#------------------------------------------------------------------------------ #$Date: 2021-05-07 05:26:07 +0300 (Fri, 07 May 2021) $ #$Revision: 265025 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/73/7707358.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_7707358 loop_ _publ_author_name 'Wang, Kuiyuan' 'Prior, Timothy J.' 'Hughes, David L.' 'Arbaoui, Abdessamad' 'Redshaw, Carl' _publ_section_title ; Coordination chemistry of [2+2] Schiff-base macrocycles derived from the dianilines [(2-NH2C6H4)2X] (X = CH2CH2, O): Structural studies and ROP capability towards cyclic esters. ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00711D _journal_year 2021 _chemical_formula_moiety '2(C52 H52 Br Fe N4 O2), C2 H3 N, Br6 Fe2 O' _chemical_formula_sum 'C106 H107 Br8 Fe4 N9 O5' _chemical_formula_weight 2449.68 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-04-28 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257) ; _audit_update_record ; 2021-04-29 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _cell_angle_alpha 67.263(5) _cell_angle_beta 88.642(4) _cell_angle_gamma 81.638(4) _cell_formula_units_Z 1 _cell_length_a 13.6454(5) _cell_length_b 13.9070(7) _cell_length_c 15.6432(8) _cell_measurement_reflns_used 20939 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 2.114 _cell_measurement_theta_min 27.504 _cell_volume 2707.0(2) _computing_cell_refinement 'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)' _computing_data_collection 'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)' _computing_data_reduction 'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 28.5714 _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'four-circle \k goniometer' _diffrn_measurement_device_type 'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen MicroLoop' _diffrn_radiation_collimation 0.2 _diffrn_radiation_monochromator 'Confocal mirrors, VHF Varimax' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_unetI/netI 0.0583 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 12337 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_min 3.156 _diffrn_source 'Rotating Anode' _diffrn_source_current 55.0 _diffrn_source_power 2.475 _diffrn_source_target Mo _diffrn_source_type 'Rigaku FRE+' _diffrn_source_voltage 45.0 _exptl_absorpt_coefficient_mu 3.531 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.5920 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.503 _exptl_crystal_description needle _exptl_crystal_F_000 1230 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.01 _refine_diff_density_max 1.531 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.131 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 604 _refine_ls_number_reflns 12337 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0605 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+8.1221P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1483 _refine_ls_wR_factor_ref 0.1638 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8627 _reflns_number_total 12337 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00711d2.cif _cod_data_source_block FeROP2 _cod_database_code 7707358 _shelx_shelxl_version_number 2018/3 _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 0.966 _shelx_estimated_absorpt_t_min 0.417 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.840(5) 0.160(5) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances Fe2-Br2A \\sim Fe2-Br2B \\sim Fe2-Br4A \\sim Fe2-Br4B with sigma of 0.02 4. Uiso/Uaniso restraints and constraints Uanis(Br2A) = Uanis(Br2B) Uanis(Br4A) = Uanis(Br4B) 5. Others Sof(Br2B)=Sof(Br4B)=1-FVAR(1) Sof(Br2A)=Sof(Br4A)=FVAR(1) Fixed Sof: N5(0.5) C61(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) 6.a Secondary CH2 refined with riding coordinates: C18(H18A,H18B), C19(H19A,H19B), C44(H44A,H44B), C45(H45A,H45B) 6.b Me refined with riding coordinates: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C) 6.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C29(H29), C31(H31), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), N2(H2), N4(H4) 6.d Idealised Me refined as rotating group: C62(H62A,H62B,H62C) ; _shelx_res_file ; TITL shelxt_a.res in P-1 2016ncs0208.res created by SHELXL-2018/3 at 21:27:57 on 28-Apr-2021 CELL 0.71073 13.6454 13.907 15.6432 67.263 88.642 81.638 ZERR 1 0.0005 0.0007 0.0008 0.005 0.004 0.004 LATT 1 SFAC C H Br Fe N O UNIT 106 107 8 4 9 5 EADP Br2A Br2B EADP Br4A Br4B SADI Fe2 Br2A Fe2 Br2B Fe2 Br4A Fe2 Br4B L.S. 4 PLAN 17 SIZE 0.01 0.015 0.3 TEMP -173(2) CONF MORE -1 BOND $H LIST 4 fmap 2 acta MERG 0 SHEL 6.5 0.65 OMIT -8 5 2 OMIT 2 -5 1 OMIT 5 5 5 OMIT 4 -1 4 REM REM REM WGHT 0.069700 8.122101 BASF 0.16001 FVAR 1.08677 0.80863 C1 1 0.644125 0.109448 0.467987 11.00000 0.01945 0.01367 = 0.02011 -0.00792 -0.00012 -0.00087 C2 1 0.745577 0.113139 0.448437 11.00000 0.01966 0.02236 = 0.01954 -0.00806 -0.00088 -0.00160 C3 1 0.818411 0.054355 0.518311 11.00000 0.01946 0.02660 = 0.02579 -0.00987 0.00171 -0.00383 AFIX 43 H3 2 0.885982 0.057263 0.502927 11.00000 -1.20000 AFIX 0 C4 1 0.797272 -0.008367 0.609432 11.00000 0.02473 0.02462 = 0.01959 -0.00654 -0.00070 -0.00234 C5 1 0.697206 -0.008479 0.628804 11.00000 0.02277 0.01832 = 0.02191 -0.00504 0.00044 -0.00560 AFIX 43 H5 2 0.679671 -0.048152 0.690223 11.00000 -1.20000 AFIX 0 C6 1 0.621044 0.047258 0.561865 11.00000 0.02183 0.01553 = 0.02123 -0.00839 0.00140 -0.00431 C7 1 0.879391 -0.072053 0.682832 11.00000 0.02534 0.03455 = 0.02536 -0.00078 -0.00365 -0.00865 C8 1 0.965669 -0.012859 0.675236 11.00000 0.03326 0.05799 = 0.04660 0.00270 -0.01323 -0.01294 AFIX 33 H8A 2 0.988324 0.011372 0.611454 11.00000 -1.50000 H8B 2 0.944767 0.048060 0.691704 11.00000 -1.50000 H8C 2 1.019942 -0.059568 0.717616 11.00000 -1.50000 AFIX 0 C9 1 0.921366 -0.170519 0.661141 11.00000 0.05436 0.04268 = 0.07810 -0.01968 -0.03229 0.00971 AFIX 33 H9A 2 0.945935 -0.147371 0.598042 11.00000 -1.50000 H9B 2 0.975803 -0.212725 0.705487 11.00000 -1.50000 H9C 2 0.868694 -0.213232 0.666285 11.00000 -1.50000 AFIX 0 C10 1 0.842557 -0.110496 0.779763 11.00000 0.03869 0.16458 = 0.02760 0.01682 -0.00758 -0.01927 AFIX 33 H10A 2 0.786666 -0.148591 0.782898 11.00000 -1.50000 H10B 2 0.896066 -0.157812 0.822794 11.00000 -1.50000 H10C 2 0.820891 -0.050184 0.796883 11.00000 -1.50000 AFIX 0 C11 1 0.521812 0.050129 0.591647 11.00000 0.02069 0.01604 = 0.01634 -0.00388 -0.00049 -0.00196 AFIX 43 H11 2 0.510670 0.009682 0.654750 11.00000 -1.20000 AFIX 0 C12 1 0.346101 0.124555 0.563939 11.00000 0.02157 0.02051 = 0.02571 -0.01205 -0.00001 -0.00484 C13 1 0.313125 0.058386 0.648831 11.00000 0.02118 0.01844 = 0.02654 -0.00613 0.00437 -0.00209 AFIX 43 H13 2 0.356061 -0.001502 0.688975 11.00000 -1.20000 AFIX 0 C14 1 0.216825 0.081447 0.673588 11.00000 0.02680 0.02309 = 0.03029 -0.00737 0.00936 -0.00719 AFIX 43 H14 2 0.193207 0.036389 0.730474 11.00000 -1.20000 AFIX 0 C15 1 0.155458 0.169448 0.615911 11.00000 0.02045 0.02901 = 0.03596 -0.00968 0.00596 -0.00223 AFIX 43 H15 2 0.090204 0.186004 0.633796 11.00000 -1.20000 AFIX 0 C16 1 0.188888 0.233891 0.531745 11.00000 0.01817 0.02632 = 0.03487 -0.01034 -0.00250 -0.00271 AFIX 43 H16 2 0.145294 0.293389 0.491927 11.00000 -1.20000 AFIX 0 C17 1 0.284729 0.213525 0.504198 11.00000 0.02168 0.02225 = 0.02169 -0.01063 0.00127 -0.00370 C18 1 0.318464 0.291850 0.414456 11.00000 0.01792 0.02755 = 0.02042 -0.00729 -0.00111 0.00162 AFIX 23 H18A 2 0.261798 0.321489 0.369006 11.00000 -1.20000 H18B 2 0.370496 0.254513 0.388530 11.00000 -1.20000 AFIX 0 C19 1 0.359771 0.383232 0.428143 11.00000 0.02267 0.01789 = 0.02716 -0.00188 0.00453 -0.00167 AFIX 23 H19A 2 0.369254 0.437506 0.366314 11.00000 -1.20000 H19B 2 0.309483 0.415920 0.459316 11.00000 -1.20000 AFIX 0 C20 1 0.456571 0.352081 0.483935 11.00000 0.02594 0.01401 = 0.02104 -0.00704 -0.00020 -0.00205 C21 1 0.457394 0.312101 0.581170 11.00000 0.02464 0.02047 = 0.02702 -0.01151 0.00777 -0.00178 AFIX 43 H21 2 0.396395 0.305129 0.611955 11.00000 -1.20000 AFIX 0 C22 1 0.545642 0.282546 0.633230 11.00000 0.03412 0.02722 = 0.01857 -0.01074 0.00170 -0.00425 AFIX 43 H22 2 0.544585 0.253556 0.699032 11.00000 -1.20000 AFIX 0 C23 1 0.635378 0.295099 0.589718 11.00000 0.02959 0.03390 = 0.02222 -0.01229 -0.00390 -0.00654 AFIX 43 H23 2 0.695385 0.276949 0.625673 11.00000 -1.20000 AFIX 0 C24 1 0.637487 0.334372 0.493175 11.00000 0.02367 0.02630 = 0.01811 -0.00902 0.00106 -0.00450 AFIX 43 H24 2 0.698780 0.342279 0.462987 11.00000 -1.20000 AFIX 0 C25 1 0.548362 0.361970 0.441334 11.00000 0.02368 0.01765 = 0.01923 -0.01064 0.00185 -0.00412 C26 1 0.567785 0.497487 0.300303 11.00000 0.01903 0.02225 = 0.02633 -0.01237 0.00104 -0.00271 AFIX 43 H26 2 0.563925 0.537665 0.337805 11.00000 -1.20000 AFIX 0 C27 1 0.588598 0.505500 0.136999 11.00000 0.01689 0.01532 = 0.01789 -0.00434 -0.00178 -0.00231 C28 1 0.617767 0.566958 0.045109 11.00000 0.01927 0.01876 = 0.01747 -0.00378 -0.00036 -0.00299 C29 1 0.639888 0.669690 0.022793 11.00000 0.02745 0.01673 = 0.01898 -0.00372 -0.00316 -0.00360 AFIX 43 H29 2 0.659067 0.708268 -0.038308 11.00000 -1.20000 AFIX 0 C30 1 0.634549 0.716367 0.087286 11.00000 0.02746 0.01917 = 0.01973 -0.00485 -0.00196 -0.00432 C31 1 0.607777 0.654693 0.176645 11.00000 0.02738 0.02044 = 0.02224 -0.00863 -0.00016 -0.00269 AFIX 43 H31 2 0.603890 0.684690 0.222062 11.00000 -1.20000 AFIX 0 C32 1 0.586371 0.551815 0.203468 11.00000 0.02004 0.01835 = 0.01952 -0.00603 0.00080 -0.00136 C33 1 0.662720 0.826429 0.061271 11.00000 0.05555 0.02290 = 0.02695 -0.01081 0.00209 -0.01358 C34 1 0.644539 0.867027 0.139644 11.00000 0.10477 0.02931 = 0.03264 -0.01587 0.00282 -0.02349 AFIX 33 H34A 2 0.681914 0.817308 0.195870 11.00000 -1.50000 H34B 2 0.666449 0.936117 0.120978 11.00000 -1.50000 H34C 2 0.573662 0.873537 0.152044 11.00000 -1.50000 AFIX 0 C35 1 0.774712 0.820606 0.040445 11.00000 0.05857 0.04499 = 0.07145 -0.01847 0.01073 -0.03271 AFIX 33 H35A 2 0.813375 0.770946 0.095898 11.00000 -1.50000 H35B 2 0.787151 0.796583 -0.010568 11.00000 -1.50000 H35C 2 0.794325 0.890612 0.022854 11.00000 -1.50000 AFIX 0 C36 1 0.604421 0.904057 -0.025956 11.00000 0.08873 0.01750 = 0.03862 -0.00446 -0.01221 -0.01017 AFIX 33 H36A 2 0.623036 0.974257 -0.041980 11.00000 -1.50000 H36B 2 0.619439 0.881018 -0.077252 11.00000 -1.50000 H36C 2 0.533304 0.906807 -0.014720 11.00000 -1.50000 AFIX 0 C37 1 0.635102 0.523747 -0.023901 11.00000 0.02342 0.01978 = 0.01774 -0.00411 -0.00211 -0.00332 AFIX 43 H37 2 0.655202 0.567353 -0.083086 11.00000 -1.20000 AFIX 0 C38 1 0.653902 0.371064 -0.067822 11.00000 0.02253 0.02380 = 0.02236 -0.01268 -0.00058 -0.00312 C39 1 0.672874 0.424379 -0.160910 11.00000 0.03649 0.02348 = 0.02600 -0.01191 -0.00438 0.00382 AFIX 43 H39 2 0.662661 0.499253 -0.187629 11.00000 -1.20000 AFIX 0 C40 1 0.706667 0.367718 -0.214239 11.00000 0.04526 0.03054 = 0.01740 -0.01086 -0.00542 0.00622 AFIX 43 H40 2 0.720788 0.403431 -0.277521 11.00000 -1.20000 AFIX 0 C41 1 0.719912 0.257515 -0.174399 11.00000 0.04424 0.03301 = 0.03184 -0.01965 0.00047 0.00159 AFIX 43 H41 2 0.742419 0.218148 -0.210817 11.00000 -1.20000 AFIX 0 C42 1 0.700502 0.206536 -0.083209 11.00000 0.05725 0.02159 = 0.02957 -0.01411 0.00120 -0.00497 AFIX 43 H42 2 0.710007 0.131655 -0.057238 11.00000 -1.20000 AFIX 0 C43 1 0.667262 0.260556 -0.027011 11.00000 0.03524 0.02199 = 0.03053 -0.01269 0.00458 -0.00663 C44 1 0.654401 0.199481 0.074732 11.00000 0.05703 0.01942 = 0.03536 -0.01116 0.01753 -0.01653 AFIX 23 H44A 2 0.629085 0.133411 0.082806 11.00000 -1.20000 H44B 2 0.604382 0.241542 0.098164 11.00000 -1.20000 AFIX 0 C45 1 0.752471 0.172091 0.132908 11.00000 0.06924 0.02485 = 0.01913 -0.00314 0.01512 0.00622 AFIX 23 H45A 2 0.740425 0.126270 0.197549 11.00000 -1.20000 H45B 2 0.802077 0.130743 0.108435 11.00000 -1.20000 AFIX 0 C46 1 0.796327 0.264818 0.134435 11.00000 0.02580 0.03604 = 0.01943 -0.00068 -0.00093 0.01002 C47 1 0.853665 0.321000 0.061494 11.00000 0.02862 0.06187 = 0.02832 -0.00249 0.00513 0.00163 AFIX 43 H47 2 0.866413 0.297972 0.011959 11.00000 -1.20000 AFIX 0 C48 1 0.891558 0.406924 0.059061 11.00000 0.02911 0.09192 = 0.02307 0.00718 0.00289 -0.01925 AFIX 43 H48 2 0.929063 0.443577 0.007947 11.00000 -1.20000 AFIX 0 C49 1 0.875581 0.441183 0.131036 11.00000 0.03949 0.07203 = 0.03415 0.00568 -0.00626 -0.03242 AFIX 43 H49 2 0.901542 0.501710 0.129209 11.00000 -1.20000 AFIX 0 C50 1 0.821092 0.386363 0.206421 11.00000 0.03329 0.04554 = 0.02992 -0.00327 0.00120 -0.01699 AFIX 43 H50 2 0.810645 0.408951 0.256425 11.00000 -1.20000 AFIX 0 C51 1 0.782442 0.299185 0.208020 11.00000 0.01885 0.02971 = 0.01956 0.00054 0.00152 -0.00085 C52 1 0.780297 0.177167 0.358561 11.00000 0.01595 0.02678 = 0.02842 -0.00962 0.00462 -0.00540 AFIX 43 H52 2 0.849977 0.169671 0.351428 11.00000 -1.20000 AFIX 0 N1 5 0.726908 0.242842 0.287682 11.00000 0.02036 0.02259 = 0.01677 -0.00705 0.00066 -0.00129 N2 5 0.445502 0.104615 0.537920 11.00000 0.01865 0.01641 = 0.01953 -0.00566 0.00367 -0.00357 AFIX 43 H2 2 0.456410 0.132627 0.478250 11.00000 -1.20000 AFIX 0 N3 5 0.555827 0.399542 0.341308 11.00000 0.01782 0.02034 = 0.01820 -0.00745 0.00076 -0.00173 N4 5 0.624572 0.426686 -0.009391 11.00000 0.02472 0.02153 = 0.01879 -0.00860 0.00045 -0.00460 AFIX 43 H4 2 0.596196 0.391815 0.042237 11.00000 -1.20000 AFIX 0 N5 5 0.939964 -0.033631 0.123050 10.50000 0.06380 O1 6 0.572600 0.158845 0.405679 11.00000 0.01931 0.01667 = 0.01639 -0.00215 -0.00272 -0.00102 O2 6 0.567747 0.410523 0.155842 11.00000 0.02601 0.01518 = 0.01720 -0.00484 0.00201 -0.00461 O3 6 1.000000 0.500000 0.500000 10.50000 0.06437 0.06670 = 0.06102 -0.00209 -0.02344 -0.03783 FE1 4 0.569956 0.285036 0.281352 11.00000 0.01937 0.01557 = 0.01602 -0.00460 0.00053 -0.00321 FE2 4 0.950912 0.467523 0.414055 11.00000 0.03150 0.03425 = 0.05647 -0.00902 -0.01871 -0.00484 BR1 3 0.437221 0.219456 0.220930 11.00000 0.03287 0.02479 = 0.01932 -0.00438 -0.00237 -0.01266 BR2A 3 0.909906 0.294272 0.492969 21.00000 0.02361 0.03690 = 0.07999 -0.01404 -0.00341 -0.00364 BR3 3 0.803584 0.581709 0.343633 11.00000 0.03607 0.04184 = 0.05477 -0.02634 -0.01503 0.00936 BR4A 3 1.067043 0.477075 0.294842 21.00000 0.03385 0.04766 = 0.07314 -0.01573 -0.00905 0.00268 C61 1 0.973785 -0.119999 0.155969 10.50000 0.04921 C62 1 1.007820 -0.233063 0.206353 10.50000 0.06162 AFIX 137 H62A 2 1.042338 -0.244209 0.264391 10.50000 -1.50000 H62B 2 1.053190 -0.259238 0.168045 10.50000 -1.50000 H62C 2 0.950645 -0.271200 0.220249 10.50000 -1.50000 AFIX 0 BR2B 3 0.926857 0.290676 0.453635 -21.00000 0.02361 0.03690 = 0.07999 -0.01404 -0.00341 -0.00364 BR4B 3 1.078022 0.488997 0.310177 -21.00000 0.03385 0.04766 = 0.07314 -0.01573 -0.00905 0.00268 HKLF 5 REM shelxt_a.res in P-1 REM wR2 = 0.1638, GooF = S = 1.049, Restrained GooF = 1.050 for all data REM R1 = 0.0605 for 8627 Fo > 4sig(Fo) and 0.0965 for all 12337 data REM 604 parameters refined using 6 restraints END WGHT 0.0696 8.1287 REM Highest difference peak 1.531, deepest hole -0.804, 1-sigma level 0.131 Q1 1 1.1134 -0.2733 0.3234 11.00000 0.05 1.53 Q2 1 0.5295 0.2667 0.2603 11.00000 0.05 1.29 Q3 1 0.4733 0.2349 0.2372 11.00000 0.05 1.17 Q4 1 0.6550 0.3249 0.3272 11.00000 0.05 1.13 Q5 1 0.8577 -0.1825 0.7285 11.00000 0.05 1.06 Q6 1 0.8434 -0.0059 0.7651 11.00000 0.05 1.01 Q7 1 0.7396 0.8691 -0.1170 11.00000 0.05 0.95 Q8 1 0.3708 0.1858 0.1933 11.00000 0.05 0.87 Q9 1 0.3414 0.1696 0.1715 11.00000 0.05 0.86 Q10 1 1.0137 -0.1888 0.0833 11.00000 0.05 0.84 Q11 1 0.9865 -0.0284 0.0709 11.00000 0.05 0.81 Q12 1 0.8945 0.6058 0.4057 11.00000 0.05 0.78 Q13 1 0.7557 0.3694 0.3795 11.00000 0.05 0.77 Q14 1 0.8177 0.7302 -0.0450 11.00000 0.05 0.75 Q15 1 0.7991 0.4652 -0.3661 11.00000 0.05 0.69 Q16 1 1.1012 -0.1219 0.0982 11.00000 0.05 0.68 Q17 1 0.7941 0.0694 -0.1536 11.00000 0.05 0.64 ; _shelx_res_checksum 88479 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.6441(3) 0.1094(3) 0.4680(3) 0.0175(9) Uani 1 1 d . . . . . C2 C 0.7456(4) 0.1131(4) 0.4484(3) 0.0207(10) Uani 1 1 d . . . . . C3 C 0.8184(4) 0.0544(4) 0.5183(3) 0.0240(10) Uani 1 1 d . . . . . H3 H 0.885982 0.057263 0.502927 0.029 Uiso 1 1 calc R U . . . C4 C 0.7973(4) -0.0084(4) 0.6094(3) 0.0237(10) Uani 1 1 d . . . . . C5 C 0.6972(4) -0.0085(4) 0.6288(3) 0.0216(10) Uani 1 1 d . . . . . H5 H 0.679671 -0.048152 0.690223 0.026 Uiso 1 1 calc R U . . . C6 C 0.6210(4) 0.0473(4) 0.5619(3) 0.0190(10) Uani 1 1 d . . . . . C7 C 0.8794(4) -0.0721(4) 0.6828(4) 0.0312(12) Uani 1 1 d . . . . . C8 C 0.9657(5) -0.0129(6) 0.6752(5) 0.0521(18) Uani 1 1 d . . . . . H8A H 0.988324 0.011372 0.611454 0.078 Uiso 1 1 calc R U . . . H8B H 0.944767 0.048060 0.691704 0.078 Uiso 1 1 calc R U . . . H8C H 1.019942 -0.059568 0.717616 0.078 Uiso 1 1 calc R U . . . C9 C 0.9214(6) -0.1705(5) 0.6611(6) 0.061(2) Uani 1 1 d . . . . . H9A H 0.945935 -0.147371 0.598042 0.091 Uiso 1 1 calc R U . . . H9B H 0.975803 -0.212725 0.705487 0.091 Uiso 1 1 calc R U . . . H9C H 0.868694 -0.213232 0.666285 0.091 Uiso 1 1 calc R U . . . C10 C 0.8426(6) -0.1105(9) 0.7798(5) 0.093(4) Uani 1 1 d . . . . . H10A H 0.786666 -0.148591 0.782898 0.139 Uiso 1 1 calc R U . . . H10B H 0.896066 -0.157812 0.822794 0.139 Uiso 1 1 calc R U . . . H10C H 0.820891 -0.050184 0.796883 0.139 Uiso 1 1 calc R U . . . C11 C 0.5218(3) 0.0501(4) 0.5916(3) 0.0185(9) Uani 1 1 d . . . . . H11 H 0.510670 0.009682 0.654750 0.022 Uiso 1 1 calc R U . . . C12 C 0.3461(4) 0.1246(4) 0.5639(3) 0.0214(10) Uani 1 1 d . . . . . C13 C 0.3131(4) 0.0584(4) 0.6488(4) 0.0230(10) Uani 1 1 d . . . . . H13 H 0.356061 -0.001502 0.688975 0.028 Uiso 1 1 calc R U . . . C14 C 0.2168(4) 0.0814(4) 0.6736(4) 0.0274(11) Uani 1 1 d . . . . . H14 H 0.193207 0.036389 0.730474 0.033 Uiso 1 1 calc R U . . . C15 C 0.1555(4) 0.1694(4) 0.6159(4) 0.0296(12) Uani 1 1 d . . . . . H15 H 0.090204 0.186004 0.633796 0.036 Uiso 1 1 calc R U . . . C16 C 0.1889(4) 0.2339(4) 0.5317(4) 0.0269(11) Uani 1 1 d . . . . . H16 H 0.145294 0.293389 0.491927 0.032 Uiso 1 1 calc R U . . . C17 C 0.2847(4) 0.2135(4) 0.5042(3) 0.0212(10) Uani 1 1 d . . . . . C18 C 0.3185(4) 0.2918(4) 0.4145(3) 0.0231(10) Uani 1 1 d . . . . . H18A H 0.261798 0.321489 0.369006 0.028 Uiso 1 1 calc R U . . . H18B H 0.370496 0.254513 0.388530 0.028 Uiso 1 1 calc R U . . . C19 C 0.3598(4) 0.3832(4) 0.4281(4) 0.0249(11) Uani 1 1 d . . . . . H19A H 0.369254 0.437506 0.366314 0.030 Uiso 1 1 calc R U . . . H19B H 0.309483 0.415920 0.459316 0.030 Uiso 1 1 calc R U . . . C20 C 0.4566(4) 0.3521(4) 0.4839(3) 0.0203(10) Uani 1 1 d . . . . . C21 C 0.4574(4) 0.3121(4) 0.5812(3) 0.0236(10) Uani 1 1 d . . . . . H21 H 0.396395 0.305129 0.611955 0.028 Uiso 1 1 calc R U . . . C22 C 0.5456(4) 0.2825(4) 0.6332(4) 0.0261(11) Uani 1 1 d . . . . . H22 H 0.544585 0.253556 0.699032 0.031 Uiso 1 1 calc R U . . . C23 C 0.6354(4) 0.2951(4) 0.5897(4) 0.0279(11) Uani 1 1 d . . . . . H23 H 0.695385 0.276949 0.625673 0.033 Uiso 1 1 calc R U . . . C24 C 0.6375(4) 0.3344(4) 0.4932(3) 0.0225(10) Uani 1 1 d . . . . . H24 H 0.698780 0.342279 0.462987 0.027 Uiso 1 1 calc R U . . . C25 C 0.5484(4) 0.3620(4) 0.4413(3) 0.0190(9) Uani 1 1 d . . . . . C26 C 0.5678(3) 0.4975(4) 0.3003(3) 0.0217(10) Uani 1 1 d . . . . . H26 H 0.563925 0.537665 0.337805 0.026 Uiso 1 1 calc R U . . . C27 C 0.5886(3) 0.5055(3) 0.1370(3) 0.0173(9) Uani 1 1 d . . . . . C28 C 0.6178(3) 0.5670(4) 0.0451(3) 0.0195(10) Uani 1 1 d . . . . . C29 C 0.6399(4) 0.6697(4) 0.0228(3) 0.0219(10) Uani 1 1 d . . . . . H29 H 0.659067 0.708268 -0.038308 0.026 Uiso 1 1 calc R U . . . C30 C 0.6345(4) 0.7164(4) 0.0873(3) 0.0228(10) Uani 1 1 d . . . . . C31 C 0.6078(4) 0.6547(4) 0.1766(3) 0.0233(10) Uani 1 1 d . . . . . H31 H 0.603890 0.684690 0.222062 0.028 Uiso 1 1 calc R U . . . C32 C 0.5864(3) 0.5518(4) 0.2035(3) 0.0199(10) Uani 1 1 d . . . . . C33 C 0.6627(5) 0.8264(4) 0.0613(4) 0.0340(13) Uani 1 1 d . . . . . C34 C 0.6445(7) 0.8670(5) 0.1396(4) 0.0529(19) Uani 1 1 d . . . . . H34A H 0.681914 0.817308 0.195870 0.079 Uiso 1 1 calc R U . . . H34B H 0.666449 0.936117 0.120978 0.079 Uiso 1 1 calc R U . . . H34C H 0.573662 0.873537 0.152044 0.079 Uiso 1 1 calc R U . . . C35 C 0.7747(6) 0.8206(6) 0.0404(6) 0.057(2) Uani 1 1 d . . . . . H35A H 0.813375 0.770946 0.095898 0.086 Uiso 1 1 calc R U . . . H35B H 0.787151 0.796583 -0.010568 0.086 Uiso 1 1 calc R U . . . H35C H 0.794325 0.890612 0.022854 0.086 Uiso 1 1 calc R U . . . C36 C 0.6044(6) 0.9041(4) -0.0260(4) 0.0497(18) Uani 1 1 d . . . . . H36A H 0.623036 0.974257 -0.041980 0.075 Uiso 1 1 calc R U . . . H36B H 0.619439 0.881018 -0.077252 0.075 Uiso 1 1 calc R U . . . H36C H 0.533304 0.906807 -0.014720 0.075 Uiso 1 1 calc R U . . . C37 C 0.6351(4) 0.5237(4) -0.0239(3) 0.0212(10) Uani 1 1 d . . . . . H37 H 0.655202 0.567353 -0.083086 0.025 Uiso 1 1 calc R U . . . C38 C 0.6539(4) 0.3711(4) -0.0678(3) 0.0218(10) Uani 1 1 d . . . . . C39 C 0.6729(4) 0.4244(4) -0.1609(4) 0.0287(12) Uani 1 1 d . . . . . H39 H 0.662661 0.499253 -0.187629 0.034 Uiso 1 1 calc R U . . . C40 C 0.7067(4) 0.3677(4) -0.2142(4) 0.0317(12) Uani 1 1 d . . . . . H40 H 0.720788 0.403431 -0.277521 0.038 Uiso 1 1 calc R U . . . C41 C 0.7199(5) 0.2575(4) -0.1744(4) 0.0350(13) Uani 1 1 d . . . . . H41 H 0.742419 0.218148 -0.210817 0.042 Uiso 1 1 calc R U . . . C42 C 0.7005(5) 0.2065(4) -0.0832(4) 0.0349(13) Uani 1 1 d . . . . . H42 H 0.710007 0.131655 -0.057238 0.042 Uiso 1 1 calc R U . . . C43 C 0.6673(4) 0.2606(4) -0.0270(4) 0.0283(11) Uani 1 1 d . . . . . C44 C 0.6544(5) 0.1995(4) 0.0747(4) 0.0362(14) Uani 1 1 d . . . . . H44A H 0.629085 0.133411 0.082806 0.043 Uiso 1 1 calc R U . . . H44B H 0.604382 0.241542 0.098164 0.043 Uiso 1 1 calc R U . . . C45 C 0.7525(5) 0.1721(4) 0.1329(4) 0.0410(16) Uani 1 1 d . . . . . H45A H 0.740425 0.126270 0.197549 0.049 Uiso 1 1 calc R U . . . H45B H 0.802077 0.130743 0.108435 0.049 Uiso 1 1 calc R U . . . C46 C 0.7963(4) 0.2648(4) 0.1344(4) 0.0317(12) Uani 1 1 d . . . . . C47 C 0.8537(4) 0.3210(6) 0.0615(4) 0.0452(16) Uani 1 1 d . . . . . H47 H 0.866413 0.297972 0.011959 0.054 Uiso 1 1 calc R U . . . C48 C 0.8916(5) 0.4069(7) 0.0591(4) 0.056(2) Uani 1 1 d . . . . . H48 H 0.929063 0.443577 0.007947 0.067 Uiso 1 1 calc R U . . . C49 C 0.8756(5) 0.4412(6) 0.1310(4) 0.054(2) Uani 1 1 d . . . . . H49 H 0.901542 0.501710 0.129209 0.065 Uiso 1 1 calc R U . . . C50 C 0.8211(4) 0.3864(5) 0.2064(4) 0.0385(14) Uani 1 1 d . . . . . H50 H 0.810645 0.408951 0.256425 0.046 Uiso 1 1 calc R U . . . C51 C 0.7824(4) 0.2992(4) 0.2080(3) 0.0261(11) Uani 1 1 d . . . . . C52 C 0.7803(4) 0.1772(4) 0.3586(4) 0.0239(11) Uani 1 1 d . . . . . H52 H 0.849977 0.169671 0.351428 0.029 Uiso 1 1 calc R U . . . N1 N 0.7269(3) 0.2428(3) 0.2877(3) 0.0203(8) Uani 1 1 d . . . . . N2 N 0.4455(3) 0.1046(3) 0.5379(3) 0.0185(8) Uani 1 1 d . . . . . H2 H 0.456410 0.132627 0.478250 0.022 Uiso 1 1 calc R U . . . N3 N 0.5558(3) 0.3995(3) 0.3413(3) 0.0189(8) Uani 1 1 d . . . . . N4 N 0.6246(3) 0.4267(3) -0.0094(3) 0.0213(9) Uani 1 1 d . . . . . H4 H 0.596196 0.391815 0.042237 0.026 Uiso 1 1 calc R U . . . N5 N 0.9400(10) -0.0336(11) 0.1231(9) 0.064(3) Uiso 0.5 1 d . . P . . O1 O 0.5726(2) 0.1588(2) 0.4057(2) 0.0189(7) Uani 1 1 d . . . . . O2 O 0.5677(2) 0.4105(2) 0.1558(2) 0.0198(7) Uani 1 1 d . . . . . O3 O 1.000000 0.500000 0.500000 0.067(2) Uani 1 2 d S . P . . Fe1 Fe 0.56996(5) 0.28504(5) 0.28135(5) 0.01738(15) Uani 1 1 d . . . . . Fe2 Fe 0.95091(6) 0.46752(7) 0.41406(7) 0.0430(2) Uani 1 1 d D . . . . Br1 Br 0.43722(4) 0.21946(4) 0.22093(3) 0.02598(13) Uani 1 1 d . . . . . Br2A Br 0.90991(10) 0.29427(8) 0.49297(17) 0.0495(5) Uani 0.809(5) 1 d D . P . . Br3 Br 0.80358(5) 0.58171(5) 0.34363(5) 0.04322(17) Uani 1 1 d . . . . . Br4A Br 1.06704(15) 0.4771(2) 0.29484(17) 0.0546(4) Uani 0.809(5) 1 d D . P . . C61 C 0.9738(11) -0.1200(11) 0.1560(10) 0.049(3) Uiso 0.5 1 d . . P . . C62 C 1.0078(12) -0.2331(12) 0.2064(11) 0.062(4) Uiso 0.5 1 d . . P . . H62A H 1.042338 -0.244209 0.264391 0.092 Uiso 0.5 1 calc R U P . . H62B H 1.053190 -0.259238 0.168045 0.092 Uiso 0.5 1 calc R U P . . H62C H 0.950645 -0.271200 0.220249 0.092 Uiso 0.5 1 calc R U P . . Br2B Br 0.9269(4) 0.2907(4) 0.4536(6) 0.0495(5) Uani 0.191(5) 1 d D . P . . Br4B Br 1.0780(7) 0.4890(10) 0.3102(8) 0.0546(4) Uani 0.191(5) 1 d D . P . . 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 0.019(2) 0.014(2) 0.020(2) -0.0079(18) -0.0001(18) -0.0009(17) C2 0.020(2) 0.022(2) 0.020(2) -0.008(2) -0.0009(19) -0.0016(19) C3 0.019(2) 0.027(3) 0.026(3) -0.010(2) 0.002(2) -0.004(2) C4 0.025(3) 0.025(3) 0.020(3) -0.007(2) -0.001(2) -0.002(2) C5 0.023(2) 0.018(2) 0.022(2) -0.005(2) 0.000(2) -0.0056(19) C6 0.022(2) 0.016(2) 0.021(2) -0.0084(19) 0.0014(19) -0.0043(18) C7 0.025(3) 0.035(3) 0.025(3) -0.001(2) -0.004(2) -0.009(2) C8 0.033(3) 0.058(4) 0.047(4) 0.003(3) -0.013(3) -0.013(3) C9 0.054(5) 0.043(4) 0.078(5) -0.020(4) -0.032(4) 0.010(3) C10 0.039(4) 0.165(10) 0.028(4) 0.017(5) -0.008(3) -0.019(5) C11 0.021(2) 0.016(2) 0.016(2) -0.0039(18) -0.0005(18) -0.0020(18) C12 0.022(2) 0.021(2) 0.026(3) -0.012(2) 0.000(2) -0.0048(19) C13 0.021(2) 0.018(2) 0.027(3) -0.006(2) 0.004(2) -0.0021(19) C14 0.027(3) 0.023(3) 0.030(3) -0.007(2) 0.009(2) -0.007(2) C15 0.020(3) 0.029(3) 0.036(3) -0.010(2) 0.006(2) -0.002(2) C16 0.018(2) 0.026(3) 0.035(3) -0.010(2) -0.002(2) -0.003(2) C17 0.022(2) 0.022(2) 0.022(2) -0.011(2) 0.0013(19) -0.0037(19) C18 0.018(2) 0.028(3) 0.020(2) -0.007(2) -0.0011(19) 0.002(2) C19 0.023(3) 0.018(2) 0.027(3) -0.002(2) 0.005(2) -0.0017(19) C20 0.026(3) 0.014(2) 0.021(2) -0.0070(19) 0.000(2) -0.0020(19) C21 0.025(3) 0.020(2) 0.027(3) -0.012(2) 0.008(2) -0.002(2) C22 0.034(3) 0.027(3) 0.019(2) -0.011(2) 0.002(2) -0.004(2) C23 0.030(3) 0.034(3) 0.022(3) -0.012(2) -0.004(2) -0.007(2) C24 0.024(3) 0.026(3) 0.018(2) -0.009(2) 0.0011(19) -0.004(2) C25 0.024(2) 0.018(2) 0.019(2) -0.0106(19) 0.0018(19) -0.0041(19) C26 0.019(2) 0.022(2) 0.026(3) -0.012(2) 0.001(2) -0.0027(19) C27 0.017(2) 0.015(2) 0.018(2) -0.0043(18) -0.0018(18) -0.0023(17) C28 0.019(2) 0.019(2) 0.017(2) -0.0038(19) -0.0004(18) -0.0030(18) C29 0.027(3) 0.017(2) 0.019(2) -0.0037(19) -0.003(2) -0.0036(19) C30 0.027(3) 0.019(2) 0.020(2) -0.005(2) -0.002(2) -0.004(2) C31 0.027(3) 0.020(2) 0.022(3) -0.009(2) 0.000(2) -0.003(2) C32 0.020(2) 0.018(2) 0.020(2) -0.0060(19) 0.0008(19) -0.0014(18) C33 0.056(4) 0.023(3) 0.027(3) -0.011(2) 0.002(3) -0.014(3) C34 0.105(6) 0.029(3) 0.033(3) -0.016(3) 0.003(4) -0.023(4) C35 0.059(5) 0.045(4) 0.071(5) -0.018(4) 0.011(4) -0.033(4) C36 0.089(5) 0.017(3) 0.039(4) -0.004(3) -0.012(3) -0.010(3) C37 0.023(3) 0.020(2) 0.018(2) -0.0041(19) -0.0021(19) -0.0033(19) C38 0.023(2) 0.024(2) 0.022(3) -0.013(2) -0.001(2) -0.003(2) C39 0.036(3) 0.023(3) 0.026(3) -0.012(2) -0.004(2) 0.004(2) C40 0.045(3) 0.031(3) 0.017(3) -0.011(2) -0.005(2) 0.006(2) C41 0.044(3) 0.033(3) 0.032(3) -0.020(3) 0.000(3) 0.002(3) C42 0.057(4) 0.022(3) 0.030(3) -0.014(2) 0.001(3) -0.005(3) C43 0.035(3) 0.022(3) 0.031(3) -0.013(2) 0.005(2) -0.007(2) C44 0.057(4) 0.019(3) 0.035(3) -0.011(2) 0.018(3) -0.017(3) C45 0.069(5) 0.025(3) 0.019(3) -0.003(2) 0.015(3) 0.006(3) C46 0.026(3) 0.036(3) 0.019(3) -0.001(2) -0.001(2) 0.010(2) C47 0.029(3) 0.062(4) 0.028(3) -0.002(3) 0.005(3) 0.002(3) C48 0.029(3) 0.092(6) 0.023(3) 0.007(3) 0.003(3) -0.019(4) C49 0.039(4) 0.072(5) 0.034(4) 0.006(3) -0.006(3) -0.032(3) C50 0.033(3) 0.046(4) 0.030(3) -0.003(3) 0.001(2) -0.017(3) C51 0.019(2) 0.030(3) 0.020(3) 0.001(2) 0.002(2) -0.001(2) C52 0.016(2) 0.027(3) 0.028(3) -0.010(2) 0.005(2) -0.005(2) N1 0.020(2) 0.023(2) 0.017(2) -0.0070(17) 0.0007(16) -0.0013(16) N2 0.019(2) 0.0164(19) 0.020(2) -0.0057(16) 0.0037(16) -0.0036(16) N3 0.018(2) 0.020(2) 0.018(2) -0.0074(16) 0.0008(16) -0.0017(16) N4 0.025(2) 0.022(2) 0.019(2) -0.0086(17) 0.0004(17) -0.0046(17) O1 0.0193(17) 0.0167(16) 0.0164(16) -0.0022(13) -0.0027(13) -0.0010(13) O2 0.0260(18) 0.0152(16) 0.0172(16) -0.0048(13) 0.0020(14) -0.0046(13) O3 0.064(5) 0.067(5) 0.061(5) -0.002(4) -0.023(4) -0.038(4) Fe1 0.0194(3) 0.0156(3) 0.0160(3) -0.0046(3) 0.0005(3) -0.0032(3) Fe2 0.0315(5) 0.0342(5) 0.0565(6) -0.0090(4) -0.0187(4) -0.0048(4) Br1 0.0329(3) 0.0248(3) 0.0193(3) -0.0044(2) -0.0024(2) -0.0127(2) Br2A 0.0236(5) 0.0369(4) 0.0800(12) -0.0140(5) -0.0034(6) -0.0036(3) Br3 0.0361(3) 0.0418(3) 0.0548(4) -0.0263(3) -0.0150(3) 0.0094(3) Br4A 0.0338(6) 0.0477(8) 0.0731(10) -0.0157(5) -0.0090(6) 0.0027(4) Br2B 0.0236(5) 0.0369(4) 0.0800(12) -0.0140(5) -0.0034(6) -0.0036(3) Br4B 0.0338(6) 0.0477(8) 0.0731(10) -0.0157(5) -0.0090(6) 0.0027(4) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' 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 C2 C1 C6 116.9(4) . . ? O1 C1 C2 123.2(4) . . ? O1 C1 C6 119.9(4) . . ? C1 C2 C52 123.4(4) . . ? C3 C2 C1 119.8(4) . . ? C3 C2 C52 116.8(4) . . ? C2 C3 H3 118.0 . . ? C4 C3 C2 123.9(5) . . ? C4 C3 H3 118.0 . . ? C3 C4 C7 121.9(5) . . ? C5 C4 C3 115.8(4) . . ? C5 C4 C7 122.3(4) . . ? C4 C5 H5 118.5 . . ? C4 C5 C6 123.1(5) . . ? C6 C5 H5 118.5 . . ? C5 C6 C1 120.4(4) . . ? C5 C6 C11 118.0(4) . . ? C11 C6 C1 121.2(4) . . ? C4 C7 C9 106.6(5) . . ? C8 C7 C4 112.1(5) . . ? C8 C7 C9 105.6(6) . . ? C10 C7 C4 113.0(5) . . ? C10 C7 C8 111.0(6) . . ? C10 C7 C9 107.9(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11 118.0 . . ? N2 C11 C6 124.0(4) . . ? N2 C11 H11 118.0 . . ? C13 C12 N2 120.4(4) . . ? C17 C12 C13 121.5(5) . . ? C17 C12 N2 118.1(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 C12 119.1(5) . . ? C14 C13 H13 120.4 . . ? C13 C14 H14 119.9 . . ? C15 C14 C13 120.2(5) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 120.0 . . ? C14 C15 C16 120.0(5) . . ? C16 C15 H15 120.0 . . ? C15 C16 H16 119.2 . . ? C15 C16 C17 121.6(5) . . ? C17 C16 H16 119.2 . . ? C12 C17 C18 123.8(4) . . ? C16 C17 C12 117.5(5) . . ? C16 C17 C18 118.6(4) . . ? C17 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C17 C18 C19 112.5(4) . . ? H18A C18 H18B 107.8 . . ? C19 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C18 C19 H19A 108.5 . . ? C18 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C20 C19 C18 115.2(4) . . ? C20 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? C21 C20 C19 120.6(4) . . ? C21 C20 C25 117.5(4) . . ? C25 C20 C19 121.9(4) . . ? C20 C21 H21 119.4 . . ? C22 C21 C20 121.2(5) . . ? C22 C21 H21 119.4 . . ? C21 C22 H22 119.8 . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22 119.8 . . ? C22 C23 H23 120.0 . . ? C22 C23 C24 120.0(5) . . ? C24 C23 H23 120.0 . . ? C23 C24 H24 120.4 . . ? C23 C24 C25 119.2(5) . . ? C25 C24 H24 120.4 . . ? C20 C25 N3 121.8(4) . . ? C24 C25 C20 121.7(4) . . ? C24 C25 N3 116.5(4) . . ? C32 C26 H26 116.7 . . ? N3 C26 H26 116.7 . . ? N3 C26 C32 126.7(4) . . ? C32 C27 C28 117.0(4) . . ? O2 C27 C28 119.6(4) . . ? O2 C27 C32 123.4(4) . . ? C29 C28 C27 120.8(4) . . ? C29 C28 C37 117.0(4) . . ? C37 C28 C27 121.9(4) . . ? C28 C29 H29 118.9 . . ? C30 C29 C28 122.2(5) . . ? C30 C29 H29 118.9 . . ? C29 C30 C31 116.2(4) . . ? C29 C30 C33 120.5(4) . . ? C31 C30 C33 123.2(4) . . ? C30 C31 H31 117.8 . . ? C32 C31 C30 124.4(5) . . ? C32 C31 H31 117.8 . . ? C27 C32 C26 123.9(4) . . ? C31 C32 C26 116.5(4) . . ? C31 C32 C27 119.5(4) . . ? C30 C33 C34 112.4(5) . . ? C30 C33 C35 108.0(5) . . ? C34 C33 C35 108.5(6) . . ? C36 C33 C30 110.2(5) . . ? C36 C33 C34 109.2(5) . . ? C36 C33 C35 108.4(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C28 C37 H37 118.5 . . ? N4 C37 C28 122.9(4) . . ? N4 C37 H37 118.5 . . ? C39 C38 C43 121.3(5) . . ? C39 C38 N4 121.2(4) . . ? C43 C38 N4 117.5(4) . . ? C38 C39 H39 120.2 . . ? C40 C39 C38 119.7(5) . . ? C40 C39 H39 120.2 . . ? C39 C40 H40 120.2 . . ? C39 C40 C41 119.6(5) . . ? C41 C40 H40 120.2 . . ? C40 C41 H41 120.0 . . ? C42 C41 C40 120.0(5) . . ? C42 C41 H41 120.0 . . ? C41 C42 H42 118.9 . . ? C41 C42 C43 122.2(5) . . ? C43 C42 H42 118.9 . . ? C38 C43 C44 123.1(5) . . ? C42 C43 C38 117.3(5) . . ? C42 C43 C44 119.4(5) . . ? C43 C44 H44A 109.1 . . ? C43 C44 H44B 109.1 . . ? C43 C44 C45 112.5(5) . . ? H44A C44 H44B 107.8 . . ? C45 C44 H44A 109.1 . . ? C45 C44 H44B 109.1 . . ? C44 C45 H45A 108.4 . . ? C44 C45 H45B 108.4 . . ? H45A C45 H45B 107.4 . . ? C46 C45 C44 115.7(5) . . ? C46 C45 H45A 108.4 . . ? C46 C45 H45B 108.4 . . ? C47 C46 C45 120.9(6) . . ? C47 C46 C51 116.9(6) . . ? C51 C46 C45 122.3(5) . . ? C46 C47 H47 118.8 . . ? C48 C47 C46 122.5(7) . . ? C48 C47 H47 118.8 . . ? C47 C48 H48 120.0 . . ? C47 C48 C49 120.0(6) . . ? C49 C48 H48 120.0 . . ? C48 C49 H49 120.1 . . ? C48 C49 C50 119.7(7) . . ? C50 C49 H49 120.1 . . ? C49 C50 H50 120.1 . . ? C51 C50 C49 119.8(6) . . ? C51 C50 H50 120.1 . . ? C46 C51 N1 120.2(5) . . ? C50 C51 C46 121.1(5) . . ? C50 C51 N1 118.8(5) . . ? C2 C52 H52 116.5 . . ? N1 C52 C2 127.1(4) . . ? N1 C52 H52 116.5 . . ? C51 N1 Fe1 118.3(3) . . ? C52 N1 C51 114.9(4) . . ? C52 N1 Fe1 126.5(3) . . ? C11 N2 C12 127.8(4) . . ? C11 N2 H2 116.1 . . ? C12 N2 H2 116.1 . . ? C25 N3 Fe1 117.2(3) . . ? C26 N3 C25 115.3(4) . . ? C26 N3 Fe1 126.6(3) . . ? C37 N4 C38 127.3(4) . . ? C37 N4 H4 116.3 . . ? C38 N4 H4 116.3 . . ? C1 O1 Fe1 130.8(3) . . ? C27 O2 Fe1 129.8(3) . . ? Fe2 O3 Fe2 180.00(7) 2_766 . ? N1 Fe1 Br1 130.28(11) . . ? N3 Fe1 N1 100.78(15) . . ? N3 Fe1 Br1 128.93(11) . . ? O1 Fe1 N1 85.53(14) . . ? O1 Fe1 N3 94.83(14) . . ? O1 Fe1 O2 179.35(14) . . ? O1 Fe1 Br1 89.71(9) . . ? O2 Fe1 N1 94.24(14) . . ? O2 Fe1 N3 85.80(14) . . ? O2 Fe1 Br1 89.97(9) . . ? O3 Fe2 Br2A 105.40(7) . . ? O3 Fe2 Br3 111.78(5) . . ? O3 Fe2 Br4A 111.04(6) . . ? O3 Fe2 Br2B 117.8(2) . . ? O3 Fe2 Br4B 102.0(2) . . ? Br2A Fe2 Br4A 112.66(8) . . ? Br3 Fe2 Br2A 108.00(4) . . ? Br3 Fe2 Br4A 107.95(7) . . ? Br2B Fe2 Br2A 16.19(19) . . ? Br2B Fe2 Br3 109.62(13) . . ? Br2B Fe2 Br4A 97.4(2) . . ? Br4B Fe2 Br2A 118.0(3) . . ? Br4B Fe2 Br3 111.4(3) . . ? Br4B Fe2 Br4A 9.2(2) . . ? Br4B Fe2 Br2B 103.6(3) . . ? Br2B Br2A Fe2 79.9(5) . . ? N5 C61 C62 173.1(17) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Br2A Br2B Fe2 83.9(5) . . ? 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 C2 1.415(7) . ? C1 C6 1.442(7) . ? C1 O1 1.307(6) . ? C2 C3 1.405(7) . ? C2 C52 1.455(7) . ? C3 H3 0.9500 . ? C3 C4 1.403(7) . ? C4 C5 1.392(7) . ? C4 C7 1.531(7) . ? C5 H5 0.9500 . ? C5 C6 1.403(7) . ? C6 C11 1.422(7) . ? C7 C8 1.509(8) . ? C7 C9 1.562(9) . ? C7 C10 1.501(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 0.9500 . ? C11 N2 1.298(6) . ? C12 C13 1.400(7) . ? C12 C17 1.396(7) . ? C12 N2 1.426(6) . ? C13 H13 0.9500 . ? C13 C14 1.389(7) . ? C14 H14 0.9500 . ? C14 C15 1.377(7) . ? C15 H15 0.9500 . ? C15 C16 1.387(8) . ? C16 H16 0.9500 . ? C16 C17 1.391(7) . ? C17 C18 1.517(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.550(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.513(7) . ? C20 C21 1.403(7) . ? C20 C25 1.404(7) . ? C21 H21 0.9500 . ? C21 C22 1.388(7) . ? C22 H22 0.9500 . ? C22 C23 1.387(8) . ? C23 H23 0.9500 . ? C23 C24 1.395(7) . ? C24 H24 0.9500 . ? C24 C25 1.398(7) . ? C25 N3 1.452(6) . ? C26 H26 0.9500 . ? C26 C32 1.443(7) . ? C26 N3 1.295(6) . ? C27 C28 1.441(6) . ? C27 C32 1.417(7) . ? C27 O2 1.310(5) . ? C28 C29 1.410(7) . ? C28 C37 1.425(7) . ? C29 H29 0.9500 . ? C29 C30 1.391(7) . ? C30 C31 1.401(7) . ? C30 C33 1.529(7) . ? C31 H31 0.9500 . ? C31 C32 1.400(7) . ? C33 C34 1.537(8) . ? C33 C35 1.552(9) . ? C33 C36 1.524(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37 0.9500 . ? C37 N4 1.309(6) . ? C38 C39 1.393(7) . ? C38 C43 1.403(7) . ? C38 N4 1.426(6) . ? C39 H39 0.9500 . ? C39 C40 1.383(7) . ? C40 H40 0.9500 . ? C40 C41 1.399(8) . ? C41 H41 0.9500 . ? C41 C42 1.365(8) . ? C42 H42 0.9500 . ? C42 C43 1.391(7) . ? C43 C44 1.507(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.551(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.507(9) . ? C46 C47 1.404(8) . ? C46 C51 1.406(8) . ? C47 H47 0.9500 . ? C47 C48 1.357(11) . ? C48 H48 0.9500 . ? C48 C49 1.384(11) . ? C49 H49 0.9500 . ? C49 C50 1.398(8) . ? C50 H50 0.9500 . ? C50 C51 1.382(8) . ? C51 N1 1.454(6) . ? C52 H52 0.9500 . ? C52 N1 1.287(6) . ? N1 Fe1 2.131(4) . ? N2 H2 0.8800 . ? N3 Fe1 2.124(4) . ? N4 H4 0.8800 . ? N5 C61 1.137(18) . ? O1 Fe1 2.052(3) . ? O2 Fe1 2.059(3) . ? O3 Fe2 1.7494(9) . ? O3 Fe2 1.7493(9) 2_766 ? Fe1 Br1 2.4967(8) . ? Fe2 Br2A 2.3880(14) . ? Fe2 Br3 2.3666(10) . ? Fe2 Br4A 2.395(2) . ? Fe2 Br2B 2.364(5) . ? Fe2 Br4B 2.319(11) . ? Br2A Br2B 0.670(8) . ? C61 C62 1.47(2) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? 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_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -1.2(8) . . . . ? C1 C2 C52 N1 4.7(8) . . . . ? C1 C6 C11 N2 2.2(7) . . . . ? C2 C1 C6 C5 -1.6(6) . . . . ? C2 C1 C6 C11 171.2(4) . . . . ? C2 C1 O1 Fe1 -20.9(6) . . . . ? C2 C3 C4 C5 -1.1(7) . . . . ? C2 C3 C4 C7 179.3(5) . . . . ? C2 C52 N1 C51 177.6(5) . . . . ? C2 C52 N1 Fe1 3.4(7) . . . . ? C3 C2 C52 N1 -174.1(5) . . . . ? C3 C4 C5 C6 2.0(7) . . . . ? C3 C4 C7 C8 38.7(8) . . . . ? C3 C4 C7 C9 -76.4(6) . . . . ? C3 C4 C7 C10 165.2(7) . . . . ? C4 C5 C6 C1 -0.7(7) . . . . ? C4 C5 C6 C11 -173.7(4) . . . . ? C5 C4 C7 C8 -140.9(6) . . . . ? C5 C4 C7 C9 103.9(6) . . . . ? C5 C4 C7 C10 -14.5(9) . . . . ? C5 C6 C11 N2 175.2(4) . . . . ? C6 C1 C2 C3 2.5(7) . . . . ? C6 C1 C2 C52 -176.4(4) . . . . ? C6 C1 O1 Fe1 159.3(3) . . . . ? C6 C11 N2 C12 -170.0(4) . . . . ? C7 C4 C5 C6 -178.4(5) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C12 C17 C18 C19 -90.4(6) . . . . ? C13 C12 C17 C16 -0.5(7) . . . . ? C13 C12 C17 C18 175.9(5) . . . . ? C13 C12 N2 C11 -21.2(7) . . . . ? C13 C14 C15 C16 1.6(8) . . . . ? C14 C15 C16 C17 -1.5(8) . . . . ? C15 C16 C17 C12 0.9(7) . . . . ? C15 C16 C17 C18 -175.6(5) . . . . ? C16 C17 C18 C19 85.8(5) . . . . ? C17 C12 C13 C14 0.6(7) . . . . ? C17 C12 N2 C11 156.4(5) . . . . ? C17 C18 C19 C20 68.1(6) . . . . ? C18 C19 C20 C21 -84.3(6) . . . . ? C18 C19 C20 C25 95.9(5) . . . . ? C19 C20 C21 C22 179.6(4) . . . . ? C19 C20 C25 C24 179.1(4) . . . . ? C19 C20 C25 N3 -2.0(7) . . . . ? C20 C21 C22 C23 2.0(7) . . . . ? C20 C25 N3 C26 100.5(5) . . . . ? C20 C25 N3 Fe1 -89.3(5) . . . . ? C21 C20 C25 C24 -0.7(7) . . . . ? C21 C20 C25 N3 178.2(4) . . . . ? C21 C22 C23 C24 -2.1(8) . . . . ? C22 C23 C24 C25 0.8(7) . . . . ? C23 C24 C25 C20 0.6(7) . . . . ? C23 C24 C25 N3 -178.3(4) . . . . ? C24 C25 N3 C26 -80.6(5) . . . . ? C24 C25 N3 Fe1 89.6(4) . . . . ? C25 C20 C21 C22 -0.6(7) . . . . ? C27 C28 C29 C30 -0.2(7) . . . . ? C27 C28 C37 N4 1.0(7) . . . . ? C28 C27 C32 C26 -174.1(4) . . . . ? C28 C27 C32 C31 2.8(7) . . . . ? C28 C27 O2 Fe1 157.0(3) . . . . ? C28 C29 C30 C31 1.2(7) . . . . ? C28 C29 C30 C33 177.8(5) . . . . ? C28 C37 N4 C38 -169.8(5) . . . . ? C29 C28 C37 N4 174.8(5) . . . . ? C29 C30 C31 C32 -0.3(8) . . . . ? C29 C30 C33 C34 175.8(5) . . . . ? C29 C30 C33 C35 -64.4(7) . . . . ? C29 C30 C33 C36 53.8(7) . . . . ? C30 C31 C32 C26 175.3(5) . . . . ? C30 C31 C32 C27 -1.8(8) . . . . ? C31 C30 C33 C34 -7.9(8) . . . . ? C31 C30 C33 C35 111.9(6) . . . . ? C31 C30 C33 C36 -129.9(6) . . . . ? C32 C26 N3 C25 173.9(4) . . . . ? C32 C26 N3 Fe1 4.7(7) . . . . ? C32 C27 C28 C29 -1.9(7) . . . . ? C32 C27 C28 C37 171.7(4) . . . . ? C32 C27 O2 Fe1 -21.5(6) . . . . ? C33 C30 C31 C32 -176.7(5) . . . . ? C37 C28 C29 C30 -174.1(5) . . . . ? C38 C39 C40 C41 1.0(8) . . . . ? C38 C43 C44 C45 -91.2(6) . . . . ? C39 C38 C43 C42 0.2(8) . . . . ? C39 C38 C43 C44 175.7(5) . . . . ? C39 C38 N4 C37 -18.5(8) . . . . ? C39 C40 C41 C42 -0.7(9) . . . . ? C40 C41 C42 C43 0.1(10) . . . . ? C41 C42 C43 C38 0.1(9) . . . . ? C41 C42 C43 C44 -175.6(6) . . . . ? C42 C43 C44 C45 84.2(6) . . . . ? C43 C38 C39 C40 -0.8(8) . . . . ? C43 C38 N4 C37 158.7(5) . . . . ? C43 C44 C45 C46 63.7(6) . . . . ? C44 C45 C46 C47 -81.8(7) . . . . ? C44 C45 C46 C51 98.4(6) . . . . ? C45 C46 C47 C48 177.8(6) . . . . ? C45 C46 C51 C50 -178.1(5) . . . . ? C45 C46 C51 N1 2.0(8) . . . . ? C46 C47 C48 C49 1.1(10) . . . . ? C46 C51 N1 C52 98.4(6) . . . . ? C46 C51 N1 Fe1 -86.9(5) . . . . ? C47 C46 C51 C50 2.0(8) . . . . ? C47 C46 C51 N1 -177.8(5) . . . . ? C47 C48 C49 C50 0.6(10) . . . . ? C48 C49 C50 C51 -0.8(10) . . . . ? C49 C50 C51 C46 -0.5(9) . . . . ? C49 C50 C51 N1 179.4(5) . . . . ? C50 C51 N1 C52 -81.5(6) . . . . ? C50 C51 N1 Fe1 93.2(5) . . . . ? C51 C46 C47 C48 -2.4(9) . . . . ? C52 C2 C3 C4 177.7(5) . . . . ? N2 C12 C13 C14 178.1(4) . . . . ? N2 C12 C17 C16 -178.0(4) . . . . ? N2 C12 C17 C18 -1.7(7) . . . . ? N3 C26 C32 C27 3.8(8) . . . . ? N3 C26 C32 C31 -173.1(5) . . . . ? N4 C38 C39 C40 176.3(5) . . . . ? N4 C38 C43 C42 -177.0(5) . . . . ? N4 C38 C43 C44 -1.5(8) . . . . ? O1 C1 C2 C3 -177.4(4) . . . . ? O1 C1 C2 C52 3.8(7) . . . . ? O1 C1 C6 C5 178.3(4) . . . . ? O1 C1 C6 C11 -8.9(7) . . . . ? O2 C27 C28 C29 179.5(4) . . . . ? O2 C27 C28 C37 -6.9(7) . . . . ? O2 C27 C32 C26 4.5(7) . . . . ? O2 C27 C32 C31 -178.7(4) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.840(5) 2 0.160(5)