# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Baskar Viswanathan' _publ_contact_author_email baskarviswanathan@googlemail.com _publ_author_name 'Baskar Viswanathan' data_1 _database_code_depnum_ccdc_archive 'CCDC 808827' #TrackingRef '- cif all in one.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H72 Cl4 N4 O10 Sb4' _chemical_formula_sum 'C88 H72 Cl4 N4 O10 Sb4' _chemical_formula_weight 1974.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I4(1)/a ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.4622(10) _cell_length_b 19.4622(10) _cell_length_c 20.882(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7909.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 8942 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 1.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7468 _exptl_absorpt_correction_T_max 0.8604 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(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 36644 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.08 _reflns_number_total 3503 _reflns_number_gt 3238 _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. ; _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^)+(0.0388P)^2^+33.9442P] 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 3503 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 C17 C 0.38937(18) 0.1357(2) 0.9709(2) 0.0749(15) Uani 1 1 d G . . C18 C 0.4511(2) 0.17161(19) 0.9700(3) 0.127(3) Uani 1 1 d G . . H18 H 0.4529 0.2163 0.9857 0.153 Uiso 1 1 calc R . . C19 C 0.50999(18) 0.1408(3) 0.9458(3) 0.152(5) Uani 1 1 d G . . H19 H 0.5513 0.1648 0.9452 0.183 Uiso 1 1 calc R . . C20 C 0.5072(2) 0.0740(3) 0.9224(3) 0.101(2) Uani 1 1 d G . . H20 H 0.5466 0.0533 0.9061 0.121 Uiso 1 1 calc R . . C21 C 0.4455(2) 0.0380(2) 0.9232(2) 0.127(3) Uani 1 1 d G . . H21 H 0.4436 -0.0067 0.9076 0.153 Uiso 1 1 calc R . . C22 C 0.38659(19) 0.0688(2) 0.9475(2) 0.0746(16) Uani 1 1 d G . . H22 H 0.3453 0.0448 0.9481 0.090 Uiso 1 1 calc R . . Sb1 Sb 0.498319(10) 0.161300(10) 0.312629(9) 0.01908(9) Uani 1 1 d . . . O2 O 0.43339(11) 0.17375(10) 0.38269(10) 0.0209(4) Uani 1 1 d . . . O3 O 0.5000 0.2500 0.27042(14) 0.0228(6) Uani 1 2 d S . . O1 O 0.57161(11) 0.12101(11) 0.25181(10) 0.0243(5) Uani 1 1 d . . . N1 N 0.51453(13) 0.05539(13) 0.35149(12) 0.0223(5) Uani 1 1 d . . . C15 C 0.35458(17) 0.11316(17) 0.27323(16) 0.0283(7) Uani 1 1 d . . . H15 H 0.3446 0.1236 0.3157 0.034 Uiso 1 1 calc R . . C1 C 0.56163(16) 0.02043(16) 0.31593(16) 0.0251(7) Uani 1 1 d . . . C10 C 0.42042(16) 0.12243(15) 0.25046(15) 0.0239(6) Uani 1 1 d . . . C6 C 0.58104(18) -0.04745(18) 0.33146(18) 0.0329(8) Uani 1 1 d . . . C8 C 0.50384(18) -0.04005(18) 0.42094(17) 0.0313(8) Uani 1 1 d . . . H8 H 0.4837 -0.0593 0.4571 0.038 Uiso 1 1 calc R . . C11 C 0.43450(19) 0.1086(2) 0.18605(16) 0.0342(8) Uani 1 1 d . . . H11 H 0.4785 0.1158 0.1700 0.041 Uiso 1 1 calc R . . C9 C 0.48598(17) 0.02650(17) 0.40185(16) 0.0269(7) Uani 1 1 d . . . H9 H 0.4533 0.0508 0.4252 0.032 Uiso 1 1 calc R . . C7 C 0.55069(18) -0.07663(18) 0.38650(19) 0.0351(8) Uani 1 1 d . . . H7 H 0.5627 -0.1208 0.3992 0.042 Uiso 1 1 calc R . . C14 C 0.30285(18) 0.08833(18) 0.23343(18) 0.0333(8) Uani 1 1 d . . . H14 H 0.2585 0.0818 0.2489 0.040 Uiso 1 1 calc R . . C13 C 0.31859(19) 0.07372(18) 0.17099(18) 0.0357(8) Uani 1 1 d . . . C2 C 0.58966(16) 0.05573(16) 0.26226(16) 0.0257(7) Uani 1 1 d . . . C12 C 0.3833(2) 0.0844(2) 0.14608(18) 0.0393(9) Uani 1 1 d . . . H12 H 0.3923 0.0755 0.1031 0.047 Uiso 1 1 calc R . . C4 C 0.6519(2) -0.0481(2) 0.2378(2) 0.0507(11) Uani 1 1 d . . . H4 H 0.6819 -0.0712 0.2107 0.061 Uiso 1 1 calc R . . C3 C 0.63342(19) 0.02026(19) 0.22292(19) 0.0372(8) Uani 1 1 d . . . H3 H 0.6510 0.0412 0.1864 0.045 Uiso 1 1 calc R . . C5 C 0.6275(2) -0.0815(2) 0.2903(2) 0.0492(11) Uani 1 1 d . . . H5 H 0.6412 -0.1263 0.2989 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.25378(6) 0.04228(6) 0.12151(6) 0.0557(3) Uani 1 1 d . . . C16 C 0.3289(3) 0.1671(4) 0.9946(3) 0.094(2) Uani 1 1 d . . . H16A H 0.3370 0.1837 1.0373 0.141 Uiso 1 1 calc R . . H16B H 0.2923 0.1341 0.9953 0.141 Uiso 1 1 calc R . . H16C H 0.3164 0.2048 0.9674 0.141 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 C17 0.082(4) 0.077(4) 0.066(3) 0.004(3) -0.003(3) -0.001(3) C18 0.067(4) 0.081(5) 0.234(11) 0.000(6) -0.008(6) -0.028(4) C19 0.089(6) 0.068(5) 0.300(16) -0.020(7) -0.020(7) 0.002(4) C20 0.073(4) 0.131(7) 0.099(5) 0.003(5) 0.006(4) 0.001(4) C21 0.114(7) 0.114(7) 0.153(8) -0.031(6) 0.002(6) -0.020(5) C22 0.067(3) 0.067(3) 0.090(4) -0.018(3) 0.000(3) -0.017(3) Sb1 0.02148(13) 0.01868(13) 0.01709(13) -0.00067(7) -0.00033(7) 0.00050(7) O2 0.0227(11) 0.0207(11) 0.0193(11) -0.0023(8) 0.0026(8) 0.0001(8) O3 0.0322(17) 0.0175(14) 0.0186(15) 0.000 0.000 0.0023(12) O1 0.0271(11) 0.0228(11) 0.0231(11) -0.0012(9) 0.0035(9) 0.0012(9) N1 0.0221(13) 0.0230(13) 0.0218(13) 0.0005(11) -0.0025(10) -0.0023(10) C15 0.0340(18) 0.0259(16) 0.0248(17) -0.0001(13) -0.0043(14) -0.0038(14) C1 0.0210(16) 0.0243(16) 0.0300(17) -0.0031(13) -0.0015(13) 0.0002(12) C10 0.0308(17) 0.0186(15) 0.0222(15) -0.0013(12) -0.0058(13) 0.0031(12) C6 0.0311(18) 0.0259(17) 0.042(2) 0.0020(15) 0.0012(15) 0.0032(14) C8 0.0320(18) 0.0311(18) 0.0309(18) 0.0093(14) -0.0025(14) -0.0039(14) C11 0.0331(19) 0.042(2) 0.0274(18) -0.0055(15) -0.0025(14) 0.0050(16) C9 0.0256(16) 0.0293(17) 0.0257(17) -0.0003(13) -0.0013(13) -0.0019(13) C7 0.0327(19) 0.0257(17) 0.047(2) 0.0080(16) -0.0036(16) 0.0018(14) C14 0.0307(18) 0.0318(18) 0.037(2) 0.0002(15) -0.0080(15) -0.0025(14) C13 0.040(2) 0.0301(18) 0.037(2) -0.0063(15) -0.0182(16) 0.0025(15) C2 0.0248(16) 0.0253(16) 0.0271(17) -0.0022(13) -0.0006(13) 0.0003(13) C12 0.048(2) 0.044(2) 0.0255(18) -0.0098(16) -0.0091(16) 0.0085(17) C4 0.051(2) 0.035(2) 0.066(3) -0.003(2) 0.026(2) 0.0130(18) C3 0.0354(19) 0.0324(19) 0.044(2) -0.0021(16) 0.0140(17) 0.0016(15) C5 0.050(2) 0.0264(19) 0.072(3) 0.0049(19) 0.017(2) 0.0141(17) Cl1 0.0507(6) 0.0627(7) 0.0537(6) -0.0226(5) -0.0280(5) 0.0027(5) C16 0.074(4) 0.119(6) 0.089(5) 0.022(4) -0.002(4) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C17 C18 1.3900 . ? C17 C22 1.3900 . ? C17 C16 1.416(7) . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? Sb1 O3 1.9386(13) . ? Sb1 O2 1.947(2) 16_656 ? Sb1 O2 1.948(2) . ? Sb1 O1 2.065(2) . ? Sb1 C10 2.134(3) . ? Sb1 N1 2.238(3) . ? O2 Sb1 1.947(2) 11_666 ? O3 Sb1 1.9386(13) 6_554 ? O1 C2 1.336(4) . ? N1 C9 1.316(4) . ? N1 C1 1.362(4) . ? C15 C10 1.379(5) . ? C15 C14 1.392(5) . ? C15 H15 0.9300 . ? C1 C6 1.412(5) . ? C1 C2 1.423(5) . ? C10 C11 1.399(5) . ? C6 C7 1.411(5) . ? C6 C5 1.413(5) . ? C8 C7 1.362(5) . ? C8 C9 1.399(5) . ? C8 H8 0.9300 . ? C11 C12 1.383(5) . ? C11 H11 0.9300 . ? C9 H9 0.9300 . ? C7 H7 0.9300 . ? C14 C13 1.369(5) . ? C14 H14 0.9300 . ? C13 C12 1.378(6) . ? C13 Cl1 1.742(3) . ? C2 C3 1.370(5) . ? C12 H12 0.9300 . ? C4 C5 1.359(6) . ? C4 C3 1.413(5) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C5 H5 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 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 C18 C17 C22 120.0 . . ? C18 C17 C16 120.3(4) . . ? C22 C17 C16 119.7(4) . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 120.0 . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? O3 Sb1 O2 93.26(8) . 16_656 ? O3 Sb1 O2 103.98(8) . . ? O2 Sb1 O2 92.14(8) 16_656 . ? O3 Sb1 O1 92.69(8) . . ? O2 Sb1 O1 84.63(9) 16_656 . ? O2 Sb1 O1 163.19(8) . . ? O3 Sb1 C10 92.92(10) . . ? O2 Sb1 C10 171.29(10) 16_656 . ? O2 Sb1 C10 92.30(11) . . ? O1 Sb1 C10 88.97(11) . . ? O3 Sb1 N1 169.37(8) . . ? O2 Sb1 N1 83.16(9) 16_656 . ? O2 Sb1 N1 86.20(9) . . ? O1 Sb1 N1 77.05(9) . . ? C10 Sb1 N1 89.67(10) . . ? Sb1 O2 Sb1 132.89(11) 11_666 . ? Sb1 O3 Sb1 125.91(15) . 6_554 ? C2 O1 Sb1 116.26(19) . . ? C9 N1 C1 120.4(3) . . ? C9 N1 Sb1 128.6(2) . . ? C1 N1 Sb1 110.9(2) . . ? C10 C15 C14 120.8(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N1 C1 C6 121.5(3) . . ? N1 C1 C2 116.5(3) . . ? C6 C1 C2 122.0(3) . . ? C15 C10 C11 119.2(3) . . ? C15 C10 Sb1 119.8(2) . . ? C11 C10 Sb1 120.9(3) . . ? C7 C6 C1 116.8(3) . . ? C7 C6 C5 125.1(3) . . ? C1 C6 C5 118.1(3) . . ? C7 C8 C9 120.0(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? N1 C9 C8 121.2(3) . . ? N1 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C13 C14 C15 118.6(3) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C13 C12 122.2(3) . . ? C14 C13 Cl1 118.4(3) . . ? C12 C13 Cl1 119.4(3) . . ? O1 C2 C3 123.0(3) . . ? O1 C2 C1 119.1(3) . . ? C3 C2 C1 117.9(3) . . ? C13 C12 C11 118.8(3) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C5 C4 C3 122.6(4) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C4 C5 C6 119.3(4) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.080 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.090 #===========================================================================END data_2 _database_code_depnum_ccdc_archive 'CCDC 808828' #TrackingRef '- cif all in one.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H72 Br4 N4 O10 Sb4' _chemical_formula_sum 'C88 H72 Br4 N4 O10 Sb4' _chemical_formula_weight 2152.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I4(1)/a ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.226(9) _cell_length_b 19.226(9) _cell_length_c 21.370(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7899(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5782 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 25.13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 3.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5182 _exptl_absorpt_correction_T_max 0.7248 _exptl_absorpt_process_details brukarsadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 26544 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3472 _reflns_number_gt 2956 _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. one heavily disordered toluene molecule modeled using DFIX DANG EADP constraints so that the number of restaints were 59. ; _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^)+(0.0762P)^2^+108.0603P] 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 3472 _refine_ls_number_parameters 214 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.065 _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 Br1 Br 0.20685(7) 0.49978(6) -0.12930(5) 0.0746(4) Uani 1 1 d . . . C1 C 0.2317(4) 0.1876(4) 0.0667(3) 0.0324(15) Uani 1 1 d . . . C2 C 0.1959(4) 0.1586(3) 0.0149(3) 0.0313(15) Uani 1 1 d . . . C3 C 0.2321(4) 0.1165(4) -0.0235(4) 0.048(2) Uani 1 1 d . . . H3 H 0.2110 0.0993 -0.0595 0.058 Uiso 1 1 calc R . . C4 C 0.3006(5) 0.0983(5) -0.0101(6) 0.071(3) Uani 1 1 d . . . H4 H 0.3239 0.0682 -0.0369 0.085 Uiso 1 1 calc R . . C5 C 0.3344(5) 0.1230(6) 0.0408(6) 0.071(3) Uani 1 1 d . . . H5 H 0.3800 0.1097 0.0487 0.085 Uiso 1 1 calc R . . C6 C 0.3006(4) 0.1687(4) 0.0816(5) 0.050(2) Uani 1 1 d . . . C7 C 0.3298(4) 0.1975(4) 0.1351(4) 0.046(2) Uani 1 1 d . . . H7 H 0.3745 0.1853 0.1474 0.055 Uiso 1 1 calc R . . C8 C 0.2923(4) 0.2436(4) 0.1693(4) 0.0386(17) Uani 1 1 d . . . H8 H 0.3117 0.2635 0.2050 0.046 Uiso 1 1 calc R . . C9 C 0.2250(4) 0.2613(4) 0.1513(3) 0.0306(15) Uani 1 1 d . . . H9 H 0.2002 0.2935 0.1748 0.037 Uiso 1 1 calc R . . C10 C 0.1289(4) 0.3273(4) 0.0036(3) 0.0302(15) Uani 1 1 d . . . C11 C 0.1335(4) 0.3950(4) 0.0228(3) 0.0367(17) Uani 1 1 d . . . H11 H 0.1204 0.4061 0.0634 0.044 Uiso 1 1 calc R . . C12 C 0.1567(4) 0.4472(4) -0.0159(4) 0.0407(18) Uani 1 1 d . . . H12 H 0.1595 0.4929 -0.0021 0.049 Uiso 1 1 calc R . . C13 C 0.1753(4) 0.4297(4) -0.0750(4) 0.044(2) Uani 1 1 d . . . C14 C 0.1684(5) 0.3635(5) -0.0979(4) 0.059(3) Uani 1 1 d . . . H14 H 0.1798 0.3534 -0.1393 0.071 Uiso 1 1 calc R . . C15 C 0.1441(5) 0.3118(5) -0.0580(4) 0.051(2) Uani 1 1 d . . . H15 H 0.1380 0.2667 -0.0728 0.061 Uiso 1 1 calc R . . C16 C 0.3314(14) 0.8291(15) -0.0068(13) 0.279(8) Uani 1 1 d DU . . H16A H 0.2940 0.8615 -0.0129 0.418 Uiso 1 1 calc R . . H16B H 0.3156 0.7909 0.0184 0.418 Uiso 1 1 calc R . . H16C H 0.3468 0.8120 -0.0467 0.418 Uiso 1 1 calc R . . C17 C 0.3889(11) 0.8640(13) 0.0246(9) 0.279(8) Uani 1 1 d DU . . C18 C 0.3848(13) 0.9277(13) 0.0531(11) 0.279(8) Uani 1 1 d DU . . H18 H 0.3434 0.9526 0.0535 0.334 Uiso 1 1 calc R . . C19 C 0.4445(16) 0.9542(12) 0.0814(11) 0.279(8) Uani 1 1 d DU . . H19 H 0.4434 0.9975 0.1009 0.334 Uiso 1 1 calc R . . C20 C 0.5053(12) 0.9158(16) 0.0804(11) 0.279(8) Uani 1 1 d DU . . H20 H 0.5451 0.9331 0.0995 0.334 Uiso 1 1 calc R . . C21 C 0.5071(13) 0.8512(15) 0.0509(13) 0.279(8) Uani 1 1 d DU . . H21 H 0.5483 0.8260 0.0504 0.334 Uiso 1 1 calc R . . C22 C 0.4483(14) 0.8238(12) 0.0221(11) 0.279(8) Uani 1 1 d DU . . H22 H 0.4490 0.7808 0.0022 0.334 Uiso 1 1 calc R . . N1 N 0.1961(3) 0.2337(3) 0.1021(2) 0.0264(12) Uani 1 1 d . . . O1 O 0.1294(2) 0.1760(2) 0.0063(2) 0.0283(10) Uani 1 1 d . . . O2 O 0.0669(2) 0.1724(2) 0.11800(19) 0.0235(9) Uani 1 1 d . . . O3 O 0.0000 0.2500 0.0236(3) 0.0262(13) Uani 1 2 d S . . Sb1 Sb 0.08956(2) 0.25034(2) 0.064691(18) 0.02252(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0968(8) 0.0589(6) 0.0681(7) 0.0356(5) 0.0483(6) 0.0154(5) C1 0.028(4) 0.028(4) 0.041(4) 0.001(3) 0.002(3) -0.002(3) C2 0.036(4) 0.026(3) 0.032(4) 0.001(3) 0.008(3) -0.002(3) C3 0.036(4) 0.049(5) 0.060(5) -0.025(4) 0.004(4) -0.002(4) C4 0.040(5) 0.063(6) 0.108(9) -0.054(6) 0.009(5) 0.005(4) C5 0.027(4) 0.071(7) 0.114(9) -0.044(6) -0.008(5) 0.015(4) C6 0.036(4) 0.038(4) 0.076(6) -0.010(4) -0.003(4) 0.005(3) C7 0.032(4) 0.042(4) 0.065(5) -0.002(4) -0.012(4) 0.005(3) C8 0.041(4) 0.034(4) 0.041(4) 0.005(3) -0.010(3) -0.006(3) C9 0.033(4) 0.031(4) 0.028(3) 0.000(3) -0.002(3) -0.002(3) C10 0.030(3) 0.041(4) 0.020(3) 0.008(3) 0.005(3) 0.005(3) C11 0.042(4) 0.044(4) 0.023(3) 0.005(3) 0.002(3) -0.010(3) C12 0.040(4) 0.047(4) 0.035(4) 0.013(3) 0.003(3) -0.006(3) C13 0.040(4) 0.046(5) 0.045(5) 0.021(4) 0.016(4) 0.005(4) C14 0.084(7) 0.061(6) 0.031(4) 0.014(4) 0.025(4) 0.020(5) C15 0.077(6) 0.040(5) 0.036(4) 0.009(3) 0.021(4) 0.013(4) C16 0.225(15) 0.265(18) 0.346(19) 0.020(14) 0.015(15) 0.051(13) C17 0.225(15) 0.265(18) 0.346(19) 0.020(14) 0.015(15) 0.051(13) C18 0.225(15) 0.265(18) 0.346(19) 0.020(14) 0.015(15) 0.051(13) C19 0.225(15) 0.265(18) 0.346(19) 0.020(14) 0.015(15) 0.051(13) C20 0.225(15) 0.265(18) 0.346(19) 0.020(14) 0.015(15) 0.051(13) C21 0.225(15) 0.265(18) 0.346(19) 0.020(14) 0.015(15) 0.051(13) C22 0.225(15) 0.265(18) 0.346(19) 0.020(14) 0.015(15) 0.051(13) N1 0.029(3) 0.028(3) 0.022(3) 0.002(2) 0.002(2) -0.001(2) O1 0.029(2) 0.033(2) 0.023(2) -0.0017(19) 0.0031(18) -0.0006(19) O2 0.026(2) 0.026(2) 0.019(2) 0.0032(17) 0.0014(17) 0.0043(18) O3 0.024(3) 0.040(4) 0.014(3) 0.000 0.000 0.003(3) Sb1 0.0249(3) 0.0279(3) 0.0148(2) 0.00095(15) 0.00117(15) 0.00125(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C13 1.878(7) . ? C1 N1 1.351(9) . ? C1 C6 1.409(11) . ? C1 C2 1.417(10) . ? C2 O1 1.334(9) . ? C2 C3 1.347(10) . ? C3 C4 1.393(13) . ? C3 H3 0.9300 . ? C4 C5 1.353(14) . ? C4 H4 0.9300 . ? C5 C6 1.398(13) . ? C5 H5 0.9300 . ? C6 C7 1.389(12) . ? C7 C8 1.355(12) . ? C7 H7 0.9300 . ? C8 C9 1.392(10) . ? C8 H8 0.9300 . ? C9 N1 1.302(9) . ? C9 H9 0.9300 . ? C10 C11 1.367(11) . ? C10 C15 1.381(10) . ? C10 Sb1 2.114(7) . ? C11 C12 1.375(10) . ? C11 H11 0.9300 . ? C12 C13 1.355(11) . ? C12 H12 0.9300 . ? C13 C14 1.369(13) . ? C14 C15 1.391(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.458(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.370(9) . ? C17 C22 1.380(10) . ? C18 C19 1.393(9) . ? C18 H18 0.9300 . ? C19 C20 1.383(9) . ? C19 H19 0.9300 . ? C20 C21 1.393(9) . ? C20 H20 0.9300 . ? C21 C22 1.389(10) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? N1 Sb1 2.222(6) . ? O1 Sb1 2.046(5) . ? O2 Sb1 1.933(4) . ? O2 Sb1 1.938(4) 15 ? O3 Sb1 1.933(3) 6_454 ? O3 Sb1 1.933(3) . ? Sb1 O2 1.938(4) 12_666 ? 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 C1 C6 121.2(7) . . ? N1 C1 C2 116.7(6) . . ? C6 C1 C2 122.1(7) . . ? O1 C2 C3 124.2(7) . . ? O1 C2 C1 118.3(6) . . ? C3 C2 C1 117.4(7) . . ? C2 C3 C4 121.0(8) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 122.1(8) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 119.9(8) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 125.2(8) . . ? C7 C6 C1 117.6(8) . . ? C5 C6 C1 117.2(8) . . ? C8 C7 C6 119.3(7) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 120.3(7) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? N1 C9 C8 121.4(7) . . ? N1 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C15 118.6(7) . . ? C11 C10 Sb1 120.3(5) . . ? C15 C10 Sb1 120.8(6) . . ? C10 C11 C12 122.3(7) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 117.7(8) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C12 C13 C14 122.5(7) . . ? C12 C13 Br1 118.9(7) . . ? C14 C13 Br1 118.5(6) . . ? C13 C14 C15 118.5(8) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C10 C15 C14 120.0(8) . . ? C10 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 124.5(15) . . ? C18 C17 C16 124.9(18) . . ? C22 C17 C16 111(2) . . ? C17 C18 C19 118.2(12) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C20 C19 C18 119.6(13) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.3(12) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 121.2(15) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C17 C22 C21 116.3(16) . . ? C17 C22 H22 121.9 . . ? C21 C22 H22 121.9 . . ? C9 N1 C1 120.2(6) . . ? C9 N1 Sb1 128.7(5) . . ? C1 N1 Sb1 111.1(4) . . ? C2 O1 Sb1 116.7(4) . . ? Sb1 O2 Sb1 132.7(2) . 15 ? Sb1 O3 Sb1 126.0(3) 6_454 . ? O2 Sb1 O3 93.67(17) . . ? O2 Sb1 O2 92.73(16) . 12_666 ? O3 Sb1 O2 103.53(17) . 12_666 ? O2 Sb1 O1 84.41(18) . . ? O3 Sb1 O1 93.09(17) . . ? O2 Sb1 O1 163.29(18) 12_666 . ? O2 Sb1 C10 171.1(2) . . ? O3 Sb1 C10 92.3(2) . . ? O2 Sb1 C10 92.2(2) 12_666 . ? O1 Sb1 C10 88.7(2) . . ? O2 Sb1 N1 83.37(19) . . ? O3 Sb1 N1 169.79(16) . . ? O2 Sb1 N1 86.40(19) 12_666 . ? O1 Sb1 N1 76.92(19) . . ? C10 Sb1 N1 89.6(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.237 _refine_diff_density_min -1.289 _refine_diff_density_rms 0.164 #===========================================================================END data_3 _database_code_depnum_ccdc_archive 'CCDC 808829' #TrackingRef '- cif all in one.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H70 Cl4 N10 O11 Sb4' _chemical_formula_sum 'C96 H70 Cl4 N10 O11 Sb4' _chemical_formula_weight 2168.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.029(10) _cell_length_b 21.285(10) _cell_length_c 21.577(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.200(7) _cell_angle_gamma 90.00 _cell_volume 9161(7) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 8750 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.16 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4304 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7378 _exptl_absorpt_correction_T_max 0.8549 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(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 84836 _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16131 _reflns_number_gt 14023 _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. one heavily disorded solvent toluene molecule have been squeezed out for better refinement convergence ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+7.7319P] 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 16131 _refine_ls_number_parameters 1128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.688524(16) 0.669669(13) 0.534854(14) 0.02277(9) Uani 1 1 d . . . Sb3 Sb 0.848376(15) 0.644661(13) 0.607520(14) 0.02229(9) Uani 1 1 d . . . Sb2 Sb 0.712013(15) 0.671678(13) 0.700729(13) 0.02029(9) Uani 1 1 d . . . Sb4 Sb 0.774197(15) 0.795629(13) 0.619306(13) 0.02026(9) Uani 1 1 d . . . O3 O 0.66190(15) 0.66585(14) 0.61998(14) 0.0236(7) Uani 1 1 d . . . O2 O 0.72641(15) 0.75342(13) 0.54791(13) 0.0235(7) Uani 1 1 d . . . O1 O 0.77789(16) 0.63244(14) 0.54058(14) 0.0268(7) Uani 1 1 d . . . O6 O 0.73305(15) 0.75951(13) 0.68860(14) 0.0236(7) Uani 1 1 d . . . O5 O 0.78843(15) 0.62652(13) 0.67170(14) 0.0240(7) Uani 1 1 d . . . O4 O 0.84628(14) 0.73417(14) 0.62535(14) 0.0234(7) Uani 1 1 d . . . Cl3 Cl 0.84463(8) 0.66786(9) 0.99286(7) 0.0618(5) Uani 1 1 d . . . O10 O 0.83794(15) 0.84931(13) 0.67429(14) 0.0235(7) Uani 1 1 d . . . O8 O 0.62365(15) 0.69321(14) 0.73350(14) 0.0241(7) Uani 1 1 d . . . O7 O 0.68627(17) 0.68799(14) 0.44265(14) 0.0292(8) Uani 1 1 d . . . O9 O 0.87006(17) 0.55234(14) 0.60783(14) 0.0289(7) Uani 1 1 d . . . N1 N 0.5919(2) 0.71940(18) 0.51866(18) 0.0284(9) Uani 1 1 d . . . N5 N 0.92735(19) 0.64037(18) 0.68497(19) 0.0279(9) Uani 1 1 d . . . N7 N 0.8327(2) 0.83828(18) 0.54917(19) 0.0289(9) Uani 1 1 d . . . N8 N 0.8121(2) 0.84169(19) 0.48836(18) 0.0321(10) Uani 1 1 d . . . H8 H 0.7729 0.8310 0.4723 0.038 Uiso 1 1 calc R . . N3 N 0.67173(19) 0.57730(17) 0.71480(17) 0.0255(8) Uani 1 1 d . . . N6 N 0.9620(2) 0.69049(19) 0.7080(2) 0.0345(10) Uani 1 1 d . . . H6 H 0.9591 0.7275 0.6921 0.041 Uiso 1 1 calc R . . N2 N 0.5433(2) 0.71766(19) 0.55696(19) 0.0323(10) Uani 1 1 d . . . H2 H 0.5433 0.6932 0.5887 0.039 Uiso 1 1 calc R . . N4 N 0.7091(2) 0.52507(18) 0.72245(19) 0.0331(10) Uani 1 1 d . . . H4 H 0.7521 0.5242 0.7225 0.040 Uiso 1 1 calc R . . C52 C 0.7543(2) 0.6697(2) 0.7941(2) 0.0217(10) Uani 1 1 d . . . C39 C 0.5642(2) 0.6693(2) 0.7144(2) 0.0248(10) Uani 1 1 d . . . C60 C 0.9173(3) 0.8360(2) 0.7858(3) 0.0373(13) Uani 1 1 d . . . H60 H 0.8713 0.8300 0.7854 0.045 Uiso 1 1 calc R . . C20 C 0.8731(2) 0.5154(2) 0.6587(2) 0.0270(10) Uani 1 1 d . . . C30 C 0.9445(2) 0.5922(2) 0.7230(2) 0.0289(11) Uani 1 1 d . . . C21 C 0.8360(2) 0.4579(2) 0.6539(2) 0.0300(11) Uani 1 1 d . . . C58 C 0.9050(2) 0.8507(2) 0.6717(2) 0.0280(11) Uani 1 1 d . . . C14 C 0.6440(2) 0.5814(2) 0.5125(2) 0.0286(11) Uani 1 1 d . . . C38 C 0.9044(3) 0.6901(2) 0.4899(3) 0.0409(14) Uani 1 1 d . . . H38 H 0.8636 0.7112 0.4852 0.049 Uiso 1 1 calc R . . C11 C 0.5750(2) 0.7640(2) 0.4760(2) 0.0287(11) Uani 1 1 d . . . C71 C 0.7074(2) 0.8733(2) 0.6077(2) 0.0239(10) Uani 1 1 d . . . C28 C 0.9163(3) 0.4862(2) 0.7621(2) 0.0360(12) Uani 1 1 d . . . H28 H 0.9424 0.4959 0.7987 0.043 Uiso 1 1 calc R . . C10 C 0.6208(3) 0.7818(2) 0.4301(2) 0.0299(11) Uani 1 1 d . . . C1 C 0.6744(3) 0.7450(2) 0.4173(2) 0.0279(11) Uani 1 1 d . . . C33 C 0.9220(2) 0.6566(2) 0.5443(2) 0.0297(11) Uani 1 1 d . . . C59 C 0.9456(3) 0.8466(2) 0.7297(3) 0.0331(12) Uani 1 1 d . . . C12 C 0.5130(3) 0.7882(2) 0.4876(2) 0.0367(12) Uani 1 1 d . . . H12 H 0.4885 0.8186 0.4644 0.044 Uiso 1 1 calc R . . C70 C 0.8604(3) 0.8637(3) 0.4564(3) 0.0466(15) Uani 1 1 d . . . H70 H 0.8577 0.8698 0.4136 0.056 Uiso 1 1 calc R . . C54 C 0.8488(3) 0.6876(3) 0.8693(2) 0.0382(13) Uani 1 1 d . . . H54 H 0.8930 0.7002 0.8786 0.046 Uiso 1 1 calc R . . C68 C 0.8958(3) 0.8586(2) 0.5560(2) 0.0306(11) Uani 1 1 d . . . C40 C 0.5093(2) 0.7120(2) 0.7033(2) 0.0290(11) Uani 1 1 d . . . C73 C 0.5955(3) 0.9107(3) 0.5788(2) 0.0408(13) Uani 1 1 d . . . H73 H 0.5504 0.9024 0.5678 0.049 Uiso 1 1 calc R . . C31 C 0.9918(3) 0.6127(3) 0.7696(3) 0.0450(14) Uani 1 1 d . . . H31 H 1.0127 0.5888 0.8018 0.054 Uiso 1 1 calc R . . C67 C 0.9347(2) 0.8581(2) 0.6167(3) 0.0352(12) Uani 1 1 d . . . C46 C 0.4345(3) 0.6239(3) 0.6784(2) 0.0376(12) Uani 1 1 d . . . H46 H 0.3917 0.6084 0.6671 0.045 Uiso 1 1 calc R . . C72 C 0.6404(3) 0.8623(2) 0.5918(2) 0.0341(12) Uani 1 1 d . . . H72 H 0.6249 0.8211 0.5897 0.041 Uiso 1 1 calc R . . C48 C 0.5527(2) 0.6047(2) 0.7071(2) 0.0275(10) Uani 1 1 d . . . C37 C 0.9468(4) 0.6924(3) 0.4427(3) 0.0598(19) Uani 1 1 d . . . H37 H 0.9345 0.7145 0.4062 0.072 Uiso 1 1 calc R . . C7 C 0.7103(3) 0.8272(2) 0.3473(2) 0.0390(13) Uani 1 1 d . . . C64 C 1.0161(3) 0.8554(3) 0.7305(3) 0.0449(14) Uani 1 1 d . . . C47 C 0.4864(3) 0.5835(2) 0.6893(2) 0.0342(12) Uani 1 1 d . . . H47 H 0.4785 0.5406 0.6851 0.041 Uiso 1 1 calc R . . C29 C 0.9119(2) 0.5305(2) 0.7128(2) 0.0301(11) Uani 1 1 d . . . C53 C 0.8204(2) 0.6875(2) 0.8084(2) 0.0308(11) Uani 1 1 d . . . H53 H 0.8461 0.6995 0.7767 0.037 Uiso 1 1 calc R . . C45 C 0.4447(3) 0.6892(3) 0.6840(2) 0.0338(12) Uani 1 1 d . . . C2 C 0.7196(3) 0.7667(2) 0.3746(2) 0.0343(12) Uani 1 1 d . . . C9 C 0.6116(3) 0.8414(3) 0.4009(3) 0.0409(13) Uani 1 1 d . . . H9 H 0.5751 0.8660 0.4094 0.049 Uiso 1 1 calc R . . C32 C 1.0014(3) 0.6753(3) 0.7585(3) 0.0462(15) Uani 1 1 d . . . H32 H 1.0302 0.7021 0.7821 0.055 Uiso 1 1 calc R . . C57 C 0.7171(2) 0.6518(2) 0.8422(2) 0.0334(12) Uani 1 1 d . . . H57 H 0.6724 0.6402 0.8334 0.040 Uiso 1 1 calc R . . C56 C 0.7449(3) 0.6507(3) 0.9028(3) 0.0402(13) Uani 1 1 d . . . H56 H 0.7197 0.6380 0.9348 0.048 Uiso 1 1 calc R . . C55 C 0.8108(3) 0.6689(3) 0.9155(2) 0.0358(12) Uani 1 1 d . . . C49 C 0.6077(2) 0.5592(2) 0.7168(2) 0.0291(11) Uani 1 1 d . . . Cl4 Cl 0.56180(9) 1.03303(8) 0.56760(9) 0.0667(5) Uani 1 1 d . . . Cl2 Cl 1.05751(14) 0.66026(12) 0.38913(12) 0.1175(11) Uani 1 1 d . . . C27 C 0.8841(3) 0.4308(2) 0.7578(2) 0.0391(13) Uani 1 1 d . . . H27 H 0.8895 0.4024 0.7906 0.047 Uiso 1 1 calc R . . C25 C 0.8055(3) 0.3587(2) 0.6987(3) 0.0424(14) Uani 1 1 d . . . H25 H 0.8097 0.3298 0.7312 0.051 Uiso 1 1 calc R . . C74 C 0.6185(3) 0.9711(3) 0.5824(3) 0.0410(13) Uani 1 1 d . . . C75 C 0.6848(3) 0.9847(2) 0.5997(3) 0.0446(14) Uani 1 1 d . . . H75 H 0.6994 1.0261 0.6034 0.054 Uiso 1 1 calc R . . C26 C 0.8423(3) 0.4151(2) 0.7042(2) 0.0333(12) Uani 1 1 d . . . C13 C 0.4948(3) 0.7586(2) 0.5398(2) 0.0373(12) Uani 1 1 d . . . H13 H 0.4561 0.7657 0.5595 0.045 Uiso 1 1 calc R . . C41 C 0.5199(3) 0.7768(2) 0.7102(3) 0.0377(12) Uani 1 1 d . . . H41 H 0.5624 0.7920 0.7231 0.045 Uiso 1 1 calc R . . C50 C 0.6066(3) 0.4950(2) 0.7267(3) 0.0411(13) Uani 1 1 d . . . H50 H 0.5689 0.4703 0.7305 0.049 Uiso 1 1 calc R . . C24 C 0.7644(3) 0.3457(3) 0.6474(3) 0.0498(15) Uani 1 1 d . . . H24 H 0.7408 0.3080 0.6447 0.060 Uiso 1 1 calc R . . C51 C 0.6713(3) 0.4749(2) 0.7299(3) 0.0436(14) Uani 1 1 d . . . H51 H 0.6862 0.4338 0.7361 0.052 Uiso 1 1 calc R . . C44 C 0.3925(3) 0.7335(3) 0.6709(3) 0.0424(14) Uani 1 1 d . . . H44 H 0.3496 0.7195 0.6575 0.051 Uiso 1 1 calc R . . C17 C 0.6012(4) 0.4596(3) 0.4943(3) 0.0556(18) Uani 1 1 d . . . C76 C 0.7297(3) 0.9351(2) 0.6117(2) 0.0359(12) Uani 1 1 d . . . H76 H 0.7748 0.9434 0.6225 0.043 Uiso 1 1 calc R . . C42 C 0.4679(3) 0.8175(3) 0.6982(3) 0.0506(16) Uani 1 1 d . . . H42 H 0.4752 0.8604 0.7036 0.061 Uiso 1 1 calc R . . C22 C 0.7927(3) 0.4434(3) 0.6015(3) 0.0452(14) Uani 1 1 d . . . H22 H 0.7881 0.4714 0.5683 0.054 Uiso 1 1 calc R . . C34 C 0.9850(3) 0.6288(3) 0.5525(3) 0.0438(14) Uani 1 1 d . . . H34 H 0.9988 0.6084 0.5895 0.053 Uiso 1 1 calc R . . C8 C 0.6547(3) 0.8632(3) 0.3611(3) 0.0425(14) Uani 1 1 d . . . H8A H 0.6474 0.9024 0.3427 0.051 Uiso 1 1 calc R . . C3 C 0.7744(3) 0.7299(3) 0.3591(2) 0.0463(14) Uani 1 1 d . . . H3 H 0.7809 0.6900 0.3763 0.056 Uiso 1 1 calc R . . C6 C 0.7578(3) 0.8494(3) 0.3085(3) 0.0502(16) Uani 1 1 d . . . H6A H 0.7533 0.8896 0.2917 0.060 Uiso 1 1 calc R . . C61 C 0.9564(3) 0.8344(3) 0.8412(3) 0.0502(16) Uani 1 1 d . . . H61 H 0.9370 0.8268 0.8781 0.060 Uiso 1 1 calc R . . C35 C 1.0274(3) 0.6318(3) 0.5049(3) 0.0622(19) Uani 1 1 d . . . H35 H 1.0697 0.6134 0.5103 0.075 Uiso 1 1 calc R . . C69 C 0.9148(3) 0.8759(3) 0.4972(3) 0.0457(14) Uani 1 1 d . . . H69 H 0.9559 0.8921 0.4880 0.055 Uiso 1 1 calc R . . C23 C 0.7571(3) 0.3885(3) 0.5981(3) 0.0570(17) Uani 1 1 d . . . H23 H 0.7280 0.3797 0.5631 0.068 Uiso 1 1 calc R . . C63 C 1.0548(3) 0.8547(3) 0.7891(4) 0.0598(18) Uani 1 1 d . . . H63 H 1.1008 0.8615 0.7909 0.072 Uiso 1 1 calc R . . C43 C 0.4043(3) 0.7958(3) 0.6779(3) 0.0482(15) Uani 1 1 d . . . H43 H 0.3695 0.8243 0.6690 0.058 Uiso 1 1 calc R . . C66 C 1.0052(3) 0.8652(3) 0.6193(3) 0.0550(16) Uani 1 1 d . . . H66 H 1.0254 0.8705 0.5825 0.066 Uiso 1 1 calc R . . C62 C 1.0256(4) 0.8442(3) 0.8425(3) 0.0597(19) Uani 1 1 d . . . H62 H 1.0518 0.8436 0.8803 0.072 Uiso 1 1 calc R . . C5 C 0.8103(4) 0.8126(3) 0.2952(3) 0.0591(18) Uani 1 1 d . . . H5 H 0.8416 0.8280 0.2697 0.071 Uiso 1 1 calc R . . C19 C 0.6122(4) 0.5489(3) 0.5561(3) 0.076(3) Uani 1 1 d . . . H19 H 0.6044 0.5688 0.5931 0.091 Uiso 1 1 calc R . . C36 C 1.0075(4) 0.6615(3) 0.4507(4) 0.069(2) Uani 1 1 d . . . C18 C 0.5913(5) 0.4877(3) 0.5467(3) 0.078(3) Uani 1 1 d . . . H18 H 0.5703 0.4665 0.5773 0.094 Uiso 1 1 calc R . . Cl1 Cl 0.57806(14) 0.38061(8) 0.48435(9) 0.0956(8) Uani 1 1 d . . . C15 C 0.6535(4) 0.5512(3) 0.4583(3) 0.066(2) Uani 1 1 d . . . H15 H 0.6734 0.5724 0.4271 0.079 Uiso 1 1 calc R . . C16 C 0.6336(5) 0.4887(3) 0.4492(3) 0.082(3) Uani 1 1 d . . . H16 H 0.6422 0.4674 0.4132 0.098 Uiso 1 1 calc R . . C86 C 0.3386(3) 0.9606(3) 0.7820(3) 0.0499(15) Uani 1 1 d . . . C78 C 0.2592(4) 0.9681(3) 0.6899(3) 0.0547(16) Uani 1 1 d . . . C84 C 0.3791(4) 0.9697(3) 0.6801(3) 0.0592(18) Uani 1 1 d . . . H84 H 0.4147 0.9710 0.6552 0.071 Uiso 1 1 calc R . . C77 C 0.2737(3) 0.9610(3) 0.7547(3) 0.0530(16) Uani 1 1 d . . . C85 C 0.3914(3) 0.9653(3) 0.7430(3) 0.0571(17) Uani 1 1 d . . . H85 H 0.4355 0.9655 0.7607 0.069 Uiso 1 1 calc R . . C83 C 0.3127(4) 0.9721(3) 0.6523(3) 0.0579(17) Uani 1 1 d . . . C82 C 0.2976(5) 0.9806(3) 0.5872(4) 0.072(2) Uani 1 1 d . . . H82 H 0.3323 0.9824 0.5614 0.086 Uiso 1 1 calc R . . C81 C 0.2339(5) 0.9862(4) 0.5626(4) 0.084(2) Uani 1 1 d . . . H81 H 0.2252 0.9922 0.5199 0.101 Uiso 1 1 calc R . . C79 C 0.1931(4) 0.9745(3) 0.6621(3) 0.071(2) Uani 1 1 d . . . H79 H 0.1575 0.9728 0.6869 0.085 Uiso 1 1 calc R . . C80 C 0.1805(5) 0.9832(4) 0.5998(4) 0.084(2) Uani 1 1 d . . . H80 H 0.1366 0.9870 0.5821 0.101 Uiso 1 1 calc R . . O11 O 0.2196(2) 0.9544(3) 0.7880(2) 0.0757(15) Uani 1 1 d . . . H11 H 0.2320 0.9536 0.8252 0.114 Uiso 1 1 calc R . . N9 N 0.3042(3) 0.9414(2) 0.8859(3) 0.0584(14) Uani 1 1 d . . . C87 C 0.3531(3) 0.9583(3) 0.8496(3) 0.0570(17) Uani 1 1 d . . . C88 C 0.4115(4) 0.9740(3) 0.8877(4) 0.072(2) Uani 1 1 d . . . H88 H 0.4526 0.9868 0.8750 0.086 Uiso 1 1 calc R . . N10 N 0.3317(3) 0.9474(3) 0.9447(3) 0.0673(16) Uani 1 1 d . . . H10 H 0.3107 0.9396 0.9769 0.081 Uiso 1 1 calc R . . C89 C 0.3950(4) 0.9666(3) 0.9475(4) 0.073(2) Uani 1 1 d . . . H89 H 0.4230 0.9737 0.9836 0.087 Uiso 1 1 calc R . . C4 C 0.8176(4) 0.7521(3) 0.3195(3) 0.0582(17) Uani 1 1 d . . . H4A H 0.8524 0.7267 0.3084 0.070 Uiso 1 1 calc R . . C95 C 0.0726(4) 0.8540(5) 0.4375(4) 0.076(2) Uani 1 1 d . . . C94 C 0.0851(4) 0.9154(5) 0.4536(4) 0.089(3) Uani 1 1 d . . . H94 H 0.1138 0.9252 0.4886 0.107 Uiso 1 1 calc R . . C90 C 0.0294(4) 0.8409(5) 0.3860(4) 0.077(2) Uani 1 1 d . . . H90 H 0.0208 0.7993 0.3747 0.092 Uiso 1 1 calc R . . C92 C 0.0100(6) 0.9477(6) 0.3670(5) 0.105(3) Uani 1 1 d . . . H92 H -0.0129 0.9788 0.3434 0.126 Uiso 1 1 calc R . . C91 C 0.0002(4) 0.8861(5) 0.3527(4) 0.078(2) Uani 1 1 d . . . H91 H -0.0283 0.8757 0.3178 0.093 Uiso 1 1 calc R . . C96 C 0.1005(6) 0.8008(7) 0.4770(7) 0.155(5) Uani 1 1 d . . . H96A H 0.0646 0.7788 0.4941 0.232 Uiso 1 1 calc R . . H96B H 0.1309 0.8169 0.5102 0.232 Uiso 1 1 calc R . . H96C H 0.1241 0.7725 0.4520 0.232 Uiso 1 1 calc R . . C93 C 0.0544(7) 0.9632(5) 0.4169(7) 0.124(5) Uani 1 1 d . . . H93 H 0.0639 1.0051 0.4262 0.148 Uiso 1 1 calc R . . C65 C 1.0435(3) 0.8645(3) 0.6733(3) 0.0630(19) Uani 1 1 d . . . H65 H 1.0895 0.8702 0.6731 0.076 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 Sb1 0.02758(18) 0.01877(16) 0.02125(17) -0.00056(11) -0.00165(13) -0.00234(12) Sb3 0.02390(17) 0.01872(16) 0.02457(17) -0.00012(12) 0.00388(13) 0.00166(12) Sb2 0.02076(17) 0.01884(16) 0.02117(16) 0.00054(11) 0.00126(12) -0.00040(11) Sb4 0.02113(17) 0.01624(15) 0.02331(17) -0.00063(11) 0.00146(12) -0.00098(11) O3 0.0244(17) 0.0267(17) 0.0188(16) 0.0002(13) -0.0025(13) -0.0057(13) O2 0.0289(18) 0.0195(15) 0.0209(16) -0.0027(12) -0.0039(13) -0.0058(13) O1 0.0279(18) 0.0239(16) 0.0286(18) -0.0035(13) 0.0029(14) 0.0005(14) O6 0.0294(18) 0.0146(15) 0.0272(17) 0.0005(12) 0.0047(14) -0.0019(13) O5 0.0229(17) 0.0202(15) 0.0300(17) 0.0031(13) 0.0083(14) 0.0006(13) O4 0.0191(16) 0.0195(15) 0.0315(17) -0.0013(13) 0.0014(13) 0.0020(12) Cl3 0.0447(9) 0.1106(14) 0.0281(7) 0.0063(8) -0.0081(7) -0.0107(9) O10 0.0220(17) 0.0210(16) 0.0271(17) -0.0050(13) 0.0001(13) -0.0036(13) O8 0.0196(17) 0.0252(16) 0.0276(17) -0.0011(13) 0.0029(13) -0.0004(13) O7 0.046(2) 0.0235(17) 0.0172(16) 0.0020(13) -0.0023(15) -0.0013(15) O9 0.041(2) 0.0173(16) 0.0285(18) -0.0004(13) 0.0051(15) 0.0038(14) N1 0.027(2) 0.031(2) 0.027(2) 0.0016(17) -0.0037(18) -0.0019(17) N5 0.021(2) 0.027(2) 0.035(2) -0.0039(17) -0.0025(17) 0.0053(17) N7 0.031(2) 0.025(2) 0.031(2) 0.0005(17) 0.0045(18) -0.0046(17) N8 0.036(3) 0.036(2) 0.023(2) 0.0031(17) 0.0007(19) -0.0035(19) N3 0.028(2) 0.021(2) 0.027(2) 0.0038(16) 0.0044(17) 0.0025(17) N6 0.032(2) 0.025(2) 0.045(3) 0.0001(19) -0.004(2) -0.0052(18) N2 0.031(2) 0.036(2) 0.029(2) 0.0003(18) -0.0012(19) -0.0065(19) N4 0.032(2) 0.025(2) 0.043(3) 0.0012(18) 0.0091(19) 0.0027(18) C52 0.022(2) 0.024(2) 0.018(2) 0.0031(17) -0.0010(18) 0.0046(18) C39 0.022(3) 0.027(2) 0.025(2) 0.0009(19) 0.005(2) -0.0039(19) C60 0.043(3) 0.025(3) 0.041(3) -0.002(2) -0.008(3) -0.002(2) C20 0.027(3) 0.021(2) 0.034(3) 0.002(2) 0.008(2) 0.0097(19) C30 0.028(3) 0.025(2) 0.034(3) 0.000(2) 0.003(2) 0.004(2) C21 0.032(3) 0.021(2) 0.038(3) 0.001(2) 0.009(2) 0.007(2) C58 0.025(3) 0.018(2) 0.040(3) -0.005(2) 0.002(2) -0.0025(19) C14 0.034(3) 0.022(2) 0.028(3) -0.0028(19) -0.005(2) -0.007(2) C38 0.046(3) 0.030(3) 0.051(3) 0.009(2) 0.025(3) 0.017(2) C11 0.032(3) 0.027(3) 0.024(2) -0.003(2) -0.009(2) -0.005(2) C71 0.027(3) 0.020(2) 0.025(2) 0.0026(18) 0.002(2) 0.0047(19) C28 0.041(3) 0.035(3) 0.031(3) 0.006(2) 0.002(2) 0.009(2) C10 0.035(3) 0.028(3) 0.025(2) -0.001(2) -0.008(2) -0.001(2) C1 0.041(3) 0.023(2) 0.018(2) 0.0034(18) -0.006(2) -0.007(2) C33 0.029(3) 0.027(2) 0.035(3) 0.002(2) 0.016(2) 0.006(2) C59 0.032(3) 0.019(2) 0.047(3) -0.006(2) -0.004(2) 0.000(2) C12 0.031(3) 0.039(3) 0.038(3) 0.003(2) -0.008(2) 0.000(2) C70 0.055(4) 0.050(4) 0.036(3) 0.009(3) 0.012(3) -0.005(3) C54 0.022(3) 0.051(3) 0.041(3) 0.003(3) 0.000(2) -0.005(2) C68 0.032(3) 0.030(3) 0.031(3) -0.003(2) 0.008(2) -0.002(2) C40 0.025(3) 0.034(3) 0.028(3) 0.000(2) 0.003(2) 0.003(2) C73 0.028(3) 0.049(3) 0.042(3) -0.010(3) -0.011(2) 0.006(2) C31 0.044(3) 0.041(3) 0.046(3) -0.001(3) -0.014(3) 0.006(3) C67 0.023(3) 0.037(3) 0.046(3) -0.003(2) 0.005(2) -0.005(2) C46 0.023(3) 0.047(3) 0.042(3) 0.000(2) -0.002(2) -0.007(2) C72 0.032(3) 0.026(3) 0.043(3) -0.008(2) -0.001(2) 0.001(2) C48 0.029(3) 0.028(2) 0.026(2) 0.0004(19) 0.004(2) 0.001(2) C37 0.078(5) 0.051(4) 0.056(4) 0.020(3) 0.036(4) 0.025(3) C7 0.054(4) 0.041(3) 0.021(3) 0.006(2) -0.004(2) -0.009(3) C64 0.030(3) 0.045(3) 0.057(4) -0.003(3) -0.008(3) -0.002(2) C47 0.035(3) 0.030(3) 0.037(3) -0.004(2) 0.001(2) -0.010(2) C29 0.029(3) 0.030(3) 0.031(3) 0.002(2) 0.007(2) 0.009(2) C53 0.025(3) 0.035(3) 0.032(3) 0.005(2) -0.002(2) -0.002(2) C45 0.033(3) 0.044(3) 0.024(3) -0.001(2) -0.002(2) 0.000(2) C2 0.048(3) 0.029(3) 0.025(3) 0.000(2) -0.002(2) 0.000(2) C9 0.039(3) 0.036(3) 0.046(3) 0.005(2) 0.000(3) 0.003(2) C32 0.038(3) 0.041(3) 0.057(4) -0.006(3) -0.012(3) -0.003(3) C57 0.022(3) 0.051(3) 0.027(3) 0.003(2) 0.000(2) -0.004(2) C56 0.033(3) 0.056(4) 0.033(3) 0.003(3) 0.012(2) -0.005(3) C55 0.029(3) 0.052(3) 0.025(3) -0.001(2) -0.006(2) -0.001(2) C49 0.035(3) 0.030(3) 0.023(2) 0.0001(19) 0.005(2) -0.007(2) Cl4 0.0735(12) 0.0490(9) 0.0743(11) 0.0044(8) -0.0120(9) 0.0348(8) Cl2 0.137(2) 0.1150(18) 0.1166(19) 0.0458(15) 0.1025(18) 0.0638(16) C27 0.049(3) 0.037(3) 0.034(3) 0.014(2) 0.014(3) 0.009(3) C25 0.051(4) 0.029(3) 0.051(4) 0.009(2) 0.026(3) 0.003(3) C74 0.045(3) 0.037(3) 0.040(3) 0.002(2) -0.003(3) 0.016(3) C75 0.054(4) 0.019(3) 0.062(4) 0.009(2) 0.010(3) 0.005(2) C26 0.034(3) 0.022(2) 0.046(3) 0.002(2) 0.015(2) 0.008(2) C13 0.025(3) 0.043(3) 0.043(3) -0.002(2) -0.004(2) -0.003(2) C41 0.027(3) 0.036(3) 0.051(3) -0.006(2) 0.005(2) -0.001(2) C50 0.038(3) 0.023(3) 0.064(4) 0.009(2) 0.014(3) -0.003(2) C24 0.053(4) 0.030(3) 0.068(4) -0.004(3) 0.014(3) -0.005(3) C51 0.048(4) 0.019(3) 0.065(4) 0.009(2) 0.014(3) 0.001(2) C44 0.019(3) 0.062(4) 0.045(3) 0.000(3) -0.002(2) 0.005(3) C17 0.091(5) 0.033(3) 0.039(3) -0.001(3) -0.016(3) -0.026(3) C76 0.034(3) 0.026(3) 0.048(3) 0.002(2) 0.006(2) -0.002(2) C42 0.047(4) 0.034(3) 0.071(4) 0.005(3) 0.005(3) 0.014(3) C22 0.054(4) 0.032(3) 0.050(4) 0.001(3) 0.006(3) -0.004(3) C34 0.041(3) 0.041(3) 0.052(4) 0.016(3) 0.017(3) 0.009(3) C8 0.054(4) 0.031(3) 0.042(3) 0.012(2) 0.000(3) 0.002(3) C3 0.068(4) 0.042(3) 0.031(3) 0.009(2) 0.012(3) 0.004(3) C6 0.068(4) 0.046(3) 0.037(3) 0.012(3) 0.005(3) -0.007(3) C61 0.067(5) 0.036(3) 0.044(4) 0.003(3) -0.013(3) -0.001(3) C35 0.059(4) 0.051(4) 0.082(5) 0.014(4) 0.037(4) 0.030(3) C69 0.039(3) 0.052(4) 0.049(4) 0.005(3) 0.021(3) -0.011(3) C23 0.061(4) 0.036(3) 0.072(4) -0.004(3) -0.010(3) -0.011(3) C63 0.036(4) 0.062(4) 0.078(5) 0.001(4) -0.015(3) -0.005(3) C43 0.034(3) 0.053(4) 0.057(4) 0.009(3) 0.001(3) 0.019(3) C66 0.041(4) 0.072(4) 0.053(4) -0.001(3) 0.013(3) -0.012(3) C62 0.061(5) 0.048(4) 0.063(5) 0.003(3) -0.032(4) 0.001(3) C5 0.074(5) 0.064(4) 0.044(4) 0.016(3) 0.026(3) -0.006(4) C19 0.143(7) 0.045(4) 0.043(4) -0.016(3) 0.027(4) -0.050(4) C36 0.090(6) 0.050(4) 0.075(5) 0.017(4) 0.054(4) 0.027(4) C18 0.144(8) 0.053(4) 0.042(4) -0.007(3) 0.028(4) -0.047(5) Cl1 0.180(2) 0.0468(10) 0.0564(11) -0.0070(8) -0.0104(13) -0.0606(13) C15 0.118(6) 0.045(4) 0.037(3) -0.007(3) 0.013(4) -0.039(4) C16 0.149(8) 0.055(4) 0.043(4) -0.021(3) 0.016(4) -0.044(5) C86 0.059(4) 0.038(3) 0.053(4) 0.006(3) 0.005(3) -0.004(3) C78 0.068(5) 0.034(3) 0.062(4) -0.005(3) 0.006(4) -0.012(3) C84 0.075(5) 0.034(3) 0.072(5) 0.004(3) 0.026(4) 0.004(3) C77 0.057(4) 0.046(4) 0.059(4) 0.005(3) 0.015(3) -0.012(3) C85 0.059(4) 0.042(4) 0.072(5) 0.007(3) 0.014(4) 0.010(3) C83 0.078(5) 0.031(3) 0.067(4) -0.006(3) 0.016(4) -0.009(3) C82 0.098(6) 0.052(4) 0.066(5) -0.005(4) 0.010(4) -0.019(4) C81 0.112(8) 0.073(5) 0.067(5) -0.001(4) 0.001(5) -0.016(5) C79 0.083(6) 0.070(5) 0.059(5) 0.003(4) 0.002(4) -0.019(4) C80 0.092(6) 0.081(6) 0.077(6) 0.003(5) -0.013(5) -0.012(5) O11 0.064(3) 0.106(4) 0.057(3) 0.014(3) 0.002(2) -0.017(3) N9 0.069(4) 0.047(3) 0.059(4) 0.010(3) 0.010(3) -0.007(3) C87 0.063(4) 0.038(3) 0.069(4) 0.013(3) 0.002(4) -0.002(3) C88 0.077(5) 0.059(4) 0.076(5) 0.032(4) -0.009(4) -0.015(4) N10 0.085(5) 0.060(4) 0.055(4) 0.016(3) 0.001(3) -0.007(3) C89 0.084(6) 0.064(5) 0.065(5) 0.030(4) -0.019(4) -0.021(4) C4 0.071(5) 0.062(4) 0.044(4) 0.008(3) 0.022(3) 0.011(3) C95 0.044(4) 0.106(7) 0.080(6) 0.010(5) 0.021(4) 0.000(4) C94 0.062(5) 0.117(8) 0.094(7) -0.051(6) 0.035(5) -0.041(5) C90 0.061(5) 0.105(7) 0.067(5) -0.011(5) 0.018(4) -0.019(5) C92 0.106(8) 0.117(9) 0.100(8) -0.013(7) 0.053(7) -0.027(7) C91 0.075(6) 0.101(7) 0.062(5) -0.004(5) 0.031(4) -0.017(5) C96 0.095(9) 0.202(15) 0.167(13) 0.014(11) 0.012(9) -0.008(9) C93 0.139(11) 0.071(7) 0.176(13) -0.029(8) 0.100(10) -0.026(7) C65 0.027(3) 0.086(5) 0.077(5) 0.001(4) 0.007(3) -0.009(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 Sb1 O2 1.948(3) . ? Sb1 O1 1.951(3) . ? Sb1 O3 1.960(3) . ? Sb1 O7 2.024(3) . ? Sb1 C14 2.116(5) . ? Sb1 N1 2.206(4) . ? Sb3 O1 1.943(3) . ? Sb3 O4 1.945(3) . ? Sb3 O5 1.952(3) . ? Sb3 O9 2.012(3) . ? Sb3 C33 2.113(5) . ? Sb3 N5 2.196(4) . ? Sb2 O3 1.934(3) . ? Sb2 O6 1.939(3) . ? Sb2 O5 1.958(3) . ? Sb2 O8 2.017(3) . ? Sb2 C52 2.114(4) . ? Sb2 N3 2.196(4) . ? Sb4 O6 1.931(3) . ? Sb4 O4 1.944(3) . ? Sb4 O2 1.957(3) . ? Sb4 O10 2.017(3) . ? Sb4 C71 2.128(4) . ? Sb4 N7 2.192(4) . ? Cl3 C55 1.745(5) . ? O10 C58 1.349(6) . ? O8 C39 1.326(5) . ? O7 C1 1.343(5) . ? O9 C20 1.346(5) . ? N1 N2 1.332(6) . ? N1 C11 1.345(6) . ? N5 C30 1.339(6) . ? N5 N6 1.344(5) . ? N7 C68 1.331(6) . ? N7 N8 1.341(6) . ? N8 C70 1.324(7) . ? N8 H8 0.8600 . ? N3 N4 1.342(5) . ? N3 C49 1.344(6) . ? N6 C32 1.327(7) . ? N6 H6 0.8600 . ? N2 C13 1.332(6) . ? N2 H2 0.8600 . ? N4 C51 1.328(6) . ? N4 H4 0.8600 . ? C52 C57 1.386(6) . ? C52 C53 1.386(7) . ? C39 C48 1.400(6) . ? C39 C40 1.428(7) . ? C60 C61 1.369(8) . ? C60 C59 1.400(8) . ? C60 H60 0.9300 . ? C20 C29 1.381(7) . ? C20 C21 1.430(7) . ? C30 C31 1.388(7) . ? C30 C29 1.474(7) . ? C21 C22 1.397(8) . ? C21 C26 1.413(7) . ? C58 C67 1.384(7) . ? C58 C59 1.434(7) . ? C14 C15 1.363(7) . ? C14 C19 1.370(8) . ? C38 C37 1.384(8) . ? C38 C33 1.392(7) . ? C38 H38 0.9300 . ? C11 C12 1.388(7) . ? C11 C10 1.459(7) . ? C71 C72 1.375(7) . ? C71 C76 1.388(7) . ? C28 C27 1.345(7) . ? C28 C29 1.417(7) . ? C28 H28 0.9300 . ? C10 C1 1.377(7) . ? C10 C9 1.422(7) . ? C1 C2 1.426(7) . ? C33 C34 1.391(7) . ? C59 C64 1.423(7) . ? C12 C13 1.368(7) . ? C12 H12 0.9300 . ? C70 C69 1.361(8) . ? C70 H70 0.9300 . ? C54 C55 1.368(7) . ? C54 C53 1.382(7) . ? C54 H54 0.9300 . ? C68 C69 1.407(7) . ? C68 C67 1.462(7) . ? C40 C41 1.402(7) . ? C40 C45 1.408(7) . ? C73 C74 1.364(8) . ? C73 C72 1.380(7) . ? C73 H73 0.9300 . ? C31 C32 1.370(8) . ? C31 H31 0.9300 . ? C67 C66 1.417(8) . ? C46 C47 1.352(7) . ? C46 C45 1.410(7) . ? C46 H46 0.9300 . ? C72 H72 0.9300 . ? C48 C47 1.423(7) . ? C48 C49 1.467(7) . ? C37 C36 1.381(10) . ? C37 H37 0.9300 . ? C7 C6 1.405(8) . ? C7 C8 1.406(8) . ? C7 C2 1.421(7) . ? C64 C65 1.410(9) . ? C64 C63 1.422(9) . ? C47 H47 0.9300 . ? C53 H53 0.9300 . ? C45 C44 1.417(7) . ? C2 C3 1.414(8) . ? C9 C8 1.353(8) . ? C9 H9 0.9300 . ? C32 H32 0.9300 . ? C57 C56 1.375(7) . ? C57 H57 0.9300 . ? C56 C55 1.378(7) . ? C56 H56 0.9300 . ? C49 C50 1.384(7) . ? Cl4 C74 1.751(5) . ? Cl2 C36 1.735(6) . ? C27 C26 1.404(8) . ? C27 H27 0.9300 . ? C25 C24 1.347(9) . ? C25 C26 1.408(7) . ? C25 H25 0.9300 . ? C74 C75 1.378(8) . ? C75 C76 1.395(7) . ? C75 H75 0.9300 . ? C13 H13 0.9300 . ? C41 C42 1.361(8) . ? C41 H41 0.9300 . ? C50 C51 1.360(8) . ? C50 H50 0.9300 . ? C24 C23 1.398(9) . ? C24 H24 0.9300 . ? C51 H51 0.9300 . ? C44 C43 1.354(8) . ? C44 H44 0.9300 . ? C17 C18 1.309(9) . ? C17 C16 1.367(9) . ? C17 Cl1 1.753(6) . ? C76 H76 0.9300 . ? C42 C43 1.389(9) . ? C42 H42 0.9300 . ? C22 C23 1.367(8) . ? C22 H22 0.9300 . ? C34 C35 1.392(8) . ? C34 H34 0.9300 . ? C8 H8A 0.9300 . ? C3 C4 1.357(8) . ? C3 H3 0.9300 . ? C6 C5 1.364(9) . ? C6 H6A 0.9300 . ? C61 C62 1.398(9) . ? C61 H61 0.9300 . ? C35 C36 1.356(10) . ? C35 H35 0.9300 . ? C69 H69 0.9300 . ? C23 H23 0.9300 . ? C63 C62 1.357(10) . ? C63 H63 0.9300 . ? C43 H43 0.9300 . ? C66 C65 1.335(9) . ? C66 H66 0.9300 . ? C62 H62 0.9300 . ? C5 C4 1.394(9) . ? C5 H5 0.9300 . ? C19 C18 1.378(8) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C15 C16 1.397(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C86 C77 1.378(9) . ? C86 C85 1.414(9) . ? C86 C87 1.460(9) . ? C78 C83 1.405(9) . ? C78 C79 1.408(10) . ? C78 C77 1.411(9) . ? C84 C85 1.361(9) . ? C84 C83 1.408(10) . ? C84 H84 0.9300 . ? C77 O11 1.360(7) . ? C85 H85 0.9300 . ? C83 C82 1.422(10) . ? C82 C81 1.341(11) . ? C82 H82 0.9300 . ? C81 C80 1.397(12) . ? C81 H81 0.9300 . ? C79 C80 1.358(10) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? O11 H11 0.8200 . ? N9 N10 1.344(7) . ? N9 C87 1.357(8) . ? C87 C88 1.409(10) . ? C88 C89 1.371(10) . ? C88 H88 0.9300 . ? N10 C89 1.328(9) . ? N10 H10 0.8600 . ? C89 H89 0.9300 . ? C4 H4A 0.9300 . ? C95 C94 1.370(12) . ? C95 C90 1.373(11) . ? C95 C96 1.496(14) . ? C94 C93 1.398(15) . ? C94 H94 0.9300 . ? C90 C91 1.308(11) . ? C90 H90 0.9300 . ? C92 C91 1.357(13) . ? C92 C93 1.374(15) . ? C92 H92 0.9300 . ? C91 H91 0.9300 . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? C93 H93 0.9300 . ? C65 H65 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sb1 O1 91.11(13) . . ? O2 Sb1 O3 92.17(12) . . ? O1 Sb1 O3 104.46(13) . . ? O2 Sb1 O7 86.54(12) . . ? O1 Sb1 O7 94.54(14) . . ? O3 Sb1 O7 160.98(13) . . ? O2 Sb1 C14 174.81(15) . . ? O1 Sb1 C14 91.11(16) . . ? O3 Sb1 C14 91.83(16) . . ? O7 Sb1 C14 88.60(16) . . ? O2 Sb1 N1 84.76(14) . . ? O1 Sb1 N1 172.59(14) . . ? O3 Sb1 N1 81.89(14) . . ? O7 Sb1 N1 79.10(14) . . ? C14 Sb1 N1 92.52(17) . . ? O1 Sb3 O4 104.53(13) . . ? O1 Sb3 O5 92.79(14) . . ? O4 Sb3 O5 91.59(12) . . ? O1 Sb3 O9 90.79(13) . . ? O4 Sb3 O9 164.68(13) . . ? O5 Sb3 O9 87.18(12) . . ? O1 Sb3 C33 92.22(18) . . ? O4 Sb3 C33 92.23(16) . . ? O5 Sb3 C33 172.74(16) . . ? O9 Sb3 C33 87.50(16) . . ? O1 Sb3 N5 169.88(13) . . ? O4 Sb3 N5 85.25(13) . . ? O5 Sb3 N5 84.19(14) . . ? O9 Sb3 N5 79.43(14) . . ? C33 Sb3 N5 89.98(18) . . ? O3 Sb2 O6 92.38(13) . . ? O3 Sb2 O5 92.14(13) . . ? O6 Sb2 O5 104.15(13) . . ? O3 Sb2 O8 85.99(13) . . ? O6 Sb2 O8 92.10(12) . . ? O5 Sb2 O8 163.72(12) . . ? O3 Sb2 C52 170.93(15) . . ? O6 Sb2 C52 94.31(15) . . ? O5 Sb2 C52 92.16(15) . . ? O8 Sb2 C52 87.65(15) . . ? O3 Sb2 N3 84.19(13) . . ? O6 Sb2 N3 170.92(13) . . ? O5 Sb2 N3 84.42(13) . . ? O8 Sb2 N3 79.30(13) . . ? C52 Sb2 N3 88.28(15) . . ? O6 Sb4 O4 92.67(13) . . ? O6 Sb4 O2 102.36(13) . . ? O4 Sb4 O2 92.93(13) . . ? O6 Sb4 O10 93.55(13) . . ? O4 Sb4 O10 85.13(13) . . ? O2 Sb4 O10 164.05(12) . . ? O6 Sb4 C71 95.29(15) . . ? O4 Sb4 C71 170.51(15) . . ? O2 Sb4 C71 90.39(15) . . ? O10 Sb4 C71 89.23(15) . . ? O6 Sb4 N7 172.48(14) . . ? O4 Sb4 N7 83.40(14) . . ? O2 Sb4 N7 84.29(14) . . ? O10 Sb4 N7 79.76(14) . . ? C71 Sb4 N7 88.10(16) . . ? Sb2 O3 Sb1 132.72(17) . . ? Sb1 O2 Sb4 133.66(16) . . ? Sb3 O1 Sb1 126.38(16) . . ? Sb4 O6 Sb2 126.98(15) . . ? Sb3 O5 Sb2 132.75(16) . . ? Sb4 O4 Sb3 132.47(16) . . ? C58 O10 Sb4 124.5(3) . . ? C39 O8 Sb2 126.6(3) . . ? C1 O7 Sb1 124.1(3) . . ? C20 O9 Sb3 124.5(3) . . ? N2 N1 C11 107.0(4) . . ? N2 N1 Sb1 124.6(3) . . ? C11 N1 Sb1 127.6(3) . . ? C30 N5 N6 106.7(4) . . ? C30 N5 Sb3 128.7(3) . . ? N6 N5 Sb3 124.1(3) . . ? C68 N7 N8 107.1(4) . . ? C68 N7 Sb4 128.3(3) . . ? N8 N7 Sb4 124.2(3) . . ? C70 N8 N7 110.7(4) . . ? C70 N8 H8 124.6 . . ? N7 N8 H8 124.6 . . ? N4 N3 C49 106.4(4) . . ? N4 N3 Sb2 124.5(3) . . ? C49 N3 Sb2 129.1(3) . . ? C32 N6 N5 111.1(4) . . ? C32 N6 H6 124.5 . . ? N5 N6 H6 124.5 . . ? C13 N2 N1 111.3(4) . . ? C13 N2 H2 124.3 . . ? N1 N2 H2 124.3 . . ? C51 N4 N3 111.3(4) . . ? C51 N4 H4 124.4 . . ? N3 N4 H4 124.4 . . ? C57 C52 C53 118.5(4) . . ? C57 C52 Sb2 121.6(3) . . ? C53 C52 Sb2 120.0(3) . . ? O8 C39 C48 123.0(4) . . ? O8 C39 C40 117.6(4) . . ? C48 C39 C40 119.3(4) . . ? C61 C60 C59 121.0(6) . . ? C61 C60 H60 119.5 . . ? C59 C60 H60 119.5 . . ? O9 C20 C29 122.3(4) . . ? O9 C20 C21 117.1(4) . . ? C29 C20 C21 120.5(4) . . ? N5 C30 C31 108.8(4) . . ? N5 C30 C29 120.4(4) . . ? C31 C30 C29 130.7(5) . . ? C22 C21 C26 118.9(5) . . ? C22 C21 C20 121.9(5) . . ? C26 C21 C20 119.2(5) . . ? O10 C58 C67 123.1(4) . . ? O10 C58 C59 116.8(4) . . ? C67 C58 C59 120.1(5) . . ? C15 C14 C19 117.4(5) . . ? C15 C14 Sb1 121.7(4) . . ? C19 C14 Sb1 120.3(4) . . ? C37 C38 C33 120.9(5) . . ? C37 C38 H38 119.6 . . ? C33 C38 H38 119.6 . . ? N1 C11 C12 108.1(4) . . ? N1 C11 C10 120.9(4) . . ? C12 C11 C10 130.9(5) . . ? C72 C71 C76 118.6(4) . . ? C72 C71 Sb4 119.0(3) . . ? C76 C71 Sb4 122.2(4) . . ? C27 C28 C29 122.3(5) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C1 C10 C9 119.4(5) . . ? C1 C10 C11 122.5(4) . . ? C9 C10 C11 117.9(5) . . ? O7 C1 C10 123.0(4) . . ? O7 C1 C2 117.1(4) . . ? C10 C1 C2 119.8(4) . . ? C34 C33 C38 118.8(5) . . ? C34 C33 Sb3 123.1(4) . . ? C38 C33 Sb3 117.9(4) . . ? C60 C59 C64 119.3(5) . . ? C60 C59 C58 121.5(5) . . ? C64 C59 C58 119.1(5) . . ? C13 C12 C11 106.7(5) . . ? C13 C12 H12 126.7 . . ? C11 C12 H12 126.7 . . ? N8 C70 C69 108.2(5) . . ? N8 C70 H70 125.9 . . ? C69 C70 H70 125.9 . . ? C55 C54 C53 118.9(5) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? N7 C68 C69 108.5(5) . . ? N7 C68 C67 121.3(4) . . ? C69 C68 C67 130.1(5) . . ? C41 C40 C45 119.7(5) . . ? C41 C40 C39 120.1(5) . . ? C45 C40 C39 120.2(4) . . ? C74 C73 C72 118.9(5) . . ? C74 C73 H73 120.6 . . ? C72 C73 H73 120.6 . . ? C32 C31 C30 106.2(5) . . ? C32 C31 H31 126.9 . . ? C30 C31 H31 126.9 . . ? C58 C67 C66 118.8(5) . . ? C58 C67 C68 122.2(4) . . ? C66 C67 C68 119.0(5) . . ? C47 C46 C45 120.6(5) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C71 C72 C73 121.7(5) . . ? C71 C72 H72 119.2 . . ? C73 C72 H72 119.2 . . ? C39 C48 C47 118.8(4) . . ? C39 C48 C49 121.3(4) . . ? C47 C48 C49 119.9(4) . . ? C36 C37 C38 118.9(6) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C6 C7 C8 122.3(5) . . ? C6 C7 C2 118.9(5) . . ? C8 C7 C2 118.8(5) . . ? C65 C64 C63 123.8(6) . . ? C65 C64 C59 118.2(5) . . ? C63 C64 C59 118.0(6) . . ? C46 C47 C48 121.9(5) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C20 C29 C28 118.2(5) . . ? C20 C29 C30 122.7(4) . . ? C28 C29 C30 118.9(5) . . ? C54 C53 C52 121.0(5) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C40 C45 C46 119.1(5) . . ? C40 C45 C44 118.2(5) . . ? C46 C45 C44 122.6(5) . . ? C3 C2 C7 118.7(5) . . ? C3 C2 C1 121.7(5) . . ? C7 C2 C1 119.7(5) . . ? C8 C9 C10 121.5(5) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? N6 C32 C31 107.3(5) . . ? N6 C32 H32 126.3 . . ? C31 C32 H32 126.3 . . ? C56 C57 C52 121.2(5) . . ? C56 C57 H57 119.4 . . ? C52 C57 H57 119.4 . . ? C57 C56 C55 118.8(5) . . ? C57 C56 H56 120.6 . . ? C55 C56 H56 120.6 . . ? C54 C55 C56 121.6(5) . . ? C54 C55 Cl3 120.5(4) . . ? C56 C55 Cl3 117.9(4) . . ? N3 C49 C50 108.4(4) . . ? N3 C49 C48 120.8(4) . . ? C50 C49 C48 130.8(5) . . ? C28 C27 C26 120.8(5) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C24 C25 C26 121.4(5) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C73 C74 C75 121.7(5) . . ? C73 C74 Cl4 119.3(4) . . ? C75 C74 Cl4 119.0(4) . . ? C74 C75 C76 118.6(5) . . ? C74 C75 H75 120.7 . . ? C76 C75 H75 120.7 . . ? C27 C26 C25 122.6(5) . . ? C27 C26 C21 118.9(5) . . ? C25 C26 C21 118.4(5) . . ? N2 C13 C12 106.8(5) . . ? N2 C13 H13 126.6 . . ? C12 C13 H13 126.6 . . ? C42 C41 C40 120.1(5) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C51 C50 C49 106.9(5) . . ? C51 C50 H50 126.5 . . ? C49 C50 H50 126.5 . . ? C25 C24 C23 120.3(6) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? N4 C51 C50 107.0(4) . . ? N4 C51 H51 126.5 . . ? C50 C51 H51 126.5 . . ? C43 C44 C45 120.7(5) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C18 C17 C16 121.8(6) . . ? C18 C17 Cl1 119.0(5) . . ? C16 C17 Cl1 119.0(5) . . ? C71 C76 C75 120.5(5) . . ? C71 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C41 C42 C43 120.8(6) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C23 C22 C21 121.1(6) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C33 C34 C35 119.6(5) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C6 C7 120.5(6) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C60 C61 C62 120.0(6) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C70 C69 C68 105.4(5) . . ? C70 C69 H69 127.3 . . ? C68 C69 H69 127.3 . . ? C22 C23 C24 119.9(6) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C62 C63 C64 120.9(6) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? C44 C43 C42 120.5(5) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C65 C66 C67 121.7(6) . . ? C65 C66 H66 119.1 . . ? C67 C66 H66 119.1 . . ? C63 C62 C61 120.8(6) . . ? C63 C62 H62 119.6 . . ? C61 C62 H62 119.6 . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C14 C19 C18 122.1(6) . . ? C14 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C35 C36 C37 121.1(6) . . ? C35 C36 Cl2 120.6(5) . . ? C37 C36 Cl2 118.3(6) . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 118.6(6) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C77 C86 C85 118.2(6) . . ? C77 C86 C87 121.5(6) . . ? C85 C86 C87 120.3(6) . . ? C83 C78 C79 119.1(7) . . ? C83 C78 C77 118.6(7) . . ? C79 C78 C77 122.2(7) . . ? C85 C84 C83 120.3(7) . . ? C85 C84 H84 119.8 . . ? C83 C84 H84 119.8 . . ? O11 C77 C86 122.7(6) . . ? O11 C77 C78 115.6(6) . . ? C86 C77 C78 121.8(6) . . ? C84 C85 C86 121.4(7) . . ? C84 C85 H85 119.3 . . ? C86 C85 H85 119.3 . . ? C78 C83 C84 119.6(7) . . ? C78 C83 C82 118.1(7) . . ? C84 C83 C82 122.2(7) . . ? C81 C82 C83 120.9(8) . . ? C81 C82 H82 119.6 . . ? C83 C82 H82 119.6 . . ? C82 C81 C80 121.2(8) . . ? C82 C81 H81 119.4 . . ? C80 C81 H81 119.4 . . ? C80 C79 C78 121.2(8) . . ? C80 C79 H79 119.4 . . ? C78 C79 H79 119.4 . . ? C79 C80 C81 119.5(9) . . ? C79 C80 H80 120.3 . . ? C81 C80 H80 120.3 . . ? C77 O11 H11 109.5 . . ? N10 N9 C87 105.4(6) . . ? N9 C87 C88 109.3(6) . . ? N9 C87 C86 119.7(6) . . ? C88 C87 C86 130.9(6) . . ? C89 C88 C87 105.3(7) . . ? C89 C88 H88 127.4 . . ? C87 C88 H88 127.4 . . ? C89 N10 N9 112.3(6) . . ? C89 N10 H10 123.8 . . ? N9 N10 H10 123.8 . . ? N10 C89 C88 107.7(7) . . ? N10 C89 H89 126.1 . . ? C88 C89 H89 126.1 . . ? C3 C4 C5 120.5(6) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C94 C95 C90 119.2(9) . . ? C94 C95 C96 121.8(10) . . ? C90 C95 C96 118.8(10) . . ? C95 C94 C93 119.3(9) . . ? C95 C94 H94 120.4 . . ? C93 C94 H94 120.4 . . ? C91 C90 C95 120.8(9) . . ? C91 C90 H90 119.6 . . ? C95 C90 H90 119.6 . . ? C91 C92 C93 118.7(12) . . ? C91 C92 H92 120.7 . . ? C93 C92 H92 120.7 . . ? C90 C91 C92 122.6(10) . . ? C90 C91 H91 118.7 . . ? C92 C91 H91 118.7 . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C92 C93 C94 119.3(10) . . ? C92 C93 H93 120.3 . . ? C94 C93 H93 120.3 . . ? C66 C65 C64 121.8(6) . . ? C66 C65 H65 119.1 . . ? C64 C65 H65 119.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.295 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.136 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.196 0.700 0.627 209.2 42.5 2 0.304 0.200 0.873 209.2 43.0 3 0.696 0.800 0.127 209.1 42.7 4 0.804 0.300 0.373 209.1 43.0 _platon_squeeze_details ; ; #=================================================================END data_4 _database_code_depnum_ccdc_archive 'CCDC 808830' #TrackingRef '- cif all in one.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C186 H138 Br8 N18 O21 Sb8' _chemical_formula_sum 'C186 H138 Br8 N18 O21 Sb8' _chemical_formula_weight 4574.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 17.3569(12) _cell_length_b 21.1518(14) _cell_length_c 24.9421(17) _cell_angle_alpha 79.6580(10) _cell_angle_beta 85.4730(10) _cell_angle_gamma 76.5070(10) _cell_volume 8753.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7699 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4472 _exptl_absorpt_coefficient_mu 3.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5476 _exptl_absorpt_correction_T_max 0.7064 _exptl_absorpt_process_details brukarsdabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 84882 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 30737 _reflns_number_gt 26099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _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.heavily disordered two toluene solvent molecules have been squeezed out for the better refinement convergence. free ligand molecule modeled using FLAT DFIX EADP constraints.so that the number of restaints were 115. ; _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^)+(0.0538P)^2^+15.1504P] 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 30737 _refine_ls_number_parameters 2066 _refine_ls_number_restraints 115 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br2 Br 0.49941(4) 1.28511(4) 0.05209(5) 0.0995(4) Uani 1 1 d D . . Br9 Br 1.03023(3) 0.60757(3) 0.46358(2) 0.03181(13) Uani 1 1 d . . . Br7 Br 1.27852(3) 0.33861(3) 0.01906(2) 0.03219(13) Uani 1 1 d . . . Sb1 Sb 0.700734(16) 0.924539(14) 0.222213(11) 0.01327(7) Uani 1 1 d . . . Sb2 Sb 0.496382(17) 0.979687(14) 0.191086(12) 0.01433(7) Uani 1 1 d . . . Sb5 Sb 0.822997(17) 0.382675(14) 0.304131(12) 0.01537(7) Uani 1 1 d . . . Sb3 Sb 0.574364(17) 0.818427(14) 0.264559(12) 0.01417(7) Uani 1 1 d . . . Sb7 Sb 0.953430(17) 0.248895(14) 0.260627(12) 0.01373(7) Uani 1 1 d . . . Sb6 Sb 0.970574(17) 0.410902(14) 0.198774(12) 0.01472(7) Uani 1 1 d . . . Sb4 Sb 0.548911(17) 0.963271(14) 0.324970(12) 0.01372(7) Uani 1 1 d . . . Sb8 Sb 1.028423(17) 0.353178(14) 0.332194(12) 0.01551(7) Uani 1 1 d . . . Br4 Br 0.20264(3) 0.97211(3) 0.47228(2) 0.02940(12) Uani 1 1 d . . . Br1 Br 1.03856(3) 0.78903(3) 0.35757(2) 0.03247(13) Uani 1 1 d . . . Br8 Br 0.97921(3) -0.04352(2) 0.43263(2) 0.03354(13) Uani 1 1 d . . . Br5 Br 0.56093(3) 0.60838(3) 0.09074(2) 0.03520(13) Uani 1 1 d . . . O4 O 0.56407(17) 0.86920(14) 0.32353(12) 0.0151(6) Uani 1 1 d . . . O15 O 1.03765(17) 0.40302(14) 0.25983(12) 0.0160(6) Uani 1 1 d . . . O3 O 0.64729(17) 0.96710(14) 0.28275(12) 0.0142(6) Uani 1 1 d . . . O7 O 0.76330(17) 0.90636(14) 0.15252(12) 0.0164(7) Uani 1 1 d . . . O14 O 0.95735(17) 0.32129(14) 0.20113(12) 0.0157(6) Uani 1 1 d . . . O5 O 0.49696(17) 0.88770(14) 0.22121(12) 0.0172(7) Uani 1 1 d . . . O9 O 0.62887(17) 0.74087(14) 0.31883(12) 0.0163(7) Uani 1 1 d . . . O18 O 0.96549(18) 0.50762(15) 0.17814(13) 0.0204(7) Uani 1 1 d . . . O19 O 0.90232(18) 0.21208(15) 0.20649(12) 0.0170(7) Uani 1 1 d . . . O6 O 0.48460(17) 1.00505(14) 0.26247(12) 0.0156(6) Uani 1 1 d . . . O11 O 0.87344(17) 0.43274(14) 0.24292(12) 0.0171(7) Uani 1 1 d . . . O16 O 1.02932(17) 0.27326(14) 0.30261(12) 0.0165(7) Uani 1 1 d . . . O1 O 0.67447(17) 0.83862(14) 0.23668(12) 0.0152(6) Uani 1 1 d . . . N1 N 0.7345(2) 1.01915(18) 0.19366(15) 0.0167(8) Uani 1 1 d . . . O12 O 0.85240(17) 0.29245(14) 0.28983(12) 0.0168(7) Uani 1 1 d . . . O2 O 0.61071(17) 0.96126(14) 0.17577(12) 0.0153(6) Uani 1 1 d . . . O13 O 0.91438(17) 0.36844(15) 0.34923(12) 0.0175(7) Uani 1 1 d . . . N13 N 1.0603(2) 0.19818(18) 0.21807(15) 0.0174(8) Uani 1 1 d . . . O8 O 0.37869(17) 0.99156(15) 0.18114(13) 0.0188(7) Uani 1 1 d . . . N9 N 0.7845(2) 0.47899(18) 0.33114(15) 0.0180(8) Uani 1 1 d . . . O20 O 1.14716(18) 0.32174(14) 0.33653(13) 0.0184(7) Uani 1 1 d . . . C30 C 0.2505(3) 0.9682(3) 0.2488(2) 0.0270(11) Uani 1 1 d . . . H30 H 0.2752 1.0022 0.2540 0.032 Uiso 1 1 calc R . . O17 O 0.76448(19) 0.35626(15) 0.37444(13) 0.0210(7) Uani 1 1 d . . . C108 C 0.8984(3) 0.5547(2) 0.17220(19) 0.0187(10) Uani 1 1 d . . . N14 N 1.1326(2) 0.17747(19) 0.23934(16) 0.0216(9) Uani 1 1 d . . . H14 H 1.1440 0.1827 0.2718 0.026 Uiso 1 1 calc R . . N11 N 0.8904(2) 0.43682(18) 0.12986(15) 0.0181(8) Uani 1 1 d . . . C152 C 1.0350(3) 0.4322(2) 0.37281(19) 0.0184(10) Uani 1 1 d . . . N16 N 0.9821(2) 0.2835(2) 0.45007(16) 0.0227(9) Uani 1 1 d . . . H16 H 0.9379 0.3140 0.4505 0.027 Uiso 1 1 calc R . . N5 N 0.4707(2) 0.78607(18) 0.30770(15) 0.0190(8) Uani 1 1 d . . . C14 C 0.8091(3) 0.8902(2) 0.26368(19) 0.0178(10) Uani 1 1 d . . . C95 C 0.7138(3) 0.4067(2) 0.2637(2) 0.0193(10) Uani 1 1 d . . . C128 C 0.9598(3) 0.1572(2) 0.31444(18) 0.0168(9) Uani 1 1 d . . . C10 C 0.7506(3) 0.8148(3) 0.0224(2) 0.0276(11) Uani 1 1 d . . . H10 H 0.7548 0.7686 0.0277 0.033 Uiso 1 1 calc R . . C65 C 0.7041(3) 1.2164(2) 0.2983(2) 0.0232(11) Uani 1 1 d . . . H65 H 0.7498 1.2328 0.3013 0.028 Uiso 1 1 calc R . . N7 N 0.6273(2) 0.92959(18) 0.39503(15) 0.0173(8) Uani 1 1 d . . . N8 N 0.6421(2) 0.86774(18) 0.42485(15) 0.0201(8) Uani 1 1 d . . . H8 H 0.6143 0.8381 0.4241 0.024 Uiso 1 1 calc R . . C43 C 0.5213(3) 0.7166(2) 0.4510(2) 0.0265(11) Uani 1 1 d . . . H43 H 0.4688 0.7182 0.4656 0.032 Uiso 1 1 calc R . . C109 C 1.0681(3) 0.3932(2) 0.14223(19) 0.0186(10) Uani 1 1 d . . . N10 N 0.7793(2) 0.53657(18) 0.29686(16) 0.0196(8) Uani 1 1 d . . . H10A H 0.7935 0.5402 0.2620 0.024 Uiso 1 1 calc R . . C70 C 0.6233(3) 1.0665(2) 0.35025(18) 0.0177(10) Uani 1 1 d . . . C52 C 0.5729(3) 0.7517(2) 0.21042(18) 0.0170(9) Uani 1 1 d . . . C26 C 0.2448(3) 0.8778(3) 0.2005(2) 0.0294(12) Uani 1 1 d . . . C71 C 0.4465(3) 0.9617(2) 0.37688(18) 0.0161(9) Uani 1 1 d . . . C49 C 0.7539(3) 0.7153(2) 0.38786(19) 0.0203(10) Uani 1 1 d . . . H49 H 0.7636 0.7286 0.3500 0.024 Uiso 1 1 calc R . . C34 C 0.4338(3) 1.1095(2) 0.11051(17) 0.0256(5) Uani 1 1 d D . . H34 H 0.3939 1.0883 0.1035 0.031 Uiso 1 1 calc R . . C56 C 0.5657(3) 0.7321(2) 0.1187(2) 0.0242(11) Uani 1 1 d . . . H56 H 0.5635 0.7478 0.0806 0.029 Uiso 1 1 calc R . . N12 N 0.8745(2) 0.39311(19) 0.10166(16) 0.0206(9) Uani 1 1 d . . . H12 H 0.8994 0.3514 0.1051 0.025 Uiso 1 1 calc R . . C121 C 0.8731(3) 0.2385(2) 0.0599(2) 0.0254(11) Uani 1 1 d . . . C132 C 0.9715(3) 0.0392(2) 0.3290(2) 0.0241(11) Uani 1 1 d . . . H132 H 0.9755 -0.0004 0.3151 0.029 Uiso 1 1 calc R . . C32 C 0.3468(3) 0.9424(2) 0.1728(2) 0.0213(10) Uani 1 1 d . . . C76 C 0.3891(3) 0.9335(2) 0.3611(2) 0.0237(11) Uani 1 1 d . . . H76 H 0.3991 0.9128 0.3296 0.028 Uiso 1 1 calc R . . C33 C 0.4888(3) 1.0781(2) 0.14985(18) 0.0256(5) Uani 1 1 d D . . C46 C 0.7273(3) 0.6781(2) 0.4997(2) 0.0294(12) Uani 1 1 d . . . H46 H 0.7189 0.6656 0.5378 0.035 Uiso 1 1 calc R . . N15 N 1.0396(2) 0.28336(18) 0.41021(15) 0.0183(8) Uani 1 1 d . . . C129 C 0.9598(3) 0.1549(2) 0.36994(19) 0.0215(10) Uani 1 1 d . . . H129 H 0.9559 0.1945 0.3840 0.026 Uiso 1 1 calc R . . C22 C 0.4422(3) 0.9169(2) 0.09582(19) 0.0212(10) Uani 1 1 d . . . C51 C 0.6109(3) 0.7312(2) 0.37236(18) 0.0177(10) Uani 1 1 d . . . N6 N 0.3979(2) 0.80006(19) 0.28749(17) 0.0236(9) Uani 1 1 d . . . H6 H 0.3857 0.8207 0.2543 0.028 Uiso 1 1 calc R . . N3 N 0.4944(2) 0.94694(18) 0.11188(16) 0.0195(8) Uani 1 1 d . . . C8 C 0.7362(3) 0.9186(3) -0.0390(2) 0.0252(11) Uani 1 1 d . . . H8A H 0.7309 0.9428 -0.0750 0.030 Uiso 1 1 calc R . . C117 C 1.0670(3) 0.1819(2) 0.16797(19) 0.0204(10) Uani 1 1 d . . . C126 C 0.8575(3) 0.2393(2) 0.11668(19) 0.0209(10) Uani 1 1 d . . . N2 N 0.7447(2) 1.06074(18) 0.22601(15) 0.0189(8) Uani 1 1 d . . . H2 H 0.7383 1.0540 0.2618 0.023 Uiso 1 1 calc R . . C9 C 0.7422(3) 0.8519(3) -0.0301(2) 0.0276(12) Uani 1 1 d . . . H9 H 0.7406 0.8304 -0.0601 0.033 Uiso 1 1 calc R . . C114 C 1.1286(3) 0.3374(2) 0.1557(2) 0.0223(10) Uani 1 1 d . . . H114 H 1.1269 0.3102 0.1903 0.027 Uiso 1 1 calc R . . C17 C 0.9460(3) 0.8345(2) 0.31940(19) 0.0209(10) Uani 1 1 d . . . C118 C 0.9990(3) 0.2006(2) 0.13255(19) 0.0210(10) Uani 1 1 d . . . C45 C 0.6617(3) 0.6961(2) 0.46512(19) 0.0231(11) Uani 1 1 d . . . C146 C 1.1851(3) 0.2578(2) 0.3441(2) 0.0211(10) Uani 1 1 d . . . C67 C 0.5752(3) 1.2314(2) 0.2620(2) 0.0246(11) Uani 1 1 d . . . H67 H 0.5339 1.2579 0.2397 0.029 Uiso 1 1 calc R . . C74 C 0.3048(3) 0.9642(2) 0.43537(19) 0.0219(10) Uani 1 1 d . . . C73 C 0.3609(3) 0.9914(3) 0.4538(2) 0.0288(12) Uani 1 1 d . . . H73 H 0.3510 1.0106 0.4860 0.035 Uiso 1 1 calc R . . C97 C 0.7922(3) 0.4864(2) 0.07395(19) 0.0236(11) Uani 1 1 d . . . H97 H 0.7515 0.5190 0.0551 0.028 Uiso 1 1 calc R . . C69 C 0.6296(3) 1.1306(2) 0.32238(18) 0.0176(10) Uani 1 1 d . . . C18 C 0.8737(3) 0.8391(2) 0.34776(19) 0.0207(10) Uani 1 1 d . . . H18 H 0.8712 0.8236 0.3859 0.025 Uiso 1 1 calc R . . C59 C 0.7325(3) 0.9150(2) 0.44526(19) 0.0226(10) Uani 1 1 d . . . H59 H 0.7768 0.9228 0.4609 0.027 Uiso 1 1 calc R . . C6 C 0.7310(3) 1.0205(2) -0.00097(19) 0.0227(11) Uani 1 1 d . . . H6A H 0.7245 1.0465 -0.0362 0.027 Uiso 1 1 calc R . . C88 C 0.7763(3) 0.3257(2) 0.4699(2) 0.0226(10) Uani 1 1 d . . . C80 C 0.7590(3) 0.4414(2) 0.42784(19) 0.0227(10) Uani 1 1 d . . . C20 C 0.5391(3) 0.9175(2) 0.0323(2) 0.0254(11) Uani 1 1 d . . . H20 H 0.5720 0.9113 0.0005 0.030 Uiso 1 1 calc R . . C99 C 0.8388(3) 0.5522(2) 0.13892(19) 0.0190(10) Uani 1 1 d . . . C23 C 0.3740(3) 0.9055(2) 0.1315(2) 0.0219(10) Uani 1 1 d . . . C5 C 0.7336(3) 1.0498(2) 0.04298(19) 0.0216(10) Uani 1 1 d . . . H5 H 0.7289 1.0962 0.0378 0.026 Uiso 1 1 calc R . . C4 C 0.7433(3) 1.0126(2) 0.09643(18) 0.0178(10) Uani 1 1 d . . . C62 C 0.7555(3) 1.0493(2) 0.38248(19) 0.0218(10) Uani 1 1 d . . . H62 H 0.7988 1.0215 0.4023 0.026 Uiso 1 1 calc R . . C107 C 0.8917(3) 0.6085(2) 0.1999(2) 0.0215(10) Uani 1 1 d . . . C40 C 0.3866(3) 0.7488(3) 0.3711(2) 0.0341(13) Uani 1 1 d . . . H40 H 0.3655 0.7289 0.4044 0.041 Uiso 1 1 calc R . . C136 C 1.0967(3) 0.2286(2) 0.42365(19) 0.0214(10) Uani 1 1 d . . . C149 C 1.0334(3) 0.5359(2) 0.4266(2) 0.0231(11) Uani 1 1 d . . . C50 C 0.6755(3) 0.7141(2) 0.40824(19) 0.0189(10) Uani 1 1 d . . . C134 C 1.0022(3) 0.2304(3) 0.4889(2) 0.0307(12) Uani 1 1 d . . . H134 H 0.9717 0.2195 0.5211 0.037 Uiso 1 1 calc R . . C119 C 1.0127(3) 0.2031(3) 0.0756(2) 0.0281(12) Uani 1 1 d . . . H119 H 1.0657 0.1924 0.0615 0.034 Uiso 1 1 calc R . . N4 N 0.5528(2) 0.94697(19) 0.07312(15) 0.0204(9) Uani 1 1 d . . . H4 H 0.5943 0.9639 0.0742 0.024 Uiso 1 1 calc R . . C41 C 0.4654(3) 0.7541(2) 0.3595(2) 0.0216(10) Uani 1 1 d . . . C15 C 0.8825(3) 0.8876(2) 0.23700(19) 0.0207(10) Uani 1 1 d . . . H15 H 0.8857 0.9053 0.1993 0.025 Uiso 1 1 calc R . . C2 C 0.7702(3) 1.1064(2) 0.1426(2) 0.0239(11) Uani 1 1 d . . . H2A H 0.7843 1.1359 0.1120 0.029 Uiso 1 1 calc R . . C133 C 0.9654(3) 0.0991(2) 0.2942(2) 0.0231(11) Uani 1 1 d . . . H133 H 0.9650 0.1005 0.2559 0.028 Uiso 1 1 calc R . . C61 C 0.6856(3) 1.0259(2) 0.38004(18) 0.0186(10) Uani 1 1 d . . . C131 C 0.9718(3) 0.0386(2) 0.3843(2) 0.0233(11) Uani 1 1 d . . . C150 C 1.0984(3) 0.4841(2) 0.4303(2) 0.0263(11) Uani 1 1 d . . . H150 H 1.1422 0.4838 0.4510 0.032 Uiso 1 1 calc R . . C64 C 0.6993(3) 1.1531(2) 0.32630(19) 0.0202(10) Uani 1 1 d . . . C28 C 0.1507(3) 0.9052(3) 0.2749(3) 0.0398(15) Uani 1 1 d . . . H28 H 0.1066 0.8969 0.2979 0.048 Uiso 1 1 calc R . . C3 C 0.7495(3) 1.0463(2) 0.14202(18) 0.0173(10) Uani 1 1 d . . . C79 C 0.7578(3) 0.4934(2) 0.38026(19) 0.0208(10) Uani 1 1 d . . . C116 C 1.1456(3) 0.1489(2) 0.1586(2) 0.0278(12) Uani 1 1 d . . . H116 H 1.1673 0.1309 0.1270 0.033 Uiso 1 1 calc R . . C25 C 0.2751(3) 0.8400(3) 0.1599(2) 0.0345(13) Uani 1 1 d . . . H25 H 0.2522 0.8046 0.1555 0.041 Uiso 1 1 calc R . . C60 C 0.6823(3) 0.9594(2) 0.40697(18) 0.0186(10) Uani 1 1 d . . . C86 C 0.8014(3) 0.2107(3) 0.5107(3) 0.0387(14) Uani 1 1 d . . . H86 H 0.8107 0.1656 0.5072 0.046 Uiso 1 1 calc R . . C138 C 1.2086(3) 0.1449(2) 0.3917(2) 0.0302(12) Uani 1 1 d . . . H138 H 1.1949 0.1130 0.4205 0.036 Uiso 1 1 calc R . . C130 C 0.9653(3) 0.0955(2) 0.4058(2) 0.0255(11) Uani 1 1 d . . . H130 H 0.9646 0.0941 0.4441 0.031 Uiso 1 1 calc R . . C85 C 0.7999(3) 0.2282(3) 0.5622(2) 0.0368(14) Uani 1 1 d . . . H85 H 0.8086 0.1948 0.5936 0.044 Uiso 1 1 calc R . . C112 C 1.1928(3) 0.3607(2) 0.0693(2) 0.0241(11) Uani 1 1 d . . . C124 C 0.7176(3) 0.2798(2) 0.1013(2) 0.0271(11) Uani 1 1 d . . . H124 H 0.6650 0.2949 0.1147 0.033 Uiso 1 1 calc R . . C54 C 0.5678(3) 0.6434(2) 0.1948(2) 0.0284(12) Uani 1 1 d . . . H54 H 0.5673 0.5985 0.2083 0.034 Uiso 1 1 calc R . . C98 C 0.8399(3) 0.4952(2) 0.11354(18) 0.0188(10) Uani 1 1 d . . . C13 C 0.7500(2) 0.9454(2) 0.10411(18) 0.0165(9) Uani 1 1 d . . . C90 C 0.6416(3) 0.4244(2) 0.2908(2) 0.0285(12) Uani 1 1 d . . . H90 H 0.6401 0.4253 0.3288 0.034 Uiso 1 1 calc R . . C38 C 0.5468(3) 1.1096(2) 0.15983(19) 0.0256(5) Uani 1 1 d D . . H38 H 0.5848 1.0882 0.1864 0.031 Uiso 1 1 calc R . . C87 C 0.7897(3) 0.2586(2) 0.4649(2) 0.0305(12) Uani 1 1 d . . . H87 H 0.7906 0.2464 0.4300 0.037 Uiso 1 1 calc R . . C31 C 0.2803(3) 0.9298(2) 0.2076(2) 0.0238(11) Uani 1 1 d . . . C68 C 0.5681(3) 1.1708(2) 0.28952(19) 0.0205(10) Uani 1 1 d . . . H68 H 0.5214 1.1556 0.2865 0.025 Uiso 1 1 calc R . . C11 C 0.7527(3) 0.8449(2) 0.0661(2) 0.0216(10) Uani 1 1 d . . . H11 H 0.7579 0.8195 0.1016 0.026 Uiso 1 1 calc R . . C37 C 0.5503(3) 1.1717(2) 0.13177(19) 0.0256(5) Uani 1 1 d D . . H37 H 0.5895 1.1934 0.1389 0.031 Uiso 1 1 calc R . . C58 C 0.7051(3) 0.8583(2) 0.4555(2) 0.0245(11) Uani 1 1 d . . . H58 H 0.7267 0.8193 0.4799 0.029 Uiso 1 1 calc R . . C141 C 1.3551(3) 0.1546(3) 0.2742(2) 0.0326(13) Uani 1 1 d . . . H141 H 1.3844 0.1102 0.2777 0.039 Uiso 1 1 calc R . . C120 C 0.9525(3) 0.2204(3) 0.0405(2) 0.0315(12) Uani 1 1 d . . . H120 H 0.9638 0.2202 0.0026 0.038 Uiso 1 1 calc R . . C110 C 1.0716(3) 0.4331(2) 0.0918(2) 0.0256(11) Uani 1 1 d . . . H110 H 1.0313 0.4718 0.0826 0.031 Uiso 1 1 calc R . . C122 C 0.8073(3) 0.2565(3) 0.0253(2) 0.0335(13) Uani 1 1 d . . . H122 H 0.8161 0.2554 -0.0126 0.040 Uiso 1 1 calc R . . C78 C 0.7357(3) 0.5616(2) 0.3764(2) 0.0323(13) Uani 1 1 d . . . H78 H 0.7151 0.5854 0.4052 0.039 Uiso 1 1 calc R . . C55 C 0.5646(3) 0.6671(2) 0.1394(2) 0.0250(11) Uani 1 1 d . . . C57 C 0.5700(3) 0.7741(2) 0.15498(19) 0.0222(10) Uani 1 1 d . . . H57 H 0.5710 0.8188 0.1413 0.027 Uiso 1 1 calc R . . C35 C 0.4364(3) 1.1711(2) 0.08154(18) 0.0256(5) Uani 1 1 d D . . H35 H 0.3991 1.1924 0.0545 0.031 Uiso 1 1 calc R . . C53 C 0.5716(3) 0.6856(2) 0.2302(2) 0.0236(11) Uani 1 1 d . . . H53 H 0.5735 0.6697 0.2683 0.028 Uiso 1 1 calc R . . C72 C 0.4323(3) 0.9898(2) 0.4238(2) 0.0243(11) Uani 1 1 d . . . H72 H 0.4716 1.0081 0.4357 0.029 Uiso 1 1 calc R . . C21 C 0.4689(3) 0.8979(2) 0.0450(2) 0.0246(11) Uani 1 1 d . . . H21 H 0.4435 0.8761 0.0239 0.030 Uiso 1 1 calc R . . C135 C 1.0741(3) 0.1952(3) 0.4738(2) 0.0276(11) Uani 1 1 d . . . H135 H 1.1035 0.1553 0.4935 0.033 Uiso 1 1 calc R . . C89 C 0.7677(3) 0.3761(2) 0.4223(2) 0.0218(10) Uani 1 1 d . . . C63 C 0.7620(3) 1.1107(2) 0.3571(2) 0.0259(11) Uani 1 1 d . . . H63 H 0.8091 1.1252 0.3601 0.031 Uiso 1 1 calc R . . C96 C 0.8157(3) 0.4218(2) 0.06771(19) 0.0247(11) Uani 1 1 d . . . H96 H 0.7941 0.4009 0.0436 0.030 Uiso 1 1 calc R . . C42 C 0.5339(3) 0.7336(2) 0.39378(19) 0.0194(10) Uani 1 1 d . . . C123 C 0.7331(3) 0.2750(3) 0.0453(2) 0.0343(13) Uani 1 1 d . . . H123 H 0.6901 0.2851 0.0216 0.041 Uiso 1 1 calc R . . C1 C 0.7659(3) 1.1139(2) 0.1962(2) 0.0254(11) Uani 1 1 d . . . H1 H 0.7761 1.1502 0.2099 0.030 Uiso 1 1 calc R . . C100 C 0.7733(3) 0.6073(2) 0.1308(2) 0.0237(11) Uani 1 1 d . . . H100 H 0.7329 0.6068 0.1075 0.028 Uiso 1 1 calc R . . C16S C 0.4754(5) 0.3024(4) 0.3682(3) 0.067(2) Uani 1 1 d . . . H16S H 0.4747 0.3441 0.3463 0.081 Uiso 1 1 calc R . . C137 C 1.1642(3) 0.2120(2) 0.3865(2) 0.0219(10) Uani 1 1 d . . . C115 C 1.1843(3) 0.1479(3) 0.2040(2) 0.0286(12) Uani 1 1 d . . . H115 H 1.2390 0.1293 0.2097 0.034 Uiso 1 1 calc R . . C84 C 0.7861(3) 0.2926(3) 0.5676(2) 0.0328(13) Uani 1 1 d . . . H84 H 0.7847 0.3035 0.6031 0.039 Uiso 1 1 calc R . . C125 C 0.7793(3) 0.2625(2) 0.1357(2) 0.0214(10) Uani 1 1 d . . . H125 H 0.7692 0.2661 0.1731 0.026 Uiso 1 1 calc R . . C102 C 0.8257(3) 0.6626(2) 0.1913(2) 0.0214(10) Uani 1 1 d . . . C19S C 0.4792(5) 0.1809(5) 0.4326(3) 0.072(2) Uani 1 1 d . . . H19S H 0.4796 0.1390 0.4543 0.086 Uiso 1 1 calc R . . C29 C 0.1861(3) 0.9566(3) 0.2814(2) 0.0359(13) Uani 1 1 d . . . H29 H 0.1654 0.9833 0.3084 0.043 Uiso 1 1 calc R . . C7 C 0.7379(3) 0.9516(2) 0.00549(19) 0.0219(10) Uani 1 1 d . . . C48 C 0.8158(3) 0.6974(2) 0.4224(2) 0.0247(11) Uani 1 1 d . . . H48 H 0.8681 0.6979 0.4083 0.030 Uiso 1 1 calc R . . C82 C 0.7588(3) 0.4113(3) 0.5266(2) 0.0324(12) Uani 1 1 d . . . H82 H 0.7530 0.4243 0.5615 0.039 Uiso 1 1 calc R . . C103 C 0.8190(3) 0.7161(2) 0.2200(2) 0.0246(11) Uani 1 1 d . . . H103 H 0.7754 0.7530 0.2140 0.030 Uiso 1 1 calc R . . C139 C 1.2700(3) 0.1262(2) 0.3560(2) 0.0334(13) Uani 1 1 d . . . H139 H 1.2984 0.0815 0.3605 0.040 Uiso 1 1 calc R . . C94 C 0.7150(3) 0.4068(2) 0.2080(2) 0.0238(11) Uani 1 1 d . . . H94 H 0.7644 0.3959 0.1887 0.029 Uiso 1 1 calc R . . C143 C 1.3317(3) 0.2659(3) 0.2268(2) 0.0327(13) Uani 1 1 d . . . H143 H 1.3458 0.2974 0.1978 0.039 Uiso 1 1 calc R . . C106 C 0.9482(3) 0.6087(2) 0.2376(2) 0.0329(13) Uani 1 1 d . . . H106 H 0.9925 0.5725 0.2441 0.040 Uiso 1 1 calc R . . C113 C 1.1908(3) 0.3214(2) 0.1192(2) 0.0250(11) Uani 1 1 d . . . H113 H 1.2320 0.2833 0.1285 0.030 Uiso 1 1 calc R . . C83 C 0.7737(3) 0.3437(3) 0.5226(2) 0.0261(11) Uani 1 1 d . . . C12 C 0.7473(3) 0.9132(2) 0.05899(19) 0.0191(10) Uani 1 1 d . . . C77 C 0.7497(3) 0.5877(2) 0.3229(2) 0.0301(12) Uani 1 1 d . . . H77 H 0.7402 0.6332 0.3074 0.036 Uiso 1 1 calc R . . C36 C 0.4942(3) 1.2008(2) 0.09281(19) 0.0256(5) Uani 1 1 d D . . C47 C 0.8021(3) 0.6784(2) 0.4786(2) 0.0281(12) Uani 1 1 d . . . H47 H 0.8454 0.6657 0.5022 0.034 Uiso 1 1 calc R . . C19 C 0.8051(3) 0.8667(2) 0.31976(19) 0.0195(10) Uani 1 1 d . . . H19 H 0.7549 0.8697 0.3386 0.023 Uiso 1 1 calc R . . C39 C 0.3464(3) 0.7779(3) 0.3252(2) 0.0344(13) Uani 1 1 d . . . H39 H 0.2915 0.7818 0.3207 0.041 Uiso 1 1 calc R . . C144 C 1.2706(3) 0.2852(3) 0.2625(2) 0.0273(11) Uani 1 1 d . . . H144 H 1.2421 0.3299 0.2578 0.033 Uiso 1 1 calc R . . C44 C 0.5827(3) 0.6982(2) 0.4856(2) 0.0276(12) Uani 1 1 d . . . H44 H 0.5725 0.6867 0.5237 0.033 Uiso 1 1 calc R . . C101 C 0.7672(3) 0.6606(2) 0.1555(2) 0.0251(11) Uani 1 1 d . . . H101 H 0.7232 0.6969 0.1487 0.030 Uiso 1 1 calc R . . C111 C 1.1335(3) 0.4168(3) 0.0550(2) 0.0291(12) Uani 1 1 d . . . H111 H 1.1356 0.4436 0.0202 0.035 Uiso 1 1 calc R . . C142 C 1.3738(3) 0.2005(3) 0.2327(2) 0.0336(13) Uani 1 1 d . . . H142 H 1.4160 0.1878 0.2074 0.040 Uiso 1 1 calc R . . C18S C 0.4153(5) 0.2148(5) 0.4030(4) 0.072(2) Uani 1 1 d . . . H18S H 0.3708 0.1954 0.4049 0.087 Uiso 1 1 calc R . . C151 C 1.0986(3) 0.4321(2) 0.40307(19) 0.0212(10) Uani 1 1 d . . . H151 H 1.1431 0.3960 0.4053 0.025 Uiso 1 1 calc R . . C81 C 0.7527(3) 0.4575(3) 0.4811(2) 0.0300(12) Uani 1 1 d . . . H81 H 0.7438 0.5026 0.4849 0.036 Uiso 1 1 calc R . . C24 C 0.3374(3) 0.8536(3) 0.1265(2) 0.0297(12) Uani 1 1 d . . . H24 H 0.3569 0.8275 0.0989 0.036 Uiso 1 1 calc R . . C27 C 0.1789(3) 0.8673(3) 0.2361(2) 0.0359(13) Uani 1 1 d . . . H27 H 0.1541 0.8328 0.2325 0.043 Uiso 1 1 calc R . . C75 C 0.3181(3) 0.9349(2) 0.3901(2) 0.0241(11) Uani 1 1 d . . . H75 H 0.2791 0.9158 0.3787 0.029 Uiso 1 1 calc R . . C145 C 1.2491(3) 0.2390(2) 0.3066(2) 0.0214(10) Uani 1 1 d . . . C140 C 1.2923(3) 0.1725(2) 0.3122(2) 0.0270(11) Uani 1 1 d . . . C20S C 0.5441(4) 0.2100(4) 0.4298(3) 0.058(2) Uani 1 1 d . . . C16 C 0.9513(3) 0.8593(2) 0.2651(2) 0.0246(11) Uani 1 1 d . . . H16A H 1.0017 0.8571 0.2468 0.030 Uiso 1 1 calc R . . C17S C 0.4113(5) 0.2752(5) 0.3707(3) 0.072(2) Uani 1 1 d . . . H17S H 0.3655 0.2972 0.3508 0.087 Uiso 1 1 calc R . . C15S C 0.5427(4) 0.2692(4) 0.3979(3) 0.0523(19) Uani 1 1 d . . . H15S H 0.5874 0.2883 0.3955 0.063 Uiso 1 1 calc R . . C66 C 0.6437(3) 1.2543(2) 0.2669(2) 0.0263(11) Uani 1 1 d . . . H66 H 0.6480 1.2967 0.2482 0.032 Uiso 1 1 calc R . . O10 O 0.55444(17) 1.04887(14) 0.34697(12) 0.0158(6) Uani 1 1 d . . . C93 C 0.6458(3) 0.4223(2) 0.1802(2) 0.0299(12) Uani 1 1 d . . . H93 H 0.6471 0.4218 0.1422 0.036 Uiso 1 1 calc R . . C92 C 0.5745(3) 0.4385(3) 0.2087(2) 0.0329(13) Uani 1 1 d . . . C104 C 0.8741(3) 0.7149(2) 0.2556(2) 0.0308(12) Uani 1 1 d . . . H104 H 0.8688 0.7508 0.2747 0.037 Uiso 1 1 calc R . . C105 C 0.9393(4) 0.6609(3) 0.2649(3) 0.0397(14) Uani 1 1 d . . . H105 H 0.9775 0.6606 0.2902 0.048 Uiso 1 1 calc R . . C91 C 0.5707(3) 0.4411(3) 0.2633(2) 0.0338(13) Uani 1 1 d . . . H91 H 0.5212 0.4539 0.2820 0.041 Uiso 1 1 calc R . . C147 C 0.9715(3) 0.4855(3) 0.3695(3) 0.0382(14) Uani 1 1 d . . . H147 H 0.9279 0.4864 0.3484 0.046 Uiso 1 1 calc R . . C148 C 0.9699(3) 0.5381(3) 0.3962(3) 0.0388(15) Uani 1 1 d . . . H148 H 0.9258 0.5747 0.3935 0.047 Uiso 1 1 calc R . . C13S C 0.6533(4) 0.4066(3) 0.9268(3) 0.0488(16) Uani 1 1 d . . . C11S C 0.6005(5) 0.4711(4) 0.9972(3) 0.062(2) Uani 1 1 d . . . H11S H 0.5707 0.4758 1.0304 0.074 Uiso 1 1 calc R . . C12S C 0.6087(4) 0.4159(4) 0.9743(3) 0.0571(18) Uani 1 1 d . . . H12S H 0.5828 0.3824 0.9918 0.068 Uiso 1 1 calc R . . C10S C 0.6364(4) 0.5194(4) 0.9709(3) 0.065(2) Uani 1 1 d . . . H10S H 0.6293 0.5589 0.9857 0.077 Uiso 1 1 calc R . . C6S C 0.9734(5) 0.2871(4) 0.8863(3) 0.062(2) Uani 1 1 d . . . C9S C 0.6822(5) 0.5137(4) 0.9241(4) 0.067(2) Uani 1 1 d . . . H9S H 0.7076 0.5478 0.9072 0.080 Uiso 1 1 calc R . . C1S C 0.9109(4) 0.3377(4) 0.8984(3) 0.0595(19) Uani 1 1 d . . . H1S H 0.8611 0.3433 0.8828 0.071 Uiso 1 1 calc R . . C8S C 0.6906(5) 0.4563(4) 0.9020(3) 0.067(2) Uani 1 1 d . . . H8S H 0.7223 0.4511 0.8696 0.080 Uiso 1 1 calc R . . C2S C 0.9193(5) 0.3794(4) 0.9319(4) 0.072(2) Uani 1 1 d . . . H2S H 0.8754 0.4134 0.9394 0.087 Uiso 1 1 calc R . . C14S C 0.6616(5) 0.3450(4) 0.9004(3) 0.070(2) Uani 1 1 d . . . H14A H 0.6341 0.3140 0.9237 0.105 Uiso 1 1 calc R . . H14B H 0.7179 0.3240 0.8963 0.105 Uiso 1 1 calc R . . H14C H 0.6382 0.3577 0.8645 0.105 Uiso 1 1 calc R . . C5S C 1.0444(5) 0.2818(5) 0.9100(4) 0.080(3) Uani 1 1 d . . . H5S H 1.0888 0.2480 0.9028 0.096 Uiso 1 1 calc R . . C7S C 0.9621(7) 0.2407(4) 0.8503(3) 0.095(3) Uani 1 1 d . . . H7S1 H 1.0099 0.2301 0.8270 0.143 Uiso 1 1 calc R . . H7S2 H 0.9166 0.2616 0.8275 0.143 Uiso 1 1 calc R . . H7S3 H 0.9524 0.2002 0.8729 0.143 Uiso 1 1 calc R . . C4S C 1.0524(5) 0.3255(5) 0.9445(4) 0.084(3) Uani 1 1 d . . . H4S H 1.1019 0.3211 0.9601 0.101 Uiso 1 1 calc R . . C3S C 0.9908(6) 0.3730(4) 0.9554(3) 0.074(2) Uani 1 1 d . . . H3S H 0.9960 0.4022 0.9791 0.089 Uiso 1 1 calc R . . C21S C 0.6116(7) 0.1749(5) 0.4616(4) 0.111(4) Uani 1 1 d . . . H21A H 0.6481 0.2039 0.4617 0.166 Uiso 1 1 calc R . . H21B H 0.6390 0.1362 0.4456 0.166 Uiso 1 1 calc R . . H21C H 0.5936 0.1606 0.4992 0.166 Uiso 1 1 calc R . . C127 C 0.9218(3) 0.2174(2) 0.15313(18) 0.0174(10) Uani 1 1 d . . . Br6 Br 0.47873(4) 0.45792(3) 0.17010(3) 0.05255(18) Uani 1 1 d . . . C163 C 0.2371(6) 0.5314(5) 0.2666(4) 0.1082(15) Uani 1 1 d DU . . C161 C 0.3402(4) 0.5903(4) 0.2767(3) 0.0877(9) Uani 1 1 d DU . . H161 H 0.3207 0.6208 0.2453 0.105 Uiso 1 1 calc R . . C160 C 0.4052(4) 0.5972(4) 0.3028(3) 0.0877(9) Uani 1 1 d DU . . H160 H 0.4293 0.6326 0.2873 0.105 Uiso 1 1 calc R . . C159 C 0.4377(4) 0.5567(3) 0.3497(3) 0.0877(9) Uani 1 1 d DU . . C162 C 0.3042(4) 0.5380(3) 0.2973(3) 0.0877(9) Uani 1 1 d DU . . C153 C 0.3353(3) 0.4963(3) 0.3441(2) 0.0877(9) Uani 1 1 d DU . . C154 C 0.4007(3) 0.5047(3) 0.3688(2) 0.0877(9) Uani 1 1 d DU . . C155 C 0.4318(4) 0.4619(3) 0.4150(2) 0.0877(9) Uani 1 1 d DU . . H155 H 0.4070 0.4268 0.4300 0.105 Uiso 1 1 calc R . . C156 C 0.4976(4) 0.4681(4) 0.4405(3) 0.0877(9) Uani 1 1 d DU . . H156 H 0.5179 0.4378 0.4718 0.105 Uiso 1 1 calc R . . C158 C 0.5042(4) 0.5658(4) 0.3726(3) 0.0877(9) Uani 1 1 d DU . . H158 H 0.5287 0.6012 0.3579 0.105 Uiso 1 1 calc R . . C157 C 0.5327(5) 0.5203(3) 0.4182(3) 0.0877(9) Uani 1 1 d DU . . H157 H 0.5779 0.5251 0.4348 0.105 Uiso 1 1 calc R . . C165 C 0.1431(6) 0.5369(5) 0.2104(4) 0.1082(15) Uani 1 1 d DU . . H165 H 0.1069 0.5519 0.1817 0.130 Uiso 1 1 calc R . . C164 C 0.1989(6) 0.5690(5) 0.2253(4) 0.1082(15) Uani 1 1 d DU . . H164 H 0.2072 0.6109 0.2083 0.130 Uiso 1 1 calc R . . O21 O 0.3013(4) 0.4431(3) 0.3671(3) 0.123(3) Uani 1 1 d D . . H21D H 0.2520 0.4541 0.3636 0.185 Uiso 1 1 calc R . . N17 N 0.2127(5) 0.4740(4) 0.2816(3) 0.1082(15) Uani 1 1 d DU . . N18 N 0.1535(5) 0.4782(4) 0.2473(3) 0.1082(15) Uani 1 1 d DU . . H18A H 0.1258 0.4480 0.2485 0.130 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 Br2 0.0469(4) 0.0571(5) 0.1742(10) 0.0811(6) -0.0507(5) -0.0320(4) Br9 0.0293(3) 0.0255(3) 0.0460(3) -0.0210(2) -0.0034(2) -0.0047(2) Br7 0.0307(3) 0.0298(3) 0.0319(3) -0.0054(2) 0.0112(2) -0.0024(2) Sb1 0.01279(15) 0.01193(14) 0.01426(15) -0.00157(11) 0.00000(11) -0.00173(11) Sb2 0.01327(15) 0.01258(15) 0.01635(15) -0.00154(11) -0.00154(12) -0.00167(11) Sb5 0.01478(15) 0.01190(15) 0.01935(16) -0.00398(12) -0.00032(12) -0.00190(12) Sb3 0.01474(15) 0.01111(14) 0.01613(15) -0.00202(11) 0.00019(12) -0.00229(11) Sb7 0.01596(15) 0.01004(14) 0.01508(15) -0.00246(11) -0.00020(12) -0.00252(11) Sb6 0.01523(15) 0.01042(14) 0.01789(16) -0.00141(11) -0.00113(12) -0.00218(11) Sb4 0.01384(15) 0.01154(15) 0.01520(15) -0.00224(11) 0.00076(11) -0.00208(11) Sb8 0.01559(15) 0.01113(15) 0.01978(16) -0.00354(12) -0.00319(12) -0.00135(12) Br4 0.0245(3) 0.0293(3) 0.0362(3) -0.0089(2) 0.0127(2) -0.0116(2) Br1 0.0182(3) 0.0449(3) 0.0274(3) 0.0067(2) -0.0057(2) -0.0013(2) Br8 0.0391(3) 0.0209(3) 0.0370(3) 0.0120(2) -0.0098(2) -0.0096(2) Br5 0.0442(3) 0.0316(3) 0.0363(3) -0.0185(2) -0.0048(3) -0.0106(2) O4 0.0205(16) 0.0116(15) 0.0136(15) -0.0038(12) -0.0018(13) -0.0028(13) O15 0.0171(16) 0.0138(15) 0.0171(16) -0.0017(13) -0.0039(13) -0.0034(13) O3 0.0139(15) 0.0141(15) 0.0136(15) -0.0033(12) 0.0038(12) -0.0015(12) O7 0.0159(16) 0.0177(16) 0.0148(16) -0.0023(13) 0.0011(12) -0.0033(13) O14 0.0197(16) 0.0120(15) 0.0152(16) -0.0011(12) 0.0018(13) -0.0049(13) O5 0.0159(16) 0.0120(15) 0.0224(17) 0.0012(13) -0.0045(13) -0.0028(13) O9 0.0180(16) 0.0125(15) 0.0148(16) -0.0003(12) 0.0011(13) 0.0016(13) O18 0.0175(16) 0.0118(16) 0.0306(19) -0.0005(14) -0.0035(14) -0.0020(13) O19 0.0214(17) 0.0179(16) 0.0144(16) -0.0048(13) 0.0007(13) -0.0084(13) O6 0.0147(15) 0.0148(16) 0.0156(16) -0.0022(12) -0.0014(12) -0.0001(12) O11 0.0167(16) 0.0133(16) 0.0203(17) -0.0023(13) 0.0011(13) -0.0021(13) O16 0.0163(16) 0.0127(15) 0.0210(17) -0.0067(13) -0.0022(13) -0.0007(12) O1 0.0145(15) 0.0104(15) 0.0198(16) -0.0023(12) 0.0008(13) -0.0015(12) N1 0.0147(19) 0.017(2) 0.018(2) -0.0019(16) -0.0016(15) -0.0030(15) O12 0.0154(16) 0.0124(15) 0.0224(17) -0.0046(13) 0.0030(13) -0.0030(12) O2 0.0135(15) 0.0160(16) 0.0150(16) -0.0015(12) -0.0005(12) -0.0014(12) O13 0.0156(16) 0.0174(16) 0.0205(17) -0.0055(13) -0.0022(13) -0.0031(13) N13 0.0153(19) 0.0135(19) 0.023(2) -0.0045(16) 0.0008(16) -0.0025(15) O8 0.0145(16) 0.0161(16) 0.0255(18) -0.0030(13) -0.0031(13) -0.0027(13) N9 0.017(2) 0.0138(19) 0.022(2) -0.0023(16) -0.0018(16) -0.0008(16) O20 0.0173(16) 0.0125(16) 0.0252(18) -0.0043(13) -0.0008(13) -0.0020(13) C30 0.018(3) 0.033(3) 0.028(3) -0.004(2) 0.000(2) -0.005(2) O17 0.0229(17) 0.0178(17) 0.0224(18) -0.0055(14) 0.0042(14) -0.0051(14) C108 0.018(2) 0.013(2) 0.023(3) 0.0020(19) 0.0012(19) -0.0033(19) N14 0.018(2) 0.022(2) 0.022(2) -0.0034(17) -0.0021(17) 0.0010(17) N11 0.020(2) 0.0146(19) 0.020(2) -0.0020(16) 0.0006(16) -0.0056(16) C152 0.019(2) 0.013(2) 0.023(2) -0.0048(19) -0.0014(19) -0.0030(19) N16 0.022(2) 0.025(2) 0.021(2) -0.0065(18) 0.0016(17) -0.0049(18) N5 0.016(2) 0.018(2) 0.022(2) -0.0047(16) 0.0028(16) -0.0032(16) C14 0.017(2) 0.014(2) 0.022(2) -0.0031(19) -0.0025(19) -0.0021(18) C95 0.015(2) 0.013(2) 0.030(3) -0.0022(19) -0.007(2) -0.0031(18) C128 0.014(2) 0.015(2) 0.021(2) -0.0006(18) 0.0006(18) -0.0037(18) C10 0.030(3) 0.024(3) 0.030(3) -0.010(2) 0.002(2) -0.008(2) C65 0.025(3) 0.020(3) 0.027(3) -0.006(2) 0.007(2) -0.012(2) N7 0.017(2) 0.016(2) 0.016(2) 0.0004(15) 0.0034(15) -0.0006(16) N8 0.025(2) 0.014(2) 0.021(2) -0.0020(16) 0.0006(17) -0.0049(17) C43 0.025(3) 0.022(3) 0.028(3) -0.001(2) 0.008(2) -0.002(2) C109 0.018(2) 0.016(2) 0.022(2) -0.0025(19) 0.0003(19) -0.0049(19) N10 0.023(2) 0.0127(19) 0.022(2) -0.0011(16) -0.0003(17) -0.0024(16) C70 0.016(2) 0.018(2) 0.020(2) -0.0084(19) 0.0017(18) -0.0016(19) C52 0.016(2) 0.015(2) 0.020(2) -0.0047(19) -0.0001(18) -0.0034(18) C26 0.020(3) 0.028(3) 0.039(3) 0.004(2) -0.009(2) -0.007(2) C71 0.014(2) 0.011(2) 0.021(2) -0.0014(18) 0.0023(18) -0.0008(18) C49 0.025(3) 0.013(2) 0.020(2) -0.0013(19) -0.002(2) -0.0007(19) C34 0.0212(10) 0.0203(10) 0.0319(12) 0.0046(9) -0.0030(9) -0.0038(8) C56 0.024(3) 0.025(3) 0.021(3) -0.006(2) -0.004(2) 0.000(2) N12 0.023(2) 0.014(2) 0.025(2) -0.0027(16) -0.0028(17) -0.0044(16) C121 0.036(3) 0.022(3) 0.021(3) -0.002(2) -0.004(2) -0.011(2) C132 0.028(3) 0.015(2) 0.029(3) -0.005(2) 0.003(2) -0.004(2) C32 0.014(2) 0.017(2) 0.031(3) 0.001(2) -0.009(2) -0.0008(19) C76 0.030(3) 0.018(2) 0.026(3) -0.010(2) 0.003(2) -0.008(2) C33 0.0212(10) 0.0203(10) 0.0319(12) 0.0046(9) -0.0030(9) -0.0038(8) C46 0.039(3) 0.024(3) 0.020(3) -0.002(2) -0.007(2) 0.004(2) N15 0.021(2) 0.017(2) 0.016(2) -0.0044(16) -0.0015(16) -0.0036(16) C129 0.024(3) 0.018(2) 0.025(3) -0.006(2) -0.004(2) -0.007(2) C22 0.021(2) 0.016(2) 0.024(3) 0.000(2) -0.007(2) -0.0003(19) C51 0.024(2) 0.008(2) 0.020(2) -0.0007(18) -0.0011(19) -0.0022(18) N6 0.018(2) 0.023(2) 0.029(2) 0.0011(18) -0.0045(17) -0.0048(17) N3 0.019(2) 0.018(2) 0.022(2) -0.0024(16) -0.0026(17) -0.0037(16) C8 0.024(3) 0.035(3) 0.018(3) -0.010(2) 0.001(2) -0.008(2) C117 0.024(3) 0.014(2) 0.024(3) -0.0055(19) 0.008(2) -0.0051(19) C126 0.029(3) 0.014(2) 0.021(2) -0.0021(19) 0.000(2) -0.009(2) N2 0.024(2) 0.019(2) 0.016(2) -0.0055(16) 0.0010(16) -0.0085(17) C9 0.023(3) 0.039(3) 0.023(3) -0.015(2) -0.001(2) -0.006(2) C114 0.021(2) 0.019(2) 0.023(3) 0.004(2) 0.000(2) -0.002(2) C17 0.018(2) 0.023(3) 0.021(3) -0.001(2) -0.007(2) -0.002(2) C118 0.028(3) 0.016(2) 0.020(2) -0.0059(19) 0.002(2) -0.006(2) C45 0.033(3) 0.016(2) 0.017(2) -0.0005(19) 0.003(2) -0.002(2) C146 0.018(2) 0.016(2) 0.031(3) -0.005(2) -0.012(2) -0.0014(19) C67 0.030(3) 0.018(2) 0.023(3) 0.000(2) 0.001(2) -0.003(2) C74 0.017(2) 0.022(3) 0.025(3) -0.002(2) 0.009(2) -0.005(2) C73 0.030(3) 0.037(3) 0.022(3) -0.010(2) 0.004(2) -0.011(2) C97 0.024(3) 0.025(3) 0.021(3) 0.001(2) -0.003(2) -0.006(2) C69 0.019(2) 0.016(2) 0.017(2) -0.0058(18) 0.0021(19) -0.0018(19) C18 0.025(3) 0.018(2) 0.018(2) -0.0018(19) 0.001(2) -0.004(2) C59 0.021(3) 0.022(3) 0.021(3) -0.004(2) -0.006(2) 0.002(2) C6 0.024(3) 0.027(3) 0.016(2) 0.002(2) -0.002(2) -0.008(2) C88 0.016(2) 0.023(3) 0.028(3) -0.001(2) 0.004(2) -0.006(2) C80 0.024(3) 0.021(3) 0.022(3) -0.004(2) -0.003(2) -0.003(2) C20 0.023(3) 0.029(3) 0.021(3) -0.006(2) -0.001(2) 0.001(2) C99 0.018(2) 0.014(2) 0.022(2) 0.0007(19) 0.0012(19) -0.0020(19) C23 0.019(2) 0.020(2) 0.025(3) -0.001(2) -0.008(2) -0.001(2) C5 0.023(3) 0.019(2) 0.021(3) 0.001(2) 0.000(2) -0.006(2) C4 0.014(2) 0.022(2) 0.018(2) -0.0031(19) 0.0034(18) -0.0063(19) C62 0.019(2) 0.023(3) 0.022(3) -0.001(2) -0.002(2) -0.003(2) C107 0.021(2) 0.015(2) 0.028(3) -0.002(2) 0.001(2) -0.007(2) C40 0.024(3) 0.035(3) 0.039(3) 0.005(3) 0.005(2) -0.010(2) C136 0.023(3) 0.018(2) 0.024(3) 0.001(2) -0.008(2) -0.006(2) C149 0.030(3) 0.018(2) 0.027(3) -0.013(2) 0.003(2) -0.009(2) C50 0.023(2) 0.009(2) 0.023(3) -0.0030(18) 0.001(2) -0.0018(19) C134 0.039(3) 0.043(3) 0.016(3) -0.003(2) -0.001(2) -0.022(3) C119 0.031(3) 0.030(3) 0.024(3) -0.007(2) 0.008(2) -0.009(2) N4 0.018(2) 0.021(2) 0.022(2) -0.0040(17) 0.0002(17) -0.0045(17) C41 0.020(2) 0.019(2) 0.025(3) -0.005(2) 0.005(2) -0.003(2) C15 0.019(2) 0.024(3) 0.018(2) 0.0003(19) -0.0020(19) -0.006(2) C2 0.029(3) 0.022(3) 0.021(3) -0.002(2) 0.007(2) -0.010(2) C133 0.031(3) 0.018(2) 0.018(2) -0.0051(19) 0.002(2) -0.001(2) C61 0.018(2) 0.019(2) 0.017(2) -0.0044(19) -0.0011(19) -0.0005(19) C131 0.021(3) 0.018(2) 0.027(3) 0.008(2) -0.006(2) -0.005(2) C150 0.026(3) 0.024(3) 0.030(3) -0.007(2) -0.008(2) -0.003(2) C64 0.019(2) 0.023(3) 0.022(3) -0.011(2) 0.0077(19) -0.008(2) C28 0.018(3) 0.045(4) 0.049(4) 0.013(3) 0.002(3) -0.009(3) C3 0.015(2) 0.017(2) 0.018(2) -0.0003(18) 0.0012(18) -0.0014(18) C79 0.020(2) 0.019(2) 0.022(3) -0.004(2) -0.003(2) -0.0016(19) C116 0.026(3) 0.026(3) 0.029(3) -0.013(2) 0.009(2) 0.001(2) C25 0.028(3) 0.029(3) 0.048(4) -0.002(3) -0.008(3) -0.009(2) C60 0.017(2) 0.020(2) 0.019(2) -0.0074(19) -0.0001(19) -0.0008(19) C86 0.031(3) 0.023(3) 0.054(4) 0.007(3) 0.006(3) -0.003(2) C138 0.031(3) 0.021(3) 0.037(3) 0.005(2) -0.010(2) -0.006(2) C130 0.033(3) 0.024(3) 0.020(3) 0.002(2) -0.008(2) -0.007(2) C85 0.025(3) 0.038(3) 0.039(3) 0.015(3) 0.003(2) -0.010(2) C112 0.024(3) 0.024(3) 0.026(3) -0.005(2) 0.005(2) -0.008(2) C124 0.024(3) 0.019(3) 0.038(3) -0.002(2) -0.007(2) -0.006(2) C54 0.040(3) 0.018(3) 0.030(3) -0.007(2) 0.005(2) -0.011(2) C98 0.017(2) 0.020(2) 0.019(2) 0.0001(19) 0.0014(19) -0.0047(19) C13 0.008(2) 0.023(2) 0.017(2) -0.0004(19) 0.0020(17) -0.0035(18) C90 0.023(3) 0.025(3) 0.039(3) -0.014(2) 0.000(2) -0.002(2) C38 0.0212(10) 0.0203(10) 0.0319(12) 0.0046(9) -0.0030(9) -0.0038(8) C87 0.029(3) 0.023(3) 0.037(3) -0.001(2) 0.011(2) -0.007(2) C31 0.014(2) 0.024(3) 0.030(3) 0.004(2) -0.006(2) -0.002(2) C68 0.022(2) 0.021(2) 0.020(2) -0.006(2) 0.001(2) -0.006(2) C11 0.019(2) 0.020(2) 0.023(3) -0.003(2) 0.003(2) -0.001(2) C37 0.0212(10) 0.0203(10) 0.0319(12) 0.0046(9) -0.0030(9) -0.0038(8) C58 0.027(3) 0.020(3) 0.022(3) -0.002(2) -0.005(2) 0.002(2) C141 0.020(3) 0.031(3) 0.045(3) -0.018(3) -0.006(2) 0.007(2) C120 0.045(3) 0.037(3) 0.016(3) -0.005(2) -0.001(2) -0.015(3) C110 0.019(2) 0.019(3) 0.034(3) 0.003(2) 0.000(2) 0.000(2) C122 0.048(4) 0.033(3) 0.020(3) 0.005(2) -0.012(2) -0.015(3) C78 0.046(3) 0.017(3) 0.032(3) -0.009(2) 0.005(3) -0.003(2) C55 0.024(3) 0.026(3) 0.029(3) -0.017(2) -0.001(2) -0.005(2) C57 0.022(3) 0.016(2) 0.026(3) -0.001(2) -0.005(2) 0.000(2) C35 0.0212(10) 0.0203(10) 0.0319(12) 0.0046(9) -0.0030(9) -0.0038(8) C53 0.030(3) 0.019(2) 0.023(3) -0.002(2) 0.003(2) -0.008(2) C72 0.020(3) 0.031(3) 0.025(3) -0.006(2) 0.001(2) -0.011(2) C21 0.027(3) 0.026(3) 0.022(3) -0.009(2) -0.007(2) -0.003(2) C135 0.029(3) 0.029(3) 0.024(3) 0.004(2) -0.008(2) -0.010(2) C89 0.016(2) 0.022(3) 0.025(3) -0.002(2) 0.001(2) -0.001(2) C63 0.019(3) 0.031(3) 0.030(3) -0.005(2) -0.004(2) -0.010(2) C96 0.033(3) 0.024(3) 0.020(3) -0.004(2) -0.002(2) -0.010(2) C42 0.023(2) 0.012(2) 0.022(2) -0.0015(19) 0.003(2) -0.0053(19) C123 0.039(3) 0.033(3) 0.031(3) 0.007(2) -0.015(3) -0.013(3) C1 0.033(3) 0.018(2) 0.029(3) -0.005(2) 0.003(2) -0.013(2) C100 0.024(3) 0.021(3) 0.026(3) -0.002(2) -0.005(2) -0.003(2) C16S 0.068(5) 0.092(6) 0.043(4) -0.035(4) 0.014(4) -0.009(5) C137 0.019(2) 0.018(2) 0.027(3) -0.001(2) -0.008(2) -0.0002(19) C115 0.019(3) 0.027(3) 0.035(3) -0.003(2) 0.004(2) 0.000(2) C84 0.022(3) 0.050(4) 0.026(3) 0.006(3) -0.005(2) -0.015(3) C125 0.026(3) 0.017(2) 0.022(3) -0.0012(19) -0.003(2) -0.007(2) C102 0.023(3) 0.014(2) 0.026(3) -0.0006(19) 0.003(2) -0.0044(19) C19S 0.076(6) 0.086(6) 0.070(5) -0.051(5) 0.023(5) -0.028(5) C29 0.019(3) 0.047(4) 0.036(3) -0.001(3) 0.003(2) -0.002(2) C7 0.013(2) 0.031(3) 0.020(2) -0.004(2) 0.0008(19) -0.003(2) C48 0.022(3) 0.021(3) 0.030(3) -0.005(2) -0.001(2) -0.001(2) C82 0.038(3) 0.042(3) 0.020(3) -0.009(2) -0.001(2) -0.012(3) C103 0.025(3) 0.010(2) 0.035(3) -0.002(2) 0.006(2) 0.000(2) C139 0.027(3) 0.014(3) 0.055(4) -0.004(2) -0.011(3) 0.006(2) C94 0.019(2) 0.021(3) 0.032(3) -0.002(2) -0.002(2) -0.008(2) C143 0.026(3) 0.045(3) 0.026(3) -0.005(2) 0.002(2) -0.007(3) C106 0.036(3) 0.016(3) 0.049(3) -0.010(2) -0.015(3) -0.002(2) C113 0.021(3) 0.019(3) 0.031(3) 0.000(2) -0.002(2) -0.001(2) C83 0.017(2) 0.032(3) 0.028(3) 0.001(2) -0.004(2) -0.009(2) C12 0.012(2) 0.024(3) 0.020(2) -0.005(2) 0.0016(18) -0.0011(19) C77 0.039(3) 0.014(2) 0.035(3) -0.007(2) 0.004(2) -0.002(2) C36 0.0212(10) 0.0203(10) 0.0319(12) 0.0046(9) -0.0030(9) -0.0038(8) C47 0.029(3) 0.022(3) 0.029(3) 0.000(2) -0.008(2) 0.003(2) C19 0.019(2) 0.017(2) 0.022(3) -0.0046(19) 0.0033(19) -0.0038(19) C39 0.021(3) 0.039(3) 0.042(3) 0.002(3) 0.002(2) -0.012(2) C144 0.018(3) 0.028(3) 0.031(3) -0.004(2) -0.003(2) 0.004(2) C44 0.033(3) 0.024(3) 0.021(3) 0.001(2) 0.006(2) -0.002(2) C101 0.020(3) 0.019(3) 0.030(3) -0.001(2) 0.003(2) 0.004(2) C111 0.028(3) 0.028(3) 0.024(3) 0.007(2) 0.003(2) -0.002(2) C142 0.021(3) 0.052(4) 0.028(3) -0.017(3) 0.000(2) -0.002(3) C18S 0.065(5) 0.102(7) 0.066(6) -0.049(5) 0.000(4) -0.025(5) C151 0.024(3) 0.019(2) 0.020(2) -0.0048(19) -0.003(2) 0.000(2) C81 0.034(3) 0.028(3) 0.030(3) -0.011(2) -0.002(2) -0.006(2) C24 0.029(3) 0.026(3) 0.035(3) -0.005(2) -0.007(2) -0.005(2) C27 0.023(3) 0.034(3) 0.052(4) 0.003(3) -0.004(3) -0.014(2) C75 0.020(3) 0.021(3) 0.034(3) -0.006(2) 0.001(2) -0.009(2) C145 0.013(2) 0.023(3) 0.026(3) -0.003(2) -0.005(2) -0.0009(19) C140 0.019(3) 0.024(3) 0.038(3) -0.008(2) -0.007(2) 0.001(2) C20S 0.062(5) 0.063(5) 0.041(4) -0.027(4) -0.004(3) 0.015(4) C16 0.015(2) 0.029(3) 0.028(3) -0.004(2) 0.003(2) -0.003(2) C17S 0.056(5) 0.113(8) 0.052(5) -0.041(5) -0.005(4) -0.008(5) C15S 0.036(4) 0.087(6) 0.046(4) -0.039(4) 0.019(3) -0.021(4) C66 0.032(3) 0.016(2) 0.031(3) -0.005(2) 0.007(2) -0.009(2) O10 0.0104(15) 0.0132(15) 0.0240(17) -0.0061(13) 0.0019(13) -0.0017(12) C93 0.035(3) 0.027(3) 0.029(3) 0.005(2) -0.009(2) -0.014(2) C92 0.019(3) 0.027(3) 0.050(4) 0.006(3) -0.014(2) -0.006(2) C104 0.042(3) 0.016(3) 0.037(3) -0.008(2) 0.003(3) -0.009(2) C105 0.045(4) 0.027(3) 0.051(4) -0.013(3) -0.018(3) -0.007(3) C91 0.019(3) 0.025(3) 0.056(4) -0.008(3) -0.003(2) 0.000(2) C147 0.028(3) 0.024(3) 0.065(4) -0.017(3) -0.022(3) 0.003(2) C148 0.024(3) 0.023(3) 0.072(4) -0.023(3) -0.018(3) 0.005(2) C13S 0.052(4) 0.038(4) 0.056(4) -0.007(3) -0.015(3) -0.004(3) C11S 0.066(5) 0.060(5) 0.065(5) -0.016(4) -0.020(4) -0.015(4) C12S 0.047(4) 0.056(4) 0.066(5) -0.008(4) -0.010(4) -0.005(3) C10S 0.057(5) 0.071(5) 0.070(5) -0.013(4) -0.016(4) -0.017(4) C6S 0.059(5) 0.059(5) 0.052(4) 0.020(4) 0.023(4) -0.010(4) C9S 0.070(5) 0.060(5) 0.079(6) -0.005(4) -0.019(5) -0.031(4) C1S 0.046(4) 0.058(5) 0.066(5) 0.005(4) -0.007(4) -0.005(4) C8S 0.065(5) 0.077(6) 0.064(5) -0.013(4) -0.007(4) -0.023(4) C2S 0.078(6) 0.045(4) 0.085(6) 0.009(4) -0.020(5) -0.006(4) C14S 0.065(5) 0.073(5) 0.075(6) -0.017(4) -0.006(4) -0.017(4) C5S 0.050(5) 0.085(6) 0.068(6) 0.039(5) 0.027(4) 0.010(4) C7S 0.154(10) 0.078(6) 0.049(5) -0.013(4) 0.036(6) -0.029(6) C4S 0.059(5) 0.105(8) 0.074(6) 0.048(6) -0.009(5) -0.037(6) C3S 0.085(6) 0.064(5) 0.073(6) 0.021(4) -0.022(5) -0.033(5) C21S 0.139(10) 0.094(7) 0.074(7) -0.029(6) -0.007(6) 0.036(7) C127 0.027(3) 0.010(2) 0.017(2) -0.0054(18) 0.0048(19) -0.0088(19) Br6 0.0290(3) 0.0574(4) 0.0672(5) 0.0086(3) -0.0233(3) -0.0090(3) C163 0.129(4) 0.101(3) 0.110(3) 0.024(2) -0.047(3) -0.073(3) C161 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C160 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C159 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C162 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C153 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C154 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C155 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C156 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C158 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C157 0.094(2) 0.087(2) 0.084(2) -0.0056(16) -0.0148(16) -0.0286(18) C165 0.129(4) 0.101(3) 0.110(3) 0.024(2) -0.047(3) -0.073(3) C164 0.129(4) 0.101(3) 0.110(3) 0.024(2) -0.047(3) -0.073(3) O21 0.118(6) 0.084(5) 0.153(7) 0.028(5) 0.027(6) -0.039(4) N17 0.129(4) 0.101(3) 0.110(3) 0.024(2) -0.047(3) -0.073(3) N18 0.129(4) 0.101(3) 0.110(3) 0.024(2) -0.047(3) -0.073(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 Br2 C36 1.905(5) . ? Br9 C149 1.900(4) . ? Br7 C112 1.896(5) . ? Sb1 O1 1.941(3) . ? Sb1 O2 1.945(3) . ? Sb1 O3 1.957(3) . ? Sb1 O7 2.024(3) . ? Sb1 C14 2.129(4) . ? Sb1 N1 2.197(4) . ? Sb2 O6 1.932(3) . ? Sb2 O2 1.951(3) . ? Sb2 O5 1.954(3) . ? Sb2 O8 2.029(3) . ? Sb2 C33 2.129(5) . ? Sb2 N3 2.213(4) . ? Sb5 O12 1.947(3) . ? Sb5 O13 1.952(3) . ? Sb5 O11 1.965(3) . ? Sb5 O17 2.013(3) . ? Sb5 C95 2.130(4) . ? Sb5 N9 2.199(4) . ? Sb3 O1 1.932(3) . ? Sb3 O4 1.946(3) . ? Sb3 O5 1.965(3) . ? Sb3 O9 2.025(3) . ? Sb3 C52 2.127(4) . ? Sb3 N5 2.207(4) . ? Sb7 O12 1.934(3) . ? Sb7 O14 1.941(3) . ? Sb7 O16 1.956(3) . ? Sb7 O19 2.026(3) . ? Sb7 C128 2.136(4) . ? Sb7 N13 2.211(4) . ? Sb6 O11 1.948(3) . ? Sb6 O15 1.950(3) . ? Sb6 O14 1.952(3) . ? Sb6 O18 2.001(3) . ? Sb6 C109 2.124(5) . ? Sb6 N11 2.207(4) . ? Sb4 O6 1.943(3) . ? Sb4 O3 1.945(3) . ? Sb4 O4 1.952(3) . ? Sb4 O10 2.009(3) . ? Sb4 C71 2.117(4) . ? Sb4 N7 2.211(4) . ? Sb8 O15 1.935(3) . ? Sb8 O13 1.955(3) . ? Sb8 O16 1.959(3) . ? Sb8 O20 2.018(3) . ? Sb8 C152 2.132(4) . ? Sb8 N15 2.213(4) . ? Br4 C74 1.918(4) . ? Br1 C17 1.899(4) . ? Br8 C131 1.913(5) . ? Br5 C55 1.899(5) . ? O7 C13 1.338(5) . ? O9 C51 1.337(5) . ? O18 C108 1.343(5) . ? O19 C127 1.338(5) . ? N1 N2 1.344(5) . ? N1 C3 1.344(6) . ? N13 C117 1.344(6) . ? N13 N14 1.346(5) . ? O8 C32 1.340(5) . ? N9 C79 1.337(6) . ? N9 N10 1.345(5) . ? O20 C146 1.346(5) . ? C30 C29 1.372(7) . ? C30 C31 1.416(7) . ? C30 H30 0.9500 . ? O17 C89 1.344(6) . ? C108 C99 1.392(6) . ? C108 C107 1.411(6) . ? N14 C115 1.337(6) . ? N14 H14 0.8800 . ? N11 N12 1.345(5) . ? N11 C98 1.352(6) . ? C152 C147 1.376(7) . ? C152 C151 1.385(6) . ? N16 C134 1.341(6) . ? N16 N15 1.351(5) . ? N16 H16 0.8800 . ? N5 N6 1.345(5) . ? N5 C41 1.353(6) . ? C14 C15 1.384(6) . ? C14 C19 1.400(6) . ? C95 C90 1.381(7) . ? C95 C94 1.386(7) . ? C128 C129 1.376(6) . ? C128 C133 1.391(6) . ? C10 C11 1.362(7) . ? C10 C9 1.401(7) . ? C10 H10 0.9500 . ? C65 C66 1.366(7) . ? C65 C64 1.413(7) . ? C65 H65 0.9500 . ? N7 C60 1.338(6) . ? N7 N8 1.362(5) . ? N8 C58 1.339(6) . ? N8 H8 0.8800 . ? C43 C44 1.365(7) . ? C43 C42 1.420(7) . ? C43 H43 0.9500 . ? C109 C110 1.390(7) . ? C109 C114 1.394(6) . ? N10 C77 1.340(6) . ? N10 H10A 0.8800 . ? C70 O10 1.344(5) . ? C70 C61 1.386(6) . ? C70 C69 1.432(6) . ? C52 C57 1.380(6) . ? C52 C53 1.401(6) . ? C26 C25 1.398(8) . ? C26 C31 1.422(7) . ? C26 C27 1.426(7) . ? C71 C72 1.386(6) . ? C71 C76 1.390(6) . ? C49 C48 1.371(7) . ? C49 C50 1.419(7) . ? C49 H49 0.9500 . ? C34 C35 1.380(7) . ? C34 C33 1.391(7) . ? C34 H34 0.9500 . ? C56 C55 1.382(7) . ? C56 C57 1.395(7) . ? C56 H56 0.9500 . ? N12 C96 1.338(6) . ? N12 H12 0.8800 . ? C121 C120 1.411(7) . ? C121 C126 1.424(7) . ? C121 C122 1.425(7) . ? C132 C131 1.376(7) . ? C132 C133 1.390(7) . ? C132 H132 0.9500 . ? C32 C23 1.390(7) . ? C32 C31 1.435(7) . ? C76 C75 1.376(7) . ? C76 H76 0.9500 . ? C33 C38 1.390(7) . ? C46 C47 1.362(7) . ? C46 C45 1.420(7) . ? C46 H46 0.9500 . ? N15 C136 1.347(6) . ? C129 C130 1.395(7) . ? C129 H129 0.9500 . ? C22 N3 1.342(6) . ? C22 C21 1.408(7) . ? C22 C23 1.464(7) . ? C51 C42 1.393(6) . ? C51 C50 1.428(6) . ? N6 C39 1.346(6) . ? N6 H6 0.8800 . ? N3 N4 1.345(5) . ? C8 C9 1.368(7) . ? C8 C7 1.418(7) . ? C8 H8A 0.9500 . ? C117 C116 1.402(7) . ? C117 C118 1.467(7) . ? C126 C125 1.407(7) . ? C126 C127 1.433(7) . ? N2 C1 1.343(6) . ? N2 H2 0.8800 . ? C9 H9 0.9500 . ? C114 C113 1.376(7) . ? C114 H114 0.9500 . ? C17 C16 1.365(7) . ? C17 C18 1.383(7) . ? C118 C127 1.385(7) . ? C118 C119 1.416(7) . ? C45 C50 1.417(6) . ? C45 C44 1.419(7) . ? C146 C137 1.388(7) . ? C146 C145 1.424(7) . ? C67 C68 1.368(7) . ? C67 C66 1.406(7) . ? C67 H67 0.9500 . ? C74 C75 1.363(7) . ? C74 C73 1.384(7) . ? C73 C72 1.392(7) . ? C73 H73 0.9500 . ? C97 C96 1.367(7) . ? C97 C98 1.400(7) . ? C97 H97 0.9500 . ? C69 C68 1.414(6) . ? C69 C64 1.417(6) . ? C18 C19 1.381(6) . ? C18 H18 0.9500 . ? C59 C58 1.365(7) . ? C59 C60 1.407(6) . ? C59 H59 0.9500 . ? C6 C5 1.362(7) . ? C6 C7 1.415(7) . ? C6 H6A 0.9500 . ? C88 C87 1.412(7) . ? C88 C83 1.427(7) . ? C88 C89 1.437(7) . ? C80 C89 1.385(7) . ? C80 C81 1.418(7) . ? C80 C79 1.464(7) . ? C20 N4 1.349(6) . ? C20 C21 1.372(7) . ? C20 H20 0.9500 . ? C99 C100 1.423(6) . ? C99 C98 1.456(6) . ? C23 C24 1.419(7) . ? C5 C4 1.422(6) . ? C5 H5 0.9500 . ? C4 C13 1.379(6) . ? C4 C3 1.469(6) . ? C62 C63 1.364(7) . ? C62 C61 1.423(6) . ? C62 H62 0.9500 . ? C107 C106 1.413(7) . ? C107 C102 1.418(6) . ? C40 C39 1.359(8) . ? C40 C41 1.401(7) . ? C40 H40 0.9500 . ? C136 C135 1.397(7) . ? C136 C137 1.451(7) . ? C149 C150 1.371(7) . ? C149 C148 1.375(7) . ? C134 C135 1.360(7) . ? C134 H134 0.9500 . ? C119 C120 1.359(7) . ? C119 H119 0.9500 . ? N4 H4 0.8800 . ? C41 C42 1.456(7) . ? C15 C16 1.389(6) . ? C15 H15 0.9500 . ? C2 C1 1.370(7) . ? C2 C3 1.402(6) . ? C2 H2A 0.9500 . ? C133 H133 0.9500 . ? C61 C60 1.459(6) . ? C131 C130 1.381(7) . ? C150 C151 1.392(7) . ? C150 H150 0.9500 . ? C64 C63 1.416(7) . ? C28 C27 1.357(8) . ? C28 C29 1.407(8) . ? C28 H28 0.9500 . ? C79 C78 1.390(7) . ? C116 C115 1.356(7) . ? C116 H116 0.9500 . ? C25 C24 1.366(8) . ? C25 H25 0.9500 . ? C86 C87 1.376(7) . ? C86 C85 1.396(8) . ? C86 H86 0.9500 . ? C138 C139 1.366(8) . ? C138 C137 1.436(7) . ? C138 H138 0.9500 . ? C130 H130 0.9500 . ? C85 C84 1.357(8) . ? C85 H85 0.9500 . ? C112 C113 1.369(7) . ? C112 C111 1.388(7) . ? C124 C125 1.366(7) . ? C124 C123 1.416(8) . ? C124 H124 0.9500 . ? C54 C53 1.379(7) . ? C54 C55 1.385(7) . ? C54 H54 0.9500 . ? C13 C12 1.425(6) . ? C90 C91 1.399(7) . ? C90 H90 0.9500 . ? C38 C37 1.384(7) . ? C38 H38 0.9500 . ? C87 H87 0.9500 . ? C68 H68 0.9500 . ? C11 C12 1.406(7) . ? C11 H11 0.9500 . ? C37 C36 1.388(7) . ? C37 H37 0.9500 . ? C58 H58 0.9500 . ? C141 C142 1.361(8) . ? C141 C140 1.415(7) . ? C141 H141 0.9500 . ? C120 H120 0.9500 . ? C110 C111 1.379(7) . ? C110 H110 0.9500 . ? C122 C123 1.339(8) . ? C122 H122 0.9500 . ? C78 C77 1.377(7) . ? C78 H78 0.9500 . ? C57 H57 0.9500 . ? C35 C36 1.371(7) . ? C35 H35 0.9500 . ? C53 H53 0.9500 . ? C72 H72 0.9500 . ? C21 H21 0.9500 . ? C135 H135 0.9500 . ? C63 H63 0.9500 . ? C96 H96 0.9500 . ? C123 H123 0.9500 . ? C1 H1 0.9500 . ? C100 C101 1.357(7) . ? C100 H100 0.9500 . ? C16S C17S 1.358(11) . ? C16S C15S 1.404(10) . ? C16S H16S 0.9500 . ? C115 H115 0.9500 . ? C84 C83 1.405(7) . ? C84 H84 0.9500 . ? C125 H125 0.9500 . ? C102 C101 1.418(7) . ? C102 C103 1.421(7) . ? C19S C18S 1.363(12) . ? C19S C20S 1.397(11) . ? C19S H19S 0.9500 . ? C29 H29 0.9500 . ? C7 C12 1.432(6) . ? C48 C47 1.405(7) . ? C48 H48 0.9500 . ? C82 C81 1.353(7) . ? C82 C83 1.411(7) . ? C82 H82 0.9500 . ? C103 C104 1.348(7) . ? C103 H103 0.9500 . ? C139 C140 1.424(8) . ? C139 H139 0.9500 . ? C94 C93 1.377(7) . ? C94 H94 0.9500 . ? C143 C144 1.365(7) . ? C143 C142 1.394(8) . ? C143 H143 0.9500 . ? C106 C105 1.371(7) . ? C106 H106 0.9500 . ? C113 H113 0.9500 . ? C77 H77 0.9500 . ? C47 H47 0.9500 . ? C19 H19 0.9500 . ? C39 H39 0.9500 . ? C144 C145 1.423(7) . ? C144 H144 0.9500 . ? C44 H44 0.9500 . ? C101 H101 0.9500 . ? C111 H111 0.9500 . ? C142 H142 0.9500 . ? C18S C17S 1.374(12) . ? C18S H18S 0.9500 . ? C151 H151 0.9500 . ? C81 H81 0.9500 . ? C24 H24 0.9500 . ? C27 H27 0.9500 . ? C75 H75 0.9500 . ? C145 C140 1.420(7) . ? C20S C15S 1.353(10) . ? C20S C21S 1.443(11) . ? C16 H16A 0.9500 . ? C17S H17S 0.9500 . ? C15S H15S 0.9500 . ? C66 H66 0.9500 . ? C93 C92 1.380(8) . ? C93 H93 0.9500 . ? C92 C91 1.368(8) . ? C92 Br6 1.911(5) . ? C104 C105 1.408(8) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C91 H91 0.9500 . ? C147 C148 1.388(7) . ? C147 H147 0.9500 . ? C148 H148 0.9500 . ? C13S C12S 1.383(10) . ? C13S C8S 1.388(10) . ? C13S C14S 1.534(10) . ? C11S C10S 1.362(10) . ? C11S C12S 1.364(10) . ? C11S H11S 0.9500 . ? C12S H12S 0.9500 . ? C10S C9S 1.366(11) . ? C10S H10S 0.9500 . ? C6S C5S 1.381(12) . ? C6S C1S 1.392(10) . ? C6S C7S 1.496(12) . ? C9S C8S 1.395(11) . ? C9S H9S 0.9500 . ? C1S C2S 1.356(11) . ? C1S H1S 0.9500 . ? C8S H8S 0.9500 . ? C2S C3S 1.382(11) . ? C2S H2S 0.9500 . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? C5S C4S 1.407(13) . ? C5S H5S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C4S C3S 1.334(13) . ? C4S H4S 0.9500 . ? C3S H3S 0.9500 . ? C21S H21A 0.9800 . ? C21S H21B 0.9800 . ? C21S H21C 0.9800 . ? C163 C164 1.304(13) . ? C163 N17 1.358(11) . ? C163 C162 1.490(12) . ? C161 C162 1.3935(10) . ? C161 C160 1.3938(10) . ? C161 H161 0.9500 . ? C160 C159 1.3933(10) . ? C160 H160 0.9500 . ? C159 C158 1.3934(10) . ? C159 C154 1.3935(10) . ? C162 C153 1.3938(10) . ? C153 C154 1.3939(10) . ? C153 O21 1.403(9) . ? C154 C155 1.3925(10) . ? C155 C156 1.3922(10) . ? C155 H155 0.9500 . ? C156 C157 1.3926(10) . ? C156 H156 0.9500 . ? C158 C157 1.3924(10) . ? C158 H158 0.9500 . ? C157 H157 0.9500 . ? C165 N18 1.391(11) . ? C165 C164 1.412(12) . ? C165 H165 0.9500 . ? C164 H164 0.9500 . ? O21 H21D 0.8400 . ? N17 N18 1.365(10) . ? N18 H18A 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sb1 O2 91.69(12) . . ? O1 Sb1 O3 103.50(12) . . ? O2 Sb1 O3 92.64(12) . . ? O1 Sb1 O7 93.02(12) . . ? O2 Sb1 O7 85.51(12) . . ? O3 Sb1 O7 163.43(12) . . ? O1 Sb1 C14 93.49(15) . . ? O2 Sb1 C14 171.83(15) . . ? O3 Sb1 C14 92.29(15) . . ? O7 Sb1 C14 87.91(15) . . ? O1 Sb1 N1 171.69(13) . . ? O2 Sb1 N1 85.19(13) . . ? O3 Sb1 N1 84.37(13) . . ? O7 Sb1 N1 79.07(13) . . ? C14 Sb1 N1 88.82(15) . . ? O6 Sb2 O2 103.88(12) . . ? O6 Sb2 O5 92.65(13) . . ? O2 Sb2 O5 93.19(12) . . ? O6 Sb2 O8 95.62(12) . . ? O2 Sb2 O8 160.48(12) . . ? O5 Sb2 O8 86.65(12) . . ? O6 Sb2 C33 93.33(14) . . ? O2 Sb2 C33 89.04(14) . . ? O5 Sb2 C33 172.92(16) . . ? O8 Sb2 C33 89.00(15) . . ? O6 Sb2 N3 172.32(13) . . ? O2 Sb2 N3 83.14(13) . . ? O5 Sb2 N3 83.75(13) . . ? O8 Sb2 N3 77.44(13) . . ? C33 Sb2 N3 89.85(15) . . ? O12 Sb5 O13 91.88(12) . . ? O12 Sb5 O11 103.98(12) . . ? O13 Sb5 O11 92.00(13) . . ? O12 Sb5 O17 92.31(12) . . ? O13 Sb5 O17 85.38(13) . . ? O11 Sb5 O17 163.59(12) . . ? O12 Sb5 C95 94.81(15) . . ? O13 Sb5 C95 171.40(15) . . ? O11 Sb5 C95 91.61(15) . . ? O17 Sb5 C95 88.96(16) . . ? O12 Sb5 N9 172.38(13) . . ? O13 Sb5 N9 86.19(13) . . ? O11 Sb5 N9 83.47(13) . . ? O17 Sb5 N9 80.19(13) . . ? C95 Sb5 N9 86.48(15) . . ? O1 Sb3 O4 94.07(12) . . ? O1 Sb3 O5 102.73(12) . . ? O4 Sb3 O5 92.05(12) . . ? O1 Sb3 O9 91.85(12) . . ? O4 Sb3 O9 85.87(12) . . ? O5 Sb3 O9 165.38(12) . . ? O1 Sb3 C52 95.51(15) . . ? O4 Sb3 C52 169.03(15) . . ? O5 Sb3 C52 91.04(15) . . ? O9 Sb3 C52 88.49(15) . . ? O1 Sb3 N5 170.87(13) . . ? O4 Sb3 N5 82.65(13) . . ? O5 Sb3 N5 85.95(13) . . ? O9 Sb3 N5 79.44(13) . . ? C52 Sb3 N5 87.08(15) . . ? O12 Sb7 O14 93.63(12) . . ? O12 Sb7 O16 102.66(12) . . ? O14 Sb7 O16 92.94(12) . . ? O12 Sb7 O19 93.02(12) . . ? O14 Sb7 O19 84.82(12) . . ? O16 Sb7 O19 164.28(12) . . ? O12 Sb7 C128 95.50(15) . . ? O14 Sb7 C128 168.62(15) . . ? O16 Sb7 C128 91.68(15) . . ? O19 Sb7 C128 87.92(15) . . ? O12 Sb7 N13 172.51(13) . . ? O14 Sb7 N13 83.63(13) . . ? O16 Sb7 N13 84.48(13) . . ? O19 Sb7 N13 79.81(13) . . ? C128 Sb7 N13 86.46(15) . . ? O11 Sb6 O15 92.72(13) . . ? O11 Sb6 O14 91.52(12) . . ? O15 Sb6 O14 103.84(12) . . ? O11 Sb6 O18 88.01(12) . . ? O15 Sb6 O18 92.23(12) . . ? O14 Sb6 O18 163.93(13) . . ? O11 Sb6 C109 172.95(15) . . ? O15 Sb6 C109 93.72(15) . . ? O14 Sb6 C109 89.73(15) . . ? O18 Sb6 C109 88.88(15) . . ? O11 Sb6 N11 84.47(13) . . ? O15 Sb6 N11 170.88(13) . . ? O14 Sb6 N11 84.94(13) . . ? O18 Sb6 N11 79.03(13) . . ? C109 Sb6 N11 88.72(16) . . ? O6 Sb4 O3 92.57(12) . . ? O6 Sb4 O4 103.75(12) . . ? O3 Sb4 O4 91.71(12) . . ? O6 Sb4 O10 94.32(12) . . ? O3 Sb4 O10 87.25(12) . . ? O4 Sb4 O10 161.93(12) . . ? O6 Sb4 C71 91.43(15) . . ? O3 Sb4 C71 174.66(15) . . ? O4 Sb4 C71 90.78(14) . . ? O10 Sb4 C71 88.92(14) . . ? O6 Sb4 N7 171.64(13) . . ? O3 Sb4 N7 83.99(13) . . ? O4 Sb4 N7 84.01(13) . . ? O10 Sb4 N7 77.94(13) . . ? C71 Sb4 N7 91.57(15) . . ? O15 Sb8 O13 104.63(13) . . ? O15 Sb8 O16 91.67(12) . . ? O13 Sb8 O16 92.46(12) . . ? O15 Sb8 O20 92.06(12) . . ? O13 Sb8 O20 163.31(13) . . ? O16 Sb8 O20 87.15(12) . . ? O15 Sb8 C152 94.32(15) . . ? O13 Sb8 C152 89.81(15) . . ? O16 Sb8 C152 172.84(15) . . ? O20 Sb8 C152 88.73(15) . . ? O15 Sb8 N15 168.81(13) . . ? O13 Sb8 N15 85.14(13) . . ? O16 Sb8 N15 82.34(13) . . ? O20 Sb8 N15 78.26(13) . . ? C152 Sb8 N15 91.10(16) . . ? Sb3 O4 Sb4 132.99(15) . . ? Sb8 O15 Sb6 126.84(15) . . ? Sb4 O3 Sb1 133.67(16) . . ? C13 O7 Sb1 124.0(3) . . ? Sb7 O14 Sb6 132.69(16) . . ? Sb2 O5 Sb3 131.98(16) . . ? C51 O9 Sb3 124.8(3) . . ? C108 O18 Sb6 125.0(3) . . ? C127 O19 Sb7 124.7(3) . . ? Sb2 O6 Sb4 126.89(15) . . ? Sb6 O11 Sb5 133.37(16) . . ? Sb7 O16 Sb8 132.79(15) . . ? Sb3 O1 Sb1 127.30(15) . . ? N2 N1 C3 107.2(4) . . ? N2 N1 Sb1 125.1(3) . . ? C3 N1 Sb1 127.8(3) . . ? Sb7 O12 Sb5 126.74(15) . . ? Sb1 O2 Sb2 132.52(16) . . ? Sb5 O13 Sb8 132.56(16) . . ? C117 N13 N14 107.1(4) . . ? C117 N13 Sb7 128.4(3) . . ? N14 N13 Sb7 124.5(3) . . ? C32 O8 Sb2 122.6(3) . . ? C79 N9 N10 107.1(4) . . ? C79 N9 Sb5 129.9(3) . . ? N10 N9 Sb5 122.9(3) . . ? C146 O20 Sb8 123.8(3) . . ? C29 C30 C31 120.4(5) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C89 O17 Sb5 126.8(3) . . ? O18 C108 C99 122.0(4) . . ? O18 C108 C107 117.0(4) . . ? C99 C108 C107 121.0(4) . . ? C115 N14 N13 110.1(4) . . ? C115 N14 H14 124.9 . . ? N13 N14 H14 124.9 . . ? N12 N11 C98 107.0(4) . . ? N12 N11 Sb6 124.5(3) . . ? C98 N11 Sb6 127.7(3) . . ? C147 C152 C151 118.5(4) . . ? C147 C152 Sb8 117.8(3) . . ? C151 C152 Sb8 123.7(3) . . ? C134 N16 N15 110.2(4) . . ? C134 N16 H16 124.9 . . ? N15 N16 H16 124.9 . . ? N6 N5 C41 107.2(4) . . ? N6 N5 Sb3 124.7(3) . . ? C41 N5 Sb3 127.9(3) . . ? C15 C14 C19 119.4(4) . . ? C15 C14 Sb1 122.6(3) . . ? C19 C14 Sb1 118.0(3) . . ? C90 C95 C94 118.7(4) . . ? C90 C95 Sb5 122.1(4) . . ? C94 C95 Sb5 119.2(3) . . ? C129 C128 C133 119.1(4) . . ? C129 C128 Sb7 120.0(3) . . ? C133 C128 Sb7 120.9(3) . . ? C11 C10 C9 120.2(5) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C66 C65 C64 120.7(4) . . ? C66 C65 H65 119.6 . . ? C64 C65 H65 119.6 . . ? C60 N7 N8 107.1(4) . . ? C60 N7 Sb4 125.9(3) . . ? N8 N7 Sb4 125.2(3) . . ? C58 N8 N7 110.5(4) . . ? C58 N8 H8 124.7 . . ? N7 N8 H8 124.7 . . ? C44 C43 C42 121.7(5) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C110 C109 C114 119.3(4) . . ? C110 C109 Sb6 122.5(3) . . ? C114 C109 Sb6 118.1(3) . . ? C77 N10 N9 111.0(4) . . ? C77 N10 H10A 124.5 . . ? N9 N10 H10A 124.5 . . ? O10 C70 C61 122.5(4) . . ? O10 C70 C69 117.0(4) . . ? C61 C70 C69 120.5(4) . . ? C57 C52 C53 119.1(4) . . ? C57 C52 Sb3 119.7(3) . . ? C53 C52 Sb3 121.1(3) . . ? C25 C26 C31 119.7(5) . . ? C25 C26 C27 123.3(5) . . ? C31 C26 C27 117.1(5) . . ? C72 C71 C76 118.7(4) . . ? C72 C71 Sb4 123.9(3) . . ? C76 C71 Sb4 117.3(3) . . ? C48 C49 C50 120.6(4) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C35 C34 C33 120.8(5) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C55 C56 C57 118.6(5) . . ? C55 C56 H56 120.7 . . ? C57 C56 H56 120.7 . . ? C96 N12 N11 110.7(4) . . ? C96 N12 H12 124.6 . . ? N11 N12 H12 124.6 . . ? C120 C121 C126 118.9(5) . . ? C120 C121 C122 123.3(5) . . ? C126 C121 C122 117.9(5) . . ? C131 C132 C133 118.4(4) . . ? C131 C132 H132 120.8 . . ? C133 C132 H132 120.8 . . ? O8 C32 C23 122.8(4) . . ? O8 C32 C31 117.2(4) . . ? C23 C32 C31 120.0(4) . . ? C75 C76 C71 121.2(4) . . ? C75 C76 H76 119.4 . . ? C71 C76 H76 119.4 . . ? C38 C33 C34 119.0(4) . . ? C38 C33 Sb2 117.2(3) . . ? C34 C33 Sb2 123.5(4) . . ? C47 C46 C45 120.6(5) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C136 N15 N16 107.4(4) . . ? C136 N15 Sb8 127.7(3) . . ? N16 N15 Sb8 124.2(3) . . ? C128 C129 C130 121.0(4) . . ? C128 C129 H129 119.5 . . ? C130 C129 H129 119.5 . . ? N3 C22 C21 108.8(4) . . ? N3 C22 C23 120.0(4) . . ? C21 C22 C23 131.0(4) . . ? O9 C51 C42 123.1(4) . . ? O9 C51 C50 117.1(4) . . ? C42 C51 C50 119.7(4) . . ? N5 N6 C39 110.3(4) . . ? N5 N6 H6 124.9 . . ? C39 N6 H6 124.9 . . ? C22 N3 N4 107.2(4) . . ? C22 N3 Sb2 128.1(3) . . ? N4 N3 Sb2 124.2(3) . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? N13 C117 C116 108.4(4) . . ? N13 C117 C118 120.8(4) . . ? C116 C117 C118 130.7(4) . . ? C125 C126 C121 119.1(4) . . ? C125 C126 C127 121.5(4) . . ? C121 C126 C127 119.4(4) . . ? C1 N2 N1 110.6(4) . . ? C1 N2 H2 124.7 . . ? N1 N2 H2 124.7 . . ? C8 C9 C10 121.3(5) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C113 C114 C109 120.5(4) . . ? C113 C114 H114 119.7 . . ? C109 C114 H114 119.7 . . ? C16 C17 C18 121.7(4) . . ? C16 C17 Br1 120.3(4) . . ? C18 C17 Br1 117.9(3) . . ? C127 C118 C119 119.1(4) . . ? C127 C118 C117 121.9(4) . . ? C119 C118 C117 119.1(4) . . ? C50 C45 C44 118.7(4) . . ? C50 C45 C46 118.9(5) . . ? C44 C45 C46 122.4(4) . . ? O20 C146 C137 122.3(4) . . ? O20 C146 C145 116.7(4) . . ? C137 C146 C145 121.0(4) . . ? C68 C67 C66 119.9(5) . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C75 C74 C73 122.2(4) . . ? C75 C74 Br4 118.6(4) . . ? C73 C74 Br4 119.1(4) . . ? C74 C73 C72 118.2(5) . . ? C74 C73 H73 120.9 . . ? C72 C73 H73 120.9 . . ? C96 C97 C98 106.4(4) . . ? C96 C97 H97 126.8 . . ? C98 C97 H97 126.8 . . ? C68 C69 C64 119.6(4) . . ? C68 C69 C70 120.8(4) . . ? C64 C69 C70 119.6(4) . . ? C19 C18 C17 118.9(4) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C58 C59 C60 106.6(4) . . ? C58 C59 H59 126.7 . . ? C60 C59 H59 126.7 . . ? C5 C6 C7 120.5(4) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C87 C88 C83 119.7(5) . . ? C87 C88 C89 120.6(5) . . ? C83 C88 C89 119.6(4) . . ? C89 C80 C81 118.7(5) . . ? C89 C80 C79 121.5(4) . . ? C81 C80 C79 119.8(4) . . ? N4 C20 C21 107.5(4) . . ? N4 C20 H20 126.2 . . ? C21 C20 H20 126.2 . . ? C108 C99 C100 118.2(4) . . ? C108 C99 C98 122.8(4) . . ? C100 C99 C98 119.1(4) . . ? C32 C23 C24 118.8(5) . . ? C32 C23 C22 121.1(4) . . ? C24 C23 C22 120.0(4) . . ? C6 C5 C4 121.4(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C13 C4 C5 119.5(4) . . ? C13 C4 C3 121.3(4) . . ? C5 C4 C3 119.1(4) . . ? C63 C62 C61 121.6(4) . . ? C63 C62 H62 119.2 . . ? C61 C62 H62 119.2 . . ? C108 C107 C106 121.4(4) . . ? C108 C107 C102 119.7(4) . . ? C106 C107 C102 118.9(4) . . ? C39 C40 C41 106.5(5) . . ? C39 C40 H40 126.8 . . ? C41 C40 H40 126.8 . . ? N15 C136 C135 107.8(4) . . ? N15 C136 C137 120.5(4) . . ? C135 C136 C137 131.6(4) . . ? C150 C149 C148 121.9(4) . . ? C150 C149 Br9 119.9(4) . . ? C148 C149 Br9 118.2(4) . . ? C45 C50 C49 119.0(4) . . ? C45 C50 C51 120.1(4) . . ? C49 C50 C51 120.9(4) . . ? N16 C134 C135 107.5(4) . . ? N16 C134 H134 126.2 . . ? C135 C134 H134 126.2 . . ? C120 C119 C118 122.1(5) . . ? C120 C119 H119 119.0 . . ? C118 C119 H119 119.0 . . ? N3 N4 C20 110.7(4) . . ? N3 N4 H4 124.7 . . ? C20 N4 H4 124.7 . . ? N5 C41 C40 108.1(4) . . ? N5 C41 C42 121.3(4) . . ? C40 C41 C42 130.6(5) . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C1 C2 C3 106.0(4) . . ? C1 C2 H2A 127.0 . . ? C3 C2 H2A 127.0 . . ? C132 C133 C128 121.0(4) . . ? C132 C133 H133 119.5 . . ? C128 C133 H133 119.5 . . ? C70 C61 C62 118.7(4) . . ? C70 C61 C60 121.8(4) . . ? C62 C61 C60 119.5(4) . . ? C132 C131 C130 122.2(4) . . ? C132 C131 Br8 118.7(4) . . ? C130 C131 Br8 119.2(4) . . ? C149 C150 C151 118.4(4) . . ? C149 C150 H150 120.8 . . ? C151 C150 H150 120.8 . . ? C65 C64 C63 122.8(4) . . ? C65 C64 C69 118.4(4) . . ? C63 C64 C69 118.8(4) . . ? C27 C28 C29 120.7(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? N1 C3 C2 108.6(4) . . ? N1 C3 C4 120.6(4) . . ? C2 C3 C4 130.8(4) . . ? N9 C79 C78 108.7(4) . . ? N9 C79 C80 121.1(4) . . ? C78 C79 C80 130.1(4) . . ? C115 C116 C117 105.9(4) . . ? C115 C116 H116 127.0 . . ? C117 C116 H116 127.0 . . ? C24 C25 C26 120.2(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? N7 C60 C59 108.3(4) . . ? N7 C60 C61 121.3(4) . . ? C59 C60 C61 130.3(4) . . ? C87 C86 C85 120.4(5) . . ? C87 C86 H86 119.8 . . ? C85 C86 H86 119.8 . . ? C139 C138 C137 121.3(5) . . ? C139 C138 H138 119.4 . . ? C137 C138 H138 119.4 . . ? C131 C130 C129 118.3(4) . . ? C131 C130 H130 120.8 . . ? C129 C130 H130 120.8 . . ? C84 C85 C86 120.2(5) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C113 C112 C111 121.3(5) . . ? C113 C112 Br7 119.3(4) . . ? C111 C112 Br7 119.4(4) . . ? C125 C124 C123 119.2(5) . . ? C125 C124 H124 120.4 . . ? C123 C124 H124 120.4 . . ? C53 C54 C55 119.3(5) . . ? C53 C54 H54 120.4 . . ? C55 C54 H54 120.4 . . ? N11 C98 C97 108.2(4) . . ? N11 C98 C99 120.7(4) . . ? C97 C98 C99 131.1(4) . . ? O7 C13 C4 123.2(4) . . ? O7 C13 C12 116.2(4) . . ? C4 C13 C12 120.5(4) . . ? C95 C90 C91 121.1(5) . . ? C95 C90 H90 119.4 . . ? C91 C90 H90 119.4 . . ? C37 C38 C33 121.3(5) . . ? C37 C38 H38 119.3 . . ? C33 C38 H38 119.3 . . ? C86 C87 C88 120.0(5) . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C30 C31 C26 120.2(5) . . ? C30 C31 C32 120.6(4) . . ? C26 C31 C32 119.2(5) . . ? C67 C68 C69 120.5(4) . . ? C67 C68 H68 119.8 . . ? C69 C68 H68 119.8 . . ? C10 C11 C12 120.7(5) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C38 C37 C36 117.4(5) . . ? C38 C37 H37 121.3 . . ? C36 C37 H37 121.3 . . ? N8 C58 C59 107.5(4) . . ? N8 C58 H58 126.3 . . ? C59 C58 H58 126.3 . . ? C142 C141 C140 120.5(5) . . ? C142 C141 H141 119.8 . . ? C140 C141 H141 119.8 . . ? C119 C120 C121 120.5(5) . . ? C119 C120 H120 119.8 . . ? C121 C120 H120 119.8 . . ? C111 C110 C109 120.2(4) . . ? C111 C110 H110 119.9 . . ? C109 C110 H110 119.9 . . ? C123 C122 C121 121.2(5) . . ? C123 C122 H122 119.4 . . ? C121 C122 H122 119.4 . . ? C77 C78 C79 106.7(4) . . ? C77 C78 H78 126.7 . . ? C79 C78 H78 126.7 . . ? C56 C55 C54 121.4(4) . . ? C56 C55 Br5 119.5(4) . . ? C54 C55 Br5 119.1(4) . . ? C52 C57 C56 121.0(4) . . ? C52 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? C36 C35 C34 118.4(5) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C54 C53 C52 120.6(5) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C71 C72 C73 120.8(4) . . ? C71 C72 H72 119.6 . . ? C73 C72 H72 119.6 . . ? C20 C21 C22 105.8(4) . . ? C20 C21 H21 127.1 . . ? C22 C21 H21 127.1 . . ? C134 C135 C136 107.0(5) . . ? C134 C135 H135 126.5 . . ? C136 C135 H135 126.5 . . ? O17 C89 C80 123.6(4) . . ? O17 C89 C88 116.4(4) . . ? C80 C89 C88 119.8(4) . . ? C62 C63 C64 120.8(4) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? N12 C96 C97 107.6(4) . . ? N12 C96 H96 126.2 . . ? C97 C96 H96 126.2 . . ? C51 C42 C43 119.2(4) . . ? C51 C42 C41 122.1(4) . . ? C43 C42 C41 118.7(4) . . ? C122 C123 C124 121.2(5) . . ? C122 C123 H123 119.4 . . ? C124 C123 H123 119.4 . . ? N2 C1 C2 107.6(4) . . ? N2 C1 H1 126.2 . . ? C2 C1 H1 126.2 . . ? C101 C100 C99 121.7(5) . . ? C101 C100 H100 119.1 . . ? C99 C100 H100 119.1 . . ? C17S C16S C15S 120.5(9) . . ? C17S C16S H16S 119.8 . . ? C15S C16S H16S 119.8 . . ? C146 C137 C138 118.4(5) . . ? C146 C137 C136 122.4(4) . . ? C138 C137 C136 119.1(4) . . ? N14 C115 C116 108.4(4) . . ? N14 C115 H115 125.8 . . ? C116 C115 H115 125.8 . . ? C85 C84 C83 122.2(5) . . ? C85 C84 H84 118.9 . . ? C83 C84 H84 118.9 . . ? C124 C125 C126 121.2(5) . . ? C124 C125 H125 119.4 . . ? C126 C125 H125 119.4 . . ? C101 C102 C107 118.5(4) . . ? C101 C102 C103 122.2(4) . . ? C107 C102 C103 119.2(4) . . ? C18S C19S C20S 117.5(9) . . ? C18S C19S H19S 121.3 . . ? C20S C19S H19S 121.3 . . ? C30 C29 C28 119.9(5) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C6 C7 C8 122.7(4) . . ? C6 C7 C12 119.0(4) . . ? C8 C7 C12 118.3(4) . . ? C49 C48 C47 120.2(5) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C81 C82 C83 120.4(5) . . ? C81 C82 H82 119.8 . . ? C83 C82 H82 119.8 . . ? C104 C103 C102 120.4(5) . . ? C104 C103 H103 119.8 . . ? C102 C103 H103 119.8 . . ? C138 C139 C140 121.2(5) . . ? C138 C139 H139 119.4 . . ? C140 C139 H139 119.4 . . ? C93 C94 C95 121.1(5) . . ? C93 C94 H94 119.4 . . ? C95 C94 H94 119.4 . . ? C144 C143 C142 120.6(5) . . ? C144 C143 H143 119.7 . . ? C142 C143 H143 119.7 . . ? C105 C106 C107 120.2(5) . . ? C105 C106 H106 119.9 . . ? C107 C106 H106 119.9 . . ? C112 C113 C114 119.4(4) . . ? C112 C113 H113 120.3 . . ? C114 C113 H113 120.3 . . ? C84 C83 C82 123.8(5) . . ? C84 C83 C88 117.5(5) . . ? C82 C83 C88 118.7(5) . . ? C11 C12 C13 121.4(4) . . ? C11 C12 C7 119.5(4) . . ? C13 C12 C7 119.1(4) . . ? N10 C77 C78 106.5(4) . . ? N10 C77 H77 126.7 . . ? C78 C77 H77 126.7 . . ? C35 C36 C37 123.0(5) . . ? C35 C36 Br2 118.7(4) . . ? C37 C36 Br2 118.3(4) . . ? C46 C47 C48 120.7(5) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C18 C19 C14 120.2(4) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? N6 C39 C40 107.9(5) . . ? N6 C39 H39 126.0 . . ? C40 C39 H39 126.0 . . ? C143 C144 C145 120.6(5) . . ? C143 C144 H144 119.7 . . ? C145 C144 H144 119.7 . . ? C43 C44 C45 120.5(5) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C100 C101 C102 120.8(4) . . ? C100 C101 H101 119.6 . . ? C102 C101 H101 119.6 . . ? C110 C111 C112 119.3(5) . . ? C110 C111 H111 120.4 . . ? C112 C111 H111 120.4 . . ? C141 C142 C143 120.8(5) . . ? C141 C142 H142 119.6 . . ? C143 C142 H142 119.6 . . ? C19S C18S C17S 124.0(8) . . ? C19S C18S H18S 118.0 . . ? C17S C18S H18S 118.0 . . ? C152 C151 C150 121.2(4) . . ? C152 C151 H151 119.4 . . ? C150 C151 H151 119.4 . . ? C82 C81 C80 122.6(5) . . ? C82 C81 H81 118.7 . . ? C80 C81 H81 118.7 . . ? C25 C24 C23 122.1(5) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C28 C27 C26 121.8(5) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C74 C75 C76 118.9(4) . . ? C74 C75 H75 120.6 . . ? C76 C75 H75 120.6 . . ? C140 C145 C144 118.3(4) . . ? C140 C145 C146 120.0(4) . . ? C144 C145 C146 121.7(4) . . ? C141 C140 C145 119.2(5) . . ? C141 C140 C139 122.6(5) . . ? C145 C140 C139 118.2(5) . . ? C15S C20S C19S 120.1(7) . . ? C15S C20S C21S 122.0(9) . . ? C19S C20S C21S 117.8(9) . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C16S C17S C18S 117.5(8) . . ? C16S C17S H17S 121.2 . . ? C18S C17S H17S 121.2 . . ? C20S C15S C16S 120.4(7) . . ? C20S C15S H15S 119.8 . . ? C16S C15S H15S 119.8 . . ? C65 C66 C67 120.8(4) . . ? C65 C66 H66 119.6 . . ? C67 C66 H66 119.6 . . ? C70 O10 Sb4 122.8(3) . . ? C94 C93 C92 118.8(5) . . ? C94 C93 H93 120.6 . . ? C92 C93 H93 120.6 . . ? C91 C92 C93 122.0(5) . . ? C91 C92 Br6 119.5(4) . . ? C93 C92 Br6 118.5(4) . . ? C103 C104 C105 120.7(5) . . ? C103 C104 H104 119.6 . . ? C105 C104 H104 119.6 . . ? C106 C105 C104 120.5(5) . . ? C106 C105 H105 119.7 . . ? C104 C105 H105 119.7 . . ? C92 C91 C90 118.2(5) . . ? C92 C91 H91 120.9 . . ? C90 C91 H91 120.9 . . ? C152 C147 C148 121.5(5) . . ? C152 C147 H147 119.3 . . ? C148 C147 H147 119.3 . . ? C149 C148 C147 118.5(5) . . ? C149 C148 H148 120.8 . . ? C147 C148 H148 120.8 . . ? C12S C13S C8S 117.5(7) . . ? C12S C13S C14S 122.9(7) . . ? C8S C13S C14S 119.6(7) . . ? C10S C11S C12S 117.9(8) . . ? C10S C11S H11S 121.1 . . ? C12S C11S H11S 121.1 . . ? C11S C12S C13S 122.7(8) . . ? C11S C12S H12S 118.6 . . ? C13S C12S H12S 118.6 . . ? C11S C10S C9S 122.9(8) . . ? C11S C10S H10S 118.5 . . ? C9S C10S H10S 118.5 . . ? C5S C6S C1S 116.5(8) . . ? C5S C6S C7S 122.8(8) . . ? C1S C6S C7S 120.7(8) . . ? C10S C9S C8S 118.0(8) . . ? C10S C9S H9S 121.0 . . ? C8S C9S H9S 121.0 . . ? C2S C1S C6S 121.7(8) . . ? C2S C1S H1S 119.2 . . ? C6S C1S H1S 119.2 . . ? C13S C8S C9S 120.9(8) . . ? C13S C8S H8S 119.6 . . ? C9S C8S H8S 119.6 . . ? C1S C2S C3S 120.9(8) . . ? C1S C2S H2S 119.5 . . ? C3S C2S H2S 119.5 . . ? C13S C14S H14A 109.5 . . ? C13S C14S H14B 109.5 . . ? H14A C14S H14B 109.5 . . ? C13S C14S H14C 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? C6S C5S C4S 121.2(8) . . ? C6S C5S H5S 119.4 . . ? C4S C5S H5S 119.4 . . ? C6S C7S H7S1 109.5 . . ? C6S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C6S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C3S C4S C5S 120.3(9) . . ? C3S C4S H4S 119.8 . . ? C5S C4S H4S 119.8 . . ? C4S C3S C2S 119.3(9) . . ? C4S C3S H3S 120.3 . . ? C2S C3S H3S 120.3 . . ? C20S C21S H21A 109.5 . . ? C20S C21S H21B 109.5 . . ? H21A C21S H21B 109.5 . . ? C20S C21S H21C 109.5 . . ? H21A C21S H21C 109.5 . . ? H21B C21S H21C 109.5 . . ? O19 C127 C118 123.5(4) . . ? O19 C127 C126 116.5(4) . . ? C118 C127 C126 119.9(4) . . ? C164 C163 N17 112.2(9) . . ? C164 C163 C162 132.2(9) . . ? N17 C163 C162 115.5(8) . . ? C162 C161 C160 119.2(8) . . ? C162 C161 H161 120.4 . . ? C160 C161 H161 120.4 . . ? C159 C160 C161 125.6(8) . . ? C159 C160 H160 117.2 . . ? C161 C160 H160 117.2 . . ? C160 C159 C158 122.2(6) . . ? C160 C159 C154 113.6(6) . . ? C158 C159 C154 124.1(6) . . ? C161 C162 C153 116.9(8) . . ? C161 C162 C163 117.0(7) . . ? C153 C162 C163 126.1(7) . . ? C162 C153 C154 122.1(7) . . ? C162 C153 O21 119.7(7) . . ? C154 C153 O21 118.2(7) . . ? C155 C154 C159 116.0(6) . . ? C155 C154 C153 121.4(6) . . ? C159 C154 C153 122.6(6) . . ? C156 C155 C154 123.2(8) . . ? C156 C155 H155 118.4 . . ? C154 C155 H155 118.4 . . ? C155 C156 C157 117.4(8) . . ? C155 C156 H156 121.3 . . ? C157 C156 H156 121.3 . . ? C157 C158 C159 116.4(7) . . ? C157 C158 H158 121.8 . . ? C159 C158 H158 121.8 . . ? C158 C157 C156 122.8(8) . . ? C158 C157 H157 118.6 . . ? C156 C157 H157 118.6 . . ? N18 C165 C164 103.9(8) . . ? N18 C165 H165 128.0 . . ? C164 C165 H165 128.0 . . ? C163 C164 C165 108.4(9) . . ? C163 C164 H164 125.8 . . ? C165 C164 H164 125.8 . . ? C153 O21 H21D 109.5 . . ? C163 N17 N18 105.0(8) . . ? N17 N18 C165 110.5(7) . . ? N17 N18 H18A 124.8 . . ? C165 N18 H18A 124.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.955 _refine_diff_density_min -3.023 _refine_diff_density_rms 0.127 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 409.4 76.0 2 0.162 0.679 0.288 56.2 9.0 3 0.291 0.415 0.187 13.5 0.7 4 0.382 0.383 0.268 13.2 0.2 5 0.390 0.714 0.198 14.8 -0.5 6 0.408 0.618 0.469 9.5 0.3 7 0.591 0.382 0.531 9.4 0.4 8 0.610 0.286 0.802 14.8 -0.4 9 0.622 0.615 0.736 13.7 0.1 10 0.715 0.584 0.817 13.0 0.6 11 0.838 0.321 0.712 56.1 8.3 _platon_squeeze_details ; ; #==========================================================END data_5 _database_code_depnum_ccdc_archive 'CCDC 808831' #TrackingRef '- cif all in one.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H64 Cl4 N8 O8 Sb4' _chemical_formula_sum 'C90 H64 Cl4 N8 O8 Sb4' _chemical_formula_weight 2014.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 11.1209(9) _cell_length_b 11.5866(10) _cell_length_c 17.2087(14) _cell_angle_alpha 83.262(2) _cell_angle_beta 81.3270(10) _cell_angle_gamma 69.8120(10) _cell_volume 2052.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4010 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7155 _exptl_absorpt_correction_T_max 0.8410 _exptl_absorpt_process_details brukarsadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 19965 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7219 _reflns_number_gt 6117 _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. one heavily disorded solvent toluene molecule has been squeezed out for the better refinement convergence. ; _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^)+(0.0397P)^2^+1.0070P] 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 7219 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 C1 C 0.3189(5) 0.3869(5) 0.7212(3) 0.0160(12) Uani 1 1 d . . . C2 C 0.4342(5) 0.2924(5) 0.7427(3) 0.0160(12) Uani 1 1 d . . . C3 C 0.5161(5) 0.2108(5) 0.6882(3) 0.0197(13) Uani 1 1 d . . . H3 H 0.4960 0.2176 0.6369 0.024 Uiso 1 1 calc R . . C4 C 0.6250(5) 0.1212(5) 0.7098(3) 0.0218(13) Uani 1 1 d . . . H4 H 0.6784 0.0677 0.6729 0.026 Uiso 1 1 calc R . . C5 C 0.6579(5) 0.1083(5) 0.7866(3) 0.0221(13) Uani 1 1 d . . . H5 H 0.7329 0.0474 0.8004 0.026 Uiso 1 1 calc R . . C6 C 0.5781(6) 0.1867(5) 0.8411(3) 0.0263(14) Uani 1 1 d . . . H6 H 0.5988 0.1776 0.8924 0.032 Uiso 1 1 calc R . . C7 C 0.4659(5) 0.2802(5) 0.8206(3) 0.0200(13) Uani 1 1 d . . . C8 C 0.3828(5) 0.3628(5) 0.8761(3) 0.0224(13) Uani 1 1 d . . . H8 H 0.4030 0.3563 0.9273 0.027 Uiso 1 1 calc R . . C9 C 0.2734(5) 0.4514(5) 0.8543(3) 0.0201(13) Uani 1 1 d . . . H9 H 0.2198 0.5043 0.8914 0.024 Uiso 1 1 calc R . . C10 C 0.2389(5) 0.4656(5) 0.7770(3) 0.0187(12) Uani 1 1 d . . . C11 C 0.1201(5) 0.5643(5) 0.7584(3) 0.0152(12) Uani 1 1 d . . . C12 C 0.0441(5) 0.6712(5) 0.7954(3) 0.0189(13) Uani 1 1 d . . . H12 H 0.0583 0.6993 0.8405 0.023 Uiso 1 1 calc R . . C13 C -0.0567(5) 0.7264(5) 0.7504(3) 0.0162(12) Uani 1 1 d . . . H13 H -0.1243 0.7989 0.7614 0.019 Uiso 1 1 calc R . . C14 C 0.0876(5) 0.2825(5) 0.6943(3) 0.0160(12) Uani 1 1 d . . . C15 C 0.1828(5) 0.1667(5) 0.7052(3) 0.0206(13) Uani 1 1 d . . . H15 H 0.2638 0.1494 0.6760 0.025 Uiso 1 1 calc R . . C16 C 0.1557(5) 0.0793(5) 0.7591(3) 0.0206(13) Uani 1 1 d . . . H16 H 0.2183 0.0026 0.7669 0.025 Uiso 1 1 calc R . . C17 C 0.0357(6) 0.1057(5) 0.8014(3) 0.0212(13) Uani 1 1 d . . . C18 C -0.0590(5) 0.2197(5) 0.7916(3) 0.0225(13) Uani 1 1 d . . . H18 H -0.1396 0.2367 0.8211 0.027 Uiso 1 1 calc R . . C19 C -0.0318(5) 0.3065(5) 0.7380(3) 0.0175(12) Uani 1 1 d . . . H19 H -0.0949 0.3831 0.7308 0.021 Uiso 1 1 calc R . . C20 C -0.1357(5) 0.9122(5) 0.4962(3) 0.0137(12) Uani 1 1 d . . . C21 C -0.2296(5) 1.0248(5) 0.4707(3) 0.0161(12) Uani 1 1 d . . . C22 C -0.3590(5) 1.0617(5) 0.5069(3) 0.0208(13) Uani 1 1 d . . . H22 H -0.3851 1.0111 0.5469 0.025 Uiso 1 1 calc R . . C23 C -0.4460(5) 1.1723(5) 0.4828(3) 0.0243(14) Uani 1 1 d . . . H23 H -0.5314 1.1957 0.5058 0.029 Uiso 1 1 calc R . . C24 C -0.4063(6) 1.2498(5) 0.4237(3) 0.0256(14) Uani 1 1 d . . . H24 H -0.4643 1.3268 0.4102 0.031 Uiso 1 1 calc R . . C25 C -0.2845(5) 1.2141(5) 0.3859(3) 0.0208(13) Uani 1 1 d . . . H25 H -0.2613 1.2657 0.3453 0.025 Uiso 1 1 calc R . . C26 C -0.1925(5) 1.1001(5) 0.4070(3) 0.0171(12) Uani 1 1 d . . . C27 C -0.0666(5) 1.0579(5) 0.3669(3) 0.0192(13) Uani 1 1 d . . . H27 H -0.0417 1.1063 0.3249 0.023 Uiso 1 1 calc R . . C28 C 0.0190(5) 0.9465(5) 0.3893(3) 0.0171(12) Uani 1 1 d . . . H28 H 0.1007 0.9191 0.3612 0.021 Uiso 1 1 calc R . . C29 C -0.0140(5) 0.8718(5) 0.4547(3) 0.0160(12) Uani 1 1 d . . . C30 C 0.0821(5) 0.7547(5) 0.4748(3) 0.0172(12) Uani 1 1 d . . . C31 C 0.2132(5) 0.7030(5) 0.4483(3) 0.0211(13) Uani 1 1 d . . . H31 H 0.2624 0.7383 0.4111 0.025 Uiso 1 1 calc R . . C32 C 0.2546(5) 0.5897(5) 0.4884(3) 0.0190(13) Uani 1 1 d . . . H32 H 0.3383 0.5342 0.4825 0.023 Uiso 1 1 calc R . . C33 C -0.3049(5) 0.6885(5) 0.6559(3) 0.0172(12) Uani 1 1 d . . . C34 C -0.3390(5) 0.5858(5) 0.6841(3) 0.0184(12) Uani 1 1 d . . . H34 H -0.2887 0.5092 0.6662 0.022 Uiso 1 1 calc R . . C35 C -0.4468(5) 0.5951(5) 0.7385(3) 0.0171(12) Uani 1 1 d . . . H35 H -0.4700 0.5261 0.7569 0.021 Uiso 1 1 calc R . . C36 C -0.5187(5) 0.7098(5) 0.7645(3) 0.0211(13) Uani 1 1 d . . . C37 C -0.4859(5) 0.8125(5) 0.7389(3) 0.0201(13) Uani 1 1 d . . . H37 H -0.5355 0.8885 0.7580 0.024 Uiso 1 1 calc R . . C38 C -0.3786(5) 0.8027(5) 0.6845(3) 0.0175(12) Uani 1 1 d . . . H38 H -0.3556 0.8721 0.6669 0.021 Uiso 1 1 calc R . . C39 C 0.7516(8) 0.5324(8) 0.9005(4) 0.052(2) Uani 1 1 d . . . H39 H 0.7308 0.6087 0.8722 0.062 Uiso 1 1 calc R . . C40 C 0.8773(8) 0.4708(7) 0.9157(4) 0.048(2) Uani 1 1 d . . . H40 H 0.9407 0.5061 0.8975 0.058 Uiso 1 1 calc R . . C41 C 0.9101(7) 0.3566(7) 0.9578(4) 0.0435(19) Uani 1 1 d . . . C42 C 0.8138(7) 0.3054(6) 0.9848(4) 0.0370(17) Uani 1 1 d . . . H42 H 0.8333 0.2293 1.0134 0.044 Uiso 1 1 calc R . . C43 C 0.6892(7) 0.3691(7) 0.9687(4) 0.0427(18) Uani 1 1 d . . . H43 H 0.6250 0.3347 0.9867 0.051 Uiso 1 1 calc R . . C44 C 0.6576(8) 0.4810(8) 0.9271(4) 0.055(2) Uani 1 1 d . . . H44 H 0.5729 0.5221 0.9169 0.066 Uiso 1 1 calc R . . C45 C 1.0451(7) 0.2892(8) 0.9705(5) 0.062(2) Uani 1 1 d . . . H45A H 1.0975 0.2753 0.9205 0.093 Uiso 1 1 calc R . . H45B H 1.0510 0.2115 0.9990 0.093 Uiso 1 1 calc R . . H45C H 1.0750 0.3368 1.0003 0.093 Uiso 1 1 calc R . . Cl2 Cl -0.65607(14) 0.72465(14) 0.83149(9) 0.0290(4) Uani 1 1 d . . . Cl1 Cl 0.00108(15) -0.00644(14) 0.86909(9) 0.0343(4) Uani 1 1 d . . . N1 N 0.0654(4) 0.5605(4) 0.6948(2) 0.0156(10) Uani 1 1 d . . . N2 N -0.0431(4) 0.6608(4) 0.6892(2) 0.0155(10) Uani 1 1 d . . . N3 N 0.0510(4) 0.6729(4) 0.5286(2) 0.0138(10) Uani 1 1 d . . . N4 N 0.1568(4) 0.5710(4) 0.5371(3) 0.0152(10) Uani 1 1 d . . . O2 O -0.0539(3) 0.4946(3) 0.58935(19) 0.0124(8) Uani 1 1 d . . . O1 O -0.1972(3) 0.6771(3) 0.4779(2) 0.0135(8) Uani 1 1 d . . . O3 O 0.2980(3) 0.3963(3) 0.6440(2) 0.0151(8) Uani 1 1 d . . . O4 O -0.1716(3) 0.8542(3) 0.5650(2) 0.0144(8) Uani 1 1 d . . . Sb1 Sb 0.12473(3) 0.42070(3) 0.61211(2) 0.01373(11) Uani 1 1 d . . . Sb2 Sb -0.13478(3) 0.67255(3) 0.57844(2) 0.01308(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(3) 0.018(3) 0.019(3) -0.004(2) 0.000(2) -0.010(2) C2 0.021(3) 0.017(3) 0.015(3) -0.001(2) -0.002(2) -0.013(2) C3 0.019(3) 0.025(3) 0.018(3) -0.001(2) 0.000(2) -0.011(3) C4 0.016(3) 0.020(3) 0.023(3) 0.004(3) 0.004(3) -0.004(2) C5 0.019(3) 0.021(3) 0.022(3) 0.005(3) -0.005(3) -0.002(3) C6 0.030(4) 0.025(3) 0.021(3) -0.001(3) -0.004(3) -0.005(3) C7 0.021(3) 0.019(3) 0.021(3) 0.004(2) -0.002(3) -0.010(3) C8 0.024(3) 0.027(3) 0.017(3) 0.003(3) -0.007(3) -0.008(3) C9 0.020(3) 0.024(3) 0.016(3) -0.005(2) 0.004(2) -0.009(3) C10 0.022(3) 0.021(3) 0.018(3) -0.001(2) 0.000(2) -0.014(3) C11 0.021(3) 0.019(3) 0.009(3) 0.001(2) 0.005(2) -0.014(2) C12 0.023(3) 0.019(3) 0.014(3) -0.004(2) 0.001(2) -0.006(3) C13 0.013(3) 0.016(3) 0.016(3) -0.005(2) 0.008(2) -0.004(2) C14 0.014(3) 0.018(3) 0.015(3) -0.001(2) 0.001(2) -0.005(2) C15 0.013(3) 0.018(3) 0.025(3) 0.000(3) -0.001(2) 0.001(2) C16 0.020(3) 0.016(3) 0.025(3) -0.001(3) -0.009(3) -0.001(2) C17 0.032(3) 0.021(3) 0.015(3) 0.005(2) -0.004(3) -0.017(3) C18 0.020(3) 0.025(3) 0.019(3) -0.004(3) 0.004(3) -0.006(3) C19 0.017(3) 0.017(3) 0.014(3) -0.001(2) 0.001(2) -0.002(2) C20 0.019(3) 0.013(3) 0.011(3) 0.000(2) -0.003(2) -0.008(2) C21 0.016(3) 0.018(3) 0.014(3) -0.007(2) 0.003(2) -0.006(2) C22 0.025(3) 0.024(3) 0.014(3) 0.002(2) -0.001(2) -0.010(3) C23 0.017(3) 0.031(4) 0.020(3) -0.005(3) 0.005(3) -0.004(3) C24 0.028(3) 0.024(3) 0.019(3) -0.003(3) -0.010(3) 0.003(3) C25 0.029(3) 0.022(3) 0.013(3) 0.000(2) -0.001(3) -0.010(3) C26 0.018(3) 0.019(3) 0.017(3) 0.002(2) -0.004(2) -0.009(2) C27 0.023(3) 0.023(3) 0.016(3) 0.000(2) -0.001(2) -0.013(3) C28 0.014(3) 0.025(3) 0.012(3) -0.009(2) 0.006(2) -0.007(2) C29 0.017(3) 0.018(3) 0.017(3) -0.007(2) -0.002(2) -0.010(2) C30 0.017(3) 0.017(3) 0.019(3) -0.001(2) 0.000(2) -0.009(2) C31 0.020(3) 0.028(3) 0.019(3) -0.003(3) 0.004(2) -0.015(3) C32 0.012(3) 0.020(3) 0.022(3) -0.005(3) 0.002(2) -0.001(2) C33 0.012(3) 0.022(3) 0.018(3) -0.004(2) 0.002(2) -0.006(2) C34 0.014(3) 0.019(3) 0.018(3) 0.000(2) -0.006(2) 0.000(2) C35 0.014(3) 0.020(3) 0.017(3) 0.003(2) -0.001(2) -0.008(2) C36 0.017(3) 0.029(3) 0.017(3) 0.000(3) 0.001(2) -0.008(3) C37 0.022(3) 0.019(3) 0.014(3) -0.005(2) 0.002(2) -0.001(2) C38 0.017(3) 0.018(3) 0.018(3) 0.001(2) 0.002(2) -0.009(2) C39 0.050(5) 0.063(5) 0.040(5) -0.015(4) 0.019(4) -0.021(4) C40 0.076(6) 0.036(4) 0.039(4) -0.006(4) 0.016(4) -0.033(4) C41 0.046(5) 0.058(5) 0.028(4) -0.013(4) 0.012(3) -0.022(4) C42 0.054(5) 0.040(4) 0.019(3) -0.006(3) 0.001(3) -0.019(4) C43 0.042(5) 0.067(5) 0.023(4) -0.011(4) 0.006(3) -0.026(4) C44 0.051(5) 0.068(6) 0.029(4) -0.005(4) 0.005(4) -0.002(4) C45 0.049(5) 0.088(7) 0.053(5) -0.012(5) 0.004(4) -0.032(5) Cl2 0.0215(8) 0.0351(9) 0.0262(8) -0.0033(7) 0.0115(6) -0.0097(7) Cl1 0.0366(9) 0.0272(8) 0.0348(9) 0.0116(7) -0.0004(7) -0.0112(7) N1 0.017(2) 0.016(2) 0.013(2) 0.0013(19) 0.0007(19) -0.007(2) N2 0.015(2) 0.016(2) 0.013(2) -0.0030(19) 0.0029(19) -0.004(2) N3 0.012(2) 0.016(2) 0.015(2) -0.0020(19) 0.0003(19) -0.0081(19) N4 0.012(2) 0.013(2) 0.017(2) -0.0010(19) 0.0021(19) -0.0021(19) O2 0.0088(18) 0.0114(18) 0.0135(19) -0.0008(15) -0.0006(15) 0.0008(15) O1 0.0099(18) 0.0159(19) 0.0124(19) -0.0077(15) 0.0011(15) -0.0003(15) O3 0.0073(18) 0.024(2) 0.012(2) -0.0024(16) -0.0023(15) -0.0020(16) O4 0.017(2) 0.0138(19) 0.0126(19) -0.0037(15) 0.0036(15) -0.0066(16) Sb1 0.0117(2) 0.0152(2) 0.0126(2) -0.00214(15) 0.00076(15) -0.00295(15) Sb2 0.01126(19) 0.0139(2) 0.0126(2) -0.00171(15) 0.00204(14) -0.00355(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.368(6) . ? C1 C10 1.391(7) . ? C1 C2 1.435(7) . ? C2 C3 1.399(7) . ? C2 C7 1.416(7) . ? C3 C4 1.364(7) . ? C3 H3 0.9300 . ? C4 C5 1.401(8) . ? C4 H4 0.9300 . ? C5 C6 1.373(8) . ? C5 H5 0.9300 . ? C6 C7 1.402(8) . ? C6 H6 0.9300 . ? C7 C8 1.422(8) . ? C8 C9 1.364(8) . ? C8 H8 0.9300 . ? C9 C10 1.415(7) . ? C9 H9 0.9300 . ? C10 C11 1.468(8) . ? C11 N1 1.342(7) . ? C11 C12 1.397(7) . ? C12 C13 1.384(7) . ? C12 H12 0.9300 . ? C13 N2 1.330(6) . ? C13 H13 0.9300 . ? C14 C19 1.378(7) . ? C14 C15 1.407(7) . ? C14 Sb1 2.117(5) . ? C15 C16 1.372(8) . ? C15 H15 0.9300 . ? C16 C17 1.372(8) . ? C16 H16 0.9300 . ? C17 C18 1.387(8) . ? C17 Cl1 1.746(5) . ? C18 C19 1.365(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O4 1.367(6) . ? C20 C29 1.383(7) . ? C20 C21 1.431(7) . ? C21 C22 1.417(7) . ? C21 C26 1.422(7) . ? C22 C23 1.375(8) . ? C22 H22 0.9300 . ? C23 C24 1.399(8) . ? C23 H23 0.9300 . ? C24 C25 1.356(8) . ? C24 H24 0.9300 . ? C25 C26 1.411(7) . ? C25 H25 0.9300 . ? C26 C27 1.411(8) . ? C27 C28 1.367(7) . ? C27 H27 0.9300 . ? C28 C29 1.420(7) . ? C28 H28 0.9300 . ? C29 C30 1.450(7) . ? C30 N3 1.340(7) . ? C30 C31 1.398(7) . ? C31 C32 1.370(8) . ? C31 H31 0.9300 . ? C32 N4 1.334(6) . ? C32 H32 0.9300 . ? C33 C34 1.384(7) . ? C33 C38 1.395(7) . ? C33 Sb2 2.109(5) . ? C34 C35 1.386(7) . ? C34 H34 0.9300 . ? C35 C36 1.380(7) . ? C35 H35 0.9300 . ? C36 C37 1.368(8) . ? C36 Cl2 1.739(5) . ? C37 C38 1.381(7) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C44 1.370(10) . ? C39 C40 1.383(10) . ? C39 H39 0.9300 . ? C40 C41 1.389(10) . ? C40 H40 0.9300 . ? C41 C42 1.392(9) . ? C41 C45 1.470(10) . ? C42 C43 1.380(9) . ? C42 H42 0.9300 . ? C43 C44 1.365(10) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? N1 N2 1.362(6) . ? N1 Sb1 2.146(4) . ? N2 Sb2 2.264(4) . ? N3 N4 1.362(6) . ? N3 Sb2 2.116(4) . ? N4 Sb1 2.141(4) . ? O2 Sb2 1.943(3) . ? O2 Sb1 1.953(3) . ? O1 Sb1 1.933(3) 2_566 ? O1 Sb2 1.948(3) . ? O3 Sb1 2.000(3) . ? O4 Sb2 1.992(3) . ? Sb1 O1 1.933(3) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C1 C10 124.0(5) . . ? O3 C1 C2 116.2(4) . . ? C10 C1 C2 119.8(5) . . ? C3 C2 C7 119.0(5) . . ? C3 C2 C1 121.3(5) . . ? C7 C2 C1 119.7(5) . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 121.2(5) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 119.3(5) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 120.9(5) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 119.2(5) . . ? C6 C7 C8 121.6(5) . . ? C2 C7 C8 119.1(5) . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 122.2(5) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C1 C10 C9 119.2(5) . . ? C1 C10 C11 122.3(5) . . ? C9 C10 C11 118.6(5) . . ? N1 C11 C12 107.5(5) . . ? N1 C11 C10 120.0(5) . . ? C12 C11 C10 132.5(5) . . ? C13 C12 C11 105.3(5) . . ? C13 C12 H12 127.4 . . ? C11 C12 H12 127.4 . . ? N2 C13 C12 110.2(5) . . ? N2 C13 H13 124.9 . . ? C12 C13 H13 124.9 . . ? C19 C14 C15 119.4(5) . . ? C19 C14 Sb1 119.5(4) . . ? C15 C14 Sb1 121.1(4) . . ? C16 C15 C14 119.6(5) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.6(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 121.4(5) . . ? C16 C17 Cl1 119.4(4) . . ? C18 C17 Cl1 119.1(4) . . ? C19 C18 C17 118.9(5) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C14 121.1(5) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? O4 C20 C29 123.5(5) . . ? O4 C20 C21 116.1(4) . . ? C29 C20 C21 120.2(5) . . ? C22 C21 C26 119.4(5) . . ? C22 C21 C20 121.4(5) . . ? C26 C21 C20 119.2(5) . . ? C23 C22 C21 120.0(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.1(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.9(5) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 121.1(5) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 122.6(5) . . ? C27 C26 C21 119.2(5) . . ? C25 C26 C21 118.2(5) . . ? C28 C27 C26 120.5(5) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 121.4(5) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C20 C29 C28 119.3(5) . . ? C20 C29 C30 122.5(5) . . ? C28 C29 C30 118.2(5) . . ? N3 C30 C31 107.1(5) . . ? N3 C30 C29 120.8(5) . . ? C31 C30 C29 132.1(5) . . ? C32 C31 C30 106.0(5) . . ? C32 C31 H31 127.0 . . ? C30 C31 H31 127.0 . . ? N4 C32 C31 109.8(5) . . ? N4 C32 H32 125.1 . . ? C31 C32 H32 125.1 . . ? C34 C33 C38 119.3(5) . . ? C34 C33 Sb2 121.1(4) . . ? C38 C33 Sb2 119.5(4) . . ? C33 C34 C35 121.1(5) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 118.1(5) . . ? C36 C35 H35 121.0 . . ? C34 C35 H35 121.0 . . ? C37 C36 C35 122.1(5) . . ? C37 C36 Cl2 118.9(4) . . ? C35 C36 Cl2 119.0(4) . . ? C36 C37 C38 119.6(5) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C33 119.9(5) . . ? C37 C38 H38 120.1 . . ? C33 C38 H38 120.1 . . ? C44 C39 C40 120.1(8) . . ? C44 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 120.7(7) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C40 C41 C42 118.8(7) . . ? C40 C41 C45 120.3(7) . . ? C42 C41 C45 120.8(7) . . ? C43 C42 C41 119.1(7) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C44 C43 C42 121.9(7) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C43 C44 C39 119.4(8) . . ? C43 C44 H44 120.3 . . ? C39 C44 H44 120.3 . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C11 N1 N2 109.9(4) . . ? C11 N1 Sb1 128.5(4) . . ? N2 N1 Sb1 121.5(3) . . ? C13 N2 N1 107.1(4) . . ? C13 N2 Sb2 139.7(4) . . ? N1 N2 Sb2 113.0(3) . . ? C30 N3 N4 109.8(4) . . ? C30 N3 Sb2 128.3(4) . . ? N4 N3 Sb2 120.7(3) . . ? C32 N4 N3 107.3(4) . . ? C32 N4 Sb1 136.4(4) . . ? N3 N4 Sb1 116.0(3) . . ? Sb2 O2 Sb1 120.82(17) . . ? Sb1 O1 Sb2 131.96(18) 2_566 . ? C1 O3 Sb1 122.4(3) . . ? C20 O4 Sb2 122.6(3) . . ? O1 Sb1 O2 99.73(14) 2_566 . ? O1 Sb1 O3 93.14(14) 2_566 . ? O2 Sb1 O3 162.79(14) . . ? O1 Sb1 C14 98.72(17) 2_566 . ? O2 Sb1 C14 94.34(17) . . ? O3 Sb1 C14 94.95(17) . . ? O1 Sb1 N4 86.23(15) 2_566 . ? O2 Sb1 N4 85.11(15) . . ? O3 Sb1 N4 84.38(15) . . ? C14 Sb1 N4 175.04(18) . . ? O1 Sb1 N1 165.68(15) 2_566 . ? O2 Sb1 N1 82.92(15) . . ? O3 Sb1 N1 81.86(15) . . ? C14 Sb1 N1 95.09(18) . . ? N4 Sb1 N1 79.95(16) . . ? O2 Sb2 O1 95.82(14) . . ? O2 Sb2 O4 165.40(14) . . ? O1 Sb2 O4 90.21(14) . . ? O2 Sb2 C33 98.72(18) . . ? O1 Sb2 C33 100.35(17) . . ? O4 Sb2 C33 93.24(18) . . ? O2 Sb2 N3 84.83(15) . . ? O1 Sb2 N3 95.13(15) . . ? O4 Sb2 N3 81.38(15) . . ? C33 Sb2 N3 163.65(18) . . ? O2 Sb2 N2 81.99(14) . . ? O1 Sb2 N2 174.58(14) . . ? O4 Sb2 N2 90.81(15) . . ? C33 Sb2 N2 84.91(18) . . ? N3 Sb2 N2 79.77(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.390 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.131 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 1.000 210.9 45.9 _platon_squeeze_details ; ;