# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2002 data_C70Ar3Tl _database_code_CSD 180836 _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Sawamura, Masaya' 'Toganoh, Motoki' 'Iikura, Hitoshi' 'Hirai, Atsushi' 'Nakamura, Eiichi' _publ_contact_author 'Prof Eiichi Nakamura' _publ_contact_author_address ; Eiichi Nakamura Department of Chemistry, The University of Tokyo, Bunkyo-ku, Tokyo 113-0033, Japan ; _publ_contact_author_email 'nakamura@chem.s.u-tokyo.ac.jp' _publ_requested_journal ' Journal of Materials Chemistry' _publ_section_title ; Cu(I)-Mediated Regioselective Tri-addition of Grignard Reagent to [70]Fullerene. Synthesis of Indenyl-type Metal Ligand Embedded into Graphitic Structure ; #------------------------------------------------------------------------------ _audit_creation_date '2002-01-23T02:05:58-00:00' _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ? #------------------------------------------------------------------------------ _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' #------------------------------------------------------------------------------ _chemical_compound_source 'synthesis as described' _chemical_name_common 'C70Ar3Tl' _chemical_formula_weight 1774.36 _chemical_formula_analytical ? _chemical_formula_sum 'C103 H20 Cl4 F9 Tl' _chemical_formula_moiety 'C103 H20 Cl4 F9 Tl1' _chemical_formula_structural 'C103 H20 Cl4 F9 TL1' _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 18.419(5) _cell_length_b 17.565(5) _cell_length_c 20.638(5) _cell_angle_alpha 90.000 _cell_angle_beta 109.861(5) _cell_angle_gamma 90.000 _cell_volume 6280(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71069 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _exptl_crystal_description 'prism' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_meas 'not measured' _exptl_absorpt_coefficient_mu 2.833 _exptl_crystal_F_000 3472 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_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. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'MacScienceDIP2030' _diffrn_measurement_method scanning _diffrn_reflns_number 5791 _reflns_number_total 5791 _reflns_number_gt 2323 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_unetI/netI 0.1645 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.32 _diffrn_reflns_theta_max 25.91 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.473 _diffrn_measured_fraction_theta_max 0.473 #------------------------------------------------------------------------------ _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^)+(0.1515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5791 _refine_ls_number_parameters 785 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2232 _refine_ls_R_factor_gt 0.0972 _refine_ls_wR_factor_ref 0.3192 _refine_ls_wR_factor_gt 0.2408 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.317 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.127 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #------------------------------------------------------------------------------ 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 Tl1 Tl 0.85593(7) -0.73101(9) -0.28951(6) 0.0702(5) Uani 1 1 d . . . C1 C 0.9306(12) -0.7747(18) -0.3858(9) 0.043(7) Uani 1 1 d . . . C2 C 0.9368(14) -0.6956(19) -0.3861(12) 0.051(7) Uani 1 1 d . . . C3 C 0.9860(15) -0.6662(18) -0.3211(12) 0.053(8) Uani 1 1 d . . . C4 C 1.0163(13) -0.7341(17) -0.2849(12) 0.043(6) Uani 1 1 d . . . C5 C 0.9827(12) -0.7983(17) -0.3206(11) 0.041(7) Uani 1 1 d . . . C6 C 0.9087(14) -0.8248(18) -0.4465(10) 0.051(8) Uani 1 1 d . . . C7 C 0.9080(14) -0.6473(15) -0.4525(10) 0.040(6) Uani 1 1 d . . . C8 C 1.0290(14) -0.5943(16) -0.3141(11) 0.042(7) Uani 1 1 d . . . C9 C 1.0930(13) -0.7301(18) -0.2326(11) 0.043(6) Uani 1 1 d . . . C10 C 1.0239(12) -0.8703(17) -0.3091(12) 0.042(7) Uani 1 1 d . . . C11 C 0.9159(13) -0.7823(19) -0.5057(11) 0.047(7) Uani 1 1 d . . . C12 C 0.9209(14) -0.702(2) -0.5098(12) 0.051(8) Uani 1 1 d . . . C13 C 0.9746(14) -0.5947(15) -0.4454(12) 0.042(7) Uani 1 1 d . . . C14 C 1.0322(17) -0.5678(16) -0.3853(13) 0.054(7) Uani 1 1 d . . . C15 C 1.1140(14) -0.6083(15) -0.2798(11) 0.040(6) Uani 1 1 d . . . C16 C 1.1449(14) -0.6707(18) -0.2354(13) 0.052(8) Uani 1 1 d . . . C17 C 1.1249(12) -0.808(2) -0.2185(11) 0.054(9) Uani 1 1 d . . . C18 C 1.0892(16) -0.8760(17) -0.2525(11) 0.050(7) Uani 1 1 d . . . C19 C 1.0112(13) -0.914(2) -0.3727(13) 0.060(9) Uani 1 1 d . . . C20 C 0.9660(13) -0.8873(14) -0.4355(10) 0.036(6) Uani 1 1 d . . . C21 C 0.9605(13) -0.8284(16) -0.5357(10) 0.038(6) Uani 1 1 d . . . C22 C 1.0017(15) -0.796(2) -0.5751(11) 0.065(10) Uani 1 1 d . . . C23 C 1.0055(13) -0.711(2) -0.5798(11) 0.063(11) Uani 1 1 d . . . C24 C 0.9637(15) -0.6670(17) -0.5450(12) 0.048(7) Uani 1 1 d . . . C25 C 1.0001(12) -0.6018(15) -0.5061(11) 0.036(6) Uani 1 1 d . . . C26 C 1.0729(15) -0.5778(15) -0.5029(12) 0.047(7) Uani 1 1 d . . . C27 C 1.1280(15) -0.5543(18) -0.4382(13) 0.057(7) Uiso 1 1 d . . . C28 C 1.1079(16) -0.5525(19) -0.3802(12) 0.059(8) Uani 1 1 d . . . C29 C 1.1605(14) -0.5744(16) -0.3148(11) 0.049(7) Uani 1 1 d . . . C30 C 1.2350(13) -0.6038(17) -0.3062(13) 0.051(8) Uani 1 1 d . . . C31 C 1.2668(16) -0.6467(16) -0.2522(12) 0.051(7) Uani 1 1 d . . . C32 C 1.2252(15) -0.6837(16) -0.2163(11) 0.045(7) Uani 1 1 d . . . C33 C 1.2563(15) -0.7566(15) -0.1932(12) 0.046(7) Uani 1 1 d . . . C34 C 1.2112(15) -0.8223(19) -0.1979(12) 0.054(8) Uani 1 1 d . . . C35 C 1.2249(15) -0.8973(19) -0.2150(12) 0.051(7) Uani 1 1 d . . . C36 C 1.1498(15) -0.9275(17) -0.2524(13) 0.049(7) Uani 1 1 d . . . C37 C 1.1466(14) -0.9694(17) -0.3095(12) 0.046(6) Uiso 1 1 d . . . C38 C 1.0764(14) -0.9647(15) -0.3720(13) 0.048(7) Uani 1 1 d . . . C39 C 1.1016(15) -0.9716(16) -0.4310(12) 0.045(7) Uani 1 1 d . . . C40 C 1.0605(15) -0.9239(17) -0.4912(12) 0.050(7) Uani 1 1 d . . . C41 C 0.9900(14) -0.8875(18) -0.4946(13) 0.049(7) Uani 1 1 d . . . C42 C 1.1074(15) -0.8874(19) -0.5281(13) 0.058(7) Uiso 1 1 d . . . C43 C 1.0807(14) -0.8244(17) -0.5653(11) 0.044(6) Uiso 1 1 d . . . C44 C 1.1258(13) -0.7620(17) -0.5673(11) 0.045(6) Uiso 1 1 d . . . C45 C 1.0851(16) -0.690(2) -0.5710(13) 0.063(7) Uiso 1 1 d . . . C46 C 1.1169(13) -0.6255(17) -0.5357(11) 0.047(6) Uiso 1 1 d . . . C47 C 1.1961(14) -0.6263(18) -0.4930(12) 0.053(7) Uiso 1 1 d . . . C48 C 1.2038(13) -0.5903(16) -0.4330(11) 0.046(6) Uiso 1 1 d . . . C49 C 1.2594(15) -0.6066(19) -0.3661(13) 0.060(7) Uiso 1 1 d . . . C50 C 1.3147(16) -0.6630(19) -0.3652(13) 0.060(7) Uiso 1 1 d . . . C51 C 1.3535(13) -0.7073(17) -0.3069(11) 0.047(6) Uiso 1 1 d . . . C52 C 1.3320(14) -0.6994(18) -0.2522(12) 0.051(6) Uiso 1 1 d . . . C53 C 1.3258(15) -0.771(2) -0.2121(13) 0.061(7) Uiso 1 1 d . . . C54 C 1.3402(15) -0.8388(18) -0.2363(12) 0.054(7) Uiso 1 1 d . . . C55 C 1.2875(14) -0.9027(17) -0.2362(11) 0.047(6) Uiso 1 1 d . . . C56 C 1.2799(15) -0.9476(18) -0.2962(13) 0.058(7) Uiso 1 1 d . . . C57 C 1.2086(13) -0.9775(16) -0.3326(11) 0.043(6) Uiso 1 1 d . . . C58 C 1.1839(13) -0.9783(16) -0.4062(11) 0.041(6) Uiso 1 1 d . . . C59 C 1.2214(15) -0.9457(19) -0.4417(12) 0.058(7) Uiso 1 1 d . . . C60 C 1.1879(14) -0.8978(17) -0.4997(11) 0.044(6) Uiso 1 1 d . . . C61 C 1.2333(14) -0.8329(17) -0.5041(11) 0.048(6) Uiso 1 1 d . . . C62 C 1.2082(15) -0.764(2) -0.5262(13) 0.058(7) Uiso 1 1 d . . . C63 C 1.2437(13) -0.6964(16) -0.4889(11) 0.042(6) Uiso 1 1 d . . . C64 C 1.3077(14) -0.7043(17) -0.4276(12) 0.050(6) Uiso 1 1 d . . . C65 C 1.3361(15) -0.7795(19) -0.4060(12) 0.057(7) Uiso 1 1 d . . . C66 C 1.3690(13) -0.7809(16) -0.3312(11) 0.043(6) Uiso 1 1 d . . . C67 C 1.3621(14) -0.8441(17) -0.2944(12) 0.051(7) Uiso 1 1 d . . . C68 C 1.3249(14) -0.9143(17) -0.3342(12) 0.049(6) Uiso 1 1 d . . . C69 C 1.2991(14) -0.9120(17) -0.4044(12) 0.051(7) Uiso 1 1 d . . . C70 C 1.3063(13) -0.8461(16) -0.4423(11) 0.045(6) Uiso 1 1 d . . . C71 C 0.8251(14) -0.8608(18) -0.4621(12) 0.051(8) Uani 1 1 d . . . C72 C 0.8143(15) -0.9037(18) -0.4104(15) 0.059(9) Uani 1 1 d . . . H72 H 0.8538 -0.9095 -0.3683 0.071 Uiso 1 1 calc R . . C73 C 0.7431(16) -0.9384(19) -0.4224(11) 0.061(9) Uani 1 1 d . . . H73 H 0.7352 -0.9685 -0.3883 0.074 Uiso 1 1 calc R . . C74 C 0.6836(12) -0.9287(17) -0.4849(13) 0.049(8) Uani 1 1 d . . . C75 C 0.6975(15) -0.8912(18) -0.5316(13) 0.054(7) Uiso 1 1 d . . . H75 H 0.6598 -0.8912 -0.5751 0.065 Uiso 1 1 calc R . . C76 C 0.7630(13) -0.8510(18) -0.5237(12) 0.061(9) Uani 1 1 d . . . H76 H 0.7665 -0.8182 -0.5578 0.073 Uiso 1 1 calc R . . C77 C 0.8289(13) -0.6098(16) -0.4715(11) 0.040(6) Uani 1 1 d . . . C78 C 0.7716(12) -0.6255(15) -0.5288(10) 0.039(6) Uani 1 1 d . . . H78 H 0.7787 -0.6594 -0.5608 0.046 Uiso 1 1 calc R . . C79 C 0.7004(14) -0.5907(17) -0.5406(11) 0.049(8) Uani 1 1 d . . . H79 H 0.6586 -0.6018 -0.5798 0.059 Uiso 1 1 calc R . . C80 C 0.6938(15) -0.5410(17) -0.4940(13) 0.051(7) Uiso 1 1 d . . . C81 C 0.7508(14) -0.5206(17) -0.4346(12) 0.051(7) Uani 1 1 d . . . H81 H 0.7438 -0.4847 -0.4041 0.062 Uiso 1 1 calc R . . C82 C 0.8205(13) -0.5584(16) -0.4238(12) 0.043(7) Uani 1 1 d . . . H82 H 0.862 -0.5488 -0.3838 0.052 Uiso 1 1 calc R . . C83 C 0.9995(13) -0.5315(17) -0.2756(11) 0.045(6) Uiso 1 1 d . . . C84 C 0.9932(14) -0.4561(17) -0.3017(12) 0.051(7) Uani 1 1 d . . . H84 H 1.0095 -0.4451 -0.3387 0.061 Uiso 1 1 calc R . . C85 C 0.9627(14) -0.3982(17) -0.2723(11) 0.049(7) Uani 1 1 d . . . H85 H 0.9557 -0.3494 -0.2907 0.059 Uiso 1 1 calc R . . C86 C 0.9436(17) -0.415(2) -0.2165(15) 0.070(10) Uani 1 1 d . . . C87 C 0.952(2) -0.488(2) -0.1914(15) 0.084(11) Uani 1 1 d . . . H87 H 0.9398 -0.4991 -0.1524 0.101 Uiso 1 1 calc R . . C88 C 0.979(2) -0.547(2) -0.2223(15) 0.090(12) Uani 1 1 d . . . H88 H 0.9831 -0.5968 -0.2053 0.108 Uiso 1 1 calc R . . C89 C 0.6097(15) -0.970(2) -0.4977(18) 0.058(8) Uani 1 1 d . . . C90 C 0.6225(18) -0.502(2) -0.5034(14) 0.065(8) Uiso 1 1 d . . . C91 C 0.9115(17) -0.348(2) -0.1802(14) 0.070(11) Uani 1 1 d . . . C201 C 0.6614(17) -0.605(2) -0.2355(15) 0.074(9) Uiso 1 1 d . . . C202 C 0.6256(19) -0.622(2) -0.3049(16) 0.087(10) Uiso 1 1 d . . . C203 C 0.540(2) -0.612(3) -0.3398(19) 0.104(12) Uiso 1 1 d . . . H203 H 0.5139 -0.6228 -0.386 0.125 Uiso 1 1 calc R . . C204 C 0.504(2) -0.583(2) -0.292(2) 0.104(12) Uiso 1 1 d . . . H204 H 0.4531 -0.5677 -0.3094 0.125 Uiso 1 1 calc R . . C205 C 0.538(2) -0.579(2) -0.2307(19) 0.096(12) Uiso 1 1 d . . . H205 H 0.5086 -0.5737 -0.2024 0.116 Uiso 1 1 calc R . . C206 C 0.6215(19) -0.581(2) -0.1975(17) 0.083(10) Uiso 1 1 d . . . H206 H 0.6452 -0.5667 -0.1518 0.1 Uiso 1 1 calc R . . C301 C 0.3606 -0.6983 -0.6307 0.096(11) Uiso 1 1 d . . . C302 C 0.4084 -0.6593 -0.6611 0.20(3) Uiso 1 1 d . . . C303 C 0.4821 -0.6796 -0.6358 0.21(3) Uiso 1 1 d . . . H303 H 0.5176 -0.6549 -0.6515 0.251 Uiso 1 1 calc R . . C304 C 0.5085 -0.7378 -0.5854 0.144(18) Uiso 1 1 d . . . H304 H 0.5602 -0.7508 -0.5647 0.173 Uiso 1 1 calc R . . C305 C 0.4502 -0.772 -0.5711 0.47(9) Uiso 1 1 d . . . H305 H 0.4626 -0.8167 -0.5455 0.566 Uiso 1 1 calc R . . C306 C 0.3723 -0.7481 -0.5903 0.149(18) Uiso 1 1 d . . . H306 H 0.3357 -0.7688 -0.5735 0.179 Uiso 1 1 calc R . . F1 F 0.5746(11) -0.9888(14) -0.5605(11) 0.106(8) Uani 1 1 d . . . F2 F 0.6120(11) -1.0288(17) -0.4621(13) 0.136(10) Uani 1 1 d . . . F3 F 0.5617(11) -0.9275(14) -0.4784(13) 0.126(9) Uani 1 1 d . . . F4 F 0.5636(11) -0.5226(19) -0.5597(14) 0.188(17) Uani 1 1 d . . . F5 F 0.6181(12) -0.4284(17) -0.511(2) 0.186(14) Uani 1 1 d . . . F6 F 0.5898(13) -0.501(2) -0.4581(11) 0.177(15) Uani 1 1 d . . . F7 F 0.8934(15) -0.2933(11) -0.2214(11) 0.111(8) Uani 1 1 d . . . F8 F 0.8531(8) -0.3758(11) -0.1637(8) 0.078(5) Uani 1 1 d . . . F9 F 0.9688(11) -0.3286(13) -0.1238(10) 0.101(7) Uani 1 1 d . . . Cl1 Cl 0.7609(5) -0.6143(8) -0.2046(5) 0.113(4) Uani 1 1 d . . . Cl2 Cl 0.6706(5) -0.6601(7) -0.3603(4) 0.098(3) Uani 1 1 d . . . Cl3 Cl 0.2569 -0.6784 -0.6592 0.186(6) Uiso 1 1 d . . . Cl4 Cl 0.3698 -0.5826 -0.7098 0.169(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.0684(8) 0.0722(12) 0.0761(8) 0.0021(7) 0.0323(6) 0.0055(8) C1 0.042(13) 0.05(2) 0.020(10) 0.004(12) -0.009(8) -0.019(14) C2 0.055(17) 0.04(2) 0.056(16) -0.014(14) 0.024(13) -0.011(15) C3 0.052(17) 0.04(2) 0.049(15) -0.010(13) -0.007(12) 0.020(15) C4 0.050(15) 0.020(18) 0.057(14) -0.001(13) 0.014(11) -0.004(14) C5 0.026(12) 0.04(2) 0.052(14) 0.014(12) 0.006(10) 0.013(12) C6 0.058(17) 0.07(3) 0.030(13) 0.001(12) 0.025(11) 0.024(16) C7 0.057(16) 0.023(19) 0.039(13) 0.008(10) 0.017(11) 0.001(13) C8 0.052(16) 0.03(2) 0.048(14) -0.005(11) 0.020(12) 0.001(13) C9 0.033(13) 0.04(2) 0.053(13) -0.004(13) 0.011(10) -0.016(15) C10 0.031(13) 0.04(2) 0.054(14) 0.013(12) 0.015(11) -0.003(12) C11 0.039(14) 0.05(3) 0.046(13) -0.001(13) 0.011(10) 0.015(14) C12 0.039(15) 0.06(3) 0.045(14) 0.000(13) 0.008(11) 0.016(14) C13 0.047(15) 0.022(19) 0.050(14) -0.019(11) 0.007(11) -0.003(12) C14 0.08(2) 0.02(2) 0.069(17) 0.022(13) 0.033(15) 0.020(16) C15 0.049(15) 0.014(18) 0.045(13) 0.003(11) -0.001(11) 0.020(12) C16 0.033(14) 0.04(2) 0.074(17) -0.037(15) 0.013(12) 0.011(14) C17 0.027(14) 0.08(3) 0.036(13) -0.016(14) -0.008(11) -0.019(14) C18 0.075(19) 0.04(2) 0.034(13) 0.012(11) 0.011(12) -0.004(15) C19 0.025(13) 0.10(3) 0.059(17) -0.012(16) 0.019(12) -0.019(15) C20 0.051(15) 0.029(18) 0.035(12) -0.003(10) 0.023(11) 0.005(13) C21 0.041(14) 0.03(2) 0.029(12) -0.005(11) -0.002(10) -0.009(12) C22 0.057(18) 0.10(3) 0.022(12) 0.026(13) -0.001(11) 0.026(17) C23 0.031(14) 0.12(4) 0.032(13) -0.019(15) 0.006(10) -0.004(16) C24 0.051(16) 0.03(2) 0.054(15) -0.005(12) 0.008(12) -0.014(14) C25 0.016(11) 0.04(2) 0.056(14) -0.002(12) 0.012(10) -0.004(11) C26 0.060(17) 0.021(19) 0.062(15) 0.029(12) 0.026(13) 0.021(13) C28 0.056(18) 0.07(3) 0.036(14) 0.004(13) 0.001(12) -0.008(16) C29 0.058(17) 0.04(2) 0.037(13) -0.012(12) 0.001(12) 0.004(14) C30 0.026(13) 0.05(2) 0.070(17) 0.038(14) 0.006(11) 0.019(12) C31 0.076(19) 0.02(2) 0.060(15) 0.000(12) 0.022(14) -0.021(15) C32 0.074(19) 0.010(18) 0.044(13) -0.008(11) 0.009(12) 0.005(14) C33 0.063(17) 0.01(2) 0.070(16) -0.009(11) 0.030(13) -0.019(12) C34 0.052(17) 0.05(3) 0.056(16) 0.021(14) 0.010(13) 0.002(15) C35 0.061(18) 0.04(2) 0.051(15) 0.014(13) 0.022(13) 0.020(15) C36 0.050(16) 0.03(2) 0.070(17) 0.024(13) 0.021(13) 0.025(14) C38 0.052(17) 0.014(19) 0.084(18) -0.021(13) 0.030(14) -0.017(13) C39 0.057(17) 0.03(2) 0.052(14) -0.008(11) 0.017(12) 0.006(13) C40 0.063(18) 0.03(2) 0.049(14) -0.001(12) 0.008(12) 0.014(14) C41 0.048(16) 0.04(2) 0.055(16) -0.027(14) 0.014(12) -0.008(15) C71 0.050(16) 0.05(2) 0.057(15) -0.016(13) 0.020(12) 0.025(14) C72 0.036(16) 0.06(3) 0.08(2) 0.014(16) 0.022(13) -0.009(14) C73 0.067(19) 0.08(3) 0.029(13) -0.001(13) 0.010(12) 0.029(18) C74 0.019(12) 0.07(2) 0.071(17) 0.012(14) 0.027(11) -0.010(13) C76 0.041(15) 0.08(3) 0.047(15) 0.009(14) -0.010(12) -0.013(15) C77 0.048(15) 0.03(2) 0.042(13) 0.003(11) 0.019(11) 0.022(13) C78 0.029(12) 0.04(2) 0.031(11) -0.004(10) -0.007(10) -0.008(12) C79 0.039(15) 0.06(2) 0.042(14) 0.016(12) 0.004(11) -0.002(13) C81 0.045(15) 0.05(2) 0.061(16) 0.018(13) 0.018(12) -0.005(14) C82 0.034(14) 0.04(2) 0.058(15) 0.000(12) 0.015(11) 0.007(12) C84 0.049(16) 0.04(2) 0.053(15) -0.009(13) 0.008(12) 0.016(14) C85 0.066(18) 0.05(2) 0.035(12) -0.003(11) 0.017(12) -0.016(15) C86 0.07(2) 0.08(3) 0.07(2) -0.028(18) 0.040(16) -0.028(19) C87 0.12(3) 0.06(3) 0.052(18) 0.011(18) 0.003(18) -0.01(2) C88 0.13(3) 0.09(4) 0.07(2) 0.015(19) 0.054(19) 0.03(2) C89 0.025(15) 0.05(3) 0.10(2) 0.016(18) 0.028(15) -0.004(14) C91 0.044(18) 0.12(4) 0.054(18) -0.005(18) 0.022(14) 0.005(18) F1 0.070(12) 0.14(2) 0.116(15) -0.040(14) 0.043(11) -0.052(13) F2 0.061(13) 0.15(3) 0.19(2) 0.05(2) 0.030(13) -0.031(15) F3 0.069(13) 0.10(2) 0.22(2) -0.069(17) 0.069(14) -0.013(13) F4 0.074(14) 0.21(4) 0.21(2) -0.15(2) -0.038(15) 0.067(17) F5 0.062(14) 0.10(3) 0.41(5) 0.04(3) 0.10(2) 0.013(15) F6 0.092(16) 0.33(5) 0.136(19) 0.08(2) 0.074(14) 0.12(2) F7 0.24(3) 0.013(14) 0.131(17) 0.021(11) 0.128(17) 0.040(14) F8 0.046(9) 0.089(18) 0.102(13) 0.006(10) 0.030(9) 0.006(10) F9 0.078(13) 0.11(2) 0.120(15) -0.043(13) 0.042(11) -0.011(12) Cl1 0.062(5) 0.149(13) 0.112(7) -0.043(7) 0.008(5) 0.016(6) Cl2 0.095(7) 0.104(11) 0.099(6) 0.000(5) 0.039(5) 0.001(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 Tl1 C1 2.88(2) . ? Tl1 C2 2.93(3) . ? Tl1 C3 2.92(3) . ? Tl1 C4 2.92(3) . ? Tl1 C5 2.88(2) . ? C1 C2 1.39(4) . ? C1 C5 1.42(3) . ? C1 C6 1.47(3) . ? C2 C3 1.44(3) . ? C2 C7 1.54(3) . ? C3 C4 1.42(4) . ? C3 C8 1.47(4) . ? C4 C5 1.37(4) . ? C4 C9 1.46(3) . ? C5 C10 1.45(4) . ? C6 C11 1.48(3) . ? C6 C20 1.49(3) . ? C6 C71 1.59(4) . ? C7 C13 1.50(3) . ? C7 C77 1.52(3) . ? C7 C12 1.61(3) . ? C8 C15 1.50(3) . ? C8 C14 1.56(3) . ? C8 C83 1.56(3) . ? C9 C16 1.43(4) . ? C9 C17 1.48(4) . ? C10 C18 1.37(3) . ? C10 C19 1.47(4) . ? C11 C12 1.41(4) . ? C11 C21 1.44(3) . ? C12 C24 1.39(4) . ? C13 C14 1.41(3) . ? C13 C25 1.49(3) . ? C14 C28 1.39(4) . ? C15 C16 1.42(4) . ? C15 C29 1.42(3) . ? C16 C32 1.41(3) . ? C17 C18 1.43(4) . ? C17 C34 1.52(4) . ? C18 C36 1.44(4) . ? C19 C20 1.36(3) . ? C19 C38 1.49(4) . ? C20 C41 1.43(3) . ? C21 C41 1.33(4) . ? C21 C22 1.41(3) . ? C22 C43 1.49(3) . ? C22 C23 1.50(5) . ? C23 C24 1.44(4) . ? C23 C45 1.46(4) . ? C24 C25 1.43(3) . ? C25 C26 1.38(3) . ? C26 C27 1.44(3) . ? C26 C46 1.48(3) . ? C27 C28 1.37(3) . ? C27 C48 1.50(3) . ? C28 C29 1.42(3) . ? C29 C30 1.42(3) . ? C30 C31 1.31(3) . ? C30 C49 1.45(3) . ? C31 C32 1.39(3) . ? C31 C52 1.52(4) . ? C32 C33 1.42(4) . ? C33 C34 1.41(4) . ? C33 C53 1.48(4) . ? C34 C35 1.41(4) . ? C35 C55 1.37(3) . ? C35 C36 1.44(4) . ? C36 C37 1.37(3) . ? C37 C57 1.39(3) . ? C37 C38 1.49(3) . ? C38 C39 1.45(3) . ? C39 C58 1.43(3) . ? C39 C40 1.48(3) . ? C40 C41 1.43(3) . ? C40 C42 1.48(4) . ? C42 C43 1.34(4) . ? C42 C60 1.41(3) . ? C43 C44 1.39(3) . ? C44 C45 1.46(4) . ? C44 C62 1.47(3) . ? C45 C46 1.37(4) . ? C46 C47 1.43(3) . ? C47 C48 1.35(3) . ? C47 C63 1.50(4) . ? C48 C49 1.44(3) . ? C49 C50 1.42(4) . ? C50 C51 1.41(3) . ? C50 C64 1.44(3) . ? C51 C52 1.32(3) . ? C51 C66 1.45(4) . ? C52 C53 1.54(4) . ? C53 C54 1.35(4) . ? C54 C67 1.39(3) . ? C54 C55 1.48(4) . ? C55 C56 1.43(3) . ? C56 C57 1.38(3) . ? C56 C68 1.45(3) . ? C57 C58 1.43(3) . ? C58 C59 1.30(3) . ? C59 C60 1.42(4) . ? C59 C69 1.50(3) . ? C60 C61 1.43(4) . ? C61 C62 1.32(4) . ? C61 C70 1.52(3) . ? C62 C63 1.45(4) . ? C63 C64 1.41(3) . ? C64 C65 1.43(4) . ? C65 C70 1.40(4) . ? C65 C66 1.45(3) . ? C66 C67 1.37(3) . ? C67 C68 1.51(4) . ? C68 C69 1.36(3) . ? C69 C70 1.43(4) . ? C71 C72 1.37(4) . ? C71 C76 1.40(3) . ? C72 C73 1.39(4) . ? C73 C74 1.39(3) . ? C74 C75 1.26(3) . ? C74 C89 1.49(3) . ? C75 C76 1.36(3) . ? C77 C78 1.32(3) . ? C77 C82 1.38(3) . ? C78 C79 1.39(3) . ? C79 C80 1.33(4) . ? C80 C81 1.36(3) . ? C80 C90 1.44(4) . ? C81 C82 1.39(3) . ? C83 C88 1.30(3) . ? C83 C84 1.42(4) . ? C84 C85 1.40(3) . ? C85 C86 1.35(3) . ? C86 C87 1.38(5) . ? C86 C91 1.61(5) . ? C87 C88 1.39(5) . ? C89 F2 1.25(3) . ? C89 F1 1.28(3) . ? C89 F3 1.32(3) . ? C90 F5 1.29(4) . ? C90 F6 1.27(3) . ? C90 F4 1.34(3) . ? C91 F7 1.25(4) . ? C91 F9 1.32(3) . ? C91 F8 1.33(3) . ? C201 C206 1.31(4) . ? C201 C202 1.39(4) . ? C201 Cl1 1.73(3) . ? C202 C203 1.50(4) . ? C202 Cl2 1.76(3) . ? C203 C204 1.45(5) . ? C204 C205 1.21(4) . ? C205 C206 1.45(4) . ? C301 C306 1.1759(2) . ? C301 C302 1.4171(2) . ? C301 Cl3 1.8316(5) . ? C302 C303 1.3272(3) . ? C302 Cl4 1.6875(3) . ? C303 C304 1.4203(3) . ? C304 C305 1.3480(3) . ? C305 C306 1.4162(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 C5 Tl1 C1 28.6(6) . . ? C2 C1 C5 105(2) . . ? C2 C1 C6 126(2) . . ? C5 C1 C6 122(3) . . ? C2 C1 Tl1 78.3(15) . . ? C5 C1 Tl1 75.6(13) . . ? C6 C1 Tl1 133.6(15) . . ? C1 C2 C3 112(2) . . ? C1 C2 C7 123(2) . . ? C3 C2 C7 123(3) . . ? C4 C3 C2 102(3) . . ? C4 C3 C8 125(2) . . ? C2 C3 C8 123(3) . . ? C5 C4 C3 113(2) . . ? C5 C4 C9 126(3) . . ? C3 C4 C9 117(3) . . ? C4 C5 C1 108(2) . . ? C4 C5 C10 121(2) . . ? C1 C5 C10 124(2) . . ? C4 C5 Tl1 78.2(15) . . ? C1 C5 Tl1 75.7(14) . . ? C10 C5 Tl1 137.7(16) . . ? C1 C6 C11 109(3) . . ? C1 C6 C20 110(2) . . ? C11 C6 C20 104.0(18) . . ? C1 C6 C71 112.1(17) . . ? C11 C6 C71 113(2) . . ? C20 C6 C71 109(2) . . ? C13 C7 C77 116(2) . . ? C13 C7 C2 103.1(19) . . ? C77 C7 C2 118.4(18) . . ? C13 C7 C12 97.0(19) . . ? C77 C7 C12 116.1(18) . . ? C2 C7 C12 103(2) . . ? C3 C8 C15 110(2) . . ? C3 C8 C14 111(2) . . ? C15 C8 C14 97.1(19) . . ? C3 C8 C83 113(2) . . ? C15 C8 C83 111(2) . . ? C14 C8 C83 114(2) . . ? C16 C9 C4 120(2) . . ? C16 C9 C17 117(2) . . ? C4 C9 C17 109(2) . . ? C18 C10 C5 118(3) . . ? C18 C10 C19 123(3) . . ? C5 C10 C19 113(2) . . ? C12 C11 C21 118(2) . . ? C12 C11 C6 125(2) . . ? C21 C11 C6 107(2) . . ? C24 C12 C11 123(2) . . ? C24 C12 C7 112(3) . . ? C11 C12 C7 122(2) . . ? C14 C13 C25 114(2) . . ? C14 C13 C7 130(2) . . ? C25 C13 C7 110.3(19) . . ? C28 C14 C13 125(2) . . ? C28 C14 C8 110(2) . . ? C13 C14 C8 118(3) . . ? C16 C15 C29 118(2) . . ? C16 C15 C8 124(2) . . ? C29 C15 C8 114(2) . . ? C32 C16 C15 117(3) . . ? C32 C16 C9 121(3) . . ? C15 C16 C9 118(2) . . ? C18 C17 C9 126(2) . . ? C18 C17 C34 105(3) . . ? C9 C17 C34 121(2) . . ? C10 C18 C36 120(2) . . ? C10 C18 C17 119(3) . . ? C36 C18 C17 107(3) . . ? C20 C19 C10 121(3) . . ? C20 C19 C38 117(2) . . ? C10 C19 C38 115(2) . . ? C19 C20 C41 123(2) . . ? C19 C20 C6 125(2) . . ? C41 C20 C6 106(2) . . ? C41 C21 C22 120(2) . . ? C41 C21 C11 109(2) . . ? C22 C21 C11 121(3) . . ? C21 C22 C43 119(2) . . ? C21 C22 C23 119(3) . . ? C43 C22 C23 106(3) . . ? C24 C23 C45 119(3) . . ? C24 C23 C22 117(2) . . ? C45 C23 C22 108(3) . . ? C12 C24 C25 108(2) . . ? C12 C24 C23 121(3) . . ? C25 C24 C23 119(2) . . ? C26 C25 C24 122(2) . . ? C26 C25 C13 121(2) . . ? C24 C25 C13 109(2) . . ? C25 C26 C27 120(2) . . ? C25 C26 C46 119(3) . . ? C27 C26 C46 105(2) . . ? C28 C27 C26 120(2) . . ? C28 C27 C48 118(2) . . ? C26 C27 C48 107(2) . . ? C27 C28 C14 119(2) . . ? C27 C28 C29 122(3) . . ? C14 C28 C29 111(2) . . ? C30 C29 C15 120(2) . . ? C30 C29 C28 122(2) . . ? C15 C29 C28 105(2) . . ? C31 C30 C29 117(2) . . ? C31 C30 C49 122(3) . . ? C29 C30 C49 118(2) . . ? C30 C31 C32 124(3) . . ? C30 C31 C52 118(2) . . ? C32 C31 C52 107(2) . . ? C31 C32 C16 119(3) . . ? C31 C32 C33 112(2) . . ? C16 C32 C33 120(3) . . ? C34 C33 C32 124(3) . . ? C34 C33 C53 112(3) . . ? C32 C33 C53 111(2) . . ? C33 C34 C35 129(3) . . ? C33 C34 C17 115(3) . . ? C35 C34 C17 110(3) . . ? C55 C35 C34 113(3) . . ? C55 C35 C36 124(2) . . ? C34 C35 C36 105(2) . . ? C37 C36 C18 122(2) . . ? C37 C36 C35 114(2) . . ? C18 C36 C35 112(3) . . ? C36 C37 C57 123(2) . . ? C36 C37 C38 119(2) . . ? C57 C37 C38 106.4(19) . . ? C39 C38 C37 107(2) . . ? C39 C38 C19 122(2) . . ? C37 C38 C19 120(2) . . ? C58 C39 C38 108(2) . . ? C58 C39 C40 122(2) . . ? C38 C39 C40 116(2) . . ? C41 C40 C39 120(2) . . ? C41 C40 C42 118(3) . . ? C39 C40 C42 117(2) . . ? C21 C41 C20 111(2) . . ? C21 C41 C40 123(2) . . ? C20 C41 C40 120(2) . . ? C43 C42 C60 118(3) . . ? C43 C42 C40 119(2) . . ? C60 C42 C40 117(2) . . ? C42 C43 C44 124(2) . . ? C42 C43 C22 121(2) . . ? C44 C43 C22 107(3) . . ? C43 C44 C45 113(2) . . ? C43 C44 C62 119(3) . . ? C45 C44 C62 118(3) . . ? C46 C45 C44 125(3) . . ? C46 C45 C23 120(3) . . ? C44 C45 C23 105(3) . . ? C45 C46 C47 119(3) . . ? C45 C46 C26 121(2) . . ? C47 C46 C26 109(2) . . ? C48 C47 C46 109(2) . . ? C48 C47 C63 117(2) . . ? C46 C47 C63 120(3) . . ? C47 C48 C49 127(3) . . ? C47 C48 C27 109(2) . . ? C49 C48 C27 119(2) . . ? C50 C49 C48 115(2) . . ? C50 C49 C30 116(2) . . ? C48 C49 C30 119(2) . . ? C51 C50 C49 124(2) . . ? C51 C50 C64 110(3) . . ? C49 C50 C64 120(2) . . ? C52 C51 C50 117(3) . . ? C52 C51 C66 123(3) . . ? C50 C51 C66 107(2) . . ? C51 C52 C31 122(2) . . ? C51 C52 C53 118(3) . . ? C31 C52 C53 107(2) . . ? C54 C53 C33 123(3) . . ? C54 C53 C52 118(2) . . ? C33 C53 C52 103(2) . . ? C53 C54 C67 122(3) . . ? C53 C54 C55 117(2) . . ? C67 C54 C55 109(2) . . ? C35 C55 C56 118(2) . . ? C35 C55 C54 125(3) . . ? C56 C55 C54 107(2) . . ? C57 C56 C55 118(2) . . ? C57 C56 C68 118(2) . . ? C55 C56 C68 110(3) . . ? C56 C57 C37 121(2) . . ? C56 C57 C58 119(2) . . ? C37 C57 C58 111.3(19) . . ? C59 C58 C57 124(2) . . ? C59 C58 C39 118(2) . . ? C57 C58 C39 107.2(19) . . ? C58 C59 C60 125(2) . . ? C58 C59 C69 119(2) . . ? C60 C59 C69 105(3) . . ? C42 C60 C59 121(2) . . ? C42 C60 C61 115(3) . . ? C59 C60 C61 115(2) . . ? C62 C61 C60 127(2) . . ? C62 C61 C70 122(3) . . ? C60 C61 C70 101(2) . . ? C61 C62 C63 122(2) . . ? C61 C62 C44 113(3) . . ? C63 C62 C44 119(3) . . ? C64 C63 C62 119(3) . . ? C64 C63 C47 115(2) . . ? C62 C63 C47 120(2) . . ? C63 C64 C65 118(3) . . ? C63 C64 C50 123(2) . . ? C65 C64 C50 106(2) . . ? C70 C65 C64 125(2) . . ? C70 C65 C66 120(3) . . ? C64 C65 C66 109(2) . . ? C67 C66 C51 118(2) . . ? C67 C66 C65 121(2) . . ? C51 C66 C65 107(2) . . ? C66 C67 C54 122(3) . . ? C66 C67 C68 118(2) . . ? C54 C67 C68 108(2) . . ? C69 C68 C56 122(2) . . ? C69 C68 C67 119(2) . . ? C56 C68 C67 106(2) . . ? C68 C69 C70 123(2) . . ? C68 C69 C59 118(2) . . ? C70 C69 C59 107(2) . . ? C65 C70 C69 118(2) . . ? C65 C70 C61 113(2) . . ? C69 C70 C61 111(2) . . ? C72 C71 C76 119(3) . . ? C72 C71 C6 117(2) . . ? C76 C71 C6 125(2) . . ? C71 C72 C73 119(3) . . ? C74 C73 C72 121(3) . . ? C75 C74 C73 118(3) . . ? C75 C74 C89 122(3) . . ? C73 C74 C89 119(3) . . ? C74 C75 C76 125(3) . . ? C75 C76 C71 118(3) . . ? C78 C77 C82 122(2) . . ? C78 C77 C7 123(2) . . ? C82 C77 C7 115(2) . . ? C77 C78 C79 119(2) . . ? C80 C79 C78 118(2) . . ? C79 C80 C81 126(3) . . ? C79 C80 C90 121(3) . . ? C81 C80 C90 112(3) . . ? C80 C81 C82 114(3) . . ? C77 C82 C81 121(2) . . ? C88 C83 C84 121(3) . . ? C88 C83 C8 122(3) . . ? C84 C83 C8 118(2) . . ? C85 C84 C83 120(3) . . ? C86 C85 C84 118(3) . . ? C85 C86 C87 120(3) . . ? C85 C86 C91 119(3) . . ? C87 C86 C91 122(3) . . ? C86 C87 C88 123(3) . . ? C83 C88 C87 118(4) . . ? F2 C89 F1 107(3) . . ? F2 C89 F3 101(3) . . ? F1 C89 F3 107(2) . . ? F2 C89 C74 117(3) . . ? F1 C89 C74 115(2) . . ? F3 C89 C74 109(3) . . ? F5 C90 F6 93(3) . . ? F5 C90 F4 100(3) . . ? F6 C90 F4 101(3) . . ? F5 C90 C80 121(3) . . ? F6 C90 C80 123(3) . . ? F4 C90 C80 115(3) . . ? F7 C91 F9 110(4) . . ? F7 C91 F8 114(3) . . ? F9 C91 F8 110(2) . . ? F7 C91 C86 108(2) . . ? F9 C91 C86 107(2) . . ? F8 C91 C86 108(3) . . ? C206 C201 C202 121(3) . . ? C206 C201 Cl1 123(3) . . ? C202 C201 Cl1 115(2) . . ? C201 C202 C203 121(3) . . ? C201 C202 Cl2 126(3) . . ? C203 C202 Cl2 112(2) . . ? C204 C203 C202 111(3) . . ? C205 C204 C203 123(4) . . ? C204 C205 C206 126(4) . . ? C201 C206 C205 116(3) . . ? C306 C301 C302 132.913(11) . . ? C306 C301 Cl3 106.792(6) . . ? C302 C301 Cl3 120.121(15) . . ? C303 C302 C301 113.693(17) . . ? C303 C302 Cl4 128.007(4) . . ? C301 C302 Cl4 116.797(15) . . ? C302 C303 C304 122.090(6) . . ? C305 C304 C303 112.370(14) . . ? C304 C305 C306 127.818(16) . . ? C301 C306 C305 110.057(7) . . ? #==END