Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Magnus Sandstrom' _publ_contact_author_address ; Prof Magnus Sandstrom Structural Chemistry Stockholm University Stockholm SE-106 91 SWEDEN ; _publ_contact_author_email MAGNUSS@STRUC.SU.SE _publ_section_title ; Dimethylsulfoxide Solvates of the Aluminium(III), Gallium(III) and Indium(III) Ions. A Crystallographic, EXAFS and Vibrational Spectroscopic Study. ; loop_ _publ_author_name _publ_author_address 'Alireza Molla-Abbassi' ; Structural Chemistry Arrhenius Laboratory Stockholm University SE-106 91 Stockholm Sweden ; 'Mikhail Skripkin' ; St. Petersburg State University Department of Chemistry Universitetskii pr. 2, 198904 St.Petersburg Russia ; 'Mikael Kritikos' ; Structural Chemistry Arrhenius Laboratory Stockholm University SE-106 91 Stockholm Sweden ; 'Ingmar Persson' ; Department of Chemistry Swedish University of Agricultural Sciences P. O. Box 7015 SE-750 07 Uppsala Sweden ; 'Janos Mink' ; Institute of Isotopes and Surface Chemistry, Chemical Research Center of the Hungarian Academy of Sciences P.O. Box 77, H-1525 Budapest and Analytical Chemistry Department University of Veszprem, P.O. 158 Hungary ; ; M.Sandstrom ; ; Structural Chemistry Arrhenius Laboratory Stockholm University SE-106 91 Stockholm Sweden ; ############################################################# data_complex1 _database_code_CSD 199307 #data_aldmso _audit_creation_date 2002-11-29 _audit_creation_method 'X-RED, SHELXL-97 ' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Al I3 O6 S6' _chemical_formula_weight 876.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.7617(11) _cell_length_b 10.7617(11) _cell_length_c 24.599(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2467.2(5) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4115 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.0 _exptl_crystal_description 'block shape' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.096 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas 1.80 _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'flotation method' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 3.279 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.534 _exptl_absorpt_correction_T_max 0.670 _exptl_absorpt_process_details ; The crystal shape and size were optimized using equivalent reflections with the program X-Shape. Absorption correction was made with the program X-Red ; _exptl_special_details ; ? ; _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 'STOE IPDS' _diffrn_measurement_method 'Area detector - phi oscillation' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7819 _diffrn_reflns_av_R_equivalents 0.1250 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.06 _reflns_number_total 1342 _reflns_number_gt 885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software, by Stoe &Cie (1997)' _computing_cell_refinement 'IPDS Software, Stoe & Cie (1997)' _computing_data_reduction 'IPDS Software, Stoe & Cie (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 2000), DIAMOND (Brandenburg, 1999)' _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_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0562P)^2^+4.2867P] 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 1342 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 Al Al 0.0000 0.0000 0.0000 0.0401(9) Uani 1 6 d S . . I1 I 0.3333 0.6667 0.1667 0.0630(4) Uani 1 6 d S . . I2 I 0.3333 0.6667 -0.08326(3) 0.0503(3) Uani 1 3 d S . . S1 S 0.09229(16) 0.26977(16) 0.06980(7) 0.0466(4) Uani 1 1 d . . . O1 O -0.0257(5) 0.1315(5) 0.04299(18) 0.0489(10) Uani 1 1 d . . . C1 C 0.0775(10) 0.4088(8) 0.0370(3) 0.0656(19) Uani 1 1 d . . . H1A H 0.1146 0.4211 0.0006 0.098 Uiso 1 1 calc R . . H1B H 0.1315 0.4967 0.0568 0.098 Uiso 1 1 calc R . . H1C H -0.0215 0.3838 0.0356 0.098 Uiso 1 1 calc R . . C2 C 0.0136(10) 0.2715(9) 0.1330(3) 0.067(2) Uani 1 1 d . . . H2A H -0.0835 0.2496 0.1273 0.101 Uiso 1 1 calc R . . H2B H 0.0676 0.3648 0.1493 0.101 Uiso 1 1 calc R . . H2C H 0.0143 0.2011 0.1568 0.101 Uiso 1 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 Al 0.0324(13) 0.0324(13) 0.056(2) 0.000 0.000 0.0162(6) I1 0.0513(4) 0.0513(4) 0.0863(8) 0.000 0.000 0.0257(2) I2 0.0521(3) 0.0521(3) 0.0466(4) 0.000 0.000 0.02605(16) S1 0.0398(8) 0.0376(8) 0.0600(9) -0.0020(7) -0.0006(7) 0.0176(7) O1 0.041(2) 0.042(2) 0.065(2) -0.0062(19) 0.0047(19) 0.0222(19) C1 0.082(5) 0.049(4) 0.064(4) 0.015(3) 0.012(4) 0.032(4) C2 0.086(6) 0.066(5) 0.045(4) 0.003(3) 0.002(3) 0.035(4) _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 Al O1 1.894(4) 3 ? Al O1 1.894(4) 11 ? Al O1 1.894(4) . ? Al O1 1.894(4) 2 ? Al O1 1.894(4) 12 ? Al O1 1.894(4) 10 ? S1 O1 1.540(5) . ? S1 C2 1.776(8) . ? S1 C1 1.776(7) . ? 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 Al O1 88.1(2) 3 11 ? O1 Al O1 91.9(2) 3 . ? O1 Al O1 88.1(2) 11 . ? O1 Al O1 91.9(2) 3 2 ? O1 Al O1 180.0(3) 11 2 ? O1 Al O1 91.9(2) . 2 ? O1 Al O1 180.0(3) 3 12 ? O1 Al O1 91.9(2) 11 12 ? O1 Al O1 88.1(2) . 12 ? O1 Al O1 88.1(2) 2 12 ? O1 Al O1 88.1(2) 3 10 ? O1 Al O1 91.9(2) 11 10 ? O1 Al O1 180.0(3) . 10 ? O1 Al O1 88.1(2) 2 10 ? O1 Al O1 91.9(2) 12 10 ? O1 S1 C2 102.6(3) . . ? O1 S1 C1 104.0(3) . . ? C2 S1 C1 98.4(4) . . ? S1 O1 Al 127.1(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.660 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.173 #end data_complex1 data_complex2 _database_code_CSD 199308 # data_gadmso _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Ga I3 O6 S6' _chemical_formula_weight 919.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.9272(13) _cell_length_b 10.9272(13) _cell_length_c 23.868(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2468.1(6) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.0 _exptl_crystal_description 'block shape' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.064 _exptl_crystal_size_min 0.064 _exptl_crystal_density_meas 1.85 _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'flotation method' _exptl_crystal_F_000 1326 _exptl_absorpt_coefficient_mu 4.052 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.509 _exptl_absorpt_correction_T_max 0.586 _exptl_absorpt_process_details ; The crystal shape and size were optimized using equivalent reflections with the program X-Shape. Absorption correction was made with the program X-Red ; _exptl_special_details ; ? ; _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 'STOE IPDS' _diffrn_measurement_method 'Area detector - phi oscillation' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6431 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.07 _reflns_number_total 1085 _reflns_number_gt 651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software, by Stoe &Cie (1997)' _computing_cell_refinement 'IPDS Software, Stoe & Cie (1997)' _computing_data_reduction 'IPDS Software, Stoe & Cie (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 2000), DIAMOND (Brandenburg, 1999)' _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^)+(0.0691P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(2) _refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1085 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Ga Ga 0.0000 0.0000 0.0000 0.0505(5) Uani 1 6 d S . . I1 I 0.3333 0.6667 0.1667 0.0733(4) Uani 1 6 d S . . I2 I 0.3333 0.6667 -0.08309(4) 0.0573(3) Uani 1 3 d S . . S1 S 0.08657(17) -0.18292(17) 0.07125(8) 0.0552(5) Uani 1 1 d . . . O1 O -0.0323(4) -0.1633(4) 0.0462(2) 0.0582(12) Uani 1 1 d . . . C1 C 0.0731(10) -0.3315(9) 0.0356(4) 0.075(2) Uani 1 1 d . . . H1A H -0.0229 -0.4076 0.0368 0.11(3) Uiso 1 1 calc R . . H1B H 0.1332 -0.3606 0.0535 0.10(3) Uiso 1 1 calc R . . H1C H 0.1018 -0.3068 -0.0026 0.08(2) Uiso 1 1 calc R . . C2 C 0.0151(10) -0.2650(10) 0.1366(3) 0.074(2) Uani 1 1 d . . . H2A H -0.0753 -0.3479 0.1307 0.08(3) Uiso 1 1 calc R . . H2B H 0.0041 -0.2003 0.1604 0.08(2) Uiso 1 1 calc R . . H2C H 0.0778 -0.2912 0.1541 0.13(4) Uiso 1 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 Ga 0.0363(5) 0.0363(5) 0.0789(12) 0.000 0.000 0.0181(3) I1 0.0563(5) 0.0563(5) 0.1071(11) 0.000 0.000 0.0282(2) I2 0.0565(4) 0.0565(4) 0.0589(5) 0.000 0.000 0.02827(19) S1 0.0426(8) 0.0459(9) 0.0802(11) 0.0012(8) 0.0010(8) 0.0245(7) O1 0.043(2) 0.045(2) 0.086(3) 0.008(2) 0.000(2) 0.0226(19) C1 0.091(6) 0.075(5) 0.082(6) 0.000(4) 0.017(5) 0.059(5) C2 0.082(6) 0.087(6) 0.068(5) -0.006(4) 0.004(4) 0.054(5) _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 Ga O1 1.974(4) 11 ? Ga O1 1.974(4) 2 ? Ga O1 1.974(4) 3 ? Ga O1 1.974(4) 10 ? Ga O1 1.974(4) . ? Ga O1 1.974(4) 12 ? S1 O1 1.539(5) . ? S1 C1 1.773(8) . ? S1 C2 1.774(8) . ? 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 Ga O1 180.0(5) 11 2 ? O1 Ga O1 88.2(2) 11 3 ? O1 Ga O1 91.8(2) 2 3 ? O1 Ga O1 91.8(2) 11 10 ? O1 Ga O1 88.2(2) 2 10 ? O1 Ga O1 88.2(2) 3 10 ? O1 Ga O1 88.2(2) 11 . ? O1 Ga O1 91.8(2) 2 . ? O1 Ga O1 91.8(2) 3 . ? O1 Ga O1 180.0(3) 10 . ? O1 Ga O1 91.8(2) 11 12 ? O1 Ga O1 88.2(2) 2 12 ? O1 Ga O1 180.0(3) 3 12 ? O1 Ga O1 91.8(2) 10 12 ? O1 Ga O1 88.2(2) . 12 ? O1 S1 C1 104.6(4) . . ? O1 S1 C2 102.9(3) . . ? C1 S1 C2 98.3(4) . . ? S1 O1 Ga 124.1(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.888 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.126 #end data_complex2 data_complex3 _database_code_CSD 199309 #data_indmso _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 I3 In O6 S6' _chemical_formula_weight 964.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 11.3584(17) _cell_length_b 11.3584(17) _cell_length_c 21.512(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2403.5(7) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.1 _exptl_crystal_description 'block shape' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 1.97 _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'flotation method' _exptl_crystal_F_000 1381 _exptl_absorpt_coefficient_mu 4.040 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.521 _exptl_absorpt_correction_T_max 0.590 _exptl_absorpt_process_details ; The crystal shape and size were optimized using equivalent reflections with the program X-Shape. Absorption correction was made with the program X-Red ; _exptl_special_details ; ? ; _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 'STOE IPDS' _diffrn_measurement_method 'Area detector - phi oscillation' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6285 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 26.16 _reflns_number_total 1059 _reflns_number_gt 579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software, by Stoe &Cie (1997)' _computing_cell_refinement 'IPDS Software, Stoe & Cie (1997)' _computing_data_reduction 'IPDS Software, Stoe & Cie (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 2000), DIAMOND (Brandenburg, 1999)' _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^)+(0.0260P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00039(5) _refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1059 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.858 _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 In In 0.0000 0.0000 0.0000 0.0358(2) Uani 1 6 d S . . I1 I 0.3333 0.6667 0.1667 0.0584(3) Uani 1 6 d S . . I2 I 0.3333 0.6667 -0.08545(3) 0.0504(2) Uani 1 3 d S . . S1 S 0.07566(12) 0.27433(12) 0.07791(7) 0.0414(3) Uani 1 1 d . . . O1 O -0.0383(3) 0.1358(3) 0.05422(15) 0.0416(8) Uani 1 1 d . . . C1 C 0.0612(7) 0.3957(5) 0.0305(3) 0.0653(17) Uani 1 1 d . . . H1A H 0.0820 0.3862 -0.0119 0.075(19) Uiso 1 1 calc R . . H1B H 0.1238 0.4858 0.0449 0.10(2) Uiso 1 1 calc R . . H1C H -0.0298 0.3802 0.0329 0.10(3) Uiso 1 1 calc R . . C2 C 0.0078(6) 0.2985(5) 0.1474(2) 0.0532(14) Uani 1 1 d . . . H2A H -0.0011 0.2322 0.1775 0.072(18) Uiso 1 1 calc R . . H2B H -0.0799 0.2883 0.1392 0.09(2) Uiso 1 1 calc R . . H2C H 0.0675 0.3881 0.1632 0.08(2) Uiso 1 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 In 0.0270(3) 0.0270(3) 0.0533(5) 0.000 0.000 0.01352(14) I1 0.0368(3) 0.0368(3) 0.1016(8) 0.000 0.000 0.01842(16) I2 0.0437(2) 0.0437(2) 0.0639(4) 0.000 0.000 0.02184(12) S1 0.0312(6) 0.0300(6) 0.0606(7) -0.0026(6) -0.0004(6) 0.0136(5) O1 0.0332(16) 0.0304(17) 0.060(2) -0.0088(15) 0.0001(15) 0.0150(14) C1 0.088(5) 0.041(3) 0.062(4) 0.019(3) 0.014(3) 0.029(3) C2 0.057(4) 0.040(3) 0.049(3) -0.003(3) 0.005(3) 0.014(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 In O1 2.145(3) 10 ? In O1 2.145(3) 12 ? In O1 2.145(3) 3 ? In O1 2.145(3) 11 ? In O1 2.145(3) . ? In O1 2.145(3) 2 ? S1 O1 1.541(3) . ? S1 C2 1.765(5) . ? S1 C1 1.787(5) . ? 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 In O1 93.23(12) 10 12 ? O1 In O1 86.77(12) 10 3 ? O1 In O1 180.0(2) 12 3 ? O1 In O1 93.23(12) 10 11 ? O1 In O1 93.23(12) 12 11 ? O1 In O1 86.77(12) 3 11 ? O1 In O1 180.0(2) 10 . ? O1 In O1 86.77(12) 12 . ? O1 In O1 93.23(12) 3 . ? O1 In O1 86.77(12) 11 . ? O1 In O1 86.77(12) 10 2 ? O1 In O1 86.77(12) 12 2 ? O1 In O1 93.23(12) 3 2 ? O1 In O1 180.00(14) 11 2 ? O1 In O1 93.23(12) . 2 ? O1 S1 C2 103.3(2) . . ? O1 S1 C1 104.1(2) . . ? C2 S1 C1 98.5(3) . . ? S1 O1 In 123.06(17) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.478 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.102 #end data_complex3 #=========================================================================== #======================================================================= # END of CIF #=========================================================================== #=======================================================================