Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof Stephen J. Loeb' _publ_contact_author_address ; Department of Chemistry & Biochemistry University of Windsor Windsor Ontario N9B 3P4 CANADA ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_contact_author_email loeb@uwindsor.ca _publ_requested_journal 'Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; This structure is part of a study on the use of rotaxanes as chelating ligands ; _publ_section_title ; Iron(II) complexes utilising terpyridine containing [2]rotaxanes as ligands ; loop_ _publ_author_name _publ_author_address 'Loeb, Stephen J.' ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; 'Davidson, Gregory J. E.' ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; data_Dinaphtho-24-crown-8-ether_terpy_capped_[2]rotaxane _database_code_CSD 215956 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H77 Cl F6 N6 O15.50 S2' _chemical_formula_weight 1548.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 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 27.432(4) _cell_length_b 19.886(3) _cell_length_c 14.4704(19) _cell_angle_alpha 90.00 _cell_angle_beta 100.981(3) _cell_angle_gamma 90.00 _cell_volume 7749.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.225076 _exptl_absorpt_correction_T_max 0.256575 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 21369 _diffrn_reflns_av_R_equivalents 0.1781 _diffrn_reflns_av_sigmaI/netI 0.2132 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 18.85 _reflns_number_total 6076 _reflns_number_gt 1874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.1459P)^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_extinction_coef ? _refine_ls_number_reflns 6076 _refine_ls_number_parameters 976 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.2596 _refine_ls_R_factor_gt 0.1096 _refine_ls_wR_factor_ref 0.3278 _refine_ls_wR_factor_gt 0.2508 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.023 _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 O1 O 1.9741(6) 0.7999(8) 1.2311(8) 0.083(4) Uani 1 1 d . . . O2 O 1.9032(8) 0.9042(9) 1.1640(16) 0.164(9) Uani 1 1 d . . . O3 O 1.8557(5) 0.9085(9) 0.9794(11) 0.103(5) Uani 1 1 d . . . O4 O 1.7734(5) 0.8207(9) 0.8705(8) 0.090(4) Uani 1 1 d . . . O5 O 1.7659(5) 0.6956(8) 0.8586(8) 0.080(4) Uani 1 1 d . . . O6 O 1.8462(4) 0.5957(7) 0.9100(9) 0.081(4) Uani 1 1 d . . . O7 O 1.8891(5) 0.5825(7) 1.1104(11) 0.093(4) Uani 1 1 d . . . O8 O 1.9601(6) 0.6734(7) 1.2290(8) 0.096(5) Uani 1 1 d . . . N1 N 1.5863(8) 0.5390(16) 1.1115(17) 0.149(9) Uani 1 1 d . . . N2 N 1.5555(6) 0.7092(13) 1.1133(11) 0.084(6) Uani 1 1 d . . . N3 N 1.5616(7) 0.8887(19) 1.1253(13) 0.117(7) Uani 1 1 d . . . N4 N 1.8092(5) 0.7465(10) 1.1000(8) 0.053(4) Uani 1 1 d . . . N5 N 1.9248(5) 0.7486(10) 0.9947(8) 0.053(4) Uani 1 1 d . . . N6 N 2.1746(5) 0.7592(10) 0.9557(8) 0.054(4) Uani 1 1 d . . . C1 C 1.5677(15) 0.474(2) 1.118(3) 0.24(2) Uani 1 1 d . . . H1A H 1.5875 0.4360 1.1147 0.292 Uiso 1 1 calc R . . C2 C 1.5199(18) 0.468(2) 1.129(3) 0.187(16) Uani 1 1 d . . . H2A H 1.5058 0.4251 1.1283 0.224 Uiso 1 1 calc R . . C3 C 1.4930(16) 0.521(3) 1.141(3) 0.22(2) Uani 1 1 d . . . H3A H 1.4608 0.5157 1.1518 0.262 Uiso 1 1 calc R . . C4 C 1.5133(12) 0.5847(17) 1.1380(19) 0.165(13) Uani 1 1 d . . . H4A H 1.4945 0.6226 1.1452 0.198 Uiso 1 1 calc R . . C5 C 1.5595(11) 0.5913(18) 1.1248(15) 0.104(9) Uani 1 1 d . . . C6 C 1.5848(11) 0.6577(15) 1.1203(14) 0.086(7) Uani 1 1 d U . . C7 C 1.6334(8) 0.6620(11) 1.1153(11) 0.076(6) Uani 1 1 d . . . H7A H 1.6520 0.6229 1.1156 0.092 Uiso 1 1 calc R . . C8 C 1.6558(7) 0.7231(11) 1.1098(10) 0.048(5) Uani 1 1 d . . . C9 C 1.6255(8) 0.7800(10) 1.1120(10) 0.062(5) Uani 1 1 d . . . H9A H 1.6387 0.8231 1.1122 0.074 Uiso 1 1 calc R . . C10 C 1.5751(8) 0.7702(14) 1.1138(13) 0.073(6) Uani 1 1 d . . . C11 C 1.5395(14) 0.8272(17) 1.1099(15) 0.094(8) Uani 1 1 d . . . C12 C 1.4903(13) 0.8189(15) 1.0948(16) 0.114(9) Uani 1 1 d . . . H12A H 1.4768 0.7759 1.0907 0.137 Uiso 1 1 calc R . . C13 C 1.4609(11) 0.872(2) 1.0857(18) 0.133(11) Uani 1 1 d . . . H13A H 1.4268 0.8669 1.0678 0.159 Uiso 1 1 calc R . . C14 C 1.4814(15) 0.936(2) 1.1032(18) 0.150(12) Uani 1 1 d . . . H14A H 1.4615 0.9744 1.1020 0.180 Uiso 1 1 calc R . . C15 C 1.5330(15) 0.9408(17) 1.122(2) 0.158(12) Uani 1 1 d . . . H15A H 1.5476 0.9830 1.1335 0.189 Uiso 1 1 calc R . . C16 C 1.7093(7) 0.7311(11) 1.1100(11) 0.051(5) Uani 1 1 d . . . C17 C 1.7418(9) 0.6764(9) 1.1159(13) 0.077(6) Uani 1 1 d . . . H17A H 1.7298 0.6333 1.1231 0.092 Uiso 1 1 calc R . . C18 C 1.7892(9) 0.6846(11) 1.1115(12) 0.074(6) Uani 1 1 d . . . H18A H 1.8097 0.6470 1.1164 0.089 Uiso 1 1 calc R . . C19 C 1.7788(9) 0.8016(9) 1.0970(10) 0.062(6) Uani 1 1 d . . . H19A H 1.7917 0.8444 1.0920 0.074 Uiso 1 1 calc R . . C20 C 1.7302(7) 0.7941(11) 1.1014(12) 0.063(6) Uani 1 1 d . . . H20A H 1.7102 0.8322 1.0986 0.076 Uiso 1 1 calc R . . C21 C 1.8641(5) 0.7533(8) 1.0984(11) 0.054(5) Uani 1 1 d . . . H21A H 1.8830 0.7195 1.1386 0.065 Uiso 1 1 calc R . . H21B H 1.8760 0.7974 1.1207 0.065 Uiso 1 1 calc R . . C22 C 1.8701(6) 0.7431(9) 0.9945(12) 0.071(5) Uani 1 1 d . . . H22A H 1.8578 0.6993 0.9717 0.085 Uiso 1 1 calc R . . H22B H 1.8519 0.7774 0.9544 0.085 Uiso 1 1 calc R . . C23 C 1.9522(9) 0.6913(10) 0.9948(10) 0.059(5) Uani 1 1 d . . . H23A H 1.9373 0.6495 0.9973 0.070 Uiso 1 1 calc R . . C24 C 2.0002(8) 0.6951(11) 0.9914(12) 0.070(6) Uani 1 1 d . . . H24A H 2.0177 0.6550 0.9920 0.084 Uiso 1 1 calc R . . C25 C 2.0251(6) 0.7523(11) 0.9872(11) 0.045(5) Uani 1 1 d . . . C26 C 1.9970(8) 0.8068(11) 0.9829(11) 0.068(6) Uani 1 1 d . . . H26A H 2.0120 0.8479 0.9749 0.081 Uiso 1 1 calc R . . C27 C 1.9472(9) 0.8080(11) 0.9893(12) 0.070(6) Uani 1 1 d . . . H27A H 1.9301 0.8483 0.9898 0.084 Uiso 1 1 calc R . . C28 C 2.0754(6) 0.7543(9) 0.9767(9) 0.040(4) Uani 1 1 d U . . C29 C 2.1026(6) 0.6974(9) 0.9723(10) 0.050(5) Uani 1 1 d . . . H29A H 2.0883 0.6554 0.9762 0.060 Uiso 1 1 calc R . . C30 C 2.1518(8) 0.7022(11) 0.9621(12) 0.070(6) Uani 1 1 d . . . H30A H 2.1695 0.6626 0.9596 0.084 Uiso 1 1 calc R . . C31 C 2.1500(8) 0.8176(10) 0.9652(13) 0.085(7) Uani 1 1 d . . . H31A H 2.1659 0.8590 0.9664 0.102 Uiso 1 1 calc R . . C32 C 2.1008(7) 0.8135(8) 0.9729(10) 0.053(5) Uani 1 1 d . . . H32A H 2.0836 0.8535 0.9756 0.064 Uiso 1 1 calc R . . C33 C 2.2279(6) 0.7591(9) 0.9418(11) 0.063(5) Uani 1 1 d . . . H33A H 2.2318 0.7237 0.8977 0.076 Uiso 1 1 calc R . . H33B H 2.2346 0.8016 0.9137 0.076 Uiso 1 1 calc R . . C34 C 2.2657(7) 0.7489(13) 1.0306(13) 0.059(5) Uani 1 1 d . . . C35 C 2.2805(7) 0.6894(12) 1.0647(15) 0.083(7) Uani 1 1 d . . . H35A H 2.2655 0.6521 1.0323 0.100 Uiso 1 1 calc R . . C36 C 2.3156(7) 0.6772(10) 1.1426(15) 0.079(6) Uani 1 1 d . . . H36A H 2.3264 0.6335 1.1576 0.094 Uiso 1 1 calc R . . C37 C 2.3359(6) 0.7320(11) 1.2012(14) 0.059(6) Uani 1 1 d . . . C38 C 2.3207(8) 0.7922(14) 1.1655(15) 0.104(8) Uani 1 1 d . . . H38A H 2.3348 0.8303 1.1969 0.125 Uiso 1 1 calc R . . C39 C 2.2843(8) 0.8010(11) 1.0825(18) 0.083(6) Uani 1 1 d . . . H39A H 2.2734 0.8441 1.0642 0.100 Uiso 1 1 calc R . . C40 C 2.3754(8) 0.7226(12) 1.2917(15) 0.083(6) Uani 1 1 d . . . C41 C 2.3445(7) 0.7176(12) 1.3667(16) 0.131(9) Uani 1 1 d . . . H41A H 2.3659 0.7130 1.4272 0.196 Uiso 1 1 calc R . . H41B H 2.3231 0.6792 1.3548 0.196 Uiso 1 1 calc R . . H41C H 2.3248 0.7576 1.3661 0.196 Uiso 1 1 calc R . . C42 C 2.4039(8) 0.6563(13) 1.2901(14) 0.156(11) Uani 1 1 d . . . H42A H 2.4273 0.6513 1.3482 0.234 Uiso 1 1 calc R . . H42B H 2.4212 0.6568 1.2385 0.234 Uiso 1 1 calc R . . H42C H 2.3809 0.6194 1.2828 0.234 Uiso 1 1 calc R . . C43 C 2.4093(9) 0.7835(15) 1.3081(14) 0.189(15) Uani 1 1 d . . . H43A H 2.4322 0.7784 1.3667 0.284 Uiso 1 1 calc R . . H43B H 2.3898 0.8233 1.3102 0.284 Uiso 1 1 calc R . . H43C H 2.4274 0.7872 1.2577 0.284 Uiso 1 1 calc R . . C44 C 2.0088(8) 0.6952(17) 1.2306(11) 0.074(7) Uani 1 1 d . . . C45 C 2.0450(11) 0.6459(10) 1.2266(11) 0.078(7) Uani 1 1 d . . . H45A H 2.0384 0.6001 1.2276 0.094 Uiso 1 1 calc R . . C46 C 2.0929(9) 0.6723(14) 1.2210(11) 0.065(6) Uani 1 1 d . . . C47 C 2.1331(12) 0.6260(11) 1.2149(14) 0.104(8) Uani 1 1 d . . . H47A H 2.1273 0.5800 1.2149 0.125 Uiso 1 1 calc R . . C48 C 2.1784(10) 0.6488(15) 1.2095(14) 0.097(8) Uani 1 1 d . . . H48A H 2.2036 0.6184 1.2049 0.116 Uiso 1 1 calc R . . C49 C 2.1884(8) 0.7178(15) 1.2107(12) 0.077(7) Uani 1 1 d . . . H49A H 2.2201 0.7334 1.2084 0.092 Uiso 1 1 calc R . . C50 C 2.1498(9) 0.7630(11) 1.2153(9) 0.072(6) Uani 1 1 d . . . H50A H 2.1560 0.8089 1.2131 0.086 Uiso 1 1 calc R . . C51 C 2.1020(10) 0.7412(12) 1.2233(11) 0.064(6) Uani 1 1 d . . . C52 C 2.0619(12) 0.7849(10) 1.2245(11) 0.071(6) Uani 1 1 d . . . H52A H 2.0667 0.8310 1.2204 0.085 Uiso 1 1 calc R . . C53 C 2.0172(11) 0.7622(13) 1.2312(11) 0.064(6) Uani 1 1 d . . . C54 C 1.9841(7) 0.8705(13) 1.2416(13) 0.096(7) Uani 1 1 d . . . H54A H 1.9968 0.8874 1.1879 0.115 Uiso 1 1 calc R . . H54B H 2.0087 0.8788 1.2981 0.115 Uiso 1 1 calc R . . C55 C 1.9379(9) 0.9038(11) 1.2481(15) 0.119(9) Uani 1 1 d . . . H55A H 1.9233 0.8816 1.2960 0.143 Uiso 1 1 calc R . . H55B H 1.9450 0.9499 1.2682 0.143 Uiso 1 1 calc R . . C56 C 1.8990(13) 0.9506(17) 1.1209(16) 0.167(15) Uani 1 1 d . . . H56A H 1.9312 0.9567 1.1033 0.200 Uiso 1 1 calc R . . H56B H 1.8963 0.9863 1.1652 0.200 Uiso 1 1 calc R . . C57 C 1.8624(8) 0.9689(9) 1.034(2) 0.108(9) Uani 1 1 d . . . H57A H 1.8312 0.9833 1.0505 0.130 Uiso 1 1 calc R . . H57B H 1.8751 1.0048 1.0004 0.130 Uiso 1 1 calc R . . C58 C 1.8278(10) 0.9135(11) 0.8896(19) 0.117(8) Uani 1 1 d . . . H58A H 1.8434 0.8855 0.8487 0.141 Uiso 1 1 calc R . . H58B H 1.8301 0.9596 0.8689 0.141 Uiso 1 1 calc R . . C59 C 1.7756(8) 0.8957(16) 0.8739(15) 0.119(9) Uani 1 1 d . . . H59A H 1.7581 0.9147 0.8151 0.142 Uiso 1 1 calc R . . H59B H 1.7604 0.9125 0.9247 0.142 Uiso 1 1 calc R . . C60 C 1.7259(10) 0.7984(16) 0.8660(12) 0.078(7) Uani 1 1 d . . . C61 C 1.6842(9) 0.8364(12) 0.8667(12) 0.083(7) Uani 1 1 d . . . H61A H 1.6868 0.8830 0.8704 0.099 Uiso 1 1 calc R . . C62 C 1.6361(9) 0.8047(19) 0.8616(11) 0.084(8) Uani 1 1 d . . . C63 C 1.5932(12) 0.8411(11) 0.8674(11) 0.091(7) Uani 1 1 d . . . H63A H 1.5935 0.8878 0.8720 0.109 Uiso 1 1 calc R . . C64 C 1.5489(11) 0.803(2) 0.8659(18) 0.134(15) Uani 1 1 d . . . H64A H 1.5193 0.8267 0.8631 0.160 Uiso 1 1 calc R . . C65 C 1.5474(16) 0.736(2) 0.868(2) 0.175(19) Uani 1 1 d . . . H65A H 1.5181 0.7137 0.8736 0.209 Uiso 1 1 calc R . . C66 C 1.5887(11) 0.6994(14) 0.8626(13) 0.110(9) Uani 1 1 d . . . H66A H 1.5881 0.6526 0.8604 0.132 Uiso 1 1 calc R . . C67 C 1.6344(9) 0.7375(18) 0.8603(12) 0.075(8) Uani 1 1 d . . . C68 C 1.6771(10) 0.6996(11) 0.8573(11) 0.077(6) Uani 1 1 d . . . H68A H 1.6743 0.6530 0.8531 0.092 Uiso 1 1 calc R . . C69 C 1.7230(8) 0.7285(14) 0.8605(12) 0.063(6) Uani 1 1 d . . . C70 C 1.7605(7) 0.6236(12) 0.8374(12) 0.087(7) Uani 1 1 d . . . H70A H 1.7361 0.6167 0.7801 0.104 Uiso 1 1 calc R . . H70B H 1.7493 0.6002 0.8884 0.104 Uiso 1 1 calc R . . C71 C 1.8104(7) 0.5965(12) 0.8252(12) 0.111(9) Uani 1 1 d . . . H71A H 1.8061 0.5511 0.8006 0.134 Uiso 1 1 calc R . . H71B H 1.8228 0.6239 0.7793 0.134 Uiso 1 1 calc R . . C72 C 1.8384(7) 0.5394(11) 0.9702(18) 0.099(7) Uani 1 1 d . . . H72A H 1.8104 0.5491 1.0003 0.119 Uiso 1 1 calc R . . H72B H 1.8306 0.4992 0.9323 0.119 Uiso 1 1 calc R . . C73 C 1.8816(7) 0.5281(12) 1.0402(16) 0.104(8) Uani 1 1 d . . . H73A H 1.9104 0.5253 1.0104 0.124 Uiso 1 1 calc R . . H73B H 1.8785 0.4856 1.0713 0.124 Uiso 1 1 calc R . . C74 C 1.9307(14) 0.5660(12) 1.185(2) 0.24(2) Uani 1 1 d . . . H74A H 1.9209 0.5274 1.2183 0.294 Uiso 1 1 calc R . . H74B H 1.9576 0.5512 1.1552 0.294 Uiso 1 1 calc R . . C75 C 1.9484(10) 0.6082(15) 1.2460(16) 0.129(9) Uani 1 1 d U . . H75A H 1.9787 0.5883 1.2810 0.155 Uiso 1 1 calc R . . H75B H 1.9254 0.6106 1.2892 0.155 Uiso 1 1 calc R . . S1 S 1.73362(19) 1.0179(3) 1.1106(4) 0.0773(17) Uani 1 1 d DU . . O9 O 1.7505(4) 0.9497(5) 1.1061(8) 0.098(4) Uani 1 1 d DU . . O10 O 1.7632(4) 1.0682(5) 1.0743(8) 0.097(4) Uani 1 1 d DU . . O11 O 1.7183(5) 1.0359(6) 1.1977(9) 0.130(5) Uani 1 1 d DU . . C76 C 1.6754(6) 1.0179(8) 1.0238(12) 0.114(8) Uani 1 1 d DU . . F1 F 1.6852(5) 1.0088(7) 0.9376(9) 0.155(5) Uani 1 1 d DU . . F2 F 1.6517(4) 1.0749(7) 1.0229(9) 0.174(6) Uani 1 1 d DU . . F3 F 1.6464(5) 0.9684(7) 1.0404(10) 0.185(6) Uani 1 1 d DU . . S2 S 1.7867(3) 0.4593(4) 1.1707(5) 0.144(3) Uani 1 1 d DU . . O12 O 1.7858(6) 0.5283(6) 1.1695(9) 0.133(6) Uani 1 1 d DU . . O13 O 1.7874(6) 0.4249(7) 1.0909(11) 0.181(8) Uani 1 1 d DU . . O14 O 1.814(2) 0.4329(11) 1.2531(18) 0.61(5) Uani 1 1 d DU . . C77 C 1.7281(9) 0.4324(11) 1.2010(17) 0.41(3) Uani 1 1 d DU . . F4 F 1.7291(11) 0.3724(13) 1.1993(19) 0.45(2) Uani 1 1 d DU . . F5 F 1.7334(15) 0.4568(14) 1.276(2) 0.57(4) Uani 1 1 d DU . . F6 F 1.6984(11) 0.458(2) 1.140(3) 0.66(4) Uani 1 1 d DU . . Cl1 Cl 2.0000 0.5000 1.0000 0.416(15) Uani 1 2 d S . . Cl2 Cl 2.0000 1.0000 1.0000 0.474(16) Uani 1 2 d S . . O2W O 1.6410(9) 0.5317(15) 0.770(2) 0.343(16) Uani 1 1 d . . . O1W O 1.664(3) 0.528(3) 0.960(5) 0.43(5) Uani 0.50 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 O1 0.097(13) 0.064(11) 0.086(10) -0.023(8) 0.017(8) 0.004(10) O2 0.209(19) 0.093(14) 0.135(19) -0.006(12) -0.109(17) 0.023(14) O3 0.082(11) 0.126(16) 0.093(12) 0.018(11) -0.003(9) 0.025(10) O4 0.060(12) 0.114(14) 0.091(11) 0.031(9) 0.002(8) -0.010(11) O5 0.064(11) 0.095(12) 0.078(10) -0.018(8) 0.006(8) 0.001(10) O6 0.079(10) 0.088(11) 0.071(10) -0.024(8) 0.004(8) -0.005(9) O7 0.093(11) 0.080(11) 0.088(11) -0.004(9) -0.025(8) -0.005(9) O8 0.121(14) 0.082(11) 0.071(10) 0.040(8) -0.017(8) -0.020(10) N1 0.069(16) 0.13(2) 0.24(3) 0.03(2) 0.011(15) -0.027(17) N2 0.067(14) 0.114(17) 0.072(12) 0.006(12) 0.016(9) -0.031(15) N3 0.059(15) 0.16(2) 0.138(17) 0.039(17) 0.024(12) 0.06(2) N4 0.038(11) 0.080(13) 0.040(9) -0.002(9) 0.003(7) -0.019(12) N5 0.054(12) 0.039(11) 0.068(10) 0.000(9) 0.015(8) 0.017(12) N6 0.047(12) 0.074(14) 0.036(9) 0.003(9) -0.001(7) -0.007(12) C1 0.14(3) 0.16(4) 0.45(6) 0.05(4) 0.10(4) -0.06(3) C2 0.18(4) 0.20(4) 0.19(3) -0.03(3) 0.04(3) -0.03(4) C3 0.20(5) 0.27(5) 0.22(4) -0.13(4) 0.11(3) -0.18(4) C4 0.07(2) 0.18(4) 0.25(3) 0.00(3) 0.05(2) -0.04(2) C5 0.07(2) 0.15(3) 0.078(16) 0.017(17) -0.009(14) 0.00(2) C6 0.085(11) 0.090(11) 0.085(10) 0.006(9) 0.018(9) -0.007(10) C7 0.075(17) 0.077(17) 0.081(15) 0.002(12) 0.027(12) -0.024(14) C8 0.024(13) 0.088(17) 0.031(11) 0.019(10) 0.002(8) 0.003(15) C9 0.041(15) 0.089(18) 0.054(13) -0.013(10) 0.007(10) 0.009(14) C10 0.029(17) 0.11(2) 0.083(15) -0.017(14) 0.010(11) 0.024(16) C11 0.09(3) 0.12(3) 0.069(16) 0.029(16) 0.013(16) 0.00(3) C12 0.06(2) 0.15(3) 0.12(2) 0.035(18) 0.003(17) 0.03(2) C13 0.09(3) 0.18(3) 0.11(2) 0.01(2) -0.040(16) 0.02(3) C14 0.11(3) 0.19(4) 0.13(2) -0.02(2) -0.02(2) 0.10(3) C15 0.10(3) 0.15(3) 0.22(3) 0.04(2) 0.04(2) 0.06(2) C16 0.058(17) 0.041(14) 0.050(12) -0.025(10) 0.000(10) -0.009(15) C17 0.072(16) 0.035(15) 0.132(18) 0.017(12) 0.037(14) -0.010(15) C18 0.067(18) 0.07(2) 0.087(16) 0.009(12) 0.026(13) 0.005(14) C19 0.090(19) 0.036(13) 0.055(13) 0.001(10) 0.006(12) 0.033(14) C20 0.021(13) 0.077(19) 0.098(15) -0.022(12) 0.027(10) 0.019(12) C21 0.034(13) 0.074(14) 0.053(13) -0.002(10) 0.001(9) 0.005(10) C22 0.062(16) 0.071(15) 0.084(17) -0.009(11) 0.024(11) 0.008(12) C23 0.085(18) 0.037(16) 0.060(13) -0.010(10) 0.029(12) -0.036(14) C24 0.034(15) 0.060(18) 0.117(17) -0.005(12) 0.013(12) 0.009(13) C25 0.023(12) 0.030(12) 0.086(14) -0.017(11) 0.017(9) 0.005(14) C26 0.042(14) 0.09(2) 0.090(15) 0.014(12) 0.048(11) -0.019(13) C27 0.10(2) 0.033(15) 0.087(15) -0.004(11) 0.034(13) 0.006(13) C28 0.052(9) 0.035(8) 0.032(8) -0.011(7) 0.006(7) -0.003(9) C29 0.034(12) 0.044(13) 0.073(13) -0.003(10) 0.014(10) 0.006(10) C30 0.069(18) 0.068(18) 0.080(16) 0.011(12) 0.029(12) 0.025(14) C31 0.045(15) 0.046(16) 0.17(2) 0.008(14) 0.041(14) -0.009(13) C32 0.045(13) 0.025(12) 0.088(14) 0.002(9) 0.008(10) 0.006(10) C33 0.050(13) 0.082(15) 0.055(14) -0.032(11) 0.003(11) -0.014(11) C34 0.060(14) 0.063(16) 0.047(14) 0.010(15) -0.008(12) -0.023(15) C35 0.085(17) 0.08(2) 0.072(18) -0.002(14) -0.024(14) -0.042(14) C36 0.085(16) 0.068(16) 0.057(14) 0.003(12) -0.050(12) 0.005(13) C37 0.031(12) 0.077(17) 0.062(15) 0.010(15) -0.012(11) 0.031(13) C38 0.075(18) 0.14(3) 0.078(19) -0.007(17) -0.022(15) -0.041(18) C39 0.063(15) 0.066(18) 0.107(19) 0.037(15) -0.015(14) 0.010(13) C40 0.052(15) 0.12(2) 0.079(17) 0.008(15) 0.017(15) 0.003(15) C41 0.055(15) 0.19(3) 0.13(2) 0.008(18) -0.014(15) 0.037(15) C42 0.14(2) 0.18(3) 0.12(2) -0.009(19) -0.040(16) 0.08(2) C43 0.13(2) 0.33(4) 0.078(18) 0.06(2) -0.060(15) -0.10(3) C44 0.051(18) 0.13(3) 0.031(12) 0.026(13) -0.022(10) -0.04(2) C45 0.078(19) 0.074(17) 0.074(15) 0.028(12) -0.005(13) 0.033(19) C46 0.052(18) 0.09(2) 0.047(13) -0.002(12) -0.018(11) 0.007(17) C47 0.13(2) 0.064(17) 0.107(18) 0.016(13) -0.007(18) 0.01(2) C48 0.08(2) 0.10(3) 0.112(18) 0.060(17) 0.008(15) 0.027(17) C49 0.049(16) 0.12(2) 0.059(14) 0.023(14) 0.016(11) 0.002(17) C50 0.063(16) 0.13(2) 0.016(11) -0.015(11) -0.019(11) -0.019(18) C51 0.09(2) 0.038(17) 0.047(13) 0.017(11) -0.019(12) -0.003(18) C52 0.10(2) 0.051(16) 0.055(14) -0.009(11) -0.005(13) -0.01(2) C53 0.09(2) 0.06(2) 0.036(12) -0.023(11) 0.005(12) -0.042(19) C54 0.073(18) 0.11(2) 0.100(18) -0.042(15) 0.011(13) 0.004(16) C55 0.12(2) 0.12(2) 0.10(2) -0.053(15) -0.036(17) 0.038(18) C56 0.25(4) 0.19(4) 0.044(17) 0.07(2) -0.025(19) -0.04(3) C57 0.109(19) 0.013(12) 0.22(3) -0.020(17) 0.064(19) 0.001(13) C58 0.11(2) 0.079(18) 0.17(3) 0.012(17) 0.03(2) -0.023(16) C59 0.064(19) 0.18(3) 0.12(2) 0.07(2) 0.040(14) 0.03(2) C60 0.07(2) 0.11(3) 0.056(14) 0.013(14) 0.006(13) -0.04(2) C61 0.025(14) 0.12(2) 0.093(16) -0.017(13) -0.016(12) -0.002(16) C62 0.07(3) 0.15(3) 0.014(12) -0.029(15) -0.013(11) 0.05(2) C63 0.10(2) 0.108(19) 0.053(14) -0.004(12) -0.003(14) 0.06(2) C64 0.035(19) 0.29(5) 0.083(19) 0.01(3) 0.041(14) 0.02(3) C65 0.13(4) 0.27(5) 0.12(2) 0.04(3) 0.01(2) 0.08(4) C66 0.054(18) 0.17(3) 0.099(18) -0.009(16) -0.007(15) 0.00(2) C67 0.05(2) 0.14(3) 0.032(13) -0.013(15) 0.006(10) 0.05(2) C68 0.073(18) 0.108(19) 0.053(14) 0.014(12) 0.019(12) 0.00(2) C69 0.045(19) 0.08(2) 0.056(13) 0.006(12) -0.004(11) -0.005(17) C70 0.054(15) 0.14(2) 0.055(14) -0.036(13) -0.018(10) 0.034(15) C71 0.058(16) 0.23(3) 0.041(14) -0.052(15) -0.005(12) 0.008(16) C72 0.059(16) 0.066(17) 0.17(2) -0.045(16) 0.009(17) 0.000(13) C73 0.048(15) 0.12(2) 0.13(2) 0.025(18) -0.007(14) 0.033(15) C74 0.41(5) 0.08(2) 0.16(3) 0.10(2) -0.15(3) -0.07(3) C75 0.127(12) 0.127(13) 0.126(12) 0.024(10) 0.009(9) -0.013(10) S1 0.077(4) 0.063(4) 0.093(4) 0.006(3) 0.017(3) 0.009(3) O9 0.101(11) 0.063(7) 0.131(11) 0.022(8) 0.024(8) 0.029(8) O10 0.085(10) 0.083(9) 0.121(11) 0.038(8) 0.019(8) -0.004(8) O11 0.162(14) 0.127(12) 0.121(11) -0.004(9) 0.078(10) 0.018(11) C76 0.055(16) 0.136(17) 0.150(18) 0.02(2) 0.018(17) 0.014(11) F1 0.143(12) 0.181(14) 0.130(12) -0.004(9) 0.000(8) 0.007(9) F2 0.101(10) 0.169(11) 0.215(13) -0.039(11) -0.063(9) 0.069(9) F3 0.102(11) 0.211(13) 0.235(14) 0.021(13) 0.013(10) -0.059(10) S2 0.242(10) 0.078(5) 0.117(6) -0.019(5) 0.050(6) -0.011(6) O12 0.194(16) 0.068(8) 0.157(13) -0.019(9) 0.084(11) -0.011(11) O13 0.206(18) 0.132(14) 0.240(16) -0.114(13) 0.130(15) -0.062(13) O14 1.15(12) 0.15(2) 0.34(3) 0.01(2) -0.36(5) 0.07(4) C77 0.60(8) 0.31(3) 0.33(4) -0.09(3) 0.15(5) -0.42(4) F4 0.62(5) 0.33(3) 0.56(4) -0.23(3) 0.49(4) -0.31(3) F5 0.94(8) 0.40(4) 0.54(5) -0.29(4) 0.59(5) -0.47(5) F6 0.19(3) 0.69(6) 1.04(8) -0.45(6) -0.05(4) 0.15(4) Cl1 0.173(13) 0.60(4) 0.51(3) -0.31(3) 0.145(16) 0.083(18) Cl2 0.38(3) 0.45(3) 0.66(4) 0.16(3) 0.26(3) -0.20(2) O2W 0.25(3) 0.32(3) 0.47(4) -0.17(3) 0.08(3) 0.01(2) O1W 0.69(13) 0.30(7) 0.44(9) -0.08(6) 0.43(10) -0.18(8) _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 O1 C53 1.40(2) . ? O1 C54 1.43(2) . ? O2 C56 1.11(2) . ? O2 C55 1.39(2) . ? O3 C58 1.38(2) . ? O3 C57 1.435(19) . ? O4 C60 1.37(2) . ? O4 C59 1.49(3) . ? O5 C69 1.35(2) . ? O5 C70 1.47(2) . ? O6 C71 1.417(18) . ? O6 C72 1.46(2) . ? O7 C74 1.45(3) . ? O7 C73 1.47(2) . ? O8 C75 1.37(3) . ? O8 C44 1.400(19) . ? N1 C5 1.31(3) . ? N1 C1 1.41(3) . ? N2 C6 1.29(2) . ? N2 C10 1.33(2) . ? N3 C15 1.30(3) . ? N3 C11 1.36(3) . ? N4 C18 1.37(2) . ? N4 C19 1.372(18) . ? N4 C21 1.516(16) . ? N5 C27 1.341(19) . ? N5 C23 1.36(2) . ? N5 C22 1.503(18) . ? N6 C30 1.31(2) . ? N6 C31 1.36(2) . ? N6 C33 1.513(18) . ? C1 C2 1.36(4) . ? C2 C3 1.32(5) . ? C3 C4 1.39(4) . ? C4 C5 1.32(3) . ? C5 C6 1.50(3) . ? C6 C7 1.35(2) . ? C7 C8 1.37(2) . ? C8 C9 1.41(2) . ? C8 C16 1.48(2) . ? C9 C10 1.40(2) . ? C10 C11 1.49(3) . ? C11 C12 1.34(3) . ? C12 C13 1.32(3) . ? C13 C14 1.40(3) . ? C14 C15 1.39(3) . ? C16 C20 1.39(2) . ? C16 C17 1.40(2) . ? C17 C18 1.33(2) . ? C19 C20 1.35(2) . ? C21 C22 1.556(18) . ? C23 C24 1.33(2) . ? C24 C25 1.33(2) . ? C25 C26 1.32(2) . ? C25 C28 1.42(2) . ? C26 C27 1.39(2) . ? C28 C29 1.365(19) . ? C28 C32 1.374(19) . ? C29 C30 1.39(2) . ? C31 C32 1.376(19) . ? C33 C34 1.50(2) . ? C34 C35 1.32(2) . ? C34 C39 1.32(2) . ? C35 C36 1.36(2) . ? C36 C37 1.43(2) . ? C37 C38 1.34(3) . ? C37 C40 1.54(2) . ? C38 C39 1.42(2) . ? C40 C41 1.50(2) . ? C40 C43 1.52(3) . ? C40 C42 1.53(3) . ? C44 C53 1.35(3) . ? C44 C45 1.40(3) . ? C45 C46 1.43(2) . ? C46 C51 1.39(2) . ? C46 C47 1.45(3) . ? C47 C48 1.34(3) . ? C48 C49 1.40(3) . ? C49 C50 1.40(2) . ? C50 C51 1.41(2) . ? C51 C52 1.41(2) . ? C52 C53 1.33(2) . ? C54 C55 1.45(2) . ? C56 C57 1.49(3) . ? C58 C59 1.45(2) . ? C60 C61 1.37(3) . ? C60 C69 1.39(2) . ? C61 C62 1.45(3) . ? C62 C67 1.34(3) . ? C62 C63 1.40(3) . ? C63 C64 1.43(3) . ? C64 C65 1.35(4) . ? C65 C66 1.36(3) . ? C66 C67 1.47(3) . ? C67 C68 1.40(2) . ? C68 C69 1.38(2) . ? C70 C71 1.51(2) . ? C72 C73 1.42(2) . ? C74 C75 1.25(3) . ? S1 O9 1.438(10) . ? S1 O10 1.449(10) . ? S1 O11 1.448(11) . ? S1 C76 1.835(16) . ? C76 F2 1.306(13) . ? C76 F3 1.316(14) . ? C76 F1 1.337(14) . ? S2 O13 1.345(12) . ? S2 O12 1.373(12) . ? S2 O14 1.381(15) . ? S2 C77 1.83(2) . ? C77 F5 1.175(19) . ? C77 F6 1.19(2) . ? C77 F4 1.195(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C53 O1 C54 112.3(17) . . ? C56 O2 C55 118(3) . . ? C58 O3 C57 117(2) . . ? C60 O4 C59 110.9(19) . . ? C69 O5 C70 115.0(17) . . ? C71 O6 C72 111.6(16) . . ? C74 O7 C73 109.5(18) . . ? C75 O8 C44 123(2) . . ? C5 N1 C1 120(3) . . ? C6 N2 C10 119(2) . . ? C15 N3 C11 118(3) . . ? C18 N4 C19 117.7(14) . . ? C18 N4 C21 120.2(18) . . ? C19 N4 C21 122.0(18) . . ? C27 N5 C23 118.4(15) . . ? C27 N5 C22 122.1(17) . . ? C23 N5 C22 119.3(19) . . ? C30 N6 C31 118.6(15) . . ? C30 N6 C33 119.7(18) . . ? C31 N6 C33 121.6(18) . . ? C2 C1 N1 117(4) . . ? C3 C2 C1 122(5) . . ? C2 C3 C4 119(4) . . ? C5 C4 C3 120(3) . . ? N1 C5 C4 121(3) . . ? N1 C5 C6 115(3) . . ? C4 C5 C6 124(3) . . ? N2 C6 C7 123(3) . . ? N2 C6 C5 115(3) . . ? C7 C6 C5 122(3) . . ? C6 C7 C8 121(2) . . ? C7 C8 C9 116.1(16) . . ? C7 C8 C16 123(2) . . ? C9 C8 C16 120(2) . . ? C10 C9 C8 118.5(19) . . ? N2 C10 C9 122(2) . . ? N2 C10 C11 116(2) . . ? C9 C10 C11 122(3) . . ? C12 C11 N3 123(3) . . ? C12 C11 C10 123(3) . . ? N3 C11 C10 114(3) . . ? C13 C12 C11 120(3) . . ? C12 C13 C14 120(3) . . ? C15 C14 C13 117(3) . . ? N3 C15 C14 123(3) . . ? C20 C16 C17 115.9(16) . . ? C20 C16 C8 121(2) . . ? C17 C16 C8 123(2) . . ? C18 C17 C16 121.5(18) . . ? C17 C18 N4 122.4(18) . . ? C20 C19 N4 120.7(17) . . ? C19 C20 C16 121.8(17) . . ? N4 C21 C22 107.0(11) . . ? N5 C22 C21 106.2(13) . . ? C24 C23 N5 120.2(17) . . ? C23 C24 C25 124.7(19) . . ? C26 C25 C24 113.7(16) . . ? C26 C25 C28 122.7(19) . . ? C24 C25 C28 123.1(19) . . ? C25 C26 C27 125.5(18) . . ? N5 C27 C26 117.3(17) . . ? C29 C28 C32 114.9(15) . . ? C29 C28 C25 122.3(18) . . ? C32 C28 C25 122.8(18) . . ? C28 C29 C30 120.0(17) . . ? N6 C30 C29 123.7(18) . . ? N6 C31 C32 118.0(16) . . ? C28 C32 C31 124.5(16) . . ? C34 C33 N6 114.4(13) . . ? C35 C34 C39 115.6(18) . . ? C35 C34 C33 124(2) . . ? C39 C34 C33 121(2) . . ? C34 C35 C36 126.3(19) . . ? C35 C36 C37 119.4(18) . . ? C38 C37 C36 113.3(17) . . ? C38 C37 C40 124(2) . . ? C36 C37 C40 123(2) . . ? C37 C38 C39 124(2) . . ? C34 C39 C38 121.1(19) . . ? C41 C40 C43 111(2) . . ? C41 C40 C42 108.2(19) . . ? C43 C40 C42 113(2) . . ? C41 C40 C37 102.6(17) . . ? C43 C40 C37 110.3(18) . . ? C42 C40 C37 111.6(18) . . ? C53 C44 O8 118(3) . . ? C53 C44 C45 124(2) . . ? O8 C44 C45 118(3) . . ? C44 C45 C46 114(2) . . ? C51 C46 C45 121(2) . . ? C51 C46 C47 119(2) . . ? C45 C46 C47 119(3) . . ? C48 C47 C46 121(2) . . ? C47 C48 C49 121(2) . . ? C48 C49 C50 119(2) . . ? C49 C50 C51 122(2) . . ? C46 C51 C50 118(2) . . ? C46 C51 C52 118(2) . . ? C50 C51 C52 124(2) . . ? C53 C52 C51 122(2) . . ? C52 C53 C44 120(2) . . ? C52 C53 O1 128(2) . . ? C44 C53 O1 113(2) . . ? O1 C54 C55 107.6(19) . . ? O2 C55 C54 113.9(18) . . ? O2 C56 C57 131(3) . . ? O3 C57 C56 104.8(19) . . ? O3 C58 C59 119(2) . . ? C58 C59 O4 106.3(19) . . ? O4 C60 C61 128(3) . . ? O4 C60 C69 112(3) . . ? C61 C60 C69 121(2) . . ? C60 C61 C62 121(2) . . ? C67 C62 C63 119(3) . . ? C67 C62 C61 118(2) . . ? C63 C62 C61 123(3) . . ? C62 C63 C64 117(2) . . ? C65 C64 C63 124(3) . . ? C64 C65 C66 120(4) . . ? C65 C66 C67 117(3) . . ? C62 C67 C68 121(3) . . ? C62 C67 C66 123(2) . . ? C68 C67 C66 116(3) . . ? C69 C68 C67 123(2) . . ? O5 C69 C68 126(2) . . ? O5 C69 C60 116(2) . . ? C68 C69 C60 117(2) . . ? O5 C70 C71 108.3(18) . . ? O6 C71 C70 113.4(14) . . ? C73 C72 O6 110.3(17) . . ? C72 C73 O7 111.2(17) . . ? C75 C74 O7 121(3) . . ? C74 C75 O8 126(2) . . ? O9 S1 O10 115.3(7) . . ? O9 S1 O11 115.0(7) . . ? O10 S1 O11 114.8(7) . . ? O9 S1 C76 102.4(8) . . ? O10 S1 C76 103.1(8) . . ? O11 S1 C76 103.7(9) . . ? F2 C76 F3 109.6(13) . . ? F2 C76 F1 107.3(13) . . ? F3 C76 F1 107.8(14) . . ? F2 C76 S1 111.9(12) . . ? F3 C76 S1 110.6(13) . . ? F1 C76 S1 109.5(12) . . ? O13 S2 O12 120.0(9) . . ? O13 S2 O14 117.1(13) . . ? O12 S2 O14 113.4(11) . . ? O13 S2 C77 102.4(11) . . ? O12 S2 C77 106.2(11) . . ? O14 S2 C77 92(3) . . ? F5 C77 F6 117.1(19) . . ? F5 C77 F4 115.6(17) . . ? F6 C77 F4 115.1(17) . . ? F5 C77 S2 98(2) . . ? F6 C77 S2 102(2) . . ? F4 C77 S2 105.1(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 18.85 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.849 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.074