#------------------------------------------------------------------------------ #$Date: 2019-05-17 04:33:54 +0300 (Fri, 17 May 2019) $ #$Revision: 215229 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700008.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7700008 loop_ _publ_author_name 'Liu, Xiaoqing' 'Wang, Yu-Xia' 'Han, Zongsu' 'Han, Tian' 'Shi, Wei' 'Peng, Cheng' _publ_section_title ; Tuning the Magnetization Dynamics of TbIII-Based Single-Chain Magnets Through Substitution on the Nitronyl Nitroxide Radical ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT01704F _journal_year 2019 _chemical_formula_moiety '0.5(C64 H44 F36 N4 O16 S2 Tb2)' _chemical_formula_sum 'C32 H22 F18 N2 O8 S Tb' _chemical_formula_weight 1095.49 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-01-10 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-03-22 deposited with the CCDC. 2019-05-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 129.695(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 20.8845(9) _cell_length_b 17.2985(7) _cell_length_c 29.7057(11) _cell_measurement_reflns_used 6834 _cell_measurement_temperature 120(10) _cell_measurement_theta_max 29.2117 _cell_measurement_theta_min 2.9168 _cell_volume 8257.6(6) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 120(10) _diffrn_detector_area_resol_mean 16.2116 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 39.00 93.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 18.1935 178.0000 90.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega -95.00 -36.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -18.6622 -178.0000 150.0000 59 #__ type_ start__ end____ width___ exp.time_ 3 omega -95.00 -39.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -18.6622 -178.0000 -30.0000 56 #__ type_ start__ end____ width___ exp.time_ 4 omega 17.00 49.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -18.6622 37.0000 120.0000 32 #__ type_ start__ end____ width___ exp.time_ 5 omega -56.00 3.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -18.6622 -57.0000 120.0000 59 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0098778000 _diffrn_orient_matrix_UB_12 -0.0362159000 _diffrn_orient_matrix_UB_13 0.0106499000 _diffrn_orient_matrix_UB_21 0.0304382000 _diffrn_orient_matrix_UB_22 -0.0044729000 _diffrn_orient_matrix_UB_23 0.0157392000 _diffrn_orient_matrix_UB_31 -0.0116610000 _diffrn_orient_matrix_UB_32 0.0186716000 _diffrn_orient_matrix_UB_33 0.0245683000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_unetI/netI 0.0904 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 36659 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.009 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_min 2.923 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.893 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic light blue' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.762 _exptl_crystal_description plate _exptl_crystal_F_000 4280 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.405 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.135 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1185 _refine_ls_number_reflns 14526 _refine_ls_number_restraints 132 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0441 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.0796 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11283 _reflns_number_total 14526 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01704f2.cif _cod_data_source_block 1 _cod_database_code 7700008 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C1H1N1O1TB1 _chemical_oxdiff_usercomment TBL11A _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.764 _shelx_estimated_absorpt_t_min 0.703 _reflns_odcompleteness_completeness 99.78 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C59-F30A 1.31 with sigma of 0.02 C59-F28B 1.31 with sigma of 0.02 C59-F29B 1.31 with sigma of 0.02 F30A-F29B 2.2 with sigma of 0.02 F29B-F28B 2.2 with sigma of 0.02 F28B-F30A 2.2 with sigma of 0.02 C59-F30B 1.31 with sigma of 0.02 C59-F28A 1.31 with sigma of 0.02 C59-F29A 1.31 with sigma of 0.02 F30B-F29A 2.2 with sigma of 0.02 F29A-F28A 2.2 with sigma of 0.02 F28A-F30B 2.2 with sigma of 0.02 C58-F27A 1.31 with sigma of 0.02 C58-F26B 1.31 with sigma of 0.02 C58-F25A 1.31 with sigma of 0.02 F25A-F26B 2.2 with sigma of 0.02 F26B-F27A 2.2 with sigma of 0.02 F27A-F25A 2.2 with sigma of 0.02 C63-F32B 1.32 with sigma of 0.02 C63-F33A 1.32 with sigma of 0.02 C63-F31B 1.32 with sigma of 0.02 F32B-F33A 2.13 with sigma of 0.02 F33A-F31B 2.13 with sigma of 0.02 F31B-F32B 2.13 with sigma of 0.02 C63-F32A 1.32 with sigma of 0.02 C63-F33B 1.32 with sigma of 0.02 C63-F31A 1.32 with sigma of 0.02 F32A-F33B 2.13 with sigma of 0.02 F33B-F31A 2.13 with sigma of 0.02 F31A-F32A 2.13 with sigma of 0.02 C58-F27B 1.31 with sigma of 0.02 C58-F26A 1.31 with sigma of 0.02 C58-F25B 1.31 with sigma of 0.02 F25B-F26A 2.2 with sigma of 0.02 F26A-F27B 2.2 with sigma of 0.02 F27B-F25B 2.2 with sigma of 0.02 3. Rigid bond restraints F31B, F32B, F33A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 F32A, F33B, F31A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints F32B \\sim F33A \\sim F31B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 F32A \\sim F33B \\sim F31A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(F28A) \\sim Ueq, Uanis(F28B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(F32B) \\sim Ueq, Uanis(F33A) \\sim Ueq, Uanis(F31B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(F32A) \\sim Ueq, Uanis(F33B) \\sim Ueq, Uanis(F31A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(F27B) \\sim Ueq, Uanis(F25B) \\sim Ueq, Uanis(F26A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(F27A) \\sim Ueq, Uanis(F26B) \\sim Ueq, Uanis(F25A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(F31B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(F30B) = Uanis(F29A) = Uanis(F28A) Uanis(F28B) = Uanis(F29B) = Uanis(F30A) 5. Others Sof(F28B)=Sof(F29B)=Sof(F30A)=1-FVAR(1) Sof(F28A)=Sof(F29A)=Sof(F30B)=FVAR(1) Sof(F25B)=Sof(F26A)=Sof(F27B)=1-FVAR(2) Sof(F25A)=Sof(F26B)=Sof(F27A)=FVAR(2) Sof(F31B)=Sof(F32B)=Sof(F33A)=1-FVAR(3) Sof(F31A)=Sof(F32A)=Sof(F33B)=FVAR(3) 6.a Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C19(H19), C24(H24), C29(H29), C35(H35), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C51(H51), C56(H56), C61(H61) 6.b Idealised Me refined as rotating group: C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,H17b, H17c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C49(H49a, H49b,H49c) ; _shelx_res_file ; TITL P120917F1 in P21/n #14 P21/c p120917f1.res created by SHELXL-2018/3 at 10:48:19 on 10-Jan-2019 CELL 0.71073 20.8845 17.2985 29.7057 90 129.695 90 ZERR 8 0.0009 0.0007 0.0011 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F N O S Tb UNIT 256 176 144 16 64 8 8 DFIX 1.31 C59 F30A DFIX 1.31 C59 F28B DFIX 1.31 C59 F29B DFIX 2.2 F30A F29B DFIX 2.2 F29B F28B DFIX 2.2 F28B F30A DFIX 1.31 C59 F30B DFIX 1.31 C59 F28A DFIX 1.31 C59 F29A DFIX 2.2 F30B F29A DFIX 2.2 F29A F28A DFIX 2.2 F28A F30B DFIX 1.31 C58 F27A DFIX 1.31 C58 F26B DFIX 1.31 C58 F25A DFIX 2.2 F25A F26B DFIX 2.2 F26B F27A DFIX 2.2 F27A F25A DFIX 1.32 C63 F32B DFIX 1.32 C63 F33A DFIX 1.32 C63 F31B DFIX 2.13 F32B F33A DFIX 2.13 F33A F31B DFIX 2.13 F31B F32B DFIX 1.32 C63 F32A DFIX 1.32 C63 F33B DFIX 1.32 C63 F31A DFIX 2.13 F32A F33B DFIX 2.13 F33B F31A DFIX 2.13 F31A F32A DFIX 1.31 C58 F27B DFIX 1.31 C58 F26A DFIX 1.31 C58 F25B DFIX 2.2 F25B F26A DFIX 2.2 F26A F27B DFIX 2.2 F27B F25B DELU F31B F32B F33A DELU F32A F33B F31A SIMU F32B F33A F31B SIMU F32A F33B F31A ISOR 0.002 0.004 C59 C58 ISOR 0.001 0.002 F28A F28B ISOR 0.005 0.01 F32B F33A F31B ISOR 0.005 0.01 F32A F33B F31A ISOR 0.005 0.01 F27B F25B F26A ISOR 0.005 0.01 F27A F26B F25A ISOR 0.002 0.004 F31B EADP F30B F29A F28A EADP F28B F29B F30A L.S. 10 PLAN 20 SIZE 0.15 0.15 0.2 TEMP -153(10) BOND $H htab conf ABIN fmap 2 acta OMIT -3 50.02 OMIT -1 0 22 OMIT -9 0 28 OMIT -13 7 19 OMIT -3 0 28 OMIT -4 1 2 OMIT -13 6 31 OMIT -14 6 32 OMIT -3 2 4 REM REM REM WGHT 0.010000 FVAR 0.60820 0.58272 0.49599 0.89198 C1 1 0.025920 0.571481 0.236960 11.00000 0.01124 0.01333 = 0.01669 -0.00359 0.00729 0.00173 C2 1 0.105049 0.570027 0.295238 11.00000 0.02225 0.00763 = 0.01959 -0.00087 0.01381 0.00250 C3 1 0.169307 0.621909 0.320360 11.00000 0.01959 0.01230 = 0.01938 0.00247 0.01222 0.00121 AFIX 43 H3 2 0.166679 0.667406 0.301325 11.00000 -1.20000 AFIX 0 C4 1 0.240305 0.600269 0.377976 11.00000 0.01597 0.01682 = 0.01743 -0.00096 0.00896 0.00063 C5 1 0.224931 0.533232 0.393880 11.00000 0.01811 0.02847 = 0.01727 0.00678 -0.00386 -0.00962 AFIX 43 H5 2 0.264389 0.510287 0.431311 11.00000 -1.20000 AFIX 0 C6 1 0.318998 0.643682 0.417168 11.00000 0.01874 0.02346 = 0.01212 0.00089 0.00775 -0.00138 C7 1 0.322410 0.723130 0.410982 11.00000 0.02221 0.02347 = 0.02597 -0.00295 0.01615 -0.00381 AFIX 43 H7 2 0.274424 0.749831 0.379085 11.00000 -1.20000 AFIX 0 C8 1 0.396170 0.763261 0.451576 11.00000 0.03064 0.02816 = 0.03706 -0.00711 0.02540 -0.01246 AFIX 43 H8 2 0.398205 0.817313 0.446942 11.00000 -1.20000 AFIX 0 C9 1 0.466225 0.725791 0.498347 11.00000 0.02288 0.05993 = 0.02274 -0.00758 0.01150 -0.02092 AFIX 43 H9 2 0.515762 0.754103 0.526318 11.00000 -1.20000 AFIX 0 C10 1 0.464261 0.647403 0.504429 11.00000 0.02252 0.05601 = 0.02154 0.00766 0.00773 -0.00725 AFIX 43 H10 2 0.512793 0.621098 0.536163 11.00000 -1.20000 AFIX 0 C11 1 0.391182 0.606651 0.464094 11.00000 0.02218 0.03081 = 0.02484 0.00376 0.00971 -0.00212 AFIX 43 H11 2 0.390350 0.552373 0.468569 11.00000 -1.20000 AFIX 0 C12 1 -0.080619 0.608271 0.138279 11.00000 0.02585 0.01826 = 0.00779 -0.00215 0.00506 -0.00387 C13 1 -0.109715 0.534984 0.152157 11.00000 0.02301 0.01414 = 0.01904 -0.00039 0.00713 0.00164 C14 1 -0.046035 0.590950 0.107866 11.00000 0.04280 0.03210 = 0.02236 -0.00454 0.01867 -0.00369 AFIX 137 H14A 2 -0.004253 0.549879 0.128967 11.00000 -1.50000 H14B 2 -0.020161 0.637635 0.107100 11.00000 -1.50000 H14C 2 -0.091152 0.574049 0.067712 11.00000 -1.50000 AFIX 0 C15 1 -0.144824 0.672709 0.107417 11.00000 0.02696 0.01846 = 0.02108 0.00610 -0.00073 -0.00149 AFIX 137 H15A 2 -0.195389 0.653614 0.069998 11.00000 -1.50000 H15B 2 -0.122259 0.716264 0.100344 11.00000 -1.50000 H15C 2 -0.158218 0.689790 0.132012 11.00000 -1.50000 AFIX 0 C16 1 -0.143235 0.469614 0.108038 11.00000 0.03202 0.02197 = 0.01610 -0.00514 0.00260 -0.00499 AFIX 137 H16A 2 -0.190478 0.488405 0.069062 11.00000 -1.50000 H16B 2 -0.161489 0.426945 0.119166 11.00000 -1.50000 H16C 2 -0.099332 0.451383 0.107464 11.00000 -1.50000 AFIX 0 C17 1 -0.169484 0.553603 0.163375 11.00000 0.01822 0.02883 = 0.04045 -0.00267 0.01247 -0.00587 AFIX 137 H17A 2 -0.147943 0.597372 0.190452 11.00000 -1.50000 H17B 2 -0.175070 0.508445 0.180557 11.00000 -1.50000 H17C 2 -0.224025 0.567011 0.126359 11.00000 -1.50000 AFIX 0 C18 1 -0.142361 0.348133 0.265535 11.00000 0.02374 0.01497 = 0.03420 -0.00125 0.01561 -0.00033 C19 1 -0.087199 0.364953 0.325505 11.00000 0.02771 0.02765 = 0.04234 -0.01027 0.02879 -0.00257 AFIX 43 H19 2 -0.108097 0.376671 0.345248 11.00000 -1.20000 AFIX 0 C20 1 -0.001437 0.364479 0.356249 11.00000 0.03917 0.01223 = 0.02929 -0.00028 0.02501 -0.00302 C21 1 -0.235891 0.346694 0.234955 11.00000 0.03513 0.04035 = 0.06919 -0.01110 0.03892 -0.00193 C22 1 0.056307 0.381775 0.422205 11.00000 0.04863 0.04725 = 0.02804 -0.00747 0.02683 -0.00054 C23 1 0.000478 0.171144 0.170168 11.00000 0.02606 0.01784 = 0.02776 -0.00059 0.01921 0.00065 C24 1 -0.070852 0.192796 0.115452 11.00000 0.02824 0.02598 = 0.02029 -0.00785 0.01329 0.00380 AFIX 43 H24 2 -0.083576 0.169374 0.081643 11.00000 -1.20000 AFIX 0 C25 1 -0.124346 0.248295 0.109023 11.00000 0.01579 0.02005 = 0.01391 -0.00196 0.00626 -0.00865 C26 1 0.055600 0.109084 0.172754 11.00000 0.03115 0.03012 = 0.02706 -0.00017 0.01593 0.01392 C27 1 -0.201449 0.265574 0.045243 11.00000 0.02721 0.02544 = 0.02598 -0.00494 0.01685 -0.00798 C28 1 0.194775 0.317519 0.303993 11.00000 0.01404 0.01698 = 0.03393 -0.00560 0.01199 -0.00233 C29 1 0.182206 0.335004 0.253308 11.00000 0.01822 0.02667 = 0.02626 -0.00121 0.01431 -0.00402 AFIX 43 H29 2 0.228631 0.336717 0.254380 11.00000 -1.20000 AFIX 0 C30 1 0.103109 0.350091 0.200928 11.00000 0.03057 0.00925 = 0.03061 -0.00027 0.02288 -0.00009 C31 1 0.282967 0.307509 0.361462 11.00000 0.02045 0.04255 = 0.03051 -0.00265 0.01436 -0.00035 C32 1 0.095436 0.365332 0.147162 11.00000 0.03348 0.03328 = 0.03205 0.00674 0.02499 0.00168 C33 1 0.532393 0.320404 0.259307 11.00000 0.01697 0.01189 = 0.01727 -0.00103 0.01079 -0.00171 C34 1 0.516945 0.323113 0.204893 11.00000 0.01489 0.01887 = 0.01298 -0.00148 0.00961 -0.00312 C35 1 0.478326 0.379520 0.162727 11.00000 0.01777 0.01270 = 0.02073 -0.00161 0.01231 0.00006 AFIX 43 H35 2 0.452774 0.423776 0.164195 11.00000 -1.20000 AFIX 0 C36 1 0.480432 0.365147 0.117165 11.00000 0.01514 0.01660 = 0.01799 -0.00450 0.01050 -0.00057 C37 1 0.521430 0.297618 0.126324 11.00000 0.02362 0.01509 = 0.01937 -0.00266 0.01434 -0.00368 AFIX 43 H37 2 0.528848 0.278457 0.099954 11.00000 -1.20000 AFIX 0 C38 1 0.443026 0.414802 0.064884 11.00000 0.01336 0.01858 = 0.01587 -0.00248 0.00773 -0.00353 C39 1 0.431519 0.493542 0.067140 11.00000 0.03871 0.02527 = 0.01311 0.00243 0.01420 -0.00064 AFIX 43 H39 2 0.443931 0.515358 0.101283 11.00000 -1.20000 AFIX 0 C40 1 0.401865 0.539967 0.019335 11.00000 0.03764 0.02377 = 0.02709 0.00387 0.01705 0.00412 AFIX 43 H40 2 0.394636 0.593785 0.021118 11.00000 -1.20000 AFIX 0 C41 1 0.382749 0.509078 -0.030709 11.00000 0.03319 0.03603 = 0.01836 0.00822 0.01311 -0.00209 AFIX 43 H41 2 0.362448 0.541422 -0.063221 11.00000 -1.20000 AFIX 0 C42 1 0.393202 0.431072 -0.033402 11.00000 0.02495 0.03843 = 0.01806 0.00440 0.01366 0.00532 AFIX 43 H42 2 0.380444 0.409498 -0.067719 11.00000 -1.20000 AFIX 0 C43 1 0.422335 0.384165 0.013996 11.00000 0.02811 0.02457 = 0.02622 -0.00238 0.01821 0.00067 AFIX 43 H43 2 0.428215 0.330213 0.011582 11.00000 -1.20000 AFIX 0 C44 1 0.598214 0.281671 0.356305 11.00000 0.02371 0.01475 = 0.00804 -0.00053 0.01050 -0.00348 C45 1 0.541243 0.352045 0.341177 11.00000 0.03081 0.01431 = 0.01288 -0.00027 0.01613 -0.00230 C46 1 0.688407 0.305020 0.386956 11.00000 0.02623 0.02647 = 0.01498 -0.00288 0.00975 -0.00786 AFIX 137 H46A 2 0.689069 0.346638 0.364873 11.00000 -1.50000 H46B 2 0.718944 0.260305 0.388945 11.00000 -1.50000 H46C 2 0.714873 0.323047 0.426646 11.00000 -1.50000 AFIX 0 C47 1 0.592445 0.215825 0.387371 11.00000 0.03340 0.01511 = 0.01656 0.00375 0.01269 0.00112 AFIX 137 H47A 2 0.603638 0.235526 0.422730 11.00000 -1.50000 H47B 2 0.633507 0.176042 0.398177 11.00000 -1.50000 H47C 2 0.536467 0.193409 0.361257 11.00000 -1.50000 AFIX 0 C48 1 0.580713 0.416323 0.385432 11.00000 0.05353 0.01969 = 0.02346 0.00179 0.02671 0.00287 AFIX 137 H48A 2 0.601412 0.395976 0.423407 11.00000 -1.50000 H48B 2 0.539322 0.456715 0.372656 11.00000 -1.50000 H48C 2 0.627135 0.438183 0.389082 11.00000 -1.50000 AFIX 0 C49 1 0.457273 0.328607 0.323421 11.00000 0.03298 0.02155 = 0.03189 0.00820 0.02222 0.00620 AFIX 137 H49A 2 0.434288 0.285258 0.295880 11.00000 -1.50000 H49B 2 0.418868 0.372544 0.304737 11.00000 -1.50000 H49C 2 0.464828 0.312992 0.358261 11.00000 -1.50000 AFIX 0 C50 1 0.674991 0.053364 0.267178 11.00000 0.02736 0.01386 = 0.03920 0.00582 0.02579 0.00078 C51 1 0.722303 0.037499 0.326671 11.00000 0.01752 0.02940 = 0.02663 0.00632 0.01283 0.00514 AFIX 43 H51 2 0.780642 0.030552 0.349641 11.00000 -1.20000 AFIX 0 C52 1 0.687400 0.031459 0.353652 11.00000 0.02602 0.01329 = 0.02238 0.00187 0.01159 0.00431 C53 1 0.716950 0.053898 0.240287 11.00000 0.04507 0.03817 = 0.05212 0.02252 0.03976 0.01561 C54 1 0.744975 0.009680 0.418616 11.00000 0.03097 0.02825 = 0.03684 0.00416 0.01349 0.01012 C55 1 0.294987 0.033240 0.172734 11.00000 0.02929 0.01331 = 0.01925 0.00112 0.01828 -0.00375 C56 1 0.296783 0.058734 0.217391 11.00000 0.02142 0.03115 = 0.02121 -0.00062 0.01510 -0.00100 AFIX 43 H56 2 0.245753 0.063494 0.210383 11.00000 -1.20000 AFIX 0 C57 1 0.370288 0.077778 0.272307 11.00000 0.03160 0.02363 = 0.02395 -0.00089 0.02264 0.00072 C58 1 0.209604 0.013761 0.113439 11.00000 0.03494 0.03693 = 0.03586 -0.00120 0.02278 -0.00121 C59 1 0.363820 0.098846 0.318700 11.00000 0.04760 0.05724 = 0.05244 -0.00396 0.03566 -0.00355 C60 1 0.374183 0.144124 0.098281 11.00000 0.02428 0.02046 = 0.01517 -0.00273 0.01023 -0.01061 C61 1 0.326995 0.197118 0.101114 11.00000 0.02151 0.02492 = 0.01962 0.00785 0.00867 0.00832 AFIX 43 H61 2 0.281665 0.222333 0.066412 11.00000 -1.20000 AFIX 0 C62 1 0.344730 0.213727 0.153251 11.00000 0.02481 0.01406 = 0.03503 -0.00264 0.02003 -0.00292 C63 1 0.353990 0.132101 0.038750 11.00000 0.03761 0.03588 = 0.02297 -0.00051 0.01840 0.00286 C64 1 0.290667 0.274613 0.153137 11.00000 0.03174 0.02474 = 0.02704 0.00425 0.02237 0.00535 F1 3 -0.254986 0.371798 0.266811 11.00000 0.04279 0.11704 = 0.09892 -0.05744 0.05504 -0.01774 F2 3 -0.263333 0.274660 0.218919 11.00000 0.04442 0.06074 = 0.09126 -0.03740 0.05049 -0.02605 F3 3 -0.279065 0.387399 0.185948 11.00000 0.03662 0.09320 = 0.09794 0.02217 0.03667 0.02317 F4 3 0.018506 0.411040 0.440522 11.00000 0.06933 0.12072 = 0.04232 -0.02316 0.03838 0.01169 F5 3 0.092186 0.317419 0.452322 11.00000 0.11647 0.06340 = 0.03020 0.01161 0.02716 0.02882 F6 3 0.115898 0.429593 0.438431 11.00000 0.08766 0.13069 = 0.03538 -0.04946 0.03899 -0.07478 F7 3 -0.249242 0.320689 0.040744 11.00000 0.02191 0.03177 = 0.02293 -0.00227 0.00307 0.00755 F8 3 -0.179280 0.286351 0.013683 11.00000 0.03434 0.04984 = 0.02663 0.00970 0.01629 -0.00584 F9 3 -0.249441 0.201711 0.019440 11.00000 0.02693 0.02748 = 0.01766 -0.00677 0.00816 -0.00717 F10 3 0.132504 0.132986 0.203244 11.00000 0.03221 0.05811 = 0.10602 -0.02354 0.04501 0.00016 F11 3 0.058510 0.046058 0.199515 11.00000 0.07793 0.02825 = 0.07235 0.01537 0.05679 0.02485 F12 3 0.029278 0.086246 0.121138 11.00000 0.06493 0.07413 = 0.03717 -0.00211 0.03076 0.03547 F13 3 0.300641 0.361534 0.399762 11.00000 0.03086 0.07368 = 0.03928 -0.01864 0.00172 0.00178 F14 3 0.341010 0.313026 0.355825 11.00000 0.01993 0.11481 = 0.04915 0.01426 0.02075 0.00289 F15 3 0.294003 0.240304 0.386151 11.00000 0.02499 0.05492 = 0.05370 0.02448 0.00991 0.01033 F16 3 0.165635 0.388216 0.158831 11.00000 0.05395 0.05202 = 0.05870 -0.00076 0.04694 -0.01058 F17 3 0.073286 0.300722 0.115869 11.00000 0.08575 0.06919 = 0.04337 -0.02407 0.04898 -0.03457 F18 3 0.038613 0.417534 0.112766 11.00000 0.09950 0.11376 = 0.08404 0.08026 0.08085 0.08245 F19 3 0.694361 0.113460 0.205701 11.00000 0.07969 0.05631 = 0.10028 0.03575 0.08172 0.02678 F20 3 0.799446 0.051130 0.278577 11.00000 0.03068 0.13707 = 0.07333 0.02014 0.03833 0.01255 F21 3 0.693461 -0.009082 0.206262 11.00000 0.10088 0.05390 = 0.10699 -0.00990 0.09282 0.00564 F22 3 0.746974 0.065291 0.449652 11.00000 0.08063 0.04180 = 0.02308 -0.00677 0.00918 0.01817 F23 3 0.822553 -0.005277 0.441337 11.00000 0.02937 0.13110 = 0.04336 0.03478 0.01369 0.03359 F24 3 0.718211 -0.052757 0.427994 11.00000 0.06505 0.04618 = 0.03067 0.01410 0.02352 0.00087 PART 1 F25A 3 0.173292 0.084862 0.085325 31.00000 0.03489 0.04758 = 0.03682 0.00784 0.00108 0.00085 PART 0 PART 2 F25B 3 0.150478 0.054206 0.100749 -31.00000 0.02878 0.08651 = 0.05843 -0.02677 0.00964 0.01975 F26A 3 0.212818 0.009509 0.070943 -31.00000 0.04513 0.06917 = 0.03011 -0.01046 0.02302 -0.02372 PART 0 PART 1 F26B 3 0.212410 -0.025337 0.078148 31.00000 0.03590 0.05192 = 0.04109 -0.02678 0.01124 0.00298 F27A 3 0.156711 -0.013741 0.118400 31.00000 0.03769 0.08334 = 0.03739 -0.00187 0.02012 -0.03405 PART 0 PART 2 F27B 3 0.192668 -0.063009 0.117940 -31.00000 0.04004 0.03973 = 0.05144 -0.00630 0.01364 -0.02265 F28A 3 0.424976 0.140695 0.361570 21.00000 0.04441 0.05576 = 0.03960 -0.00769 0.03104 -0.00288 PART 0 PART 1 F28B 3 0.430217 0.129595 0.366600 -21.00000 0.04628 0.04591 = 0.03828 -0.00739 0.03002 -0.00455 PART 0 PART 2 F29A 3 0.379389 0.025331 0.350242 21.00000 0.04441 0.05576 = 0.03960 -0.00769 0.03104 -0.00288 PART 0 PART 1 F29B 3 0.318874 0.058319 0.323173 -21.00000 0.04628 0.04591 = 0.03828 -0.00739 0.03002 -0.00455 F30A 3 0.309187 0.172769 0.293053 -21.00000 0.04628 0.04591 = 0.03828 -0.00739 0.03002 -0.00455 PART 0 PART 2 F30B 3 0.293922 0.117889 0.302655 21.00000 0.04441 0.05576 = 0.03960 -0.00769 0.03104 -0.00288 PART 0 PART 1 F31A 3 0.420133 0.139512 0.043402 41.00000 0.06520 0.13535 = 0.04550 -0.01747 0.04524 -0.02035 PART 0 PART 2 F31B 3 0.402034 0.078473 0.039949 -41.00000 0.03158 0.03213 = 0.02671 -0.00034 0.02011 0.00374 PART 0 PART 1 F32A 3 0.324859 0.062010 0.019488 41.00000 0.12725 0.05746 = 0.03266 -0.02152 0.04559 -0.02812 PART 0 PART 2 F32B 3 0.277053 0.109183 -0.004543 -41.00000 0.03130 0.04560 = 0.02482 -0.00801 0.02079 -0.00924 F33A 3 0.363297 0.195995 0.017938 -41.00000 0.05137 0.02584 = 0.02784 -0.00570 0.02089 -0.01078 PART 0 PART 1 F33B 3 0.296937 0.179714 -0.001999 41.00000 0.09589 0.09726 = 0.03881 0.03265 0.03941 0.05166 PART 0 F34 3 0.332562 0.339852 0.178512 11.00000 0.03932 0.02480 = 0.04549 -0.00449 0.02479 0.00826 F35 3 0.221770 0.293495 0.099643 11.00000 0.03158 0.04900 = 0.03366 0.00477 0.00930 0.02341 F36 3 0.267667 0.249600 0.183318 11.00000 0.05312 0.04033 = 0.06757 0.02252 0.05102 0.02238 TB1 7 -0.005331 0.309961 0.245941 11.00000 0.01282 0.01141 = 0.01722 -0.00022 0.00821 -0.00011 TB2 7 0.491461 0.079464 0.236143 11.00000 0.01762 0.01149 = 0.01731 0.00006 0.01194 0.00048 N1 4 -0.028769 0.512086 0.209884 11.00000 0.01388 0.01130 = 0.02185 -0.00001 0.00659 0.00075 N2 4 -0.008370 0.631805 0.199694 11.00000 0.01607 0.01174 = 0.01695 0.00295 0.00799 0.00208 N3 4 0.563565 0.259373 0.296020 11.00000 0.02276 0.01280 = 0.01776 -0.00117 0.01583 -0.00004 N4 4 0.522969 0.377995 0.285165 11.00000 0.02116 0.00992 = 0.01479 -0.00304 0.01008 -0.00272 O1 5 -0.019332 0.447652 0.235125 11.00000 0.02892 0.00840 = 0.02167 0.00020 0.01216 -0.00213 O2 5 0.023318 0.700492 0.212371 11.00000 0.01955 0.00990 = 0.02337 0.00158 0.01082 -0.00080 O3 5 -0.126437 0.331638 0.232894 11.00000 0.01509 0.01785 = 0.02580 -0.00151 0.01320 -0.00045 O4 5 0.035917 0.350089 0.337277 11.00000 0.01820 0.01639 = 0.02028 -0.00192 0.01150 -0.00201 O5 5 0.028255 0.195935 0.219354 11.00000 0.01792 0.01525 = 0.02089 0.00215 0.01229 0.00485 O6 5 -0.118426 0.285144 0.147335 11.00000 0.01484 0.01756 = 0.01329 -0.00150 0.00439 -0.00207 O7 5 0.139978 0.309314 0.309585 11.00000 0.01025 0.02644 = 0.02387 0.00201 0.00934 0.00361 O8 5 0.036109 0.351057 0.191688 11.00000 0.02013 0.02326 = 0.02342 0.00307 0.01431 0.00075 O9 5 0.578563 0.191955 0.285192 11.00000 0.01878 0.01087 = 0.02049 0.00117 0.01207 0.00170 O10 5 0.490410 0.444466 0.261547 11.00000 0.02653 0.00671 = 0.02363 0.00218 0.01544 0.00356 O11 5 0.598034 0.066001 0.231406 11.00000 0.02543 0.01746 = 0.02905 0.00233 0.02076 0.00550 O12 5 0.613450 0.041824 0.331787 11.00000 0.02107 0.01305 = 0.02314 0.00128 0.01313 0.00531 O13 5 0.443147 0.077692 0.289037 11.00000 0.02167 0.02492 = 0.02104 0.00082 0.01580 -0.00087 O14 5 0.356480 0.024065 0.174087 11.00000 0.01885 0.02244 = 0.02760 -0.00217 0.01549 -0.00063 O15 5 0.432966 0.103214 0.138438 11.00000 0.03023 0.01741 = 0.02150 0.00234 0.02059 0.00095 O16 5 0.401834 0.187231 0.203103 11.00000 0.01448 0.01773 = 0.01865 0.00319 0.00864 0.00384 S1 6 0.130184 0.494372 0.341704 11.00000 0.02870 0.02048 = 0.02504 0.00662 0.00380 -0.00912 S2 6 0.557831 0.251173 0.188993 11.00000 0.02531 0.01680 = 0.02390 0.00315 0.01851 0.00427 HKLF 4 1 1 0 0 0 -1 0 -1 0 -1 REM P120917F1 in P21/n #14 P21/c REM wR2 = 0.0796, GooF = S = 1.009, Restrained GooF = 1.034 for all data REM R1 = 0.0441 for 11283 Fo > 4sig(Fo) and 0.0630 for all 14526 data REM 1185 parameters refined using 132 restraints END WGHT 0.0101 0.0000 REM Instructions for potential hydrogen bonds HTAB C3 O2 EQIV $5 x, -y+1/2, z+1/2 HTAB C5 F32A_$5 HTAB C14 F18 EQIV $1 -x, y+1/2, -z+1/2 HTAB C15 O7_$1 HTAB C16 F7 HTAB C16 O6 HTAB C35 O10 EQIV $2 -x+1, y+1/2, -z+1/2 HTAB C35 O12_$2 EQIV $6 x+1, -y+1/2, z+1/2 HTAB C46 F9_$6 HTAB C47 F28A HTAB C47 F28B HTAB C47 O13 HTAB C48 O14_$2 HTAB C49 F14 HTAB C56 F10 REM Highest difference peak 1.405, deepest hole -1.065, 1-sigma level 0.135 Q1 1 0.2900 0.0802 0.3065 11.00000 0.05 1.40 Q2 1 0.3502 0.0390 0.3442 11.00000 0.05 1.10 Q3 1 0.2990 0.1503 0.3030 11.00000 0.05 0.97 Q4 1 -0.0378 0.2602 0.2163 11.00000 0.05 0.78 Q5 1 0.5190 0.0260 0.2624 11.00000 0.05 0.76 Q6 1 0.4110 0.0116 0.3564 11.00000 0.05 0.74 Q7 1 0.3304 0.1956 0.2922 11.00000 0.05 0.73 Q8 1 0.5286 0.1313 0.2671 11.00000 0.05 0.72 Q9 1 -0.0383 0.3524 0.2131 11.00000 0.05 0.71 Q10 1 -0.0292 0.2778 0.2605 11.00000 0.05 0.70 Q11 1 0.5700 0.2760 0.3200 11.00000 0.05 0.65 Q12 1 0.2370 0.3295 0.3314 11.00000 0.05 0.65 Q13 1 -0.1602 0.7569 0.0747 11.00000 0.05 0.61 Q14 1 0.4412 0.0483 0.2384 11.00000 0.05 0.61 Q15 1 0.4000 0.2227 0.3343 11.00000 0.05 0.61 Q16 1 0.2391 -0.0669 0.1178 11.00000 0.05 0.61 Q17 1 -0.3021 0.3157 0.1812 11.00000 0.05 0.59 Q18 1 0.5910 0.2959 0.2865 11.00000 0.05 0.58 Q19 1 0.3704 0.0533 0.0287 11.00000 0.05 0.57 Q20 1 0.0167 0.2667 0.2781 11.00000 0.05 0.57 ; _shelx_res_checksum 42718 _shelx_fab_file ; -24 0 16 0.3640 0.0717 -24 0 18 1.4521 0.0302 -24 0 20 -1.2837 0.0797 -24 0 22 1.9019 -0.0076 -24 0 24 0.0467 0.0094 -24 0 26 1.9490 0.0224 -24 0 28 2.3584 -0.0569 -24 1 15 3.0064 0.2892 -24 1 16 2.8493 0.1862 -24 1 17 0.1983 -0.0153 -24 1 18 3.7732 0.0763 -24 1 19 -1.2161 0.0369 -24 1 20 3.8932 0.1474 -24 1 21 -0.7530 -0.0586 -24 1 22 3.4766 0.0872 -24 1 23 -0.3187 0.0686 -24 1 24 4.5208 -0.0486 -24 1 25 1.1904 -0.1555 -24 1 26 0.2131 -0.0309 -24 1 27 -1.1343 0.0565 -24 1 28 -0.3781 -0.1111 -24 2 16 2.0508 -0.0373 -24 2 17 0.4581 0.0529 -24 2 18 1.0488 0.1195 -24 2 19 -2.2457 0.0918 -24 2 20 2.2658 -0.1374 -24 2 21 -0.8551 -0.0614 -24 2 22 0.0442 0.0520 -24 2 23 -1.1506 0.1443 -24 2 24 2.1562 -0.0937 -24 2 25 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-0.8469 -0.1158 13 5 1 4.0003 -0.1643 13 5 2 0.6227 -0.1455 13 5 3 4.4512 -0.0617 13 5 4 4.4313 -0.0835 13 5 5 1.1257 0.1495 13 5 6 1.3312 0.1346 13 5 7 -0.6199 0.1287 13 5 8 -0.9714 0.1820 13 5 9 2.1106 0.0605 13 5 10 -2.5004 0.1463 13 6 0 3.6161 -0.0946 13 6 1 1.2735 0.2587 13 6 2 0.4589 -0.0490 13 6 3 1.9933 0.2247 13 6 4 2.7439 -0.0885 13 6 5 3.4042 0.0824 13 6 6 6.1579 -0.0736 13 6 7 0.1664 0.0047 13 6 8 2.7946 0.2572 13 6 9 -0.8086 -0.2316 13 7 0 3.2783 -0.0235 13 7 1 2.1848 -0.1496 13 7 2 3.5605 -0.0587 13 7 3 3.1404 -0.0977 13 7 4 -2.3246 0.0550 13 7 5 3.1269 -0.0884 13 7 6 -2.2621 -0.1629 13 7 7 4.1404 0.0508 13 7 8 2.0056 -0.0959 13 7 9 1.5308 0.1732 13 8 0 -1.4141 0.0369 13 8 1 0.5823 -0.0936 13 8 2 0.3993 -0.0904 13 8 3 0.7402 -0.0882 13 8 4 0.2096 -0.1534 13 8 5 -1.4966 0.0384 13 8 6 -3.0559 -0.0612 13 8 7 -4.0717 0.0798 13 8 8 -0.9185 -0.3985 13 9 0 -1.2296 -0.1409 13 9 1 -2.4188 -0.0266 13 9 2 -1.6940 -0.0142 13 9 3 -7.1654 -0.1550 13 9 4 0.1148 -0.1255 13 9 5 -8.9456 -0.1932 13 9 6 -1.0542 0.0040 13 9 7 -9.5261 -0.2763 13 9 8 -2.3569 0.0241 13 10 0 -6.1561 -0.0108 13 10 1 1.5929 0.0659 13 10 2 -5.9716 0.1329 13 10 3 2.0677 -0.0269 13 10 4 -1.9318 0.1825 13 10 5 2.7340 0.0347 13 10 6 -0.4679 0.0065 13 10 7 2.8199 -0.1011 13 11 0 0.5201 0.0988 13 11 1 1.8379 0.0176 13 11 2 -1.7154 0.1147 13 11 3 1.5850 -0.2053 13 11 4 -1.5311 0.0296 13 11 5 0.7194 -0.2593 13 11 6 3.7321 -0.2477 13 12 0 -3.2704 -0.0097 13 12 1 -0.9975 0.0072 13 12 2 -0.5149 0.0707 13 12 3 1.8124 0.0572 13 12 4 -2.2128 0.1633 13 12 5 -0.9048 0.0177 13 13 0 0.1350 0.0179 13 13 1 -2.3710 -0.1114 13 13 2 -0.8344 -0.0830 13 13 3 0.2383 0.1358 13 14 0 0.4629 -0.0761 13 14 1 -1.6283 -0.0594 13 14 2 -3.7121 0.0176 13 15 0 2.4469 -0.0557 14 0 0 2.8846 -3.1565 14 0 2 2.1910 -2.1861 14 0 4 -1.1338 -0.9765 14 0 6 -0.8703 -0.1568 14 0 8 2.2912 0.1778 14 1 0 -0.7790 -0.0898 14 1 1 2.5827 0.2499 14 1 2 1.6719 -0.0362 14 1 3 1.3308 -0.1264 14 1 4 1.3075 0.0422 14 1 5 2.3909 -0.0749 14 1 6 -1.8172 0.2429 14 1 7 4.1597 0.2069 14 1 8 -1.2040 0.4228 14 1 9 3.0615 -0.1568 14 2 0 -0.3544 0.2623 14 2 1 2.9210 0.2897 14 2 2 -1.0958 0.1168 14 2 3 3.3687 0.5202 14 2 4 1.4760 -0.0380 14 2 5 0.2207 0.2634 14 2 6 0.2747 -0.2636 14 2 7 2.1096 0.2089 14 2 8 -1.3768 -0.0204 14 2 9 2.9369 0.1274 14 3 0 3.6301 0.1266 14 3 1 -5.2210 0.0489 14 3 2 0.1538 0.1277 14 3 3 -1.6442 0.0147 14 3 4 0.6777 0.3700 14 3 5 -1.4591 0.0455 14 3 6 0.8328 0.3369 14 3 7 -3.3287 -0.0425 14 3 8 -1.4374 0.1619 14 3 9 1.0809 0.0760 14 4 0 -3.7493 -0.0520 14 4 1 -8.0178 0.1355 14 4 2 -5.0039 0.0592 14 4 3 -7.4780 0.0835 14 4 4 -7.7223 0.1082 14 4 5 -0.1714 0.0908 14 4 6 -4.5214 0.0956 14 4 7 3.1520 0.2924 14 4 8 -3.7361 -0.0701 14 4 9 2.7952 0.2718 14 5 0 -1.1405 -0.0375 14 5 1 4.4584 -0.0877 14 5 2 3.2315 -0.0772 14 5 3 2.2163 0.1675 14 5 4 1.4580 0.0219 14 5 5 -1.2062 0.1342 14 5 6 -1.4324 0.2294 14 5 7 1.2009 0.1112 14 5 8 -2.4024 0.0406 14 6 0 -0.0729 -0.0076 14 6 1 1.2331 0.3202 14 6 2 0.1322 -0.0313 14 6 3 3.4131 0.2259 14 6 4 4.9769 -0.1257 14 6 5 2.7626 0.0962 14 6 6 3.7878 0.2503 14 6 7 0.7616 -0.2543 14 6 8 -0.8888 0.3049 14 7 0 4.9041 -0.0259 14 7 1 2.7186 -0.0713 14 7 2 0.7962 0.1067 14 7 3 2.3988 -0.0341 14 7 4 -1.5946 -0.0702 14 7 5 4.1579 0.1256 14 7 6 1.6263 -0.2675 14 7 7 2.4344 0.2119 14 8 0 -0.9979 -0.0589 14 8 1 1.6236 -0.1019 14 8 2 0.4843 -0.1444 14 8 3 0.8061 0.0578 14 8 4 -1.6690 -0.0391 14 8 5 -2.3159 0.1948 14 8 6 -2.2145 -0.2679 14 8 7 -5.5615 0.2616 14 9 0 -0.6986 -0.1019 14 9 1 -4.4367 -0.0911 14 9 2 0.3676 -0.1068 14 9 3 -7.9349 -0.1790 14 9 4 1.5550 0.0041 14 9 5 -9.3697 -0.1804 14 9 6 -0.0110 0.2082 14 10 0 -4.0833 0.0675 14 10 1 0.5847 0.0365 14 10 2 -1.7757 0.1936 14 10 3 1.0405 -0.0215 14 10 4 1.2172 0.0999 14 10 5 1.4908 0.0165 14 11 0 -0.7683 0.0668 14 11 1 2.5746 -0.1329 14 11 2 -1.9988 -0.0510 14 11 3 2.2488 -0.2514 14 11 4 1.7044 -0.2439 14 12 0 0.6579 0.0692 14 12 1 1.3272 0.0161 14 12 2 1.5301 0.1232 14 12 3 0.7781 -0.0196 14 13 0 -1.0980 -0.1512 14 13 1 0.6057 0.0591 14 14 0 -0.9858 0.0010 15 0 0 1.4370 -3.0109 15 0 2 -0.8408 -2.0821 15 0 4 -2.4114 -0.9641 15 0 6 0.2320 -0.1565 15 0 8 0.6818 0.1341 15 1 0 2.2374 -0.0919 15 1 1 1.1427 0.0907 15 1 2 3.3751 -0.1832 15 1 3 0.9406 -0.1316 15 1 4 1.1032 -0.0965 15 1 5 2.8746 0.2658 15 1 6 -0.2904 0.3137 15 1 7 1.9022 0.0074 15 1 8 2.1973 0.3256 15 2 0 -0.7669 0.2126 15 2 1 3.3081 0.4358 15 2 2 0.2078 0.1888 15 2 3 0.8164 0.4755 15 2 4 -0.1427 -0.2240 15 2 5 1.2456 0.3665 15 2 6 -1.9324 -0.1303 15 2 7 3.9550 0.3551 15 3 0 2.4659 0.0290 15 3 1 -2.4591 -0.0194 15 3 2 1.9736 0.2936 15 3 3 -0.3476 0.1467 15 3 4 3.0140 0.4312 15 3 5 -3.4059 0.1110 15 3 6 0.9294 0.1114 15 3 7 -0.5431 0.0818 15 4 0 -4.1599 -0.0451 15 4 1 -9.4267 0.0710 15 4 2 -7.8089 0.0037 15 4 3 -3.9643 -0.0700 15 4 4 -5.7585 0.2137 15 4 5 1.6736 0.2101 15 4 6 -4.4161 0.0413 15 4 7 1.2814 0.2977 15 5 0 0.0583 -0.0331 15 5 1 3.0985 0.1499 15 5 2 -0.1699 -0.0510 15 5 3 -0.9974 0.1753 15 5 4 -3.7565 0.1738 15 5 5 -0.4178 0.0577 15 5 6 -3.5457 0.1230 15 5 7 0.1547 0.3454 15 6 0 -1.5006 0.0685 15 6 1 0.8447 0.1818 15 6 2 2.9052 -0.0730 15 6 3 1.5817 0.2209 15 6 4 3.4284 0.1130 15 6 5 -0.1281 -0.1760 15 6 6 0.5111 0.4648 15 7 0 1.4984 0.0886 15 7 1 1.9276 -0.0063 15 7 2 -1.6526 0.0564 15 7 3 2.5293 0.1093 15 7 4 -1.1492 -0.2524 15 7 5 2.7428 0.2329 15 8 0 -1.5456 -0.0696 15 8 1 0.3543 0.0371 15 8 2 -1.6484 0.0446 15 8 3 -1.9038 0.2067 15 8 4 -2.5077 -0.1201 15 8 5 -5.2917 0.3949 15 9 0 -1.0626 -0.1987 15 9 1 -6.5283 -0.0956 15 9 2 -0.5438 -0.0225 15 9 3 -9.0655 -0.0217 15 9 4 0.4098 0.2318 15 10 0 -1.4861 0.1888 15 10 1 -2.2233 -0.0003 15 10 2 0.7220 0.2113 15 10 3 -2.9160 0.0197 15 11 0 -3.3217 -0.0567 15 11 1 1.5957 -0.0290 15 11 2 -1.4505 -0.2486 15 12 0 1.6932 0.1724 15 12 1 0.7194 -0.0497 16 0 0 -0.6072 -2.8610 16 0 2 -2.0465 -2.0253 16 0 4 -1.1064 -0.9154 16 0 6 0.8294 -0.2309 16 1 0 3.4062 -0.1928 16 1 1 0.5744 -0.0303 16 1 2 3.1879 -0.3925 16 1 3 2.1186 0.1582 16 1 4 1.3042 -0.0310 16 1 5 1.3830 0.1211 16 1 6 2.5947 0.1832 16 2 0 0.1076 0.2975 16 2 1 1.0506 0.4285 16 2 2 -0.5931 -0.0414 16 2 3 0.0933 0.3976 16 2 4 -1.9610 -0.2910 16 2 5 3.4375 0.4615 16 2 6 -2.1999 0.1968 16 3 0 3.8221 0.0339 16 3 1 2.0040 0.0949 16 3 2 4.8894 0.3614 16 3 3 -0.2276 0.2315 16 3 4 2.4998 0.0655 16 3 5 0.3097 0.0812 16 4 0 -4.2101 -0.1327 16 4 1 -6.7114 -0.1948 16 4 2 -3.1554 0.1005 16 4 3 -0.5367 -0.0327 16 4 4 -1.0303 0.1376 16 4 5 -0.1364 0.2086 16 5 0 -0.9484 -0.0931 16 5 1 0.7662 0.2180 16 5 2 -5.0249 -0.0026 16 5 3 -0.1864 -0.0394 16 5 4 -4.4363 0.1654 16 5 5 0.6518 0.2277 16 6 0 1.8605 -0.0017 16 6 1 0.2669 0.1141 16 6 2 3.2914 -0.0130 16 6 3 -0.7273 -0.0598 16 6 4 1.6503 0.3461 16 7 0 0.2855 0.0920 16 7 1 2.0311 -0.0249 16 7 2 -0.8280 -0.1557 16 7 3 1.9678 0.2188 16 7 4 -1.4853 -0.0537 16 8 0 -3.3471 0.0919 16 8 1 0.3113 0.1460 16 8 2 -1.9239 -0.0006 16 8 3 -3.0852 0.2726 16 9 0 -2.0643 -0.1391 16 9 1 -8.6918 0.0410 16 9 2 -1.1276 0.1655 16 10 0 0.1699 0.1513 16 10 1 -5.7971 -0.0862 16 11 0 -3.6747 -0.2365 17 0 0 -1.7366 -2.7679 17 0 2 -1.7626 -1.8682 17 0 4 1.2438 -0.8990 17 1 0 2.7995 -0.3640 17 1 1 1.0361 0.1929 17 1 2 2.3574 -0.2814 17 1 3 1.2359 0.1917 17 1 4 2.5657 -0.0196 17 2 0 -1.9634 0.1521 17 2 1 -1.3109 0.3378 17 2 2 -3.0405 -0.2365 17 2 3 2.0404 0.4200 17 2 4 -2.8314 0.0155 17 3 0 6.2032 0.2000 17 3 1 2.8585 0.2378 17 3 2 3.9657 0.0342 17 3 3 2.1444 0.1258 17 4 0 0.0335 -0.1059 17 4 1 -2.0443 -0.1837 17 4 2 3.8171 0.0848 17 4 3 -0.6824 0.0757 17 5 0 -4.0748 -0.0694 17 5 1 0.2776 -0.0910 17 5 2 -3.8404 0.1113 17 5 3 0.7614 -0.0037 17 6 0 2.9739 -0.0956 17 6 1 -0.0561 0.0175 17 6 2 1.4363 0.0564 17 7 0 3.8206 -0.0034 17 7 1 1.2879 0.0393 17 7 2 0.1941 -0.0196 17 8 0 -1.6865 0.0209 17 8 1 3.3056 0.1079 17 9 0 -2.0026 0.1524 18 0 0 -2.1824 -2.5698 18 0 2 0.3226 -1.7202 18 1 0 1.8502 -0.1809 18 1 1 0.4677 0.3235 18 1 2 1.5847 -0.0493 18 2 0 -5.5729 -0.1115 18 2 1 -0.7222 0.3748 18 2 2 -5.3248 0.1069 18 3 0 3.9899 0.0732 18 3 1 2.0971 0.1555 18 4 0 5.9858 -0.0669 18 4 1 -1.7771 0.1161 18 5 0 -4.2755 0.0899 18 5 1 -0.6973 -0.2117 18 6 0 -0.8600 -0.1512 19 0 0 0.1023 -2.4057 19 1 0 0.4061 0.2068 19 2 0 -6.5559 0.2672 0 0 0 0.0 0.0 ; _shelx_fab_checksum 38733 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0259(3) 0.5715(3) 0.23696(19) 0.0149(11) Uani 1 1 d . . . . . C2 C 0.1050(3) 0.5700(3) 0.2952(2) 0.0162(11) Uani 1 1 d . . . . . C3 C 0.1693(3) 0.6219(3) 0.32036(19) 0.0173(11) Uani 1 1 d . . . . . H3 H 0.166679 0.667406 0.301325 0.021 Uiso 1 1 calc R . . . . C4 C 0.2403(3) 0.6003(3) 0.3780(2) 0.0180(12) Uani 1 1 d . . . . . C5 C 0.2249(3) 0.5332(3) 0.3939(2) 0.0322(15) Uani 1 1 d . . . . . H5 H 0.264389 0.510287 0.431311 0.039 Uiso 1 1 calc R . . . . C6 C 0.3190(3) 0.6437(3) 0.4172(2) 0.0196(12) Uani 1 1 d . . . . . C7 C 0.3224(3) 0.7231(3) 0.4110(2) 0.0233(12) Uani 1 1 d . . . . . H7 H 0.274424 0.749831 0.379085 0.028 Uiso 1 1 calc R . . . . C8 C 0.3962(3) 0.7633(3) 0.4516(2) 0.0292(14) Uani 1 1 d . . . . . H8 H 0.398205 0.817313 0.446942 0.035 Uiso 1 1 calc R . . . . C9 C 0.4662(3) 0.7258(4) 0.4983(2) 0.0374(16) Uani 1 1 d . . . . . H9 H 0.515762 0.754103 0.526318 0.045 Uiso 1 1 calc R . . . . C10 C 0.4643(3) 0.6474(4) 0.5044(2) 0.0379(16) Uani 1 1 d . . . . . H10 H 0.512793 0.621098 0.536163 0.045 Uiso 1 1 calc R . . . . C11 C 0.3912(3) 0.6067(3) 0.4641(2) 0.0298(14) Uani 1 1 d . . . . . H11 H 0.390350 0.552373 0.468569 0.036 Uiso 1 1 calc R . . . . C12 C -0.0806(3) 0.6083(3) 0.13828(19) 0.0214(12) Uani 1 1 d . . . . . C13 C -0.1097(3) 0.5350(3) 0.1522(2) 0.0233(13) Uani 1 1 d . . . . . C14 C -0.0460(3) 0.5910(3) 0.1079(2) 0.0340(14) Uani 1 1 d . . . . . H14A H -0.004253 0.549879 0.128967 0.051 Uiso 1 1 calc GR . . . . H14B H -0.020161 0.637635 0.107100 0.051 Uiso 1 1 calc GR . . . . H14C H -0.091152 0.574049 0.067712 0.051 Uiso 1 1 calc GR . . . . C15 C -0.1448(3) 0.6727(3) 0.1074(2) 0.0337(15) Uani 1 1 d . . . . . H15A H -0.195389 0.653614 0.069998 0.051 Uiso 1 1 calc GR . . . . H15B H -0.122259 0.716264 0.100344 0.051 Uiso 1 1 calc GR . . . . H15C H -0.158218 0.689790 0.132012 0.051 Uiso 1 1 calc GR . . . . C16 C -0.1432(3) 0.4696(3) 0.1080(2) 0.0325(15) Uani 1 1 d . . . . . H16A H -0.190478 0.488405 0.069062 0.049 Uiso 1 1 calc GR . . . . H16B H -0.161489 0.426945 0.119166 0.049 Uiso 1 1 calc GR . . . . H16C H -0.099332 0.451383 0.107464 0.049 Uiso 1 1 calc GR . . . . C17 C -0.1695(3) 0.5536(3) 0.1634(2) 0.0337(15) Uani 1 1 d . . . . . H17A H -0.147943 0.597372 0.190452 0.051 Uiso 1 1 calc GR . . . . H17B H -0.175070 0.508445 0.180557 0.051 Uiso 1 1 calc GR . . . . H17C H -0.224025 0.567011 0.126359 0.051 Uiso 1 1 calc GR . . . . C18 C -0.1424(3) 0.3481(3) 0.2655(2) 0.0264(13) Uani 1 1 d . . . . . C19 C -0.0872(3) 0.3650(3) 0.3255(2) 0.0279(13) Uani 1 1 d . . . . . H19 H -0.108097 0.376671 0.345248 0.034 Uiso 1 1 calc R . . . . C20 C -0.0014(3) 0.3645(3) 0.3562(2) 0.0246(13) Uani 1 1 d . . . . . C21 C -0.2359(4) 0.3467(4) 0.2350(3) 0.0442(17) Uani 1 1 d . . . . . C22 C 0.0563(4) 0.3818(4) 0.4222(3) 0.0396(16) Uani 1 1 d . . . . . C23 C 0.0005(3) 0.1711(3) 0.1702(2) 0.0224(12) Uani 1 1 d . . . . . C24 C -0.0709(3) 0.1928(3) 0.1155(2) 0.0264(13) Uani 1 1 d . . . . . H24 H -0.083576 0.169374 0.081643 0.032 Uiso 1 1 calc R . . . . C25 C -0.1243(3) 0.2483(3) 0.1090(2) 0.0189(12) Uani 1 1 d . . . . . C26 C 0.0556(3) 0.1091(3) 0.1728(2) 0.0314(14) Uani 1 1 d . . . . . C27 C -0.2014(3) 0.2656(3) 0.0452(2) 0.0263(13) Uani 1 1 d . . . . . C28 C 0.1948(3) 0.3175(3) 0.3040(2) 0.0240(13) Uani 1 1 d . . . . . C29 C 0.1822(3) 0.3350(3) 0.2533(2) 0.0236(13) Uani 1 1 d . . . . . H29 H 0.228631 0.336717 0.254380 0.028 Uiso 1 1 calc R . . . . C30 C 0.1031(3) 0.3501(3) 0.2009(2) 0.0211(12) Uani 1 1 d . . . . . C31 C 0.2830(3) 0.3075(4) 0.3615(2) 0.0325(14) Uani 1 1 d . . . . . C32 C 0.0954(3) 0.3653(3) 0.1472(2) 0.0300(14) Uani 1 1 d . . . . . C33 C 0.5324(3) 0.3204(3) 0.2593(2) 0.0155(11) Uani 1 1 d . . . . . C34 C 0.5169(3) 0.3231(3) 0.2049(2) 0.0151(11) Uani 1 1 d . . . . . C35 C 0.4783(3) 0.3795(3) 0.16273(19) 0.0171(11) Uani 1 1 d . . . . . H35 H 0.452774 0.423776 0.164195 0.020 Uiso 1 1 calc R . . . . C36 C 0.4804(3) 0.3651(3) 0.1172(2) 0.0166(11) Uani 1 1 d . . . . . C37 C 0.5214(3) 0.2976(3) 0.1263(2) 0.0189(12) Uani 1 1 d . . . . . H37 H 0.528848 0.278457 0.099954 0.023 Uiso 1 1 calc R . . . . C38 C 0.4430(3) 0.4148(3) 0.0649(2) 0.0171(11) Uani 1 1 d . . . . . C39 C 0.4315(3) 0.4935(3) 0.0671(2) 0.0274(13) Uani 1 1 d . . . . . H39 H 0.443931 0.515358 0.101283 0.033 Uiso 1 1 calc R . . . . C40 C 0.4019(3) 0.5400(3) 0.0193(2) 0.0321(14) Uani 1 1 d . . . . . H40 H 0.394636 0.593785 0.021118 0.039 Uiso 1 1 calc R . . . . C41 C 0.3827(3) 0.5091(3) -0.0307(2) 0.0316(14) Uani 1 1 d . . . . . H41 H 0.362448 0.541422 -0.063221 0.038 Uiso 1 1 calc R . . . . C42 C 0.3932(3) 0.4311(3) -0.0334(2) 0.0272(13) Uani 1 1 d . . . . . H42 H 0.380444 0.409498 -0.067719 0.033 Uiso 1 1 calc R . . . . C43 C 0.4223(3) 0.3842(3) 0.0140(2) 0.0257(13) Uani 1 1 d . . . . . H43 H 0.428215 0.330213 0.011582 0.031 Uiso 1 1 calc R . . . . C44 C 0.5982(3) 0.2817(3) 0.35631(19) 0.0152(11) Uani 1 1 d . . . . . C45 C 0.5412(3) 0.3520(3) 0.3412(2) 0.0178(11) Uani 1 1 d . . . . . C46 C 0.6884(3) 0.3050(3) 0.3870(2) 0.0250(13) Uani 1 1 d . . . . . H46A H 0.689069 0.346638 0.364873 0.038 Uiso 1 1 calc GR . . . . H46B H 0.718944 0.260305 0.388945 0.038 Uiso 1 1 calc GR . . . . H46C H 0.714873 0.323047 0.426646 0.038 Uiso 1 1 calc GR . . . . C47 C 0.5924(3) 0.2158(3) 0.3874(2) 0.0240(13) Uani 1 1 d . . . . . H47A H 0.603638 0.235526 0.422730 0.036 Uiso 1 1 calc GR . . . . H47B H 0.633507 0.176042 0.398177 0.036 Uiso 1 1 calc GR . . . . H47C H 0.536467 0.193409 0.361257 0.036 Uiso 1 1 calc GR . . . . C48 C 0.5807(3) 0.4163(3) 0.3854(2) 0.0307(14) Uani 1 1 d . . . . . H48A H 0.601412 0.395976 0.423407 0.046 Uiso 1 1 calc GR . . . . H48B H 0.539322 0.456715 0.372656 0.046 Uiso 1 1 calc GR . . . . H48C H 0.627135 0.438183 0.389082 0.046 Uiso 1 1 calc GR . . . . C49 C 0.4573(3) 0.3286(3) 0.3234(2) 0.0277(13) Uani 1 1 d . . . . . H49A H 0.434288 0.285258 0.295880 0.042 Uiso 1 1 calc GR . . . . H49B H 0.418868 0.372544 0.304737 0.042 Uiso 1 1 calc GR . . . . H49C H 0.464828 0.312992 0.358261 0.042 Uiso 1 1 calc GR . . . . C50 C 0.6750(3) 0.0534(3) 0.2672(2) 0.0235(13) Uani 1 1 d . . . . . C51 C 0.7223(3) 0.0375(3) 0.3267(2) 0.0254(13) Uani 1 1 d . . . . . H51 H 0.780642 0.030552 0.349641 0.031 Uiso 1 1 calc R . . . . C52 C 0.6874(3) 0.0315(3) 0.3537(2) 0.0233(13) Uani 1 1 d . . . . . C53 C 0.7169(4) 0.0539(4) 0.2403(3) 0.0389(16) Uani 1 1 d . . . . . C54 C 0.7450(4) 0.0097(3) 0.4186(3) 0.0379(16) Uani 1 1 d . . . . . C55 C 0.2950(3) 0.0332(3) 0.1727(2) 0.0186(12) Uani 1 1 d . . . . . C56 C 0.2968(3) 0.0587(3) 0.2174(2) 0.0235(12) Uani 1 1 d . . . . . H56 H 0.245753 0.063494 0.210383 0.028 Uiso 1 1 calc R . . . . C57 C 0.3703(3) 0.0778(3) 0.2723(2) 0.0229(12) Uani 1 1 d . . . . . C58 C 0.2096(3) 0.0138(3) 0.1134(2) 0.0358(15) Uani 1 1 d D U . . . C59 C 0.3638(4) 0.0988(4) 0.3187(3) 0.0498(18) Uani 1 1 d D U . . . C60 C 0.3742(3) 0.1441(3) 0.0983(2) 0.0217(12) Uani 1 1 d . . . . . C61 C 0.3270(3) 0.1971(3) 0.1011(2) 0.0252(13) Uani 1 1 d . . . . . H61 H 0.281665 0.222333 0.066412 0.030 Uiso 1 1 calc R . . . . C62 C 0.3447(3) 0.2137(3) 0.1533(2) 0.0240(13) Uani 1 1 d . . . . . C63 C 0.3540(3) 0.1321(3) 0.0388(2) 0.0328(14) Uani 1 1 d D . . . . C64 C 0.2907(3) 0.2746(3) 0.1531(2) 0.0252(13) Uani 1 1 d . . . . . F1 F -0.2550(2) 0.3718(2) 0.26681(17) 0.0792(15) Uani 1 1 d . . . . . F2 F -0.26333(19) 0.2747(2) 0.21892(16) 0.0603(11) Uani 1 1 d . . . . . F3 F -0.2791(2) 0.3874(3) 0.18595(19) 0.0805(14) Uani 1 1 d . . . . . F4 F 0.0185(2) 0.4110(3) 0.44052(15) 0.0755(13) Uani 1 1 d . . . . . F5 F 0.0922(3) 0.3174(2) 0.45232(15) 0.0842(15) Uani 1 1 d . . . . . F6 F 0.1159(2) 0.4296(3) 0.43843(14) 0.0848(15) Uani 1 1 d . . . . . F7 F -0.24924(16) 0.32069(17) 0.04074(12) 0.0336(8) Uani 1 1 d . . . . . F8 F -0.17928(17) 0.28635(18) 0.01368(12) 0.0392(8) Uani 1 1 d . . . . . F9 F -0.24944(16) 0.20171(16) 0.01944(11) 0.0284(7) Uani 1 1 d . . . . . F10 F 0.1325(2) 0.1330(2) 0.20324(17) 0.0648(12) Uani 1 1 d . . . . . F11 F 0.0585(2) 0.04606(18) 0.19952(15) 0.0532(10) Uani 1 1 d . . . . . F12 F 0.0293(2) 0.0862(2) 0.12114(14) 0.0601(11) Uani 1 1 d . . . . . F13 F 0.30064(19) 0.3615(2) 0.39976(14) 0.0628(12) Uani 1 1 d . . . . . F14 F 0.34101(18) 0.3130(2) 0.35583(15) 0.0622(12) Uani 1 1 d . . . . . F15 F 0.29400(18) 0.2403(2) 0.38615(14) 0.0555(11) Uani 1 1 d . . . . . F16 F 0.16563(19) 0.38822(19) 0.15883(14) 0.0470(9) Uani 1 1 d . . . . . F17 F 0.0733(2) 0.3007(2) 0.11587(14) 0.0605(11) Uani 1 1 d . . . . . F18 F 0.0386(2) 0.4175(2) 0.11277(17) 0.0831(15) Uani 1 1 d . . . . . F19 F 0.6944(2) 0.1135(2) 0.20570(17) 0.0613(11) Uani 1 1 d . . . . . F20 F 0.7994(2) 0.0511(3) 0.27858(17) 0.0767(14) Uani 1 1 d . . . . . F21 F 0.6935(2) -0.0091(2) 0.20626(18) 0.0682(12) Uani 1 1 d . . . . . F22 F 0.7470(2) 0.0653(2) 0.44965(13) 0.0657(12) Uani 1 1 d . . . . . F23 F 0.8226(2) -0.0053(3) 0.44134(15) 0.0748(14) Uani 1 1 d . . . . . F24 F 0.7182(2) -0.0528(2) 0.42799(13) 0.0524(10) Uani 1 1 d . . . . . F25A F 0.1733(6) 0.0849(4) 0.0853(4) 0.055(3) Uani 0.496(13) 1 d D U P A 1 F25B F 0.1505(5) 0.0542(7) 0.1007(4) 0.071(4) Uani 0.504(13) 1 d D U P A 2 F26A F 0.2128(8) 0.0095(7) 0.0709(5) 0.049(3) Uani 0.504(13) 1 d D U P A 2 F26B F 0.2124(7) -0.0253(6) 0.0781(5) 0.053(4) Uani 0.496(13) 1 d D U P A 1 F27A F 0.1567(5) -0.0137(8) 0.1184(3) 0.056(4) Uani 0.496(13) 1 d D U P A 1 F27B F 0.1927(5) -0.0630(5) 0.1179(3) 0.055(3) Uani 0.504(13) 1 d D U P A 2 F28A F 0.4250(6) 0.1407(6) 0.3616(5) 0.0436(16) Uani 0.583(7) 1 d D U P B 2 F28B F 0.4302(8) 0.1296(7) 0.3666(6) 0.041(2) Uani 0.417(7) 1 d D U P B 1 F29A F 0.3794(3) 0.0253(3) 0.3502(2) 0.0436(16) Uani 0.583(7) 1 d D . P B 2 F29B F 0.3189(5) 0.0583(5) 0.3232(3) 0.041(2) Uani 0.417(7) 1 d D . P B 1 F30A F 0.3092(4) 0.1728(5) 0.2931(3) 0.041(2) Uani 0.417(7) 1 d D . P B 1 F30B F 0.2939(3) 0.1179(4) 0.3027(2) 0.0436(16) Uani 0.583(7) 1 d D . P B 2 F31A F 0.4201(3) 0.1395(4) 0.04340(18) 0.075(2) Uani 0.892(8) 1 d D U P C 1 F31B F 0.4020(16) 0.0785(14) 0.0399(12) 0.029(9) Uani 0.108(8) 1 d D U P C 2 F32A F 0.3249(4) 0.0620(3) 0.01949(18) 0.076(2) Uani 0.892(8) 1 d D U P C 1 F32B F 0.2771(11) 0.1092(18) -0.0045(11) 0.032(10) Uani 0.108(8) 1 d D U P C 2 F33A F 0.363(2) 0.1960(11) 0.0179(12) 0.038(10) Uani 0.108(8) 1 d D U P C 2 F33B F 0.2969(3) 0.1797(3) -0.00200(19) 0.080(2) Uani 0.892(8) 1 d D U P C 1 F34 F 0.33256(17) 0.33985(17) 0.17851(13) 0.0382(8) Uani 1 1 d . . . . . F35 F 0.22177(18) 0.29350(18) 0.09964(13) 0.0464(9) Uani 1 1 d . . . . . F36 F 0.26767(18) 0.24960(18) 0.18332(14) 0.0447(9) Uani 1 1 d . . . . . Tb1 Tb -0.00533(2) 0.30996(2) 0.24594(2) 0.01481(7) Uani 1 1 d . . . . . Tb2 Tb 0.49146(2) 0.07946(2) 0.23614(2) 0.01491(7) Uani 1 1 d . . . . . N1 N -0.0288(2) 0.5121(2) 0.20988(17) 0.0191(10) Uani 1 1 d . . . . . N2 N -0.0084(2) 0.6318(2) 0.19969(16) 0.0168(9) Uani 1 1 d . . . . . N3 N 0.5636(2) 0.2594(2) 0.29602(16) 0.0157(9) Uani 1 1 d . . . . . N4 N 0.5230(2) 0.3780(2) 0.28517(16) 0.0163(9) Uani 1 1 d . . . . . O1 O -0.01933(19) 0.44765(17) 0.23513(13) 0.0225(8) Uani 1 1 d . . . . . O2 O 0.02332(18) 0.70049(17) 0.21237(13) 0.0197(8) Uani 1 1 d . . . . . O3 O -0.12644(18) 0.33164(18) 0.23289(14) 0.0195(8) Uani 1 1 d . . . . . O4 O 0.03592(18) 0.35009(18) 0.33728(13) 0.0189(8) Uani 1 1 d . . . . . O5 O 0.02826(18) 0.19593(18) 0.21935(14) 0.0181(8) Uani 1 1 d . . . . . O6 O -0.11843(18) 0.28514(18) 0.14734(13) 0.0185(8) Uani 1 1 d . . . . . O7 O 0.13998(18) 0.30931(19) 0.30958(14) 0.0213(8) Uani 1 1 d . . . . . O8 O 0.03611(19) 0.35106(19) 0.19169(14) 0.0220(8) Uani 1 1 d . . . . . O9 O 0.57856(18) 0.19195(17) 0.28519(13) 0.0171(8) Uani 1 1 d . . . . . O10 O 0.49041(18) 0.44447(17) 0.26155(13) 0.0194(8) Uani 1 1 d . . . . . O11 O 0.5980(2) 0.06600(18) 0.23141(14) 0.0216(8) Uani 1 1 d . . . . . O12 O 0.61345(19) 0.04182(17) 0.33179(13) 0.0198(8) Uani 1 1 d . . . . . O13 O 0.44315(19) 0.07769(18) 0.28904(13) 0.0210(8) Uani 1 1 d . . . . . O14 O 0.35648(19) 0.02406(18) 0.17409(14) 0.0225(8) Uani 1 1 d . . . . . O15 O 0.43297(19) 0.10321(18) 0.13844(13) 0.0201(8) Uani 1 1 d . . . . . O16 O 0.40183(18) 0.18723(18) 0.20310(13) 0.0184(8) Uani 1 1 d . . . . . S1 S 0.13018(8) 0.49437(8) 0.34170(6) 0.0344(4) Uani 1 1 d . . . . . S2 S 0.55783(7) 0.25117(7) 0.18899(5) 0.0200(3) 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 0.011(3) 0.013(3) 0.017(3) -0.004(2) 0.007(2) 0.002(2) C2 0.022(3) 0.008(2) 0.020(3) -0.001(2) 0.014(2) 0.002(2) C3 0.020(3) 0.012(3) 0.019(3) 0.002(2) 0.012(2) 0.001(2) C4 0.016(3) 0.017(3) 0.017(3) -0.001(2) 0.009(2) 0.001(2) C5 0.018(3) 0.028(3) 0.017(3) 0.007(3) -0.004(3) -0.010(2) C6 0.019(3) 0.023(3) 0.012(3) 0.001(2) 0.008(2) -0.001(2) C7 0.022(3) 0.023(3) 0.026(3) -0.003(2) 0.016(3) -0.004(2) C8 0.031(3) 0.028(3) 0.037(3) -0.007(3) 0.025(3) -0.012(3) C9 0.023(3) 0.060(4) 0.023(3) -0.008(3) 0.012(3) -0.021(3) C10 0.023(3) 0.056(4) 0.022(3) 0.008(3) 0.008(3) -0.007(3) C11 0.022(3) 0.031(3) 0.025(3) 0.004(3) 0.010(3) -0.002(3) C12 0.026(3) 0.018(3) 0.008(3) -0.002(2) 0.005(2) -0.004(2) C13 0.023(3) 0.014(3) 0.019(3) 0.000(2) 0.007(3) 0.002(2) C14 0.043(4) 0.032(3) 0.022(3) -0.005(3) 0.019(3) -0.004(3) C15 0.027(3) 0.018(3) 0.021(3) 0.006(2) -0.001(3) -0.001(2) C16 0.032(3) 0.022(3) 0.016(3) -0.005(2) 0.003(3) -0.005(3) C17 0.018(3) 0.029(3) 0.040(4) -0.003(3) 0.012(3) -0.006(3) C18 0.024(3) 0.015(3) 0.034(3) -0.001(3) 0.016(3) 0.000(2) C19 0.028(3) 0.028(3) 0.042(4) -0.010(3) 0.029(3) -0.003(3) C20 0.039(4) 0.012(3) 0.029(3) 0.000(2) 0.025(3) -0.003(2) C21 0.035(4) 0.040(4) 0.069(5) -0.011(4) 0.039(4) -0.002(3) C22 0.049(4) 0.047(4) 0.028(4) -0.007(3) 0.027(3) -0.001(3) C23 0.026(3) 0.018(3) 0.028(3) -0.001(2) 0.019(3) 0.001(2) C24 0.028(3) 0.026(3) 0.020(3) -0.008(2) 0.013(3) 0.004(2) C25 0.016(3) 0.020(3) 0.014(3) -0.002(2) 0.006(2) -0.009(2) C26 0.031(4) 0.030(3) 0.027(3) 0.000(3) 0.016(3) 0.014(3) C27 0.027(3) 0.025(3) 0.026(3) -0.005(3) 0.017(3) -0.008(3) C28 0.014(3) 0.017(3) 0.034(3) -0.006(2) 0.012(3) -0.002(2) C29 0.018(3) 0.027(3) 0.026(3) -0.001(3) 0.014(3) -0.004(2) C30 0.031(3) 0.009(3) 0.031(3) 0.000(2) 0.023(3) 0.000(2) C31 0.020(3) 0.043(4) 0.031(3) -0.003(3) 0.014(3) 0.000(3) C32 0.033(4) 0.033(3) 0.032(3) 0.007(3) 0.025(3) 0.002(3) C33 0.017(3) 0.012(3) 0.017(3) -0.001(2) 0.011(2) -0.002(2) C34 0.015(3) 0.019(3) 0.013(3) -0.001(2) 0.010(2) -0.003(2) C35 0.018(3) 0.013(3) 0.021(3) -0.002(2) 0.012(2) 0.000(2) C36 0.015(3) 0.017(3) 0.018(3) -0.004(2) 0.010(2) -0.001(2) C37 0.024(3) 0.015(3) 0.019(3) -0.003(2) 0.014(2) -0.004(2) C38 0.013(3) 0.019(3) 0.016(3) -0.002(2) 0.008(2) -0.004(2) C39 0.039(3) 0.025(3) 0.013(3) 0.002(2) 0.014(3) -0.001(3) C40 0.038(4) 0.024(3) 0.027(3) 0.004(3) 0.017(3) 0.004(3) C41 0.033(3) 0.036(4) 0.018(3) 0.008(3) 0.013(3) -0.002(3) C42 0.025(3) 0.038(4) 0.018(3) 0.004(3) 0.014(3) 0.005(3) C43 0.028(3) 0.025(3) 0.026(3) -0.002(3) 0.018(3) 0.001(2) C44 0.024(3) 0.015(3) 0.008(2) -0.001(2) 0.010(2) -0.003(2) C45 0.031(3) 0.014(3) 0.013(3) 0.000(2) 0.016(2) -0.002(2) C46 0.026(3) 0.026(3) 0.015(3) -0.003(2) 0.010(3) -0.008(2) C47 0.033(3) 0.015(3) 0.017(3) 0.004(2) 0.013(3) 0.001(2) C48 0.054(4) 0.020(3) 0.023(3) 0.002(2) 0.027(3) 0.003(3) C49 0.033(3) 0.022(3) 0.032(3) 0.008(3) 0.022(3) 0.006(2) C50 0.027(3) 0.014(3) 0.039(3) 0.006(3) 0.026(3) 0.001(2) C51 0.018(3) 0.029(3) 0.027(3) 0.006(3) 0.013(3) 0.005(2) C52 0.026(3) 0.013(3) 0.022(3) 0.002(2) 0.012(3) 0.004(2) C53 0.045(4) 0.038(4) 0.052(4) 0.023(3) 0.040(4) 0.016(3) C54 0.031(4) 0.028(3) 0.037(4) 0.004(3) 0.013(3) 0.010(3) C55 0.029(3) 0.013(3) 0.019(3) 0.001(2) 0.018(3) -0.004(2) C56 0.021(3) 0.031(3) 0.021(3) -0.001(2) 0.015(3) -0.001(2) C57 0.032(3) 0.024(3) 0.024(3) -0.001(2) 0.023(3) 0.001(3) C58 0.035(2) 0.037(2) 0.036(2) -0.0012(17) 0.0228(17) -0.0012(17) C59 0.048(2) 0.057(3) 0.052(2) -0.0040(17) 0.0357(18) -0.0036(17) C60 0.024(3) 0.020(3) 0.015(3) -0.003(2) 0.010(3) -0.011(2) C61 0.022(3) 0.025(3) 0.020(3) 0.008(2) 0.009(3) 0.008(2) C62 0.025(3) 0.014(3) 0.035(3) -0.003(3) 0.020(3) -0.003(2) C63 0.038(4) 0.036(4) 0.023(3) -0.001(3) 0.018(3) 0.003(3) C64 0.032(3) 0.025(3) 0.027(3) 0.004(3) 0.022(3) 0.005(3) F1 0.043(2) 0.117(4) 0.099(3) -0.057(3) 0.055(2) -0.018(2) F2 0.044(2) 0.061(3) 0.091(3) -0.037(2) 0.050(2) -0.0260(19) F3 0.037(2) 0.093(3) 0.098(3) 0.022(3) 0.037(2) 0.023(2) F4 0.069(3) 0.121(4) 0.042(2) -0.023(2) 0.038(2) 0.012(3) F5 0.116(4) 0.063(3) 0.030(2) 0.012(2) 0.027(2) 0.029(3) F6 0.088(3) 0.131(4) 0.035(2) -0.049(3) 0.039(2) -0.075(3) F7 0.0219(18) 0.0318(18) 0.0229(17) -0.0023(14) 0.0031(15) 0.0075(14) F8 0.0343(19) 0.050(2) 0.0266(18) 0.0097(16) 0.0163(16) -0.0058(16) F9 0.0269(17) 0.0275(17) 0.0177(15) -0.0068(14) 0.0082(14) -0.0072(14) F10 0.032(2) 0.058(3) 0.106(3) -0.024(2) 0.045(2) 0.0002(19) F11 0.078(3) 0.028(2) 0.072(3) 0.0154(19) 0.057(2) 0.0249(18) F12 0.065(3) 0.074(3) 0.037(2) -0.002(2) 0.031(2) 0.035(2) F13 0.031(2) 0.074(3) 0.039(2) -0.019(2) 0.0017(18) 0.0018(19) F14 0.020(2) 0.115(4) 0.049(2) 0.014(2) 0.0208(18) 0.003(2) F15 0.025(2) 0.055(2) 0.054(2) 0.024(2) 0.0099(18) 0.0103(17) F16 0.054(2) 0.052(2) 0.059(2) -0.0008(19) 0.047(2) -0.0106(18) F17 0.086(3) 0.069(3) 0.043(2) -0.024(2) 0.049(2) -0.035(2) F18 0.099(3) 0.114(4) 0.084(3) 0.080(3) 0.081(3) 0.082(3) F19 0.080(3) 0.056(3) 0.100(3) 0.036(2) 0.082(3) 0.027(2) F20 0.031(2) 0.137(4) 0.073(3) 0.020(3) 0.038(2) 0.013(2) F21 0.101(3) 0.054(3) 0.107(3) -0.010(2) 0.093(3) 0.006(2) F22 0.081(3) 0.042(2) 0.0231(18) -0.0068(17) 0.009(2) 0.018(2) F23 0.029(2) 0.131(4) 0.043(2) 0.035(2) 0.0137(19) 0.034(2) F24 0.065(3) 0.046(2) 0.0307(19) 0.0141(18) 0.0235(19) 0.0009(19) F25A 0.035(5) 0.048(5) 0.037(5) 0.008(4) 0.001(3) 0.001(4) F25B 0.029(5) 0.087(7) 0.058(6) -0.027(5) 0.010(4) 0.020(5) F26A 0.045(5) 0.069(7) 0.030(4) -0.010(5) 0.023(4) -0.024(5) F26B 0.036(5) 0.052(6) 0.041(6) -0.027(5) 0.011(4) 0.003(5) F27A 0.038(5) 0.083(8) 0.037(4) -0.002(4) 0.020(4) -0.034(5) F27B 0.040(5) 0.040(5) 0.051(5) -0.006(4) 0.014(4) -0.023(4) F28A 0.044(2) 0.056(2) 0.040(2) -0.0077(14) 0.0310(16) -0.0029(13) F28B 0.046(3) 0.046(3) 0.038(3) -0.0074(16) 0.0300(19) -0.0046(16) F29A 0.044(2) 0.056(2) 0.040(2) -0.0077(14) 0.0310(16) -0.0029(13) F29B 0.046(3) 0.046(3) 0.038(3) -0.0074(16) 0.0300(19) -0.0046(16) F30A 0.046(3) 0.046(3) 0.038(3) -0.0074(16) 0.0300(19) -0.0046(16) F30B 0.044(2) 0.056(2) 0.040(2) -0.0077(14) 0.0310(16) -0.0029(13) F31A 0.065(3) 0.135(5) 0.045(3) -0.017(3) 0.045(3) -0.020(3) F31B 0.032(10) 0.032(10) 0.027(10) 0.000(4) 0.020(7) 0.004(4) F32A 0.127(5) 0.057(3) 0.033(3) -0.022(2) 0.046(3) -0.028(3) F32B 0.031(12) 0.046(14) 0.025(12) -0.008(8) 0.021(9) -0.009(8) F33A 0.051(14) 0.026(12) 0.028(12) -0.006(8) 0.021(9) -0.011(9) F33B 0.096(4) 0.097(4) 0.039(3) 0.033(3) 0.039(3) 0.052(3) F34 0.039(2) 0.0248(18) 0.045(2) -0.0045(16) 0.0248(17) 0.0083(15) F35 0.032(2) 0.049(2) 0.0337(19) 0.0048(17) 0.0093(17) 0.0234(16) F36 0.053(2) 0.040(2) 0.068(2) 0.0225(19) 0.051(2) 0.0224(17) Tb1 0.01282(14) 0.01141(12) 0.01722(13) -0.00022(10) 0.00821(11) -0.00011(10) Tb2 0.01762(14) 0.01149(12) 0.01731(13) 0.00006(10) 0.01194(12) 0.00048(10) N1 0.014(2) 0.011(2) 0.022(2) 0.0000(19) 0.007(2) 0.0007(18) N2 0.016(2) 0.012(2) 0.017(2) 0.0030(18) 0.0080(19) 0.0021(18) N3 0.023(2) 0.013(2) 0.018(2) -0.0012(18) 0.016(2) 0.0000(18) N4 0.021(2) 0.010(2) 0.015(2) -0.0030(18) 0.010(2) -0.0027(18) O1 0.029(2) 0.0084(17) 0.0217(19) 0.0002(15) 0.0122(17) -0.0021(15) O2 0.020(2) 0.0099(18) 0.0234(19) 0.0016(15) 0.0108(17) -0.0008(15) O3 0.0151(19) 0.0178(19) 0.026(2) -0.0015(16) 0.0132(17) -0.0005(14) O4 0.018(2) 0.0164(18) 0.0203(19) -0.0019(15) 0.0115(17) -0.0020(15) O5 0.0179(19) 0.0153(18) 0.0209(19) 0.0021(16) 0.0123(17) 0.0049(15) O6 0.0148(19) 0.0176(19) 0.0133(18) -0.0015(15) 0.0044(16) -0.0021(14) O7 0.0102(19) 0.026(2) 0.024(2) 0.0020(16) 0.0093(17) 0.0036(15) O8 0.020(2) 0.023(2) 0.023(2) 0.0031(16) 0.0143(18) 0.0008(16) O9 0.0188(19) 0.0109(17) 0.0205(18) 0.0012(15) 0.0121(16) 0.0017(14) O10 0.027(2) 0.0067(17) 0.0236(19) 0.0022(15) 0.0154(17) 0.0036(15) O11 0.025(2) 0.0175(19) 0.029(2) 0.0023(16) 0.0208(18) 0.0055(16) O12 0.021(2) 0.0130(18) 0.0231(19) 0.0013(15) 0.0131(17) 0.0053(15) O13 0.022(2) 0.025(2) 0.0210(19) 0.0008(16) 0.0158(17) -0.0009(16) O14 0.019(2) 0.022(2) 0.028(2) -0.0022(17) 0.0155(18) -0.0006(16) O15 0.030(2) 0.0174(19) 0.0215(19) 0.0023(16) 0.0206(18) 0.0009(16) O16 0.0145(19) 0.0177(18) 0.0186(19) 0.0032(16) 0.0086(16) 0.0038(15) S1 0.0287(9) 0.0205(7) 0.0250(8) 0.0066(6) 0.0038(7) -0.0091(6) S2 0.0253(8) 0.0168(7) 0.0239(7) 0.0031(6) 0.0185(6) 0.0043(6) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 C1 C2 125.9(4) . . N2 C1 C2 126.9(4) . . N2 C1 N1 107.2(4) . . C1 C2 S1 120.3(4) . . C3 C2 C1 127.9(4) . . C3 C2 S1 111.7(3) . . C2 C3 H3 123.6 . . C2 C3 C4 112.8(4) . . C4 C3 H3 123.6 . . C3 C4 C6 126.5(4) . . C5 C4 C3 110.2(4) . . C5 C4 C6 123.3(4) . . C4 C5 H5 122.7 . . C4 C5 S1 114.7(4) . . S1 C5 H5 122.7 . . C7 C6 C4 121.5(4) . . C11 C6 C4 120.2(4) . . C11 C6 C7 118.1(5) . . C6 C7 H7 120.0 . . C8 C7 C6 119.9(5) . . C8 C7 H7 120.0 . . C7 C8 H8 119.5 . . C9 C8 C7 121.0(5) . . C9 C8 H8 119.5 . . C8 C9 H9 120.1 . . C10 C9 C8 119.8(5) . . C10 C9 H9 120.1 . . C9 C10 H10 120.1 . . C9 C10 C11 119.8(5) . . C11 C10 H10 120.1 . . C6 C11 H11 119.3 . . C10 C11 C6 121.4(5) . . C10 C11 H11 119.3 . . C14 C12 C13 114.3(4) . . C14 C12 C15 111.2(4) . . C15 C12 C13 114.2(4) . . N2 C12 C13 99.0(4) . . N2 C12 C14 106.8(4) . . N2 C12 C15 110.4(4) . . C16 C13 C12 114.6(4) . . C17 C13 C12 113.4(4) . . C17 C13 C16 110.9(4) . . N1 C13 C12 99.8(4) . . N1 C13 C16 110.5(4) . . N1 C13 C17 106.8(4) . . C12 C14 H14A 109.5 . . C12 C14 H14B 109.5 . . C12 C14 H14C 109.5 . . H14A C14 H14B 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . C12 C15 H15A 109.5 . . C12 C15 H15B 109.5 . . C12 C15 H15C 109.5 . . H15A C15 H15B 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . C13 C16 H16A 109.5 . . C13 C16 H16B 109.5 . . C13 C16 H16C 109.5 . . H16A C16 H16B 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C13 C17 H17A 109.5 . . C13 C17 H17B 109.5 . . C13 C17 H17C 109.5 . . H17A C17 H17B 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . C19 C18 C21 117.1(5) . . O3 C18 C19 128.8(5) . . O3 C18 C21 114.0(5) . . C18 C19 H19 120.0 . . C20 C19 C18 120.0(5) . . C20 C19 H19 120.0 . . C19 C20 C22 117.8(5) . . O4 C20 C19 128.1(5) . . O4 C20 C22 114.0(5) . . F1 C21 C18 115.1(5) . . F1 C21 F2 108.0(5) . . F1 C21 F3 108.0(5) . . F2 C21 C18 108.7(5) . . F3 C21 C18 110.9(5) . . F3 C21 F2 105.7(5) . . F4 C22 C20 114.4(5) . . F4 C22 F5 106.0(5) . . F5 C22 C20 110.1(5) . . F6 C22 C20 112.4(5) . . F6 C22 F4 106.7(5) . . F6 C22 F5 106.8(5) . . C24 C23 C26 117.2(5) . . O5 C23 C24 128.8(5) . . O5 C23 C26 113.9(4) . . C23 C24 H24 119.4 . . C23 C24 C25 121.1(5) . . C25 C24 H24 119.4 . . C24 C25 C27 114.8(5) . . O6 C25 C24 128.9(4) . . O6 C25 C27 116.2(4) . . F10 C26 C23 111.2(5) . . F10 C26 F11 106.2(4) . . F10 C26 F12 108.4(5) . . F11 C26 C23 110.4(5) . . F12 C26 C23 114.1(4) . . F12 C26 F11 106.0(5) . . F7 C27 C25 113.1(4) . . F7 C27 F8 108.2(4) . . F7 C27 F9 107.0(4) . . F8 C27 C25 110.9(4) . . F8 C27 F9 106.6(4) . . F9 C27 C25 110.6(4) . . C29 C28 C31 119.8(5) . . O7 C28 C29 127.4(5) . . O7 C28 C31 112.8(5) . . C28 C29 H29 119.3 . . C28 C29 C30 121.4(5) . . C30 C29 H29 119.3 . . C29 C30 C32 117.4(4) . . O8 C30 C29 128.0(5) . . O8 C30 C32 114.6(4) . . F13 C31 C28 110.8(4) . . F14 C31 C28 113.5(5) . . F14 C31 F13 106.3(5) . . F15 C31 C28 112.4(5) . . F15 C31 F13 106.9(5) . . F15 C31 F14 106.6(5) . . F16 C32 C30 114.7(5) . . F16 C32 F17 105.3(4) . . F17 C32 C30 110.1(4) . . F18 C32 C30 111.9(4) . . F18 C32 F16 107.2(5) . . F18 C32 F17 107.2(5) . . N3 C33 C34 125.6(4) . . N4 C33 C34 127.6(4) . . N4 C33 N3 106.8(4) . . C33 C34 S2 119.2(4) . . C35 C34 C33 129.1(5) . . C35 C34 S2 111.5(4) . . C34 C35 H35 123.5 . . C34 C35 C36 113.1(4) . . C36 C35 H35 123.5 . . C35 C36 C38 125.8(4) . . C37 C36 C35 111.1(4) . . C37 C36 C38 123.0(4) . . C36 C37 H37 123.0 . . C36 C37 S2 114.0(4) . . S2 C37 H37 123.0 . . C39 C38 C36 120.4(4) . . C43 C38 C36 120.6(4) . . C43 C38 C39 118.9(5) . . C38 C39 H39 120.2 . . C40 C39 C38 119.7(5) . . C40 C39 H39 120.2 . . C39 C40 H40 119.6 . . C41 C40 C39 120.9(5) . . C41 C40 H40 119.6 . . C40 C41 H41 120.2 . . C40 C41 C42 119.7(5) . . C42 C41 H41 120.2 . . C41 C42 H42 120.1 . . C41 C42 C43 119.9(5) . . C43 C42 H42 120.1 . . C38 C43 H43 119.5 . . C42 C43 C38 120.9(5) . . C42 C43 H43 119.5 . . C46 C44 C45 112.9(4) . . C47 C44 C45 114.8(4) . . C47 C44 C46 112.4(4) . . N3 C44 C45 99.2(3) . . N3 C44 C46 104.5(4) . . N3 C44 C47 111.7(4) . . C48 C45 C44 115.8(4) . . C48 C45 C49 111.4(4) . . C48 C45 N4 110.7(4) . . C49 C45 C44 112.9(4) . . N4 C45 C44 99.1(4) . . N4 C45 C49 105.7(4) . . C44 C46 H46A 109.5 . . C44 C46 H46B 109.5 . . C44 C46 H46C 109.5 . . H46A C46 H46B 109.5 . . H46A C46 H46C 109.5 . . H46B C46 H46C 109.5 . . C44 C47 H47A 109.5 . . C44 C47 H47B 109.5 . . C44 C47 H47C 109.5 . . H47A C47 H47B 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . C45 C48 H48A 109.5 . . C45 C48 H48B 109.5 . . C45 C48 H48C 109.5 . . H48A C48 H48B 109.5 . . H48A C48 H48C 109.5 . . H48B C48 H48C 109.5 . . C45 C49 H49A 109.5 . . C45 C49 H49B 109.5 . . C45 C49 H49C 109.5 . . H49A C49 H49B 109.5 . . H49A C49 H49C 109.5 . . H49B C49 H49C 109.5 . . C51 C50 C53 119.3(5) . . O11 C50 C51 126.5(5) . . O11 C50 C53 114.3(5) . . C50 C51 H51 118.7 . . C52 C51 C50 122.5(5) . . C52 C51 H51 118.7 . . C51 C52 C54 117.8(5) . . O12 C52 C51 128.3(5) . . O12 C52 C54 113.9(5) . . F19 C53 C50 112.2(5) . . F19 C53 F20 108.7(5) . . F19 C53 F21 105.7(5) . . F20 C53 C50 114.8(5) . . F20 C53 F21 105.4(5) . . F21 C53 C50 109.5(5) . . F22 C54 C52 110.6(4) . . F22 C54 F23 107.8(5) . . F22 C54 F24 106.1(5) . . F23 C54 C52 114.3(5) . . F23 C54 F24 106.1(5) . . F24 C54 C52 111.6(5) . . C56 C55 C58 118.1(4) . . O14 C55 C56 127.3(5) . . O14 C55 C58 114.6(4) . . C55 C56 H56 118.7 . . C55 C56 C57 122.5(5) . . C57 C56 H56 118.7 . . C56 C57 C59 116.9(5) . . O13 C57 C56 127.7(5) . . O13 C57 C59 115.3(4) . . F25A C58 C55 106.2(5) . . F25B C58 C55 114.9(6) . . F25B C58 F26A 113.0(8) . . F25B C58 F27B 107.3(7) . . F26A C58 C55 112.3(7) . . F26A C58 F27B 102.1(7) . . F26B C58 C55 115.2(7) . . F26B C58 F25A 105.4(7) . . F26B C58 F27A 112.8(7) . . F27A C58 C55 113.5(6) . . F27A C58 F25A 102.3(7) . . F27B C58 C55 106.0(5) . . C57 C59 F30A 102.5(5) . . F28A C59 C57 115.0(8) . . F28A C59 F29A 100.1(7) . . F28B C59 C57 116.1(11) . . F28B C59 F30A 97.8(8) . . F29A C59 C57 104.9(5) . . F29B C59 C57 118.3(6) . . F29B C59 F28B 117.4(10) . . F29B C59 F30A 98.5(6) . . F30B C59 C57 118.4(6) . . F30B C59 F28A 113.6(8) . . F30B C59 F29A 101.3(6) . . C61 C60 C63 118.2(5) . . O15 C60 C61 128.3(5) . . O15 C60 C63 113.5(5) . . C60 C61 H61 119.5 . . C62 C61 C60 121.1(5) . . C62 C61 H61 119.5 . . C61 C62 C64 118.1(5) . . O16 C62 C61 128.6(5) . . O16 C62 C64 113.3(5) . . F31A C63 C60 111.6(5) . . F31A C63 F32A 107.6(5) . . F31A C63 F33B 108.2(5) . . F31B C63 C60 114.0(12) . . F32A C63 C60 109.5(5) . . F32B C63 C60 115.2(12) . . F32B C63 F31B 103.9(13) . . F32B C63 F33A 104.0(14) . . F33A C63 C60 113.7(13) . . F33A C63 F31B 104.7(14) . . F33B C63 C60 113.2(5) . . F33B C63 F32A 106.4(5) . . F34 C64 C62 111.3(4) . . F34 C64 F35 106.6(4) . . F34 C64 F36 106.5(4) . . F35 C64 C62 113.6(4) . . F36 C64 C62 110.8(4) . . F36 C64 F35 107.6(4) . . O1 Tb1 O2 143.22(11) . 2_545 O3 Tb1 O1 77.96(11) . . O3 Tb1 O2 72.81(11) . 2_545 O3 Tb1 O4 72.86(11) . . O3 Tb1 O5 126.43(11) . . O3 Tb1 O6 72.65(11) . . O3 Tb1 O7 147.79(11) . . O3 Tb1 O8 131.78(11) . . O4 Tb1 O1 77.65(11) . . O4 Tb1 O2 72.82(10) . 2_545 O4 Tb1 O5 130.70(11) . . O4 Tb1 O8 131.84(11) . . O5 Tb1 O1 144.32(11) . . O5 Tb1 O2 72.40(11) . 2_545 O6 Tb1 O1 94.31(10) . . O6 Tb1 O2 97.71(10) . 2_545 O6 Tb1 O4 145.49(11) . . O6 Tb1 O5 73.17(11) . . O6 Tb1 O8 73.74(11) . . O7 Tb1 O1 95.59(11) . . O7 Tb1 O2 97.36(11) . 2_545 O7 Tb1 O4 74.93(11) . . O7 Tb1 O5 76.10(11) . . O7 Tb1 O6 139.57(12) . . O7 Tb1 O8 72.68(11) . . O8 Tb1 O1 71.18(11) . . O8 Tb1 O2 145.59(11) . 2_545 O8 Tb1 O5 73.24(11) . . O10 Tb2 O9 137.29(10) 2_645 . O10 Tb2 O12 70.56(10) 2_645 . O10 Tb2 O14 73.24(11) 2_645 . O10 Tb2 O16 149.51(10) 2_645 . O11 Tb2 O9 74.72(11) . . O11 Tb2 O10 76.18(11) . 2_645 O11 Tb2 O12 73.21(11) . . O11 Tb2 O13 150.99(11) . . O11 Tb2 O14 128.30(11) . . O11 Tb2 O15 72.95(11) . . O11 Tb2 O16 125.95(11) . . O12 Tb2 O9 71.51(10) . . O13 Tb2 O9 94.98(11) . . O13 Tb2 O10 95.58(11) . 2_645 O13 Tb2 O12 77.81(11) . . O13 Tb2 O14 73.11(11) . . O13 Tb2 O15 136.06(11) . . O13 Tb2 O16 73.95(11) . . O14 Tb2 O9 149.07(10) . . O14 Tb2 O12 130.36(11) . . O15 Tb2 O9 101.58(11) . . O15 Tb2 O10 98.95(11) . 2_645 O15 Tb2 O12 146.08(11) . . O15 Tb2 O14 71.91(11) . . O15 Tb2 O16 72.62(11) . . O16 Tb2 O9 72.95(10) . . O16 Tb2 O12 131.80(11) . . O16 Tb2 O14 76.30(10) . . C1 N1 C13 112.7(4) . . O1 N1 C1 123.7(4) . . O1 N1 C13 122.4(4) . . C1 N2 C12 112.5(4) . . O2 N2 C1 124.6(4) . . O2 N2 C12 122.2(4) . . C33 N3 C44 112.4(4) . . O9 N3 C33 124.7(4) . . O9 N3 C44 121.4(4) . . C33 N4 C45 112.4(4) . . O10 N4 C33 124.5(4) . . O10 N4 C45 122.4(4) . . N1 O1 Tb1 154.1(3) . . N2 O2 Tb1 130.5(3) . 2 C18 O3 Tb1 135.2(3) . . C20 O4 Tb1 134.7(3) . . C23 O5 Tb1 130.7(3) . . C25 O6 Tb1 132.1(3) . . C28 O7 Tb1 135.2(3) . . C30 O8 Tb1 133.9(3) . . N3 O9 Tb2 131.6(2) . . N4 O10 Tb2 147.8(3) . 2_655 C50 O11 Tb2 136.2(3) . . C52 O12 Tb2 132.9(3) . . C57 O13 Tb2 131.4(3) . . C55 O14 Tb2 130.6(3) . . C60 O15 Tb2 134.0(3) . . C62 O16 Tb2 133.0(3) . . C5 S1 C2 90.7(2) . . C37 S2 C34 90.3(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C2 1.440(6) . C1 N1 1.354(5) . C1 N2 1.347(5) . C2 C3 1.373(6) . C2 S1 1.723(5) . C3 H3 0.9500 . C3 C4 1.423(6) . C4 C5 1.366(6) . C4 C6 1.475(6) . C5 H5 0.9500 . C5 S1 1.689(5) . C6 C7 1.394(6) . C6 C11 1.393(6) . C7 H7 0.9500 . C7 C8 1.391(6) . C8 H8 0.9500 . C8 C9 1.376(7) . C9 H9 0.9500 . C9 C10 1.372(8) . C10 H10 0.9500 . C10 C11 1.388(6) . C11 H11 0.9500 . C12 C13 1.570(7) . C12 C14 1.504(7) . C12 C15 1.520(6) . C12 N2 1.501(5) . C13 C16 1.521(6) . C13 C17 1.518(7) . C13 N1 1.501(6) . C14 H14A 0.9800 . C14 H14B 0.9800 . C14 H14C 0.9800 . C15 H15A 0.9800 . C15 H15B 0.9800 . C15 H15C 0.9800 . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . C17 H17A 0.9800 . C17 H17B 0.9800 . C17 H17C 0.9800 . C18 C19 1.401(7) . C18 C21 1.541(7) . C18 O3 1.243(6) . C19 H19 0.9500 . C19 C20 1.397(6) . C20 C22 1.538(7) . C20 O4 1.245(6) . C21 F1 1.313(7) . C21 F2 1.326(6) . C21 F3 1.323(7) . C22 F4 1.313(6) . C22 F5 1.321(7) . C22 F6 1.304(7) . C23 C24 1.381(6) . C23 C26 1.540(7) . C23 O5 1.254(6) . C24 H24 0.9500 . C24 C25 1.391(7) . C25 C27 1.541(6) . C25 O6 1.240(5) . C26 F10 1.309(6) . C26 F11 1.328(6) . C26 F12 1.316(6) . C27 F7 1.324(6) . C27 F8 1.333(6) . C27 F9 1.353(5) . C28 C29 1.387(7) . C28 C31 1.523(7) . C28 O7 1.265(6) . C29 H29 0.9500 . C29 C30 1.391(6) . C30 C32 1.523(7) . C30 O8 1.242(5) . C31 F13 1.330(6) . C31 F14 1.329(6) . C31 F15 1.314(6) . C32 F16 1.333(6) . C32 F17 1.333(6) . C32 F18 1.311(6) . C33 C34 1.433(6) . C33 N3 1.349(5) . C33 N4 1.347(6) . C34 C35 1.372(6) . C34 S2 1.737(5) . C35 H35 0.9500 . C35 C36 1.404(6) . C36 C37 1.369(6) . C36 C38 1.487(6) . C37 H37 0.9500 . C37 S2 1.697(5) . C38 C39 1.392(6) . C38 C43 1.385(6) . C39 H39 0.9500 . C39 C40 1.386(6) . C40 H40 0.9500 . C40 C41 1.377(7) . C41 H41 0.9500 . C41 C42 1.377(7) . C42 H42 0.9500 . C42 C43 1.384(6) . C43 H43 0.9500 . C44 C45 1.555(6) . C44 C46 1.533(6) . C44 C47 1.518(6) . C44 N3 1.491(5) . C45 C48 1.503(6) . C45 C49 1.529(6) . C45 N4 1.518(6) . C46 H46A 0.9800 . C46 H46B 0.9800 . C46 H46C 0.9800 . C47 H47A 0.9800 . C47 H47B 0.9800 . C47 H47C 0.9800 . C48 H48A 0.9800 . C48 H48B 0.9800 . C48 H48C 0.9800 . C49 H49A 0.9800 . C49 H49B 0.9800 . C49 H49C 0.9800 . C50 C51 1.394(7) . C50 C53 1.517(7) . C50 O11 1.256(5) . C51 H51 0.9500 . C51 C52 1.390(7) . C52 C54 1.532(7) . C52 O12 1.248(5) . C53 F19 1.312(6) . C53 F20 1.327(6) . C53 F21 1.348(7) . C54 F22 1.315(6) . C54 F23 1.323(6) . C54 F24 1.325(6) . C55 C56 1.376(6) . C55 C58 1.544(7) . C55 O14 1.269(5) . C56 H56 0.9500 . C56 C57 1.388(6) . C57 C59 1.513(7) . C57 O13 1.263(5) . C58 F25A 1.406(9) . C58 F25B 1.250(8) . C58 F26A 1.308(11) . C58 F26B 1.280(10) . C58 F27A 1.295(8) . C58 F27B 1.402(8) . C59 F28A 1.304(10) . C59 F28B 1.308(12) . C59 F29A 1.487(8) . C59 F29B 1.245(8) . C59 F30A 1.551(9) . C59 F30B 1.256(7) . C60 C61 1.387(7) . C60 C63 1.548(7) . C60 O15 1.249(5) . C61 H61 0.9500 . C61 C62 1.373(7) . C62 C64 1.542(7) . C62 O16 1.253(5) . C63 F31A 1.304(6) . C63 F31B 1.350(15) . C63 F32A 1.313(6) . C63 F32B 1.324(15) . C63 F33A 1.340(15) . C63 F33B 1.312(6) . C64 F34 1.328(6) . C64 F35 1.335(5) . C64 F36 1.331(6) . Tb1 O1 2.396(3) . Tb1 O2 2.420(3) 2_545 Tb1 O3 2.331(3) . Tb1 O4 2.366(3) . Tb1 O5 2.390(3) . Tb1 O6 2.346(3) . Tb1 O7 2.336(3) . Tb1 O8 2.373(3) . Tb2 O9 2.415(3) . Tb2 O10 2.360(3) 2_645 Tb2 O11 2.330(3) . Tb2 O12 2.396(3) . Tb2 O13 2.348(3) . Tb2 O14 2.372(3) . Tb2 O15 2.357(3) . Tb2 O16 2.365(3) . N1 O1 1.286(5) . N2 O2 1.294(4) . N3 O9 1.300(4) . N4 O10 1.291(4) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_4 C1 C2 C3 C4 -176.9(4) . C1 C2 S1 C5 178.0(4) . C1 N1 O1 Tb1 -121.8(6) . C1 N2 O2 Tb1 -89.2(5) 2 C2 C1 N1 C13 173.2(4) . C2 C1 N1 O1 5.7(7) . C2 C1 N2 C12 166.1(5) . C2 C1 N2 O2 -4.4(8) . C2 C3 C4 C5 -1.3(6) . C2 C3 C4 C6 -179.1(4) . C3 C2 S1 C5 0.6(4) . C3 C4 C5 S1 1.8(6) . C3 C4 C6 C7 23.8(8) . C3 C4 C6 C11 -160.5(5) . C4 C5 S1 C2 -1.4(5) . C4 C6 C7 C8 174.8(5) . C4 C6 C11 C10 -174.6(5) . C5 C4 C6 C7 -153.7(5) . C5 C4 C6 C11 22.0(8) . C6 C4 C5 S1 179.7(4) . C6 C7 C8 C9 -0.5(8) . C7 C6 C11 C10 1.3(8) . C7 C8 C9 C10 1.7(8) . C8 C9 C10 C11 -1.4(9) . C9 C10 C11 C6 -0.1(8) . C11 C6 C7 C8 -1.0(7) . C12 C13 N1 C1 21.9(5) . C12 C13 N1 O1 -170.4(4) . C12 N2 O2 Tb1 101.1(5) 2 C13 C12 N2 C1 27.5(5) . C13 C12 N2 O2 -161.7(4) . C13 N1 O1 Tb1 71.8(8) . C14 C12 C13 C16 -31.9(6) . C14 C12 C13 C17 -160.5(4) . C14 C12 C13 N1 86.2(5) . C14 C12 N2 C1 -91.4(5) . C14 C12 N2 O2 79.4(5) . C15 C12 C13 C16 97.7(5) . C15 C12 C13 C17 -30.9(6) . C15 C12 C13 N1 -144.2(4) . C15 C12 N2 C1 147.6(4) . C15 C12 N2 O2 -41.5(6) . C16 C13 N1 C1 143.0(4) . C16 C13 N1 O1 -49.3(6) . C17 C13 N1 C1 -96.3(5) . C17 C13 N1 O1 71.4(5) . C18 C19 C20 C22 -178.8(5) . C18 C19 C20 O4 -0.4(8) . C19 C18 C21 F1 8.9(8) . C19 C18 C21 F2 -112.4(6) . C19 C18 C21 F3 131.8(6) . C19 C18 O3 Tb1 4.6(9) . C19 C20 C22 F4 -13.6(8) . C19 C20 C22 F5 105.6(6) . C19 C20 C22 F6 -135.4(5) . C19 C20 O4 Tb1 -3.9(8) . C21 C18 C19 C20 177.7(5) . C21 C18 O3 Tb1 -173.1(3) . C22 C20 O4 Tb1 174.6(3) . C23 C24 C25 C27 -179.6(5) . C23 C24 C25 O6 0.2(9) . C24 C23 C26 F10 126.0(5) . C24 C23 C26 F11 -116.4(5) . C24 C23 C26 F12 3.0(8) . C24 C23 O5 Tb1 -16.2(8) . C24 C25 C27 F7 -177.6(4) . C24 C25 C27 F8 -55.8(6) . C24 C25 C27 F9 62.3(6) . C24 C25 O6 Tb1 18.7(8) . C26 C23 C24 C25 179.8(5) . C26 C23 O5 Tb1 162.9(3) . C27 C25 O6 Tb1 -161.5(3) . C28 C29 C30 C32 -177.5(5) . C28 C29 C30 O8 0.7(8) . C29 C28 C31 F13 116.0(6) . C29 C28 C31 F14 -3.4(7) . C29 C28 C31 F15 -124.4(5) . C29 C28 O7 Tb1 4.0(8) . C29 C30 C32 F16 -21.6(7) . C29 C30 C32 F17 96.9(5) . C29 C30 C32 F18 -144.0(5) . C29 C30 O8 Tb1 -12.2(8) . C31 C28 C29 C30 -175.3(5) . C31 C28 O7 Tb1 -177.0(3) . C32 C30 O8 Tb1 165.9(3) . C33 C34 C35 C36 175.1(4) . C33 C34 S2 C37 -175.7(4) . C33 N3 O9 Tb2 -87.7(5) . C33 N4 O10 Tb2 -115.6(5) 2_655 C34 C33 N3 C44 161.1(4) . C34 C33 N3 O9 -5.2(7) . C34 C33 N4 C45 177.0(4) . C34 C33 N4 O10 6.8(7) . C34 C35 C36 C37 -0.3(6) . C34 C35 C36 C38 179.1(4) . C35 C34 S2 C37 -0.6(4) . C35 C36 C37 S2 -0.2(5) . C35 C36 C38 C39 25.8(7) . C35 C36 C38 C43 -156.9(5) . C36 C37 S2 C34 0.5(4) . C36 C38 C39 C40 175.6(4) . C36 C38 C43 C42 -175.2(4) . C37 C36 C38 C39 -154.9(5) . C37 C36 C38 C43 22.4(7) . C38 C36 C37 S2 -179.6(3) . C38 C39 C40 C41 0.7(8) . C39 C38 C43 C42 2.1(7) . C39 C40 C41 C42 0.0(8) . C40 C41 C42 C43 0.4(8) . C41 C42 C43 C38 -1.4(8) . C43 C38 C39 C40 -1.7(7) . C44 C45 N4 C33 23.4(5) . C44 C45 N4 O10 -166.2(4) . C44 N3 O9 Tb2 107.1(4) . C45 C44 N3 C33 29.7(5) . C45 C44 N3 O9 -163.5(4) . C45 N4 O10 Tb2 75.1(6) 2_655 C46 C44 C45 C48 -36.9(6) . C46 C44 C45 C49 -167.1(4) . C46 C44 C45 N4 81.5(4) . C46 C44 N3 C33 -87.0(4) . C46 C44 N3 O9 79.8(5) . C47 C44 C45 C48 93.7(5) . C47 C44 C45 C49 -36.5(6) . C47 C44 C45 N4 -147.9(4) . C47 C44 N3 C33 151.2(4) . C47 C44 N3 O9 -42.0(6) . C48 C45 N4 C33 145.5(4) . C48 C45 N4 O10 -44.0(6) . C49 C45 N4 C33 -93.7(4) . C49 C45 N4 O10 76.8(5) . C50 C51 C52 C54 176.9(5) . C50 C51 C52 O12 -3.3(9) . C51 C50 C53 F19 -135.1(5) . C51 C50 C53 F20 -10.4(8) . C51 C50 C53 F21 107.8(6) . C51 C50 O11 Tb2 4.6(8) . C51 C52 C54 F22 118.3(6) . C51 C52 C54 F23 -3.5(7) . C51 C52 C54 F24 -123.8(5) . C51 C52 O12 Tb2 -1.7(8) . C53 C50 C51 C52 -176.1(5) . C53 C50 O11 Tb2 -177.2(3) . C54 C52 O12 Tb2 178.1(3) . C55 C56 C57 C59 -175.2(5) . C55 C56 C57 O13 2.6(9) . C56 C55 C58 F25A 78.7(8) . C56 C55 C58 F25B 32.7(11) . C56 C55 C58 F26A 163.7(8) . C56 C55 C58 F26B -165.1(8) . C56 C55 C58 F27A -32.9(10) . C56 C55 C58 F27B -85.6(8) . C56 C55 O14 Tb2 -22.0(7) . C56 C57 C59 F28A -157.5(7) . C56 C57 C59 F28B -168.3(8) . C56 C57 C59 F29A 93.6(6) . C56 C57 C59 F29B 43.9(9) . C56 C57 C59 F30A -63.1(7) . C56 C57 C59 F30B -18.5(9) . C56 C57 O13 Tb2 18.6(8) . C58 C55 C56 C57 -180.0(5) . C58 C55 O14 Tb2 157.3(3) . C59 C57 O13 Tb2 -163.5(4) . C60 C61 C62 C64 178.7(5) . C60 C61 C62 O16 0.8(9) . C61 C60 C63 F31A 127.6(6) . C61 C60 C63 F31B -178.8(15) . C61 C60 C63 F32A -113.4(6) . C61 C60 C63 F32B -58.8(17) . C61 C60 C63 F33A 61.2(17) . C61 C60 C63 F33B 5.2(8) . C61 C60 O15 Tb2 6.9(8) . C61 C62 C64 F34 -107.9(5) . C61 C62 C64 F35 12.5(7) . C61 C62 C64 F36 133.8(5) . C61 C62 O16 Tb2 -15.3(8) . C63 C60 C61 C62 -176.3(5) . C63 C60 O15 Tb2 -173.2(3) . C64 C62 O16 Tb2 166.7(3) . N1 C1 C2 C3 165.8(5) . N1 C1 C2 S1 -11.1(7) . N1 C1 N2 C12 -15.0(5) . N1 C1 N2 O2 174.4(4) . N2 C1 C2 C3 -15.5(8) . N2 C1 C2 S1 167.5(4) . N2 C1 N1 C13 -5.6(5) . N2 C1 N1 O1 -173.2(4) . N2 C12 C13 C16 -145.0(4) . N2 C12 C13 C17 86.4(5) . N2 C12 C13 N1 -26.9(4) . N3 C33 C34 C35 173.0(5) . N3 C33 C34 S2 -12.8(6) . N3 C33 N4 C45 -6.0(5) . N3 C33 N4 O10 -176.2(4) . N3 C44 C45 C48 -147.1(4) . N3 C44 C45 C49 82.7(4) . N3 C44 C45 N4 -28.7(4) . N4 C33 C34 C35 -10.5(8) . N4 C33 C34 S2 163.6(4) . N4 C33 N3 C44 -16.0(5) . N4 C33 N3 O9 177.7(4) . O3 C18 C19 C20 0.1(9) . O3 C18 C21 F1 -173.1(5) . O3 C18 C21 F2 65.6(7) . O3 C18 C21 F3 -50.1(7) . O4 C20 C22 F4 167.8(5) . O4 C20 C22 F5 -73.1(6) . O4 C20 C22 F6 45.9(7) . O5 C23 C24 C25 -1.2(9) . O5 C23 C26 F10 -53.1(6) . O5 C23 C26 F11 64.5(6) . O5 C23 C26 F12 -176.2(5) . O6 C25 C27 F7 2.6(6) . O6 C25 C27 F8 124.4(5) . O6 C25 C27 F9 -117.5(5) . O7 C28 C29 C30 3.6(8) . O7 C28 C31 F13 -63.0(6) . O7 C28 C31 F14 177.6(5) . O7 C28 C31 F15 56.5(6) . O8 C30 C32 F16 160.0(4) . O8 C30 C32 F17 -81.5(6) . O8 C30 C32 F18 37.6(7) . O11 C50 C51 C52 2.0(9) . O11 C50 C53 F19 46.6(7) . O11 C50 C53 F20 171.3(5) . O11 C50 C53 F21 -70.5(6) . O12 C52 C54 F22 -61.5(6) . O12 C52 C54 F23 176.7(4) . O12 C52 C54 F24 56.4(6) . O13 C57 C59 F28A 24.4(8) . O13 C57 C59 F28B 13.5(10) . O13 C57 C59 F29A -84.6(6) . O13 C57 C59 F29B -134.3(7) . O13 C57 C59 F30A 118.8(5) . O13 C57 C59 F30B 163.4(6) . O14 C55 C56 C57 -0.6(8) . O14 C55 C58 F25A -100.8(7) . O14 C55 C58 F25B -146.7(10) . O14 C55 C58 F26A -15.8(9) . O14 C55 C58 F26B 15.4(10) . O14 C55 C58 F27A 147.6(8) . O14 C55 C58 F27B 94.9(7) . O15 C60 C61 C62 3.6(9) . O15 C60 C63 F31A -52.3(7) . O15 C60 C63 F31B 1.3(16) . O15 C60 C63 F32A 66.7(6) . O15 C60 C63 F32B 121.3(16) . O15 C60 C63 F33A -118.7(17) . O15 C60 C63 F33B -174.7(5) . O16 C62 C64 F34 70.3(6) . O16 C62 C64 F35 -169.3(4) . O16 C62 C64 F36 -48.0(6) . S1 C2 C3 C4 0.3(5) . S2 C34 C35 C36 0.6(5) . loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons 1 0.000 -0.818 0.000 379.1 36.8 2 0.000 -0.990 0.500 379.1 36.8 3 0.450 0.002 0.908 13.6 0.0 4 0.450 0.498 0.408 13.6 0.0 5 0.550 -0.002 0.092 13.6 0.0 6 0.550 0.502 0.592 13.6 0.0