(16) C18 0.0398(19) 0.0280(19) 0.028(2) -0.0067(19) -0.0164(17) 0.0037(16) C19 0.0365(17) 0.036(2) 0.038(2) -0.016(2) -0.0172(18) 0.0043(17) C20 0.0338(17) 0.031(2) 0.033(2) -0.012(2) -0.0134(17) 0.0050(16) C21 0.0355(18) 0.029(2) 0.040(2) -0.012(2) -0.0176(18) 0.0020(16) C22 0.0398(19) 0.030(2) 0.040(2) -0.020(2) -0.0130(18) 0.0070(16) C23 0.0354(17) 0.031(2) 0.035(2) -0.016(2) -0.0136(18) 0.0070(16) C24 0.045(2) 0.0246(19) 0.038(2) -0.012(2) -0.020(2) 0.0049(16) C25 0.0365(18) 0.0278(19) 0.034(2) -0.0133(19) -0.0155(17) 0.0013(16) C26 0.0404(19) 0.030(2) 0.035(2) -0.013(2) -0.0128(18) -0.0019(17) C27 0.0358(17) 0.033(2) 0.032(2) -0.014(2) -0.0135(17) 0.0010(16) C28 0.0369(19) 0.038(2) 0.041(2) -0.020(2) -0.0171(18) 0.0037(17) C29 0.048(2) 0.032(2) 0.0230(18) -0.0062(19) -0.0200(18) 0.0020(18) C30 0.0411(19) 0.032(2) 0.039(2) -0.019(2) -0.0178(19) 0.0050(17) C31 0.0413(19) 0.033(2) 0.033(2) -0.015(2) -0.0177(18) 0.0049(17) C32 0.0346(17) 0.028(2) 0.040(2) -0.018(2) -0.0145(17) 0.0067(16) C33 0.041(2) 0.030(2) 0.036(2) -0.015(2) -0.0117(19) 0.0005(17) C34 0.0402(19) 0.0268(19) 0.034(2) -0.0169(19) -0.0127(18) 0.0029(16) C35 0.045(2) 0.0274(19) 0.034(2) -0.013(2) -0.0158(19) 0.0065(17) C36 0.046(2) 0.032(2) 0.033(2) -0.017(2) -0.0156(19) 0.0009(18) C37 0.043(2) 0.035(2) 0.043(2) -0.022(2) -0.015(2) -0.0002(18) C38 0.0401(18) 0.036(2) 0.032(2) -0.019(2) -0.0127(17) -0.0035(17) C39 0.0379(18) 0.039(2) 0.034(2) -0.021(2) -0.0120(17) -0.0005(17) C40 0.0388(18) 0.027(2) 0.032(2) -0.0044(19) -0.0196(17) 0.0036(16) C41 0.0395(18) 0.031(2) 0.0236(19) -0.0065(19) -0.0173(17) 0.0043(17) C42 0.044(2) 0.028(2) 0.0284(19) -0.0087(19) -0.0126(18) 0.0063(17) C43 0.0392(18) 0.0214(17) 0.030(2) -0.0073(18) -0.0134(18) 0.0040(15) C44 0.0378(18) 0.0215(18) 0.036(2) -0.0110(19) -0.0128(18) 0.0033(15) C45 0.0376(19) 0.030(2) 0.043(2) -0.019(2) -0.0140(18) 0.0014(16) C46 0.0347(19) 0.035(2) 0.039(2) -0.020(2) -0.0064(17) -0.0018(17) C47 0.0370(18) 0.034(2) 0.033(2) -0.015(2) -0.0102(17) -0.0018(17) C48 0.0344(18) 0.036(2) 0.033(2) -0.017(2) -0.0123(17) 0.0016(17) C49 0.0340(18) 0.036(2) 0.036(2) -0.022(2) -0.0108(17) 0.0045(16) C50 0.0368(18) 0.0255(19) 0.035(2) -0.012(2) -0.0137(18) 0.0052(16) C51 0.0405(19) 0.030(2) 0.030(2) -0.0165(19) -0.0124(17) 0.0045(17) C52 0.047(2) 0.038(2) 0.033(2) -0.022(2) -0.0114(19) 0.0022(19) C53 0.043(2) 0.039(2) 0.033(2) -0.023(2) -0.0113(18) 0.0012(17) C54 0.047(2) 0.038(2) 0.0260(19) -0.018(2) -0.0139(18) 0.0021(18) C55 0.047(2) 0.033(2) 0.0247(19) -0.0129(19) -0.0155(18) 0.0040(18) C56 0.044(2) 0.035(2) 0.0274(18) -0.0166(18) -0.0075(17) -0.0026(18) C57 0.0373(18) 0.036(2) 0.0270(19) -0.014(2) -0.0074(16) 0.0017(17) C58 0.0376(18) 0.033(2) 0.029(2) -0.0099(19) -0.0125(17) 0.0004(17) C59 0.0397(19) 0.033(2) 0.0230(19) -0.0058(19) -0.0128(17) 0.0007(17) C60 0.0415(19) 0.038(2) 0.037(2) -0.018(2) -0.0134(18) 0.0038(18) C61 0.049(2) 0.045(3) 0.039(2) -0.018(2) -0.015(2) 0.003(2) C62 0.041(2) 0.044(3) 0.035(2) -0.012(2) -0.0116(19) -0.003(2) C63 0.042(2) 0.039(2) 0.035(2) -0.019(2) -0.0158(19) 0.0084(19) C64 0.0388(19) 0.040(2) 0.049(3) -0.031(2) -0.0047(19) 0.0014(18) C65 0.048(2) 0.050(3) 0.039(2) -0.019(2) -0.015(2) -0.001(2) C66 0.041(2) 0.044(3) 0.031(2) -0.006(2) -0.0167(19) -0.005(2) C67 0.045(2) 0.034(2) 0.036(2) -0.011(2) -0.0194(19) 0.0023(18) C68 0.0433(19) 0.028(2) 0.042(2) -0.011(2) -0.020(2) 0.0029(17) C69 0.045(2) 0.038(2) 0.052(3) -0.019(3) -0.017(2) 0.002(2) C70 0.046(2) 0.034(2) 0.041(2) -0.016(2) -0.007(2) -0.0021(19) C71 0.0337(18) 0.044(3) 0.044(3) -0.021(2) -0.0120(19) 0.0006(18) C72 0.0328(18) 0.034(2) 0.045(3) -0.016(2) -0.0114(19) 0.0062(17) C73 0.052(2) 0.033(2) 0.035(2) -0.015(2) -0.016(2) 0.007(2) C74 0.045(2) 0.038(2) 0.029(2) -0.009(2) -0.0125(19) -0.0024(19) F1 0.078(2) 0.061(2) 0.062(2) -0.0365(19) 0.0006(17) -0.0074(17) F2 0.0620(17) 0.092(3) 0.0525(18) -0.037(2) -0.0015(15) -0.0200(19) F3 0.079(2) 0.130(4) 0.047(2) -0.041(3) -0.0213(19) 0.028(3) F4 0.0573(15) 0.0383(15) 0.0464(15) -0.0088(14) -0.0189(13) -0.0054(12) F5 0.0463(14) 0.0544(18) 0.0493(17) -0.0127(16) -0.0021(13) -0.0020(13) F6 0.0676(18) 0.072(2) 0.0363(14) -0.0052(16) -0.0259(15) -0.0209(17) F7 0.0370(12) 0.0559(18) 0.087(2) -0.0415(19) -0.0041(15) -0.0039(12) F8 0.0467(14) 0.080(2) 0.0479(17) -0.0400(19) -0.0069(14) 0.0038(15) F9 0.0455(14) 0.0501(19) 0.059(2) -0.0112(18) -0.0160(14) 0.0194(14) F10 0.0749(18) 0.0566(19) 0.065(2) -0.0438(19) -0.0349(16) 0.0136(15) F11 0.112(3) 0.0371(17) 0.067(2) -0.0282(18) -0.041(2) 0.0211(17) F12 0.0555(17) 0.074(2) 0.102(3) -0.064(2) 0.0172(19) -0.0115(16) F13 0.0608(15) 0.094(3) 0.0495(19) -0.045(2) -0.0093(15) -0.0084(17) F14 0.0741(18) 0.0510(17) 0.0502(16) -0.0218(15) -0.0293(15) -0.0071(14) F15 0.0692(17) 0.061(2) 0.0468(17) -0.0215(17) -0.0320(15) 0.0077(15) F16 0.097(2) 0.061(2) 0.0413(16) -0.0214(17) -0.0299(17) 0.0040(19) F17 0.0457(14) 0.079(3) 0.0508(18) 0.0025(19) -0.0226(14) 0.0018(15) F18 0.0655(17) 0.0462(17) 0.0538(17) -0.0032(15) -0.0264(15) -0.0142(14) F19 0.0517(14) 0.0380(15) 0.0392(14) -0.0059(14) -0.0152(12) -0.0068(12) F20 0.0395(12) 0.0448(16) 0.062(2) -0.0224(16) -0.0085(13) 0.0010(12) F21 0.0565(15) 0.0506(18) 0.0443(16) -0.0126(15) -0.0239(13) -0.0120(14) F22 0.0596(18) 0.0379(16) 0.072(2) 0.0021(17) -0.0073(17) 0.0081(14) F23 0.088(2) 0.0414(17) 0.064(2) -0.0312(18) -0.0380(19) 0.0209(16) F24 0.0666(19) 0.0416(17) 0.103(3) -0.020(2) -0.057(2) 0.0112(14) F25 0.0570(15) 0.0278(13) 0.0531(17) -0.0058(13) -0.0131(14) -0.0046(12) F26 0.0565(15) 0.0368(15) 0.0629(19) -0.0121(15) -0.0346(15) 0.0090(12) F27 0.0611(16) 0.0285(12) 0.0573(18) -0.0208(14) -0.0173(14) 0.0115(12) F28 0.115(3) 0.0536(19) 0.054(2) -0.0177(18) -0.059(2) 0.0095(19) F29 0.0616(18) 0.066(2) 0.0422(18) -0.0065(18) -0.0260(15) 0.0257(16) F30 0.0609(17) 0.080(3) 0.0466(17) 0.0129(18) -0.0238(16) -0.0220(18) F31 0.0502(13) 0.0355(14) 0.0399(15) -0.0048(14) -0.0168(12) -0.0065(12) F32 0.0446(12) 0.0463(15) 0.0469(15) -0.0177(14) -0.0199(12) -0.0042(11) F33 0.0383(12) 0.0431(15) 0.065(2) -0.0245(16) -0.0036(13) -0.0011(12) F34 0.0460(14) 0.056(2) 0.059(2) -0.0157(19) -0.0070(15) 0.0132(15) F35 0.0505(15) 0.088(3) 0.0518(18) -0.048(2) -0.0105(14) 0.0101(16) F36 0.0372(13) 0.0528(18) 0.087(2) -0.0374(19) -0.0044(14) -0.0014(12) F37 0.0579(16) 0.0605(19) 0.0623(19) -0.0447(17) -0.0134(14) -0.0010(14) F38 0.111(3) 0.0495(19) 0.072(2) -0.043(2) -0.050(2) 0.038(2) F39 0.0627(17) 0.0611(19) 0.0611(19) -0.0424(18) 0.0137(15) -0.0104(15) F40 0.0674(17) 0.0487(17) 0.0302(13) -0.0005(14) -0.0238(13) -0.0124(14) F41 0.0660(17) 0.0359(14) 0.0411(15) -0.0047(13) -0.0188(14) -0.0078(13) F42 0.0484(14) 0.0571(18) 0.0394(15) -0.0086(15) -0.0012(13) 0.0104(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.495(6) . ? C1 C5 1.513(6) . ? C1 C2 1.531(7) . ? C1 C61 1.600(6) . ? C2 C12 1.335(6) . ? C2 C3 1.521(6) . ? C3 C15 1.502(5) . ? C3 C4 1.535(7) . ? C3 C62 1.562(6) . ? C4 C5 1.355(6) . ? C4 C18 1.533(6) . ? C5 C6 1.534(7) . ? C6 C20 1.515(6) . ? C6 C7 1.543(6) . ? C6 C63 1.560(6) . ? C7 C22 1.342(7) . ? C7 C8 1.513(6) . ? C8 C9 1.523(7) . ? C8 C25 1.535(6) . ? C8 C64 1.561(5) . ? C9 C10 1.362(6) . ? C10 C26 1.476(6) . ? C10 C11 1.499(7) . ? C11 C29 1.523(6) . ? C11 C12 1.529(6) . ? C11 C65 1.572(6) . ? C12 C13 1.538(6) . ? C13 C14 1.501(5) . ? C13 C30 1.522(6) . ? C13 C66 1.580(8) . ? C14 C15 1.358(6) . ? C14 C33 1.545(5) . ? C15 C16 1.461(6) . ? C16 C17 1.375(7) . ? C16 C34 1.445(6) . ? C17 C37 1.423(7) . ? C17 C18 1.549(6) . ? C18 C67 1.519(6) . ? C18 C19 1.525(7) . ? C19 C20 1.367(6) . ? C19 C38 1.425(5) . ? C20 C21 1.437(6) . ? C21 C40 1.349(6) . ? C21 C22 1.471(5) . ? C22 C23 1.532(6) . ? C23 C68 1.533(6) . ? C23 C42 1.538(5) . ? C23 C24 1.541(6) . ? C24 C25 1.363(7) . ? C24 C44 1.414(6) . ? C25 C26 1.431(7) . ? C26 C27 1.360(6) . ? C27 C45 1.405(7) . ? C27 C28 1.498(6) . ? C28 C29 1.375(7) . ? C28 C47 1.420(6) . ? C29 C30 1.410(6) . ? C30 C31 1.396(6) . ? C31 C48 1.396(7) . ? C31 C32 1.461(5) . ? C32 C50 1.345(7) . ? C32 C33 1.505(6) . ? C33 C34 1.522(6) . ? C33 C69 1.541(7) . ? C34 C35 1.376(6) . ? C35 C36 1.415(7) . ? C35 C51 1.538(6) . ? C36 C37 1.423(6) . ? C36 C53 1.425(7) . ? C37 C38 1.418(7) . ? C38 C39 1.399(7) . ? C39 C40 1.428(6) . ? C39 C54 1.448(6) . ? C40 C41 1.536(6) . ? C41 C42 1.537(6) . ? C41 C70 1.538(8) . ? C41 C55 1.545(6) . ? C42 C43 1.329(6) . ? C43 C44 1.459(6) . ? C43 C57 1.531(5) . ? C44 C45 1.372(7) . ? C45 C46 1.541(5) . ? C46 C58 1.513(6) . ? C46 C71 1.551(5) . ? C46 C47 1.556(7) . ? C47 C48 1.381(6) . ? C48 C49 1.533(5) . ? C49 C59 1.487(7) . ? C49 C72 1.544(5) . ? C49 C50 1.547(6) . ? C50 C51 1.531(6) . ? C51 C52 1.541(8) . ? C51 C73 1.549(5) . ? C52 C60 1.371(7) . ? C52 C53 1.415(6) . ? C53 C54 1.398(7) . ? C54 C55 1.432(6) . ? C55 C56 1.361(6) . ? C56 C60 1.450(7) . ? C56 C57 1.540(5) . ? C57 C58 1.525(7) . ? C57 C74 1.549(6) . ? C58 C59 1.354(6) . ? C59 C60 1.490(6) . ? C61 F3 1.299(7) . ? C61 F1 1.310(6) . ? C61 F2 1.342(6) . ? C62 F5 1.315(6) . ? C62 F6 1.338(6) . ? C62 F4 1.350(6) . ? C63 F8 1.317(5) . ? C63 F7 1.321(6) . ? C63 F9 1.336(7) . ? C64 F10 1.298(6) . ? C64 F12 1.311(6) . ? C64 F11 1.343(7) . ? C65 F15 1.322(7) . ? C65 F14 1.325(6) . ? C65 F13 1.338(6) . ? C66 F16 1.318(5) . ? C66 F17 1.326(6) . ? C66 F18 1.344(6) . ? C67 F20 1.326(5) . ? C67 F21 1.342(5) . ? C67 F19 1.346(7) . ? C68 F22 1.307(6) . ? C68 F23 1.316(5) . ? C68 F24 1.332(6) . ? C69 F27 1.323(6) . ? C69 F25 1.338(6) . ? C69 F26 1.338(6) . ? C70 F29 1.303(6) . ? C70 F30 1.308(6) . ? C70 F28 1.338(6) . ? C71 F31 1.316(7) . ? C71 F32 1.330(5) . ? C71 F33 1.332(5) . ? C72 F35 1.310(6) . ? C72 F34 1.314(7) . ? C72 F36 1.325(6) . ? C73 F38 1.289(7) . ? C73 F39 1.337(6) . ? C73 F37 1.339(6) . ? C74 F40 1.317(6) . ? C74 F41 1.323(5) . ? C74 F42 1.337(6) . ? 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 C9 C1 C5 111.6(4) . . ? C9 C1 C2 110.6(4) . . ? C5 C1 C2 100.2(3) . . ? C9 C1 C61 110.5(4) . . ? C5 C1 C61 113.8(4) . . ? C2 C1 C61 109.6(4) . . ? C12 C2 C3 123.2(4) . . ? C12 C2 C1 124.6(4) . . ? C3 C2 C1 109.5(4) . . ? C15 C3 C2 109.4(3) . . ? C15 C3 C4 109.1(4) . . ? C2 C3 C4 100.3(4) . . ? C15 C3 C62 109.2(4) . . ? C2 C3 C62 114.4(4) . . ? C4 C3 C62 114.0(4) . . ? C5 C4 C18 123.2(4) . . ? C5 C4 C3 111.2(4) . . ? C18 C4 C3 124.0(4) . . ? C4 C5 C1 112.6(4) . . ? C4 C5 C6 123.5(4) . . ? C1 C5 C6 122.1(4) . . ? C20 C6 C5 109.2(3) . . ? C20 C6 C7 101.0(3) . . ? C5 C6 C7 111.2(4) . . ? C20 C6 C63 110.1(4) . . ? C5 C6 C63 113.2(4) . . ? C7 C6 C63 111.4(3) . . ? C22 C7 C8 122.9(4) . . ? C22 C7 C6 110.1(4) . . ? C8 C7 C6 123.7(4) . . ? C7 C8 C9 109.8(3) . . ? C7 C8 C25 108.4(3) . . ? C9 C8 C25 102.2(3) . . ? C7 C8 C64 114.9(4) . . ? C9 C8 C64 112.3(4) . . ? C25 C8 C64 108.5(3) . . ? C10 C9 C1 122.2(4) . . ? C10 C9 C8 109.6(4) . . ? C1 C9 C8 125.3(4) . . ? C9 C10 C26 110.8(4) . . ? C9 C10 C11 125.0(4) . . ? C26 C10 C11 120.5(4) . . ? C10 C11 C29 111.6(4) . . ? C10 C11 C12 110.3(4) . . ? C29 C11 C12 102.0(3) . . ? C10 C11 C65 108.4(4) . . ? C29 C11 C65 109.8(4) . . ? C12 C11 C65 114.8(4) . . ? C2 C12 C11 122.1(4) . . ? C2 C12 C13 122.9(4) . . ? C11 C12 C13 109.6(4) . . ? C14 C13 C30 107.6(4) . . ? C14 C13 C12 110.8(4) . . ? C30 C13 C12 100.9(4) . . ? C14 C13 C66 112.2(4) . . ? C30 C13 C66 113.2(4) . . ? C12 C13 C66 111.6(4) . . ? C15 C14 C13 122.4(4) . . ? C15 C14 C33 109.6(4) . . ? C13 C14 C33 125.5(3) . . ? C14 C15 C16 110.9(4) . . ? C14 C15 C3 124.0(4) . . ? C16 C15 C3 122.1(4) . . ? C17 C16 C34 120.8(4) . . ? C17 C16 C15 121.7(4) . . ? C34 C16 C15 107.4(4) . . ? C16 C17 C37 119.8(4) . . ? C16 C17 C18 123.5(4) . . ? C37 C17 C18 109.8(4) . . ? C67 C18 C19 113.8(4) . . ? C67 C18 C4 114.3(4) . . ? C19 C18 C4 109.7(3) . . ? C67 C18 C17 110.0(3) . . ? C19 C18 C17 99.5(3) . . ? C4 C18 C17 108.5(3) . . ? C20 C19 C38 119.5(4) . . ? C20 C19 C18 122.8(4) . . ? C38 C19 C18 109.9(4) . . ? C19 C20 C21 120.4(4) . . ? C19 C20 C6 123.9(4) . . ? C21 C20 C6 109.8(3) . . ? C40 C21 C20 120.9(4) . . ? C40 C21 C22 124.5(4) . . ? C20 C21 C22 106.1(4) . . ? C7 C22 C21 111.3(4) . . ? C7 C22 C23 126.9(4) . . ? C21 C22 C23 118.8(4) . . ? C22 C23 C68 113.3(4) . . ? C22 C23 C42 109.6(3) . . ? C68 C23 C42 112.8(4) . . ? C22 C23 C24 106.3(4) . . ? C68 C23 C24 113.4(3) . . ? C42 C23 C24 100.5(3) . . ? C25 C24 C44 120.6(4) . . ? C25 C24 C23 122.5(4) . . ? C44 C24 C23 108.6(4) . . ? C24 C25 C26 118.1(4) . . ? C24 C25 C8 125.7(4) . . ? C26 C25 C8 108.4(4) . . ? C27 C26 C25 120.6(4) . . ? C27 C26 C10 121.3(4) . . ? C25 C26 C10 107.0(4) . . ? C26 C27 C45 121.2(4) . . ? C26 C27 C28 119.2(4) . . ? C45 C27 C28 107.8(3) . . ? C29 C28 C47 121.8(4) . . ? C29 C28 C27 120.7(4) . . ? C47 C28 C27 108.5(4) . . ? C28 C29 C30 120.3(4) . . ? C28 C29 C11 122.4(4) . . ? C30 C29 C11 110.5(4) . . ? C31 C30 C29 117.1(4) . . ? C31 C30 C13 124.7(4) . . ? C29 C30 C13 111.6(3) . . ? C30 C31 C48 122.7(4) . . ? C30 C31 C32 122.3(4) . . ? C48 C31 C32 107.6(4) . . ? C50 C32 C31 111.1(4) . . ? C50 C32 C33 125.1(4) . . ? C31 C32 C33 120.1(4) . . ? C32 C33 C34 108.2(4) . . ? C32 C33 C69 112.2(4) . . ? C34 C33 C69 112.0(3) . . ? C32 C33 C14 110.1(3) . . ? C34 C33 C14 101.9(3) . . ? C69 C33 C14 111.9(4) . . ? C35 C34 C16 119.8(4) . . ? C35 C34 C33 123.8(4) . . ? C16 C34 C33 108.5(4) . . ? C34 C35 C36 119.6(4) . . ? C34 C35 C51 123.6(4) . . ? C36 C35 C51 109.4(4) . . ? C35 C36 C37 120.8(4) . . ? C35 C36 C53 109.8(4) . . ? C37 C36 C53 118.6(4) . . ? C38 C37 C36 121.3(4) . . ? C38 C37 C17 108.6(3) . . ? C36 C37 C17 118.9(4) . . ? C39 C38 C37 118.9(4) . . ? C39 C38 C19 119.3(4) . . ? C37 C38 C19 109.5(4) . . ? C38 C39 C40 120.5(4) . . ? C38 C39 C54 121.2(4) . . ? C40 C39 C54 108.5(4) . . ? C21 C40 C39 119.0(4) . . ? C21 C40 C41 123.6(4) . . ? C39 C40 C41 110.4(4) . . ? C40 C41 C42 108.2(3) . . ? C40 C41 C70 112.4(4) . . ? C42 C41 C70 115.8(4) . . ? C40 C41 C55 99.5(4) . . ? C42 C41 C55 107.4(3) . . ? C70 C41 C55 112.2(3) . . ? C43 C42 C41 124.2(4) . . ? C43 C42 C23 110.4(4) . . ? C41 C42 C23 123.3(4) . . ? C42 C43 C44 110.9(4) . . ? C42 C43 C57 125.8(4) . . ? C44 C43 C57 119.6(4) . . ? C45 C44 C24 120.9(4) . . ? C45 C44 C43 123.1(4) . . ? C24 C44 C43 107.8(4) . . ? C44 C45 C27 118.1(4) . . ? C44 C45 C46 123.0(4) . . ? C27 C45 C46 111.3(4) . . ? C58 C46 C45 110.3(4) . . ? C58 C46 C71 115.7(4) . . ? C45 C46 C71 109.3(3) . . ? C58 C46 C47 108.5(3) . . ? C45 C46 C47 100.3(3) . . ? C71 C46 C47 111.7(4) . . ? C48 C47 C28 118.0(4) . . ? C48 C47 C46 123.7(4) . . ? C28 C47 C46 110.0(4) . . ? C47 C48 C31 119.7(4) . . ? C47 C48 C49 122.5(4) . . ? C31 C48 C49 110.0(3) . . ? C59 C49 C48 108.4(3) . . ? C59 C49 C72 114.4(4) . . ? C48 C49 C72 109.8(4) . . ? C59 C49 C50 112.1(4) . . ? C48 C49 C50 100.5(3) . . ? C72 C49 C50 110.7(3) . . ? C32 C50 C51 124.1(4) . . ? C32 C50 C49 109.7(3) . . ? C51 C50 C49 122.7(4) . . ? C50 C51 C35 108.0(3) . . ? C50 C51 C52 109.2(3) . . ? C35 C51 C52 99.5(4) . . ? C50 C51 C73 115.3(4) . . ? C35 C51 C73 112.0(3) . . ? C52 C51 C73 111.6(4) . . ? C60 C52 C53 119.7(5) . . ? C60 C52 C51 123.9(4) . . ? C53 C52 C51 110.0(4) . . ? C54 C53 C52 120.0(4) . . ? C54 C53 C36 121.5(4) . . ? C52 C53 C36 108.4(4) . . ? C53 C54 C55 120.3(4) . . ? C53 C54 C39 118.5(4) . . ? C55 C54 C39 108.3(4) . . ? C56 C55 C54 119.4(4) . . ? C56 C55 C41 124.4(3) . . ? C54 C55 C41 109.9(4) . . ? C55 C56 C60 120.3(4) . . ? C55 C56 C57 123.7(4) . . ? C60 C56 C57 108.6(4) . . ? C58 C57 C43 111.2(3) . . ? C58 C57 C56 101.4(4) . . ? C43 C57 C56 107.1(3) . . ? C58 C57 C74 114.3(4) . . ? C43 C57 C74 110.8(4) . . ? C56 C57 C74 111.5(3) . . ? C59 C58 C46 123.2(4) . . ? C59 C58 C57 111.5(4) . . ? C46 C58 C57 122.7(4) . . ? C58 C59 C49 126.5(4) . . ? C58 C59 C60 109.9(4) . . ? C49 C59 C60 120.0(4) . . ? C52 C60 C56 120.2(4) . . ? C52 C60 C59 122.0(5) . . ? C56 C60 C59 106.7(4) . . ? F3 C61 F1 107.0(5) . . ? F3 C61 F2 109.3(5) . . ? F1 C61 F2 105.1(4) . . ? F3 C61 C1 111.4(4) . . ? F1 C61 C1 112.4(4) . . ? F2 C61 C1 111.4(4) . . ? F5 C62 F6 109.5(4) . . ? F5 C62 F4 107.0(4) . . ? F6 C62 F4 106.5(4) . . ? F5 C62 C3 112.8(4) . . ? F6 C62 C3 110.1(4) . . ? F4 C62 C3 110.7(3) . . ? F8 C63 F7 108.9(4) . . ? F8 C63 F9 108.7(4) . . ? F7 C63 F9 105.8(4) . . ? F8 C63 C6 112.6(4) . . ? F7 C63 C6 110.7(3) . . ? F9 C63 C6 109.9(4) . . ? F10 C64 F12 111.4(4) . . ? F10 C64 F11 105.8(4) . . ? F12 C64 F11 103.3(5) . . ? F10 C64 C8 111.8(4) . . ? F12 C64 C8 113.3(4) . . ? F11 C64 C8 110.5(4) . . ? F15 C65 F14 106.7(4) . . ? F15 C65 F13 107.2(5) . . ? F14 C65 F13 109.3(4) . . ? F15 C65 C11 111.9(4) . . ? F14 C65 C11 110.1(4) . . ? F13 C65 C11 111.4(4) . . ? F16 C66 F17 111.0(4) . . ? F16 C66 F18 106.2(4) . . ? F17 C66 F18 106.1(4) . . ? F16 C66 C13 111.0(4) . . ? F17 C66 C13 112.4(4) . . ? F18 C66 C13 109.9(4) . . ? F20 C67 F21 107.4(4) . . ? F20 C67 F19 107.9(4) . . ? F21 C67 F19 106.7(4) . . ? F20 C67 C18 112.8(4) . . ? F21 C67 C18 110.0(4) . . ? F19 C67 C18 111.8(4) . . ? F22 C68 F23 106.7(4) . . ? F22 C68 F24 108.9(5) . . ? F23 C68 F24 106.1(4) . . ? F22 C68 C23 110.5(4) . . ? F23 C68 C23 112.8(4) . . ? F24 C68 C23 111.6(4) . . ? F27 C69 F25 107.5(4) . . ? F27 C69 F26 108.1(4) . . ? F25 C69 F26 107.5(5) . . ? F27 C69 C33 111.5(5) . . ? F25 C69 C33 111.1(4) . . ? F26 C69 C33 110.8(4) . . ? F29 C70 F30 110.7(5) . . ? F29 C70 F28 104.2(4) . . ? F30 C70 F28 107.4(4) . . ? F29 C70 C41 111.0(4) . . ? F30 C70 C41 113.4(4) . . ? F28 C70 C41 109.8(4) . . ? F31 C71 F32 108.3(4) . . ? F31 C71 F33 108.0(4) . . ? F32 C71 F33 107.4(4) . . ? F31 C71 C46 110.6(4) . . ? F32 C71 C46 110.6(4) . . ? F33 C71 C46 111.9(4) . . ? F35 C72 F34 107.5(4) . . ? F35 C72 F36 106.7(4) . . ? F34 C72 F36 107.3(4) . . ? F35 C72 C49 111.8(4) . . ? F34 C72 C49 111.1(4) . . ? F36 C72 C49 112.1(3) . . ? F38 C73 F39 110.5(5) . . ? F38 C73 F37 108.1(4) . . ? F39 C73 F37 104.9(4) . . ? F38 C73 C51 112.4(4) . . ? F39 C73 C51 111.2(4) . . ? F37 C73 C51 109.3(4) . . ? F40 C74 F41 107.8(5) . . ? F40 C74 F42 108.7(4) . . ? F41 C74 F42 107.2(4) . . ? F40 C74 C57 111.4(4) . . ? F41 C74 C57 111.9(3) . . ? F42 C74 C57 109.7(4) . . ? _diffrn_measured_fraction_theta_max 0.829 _diffrn_reflns_theta_full 33.96 _diffrn_measured_fraction_theta_full 0.829 _refine_diff_density_max 0.608 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.081 # Attachment '60BR5S.CIF' data_60br5s _database_code_depnum_ccdc_archive 'CCDC 652167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 F36' _chemical_formula_weight 1548.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca 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 17.2319(5) _cell_length_b 16.5102(3) _cell_length_c 17.6880(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5032.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14829 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 0.213 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90500 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL14.1 at the PSF, BESYY, Berlin, Germany' _diffrn_radiation_monochromator Cu(113) _diffrn_measurement_device_type MAR225 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16082 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 33.71 _reflns_number_total 4219 _reflns_number_gt 3676 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The geomertical centre of the C60(CF3)12 molecule lies on an inversion centre. Several CF3 groups on the pole of the C60(CF3)12 molecule are strongly disordered between at least four positions due to the presence of three isomers with very similar molecular structure. This resulted in some short calculated contacts between F atoms and considerably increased the number of the parameters in the refinement.The use SUMP instruction for these F atoms led to a small deviation of the sum for F (35.982) instead of 36.000 in the formula. Some C(cage)-CF3 distances associated with the disordered CF3 groups seem to be too long (1.79-1.94 A). This artifact is caused by the fact that minor components of C atoms on cage could not be localized. Therefore, these C-C distances should not be considered as realistic ones because two C atoms involved are from different components of the disordered molecule. ; _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^)+(0.0900P)^2^+10.0806P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4219 _refine_ls_number_parameters 546 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.2133 _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_restrained_S_all 1.238 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 F1 F -0.07282(19) 0.4877(3) -0.33395(16) 0.0768(11) Uani 1 1 d . . . F2 F 0.04754(19) 0.5138(2) -0.33230(15) 0.0652(9) Uani 1 1 d . . . F3 F 0.1085(3) 0.8366(2) -0.0562(2) 0.0950(14) Uani 1 1 d . . . F4 F 0.3375(2) 0.5616(3) 0.0699(2) 0.1003(15) Uani 1 1 d . . . F5 F 0.2022(2) 0.7946(3) 0.0077(3) 0.0934(13) Uani 1 1 d . . . F6 F -0.0442(3) 0.7411(2) 0.25033(18) 0.0968(14) Uani 1 1 d . . . F7 F 0.0100(3) 0.3922(2) -0.32717(17) 0.0917(14) Uani 1 1 d . . . F8 F -0.2344(3) 0.6481(3) -0.1954(3) 0.1160(17) Uani 1 1 d . . . F9 F -0.2910(2) 0.5371(3) -0.1909(2) 0.1074(17) Uani 1 1 d . . . F11 F -0.1253(3) 0.7792(3) 0.1689(2) 0.1148(17) Uani 1 1 d . . . F12 F -0.2026(2) 0.5595(3) -0.27424(17) 0.1004(15) Uani 1 1 d . . . F13 F 0.3317(2) 0.5814(4) -0.0465(2) 0.1074(16) Uani 1 1 d . . . F14 F 0.3068(2) 0.6780(3) 0.0283(3) 0.1137(17) Uani 1 1 d . . . F15 F -0.0098(4) 0.8192(3) 0.1600(2) 0.132(2) Uani 1 1 d . . . F16 F 0.1032(3) 0.8408(3) 0.0636(3) 0.1168(18) Uani 1 1 d . . . C1 C -0.0120(3) 0.6889(3) -0.0860(2) 0.0447(11) Uani 1 1 d . . . C2 C 0.1721(3) 0.6022(3) -0.0570(2) 0.0468(11) Uani 1 1 d . . . C3 C -0.0519(3) 0.7002(3) 0.0443(2) 0.0461(11) Uani 1 1 d . . . C4 C 0.2044(3) 0.4825(3) 0.0106(2) 0.0459(11) Uani 1 1 d . . . C5 C 0.1193(3) 0.6631(3) -0.0623(2) 0.0447(11) Uani 1 1 d . . . C6 C -0.1400(3) 0.6398(3) -0.0500(2) 0.0426(11) Uani 1 1 d . . . C7 C 0.0577(3) 0.6581(3) -0.1183(2) 0.0443(11) Uani 1 1 d . . . C8 C -0.0195(3) 0.5606(3) -0.1919(2) 0.0440(11) Uani 1 1 d . . . C9 C 0.0027(3) 0.7137(3) -0.0089(2) 0.0446(11) Uani 1 1 d . . . C10 C 0.0730(3) 0.4551(3) -0.1833(2) 0.0462(11) Uani 1 1 d . . . C11 C 0.0916(3) 0.3862(3) -0.1443(2) 0.0473(12) Uani 1 1 d . . . C12 C 0.1616(3) 0.6032(3) 0.0829(3) 0.0526(12) Uani 1 1 d . . . C13 C -0.0823(3) 0.6539(3) -0.1063(2) 0.0435(11) Uani 1 1 d . . . C14 C -0.0860(3) 0.5890(3) -0.1613(2) 0.0445(11) Uani 1 1 d . . . C15 C 0.0471(3) 0.6504(3) 0.1349(3) 0.0528(12) Uani 1 1 d . . . C16 C -0.0351(3) 0.6828(3) 0.1285(2) 0.0485(12) Uani 1 1 d . . . C17 C 0.1092(3) 0.5298(3) -0.1632(2) 0.0476(12) Uani 1 1 d . . . C18 C -0.1605(3) 0.5397(3) -0.1484(2) 0.0458(11) Uani 1 1 d . . . C19 C 0.0903(3) 0.7124(3) 0.0053(2) 0.0472(11) Uani 1 1 d . . . C20 C -0.0075(3) 0.4725(3) -0.2174(2) 0.0456(11) Uani 1 1 d . . . C21 C -0.0062(3) 0.4656(3) -0.3032(2) 0.0493(12) Uani 1 1 d . . . C22 C 0.1054(3) 0.6628(3) 0.0766(2) 0.0472(11) Uani 1 1 d . . . C23 C 0.2972(3) 0.5978(4) 0.0179(3) 0.0620(15) Uani 1 1 d . . . C24 C 0.1859(3) 0.4617(3) -0.0673(2) 0.0478(12) Uani 1 1 d . . . C25 C -0.1485(3) 0.6103(3) 0.0845(2) 0.0488(12) Uani 1 1 d . . . C26 C 0.1810(3) 0.4332(3) 0.0670(2) 0.0442(11) Uani 1 1 d . . . C27 C 0.0546(3) 0.5940(3) -0.1688(2) 0.0452(11) Uani 1 1 d . . . C28 C 0.2119(3) 0.5753(3) 0.0166(2) 0.0460(11) Uani 1 1 d . . . C29 C -0.1239(3) 0.6617(3) 0.0244(2) 0.0459(11) Uani 1 1 d . . . C30 C 0.1668(3) 0.5338(3) -0.1072(2) 0.0456(11) Uani 1 1 d . . . C31 C 0.0668(3) 0.5802(3) 0.1760(2) 0.0497(12) Uani 1 1 d . . . C32 C 0.1262(3) 0.7968(3) 0.0051(3) 0.0566(13) Uani 1 1 d . . . C33 C 0.1414(3) 0.5517(4) 0.1486(3) 0.0611(14) Uani 1 1 d . . . C34 C -0.0528(4) 0.7560(4) 0.1776(3) 0.0668(16) Uani 1 1 d . . . C35 C -0.2228(3) 0.5689(4) -0.2029(3) 0.0602(15) Uani 1 1 d . . . F10 F 0.1814(2) 0.6875(2) 0.21382(18) 0.0742(11) Uani 1 1 d . . . F17 F 0.1949(5) 0.5790(4) 0.2855(3) 0.084(2) Uani 0.50 1 d P . . F18 F 0.2787(3) 0.6076(4) 0.1904(3) 0.0753(16) Uani 0.62 1 d P . . F19 F 0.0757(8) 0.7036(8) 0.2786(6) 0.109(4) Uani 0.38 1 d P . . F20 F 0.2508(12) 0.7275(12) 0.1187(8) 0.113(9) Uani 0.246(11) 1 d P . . F21 F 0.0970(9) 0.7969(9) 0.1871(9) 0.083(6) Uani 0.245(11) 1 d P . . C36 C 0.2252(14) 0.6596(17) 0.1534(13) 0.068(7) Uani 0.246(11) 1 d P . . C37 C 0.2045(7) 0.6027(7) 0.2135(6) 0.043(4) Uani 0.376(16) 1 d P . . C38 C 0.131(3) 0.645(2) 0.244(2) 0.059(14) Uani 0.133(16) 1 d P . . C39 C 0.0945(14) 0.7161(14) 0.2063(12) 0.060(7) Uani 0.245(11) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0639(19) 0.129(3) 0.0377(14) 0.0011(17) -0.0100(13) 0.0094(19) F2 0.073(2) 0.084(2) 0.0381(14) 0.0058(14) 0.0065(13) -0.0094(17) F3 0.130(3) 0.065(2) 0.090(3) 0.0335(19) -0.038(2) -0.029(2) F4 0.065(2) 0.140(4) 0.096(3) 0.062(3) -0.0347(19) -0.032(2) F5 0.069(2) 0.072(3) 0.140(4) 0.015(2) -0.018(2) -0.0263(19) F6 0.177(4) 0.075(3) 0.0386(16) -0.0198(16) 0.002(2) -0.002(2) F7 0.167(4) 0.069(2) 0.0389(16) -0.0110(15) 0.0065(19) 0.022(2) F8 0.103(3) 0.119(4) 0.126(4) 0.047(3) -0.012(3) 0.047(3) F9 0.061(2) 0.197(5) 0.063(2) 0.041(3) -0.0140(16) -0.042(3) F11 0.141(4) 0.113(4) 0.090(3) -0.023(2) 0.004(3) 0.072(3) F12 0.075(2) 0.192(5) 0.0340(16) 0.012(2) -0.0073(14) -0.008(3) F13 0.060(2) 0.185(5) 0.077(2) 0.011(3) 0.0177(18) 0.004(3) F14 0.075(3) 0.075(3) 0.191(5) 0.019(3) -0.008(3) -0.026(2) F15 0.245(7) 0.062(3) 0.089(3) -0.030(2) 0.061(4) -0.043(3) F16 0.175(5) 0.066(3) 0.109(3) -0.035(2) 0.054(3) -0.042(3) C1 0.052(3) 0.046(3) 0.036(2) 0.0073(18) -0.0050(18) 0.001(2) C2 0.043(2) 0.057(3) 0.040(2) 0.008(2) 0.0001(18) -0.006(2) C3 0.059(3) 0.042(3) 0.037(2) -0.0038(18) -0.0045(19) 0.008(2) C4 0.042(2) 0.054(3) 0.041(2) 0.000(2) -0.0023(17) 0.005(2) C5 0.046(2) 0.051(3) 0.037(2) 0.0056(19) -0.0032(17) -0.006(2) C6 0.046(2) 0.046(3) 0.036(2) 0.0010(18) -0.0007(17) 0.010(2) C7 0.047(2) 0.052(3) 0.034(2) 0.0061(19) -0.0024(17) -0.003(2) C8 0.055(3) 0.049(3) 0.0281(19) 0.0005(18) -0.0023(17) 0.004(2) C9 0.053(3) 0.042(3) 0.039(2) 0.0018(18) -0.0038(18) 0.000(2) C10 0.050(3) 0.059(3) 0.030(2) -0.0058(19) 0.0009(17) 0.004(2) C11 0.056(3) 0.057(3) 0.029(2) -0.0062(19) -0.0006(18) 0.011(2) C12 0.059(3) 0.052(3) 0.047(3) 0.005(2) 0.006(2) 0.001(2) C13 0.053(3) 0.044(3) 0.033(2) 0.0043(18) -0.0006(17) 0.007(2) C14 0.052(3) 0.051(3) 0.0306(19) 0.0017(18) -0.0032(17) 0.001(2) C15 0.060(3) 0.059(3) 0.039(2) 0.000(2) -0.002(2) 0.008(2) C16 0.063(3) 0.050(3) 0.032(2) -0.0049(19) -0.0038(19) 0.005(2) C17 0.047(2) 0.067(3) 0.0284(19) 0.0034(19) 0.0026(17) 0.003(2) C18 0.048(2) 0.057(3) 0.032(2) 0.0007(19) -0.0035(17) 0.005(2) C19 0.057(3) 0.045(3) 0.040(2) 0.0006(19) -0.0028(19) -0.003(2) C20 0.054(3) 0.052(3) 0.0308(19) -0.0035(18) -0.0011(18) 0.003(2) C21 0.058(3) 0.056(3) 0.033(2) -0.002(2) -0.0012(19) 0.003(2) C22 0.053(3) 0.051(3) 0.038(2) 0.0010(19) -0.0027(18) -0.007(2) C23 0.061(3) 0.068(4) 0.057(3) 0.016(3) -0.009(2) -0.011(3) C24 0.044(2) 0.065(3) 0.035(2) 0.003(2) 0.0013(17) 0.007(2) C25 0.050(3) 0.059(3) 0.037(2) -0.004(2) -0.0014(18) 0.012(2) C26 0.048(2) 0.051(3) 0.033(2) 0.0013(19) -0.0012(17) 0.004(2) C27 0.050(2) 0.055(3) 0.031(2) 0.0067(19) 0.0012(17) -0.001(2) C28 0.046(2) 0.052(3) 0.040(2) 0.0051(19) -0.0016(17) -0.003(2) C29 0.051(3) 0.050(3) 0.037(2) 0.0007(19) -0.0005(18) 0.011(2) C30 0.046(2) 0.055(3) 0.036(2) 0.0024(19) 0.0035(17) 0.000(2) C31 0.061(3) 0.053(3) 0.035(2) 0.002(2) 0.0019(19) 0.001(2) C32 0.068(3) 0.054(3) 0.048(3) 0.003(2) -0.006(2) -0.011(3) C33 0.077(4) 0.053(3) 0.053(3) 0.013(2) 0.011(2) 0.009(3) C34 0.100(5) 0.060(4) 0.041(3) -0.012(2) 0.004(3) 0.009(3) C35 0.053(3) 0.091(5) 0.036(2) 0.011(2) -0.007(2) -0.008(3) F10 0.085(2) 0.079(3) 0.0578(18) -0.0159(17) -0.0129(16) -0.021(2) F17 0.139(6) 0.079(5) 0.033(3) 0.017(3) -0.031(3) -0.052(4) F18 0.057(3) 0.093(4) 0.076(3) -0.022(3) -0.017(2) -0.001(3) F19 0.140(10) 0.115(9) 0.072(6) -0.041(6) 0.010(6) -0.031(8) F20 0.164(18) 0.121(16) 0.054(8) 0.014(8) -0.020(9) -0.090(13) F21 0.096(12) 0.060(10) 0.092(11) -0.017(7) -0.047(8) 0.001(7) C36 0.058(13) 0.088(19) 0.058(13) -0.004(12) 0.010(10) 0.004(12) C37 0.052(7) 0.044(9) 0.032(6) 0.003(5) -0.007(5) 0.012(5) C38 0.07(3) 0.04(3) 0.07(2) -0.019(18) 0.02(2) -0.014(19) C39 0.084(16) 0.046(15) 0.050(12) -0.006(9) 0.001(10) -0.023(11) _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 F1 C21 1.321(6) . ? F2 C21 1.325(6) . ? F3 C32 1.305(6) . ? F4 C23 1.298(6) . ? F5 C32 1.311(7) . ? F6 C34 1.318(6) . ? F7 C21 1.314(6) . ? F8 C35 1.330(8) . ? F9 C35 1.305(6) . ? F11 C34 1.316(8) . ? F12 C35 1.318(6) . ? F13 C23 1.314(7) . ? F14 C23 1.346(8) . ? F15 C34 1.317(8) . ? F16 C32 1.324(7) . ? C1 C13 1.389(6) . ? C1 C7 1.424(6) . ? C1 C9 1.445(6) . ? C2 C5 1.360(7) . ? C2 C30 1.439(7) . ? C2 C28 1.536(6) . ? C3 C9 1.348(7) . ? C3 C29 1.438(7) . ? C3 C16 1.544(6) . ? C4 C26 1.349(6) . ? C4 C24 1.455(6) . ? C4 C28 1.543(8) . ? C5 C7 1.455(6) . ? C5 C19 1.529(7) . ? C6 C29 1.392(6) . ? C6 C13 1.426(6) . ? C6 C26 1.430(7) 5_565 ? C7 C27 1.385(7) . ? C8 C14 1.352(6) . ? C8 C27 1.450(7) . ? C8 C20 1.537(7) . ? C9 C19 1.531(7) . ? C10 C11 1.369(7) . ? C10 C17 1.427(7) . ? C10 C20 1.540(6) . ? C11 C25 1.442(6) 5_565 ? C11 C16 1.524(7) 5_565 ? C12 C22 1.385(7) . ? C12 C33 1.481(7) . ? C12 C28 1.528(7) . ? C12 C36 1.90(3) . ? C13 C14 1.449(6) . ? C14 C18 1.535(7) . ? C15 C31 1.410(7) . ? C15 C22 1.453(7) . ? C15 C16 1.519(7) . ? C15 C39 1.85(2) . ? C16 C34 1.520(7) . ? C16 C11 1.524(7) 5_565 ? C17 C30 1.404(6) . ? C17 C27 1.420(7) . ? C18 C35 1.521(6) . ? C18 C33 1.545(8) 5_565 ? C18 C26 1.549(6) 5_565 ? C19 C32 1.525(7) . ? C19 C22 1.527(6) . ? C20 C21 1.522(6) . ? C20 C31 1.529(7) 5_565 ? C23 C28 1.516(7) . ? C24 C25 1.386(7) 5_565 ? C24 C30 1.424(7) . ? C25 C24 1.386(7) 5_565 ? C25 C29 1.424(7) . ? C25 C11 1.442(6) 5_565 ? C26 C6 1.430(7) 5_565 ? C26 C18 1.549(6) 5_565 ? C31 C33 1.453(7) . ? C31 C20 1.529(7) 5_565 ? C31 C38 1.96(4) . ? C33 C18 1.545(8) 5_565 ? C33 C37 1.792(13) . ? F10 C38 1.24(4) . ? F10 C36 1.39(2) . ? F10 C37 1.455(12) . ? F10 C39 1.58(3) . ? F17 C37 1.344(12) . ? F17 C38 1.70(5) . ? F18 C37 1.345(13) . ? F18 C36 1.42(3) . ? F19 C39 1.34(2) . ? F19 C38 1.49(4) . ? F20 C36 1.35(3) . ? F21 C39 1.38(3) . ? C36 C37 1.46(3) . ? C37 C38 1.54(4) . ? C38 C39 1.50(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 C1 C7 118.9(4) . . ? C13 C1 C9 120.9(4) . . ? C7 C1 C9 109.4(4) . . ? C5 C2 C30 119.7(4) . . ? C5 C2 C28 124.8(4) . . ? C30 C2 C28 109.0(4) . . ? C9 C3 C29 120.3(4) . . ? C9 C3 C16 125.0(4) . . ? C29 C3 C16 108.3(4) . . ? C26 C4 C24 119.5(5) . . ? C26 C4 C28 125.0(4) . . ? C24 C4 C28 108.5(4) . . ? C2 C5 C7 119.5(4) . . ? C2 C5 C19 124.0(4) . . ? C7 C5 C19 108.9(4) . . ? C29 C6 C13 118.6(4) . . ? C29 C6 C26 121.1(4) . 5_565 ? C13 C6 C26 109.6(4) . 5_565 ? C27 C7 C1 120.0(4) . . ? C27 C7 C5 120.7(4) . . ? C1 C7 C5 108.7(4) . . ? C14 C8 C27 120.2(4) . . ? C14 C8 C20 124.0(4) . . ? C27 C8 C20 108.9(4) . . ? C3 C9 C1 119.3(4) . . ? C3 C9 C19 124.8(4) . . ? C1 C9 C19 108.9(4) . . ? C11 C10 C17 119.3(4) . . ? C11 C10 C20 124.3(4) . . ? C17 C10 C20 109.3(4) . . ? C10 C11 C25 119.7(5) . 5_565 ? C10 C11 C16 124.3(4) . 5_565 ? C25 C11 C16 109.2(4) 5_565 5_565 ? C22 C12 C33 107.8(4) . . ? C22 C12 C28 123.3(4) . . ? C33 C12 C28 124.2(5) . . ? C22 C12 C36 96.2(9) . . ? C33 C12 C36 84.3(8) . . ? C28 C12 C36 108.9(7) . . ? C1 C13 C6 119.7(4) . . ? C1 C13 C14 121.4(4) . . ? C6 C13 C14 108.5(4) . . ? C8 C14 C13 119.1(4) . . ? C8 C14 C18 125.8(4) . . ? C13 C14 C18 109.3(4) . . ? C31 C15 C22 108.3(4) . . ? C31 C15 C16 123.5(5) . . ? C22 C15 C16 122.8(4) . . ? C31 C15 C39 91.4(8) . . ? C22 C15 C39 95.6(8) . . ? C16 C15 C39 104.9(9) . . ? C15 C16 C34 115.1(4) . . ? C15 C16 C11 108.6(4) . 5_565 ? C34 C16 C11 111.2(4) . 5_565 ? C15 C16 C3 108.2(4) . . ? C34 C16 C3 111.5(4) . . ? C11 C16 C3 101.3(4) 5_565 . ? C30 C17 C27 118.8(4) . . ? C30 C17 C10 121.7(4) . . ? C27 C17 C10 109.8(4) . . ? C35 C18 C14 109.2(4) . . ? C35 C18 C33 117.3(4) . 5_565 ? C14 C18 C33 109.9(4) . 5_565 ? C35 C18 C26 109.6(4) . 5_565 ? C14 C18 C26 100.1(4) . 5_565 ? C33 C18 C26 109.4(4) 5_565 5_565 ? C32 C19 C22 115.0(4) . . ? C32 C19 C5 110.6(4) . . ? C22 C19 C5 107.8(4) . . ? C32 C19 C9 112.8(4) . . ? C22 C19 C9 108.1(4) . . ? C5 C19 C9 101.6(4) . . ? C21 C20 C31 116.4(4) . 5_565 ? C21 C20 C8 111.4(4) . . ? C31 C20 C8 108.0(4) 5_565 . ? C21 C20 C10 111.3(4) . . ? C31 C20 C10 108.0(4) 5_565 . ? C8 C20 C10 100.6(4) . . ? F7 C21 F1 107.9(4) . . ? F7 C21 F2 106.2(4) . . ? F1 C21 F2 106.4(4) . . ? F7 C21 C20 113.2(4) . . ? F1 C21 C20 112.2(4) . . ? F2 C21 C20 110.6(4) . . ? C12 C22 C15 109.1(4) . . ? C12 C22 C19 124.5(4) . . ? C15 C22 C19 123.0(4) . . ? F4 C23 F13 106.1(5) . . ? F4 C23 F14 106.9(5) . . ? F13 C23 F14 105.4(5) . . ? F4 C23 C28 114.6(4) . . ? F13 C23 C28 112.0(5) . . ? F14 C23 C28 111.2(5) . . ? C25 C24 C30 120.1(4) 5_565 . ? C25 C24 C4 120.8(4) 5_565 . ? C30 C24 C4 108.9(4) . . ? C24 C25 C29 119.0(4) 5_565 . ? C24 C25 C11 120.7(4) 5_565 5_565 ? C29 C25 C11 108.7(4) . 5_565 ? C4 C26 C6 120.0(4) . 5_565 ? C4 C26 C18 125.6(4) . 5_565 ? C6 C26 C18 109.0(4) 5_565 5_565 ? C7 C27 C17 120.0(4) . . ? C7 C27 C8 120.4(4) . . ? C17 C27 C8 108.7(4) . . ? C23 C28 C12 117.6(4) . . ? C23 C28 C2 112.0(4) . . ? C12 C28 C2 108.1(4) . . ? C23 C28 C4 109.0(4) . . ? C12 C28 C4 107.7(4) . . ? C2 C28 C4 101.0(4) . . ? C6 C29 C25 119.4(5) . . ? C6 C29 C3 121.2(4) . . ? C25 C29 C3 109.8(4) . . ? C17 C30 C24 118.3(4) . . ? C17 C30 C2 121.2(4) . . ? C24 C30 C2 109.5(4) . . ? C15 C31 C33 107.9(4) . . ? C15 C31 C20 123.7(4) . 5_565 ? C33 C31 C20 124.5(5) . 5_565 ? C15 C31 C38 90.5(14) . . ? C33 C31 C38 83.0(12) . . ? C20 C31 C38 113.2(12) 5_565 . ? F3 C32 F5 106.1(5) . . ? F3 C32 F16 107.7(5) . . ? F5 C32 F16 106.7(5) . . ? F3 C32 C19 111.5(4) . . ? F5 C32 C19 112.3(5) . . ? F16 C32 C19 112.3(4) . . ? C31 C33 C12 106.5(4) . . ? C31 C33 C18 120.3(5) . 5_565 ? C12 C33 C18 120.6(4) . 5_565 ? C31 C33 C37 99.8(5) . . ? C12 C33 C37 95.2(5) . . ? C18 C33 C37 109.4(5) 5_565 . ? F11 C34 F15 106.1(6) . . ? F11 C34 F6 106.0(5) . . ? F15 C34 F6 108.4(5) . . ? F11 C34 C16 110.7(5) . . ? F15 C34 C16 112.5(5) . . ? F6 C34 C16 112.7(5) . . ? F9 C35 F12 110.2(4) . . ? F9 C35 F8 104.1(5) . . ? F12 C35 F8 104.5(5) . . ? F9 C35 C18 113.9(4) . . ? F12 C35 C18 112.5(5) . . ? F8 C35 C18 110.8(5) . . ? C38 F10 C36 122(2) . . ? C38 F10 C37 69(2) . . ? C36 F10 C37 61.9(12) . . ? C38 F10 C39 63(2) . . ? C36 F10 C39 123.4(13) . . ? C37 F10 C39 123.2(10) . . ? C37 F17 C38 59.2(14) . . ? C37 F18 C36 63.8(11) . . ? C39 F19 C38 64(2) . . ? F20 C36 F10 105(2) . . ? F20 C36 F18 119.9(19) . . ? F10 C36 F18 101.5(15) . . ? F20 C36 C37 160(2) . . ? F10 C36 C37 61.4(11) . . ? F18 C36 C37 55.6(11) . . ? F20 C36 C12 107.2(16) . . ? F10 C36 C12 110.8(14) . . ? F18 C36 C12 112.3(17) . . ? C37 C36 C12 91.3(14) . . ? F17 C37 F18 115.0(9) . . ? F17 C37 F10 104.1(8) . . ? F18 C37 F10 101.8(9) . . ? F17 C37 C36 155.1(14) . . ? F18 C37 C36 60.6(11) . . ? F10 C37 C36 56.8(11) . . ? F17 C37 C38 72.1(18) . . ? F18 C37 C38 149.3(18) . . ? F10 C37 C38 48.8(15) . . ? C36 C37 C38 100(2) . . ? F17 C37 C33 113.3(9) . . ? F18 C37 C33 114.2(8) . . ? F10 C37 C33 106.7(7) . . ? C36 C37 C33 89.1(11) . . ? C38 C37 C33 86.7(16) . . ? F10 C38 F19 105(3) . . ? F10 C38 C39 69(2) . . ? F19 C38 C39 53.0(18) . . ? F10 C38 C37 62.1(18) . . ? F19 C38 C37 164(3) . . ? C39 C38 C37 123(3) . . ? F10 C38 F17 96(3) . . ? F19 C38 F17 131(3) . . ? C39 C38 F17 165(3) . . ? C37 C38 F17 48.7(14) . . ? F10 C38 C31 116(3) . . ? F19 C38 C31 104(2) . . ? C39 C38 C31 85(2) . . ? C37 C38 C31 90.1(18) . . ? F17 C38 C31 106.4(19) . . ? F19 C39 F21 113.1(18) . . ? F19 C39 C38 63.3(18) . . ? F21 C39 C38 149(2) . . ? F19 C39 F10 95.9(16) . . ? F21 C39 F10 106.3(15) . . ? C38 C39 F10 47.4(17) . . ? F19 C39 C15 117.1(14) . . ? F21 C39 C15 114.4(15) . . ? C38 C39 C15 91.9(18) . . ? F10 C39 C15 107.6(13) . . ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 33.71 _diffrn_measured_fraction_theta_full 0.867 _refine_diff_density_max 0.467 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.075