# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yulin Yang' _publ_contact_author_email ylyang@hit.edu.cn loop_ _publ_author_name 'Guangpeng Zhou' 'Yulin Yang' 'Ruiqing Fan' 'Wenwu Cao' 'Bin Yang' data_1 _database_code_depnum_ccdc_archive 'CCDC 832523' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H20 In N2 O6' _chemical_formula_sum 'C33 H20 In N2 O6' _chemical_formula_weight 655.33 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.805(2) _cell_length_b 24.903(5) _cell_length_c 9.881(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.12(3) _cell_angle_gamma 90.00 _cell_volume 2828.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 27528 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.46 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8862 _exptl_absorpt_correction_T_max 0.9167 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27528 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6453 _reflns_number_gt 4520 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0370P)^2^+0.7141P] 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 6453 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.26610(2) 0.119455(9) 0.71861(2) 0.03278(8) Uani 1 1 d . . . O1 O 0.1773(2) 0.20347(9) 0.7327(2) 0.0413(6) Uani 1 1 d . . . O2 O 0.0939(2) 0.12817(9) 0.7680(3) 0.0453(6) Uani 1 1 d . . . O3 O 0.1984(2) 0.13482(10) 0.4756(2) 0.0502(7) Uani 1 1 d . . . O4 O 0.1805(2) 0.05722(10) 0.5713(2) 0.0545(7) Uani 1 1 d . . . O5 O -0.5521(2) 0.41119(12) 1.1275(3) 0.0608(7) Uani 1 1 d . . . O6 O -0.5875(2) 0.33178(12) 1.2046(3) 0.0586(7) Uani 1 1 d . . . N1 N 0.3281(2) 0.14083(12) 0.9593(3) 0.0403(7) Uani 1 1 d . . . N2 N 0.3151(3) 0.04125(11) 0.8485(3) 0.0418(7) Uani 1 1 d . . . C1 C 0.3323(3) 0.18943(15) 1.0136(4) 0.0525(10) Uani 1 1 d . . . H1A H 0.3213 0.2187 0.9534 0.063 Uiso 1 1 calc R . . C2 C 0.3524(4) 0.19954(17) 1.1561(4) 0.0581(11) Uani 1 1 d . . . H2A H 0.3520 0.2344 1.1895 0.070 Uiso 1 1 calc R . . C3 C 0.3725(4) 0.15706(19) 1.2446(4) 0.0636(12) Uani 1 1 d . . . H3A H 0.3864 0.1628 1.3400 0.076 Uiso 1 1 calc R . . C4 C 0.3724(3) 0.10481(16) 1.1933(4) 0.0503(10) Uani 1 1 d . . . C5 C 0.3921(4) 0.0580(2) 1.2798(4) 0.0695(13) Uani 1 1 d . . . H5A H 0.4079 0.0619 1.3759 0.083 Uiso 1 1 calc R . . C6 C 0.3881(4) 0.00908(19) 1.2250(4) 0.0688(13) Uani 1 1 d . . . H6A H 0.4023 -0.0205 1.2838 0.083 Uiso 1 1 calc R . . C7 C 0.3624(4) 0.00080(16) 1.0772(4) 0.0558(10) Uani 1 1 d . . . C8 C 0.3573(5) -0.04980(18) 1.0157(5) 0.0775(14) Uani 1 1 d . . . H8A H 0.3700 -0.0805 1.0705 0.093 Uiso 1 1 calc R . . C9 C 0.3334(5) -0.05380(16) 0.8739(5) 0.0789(15) Uani 1 1 d . . . H9A H 0.3315 -0.0872 0.8314 0.095 Uiso 1 1 calc R . . C10 C 0.3120(4) -0.00735(16) 0.7940(4) 0.0626(12) Uani 1 1 d . . . H10A H 0.2948 -0.0106 0.6977 0.075 Uiso 1 1 calc R . . C11 C 0.3413(3) 0.04552(14) 0.9887(4) 0.0402(8) Uani 1 1 d . . . C12 C 0.3476(3) 0.09860(15) 1.0473(3) 0.0397(8) Uani 1 1 d . . . C13 C 0.0957(3) 0.17951(14) 0.7684(3) 0.0382(8) Uani 1 1 d . . . C14 C 0.0042(3) 0.20873(14) 0.8197(3) 0.0378(8) Uani 1 1 d . . . C15 C -0.0928(3) 0.18194(15) 0.8401(4) 0.0505(9) Uani 1 1 d . . . H15A H -0.1029 0.1458 0.8164 0.061 Uiso 1 1 calc R . . C16 C -0.1747(3) 0.20806(16) 0.8953(4) 0.0532(10) Uani 1 1 d . . . H16A H -0.2397 0.1893 0.9077 0.064 Uiso 1 1 calc R . . C17 C -0.1620(3) 0.26200(16) 0.9327(4) 0.0453(9) Uani 1 1 d . . . C18 C -0.0633(3) 0.28840(16) 0.9133(4) 0.0560(11) Uani 1 1 d . . . H18A H -0.0519 0.3243 0.9386 0.067 Uiso 1 1 calc R . . C19 C 0.0181(3) 0.26206(15) 0.8568(4) 0.0536(10) Uani 1 1 d . . . H19A H 0.0832 0.2806 0.8438 0.064 Uiso 1 1 calc R . . C20 C -0.2513(3) 0.28935(16) 0.9929(4) 0.0464(9) Uani 1 1 d . . . C21 C -0.3189(4) 0.26000(17) 1.0645(5) 0.0618(11) Uani 1 1 d . . . H21A H -0.3057 0.2233 1.0773 0.074 Uiso 1 1 calc R . . C22 C -0.4048(3) 0.28394(17) 1.1170(4) 0.0589(11) Uani 1 1 d . . . H22A H -0.4486 0.2633 1.1648 0.071 Uiso 1 1 calc R . . C23 C -0.4269(3) 0.33846(16) 1.0995(4) 0.0456(9) Uani 1 1 d . . . C24 C -0.3580(3) 0.36844(16) 1.0315(4) 0.0557(10) Uani 1 1 d . . . H24A H -0.3699 0.4053 1.0209 0.067 Uiso 1 1 calc R . . C25 C -0.2719(3) 0.34414(17) 0.9795(4) 0.0575(11) Uani 1 1 d . . . H25A H -0.2265 0.3650 0.9343 0.069 Uiso 1 1 calc R . . C26 C -0.5267(3) 0.36266(18) 1.1474(4) 0.0480(9) Uani 1 1 d . . . C27 C 0.1639(3) 0.08710(16) 0.4642(4) 0.0444(9) Uani 1 1 d . . . C28 C 0.1076(3) 0.06321(14) 0.3279(3) 0.0415(8) Uani 1 1 d . . . C29 C 0.0726(4) 0.01001(16) 0.3194(4) 0.0616(12) Uani 1 1 d . . . H29A H 0.0777 -0.0096 0.4007 0.074 Uiso 1 1 calc R . . C30 C 0.0304(4) -0.01449(16) 0.1932(4) 0.0641(13) Uani 1 1 d . . . H30A H 0.0076 -0.0503 0.1907 0.077 Uiso 1 1 calc R . . C31 C 0.0212(3) 0.01367(14) 0.0682(3) 0.0428(8) Uani 1 1 d . . . C32 C 0.0526(3) 0.06737(15) 0.0783(4) 0.0517(10) Uani 1 1 d . . . H32A H 0.0455 0.0875 -0.0025 0.062 Uiso 1 1 calc R . . C33 C 0.0942(3) 0.09174(15) 0.2056(4) 0.0504(10) Uani 1 1 d . . . H33A H 0.1134 0.1280 0.2088 0.061 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 In1 0.03615(13) 0.03090(12) 0.03450(12) -0.00001(11) 0.01473(9) -0.00159(11) O1 0.0386(13) 0.0393(13) 0.0522(14) 0.0026(11) 0.0235(12) 0.0024(11) O2 0.0417(14) 0.0383(14) 0.0622(15) -0.0033(12) 0.0251(12) -0.0012(11) O3 0.0592(17) 0.0443(15) 0.0444(14) -0.0085(12) 0.0062(13) -0.0012(12) O4 0.0682(19) 0.0549(16) 0.0398(14) -0.0026(12) 0.0110(13) -0.0061(14) O5 0.0531(17) 0.0612(19) 0.0727(18) -0.0226(15) 0.0241(14) 0.0030(14) O6 0.0448(15) 0.0776(19) 0.0626(17) 0.0081(15) 0.0313(14) 0.0153(14) N1 0.0446(17) 0.0422(16) 0.0350(15) -0.0004(13) 0.0108(13) -0.0014(13) N2 0.0468(18) 0.0397(16) 0.0407(16) 0.0009(13) 0.0139(14) 0.0059(13) C1 0.059(3) 0.047(2) 0.050(2) -0.0055(18) 0.0085(19) -0.0047(19) C2 0.066(3) 0.056(3) 0.052(2) -0.019(2) 0.013(2) 0.000(2) C3 0.066(3) 0.081(3) 0.045(2) -0.017(2) 0.013(2) 0.006(2) C4 0.048(2) 0.066(3) 0.0394(19) 0.0013(18) 0.0136(17) 0.0125(19) C5 0.074(3) 0.095(4) 0.041(2) 0.015(2) 0.017(2) 0.026(3) C6 0.086(3) 0.072(3) 0.052(2) 0.029(2) 0.024(2) 0.028(3) C7 0.061(3) 0.054(2) 0.056(2) 0.014(2) 0.022(2) 0.017(2) C8 0.104(4) 0.057(3) 0.072(3) 0.025(2) 0.021(3) 0.018(3) C9 0.114(4) 0.038(2) 0.082(3) 0.003(2) 0.016(3) 0.012(2) C10 0.087(3) 0.046(2) 0.053(2) 0.0029(19) 0.011(2) 0.012(2) C11 0.0388(19) 0.044(2) 0.0414(18) 0.0069(16) 0.0164(16) 0.0067(16) C12 0.0335(18) 0.052(2) 0.0345(17) 0.0017(16) 0.0101(15) 0.0050(16) C13 0.0357(19) 0.043(2) 0.0369(17) -0.0022(16) 0.0104(15) 0.0018(15) C14 0.0317(18) 0.043(2) 0.0406(18) -0.0019(15) 0.0128(15) 0.0010(15) C15 0.044(2) 0.045(2) 0.067(2) -0.0054(19) 0.023(2) -0.0005(17) C16 0.038(2) 0.056(2) 0.072(3) -0.005(2) 0.026(2) -0.0047(18) C17 0.0334(19) 0.057(2) 0.048(2) -0.0066(18) 0.0157(16) 0.0012(17) C18 0.049(2) 0.048(2) 0.079(3) -0.019(2) 0.032(2) -0.0036(18) C19 0.045(2) 0.051(2) 0.074(3) -0.007(2) 0.033(2) -0.0038(18) C20 0.036(2) 0.056(2) 0.050(2) -0.0097(18) 0.0160(17) 0.0021(17) C21 0.057(3) 0.053(2) 0.086(3) 0.002(2) 0.038(2) 0.006(2) C22 0.045(2) 0.064(3) 0.078(3) -0.004(2) 0.034(2) -0.001(2) C23 0.0331(19) 0.061(2) 0.046(2) -0.0112(18) 0.0152(16) 0.0010(17) C24 0.051(2) 0.054(3) 0.069(3) -0.007(2) 0.028(2) 0.0032(19) C25 0.049(2) 0.062(3) 0.072(3) -0.003(2) 0.034(2) 0.000(2) C26 0.032(2) 0.069(3) 0.0422(19) -0.0164(19) 0.0080(16) 0.0026(18) C27 0.040(2) 0.054(2) 0.0405(19) -0.0056(18) 0.0127(16) 0.0066(18) C28 0.046(2) 0.042(2) 0.0377(18) -0.0042(16) 0.0125(16) -0.0008(16) C29 0.094(3) 0.053(2) 0.036(2) 0.0046(18) 0.011(2) -0.023(2) C30 0.103(4) 0.049(2) 0.041(2) -0.0038(18) 0.017(2) -0.036(2) C31 0.045(2) 0.047(2) 0.0367(18) -0.0036(16) 0.0096(16) -0.0121(16) C32 0.068(3) 0.047(2) 0.0355(19) 0.0028(17) 0.0020(18) -0.0072(19) C33 0.064(3) 0.037(2) 0.046(2) -0.0025(17) 0.0033(19) -0.0066(18) _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 O6 2.142(3) 4_665 ? In1 O2 2.207(2) . ? In1 O4 2.208(2) . ? In1 N2 2.332(3) . ? In1 O1 2.358(2) . ? In1 O3 2.383(2) . ? In1 N1 2.384(3) . ? In1 C13 2.641(3) . ? In1 C27 2.655(4) . ? O1 C13 1.250(4) . ? O2 C13 1.279(4) . ? O3 C27 1.253(4) . ? O4 C27 1.272(4) . ? O5 C26 1.250(5) . ? O6 C26 1.269(5) . ? O6 In1 2.142(3) 4_466 ? N1 C12 1.351(4) . ? N1 C1 1.321(4) . ? N2 C10 1.322(5) . ? N2 C11 1.353(4) . ? C1 C2 1.397(5) . ? C1 H1A 0.9300 . ? C2 C3 1.359(6) . ? C2 H2A 0.9300 . ? C3 C4 1.396(6) . ? C3 H3A 0.9300 . ? C4 C12 1.415(5) . ? C4 C5 1.433(6) . ? C5 C6 1.329(6) . ? C5 H5A 0.9300 . ? C6 C7 1.437(6) . ? C6 H6A 0.9300 . ? C7 C11 1.403(5) . ? C7 C8 1.394(6) . ? C8 C9 1.369(6) . ? C8 H8A 0.9300 . ? C9 C10 1.391(5) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.438(5) . ? C13 C14 1.484(5) . ? C14 C19 1.378(5) . ? C14 C15 1.379(5) . ? C15 C16 1.377(5) . ? C15 H15A 0.9300 . ? C16 C17 1.392(5) . ? C16 H16A 0.9300 . ? C17 C18 1.389(5) . ? C17 C20 1.488(5) . ? C18 C19 1.382(5) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.389(5) . ? C20 C25 1.387(5) . ? C21 C22 1.376(5) . ? C21 H21A 0.9300 . ? C22 C23 1.386(5) . ? C22 H22A 0.9300 . ? C23 C24 1.385(5) . ? C23 C26 1.493(5) . ? C24 C25 1.378(5) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C27 C28 1.484(5) . ? C28 C33 1.380(5) . ? C28 C29 1.385(5) . ? C29 C30 1.376(5) . ? C29 H29A 0.9300 . ? C30 C31 1.403(5) . ? C30 H30A 0.9300 . ? C31 C32 1.385(5) . ? C31 C31 1.491(6) 3 ? C32 C33 1.382(5) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? 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 O6 In1 O2 139.09(10) 4_665 . ? O6 In1 O4 127.63(10) 4_665 . ? O2 In1 O4 84.72(10) . . ? O6 In1 N2 113.96(11) 4_665 . ? O2 In1 N2 94.95(10) . . ? O4 In1 N2 78.23(10) . . ? O6 In1 O1 82.91(10) 4_665 . ? O2 In1 O1 57.01(8) . . ? O4 In1 O1 121.24(9) . . ? N2 In1 O1 140.04(9) . . ? O6 In1 O3 86.27(10) 4_665 . ? O2 In1 O3 95.26(9) . . ? O4 In1 O3 56.61(9) . . ? N2 In1 O3 132.32(9) . . ? O1 In1 O3 82.24(8) . . ? O6 In1 N1 82.44(10) 4_665 . ? O2 In1 N1 81.21(10) . . ? O4 In1 N1 143.65(10) . . ? N2 In1 N1 69.86(10) . . ? O1 In1 N1 77.47(9) . . ? O3 In1 N1 157.81(9) . . ? O6 In1 C13 110.53(11) 4_665 . ? O2 In1 C13 28.85(9) . . ? O4 In1 C13 105.44(10) . . ? N2 In1 C13 118.34(11) . . ? O1 In1 C13 28.25(9) . . ? O3 In1 C13 90.06(10) . . ? N1 In1 C13 76.24(10) . . ? O6 In1 C27 108.11(11) 4_665 . ? O2 In1 C27 89.75(10) . . ? O4 In1 C27 28.47(10) . . ? N2 In1 C27 105.69(11) . . ? O1 In1 C27 102.27(10) . . ? O3 In1 C27 28.14(10) . . ? N1 In1 C27 169.40(11) . . ? C13 In1 C27 98.42(11) . . ? C13 O1 In1 88.5(2) . . ? C13 O2 In1 94.8(2) . . ? C27 O3 In1 88.1(2) . . ? C27 O4 In1 95.7(2) . . ? C26 O6 In1 103.4(2) . 4_466 ? C12 N1 C1 117.8(3) . . ? C12 N1 In1 115.9(2) . . ? C1 N1 In1 125.8(2) . . ? C10 N2 C11 117.9(3) . . ? C10 N2 In1 124.0(2) . . ? C11 N2 In1 117.9(2) . . ? N1 C1 C2 123.9(4) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C3 C2 C1 118.3(4) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C3 C4 C12 117.1(4) . . ? C3 C4 C5 123.7(4) . . ? C12 C4 C5 119.1(4) . . ? C6 C5 C4 121.1(4) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 121.7(4) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C11 C7 C8 117.5(4) . . ? C11 C7 C6 119.1(4) . . ? C8 C7 C6 123.4(4) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C10 119.3(4) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? N2 C10 C9 123.1(4) . . ? N2 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? N2 C11 C7 122.9(3) . . ? N2 C11 C12 117.6(3) . . ? C7 C11 C12 119.5(3) . . ? N1 C12 C4 122.5(3) . . ? N1 C12 C11 118.1(3) . . ? C4 C12 C11 119.4(3) . . ? O1 C13 O2 119.3(3) . . ? O1 C13 C14 122.0(3) . . ? O2 C13 C14 118.6(3) . . ? O1 C13 In1 63.21(18) . . ? O2 C13 In1 56.37(17) . . ? C14 C13 In1 170.3(2) . . ? C19 C14 C15 118.7(3) . . ? C19 C14 C13 120.8(3) . . ? C15 C14 C13 120.4(3) . . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 121.2(4) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C18 C17 C16 117.6(3) . . ? C18 C17 C20 122.1(4) . . ? C16 C17 C20 120.3(3) . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C14 C19 C18 120.9(4) . . ? C14 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C21 C20 C25 117.3(4) . . ? C21 C20 C17 120.3(4) . . ? C25 C20 C17 122.5(4) . . ? C22 C21 C20 121.5(4) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C23 120.8(4) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C22 C23 C24 118.3(4) . . ? C22 C23 C26 119.7(4) . . ? C24 C23 C26 121.9(4) . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C24 C25 C20 121.6(4) . . ? C24 C25 H25A 119.2 . . ? C20 C25 H25A 119.2 . . ? O5 C26 O6 121.1(4) . . ? O5 C26 C23 121.2(4) . . ? O6 C26 C23 117.6(4) . . ? O3 C27 O4 119.6(3) . . ? O3 C27 C28 122.1(3) . . ? O4 C27 C28 118.2(3) . . ? O3 C27 In1 63.78(18) . . ? O4 C27 In1 55.85(17) . . ? C28 C27 In1 174.0(3) . . ? C33 C28 C29 117.8(3) . . ? C33 C28 C27 121.8(3) . . ? C29 C28 C27 120.3(3) . . ? C30 C29 C28 121.4(3) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C31 121.0(3) . . ? C29 C30 H30A 119.5 . . ? C31 C30 H30A 119.5 . . ? C32 C31 C30 117.0(3) . . ? C32 C31 C31 122.4(4) . 3 ? C30 C31 C31 120.7(4) . 3 ? C33 C32 C31 121.5(3) . . ? C33 C32 H32A 119.2 . . ? C31 C32 H32A 119.2 . . ? C28 C33 C32 121.2(3) . . ? C28 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.467 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.081 # Attachment '2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 832524' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H11 In O6' _chemical_formula_sum 'C14 H11 In O6' _chemical_formula_weight 390.05 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 Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 5.9716(12) _cell_length_b 28.516(6) _cell_length_c 7.5076(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1278.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 10580 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Hexagonal block' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7662 _exptl_absorpt_correction_T_max 0.8645 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10580 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1485 _reflns_number_gt 1336 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0855P)^2^+4.7326P] 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 1485 _refine_ls_number_parameters 107 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.018 _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 0.02292(7) 0.7500 0.08696(5) 0.0148(2) Uani 1 2 d S . . O1 O -0.0065(6) 0.67099(17) 0.0904(6) 0.0380(12) Uani 1 1 d . . . O2 O 0.3011(7) 0.69899(11) -0.0245(5) 0.0337(9) Uani 1 1 d . . . O3 O 0.1864(7) 0.7500 0.3300(6) 0.0197(9) Uani 1 2 d SD . . H3A H 0.082(18) 0.7500 0.408(15) 0.13(7) Uiso 1 2 d SD . . O4 O -0.0994(11) 0.7500 -0.1870(7) 0.0334(12) Uani 1 2 d SD . . H4A H -0.085(14) 0.7265(17) -0.255(8) 0.06(2) Uiso 1 1 d D . . C1 C 0.1852(9) 0.66435(15) 0.0281(7) 0.0258(10) Uani 1 1 d . . . C2 C 0.2782(8) 0.61573(14) 0.0146(6) 0.0228(10) Uani 1 1 d . . . C3 C 0.4849(9) 0.6075(2) -0.0620(8) 0.0318(13) Uani 1 1 d . . . H3B H 0.5673 0.6324 -0.1080 0.038 Uiso 1 1 calc R . . C4 C 0.5703(10) 0.56220(18) -0.0706(7) 0.0320(12) Uani 1 1 d . . . H4B H 0.7080 0.5570 -0.1251 0.038 Uiso 1 1 calc R . . C5 C 0.4527(8) 0.52428(15) 0.0014(6) 0.0208(9) Uani 1 1 d . . . C6 C 0.2452(9) 0.53351(17) 0.0792(6) 0.0263(11) Uani 1 1 d . . . H6A H 0.1635 0.5089 0.1284 0.032 Uiso 1 1 calc R . . C7 C 0.1583(9) 0.57866(17) 0.0848(6) 0.0271(11) Uani 1 1 d . . . H7A H 0.0188 0.5840 0.1360 0.033 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 In1 0.0140(3) 0.0139(3) 0.0167(3) 0.000 -0.00023(14) 0.000 O1 0.031(2) 0.021(2) 0.061(3) -0.0080(16) -0.0015(17) 0.0083(14) O2 0.054(2) 0.0155(15) 0.031(2) 0.0049(14) 0.0053(18) 0.0052(15) O3 0.0090(19) 0.035(2) 0.015(2) 0.000 -0.0007(16) 0.000 O4 0.051(3) 0.028(3) 0.021(3) 0.000 -0.011(2) 0.000 C1 0.038(3) 0.018(2) 0.021(2) -0.0022(18) -0.009(2) 0.0076(19) C2 0.031(2) 0.0144(19) 0.023(2) -0.0006(17) -0.0034(19) 0.0054(17) C3 0.036(3) 0.017(3) 0.042(3) 0.004(2) 0.011(2) 0.0011(18) C4 0.030(3) 0.019(2) 0.047(3) 0.003(2) 0.012(2) 0.004(2) C5 0.024(2) 0.015(2) 0.023(2) -0.0027(17) -0.0010(17) 0.0025(17) C6 0.029(3) 0.016(2) 0.034(3) 0.0019(17) 0.0053(19) 0.0006(18) C7 0.026(3) 0.021(2) 0.034(3) -0.0037(18) 0.0026(19) 0.0055(19) _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 O3 2.069(4) . ? In1 O3 2.104(4) 6_556 ? In1 O4 2.183(5) . ? In1 O1 2.260(5) 7_575 ? In1 O1 2.260(5) . ? In1 O2 2.361(4) . ? In1 O2 2.361(4) 7_575 ? O1 C1 1.251(6) . ? O2 C1 1.269(6) . ? O3 In1 2.104(4) 6_656 ? O3 H3A 0.86(2) . ? O4 H4A 0.84(2) . ? C1 C2 1.497(6) . ? C2 C3 1.382(7) . ? C2 C7 1.381(7) . ? C3 C4 1.391(7) . ? C3 H3B 0.9300 . ? C4 C5 1.398(7) . ? C4 H4B 0.9300 . ? C5 C6 1.395(7) . ? C5 C5 1.496(8) 5_665 ? C6 C7 1.389(7) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? 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 O3 In1 O3 100.91(9) . 6_556 ? O3 In1 O4 171.4(2) . . ? O3 In1 O4 87.7(2) 6_556 . ? O3 In1 O1 91.52(10) . 7_575 ? O3 In1 O1 85.54(10) 6_556 7_575 ? O4 In1 O1 89.13(11) . 7_575 ? O3 In1 O1 91.52(10) . . ? O3 In1 O1 85.54(10) 6_556 . ? O4 In1 O1 89.13(11) . . ? O1 In1 O1 170.98(19) 7_575 . ? O3 In1 O2 88.90(14) . . ? O3 In1 O2 140.98(9) 6_556 . ? O4 In1 O2 84.34(17) . . ? O1 In1 O2 132.29(13) 7_575 . ? O1 In1 O2 56.27(13) . . ? O3 In1 O2 88.90(14) . 7_575 ? O3 In1 O2 140.98(9) 6_556 7_575 ? O4 In1 O2 84.34(17) . 7_575 ? O1 In1 O2 56.27(13) 7_575 7_575 ? O1 In1 O2 132.29(13) . 7_575 ? O2 In1 O2 76.05(17) . 7_575 ? O3 In1 C1 88.54(12) . . ? O3 In1 C1 113.36(12) 6_556 . ? O4 In1 C1 88.02(13) . . ? O1 In1 C1 160.74(16) 7_575 . ? O1 In1 C1 27.92(15) . . ? O2 In1 C1 28.44(15) . . ? O2 In1 C1 104.48(15) 7_575 . ? O3 In1 C1 88.54(12) . 7_575 ? O3 In1 C1 113.36(12) 6_556 7_575 ? O4 In1 C1 88.02(13) . 7_575 ? O1 In1 C1 27.92(15) 7_575 7_575 ? O1 In1 C1 160.74(16) . 7_575 ? O2 In1 C1 104.48(15) . 7_575 ? O2 In1 C1 28.44(15) 7_575 7_575 ? C1 In1 C1 132.9(2) . 7_575 ? C1 O1 In1 94.3(3) . . ? C1 O2 In1 89.2(3) . . ? In1 O3 In1 135.4(2) . 6_656 ? In1 O3 H3A 105(10) . . ? In1 O3 H3A 120(10) 6_656 . ? In1 O4 H4A 122(5) . . ? O1 C1 O2 119.8(5) . . ? O1 C1 C2 120.3(5) . . ? O2 C1 C2 119.8(5) . . ? O1 C1 In1 57.8(3) . . ? O2 C1 In1 62.4(2) . . ? C2 C1 In1 174.4(4) . . ? C3 C2 C7 119.5(4) . . ? C3 C2 C1 121.1(5) . . ? C7 C2 C1 119.4(4) . . ? C2 C3 C4 120.2(5) . . ? C2 C3 H3B 119.9 . . ? C4 C3 H3B 119.9 . . ? C3 C4 C5 121.1(5) . . ? C3 C4 H4B 119.4 . . ? C5 C4 H4B 119.4 . . ? C6 C5 C4 117.5(4) . . ? C6 C5 C5 121.1(5) . 5_665 ? C4 C5 C5 121.4(5) . 5_665 ? C7 C6 C5 121.3(5) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C2 C7 C6 120.3(5) . . ? C2 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.150 _refine_diff_density_min -1.617 _refine_diff_density_rms 0.147 data_1 _database_code_depnum_ccdc_archive 'CCDC 832525' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C28 H16 In O8), 4(C H4 N0.50), 2(C2 N), O3, O0.50, 2(O0.25)' _chemical_formula_sum 'C30 H26 In N O9' _chemical_formula_weight 659.34 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd _symmetry_space_group_name_Hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 23.129(5) _cell_length_b 39.470(8) _cell_length_c 40.610(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 37073(13) _cell_formula_units_Z 32 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 54828 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'Octahedral block' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10688 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9180 _exptl_absorpt_correction_T_max 0.9277 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54828 _diffrn_reflns_av_R_equivalents 0.1357 _diffrn_reflns_av_sigmaI/netI 0.1778 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7904 _reflns_number_gt 3777 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The guest molecules are disordered. The occupied factors for N1, N2, C29, C30, C31, C32, O1w and O3wa are 0.5, while occupied factors for o2w and o3w are 0.25. Because of partial occupied guest molecules, the C-N bond lengths and thermal parameters for guest molecules are restrained. ; _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^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7904 _refine_ls_number_parameters 414 _refine_ls_number_restraints 143 _refine_ls_R_factor_all 0.1479 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1613 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _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 0.1250 -0.001341(8) 0.1250 0.05862(11) Uani 1 2 d SU . . In2 In -0.1250 -0.1250 0.137266(8) 0.06269(12) Uani 1 2 d SU . . O1 O 0.12597(14) 0.08511(7) 0.34804(7) 0.0969(10) Uani 1 1 d . . . O2 O 0.04151(13) 0.10229(6) 0.36414(6) 0.0812(9) Uani 1 1 d . . . O3 O -0.14711(15) -0.08597(7) 0.18099(7) 0.1045(7) Uani 1 1 d U . . O4 O -0.06132(14) -0.09323(6) 0.16256(7) 0.0887(7) Uani 1 1 d U . . O5 O 0.19754(15) 0.02871(7) 0.10315(7) 0.1073(9) Uani 1 1 d U . . O6 O 0.11686(16) 0.03670(8) 0.08169(8) 0.1181(13) Uani 1 1 d . . . O7 O 0.38825(13) 0.20873(7) -0.08373(7) 0.0924(10) Uani 1 1 d . . . O8 O 0.30225(13) 0.22103(6) -0.10078(6) 0.0770(7) Uani 1 1 d U . . C1 C 0.0788(2) 0.03681(11) 0.30564(12) 0.1088(17) Uani 1 1 d U . . H1A H 0.1186 0.0362 0.3091 0.131 Uiso 1 1 calc R . . C2 C 0.0536(3) 0.01481(11) 0.28359(13) 0.1141(19) Uani 1 1 d . . . H2A H 0.0768 -0.0007 0.2726 0.137 Uiso 1 1 calc R . . C3 C -0.0051(2) 0.01509(10) 0.27726(11) 0.0853(15) Uani 1 1 d . . . C4 C -0.0381(2) 0.03872(11) 0.29398(11) 0.1008(16) Uani 1 1 d . . . H4A H -0.0776 0.0403 0.2900 0.121 Uiso 1 1 calc R . . C5 C -0.0127(2) 0.05966(11) 0.31635(11) 0.0965(16) Uani 1 1 d . . . H5A H -0.0361 0.0747 0.3280 0.116 Uiso 1 1 calc R . . C6 C 0.0451(2) 0.05979(9) 0.32261(10) 0.0779(14) Uani 1 1 d . . . C7 C -0.1091(2) -0.04221(12) 0.23157(12) 0.1124(13) Uani 1 1 d U . . H7A H -0.1473 -0.0492 0.2331 0.135 Uiso 1 1 calc R . . C8 C -0.0853(2) -0.01993(11) 0.25446(12) 0.1116(17) Uani 1 1 d . . . H8A H -0.1085 -0.0122 0.2716 0.134 Uiso 1 1 calc R . . C9 C -0.0290(2) -0.00881(9) 0.25296(11) 0.0867(15) Uani 1 1 d . . . C10 C 0.0047(2) -0.02049(10) 0.22680(11) 0.0953(16) Uani 1 1 d . . . H10A H 0.0426 -0.0130 0.2246 0.114 Uiso 1 1 calc R . . C11 C -0.0177(2) -0.04327(9) 0.20394(11) 0.0890(15) Uani 1 1 d . . . H11A H 0.0057 -0.0514 0.1871 0.107 Uiso 1 1 calc R . . C12 C -0.0732(2) -0.05367(10) 0.20610(10) 0.0851(13) Uani 1 1 d U . . C13 C 0.0714(2) 0.08404(9) 0.34654(10) 0.0758(14) Uani 1 1 d . . . C14 C -0.0965(2) -0.07872(10) 0.18262(11) 0.0845(15) Uani 1 1 d . . . C15 C 0.2517(2) 0.07227(14) 0.05811(14) 0.156(2) Uani 1 1 d DU . . H15A H 0.2754 0.0624 0.0739 0.187 Uiso 1 1 calc R . . C16 C 0.2743(3) 0.09400(13) 0.03495(13) 0.1582(15) Uani 1 1 d DU . . H16A H 0.3142 0.0971 0.0351 0.190 Uiso 1 1 calc R . . C17 C 0.24350(18) 0.11133(9) 0.01191(10) 0.0812(13) Uani 1 1 d DU . . C18 C 0.1875(2) 0.10117(13) 0.01058(13) 0.148(2) Uani 1 1 d DU . . H18A H 0.1640 0.1102 -0.0058 0.177 Uiso 1 1 calc R . . C19 C 0.1637(3) 0.07807(13) 0.03228(12) 0.142(2) Uani 1 1 d DU . . H19A H 0.1256 0.0711 0.0292 0.171 Uiso 1 1 calc R . . C20 C 0.1940(2) 0.06548(10) 0.05764(10) 0.0892(15) Uani 1 1 d D . . C21 C 0.3439(2) 0.16897(12) -0.03203(12) 0.1134(18) Uani 1 1 d . . . H21A H 0.3823 0.1758 -0.0301 0.136 Uiso 1 1 calc R . . C22 C 0.3210(2) 0.14655(11) -0.00912(12) 0.1126(18) Uani 1 1 d . . . H22A H 0.3439 0.1390 0.0082 0.135 Uiso 1 1 calc R . . C23 C 0.2652(2) 0.13545(10) -0.01183(10) 0.0825(14) Uani 1 1 d . . . C24 C 0.2329(2) 0.14745(9) -0.03715(10) 0.0851(14) Uani 1 1 d . . . H24A H 0.1951 0.1397 -0.0395 0.102 Uiso 1 1 calc R . . C25 C 0.2544(2) 0.17116(10) -0.06013(10) 0.0848(14) Uani 1 1 d . . . H25A H 0.2306 0.1797 -0.0766 0.102 Uiso 1 1 calc R . . C26 C 0.3104(2) 0.18134(9) -0.05774(10) 0.0803(14) Uani 1 1 d . . . C27 C 0.1679(2) 0.04217(9) 0.08221(10) 0.0848(16) Uani 1 1 d . . . C28 C 0.3344(2) 0.20553(9) -0.08232(9) 0.0675(10) Uani 1 1 d U . . N1 N 0.1970(5) 0.0092(3) 0.2490(2) 0.172(2) Uani 0.50 1 d PDU . 1 C29 C 0.2540(6) 0.0096(4) 0.2372(4) 0.176(3) Uani 0.50 1 d PDU . 1 C30 C 0.2000(8) -0.0038(3) 0.2826(3) 0.180(3) Uani 0.50 1 d PDU . 1 N2 N 0.4622(6) 0.1089(3) -0.0786(2) 0.211(4) Uani 0.50 1 d PDU A 1 H2B H 0.4426 0.0892 -0.0786 0.253 Uiso 0.50 1 calc PR A 1 H2C H 0.4977 0.1050 -0.0867 0.253 Uiso 0.50 1 calc PR A 1 C31 C 0.4317(7) 0.1338(3) -0.0996(3) 0.187(4) Uani 0.50 1 d PDU A 1 H31A H 0.4342 0.1268 -0.1222 0.280 Uiso 0.50 1 calc PR A 1 H31B H 0.4494 0.1556 -0.0972 0.280 Uiso 0.50 1 calc PR A 1 H31C H 0.3919 0.1351 -0.0932 0.280 Uiso 0.50 1 calc PR A 1 C32 C 0.4669(8) 0.1215(4) -0.0450(3) 0.223(6) Uani 0.50 1 d PDU A 1 H32A H 0.4850 0.1046 -0.0315 0.334 Uiso 0.50 1 calc PR A 1 H32B H 0.4291 0.1264 -0.0366 0.334 Uiso 0.50 1 calc PR A 1 H32C H 0.4899 0.1417 -0.0449 0.334 Uiso 0.50 1 calc PR A 1 O1W O 0.1250 0.1250 0.1250 0.194(4) Uani 0.50 4 d SPU B 1 O2W O 0.2068 0.1250 0.1250 0.197(5) Uani 0.25 2 d SPU C 2 O3W O 0.3044(9) 0.0226(4) 0.1477(4) 0.1615(7) Uani 0.25 1 d PU D 1 O3WA O 0.3195(7) -0.0055(4) 0.1251(3) 0.2599(7) Uani 0.50 1 d PU E 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 0.0703(3) 0.05497(18) 0.0506(2) 0.000 0.0019(2) 0.000 In2 0.0729(3) 0.0612(2) 0.05404(19) 0.000 0.000 -0.0013(2) O1 0.085(2) 0.113(2) 0.093(2) -0.0334(16) -0.004(2) -0.0050(18) O2 0.094(2) 0.0755(15) 0.0746(17) -0.0229(13) 0.0024(16) -0.0086(15) O3 0.1084(9) 0.1056(14) 0.0995(14) -0.0482(10) -0.0147(12) 0.0006(16) O4 0.1115(10) 0.0786(13) 0.0759(17) -0.0114(11) -0.0025(10) -0.0229(11) O5 0.1176(14) 0.1080(17) 0.096(2) 0.0404(15) 0.0040(14) -0.0356(13) O6 0.121(3) 0.118(2) 0.115(2) 0.0524(18) 0.005(2) -0.016(2) O7 0.082(2) 0.1031(18) 0.0925(19) 0.0355(16) 0.0024(17) -0.0054(16) O8 0.1025(17) 0.0656(13) 0.0631(14) 0.0199(10) -0.0144(11) -0.0068(12) C1 0.093(4) 0.112(3) 0.122(3) -0.048(3) -0.010(3) 0.005(3) C2 0.115(4) 0.106(3) 0.121(4) -0.053(3) -0.007(3) 0.006(3) C3 0.088(3) 0.094(3) 0.074(3) -0.025(2) 0.009(3) -0.012(3) C4 0.088(4) 0.113(3) 0.101(3) -0.053(3) 0.003(3) -0.004(3) C5 0.084(4) 0.107(3) 0.099(3) -0.043(3) 0.010(3) 0.004(3) C6 0.084(3) 0.073(2) 0.077(3) -0.012(2) -0.008(3) 0.001(2) C7 0.098(2) 0.130(3) 0.1086(19) -0.048(2) 0.0139(15) -0.029(3) C8 0.094(4) 0.135(3) 0.106(3) -0.066(3) 0.014(3) -0.019(3) C9 0.081(3) 0.083(2) 0.096(3) -0.040(2) 0.001(3) -0.010(2) C10 0.089(3) 0.104(3) 0.093(3) -0.043(3) 0.012(3) -0.008(3) C11 0.091(4) 0.083(2) 0.093(3) -0.037(2) 0.011(3) -0.014(2) C12 0.104(3) 0.077(2) 0.074(2) -0.0231(19) -0.0058(18) -0.009(2) C13 0.099(4) 0.060(2) 0.069(2) -0.0043(19) -0.005(3) 0.003(2) C14 0.095(4) 0.083(3) 0.075(3) -0.005(2) -0.011(3) -0.002(3) C15 0.157(5) 0.171(4) 0.140(4) 0.080(3) -0.007(4) -0.039(4) C16 0.134(3) 0.187(3) 0.153(2) 0.079(2) -0.034(2) -0.013(3) C17 0.094(3) 0.073(2) 0.077(2) 0.0089(17) 0.009(2) -0.005(2) C18 0.154(5) 0.170(4) 0.119(4) 0.080(3) -0.019(3) -0.029(4) C19 0.127(4) 0.163(4) 0.136(4) 0.056(3) -0.003(4) -0.041(3) C20 0.108(4) 0.072(2) 0.088(3) 0.022(2) 0.022(3) 0.005(3) C21 0.087(4) 0.142(3) 0.112(3) 0.065(3) -0.028(3) -0.020(3) C22 0.106(4) 0.120(3) 0.112(4) 0.062(3) -0.004(3) -0.004(3) C23 0.096(4) 0.080(2) 0.072(3) 0.024(2) 0.007(3) -0.005(2) C24 0.087(3) 0.083(2) 0.085(3) 0.027(2) -0.010(3) -0.022(2) C25 0.089(3) 0.085(2) 0.080(3) 0.020(2) -0.016(3) -0.018(2) C26 0.101(4) 0.067(2) 0.074(3) 0.016(2) 0.007(3) -0.001(2) C27 0.126(4) 0.058(2) 0.070(3) 0.018(2) 0.015(3) -0.007(3) C28 0.080(2) 0.063(2) 0.060(2) 0.0155(15) -0.0048(16) -0.0089(17) N1 0.164(4) 0.175(4) 0.177(4) -0.018(4) 0.003(4) 0.010(4) C29 0.171(4) 0.176(4) 0.179(4) -0.026(4) 0.002(4) 0.000(4) C30 0.172(4) 0.183(4) 0.187(4) -0.022(4) 0.008(4) 0.001(4) N2 0.208(7) 0.208(6) 0.217(7) 0.001(6) 0.015(6) -0.015(6) C31 0.170(7) 0.195(6) 0.196(7) -0.004(6) 0.005(6) 0.017(6) C32 0.200(12) 0.237(11) 0.231(12) -0.020(10) 0.039(11) -0.001(11) O1W 0.280(8) 0.170(7) 0.132(7) 0.000 0.000 0.000 O2W 0.283(9) 0.172(8) 0.137(8) -0.002(7) 0.000 0.000 O3W 0.1616(9) 0.1614(10) 0.1614(10) 0.0001(7) -0.0003(7) 0.0001(7) O3WA 0.2599(9) 0.2600(10) 0.2599(10) 0.0001(7) -0.0001(7) 0.0000(7) _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 O8 2.234(3) 32_556 ? In1 O8 2.234(3) 30 ? In1 O5 2.238(3) . ? In1 O5 2.238(3) 11_454 ? In1 O6 2.320(3) 11_454 ? In1 O6 2.320(3) . ? In1 O7 2.321(3) 32_556 ? In1 O7 2.321(3) 30 ? In2 O4 2.190(3) 2_445 ? In2 O4 2.190(3) . ? In2 O1 2.240(3) 24 ? In2 O1 2.240(3) 27 ? In2 O2 2.327(3) 27 ? In2 O2 2.327(3) 24 ? In2 O3 2.406(3) 2_445 ? In2 O3 2.406(3) . ? O1 C13 1.263(6) . ? O1 In2 2.240(3) 19_656 ? O2 C13 1.229(5) . ? O2 In2 2.327(3) 19_656 ? O3 C14 1.207(6) . ? O4 C14 1.286(5) . ? O5 C27 1.215(5) . ? O6 C27 1.200(6) . ? O7 C28 1.253(5) . ? O7 In1 2.321(3) 18_665 ? O8 C28 1.220(4) . ? O8 In1 2.234(3) 18_665 ? C1 C2 1.377(6) . ? C1 C6 1.381(6) . ? C1 H1A 0.9300 . ? C2 C3 1.383(7) . ? C2 H2A 0.9300 . ? C3 C4 1.383(6) . ? C3 C9 1.472(6) . ? C4 C5 1.362(6) . ? C4 H4A 0.9300 . ? C5 C6 1.360(6) . ? C5 H5A 0.9300 . ? C6 C13 1.494(6) . ? C7 C8 1.393(6) . ? C7 C12 1.401(6) . ? C7 H7A 0.9300 . ? C8 C9 1.376(7) . ? C8 H8A 0.9300 . ? C9 C10 1.395(6) . ? C10 C11 1.392(6) . ? C10 H10A 0.9300 . ? C11 C12 1.349(6) . ? C11 H11A 0.9300 . ? C12 C14 1.476(6) . ? C15 C20 1.360(6) . ? C15 C16 1.376(6) . ? C15 H15A 0.9300 . ? C16 C17 1.360(6) . ? C16 H16A 0.9300 . ? C17 C18 1.357(6) . ? C17 C23 1.445(5) . ? C18 C19 1.383(6) . ? C18 H18A 0.9300 . ? C19 C20 1.342(6) . ? C19 H19A 0.9300 . ? C20 C27 1.486(6) . ? C21 C26 1.389(6) . ? C21 C22 1.389(6) . ? C21 H21A 0.9300 . ? C22 C23 1.368(7) . ? C22 H22A 0.9300 . ? C23 C24 1.356(6) . ? C24 C25 1.411(5) . ? C24 H24A 0.9300 . ? C25 C26 1.361(6) . ? C25 H25A 0.9300 . ? C26 C28 1.489(5) . ? N1 C29 1.403(14) . ? N1 C30 1.458(13) . ? N1 C29 1.465(17) 25 ? C29 N1 1.465(17) 25 ? N2 C32 1.454(13) . ? N2 C31 1.481(13) . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? 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 O8 In1 O8 121.54(13) 32_556 30 ? O8 In1 O5 82.45(11) 32_556 . ? O8 In1 O5 130.46(10) 30 . ? O8 In1 O5 130.46(10) 32_556 11_454 ? O8 In1 O5 82.45(11) 30 11_454 ? O5 In1 O5 115.99(16) . 11_454 ? O8 In1 O6 85.47(11) 32_556 11_454 ? O8 In1 O6 135.32(11) 30 11_454 ? O5 In1 O6 84.07(12) . 11_454 ? O5 In1 O6 54.36(12) 11_454 11_454 ? O8 In1 O6 135.32(11) 32_556 . ? O8 In1 O6 85.47(11) 30 . ? O5 In1 O6 54.36(12) . . ? O5 In1 O6 84.07(12) 11_454 . ? O6 In1 O6 99.34(17) 11_454 . ? O8 In1 O7 56.62(10) 32_556 32_556 ? O8 In1 O7 83.51(10) 30 32_556 ? O5 In1 O7 138.17(11) . 32_556 ? O5 In1 O7 88.55(11) 11_454 32_556 ? O6 In1 O7 84.42(11) 11_454 32_556 ? O6 In1 O7 167.45(12) . 32_556 ? O8 In1 O7 83.51(10) 32_556 30 ? O8 In1 O7 56.62(10) 30 30 ? O5 In1 O7 88.55(11) . 30 ? O5 In1 O7 138.17(11) 11_454 30 ? O6 In1 O7 167.45(12) 11_454 30 ? O6 In1 O7 84.42(11) . 30 ? O7 In1 O7 94.46(15) 32_556 30 ? O8 In1 C28 27.89(11) 32_556 32_556 ? O8 In1 C28 104.21(11) 30 32_556 ? O5 In1 C28 109.88(13) . 32_556 ? O5 In1 C28 110.65(12) 11_454 32_556 ? O6 In1 C28 83.64(12) 11_454 32_556 ? O6 In1 C28 163.08(13) . 32_556 ? O7 In1 C28 28.74(12) 32_556 32_556 ? O7 In1 C28 89.38(11) 30 32_556 ? O8 In1 C28 104.21(11) 32_556 30 ? O8 In1 C28 27.89(11) 30 30 ? O5 In1 C28 110.65(12) . 30 ? O5 In1 C28 109.88(13) 11_454 30 ? O6 In1 C28 163.08(13) 11_454 30 ? O6 In1 C28 83.64(12) . 30 ? O7 In1 C28 89.38(11) 32_556 30 ? O7 In1 C28 28.74(12) 30 30 ? C28 In1 C28 98.37(16) 32_556 30 ? O8 In1 C27 108.13(12) 32_556 11_454 ? O8 In1 C27 108.96(14) 30 11_454 ? O5 In1 C27 101.43(13) . 11_454 ? O5 In1 C27 27.32(14) 11_454 11_454 ? O6 In1 C27 27.07(14) 11_454 11_454 ? O6 In1 C27 92.72(12) . 11_454 ? O7 In1 C27 85.23(11) 32_556 11_454 ? O7 In1 C27 165.42(14) 30 11_454 ? C28 In1 C27 97.05(13) 32_556 11_454 ? C28 In1 C27 136.77(16) 30 11_454 ? O8 In1 C27 108.96(14) 32_556 . ? O8 In1 C27 108.13(12) 30 . ? O5 In1 C27 27.32(14) . . ? O5 In1 C27 101.43(13) 11_454 . ? O6 In1 C27 92.72(12) 11_454 . ? O6 In1 C27 27.07(14) . . ? O7 In1 C27 165.42(14) 32_556 . ? O7 In1 C27 85.23(11) 30 . ? C28 In1 C27 136.77(16) 32_556 . ? C28 In1 C27 97.05(13) 30 . ? C27 In1 C27 98.72(18) 11_454 . ? O4 In2 O4 124.06(15) 2_445 . ? O4 In2 O1 85.66(11) 2_445 24 ? O4 In2 O1 137.97(11) . 24 ? O4 In2 O1 137.97(11) 2_445 27 ? O4 In2 O1 85.66(11) . 27 ? O1 In2 O1 89.34(15) 24 27 ? O4 In2 O2 81.47(10) 2_445 27 ? O4 In2 O2 121.79(10) . 27 ? O1 In2 O2 88.59(10) 24 27 ? O1 In2 O2 56.67(10) 27 27 ? O4 In2 O2 121.79(10) 2_445 24 ? O4 In2 O2 81.47(10) . 24 ? O1 In2 O2 56.67(10) 24 24 ? O1 In2 O2 88.59(10) 27 24 ? O2 In2 O2 132.39(13) 27 24 ? O4 In2 O3 55.26(11) 2_445 2_445 ? O4 In2 O3 82.96(10) . 2_445 ? O1 In2 O3 94.41(11) 24 2_445 ? O1 In2 O3 166.63(12) 27 2_445 ? O2 In2 O3 136.13(10) 27 2_445 ? O2 In2 O3 82.81(10) 24 2_445 ? O4 In2 O3 82.96(10) 2_445 . ? O4 In2 O3 55.26(11) . . ? O1 In2 O3 166.63(12) 24 . ? O1 In2 O3 94.41(11) 27 . ? O2 In2 O3 82.81(10) 27 . ? O2 In2 O3 136.13(10) 24 . ? O3 In2 O3 84.87(15) 2_445 . ? O4 In2 C13 105.09(11) 2_445 24 ? O4 In2 C13 109.33(13) . 24 ? O1 In2 C13 28.75(12) 24 24 ? O1 In2 C13 88.86(11) 27 24 ? O2 In2 C13 112.01(12) 27 24 ? O2 In2 C13 27.92(12) 24 24 ? O3 In2 C13 88.30(11) 2_445 24 ? O3 In2 C13 163.79(13) . 24 ? O4 In2 C13 109.33(13) 2_445 27 ? O4 In2 C13 105.09(11) . 27 ? O1 In2 C13 88.86(11) 24 27 ? O1 In2 C13 28.75(12) 27 27 ? O2 In2 C13 27.92(12) 27 27 ? O2 In2 C13 112.01(12) 24 27 ? O3 In2 C13 163.79(13) 2_445 27 ? O3 In2 C13 88.30(11) . 27 ? C13 In2 C13 101.84(18) 24 27 ? O4 In2 C14 28.45(13) 2_445 2_445 ? O4 In2 C14 103.52(13) . 2_445 ? O1 In2 C14 90.41(12) 24 2_445 ? O1 In2 C14 166.30(14) 27 2_445 ? O2 In2 C14 109.64(13) 27 2_445 ? O2 In2 C14 102.67(12) 24 2_445 ? O3 In2 C14 26.81(13) 2_445 2_445 ? O3 In2 C14 82.92(11) . 2_445 ? C13 In2 C14 97.45(12) 24 2_445 ? C13 In2 C14 137.56(16) 27 2_445 ? O4 In2 C14 103.52(13) 2_445 . ? O4 In2 C14 28.45(13) . . ? O1 In2 C14 166.31(14) 24 . ? O1 In2 C14 90.41(12) 27 . ? O2 In2 C14 102.67(12) 27 . ? O2 In2 C14 109.64(13) 24 . ? O3 In2 C14 82.92(11) 2_445 . ? O3 In2 C14 26.81(13) . . ? C13 In2 C14 137.56(16) 24 . ? C13 In2 C14 97.45(13) 27 . ? C14 In2 C14 93.04(19) 2_445 . ? C13 O1 In2 92.7(2) . 19_656 ? C13 O2 In2 89.6(3) . 19_656 ? C14 O3 In2 89.2(3) . . ? C14 O4 In2 97.3(3) . . ? C27 O5 In1 94.9(3) . . ? C27 O6 In1 91.3(3) . . ? C28 O7 In1 88.3(2) . 18_665 ? C28 O8 In1 93.2(3) . 18_665 ? C2 C1 C6 119.9(5) . . ? C2 C1 H1A 120.0 . . ? C6 C1 H1A 120.0 . . ? C1 C2 C3 122.2(5) . . ? C1 C2 H2A 118.9 . . ? C3 C2 H2A 118.9 . . ? C2 C3 C4 117.1(4) . . ? C2 C3 C9 119.2(4) . . ? C4 C3 C9 123.7(5) . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C6 C5 C4 123.4(4) . . ? C6 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C5 C6 C1 117.4(4) . . ? C5 C6 C13 121.7(4) . . ? C1 C6 C13 120.9(4) . . ? C8 C7 C12 117.5(5) . . ? C8 C7 H7A 121.2 . . ? C12 C7 H7A 121.2 . . ? C9 C8 C7 123.1(5) . . ? C9 C8 H8A 118.5 . . ? C7 C8 H8A 118.5 . . ? C8 C9 C10 117.1(4) . . ? C8 C9 C3 121.9(4) . . ? C10 C9 C3 120.9(4) . . ? C11 C10 C9 120.9(5) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C7 120.9(4) . . ? C11 C12 C14 120.6(4) . . ? C7 C12 C14 118.5(5) . . ? O2 C13 O1 121.0(4) . . ? O2 C13 C6 121.6(4) . . ? O1 C13 C6 117.4(4) . . ? O2 C13 In2 62.5(2) . 19_656 ? O1 C13 In2 58.5(2) . 19_656 ? C6 C13 In2 175.9(3) . 19_656 ? O3 C14 O4 118.2(4) . . ? O3 C14 C12 123.3(4) . . ? O4 C14 C12 118.5(5) . . ? O3 C14 In2 64.0(2) . . ? O4 C14 In2 54.3(2) . . ? C12 C14 In2 172.7(4) . . ? C20 C15 C16 119.1(5) . . ? C20 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C17 C16 C15 125.7(6) . . ? C17 C16 H16A 117.1 . . ? C15 C16 H16A 117.1 . . ? C18 C17 C16 112.3(4) . . ? C18 C17 C23 120.0(4) . . ? C16 C17 C23 127.5(5) . . ? C17 C18 C19 123.4(5) . . ? C17 C18 H18A 118.3 . . ? C19 C18 H18A 118.3 . . ? C20 C19 C18 121.7(5) . . ? C20 C19 H19A 119.2 . . ? C18 C19 H19A 119.2 . . ? C19 C20 C15 116.8(5) . . ? C19 C20 C27 122.2(5) . . ? C15 C20 C27 120.7(4) . . ? C26 C21 C22 121.0(5) . . ? C26 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 118.0(4) . . ? C24 C23 C17 123.0(4) . . ? C22 C23 C17 119.0(4) . . ? C23 C24 C25 122.7(4) . . ? C23 C24 H24A 118.7 . . ? C25 C24 H24A 118.7 . . ? C26 C25 C24 118.9(4) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C25 C26 C21 118.8(4) . . ? C25 C26 C28 119.8(4) . . ? C21 C26 C28 121.5(4) . . ? O6 C27 O5 119.3(4) . . ? O6 C27 C20 120.0(4) . . ? O5 C27 C20 120.8(5) . . ? O6 C27 In1 61.6(2) . . ? O5 C27 In1 57.7(2) . . ? C20 C27 In1 177.4(3) . . ? O8 C28 O7 121.8(4) . . ? O8 C28 C26 120.4(4) . . ? O7 C28 C26 117.7(4) . . ? O8 C28 In1 58.9(2) . 18_665 ? O7 C28 In1 63.0(2) . 18_665 ? C26 C28 In1 179.0(3) . 18_665 ? C29 N1 C30 106.2(12) . . ? C29 N1 C29 53.8(11) . 25 ? C30 N1 C29 55.1(9) . 25 ? C29 C29 C30 119.3(17) 25 25 ? C29 C29 N1 65.5(11) 25 . ? C30 C29 N1 160.2(15) 25 . ? C29 C29 N1 60.6(11) 25 25 ? C30 C29 N1 62.2(9) 25 25 ? N1 C29 N1 126.2(11) . 25 ? C29 C30 N1 62.8(9) 25 . ? C32 N2 C31 110.5(11) . . ? C32 N2 H2B 109.5 . . ? C31 N2 H2B 109.5 . . ? C32 N2 H2C 109.5 . . ? C31 N2 H2C 109.5 . . ? H2B N2 H2C 108.1 . . ? N2 C31 H31A 109.5 . . ? N2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.469 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.071