# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Gerald Linti' _publ_contact_author_email GERALD.LINTI@ACI.UNI-HEIDELBERG.DE _publ_section_title ; Synthesis and Structure of Tri- and Octaindium Compounds ; loop_ _publ_author_name 'Gerald Linti' 'Martina Buhler' 'Kirill Yu Monakhov' 'Thomas Zessin' # Attachment 'comp_5_728993.cif' data_m40t1_CCDC_728993 _database_code_depnum_ccdc_archive 'CCDC 728993' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H53 In O Si3' _chemical_formula_weight 965.09 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' Si Si 0.0817 0.0704 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.939(2) _cell_length_b 11.342(2) _cell_length_c 22.153(4) _cell_angle_alpha 81.25(3) _cell_angle_beta 85.93(3) _cell_angle_gamma 85.45(3) _cell_volume 2456.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 23.3 _exptl_crystal_description disphenoidal _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.88188 _exptl_absorpt_correction_T_max 0.9244 _exptl_absorpt_process_details ? _exptl_special_details ; crystal very weakly diffracting; mean int/sigma 2.4 in XPRE(SHELXTL); due to this a bad Rint results. Due to intensity measurment with IPDS I, a two circle goniometer the completeness of data is usually between 0.92 and 0.99 ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'image plate, 2 circle goniometer' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15607 _diffrn_reflns_av_R_equivalents 0.2198 _diffrn_reflns_av_sigmaI/netI 0.3710 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.00 _reflns_number_total 7182 _reflns_number_gt 2761 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement STOE _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXTL 5.01' _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. ISOR restraint was applied for C56: C55 to C58 are carbon atoms of a coordinated thf molecule; which tend to have higher U values. Splitting of C56 and C57 was not applied, because the data/parameter value is already low. The 20 highest residual electron density peaks are located in the molecule, thus solvent accessible voids in the structure are empty ; _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^)+(0.0462P)^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 7182 _refine_ls_number_parameters 568 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1853 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.1941 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _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 0.61595(11) 0.71048(10) 0.73670(4) 0.0323(3) Uani 1 1 d . . . Si1 Si 0.5478(4) 0.6132(4) 0.84962(16) 0.0349(10) Uani 1 1 d . . . Si2 Si 0.6997(4) 0.5711(4) 0.65453(16) 0.0352(10) Uani 1 1 d . . . Si3 Si 0.4808(4) 0.9143(4) 0.69793(16) 0.0339(10) Uani 1 1 d . . . O1 O 0.8077(10) 0.7919(9) 0.7614(4) 0.048(3) Uani 1 1 d . . . C1 C 0.3658(15) 0.5979(13) 0.8694(6) 0.039(4) Uani 1 1 d . . . C2 C 0.2960(16) 0.6385(15) 0.9203(7) 0.058(5) Uani 1 1 d . . . H2 H 0.3424 0.6852 0.9431 0.069 Uiso 1 1 calc R . . C3 C 0.1640(18) 0.6151(16) 0.9396(6) 0.060(5) Uani 1 1 d . . . H3 H 0.1219 0.6485 0.9735 0.071 Uiso 1 1 calc R . . C4 C 0.0955(16) 0.5463(16) 0.9110(8) 0.060(5) Uani 1 1 d . . . H4 H 0.0066 0.5268 0.9255 0.072 Uiso 1 1 calc R . . C5 C 0.1565(16) 0.5039(16) 0.8597(8) 0.059(5) Uani 1 1 d . . . H5 H 0.1098 0.4550 0.8382 0.071 Uiso 1 1 calc R . . C6 C 0.2832(18) 0.5328(16) 0.8407(7) 0.065(5) Uani 1 1 d . . . H6 H 0.3197 0.5060 0.8039 0.077 Uiso 1 1 calc R . . C7 C 0.6279(16) 0.4587(13) 0.8744(6) 0.044(4) Uani 1 1 d . . . C8 C 0.5675(15) 0.3743(12) 0.9191(5) 0.037(4) Uani 1 1 d . . . H8 H 0.4814 0.3958 0.9373 0.045 Uiso 1 1 calc R . . C9 C 0.6256(16) 0.2641(14) 0.9374(6) 0.044(4) Uani 1 1 d . . . H9 H 0.5777 0.2099 0.9665 0.053 Uiso 1 1 calc R . . C10 C 0.7486(18) 0.2295(15) 0.9156(7) 0.059(5) Uani 1 1 d . . . H10 H 0.7915 0.1552 0.9325 0.071 Uiso 1 1 calc R . . C11 C 0.8145(18) 0.3027(13) 0.8679(7) 0.065(5) Uani 1 1 d . . . H11 H 0.8982 0.2768 0.8490 0.078 Uiso 1 1 calc R . . C12 C 0.7520(16) 0.4147(14) 0.8494(7) 0.055(5) Uani 1 1 d . . . H12 H 0.7965 0.4654 0.8173 0.066 Uiso 1 1 calc R . . C13 C 0.6085(15) 0.7118(14) 0.9035(6) 0.044(4) Uani 1 1 d . . . C14 C 0.5681(17) 0.8291(15) 0.8987(7) 0.054(5) Uani 1 1 d . . . H14 H 0.5045 0.8616 0.8695 0.065 Uiso 1 1 calc R . . C15 C 0.6160(17) 0.9032(15) 0.9349(7) 0.058(5) Uani 1 1 d . . . H15 H 0.5868 0.9858 0.9293 0.070 Uiso 1 1 calc R . . C16 C 0.7044(19) 0.8603(17) 0.9782(6) 0.067(6) Uani 1 1 d . . . H16 H 0.7357 0.9115 1.0036 0.080 Uiso 1 1 calc R . . C17 C 0.7464(16) 0.7444(16) 0.9846(7) 0.054(5) Uani 1 1 d . . . H17 H 0.8092 0.7132 1.0144 0.065 Uiso 1 1 calc R . . C18 C 0.6993(14) 0.6687(14) 0.9479(6) 0.042(4) Uani 1 1 d . . . H18 H 0.7298 0.5865 0.9534 0.050 Uiso 1 1 calc R . . C19 C 0.7816(13) 0.6474(12) 0.5805(6) 0.032(3) Uani 1 1 d . . . C20 C 0.7185(15) 0.7404(13) 0.5454(6) 0.042(4) Uani 1 1 d . . . H20 H 0.6307 0.7691 0.5587 0.050 Uiso 1 1 calc R . . C21 C 0.7778(19) 0.7969(16) 0.4894(7) 0.071(6) Uani 1 1 d . . . H21 H 0.7300 0.8613 0.4655 0.085 Uiso 1 1 calc R . . C22 C 0.9063(18) 0.7567(14) 0.4701(6) 0.051(4) Uani 1 1 d . . . H22 H 0.9492 0.7969 0.4339 0.061 Uiso 1 1 calc R . . C23 C 0.9707(18) 0.6620(14) 0.5018(6) 0.056(5) Uani 1 1 d . . . H23 H 1.0567 0.6319 0.4870 0.068 Uiso 1 1 calc R . . C24 C 0.9091(15) 0.6067(13) 0.5578(6) 0.044(4) Uani 1 1 d . . . H24 H 0.9560 0.5401 0.5806 0.053 Uiso 1 1 calc R . . C25 C 0.8156(13) 0.4384(14) 0.6808(5) 0.033(4) Uani 1 1 d . . . C26 C 0.8011(15) 0.3247(13) 0.6694(6) 0.036(4) Uani 1 1 d . . . H26 H 0.7245 0.3119 0.6485 0.044 Uiso 1 1 calc R . . C27 C 0.8881(19) 0.2300(19) 0.6857(8) 0.066(5) Uani 1 1 d . . . H27 H 0.8696 0.1534 0.6773 0.079 Uiso 1 1 calc R . . C28 C 1.0030(19) 0.2421(17) 0.7143(8) 0.062(5) Uani 1 1 d . . . H28 H 1.0659 0.1758 0.7246 0.075 Uiso 1 1 calc R . . C29 C 1.0241(16) 0.353(2) 0.7275(7) 0.064(5) Uani 1 1 d . . . H29 H 1.1001 0.3654 0.7490 0.076 Uiso 1 1 calc R . . C30 C 0.9292(16) 0.4495(14) 0.7083(7) 0.046(4) Uani 1 1 d . . . H30 H 0.9473 0.5271 0.7153 0.055 Uiso 1 1 calc R . . C31 C 0.5384(14) 0.5067(13) 0.6377(6) 0.043(4) Uani 1 1 d . . . C32 C 0.4779(15) 0.5322(14) 0.5826(7) 0.047(4) Uani 1 1 d . . . H32 H 0.5210 0.5815 0.5495 0.056 Uiso 1 1 calc R . . C33 C 0.3595(16) 0.4887(15) 0.5749(7) 0.056(5) Uani 1 1 d . . . H33 H 0.3176 0.5138 0.5374 0.067 Uiso 1 1 calc R . . C34 C 0.2968(15) 0.4100(15) 0.6187(7) 0.053(5) Uani 1 1 d . . . H34 H 0.2163 0.3754 0.6118 0.063 Uiso 1 1 calc R . . C35 C 0.3578(15) 0.3842(14) 0.6730(7) 0.046(4) Uani 1 1 d . . . H35 H 0.3167 0.3323 0.7056 0.055 Uiso 1 1 calc R . . C36 C 0.4726(16) 0.4297(14) 0.6814(7) 0.056(5) Uani 1 1 d . . . H36 H 0.5112 0.4076 0.7198 0.067 Uiso 1 1 calc R . . C37 C 0.3187(14) 0.8773(13) 0.6692(6) 0.035(4) Uani 1 1 d . . . C38 C 0.2936(15) 0.7630(15) 0.6634(7) 0.048(4) Uani 1 1 d . . . H38 H 0.3613 0.7007 0.6738 0.058 Uiso 1 1 calc R . . C39 C 0.1717(16) 0.7339(13) 0.6426(7) 0.049(4) Uani 1 1 d . . . H39 H 0.1558 0.6532 0.6403 0.058 Uiso 1 1 calc R . . C40 C 0.0757(15) 0.8256(15) 0.6257(7) 0.048(4) Uani 1 1 d . . . H40 H -0.0072 0.8083 0.6112 0.058 Uiso 1 1 calc R . . C41 C 0.0998(16) 0.9409(15) 0.6297(6) 0.046(4) Uani 1 1 d . . . H41 H 0.0349 1.0046 0.6175 0.055 Uiso 1 1 calc R . . C42 C 0.2158(15) 0.9624(14) 0.6509(6) 0.045(4) Uani 1 1 d . . . H42 H 0.2296 1.0433 0.6538 0.054 Uiso 1 1 calc R . . C43 C 0.5758(13) 1.0153(12) 0.6331(6) 0.031(3) Uani 1 1 d . . . C44 C 0.5166(15) 1.1257(13) 0.6111(7) 0.047(4) Uani 1 1 d . . . H44 H 0.4335 1.1533 0.6297 0.057 Uiso 1 1 calc R . . C45 C 0.5777(17) 1.1971(14) 0.5618(7) 0.050(4) Uani 1 1 d . . . H45 H 0.5350 1.2723 0.5459 0.060 Uiso 1 1 calc R . . C46 C 0.6975(17) 1.1593(15) 0.5367(7) 0.058(5) Uani 1 1 d . . . H46 H 0.7365 1.2074 0.5020 0.069 Uiso 1 1 calc R . . C47 C 0.7657(16) 1.0530(15) 0.5596(6) 0.052(4) Uani 1 1 d . . . H47 H 0.8531 1.0299 0.5433 0.063 Uiso 1 1 calc R . . C48 C 0.7000(16) 0.9803(15) 0.6082(6) 0.052(4) Uani 1 1 d . . . H48 H 0.7427 0.9052 0.6242 0.062 Uiso 1 1 calc R . . C49 C 0.4274(13) 1.0154(13) 0.7579(6) 0.034(4) Uani 1 1 d . . . C50 C 0.3104(15) 0.9960(15) 0.7970(7) 0.055(5) Uani 1 1 d . . . H50 H 0.2594 0.9297 0.7945 0.066 Uiso 1 1 calc R . . C51 C 0.2689(19) 1.072(2) 0.8389(8) 0.079(6) Uani 1 1 d . . . H51 H 0.1851 1.0629 0.8620 0.095 Uiso 1 1 calc R . . C52 C 0.345(2) 1.1568(18) 0.8467(7) 0.066(6) Uani 1 1 d . . . H52 H 0.3198 1.2044 0.8780 0.079 Uiso 1 1 calc R . . C53 C 0.459(2) 1.1777(17) 0.8118(8) 0.074(6) Uani 1 1 d . . . H53 H 0.5132 1.2390 0.8184 0.089 Uiso 1 1 calc R . . C54 C 0.4952(16) 1.1098(13) 0.7661(6) 0.048(4) Uani 1 1 d . . . H54 H 0.5714 1.1300 0.7393 0.058 Uiso 1 1 calc R . . C55 C 0.9158(15) 0.7305(14) 0.7926(7) 0.052(5) Uani 1 1 d . . . H55A H 0.9791 0.6914 0.7640 0.062 Uiso 1 1 calc R . . H55B H 0.8823 0.6682 0.8252 0.062 Uiso 1 1 calc R . . C56 C 0.985(2) 0.819(2) 0.8195(10) 0.106(7) Uani 1 1 d U . . H56A H 0.9784 0.8002 0.8647 0.127 Uiso 1 1 calc R . . H56B H 1.0817 0.8169 0.8053 0.127 Uiso 1 1 calc R . . C57 C 0.925(2) 0.9274(17) 0.8018(10) 0.096(7) Uani 1 1 d . . . H57A H 0.9899 0.9769 0.7751 0.116 Uiso 1 1 calc R . . H57B H 0.8992 0.9670 0.8381 0.116 Uiso 1 1 calc R . . C58 C 0.8053(16) 0.9188(15) 0.7687(7) 0.057(5) Uani 1 1 d . . . H58A H 0.8095 0.9702 0.7284 0.069 Uiso 1 1 calc R . . H58B H 0.7222 0.9432 0.7924 0.069 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 0.0361(7) 0.0377(6) 0.0210(5) 0.0031(4) -0.0013(4) -0.0038(5) Si1 0.035(3) 0.045(3) 0.0227(19) 0.0018(18) 0.0020(17) -0.006(2) Si2 0.038(3) 0.037(2) 0.030(2) -0.0039(18) -0.0023(18) -0.003(2) Si3 0.032(3) 0.040(2) 0.028(2) -0.0002(18) -0.0025(18) 0.001(2) O1 0.053(8) 0.046(7) 0.040(6) 0.003(5) -0.011(5) 0.009(6) C1 0.052(11) 0.044(9) 0.021(7) 0.006(7) -0.015(7) -0.009(8) C2 0.059(12) 0.079(13) 0.040(9) -0.019(9) 0.002(9) -0.013(10) C3 0.068(13) 0.084(14) 0.021(8) 0.001(8) 0.014(8) 0.004(11) C4 0.042(12) 0.075(13) 0.061(11) -0.001(10) 0.007(9) -0.021(10) C5 0.037(11) 0.079(14) 0.066(12) -0.016(10) -0.006(9) -0.016(10) C6 0.065(14) 0.080(14) 0.046(10) -0.006(9) 0.010(9) -0.005(11) C7 0.045(11) 0.051(10) 0.039(9) -0.012(8) -0.008(8) -0.006(8) C8 0.059(11) 0.040(9) 0.009(6) 0.011(6) 0.006(6) -0.016(8) C9 0.041(11) 0.057(11) 0.027(8) 0.021(7) -0.009(7) -0.002(9) C10 0.068(14) 0.049(11) 0.053(10) 0.014(8) -0.008(10) 0.002(10) C11 0.079(14) 0.037(10) 0.067(11) 0.006(9) 0.030(10) 0.016(9) C12 0.054(12) 0.040(10) 0.062(11) 0.012(8) 0.011(9) 0.001(9) C13 0.039(11) 0.044(11) 0.040(9) 0.015(7) 0.017(7) -0.007(8) C14 0.065(13) 0.045(11) 0.051(10) 0.016(8) -0.008(9) -0.022(9) C15 0.076(14) 0.056(11) 0.044(10) 0.003(9) 0.001(9) -0.030(10) C16 0.109(17) 0.079(15) 0.016(8) -0.003(8) 0.007(9) -0.047(13) C17 0.060(13) 0.059(12) 0.039(9) 0.010(9) -0.002(8) -0.010(10) C18 0.041(11) 0.050(10) 0.028(8) 0.015(7) -0.007(7) 0.000(8) C19 0.024(9) 0.038(9) 0.032(7) 0.000(7) -0.006(7) -0.002(7) C20 0.048(11) 0.044(10) 0.030(8) -0.002(7) 0.001(7) 0.001(8) C21 0.070(14) 0.082(14) 0.047(10) 0.033(9) 0.002(10) -0.012(11) C22 0.072(14) 0.053(11) 0.030(8) -0.003(8) -0.002(9) -0.021(10) C23 0.093(14) 0.040(10) 0.037(9) -0.012(8) 0.028(9) -0.023(10) C24 0.054(11) 0.045(10) 0.031(8) -0.003(7) 0.005(7) -0.001(8) C25 0.015(9) 0.070(12) 0.014(6) -0.003(7) -0.002(6) -0.016(8) C26 0.033(10) 0.043(10) 0.034(8) -0.009(7) -0.003(7) 0.001(8) C27 0.043(13) 0.090(16) 0.062(11) -0.007(10) 0.006(10) -0.005(12) C28 0.062(15) 0.063(14) 0.050(10) 0.012(10) 0.010(10) 0.016(11) C29 0.032(11) 0.125(18) 0.033(9) -0.017(11) 0.001(7) 0.004(12) C30 0.045(12) 0.036(10) 0.060(10) -0.024(8) 0.006(9) 0.002(9) C31 0.043(10) 0.049(10) 0.024(7) 0.030(7) 0.004(7) 0.003(8) C32 0.033(11) 0.055(11) 0.053(10) -0.008(8) -0.002(8) -0.002(9) C33 0.045(12) 0.069(12) 0.054(10) -0.006(9) -0.010(9) -0.006(10) C34 0.036(10) 0.074(12) 0.059(10) -0.036(9) 0.005(8) -0.024(9) C35 0.027(10) 0.061(11) 0.051(10) -0.002(8) -0.013(8) -0.012(8) C36 0.057(13) 0.062(11) 0.048(10) -0.006(9) 0.003(9) -0.018(10) C37 0.032(10) 0.032(9) 0.037(8) 0.004(7) 0.000(7) 0.006(8) C38 0.026(10) 0.067(13) 0.056(10) -0.021(9) -0.009(8) 0.000(9) C39 0.046(12) 0.023(9) 0.080(12) -0.018(8) -0.012(9) 0.007(8) C40 0.034(11) 0.056(12) 0.059(10) -0.021(9) 0.010(8) -0.015(9) C41 0.033(11) 0.055(12) 0.047(9) 0.007(8) -0.011(8) -0.003(9) C42 0.026(10) 0.045(10) 0.061(10) 0.010(8) -0.008(8) -0.018(9) C43 0.013(8) 0.033(9) 0.043(8) 0.001(7) -0.006(7) 0.012(7) C44 0.032(10) 0.049(11) 0.056(10) 0.007(8) -0.005(8) 0.001(8) C45 0.060(13) 0.043(10) 0.045(10) 0.005(8) -0.007(9) -0.001(9) C46 0.048(13) 0.053(12) 0.062(11) 0.014(9) -0.002(10) 0.003(9) C47 0.040(11) 0.068(12) 0.046(9) 0.001(9) -0.001(8) -0.010(9) C48 0.056(12) 0.062(11) 0.034(9) 0.008(8) -0.006(8) -0.010(9) C49 0.021(9) 0.040(9) 0.043(9) -0.005(7) -0.027(7) 0.005(7) C50 0.045(11) 0.063(12) 0.057(10) -0.012(9) 0.013(9) -0.016(9) C51 0.060(14) 0.13(2) 0.052(12) -0.038(13) 0.007(10) 0.006(14) C52 0.084(17) 0.094(16) 0.018(8) -0.028(9) -0.013(10) 0.043(13) C53 0.092(16) 0.076(14) 0.058(12) -0.034(11) -0.021(12) 0.029(12) C54 0.075(13) 0.042(10) 0.024(8) 0.006(7) -0.002(8) 0.001(9) C55 0.039(12) 0.056(11) 0.061(10) 0.010(9) -0.016(8) -0.028(9) C56 0.107(8) 0.105(8) 0.107(8) -0.015(3) -0.011(3) -0.009(3) C57 0.090(18) 0.067(15) 0.15(2) -0.046(14) -0.047(15) 0.003(13) C58 0.042(12) 0.073(13) 0.058(11) -0.008(9) -0.013(9) 0.001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 O1 2.317(10) . ? In1 Si3 2.636(4) . ? In1 Si2 2.638(4) . ? In1 Si1 2.640(4) . ? Si1 C1 1.846(15) . ? Si1 C7 1.885(16) . ? Si1 C13 1.912(16) . ? Si2 C25 1.866(15) . ? Si2 C31 1.895(15) . ? Si2 C19 1.895(13) . ? Si3 C37 1.873(15) . ? Si3 C49 1.906(14) . ? Si3 C43 1.936(13) . ? O1 C55 1.398(16) . ? O1 C58 1.471(18) . ? C1 C6 1.39(2) . ? C1 C2 1.401(19) . ? C2 C3 1.38(2) . ? C3 C4 1.33(2) . ? C4 C5 1.38(2) . ? C5 C6 1.35(2) . ? C7 C12 1.40(2) . ? C7 C8 1.406(17) . ? C8 C9 1.351(19) . ? C9 C10 1.33(2) . ? C10 C11 1.40(2) . ? C11 C12 1.39(2) . ? C13 C14 1.35(2) . ? C13 C18 1.389(18) . ? C14 C15 1.38(2) . ? C15 C16 1.36(2) . ? C16 C17 1.34(2) . ? C17 C18 1.39(2) . ? C19 C20 1.352(17) . ? C19 C24 1.400(18) . ? C20 C21 1.418(19) . ? C21 C22 1.38(2) . ? C22 C23 1.33(2) . ? C23 C24 1.424(18) . ? C25 C30 1.343(18) . ? C25 C26 1.372(19) . ? C26 C27 1.35(2) . ? C27 C28 1.37(2) . ? C28 C29 1.37(2) . ? C29 C30 1.42(2) . ? C31 C36 1.368(18) . ? C31 C32 1.380(19) . ? C32 C33 1.344(19) . ? C33 C34 1.366(19) . ? C34 C35 1.368(19) . ? C35 C36 1.325(19) . ? C37 C38 1.366(19) . ? C37 C42 1.387(19) . ? C38 C39 1.407(19) . ? C39 C40 1.381(19) . ? C40 C41 1.37(2) . ? C41 C42 1.329(18) . ? C43 C48 1.370(19) . ? C43 C44 1.374(18) . ? C44 C45 1.391(18) . ? C45 C46 1.34(2) . ? C46 C47 1.38(2) . ? C47 C48 1.408(18) . ? C49 C54 1.351(19) . ? C49 C50 1.410(18) . ? C50 C51 1.38(2) . ? C51 C52 1.31(2) . ? C52 C53 1.34(2) . ? C53 C54 1.37(2) . ? C55 C56 1.48(2) . ? C56 C57 1.34(2) . ? C57 C58 1.46(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 O1 In1 Si3 97.0(3) . . ? O1 In1 Si2 105.7(3) . . ? Si3 In1 Si2 117.38(12) . . ? O1 In1 Si1 95.5(2) . . ? Si3 In1 Si1 115.26(13) . . ? Si2 In1 Si1 119.42(13) . . ? C1 Si1 C7 103.8(7) . . ? C1 Si1 C13 106.8(6) . . ? C7 Si1 C13 105.6(7) . . ? C1 Si1 In1 116.8(4) . . ? C7 Si1 In1 115.6(5) . . ? C13 Si1 In1 107.4(4) . . ? C25 Si2 C31 105.0(6) . . ? C25 Si2 C19 106.2(6) . . ? C31 Si2 C19 109.3(5) . . ? C25 Si2 In1 116.5(4) . . ? C31 Si2 In1 103.0(5) . . ? C19 Si2 In1 116.1(4) . . ? C37 Si3 C49 105.0(6) . . ? C37 Si3 C43 108.7(6) . . ? C49 Si3 C43 104.7(6) . . ? C37 Si3 In1 107.5(5) . . ? C49 Si3 In1 116.3(4) . . ? C43 Si3 In1 114.2(4) . . ? C55 O1 C58 108.4(11) . . ? C55 O1 In1 126.6(8) . . ? C58 O1 In1 120.9(8) . . ? C6 C1 C2 110.5(14) . . ? C6 C1 Si1 125.1(12) . . ? C2 C1 Si1 124.0(11) . . ? C3 C2 C1 124.4(15) . . ? C4 C3 C2 120.7(15) . . ? C3 C4 C5 118.5(15) . . ? C6 C5 C4 119.1(16) . . ? C5 C6 C1 126.6(16) . . ? C12 C7 C8 112.8(14) . . ? C12 C7 Si1 123.9(11) . . ? C8 C7 Si1 123.3(12) . . ? C9 C8 C7 123.3(14) . . ? C10 C9 C8 121.6(14) . . ? C9 C10 C11 120.0(15) . . ? C12 C11 C10 116.9(15) . . ? C11 C12 C7 124.9(14) . . ? C14 C13 C18 116.4(15) . . ? C14 C13 Si1 121.1(13) . . ? C18 C13 Si1 122.5(12) . . ? C13 C14 C15 122.1(17) . . ? C16 C15 C14 121.1(17) . . ? C17 C16 C15 118.6(16) . . ? C16 C17 C18 120.8(16) . . ? C13 C18 C17 121.0(15) . . ? C20 C19 C24 116.2(12) . . ? C20 C19 Si2 122.2(11) . . ? C24 C19 Si2 121.5(10) . . ? C19 C20 C21 122.7(15) . . ? C22 C21 C20 118.9(15) . . ? C23 C22 C21 120.7(15) . . ? C22 C23 C24 119.3(16) . . ? C19 C24 C23 122.0(14) . . ? C30 C25 C26 113.9(14) . . ? C30 C25 Si2 121.6(12) . . ? C26 C25 Si2 124.3(11) . . ? C27 C26 C25 124.4(15) . . ? C26 C27 C28 121.1(19) . . ? C27 C28 C29 117.8(17) . . ? C28 C29 C30 118.1(16) . . ? C25 C30 C29 124.5(15) . . ? C36 C31 C32 114.8(14) . . ? C36 C31 Si2 120.7(11) . . ? C32 C31 Si2 124.5(10) . . ? C33 C32 C31 121.4(14) . . ? C32 C33 C34 122.7(15) . . ? C33 C34 C35 115.5(14) . . ? C36 C35 C34 121.8(15) . . ? C35 C36 C31 123.6(15) . . ? C38 C37 C42 114.3(13) . . ? C38 C37 Si3 122.1(11) . . ? C42 C37 Si3 123.6(11) . . ? C37 C38 C39 122.7(15) . . ? C40 C39 C38 118.3(15) . . ? C41 C40 C39 120.1(15) . . ? C42 C41 C40 118.7(15) . . ? C41 C42 C37 125.9(15) . . ? C48 C43 C44 118.9(13) . . ? C48 C43 Si3 122.1(10) . . ? C44 C43 Si3 119.0(10) . . ? C43 C44 C45 120.5(14) . . ? C46 C45 C44 119.6(15) . . ? C45 C46 C47 122.3(15) . . ? C46 C47 C48 117.1(15) . . ? C43 C48 C47 121.5(15) . . ? C54 C49 C50 115.2(14) . . ? C54 C49 Si3 123.8(11) . . ? C50 C49 Si3 121.0(11) . . ? C51 C50 C49 120.9(16) . . ? C52 C51 C50 119.8(17) . . ? C51 C52 C53 121.5(17) . . ? C52 C53 C54 119.4(19) . . ? C49 C54 C53 122.7(16) . . ? O1 C55 C56 107.4(15) . . ? C57 C56 C55 108.3(19) . . ? C56 C57 C58 110.9(18) . . ? C57 C58 O1 104.6(13) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.527 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.136 # Attachment 'comp_6_728994.cif' data_mah191_comp_6_CCDC_728994 _database_code_depnum_ccdc_archive 'CCDC 728994' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H130 In8 Si8 _ 3 C7 H8' _chemical_formula_sum 'C165 H144 In8 Si8' _chemical_formula_weight 3270.08 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' Si Si 0.0817 0.0704 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.251(3) _cell_length_b 16.756(3) _cell_length_c 30.599(4) _cell_angle_alpha 79.021(17) _cell_angle_beta 85.710(17) _cell_angle_gamma 63.590(16) _cell_volume 7325(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 22.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.178 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.058 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3276 _exptl_absorpt_coefficient_mu 1.352 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7920 _exptl_absorpt_correction_T_max 0.9122 _exptl_absorpt_process_details ? _exptl_special_details ; crystal was weakly diffracting, which did not allow to observe intensity above theta = 22 ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'image plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38433 _diffrn_reflns_av_R_equivalents 0.2359 _diffrn_reflns_av_sigmaI/netI 0.4069 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 22.34 _reflns_number_total 17693 _reflns_number_gt 5604 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement 'STOE XCELL' _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXTL 5.01' _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. For smoothing ADP parameters for phnyl carbon atoms the soft restraint simu was used.Disordered toluene solvent molecules were modelled part -1 and without hydrogen atoms ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 17693 _refine_ls_number_parameters 1660 _refine_ls_number_restraints 1373 _refine_ls_R_factor_all 0.2018 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 0.627 _refine_ls_restrained_S_all 0.607 _refine_ls_shift/su_max 0.005 _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 0.73866(8) 0.31426(8) 0.65801(4) 0.0389(3) Uani 1 1 d . . . In2 In 0.84733(8) 0.12176(8) 0.69381(4) 0.0365(3) Uani 1 1 d . . . In3 In 0.70995(7) 0.27420(8) 0.75123(4) 0.0367(3) Uani 1 1 d . . . In4 In 0.80149(8) 0.39550(7) 0.71913(4) 0.0378(3) Uani 1 1 d . . . In5 In 0.93777(7) 0.25368(8) 0.67641(4) 0.0354(3) Uani 1 1 d . . . In6 In 1.01536(7) 0.08104(8) 0.74014(4) 0.0396(4) Uani 1 1 d . . . In7 In 0.84827(8) 0.09793(8) 0.79227(4) 0.0401(4) Uani 1 1 d . . . In8 In 0.91176(8) 0.23736(8) 0.78466(4) 0.0381(4) Uani 1 1 d . . . Si1 Si 0.6284(3) 0.4011(3) 0.59080(16) 0.0369(13) Uani 1 1 d . . . Si2 Si 0.8362(3) 0.0243(3) 0.63993(17) 0.0397(13) Uani 1 1 d . . . Si3 Si 0.5493(3) 0.2892(3) 0.78168(18) 0.0381(13) Uani 1 1 d . . . Si4 Si 0.7416(3) 0.5685(3) 0.70995(17) 0.0387(13) Uani 1 1 d . . . Si5 Si 1.0735(3) 0.2719(3) 0.63049(17) 0.0400(13) Uani 1 1 d . . . Si6 Si 1.1752(3) -0.0573(3) 0.75288(17) 0.0402(13) Uani 1 1 d . . . Si7 Si 0.8438(3) -0.0102(3) 0.86319(17) 0.0399(13) Uani 1 1 d . . . Si8 Si 0.9520(3) 0.3055(3) 0.84537(17) 0.0428(13) Uani 1 1 d . . . C1 C 0.5293(10) 0.5112(11) 0.6025(6) 0.044(4) Uani 1 1 d U . . C2 C 0.4466(10) 0.5449(11) 0.5787(6) 0.050(4) Uani 1 1 d U . . H2A H 0.4385 0.5118 0.5587 0.060 Uiso 1 1 calc R . . C3 C 0.3770(11) 0.6281(11) 0.5852(6) 0.054(5) Uani 1 1 d U . . H3A H 0.3226 0.6527 0.5676 0.065 Uiso 1 1 calc R . . C4 C 0.3817(11) 0.6758(11) 0.6145(6) 0.054(5) Uani 1 1 d U . . H4A H 0.3325 0.7324 0.6181 0.065 Uiso 1 1 calc R . . C5 C 0.4637(12) 0.6377(11) 0.6398(7) 0.060(5) Uani 1 1 d U . . H5A H 0.4697 0.6672 0.6621 0.073 Uiso 1 1 calc R . . C6 C 0.5325(11) 0.5602(11) 0.6323(6) 0.054(5) Uani 1 1 d U . . H6A H 0.5878 0.5376 0.6490 0.064 Uiso 1 1 calc R . . C7 C 0.6901(10) 0.4327(10) 0.5419(5) 0.039(4) Uani 1 1 d U . . C8 C 0.6510(11) 0.5065(11) 0.5100(6) 0.047(4) Uani 1 1 d U . . H8A H 0.5875 0.5452 0.5126 0.056 Uiso 1 1 calc R . . C9 C 0.6963(11) 0.5291(12) 0.4746(6) 0.060(5) Uani 1 1 d U . . H9A H 0.6632 0.5809 0.4529 0.072 Uiso 1 1 calc R . . C10 C 0.7910(12) 0.4778(12) 0.4691(6) 0.066(5) Uani 1 1 d U . . H10A H 0.8241 0.4926 0.4445 0.079 Uiso 1 1 calc R . . C11 C 0.8291(12) 0.4092(12) 0.5003(6) 0.064(5) Uani 1 1 d U . . H11A H 0.8935 0.3737 0.4982 0.077 Uiso 1 1 calc R . . C12 C 0.7848(11) 0.3813(12) 0.5373(6) 0.060(5) Uani 1 1 d U . . H12A H 0.8184 0.3289 0.5586 0.072 Uiso 1 1 calc R . . C13 C 0.5783(10) 0.3305(9) 0.5753(6) 0.036(4) Uani 1 1 d U . . C14 C 0.5825(10) 0.3115(11) 0.5336(6) 0.051(4) Uani 1 1 d U . . H14A H 0.6150 0.3329 0.5111 0.061 Uiso 1 1 calc R . . C15 C 0.5389(10) 0.2602(11) 0.5234(7) 0.058(5) Uani 1 1 d U . . H15A H 0.5424 0.2469 0.4943 0.070 Uiso 1 1 calc R . . C16 C 0.4919(13) 0.2304(11) 0.5559(8) 0.071(6) Uani 1 1 d U . . H16A H 0.4630 0.1963 0.5484 0.085 Uiso 1 1 calc R . . C17 C 0.4842(12) 0.2464(11) 0.5978(7) 0.068(5) Uani 1 1 d U . . H17A H 0.4524 0.2235 0.6201 0.081 Uiso 1 1 calc R . . C18 C 0.5275(11) 0.3005(10) 0.6066(6) 0.053(4) Uani 1 1 d U . . H18A H 0.5209 0.3165 0.6353 0.063 Uiso 1 1 calc R . . C19 C 0.8094(11) 0.0774(10) 0.5808(6) 0.043(4) Uani 1 1 d U . . C20 C 0.8497(12) 0.1337(12) 0.5587(7) 0.065(5) Uani 1 1 d U . . H20A H 0.8819 0.1541 0.5751 0.077 Uiso 1 1 calc R . . C21 C 0.8410(15) 0.1583(13) 0.5126(7) 0.083(6) Uani 1 1 d U . . H21A H 0.8745 0.1886 0.4967 0.099 Uiso 1 1 calc R . . C22 C 0.7829(14) 0.1384(11) 0.4896(7) 0.075(5) Uani 1 1 d U . . H22A H 0.7701 0.1642 0.4590 0.091 Uiso 1 1 calc R . . C23 C 0.7455(13) 0.0857(12) 0.5087(7) 0.069(5) Uani 1 1 d U . . H23A H 0.7135 0.0655 0.4922 0.083 Uiso 1 1 calc R . . C24 C 0.7557(12) 0.0617(10) 0.5541(6) 0.059(5) Uani 1 1 d U . . H24A H 0.7219 0.0306 0.5687 0.070 Uiso 1 1 calc R . . C25 C 0.7488(10) -0.0134(10) 0.6622(6) 0.040(4) Uani 1 1 d U . . C26 C 0.6592(11) 0.0499(11) 0.6709(7) 0.061(5) Uani 1 1 d U . . H26A H 0.6453 0.1124 0.6655 0.073 Uiso 1 1 calc R . . C27 C 0.5910(12) 0.0248(13) 0.6870(7) 0.072(6) Uani 1 1 d U . . H27A H 0.5338 0.0696 0.6950 0.086 Uiso 1 1 calc R . . C28 C 0.6032(11) -0.0620(13) 0.6919(7) 0.069(5) Uani 1 1 d U . . H28A H 0.5551 -0.0789 0.7009 0.082 Uiso 1 1 calc R . . C29 C 0.6905(11) -0.1241(11) 0.6826(7) 0.059(5) Uani 1 1 d U . . H29A H 0.7040 -0.1864 0.6864 0.070 Uiso 1 1 calc R . . C30 C 0.7565(11) -0.0983(11) 0.6685(6) 0.055(5) Uani 1 1 d U . . H30A H 0.8145 -0.1444 0.6623 0.066 Uiso 1 1 calc R . . C31 C 0.9491(10) -0.0817(10) 0.6400(6) 0.039(4) Uani 1 1 d U . . C32 C 0.9830(14) -0.1154(13) 0.6009(7) 0.086(7) Uani 1 1 d U . . H32A H 0.9510 -0.0840 0.5735 0.103 Uiso 1 1 calc R . . C33 C 1.0626(14) -0.1938(13) 0.6018(7) 0.089(7) Uani 1 1 d U . . H33A H 1.0863 -0.2147 0.5746 0.107 Uiso 1 1 calc R . . C34 C 1.1068(12) -0.2408(14) 0.6392(7) 0.072(6) Uani 1 1 d U . . H34A H 1.1601 -0.2963 0.6386 0.086 Uiso 1 1 calc R . . C35 C 1.0782(11) -0.2120(11) 0.6787(6) 0.056(5) Uani 1 1 d U . . H35A H 1.1114 -0.2451 0.7056 0.067 Uiso 1 1 calc R . . C36 C 0.9991(12) -0.1325(11) 0.6779(6) 0.055(5) Uani 1 1 d U . . H36A H 0.9779 -0.1115 0.7052 0.067 Uiso 1 1 calc R . . C37 C 0.4624(9) 0.3460(10) 0.7361(6) 0.037(4) Uani 1 1 d U . . C38 C 0.4077(10) 0.3098(10) 0.7224(6) 0.044(4) Uani 1 1 d U . . H38A H 0.4161 0.2513 0.7371 0.053 Uiso 1 1 calc R . . C39 C 0.3446(11) 0.3520(11) 0.6900(6) 0.056(5) Uani 1 1 d U . . H39A H 0.3178 0.3192 0.6792 0.067 Uiso 1 1 calc R . . C40 C 0.3180(12) 0.4393(12) 0.6721(6) 0.068(5) Uani 1 1 d U . . H40A H 0.2674 0.4702 0.6519 0.082 Uiso 1 1 calc R . . C41 C 0.3651(10) 0.4840(11) 0.6835(6) 0.054(5) Uani 1 1 d U . . H41A H 0.3493 0.5449 0.6700 0.065 Uiso 1 1 calc R . . C42 C 0.4356(9) 0.4388(10) 0.7149(5) 0.036(4) Uani 1 1 d U . . H42A H 0.4674 0.4701 0.7227 0.043 Uiso 1 1 calc R . . C43 C 0.5140(10) 0.3615(10) 0.8260(6) 0.039(4) Uani 1 1 d U . . C44 C 0.4210(10) 0.4253(11) 0.8291(6) 0.050(5) Uani 1 1 d U . . H44A H 0.3773 0.4353 0.8073 0.060 Uiso 1 1 calc R . . C45 C 0.3950(13) 0.4718(13) 0.8635(7) 0.073(6) Uani 1 1 d U . . H45A H 0.3327 0.5149 0.8646 0.088 Uiso 1 1 calc R . . C46 C 0.4529(15) 0.4601(13) 0.8961(7) 0.088(7) Uani 1 1 d U . . H46A H 0.4329 0.4957 0.9190 0.106 Uiso 1 1 calc R . . C47 C 0.5449(14) 0.3929(14) 0.8950(7) 0.079(6) Uani 1 1 d U . . H47A H 0.5868 0.3789 0.9184 0.094 Uiso 1 1 calc R . . C48 C 0.5718(11) 0.3491(11) 0.8598(6) 0.055(5) Uani 1 1 d U . . H48A H 0.6345 0.3071 0.8585 0.066 Uiso 1 1 calc R . . C49 C 0.5428(9) 0.1830(10) 0.8064(6) 0.040(4) Uani 1 1 d U . . C50 C 0.4826(11) 0.1797(11) 0.8391(7) 0.069(5) Uani 1 1 d U . . H50A H 0.4494 0.2332 0.8513 0.083 Uiso 1 1 calc R . . C51 C 0.4640(10) 0.1073(12) 0.8565(6) 0.057(5) Uani 1 1 d U . . H51A H 0.4210 0.1101 0.8796 0.069 Uiso 1 1 calc R . . C52 C 0.5142(12) 0.0273(13) 0.8373(7) 0.079(6) Uani 1 1 d U . . H52A H 0.5051 -0.0251 0.8485 0.094 Uiso 1 1 calc R . . C53 C 0.5744(11) 0.0244(11) 0.8035(7) 0.064(5) Uani 1 1 d U . . H53A H 0.6044 -0.0274 0.7897 0.077 Uiso 1 1 calc R . . C54 C 0.5910(10) 0.1045(11) 0.7894(6) 0.056(5) Uani 1 1 d U . . H54A H 0.6365 0.1022 0.7676 0.067 Uiso 1 1 calc R . . C55 C 0.7096(9) 0.6168(9) 0.6500(5) 0.028(3) Uani 1 1 d U . . C56 C 0.7562(11) 0.5734(11) 0.6161(6) 0.046(4) Uani 1 1 d U . . H56A H 0.8062 0.5152 0.6234 0.055 Uiso 1 1 calc R . . C57 C 0.7353(11) 0.6087(11) 0.5724(6) 0.043(4) Uani 1 1 d U . . H57A H 0.7692 0.5745 0.5503 0.052 Uiso 1 1 calc R . . C58 C 0.6643(12) 0.6947(12) 0.5600(7) 0.063(5) Uani 1 1 d U . . H58A H 0.6495 0.7210 0.5296 0.075 Uiso 1 1 calc R . . C59 C 0.6166(11) 0.7401(12) 0.5933(7) 0.061(5) Uani 1 1 d U . . H59A H 0.5663 0.7982 0.5857 0.074 Uiso 1 1 calc R . . C60 C 0.6391(10) 0.7045(10) 0.6371(6) 0.048(4) Uani 1 1 d U . . H60A H 0.6067 0.7395 0.6592 0.057 Uiso 1 1 calc R . . C61 C 0.8320(10) 0.6037(9) 0.7248(6) 0.035(4) Uani 1 1 d U . . C62 C 0.8740(10) 0.6388(11) 0.6935(6) 0.046(4) Uani 1 1 d U . . H62A H 0.8575 0.6474 0.6632 0.055 Uiso 1 1 calc R . . C63 C 0.9403(12) 0.6633(12) 0.7030(7) 0.065(5) Uani 1 1 d U . . H63A H 0.9691 0.6881 0.6800 0.078 Uiso 1 1 calc R . . C64 C 0.9631(13) 0.6507(13) 0.7465(8) 0.076(6) Uani 1 1 d U . . H64A H 1.0088 0.6667 0.7540 0.091 Uiso 1 1 calc R . . C65 C 0.9217(13) 0.6157(12) 0.7791(8) 0.075(5) Uani 1 1 d U . . H65A H 0.9388 0.6071 0.8092 0.091 Uiso 1 1 calc R . . C66 C 0.8562(12) 0.5927(11) 0.7694(6) 0.056(5) Uani 1 1 d U . . H66A H 0.8266 0.5692 0.7926 0.067 Uiso 1 1 calc R . . C67 C 0.6409(10) 0.6130(10) 0.7465(6) 0.046(4) Uani 1 1 d U . . C68 C 0.5826(9) 0.5727(10) 0.7566(6) 0.045(4) Uani 1 1 d U . . H68A H 0.5966 0.5196 0.7449 0.054 Uiso 1 1 calc R . . C69 C 0.5057(11) 0.6038(12) 0.7824(7) 0.068(5) Uani 1 1 d U . . H69A H 0.4664 0.5748 0.7875 0.082 Uiso 1 1 calc R . . C70 C 0.4877(11) 0.6806(12) 0.8010(7) 0.068(5) Uani 1 1 d U . . H70A H 0.4383 0.7014 0.8210 0.082 Uiso 1 1 calc R . . C71 C 0.5413(11) 0.7253(12) 0.7901(7) 0.065(5) Uani 1 1 d U . . H71A H 0.5253 0.7806 0.8001 0.078 Uiso 1 1 calc R . . C72 C 0.6166(11) 0.6909(11) 0.7653(6) 0.053(5) Uani 1 1 d U . . H72A H 0.6553 0.7206 0.7603 0.063 Uiso 1 1 calc R . . C73 C 1.0922(10) 0.2285(11) 0.5770(6) 0.046(4) Uani 1 1 d U . . C74 C 1.1361(11) 0.2561(12) 0.5434(6) 0.057(5) Uani 1 1 d U . . H74A H 1.1557 0.3000 0.5471 0.068 Uiso 1 1 calc R . . C75 C 1.1550(12) 0.2244(13) 0.5031(7) 0.071(5) Uani 1 1 d U . . H75A H 1.1866 0.2464 0.4803 0.085 Uiso 1 1 calc R . . C76 C 1.1271(13) 0.1609(13) 0.4968(7) 0.080(6) Uani 1 1 d U . . H76A H 1.1400 0.1373 0.4699 0.096 Uiso 1 1 calc R . . C77 C 1.0797(13) 0.1325(13) 0.5307(8) 0.081(6) Uani 1 1 d U . . H77A H 1.0573 0.0915 0.5254 0.097 Uiso 1 1 calc R . . C78 C 1.0630(12) 0.1585(11) 0.5705(7) 0.067(5) Uani 1 1 d U . . H78A H 1.0341 0.1337 0.5935 0.080 Uiso 1 1 calc R . . C79 C 1.1767(10) 0.2160(10) 0.6650(6) 0.039(4) Uani 1 1 d U . . C80 C 1.1824(11) 0.2246(9) 0.7093(6) 0.042(4) Uani 1 1 d U . . H80A H 1.1263 0.2579 0.7232 0.050 Uiso 1 1 calc R . . C81 C 1.2626(11) 0.1890(10) 0.7349(6) 0.051(4) Uani 1 1 d U . . H81A H 1.2637 0.2063 0.7625 0.061 Uiso 1 1 calc R . . C82 C 1.3402(11) 0.1268(12) 0.7172(6) 0.057(5) Uani 1 1 d U . . H82A H 1.3938 0.0935 0.7354 0.068 Uiso 1 1 calc R . . C83 C 1.3433(11) 0.1113(11) 0.6752(7) 0.054(5) Uani 1 1 d U . . H83A H 1.3991 0.0708 0.6637 0.065 Uiso 1 1 calc R . . C84 C 1.2646(10) 0.1547(11) 0.6491(6) 0.053(5) Uani 1 1 d U . . H84A H 1.2681 0.1441 0.6195 0.064 Uiso 1 1 calc R . . C85 C 1.0433(9) 0.3949(9) 0.6154(5) 0.031(4) Uani 1 1 d U . . C86 C 0.9917(10) 0.4489(11) 0.5780(6) 0.049(4) Uani 1 1 d U . . H86A H 0.9675 0.4231 0.5604 0.058 Uiso 1 1 calc R . . C87 C 0.9736(11) 0.5383(11) 0.5650(7) 0.061(5) Uani 1 1 d U . . H87A H 0.9404 0.5719 0.5382 0.073 Uiso 1 1 calc R . . C88 C 1.0043(11) 0.5800(12) 0.5914(7) 0.066(5) Uani 1 1 d U . . H88A H 0.9872 0.6431 0.5842 0.079 Uiso 1 1 calc R . . C89 C 1.0578(12) 0.5297(11) 0.6267(6) 0.058(5) Uani 1 1 d U . . H89A H 1.0816 0.5567 0.6438 0.069 Uiso 1 1 calc R . . C90 C 1.0799(11) 0.4351(11) 0.6392(6) 0.053(4) Uani 1 1 d U . . H90A H 1.1198 0.3997 0.6639 0.064 Uiso 1 1 calc R . . C91 C 1.2356(10) -0.0492(10) 0.7998(6) 0.042(4) Uani 1 1 d U . . C92 C 1.2224(12) 0.0365(11) 0.8093(7) 0.065(5) Uani 1 1 d U . . H92A H 1.1807 0.0914 0.7919 0.078 Uiso 1 1 calc R . . C93 C 1.2711(13) 0.0383(13) 0.8442(7) 0.074(6) Uani 1 1 d U . . H93A H 1.2665 0.0949 0.8484 0.089 Uiso 1 1 calc R . . C94 C 1.3247(12) -0.0371(13) 0.8724(7) 0.070(5) Uani 1 1 d U . . H94A H 1.3515 -0.0324 0.8977 0.084 Uiso 1 1 calc R . . C95 C 1.3400(12) -0.1174(13) 0.8647(7) 0.072(6) Uani 1 1 d U . . H95A H 1.3808 -0.1709 0.8835 0.086 Uiso 1 1 calc R . . C96 C 1.2953(11) -0.1233(11) 0.8287(6) 0.057(5) Uani 1 1 d U . . H96A H 1.3070 -0.1818 0.8240 0.069 Uiso 1 1 calc R . . C97 C 1.1714(10) -0.1687(10) 0.7684(6) 0.045(4) Uani 1 1 d U . . C98 C 1.1052(12) -0.1828(12) 0.7918(6) 0.051(4) Uani 1 1 d U . . H98A H 1.0559 -0.1322 0.8015 0.061 Uiso 1 1 calc R . . C99 C 1.1030(13) -0.2668(12) 0.8033(6) 0.059(5) Uani 1 1 d U . . H99A H 1.0524 -0.2725 0.8187 0.071 Uiso 1 1 calc R . . C100 C 1.1784(13) -0.3422(12) 0.7912(6) 0.066(5) Uani 1 1 d U . . H10B H 1.1797 -0.4005 0.7983 0.079 Uiso 1 1 calc R . . C101 C 1.2483(13) -0.3317(12) 0.7696(7) 0.063(5) Uani 1 1 d U . . H10C H 1.3017 -0.3836 0.7639 0.076 Uiso 1 1 calc R . . C102 C 1.2446(10) -0.2468(11) 0.7553(6) 0.050(4) Uani 1 1 d U . . H10D H 1.2914 -0.2404 0.7365 0.060 Uiso 1 1 calc R . . C103 C 1.2440(10) -0.0627(10) 0.7008(6) 0.041(4) Uani 1 1 d U . . C104 C 1.2027(12) -0.0468(11) 0.6597(7) 0.058(5) Uani 1 1 d U . . H10E H 1.1385 -0.0288 0.6583 0.070 Uiso 1 1 calc R . . C105 C 1.2530(13) -0.0567(12) 0.6204(7) 0.069(5) Uani 1 1 d U . . H10F H 1.2226 -0.0412 0.5926 0.083 Uiso 1 1 calc R . . C106 C 1.3474(12) -0.0891(11) 0.6223(7) 0.061(5) Uani 1 1 d U . . H10G H 1.3831 -0.0996 0.5961 0.073 Uiso 1 1 calc R . . C107 C 1.3874(12) -0.1053(11) 0.6615(7) 0.058(5) Uani 1 1 d U . . H10H H 1.4520 -0.1259 0.6627 0.070 Uiso 1 1 calc R . . C108 C 1.3388(10) -0.0935(10) 0.6998(6) 0.048(4) Uani 1 1 d U . . H10I H 1.3709 -0.1067 0.7270 0.058 Uiso 1 1 calc R . . C109 C 0.7983(10) -0.0876(10) 0.8510(6) 0.038(4) Uani 1 1 d U . . C110 C 0.8095(11) -0.1169(11) 0.8106(6) 0.052(4) Uani 1 1 d U . . H11B H 0.8392 -0.0933 0.7875 0.063 Uiso 1 1 calc R . . C111 C 0.7809(12) -0.1774(11) 0.8018(7) 0.061(5) Uani 1 1 d U . . H11C H 0.7866 -0.1916 0.7728 0.073 Uiso 1 1 calc R . . C112 C 0.7435(12) -0.2175(12) 0.8356(7) 0.062(5) Uani 1 1 d U . . H11D H 0.7236 -0.2602 0.8302 0.074 Uiso 1 1 calc R . . C113 C 0.7353(11) -0.1959(11) 0.8766(7) 0.056(5) Uani 1 1 d U . . H11E H 0.7112 -0.2247 0.9002 0.067 Uiso 1 1 calc R . . C114 C 0.7618(11) -0.1324(11) 0.8841(6) 0.051(4) Uani 1 1 d U . . H11F H 0.7550 -0.1182 0.9131 0.061 Uiso 1 1 calc R . . C115 C 0.9664(10) -0.0822(10) 0.8830(5) 0.037(4) Uani 1 1 d U . . C116 C 1.0042(11) -0.1766(10) 0.8971(6) 0.049(5) Uani 1 1 d U . . H11G H 0.9654 -0.2054 0.8971 0.059 Uiso 1 1 calc R . . C117 C 1.0906(11) -0.2277(12) 0.9105(6) 0.057(5) Uani 1 1 d U . . H11H H 1.1122 -0.2909 0.9208 0.069 Uiso 1 1 calc R . . C118 C 1.1507(11) -0.1854(12) 0.9090(6) 0.054(5) Uani 1 1 d U . . H11I H 1.2140 -0.2209 0.9165 0.065 Uiso 1 1 calc R . . C119 C 1.1164(11) -0.0947(12) 0.8968(6) 0.056(5) Uani 1 1 d U . . H11J H 1.1555 -0.0661 0.8968 0.067 Uiso 1 1 calc R . . C120 C 1.0264(11) -0.0434(11) 0.8845(5) 0.046(4) Uani 1 1 d U . . H12B H 1.0039 0.0205 0.8767 0.055 Uiso 1 1 calc R . . C121 C 0.7721(11) 0.0573(10) 0.9073(6) 0.042(4) Uani 1 1 d U . . C122 C 0.6779(11) 0.0823(11) 0.9088(6) 0.053(4) Uani 1 1 d U . . H12C H 0.6499 0.0662 0.8880 0.063 Uiso 1 1 calc R . . C123 C 0.6257(12) 0.1308(13) 0.9409(7) 0.075(6) Uani 1 1 d U . . H12D H 0.5627 0.1434 0.9444 0.090 Uiso 1 1 calc R . . C124 C 0.6668(14) 0.1603(14) 0.9676(7) 0.087(7) Uani 1 1 d U . . H12E H 0.6293 0.2019 0.9862 0.105 Uiso 1 1 calc R . . C125 C 0.7562(14) 0.1330(14) 0.9683(7) 0.090(7) Uani 1 1 d U . . H12F H 0.7838 0.1470 0.9902 0.108 Uiso 1 1 calc R . . C126 C 0.8081(12) 0.0847(11) 0.9374(6) 0.055(5) Uani 1 1 d U . . H12G H 0.8720 0.0691 0.9365 0.066 Uiso 1 1 calc R . . C127 C 0.9781(14) 0.2284(12) 0.9006(6) 0.059(5) Uani 1 1 d U . . C128 C 1.0577(16) 0.1463(15) 0.9083(7) 0.092(6) Uani 1 1 d U . . H12H H 1.0987 0.1287 0.8843 0.111 Uiso 1 1 calc R . . C129 C 1.0798(17) 0.0882(14) 0.9504(8) 0.094(6) Uani 1 1 d U . . H12I H 1.1327 0.0315 0.9549 0.112 Uiso 1 1 calc R . . C130 C 1.019(2) 0.1191(16) 0.9849(8) 0.112(8) Uani 1 1 d U . . H13A H 1.0304 0.0828 1.0138 0.135 Uiso 1 1 calc R . . C131 C 0.950(2) 0.1950(17) 0.9780(8) 0.122(8) Uani 1 1 d U . . H13B H 0.9131 0.2156 1.0028 0.147 Uiso 1 1 calc R . . C132 C 0.9235(16) 0.2498(14) 0.9371(7) 0.082(6) Uani 1 1 d U . . H13C H 0.8670 0.3032 0.9341 0.099 Uiso 1 1 calc R . . C133 C 0.8538(10) 0.4130(10) 0.8575(5) 0.036(4) Uani 1 1 d U . . C134 C 0.7625(11) 0.4373(11) 0.8514(6) 0.049(4) Uani 1 1 d U . . H13D H 0.7453 0.4005 0.8378 0.059 Uiso 1 1 calc R . . C135 C 0.6936(12) 0.5162(12) 0.8649(6) 0.060(5) Uani 1 1 d U . . H13E H 0.6310 0.5326 0.8592 0.073 Uiso 1 1 calc R . . C136 C 0.7140(12) 0.5675(12) 0.8853(6) 0.056(5) Uani 1 1 d U . . H13F H 0.6663 0.6186 0.8953 0.067 Uiso 1 1 calc R . . C137 C 0.8078(12) 0.5464(11) 0.8925(6) 0.056(5) Uani 1 1 d U . . H13G H 0.8237 0.5848 0.9056 0.068 Uiso 1 1 calc R . . C138 C 0.8735(12) 0.4696(11) 0.8799(5) 0.045(4) Uani 1 1 d U . . H13H H 0.9359 0.4528 0.8865 0.054 Uiso 1 1 calc R . . C139 C 1.0515(10) 0.3297(10) 0.8277(6) 0.038(4) Uani 1 1 d U . . C140 C 1.0519(11) 0.3791(11) 0.7865(6) 0.051(4) Uani 1 1 d U . . H14B H 1.0028 0.3973 0.7662 0.061 Uiso 1 1 calc R . . C141 C 1.1222(12) 0.4026(13) 0.7744(7) 0.066(5) Uani 1 1 d U . . H14C H 1.1185 0.4394 0.7461 0.079 Uiso 1 1 calc R . . C142 C 1.1993(13) 0.3750(14) 0.8014(7) 0.076(6) Uani 1 1 d U . . H14D H 1.2484 0.3903 0.7922 0.091 Uiso 1 1 calc R . . C143 C 1.1986(12) 0.3244(13) 0.8423(8) 0.077(6) Uani 1 1 d U . . H14E H 1.2490 0.3035 0.8621 0.092 Uiso 1 1 calc R . . C144 C 1.1287(11) 0.3035(12) 0.8549(7) 0.061(5) Uani 1 1 d U . . H14F H 1.1314 0.2692 0.8838 0.073 Uiso 1 1 calc R . . C145 C 1.0099(15) -0.3919(13) 0.9651(9) 0.081(6) Uani 1 1 d U . . C146 C 1.0013(15) -0.4043(15) 0.9217(9) 0.093(7) Uani 1 1 d U . . H14G H 0.9423 -0.3784 0.9081 0.111 Uiso 1 1 calc R . . C147 C 1.0806(19) -0.4554(15) 0.8985(9) 0.107(8) Uani 1 1 d U . . H14H H 1.0785 -0.4564 0.8676 0.128 Uiso 1 1 calc R . . C148 C 1.1567(18) -0.5012(16) 0.9220(10) 0.114(9) Uani 1 1 d U . . H14I H 1.2095 -0.5421 0.9087 0.137 Uiso 1 1 calc R . . C149 C 1.1631(18) -0.4924(15) 0.9650(10) 0.126(10) Uani 1 1 d U . . H14J H 1.2198 -0.5287 0.9805 0.152 Uiso 1 1 calc R . . C150 C 1.093(2) -0.4349(15) 0.9863(9) 0.132(10) Uani 1 1 d U . . H15B H 1.1009 -0.4248 1.0149 0.158 Uiso 1 1 calc R . . C151 C 0.9264(18) -0.3320(17) 0.9879(10) 0.164(11) Uani 1 1 d U . . H15C H 0.8815 -0.3569 0.9914 0.245 Uiso 1 1 calc R . . H15D H 0.8991 -0.2711 0.9699 0.245 Uiso 1 1 calc R . . H15E H 0.9440 -0.3289 1.0172 0.245 Uiso 1 1 calc R . . C152 C 0.340(3) 0.162(2) 0.9869(14) 0.183(13) Uani 1 1 d U . . C153 C 0.330(2) 0.2359(19) 0.9753(12) 0.165(11) Uani 1 1 d U . . H15F H 0.2819 0.2740 0.9542 0.198 Uiso 1 1 calc R . . C154 C 0.3858(18) 0.2761(18) 0.9906(14) 0.198(17) Uani 1 1 d U . . H15G H 0.3840 0.3335 0.9785 0.238 Uiso 1 1 calc R . . C155 C 0.442(2) 0.213(2) 1.0265(13) 0.182(14) Uani 1 1 d U . . H15H H 0.4765 0.2268 1.0450 0.219 Uiso 1 1 calc R . . C156 C 0.442(2) 0.136(2) 1.0315(13) 0.195(13) Uani 1 1 d U . . H15I H 0.4931 0.0927 1.0498 0.234 Uiso 1 1 calc R . . C157 C 0.393(2) 0.094(2) 1.0195(11) 0.177(13) Uani 1 1 d DU . . H15J H 0.3960 0.0357 1.0304 0.213 Uiso 1 1 calc R . . C158 C 0.288(2) 0.118(2) 0.9760(10) 0.218(16) Uani 1 1 d DU . . H15L H 0.2778 0.1304 0.9437 0.327 Uiso 1 1 calc R . . H15M H 0.2279 0.1405 0.9909 0.327 Uiso 1 1 calc R . . H15N H 0.3214 0.0524 0.9862 0.327 Uiso 1 1 calc R . . C159 C 1.429(2) 0.0396(16) 0.5262(13) 0.134(12) Uani 1 1 d U . . H159 H 1.3779 0.0699 0.5438 0.160 Uiso 1 1 calc R . . C160 C 1.514(2) -0.0022(17) 0.5420(12) 0.145(12) Uani 1 1 d DU . . C161 C 1.580(2) -0.0358(17) 0.5176(15) 0.153(12) Uani 1 1 d U . . H161 H 1.6399 -0.0607 0.5297 0.183 Uiso 1 1 calc R . . C162 C 1.552(4) -0.015(4) 0.5882(15) 0.21(3) Uani 0.50 1 d PDU A -1 H16B H 1.6076 -0.0728 0.5939 0.310 Uiso 0.50 1 calc PR A -1 H16C H 1.5058 -0.0161 0.6105 0.310 Uiso 0.50 1 calc PR A -1 H16D H 1.5671 0.0345 0.5900 0.310 Uiso 0.50 1 calc PR A -1 C163 C 0.609(3) 0.466(3) 0.9881(19) 0.131(13) Uani 0.50 1 d PDU B -1 C164 C 0.534(2) 0.547(2) 0.9766(10) 0.125(9) Uani 1 1 d DU B -1 C165 C 0.449(3) 0.618(3) 0.969(2) 0.129(18) Uani 0.50 1 d PDU B -1 C166 C 0.617(5) 0.380(3) 1.0189(17) 0.127(14) Uani 0.50 1 d PDU B -1 C167 C 0.551(4) 0.471(4) 0.995(2) 0.124(12) Uani 0.50 1 d PU B -1 C168 C 0.654(4) 0.410(5) 1.001(2) 0.127(14) Uani 0.50 1 d PU B -1 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 0.0370(7) 0.0380(7) 0.0390(10) -0.0022(6) -0.0104(6) -0.0141(6) In2 0.0381(7) 0.0299(7) 0.0428(10) -0.0077(6) -0.0049(6) -0.0147(6) In3 0.0273(7) 0.0323(7) 0.0478(10) -0.0068(6) 0.0014(6) -0.0110(6) In4 0.0354(7) 0.0264(7) 0.0488(10) -0.0063(6) -0.0048(6) -0.0104(6) In5 0.0312(7) 0.0333(7) 0.0401(10) -0.0024(6) 0.0020(6) -0.0144(6) In6 0.0275(7) 0.0326(7) 0.0488(10) -0.0039(6) -0.0007(6) -0.0056(6) In7 0.0365(7) 0.0350(7) 0.0427(10) 0.0010(6) 0.0008(6) -0.0135(6) In8 0.0414(8) 0.0333(7) 0.0394(10) -0.0069(7) -0.0079(6) -0.0149(6) Si1 0.034(3) 0.039(3) 0.035(4) -0.003(2) -0.004(2) -0.015(2) Si2 0.041(3) 0.037(3) 0.043(4) -0.003(2) -0.009(2) -0.019(2) Si3 0.027(3) 0.028(3) 0.058(4) -0.008(2) 0.000(2) -0.010(2) Si4 0.040(3) 0.035(3) 0.045(4) -0.011(2) -0.001(2) -0.018(2) Si5 0.033(3) 0.028(3) 0.053(4) -0.011(2) 0.000(2) -0.006(2) Si6 0.031(3) 0.039(3) 0.042(4) -0.002(2) 0.002(2) -0.010(2) Si7 0.038(3) 0.036(3) 0.040(4) -0.001(2) 0.002(2) -0.014(2) Si8 0.050(3) 0.039(3) 0.040(4) -0.012(3) -0.002(3) -0.018(2) C1 0.040(8) 0.052(10) 0.035(12) -0.010(7) 0.002(7) -0.016(7) C2 0.039(9) 0.049(9) 0.060(13) -0.016(9) 0.009(7) -0.017(7) C3 0.038(8) 0.048(10) 0.068(14) -0.007(8) -0.009(8) -0.010(6) C4 0.049(9) 0.045(10) 0.054(13) -0.008(8) 0.011(8) -0.009(7) C5 0.068(11) 0.035(9) 0.079(14) -0.018(9) -0.011(9) -0.018(7) C6 0.043(9) 0.045(10) 0.082(14) -0.021(9) 0.009(8) -0.025(6) C7 0.040(7) 0.039(9) 0.027(10) 0.005(6) -0.009(7) -0.011(7) C8 0.044(9) 0.046(10) 0.038(12) 0.007(7) -0.006(7) -0.014(7) C9 0.048(8) 0.084(12) 0.038(12) 0.019(9) -0.011(8) -0.029(8) C10 0.060(9) 0.073(13) 0.043(12) 0.012(8) 0.013(9) -0.021(9) C11 0.050(9) 0.065(12) 0.053(13) 0.005(8) 0.012(8) -0.011(8) C12 0.049(8) 0.056(11) 0.033(12) 0.015(8) 0.006(8) 0.004(7) C13 0.030(8) 0.013(8) 0.055(11) -0.001(7) -0.024(7) 0.000(6) C14 0.031(9) 0.048(11) 0.062(10) -0.007(9) -0.024(8) -0.004(7) C15 0.026(9) 0.049(11) 0.081(12) -0.021(9) -0.033(8) 0.009(7) C16 0.073(12) 0.031(10) 0.116(15) -0.007(11) -0.033(11) -0.026(8) C17 0.063(11) 0.048(11) 0.092(13) 0.014(10) -0.023(10) -0.031(8) C18 0.063(11) 0.021(9) 0.061(11) 0.005(8) -0.019(8) -0.008(7) C19 0.064(11) 0.028(9) 0.038(10) -0.013(7) 0.000(8) -0.020(7) C20 0.090(13) 0.069(12) 0.043(10) -0.007(10) 0.003(10) -0.043(9) C21 0.143(16) 0.086(13) 0.043(10) -0.006(10) 0.004(11) -0.074(11) C22 0.122(15) 0.032(11) 0.062(12) 0.000(9) -0.029(10) -0.022(9) C23 0.101(13) 0.048(11) 0.062(11) -0.016(10) -0.029(11) -0.027(9) C24 0.084(12) 0.029(9) 0.057(10) -0.017(8) -0.019(9) -0.013(8) C25 0.029(7) 0.038(8) 0.069(12) -0.023(8) -0.006(7) -0.023(6) C26 0.047(9) 0.038(8) 0.104(15) -0.036(10) 0.006(10) -0.016(6) C27 0.034(9) 0.066(9) 0.114(16) -0.047(12) 0.019(10) -0.011(8) C28 0.041(8) 0.083(11) 0.097(15) -0.026(12) 0.010(10) -0.039(8) C29 0.055(9) 0.033(8) 0.100(15) -0.017(9) -0.005(10) -0.028(6) C30 0.040(8) 0.037(7) 0.096(15) -0.022(10) 0.004(9) -0.021(7) C31 0.049(9) 0.037(9) 0.039(10) -0.018(7) 0.001(7) -0.021(7) C32 0.101(14) 0.068(12) 0.034(10) -0.006(10) 0.006(10) 0.009(9) C33 0.085(14) 0.082(14) 0.045(11) -0.010(10) 0.019(10) 0.010(9) C34 0.042(10) 0.087(13) 0.066(13) -0.018(10) -0.003(9) -0.007(9) C35 0.056(10) 0.054(10) 0.061(11) -0.013(9) -0.017(9) -0.022(7) C36 0.068(11) 0.053(10) 0.043(10) -0.009(8) -0.010(8) -0.023(7) C37 0.013(7) 0.044(7) 0.059(11) -0.003(7) 0.000(6) -0.020(6) C38 0.033(9) 0.025(8) 0.079(13) -0.003(8) -0.003(7) -0.018(7) C39 0.059(11) 0.048(9) 0.073(14) -0.015(9) -0.019(8) -0.029(9) C40 0.059(11) 0.070(10) 0.069(14) 0.018(9) -0.030(9) -0.028(9) C41 0.039(10) 0.042(9) 0.076(14) 0.008(8) -0.001(8) -0.019(7) C42 0.021(8) 0.031(7) 0.058(12) -0.016(7) 0.015(6) -0.013(7) C43 0.039(8) 0.048(10) 0.031(10) 0.005(8) 0.012(7) -0.027(7) C44 0.034(7) 0.063(12) 0.050(12) -0.006(9) -0.001(8) -0.020(7) C45 0.073(11) 0.070(13) 0.050(14) -0.011(10) 0.013(8) -0.009(9) C46 0.098(13) 0.079(14) 0.079(15) -0.048(12) 0.005(10) -0.019(10) C47 0.082(11) 0.083(14) 0.077(14) -0.030(11) -0.003(10) -0.034(9) C48 0.033(8) 0.057(11) 0.079(14) -0.023(9) -0.007(7) -0.019(8) C49 0.008(7) 0.051(8) 0.055(10) -0.001(7) -0.002(6) -0.012(6) C50 0.037(10) 0.041(8) 0.083(14) 0.023(9) 0.026(8) 0.006(8) C51 0.033(10) 0.060(10) 0.081(14) -0.005(9) 0.012(8) -0.028(8) C52 0.058(12) 0.064(10) 0.102(17) -0.006(10) 0.012(9) -0.022(9) C53 0.044(11) 0.035(8) 0.088(15) -0.003(9) 0.001(8) 0.001(8) C54 0.031(9) 0.042(9) 0.075(13) -0.006(8) 0.002(8) -0.001(7) C55 0.033(8) 0.020(7) 0.037(9) 0.006(6) 0.004(6) -0.021(6) C56 0.054(10) 0.055(10) 0.029(9) 0.002(7) -0.005(7) -0.028(7) C57 0.056(10) 0.053(9) 0.033(8) -0.001(8) -0.019(8) -0.035(7) C58 0.065(12) 0.064(11) 0.059(11) 0.009(8) -0.022(9) -0.033(8) C59 0.043(10) 0.048(10) 0.066(11) 0.025(8) -0.014(9) -0.008(8) C60 0.041(9) 0.031(8) 0.061(10) 0.007(8) -0.024(8) -0.010(6) C61 0.036(8) 0.006(7) 0.054(10) 0.007(7) -0.009(7) -0.005(6) C62 0.044(10) 0.056(11) 0.049(10) -0.018(8) 0.011(8) -0.030(8) C63 0.061(11) 0.070(12) 0.094(12) -0.042(11) 0.015(10) -0.046(9) C64 0.063(12) 0.085(13) 0.110(15) -0.036(13) -0.009(11) -0.050(9) C65 0.078(13) 0.070(13) 0.087(13) -0.022(11) -0.017(10) -0.034(9) C66 0.058(11) 0.055(11) 0.053(9) 0.007(9) -0.006(9) -0.028(8) C67 0.025(8) 0.031(9) 0.084(13) -0.026(8) -0.003(7) -0.008(7) C68 0.011(7) 0.032(8) 0.092(12) -0.033(8) -0.002(7) 0.000(6) C69 0.027(9) 0.061(11) 0.103(16) -0.019(10) 0.010(8) -0.006(8) C70 0.018(8) 0.069(11) 0.096(14) -0.034(9) 0.017(8) 0.004(7) C71 0.036(10) 0.049(10) 0.089(15) -0.021(9) 0.009(8) 0.003(7) C72 0.039(9) 0.049(10) 0.080(14) -0.043(9) 0.011(8) -0.018(8) C73 0.035(10) 0.042(10) 0.040(11) -0.005(8) 0.008(7) -0.001(7) C74 0.050(11) 0.059(11) 0.056(13) -0.019(9) 0.018(9) -0.019(8) C75 0.075(12) 0.069(13) 0.053(12) -0.018(10) 0.032(10) -0.021(9) C76 0.084(14) 0.062(13) 0.074(13) -0.036(11) 0.015(10) -0.006(9) C77 0.091(14) 0.068(13) 0.087(15) -0.032(11) 0.012(11) -0.033(10) C78 0.070(12) 0.032(10) 0.083(13) -0.023(9) 0.015(10) -0.007(8) C79 0.049(8) 0.030(9) 0.052(10) -0.019(8) 0.014(7) -0.028(6) C80 0.045(8) 0.018(8) 0.052(10) -0.011(8) 0.006(7) -0.003(7) C81 0.047(9) 0.030(9) 0.072(12) -0.008(8) -0.010(7) -0.014(7) C82 0.032(8) 0.065(11) 0.066(11) 0.004(9) -0.015(8) -0.019(7) C83 0.033(8) 0.061(11) 0.076(12) -0.016(10) 0.002(7) -0.027(7) C84 0.044(9) 0.066(11) 0.038(10) -0.014(9) 0.007(6) -0.013(8) C85 0.021(8) 0.027(8) 0.045(11) -0.004(6) 0.015(6) -0.015(6) C86 0.030(9) 0.055(9) 0.061(12) 0.006(8) 0.000(7) -0.025(8) C87 0.049(10) 0.047(9) 0.067(13) 0.015(8) 0.007(9) -0.014(8) C88 0.053(12) 0.041(9) 0.079(15) -0.009(8) 0.014(9) -0.001(8) C89 0.070(12) 0.036(8) 0.066(13) -0.022(8) 0.019(8) -0.021(9) C90 0.067(11) 0.039(8) 0.050(12) -0.014(8) 0.000(8) -0.018(8) C91 0.032(9) 0.037(8) 0.044(11) -0.006(7) -0.003(7) -0.005(7) C92 0.066(11) 0.040(7) 0.094(15) 0.006(9) -0.029(9) -0.031(9) C93 0.090(14) 0.058(9) 0.093(16) -0.005(9) -0.022(10) -0.049(10) C94 0.070(12) 0.085(11) 0.074(14) -0.006(9) -0.024(9) -0.049(10) C95 0.053(11) 0.057(9) 0.073(14) -0.010(10) -0.028(9) 0.008(9) C96 0.052(11) 0.037(8) 0.070(14) -0.011(8) -0.017(8) -0.005(8) C97 0.017(8) 0.045(8) 0.046(12) 0.012(8) -0.014(7) 0.004(6) C98 0.066(10) 0.064(9) 0.031(12) -0.015(9) 0.009(8) -0.033(8) C99 0.081(11) 0.076(10) 0.037(12) -0.014(9) -0.004(9) -0.048(8) C100 0.078(12) 0.055(9) 0.069(15) 0.012(9) -0.017(9) -0.039(8) C101 0.054(10) 0.043(7) 0.086(15) -0.004(9) -0.015(9) -0.016(8) C102 0.031(8) 0.049(8) 0.069(13) -0.006(9) -0.010(8) -0.018(7) C103 0.020(7) 0.036(9) 0.059(10) -0.019(9) 0.003(7) -0.001(7) C104 0.040(9) 0.061(11) 0.068(12) -0.015(11) 0.005(6) -0.016(9) C105 0.068(9) 0.075(12) 0.059(11) -0.025(11) 0.006(8) -0.023(11) C106 0.062(9) 0.051(11) 0.068(11) -0.017(11) 0.030(9) -0.026(9) C107 0.038(9) 0.046(10) 0.089(13) -0.041(11) 0.025(7) -0.010(8) C108 0.032(7) 0.037(9) 0.067(11) -0.023(9) 0.002(7) -0.003(8) C109 0.048(10) 0.030(9) 0.030(10) 0.009(7) -0.018(8) -0.015(7) C110 0.058(11) 0.046(10) 0.058(10) -0.018(8) -0.002(9) -0.023(8) C111 0.080(12) 0.047(11) 0.066(12) -0.016(9) -0.007(9) -0.034(8) C112 0.066(12) 0.043(11) 0.085(13) -0.018(9) -0.001(10) -0.030(8) C113 0.065(11) 0.036(10) 0.075(12) -0.010(9) -0.003(10) -0.028(8) C114 0.055(10) 0.053(11) 0.053(11) -0.003(8) -0.010(8) -0.032(8) C115 0.044(8) 0.042(7) 0.020(10) 0.003(8) -0.002(7) -0.019(6) C116 0.047(8) 0.039(8) 0.058(13) 0.003(9) -0.010(9) -0.019(7) C117 0.046(9) 0.048(9) 0.068(13) -0.005(9) -0.014(9) -0.011(6) C118 0.038(9) 0.063(8) 0.048(12) 0.004(10) -0.014(9) -0.014(7) C119 0.041(8) 0.056(8) 0.060(13) 0.007(10) -0.007(9) -0.018(8) C120 0.053(9) 0.043(8) 0.046(12) -0.010(8) -0.015(9) -0.021(6) C121 0.045(8) 0.032(9) 0.031(11) -0.003(7) 0.000(7) -0.001(8) C122 0.058(8) 0.044(11) 0.059(13) -0.013(8) 0.006(8) -0.023(9) C123 0.045(9) 0.105(15) 0.057(15) -0.026(10) 0.012(8) -0.015(10) C124 0.063(9) 0.102(15) 0.077(15) -0.055(11) 0.010(10) -0.005(11) C125 0.073(10) 0.118(16) 0.077(15) -0.062(11) -0.002(11) -0.021(12) C126 0.043(9) 0.057(11) 0.054(13) -0.015(9) -0.001(8) -0.010(8) C127 0.119(14) 0.053(10) 0.043(11) -0.013(8) -0.003(9) -0.069(9) C128 0.143(15) 0.086(13) 0.048(12) -0.006(10) -0.026(11) -0.049(10) C129 0.164(17) 0.066(12) 0.074(15) 0.012(9) -0.035(11) -0.075(11) C130 0.22(2) 0.087(14) 0.044(12) 0.006(11) -0.037(11) -0.078(13) C131 0.22(2) 0.095(16) 0.041(11) 0.008(10) -0.010(13) -0.070(13) C132 0.140(15) 0.085(13) 0.036(12) 0.006(9) 0.002(10) -0.070(11) C133 0.048(7) 0.053(9) 0.026(11) -0.014(7) 0.013(8) -0.039(7) C134 0.056(8) 0.065(10) 0.040(12) -0.010(8) -0.002(9) -0.038(8) C135 0.043(8) 0.067(12) 0.071(14) -0.008(9) -0.009(9) -0.024(7) C136 0.059(8) 0.056(11) 0.049(13) -0.010(8) 0.002(9) -0.020(8) C137 0.067(9) 0.050(10) 0.072(14) -0.025(9) 0.008(10) -0.039(8) C138 0.061(9) 0.056(10) 0.034(11) -0.022(8) 0.005(8) -0.035(7) C139 0.052(8) 0.030(8) 0.039(9) -0.028(6) -0.001(6) -0.016(7) C140 0.060(10) 0.048(10) 0.060(10) -0.019(8) 0.010(8) -0.033(8) C141 0.074(12) 0.083(13) 0.073(12) -0.031(9) 0.012(8) -0.058(10) C142 0.060(10) 0.102(15) 0.083(14) -0.048(11) 0.021(9) -0.041(11) C143 0.034(9) 0.091(14) 0.097(13) -0.033(10) 0.009(9) -0.015(9) C144 0.052(10) 0.072(12) 0.066(11) -0.033(9) 0.002(7) -0.027(9) C145 0.100(12) 0.047(13) 0.119(17) -0.011(12) 0.006(10) -0.056(10) C146 0.082(12) 0.101(18) 0.135(18) -0.016(14) -0.018(12) -0.074(12) C147 0.141(19) 0.074(18) 0.104(18) 0.000(13) -0.006(12) -0.052(15) C148 0.110(15) 0.080(18) 0.14(2) -0.007(17) 0.011(14) -0.034(13) C149 0.133(16) 0.053(16) 0.14(2) 0.027(15) -0.045(16) -0.001(13) C150 0.178(19) 0.056(16) 0.110(19) 0.001(14) -0.061(16) -0.003(15) C151 0.166(19) 0.10(2) 0.21(3) -0.03(2) 0.09(2) -0.061(16) C152 0.18(3) 0.14(2) 0.25(4) -0.01(2) 0.105(19) -0.11(2) C153 0.17(3) 0.078(17) 0.23(4) -0.044(17) 0.06(2) -0.047(17) C154 0.08(2) 0.066(17) 0.41(5) -0.06(2) 0.03(2) 0.006(14) C155 0.14(3) 0.12(2) 0.27(4) -0.09(3) 0.08(2) -0.04(2) C156 0.14(3) 0.12(2) 0.29(4) -0.02(2) 0.095(19) -0.05(2) C157 0.25(4) 0.10(2) 0.18(3) -0.037(16) 0.13(2) -0.09(2) C158 0.36(4) 0.26(4) 0.16(3) -0.15(3) 0.16(3) -0.23(3) C159 0.090(12) 0.073(19) 0.24(3) -0.05(2) 0.099(19) -0.045(14) C160 0.120(16) 0.046(16) 0.27(3) -0.01(2) 0.057(18) -0.053(15) C161 0.069(12) 0.071(18) 0.29(4) 0.00(2) 0.032(18) -0.022(13) C162 0.19(5) 0.09(4) 0.33(5) -0.09(6) 0.01(3) -0.03(4) C163 0.16(2) 0.14(2) 0.11(2) -0.07(2) -0.01(2) -0.057(16) C164 0.15(2) 0.14(2) 0.10(2) -0.065(17) -0.019(16) -0.063(15) C165 0.15(3) 0.15(3) 0.10(4) -0.02(3) -0.02(3) -0.07(2) C166 0.14(3) 0.14(2) 0.12(3) -0.070(19) -0.02(2) -0.056(19) C167 0.16(2) 0.13(2) 0.11(2) -0.074(19) -0.03(2) -0.059(17) C168 0.15(2) 0.13(2) 0.12(3) -0.08(2) -0.02(2) -0.059(17) _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 Si1 2.579(5) . ? In1 In3 2.855(2) . ? In1 In2 2.9323(18) . ? In1 In4 2.9807(17) . ? In1 In5 2.9917(17) . ? In2 Si2 2.597(5) . ? In2 In6 2.9129(18) . ? In2 In7 2.963(2) . ? In2 In5 3.1071(18) . ? In2 In3 3.2626(18) . ? In3 Si3 2.625(5) . ? In3 In7 2.9080(18) . ? In3 In4 3.0031(19) . ? In3 In8 3.2624(17) . ? In4 Si4 2.579(5) . ? In4 In5 2.8858(18) . ? In4 In8 2.9227(19) . ? In5 Si5 2.628(5) . ? In5 In6 2.9554(19) . ? In5 In8 3.2821(19) . ? In6 Si6 2.593(4) . ? In6 In8 2.9401(18) . ? In6 In7 2.9728(18) . ? In7 Si7 2.568(5) . ? In7 In8 2.9117(18) . ? In8 Si8 2.615(5) . ? Si1 C13 1.850(15) . ? Si1 C7 1.863(17) . ? Si1 C1 1.910(16) . ? Si2 C25 1.837(16) . ? Si2 C19 1.848(17) . ? Si2 C31 1.903(15) . ? Si3 C49 1.842(16) . ? Si3 C37 1.853(16) . ? Si3 C43 1.879(17) . ? Si4 C67 1.856(17) . ? Si4 C55 1.869(16) . ? Si4 C61 1.920(15) . ? Si5 C79 1.815(16) . ? Si5 C85 1.864(14) . ? Si5 C73 1.866(17) . ? Si6 C91 1.857(16) . ? Si6 C97 1.863(17) . ? Si6 C103 1.870(17) . ? Si7 C109 1.855(16) . ? Si7 C115 1.887(15) . ? Si7 C121 1.905(16) . ? Si8 C139 1.854(17) . ? Si8 C127 1.870(19) . ? Si8 C133 1.881(16) . ? C1 C6 1.36(2) . ? C1 C2 1.40(2) . ? C2 C3 1.391(19) . ? C3 C4 1.34(2) . ? C4 C5 1.41(2) . ? C5 C6 1.33(2) . ? C7 C8 1.35(2) . ? C7 C12 1.401(19) . ? C8 C9 1.35(2) . ? C9 C10 1.41(2) . ? C10 C11 1.29(2) . ? C11 C12 1.41(2) . ? C13 C14 1.36(2) . ? C13 C18 1.39(2) . ? C14 C15 1.42(2) . ? C15 C16 1.36(2) . ? C16 C17 1.35(2) . ? C17 C18 1.44(2) . ? C19 C24 1.38(2) . ? C19 C20 1.42(2) . ? C20 C21 1.39(2) . ? C21 C22 1.40(2) . ? C22 C23 1.31(2) . ? C23 C24 1.37(2) . ? C25 C30 1.348(19) . ? C25 C26 1.41(2) . ? C26 C27 1.38(2) . ? C27 C28 1.36(2) . ? C28 C29 1.38(2) . ? C29 C30 1.34(2) . ? C31 C36 1.37(2) . ? C31 C32 1.39(2) . ? C32 C33 1.37(2) . ? C33 C34 1.31(2) . ? C34 C35 1.36(2) . ? C35 C36 1.38(2) . ? C37 C38 1.404(19) . ? C37 C42 1.45(2) . ? C38 C39 1.33(2) . ? C39 C40 1.34(2) . ? C40 C41 1.38(2) . ? C41 C42 1.39(2) . ? C43 C48 1.37(2) . ? C43 C44 1.419(19) . ? C44 C45 1.36(2) . ? C45 C46 1.35(2) . ? C46 C47 1.42(2) . ? C47 C48 1.35(2) . ? C49 C50 1.36(2) . ? C49 C54 1.38(2) . ? C50 C51 1.38(2) . ? C51 C52 1.43(2) . ? C52 C53 1.36(2) . ? C53 C54 1.46(2) . ? C55 C56 1.36(2) . ? C55 C60 1.406(18) . ? C56 C57 1.36(2) . ? C57 C58 1.39(2) . ? C58 C59 1.37(2) . ? C59 C60 1.37(2) . ? C61 C62 1.33(2) . ? C61 C66 1.40(2) . ? C62 C63 1.38(2) . ? C63 C64 1.36(2) . ? C64 C65 1.35(3) . ? C65 C66 1.35(2) . ? C67 C68 1.38(2) . ? C67 C72 1.410(19) . ? C68 C69 1.37(2) . ? C69 C70 1.41(2) . ? C70 C71 1.37(2) . ? C71 C72 1.34(2) . ? C73 C74 1.34(2) . ? C73 C78 1.50(2) . ? C74 C75 1.39(2) . ? C75 C76 1.38(2) . ? C76 C77 1.39(3) . ? C77 C78 1.34(2) . ? C79 C80 1.40(2) . ? C79 C84 1.453(19) . ? C80 C81 1.40(2) . ? C81 C82 1.38(2) . ? C82 C83 1.35(2) . ? C83 C84 1.38(2) . ? C85 C86 1.38(2) . ? C85 C90 1.40(2) . ? C86 C87 1.37(2) . ? C87 C88 1.41(2) . ? C88 C89 1.33(2) . ? C89 C90 1.44(2) . ? C91 C96 1.38(2) . ? C91 C92 1.44(2) . ? C92 C93 1.39(2) . ? C93 C94 1.35(2) . ? C94 C95 1.32(2) . ? C95 C96 1.41(2) . ? C97 C98 1.33(2) . ? C97 C102 1.43(2) . ? C98 C99 1.40(2) . ? C99 C100 1.40(2) . ? C100 C101 1.33(2) . ? C101 C102 1.38(2) . ? C103 C108 1.391(19) . ? C103 C104 1.39(2) . ? C104 C105 1.39(2) . ? C105 C106 1.38(2) . ? C106 C107 1.33(2) . ? C107 C108 1.36(2) . ? C109 C110 1.39(2) . ? C109 C114 1.40(2) . ? C110 C111 1.36(2) . ? C111 C112 1.38(2) . ? C112 C113 1.35(2) . ? C113 C114 1.37(2) . ? C115 C120 1.40(2) . ? C115 C116 1.407(19) . ? C116 C117 1.324(19) . ? C117 C118 1.43(2) . ? C118 C119 1.35(2) . ? C119 C120 1.363(19) . ? C121 C126 1.37(2) . ? C121 C122 1.40(2) . ? C122 C123 1.38(2) . ? C123 C124 1.37(2) . ? C124 C125 1.32(2) . ? C125 C126 1.35(2) . ? C127 C132 1.37(2) . ? C127 C128 1.40(2) . ? C128 C129 1.42(3) . ? C129 C130 1.40(3) . ? C130 C131 1.26(3) . ? C131 C132 1.37(3) . ? C133 C134 1.370(19) . ? C133 C138 1.422(19) . ? C134 C135 1.41(2) . ? C135 C136 1.31(2) . ? C136 C137 1.43(2) . ? C137 C138 1.36(2) . ? C139 C140 1.37(2) . ? C139 C144 1.41(2) . ? C140 C141 1.37(2) . ? C141 C142 1.40(2) . ? C142 C143 1.37(3) . ? C143 C144 1.34(2) . ? C145 C150 1.36(3) . ? C145 C146 1.41(3) . ? C145 C151 1.50(3) . ? C146 C147 1.42(3) . ? C147 C148 1.31(3) . ? C148 C149 1.37(3) . ? C149 C150 1.34(3) . ? C152 C153 1.16(3) . ? C152 C157 1.37(4) . ? C152 C158 1.44(4) . ? C153 C154 1.50(4) . ? C154 C155 1.42(4) . ? C155 C156 1.27(4) . ? C156 C157 1.38(4) . ? C159 C160 1.32(3) . ? C159 C161 1.38(4) 2_856 ? C160 C161 1.23(3) . ? C160 C162 1.520(2) . ? C161 C159 1.38(4) 2_856 ? C163 C167 0.92(8) . ? C163 C168 0.93(7) . ? C163 C164 1.360(2) . ? C163 C166 1.520(2) . ? C164 C167 1.21(6) . ? C164 C165 1.360(2) . ? C166 C168 1.01(8) . ? C166 C167 1.49(8) . ? C167 C168 1.52(6) . ? 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 Si1 In1 In3 133.10(12) . . ? Si1 In1 In2 133.97(11) . . ? In3 In1 In2 68.61(5) . . ? Si1 In1 In4 126.20(11) . . ? In3 In1 In4 61.89(4) . . ? In2 In1 In4 99.67(5) . . ? Si1 In1 In5 135.99(12) . . ? In3 In1 In5 89.53(5) . . ? In2 In1 In5 63.26(4) . . ? In4 In1 In5 57.79(4) . . ? Si2 In2 In6 123.96(11) . . ? Si2 In2 In1 109.62(11) . . ? In6 In2 In1 114.34(5) . . ? Si2 In2 In7 132.00(13) . . ? In6 In2 In7 60.78(5) . . ? In1 In2 In7 108.42(5) . . ? Si2 In2 In5 127.77(13) . . ? In6 In2 In5 58.70(4) . . ? In1 In2 In5 59.30(4) . . ? In7 In2 In5 96.68(5) . . ? Si2 In2 In3 138.47(11) . . ? In6 In2 In3 95.95(5) . . ? In1 In2 In3 54.58(4) . . ? In7 In2 In3 55.44(4) . . ? In5 In2 In3 80.53(4) . . ? Si3 In3 In1 121.02(12) . . ? Si3 In3 In7 107.63(11) . . ? In1 In3 In7 112.13(5) . . ? Si3 In3 In4 138.17(11) . . ? In1 In3 In4 61.10(4) . . ? In7 In3 In4 108.71(5) . . ? Si3 In3 In8 141.62(12) . . ? In1 In3 In8 97.09(5) . . ? In7 In3 In8 55.96(4) . . ? In4 In3 In8 55.43(4) . . ? Si3 In3 In2 125.15(11) . . ? In1 In3 In2 56.81(4) . . ? In7 In3 In2 57.04(4) . . ? In4 In3 In2 92.21(5) . . ? In8 In3 In2 78.01(4) . . ? Si4 In4 In5 135.83(13) . . ? Si4 In4 In8 136.47(12) . . ? In5 In4 In8 68.81(5) . . ? Si4 In4 In1 120.99(12) . . ? In5 In4 In1 61.30(4) . . ? In8 In4 In1 102.15(5) . . ? Si4 In4 In3 131.67(12) . . ? In5 In4 In3 88.74(5) . . ? In8 In4 In3 66.79(4) . . ? In1 In4 In3 57.00(4) . . ? Si5 In5 In4 122.52(11) . . ? Si5 In5 In6 108.25(11) . . ? In4 In5 In6 110.40(6) . . ? Si5 In5 In1 134.78(12) . . ? In4 In5 In1 60.91(4) . . ? In6 In5 In1 111.35(5) . . ? Si5 In5 In2 139.07(11) . . ? In4 In5 In2 97.81(5) . . ? In6 In5 In2 57.37(4) . . ? In1 In5 In2 57.44(4) . . ? Si5 In5 In8 126.57(12) . . ? In4 In5 In8 56.13(4) . . ? In6 In5 In8 55.95(4) . . ? In1 In5 In8 94.01(5) . . ? In2 In5 In8 79.95(5) . . ? Si6 In6 In2 134.59(12) . . ? Si6 In6 In8 134.50(13) . . ? In2 In6 In8 89.12(5) . . ? Si6 In6 In5 135.21(12) . . ? In2 In6 In5 63.93(4) . . ? In8 In6 In5 67.66(5) . . ? Si6 In6 In7 124.93(12) . . ? In2 In6 In7 60.44(4) . . ? In8 In6 In7 59.00(4) . . ? In5 In6 In7 99.83(5) . . ? Si7 In7 In3 131.01(11) . . ? Si7 In7 In8 127.06(12) . . ? In3 In7 In8 68.19(4) . . ? Si7 In7 In2 142.58(12) . . ? In3 In7 In2 67.51(5) . . ? In8 In7 In2 88.70(5) . . ? Si7 In7 In6 125.60(11) . . ? In3 In7 In6 102.72(5) . . ? In8 In7 In6 59.94(4) . . ? In2 In7 In6 58.78(4) . . ? Si8 In8 In7 131.27(13) . . ? Si8 In8 In4 104.06(12) . . ? In7 In8 In4 110.85(5) . . ? Si8 In8 In6 134.44(11) . . ? In7 In8 In6 61.06(4) . . ? In4 In8 In6 109.80(6) . . ? Si8 In8 In3 128.73(12) . . ? In7 In8 In3 55.85(4) . . ? In4 In8 In3 57.78(4) . . ? In6 In8 In3 95.42(5) . . ? Si8 In8 In5 134.33(13) . . ? In7 In8 In5 93.97(5) . . ? In4 In8 In5 55.06(4) . . ? In6 In8 In5 56.39(4) . . ? In3 In8 In5 78.00(4) . . ? C13 Si1 C7 108.7(8) . . ? C13 Si1 C1 107.7(7) . . ? C7 Si1 C1 106.6(7) . . ? C13 Si1 In1 110.2(5) . . ? C7 Si1 In1 110.8(5) . . ? C1 Si1 In1 112.7(5) . . ? C25 Si2 C19 109.1(8) . . ? C25 Si2 C31 106.8(7) . . ? C19 Si2 C31 105.6(7) . . ? C25 Si2 In2 107.1(5) . . ? C19 Si2 In2 117.5(5) . . ? C31 Si2 In2 110.2(5) . . ? C49 Si3 C37 106.8(7) . . ? C49 Si3 C43 106.8(8) . . ? C37 Si3 C43 108.3(7) . . ? C49 Si3 In3 116.5(5) . . ? C37 Si3 In3 109.7(5) . . ? C43 Si3 In3 108.5(5) . . ? C67 Si4 C55 111.4(7) . . ? C67 Si4 C61 108.7(7) . . ? C55 Si4 C61 107.6(7) . . ? C67 Si4 In4 108.7(5) . . ? C55 Si4 In4 107.3(5) . . ? C61 Si4 In4 113.2(4) . . ? C79 Si5 C85 109.0(7) . . ? C79 Si5 C73 111.5(7) . . ? C85 Si5 C73 106.4(8) . . ? C79 Si5 In5 109.0(6) . . ? C85 Si5 In5 108.4(4) . . ? C73 Si5 In5 112.4(6) . . ? C91 Si6 C97 105.4(8) . . ? C91 Si6 C103 110.9(7) . . ? C97 Si6 C103 106.3(7) . . ? C91 Si6 In6 109.7(5) . . ? C97 Si6 In6 114.5(5) . . ? C103 Si6 In6 109.9(5) . . ? C109 Si7 C115 107.3(7) . . ? C109 Si7 C121 110.9(8) . . ? C115 Si7 C121 110.7(7) . . ? C109 Si7 In7 111.0(5) . . ? C115 Si7 In7 106.8(5) . . ? C121 Si7 In7 110.0(5) . . ? C139 Si8 C127 109.5(8) . . ? C139 Si8 C133 108.2(7) . . ? C127 Si8 C133 103.5(8) . . ? C139 Si8 In8 110.3(5) . . ? C127 Si8 In8 112.0(5) . . ? C133 Si8 In8 113.1(5) . . ? C6 C1 C2 116.9(15) . . ? C6 C1 Si1 124.8(13) . . ? C2 C1 Si1 118.3(12) . . ? C3 C2 C1 117.9(16) . . ? C4 C3 C2 124.2(17) . . ? C3 C4 C5 116.4(16) . . ? C6 C5 C4 119.8(17) . . ? C5 C6 C1 124.5(18) . . ? C8 C7 C12 114.9(16) . . ? C8 C7 Si1 124.6(13) . . ? C12 C7 Si1 120.5(12) . . ? C7 C8 C9 124.3(17) . . ? C8 C9 C10 121.7(16) . . ? C11 C10 C9 114.1(18) . . ? C10 C11 C12 126.5(18) . . ? C7 C12 C11 118.5(15) . . ? C14 C13 C18 117.5(16) . . ? C14 C13 Si1 123.7(15) . . ? C18 C13 Si1 118.6(13) . . ? C13 C14 C15 120.8(18) . . ? C16 C15 C14 119.2(19) . . ? C17 C16 C15 123.7(19) . . ? C16 C17 C18 115.5(19) . . ? C13 C18 C17 123.1(18) . . ? C24 C19 C20 114.8(18) . . ? C24 C19 Si2 124.2(14) . . ? C20 C19 Si2 120.8(14) . . ? C21 C20 C19 118.4(18) . . ? C20 C21 C22 120(2) . . ? C23 C22 C21 123(2) . . ? C22 C23 C24 115.6(19) . . ? C23 C24 C19 127(2) . . ? C30 C25 C26 112.0(15) . . ? C30 C25 Si2 127.1(12) . . ? C26 C25 Si2 120.6(12) . . ? C27 C26 C25 122.6(16) . . ? C28 C27 C26 122.0(16) . . ? C27 C28 C29 115.3(17) . . ? C30 C29 C28 121.3(16) . . ? C29 C30 C25 126.5(16) . . ? C36 C31 C32 115.7(16) . . ? C36 C31 Si2 123.3(13) . . ? C32 C31 Si2 120.9(13) . . ? C33 C32 C31 120.2(18) . . ? C34 C33 C32 122(2) . . ? C33 C34 C35 121.6(19) . . ? C34 C35 C36 116.9(18) . . ? C31 C36 C35 123.9(17) . . ? C38 C37 C42 112.4(14) . . ? C38 C37 Si3 125.0(12) . . ? C42 C37 Si3 122.1(11) . . ? C39 C38 C37 124.3(16) . . ? C38 C39 C40 121.8(17) . . ? C39 C40 C41 119.2(16) . . ? C40 C41 C42 119.4(16) . . ? C41 C42 C37 122.2(14) . . ? C48 C43 C44 116.3(16) . . ? C48 C43 Si3 123.1(12) . . ? C44 C43 Si3 120.2(13) . . ? C45 C44 C43 119.6(17) . . ? C46 C45 C44 123.6(19) . . ? C45 C46 C47 117.6(19) . . ? C48 C47 C46 118.8(19) . . ? C47 C48 C43 124.0(17) . . ? C50 C49 C54 115.7(16) . . ? C50 C49 Si3 122.1(13) . . ? C54 C49 Si3 121.9(13) . . ? C49 C50 C51 127.3(18) . . ? C50 C51 C52 115.5(18) . . ? C53 C52 C51 121.9(19) . . ? C52 C53 C54 117.2(18) . . ? C49 C54 C53 122.3(17) . . ? C56 C55 C60 115.6(16) . . ? C56 C55 Si4 123.2(12) . . ? C60 C55 Si4 121.0(12) . . ? C57 C56 C55 123.8(17) . . ? C56 C57 C58 120.1(18) . . ? C59 C58 C57 117.5(18) . . ? C60 C59 C58 121.9(17) . . ? C59 C60 C55 121.0(17) . . ? C62 C61 C66 117.9(16) . . ? C62 C61 Si4 121.5(14) . . ? C66 C61 Si4 120.6(13) . . ? C61 C62 C63 122.9(18) . . ? C64 C63 C62 118(2) . . ? C65 C64 C63 120.8(19) . . ? C64 C65 C66 121(2) . . ? C65 C66 C61 119.7(19) . . ? C68 C67 C72 114.5(15) . . ? C68 C67 Si4 122.1(12) . . ? C72 C67 Si4 123.4(12) . . ? C69 C68 C67 124.8(16) . . ? C68 C69 C70 117.1(17) . . ? C71 C70 C69 120.1(17) . . ? C72 C71 C70 119.9(18) . . ? C71 C72 C67 123.3(17) . . ? C74 C73 C78 116.9(17) . . ? C74 C73 Si5 121.0(15) . . ? C78 C73 Si5 122.0(14) . . ? C73 C74 C75 124.1(19) . . ? C76 C75 C74 119(2) . . ? C75 C76 C77 118(2) . . ? C78 C77 C76 125(2) . . ? C77 C78 C73 117(2) . . ? C80 C79 C84 111.9(15) . . ? C80 C79 Si5 125.6(12) . . ? C84 C79 Si5 122.5(13) . . ? C81 C80 C79 126.2(16) . . ? C82 C81 C80 115.5(17) . . ? C83 C82 C81 123.0(16) . . ? C82 C83 C84 119.4(16) . . ? C83 C84 C79 123.0(17) . . ? C86 C85 C90 116.3(15) . . ? C86 C85 Si5 122.5(13) . . ? C90 C85 Si5 120.9(12) . . ? C87 C86 C85 123.1(17) . . ? C86 C87 C88 120.0(19) . . ? C89 C88 C87 119.0(18) . . ? C88 C89 C90 120.8(18) . . ? C85 C90 C89 120.5(16) . . ? C96 C91 C92 114.3(16) . . ? C96 C91 Si6 123.8(13) . . ? C92 C91 Si6 121.9(12) . . ? C93 C92 C91 119.3(16) . . ? C94 C93 C92 122.6(18) . . ? C95 C94 C93 120.0(19) . . ? C94 C95 C96 119.4(17) . . ? C91 C96 C95 124.0(17) . . ? C98 C97 C102 115.6(16) . . ? C98 C97 Si6 125.2(13) . . ? C102 C97 Si6 119.2(13) . . ? C97 C98 C99 124.8(18) . . ? C98 C99 C100 117.4(19) . . ? C101 C100 C99 119.7(19) . . ? C100 C101 C102 121.3(18) . . ? C101 C102 C97 120.7(18) . . ? C108 C103 C104 115.0(16) . . ? C108 C103 Si6 124.4(13) . . ? C104 C103 Si6 120.1(12) . . ? C105 C104 C103 121.8(17) . . ? C106 C105 C104 119.6(19) . . ? C107 C106 C105 118.7(18) . . ? C106 C107 C108 122.2(18) . . ? C107 C108 C103 122.5(17) . . ? C110 C109 C114 113.3(16) . . ? C110 C109 Si7 123.7(14) . . ? C114 C109 Si7 122.3(13) . . ? C111 C110 C109 124.5(19) . . ? C110 C111 C112 119.0(19) . . ? C113 C112 C111 119.6(18) . . ? C112 C113 C114 120.1(19) . . ? C113 C114 C109 123.3(18) . . ? C120 C115 C116 115.4(14) . . ? C120 C115 Si7 120.9(12) . . ? C116 C115 Si7 123.7(12) . . ? C117 C116 C115 124.0(17) . . ? C116 C117 C118 118.4(17) . . ? C119 C118 C117 119.3(16) . . ? C118 C119 C120 120.9(17) . . ? C119 C120 C115 121.8(16) . . ? C126 C121 C122 117.6(16) . . ? C126 C121 Si7 123.2(13) . . ? C122 C121 Si7 119.2(13) . . ? C123 C122 C121 119.4(17) . . ? C124 C123 C122 118.6(18) . . ? C125 C124 C123 122.3(19) . . ? C124 C125 C126 118.9(19) . . ? C125 C126 C121 122.4(18) . . ? C132 C127 C128 115(2) . . ? C132 C127 Si8 122.8(16) . . ? C128 C127 Si8 122.0(16) . . ? C127 C128 C129 123(2) . . ? C130 C129 C128 116(2) . . ? C131 C130 C129 120(3) . . ? C130 C131 C132 125(3) . . ? C131 C132 C127 121(2) . . ? C134 C133 C138 115.7(15) . . ? C134 C133 Si8 125.6(12) . . ? C138 C133 Si8 118.2(12) . . ? C133 C134 C135 121.2(16) . . ? C136 C135 C134 121.6(17) . . ? C135 C136 C137 120.1(17) . . ? C138 C137 C136 117.8(16) . . ? C137 C138 C133 123.4(16) . . ? C140 C139 C144 115.3(17) . . ? C140 C139 Si8 120.4(12) . . ? C144 C139 Si8 124.3(15) . . ? C139 C140 C141 120.8(18) . . ? C140 C141 C142 123(2) . . ? C143 C142 C141 115(2) . . ? C144 C143 C142 122(2) . . ? C143 C144 C139 124(2) . . ? C150 C145 C146 120(2) . . ? C150 C145 C151 120(3) . . ? C146 C145 C151 119(2) . . ? C145 C146 C147 120(2) . . ? C148 C147 C146 116(3) . . ? C147 C148 C149 123(3) . . ? C150 C149 C148 123(3) . . ? C149 C150 C145 117(3) . . ? C153 C152 C157 133(5) . . ? C153 C152 C158 130(5) . . ? C157 C152 C158 97(2) . . ? C152 C153 C154 126(4) . . ? C155 C154 C153 107(3) . . ? C156 C155 C154 114(4) . . ? C155 C156 C157 141(4) . . ? C152 C157 C156 98(3) . . ? C160 C159 C161 115(2) . 2_856 ? C161 C160 C159 121(4) . . ? C161 C160 C162 108(4) . . ? C159 C160 C162 131(4) . . ? C160 C161 C159 124(3) . 2_856 ? C167 C163 C168 111(8) . . ? C167 C163 C164 61(4) . . ? C168 C163 C164 169(9) . . ? C167 C163 C166 70(6) . . ? C168 C163 C166 40(5) . . ? C164 C163 C166 130(6) . . ? C167 C164 C165 126(5) . . ? C167 C164 C163 42(4) . . ? C165 C164 C163 168(5) . . ? C168 C166 C167 72(5) . . ? C168 C166 C163 37(4) . . ? C167 C166 C163 36(4) . . ? C163 C167 C164 78(5) . . ? C163 C167 C166 74(4) . . ? C164 C167 C166 150(6) . . ? C163 C167 C168 35(4) . . ? C164 C167 C168 112(6) . . ? C166 C167 C168 39(3) . . ? C163 C168 C166 103(7) . . ? C163 C168 C167 35(5) . . ? C166 C168 C167 68(5) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 22.34 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.035 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.105 # Attachment 'Comp_7_728995.cif' data_m39abso_Comp_7_CCDC_ _database_code_depnum_ccdc_archive 'CCDC 728995' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C132 H138 O6 Si6 In3 Na _ (OC4H8)4_C6H6' _chemical_formula_sum 'C154 H176 In3 Na O10 Si6' _chemical_formula_weight 2722.94 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.708(3) _cell_length_b 14.115(3) _cell_length_c 19.749(4) _cell_angle_alpha 72.28(3) _cell_angle_beta 79.83(3) _cell_angle_gamma 81.56(3) _cell_volume 3565(1) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 23.9 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1422 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7997 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'image plate, 2 circle goniometer' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22330 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.1232 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.90 _reflns_number_total 10322 _reflns_number_gt 6225 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement STOE _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXTL 5.01' _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. Disordered thf molecules are refined with split positions (50:50). Several ADP of thf molecules are still high, indicating further disorder, which is not reasonable to resolve. SIMU and DFIX were used on solvent molecules ; _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^)+(0.0694P)^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 10322 _refine_ls_number_parameters 832 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.5000 0.0000 0.5000 0.0345(2) Uani 1 2 d S . . In2 In 0.52295(3) -0.04891(3) 0.64653(2) 0.03067(15) Uani 1 1 d . . . Si4 Si 0.71081(14) -0.02585(13) 0.64603(11) 0.0369(5) Uani 1 1 d . . . Si5 Si 0.48106(14) -0.23603(12) 0.69778(10) 0.0339(4) Uani 1 1 d . . . Si6 Si 0.39571(14) 0.07483(13) 0.70314(10) 0.0350(5) Uani 1 1 d . . . C1 C 0.5232(7) 0.3472(6) 0.6221(6) 0.082(3) Uani 1 1 d . . . H1A H 0.5878 0.3678 0.6031 0.099 Uiso 1 1 calc R . . C2 C 0.8702(6) -0.2671(6) 0.5816(5) 0.060(2) Uani 1 1 d . . . H2A H 0.8564 -0.3304 0.5801 0.072 Uiso 1 1 calc R . . C4 C 0.4016(7) 0.0686(7) 0.9161(5) 0.076(3) Uani 1 1 d . . . H4A H 0.4080 0.1144 0.9413 0.092 Uiso 1 1 calc R . . C5 C 0.7695(7) 0.3042(6) 0.5133(5) 0.065(2) Uani 1 1 d . . . H5A H 0.7792 0.3712 0.4863 0.078 Uiso 1 1 calc R . . C6 C 0.4452(7) 0.4167(6) 0.6285(5) 0.064(2) Uani 1 1 d . . . H6A H 0.4550 0.4856 0.6143 0.077 Uiso 1 1 calc R . . C7 C 0.6792(7) -0.4331(6) 0.5622(6) 0.078(3) Uani 1 1 d . . . H7A H 0.7205 -0.4712 0.5340 0.094 Uiso 1 1 calc R . . C8 C 0.6650(6) -0.0169(7) 0.7906(5) 0.071(3) Uani 1 1 d . . . H8A H 0.6021 0.0119 0.7762 0.085 Uiso 1 1 calc R . . C9 C 0.5853(6) -0.2594(6) 0.8162(5) 0.066(2) Uani 1 1 d . . . H9A H 0.6259 -0.2127 0.7821 0.079 Uiso 1 1 calc R . . C10 C 0.5093(6) 0.2468(6) 0.6429(5) 0.069(3) Uani 1 1 d . . . H10A H 0.5653 0.1999 0.6376 0.083 Uiso 1 1 calc R . . C11 C 0.8292(6) -0.0819(6) 0.7643(5) 0.064(2) Uani 1 1 d . . . H11A H 0.8829 -0.1013 0.7321 0.077 Uiso 1 1 calc R . . C12 C 0.3534(7) 0.3869(5) 0.6553(5) 0.064(2) Uani 1 1 d . . . H12A H 0.2981 0.4348 0.6598 0.077 Uiso 1 1 calc R . . C13 C 0.7192(6) 0.1450(5) 0.5224(4) 0.0501(19) Uani 1 1 d . . . H13A H 0.6962 0.1031 0.5002 0.060 Uiso 1 1 calc R . . C14 C 0.1738(6) -0.2014(6) 0.6873(5) 0.059(2) Uani 1 1 d . . . H14A H 0.1231 -0.1471 0.6798 0.070 Uiso 1 1 calc R . . C15 C 0.9657(6) -0.2389(6) 0.5590(4) 0.057(2) Uani 1 1 d . . . H15A H 1.0178 -0.2834 0.5438 0.069 Uiso 1 1 calc R . . C16 C 0.2253(6) -0.3737(5) 0.7087(4) 0.0490(19) Uani 1 1 d . . . H16A H 0.2099 -0.4400 0.7168 0.059 Uiso 1 1 calc R . . C17 C 0.7915(6) 0.2683(6) 0.5818(5) 0.061(2) Uani 1 1 d . . . H17A H 0.8164 0.3108 0.6024 0.073 Uiso 1 1 calc R . . C18 C 0.4002(6) 0.1027(6) 0.8424(4) 0.055(2) Uani 1 1 d . . . H18A H 0.4055 0.1713 0.8177 0.066 Uiso 1 1 calc R . . C19 C 0.9072(5) -0.0825(5) 0.5830(4) 0.0487(19) Uani 1 1 d . . . H19A H 0.9207 -0.0182 0.5825 0.058 Uiso 1 1 calc R . . C20 C 0.2436(6) 0.0977(5) 0.6153(4) 0.054(2) Uani 1 1 d . . . H20A H 0.2956 0.1148 0.5763 0.064 Uiso 1 1 calc R . . C21 C 0.0884(6) 0.0486(6) 0.7262(5) 0.061(2) Uani 1 1 d . . . H21A H 0.0353 0.0324 0.7644 0.073 Uiso 1 1 calc R . . C22 C 0.2703(5) -0.1832(5) 0.6874(4) 0.051(2) Uani 1 1 d . . . H22A H 0.2837 -0.1165 0.6806 0.061 Uiso 1 1 calc R . . C23 C 0.3856(6) -0.0637(5) 0.8439(4) 0.0486(19) Uani 1 1 d . . . H23A H 0.3805 -0.1110 0.8195 0.058 Uiso 1 1 calc R . . C24 C 0.1502(6) -0.2959(6) 0.6977(4) 0.054(2) Uani 1 1 d . . . H24A H 0.0839 -0.3080 0.6975 0.065 Uiso 1 1 calc R . . C25 C 0.5544(6) -0.2962(5) 0.5727(4) 0.0488(19) Uani 1 1 d . . . H25A H 0.5101 -0.2419 0.5505 0.059 Uiso 1 1 calc R . . C26 C 0.7331(6) 0.2425(6) 0.4839(5) 0.059(2) Uani 1 1 d . . . H26A H 0.7173 0.2674 0.4363 0.070 Uiso 1 1 calc R . . C27 C 0.6844(6) -0.4567(6) 0.6335(6) 0.062(2) Uani 1 1 d . . . H27A H 0.7276 -0.5122 0.6556 0.075 Uiso 1 1 calc R . . C28 C 0.3403(6) 0.2858(5) 0.6764(5) 0.058(2) Uani 1 1 d . . . H28A H 0.2753 0.2663 0.6955 0.069 Uiso 1 1 calc R . . C29 C 0.8109(5) -0.1106(5) 0.6077(4) 0.0366(16) Uani 1 1 d . . . C30 C 0.9847(5) -0.1464(6) 0.5587(4) 0.052(2) Uani 1 1 d . . . H30A H 1.0496 -0.1255 0.5423 0.063 Uiso 1 1 calc R . . C31 C 0.7953(5) -0.2052(5) 0.6061(4) 0.051(2) Uani 1 1 d . . . H31A H 0.7308 -0.2273 0.6225 0.061 Uiso 1 1 calc R . . C34 C 0.3233(5) -0.3567(5) 0.7081(4) 0.0443(18) Uani 1 1 d . . . H34A H 0.3734 -0.4116 0.7150 0.053 Uiso 1 1 calc R . . C35 C 0.7383(5) 0.1065(5) 0.5932(4) 0.0385(17) Uani 1 1 d . . . C36 C 0.4176(5) 0.2117(5) 0.6710(4) 0.0424(18) Uani 1 1 d . . . C37 C 0.7780(5) 0.1702(5) 0.6218(4) 0.050(2) Uani 1 1 d . . . H37A H 0.7957 0.1459 0.6688 0.060 Uiso 1 1 calc R . . C38 C 0.1469(7) 0.0970(6) 0.6021(6) 0.069(3) Uani 1 1 d . . . H38A H 0.1335 0.1142 0.5540 0.083 Uiso 1 1 calc R . . C39 C 0.6149(7) -0.3550(6) 0.5306(5) 0.065(2) Uani 1 1 d . . . H39A H 0.6106 -0.3399 0.4809 0.078 Uiso 1 1 calc R . . C40 C 0.2640(5) 0.0729(4) 0.6864(4) 0.0370(17) Uani 1 1 d . . . C41 C 0.5590(5) -0.3171(4) 0.6450(4) 0.0376(17) Uani 1 1 d . . . C42 C 0.1839(6) 0.0487(5) 0.7401(5) 0.049(2) Uani 1 1 d . . . H42A H 0.1951 0.0315 0.7887 0.059 Uiso 1 1 calc R . . C43 C 0.7361(6) -0.0431(5) 0.7405(4) 0.0459(19) Uani 1 1 d . . . C44 C 0.3491(5) -0.2598(4) 0.6973(3) 0.0349(16) Uani 1 1 d . . . C45 C 0.3911(5) 0.0355(5) 0.8043(4) 0.0393(17) Uani 1 1 d . . . C46 C 0.6256(6) -0.3985(5) 0.6737(5) 0.053(2) Uani 1 1 d . . . H46A H 0.6309 -0.4149 0.7233 0.064 Uiso 1 1 calc R . . C47 C 0.5082(5) -0.2908(5) 0.7935(4) 0.0423(18) Uani 1 1 d . . . C51 C 0.4695(8) -0.3889(7) 0.9168(5) 0.086(3) Uani 1 1 d . . . H51A H 0.4274 -0.4327 0.9521 0.104 Uiso 1 1 calc R . . C52 C 0.3939(7) -0.0310(8) 0.9533(5) 0.077(3) Uani 1 1 d . . . H52A H 0.3933 -0.0535 1.0039 0.093 Uiso 1 1 calc R . . C53 C 0.6767(8) -0.0285(8) 0.8601(5) 0.085(3) Uani 1 1 d . . . H53A H 0.6230 -0.0113 0.8932 0.102 Uiso 1 1 calc R . . C54 C 0.0722(7) 0.0721(6) 0.6567(6) 0.072(3) Uani 1 1 d . . . H54A H 0.0073 0.0709 0.6465 0.086 Uiso 1 1 calc R . . C55 C 0.8424(7) -0.0916(7) 0.8333(5) 0.076(3) Uani 1 1 d . . . H55A H 0.9057 -0.1175 0.8480 0.091 Uiso 1 1 calc R . . C56 C 0.5483(7) -0.3584(6) 0.9361(5) 0.069(3) Uani 1 1 d . . . H56A H 0.5629 -0.3829 0.9840 0.083 Uiso 1 1 calc R . . C57 C 0.7691(8) -0.0660(7) 0.8806(5) 0.074(3) Uani 1 1 d . . . H57A H 0.7805 -0.0736 0.9281 0.088 Uiso 1 1 calc R . . C58 C 0.6050(8) -0.2927(7) 0.8854(5) 0.081(3) Uani 1 1 d . . . H58A H 0.6589 -0.2696 0.8982 0.097 Uiso 1 1 calc R . . C59 C 0.4509(7) -0.3566(6) 0.8469(5) 0.071(3) Uani 1 1 d . . . H59A H 0.3968 -0.3801 0.8348 0.086 Uiso 1 1 calc R . . C60 C 0.3871(7) -0.0966(6) 0.9160(4) 0.063(2) Uani 1 1 d . . . H60A H 0.3833 -0.1655 0.9406 0.076 Uiso 1 1 calc R . . C81 C 0.1982(12) -0.2449(11) 0.8899(10) 0.163(7) Uani 1 1 d . . . H81A H 0.2423 -0.2349 0.9213 0.196 Uiso 1 1 calc R . . H81B H 0.2308 -0.2242 0.8395 0.196 Uiso 1 1 calc R . . C82 C 0.1065(12) -0.1906(10) 0.8978(9) 0.150(6) Uani 1 1 d . . . H82A H 0.0770 -0.1705 0.8527 0.179 Uiso 1 1 calc R . . H82B H 0.1133 -0.1297 0.9109 0.179 Uiso 1 1 calc R . . C83 C 0.1776(9) -0.3496(9) 0.9107(8) 0.115(4) Uani 1 1 d . . . H83A H 0.1784 -0.3715 0.8675 0.139 Uiso 1 1 calc R . . H83B H 0.2287 -0.3929 0.9390 0.139 Uiso 1 1 calc R . . C84 C 0.0425(9) -0.2590(7) 0.9571(6) 0.106(4) Uani 1 1 d . . . H84A H 0.0480 -0.2512 1.0044 0.127 Uiso 1 1 calc R . . H84B H -0.0282 -0.2450 0.9494 0.127 Uiso 1 1 calc R . . C85 C -0.1521(10) -0.5207(9) 0.8848(7) 0.117(4) Uani 1 1 d . . . H85A H -0.2115 -0.5287 0.9220 0.140 Uiso 1 1 calc R . . H85B H -0.1178 -0.5879 0.8858 0.140 Uiso 1 1 calc R . . C86 C -0.1256(13) -0.3849(14) 0.7841(7) 0.168(8) Uani 1 1 d . . . H86A H -0.1699 -0.3239 0.7652 0.202 Uiso 1 1 calc R . . H86B H -0.0741 -0.3953 0.7443 0.202 Uiso 1 1 calc R . . C87 C -0.1822(13) -0.4699(11) 0.8134(8) 0.146(6) Uani 1 1 d . . . H87A H -0.1669 -0.5150 0.7823 0.175 Uiso 1 1 calc R . . H87B H -0.2545 -0.4482 0.8176 0.175 Uiso 1 1 calc R . . C88 C -0.0791(10) -0.3746(9) 0.8418(6) 0.111(4) Uani 1 1 d . . . H88A H -0.0082 -0.3635 0.8247 0.133 Uiso 1 1 calc R . . H88B H -0.1128 -0.3164 0.8576 0.133 Uiso 1 1 calc R . . C89 C 0.2334(12) -0.6540(12) 0.8589(8) 0.160(6) Uani 1 1 d U . . H89A H 0.2282 -0.7227 0.8578 0.192 Uiso 1 1 calc R . . H89B H 0.2667 -0.6165 0.8116 0.192 Uiso 1 1 calc R . . C90 C 0.2874(12) -0.6562(15) 0.9138(10) 0.180(7) Uani 1 1 d U . . H90A H 0.3242 -0.7230 0.9304 0.216 Uiso 1 1 calc R . . H90B H 0.3362 -0.6059 0.8957 0.216 Uiso 1 1 calc R . . C91 C 0.2211(9) -0.6354(11) 0.9696(7) 0.126(5) Uani 1 1 d U . . H91A H 0.2487 -0.5899 0.9892 0.151 Uiso 1 1 calc R . . H91B H 0.2093 -0.6979 1.0085 0.151 Uiso 1 1 calc R . . C92 C 0.1341(9) -0.6040(9) 0.8756(6) 0.104(4) Uani 1 1 d U . . H92A H 0.1238 -0.5390 0.8389 0.125 Uiso 1 1 calc R . . H92B H 0.0818 -0.6460 0.8764 0.125 Uiso 1 1 calc R . . O4 O 0.076(3) 0.437(3) 0.670(2) 0.221(15) Uani 0.50 1 d PDU A 1 C93 C 0.003(5) 0.395(5) 0.6028(18) 0.398(18) Uani 0.50 1 d PD A 1 H93A H 0.0066 0.3489 0.5735 0.477 Uiso 0.50 1 calc PR A 1 H93B H -0.0427 0.4548 0.5832 0.477 Uiso 0.50 1 calc PR A 1 C94 C -0.037(4) 0.347(4) 0.6759(17) 0.374(12) Uani 0.50 1 d PD A 1 H94A H -0.1046 0.3786 0.6889 0.449 Uiso 0.50 1 calc PR A 1 H94B H -0.0416 0.2750 0.6829 0.449 Uiso 0.50 1 calc PR A 1 C95 C 0.086(3) 0.422(4) 0.5972(17) 0.20(2) Uani 0.50 1 d PD A 1 H95A H 0.0970 0.4841 0.5580 0.242 Uiso 0.50 1 calc PR A 1 H95B H 0.1399 0.3688 0.5906 0.242 Uiso 0.50 1 calc PR A 1 C96 C 0.022(4) 0.358(4) 0.7117(16) 0.55(3) Uani 0.50 1 d PD A 1 H96A H 0.0674 0.2965 0.7258 0.655 Uiso 0.50 1 calc PR A 1 H96B H -0.0140 0.3733 0.7559 0.655 Uiso 0.50 1 calc PR A 1 O4A O 0.082(2) 0.4131(16) 0.7051(11) 0.115(7) Uani 0.50 1 d PDU B 2 C93A C 0.001(4) 0.445(3) 0.616(3) 0.28(4) Uani 0.50 1 d PD B 2 H93C H 0.0135 0.4551 0.5632 0.337 Uiso 0.50 1 calc PR B 2 H93D H -0.0660 0.4765 0.6281 0.337 Uiso 0.50 1 calc PR B 2 C94A C 0.006(4) 0.339(2) 0.652(3) 0.40(7) Uani 0.50 1 d PD B 2 H94C H -0.0617 0.3174 0.6672 0.482 Uiso 0.50 1 calc PR B 2 H94D H 0.0441 0.3008 0.6198 0.482 Uiso 0.50 1 calc PR B 2 C95A C 0.064(4) 0.484(2) 0.633(2) 0.17(2) Uani 0.50 1 d PD B 2 H95C H 0.0374 0.5513 0.6373 0.204 Uiso 0.50 1 calc PR B 2 H95D H 0.1254 0.4890 0.5981 0.204 Uiso 0.50 1 calc PR B 2 C96A C 0.0480(18) 0.3273(14) 0.704(2) 0.20(3) Uani 0.50 1 d PD B 2 H96C H 0.1047 0.2752 0.7036 0.244 Uiso 0.50 1 calc PR B 2 H96D H 0.0010 0.3032 0.7482 0.244 Uiso 0.50 1 calc PR B 2 O5 O -0.307(3) -0.698(3) 0.8858(15) 0.41(2) Uani 1 1 d D . . C101 C -0.327(3) -0.723(2) 0.7901(12) 0.271(18) Uani 1 1 d D . . H10B H -0.3411 -0.7792 0.7744 0.325 Uiso 1 1 calc R . . H10C H -0.2966 -0.6735 0.7474 0.325 Uiso 1 1 calc R . . C102 C -0.4194(18) -0.677(2) 0.8174(18) 0.223(11) Uani 1 1 d D . . H10D H -0.4323 -0.6074 0.7879 0.268 Uiso 1 1 calc R . . H10E H -0.4755 -0.7149 0.8183 0.268 Uiso 1 1 calc R . . C103 C -0.2667(17) -0.7546(19) 0.834(2) 0.31(3) Uani 1 1 d D . . H10F H -0.1983 -0.7390 0.8116 0.371 Uiso 1 1 calc R . . H10G H -0.2669 -0.8275 0.8569 0.371 Uiso 1 1 calc R . . C104 C -0.408(3) -0.681(3) 0.8791(16) 0.280(18) Uani 1 1 d D . . H10H H -0.4441 -0.7350 0.9144 0.336 Uiso 1 1 calc R . . H10I H -0.4361 -0.6168 0.8891 0.336 Uiso 1 1 calc R . . Na1 Na 0.0000 -0.5000 1.0000 0.0655(12) Uani 1 2 d S . . O1 O 0.0810(5) -0.3563(4) 0.9530(3) 0.0764(17) Uani 1 1 d . . . O2 O -0.0865(5) -0.4609(5) 0.8985(3) 0.0790(18) Uani 1 1 d . . . O3 O 0.1297(4) -0.5895(5) 0.9436(3) 0.0761(18) Uani 1 1 d . . . C120 C 0.089(3) 0.028(4) 0.972(3) 0.31(3) Uani 1 1 d D . . H120 H 0.1563 0.0426 0.9577 0.371 Uiso 1 1 calc R . . C121 C 0.022(4) 0.086(3) 0.9258(19) 0.40(4) Uani 1 1 d D . . H121 H 0.0381 0.1354 0.8818 0.483 Uiso 1 1 calc R . . C122 C -0.072(3) 0.055(4) 0.957(3) 0.31(3) Uani 1 1 d D . . H122 H -0.1275 0.0876 0.9340 0.376 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 0.0344(4) 0.0364(4) 0.0335(4) -0.0103(3) -0.0060(4) -0.0035(3) In2 0.0287(3) 0.0322(3) 0.0325(3) -0.0113(2) -0.0049(2) -0.00229(19) Si4 0.0256(11) 0.0434(10) 0.0438(12) -0.0149(9) -0.0059(10) -0.0035(8) Si5 0.0327(11) 0.0307(9) 0.0371(11) -0.0081(8) -0.0034(10) -0.0043(8) Si6 0.0292(11) 0.0370(10) 0.0414(12) -0.0164(8) -0.0045(10) -0.0007(8) C1 0.049(5) 0.047(5) 0.155(10) -0.043(6) 0.014(6) -0.018(4) C2 0.046(5) 0.046(4) 0.088(7) -0.024(4) 0.004(5) -0.007(4) C4 0.100(8) 0.078(7) 0.069(7) -0.044(5) -0.021(6) -0.005(5) C5 0.064(6) 0.046(5) 0.072(7) -0.007(4) 0.013(5) -0.011(4) C6 0.061(6) 0.043(4) 0.093(7) -0.031(4) 0.004(6) -0.011(4) C7 0.075(7) 0.049(5) 0.113(9) -0.047(6) 0.031(7) -0.015(5) C8 0.037(5) 0.139(8) 0.054(6) -0.056(6) -0.011(5) 0.003(5) C9 0.066(6) 0.073(5) 0.057(6) 0.003(4) -0.027(5) -0.024(4) C10 0.027(4) 0.047(5) 0.135(9) -0.039(5) 0.006(5) -0.001(3) C11 0.040(5) 0.091(6) 0.058(6) -0.012(5) -0.019(5) -0.001(4) C12 0.062(6) 0.035(4) 0.094(7) -0.033(4) 0.008(5) 0.007(4) C13 0.049(5) 0.053(5) 0.048(5) -0.013(4) 0.000(4) -0.014(4) C14 0.038(5) 0.056(5) 0.093(7) -0.037(5) -0.019(5) 0.008(4) C15 0.036(5) 0.060(5) 0.068(6) -0.018(4) -0.002(5) 0.014(4) C16 0.045(5) 0.053(4) 0.050(5) -0.014(4) -0.002(4) -0.016(4) C17 0.045(5) 0.054(5) 0.092(7) -0.036(5) 0.002(5) -0.015(4) C18 0.068(6) 0.061(5) 0.041(5) -0.025(4) -0.008(4) -0.001(4) C19 0.032(4) 0.057(4) 0.062(5) -0.022(4) -0.007(4) -0.009(4) C20 0.047(5) 0.056(5) 0.060(6) -0.020(4) -0.015(5) 0.005(4) C21 0.034(5) 0.064(5) 0.091(7) -0.035(5) -0.004(5) -0.001(4) C22 0.044(5) 0.043(4) 0.072(6) -0.026(4) -0.016(4) 0.007(3) C23 0.050(5) 0.054(5) 0.044(5) -0.021(4) -0.001(4) -0.003(4) C24 0.030(4) 0.077(6) 0.062(6) -0.030(4) 0.001(4) -0.015(4) C25 0.054(5) 0.042(4) 0.055(5) -0.022(4) -0.001(4) -0.006(3) C26 0.065(6) 0.053(5) 0.050(5) -0.007(4) 0.005(5) -0.012(4) C27 0.046(5) 0.041(4) 0.096(8) -0.024(5) 0.003(5) 0.005(4) C28 0.040(5) 0.050(5) 0.084(6) -0.034(4) 0.013(5) -0.003(4) C29 0.027(4) 0.042(4) 0.041(4) -0.013(3) -0.005(4) -0.004(3) C30 0.025(4) 0.072(5) 0.054(5) -0.012(4) -0.003(4) -0.004(4) C31 0.032(4) 0.050(4) 0.068(6) -0.018(4) 0.007(4) -0.012(3) C34 0.044(5) 0.035(4) 0.054(5) -0.012(3) -0.006(4) -0.004(3) C35 0.023(4) 0.041(4) 0.054(5) -0.020(3) 0.002(4) -0.003(3) C36 0.036(4) 0.041(4) 0.056(5) -0.023(3) -0.005(4) -0.001(3) C37 0.038(5) 0.053(5) 0.061(5) -0.019(4) -0.003(4) -0.010(4) C38 0.060(6) 0.078(6) 0.077(7) -0.030(5) -0.037(6) 0.017(5) C39 0.086(7) 0.055(5) 0.058(6) -0.028(4) 0.012(5) -0.019(5) C40 0.032(4) 0.034(4) 0.046(5) -0.015(3) -0.007(4) 0.001(3) C41 0.036(4) 0.030(3) 0.048(5) -0.010(3) -0.005(4) -0.011(3) C42 0.037(5) 0.054(4) 0.058(5) -0.018(4) -0.008(5) -0.002(4) C43 0.047(5) 0.051(4) 0.044(5) -0.014(4) -0.007(4) -0.015(4) C44 0.038(4) 0.032(3) 0.035(4) -0.012(3) -0.003(4) -0.005(3) C45 0.030(4) 0.040(4) 0.050(5) -0.019(3) -0.007(4) 0.005(3) C46 0.042(5) 0.047(4) 0.075(6) -0.028(4) -0.007(5) 0.000(4) C47 0.047(5) 0.038(4) 0.037(4) -0.006(3) -0.003(4) 0.000(3) C51 0.095(8) 0.080(6) 0.066(7) 0.020(5) -0.020(6) -0.029(6) C52 0.083(7) 0.110(8) 0.035(5) -0.020(5) -0.009(5) 0.002(6) C53 0.066(7) 0.135(9) 0.070(7) -0.057(6) -0.011(6) 0.003(6) C54 0.045(6) 0.074(6) 0.112(9) -0.045(6) -0.031(7) 0.009(5) C55 0.067(7) 0.098(7) 0.058(6) -0.006(5) -0.040(6) 0.006(5) C56 0.083(7) 0.070(6) 0.045(6) 0.000(5) -0.027(6) 0.004(5) C57 0.092(8) 0.091(7) 0.050(6) -0.022(5) -0.020(6) -0.028(6) C58 0.092(8) 0.095(7) 0.061(6) -0.008(5) -0.035(6) -0.023(6) C59 0.076(7) 0.078(6) 0.054(6) 0.009(5) -0.025(5) -0.030(5) C60 0.076(7) 0.073(5) 0.039(5) -0.015(4) -0.009(5) -0.001(5) C81 0.121(13) 0.122(12) 0.23(2) -0.044(12) 0.045(14) -0.054(10) C82 0.134(13) 0.084(9) 0.186(16) 0.022(9) 0.010(13) -0.037(9) C83 0.089(9) 0.108(9) 0.145(12) -0.040(8) 0.025(9) -0.038(7) C84 0.119(10) 0.076(7) 0.108(9) -0.013(6) 0.004(8) -0.012(7) C85 0.123(11) 0.129(10) 0.118(10) -0.029(8) -0.055(9) -0.035(8) C86 0.174(16) 0.237(18) 0.079(10) 0.038(10) -0.062(11) -0.096(14) C87 0.175(16) 0.154(13) 0.129(12) -0.033(10) -0.099(12) -0.004(11) C88 0.125(11) 0.117(9) 0.077(8) 0.002(7) -0.034(8) -0.012(8) C89 0.157(13) 0.195(13) 0.113(11) -0.078(10) -0.013(10) 0.096(11) C90 0.114(12) 0.283(17) 0.176(14) -0.148(13) -0.031(11) 0.066(12) C91 0.082(8) 0.176(12) 0.125(11) -0.071(9) -0.042(8) 0.063(8) C92 0.105(9) 0.130(9) 0.083(8) -0.050(7) -0.018(7) 0.016(7) O4 0.22(3) 0.22(3) 0.24(4) -0.06(3) -0.06(3) -0.05(3) C93 0.58(6) 0.57(6) 0.15(4) -0.05(6) -0.03(6) -0.519 C94 0.72(5) 0.43(3) 0.08(2) -0.05(3) 0.01(4) -0.525 C95 0.12(3) 0.40(8) 0.09(3) -0.08(4) 0.04(3) -0.09(4) C96 0.99(11) 0.47(5) 0.29(7) -0.29(6) 0.38(7) -0.625 O4A 0.152(16) 0.094(12) 0.093(14) -0.021(10) -0.039(13) 0.019(11) C93A 0.26(7) 0.20(5) 0.41(10) -0.02(6) -0.26(8) 0.01(5) C94A 0.46(10) 0.07(2) 0.83(16) -0.16(5) -0.54(11) 0.11(4) C95A 0.28(5) 0.10(2) 0.13(3) 0.07(2) -0.13(3) -0.09(3) C96A 0.067(17) 0.036(13) 0.47(8) 0.04(2) -0.12(3) -0.007(11) O5 0.54(5) 0.42(4) 0.37(3) -0.11(3) -0.22(4) -0.23(4) C101 0.33(4) 0.28(3) 0.16(2) -0.10(2) 0.01(2) 0.13(3) C102 0.19(3) 0.27(3) 0.24(3) -0.05(2) -0.06(2) -0.09(2) C103 0.16(2) 0.15(2) 0.61(8) -0.06(3) -0.15(3) 0.032(16) C104 0.28(4) 0.42(5) 0.18(3) -0.16(3) -0.01(3) -0.02(4) Na1 0.060(3) 0.068(3) 0.068(3) -0.019(2) -0.009(3) -0.005(2) O1 0.074(5) 0.066(4) 0.084(5) -0.017(3) 0.003(4) -0.015(3) O2 0.084(5) 0.088(4) 0.065(4) -0.008(3) -0.028(4) -0.018(4) O3 0.057(4) 0.094(4) 0.074(4) -0.031(4) -0.011(4) 0.021(3) C120 0.19(2) 0.41(6) 0.53(7) -0.42(6) -0.19(4) 0.11(3) C121 0.30(4) 0.57(8) 0.59(7) -0.54(7) 0.02(6) -0.14(5) C122 0.27(4) 0.33(5) 0.52(8) -0.35(5) -0.22(5) 0.10(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 In2 2.8269(8) . ? In1 In2 2.8269(8) 2_656 ? In2 Si5 2.6350(19) . ? In2 Si6 2.636(2) . ? In2 Si4 2.6407(19) . ? Si4 C43 1.894(7) . ? Si4 C29 1.895(7) . ? Si4 C35 1.898(7) . ? Si5 C41 1.874(7) . ? Si5 C44 1.890(7) . ? Si5 C47 1.893(7) . ? Si6 C36 1.892(7) . ? Si6 C45 1.895(7) . ? Si6 C40 1.898(7) . ? C1 C6 1.357(11) . ? C1 C10 1.383(10) . ? C2 C31 1.368(10) . ? C2 C15 1.383(11) . ? C4 C52 1.384(13) . ? C4 C18 1.390(11) . ? C5 C17 1.363(12) . ? C5 C26 1.372(11) . ? C6 C12 1.350(11) . ? C7 C27 1.357(13) . ? C7 C39 1.368(12) . ? C8 C43 1.357(11) . ? C8 C53 1.368(11) . ? C9 C58 1.364(11) . ? C9 C47 1.394(10) . ? C10 C36 1.380(10) . ? C11 C55 1.370(12) . ? C11 C43 1.414(10) . ? C12 C28 1.389(10) . ? C13 C26 1.378(10) . ? C13 C35 1.394(10) . ? C14 C24 1.365(10) . ? C14 C22 1.385(10) . ? C15 C30 1.366(10) . ? C16 C24 1.384(10) . ? C16 C34 1.395(10) . ? C17 C37 1.390(11) . ? C18 C45 1.409(9) . ? C19 C29 1.395(9) . ? C19 C30 1.405(10) . ? C20 C38 1.398(11) . ? C20 C40 1.408(10) . ? C21 C54 1.361(12) . ? C21 C42 1.384(10) . ? C22 C44 1.407(9) . ? C23 C60 1.360(10) . ? C23 C45 1.386(10) . ? C25 C41 1.378(10) . ? C25 C39 1.429(11) . ? C27 C46 1.390(11) . ? C28 C36 1.389(9) . ? C29 C31 1.393(9) . ? C34 C44 1.407(9) . ? C35 C37 1.409(9) . ? C38 C54 1.349(13) . ? C40 C42 1.388(10) . ? C41 C46 1.397(9) . ? C47 C59 1.385(11) . ? C51 C56 1.370(13) . ? C51 C59 1.373(12) . ? C52 C60 1.368(12) . ? C53 C57 1.379(13) . ? C55 C57 1.333(13) . ? C56 C58 1.356(13) . ? C81 C82 1.383(18) . ? C81 C83 1.465(16) . ? C82 C84 1.507(16) . ? C83 O1 1.436(12) . ? C84 O1 1.417(11) . ? C85 O2 1.430(11) . ? C85 C87 1.476(15) . ? C86 C87 1.437(18) . ? C86 C88 1.453(15) . ? C88 O2 1.384(11) . ? C89 C90 1.407(17) . ? C89 C92 1.470(15) . ? C90 C91 1.375(17) . ? C91 O3 1.428(11) . ? C92 O3 1.409(11) . ? O4 C96 1.39(2) . ? O4 C95 1.50(3) . ? C93 C95 1.23(3) . ? C93 C94 1.45(3) . ? C94 C96 1.22(3) . ? O4A C96A 1.37(2) . ? O4A C95A 1.51(3) . ? C93A C95A 1.23(3) . ? C93A C94A 1.44(3) . ? C94A C96A 1.22(3) . ? O5 C104 1.39(2) . ? O5 C103 1.47(3) . ? C101 C103 1.25(3) . ? C101 C102 1.42(2) . ? C102 C104 1.24(2) . ? Na1 O1 2.315(6) . ? Na1 O1 2.315(6) 2_547 ? Na1 O3 2.345(6) 2_547 ? Na1 O3 2.345(6) . ? Na1 O2 2.388(6) 2_547 ? Na1 O2 2.388(6) . ? C120 C121 1.40(3) . ? C120 C122 1.52(5) 2_557 ? C121 C122 1.40(3) . ? C122 C120 1.52(5) 2_557 ? 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 In2 In1 In2 180.0 . 2_656 ? Si5 In2 Si6 113.21(7) . . ? Si5 In2 Si4 113.77(6) . . ? Si6 In2 Si4 113.18(6) . . ? Si5 In2 In1 103.44(5) . . ? Si6 In2 In1 107.27(5) . . ? Si4 In2 In1 104.87(6) . . ? C43 Si4 C29 105.7(3) . . ? C43 Si4 C35 106.0(3) . . ? C29 Si4 C35 105.7(3) . . ? C43 Si4 In2 110.5(3) . . ? C29 Si4 In2 118.0(2) . . ? C35 Si4 In2 110.2(2) . . ? C41 Si5 C44 103.8(3) . . ? C41 Si5 C47 106.3(3) . . ? C44 Si5 C47 106.9(3) . . ? C41 Si5 In2 111.6(2) . . ? C44 Si5 In2 116.6(2) . . ? C47 Si5 In2 110.9(2) . . ? C36 Si6 C45 106.3(3) . . ? C36 Si6 C40 104.5(3) . . ? C45 Si6 C40 105.8(3) . . ? C36 Si6 In2 117.4(2) . . ? C45 Si6 In2 110.4(2) . . ? C40 Si6 In2 111.5(2) . . ? C6 C1 C10 120.5(8) . . ? C31 C2 C15 120.9(7) . . ? C52 C4 C18 121.1(8) . . ? C17 C5 C26 119.3(7) . . ? C12 C6 C1 119.4(7) . . ? C27 C7 C39 120.6(8) . . ? C43 C8 C53 125.2(8) . . ? C58 C9 C47 122.9(8) . . ? C36 C10 C1 122.8(7) . . ? C55 C11 C43 120.5(9) . . ? C6 C12 C28 119.7(7) . . ? C26 C13 C35 121.4(7) . . ? C24 C14 C22 121.2(7) . . ? C30 C15 C2 119.5(7) . . ? C24 C16 C34 121.4(7) . . ? C5 C17 C37 120.9(7) . . ? C4 C18 C45 120.0(7) . . ? C29 C19 C30 122.0(7) . . ? C38 C20 C40 120.0(9) . . ? C54 C21 C42 118.7(9) . . ? C14 C22 C44 122.4(7) . . ? C60 C23 C45 123.1(7) . . ? C14 C24 C16 118.3(7) . . ? C41 C25 C39 121.2(7) . . ? C5 C26 C13 120.9(8) . . ? C7 C27 C46 119.0(8) . . ? C12 C28 C36 123.3(8) . . ? C31 C29 C19 116.3(6) . . ? C31 C29 Si4 123.0(5) . . ? C19 C29 Si4 120.6(5) . . ? C15 C30 C19 119.3(7) . . ? C2 C31 C29 121.9(7) . . ? C16 C34 C44 121.1(6) . . ? C13 C35 C37 116.8(6) . . ? C13 C35 Si4 120.0(5) . . ? C37 C35 Si4 123.3(6) . . ? C10 C36 C28 114.4(6) . . ? C10 C36 Si6 124.3(5) . . ? C28 C36 Si6 121.3(6) . . ? C17 C37 C35 120.7(7) . . ? C54 C38 C20 120.9(9) . . ? C7 C39 C25 119.7(8) . . ? C42 C40 C20 116.3(6) . . ? C42 C40 Si6 124.4(5) . . ? C20 C40 Si6 119.3(6) . . ? C25 C41 C46 115.9(7) . . ? C25 C41 Si5 119.9(5) . . ? C46 C41 Si5 124.2(6) . . ? C21 C42 C40 123.1(8) . . ? C8 C43 C11 114.8(7) . . ? C8 C43 Si4 121.6(6) . . ? C11 C43 Si4 123.6(6) . . ? C22 C44 C34 115.6(6) . . ? C22 C44 Si5 122.8(5) . . ? C34 C44 Si5 121.6(5) . . ? C23 C45 C18 116.5(7) . . ? C23 C45 Si6 120.8(5) . . ? C18 C45 Si6 122.5(5) . . ? C27 C46 C41 123.5(8) . . ? C59 C47 C9 114.9(7) . . ? C59 C47 Si5 124.4(6) . . ? C9 C47 Si5 120.4(6) . . ? C56 C51 C59 120.6(9) . . ? C60 C52 C4 118.8(8) . . ? C8 C53 C57 117.8(9) . . ? C38 C54 C21 121.0(8) . . ? C57 C55 C11 122.0(8) . . ? C58 C56 C51 118.7(8) . . ? C55 C57 C53 119.7(8) . . ? C56 C58 C9 120.6(9) . . ? C51 C59 C47 122.3(8) . . ? C23 C60 C52 120.4(8) . . ? C82 C81 C83 105.7(12) . . ? C81 C82 C84 105.9(12) . . ? O1 C83 C81 107.2(10) . . ? O1 C84 C82 104.3(10) . . ? O2 C85 C87 107.9(10) . . ? C87 C86 C88 107.3(11) . . ? C86 C87 C85 105.7(11) . . ? O2 C88 C86 108.9(11) . . ? C90 C89 C92 106.3(11) . . ? C91 C90 C89 108.2(13) . . ? C90 C91 O3 108.8(11) . . ? O3 C92 C89 106.9(9) . . ? C96 O4 C95 101(2) . . ? C95 C93 C94 113(3) . . ? C96 C94 C93 104(2) . . ? C93 C95 O4 97(2) . . ? C94 C96 O4 108(2) . . ? C96A O4A C95A 102.4(19) . . ? C95A C93A C94A 111(2) . . ? C96A C94A C93A 106(2) . . ? C93A C95A O4A 103(2) . . ? C94A C96A O4A 113(2) . . ? C104 O5 C103 102.9(17) . . ? C103 C101 C102 114(2) . . ? C104 C102 C101 104(2) . . ? C101 C103 O5 100.6(18) . . ? C102 C104 O5 110(2) . . ? O1 Na1 O1 180.000(1) . 2_547 ? O1 Na1 O3 89.2(2) . 2_547 ? O1 Na1 O3 90.8(2) 2_547 2_547 ? O1 Na1 O3 90.8(2) . . ? O1 Na1 O3 89.2(2) 2_547 . ? O3 Na1 O3 180.0(3) 2_547 . ? O1 Na1 O2 88.0(2) . 2_547 ? O1 Na1 O2 92.0(2) 2_547 2_547 ? O3 Na1 O2 90.2(2) 2_547 2_547 ? O3 Na1 O2 89.8(2) . 2_547 ? O1 Na1 O2 92.0(2) . . ? O1 Na1 O2 88.0(2) 2_547 . ? O3 Na1 O2 89.8(2) 2_547 . ? O3 Na1 O2 90.2(2) . . ? O2 Na1 O2 180.000(1) 2_547 . ? C84 O1 C83 108.0(8) . . ? C84 O1 Na1 126.6(6) . . ? C83 O1 Na1 125.3(6) . . ? C88 O2 C85 108.5(8) . . ? C88 O2 Na1 124.3(6) . . ? C85 O2 Na1 127.1(6) . . ? C92 O3 C91 106.9(8) . . ? C92 O3 Na1 126.2(6) . . ? C91 O3 Na1 126.9(6) . . ? C121 C120 C122 131(4) . 2_557 ? C122 C121 C120 106(3) . . ? C121 C122 C120 123(4) . 2_557 ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 23.90 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 2.383 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.098 # Attachment 'comp_8_728996.cif' data_m38_comp_8 _database_code_depnum_ccdc_archive 'CCDC 728996' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H120 In8 Si8 _ Li2 O10.5 C42 H84' _chemical_formula_sum 'C186 H204 In8 Li2 O10.50 Si8' _chemical_formula_weight 3764.65 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' Si Si 0.0817 0.0704 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 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 66.057(8) _cell_length_b 17.775(2) _cell_length_c 38.004(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.52(2) _cell_angle_gamma 90.00 _cell_volume 43872(15) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15312 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; typical crystals were only very weakly diffracting and no intensities could be collected at theat larger than 44. Due to the large cell dimensions ( a axis) peak overlap affected intensities. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'image plate, 2 circle goniometer' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27009 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -71 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 22.49 _reflns_number_total 11798 _reflns_number_gt 8944 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement STOE _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXTL 5.01' _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 structure is severely disordered in the Li(thf)n and thf parts. It was only partially possible to resolve the disorder. Consequently, the quality of this structure is very low. Due to the low theta values collected only a very low data/parameter ratio results which gives very bad bonding parameter ESD's an dnon trustable ADPs. This structure allows only for resolving the cluster core In8Si8 properly. ; _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^)+(0.1372P)^2^+4810.1870P] 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 11798 _refine_ls_number_parameters 2301 _refine_ls_number_restraints 2911 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_gt 0.1124 _refine_ls_wR_factor_ref 0.3108 _refine_ls_wR_factor_gt 0.2861 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.004 _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 0.10108(3) 0.59193(9) 0.37668(6) 0.0372(8) Uani 1 1 d . . . In2 In 0.10175(3) 0.74781(9) 0.39382(6) 0.0376(8) Uani 1 1 d . . . In3 In 0.11387(4) 0.76143(9) 0.32571(6) 0.0395(8) Uani 1 1 d . . . In4 In 0.11831(4) 0.60436(9) 0.31317(6) 0.0381(8) Uani 1 1 d . . . In5 In 0.14631(3) 0.55616(9) 0.37933(6) 0.0404(8) Uani 1 1 d . . . In6 In 0.13625(3) 0.65345(9) 0.43226(6) 0.0382(8) Uani 1 1 d . . . In7 In 0.14544(3) 0.78619(9) 0.39380(6) 0.0365(8) Uani 1 1 d . . . In8 In 0.15655(3) 0.68953(9) 0.34147(7) 0.0374(8) Uani 1 1 d . . . Si1 Si 0.07233(14) 0.4963(4) 0.3853(3) 0.040(3) Uani 1 1 d . . . Si2 Si 0.07110(14) 0.8156(4) 0.4144(3) 0.043(3) Uani 1 1 d . . . Si3 Si 0.09867(15) 0.8628(4) 0.2780(3) 0.044(3) Uani 1 1 d . . . Si4 Si 0.10686(14) 0.5402(4) 0.2515(3) 0.040(3) Uani 1 1 d . . . Si5 Si 0.16895(14) 0.4352(3) 0.3925(3) 0.037(3) Uani 1 1 d . . . Si6 Si 0.14613(14) 0.6368(4) 0.5015(3) 0.040(3) Uani 1 1 d . . . Si7 Si 0.16661(13) 0.9034(4) 0.4205(2) 0.035(3) Uani 1 1 d . . . Si8 Si 0.18946(15) 0.7006(4) 0.3127(3) 0.043(3) Uani 1 1 d . . . C1 C 0.0809(5) 0.3967(14) 0.3803(9) 0.041(8) Uani 1 1 d U . . C2 C 0.0678(5) 0.3421(12) 0.3630(8) 0.036(8) Uani 1 1 d U . . H2A H 0.0541 0.3556 0.3527 0.044 Uiso 1 1 calc R . . C3 C 0.0744(5) 0.2660(15) 0.3601(9) 0.057(10) Uani 1 1 d U . . H3A H 0.0656 0.2290 0.3472 0.068 Uiso 1 1 calc R . . C4 C 0.0940(5) 0.2494(17) 0.3768(9) 0.062(10) Uani 1 1 d U . . H4A H 0.0985 0.1987 0.3767 0.075 Uiso 1 1 calc R . . C5 C 0.1081(6) 0.3041(17) 0.3947(10) 0.068(11) Uani 1 1 d U . . H5A H 0.1218 0.2921 0.4056 0.082 Uiso 1 1 calc R . . C6 C 0.1001(5) 0.3761(16) 0.3948(9) 0.058(10) Uani 1 1 d U . . H6A H 0.1091 0.4142 0.4061 0.070 Uiso 1 1 calc R . . C7 C 0.0482(5) 0.5068(14) 0.3493(9) 0.045(9) Uani 1 1 d U . . C8 C 0.0294(5) 0.4872(14) 0.3588(9) 0.044(9) Uani 1 1 d U . . H8A H 0.0284 0.4729 0.3825 0.053 Uiso 1 1 calc R . . C9 C 0.0115(6) 0.4898(16) 0.3307(11) 0.065(11) Uani 1 1 d U . . H9A H -0.0014 0.4742 0.3360 0.078 Uiso 1 1 calc R . . C10 C 0.0123(6) 0.5132(16) 0.2978(10) 0.059(10) Uani 1 1 d U . . H10A H 0.0001 0.5146 0.2802 0.071 Uiso 1 1 calc R . . C11 C 0.0302(6) 0.5348(18) 0.2892(11) 0.077(12) Uani 1 1 d U . . H11A H 0.0304 0.5517 0.2655 0.092 Uiso 1 1 calc R . . C12 C 0.0485(6) 0.5331(18) 0.3139(11) 0.073(11) Uani 1 1 d U . . H12A H 0.0610 0.5492 0.3073 0.088 Uiso 1 1 calc R . . C13 C 0.0638(4) 0.5050(13) 0.4287(8) 0.039(8) Uani 1 1 d U . . C14 C 0.0638(4) 0.5750(14) 0.4474(9) 0.040(8) Uani 1 1 d U . . H14A H 0.0694 0.6175 0.4374 0.048 Uiso 1 1 calc R . . C15 C 0.0566(5) 0.5856(17) 0.4782(10) 0.058(10) Uani 1 1 d U . . H15A H 0.0576 0.6331 0.4899 0.070 Uiso 1 1 calc R . . C16 C 0.0480(5) 0.5250(19) 0.4917(11) 0.078(12) Uani 1 1 d U . . H16A H 0.0428 0.5311 0.5133 0.094 Uiso 1 1 calc R . . C17 C 0.0463(5) 0.4538(17) 0.4751(10) 0.065(10) Uani 1 1 d U . . H17A H 0.0399 0.4128 0.4846 0.078 Uiso 1 1 calc R . . C18 C 0.0546(5) 0.4462(15) 0.4441(9) 0.050(9) Uani 1 1 d U . . H18A H 0.0540 0.3982 0.4330 0.060 Uiso 1 1 calc R . . C19 C 0.0667(4) 0.7923(11) 0.4601(8) 0.021(7) Uani 1 1 d U . . C20 C 0.0484(5) 0.7979(13) 0.4708(9) 0.038(8) Uani 1 1 d U . . H20A H 0.0369 0.8113 0.4531 0.046 Uiso 1 1 calc R . . C21 C 0.0450(6) 0.7855(16) 0.5057(10) 0.057(10) Uani 1 1 d U . . H21A H 0.0316 0.7901 0.5114 0.069 Uiso 1 1 calc R . . C22 C 0.0613(5) 0.7668(15) 0.5308(10) 0.053(10) Uani 1 1 d U . . H22A H 0.0594 0.7575 0.5546 0.063 Uiso 1 1 calc R . . C23 C 0.0808(6) 0.7606(17) 0.5232(11) 0.068(11) Uani 1 1 d U . . H23A H 0.0922 0.7485 0.5413 0.082 Uiso 1 1 calc R . . C24 C 0.0831(5) 0.7725(14) 0.4886(9) 0.047(9) Uani 1 1 d U . . H24A H 0.0965 0.7673 0.4832 0.057 Uiso 1 1 calc R . . C25 C 0.0463(5) 0.7903(14) 0.3833(9) 0.046(9) Uani 1 1 d U . . C26 C 0.0423(5) 0.7194(13) 0.3687(8) 0.037(8) Uani 1 1 d U . . H26A H 0.0526 0.6818 0.3727 0.045 Uiso 1 1 calc R . . C27 C 0.0241(5) 0.7034(16) 0.3493(10) 0.059(10) Uani 1 1 d U . . H27A H 0.0223 0.6540 0.3397 0.070 Uiso 1 1 calc R . . C28 C 0.0072(5) 0.7513(16) 0.3413(9) 0.058(10) Uani 1 1 d U . . H28A H -0.0053 0.7369 0.3263 0.070 Uiso 1 1 calc R . . C29 C 0.0101(5) 0.8211(16) 0.3568(9) 0.057(10) Uani 1 1 d U . . H29A H -0.0008 0.8565 0.3534 0.068 Uiso 1 1 calc R . . C30 C 0.0288(5) 0.8401(14) 0.3771(8) 0.041(8) Uani 1 1 d U . . H30A H 0.0303 0.8886 0.3878 0.050 Uiso 1 1 calc R . . C31 C 0.0725(4) 0.9223(11) 0.4130(7) 0.015(6) Uani 1 1 d U . . C32 C 0.0631(4) 0.9661(14) 0.4372(8) 0.043(8) Uani 1 1 d U . . H32A H 0.0577 0.9434 0.4561 0.052 Uiso 1 1 calc R . . C33 C 0.0622(5) 1.0460(17) 0.4315(10) 0.065(10) Uani 1 1 d U . . H33A H 0.0559 1.0771 0.4467 0.078 Uiso 1 1 calc R . . C34 C 0.0706(5) 1.0786(18) 0.4038(10) 0.063(10) Uani 1 1 d U . . H34A H 0.0700 1.1316 0.4007 0.076 Uiso 1 1 calc R . . C35 C 0.0797(5) 1.0356(17) 0.3810(10) 0.064(10) Uani 1 1 d U . . H35A H 0.0857 1.0592 0.3630 0.077 Uiso 1 1 calc R . . C36 C 0.0801(5) 0.9569(15) 0.3843(9) 0.053(9) Uani 1 1 d U . . H36A H 0.0855 0.9270 0.3674 0.064 Uiso 1 1 calc R . . C37 C 0.0702(5) 0.8524(14) 0.2636(9) 0.045(9) Uani 1 1 d U . . C38 C 0.0608(5) 0.8751(14) 0.2278(9) 0.048(9) Uani 1 1 d U . . H38A H 0.0690 0.8901 0.2110 0.058 Uiso 1 1 calc R . . C39 C 0.0390(6) 0.8745(18) 0.2182(11) 0.078(12) Uani 1 1 d U . . H39A H 0.0328 0.8941 0.1955 0.094 Uiso 1 1 calc R . . C40 C 0.0266(6) 0.8472(16) 0.2398(11) 0.063(10) Uani 1 1 d U . . H40A H 0.0121 0.8440 0.2322 0.076 Uiso 1 1 calc R . . C41 C 0.0359(6) 0.8244(18) 0.2732(11) 0.073(12) Uani 1 1 d U . . H41A H 0.0275 0.8043 0.2887 0.088 Uiso 1 1 calc R . . C42 C 0.0562(6) 0.8289(17) 0.2850(11) 0.070(11) Uani 1 1 d U . . H42A H 0.0614 0.8155 0.3092 0.084 Uiso 1 1 calc R . . C43 C 0.1041(5) 0.9618(13) 0.2942(8) 0.034(8) Uani 1 1 d U . . C44 C 0.1222(5) 0.9851(15) 0.3157(9) 0.049(9) Uani 1 1 d U . . H44A H 0.1318 0.9469 0.3251 0.059 Uiso 1 1 calc R . . C45 C 0.1279(6) 1.0585(18) 0.3247(10) 0.076(12) Uani 1 1 d U . . H45A H 0.1412 1.0722 0.3371 0.091 Uiso 1 1 calc R . . C46 C 0.1116(6) 1.1128(18) 0.3136(10) 0.065(10) Uani 1 1 d U . . H46A H 0.1143 1.1637 0.3204 0.077 Uiso 1 1 calc R . . C47 C 0.0926(5) 1.0963(15) 0.2941(9) 0.048(9) Uani 1 1 d U . . H47A H 0.0827 1.1348 0.2875 0.057 Uiso 1 1 calc R . . C48 C 0.0881(5) 1.0228(14) 0.2842(8) 0.044(9) Uani 1 1 d U . . H48A H 0.0749 1.0103 0.2711 0.053 Uiso 1 1 calc R . . C49 C 0.1091(5) 0.8581(13) 0.2355(8) 0.039(8) Uani 1 1 d U . . C50 C 0.1100(5) 0.9213(16) 0.2122(10) 0.059(10) Uani 1 1 d U . . H50A H 0.1063 0.9700 0.2191 0.071 Uiso 1 1 calc R . . C51 C 0.1164(6) 0.912(2) 0.1796(12) 0.092(13) Uani 1 1 d U . . H51A H 0.1182 0.9549 0.1657 0.110 Uiso 1 1 calc R . . C52 C 0.1202(5) 0.8428(19) 0.1673(11) 0.079(12) Uani 1 1 d U . . H52A H 0.1231 0.8365 0.1439 0.095 Uiso 1 1 calc R . . C53 C 0.1198(5) 0.7810(19) 0.1899(11) 0.073(11) Uani 1 1 d U . . H53A H 0.1238 0.7332 0.1824 0.088 Uiso 1 1 calc R . . C54 C 0.1138(5) 0.7868(15) 0.2225(9) 0.046(9) Uani 1 1 d U . . H54A H 0.1129 0.7429 0.2364 0.055 Uiso 1 1 calc R . . C55 C 0.0792(4) 0.5655(13) 0.2320(8) 0.033(8) Uani 1 1 d U . . C56 C 0.0704(5) 0.6342(15) 0.2393(9) 0.048(9) Uani 1 1 d U . . H56A H 0.0781 0.6679 0.2559 0.058 Uiso 1 1 calc R . . C57 C 0.0511(5) 0.6537(16) 0.2233(9) 0.053(9) Uani 1 1 d U . . H57A H 0.0459 0.7007 0.2294 0.064 Uiso 1 1 calc R . . C58 C 0.0385(5) 0.6089(16) 0.1983(9) 0.058(10) Uani 1 1 d U . . H58A H 0.0249 0.6232 0.1874 0.069 Uiso 1 1 calc R . . C59 C 0.0476(5) 0.5397(15) 0.1904(9) 0.049(9) Uani 1 1 d U . . H59A H 0.0400 0.5066 0.1734 0.059 Uiso 1 1 calc R . . C60 C 0.0663(5) 0.5203(17) 0.2061(10) 0.061(10) Uani 1 1 d U . . H60A H 0.0715 0.4734 0.1998 0.074 Uiso 1 1 calc R . . C61 C 0.1060(5) 0.4345(15) 0.2518(9) 0.050(9) Uani 1 1 d U . . C62 C 0.1003(4) 0.3941(14) 0.2809(9) 0.046(9) Uani 1 1 d U . . H62A H 0.0978 0.4209 0.3013 0.055 Uiso 1 1 calc R . . C63 C 0.0983(5) 0.3169(15) 0.2799(9) 0.051(9) Uani 1 1 d U . . H63A H 0.0943 0.2906 0.2993 0.061 Uiso 1 1 calc R . . C64 C 0.1022(5) 0.2781(18) 0.2500(10) 0.061(10) Uani 1 1 d U . . H64A H 0.1006 0.2250 0.2494 0.074 Uiso 1 1 calc R . . C65 C 0.1083(5) 0.3128(17) 0.2215(10) 0.067(11) Uani 1 1 d U . . H65A H 0.1108 0.2843 0.2016 0.081 Uiso 1 1 calc R . . C66 C 0.1107(4) 0.3889(14) 0.2222(8) 0.044(8) Uani 1 1 d U . . H66A H 0.1154 0.4130 0.2029 0.053 Uiso 1 1 calc R . . C67 C 0.1221(5) 0.5675(12) 0.2174(9) 0.028(7) Uani 1 1 d U . . C68 C 0.1426(6) 0.5906(18) 0.2273(12) 0.074(12) Uani 1 1 d U . . H68A H 0.1486 0.5949 0.2520 0.089 Uiso 1 1 calc R . . C69 C 0.1542(8) 0.607(2) 0.2020(14) 0.110(16) Uani 1 1 d U . . H69A H 0.1681 0.6224 0.2092 0.132 Uiso 1 1 calc R . . C70 C 0.1462(6) 0.6017(17) 0.1666(12) 0.070(11) Uani 1 1 d U . . H70A H 0.1548 0.6099 0.1494 0.084 Uiso 1 1 calc R . . C71 C 0.1260(5) 0.5847(15) 0.1555(10) 0.059(10) Uani 1 1 d U . . H71A H 0.1202 0.5853 0.1307 0.070 Uiso 1 1 calc R . . C72 C 0.1138(6) 0.5663(15) 0.1805(10) 0.056(10) Uani 1 1 d U . . H72A H 0.0998 0.5528 0.1726 0.067 Uiso 1 1 calc R . . C73 C 0.1722(2) 0.3774(6) 0.3516(4) 0.031(8) Uani 1 1 d GU . . C74 C 0.1899(2) 0.3367(9) 0.3501(4) 0.057(10) Uani 1 1 d GU . . H74A H 0.2018 0.3432 0.3681 0.068 Uiso 1 1 calc R . . C75 C 0.1903(3) 0.2864(9) 0.3222(5) 0.051(9) Uani 1 1 d GU . . H75A H 0.2025 0.2585 0.3211 0.062 Uiso 1 1 calc R . . C76 C 0.1729(3) 0.2769(9) 0.2958(4) 0.087(13) Uani 1 1 d GU . . H76A H 0.1732 0.2426 0.2768 0.105 Uiso 1 1 calc R . . C77 C 0.1551(3) 0.3177(12) 0.2974(3) 0.082(12) Uani 1 1 d GU . . H77A H 0.1432 0.3112 0.2794 0.099 Uiso 1 1 calc R . . C78 C 0.1548(2) 0.3680(10) 0.3253(4) 0.069(11) Uani 1 1 d GU . . H78A H 0.1426 0.3958 0.3264 0.082 Uiso 1 1 calc R . . C79 C 0.1599(3) 0.3697(9) 0.4257(4) 0.030(7) Uani 1 1 d GU . . C80 C 0.1632(3) 0.2897(8) 0.4220(4) 0.046(9) Uani 1 1 d GU . . H80A H 0.1687 0.2702 0.4024 0.055 Uiso 1 1 calc R . . C81 C 0.1582(5) 0.2427(16) 0.4481(9) 0.052(9) Uani 1 1 d U . . H81A H 0.1602 0.1901 0.4458 0.062 Uiso 1 1 calc R . . C82 C 0.1506(5) 0.2678(17) 0.4766(10) 0.067(11) Uani 1 1 d U . . H82A H 0.1472 0.2341 0.4941 0.081 Uiso 1 1 calc R . . C83 C 0.1479(6) 0.3461(19) 0.4793(11) 0.080(12) Uani 1 1 d U . . H83A H 0.1421 0.3649 0.4988 0.096 Uiso 1 1 calc R . . C84 C 0.1532(5) 0.3963(16) 0.4552(9) 0.058(10) Uani 1 1 d U . . H84A H 0.1522 0.4489 0.4589 0.070 Uiso 1 1 calc R . . C85 C 0.1965(5) 0.4636(14) 0.4137(9) 0.041(8) Uani 1 1 d U . . C86 C 0.2087(5) 0.4139(15) 0.4370(8) 0.044(9) Uani 1 1 d U . . H86A H 0.2032 0.3676 0.4434 0.053 Uiso 1 1 calc R . . C87 C 0.2293(5) 0.4334(17) 0.4507(9) 0.060(10) Uani 1 1 d U . . H87A H 0.2375 0.4001 0.4669 0.072 Uiso 1 1 calc R . . C88 C 0.2377(6) 0.4993(19) 0.4415(10) 0.078(12) Uani 1 1 d U . . H88A H 0.2515 0.5120 0.4514 0.094 Uiso 1 1 calc R . . C89 C 0.2259(5) 0.5463(17) 0.4177(10) 0.061(10) Uani 1 1 d U . . H89A H 0.2319 0.5915 0.4111 0.074 Uiso 1 1 calc R . . C90 C 0.2062(5) 0.5314(15) 0.4034(9) 0.052(9) Uani 1 1 d U . . H90A H 0.1986 0.5651 0.3865 0.062 Uiso 1 1 calc R . . C91 C 0.1389(4) 0.7199(13) 0.5266(9) 0.038(8) Uani 1 1 d U . . C92 C 0.1407(5) 0.7941(16) 0.5164(10) 0.067(11) Uani 1 1 d U . . H92A H 0.1452 0.8027 0.4943 0.081 Uiso 1 1 calc R . . C93 C 0.1366(5) 0.8569(17) 0.5357(10) 0.063(10) Uani 1 1 d U . . H93A H 0.1358 0.9058 0.5255 0.075 Uiso 1 1 calc R . . C94 C 0.1337(5) 0.8455(18) 0.5702(11) 0.072(11) Uani 1 1 d U . . H94A H 0.1329 0.8876 0.5853 0.086 Uiso 1 1 calc R . . C95 C 0.1321(5) 0.7742(18) 0.5832(11) 0.074(11) Uani 1 1 d U . . H95A H 0.1287 0.7679 0.6062 0.089 Uiso 1 1 calc R . . C96 C 0.1352(5) 0.7099(18) 0.5630(10) 0.069(11) Uani 1 1 d U . . H96A H 0.1350 0.6610 0.5730 0.083 Uiso 1 1 calc R . . C97 C 0.1752(5) 0.6252(14) 0.5158(9) 0.038(8) Uani 1 1 d U . . C98 C 0.1846(5) 0.6464(15) 0.5498(10) 0.051(9) Uani 1 1 d U . . H98A H 0.1766 0.6694 0.5652 0.062 Uiso 1 1 calc R . . C99 C 0.2060(6) 0.6345(18) 0.5620(11) 0.072(11) Uani 1 1 d U . . H99A H 0.2123 0.6525 0.5850 0.086 Uiso 1 1 calc R . . C100 C 0.2178(6) 0.5975(17) 0.5413(11) 0.066(11) Uani 1 1 d U . . H10B H 0.2318 0.5845 0.5495 0.079 Uiso 1 1 calc R . . C101 C 0.2072(6) 0.5812(18) 0.5074(12) 0.078(12) Uani 1 1 d U . . H10C H 0.2153 0.5612 0.4913 0.094 Uiso 1 1 calc R . . C102 C 0.1867(5) 0.5897(15) 0.4937(10) 0.055(10) Uani 1 1 d U . . H10D H 0.1808 0.5724 0.4704 0.066 Uiso 1 1 calc R . . C103 C 0.1340(5) 0.5523(13) 0.5182(8) 0.034(8) Uani 1 1 d U . . C104 C 0.1439(5) 0.5098(14) 0.5476(8) 0.045(9) Uani 1 1 d U . . H10E H 0.1575 0.5227 0.5590 0.054 Uiso 1 1 calc R . . C105 C 0.1336(5) 0.4466(15) 0.5604(9) 0.048(9) Uani 1 1 d U . . H10F H 0.1406 0.4166 0.5795 0.057 Uiso 1 1 calc R . . C106 C 0.1144(5) 0.4306(16) 0.5454(10) 0.058(10) Uani 1 1 d U . . H10G H 0.1075 0.3913 0.5554 0.070 Uiso 1 1 calc R . . C107 C 0.1040(5) 0.4689(17) 0.5158(10) 0.063(10) Uani 1 1 d U . . H10H H 0.0906 0.4534 0.5042 0.075 Uiso 1 1 calc R . . C108 C 0.1136(5) 0.5306(16) 0.5037(10) 0.060(10) Uani 1 1 d U . . H10I H 0.1062 0.5595 0.4846 0.073 Uiso 1 1 calc R . . C109 C 0.1733(4) 0.9672(13) 0.3847(8) 0.034(8) Uani 1 1 d U . . C110 C 0.1761(4) 1.0455(13) 0.3908(9) 0.043(8) Uani 1 1 d U . . H11B H 0.1740 1.0661 0.4130 0.052 Uiso 1 1 calc R . . C111 C 0.1817(5) 1.0933(17) 0.3650(10) 0.067(10) Uani 1 1 d U . . H11C H 0.1837 1.1454 0.3700 0.080 Uiso 1 1 calc R . . C112 C 0.1846(6) 1.0660(19) 0.3328(11) 0.080(12) Uani 1 1 d U . . H11D H 0.1881 1.0991 0.3152 0.096 Uiso 1 1 calc R . . C113 C 0.1822(5) 0.9883(16) 0.3258(10) 0.064(10) Uani 1 1 d U . . H11E H 0.1839 0.9681 0.3034 0.077 Uiso 1 1 calc R . . C114 C 0.1773(5) 0.9418(16) 0.3527(9) 0.054(9) Uani 1 1 d U . . H11F H 0.1768 0.8891 0.3485 0.065 Uiso 1 1 calc R . . C115 C 0.1909(4) 0.8734(13) 0.4490(8) 0.035(8) Uani 1 1 d U . . C116 C 0.2090(5) 0.9198(15) 0.4546(9) 0.044(9) Uani 1 1 d U . . H11G H 0.2088 0.9652 0.4413 0.053 Uiso 1 1 calc R . . C117 C 0.2260(5) 0.9022(16) 0.4775(9) 0.051(9) Uani 1 1 d U . . H11H H 0.2373 0.9361 0.4801 0.062 Uiso 1 1 calc R . . C118 C 0.2282(6) 0.8373(17) 0.4978(10) 0.067(11) Uani 1 1 d U . . H11I H 0.2406 0.8255 0.5139 0.080 Uiso 1 1 calc R . . C119 C 0.2115(5) 0.7915(18) 0.4932(10) 0.063(10) Uani 1 1 d U . . H11J H 0.2123 0.7458 0.5064 0.076 Uiso 1 1 calc R . . C120 C 0.1934(5) 0.8081(14) 0.4704(9) 0.044(9) Uani 1 1 d U . . H12B H 0.1822 0.7742 0.4691 0.052 Uiso 1 1 calc R . . C121 C 0.1533(5) 0.9652(12) 0.4502(8) 0.030(7) Uani 1 1 d U . . C122 C 0.1641(5) 1.0025(15) 0.4798(9) 0.057(10) Uani 1 1 d U . . H12C H 0.1786 0.9968 0.4859 0.068 Uiso 1 1 calc R . . C123 C 0.1535(5) 1.0503(16) 0.5019(10) 0.058(10) Uani 1 1 d U . . H12D H 0.1605 1.0729 0.5233 0.070 Uiso 1 1 calc R . . C124 C 0.1337(5) 1.0601(15) 0.4902(9) 0.055(9) Uani 1 1 d U . . H12E H 0.1270 1.0940 0.5037 0.066 Uiso 1 1 calc R . . C125 C 0.1210(7) 1.026(2) 0.4598(11) 0.092(13) Uani 1 1 d U . . H12F H 0.1066 1.0354 0.4540 0.110 Uiso 1 1 calc R . . C126 C 0.1315(6) 0.9771(19) 0.4384(11) 0.082(12) Uani 1 1 d U . . H12G H 0.1243 0.9535 0.4174 0.099 Uiso 1 1 calc R . . C127 C 0.2133(4) 0.7148(13) 0.3481(8) 0.032(8) Uani 1 1 d U . . C128 C 0.2329(5) 0.6874(15) 0.3439(10) 0.051(9) Uani 1 1 d U . . H12H H 0.2343 0.6598 0.3231 0.061 Uiso 1 1 calc R . . C129 C 0.2498(5) 0.7009(15) 0.3700(9) 0.050(9) Uani 1 1 d U . . H12I H 0.2629 0.6840 0.3666 0.060 Uiso 1 1 calc R . . C130 C 0.2482(5) 0.7368(16) 0.3997(10) 0.056(10) Uani 1 1 d U . . H13A H 0.2601 0.7451 0.4174 0.067 Uiso 1 1 calc R . . C131 C 0.2293(6) 0.7626(19) 0.4055(11) 0.081(12) Uani 1 1 d U . . H13B H 0.2285 0.7890 0.4269 0.098 Uiso 1 1 calc R . . C132 C 0.2113(5) 0.7498(15) 0.3799(9) 0.053(9) Uani 1 1 d U . . H13C H 0.1982 0.7648 0.3843 0.063 Uiso 1 1 calc R . . C133 C 0.1894(5) 0.7824(14) 0.2812(9) 0.039(8) Uani 1 1 d U . . C134 C 0.1710(6) 0.8059(17) 0.2608(10) 0.068(11) Uani 1 1 d U . . H13D H 0.1586 0.7812 0.2637 0.082 Uiso 1 1 calc R . . C135 C 0.1699(6) 0.863(2) 0.2365(11) 0.088(13) Uani 1 1 d U . . H13E H 0.1571 0.8769 0.2223 0.105 Uiso 1 1 calc R . . C136 C 0.1880(6) 0.901(2) 0.2331(11) 0.088(13) Uani 1 1 d U . . H13F H 0.1875 0.9427 0.2171 0.106 Uiso 1 1 calc R . . C137 C 0.2058(6) 0.8797(18) 0.2521(10) 0.074(11) Uani 1 1 d U . . H13G H 0.2181 0.9045 0.2490 0.089 Uiso 1 1 calc R . . C138 C 0.2068(6) 0.8203(17) 0.2769(10) 0.071(11) Uani 1 1 d U . . H13H H 0.2197 0.8065 0.2909 0.085 Uiso 1 1 calc R . . C139 C 0.1945(5) 0.6150(15) 0.2856(9) 0.044(9) Uani 1 1 d U . . C140 C 0.2062(5) 0.6215(17) 0.2582(10) 0.062(10) Uani 1 1 d U . . H14B H 0.2108 0.6692 0.2517 0.074 Uiso 1 1 calc R . . C141 C 0.2108(6) 0.556(2) 0.2409(11) 0.084(12) Uani 1 1 d U . . H14C H 0.2186 0.5605 0.2224 0.100 Uiso 1 1 calc R . . C142 C 0.2049(6) 0.487(2) 0.2490(11) 0.088(13) Uani 1 1 d U . . H14D H 0.2085 0.4438 0.2367 0.105 Uiso 1 1 calc R . . C143 C 0.1932(6) 0.4799(18) 0.2764(10) 0.068(11) Uani 1 1 d U . . H14E H 0.1884 0.4320 0.2823 0.081 Uiso 1 1 calc R . . C144 C 0.1887(4) 0.5439(15) 0.2944(10) 0.056(11) Uani 1 1 d . . . H14F H 0.1813 0.5386 0.3135 0.068 Uiso 1 1 calc R . . Li1 Li 0.0000 1.186(4) 0.2500 0.07(3) Uani 1 2 d S . . O1 O 0.0222(5) 1.2469(18) 0.2398(10) 0.133(11) Uani 1 1 d U . . C145 C 0.0219(11) 1.276(4) 0.2076(19) 0.21(2) Uani 1 1 d U . . H14G H 0.0091 1.3048 0.1990 0.257 Uiso 1 1 calc R . . H14H H 0.0239 1.2377 0.1898 0.257 Uiso 1 1 calc R . . C146 C 0.0421(10) 1.333(4) 0.2174(18) 0.19(2) Uani 1 1 d U . . H14I H 0.0551 1.3049 0.2172 0.232 Uiso 1 1 calc R . . H14J H 0.0412 1.3751 0.2003 0.232 Uiso 1 1 calc R . . C147 C 0.0410(12) 1.357(4) 0.251(2) 0.25(2) Uani 1 1 d U . . H14K H 0.0294 1.3923 0.2501 0.295 Uiso 1 1 calc R . . H14L H 0.0539 1.3820 0.2619 0.295 Uiso 1 1 calc R . . C148 C 0.0376(10) 1.287(4) 0.2700(19) 0.21(2) Uani 1 1 d U . . H14M H 0.0314 1.2977 0.2913 0.257 Uiso 1 1 calc R . . H14N H 0.0505 1.2583 0.2771 0.257 Uiso 1 1 calc R . . O2 O 0.0119(5) 1.1228(17) 0.2876(10) 0.128(11) Uani 1 1 d U . . C149 C 0.0331(13) 1.094(5) 0.289(2) 0.28(3) Uani 1 1 d U . . H14O H 0.0370 1.0891 0.2656 0.342 Uiso 1 1 calc R . . H14P H 0.0435 1.1242 0.3055 0.342 Uiso 1 1 calc R . . C150 C 0.0296(11) 1.022(4) 0.305(2) 0.21(2) Uani 1 1 d U . . H15B H 0.0243 0.9871 0.2848 0.251 Uiso 1 1 calc R . . H15C H 0.0431 1.0020 0.3169 0.251 Uiso 1 1 calc R . . C151 C 0.0177(12) 1.019(5) 0.326(2) 0.24(3) Uani 1 1 d U . . H15D H 0.0251 1.0158 0.3513 0.290 Uiso 1 1 calc R . . H15E H 0.0079 0.9767 0.3211 0.290 Uiso 1 1 calc R . . C152 C 0.0073(13) 1.095(5) 0.318(2) 0.27(3) Uani 1 1 d U . . H15F H -0.0078 1.0887 0.3153 0.328 Uiso 1 1 calc R . . H15G H 0.0119 1.1300 0.3380 0.328 Uiso 1 1 calc R . . Li2 Li -0.0278(11) 0.822(3) 0.467(2) 0.051(17) Uani 0.75 1 d PU . . O3 O -0.0647(8) 0.780(3) 0.4060(12) 0.107(16) Uani 0.50 1 d PDU . . C201 C -0.0555(9) 0.800(3) 0.3778(16) 0.071(9) Uani 0.50 1 d PDU . . H20B H -0.0599 0.8509 0.3696 0.086 Uiso 0.50 1 calc PR . . H20C H -0.0404 0.8000 0.3857 0.086 Uiso 0.50 1 calc PR . . C202 C -0.0600(10) 0.756(3) 0.3529(13) 0.072(9) Uani 0.50 1 d PDU . . H20D H -0.0474 0.7394 0.3446 0.086 Uiso 0.50 1 calc PR . . H20E H -0.0690 0.7814 0.3328 0.086 Uiso 0.50 1 calc PR . . C203 C -0.0696(10) 0.697(2) 0.3624(15) 0.071(9) Uani 0.50 1 d PDU . . H20F H -0.0817 0.6837 0.3439 0.086 Uiso 0.50 1 calc PR . . H20G H -0.0603 0.6529 0.3667 0.086 Uiso 0.50 1 calc PR . . C204 C -0.0752(9) 0.718(3) 0.3918(15) 0.072(9) Uani 0.50 1 d PDU . . H20H H -0.0729 0.6769 0.4094 0.086 Uiso 0.50 1 calc PR . . H20I H -0.0901 0.7300 0.3868 0.086 Uiso 0.50 1 calc PR . . O4 O 0.0732(7) 0.781(2) 0.0200(11) 0.073(13) Uani 0.50 1 d PDU . . C205 C 0.0931(7) 0.790(4) 0.0151(15) 0.085(10) Uani 0.50 1 d PDU . . H20J H 0.0974 0.8425 0.0205 0.101 Uiso 0.50 1 calc PR . . H20K H 0.1022 0.7569 0.0321 0.101 Uiso 0.50 1 calc PR . . C206 C 0.0952(8) 0.774(4) -0.0155(16) 0.084(10) Uani 0.50 1 d PDU . . H20L H 0.1080 0.7454 -0.0149 0.101 Uiso 0.50 1 calc PR . . H20M H 0.0961 0.8213 -0.0291 0.101 Uiso 0.50 1 calc PR . . C207 C 0.0794(10) 0.735(4) -0.0310(14) 0.084(10) Uani 0.50 1 d PDU . . H20N H 0.0741 0.7542 -0.0554 0.101 Uiso 0.50 1 calc PR . . H20O H 0.0832 0.6813 -0.0327 0.101 Uiso 0.50 1 calc PR . . C208 C 0.0659(7) 0.743(4) -0.0106(16) 0.085(10) Uani 0.50 1 d PDU . . H20P H 0.0612 0.6925 -0.0043 0.101 Uiso 0.50 1 calc PR . . H20Q H 0.0538 0.7699 -0.0239 0.101 Uiso 0.50 1 calc PR . . O5 O -0.0071(13) 0.926(3) 0.444(2) 0.20(2) Uani 0.50 1 d PDU . . C213 C -0.0176(12) 0.973(5) 0.418(2) 0.16(3) Uani 0.50 1 d PDU . . H21H H -0.0143 0.9585 0.3950 0.189 Uiso 0.50 1 calc PR . . H21I H -0.0326 0.9656 0.4171 0.189 Uiso 0.50 1 calc PR . . C214 C -0.0132(16) 1.039(4) 0.425(3) 0.22(3) Uani 0.50 1 d PDU . . H21J H -0.0245 1.0642 0.4337 0.265 Uiso 0.50 1 calc PR . . H21K H -0.0112 1.0641 0.4024 0.265 Uiso 0.50 1 calc PR . . C215 C 0.0037(16) 1.043(4) 0.449(3) 0.19(3) Uani 0.50 1 d PDU . . H21L H 0.0149 1.0661 0.4380 0.232 Uiso 0.50 1 calc PR . . H21M H 0.0015 1.0743 0.4692 0.232 Uiso 0.50 1 calc PR . . C216 C 0.0081(10) 0.975(5) 0.458(2) 0.13(2) Uani 0.50 1 d PDU . . H21N H 0.0105 0.9714 0.4847 0.152 Uiso 0.50 1 calc PR . . H21O H 0.0210 0.9594 0.4503 0.152 Uiso 0.50 1 calc PR . . O6 O 0.0676(7) 0.936(2) 0.0573(13) 0.083(8) Uani 0.50 1 d PDU . . C217 C 0.0689(9) 0.992(3) 0.0326(13) 0.083(8) Uani 0.50 1 d PDU . . H21P H 0.0692 0.9681 0.0090 0.100 Uiso 0.50 1 calc PR . . H21Q H 0.0565 1.0239 0.0300 0.100 Uiso 0.50 1 calc PR . . C218 C 0.0843(9) 1.030(3) 0.0413(16) 0.083(8) Uani 0.50 1 d PDU . . H21R H 0.0805 1.0844 0.0389 0.100 Uiso 0.50 1 calc PR . . H21S H 0.0942 1.0200 0.0252 0.100 Uiso 0.50 1 calc PR . . C219 C 0.0929(8) 1.016(3) 0.0744(16) 0.083(8) Uani 0.50 1 d PDU . . H21T H 0.1081 1.0157 0.0773 0.100 Uiso 0.50 1 calc PR . . H21U H 0.0887 1.0533 0.0910 0.100 Uiso 0.50 1 calc PR . . C220 C 0.0859(9) 0.950(3) 0.0796(14) 0.083(8) Uani 0.50 1 d PDU . . H22B H 0.0839 0.9453 0.1048 0.100 Uiso 0.50 1 calc PR . . H22C H 0.0961 0.9112 0.0756 0.100 Uiso 0.50 1 calc PR . . O7 O 0.0091(9) 0.680(2) 0.0436(14) 0.113(17) Uani 0.50 1 d PDU . . C221 C 0.0174(11) 0.610(3) 0.042(2) 0.12(2) Uani 0.50 1 d PDU . . H22D H 0.0141 0.5912 0.0174 0.143 Uiso 0.50 1 calc PR . . H22E H 0.0326 0.6139 0.0490 0.143 Uiso 0.50 1 calc PR . . C222 C 0.0111(11) 0.565(2) 0.0622(19) 0.09(2) Uani 0.50 1 d PDU . . H22F H 0.0229 0.5415 0.0781 0.110 Uiso 0.50 1 calc PR . . H22G H 0.0030 0.5255 0.0479 0.110 Uiso 0.50 1 calc PR . . C223 C -0.0004(9) 0.600(3) 0.0815(14) 0.059(12) Uani 0.50 1 d PDU . . H22H H -0.0133 0.5717 0.0818 0.071 Uiso 0.50 1 calc PR . . H22I H 0.0070 0.6070 0.1064 0.071 Uiso 0.50 1 calc PR . . C224 C -0.0043(8) 0.665(2) 0.0655(16) 0.059(12) Uani 0.50 1 d PDU . . H22J H -0.0036 0.7047 0.0838 0.071 Uiso 0.50 1 calc PR . . H22K H -0.0185 0.6639 0.0514 0.071 Uiso 0.50 1 calc PR . . O8 O -0.0089(12) 0.741(4) 0.5569(14) 0.17(2) Uani 0.50 1 d PDU . . C241 C 0.0055(12) 0.691(5) 0.573(2) 0.14(3) Uani 0.50 1 d PDU . . H24D H 0.0040 0.6430 0.5595 0.172 Uiso 0.50 1 calc PR . . H24E H 0.0194 0.7108 0.5731 0.172 Uiso 0.50 1 calc PR . . C242 C 0.0036(10) 0.678(3) 0.6042(18) 0.10(2) Uani 0.50 1 d PDU . . H24F H 0.0173 0.6783 0.6200 0.122 Uiso 0.50 1 calc PR . . H24G H -0.0027 0.6279 0.6058 0.122 Uiso 0.50 1 calc PR . . C243 C -0.0081(11) 0.730(4) 0.6146(15) 0.09(2) Uani 0.50 1 d PDU . . H24H H -0.0171 0.7084 0.6301 0.106 Uiso 0.50 1 calc PR . . H24I H 0.0003 0.7708 0.6276 0.106 Uiso 0.50 1 calc PR . . C244 C -0.0188(9) 0.754(4) 0.585(2) 0.11(2) Uani 0.50 1 d PDU . . H24J H -0.0213 0.8088 0.5865 0.138 Uiso 0.50 1 calc PR . . H24K H -0.0323 0.7284 0.5800 0.138 Uiso 0.50 1 calc PR . . Li3 Li 0.2483(9) 1.201(2) 0.3474(16) 0.017(12) Uani 0.75 1 d PU . . O9 O 0.2556(7) 1.3555(19) 0.3503(12) 0.080(13) Uani 0.50 1 d PDU . . C245 C 0.2679(8) 1.388(3) 0.3291(17) 0.080(10) Uani 0.50 1 d PDU . . H24L H 0.2818 1.3969 0.3435 0.095 Uiso 0.50 1 calc PR . . H24M H 0.2694 1.3530 0.3095 0.095 Uiso 0.50 1 calc PR . . C246 C 0.2607(10) 1.448(3) 0.3164(15) 0.080(10) Uani 0.50 1 d PDU . . H24N H 0.2531 1.4399 0.2917 0.095 Uiso 0.50 1 calc PR . . H24O H 0.2719 1.4844 0.3156 0.095 Uiso 0.50 1 calc PR . . C247 C 0.2482(10) 1.474(2) 0.3365(18) 0.079(10) Uani 0.50 1 d PDU . . H24P H 0.2553 1.5094 0.3547 0.095 Uiso 0.50 1 calc PR . . H24Q H 0.2362 1.4994 0.3220 0.095 Uiso 0.50 1 calc PR . . C248 C 0.2425(8) 1.414(3) 0.3516(17) 0.079(10) Uani 0.50 1 d PDU . . H24R H 0.2285 1.3988 0.3393 0.095 Uiso 0.50 1 calc PR . . H24S H 0.2418 1.4247 0.3768 0.095 Uiso 0.50 1 calc PR . . O10 O 0.2319(8) 1.182(3) 0.2787(11) 0.088(14) Uani 0.50 1 d PDU . . C249 C 0.2327(15) 1.235(3) 0.2532(17) 0.14(2) Uani 0.50 1 d PDU . . H24T H 0.2245 1.2796 0.2582 0.164 Uiso 0.50 1 calc PR . . H24U H 0.2471 1.2520 0.2546 0.164 Uiso 0.50 1 calc PR . . C250 C 0.2260(15) 1.212(4) 0.2231(14) 0.13(2) Uani 0.50 1 d PDU . . H25A H 0.2362 1.2222 0.2075 0.159 Uiso 0.50 1 calc PR . . H25B H 0.2132 1.2397 0.2130 0.159 Uiso 0.50 1 calc PR . . C251 C 0.2223(15) 1.141(4) 0.2237(15) 0.14(2) Uani 0.50 1 d PDU . . H25C H 0.2082 1.1292 0.2106 0.168 Uiso 0.50 1 calc PR . . H25D H 0.2323 1.1118 0.2127 0.168 Uiso 0.50 1 calc PR . . C252 C 0.2240(13) 1.124(3) 0.2574(17) 0.11(2) Uani 0.50 1 d PDU . . H25E H 0.2330 1.0795 0.2628 0.126 Uiso 0.50 1 calc PR . . H25F H 0.2103 1.1110 0.2625 0.126 Uiso 0.50 1 calc PR . . O11 O 0.2388(6) 1.152(2) 0.4233(11) 0.065(12) Uani 0.50 1 d PDU . . C253 C 0.2267(10) 1.212(2) 0.4287(16) 0.078(10) Uani 0.50 1 d PDU . . H25G H 0.2351 1.2584 0.4309 0.094 Uiso 0.50 1 calc PR . . H25H H 0.2156 1.2176 0.4076 0.094 Uiso 0.50 1 calc PR . . C254 C 0.2190(10) 1.205(3) 0.4555(16) 0.078(10) Uani 0.50 1 d PDU . . H25I H 0.2040 1.2134 0.4494 0.094 Uiso 0.50 1 calc PR . . H25J H 0.2250 1.2422 0.4737 0.094 Uiso 0.50 1 calc PR . . C255 C 0.2225(10) 1.137(3) 0.4687(15) 0.078(10) Uani 0.50 1 d PDU . . H25K H 0.2280 1.1391 0.4947 0.094 Uiso 0.50 1 calc PR . . H25L H 0.2097 1.1066 0.4646 0.094 Uiso 0.50 1 calc PR . . C256 C 0.2360(10) 1.109(3) 0.4515(15) 0.078(10) Uani 0.50 1 d PDU . . H25M H 0.2316 1.0583 0.4428 0.093 Uiso 0.50 1 calc PR . . H25N H 0.2493 1.1041 0.4682 0.093 Uiso 0.50 1 calc PR . . O12 O 0.2523(6) 1.0329(17) 0.3690(11) 0.055(11) Uani 0.50 1 d PDU . . C261 C 0.2388(8) 0.977(3) 0.3733(16) 0.083(10) Uani 0.50 1 d PDU . . H26D H 0.2428 0.9548 0.3974 0.100 Uiso 0.50 1 calc PR . . H26E H 0.2248 0.9988 0.3715 0.100 Uiso 0.50 1 calc PR . . C262 C 0.2384(9) 0.928(3) 0.3508(18) 0.083(10) Uani 0.50 1 d PDU . . H26F H 0.2259 0.9333 0.3321 0.100 Uiso 0.50 1 calc PR . . H26G H 0.2378 0.8777 0.3622 0.100 Uiso 0.50 1 calc PR . . C263 C 0.2547(10) 0.932(3) 0.3362(17) 0.083(10) Uani 0.50 1 d PDU . . H26H H 0.2645 0.8908 0.3450 0.100 Uiso 0.50 1 calc PR . . H26I H 0.2510 0.9283 0.3098 0.100 Uiso 0.50 1 calc PR . . C264 C 0.2625(9) 0.997(3) 0.3461(17) 0.083(10) Uani 0.50 1 d PDU . . H26J H 0.2622 1.0287 0.3246 0.100 Uiso 0.50 1 calc PR . . H26K H 0.2771 0.9904 0.3577 0.100 Uiso 0.50 1 calc PR . . O13 O 0.2848(8) 1.146(4) 0.4092(14) 0.126(18) Uani 0.50 1 d PDU . . C265 C 0.2987(13) 1.098(3) 0.429(2) 0.14(2) Uani 0.50 1 d PDU . . H26L H 0.2920 1.0486 0.4314 0.165 Uiso 0.50 1 calc PR . . H26M H 0.3102 1.0886 0.4158 0.165 Uiso 0.50 1 calc PR . . C266 C 0.3055(13) 1.123(5) 0.4583(18) 0.14(2) Uani 0.50 1 d PDU . . H26N H 0.3206 1.1148 0.4643 0.165 Uiso 0.50 1 calc PR . . H26O H 0.2991 1.0975 0.4766 0.165 Uiso 0.50 1 calc PR . . C267 C 0.3017(15) 1.195(5) 0.459(2) 0.17(3) Uani 0.50 1 d PDU . . H26P H 0.2941 1.2078 0.4783 0.206 Uiso 0.50 1 calc PR . . H26Q H 0.3147 1.2248 0.4625 0.206 Uiso 0.50 1 calc PR . . C268 C 0.2906(16) 1.209(3) 0.428(2) 0.19(3) Uani 0.50 1 d PDU . . H26R H 0.2986 1.2412 0.4138 0.234 Uiso 0.50 1 calc PR . . H26S H 0.2782 1.2380 0.4309 0.234 Uiso 0.50 1 calc PR . . O14 O 0.0874(6) 0.644(2) 0.6180(14) 0.106(16) Uani 0.50 1 d PDU . . C209 C 0.0667(7) 0.635(2) 0.6170(16) 0.042(15) Uani 0.50 1 d PDU . . H20R H 0.0639 0.6384 0.6416 0.051 Uiso 0.50 1 calc PR . . H20S H 0.0592 0.6763 0.6028 0.051 Uiso 0.50 1 calc PR . . C210 C 0.0605(6) 0.575(3) 0.6039(18) 0.066(18) Uani 0.50 1 d PDU . . H21B H 0.0504 0.5834 0.5815 0.080 Uiso 0.50 1 calc PR . . H21C H 0.0533 0.5471 0.6207 0.080 Uiso 0.50 1 calc PR . . C211 C 0.0757(7) 0.5342(18) 0.5970(15) 0.035(14) Uani 0.50 1 d PDU . . H21D H 0.0795 0.4943 0.6151 0.042 Uiso 0.50 1 calc PR . . H21E H 0.0722 0.5108 0.5730 0.042 Uiso 0.50 1 calc PR . . C212 C 0.0907(6) 0.583(2) 0.5981(15) 0.049(15) Uani 0.50 1 d PDU . . H21F H 0.0916 0.5987 0.5735 0.059 Uiso 0.50 1 calc PR . . H21G H 0.1039 0.5584 0.6087 0.059 Uiso 0.50 1 calc PR . . O15 O 0.1554(7) 1.084(3) 0.2324(12) 0.102(16) Uani 0.50 1 d PDU . . C225 C 0.1370(8) 1.121(3) 0.2273(13) 0.051(16) Uani 0.50 1 d PDU . . H22L H 0.1273 1.0936 0.2396 0.061 Uiso 0.50 1 calc PR . . H22M H 0.1391 1.1720 0.2383 0.061 Uiso 0.50 1 calc PR . . C226 C 0.1295(6) 1.128(2) 0.1955(14) 0.027(13) Uani 0.50 1 d PDU . . H22N H 0.1242 1.1794 0.1906 0.032 Uiso 0.50 1 calc PR . . H22O H 0.1179 1.0922 0.1891 0.032 Uiso 0.50 1 calc PR . . C227 C 0.1434(9) 1.114(3) 0.1761(11) 0.052(16) Uani 0.50 1 d PDU . . H22P H 0.1379 1.0793 0.1561 0.062 Uiso 0.50 1 calc PR . . H22Q H 0.1481 1.1606 0.1662 0.062 Uiso 0.50 1 calc PR . . C228 C 0.1583(8) 1.082(4) 0.1980(15) 0.11(2) Uani 0.50 1 d PDU . . H22R H 0.1714 1.1078 0.1963 0.136 Uiso 0.50 1 calc PR . . H22S H 0.1596 1.0289 0.1907 0.136 Uiso 0.50 1 calc PR . . O16 O 0.0423(6) 0.881(3) 0.6520(17) 0.142(19) Uani 0.50 1 d PDU . . C237 C 0.0567(10) 0.840(3) 0.6384(15) 0.09(2) Uani 0.50 1 d PDU . . H23P H 0.0522 0.7873 0.6355 0.106 Uiso 0.50 1 calc PR . . H23Q H 0.0579 0.8602 0.6145 0.106 Uiso 0.50 1 calc PR . . C238 C 0.0735(8) 0.843(3) 0.6582(17) 0.063(17) Uani 0.50 1 d PDU . . H23R H 0.0844 0.8525 0.6439 0.075 Uiso 0.50 1 calc PR . . H23S H 0.0764 0.7949 0.6709 0.075 Uiso 0.50 1 calc PR . . C239 C 0.0737(8) 0.898(4) 0.6815(17) 0.09(2) Uani 0.50 1 d PDU . . H23T H 0.0763 0.8775 0.7063 0.112 Uiso 0.50 1 calc PR . . H23U H 0.0845 0.9351 0.6793 0.112 Uiso 0.50 1 calc PR . . C240 C 0.0555(9) 0.927(3) 0.6737(19) 0.10(2) Uani 0.50 1 d PDU . . H24B H 0.0564 0.9763 0.6617 0.126 Uiso 0.50 1 calc PR . . H24C H 0.0502 0.9368 0.6960 0.126 Uiso 0.50 1 calc PR . . O17 O 0.1555(7) 0.396(3) 0.1676(15) 0.115(17) Uani 0.50 1 d PDU . . C257 C 0.1626(9) 0.340(4) 0.1914(16) 0.10(2) Uani 0.50 1 d PDU . . H25O H 0.1655 0.3612 0.2159 0.120 Uiso 0.50 1 calc PR . . H25P H 0.1518 0.3011 0.1907 0.120 Uiso 0.50 1 calc PR . . C258 C 0.1783(8) 0.311(2) 0.1846(15) 0.050(16) Uani 0.50 1 d PDU . . H25Q H 0.1755 0.2575 0.1782 0.060 Uiso 0.50 1 calc PR . . H25R H 0.1893 0.3129 0.2061 0.060 Uiso 0.50 1 calc PR . . C259 C 0.1843(8) 0.346(3) 0.1582(16) 0.076(19) Uani 0.50 1 d PDU . . H25S H 0.1990 0.3600 0.1647 0.091 Uiso 0.50 1 calc PR . . H25T H 0.1823 0.3139 0.1365 0.091 Uiso 0.50 1 calc PR . . C260 C 0.1727(10) 0.405(3) 0.1531(18) 0.11(2) Uani 0.50 1 d PDU . . H26B H 0.1687 0.4148 0.1271 0.136 Uiso 0.50 1 calc PR . . H26C H 0.1805 0.4495 0.1641 0.136 Uiso 0.50 1 calc PR . . O18 O 0.2989(9) 0.526(2) 0.4090(15) 0.130(18) Uani 0.50 1 d PDU . . C269 C 0.3020(12) 0.587(3) 0.4320(13) 0.10(2) Uani 0.50 1 d PDU . . H26T H 0.2894 0.5953 0.4420 0.115 Uiso 0.50 1 calc PR . . H26U H 0.3133 0.5744 0.4521 0.115 Uiso 0.50 1 calc PR . . C270 C 0.3064(12) 0.644(2) 0.4172(15) 0.08(2) Uani 0.50 1 d PDU . . H27B H 0.3190 0.6666 0.4313 0.101 Uiso 0.50 1 calc PR . . H27C H 0.2950 0.6810 0.4161 0.101 Uiso 0.50 1 calc PR . . C271 C 0.3093(9) 0.629(2) 0.3849(14) 0.047(15) Uani 0.50 1 d PDU . . H27D H 0.2997 0.6585 0.3669 0.056 Uiso 0.50 1 calc PR . . H27E H 0.3236 0.6408 0.3824 0.056 Uiso 0.50 1 calc PR . . C272 C 0.3056(11) 0.558(2) 0.3809(13) 0.071(18) Uani 0.50 1 d PDU . . H27F H 0.3184 0.5319 0.3774 0.085 Uiso 0.50 1 calc PR . . H27G H 0.2952 0.5498 0.3590 0.085 Uiso 0.50 1 calc PR . . O19 O 0.1363(7) 0.849(3) 0.0804(15) 0.124(18) Uani 0.50 1 d PDU . . C273 C 0.1460(10) 0.782(2) 0.090(2) 0.10(2) Uani 0.50 1 d PDU . . H27H H 0.1365 0.7481 0.0994 0.116 Uiso 0.50 1 calc PR . . H27I H 0.1494 0.7581 0.0679 0.116 Uiso 0.50 1 calc PR . . C274 C 0.1618(11) 0.790(3) 0.112(2) 0.17(3) Uani 0.50 1 d PDU . . H27J H 0.1730 0.7589 0.1050 0.199 Uiso 0.50 1 calc PR . . H27K H 0.1595 0.7723 0.1356 0.199 Uiso 0.50 1 calc PR . . C275 C 0.1672(8) 0.860(4) 0.114(2) 0.11(2) Uani 0.50 1 d PDU . . H27L H 0.1717 0.8765 0.1388 0.135 Uiso 0.50 1 calc PR . . H27M H 0.1785 0.8698 0.1003 0.135 Uiso 0.50 1 calc PR . . C276 C 0.1505(10) 0.896(2) 0.099(2) 0.09(2) Uani 0.50 1 d PDU . . H27N H 0.1542 0.9351 0.0826 0.110 Uiso 0.50 1 calc PR . . H27O H 0.1446 0.9214 0.1179 0.110 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0415(16) 0.0222(9) 0.051(2) -0.0067(10) 0.0174(16) -0.0070(9) In2 0.0430(16) 0.0211(9) 0.053(2) 0.0006(10) 0.0212(16) 0.0016(9) In3 0.0560(18) 0.0244(10) 0.0396(19) 0.0030(10) 0.0128(17) 0.0082(10) In4 0.0528(17) 0.0257(10) 0.0376(19) -0.0030(10) 0.0135(16) -0.0057(10) In5 0.0522(17) 0.0243(10) 0.047(2) 0.0034(10) 0.0149(17) 0.0084(10) In6 0.0537(17) 0.0239(10) 0.0371(19) -0.0015(10) 0.0086(16) -0.0037(10) In7 0.0461(17) 0.0235(9) 0.0426(19) -0.0061(10) 0.0153(16) -0.0105(9) In8 0.0395(16) 0.0245(9) 0.053(2) -0.0041(10) 0.0209(16) -0.0031(9) Si1 0.054(7) 0.022(4) 0.049(8) -0.011(4) 0.022(7) -0.007(4) Si2 0.049(7) 0.018(4) 0.065(8) -0.005(4) 0.021(7) 0.000(4) Si3 0.058(7) 0.029(4) 0.047(8) 0.002(4) 0.018(7) 0.006(4) Si4 0.050(7) 0.028(4) 0.046(8) -0.007(4) 0.020(7) -0.009(4) Si5 0.050(7) 0.020(4) 0.046(7) 0.002(4) 0.018(6) 0.009(4) Si6 0.048(7) 0.034(4) 0.035(7) 0.001(4) 0.001(7) 0.000(4) Si7 0.044(6) 0.026(4) 0.040(7) -0.009(4) 0.022(6) -0.008(4) Si8 0.055(7) 0.033(4) 0.048(8) -0.004(4) 0.027(7) -0.001(4) C1 0.040(11) 0.038(10) 0.044(12) -0.008(8) 0.007(9) -0.007(8) C2 0.038(11) 0.028(9) 0.040(12) -0.003(8) -0.001(9) -0.002(8) C3 0.060(13) 0.051(11) 0.059(13) -0.001(9) 0.008(9) -0.003(8) C4 0.068(13) 0.057(11) 0.064(13) -0.001(9) 0.016(9) 0.004(9) C5 0.065(13) 0.065(12) 0.072(14) 0.003(9) 0.006(9) 0.008(9) C6 0.063(13) 0.053(11) 0.059(13) -0.006(9) 0.011(9) -0.004(9) C7 0.047(12) 0.041(10) 0.049(12) -0.003(8) 0.014(9) 0.004(8) C8 0.041(12) 0.045(10) 0.045(12) -0.001(8) 0.005(9) -0.007(8) C9 0.063(13) 0.066(12) 0.066(14) -0.002(9) 0.008(9) -0.005(9) C10 0.054(13) 0.065(12) 0.058(13) 0.001(9) 0.011(9) -0.003(9) C11 0.077(14) 0.082(13) 0.074(15) 0.003(9) 0.017(9) -0.004(9) C12 0.074(14) 0.073(13) 0.073(14) 0.001(9) 0.013(9) 0.000(9) C13 0.037(11) 0.039(10) 0.040(12) -0.002(8) 0.009(9) 0.002(8) C14 0.043(12) 0.038(10) 0.041(12) 0.005(8) 0.011(9) -0.008(8) C15 0.063(13) 0.056(11) 0.058(13) -0.003(9) 0.016(9) -0.003(9) C16 0.079(14) 0.079(13) 0.078(15) 0.000(9) 0.020(9) 0.001(9) C17 0.065(13) 0.064(12) 0.065(14) 0.006(9) 0.012(9) -0.003(9) C18 0.050(12) 0.050(11) 0.051(13) -0.002(8) 0.012(9) -0.003(8) C19 0.023(11) 0.017(8) 0.021(11) -0.002(8) 0.000(9) 0.000(8) C20 0.044(12) 0.035(10) 0.034(12) 0.009(8) 0.005(9) 0.001(8) C21 0.056(13) 0.058(11) 0.060(13) 0.001(9) 0.015(9) -0.001(9) C22 0.054(13) 0.053(11) 0.050(13) 0.000(8) 0.007(9) -0.007(9) C23 0.068(14) 0.070(12) 0.067(14) -0.004(9) 0.011(9) -0.001(9) C24 0.048(12) 0.050(11) 0.046(13) 0.004(8) 0.014(9) 0.000(8) C25 0.048(12) 0.044(10) 0.044(12) -0.004(8) 0.008(9) -0.003(8) C26 0.037(11) 0.034(10) 0.041(12) 0.002(8) 0.008(9) -0.001(8) C27 0.058(13) 0.052(11) 0.065(13) -0.004(9) 0.009(9) 0.000(9) C28 0.056(13) 0.058(11) 0.059(13) 0.003(9) 0.006(9) -0.002(9) C29 0.054(13) 0.058(11) 0.057(13) -0.002(9) 0.005(9) 0.005(9) C30 0.042(12) 0.040(10) 0.041(12) -0.011(8) 0.007(9) 0.002(8) C31 0.013(10) 0.016(8) 0.016(11) 0.005(7) 0.002(9) 0.004(7) C32 0.047(12) 0.039(10) 0.045(12) 0.002(8) 0.010(9) 0.000(8) C33 0.068(13) 0.061(12) 0.068(14) -0.008(9) 0.016(9) -0.003(9) C34 0.067(13) 0.060(12) 0.063(13) 0.005(9) 0.013(9) -0.002(9) C35 0.065(13) 0.064(12) 0.065(13) 0.002(9) 0.014(9) -0.008(9) C36 0.058(12) 0.050(11) 0.053(13) -0.004(8) 0.012(9) -0.001(8) C37 0.045(12) 0.043(10) 0.046(12) 0.008(8) 0.008(9) 0.005(8) C38 0.047(12) 0.051(11) 0.046(13) 0.004(8) 0.010(9) 0.001(8) C39 0.079(15) 0.078(13) 0.076(15) 0.003(9) 0.012(9) 0.003(9) C40 0.061(13) 0.063(12) 0.065(14) -0.002(9) 0.009(9) 0.001(9) C41 0.071(14) 0.076(13) 0.074(14) -0.001(9) 0.015(9) 0.002(9) C42 0.068(14) 0.073(13) 0.067(14) -0.002(9) 0.012(9) -0.002(9) C43 0.037(11) 0.031(9) 0.034(12) -0.002(8) 0.006(9) 0.001(8) C44 0.050(12) 0.046(10) 0.052(13) -0.001(8) 0.011(9) -0.002(8) C45 0.070(14) 0.078(13) 0.078(14) -0.002(9) 0.007(9) -0.006(9) C46 0.069(13) 0.062(12) 0.063(14) -0.005(9) 0.013(9) 0.005(9) C47 0.046(12) 0.047(10) 0.051(12) -0.001(8) 0.012(9) 0.001(8) C48 0.045(12) 0.041(10) 0.045(12) 0.004(8) 0.006(9) -0.002(8) C49 0.042(11) 0.035(10) 0.038(12) 0.001(8) 0.006(9) 0.005(8) C50 0.062(13) 0.058(12) 0.058(13) -0.001(9) 0.012(9) -0.002(9) C51 0.095(16) 0.089(15) 0.090(16) 0.007(9) 0.015(9) -0.004(9) C52 0.080(14) 0.083(13) 0.076(15) -0.004(9) 0.020(9) 0.000(9) C53 0.075(14) 0.071(13) 0.073(14) -0.003(9) 0.013(9) 0.003(9) C54 0.050(12) 0.045(10) 0.044(12) 0.000(8) 0.013(9) -0.002(8) C55 0.039(11) 0.032(9) 0.029(12) -0.001(8) 0.007(9) -0.003(8) C56 0.046(12) 0.046(10) 0.052(12) -0.006(8) 0.008(9) 0.000(8) C57 0.053(12) 0.050(11) 0.055(13) -0.001(9) 0.004(9) 0.003(9) C58 0.053(13) 0.062(12) 0.059(13) 0.004(9) 0.009(9) 0.000(9) C59 0.053(12) 0.048(11) 0.048(13) 0.002(8) 0.011(9) -0.006(8) C60 0.061(13) 0.060(12) 0.064(13) -0.001(9) 0.015(9) -0.006(9) C61 0.052(12) 0.049(11) 0.050(13) -0.006(9) 0.007(9) -0.002(8) C62 0.046(12) 0.044(10) 0.047(12) -0.002(8) 0.006(9) -0.003(8) C63 0.053(12) 0.051(11) 0.052(13) 0.005(8) 0.016(9) -0.004(8) C64 0.064(13) 0.060(11) 0.061(13) -0.001(9) 0.013(9) -0.002(9) C65 0.071(13) 0.062(12) 0.069(14) 0.002(9) 0.012(9) 0.000(9) C66 0.047(12) 0.040(10) 0.043(12) -0.003(8) 0.006(9) -0.002(8) C67 0.030(11) 0.029(9) 0.027(11) -0.013(8) 0.006(9) 0.004(8) C68 0.076(14) 0.076(13) 0.072(14) -0.004(9) 0.018(9) -0.003(9) C69 0.107(18) 0.112(17) 0.110(18) -0.002(9) 0.021(10) -0.009(9) C70 0.068(14) 0.075(13) 0.070(14) -0.001(9) 0.019(9) 0.005(9) C71 0.060(13) 0.060(11) 0.056(13) -0.006(9) 0.014(9) -0.002(9) C72 0.057(13) 0.055(11) 0.055(13) -0.001(9) 0.011(9) -0.004(8) C73 0.028(11) 0.032(9) 0.030(12) -0.001(8) 0.001(9) 0.004(8) C74 0.058(13) 0.055(11) 0.058(13) -0.003(9) 0.013(9) 0.008(9) C75 0.051(12) 0.048(11) 0.055(13) 0.000(8) 0.011(9) 0.003(8) C76 0.092(15) 0.084(14) 0.086(15) -0.002(9) 0.017(9) 0.001(9) C77 0.079(15) 0.084(14) 0.084(15) -0.005(9) 0.013(9) 0.003(9) C78 0.066(14) 0.070(12) 0.069(14) -0.012(9) 0.009(9) 0.003(9) C79 0.029(11) 0.029(9) 0.032(11) 0.003(8) 0.006(9) -0.001(8) C80 0.051(12) 0.042(10) 0.048(12) 0.000(8) 0.016(9) 0.003(8) C81 0.053(12) 0.048(11) 0.054(13) 0.004(9) 0.010(9) -0.002(8) C82 0.072(13) 0.062(12) 0.071(14) 0.008(9) 0.021(9) 0.000(9) C83 0.083(14) 0.078(13) 0.081(15) 0.000(9) 0.019(9) -0.001(9) C84 0.064(13) 0.052(11) 0.059(13) -0.001(9) 0.013(9) 0.000(8) C85 0.044(12) 0.039(10) 0.043(12) -0.004(8) 0.013(9) 0.003(8) C86 0.044(12) 0.042(10) 0.045(12) 0.001(8) 0.004(9) 0.003(8) C87 0.062(13) 0.060(12) 0.058(13) -0.003(9) 0.009(9) 0.008(9) C88 0.076(14) 0.078(13) 0.079(15) -0.007(9) 0.010(9) -0.001(9) C89 0.062(13) 0.059(12) 0.064(13) -0.001(9) 0.015(9) -0.005(9) C90 0.052(12) 0.051(11) 0.054(13) -0.001(8) 0.014(9) 0.001(8) C91 0.040(11) 0.032(9) 0.041(12) 0.009(8) 0.004(9) 0.001(8) C92 0.071(13) 0.061(12) 0.070(14) -0.008(9) 0.014(9) 0.002(9) C93 0.063(13) 0.061(12) 0.065(13) -0.005(9) 0.014(9) 0.000(9) C94 0.074(14) 0.070(13) 0.071(14) -0.006(9) 0.010(9) 0.003(9) C95 0.074(14) 0.076(13) 0.073(14) -0.005(9) 0.013(9) 0.003(9) C96 0.074(14) 0.066(12) 0.068(14) -0.006(9) 0.014(9) -0.001(9) C97 0.041(12) 0.041(10) 0.033(12) 0.003(8) 0.009(9) 0.002(8) C98 0.050(12) 0.051(11) 0.053(13) 0.002(9) 0.010(9) -0.001(8) C99 0.072(14) 0.071(13) 0.070(14) 0.003(9) 0.011(9) -0.001(9) C100 0.063(13) 0.069(12) 0.067(14) 0.000(9) 0.013(9) 0.003(9) C101 0.078(15) 0.080(13) 0.077(15) -0.007(9) 0.017(9) 0.006(9) C102 0.055(13) 0.056(11) 0.053(13) -0.002(9) 0.007(9) 0.008(9) C103 0.040(11) 0.033(9) 0.030(12) -0.005(8) 0.008(9) 0.002(8) C104 0.049(12) 0.043(10) 0.044(12) 0.004(8) 0.009(9) -0.002(8) C105 0.052(12) 0.048(10) 0.043(12) 0.008(8) 0.010(9) -0.001(8) C106 0.059(13) 0.058(11) 0.060(13) 0.002(9) 0.016(9) -0.005(9) C107 0.060(13) 0.064(12) 0.064(13) -0.001(9) 0.011(9) -0.007(9) C108 0.063(13) 0.059(11) 0.059(13) 0.006(9) 0.011(9) 0.002(9) C109 0.038(11) 0.030(9) 0.034(12) -0.008(8) 0.002(9) -0.005(8) C110 0.049(12) 0.038(10) 0.045(12) 0.006(8) 0.013(9) -0.008(8) C111 0.077(13) 0.056(12) 0.067(13) 0.008(9) 0.016(9) -0.006(9) C112 0.080(14) 0.079(13) 0.080(15) 0.006(9) 0.017(9) -0.008(9) C113 0.067(13) 0.062(12) 0.064(13) 0.000(9) 0.013(9) 0.000(9) C114 0.057(12) 0.054(11) 0.053(13) -0.002(9) 0.018(9) 0.004(8) C115 0.039(11) 0.033(9) 0.034(12) -0.004(8) 0.005(9) 0.003(8) C116 0.046(12) 0.045(10) 0.042(12) 0.000(8) 0.012(9) 0.004(8) C117 0.051(12) 0.051(11) 0.052(13) -0.002(9) 0.011(9) -0.002(8) C118 0.069(13) 0.067(12) 0.065(14) -0.001(9) 0.014(9) 0.005(9) C119 0.061(13) 0.067(12) 0.061(14) 0.006(9) 0.009(9) -0.003(9) C120 0.042(12) 0.044(10) 0.043(12) 0.000(8) 0.004(9) -0.006(8) C121 0.034(11) 0.026(9) 0.028(11) -0.004(8) 0.003(9) -0.002(8) C122 0.056(13) 0.056(11) 0.057(13) -0.001(9) 0.010(9) 0.001(9) C123 0.062(13) 0.056(11) 0.057(13) -0.004(9) 0.011(9) -0.006(9) C124 0.058(13) 0.048(11) 0.058(13) -0.002(9) 0.007(9) 0.006(8) C125 0.091(15) 0.091(15) 0.094(16) 0.000(9) 0.018(9) 0.003(9) C126 0.083(15) 0.081(14) 0.085(15) -0.005(9) 0.022(9) -0.001(9) C127 0.033(11) 0.031(9) 0.032(12) -0.005(8) 0.009(9) 0.001(8) C128 0.048(12) 0.053(11) 0.051(13) -0.003(8) 0.007(9) -0.002(8) C129 0.045(12) 0.053(11) 0.051(13) -0.003(9) 0.008(9) -0.001(8) C130 0.051(13) 0.059(11) 0.058(13) -0.001(9) 0.010(9) -0.003(9) C131 0.082(15) 0.079(13) 0.083(15) -0.009(9) 0.016(9) 0.003(9) C132 0.054(12) 0.054(11) 0.050(13) 0.001(9) 0.011(9) 0.002(8) C133 0.039(11) 0.040(10) 0.038(12) -0.005(8) 0.011(9) -0.005(8) C134 0.070(14) 0.065(12) 0.071(14) 0.011(9) 0.015(9) 0.001(9) C135 0.089(15) 0.085(14) 0.089(15) 0.004(9) 0.015(9) 0.007(9) C136 0.088(15) 0.088(14) 0.088(16) 0.006(9) 0.016(9) 0.005(9) C137 0.071(14) 0.077(13) 0.074(14) 0.007(9) 0.015(9) -0.003(9) C138 0.071(14) 0.071(12) 0.072(14) 0.005(9) 0.018(9) -0.005(9) C139 0.040(12) 0.047(11) 0.046(12) -0.006(8) 0.007(9) -0.002(8) C140 0.063(13) 0.062(12) 0.060(13) -0.006(9) 0.009(9) 0.001(9) C141 0.084(15) 0.087(14) 0.081(15) -0.005(9) 0.019(9) 0.007(9) C142 0.089(15) 0.086(14) 0.087(15) -0.007(9) 0.016(9) 0.002(9) C143 0.072(14) 0.063(12) 0.070(14) -0.001(9) 0.014(9) 0.003(9) C144 0.03(2) 0.050(18) 0.08(3) -0.014(19) 0.00(2) 0.036(16) Li1 0.07(6) 0.06(5) 0.08(8) 0.000 0.03(7) 0.000 O1 0.133(11) 0.133(11) 0.133(11) 0.0001(10) 0.024(2) -0.0002(10) C145 0.21(2) 0.21(2) 0.21(2) 0.0000(10) 0.039(4) -0.0001(10) C146 0.19(2) 0.19(2) 0.19(2) 0.0000(10) 0.035(4) -0.0001(10) C147 0.25(2) 0.25(2) 0.25(2) 0.0000(10) 0.045(5) 0.0000(10) C148 0.21(2) 0.21(2) 0.21(2) 0.0000(10) 0.039(4) 0.0000(10) O2 0.128(11) 0.128(11) 0.128(11) 0.0001(10) 0.023(2) 0.0001(10) C149 0.28(3) 0.28(3) 0.28(3) 0.0000(10) 0.052(5) 0.0000(10) C150 0.21(2) 0.21(2) 0.21(2) 0.0000(10) 0.038(4) 0.0001(10) C151 0.24(3) 0.24(3) 0.24(3) 0.0001(10) 0.044(5) 0.0000(10) C152 0.27(3) 0.27(3) 0.27(3) 0.0000(10) 0.050(5) 0.0001(10) Li2 0.051(17) 0.051(17) 0.051(17) 0.0000(10) 0.009(3) 0.0000(10) O3 0.107(16) 0.107(16) 0.107(16) -0.0001(10) 0.020(3) 0.0000(10) C201 0.071(9) 0.071(9) 0.071(9) 0.0000(10) 0.0130(19) 0.0000(10) C202 0.072(9) 0.072(9) 0.071(9) 0.0000(9) 0.0131(19) 0.0000(9) C203 0.071(9) 0.071(9) 0.071(9) 0.0000(9) 0.0131(19) 0.0000(9) C204 0.072(9) 0.072(9) 0.072(9) 0.0000(10) 0.0131(19) 0.0000(10) O4 0.073(13) 0.073(13) 0.073(13) -0.0001(10) 0.013(3) -0.0001(10) C205 0.084(10) 0.085(10) 0.084(10) 0.0000(10) 0.015(2) 0.0000(10) C206 0.084(10) 0.084(10) 0.084(10) 0.0000(9) 0.015(2) 0.0000(9) C207 0.084(10) 0.084(10) 0.084(10) 0.0000(9) 0.015(2) 0.0000(9) C208 0.085(10) 0.085(10) 0.085(10) -0.0001(10) 0.015(2) -0.0001(10) O5 0.20(2) 0.20(2) 0.20(2) 0.0000(10) 0.036(4) 0.0000(10) C213 0.16(3) 0.16(3) 0.16(3) 0.0000(10) 0.029(5) 0.0000(10) C214 0.22(3) 0.22(3) 0.22(3) 0.0000(10) 0.040(5) 0.0000(10) C215 0.19(3) 0.19(3) 0.19(3) 0.0000(10) 0.035(5) 0.0000(10) C216 0.13(2) 0.13(2) 0.13(2) 0.0000(10) 0.023(4) 0.0000(10) O6 0.083(8) 0.083(8) 0.083(8) 0.0001(9) 0.0151(17) 0.0000(9) C217 0.083(8) 0.083(8) 0.083(8) 0.0000(9) 0.0152(17) 0.0000(9) C218 0.083(8) 0.083(8) 0.083(8) 0.0000(9) 0.0152(17) -0.0001(9) C219 0.083(8) 0.083(8) 0.083(8) 0.0000(9) 0.0152(17) -0.0001(9) C220 0.083(8) 0.083(8) 0.083(8) 0.0000(9) 0.0152(17) 0.0000(9) O7 0.113(17) 0.113(17) 0.113(17) 0.0001(10) 0.021(3) 0.0000(10) C221 0.12(2) 0.12(2) 0.12(2) 0.0000(10) 0.022(4) 0.0000(10) C222 0.09(2) 0.09(2) 0.09(2) 0.0000(10) 0.017(4) 0.0000(10) C223 0.059(12) 0.059(12) 0.059(12) 0.0000(10) 0.011(2) 0.0000(10) C224 0.059(12) 0.059(12) 0.059(12) 0.0000(10) 0.011(2) 0.0000(10) O8 0.17(2) 0.17(2) 0.17(2) 0.0000(10) 0.031(4) 0.0000(10) C241 0.14(3) 0.14(3) 0.14(3) 0.0000(10) 0.026(5) 0.0000(10) C242 0.10(2) 0.10(2) 0.10(2) 0.0000(10) 0.019(4) 0.0000(10) C243 0.09(2) 0.09(2) 0.09(2) 0.0000(10) 0.016(4) 0.0000(10) C244 0.11(2) 0.11(2) 0.11(2) 0.0000(10) 0.021(4) 0.0000(10) Li3 0.017(12) 0.017(12) 0.017(12) 0.0001(10) 0.003(2) 0.0000(10) O9 0.080(14) 0.080(14) 0.080(14) 0.0001(10) 0.015(3) -0.0001(10) C245 0.080(10) 0.080(10) 0.080(10) 0.0000(10) 0.015(2) 0.0000(10) C246 0.080(10) 0.080(10) 0.080(10) 0.0000(9) 0.015(2) 0.0000(9) C247 0.079(10) 0.079(10) 0.079(10) 0.0000(9) 0.015(2) 0.0000(9) C248 0.079(10) 0.079(10) 0.079(10) 0.0000(10) 0.015(2) 0.0000(10) O10 0.088(14) 0.088(14) 0.088(14) 0.0000(10) 0.016(3) 0.0000(10) C249 0.14(2) 0.14(2) 0.14(2) 0.0000(10) 0.025(5) 0.0000(10) C250 0.13(2) 0.13(2) 0.13(2) 0.0000(10) 0.024(5) 0.0000(10) C251 0.14(2) 0.14(2) 0.14(2) 0.0000(10) 0.026(5) 0.0000(10) C252 0.11(2) 0.11(2) 0.11(2) 0.0000(10) 0.019(4) 0.0000(10) O11 0.065(12) 0.065(12) 0.065(12) 0.0000(10) 0.012(2) -0.0001(10) C253 0.078(10) 0.078(10) 0.078(10) 0.0000(10) 0.014(2) 0.0000(10) C254 0.078(10) 0.078(10) 0.078(10) 0.0000(9) 0.014(2) 0.0000(9) C255 0.078(10) 0.078(10) 0.078(10) 0.0000(9) 0.014(2) 0.0000(9) C256 0.078(10) 0.078(10) 0.078(10) 0.0000(10) 0.014(2) 0.0000(10) O12 0.055(11) 0.054(11) 0.055(11) 0.0000(10) 0.010(2) 0.0000(10) C261 0.083(10) 0.083(10) 0.083(10) 0.0000(10) 0.015(2) 0.0000(10) C262 0.083(10) 0.083(10) 0.083(10) 0.0000(9) 0.015(2) 0.0000(9) C263 0.083(10) 0.083(10) 0.083(10) -0.0001(9) 0.015(2) 0.0000(9) C264 0.083(10) 0.084(10) 0.083(10) 0.0000(10) 0.015(2) 0.0000(10) O13 0.126(18) 0.126(18) 0.126(18) 0.0000(10) 0.023(3) 0.0000(10) C265 0.14(2) 0.14(2) 0.14(2) 0.0000(10) 0.025(5) 0.0000(10) C266 0.14(2) 0.14(2) 0.14(2) 0.0000(10) 0.025(5) 0.0000(10) C267 0.17(3) 0.17(3) 0.17(3) 0.0000(10) 0.031(5) 0.0000(10) C268 0.19(3) 0.19(3) 0.19(3) 0.0000(10) 0.036(5) 0.0000(10) O14 0.106(16) 0.106(16) 0.106(16) 0.0000(10) 0.019(3) 0.0000(10) C209 0.042(15) 0.042(15) 0.042(15) 0.0000(10) 0.008(3) 0.0000(10) C210 0.066(18) 0.066(18) 0.066(18) 0.0000(10) 0.012(3) 0.0000(10) C211 0.035(14) 0.035(14) 0.035(14) 0.0000(10) 0.006(3) 0.0000(10) C212 0.049(16) 0.049(16) 0.049(16) 0.0000(10) 0.009(3) 0.0000(10) O15 0.102(16) 0.102(16) 0.102(16) 0.0000(10) 0.019(3) 0.0000(10) C225 0.051(16) 0.051(16) 0.051(16) 0.0000(10) 0.009(3) 0.0000(10) C226 0.027(13) 0.027(13) 0.027(13) 0.0000(10) 0.005(3) 0.0001(10) C227 0.052(16) 0.052(16) 0.052(16) 0.0001(10) 0.009(3) 0.0000(10) C228 0.11(2) 0.11(2) 0.11(2) 0.0000(10) 0.021(4) 0.0000(10) O16 0.142(19) 0.142(19) 0.142(19) 0.0000(10) 0.026(4) 0.0000(10) C237 0.09(2) 0.09(2) 0.09(2) 0.0000(10) 0.016(4) 0.0000(10) C238 0.063(17) 0.063(17) 0.063(17) 0.0000(10) 0.011(3) 0.0001(10) C239 0.09(2) 0.09(2) 0.09(2) 0.0000(10) 0.017(4) 0.0000(10) C240 0.10(2) 0.10(2) 0.10(2) -0.0001(10) 0.019(4) 0.0000(10) O17 0.115(17) 0.115(17) 0.115(17) 0.0000(10) 0.021(3) 0.0000(10) C257 0.10(2) 0.10(2) 0.10(2) 0.0000(10) 0.018(4) 0.0000(10) C258 0.050(16) 0.050(16) 0.050(16) 0.0000(10) 0.009(3) 0.0001(10) C259 0.076(19) 0.076(19) 0.076(19) 0.0000(10) 0.014(4) 0.0001(10) C260 0.11(2) 0.11(2) 0.11(2) 0.0000(10) 0.021(4) 0.0000(10) O18 0.130(18) 0.130(18) 0.130(18) 0.0000(10) 0.024(3) -0.0001(10) C269 0.10(2) 0.10(2) 0.10(2) 0.0000(10) 0.018(4) 0.0000(10) C270 0.08(2) 0.08(2) 0.08(2) -0.0001(10) 0.015(4) 0.0000(10) C271 0.047(15) 0.047(15) 0.047(15) 0.0001(10) 0.009(3) 0.0000(10) C272 0.071(18) 0.071(18) 0.071(18) -0.0001(10) 0.013(3) 0.0000(10) O19 0.124(18) 0.124(18) 0.124(18) 0.0000(10) 0.023(3) 0.0000(10) C273 0.10(2) 0.10(2) 0.10(2) 0.0000(10) 0.018(4) 0.0000(10) C274 0.17(3) 0.17(3) 0.17(3) 0.0000(10) 0.030(5) 0.0000(10) C275 0.11(2) 0.11(2) 0.11(2) 0.0000(10) 0.021(4) 0.0000(10) C276 0.09(2) 0.09(2) 0.09(2) 0.0000(10) 0.017(4) 0.0000(10) _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 Si1 2.614(8) . ? In1 In2 2.845(2) . ? In1 In4 2.859(3) . ? In1 In5 3.038(3) . ? In1 In6 3.044(3) . ? In2 Si2 2.596(9) . ? In2 In3 2.856(3) . ? In2 In7 2.965(3) . ? In2 In6 2.988(3) . ? In3 Si3 2.624(9) . ? In3 In4 2.856(2) . ? In3 In7 3.044(3) . ? In3 In8 3.053(3) . ? In4 Si4 2.592(9) . ? In4 In5 2.963(3) . ? In4 In8 2.973(3) . ? In5 Si5 2.614(7) . ? In5 In6 2.823(3) . ? In5 In8 2.916(3) . ? In6 Si6 2.609(10) . ? In6 In7 2.897(3) . ? In7 Si7 2.609(7) . ? In7 In8 2.825(3) . ? In8 Si8 2.614(10) . ? Si1 C13 1.85(3) . ? Si1 C1 1.88(3) . ? Si1 C7 1.91(3) . ? Si2 C19 1.86(3) . ? Si2 C25 1.89(3) . ? Si2 C31 1.90(2) . ? Si3 C49 1.87(3) . ? Si3 C37 1.87(3) . ? Si3 C43 1.88(3) . ? Si4 C67 1.85(3) . ? Si4 C61 1.88(3) . ? Si4 C55 1.90(3) . ? Si5 C79 1.893(17) . ? Si5 C73 1.905(16) . ? Si5 C85 1.92(3) . ? Si6 C103 1.87(3) . ? Si6 C91 1.87(3) . ? Si6 C97 1.91(3) . ? Si7 C115 1.84(3) . ? Si7 C109 1.88(3) . ? Si7 C121 1.90(3) . ? Si8 C133 1.88(3) . ? Si8 C127 1.89(3) . ? Si8 C139 1.90(3) . ? C1 C6 1.34(4) . ? C1 C2 1.38(4) . ? C2 C3 1.43(4) . ? C3 C4 1.37(4) . ? C4 C5 1.43(4) . ? C5 C6 1.38(4) . ? C7 C8 1.40(4) . ? C7 C12 1.43(4) . ? C8 C9 1.44(4) . ? C9 C10 1.33(4) . ? C10 C11 1.34(4) . ? C11 C12 1.39(4) . ? C13 C18 1.39(4) . ? C13 C14 1.43(4) . ? C14 C15 1.35(4) . ? C15 C16 1.36(4) . ? C16 C17 1.41(4) . ? C17 C18 1.39(4) . ? C19 C20 1.35(3) . ? C19 C24 1.43(4) . ? C20 C21 1.41(4) . ? C21 C22 1.34(4) . ? C22 C23 1.37(4) . ? C23 C24 1.36(4) . ? C25 C26 1.38(4) . ? C25 C30 1.44(4) . ? C26 C27 1.32(4) . ? C27 C28 1.39(4) . ? C28 C29 1.37(4) . ? C29 C30 1.37(4) . ? C31 C36 1.43(4) . ? C31 C32 1.43(4) . ? C32 C33 1.44(4) . ? C33 C34 1.40(4) . ? C34 C35 1.37(4) . ? C35 C36 1.40(4) . ? C37 C42 1.40(4) . ? C37 C38 1.45(4) . ? C38 C39 1.42(4) . ? C39 C40 1.35(4) . ? C40 C41 1.36(4) . ? C41 C42 1.34(4) . ? C43 C44 1.39(4) . ? C43 C48 1.51(4) . ? C44 C45 1.38(4) . ? C45 C46 1.45(4) . ? C46 C47 1.37(4) . ? C47 C48 1.37(4) . ? C49 C54 1.42(4) . ? C49 C50 1.44(4) . ? C50 C51 1.39(5) . ? C51 C52 1.35(5) . ? C52 C53 1.40(5) . ? C53 C54 1.37(4) . ? C55 C56 1.40(4) . ? C55 C60 1.43(4) . ? C56 C57 1.35(4) . ? C57 C58 1.39(4) . ? C58 C59 1.42(4) . ? C59 C60 1.31(4) . ? C61 C62 1.42(4) . ? C61 C66 1.46(4) . ? C62 C63 1.38(3) . ? C63 C64 1.39(4) . ? C64 C65 1.37(4) . ? C65 C66 1.36(4) . ? C67 C68 1.40(4) . ? C67 C72 1.41(4) . ? C68 C69 1.37(5) . ? C69 C70 1.35(5) . ? C70 C71 1.36(4) . ? C71 C72 1.39(4) . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C79 C84 1.36(3) . ? C79 C80 1.4491 . ? C80 C81 1.38(3) . ? C81 C82 1.35(4) . ? C82 C83 1.41(4) . ? C83 C84 1.37(4) . ? C85 C86 1.40(4) . ? C85 C90 1.45(4) . ? C86 C87 1.41(4) . ? C87 C88 1.37(4) . ? C88 C89 1.36(4) . ? C89 C90 1.34(4) . ? C91 C92 1.39(4) . ? C91 C96 1.46(4) . ? C92 C93 1.39(4) . ? C93 C94 1.37(4) . ? C94 C95 1.37(4) . ? C95 C96 1.41(4) . ? C97 C98 1.38(4) . ? C97 C102 1.39(4) . ? C98 C99 1.42(4) . ? C99 C100 1.37(4) . ? C100 C101 1.38(4) . ? C101 C102 1.37(4) . ? C103 C104 1.41(4) . ? C103 C108 1.41(4) . ? C104 C105 1.44(4) . ? C105 C106 1.32(4) . ? C106 C107 1.39(4) . ? C107 C108 1.39(4) . ? C109 C114 1.37(4) . ? C109 C110 1.42(3) . ? C110 C111 1.40(4) . ? C111 C112 1.36(4) . ? C112 C113 1.41(4) . ? C113 C114 1.40(4) . ? C115 C120 1.41(4) . ? C115 C116 1.44(4) . ? C116 C117 1.33(4) . ? C117 C118 1.38(4) . ? C118 C119 1.36(4) . ? C119 C120 1.37(4) . ? C121 C122 1.39(4) . ? C121 C126 1.45(4) . ? C122 C123 1.46(4) . ? C123 C124 1.31(4) . ? C124 C125 1.43(4) . ? C125 C126 1.45(5) . ? C127 C132 1.39(4) . ? C127 C128 1.42(4) . ? C128 C129 1.37(4) . ? C129 C130 1.32(4) . ? C130 C131 1.38(4) . ? C131 C132 1.41(4) . ? C133 C138 1.37(4) . ? C133 C134 1.38(4) . ? C134 C135 1.37(5) . ? C135 C136 1.40(5) . ? C136 C137 1.32(4) . ? C137 C138 1.41(4) . ? C139 C144 1.38(4) . ? C139 C140 1.41(4) . ? C140 C141 1.40(4) . ? C141 C142 1.34(5) . ? C142 C143 1.41(4) . ? C143 C144 1.39(4) . ? Li1 O2 1.88(5) . ? Li1 O2 1.88(5) 2 ? Li1 O1 1.92(5) . ? Li1 O1 1.92(5) 2 ? O1 C145 1.33(7) . ? O1 C148 1.56(6) . ? C145 C146 1.65(7) . ? C146 C147 1.35(8) . ? C147 C148 1.47(8) . ? O2 C152 1.34(8) . ? O2 C149 1.48(8) . ? C149 C150 1.44(9) . ? C150 C151 1.23(8) . ? C151 C152 1.52(9) . ? Li2 O5 2.55(9) . ? O3 C204 1.36(2) . ? O3 C201 1.37(2) . ? C201 C202 1.22(2) . ? C202 C203 1.31(2) . ? C203 C204 1.30(2) . ? O4 C208 1.35(2) . ? O4 C205 1.37(2) . ? C205 C206 1.23(2) . ? C206 C207 1.30(2) . ? C207 C208 1.29(2) . ? O5 C216 1.35(2) . ? O5 C213 1.37(2) . ? C213 C214 1.22(3) . ? C214 C215 1.30(2) . ? C215 C216 1.30(2) . ? O6 C220 1.36(2) . ? O6 C217 1.38(2) . ? C217 C218 1.22(2) . ? C218 C219 1.31(2) . ? C218 C220 2.04(3) . ? C219 C220 1.30(2) . ? O7 C224 1.36(2) . ? O7 C221 1.37(2) . ? C221 C222 1.22(2) . ? C222 C223 1.30(2) . ? C223 C224 1.30(2) . ? O8 C244 1.36(2) . ? O8 C241 1.37(2) . ? C241 C242 1.23(2) . ? C242 C243 1.31(2) . ? C243 C244 1.30(2) . ? Li3 O10 2.66(7) . ? O9 C248 1.35(2) . ? O9 C245 1.37(2) . ? C245 C246 1.23(2) . ? C246 C247 1.31(2) . ? C247 C248 1.30(2) . ? O10 C252 1.35(2) . ? O10 C249 1.37(2) . ? C249 C250 1.22(2) . ? C250 C251 1.30(2) . ? C251 C252 1.30(2) . ? O11 C256 1.36(2) . ? O11 C253 1.37(2) . ? C253 C254 1.23(2) . ? C254 C255 1.30(2) . ? C255 C256 1.30(2) . ? O12 C264 1.35(2) . ? O12 C261 1.37(2) . ? C261 C262 1.22(2) . ? C262 C263 1.30(2) . ? C263 C264 1.30(2) . ? O13 C268 1.36(2) . ? O13 C265 1.37(2) . ? C265 C266 1.22(2) . ? C266 C267 1.30(2) . ? C267 C268 1.30(2) . ? O14 C212 1.36(2) . ? O14 C209 1.37(2) . ? C209 C210 1.22(2) . ? C210 C211 1.30(2) . ? C211 C212 1.30(2) . ? O15 C228 1.36(2) . ? O15 C225 1.37(2) . ? C225 C226 1.23(2) . ? C226 C227 1.30(2) . ? C227 C228 1.29(2) . ? O16 C240 1.36(2) . ? O16 C237 1.37(2) . ? C237 C238 1.22(2) . ? C238 C239 1.31(2) . ? C239 C240 1.30(2) . ? O17 C260 1.36(2) . ? O17 C257 1.37(2) . ? C257 C258 1.23(2) . ? C258 C259 1.30(2) . ? C259 C260 1.30(2) . ? O18 C272 1.35(2) . ? O18 C269 1.37(2) . ? C269 C270 1.23(2) . ? C270 C271 1.31(2) . ? C271 C272 1.29(2) . ? O19 C276 1.35(2) . ? O19 C273 1.37(2) . ? C273 C274 1.23(2) . ? C274 C275 1.31(2) . ? C275 C276 1.30(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 Si1 In1 In2 125.87(19) . . ? Si1 In1 In4 124.5(2) . . ? In2 In1 In4 97.25(8) . . ? Si1 In1 In5 126.33(19) . . ? In2 In1 In5 102.84(8) . . ? In4 In1 In5 60.23(8) . . ? Si1 In1 In6 128.8(2) . . ? In2 In1 In6 60.87(7) . . ? In4 In1 In6 100.79(9) . . ? In5 In1 In6 55.31(7) . . ? Si2 In2 In1 122.72(18) . . ? Si2 In2 In3 126.6(2) . . ? In1 In2 In3 82.54(8) . . ? Si2 In2 In7 134.90(18) . . ? In1 In2 In7 101.44(8) . . ? In3 In2 In7 63.02(8) . . ? Si2 In2 In6 132.9(2) . . ? In1 In2 In6 62.86(7) . . ? In3 In2 In6 100.11(9) . . ? In7 In2 In6 58.25(7) . . ? Si3 In3 In2 123.3(2) . . ? Si3 In3 In4 126.4(2) . . ? In2 In3 In4 97.05(8) . . ? Si3 In3 In7 127.2(2) . . ? In2 In3 In7 60.24(8) . . ? In4 In3 In7 102.00(8) . . ? Si3 In3 In8 130.3(2) . . ? In2 In3 In8 100.86(9) . . ? In4 In3 In8 60.30(7) . . ? In7 In3 In8 55.19(7) . . ? Si4 In4 In3 123.99(19) . . ? Si4 In4 In1 129.4(2) . . ? In3 In4 In1 82.29(8) . . ? Si4 In4 In5 132.37(19) . . ? In3 In4 In5 102.02(9) . . ? In1 In4 In5 62.89(8) . . ? Si4 In4 In8 129.8(2) . . ? In3 In4 In8 63.14(7) . . ? In1 In4 In8 100.18(9) . . ? In5 In4 In8 58.85(7) . . ? Si5 In5 In6 124.6(2) . . ? Si5 In5 In8 125.9(2) . . ? In6 In5 In8 87.68(8) . . ? Si5 In5 In4 130.3(2) . . ? In6 In5 In4 103.65(8) . . ? In8 In5 In4 60.75(7) . . ? Si5 In5 In1 134.7(2) . . ? In6 In5 In1 62.45(8) . . ? In8 In5 In1 97.40(8) . . ? In4 In5 In1 56.88(8) . . ? Si6 In6 In5 126.94(19) . . ? Si6 In6 In7 124.36(18) . . ? In5 In6 In7 92.36(9) . . ? Si6 In6 In2 125.8(2) . . ? In5 In6 In2 104.67(10) . . ? In7 In6 In2 60.49(7) . . ? Si6 In6 In1 132.7(2) . . ? In5 In6 In1 62.25(7) . . ? In7 In6 In1 98.40(9) . . ? In2 In6 In1 56.28(7) . . ? Si7 In7 In8 124.7(2) . . ? Si7 In7 In6 126.9(2) . . ? In8 In7 In6 88.01(8) . . ? Si7 In7 In2 129.5(2) . . ? In8 In7 In2 103.79(9) . . ? In6 In7 In2 61.26(7) . . ? Si7 In7 In3 132.9(2) . . ? In8 In7 In3 62.57(8) . . ? In6 In7 In3 97.88(8) . . ? In2 In7 In3 56.73(8) . . ? Si8 In8 In7 126.31(19) . . ? Si8 In8 In5 123.61(18) . . ? In7 In8 In5 91.92(9) . . ? Si8 In8 In4 127.1(2) . . ? In7 In8 In4 104.56(9) . . ? In5 In8 In4 60.40(7) . . ? Si8 In8 In3 134.0(2) . . ? In7 In8 In3 62.24(8) . . ? In5 In8 In3 98.51(9) . . ? In4 In8 In3 56.56(7) . . ? C13 Si1 C1 108.4(13) . . ? C13 Si1 C7 106.3(14) . . ? C1 Si1 C7 104.3(13) . . ? C13 Si1 In1 114.0(9) . . ? C1 Si1 In1 111.1(10) . . ? C7 Si1 In1 112.2(10) . . ? C19 Si2 C25 105.5(13) . . ? C19 Si2 C31 105.3(11) . . ? C25 Si2 C31 105.1(11) . . ? C19 Si2 In2 116.2(9) . . ? C25 Si2 In2 109.6(10) . . ? C31 Si2 In2 114.3(9) . . ? C49 Si3 C37 104.6(15) . . ? C49 Si3 C43 104.4(12) . . ? C37 Si3 C43 108.0(13) . . ? C49 Si3 In3 114.3(9) . . ? C37 Si3 In3 111.8(10) . . ? C43 Si3 In3 113.0(10) . . ? C67 Si4 C61 106.7(13) . . ? C67 Si4 C55 105.9(14) . . ? C61 Si4 C55 102.3(12) . . ? C67 Si4 In4 114.4(10) . . ? C61 Si4 In4 115.9(11) . . ? C55 Si4 In4 110.5(9) . . ? C79 Si5 C73 107.9(6) . . ? C79 Si5 C85 105.8(12) . . ? C73 Si5 C85 104.3(11) . . ? C79 Si5 In5 113.2(6) . . ? C73 Si5 In5 115.7(6) . . ? C85 Si5 In5 109.3(8) . . ? C103 Si6 C91 107.2(13) . . ? C103 Si6 C97 106.8(13) . . ? C91 Si6 C97 106.1(13) . . ? C103 Si6 In6 113.0(10) . . ? C91 Si6 In6 112.7(10) . . ? C97 Si6 In6 110.7(11) . . ? C115 Si7 C109 107.8(13) . . ? C115 Si7 C121 105.3(13) . . ? C109 Si7 C121 105.9(12) . . ? C115 Si7 In7 110.2(8) . . ? C109 Si7 In7 112.4(9) . . ? C121 Si7 In7 114.9(9) . . ? C133 Si8 C127 104.7(13) . . ? C133 Si8 C139 104.8(14) . . ? C127 Si8 C139 106.7(13) . . ? C133 Si8 In8 114.7(10) . . ? C127 Si8 In8 111.0(10) . . ? C139 Si8 In8 114.1(11) . . ? C6 C1 C2 118(3) . . ? C6 C1 Si1 120(2) . . ? C2 C1 Si1 122(2) . . ? C1 C2 C3 122(3) . . ? C4 C3 C2 116(3) . . ? C3 C4 C5 124(3) . . ? C6 C5 C4 115(3) . . ? C1 C6 C5 126(3) . . ? C8 C7 C12 119(3) . . ? C8 C7 Si1 117(3) . . ? C12 C7 Si1 124(3) . . ? C7 C8 C9 117(3) . . ? C10 C9 C8 122(4) . . ? C9 C10 C11 121(4) . . ? C10 C11 C12 122(4) . . ? C11 C12 C7 119(4) . . ? C18 C13 C14 114(3) . . ? C18 C13 Si1 123(2) . . ? C14 C13 Si1 123(2) . . ? C15 C14 C13 125(3) . . ? C14 C15 C16 117(3) . . ? C15 C16 C17 123(4) . . ? C18 C17 C16 117(3) . . ? C13 C18 C17 124(3) . . ? C20 C19 C24 113(3) . . ? C20 C19 Si2 124(2) . . ? C24 C19 Si2 123(2) . . ? C19 C20 C21 125(3) . . ? C22 C21 C20 118(3) . . ? C21 C22 C23 122(4) . . ? C24 C23 C22 118(4) . . ? C23 C24 C19 124(3) . . ? C26 C25 C30 114(3) . . ? C26 C25 Si2 123(2) . . ? C30 C25 Si2 122(2) . . ? C27 C26 C25 121(3) . . ? C26 C27 C28 127(3) . . ? C29 C28 C27 115(3) . . ? C28 C29 C30 120(3) . . ? C29 C30 C25 123(3) . . ? C36 C31 C32 121(2) . . ? C36 C31 Si2 118.5(19) . . ? C32 C31 Si2 119.9(19) . . ? C31 C32 C33 117(3) . . ? C34 C33 C32 121(3) . . ? C35 C34 C33 121(3) . . ? C34 C35 C36 120(3) . . ? C35 C36 C31 119(3) . . ? C42 C37 C38 114(3) . . ? C42 C37 Si3 127(3) . . ? C38 C37 Si3 119(3) . . ? C39 C38 C37 119(3) . . ? C40 C39 C38 123(4) . . ? C39 C40 C41 117(4) . . ? C42 C41 C40 123(4) . . ? C41 C42 C37 123(4) . . ? C44 C43 C48 115(2) . . ? C44 C43 Si3 125(2) . . ? C48 C43 Si3 121(2) . . ? C45 C44 C43 126(3) . . ? C44 C45 C46 114(3) . . ? C47 C46 C45 125(3) . . ? C46 C47 C48 119(3) . . ? C47 C48 C43 121(3) . . ? C54 C49 C50 116(3) . . ? C54 C49 Si3 119(2) . . ? C50 C49 Si3 124(2) . . ? C51 C50 C49 121(3) . . ? C52 C51 C50 122(4) . . ? C51 C52 C53 118(4) . . ? C54 C53 C52 123(3) . . ? C53 C54 C49 120(3) . . ? C56 C55 C60 114(3) . . ? C56 C55 Si4 122(2) . . ? C60 C55 Si4 123(2) . . ? C57 C56 C55 122(3) . . ? C56 C57 C58 124(3) . . ? C57 C58 C59 114(3) . . ? C60 C59 C58 122(3) . . ? C59 C60 C55 124(3) . . ? C62 C61 C66 116(3) . . ? C62 C61 Si4 121(2) . . ? C66 C61 Si4 123(2) . . ? C63 C62 C61 121(3) . . ? C62 C63 C64 119(3) . . ? C65 C64 C63 123(3) . . ? C66 C65 C64 119(3) . . ? C65 C66 C61 122(3) . . ? C68 C67 C72 117(3) . . ? C68 C67 Si4 121(3) . . ? C72 C67 Si4 122(2) . . ? C69 C68 C67 121(4) . . ? C70 C69 C68 121(5) . . ? C69 C70 C71 121(5) . . ? C70 C71 C72 120(4) . . ? C71 C72 C67 121(3) . . ? C74 C73 C78 120.0 . . ? C74 C73 Si5 122.5(8) . . ? C78 C73 Si5 116.8(8) . . ? C75 C74 C73 120.0 . . ? C76 C75 C74 120.0 . . ? C75 C76 C77 120.0 . . ? C78 C77 C76 120.0 . . ? C77 C78 C73 120.0 . . ? C84 C79 C80 119.8(16) . . ? C84 C79 Si5 121.6(17) . . ? C80 C79 Si5 117.9(4) . . ? C81 C80 C79 117.7(17) . . ? C82 C81 C80 123(3) . . ? C81 C82 C83 117(3) . . ? C84 C83 C82 123(4) . . ? C79 C84 C83 119(3) . . ? C86 C85 C90 118(3) . . ? C86 C85 Si5 120(2) . . ? C90 C85 Si5 122(2) . . ? C85 C86 C87 119(3) . . ? C88 C87 C86 122(3) . . ? C89 C88 C87 119(4) . . ? C90 C89 C88 123(3) . . ? C89 C90 C85 120(3) . . ? C92 C91 C96 115(3) . . ? C92 C91 Si6 124(3) . . ? C96 C91 Si6 119(2) . . ? C91 C92 C93 125(4) . . ? C94 C93 C92 117(3) . . ? C95 C94 C93 121(3) . . ? C94 C95 C96 122(4) . . ? C95 C96 C91 119(3) . . ? C98 C97 C102 119(3) . . ? C98 C97 Si6 120(3) . . ? C102 C97 Si6 121(3) . . ? C97 C98 C99 121(4) . . ? C100 C99 C98 121(4) . . ? C99 C100 C101 113(4) . . ? C102 C101 C100 129(4) . . ? C101 C102 C97 116(4) . . ? C104 C103 C108 116(3) . . ? C104 C103 Si6 122(2) . . ? C108 C103 Si6 122(2) . . ? C103 C104 C105 120(3) . . ? C106 C105 C104 120(3) . . ? C105 C106 C107 123(3) . . ? C106 C107 C108 118(3) . . ? C107 C108 C103 123(3) . . ? C114 C109 C110 115(3) . . ? C114 C109 Si7 123(2) . . ? C110 C109 Si7 121(2) . . ? C111 C110 C109 122(3) . . ? C112 C111 C110 121(3) . . ? C111 C112 C113 120(4) . . ? C114 C113 C112 118(4) . . ? C109 C114 C113 124(3) . . ? C120 C115 C116 112(3) . . ? C120 C115 Si7 125(2) . . ? C116 C115 Si7 122(2) . . ? C117 C116 C115 123(3) . . ? C116 C117 C118 124(3) . . ? C119 C118 C117 115(3) . . ? C118 C119 C120 123(3) . . ? C119 C120 C115 123(3) . . ? C122 C121 C126 121(3) . . ? C122 C121 Si7 122(2) . . ? C126 C121 Si7 116(2) . . ? C121 C122 C123 121(3) . . ? C124 C123 C122 116(3) . . ? C123 C124 C125 128(4) . . ? C124 C125 C126 116(4) . . ? C121 C126 C125 118(4) . . ? C132 C127 C128 119(3) . . ? C132 C127 Si8 119(2) . . ? C128 C127 Si8 122(2) . . ? C129 C128 C127 120(3) . . ? C130 C129 C128 121(3) . . ? C129 C130 C131 121(4) . . ? C130 C131 C132 120(4) . . ? C127 C132 C131 118(3) . . ? C138 C133 C134 117(3) . . ? C138 C133 Si8 123(3) . . ? C134 C133 Si8 119(2) . . ? C135 C134 C133 122(4) . . ? C134 C135 C136 119(4) . . ? C137 C136 C135 120(4) . . ? C136 C137 C138 121(4) . . ? C133 C138 C137 121(4) . . ? C144 C139 C140 118(3) . . ? C144 C139 Si8 121(3) . . ? C140 C139 Si8 121(2) . . ? C141 C140 C139 118(3) . . ? C142 C141 C140 124(4) . . ? C141 C142 C143 118(4) . . ? C144 C143 C142 119(3) . . ? C139 C144 C143 122(4) . . ? O2 Li1 O2 106(4) . 2 ? O2 Li1 O1 105.2(15) . . ? O2 Li1 O1 114.5(16) 2 . ? O2 Li1 O1 114.5(16) . 2 ? O2 Li1 O1 105.2(15) 2 2 ? O1 Li1 O1 112(4) . 2 ? C145 O1 C148 113(5) . . ? C145 O1 Li1 122(4) . . ? C148 O1 Li1 122(4) . . ? O1 C145 C146 99(5) . . ? C147 C146 C145 103(6) . . ? C146 C147 C148 104(7) . . ? C147 C148 O1 99(6) . . ? C152 O2 C149 101(5) . . ? C152 O2 Li1 138(5) . . ? C149 O2 Li1 121(5) . . ? C150 C149 O2 96(6) . . ? C151 C150 C149 118(8) . . ? C150 C151 C152 98(7) . . ? O2 C152 C151 110(7) . . ? C204 O3 C201 99(2) . . ? C202 C201 O3 111(2) . . ? C201 C202 C203 111(3) . . ? C204 C203 C202 103(2) . . ? C203 C204 O3 112(2) . . ? C208 O4 C205 98(2) . . ? C206 C205 O4 112(3) . . ? C205 C206 C207 109(3) . . ? C208 C207 C206 105(2) . . ? C207 C208 O4 113(2) . . ? C216 O5 C213 98(2) . . ? C216 O5 Li2 137(7) . . ? C213 O5 Li2 117(6) . . ? C214 C213 O5 111(3) . . ? C213 C214 C215 110(3) . . ? C216 C215 C214 105(2) . . ? C215 C216 O5 112(2) . . ? C220 O6 C217 98(2) . . ? C218 C217 O6 112(2) . . ? C217 C218 C219 110(3) . . ? C217 C218 C220 74.1(18) . . ? C219 C218 C220 38.4(14) . . ? C220 C219 C218 103(2) . . ? C219 C220 O6 111(2) . . ? C219 C220 C218 38.7(14) . . ? O6 C220 C218 75.8(15) . . ? C224 O7 C221 98(2) . . ? C222 C221 O7 113(2) . . ? C221 C222 C223 110(3) . . ? C224 C223 C222 104(2) . . ? C223 C224 O7 112(2) . . ? C244 O8 C241 99(2) . . ? C242 C241 O8 112(2) . . ? C241 C242 C243 109(3) . . ? C244 C243 C242 103(3) . . ? C243 C244 O8 111(3) . . ? C248 O9 C245 98.8(19) . . ? C246 C245 O9 111(2) . . ? C245 C246 C247 108(3) . . ? C248 C247 C246 103(2) . . ? C247 C248 O9 112(2) . . ? C252 O10 C249 99(2) . . ? C252 O10 Li3 137(4) . . ? C249 O10 Li3 123(4) . . ? C250 C249 O10 112(2) . . ? C249 C250 C251 110(3) . . ? C252 C251 C250 105(2) . . ? C251 C252 O10 112(2) . . ? C256 O11 C253 98.6(19) . . ? C254 C253 O11 113(2) . . ? C253 C254 C255 110(2) . . ? C256 C255 C254 104(2) . . ? C255 C256 O11 113(2) . . ? C264 O12 C261 98.4(19) . . ? C262 C261 O12 112(3) . . ? C261 C262 C263 110(3) . . ? C264 C263 C262 104(2) . . ? C263 C264 O12 113(2) . . ? C268 O13 C265 98(2) . . ? C266 C265 O13 111(3) . . ? C265 C266 C267 110(3) . . ? C268 C267 C266 105(2) . . ? C267 C268 O13 112(3) . . ? C212 O14 C209 99(2) . . ? C210 C209 O14 112(2) . . ? C209 C210 C211 110(2) . . ? C212 C211 C210 104(2) . . ? C211 C212 O14 111(2) . . ? C228 O15 C225 99(2) . . ? C226 C225 O15 112(2) . . ? C225 C226 C227 110(2) . . ? C228 C227 C226 105(2) . . ? C227 C228 O15 112(2) . . ? C240 O16 C237 98(2) . . ? C238 C237 O16 111(3) . . ? C237 C238 C239 110(2) . . ? C240 C239 C238 105(2) . . ? C239 C240 O16 111(2) . . ? C260 O17 C257 98(2) . . ? C258 C257 O17 112(2) . . ? C257 C258 C259 111(2) . . ? C260 C259 C258 104(2) . . ? C259 C260 O17 111(2) . . ? C272 O18 C269 99(2) . . ? C270 C269 O18 112(2) . . ? C269 C270 C271 110(2) . . ? C272 C271 C270 105(2) . . ? C271 C272 O18 113(2) . . ? C276 O19 C273 99(2) . . ? C274 C273 O19 112(3) . . ? C273 C274 C275 109(3) . . ? C276 C275 C274 104(2) . . ? C275 C276 O19 112(2) . . ? _diffrn_measured_fraction_theta_max 0.412 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.412 _refine_diff_density_max 0.953 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.172 # Attachment 'comp_9_728997.cif' data_tze5abso_comp9_CCDC_728997 _database_code_depnum_ccdc_archive 'CCDC 728997' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 In2 Li2 O6 Si3' _chemical_formula_weight 1144.91 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.160(3) _cell_length_b 14.200(3) _cell_length_c 14.688(3) _cell_angle_alpha 81.40(3) _cell_angle_beta 81.72(3) _cell_angle_gamma 89.42(3) _cell_volume 2889.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 23.8 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max .47 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.68762 _exptl_absorpt_correction_T_max 0.78202 _exptl_absorpt_process_details '13 faces' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'image plate, 2 circle goniometer' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18260 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 23.90 _reflns_number_total 8387 _reflns_number_gt 5765 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement STOE _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXTL 5.01' _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. Large ADP for the O and C atoms as well as for the attached lithium atoms indicate disorder, as is usaula for thf. Refining the thf molecules in a split model (SOF 10.5)gave partially better ADP but did greatly change the R values. For clarity here the non disordered model with large ADP is given ; _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^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8387 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 -0.26062(3) 0.70218(3) -0.29701(3) 0.02484(13) Uani 1 1 d . . . In2 In -0.12821(3) 0.59796(3) -0.40058(3) 0.03237(15) Uani 1 1 d . . . Si1 Si -0.34715(12) 0.80696(11) -0.41985(11) 0.0294(4) Uani 1 1 d . . . Si2 Si -0.16434(12) 0.80697(11) -0.21142(11) 0.0301(4) Uani 1 1 d . . . Si3 Si -0.37563(12) 0.58831(11) -0.17669(10) 0.0295(4) Uani 1 1 d . . . O1 O -0.0839(5) 0.3221(4) -0.2658(4) 0.0846(19) Uani 1 1 d . . . O2 O 0.0015(4) 0.5341(4) -0.3600(4) 0.0445(14) Uani 1 1 d . . . O3 O -0.1578(4) 0.4686(3) -0.4485(3) 0.0441(12) Uani 1 1 d . . . O4 O -0.0411(4) 0.6505(4) -0.5291(4) 0.0429(14) Uani 1 1 d . . . O5 O 0.1460(8) 0.3698(7) -0.2945(6) 0.150(4) Uani 1 1 d . . . O6 O -0.1631(5) 0.3009(6) -0.5651(7) 0.147(4) Uani 1 1 d . . . C1 C -0.4466(5) 0.7449(5) -0.4629(5) 0.0465(17) Uani 1 1 d . . . H1A H -0.4765 0.7904 -0.5067 0.070 Uiso 1 1 calc R . . H1B H -0.4944 0.7200 -0.4099 0.070 Uiso 1 1 calc R . . H1C H -0.4200 0.6922 -0.4942 0.070 Uiso 1 1 calc R . . C2 C -0.2591(5) 0.8575(4) -0.5276(4) 0.0349(15) Uani 1 1 d . . . C3 C -0.2875(6) 0.8833(5) -0.6139(4) 0.056(2) Uani 1 1 d . . . H3A H -0.3528 0.8768 -0.6207 0.067 Uiso 1 1 calc R . . C4 C -0.2216(7) 0.9188(7) -0.6911(5) 0.077(3) Uani 1 1 d . . . H4B H -0.2427 0.9357 -0.7499 0.093 Uiso 1 1 calc R . . C5 C -0.1260(7) 0.9298(6) -0.6837(5) 0.071(2) Uani 1 1 d . . . H5A H -0.0815 0.9531 -0.7370 0.085 Uiso 1 1 calc R . . C6 C -0.0968(5) 0.9068(5) -0.5990(5) 0.0495(18) Uani 1 1 d . . . H6A H -0.0318 0.9159 -0.5927 0.059 Uiso 1 1 calc R . . C7 C -0.1615(5) 0.8701(4) -0.5214(4) 0.0405(16) Uani 1 1 d . . . H7A H -0.1396 0.8531 -0.4630 0.049 Uiso 1 1 calc R . . C8 C -0.4049(5) 0.9121(4) -0.3678(4) 0.0329(15) Uani 1 1 d . . . C9 C -0.3640(5) 1.0048(4) -0.3869(4) 0.0434(17) Uani 1 1 d . . . H9A H -0.3070 1.0165 -0.4299 0.052 Uiso 1 1 calc R . . C10 C -0.4052(6) 1.0783(5) -0.3445(5) 0.055(2) Uani 1 1 d . . . H10A H -0.3772 1.1401 -0.3604 0.066 Uiso 1 1 calc R . . C11 C -0.4873(6) 1.0638(5) -0.2783(5) 0.054(2) Uani 1 1 d . . . H11A H -0.5142 1.1144 -0.2478 0.065 Uiso 1 1 calc R . . C12 C -0.5285(6) 0.9729(5) -0.2585(5) 0.055(2) Uani 1 1 d . . . H12A H -0.5851 0.9611 -0.2149 0.066 Uiso 1 1 calc R . . C13 C -0.4873(5) 0.9005(5) -0.3022(4) 0.0416(16) Uani 1 1 d . . . H13A H -0.5164 0.8391 -0.2869 0.050 Uiso 1 1 calc R . . C14 C -0.1066(5) 0.9180(5) -0.2854(5) 0.0516(19) Uani 1 1 d . . . H14A H -0.0753 0.9546 -0.2464 0.077 Uiso 1 1 calc R . . H14B H -0.1556 0.9571 -0.3131 0.077 Uiso 1 1 calc R . . H14C H -0.0591 0.8998 -0.3349 0.077 Uiso 1 1 calc R . . C15 C -0.2444(4) 0.8549(4) -0.1125(4) 0.0332(15) Uani 1 1 d . . . C16 C -0.3044(5) 0.9327(5) -0.1334(4) 0.0420(17) Uani 1 1 d . . . H16A H -0.3043 0.9606 -0.1964 0.050 Uiso 1 1 calc R . . C17 C -0.3630(5) 0.9688(6) -0.0638(5) 0.058(2) Uani 1 1 d . . . H17A H -0.4041 1.0201 -0.0797 0.070 Uiso 1 1 calc R . . C18 C -0.3631(5) 0.9316(6) 0.0290(5) 0.060(2) Uani 1 1 d . . . H18A H -0.4029 0.9580 0.0764 0.072 Uiso 1 1 calc R . . C19 C -0.3048(5) 0.8558(6) 0.0520(5) 0.054(2) Uani 1 1 d . . . H19A H -0.3046 0.8297 0.1154 0.065 Uiso 1 1 calc R . . C20 C -0.2463(5) 0.8174(5) -0.0178(4) 0.0426(16) Uani 1 1 d . . . H20A H -0.2069 0.7650 -0.0011 0.051 Uiso 1 1 calc R . . C21 C -0.0667(4) 0.7355(4) -0.1555(4) 0.0347(15) Uani 1 1 d . . . C22 C -0.0637(5) 0.6371(5) -0.1434(4) 0.0507(19) Uani 1 1 d . . . H22A H -0.1130 0.6033 -0.1627 0.061 Uiso 1 1 calc R . . C23 C 0.0088(6) 0.5849(6) -0.1039(5) 0.064(2) Uani 1 1 d . . . H23A H 0.0083 0.5173 -0.0977 0.077 Uiso 1 1 calc R . . C24 C 0.0798(6) 0.6310(7) -0.0743(6) 0.066(2) Uani 1 1 d . . . H24A H 0.1283 0.5957 -0.0465 0.079 Uiso 1 1 calc R . . C25 C 0.0812(6) 0.7302(8) -0.0850(6) 0.082(3) Uani 1 1 d . . . H25A H 0.1309 0.7630 -0.0652 0.098 Uiso 1 1 calc R . . C26 C 0.0081(5) 0.7815(6) -0.1256(6) 0.062(2) Uani 1 1 d . . . H26A H 0.0094 0.8491 -0.1329 0.074 Uiso 1 1 calc R . . C27 C -0.3259(5) 0.5372(5) -0.0666(4) 0.0476(18) Uani 1 1 d . . . H27A H -0.3738 0.4951 -0.0258 0.071 Uiso 1 1 calc R . . H27B H -0.3100 0.5892 -0.0343 0.071 Uiso 1 1 calc R . . H27C H -0.2683 0.5009 -0.0828 0.071 Uiso 1 1 calc R . . C28 C -0.4881(5) 0.6576(4) -0.1380(4) 0.0338(15) Uani 1 1 d . . . C29 C -0.4826(5) 0.7252(5) -0.0788(4) 0.0419(16) Uani 1 1 d . . . H29A H -0.4246 0.7338 -0.0555 0.050 Uiso 1 1 calc R . . C30 C -0.5627(5) 0.7809(5) -0.0533(5) 0.0514(19) Uani 1 1 d . . . H30A H -0.5577 0.8274 -0.0140 0.062 Uiso 1 1 calc R . . C31 C -0.6477(5) 0.7685(5) -0.0849(5) 0.0545(19) Uani 1 1 d . . . H31A H -0.7017 0.8054 -0.0669 0.065 Uiso 1 1 calc R . . C32 C -0.6537(5) 0.7013(6) -0.1434(5) 0.058(2) Uani 1 1 d . . . H32A H -0.7117 0.6929 -0.1667 0.070 Uiso 1 1 calc R . . C33 C -0.5753(5) 0.6465(5) -0.1680(4) 0.0440(17) Uani 1 1 d . . . H33A H -0.5815 0.5996 -0.2068 0.053 Uiso 1 1 calc R . . C34 C -0.4197(5) 0.4847(4) -0.2297(4) 0.0330(14) Uani 1 1 d . . . C35 C -0.4588(5) 0.4026(5) -0.1731(5) 0.0508(19) Uani 1 1 d . . . H35A H -0.4603 0.3968 -0.1076 0.061 Uiso 1 1 calc R . . C36 C -0.4954(6) 0.3293(5) -0.2109(6) 0.062(2) Uani 1 1 d . . . H36A H -0.5261 0.2763 -0.1708 0.075 Uiso 1 1 calc R . . C37 C -0.4879(6) 0.3326(5) -0.3060(6) 0.058(2) Uani 1 1 d . . . H37A H -0.5091 0.2803 -0.3314 0.070 Uiso 1 1 calc R . . C38 C -0.4492(6) 0.4124(5) -0.3636(5) 0.0516(19) Uani 1 1 d . . . H38A H -0.4466 0.4170 -0.4291 0.062 Uiso 1 1 calc R . . C39 C -0.4135(5) 0.4874(5) -0.3247(4) 0.0447(17) Uani 1 1 d . . . H39A H -0.3844 0.5411 -0.3649 0.054 Uiso 1 1 calc R . . C40 C -0.1515(9) 0.3571(8) -0.1992(7) 0.115(4) Uani 1 1 d . . . H40A H -0.1856 0.4117 -0.2291 0.138 Uiso 1 1 calc R . . H40B H -0.1192 0.3786 -0.1504 0.138 Uiso 1 1 calc R . . C41 C -0.2194(10) 0.2787(11) -0.1580(11) 0.155(6) Uani 1 1 d . . . H41A H -0.2007 0.2447 -0.0995 0.186 Uiso 1 1 calc R . . H41B H -0.2849 0.3031 -0.1449 0.186 Uiso 1 1 calc R . . C42 C -0.2135(12) 0.2202(13) -0.2249(11) 0.178(8) Uani 1 1 d . . . H42A H -0.2619 0.2382 -0.2665 0.214 Uiso 1 1 calc R . . H42B H -0.2255 0.1532 -0.1954 0.214 Uiso 1 1 calc R . . C43 C -0.1191(12) 0.2304(9) -0.2773(9) 0.147(6) Uani 1 1 d . . . H43A H -0.0772 0.1791 -0.2532 0.176 Uiso 1 1 calc R . . H43B H -0.1214 0.2274 -0.3438 0.176 Uiso 1 1 calc R . . C44 C 0.1543(13) 0.3404(10) -0.2005(10) 0.180(8) Uani 1 1 d . . . H44A H 0.1753 0.2734 -0.1903 0.216 Uiso 1 1 calc R . . H44B H 0.0925 0.3461 -0.1606 0.216 Uiso 1 1 calc R . . C45 C 0.2251(11) 0.4039(10) -0.1804(9) 0.128(5) Uani 1 1 d . . . H45A H 0.2802 0.3673 -0.1601 0.154 Uiso 1 1 calc R . . H45B H 0.1975 0.4398 -0.1303 0.154 Uiso 1 1 calc R . . C46 C 0.2555(12) 0.4696(9) -0.2670(11) 0.152(6) Uani 1 1 d . . . H46A H 0.2247 0.5321 -0.2637 0.183 Uiso 1 1 calc R . . H46B H 0.3256 0.4794 -0.2758 0.183 Uiso 1 1 calc R . . C47 C 0.2290(7) 0.4297(15) -0.3425(7) 0.178(9) Uani 1 1 d . . . H47A H 0.2808 0.3909 -0.3703 0.213 Uiso 1 1 calc R . . H47B H 0.2104 0.4794 -0.3913 0.213 Uiso 1 1 calc R . . C48 C -0.1161(9) 0.2346(10) -0.6115(12) 0.164(7) Uani 1 1 d . . . H48A H -0.0739 0.1970 -0.5721 0.196 Uiso 1 1 calc R . . H48B H -0.0765 0.2658 -0.6690 0.196 Uiso 1 1 calc R . . C49 C -0.1851(10) 0.1757(11) -0.6334(14) 0.179(8) Uani 1 1 d . . . H49A H -0.1762 0.1093 -0.6043 0.215 Uiso 1 1 calc R . . H49B H -0.1777 0.1771 -0.7017 0.215 Uiso 1 1 calc R . . C50 C -0.2778(7) 0.2065(8) -0.6010(7) 0.090(3) Uani 1 1 d . . . H50A H -0.3159 0.1538 -0.5611 0.108 Uiso 1 1 calc R . . H50B H -0.3120 0.2314 -0.6536 0.108 Uiso 1 1 calc R . . C51 C -0.2600(7) 0.2819(8) -0.5477(9) 0.117(4) Uani 1 1 d . . . H51A H -0.2960 0.3397 -0.5672 0.141 Uiso 1 1 calc R . . H51B H -0.2802 0.2607 -0.4804 0.141 Uiso 1 1 calc R . . Li1 Li 0.0109(19) 0.4034(12) -0.3608(13) 0.139(10) Uani 1 1 d . . . Li2 Li -0.0782(15) 0.3929(13) -0.5196(13) 0.106(6) Uani 1 1 d . . . C62 C -0.0780(13) 1.0226(12) -0.0217(14) 0.143(6) Uani 1 1 d . . . H62A H -0.1341 1.0012 -0.0467 0.171 Uiso 1 1 calc R . . H62B H -0.0950 1.0839 0.0004 0.171 Uiso 1 1 calc R . . C61 C -0.0656(14) 0.9586(18) 0.0538(12) 0.220(13) Uani 1 1 d . . . H61A H -0.1196 0.9655 0.1030 0.264 Uiso 1 1 calc R . . H61B H -0.0714 0.8943 0.0367 0.264 Uiso 1 1 calc R . . C63 C -0.0104(18) 1.0395(14) -0.0897(13) 0.183(8) Uani 1 1 d . . . H63A H -0.0076 0.9889 -0.1296 0.219 Uiso 1 1 calc R . . H63B H -0.0200 1.1014 -0.1281 0.219 Uiso 1 1 calc R . . H2 H 0.006(5) 0.550(5) -0.325(5) 0.03(3) Uiso 1 1 d . . . H3 H -0.208(5) 0.447(5) -0.431(5) 0.06(3) Uiso 1 1 d . . . H4 H -0.051(6) 0.689(5) -0.545(5) 0.03(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0278(3) 0.0227(2) 0.0247(2) -0.00812(16) -0.00132(18) 0.00109(19) In2 0.0346(3) 0.0324(3) 0.0311(2) -0.0125(2) -0.0007(2) 0.0084(2) Si1 0.0324(10) 0.0293(9) 0.0270(8) -0.0061(7) -0.0047(7) 0.0041(8) Si2 0.0298(10) 0.0306(9) 0.0320(9) -0.0128(7) -0.0028(7) -0.0023(8) Si3 0.0349(10) 0.0264(9) 0.0267(8) -0.0054(7) -0.0005(7) -0.0041(8) O1 0.102(5) 0.055(4) 0.078(4) 0.002(3) 0.038(4) 0.007(4) O2 0.052(3) 0.056(3) 0.032(3) -0.020(3) -0.015(2) 0.024(3) O3 0.042(3) 0.041(3) 0.051(3) -0.023(2) 0.004(3) -0.004(3) O4 0.047(3) 0.034(3) 0.045(3) -0.007(3) 0.003(2) 0.007(3) O5 0.217(11) 0.149(7) 0.100(6) -0.018(5) -0.082(7) 0.023(8) O6 0.073(5) 0.146(7) 0.239(9) -0.166(7) 0.064(6) -0.051(5) C1 0.049(5) 0.051(4) 0.043(4) -0.015(3) -0.012(3) 0.002(4) C2 0.039(4) 0.032(3) 0.033(3) -0.005(3) -0.002(3) 0.001(3) C3 0.057(5) 0.072(5) 0.036(4) 0.005(4) -0.011(4) -0.015(4) C4 0.091(8) 0.101(7) 0.036(4) 0.006(4) -0.011(5) -0.013(6) C5 0.092(8) 0.065(5) 0.045(5) 0.000(4) 0.017(5) -0.018(5) C6 0.050(5) 0.050(4) 0.046(4) -0.005(3) -0.001(4) 0.004(4) C7 0.045(5) 0.038(4) 0.037(4) -0.004(3) -0.004(3) 0.004(3) C8 0.042(4) 0.031(3) 0.026(3) -0.004(3) -0.007(3) 0.006(3) C9 0.046(4) 0.037(4) 0.041(4) 0.003(3) 0.005(3) 0.000(3) C10 0.073(6) 0.030(4) 0.059(4) -0.005(3) 0.001(4) 0.004(4) C11 0.082(6) 0.036(4) 0.045(4) -0.011(3) -0.009(4) 0.027(4) C12 0.067(6) 0.053(5) 0.040(4) -0.012(3) 0.009(4) 0.009(4) C13 0.045(4) 0.036(4) 0.042(4) -0.007(3) -0.001(3) 0.010(3) C14 0.057(5) 0.044(4) 0.054(4) -0.014(3) 0.000(4) -0.010(4) C15 0.033(4) 0.036(3) 0.032(3) -0.019(3) 0.001(3) -0.004(3) C16 0.050(4) 0.045(4) 0.036(3) -0.025(3) -0.004(3) 0.009(4) C17 0.051(5) 0.058(5) 0.070(5) -0.029(4) -0.008(4) 0.009(4) C18 0.057(5) 0.093(6) 0.041(4) -0.051(4) 0.002(4) 0.004(5) C19 0.054(5) 0.072(5) 0.040(4) -0.024(4) -0.002(4) 0.002(4) C20 0.040(4) 0.046(4) 0.041(4) -0.003(3) -0.006(3) -0.003(3) C21 0.027(4) 0.043(4) 0.037(3) -0.024(3) 0.000(3) 0.009(3) C22 0.049(5) 0.062(5) 0.042(4) -0.011(3) -0.007(3) 0.001(4) C23 0.071(6) 0.058(5) 0.066(5) -0.006(4) -0.026(5) 0.020(5) C24 0.044(5) 0.090(7) 0.068(5) -0.020(5) -0.021(4) 0.025(5) C25 0.044(5) 0.124(9) 0.092(7) -0.037(6) -0.036(5) 0.002(6) C26 0.047(5) 0.065(5) 0.083(6) -0.031(4) -0.020(4) 0.004(4) C27 0.055(5) 0.048(4) 0.039(4) -0.003(3) -0.009(3) -0.002(4) C28 0.044(4) 0.030(3) 0.027(3) -0.006(3) 0.000(3) -0.011(3) C29 0.045(4) 0.043(4) 0.039(4) -0.012(3) 0.001(3) -0.007(4) C30 0.057(5) 0.047(4) 0.050(4) -0.023(3) 0.011(4) -0.001(4) C31 0.042(5) 0.056(5) 0.061(5) -0.007(4) 0.004(4) 0.007(4) C32 0.038(5) 0.080(6) 0.059(5) -0.019(4) -0.009(4) 0.011(4) C33 0.039(4) 0.047(4) 0.045(4) -0.010(3) 0.002(3) -0.006(4) C34 0.038(4) 0.027(3) 0.034(3) -0.010(3) -0.002(3) 0.000(3) C35 0.067(5) 0.035(4) 0.048(4) -0.006(3) 0.001(4) -0.016(4) C36 0.075(6) 0.033(4) 0.077(6) 0.001(4) -0.017(5) -0.013(4) C37 0.078(6) 0.033(4) 0.074(5) -0.026(4) -0.023(5) -0.004(4) C38 0.069(5) 0.044(4) 0.048(4) -0.018(3) -0.017(4) -0.003(4) C39 0.061(5) 0.032(3) 0.044(4) -0.013(3) -0.009(3) 0.002(3) C40 0.162(12) 0.089(7) 0.077(7) -0.029(6) 0.054(7) 0.000(8) C41 0.118(12) 0.149(13) 0.165(14) -0.002(11) 0.062(10) 0.012(11) C42 0.177(17) 0.208(17) 0.146(13) -0.089(13) 0.058(12) -0.107(14) C43 0.200(16) 0.081(8) 0.131(10) -0.022(7) 0.075(10) -0.005(10) C44 0.28(2) 0.137(11) 0.150(13) 0.026(10) -0.162(15) -0.023(13) C45 0.160(13) 0.134(11) 0.103(9) -0.038(9) -0.045(9) 0.034(10) C46 0.178(15) 0.111(10) 0.170(13) 0.021(10) -0.072(12) -0.071(10) C47 0.049(6) 0.44(3) 0.043(5) -0.023(10) -0.002(5) -0.102(11) C48 0.087(9) 0.164(13) 0.269(18) -0.165(14) 0.011(11) -0.009(9) C49 0.098(11) 0.145(13) 0.32(2) -0.142(15) 0.009(13) -0.016(10) C50 0.077(7) 0.112(8) 0.085(7) -0.023(6) -0.013(6) -0.014(7) C51 0.071(8) 0.115(9) 0.171(11) -0.081(9) 0.031(8) -0.019(7) Li1 0.22(3) 0.060(10) 0.098(13) -0.011(9) 0.095(15) 0.024(13) Li2 0.131(17) 0.086(12) 0.105(13) -0.008(10) -0.042(12) 0.022(12) C62 0.193(19) 0.142(12) 0.117(11) -0.078(10) -0.043(13) -0.010(12) C61 0.191(18) 0.42(3) 0.073(10) -0.081(16) -0.024(11) -0.15(2) C63 0.22(2) 0.183(17) 0.132(15) -0.022(13) 0.018(18) -0.077(16) _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 Si2 2.5976(17) . ? In1 Si3 2.600(2) . ? In1 Si1 2.6014(18) . ? In1 In2 2.7956(10) . ? In2 O3 2.129(5) . ? In2 O4 2.137(5) . ? In2 O2 2.161(5) . ? In2 Li2 2.99(2) 2_564 ? In2 Li1 3.40(2) . ? Si1 C1 1.899(7) . ? Si1 C8 1.902(6) . ? Si1 C2 1.920(6) . ? Si2 C14 1.895(7) . ? Si2 C21 1.914(6) . ? Si2 C15 1.914(6) . ? Si3 C27 1.898(6) . ? Si3 C34 1.914(6) . ? Si3 C28 1.924(6) . ? O1 C40 1.409(10) . ? O1 C43 1.440(14) . ? O1 Li1 2.023(19) . ? O2 Li1 1.861(17) . ? O2 Li2 2.07(2) 2_564 ? O3 Li2 1.87(2) . ? O4 Li1 1.885(18) 2_564 ? O4 Li2 1.985(19) 2_564 ? O5 C44 1.403(13) . ? O5 C47 1.486(14) . ? O5 Li1 2.28(3) . ? O6 C48 1.357(11) . ? O6 C51 1.381(11) . ? O6 Li2 2.03(2) . ? C2 C3 1.381(8) . ? C2 C7 1.413(9) . ? C3 C4 1.395(11) . ? C4 C5 1.387(12) . ? C5 C6 1.360(10) . ? C6 C7 1.394(9) . ? C8 C13 1.397(9) . ? C8 C9 1.416(9) . ? C9 C10 1.377(9) . ? C10 C11 1.399(10) . ? C11 C12 1.394(10) . ? C12 C13 1.373(9) . ? C15 C20 1.409(8) . ? C15 C16 1.412(8) . ? C16 C17 1.380(9) . ? C17 C18 1.386(10) . ? C18 C19 1.381(10) . ? C19 C20 1.395(9) . ? C21 C22 1.383(9) . ? C21 C26 1.405(9) . ? C22 C23 1.403(10) . ? C23 C24 1.362(11) . ? C24 C25 1.394(12) . ? C25 C26 1.410(11) . ? C28 C33 1.388(9) . ? C28 C29 1.397(8) . ? C29 C30 1.415(9) . ? C30 C31 1.372(10) . ? C31 C32 1.386(10) . ? C32 C33 1.386(9) . ? C34 C39 1.379(8) . ? C34 C35 1.395(9) . ? C35 C36 1.388(10) . ? C36 C37 1.379(10) . ? C37 C38 1.375(10) . ? C38 C39 1.413(9) . ? C40 C41 1.477(16) . ? C41 C42 1.371(17) . ? C42 C43 1.441(18) . ? C44 C45 1.445(17) . ? C45 C46 1.473(17) . ? C46 C47 1.416(16) . ? C48 C49 1.395(15) . ? C49 C50 1.419(15) . ? C50 C51 1.462(13) . ? Li1 O4 1.885(18) 2_564 ? Li1 Li2 2.83(3) . ? Li1 Li2 3.23(3) 2_564 ? Li2 O4 1.985(19) 2_564 ? Li2 O2 2.07(2) 2_564 ? Li2 In2 2.99(2) 2_564 ? Li2 Li1 3.23(3) 2_564 ? C62 C63 1.28(2) . ? C62 C61 1.36(2) . ? C62 C61 2.03(2) 2_575 ? C61 C63 1.27(2) 2_575 ? C61 C62 2.03(2) 2_575 ? C63 C61 1.27(2) 2_575 ? 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 Si2 In1 Si3 110.00(6) . . ? Si2 In1 Si1 110.99(6) . . ? Si3 In1 Si1 113.19(6) . . ? Si2 In1 In2 107.03(4) . . ? Si3 In1 In2 110.49(4) . . ? Si1 In1 In2 104.87(4) . . ? O3 In2 O4 92.0(2) . . ? O3 In2 O2 88.1(2) . . ? O4 In2 O2 85.1(2) . . ? O3 In2 In1 125.45(15) . . ? O4 In2 In1 126.37(16) . . ? O2 In2 In1 127.38(14) . . ? O3 In2 Li2 95.5(4) . 2_564 ? O4 In2 Li2 41.6(4) . 2_564 ? O2 In2 Li2 44.0(4) . 2_564 ? In1 In2 Li2 139.1(4) . 2_564 ? O3 In2 Li1 59.2(5) . . ? O4 In2 Li1 92.7(3) . . ? O2 In2 Li1 29.6(5) . . ? In1 In2 Li1 137.7(3) . . ? Li2 In2 Li1 60.2(5) 2_564 . ? C1 Si1 C8 105.8(3) . . ? C1 Si1 C2 106.9(3) . . ? C8 Si1 C2 107.4(3) . . ? C1 Si1 In1 115.4(2) . . ? C8 Si1 In1 109.59(17) . . ? C2 Si1 In1 111.32(19) . . ? C14 Si2 C21 107.8(3) . . ? C14 Si2 C15 103.8(3) . . ? C21 Si2 C15 106.2(2) . . ? C14 Si2 In1 115.5(2) . . ? C21 Si2 In1 111.43(19) . . ? C15 Si2 In1 111.44(19) . . ? C27 Si3 C34 108.1(3) . . ? C27 Si3 C28 106.4(3) . . ? C34 Si3 C28 105.6(3) . . ? C27 Si3 In1 115.2(2) . . ? C34 Si3 In1 112.16(19) . . ? C28 Si3 In1 108.65(19) . . ? C40 O1 C43 106.5(9) . . ? C40 O1 Li1 125.0(7) . . ? C43 O1 Li1 124.5(8) . . ? Li1 O2 Li2 110.1(7) . 2_564 ? Li1 O2 In2 115.5(10) . . ? Li2 O2 In2 89.6(5) 2_564 . ? Li2 O3 In2 130.3(7) . . ? Li1 O4 Li2 94.0(11) 2_564 2_564 ? Li1 O4 In2 130.9(7) 2_564 . ? Li2 O4 In2 92.7(6) 2_564 . ? C44 O5 C47 111.2(10) . . ? C44 O5 Li1 128.6(11) . . ? C47 O5 Li1 112.7(8) . . ? C48 O6 C51 111.0(7) . . ? C48 O6 Li2 115.1(9) . . ? C51 O6 Li2 133.1(8) . . ? C3 C2 C7 117.1(6) . . ? C3 C2 Si1 122.1(5) . . ? C7 C2 Si1 120.8(4) . . ? C2 C3 C4 120.8(7) . . ? C5 C4 C3 121.2(7) . . ? C6 C5 C4 119.0(7) . . ? C5 C6 C7 120.5(7) . . ? C6 C7 C2 121.4(6) . . ? C13 C8 C9 115.6(5) . . ? C13 C8 Si1 121.4(5) . . ? C9 C8 Si1 122.8(5) . . ? C10 C9 C8 121.3(6) . . ? C9 C10 C11 121.5(7) . . ? C12 C11 C10 118.0(6) . . ? C13 C12 C11 119.9(7) . . ? C12 C13 C8 123.7(6) . . ? C20 C15 C16 117.0(5) . . ? C20 C15 Si2 123.5(5) . . ? C16 C15 Si2 119.5(4) . . ? C17 C16 C15 120.9(6) . . ? C16 C17 C18 121.1(7) . . ? C19 C18 C17 119.4(6) . . ? C18 C19 C20 120.1(6) . . ? C19 C20 C15 121.4(6) . . ? C22 C21 C26 115.8(6) . . ? C22 C21 Si2 123.1(5) . . ? C26 C21 Si2 121.0(5) . . ? C21 C22 C23 123.1(7) . . ? C24 C23 C22 120.0(8) . . ? C23 C24 C25 119.8(7) . . ? C24 C25 C26 119.3(8) . . ? C21 C26 C25 122.0(8) . . ? C33 C28 C29 117.2(6) . . ? C33 C28 Si3 123.4(4) . . ? C29 C28 Si3 119.3(5) . . ? C28 C29 C30 120.5(6) . . ? C31 C30 C29 120.7(6) . . ? C30 C31 C32 119.0(7) . . ? C31 C32 C33 120.3(7) . . ? C32 C33 C28 122.2(6) . . ? C39 C34 C35 117.4(6) . . ? C39 C34 Si3 121.8(5) . . ? C35 C34 Si3 120.9(4) . . ? C36 C35 C34 121.1(6) . . ? C37 C36 C35 120.7(7) . . ? C38 C37 C36 119.4(6) . . ? C37 C38 C39 119.5(6) . . ? C34 C39 C38 121.7(7) . . ? O1 C40 C41 107.6(9) . . ? C42 C41 C40 104.0(11) . . ? C41 C42 C43 108.0(13) . . ? O1 C43 C42 106.1(10) . . ? O5 C44 C45 104.8(12) . . ? C44 C45 C46 106.8(11) . . ? C47 C46 C45 108.7(11) . . ? C46 C47 O5 100.5(9) . . ? O6 C48 C49 107.1(10) . . ? C48 C49 C50 110.2(11) . . ? C49 C50 C51 103.8(10) . . ? O6 C51 C50 106.9(8) . . ? O2 Li1 O4 122.9(10) . 2_564 ? O2 Li1 O1 115.4(8) . . ? O4 Li1 O1 111.9(11) 2_564 . ? O2 Li1 O5 101.4(13) . . ? O4 Li1 O5 100.6(9) 2_564 . ? O1 Li1 O5 99.3(9) . . ? O2 Li1 Li2 98.3(10) . . ? O4 Li1 Li2 44.4(7) 2_564 . ? O1 Li1 Li2 98.0(12) . . ? O5 Li1 Li2 144.9(8) . . ? O2 Li1 Li2 37.1(5) . 2_564 ? O4 Li1 Li2 88.0(7) 2_564 2_564 ? O1 Li1 Li2 150.5(9) . 2_564 ? O5 Li1 Li2 98.0(9) . 2_564 ? Li2 Li1 Li2 80.8(8) . 2_564 ? O2 Li1 In2 34.9(5) . . ? O4 Li1 In2 109.7(10) 2_564 . ? O1 Li1 In2 98.2(8) . . ? O5 Li1 In2 136.0(9) . . ? Li2 Li1 In2 70.4(7) . . ? Li2 Li1 In2 53.4(5) 2_564 . ? O3 Li2 O4 116.2(9) . 2_564 ? O3 Li2 O6 107.3(11) . . ? O4 Li2 O6 121.1(9) 2_564 . ? O3 Li2 O2 114.9(9) . 2_564 ? O4 Li2 O2 91.4(9) 2_564 2_564 ? O6 Li2 O2 104.6(9) . 2_564 ? O3 Li2 Li1 74.7(7) . . ? O4 Li2 Li1 41.6(5) 2_564 . ? O6 Li2 Li1 138.2(10) . . ? O2 Li2 Li1 112.2(10) 2_564 . ? O3 Li2 In2 134.2(9) . 2_564 ? O4 Li2 In2 45.6(5) 2_564 2_564 ? O6 Li2 In2 117.5(8) . 2_564 ? O2 Li2 In2 46.4(5) 2_564 2_564 ? Li1 Li2 In2 77.9(6) . 2_564 ? O3 Li2 Li1 82.6(7) . 2_564 ? O4 Li2 Li1 101.2(10) 2_564 2_564 ? O6 Li2 Li1 122.6(9) . 2_564 ? O2 Li2 Li1 32.8(4) 2_564 2_564 ? Li1 Li2 Li1 99.2(8) . 2_564 ? In2 Li2 Li1 66.3(6) 2_564 2_564 ? C63 C62 C61 119.9(19) . . ? C63 C62 C61 36.9(12) . 2_575 ? C61 C62 C61 90.1(13) . 2_575 ? C63 C61 C62 120(2) 2_575 . ? C63 C61 C62 37.2(10) 2_575 2_575 ? C62 C61 C62 89.9(13) . 2_575 ? C61 C63 C62 105.9(19) 2_575 . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 23.90 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.940 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.113 # Attachment 'comp_10__728998.cif' data_km20abs_comp10 _database_code_depnum_ccdc_archive 'CCDC 728998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H57 In Si3' _chemical_formula_weight 833.03 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' Si Si 0.0817 0.0704 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.999(2) _cell_length_b 11.893(2) _cell_length_c 18.651(4) _cell_angle_alpha 87.01(3) _cell_angle_beta 86.06(3) _cell_angle_gamma 78.24(3) _cell_volume 2164.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8035 _exptl_absorpt_correction_T_max 0.8931 _exptl_absorpt_process_details '13 faces' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'image plate, 2 circle goniometer' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20226 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9234 _reflns_number_gt 6542 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement STOE _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0348P)^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 9234 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.834 _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 0.66866(2) 0.71044(2) 0.739211(12) 0.02552(7) Uani 1 1 d . . . Si1 Si 0.74311(9) 0.82185(8) 0.62614(5) 0.0317(2) Uani 1 1 d . . . Si2 Si 0.55926(8) 0.81052(7) 0.85681(4) 0.02509(18) Uani 1 1 d . . . Si3 Si 0.75317(8) 0.48624(7) 0.74181(5) 0.02677(18) Uani 1 1 d . . . C1 C 0.6762(4) 0.9820(3) 0.6181(2) 0.0469(9) Uani 1 1 d . . . C2 C 0.6985(6) 1.0388(4) 0.6852(3) 0.0813(16) Uani 1 1 d . . . H2A H 0.6628 1.1217 0.6801 0.122 Uiso 1 1 calc R . . H2B H 0.7966 1.0248 0.6928 0.122 Uiso 1 1 calc R . . H2C H 0.6506 1.0068 0.7266 0.122 Uiso 1 1 calc R . . C3 C 0.5233(5) 1.0052(4) 0.6056(3) 0.0703(14) Uani 1 1 d . . . H3A H 0.4896 1.0880 0.5980 0.105 Uiso 1 1 calc R . . H3B H 0.4737 0.9771 0.6477 0.105 Uiso 1 1 calc R . . H3C H 0.5085 0.9653 0.5631 0.105 Uiso 1 1 calc R . . C4 C 0.7503(5) 1.0340(4) 0.5548(3) 0.0725(14) Uani 1 1 d . . . H4A H 0.7128 1.1167 0.5502 0.109 Uiso 1 1 calc R . . H4B H 0.7376 0.9973 0.5106 0.109 Uiso 1 1 calc R . . H4C H 0.8481 1.0215 0.5629 0.109 Uiso 1 1 calc R . . C5 C 0.9329(3) 0.7957(3) 0.63547(18) 0.0361(8) Uani 1 1 d . . . C6 C 1.0339(4) 0.7700(4) 0.5806(2) 0.0554(11) Uani 1 1 d . . . H6A H 1.0080 0.7643 0.5331 0.066 Uiso 1 1 calc R . . C7 C 1.1700(4) 0.7525(5) 0.5934(2) 0.0666(13) Uani 1 1 d . . . H7A H 1.2366 0.7359 0.5545 0.080 Uiso 1 1 calc R . . C8 C 1.2111(4) 0.7586(4) 0.6607(2) 0.0624(12) Uani 1 1 d . . . H8A H 1.3058 0.7450 0.6692 0.075 Uiso 1 1 calc R . . C9 C 1.1156(4) 0.7842(4) 0.7158(2) 0.0629(13) Uani 1 1 d . . . H9A H 1.1430 0.7896 0.7630 0.076 Uiso 1 1 calc R . . C10 C 0.9801(4) 0.8021(4) 0.70311(19) 0.0495(10) Uani 1 1 d . . . H10A H 0.9148 0.8198 0.7424 0.059 Uiso 1 1 calc R . . C11 C 0.6921(3) 0.7544(3) 0.54589(17) 0.0332(7) Uani 1 1 d . . . C12 C 0.7547(4) 0.7573(4) 0.47784(19) 0.0500(10) Uani 1 1 d . . . H12A H 0.8309 0.7937 0.4696 0.060 Uiso 1 1 calc R . . C13 C 0.7079(4) 0.7078(4) 0.4211(2) 0.0604(12) Uani 1 1 d . . . H13A H 0.7541 0.7094 0.3749 0.072 Uiso 1 1 calc R . . C14 C 0.5977(4) 0.6574(4) 0.4302(2) 0.0584(11) Uani 1 1 d . . . H14A H 0.5668 0.6233 0.3912 0.070 Uiso 1 1 calc R . . C15 C 0.5321(4) 0.6565(4) 0.4969(2) 0.0547(11) Uani 1 1 d . . . H15A H 0.4531 0.6235 0.5043 0.066 Uiso 1 1 calc R . . C16 C 0.5799(4) 0.7029(3) 0.5527(2) 0.0449(9) Uani 1 1 d . . . H16A H 0.5335 0.6997 0.5987 0.054 Uiso 1 1 calc R . . C17 C 0.4983(3) 0.7108(3) 0.92937(17) 0.0306(7) Uani 1 1 d . . . C18 C 0.4772(5) 0.7649(4) 1.0017(2) 0.0624(12) Uani 1 1 d . . . H18A H 0.4477 0.7111 1.0380 0.094 Uiso 1 1 calc R . . H18B H 0.4070 0.8355 0.9993 0.094 Uiso 1 1 calc R . . H18C H 0.5633 0.7833 1.0148 0.094 Uiso 1 1 calc R . . C19 C 0.6016(4) 0.5981(3) 0.9342(2) 0.0567(12) Uani 1 1 d . . . H19A H 0.5652 0.5444 0.9681 0.085 Uiso 1 1 calc R . . H19B H 0.6873 0.6121 0.9509 0.085 Uiso 1 1 calc R . . H19C H 0.6190 0.5649 0.8866 0.085 Uiso 1 1 calc R . . C20 C 0.3635(4) 0.6853(4) 0.9090(2) 0.0535(11) Uani 1 1 d . . . H20A H 0.3304 0.6346 0.9462 0.080 Uiso 1 1 calc R . . H20B H 0.3770 0.6474 0.8629 0.080 Uiso 1 1 calc R . . H20C H 0.2960 0.7573 0.9047 0.080 Uiso 1 1 calc R . . C21 C 0.4135(3) 0.9368(3) 0.84541(17) 0.0280(7) Uani 1 1 d . . . C22 C 0.3672(3) 1.0134(3) 0.89955(19) 0.0365(8) Uani 1 1 d . . . H22A H 0.4156 1.0060 0.9422 0.044 Uiso 1 1 calc R . . C23 C 0.2532(3) 1.1000(3) 0.8935(2) 0.0441(9) Uani 1 1 d . . . H23A H 0.2236 1.1507 0.9317 0.053 Uiso 1 1 calc R . . C24 C 0.1835(4) 1.1126(3) 0.8327(2) 0.0489(10) Uani 1 1 d . . . H24A H 0.1053 1.1727 0.8283 0.059 Uiso 1 1 calc R . . C25 C 0.2249(4) 1.0399(4) 0.7781(2) 0.0501(10) Uani 1 1 d . . . H25A H 0.1758 1.0488 0.7357 0.060 Uiso 1 1 calc R . . C26 C 0.3397(3) 0.9523(3) 0.78453(19) 0.0390(8) Uani 1 1 d . . . H26A H 0.3679 0.9019 0.7461 0.047 Uiso 1 1 calc R . . C27 C 0.7141(3) 0.8622(3) 0.88397(15) 0.0272(6) Uani 1 1 d . . . C28 C 0.8362(3) 0.7826(3) 0.89191(18) 0.0377(8) Uani 1 1 d . . . H28A H 0.8370 0.7032 0.8877 0.045 Uiso 1 1 calc R . . C29 C 0.9552(4) 0.8163(4) 0.90564(19) 0.0487(10) Uani 1 1 d . . . H29A H 1.0366 0.7602 0.9114 0.058 Uiso 1 1 calc R . . C30 C 0.9565(4) 0.9290(4) 0.9110(2) 0.0564(12) Uani 1 1 d . . . H30A H 1.0390 0.9521 0.9203 0.068 Uiso 1 1 calc R . . C31 C 0.8395(4) 1.0097(4) 0.9031(2) 0.0570(11) Uani 1 1 d . . . H31A H 0.8405 1.0888 0.9071 0.068 Uiso 1 1 calc R . . C32 C 0.7195(4) 0.9764(3) 0.88908(19) 0.0402(8) Uani 1 1 d . . . H32A H 0.6391 1.0335 0.8829 0.048 Uiso 1 1 calc R . . C33 C 0.8552(3) 0.4159(3) 0.65963(18) 0.0340(7) Uani 1 1 d . . . C34 C 0.7578(4) 0.4059(4) 0.6021(2) 0.0610(12) Uani 1 1 d . . . H34A H 0.8103 0.3721 0.5595 0.092 Uiso 1 1 calc R . . H34B H 0.7057 0.4825 0.5891 0.092 Uiso 1 1 calc R . . H34C H 0.6946 0.3568 0.6208 0.092 Uiso 1 1 calc R . . C35 C 0.9302(4) 0.2945(3) 0.6801(2) 0.0484(9) Uani 1 1 d . . . H35A H 0.9796 0.2583 0.6374 0.073 Uiso 1 1 calc R . . H35B H 0.8637 0.2490 0.6997 0.073 Uiso 1 1 calc R . . H35C H 0.9953 0.2983 0.7164 0.073 Uiso 1 1 calc R . . C36 C 0.9571(4) 0.4861(4) 0.6300(2) 0.0536(10) Uani 1 1 d . . . H36A H 1.0123 0.4467 0.5898 0.080 Uiso 1 1 calc R . . H36B H 1.0169 0.4955 0.6677 0.080 Uiso 1 1 calc R . . H36C H 0.9084 0.5618 0.6130 0.080 Uiso 1 1 calc R . . C37 C 0.5918(3) 0.4275(3) 0.75655(17) 0.0299(7) Uani 1 1 d . . . C38 C 0.5878(3) 0.3143(3) 0.77654(19) 0.0397(8) Uani 1 1 d . . . H38A H 0.6706 0.2615 0.7851 0.048 Uiso 1 1 calc R . . C39 C 0.4652(4) 0.2770(3) 0.7842(2) 0.0457(9) Uani 1 1 d . . . H39A H 0.4645 0.1995 0.7992 0.055 Uiso 1 1 calc R . . C40 C 0.3451(4) 0.3504(3) 0.7703(2) 0.0484(10) Uani 1 1 d . . . H40A H 0.2612 0.3242 0.7758 0.058 Uiso 1 1 calc R . . C41 C 0.3463(3) 0.4610(3) 0.7487(2) 0.0465(9) Uani 1 1 d . . . H41A H 0.2634 0.5122 0.7380 0.056 Uiso 1 1 calc R . . C42 C 0.4677(3) 0.4985(3) 0.74246(19) 0.0369(8) Uani 1 1 d . . . H42A H 0.4666 0.5764 0.7279 0.044 Uiso 1 1 calc R . . C43 C 0.8665(3) 0.4476(3) 0.81985(17) 0.0304(7) Uani 1 1 d . . . C44 C 0.8441(4) 0.3693(3) 0.87471(19) 0.0433(9) Uani 1 1 d . . . H44A H 0.7690 0.3318 0.8737 0.052 Uiso 1 1 calc R . . C45 C 0.9294(4) 0.3453(4) 0.9307(2) 0.0512(10) Uani 1 1 d . . . H45A H 0.9111 0.2923 0.9681 0.061 Uiso 1 1 calc R . . C46 C 1.0370(4) 0.3945(4) 0.9337(2) 0.0545(11) Uani 1 1 d . . . H46A H 1.0965 0.3743 0.9719 0.065 Uiso 1 1 calc R . . C47 C 1.0617(4) 0.4741(4) 0.8818(2) 0.0518(10) Uani 1 1 d . . . H47A H 1.1368 0.5112 0.8843 0.062 Uiso 1 1 calc R . . C48 C 0.9756(3) 0.5002(3) 0.82525(19) 0.0404(8) Uani 1 1 d . . . H48A H 0.9927 0.5560 0.7893 0.048 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 0.02753(11) 0.02657(12) 0.02290(11) -0.00148(9) -0.00043(7) -0.00666(8) Si1 0.0399(5) 0.0306(5) 0.0242(4) -0.0001(4) 0.0020(4) -0.0074(4) Si2 0.0283(4) 0.0246(4) 0.0229(4) -0.0020(4) 0.0009(3) -0.0069(3) Si3 0.0270(4) 0.0256(4) 0.0277(4) -0.0018(4) -0.0019(3) -0.0048(3) C1 0.069(2) 0.032(2) 0.036(2) 0.0048(17) 0.0060(17) -0.0084(17) C2 0.137(5) 0.034(2) 0.067(3) -0.012(3) 0.004(3) -0.005(3) C3 0.078(3) 0.053(3) 0.065(3) 0.010(2) 0.006(2) 0.017(2) C4 0.099(4) 0.045(3) 0.066(3) 0.023(2) 0.016(3) -0.011(2) C5 0.0456(19) 0.0350(19) 0.0310(17) 0.0017(16) -0.0023(14) -0.0162(15) C6 0.046(2) 0.086(3) 0.0328(19) -0.007(2) 0.0000(16) -0.011(2) C7 0.043(2) 0.102(4) 0.053(3) -0.008(3) 0.0052(19) -0.011(2) C8 0.046(2) 0.083(3) 0.061(3) 0.000(3) -0.010(2) -0.018(2) C9 0.062(3) 0.095(4) 0.042(2) 0.006(2) -0.0151(19) -0.037(2) C10 0.057(2) 0.069(3) 0.0300(18) -0.0054(19) -0.0016(16) -0.031(2) C11 0.0367(17) 0.0345(18) 0.0271(16) -0.0030(15) -0.0014(13) -0.0037(14) C12 0.041(2) 0.078(3) 0.0328(19) -0.011(2) 0.0014(15) -0.0148(19) C13 0.046(2) 0.097(4) 0.037(2) -0.023(2) -0.0020(17) -0.005(2) C14 0.048(2) 0.068(3) 0.058(3) -0.028(2) -0.0171(19) 0.002(2) C15 0.050(2) 0.062(3) 0.055(3) -0.001(2) -0.0130(19) -0.0146(19) C16 0.045(2) 0.055(2) 0.0357(19) 0.0007(19) -0.0038(15) -0.0132(17) C17 0.0353(16) 0.0288(17) 0.0281(16) -0.0022(14) 0.0037(12) -0.0085(13) C18 0.106(3) 0.058(3) 0.0273(19) -0.005(2) 0.017(2) -0.034(2) C19 0.051(2) 0.044(2) 0.064(3) 0.027(2) 0.0183(19) 0.0013(17) C20 0.047(2) 0.059(3) 0.059(3) 0.011(2) 0.0017(18) -0.0241(18) C21 0.0272(15) 0.0248(16) 0.0314(16) -0.0014(14) 0.0013(12) -0.0054(12) C22 0.0360(17) 0.0342(19) 0.0382(18) -0.0007(16) -0.0009(14) -0.0053(14) C23 0.0398(19) 0.034(2) 0.057(2) -0.0048(19) 0.0076(17) -0.0073(15) C24 0.0325(18) 0.038(2) 0.071(3) 0.010(2) 0.0052(17) -0.0017(15) C25 0.039(2) 0.057(3) 0.052(2) 0.010(2) -0.0108(17) -0.0072(17) C26 0.0357(17) 0.044(2) 0.0364(18) -0.0016(17) -0.0029(14) -0.0050(15) C27 0.0321(15) 0.0318(17) 0.0196(14) -0.0015(13) 0.0009(11) -0.0117(12) C28 0.0366(18) 0.044(2) 0.0333(18) 0.0027(16) -0.0011(14) -0.0109(15) C29 0.0345(18) 0.073(3) 0.039(2) 0.015(2) -0.0044(15) -0.0154(18) C30 0.045(2) 0.088(3) 0.048(2) 0.004(2) -0.0070(17) -0.040(2) C31 0.067(3) 0.051(3) 0.063(3) -0.002(2) -0.007(2) -0.034(2) C32 0.0438(19) 0.037(2) 0.043(2) -0.0049(17) -0.0019(15) -0.0146(15) C33 0.0340(16) 0.0312(18) 0.0356(18) -0.0069(15) 0.0005(13) -0.0028(13) C34 0.059(2) 0.079(3) 0.040(2) -0.023(2) -0.0081(18) 0.006(2) C35 0.052(2) 0.037(2) 0.051(2) -0.0101(19) 0.0094(17) 0.0037(16) C36 0.060(2) 0.051(2) 0.048(2) -0.011(2) 0.0230(18) -0.0137(19) C37 0.0344(16) 0.0272(16) 0.0294(16) -0.0062(14) -0.0006(12) -0.0083(13) C38 0.0430(19) 0.0316(19) 0.044(2) -0.0036(17) 0.0008(15) -0.0073(14) C39 0.053(2) 0.038(2) 0.050(2) -0.0050(19) 0.0065(17) -0.0209(17) C40 0.041(2) 0.051(2) 0.059(2) -0.011(2) 0.0058(17) -0.0232(17) C41 0.0321(18) 0.047(2) 0.060(2) -0.007(2) -0.0005(16) -0.0070(15) C42 0.0369(18) 0.0331(19) 0.043(2) -0.0049(17) -0.0031(14) -0.0109(14) C43 0.0292(15) 0.0297(17) 0.0295(16) -0.0025(14) -0.0035(12) 0.0015(12) C44 0.046(2) 0.041(2) 0.040(2) 0.0031(18) -0.0056(15) -0.0017(16) C45 0.056(2) 0.054(3) 0.037(2) 0.0019(19) -0.0076(17) 0.0048(19) C46 0.055(2) 0.059(3) 0.040(2) -0.011(2) -0.0166(18) 0.017(2) C47 0.0372(19) 0.066(3) 0.052(2) -0.022(2) -0.0072(17) -0.0033(18) C48 0.0366(18) 0.047(2) 0.0376(19) -0.0073(18) -0.0036(14) -0.0067(15) _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 Si1 2.5793(11) . ? In1 Si2 2.6145(12) . ? In1 Si3 2.6268(11) . ? Si1 C5 1.878(3) . ? Si1 C11 1.881(4) . ? Si1 C1 1.888(4) . ? Si2 C21 1.882(3) . ? Si2 C27 1.887(3) . ? Si2 C17 1.904(3) . ? Si3 C37 1.883(3) . ? Si3 C43 1.886(3) . ? Si3 C33 1.914(3) . ? C1 C2 1.503(6) . ? C1 C4 1.522(5) . ? C1 C3 1.530(6) . ? C5 C10 1.388(5) . ? C5 C6 1.388(5) . ? C6 C7 1.369(5) . ? C7 C8 1.359(6) . ? C8 C9 1.356(6) . ? C9 C10 1.364(5) . ? C11 C12 1.378(5) . ? C11 C16 1.380(5) . ? C12 C13 1.389(6) . ? C13 C14 1.356(6) . ? C14 C15 1.366(6) . ? C15 C16 1.360(6) . ? C17 C18 1.508(5) . ? C17 C20 1.518(5) . ? C17 C19 1.519(5) . ? C21 C26 1.381(4) . ? C21 C22 1.387(5) . ? C22 C23 1.378(5) . ? C23 C24 1.358(6) . ? C24 C25 1.358(6) . ? C25 C26 1.391(5) . ? C27 C32 1.379(5) . ? C27 C28 1.395(4) . ? C28 C29 1.374(5) . ? C29 C30 1.353(6) . ? C30 C31 1.365(6) . ? C31 C32 1.382(5) . ? C33 C36 1.504(5) . ? C33 C34 1.523(5) . ? C33 C35 1.527(5) . ? C37 C42 1.384(4) . ? C37 C38 1.386(5) . ? C38 C39 1.383(5) . ? C39 C40 1.364(5) . ? C40 C41 1.358(5) . ? C41 C42 1.373(5) . ? C43 C48 1.376(5) . ? C43 C44 1.386(5) . ? C44 C45 1.375(5) . ? C45 C46 1.331(6) . ? C46 C47 1.364(6) . ? C47 C48 1.390(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 In1 Si2 123.14(3) . . ? Si1 In1 Si3 116.35(4) . . ? Si2 In1 Si3 119.39(4) . . ? C5 Si1 C11 114.05(15) . . ? C5 Si1 C1 108.35(17) . . ? C11 Si1 C1 108.39(16) . . ? C5 Si1 In1 100.45(10) . . ? C11 Si1 In1 107.24(11) . . ? C1 Si1 In1 118.44(12) . . ? C21 Si2 C27 109.57(14) . . ? C21 Si2 C17 106.59(14) . . ? C27 Si2 C17 111.28(13) . . ? C21 Si2 In1 116.32(11) . . ? C27 Si2 In1 97.98(10) . . ? C17 Si2 In1 114.89(11) . . ? C37 Si3 C43 111.78(14) . . ? C37 Si3 C33 108.13(15) . . ? C43 Si3 C33 106.47(14) . . ? C37 Si3 In1 104.51(10) . . ? C43 Si3 In1 106.92(11) . . ? C33 Si3 In1 119.12(11) . . ? C2 C1 C4 108.4(4) . . ? C2 C1 C3 109.6(4) . . ? C4 C1 C3 108.8(3) . . ? C2 C1 Si1 110.7(3) . . ? C4 C1 Si1 110.1(3) . . ? C3 C1 Si1 109.3(3) . . ? C10 C5 C6 115.2(3) . . ? C10 C5 Si1 118.4(3) . . ? C6 C5 Si1 126.3(3) . . ? C7 C6 C5 121.6(4) . . ? C8 C7 C6 121.0(4) . . ? C9 C8 C7 119.3(4) . . ? C8 C9 C10 119.8(4) . . ? C9 C10 C5 123.1(4) . . ? C12 C11 C16 115.8(3) . . ? C12 C11 Si1 124.8(3) . . ? C16 C11 Si1 119.4(3) . . ? C11 C12 C13 120.9(4) . . ? C14 C13 C12 121.4(4) . . ? C13 C14 C15 118.5(4) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C11 123.4(4) . . ? C18 C17 C20 108.9(3) . . ? C18 C17 C19 109.5(3) . . ? C20 C17 C19 108.3(3) . . ? C18 C17 Si2 111.4(2) . . ? C20 C17 Si2 108.6(2) . . ? C19 C17 Si2 110.0(2) . . ? C26 C21 C22 116.4(3) . . ? C26 C21 Si2 121.2(3) . . ? C22 C21 Si2 122.2(2) . . ? C23 C22 C21 122.1(3) . . ? C24 C23 C22 119.8(4) . . ? C25 C24 C23 120.3(3) . . ? C24 C25 C26 119.7(4) . . ? C21 C26 C25 121.7(4) . . ? C32 C27 C28 116.7(3) . . ? C32 C27 Si2 124.0(2) . . ? C28 C27 Si2 118.9(3) . . ? C29 C28 C27 121.6(4) . . ? C30 C29 C28 120.1(4) . . ? C29 C30 C31 120.1(3) . . ? C30 C31 C32 120.1(4) . . ? C27 C32 C31 121.4(4) . . ? C36 C33 C34 109.6(3) . . ? C36 C33 C35 109.6(3) . . ? C34 C33 C35 107.6(3) . . ? C36 C33 Si3 110.3(3) . . ? C34 C33 Si3 109.5(2) . . ? C35 C33 Si3 110.1(2) . . ? C42 C37 C38 116.2(3) . . ? C42 C37 Si3 119.1(2) . . ? C38 C37 Si3 124.6(2) . . ? C39 C38 C37 121.1(3) . . ? C40 C39 C38 120.6(3) . . ? C41 C40 C39 119.6(3) . . ? C40 C41 C42 119.7(3) . . ? C41 C42 C37 122.7(3) . . ? C48 C43 C44 116.7(3) . . ? C48 C43 Si3 120.1(2) . . ? C44 C43 Si3 123.2(3) . . ? C45 C44 C43 120.6(4) . . ? C46 C45 C44 121.6(4) . . ? C45 C46 C47 119.9(3) . . ? C46 C47 C48 119.1(4) . . ? C43 C48 C47 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.637 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.079