# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2006 data_(ET3S)I3 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Nov 2 19:04:16 1998' _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 9.894(2) _cell_length_b 13.846(3) _cell_length_c 19.856(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2719(1) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rectangular' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 2.441 _exptl_crystal_density_meas ? _chemical_formula_weight 499.96 _chemical_formula_analytical ? _chemical_formula_sum 'C6 H15 I3 S ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1808.00 _exptl_absorpt_coefficient_mu 7.003 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 0.463 _exptl_absorpt_correction_T_min 0.238 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150 _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 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count '120 min' _diffrn_standards_decay_% -10.09 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -2 2 2 0 2 3 5 5 _diffrn_reflns_number 2725 _reflns_number_total 2725 _reflns_number_observed 1320 _reflns_observed_criterion '3.00 Sigma' _diffrn_reflns_av_R_equivalents 0.00 _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 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 25 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.06457 _diffrn_orient_matrix_UB_12 -0.05349 _diffrn_orient_matrix_UB_13 -0.01048 _diffrn_orient_matrix_UB_21 -0.01194 _diffrn_orient_matrix_UB_22 0.01265 _diffrn_orient_matrix_UB_23 -0.04916 _diffrn_orient_matrix_UB_31 0.07705 _diffrn_orient_matrix_UB_32 0.04697 _diffrn_orient_matrix_UB_33 0.00127 #------------------------------------------------------------------------------ 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 I 0 24 -0.474 1.812 'International Tables' S 0 8 0.125 0.123 'International Tables' C 0 48 0.003 0.002 'International Tables' H 0 120 0.000 0.000 '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 I(1) 0.1084(3) 0.2500 -0.0488(1) 0.0269(8) Uij ? ? I(2) 0.3579(3) 0.2500 -0.1303(1) 0.0252(8) Uij ? ? I(3) 0.5857(3) 0.2500 -0.2209(1) 0.0304(9) Uij ? ? I(4) 0.3654(3) 0.2500 0.2388(2) 0.0365(9) Uij ? ? I(5) 0.5506(3) 0.2500 0.1236(1) 0.0267(8) Uij ? ? I(6) 0.7328(3) 0.2500 0.0071(1) 0.0323(9) Uij ? ? S(1) 0.1145(8) -0.0079(5) 0.0861(4) 0.028(2) Uij ? ? C(1) 0.126(2) -0.080(2) 0.160(1) 0.024(7) Uij ? ? C(2) 0.145(3) -0.028(2) 0.225(2) 0.051(10) Uij ? ? C(3) -0.017(3) 0.078(2) 0.111(1) 0.028(7) Uij ? ? C(4) -0.155(3) 0.032(2) 0.120(2) 0.044(9) Uij ? ? C(5) 0.262(3) 0.064(2) 0.087(2) 0.040(8) Uij ? ? C(6) 0.392(4) -0.001(2) 0.079(2) 0.06(1) Uij ? ? H(1) 0.1556 -0.0724 0.2640 0.0253 Uij ? ? H(2) 0.2279 0.0109 0.2261 0.0253 Uij ? ? H(3) 0.0723 0.0135 0.2356 0.0253 Uij ? ? H(4) -0.2217 0.0805 0.1310 0.0253 Uij ? ? H(5) -0.1820 0.0078 0.0749 0.0253 Uij ? ? H(6) -0.1546 -0.0171 0.1499 0.0253 Uij ? ? H(7) 0.3926 -0.0480 0.1127 0.0253 Uij ? ? H(8) 0.3820 -0.0347 0.0353 0.0253 Uij ? ? H(9) 0.4708 0.0350 0.0775 0.0253 Uij ? ? H(10) 0.0501 -0.1211 0.1633 0.0253 Uij ? ? H(11) 0.2057 -0.1237 0.1538 0.0253 Uij ? ? H(12) 0.0089 0.1067 0.1552 0.0253 Uij ? ? H(13) -0.0187 0.1320 0.0803 0.0253 Uij ? ? H(14) 0.2622 0.1125 0.0517 0.0253 Uij ? ? H(15) 0.2727 0.0991 0.1291 0.0253 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 I(1) 0.034(2) 0.029(1) 0.018(2) 0.0000 0.007(2) 0.0000 I(2) 0.029(2) 0.028(2) 0.018(1) 0.0000 -0.006(1) 0.0000 I(3) 0.027(2) 0.038(2) 0.026(2) 0.0000 0.000(1) 0.0000 I(4) 0.047(2) 0.034(2) 0.028(2) 0.0000 0.001(2) 0.0000 I(5) 0.027(2) 0.020(1) 0.033(2) 0.0000 -0.003(1) 0.0000 I(6) 0.038(2) 0.032(2) 0.027(2) 0.0000 0.003(2) 0.0000 S(1) 0.034(4) 0.025(4) 0.024(4) -0.001(4) -0.005(4) 0.0001(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.25885E-7 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1320 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0662 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0735 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.559 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -2.24 _refine_diff_density_max 2.68 #------------------------------------------------------------------------------ _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 I1 I2 2.951(4) ? ? yes I2 I3 2.884(4) ? ? yes I4 I5 2.930(4) ? ? yes I5 I6 2.932(4) ? ? yes S1 C1 1.77(3) ? ? yes S1 C3 1.83(3) ? ? yes S1 C5 1.76(3) ? ? yes C1 C2 1.50(4) ? ? yes C3 C4 1.52(4) ? ? yes C5 C6 1.57(4) ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 I2 I3 174.6(1) ? ? ? yes I4 I5 I6 179.2(1) ? ? ? yes C1 S1 C3 101(1) ? ? ? yes C1 S1 C5 104(1) ? ? ? yes C3 S1 C5 102(1) ? ? ? yes S1 C1 C2 116(1) ? ? ? yes S1 C3 C4 113(1) ? ? ? yes S1 C5 C6 111(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc. Dalton. Trans.' _publ_contact_author ; Prof. Lars Kloo Inorganic Chemistry, Department of Chemistry, Royal Institute of Chemistry, S-1044 Stockholm, Sweden ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' +46-8-7909349 ' _publ_contact_author_email ' Larsa@inorg.kth.se' loop_ _publ_author_name _publ_author_address ' Lars Kloo' ; Inorganic Chemistry, Department of Chemistry, Royal Institute of Chemistry, S-1044 Stockholm, Sweden ; 'Svensson, Per H.' ; Viale Risorgimento 4, I-40136 Bologna, Italy Fax: {051-6443690} E-mail: {pers@ms.fci.unibo.it} ; _publ_section_title ; A Vibrational Spectroscopic, Structural and Quantum Chemical Study of the Triiodide Ion ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ; _publ_section_references ; ENTER OTHER REFERENCES ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_Me3SI5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H9 I5 S' _chemical_formula_weight 711.66 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ama2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y, z' '-x+1/2, y, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.841(2) _cell_length_b 9.3342(11) _cell_length_c 9.363(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1384.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description 'cubic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.415 _exptl_crystal_density_method ? _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 11.333 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_correction_T_max 0.322 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '120' _diffrn_standards_decay_% ? _diffrn_reflns_number 585 _diffrn_reflns_av_R_equivalents 0.1195 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 18.72 _reflns_number_total 308 _reflns_number_observed 305 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0629P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.30(40) _refine_ls_number_reflns 308 _refine_ls_number_parameters 40 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_obs 0.0455 _refine_ls_wR_factor_all 0.1168 _refine_ls_wR_factor_obs 0.1160 _refine_ls_goodness_of_fit_all 1.202 _refine_ls_goodness_of_fit_obs 1.200 _refine_ls_restrained_S_all 1.199 _refine_ls_restrained_S_obs 1.198 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group I1 I 0.7500 0.4359(3) 0.9403(3) 0.0163(13) Uani 1 d S . I2 I 0.61423(11) 0.1054(2) 0.6177(2) 0.0156(11) Uani 1 d . . I3 I 0.5083(2) 0.2621(2) 0.7960(3) 0.0236(12) Uani 1 d . . S1 S 0.7500 1.0373(20) 0.9352(27) 0.017(9) Uiso 0.60(4) d SP . S2 S 0.7500 0.9130(23) 1.0530(33) 0.004(11) Uiso 0.40(4) d SP . C1 C 0.7500 0.8582(58) 0.8718(54) 0.033(14) Uiso 1 d S . C2 C 0.6601(25) 1.0415(34) 1.0519(41) 0.041(10) 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 I1 0.014(2) 0.020(2) 0.015(2) 0.001(2) 0.000 0.000 I2 0.010(2) 0.0182(14) 0.018(2) 0.0078(10) -0.0012(12) -0.0015(7) I3 0.014(2) 0.025(2) 0.032(2) -0.0051(10) -0.0003(13) 0.0047(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 I1 I2 3.144(3) 5 ? I1 I2 3.144(3) 8_655 ? I2 I3 2.783(3) . ? I2 I1 3.144(3) 5_544 ? S1 S2 1.60(4) . ? S1 C1 1.77(6) . ? S1 C2 1.80(4) 4_655 ? S1 C2 1.80(4) . ? S2 C1 1.77(6) . ? S2 C2 1.86(4) 4_655 ? S2 C2 1.86(4) . ? 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 I2 I1 I2 86.33(10) 5 8_655 ? I3 I2 I1 173.67(10) . 5_544 ? S2 S1 C1 63.1(19) . . ? S2 S1 C2 66.2(14) . 4_655 ? C1 S1 C2 103.0(17) . 4_655 ? S2 S1 C2 66.2(14) . . ? C1 S1 C2 103.0(17) . . ? C2 S1 C2 105.0(27) 4_655 . ? S1 S2 C1 63.2(23) . . ? S1 S2 C2 61.9(13) . 4_655 ? C1 S2 C2 100.4(21) . 4_655 ? S1 S2 C2 61.9(13) . . ? C1 S2 C2 100.4(21) . . ? C2 S2 C2 99.8(23) 4_655 . ? S2 C1 S1 53.6(20) . . ? S1 C2 S2 51.8(17) . . ? _refine_diff_density_max 1.430 _refine_diff_density_min -1.283 _refine_diff_density_rms 0.366 #------------------------------------------------------------------------------ __publ_requested_journal 'J. Chem. Soc. Dalton. Trans.' _publ_contact_author ; Prof. Lars Kloo Inorganic Chemistry, Department of Chemistry, Royal Institute of Chemistry, S-1044 Stockholm, Sweden ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' +46-8-7909349 ' _publ_contact_author_email ' Larsa@inorg.kth.se' loop_ _publ_author_name _publ_author_address ' Lars Kloo' ; Inorganic Chemistry, Department of Chemistry, Royal Institute of Chemistry, S-1044 Stockholm, Sweden ; 'Svensson, Per H.' ; Viale Risorgimento 4, I-40136 Bologna, Italy Fax: {051-6443690} E-mail: {pers@ms.fci.unibo.it} ; _publ_section_title ; A Vibrational Spectroscopic, Structural and Quantum Chemical Study of the Triiodide Ion ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ; _publ_section_references ; ENTER OTHER REFERENCES ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_(Me3S)IBr2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H9 Br2 I S' _chemical_formula_weight 363.88 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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 15.0570(8) _cell_length_b 9.7571(5) _cell_length_c 14.9825(8) _cell_angle_alpha 90.00 _cell_angle_beta 115.99 _cell_angle_gamma 90.00 _cell_volume 1978.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5033 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 60.0 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.443 _exptl_crystal_density_method ? _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 11.444 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.055 _exptl_absorpt_correction_T_max 0.226 _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 'Siemens Smart CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5978 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1942 _reflns_number_observed 1454 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 98 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^)+(0.0501P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1844 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_obs 0.0397 _refine_ls_wR_factor_all 0.0994 _refine_ls_wR_factor_obs 0.0913 _refine_ls_goodness_of_fit_all 0.998 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_restrained_S_all 0.997 _refine_ls_restrained_S_obs 1.063 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group I1 I 0.5000 0.39124(6) 0.2500 0.0674(2) Uani 1 d S . I2 I 0.0000 0.5000 0.0000 0.0658(2) Uani 1 d S . Br1 Br 0.69770(7) 0.39201(8) 0.36569(6) 0.0845(3) Uani 1 d . . Br2 Br 0.01298(6) 0.72849(8) 0.90358(6) 0.0787(3) Uani 1 d . . S1 S 0.24334(12) 0.5812(2) 0.90806(11) 0.0567(4) Uani 1 d . . C1 C 0.3476(5) 0.4881(7) 0.9143(6) 0.074(2) Uani 1 d . . H1A H 0.3525(5) 0.4026(7) 0.9478(6) 0.111 Uiso 1 calc R . H1B H 0.4065(5) 0.5409(7) 0.9501(6) 0.111 Uiso 1 calc R . H1C H 0.3401(5) 0.4707(7) 0.8483(6) 0.111 Uiso 1 calc R . C2 C 0.2455(6) 0.7334(6) 0.8450(5) 0.075(2) Uani 1 d . . H2A H 0.2957(6) 0.7935(6) 0.8898(5) 0.112 Uiso 1 calc R . H2B H 0.1824(6) 0.7779(6) 0.8209(5) 0.112 Uiso 1 calc R . H2C H 0.2596(6) 0.7114(6) 0.7901(5) 0.112 Uiso 1 calc R . C3 C 0.1470(5) 0.4889(7) 0.8121(8) 0.100(3) Uani 1 d . . H3A H 0.1382(5) 0.4021(7) 0.8373(8) 0.150 Uiso 1 calc R . H3B H 0.1640(5) 0.4741(7) 0.7581(8) 0.150 Uiso 1 calc R . H3C H 0.0868(5) 0.5406(7) 0.7889(8) 0.150 Uiso 1 calc R . 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 I1 0.1045(5) 0.0390(3) 0.0826(4) 0.000 0.0632(4) 0.000 I2 0.0461(3) 0.0699(4) 0.0681(4) -0.0131(3) 0.0127(3) 0.0054(3) Br1 0.1046(6) 0.0674(5) 0.0903(5) -0.0267(4) 0.0510(5) -0.0207(4) Br2 0.0713(5) 0.0663(5) 0.0903(5) -0.0034(4) 0.0278(4) 0.0087(4) S1 0.0651(10) 0.0512(9) 0.0592(9) 0.0079(7) 0.0321(8) 0.0168(7) C1 0.058(4) 0.075(5) 0.090(5) 0.006(4) 0.033(4) 0.021(3) C2 0.102(6) 0.044(4) 0.077(4) 0.000(3) 0.038(4) 0.002(4) C3 0.062(5) 0.043(4) 0.163(9) -0.018(5) 0.020(5) -0.005(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 I1 Br1 2.7098(9) . ? I1 Br1 2.7098(9) 2_655 ? I2 Br2 2.7098(8) 1_554 ? I2 Br2 2.7098(8) 5_566 ? Br2 I2 2.7098(8) 1_556 ? S1 C2 1.768(6) . ? S1 C3 1.776(8) . ? S1 C1 1.781(6) . ? 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 Br1 I1 Br1 179.68(4) . 2_655 ? Br2 I2 Br2 180.0 1_554 5_566 ? C2 S1 C3 101.1(4) . . ? C2 S1 C1 103.5(4) . . ? C3 S1 C1 99.9(4) . . ? _refine_diff_density_max 0.578 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.133 #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc. Dalton. Trans.' _publ_contact_author ; Prof. Lars Kloo Inorganic Chemistry, Department of Chemistry, Royal Institute of Chemistry, S-1044 Stockholm, Sweden ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' +46-8-7909349 ' _publ_contact_author_email ' Larsa@inorg.kth.se' loop_ _publ_author_name _publ_author_address ' Lars Kloo' ; Inorganic Chemistry, Department of Chemistry, Royal Institute of Chemistry, S-1044 Stockholm, Sweden ; 'Svensson, Per H.' ; Viale Risorgimento 4, I-40136 Bologna, Italy Fax: {051-6443690} E-mail: {pers@ms.fci.unibo.it} ; _publ_section_title ; A Vibrational Spectroscopic, Structural and Quantum Chemical Study of the Triiodide Ion ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ; _publ_section_references ; ENTER OTHER REFERENCES ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;