# Supplementary Material (ESI) for Faraday Discussions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Faraday Discuss.' _journal_coden_cambridge 0169 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof A.J. Blake' _publ_contact_author_email A.J.Blake@nottingham.ac.uk loop_ _publ_author_name S.Yang S.K.Callear J.Sun A.J.Blake W.I.F.David ; A.J.Ramirez-Cuesta ; N.R.Champness M.Schroder data_NOTT-210 _database_code_depnum_ccdc_archive 'CCDC 799919' #TrackingRef '- nott210-213.cif' _refine_special_details ; Due to large pore voids (\~73% - see PLATON SQUEZE details) contained in the structural model, the crystal diffracted rather weakly with almost no diffraction at high resolution (<0.9 Angstrom). We believe that there is inherent limit of the data quality. The final data reduction was selected to cut off high resolution data using CrysAlis software. The phenyl ring of the ligand containing C6 and C7 is rotationally disordered over two equally-occupied orientations. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.014 -0.009 -0.005 1914 570 _platon_squeeze_details ; Approximately 73% of the unit cell volume comprises a large region of disordered solvent and counter-cations which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent/cation region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 570 electrons per unit cell, which were assigned to be 2.0 DMF and 4.0 water molecules per indium. The final formula was calculated from the TGA combined with elemental analysis data. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'In (C22 O8 H10) (C2 H8 N), 2(C3 H7 N O), 4(H2 O)' _chemical_formula_sum 'C30 H40 In N3 O14' _chemical_formula_weight 781.47 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' In In -0.7276 1.3100 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/mmc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' 'x, -y, -z' 'y, x, -z+1/2' '-x, y, -z' '-y, -x, -z+1/2' '-x, -y, -z' 'y, -x, -z-1/2' 'x, y, -z' '-y, x, -z-1/2' '-x, y, z' '-y, -x, z-1/2' 'x, -y, z' 'y, x, z-1/2' _cell_length_a 9.9532(3) _cell_length_b 9.9532(3) _cell_length_c 26.7005(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2645.12(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 700 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 33.22 _exptl_crystal_description Octahedron _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.981 _exptl_crystal_density_method ? _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CrysAlis CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 16.546 _diffrn_reflns_number 24345 _diffrn_reflns_av_R_equivalents 0.0899 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1073 _reflns_number_gt 774 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.115P)^2^+1.00P] 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 1073 _refine_ls_number_parameters 49 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.174 _refine_ls_wR_factor_gt 0.167 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.01 _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 0.5000 0.5000 0.2500 0.0530(5) Uani 1 8 d SU . . O1 O 0.3557(5) 0.5000 0.18755(18) 0.0710(14) Uani 1 2 d SU . . O2 O 0.2569(6) 0.5000 0.2605(2) 0.099(2) Uani 1 2 d SU . . C1 C 0.2529(9) 0.5000 0.2134(4) 0.087(3) Uani 1 2 d SU . . C2 C 0.1205(7) 0.5000 0.1875(3) 0.080(2) Uani 1 2 d SU . . C3 C 0.1225(8) 0.5000 0.1363(3) 0.093(3) Uani 1 2 d SU . . H3 H 0.2048 0.5000 0.1198 0.112 Uiso 1 2 calc SR . . C4 C 0.0000 0.5000 0.2142(4) 0.080(3) Uani 1 4 d SU . . H4 H 0.0000 0.5000 0.2491 0.096 Uiso 1 4 calc SR . . C5 C 0.0000 0.5000 0.1070(4) 0.098(4) Uani 1 4 d SU . . C6 C 0.0000 0.5000 0.0527(5) 0.116(6) Uani 1 4 d SU . . C7 C 0.1109(15) 0.460(2) 0.0272(4) 0.163(9) Uiso 0.50 1 d PU . . H7A H 0.1898 0.4361 0.0459 0.196 Uiso 0.50 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 0.0572(5) 0.0572(5) 0.0448(7) 0.000 0.000 0.000 O1 0.043(3) 0.092(4) 0.079(4) 0.000 0.001(3) 0.000 O2 0.061(4) 0.157(7) 0.079(5) 0.000 -0.009(3) 0.000 C1 0.059(5) 0.117(7) 0.084(6) 0.000 -0.015(5) 0.000 C2 0.055(5) 0.111(7) 0.073(6) 0.000 -0.012(4) 0.000 C3 0.053(5) 0.145(9) 0.080(6) 0.000 -0.004(4) 0.000 C4 0.044(6) 0.125(11) 0.071(8) 0.000 0.000 0.000 C5 0.066(8) 0.158(14) 0.068(8) 0.000 0.000 0.000 C6 0.051(8) 0.213(18) 0.083(9) 0.000 0.000 0.000 _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 2.201(5) . ? In1 O2 2.436(6) . ? O1 C1 1.235(10) . ? O2 C1 1.258(11) . ? C1 C2 1.488(11) . ? C2 C3 1.368(10) . ? C2 C4 1.395(9) . ? C3 C5 1.449(10) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.450(17) . ? C6 C7 1.358(15) . ? C7 C7 1.45(2) 11 ? C7 H7A 0.9601 . ? 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 125.03(16) 10_566 . ? O1 In1 O1 81.5(3) 3_665 . ? O1 In1 O2 84.98(9) 10_566 . ? O1 In1 O2 137.4(2) 3_665 . ? O1 In1 O2 55.88(17) . . ? O2 In1 O2 166.7(3) . 3_665 ? O2 In1 O2 90.76(3) . 10_566 ? C1 O1 In1 96.7(5) . . ? C1 O2 In1 85.2(5) . . ? O1 C1 O2 122.2(8) . . ? O1 C1 C2 118.3(9) . . ? O2 C1 C2 119.5(8) . . ? C3 C2 C4 121.6(8) . . ? C3 C2 C1 116.8(8) . . ? C4 C2 C1 121.6(8) . . ? C2 C3 C5 121.8(8) . . ? C2 C3 H3 119.1 . . ? C5 C3 H3 119.1 . . ? C2 C4 C2 118.5(10) 3_565 . ? C2 C4 H4 120.7 3_565 . ? C2 C4 H4 120.7 . . ? C3 C5 C6 122.7(5) 3_565 . ? C3 C5 C6 122.7(5) . . ? C7 C6 C7 119.8(16) 13 15_565 ? C7 C6 C5 120.1(8) . . ? C7 C6 C5 120.1(8) 13 . ? C7 C6 C5 120.1(8) 3_565 . ? C7 C6 C5 120.1(8) 15_565 . ? C6 C7 C7 120.1(8) . 11 ? C7 C7 H7A 121.4 11 . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.35 _refine_diff_density_min -0.49 _refine_diff_density_rms 0.09 #===END of CIF data_NOTT-211 _database_code_depnum_ccdc_archive 'CCDC 799920' #TrackingRef '- nott210-213.cif' _refine_special_details ; Due to large pore voids (\~65% - see PLATON SQUEZE details) contained in the structural model, the crystal diffracted rather weakly with almost no diffraction at high resolution (<0.9 Angstrom). We believe that there is inherent limit of the data quality. The final data reduction was selected to cut off high resolution data using CrysAlis software. The phenyl ring of the ligand containing C6 and C7 is rotationally disordered over two equally-occupied orientations. The methyl group of ligand containing C8 is disordered over four equally-occupied orientations. Therefore, C6, C7, and C8 were refined isotropically. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.027 -0.017 -0.008 1660 28 _platon_squeeze_details ; Approximately 65% of the unit cell volume comprises a large region of disordered solvent and counter-cations which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent/cation region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 28 electrons per unit cell, which were assigned to be 2.0 DMF and 2.0 water molecules per indium. The final formula was calculated from the TGA combined with elemental analysis data. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'In (C24 O8 H12) (C2 H8 N), 2(C3 H7 N O), 2(H2 O)' _chemical_formula_sum 'C32 H38 In N3 O12' _chemical_formula_weight 771.47 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/mmc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, y, -z' 'x, -y, -z' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x, -y, z' '-x, y, z' '-y, -x, z-1/2' 'y, x, z-1/2' _cell_length_a 9.9617(4) _cell_length_b 9.9617(4) _cell_length_c 26.747(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2654.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 790 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 33.22 _exptl_crystal_description Octahedron _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.965 _exptl_crystal_density_method ? _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CrysAlis CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 16.5467 _diffrn_reflns_number 8753 _diffrn_reflns_av_R_equivalents 0.130 _diffrn_reflns_av_sigmaI/netI 0.169 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 23.24 _reflns_number_total 1084 _reflns_number_gt 503 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.060P)^2^+6.000P] 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 1084 _refine_ls_number_parameters 51 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.178 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.189 _refine_ls_wR_factor_gt 0.173 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.5000 0.5000 0.2500 0.0684(8) Uani 1 8 d SU . . O1 O 0.2608(11) 0.5000 0.2408(3) 0.121(4) Uani 1 2 d SU . . O2 O 0.5000 0.3562(9) 0.1878(3) 0.088(3) Uani 1 2 d SU . . C1 C 0.5000 0.2497(14) 0.2137(5) 0.083(4) Uani 1 2 d SU . . C2 C 0.5000 0.1196(13) 0.1871(5) 0.092(5) Uani 1 2 d SU . . C3 C 0.5000 0.0000 0.2122(7) 0.087(7) Uani 1 4 d SU . . H3A H 0.5000 0.0000 0.2470 0.105 Uiso 1 4 calc SR . . C4 C 0.5000 0.1194(13) 0.1337(5) 0.107(6) Uani 1 2 d SU . . H4A H 0.5000 0.2003 0.1163 0.128 Uiso 1 2 calc SR . . C5 C 0.5000 0.0000 0.1078(7) 0.126(10) Uani 1 4 d SDU . . C6 C 0.5000 0.0000 0.0512(7) 0.131(9) Uiso 1 4 d SDU . . C7 C 0.389(2) 0.058(2) 0.0298(6) 0.121(9) Uiso 0.50 1 d PDU . . C8 C 0.258(3) 0.117(5) 0.0477(17) 0.148(18) Uiso 0.25 1 d PDU . . H8A H 0.2083 0.1500 0.0196 0.177 Uiso 0.25 1 calc PR . . H8B H 0.2763 0.1896 0.0703 0.177 Uiso 0.25 1 calc PR . . H8C H 0.2073 0.0491 0.0645 0.177 Uiso 0.25 1 calc 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 0.0824(11) 0.0824(11) 0.0404(9) 0.000 0.000 0.000 O1 0.127(8) 0.205(11) 0.031(6) 0.000 0.012(5) 0.000 O2 0.141(9) 0.044(6) 0.078(6) -0.007(5) 0.000 0.000 C1 0.139(13) 0.035(7) 0.075(9) 0.007(7) 0.000 0.000 C2 0.153(14) 0.024(7) 0.098(9) 0.005(7) 0.000 0.000 C3 0.15(2) 0.027(10) 0.086(12) 0.000 0.000 0.000 C4 0.219(18) 0.033(9) 0.069(8) -0.006(7) 0.000 0.000 C5 0.23(3) 0.092(17) 0.057(12) 0.000 0.000 0.000 _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 O2 2.195(8) . ? In1 O1 2.395(11) . ? O1 C1 1.223(14) 11_566 ? O2 C1 1.266(13) . ? C1 C2 1.477(16) . ? C2 C3 1.368(15) . ? C2 C4 1.429(17) . ? C3 C2 1.368(15) 2_655 ? C4 C5 1.377(14) . ? C5 C4 1.376(14) 2_655 ? C5 C6 1.513(10) . ? C6 C7 1.38(2) . ? C7 C8 1.503(10) . ? 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 In1 O2 125.0(3) 11_566 . ? O2 In1 O2 81.5(5) 2_665 . ? O2 In1 O1 55.1(3) 11_566 . ? O2 In1 O1 85.53(14) . . ? O2 In1 O1 136.6(3) . 11_566 ? O1 In1 O1 90.61(4) . 11_566 ? O2 In1 O1 85.54(14) . 2_665 ? O1 In1 O1 168.2(4) . 2_665 ? C1 O1 In1 89.3(9) 11_566 . ? C1 O2 In1 97.7(8) . . ? O1 C1 O2 117.8(14) 12_656 . ? O1 C1 C2 124.0(14) 12_656 . ? O2 C1 C2 118.2(12) . . ? C3 C2 C4 119.3(14) . . ? C3 C2 C1 121.8(13) . . ? C4 C2 C1 118.9(12) . . ? C2 C3 C2 121.1(18) . 2_655 ? C5 C4 C2 120.3(13) . . ? C4 C5 C4 119.5(17) 2_655 . ? C4 C5 C6 120.2(9) 2_655 . ? C4 C5 C6 120.2(9) . . ? C7 C6 C5 114.6(11) 13 . ? C7 C6 C5 114.6(11) 14_655 . ? C7 C6 C5 114.6(11) 2_655 . ? C7 C6 C5 114.6(11) . . ? C8 C7 C7 119(2) . 6 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.12 _refine_diff_density_min -0.34 _refine_diff_density_rms 0.08 #===END of CIF data_NOTT-212 _database_code_depnum_ccdc_archive 'CCDC 799921' #TrackingRef '- nott210-213.cif' _refine_special_details ; Due to large pore voids (\~70% - see PLATON SQUEZE details) contained in the structural model, although data was collected using synchrotron radiation, the crystal diffracted rather weakly with almost no diffraction at high resolution (<0.9 Angstrom). We believe that there is inherent limit of the data quality. The final data reduction was selected to cut off high resolution data using Bruker software. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.023 0.217 -0.002 14633 1559 _platon_squeeze_details ; Approximately 70% of the unit cell volume comprises a large region of disordered solvent and counter-cations which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent/cation region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 1559 electrons per unit cell, which were assigned to be 2.0 DMF and 4.0 water molecules per indium. The final formula was calculated from the TGA combined with elemental analysis data. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'In (C22 O8 H6 F4) (C2 H8 N), 2(C3 H7 N O), 4.0(H2 O)' _chemical_formula_sum 'C30 H36 F4 In N3 O14' _chemical_formula_weight 853.44 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' N N 0.0061 0.0033 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/acd' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 19.807(5) _cell_length_b 19.807(5) _cell_length_c 53.454(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20971(8) _cell_formula_units_Z 16 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 937 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 24.84 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.081 _exptl_crystal_density_method ? _exptl_crystal_F_000 6944 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6943 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEXII CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean 66.06 _diffrn_reflns_number 61209 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.022 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 22.69 _reflns_number_total 3732 _reflns_number_gt 2959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.093P)^2^+40.85P] 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 3732 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.177 _refine_ls_wR_factor_gt 0.168 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.001 _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 0.756915(17) 0.006915(17) 0.1250 0.0579(3) Uani 1 2 d S . . O1 O 0.3827(2) 0.0032(2) 0.13142(8) 0.1064(14) Uani 1 1 d . . . O2 O 0.33033(16) -0.01273(18) 0.09579(7) 0.0843(10) Uani 1 1 d . . . O3 O 0.64166(18) 0.00522(16) 0.12862(6) 0.0737(9) Uani 1 1 d . . . O4 O 0.68837(15) 0.00914(15) 0.09170(5) 0.0674(8) Uani 1 1 d . . . F1 F 0.57550(17) 0.0949(2) 0.02376(5) 0.1129(12) Uani 1 1 d . . . F2 F 0.56952(16) 0.0949(2) -0.02570(5) 0.1124(12) Uani 1 1 d . . . C1 C 0.3838(3) -0.0043(3) 0.10824(12) 0.0842(15) Uani 1 1 d . . . C2 C 0.6366(3) 0.0061(2) 0.10514(9) 0.0707(13) Uani 1 1 d . . . C3 C 0.5691(2) 0.0045(3) 0.09287(9) 0.0728(13) Uani 1 1 d . . . C4 C 0.5095(2) 0.0032(2) 0.10657(10) 0.0788(15) Uani 1 1 d . . . H4 H 0.5108 0.0055 0.1243 0.095 Uiso 1 1 calc R . . C5 C 0.4478(3) -0.0016(3) 0.09425(9) 0.0830(15) Uani 1 1 d . . . C6 C 0.4464(3) -0.0043(3) 0.06853(10) 0.0894(17) Uani 1 1 d . . . H6 H 0.4041 -0.0079 0.0602 0.107 Uiso 1 1 calc R . . C7 C 0.5054(2) -0.0017(3) 0.05436(11) 0.093(2) Uani 1 1 d . . . C8 C 0.5672(2) 0.0021(3) 0.06683(9) 0.0812(15) Uani 1 1 d . . . H8 H 0.6080 0.0030 0.0575 0.097 Uiso 1 1 calc R . . C9 C 0.5023(2) -0.0013(3) 0.02679(10) 0.086(2) Uani 1 1 d . . . C10 C 0.5377(3) 0.0472(4) 0.01253(10) 0.1002(19) Uani 1 1 d . . . C11 C 0.5356(3) 0.0461(4) -0.01352(10) 0.0995(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 In1 0.0691(3) 0.0691(3) 0.0355(3) 0.00185(12) -0.00185(12) -0.00173(17) O1 0.092(3) 0.152(4) 0.076(3) 0.010(2) 0.021(2) 0.002(2) O2 0.052(2) 0.114(3) 0.087(2) 0.0029(19) 0.0093(18) -0.0020(17) O3 0.067(2) 0.109(3) 0.0449(18) 0.0055(15) 0.0016(14) -0.0020(15) O4 0.0580(18) 0.092(2) 0.0525(17) 0.0062(14) -0.0019(15) 0.0112(14) F1 0.101(2) 0.171(3) 0.0669(19) 0.007(2) -0.0089(17) -0.023(2) F2 0.094(2) 0.174(3) 0.0693(19) 0.014(2) -0.0018(16) -0.029(2) C1 0.070(4) 0.107(4) 0.075(4) 0.005(3) 0.019(3) 0.005(3) C2 0.081(3) 0.081(3) 0.050(3) 0.002(2) -0.003(2) 0.003(2) C3 0.059(3) 0.104(4) 0.056(3) 0.010(2) -0.004(2) 0.009(2) C4 0.069(3) 0.111(4) 0.057(3) 0.000(3) 0.006(2) 0.002(2) C5 0.058(3) 0.128(5) 0.063(3) 0.014(3) 0.002(2) 0.002(2) C6 0.057(3) 0.142(5) 0.070(3) 0.019(3) -0.004(2) -0.006(3) C7 0.061(3) 0.162(6) 0.056(3) 0.000(3) -0.002(2) 0.004(3) C8 0.057(3) 0.132(5) 0.055(3) 0.005(3) -0.002(2) 0.012(3) C9 0.034(2) 0.170(6) 0.055(3) 0.007(3) -0.0033(19) 0.002(3) C10 0.068(3) 0.170(6) 0.063(3) 0.009(4) -0.012(3) -0.014(4) C11 0.070(4) 0.166(6) 0.063(3) 0.016(4) -0.006(3) -0.002(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 In1 O2 2.137(3) 20_656 ? In1 O4 2.239(3) . ? In1 O3 2.291(4) . ? In1 O1 2.523(5) 20_656 ? O1 C1 1.248(7) . ? O2 C1 1.262(7) . ? O3 C2 1.259(5) . ? O4 C2 1.254(6) . ? F1 C10 1.347(7) . ? F2 C11 1.346(7) . ? C1 C5 1.474(7) . ? C2 C3 1.488(7) . ? C3 C4 1.391(7) . ? C3 C8 1.393(7) . ? C4 C5 1.390(7) . ? C5 C6 1.376(7) . ? C6 C7 1.394(7) . ? C7 C8 1.396(7) . ? C7 C9 1.475(8) . ? C9 C11 1.361(8) 17_655 ? C9 C10 1.412(8) . ? C10 C11 1.393(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 O2 In1 O2 117.42(19) 20_656 21_655 ? O2 In1 O4 80.26(13) 20_656 15_534 ? O2 In1 O4 126.88(12) 20_656 . ? O4 In1 O4 130.97(16) 15_534 . ? O2 In1 O3 137.79(13) 20_656 15_534 ? O2 In1 O3 90.11(12) 20_656 . ? O4 In1 O3 86.76(11) 15_534 . ? O4 In1 O3 57.54(11) . . ? O3 In1 O3 88.74(16) 15_534 . ? O2 In1 O1 84.34(13) 20_656 21_655 ? O4 In1 O1 79.89(13) 15_534 21_655 ? O3 In1 O1 166.22(14) . 21_655 ? O2 In1 O1 55.35(13) 20_656 20_656 ? O4 In1 O1 135.11(12) 15_534 20_656 ? O3 In1 O1 86.96(12) . 20_656 ? O1 In1 O1 100.09(19) 21_655 20_656 ? C1 O1 In1 82.7(3) . 27_565 ? C1 O2 In1 100.3(3) . 27_565 ? C2 O3 In1 89.7(3) . . ? C2 O4 In1 92.3(3) . . ? O1 C1 O2 121.7(5) . . ? O1 C1 C5 121.0(6) . . ? O2 C1 C5 117.3(5) . . ? O4 C2 O3 120.4(5) . . ? O4 C2 C3 118.9(4) . . ? O3 C2 C3 120.7(5) . . ? C4 C3 C8 120.1(4) . . ? C4 C3 C2 122.1(4) . . ? C8 C3 C2 117.8(4) . . ? C5 C4 C3 119.9(5) . . ? C6 C5 C4 119.6(5) . . ? C6 C5 C1 119.2(5) . . ? C4 C5 C1 121.2(5) . . ? C5 C6 C7 121.6(5) . . ? C6 C7 C8 118.6(5) . . ? C6 C7 C9 120.6(4) . . ? C8 C7 C9 120.8(4) . . ? C3 C8 C7 120.2(5) . . ? C11 C9 C10 115.8(5) 17_655 . ? C11 C9 C7 122.6(5) 17_655 . ? C10 C9 C7 121.5(5) . . ? F1 C10 C11 118.2(5) . . ? F1 C10 C9 120.8(5) . . ? C11 C10 C9 120.9(6) . . ? F2 C11 C9 119.5(5) . 17_655 ? F2 C11 C10 117.2(6) . . ? C9 C11 C10 123.2(6) 17_655 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 22.69 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.30 _refine_diff_density_min -0.77 _refine_diff_density_rms 0.06 #===END of CIF data_NOTT-213 _database_code_depnum_ccdc_archive 'CCDC 799922' #TrackingRef '- nott210-213.cif' _refine_special_details ; Due to large pore voids (\~60% - see PLATON SQUEZE details) contained in the structural model, the crystal diffracted rather weakly with almost no diffraction at high resolution (<0.9 Angstrom). We believe that there is inherent limit of the data quality. The final data reduction was selected to cut off high resolution data using CrysAlis software. The phenyl ring of the ligand containing C6, C7, C8 and C9 is rotationally disordered over four equally-occupied orientations.Therefore, C6, C7, C8 and C9 were refined isotropically. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.019 0.436 -0.004 1529 30 _platon_squeeze_details ; Approximately 65% of the unit cell volume comprises a large region of disordered solvent and counter-cations which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent/cation region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 30 electrons per unit cell, which were assigned to be 2.0 DMF and 2.0 water molecules per indium. The final formula was calculated from the TGA combined with elemental analysis data. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'In (C26 O8 H10) (C2 H8 N), 2(C3 H7 N O), 2(H2 O)' _chemical_formula_sum 'C34 H36 In N3 O12' _chemical_formula_weight 793.48 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/mmc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, y, -z' 'x, -y, -z' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x, -y, z' '-x, y, z' '-y, -x, z-1/2' 'y, x, z-1/2' _cell_length_a 9.9617(4) _cell_length_b 9.9617(4) _cell_length_c 26.747(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2654.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 760 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 33.22 _exptl_crystal_description Octahedron _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.993 _exptl_crystal_density_method ? _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CrysAlis CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 16.5467 _diffrn_reflns_number 24009 _diffrn_reflns_av_R_equivalents 0.093 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 23.24 _reflns_number_total 1085 _reflns_number_gt 696 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.043P)^2^+2.000P] 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 1085 _refine_ls_number_parameters 55 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.105 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.00 _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 0.5000 0.5000 0.2500 0.0562(3) Uani 1 8 d SU . . O1 O 0.2575(5) 0.5000 0.24041(15) 0.1041(18) Uani 1 2 d SU . . O2 O 0.5000 0.3581(4) 0.18774(17) 0.0848(14) Uani 1 2 d SU . . C1 C 0.5000 0.2525(7) 0.2136(3) 0.074(2) Uani 1 2 d SU . . C2 C 0.5000 0.1188(6) 0.1864(3) 0.0751(19) Uani 1 2 d SU . . C3 C 0.5000 0.0000 0.2131(3) 0.069(3) Uani 1 4 d SU . . H3A H 0.5000 0.0000 0.2478 0.083 Uiso 1 4 calc SR . . C4 C 0.5000 0.1202(7) 0.1350(2) 0.090(2) Uani 1 2 d SU . . H4A H 0.5000 0.2012 0.1177 0.108 Uiso 1 2 calc SR . . C5 C 0.5000 0.0000 0.1093(3) 0.103(4) Uani 1 4 d SU . . C6 C 0.5000 0.0000 0.0514(5) 0.109(4) Uiso 1 4 d SDU . . C7 C 0.3821(11) 0.0536(10) 0.02725(17) 0.118(4) Uiso 0.50 1 d PDU . . C8 C 0.2555(18) 0.094(2) 0.0501(10) 0.139(9) Uiso 0.25 1 d PDU . -1 H8A H 0.2485 0.0746 0.0852 0.167 Uiso 0.25 1 d PR . -1 C9 C 0.135(3) 0.148(2) 0.0272(2) 0.226(17) Uiso 0.25 1 d PD A -2 H9A H 0.0594 0.1830 0.0455 0.271 Uiso 0.25 1 d PR A -2 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 0.0666(4) 0.0666(4) 0.0355(4) 0.000 0.000 0.000 O1 0.081(3) 0.182(5) 0.049(3) 0.000 0.015(2) 0.000 O2 0.124(4) 0.050(3) 0.080(3) -0.008(3) 0.000 0.000 C1 0.084(5) 0.059(5) 0.079(5) -0.005(4) 0.000 0.000 C2 0.100(5) 0.049(4) 0.076(5) -0.006(4) 0.000 0.000 C3 0.101(8) 0.045(6) 0.062(6) 0.000 0.000 0.000 C4 0.166(8) 0.048(4) 0.056(4) -0.008(4) 0.000 0.000 C5 0.179(13) 0.076(8) 0.052(6) 0.000 0.000 0.000 _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 O2 2.184(4) . ? In1 O1 2.430(5) . ? O1 C1 1.230(8) 11_566 ? O2 C1 1.259(7) . ? C1 C2 1.518(8) . ? C2 C4 1.377(9) . ? C2 C3 1.381(8) . ? C4 C5 1.380(7) . ? C5 C6 1.549(15) . ? C6 C7 1.443(8) . ? C7 C8 1.457(10) . ? C7 C7 1.458(9) 10 ? 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 In1 O2 125.53(16) . 11_566 ? O2 In1 O2 80.7(3) . 2_665 ? O2 In1 O1 136.39(16) . 11_566 ? O2 In1 O1 85.38(7) . . ? O2 In1 O1 55.73(16) 11_566 . ? O1 In1 O1 90.64(2) 11_566 . ? O1 In1 O1 167.88(19) 2_665 . ? C1 O1 In1 86.2(5) 11_566 . ? C1 O2 In1 96.9(4) . . ? O1 C1 O2 121.1(7) 12_656 . ? O1 C1 C2 120.9(7) 12_656 . ? O2 C1 C2 118.0(6) . . ? C4 C2 C3 121.6(7) . . ? C4 C2 C1 118.1(6) . . ? C3 C2 C1 120.3(6) . . ? C2 C3 C2 118.0(8) 2_655 . ? C2 C4 C5 119.3(7) . . ? C4 C5 C4 120.4(9) 2_655 . ? C4 C5 C6 119.8(4) 2_655 . ? C4 C5 C6 119.8(4) . . ? C8 C7 C7 120.0(10) . 6 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.62 _refine_diff_density_min -0.26 _refine_diff_density_rms 0.05 #===END of CIF