# Electronic Supplementary Material (ESI) for Nanoscale # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1542 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Wang, Xun' 'Xu, Biao' 'Wang, Ruji' _publ_contact_author_name 'Prof. Xun Wang' _publ_contact_author_email wangxun@mail.tsinghua.edu.cn _publ_section_title ; Simplifying the Growth of Hybrid Single Crystals by Using Nanoparticle Precursors: the Case of AgI ; # Attachment '- 2.cif' data_shelx _database_code_depnum_ccdc_archive 'CCDC 863848' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C13 H22 N), Ag4 I8' _chemical_formula_sum 'C52 H88 Ag4 I8 N4' _chemical_formula_weight 2215.94 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0164(8) _cell_length_b 12.4022(9) _cell_length_c 14.8694(10) _cell_angle_alpha 89.2116(19) _cell_angle_beta 73.399(2) _cell_angle_gamma 73.308(2) _cell_volume 1690.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7683 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 4.827 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.122 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 RAXIS-RAPID _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16829 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7683 _reflns_number_gt 4281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku' _computing_cell_refinement 'CrystalClear, Rigaku' _computing_data_reduction 'CrystalClear, Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _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^)+(0.0050P)^2^+20.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0040(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7683 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.93137(13) 0.42069(10) 0.60166(7) 0.0650(3) Uani 1 1 d . . . Ag2 Ag 0.80093(13) 0.26857(10) 0.79514(7) 0.0632(3) Uani 1 1 d . . . I1 I 0.81422(10) 0.49103(7) 0.80363(6) 0.0533(3) Uani 1 1 d . . . I2 I 0.89995(10) 0.19362(7) 0.60808(6) 0.0546(3) Uani 1 1 d . . . I3 I 0.78175(10) 0.56243(8) 0.48437(6) 0.0515(3) Uani 1 1 d . . . I4 I 0.71295(14) 0.16186(9) 0.94931(6) 0.0720(3) Uani 1 1 d . . . N1 N 0.3057(10) 0.5481(8) 0.8213(6) 0.038(2) Uani 1 1 d . . . N2 N 0.3185(10) 0.1041(7) 0.2840(6) 0.035(2) Uani 1 1 d . . . C1 C 0.3140(13) 0.7311(9) 0.7409(8) 0.040(3) Uani 1 1 d . . . C2 C 0.2129(15) 0.8345(11) 0.7795(9) 0.054(3) Uani 1 1 d . . . H2A H 0.1800 0.8491 0.8446 0.065 Uiso 1 1 calc R . . C3 C 0.1617(18) 0.9141(12) 0.7248(11) 0.067(4) Uani 1 1 d . . . H3A H 0.0947 0.9825 0.7528 0.080 Uiso 1 1 calc R . . C4 C 0.2069(17) 0.8958(12) 0.6289(12) 0.067(4) Uani 1 1 d . . . H4A H 0.1697 0.9506 0.5919 0.080 Uiso 1 1 calc R . . C5 C 0.3096(16) 0.7939(13) 0.5871(10) 0.063(4) Uani 1 1 d . . . H5A H 0.3415 0.7804 0.5219 0.075 Uiso 1 1 calc R . . C6 C 0.3627(15) 0.7145(11) 0.6425(8) 0.052(3) Uani 1 1 d . . . H6A H 0.4330 0.6476 0.6143 0.062 Uiso 1 1 calc R . . C7 C 0.3709(13) 0.6461(10) 0.8026(9) 0.047(3) Uani 1 1 d . . . H7A H 0.3553 0.6848 0.8626 0.056 Uiso 1 1 calc R . . H7B H 0.4754 0.6151 0.7746 0.056 Uiso 1 1 calc R . . C8 C 0.3701(15) 0.4823(10) 0.8913(8) 0.049(3) Uani 1 1 d . . . H8A H 0.3447 0.5316 0.9476 0.058 Uiso 1 1 calc R . . H8B H 0.4754 0.4592 0.8656 0.058 Uiso 1 1 calc R . . C9 C 0.3214(19) 0.3774(12) 0.9194(10) 0.073(5) Uani 1 1 d . . . H9A H 0.3698 0.3392 0.9631 0.110 Uiso 1 1 calc R . . H9B H 0.3462 0.3276 0.8643 0.110 Uiso 1 1 calc R . . H9C H 0.2178 0.3994 0.9482 0.110 Uiso 1 1 calc R . . C10 C 0.1410(13) 0.5901(11) 0.8563(8) 0.047(3) Uani 1 1 d . . . H10A H 0.1037 0.5259 0.8575 0.056 Uiso 1 1 calc R . . H10B H 0.1065 0.6396 0.8114 0.056 Uiso 1 1 calc R . . C11 C 0.0766(16) 0.6529(12) 0.9527(9) 0.065(4) Uani 1 1 d . . . H11A H -0.0279 0.6757 0.9686 0.097 Uiso 1 1 calc R . . H11B H 0.1096 0.7183 0.9522 0.097 Uiso 1 1 calc R . . H11C H 0.1073 0.6043 0.9985 0.097 Uiso 1 1 calc R . . C12 C 0.3417(14) 0.4754(11) 0.7304(7) 0.048(3) Uani 1 1 d . . . H12A H 0.2888 0.4198 0.7437 0.058 Uiso 1 1 calc R . . H12B H 0.3055 0.5234 0.6852 0.058 Uiso 1 1 calc R . . C13 C 0.5002(17) 0.4145(12) 0.6851(9) 0.071(4) Uani 1 1 d . . . H13A H 0.5104 0.3697 0.6300 0.107 Uiso 1 1 calc R . . H13B H 0.5379 0.3663 0.7287 0.107 Uiso 1 1 calc R . . H13C H 0.5534 0.4685 0.6676 0.107 Uiso 1 1 calc R . . C14 C 0.5383(13) -0.0745(9) 0.2308(7) 0.038(3) Uani 1 1 d . . . C15 C 0.6049(16) -0.1401(10) 0.2932(8) 0.052(3) Uani 1 1 d . . . H15A H 0.5478 -0.1483 0.3529 0.062 Uiso 1 1 calc R . . C16 C 0.7542(17) -0.1927(13) 0.2671(10) 0.066(4) Uani 1 1 d . . . H16A H 0.7965 -0.2358 0.3091 0.079 Uiso 1 1 calc R . . C17 C 0.8384(17) -0.1810(12) 0.1802(11) 0.063(4) Uani 1 1 d . . . H17A H 0.9386 -0.2156 0.1634 0.076 Uiso 1 1 calc R . . C18 C 0.7769(16) -0.1181(12) 0.1159(9) 0.058(4) Uani 1 1 d . . . H18A H 0.8357 -0.1119 0.0563 0.070 Uiso 1 1 calc R . . C19 C 0.6268(14) -0.0642(10) 0.1410(8) 0.050(3) Uani 1 1 d . . . H19A H 0.5857 -0.0217 0.0983 0.060 Uiso 1 1 calc R . . C20 C 0.3787(13) -0.0226(9) 0.2587(8) 0.041(3) Uani 1 1 d . . . H20A H 0.3363 -0.0599 0.3125 0.049 Uiso 1 1 calc R . . H20B H 0.3440 -0.0395 0.2075 0.049 Uiso 1 1 calc R . . C21 C 0.3630(15) 0.1703(10) 0.2013(8) 0.049(3) Uani 1 1 d . . . H21A H 0.4686 0.1475 0.1782 0.059 Uiso 1 1 calc R . . H21B H 0.3307 0.2496 0.2229 0.059 Uiso 1 1 calc R . . C22 C 0.3040(18) 0.1576(13) 0.1191(8) 0.069(4) Uani 1 1 d . . . H22A H 0.3386 0.2024 0.0697 0.104 Uiso 1 1 calc R . . H22B H 0.1993 0.1826 0.1401 0.104 Uiso 1 1 calc R . . H22C H 0.3370 0.0797 0.0958 0.104 Uiso 1 1 calc R . . C23 C 0.3823(14) 0.1345(11) 0.3578(8) 0.048(3) Uani 1 1 d . . . H23A H 0.4878 0.1068 0.3336 0.058 Uiso 1 1 calc R . . H23B H 0.3558 0.2162 0.3661 0.058 Uiso 1 1 calc R . . C24 C 0.3362(17) 0.0901(14) 0.4531(9) 0.071(4) Uani 1 1 d . . . H24A H 0.3802 0.1158 0.4947 0.106 Uiso 1 1 calc R . . H24B H 0.3670 0.0090 0.4468 0.106 Uiso 1 1 calc R . . H24C H 0.2320 0.1170 0.4784 0.106 Uiso 1 1 calc R . . C25 C 0.1564(12) 0.1321(9) 0.3196(8) 0.040(3) Uani 1 1 d . . . H25A H 0.1322 0.0909 0.3749 0.047 Uiso 1 1 calc R . . H25B H 0.1230 0.1042 0.2721 0.047 Uiso 1 1 calc R . . C26 C 0.0707(13) 0.2562(10) 0.3453(9) 0.052(3) Uani 1 1 d . . . H26A H -0.0317 0.2637 0.3676 0.077 Uiso 1 1 calc R . . H26B H 0.0898 0.2981 0.2907 0.077 Uiso 1 1 calc R . . H26C H 0.1000 0.2850 0.3938 0.077 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 Ag1 0.0669(8) 0.0702(8) 0.0558(6) 0.0115(5) -0.0110(5) -0.0245(6) Ag2 0.0640(8) 0.0722(8) 0.0563(6) 0.0127(5) -0.0174(5) -0.0253(6) I1 0.0638(6) 0.0543(5) 0.0439(5) 0.0084(3) -0.0129(4) -0.0241(4) I2 0.0593(6) 0.0523(5) 0.0472(5) 0.0063(4) -0.0045(4) -0.0199(4) I3 0.0482(5) 0.0619(6) 0.0436(4) 0.0038(4) -0.0109(4) -0.0174(4) I4 0.1070(9) 0.0824(7) 0.0450(5) 0.0106(4) -0.0213(5) -0.0574(7) N1 0.034(5) 0.045(6) 0.040(5) 0.005(4) -0.010(4) -0.018(4) N2 0.033(5) 0.036(5) 0.034(5) 0.009(4) -0.006(4) -0.014(4) C1 0.040(7) 0.033(6) 0.050(7) 0.011(5) -0.010(5) -0.015(5) C2 0.063(9) 0.047(8) 0.055(8) -0.001(6) -0.018(7) -0.022(7) C3 0.080(11) 0.050(8) 0.072(10) 0.008(7) -0.022(8) -0.024(8) C4 0.061(10) 0.056(9) 0.098(12) 0.040(8) -0.044(9) -0.022(8) C5 0.059(9) 0.081(10) 0.052(8) 0.033(7) -0.027(7) -0.017(8) C6 0.059(9) 0.057(8) 0.037(6) -0.001(5) -0.002(6) -0.025(7) C7 0.037(7) 0.051(7) 0.057(7) 0.005(6) -0.010(6) -0.024(6) C8 0.055(8) 0.052(8) 0.044(7) 0.012(5) -0.022(6) -0.017(6) C9 0.100(13) 0.061(9) 0.066(9) 0.023(7) -0.022(9) -0.037(9) C10 0.039(7) 0.053(8) 0.052(7) 0.004(5) -0.011(6) -0.020(6) C11 0.065(10) 0.077(10) 0.047(8) -0.008(7) 0.001(7) -0.030(8) C12 0.055(8) 0.061(8) 0.025(5) -0.006(5) -0.002(5) -0.019(6) C13 0.081(11) 0.065(10) 0.048(8) -0.012(7) 0.004(7) -0.012(8) C14 0.042(7) 0.034(6) 0.042(6) 0.001(4) -0.020(5) -0.010(5) C15 0.063(9) 0.049(8) 0.041(7) 0.005(5) -0.018(6) -0.012(7) C16 0.067(10) 0.070(10) 0.057(9) -0.009(7) -0.020(8) -0.011(8) C17 0.051(9) 0.059(9) 0.084(11) -0.004(7) -0.032(8) -0.009(7) C18 0.055(9) 0.065(9) 0.043(7) -0.005(6) -0.004(6) -0.012(7) C19 0.053(8) 0.048(7) 0.038(6) -0.004(5) -0.003(6) -0.009(6) C20 0.056(8) 0.037(6) 0.039(6) 0.011(5) -0.017(5) -0.024(6) C21 0.055(8) 0.036(6) 0.053(7) 0.015(5) -0.009(6) -0.016(6) C22 0.097(12) 0.080(10) 0.028(6) 0.005(6) -0.023(7) -0.018(9) C23 0.050(8) 0.057(8) 0.046(7) -0.002(5) -0.015(6) -0.028(6) C24 0.067(10) 0.092(12) 0.045(8) 0.012(7) -0.022(7) -0.008(9) C25 0.031(6) 0.038(6) 0.043(6) 0.002(5) -0.002(5) -0.009(5) C26 0.035(7) 0.045(7) 0.071(8) 0.016(6) -0.012(6) -0.009(6) _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 Ag1 I3 2.8592(15) 2_766 ? Ag1 I3 2.8764(15) . ? Ag1 I2 2.9195(15) . ? Ag1 I1 2.9373(13) . ? Ag2 I4 2.6862(14) . ? Ag2 I2 2.7477(14) . ? Ag2 I1 2.8065(15) . ? I3 Ag1 2.8592(15) 2_766 ? N1 C8 1.491(14) . ? N1 C10 1.513(15) . ? N1 C7 1.524(14) . ? N1 C12 1.530(13) . ? N2 C25 1.492(14) . ? N2 C21 1.502(13) . ? N2 C23 1.519(14) . ? N2 C20 1.522(14) . ? C1 C2 1.394(17) . ? C1 C6 1.400(16) . ? C1 C7 1.485(16) . ? C2 C3 1.352(19) . ? C2 H2A 0.9300 . ? C3 C4 1.37(2) . ? C3 H3A 0.9300 . ? C4 C5 1.40(2) . ? C4 H4A 0.9300 . ? C5 C6 1.364(17) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.529(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.513(16) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.503(18) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C19 1.403(16) . ? C14 C15 1.411(16) . ? C14 C20 1.477(16) . ? C15 C16 1.389(19) . ? C15 H15A 0.9300 . ? C16 C17 1.36(2) . ? C16 H16A 0.9300 . ? C17 C18 1.394(19) . ? C17 H17A 0.9300 . ? C18 C19 1.398(18) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.530(17) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.509(17) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.524(15) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 Ag1 I3 98.86(4) 2_766 . ? I3 Ag1 I2 116.43(5) 2_766 . ? I3 Ag1 I2 113.93(5) . . ? I3 Ag1 I1 114.58(5) 2_766 . ? I3 Ag1 I1 114.94(5) . . ? I2 Ag1 I1 99.04(4) . . ? I4 Ag2 I2 130.47(5) . . ? I4 Ag2 I1 122.84(5) . . ? I2 Ag2 I1 106.66(4) . . ? Ag2 I1 Ag1 76.52(4) . . ? Ag2 I2 Ag1 77.73(4) . . ? Ag1 I3 Ag1 81.14(4) 2_766 . ? C8 N1 C10 112.3(9) . . ? C8 N1 C7 106.0(9) . . ? C10 N1 C7 111.2(9) . . ? C8 N1 C12 111.4(9) . . ? C10 N1 C12 105.3(9) . . ? C7 N1 C12 110.8(8) . . ? C25 N2 C21 110.7(9) . . ? C25 N2 C23 111.8(8) . . ? C21 N2 C23 106.1(9) . . ? C25 N2 C20 107.4(8) . . ? C21 N2 C20 112.0(8) . . ? C23 N2 C20 108.9(9) . . ? C2 C1 C6 116.9(11) . . ? C2 C1 C7 120.4(11) . . ? C6 C1 C7 122.6(11) . . ? C3 C2 C1 121.6(13) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C2 C3 C4 121.0(14) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C3 C4 C5 119.4(13) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 119.4(13) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C1 121.7(13) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? C1 C7 N1 116.8(10) . . ? C1 C7 H7A 108.1 . . ? N1 C7 H7A 108.1 . . ? C1 C7 H7B 108.1 . . ? N1 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C9 115.0(11) . . ? N1 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? N1 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 115.7(10) . . ? N1 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? N1 C10 H10B 108.3 . . ? C11 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N1 116.2(11) . . ? C13 C12 H12A 108.2 . . ? N1 C12 H12A 108.2 . . ? C13 C12 H12B 108.2 . . ? N1 C12 H12B 108.2 . . ? H12A C12 H12B 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 118.3(11) . . ? C19 C14 C20 121.4(10) . . ? C15 C14 C20 120.2(11) . . ? C16 C15 C14 121.1(12) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C17 C16 C15 119.8(14) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 120.9(14) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C17 C18 C19 120.1(13) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 119.7(12) . . ? C18 C19 H19A 120.1 . . ? C14 C19 H19A 120.1 . . ? C14 C20 N2 118.4(9) . . ? C14 C20 H20A 107.7 . . ? N2 C20 H20A 107.7 . . ? C14 C20 H20B 107.7 . . ? N2 C20 H20B 107.7 . . ? H20A C20 H20B 107.1 . . ? N2 C21 C22 115.6(10) . . ? N2 C21 H21A 108.4 . . ? C22 C21 H21A 108.4 . . ? N2 C21 H21B 108.4 . . ? C22 C21 H21B 108.4 . . ? H21A C21 H21B 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N2 116.2(10) . . ? C24 C23 H23A 108.2 . . ? N2 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? N2 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 C26 117.0(9) . . ? N2 C25 H25A 108.0 . . ? C26 C25 H25A 108.0 . . ? N2 C25 H25B 108.0 . . ? C26 C25 H25B 108.0 . . ? H25A C25 H25B 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.817 _refine_diff_density_min -2.471 _refine_diff_density_rms 0.299 # Attachment '- 3.cif' data_3a _database_code_depnum_ccdc_archive 'CCDC 863849' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H34 N, Ag2 I3' _chemical_formula_sum 'C15 H34 Ag2 I3 N' _chemical_formula_weight 824.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1475(6) _cell_length_b 9.7391(7) _cell_length_c 18.189(2) _cell_angle_alpha 102.28(2) _cell_angle_beta 98.07(3) _cell_angle_gamma 90.85(2) _cell_volume 1223.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6774 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 26.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 5.381 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.515 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.1X0.1 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10696 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4785 _reflns_number_gt 2680 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear, Rigaku' _computing_cell_refinement 'CrystalClear, Rigaku' _computing_data_reduction 'CrystalClear, Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _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^)+(0.0100P)^2^+4.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00211(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4785 _refine_ls_number_parameters 195 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.306 _refine_ls_restrained_S_all 1.307 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL XuB-3 in P-1 CELL 0.71073 7.1475 9.7391 18.1890 102.280 98.070 90.850 ZERR 2.00 0.0006 0.0007 0.0020 0.020 0.030 0.020 LATT 1 SFAC C H N Ag I UNIT 30 68 2 4 6 OMIT -4 52 L.S. 8 DAMP 500 ACTA BOND $H FMAP 2 PLAN 10 DFIX 1.54 0.01 C9 C10 C10 C11 C11 C12 WGHT 0.010000 4.000000 EXTI 0.002106 FVAR 0.15299 AG1 4 0.527295 0.967172 0.085003 11.00000 0.07582 0.09115 = 0.12427 0.03179 -0.00077 -0.00233 AG2 4 0.033210 0.966373 0.083103 11.00000 0.07991 0.09006 = 0.12152 0.03368 0.02209 0.01025 I1 5 0.269685 1.175511 0.044014 11.00000 0.05289 0.06582 = 0.08973 0.01820 0.00417 -0.00121 I2 5 0.281455 0.748655 0.101217 11.00000 0.05231 0.07982 = 0.13738 0.03697 0.01155 0.00466 I3 5 -0.173679 1.068105 0.200040 11.00000 0.06854 0.06449 = 0.09633 0.01501 0.00800 -0.00041 N1 3 0.806740 0.531054 0.168975 11.00000 0.04119 0.06034 = 0.11650 0.03235 0.00888 0.00112 C1 1 0.636734 0.465779 0.189690 11.00000 0.05171 0.08845 = 0.10975 0.02180 0.00177 -0.00519 AFIX 23 H1A 2 0.616308 0.370826 0.159058 11.00000 -1.20000 H1B 2 0.527898 0.517981 0.175553 11.00000 -1.20000 AFIX 0 C2 1 0.642122 0.458463 0.271596 11.00000 0.05836 0.07906 = 0.11929 0.02562 0.00042 -0.00045 AFIX 23 H2A 2 0.671137 0.551527 0.303709 11.00000 -1.20000 H2B 2 0.740901 0.397458 0.285426 11.00000 -1.20000 AFIX 0 C3 1 0.454043 0.402570 0.284318 11.00000 0.06241 0.12273 = 0.08009 0.02025 0.01064 -0.01179 AFIX 23 H3A 2 0.357376 0.464442 0.269626 11.00000 -1.20000 H3B 2 0.425930 0.310999 0.250488 11.00000 -1.20000 AFIX 0 C4 1 0.438776 0.387945 0.363212 11.00000 0.08573 0.11516 = 0.08699 0.01486 0.00290 -0.01009 AFIX 23 H4A 2 0.475139 0.477674 0.397827 11.00000 -1.20000 H4B 2 0.528044 0.320177 0.376754 11.00000 -1.20000 AFIX 0 C5 1 0.243552 0.341674 0.374464 11.00000 0.07858 0.15868 = 0.12379 0.07020 0.00670 -0.00675 AFIX 23 H5A 2 0.156488 0.411788 0.362280 11.00000 -1.20000 H5B 2 0.205978 0.254685 0.337576 11.00000 -1.20000 AFIX 0 C6 1 0.217583 0.318855 0.449974 11.00000 0.10081 0.13434 = 0.10488 0.02881 0.01420 -0.02049 AFIX 23 H6A 2 0.254168 0.405373 0.487379 11.00000 -1.20000 H6B 2 0.302348 0.247579 0.462411 11.00000 -1.20000 AFIX 0 C7 1 0.022733 0.274744 0.456472 11.00000 0.08871 0.15849 = 0.10121 0.02328 0.01796 -0.02985 AFIX 23 H7A 2 -0.015523 0.189910 0.417988 11.00000 -1.20000 H7B 2 -0.061538 0.347485 0.445777 11.00000 -1.20000 AFIX 0 C8 1 -0.001633 0.246713 0.533937 11.00000 0.10064 0.15919 = 0.12950 0.02973 0.02313 -0.02729 AFIX 23 H8A 2 0.085065 0.175897 0.545419 11.00000 -1.20000 H8B 2 0.032468 0.332328 0.572336 11.00000 -1.20000 AFIX 0 C9 1 -0.193446 0.199217 0.538601 11.00000 0.10302 0.19398 = 0.15474 0.03254 0.04872 -0.03481 AFIX 23 H9A 2 -0.227997 0.115690 0.498760 11.00000 -1.20000 H9B 2 -0.278684 0.271462 0.527994 11.00000 -1.20000 AFIX 0 C10 1 -0.226222 0.165480 0.613780 11.00000 0.14837 0.18173 = 0.17814 0.01463 0.04419 -0.05321 AFIX 23 H10A 2 -0.189503 0.246908 0.654764 11.00000 -1.20000 H10B 2 -0.149064 0.088542 0.623794 11.00000 -1.20000 AFIX 0 C11 1 -0.436363 0.124360 0.610615 11.00000 0.21856 0.27149 = 0.21748 0.02540 0.03214 -0.09252 AFIX 23 H11A 2 -0.511854 0.206762 0.613440 11.00000 -1.20000 H11B 2 -0.482152 0.057473 0.563600 11.00000 -1.20000 AFIX 0 C12 1 -0.448719 0.059023 0.678349 11.00000 0.33574 0.26620 = 0.24044 0.04175 0.08476 -0.08580 AFIX 137 H12A 2 -0.577385 0.028714 0.677877 11.00000 -1.50000 H12B 2 -0.406642 0.127296 0.724442 11.00000 -1.50000 H12C 2 -0.369964 -0.020365 0.675669 11.00000 -1.50000 AFIX 0 C13 1 0.771681 0.527331 0.086683 11.00000 0.10124 0.27494 = 0.10062 0.07696 0.00472 -0.00896 AFIX 137 H13A 2 0.787173 0.433777 0.058820 11.00000 -1.50000 H13B 2 0.859985 0.591436 0.074629 11.00000 -1.50000 H13C 2 0.645067 0.554357 0.073045 11.00000 -1.50000 AFIX 0 C14 1 0.981469 0.457816 0.187784 11.00000 0.07223 0.11652 = 0.28282 0.12714 0.05795 0.04477 AFIX 137 H14A 2 0.965537 0.360637 0.162006 11.00000 -1.50000 H14B 2 1.006138 0.464431 0.241711 11.00000 -1.50000 H14C 2 1.085933 0.500934 0.171819 11.00000 -1.50000 AFIX 0 C15 1 0.830354 0.682484 0.208322 11.00000 0.16282 0.05646 = 0.17825 -0.00941 0.06668 -0.02967 AFIX 137 H15A 2 0.891626 0.690576 0.259621 11.00000 -1.50000 H15B 2 0.708466 0.722475 0.208857 11.00000 -1.50000 H15C 2 0.906166 0.731849 0.181808 11.00000 -1.50000 HKLF 4 REM XuB-3 in P-1 REM R1 = 0.0450 for 2680 Fo > 4sig(Fo) and 0.0940 for all 4785 data REM 195 parameters refined using 3 restraints END ; 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 Ag1 Ag 0.52729(11) 0.96717(8) 0.08500(6) 0.0974(3) Uani 1 1 d . . . Ag2 Ag 0.03321(11) 0.96637(8) 0.08310(5) 0.0948(3) Uani 1 1 d . . . I1 I 0.26968(8) 1.17551(6) 0.04401(4) 0.06994(18) Uani 1 1 d . . . I2 I 0.28146(8) 0.74866(6) 0.10122(5) 0.0880(2) Uani 1 1 d . . . I3 I -0.17368(9) 1.06810(6) 0.20004(4) 0.0773(2) Uani 1 1 d . . . N1 N 0.8067(9) 0.5311(6) 0.1690(5) 0.071(2) Uani 1 1 d . . . C1 C 0.6367(12) 0.4658(10) 0.1897(6) 0.084(3) Uani 1 1 d . . . H1A H 0.6163 0.3708 0.1591 0.101 Uiso 1 1 calc R . . H1B H 0.5279 0.5180 0.1756 0.101 Uiso 1 1 calc R . . C2 C 0.6421(12) 0.4585(10) 0.2716(6) 0.086(3) Uani 1 1 d . . . H2A H 0.6711 0.5515 0.3037 0.103 Uiso 1 1 calc R . . H2B H 0.7409 0.3975 0.2854 0.103 Uiso 1 1 calc R . . C3 C 0.4540(13) 0.4026(11) 0.2843(6) 0.089(3) Uani 1 1 d . . . H3A H 0.3574 0.4644 0.2696 0.107 Uiso 1 1 calc R . . H3B H 0.4259 0.3110 0.2505 0.107 Uiso 1 1 calc R . . C4 C 0.4388(14) 0.3879(12) 0.3632(6) 0.098(4) Uani 1 1 d . . . H4A H 0.4751 0.4777 0.3978 0.118 Uiso 1 1 calc R . . H4B H 0.5280 0.3202 0.3768 0.118 Uiso 1 1 calc R . . C5 C 0.2436(15) 0.3417(13) 0.3745(7) 0.115(4) Uani 1 1 d . . . H5A H 0.1565 0.4118 0.3623 0.138 Uiso 1 1 calc R . . H5B H 0.2060 0.2547 0.3376 0.138 Uiso 1 1 calc R . . C6 C 0.2176(16) 0.3189(13) 0.4500(7) 0.113(4) Uani 1 1 d . . . H6A H 0.2542 0.4054 0.4874 0.136 Uiso 1 1 calc R . . H6B H 0.3023 0.2476 0.4624 0.136 Uiso 1 1 calc R . . C7 C 0.0227(15) 0.2747(14) 0.4565(7) 0.117(4) Uani 1 1 d . . . H7A H -0.0155 0.1899 0.4180 0.140 Uiso 1 1 calc R . . H7B H -0.0615 0.3475 0.4458 0.140 Uiso 1 1 calc R . . C8 C -0.0016(17) 0.2467(14) 0.5339(8) 0.130(5) Uani 1 1 d . . . H8A H 0.0851 0.1759 0.5454 0.156 Uiso 1 1 calc R . . H8B H 0.0325 0.3323 0.5723 0.156 Uiso 1 1 calc R . . C9 C -0.1934(17) 0.1992(15) 0.5386(6) 0.149(6) Uani 1 1 d D . . H9A H -0.2280 0.1157 0.4988 0.179 Uiso 1 1 calc R . . H9B H -0.2787 0.2715 0.5280 0.179 Uiso 1 1 calc R . . C10 C -0.2262(13) 0.1655(16) 0.6138(7) 0.172(7) Uani 1 1 d D . . H10A H -0.1895 0.2469 0.6548 0.206 Uiso 1 1 calc R . . H10B H -0.1491 0.0885 0.6238 0.206 Uiso 1 1 calc R . . C11 C -0.4364(16) 0.1244(16) 0.6106(8) 0.241(11) Uani 1 1 d D . . H11A H -0.5119 0.2068 0.6134 0.289 Uiso 1 1 calc R . . H11B H -0.4822 0.0575 0.5636 0.289 Uiso 1 1 calc R . . C12 C -0.449(3) 0.059(2) 0.6783(10) 0.280(13) Uani 1 1 d D . . H12A H -0.5774 0.0287 0.6779 0.419 Uiso 1 1 calc R . . H12B H -0.4066 0.1273 0.7244 0.419 Uiso 1 1 calc R . . H12C H -0.3700 -0.0204 0.6757 0.419 Uiso 1 1 calc R . . C13 C 0.7717(18) 0.5273(18) 0.0867(7) 0.155(6) Uani 1 1 d . . . H13A H 0.7872 0.4338 0.0588 0.232 Uiso 1 1 calc R . . H13B H 0.8600 0.5914 0.0746 0.232 Uiso 1 1 calc R . . H13C H 0.6451 0.5544 0.0730 0.232 Uiso 1 1 calc R . . C14 C 0.9815(14) 0.4578(11) 0.1878(9) 0.141(5) Uani 1 1 d . . . H14A H 0.9655 0.3606 0.1620 0.212 Uiso 1 1 calc R . . H14B H 1.0061 0.4644 0.2417 0.212 Uiso 1 1 calc R . . H14C H 1.0859 0.5009 0.1718 0.212 Uiso 1 1 calc R . . C15 C 0.8304(18) 0.6825(9) 0.2083(8) 0.134(5) Uani 1 1 d . . . H15A H 0.8916 0.6906 0.2596 0.201 Uiso 1 1 calc R . . H15B H 0.7085 0.7225 0.2089 0.201 Uiso 1 1 calc R . . H15C H 0.9062 0.7318 0.1818 0.201 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 Ag1 0.0758(5) 0.0911(5) 0.1243(7) 0.0318(5) -0.0008(5) -0.0023(4) Ag2 0.0799(5) 0.0901(5) 0.1215(7) 0.0337(5) 0.0221(5) 0.0103(4) I1 0.0529(3) 0.0658(3) 0.0897(4) 0.0182(3) 0.0042(3) -0.0012(2) I2 0.0523(3) 0.0798(4) 0.1374(6) 0.0370(4) 0.0116(4) 0.0047(3) I3 0.0685(4) 0.0645(3) 0.0963(5) 0.0150(3) 0.0080(3) -0.0004(3) N1 0.041(4) 0.060(4) 0.116(6) 0.032(4) 0.009(4) 0.001(3) C1 0.052(5) 0.088(6) 0.110(8) 0.022(6) 0.002(5) -0.005(5) C2 0.058(6) 0.079(6) 0.119(9) 0.026(6) 0.000(6) 0.000(4) C3 0.062(6) 0.123(8) 0.080(7) 0.020(6) 0.011(5) -0.012(5) C4 0.086(7) 0.115(8) 0.087(8) 0.015(7) 0.003(6) -0.010(6) C5 0.079(7) 0.159(10) 0.124(10) 0.070(8) 0.007(7) -0.007(7) C6 0.101(9) 0.134(9) 0.105(9) 0.029(8) 0.014(7) -0.020(7) C7 0.089(8) 0.158(10) 0.101(9) 0.023(8) 0.018(7) -0.030(8) C8 0.101(9) 0.159(11) 0.129(11) 0.030(9) 0.023(8) -0.027(8) C9 0.103(9) 0.194(13) 0.155(13) 0.033(11) 0.049(9) -0.035(9) C10 0.148(13) 0.182(14) 0.178(16) 0.015(12) 0.044(12) -0.053(11) C11 0.22(2) 0.27(2) 0.22(2) 0.025(19) 0.032(18) -0.093(18) C12 0.34(3) 0.27(2) 0.24(3) 0.04(2) 0.08(2) -0.09(2) C13 0.101(10) 0.275(17) 0.101(10) 0.077(11) 0.005(8) -0.009(10) C14 0.072(6) 0.117(7) 0.283(15) 0.127(8) 0.058(8) 0.045(5) C15 0.163(11) 0.056(6) 0.178(13) -0.009(7) 0.067(10) -0.030(6) _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 Ag1 I3 2.7784(14) 1_655 ? Ag1 I2 2.8293(12) . ? Ag1 I1 2.9038(12) . ? Ag1 I1 3.0286(14) 2_675 ? Ag2 I3 2.7789(13) . ? Ag2 I2 2.8280(11) . ? Ag2 I1 2.8917(12) . ? Ag2 I1 3.0148(14) 2_575 ? I3 Ag1 2.7785(14) 1_455 ? N1 C13 1.475(14) . ? N1 C14 1.482(11) . ? N1 C15 1.492(10) . ? N1 C1 1.493(11) . ? C1 C2 1.502(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.509(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.491(14) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.514(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.473(16) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.479(14) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.524(17) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.460(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.520(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.539(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.514(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 Ag1 I2 119.11(4) 1_655 . ? I3 Ag1 I1 115.87(4) 1_655 . ? I2 Ag1 I1 103.23(3) . . ? I3 Ag1 I1 102.11(3) 1_655 2_675 ? I2 Ag1 I1 102.73(4) . 2_675 ? I1 Ag1 I1 113.35(4) . 2_675 ? I3 Ag2 I2 117.82(4) . . ? I3 Ag2 I1 115.01(4) . . ? I2 Ag2 I1 103.57(3) . . ? I3 Ag2 I1 102.44(3) . 2_575 ? I2 Ag2 I1 103.39(4) . 2_575 ? I1 Ag2 I1 114.42(4) . 2_575 ? Ag2 I1 Ag1 74.96(3) . . ? Ag2 I1 Ag2 65.58(4) . 2_575 ? Ag1 I1 Ag2 109.26(3) . 2_575 ? Ag2 I1 Ag1 108.57(3) . 2_675 ? Ag1 I1 Ag1 66.65(4) . 2_675 ? Ag2 I1 Ag1 73.62(3) 2_575 2_675 ? Ag2 I2 Ag1 77.13(3) . . ? Ag1 I3 Ag2 81.32(3) 1_455 . ? C13 N1 C14 110.1(9) . . ? C13 N1 C15 106.5(10) . . ? C14 N1 C15 109.9(8) . . ? C13 N1 C1 108.0(8) . . ? C14 N1 C1 112.3(8) . . ? C15 N1 C1 109.8(8) . . ? N1 C1 C2 117.0(7) . . ? N1 C1 H1A 108.0 . . ? C2 C1 H1A 108.0 . . ? N1 C1 H1B 108.0 . . ? C2 C1 H1B 108.0 . . ? H1A C1 H1B 107.3 . . ? C1 C2 C3 110.3(8) . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 116.4(8) . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? C2 C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? C3 C4 C5 114.5(9) . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C4 118.1(10) . . ? C6 C5 H5A 107.8 . . ? C4 C5 H5A 107.8 . . ? C6 C5 H5B 107.8 . . ? C4 C5 H5B 107.8 . . ? H5A C5 H5B 107.1 . . ? C5 C6 C7 114.8(10) . . ? C5 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? C7 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 114.5(10) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 113.7(10) . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 116.4(10) . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9B 108.2 . . ? C10 C9 H9B 108.2 . . ? H9A C9 H9B 107.3 . . ? C9 C10 C11 109.9(10) . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C12 C11 C10 106.4(13) . . ? C12 C11 H11A 110.4 . . ? C10 C11 H11A 110.4 . . ? C12 C11 H11B 110.4 . . ? C10 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.101 _refine_diff_density_min -1.422 _refine_diff_density_rms 0.187 # start Validation Reply Form _vrf_PLAT242_ALERT_2_B ; PROBLEM: Check Low Ueq as Compared to Neighbors for N1 RESPONSE: The terminal group of -N(CH3)3 rotates around the single bond, N1-C1, which gives big U(eq.) to C13, C14 and C15. ; # end Validation Reply Form # Attachment '- 4.cif' data_4a _database_code_depnum_ccdc_archive 'CCDC 863850' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H56 N, Ag4 I5' _chemical_formula_sum 'C26 H56 Ag4 I5 N' _chemical_formula_weight 1448.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.189(3) _cell_length_b 10.093(3) _cell_length_c 23.519(9) _cell_angle_alpha 83.515(13) _cell_angle_beta 88.522(13) _cell_angle_gamma 68.316(12) _cell_volume 2013.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5476 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 5.765 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.304 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17431 _diffrn_reflns_av_R_equivalents 0.1185 _diffrn_reflns_av_sigmaI/netI 0.1479 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6953 _reflns_number_gt 3391 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _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^)+(0.0010P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.01105(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6953 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1608 _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_restrained_S_all 1.277 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL XuB-2 in P-1 CELL 0.71073 9.1890 10.0930 23.5191 83.515 88.522 68.316 ZERR 2.00 0.0028 0.0028 0.0086 0.013 0.013 0.012 LATT 1 SFAC C H N AG I UNIT 52 112 2 8 10 OMIT -4 50.1 L.S. 8 DAMP 500 ACTA BOND $H FMAP 2 PLAN 10 WGHT 0.001000 2.500000 EXTI 0.011053 FVAR 0.07084 I1 5 1.250356 -0.021208 1.142801 11.00000 0.05154 0.05295 = 0.05703 -0.00163 -0.00072 -0.01479 I2 5 1.012846 0.457897 1.141824 11.00000 0.04168 0.05110 = 0.05841 -0.00802 0.00356 -0.01848 I3 5 1.390878 0.261377 0.999141 11.00000 0.04590 0.05095 = 0.05147 -0.00598 0.00253 -0.01916 I4 5 0.873720 0.245537 0.999573 11.00000 0.04135 0.05763 = 0.04312 -0.00601 0.00255 -0.01188 I5 5 0.752561 0.944114 1.139327 11.00000 0.05364 0.05474 = 0.05604 -0.01072 0.00661 -0.01962 AG1 4 1.127417 0.247787 1.069152 11.00000 0.07101 0.06946 = 0.07333 -0.01500 0.00089 -0.02098 AG2 4 0.881655 0.708528 1.070488 11.00000 0.07142 0.06695 = 0.07409 -0.00198 0.00467 -0.02114 AG3 4 1.506513 0.016469 0.932425 11.00000 0.07796 0.08068 = 0.07270 -0.00647 0.00358 -0.02413 AG4 4 0.998518 0.020043 0.925309 11.00000 0.06886 0.07519 = 0.07962 -0.00847 0.00437 -0.02532 N1 3 0.490366 0.538259 0.836819 11.00000 0.04059 0.04541 = 0.03293 -0.00356 -0.00499 -0.01832 C1 1 0.418958 0.454726 0.804578 11.00000 0.04250 0.05190 = 0.04669 -0.00426 0.00361 -0.03473 AFIX 23 H1A 2 0.399028 0.383491 0.831541 11.00000 -1.20000 H1B 2 0.318911 0.520019 0.788210 11.00000 -1.20000 AFIX 0 C2 1 0.518608 0.380554 0.757661 11.00000 0.04055 0.04886 = 0.02282 -0.00865 0.00821 -0.02417 AFIX 23 H2A 2 0.620768 0.318215 0.773262 11.00000 -1.20000 H2B 2 0.533318 0.451478 0.729072 11.00000 -1.20000 AFIX 0 C3 1 0.444522 0.293389 0.729952 11.00000 0.06871 0.05006 = 0.06776 -0.01954 0.01022 -0.03502 AFIX 23 H3A 2 0.344252 0.357582 0.713384 11.00000 -1.20000 H3B 2 0.424242 0.227319 0.759433 11.00000 -1.20000 AFIX 0 C4 1 0.540890 0.207450 0.683391 11.00000 0.08030 0.04036 = 0.06582 -0.01838 0.01863 -0.02266 AFIX 23 H4A 2 0.642002 0.144227 0.699595 11.00000 -1.20000 H4B 2 0.488165 0.147883 0.671133 11.00000 -1.20000 AFIX 0 C5 1 0.566760 0.299360 0.631441 11.00000 0.06786 0.03853 = 0.06889 -0.01535 0.00509 -0.01053 AFIX 23 H5A 2 0.621015 0.357840 0.643557 11.00000 -1.20000 H5B 2 0.465712 0.363575 0.615517 11.00000 -1.20000 AFIX 0 C6 1 0.661538 0.212338 0.584509 11.00000 0.06839 0.05271 = 0.05572 -0.00847 0.00440 -0.01603 AFIX 23 H6A 2 0.762052 0.148619 0.601039 11.00000 -1.20000 H6B 2 0.607413 0.152584 0.573550 11.00000 -1.20000 AFIX 0 C7 1 0.691354 0.293336 0.531503 11.00000 0.08218 0.05307 = 0.04581 -0.00110 -0.01335 -0.01132 AFIX 23 H7A 2 0.750980 0.348807 0.542093 11.00000 -1.20000 H7B 2 0.591280 0.360921 0.516038 11.00000 -1.20000 AFIX 0 C8 1 0.776469 0.207165 0.484810 11.00000 0.08884 0.06084 = 0.05202 -0.00774 -0.02389 -0.00951 AFIX 23 H8A 2 0.715383 0.153860 0.473351 11.00000 -1.20000 H8B 2 0.875365 0.137748 0.500474 11.00000 -1.20000 AFIX 0 C9 1 0.809710 0.289630 0.432269 11.00000 0.08665 0.06741 = 0.06411 -0.00143 0.00421 -0.02895 AFIX 23 H9A 2 0.711258 0.359261 0.416338 11.00000 -1.20000 H9B 2 0.871996 0.342247 0.443337 11.00000 -1.20000 AFIX 0 C10 1 0.893570 0.199503 0.386971 11.00000 0.05415 0.08008 = 0.06261 -0.00026 0.00478 -0.02595 AFIX 23 H10A 2 0.988654 0.126609 0.403958 11.00000 -1.20000 H10B 2 0.828398 0.150389 0.375141 11.00000 -1.20000 AFIX 0 C11 1 0.936984 0.273001 0.335018 11.00000 0.08370 0.09409 = 0.08235 0.00667 0.02973 -0.03345 AFIX 23 H11A 2 1.001504 0.322737 0.346848 11.00000 -1.20000 H11B 2 0.841833 0.345352 0.317828 11.00000 -1.20000 AFIX 0 C12 1 1.026299 0.177690 0.287680 11.00000 0.11491 0.12317 = 0.07778 -0.00348 0.03994 -0.03606 AFIX 33 H12A 2 1.047215 0.237164 0.256243 11.00000 -1.50000 H12B 2 0.963086 0.129603 0.274447 11.00000 -1.50000 H12C 2 1.123378 0.107846 0.303315 11.00000 -1.50000 AFIX 0 C13 1 0.540541 0.642963 0.798557 11.00000 0.03255 0.03917 = 0.05688 -0.00757 -0.00004 -0.01117 AFIX 23 H13A 2 0.577087 0.697126 0.822407 11.00000 -1.20000 H13B 2 0.628498 0.589235 0.776256 11.00000 -1.20000 AFIX 0 C14 1 0.416064 0.746824 0.758209 11.00000 0.05747 0.05522 = 0.03882 0.00374 -0.00617 -0.01415 AFIX 23 H14A 2 0.337618 0.814234 0.779942 11.00000 -1.20000 H14B 2 0.365078 0.694674 0.739270 11.00000 -1.20000 AFIX 0 C15 1 0.481281 0.829551 0.713172 11.00000 0.10745 0.05432 = 0.06011 -0.00974 0.01372 -0.02056 AFIX 23 H15A 2 0.552362 0.863319 0.731504 11.00000 -1.20000 H15B 2 0.395898 0.912807 0.695768 11.00000 -1.20000 AFIX 0 C16 1 0.570292 0.735500 0.665405 11.00000 0.10258 0.05449 = 0.06226 0.00931 0.04379 -0.02073 AFIX 23 H16A 2 0.666903 0.664082 0.681963 11.00000 -1.20000 H16B 2 0.506817 0.684709 0.653639 11.00000 -1.20000 AFIX 0 C17 1 0.608908 0.812530 0.614176 11.00000 0.06370 0.06043 = 0.05075 0.00771 0.00922 -0.02068 AFIX 23 H17A 2 0.673321 0.862590 0.625800 11.00000 -1.20000 H17B 2 0.512507 0.884434 0.597684 11.00000 -1.20000 AFIX 0 C18 1 0.693406 0.720797 0.568357 11.00000 0.08636 0.06551 = 0.04680 -0.00618 0.00543 -0.02961 AFIX 23 H18A 2 0.793211 0.653343 0.584103 11.00000 -1.20000 H18B 2 0.632557 0.665514 0.558726 11.00000 -1.20000 AFIX 0 C19 1 0.722982 0.799194 0.514903 11.00000 0.09724 0.06595 = 0.05761 0.00780 -0.03586 -0.01640 AFIX 23 H19A 2 0.783338 0.854674 0.524798 11.00000 -1.20000 H19B 2 0.622902 0.866773 0.499440 11.00000 -1.20000 AFIX 0 C20 1 0.806380 0.711807 0.468669 11.00000 0.06831 0.05283 = 0.05721 -0.01118 0.00008 -0.00401 AFIX 23 H20A 2 0.745782 0.656393 0.458936 11.00000 -1.20000 H20B 2 0.906107 0.644032 0.484348 11.00000 -1.20000 AFIX 0 C21 1 0.838088 0.788916 0.413987 11.00000 0.08133 0.06938 = 0.05237 0.00516 -0.00775 -0.01797 AFIX 23 H21A 2 0.738256 0.853187 0.397102 11.00000 -1.20000 H21B 2 0.894669 0.847820 0.423680 11.00000 -1.20000 AFIX 0 C22 1 0.928082 0.698364 0.369594 11.00000 0.06694 0.07487 = 0.06248 -0.01601 0.00262 -0.00994 AFIX 23 H22A 2 0.873120 0.637329 0.360838 11.00000 -1.20000 H22B 2 1.029079 0.636111 0.386195 11.00000 -1.20000 AFIX 0 C23 1 0.956587 0.775098 0.313685 11.00000 0.08769 0.13158 = 0.06736 -0.00476 -0.00436 -0.04075 AFIX 23 H23A 2 0.856029 0.839025 0.297260 11.00000 -1.20000 H23B 2 1.014473 0.834011 0.322062 11.00000 -1.20000 AFIX 0 C24 1 1.043071 0.681448 0.270056 11.00000 0.05919 0.17233 = 0.11139 -0.03375 0.02949 0.00059 AFIX 33 H24A 2 1.053123 0.739746 0.236133 11.00000 -1.50000 H24B 2 0.986757 0.623010 0.260929 11.00000 -1.50000 H24C 2 1.145310 0.620973 0.284866 11.00000 -1.50000 AFIX 0 C25 1 0.626750 0.439970 0.874060 11.00000 0.03922 0.05882 = 0.06800 0.01955 -0.01759 -0.00566 AFIX 33 H25A 2 0.668779 0.496090 0.894026 11.00000 -1.50000 H25B 2 0.706285 0.381198 0.850657 11.00000 -1.50000 H25C 2 0.592211 0.379904 0.901259 11.00000 -1.50000 AFIX 0 C26 1 0.363998 0.622712 0.877262 11.00000 0.05930 0.06585 = 0.05082 -0.04620 0.02674 -0.02498 AFIX 33 H26A 2 0.404830 0.677557 0.898473 11.00000 -1.50000 H26B 2 0.334596 0.556919 0.903318 11.00000 -1.50000 H26C 2 0.273838 0.686274 0.855191 11.00000 -1.50000 HKLF 4 REM XuB-2 in P-1 REM R1 = 0.0766 for 3391 Fo > 4sig(Fo) and 0.1034 for all 6953 data REM 326 parameters refined using 0 restraints END ; 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 I1 I 1.25036(9) -0.02121(8) 1.14280(4) 0.0555(3) Uani 1 1 d . . . I2 I 1.01285(9) 0.45790(7) 1.14182(4) 0.0499(2) Uani 1 1 d . . . I3 I 1.39088(9) 0.26138(7) 0.99914(4) 0.0491(2) Uani 1 1 d . . . I4 I 0.87372(8) 0.24554(7) 0.99957(3) 0.0492(2) Uani 1 1 d . . . I5 I 0.75256(9) 0.94411(8) 1.13933(4) 0.0546(2) Uani 1 1 d . . . Ag1 Ag 1.12742(13) 0.24779(10) 1.06915(5) 0.0721(4) Uani 1 1 d . . . Ag2 Ag 0.88165(13) 0.70853(10) 1.07049(5) 0.0726(4) Uani 1 1 d . . . Ag3 Ag 1.50651(13) 0.01647(11) 0.93243(5) 0.0788(4) Uani 1 1 d . . . Ag4 Ag 0.99852(13) 0.02004(11) 0.92531(5) 0.0750(4) Uani 1 1 d . . . N1 N 0.4904(9) 0.5383(8) 0.8368(4) 0.039(2) Uani 1 1 d . . . C1 C 0.4190(11) 0.4547(10) 0.8046(5) 0.042(3) Uani 1 1 d . . . H1A H 0.3990 0.3835 0.8315 0.051 Uiso 1 1 calc R . . H1B H 0.3189 0.5200 0.7882 0.051 Uiso 1 1 calc R . . C2 C 0.5186(11) 0.3806(9) 0.7577(4) 0.035(3) Uani 1 1 d . . . H2A H 0.6208 0.3182 0.7733 0.042 Uiso 1 1 calc R . . H2B H 0.5333 0.4515 0.7291 0.042 Uiso 1 1 calc R . . C3 C 0.4445(13) 0.2934(10) 0.7300(5) 0.058(4) Uani 1 1 d . . . H3A H 0.3443 0.3576 0.7134 0.069 Uiso 1 1 calc R . . H3B H 0.4242 0.2273 0.7594 0.069 Uiso 1 1 calc R . . C4 C 0.5409(14) 0.2075(10) 0.6834(5) 0.061(4) Uani 1 1 d . . . H4A H 0.6420 0.1442 0.6996 0.074 Uiso 1 1 calc R . . H4B H 0.4882 0.1479 0.6711 0.074 Uiso 1 1 calc R . . C5 C 0.5668(14) 0.2994(10) 0.6314(5) 0.060(4) Uani 1 1 d . . . H5A H 0.6210 0.3578 0.6436 0.072 Uiso 1 1 calc R . . H5B H 0.4657 0.3636 0.6155 0.072 Uiso 1 1 calc R . . C6 C 0.6615(14) 0.2123(11) 0.5845(5) 0.061(4) Uani 1 1 d . . . H6A H 0.7621 0.1486 0.6010 0.073 Uiso 1 1 calc R . . H6B H 0.6074 0.1526 0.5736 0.073 Uiso 1 1 calc R . . C7 C 0.6914(15) 0.2933(11) 0.5315(5) 0.064(4) Uani 1 1 d . . . H7A H 0.7510 0.3488 0.5421 0.077 Uiso 1 1 calc R . . H7B H 0.5913 0.3609 0.5160 0.077 Uiso 1 1 calc R . . C8 C 0.7765(15) 0.2072(12) 0.4848(5) 0.072(5) Uani 1 1 d . . . H8A H 0.7154 0.1539 0.4734 0.086 Uiso 1 1 calc R . . H8B H 0.8754 0.1377 0.5005 0.086 Uiso 1 1 calc R . . C9 C 0.8097(15) 0.2896(12) 0.4323(6) 0.073(5) Uani 1 1 d . . . H9A H 0.7113 0.3593 0.4163 0.088 Uiso 1 1 calc R . . H9B H 0.8720 0.3422 0.4433 0.088 Uiso 1 1 calc R . . C10 C 0.8936(14) 0.1995(12) 0.3870(6) 0.066(4) Uani 1 1 d . . . H10A H 0.9887 0.1266 0.4040 0.079 Uiso 1 1 calc R . . H10B H 0.8284 0.1504 0.3751 0.079 Uiso 1 1 calc R . . C11 C 0.9370(16) 0.2730(13) 0.3350(6) 0.088(5) Uani 1 1 d . . . H11A H 1.0015 0.3227 0.3468 0.106 Uiso 1 1 calc R . . H11B H 0.8418 0.3454 0.3178 0.106 Uiso 1 1 calc R . . C12 C 1.0263(17) 0.1777(14) 0.2877(7) 0.109(6) Uani 1 1 d . . . H12A H 1.0472 0.2372 0.2562 0.163 Uiso 1 1 calc R . . H12B H 0.9631 0.1296 0.2744 0.163 Uiso 1 1 calc R . . H12C H 1.1234 0.1078 0.3033 0.163 Uiso 1 1 calc R . . C13 C 0.5405(11) 0.6430(10) 0.7986(5) 0.043(3) Uani 1 1 d . . . H13A H 0.5771 0.6971 0.8224 0.052 Uiso 1 1 calc R . . H13B H 0.6285 0.5892 0.7763 0.052 Uiso 1 1 calc R . . C14 C 0.4161(13) 0.7468(11) 0.7582(5) 0.053(4) Uani 1 1 d . . . H14A H 0.3376 0.8142 0.7799 0.064 Uiso 1 1 calc R . . H14B H 0.3651 0.6947 0.7393 0.064 Uiso 1 1 calc R . . C15 C 0.4813(16) 0.8296(12) 0.7132(6) 0.077(5) Uani 1 1 d . . . H15A H 0.5524 0.8633 0.7315 0.092 Uiso 1 1 calc R . . H15B H 0.3959 0.9128 0.6958 0.092 Uiso 1 1 calc R . . C16 C 0.5703(15) 0.7355(12) 0.6654(6) 0.078(5) Uani 1 1 d . . . H16A H 0.6669 0.6641 0.6820 0.093 Uiso 1 1 calc R . . H16B H 0.5068 0.6847 0.6536 0.093 Uiso 1 1 calc R . . C17 C 0.6089(14) 0.8125(11) 0.6142(5) 0.060(4) Uani 1 1 d . . . H17A H 0.6733 0.8626 0.6258 0.072 Uiso 1 1 calc R . . H17B H 0.5125 0.8844 0.5977 0.072 Uiso 1 1 calc R . . C18 C 0.6934(15) 0.7208(12) 0.5684(5) 0.066(4) Uani 1 1 d . . . H18A H 0.7932 0.6533 0.5841 0.079 Uiso 1 1 calc R . . H18B H 0.6326 0.6655 0.5587 0.079 Uiso 1 1 calc R . . C19 C 0.7230(16) 0.7992(12) 0.5149(6) 0.078(5) Uani 1 1 d . . . H19A H 0.7833 0.8547 0.5248 0.094 Uiso 1 1 calc R . . H19B H 0.6229 0.8668 0.4994 0.094 Uiso 1 1 calc R . . C20 C 0.8064(14) 0.7118(11) 0.4687(6) 0.064(4) Uani 1 1 d . . . H20A H 0.7458 0.6564 0.4589 0.077 Uiso 1 1 calc R . . H20B H 0.9061 0.6440 0.4843 0.077 Uiso 1 1 calc R . . C21 C 0.8381(15) 0.7889(12) 0.4140(6) 0.071(4) Uani 1 1 d . . . H21A H 0.7383 0.8532 0.3971 0.086 Uiso 1 1 calc R . . H21B H 0.8947 0.8478 0.4237 0.086 Uiso 1 1 calc R . . C22 C 0.9281(15) 0.6984(12) 0.3696(6) 0.072(5) Uani 1 1 d . . . H22A H 0.8731 0.6373 0.3608 0.087 Uiso 1 1 calc R . . H22B H 1.0291 0.6361 0.3862 0.087 Uiso 1 1 calc R . . C23 C 0.9566(17) 0.7751(15) 0.3137(7) 0.096(6) Uani 1 1 d . . . H23A H 0.8560 0.8390 0.2973 0.115 Uiso 1 1 calc R . . H23B H 1.0145 0.8340 0.3221 0.115 Uiso 1 1 calc R . . C24 C 1.0431(16) 0.6814(17) 0.2701(7) 0.126(7) Uani 1 1 d . . . H24A H 1.0531 0.7397 0.2361 0.189 Uiso 1 1 calc R . . H24B H 0.9868 0.6230 0.2609 0.189 Uiso 1 1 calc R . . H24C H 1.1453 0.6210 0.2849 0.189 Uiso 1 1 calc R . . C25 C 0.6267(12) 0.4400(11) 0.8741(5) 0.061(4) Uani 1 1 d . . . H25A H 0.6688 0.4961 0.8940 0.091 Uiso 1 1 calc R . . H25B H 0.7063 0.3812 0.8507 0.091 Uiso 1 1 calc R . . H25C H 0.5922 0.3799 0.9013 0.091 Uiso 1 1 calc R . . C26 C 0.3640(12) 0.6227(10) 0.8773(5) 0.055(3) Uani 1 1 d . . . H26A H 0.4048 0.6776 0.8985 0.083 Uiso 1 1 calc R . . H26B H 0.3346 0.5569 0.9033 0.083 Uiso 1 1 calc R . . H26C H 0.2738 0.6863 0.8552 0.083 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 I1 0.0515(5) 0.0530(4) 0.0570(6) -0.0016(4) -0.0007(4) -0.0148(4) I2 0.0417(4) 0.0511(4) 0.0584(6) -0.0080(4) 0.0036(4) -0.0185(4) I3 0.0459(4) 0.0509(4) 0.0515(6) -0.0060(4) 0.0025(4) -0.0192(4) I4 0.0414(4) 0.0576(5) 0.0431(6) -0.0060(4) 0.0025(4) -0.0119(4) I5 0.0536(5) 0.0547(4) 0.0560(6) -0.0107(4) 0.0066(4) -0.0196(4) Ag1 0.0710(7) 0.0695(6) 0.0733(9) -0.0150(6) 0.0009(6) -0.0210(6) Ag2 0.0714(7) 0.0669(6) 0.0741(9) -0.0020(6) 0.0047(6) -0.0211(6) Ag3 0.0780(8) 0.0807(7) 0.0727(9) -0.0065(6) 0.0036(7) -0.0241(6) Ag4 0.0689(7) 0.0752(6) 0.0796(9) -0.0085(6) 0.0044(7) -0.0253(6) N1 0.041(5) 0.045(5) 0.033(6) -0.004(4) -0.005(4) -0.018(4) C1 0.043(6) 0.052(6) 0.047(8) -0.004(5) 0.004(6) -0.035(5) C2 0.041(6) 0.049(5) 0.023(6) -0.009(5) 0.008(5) -0.024(5) C3 0.069(8) 0.050(6) 0.068(10) -0.020(6) 0.010(7) -0.035(6) C4 0.080(9) 0.040(6) 0.066(10) -0.018(6) 0.019(8) -0.023(6) C5 0.068(8) 0.039(6) 0.069(10) -0.015(6) 0.005(8) -0.011(6) C6 0.068(8) 0.053(7) 0.056(10) -0.008(6) 0.004(7) -0.016(6) C7 0.082(9) 0.053(7) 0.046(9) -0.001(6) -0.013(8) -0.011(7) C8 0.089(10) 0.061(7) 0.052(10) -0.008(7) -0.024(8) -0.010(7) C9 0.087(10) 0.067(8) 0.064(11) -0.001(7) 0.004(9) -0.029(7) C10 0.054(8) 0.080(8) 0.063(10) 0.000(7) 0.005(7) -0.026(7) C11 0.084(10) 0.094(10) 0.082(13) 0.007(9) 0.030(9) -0.033(8) C12 0.115(13) 0.123(12) 0.078(14) -0.003(10) 0.040(11) -0.036(10) C13 0.033(6) 0.039(6) 0.057(9) -0.008(5) 0.000(6) -0.011(5) C14 0.057(8) 0.055(7) 0.039(8) 0.004(6) -0.006(6) -0.014(6) C15 0.107(11) 0.054(7) 0.060(11) -0.010(7) 0.014(9) -0.021(8) C16 0.103(10) 0.054(7) 0.062(10) 0.009(7) 0.044(8) -0.021(7) C17 0.064(8) 0.060(7) 0.051(9) 0.008(6) 0.009(7) -0.021(6) C18 0.086(9) 0.066(7) 0.047(9) -0.006(7) 0.005(8) -0.030(7) C19 0.097(11) 0.066(8) 0.058(10) 0.008(7) -0.036(9) -0.016(8) C20 0.068(9) 0.053(7) 0.057(10) -0.011(7) 0.000(8) -0.004(7) C21 0.081(10) 0.069(8) 0.052(10) 0.005(7) -0.008(8) -0.018(7) C22 0.067(9) 0.075(8) 0.062(11) -0.016(8) 0.003(8) -0.010(7) C23 0.088(11) 0.132(12) 0.067(13) -0.005(10) -0.004(10) -0.041(10) C24 0.059(11) 0.172(16) 0.111(17) -0.034(13) 0.029(11) 0.001(11) C25 0.039(7) 0.059(7) 0.068(10) 0.020(7) -0.018(7) -0.006(6) C26 0.059(7) 0.066(7) 0.051(8) -0.046(6) 0.027(6) -0.025(6) _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 I1 Ag4 2.8215(16) 2_757 ? I1 Ag3 2.8249(17) 2_857 ? I1 Ag1 2.9017(15) . ? I2 Ag2 2.7494(15) . ? I2 Ag1 2.7573(15) . ? I3 Ag3 2.9066(15) 2_857 ? I3 Ag3 2.9241(15) . ? I3 Ag1 2.9291(16) . ? I3 Ag2 2.9296(15) 2_767 ? I4 Ag1 2.8909(15) . ? I4 Ag2 2.8964(16) 2_767 ? I4 Ag4 2.8977(15) 2_757 ? I4 Ag4 2.9003(15) . ? I5 Ag4 2.8252(16) 2_767 ? I5 Ag3 2.8336(16) 2_767 ? I5 Ag2 2.8928(15) . ? Ag2 I4 2.8964(16) 2_767 ? Ag2 I3 2.9297(15) 2_767 ? Ag3 I1 2.8248(17) 2_857 ? Ag3 I5 2.8336(16) 2_767 ? Ag3 I3 2.9066(15) 2_857 ? Ag4 I1 2.8215(16) 2_757 ? Ag4 I5 2.8252(16) 2_767 ? Ag4 I4 2.8977(15) 2_757 ? N1 C13 1.504(12) . ? N1 C25 1.504(11) . ? N1 C1 1.515(12) . ? N1 C26 1.541(12) . ? C1 C2 1.498(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.502(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.527(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.517(16) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.534(15) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.488(16) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.498(16) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.500(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.488(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.480(17) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.565(18) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.501(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.522(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.566(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.467(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.507(15) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.482(17) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.491(16) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.506(17) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.491(16) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.516(18) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.483(18) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag4 I1 Ag3 106.80(5) 2_757 2_857 ? Ag4 I1 Ag1 70.40(4) 2_757 . ? Ag3 I1 Ag1 73.77(4) 2_857 . ? Ag2 I2 Ag1 104.64(5) . . ? Ag3 I3 Ag3 65.68(5) 2_857 . ? Ag3 I3 Ag1 72.18(4) 2_857 . ? Ag3 I3 Ag1 110.16(4) . . ? Ag3 I3 Ag2 108.61(4) 2_857 2_767 ? Ag3 I3 Ag2 76.33(4) . 2_767 ? Ag1 I3 Ag2 67.69(4) . 2_767 ? Ag1 I4 Ag2 68.64(5) . 2_767 ? Ag1 I4 Ag4 69.50(4) . 2_757 ? Ag2 I4 Ag4 110.19(4) 2_767 2_757 ? Ag1 I4 Ag4 108.56(4) . . ? Ag2 I4 Ag4 69.89(4) 2_767 . ? Ag4 I4 Ag4 74.03(5) 2_757 . ? Ag4 I5 Ag3 110.94(5) 2_767 2_767 ? Ag4 I5 Ag2 70.98(4) 2_767 . ? Ag3 I5 Ag2 78.34(4) 2_767 . ? I2 Ag1 I4 109.52(4) . . ? I2 Ag1 I1 105.60(5) . . ? I4 Ag1 I1 109.01(4) . . ? I2 Ag1 I3 115.25(4) . . ? I4 Ag1 I3 111.58(5) . . ? I1 Ag1 I3 105.48(4) . . ? I2 Ag2 I5 108.88(5) . . ? I2 Ag2 I4 108.43(4) . 2_767 ? I5 Ag2 I4 108.61(4) . 2_767 ? I2 Ag2 I3 117.29(5) . 2_767 ? I5 Ag2 I3 101.78(4) . 2_767 ? I4 Ag2 I3 111.41(5) 2_767 2_767 ? I1 Ag3 I5 105.25(5) 2_857 2_767 ? I1 Ag3 I3 108.13(4) 2_857 2_857 ? I5 Ag3 I3 111.39(5) 2_767 2_857 ? I1 Ag3 I3 113.98(5) 2_857 . ? I5 Ag3 I3 103.37(4) 2_767 . ? I3 Ag3 I3 114.32(5) 2_857 . ? I1 Ag4 I5 113.35(5) 2_757 2_767 ? I1 Ag4 I4 111.09(4) 2_757 2_757 ? I5 Ag4 I4 107.69(4) 2_767 2_757 ? I1 Ag4 I4 108.10(4) 2_757 . ? I5 Ag4 I4 110.40(4) 2_767 . ? I4 Ag4 I4 105.97(5) 2_757 . ? C13 N1 C25 109.4(8) . . ? C13 N1 C1 113.5(8) . . ? C25 N1 C1 111.6(7) . . ? C13 N1 C26 108.4(7) . . ? C25 N1 C26 106.7(8) . . ? C1 N1 C26 106.9(8) . . ? C2 C1 N1 114.3(8) . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? N1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 C3 111.2(8) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 115.3(9) . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C3 114.0(8) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 113.7(8) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 117.6(9) . . ? C7 C6 H6A 107.9 . . ? C5 C6 H6A 107.9 . . ? C7 C6 H6B 107.9 . . ? C5 C6 H6B 107.9 . . ? H6A C6 H6B 107.2 . . ? C6 C7 C8 116.9(10) . . ? C6 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? C6 C7 H7B 108.1 . . ? C8 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C7 C8 C9 116.4(10) . . ? C7 C8 H8A 108.2 . . ? C9 C8 H8A 108.2 . . ? C7 C8 H8B 108.2 . . ? C9 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 114.4(10) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C9 117.4(11) . . ? C11 C10 H10A 108.0 . . ? C9 C10 H10A 108.0 . . ? C11 C10 H10B 108.0 . . ? C9 C10 H10B 108.0 . . ? H10A C10 H10B 107.2 . . ? C10 C11 C12 117.2(11) . . ? C10 C11 H11A 108.0 . . ? C12 C11 H11A 108.0 . . ? C10 C11 H11B 108.0 . . ? C12 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N1 115.2(9) . . ? C14 C13 H13A 108.5 . . ? N1 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? N1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C13 C14 C15 112.5(10) . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 112.1(9) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 116.1(10) . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 115.5(10) . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17B 108.4 . . ? C18 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 115.7(10) . . ? C19 C18 H18A 108.4 . . ? C17 C18 H18A 108.4 . . ? C19 C18 H18B 108.4 . . ? C17 C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? C18 C19 C20 117.2(10) . . ? C18 C19 H19A 108.0 . . ? C20 C19 H19A 108.0 . . ? C18 C19 H19B 108.0 . . ? C20 C19 H19B 108.0 . . ? H19A C19 H19B 107.3 . . ? C19 C20 C21 118.2(10) . . ? C19 C20 H20A 107.8 . . ? C21 C20 H20A 107.8 . . ? C19 C20 H20B 107.8 . . ? C21 C20 H20B 107.8 . . ? H20A C20 H20B 107.1 . . ? C22 C21 C20 117.0(10) . . ? C22 C21 H21A 108.1 . . ? C20 C21 H21A 108.1 . . ? C22 C21 H21B 108.1 . . ? C20 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C21 C22 C23 117.4(11) . . ? C21 C22 H22A 108.0 . . ? C23 C22 H22A 108.0 . . ? C21 C22 H22B 108.0 . . ? C23 C22 H22B 108.0 . . ? H22A C22 H22B 107.2 . . ? C24 C23 C22 115.8(13) . . ? C24 C23 H23A 108.3 . . ? C22 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? C22 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 H26A 109.5 . . ? N1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.989 _refine_diff_density_min -2.160 _refine_diff_density_rms 0.402 # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 863851' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '16(C13 H21 Cl N), 4(Ag4 I8), C H2 Cl2' _chemical_formula_sum 'C209 H338 Ag16 Cl18 I32 N16' _chemical_formula_weight 9499.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 12.263(3) _cell_length_b 24.775(5) _cell_length_c 24.888(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.51(3) _cell_angle_gamma 90.00 _cell_volume 7559(3) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 48955 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.5 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4458 _exptl_absorpt_coefficient_mu 4.480 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.036 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.1X0.1 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 60557 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.1401 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.50 _reflns_number_total 26101 _reflns_number_gt 19314 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear, Rigaku' _computing_cell_refinement 'CrystalClear, Rigaku' _computing_data_reduction 'CrystalClear, Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _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^)+(0.0010P)^2^+5.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00122(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.438(17) _refine_ls_number_reflns 26101 _refine_ls_number_parameters 1326 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2046 _refine_ls_wR_factor_gt 0.1897 _refine_ls_goodness_of_fit_ref 1.458 _refine_ls_restrained_S_all 1.458 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL XuB-5 in Pc CELL 0.71073 12.2631 24.7754 24.8882 90.000 91.515 90.000 ZERR 1.00 0.0025 0.0050 0.0050 0.000 0.030 0.000 LATT -1 SYMM X, -Y, 0.5+Z SFAC C H N CL AG I UNIT 209 338 16 18 16 32 OMIT -2 51 OMIT 6 19 -5 OMIT 7 16 -14 OMIT 7 18 -14 L.S. 4 DAMP 1500 ACTA BOND $H FMAP 2 PLAN 10 TWIN DFIX 1.46 0.01 N1 C1 N1 C8 N1 C10 N1 C12 N2 C14 N2 C21 N2 C23 N2 C25 DFIX 1.46 0.01 N3 C27 N3 C34 N3 C36 N3 C38 N4 C40 N4 C47 N4 C49 N4 C51 DFIX 1.46 0.01 N5 C53 N5 C60 N5 C62 N5 C64 N6 C66 N6 C73 N6 C75 N6 C77 DFIX 1.46 0.01 N7 C79 N7 C86 N7 C88 N7 C90 N8 C92 N8 C99 N8 C101 N8 C103 DFIX 1.54 0.01 C8 C9 C10 C11 C12 C13 C21 C22 C23 C24 C25 C26 DFIX 1.54 0.01 C34 C35 C36 C37 C38 C39 C47 C48 C49 C50 C51 C52 DFIX 1.54 0.01 C60 C61 C62 C63 C64 C65 C73 C74 C75 C76 C77 C78 DFIX 1.54 0.01 C86 C87 C88 C89 C90 C91 C99 C100 C101 C102 C103 C104 DFIX 1.72 0.01 CL9 C105 CL10 C105 DFIX 1.39 0.01 C29 C30 C31 C32 C80 C85 C81 C82 C84 C85 C97 C98 C2 C7 C41 C46 ISOR 0.01 C27 C31 WGHT 0.001000 5.000000 EXTI 0.001216 BASF 0.43818 FVAR 0.05030 I1 6 0.591692 0.534598 0.226132 11.00000 0.05159 0.04320 = 0.06095 -0.00079 -0.00256 0.00004 I2 6 0.234944 0.593733 0.181943 11.00000 0.06403 0.06234 = 0.07307 0.00975 0.00177 0.00686 I3 6 0.302023 0.409880 0.224326 11.00000 0.06672 0.05420 = 0.06852 -0.00322 -0.00529 -0.00261 I4 6 0.320868 0.545010 0.358948 11.00000 0.05388 0.05849 = 0.06201 0.00102 0.00924 0.00146 I5 6 0.205176 0.369978 0.398447 11.00000 0.06740 0.05995 = 0.07904 0.01201 0.00083 -0.01059 I6 6 0.575728 0.404536 0.360134 11.00000 0.05824 0.05024 = 0.06633 0.00248 -0.00240 0.00644 I7 6 0.666523 0.355484 0.187034 11.00000 0.09097 0.05915 = 0.08585 -0.00965 0.02296 0.00187 I8 6 0.668685 0.583650 0.407930 11.00000 0.07474 0.05836 = 0.05581 -0.00615 -0.00101 -0.01232 I9 6 0.565222 1.037448 0.339188 11.00000 0.06064 0.05305 = 0.06988 -0.00077 -0.00016 -0.00376 I10 6 0.224767 1.095118 0.387296 11.00000 0.09383 0.05545 = 0.05975 -0.00164 0.01587 0.01158 I11 6 0.294333 0.906893 0.345404 11.00000 0.05675 0.05862 = 0.06129 0.00168 0.00160 0.00190 I12 6 0.295844 1.038182 0.210823 11.00000 0.07038 0.04764 = 0.05026 -0.00259 0.00206 0.00196 I13 6 0.194847 0.863690 0.162452 11.00000 0.11362 0.07270 = 0.06994 -0.01357 -0.01963 -0.00186 I14 6 0.554338 0.898430 0.215278 11.00000 0.08453 0.05021 = 0.08353 -0.00186 0.01326 -0.00049 I15 6 0.660055 0.856710 0.392289 11.00000 0.08127 0.05893 = 0.07839 0.00731 0.00386 0.01009 I16 6 0.662301 1.062083 0.154000 11.00000 0.08337 0.09610 = 0.08742 0.03474 -0.01065 -0.02335 AG1 5 0.354204 0.523848 0.245040 11.00000 0.07577 0.06877 = 0.07762 0.00852 -0.00254 0.00733 AG2 5 0.345431 0.430603 0.337700 11.00000 0.07357 0.06834 = 0.08295 0.00616 0.00508 -0.00677 AG3 5 0.533956 0.421802 0.244442 11.00000 0.08476 0.06113 = 0.08139 -0.00639 0.00428 0.00153 AG4 5 0.546232 0.518899 0.338915 11.00000 0.07020 0.06617 = 0.07452 -0.00926 -0.00207 -0.00425 AG5 5 0.333822 1.020159 0.326447 11.00000 0.07207 0.07304 = 0.07226 -0.00667 0.00622 0.00370 AG6 5 0.327460 0.922016 0.231148 11.00000 0.09959 0.06598 = 0.08027 -0.00975 -0.00938 0.00108 AG7 5 0.530521 0.921915 0.328693 11.00000 0.08727 0.07094 = 0.09445 0.00503 -0.00017 0.00838 AG8 5 0.530322 1.014030 0.226225 11.00000 0.09204 0.07025 = 0.08102 0.00546 0.00584 -0.00533 CL1 4 1.179917 0.609610 0.481669 11.00000 0.11646 0.18748 = 0.10050 0.00686 0.01367 0.08091 CL2 4 0.666974 0.160832 0.412610 11.00000 0.19512 0.08965 = 0.31625 0.06375 -0.16186 -0.06653 CL3 4 0.782931 0.311231 0.576849 11.00000 0.19119 0.24321 = 0.16051 0.06059 0.10639 0.05799 CL4 4 -0.051715 0.173635 0.162692 11.00000 0.15569 0.17831 = 0.17048 0.03600 -0.08803 -0.04832 CL5 4 0.935821 0.405096 0.509104 11.00000 0.08623 0.10495 = 0.14993 -0.03327 0.02128 0.02291 CL6 4 0.122285 1.228759 0.051493 11.00000 0.11337 0.08351 = 0.27622 -0.02027 0.01767 0.04264 CL7 4 1.097189 0.720734 0.370691 11.00000 0.12081 0.21135 = 0.21492 -0.06725 0.03455 -0.05579 CL8 4 0.969316 0.878718 0.512433 11.00000 0.15307 0.11731 = 0.17830 0.05157 -0.03836 -0.03790 N1 3 0.754519 0.722484 0.520615 11.00000 0.05699 0.04775 = 0.05100 0.00156 0.00580 -0.00117 N2 3 1.099718 0.221493 0.504137 11.00000 0.07719 0.04525 = 0.04952 0.01406 -0.00472 -0.00531 N3 3 0.492610 0.282974 0.768728 11.00000 0.05854 0.01881 = 0.05646 -0.00028 -0.00529 0.00638 N4 3 0.411794 0.220362 0.257304 11.00000 0.07146 0.03721 = 0.07315 0.01410 -0.01067 -0.01366 N5 3 0.455138 0.469895 0.539215 11.00000 0.06003 0.06567 = 0.03625 0.01131 -0.00437 -0.00432 N6 3 0.373231 1.018851 0.030868 11.00000 0.08562 0.04262 = 0.04388 0.00785 -0.00316 0.01203 N7 3 0.949547 0.504263 0.300735 11.00000 0.02860 0.11749 = 0.07361 0.02080 -0.00215 -0.01213 N8 3 0.941874 0.981334 0.288668 11.00000 0.02757 0.09058 = 0.16250 0.03738 -0.01458 -0.01369 C1 1 0.787634 0.667093 0.535218 11.00000 0.07314 0.02741 = 0.05000 -0.00811 -0.00035 -0.01403 AFIX 23 H1A 2 0.769390 0.643554 0.505161 11.00000 -1.20000 H1B 2 0.744643 0.655540 0.565290 11.00000 -1.20000 AFIX 0 C2 1 0.909817 0.658922 0.550550 11.00000 0.09752 0.05191 = 0.03404 0.00096 -0.00765 0.00675 C3 1 0.942618 0.662481 0.604383 11.00000 0.05256 0.06678 = 0.10579 0.00569 -0.02138 0.00628 AFIX 43 H3A 2 0.892086 0.672063 0.629912 11.00000 -1.20000 AFIX 0 C4 1 1.052900 0.651613 0.620982 11.00000 0.08528 0.09087 = 0.08346 -0.00913 -0.00815 0.00608 AFIX 43 H4A 2 1.077506 0.656977 0.656244 11.00000 -1.20000 AFIX 0 C5 1 1.119542 0.633114 0.582674 11.00000 0.06583 0.06235 = 0.10192 0.01243 0.01714 0.03892 AFIX 43 H5A 2 1.190563 0.623283 0.592363 11.00000 -1.20000 AFIX 0 C6 1 1.085697 0.628451 0.530271 11.00000 0.05694 0.08183 = 0.07790 -0.00011 -0.00218 0.03060 C7 1 0.983823 0.639736 0.513830 11.00000 0.07374 0.05125 = 0.05084 -0.00258 0.01246 0.00471 AFIX 43 H7A 2 0.962506 0.634791 0.478030 11.00000 -1.20000 AFIX 0 C8 1 0.825330 0.748392 0.481103 11.00000 0.07732 0.03740 = 0.06804 -0.00061 -0.00716 -0.01624 AFIX 23 H8A 2 0.899693 0.747826 0.495379 11.00000 -1.20000 H8B 2 0.803745 0.785915 0.477548 11.00000 -1.20000 AFIX 0 C9 1 0.824242 0.722914 0.424614 11.00000 0.11522 0.05705 = 0.08198 -0.01160 -0.00332 0.01825 AFIX 33 H9A 2 0.895856 0.725181 0.410104 11.00000 -1.50000 H9B 2 0.773353 0.741952 0.401582 11.00000 -1.50000 H9C 2 0.802839 0.685735 0.426962 11.00000 -1.50000 AFIX 0 C10 1 0.760419 0.754232 0.570515 11.00000 0.10207 0.05481 = 0.06536 -0.01581 0.00659 0.00332 AFIX 23 H10A 2 0.836422 0.757781 0.581757 11.00000 -1.20000 H10B 2 0.723687 0.734352 0.598321 11.00000 -1.20000 AFIX 0 C11 1 0.709832 0.811173 0.566439 11.00000 0.18199 0.04645 = 0.11146 -0.05985 -0.01559 0.02408 AFIX 33 H11A 2 0.714008 0.828303 0.601031 11.00000 -1.50000 H11B 2 0.634853 0.808343 0.554693 11.00000 -1.50000 H11C 2 0.749170 0.832292 0.541059 11.00000 -1.50000 AFIX 0 C12 1 0.642647 0.720719 0.497921 11.00000 0.04505 0.04009 = 0.09979 -0.00741 0.00676 0.00614 AFIX 23 H12A 2 0.639491 0.694269 0.469186 11.00000 -1.20000 H12B 2 0.625109 0.755637 0.482326 11.00000 -1.20000 AFIX 0 C13 1 0.555744 0.706427 0.539254 11.00000 0.06420 0.18864 = 0.13386 0.02882 0.02597 -0.01751 AFIX 33 H13A 2 0.486888 0.721684 0.528017 11.00000 -1.50000 H13B 2 0.577247 0.720789 0.573758 11.00000 -1.50000 H13C 2 0.548989 0.667908 0.541722 11.00000 -1.50000 AFIX 0 C14 1 1.066562 0.224700 0.446456 11.00000 0.15150 0.06196 = 0.02394 0.01230 0.00312 0.03462 AFIX 23 H14A 2 1.084278 0.190548 0.429745 11.00000 -1.20000 H14B 2 1.110632 0.252233 0.429809 11.00000 -1.20000 AFIX 0 C15 1 0.948343 0.237013 0.433460 11.00000 0.08984 0.05984 = 0.05985 0.00669 -0.02883 0.04195 C16 1 0.916338 0.289901 0.424360 11.00000 0.06443 0.05151 = 0.07749 0.00301 -0.02553 -0.00126 AFIX 43 H16A 2 0.969474 0.316676 0.425974 11.00000 -1.20000 AFIX 0 C17 1 0.813208 0.304577 0.413380 11.00000 0.08980 0.02917 = 0.10247 0.00462 -0.01313 -0.01557 AFIX 43 H17A 2 0.795893 0.340757 0.408018 11.00000 -1.20000 AFIX 0 C18 1 0.731895 0.265424 0.410014 11.00000 0.08519 0.06407 = 0.11969 0.01080 -0.03621 0.00455 AFIX 43 H18A 2 0.659671 0.274598 0.402190 11.00000 -1.20000 AFIX 0 C19 1 0.764614 0.208875 0.419322 11.00000 0.09960 0.02529 = 0.13254 0.02887 -0.01137 -0.00700 C20 1 0.876233 0.197768 0.427916 11.00000 0.08011 0.05101 = 0.13162 -0.01628 -0.06627 0.00760 AFIX 43 H20A 2 0.899608 0.162089 0.429721 11.00000 -1.20000 AFIX 0 C21 1 1.085932 0.276270 0.526216 11.00000 0.09090 0.05578 = 0.07191 -0.00263 -0.00807 0.01482 AFIX 23 H21A 2 1.008553 0.284404 0.526097 11.00000 -1.20000 H21B 2 1.119780 0.301677 0.502135 11.00000 -1.20000 AFIX 0 C22 1 1.132632 0.286115 0.583048 11.00000 0.20227 0.05070 = 0.06969 -0.02655 -0.02790 0.02246 AFIX 33 H22A 2 1.101729 0.318523 0.597321 11.00000 -1.50000 H22B 2 1.210439 0.289869 0.581803 11.00000 -1.50000 H22C 2 1.115001 0.256124 0.605647 11.00000 -1.50000 AFIX 0 C23 1 1.028101 0.184847 0.533401 11.00000 0.05445 0.07602 = 0.06024 -0.01102 0.01439 0.01195 AFIX 23 H23A 2 0.953459 0.196427 0.526560 11.00000 -1.20000 H23B 2 1.043550 0.189730 0.571516 11.00000 -1.20000 AFIX 0 C24 1 1.033925 0.123741 0.521307 11.00000 0.08393 0.03837 = 0.10783 0.00246 -0.00265 0.01155 AFIX 33 H24A 2 1.022029 0.103742 0.553666 11.00000 -1.50000 H24B 2 1.104538 0.115071 0.507957 11.00000 -1.50000 H24C 2 0.978825 0.114455 0.494785 11.00000 -1.50000 AFIX 0 C25 1 1.214185 0.203505 0.507643 11.00000 0.07513 0.03524 = 0.06285 0.01463 0.00589 -0.00780 AFIX 23 H25A 2 1.218066 0.169112 0.489169 11.00000 -1.20000 H25B 2 1.231649 0.196593 0.545256 11.00000 -1.20000 AFIX 0 C26 1 1.305191 0.239287 0.486035 11.00000 0.07793 0.09057 = 0.15434 0.08552 0.00882 0.02558 AFIX 33 H26A 2 1.370082 0.218140 0.482078 11.00000 -1.50000 H26B 2 1.319798 0.268305 0.510755 11.00000 -1.50000 H26C 2 1.282655 0.253814 0.451749 11.00000 -1.50000 AFIX 0 C27 1 0.485445 0.315014 0.719195 11.00000 0.04931 0.02313 = 0.06114 0.00092 0.00475 -0.00409 AFIX 23 H27A 2 0.527625 0.347707 0.725056 11.00000 -1.20000 H27B 2 0.409960 0.325796 0.713589 11.00000 -1.20000 AFIX 0 C28 1 0.522147 0.289925 0.669041 11.00000 0.06535 0.02714 = 0.08415 -0.01395 -0.00581 -0.00673 C29 1 0.469052 0.248734 0.641947 11.00000 0.09222 0.04265 = 0.08971 0.01017 -0.01248 -0.02107 AFIX 43 H29A 2 0.404732 0.235219 0.655656 11.00000 -1.20000 AFIX 0 C30 1 0.508015 0.226663 0.594947 11.00000 0.23370 0.05882 = 0.11145 -0.02653 -0.05282 0.00966 AFIX 43 H30A 2 0.469044 0.199930 0.576560 11.00000 -1.20000 AFIX 0 C31 1 0.610048 0.246080 0.575324 11.00000 0.11336 0.08334 = 0.10031 0.01181 0.00342 0.02326 AFIX 43 H31A 2 0.636840 0.232263 0.543534 11.00000 -1.20000 AFIX 0 C32 1 0.669178 0.285479 0.603591 11.00000 0.11862 0.03673 = 0.09305 -0.01641 0.03825 -0.00645 C33 1 0.621213 0.308253 0.648226 11.00000 0.07647 0.05087 = 0.09765 0.01122 -0.00507 0.02176 AFIX 43 H33A 2 0.656356 0.337078 0.665215 11.00000 -1.20000 AFIX 0 C34 1 0.416319 0.237211 0.768446 11.00000 0.10096 0.04835 = 0.05608 -0.00642 0.01222 -0.01983 AFIX 23 H34A 2 0.428050 0.216947 0.801443 11.00000 -1.20000 H34B 2 0.433910 0.213572 0.738839 11.00000 -1.20000 AFIX 0 C35 1 0.294319 0.251997 0.763300 11.00000 0.09433 0.07871 = 0.11460 -0.04355 0.02859 -0.02775 AFIX 33 H35A 2 0.253377 0.220949 0.751545 11.00000 -1.50000 H35B 2 0.284626 0.280582 0.737575 11.00000 -1.50000 H35C 2 0.269016 0.263663 0.797578 11.00000 -1.50000 AFIX 0 C36 1 0.601891 0.259576 0.777936 11.00000 0.07068 0.05448 = 0.07892 0.04267 0.02786 0.01347 AFIX 23 H36A 2 0.618874 0.237101 0.747361 11.00000 -1.20000 H36B 2 0.599975 0.236364 0.809283 11.00000 -1.20000 AFIX 0 C37 1 0.694494 0.300954 0.786459 11.00000 0.06400 0.14124 = 0.07390 0.01123 0.01227 -0.03233 AFIX 33 H37A 2 0.759833 0.282617 0.798213 11.00000 -1.50000 H37B 2 0.674129 0.326698 0.813221 11.00000 -1.50000 H37C 2 0.707233 0.319336 0.753254 11.00000 -1.50000 AFIX 0 C38 1 0.468665 0.322009 0.811578 11.00000 0.10691 0.07539 = 0.04446 0.00482 0.03116 0.01294 AFIX 23 H38A 2 0.399271 0.339068 0.802779 11.00000 -1.20000 H38B 2 0.524053 0.349957 0.811441 11.00000 -1.20000 AFIX 0 C39 1 0.463495 0.299113 0.868863 11.00000 0.15972 0.06524 = 0.09387 -0.02137 0.06306 -0.03431 AFIX 33 H39A 2 0.474727 0.327727 0.894423 11.00000 -1.50000 H39B 2 0.519256 0.272276 0.874039 11.00000 -1.50000 H39C 2 0.393274 0.283036 0.873900 11.00000 -1.50000 AFIX 0 C40 1 0.318327 0.185929 0.269469 11.00000 0.07919 0.03811 = 0.06735 -0.00054 0.00196 -0.02732 AFIX 23 H40A 2 0.325027 0.175904 0.307086 11.00000 -1.20000 H40B 2 0.325020 0.153014 0.248712 11.00000 -1.20000 AFIX 0 C41 1 0.199468 0.208367 0.259205 11.00000 0.08156 0.06992 = 0.07254 0.01610 0.00978 -0.00678 C42 1 0.134703 0.189070 0.217981 11.00000 0.18212 0.03982 = 0.08149 -0.00220 -0.05272 -0.01283 AFIX 43 H42A 2 0.161226 0.163348 0.194452 11.00000 -1.20000 AFIX 0 C43 1 0.029300 0.208272 0.211710 11.00000 0.12064 0.08789 = 0.15106 0.00781 -0.07039 0.03822 C44 1 -0.009028 0.248165 0.244433 11.00000 0.07108 0.13422 = 0.13549 0.03173 0.01361 0.00983 AFIX 43 H44A 2 -0.079887 0.261134 0.240119 11.00000 -1.20000 AFIX 0 C45 1 0.058733 0.267982 0.282912 11.00000 0.10783 0.09984 = 0.10624 -0.00574 0.01838 0.01701 AFIX 43 H45A 2 0.034009 0.295848 0.304465 11.00000 -1.20000 AFIX 0 C46 1 0.161000 0.249282 0.291690 11.00000 0.06588 0.06302 = 0.12480 -0.04608 -0.01939 0.02281 AFIX 43 H46A 2 0.205060 0.263621 0.319126 11.00000 -1.20000 AFIX 0 C47 1 0.425104 0.267256 0.293362 11.00000 0.08353 0.03609 = 0.10860 -0.00884 -0.01783 -0.01872 AFIX 23 H47A 2 0.365153 0.292133 0.286768 11.00000 -1.20000 H47B 2 0.492226 0.285855 0.285118 11.00000 -1.20000 AFIX 0 C48 1 0.428293 0.251301 0.353175 11.00000 0.15972 0.05606 = 0.07856 -0.02453 -0.03779 0.02115 AFIX 33 H48A 2 0.453559 0.281353 0.374434 11.00000 -1.50000 H48B 2 0.476919 0.221304 0.358553 11.00000 -1.50000 H48C 2 0.356390 0.241300 0.363832 11.00000 -1.50000 AFIX 0 C49 1 0.500757 0.181062 0.263016 11.00000 0.14434 0.04764 = 0.08024 0.00459 0.01584 0.02382 AFIX 23 H49A 2 0.488619 0.152593 0.236779 11.00000 -1.20000 H49B 2 0.497710 0.164821 0.298407 11.00000 -1.20000 AFIX 0 C50 1 0.616377 0.204223 0.255813 11.00000 0.07615 0.10934 = 0.19251 0.04595 0.01927 0.01430 AFIX 33 H50A 2 0.669631 0.177136 0.265035 11.00000 -1.50000 H50B 2 0.626768 0.234977 0.278848 11.00000 -1.50000 H50C 2 0.624602 0.214953 0.219078 11.00000 -1.50000 AFIX 0 C51 1 0.410603 0.241557 0.202231 11.00000 0.05822 0.14293 = 0.10432 0.04209 0.01761 -0.00449 AFIX 23 H51A 2 0.476338 0.262862 0.198517 11.00000 -1.20000 H51B 2 0.349503 0.266297 0.198841 11.00000 -1.20000 AFIX 0 C52 1 0.403233 0.202933 0.153909 11.00000 0.21485 0.18782 = 0.07679 -0.00286 0.01713 -0.09178 AFIX 33 H52A 2 0.374356 0.221918 0.123063 11.00000 -1.50000 H52B 2 0.356096 0.173283 0.162102 11.00000 -1.50000 H52C 2 0.474647 0.189486 0.146392 11.00000 -1.50000 AFIX 0 C53 1 0.545515 0.489809 0.507049 11.00000 0.03705 0.03255 = 0.06502 -0.00533 0.00760 -0.00293 AFIX 23 H53A 2 0.531953 0.527492 0.498674 11.00000 -1.20000 H53B 2 0.544703 0.470193 0.473311 11.00000 -1.20000 AFIX 0 C54 1 0.659206 0.485164 0.532639 11.00000 0.05611 0.05120 = 0.07962 -0.00539 0.01138 0.01570 C55 1 0.738867 0.450064 0.513474 11.00000 0.08286 0.04078 = 0.08173 -0.00280 0.01503 0.00001 AFIX 43 H55A 2 0.718018 0.425667 0.486726 11.00000 -1.20000 AFIX 0 C56 1 0.844165 0.449259 0.531260 11.00000 0.06400 0.05112 = 0.07947 0.00462 0.02420 0.00961 C57 1 0.877315 0.488555 0.564887 11.00000 0.06775 0.08080 = 0.11910 -0.01113 -0.01132 0.00566 AFIX 43 H57A 2 0.951175 0.491914 0.573698 11.00000 -1.20000 AFIX 0 C58 1 0.802454 0.524939 0.587198 11.00000 0.03964 0.05727 = 0.13365 -0.02181 -0.00346 -0.01129 AFIX 43 H58A 2 0.825196 0.548970 0.613924 11.00000 -1.20000 AFIX 0 C59 1 0.693102 0.524533 0.568646 11.00000 0.07946 0.03476 = 0.09517 -0.02307 0.01357 -0.00419 AFIX 43 H59A 2 0.644311 0.550413 0.580462 11.00000 -1.20000 AFIX 0 C60 1 0.471231 0.415079 0.560681 11.00000 0.07333 0.07882 = 0.06627 0.04398 0.00162 0.00279 AFIX 23 H60A 2 0.411071 0.406413 0.583699 11.00000 -1.20000 H60B 2 0.537674 0.414477 0.582703 11.00000 -1.20000 AFIX 0 C61 1 0.478808 0.371559 0.517286 11.00000 0.10574 0.04256 = 0.15629 0.03963 -0.00721 0.01134 AFIX 33 H61A 2 0.470072 0.336614 0.533272 11.00000 -1.50000 H61B 2 0.548746 0.373586 0.500961 11.00000 -1.50000 H61C 2 0.422358 0.377181 0.490408 11.00000 -1.50000 AFIX 0 C62 1 0.438493 0.505085 0.585744 11.00000 0.06486 0.07254 = 0.06203 0.01836 -0.00979 -0.02155 AFIX 23 H62A 2 0.501445 0.501210 0.609859 11.00000 -1.20000 H62B 2 0.375874 0.491551 0.604580 11.00000 -1.20000 AFIX 0 C63 1 0.420595 0.565754 0.575780 11.00000 0.12069 0.08057 = 0.08393 0.00369 0.01014 0.05717 AFIX 33 H63A 2 0.422344 0.584556 0.609519 11.00000 -1.50000 H63B 2 0.351027 0.571220 0.558019 11.00000 -1.50000 H63C 2 0.477245 0.579351 0.553582 11.00000 -1.50000 AFIX 0 C64 1 0.355822 0.473751 0.504671 11.00000 0.04702 0.08221 = 0.07609 0.00274 -0.01097 0.00591 AFIX 23 H64A 2 0.364568 0.450235 0.473923 11.00000 -1.20000 H64B 2 0.349966 0.510415 0.491231 11.00000 -1.20000 AFIX 0 C65 1 0.247776 0.459034 0.531548 11.00000 0.09324 0.11627 = 0.08943 0.00114 0.00094 0.01715 AFIX 33 H65A 2 0.188499 0.462463 0.505801 11.00000 -1.50000 H65B 2 0.236182 0.482969 0.561188 11.00000 -1.50000 H65C 2 0.251452 0.422517 0.544368 11.00000 -1.50000 AFIX 0 C66 1 0.387871 1.070129 0.060904 11.00000 0.06616 0.04801 = 0.04811 -0.02346 -0.00250 -0.01041 AFIX 23 H66A 2 0.463980 1.072926 0.072187 11.00000 -1.20000 H66B 2 0.345464 1.067971 0.093185 11.00000 -1.20000 AFIX 0 C67 1 0.356995 1.120706 0.032135 11.00000 0.04593 0.05018 = 0.05138 -0.00261 0.00006 -0.00117 C68 1 0.264178 1.147074 0.050647 11.00000 0.04916 0.05557 = 0.09167 -0.00942 0.00100 0.01967 AFIX 43 H68A 2 0.223959 1.131886 0.077967 11.00000 -1.20000 AFIX 0 C69 1 0.233309 1.194905 0.028478 11.00000 0.09853 0.04668 = 0.16640 -0.00727 -0.02427 0.05396 C70 1 0.290283 1.212601 -0.014535 11.00000 0.15616 0.06137 = 0.12824 0.06354 -0.06358 -0.03342 AFIX 43 H70A 2 0.260584 1.240738 -0.034866 11.00000 -1.20000 AFIX 0 C71 1 0.390616 1.191208 -0.030144 11.00000 0.12188 0.13652 = 0.14121 0.09922 0.01464 0.03379 AFIX 43 H71A 2 0.434869 1.208181 -0.054780 11.00000 -1.20000 AFIX 0 C72 1 0.416526 1.145395 -0.007092 11.00000 0.09475 0.03628 = 0.08052 0.01177 0.00782 -0.01150 AFIX 43 H72A 2 0.479689 1.128234 -0.017953 11.00000 -1.20000 AFIX 0 C73 1 0.260631 1.012413 0.009788 11.00000 0.06606 0.03320 = 0.08388 -0.01804 -0.02370 -0.00486 AFIX 23 H73A 2 0.256527 0.979803 -0.011739 11.00000 -1.20000 H73B 2 0.243110 1.042635 -0.013665 11.00000 -1.20000 AFIX 0 C74 1 0.174677 1.009181 0.053567 11.00000 0.06604 0.05932 = 0.09991 -0.01300 0.00589 -0.00499 AFIX 33 H74A 2 0.103500 1.005378 0.037006 11.00000 -1.50000 H74B 2 0.177172 1.041553 0.074763 11.00000 -1.50000 H74C 2 0.189706 0.978596 0.076258 11.00000 -1.50000 AFIX 0 C75 1 0.403423 0.974756 0.068016 11.00000 0.07223 0.05069 = 0.06019 -0.00904 0.01434 0.01502 AFIX 23 H75A 2 0.356860 0.977487 0.098803 11.00000 -1.20000 H75B 2 0.477538 0.981369 0.080940 11.00000 -1.20000 AFIX 0 C76 1 0.397812 0.915884 0.047837 11.00000 0.13668 0.02140 = 0.09426 0.00924 -0.00105 0.00801 AFIX 33 H76A 2 0.382408 0.892345 0.077321 11.00000 -1.50000 H76B 2 0.466444 0.906056 0.032941 11.00000 -1.50000 H76C 2 0.341094 0.912637 0.020699 11.00000 -1.50000 AFIX 0 C77 1 0.439289 1.017982 -0.018256 11.00000 0.09183 0.04559 = 0.03584 -0.00186 0.00073 -0.02878 AFIX 23 H77A 2 0.417547 1.048538 -0.040428 11.00000 -1.20000 H77B 2 0.420672 0.985542 -0.038300 11.00000 -1.20000 AFIX 0 C78 1 0.564293 1.019713 -0.010240 11.00000 0.13475 0.05872 = 0.05915 0.02127 0.03785 0.03250 AFIX 33 H78A 2 0.597924 1.018993 -0.044628 11.00000 -1.50000 H78B 2 0.587983 0.989001 0.010489 11.00000 -1.50000 H78C 2 0.584835 1.052224 0.008415 11.00000 -1.50000 AFIX 0 C79 1 0.881925 0.552845 0.297780 11.00000 0.04850 0.11230 = 0.11142 0.00529 -0.00527 0.03824 AFIX 23 H79A 2 0.841745 0.555121 0.330756 11.00000 -1.20000 H79B 2 0.828811 0.548043 0.268598 11.00000 -1.20000 AFIX 0 C80 1 0.940409 0.608878 0.289242 11.00000 0.07496 0.10447 = 0.09698 0.01788 0.05614 0.02143 C81 1 0.985866 0.636249 0.332996 11.00000 0.06432 0.13125 = 0.08761 -0.00871 0.01381 -0.00678 AFIX 43 H81A 2 0.981652 0.623905 0.368168 11.00000 -1.20000 AFIX 0 C82 1 1.038164 0.683731 0.319367 11.00000 0.08154 0.07355 = 0.17073 -0.03579 0.02043 -0.00261 C83 1 1.024976 0.708748 0.269287 11.00000 0.06060 0.11867 = 0.24951 -0.03738 0.03775 0.01153 AFIX 43 H83A 2 1.049642 0.743938 0.264965 11.00000 -1.20000 AFIX 0 C84 1 0.976911 0.682817 0.226743 11.00000 0.14661 0.10977 = 0.13277 0.01234 0.02418 0.01231 AFIX 43 H84A 2 0.972978 0.697785 0.192479 11.00000 -1.20000 AFIX 0 C85 1 0.933954 0.632146 0.238241 11.00000 0.07785 0.12566 = 0.16098 0.04010 0.01334 0.02700 AFIX 43 H85A 2 0.899343 0.612946 0.210580 11.00000 -1.20000 AFIX 0 C86 1 1.020186 0.505480 0.349350 11.00000 0.05729 0.14314 = 0.15537 0.07450 -0.01014 0.04240 AFIX 23 H86A 2 1.065844 0.537357 0.347438 11.00000 -1.20000 H86B 2 1.068127 0.474381 0.348240 11.00000 -1.20000 AFIX 0 C87 1 0.965939 0.505688 0.404378 11.00000 0.11114 0.16279 = 0.15651 0.04842 -0.04705 0.02785 AFIX 33 H87A 2 1.020884 0.509513 0.432314 11.00000 -1.50000 H87B 2 0.927415 0.472373 0.409162 11.00000 -1.50000 H87C 2 0.915662 0.535308 0.406001 11.00000 -1.50000 AFIX 0 C88 1 0.865907 0.462997 0.307128 11.00000 0.08284 0.09319 = 0.16709 0.08546 -0.02563 0.01205 AFIX 23 H88A 2 0.809975 0.467477 0.279194 11.00000 -1.20000 H88B 2 0.831942 0.467932 0.341542 11.00000 -1.20000 AFIX 0 C89 1 0.912286 0.405475 0.304167 11.00000 0.14622 0.21042 = 0.16916 0.07734 -0.05187 -0.10063 AFIX 33 H89A 2 0.908597 0.388649 0.338818 11.00000 -1.50000 H89B 2 0.986884 0.406999 0.293502 11.00000 -1.50000 H89C 2 0.870345 0.384848 0.278334 11.00000 -1.50000 AFIX 0 C90 1 1.027736 0.496459 0.257580 11.00000 0.05319 0.07137 = 0.14698 0.02206 0.04309 0.00176 AFIX 23 H90A 2 1.071581 0.464694 0.265415 11.00000 -1.20000 H90B 2 1.076329 0.527313 0.256553 11.00000 -1.20000 AFIX 0 C91 1 0.970462 0.489653 0.202118 11.00000 0.11579 0.12333 = 0.09491 -0.00606 0.05341 -0.00261 AFIX 33 H91A 2 0.999697 0.458679 0.184339 11.00000 -1.50000 H91B 2 0.982411 0.521285 0.180787 11.00000 -1.50000 H91C 2 0.893606 0.484756 0.206685 11.00000 -1.50000 AFIX 0 C92 1 1.007761 0.987160 0.338185 11.00000 0.04266 0.02267 = 0.34584 0.01928 0.00451 0.00979 AFIX 23 H92A 2 1.063741 0.959512 0.337804 11.00000 -1.20000 H92B 2 1.044752 1.021696 0.336417 11.00000 -1.20000 AFIX 0 C93 1 0.956177 0.984281 0.390361 11.00000 0.02765 0.10896 = 0.13574 0.00235 -0.00188 0.00399 C94 1 0.980264 0.937056 0.426897 11.00000 0.05843 0.07637 = 0.13437 0.01085 -0.00581 0.00791 AFIX 43 H94A 2 1.028522 0.910212 0.416700 11.00000 -1.20000 AFIX 0 C95 1 0.931170 0.934247 0.474335 11.00000 0.13075 0.12949 = 0.09970 0.04230 -0.04856 -0.09473 C96 1 0.860481 0.967361 0.500690 11.00000 0.06303 0.20213 = 0.16967 -0.00975 -0.01414 -0.00330 AFIX 43 H96A 2 0.830825 0.961686 0.534231 11.00000 -1.20000 AFIX 0 C97 1 0.842139 1.012227 0.465851 11.00000 0.11405 0.09441 = 0.14397 -0.03488 0.04308 -0.04407 AFIX 43 H97A 2 0.795017 1.038721 0.477965 11.00000 -1.20000 AFIX 0 C98 1 0.886746 1.020955 0.415682 11.00000 0.05771 0.15467 = 0.18330 0.06017 -0.02622 0.02277 AFIX 43 H98A 2 0.869554 1.052967 0.397876 11.00000 -1.20000 AFIX 0 C99 1 0.881354 0.931063 0.295393 11.00000 0.09432 0.12062 = 0.13697 0.07189 0.00816 -0.03556 AFIX 23 H99A 2 0.821010 0.930381 0.269406 11.00000 -1.20000 H99B 2 0.850804 0.930824 0.330947 11.00000 -1.20000 AFIX 0 C100 1 0.949454 0.879508 0.288600 11.00000 0.22301 0.07808 = 0.15678 0.02723 -0.04183 -0.01542 AFIX 33 H10G 2 0.903763 0.848436 0.292963 11.00000 -1.50000 H10H 2 1.007556 0.878861 0.315211 11.00000 -1.50000 H10I 2 0.979556 0.879044 0.253386 11.00000 -1.50000 AFIX 0 C101 1 1.016927 0.987678 0.244503 11.00000 0.04539 0.08564 = 0.16062 0.01085 0.01780 -0.01234 AFIX 23 H10C 2 1.073384 0.960401 0.248133 11.00000 -1.20000 H10D 2 1.051971 1.022657 0.247887 11.00000 -1.20000 AFIX 0 C102 1 0.964146 0.983263 0.187782 11.00000 0.11047 0.13825 = 0.22664 0.05609 0.08526 0.07680 AFIX 33 H10J 2 1.020041 0.983645 0.161496 11.00000 -1.50000 H10K 2 0.915785 1.013235 0.181654 11.00000 -1.50000 H10L 2 0.923736 0.950160 0.184865 11.00000 -1.50000 AFIX 0 C103 1 0.854810 1.021511 0.285989 11.00000 0.06193 0.16218 = 0.18750 -0.03482 -0.00039 0.07272 AFIX 23 H10E 2 0.807273 1.016427 0.316113 11.00000 -1.20000 H10F 2 0.811657 1.016309 0.253172 11.00000 -1.20000 AFIX 0 C104 1 0.900212 1.079428 0.287240 11.00000 0.17187 0.13466 = 0.22300 0.04525 -0.01391 -0.00967 AFIX 33 H10M 2 0.840816 1.104677 0.286856 11.00000 -1.50000 H10N 2 0.943902 1.085258 0.256328 11.00000 -1.50000 H10O 2 0.944238 1.084471 0.319316 11.00000 -1.50000 AFIX 0 CL9 4 0.725003 0.119223 0.548593 10.50000 0.09762 0.07333 = 0.17989 -0.02844 0.05093 0.02109 CL10 4 0.834343 0.159991 0.643723 10.50000 0.08694 0.17287 = 0.13450 0.05384 0.01679 -0.01336 C105 1 0.784204 0.104864 0.609853 10.50000 0.14245 0.13687 = 0.39013 0.12147 0.22318 0.08131 AFIX 23 H10P 2 0.843373 0.079540 0.604781 10.50000 -1.20000 H10Q 2 0.730676 0.087260 0.631888 10.50000 -1.20000 HKLF 4 REM XuB-5 in Pc REM R1 = 0.0867 for 19314 Fo > 4sig(Fo) and 0.1058 for all 26101 data REM 1326 parameters refined using 80 restraints END ; 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 I1 I 0.59169(5) 0.53460(3) 0.22613(3) 0.05199(19) Uani 1 1 d . . . I2 I 0.23494(6) 0.59373(3) 0.18194(3) 0.0665(2) Uani 1 1 d . . . I3 I 0.30202(6) 0.40988(3) 0.22433(3) 0.0633(2) Uani 1 1 d . . . I4 I 0.32087(6) 0.54501(3) 0.35895(3) 0.0580(2) Uani 1 1 d . . . I5 I 0.20518(6) 0.36998(4) 0.39845(4) 0.0688(2) Uani 1 1 d . . . I6 I 0.57573(6) 0.40454(3) 0.36013(3) 0.0583(2) Uani 1 1 d . . . I7 I 0.66652(8) 0.35548(4) 0.18703(4) 0.0783(3) Uani 1 1 d . . . I8 I 0.66868(6) 0.58365(3) 0.40793(3) 0.0630(2) Uani 1 1 d . . . I9 I 0.56522(6) 1.03745(3) 0.33919(3) 0.0612(2) Uani 1 1 d . . . I10 I 0.22477(7) 1.09512(3) 0.38730(3) 0.0694(3) Uani 1 1 d . . . I11 I 0.29433(6) 0.90689(3) 0.34540(3) 0.0589(2) Uani 1 1 d . . . I12 I 0.29584(6) 1.03818(3) 0.21082(3) 0.0561(2) Uani 1 1 d . . . I13 I 0.19485(8) 0.86369(4) 0.16245(4) 0.0858(3) Uani 1 1 d . . . I14 I 0.55434(7) 0.89843(3) 0.21528(4) 0.0726(3) Uani 1 1 d . . . I15 I 0.66006(7) 0.85671(4) 0.39229(4) 0.0728(3) Uani 1 1 d . . . I16 I 0.66230(8) 1.06208(4) 0.15400(4) 0.0892(3) Uani 1 1 d . . . Ag1 Ag 0.35420(8) 0.52385(4) 0.24504(4) 0.0741(3) Uani 1 1 d . . . Ag2 Ag 0.34543(8) 0.43060(5) 0.33770(4) 0.0749(3) Uani 1 1 d . . . Ag3 Ag 0.53396(9) 0.42180(4) 0.24444(4) 0.0757(3) Uani 1 1 d . . . Ag4 Ag 0.54623(8) 0.51890(4) 0.33892(4) 0.0704(3) Uani 1 1 d . . . Ag5 Ag 0.33382(8) 1.02016(4) 0.32645(4) 0.0724(3) Uani 1 1 d . . . Ag6 Ag 0.32746(9) 0.92202(5) 0.23115(5) 0.0822(4) Uani 1 1 d . . . Ag7 Ag 0.53052(9) 0.92191(5) 0.32869(5) 0.0843(4) Uani 1 1 d . . . Ag8 Ag 0.53032(9) 1.01403(5) 0.22622(5) 0.0810(4) Uani 1 1 d . . . Cl1 Cl 1.1799(4) 0.6096(2) 0.48167(19) 0.1346(18) Uani 1 1 d . . . Cl2 Cl 0.6670(4) 0.1608(2) 0.4126(3) 0.203(2) Uani 1 1 d . . . Cl3 Cl 0.7829(5) 0.3112(3) 0.5768(2) 0.197(3) Uani 1 1 d . . . Cl4 Cl -0.0517(4) 0.1736(3) 0.1627(2) 0.170(2) Uani 1 1 d . . . Cl5 Cl 0.9358(3) 0.40510(19) 0.5091(2) 0.1134(16) Uani 1 1 d . . . Cl6 Cl 0.1223(4) 1.22876(19) 0.0515(3) 0.157(3) Uani 1 1 d . . . Cl7 Cl 1.0972(5) 0.7207(3) 0.3707(3) 0.182(3) Uani 1 1 d . . . Cl8 Cl 0.9693(5) 0.8787(2) 0.5124(3) 0.150(2) Uani 1 1 d . . . N1 N 0.7545(4) 0.7225(2) 0.5206(2) 0.052(3) Uani 1 1 d D . . N2 N 1.0997(4) 0.2215(2) 0.5041(2) 0.057(3) Uani 1 1 d D . . N3 N 0.4926(4) 0.28297(18) 0.7687(2) 0.045(2) Uani 1 1 d D . . N4 N 0.4118(4) 0.22036(19) 0.2573(2) 0.061(3) Uani 1 1 d D . . N5 N 0.4551(4) 0.4699(2) 0.53922(19) 0.054(3) Uani 1 1 d D . . N6 N 0.3732(4) 1.0189(2) 0.03087(19) 0.057(3) Uani 1 1 d D . . N7 N 0.9495(4) 0.5043(2) 0.3007(2) 0.073(3) Uani 1 1 d D . . N8 N 0.9419(4) 0.9813(2) 0.2887(2) 0.094(4) Uani 1 1 d D . . C1 C 0.7876(8) 0.6671(2) 0.5352(4) 0.050(3) Uani 1 1 d D . . H1A H 0.7694 0.6436 0.5052 0.060 Uiso 1 1 calc R . . H1B H 0.7446 0.6555 0.5653 0.060 Uiso 1 1 calc R . . C2 C 0.9098(7) 0.6589(4) 0.5505(3) 0.061(3) Uani 1 1 d D . . C3 C 0.9426(9) 0.6625(5) 0.6044(6) 0.075(4) Uani 1 1 d . . . H3A H 0.8921 0.6721 0.6299 0.091 Uiso 1 1 calc R . . C4 C 1.0529(11) 0.6516(6) 0.6210(6) 0.087(5) Uani 1 1 d . . . H4A H 1.0775 0.6570 0.6562 0.104 Uiso 1 1 calc R . . C5 C 1.1195(10) 0.6331(5) 0.5827(6) 0.076(4) Uani 1 1 d . . . H5A H 1.1906 0.6233 0.5924 0.092 Uiso 1 1 calc R . . C6 C 1.0857(9) 0.6285(6) 0.5303(5) 0.072(4) Uani 1 1 d . . . C7 C 0.9838(7) 0.6397(4) 0.5138(4) 0.058(3) Uani 1 1 d D . . H7A H 0.9625 0.6348 0.4780 0.070 Uiso 1 1 calc R . . C8 C 0.8253(7) 0.7484(3) 0.4811(2) 0.061(3) Uani 1 1 d D . . H8A H 0.8997 0.7478 0.4954 0.073 Uiso 1 1 calc R . . H8B H 0.8037 0.7859 0.4775 0.073 Uiso 1 1 calc R . . C9 C 0.8242(12) 0.7229(4) 0.4246(3) 0.085(5) Uani 1 1 d D . . H9A H 0.8959 0.7252 0.4101 0.127 Uiso 1 1 calc R . . H9B H 0.7734 0.7420 0.4016 0.127 Uiso 1 1 calc R . . H9C H 0.8028 0.6857 0.4270 0.127 Uiso 1 1 calc R . . C10 C 0.7604(9) 0.7542(3) 0.5705(3) 0.074(4) Uani 1 1 d D . . H10A H 0.8364 0.7578 0.5818 0.089 Uiso 1 1 calc R . . H10B H 0.7237 0.7344 0.5983 0.089 Uiso 1 1 calc R . . C11 C 0.7098(11) 0.8112(3) 0.5664(6) 0.114(6) Uani 1 1 d D . . H11A H 0.7140 0.8283 0.6010 0.170 Uiso 1 1 calc R . . H11B H 0.6349 0.8083 0.5547 0.170 Uiso 1 1 calc R . . H11C H 0.7492 0.8323 0.5411 0.170 Uiso 1 1 calc R . . C12 C 0.6426(4) 0.7207(4) 0.4979(3) 0.062(4) Uani 1 1 d D . . H12A H 0.6395 0.6943 0.4692 0.074 Uiso 1 1 calc R . . H12B H 0.6251 0.7556 0.4823 0.074 Uiso 1 1 calc R . . C13 C 0.5557(8) 0.7064(7) 0.5393(5) 0.128(7) Uani 1 1 d D . . H13A H 0.4869 0.7217 0.5280 0.193 Uiso 1 1 calc R . . H13B H 0.5772 0.7208 0.5738 0.193 Uiso 1 1 calc R . . H13C H 0.5490 0.6679 0.5417 0.193 Uiso 1 1 calc R . . C14 C 1.0666(11) 0.2247(5) 0.4465(3) 0.079(4) Uani 1 1 d D . . H14A H 1.0843 0.1905 0.4297 0.095 Uiso 1 1 calc R . . H14B H 1.1106 0.2522 0.4298 0.095 Uiso 1 1 calc R . . C15 C 0.9483(10) 0.2370(5) 0.4335(5) 0.070(4) Uani 1 1 d . . . C16 C 0.9163(9) 0.2899(5) 0.4244(5) 0.065(4) Uani 1 1 d . . . H16A H 0.9695 0.3167 0.4260 0.078 Uiso 1 1 calc R . . C17 C 0.8132(11) 0.3046(5) 0.4134(5) 0.074(4) Uani 1 1 d . . . H17A H 0.7959 0.3408 0.4080 0.089 Uiso 1 1 calc R . . C18 C 0.7319(12) 0.2654(6) 0.4100(6) 0.090(5) Uani 1 1 d . . . H18A H 0.6597 0.2746 0.4022 0.108 Uiso 1 1 calc R . . C19 C 0.7646(12) 0.2089(5) 0.4193(6) 0.086(5) Uani 1 1 d . . . C20 C 0.8762(10) 0.1978(6) 0.4279(6) 0.089(4) Uani 1 1 d . . . H20A H 0.8996 0.1621 0.4297 0.107 Uiso 1 1 calc R . . C21 C 1.0859(9) 0.2763(3) 0.5262(3) 0.073(4) Uani 1 1 d D . . H21A H 1.0086 0.2844 0.5261 0.088 Uiso 1 1 calc R . . H21B H 1.1198 0.3017 0.5021 0.088 Uiso 1 1 calc R . . C22 C 1.1326(13) 0.2861(5) 0.5830(3) 0.108(6) Uani 1 1 d D . . H22A H 1.1017 0.3185 0.5973 0.162 Uiso 1 1 calc R . . H22B H 1.2104 0.2899 0.5818 0.162 Uiso 1 1 calc R . . H22C H 1.1150 0.2561 0.6056 0.162 Uiso 1 1 calc R . . C23 C 1.0281(7) 0.1848(2) 0.5334(4) 0.063(4) Uani 1 1 d D . . H23A H 0.9535 0.1964 0.5266 0.076 Uiso 1 1 calc R . . H23B H 1.0436 0.1897 0.5715 0.076 Uiso 1 1 calc R . . C24 C 1.0339(11) 0.1237(3) 0.5213(6) 0.077(4) Uani 1 1 d D . . H24A H 1.0220 0.1037 0.5537 0.115 Uiso 1 1 calc R . . H24B H 1.1045 0.1151 0.5080 0.115 Uiso 1 1 calc R . . H24C H 0.9788 0.1145 0.4948 0.115 Uiso 1 1 calc R . . C25 C 1.2142(4) 0.2035(3) 0.5076(4) 0.058(3) Uani 1 1 d D . . H25A H 1.2181 0.1691 0.4892 0.069 Uiso 1 1 calc R . . H25B H 1.2316 0.1966 0.5453 0.069 Uiso 1 1 calc R . . C26 C 1.3052(7) 0.2393(4) 0.4860(6) 0.108(5) Uani 1 1 d D . . H26A H 1.3701 0.2181 0.4821 0.161 Uiso 1 1 calc R . . H26B H 1.3198 0.2683 0.5108 0.161 Uiso 1 1 calc R . . H26C H 1.2827 0.2538 0.4517 0.161 Uiso 1 1 calc R . . C27 C 0.4854(8) 0.3150(3) 0.7192(3) 0.044(2) Uani 1 1 d DU . . H27A H 0.5276 0.3477 0.7251 0.053 Uiso 1 1 calc R . . H27B H 0.4100 0.3258 0.7136 0.053 Uiso 1 1 calc R . . C28 C 0.5221(9) 0.2899(4) 0.6690(5) 0.059(3) Uani 1 1 d . . . C29 C 0.4691(9) 0.2487(4) 0.6419(3) 0.075(4) Uani 1 1 d D . . H29A H 0.4047 0.2352 0.6557 0.090 Uiso 1 1 calc R . . C30 C 0.5080(14) 0.2267(6) 0.5949(4) 0.136(8) Uani 1 1 d D . . H30A H 0.4690 0.1999 0.5766 0.163 Uiso 1 1 calc R . . C31 C 0.6100(9) 0.2461(4) 0.5753(5) 0.099(4) Uani 1 1 d DU . . H31A H 0.6368 0.2323 0.5435 0.119 Uiso 1 1 calc R . . C32 C 0.6692(10) 0.2855(4) 0.6036(5) 0.082(4) Uani 1 1 d D . . C33 C 0.6212(10) 0.3083(5) 0.6482(5) 0.075(4) Uani 1 1 d . . . H33A H 0.6564 0.3371 0.6652 0.090 Uiso 1 1 calc R . . C34 C 0.4163(5) 0.2372(3) 0.7684(5) 0.068(4) Uani 1 1 d D . . H34A H 0.4281 0.2169 0.8014 0.082 Uiso 1 1 calc R . . H34B H 0.4339 0.2136 0.7388 0.082 Uiso 1 1 calc R . . C35 C 0.2943(6) 0.2520(6) 0.7633(6) 0.095(5) Uani 1 1 d D . . H35A H 0.2534 0.2209 0.7515 0.143 Uiso 1 1 calc R . . H35B H 0.2846 0.2806 0.7376 0.143 Uiso 1 1 calc R . . H35C H 0.2690 0.2637 0.7976 0.143 Uiso 1 1 calc R . . C36 C 0.6019(4) 0.2596(3) 0.7779(5) 0.068(3) Uani 1 1 d D . . H36A H 0.6189 0.2371 0.7474 0.081 Uiso 1 1 calc R . . H36B H 0.6000 0.2364 0.8093 0.081 Uiso 1 1 calc R . . C37 C 0.6945(7) 0.3010(4) 0.7865(5) 0.093(5) Uani 1 1 d D . . H37A H 0.7598 0.2826 0.7982 0.139 Uiso 1 1 calc R . . H37B H 0.6741 0.3267 0.8132 0.139 Uiso 1 1 calc R . . H37C H 0.7072 0.3193 0.7533 0.139 Uiso 1 1 calc R . . C38 C 0.4687(11) 0.3220(3) 0.8116(2) 0.075(4) Uani 1 1 d D . . H38A H 0.3993 0.3391 0.8028 0.090 Uiso 1 1 calc R . . H38B H 0.5241 0.3500 0.8114 0.090 Uiso 1 1 calc R . . C39 C 0.4635(13) 0.2991(5) 0.8689(3) 0.105(5) Uani 1 1 d D . . H39A H 0.4747 0.3277 0.8944 0.158 Uiso 1 1 calc R . . H39B H 0.5193 0.2723 0.8740 0.158 Uiso 1 1 calc R . . H39C H 0.3933 0.2830 0.8739 0.158 Uiso 1 1 calc R . . C40 C 0.3183(6) 0.1859(4) 0.2695(5) 0.062(3) Uani 1 1 d D . . H40A H 0.3250 0.1759 0.3071 0.074 Uiso 1 1 calc R . . H40B H 0.3250 0.1530 0.2487 0.074 Uiso 1 1 calc R . . C41 C 0.1995(9) 0.2084(3) 0.2592(4) 0.075(4) Uani 1 1 d D . . C42 C 0.1347(14) 0.1891(5) 0.2180(6) 0.102(6) Uani 1 1 d . . . H42A H 0.1612 0.1633 0.1945 0.123 Uiso 1 1 calc R . . C43 C 0.0293(13) 0.2083(7) 0.2117(8) 0.121(6) Uani 1 1 d . . . C44 C -0.0090(13) 0.2482(8) 0.2444(8) 0.113(6) Uani 1 1 d . . . H44A H -0.0799 0.2611 0.2401 0.136 Uiso 1 1 calc R . . C45 C 0.0587(14) 0.2680(7) 0.2829(7) 0.104(6) Uani 1 1 d . . . H45A H 0.0340 0.2958 0.3045 0.125 Uiso 1 1 calc R . . C46 C 0.1610(9) 0.2493(4) 0.2917(5) 0.085(4) Uani 1 1 d D . . H46A H 0.2051 0.2636 0.3191 0.102 Uiso 1 1 calc R . . C47 C 0.4251(11) 0.2673(3) 0.2934(2) 0.076(4) Uani 1 1 d D . . H47A H 0.3652 0.2921 0.2868 0.092 Uiso 1 1 calc R . . H47B H 0.4922 0.2859 0.2851 0.092 Uiso 1 1 calc R . . C48 C 0.4283(14) 0.2513(5) 0.3532(3) 0.099(5) Uani 1 1 d D . . H48A H 0.4536 0.2814 0.3744 0.148 Uiso 1 1 calc R . . H48B H 0.4769 0.2213 0.3586 0.148 Uiso 1 1 calc R . . H48C H 0.3564 0.2413 0.3638 0.148 Uiso 1 1 calc R . . C49 C 0.5008(5) 0.1811(3) 0.2630(6) 0.091(5) Uani 1 1 d D . . H49A H 0.4886 0.1526 0.2368 0.109 Uiso 1 1 calc R . . H49B H 0.4977 0.1648 0.2984 0.109 Uiso 1 1 calc R . . C50 C 0.6164(6) 0.2042(6) 0.2558(8) 0.126(8) Uani 1 1 d D . . H50A H 0.6696 0.1771 0.2650 0.189 Uiso 1 1 calc R . . H50B H 0.6268 0.2350 0.2788 0.189 Uiso 1 1 calc R . . H50C H 0.6246 0.2150 0.2191 0.189 Uiso 1 1 calc R . . C51 C 0.4106(11) 0.2416(4) 0.2022(2) 0.102(6) Uani 1 1 d D . . H51A H 0.4763 0.2629 0.1985 0.122 Uiso 1 1 calc R . . H51B H 0.3495 0.2663 0.1988 0.122 Uiso 1 1 calc R . . C52 C 0.4032(18) 0.2029(5) 0.1539(4) 0.160(9) Uani 1 1 d D . . H52A H 0.3744 0.2219 0.1231 0.239 Uiso 1 1 calc R . . H52B H 0.3561 0.1733 0.1621 0.239 Uiso 1 1 calc R . . H52C H 0.4746 0.1895 0.1464 0.239 Uiso 1 1 calc R . . C53 C 0.5455(5) 0.4898(4) 0.5070(3) 0.045(3) Uani 1 1 d D . . H53A H 0.5320 0.5275 0.4987 0.054 Uiso 1 1 calc R . . H53B H 0.5447 0.4702 0.4733 0.054 Uiso 1 1 calc R . . C54 C 0.6592(9) 0.4852(5) 0.5326(5) 0.062(4) Uani 1 1 d . . . C55 C 0.7389(10) 0.4501(5) 0.5135(5) 0.068(4) Uani 1 1 d . . . H55A H 0.7180 0.4257 0.4867 0.082 Uiso 1 1 calc R . . C56 C 0.8442(9) 0.4493(5) 0.5313(5) 0.064(4) Uani 1 1 d . . . C57 C 0.8773(11) 0.4886(6) 0.5649(6) 0.089(5) Uani 1 1 d . . . H57A H 0.9512 0.4919 0.5737 0.107 Uiso 1 1 calc R . . C58 C 0.8025(9) 0.5249(5) 0.5872(6) 0.077(4) Uani 1 1 d . . . H58A H 0.8252 0.5490 0.6139 0.092 Uiso 1 1 calc R . . C59 C 0.6931(10) 0.5245(4) 0.5686(5) 0.070(4) Uani 1 1 d . . . H59A H 0.6443 0.5504 0.5805 0.084 Uiso 1 1 calc R . . C60 C 0.4712(10) 0.4151(2) 0.5607(3) 0.073(4) Uani 1 1 d D . . H60A H 0.4111 0.4064 0.5837 0.087 Uiso 1 1 calc R . . H60B H 0.5377 0.4145 0.5827 0.087 Uiso 1 1 calc R . . C61 C 0.4788(12) 0.3716(4) 0.5173(4) 0.102(6) Uani 1 1 d D . . H61A H 0.4701 0.3366 0.5333 0.153 Uiso 1 1 calc R . . H61B H 0.5487 0.3736 0.5010 0.153 Uiso 1 1 calc R . . H61C H 0.4224 0.3772 0.4904 0.153 Uiso 1 1 calc R . . C62 C 0.4385(9) 0.5051(2) 0.5857(3) 0.067(4) Uani 1 1 d D . . H62A H 0.5014 0.5012 0.6099 0.080 Uiso 1 1 calc R . . H62B H 0.3759 0.4916 0.6046 0.080 Uiso 1 1 calc R . . C63 C 0.4206(12) 0.5658(3) 0.5758(6) 0.095(5) Uani 1 1 d D . . H63A H 0.4223 0.5846 0.6095 0.142 Uiso 1 1 calc R . . H63B H 0.3510 0.5712 0.5580 0.142 Uiso 1 1 calc R . . H63C H 0.4772 0.5794 0.5536 0.142 Uiso 1 1 calc R . . C64 C 0.3558(4) 0.4738(5) 0.5047(3) 0.069(4) Uani 1 1 d D . . H64A H 0.3646 0.4502 0.4739 0.082 Uiso 1 1 calc R . . H64B H 0.3500 0.5104 0.4912 0.082 Uiso 1 1 calc R . . C65 C 0.2478(7) 0.4590(6) 0.5315(5) 0.100(6) Uani 1 1 d D . . H65A H 0.1885 0.4625 0.5058 0.150 Uiso 1 1 calc R . . H65B H 0.2362 0.4830 0.5612 0.150 Uiso 1 1 calc R . . H65C H 0.2515 0.4225 0.5444 0.150 Uiso 1 1 calc R . . C66 C 0.3879(9) 1.0701(3) 0.0609(4) 0.054(3) Uani 1 1 d D . . H66A H 0.4640 1.0729 0.0722 0.065 Uiso 1 1 calc R . . H66B H 0.3455 1.0680 0.0932 0.065 Uiso 1 1 calc R . . C67 C 0.3570(8) 1.1207(4) 0.0321(4) 0.049(3) Uani 1 1 d . . . C68 C 0.2642(9) 1.1471(5) 0.0506(5) 0.065(4) Uani 1 1 d . . . H68A H 0.2240 1.1319 0.0780 0.079 Uiso 1 1 calc R . . C69 C 0.2333(12) 1.1949(5) 0.0285(7) 0.104(6) Uani 1 1 d . . . C70 C 0.2903(15) 1.2126(5) -0.0145(7) 0.116(6) Uani 1 1 d . . . H70A H 0.2606 1.2407 -0.0349 0.140 Uiso 1 1 calc R . . C71 C 0.3906(15) 1.1912(7) -0.0301(7) 0.133(7) Uani 1 1 d . . . H71A H 0.4349 1.2082 -0.0548 0.160 Uiso 1 1 calc R . . C72 C 0.4165(11) 1.1454(5) -0.0071(5) 0.070(4) Uani 1 1 d . . . H72A H 0.4797 1.1282 -0.0180 0.085 Uiso 1 1 calc R . . C73 C 0.2606(4) 1.0124(4) 0.0098(3) 0.061(3) Uani 1 1 d D . . H73A H 0.2565 0.9798 -0.0117 0.074 Uiso 1 1 calc R . . H73B H 0.2431 1.0426 -0.0137 0.074 Uiso 1 1 calc R . . C74 C 0.1747(7) 1.0092(5) 0.0536(4) 0.075(4) Uani 1 1 d D . . H74A H 0.1035 1.0054 0.0370 0.113 Uiso 1 1 calc R . . H74B H 0.1772 1.0416 0.0748 0.113 Uiso 1 1 calc R . . H74C H 0.1897 0.9786 0.0763 0.113 Uiso 1 1 calc R . . C75 C 0.4034(9) 0.9748(2) 0.0680(3) 0.061(3) Uani 1 1 d D . . H75A H 0.3569 0.9775 0.0988 0.073 Uiso 1 1 calc R . . H75B H 0.4775 0.9814 0.0809 0.073 Uiso 1 1 calc R . . C76 C 0.3978(13) 0.9159(3) 0.0478(5) 0.084(5) Uani 1 1 d D . . H76A H 0.3824 0.8923 0.0773 0.126 Uiso 1 1 calc R . . H76B H 0.4664 0.9061 0.0329 0.126 Uiso 1 1 calc R . . H76C H 0.3411 0.9126 0.0207 0.126 Uiso 1 1 calc R . . C77 C 0.4393(5) 1.0180(4) -0.0183(3) 0.058(3) Uani 1 1 d D . . H77A H 0.4175 1.0485 -0.0404 0.069 Uiso 1 1 calc R . . H77B H 0.4207 0.9855 -0.0383 0.069 Uiso 1 1 calc R . . C78 C 0.5643(6) 1.0197(5) -0.0102(5) 0.084(4) Uani 1 1 d D . . H78A H 0.5979 1.0190 -0.0446 0.125 Uiso 1 1 calc R . . H78B H 0.5880 0.9890 0.0105 0.125 Uiso 1 1 calc R . . H78C H 0.5848 1.0522 0.0084 0.125 Uiso 1 1 calc R . . C79 C 0.8819(7) 0.5528(3) 0.2978(6) 0.091(5) Uani 1 1 d D . . H79A H 0.8417 0.5551 0.3308 0.109 Uiso 1 1 calc R . . H79B H 0.8288 0.5480 0.2686 0.109 Uiso 1 1 calc R . . C80 C 0.9404(11) 0.6089(5) 0.2892(3) 0.091(4) Uani 1 1 d D . . C81 C 0.9859(8) 0.6362(3) 0.3330(6) 0.094(6) Uani 1 1 d D . . H81A H 0.9817 0.6239 0.3682 0.113 Uiso 1 1 calc R . . C82 C 1.0382(10) 0.6837(4) 0.3194(7) 0.108(6) Uani 1 1 d D . . C83 C 1.0250(13) 0.7087(8) 0.2693(10) 0.142(9) Uani 1 1 d . . . H83A H 1.0496 0.7439 0.2650 0.171 Uiso 1 1 calc R . . C84 C 0.9769(12) 0.6828(3) 0.2267(8) 0.129(8) Uani 1 1 d D . . H84A H 0.9730 0.6978 0.1925 0.155 Uiso 1 1 calc R . . C85 C 0.9340(11) 0.6321(4) 0.2382(4) 0.121(7) Uani 1 1 d D . . H85A H 0.8993 0.6129 0.2106 0.146 Uiso 1 1 calc R . . C86 C 1.0202(7) 0.5055(7) 0.3494(2) 0.119(6) Uani 1 1 d D . . H86A H 1.0658 0.5374 0.3474 0.143 Uiso 1 1 calc R . . H86B H 1.0681 0.4744 0.3482 0.143 Uiso 1 1 calc R . . C87 C 0.9659(10) 0.5057(8) 0.4044(3) 0.144(8) Uani 1 1 d D . . H87A H 1.0209 0.5095 0.4323 0.217 Uiso 1 1 calc R . . H87B H 0.9274 0.4724 0.4092 0.217 Uiso 1 1 calc R . . H87C H 0.9157 0.5353 0.4060 0.217 Uiso 1 1 calc R . . C88 C 0.8659(6) 0.4630(2) 0.3071(7) 0.115(6) Uani 1 1 d D . . H88A H 0.8100 0.4675 0.2792 0.138 Uiso 1 1 calc R . . H88B H 0.8319 0.4679 0.3415 0.138 Uiso 1 1 calc R . . C89 C 0.9123(12) 0.4055(3) 0.3042(9) 0.176(9) Uani 1 1 d D . . H89A H 0.9086 0.3886 0.3388 0.264 Uiso 1 1 calc R . . H89B H 0.9869 0.4070 0.2935 0.264 Uiso 1 1 calc R . . H89C H 0.8703 0.3848 0.2783 0.264 Uiso 1 1 calc R . . C90 C 1.0277(6) 0.4965(6) 0.2576(2) 0.090(5) Uani 1 1 d D . . H90A H 1.0716 0.4647 0.2654 0.108 Uiso 1 1 calc R . . H90B H 1.0763 0.5273 0.2566 0.108 Uiso 1 1 calc R . . C91 C 0.9705(10) 0.4897(7) 0.2021(3) 0.110(6) Uani 1 1 d D . . H91A H 0.9997 0.4587 0.1843 0.166 Uiso 1 1 calc R . . H91B H 0.9824 0.5213 0.1808 0.166 Uiso 1 1 calc R . . H91C H 0.8936 0.4848 0.2067 0.166 Uiso 1 1 calc R . . C92 C 1.0078(8) 0.9872(5) 0.3382(4) 0.137(9) Uani 1 1 d D . . H92A H 1.0637 0.9595 0.3378 0.164 Uiso 1 1 calc R . . H92B H 1.0448 1.0217 0.3364 0.164 Uiso 1 1 calc R . . C93 C 0.9562(9) 0.9843(7) 0.3904(7) 0.091(5) Uani 1 1 d . . . C94 C 0.9803(11) 0.9371(6) 0.4269(7) 0.090(5) Uani 1 1 d . . . H94A H 1.0285 0.9102 0.4167 0.108 Uiso 1 1 calc R . . C95 C 0.9312(13) 0.9342(7) 0.4743(7) 0.121(5) Uani 1 1 d . . . C96 C 0.8605(13) 0.9674(9) 0.5007(9) 0.145(9) Uani 1 1 d . . . H96A H 0.8308 0.9617 0.5342 0.174 Uiso 1 1 calc R . . C97 C 0.8421(10) 1.0122(7) 0.4659(3) 0.117(6) Uani 1 1 d D . . H97A H 0.7950 1.0387 0.4780 0.140 Uiso 1 1 calc R . . C98 C 0.8867(10) 1.0210(8) 0.4157(4) 0.132(8) Uani 1 1 d D . . H98A H 0.8696 1.0530 0.3979 0.159 Uiso 1 1 calc R . . C99 C 0.8814(7) 0.9311(2) 0.2954(6) 0.117(6) Uani 1 1 d D . . H99A H 0.8210 0.9304 0.2694 0.141 Uiso 1 1 calc R . . H99B H 0.8508 0.9308 0.3309 0.141 Uiso 1 1 calc R . . C100 C 0.9495(11) 0.8795(4) 0.2886(9) 0.153(9) Uani 1 1 d D . . H10G H 0.9038 0.8484 0.2930 0.230 Uiso 1 1 calc R . . H10H H 1.0076 0.8789 0.3152 0.230 Uiso 1 1 calc R . . H10I H 0.9796 0.8790 0.2534 0.230 Uiso 1 1 calc R . . C101 C 1.0169(6) 0.9877(6) 0.2445(2) 0.097(6) Uani 1 1 d D . . H10C H 1.0734 0.9604 0.2481 0.116 Uiso 1 1 calc R . . H10D H 1.0520 1.0227 0.2479 0.116 Uiso 1 1 calc R . . C102 C 0.9641(10) 0.9833(8) 0.1878(3) 0.157(8) Uani 1 1 d D . . H10J H 1.0200 0.9836 0.1615 0.236 Uiso 1 1 calc R . . H10K H 0.9158 1.0132 0.1817 0.236 Uiso 1 1 calc R . . H10L H 0.9237 0.9502 0.1849 0.236 Uiso 1 1 calc R . . C103 C 0.8548(6) 1.0215(2) 0.2860(8) 0.137(8) Uani 1 1 d D . . H10E H 0.8073 1.0164 0.3161 0.165 Uiso 1 1 calc R . . H10F H 0.8117 1.0163 0.2532 0.165 Uiso 1 1 calc R . . C104 C 0.9002(14) 1.0794(4) 0.2872(10) 0.177(12) Uani 1 1 d D . . H10M H 0.8408 1.1047 0.2869 0.265 Uiso 1 1 calc R . . H10N H 0.9439 1.0853 0.2563 0.265 Uiso 1 1 calc R . . H10O H 0.9442 1.0845 0.3193 0.265 Uiso 1 1 calc R . . Cl9 Cl 0.7250(6) 0.1192(3) 0.5486(3) 0.116(3) Uani 0.50 1 d PD . . Cl10 Cl 0.8343(7) 0.1600(3) 0.6437(3) 0.131(4) Uani 0.50 1 d PD . . C105 C 0.7842(12) 0.1049(4) 0.6099(4) 0.219(14) Uani 0.50 1 d PD . . H10P H 0.8434 0.0795 0.6048 0.263 Uiso 0.50 1 calc PR . . H10Q H 0.7307 0.0873 0.6319 0.263 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 I1 0.0516(3) 0.0432(4) 0.0609(4) -0.0008(3) -0.0026(3) 0.0000(3) I2 0.0640(4) 0.0623(5) 0.0731(5) 0.0097(4) 0.0018(4) 0.0069(4) I3 0.0667(4) 0.0542(5) 0.0685(5) -0.0032(4) -0.0053(4) -0.0026(4) I4 0.0539(4) 0.0585(4) 0.0620(4) 0.0010(4) 0.0092(3) 0.0015(4) I5 0.0674(4) 0.0599(5) 0.0790(5) 0.0120(4) 0.0008(4) -0.0106(4) I6 0.0582(4) 0.0502(4) 0.0663(5) 0.0025(4) -0.0024(3) 0.0064(4) I7 0.0910(6) 0.0592(5) 0.0858(6) -0.0096(4) 0.0230(4) 0.0019(5) I8 0.0747(5) 0.0584(5) 0.0558(4) -0.0062(4) -0.0010(3) -0.0123(4) I9 0.0606(4) 0.0530(5) 0.0699(5) -0.0008(4) -0.0002(3) -0.0038(4) I10 0.0938(5) 0.0554(5) 0.0598(5) -0.0016(4) 0.0159(4) 0.0116(4) I11 0.0568(4) 0.0586(5) 0.0613(5) 0.0017(4) 0.0016(3) 0.0019(4) I12 0.0704(4) 0.0476(4) 0.0503(4) -0.0026(3) 0.0021(3) 0.0020(4) I13 0.1136(7) 0.0727(6) 0.0699(6) -0.0136(5) -0.0196(5) -0.0019(6) I14 0.0845(5) 0.0502(5) 0.0835(6) -0.0019(4) 0.0133(4) -0.0005(4) I15 0.0813(5) 0.0589(5) 0.0784(6) 0.0073(4) 0.0039(4) 0.0101(4) I16 0.0834(5) 0.0961(7) 0.0874(6) 0.0347(5) -0.0107(4) -0.0233(5) Ag1 0.0758(6) 0.0688(6) 0.0776(7) 0.0085(5) -0.0025(5) 0.0073(5) Ag2 0.0736(6) 0.0683(6) 0.0829(7) 0.0062(5) 0.0051(5) -0.0068(5) Ag3 0.0848(6) 0.0611(6) 0.0814(7) -0.0064(5) 0.0043(5) 0.0015(6) Ag4 0.0702(5) 0.0662(6) 0.0745(6) -0.0093(5) -0.0021(4) -0.0043(5) Ag5 0.0721(6) 0.0730(7) 0.0723(6) -0.0067(5) 0.0062(5) 0.0037(5) Ag6 0.0996(7) 0.0660(7) 0.0803(7) -0.0098(6) -0.0094(6) 0.0011(6) Ag7 0.0873(7) 0.0709(7) 0.0944(8) 0.0050(6) -0.0002(6) 0.0084(6) Ag8 0.0920(7) 0.0703(7) 0.0810(7) 0.0055(6) 0.0058(5) -0.0053(6) Cl1 0.116(3) 0.187(5) 0.101(3) 0.007(3) 0.014(2) 0.081(3) Cl2 0.195(4) 0.090(3) 0.316(6) 0.064(4) -0.162(4) -0.067(3) Cl3 0.191(5) 0.243(7) 0.161(4) 0.061(5) 0.106(4) 0.058(5) Cl4 0.156(3) 0.178(6) 0.170(4) 0.036(4) -0.088(3) -0.048(4) Cl5 0.086(2) 0.105(3) 0.150(4) -0.033(3) 0.021(2) 0.023(2) Cl6 0.113(3) 0.084(3) 0.276(7) -0.020(4) 0.018(4) 0.043(3) Cl7 0.121(4) 0.211(6) 0.215(7) -0.067(5) 0.035(4) -0.056(4) Cl8 0.153(4) 0.117(4) 0.178(5) 0.052(4) -0.038(4) -0.038(3) N1 0.057(5) 0.048(5) 0.051(5) 0.002(4) 0.006(4) -0.001(4) N2 0.077(6) 0.045(5) 0.050(5) 0.014(4) -0.005(4) -0.005(5) N3 0.059(5) 0.019(4) 0.056(5) 0.000(4) -0.005(4) 0.006(4) N4 0.071(6) 0.037(5) 0.073(6) 0.014(4) -0.011(5) -0.014(5) N5 0.060(5) 0.066(6) 0.036(5) 0.011(4) -0.004(4) -0.004(5) N6 0.086(6) 0.043(5) 0.044(5) 0.008(4) -0.003(4) 0.012(5) N7 0.029(4) 0.117(9) 0.074(6) 0.021(6) -0.002(4) -0.012(6) N8 0.028(4) 0.091(8) 0.162(11) 0.037(8) -0.015(5) -0.014(6) C1 0.073(6) 0.027(5) 0.050(6) -0.008(4) 0.000(5) -0.014(5) C2 0.098(8) 0.052(7) 0.034(6) 0.001(5) -0.008(5) 0.007(6) C3 0.053(6) 0.067(9) 0.106(10) 0.006(8) -0.021(6) 0.006(6) C4 0.085(9) 0.091(11) 0.083(10) -0.009(8) -0.008(7) 0.006(9) C5 0.066(7) 0.062(7) 0.102(10) 0.012(7) 0.017(6) 0.039(6) C6 0.057(6) 0.082(9) 0.078(8) 0.000(7) -0.002(6) 0.031(7) C7 0.074(7) 0.051(7) 0.051(6) -0.003(5) 0.012(5) 0.005(6) C8 0.077(7) 0.037(6) 0.068(7) -0.001(5) -0.007(6) -0.016(6) C9 0.115(11) 0.057(8) 0.082(10) -0.012(7) -0.003(8) 0.018(8) C10 0.102(9) 0.055(7) 0.065(8) -0.016(6) 0.007(7) 0.003(7) C11 0.182(16) 0.046(7) 0.111(11) -0.060(7) -0.016(10) 0.024(9) C12 0.045(6) 0.040(6) 0.100(9) -0.007(6) 0.007(6) 0.006(5) C13 0.064(9) 0.189(18) 0.134(14) 0.029(14) 0.026(9) -0.018(11) C14 0.151(12) 0.062(8) 0.024(6) 0.012(5) 0.003(6) 0.035(8) C15 0.090(7) 0.060(7) 0.060(7) 0.007(6) -0.029(6) 0.042(6) C16 0.064(6) 0.052(7) 0.077(8) 0.003(6) -0.026(5) -0.001(6) C17 0.090(9) 0.029(6) 0.102(10) 0.005(6) -0.013(7) -0.016(6) C18 0.085(8) 0.064(9) 0.120(11) 0.011(8) -0.036(8) 0.005(8) C19 0.100(10) 0.025(6) 0.133(12) 0.029(7) -0.011(8) -0.007(7) C20 0.080(7) 0.051(8) 0.132(10) -0.016(7) -0.066(7) 0.008(7) C21 0.091(9) 0.056(8) 0.072(8) -0.003(6) -0.008(7) 0.015(7) C22 0.202(17) 0.051(8) 0.070(9) -0.027(7) -0.028(10) 0.022(10) C23 0.054(6) 0.076(8) 0.060(7) -0.011(6) 0.014(5) 0.012(6) C24 0.084(8) 0.038(7) 0.108(11) 0.002(7) -0.003(7) 0.012(7) C25 0.075(7) 0.035(6) 0.063(7) 0.015(5) 0.006(5) -0.008(5) C26 0.078(8) 0.091(8) 0.154(12) 0.086(8) 0.009(8) 0.026(8) C27 0.049(4) 0.023(4) 0.061(5) 0.001(4) 0.005(4) -0.004(4) C28 0.065(7) 0.027(5) 0.084(8) -0.014(5) -0.006(6) -0.007(5) C29 0.092(9) 0.043(7) 0.090(9) 0.010(6) -0.012(7) -0.021(7) C30 0.23(2) 0.059(10) 0.111(13) -0.027(9) -0.053(14) 0.010(12) C31 0.113(7) 0.083(6) 0.100(7) 0.012(5) 0.003(5) 0.023(5) C32 0.119(10) 0.037(6) 0.093(9) -0.016(6) 0.038(8) -0.006(7) C33 0.076(8) 0.051(7) 0.098(10) 0.011(7) -0.005(7) 0.022(7) C34 0.101(9) 0.048(7) 0.056(7) -0.006(6) 0.012(6) -0.020(7) C35 0.094(9) 0.079(9) 0.115(11) -0.044(8) 0.029(8) -0.028(8) C36 0.071(7) 0.054(6) 0.079(7) 0.043(5) 0.028(5) 0.013(6) C37 0.064(7) 0.141(13) 0.074(9) 0.011(9) 0.012(6) -0.032(9) C38 0.107(9) 0.075(9) 0.044(6) 0.005(6) 0.031(6) 0.013(8) C39 0.160(13) 0.065(9) 0.094(10) -0.021(8) 0.063(9) -0.034(9) C40 0.079(7) 0.038(6) 0.067(7) -0.001(5) 0.002(6) -0.027(6) C41 0.082(8) 0.070(8) 0.073(8) 0.016(7) 0.010(6) -0.007(7) C42 0.182(14) 0.040(7) 0.081(9) -0.002(7) -0.053(9) -0.013(9) C43 0.121(10) 0.088(11) 0.151(14) 0.008(11) -0.070(9) 0.038(10) C44 0.071(9) 0.134(15) 0.135(14) 0.032(13) 0.014(9) 0.010(11) C45 0.108(12) 0.100(13) 0.106(12) -0.006(10) 0.018(9) 0.017(10) C46 0.066(7) 0.063(8) 0.125(11) -0.046(7) -0.019(7) 0.023(7) C47 0.084(8) 0.036(7) 0.109(10) -0.009(7) -0.018(7) -0.019(6) C48 0.160(13) 0.056(8) 0.079(9) -0.025(7) -0.038(9) 0.021(9) C49 0.144(13) 0.048(8) 0.080(10) 0.005(7) 0.016(9) 0.024(8) C50 0.076(10) 0.109(13) 0.193(19) 0.046(13) 0.019(11) 0.014(10) C51 0.058(7) 0.143(14) 0.104(11) 0.042(10) 0.018(7) -0.004(9) C52 0.21(2) 0.188(19) 0.077(12) -0.003(13) 0.017(12) -0.092(16) C53 0.037(5) 0.033(5) 0.065(6) -0.005(5) 0.008(4) -0.003(4) C54 0.056(6) 0.051(7) 0.080(8) -0.005(6) 0.011(5) 0.016(6) C55 0.083(8) 0.041(6) 0.082(9) -0.003(6) 0.015(6) 0.000(6) C56 0.064(7) 0.051(7) 0.079(8) 0.005(6) 0.024(6) 0.010(6) C57 0.068(8) 0.081(10) 0.119(12) -0.011(9) -0.011(8) 0.006(8) C58 0.040(6) 0.057(8) 0.134(12) -0.022(8) -0.003(6) -0.011(6) C59 0.079(8) 0.035(6) 0.095(9) -0.023(6) 0.014(7) -0.004(6) C60 0.073(7) 0.079(8) 0.066(7) 0.044(6) 0.002(6) 0.003(7) C61 0.106(11) 0.043(7) 0.156(15) 0.040(8) -0.007(10) 0.011(8) C62 0.065(6) 0.073(8) 0.062(7) 0.018(6) -0.010(5) -0.022(6) C63 0.121(10) 0.081(9) 0.084(10) 0.004(8) 0.010(8) 0.057(8) C64 0.047(6) 0.082(9) 0.076(8) 0.003(7) -0.011(5) 0.006(6) C65 0.093(10) 0.116(13) 0.089(11) 0.001(10) 0.001(8) 0.017(10) C66 0.066(6) 0.048(6) 0.048(6) -0.023(5) -0.002(5) -0.010(6) C67 0.046(5) 0.050(6) 0.051(6) -0.003(5) 0.000(4) -0.001(5) C68 0.049(6) 0.056(7) 0.092(9) -0.009(6) 0.001(6) 0.020(6) C69 0.099(9) 0.047(7) 0.166(15) -0.007(8) -0.024(9) 0.054(7) C70 0.156(13) 0.061(8) 0.128(11) 0.064(7) -0.064(10) -0.033(9) C71 0.122(13) 0.137(12) 0.141(13) 0.099(10) 0.015(10) 0.034(11) C72 0.095(9) 0.036(6) 0.081(9) 0.012(6) 0.008(7) -0.012(6) C73 0.066(6) 0.033(6) 0.084(8) -0.018(5) -0.024(5) -0.005(5) C74 0.066(7) 0.059(8) 0.100(10) -0.013(7) 0.006(7) -0.005(7) C75 0.072(7) 0.051(7) 0.060(7) -0.009(5) 0.014(5) 0.015(6) C76 0.137(12) 0.021(6) 0.094(10) 0.009(6) -0.001(9) 0.008(7) C77 0.092(8) 0.046(6) 0.036(6) -0.002(5) 0.001(5) -0.029(6) C78 0.135(11) 0.059(8) 0.059(7) 0.021(6) 0.038(7) 0.033(8) C79 0.049(6) 0.112(12) 0.111(11) 0.005(9) -0.005(6) 0.038(7) C80 0.075(7) 0.104(10) 0.097(9) 0.018(9) 0.056(6) 0.021(8) C81 0.064(8) 0.131(14) 0.088(10) -0.009(10) 0.014(7) -0.007(9) C82 0.082(10) 0.074(10) 0.171(16) -0.036(10) 0.020(10) -0.003(9) C83 0.061(9) 0.119(15) 0.25(2) -0.037(16) 0.038(12) 0.012(10) C84 0.147(16) 0.110(15) 0.133(16) 0.012(13) 0.024(13) 0.012(13) C85 0.078(10) 0.126(15) 0.161(17) 0.040(13) 0.013(10) 0.027(10) C86 0.057(7) 0.143(13) 0.155(14) 0.074(11) -0.010(8) 0.042(9) C87 0.111(12) 0.163(18) 0.157(16) 0.048(15) -0.047(11) 0.028(13) C88 0.083(9) 0.093(9) 0.167(13) 0.085(9) -0.026(9) 0.012(8) C89 0.146(14) 0.21(2) 0.169(19) 0.077(16) -0.052(13) -0.101(14) C90 0.053(6) 0.071(9) 0.147(12) 0.022(8) 0.043(7) 0.002(7) C91 0.116(11) 0.123(14) 0.095(10) -0.006(10) 0.053(8) -0.003(11) C92 0.043(7) 0.023(7) 0.35(3) 0.019(11) 0.005(11) 0.010(6) C93 0.028(5) 0.109(12) 0.136(13) 0.002(10) -0.002(6) 0.004(7) C94 0.058(7) 0.076(10) 0.134(13) 0.011(9) -0.006(8) 0.008(8) C95 0.131(10) 0.129(11) 0.100(11) 0.042(9) -0.049(8) -0.095(9) C96 0.063(9) 0.20(2) 0.170(19) -0.010(18) -0.014(10) -0.003(13) C97 0.114(12) 0.094(12) 0.144(15) -0.035(11) 0.043(10) -0.044(10) C98 0.058(8) 0.155(17) 0.183(17) 0.060(14) -0.026(9) 0.023(10) C99 0.094(10) 0.121(11) 0.137(13) 0.072(10) 0.008(9) -0.036(9) C100 0.22(2) 0.078(12) 0.157(18) 0.027(13) -0.042(16) -0.015(15) C101 0.045(7) 0.086(11) 0.161(15) 0.011(10) 0.018(8) -0.012(7) C102 0.110(11) 0.138(15) 0.23(2) 0.056(14) 0.085(12) 0.077(11) C103 0.062(7) 0.162(15) 0.188(18) -0.035(13) 0.000(9) 0.073(9) C104 0.17(2) 0.135(19) 0.22(3) 0.05(2) -0.01(2) -0.010(18) Cl9 0.098(5) 0.073(5) 0.180(8) -0.028(5) 0.051(5) 0.021(4) Cl10 0.087(5) 0.173(9) 0.134(7) 0.054(7) 0.017(5) -0.013(6) C105 0.142(15) 0.14(3) 0.39(4) 0.12(2) 0.223(17) 0.081(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ag4 2.9024(14) . ? I1 Ag3 2.9216(14) . ? I1 Ag1 2.9743(14) . ? I2 Ag1 2.7352(14) . ? I3 Ag3 2.8900(14) . ? I3 Ag2 2.9033(15) . ? I3 Ag1 2.9378(15) . ? I4 Ag4 2.8944(13) . ? I4 Ag2 2.9005(15) . ? I4 Ag1 2.9224(15) . ? I5 Ag2 2.7636(15) . ? I6 Ag4 2.9031(14) . ? I6 Ag2 2.9362(14) . ? I6 Ag3 2.9425(15) . ? I7 Ag3 2.7398(15) . ? I8 Ag4 2.7645(14) . ? I9 Ag5 2.8790(14) . ? I9 Ag8 2.8914(15) . ? I9 Ag7 2.9046(16) . ? I10 Ag5 2.7637(14) . ? I11 Ag5 2.8886(14) . ? I11 Ag6 2.9073(15) . ? I11 Ag7 2.9605(15) . ? I12 Ag5 2.9371(14) . ? I12 Ag6 2.9460(15) . ? I12 Ag8 2.9521(15) . ? I13 Ag6 2.7403(16) . ? I14 Ag6 2.8803(16) . ? I14 Ag8 2.8927(15) . ? I14 Ag7 2.9043(16) . ? I15 Ag7 2.7396(16) . ? I16 Ag8 2.7243(16) . ? Ag1 Ag2 3.2680(16) . ? Ag1 Ag4 3.2754(17) . ? Ag1 Ag3 3.3545(16) . ? Ag2 Ag4 3.2933(15) . ? Ag2 Ag3 3.3261(18) . ? Ag3 Ag4 3.3644(16) . ? Ag6 Ag8 3.3789(17) . ? Cl1 C6 1.758(13) . ? Cl2 C19 1.693(14) . ? Cl3 C32 1.687(14) . ? Cl4 C43 1.774(18) . ? Cl5 C56 1.673(12) . ? Cl6 C69 1.711(15) . ? Cl7 C82 1.717(17) . ? Cl8 C95 1.728(17) . ? N1 C10 1.470(7) . ? N1 C12 1.470(7) . ? N1 C1 1.474(7) . ? N1 C8 1.476(7) . ? N2 C23 1.470(7) . ? N2 C25 1.473(7) . ? N2 C21 1.476(7) . ? N2 C14 1.484(7) . ? N3 C27 1.467(7) . ? N3 C34 1.470(7) . ? N3 C36 1.472(7) . ? N3 C38 1.475(7) . ? N4 C49 1.466(7) . ? N4 C40 1.467(7) . ? N4 C51 1.468(7) . ? N4 C47 1.474(7) . ? N5 C62 1.468(7) . ? N5 C53 1.470(7) . ? N5 C60 1.471(7) . ? N5 C64 1.475(7) . ? N6 C75 1.472(7) . ? N6 C73 1.473(7) . ? N6 C66 1.483(7) . ? N6 C77 1.485(7) . ? N7 C88 1.460(7) . ? N7 C79 1.462(8) . ? N7 C86 1.470(7) . ? N7 C90 1.471(7) . ? N8 C103 1.460(7) . ? N8 C101 1.461(7) . ? N8 C99 1.462(7) . ? N8 C92 1.463(8) . ? C1 C2 1.550(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.389(8) . ? C2 C3 1.391(16) . ? C3 C4 1.429(17) . ? C3 H3A 0.9300 . ? C4 C5 1.352(19) . ? C4 H4A 0.9300 . ? C5 C6 1.363(18) . ? C5 H5A 0.9300 . ? C6 C7 1.334(14) . ? C7 H7A 0.9300 . ? C8 C9 1.541(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.543(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.542(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.508(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.319(17) . ? C15 C16 1.385(17) . ? C16 C17 1.337(17) . ? C16 H16A 0.9300 . ? C17 C18 1.392(18) . ? C17 H17A 0.9300 . ? C18 C19 1.474(18) . ? C18 H18A 0.9300 . ? C19 C20 1.407(18) . ? C20 H20A 0.9300 . ? C21 C22 1.531(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.546(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.534(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.475(14) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.377(14) . ? C28 C33 1.408(17) . ? C29 C30 1.388(9) . ? C29 H29A 0.9300 . ? C30 C31 1.44(2) . ? C30 H30A 0.9300 . ? C31 C32 1.395(9) . ? C31 H31A 0.9300 . ? C32 C33 1.390(17) . ? C33 H33A 0.9300 . ? C34 C35 1.542(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.540(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.537(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.575(14) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.367(17) . ? C41 C46 1.387(8) . ? C42 C43 1.38(2) . ? C42 H42A 0.9300 . ? C43 C44 1.37(3) . ? C44 C45 1.34(2) . ? C44 H44A 0.9300 . ? C45 C46 1.35(2) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 C48 1.540(8) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.544(8) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.538(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.522(14) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C59 1.381(16) . ? C54 C55 1.401(16) . ? C55 C56 1.354(17) . ? C55 H55A 0.9300 . ? C56 C57 1.340(19) . ? C57 C58 1.411(19) . ? C57 H57A 0.9300 . ? C58 C59 1.407(17) . ? C58 H58A 0.9300 . ? C59 H59A 0.9300 . ? C60 C61 1.531(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 C63 1.538(7) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.544(8) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 C67 1.487(13) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C72 1.378(16) . ? C67 C68 1.401(15) . ? C68 C69 1.357(18) . ? C68 H68A 0.9300 . ? C69 C70 1.37(2) . ? C70 C71 1.40(2) . ? C70 H70A 0.9300 . ? C71 C72 1.31(2) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C73 C74 1.538(8) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 C76 1.544(7) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 C78 1.541(7) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 C80 1.579(15) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 C81 1.387(16) . ? C80 C85 1.394(8) . ? C81 C82 1.386(9) . ? C81 H81A 0.9300 . ? C82 C83 1.40(3) . ? C83 C84 1.36(3) . ? C83 H83A 0.9300 . ? C84 C85 1.394(9) . ? C84 H84A 0.9300 . ? C85 H85A 0.9300 . ? C86 C87 1.538(8) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 C89 1.537(8) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 C91 1.541(8) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 C93 1.461(19) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C98 1.41(2) . ? C93 C94 1.51(2) . ? C94 C95 1.34(2) . ? C94 H94A 0.9300 . ? C95 C96 1.37(3) . ? C96 C97 1.42(3) . ? C96 H96A 0.9300 . ? C97 C98 1.393(9) . ? C97 H97A 0.9300 . ? C98 H98A 0.9300 . ? C99 C100 1.538(9) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10G 0.9600 . ? C100 H10H 0.9600 . ? C100 H10I 0.9600 . ? C101 C102 1.541(8) . ? C101 H10C 0.9700 . ? C101 H10D 0.9700 . ? C102 H10J 0.9600 . ? C102 H10K 0.9600 . ? C102 H10L 0.9600 . ? C103 C104 1.539(8) . ? C103 H10E 0.9700 . ? C103 H10F 0.9700 . ? C104 H10M 0.9600 . ? C104 H10N 0.9600 . ? C104 H10O 0.9600 . ? Cl9 C105 1.709(8) . ? Cl10 C105 1.711(8) . ? C105 H10P 0.9700 . ? C105 H10Q 0.9700 . ? 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 Ag4 I1 Ag3 70.58(3) . . ? Ag4 I1 Ag1 67.73(4) . . ? Ag3 I1 Ag1 69.35(3) . . ? Ag3 I3 Ag2 70.08(4) . . ? Ag3 I3 Ag1 70.28(3) . . ? Ag2 I3 Ag1 68.04(4) . . ? Ag4 I4 Ag2 69.26(3) . . ? Ag4 I4 Ag1 68.54(4) . . ? Ag2 I4 Ag1 68.28(4) . . ? Ag4 I6 Ag2 68.66(3) . . ? Ag4 I6 Ag3 70.27(3) . . ? Ag2 I6 Ag3 68.92(4) . . ? Ag5 I9 Ag8 75.10(5) . . ? Ag5 I9 Ag7 72.65(4) . . ? Ag8 I9 Ag7 72.38(4) . . ? Ag5 I11 Ag6 71.74(4) . . ? Ag5 I11 Ag7 71.70(4) . . ? Ag6 I11 Ag7 71.57(5) . . ? Ag5 I12 Ag6 70.52(3) . . ? Ag5 I12 Ag8 73.34(4) . . ? Ag6 I12 Ag8 69.90(4) . . ? Ag6 I14 Ag8 71.65(4) . . ? Ag6 I14 Ag7 72.77(5) . . ? Ag8 I14 Ag7 72.36(4) . . ? I2 Ag1 I4 110.92(5) . . ? I2 Ag1 I3 113.39(5) . . ? I4 Ag1 I3 107.89(4) . . ? I2 Ag1 I1 111.31(5) . . ? I4 Ag1 I1 107.46(5) . . ? I3 Ag1 I1 105.54(4) . . ? I2 Ag1 Ag2 145.64(5) . . ? I4 Ag1 Ag2 55.54(3) . . ? I3 Ag1 Ag2 55.48(3) . . ? I1 Ag1 Ag2 103.04(4) . . ? I2 Ag1 Ag4 142.81(5) . . ? I4 Ag1 Ag4 55.33(3) . . ? I3 Ag1 Ag4 103.79(4) . . ? I1 Ag1 Ag4 55.09(3) . . ? Ag2 Ag1 Ag4 60.44(3) . . ? I2 Ag1 Ag3 144.69(5) . . ? I4 Ag1 Ag3 104.38(4) . . ? I3 Ag1 Ag3 54.19(3) . . ? I1 Ag1 Ag3 54.58(3) . . ? Ag2 Ag1 Ag3 60.28(4) . . ? Ag4 Ag1 Ag3 60.98(3) . . ? I5 Ag2 I4 111.24(5) . . ? I5 Ag2 I3 109.56(5) . . ? I4 Ag2 I3 109.44(4) . . ? I5 Ag2 I6 112.69(5) . . ? I4 Ag2 I6 106.52(4) . . ? I3 Ag2 I6 107.26(5) . . ? I5 Ag2 Ag1 143.40(5) . . ? I4 Ag2 Ag1 56.18(3) . . ? I3 Ag2 Ag1 56.48(3) . . ? I6 Ag2 Ag1 103.90(4) . . ? I5 Ag2 Ag4 146.30(5) . . ? I4 Ag2 Ag4 55.28(3) . . ? I3 Ag2 Ag4 104.14(5) . . ? I6 Ag2 Ag4 55.19(3) . . ? Ag1 Ag2 Ag4 59.89(4) . . ? I5 Ag2 Ag3 143.15(5) . . ? I4 Ag2 Ag3 105.59(4) . . ? I3 Ag2 Ag3 54.77(3) . . ? I6 Ag2 Ag3 55.63(3) . . ? Ag1 Ag2 Ag3 61.15(4) . . ? Ag4 Ag2 Ag3 61.09(3) . . ? I7 Ag3 I3 116.31(5) . . ? I7 Ag3 I1 110.04(5) . . ? I3 Ag3 I1 108.19(4) . . ? I7 Ag3 I6 109.44(5) . . ? I3 Ag3 I6 107.44(5) . . ? I1 Ag3 I6 104.78(4) . . ? I7 Ag3 Ag2 146.74(5) . . ? I3 Ag3 Ag2 55.15(4) . . ? I1 Ag3 Ag2 102.82(4) . . ? I6 Ag3 Ag2 55.45(3) . . ? I7 Ag3 Ag1 148.57(5) . . ? I3 Ag3 Ag1 55.53(3) . . ? I1 Ag3 Ag1 56.07(3) . . ? I6 Ag3 Ag1 101.69(4) . . ? Ag2 Ag3 Ag1 58.57(3) . . ? I7 Ag3 Ag4 140.99(5) . . ? I3 Ag3 Ag4 102.70(4) . . ? I1 Ag3 Ag4 54.45(3) . . ? I6 Ag3 Ag4 54.31(3) . . ? Ag2 Ag3 Ag4 58.97(3) . . ? Ag1 Ag3 Ag4 58.35(4) . . ? I8 Ag4 I4 105.59(4) . . ? I8 Ag4 I1 114.08(4) . . ? I4 Ag4 I1 110.20(5) . . ? I8 Ag4 I6 112.97(4) . . ? I4 Ag4 I6 107.56(4) . . ? I1 Ag4 I6 106.29(4) . . ? I8 Ag4 Ag1 142.18(5) . . ? I4 Ag4 Ag1 56.14(3) . . ? I1 Ag4 Ag1 57.18(3) . . ? I6 Ag4 Ag1 104.48(4) . . ? I8 Ag4 Ag2 141.71(5) . . ? I4 Ag4 Ag2 55.45(3) . . ? I1 Ag4 Ag2 104.05(4) . . ? I6 Ag4 Ag2 56.14(3) . . ? Ag1 Ag4 Ag2 59.67(3) . . ? I8 Ag4 Ag3 149.62(4) . . ? I4 Ag4 Ag3 104.77(4) . . ? I1 Ag4 Ag3 54.98(3) . . ? I6 Ag4 Ag3 55.41(3) . . ? Ag1 Ag4 Ag3 60.67(3) . . ? Ag2 Ag4 Ag3 59.93(4) . . ? I10 Ag5 I9 109.24(5) . . ? I10 Ag5 I11 118.53(5) . . ? I9 Ag5 I11 107.19(4) . . ? I10 Ag5 I12 111.61(4) . . ? I9 Ag5 I12 102.45(5) . . ? I11 Ag5 I12 106.55(4) . . ? I13 Ag6 I14 111.53(5) . . ? I13 Ag6 I11 116.51(5) . . ? I14 Ag6 I11 105.57(5) . . ? I13 Ag6 I12 109.56(5) . . ? I14 Ag6 I12 107.33(4) . . ? I11 Ag6 I12 105.82(4) . . ? I13 Ag6 Ag8 139.33(5) . . ? I14 Ag6 Ag8 54.35(3) . . ? I11 Ag6 Ag8 104.15(5) . . ? I12 Ag6 Ag8 55.13(3) . . ? I15 Ag7 I14 111.82(5) . . ? I15 Ag7 I9 116.60(5) . . ? I14 Ag7 I9 105.46(5) . . ? I15 Ag7 I11 113.53(5) . . ? I14 Ag7 I11 103.61(5) . . ? I9 Ag7 I11 104.64(4) . . ? I16 Ag8 I9 118.60(5) . . ? I16 Ag8 I14 107.87(5) . . ? I9 Ag8 I14 106.11(4) . . ? I16 Ag8 I12 114.79(5) . . ? I9 Ag8 I12 101.78(5) . . ? I14 Ag8 I12 106.84(4) . . ? I16 Ag8 Ag6 140.32(5) . . ? I9 Ag8 Ag6 100.97(5) . . ? I14 Ag8 Ag6 54.01(3) . . ? I12 Ag8 Ag6 54.96(3) . . ? C10 N1 C12 111.4(6) . . ? C10 N1 C1 106.4(6) . . ? C12 N1 C1 108.4(6) . . ? C10 N1 C8 108.3(6) . . ? C12 N1 C8 108.4(6) . . ? C1 N1 C8 114.0(6) . . ? C23 N2 C25 111.4(6) . . ? C23 N2 C21 107.9(6) . . ? C25 N2 C21 112.0(7) . . ? C23 N2 C14 111.1(7) . . ? C25 N2 C14 108.0(7) . . ? C21 N2 C14 106.3(6) . . ? C27 N3 C34 112.9(7) . . ? C27 N3 C36 112.2(7) . . ? C34 N3 C36 105.9(5) . . ? C27 N3 C38 104.1(5) . . ? C34 N3 C38 111.7(7) . . ? C36 N3 C38 110.1(7) . . ? C49 N4 C40 100.2(5) . . ? C49 N4 C51 108.5(8) . . ? C40 N4 C51 114.4(8) . . ? C49 N4 C47 113.2(7) . . ? C40 N4 C47 114.0(7) . . ? C51 N4 C47 106.5(5) . . ? C62 N5 C53 110.7(6) . . ? C62 N5 C60 106.4(5) . . ? C53 N5 C60 114.3(7) . . ? C62 N5 C64 106.9(7) . . ? C53 N5 C64 106.5(5) . . ? C60 N5 C64 111.9(7) . . ? C75 N6 C73 111.2(7) . . ? C75 N6 C66 107.1(5) . . ? C73 N6 C66 111.9(7) . . ? C75 N6 C77 111.9(6) . . ? C73 N6 C77 103.4(5) . . ? C66 N6 C77 111.5(7) . . ? C88 N7 C79 100.5(6) . . ? C88 N7 C86 109.0(9) . . ? C79 N7 C86 110.2(9) . . ? C88 N7 C90 117.4(8) . . ? C79 N7 C90 116.8(8) . . ? C86 N7 C90 102.8(5) . . ? C103 N8 C101 111.5(10) . . ? C103 N8 C99 102.3(5) . . ? C101 N8 C99 120.7(9) . . ? C103 N8 C92 111.0(10) . . ? C101 N8 C92 106.2(6) . . ? C99 N8 C92 105.0(8) . . ? N1 C1 C2 116.1(7) . . ? N1 C1 H1A 108.3 . . ? C2 C1 H1A 108.3 . . ? N1 C1 H1B 108.3 . . ? C2 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C7 C2 C3 118.6(9) . . ? C7 C2 C1 121.8(8) . . ? C3 C2 C1 118.8(8) . . ? C2 C3 C4 120.9(12) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 116.4(13) . . ? C5 C4 H4A 121.8 . . ? C3 C4 H4A 121.8 . . ? C4 C5 C6 121.9(12) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C7 C6 C5 122.3(11) . . ? C7 C6 Cl1 118.2(9) . . ? C5 C6 Cl1 119.5(9) . . ? C6 C7 C2 119.5(10) . . ? C6 C7 H7A 120.2 . . ? C2 C7 H7A 120.2 . . ? N1 C8 C9 116.0(7) . . ? N1 C8 H8A 108.3 . . ? C9 C8 H8A 108.3 . . ? N1 C8 H8B 108.3 . . ? C9 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 115.0(7) . . ? N1 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? N1 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 113.9(7) . . ? N1 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? N1 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C15 117.1(9) . . ? N2 C14 H14A 108.0 . . ? C15 C14 H14A 108.0 . . ? N2 C14 H14B 108.0 . . ? C15 C14 H14B 108.0 . . ? H14A C14 H14B 107.3 . . ? C20 C15 C16 119.6(11) . . ? C20 C15 C14 120.8(11) . . ? C16 C15 C14 119.5(11) . . ? C17 C16 C15 123.6(12) . . ? C17 C16 H16A 118.2 . . ? C15 C16 H16A 118.2 . . ? C16 C17 C18 119.7(12) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C17 C18 C19 117.5(12) . . ? C17 C18 H18A 121.3 . . ? C19 C18 H18A 121.3 . . ? C20 C19 C18 118.0(12) . . ? C20 C19 Cl2 124.1(10) . . ? C18 C19 Cl2 117.6(11) . . ? C15 C20 C19 121.2(12) . . ? C15 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? N2 C21 C22 116.5(7) . . ? N2 C21 H21A 108.2 . . ? C22 C21 H21A 108.2 . . ? N2 C21 H21B 108.2 . . ? C22 C21 H21B 108.2 . . ? H21A C21 H21B 107.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 C24 118.5(7) . . ? N2 C23 H23A 107.7 . . ? C24 C23 H23A 107.7 . . ? N2 C23 H23B 107.7 . . ? C24 C23 H23B 107.7 . . ? H23A C23 H23B 107.1 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 C26 120.4(7) . . ? N2 C25 H25A 107.2 . . ? C26 C25 H25A 107.2 . . ? N2 C25 H25B 107.2 . . ? C26 C25 H25B 107.2 . . ? H25A C25 H25B 106.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 118.0(7) . . ? N3 C27 H27A 107.8 . . ? C28 C27 H27A 107.8 . . ? N3 C27 H27B 107.8 . . ? C28 C27 H27B 107.8 . . ? H27A C27 H27B 107.1 . . ? C29 C28 C33 117.4(11) . . ? C29 C28 C27 125.1(10) . . ? C33 C28 C27 117.4(10) . . ? C28 C29 C30 122.4(12) . . ? C28 C29 H29A 118.8 . . ? C30 C29 H29A 118.8 . . ? C29 C30 C31 118.5(12) . . ? C29 C30 H30A 120.8 . . ? C31 C30 H30A 120.8 . . ? C32 C31 C30 120.5(11) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C33 C32 C31 117.5(12) . . ? C33 C32 Cl3 122.2(9) . . ? C31 C32 Cl3 119.3(10) . . ? C32 C33 C28 123.4(12) . . ? C32 C33 H33A 118.3 . . ? C28 C33 H33A 118.3 . . ? N3 C34 C35 115.7(7) . . ? N3 C34 H34A 108.4 . . ? C35 C34 H34A 108.4 . . ? N3 C34 H34B 108.4 . . ? C35 C34 H34B 108.4 . . ? H34A C34 H34B 107.4 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C37 115.1(6) . . ? N3 C36 H36A 108.5 . . ? C37 C36 H36A 108.5 . . ? N3 C36 H36B 108.5 . . ? C37 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 C39 116.3(7) . . ? N3 C38 H38A 108.2 . . ? C39 C38 H38A 108.2 . . ? N3 C38 H38B 108.2 . . ? C39 C38 H38B 108.2 . . ? H38A C38 H38B 107.4 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 C41 119.1(7) . . ? N4 C40 H40A 107.5 . . ? C41 C40 H40A 107.5 . . ? N4 C40 H40B 107.5 . . ? C41 C40 H40B 107.5 . . ? H40A C40 H40B 107.0 . . ? C42 C41 C46 119.6(12) . . ? C42 C41 C40 121.0(10) . . ? C46 C41 C40 119.4(10) . . ? C41 C42 C43 119.2(14) . . ? C41 C42 H42A 120.4 . . ? C43 C42 H42A 120.4 . . ? C44 C43 C42 121.0(16) . . ? C44 C43 Cl4 124.2(13) . . ? C42 C43 Cl4 114.6(13) . . ? C45 C44 C43 118.1(16) . . ? C45 C44 H44A 120.9 . . ? C43 C44 H44A 120.9 . . ? C44 C45 C46 123.0(16) . . ? C44 C45 H45A 118.5 . . ? C46 C45 H45A 118.5 . . ? C45 C46 C41 119.0(12) . . ? C45 C46 H46A 120.5 . . ? C41 C46 H46A 120.5 . . ? N4 C47 C48 112.7(7) . . ? N4 C47 H47A 109.1 . . ? C48 C47 H47A 109.1 . . ? N4 C47 H47B 109.1 . . ? C48 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N4 C49 C50 115.2(7) . . ? N4 C49 H49A 108.5 . . ? C50 C49 H49A 108.5 . . ? N4 C49 H49B 108.5 . . ? C50 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N4 C51 C52 120.4(8) . . ? N4 C51 H51A 107.2 . . ? C52 C51 H51A 107.2 . . ? N4 C51 H51B 107.2 . . ? C52 C51 H51B 107.2 . . ? H51A C51 H51B 106.8 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N5 C53 C54 116.3(8) . . ? N5 C53 H53A 108.2 . . ? C54 C53 H53A 108.2 . . ? N5 C53 H53B 108.2 . . ? C54 C53 H53B 108.2 . . ? H53A C53 H53B 107.4 . . ? C59 C54 C55 117.3(11) . . ? C59 C54 C53 118.3(10) . . ? C55 C54 C53 122.9(11) . . ? C56 C55 C54 124.4(12) . . ? C56 C55 H55A 117.8 . . ? C54 C55 H55A 117.8 . . ? C57 C56 C55 117.7(11) . . ? C57 C56 Cl5 119.1(10) . . ? C55 C56 Cl5 123.0(10) . . ? C56 C57 C58 121.3(12) . . ? C56 C57 H57A 119.3 . . ? C58 C57 H57A 119.3 . . ? C59 C58 C57 119.4(12) . . ? C59 C58 H58A 120.3 . . ? C57 C58 H58A 120.3 . . ? C54 C59 C58 119.1(11) . . ? C54 C59 H59A 120.5 . . ? C58 C59 H59A 120.5 . . ? N5 C60 C61 113.8(6) . . ? N5 C60 H60A 108.8 . . ? C61 C60 H60A 108.8 . . ? N5 C60 H60B 108.8 . . ? C61 C60 H60B 108.8 . . ? H60A C60 H60B 107.7 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N5 C62 C63 118.4(7) . . ? N5 C62 H62A 107.7 . . ? C63 C62 H62A 107.7 . . ? N5 C62 H62B 107.7 . . ? C63 C62 H62B 107.7 . . ? H62A C62 H62B 107.1 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N5 C64 C65 115.9(7) . . ? N5 C64 H64A 108.3 . . ? C65 C64 H64A 108.3 . . ? N5 C64 H64B 108.3 . . ? C65 C64 H64B 108.3 . . ? H64A C64 H64B 107.4 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N6 C66 C67 117.0(7) . . ? N6 C66 H66A 108.1 . . ? C67 C66 H66A 108.1 . . ? N6 C66 H66B 108.1 . . ? C67 C66 H66B 108.1 . . ? H66A C66 H66B 107.3 . . ? C72 C67 C68 118.5(11) . . ? C72 C67 C66 125.6(10) . . ? C68 C67 C66 115.7(10) . . ? C69 C68 C67 119.6(12) . . ? C69 C68 H68A 120.2 . . ? C67 C68 H68A 120.2 . . ? C68 C69 C70 117.1(13) . . ? C68 C69 Cl6 120.5(13) . . ? C70 C69 Cl6 122.2(12) . . ? C69 C70 C71 124.5(14) . . ? C69 C70 H70A 117.8 . . ? C71 C70 H70A 117.8 . . ? C72 C71 C70 114.3(15) . . ? C72 C71 H71A 122.9 . . ? C70 C71 H71A 122.9 . . ? C71 C72 C67 124.7(14) . . ? C71 C72 H72A 117.6 . . ? C67 C72 H72A 117.6 . . ? N6 C73 C74 114.0(6) . . ? N6 C73 H73A 108.7 . . ? C74 C73 H73A 108.7 . . ? N6 C73 H73B 108.7 . . ? C74 C73 H73B 108.7 . . ? H73A C73 H73B 107.6 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N6 C75 C76 119.2(7) . . ? N6 C75 H75A 107.5 . . ? C76 C75 H75A 107.5 . . ? N6 C75 H75B 107.5 . . ? C76 C75 H75B 107.5 . . ? H75A C75 H75B 107.0 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N6 C77 C78 117.1(7) . . ? N6 C77 H77A 108.0 . . ? C78 C77 H77A 108.0 . . ? N6 C77 H77B 108.0 . . ? C78 C77 H77B 108.0 . . ? H77A C77 H77B 107.3 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N7 C79 C80 118.1(8) . . ? N7 C79 H79A 107.8 . . ? C80 C79 H79A 107.8 . . ? N7 C79 H79B 107.8 . . ? C80 C79 H79B 107.8 . . ? H79A C79 H79B 107.1 . . ? C81 C80 C85 121.6(11) . . ? C81 C80 C79 119.9(9) . . ? C85 C80 C79 118.1(10) . . ? C82 C81 C80 113.7(13) . . ? C82 C81 H81A 123.2 . . ? C80 C81 H81A 123.2 . . ? C81 C82 C83 123.4(16) . . ? C81 C82 Cl7 117.4(13) . . ? C83 C82 Cl7 117.6(10) . . ? C84 C83 C82 121.5(17) . . ? C84 C83 H83A 119.2 . . ? C82 C83 H83A 119.2 . . ? C83 C84 C85 115.1(17) . . ? C83 C84 H84A 122.5 . . ? C85 C84 H84A 122.5 . . ? C84 C85 C80 123.1(13) . . ? C84 C85 H85A 118.4 . . ? C80 C85 H85A 118.4 . . ? N7 C86 C87 118.3(7) . . ? N7 C86 H86A 107.7 . . ? C87 C86 H86A 107.7 . . ? N7 C86 H86B 107.7 . . ? C87 C86 H86B 107.7 . . ? H86A C86 H86B 107.1 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N7 C88 C89 112.5(8) . . ? N7 C88 H88A 109.1 . . ? C89 C88 H88A 109.1 . . ? N7 C88 H88B 109.1 . . ? C89 C88 H88B 109.1 . . ? H88A C88 H88B 107.8 . . ? C88 C89 H89A 109.5 . . ? C88 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C88 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N7 C90 C91 112.2(7) . . ? N7 C90 H90A 109.2 . . ? C91 C90 H90A 109.2 . . ? N7 C90 H90B 109.2 . . ? C91 C90 H90B 109.2 . . ? H90A C90 H90B 107.9 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C93 C92 N8 120.1(9) . . ? C93 C92 H92A 107.3 . . ? N8 C92 H92A 107.3 . . ? C93 C92 H92B 107.3 . . ? N8 C92 H92B 107.3 . . ? H92A C92 H92B 106.9 . . ? C98 C93 C92 130.4(14) . . ? C98 C93 C94 110.1(13) . . ? C92 C93 C94 119.5(13) . . ? C95 C94 C93 119.1(14) . . ? C95 C94 H94A 120.5 . . ? C93 C94 H94A 120.5 . . ? C94 C95 C96 133.9(18) . . ? C94 C95 Cl8 113.8(14) . . ? C96 C95 Cl8 112.3(15) . . ? C95 C96 C97 105.5(18) . . ? C95 C96 H96A 127.3 . . ? C97 C96 H96A 127.3 . . ? C98 C97 C96 127.4(16) . . ? C98 C97 H97A 116.3 . . ? C96 C97 H97A 116.3 . . ? C97 C98 C93 123.9(16) . . ? C97 C98 H98A 118.0 . . ? C93 C98 H98A 118.0 . . ? N8 C99 C100 114.6(8) . . ? N8 C99 H99A 108.6 . . ? C100 C99 H99A 108.6 . . ? N8 C99 H99B 108.6 . . ? C100 C99 H99B 108.6 . . ? H99A C99 H99B 107.6 . . ? C99 C100 H10G 109.5 . . ? C99 C100 H10H 109.5 . . ? H10G C100 H10H 109.5 . . ? C99 C100 H10I 109.5 . . ? H10G C100 H10I 109.5 . . ? H10H C100 H10I 109.5 . . ? N8 C101 C102 115.1(7) . . ? N8 C101 H10C 108.5 . . ? C102 C101 H10C 108.5 . . ? N8 C101 H10D 108.5 . . ? C102 C101 H10D 108.5 . . ? H10C C101 H10D 107.5 . . ? C101 C102 H10J 109.5 . . ? C101 C102 H10K 109.5 . . ? H10J C102 H10K 109.5 . . ? C101 C102 H10L 109.5 . . ? H10J C102 H10L 109.5 . . ? H10K C102 H10L 109.5 . . ? N8 C103 C104 111.8(8) . . ? N8 C103 H10E 109.3 . . ? C104 C103 H10E 109.3 . . ? N8 C103 H10F 109.3 . . ? C104 C103 H10F 109.3 . . ? H10E C103 H10F 107.9 . . ? C103 C104 H10M 109.5 . . ? C103 C104 H10N 109.5 . . ? H10M C104 H10N 109.5 . . ? C103 C104 H10O 109.5 . . ? H10M C104 H10O 109.5 . . ? H10N C104 H10O 109.5 . . ? Cl9 C105 Cl10 114.3(7) . . ? Cl9 C105 H10P 108.7 . . ? Cl10 C105 H10P 108.7 . . ? Cl9 C105 H10Q 108.7 . . ? Cl10 C105 H10Q 108.7 . . ? H10P C105 H10Q 107.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.864 _refine_diff_density_min -2.036 _refine_diff_density_rms 0.223