# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1894 data_97019c _audit_creation_date 1999-10-19T20:00:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category 'Full Article' _publ_contact_author_address ; Department of Civil Engineering and Geological Sciences University of Notre Dame Notre Dame, IN 46656 ; _publ_contact_author_email ccahill@nd.edu _publ_requested_journal 'Dalton Transactions' _publ_section_title 'On the formation of framework indium-sulfides' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C4 H12 In10 N S18' _chemical_formula_weight 1799.43 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 19.63980 _cell_length_b 19.63980 _cell_length_c 31.8342(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 12279.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 24.95 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'Trigonal antiprism' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.947 _exptl_crystal_F_000 6568 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.297 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.954 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 58366 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 24.95 _reflns_number_total 10569 _reflns_number_gt 7889 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'SAINT V5.1 (Bruker-AXS, 1998)' _computing_molecular_graphics 'Wingx (Farrugia, 1998)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Considerable void space is found within the extraframework region of this structure. One ordered DEA cation is contained in the model. Severe disorder prevented locating any other ordered cations. The program SQUEEZE (Sluis, P. v.d.; Spek, A. L. Acta Crystallogr., Sect A 1990, 46, 194-201) was used to examine the void. It was determined that 43.9% of the volume of the unit cell, or 5394.4 A^3, was void space. A volume of this size could potentially host 7 DEA cations. The data were treated and the effects of the disordered solvent were removed. Thus the chemical formula reported herein contains only ordered solvent species. It is assumed that 5 other DEA cations are hosted within the voids for charge balance. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^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_extinction_method none _refine_ls_number_reflns 10569 _refine_ls_number_parameters 274 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_gt 0.071 _refine_ls_wR_factor_all 0.074 _refine_ls_goodness_of_fit_gt 1.131 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/su_max -0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.17(4) _refine_diff_density_max 0.702 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.125 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group In1 In 0.75546(4) 0.39530(4) 0.00018(2) 0.0322(2) Uani 1 d . . In2 In 0.74363(4) 0.24870(4) -0.09207(2) 0.0339(2) Uani 1 d . . In3 In 0.68634(4) 0.10588(3) -0.00323(2) 0.0318(2) Uani 1 d . . In4 In 0.69841(4) 0.25330(4) 0.09039(2) 0.0302(2) Uani 1 d . . In5 In 0.63724(4) 0.41800(4) -0.09753(2) 0.0360(2) Uani 1 d . . In6 In 0.57889(4) 0.28337(4) -0.01304(2) 0.0320(2) Uani 1 d . . In7 In 0.53245(4) 0.14356(4) 0.07177(2) 0.0334(2) Uani 1 d . . In8 In 0.86935(4) 0.36065(4) 0.09917(2) 0.0347(2) Uani 1 d . . In9 In 0.86237(4) 0.21671(4) 0.01436(2) 0.0311(2) Uani 1 d . . In10 In 0.84618(4) 0.07895(4) -0.07533(2) 0.0338(2) Uani 1 d . . S1 S 0.8325(2) 0.45017(14) 0.04909(9) 0.0480(8) Uani 1 d . . S2 S 0.82153(13) 0.30411(14) -0.03844(8) 0.0359(7) Uani 1 d . . S3 S 0.8078(2) 0.1616(2) -0.12963(9) 0.0541(9) Uani 1 d . . S4 S 0.75009(15) 0.01865(14) -0.04172(9) 0.0490(8) Uani 1 d . . S5 S 0.76216(13) 0.16208(13) 0.05097(8) 0.0345(7) Uani 1 d . . S6 S 0.77300(14) 0.31115(14) 0.14050(8) 0.0400(7) Uani 1 d . . S7 S 0.59935(14) 0.20536(15) 0.12556(9) 0.0445(8) Uani 1 d . . S8 S 0.65578(13) 0.34205(13) 0.03913(8) 0.0345(7) Uani 1 d . . S9 S 0.71496(15) 0.48039(14) -0.04979(9) 0.0453(8) Uani 1 d . . S10 S 0.7017(2) 0.3351(2) -0.14045(8) 0.0507(9) Uani 1 d . . S11 S 0.64399(13) 0.19526(14) -0.05432(8) 0.0365(7) Uani 1 d . . S12 S 0.59411(15) 0.05125(14) 0.03367(10) 0.0491(8) Uani 1 d . . S13 S 0.48253(14) 0.22662(15) 0.02058(9) 0.0466(8) Uani 1 d . . S14 S 0.53667(14) 0.37157(15) -0.05977(9) 0.0471(8) Uani 1 d . . S15 S 0.94106(14) 0.42574(14) 0.14753(9) 0.0463(8) Uani 1 d . . S16 S 0.93697(14) 0.26990(14) 0.06535(9) 0.0483(8) Uani 1 d . . S17 S 0.92464(13) 0.12535(14) -0.02035(8) 0.0386(7) Uani 1 d . . S18 S 0.92663(14) -0.00160(15) -0.10760(9) 0.0456(8) Uani 1 d . . C11 C 1.1153(13) 0.0820(11) -0.0527(7) 0.285(15) Uiso 1 d D . H11A H 1.1202(13) 0.0337(11) -0.0560(7) 0.428 Uiso 1 d R . H11B H 1.0831(13) 0.0914(11) -0.0308(7) 0.428 Uiso 1 d R . H11C H 1.1586(13) 0.1016(11) -0.0455(7) 0.428 Uiso 1 d R . C12 C 1.0895(15) 0.1139(11) -0.0952(7) 0.333(18) Uiso 1 d D . H12A H 1.1277(15) 0.1216(11) -0.1139(7) 0.4 Uiso 1 calc R . H12B H 1.0580(15) 0.0829(11) -0.1088(7) 0.4 Uiso 1 calc R . N11 N 1.0546(7) 0.1801(7) -0.0858(5) 0.169(7) Uiso 1 d D . H11C H 1.0867(7) 0.2116(7) -0.0805(5) 0.203 Uiso 1 calc R . H11D H 1.0300(7) 0.1749(7) -0.0622(5) 0.203 Uiso 1 calc R . C13 C 1.0084(8) 0.2073(8) -0.1195(4) 0.143(7) Uiso 1 d D . H13A H 0.9732(8) 0.1742(8) -0.1259(4) 0.172 Uiso 1 calc R . H13B H 1.0342(8) 0.2160(8) -0.1449(4) 0.172 Uiso 1 calc R . C14 C 0.9756(9) 0.2748(8) -0.1031(5) 0.163(8) Uiso 1 d D . H14A H 0.9269(9) 0.2715(8) -0.1050(5) 0.245 Uiso 1 d R . H14B H 0.9911(9) 0.3123(8) -0.1200(5) 0.245 Uiso 1 d R . H14C H 0.9887(9) 0.2821(8) -0.0744(5) 0.245 Uiso 1 d 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 0.0327(4) 0.0326(4) 0.0314(4) 0.0023(4) -0.0053(4) 0.0001(4) In2 0.0333(5) 0.0371(5) 0.0314(4) 0.0022(4) 0.0000(4) 0.0037(4) In3 0.0278(4) 0.0322(4) 0.0353(4) -0.0028(4) 0.0042(4) 0.0000(4) In4 0.0302(4) 0.0315(4) 0.0289(4) 0.0000(4) 0.0022(3) -0.0017(4) In5 0.0348(5) 0.0362(5) 0.0370(4) 0.0118(4) -0.0035(4) 0.0002(4) In6 0.0282(4) 0.0334(4) 0.0344(5) 0.0079(4) -0.0002(3) 0.0007(4) In7 0.0300(4) 0.0339(5) 0.0363(5) 0.0019(4) 0.0067(4) -0.0026(4) In8 0.0315(5) 0.0340(5) 0.0385(4) -0.0016(4) -0.0088(4) -0.0005(4) In9 0.0270(4) 0.0345(5) 0.0317(4) -0.0048(3) -0.0004(4) 0.0034(3) In10 0.0320(5) 0.0346(5) 0.0348(4) -0.0073(4) 0.0053(4) 0.0014(4) S1 0.058(2) 0.039(2) 0.047(2) 0.0001(15) -0.016(2) -0.0046(15) S2 0.031(2) 0.043(2) 0.034(2) 0.0049(14) -0.0005(13) 0.0033(14) S3 0.059(2) 0.069(2) 0.034(2) -0.006(2) 0.002(2) 0.022(2) S4 0.043(2) 0.043(2) 0.061(2) -0.011(2) 0.018(2) 0.001(2) S5 0.039(2) 0.033(2) 0.0316(15) -0.0013(12) 0.0027(13) 0.0056(13) S6 0.039(2) 0.043(2) 0.037(2) -0.0042(14) -0.0058(14) -0.0068(14) S7 0.043(2) 0.054(2) 0.036(2) -0.0003(15) 0.0096(14) -0.0125(15) S8 0.033(2) 0.038(2) 0.032(2) 0.0085(13) 0.0004(13) -0.0026(13) S9 0.048(2) 0.038(2) 0.050(2) 0.0154(15) -0.013(2) -0.0023(14) S10 0.059(2) 0.061(2) 0.032(2) 0.0106(15) -0.0015(15) 0.019(2) S11 0.030(2) 0.042(2) 0.037(2) 0.0049(14) 0.0025(13) 0.0033(14) S12 0.041(2) 0.037(2) 0.069(2) -0.006(2) 0.020(2) -0.0084(15) S13 0.027(2) 0.052(2) 0.061(2) 0.016(2) -0.0059(15) -0.0036(14) S14 0.037(2) 0.044(2) 0.060(2) 0.018(2) -0.001(2) 0.0025(14) S15 0.038(2) 0.045(2) 0.057(2) -0.003(2) -0.026(2) 0.0014(15) S16 0.037(2) 0.047(2) 0.061(2) -0.020(2) -0.017(2) 0.0072(14) S17 0.033(2) 0.045(2) 0.038(2) -0.0137(14) 0.0024(13) 0.0040(13) S18 0.039(2) 0.047(2) 0.050(2) -0.026(2) -0.002(2) 0.0018(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 2.423(3) . ? In1 S9 2.441(3) . ? In1 S2 2.530(3) . ? In1 S8 2.542(3) . ? In2 S10 2.435(3) . ? In2 S3 2.438(3) . ? In2 S11 2.525(3) . ? In2 S2 2.538(3) . ? In3 S12 2.411(3) . ? In3 S4 2.450(3) . ? In3 S5 2.532(3) . ? In3 S11 2.533(3) . ? In4 S7 2.434(3) . ? In4 S6 2.446(3) . ? In4 S5 2.520(3) . ? In4 S8 2.530(3) . ? In5 S18 2.471(3) 5_654 ? In5 S10 2.474(3) . ? In5 S9 2.478(3) . ? In5 S14 2.486(3) . ? In6 S14 2.429(3) . ? In6 S13 2.443(3) . ? In6 S11 2.521(3) . ? In6 S8 2.523(3) . ? In7 S15 2.456(3) 6_455 ? In7 S7 2.476(3) . ? In7 S12 2.495(3) . ? In7 S13 2.506(3) . ? In8 S15 2.447(3) . ? In8 S16 2.470(3) . ? In8 S1 2.482(3) . ? In8 S6 2.501(3) . ? In9 S16 2.424(3) . ? In9 S17 2.436(3) . ? In9 S5 2.526(3) . ? In9 S2 2.533(3) . ? In10 S18 2.460(3) . ? In10 S4 2.472(3) . ? In10 S3 2.488(3) . ? In10 S17 2.504(3) . ? S15 In7 2.456(3) 6 ? S18 In5 2.471(3) 5_644 ? C11 C12 1.57(2) . ? C12 N11 1.499(5) . ? N11 C13 1.502(4) . ? C13 C14 1.56(2) . ? 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 S1 In1 S9 108.52(10) . . ? S1 In1 S2 107.87(10) . . ? S9 In1 S2 109.57(10) . . ? S1 In1 S8 110.50(10) . . ? S9 In1 S8 110.41(9) . . ? S2 In1 S8 109.91(9) . . ? S10 In2 S3 110.70(10) . . ? S10 In2 S11 109.18(10) . . ? S3 In2 S11 110.00(10) . . ? S10 In2 S2 109.30(10) . . ? S3 In2 S2 108.63(10) . . ? S11 In2 S2 108.98(9) . . ? S12 In3 S4 108.44(10) . . ? S12 In3 S5 107.69(10) . . ? S4 In3 S5 110.18(10) . . ? S12 In3 S11 112.00(10) . . ? S4 In3 S11 109.34(10) . . ? S5 In3 S11 109.18(9) . . ? S7 In4 S6 111.00(9) . . ? S7 In4 S5 110.55(9) . . ? S6 In4 S5 110.94(9) . . ? S7 In4 S8 107.38(9) . . ? S6 In4 S8 107.39(9) . . ? S5 In4 S8 109.44(9) . . ? S18 In5 S10 111.16(10) 5_654 . ? S18 In5 S9 110.56(10) 5_654 . ? S10 In5 S9 110.42(10) . . ? S18 In5 S14 96.35(9) 5_654 . ? S10 In5 S14 115.62(10) . . ? S9 In5 S14 111.97(10) . . ? S14 In6 S13 109.22(10) . . ? S14 In6 S11 110.09(10) . . ? S13 In6 S11 107.95(10) . . ? S14 In6 S8 106.35(10) . . ? S13 In6 S8 112.55(9) . . ? S11 In6 S8 110.67(9) . . ? S15 In7 S7 112.60(10) 6_455 . ? S15 In7 S12 98.37(9) 6_455 . ? S7 In7 S12 115.78(10) . . ? S15 In7 S13 109.50(10) 6_455 . ? S7 In7 S13 109.78(10) . . ? S12 In7 S13 110.29(11) . . ? S15 In8 S16 109.98(9) . . ? S15 In8 S1 101.66(10) . . ? S16 In8 S1 112.84(10) . . ? S15 In8 S6 107.91(10) . . ? S16 In8 S6 110.83(10) . . ? S1 In8 S6 113.11(10) . . ? S16 In9 S17 108.53(9) . . ? S16 In9 S5 110.18(10) . . ? S17 In9 S5 106.71(9) . . ? S16 In9 S2 110.11(10) . . ? S17 In9 S2 110.93(9) . . ? S5 In9 S2 110.32(9) . . ? S18 In10 S4 111.28(10) . . ? S18 In10 S3 108.90(10) . . ? S4 In10 S3 112.44(11) . . ? S18 In10 S17 97.51(9) . . ? S4 In10 S17 109.99(10) . . ? S3 In10 S17 115.78(10) . . ? In1 S1 In8 106.25(11) . . ? In1 S2 In9 108.65(10) . . ? In1 S2 In2 108.74(10) . . ? In9 S2 In2 110.29(10) . . ? In2 S3 In10 105.88(11) . . ? In3 S4 In10 105.76(11) . . ? In4 S5 In9 108.35(10) . . ? In4 S5 In3 110.91(10) . . ? In9 S5 In3 109.20(10) . . ? In4 S6 In8 106.89(10) . . ? In4 S7 In7 107.19(10) . . ? In6 S8 In4 107.94(10) . . ? In6 S8 In1 109.13(9) . . ? In4 S8 In1 110.07(10) . . ? In1 S9 In5 105.19(10) . . ? In2 S10 In5 106.40(10) . . ? In6 S11 In2 110.85(10) . . ? In6 S11 In3 107.90(10) . . ? In2 S11 In3 109.82(10) . . ? In3 S12 In7 106.15(11) . . ? In6 S13 In7 106.19(10) . . ? In6 S14 In5 106.65(11) . . ? In8 S15 In7 112.43(11) . 6 ? In9 S16 In8 106.14(10) . . ? In9 S17 In10 106.03(10) . . ? In10 S18 In5 109.04(11) . 5_644 ? N11 C12 C11 108.8(11) . . ? C12 N11 C13 116.3(17) . . ? N11 C13 C14 108.2(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S9 In1 S1 In8 179.07(11) . . . . ? S2 In1 S1 In8 -62.29(13) . . . . ? S8 In1 S1 In8 57.88(14) . . . . ? S15 In8 S1 In1 -177.26(11) . . . . ? S16 In8 S1 In1 65.00(14) . . . . ? S6 In8 S1 In1 -61.82(14) . . . . ? S1 In1 S2 In9 62.19(12) . . . . ? S9 In1 S2 In9 -179.84(10) . . . . ? S8 In1 S2 In9 -58.35(12) . . . . ? S1 In1 S2 In2 -177.74(10) . . . . ? S9 In1 S2 In2 -59.78(12) . . . . ? S8 In1 S2 In2 61.71(11) . . . . ? S16 In9 S2 In1 -61.06(12) . . . . ? S17 In9 S2 In1 178.79(9) . . . . ? S5 In9 S2 In1 60.76(12) . . . . ? S16 In9 S2 In2 179.84(10) . . . . ? S17 In9 S2 In2 59.69(12) . . . . ? S5 In9 S2 In2 -58.34(12) . . . . ? S10 In2 S2 In1 58.61(12) . . . . ? S3 In2 S2 In1 179.50(10) . . . . ? S11 In2 S2 In1 -60.65(12) . . . . ? S10 In2 S2 In9 177.65(10) . . . . ? S3 In2 S2 In9 -61.46(13) . . . . ? S11 In2 S2 In9 58.39(12) . . . . ? S10 In2 S3 In10 179.86(11) . . . . ? S11 In2 S3 In10 -59.38(13) . . . . ? S2 In2 S3 In10 59.83(14) . . . . ? S18 In10 S3 In2 -171.13(10) . . . . ? S4 In10 S3 In2 65.06(14) . . . . ? S17 In10 S3 In2 -62.54(14) . . . . ? S12 In3 S4 In10 -177.27(11) . . . . ? S5 In3 S4 In10 -59.64(13) . . . . ? S11 In3 S4 In10 60.36(13) . . . . ? S18 In10 S4 In3 171.90(10) . . . . ? S3 In10 S4 In3 -65.62(14) . . . . ? S17 In10 S4 In3 64.99(13) . . . . ? S7 In4 S5 In9 178.84(9) . . . . ? S6 In4 S5 In9 -57.56(12) . . . . ? S8 In4 S5 In9 60.77(12) . . . . ? S7 In4 S5 In3 59.00(13) . . . . ? S6 In4 S5 In3 -177.40(10) . . . . ? S8 In4 S5 In3 -59.08(12) . . . . ? S16 In9 S5 In4 59.79(12) . . . . ? S17 In9 S5 In4 177.42(9) . . . . ? S2 In9 S5 In4 -61.99(12) . . . . ? S16 In9 S5 In3 -179.30(9) . . . . ? S17 In9 S5 In3 -61.67(11) . . . . ? S2 In9 S5 In3 58.92(12) . . . . ? S12 In3 S5 In4 -62.72(12) . . . . ? S4 In3 S5 In4 179.19(10) . . . . ? S11 In3 S5 In4 59.09(12) . . . . ? S12 In3 S5 In9 177.95(10) . . . . ? S4 In3 S5 In9 59.85(12) . . . . ? S11 In3 S5 In9 -60.24(11) . . . . ? S7 In4 S6 In8 -178.04(10) . . . . ? S5 In4 S6 In8 58.62(12) . . . . ? S8 In4 S6 In8 -60.94(12) . . . . ? S15 In8 S6 In4 176.15(9) . . . . ? S16 In8 S6 In4 -63.37(12) . . . . ? S1 In8 S6 In4 64.50(13) . . . . ? S6 In4 S7 In7 -177.00(10) . . . . ? S5 In4 S7 In7 -53.43(13) . . . . ? S8 In4 S7 In7 65.90(13) . . . . ? S15 In7 S7 In4 169.84(10) 6_455 . . . ? S12 In7 S7 In4 57.76(14) . . . . ? S13 In7 S7 In4 -67.90(13) . . . . ? S14 In6 S8 In4 178.10(10) . . . . ? S13 In6 S8 In4 58.54(12) . . . . ? S11 In6 S8 In4 -62.35(11) . . . . ? S14 In6 S8 In1 -62.30(12) . . . . ? S13 In6 S8 In1 178.15(9) . . . . ? S11 In6 S8 In1 57.26(12) . . . . ? S7 In4 S8 In6 -60.71(12) . . . . ? S6 In4 S8 In6 179.85(9) . . . . ? S5 In4 S8 In6 59.33(11) . . . . ? S7 In4 S8 In1 -179.72(10) . . . . ? S6 In4 S8 In1 60.83(12) . . . . ? S5 In4 S8 In1 -59.68(12) . . . . ? S1 In1 S8 In6 -178.67(9) . . . . ? S9 In1 S8 In6 61.27(12) . . . . ? S2 In1 S8 In6 -59.73(12) . . . . ? S1 In1 S8 In4 -60.39(13) . . . . ? S9 In1 S8 In4 179.54(10) . . . . ? S2 In1 S8 In4 58.55(12) . . . . ? S1 In1 S9 In5 -179.95(11) . . . . ? S2 In1 S9 In5 62.50(13) . . . . ? S8 In1 S9 In5 -58.70(13) . . . . ? S18 In5 S9 In1 169.24(10) 5_654 . . . ? S10 In5 S9 In1 -67.32(13) . . . . ? S14 In5 S9 In1 63.05(13) . . . . ? S3 In2 S10 In5 179.35(11) . . . . ? S11 In2 S10 In5 58.11(14) . . . . ? S2 In2 S10 In5 -61.02(13) . . . . ? S18 In5 S10 In2 -169.83(10) 5_654 . . . ? S9 In5 S10 In2 67.08(13) . . . . ? S14 In5 S10 In2 -61.34(14) . . . . ? S14 In6 S11 In2 59.50(13) . . . . ? S13 In6 S11 In2 178.63(10) . . . . ? S8 In6 S11 In2 -57.79(12) . . . . ? S14 In6 S11 In3 179.79(10) . . . . ? S13 In6 S11 In3 -61.08(12) . . . . ? S8 In6 S11 In3 62.50(12) . . . . ? S10 In2 S11 In6 -60.32(13) . . . . ? S3 In2 S11 In6 178.01(10) . . . . ? S2 In2 S11 In6 59.01(12) . . . . ? S10 In2 S11 In3 -179.46(10) . . . . ? S3 In2 S11 In3 58.87(13) . . . . ? S2 In2 S11 In3 -60.13(12) . . . . ? S12 In3 S11 In6 59.73(13) . . . . ? S4 In3 S11 In6 179.95(10) . . . . ? S5 In3 S11 In6 -59.44(12) . . . . ? S12 In3 S11 In2 -179.34(10) . . . . ? S4 In3 S11 In2 -59.11(13) . . . . ? S5 In3 S11 In2 61.49(12) . . . . ? S4 In3 S12 In7 179.97(11) . . . . ? S5 In3 S12 In7 60.76(13) . . . . ? S11 In3 S12 In7 -59.28(14) . . . . ? S15 In7 S12 In3 177.45(12) 6_455 . . . ? S7 In7 S12 In3 -62.40(15) . . . . ? S13 In7 S12 In3 62.99(14) . . . . ? S14 In6 S13 In7 -175.74(11) . . . . ? S11 In6 S13 In7 64.58(13) . . . . ? S8 In6 S13 In7 -57.86(13) . . . . ? S15 In7 S13 In6 -174.03(10) 6_455 . . . ? S7 In7 S13 In6 61.88(13) . . . . ? S12 In7 S13 In6 -66.85(13) . . . . ? S13 In6 S14 In5 -174.46(11) . . . . ? S11 In6 S14 In5 -56.10(14) . . . . ? S8 In6 S14 In5 63.83(13) . . . . ? S18 In5 S14 In6 177.31(12) 5_654 . . . ? S10 In5 S14 In6 60.17(14) . . . . ? S9 In5 S14 In6 -67.48(13) . . . . ? S16 In8 S15 In7 -30.3(2) . . . 6 ? S1 In8 S15 In7 -150.09(12) . . . 6 ? S6 In8 S15 In7 90.70(13) . . . 6 ? S17 In9 S16 In8 -179.49(10) . . . . ? S5 In9 S16 In8 -62.99(13) . . . . ? S2 In9 S16 In8 58.92(14) . . . . ? S15 In8 S16 In9 -175.20(11) . . . . ? S1 In8 S16 In9 -62.46(14) . . . . ? S6 In8 S16 In9 65.56(14) . . . . ? S16 In9 S17 In10 -176.41(10) . . . . ? S5 In9 S17 In10 64.87(12) . . . . ? S2 In9 S17 In10 -55.33(12) . . . . ? S18 In10 S17 In9 174.88(11) . . . . ? S4 In10 S17 In9 -69.17(12) . . . . ? S3 In10 S17 In9 59.64(13) . . . . ? S4 In10 S18 In5 50.36(15) . . . 5_644 ? S3 In10 S18 In5 -74.14(14) . . . 5_644 ? S17 In10 S18 In5 165.28(11) . . . 5_644 ? C11 C12 N11 C13 -162(2) . . . . ? C12 N11 C13 C14 178(2) . . . . ? #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 1999-10-18 at 17:30:54 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta3 # Request file : d:\wingx\files\archive.dat # CIF files read : 97086a data_97086a _audit_creation_date 1999-10-18T17:30:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category 'Full Paper' _publ_contact_author_name 'Dr. Christopher L. Cahill' _publ_contact_author_address ; Department of Civil Engineering and Geological Sciences University of Notre Dame Notre Dame, IN 46656 ; _publ_contact_author_email ccahill@nd.edu _publ_requested_journal 'Dalton Transactions' _publ_section_title 'On the formation of framework indium-sulfides' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'In10 S18' _chemical_formula_weight 1725.28 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/amd 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+1/2' 'x, -y, -z' 'y+1/4, x+3/4, -z+1/4' '-y+1/4, -x+1/4, -z+3/4' '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' 'x+1/2, -y+1/2, -z+1/2' 'y+3/4, x+5/4, -z+3/4' '-y+3/4, -x+3/4, -z+5/4' '-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-1/2' '-x, y, z' '-y-1/4, -x-3/4, z-1/4' 'y-1/4, x-1/4, z-3/4' '-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' '-x+1/2, y+1/2, z+1/2' '-y+1/4, -x-1/4, z+1/4' 'y+1/4, x+1/4, z-1/4' _cell_length_a 11.79580 _cell_length_b 11.79580 _cell_length_c 47.0929(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6552.55(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5644 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 24.95 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.749 _exptl_crystal_F_000 3112 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.021 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 14773 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.95 _reflns_number_total 1589 _reflns_number_gt 1061 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'SAINT V5.1 (Bruker-AXS, 1998)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Severe disorder of organic molecules (Diethylamine) in the extra-framework region of this structure prevented adequate modeling. Thus the data have been corrected for the effects of disordered species with the program SQUEEZE (Sluis, P. v.d.; Spek, A. L. Acta Crystallogr., Sect A 1990, 46, 194-201). A potential solvent volume of 3640.3 A^3 per unit cell volume of 6552.5 A^3, or 55.6% was found. The refinement improved by 1% in this step. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^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_extinction_method none _refine_ls_number_reflns 1589 _refine_ls_number_parameters 41 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_gt 0.1204 _refine_ls_wR_factor_all 0.1254 _refine_ls_goodness_of_fit_gt 1.118 _refine_ls_goodness_of_fit_all 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_restrained_S_obs 1.118 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.903 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.189 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group In1 In 0.16689(6) 0.25 0.066077(14) 0.0337(3) Uani 1 d S . In2 In 0.5 0.25 0.06240(2) 0.0303(3) Uani 1 d S . In3 In 0.32785(4) 0.42215(4) 0.125 0.0310(3) Uani 1 d S . S1 S 0.3302(2) 0.25 0.03302(5) 0.0393(7) Uani 1 d S . S2 S 0.5 0.4234(2) 0.09353(5) 0.0330(6) Uani 1 d S . S3 S 0.1578(2) 0.4228(2) 0.09596(4) 0.0437(6) Uani 1 d . . S4 S 0 0.25 0.03407(7) 0.0376(10) Uani 1 d S . 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 0.0246(4) 0.0493(5) 0.0271(4) 0 -0.0044(3) 0 In2 0.0239(6) 0.0421(7) 0.0249(5) 0 0 0 In3 0.0313(3) 0.0313(3) 0.0304(4) -0.0031(2) -0.0031(2) 0.0013(3) S1 0.031(2) 0.059(2) 0.0285(13) 0 -0.0008(12) 0 S2 0.033(2) 0.038(2) 0.0276(13) 0.0003(12) 0 0 S3 0.0365(12) 0.0490(14) 0.0457(13) -0.0081(10) -0.0118(9) 0.0121(9) S4 0.023(2) 0.071(3) 0.019(2) 0 0 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 2.477(3) . ? In1 S4 2.480(2) . ? In1 S3 2.480(2) . ? In1 S3 2.480(2) 29 ? In2 S1 2.434(3) . ? In2 S1 2.434(3) 10_554 ? In2 S2 2.516(3) 10_554 ? In2 S2 2.516(3) . ? In3 S3 2.428(2) 16_554 ? In3 S3 2.428(2) . ? In3 S2 2.5140(14) . ? In3 S2 2.5140(14) 20_656 ? S2 In3 2.5140(14) 27_565 ? S4 In1 2.479(2) 10_454 ? 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 S1 In1 S4 103.62(9) . . ? S1 In1 S3 112.98(6) . . ? S4 In1 S3 108.10(6) . . ? S1 In1 S3 112.98(6) . 29 ? S4 In1 S3 108.10(6) . 29 ? S3 In1 S3 110.62(10) . 29 ? S1 In2 S1 110.73(12) . 10_554 ? S1 In2 S2 109.34(4) . 10_554 ? S1 In2 S2 109.34(4) 10_554 10_554 ? S1 In2 S2 109.34(4) . . ? S1 In2 S2 109.34(4) 10_554 . ? S2 In2 S2 108.73(12) 10_554 . ? S3 In3 S3 108.17(10) 16_554 . ? S3 In3 S2 109.27(8) 16_554 . ? S3 In3 S2 109.59(6) . . ? S3 In3 S2 109.59(6) 16_554 20_656 ? S3 In3 S2 109.28(8) . 20_656 ? S2 In3 S2 110.90(12) . 20_656 ? In2 S1 In1 106.43(10) . . ? In3 S2 In3 107.75(9) 27_565 . ? In3 S2 In2 109.81(7) 27_565 . ? In3 S2 In2 109.81(7) . . ? In3 S3 In1 106.33(8) . . ? In1 S4 In1 105.11(12) 10_454 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 In2 S1 In1 180 10_554 . . . ? S2 In2 S1 In1 59.47(6) 10_554 . . . ? S2 In2 S1 In1 -59.47(6) . . . . ? S4 In1 S1 In2 180 . . . . ? S3 In1 S1 In2 63.26(6) . . . . ? S3 In1 S1 In2 -63.26(6) 29 . . . ? S3 In3 S2 In3 61.77(11) 16_554 . . 27_565 ? S3 In3 S2 In3 -179.87(8) . . . 27_565 ? S2 In3 S2 In3 -59.15(7) 20_656 . . 27_565 ? S3 In3 S2 In2 -178.67(7) 16_554 . . . ? S3 In3 S2 In2 -60.31(10) . . . . ? S2 In3 S2 In2 60.42(7) 20_656 . . . ? S1 In2 S2 In3 178.46(7) . . . 27_565 ? S1 In2 S2 In3 -60.16(11) 10_554 . . 27_565 ? S2 In2 S2 In3 59.15(7) 10_554 . . 27_565 ? S1 In2 S2 In3 60.16(11) . . . . ? S1 In2 S2 In3 -178.46(7) 10_554 . . . ? S2 In2 S2 In3 -59.15(7) 10_554 . . . ? S3 In3 S3 In1 178.53(10) 16_554 . . . ? S2 In3 S3 In1 59.48(10) . . . . ? S2 In3 S3 In1 -62.22(10) 20_656 . . . ? S1 In1 S3 In3 -63.20(10) . . . . ? S4 In1 S3 In3 -177.25(7) . . . . ? S3 In1 S3 In3 64.57(12) 29 . . . ? S1 In1 S4 In1 180 . . . 10_454 ? S3 In1 S4 In1 -59.89(6) . . . 10_454 ? S3 In1 S4 In1 59.88(6) 29 . . 10_454 ? #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 1999-10-18 at 09:28:25 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta3 # Request file : d:\wingx\files\archive.dat # CIF files read : orgsqz data_orgsqz _audit_creation_date 1999-10-18T09:28:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FA _publ_contact_author_name 'Dr. Christopher L. Cahill' _publ_contact_author_address ; Department of Civil Engineering and Geological Sciences University of Notre Dame Notre Dame, IN 46656 ; _publ_contact_author_email ccahill@nd.edu _publ_requested_journal 'Dalton Transactions' _publ_section_title 'On the formation of framework indium-sulfides' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C24 H64 In4 N4 S10' _chemical_formula_weight 1188.8 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.322(2) _cell_length_b 30.803(6) _cell_length_c 15.861(3) _cell_angle_alpha 90 _cell_angle_beta 105.75(3) _cell_angle_gamma 90 _cell_volume 4853.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2079 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 28.81 _cell_measurement_wavelength 0.643 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.617 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.643 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator 'Si (111)' _diffrn_detector 'Bruker 1K CCD' _diffrn_measurement_device 'Huber 4-Circle' _diffrn_measurement_method 'Phi rotation' _diffrn_reflns_number 19630 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.2 _diffrn_reflns_theta_max 28.81 _diffrn_reflns_theta_full 28.81 _diffrn_measured_fraction_theta_full 0.75 _diffrn_measured_fraction_theta_max 0.75 _reflns_number_total 6437 _reflns_number_gt 2999 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'SAINT V5.1 (Bruker-AXS, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Wingx (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 chemical formula reported contains two unique dipropylamine (DPA) molecules(and symmetry equivalents). Severe disorder allowed modelling of only one of these molecules. Treatment of the data based on a model containing one cation position was done with SQUEEZE (Sluis, P. v.d.; Spek, A. L. Acta Crystallogr., Sect A 1990, 46, 194-201) The refinement continued using the treated data. Thus the refinement reported herein is based on reflections from which the contribution from the disordered DPA molecule has been removed. The chemical formula however, contains the second, assumed, DPA cation. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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_number_reflns 6437 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1329 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2703 _refine_ls_wR_factor_gt 0.2581 _refine_ls_goodness_of_fit_ref 1.367 _refine_ls_restrained_S_all 1.367 _refine_ls_shift/su_max 0.123 _refine_ls_shift/su_mean 0.011 _refine_diff_density_max 1.373 _refine_diff_density_min -2.472 _refine_diff_density_rms 0.427 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.82528(7) 0.06915(3) 0.67548(6) 0.0463(3) Uani 1 1 d . . . In2 In 0.93328(8) 0.15711(3) 0.85162(6) 0.0532(3) Uani 1 1 d . . . S3 S 0.7385(3) 0.11016(12) 0.7831(2) 0.0580(9) Uani 1 1 d . . . S4 S 1 0.01777(15) 0.75 0.0516(11) Uani 1 2 d S . . S5 S 0.8763(3) 0.11419(12) 0.5610(2) 0.0582(9) Uani 1 1 d . . . S6 S 1 0.20647(19) 0.75 0.0743(15) Uani 1 2 d S . . S7 S 0.6256(3) 0.02690(14) 0.5885(3) 0.0703(11) Uani 1 1 d . . . S8 S 0.8514(5) 0.20407(15) 0.9552(4) 0.0928(15) Uani 1 1 d . . . N1 N 0.7391(12) 0.0317(4) 0.9310(8) 0.068(3) Uiso 1 1 d . . . H1 H 0.6614 0.0435 0.9102 0.082 Uiso 1 1 calc R . . C2 C 1.2197(14) -0.0081(5) 0.6044(10) 0.066(4) Uiso 1 1 d . . . H2A H 1.145 -0.0019 0.6287 0.079 Uiso 1 1 calc R . . H2B H 1.1897 -0.0291 0.5577 0.079 Uiso 1 1 calc R . . C3 C 0.8432(16) -0.0499(5) 0.5057(10) 0.077(4) Uiso 1 1 d . . . H3A H 0.8728 -0.0275 0.5498 0.093 Uiso 1 1 calc R . . H3B H 0.9203 -0.0587 0.4859 0.093 Uiso 1 1 calc R . . C4 C 0.7939(17) 0.0878(5) 1.0457(11) 0.083(5) Uiso 1 1 d . . . H4A H 0.755 0.1087 1.0002 0.1 Uiso 1 1 calc R . . H4B H 0.7231 0.0782 1.0711 0.1 Uiso 1 1 calc R . . C5 C 0.3246(17) -0.0250(6) 0.6682(11) 0.092(5) Uiso 1 1 d . . . H5A H 0.3538 -0.0039 0.7149 0.11 Uiso 1 1 calc R . . H5B H 0.3996 -0.0306 0.6438 0.11 Uiso 1 1 calc R . . C6 C 1.285(2) -0.0680(6) 0.7070(14) 0.116(7) Uiso 1 1 d . . . H6A H 1.3431 -0.091 0.6988 0.173 Uiso 1 1 calc R . . H6B H 1.1933 -0.0751 0.6776 0.173 Uiso 1 1 calc R . . H6C H 1.2941 -0.0642 0.7684 0.173 Uiso 1 1 calc R . . C7 C 0.901(2) 0.1095(7) 1.1147(13) 0.118(7) Uiso 1 1 d . . . H7A H 0.8628 0.1337 1.1379 0.177 Uiso 1 1 calc R . . H7B H 0.9703 0.1196 1.0899 0.177 Uiso 1 1 calc R . . H7C H 0.938 0.0892 1.1609 0.177 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 0.0331(4) 0.0575(5) 0.0481(6) -0.0106(4) 0.0107(3) -0.0034(3) In2 0.0431(4) 0.0576(6) 0.0591(7) -0.0130(5) 0.0142(4) -0.0030(4) S3 0.0384(14) 0.073(2) 0.064(2) -0.0243(18) 0.0158(14) -0.0036(14) S4 0.042(2) 0.050(2) 0.064(3) 0 0.0156(19) 0 S5 0.0443(15) 0.071(2) 0.057(2) -0.0002(18) 0.0098(14) 0.0014(15) S6 0.078(3) 0.064(3) 0.086(4) 0 0.031(3) 0 S7 0.0474(17) 0.093(3) 0.069(3) -0.032(2) 0.0134(16) -0.0225(17) S8 0.099(3) 0.079(3) 0.112(4) -0.045(3) 0.049(3) -0.007(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S4 2.449(3) . ? In1 S5 2.453(4) . ? In1 S3 2.479(3) . ? In1 S7 2.510(3) . ? In2 S6 2.447(4) . ? In2 S5 2.460(4) 2_756 ? In2 S3 2.476(3) . ? In2 S8 2.503(4) . ? S4 In1 2.449(3) 2_756 ? S5 In2 2.460(4) 2_756 ? S6 In2 2.447(4) 2_756 ? N1 C2 1.459(17) 2_756 ? N1 C3 1.477(19) 6_556 ? C2 C5 1.37(2) 1_655 ? C2 N1 1.459(17) 2_756 ? C3 N1 1.477(19) 6 ? C3 C4 1.48(2) 6 ? C4 C7 1.48(2) . ? C4 C3 1.48(2) 6_556 ? C5 C2 1.37(2) 1_455 ? C5 C6 1.56(2) 1_455 ? C6 C5 1.56(2) 1_655 ? 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 S4 In1 S5 116.40(9) . . ? S4 In1 S3 110.70(10) . . ? S5 In1 S3 114.33(14) . . ? S4 In1 S7 108.50(14) . . ? S5 In1 S7 101.29(13) . . ? S3 In1 S7 104.26(12) . . ? S6 In2 S5 112.36(10) . 2_756 ? S6 In2 S3 114.47(11) . . ? S5 In2 S3 111.28(13) 2_756 . ? S6 In2 S8 106.21(17) . . ? S5 In2 S8 107.54(16) 2_756 . ? S3 In2 S8 104.29(14) . . ? In2 S3 In1 101.39(11) . . ? In1 S4 In1 99.48(17) 2_756 . ? In1 S5 In2 100.72(13) . 2_756 ? In2 S6 In2 103.2(2) 2_756 . ? C2 N1 C3 113.7(12) 2_756 6_556 ? C5 C2 N1 110.4(13) 1_655 2_756 ? N1 C3 C4 112.5(13) 6 6 ? C7 C4 C3 113.4(15) . 6_556 ? C2 C5 C6 112.0(16) 1_455 1_455 ? #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 1999-10-18 at 14:43:33 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta3 # Request file : d:\wingx\files\archive.dat # CIF files read : cb4_135s data_cb4_135s _audit_creation_date 1999-10-18T14:43:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_contact_author_name 'Dr. Christopher L. Cahill' _publ_contact_author_address ; Department of Civil Engineering and Geological Sciences University of Notre Dame Notre Dame, IN 46656 ; _publ_contact_author_email ccahill@nd.edu _publ_requested_journal 'Dalton Transactions' _publ_requested_category 'Full Article' _publ_section_title 'On the formation of framework indium-sulfides' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C52 H56 In9 N8 S17' _chemical_formula_weight 2371.5 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 11.505(1) _cell_length_b 28.708(1) _cell_length_c 26.240(1) _cell_angle_alpha 90 _cell_angle_beta 101.95(1) _cell_angle_gamma 90 _cell_volume 8481(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6460 _cell_measurement_theta_min 0.96 _cell_measurement_theta_max 22.4 _cell_measurement_wavelength 0.643 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.006 _exptl_crystal_density_diffrn 1.855 _exptl_crystal_F_000 4536 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.853 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.643 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator 'Si(111)' _diffrn_detector 'Bruker 1K CCD' _diffrn_measurement_device 'Huber 4-Circle' _diffrn_measurement_method 'Phi rotation' _diffrn_reflns_number 33002 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 22.24 _diffrn_reflns_theta_full 22.24 _diffrn_measured_fraction_theta_full 0.64 _diffrn_measured_fraction_theta_max 0.64 _reflns_number_total 9274 _reflns_number_gt 6537 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'SAINT V5.1 (Bruker, 1998)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'SAINT V5.1 (Bruker-AXS, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Wingx (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _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_number_reflns 9274 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.2163 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 0.83 _refine_ls_restrained_S_all 0.83 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.292 _refine_diff_density_min -2.392 _refine_diff_density_rms 0.471 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.16822(9) 0.63571(4) 0.44726(4) 0.0318(4) Uani 1 1 d . . . In2 In 0.38138(9) 0.71520(4) 0.55883(4) 0.0307(4) Uani 1 1 d . . . In3 In -0.16938(9) 0.64263(4) 0.43400(4) 0.0322(4) Uani 1 1 d . . . In4 In 0.51547(9) 0.63905(4) 0.46190(4) 0.0332(4) Uani 1 1 d . . . In5 In 0.03197(9) 0.73947(4) 0.51915(4) 0.0316(4) Uani 1 1 d . . . In6 In -0.02571(9) 0.74824(4) 0.37418(4) 0.0335(4) Uani 1 1 d . . . In7 In 0.15170(9) 0.71293(4) 0.77552(4) 0.0357(4) Uani 1 1 d . . . In8 In 0.21000(10) 0.74648(4) 0.66217(4) 0.0346(4) Uani 1 1 d . . . In9 In 0.33759(9) 0.75023(4) 0.41144(4) 0.0310(4) Uani 1 1 d . . . S10 S 0.1614(3) 0.69842(14) 0.38051(15) 0.0325(10) Uani 1 1 d . . . S11 S -0.0046(3) 0.58680(15) 0.43760(17) 0.0393(11) Uani 1 1 d . . . S12 S 0.5351(3) 0.65733(15) 0.55538(16) 0.0378(11) Uani 1 1 d . . . S13 S -0.1934(3) 0.69481(16) 0.35725(16) 0.0417(11) Uani 1 1 d . . . S14 S -0.1494(3) 0.69349(14) 0.51115(16) 0.0338(10) Uani 1 1 d . . . S15 S 0.3368(3) 0.58825(15) 0.43596(17) 0.0379(11) Uani 1 1 d . . . S16 S 0.0530(4) 0.78431(15) 0.59940(16) 0.0428(12) Uani 1 1 d . . . S17 S 0.0140(4) 0.79769(15) 0.45026(16) 0.0378(11) Uani 1 1 d . . . S18 S -0.0485(4) 0.7895(2) 0.29123(19) 0.0609(15) Uani 1 1 d . . . S19 S -0.3324(3) 0.58921(15) 0.43917(19) 0.0446(12) Uani 1 1 d . . . S20 S 0.1848(3) 0.67436(14) 0.53544(15) 0.0320(10) Uani 1 1 d . . . S21 S 0.3663(3) 0.78248(14) 0.49973(15) 0.0350(11) Uani 1 1 d . . . S22 S 0.5207(3) 0.70946(14) 0.40850(16) 0.0358(11) Uani 1 1 d . . . S23 S 0.2085(4) 0.79022(16) 0.74439(16) 0.0426(12) Uani 1 1 d . . . S24 S 0.4140(3) 0.74857(15) 0.64703(16) 0.0395(12) Uani 1 1 d . . . S25 S 0.3130(4) 0.68656(15) 0.84676(16) 0.0386(11) Uani 1 1 d . . . S26 S 0.1729(4) 0.66832(15) 0.69643(16) 0.0391(11) Uani 1 1 d . . . N1 N -0.0269(12) 0.8412(5) 0.7675(6) 0.054(4) Uani 1 1 d . . . N2 N 0.2252(14) 0.8798(5) 0.4466(7) 0.070(5) Uani 1 1 d . . . N3 N 0.4495(16) 0.8381(6) 0.7965(7) 0.066(5) Uani 1 1 d . . . N4 N -0.3365(12) 0.7702(5) 0.5209(5) 0.044(4) Uani 1 1 d . . . N5 N 0.1732(14) 0.8786(5) 0.5464(6) 0.063(5) Uani 1 1 d . . . N6 N 0.3607(19) 0.5599(7) 0.5534(7) 0.094(6) Uani 1 1 d . . . N7 N 0.4911(11) 0.6925(5) 0.7610(5) 0.041(4) Uani 1 1 d . . . N8 N -0.0733(13) 0.6398(6) 0.6170(6) 0.056(4) Uani 1 1 d . . . C1 C 0.1812(16) 1.0670(7) 0.8333(8) 0.056(5) Uani 1 1 d . . . C2 C -0.2902(16) 0.8106(7) 0.4963(7) 0.056(5) Uani 1 1 d . . . H2 H -0.2457 0.8078 0.4706 0.067 Uiso 1 1 calc R . . C3 C -0.3001(14) 0.7720(7) 0.5771(7) 0.050(5) Uani 1 1 d . . . H3 H -0.2591 0.748 0.5969 0.06 Uiso 1 1 calc R . . C4 C -0.3224(16) 0.8559(6) 0.5169(7) 0.053(5) Uani 1 1 d . . . H4 H -0.3603 0.88 0.4961 0.064 Uiso 1 1 calc R . . C5 C 0.206(2) 1.0228(8) 0.5855(7) 0.084(7) Uani 1 1 d . . . H5A H 0.1304 1.0381 0.5732 0.101 Uiso 1 1 calc R . . H5B H 0.2509 1.0263 0.5582 0.101 Uiso 1 1 calc R . . C6 C -0.0025(18) 0.8944(6) 0.6970(7) 0.059(6) Uani 1 1 d . . . H6 H 0.0372 0.8938 0.6695 0.07 Uiso 1 1 calc R . . C7 C -0.0717(17) 0.8537(7) 0.7119(7) 0.066(6) Uani 1 1 d . . . H7 H -0.1335 0.8386 0.6895 0.079 Uiso 1 1 calc R . . C8 C -0.0052(16) 0.9379(7) 0.7330(7) 0.058(5) Uani 1 1 d . . . C9 C 0.0400(15) 0.9232(6) 0.7895(6) 0.051(5) Uani 1 1 d . . . H9 H 0.1012 0.9374 0.8132 0.061 Uiso 1 1 calc R . . C13 C 0.6499(15) 0.6787(6) 0.8389(7) 0.048(5) Uani 1 1 d . . . H13 H 0.6652 0.6894 0.8731 0.057 Uiso 1 1 calc R . . C14 C -0.3322(16) 0.8720(6) 0.3256(7) 0.048(5) Uani 1 1 d . . . C15 C -0.1566(15) 0.8854(6) 0.1916(7) 0.052(5) Uani 1 1 d . . . H15 H -0.1447 0.8794 0.2272 0.063 Uiso 1 1 calc R . . C16 C 0.5081(17) 0.6435(8) 0.7466(8) 0.073(7) Uani 1 1 d . . . H16 H 0.4933 0.6334 0.7122 0.088 Uiso 1 1 calc R . . C18 C -0.3343(16) 0.8158(7) 0.6004(8) 0.061(6) Uani 1 1 d . . . H18 H -0.3795 0.8171 0.6258 0.073 Uiso 1 1 calc R . . C19 C -0.2856(18) 0.8583(6) 0.5770(7) 0.055(5) Uani 1 1 d . . . C20 C 0.0694(16) 1.0224(6) 0.7501(7) 0.056(5) Uani 1 1 d . . . H20A H 0.0591 1.0492 0.7271 0.067 Uiso 1 1 calc R . . H20B H 0.0025 1.0216 0.7673 0.067 Uiso 1 1 calc R . . C21 C 0.3933(17) 0.9152(9) 0.7634(12) 0.101(9) Uani 1 1 d . . . H21 H 0.3255 0.9337 0.7558 0.122 Uiso 1 1 calc R . . C22 C 0.0673(16) 0.9777(7) 0.7167(7) 0.060(6) Uani 1 1 d . . . H22A H 0.0347 0.9854 0.6805 0.072 Uiso 1 1 calc R . . H22B H 0.1482 0.9671 0.719 0.072 Uiso 1 1 calc R . . C23 C -0.094(2) 0.5562(7) 0.6345(7) 0.067(6) Uani 1 1 d . . . H23 H -0.0456 0.5299 0.638 0.081 Uiso 1 1 calc R . . C24 C -0.335(2) 0.9013(8) 0.5995(9) 0.086(7) Uani 1 1 d . . . H24A H -0.3208 0.8979 0.6371 0.103 Uiso 1 1 calc R . . H24B H -0.4208 0.9017 0.5868 0.103 Uiso 1 1 calc R . . C25 C 0.3456(16) 0.8939(7) 0.4507(8) 0.069(6) Uani 1 1 d . . . H25 H 0.4087 0.8731 0.4583 0.082 Uiso 1 1 calc R . . C26 C 0.457(2) 0.5347(7) 0.5820(7) 0.072(6) Uani 1 1 d . . . H26 H 0.5165 0.5205 0.5685 0.086 Uiso 1 1 calc R . . C27 C 0.446(2) 0.5347(8) 0.6390(8) 0.089(8) Uani 1 1 d . . . H27 H 0.5079 0.5445 0.6656 0.107 Uiso 1 1 calc R . . C28 C 0.6059(17) 0.7103(7) 0.7930(8) 0.072(6) Uani 1 1 d . . . H28 H 0.6445 0.7371 0.7857 0.086 Uiso 1 1 calc R . . C29 C 0.5504(16) 0.6118(6) 0.7914(8) 0.064(6) Uani 1 1 d . . . H29 H 0.5102 0.5851 0.7978 0.077 Uiso 1 1 calc R . . C31 C 0.5975(18) 0.9429(7) 0.7575(8) 0.072(6) Uani 1 1 d . . . H31A H 0.6166 0.9334 0.7938 0.086 Uiso 1 1 calc R . . H31B H 0.663 0.9334 0.7418 0.086 Uiso 1 1 calc R . . C34 C 0.1381(15) 0.9015(6) 0.4010(7) 0.060(6) Uani 1 1 d . . . H34 H 0.0753 0.8849 0.3811 0.072 Uiso 1 1 calc R . . C35 C 0.484(2) 0.9167(7) 0.7299(7) 0.065(6) Uani 1 1 d . . . C36 C 0.1604(17) 0.9500(7) 0.3910(8) 0.071(6) Uani 1 1 d . . . H36 H 0.1003 0.9722 0.384 0.085 Uiso 1 1 calc R . . C37 C 0.292(2) 0.9617(7) 0.3929(9) 0.078(7) Uani 1 1 d . . . C38 C 0.1850(16) 1.0290(7) 0.7922(7) 0.059(5) Uani 1 1 d . . . H38A H 0.2044 0.9997 0.8101 0.07 Uiso 1 1 calc R . . H38B H 0.2491 1.0364 0.7746 0.07 Uiso 1 1 calc R . . C39 C -0.0320(16) 0.8812(7) 0.8008(7) 0.061(6) Uani 1 1 d . . . H39 H -0.0755 0.8812 0.827 0.073 Uiso 1 1 calc R . . C40 C 0.364(2) 0.9464(7) 0.4416(10) 0.084(7) Uani 1 1 d . . . C41 C 0.330(2) 0.5177(8) 0.6493(8) 0.076(6) Uani 1 1 d . . . C42 C 0.0865(17) 0.9552(8) 0.5462(8) 0.074(7) Uani 1 1 d . . . H42 H 0.0443 0.9745 0.5204 0.089 Uiso 1 1 calc R . . C43 C 0.235(2) 0.5386(7) 0.5563(8) 0.077(7) Uani 1 1 d . . . H43 H 0.1781 0.5273 0.5284 0.092 Uiso 1 1 calc R . . C44 C 0.2910(18) 0.9427(8) 0.5895(8) 0.074(6) Uani 1 1 d . . . H44 H 0.3659 0.9548 0.5894 0.089 Uiso 1 1 calc R . . C45 C 0.0646(17) 0.9029(7) 0.5482(8) 0.065(6) Uani 1 1 d . . . H45 H -0.0072 0.889 0.5503 0.078 Uiso 1 1 calc R . . C46 C 0.181(2) 0.9724(7) 0.5892(7) 0.067(6) Uani 1 1 d . . . C47 C 0.4151(19) 0.8827(11) 0.8099(9) 0.088(8) Uani 1 1 d . . . H47 H 0.4069 0.8912 0.8432 0.105 Uiso 1 1 calc R . . C48 C 0.2637(17) 0.8910(7) 0.5900(7) 0.071(7) Uani 1 1 d . . . H48 H 0.3011 0.8703 0.6154 0.086 Uiso 1 1 calc R . . C49 C 0.312(2) 0.5234(8) 0.7073(8) 0.090(8) Uani 1 1 d . . . H49A H 0.3155 0.5561 0.7168 0.108 Uiso 1 1 calc R . . H49B H 0.2348 0.5114 0.71 0.108 Uiso 1 1 calc R . . C50 C 0.588(2) 0.9960(6) 0.7551(7) 0.073(7) Uani 1 1 d . . . H50A H 0.512 1.0048 0.7628 0.088 Uiso 1 1 calc R . . H50B H 0.5873 1.0058 0.7197 0.088 Uiso 1 1 calc R . . C51 C 0.284(2) 1.0509(7) 0.4133(9) 0.080(7) Uani 1 1 d . . . H51A H 0.3163 1.0433 0.4496 0.096 Uiso 1 1 calc R . . H51B H 0.1988 1.0533 0.4087 0.096 Uiso 1 1 calc R . . C52 C 0.315(2) 1.0114(7) 0.3786(8) 0.080(7) Uani 1 1 d . . . H52A H 0.2702 1.0168 0.3434 0.096 Uiso 1 1 calc R . . H52B H 0.3982 1.0139 0.3778 0.096 Uiso 1 1 calc R . . C53 C 0.272(2) 1.0502(8) 0.6322(8) 0.082(7) Uani 1 1 d . . . H53A H 0.2275 1.0474 0.6598 0.098 Uiso 1 1 calc R . . H53B H 0.3484 1.0357 0.6446 0.098 Uiso 1 1 calc R . . C54 C -0.1545(16) 0.6510(7) 0.6494(7) 0.057(5) Uani 1 1 d . . . H54 H -0.2012 0.6777 0.6452 0.068 Uiso 1 1 calc R . . C55 C -0.2912(18) 0.8997(7) 0.3761(7) 0.064(6) Uani 1 1 d . . . C56 C -0.0953(19) 0.5939(9) 0.5954(9) 0.080(7) Uani 1 1 d . . . H56 H -0.1095 0.5882 0.5598 0.097 Uiso 1 1 calc R . . C57 C 0.223(2) 0.5404(9) 0.6152(9) 0.101(9) Uani 1 1 d . . . H57 H 0.1603 0.5536 0.6272 0.121 Uiso 1 1 calc R . . C58 C 0.507(2) 0.8653(7) 0.7192(10) 0.083(7) Uani 1 1 d . . . H58 H 0.5024 0.8537 0.6857 0.099 Uiso 1 1 calc R . . C59 C 0.538(2) 0.8367(7) 0.7653(10) 0.081(7) Uani 1 1 d . . . H59 H 0.6068 0.8191 0.7738 0.098 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 0.0185(6) 0.0456(8) 0.0304(7) 0.0023(5) 0.0031(5) 0.0005(5) In2 0.0232(6) 0.0453(8) 0.0225(7) 0.0008(5) 0.0022(5) -0.0004(5) In3 0.0182(6) 0.0476(8) 0.0297(7) -0.0021(6) 0.0024(5) -0.0025(5) In4 0.0202(6) 0.0439(8) 0.0351(8) 0.0004(6) 0.0053(5) 0.0024(5) In5 0.0259(6) 0.0435(8) 0.0237(7) -0.0006(5) 0.0012(5) -0.0012(5) In6 0.0250(6) 0.0513(8) 0.0237(7) 0.0048(5) 0.0037(5) 0.0030(5) In7 0.0287(6) 0.0560(9) 0.0225(7) -0.0041(6) 0.0055(5) -0.0030(5) In8 0.0289(6) 0.0543(9) 0.0192(7) -0.0014(5) 0.0018(5) -0.0017(5) In9 0.0246(6) 0.0424(8) 0.0244(7) 0.0007(5) 0.0013(5) 0.0008(5) S10 0.023(2) 0.044(3) 0.029(2) 0.004(2) 0.0021(18) -0.0033(18) S11 0.022(2) 0.043(3) 0.053(3) 0.000(2) 0.008(2) -0.0008(18) S12 0.027(2) 0.052(3) 0.033(3) 0.000(2) 0.0013(19) 0.007(2) S13 0.029(2) 0.059(3) 0.032(3) 0.006(2) -0.0039(19) -0.003(2) S14 0.025(2) 0.046(3) 0.030(2) -0.008(2) 0.0045(18) -0.0035(18) S15 0.022(2) 0.046(3) 0.048(3) -0.005(2) 0.012(2) 0.0008(18) S16 0.045(3) 0.054(3) 0.026(3) -0.007(2) -0.001(2) 0.007(2) S17 0.041(2) 0.043(3) 0.027(2) 0.000(2) 0.003(2) -0.005(2) S18 0.034(2) 0.109(4) 0.041(3) 0.034(3) 0.012(2) 0.018(3) S19 0.024(2) 0.040(3) 0.073(3) -0.014(2) 0.016(2) -0.0041(18) S20 0.024(2) 0.046(3) 0.025(2) 0.0000(19) 0.0016(18) -0.0019(18) S21 0.031(2) 0.046(3) 0.025(2) 0.0029(19) -0.0013(19) 0.0051(19) S22 0.023(2) 0.047(3) 0.037(3) 0.004(2) 0.0077(19) 0.0020(18) S23 0.047(3) 0.055(3) 0.025(3) -0.004(2) 0.007(2) -0.003(2) S24 0.026(2) 0.066(3) 0.025(2) -0.006(2) 0.0007(19) -0.0066(19) S25 0.041(2) 0.049(3) 0.024(2) -0.003(2) 0.0000(19) -0.001(2) S26 0.039(2) 0.052(3) 0.026(2) -0.003(2) 0.007(2) -0.001(2) N1 0.048(9) 0.073(11) 0.035(9) 0.000(9) -0.002(7) 0.002(8) N2 0.054(10) 0.060(11) 0.097(14) 0.004(10) 0.019(10) 0.008(8) N3 0.072(12) 0.073(13) 0.043(11) 0.012(9) -0.011(9) -0.017(10) N4 0.044(8) 0.053(10) 0.038(10) 0.014(8) 0.014(7) -0.009(7) N5 0.067(11) 0.064(11) 0.056(11) 0.005(8) 0.008(9) -0.004(9) N6 0.122(17) 0.100(16) 0.071(14) 0.024(12) 0.042(13) 0.007(14) N7 0.035(8) 0.036(9) 0.049(9) -0.004(7) 0.002(7) 0.011(6) N8 0.044(9) 0.086(14) 0.038(10) 0.010(9) 0.004(8) -0.012(9) C1 0.056(12) 0.061(15) 0.053(14) -0.003(11) 0.012(11) 0.011(10) C2 0.055(12) 0.077(16) 0.042(12) -0.007(11) 0.026(10) 0.001(11) C3 0.035(10) 0.058(14) 0.060(14) 0.009(11) 0.015(10) 0.011(9) C4 0.067(13) 0.049(13) 0.048(13) 0.013(10) 0.020(10) 0.016(10) C5 0.13(2) 0.081(18) 0.034(13) -0.018(11) 0.007(13) -0.022(15) C6 0.098(16) 0.063(14) 0.020(11) -0.012(9) 0.024(10) -0.009(12) C7 0.063(13) 0.075(15) 0.047(13) 0.007(11) -0.019(10) -0.017(11) C8 0.055(12) 0.063(14) 0.054(13) 0.002(11) 0.008(10) -0.005(11) C9 0.045(10) 0.078(14) 0.024(10) 0.023(9) -0.009(8) -0.012(10) C13 0.057(12) 0.049(13) 0.033(11) 0.006(9) 0.000(9) 0.002(9) C14 0.055(11) 0.039(12) 0.050(12) 0.000(9) 0.011(10) -0.009(9) C15 0.064(12) 0.046(13) 0.046(13) -0.009(10) 0.009(10) 0.003(10) C16 0.071(14) 0.098(19) 0.039(13) 0.007(12) -0.013(11) 0.007(12) C18 0.054(12) 0.076(17) 0.062(14) -0.012(12) 0.033(11) -0.022(11) C19 0.086(14) 0.022(12) 0.057(14) -0.022(10) 0.016(11) 0.006(10) C20 0.068(13) 0.056(13) 0.042(12) 0.002(10) 0.010(10) 0.016(10) C21 0.036(12) 0.10(2) 0.16(3) -0.020(19) 0.000(16) 0.036(12) C22 0.057(12) 0.069(15) 0.050(13) -0.011(11) 0.005(10) 0.018(11) C23 0.121(19) 0.066(15) 0.024(12) 0.024(11) 0.038(13) 0.024(13) C24 0.084(16) 0.10(2) 0.075(17) -0.002(14) 0.009(13) -0.016(14) C25 0.039(11) 0.055(15) 0.098(17) -0.011(11) -0.020(11) 0.008(9) C26 0.105(18) 0.076(16) 0.032(13) 0.012(11) 0.011(12) 0.007(13) C27 0.10(2) 0.099(19) 0.052(16) 0.024(13) -0.009(13) -0.021(15) C28 0.056(13) 0.068(15) 0.086(17) 0.015(12) -0.001(12) -0.016(11) C29 0.057(12) 0.047(13) 0.080(16) -0.010(11) -0.008(11) -0.010(10) C31 0.084(16) 0.080(18) 0.059(15) -0.006(12) 0.034(13) 0.024(13) C34 0.052(12) 0.043(13) 0.068(14) 0.010(10) -0.028(10) -0.014(9) C35 0.088(17) 0.056(15) 0.043(12) -0.005(10) -0.005(12) 0.002(12) C36 0.060(13) 0.061(16) 0.086(17) 0.015(12) 0.004(12) 0.027(11) C37 0.100(18) 0.041(15) 0.084(17) 0.035(12) -0.001(14) -0.014(12) C38 0.058(12) 0.072(14) 0.043(12) 0.009(11) 0.004(10) 0.014(10) C39 0.048(11) 0.099(17) 0.039(12) 0.017(12) 0.017(10) 0.010(11) C40 0.082(16) 0.054(16) 0.11(2) 0.026(13) 0.008(15) -0.013(12) C41 0.077(15) 0.094(17) 0.062(16) 0.020(13) 0.023(13) -0.008(13) C42 0.056(13) 0.091(19) 0.068(15) -0.007(12) -0.004(11) 0.010(12) C43 0.094(17) 0.075(16) 0.052(15) 0.015(11) -0.007(12) 0.002(13) C44 0.053(13) 0.104(19) 0.058(14) 0.001(12) -0.004(11) -0.002(13) C45 0.057(13) 0.045(14) 0.092(17) 0.000(11) 0.013(12) -0.010(10) C46 0.109(18) 0.045(14) 0.046(13) -0.015(10) 0.015(12) -0.011(12) C47 0.062(15) 0.16(3) 0.039(14) -0.008(17) 0.009(12) -0.020(16) C48 0.065(14) 0.073(16) 0.055(14) 0.017(11) -0.034(11) -0.018(11) C49 0.17(3) 0.071(16) 0.036(14) 0.004(11) 0.033(15) 0.009(16) C50 0.14(2) 0.049(15) 0.037(13) 0.008(10) 0.033(13) 0.003(13) C51 0.095(17) 0.065(17) 0.085(18) 0.037(14) 0.027(14) 0.012(13) C52 0.105(18) 0.070(17) 0.059(15) -0.021(13) 0.008(13) 0.018(14) C53 0.098(18) 0.095(19) 0.044(14) -0.020(12) -0.005(12) -0.023(14) C54 0.045(11) 0.064(14) 0.051(13) 0.011(11) -0.011(10) 0.005(10) C55 0.089(15) 0.049(14) 0.048(13) -0.016(10) -0.001(11) -0.024(11) C56 0.084(16) 0.11(2) 0.054(15) 0.003(15) 0.026(13) 0.011(14) C57 0.083(17) 0.15(2) 0.077(19) 0.032(16) 0.027(14) 0.066(17) C58 0.12(2) 0.066(17) 0.074(18) -0.020(14) 0.041(15) 0.008(14) C59 0.076(16) 0.063(16) 0.11(2) 0.027(15) 0.028(16) 0.014(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S11 2.405(4) . ? In1 S15 2.440(4) . ? In1 S10 2.502(4) . ? In1 S20 2.536(4) . ? In2 S12 2.444(4) . ? In2 S24 2.459(4) . ? In2 S21 2.461(4) . ? In2 S20 2.509(4) . ? In3 S19 2.450(4) . ? In3 S14 2.467(4) . ? In3 S11 2.471(4) . ? In3 S13 2.478(4) . ? In4 S19 2.431(4) 1_655 ? In4 S22 2.469(4) . ? In4 S12 2.470(4) . ? In4 S15 2.497(4) . ? In5 S16 2.436(4) . ? In5 S17 2.439(4) . ? In5 S14 2.442(4) . ? In5 S20 2.542(4) . ? In6 S17 2.414(4) . ? In6 S13 2.434(4) . ? In6 S18 2.443(5) . ? In6 S10 2.563(4) . ? In7 S18 2.426(5) 4_576 ? In7 S25 2.461(4) . ? In7 S26 2.493(4) . ? In7 S23 2.500(5) . ? In7 In8 3.3237(17) . ? In8 S16 2.432(4) . ? In8 S24 2.462(4) . ? In8 S26 2.489(4) . ? In8 S23 2.499(4) . ? In9 S22 2.427(4) . ? In9 S21 2.451(4) . ? In9 S25 2.461(4) 4_575 ? In9 S10 2.510(4) . ? S18 In7 2.426(5) 4_575 ? S19 In4 2.431(4) 1_455 ? S25 In9 2.461(4) 4_576 ? N1 C39 1.45(2) . ? N1 C7 1.48(2) . ? N2 C25 1.43(2) . ? N2 C34 1.52(2) . ? N3 C47 1.41(3) . ? N3 C59 1.43(3) . ? N4 C3 1.45(2) . ? N4 C2 1.48(2) . ? N5 C48 1.42(2) . ? N5 C45 1.44(2) . ? N6 C26 1.40(3) . ? N6 C43 1.59(3) . ? N7 C16 1.48(2) . ? N7 C28 1.50(2) . ? N8 C54 1.42(2) . ? N8 C56 1.44(3) . ? C1 C23 1.47(3) 2_556 ? C1 C15 1.52(3) 3_576 ? C1 C38 1.54(3) . ? C2 C4 1.49(2) . ? C3 C18 1.49(3) . ? C4 C19 1.55(3) . ? C5 C46 1.49(3) . ? C5 C53 1.52(3) . ? C6 C7 1.51(3) . ? C6 C8 1.57(3) . ? C8 C9 1.53(2) . ? C8 C22 1.53(3) . ? C9 C39 1.53(3) . ? C13 C28 1.51(3) . ? C13 C14 1.52(2) 4_676 ? C14 C13 1.52(2) 4_475 ? C14 C29 1.53(2) 4_475 ? C14 C55 1.53(2) . ? C15 C1 1.52(3) 3_576 ? C15 C54 1.53(3) 4_575 ? C16 C29 1.49(3) . ? C18 C19 1.52(3) . ? C19 C24 1.53(3) . ? C20 C38 1.55(2) . ? C20 C22 1.55(2) . ? C21 C35 1.50(3) . ? C21 C47 1.52(3) . ? C23 C1 1.47(3) 2_546 ? C23 C56 1.49(3) . ? C24 C51 1.56(3) 3_576 ? C25 C40 1.55(3) . ? C26 C27 1.52(3) . ? C27 C41 1.50(3) . ? C29 C14 1.53(2) 4_676 ? C31 C50 1.53(3) . ? C31 C35 1.55(3) . ? C34 C36 1.45(3) . ? C35 C58 1.54(3) . ? C36 C37 1.54(3) . ? C37 C40 1.44(3) . ? C37 C52 1.51(3) . ? C41 C57 1.51(3) . ? C41 C49 1.59(3) . ? C42 C46 1.48(3) . ? C42 C45 1.53(3) . ? C43 C57 1.58(3) . ? C44 C48 1.52(3) . ? C44 C46 1.52(3) . ? C49 C50 1.56(3) 2_646 ? C50 C49 1.56(3) 2_656 ? C51 C52 1.54(3) . ? C51 C24 1.56(3) 3_576 ? C53 C55 1.48(3) 3_576 ? C54 C15 1.53(3) 4_576 ? C55 C53 1.48(3) 3_576 ? C58 C59 1.44(3) . ? 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 S11 In1 S15 108.78(15) . . ? S11 In1 S10 116.30(14) . . ? S15 In1 S10 103.11(14) . . ? S11 In1 S20 104.75(14) . . ? S15 In1 S20 116.46(14) . . ? S10 In1 S20 107.92(14) . . ? S12 In2 S24 109.34(14) . . ? S12 In2 S21 117.88(15) . . ? S24 In2 S21 105.23(14) . . ? S12 In2 S20 107.20(14) . . ? S24 In2 S20 111.38(14) . . ? S21 In2 S20 105.80(13) . . ? S19 In3 S14 105.49(15) . . ? S19 In3 S11 100.47(14) . . ? S14 In3 S11 114.47(14) . . ? S19 In3 S13 117.87(15) . . ? S14 In3 S13 106.42(15) . . ? S11 In3 S13 112.22(15) . . ? S19 In4 S22 103.86(15) 1_655 . ? S19 In4 S12 116.57(15) 1_655 . ? S22 In4 S12 112.37(15) . . ? S19 In4 S15 100.56(14) 1_655 . ? S22 In4 S15 116.17(14) . . ? S12 In4 S15 107.08(15) . . ? S16 In5 S17 104.74(15) . . ? S16 In5 S14 106.80(15) . . ? S17 In5 S14 111.67(14) . . ? S16 In5 S20 107.71(14) . . ? S17 In5 S20 125.28(14) . . ? S14 In5 S20 99.51(13) . . ? S17 In6 S13 121.88(15) . . ? S17 In6 S18 114.59(18) . . ? S13 In6 S18 102.17(16) . . ? S17 In6 S10 105.30(14) . . ? S13 In6 S10 106.45(14) . . ? S18 In6 S10 105.15(15) . . ? S18 In7 S25 117.04(17) 4_576 . ? S18 In7 S26 112.83(15) 4_576 . ? S25 In7 S26 106.46(14) . . ? S18 In7 S23 113.83(18) 4_576 . ? S25 In7 S23 108.31(14) . . ? S26 In7 S23 96.18(15) . . ? S18 In7 In8 122.49(13) 4_576 . ? S25 In7 In8 120.43(11) . . ? S26 In7 In8 48.10(10) . . ? S23 In7 In8 48.31(10) . . ? S16 In8 S24 118.60(16) . . ? S16 In8 S26 119.23(15) . . ? S24 In8 S26 108.77(15) . . ? S16 In8 S23 102.74(15) . . ? S24 In8 S23 107.81(15) . . ? S26 In8 S23 96.31(15) . . ? S16 In8 In7 118.31(12) . . ? S24 In8 In7 121.93(11) . . ? S26 In8 In7 48.20(10) . . ? S23 In8 In7 48.34(11) . . ? S22 In9 S21 105.45(14) . . ? S22 In9 S25 108.06(15) . 4_575 ? S21 In9 S25 110.19(14) . 4_575 ? S22 In9 S10 110.60(14) . . ? S21 In9 S10 118.00(14) . . ? S25 In9 S10 104.27(14) 4_575 . ? In1 S10 In9 107.24(14) . . ? In1 S10 In6 110.52(15) . . ? In9 S10 In6 107.51(16) . . ? In1 S11 In3 103.65(16) . . ? In2 S12 In4 105.35(15) . . ? In6 S13 In3 106.51(15) . . ? In5 S14 In3 108.81(16) . . ? In1 S15 In4 105.71(16) . . ? In8 S16 In5 105.87(17) . . ? In6 S17 In5 100.38(16) . . ? In7 S18 In6 102.00(16) 4_575 . ? In4 S19 In3 104.11(16) 1_455 . ? In2 S20 In1 108.64(15) . . ? In2 S20 In5 104.70(15) . . ? In1 S20 In5 104.59(13) . . ? In9 S21 In2 105.99(16) . . ? In9 S22 In4 104.67(15) . . ? In8 S23 In7 83.35(14) . . ? In2 S24 In8 100.32(14) . . ? In9 S25 In7 104.81(16) 4_576 . ? In8 S26 In7 83.70(14) . . ? C39 N1 C7 110.6(15) . . ? C25 N2 C34 114.3(16) . . ? C47 N3 C59 116.0(17) . . ? C3 N4 C2 111.3(14) . . ? C48 N5 C45 110.2(16) . . ? C26 N6 C43 113.7(17) . . ? C16 N7 C28 108.6(13) . . ? C54 N8 C56 111.0(15) . . ? C23 C1 C15 110.5(16) 2_556 3_576 ? C23 C1 C38 112.0(16) 2_556 . ? C15 C1 C38 111.5(16) 3_576 . ? N4 C2 C4 112.8(15) . . ? N4 C3 C18 113.7(15) . . ? C2 C4 C19 111.9(15) . . ? C46 C5 C53 121.5(19) . . ? C7 C6 C8 112.5(16) . . ? N1 C7 C6 110.3(15) . . ? C9 C8 C22 112.6(15) . . ? C9 C8 C6 108.5(15) . . ? C22 C8 C6 110.3(15) . . ? C8 C9 C39 108.6(15) . . ? C28 C13 C14 115.7(16) . 4_676 ? C13 C14 C29 106.3(14) 4_475 4_475 ? C13 C14 C55 109.4(15) 4_475 . ? C29 C14 C55 114.9(16) 4_475 . ? C1 C15 C54 109.6(16) 3_576 4_575 ? N7 C16 C29 114.9(16) . . ? C3 C18 C19 111.2(15) . . ? C18 C19 C24 107.0(17) . . ? C18 C19 C4 109.2(14) . . ? C24 C19 C4 112.5(16) . . ? C38 C20 C22 114.4(15) . . ? C35 C21 C47 118.0(17) . . ? C8 C22 C20 114.0(15) . . ? C1 C23 C56 109.2(17) 2_546 . ? C19 C24 C51 116.1(18) . 3_576 ? N2 C25 C40 115.3(16) . . ? N6 C26 C27 108(2) . . ? C41 C27 C26 115.7(19) . . ? N7 C28 C13 110.6(15) . . ? C16 C29 C14 112.3(16) . 4_676 ? C50 C31 C35 114.8(18) . . ? C36 C34 N2 115.0(15) . . ? C21 C35 C58 104.4(18) . . ? C21 C35 C31 111.3(17) . . ? C58 C35 C31 113.1(18) . . ? C34 C36 C37 114.4(16) . . ? C40 C37 C52 114.1(19) . . ? C40 C37 C36 110.2(18) . . ? C52 C37 C36 114.8(18) . . ? C1 C38 C20 116.0(15) . . ? N1 C39 C9 114.6(16) . . ? C37 C40 C25 111.2(18) . . ? C27 C41 C57 113.5(18) . . ? C27 C41 C49 116(2) . . ? C57 C41 C49 105.6(19) . . ? C46 C42 C45 113.8(18) . . ? C57 C43 N6 107.2(18) . . ? C48 C44 C46 111.9(18) . . ? N5 C45 C42 109.0(16) . . ? C42 C46 C5 113.4(18) . . ? C42 C46 C44 107.1(16) . . ? C5 C46 C44 112(2) . . ? N3 C47 C21 111.7(19) . . ? N5 C48 C44 110.9(16) . . ? C50 C49 C41 108.9(18) 2_646 . ? C31 C50 C49 116.0(19) . 2_656 ? C52 C51 C24 112.4(18) . 3_576 ? C37 C52 C51 118.5(19) . . ? C55 C53 C5 116.8(18) 3_576 . ? N8 C54 C15 112.9(15) . 4_576 ? C53 C55 C14 114.0(16) 3_576 . ? N8 C56 C23 115.0(18) . . ? C41 C57 C43 110.0(18) . . ? C59 C58 C35 114.5(19) . . ? N3 C59 C58 112.8(19) . . ? #===END