# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Charles L. B. Macdonald' 'Christopher G. Andrews' 'Andrea M. Corrente' 'Bobby D. Ellis' 'Alexis Taylor' _publ_contact_author_name 'Prof Charles L. B. Macdonald' _publ_contact_author_address ; Dept. Chemistry and Biochemistry University of Windsor 401 Sunset Ave. Windsor Ontario N9B 3P4 CANADA ; _publ_contact_author_email CMACD@UWINDSOR.CA _publ_requested_journal 'Chemical Communications' _publ_section_title ; Indium (I) trifluoromethanesulfonate and other soluble salts for univalent indium chemistry ; data_p1b _database_code_depnum_ccdc_archive 'CCDC 222071' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Charles L.B. Macdonald et al. Submitted to Chem. Commun. Oct 2003 e-mail cmacd@uwindsor.ca ; _chemical_name_common 'indium(I) trifluoromethanesulfonate' _chemical_melting_point 162-165 _chemical_formula_moiety [In][CF3O3S] _chemical_formula_sum 'C H0 F3 In O3 S' _chemical_formula_weight 263.89 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' In In -0.7276 1.3100 '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 4.8934(4) _cell_length_b 7.2298(6) _cell_length_c 16.9499(15) _cell_angle_alpha 91.011(2) _cell_angle_beta 93.835(2) _cell_angle_gamma 101.711(2) _cell_volume 585.56(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4910 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.51 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.993 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 4.389 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; crystals were coated in Nujol and placed rapidly in the N2 cold stream ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5324 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2619 _reflns_number_gt 2504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0150P)^2^+8.0836P] 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 2619 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.314 _refine_ls_restrained_S_all 1.314 _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 C11 C 0.376(2) 0.2872(14) 0.8287(5) 0.034(2) Uani 1 1 d . . . C21 C 0.476(2) 0.8050(13) 0.6754(6) 0.034(2) Uani 1 1 d . . . O11 O 0.2155(13) 0.0995(9) 0.9509(4) 0.0306(13) Uani 1 1 d . . . O12 O 0.5709(14) 0.0012(9) 0.8772(4) 0.0354(15) Uani 1 1 d . . . O13 O 0.6832(13) 0.2909(9) 0.9591(4) 0.0331(14) Uani 1 1 d . . . O21 O 0.6981(13) 0.7971(9) 0.5413(4) 0.0332(14) Uani 1 1 d . . . O22 O 0.2360(13) 0.6083(9) 0.5526(4) 0.0315(14) Uani 1 1 d . . . O23 O 0.6310(15) 0.5129(10) 0.6201(4) 0.0377(15) Uani 1 1 d . . . F11 F 0.1726(14) 0.1790(10) 0.7836(4) 0.0509(16) Uani 1 1 d . . . F12 F 0.5902(15) 0.3469(10) 0.7873(4) 0.0541(17) Uani 1 1 d . . . F13 F 0.2818(15) 0.4364(9) 0.8535(4) 0.0496(16) Uani 1 1 d . . . F21 F 0.3712(16) 0.9532(9) 0.6544(4) 0.0556(18) Uani 1 1 d . . . F22 F 0.3019(14) 0.7017(9) 0.7221(4) 0.0506(16) Uani 1 1 d . . . F23 F 0.7183(15) 0.8667(11) 0.7150(4) 0.0605(19) Uani 1 1 d . . . S1 S 0.4776(4) 0.1567(3) 0.91276(12) 0.0230(4) Uani 1 1 d . . . S2 S 0.5192(4) 0.6670(3) 0.58799(12) 0.0243(4) Uani 1 1 d . . . In1 In 0.08540(14) 0.24303(9) 0.08002(4) 0.03195(19) Uani 1 1 d . . . In2 In 0.04859(14) 0.73519(9) 0.42230(4) 0.03266(19) 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 C11 0.043(5) 0.035(5) 0.027(4) 0.006(4) 0.005(4) 0.012(4) C21 0.037(5) 0.032(5) 0.033(5) -0.005(4) 0.007(4) 0.007(4) O11 0.027(3) 0.032(3) 0.033(3) 0.003(3) 0.009(3) 0.004(3) O12 0.040(4) 0.031(3) 0.040(4) -0.003(3) 0.001(3) 0.020(3) O13 0.032(3) 0.028(3) 0.036(3) -0.001(3) -0.006(3) 0.001(3) O21 0.035(3) 0.030(3) 0.034(3) -0.002(3) 0.014(3) 0.002(3) O22 0.027(3) 0.037(4) 0.028(3) -0.002(3) 0.000(2) 0.003(3) O23 0.044(4) 0.039(4) 0.037(4) 0.006(3) 0.007(3) 0.024(3) F11 0.056(4) 0.057(4) 0.037(3) -0.004(3) -0.024(3) 0.013(3) F12 0.061(4) 0.064(4) 0.040(3) 0.026(3) 0.019(3) 0.014(3) F13 0.065(4) 0.035(3) 0.056(4) 0.009(3) 0.002(3) 0.028(3) F21 0.077(5) 0.033(3) 0.066(4) -0.002(3) 0.020(4) 0.027(3) F22 0.059(4) 0.048(4) 0.044(3) -0.005(3) 0.026(3) 0.002(3) F23 0.053(4) 0.074(5) 0.046(4) -0.029(3) 0.000(3) -0.004(3) S1 0.0227(9) 0.0227(9) 0.0239(9) 0.0020(7) 0.0010(7) 0.0055(7) S2 0.0236(9) 0.0244(10) 0.0251(9) -0.0012(8) 0.0025(8) 0.0055(7) In1 0.0336(4) 0.0262(3) 0.0358(4) -0.0060(3) -0.0002(3) 0.0070(3) In2 0.0351(4) 0.0277(3) 0.0356(4) 0.0074(3) 0.0037(3) 0.0064(3) _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 C11 F12 1.304(11) . ? C11 F11 1.322(11) . ? C11 F13 1.328(11) . ? C11 S1 1.820(9) . ? C21 F23 1.313(12) . ? C21 F21 1.323(11) . ? C21 F22 1.328(11) . ? C21 S2 1.819(9) . ? O11 S1 1.462(6) . ? O11 In1 2.579(6) 1_556 ? O12 S1 1.434(6) . ? O13 S1 1.428(6) . ? O21 S2 1.436(6) . ? O22 S2 1.450(6) . ? O22 In2 2.589(6) . ? O23 S2 1.437(7) . ? In1 O11 2.579(6) 1_554 ? 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 F12 C11 F11 110.0(8) . . ? F12 C11 F13 108.3(8) . . ? F11 C11 F13 107.8(8) . . ? F12 C11 S1 110.4(7) . . ? F11 C11 S1 110.2(7) . . ? F13 C11 S1 110.2(6) . . ? F23 C21 F21 108.1(8) . . ? F23 C21 F22 109.3(8) . . ? F21 C21 F22 108.2(8) . . ? F23 C21 S2 110.5(7) . . ? F21 C21 S2 110.1(7) . . ? F22 C21 S2 110.6(6) . . ? S1 O11 In1 126.4(4) . 1_556 ? S2 O22 In2 124.7(4) . . ? O13 S1 O12 116.8(4) . . ? O13 S1 O11 113.4(4) . . ? O12 S1 O11 113.2(4) . . ? O13 S1 C11 104.8(4) . . ? O12 S1 C11 103.8(4) . . ? O11 S1 C11 102.8(4) . . ? O21 S2 O23 116.9(4) . . ? O21 S2 O22 113.6(4) . . ? O23 S2 O22 113.0(4) . . ? O21 S2 C21 104.7(4) . . ? O23 S2 C21 103.4(4) . . ? O22 S2 C21 103.3(4) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.185 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.196