# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2014 data_1H6_ReO4 _publ_contact_author ; Dr. Valeria Amendola Dipartimento di Chimica University of Pavia via Taramelli 12, I-27100 Pavia, ITALY ; _publ_contact_author_email ; valeria.amendola@unipv.it ; loop_ _publ_author_name _publ_author_address 'Amendola V.' 'Dipartimento di Chimica,University of Pavia, Italy' 'Bergamaschi G.' 'Dipartimento di Chimica, University of Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, Univerity of Pavia, Italy' 'Alberto R.' 'Institute of Inorganic Chemistry, University of Zurich' 'Braband H.' 'Institute of Inorganic Chemistry, University of Zurich' _publ_requested_journal 'Nature Chem.' _journal_name_full ; Nature Chemistry ; _publ_section_title ; A fluorescent sensor for 99Tc pertechnetate in water ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; (4,8,14,18,23,27-hexa-azonia-1,11-diaza-6(9,10)-anthracena-16,25(1,4)-dibenzena bicyclo[9.9.9]nonacosaphane perrhenate clathrate) penta(triflate) heptahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C44 H64 N8, 5(C F3 O3 S), O4 Re, 7 (H2 O)' _chemical_formula_sum 'C49 H78 F15 N8 O26 Re S5' _chemical_formula_weight 1826.64 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' F F 0.0171 0.0103 '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' Re Re -1.0185 7.2310 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _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 12.949(2) _cell_length_b 17.658(3) _cell_length_c 32.897(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.081(5) _cell_angle_gamma 90.00 _cell_volume 7522(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5975 _cell_measurement_theta_min 2 _cell_measurement_theta_max 19 _exptl_crystal_description PRISM _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 1.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Axs Smart-Apex CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_decay_% 0 _diffrn_reflns_number 50398 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13198 _reflns_number_gt 8964 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker-Axs Inc)' _computing_cell_refinement 'SAINT (Bruker-Axs Inc)' _computing_data_reduction 'SAINT (Bruker-Axs Inc)' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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. Selected single crystals show a poor X-ray diffraction quality: in general, diffracted intensities at theta value greater than 20 degree are very weak. The geometrical details of the cage and of the enclosed perrhenate anion have an accuracy suitable to the aims of this work. However, the poor X-ray diffraction quality of the data imposes the use of soft restraints (ISOR and DELU instructions) on the least-square procedures involving the Uij values of several atoms belonging to triflate counterions. Also the molecular geometries of one triflate counterion have been restrained using the SAME instruction to be the same of the best characterized triflate in the crystal structure. Positions of H atoms belonging to water solvent molecules remain undetermined. ; _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^)+(0.1016P)^2^+3.4410P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13198 _refine_ls_number_parameters 937 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1786 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.003 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 Re1 Re 0.72662(2) 0.146197(17) 0.124538(9) 0.05854(13) Uani 1 1 d . . . O1 O 0.6710(5) 0.2320(3) 0.11354(16) 0.0794(15) Uani 1 1 d . . . O2 O 0.8526(5) 0.1608(3) 0.13843(19) 0.0851(17) Uani 1 1 d . . . O3 O 0.7215(5) 0.0902(3) 0.08185(15) 0.0774(15) Uani 1 1 d . . . O4 O 0.6636(4) 0.1002(3) 0.16323(14) 0.0737(14) Uani 1 1 d . . . C1 C 0.6420(8) 0.4043(6) 0.0243(3) 0.096(3) Uani 1 1 d . . . H1A H 0.6506 0.4416 0.0029 0.116 Uiso 1 1 calc R . . H1B H 0.6113 0.4297 0.0475 0.116 Uiso 1 1 calc R . . C2 C 0.5671(8) 0.3428(5) 0.0093(3) 0.093(3) Uani 1 1 d . . . H2A H 0.5016 0.3661 0.0024 0.112 Uiso 1 1 calc R . . H2B H 0.5948 0.3201 -0.0152 0.112 Uiso 1 1 calc R . . C3 C 0.4602(7) 0.2320(6) 0.0296(3) 0.089(3) Uani 1 1 d . . . H3A H 0.4663 0.2156 0.0016 0.107 Uiso 1 1 calc R . . H3B H 0.3965 0.2605 0.0321 0.107 Uiso 1 1 calc R . . C4 C 0.4547(6) 0.1635(5) 0.0567(3) 0.074(2) Uani 1 1 d . . . C5 C 0.4634(8) 0.0916(7) 0.0407(3) 0.096(3) Uani 1 1 d . . . H5 H 0.4731 0.0853 0.0129 0.115 Uiso 1 1 calc R . . C6 C 0.4578(8) 0.0285(6) 0.0659(3) 0.100(3) Uani 1 1 d . . . H6 H 0.4639 -0.0196 0.0546 0.119 Uiso 1 1 calc R . . C7 C 0.4438(6) 0.0355(5) 0.1060(3) 0.075(2) Uani 1 1 d . . . C8 C 0.4330(7) 0.1077(6) 0.1229(3) 0.082(2) Uani 1 1 d . . . H8 H 0.4222 0.1136 0.1507 0.098 Uiso 1 1 calc R . . C9 C 0.4383(7) 0.1691(6) 0.0983(3) 0.083(3) Uani 1 1 d . . . H9 H 0.4307 0.2170 0.1097 0.100 Uiso 1 1 calc R . . C10 C 0.4385(7) -0.0346(5) 0.1329(3) 0.085(3) Uani 1 1 d . . . H10A H 0.3735 -0.0343 0.1475 0.102 Uiso 1 1 calc R . . H10B H 0.4395 -0.0793 0.1158 0.102 Uiso 1 1 calc R . . C11 C 0.5299(7) -0.1148(5) 0.1838(3) 0.087(3) Uani 1 1 d . . . H11A H 0.5547 -0.1527 0.1649 0.104 Uiso 1 1 calc R . . H11B H 0.4611 -0.1295 0.1924 0.104 Uiso 1 1 calc R . . C12 C 0.6003(7) -0.1130(6) 0.2205(3) 0.090(3) Uani 1 1 d . . . H12A H 0.5703 -0.0796 0.2407 0.108 Uiso 1 1 calc R . . H12B H 0.6030 -0.1634 0.2322 0.108 Uiso 1 1 calc R . . C13 C 0.7952(9) 0.4378(5) 0.0590(3) 0.100(3) Uani 1 1 d . . . H13A H 0.7918 0.4841 0.0431 0.120 Uiso 1 1 calc R . . H13B H 0.8675 0.4247 0.0622 0.120 Uiso 1 1 calc R . . C14 C 0.7499(8) 0.4531(5) 0.1006(3) 0.088(3) Uani 1 1 d . . . H14A H 0.7902 0.4922 0.1139 0.106 Uiso 1 1 calc R . . H14B H 0.6800 0.4720 0.0973 0.106 Uiso 1 1 calc R . . C15 C 0.7222(9) 0.4035(5) 0.1708(3) 0.097(3) Uani 1 1 d . . . H15A H 0.7735 0.4386 0.1812 0.116 Uiso 1 1 calc R . . H15B H 0.6555 0.4284 0.1718 0.116 Uiso 1 1 calc R . . C16 C 0.7198(9) 0.3349(5) 0.1971(3) 0.085(3) Uani 1 1 d . . . C17 C 0.6263(8) 0.2998(5) 0.2046(3) 0.087(3) Uani 1 1 d . . . H17 H 0.5657 0.3189 0.1934 0.105 Uiso 1 1 calc R . . C18 C 0.6238(8) 0.2365(5) 0.2288(3) 0.087(3) Uani 1 1 d . . . H18 H 0.5608 0.2127 0.2335 0.104 Uiso 1 1 calc R . . C19 C 0.7121(8) 0.2070(5) 0.2464(2) 0.080(2) Uani 1 1 d . . . C20 C 0.8035(9) 0.2442(6) 0.2377(3) 0.101(3) Uani 1 1 d . . . H20 H 0.8642 0.2256 0.2491 0.121 Uiso 1 1 calc R . . C21 C 0.8096(9) 0.3054(6) 0.2140(3) 0.096(3) Uani 1 1 d . . . H21 H 0.8732 0.3280 0.2088 0.115 Uiso 1 1 calc R . . C22 C 0.7046(9) 0.1369(5) 0.2721(3) 0.090(3) Uani 1 1 d . . . H22A H 0.7543 0.1401 0.2941 0.108 Uiso 1 1 calc R . . H22B H 0.6362 0.1339 0.2839 0.108 Uiso 1 1 calc R . . C23 C 0.7137(8) -0.0015(5) 0.2733(2) 0.087(3) Uani 1 1 d . . . H23A H 0.6414 -0.0092 0.2797 0.104 Uiso 1 1 calc R . . H23B H 0.7508 0.0054 0.2987 0.104 Uiso 1 1 calc R . . C24 C 0.7550(8) -0.0715(6) 0.2519(3) 0.089(3) Uani 1 1 d . . . H24A H 0.8285 -0.0651 0.2475 0.107 Uiso 1 1 calc R . . H24B H 0.7458 -0.1148 0.2696 0.107 Uiso 1 1 calc R . . C25 C 0.8017(9) 0.3594(6) -0.0015(3) 0.104(3) Uani 1 1 d . . . H25A H 0.8111 0.4065 -0.0163 0.125 Uiso 1 1 calc R . . H25B H 0.7599 0.3264 -0.0184 0.125 Uiso 1 1 calc R . . C26 C 0.9074(7) 0.3226(5) 0.0040(3) 0.086(3) Uani 1 1 d . . . H26A H 0.9378 0.3136 -0.0225 0.104 Uiso 1 1 calc R . . H26B H 0.9523 0.3569 0.0187 0.104 Uiso 1 1 calc R . . C27 C 0.9894(6) 0.1967(5) 0.0157(3) 0.080(2) Uani 1 1 d . . . H27A H 0.9836 0.1815 -0.0126 0.096 Uiso 1 1 calc R . . H27B H 1.0546 0.2230 0.0191 0.096 Uiso 1 1 calc R . . C28 C 0.9881(6) 0.1265(5) 0.0425(2) 0.065(2) Uani 1 1 d . . . C29 C 0.9276(5) 0.0629(5) 0.0307(2) 0.0606(19) Uani 1 1 d . . . C30 C 0.8694(6) 0.0624(5) -0.0060(2) 0.070(2) Uani 1 1 d . . . H30 H 0.8715 0.1045 -0.0230 0.084 Uiso 1 1 calc R . . C31 C 0.8111(7) 0.0022(6) -0.0169(3) 0.080(2) Uani 1 1 d . . . H31 H 0.7735 0.0035 -0.0410 0.096 Uiso 1 1 calc R . . C32 C 0.8072(6) -0.0616(5) 0.0078(3) 0.075(2) Uani 1 1 d . . . H32 H 0.7674 -0.1029 -0.0001 0.091 Uiso 1 1 calc R . . C33 C 0.8598(6) -0.0643(5) 0.0424(2) 0.073(2) Uani 1 1 d . . . H33 H 0.8555 -0.1078 0.0583 0.087 Uiso 1 1 calc R . . C34 C 0.9232(6) -0.0023(5) 0.0566(2) 0.064(2) Uani 1 1 d . . . C35 C 0.9791(6) -0.0042(5) 0.0937(2) 0.068(2) Uani 1 1 d . . . C36 C 1.0429(6) 0.0564(5) 0.1037(2) 0.070(2) Uani 1 1 d . . . C37 C 1.1055(7) 0.0570(6) 0.1396(3) 0.086(3) Uani 1 1 d . . . H37 H 1.1052 0.0150 0.1567 0.103 Uiso 1 1 calc R . . C38 C 1.1645(8) 0.1166(8) 0.1493(3) 0.107(3) Uani 1 1 d . . . H38 H 1.2036 0.1151 0.1730 0.128 Uiso 1 1 calc R . . C39 C 1.1690(8) 0.1811(8) 0.1246(4) 0.108(3) Uani 1 1 d . . . H39 H 1.2103 0.2218 0.1323 0.130 Uiso 1 1 calc R . . C40 C 1.1154(7) 0.1844(6) 0.0909(3) 0.087(3) Uani 1 1 d . . . H40 H 1.1211 0.2273 0.0746 0.104 Uiso 1 1 calc R . . C41 C 1.0475(6) 0.1238(5) 0.0780(2) 0.071(2) Uani 1 1 d . . . C42 C 0.9720(6) -0.0722(5) 0.1208(2) 0.076(2) Uani 1 1 d . . . H42A H 1.0326 -0.0744 0.1381 0.092 Uiso 1 1 calc R . . H42B H 0.9706 -0.1177 0.1043 0.092 Uiso 1 1 calc R . . C43 C 0.8697(8) -0.1314(5) 0.1763(3) 0.086(3) Uani 1 1 d . . . H43A H 0.9130 -0.1190 0.1994 0.103 Uiso 1 1 calc R . . H43B H 0.8983 -0.1764 0.1637 0.103 Uiso 1 1 calc R . . C44 C 0.7619(8) -0.1501(5) 0.1918(3) 0.085(3) Uani 1 1 d . . . H44A H 0.7207 -0.1673 0.1690 0.102 Uiso 1 1 calc R . . H44B H 0.7676 -0.1921 0.2107 0.102 Uiso 1 1 calc R . . N1 N 0.7428(6) 0.3763(4) 0.0360(2) 0.0785(19) Uani 1 1 d . . . N2 N 0.5494(5) 0.2827(4) 0.03980(19) 0.0760(18) Uani 1 1 d . . . H2C H 0.5378 0.3044 0.0641 0.091 Uiso 1 1 calc R . . H2D H 0.6069 0.2544 0.0420 0.091 Uiso 1 1 calc R . . N3 N 0.5239(5) -0.0399(4) 0.1625(2) 0.0732(18) Uani 1 1 d . . . H3C H 0.5163 -0.0031 0.1812 0.088 Uiso 1 1 calc R . . H3D H 0.5840 -0.0316 0.1495 0.088 Uiso 1 1 calc R . . N4 N 0.7477(5) 0.3842(4) 0.12734(19) 0.0762(19) Uani 1 1 d . . . H4A H 0.8097 0.3612 0.1265 0.091 Uiso 1 1 calc R . . H4B H 0.7003 0.3515 0.1177 0.091 Uiso 1 1 calc R . . N5 N 0.7245(6) 0.0676(4) 0.24824(18) 0.0779(19) Uani 1 1 d . . . H5A H 0.7888 0.0696 0.2379 0.093 Uiso 1 1 calc R . . H5B H 0.6798 0.0654 0.2273 0.093 Uiso 1 1 calc R . . N6 N 0.9007(5) 0.2501(4) 0.0263(2) 0.0805(19) Uani 1 1 d . . . H6A H 0.8403 0.2274 0.0203 0.097 Uiso 1 1 calc R . . H6B H 0.9017 0.2595 0.0532 0.097 Uiso 1 1 calc R . . N7 N 0.8751(5) -0.0692(4) 0.14718(18) 0.0698(17) Uani 1 1 d . . . H7B H 0.8740 -0.0250 0.1608 0.084 Uiso 1 1 calc R . . H7A H 0.8190 -0.0707 0.1310 0.084 Uiso 1 1 calc R . . N8 N 0.7052(5) -0.0881(4) 0.21228(19) 0.0696(17) Uani 1 1 d . . . C45 C 0.3992(8) 0.4898(7) 0.1090(4) 0.115(4) Uani 1 1 d D . . F1 F 0.4315(8) 0.5080(5) 0.0731(3) 0.184(4) Uani 1 1 d D . . F2 F 0.4545(10) 0.5307(5) 0.1329(3) 0.212(5) Uani 1 1 d D . . F3 F 0.3067(7) 0.5182(4) 0.1116(3) 0.199(4) Uani 1 1 d D . . O5 O 0.5097(5) 0.3738(4) 0.1115(2) 0.0985(19) Uani 1 1 d D . . O6 O 0.3384(8) 0.3608(5) 0.0914(4) 0.192(5) Uani 1 1 d D . . O7 O 0.3747(9) 0.3900(5) 0.1594(3) 0.190(5) Uani 1 1 d D . . S1 S 0.4049(2) 0.39357(15) 0.11868(9) 0.0994(8) Uani 1 1 d D . . C46 C 0.6473(15) -0.3160(9) 0.0934(5) 0.152(7) Uani 1 1 d . . . F4 F 0.7028(10) -0.3733(5) 0.1020(4) 0.240(6) Uani 1 1 d . . . F5 F 0.5721(10) -0.3390(6) 0.0719(4) 0.242(7) Uani 1 1 d . . . F6 F 0.6115(10) -0.2914(7) 0.1278(4) 0.211(5) Uani 1 1 d . . . O8 O 0.6396(6) -0.1856(4) 0.0614(2) 0.122(3) Uani 1 1 d . . . O9 O 0.7966(6) -0.2218(4) 0.0962(2) 0.123(3) Uani 1 1 d . . . O10 O 0.7519(9) -0.2753(7) 0.0299(3) 0.182(4) Uani 1 1 d . . . S2 S 0.7194(3) -0.24273(16) 0.06728(9) 0.1091(9) Uani 1 1 d . . . C47 C 0.3584(15) 0.1258(13) 0.2601(8) 0.206(9) Uani 1 1 d U . . F7 F 0.3317(10) 0.1739(7) 0.2316(5) 0.246(7) Uani 1 1 d . . . F8 F 0.2678(11) 0.1234(9) 0.2874(6) 0.374(13) Uani 1 1 d . . . F9 F 0.4127(8) 0.1731(6) 0.2871(3) 0.201(5) Uani 1 1 d U . . O11 O 0.4886(5) 0.0682(4) 0.22640(19) 0.101(2) Uani 1 1 d . . . O12 O 0.3194(7) 0.0145(6) 0.2268(3) 0.156(3) Uani 1 1 d . . . O13 O 0.4249(9) 0.0153(8) 0.2880(3) 0.221(6) Uani 1 1 d . . . S3 S 0.3971(2) 0.0487(2) 0.24854(8) 0.1031(8) Uani 1 1 d . . . C48 C 0.7114(13) 0.2557(10) -0.1226(5) 0.143(6) Uani 1 1 d . . . F10 F 0.6293(7) 0.2369(5) -0.1435(2) 0.170(3) Uani 1 1 d . . . F11 F 0.6881(12) 0.3124(5) -0.0994(4) 0.259(8) Uani 1 1 d . . . F12 F 0.7821(10) 0.2799(9) -0.1471(4) 0.299(10) Uani 1 1 d . . . O14 O 0.7810(6) 0.1228(6) -0.1209(3) 0.142(3) Uani 1 1 d . . . O15 O 0.6721(5) 0.1626(4) -0.0672(2) 0.107(2) Uani 1 1 d . . . O16 O 0.8458(5) 0.2105(4) -0.0709(2) 0.114(2) Uani 1 1 d . . . S4 S 0.75987(19) 0.17961(15) -0.09206(7) 0.0831(6) Uani 1 1 d . . . C49 C 0.9710(10) 0.6268(8) 0.1469(5) 0.322(19) Uani 1 1 d DU . . F13 F 0.959(2) 0.6212(13) 0.1080(4) 0.53(2) Uani 1 1 d D . . F14 F 0.8827(11) 0.6484(8) 0.1604(6) 0.353(12) Uani 1 1 d DU . . F15 F 1.0316(14) 0.6845(8) 0.1524(10) 0.64(3) Uani 1 1 d DU . . O17 O 1.0954(11) 0.5190(11) 0.1414(5) 0.49(2) Uani 1 1 d D . . O18 O 0.9375(9) 0.4967(7) 0.1732(4) 0.251(7) Uani 1 1 d D . . O19 O 1.0599(14) 0.5727(10) 0.2053(4) 0.372(14) Uani 1 1 d DU . . S5 S 1.0171(3) 0.5453(3) 0.16814(18) 0.184(2) Uani 1 1 d DU . . O1W O 0.9328(5) 0.3006(4) 0.11037(19) 0.0932(18) Uani 1 1 d . . . O2W O 0.7012(4) 0.1819(3) 0.01372(17) 0.0807(15) Uani 1 1 d . . . O3W O 0.6804(4) -0.0579(3) 0.10462(16) 0.0773(15) Uani 1 1 d . . . O4W O 0.9110(4) 0.0574(4) 0.20063(17) 0.0861(16) Uani 1 1 d . . . O5W O 1.0830(9) -0.0131(9) 0.2364(3) 0.237(7) Uani 1 1 d . . . O6W O 1.1047(11) 0.3808(10) 0.1143(10) 0.46(2) Uani 1 1 d . . . O7W O 0.833(2) -0.3763(17) -0.0248(11) 0.50(2) 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 Re1 0.0625(2) 0.0559(2) 0.05724(19) -0.00247(14) 0.00435(13) 0.00144(15) O1 0.096(4) 0.061(3) 0.081(4) -0.008(3) -0.007(3) 0.008(3) O2 0.078(4) 0.084(4) 0.094(4) 0.009(3) -0.003(3) -0.004(3) O3 0.105(4) 0.064(3) 0.063(3) -0.001(3) 0.013(3) 0.004(3) O4 0.082(4) 0.083(4) 0.057(3) -0.002(3) 0.006(3) -0.012(3) C1 0.100(7) 0.092(7) 0.097(7) 0.028(6) -0.011(6) 0.015(6) C2 0.102(7) 0.095(7) 0.082(6) 0.015(5) -0.018(5) 0.014(6) C3 0.086(6) 0.106(8) 0.076(5) -0.017(5) -0.027(5) 0.016(6) C4 0.070(5) 0.081(6) 0.070(5) -0.013(4) -0.020(4) 0.007(4) C5 0.102(7) 0.112(9) 0.072(6) -0.027(6) -0.008(5) -0.010(6) C6 0.121(8) 0.086(7) 0.091(7) -0.031(6) -0.003(6) -0.016(6) C7 0.057(5) 0.076(6) 0.093(6) -0.011(5) -0.008(4) -0.013(4) C8 0.080(6) 0.091(7) 0.074(5) -0.009(5) 0.007(4) -0.002(5) C9 0.079(6) 0.087(7) 0.085(6) -0.024(5) 0.001(5) 0.010(5) C10 0.076(6) 0.090(7) 0.090(6) -0.016(5) -0.002(5) -0.027(5) C11 0.087(6) 0.069(6) 0.104(7) 0.005(5) 0.020(5) -0.017(5) C12 0.102(7) 0.084(6) 0.086(6) 0.015(5) 0.017(5) 0.005(6) C13 0.130(8) 0.063(6) 0.107(7) 0.012(5) 0.000(6) -0.017(6) C14 0.103(7) 0.058(5) 0.103(7) -0.010(5) 0.004(5) 0.002(5) C15 0.137(9) 0.065(6) 0.089(6) -0.021(5) 0.018(6) -0.009(6) C16 0.117(8) 0.066(6) 0.072(5) -0.021(4) 0.008(5) 0.000(5) C17 0.093(7) 0.081(7) 0.088(6) -0.019(5) 0.013(5) -0.004(5) C18 0.101(7) 0.077(6) 0.083(6) -0.010(5) 0.008(5) 0.001(5) C19 0.093(7) 0.084(6) 0.062(5) -0.021(4) 0.000(5) 0.004(5) C20 0.104(8) 0.099(8) 0.098(7) -0.016(6) -0.021(6) -0.003(6) C21 0.101(8) 0.082(7) 0.106(7) -0.008(6) -0.007(6) -0.022(6) C22 0.128(8) 0.082(7) 0.059(5) -0.008(4) -0.001(5) 0.011(6) C23 0.111(7) 0.093(7) 0.056(5) 0.008(4) 0.008(5) 0.006(5) C24 0.105(7) 0.095(7) 0.068(5) 0.014(5) 0.003(5) 0.005(6) C25 0.126(9) 0.090(7) 0.097(7) 0.029(6) 0.006(6) 0.009(6) C26 0.094(7) 0.080(6) 0.085(6) 0.019(5) 0.005(5) 0.001(5) C27 0.073(5) 0.092(7) 0.076(5) 0.003(5) 0.013(4) 0.007(5) C28 0.052(4) 0.077(5) 0.067(5) 0.004(4) 0.015(4) 0.011(4) C29 0.049(4) 0.079(5) 0.054(4) 0.000(4) 0.011(3) 0.017(4) C30 0.059(5) 0.083(6) 0.068(5) 0.007(4) 0.013(4) 0.017(4) C31 0.070(5) 0.107(8) 0.064(5) -0.004(5) 0.008(4) 0.017(5) C32 0.063(5) 0.090(6) 0.074(5) -0.004(5) 0.011(4) 0.009(4) C33 0.071(5) 0.083(6) 0.065(5) 0.002(4) 0.017(4) 0.016(5) C34 0.056(4) 0.071(5) 0.066(5) 0.001(4) 0.019(4) 0.013(4) C35 0.063(5) 0.082(6) 0.060(5) 0.004(4) 0.008(4) 0.020(4) C36 0.055(4) 0.087(6) 0.068(5) -0.001(4) 0.004(4) 0.010(4) C37 0.070(5) 0.110(8) 0.077(6) 0.006(5) -0.005(4) 0.009(5) C38 0.084(7) 0.140(10) 0.097(8) -0.016(8) -0.021(6) 0.000(7) C39 0.072(7) 0.130(10) 0.122(9) -0.018(8) -0.015(6) -0.018(7) C40 0.077(6) 0.083(6) 0.101(7) -0.011(5) 0.002(5) 0.004(5) C41 0.053(4) 0.090(6) 0.070(5) -0.004(4) 0.009(4) 0.017(4) C42 0.064(5) 0.090(6) 0.075(5) 0.006(4) 0.013(4) 0.019(4) C43 0.104(7) 0.074(6) 0.080(6) 0.017(4) 0.021(5) 0.022(5) C44 0.105(7) 0.067(6) 0.083(6) 0.014(4) 0.014(5) 0.007(5) N1 0.090(5) 0.063(4) 0.083(5) 0.007(4) 0.003(4) 0.015(4) N2 0.076(4) 0.087(5) 0.064(4) -0.004(4) -0.007(3) 0.013(4) N3 0.068(4) 0.071(5) 0.080(4) -0.010(3) 0.009(3) -0.014(3) N4 0.092(5) 0.047(4) 0.089(5) -0.009(3) -0.001(4) 0.004(3) N5 0.095(5) 0.084(5) 0.054(4) -0.004(3) 0.004(3) 0.007(4) N6 0.081(5) 0.075(5) 0.085(5) 0.009(4) 0.012(4) 0.005(4) N7 0.074(4) 0.068(4) 0.068(4) 0.007(3) 0.002(3) 0.009(3) N8 0.083(4) 0.060(4) 0.065(4) 0.003(3) 0.009(3) -0.008(3) C45 0.121(9) 0.110(10) 0.113(9) 0.006(8) 0.016(7) 0.038(8) F1 0.249(10) 0.160(7) 0.143(6) 0.057(6) 0.043(7) 0.072(7) F2 0.329(15) 0.101(6) 0.205(9) -0.015(6) -0.053(9) -0.034(7) F3 0.156(7) 0.111(6) 0.331(13) 0.038(7) 0.060(8) 0.062(5) O5 0.094(4) 0.091(4) 0.111(5) -0.009(4) 0.019(4) 0.019(4) O6 0.143(8) 0.128(8) 0.305(16) -0.080(9) -0.065(9) 0.026(6) O7 0.273(13) 0.124(7) 0.173(9) 0.035(6) 0.136(9) 0.067(8) S1 0.1010(19) 0.0745(17) 0.123(2) -0.0154(15) 0.0214(16) 0.0107(14) C46 0.212(17) 0.090(10) 0.155(13) 0.008(10) -0.106(14) -0.024(11) F4 0.299(14) 0.077(5) 0.345(15) 0.059(8) -0.143(12) -0.013(7) F5 0.298(13) 0.184(9) 0.243(11) 0.078(8) -0.153(11) -0.138(9) F6 0.276(13) 0.183(11) 0.174(9) 0.053(8) -0.029(9) -0.067(9) O8 0.146(6) 0.079(5) 0.142(6) 0.012(4) -0.056(5) 0.012(5) O9 0.130(6) 0.092(5) 0.148(6) 0.007(4) -0.064(5) -0.009(4) O10 0.213(11) 0.195(11) 0.139(8) -0.056(7) -0.011(7) 0.030(8) S2 0.139(2) 0.0760(18) 0.112(2) -0.0041(15) -0.0422(19) -0.0043(17) C47 0.128(13) 0.166(19) 0.32(3) 0.051(16) -0.058(17) -0.067(13) F7 0.248(13) 0.153(9) 0.337(17) -0.053(10) -0.087(12) 0.079(9) F8 0.231(12) 0.339(17) 0.55(3) -0.227(18) 0.270(17) -0.108(12) F9 0.214(9) 0.186(8) 0.204(9) -0.093(7) 0.106(8) -0.054(7) O11 0.120(5) 0.085(4) 0.097(4) -0.005(3) 0.045(4) -0.008(4) O12 0.135(7) 0.150(8) 0.182(9) -0.047(7) -0.003(6) -0.033(6) O13 0.200(11) 0.297(15) 0.165(9) 0.132(10) 0.013(8) -0.033(10) S3 0.110(2) 0.111(2) 0.0882(17) -0.0067(16) 0.0256(15) -0.0175(18) C48 0.169(14) 0.127(13) 0.132(11) 0.041(10) -0.062(10) -0.055(11) F10 0.181(7) 0.156(7) 0.173(7) 0.058(5) -0.108(6) -0.037(6) F11 0.371(18) 0.078(6) 0.328(16) 0.021(8) -0.201(15) 0.020(8) F12 0.259(12) 0.43(2) 0.213(11) 0.236(14) -0.104(9) -0.183(14) O14 0.096(6) 0.163(8) 0.167(8) -0.065(6) -0.005(5) 0.009(5) O15 0.103(5) 0.133(6) 0.086(4) 0.026(4) -0.001(4) -0.023(4) O16 0.115(5) 0.122(6) 0.106(5) 0.033(4) -0.046(4) -0.045(5) S4 0.0858(16) 0.0862(16) 0.0773(14) 0.0119(12) -0.0135(12) -0.0102(13) C49 0.103(13) 0.35(4) 0.51(5) 0.23(3) -0.016(18) -0.030(17) F13 0.48(4) 0.70(5) 0.40(3) 0.38(3) 0.11(3) 0.21(4) F14 0.215(15) 0.33(2) 0.51(3) 0.141(19) 0.046(18) 0.036(14) F15 0.28(2) 0.41(3) 1.23(7) 0.29(4) -0.14(3) -0.17(2) O17 0.227(19) 0.70(6) 0.55(4) -0.30(4) 0.00(2) 0.18(3) O18 0.180(11) 0.273(16) 0.300(17) 0.111(14) -0.011(11) -0.080(12) O19 0.37(2) 0.50(4) 0.244(17) 0.047(17) -0.176(18) 0.05(2) S5 0.105(3) 0.209(5) 0.237(6) 0.041(4) -0.011(3) 0.011(3) O1W 0.083(4) 0.088(4) 0.109(5) -0.005(4) 0.002(3) 0.009(3) O2W 0.073(3) 0.085(4) 0.084(4) 0.000(3) 0.018(3) 0.008(3) O3W 0.081(4) 0.073(4) 0.078(3) -0.001(3) 0.010(3) 0.008(3) O4W 0.081(4) 0.103(5) 0.075(4) -0.008(3) -0.002(3) 0.007(3) O5W 0.169(9) 0.359(18) 0.181(10) 0.115(11) -0.062(8) 0.010(11) O6W 0.126(10) 0.203(15) 1.04(7) -0.20(3) 0.05(2) -0.047(10) O7W 0.43(4) 0.46(4) 0.61(5) -0.25(4) -0.20(4) 0.13(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Re1 O2 1.712(6) . ? Re1 O1 1.715(5) . ? Re1 O4 1.717(5) . ? Re1 O3 1.719(5) . ? C1 N1 1.448(11) . ? C1 C2 1.537(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.479(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.499(11) . ? C3 C4 1.503(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.379(13) . ? C4 C9 1.388(12) . ? C5 C6 1.389(14) . ? C5 H5 0.9300 . ? C6 C7 1.341(12) . ? C6 H6 0.9300 . ? C7 C8 1.398(12) . ? C7 C10 1.523(12) . ? C8 C9 1.355(13) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N3 1.476(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N3 1.499(11) . ? C11 C12 1.511(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N8 1.454(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.487(11) . ? C13 C14 1.514(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.501(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.488(13) . ? C15 N4 1.506(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.383(13) . ? C16 C21 1.390(14) . ? C17 C18 1.373(13) . ? C17 H17 0.9300 . ? C18 C19 1.381(13) . ? C18 H18 0.9300 . ? C19 C20 1.384(13) . ? C19 C22 1.503(13) . ? C20 C21 1.336(14) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 N5 1.475(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N5 1.480(10) . ? C23 C24 1.519(12) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N8 1.482(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N1 1.481(12) . ? C25 C26 1.526(14) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N6 1.477(11) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.521(11) . ? C27 N6 1.528(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C41 1.399(11) . ? C28 C29 1.424(11) . ? C29 C30 1.422(11) . ? C29 C34 1.436(11) . ? C30 C31 1.352(12) . ? C30 H30 0.9300 . ? C31 C32 1.390(12) . ? C31 H31 0.9300 . ? C32 C33 1.328(11) . ? C32 H32 0.9300 . ? C33 C34 1.445(12) . ? C33 H33 0.9300 . ? C34 C35 1.416(11) . ? C35 C36 1.392(12) . ? C35 C42 1.498(11) . ? C36 C37 1.432(11) . ? C36 C41 1.460(12) . ? C37 C38 1.338(14) . ? C37 H37 0.9300 . ? C38 C39 1.399(17) . ? C38 H38 0.9300 . ? C39 C40 1.310(13) . ? C39 H39 0.9300 . ? C40 C41 1.448(13) . ? C40 H40 0.9300 . ? C42 N7 1.528(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 N7 1.459(10) . ? C43 C44 1.522(13) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N8 1.481(10) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 H7B 0.9000 . ? N7 H7A 0.9000 . ? C45 F2 1.284(12) . ? C45 F1 1.293(12) . ? C45 F3 1.302(11) . ? C45 S1 1.731(12) . ? O5 S1 1.421(6) . ? O6 S1 1.370(9) . ? O7 S1 1.397(8) . ? C46 F5 1.269(15) . ? C46 F4 1.272(18) . ? C46 F6 1.30(2) . ? C46 S2 1.813(18) . ? O8 S2 1.457(8) . ? O9 S2 1.428(7) . ? O10 S2 1.422(9) . ? C47 F7 1.31(2) . ? C47 F9 1.41(2) . ? C47 F8 1.48(2) . ? C47 S3 1.50(3) . ? O11 S3 1.433(6) . ? O12 S3 1.373(9) . ? O13 S3 1.471(10) . ? C48 F12 1.294(18) . ? C48 F11 1.30(2) . ? C48 F10 1.307(13) . ? C48 S4 1.791(15) . ? O14 S4 1.407(8) . ? O15 S4 1.434(7) . ? O16 S4 1.422(6) . ? C49 F14 1.285(14) . ? C49 F13 1.291(15) . ? C49 F15 1.298(13) . ? C49 S5 1.707(13) . ? O17 S5 1.420(9) . ? O18 S5 1.352(9) . ? O19 S5 1.426(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Re1 O1 108.8(3) . . ? O2 Re1 O4 109.1(3) . . ? O1 Re1 O4 112.0(3) . . ? O2 Re1 O3 109.9(3) . . ? O1 Re1 O3 108.7(3) . . ? O4 Re1 O3 108.4(3) . . ? N1 C1 C2 114.4(8) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N2 C2 C1 112.8(8) . . ? N2 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N2 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 112.6(7) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C9 117.0(9) . . ? C5 C4 C3 120.7(8) . . ? C9 C4 C3 122.2(8) . . ? C4 C5 C6 120.5(9) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 121.3(9) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 119.3(9) . . ? C6 C7 C10 120.2(9) . . ? C8 C7 C10 120.4(8) . . ? C9 C8 C7 119.1(8) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.5 . . ? C8 C9 C4 122.7(9) . . ? C8 C9 H9 118.6 . . ? C4 C9 H9 118.6 . . ? N3 C10 C7 113.6(7) . . ? N3 C10 H10A 108.8 . . ? C7 C10 H10A 108.9 . . ? N3 C10 H10B 108.8 . . ? C7 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N3 C11 C12 112.7(7) . . ? N3 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N3 C11 H11B 109.0 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N8 C12 C11 114.8(7) . . ? N8 C12 H12A 108.6 . . ? C11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? C11 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? N1 C13 C14 114.3(8) . . ? N1 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? N1 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? N4 C14 C13 113.2(7) . . ? N4 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? N4 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.8 . . ? C16 C15 N4 111.8(7) . . ? C16 C15 H15A 109.2 . . ? N4 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? N4 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C21 119.5(10) . . ? C17 C16 C15 119.3(10) . . ? C21 C16 C15 121.2(10) . . ? C18 C17 C16 119.4(10) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 121.9(10) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C18 C19 C20 116.3(10) . . ? C18 C19 C22 119.4(9) . . ? C20 C19 C22 124.2(10) . . ? C21 C20 C19 123.7(11) . . ? C21 C20 H20 118.1 . . ? C19 C20 H20 118.1 . . ? C20 C21 C16 119.1(10) . . ? C20 C21 H21 120.4 . . ? C16 C21 H21 120.4 . . ? N5 C22 C19 111.9(7) . . ? N5 C22 H22A 109.2 . . ? C19 C22 H22A 109.2 . . ? N5 C22 H22B 109.2 . . ? C19 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? N5 C23 C24 112.3(6) . . ? N5 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? N5 C23 H23B 109.2 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? N8 C24 C23 114.6(8) . . ? N8 C24 H24A 108.6 . . ? C23 C24 H24A 108.6 . . ? N8 C24 H24B 108.6 . . ? C23 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? N1 C25 C26 116.7(8) . . ? N1 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? N1 C25 H25B 108.1 . . ? C26 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? N6 C26 C25 112.0(8) . . ? N6 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? N6 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 N6 111.2(6) . . ? C28 C27 H27A 109.4 . . ? N6 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? N6 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C41 C28 C29 120.2(7) . . ? C41 C28 C27 120.5(8) . . ? C29 C28 C27 119.3(7) . . ? C30 C29 C28 121.9(7) . . ? C30 C29 C34 118.6(8) . . ? C28 C29 C34 119.5(7) . . ? C31 C30 C29 121.6(8) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C32 120.3(8) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 120.8(9) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 122.7(8) . . ? C32 C33 H33 118.6 . . ? C34 C33 H33 118.6 . . ? C35 C34 C29 120.7(8) . . ? C35 C34 C33 123.3(8) . . ? C29 C34 C33 116.0(7) . . ? C36 C35 C34 119.3(7) . . ? C36 C35 C42 120.8(7) . . ? C34 C35 C42 119.9(8) . . ? C35 C36 C37 122.5(8) . . ? C35 C36 C41 120.9(7) . . ? C37 C36 C41 116.6(8) . . ? C38 C37 C36 121.6(10) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C39 121.8(10) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C40 C39 C38 120.3(11) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 122.3(10) . . ? C39 C40 H40 118.8 . . ? C41 C40 H40 118.8 . . ? C28 C41 C40 123.4(9) . . ? C28 C41 C36 119.3(8) . . ? C40 C41 C36 117.3(8) . . ? C35 C42 N7 111.2(6) . . ? C35 C42 H42A 109.4 . . ? N7 C42 H42A 109.4 . . ? C35 C42 H42B 109.4 . . ? N7 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? N7 C43 C44 115.4(7) . . ? N7 C43 H43A 108.4 . . ? C44 C43 H43A 108.4 . . ? N7 C43 H43B 108.4 . . ? C44 C43 H43B 108.4 . . ? H43A C43 H43B 107.5 . . ? N8 C44 C43 116.6(7) . . ? N8 C44 H44A 108.1 . . ? C43 C44 H44A 108.1 . . ? N8 C44 H44B 108.1 . . ? C43 C44 H44B 108.1 . . ? H44A C44 H44B 107.3 . . ? C1 N1 C25 108.2(8) . . ? C1 N1 C13 107.3(8) . . ? C25 N1 C13 109.6(8) . . ? C2 N2 C3 113.4(7) . . ? C2 N2 H2C 108.9 . . ? C3 N2 H2C 108.9 . . ? C2 N2 H2D 108.9 . . ? C3 N2 H2D 108.9 . . ? H2C N2 H2D 107.7 . . ? C10 N3 C11 113.7(7) . . ? C10 N3 H3C 108.8 . . ? C11 N3 H3C 108.8 . . ? C10 N3 H3D 108.8 . . ? C11 N3 H3D 108.8 . . ? H3C N3 H3D 107.7 . . ? C14 N4 C15 112.2(6) . . ? C14 N4 H4A 109.2 . . ? C15 N4 H4A 109.2 . . ? C14 N4 H4B 109.2 . . ? C15 N4 H4B 109.2 . . ? H4A N4 H4B 107.9 . . ? C22 N5 C23 111.8(6) . . ? C22 N5 H5A 109.3 . . ? C23 N5 H5A 109.3 . . ? C22 N5 H5B 109.3 . . ? C23 N5 H5B 109.3 . . ? H5A N5 H5B 107.9 . . ? C26 N6 C27 112.1(6) . . ? C26 N6 H6A 109.2 . . ? C27 N6 H6A 109.2 . . ? C26 N6 H6B 109.2 . . ? C27 N6 H6B 109.2 . . ? H6A N6 H6B 107.9 . . ? C43 N7 C42 112.9(6) . . ? C43 N7 H7B 109.0 . . ? C42 N7 H7B 109.0 . . ? C43 N7 H7A 109.0 . . ? C42 N7 H7A 109.0 . . ? H7B N7 H7A 107.8 . . ? C12 N8 C44 109.0(7) . . ? C12 N8 C24 107.5(7) . . ? C44 N8 C24 109.3(7) . . ? F2 C45 F1 103.9(11) . . ? F2 C45 F3 104.8(11) . . ? F1 C45 F3 105.3(10) . . ? F2 C45 S1 114.5(8) . . ? F1 C45 S1 113.5(9) . . ? F3 C45 S1 113.8(9) . . ? O6 S1 O7 115.6(8) . . ? O6 S1 O5 112.7(5) . . ? O7 S1 O5 114.7(6) . . ? O6 S1 C45 105.5(5) . . ? O7 S1 C45 102.1(6) . . ? O5 S1 C45 104.5(5) . . ? F5 C46 F4 107.7(14) . . ? F5 C46 F6 109(2) . . ? F4 C46 F6 105.9(14) . . ? F5 C46 S2 111.1(11) . . ? F4 C46 S2 112.4(15) . . ? F6 C46 S2 111.0(11) . . ? O10 S2 O9 118.3(6) . . ? O10 S2 O8 112.0(6) . . ? O9 S2 O8 114.0(5) . . ? O10 S2 C46 105.9(8) . . ? O9 S2 C46 103.3(6) . . ? O8 S2 C46 101.0(7) . . ? F7 C47 F9 101.5(17) . . ? F7 C47 F8 104(2) . . ? F9 C47 F8 91.7(19) . . ? F7 C47 S3 120(2) . . ? F9 C47 S3 122.2(16) . . ? F8 C47 S3 113.2(14) . . ? O12 S3 O11 116.5(5) . . ? O12 S3 O13 117.6(7) . . ? O11 S3 O13 110.1(6) . . ? O12 S3 C47 106.6(9) . . ? O11 S3 C47 100.8(8) . . ? O13 S3 C47 102.7(12) . . ? F12 C48 F11 106.1(15) . . ? F12 C48 F10 109.5(13) . . ? F11 C48 F10 108.4(17) . . ? F12 C48 S4 110.5(14) . . ? F11 C48 S4 109.3(10) . . ? F10 C48 S4 112.9(10) . . ? O14 S4 O16 116.8(5) . . ? O14 S4 O15 113.0(5) . . ? O16 S4 O15 114.9(4) . . ? O14 S4 C48 103.0(7) . . ? O16 S4 C48 105.2(5) . . ? O15 S4 C48 101.6(7) . . ? F14 C49 F13 105.1(13) . . ? F14 C49 F15 104.9(14) . . ? F13 C49 F15 105.7(12) . . ? F14 C49 S5 114.7(10) . . ? F13 C49 S5 112.5(11) . . ? F15 C49 S5 113.2(11) . . ? O18 S5 O17 114.4(9) . . ? O18 S5 O19 113.9(9) . . ? O17 S5 O19 111.4(8) . . ? O18 S5 C49 108.6(6) . . ? O17 S5 C49 105.8(8) . . ? O19 S5 C49 101.6(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.923 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.110 _iucr_refine_instructions_details ; TITL 1H6_ReO4 in P 21/c CELL 0.71073 12.9487 17.6577 32.8972 90.000 90.081 90.000 ZERR 4.00 0.0021 0.0030 0.0053 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H F N O RE S UNIT 196 312 60 32 104 4 20 MERG 2 FMAP 2 OMIT -2 50 DELU 0.01 0.01 F9 C47 DELU 0.01 0.01 S5 O19 DELU 0.01 0.01 F14 C49 PLAN 25 SIZE 0.3 0.15 0.1 ISOR 0.1 0.1 C49 F15 HTAB ACTA BOND $H L.S. 6 LIST 4 WGHT 0.101600 3.441000 FVAR 0.16394 RE1 6 0.726619 0.146197 0.124538 11.00000 0.06251 0.05587 = 0.05724 -0.00247 0.00435 0.00144 O1 5 0.671031 0.231959 0.113535 11.00000 0.09637 0.06067 = 0.08110 -0.00838 -0.00737 0.00755 O2 5 0.852555 0.160751 0.138432 11.00000 0.07761 0.08383 = 0.09392 0.00933 -0.00304 -0.00350 O3 5 0.721488 0.090158 0.081852 11.00000 0.10547 0.06382 = 0.06281 -0.00097 0.01291 0.00438 O4 5 0.663567 0.100196 0.163231 11.00000 0.08161 0.08301 = 0.05651 -0.00186 0.00620 -0.01248 C1 1 0.642003 0.404304 0.024309 11.00000 0.10026 0.09164 = 0.09721 0.02757 -0.01088 0.01500 AFIX 23 H1A 2 0.650605 0.441609 0.002936 11.00000 -1.20000 H1B 2 0.611253 0.429730 0.047458 11.00000 -1.20000 AFIX 0 C2 1 0.567140 0.342763 0.009292 11.00000 0.10181 0.09504 = 0.08213 0.01528 -0.01763 0.01403 AFIX 23 H2A 2 0.501575 0.366086 0.002422 11.00000 -1.20000 H2B 2 0.594800 0.320060 -0.015236 11.00000 -1.20000 AFIX 0 C3 1 0.460185 0.231998 0.029641 11.00000 0.08601 0.10598 = 0.07577 -0.01700 -0.02729 0.01570 AFIX 23 H3A 2 0.466288 0.215587 0.001607 11.00000 -1.20000 H3B 2 0.396473 0.260503 0.032140 11.00000 -1.20000 AFIX 0 C4 1 0.454742 0.163505 0.056703 11.00000 0.06953 0.08106 = 0.07016 -0.01320 -0.01975 0.00707 C5 1 0.463425 0.091580 0.040725 11.00000 0.10240 0.11239 = 0.07173 -0.02744 -0.00813 -0.01016 AFIX 43 H5 2 0.473102 0.085271 0.012924 11.00000 -1.20000 AFIX 0 C6 1 0.457824 0.028474 0.065855 11.00000 0.12144 0.08635 = 0.09095 -0.03127 -0.00281 -0.01583 AFIX 43 H6 2 0.463927 -0.019605 0.054569 11.00000 -1.20000 AFIX 0 C7 1 0.443798 0.035507 0.106044 11.00000 0.05704 0.07630 = 0.09253 -0.01059 -0.00771 -0.01292 C8 1 0.432968 0.107750 0.122924 11.00000 0.07993 0.09058 = 0.07437 -0.00944 0.00703 -0.00152 AFIX 43 H8 2 0.422239 0.113611 0.150693 11.00000 -1.20000 AFIX 0 C9 1 0.438321 0.169111 0.098265 11.00000 0.07869 0.08666 = 0.08474 -0.02384 0.00101 0.01004 AFIX 43 H9 2 0.430669 0.216966 0.109678 11.00000 -1.20000 AFIX 0 C10 1 0.438535 -0.034613 0.132907 11.00000 0.07619 0.09025 = 0.08951 -0.01616 -0.00181 -0.02723 AFIX 23 H10A 2 0.373529 -0.034330 0.147523 11.00000 -1.20000 H10B 2 0.439466 -0.079289 0.115754 11.00000 -1.20000 AFIX 0 C11 1 0.529874 -0.114757 0.183843 11.00000 0.08733 0.06910 = 0.10360 0.00460 0.01995 -0.01656 AFIX 23 H11A 2 0.554685 -0.152730 0.164921 11.00000 -1.20000 H11B 2 0.461105 -0.129505 0.192412 11.00000 -1.20000 AFIX 0 C12 1 0.600270 -0.113015 0.220514 11.00000 0.10181 0.08353 = 0.08581 0.01522 0.01746 0.00458 AFIX 23 H12A 2 0.570331 -0.079606 0.240721 11.00000 -1.20000 H12B 2 0.602959 -0.163434 0.232173 11.00000 -1.20000 AFIX 0 C13 1 0.795243 0.437843 0.058995 11.00000 0.13041 0.06332 = 0.10730 0.01152 -0.00043 -0.01697 AFIX 23 H13A 2 0.791822 0.484054 0.043107 11.00000 -1.20000 H13B 2 0.867546 0.424725 0.062182 11.00000 -1.20000 AFIX 0 C14 1 0.749904 0.453064 0.100585 11.00000 0.10325 0.05757 = 0.10321 -0.01037 0.00405 0.00226 AFIX 23 H14A 2 0.790197 0.492244 0.113859 11.00000 -1.20000 H14B 2 0.680047 0.471980 0.097340 11.00000 -1.20000 AFIX 0 C15 1 0.722243 0.403478 0.170792 11.00000 0.13668 0.06470 = 0.08887 -0.02074 0.01811 -0.00890 AFIX 23 H15A 2 0.773481 0.438558 0.181219 11.00000 -1.20000 H15B 2 0.655514 0.428370 0.171769 11.00000 -1.20000 AFIX 0 C16 1 0.719769 0.334895 0.197058 11.00000 0.11651 0.06554 = 0.07218 -0.02102 0.00803 -0.00047 C17 1 0.626279 0.299786 0.204612 11.00000 0.09267 0.08083 = 0.08823 -0.01905 0.01271 -0.00354 AFIX 43 H17 2 0.565666 0.318880 0.193401 11.00000 -1.20000 AFIX 0 C18 1 0.623789 0.236477 0.228817 11.00000 0.10065 0.07699 = 0.08349 -0.00991 0.00753 0.00130 AFIX 43 H18 2 0.560840 0.212716 0.233535 11.00000 -1.20000 AFIX 0 C19 1 0.712066 0.207044 0.246367 11.00000 0.09264 0.08379 = 0.06208 -0.02104 -0.00028 0.00375 C20 1 0.803529 0.244233 0.237716 11.00000 0.10425 0.09895 = 0.09843 -0.01620 -0.02090 -0.00288 AFIX 43 H20 2 0.864189 0.225567 0.249096 11.00000 -1.20000 AFIX 0 C21 1 0.809634 0.305399 0.213955 11.00000 0.10103 0.08156 = 0.10587 -0.00810 -0.00692 -0.02164 AFIX 43 H21 2 0.873170 0.327960 0.208782 11.00000 -1.20000 AFIX 0 C22 1 0.704631 0.136859 0.272052 11.00000 0.12819 0.08165 = 0.05916 -0.00821 -0.00070 0.01142 AFIX 23 H22A 2 0.754287 0.140056 0.294090 11.00000 -1.20000 H22B 2 0.636200 0.133930 0.283907 11.00000 -1.20000 AFIX 0 C23 1 0.713718 -0.001529 0.273306 11.00000 0.11121 0.09262 = 0.05583 0.00812 0.00771 0.00637 AFIX 23 H23A 2 0.641379 -0.009172 0.279735 11.00000 -1.20000 H23B 2 0.750790 0.005427 0.298675 11.00000 -1.20000 AFIX 0 C24 1 0.754952 -0.071487 0.251892 11.00000 0.10502 0.09485 = 0.06844 0.01418 0.00318 0.00491 AFIX 23 H24A 2 0.828512 -0.065076 0.247549 11.00000 -1.20000 H24B 2 0.745771 -0.114839 0.269633 11.00000 -1.20000 AFIX 0 C25 1 0.801678 0.359444 -0.001479 11.00000 0.12638 0.08996 = 0.09681 0.02934 0.00617 0.00931 AFIX 23 H25A 2 0.811118 0.406455 -0.016269 11.00000 -1.20000 H25B 2 0.759863 0.326438 -0.018374 11.00000 -1.20000 AFIX 0 C26 1 0.907368 0.322551 0.003990 11.00000 0.09435 0.07973 = 0.08469 0.01916 0.00548 0.00088 AFIX 23 H26A 2 0.937775 0.313560 -0.022505 11.00000 -1.20000 H26B 2 0.952301 0.356918 0.018723 11.00000 -1.20000 AFIX 0 C27 1 0.989411 0.196650 0.015668 11.00000 0.07324 0.09154 = 0.07593 0.00268 0.01335 0.00739 AFIX 23 H27A 2 0.983623 0.181542 -0.012592 11.00000 -1.20000 H27B 2 1.054609 0.222953 0.019099 11.00000 -1.20000 AFIX 0 C28 1 0.988135 0.126549 0.042534 11.00000 0.05186 0.07714 = 0.06736 0.00450 0.01497 0.01150 C29 1 0.927599 0.062917 0.030654 11.00000 0.04932 0.07857 = 0.05406 -0.00009 0.01056 0.01684 C30 1 0.869402 0.062398 -0.006042 11.00000 0.05889 0.08330 = 0.06835 0.00701 0.01296 0.01653 AFIX 43 H30 2 0.871502 0.104532 -0.022983 11.00000 -1.20000 AFIX 0 C31 1 0.811120 0.002190 -0.016905 11.00000 0.06962 0.10737 = 0.06351 -0.00436 0.00760 0.01662 AFIX 43 H31 2 0.773465 0.003470 -0.040989 11.00000 -1.20000 AFIX 0 C32 1 0.807240 -0.061627 0.007774 11.00000 0.06328 0.08968 = 0.07358 -0.00356 0.01132 0.00941 AFIX 43 H32 2 0.767400 -0.102947 -0.000083 11.00000 -1.20000 AFIX 0 C33 1 0.859763 -0.064284 0.042444 11.00000 0.07102 0.08268 = 0.06476 0.00227 0.01717 0.01582 AFIX 43 H33 2 0.855512 -0.107822 0.058261 11.00000 -1.20000 AFIX 0 C34 1 0.923247 -0.002348 0.056621 11.00000 0.05630 0.07130 = 0.06562 0.00118 0.01867 0.01278 C35 1 0.979059 -0.004221 0.093659 11.00000 0.06293 0.08186 = 0.06019 0.00445 0.00835 0.02025 C36 1 1.042862 0.056420 0.103729 11.00000 0.05469 0.08685 = 0.06774 -0.00139 0.00377 0.01036 C37 1 1.105536 0.057009 0.139636 11.00000 0.06964 0.10995 = 0.07717 0.00590 -0.00469 0.00869 AFIX 43 H37 2 1.105241 0.014965 0.156662 11.00000 -1.20000 AFIX 0 C38 1 1.164516 0.116625 0.149269 11.00000 0.08353 0.14013 = 0.09665 -0.01644 -0.02052 -0.00017 AFIX 43 H38 2 1.203583 0.115136 0.172999 11.00000 -1.20000 AFIX 0 C39 1 1.169038 0.181115 0.124640 11.00000 0.07227 0.13021 = 0.12217 -0.01801 -0.01474 -0.01844 AFIX 43 H39 2 1.210322 0.221823 0.132260 11.00000 -1.20000 AFIX 0 C40 1 1.115408 0.184445 0.090896 11.00000 0.07688 0.08291 = 0.10138 -0.01080 0.00218 0.00447 AFIX 43 H40 2 1.121131 0.227283 0.074608 11.00000 -1.20000 AFIX 0 C41 1 1.047507 0.123781 0.078050 11.00000 0.05337 0.08964 = 0.07038 -0.00356 0.00948 0.01739 C42 1 0.971967 -0.072193 0.120762 11.00000 0.06432 0.09000 = 0.07483 0.00581 0.01329 0.01934 AFIX 23 H42A 2 1.032606 -0.074446 0.138066 11.00000 -1.20000 H42B 2 0.970551 -0.117709 0.104261 11.00000 -1.20000 AFIX 0 C43 1 0.869666 -0.131410 0.176320 11.00000 0.10423 0.07405 = 0.07988 0.01735 0.02072 0.02179 AFIX 23 H43A 2 0.913020 -0.118970 0.199445 11.00000 -1.20000 H43B 2 0.898256 -0.176401 0.163702 11.00000 -1.20000 AFIX 0 C44 1 0.761930 -0.150106 0.191814 11.00000 0.10503 0.06713 = 0.08315 0.01379 0.01433 0.00655 AFIX 23 H44A 2 0.720745 -0.167309 0.168957 11.00000 -1.20000 H44B 2 0.767608 -0.192113 0.210686 11.00000 -1.20000 AFIX 0 N1 4 0.742846 0.376328 0.036018 11.00000 0.08967 0.06298 = 0.08296 0.00693 0.00312 0.01470 N2 4 0.549408 0.282686 0.039802 11.00000 0.07640 0.08724 = 0.06424 -0.00382 -0.00704 0.01342 AFIX 23 H2C 2 0.537845 0.304418 0.064121 11.00000 -1.20000 H2D 2 0.606936 0.254367 0.041994 11.00000 -1.20000 AFIX 0 N3 4 0.523941 -0.039861 0.162522 11.00000 0.06836 0.07119 = 0.08008 -0.01038 0.00857 -0.01445 AFIX 23 H3C 2 0.516279 -0.003080 0.181216 11.00000 -1.20000 H3D 2 0.583971 -0.031564 0.149505 11.00000 -1.20000 AFIX 0 N4 4 0.747656 0.384210 0.127340 11.00000 0.09186 0.04731 = 0.08933 -0.00925 -0.00134 0.00410 AFIX 23 H4A 2 0.809654 0.361232 0.126464 11.00000 -1.20000 H4B 2 0.700262 0.351469 0.117741 11.00000 -1.20000 AFIX 0 N5 4 0.724486 0.067592 0.248243 11.00000 0.09539 0.08447 = 0.05372 -0.00381 0.00380 0.00733 AFIX 23 H5A 2 0.788781 0.069569 0.237941 11.00000 -1.20000 H5B 2 0.679776 0.065389 0.227305 11.00000 -1.20000 AFIX 0 N6 4 0.900661 0.250115 0.026303 11.00000 0.08146 0.07492 = 0.08504 0.00946 0.01217 0.00488 AFIX 23 H6A 2 0.840267 0.227433 0.020341 11.00000 -1.20000 H6B 2 0.901661 0.259473 0.053194 11.00000 -1.20000 AFIX 0 N7 4 0.875137 -0.069234 0.147183 11.00000 0.07360 0.06787 = 0.06790 0.00724 0.00228 0.00895 AFIX 23 H7B 2 0.874048 -0.025005 0.160772 11.00000 -1.20000 H7A 2 0.819017 -0.070733 0.131031 11.00000 -1.20000 AFIX 0 N8 4 0.705207 -0.088110 0.212281 11.00000 0.08326 0.06044 = 0.06507 0.00337 0.00931 -0.00781 C45 1 0.399244 0.489816 0.108980 11.00000 0.12069 0.11045 = 0.11305 0.00610 0.01591 0.03783 F1 3 0.431451 0.508016 0.073102 11.00000 0.24897 0.16011 = 0.14319 0.05737 0.04330 0.07159 F2 3 0.454468 0.530654 0.132917 11.00000 0.32852 0.10123 = 0.20478 -0.01475 -0.05276 -0.03424 F3 3 0.306677 0.518155 0.111641 11.00000 0.15579 0.11125 = 0.33064 0.03750 0.06046 0.06171 O5 5 0.509714 0.373814 0.111476 11.00000 0.09402 0.09051 = 0.11091 -0.00900 0.01865 0.01879 O6 5 0.338441 0.360837 0.091420 11.00000 0.14309 0.12848 = 0.30546 -0.07968 -0.06516 0.02607 O7 5 0.374703 0.389979 0.159377 11.00000 0.27269 0.12360 = 0.17283 0.03546 0.13587 0.06677 S1 7 0.404940 0.393573 0.118680 11.00000 0.10099 0.07448 = 0.12285 -0.01538 0.02143 0.01068 C46 1 0.647274 -0.316049 0.093378 11.00000 0.21230 0.08966 = 0.15519 0.00837 -0.10648 -0.02419 F4 3 0.702791 -0.373292 0.102038 11.00000 0.29935 0.07661 = 0.34510 0.05888 -0.14297 -0.01284 F5 3 0.572103 -0.338967 0.071886 11.00000 0.29768 0.18431 = 0.24299 0.07796 -0.15348 -0.13822 F6 3 0.611456 -0.291369 0.127802 11.00000 0.27606 0.18290 = 0.17411 0.05286 -0.02898 -0.06663 O8 5 0.639593 -0.185628 0.061359 11.00000 0.14600 0.07921 = 0.14206 0.01153 -0.05623 0.01228 O9 5 0.796604 -0.221845 0.096221 11.00000 0.13009 0.09180 = 0.14769 0.00663 -0.06376 -0.00945 O10 5 0.751939 -0.275294 0.029876 11.00000 0.21336 0.19468 = 0.13872 -0.05588 -0.01057 0.02963 S2 7 0.719433 -0.242735 0.067280 11.00000 0.13930 0.07599 = 0.11188 -0.00412 -0.04216 -0.00427 C47 1 0.358427 0.125806 0.260125 11.00000 0.12751 0.16582 = 0.32481 0.05095 -0.05816 -0.06702 F7 3 0.331710 0.173864 0.231589 11.00000 0.24826 0.15258 = 0.33686 -0.05330 -0.08661 0.07896 F8 3 0.267763 0.123428 0.287439 11.00000 0.23114 0.33894 = 0.55168 -0.22653 0.27020 -0.10793 F9 3 0.412738 0.173079 0.287085 11.00000 0.21352 0.18599 = 0.20405 -0.09302 0.10568 -0.05376 O11 5 0.488592 0.068178 0.226396 11.00000 0.12050 0.08472 = 0.09696 -0.00460 0.04452 -0.00797 O12 5 0.319447 0.014539 0.226777 11.00000 0.13497 0.15029 = 0.18248 -0.04696 -0.00318 -0.03265 O13 5 0.424891 0.015314 0.288046 11.00000 0.19984 0.29684 = 0.16526 0.13219 0.01335 -0.03301 S3 7 0.397131 0.048658 0.248545 11.00000 0.11018 0.11096 = 0.08819 -0.00671 0.02564 -0.01751 C48 1 0.711359 0.255664 -0.122626 11.00000 0.16900 0.12738 = 0.13151 0.04149 -0.06248 -0.05482 F10 3 0.629266 0.236944 -0.143469 11.00000 0.18114 0.15616 = 0.17260 0.05826 -0.10787 -0.03720 F11 3 0.688104 0.312429 -0.099375 11.00000 0.37069 0.07821 = 0.32836 0.02053 -0.20079 0.02032 F12 3 0.782142 0.279902 -0.147134 11.00000 0.25920 0.42565 = 0.21262 0.23612 -0.10449 -0.18324 O14 5 0.781021 0.122776 -0.120850 11.00000 0.09578 0.16277 = 0.16722 -0.06535 -0.00503 0.00897 O15 5 0.672121 0.162567 -0.067167 11.00000 0.10261 0.13291 = 0.08570 0.02624 -0.00063 -0.02291 O16 5 0.845850 0.210500 -0.070878 11.00000 0.11471 0.12214 = 0.10599 0.03307 -0.04601 -0.04545 S4 7 0.759865 0.179610 -0.092064 11.00000 0.08584 0.08617 = 0.07728 0.01185 -0.01349 -0.01022 SAME 0.01 0.01 C45 F1 F2 F3 O5 O6 O7 S1 C49 1 0.971027 0.626806 0.146865 11.00000 0.10277 0.35058 = 0.51254 0.23312 -0.01629 -0.02956 F13 3 0.959005 0.621195 0.108029 11.00000 0.48246 0.70211 = 0.40125 0.37995 0.10559 0.20885 F14 3 0.882731 0.648366 0.160412 11.00000 0.21471 0.33414 = 0.50986 0.14078 0.04574 0.03608 F15 3 1.031577 0.684522 0.152381 11.00000 0.27672 0.41220 = 1.23039 0.29218 -0.13895 -0.17003 O17 5 1.095398 0.519015 0.141449 11.00000 0.22727 0.70257 = 0.54821 -0.29817 0.00345 0.18457 O18 5 0.937527 0.496748 0.173178 11.00000 0.17978 0.27308 = 0.29979 0.11147 -0.01138 -0.07964 O19 5 1.059911 0.572732 0.205316 11.00000 0.37361 0.49930 = 0.24367 0.04659 -0.17578 0.04549 S5 7 1.017141 0.545349 0.168136 11.00000 0.10532 0.20893 = 0.23745 0.04104 -0.01125 0.01100 O1W 5 0.932755 0.300589 0.110374 11.00000 0.08346 0.08751 = 0.10877 -0.00478 0.00168 0.00906 O2W 5 0.701166 0.181868 0.013718 11.00000 0.07270 0.08509 = 0.08432 -0.00034 0.01839 0.00820 O3W 5 0.680358 -0.057865 0.104622 11.00000 0.08056 0.07344 = 0.07794 -0.00134 0.00973 0.00817 O4W 5 0.911001 0.057436 0.200632 11.00000 0.08063 0.10328 = 0.07450 -0.00756 -0.00156 0.00703 O5W 5 1.083003 -0.013057 0.236402 11.00000 0.16890 0.35908 = 0.18142 0.11521 -0.06167 0.01048 O6W 5 1.104667 0.380831 0.114282 11.00000 0.12622 0.20260 = 1.03847 -0.20273 0.05300 -0.04667 O7W 5 0.832799 -0.376299 -0.024768 11.00000 0.43229 0.45536 = 0.61077 -0.24575 -0.19520 0.12812 HKLF 4 REM 1H6_ReO4 in P 21/c REM R1 = 0.0595 for 8964 Fo > 4sig(Fo) and 0.0930 for all 13198 data REM 937 parameters refined using 34 restraints END ; _database_code_depnum_ccdc_archive 'CCDC 961776' #===END data_1H6_TcO4 _publ_contact_author ; Dr. Valeria Amendola Dipartimento di Chimica University of Pavia via Taramelli 12, I-27100 Pavia, ITALY ; _publ_contact_author_email ; valeria.amendola@unipv.it ; loop_ _publ_author_name _publ_author_address 'Amendola V.' 'Dipartimento di Chimica,University of Pavia, Italy' 'Bergamaschi G.' 'Dipartimento di Chimica, University of Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, Univerity of Pavia, Italy' 'Alberto R.' 'Institute of Inorganic Chemistry, University of Zurich' 'Braband H.' 'Institute of Inorganic Chemistry, University of Zurich' _publ_requested_journal 'Nature Chem.' _journal_name_full ; Nature Chemistry ; _publ_section_title ; A fluorescent sensor for 99Tc pertechnetate in water ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; (4,8,14,18,23,27-hexa-azonia-1,11-diaza-6(9,10)-anthracena-16,25(1,4)-dibenzena bicyclo[9.9.9]nonacosaphane pertechnetate clathrate) penta(triflate) heptahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C44 H64 N8, 5(C F3 O3 S), O4 Tc, 7 (H2 O)' _chemical_formula_sum 'C49 H78 F15 N8 O26 S5 Tc' _chemical_formula_weight 1738.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tc Tc 0.0057 3.0049 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _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 13.0099(2) _cell_length_b 17.5570(4) _cell_length_c 32.9333(4) _cell_angle_alpha 90.00 _cell_angle_beta 89.2260(10) _cell_angle_gamma 90.00 _cell_volume 7521.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 3.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.548 _exptl_absorpt_process_details ; CrysAlis-pro Software System (Agilent Tech., 2011) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Agilent SuperNova, Atlas-CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 46828 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 67.00 _reflns_number_total 12810 _reflns_number_gt 10772 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis-pro (Agilent, 2011)' _computing_cell_refinement 'CrysAlis-pro (Agilent, 2011)' _computing_data_reduction 'CrysAlis-pro (Agilent, 2011)' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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. Selected single crystals show a poor X-ray diffraction quality. The geometrical details of the cage and of the enclosed pertechnetate anion have an accuracy suitable to the aims of this work. However, the poor X-ray diffraction quality of the data imposes the use of soft restraints (ISOR and DELU instructions) on the least-square procedures involving the Uij values of several atoms belonging to triflate counterions. Also the molecular geometries of the triflate counterions have been restrained using the SAME instruction to be the same of the best characterized triflate in the crystal structure. Positions of H atoms belonging to water solvent molecules remain undetermined. The non standard monoclinic setting has been used to emphasize the isomorphism with the crystal structure containing (ReO4)- oxo-anion. ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12810 _refine_ls_number_parameters 937 _refine_ls_number_restraints 197 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.3800 _refine_ls_wR_factor_gt 0.3608 _refine_ls_goodness_of_fit_ref 1.717 _refine_ls_restrained_S_all 1.723 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 Tc1 Tc 0.71935(4) 0.14342(3) 0.123285(15) 0.0561(3) Uani 1 1 d . . . O1 O 0.6637(4) 0.2290(3) 0.11219(17) 0.0705(13) Uani 1 1 d . . . O2 O 0.8434(4) 0.1588(3) 0.13546(19) 0.0750(14) Uani 1 1 d . . . O3 O 0.7144(5) 0.0861(3) 0.08094(14) 0.0680(13) Uani 1 1 d . . . O4 O 0.6574(4) 0.0989(3) 0.16258(14) 0.0654(12) Uani 1 1 d . . . C1 C 0.6298(8) 0.3975(6) 0.0224(4) 0.108(4) Uani 1 1 d . . . H1A H 0.6373 0.4344 0.0006 0.130 Uiso 1 1 calc R . . H1B H 0.5985 0.4235 0.0454 0.130 Uiso 1 1 calc R . . C2 C 0.5592(8) 0.3362(6) 0.0089(3) 0.091(3) Uani 1 1 d . . . H2A H 0.5866 0.3138 -0.0159 0.110 Uiso 1 1 calc R . . H2B H 0.4930 0.3586 0.0027 0.110 Uiso 1 1 calc R . . C3 C 0.4538(7) 0.2222(6) 0.0306(3) 0.084(2) Uani 1 1 d . . . H3A H 0.3902 0.2508 0.0330 0.101 Uiso 1 1 calc R . . H3B H 0.4603 0.2044 0.0028 0.101 Uiso 1 1 calc R . . C4 C 0.4491(6) 0.1550(4) 0.0586(2) 0.0643(17) Uani 1 1 d . . . C5 C 0.4617(8) 0.0828(6) 0.0427(3) 0.084(3) Uani 1 1 d . . . H5 H 0.4747 0.0762 0.0151 0.101 Uiso 1 1 calc R . . C6 C 0.4547(8) 0.0203(5) 0.0682(3) 0.080(2) Uani 1 1 d . . . H6 H 0.4602 -0.0283 0.0572 0.096 Uiso 1 1 calc R . . C7 C 0.4400(6) 0.0282(5) 0.1090(2) 0.072(2) Uani 1 1 d . . . C8 C 0.4291(6) 0.1007(5) 0.1251(2) 0.0685(18) Uani 1 1 d . . . H8 H 0.4186 0.1069 0.1529 0.082 Uiso 1 1 calc R . . C9 C 0.4337(6) 0.1635(5) 0.1002(2) 0.0706(19) Uani 1 1 d . . . H9 H 0.4264 0.2119 0.1112 0.085 Uiso 1 1 calc R . . C10 C 0.4354(7) -0.0410(6) 0.1367(3) 0.087(3) Uani 1 1 d . . . H10A H 0.3704 -0.0408 0.1515 0.104 Uiso 1 1 calc R . . H10B H 0.4378 -0.0868 0.1202 0.104 Uiso 1 1 calc R . . C11 C 0.5270(8) -0.1180(5) 0.1893(3) 0.086(3) Uani 1 1 d . . . H11A H 0.4587 -0.1323 0.1986 0.103 Uiso 1 1 calc R . . H11B H 0.5517 -0.1574 0.1710 0.103 Uiso 1 1 calc R . . C12 C 0.5971(9) -0.1137(5) 0.2252(3) 0.091(3) Uani 1 1 d . . . H12A H 0.5682 -0.0781 0.2448 0.109 Uiso 1 1 calc R . . H12B H 0.5997 -0.1633 0.2381 0.109 Uiso 1 1 calc R . . C13 C 0.7845(8) 0.4346(5) 0.0546(4) 0.102(3) Uani 1 1 d . . . H13A H 0.7793 0.4800 0.0381 0.123 Uiso 1 1 calc R . . H13B H 0.8568 0.4223 0.0572 0.123 Uiso 1 1 calc R . . C14 C 0.7394(8) 0.4513(5) 0.0969(4) 0.096(3) Uani 1 1 d . . . H14A H 0.7780 0.4926 0.1090 0.115 Uiso 1 1 calc R . . H14B H 0.6690 0.4683 0.0941 0.115 Uiso 1 1 calc R . . C15 C 0.7184(9) 0.4027(5) 0.1682(3) 0.097(3) Uani 1 1 d . . . H15A H 0.6527 0.4286 0.1701 0.116 Uiso 1 1 calc R . . H15B H 0.7706 0.4371 0.1781 0.116 Uiso 1 1 calc R . . C16 C 0.7151(8) 0.3333(5) 0.1947(3) 0.084(3) Uani 1 1 d . . . C17 C 0.6213(7) 0.3009(5) 0.2046(3) 0.077(2) Uani 1 1 d . . . H17 H 0.5608 0.3220 0.1949 0.092 Uiso 1 1 calc R . . C18 C 0.6182(7) 0.2374(5) 0.2289(3) 0.076(2) Uani 1 1 d . . . H18 H 0.5551 0.2146 0.2345 0.091 Uiso 1 1 calc R . . C19 C 0.7092(7) 0.2053(5) 0.2458(3) 0.077(2) Uani 1 1 d . . . C20 C 0.8027(8) 0.2399(7) 0.2342(3) 0.096(3) Uani 1 1 d . . . H20 H 0.8642 0.2190 0.2431 0.115 Uiso 1 1 calc R . . C21 C 0.8049(8) 0.3045(7) 0.2099(4) 0.105(4) Uani 1 1 d . . . H21 H 0.8672 0.3283 0.2039 0.125 Uiso 1 1 calc R . . C22 C 0.7038(9) 0.1377(5) 0.2721(3) 0.085(3) Uani 1 1 d . . . H22A H 0.6371 0.1356 0.2856 0.101 Uiso 1 1 calc R . . H22B H 0.7559 0.1412 0.2928 0.101 Uiso 1 1 calc R . . C23 C 0.7144(8) -0.0009(6) 0.2746(2) 0.085(3) Uani 1 1 d . . . H23A H 0.6439 -0.0086 0.2837 0.102 Uiso 1 1 calc R . . H23B H 0.7563 0.0073 0.2983 0.102 Uiso 1 1 calc R . . C24 C 0.7531(9) -0.0731(6) 0.2512(3) 0.098(3) Uani 1 1 d . . . H24A H 0.8257 -0.0666 0.2450 0.118 Uiso 1 1 calc R . . H24B H 0.7465 -0.1167 0.2691 0.118 Uiso 1 1 calc R . . C25 C 0.7941(8) 0.3503(5) -0.0040(4) 0.094(3) Uani 1 1 d . . . H25A H 0.7536 0.3147 -0.0196 0.113 Uiso 1 1 calc R . . H25B H 0.8022 0.3960 -0.0202 0.113 Uiso 1 1 calc R . . C26 C 0.8985(7) 0.3162(5) 0.0014(3) 0.085(3) Uani 1 1 d . . . H26A H 0.9420 0.3523 0.0154 0.102 Uiso 1 1 calc R . . H26B H 0.9293 0.3061 -0.0250 0.102 Uiso 1 1 calc R . . C27 C 0.9819(6) 0.1894(5) 0.0149(3) 0.074(2) Uani 1 1 d . . . H27A H 1.0466 0.2160 0.0185 0.089 Uiso 1 1 calc R . . H27B H 0.9775 0.1745 -0.0134 0.089 Uiso 1 1 calc R . . C28 C 0.9793(5) 0.1183(4) 0.0417(2) 0.0628(17) Uani 1 1 d . . . C29 C 0.9217(5) 0.0569(4) 0.03024(19) 0.0580(16) Uani 1 1 d . . . C30 C 0.8656(5) 0.0550(5) -0.00694(19) 0.0639(19) Uani 1 1 d . . . H30 H 0.8694 0.0968 -0.0242 0.077 Uiso 1 1 calc R . . C31 C 0.8081(6) -0.0048(5) -0.0178(2) 0.070(2) Uani 1 1 d . . . H31 H 0.7729 -0.0037 -0.0421 0.084 Uiso 1 1 calc R . . C32 C 0.8006(6) -0.0692(6) 0.0074(2) 0.074(2) Uani 1 1 d . . . H32 H 0.7601 -0.1106 0.0002 0.089 Uiso 1 1 calc R . . C33 C 0.8547(6) -0.0691(5) 0.0428(2) 0.0646(18) Uani 1 1 d . . . H33 H 0.8507 -0.1121 0.0592 0.077 Uiso 1 1 calc R . . C34 C 0.9155(5) -0.0083(4) 0.05590(19) 0.0584(16) Uani 1 1 d . . . C35 C 0.9712(5) -0.0098(5) 0.0921(2) 0.0637(18) Uani 1 1 d . . . C36 C 1.0336(5) 0.0499(5) 0.1025(2) 0.0637(18) Uani 1 1 d . . . C37 C 1.0964(7) 0.0498(6) 0.1383(3) 0.082(2) Uani 1 1 d . . . H37 H 1.0936 0.0075 0.1552 0.099 Uiso 1 1 calc R . . C38 C 1.1594(8) 0.1081(7) 0.1484(4) 0.095(3) Uani 1 1 d . . . H38 H 1.1994 0.1045 0.1715 0.114 Uiso 1 1 calc R . . C39 C 1.1645(7) 0.1730(7) 0.1244(4) 0.098(3) Uani 1 1 d . . . H39 H 1.2062 0.2136 0.1318 0.117 Uiso 1 1 calc R . . C40 C 1.1064(6) 0.1768(5) 0.0892(3) 0.079(2) Uani 1 1 d . . . H40 H 1.1113 0.2202 0.0731 0.095 Uiso 1 1 calc R . . C41 C 1.0396(6) 0.1169(5) 0.0769(2) 0.0683(19) Uani 1 1 d . . . C42 C 0.9609(7) -0.0794(5) 0.1197(2) 0.072(2) Uani 1 1 d . . . H42A H 1.0220 -0.0840 0.1360 0.086 Uiso 1 1 calc R . . H42B H 0.9555 -0.1249 0.1031 0.086 Uiso 1 1 calc R . . C43 C 0.8608(9) -0.1379(5) 0.1775(3) 0.083(3) Uani 1 1 d . . . H43A H 0.8868 -0.1837 0.1645 0.100 Uiso 1 1 calc R . . H43B H 0.9048 -0.1264 0.2002 0.100 Uiso 1 1 calc R . . C44 C 0.7556(11) -0.1520(5) 0.1927(3) 0.099(4) Uani 1 1 d . . . H44A H 0.7579 -0.1959 0.2106 0.119 Uiso 1 1 calc R . . H44B H 0.7138 -0.1661 0.1697 0.119 Uiso 1 1 calc R . . N1 N 0.7323(6) 0.3712(4) 0.0339(3) 0.085(2) Uani 1 1 d . . . N2 N 0.5436(5) 0.2742(4) 0.04006(19) 0.0679(15) Uani 1 1 d . . . H2C H 0.5328 0.2957 0.0646 0.081 Uiso 1 1 calc R . . H2D H 0.6013 0.2461 0.0414 0.081 Uiso 1 1 calc R . . N3 N 0.5208(5) -0.0433(4) 0.16631(19) 0.0686(16) Uani 1 1 d . . . H3C H 0.5123 -0.0051 0.1843 0.082 Uiso 1 1 calc R . . H3D H 0.5807 -0.0354 0.1529 0.082 Uiso 1 1 calc R . . N4 N 0.7411(6) 0.3848(4) 0.1247(2) 0.082(2) Uani 1 1 d . . . H4A H 0.8036 0.3629 0.1229 0.099 Uiso 1 1 calc R . . H4B H 0.6949 0.3504 0.1161 0.099 Uiso 1 1 calc R . . N5 N 0.7201(7) 0.0671(4) 0.2479(2) 0.081(2) Uani 1 1 d . . . H5A H 0.7820 0.0689 0.2354 0.098 Uiso 1 1 calc R . . H5B H 0.6717 0.0638 0.2287 0.098 Uiso 1 1 calc R . . N6 N 0.8931(5) 0.2425(4) 0.0256(2) 0.0703(16) Uani 1 1 d . . . H6A H 0.8333 0.2189 0.0206 0.084 Uiso 1 1 calc R . . H6B H 0.8946 0.2534 0.0523 0.084 Uiso 1 1 calc R . . N7 N 0.8660(6) -0.0731(4) 0.14756(18) 0.0723(17) Uani 1 1 d . . . H7A H 0.8090 -0.0732 0.1324 0.087 Uiso 1 1 calc R . . H7B H 0.8682 -0.0287 0.1612 0.087 Uiso 1 1 calc R . . N8 N 0.7018(6) -0.0897(4) 0.2148(2) 0.079(2) Uani 1 1 d . . . C46 C 0.6217(6) -0.3155(4) 0.1007(3) 0.131(6) Uani 1 1 d D . . F4 F 0.6742(7) -0.3760(4) 0.1095(3) 0.181(5) Uani 1 1 d D . . F5 F 0.5406(7) -0.3366(5) 0.0804(3) 0.186(5) Uani 1 1 d D . . F6 F 0.5887(6) -0.2855(4) 0.1345(2) 0.150(3) Uani 1 1 d D . . S2 S 0.6959(3) -0.24699(14) 0.07133(9) 0.1120(10) Uani 1 1 d D . . O8 O 0.6236(5) -0.1872(3) 0.0653(2) 0.109(2) Uani 1 1 d D . . O9 O 0.7790(5) -0.2273(4) 0.0969(2) 0.103(2) Uani 1 1 d D . . O10 O 0.7234(8) -0.2876(6) 0.0347(2) 0.180(6) Uani 1 1 d D . . C45 C 0.3913(6) 0.4861(4) 0.1059(2) 0.107(4) Uani 1 1 d D . . F1 F 0.4246(8) 0.5000(5) 0.0695(2) 0.207(6) Uani 1 1 d D . . F2 F 0.4463(8) 0.5280(4) 0.1305(3) 0.165(4) Uani 1 1 d D . . F3 F 0.2976(5) 0.5111(4) 0.1090(3) 0.179(5) Uani 1 1 d D . . S1 S 0.4017(2) 0.38695(12) 0.11954(9) 0.0951(8) Uani 1 1 d D . . O5 O 0.5071(4) 0.3690(3) 0.11023(19) 0.0871(18) Uani 1 1 d D . . O6 O 0.3309(7) 0.3485(5) 0.0942(4) 0.225(9) Uani 1 1 d D . . O7 O 0.3780(9) 0.3853(6) 0.1622(2) 0.208(8) Uani 1 1 d D . . C47 C 0.3407(6) 0.1365(4) 0.2601(3) 0.174(10) Uani 1 1 d D . . F7 F 0.3182(10) 0.1683(6) 0.2258(3) 0.216(7) Uani 1 1 d D . . F8 F 0.2562(7) 0.1263(6) 0.2813(5) 0.339(14) Uani 1 1 d D . . F9 F 0.3974(6) 0.1836(4) 0.2805(2) 0.152(4) Uani 1 1 d D . . S3 S 0.4046(3) 0.04649(17) 0.25210(8) 0.1175(12) Uani 1 1 d D . . O11 O 0.4935(4) 0.0668(3) 0.22877(16) 0.0818(17) Uani 1 1 d D . . O12 O 0.3339(7) -0.0008(6) 0.2329(3) 0.206(7) Uani 1 1 d D . . O13 O 0.4310(8) 0.0233(6) 0.2937(2) 0.231(9) Uani 1 1 d D . . C48 C 0.7223(6) 0.2559(5) -0.1253(2) 0.175(10) Uani 1 1 d D . . F10 F 0.6413(5) 0.2391(4) -0.1464(2) 0.133(3) Uani 1 1 d D . . F11 F 0.6993(9) 0.3151(4) -0.1029(3) 0.228(8) Uani 1 1 d D . . F12 F 0.7943(6) 0.2762(7) -0.1504(3) 0.228(8) Uani 1 1 d D . . S4 S 0.76170(16) 0.17710(13) -0.09376(6) 0.0780(6) Uani 1 1 d D . . O14 O 0.7847(5) 0.1190(4) -0.1227(2) 0.120(3) Uani 1 1 d D . . O15 O 0.6735(4) 0.1619(3) -0.06877(17) 0.0828(16) Uani 1 1 d D . . O16 O 0.8494(5) 0.2061(4) -0.07221(17) 0.097(2) Uani 1 1 d D . . C49 C 0.9494(8) 0.6287(5) 0.1342(4) 0.167(8) Uani 1 1 d D . . F13 F 0.9082(9) 0.6070(7) 0.1003(3) 0.204(5) Uani 1 1 d D . . F14 F 0.8746(9) 0.6550(7) 0.1573(4) 0.255(9) Uani 1 1 d D . . F15 F 1.0102(8) 0.6843(5) 0.1263(5) 0.272(9) Uani 1 1 d D . . S5 S 1.0121(3) 0.5504(3) 0.1598(2) 0.203(3) Uani 1 1 d DU . . O17 O 1.0854(9) 0.5251(7) 0.1304(5) 0.294(13) Uani 1 1 d DU . . O18 O 0.9334(7) 0.4996(6) 0.1702(5) 0.225(8) Uani 1 1 d D . . O19 O 1.0608(15) 0.5881(10) 0.1943(4) 0.48(2) Uani 1 1 d DU . . O1W O 0.9228(4) 0.2985(3) 0.1074(2) 0.0812(15) Uani 1 1 d . . . O2W O 0.6961(4) 0.1770(3) 0.01347(17) 0.0737(14) Uani 1 1 d . . . O3W O 0.6752(4) -0.0602(3) 0.10777(15) 0.0669(13) Uani 1 1 d . . . O4W O 0.8990(6) 0.0571(4) 0.19874(19) 0.0907(18) Uani 1 1 d . . . O5W O 1.062(3) -0.027(2) 0.2410(7) 0.44(3) Uani 1 1 d . . . O6W O 1.1080(12) 0.3630(7) 0.1289(9) 0.264(13) Uani 1 1 d . . . O7W O 1.0524(14) 0.4788(11) 0.0311(6) 0.244(9) 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 Tc1 0.0652(4) 0.0413(4) 0.0609(4) -0.00630(17) 0.0236(3) 0.00034(18) O1 0.076(3) 0.039(3) 0.096(4) -0.011(2) 0.014(3) 0.006(2) O2 0.065(3) 0.058(3) 0.100(4) 0.006(3) 0.023(3) 0.002(2) O3 0.101(4) 0.046(3) 0.056(2) -0.0094(18) 0.031(2) 0.003(2) O4 0.075(3) 0.063(3) 0.058(2) -0.011(2) 0.015(2) -0.006(2) C1 0.089(7) 0.081(7) 0.154(10) 0.057(7) 0.019(6) 0.027(5) C2 0.081(6) 0.090(6) 0.103(7) 0.034(5) 0.020(5) 0.018(5) C3 0.073(5) 0.088(6) 0.092(6) -0.005(4) -0.003(4) 0.008(4) C4 0.060(4) 0.063(4) 0.069(4) -0.011(3) -0.002(3) -0.005(3) C5 0.096(6) 0.085(6) 0.071(5) -0.032(4) 0.009(4) -0.021(5) C6 0.101(6) 0.066(5) 0.074(5) -0.021(4) 0.013(4) -0.025(4) C7 0.063(4) 0.081(5) 0.070(4) -0.027(4) 0.017(3) -0.027(4) C8 0.069(4) 0.068(5) 0.068(4) -0.013(3) 0.012(3) 0.000(3) C9 0.072(4) 0.057(4) 0.082(5) -0.021(4) 0.013(4) 0.004(3) C10 0.090(6) 0.081(6) 0.088(5) -0.015(4) 0.034(5) -0.035(5) C11 0.110(7) 0.057(5) 0.090(6) 0.005(4) 0.040(5) -0.016(4) C12 0.132(8) 0.062(5) 0.078(5) 0.020(4) 0.051(6) 0.004(5) C13 0.090(6) 0.046(5) 0.169(10) 0.014(5) 0.038(6) -0.003(4) C14 0.089(6) 0.035(4) 0.162(10) -0.003(4) 0.035(6) -0.001(4) C15 0.114(7) 0.049(5) 0.127(8) -0.029(5) 0.037(6) -0.012(4) C16 0.092(6) 0.063(5) 0.097(6) -0.038(4) 0.020(5) -0.006(4) C17 0.084(5) 0.063(5) 0.082(5) -0.029(4) 0.015(4) 0.003(4) C18 0.079(5) 0.068(5) 0.081(5) -0.017(4) 0.020(4) 0.001(4) C19 0.090(6) 0.072(5) 0.069(4) -0.033(4) 0.000(4) 0.006(4) C20 0.085(6) 0.091(7) 0.112(7) -0.040(6) -0.010(5) 0.003(5) C21 0.075(6) 0.097(8) 0.142(9) -0.049(7) 0.016(6) -0.018(5) C22 0.104(7) 0.092(7) 0.058(4) -0.023(4) 0.000(4) 0.027(5) C23 0.107(7) 0.099(6) 0.048(4) 0.012(4) 0.019(4) 0.023(5) C24 0.123(8) 0.112(8) 0.060(5) 0.026(4) 0.029(5) 0.044(6) C25 0.079(6) 0.070(6) 0.133(8) 0.039(5) 0.028(6) 0.005(4) C26 0.077(5) 0.075(6) 0.103(6) 0.030(4) 0.022(5) 0.000(4) C27 0.057(4) 0.080(5) 0.083(5) 0.017(4) 0.020(3) 0.009(3) C28 0.060(4) 0.067(5) 0.061(4) 0.007(3) 0.018(3) 0.020(3) C29 0.050(3) 0.073(5) 0.051(3) 0.008(3) 0.020(3) 0.022(3) C30 0.050(3) 0.095(5) 0.046(3) 0.011(3) 0.015(3) 0.025(3) C31 0.056(4) 0.102(6) 0.052(4) 0.003(3) 0.012(3) 0.019(4) C32 0.061(4) 0.101(6) 0.059(4) -0.006(4) 0.020(3) 0.007(4) C33 0.065(4) 0.074(5) 0.055(3) 0.010(3) 0.023(3) 0.024(3) C34 0.056(3) 0.069(4) 0.050(3) 0.008(3) 0.021(3) 0.020(3) C35 0.058(4) 0.080(5) 0.053(3) 0.007(3) 0.018(3) 0.027(3) C36 0.055(3) 0.077(5) 0.059(4) 0.005(3) 0.016(3) 0.023(3) C37 0.073(5) 0.102(7) 0.071(5) 0.003(4) 0.005(4) 0.025(5) C38 0.074(6) 0.101(8) 0.111(7) -0.005(6) -0.013(5) 0.009(5) C39 0.061(5) 0.110(8) 0.122(8) -0.012(6) -0.003(5) 0.017(5) C40 0.064(4) 0.076(6) 0.098(6) 0.003(4) 0.004(4) 0.013(4) C41 0.055(4) 0.082(5) 0.068(4) 0.003(3) 0.016(3) 0.024(3) C42 0.076(5) 0.080(5) 0.058(4) 0.007(3) 0.015(3) 0.017(4) C43 0.123(8) 0.060(5) 0.066(5) 0.011(3) 0.026(5) 0.010(4) C44 0.153(10) 0.066(6) 0.077(5) 0.022(4) 0.041(6) 0.020(5) N1 0.077(4) 0.061(4) 0.115(6) 0.027(4) 0.032(4) 0.022(3) N2 0.062(3) 0.070(4) 0.072(4) 0.012(3) 0.011(3) 0.013(3) N3 0.072(4) 0.058(4) 0.075(4) -0.006(3) 0.024(3) -0.012(3) N4 0.075(4) 0.041(4) 0.130(6) -0.017(3) 0.021(4) -0.011(3) N5 0.109(6) 0.074(5) 0.060(3) -0.013(3) 0.014(3) 0.019(4) N6 0.067(4) 0.058(4) 0.085(4) 0.014(3) 0.023(3) 0.004(3) N7 0.095(5) 0.063(4) 0.059(3) 0.001(3) 0.024(3) 0.011(3) N8 0.108(5) 0.062(4) 0.066(4) 0.010(3) 0.036(4) 0.006(3) C46 0.165(12) 0.046(7) 0.186(14) -0.001(6) -0.087(11) -0.007(6) F4 0.245(11) 0.053(4) 0.248(11) 0.024(5) -0.084(9) 0.008(5) F5 0.212(11) 0.100(6) 0.249(12) 0.044(7) -0.105(10) -0.041(6) F6 0.173(8) 0.100(6) 0.178(8) 0.017(5) -0.026(7) -0.008(5) S2 0.161(3) 0.0551(15) 0.121(2) -0.0072(12) -0.0416(19) 0.0203(14) O8 0.139(6) 0.062(4) 0.127(6) 0.003(3) -0.051(5) -0.001(4) O9 0.116(5) 0.069(4) 0.125(5) -0.002(3) -0.038(4) 0.015(4) O10 0.233(14) 0.160(10) 0.149(9) -0.067(8) -0.053(9) 0.075(10) C45 0.131(9) 0.080(7) 0.109(8) 0.015(5) 0.043(7) 0.035(6) F1 0.258(13) 0.224(11) 0.137(7) 0.088(7) 0.068(8) 0.140(10) F2 0.229(12) 0.079(5) 0.187(9) 0.005(5) 0.002(8) -0.011(6) F3 0.117(6) 0.093(5) 0.326(13) 0.041(6) 0.078(7) 0.056(4) S1 0.0883(15) 0.0554(13) 0.140(2) -0.0015(11) 0.0435(14) 0.0115(10) O5 0.086(4) 0.076(4) 0.099(4) 0.009(3) 0.023(3) 0.026(3) O6 0.119(8) 0.098(8) 0.46(3) -0.106(11) -0.034(12) 0.016(6) O7 0.277(16) 0.129(8) 0.211(12) 0.060(8) 0.182(12) 0.076(9) C47 0.112(10) 0.101(10) 0.31(3) -0.096(14) 0.111(14) -0.014(8) F7 0.227(13) 0.252(14) 0.170(9) -0.029(9) -0.077(9) 0.116(11) F8 0.204(12) 0.213(12) 0.59(3) -0.180(17) 0.277(18) -0.068(10) F9 0.191(8) 0.087(5) 0.175(7) -0.051(5) 0.091(6) -0.020(5) S3 0.140(2) 0.111(2) 0.0998(18) -0.0267(15) 0.0674(18) -0.0429(18) O11 0.108(4) 0.062(3) 0.074(3) -0.002(2) 0.043(3) -0.001(3) O12 0.193(12) 0.177(11) 0.244(15) -0.091(11) 0.101(11) -0.100(10) O13 0.252(15) 0.205(13) 0.232(14) 0.160(12) 0.130(12) 0.081(11) C48 0.153(13) 0.166(16) 0.207(17) 0.151(15) -0.099(13) -0.084(12) F10 0.122(5) 0.139(6) 0.140(5) 0.062(5) -0.063(5) -0.033(4) F11 0.296(15) 0.058(5) 0.335(16) 0.051(7) -0.194(14) -0.020(6) F12 0.180(9) 0.333(16) 0.172(8) 0.183(10) -0.073(7) -0.136(10) S4 0.0727(11) 0.0828(14) 0.0786(12) 0.0273(10) -0.0063(9) -0.0105(9) O14 0.092(5) 0.146(8) 0.123(7) -0.012(5) 0.004(5) 0.014(5) O15 0.080(4) 0.080(4) 0.088(4) 0.026(3) 0.003(3) -0.013(3) O16 0.096(4) 0.107(5) 0.089(4) 0.043(3) -0.025(3) -0.036(4) C49 0.137(15) 0.158(17) 0.21(2) 0.040(15) -0.008(15) -0.033(13) F13 0.181(11) 0.190(12) 0.241(14) 0.030(10) -0.041(10) -0.029(9) F14 0.159(11) 0.198(13) 0.41(3) 0.080(14) 0.042(14) 0.076(10) F15 0.150(10) 0.174(12) 0.49(3) 0.100(15) -0.052(13) -0.045(9) S5 0.100(3) 0.168(4) 0.340(8) 0.116(5) 0.053(4) 0.051(3) O17 0.167(14) 0.139(12) 0.57(4) -0.068(17) 0.119(19) -0.022(10) O18 0.121(8) 0.195(13) 0.36(2) 0.142(14) -0.005(11) -0.022(8) O19 0.39(3) 0.58(5) 0.48(4) 0.12(3) -0.28(3) -0.04(3) O1W 0.068(3) 0.055(3) 0.120(5) -0.003(3) 0.011(3) 0.003(2) O2W 0.070(3) 0.065(3) 0.085(3) 0.015(2) 0.027(3) 0.009(2) O3W 0.089(3) 0.048(3) 0.063(3) -0.0012(19) 0.024(2) 0.010(2) O4W 0.102(5) 0.089(4) 0.081(4) -0.010(3) 0.021(3) 0.004(3) O5W 0.54(5) 0.53(5) 0.26(2) -0.12(3) -0.25(3) 0.31(4) O6W 0.126(10) 0.104(10) 0.56(4) 0.002(13) -0.014(17) -0.015(7) O7W 0.192(15) 0.224(17) 0.32(2) 0.083(16) 0.016(14) -0.050(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Tc1 O2 1.689(6) . ? Tc1 O4 1.705(5) . ? Tc1 O1 1.710(5) . ? Tc1 O3 1.722(4) . ? C1 N1 1.466(13) . ? C1 C2 1.487(18) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.509(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.498(13) . ? C3 N2 1.518(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.381(11) . ? C4 C9 1.390(11) . ? C5 C6 1.383(14) . ? C5 H5 0.9300 . ? C6 C7 1.362(11) . ? C6 H6 0.9300 . ? C7 C8 1.386(11) . ? C7 C10 1.520(13) . ? C8 C9 1.375(12) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N3 1.488(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.506(16) . ? C11 N3 1.517(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N8 1.463(13) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.474(14) . ? C13 C14 1.530(15) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.484(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.492(12) . ? C15 C16 1.499(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.375(16) . ? C16 C17 1.381(13) . ? C17 C18 1.373(13) . ? C17 H17 0.9300 . ? C18 C19 1.431(13) . ? C18 H18 0.9300 . ? C19 C20 1.408(15) . ? C19 C22 1.471(14) . ? C20 C21 1.390(18) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 N5 1.488(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N5 1.483(11) . ? C23 C24 1.563(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N8 1.411(14) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.497(13) . ? C25 N1 1.521(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N6 1.519(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N6 1.523(9) . ? C27 C28 1.531(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.369(11) . ? C28 C41 1.407(11) . ? C29 C34 1.425(9) . ? C29 C30 1.434(10) . ? C30 C31 1.340(12) . ? C30 H30 0.9300 . ? C31 C32 1.403(12) . ? C31 H31 0.9300 . ? C32 C33 1.371(12) . ? C32 H32 0.9300 . ? C33 C34 1.399(12) . ? C33 H33 0.9300 . ? C34 C35 1.403(10) . ? C35 C36 1.373(12) . ? C35 C42 1.526(10) . ? C36 C37 1.441(12) . ? C36 C41 1.450(11) . ? C37 C38 1.356(15) . ? C37 H37 0.9300 . ? C38 C39 1.388(17) . ? C38 H38 0.9300 . ? C39 C40 1.394(14) . ? C39 H39 0.9300 . ? C40 C41 1.427(13) . ? C40 H40 0.9300 . ? C42 N7 1.533(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.473(16) . ? C43 N7 1.505(9) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N8 1.484(11) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 H5B 0.9000 . ? N5 H5A 0.9000 . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 H7B 0.9000 . ? N7 H7A 0.9000 . ? C46 F4 1.297(8) . ? C46 F6 1.298(8) . ? C46 F5 1.311(8) . ? C46 S2 1.814(7) . ? S2 O9 1.421(6) . ? S2 O8 1.425(5) . ? S2 O10 1.442(6) . ? C45 F1 1.293(8) . ? C45 F3 1.300(8) . ? C45 F2 1.315(9) . ? C45 S1 1.803(7) . ? S1 O6 1.421(7) . ? S1 O7 1.435(7) . ? S1 O5 1.436(5) . ? C47 F7 1.297(9) . ? C47 F9 1.302(8) . ? C47 F8 1.308(8) . ? C47 S3 1.803(7) . ? S3 O12 1.397(7) . ? S3 O11 1.426(5) . ? S3 O13 1.474(7) . ? C48 F12 1.293(8) . ? C48 F10 1.305(8) . ? C48 F11 1.306(9) . ? C48 S4 1.808(6) . ? S4 O14 1.425(6) . ? S4 O15 1.428(5) . ? S4 O16 1.444(5) . ? C49 F15 1.281(9) . ? C49 F13 1.302(9) . ? C49 F14 1.312(9) . ? C49 S5 1.812(8) . ? S5 O18 1.397(7) . ? S5 O17 1.421(7) . ? S5 O19 1.467(8) . ? 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 O2 Tc1 O4 109.7(3) . . ? O2 Tc1 O1 108.6(3) . . ? O4 Tc1 O1 111.6(3) . . ? O2 Tc1 O3 109.4(3) . . ? O4 Tc1 O3 108.9(2) . . ? O1 Tc1 O3 108.7(3) . . ? N1 C1 C2 114.7(9) . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C1 C2 N2 113.4(9) . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? N2 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C4 C3 N2 111.8(7) . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? N2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C9 119.1(8) . . ? C5 C4 C3 119.1(8) . . ? C9 C4 C3 121.8(7) . . ? C4 C5 C6 119.4(8) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 121.7(8) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 118.9(8) . . ? C6 C7 C10 121.0(8) . . ? C8 C7 C10 120.1(7) . . ? C9 C8 C7 120.3(7) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C4 120.5(7) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? N3 C10 C7 113.0(6) . . ? N3 C10 H10A 109.0 . . ? C7 C10 H10A 109.0 . . ? N3 C10 H10B 109.0 . . ? C7 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 N3 112.7(7) . . ? C12 C11 H11A 109.1 . . ? N3 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? N3 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N8 C12 C11 113.7(6) . . ? N8 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? N1 C13 C14 113.1(7) . . ? N1 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N1 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N4 C14 C13 113.6(7) . . ? N4 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? N4 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N4 C15 C16 113.0(7) . . ? N4 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N4 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 121.0(11) . . ? C21 C16 C15 119.5(10) . . ? C17 C16 C15 119.4(10) . . ? C18 C17 C16 119.4(10) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 122.0(9) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C20 C19 C18 116.1(10) . . ? C20 C19 C22 122.8(10) . . ? C18 C19 C22 121.0(9) . . ? C21 C20 C19 121.3(10) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C16 C21 C20 119.9(10) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C19 C22 N5 110.6(7) . . ? C19 C22 H22A 109.5 . . ? N5 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? N5 C23 C24 110.3(6) . . ? N5 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N5 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N8 C24 C23 115.7(8) . . ? N8 C24 H24A 108.4 . . ? C23 C24 H24A 108.4 . . ? N8 C24 H24B 108.3 . . ? C23 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C26 C25 N1 118.0(9) . . ? C26 C25 H25A 107.8 . . ? N1 C25 H25A 107.8 . . ? C26 C25 H25B 107.8 . . ? N1 C25 H25B 107.8 . . ? H25A C25 H25B 107.1 . . ? C25 C26 N6 111.6(7) . . ? C25 C26 H26A 109.3 . . ? N6 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? N6 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? N6 C27 C28 110.7(5) . . ? N6 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N6 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C41 121.8(7) . . ? C29 C28 C27 119.3(7) . . ? C41 C28 C27 118.8(8) . . ? C28 C29 C34 119.7(7) . . ? C28 C29 C30 122.8(7) . . ? C34 C29 C30 117.5(7) . . ? C31 C30 C29 122.5(7) . . ? C31 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C30 C31 C32 120.6(7) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 118.0(8) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C32 C33 C34 124.2(7) . . ? C32 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C33 C34 C35 123.2(7) . . ? C33 C34 C29 117.2(6) . . ? C35 C34 C29 119.6(7) . . ? C36 C35 C34 120.8(7) . . ? C36 C35 C42 120.6(7) . . ? C34 C35 C42 118.6(8) . . ? C35 C36 C37 123.2(7) . . ? C35 C36 C41 120.1(7) . . ? C37 C36 C41 116.8(8) . . ? C38 C37 C36 123.5(9) . . ? C38 C37 H37 118.3 . . ? C36 C37 H37 118.3 . . ? C37 C38 C39 120.2(10) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 119.4(11) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C39 C40 C41 122.7(9) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C28 C41 C40 124.7(8) . . ? C28 C41 C36 117.9(8) . . ? C40 C41 C36 117.4(7) . . ? C35 C42 N7 111.2(6) . . ? C35 C42 H42A 109.4 . . ? N7 C42 H42A 109.4 . . ? C35 C42 H42B 109.4 . . ? N7 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C44 C43 N7 112.6(8) . . ? C44 C43 H43A 109.1 . . ? N7 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? N7 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C43 C44 N8 118.2(9) . . ? C43 C44 H44A 107.8 . . ? N8 C44 H44A 107.8 . . ? C43 C44 H44B 107.8 . . ? N8 C44 H44B 107.8 . . ? H44A C44 H44B 107.1 . . ? C1 N1 C13 108.0(8) . . ? C1 N1 C25 109.6(9) . . ? C13 N1 C25 108.7(8) . . ? C2 N2 C3 113.0(7) . . ? C2 N2 H2C 109.0 . . ? C3 N2 H2C 109.0 . . ? C2 N2 H2D 109.0 . . ? C3 N2 H2D 109.0 . . ? H2C N2 H2D 107.8 . . ? C10 N3 C11 113.3(7) . . ? C10 N3 H3C 108.9 . . ? C11 N3 H3C 108.9 . . ? C10 N3 H3D 108.9 . . ? C11 N3 H3D 108.9 . . ? H3C N3 H3D 107.7 . . ? C14 N4 C15 115.0(7) . . ? C14 N4 H4A 108.5 . . ? C15 N4 H4A 108.5 . . ? C14 N4 H4B 108.5 . . ? C15 N4 H4B 108.5 . . ? H4A N4 H4B 107.5 . . ? C23 N5 C22 110.3(7) . . ? C23 N5 H5B 109.6 . . ? C22 N5 H5B 109.6 . . ? C23 N5 H5A 109.6 . . ? C22 N5 H5A 109.6 . . ? H5B N5 H5A 108.1 . . ? C26 N6 C27 111.7(6) . . ? C26 N6 H6A 109.3 . . ? C27 N6 H6A 109.3 . . ? C26 N6 H6B 109.3 . . ? C27 N6 H6B 109.3 . . ? H6A N6 H6B 107.9 . . ? C43 N7 C42 111.5(6) . . ? C43 N7 H7B 109.3 . . ? C42 N7 H7B 109.3 . . ? C43 N7 H7A 109.3 . . ? C42 N7 H7A 109.3 . . ? H7B N7 H7A 108.0 . . ? C24 N8 C12 108.0(7) . . ? C24 N8 C44 110.2(8) . . ? C12 N8 C44 109.6(8) . . ? F4 C46 F6 108.1(7) . . ? F4 C46 F5 108.1(7) . . ? F6 C46 F5 107.0(8) . . ? F4 C46 S2 112.6(6) . . ? F6 C46 S2 110.9(5) . . ? F5 C46 S2 110.0(6) . . ? O9 S2 O8 114.3(4) . . ? O9 S2 O10 115.6(5) . . ? O8 S2 O10 113.9(5) . . ? O9 S2 C46 104.4(4) . . ? O8 S2 C46 102.5(4) . . ? O10 S2 C46 104.1(5) . . ? F1 C45 F3 108.1(7) . . ? F1 C45 F2 106.8(7) . . ? F3 C45 F2 106.2(7) . . ? F1 C45 S1 112.9(6) . . ? F3 C45 S1 112.4(6) . . ? F2 C45 S1 110.1(6) . . ? O6 S1 O7 115.7(6) . . ? O6 S1 O5 113.3(5) . . ? O7 S1 O5 113.3(5) . . ? O6 S1 C45 105.1(5) . . ? O7 S1 C45 104.4(4) . . ? O5 S1 C45 103.4(3) . . ? F7 C47 F9 108.2(8) . . ? F7 C47 F8 109.1(8) . . ? F9 C47 F8 106.7(7) . . ? F7 C47 S3 111.1(6) . . ? F9 C47 S3 111.7(6) . . ? F8 C47 S3 109.9(6) . . ? O12 S3 O11 116.1(4) . . ? O12 S3 O13 114.8(5) . . ? O11 S3 O13 111.8(5) . . ? O12 S3 C47 106.4(5) . . ? O11 S3 C47 103.2(3) . . ? O13 S3 C47 102.7(5) . . ? F12 C48 F10 107.6(7) . . ? F12 C48 F11 107.5(7) . . ? F10 C48 F11 107.6(7) . . ? F12 C48 S4 111.7(6) . . ? F10 C48 S4 111.8(5) . . ? F11 C48 S4 110.5(6) . . ? O14 S4 O15 114.3(4) . . ? O14 S4 O16 114.9(4) . . ? O15 S4 O16 114.6(4) . . ? O14 S4 C48 102.9(4) . . ? O15 S4 C48 104.0(3) . . ? O16 S4 C48 104.1(3) . . ? F15 C49 F13 108.1(8) . . ? F15 C49 F14 107.4(9) . . ? F13 C49 F14 106.9(8) . . ? F15 C49 S5 113.1(7) . . ? F13 C49 S5 111.8(7) . . ? F14 C49 S5 109.3(7) . . ? O18 S5 O17 116.8(6) . . ? O18 S5 O19 114.8(7) . . ? O17 S5 O19 112.0(6) . . ? O18 S5 C49 105.4(5) . . ? O17 S5 C49 102.8(5) . . ? O19 S5 C49 102.8(6) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.595 _refine_diff_density_min -1.351 _refine_diff_density_rms 0.149 _iucr_refine_instructions_details ; TITL 1H6_TcO4 in P 21/c CELL 1.54184 13.0099 17.5570 32.9333 90.000 89.226 90.000 ZERR 4 0.0002 0.0004 0.0004 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H F N O S TC UNIT 196 312 60 32 104 20 4 MERG 2 OMIT -2 134 FMAP 2 PLAN 25 ACTA BOND $H delu 0.01 0.01 s5 o17 ISOR 0.05 0.05 O19 LIST 4 L.S. 6 WGHT 0.200000 FVAR 1.91183 TC1 7 0.719348 0.143424 0.123285 11.00000 0.06522 0.04135 = 0.06094 -0.00630 0.02364 0.00034 O1 5 0.663670 0.229024 0.112192 11.00000 0.07637 0.03888 = 0.09592 -0.01147 0.01430 0.00639 O2 5 0.843365 0.158771 0.135462 11.00000 0.06547 0.05842 = 0.10040 0.00605 0.02293 0.00225 O3 5 0.714398 0.086069 0.080945 11.00000 0.10072 0.04649 = 0.05607 -0.00937 0.03103 0.00338 O4 5 0.657368 0.098896 0.162578 11.00000 0.07506 0.06310 = 0.05772 -0.01104 0.01525 -0.00622 C1 1 0.629816 0.397517 0.022377 11.00000 0.08932 0.08073 = 0.15448 0.05739 0.01869 0.02734 AFIX 23 H1A 2 0.637337 0.434405 0.000612 11.00000 -1.20000 H1B 2 0.598484 0.423456 0.045416 11.00000 -1.20000 AFIX 0 C2 1 0.559166 0.336217 0.008873 11.00000 0.08113 0.08983 = 0.10282 0.03417 0.01972 0.01826 AFIX 23 H2A 2 0.586595 0.313763 -0.015907 11.00000 -1.20000 H2B 2 0.493024 0.358565 0.002670 11.00000 -1.20000 AFIX 0 C3 1 0.453767 0.222223 0.030603 11.00000 0.07281 0.08836 = 0.09225 -0.00516 -0.00292 0.00846 AFIX 23 H3A 2 0.390201 0.250838 0.033029 11.00000 -1.20000 H3B 2 0.460264 0.204442 0.002800 11.00000 -1.20000 AFIX 0 C4 1 0.449070 0.155015 0.058592 11.00000 0.06026 0.06336 = 0.06934 -0.01147 -0.00206 -0.00514 C5 1 0.461673 0.082798 0.042692 11.00000 0.09633 0.08533 = 0.07092 -0.03164 0.00856 -0.02107 AFIX 43 H5 2 0.474732 0.076209 0.015082 11.00000 -1.20000 AFIX 0 C6 1 0.454710 0.020330 0.068178 11.00000 0.10057 0.06578 = 0.07437 -0.02092 0.01259 -0.02549 AFIX 43 H6 2 0.460229 -0.028292 0.057159 11.00000 -1.20000 AFIX 0 C7 1 0.439977 0.028175 0.109003 11.00000 0.06337 0.08123 = 0.06989 -0.02665 0.01657 -0.02683 C8 1 0.429055 0.100684 0.125108 11.00000 0.06931 0.06804 = 0.06782 -0.01267 0.01218 -0.00026 AFIX 43 H8 2 0.418556 0.106916 0.152898 11.00000 -1.20000 AFIX 0 C9 1 0.433670 0.163476 0.100184 11.00000 0.07231 0.05738 = 0.08172 -0.02083 0.01302 0.00375 AFIX 43 H9 2 0.426431 0.211949 0.111244 11.00000 -1.20000 AFIX 0 C10 1 0.435381 -0.041027 0.136723 11.00000 0.08971 0.08082 = 0.08821 -0.01482 0.03440 -0.03539 AFIX 23 H10A 2 0.370376 -0.040828 0.151499 11.00000 -1.20000 H10B 2 0.437812 -0.086797 0.120242 11.00000 -1.20000 AFIX 0 C11 1 0.527041 -0.118019 0.189273 11.00000 0.10964 0.05715 = 0.08982 0.00452 0.04014 -0.01596 AFIX 23 H11A 2 0.458674 -0.132335 0.198582 11.00000 -1.20000 H11B 2 0.551719 -0.157443 0.170955 11.00000 -1.20000 AFIX 0 C12 1 0.597091 -0.113665 0.225238 11.00000 0.13164 0.06199 = 0.07842 0.02032 0.05108 0.00386 AFIX 23 H12A 2 0.568210 -0.078104 0.244833 11.00000 -1.20000 H12B 2 0.599724 -0.163326 0.238089 11.00000 -1.20000 AFIX 0 C13 1 0.784462 0.434565 0.054643 11.00000 0.09025 0.04609 = 0.16888 0.01367 0.03846 -0.00335 AFIX 23 H13A 2 0.779337 0.480049 0.038074 11.00000 -1.20000 H13B 2 0.856792 0.422289 0.057157 11.00000 -1.20000 AFIX 0 C14 1 0.739445 0.451297 0.096875 11.00000 0.08881 0.03488 = 0.16204 -0.00272 0.03464 -0.00123 AFIX 23 H14A 2 0.777996 0.492582 0.108966 11.00000 -1.20000 H14B 2 0.668961 0.468303 0.094059 11.00000 -1.20000 AFIX 0 C15 1 0.718374 0.402673 0.168152 11.00000 0.11372 0.04893 = 0.12663 -0.02862 0.03688 -0.01160 AFIX 23 H15A 2 0.652669 0.428625 0.170084 11.00000 -1.20000 H15B 2 0.770578 0.437139 0.178104 11.00000 -1.20000 AFIX 0 C16 1 0.715051 0.333274 0.194653 11.00000 0.09245 0.06274 = 0.09733 -0.03780 0.02024 -0.00617 C17 1 0.621268 0.300920 0.204586 11.00000 0.08434 0.06326 = 0.08223 -0.02871 0.01478 0.00326 AFIX 43 H17 2 0.560755 0.321961 0.194896 11.00000 -1.20000 AFIX 0 C18 1 0.618192 0.237432 0.228889 11.00000 0.07933 0.06752 = 0.08079 -0.01711 0.01968 0.00141 AFIX 43 H18 2 0.555082 0.214618 0.234524 11.00000 -1.20000 AFIX 0 C19 1 0.709171 0.205274 0.245823 11.00000 0.08999 0.07241 = 0.06947 -0.03346 0.00008 0.00582 C20 1 0.802689 0.239871 0.234241 11.00000 0.08479 0.09076 = 0.11225 -0.03966 -0.00989 0.00334 AFIX 43 H20 2 0.864203 0.219044 0.243064 11.00000 -1.20000 AFIX 0 C21 1 0.804942 0.304512 0.209892 11.00000 0.07458 0.09660 = 0.14199 -0.04925 0.01586 -0.01805 AFIX 43 H21 2 0.867199 0.328296 0.203911 11.00000 -1.20000 AFIX 0 C22 1 0.703775 0.137658 0.272127 11.00000 0.10371 0.09241 = 0.05759 -0.02319 -0.00032 0.02668 AFIX 23 H22A 2 0.637058 0.135615 0.285591 11.00000 -1.20000 H22B 2 0.755883 0.141178 0.292833 11.00000 -1.20000 AFIX 0 C23 1 0.714387 -0.000854 0.274580 11.00000 0.10693 0.09852 = 0.04800 0.01192 0.01948 0.02256 AFIX 23 H23A 2 0.643943 -0.008605 0.283684 11.00000 -1.20000 H23B 2 0.756334 0.007282 0.298318 11.00000 -1.20000 AFIX 0 C24 1 0.753097 -0.073055 0.251213 11.00000 0.12295 0.11164 = 0.05958 0.02596 0.02887 0.04395 AFIX 23 H24A 2 0.825661 -0.066563 0.244997 11.00000 -1.20000 H24B 2 0.746463 -0.116655 0.269148 11.00000 -1.20000 AFIX 0 C25 1 0.794138 0.350326 -0.003966 11.00000 0.07887 0.06982 = 0.13310 0.03897 0.02794 0.00504 AFIX 23 H25A 2 0.753584 0.314750 -0.019599 11.00000 -1.20000 H25B 2 0.802188 0.396033 -0.020246 11.00000 -1.20000 AFIX 0 C26 1 0.898480 0.316173 0.001433 11.00000 0.07653 0.07546 = 0.10251 0.03013 0.02151 0.00039 AFIX 23 H26A 2 0.941996 0.352273 0.015402 11.00000 -1.20000 H26B 2 0.929276 0.306097 -0.025012 11.00000 -1.20000 AFIX 0 C27 1 0.981924 0.189429 0.014855 11.00000 0.05726 0.08026 = 0.08319 0.01694 0.02009 0.00904 AFIX 23 H27A 2 1.046553 0.215970 0.018461 11.00000 -1.20000 H27B 2 0.977494 0.174504 -0.013425 11.00000 -1.20000 AFIX 0 C28 1 0.979288 0.118276 0.041747 11.00000 0.05991 0.06746 = 0.06060 0.00725 0.01838 0.01989 C29 1 0.921676 0.056925 0.030242 11.00000 0.05036 0.07254 = 0.05060 0.00837 0.02034 0.02158 C30 1 0.865637 0.054953 -0.006944 11.00000 0.04975 0.09536 = 0.04611 0.01132 0.01506 0.02538 AFIX 43 H30 2 0.869362 0.096782 -0.024227 11.00000 -1.20000 AFIX 0 C31 1 0.808101 -0.004847 -0.017754 11.00000 0.05621 0.10155 = 0.05232 0.00280 0.01232 0.01853 AFIX 43 H31 2 0.772870 -0.003696 -0.042130 11.00000 -1.20000 AFIX 0 C32 1 0.800574 -0.069164 0.007393 11.00000 0.06142 0.10051 = 0.05916 -0.00572 0.02048 0.00721 AFIX 43 H32 2 0.760124 -0.110598 0.000246 11.00000 -1.20000 AFIX 0 C33 1 0.854671 -0.069053 0.042819 11.00000 0.06472 0.07371 = 0.05462 0.01049 0.02334 0.02364 AFIX 43 H33 2 0.850677 -0.112103 0.059218 11.00000 -1.20000 AFIX 0 C34 1 0.915528 -0.008326 0.055900 11.00000 0.05571 0.06909 = 0.04987 0.00797 0.02083 0.02011 C35 1 0.971163 -0.009821 0.092107 11.00000 0.05767 0.07978 = 0.05316 0.00722 0.01815 0.02698 C36 1 1.033615 0.049904 0.102540 11.00000 0.05467 0.07692 = 0.05912 0.00501 0.01603 0.02333 C37 1 1.096404 0.049784 0.138255 11.00000 0.07314 0.10248 = 0.07085 0.00315 0.00499 0.02492 AFIX 43 H37 2 1.093561 0.007489 0.155235 11.00000 -1.20000 AFIX 0 C38 1 1.159413 0.108077 0.148414 11.00000 0.07413 0.10075 = 0.11124 -0.00491 -0.01257 0.00874 AFIX 43 H38 2 1.199385 0.104536 0.171536 11.00000 -1.20000 AFIX 0 C39 1 1.164472 0.173021 0.124427 11.00000 0.06120 0.11015 = 0.12163 -0.01162 -0.00282 0.01677 AFIX 43 H39 2 1.206232 0.213603 0.131773 11.00000 -1.20000 AFIX 0 C40 1 1.106359 0.176844 0.089215 11.00000 0.06366 0.07628 = 0.09814 0.00297 0.00368 0.01254 AFIX 43 H40 2 1.111332 0.220224 0.073102 11.00000 -1.20000 AFIX 0 C41 1 1.039564 0.116905 0.076894 11.00000 0.05526 0.08168 = 0.06763 0.00311 0.01621 0.02444 C42 1 0.960917 -0.079379 0.119653 11.00000 0.07622 0.08022 = 0.05839 0.00702 0.01529 0.01663 AFIX 23 H42A 2 1.022018 -0.084014 0.136027 11.00000 -1.20000 H42B 2 0.955510 -0.124890 0.103120 11.00000 -1.20000 AFIX 0 C43 1 0.860836 -0.137881 0.177452 11.00000 0.12297 0.05971 = 0.06555 0.01061 0.02610 0.01012 AFIX 23 H43A 2 0.886829 -0.183735 0.164486 11.00000 -1.20000 H43B 2 0.904809 -0.126440 0.200209 11.00000 -1.20000 AFIX 0 C44 1 0.755605 -0.152021 0.192683 11.00000 0.15314 0.06558 = 0.07704 0.02152 0.04106 0.01960 AFIX 23 H44A 2 0.757864 -0.195864 0.210571 11.00000 -1.20000 H44B 2 0.713831 -0.166065 0.169685 11.00000 -1.20000 AFIX 0 N1 4 0.732320 0.371248 0.033930 11.00000 0.07725 0.06066 = 0.11517 0.02735 0.03218 0.02242 N2 4 0.543572 0.274175 0.040062 11.00000 0.06152 0.06967 = 0.07206 0.01156 0.01133 0.01300 AFIX 23 H2C 2 0.532817 0.295677 0.064560 11.00000 -1.20000 H2D 2 0.601262 0.246053 0.041418 11.00000 -1.20000 AFIX 0 N3 4 0.520801 -0.043284 0.166311 11.00000 0.07194 0.05795 = 0.07508 -0.00605 0.02435 -0.01223 AFIX 23 H3C 2 0.512340 -0.005065 0.184259 11.00000 -1.20000 H3D 2 0.580657 -0.035449 0.152938 11.00000 -1.20000 AFIX 0 N4 4 0.741113 0.384771 0.124673 11.00000 0.07536 0.04079 = 0.13013 -0.01663 0.02099 -0.01068 AFIX 23 H4A 2 0.803570 0.362876 0.122946 11.00000 -1.20000 H4B 2 0.694851 0.350442 0.116089 11.00000 -1.20000 AFIX 0 N5 4 0.720051 0.067072 0.247898 11.00000 0.10941 0.07438 = 0.05977 -0.01296 0.01421 0.01900 AFIX 23 H5B 2 0.671741 0.063763 0.228673 11.00000 -1.20000 H5A 2 0.782003 0.068869 0.235440 11.00000 -1.20000 AFIX 0 N6 4 0.893103 0.242531 0.025599 11.00000 0.06714 0.05776 = 0.08547 0.01390 0.02275 0.00385 AFIX 23 H6A 2 0.833254 0.218862 0.020558 11.00000 -1.20000 H6B 2 0.894602 0.253379 0.052293 11.00000 -1.20000 AFIX 0 N7 4 0.866037 -0.073093 0.147564 11.00000 0.09460 0.06322 = 0.05851 0.00093 0.02371 0.01122 AFIX 23 H7B 2 0.868154 -0.028668 0.161162 11.00000 -1.20000 H7A 2 0.808978 -0.073192 0.132414 11.00000 -1.20000 AFIX 0 N8 4 0.701823 -0.089718 0.214787 11.00000 0.10834 0.06198 = 0.06635 0.01028 0.03589 0.00647 C46 1 0.621705 -0.315493 0.100740 11.00000 0.16491 0.04618 = 0.18561 -0.00133 -0.08720 -0.00670 F4 3 0.674190 -0.375991 0.109475 11.00000 0.24490 0.05295 = 0.24843 0.02440 -0.08399 0.00826 F5 3 0.540557 -0.336625 0.080449 11.00000 0.21212 0.09966 = 0.24878 0.04420 -0.10493 -0.04135 F6 3 0.588656 -0.285523 0.134508 11.00000 0.17313 0.09962 = 0.17814 0.01688 -0.02640 -0.00813 S2 6 0.695858 -0.246989 0.071335 11.00000 0.16144 0.05507 = 0.12060 -0.00724 -0.04156 0.02028 O8 5 0.623581 -0.187157 0.065322 11.00000 0.13902 0.06239 = 0.12675 0.00298 -0.05075 -0.00075 O9 5 0.778960 -0.227312 0.096867 11.00000 0.11576 0.06948 = 0.12483 -0.00182 -0.03776 0.01493 O10 5 0.723417 -0.287612 0.034712 11.00000 0.23291 0.16022 = 0.14920 -0.06698 -0.05273 0.07534 SAME 0.01 0.01 C46 F4 F5 F6 S2 O8 O9 O10 C45 1 0.391336 0.486051 0.105866 11.00000 0.13135 0.07961 = 0.10916 0.01478 0.04281 0.03492 F1 3 0.424613 0.499972 0.069451 11.00000 0.25822 0.22427 = 0.13714 0.08782 0.06846 0.14034 F2 3 0.446304 0.527981 0.130524 11.00000 0.22883 0.07944 = 0.18712 0.00530 0.00250 -0.01107 F3 3 0.297581 0.511142 0.108986 11.00000 0.11697 0.09258 = 0.32568 0.04128 0.07756 0.05602 S1 6 0.401661 0.386946 0.119535 11.00000 0.08827 0.05544 = 0.14046 -0.00155 0.04346 0.01151 O5 5 0.507056 0.369041 0.110234 11.00000 0.08551 0.07610 = 0.09910 0.00853 0.02349 0.02631 O6 5 0.330894 0.348516 0.094204 11.00000 0.11935 0.09765 = 0.45912 -0.10600 -0.03441 0.01645 O7 5 0.377991 0.385286 0.162205 11.00000 0.27741 0.12923 = 0.21102 0.06011 0.18249 0.07586 SAME 0.01 0.01 C46 F4 F5 F6 S2 O8 O9 O10 C47 1 0.340675 0.136473 0.260083 11.00000 0.11170 0.10106 = 0.30622 -0.09604 0.11059 -0.01404 F7 3 0.318154 0.168274 0.225780 11.00000 0.22716 0.25246 = 0.17041 -0.02938 -0.07705 0.11559 F8 3 0.256176 0.126294 0.281347 11.00000 0.20442 0.21273 = 0.59308 -0.17980 0.27673 -0.06798 F9 3 0.397356 0.183599 0.280515 11.00000 0.19112 0.08747 = 0.17464 -0.05075 0.09115 -0.01959 S3 6 0.404584 0.046491 0.252100 11.00000 0.13955 0.11138 = 0.09977 -0.02670 0.06739 -0.04286 O11 5 0.493524 0.066813 0.228773 11.00000 0.10796 0.06249 = 0.07377 -0.00160 0.04304 -0.00073 O12 5 0.333855 -0.000805 0.232887 11.00000 0.19299 0.17727 = 0.24380 -0.09079 0.10140 -0.10033 O13 5 0.431005 0.023270 0.293680 11.00000 0.25233 0.20481 = 0.23180 0.15968 0.12973 0.08149 SAME 0.01 0.01 C46 F4 F5 F6 S2 O8 O9 O10 C48 1 0.722256 0.255937 -0.125251 11.00000 0.15339 0.16637 = 0.20666 0.15105 -0.09883 -0.08422 F10 3 0.641270 0.239130 -0.146424 11.00000 0.12181 0.13910 = 0.14034 0.06186 -0.06287 -0.03339 F11 3 0.699349 0.315107 -0.102880 11.00000 0.29572 0.05827 = 0.33524 0.05073 -0.19351 -0.01977 F12 3 0.794290 0.276248 -0.150449 11.00000 0.18041 0.33331 = 0.17173 0.18285 -0.07325 -0.13560 S4 6 0.761700 0.177098 -0.093758 11.00000 0.07266 0.08281 = 0.07860 0.02733 -0.00634 -0.01052 O14 5 0.784713 0.118992 -0.122671 11.00000 0.09194 0.14640 = 0.12274 -0.01229 0.00406 0.01366 O15 5 0.673534 0.161926 -0.068773 11.00000 0.08011 0.08034 = 0.08796 0.02596 0.00335 -0.01271 O16 5 0.849366 0.206067 -0.072211 11.00000 0.09579 0.10657 = 0.08872 0.04305 -0.02484 -0.03644 SAME 0.01 0.01 C46 F4 F5 F6 S2 O8 O9 O10 C49 1 0.949447 0.628684 0.134167 11.00000 0.13744 0.15782 = 0.20555 0.03994 -0.00774 -0.03318 F13 3 0.908246 0.607017 0.100255 11.00000 0.18067 0.18981 = 0.24147 0.02978 -0.04128 -0.02874 F14 3 0.874619 0.654963 0.157320 11.00000 0.15887 0.19780 = 0.40622 0.07978 0.04247 0.07559 F15 3 1.010192 0.684331 0.126327 11.00000 0.15046 0.17396 = 0.49285 0.09957 -0.05216 -0.04531 S5 6 1.012053 0.550396 0.159796 11.00000 0.10009 0.16826 = 0.34034 0.11608 0.05305 0.05134 O17 5 1.085448 0.525082 0.130433 11.00000 0.16681 0.13927 = 0.57343 -0.06803 0.11895 -0.02175 O18 5 0.933357 0.499634 0.170238 11.00000 0.12097 0.19479 = 0.35910 0.14198 -0.00467 -0.02165 O19 5 1.060823 0.588059 0.194314 11.00000 0.38681 0.58127 = 0.48380 0.11553 -0.27949 -0.03638 O1W 5 0.922818 0.298549 0.107431 11.00000 0.06833 0.05490 = 0.11991 -0.00343 0.01109 0.00272 O2W 5 0.696080 0.177049 0.013466 11.00000 0.06994 0.06544 = 0.08484 0.01484 0.02652 0.00900 O3W 5 0.675247 -0.060165 0.107768 11.00000 0.08902 0.04772 = 0.06326 -0.00124 0.02433 0.00975 O4W 5 0.898992 0.057064 0.198743 11.00000 0.10221 0.08858 = 0.08073 -0.00960 0.02101 0.00404 O5W 5 1.061983 -0.026647 0.241024 11.00000 0.54475 0.53020 = 0.25863 -0.11917 -0.24575 0.30633 O6W 5 1.108046 0.362957 0.128922 11.00000 0.12607 0.10424 = 0.56283 0.00152 -0.01419 -0.01504 O7W 5 1.052356 0.478789 0.031086 11.00000 0.19189 0.22427 = 0.31572 0.08315 0.01599 -0.04957 HKLF 4 REM 1H6_TcO4 in P 21/c REM R1 = 0.1125 for 10772 Fo > 4sig(Fo) and 0.1240 for all 12810 data REM 937 parameters refined using 197 restraints END ; _database_code_depnum_ccdc_archive 'CCDC 961777'