# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- ZBHAN110415.cif' #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; 'Han, Zheng-Bo' College of Chemistry liaoning University Shenyang, 110036 People's Republic of China ; _publ_contact_author_phone 86-24-62207849 _publ_contact_author_fax 86-24-62202380 _publ_contact_author_email ceshzb@lnu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to Dalton Trans. April 10, 2011 ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Zheng-Bo Han' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Bi-Ye Li' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Jian-Wei Ji' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Hai-Yan An' ; Department of Chemistry Dalian University of Technology Dalian 116023 People's Republic of China ; 'Ming-Hua Zeng' ; Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources(Ministry of Education) School of Chemistry & Chemical Engineering Guangxi Normal University Guilin 541004 People's Republic of China ; _publ_contact_author_name 'Han, Zheng-Bo' #====================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 821438' #TrackingRef '- ZBHAN110415.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6.50 In O9.75' _chemical_formula_weight 397.47 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(2)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z' 'y, -x+y, z+2/3' 'x-y, x, z+1/3' 'y, x, -z+2/3' 'x-y, -y, -z' '-x, -x+y, -z+1/3' '-y, -x, -z+2/3' '-x+y, y, -z' 'x, x-y, -z+1/3' _cell_length_a 9.038(2) _cell_length_b 9.038(2) _cell_length_c 18.975(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1342.2(9) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 581 _exptl_absorpt_coefficient_mu 1.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6353 _exptl_absorpt_correction_T_max 0.7602 _exptl_absorpt_process_details sadabs _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11174 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.99 _reflns_number_total 893 _reflns_number_gt 594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 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^)+(0.1360P)^2^+0.2146P] 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 SHELXL _refine_ls_extinction_coef 0.029(7) _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 0.2(8) _refine_ls_number_reflns 893 _refine_ls_number_parameters 50 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.2116 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _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 In1 In 1.0000 0.0000 0.1667 0.0215(6) Uani 1 4 d S . . C1 C 0.7692(10) -0.0016(12) 0.0778(4) 0.0328(19) Uani 1 1 d . . . O1 O 0.8535(10) 0.1120(11) 0.1252(3) 0.081(3) Uani 1 1 d . . . C3 C 0.5000 0.0000 0.0715(5) 0.034(3) Uani 1 2 d S . . H3A H 0.5000 0.0000 0.1215 0.041 Uiso 1 2 calc SR . . C2 C 0.6311(9) -0.0031(11) 0.0381(3) 0.0294(19) Uani 1 1 d . . . O2 O 0.8137(10) -0.1123(10) 0.0695(4) 0.085(3) Uani 1 1 d . . . O1W O 0.685(5) -0.462(9) 0.0449(18) 0.35(3) Uiso 0.44 1 d P . . H1WA H 0.7146 -0.5183 0.0713 0.417 Uiso 0.44 1 d PR . . H1WB H 0.6171 -0.5107 0.0106 0.417 Uiso 0.44 1 d PR . . 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 In1 0.0186(8) 0.0250(8) 0.0187(9) 0.000 0.000 0.0093(4) C1 0.027(5) 0.054(5) 0.018(3) -0.012(4) 0.004(3) 0.021(4) O1 0.091(7) 0.147(8) 0.060(4) -0.049(5) -0.036(4) 0.101(7) C3 0.023(6) 0.046(7) 0.019(5) 0.000 0.000 0.008(6) C2 0.025(4) 0.038(4) 0.029(4) -0.003(4) 0.007(3) 0.019(4) O2 0.060(5) 0.059(5) 0.154(8) -0.057(5) -0.066(5) 0.045(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 In1 O1 2.177(6) 9_765 ? In1 O1 2.177(6) 12_545 ? In1 O1 2.177(6) . ? In1 O1 2.177(6) 4_755 ? In1 O2 2.358(6) 9_765 ? In1 O2 2.358(6) 12_545 ? In1 O2 2.358(6) . ? In1 O2 2.358(6) 4_755 ? In1 C1 2.677(8) 9_765 ? In1 C1 2.677(8) 12_545 ? In1 C1 2.677(8) . ? In1 C1 2.677(8) 4_755 ? C1 O2 1.261(10) . ? C1 O1 1.288(10) . ? C1 C2 1.452(10) . ? C3 C2 1.356(8) 4_655 ? C3 C2 1.356(8) . ? C3 H3A 0.9500 . ? C2 C2 1.447(12) 8 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? 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 In1 O1 137.6(3) 9_765 12_545 ? O1 In1 O1 79.4(4) 9_765 . ? O1 In1 O1 116.4(5) 12_545 . ? O1 In1 O1 116.4(5) 9_765 4_755 ? O1 In1 O1 79.4(4) 12_545 4_755 ? O1 In1 O1 137.6(3) . 4_755 ? O1 In1 O2 56.5(2) 9_765 9_765 ? O1 In1 O2 89.2(2) 12_545 9_765 ? O1 In1 O2 131.7(3) . 9_765 ? O1 In1 O2 84.3(3) 4_755 9_765 ? O1 In1 O2 89.2(2) 9_765 12_545 ? O1 In1 O2 56.5(2) 12_545 12_545 ? O1 In1 O2 84.3(3) . 12_545 ? O1 In1 O2 131.7(3) 4_755 12_545 ? O2 In1 O2 77.1(5) 9_765 12_545 ? O1 In1 O2 131.7(3) 9_765 . ? O1 In1 O2 84.3(3) 12_545 . ? O1 In1 O2 56.5(2) . . ? O1 In1 O2 89.2(2) 4_755 . ? O2 In1 O2 171.6(3) 9_765 . ? O2 In1 O2 103.6(4) 12_545 . ? O1 In1 O2 84.3(3) 9_765 4_755 ? O1 In1 O2 131.7(3) 12_545 4_755 ? O1 In1 O2 89.2(2) . 4_755 ? O1 In1 O2 56.5(2) 4_755 4_755 ? O2 In1 O2 103.6(4) 9_765 4_755 ? O2 In1 O2 171.6(3) 12_545 4_755 ? O2 In1 O2 77.1(5) . 4_755 ? O1 In1 C1 28.5(2) 9_765 9_765 ? O1 In1 C1 115.1(2) 12_545 9_765 ? O1 In1 C1 106.7(3) . 9_765 ? O1 In1 C1 99.7(3) 4_755 9_765 ? O2 In1 C1 28.1(2) 9_765 9_765 ? O2 In1 C1 84.1(2) 12_545 9_765 ? O2 In1 C1 159.8(2) . 9_765 ? O2 In1 C1 92.7(2) 4_755 9_765 ? O1 In1 C1 115.1(2) 9_765 12_545 ? O1 In1 C1 28.5(2) 12_545 12_545 ? O1 In1 C1 99.7(3) . 12_545 ? O1 In1 C1 106.7(3) 4_755 12_545 ? O2 In1 C1 84.1(2) 9_765 12_545 ? O2 In1 C1 28.1(2) 12_545 12_545 ? O2 In1 C1 92.7(2) . 12_545 ? O2 In1 C1 159.8(2) 4_755 12_545 ? C1 In1 C1 101.9(3) 9_765 12_545 ? O1 In1 C1 106.7(3) 9_765 . ? O1 In1 C1 99.7(3) 12_545 . ? O1 In1 C1 28.5(2) . . ? O1 In1 C1 115.1(2) 4_755 . ? O2 In1 C1 159.8(2) 9_765 . ? O2 In1 C1 92.7(2) 12_545 . ? O2 In1 C1 28.1(2) . . ? O2 In1 C1 84.1(2) 4_755 . ? C1 In1 C1 134.8(4) 9_765 . ? C1 In1 C1 95.1(4) 12_545 . ? O1 In1 C1 99.7(3) 9_765 4_755 ? O1 In1 C1 106.7(3) 12_545 4_755 ? O1 In1 C1 115.1(2) . 4_755 ? O1 In1 C1 28.5(2) 4_755 4_755 ? O2 In1 C1 92.7(2) 9_765 4_755 ? O2 In1 C1 159.8(2) 12_545 4_755 ? O2 In1 C1 84.1(2) . 4_755 ? O2 In1 C1 28.1(2) 4_755 4_755 ? C1 In1 C1 95.1(4) 9_765 4_755 ? C1 In1 C1 134.8(4) 12_545 4_755 ? C1 In1 C1 101.9(3) . 4_755 ? O2 C1 O1 115.1(7) . . ? O2 C1 C2 122.7(7) . . ? O1 C1 C2 122.2(7) . . ? O2 C1 In1 61.8(4) . . ? O1 C1 In1 53.7(4) . . ? C2 C1 In1 172.3(5) . . ? C1 O1 In1 97.8(5) . . ? C2 C3 C2 124.3(10) 4_655 . ? C2 C3 H3A 117.8 4_655 . ? C2 C3 H3A 117.8 . . ? C3 C2 C2 117.8(5) . 8 ? C3 C2 C1 120.8(7) . . ? C2 C2 C1 121.3(4) 8 . ? C1 O2 In1 90.1(5) . . ? H1WA O1W H1WB 120.0 . . ? 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 O1 In1 C1 O2 155.7(7) 9_765 . . . ? O1 In1 C1 O2 -57.8(7) 12_545 . . . ? O1 In1 C1 O2 172.9(11) . . . . ? O1 In1 C1 O2 24.9(8) 4_755 . . . ? O2 In1 C1 O2 -172.8(3) 9_765 . . . ? O2 In1 C1 O2 -114.3(7) 12_545 . . . ? O2 In1 C1 O2 73.5(8) 4_755 . . . ? C1 In1 C1 O2 161.4(7) 9_765 . . . ? C1 In1 C1 O2 -86.2(8) 12_545 . . . ? C1 In1 C1 O2 51.7(6) 4_755 . . . ? O1 In1 C1 O1 -17.2(8) 9_765 . . . ? O1 In1 C1 O1 129.3(6) 12_545 . . . ? O1 In1 C1 O1 -148.0(4) 4_755 . . . ? O2 In1 C1 O1 14.3(12) 9_765 . . . ? O2 In1 C1 O1 72.8(6) 12_545 . . . ? O2 In1 C1 O1 -172.9(11) . . . . ? O2 In1 C1 O1 -99.4(6) 4_755 . . . ? C1 In1 C1 O1 -11.5(6) 9_765 . . . ? C1 In1 C1 O1 100.9(6) 12_545 . . . ? C1 In1 C1 O1 -121.2(7) 4_755 . . . ? O1 In1 C1 C2 -77(5) 9_765 . . . ? O1 In1 C1 C2 69(5) 12_545 . . . ? O1 In1 C1 C2 -60(4) . . . . ? O1 In1 C1 C2 152(5) 4_755 . . . ? O2 In1 C1 C2 -46(5) 9_765 . . . ? O2 In1 C1 C2 13(5) 12_545 . . . ? O2 In1 C1 C2 127(5) . . . . ? O2 In1 C1 C2 -159(5) 4_755 . . . ? C1 In1 C1 C2 -72(5) 9_765 . . . ? C1 In1 C1 C2 41(4) 12_545 . . . ? C1 In1 C1 C2 179(5) 4_755 . . . ? O2 C1 O1 In1 -6.9(10) . . . . ? C2 C1 O1 In1 172.1(6) . . . . ? O1 In1 O1 C1 163.3(8) 9_765 . . . ? O1 In1 O1 C1 -58.5(6) 12_545 . . . ? O1 In1 O1 C1 45.5(5) 4_755 . . . ? O2 In1 O1 C1 -173.5(6) 9_765 . . . ? O2 In1 O1 C1 -106.4(6) 12_545 . . . ? O2 In1 O1 C1 4.0(6) . . . . ? O2 In1 O1 C1 78.9(6) 4_755 . . . ? C1 In1 O1 C1 171.5(4) 9_765 . . . ? C1 In1 O1 C1 -82.8(6) 12_545 . . . ? C1 In1 O1 C1 67.5(8) 4_755 . . . ? C2 C3 C2 C2 2.2(7) 4_655 . . 8 ? C2 C3 C2 C1 178.3(8) 4_655 . . . ? O2 C1 C2 C3 126.2(10) . . . . ? O1 C1 C2 C3 -52.7(12) . . . . ? In1 C1 C2 C3 3(5) . . . . ? O2 C1 C2 C2 -57.8(15) . . . 8 ? O1 C1 C2 C2 123.3(12) . . . 8 ? In1 C1 C2 C2 179(4) . . . 8 ? O1 C1 O2 In1 6.3(10) . . . . ? C2 C1 O2 In1 -172.7(7) . . . . ? O1 In1 O2 C1 -31.8(9) 9_765 . . . ? O1 In1 O2 C1 123.0(7) 12_545 . . . ? O1 In1 O2 C1 -4.1(6) . . . . ? O1 In1 O2 C1 -157.5(7) 4_755 . . . ? O2 In1 O2 C1 162.8(7) 9_765 . . . ? O2 In1 O2 C1 69.5(6) 12_545 . . . ? O2 In1 O2 C1 -101.9(8) 4_755 . . . ? C1 In1 O2 C1 -40.9(15) 9_765 . . . ? C1 In1 O2 C1 95.8(8) 12_545 . . . ? C1 In1 O2 C1 -129.5(6) 4_755 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.163 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.274 #End of Crystallographic Information File