Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Magnus Sandstrom' 'Alireza Molla Abbassi' 'Lars Eriksson' 'Janos Mink' 'Ingmar Persson' 'Mikhail Skripkin' 'Ann-Sofi Ullstrom' _publ_contact_author_name 'Prof Magnus Sandstrom' _publ_contact_author_address ; Structural Chemistry Stockholm University Stockholm SWEDEN ; _publ_contact_author_phone '46 8 161252' _publ_contact_author_fax '46 8 163118' _publ_contact_author_email magnuss@struc.su.se _publ_requestd_journal 'J. Chem. Soc. Dalton Trans.' #========================================================================= _publ_section_title ; Structure and Bonding of Bisaquamercuty (II) and Trisaquathallium(III) Trifluoromethanesulfonate ; data_hg8m0207 _database_code_CSD 188198 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H4 F6 Hg O8 S2' _chemical_formula_weight 534.76 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.878(3) _cell_length_b 7.977(3) _cell_length_c 9.831(4) _cell_angle_alpha 98.339(7) _cell_angle_beta 98.779(7) _cell_angle_gamma 96.104(7) _cell_volume 598.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3726 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description thin_slab _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 13.311 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0205 _exptl_absorpt_correction_T_max 0.2950 _exptl_absorpt_process_details 'X-RED 1.09 (STOE, 1997b)' _exptl_special_details ; Crystal decay was monitored by collecting duplicate frames at the end of the experiment and was found to be negligible. ; _diffrn_ambient_temperature 295(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 SMART area detector' _diffrn_measurement_method '\w-scan' _diffrn_detector_area_resol_mean 11.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3726 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.36 _reflns_number_total 2572 _reflns_number_gt 2373 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SMART (Bruker,1995)' _computing_data_reduction 'SAINT (Bruker,1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Bergerhoff, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2572 _refine_ls_number_parameters 190 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.28371(3) 0.26057(3) 0.49539(3) 0.04124(19) Uani 1 1 d DU . . O1A O 0.4317(9) 0.1761(9) 0.6641(8) 0.0477(15) Uani 1 1 d DU . . H1AA H 0.540(6) 0.250(9) 0.685(13) 0.072 Uiso 1 1 d D . . H1AB H 0.462(11) 0.065(4) 0.632(9) 0.072 Uiso 1 1 d D . . O1B O 0.1395(8) 0.3484(9) 0.3265(8) 0.0487(15) Uani 1 1 d DU . . H1BA H 0.183(12) 0.468(4) 0.335(12) 0.073 Uiso 1 1 d D . . H1BB H 0.017(3) 0.348(13) 0.324(14) 0.073 Uiso 1 1 d D . . S1 S 0.3802(2) 0.6998(3) 0.6878(2) 0.0371(4) Uani 1 1 d DU . . O11 O 0.2006(8) 0.7063(12) 0.6634(10) 0.071(2) Uani 1 1 d DU . . O12 O 0.4877(8) 0.8464(8) 0.6595(9) 0.0559(17) Uani 1 1 d DU . . O13 O 0.4384(14) 0.5445(10) 0.6268(11) 0.079(3) Uani 1 1 d DU . . C1 C 0.4362(17) 0.7062(19) 0.8710(13) 0.087(5) Uani 1 1 d DU . . F1A F 0.401(3) 0.850(2) 0.9395(13) 0.179(8) Uani 1 1 d DU . . F1B F 0.3448(18) 0.578(2) 0.9118(14) 0.151(6) Uani 1 1 d DU . . F1C F 0.6018(13) 0.698(2) 0.9088(12) 0.141(6) Uani 1 1 d DU . . S2 S -0.0984(2) 0.2083(2) 0.6705(2) 0.0341(4) Uani 1 1 d DU . . O21 O -0.2321(7) 0.3165(8) 0.6923(8) 0.0472(14) Uani 1 1 d DU . . O22 O 0.0500(8) 0.2995(9) 0.6326(8) 0.0504(15) Uani 1 1 d DU . . O23 O -0.1630(12) 0.0455(9) 0.5848(8) 0.0614(19) Uani 1 1 d DU . . C2 C -0.0239(14) 0.1550(15) 0.8421(12) 0.066(3) Uani 1 1 d DU . . F2A F -0.1487(14) 0.0636(16) 0.8824(11) 0.105(3) Uani 1 1 d DU . . F2B F 0.0275(17) 0.2970(16) 0.9348(10) 0.114(4) Uani 1 1 d DU . . F2C F 0.1088(14) 0.0701(16) 0.8347(11) 0.115(4) Uani 1 1 d DU . . 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 Hg1 0.0281(2) 0.0291(2) 0.0666(3) 0.00728(14) 0.00851(14) 0.00439(12) O1A 0.034(3) 0.035(3) 0.077(4) 0.017(3) 0.012(3) 0.005(2) O1B 0.031(3) 0.041(3) 0.077(4) 0.019(3) 0.012(3) 0.003(3) S1 0.0246(8) 0.0326(9) 0.0535(10) 0.0110(8) 0.0044(7) -0.0013(7) O11 0.026(3) 0.091(6) 0.099(6) 0.040(5) 0.002(3) 0.002(3) O12 0.035(3) 0.041(3) 0.098(5) 0.028(3) 0.020(3) 0.000(3) O13 0.079(6) 0.047(4) 0.103(7) -0.011(4) 0.018(5) 0.002(4) C1 0.073(8) 0.132(15) 0.053(6) 0.028(8) 0.002(6) -0.005(9) F1A 0.22(2) 0.198(16) 0.105(8) -0.055(9) 0.051(10) 0.034(14) F1B 0.129(10) 0.220(17) 0.123(9) 0.114(11) 0.024(8) -0.012(10) F1C 0.072(6) 0.242(18) 0.104(7) 0.076(10) -0.030(5) -0.001(8) S2 0.0255(8) 0.0276(8) 0.0493(10) 0.0093(7) 0.0050(7) 0.0015(6) O21 0.029(3) 0.038(3) 0.076(4) 0.013(3) 0.010(3) 0.007(2) O22 0.033(3) 0.047(3) 0.071(4) 0.009(3) 0.011(3) 0.002(3) O23 0.072(5) 0.034(3) 0.073(5) 0.002(3) 0.007(4) -0.002(3) C2 0.056(6) 0.085(8) 0.067(6) 0.036(6) 0.010(5) 0.027(6) F2A 0.113(8) 0.130(9) 0.092(6) 0.067(6) 0.035(6) 0.010(7) F2B 0.122(9) 0.134(10) 0.065(5) -0.004(5) -0.021(5) 0.006(8) F2C 0.094(6) 0.161(10) 0.125(7) 0.083(7) 0.027(6) 0.080(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 O1A 2.113(7) . yes Hg1 O1B 2.114(7) . yes Hg1 O22 2.463(6) . yes Hg1 O23 2.491(7) 2_556 yes Hg1 O13 2.523(9) . yes Hg1 O12 2.660(7) 2_666 yes Hg1 O13 3.045(11) 2_666 ? Hg1 S1 3.435(2) 2_666 ? O1A H1AA 0.963(10) . ? O1A H1AB 0.963(10) . ? O1B H1BA 0.965(10) . ? O1B H1BB 0.962(10) . ? S1 O11 1.406(6) . yes S1 O13 1.448(8) . yes S1 O12 1.455(6) . yes S1 C1 1.779(13) . yes S1 Hg1 3.435(2) 2_666 ? O12 Hg1 2.660(7) 2_666 ? O13 Hg1 3.045(11) 2_666 ? C1 F1C 1.313(14) . yes C1 F1A 1.321(15) . yes C1 F1B 1.332(15) . yes S2 O22 1.437(6) . yes S2 O23 1.438(7) . yes S2 O21 1.453(6) . yes S2 C2 1.825(11) . yes O23 Hg1 2.491(7) 2_556 ? C2 F2A 1.306(13) . yes C2 F2C 1.311(12) . yes C2 F2B 1.329(14) . yes 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 O1A Hg1 O1B 179.0(2) . . ? O1A Hg1 O22 90.1(3) . . ? O1B Hg1 O22 90.6(3) . . ? O1A Hg1 O23 86.1(3) . 2_556 ? O1B Hg1 O23 94.7(3) . 2_556 ? O22 Hg1 O23 90.3(3) . 2_556 ? O1A Hg1 O13 80.4(3) . . ? O1B Hg1 O13 98.8(3) . . ? O22 Hg1 O13 88.0(3) . . ? O23 Hg1 O13 166.4(3) 2_556 . ? O1A Hg1 O12 87.4(3) . 2_666 ? O1B Hg1 O12 92.1(3) . 2_666 ? O22 Hg1 O12 168.7(2) . 2_666 ? O23 Hg1 O12 78.6(2) 2_556 2_666 ? O13 Hg1 O12 102.4(3) . 2_666 ? O1A Hg1 O13 102.2(3) . 2_666 ? O1B Hg1 O13 76.8(3) . 2_666 ? O22 Hg1 O13 142.8(2) . 2_666 ? O23 Hg1 O13 125.1(3) 2_556 2_666 ? O13 Hg1 O13 60.3(4) . 2_666 ? O12 Hg1 O13 48.4(2) 2_666 2_666 ? O1A Hg1 S1 94.46(19) . 2_666 ? O1B Hg1 S1 84.76(19) . 2_666 ? O22 Hg1 S1 167.70(16) . 2_666 ? O23 Hg1 S1 101.4(2) 2_556 2_666 ? O13 Hg1 S1 81.5(2) . 2_666 ? O12 Hg1 S1 23.52(13) 2_666 2_666 ? O13 Hg1 S1 24.90(15) 2_666 2_666 ? Hg1 O1A H1AA 106(7) . . ? Hg1 O1A H1AB 109(5) . . ? H1AA O1A H1AB 104(2) . . ? Hg1 O1B H1BA 106(6) . . ? Hg1 O1B H1BB 118(8) . . ? H1BA O1B H1BB 103(2) . . ? O11 S1 O13 116.5(6) . . ? O11 S1 O12 115.7(4) . . ? O13 S1 O12 109.1(5) . . ? O11 S1 C1 105.2(6) . . ? O13 S1 C1 104.5(7) . . ? O12 S1 C1 104.4(6) . . ? O11 S1 Hg1 137.0(4) . 2_666 ? O13 S1 Hg1 62.3(4) . 2_666 ? O12 S1 Hg1 46.8(3) . 2_666 ? C1 S1 Hg1 116.9(4) . 2_666 ? S1 O12 Hg1 109.7(4) . 2_666 ? S1 O13 Hg1 133.7(6) . . ? S1 O13 Hg1 92.8(4) . 2_666 ? Hg1 O13 Hg1 119.7(3) . 2_666 ? F1C C1 F1A 107.4(14) . . ? F1C C1 F1B 108.9(12) . . ? F1A C1 F1B 107.2(14) . . ? F1C C1 S1 111.9(10) . . ? F1A C1 S1 110.5(11) . . ? F1B C1 S1 110.8(10) . . ? O22 S2 O23 115.4(5) . . ? O22 S2 O21 112.0(4) . . ? O23 S2 O21 113.6(5) . . ? O22 S2 C2 105.8(5) . . ? O23 S2 C2 104.1(5) . . ? O21 S2 C2 104.6(5) . . ? S2 O22 Hg1 142.2(4) . . ? S2 O23 Hg1 163.0(5) . 2_556 ? F2A C2 F2C 110.3(11) . . ? F2A C2 F2B 109.2(11) . . ? F2C C2 F2B 108.3(11) . . ? F2A C2 S2 110.2(8) . . ? F2C C2 S2 108.7(8) . . ? F2B C2 S2 110.1(9) . . ? _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.856 _refine_diff_density_max 2.290 _refine_diff_density_min -2.236 _refine_diff_density_rms 0.254 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1A H1AA O21 0.96(1) 1.80(1) 2.720(9) 158 1_655 yes O1A H1AB O12 0.96(1) 1.83(1) 2.708(9) 150 1_545 yes O1B H1BA O21 0.96(1) 1.78(1) 2.735(9) 166 2_566 yes O1B H1BB O11 0.96(1) 1.75(1) 2.688(9) 164 2_566 yes ############################################################################## data_tl2d1 _database_code_CSD 188199 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H6 F9 O12 S3 Tl' _chemical_formula_weight 705.63 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' 'S' 'S' 0.1246 0.1234 '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' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.990(9) _cell_length_b 13.376(4) _cell_length_c 19.133(6) _cell_angle_alpha 90.00 _cell_angle_beta 149.737(18) _cell_angle_gamma 90.00 _cell_volume 3481(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 22.0 _exptl_crystal_description slab _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 9.787 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.303 _exptl_absorpt_correction_T_max 0.734 _exptl_absorpt_process_details 'X-RED 1.09 (STOE, 1997b)' _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 'STOE IPDS' _diffrn_detector_area_resol_mean 6.7 _diffrn_measurement_method 'area detector' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7288 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 20.92 _reflns_number_total 1822 _reflns_number_gt 1350 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Expose (STOE, 1997a)' _computing_cell_refinement 'Cell (STOE, 1997a)' _computing_data_reduction 'Integrate(STOE, 1997a) & X-RED (STOE, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Bergerhoff, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1822 _refine_ls_number_parameters 271 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl1 Tl 0.10726(4) 0.22086(4) 0.54299(5) 0.0271(2) Uani 1 1 d . . . O1 O 0.1529(7) 0.2723(9) 0.4955(9) 0.045(3) Uani 1 1 d D . . H11 H 0.218(4) 0.298(10) 0.568(8) 0.068 Uiso 1 1 d D . . H12 H 0.116(7) 0.300(9) 0.412(6) 0.068 Uiso 1 1 d D . . O2 O 0.0600(7) 0.1781(7) 0.5922(9) 0.036(3) Uani 1 1 d D . . H21 H -0.006(4) 0.197(7) 0.525(10) 0.054 Uiso 1 1 d D . . H22 H 0.064(7) 0.108(3) 0.609(12) 0.054 Uiso 1 1 d D . . O3 O 0.2140(7) 0.0983(7) 0.6700(10) 0.036(3) Uani 1 1 d D . . H31 H 0.170(5) 0.043(5) 0.609(9) 0.054 Uiso 1 1 d D . . H32 H 0.257(7) 0.096(9) 0.683(13) 0.054 Uiso 1 1 d D . . S1 S 0.3181(3) 0.3188(3) 0.8745(3) 0.0291(10) Uani 1 1 d . . . O11 O 0.3560(7) 0.4157(7) 0.9369(9) 0.046(3) Uani 1 1 d . . . O12 O 0.3791(8) 0.2559(7) 0.9070(11) 0.049(3) Uani 1 1 d . . . O13 O 0.2143(7) 0.3253(7) 0.7237(8) 0.036(3) Uani 1 1 d . . . C1 C 0.3074(14) 0.2533(12) 0.9457(17) 0.048(5) Uani 1 1 d . . . F11 F 0.2754(7) 0.1628(7) 0.8974(9) 0.062(3) Uani 1 1 d . . . F12 F 0.3963(8) 0.2482(7) 1.0818(9) 0.084(4) Uani 1 1 d . . . F13 F 0.2515(10) 0.3033(8) 0.9199(13) 0.090(4) Uani 1 1 d . . . S2 S -0.0987(3) 0.0795(3) 0.2685(4) 0.0311(10) Uani 1 1 d . . . O21 O -0.0003(8) 0.1138(7) 0.3664(10) 0.044(3) Uani 1 1 d . . . O22 O -0.1683(8) 0.1580(7) 0.1848(11) 0.053(3) Uani 1 1 d . . . O23 O -0.0978(8) 0.0152(7) 0.3290(10) 0.053(3) Uani 1 1 d . . . C2 C -0.1322(14) -0.0014(13) 0.1540(18) 0.047(5) Uani 1 1 d . . . F21 F -0.1246(8) 0.0464(8) 0.1038(10) 0.080(3) Uani 1 1 d . . . F22 F -0.2253(8) -0.0269(8) 0.0492(9) 0.075(3) Uani 1 1 d . . . F23 F -0.0757(9) -0.0809(8) 0.2220(12) 0.088(4) Uani 1 1 d . . . S3 S -0.0677(3) 0.3888(3) 0.2967(4) 0.0301(10) Uani 1 1 d . . . O31 O 0.0004(7) 0.3409(7) 0.4297(9) 0.037(3) Uani 1 1 d . . . O32 O -0.0601(8) 0.3448(8) 0.2382(10) 0.048(3) Uani 1 1 d . . . O33 O -0.1629(8) 0.4046(8) 0.2097(11) 0.052(3) Uani 1 1 d . . . C3 C -0.0152(17) 0.5129(13) 0.353(2) 0.060(5) Uani 1 1 d . . . F31 F 0.0755(10) 0.5054(9) 0.4406(14) 0.109(5) Uani 1 1 d . . . F32 F -0.0641(10) 0.5653(8) 0.2467(13) 0.097(4) Uani 1 1 d . . . F33 F -0.0192(13) 0.5607(8) 0.4061(16) 0.126(6) 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 Tl1 0.0204(3) 0.0362(3) 0.0204(3) -0.0020(3) 0.0170(3) -0.0023(3) O1 0.021(6) 0.085(8) 0.020(5) 0.009(6) 0.016(5) -0.003(6) O2 0.026(6) 0.049(6) 0.032(5) 0.011(5) 0.025(6) 0.008(5) O3 0.034(7) 0.045(6) 0.032(6) -0.004(5) 0.029(6) -0.002(5) S1 0.026(2) 0.030(2) 0.024(2) -0.0028(16) 0.021(2) -0.0038(17) O11 0.034(7) 0.028(6) 0.028(6) -0.001(5) 0.020(6) -0.001(5) O12 0.048(8) 0.052(8) 0.058(7) 0.000(5) 0.047(7) 0.007(5) O13 0.028(7) 0.046(6) 0.021(5) -0.004(4) 0.019(5) -0.007(5) C1 0.058(14) 0.047(13) 0.043(11) 0.005(8) 0.044(12) 0.004(9) F11 0.078(8) 0.045(6) 0.072(6) 0.001(5) 0.066(7) -0.010(5) F12 0.085(9) 0.096(10) 0.039(6) 0.004(5) 0.048(7) -0.009(6) F13 0.138(11) 0.101(9) 0.130(10) 0.009(7) 0.131(10) 0.018(7) S2 0.024(3) 0.035(2) 0.023(2) -0.0057(18) 0.019(2) -0.004(2) O21 0.032(7) 0.053(7) 0.038(6) -0.018(5) 0.030(6) -0.010(5) O22 0.045(8) 0.042(7) 0.059(7) 0.016(6) 0.043(7) 0.018(6) O23 0.073(9) 0.052(7) 0.054(7) -0.009(6) 0.058(7) -0.015(6) C2 0.047(14) 0.056(12) 0.037(10) -0.025(10) 0.037(11) -0.027(10) F21 0.083(9) 0.128(9) 0.061(6) -0.029(6) 0.067(7) -0.038(7) F22 0.052(8) 0.114(9) 0.039(6) -0.032(6) 0.036(7) -0.042(6) F23 0.103(10) 0.071(8) 0.077(7) -0.010(6) 0.076(8) 0.017(7) S3 0.025(3) 0.041(2) 0.027(2) 0.0051(17) 0.023(2) 0.0045(18) O31 0.039(7) 0.049(6) 0.028(5) 0.011(5) 0.030(6) 0.016(5) O32 0.049(8) 0.070(8) 0.042(6) -0.006(6) 0.042(6) 0.001(6) O33 0.031(8) 0.080(8) 0.045(7) 0.026(6) 0.033(7) 0.021(6) C3 0.058(16) 0.051(12) 0.061(13) 0.017(10) 0.051(13) 0.010(10) F31 0.068(10) 0.082(9) 0.099(9) -0.016(7) 0.061(9) -0.035(7) F32 0.123(11) 0.073(8) 0.109(10) 0.029(7) 0.102(10) 0.013(7) F33 0.239(18) 0.063(8) 0.185(14) -0.036(8) 0.199(16) -0.023(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl1 O1 2.181(9) . yes Tl1 O31 2.190(9) . yes Tl1 O3 2.191(10) . yes Tl1 O2 2.217(9) . yes Tl1 O21 2.225(9) . yes Tl1 O13 2.235(8) . yes Tl1 H31 2.53(8) . ? O1 H11 0.961(11) . ? O1 H12 0.964(11) . ? O2 H21 0.962(11) . ? O2 H22 0.962(11) . ? O3 H31 0.962(11) . ? O3 H32 0.960(11) . ? S1 O12 1.427(11) . yes S1 O11 1.429(9) . yes S1 O13 1.490(9) . yes S1 C1 1.841(17) . yes C1 F13 1.30(2) . yes C1 F11 1.299(16) . yes C1 F12 1.322(19) . yes S2 O22 1.415(10) . yes S2 O23 1.426(10) . yes S2 O21 1.475(11) . yes S2 C2 1.833(15) . yes C2 F21 1.309(17) . yes C2 F23 1.313(19) . yes C2 F22 1.321(18) . yes S3 O33 1.424(11) . yes S3 O32 1.427(10) . yes S3 O31 1.477(9) . yes S3 C3 1.813(19) . yes C3 F33 1.28(2) . yes C3 F31 1.31(2) . yes C3 F32 1.317(19) . yes 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 O1 Tl1 O31 95.2(4) . . ? O1 Tl1 O3 91.4(4) . . ? O31 Tl1 O3 173.0(3) . . ? O1 Tl1 O2 176.5(4) . . ? O31 Tl1 O2 82.0(3) . . ? O3 Tl1 O2 91.3(3) . . ? O1 Tl1 O21 92.1(4) . . ? O31 Tl1 O21 95.4(4) . . ? O3 Tl1 O21 86.8(4) . . ? O2 Tl1 O21 90.2(4) . . ? O1 Tl1 O13 90.4(4) . . ? O31 Tl1 O13 84.9(3) . . ? O3 Tl1 O13 92.7(3) . . ? O2 Tl1 O13 87.3(3) . . ? O21 Tl1 O13 177.5(3) . . ? O1 Tl1 H31 98(2) . . ? O31 Tl1 H31 157.3(12) . . ? O3 Tl1 H31 22.0(11) . . ? O2 Tl1 H31 86(2) . . ? O21 Tl1 H31 65.6(15) . . ? O13 Tl1 H31 113.7(16) . . ? Tl1 O1 H11 120(7) . . ? Tl1 O1 H12 131(7) . . ? H11 O1 H12 104(2) . . ? Tl1 O2 H21 116(8) . . ? Tl1 O2 H22 116(8) . . ? H21 O2 H22 105(2) . . ? Tl1 O3 H31 99(6) . . ? Tl1 O3 H32 117(8) . . ? H31 O3 H32 105(2) . . ? O12 S1 O11 116.5(7) . . ? O12 S1 O13 114.3(6) . . ? O11 S1 O13 110.9(6) . . ? O12 S1 C1 104.9(7) . . ? O11 S1 C1 105.7(7) . . ? O13 S1 C1 103.1(7) . . ? S1 O13 Tl1 135.7(6) . . ? F13 C1 F11 111.8(16) . . ? F13 C1 F12 108.2(14) . . ? F11 C1 F12 108.3(12) . . ? F13 C1 S1 110.3(11) . . ? F11 C1 S1 110.4(11) . . ? F12 C1 S1 107.6(13) . . ? O22 S2 O23 116.1(7) . . ? O22 S2 O21 112.4(6) . . ? O23 S2 O21 114.0(6) . . ? O22 S2 C2 106.5(8) . . ? O23 S2 C2 105.0(7) . . ? O21 S2 C2 101.0(7) . . ? S2 O21 Tl1 133.2(6) . . ? F21 C2 F23 109.7(16) . . ? F21 C2 F22 108.0(14) . . ? F23 C2 F22 110.7(14) . . ? F21 C2 S2 111.1(11) . . ? F23 C2 S2 110.0(11) . . ? F22 C2 S2 107.3(12) . . ? O33 S3 O32 118.7(6) . . ? O33 S3 O31 112.5(6) . . ? O32 S3 O31 111.3(6) . . ? O33 S3 C3 104.7(9) . . ? O32 S3 C3 106.0(9) . . ? O31 S3 C3 101.6(8) . . ? S3 O31 Tl1 129.7(5) . . ? F33 C3 F31 111.6(19) . . ? F33 C3 F32 107.4(16) . . ? F31 C3 F32 106.7(17) . . ? F33 C3 S3 111.8(15) . . ? F31 C3 S3 109.1(13) . . ? F32 C3 S3 110.1(14) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 20.92 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.595 _refine_diff_density_min -2.226 _refine_diff_density_rms 0.178 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H11 O22 0.96(1) 1.70(1) 2.661(14) 174 8_556 yes O1 H12 O32 0.96(1) 1.85(1) 2.803(12) 171 2_555 yes O2 H21 O12 0.96(1) 1.74(1) 2.699(14) 174 8_455 yes O2 H22 O23 0.96(1) 1.76(1) 2.709(13) 169 5_556 yes O3 H31 O11 0.96(1) 1.76(1) 2.654(13) 153 4_546 yes O3 H32 O33 0.96(1) 1.73(1) 2.694(14) 179 8_556 yes