# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: 3-D organisation of decanuclear silver nanoclusters ; loop_ _publ_author_name 'Mir Wais Hosseini' 'Igor S. Antipin' 'Sylvie Ferlay' 'Alexander Konovalov' 'Marina N. Kozlova' ; N.Kyritsakas ; 'Svetlana Solovieva' # Attachment 'Chemcommmarinanew.cif' ###Material relevant to compound 2Ag at 173K ######## data_719024 _database_code_depnum_ccdc_archive 'CCDC 719024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 Ag5 N7 O17 S2' _chemical_formula_sum 'C36 H34 Ag5 N7 O17 S2' _chemical_formula_weight 1440.17 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n _symmetry_space_group_name_Hall '-P 4bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 13.0057(18) _cell_length_b 13.0057(18) _cell_length_c 25.768(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4358.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 2.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7161 _exptl_absorpt_correction_T_max 0.7964 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 119655 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0105 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5003 _reflns_number_gt 4397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0910P)^2^+7.0555P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5003 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1799 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.05448(5) 0.46811(4) 0.16560(2) 0.03597(18) Uani 1 1 d . . . Ag2 Ag 0.19502(4) 0.56882(4) 0.27311(2) 0.03627(18) Uani 1 1 d . . . Ag3 Ag 0.2500 0.2500 0.14299(7) 0.03627(18) Uani 1 2 d S . . S1 S 0.00687(10) 0.59566(10) 0.23558(5) 0.0136(3) Uani 1 1 d . . . C1 C -0.0171(4) 0.7231(4) 0.21283(19) 0.0122(9) Uani 1 1 d . . . C2 C -0.0491(4) 0.8024(4) 0.24592(19) 0.0119(9) Uani 1 1 d . . . C3 C -0.0612(4) 0.9006(4) 0.2245(2) 0.0134(9) Uani 1 1 d . . . C4 C -0.0360(4) 0.9203(4) 0.1735(2) 0.0145(10) Uani 1 1 d . . . H4 H -0.0449 0.9878 0.1601 0.017 Uiso 1 1 calc R . . C5 C 0.0023(4) 0.8435(4) 0.1410(2) 0.0143(10) Uani 1 1 d . . . C6 C 0.0085(4) 0.7444(4) 0.16131(19) 0.0138(9) Uani 1 1 d . . . H6 H 0.0307 0.6899 0.1395 0.017 Uiso 1 1 calc R . . O1 O -0.0659(3) 0.7880(3) 0.29815(14) 0.0150(7) Uani 1 1 d . . . C7 C 0.0296(4) 0.7851(5) 0.3263(2) 0.0212(11) Uani 1 1 d . . . H7A H 0.0770 0.8375 0.3120 0.025 Uiso 1 1 calc R . . H7B H 0.0620 0.7168 0.3219 0.025 Uiso 1 1 calc R . . C8 C 0.0129(5) 0.8055(4) 0.3832(2) 0.0187(11) Uani 1 1 d . . . C9 C 0.0993(5) 0.7955(6) 0.4156(3) 0.0329(15) Uani 1 1 d . . . H9 H 0.1629 0.7734 0.4014 0.040 Uiso 1 1 calc R . . C10 C 0.0926(6) 0.8172(6) 0.4671(3) 0.0352(16) Uani 1 1 d . . . H10 H 0.1517 0.8117 0.4886 0.042 Uiso 1 1 calc R . . C11 C -0.0009(6) 0.8473(5) 0.4882(2) 0.0288(14) Uani 1 1 d . . . C12 C -0.0889(6) 0.8546(6) 0.4570(3) 0.0375(17) Uani 1 1 d . . . H12 H -0.1532 0.8736 0.4716 0.045 Uiso 1 1 calc R . . C13 C -0.0806(5) 0.8336(6) 0.4045(2) 0.0298(14) Uani 1 1 d . . . H13 H -0.1396 0.8385 0.3829 0.036 Uiso 1 1 calc R . . C14 C 0.1277(6) 0.4946(6) 0.0428(3) 0.0336(15) Uani 1 1 d . . . N1 N 0.1082(5) 0.4949(5) 0.0856(2) 0.0376(14) Uani 1 1 d . . . C15 C 0.0355(4) 0.8697(4) 0.0855(2) 0.0173(10) Uani 1 1 d . . . C16 C 0.0886(6) 0.7786(5) 0.0590(2) 0.0285(14) Uani 1 1 d . . . H16A H 0.0418 0.7195 0.0584 0.043 Uiso 1 1 calc R . . H16B H 0.1509 0.7604 0.0783 0.043 Uiso 1 1 calc R . . H16C H 0.1070 0.7975 0.0234 0.043 Uiso 1 1 calc R . . C17 C -0.0592(5) 0.9007(5) 0.0539(2) 0.0277(13) Uani 1 1 d . . . H17A H -0.1099 0.8450 0.0548 0.042 Uiso 1 1 calc R . . H17B H -0.0389 0.9138 0.0178 0.042 Uiso 1 1 calc R . . H17C H -0.0894 0.9631 0.0687 0.042 Uiso 1 1 calc R . . C18 C 0.1123(5) 0.9601(5) 0.0869(2) 0.0278(13) Uani 1 1 d . . . H18A H 0.1346 0.9763 0.0516 0.042 Uiso 1 1 calc R . . H18B H 0.1721 0.9410 0.1079 0.042 Uiso 1 1 calc R . . H18C H 0.0789 1.0205 0.1023 0.042 Uiso 1 1 calc R . . N2 N -0.0202(9) 0.2439(6) 0.1130(3) 0.0596(18) Uani 1 1 d . . . O2 O 0.0403(18) 0.2649(9) 0.0795(5) 0.0596(18) Uani 1 1 d . . . O3 O -0.0207(6) 0.3013(5) 0.1531(3) 0.0596(18) Uani 1 1 d . . . O4 O -0.0752(8) 0.1695(6) 0.1117(5) 0.0596(18) Uani 1 1 d . . . N3 N 0.3248(4) 0.4148(5) 0.2113(2) 0.0326(13) Uani 1 1 d . . . O5 O 0.3881(5) 0.3594(5) 0.1882(2) 0.0495(15) Uani 1 1 d . . . O6 O 0.3539(4) 0.4803(4) 0.2430(2) 0.0424(13) Uani 1 1 d . . . O7 O 0.2306(4) 0.4023(5) 0.2028(3) 0.0524(16) Uani 1 1 d . . . N4 N 0.2500 0.7500 0.2057(3) 0.0263(15) Uani 1 2 d S . . O8 O 0.2291(4) 0.6690(4) 0.1825(2) 0.0375(11) Uani 1 1 d . . . O9 O 0.2500 0.7500 0.2554(3) 0.0365(16) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0526(4) 0.0347(3) 0.0206(3) -0.00018(19) 0.0146(2) 0.0035(2) Ag2 0.0261(3) 0.0341(3) 0.0486(4) 0.0011(2) -0.0036(2) 0.0022(2) Ag3 0.0261(3) 0.0341(3) 0.0486(4) 0.0011(2) -0.0036(2) 0.0022(2) S1 0.0140(6) 0.0146(6) 0.0122(5) 0.0030(4) 0.0036(4) 0.0015(4) C1 0.012(2) 0.013(2) 0.012(2) 0.0011(18) 0.0013(17) -0.0007(17) C2 0.013(2) 0.014(2) 0.009(2) 0.0000(17) 0.0021(17) -0.0003(17) C3 0.013(2) 0.013(2) 0.014(2) -0.0027(18) 0.0005(18) -0.0004(18) C4 0.017(2) 0.011(2) 0.015(2) 0.0006(18) 0.0034(19) -0.0008(18) C5 0.015(2) 0.017(2) 0.012(2) 0.0002(18) 0.0033(18) -0.0019(18) C6 0.015(2) 0.013(2) 0.013(2) -0.0012(18) 0.0033(18) 0.0008(18) O1 0.0165(17) 0.0210(18) 0.0075(16) 0.0015(13) 0.0012(13) -0.0011(14) C7 0.016(2) 0.034(3) 0.013(2) -0.002(2) -0.002(2) 0.002(2) C8 0.025(3) 0.019(3) 0.012(2) -0.0005(19) -0.001(2) -0.002(2) C9 0.021(3) 0.057(4) 0.022(3) -0.009(3) -0.004(2) -0.002(3) C10 0.030(3) 0.058(5) 0.018(3) -0.003(3) -0.012(2) -0.004(3) C11 0.044(4) 0.029(3) 0.013(3) -0.005(2) -0.005(2) 0.006(3) C12 0.039(4) 0.054(4) 0.019(3) -0.007(3) -0.004(3) 0.026(3) C13 0.030(3) 0.043(4) 0.016(3) 0.001(3) -0.003(2) 0.016(3) C14 0.034(3) 0.047(4) 0.020(3) -0.006(3) 0.004(3) -0.012(3) N1 0.047(4) 0.046(4) 0.020(3) -0.005(2) 0.010(2) -0.011(3) C15 0.022(3) 0.019(2) 0.011(2) 0.0016(19) 0.0052(19) 0.002(2) C16 0.042(4) 0.028(3) 0.015(3) 0.002(2) 0.015(2) 0.008(3) C17 0.032(3) 0.037(3) 0.015(3) 0.003(2) 0.000(2) 0.005(3) C18 0.034(3) 0.026(3) 0.023(3) 0.003(2) 0.010(2) -0.009(3) N2 0.092(5) 0.032(3) 0.055(4) 0.007(3) -0.019(4) 0.000(3) O2 0.092(5) 0.032(3) 0.055(4) 0.007(3) -0.019(4) 0.000(3) O3 0.092(5) 0.032(3) 0.055(4) 0.007(3) -0.019(4) 0.000(3) O4 0.092(5) 0.032(3) 0.055(4) 0.007(3) -0.019(4) 0.000(3) N3 0.024(3) 0.037(3) 0.037(3) 0.013(3) 0.000(2) 0.005(2) O5 0.037(3) 0.066(4) 0.045(3) -0.004(3) 0.005(2) 0.012(3) O6 0.041(3) 0.037(3) 0.050(3) 0.001(2) -0.001(2) 0.002(2) O7 0.024(3) 0.068(4) 0.065(4) 0.017(3) -0.006(3) 0.000(3) N4 0.014(3) 0.034(4) 0.031(4) 0.000 0.000 0.002(3) O8 0.029(2) 0.042(3) 0.042(3) -0.011(2) -0.003(2) 0.001(2) O9 0.031(4) 0.046(4) 0.033(4) 0.000 0.000 -0.003(3) _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 N1 2.203(6) . ? Ag1 O3 2.402(6) . ? Ag1 S1 2.5271(14) . ? Ag2 O3 2.432(7) 7_566 ? Ag2 O6 2.489(6) . ? Ag2 O9 2.5042(15) . ? Ag2 S1 2.6542(14) . ? Ag3 O7 2.523(8) 2 ? Ag3 O7 2.523(8) . ? Ag3 O5 2.571(7) . ? Ag3 O5 2.571(7) 2 ? S1 C3 1.780(5) 7_466 ? S1 C1 1.785(5) . ? C1 C6 1.396(7) . ? C1 C2 1.401(7) . ? C2 O1 1.376(6) . ? C2 C3 1.400(7) . ? C3 C4 1.380(7) . ? C3 S1 1.780(5) 8_666 ? C4 C5 1.395(7) . ? C4 H4 0.9500 . ? C5 C6 1.392(7) . ? C5 C15 1.533(7) . ? C6 H6 0.9500 . ? O1 C7 1.439(6) . ? C7 C8 1.505(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.383(9) . ? C8 C9 1.406(8) . ? C9 C10 1.359(9) . ? C9 H9 0.9500 . ? C10 C11 1.388(10) . ? C10 H10 0.9500 . ? C11 C12 1.403(10) . ? C11 C14 1.445(8) 4_465 ? C12 C13 1.384(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 N1 1.132(9) . ? C14 C11 1.445(8) 3_654 ? C15 C17 1.531(8) . ? C15 C16 1.533(8) . ? C15 C18 1.543(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N2 O2 1.200(17) . ? N2 O4 1.203(12) . ? N2 O3 1.274(10) . ? O3 Ag2 2.432(7) 8_656 ? N3 O6 1.240(9) . ? N3 O5 1.245(8) . ? N3 O7 1.255(8) . ? N4 O8 1.242(6) . ? N4 O8 1.242(6) 2_565 ? N4 O9 1.281(11) . ? O9 Ag2 2.5042(15) 2_565 ? 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 N1 Ag1 O3 98.4(2) . . ? N1 Ag1 S1 129.87(18) . . ? O3 Ag1 S1 126.1(2) . . ? O3 Ag2 O6 69.7(2) 7_566 . ? O3 Ag2 O9 102.8(2) 7_566 . ? O6 Ag2 O9 98.14(15) . . ? O3 Ag2 S1 147.39(16) 7_566 . ? O6 Ag2 S1 135.46(14) . . ? O9 Ag2 S1 94.20(7) . . ? O7 Ag3 O7 104.6(3) 2 . ? O7 Ag3 O5 95.0(2) 2 . ? O7 Ag3 O5 50.06(18) . . ? O7 Ag3 O5 50.06(18) 2 2 ? O7 Ag3 O5 95.0(2) . 2 ? O5 Ag3 O5 126.1(3) . 2 ? C3 S1 C1 106.7(2) 7_466 . ? C3 S1 Ag1 115.93(18) 7_466 . ? C1 S1 Ag1 114.69(17) . . ? C3 S1 Ag2 118.20(18) 7_466 . ? C1 S1 Ag2 113.75(17) . . ? Ag1 S1 Ag2 87.01(4) . . ? C6 C1 C2 120.2(5) . . ? C6 C1 S1 117.1(4) . . ? C2 C1 S1 122.4(4) . . ? O1 C2 C3 119.4(4) . . ? O1 C2 C1 122.8(4) . . ? C3 C2 C1 117.7(4) . . ? C4 C3 C2 121.2(5) . . ? C4 C3 S1 117.8(4) . 8_666 ? C2 C3 S1 120.6(4) . 8_666 ? C3 C4 C5 121.6(5) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 117.3(5) . . ? C6 C5 C15 122.7(5) . . ? C4 C5 C15 120.0(5) . . ? C5 C6 C1 121.8(5) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? C2 O1 C7 111.0(4) . . ? O1 C7 C8 111.2(5) . . ? O1 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? O1 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C13 C8 C9 119.4(5) . . ? C13 C8 C7 124.0(5) . . ? C9 C8 C7 116.6(5) . . ? C10 C9 C8 120.7(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.8(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.6(6) . . ? C10 C11 C14 118.7(6) . 4_465 ? C12 C11 C14 120.7(6) . 4_465 ? C13 C12 C11 118.9(6) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C8 C13 C12 120.6(6) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? N1 C14 C11 177.5(8) . 3_654 ? C14 N1 Ag1 169.0(6) . . ? C17 C15 C16 109.2(5) . . ? C17 C15 C5 109.2(4) . . ? C16 C15 C5 111.8(4) . . ? C17 C15 C18 109.4(5) . . ? C16 C15 C18 108.0(5) . . ? C5 C15 C18 109.2(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 N2 O4 123.5(12) . . ? O2 N2 O3 117.0(11) . . ? O4 N2 O3 119.3(11) . . ? N2 O3 Ag1 129.5(7) . . ? N2 O3 Ag2 107.6(5) . 8_656 ? Ag1 O3 Ag2 120.8(3) . 8_656 ? O6 N3 O5 120.7(6) . . ? O6 N3 O7 120.2(7) . . ? O5 N3 O7 119.2(7) . . ? N3 O5 Ag3 94.3(4) . . ? N3 O6 Ag2 105.6(4) . . ? N3 O7 Ag3 96.4(5) . . ? O8 N4 O8 122.4(9) . 2_565 ? O8 N4 O9 118.8(4) . . ? O8 N4 O9 118.8(4) 2_565 . ? N4 O9 Ag2 100.48(17) . 2_565 ? N4 O9 Ag2 100.48(17) . . ? Ag2 O9 Ag2 159.0(3) 2_565 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.141 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.191 #===END ###Material relevant to compound 2 at 173K ######## data_719025 _database_code_depnum_ccdc_archive 'CCDC 719025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H69 Cl3 N4 O4 S4' _chemical_formula_weight 1300.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.864(3) _cell_length_b 15.832(3) _cell_length_c 32.521(6) _cell_angle_alpha 88.665(2) _cell_angle_beta 88.330(2) _cell_angle_gamma 62.743(3) _cell_volume 6800(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1815 _cell_measurement_theta_min 6.91 _cell_measurement_theta_max 20.04 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9551 _exptl_absorpt_correction_T_max 0.9698 _exptl_absorpt_process_details sadabs _exptl_special_details ; In one of the thiacalixarene derivatives, a t-Bu group shows positional disorder over two positions. Similarly, a chloroform solvate molecule shows disorder. ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34330 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.1603 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 6.91 _diffrn_reflns_theta_max 26.80 _reflns_number_total 27324 _reflns_number_gt 14060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Restraints have been imposed on disordered solvents. ; _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^)+(0.1311P)^2^+1.6148P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27324 _refine_ls_number_parameters 1530 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1783 _refine_ls_R_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.3017 _refine_ls_wR_factor_gt 0.2571 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.94618(10) 0.57017(9) 0.06432(4) 0.0338(3) Uani 1 1 d . . . C1 C 0.9960(3) 0.4637(3) 0.09370(14) 0.0267(10) Uani 1 1 d . . . C2 C 0.9685(3) 0.4589(3) 0.13445(14) 0.0241(10) Uani 1 1 d . . . C3 C 1.0217(3) 0.3751(3) 0.15708(13) 0.0233(10) Uani 1 1 d . . . C4 C 1.1059(3) 0.2995(3) 0.13937(14) 0.0276(10) Uani 1 1 d . . . H4 H 1.1428 0.2435 0.1552 0.033 Uiso 1 1 calc R . . C5 C 1.1370(3) 0.3046(3) 0.09885(14) 0.0263(10) Uani 1 1 d . . . C6 C 1.0794(4) 0.3865(3) 0.07618(15) 0.0284(10) Uani 1 1 d . . . H6 H 1.0971 0.3901 0.0481 0.034 Uiso 1 1 calc R . . O1 O 0.8885(2) 0.5360(2) 0.15278(10) 0.0282(7) Uani 1 1 d . . . C7 C 0.9201(4) 0.5994(4) 0.17111(18) 0.0397(13) Uani 1 1 d . . . H7A H 0.9486 0.6262 0.1496 0.048 Uiso 1 1 calc R . . H7B H 0.9733 0.5643 0.1914 0.048 Uiso 1 1 calc R . . C8 C 0.8318(4) 0.6773(3) 0.19182(16) 0.0402(13) Uani 1 1 d . . . C9 C 0.7337(5) 0.6876(4) 0.1892(2) 0.0525(16) Uani 1 1 d . . . H9 H 0.7209 0.6439 0.1740 0.063 Uiso 1 1 calc R . . C10 C 0.6549(5) 0.7632(5) 0.2093(2) 0.069(2) Uani 1 1 d . . . H10 H 0.5877 0.7712 0.2077 0.083 Uiso 1 1 calc R . . C11 C 0.6734(8) 0.8272(5) 0.2318(2) 0.075(3) Uani 1 1 d . . . C12 C 0.7684(9) 0.8173(5) 0.2339(2) 0.088(3) Uani 1 1 d . . . H12 H 0.7804 0.8613 0.2493 0.106 Uiso 1 1 calc R . . C13 C 0.8482(6) 0.7439(4) 0.2139(2) 0.0638(19) Uani 1 1 d . . . H13 H 0.9144 0.7385 0.2150 0.077 Uiso 1 1 calc R . . C14 C 0.5885(7) 0.9047(5) 0.2525(2) 0.083 Uani 1 1 d . . . N1 N 0.5242(6) 0.9662(4) 0.26893(19) 0.083 Uani 1 1 d . . . C15 C 1.2342(4) 0.2221(4) 0.08131(15) 0.0373(13) Uani 1 1 d . . . C16 C 1.2501(7) 0.2378(6) 0.0362(2) 0.105(4) Uani 1 1 d . . . H16A H 1.3052 0.1799 0.0248 0.157 Uiso 1 1 calc R . . H16B H 1.2675 0.2903 0.0331 0.157 Uiso 1 1 calc R . . H16C H 1.1878 0.2535 0.0214 0.157 Uiso 1 1 calc R . . C17 C 1.3231(4) 0.2158(6) 0.1058(3) 0.070(2) Uani 1 1 d . . . H17A H 1.3155 0.1998 0.1345 0.106 Uiso 1 1 calc R . . H17B H 1.3245 0.2771 0.1044 0.106 Uiso 1 1 calc R . . H17C H 1.3865 0.1664 0.0941 0.106 Uiso 1 1 calc R . . C18 C 1.2282(5) 0.1288(5) 0.0866(3) 0.072(2) Uani 1 1 d . . . H18A H 1.1755 0.1296 0.0689 0.108 Uiso 1 1 calc R . . H18B H 1.2117 0.1210 0.1153 0.108 Uiso 1 1 calc R . . H18C H 1.2936 0.0758 0.0788 0.108 Uiso 1 1 calc R . . S2 S 1.00278(9) 0.36751(9) 0.21103(3) 0.0291(3) Uani 1 1 d . . . C19 C 0.8720(3) 0.4061(3) 0.21972(13) 0.0252(10) Uani 1 1 d . . . C20 C 0.8159(3) 0.3669(3) 0.20035(13) 0.0219(9) Uani 1 1 d . . . C21 C 0.7125(3) 0.4043(3) 0.20930(13) 0.0242(10) Uani 1 1 d . . . C22 C 0.6688(4) 0.4703(3) 0.24128(14) 0.0280(10) Uani 1 1 d . . . H22 H 0.5986 0.4941 0.2475 0.034 Uiso 1 1 calc R . . C23 C 0.7249(4) 0.5014(3) 0.26393(13) 0.0267(10) Uani 1 1 d . . . C24 C 0.8252(3) 0.4722(3) 0.25088(13) 0.0258(10) Uani 1 1 d . . . H24 H 0.8631 0.4985 0.2638 0.031 Uiso 1 1 calc R . . O2 O 0.8602(2) 0.2912(2) 0.17364(9) 0.0262(7) Uani 1 1 d . . . C25 C 0.9380(4) 0.2058(3) 0.19198(18) 0.0404(13) Uani 1 1 d . . . H25A H 0.9254 0.2058 0.2220 0.048 Uiso 1 1 calc R . . H25B H 1.0049 0.2040 0.1872 0.048 Uiso 1 1 calc R . . C26 C 0.9381(4) 0.1196(3) 0.17342(14) 0.0296(11) Uani 1 1 d . . . C27 C 1.0267(4) 0.0511(4) 0.15560(16) 0.0370(12) Uani 1 1 d . . . H27 H 1.0853 0.0607 0.1544 0.044 Uiso 1 1 calc R . . C28 C 1.0313(4) -0.0313(4) 0.13939(15) 0.0374(12) Uani 1 1 d . . . H28 H 1.0921 -0.0780 0.1272 0.045 Uiso 1 1 calc R . . C29 C 0.9439(4) -0.0434(4) 0.14162(15) 0.0357(12) Uani 1 1 d . . . C30 C 0.8547(4) 0.0231(4) 0.15919(17) 0.0412(13) Uani 1 1 d . . . H30 H 0.7959 0.0138 0.1604 0.049 Uiso 1 1 calc R . . C31 C 0.8537(4) 0.1059(4) 0.17534(16) 0.0372(12) Uani 1 1 d . . . H31 H 0.7933 0.1527 0.1877 0.045 Uiso 1 1 calc R . . C32 C 0.9476(5) -0.1293(4) 0.12555(17) 0.0465(15) Uani 1 1 d . . . N2 N 0.9488(5) -0.1961(4) 0.11270(18) 0.0651(16) Uani 1 1 d . . . C33 C 0.6791(4) 0.5614(4) 0.30285(15) 0.0347(12) Uani 1 1 d . . . C34 C 0.6687(6) 0.4945(5) 0.33561(19) 0.0622(18) Uani 1 1 d . . . H34A H 0.6263 0.4675 0.3251 0.093 Uiso 1 1 calc R . . H34B H 0.6372 0.5303 0.3607 0.093 Uiso 1 1 calc R . . H34C H 0.7358 0.4431 0.3419 0.093 Uiso 1 1 calc R . . C35 C 0.5707(4) 0.6416(5) 0.2947(2) 0.0524(16) Uani 1 1 d . . . H35A H 0.5738 0.6846 0.2732 0.079 Uiso 1 1 calc R . . H35B H 0.5419 0.6773 0.3201 0.079 Uiso 1 1 calc R . . H35C H 0.5280 0.6136 0.2858 0.079 Uiso 1 1 calc R . . C36 C 0.7409(5) 0.6079(6) 0.3171(2) 0.072(2) Uani 1 1 d . . . H36A H 0.8087 0.5589 0.3242 0.108 Uiso 1 1 calc R . . H36B H 0.7079 0.6465 0.3413 0.108 Uiso 1 1 calc R . . H36C H 0.7463 0.6486 0.2950 0.108 Uiso 1 1 calc R . . S3 S 0.63502(9) 0.35896(9) 0.18851(4) 0.0286(3) Uani 1 1 d . . . C37 C 0.6398(3) 0.3739(3) 0.13437(14) 0.0254(10) Uani 1 1 d . . . C38 C 0.6088(3) 0.4645(3) 0.11600(15) 0.0280(10) Uani 1 1 d . . . C39 C 0.6102(4) 0.4707(3) 0.07302(15) 0.0301(11) Uani 1 1 d . . . C40 C 0.6299(4) 0.3910(3) 0.04966(15) 0.0320(11) Uani 1 1 d . . . H40 H 0.6279 0.3972 0.0205 0.038 Uiso 1 1 calc R . . C41 C 0.6524(3) 0.3031(3) 0.06729(15) 0.0274(10) Uani 1 1 d . . . C42 C 0.6592(3) 0.2966(3) 0.11005(14) 0.0252(10) Uani 1 1 d . . . H42 H 0.6779 0.2367 0.1230 0.030 Uiso 1 1 calc R . . O3 O 0.5771(3) 0.5459(2) 0.13872(11) 0.0333(8) Uani 1 1 d . . . C43 C 0.4697(4) 0.5831(4) 0.1483(2) 0.0540(17) Uani 1 1 d . . . H43A H 0.4597 0.5461 0.1714 0.065 Uiso 1 1 calc R . . H43B H 0.4344 0.5768 0.1241 0.065 Uiso 1 1 calc R . . C44 C 0.4258(4) 0.6864(4) 0.16006(19) 0.0417(13) Uani 1 1 d . . . C45 C 0.3811(5) 0.7573(4) 0.13096(19) 0.0475(14) Uani 1 1 d . . . H45 H 0.3821 0.7412 0.1029 0.057 Uiso 1 1 calc R . . C46 C 0.3342(5) 0.8530(4) 0.1424(2) 0.0490(15) Uani 1 1 d . . . H46 H 0.3011 0.9015 0.1224 0.059 Uiso 1 1 calc R . . C47 C 0.3363(4) 0.8764(4) 0.18246(19) 0.0425(14) Uani 1 1 d . . . C48 C 0.3814(5) 0.8062(4) 0.2128(2) 0.0541(16) Uani 1 1 d . . . H48 H 0.3820 0.8222 0.2407 0.065 Uiso 1 1 calc R . . C49 C 0.4254(5) 0.7118(4) 0.2002(2) 0.0536(16) Uani 1 1 d . . . H49 H 0.4565 0.6629 0.2202 0.064 Uiso 1 1 calc R . . C50 C 0.2886(5) 0.9756(5) 0.1944(2) 0.0551(16) Uani 1 1 d . . . N3 N 0.2493(5) 1.0544(4) 0.2023(2) 0.0762(19) Uani 1 1 d . . . C51 C 0.6625(4) 0.2187(3) 0.04148(14) 0.0304(11) Uani 1 1 d . . . C52 C 0.6919(5) 0.2269(4) -0.00294(16) 0.0448(14) Uani 1 1 d . . . H52A H 0.6415 0.2869 -0.0149 0.067 Uiso 1 1 calc R . . H52B H 0.6946 0.1736 -0.0186 0.067 Uiso 1 1 calc R . . H52C H 0.7584 0.2257 -0.0041 0.067 Uiso 1 1 calc R . . C53 C 0.7428(5) 0.1238(4) 0.05922(17) 0.0423(13) Uani 1 1 d . . . H53A H 0.7461 0.0712 0.0428 0.063 Uiso 1 1 calc R . . H53B H 0.7244 0.1164 0.0878 0.063 Uiso 1 1 calc R . . H53C H 0.8090 0.1233 0.0583 0.063 Uiso 1 1 calc R . . C54 C 0.5591(4) 0.2193(5) 0.04298(19) 0.0472(15) Uani 1 1 d . . . H54A H 0.5081 0.2793 0.0313 0.071 Uiso 1 1 calc R . . H54B H 0.5403 0.2129 0.0716 0.071 Uiso 1 1 calc R . . H54C H 0.5626 0.1662 0.0270 0.071 Uiso 1 1 calc R . . S4 S 0.57035(11) 0.58006(9) 0.04626(4) 0.0405(3) Uani 1 1 d . . . C55 C 0.6494(4) 0.6296(3) 0.06127(15) 0.0301(11) Uani 1 1 d . . . C56 C 0.7552(4) 0.5782(3) 0.06252(14) 0.0280(10) Uani 1 1 d . . . C57 C 0.8118(4) 0.6262(3) 0.06928(14) 0.0275(10) Uani 1 1 d . . . C58 C 0.7642(4) 0.7244(3) 0.07411(14) 0.0301(11) Uani 1 1 d . . . H58 H 0.8037 0.7564 0.0785 0.036 Uiso 1 1 calc R . . C59 C 0.6591(4) 0.7764(3) 0.07254(15) 0.0343(12) Uani 1 1 d . . . C60 C 0.6041(4) 0.7269(3) 0.06608(15) 0.0348(12) Uani 1 1 d . . . H60 H 0.5324 0.7614 0.0649 0.042 Uiso 1 1 calc R . . O4 O 0.8019(3) 0.4805(2) 0.05979(10) 0.0299(7) Uani 1 1 d . . . C61 C 0.8393(4) 0.4417(3) 0.01970(15) 0.0382(13) Uani 1 1 d . . . H61A H 0.8832 0.4683 0.0079 0.046 Uiso 1 1 calc R . . H61B H 0.7822 0.4578 0.0010 0.046 Uiso 1 1 calc R . . C62 C 0.8984(4) 0.3362(3) 0.02468(15) 0.0295(11) Uani 1 1 d . . . C63 C 0.9542(4) 0.2807(4) -0.00839(15) 0.0351(12) Uani 1 1 d . . . H63 H 0.9567 0.3109 -0.0337 0.042 Uiso 1 1 calc R . . C64 C 1.0054(4) 0.1840(4) -0.00530(16) 0.0401(13) Uani 1 1 d . . . H64 H 1.0424 0.1473 -0.0283 0.048 Uiso 1 1 calc R . . C65 C 1.0027(4) 0.1397(3) 0.03212(16) 0.0358(12) Uani 1 1 d . . . C66 C 0.9490(4) 0.1944(4) 0.06516(16) 0.0353(12) Uani 1 1 d . . . H66 H 0.9484 0.1644 0.0907 0.042 Uiso 1 1 calc R . . C67 C 0.8964(4) 0.2912(3) 0.06161(15) 0.0322(11) Uani 1 1 d . . . H67 H 0.8584 0.3277 0.0845 0.039 Uiso 1 1 calc R . . C68 C 1.0573(5) 0.0376(4) 0.03698(18) 0.0514(16) Uani 1 1 d . . . N4 N 1.1013(5) -0.0418(4) 0.04278(19) 0.079(2) Uani 1 1 d . . . C69 C 0.6051(6) 0.8850(4) 0.0789(2) 0.0706(11) Uani 1 1 d . . . C70 C 0.6738(6) 0.9293(4) 0.0732(2) 0.0706(11) Uani 1 1 d . . . H70A H 0.7217 0.9096 0.0958 0.106 Uiso 1 1 calc R . . H70B H 0.6338 0.9987 0.0731 0.106 Uiso 1 1 calc R . . H70C H 0.7111 0.9090 0.0470 0.106 Uiso 1 1 calc R . . C71 C 0.5188(6) 0.9309(4) 0.0473(2) 0.0706(11) Uani 1 1 d . . . H71A H 0.4902 1.0002 0.0484 0.106 Uiso 1 1 calc R . . H71B H 0.4657 0.9121 0.0541 0.106 Uiso 1 1 calc R . . H71C H 0.5460 0.9093 0.0196 0.106 Uiso 1 1 calc R . . C72 C 0.5489(6) 0.9080(4) 0.1207(2) 0.0706(11) Uani 1 1 d . . . H72A H 0.5980 0.8821 0.1428 0.106 Uiso 1 1 calc R . . H72B H 0.5025 0.8797 0.1224 0.106 Uiso 1 1 calc R . . H72C H 0.5103 0.9771 0.1236 0.106 Uiso 1 1 calc R . . S5 S 0.38218(9) 0.52992(9) 0.27001(4) 0.0291(3) Uani 1 1 d . . . C73 C 0.4382(3) 0.4459(3) 0.31057(14) 0.0252(10) Uani 1 1 d . . . C74 C 0.4178(3) 0.4686(3) 0.35235(14) 0.0278(10) Uani 1 1 d . . . C75 C 0.4773(4) 0.4040(4) 0.38136(15) 0.0332(12) Uani 1 1 d . . . C76 C 0.5577(4) 0.3166(4) 0.36918(16) 0.0374(12) Uani 1 1 d . . . H76 H 0.5981 0.2727 0.3896 0.045 Uiso 1 1 calc R . . C77 C 0.5791(4) 0.2931(3) 0.32784(15) 0.0319(11) Uani 1 1 d . A . C78 C 0.5176(3) 0.3585(3) 0.29892(15) 0.0284(10) Uani 1 1 d . . . H78 H 0.5298 0.3434 0.2705 0.034 Uiso 1 1 calc R . . O5 O 0.3364(2) 0.5532(2) 0.36396(10) 0.0289(7) Uani 1 1 d . . . C79 C 0.3607(4) 0.6282(4) 0.37124(18) 0.0375(12) Uani 1 1 d . . . H79A H 0.3850 0.6459 0.3454 0.045 Uiso 1 1 calc R . . H79B H 0.4152 0.6076 0.3916 0.045 Uiso 1 1 calc R . . C80 C 0.2673(4) 0.7127(3) 0.38739(14) 0.0298(11) Uani 1 1 d . . . C81 C 0.1772(4) 0.7106(4) 0.39434(15) 0.0358(12) Uani 1 1 d . . . H81 H 0.1723 0.6542 0.3890 0.043 Uiso 1 1 calc R . . C82 C 0.0933(4) 0.7894(4) 0.40899(18) 0.0439(14) Uani 1 1 d . . . H82 H 0.0310 0.7871 0.4134 0.053 Uiso 1 1 calc R . . C83 C 0.1001(5) 0.8724(4) 0.41726(18) 0.0465(15) Uani 1 1 d . . . C84 C 0.1922(5) 0.8741(4) 0.41114(19) 0.0465(15) Uani 1 1 d . . . H84 H 0.1986 0.9294 0.4174 0.056 Uiso 1 1 calc R . . C85 C 0.2738(4) 0.7951(4) 0.39593(18) 0.0434(14) Uani 1 1 d . . . H85 H 0.3362 0.7970 0.3911 0.052 Uiso 1 1 calc R . . C86 C 0.0116(6) 0.9565(5) 0.4297(3) 0.074(2) Uani 1 1 d . . . N5 N -0.0590(6) 1.0234(6) 0.4392(4) 0.138(4) Uani 1 1 d . . . C87 C 0.6700(5) 0.1993(4) 0.3153(2) 0.0549(10) Uani 1 1 d . . . C88 C 0.7546(7) 0.2239(7) 0.2987(3) 0.0549(10) Uani 0.661(6) 1 d P A 1 H88A H 0.8166 0.1651 0.2933 0.082 Uiso 0.661(6) 1 calc PR A 1 H88B H 0.7677 0.2611 0.3192 0.082 Uiso 0.661(6) 1 calc PR A 1 H88C H 0.7327 0.2610 0.2731 0.082 Uiso 0.661(6) 1 calc PR A 1 C89 C 0.6432(7) 0.1561(6) 0.2783(3) 0.0549(10) Uani 0.661(6) 1 d P A 1 H89A H 0.6198 0.2026 0.2556 0.082 Uiso 0.661(6) 1 calc PR A 1 H89B H 0.5895 0.1392 0.2865 0.082 Uiso 0.661(6) 1 calc PR A 1 H89C H 0.7033 0.0989 0.2692 0.082 Uiso 0.661(6) 1 calc PR A 1 C90 C 0.7082(8) 0.1283(7) 0.3489(3) 0.0549(10) Uani 0.661(6) 1 d P A 1 H90A H 0.7611 0.0683 0.3381 0.082 Uiso 0.661(6) 1 calc PR A 1 H90B H 0.6525 0.1181 0.3607 0.082 Uiso 0.661(6) 1 calc PR A 1 H90C H 0.7364 0.1514 0.3703 0.082 Uiso 0.661(6) 1 calc PR A 1 C88A C 0.6365(14) 0.1208(12) 0.3188(6) 0.0549(10) Uani 0.339(6) 1 d P A 2 H88D H 0.5782 0.1371 0.3013 0.082 Uiso 0.339(6) 1 calc PR A 2 H88E H 0.6176 0.1151 0.3475 0.082 Uiso 0.339(6) 1 calc PR A 2 H88F H 0.6924 0.0603 0.3100 0.082 Uiso 0.339(6) 1 calc PR A 2 C89A C 0.7069(15) 0.1999(13) 0.2729(6) 0.0549(10) Uani 0.339(6) 1 d P A 2 H89D H 0.7680 0.1401 0.2677 0.082 Uiso 0.339(6) 1 calc PR A 2 H89E H 0.7229 0.2532 0.2691 0.082 Uiso 0.339(6) 1 calc PR A 2 H89F H 0.6546 0.2067 0.2536 0.082 Uiso 0.339(6) 1 calc PR A 2 C90A C 0.7557(14) 0.1692(13) 0.3484(6) 0.0549(10) Uani 0.339(6) 1 d P A 2 H90D H 0.8140 0.1097 0.3400 0.082 Uiso 0.339(6) 1 calc PR A 2 H90E H 0.7294 0.1599 0.3752 0.082 Uiso 0.339(6) 1 calc PR A 2 H90F H 0.7768 0.2192 0.3504 0.082 Uiso 0.339(6) 1 calc PR A 2 S6 S 0.47234(10) 0.42884(11) 0.43468(4) 0.0453(4) Uani 1 1 d . . . C91 C 0.3438(4) 0.4834(4) 0.45078(14) 0.0325(11) Uani 1 1 d . . . C92 C 0.2792(4) 0.4440(3) 0.44349(14) 0.0332(12) Uani 1 1 d . . . C93 C 0.1809(4) 0.4858(4) 0.46091(14) 0.0329(11) Uani 1 1 d . . . C94 C 0.1524(4) 0.5636(4) 0.48697(14) 0.0317(11) Uani 1 1 d . . . H94 H 0.0863 0.5915 0.4990 0.038 Uiso 1 1 calc R . . C95 C 0.2171(4) 0.6011(4) 0.49585(14) 0.0318(11) Uani 1 1 d . . . C96 C 0.3126(4) 0.5605(4) 0.47678(14) 0.0328(11) Uani 1 1 d . . . H96 H 0.3576 0.5863 0.4817 0.039 Uiso 1 1 calc R . . O6 O 0.3104(3) 0.3626(2) 0.41950(10) 0.0397(9) Uani 1 1 d . . . C97 C 0.3614(6) 0.2779(4) 0.4447(2) 0.065(2) Uani 1 1 d . . . H97A H 0.4239 0.2758 0.4555 0.078 Uiso 1 1 calc R . . H97B H 0.3170 0.2804 0.4684 0.078 Uiso 1 1 calc R . . C98 C 0.3872(8) 0.1926(6) 0.4215(3) 0.0995(11) Uani 1 1 d . . . C99 C 0.3967(8) 0.1864(6) 0.3792(3) 0.0995(11) Uani 1 1 d . . . H99 H 0.3875 0.2404 0.3630 0.119 Uiso 1 1 calc R . . C100 C 0.4200(8) 0.0997(6) 0.3599(3) 0.0995(11) Uani 1 1 d . . . H100 H 0.4308 0.0937 0.3310 0.119 Uiso 1 1 calc R . . C101 C 0.4270(8) 0.0209(6) 0.3846(3) 0.0995(11) Uani 1 1 d . . . C102 C 0.4120(8) 0.0285(6) 0.4270(3) 0.0995(11) Uani 1 1 d . . . H102 H 0.4168 -0.0240 0.4433 0.119 Uiso 1 1 calc R . . C103 C 0.3904(8) 0.1125(6) 0.4447(3) 0.0995(11) Uani 1 1 d . . . H103 H 0.3769 0.1189 0.4735 0.119 Uiso 1 1 calc R . . C104 C 0.4457(8) -0.0676(6) 0.3677(3) 0.0995(11) Uani 1 1 d . . . N6 N 0.4581(6) -0.1389(5) 0.3532(2) 0.0995(11) Uani 1 1 d . . . C105 C 0.1873(4) 0.6825(4) 0.52683(15) 0.0351(12) Uani 1 1 d . . . C106 C 0.2438(5) 0.7418(4) 0.51758(19) 0.0476(14) Uani 1 1 d . . . H10A H 0.3164 0.7021 0.5216 0.071 Uiso 1 1 calc R . . H10B H 0.2186 0.7960 0.5362 0.071 Uiso 1 1 calc R . . H10C H 0.2323 0.7649 0.4891 0.071 Uiso 1 1 calc R . . C107 C 0.2177(6) 0.6376(5) 0.56957(18) 0.0621(19) Uani 1 1 d . . . H10D H 0.2909 0.5964 0.5698 0.093 Uiso 1 1 calc R . . H10E H 0.1822 0.5998 0.5763 0.093 Uiso 1 1 calc R . . H10F H 0.1994 0.6877 0.5900 0.093 Uiso 1 1 calc R . . C108 C 0.0732(4) 0.7494(5) 0.5262(2) 0.0515(16) Uani 1 1 d . . . H10G H 0.0581 0.8059 0.5425 0.077 Uiso 1 1 calc R . . H10H H 0.0363 0.7165 0.5380 0.077 Uiso 1 1 calc R . . H10I H 0.0524 0.7686 0.4978 0.077 Uiso 1 1 calc R . . S7 S 0.09859(13) 0.43402(13) 0.45754(4) 0.0518(4) Uani 1 1 d . . . C109 C 0.0448(3) 0.4737(3) 0.33536(15) 0.0294(11) Uani 1 1 d . . . C110 C 0.0538(4) 0.4920(4) 0.37641(16) 0.0324(11) Uani 1 1 d . . . C111 C 0.0898(4) 0.4166(4) 0.40414(15) 0.0354(12) Uani 1 1 d . . . C112 C 0.1068(4) 0.3284(4) 0.39242(16) 0.0382(12) Uani 1 1 d . . . H112 H 0.1327 0.2778 0.4120 0.046 Uiso 1 1 calc R . . C113 C 0.0877(4) 0.3090(4) 0.35266(15) 0.0347(12) Uani 1 1 d . . . C114 C 0.0604(4) 0.3834(4) 0.32412(16) 0.0351(12) Uani 1 1 d . . . H114 H 0.0523 0.3722 0.2962 0.042 Uiso 1 1 calc R . . O7 O 0.0227(3) 0.5845(3) 0.38937(13) 0.0490(9) Uani 1 1 d . . . C115 C -0.0831(4) 0.6224(4) 0.4026(2) 0.0490(9) Uani 1 1 d . . . H11A H -0.0888 0.5852 0.4266 0.059 Uiso 1 1 calc R . . H11B H -0.1232 0.6165 0.3801 0.059 Uiso 1 1 calc R . . C116 C -0.1237(3) 0.7234(2) 0.41400(13) 0.0413(13) Uani 1 1 d G . . C117 C -0.1240(3) 0.7462(4) 0.45504(11) 0.0614(18) Uani 1 1 d G . . H117 H -0.0911 0.6972 0.4748 0.074 Uiso 1 1 calc R . . C118 C -0.1725(4) 0.8406(5) 0.46711(16) 0.090(3) Uani 1 1 d G . . H118 H -0.1726 0.8562 0.4952 0.108 Uiso 1 1 calc R . . C119 C -0.2206(5) 0.9122(3) 0.4381(3) 0.108(4) Uani 1 1 d G . . C120 C -0.2204(5) 0.8894(3) 0.3971(2) 0.138(6) Uani 1 1 d G . . H120 H -0.2533 0.9384 0.3773 0.166 Uiso 1 1 calc R . . C121 C -0.1719(4) 0.7950(4) 0.38503(11) 0.089(3) Uani 1 1 d G . . H121 H -0.1717 0.7795 0.3570 0.107 Uiso 1 1 calc R . . C122 C -0.2877(9) 1.0142(8) 0.4432(5) 0.130(5) Uani 1 1 d . . . N7 N -0.3389(9) 1.0912(8) 0.4506(5) 0.168(5) Uani 1 1 d . . . C123 C 0.0929(4) 0.2139(4) 0.34014(17) 0.0416(13) Uani 1 1 d . . . C124 C 0.1643(5) 0.1727(4) 0.30298(19) 0.0518(16) Uani 1 1 d . . . H12A H 0.2323 0.1626 0.3099 0.078 Uiso 1 1 calc R . . H12B H 0.1396 0.2171 0.2797 0.078 Uiso 1 1 calc R . . H12C H 0.1669 0.1119 0.2956 0.078 Uiso 1 1 calc R . . C125 C -0.0143(5) 0.2323(5) 0.3288(2) 0.0603(18) Uani 1 1 d . . . H12D H -0.0128 0.1727 0.3203 0.091 Uiso 1 1 calc R . . H12E H -0.0386 0.2787 0.3062 0.091 Uiso 1 1 calc R . . H12F H -0.0598 0.2571 0.3528 0.091 Uiso 1 1 calc R . . C126 C 0.1304(6) 0.1413(4) 0.37503(19) 0.0576(18) Uani 1 1 d . . . H12G H 0.1968 0.1326 0.3836 0.086 Uiso 1 1 calc R . . H12H H 0.1363 0.0806 0.3656 0.086 Uiso 1 1 calc R . . H12I H 0.0823 0.1639 0.3984 0.086 Uiso 1 1 calc R . . S8 S -0.00381(10) 0.56723(9) 0.29785(4) 0.0379(3) Uani 1 1 d . . . C127 C 0.0846(4) 0.6127(3) 0.29452(14) 0.0283(10) Uani 1 1 d . . . C128 C 0.1878(3) 0.5560(3) 0.28656(14) 0.0259(10) Uani 1 1 d . . . C129 C 0.2516(3) 0.5983(3) 0.28250(13) 0.0252(10) Uani 1 1 d . . . C130 C 0.2120(4) 0.6966(3) 0.28219(14) 0.0276(10) Uani 1 1 d . . . H130 H 0.2566 0.7242 0.2787 0.033 Uiso 1 1 calc R . . C131 C 0.1082(4) 0.7558(3) 0.28693(14) 0.0286(11) Uani 1 1 d . . . C132 C 0.0468(4) 0.7114(3) 0.29450(15) 0.0297(11) Uani 1 1 d . . . H132 H -0.0234 0.7499 0.2998 0.036 Uiso 1 1 calc R . . O8 O 0.2277(2) 0.4587(2) 0.28232(10) 0.0316(8) Uani 1 1 d . . . C133 C 0.2075(5) 0.4332(4) 0.2422(2) 0.0540(17) Uani 1 1 d . . . H13A H 0.1901 0.4871 0.2226 0.065 Uiso 1 1 calc R . . H13B H 0.1496 0.4185 0.2443 0.065 Uiso 1 1 calc R . . C134 C 0.2997(4) 0.3484(4) 0.22694(17) 0.0408(13) Uani 1 1 d . . . C135 C 0.3165(5) 0.2594(5) 0.2384(2) 0.069(2) Uani 1 1 d . . . H135 H 0.2685 0.2523 0.2562 0.083 Uiso 1 1 calc R . . C136 C 0.3995(6) 0.1801(5) 0.2255(3) 0.080(2) Uani 1 1 d . . . H136 H 0.4101 0.1189 0.2346 0.095 Uiso 1 1 calc R . . C137 C 0.4676(5) 0.1904(7) 0.1990(3) 0.071(2) Uani 1 1 d . . . C138 C 0.4513(6) 0.2776(8) 0.1856(2) 0.081(3) Uani 1 1 d . . . H138 H 0.4980 0.2839 0.1668 0.097 Uiso 1 1 calc R . . C139 C 0.3671(6) 0.3576(6) 0.1992(2) 0.0616(19) Uani 1 1 d . . . H139 H 0.3555 0.4188 0.1895 0.074 Uiso 1 1 calc R . . C140 C 0.5580(6) 0.1069(8) 0.1863(4) 0.121(5) Uani 1 1 d . . . N8 N 0.6323(5) 0.0354(5) 0.1794(2) 0.0767(15) Uani 1 1 d . . . C141 C 0.0641(6) 0.8627(6) 0.2825(3) 0.0767(15) Uani 1 1 d . . . C142 C 0.1378(7) 0.8998(5) 0.2964(4) 0.092(3) Uani 1 1 d . . . H14A H 0.1928 0.8832 0.2759 0.138 Uiso 1 1 calc R . . H14B H 0.1661 0.8708 0.3229 0.138 Uiso 1 1 calc R . . H14C H 0.1014 0.9690 0.2991 0.138 Uiso 1 1 calc R . . C143 C 0.0467(7) 0.8853(5) 0.2370(4) 0.100 Uani 1 1 d . . . H14D H 0.1115 0.8552 0.2219 0.150 Uiso 1 1 calc R . . H14E H 0.0158 0.9543 0.2327 0.150 Uiso 1 1 calc R . . H14F H 0.0014 0.8611 0.2271 0.150 Uiso 1 1 calc R . . C144 C -0.0330(7) 0.9137(5) 0.3088(4) 0.107(4) Uani 1 1 d . . . H14G H -0.0464 0.9795 0.3132 0.160 Uiso 1 1 calc R . . H14H H -0.0247 0.8809 0.3354 0.160 Uiso 1 1 calc R . . H14I H -0.0900 0.9134 0.2945 0.160 Uiso 1 1 calc R . . C145 C 0.1657(6) 0.6259(5) 0.1208(2) 0.0674(19) Uani 1 1 d . . . H145 H 0.0915 0.6583 0.1154 0.081 Uiso 1 1 calc R . . Cl1 Cl 0.2245(3) 0.6698(3) 0.08567(8) 0.1473(15) Uani 1 1 d . . . Cl2 Cl 0.2087(2) 0.50410(17) 0.11602(9) 0.1117(9) Uani 1 1 d . . . Cl3 Cl 0.1825(2) 0.65279(16) 0.17068(6) 0.0901(7) Uani 1 1 d . . . Cl4 Cl 0.5437(4) 0.2028(4) 0.53040(17) 0.0785(19) Uani 0.542(11) 1 d PD B 1 Cl5 Cl 0.3442(6) 0.2608(10) 0.5632(2) 0.140(5) Uani 0.542(11) 1 d PD B 1 Cl6 Cl 0.4331(6) 0.3894(4) 0.55317(14) 0.105(2) Uani 0.542(11) 1 d PD B 1 Cl4A Cl 0.3399(16) 0.3866(7) 0.5547(3) 0.224(10) Uani 0.458(11) 1 d PD B 2 Cl5A Cl 0.5251(11) 0.2537(19) 0.5332(4) 0.280(14) Uani 0.458(11) 1 d PD B 2 Cl6A Cl 0.3793(13) 0.2128(14) 0.5608(7) 0.221(9) Uani 0.458(11) 1 d PD B 2 C146 C 0.4448(7) 0.2800(6) 0.5658(3) 0.105(3) Uani 1 1 d D . . H146 H 0.4712 0.2640 0.5944 0.126 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0370(7) 0.0233(7) 0.0446(7) 0.0072(5) 0.0071(5) -0.0175(6) C1 0.024(2) 0.022(2) 0.036(3) 0.0020(19) 0.0003(19) -0.012(2) C2 0.024(2) 0.022(2) 0.032(2) -0.0047(19) 0.0067(18) -0.0154(19) C3 0.024(2) 0.020(2) 0.029(2) -0.0071(18) 0.0067(18) -0.0135(19) C4 0.028(2) 0.024(3) 0.032(2) -0.0022(19) 0.0009(19) -0.013(2) C5 0.030(2) 0.022(2) 0.029(2) -0.0063(19) 0.0073(19) -0.014(2) C6 0.031(3) 0.024(3) 0.032(2) -0.0019(19) 0.0075(19) -0.015(2) O1 0.0281(17) 0.0193(17) 0.0369(18) -0.0055(13) 0.0074(14) -0.0107(14) C7 0.042(3) 0.023(3) 0.059(3) -0.014(2) 0.005(3) -0.018(2) C8 0.053(3) 0.017(3) 0.039(3) -0.003(2) 0.007(2) -0.007(2) C9 0.051(4) 0.031(3) 0.061(4) 0.004(3) 0.020(3) -0.008(3) C10 0.055(4) 0.047(4) 0.070(5) 0.011(3) 0.026(3) 0.003(3) C11 0.103(7) 0.026(4) 0.067(5) -0.012(3) 0.037(4) -0.006(4) C12 0.123(8) 0.038(4) 0.069(5) -0.026(4) 0.002(5) -0.007(5) C13 0.084(5) 0.034(3) 0.063(4) -0.017(3) -0.001(4) -0.017(3) C14 0.113 0.029 0.068 0.000 0.038 0.000 N1 0.113 0.029 0.068 0.000 0.038 0.000 C15 0.037(3) 0.031(3) 0.035(3) -0.006(2) 0.010(2) -0.008(2) C16 0.090(6) 0.080(6) 0.063(5) -0.001(4) 0.044(4) 0.029(5) C17 0.027(3) 0.071(5) 0.106(6) -0.034(4) 0.011(3) -0.014(3) C18 0.057(4) 0.048(4) 0.105(6) -0.038(4) 0.020(4) -0.017(3) S2 0.0265(6) 0.0366(7) 0.0271(6) -0.0037(5) 0.0041(5) -0.0171(5) C19 0.030(2) 0.024(2) 0.023(2) -0.0015(18) 0.0037(18) -0.013(2) C20 0.030(2) 0.016(2) 0.022(2) -0.0012(16) 0.0046(17) -0.0129(19) C21 0.031(2) 0.017(2) 0.028(2) 0.0012(17) 0.0030(18) -0.014(2) C22 0.028(2) 0.027(3) 0.032(2) -0.0044(19) 0.0080(19) -0.015(2) C23 0.034(3) 0.027(3) 0.025(2) -0.0065(19) 0.0094(19) -0.019(2) C24 0.032(2) 0.030(3) 0.023(2) -0.0054(18) 0.0041(18) -0.020(2) O2 0.0308(17) 0.0190(16) 0.0260(16) -0.0020(12) 0.0022(13) -0.0091(14) C25 0.049(3) 0.021(3) 0.050(3) 0.005(2) -0.018(3) -0.014(2) C26 0.034(3) 0.020(2) 0.030(2) 0.0053(19) -0.006(2) -0.008(2) C27 0.042(3) 0.037(3) 0.040(3) 0.005(2) -0.002(2) -0.025(3) C28 0.042(3) 0.027(3) 0.036(3) -0.004(2) 0.008(2) -0.011(2) C29 0.051(3) 0.023(3) 0.031(3) 0.003(2) -0.010(2) -0.016(2) C30 0.044(3) 0.035(3) 0.049(3) 0.005(2) -0.009(2) -0.021(3) C31 0.032(3) 0.027(3) 0.044(3) 0.005(2) 0.001(2) -0.006(2) C32 0.071(4) 0.028(3) 0.043(3) 0.004(2) -0.013(3) -0.025(3) N2 0.093(4) 0.045(3) 0.066(4) -0.006(3) -0.013(3) -0.038(3) C33 0.045(3) 0.038(3) 0.028(2) -0.011(2) 0.010(2) -0.026(3) C34 0.075(5) 0.072(5) 0.041(3) -0.013(3) 0.016(3) -0.034(4) C35 0.046(3) 0.057(4) 0.055(4) -0.021(3) 0.014(3) -0.024(3) C36 0.058(4) 0.108(6) 0.071(4) -0.063(4) 0.029(3) -0.055(4) S3 0.0342(6) 0.0278(7) 0.0321(6) -0.0023(5) 0.0051(5) -0.0216(5) C37 0.024(2) 0.022(2) 0.035(2) 0.0022(19) 0.0020(18) -0.015(2) C38 0.024(2) 0.017(2) 0.046(3) -0.001(2) -0.002(2) -0.0119(19) C39 0.031(3) 0.022(3) 0.041(3) 0.005(2) -0.009(2) -0.015(2) C40 0.035(3) 0.028(3) 0.036(3) 0.005(2) -0.006(2) -0.017(2) C41 0.027(2) 0.022(2) 0.039(3) -0.001(2) -0.0010(19) -0.017(2) C42 0.026(2) 0.017(2) 0.036(3) 0.0037(18) -0.0012(19) -0.0134(19) O3 0.0369(19) 0.0177(17) 0.048(2) -0.0035(14) 0.0017(15) -0.0151(15) C43 0.037(3) 0.026(3) 0.102(5) -0.011(3) 0.011(3) -0.018(3) C44 0.033(3) 0.027(3) 0.065(4) -0.005(3) 0.009(3) -0.013(2) C45 0.058(4) 0.036(3) 0.055(4) -0.009(3) 0.005(3) -0.026(3) C46 0.055(4) 0.028(3) 0.062(4) 0.006(3) 0.004(3) -0.018(3) C47 0.038(3) 0.022(3) 0.064(4) -0.008(2) 0.009(3) -0.011(2) C48 0.055(4) 0.039(4) 0.058(4) -0.004(3) 0.001(3) -0.013(3) C49 0.057(4) 0.027(3) 0.076(5) 0.017(3) -0.011(3) -0.018(3) C50 0.050(4) 0.037(4) 0.072(4) -0.006(3) -0.001(3) -0.014(3) N3 0.082(4) 0.036(3) 0.099(5) -0.014(3) -0.009(4) -0.016(3) C51 0.038(3) 0.026(3) 0.031(2) -0.004(2) -0.002(2) -0.017(2) C52 0.058(4) 0.034(3) 0.036(3) -0.005(2) 0.005(2) -0.015(3) C53 0.063(4) 0.023(3) 0.047(3) -0.001(2) -0.008(3) -0.024(3) C54 0.044(3) 0.053(4) 0.055(3) -0.017(3) 0.002(3) -0.030(3) S4 0.0483(8) 0.0273(7) 0.0553(8) 0.0181(6) -0.0195(6) -0.0252(6) C55 0.038(3) 0.019(2) 0.039(3) 0.007(2) -0.003(2) -0.018(2) C56 0.043(3) 0.014(2) 0.033(3) 0.0066(18) -0.001(2) -0.018(2) C57 0.040(3) 0.021(2) 0.028(2) 0.0056(18) 0.004(2) -0.020(2) C58 0.042(3) 0.021(3) 0.033(3) 0.0045(19) -0.002(2) -0.020(2) C59 0.054(3) 0.018(2) 0.031(3) 0.0016(19) 0.008(2) -0.017(2) C60 0.044(3) 0.020(3) 0.042(3) 0.008(2) -0.001(2) -0.016(2) O4 0.0411(19) 0.0126(16) 0.0360(18) -0.0016(13) 0.0042(14) -0.0124(14) C61 0.058(3) 0.021(3) 0.034(3) 0.001(2) 0.000(2) -0.016(2) C62 0.038(3) 0.019(2) 0.038(3) 0.001(2) 0.000(2) -0.019(2) C63 0.055(3) 0.027(3) 0.033(3) -0.005(2) 0.009(2) -0.028(3) C64 0.059(3) 0.035(3) 0.034(3) -0.011(2) 0.014(2) -0.028(3) C65 0.044(3) 0.017(2) 0.047(3) -0.006(2) 0.006(2) -0.015(2) C66 0.045(3) 0.025(3) 0.035(3) 0.003(2) 0.004(2) -0.016(2) C67 0.044(3) 0.024(3) 0.028(2) -0.0043(19) 0.004(2) -0.016(2) C68 0.066(4) 0.028(3) 0.048(3) -0.011(3) 0.020(3) -0.012(3) N4 0.106(5) 0.029(3) 0.071(4) -0.005(3) 0.032(3) -0.006(3) C69 0.093(3) 0.0212(16) 0.091(3) -0.0045(15) 0.016(2) -0.0212(17) C70 0.093(3) 0.0212(16) 0.091(3) -0.0045(15) 0.016(2) -0.0212(17) C71 0.093(3) 0.0212(16) 0.091(3) -0.0045(15) 0.016(2) -0.0212(17) C72 0.093(3) 0.0212(16) 0.091(3) -0.0045(15) 0.016(2) -0.0212(17) S5 0.0267(6) 0.0262(6) 0.0338(6) 0.0031(5) 0.0045(5) -0.0119(5) C73 0.023(2) 0.021(2) 0.034(2) 0.0004(19) 0.0038(18) -0.0127(19) C74 0.022(2) 0.024(3) 0.035(3) -0.0027(19) 0.0037(19) -0.0081(19) C75 0.024(2) 0.038(3) 0.031(3) 0.000(2) 0.0050(19) -0.009(2) C76 0.030(3) 0.033(3) 0.040(3) 0.005(2) 0.001(2) -0.006(2) C77 0.026(2) 0.027(3) 0.037(3) 0.000(2) 0.009(2) -0.007(2) C78 0.029(2) 0.021(2) 0.035(3) -0.0024(19) 0.009(2) -0.012(2) O5 0.0242(16) 0.0216(17) 0.0351(18) -0.0057(13) 0.0041(13) -0.0057(14) C79 0.034(3) 0.032(3) 0.051(3) -0.007(2) 0.004(2) -0.020(2) C80 0.035(3) 0.026(3) 0.028(2) -0.0017(19) -0.003(2) -0.014(2) C81 0.041(3) 0.026(3) 0.039(3) -0.006(2) 0.005(2) -0.013(2) C82 0.042(3) 0.029(3) 0.056(3) -0.009(2) 0.011(3) -0.012(2) C83 0.053(4) 0.026(3) 0.049(3) -0.010(2) 0.001(3) -0.008(3) C84 0.055(4) 0.026(3) 0.062(4) -0.011(3) -0.005(3) -0.021(3) C85 0.047(3) 0.035(3) 0.053(3) -0.005(3) -0.003(3) -0.024(3) C86 0.060(4) 0.045(4) 0.112(6) -0.032(4) 0.009(4) -0.018(4) N5 0.077(5) 0.064(5) 0.253(12) -0.083(6) 0.022(6) -0.012(4) C87 0.047(2) 0.033(2) 0.066(2) -0.0028(17) 0.0140(18) -0.0030(16) C88 0.047(2) 0.033(2) 0.066(2) -0.0028(17) 0.0140(18) -0.0030(16) C89 0.047(2) 0.033(2) 0.066(2) -0.0028(17) 0.0140(18) -0.0030(16) C90 0.047(2) 0.033(2) 0.066(2) -0.0028(17) 0.0140(18) -0.0030(16) C88A 0.047(2) 0.033(2) 0.066(2) -0.0028(17) 0.0140(18) -0.0030(16) C89A 0.047(2) 0.033(2) 0.066(2) -0.0028(17) 0.0140(18) -0.0030(16) C90A 0.047(2) 0.033(2) 0.066(2) -0.0028(17) 0.0140(18) -0.0030(16) S6 0.0307(7) 0.0592(10) 0.0303(7) -0.0061(6) -0.0005(5) -0.0068(6) C91 0.033(3) 0.033(3) 0.025(2) 0.002(2) 0.002(2) -0.011(2) C92 0.050(3) 0.021(3) 0.026(2) -0.0002(19) 0.004(2) -0.015(2) C93 0.050(3) 0.028(3) 0.026(2) -0.001(2) 0.009(2) -0.024(2) C94 0.034(3) 0.036(3) 0.025(2) -0.004(2) 0.005(2) -0.017(2) C95 0.039(3) 0.030(3) 0.023(2) 0.0011(19) -0.001(2) -0.013(2) C96 0.034(3) 0.037(3) 0.025(2) -0.002(2) 0.000(2) -0.015(2) O6 0.055(2) 0.029(2) 0.0325(19) -0.0101(15) 0.0046(16) -0.0162(17) C97 0.099(6) 0.028(3) 0.059(4) 0.007(3) -0.002(4) -0.021(3) C98 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) C99 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) C100 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) C101 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) C102 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) C103 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) C104 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) N6 0.125(3) 0.0515(17) 0.112(3) -0.0207(17) 0.033(2) -0.0325(19) C105 0.043(3) 0.035(3) 0.028(2) -0.005(2) 0.003(2) -0.019(2) C106 0.050(3) 0.044(4) 0.052(3) -0.011(3) 0.006(3) -0.024(3) C107 0.095(5) 0.057(4) 0.032(3) -0.009(3) 0.003(3) -0.033(4) C108 0.045(3) 0.052(4) 0.057(4) -0.021(3) 0.010(3) -0.021(3) S7 0.0816(11) 0.0711(11) 0.0318(7) -0.0118(7) 0.0184(7) -0.0606(10) C109 0.025(2) 0.023(3) 0.047(3) 0.000(2) 0.005(2) -0.017(2) C110 0.035(3) 0.027(3) 0.045(3) -0.012(2) 0.010(2) -0.022(2) C111 0.047(3) 0.039(3) 0.033(3) -0.009(2) 0.011(2) -0.031(3) C112 0.049(3) 0.033(3) 0.040(3) 0.000(2) 0.010(2) -0.026(3) C113 0.044(3) 0.026(3) 0.037(3) -0.001(2) 0.012(2) -0.019(2) C114 0.041(3) 0.034(3) 0.035(3) -0.003(2) 0.004(2) -0.022(2) O7 0.0399(17) 0.0386(19) 0.077(2) -0.0214(16) 0.0175(16) -0.0253(15) C115 0.0399(17) 0.0386(19) 0.077(2) -0.0214(16) 0.0175(16) -0.0253(15) C116 0.038(3) 0.037(3) 0.052(3) -0.010(3) 0.013(2) -0.019(3) C117 0.045(4) 0.078(5) 0.064(4) 0.012(4) -0.006(3) -0.031(4) C118 0.064(5) 0.144(9) 0.086(6) -0.073(6) 0.037(4) -0.066(6) C119 0.091(7) 0.048(5) 0.196(12) -0.061(6) 0.066(7) -0.042(5) C120 0.124(9) 0.043(5) 0.195(12) 0.039(6) 0.080(9) 0.001(5) C121 0.082(6) 0.090(6) 0.059(5) 0.021(4) 0.021(4) -0.011(5) C122 0.115(8) 0.053(6) 0.215(13) -0.044(7) 0.066(8) -0.032(6) N7 0.147(9) 0.078(7) 0.272(15) -0.050(8) 0.057(9) -0.046(7) C123 0.055(3) 0.031(3) 0.044(3) -0.006(2) 0.012(3) -0.025(3) C124 0.076(4) 0.030(3) 0.052(4) -0.007(3) 0.018(3) -0.027(3) C125 0.063(4) 0.043(4) 0.090(5) -0.011(3) 0.008(4) -0.037(3) C126 0.096(5) 0.028(3) 0.056(4) 0.001(3) 0.017(3) -0.036(3) S8 0.0315(7) 0.0305(7) 0.0593(9) 0.0112(6) -0.0081(6) -0.0211(6) C127 0.031(3) 0.026(3) 0.033(3) 0.0061(19) -0.0044(19) -0.018(2) C128 0.029(2) 0.018(2) 0.033(2) 0.0045(18) -0.0007(19) -0.013(2) C129 0.025(2) 0.025(3) 0.025(2) 0.0044(18) -0.0008(18) -0.012(2) C130 0.035(3) 0.020(2) 0.036(3) 0.0026(19) 0.001(2) -0.020(2) C131 0.034(3) 0.020(2) 0.030(2) 0.0023(19) -0.0024(19) -0.011(2) C132 0.022(2) 0.024(3) 0.042(3) 0.005(2) -0.0017(19) -0.010(2) O8 0.0362(19) 0.0193(17) 0.043(2) 0.0012(14) -0.0055(15) -0.0158(15) C133 0.055(4) 0.037(3) 0.060(4) -0.012(3) -0.017(3) -0.012(3) C134 0.048(3) 0.034(3) 0.049(3) -0.009(2) 0.007(3) -0.026(3) C135 0.061(4) 0.035(4) 0.105(6) 0.005(3) 0.043(4) -0.019(3) C136 0.067(5) 0.038(4) 0.118(7) -0.009(4) 0.035(4) -0.012(4) C137 0.042(4) 0.087(6) 0.096(6) -0.055(5) 0.025(4) -0.038(4) C138 0.076(5) 0.136(8) 0.072(5) -0.070(5) 0.047(4) -0.084(6) C139 0.099(5) 0.072(5) 0.051(4) -0.013(3) 0.011(4) -0.071(5) C140 0.051(5) 0.134(9) 0.180(10) -0.120(8) 0.044(5) -0.043(5) N8 0.057(3) 0.070(3) 0.100(4) -0.031(3) 0.014(3) -0.026(3) C141 0.057(3) 0.070(3) 0.100(4) -0.031(3) 0.014(3) -0.026(3) C142 0.080(6) 0.025(4) 0.172(9) -0.004(4) -0.019(6) -0.024(4) C143 0.081 0.027 0.164 0.002 0.000 0.000 C144 0.089(6) 0.032(4) 0.163(9) 0.004(5) 0.059(6) 0.000(4) C145 0.074(5) 0.065(5) 0.076(5) 0.011(4) -0.015(4) -0.044(4) Cl1 0.168(3) 0.279(4) 0.0892(17) 0.072(2) -0.0468(17) -0.184(3) Cl2 0.125(2) 0.0720(15) 0.135(2) -0.0226(14) -0.0300(17) -0.0398(14) Cl3 0.1344(19) 0.0754(14) 0.0706(12) 0.0019(10) -0.0219(12) -0.0557(14) Cl4 0.049(2) 0.102(4) 0.062(3) -0.007(2) -0.0005(18) -0.015(3) Cl5 0.073(4) 0.268(13) 0.104(5) -0.071(7) 0.030(4) -0.100(6) Cl6 0.134(6) 0.100(4) 0.061(3) -0.017(2) 0.017(3) -0.038(4) Cl4A 0.30(2) 0.132(8) 0.097(6) 0.007(5) -0.011(8) 0.019(10) Cl5A 0.246(17) 0.57(4) 0.171(12) 0.168(19) -0.063(12) -0.32(2) Cl6A 0.140(12) 0.264(19) 0.303(19) 0.111(14) -0.052(11) -0.134(14) C146 0.112(8) 0.122(9) 0.076(6) -0.010(6) -0.002(5) -0.049(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.768(5) . ? S1 C57 1.780(5) . ? C1 C2 1.386(6) . ? C1 C6 1.399(6) . ? C2 O1 1.386(5) . ? C2 C3 1.398(6) . ? C3 C4 1.396(6) . ? C3 S2 1.779(5) . ? C4 C5 1.397(6) . ? C4 H4 0.9500 . ? C5 C6 1.390(7) . ? C5 C15 1.541(6) . ? C6 H6 0.9500 . ? O1 C7 1.435(6) . ? C7 C8 1.484(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.396(9) . ? C8 C13 1.402(9) . ? C9 C10 1.394(8) . ? C9 H9 0.9500 . ? C10 C11 1.392(13) . ? C10 H10 0.9500 . ? C11 C12 1.352(13) . ? C11 C14 1.456(9) . ? C12 C13 1.382(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 N1 1.136(8) . ? C15 C16 1.512(9) . ? C15 C18 1.525(10) . ? C15 C17 1.526(9) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? S2 C19 1.766(5) . ? C19 C24 1.396(6) . ? C19 C20 1.414(6) . ? C20 O2 1.385(5) . ? C20 C21 1.395(6) . ? C21 C22 1.409(6) . ? C21 S3 1.767(5) . ? C22 C23 1.382(7) . ? C22 H22 0.9500 . ? C23 C24 1.399(6) . ? C23 C33 1.543(6) . ? C24 H24 0.9500 . ? O2 C25 1.446(6) . ? C25 C26 1.504(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C31 1.368(8) . ? C26 C27 1.386(7) . ? C27 C28 1.390(7) . ? C27 H27 0.9500 . ? C28 C29 1.397(8) . ? C28 H28 0.9500 . ? C29 C30 1.378(8) . ? C29 C32 1.446(8) . ? C30 C31 1.416(8) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 N2 1.138(7) . ? C33 C36 1.503(8) . ? C33 C34 1.540(9) . ? C33 C35 1.554(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? S3 C37 1.775(5) . ? C37 C42 1.384(6) . ? C37 C38 1.413(7) . ? C38 O3 1.378(5) . ? C38 C39 1.399(7) . ? C39 C40 1.396(7) . ? C39 S4 1.768(5) . ? C40 C41 1.388(7) . ? C40 H40 0.9500 . ? C41 C42 1.395(6) . ? C41 C51 1.541(6) . ? C42 H42 0.9500 . ? O3 C43 1.453(7) . ? C43 C44 1.512(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C49 1.373(9) . ? C44 C45 1.379(8) . ? C45 C46 1.401(8) . ? C45 H45 0.9500 . ? C46 C47 1.369(8) . ? C46 H46 0.9500 . ? C47 C48 1.401(9) . ? C47 C50 1.452(8) . ? C48 C49 1.397(9) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 N3 1.142(8) . ? C51 C52 1.517(7) . ? C51 C54 1.533(8) . ? C51 C53 1.541(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? S4 C55 1.770(5) . ? C55 C60 1.380(7) . ? C55 C56 1.402(7) . ? C56 O4 1.379(5) . ? C56 C57 1.392(7) . ? C57 C58 1.393(7) . ? C58 C59 1.394(7) . ? C58 H58 0.9500 . ? C59 C60 1.389(8) . ? C59 C69 1.545(8) . ? C60 H60 0.9500 . ? O4 C61 1.438(6) . ? C61 C62 1.496(7) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C67 1.389(7) . ? C62 C63 1.394(7) . ? C63 C64 1.365(7) . ? C63 H63 0.9500 . ? C64 C65 1.399(8) . ? C64 H64 0.9500 . ? C65 C66 1.379(7) . ? C65 C68 1.447(8) . ? C66 C67 1.368(7) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 N4 1.134(7) . ? C69 C70 1.486(12) . ? C69 C72 1.535(10) . ? C69 C71 1.555(11) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? S5 C129 1.776(5) . ? S5 C73 1.780(5) . ? C73 C78 1.399(6) . ? C73 C74 1.402(6) . ? C74 C75 1.376(7) . ? C74 O5 1.383(5) . ? C75 C76 1.408(7) . ? C75 S6 1.779(5) . ? C76 C77 1.392(7) . ? C76 H76 0.9500 . ? C77 C78 1.389(7) . ? C77 C87 1.535(7) . ? C78 H78 0.9500 . ? O5 C79 1.418(6) . ? C79 C80 1.511(7) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.367(7) . ? C80 C85 1.386(7) . ? C81 C82 1.381(7) . ? C81 H81 0.9500 . ? C82 C83 1.397(8) . ? C82 H82 0.9500 . ? C83 C84 1.390(9) . ? C83 C86 1.434(9) . ? C84 C85 1.372(8) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C86 N5 1.138(9) . ? C87 C89A 1.47(2) . ? C87 C90 1.477(12) . ? C87 C88A 1.54(2) . ? C87 C89 1.547(12) . ? C87 C88 1.556(13) . ? C87 C90A 1.58(2) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C88A H88D 0.9800 . ? C88A H88E 0.9800 . ? C88A H88F 0.9800 . ? C89A H89D 0.9800 . ? C89A H89E 0.9800 . ? C89A H89F 0.9800 . ? C90A H90D 0.9800 . ? C90A H90E 0.9800 . ? C90A H90F 0.9800 . ? S6 C91 1.767(5) . ? C91 C96 1.388(7) . ? C91 C92 1.391(8) . ? C92 O6 1.401(6) . ? C92 C93 1.405(7) . ? C93 C94 1.402(7) . ? C93 S7 1.764(6) . ? C94 C95 1.381(7) . ? C94 H94 0.9500 . ? C95 C96 1.393(7) . ? C95 C105 1.544(7) . ? C96 H96 0.9500 . ? O6 C97 1.447(7) . ? C97 C98 1.446(11) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.382(13) . ? C98 C103 1.443(14) . ? C99 C100 1.409(12) . ? C99 H99 0.9500 . ? C100 C101 1.431(14) . ? C100 H100 0.9500 . ? C101 C102 1.392(13) . ? C101 C104 1.419(12) . ? C102 C103 1.355(12) . ? C102 H102 0.9500 . ? C103 H103 0.9500 . ? C104 N6 1.166(10) . ? C105 C107 1.529(8) . ? C105 C108 1.534(8) . ? C105 C106 1.538(9) . ? C106 H10A 0.9800 . ? C106 H10B 0.9800 . ? C106 H10C 0.9800 . ? C107 H10D 0.9800 . ? C107 H10E 0.9800 . ? C107 H10F 0.9800 . ? C108 H10G 0.9800 . ? C108 H10H 0.9800 . ? C108 H10I 0.9800 . ? S7 C111 1.783(5) . ? C109 C114 1.396(7) . ? C109 C110 1.396(7) . ? C109 S8 1.786(5) . ? C110 C111 1.385(8) . ? C110 O7 1.389(6) . ? C111 C112 1.362(7) . ? C112 C113 1.402(7) . ? C112 H112 0.9500 . ? C113 C114 1.395(7) . ? C113 C123 1.537(8) . ? C114 H114 0.9500 . ? O7 C115 1.458(7) . ? C115 C116 1.480(6) . ? C115 H11A 0.9900 . ? C115 H11B 0.9900 . ? C116 C117 1.3900 . ? C116 C121 1.3900 . ? C117 C118 1.3900 . ? C117 H117 0.9500 . ? C118 C119 1.3900 . ? C118 H118 0.9500 . ? C119 C120 1.3900 . ? C119 C122 1.468(11) . ? C120 C121 1.3900 . ? C120 H120 0.9500 . ? C121 H121 0.9500 . ? C122 N7 1.130(11) . ? C123 C126 1.519(8) . ? C123 C124 1.530(8) . ? C123 C125 1.537(9) . ? C124 H12A 0.9800 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? C125 H12D 0.9800 . ? C125 H12E 0.9800 . ? C125 H12F 0.9800 . ? C126 H12G 0.9800 . ? C126 H12H 0.9800 . ? C126 H12I 0.9800 . ? S8 C127 1.764(5) . ? C127 C128 1.397(6) . ? C127 C132 1.398(7) . ? C128 O8 1.384(5) . ? C128 C129 1.390(7) . ? C129 C130 1.390(6) . ? C130 C131 1.397(7) . ? C130 H130 0.9500 . ? C131 C132 1.397(7) . ? C131 C141 1.514(10) . ? C132 H132 0.9500 . ? O8 C133 1.455(6) . ? C133 C134 1.494(8) . ? C133 H13A 0.9900 . ? C133 H13B 0.9900 . ? C134 C135 1.358(9) . ? C134 C139 1.383(9) . ? C135 C136 1.360(9) . ? C135 H135 0.9500 . ? C136 C137 1.373(11) . ? C136 H136 0.9500 . ? C137 C138 1.352(13) . ? C137 C140 1.446(11) . ? C138 C139 1.381(11) . ? C138 H138 0.9500 . ? C139 H139 0.9500 . ? C140 N8 1.185(10) . ? C141 C143 1.514(13) . ? C141 C144 1.537(11) . ? C141 C142 1.543(11) . ? C142 H14A 0.9800 . ? C142 H14B 0.9800 . ? C142 H14C 0.9800 . ? C143 H14D 0.9800 . ? C143 H14E 0.9800 . ? C143 H14F 0.9800 . ? C144 H14G 0.9800 . ? C144 H14H 0.9800 . ? C144 H14I 0.9800 . ? C145 Cl1 1.738(8) . ? C145 Cl3 1.739(8) . ? C145 Cl2 1.740(8) . ? C145 H145 1.0000 . ? Cl4 C146 1.818(9) . ? Cl5 C146 1.662(11) . ? Cl6 C146 1.701(11) . ? Cl4A C146 1.733(12) . ? Cl5A C146 1.487(13) . ? Cl6A C146 1.754(14) . ? C146 H146 1.0000 . ? 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 C1 S1 C57 108.8(2) . . ? C2 C1 C6 119.9(4) . . ? C2 C1 S1 123.3(3) . . ? C6 C1 S1 115.9(4) . . ? C1 C2 O1 120.7(4) . . ? C1 C2 C3 119.4(4) . . ? O1 C2 C3 119.9(4) . . ? C4 C3 C2 119.8(4) . . ? C4 C3 S2 116.6(3) . . ? C2 C3 S2 122.4(3) . . ? C3 C4 C5 121.3(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 117.8(4) . . ? C6 C5 C15 122.5(4) . . ? C4 C5 C15 119.7(4) . . ? C5 C6 C1 121.6(4) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? C2 O1 C7 112.3(3) . . ? O1 C7 C8 109.3(4) . . ? O1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? C9 C8 C13 119.5(5) . . ? C9 C8 C7 122.4(5) . . ? C13 C8 C7 118.1(6) . . ? C10 C9 C8 118.8(7) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C11 C10 C9 120.8(8) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 120.2(6) . . ? C12 C11 C14 121.2(9) . . ? C10 C11 C14 118.7(10) . . ? C11 C12 C13 120.7(8) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 120.2(8) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? N1 C14 C11 177.9(11) . . ? C16 C15 C18 109.0(6) . . ? C16 C15 C17 109.8(7) . . ? C18 C15 C17 108.7(6) . . ? C16 C15 C5 111.4(4) . . ? C18 C15 C5 110.0(5) . . ? C17 C15 C5 107.8(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 S2 C3 107.0(2) . . ? C24 C19 C20 118.8(4) . . ? C24 C19 S2 116.7(3) . . ? C20 C19 S2 124.1(3) . . ? O2 C20 C21 118.7(4) . . ? O2 C20 C19 122.5(4) . . ? C21 C20 C19 118.8(4) . . ? C20 C21 C22 119.8(4) . . ? C20 C21 S3 123.1(3) . . ? C22 C21 S3 116.2(3) . . ? C23 C22 C21 122.1(4) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 116.8(4) . . ? C22 C23 C33 120.7(4) . . ? C24 C23 C33 122.5(4) . . ? C19 C24 C23 122.8(4) . . ? C19 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? C20 O2 C25 114.0(3) . . ? O2 C25 C26 110.0(4) . . ? O2 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? O2 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C31 C26 C27 119.6(5) . . ? C31 C26 C25 121.1(5) . . ? C27 C26 C25 119.3(5) . . ? C26 C27 C28 121.2(5) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C29 118.0(5) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? C30 C29 C28 122.3(5) . . ? C30 C29 C32 118.8(5) . . ? C28 C29 C32 118.9(5) . . ? C29 C30 C31 117.7(5) . . ? C29 C30 H30 121.2 . . ? C31 C30 H30 121.2 . . ? C26 C31 C30 121.2(5) . . ? C26 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? N2 C32 C29 178.8(7) . . ? C36 C33 C34 112.7(5) . . ? C36 C33 C23 112.5(4) . . ? C34 C33 C23 106.5(4) . . ? C36 C33 C35 107.4(5) . . ? C34 C33 C35 106.9(5) . . ? C23 C33 C35 110.7(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C21 S3 C37 106.2(2) . . ? C42 C37 C38 119.8(4) . . ? C42 C37 S3 117.8(4) . . ? C38 C37 S3 121.7(3) . . ? O3 C38 C39 119.3(4) . . ? O3 C38 C37 122.6(4) . . ? C39 C38 C37 118.1(4) . . ? C40 C39 C38 119.8(4) . . ? C40 C39 S4 117.0(4) . . ? C38 C39 S4 122.5(4) . . ? C41 C40 C39 122.6(5) . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C40 C41 C42 116.4(4) . . ? C40 C41 C51 122.0(4) . . ? C42 C41 C51 121.5(4) . . ? C37 C42 C41 122.7(4) . . ? C37 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? C38 O3 C43 109.0(4) . . ? O3 C43 C44 109.8(5) . . ? O3 C43 H43A 109.7 . . ? C44 C43 H43A 109.7 . . ? O3 C43 H43B 109.7 . . ? C44 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C49 C44 C45 118.6(5) . . ? C49 C44 C43 120.8(6) . . ? C45 C44 C43 120.6(6) . . ? C44 C45 C46 120.6(6) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 119.7(6) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 121.3(5) . . ? C46 C47 C50 119.9(5) . . ? C48 C47 C50 118.8(6) . . ? C49 C48 C47 117.0(6) . . ? C49 C48 H48 121.5 . . ? C47 C48 H48 121.5 . . ? C44 C49 C48 122.9(6) . . ? C44 C49 H49 118.6 . . ? C48 C49 H49 118.6 . . ? N3 C50 C47 177.3(7) . . ? C52 C51 C54 109.2(4) . . ? C52 C51 C41 111.9(4) . . ? C54 C51 C41 107.1(4) . . ? C52 C51 C53 108.2(4) . . ? C54 C51 C53 109.3(5) . . ? C41 C51 C53 111.1(4) . . ? 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 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C39 S4 C55 107.2(2) . . ? C60 C55 C56 119.2(5) . . ? C60 C55 S4 116.6(4) . . ? C56 C55 S4 123.5(4) . . ? O4 C56 C57 120.5(4) . . ? O4 C56 C55 120.1(4) . . ? C57 C56 C55 119.2(4) . . ? C56 C57 C58 120.5(4) . . ? C56 C57 S1 122.3(4) . . ? C58 C57 S1 116.5(4) . . ? C57 C58 C59 120.7(5) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.6 . . ? C60 C59 C58 117.8(4) . . ? C60 C59 C69 120.9(5) . . ? C58 C59 C69 121.3(5) . . ? C55 C60 C59 122.6(5) . . ? C55 C60 H60 118.7 . . ? C59 C60 H60 118.7 . . ? C56 O4 C61 116.4(3) . . ? O4 C61 C62 107.5(4) . . ? O4 C61 H61A 110.2 . . ? C62 C61 H61A 110.2 . . ? O4 C61 H61B 110.2 . . ? C62 C61 H61B 110.2 . . ? H61A C61 H61B 108.5 . . ? C67 C62 C63 118.5(4) . . ? C67 C62 C61 121.2(4) . . ? C63 C62 C61 120.2(4) . . ? C64 C63 C62 121.6(5) . . ? C64 C63 H63 119.2 . . ? C62 C63 H63 119.2 . . ? C63 C64 C65 119.2(5) . . ? C63 C64 H64 120.4 . . ? C65 C64 H64 120.4 . . ? C66 C65 C64 119.5(5) . . ? C66 C65 C68 119.4(5) . . ? C64 C65 C68 121.0(5) . . ? C67 C66 C65 120.9(5) . . ? C67 C66 H66 119.5 . . ? C65 C66 H66 119.5 . . ? C66 C67 C62 120.2(4) . . ? C66 C67 H67 119.9 . . ? C62 C67 H67 119.9 . . ? N4 C68 C65 176.5(7) . . ? C70 C69 C72 112.7(6) . . ? C70 C69 C59 113.1(6) . . ? C72 C69 C59 109.9(5) . . ? C70 C69 C71 108.3(6) . . ? C72 C69 C71 103.6(6) . . ? C59 C69 C71 108.6(6) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C129 S5 C73 107.8(2) . . ? C78 C73 C74 120.0(4) . . ? C78 C73 S5 115.8(3) . . ? C74 C73 S5 123.4(3) . . ? C75 C74 O5 120.9(4) . . ? C75 C74 C73 119.1(4) . . ? O5 C74 C73 120.0(4) . . ? C74 C75 C76 120.4(4) . . ? C74 C75 S6 124.1(4) . . ? C76 C75 S6 114.9(4) . . ? C77 C76 C75 121.3(5) . . ? C77 C76 H76 119.4 . . ? C75 C76 H76 119.4 . . ? C78 C77 C76 117.7(4) . . ? C78 C77 C87 121.9(4) . . ? C76 C77 C87 120.3(5) . . ? C77 C78 C73 121.6(4) . . ? C77 C78 H78 119.2 . . ? C73 C78 H78 119.2 . . ? C74 O5 C79 114.7(4) . . ? O5 C79 C80 109.0(4) . . ? O5 C79 H79A 109.9 . . ? C80 C79 H79A 109.9 . . ? O5 C79 H79B 109.9 . . ? C80 C79 H79B 109.9 . . ? H79A C79 H79B 108.3 . . ? C81 C80 C85 118.9(5) . . ? C81 C80 C79 122.5(4) . . ? C85 C80 C79 118.6(5) . . ? C80 C81 C82 121.0(5) . . ? C80 C81 H81 119.5 . . ? C82 C81 H81 119.5 . . ? C81 C82 C83 119.9(6) . . ? C81 C82 H82 120.1 . . ? C83 C82 H82 120.1 . . ? C84 C83 C82 119.3(5) . . ? C84 C83 C86 120.4(6) . . ? C82 C83 C86 120.2(6) . . ? C85 C84 C83 119.3(5) . . ? C85 C84 H84 120.3 . . ? C83 C84 H84 120.3 . . ? C84 C85 C80 121.6(6) . . ? C84 C85 H85 119.2 . . ? C80 C85 H85 119.2 . . ? N5 C86 C83 179.2(10) . . ? C89A C87 C90 132.2(8) . . ? C89A C87 C77 113.9(8) . . ? C90 C87 C77 113.8(6) . . ? C89A C87 C88A 108.0(12) . . ? C90 C87 C88A 60.2(9) . . ? C77 C87 C88A 107.5(8) . . ? C89A C87 C89 55.8(10) . . ? C90 C87 C89 109.5(7) . . ? C77 C87 C89 110.3(5) . . ? C88A C87 C89 55.6(9) . . ? C89A C87 C88 50.1(10) . . ? C90 C87 C88 110.5(7) . . ? C77 C87 C88 107.2(5) . . ? C88A C87 C88 144.5(8) . . ? C89 C87 C88 105.1(7) . . ? C89A C87 C90A 113.3(12) . . ? C90 C87 C90A 44.2(9) . . ? C77 C87 C90A 109.8(8) . . ? C88A C87 C90A 103.6(12) . . ? C89 C87 C90A 139.0(8) . . ? C88 C87 C90A 70.5(10) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? C87 C88A H88D 109.5 . . ? C87 C88A H88E 109.5 . . ? H88D C88A H88E 109.5 . . ? C87 C88A H88F 109.5 . . ? H88D C88A H88F 109.5 . . ? H88E C88A H88F 109.5 . . ? C87 C89A H89D 109.5 . . ? C87 C89A H89E 109.5 . . ? H89D C89A H89E 109.5 . . ? C87 C89A H89F 109.5 . . ? H89D C89A H89F 109.5 . . ? H89E C89A H89F 109.5 . . ? C87 C90A H90D 109.5 . . ? C87 C90A H90E 109.5 . . ? H90D C90A H90E 109.5 . . ? C87 C90A H90F 109.5 . . ? H90D C90A H90F 109.5 . . ? H90E C90A H90F 109.5 . . ? C91 S6 C75 107.7(2) . . ? C96 C91 C92 119.8(5) . . ? C96 C91 S6 116.9(4) . . ? C92 C91 S6 122.6(4) . . ? C91 C92 O6 121.3(5) . . ? C91 C92 C93 119.5(4) . . ? O6 C92 C93 119.2(5) . . ? C94 C93 C92 118.8(5) . . ? C94 C93 S7 118.1(4) . . ? C92 C93 S7 122.5(4) . . ? C95 C94 C93 122.4(5) . . ? C95 C94 H94 118.8 . . ? C93 C94 H94 118.8 . . ? C94 C95 C96 117.4(4) . . ? C94 C95 C105 121.8(4) . . ? C96 C95 C105 120.7(5) . . ? C91 C96 C95 122.0(5) . . ? C91 C96 H96 119.0 . . ? C95 C96 H96 119.0 . . ? C92 O6 C97 110.3(4) . . ? C98 C97 O6 111.6(6) . . ? C98 C97 H97A 109.3 . . ? O6 C97 H97A 109.3 . . ? C98 C97 H97B 109.3 . . ? O6 C97 H97B 109.3 . . ? H97A C97 H97B 108.0 . . ? C99 C98 C103 118.5(8) . . ? C99 C98 C97 125.0(8) . . ? C103 C98 C97 116.0(8) . . ? C98 C99 C100 119.9(9) . . ? C98 C99 H99 120.1 . . ? C100 C99 H99 120.1 . . ? C99 C100 C101 119.1(9) . . ? C99 C100 H100 120.4 . . ? C101 C100 H100 120.4 . . ? C102 C101 C104 115.9(9) . . ? C102 C101 C100 121.0(8) . . ? C104 C101 C100 123.0(9) . . ? C103 C102 C101 118.5(9) . . ? C103 C102 H102 120.7 . . ? C101 C102 H102 120.7 . . ? C102 C103 C98 122.5(9) . . ? C102 C103 H103 118.7 . . ? C98 C103 H103 118.7 . . ? N6 C104 C101 177.8(13) . . ? C107 C105 C108 110.2(5) . . ? C107 C105 C106 107.8(5) . . ? C108 C105 C106 108.3(5) . . ? C107 C105 C95 107.6(4) . . ? C108 C105 C95 111.1(4) . . ? C106 C105 C95 111.8(4) . . ? C105 C106 H10A 109.5 . . ? C105 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C105 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? C105 C107 H10D 109.5 . . ? C105 C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C105 C107 H10F 109.5 . . ? H10D C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C105 C108 H10G 109.5 . . ? C105 C108 H10H 109.5 . . ? H10G C108 H10H 109.5 . . ? C105 C108 H10I 109.5 . . ? H10G C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? C93 S7 C111 106.2(2) . . ? C114 C109 C110 119.8(5) . . ? C114 C109 S8 118.3(4) . . ? C110 C109 S8 121.3(4) . . ? C111 C110 O7 121.0(4) . . ? C111 C110 C109 118.4(4) . . ? O7 C110 C109 120.5(5) . . ? C112 C111 C110 120.7(5) . . ? C112 C111 S7 117.3(4) . . ? C110 C111 S7 121.5(4) . . ? C111 C112 C113 122.7(5) . . ? C111 C112 H112 118.6 . . ? C113 C112 H112 118.6 . . ? C114 C113 C112 115.9(5) . . ? C114 C113 C123 120.3(5) . . ? C112 C113 C123 123.8(5) . . ? C113 C114 C109 121.9(5) . . ? C113 C114 H114 119.0 . . ? C109 C114 H114 119.0 . . ? C110 O7 C115 107.3(4) . . ? O7 C115 C116 110.3(4) . . ? O7 C115 H11A 109.6 . . ? C116 C115 H11A 109.6 . . ? O7 C115 H11B 109.6 . . ? C116 C115 H11B 109.6 . . ? H11A C115 H11B 108.1 . . ? C117 C116 C121 120.0 . . ? C117 C116 C115 119.1(4) . . ? C121 C116 C115 120.5(4) . . ? C118 C117 C116 120.0 . . ? C118 C117 H117 120.0 . . ? C116 C117 H117 120.0 . . ? C119 C118 C117 120.0 . . ? C119 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C120 C119 C118 120.0 . . ? C120 C119 C122 108.6(8) . . ? C118 C119 C122 130.8(8) . . ? C119 C120 C121 120.0 . . ? C119 C120 H120 120.0 . . ? C121 C120 H120 120.0 . . ? C120 C121 C116 120.0 . . ? C120 C121 H121 120.0 . . ? C116 C121 H121 120.0 . . ? N7 C122 C119 174.2(15) . . ? C126 C123 C124 108.1(5) . . ? C126 C123 C125 109.2(6) . . ? C124 C123 C125 109.3(5) . . ? C126 C123 C113 111.5(5) . . ? C124 C123 C113 110.8(5) . . ? C125 C123 C113 107.9(5) . . ? C123 C124 H12A 109.5 . . ? C123 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? C123 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? C123 C125 H12D 109.5 . . ? C123 C125 H12E 109.5 . . ? H12D C125 H12E 109.5 . . ? C123 C125 H12F 109.5 . . ? H12D C125 H12F 109.5 . . ? H12E C125 H12F 109.5 . . ? C123 C126 H12G 109.5 . . ? C123 C126 H12H 109.5 . . ? H12G C126 H12H 109.5 . . ? C123 C126 H12I 109.5 . . ? H12G C126 H12I 109.5 . . ? H12H C126 H12I 109.5 . . ? C127 S8 C109 105.3(2) . . ? C128 C127 C132 118.8(4) . . ? C128 C127 S8 123.1(4) . . ? C132 C127 S8 117.5(4) . . ? O8 C128 C129 119.3(4) . . ? O8 C128 C127 121.3(4) . . ? C129 C128 C127 119.4(4) . . ? C130 C129 C128 120.4(4) . . ? C130 C129 S5 117.9(4) . . ? C128 C129 S5 121.1(4) . . ? C129 C130 C131 121.5(4) . . ? C129 C130 H130 119.2 . . ? C131 C130 H130 119.2 . . ? C130 C131 C132 116.9(4) . . ? C130 C131 C141 121.4(5) . . ? C132 C131 C141 121.7(5) . . ? C131 C132 C127 122.6(4) . . ? C131 C132 H132 118.7 . . ? C127 C132 H132 118.7 . . ? C128 O8 C133 112.0(4) . . ? O8 C133 C134 108.9(4) . . ? O8 C133 H13A 109.9 . . ? C134 C133 H13A 109.9 . . ? O8 C133 H13B 109.9 . . ? C134 C133 H13B 109.9 . . ? H13A C133 H13B 108.3 . . ? C135 C134 C139 118.2(6) . . ? C135 C134 C133 120.4(6) . . ? C139 C134 C133 121.3(6) . . ? C134 C135 C136 122.5(6) . . ? C134 C135 H135 118.7 . . ? C136 C135 H135 118.7 . . ? C135 C136 C137 118.7(8) . . ? C135 C136 H136 120.6 . . ? C137 C136 H136 120.6 . . ? C138 C137 C136 120.4(6) . . ? C138 C137 C140 120.4(8) . . ? C136 C137 C140 119.2(10) . . ? C137 C138 C139 120.3(6) . . ? C137 C138 H138 119.8 . . ? C139 C138 H138 119.8 . . ? C138 C139 C134 119.8(7) . . ? C138 C139 H139 120.1 . . ? C134 C139 H139 120.1 . . ? N8 C140 C137 174.1(14) . . ? C143 C141 C131 106.5(6) . . ? C143 C141 C144 112.7(8) . . ? C131 C141 C144 111.4(7) . . ? C143 C141 C142 107.4(8) . . ? C131 C141 C142 112.3(6) . . ? C144 C141 C142 106.6(7) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? Cl1 C145 Cl3 110.1(4) . . ? Cl1 C145 Cl2 112.3(5) . . ? Cl3 C145 Cl2 110.4(4) . . ? Cl1 C145 H145 107.9 . . ? Cl3 C145 H145 107.9 . . ? Cl2 C145 H145 107.9 . . ? Cl5A C146 Cl5 124.4(9) . . ? Cl5A C146 Cl6 80.1(10) . . ? Cl5 C146 Cl6 119.1(7) . . ? Cl5A C146 Cl4A 112.0(9) . . ? Cl5 C146 Cl4A 71.2(9) . . ? Cl6 C146 Cl4A 48.3(8) . . ? Cl5A C146 Cl6A 109.9(10) . . ? Cl5 C146 Cl6A 23.5(7) . . ? Cl6 C146 Cl6A 139.8(8) . . ? Cl4A C146 Cl6A 93.6(8) . . ? Cl5A C146 Cl4 22.8(10) . . ? Cl5 C146 Cl4 110.1(6) . . ? Cl6 C146 Cl4 102.8(5) . . ? Cl4A C146 Cl4 127.7(7) . . ? Cl6A C146 Cl4 91.0(8) . . ? Cl5A C146 H146 114.1 . . ? Cl5 C146 H146 108.1 . . ? Cl6 C146 H146 108.1 . . ? Cl4A C146 H146 121.3 . . ? Cl6A C146 H146 102.9 . . ? Cl4 C146 H146 108.1 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.80 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.986 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.090 #===END