# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Cooper, Benjamin' 'Macdonald, Charles' _publ_contact_author_name 'Macdonald, Charles' _publ_contact_author_email cmacd@uwindsor.ca _publ_section_title ; Alternative syntheses of univalent indium salts including a direct route from indium metal ; # Attachment '- In-TFA_18cr6.cif' data_p21m _database_code_depnum_ccdc_archive 'CCDC 762390' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 O6, C2 F3 In O2' _chemical_formula_sum 'C14 H24 F3 In O8' _chemical_formula_weight 492.15 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.100(3) _cell_length_b 11.571(3) _cell_length_c 9.634(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.692(3) _cell_angle_gamma 90.00 _cell_volume 976.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2880 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.72 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 1.274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details 'SADABS; Bruker, 2001' _exptl_special_details ; ? ; _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 10655 _diffrn_reflns_av_R_equivalents 0.1133 _diffrn_reflns_av_sigmaI/netI 0.1108 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2303 _reflns_number_gt 1556 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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. ; _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^)+(0.0473P)^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 2303 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 C1 C -0.2418(8) 0.2500 0.4876(8) 0.0268(16) Uani 1 2 d S . . C2 C -0.4095(9) 0.2500 0.4031(8) 0.056(3) Uani 1 2 d S . . C21 C 0.1924(6) 0.1483(5) 0.6219(6) 0.0413(14) Uani 1 1 d . . . H21A H 0.2941 0.1440 0.6033 0.050 Uiso 1 1 calc R . . H21B H 0.1140 0.1502 0.5280 0.050 Uiso 1 1 calc R . . C22 C 0.1684(6) 0.0446(5) 0.7062(6) 0.0448(15) Uani 1 1 d . . . H22A H 0.1925 -0.0268 0.6602 0.054 Uiso 1 1 calc R . . H22B H 0.2363 0.0486 0.8055 0.054 Uiso 1 1 calc R . . C23 C -0.0211(6) -0.0564(4) 0.7832(5) 0.0364(13) Uani 1 1 d . . . H23A H 0.0378 -0.0542 0.8858 0.044 Uiso 1 1 calc R . . H23B H 0.0068 -0.1276 0.7394 0.044 Uiso 1 1 calc R . . C24 C -0.1869(6) -0.0565(4) 0.7715(6) 0.0374(13) Uani 1 1 d . . . H24A H -0.2454 -0.0471 0.6694 0.045 Uiso 1 1 calc R . . H24B H -0.2163 -0.1311 0.8066 0.045 Uiso 1 1 calc R . . C25 C -0.3797(6) 0.0477(5) 0.8401(6) 0.0408(14) Uani 1 1 d . . . H25A H -0.4196 -0.0236 0.8737 0.049 Uiso 1 1 calc R . . H25B H -0.4343 0.0594 0.7372 0.049 Uiso 1 1 calc R . . C26 C -0.4070(6) 0.1484(4) 0.9264(6) 0.0392(13) Uani 1 1 d . . . H26A H -0.5150 0.1497 0.9290 0.047 Uiso 1 1 calc R . . H26B H -0.3415 0.1424 1.0266 0.047 Uiso 1 1 calc R . . O1 O -0.2266(6) 0.2500 0.6174(5) 0.0534(16) Uani 1 2 d S . . O2 O -0.1498(6) 0.2500 0.4162(6) 0.0467(14) Uani 1 2 d S . . O21 O 0.1824(5) 0.2500 0.7014(5) 0.0327(12) Uani 1 2 d S . . O22 O 0.0138(4) 0.0433(3) 0.7094(4) 0.0342(8) Uani 1 1 d . . . O23 O -0.2220(4) 0.0358(3) 0.8551(3) 0.0333(8) Uani 1 1 d . . . O24 O -0.3721(5) 0.2500 0.8616(5) 0.0355(12) Uani 1 2 d S . . F1 F -0.4374(6) 0.2500 0.2629(5) 0.099(2) Uani 1 2 d S . . F2 F -0.4795(5) 0.1597(6) 0.4367(5) 0.154(3) Uani 1 1 d . . . In In -0.05223(6) 0.2500 0.83653(5) 0.02796(18) Uani 1 2 d S . . 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 C1 0.025(4) 0.015(4) 0.040(4) 0.000 0.008(3) 0.000 C2 0.029(5) 0.108(8) 0.029(4) 0.000 0.002(4) 0.000 C21 0.030(3) 0.048(4) 0.051(3) -0.009(3) 0.020(3) 0.004(3) C22 0.029(3) 0.037(3) 0.068(4) -0.013(3) 0.013(3) 0.007(3) C23 0.043(3) 0.029(3) 0.035(3) -0.007(2) 0.007(2) 0.005(3) C24 0.046(3) 0.024(3) 0.042(3) -0.002(3) 0.011(3) -0.006(3) C25 0.038(3) 0.037(3) 0.049(3) 0.001(3) 0.014(3) -0.012(3) C26 0.034(3) 0.038(3) 0.050(3) 0.002(3) 0.018(3) -0.007(3) O1 0.041(3) 0.091(5) 0.024(3) 0.000 0.000(2) 0.000 O2 0.041(3) 0.049(4) 0.059(3) 0.000 0.029(3) 0.000 O21 0.033(3) 0.035(3) 0.032(3) 0.000 0.012(2) 0.000 O22 0.0270(19) 0.033(2) 0.043(2) -0.0011(17) 0.0098(16) 0.0032(16) O23 0.029(2) 0.034(2) 0.0367(19) -0.0047(17) 0.0086(16) -0.0041(16) O24 0.037(3) 0.032(3) 0.044(3) 0.000 0.023(2) 0.000 F1 0.068(4) 0.192(7) 0.027(3) 0.000 -0.004(3) 0.000 F2 0.093(3) 0.265(7) 0.089(3) 0.019(4) -0.003(3) -0.125(4) In 0.0263(3) 0.0319(3) 0.0237(3) 0.000 0.00334(19) 0.000 _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 C1 O2 1.218(8) . ? C1 O1 1.221(8) . ? C1 C2 1.523(10) . ? C2 F1 1.305(9) . ? C2 F2 1.309(6) . ? C2 F2 1.309(6) 4_565 ? C21 O21 1.420(5) . ? C21 C22 1.497(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O22 1.416(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O22 1.435(6) . ? C23 C24 1.482(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O23 1.424(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O23 1.410(6) . ? C25 C26 1.490(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O24 1.407(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O1 In 2.272(5) . ? O21 C21 1.420(5) 4_565 ? O24 C26 1.407(5) 4_565 ? 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 C1 O1 132.4(7) . . ? O2 C1 C2 116.1(6) . . ? O1 C1 C2 111.5(6) . . ? F1 C2 F2 106.5(5) . . ? F1 C2 F2 106.5(5) . 4_565 ? F2 C2 F2 105.9(8) . 4_565 ? F1 C2 C1 116.0(7) . . ? F2 C2 C1 110.6(5) . . ? F2 C2 C1 110.6(5) 4_565 . ? O21 C21 C22 109.4(4) . . ? O21 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? O21 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? O22 C22 C21 108.2(4) . . ? O22 C22 H22A 110.1 . . ? C21 C22 H22A 110.1 . . ? O22 C22 H22B 110.1 . . ? C21 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? O22 C23 C24 108.7(4) . . ? O22 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? O22 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? O23 C24 C23 109.6(4) . . ? O23 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? O23 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? O23 C25 C26 109.7(4) . . ? O23 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? O23 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O24 C26 C25 108.3(4) . . ? O24 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O24 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? C1 O1 In 144.0(5) . . ? C21 O21 C21 111.9(5) . 4_565 ? C22 O22 C23 112.0(4) . . ? C25 O23 C24 113.1(4) . . ? C26 O24 C26 113.4(5) 4_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 F1 0.000(1) . . . . ? O1 C1 C2 F1 180.000(2) . . . . ? O2 C1 C2 F2 121.5(5) . . . . ? O1 C1 C2 F2 -58.5(5) . . . . ? O2 C1 C2 F2 -121.5(5) . . . 4_565 ? O1 C1 C2 F2 58.5(5) . . . 4_565 ? O21 C21 C22 O22 69.4(5) . . . . ? O22 C23 C24 O23 -69.2(5) . . . . ? O23 C25 C26 O24 68.8(5) . . . . ? O2 C1 O1 In 0.000(2) . . . . ? C2 C1 O1 In 180.0 . . . . ? C22 C21 O21 C21 -175.4(3) . . . 4_565 ? C21 C22 O22 C23 177.5(4) . . . . ? C24 C23 O22 C22 -175.4(4) . . . . ? C26 C25 O23 C24 -177.9(4) . . . . ? C23 C24 O23 C25 175.0(4) . . . . ? C25 C26 O24 C26 174.5(3) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.130 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.137