# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1792 data_[Tl(Tm)2]I.2H2O.3CH2Cl2 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jul 14 10:48:43 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 17.272(3) _cell_length_b 17.2720 _cell_length_c 17.2720 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5152(1) _cell_formula_units_Z 12 _cell_measurement_temperature 295.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 33.5 _cell_measurement_theta_max 37.5 #------------------------------------------------------------------------------ _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P 21 3 ' _symmetry_Int_Tables_number 198 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +z, +x, +y' ' +y, +z, +x' '1/2+x,1/2-y, -z' '1/2+z,1/2-x, -y' '1/2+y,1/2-z, -x' ' -x,1/2+y,1/2-z' ' -z,1/2+x,1/2-y' ' -y,1/2+z,1/2-x' '1/2-x, -y,1/2+z' '1/2-z, -x,1/2+y' '1/2-y, -z,1/2+x' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 441.56 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H14 B0.67 Cl2 I0.33 N4 O0.67 S2 Tl0.33' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 4.322 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_correction_T_min 0.640 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -6.75 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 2 -1 -2 -4 4 -5 3 -1 _diffrn_reflns_number 5032 _reflns_number_total 1684 _reflns_number_observed 1373 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 7.82 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.05441 _diffrn_orient_matrix_UB_12 -0.01552 _diffrn_orient_matrix_UB_13 -0.01228 _diffrn_orient_matrix_UB_21 0.01972 _diffrn_orient_matrix_UB_22 -0.04566 _diffrn_orient_matrix_UB_23 -0.02966 _diffrn_orient_matrix_UB_31 -0.00172 _diffrn_orient_matrix_UB_32 -0.03204 _diffrn_orient_matrix_UB_33 0.04819 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 108 0.003 0.002 'International Tables' H 0 120 0.000 0.000 'International Tables' B 0 8 0.001 0.001 'International Tables' I 0 3 -0.474 1.812 'International Tables' N 0 48 0.006 0.003 'International Tables' S 0 24 0.125 0.123 'International Tables' Tl 0 3 -2.836 9.669 'International Tables' Cl 0 24 0.148 0.159 'International Tables' O 0 12 0.011 0.006 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Tl(1) -0.54206(6) -0.5421 -0.5421 0.0594 Uij ? ? I(1) -0.46197(10) 1.4620 0.9620 0.0681 Uij ? ? Cl(1) -0.6875(7) -0.2412(6) -0.5702(7) 0.1430 Uij ? ? Cl(2) -0.7608(6) -0.2319(8) -0.4223(8) 0.1576 Uij ? ? S(1) -0.5970(4) -0.4265(4) -0.4541(4) 0.0674 Uij ? ? S(2) -0.6399(4) -0.4863(4) -0.6496(4) 0.0697 Uij ? ? O(2) -0.715(1) 1.7151 1.2151 0.1025 Uij ? ? O(3) 0.627(2) 1.1273 0.3727 0.1974 Uij ? ? N(1) -0.472(1) -0.429(1) -0.353(1) 0.0725 Uij ? ? N(2) -0.581(1) -0.470(1) -0.305(1) 0.0802 Uij ? ? N(3) -0.736(1) -0.618(1) -0.647(1) 0.0735 Uij ? ? N(4) -0.786(1) -0.515(1) -0.594(1) 0.0791 Uij ? ? C(1) -0.545(2) -0.443(1) -0.369(1) 0.0632 Uij ? ? C(2) -0.460(2) -0.450(2) -0.278(2) 0.0781 Uij ? ? C(3) -0.523(2) -0.473(2) -0.247(2) 0.1001 Uij ? ? C(4) -0.661(2) -0.495(2) -0.302(2) 0.1119 Uij ? ? C(5) -0.720(1) -0.541(2) -0.629(1) 0.0597 Uij ? ? C(6) -0.809(2) -0.638(2) -0.621(2) 0.0860 Uij ? ? C(7) -0.842(2) -0.576(2) -0.588(2) 0.0939 Uij ? ? C(8) -0.793(2) -0.435(2) -0.565(2) 0.1069 Uij ? ? C(9) -0.675(2) -0.231(2) -0.471(2) 0.0975 Uij ? ? B(1) -0.403(1) -0.4025 -0.4025 0.0566 Uij ? ? B(2) -0.684(2) -0.6843 -0.6843 0.0880 Uij ? ? H(1) -0.4104 -0.4413 -0.2512 0.0916 Uij ? ? H(2) -0.5315 -0.4941 -0.1940 0.1407 Uij ? ? H(3) -0.6880 -0.4862 -0.3444 0.1158 Uij ? ? H(4) -0.6867 -0.4725 -0.2556 0.1158 Uij ? ? H(5) -0.6606 -0.5516 -0.2892 0.1158 Uij ? ? H(6) -0.8358 -0.6877 -0.6208 0.0751 Uij ? ? H(7) -0.8898 -0.5717 -0.5606 0.0884 Uij ? ? H(8) -0.7856 -0.3938 -0.5992 0.1474 Uij ? ? H(9) -0.7563 -0.4232 -0.5195 0.1474 Uij ? ? H(10) -0.8441 -0.4243 -0.5382 0.1474 Uij ? ? H(11) -0.6487 -0.1816 -0.4563 0.1125 Uij ? ? H(12) -0.6411 -0.2707 -0.4479 0.1125 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tl(1) 0.0594(5) 0.0594 0.0594 -0.0005(5) -0.0005 -0.0005 I(1) 0.0681(8) 0.0681 0.0681 -0.0008(10) -0.0008 0.0008 Cl(1) 0.16(1) 0.113(8) 0.16(1) 0.013(7) 0.003(8) -0.014(7) Cl(2) 0.106(7) 0.19(1) 0.18(1) 0.008(8) 0.022(8) 0.049(10) S(1) 0.067(4) 0.072(4) 0.062(4) 0.006(3) -0.003(4) -0.001(4) S(2) 0.075(4) 0.064(4) 0.071(4) -0.001(3) 0.005(4) -0.001(3) O(2) 0.10(1) 0.1025 0.1025 0.01(1) 0.0081 -0.0081 O(3) 0.20(2) 0.1974 0.1974 -0.04(3) 0.0410 0.0410 N(1) 0.08(2) 0.08(1) 0.05(1) 0.00(1) 0.01(1) 0.01(1) N(2) 0.09(2) 0.09(2) 0.06(1) 0.02(1) 0.02(1) -0.01(1) N(3) 0.07(1) 0.09(2) 0.06(1) 0.00(1) 0.00(1) 0.02(1) N(4) 0.04(1) 0.12(2) 0.08(1) 0.01(1) -0.01(1) -0.02(1) C(1) 0.07(1) 0.08(2) 0.04(1) 0.02(2) 0.00(1) 0.00(1) C(2) 0.06(2) 0.09(2) 0.08(2) -0.01(2) 0.01(2) -0.01(2) C(3) 0.13(3) 0.09(2) 0.09(2) 0.04(2) 0.00(2) 0.00(2) C(4) 0.07(2) 0.19(4) 0.08(2) 0.02(2) 0.03(2) 0.01(2) C(5) 0.04(1) 0.07(2) 0.07(1) -0.01(1) -0.01(1) 0.02(2) C(6) 0.06(2) 0.09(2) 0.10(2) 0.00(2) 0.01(2) 0.03(2) C(7) 0.06(2) 0.12(3) 0.09(2) -0.01(2) -0.02(2) -0.01(2) C(8) 0.12(3) 0.09(2) 0.11(3) 0.04(2) -0.02(2) -0.04(2) C(9) 0.09(2) 0.10(2) 0.10(3) 0.01(2) 0.00(2) 0.01(2) B(1) 0.06(1) 0.0566 0.0566 -0.01(1) -0.0109 -0.0109 B(2) 0.09(2) 0.0880 0.0880 -0.01(2) -0.0125 -0.0125 #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 5.54857 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1373 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_obs 0.0712 _refine_ls_wR_factor_all 0.0812 _refine_ls_wR_factor_obs 0.0748 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.514 _refine_ls_shift/esd_max 0.3550 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.41 _refine_diff_density_max 1.68 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl(1) S(1) 2.682(7) ? ? yes Tl(1) S(1) 2.682(7) ? ? yes Tl(1) S(1) 2.682(7) ? ? yes Tl(1) S(2) 2.690(7) ? ? yes Tl(1) S(2) 2.690(7) ? ? yes Tl(1) S(2) 2.690(7) ? ? yes Cl(1) C(9) 1.73(4) ? ? yes Cl(2) C(9) 1.71(3) ? ? yes S(1) C(1) 1.74(2) ? ? yes S(2) C(5) 1.71(2) ? ? yes N(1) C(1) 1.31(4) ? ? yes N(1) C(2) 1.37(3) ? ? yes N(1) B(1) 1.54(3) ? ? yes N(2) C(1) 1.36(3) ? ? yes N(2) C(3) 1.42(4) ? ? yes N(2) C(4) 1.45(4) ? ? yes N(3) C(5) 1.39(4) ? ? yes N(3) C(6) 1.39(4) ? ? yes N(3) B(2) 1.59(3) ? ? yes N(4) C(5) 1.37(3) ? ? yes N(4) C(7) 1.42(4) ? ? yes N(4) C(8) 1.46(4) ? ? yes C(2) C(3) 1.26(5) ? ? yes C(2) H(1) 0.990 ? ? no C(3) H(2) 0.995 ? ? no C(4) H(3) 0.879 ? ? no C(4) H(4) 0.993 ? ? no C(4) H(5) 1.010 ? ? no C(6) C(7) 1.34(5) ? ? yes C(6) H(6) 0.973 ? ? no C(7) H(7) 0.961 ? ? no C(8) H(8) 0.941 ? ? no C(8) H(9) 1.028 ? ? no C(8) H(10) 1.012 ? ? no C(9) H(11) 1.005 ? ? no C(9) H(12) 0.980 ? ? no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Tl(1) S(1) 92.4(2) ? ? ? yes S(1) Tl(1) S(1) 92.4(2) ? ? ? yes S(1) Tl(1) S(2) 84.4(2) ? ? ? yes S(1) Tl(1) S(2) 91.2(2) ? ? ? yes S(1) Tl(1) S(2) 175.3(2) ? ? ? yes S(1) Tl(1) S(1) 92.4(2) ? ? ? yes S(1) Tl(1) S(2) 175.3(2) ? ? ? yes S(1) Tl(1) S(2) 84.4(2) ? ? ? yes S(1) Tl(1) S(2) 91.2(2) ? ? ? yes S(1) Tl(1) S(2) 91.2(2) ? ? ? yes S(1) Tl(1) S(2) 175.3(2) ? ? ? yes S(1) Tl(1) S(2) 84.4(2) ? ? ? yes S(2) Tl(1) S(2) 92.2(2) ? ? ? yes S(2) Tl(1) S(2) 92.2(2) ? ? ? yes S(2) Tl(1) S(2) 92.2(2) ? ? ? yes Tl(1) S(1) C(1) 99.9(8) ? ? ? yes Tl(1) S(2) C(5) 99.6(8) ? ? ? yes C(1) N(1) C(2) 106(2) ? ? ? yes C(1) N(1) B(1) 133(1) ? ? ? yes C(2) N(1) B(1) 119(2) ? ? ? yes C(1) N(2) C(3) 105(2) ? ? ? yes C(1) N(2) C(4) 123(2) ? ? ? yes C(3) N(2) C(4) 130(2) ? ? ? yes C(5) N(3) C(6) 110(2) ? ? ? yes C(5) N(3) B(2) 132(1) ? ? ? yes C(6) N(3) B(2) 117(2) ? ? ? yes C(5) N(4) C(7) 110(2) ? ? ? yes C(5) N(4) C(8) 121(2) ? ? ? yes C(7) N(4) C(8) 128(2) ? ? ? yes S(1) C(1) N(1) 129(1) ? ? ? yes S(1) C(1) N(2) 120(2) ? ? ? yes N(1) C(1) N(2) 109(1) ? ? ? yes N(1) C(2) C(3) 111(2) ? ? ? yes N(1) C(2) H(1) 122.0 ? ? ? no C(3) C(2) H(1) 126.3 ? ? ? no N(2) C(3) C(2) 107(2) ? ? ? yes N(2) C(3) H(2) 123.3 ? ? ? no C(2) C(3) H(2) 129.4 ? ? ? no N(2) C(4) H(3) 115.9 ? ? ? no N(2) C(4) H(4) 110.0 ? ? ? no N(2) C(4) H(5) 106.4 ? ? ? no H(3) C(4) H(4) 111.7 ? ? ? no H(3) C(4) H(5) 110.2 ? ? ? no H(4) C(4) H(5) 101.5 ? ? ? no S(2) C(5) N(3) 129(1) ? ? ? yes S(2) C(5) N(4) 125(2) ? ? ? yes N(3) C(5) N(4) 104(2) ? ? ? yes N(3) C(6) C(7) 108(2) ? ? ? yes N(3) C(6) H(6) 130.8 ? ? ? no C(7) C(6) H(6) 120.9 ? ? ? no N(4) C(7) C(6) 106(2) ? ? ? yes N(4) C(7) H(7) 124.3 ? ? ? no C(6) C(7) H(7) 128.7 ? ? ? no N(4) C(8) H(8) 119.2 ? ? ? no N(4) C(8) H(9) 113.7 ? ? ? no N(4) C(8) H(10) 113.6 ? ? ? no H(8) C(8) H(9) 103.9 ? ? ? no H(8) C(8) H(10) 105.1 ? ? ? no H(9) C(8) H(10) 99.0 ? ? ? no Cl(1) C(9) Cl(2) 112(1) ? ? ? yes Cl(1) C(9) H(11) 113.3 ? ? ? no Cl(1) C(9) H(12) 114.7 ? ? ? no Cl(2) C(9) H(11) 105.3 ? ? ? no Cl(2) C(9) H(12) 107.8 ? ? ? no H(11) C(9) H(12) 102.7 ? ? ? no N(1) B(1) N(1) 111.3(8) ? ? ? yes N(1) B(1) N(1) 111(1) ? ? ? yes N(1) B(1) N(1) 111.3(8) ? ? ? yes N(3) B(2) N(3) 109.7(8) ? ? ? yes N(3) B(2) N(3) 109.7(8) ? ? ? yes N(3) B(2) N(3) 109(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_[Tl(Tm)2]+[TlI4]- #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 3 13:43:22 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993) ' _computing_publication_material 'SHELXL-93, (Sheldrick, 1993)' #------------------------------------------------------------------------------ _cell_length_a 10.468(2) _cell_length_b 10.543(2) _cell_length_c 10.620(2) _cell_angle_alpha 87.41(2) _cell_angle_beta 88.53(1) _cell_angle_gamma 86.64(1) _cell_volume 1168.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 203.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.3 _cell_measurement_theta_max 29.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 2.300 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 809.47 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 B I2 N6 S3 Tl ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 740.00 _exptl_absorpt_coefficient_mu 9.819 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.587 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 203.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -5.64 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5392 _reflns_number_total 5107 _reflns_number_observed 4212 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 1.97 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.09450 _diffrn_orient_matrix_UB_12 -0.01234 _diffrn_orient_matrix_UB_13 0.01145 _diffrn_orient_matrix_UB_21 0.01179 _diffrn_orient_matrix_UB_22 0.08604 _diffrn_orient_matrix_UB_23 -0.04070 _diffrn_orient_matrix_UB_31 -0.00961 _diffrn_orient_matrix_UB_32 0.03858 _diffrn_orient_matrix_UB_33 0.08427 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 24 0.003 0.002 'International Tables' H 0 32 0.000 0.000 'International Tables' B 0 2 0.001 0.001 'International Tables' I 0 4 -0.474 1.812 'International Tables' N 0 12 0.006 0.003 'International Tables' S 0 6 0.125 0.123 'International Tables' Tl 0 2 -2.836 9.669 'International Tables' #------------------------------------------------------------------------------ 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tl1 Tl 0.0000 0.0000 0.0000 0.0420(2) Uani 1 d S . Tl2 Tl 0.4598(3) 0.4136(3) 0.4166(3) 0.1357(11) Uani 0.50 d P . I1 I 0.55285(15) 0.5668(2) 0.58374(14) 0.0290(3) Uani 0.50 d P . I2 I 0.53777(12) 0.18273(12) 0.45049(12) 0.0476(3) Uani 0.50 d P . I3 I 0.53401(15) 0.50675(14) 0.1789(2) 0.0718(5) Uani 0.50 d P . I4 I 0.18436(11) 0.43331(12) 0.45840(12) 0.0495(3) Uani 0.50 d P . S1 S 0.2083(2) -0.1308(3) -0.0844(2) 0.0589(7) Uani 1 d . . S2 S -0.0879(2) -0.2024(3) 0.1289(2) 0.0511(6) Uani 1 d . . S3 S 0.1212(2) 0.0760(3) 0.2000(2) 0.0488(5) Uani 1 d . . N1 N 0.2014(7) -0.3167(9) 0.1081(8) 0.054(2) Uani 1 d . . N2 N 0.1603(9) -0.3826(12) -0.0761(10) 0.074(3) Uani 1 d . . N3 N 0.1029(7) -0.2135(8) 0.3060(7) 0.045(2) Uani 1 d . . N4 N -0.0866(8) -0.1540(10) 0.3773(8) 0.066(3) Uani 1 d . . N5 N 0.3056(7) -0.1258(9) 0.2004(7) 0.051(2) Uani 1 d . . N6 N 0.3779(8) 0.0614(9) 0.1548(7) 0.054(2) Uani 1 d . . C1 C 0.1880(8) -0.2767(11) -0.0140(10) 0.056(3) Uani 1 d . . C2 C 0.1807(10) -0.4454(11) 0.1195(12) 0.064(3) Uani 1 d . . C3 C 0.1524(12) -0.4839(13) 0.0030(13) 0.073(3) Uani 1 d . . C4 C 0.1344(14) -0.3792(17) -0.2132(12) 0.094(5) Uani 1 d . . C5 C -0.0205(9) -0.1900(10) 0.2726(8) 0.049(2) Uani 1 d . . C6 C 0.1095(11) -0.1930(12) 0.4347(9) 0.061(3) Uani 1 d . . C7 C -0.0050(12) -0.1554(14) 0.4781(9) 0.075(4) Uani 1 d . . C8 C -0.2246(12) -0.1164(18) 0.3821(12) 0.096(5) Uani 1 d . . C9 C 0.2685(9) -0.0014(10) 0.1850(8) 0.046(2) Uani 1 d . . C10 C 0.4381(9) -0.1411(12) 0.1823(10) 0.058(3) Uani 1 d . . C11 C 0.4806(9) -0.0261(13) 0.1529(10) 0.062(3) Uani 1 d . . C12 C 0.3809(11) 0.1949(12) 0.1275(12) 0.067(3) Uani 1 d . . B1 B 0.2272(10) -0.2439(12) 0.2275(11) 0.049(2) Uani 1 d . . H1 H 0.2923 -0.2912 0.2798 0.080 Uiso 1 d . . H2 H 0.1919 -0.4964 0.1957 0.083 Uiso 1 d . . H3 H 0.1215 -0.5782 -0.0185 0.100 Uiso 1 d . . H4 H 0.1480 -0.3000 -0.2453 0.133 Uiso 1 d . . H5 H 0.1889 -0.4435 -0.2514 0.133 Uiso 1 d . . H6 H 0.0470 -0.4012 -0.2235 0.133 Uiso 1 d . . H7 H 0.1874 -0.1986 0.4874 0.086 Uiso 1 d . . H8 H -0.0274 -0.1315 0.5627 0.095 Uiso 1 d . . H9 H -0.2532 -0.0959 0.4600 0.111 Uiso 1 d . . H10 H -0.2405 -0.0453 0.3211 0.111 Uiso 1 d . . H11 H -0.2714 -0.1857 0.3510 0.111 Uiso 1 d . . H12 H 0.4876 -0.2164 0.1910 0.076 Uiso 1 d . . H13 H 0.5700 -0.0066 0.1209 0.078 Uiso 1 d . . H14 H 0.4665 0.2221 0.0999 0.094 Uiso 1 d . . H15 H 0.3296 0.2212 0.0474 0.094 Uiso 1 d . . H16 H 0.3483 0.2488 0.1878 0.094 Uiso 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 0.0320(2) 0.0662(3) 0.0299(2) -0.0100(2) 0.0026(2) -0.0168(2) Tl2 0.130(2) 0.127(2) 0.159(2) -0.0472(15) -0.035(2) -0.0398(15) I1 0.0230(5) 0.0295(5) 0.0341(6) 0.0005(5) 0.0006(5) -0.0001(4) I2 0.0407(6) 0.0495(6) 0.0520(7) -0.0015(5) -0.0081(5) 0.0054(5) I3 0.0605(9) 0.0554(8) 0.0933(11) 0.0213(7) 0.0365(8) 0.0152(7) I4 0.0390(6) 0.0538(7) 0.0535(7) 0.0114(5) 0.0076(5) 0.0019(5) S1 0.0363(12) 0.104(2) 0.0402(12) -0.0242(13) 0.0103(9) -0.0222(13) S2 0.0374(11) 0.077(2) 0.0413(11) -0.0033(11) 0.0019(9) -0.0202(11) S3 0.0424(12) 0.072(2) 0.0343(10) -0.0197(10) 0.0012(9) -0.0090(11) N1 0.032(4) 0.075(6) 0.057(5) -0.030(4) 0.006(3) -0.008(4) N2 0.043(5) 0.116(9) 0.068(6) -0.053(6) 0.011(4) -0.027(5) N3 0.040(4) 0.064(5) 0.032(3) -0.013(3) 0.001(3) -0.003(3) N4 0.046(5) 0.104(7) 0.044(4) 0.006(5) 0.015(4) 0.016(5) N5 0.034(4) 0.084(6) 0.038(4) -0.025(4) -0.001(3) -0.013(4) N6 0.040(4) 0.080(6) 0.045(4) -0.020(4) -0.001(3) -0.018(4) C1 0.027(4) 0.091(8) 0.055(6) -0.040(5) 0.010(4) -0.015(4) C2 0.036(5) 0.075(7) 0.085(8) -0.032(6) 0.010(5) -0.014(5) C3 0.055(7) 0.084(9) 0.085(9) -0.042(7) 0.002(6) -0.016(6) C4 0.080(9) 0.159(14) 0.053(7) -0.056(8) 0.010(6) -0.050(9) C5 0.042(5) 0.073(6) 0.033(4) 0.001(4) 0.009(4) -0.005(4) C6 0.066(7) 0.083(8) 0.033(5) -0.003(5) 0.001(4) 0.012(6) C7 0.072(8) 0.119(11) 0.030(5) 0.001(6) -0.004(5) 0.021(7) C8 0.052(7) 0.174(15) 0.054(7) 0.015(8) 0.023(6) 0.032(8) C9 0.042(5) 0.066(6) 0.033(4) -0.021(4) -0.001(4) -0.016(4) C10 0.031(4) 0.094(8) 0.051(5) -0.028(5) -0.006(4) -0.003(5) C11 0.029(5) 0.104(9) 0.056(6) -0.019(6) -0.005(4) -0.016(5) C12 0.057(6) 0.073(7) 0.073(7) -0.018(6) 0.006(5) -0.026(6) B1 0.036(5) 0.063(6) 0.048(6) -0.017(5) -0.002(4) -0.002(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+8.0539P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_number_reflns 5107 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_obs 0.0.0542 _refine_ls_wR_factor_all 0.1410 _refine_ls_wR_factor_obs 0.1328 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.088 _refine_ls_shift/esd_max 0.016 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_min -1.764 _refine_diff_density_max 4.224 _refine_diff_density_rms 0.176 #------------------------------------------------------------------------------ _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_1 _geom_bond_site_symmetry_2 Tl1 S1 2.668(3) . ? Tl1 S1 2.668(3) 2 ? Tl1 S2 2.679(3) 2 ? Tl1 S2 2.679(3) . ? Tl1 S3 2.679(2) . ? Tl1 S3 2.679(2) 2 ? Tl2 I2 2.534(3) . ? Tl2 I1 2.690(2) . ? Tl2 I3 2.776(3) . ? Tl2 I4 2.903(3) . ? S1 C1 1.702(13) . ? S2 C5 1.711(10) . ? S3 C9 1.709(10) . ? N1 C1 1.354(14) . ? N1 C2 1.385(14) . ? N1 B1 1.550(13) . ? N2 C3 1.33(2) . ? N2 C1 1.371(13) . ? N2 C4 1.49(2) . ? N3 C5 1.354(12) . ? N3 C6 1.398(11) . ? N3 B1 1.553(13) . ? N4 C5 1.351(12) . ? N4 C7 1.386(14) . ? N4 C8 1.476(14) . ? N5 C9 1.349(13) . ? N5 C10 1.397(12) . ? N5 B1 1.543(15) . ? N6 C11 1.375(14) . ? N6 C9 1.379(12) . ? N6 C12 1.427(15) . ? C2 C3 1.36(2) . ? C6 C7 1.32(2) . ? C10 C11 1.34(2) . ? #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 S1 Tl1 S1 180.0 . 2 ? S1 Tl1 S2 86.87(9) . 2 ? S1 Tl1 S2 93.13(9) 2 2 ? S1 Tl1 S2 93.13(9) . . ? S1 Tl1 S2 86.87(9) 2 . ? S2 Tl1 S2 180.0 2 . ? S1 Tl1 S3 92.53(7) . . ? S1 Tl1 S3 87.47(7) 2 . ? S2 Tl1 S3 87.35(8) 2 . ? S2 Tl1 S3 92.65(8) . . ? S1 Tl1 S3 87.47(7) . 2 ? S1 Tl1 S3 92.53(7) 2 2 ? S2 Tl1 S3 92.65(8) 2 2 ? S2 Tl1 S3 87.35(8) . 2 ? S3 Tl1 S3 180.0 . 2 ? I2 Tl2 I1 113.17(10) . . ? I2 Tl2 I3 110.64(11) . . ? I1 Tl2 I3 106.67(9) . . ? I2 Tl2 I4 108.54(11) . . ? I1 Tl2 I4 104.97(9) . . ? I3 Tl2 I4 112.77(11) . . ? C1 S1 Tl1 101.1(3) . . ? C5 S2 Tl1 101.5(3) . . ? C9 S3 Tl1 102.2(3) . . ? C1 N1 C2 108.8(9) . . ? C1 N1 B1 131.6(9) . . ? C2 N1 B1 119.5(9) . . ? C3 N2 C1 111.5(10) . . ? C3 N2 C4 125.6(11) . . ? C1 N2 C4 122.8(13) . . ? C5 N3 C6 107.5(8) . . ? C5 N3 B1 132.1(8) . . ? C6 N3 B1 120.0(8) . . ? C5 N4 C7 109.9(9) . . ? C5 N4 C8 124.8(10) . . ? C7 N4 C8 125.3(10) . . ? C9 N5 C10 109.3(9) . . ? C9 N5 B1 131.1(8) . . ? C10 N5 B1 119.5(9) . . ? C11 N6 C9 108.8(9) . . ? C11 N6 C12 126.6(9) . . ? C9 N6 C12 124.7(9) . . ? N1 C1 N2 105.4(11) . . ? N1 C1 S1 129.7(7) . . ? N2 C1 S1 124.8(9) . . ? C3 C2 N1 107.7(12) . . ? N2 C3 C2 106.6(11) . . ? N4 C5 N3 106.9(8) . . ? N4 C5 S2 124.0(8) . . ? N3 C5 S2 129.1(7) . . ? C7 C6 N3 109.2(9) . . ? C6 C7 N4 106.5(9) . . ? N5 C9 N6 106.4(8) . . ? N5 C9 S3 131.0(7) . . ? N6 C9 S3 122.6(8) . . ? C11 C10 N5 107.2(10) . . ? C10 C11 N6 108.4(9) . . ? N5 B1 N1 113.6(8) . . ? N5 B1 N3 112.5(8) . . ? N1 B1 N3 112.2(8) . . ? #------------------------------------------------------------------------------