# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Sm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H42 Br2 F36 N4 O18 Sm2' _chemical_formula_weight 2227.48 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' 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7392(9) _cell_length_b 19.3831(15) _cell_length_c 34.180(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.5120(10) _cell_angle_gamma 90.00 _cell_volume 7691.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 24958 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Darkgreen _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 2.705 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.721 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57249 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13502 _reflns_number_gt 12468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13502 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.327788(14) 0.272924(9) 0.445831(5) 0.01647(7) Uani 1 1 d . . . Sm2 Sm 0.286252(15) 0.246789(9) 0.197128(5) 0.01886(7) Uani 1 1 d . . . Br2 Br -0.08059(3) 0.29713(2) 0.342216(14) 0.03769(12) Uani 1 1 d . . . Br1 Br 0.72665(3) 0.34253(2) 0.532017(13) 0.03412(11) Uani 1 1 d . . . O11 O 0.3851(2) 0.19613(13) 0.25830(7) 0.0212(5) Uani 1 1 d . . . O4 O 0.3058(2) 0.19170(13) 0.49757(7) 0.0238(6) Uani 1 1 d . . . O15 O 0.2580(2) 0.32651(13) 0.24803(7) 0.0243(6) Uani 1 1 d . . . O8 O 0.1329(2) 0.23557(13) 0.43478(8) 0.0264(6) Uani 1 1 d . . . O6 O 0.4602(2) 0.36868(12) 0.45103(7) 0.0198(5) Uani 1 1 d . . . O14 O 0.4452(2) 0.17756(13) 0.18261(7) 0.0234(5) Uani 1 1 d . . . O7 O 0.3201(2) 0.16454(13) 0.41189(7) 0.0258(6) Uani 1 1 d . . . O5 O 0.5080(2) 0.21844(13) 0.46526(7) 0.0238(6) Uani 1 1 d . . . O17 O 0.1959(2) 0.34626(13) 0.16179(8) 0.0290(6) Uani 1 1 d . . . O2 O 0.2907(2) 0.34143(12) 0.50150(7) 0.0206(5) Uani 1 1 d . . . O9 O 0.2216(2) 0.37189(12) 0.41949(7) 0.0202(5) Uani 1 1 d . . . N2 N 0.2500(2) 0.32991(15) 0.53426(8) 0.0188(6) Uani 1 1 d . . . O10 O 0.3674(2) 0.29350(12) 0.38007(7) 0.0195(5) Uani 1 1 d . . . O13 O 0.2284(2) 0.13001(13) 0.19752(7) 0.0242(6) Uani 1 1 d . . . O3 O 0.7675(2) 0.21507(14) 0.58060(9) 0.0340(7) Uani 1 1 d . . . F13 F 0.6007(2) 0.48571(15) 0.48107(7) 0.0496(7) Uani 1 1 d . . . N3 N 0.4078(2) 0.26736(14) 0.35045(8) 0.0159(6) Uani 1 1 d . . . F28 F 0.2528(2) 0.40752(12) 0.31546(7) 0.0363(6) Uani 1 1 d . . . F16 F 0.1707(2) 0.53436(13) 0.37883(8) 0.0463(7) Uani 1 1 d . . . N4 N 0.4163(2) 0.22058(14) 0.29319(8) 0.0168(6) Uani 1 1 d . . . O18 O 0.4285(2) 0.33269(13) 0.19482(8) 0.0256(6) Uani 1 1 d . . . O12 O -0.1213(2) 0.15970(15) 0.30252(8) 0.0305(6) Uani 1 1 d . . . C39 C 0.0280(3) 0.2371(2) 0.32490(11) 0.0235(8) Uani 1 1 d . . . C21 C 0.0833(3) 0.1791(2) 0.42517(12) 0.0298(9) Uani 1 1 d . . . C36 C 0.3447(3) 0.23476(18) 0.31981(10) 0.0182(7) Uani 1 1 d . . . C35 C 0.5412(3) 0.22959(17) 0.31023(10) 0.0177(7) Uani 1 1 d . . . F19 F 0.5973(2) 0.02890(13) 0.16544(8) 0.0431(6) Uani 1 1 d . . . F12 F -0.0882(2) 0.23463(14) 0.43825(9) 0.0519(8) Uani 1 1 d . . . F4 F 0.6970(2) 0.08596(15) 0.50002(8) 0.0573(8) Uani 1 1 d . . . C13 C 0.6200(3) 0.29273(19) 0.55729(11) 0.0227(8) Uani 1 1 d . . . F14 F 0.6506(2) 0.43131(13) 0.43270(9) 0.0506(7) Uani 1 1 d . . . C23 C 0.2447(3) 0.11865(19) 0.40409(11) 0.0271(8) Uani 1 1 d . . . F24 F 0.0921(2) 0.02031(15) 0.18131(10) 0.0625(8) Uani 1 1 d . . . C29 C 0.5672(3) 0.46930(19) 0.44400(11) 0.0246(8) Uani 1 1 d . . . F15 F 0.5631(2) 0.52764(13) 0.42297(9) 0.0564(8) Uani 1 1 d . . . F1 F 0.2589(2) 0.12885(13) 0.56434(8) 0.0451(7) Uani 1 1 d . . . F21 F 0.6049(2) 0.12748(14) 0.13838(7) 0.0474(7) Uani 1 1 d . . . C32 C 0.5291(3) 0.28302(18) 0.34328(10) 0.0176(7) Uani 1 1 d . . . F8 F 0.2087(2) 0.00989(13) 0.37084(8) 0.0507(7) Uani 1 1 d . . . C9 C 0.4656(3) 0.2243(2) 0.59704(12) 0.0269(9) Uani 1 1 d . . . H9 H 0.4143 0.2019 0.6110 0.032 Uiso 1 1 calc R . . C38 C 0.1434(3) 0.25651(18) 0.33062(11) 0.0217(8) Uani 1 1 d . . . H38 H 0.1666 0.2967 0.3444 0.026 Uiso 1 1 calc R . . F5 F 0.6582(3) 0.11649(16) 0.43951(8) 0.0583(8) Uani 1 1 d . . . F3 F 0.2119(3) 0.06210(16) 0.51460(9) 0.0670(9) Uani 1 1 d . . . F33 F 0.1659(3) 0.51525(16) 0.12774(12) 0.0884(12) Uani 1 1 d . . . F32 F 0.0781(2) 0.42560(15) 0.10276(8) 0.0501(7) Uani 1 1 d . . . F29 F 0.2773(3) 0.46500(13) 0.26331(7) 0.0517(7) Uani 1 1 d . . . C6 C 0.1343(3) 0.35846(18) 0.54006(11) 0.0208(8) Uani 1 1 d . . . C7 C 0.3074(3) 0.30128(19) 0.56685(10) 0.0200(8) Uani 1 1 d . . . F35 F 0.5332(2) 0.50230(13) 0.20080(9) 0.0527(7) Uani 1 1 d . . . F36 F 0.6191(2) 0.41791(16) 0.17846(11) 0.0681(9) Uani 1 1 d . . . F9 F 0.3603(3) 0.06506(13) 0.36188(8) 0.0558(8) Uani 1 1 d . . . F30 F 0.1126(2) 0.46550(14) 0.28340(8) 0.0551(7) Uani 1 1 d . . . F31 F 0.0490(3) 0.46154(18) 0.15884(9) 0.0692(9) Uani 1 1 d . . . F22 F 0.2365(3) -0.04849(14) 0.18842(11) 0.0690(10) Uani 1 1 d . . . F20 F 0.66096(19) 0.11517(15) 0.20081(8) 0.0506(7) Uani 1 1 d . . . C26 C 0.2465(3) 0.43287(19) 0.41370(10) 0.0227(8) Uani 1 1 d . . . C8 C 0.4280(3) 0.27997(19) 0.57290(10) 0.0214(8) Uani 1 1 d . . . C28 C 0.4518(3) 0.42981(18) 0.43809(10) 0.0206(7) Uani 1 1 d . . . C42 C 0.0743(3) 0.1340(2) 0.29175(11) 0.0254(8) Uani 1 1 d . . . H42 H 0.0525 0.0922 0.2795 0.030 Uiso 1 1 calc R . . F23 F 0.1885(3) 0.00513(15) 0.23757(9) 0.0595(8) Uani 1 1 d . . . F2 F 0.3666(3) 0.04395(15) 0.55487(9) 0.0642(9) Uani 1 1 d . . . C16 C 0.3626(3) 0.13954(19) 0.51014(11) 0.0261(8) Uani 1 1 d . . . O16 O 0.0861(2) 0.24694(13) 0.20384(8) 0.0281(6) Uani 1 1 d . . . C58 C 0.5825(3) 0.0960(2) 0.17092(11) 0.0283(9) Uani 1 1 d . . . C17 C 0.4736(3) 0.1212(2) 0.50395(11) 0.0296(9) Uani 1 1 d . . . H17 H 0.5060 0.0805 0.5149 0.035 Uiso 1 1 calc R . . C55 C 0.2751(3) 0.07280(19) 0.19293(11) 0.0247(8) Uani 1 1 d . . . C47 C 0.0233(3) 0.2912(2) 0.21639(12) 0.0293(9) Uani 1 1 d . . . C43 C 0.1878(3) 0.15472(19) 0.29588(10) 0.0224(8) Uani 1 1 d . . . H43 H 0.2413 0.1278 0.2853 0.027 Uiso 1 1 calc R . . C19 C 0.6580(4) 0.1386(2) 0.47659(14) 0.0391(10) Uani 1 1 d . . . F26 F -0.1313(3) 0.24913(18) 0.16996(10) 0.0680(10) Uani 1 1 d . . . C12 C 0.6568(3) 0.2347(2) 0.57995(12) 0.0270(9) Uani 1 1 d . . . C56 C 0.3846(3) 0.0610(2) 0.18366(11) 0.0284(9) Uani 1 1 d . . . H56 H 0.4077 0.0158 0.1802 0.034 Uiso 1 1 calc R . . C57 C 0.4601(3) 0.11355(19) 0.17949(10) 0.0231(8) Uani 1 1 d . . . C33 C 0.6090(3) 0.2536(2) 0.27823(11) 0.0255(8) Uani 1 1 d . . . H33A H 0.6145 0.2165 0.2599 0.038 Uiso 1 1 calc R . . H33B H 0.6849 0.2672 0.2901 0.038 Uiso 1 1 calc R . . H33C H 0.5705 0.2921 0.2644 0.038 Uiso 1 1 calc R . . C48 C -0.1067(4) 0.2771(3) 0.20494(14) 0.0420(11) Uani 1 1 d . . . C54 C 0.1984(3) 0.0111(2) 0.19908(14) 0.0360(10) Uani 1 1 d . . . C30 C 0.6112(3) 0.2724(2) 0.38151(11) 0.0277(9) Uani 1 1 d . . . H30A H 0.5973 0.3070 0.4003 0.041 Uiso 1 1 calc R . . H30B H 0.6892 0.2761 0.3764 0.041 Uiso 1 1 calc R . . H30C H 0.5991 0.2275 0.3920 0.041 Uiso 1 1 calc R . . C46 C 0.0564(3) 0.3491(2) 0.23936(12) 0.0324(9) Uani 1 1 d . . . H46 H 0.0005 0.3798 0.2452 0.039 Uiso 1 1 calc R . . C22 C 0.1302(3) 0.1209(2) 0.40988(12) 0.0334(9) Uani 1 1 d . . . H22 H 0.0837 0.0826 0.4034 0.040 Uiso 1 1 calc R . . C31 C 0.5285(3) 0.35750(19) 0.32959(12) 0.0267(8) Uani 1 1 d . . . H31A H 0.4785 0.3620 0.3048 0.040 Uiso 1 1 calc R . . H31B H 0.6052 0.3710 0.3263 0.040 Uiso 1 1 calc R . . H31C H 0.5014 0.3866 0.3490 0.040 Uiso 1 1 calc R . . F6 F 0.7331(2) 0.18914(16) 0.48288(12) 0.0739(11) Uani 1 1 d . . . C14 C 0.5074(3) 0.31456(19) 0.55299(10) 0.0219(8) Uani 1 1 d . . . H14 H 0.4840 0.3522 0.5369 0.026 Uiso 1 1 calc R . . F27 F -0.1692(2) 0.33469(18) 0.20344(12) 0.0822(11) Uani 1 1 d . . . C27 C 0.3547(3) 0.46469(19) 0.42052(11) 0.0248(8) Uani 1 1 d . . . H27 H 0.3614 0.5105 0.4131 0.030 Uiso 1 1 calc R . . C53 C 0.5415(4) 0.4332(2) 0.20171(13) 0.0353(10) Uani 1 1 d . . . C45 C 0.1702(3) 0.3618(2) 0.25351(11) 0.0274(9) Uani 1 1 d . . . F7 F 0.3511(2) 0.01614(14) 0.41757(9) 0.0559(7) Uani 1 1 d . . . C52 C 0.4267(3) 0.39762(19) 0.18759(11) 0.0271(8) Uani 1 1 d . . . C10 C 0.5787(3) 0.2018(2) 0.60054(12) 0.0294(9) Uani 1 1 d . . . H10 H 0.6025 0.1644 0.6168 0.035 Uiso 1 1 calc R . . C49 C 0.1305(4) 0.4534(2) 0.13567(13) 0.0405(11) Uani 1 1 d . . . F17 F 0.0962(3) 0.50126(17) 0.42876(10) 0.0717(10) Uani 1 1 d . . . F34 F 0.5820(3) 0.41692(16) 0.23780(9) 0.0771(11) Uani 1 1 d . . . C4 C 0.1548(3) 0.4344(2) 0.55056(14) 0.0375(11) Uani 1 1 d . . . H4A H 0.2074 0.4381 0.5748 0.056 Uiso 1 1 calc R . . H4B H 0.0830 0.4558 0.5537 0.056 Uiso 1 1 calc R . . H4C H 0.1869 0.4571 0.5297 0.056 Uiso 1 1 calc R . . F11 F -0.1105(2) 0.14535(19) 0.40314(13) 0.0922(14) Uani 1 1 d . . . C11 C 0.7980(4) 0.1467(2) 0.59515(15) 0.0431(11) Uani 1 1 d . . . H11A H 0.7400 0.1146 0.5839 0.065 Uiso 1 1 calc R . . H11B H 0.8034 0.1462 0.6234 0.065 Uiso 1 1 calc R . . H11C H 0.8709 0.1339 0.5878 0.065 Uiso 1 1 calc R . . C18 C 0.5366(3) 0.1628(2) 0.48171(11) 0.0273(8) Uani 1 1 d . . . F25 F -0.1434(3) 0.2366(2) 0.23053(11) 0.0924(14) Uani 1 1 d . . . C44 C 0.2018(4) 0.4253(2) 0.27925(12) 0.0343(10) Uani 1 1 d . . . C51 C 0.3363(4) 0.4364(2) 0.16862(12) 0.0326(9) Uani 1 1 d . . . H51 H 0.3480 0.4829 0.1638 0.039 Uiso 1 1 calc R . . F18 F 0.0652(2) 0.44491(16) 0.37460(12) 0.0837(12) Uani 1 1 d . . . C5 C 0.0487(3) 0.3501(2) 0.50241(11) 0.0332(10) Uani 1 1 d . . . H5A H 0.0720 0.3784 0.4819 0.050 Uiso 1 1 calc R . . H5B H -0.0264 0.3641 0.5073 0.050 Uiso 1 1 calc R . . H5C H 0.0465 0.3027 0.4943 0.050 Uiso 1 1 calc R . . C40 C -0.0076(3) 0.1753(2) 0.30585(11) 0.0238(8) Uani 1 1 d . . . C50 C 0.2270(4) 0.4071(2) 0.15647(12) 0.0314(9) Uani 1 1 d . . . F10 F -0.0461(3) 0.1373(2) 0.46497(13) 0.1058(16) Uani 1 1 d . . . C25 C 0.1439(3) 0.4783(2) 0.39793(14) 0.0369(10) Uani 1 1 d . . . C37 C 0.2232(3) 0.21555(18) 0.31575(10) 0.0181(7) Uani 1 1 d . . . C15 C 0.2999(4) 0.0926(2) 0.53632(13) 0.0388(10) Uani 1 1 d . . . C24 C 0.2903(4) 0.0520(2) 0.38805(13) 0.0363(10) Uani 1 1 d . . . C20 C -0.0423(4) 0.1741(2) 0.43294(15) 0.0426(11) Uani 1 1 d . . . C41 C -0.1591(3) 0.0999(2) 0.27976(13) 0.0365(10) Uani 1 1 d . . . H41A H -0.1372 0.1038 0.2539 0.055 Uiso 1 1 calc R . . H41B H -0.2414 0.0962 0.2774 0.055 Uiso 1 1 calc R . . H41C H -0.1242 0.0595 0.2927 0.055 Uiso 1 1 calc R . . C34 C 0.5838(3) 0.15890(19) 0.32628(11) 0.0255(8) Uani 1 1 d . . . H34A H 0.5424 0.1456 0.3473 0.038 Uiso 1 1 calc R . . H34B H 0.6646 0.1615 0.3362 0.038 Uiso 1 1 calc R . . H34C H 0.5712 0.1254 0.3054 0.038 Uiso 1 1 calc R . . O1 O 0.2567(2) 0.27214(16) 0.62822(8) 0.0356(7) Uani 1 1 d . . . N1 N 0.2325(2) 0.29650(17) 0.59307(8) 0.0237(7) Uani 1 1 d . . . C3 C 0.1113(3) 0.3130(2) 0.57541(11) 0.0234(8) Uani 1 1 d . . . C1 C 0.0474(3) 0.3484(2) 0.60533(11) 0.0360(10) Uani 1 1 d . . . H1A H 0.0928 0.3862 0.6173 0.054 Uiso 1 1 calc R . . H1B H 0.0343 0.3160 0.6254 0.054 Uiso 1 1 calc R . . H1C H -0.0251 0.3655 0.5922 0.054 Uiso 1 1 calc R . . C2 C 0.0540(3) 0.2438(2) 0.56248(13) 0.0321(10) Uani 1 1 d . . . H2A H -0.0260 0.2512 0.5527 0.048 Uiso 1 1 calc R . . H2B H 0.0611 0.2129 0.5847 0.048 Uiso 1 1 calc R . . H2C H 0.0912 0.2239 0.5419 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01755(10) 0.01680(11) 0.01553(11) -0.00122(7) 0.00398(8) -0.00069(7) Sm2 0.02030(11) 0.02039(11) 0.01587(11) -0.00188(7) 0.00257(8) -0.00087(7) Br2 0.01783(18) 0.0432(3) 0.0522(3) -0.0208(2) 0.00592(18) 0.00186(17) Br1 0.01930(18) 0.0337(2) 0.0508(3) 0.01048(19) 0.01000(18) -0.00146(16) O11 0.0230(12) 0.0247(14) 0.0155(13) -0.0046(10) 0.0020(10) -0.0008(10) O4 0.0283(13) 0.0222(14) 0.0214(14) 0.0033(11) 0.0050(11) -0.0004(11) O15 0.0257(13) 0.0244(14) 0.0233(14) -0.0011(11) 0.0051(11) 0.0047(11) O8 0.0232(13) 0.0258(14) 0.0309(16) -0.0028(11) 0.0062(12) -0.0042(11) O6 0.0228(12) 0.0192(13) 0.0175(13) -0.0016(10) 0.0033(10) -0.0008(10) O14 0.0223(12) 0.0262(14) 0.0218(14) -0.0051(11) 0.0038(11) -0.0011(11) O7 0.0300(13) 0.0221(14) 0.0263(15) -0.0057(11) 0.0072(12) -0.0040(11) O5 0.0227(13) 0.0229(14) 0.0258(14) -0.0008(11) 0.0038(11) 0.0024(11) O17 0.0301(14) 0.0270(15) 0.0289(15) 0.0031(12) 0.0011(12) 0.0017(12) O2 0.0236(12) 0.0245(13) 0.0150(13) -0.0008(10) 0.0071(11) 0.0017(10) O9 0.0213(12) 0.0199(13) 0.0201(13) 0.0029(10) 0.0054(10) 0.0017(10) N2 0.0196(14) 0.0225(16) 0.0153(15) -0.0026(12) 0.0059(12) -0.0013(12) O10 0.0213(12) 0.0244(13) 0.0138(12) -0.0026(10) 0.0060(10) -0.0008(10) O13 0.0228(12) 0.0265(14) 0.0230(14) -0.0054(11) 0.0023(11) -0.0013(11) O3 0.0227(13) 0.0333(16) 0.0461(18) 0.0129(14) 0.0057(13) 0.0066(12) F13 0.0431(14) 0.0687(19) 0.0364(15) -0.0188(13) 0.0041(12) -0.0247(14) N3 0.0193(14) 0.0171(14) 0.0115(15) -0.0017(11) 0.0023(12) -0.0020(11) F28 0.0495(14) 0.0323(13) 0.0269(13) -0.0042(10) 0.0047(11) -0.0014(11) F16 0.0424(14) 0.0367(14) 0.0595(17) 0.0237(13) 0.0069(13) 0.0114(12) N4 0.0184(14) 0.0198(15) 0.0120(15) -0.0020(11) 0.0017(12) 0.0015(12) O18 0.0255(13) 0.0254(14) 0.0258(14) -0.0017(11) 0.0040(11) -0.0007(11) O12 0.0166(12) 0.0436(17) 0.0307(16) -0.0125(13) 0.0015(12) -0.0074(12) C39 0.0171(17) 0.032(2) 0.021(2) -0.0012(16) 0.0043(16) 0.0045(15) C21 0.0235(19) 0.035(2) 0.030(2) -0.0018(18) 0.0003(17) -0.0067(17) C36 0.0180(17) 0.0232(18) 0.0132(18) 0.0023(14) 0.0017(14) -0.0003(14) C35 0.0151(16) 0.0183(18) 0.0193(19) -0.0007(14) 0.0009(15) -0.0013(13) F19 0.0381(13) 0.0332(14) 0.0614(17) -0.0043(12) 0.0183(13) 0.0119(11) F12 0.0269(13) 0.0518(17) 0.078(2) -0.0128(15) 0.0110(14) -0.0029(12) F4 0.0555(16) 0.0589(18) 0.0591(19) 0.0182(15) 0.0135(15) 0.0331(15) C13 0.0214(17) 0.0231(19) 0.024(2) -0.0001(15) 0.0061(16) -0.0039(15) F14 0.0330(13) 0.0358(14) 0.089(2) -0.0206(14) 0.0276(14) -0.0112(11) C23 0.037(2) 0.021(2) 0.022(2) -0.0015(15) 0.0023(17) -0.0041(17) F24 0.0352(14) 0.0476(17) 0.098(2) 0.0077(16) -0.0123(15) -0.0167(13) C29 0.0262(18) 0.0198(19) 0.028(2) 0.0000(16) 0.0047(16) -0.0041(15) F15 0.0397(14) 0.0374(15) 0.087(2) 0.0305(15) -0.0093(14) -0.0174(12) F1 0.0544(16) 0.0400(15) 0.0465(16) 0.0089(12) 0.0255(14) -0.0037(13) F21 0.0433(14) 0.0568(17) 0.0485(16) 0.0209(13) 0.0274(13) 0.0221(13) C32 0.0182(16) 0.0230(18) 0.0125(18) -0.0009(14) 0.0047(14) -0.0033(14) F8 0.0540(15) 0.0309(14) 0.0656(19) -0.0234(13) 0.0032(14) -0.0089(12) C9 0.0242(19) 0.034(2) 0.024(2) 0.0023(16) 0.0076(17) -0.0027(16) C38 0.0201(18) 0.0233(19) 0.020(2) -0.0009(14) -0.0019(16) -0.0008(15) F5 0.0679(19) 0.065(2) 0.0471(17) 0.0048(14) 0.0263(15) 0.0369(16) F3 0.079(2) 0.0563(19) 0.063(2) 0.0114(15) 0.0010(17) -0.0423(17) F33 0.078(2) 0.0418(18) 0.131(3) 0.040(2) -0.033(2) -0.0033(17) F32 0.0488(15) 0.0580(18) 0.0393(15) -0.0003(13) -0.0074(13) 0.0178(14) F29 0.087(2) 0.0285(13) 0.0427(16) -0.0041(12) 0.0212(15) -0.0140(14) C6 0.0199(17) 0.0223(19) 0.0217(19) 0.0010(15) 0.0077(15) 0.0017(15) C7 0.0196(17) 0.028(2) 0.0124(18) -0.0030(14) 0.0039(14) -0.0037(15) F35 0.0505(15) 0.0240(13) 0.083(2) -0.0002(13) 0.0083(15) -0.0072(12) F36 0.0387(15) 0.064(2) 0.107(3) -0.0375(19) 0.0303(17) -0.0124(14) F9 0.0732(19) 0.0344(15) 0.069(2) -0.0217(13) 0.0401(17) -0.0043(14) F30 0.0656(18) 0.0460(16) 0.0526(17) -0.0165(13) 0.0051(14) 0.0273(15) F31 0.0671(19) 0.084(2) 0.0580(19) -0.0012(17) 0.0129(17) 0.0444(18) F22 0.0598(18) 0.0259(14) 0.131(3) -0.0235(16) 0.047(2) -0.0104(13) F20 0.0236(12) 0.075(2) 0.0496(17) -0.0176(14) -0.0080(11) 0.0100(13) C26 0.0249(18) 0.027(2) 0.0167(19) -0.0003(15) 0.0049(15) 0.0066(15) C8 0.0225(18) 0.030(2) 0.0120(18) -0.0025(15) 0.0025(15) -0.0002(15) C28 0.0242(18) 0.0218(19) 0.0168(18) -0.0027(14) 0.0065(15) -0.0030(15) C42 0.0237(18) 0.027(2) 0.026(2) -0.0064(16) 0.0033(16) -0.0053(16) F23 0.074(2) 0.0508(18) 0.0577(19) 0.0055(14) 0.0236(16) -0.0159(15) F2 0.073(2) 0.0463(17) 0.079(2) 0.0383(16) 0.0296(18) 0.0167(15) C16 0.038(2) 0.0177(18) 0.022(2) 0.0018(15) 0.0031(17) -0.0022(16) O16 0.0237(14) 0.0296(15) 0.0322(16) -0.0024(12) 0.0078(13) 0.0018(11) C58 0.0269(19) 0.031(2) 0.027(2) 0.0003(17) 0.0031(17) 0.0083(17) C17 0.038(2) 0.0200(19) 0.031(2) 0.0042(16) 0.0057(18) 0.0060(17) C55 0.0293(19) 0.0204(19) 0.023(2) -0.0030(15) -0.0020(16) 0.0013(15) C47 0.0259(19) 0.037(2) 0.025(2) 0.0096(18) 0.0053(17) 0.0024(18) C43 0.0233(17) 0.027(2) 0.0175(19) -0.0015(15) 0.0061(15) -0.0014(15) C19 0.036(2) 0.034(2) 0.047(3) 0.004(2) 0.007(2) 0.011(2) F26 0.0346(16) 0.105(3) 0.060(2) -0.0202(18) -0.0062(15) 0.0082(16) C12 0.0182(18) 0.031(2) 0.031(2) -0.0010(17) 0.0026(17) 0.0017(15) C56 0.0290(19) 0.023(2) 0.033(2) -0.0056(16) 0.0040(17) 0.0040(16) C57 0.0240(18) 0.029(2) 0.0154(18) -0.0030(15) 0.0003(15) 0.0063(16) C33 0.0210(18) 0.036(2) 0.021(2) -0.0030(16) 0.0066(17) -0.0056(16) C48 0.028(2) 0.056(3) 0.040(3) 0.001(2) -0.001(2) 0.009(2) C54 0.027(2) 0.028(2) 0.054(3) -0.002(2) 0.009(2) -0.0013(17) C30 0.0216(18) 0.041(2) 0.020(2) -0.0057(17) 0.0000(16) -0.0005(16) C46 0.030(2) 0.033(2) 0.037(2) 0.0014(18) 0.0128(19) 0.0123(18) C22 0.033(2) 0.028(2) 0.041(2) -0.0049(18) 0.0105(19) -0.0135(18) C31 0.0268(18) 0.024(2) 0.031(2) -0.0028(16) 0.0108(17) -0.0068(16) F6 0.0297(14) 0.0506(19) 0.144(3) -0.015(2) 0.0229(18) 0.0075(13) C14 0.0225(17) 0.0221(18) 0.021(2) -0.0006(15) 0.0025(15) 0.0006(15) F27 0.0353(15) 0.081(2) 0.126(3) -0.025(2) -0.0048(18) 0.0270(16) C27 0.0277(19) 0.0199(19) 0.027(2) 0.0000(15) 0.0042(16) -0.0005(15) C53 0.042(2) 0.026(2) 0.038(3) 0.0016(18) 0.007(2) -0.0020(18) C45 0.038(2) 0.026(2) 0.019(2) 0.0032(15) 0.0070(17) 0.0088(17) F7 0.0662(18) 0.0316(14) 0.0643(19) -0.0059(13) -0.0086(15) 0.0155(13) C52 0.036(2) 0.024(2) 0.023(2) 0.0000(16) 0.0114(17) -0.0028(17) C10 0.0235(19) 0.033(2) 0.031(2) 0.0100(18) 0.0047(17) 0.0052(17) C49 0.049(3) 0.035(2) 0.038(3) 0.004(2) 0.007(2) 0.005(2) F17 0.0661(19) 0.073(2) 0.086(2) 0.0277(18) 0.0460(19) 0.0446(18) F34 0.095(2) 0.066(2) 0.0570(19) 0.0311(16) -0.0335(18) -0.0551(19) C4 0.034(2) 0.022(2) 0.060(3) -0.0038(19) 0.021(2) 0.0004(17) F11 0.0327(15) 0.090(3) 0.152(4) -0.071(3) 0.0069(19) -0.0193(16) C11 0.032(2) 0.039(3) 0.059(3) 0.010(2) 0.008(2) 0.008(2) C18 0.0278(19) 0.028(2) 0.025(2) -0.0063(16) 0.0017(17) 0.0038(16) F25 0.0367(17) 0.151(4) 0.086(3) 0.060(3) -0.0024(18) -0.028(2) C44 0.047(2) 0.030(2) 0.028(2) 0.0015(18) 0.012(2) 0.0078(19) C51 0.043(2) 0.024(2) 0.030(2) 0.0036(17) 0.0040(19) -0.0021(18) F18 0.0470(16) 0.0450(18) 0.139(3) 0.0235(19) -0.0513(19) 0.0001(14) C5 0.0198(18) 0.056(3) 0.025(2) 0.0084(19) 0.0070(17) 0.0027(18) C40 0.0176(17) 0.033(2) 0.020(2) -0.0007(16) 0.0024(15) -0.0046(16) C50 0.038(2) 0.029(2) 0.027(2) 0.0026(17) 0.0055(18) 0.0046(18) F10 0.0496(19) 0.122(3) 0.160(4) 0.089(3) 0.061(2) 0.029(2) C25 0.032(2) 0.028(2) 0.050(3) 0.006(2) 0.006(2) 0.0065(18) C37 0.0176(16) 0.0223(18) 0.0138(17) 0.0003(14) 0.0007(14) -0.0007(14) C15 0.048(3) 0.031(2) 0.038(3) 0.0120(19) 0.006(2) -0.001(2) C24 0.046(2) 0.025(2) 0.039(3) -0.0077(18) 0.010(2) -0.0044(19) C20 0.031(2) 0.037(3) 0.061(3) -0.011(2) 0.012(2) -0.010(2) C41 0.0220(19) 0.042(3) 0.044(3) -0.010(2) 0.0003(18) -0.0080(18) C34 0.0238(18) 0.024(2) 0.028(2) -0.0001(16) 0.0007(16) 0.0045(15) O1 0.0251(14) 0.066(2) 0.0156(15) 0.0094(13) 0.0040(12) 0.0042(14) N1 0.0203(15) 0.0373(19) 0.0132(16) -0.0003(13) 0.0010(13) -0.0019(14) C3 0.0178(17) 0.031(2) 0.022(2) -0.0004(16) 0.0032(15) -0.0016(15) C1 0.0258(19) 0.061(3) 0.023(2) 0.000(2) 0.0102(18) 0.007(2) C2 0.0191(19) 0.030(2) 0.045(3) 0.0100(18) -0.0008(19) -0.0061(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O5 2.370(2) . ? Sm1 O8 2.376(3) . ? Sm1 O9 2.390(2) . ? Sm1 O7 2.395(2) . ? Sm1 O10 2.395(2) . ? Sm1 O4 2.410(2) . ? Sm1 O6 2.410(2) . ? Sm1 O2 2.412(2) . ? Sm2 O1 2.358(3) 4_565 ? Sm2 O13 2.364(3) . ? Sm2 O18 2.367(2) . ? Sm2 O15 2.387(2) . ? Sm2 O16 2.394(3) . ? Sm2 O14 2.409(2) . ? Sm2 O17 2.433(3) . ? Sm2 O11 2.442(2) . ? Br2 C39 1.885(4) . ? Br1 C13 1.888(3) . ? O11 N4 1.285(4) . ? O4 C16 1.252(4) . ? O15 C45 1.273(4) . ? O8 C21 1.260(5) . ? O6 C28 1.264(4) . ? O14 C57 1.260(4) . ? O7 C23 1.255(4) . ? O5 C18 1.240(5) . ? O17 C50 1.256(5) . ? O2 N2 1.300(3) . ? O9 C26 1.241(4) . ? N2 C7 1.334(5) . ? N2 C6 1.507(4) . ? O10 N3 1.284(3) . ? O13 C55 1.257(4) . ? O3 C12 1.351(4) . ? O3 C11 1.441(5) . ? F13 C29 1.309(4) . ? N3 C36 1.348(5) . ? N3 C32 1.511(4) . ? F28 C44 1.338(5) . ? F16 C25 1.329(5) . ? N4 C36 1.355(4) . ? N4 C35 1.505(4) . ? O18 C52 1.282(4) . ? O12 C40 1.357(4) . ? O12 C41 1.429(5) . ? C39 C38 1.391(5) . ? C39 C40 1.399(5) . ? C21 C22 1.390(6) . ? C21 C20 1.541(5) . ? C36 C37 1.460(5) . ? C35 C33 1.518(5) . ? C35 C34 1.532(5) . ? C35 C32 1.554(5) . ? F19 C58 1.330(5) . ? F12 C20 1.315(5) . ? F4 C19 1.335(5) . ? C13 C14 1.374(5) . ? C13 C12 1.397(5) . ? F14 C29 1.328(4) . ? C23 C22 1.387(5) . ? C23 C24 1.530(5) . ? F24 C54 1.317(5) . ? C29 F15 1.337(4) . ? C29 C28 1.543(5) . ? F1 C15 1.334(5) . ? F21 C58 1.329(4) . ? C32 C31 1.517(5) . ? C32 C30 1.518(5) . ? F8 C24 1.329(5) . ? C9 C10 1.385(5) . ? C9 C8 1.390(5) . ? C38 C37 1.382(5) . ? F5 C19 1.338(5) . ? F3 C15 1.319(5) . ? F33 C49 1.310(5) . ? F32 C49 1.315(5) . ? F29 C44 1.348(5) . ? C6 C5 1.520(5) . ? C6 C4 1.526(5) . ? C6 C3 1.551(5) . ? C7 N1 1.349(4) . ? C7 C8 1.459(5) . ? F35 C53 1.342(5) . ? F36 C53 1.329(5) . ? F9 C24 1.325(5) . ? F30 C44 1.330(5) . ? F31 C49 1.339(5) . ? F22 C54 1.309(5) . ? F20 C58 1.324(5) . ? C26 C27 1.400(5) . ? C26 C25 1.526(5) . ? C8 C14 1.404(5) . ? C28 C27 1.383(5) . ? C42 C43 1.379(5) . ? C42 C40 1.391(5) . ? F23 C54 1.343(5) . ? F2 C15 1.326(5) . ? C16 C17 1.396(5) . ? C16 C15 1.538(5) . ? O16 C47 1.247(5) . ? C58 C57 1.545(5) . ? C17 C18 1.393(5) . ? C55 C56 1.388(5) . ? C55 C54 1.530(5) . ? C47 C46 1.392(6) . ? C47 C48 1.542(6) . ? C43 C37 1.393(5) . ? C19 F6 1.315(5) . ? C19 C18 1.536(5) . ? F26 C48 1.305(5) . ? C12 C10 1.391(5) . ? C56 C57 1.372(5) . ? C48 F25 1.295(6) . ? C48 F27 1.334(5) . ? C46 C45 1.373(6) . ? C53 F34 1.294(5) . ? C53 C52 1.528(6) . ? C45 C44 1.527(6) . ? F7 C24 1.341(5) . ? C52 C51 1.380(6) . ? C49 C50 1.534(6) . ? F17 C25 1.340(5) . ? F11 C20 1.322(6) . ? C51 C50 1.409(6) . ? F18 C25 1.300(5) . ? F10 C20 1.312(6) . ? O1 N1 1.283(4) . ? O1 Sm2 2.358(3) 4_566 ? N1 C3 1.496(4) . ? C3 C1 1.519(5) . ? C3 C2 1.536(5) . ? 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 O5 Sm1 O8 135.02(9) . . ? O5 Sm1 O9 149.03(8) . . ? O8 Sm1 O9 75.43(9) . . ? O5 Sm1 O7 73.32(9) . . ? O8 Sm1 O7 71.89(9) . . ? O9 Sm1 O7 122.77(9) . . ? O5 Sm1 O10 92.74(8) . . ? O8 Sm1 O10 102.58(9) . . ? O9 Sm1 O10 71.09(8) . . ? O7 Sm1 O10 71.95(8) . . ? O5 Sm1 O4 72.02(8) . . ? O8 Sm1 O4 73.29(9) . . ? O9 Sm1 O4 133.97(8) . . ? O7 Sm1 O4 77.41(8) . . ? O10 Sm1 O4 148.66(8) . . ? O5 Sm1 O6 77.49(8) . . ? O8 Sm1 O6 147.31(8) . . ? O9 Sm1 O6 72.81(8) . . ? O7 Sm1 O6 133.54(8) . . ? O10 Sm1 O6 74.24(8) . . ? O4 Sm1 O6 125.93(8) . . ? O5 Sm1 O2 106.40(8) . . ? O8 Sm1 O2 90.64(8) . . ? O9 Sm1 O2 73.16(8) . . ? O7 Sm1 O2 150.07(8) . . ? O10 Sm1 O2 137.01(8) . . ? O4 Sm1 O2 74.30(8) . . ? O6 Sm1 O2 73.00(8) . . ? O1 Sm2 O13 81.77(10) 4_565 . ? O1 Sm2 O18 94.37(9) 4_565 . ? O13 Sm2 O18 151.43(8) . . ? O1 Sm2 O15 144.41(10) 4_565 . ? O13 Sm2 O15 123.01(8) . . ? O18 Sm2 O15 75.15(8) . . ? O1 Sm2 O16 95.44(9) 4_565 . ? O13 Sm2 O16 73.37(9) . . ? O18 Sm2 O16 135.17(9) . . ? O15 Sm2 O16 71.64(9) . . ? O1 Sm2 O14 73.22(9) 4_565 . ? O13 Sm2 O14 72.52(8) . . ? O18 Sm2 O14 79.25(8) . . ? O15 Sm2 O14 134.95(8) . . ? O16 Sm2 O14 145.22(9) . . ? O1 Sm2 O17 68.82(10) 4_565 . ? O13 Sm2 O17 131.08(9) . . ? O18 Sm2 O17 71.57(9) . . ? O15 Sm2 O17 75.61(9) . . ? O16 Sm2 O17 71.63(9) . . ? O14 Sm2 O17 129.28(8) . . ? O1 Sm2 O11 140.68(9) 4_565 . ? O13 Sm2 O11 73.17(8) . . ? O18 Sm2 O11 93.63(8) . . ? O15 Sm2 O11 74.68(8) . . ? O16 Sm2 O11 105.48(9) . . ? O14 Sm2 O11 70.62(8) . . ? O17 Sm2 O11 149.37(8) . . ? N4 O11 Sm2 132.9(2) . . ? C16 O4 Sm1 132.1(2) . . ? C45 O15 Sm2 131.1(2) . . ? C21 O8 Sm1 134.7(2) . . ? C28 O6 Sm1 132.9(2) . . ? C57 O14 Sm2 133.5(2) . . ? C23 O7 Sm1 134.3(2) . . ? C18 O5 Sm1 133.3(2) . . ? C50 O17 Sm2 134.5(3) . . ? N2 O2 Sm1 135.8(2) . . ? C26 O9 Sm1 134.6(2) . . ? O2 N2 C7 125.9(3) . . ? O2 N2 C6 120.2(3) . . ? C7 N2 C6 113.4(3) . . ? N3 O10 Sm1 145.1(2) . . ? C55 O13 Sm2 135.5(2) . . ? C12 O3 C11 117.0(3) . . ? O10 N3 C36 125.0(3) . . ? O10 N3 C32 121.0(3) . . ? C36 N3 C32 113.0(3) . . ? O11 N4 C36 125.3(3) . . ? O11 N4 C35 122.0(3) . . ? C36 N4 C35 112.5(3) . . ? C52 O18 Sm2 134.8(2) . . ? C40 O12 C41 116.6(3) . . ? C38 C39 C40 121.0(3) . . ? C38 C39 Br2 118.6(3) . . ? C40 C39 Br2 120.4(3) . . ? O8 C21 C22 127.5(4) . . ? O8 C21 C20 115.3(4) . . ? C22 C21 C20 117.1(4) . . ? N3 C36 N4 107.0(3) . . ? N3 C36 C37 127.6(3) . . ? N4 C36 C37 125.4(3) . . ? N4 C35 C33 110.0(3) . . ? N4 C35 C34 106.4(3) . . ? C33 C35 C34 110.7(3) . . ? N4 C35 C32 99.8(3) . . ? C33 C35 C32 115.7(3) . . ? C34 C35 C32 113.3(3) . . ? C14 C13 C12 121.4(3) . . ? C14 C13 Br1 119.1(3) . . ? C12 C13 Br1 119.6(3) . . ? O7 C23 C22 127.9(4) . . ? O7 C23 C24 113.6(3) . . ? C22 C23 C24 118.4(4) . . ? F13 C29 F14 106.7(3) . . ? F13 C29 F15 107.3(3) . . ? F14 C29 F15 106.4(3) . . ? F13 C29 C28 112.3(3) . . ? F14 C29 C28 111.0(3) . . ? F15 C29 C28 112.9(3) . . ? N3 C32 C31 106.2(3) . . ? N3 C32 C30 109.1(3) . . ? C31 C32 C30 111.6(3) . . ? N3 C32 C35 100.0(3) . . ? C31 C32 C35 114.0(3) . . ? C30 C32 C35 114.9(3) . . ? C10 C9 C8 120.8(3) . . ? C37 C38 C39 119.5(3) . . ? N2 C6 C5 110.2(3) . . ? N2 C6 C4 105.8(3) . . ? C5 C6 C4 111.3(3) . . ? N2 C6 C3 99.1(3) . . ? C5 C6 C3 115.4(3) . . ? C4 C6 C3 113.9(3) . . ? N2 C7 N1 106.5(3) . . ? N2 C7 C8 126.5(3) . . ? N1 C7 C8 126.9(3) . . ? O9 C26 C27 128.5(3) . . ? O9 C26 C25 114.5(3) . . ? C27 C26 C25 117.0(3) . . ? C9 C8 C14 118.9(3) . . ? C9 C8 C7 121.4(3) . . ? C14 C8 C7 119.7(3) . . ? O6 C28 C27 128.8(3) . . ? O6 C28 C29 113.4(3) . . ? C27 C28 C29 117.7(3) . . ? C43 C42 C40 120.2(3) . . ? O4 C16 C17 128.0(3) . . ? O4 C16 C15 113.7(3) . . ? C17 C16 C15 118.4(3) . . ? C47 O16 Sm2 132.2(3) . . ? F20 C58 F21 108.4(3) . . ? F20 C58 F19 107.0(3) . . ? F21 C58 F19 106.5(3) . . ? F20 C58 C57 110.6(3) . . ? F21 C58 C57 111.3(3) . . ? F19 C58 C57 112.8(3) . . ? C18 C17 C16 121.2(4) . . ? O13 C55 C56 127.6(4) . . ? O13 C55 C54 113.4(3) . . ? C56 C55 C54 119.0(3) . . ? O16 C47 C46 128.2(4) . . ? O16 C47 C48 113.8(4) . . ? C46 C47 C48 118.0(4) . . ? C42 C43 C37 120.7(3) . . ? F6 C19 F4 108.0(4) . . ? F6 C19 F5 107.3(4) . . ? F4 C19 F5 106.0(4) . . ? F6 C19 C18 111.4(3) . . ? F4 C19 C18 114.0(3) . . ? F5 C19 C18 109.7(4) . . ? O3 C12 C10 124.5(4) . . ? O3 C12 C13 117.0(3) . . ? C10 C12 C13 118.5(3) . . ? C57 C56 C55 122.4(4) . . ? O14 C57 C56 128.5(3) . . ? O14 C57 C58 112.2(3) . . ? C56 C57 C58 119.3(3) . . ? F25 C48 F26 108.5(5) . . ? F25 C48 F27 107.2(4) . . ? F26 C48 F27 105.4(4) . . ? F25 C48 C47 110.6(4) . . ? F26 C48 C47 112.5(4) . . ? F27 C48 C47 112.3(4) . . ? F22 C54 F24 109.3(4) . . ? F22 C54 F23 106.3(4) . . ? F24 C54 F23 104.4(3) . . ? F22 C54 C55 114.8(3) . . ? F24 C54 C55 111.5(4) . . ? F23 C54 C55 109.8(3) . . ? C45 C46 C47 121.2(4) . . ? C23 C22 C21 121.7(4) . . ? C13 C14 C8 119.9(3) . . ? C28 C27 C26 121.7(3) . . ? F34 C53 F36 109.2(4) . . ? F34 C53 F35 106.3(4) . . ? F36 C53 F35 105.2(3) . . ? F34 C53 C52 111.9(3) . . ? F36 C53 C52 111.2(3) . . ? F35 C53 C52 112.7(4) . . ? O15 C45 C46 128.2(4) . . ? O15 C45 C44 112.6(3) . . ? C46 C45 C44 119.2(3) . . ? O18 C52 C51 127.9(4) . . ? O18 C52 C53 113.2(4) . . ? C51 C52 C53 118.9(3) . . ? C9 C10 C12 120.5(4) . . ? F33 C49 F32 108.7(4) . . ? F33 C49 F31 106.9(4) . . ? F32 C49 F31 105.6(4) . . ? F33 C49 C50 113.4(4) . . ? F32 C49 C50 112.1(4) . . ? F31 C49 C50 109.8(4) . . ? O5 C18 C17 128.4(3) . . ? O5 C18 C19 114.1(3) . . ? C17 C18 C19 117.5(3) . . ? F30 C44 F28 107.7(3) . . ? F30 C44 F29 106.5(3) . . ? F28 C44 F29 106.9(4) . . ? F30 C44 C45 113.9(4) . . ? F28 C44 C45 111.3(3) . . ? F29 C44 C45 110.2(3) . . ? C52 C51 C50 121.5(4) . . ? O12 C40 C42 124.4(3) . . ? O12 C40 C39 116.9(3) . . ? C42 C40 C39 118.7(3) . . ? O17 C50 C51 127.4(4) . . ? O17 C50 C49 114.0(4) . . ? C51 C50 C49 118.6(4) . . ? F18 C25 F16 107.7(4) . . ? F18 C25 F17 107.8(4) . . ? F16 C25 F17 105.8(3) . . ? F18 C25 C26 112.4(4) . . ? F16 C25 C26 114.4(3) . . ? F17 C25 C26 108.3(3) . . ? C38 C37 C43 119.7(3) . . ? C38 C37 C36 121.7(3) . . ? C43 C37 C36 118.6(3) . . ? F3 C15 F2 108.0(4) . . ? F3 C15 F1 107.8(4) . . ? F2 C15 F1 106.3(4) . . ? F3 C15 C16 109.9(4) . . ? F2 C15 C16 113.5(4) . . ? F1 C15 C16 111.1(3) . . ? F9 C24 F8 107.3(3) . . ? F9 C24 F7 107.0(4) . . ? F8 C24 F7 106.4(3) . . ? F9 C24 C23 111.5(3) . . ? F8 C24 C23 114.2(4) . . ? F7 C24 C23 110.1(3) . . ? F10 C20 F12 107.7(4) . . ? F10 C20 F11 108.9(4) . . ? F12 C20 F11 105.6(4) . . ? F10 C20 C21 109.2(4) . . ? F12 C20 C21 112.9(4) . . ? F11 C20 C21 112.3(4) . . ? N1 O1 Sm2 166.4(3) . 4_566 ? O1 N1 C7 124.8(3) . . ? O1 N1 C3 121.5(3) . . ? C7 N1 C3 113.1(3) . . ? N1 C3 C1 111.1(3) . . ? N1 C3 C2 106.2(3) . . ? C1 C3 C2 110.5(3) . . ? N1 C3 C6 99.8(3) . . ? C1 C3 C6 115.3(3) . . ? C2 C3 C6 113.1(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.416 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 958921' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H42 Br2 F36 N4 Nd2 O18' _chemical_formula_weight 2215.26 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' 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' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.721(2) _cell_length_b 19.431(4) _cell_length_c 34.305(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.53(3) _cell_angle_gamma 90.00 _cell_volume 7726(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 16464 _cell_measurement_theta_min 1.5924 _cell_measurement_theta_max 27.9064 _exptl_crystal_description Prism _exptl_crystal_colour Darkgreen _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4304 _exptl_absorpt_coefficient_mu 2.517 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46266 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13555 _reflns_number_gt 11572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13555 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.329207(19) 0.271959(13) 0.946476(7) 0.01872(8) Uani 1 1 d . . . Nd2 Nd 0.28648(2) 0.245730(14) 0.697687(7) 0.02147(8) Uani 1 1 d . . . Br3 Br 0.72560(4) 0.34210(3) 1.032534(18) 0.03853(15) Uani 1 1 d . . . Br4 Br -0.07811(4) 0.29510(3) 0.842977(18) 0.04328(16) Uani 1 1 d . . . O12 O 0.3885(3) 0.19509(18) 0.75913(9) 0.0239(7) Uani 1 1 d . . . O4 O 0.3077(3) 0.19066(18) 0.99884(10) 0.0277(8) Uani 1 1 d . . . O3 O 0.2900(3) 0.34115(18) 1.00230(9) 0.0231(7) Uani 1 1 d . . . O8 O 0.1328(3) 0.23218(19) 0.93518(10) 0.0311(8) Uani 1 1 d . . . O13 O 0.2573(3) 0.32584(19) 0.74897(9) 0.0280(8) Uani 1 1 d . . . O7 O 0.4619(2) 0.36905(17) 0.95126(9) 0.0216(7) Uani 1 1 d . . . N2 N 0.2490(3) 0.3299(2) 1.03475(11) 0.0204(9) Uani 1 1 d . . . O17 O 0.2291(3) 0.12768(18) 0.69797(9) 0.0249(7) Uani 1 1 d . . . O11 O 0.3689(2) 0.29179(17) 0.88037(9) 0.0214(7) Uani 1 1 d . . . O9 O 0.3213(3) 0.16242(18) 0.91226(10) 0.0281(8) Uani 1 1 d . . . N3 N 0.4092(3) 0.2663(2) 0.85071(10) 0.0188(8) Uani 1 1 d . . . C34 C 0.0306(4) 0.2354(3) 0.82538(14) 0.0259(11) Uani 1 1 d . . . N4 N 0.4190(3) 0.2198(2) 0.79408(10) 0.0178(8) Uani 1 1 d . . . F17 F 0.6015(3) 0.4861(2) 0.98081(10) 0.0581(11) Uani 1 1 d . . . O6 O 0.2224(2) 0.37186(18) 0.91960(9) 0.0234(7) Uani 1 1 d . . . O5 O 0.5099(3) 0.21605(18) 0.96670(10) 0.0265(8) Uani 1 1 d . . . O15 O 0.1954(3) 0.3465(2) 0.66201(10) 0.0329(9) Uani 1 1 d . . . O18 O 0.4457(3) 0.17501(19) 0.68286(9) 0.0271(8) Uani 1 1 d . . . C37 C 0.3468(4) 0.2341(2) 0.82041(13) 0.0182(10) Uani 1 1 d . . . O1 O 0.7673(3) 0.2157(2) 1.08165(12) 0.0402(10) Uani 1 1 d . . . O10 O -0.1197(3) 0.1587(2) 0.80259(10) 0.0343(9) Uani 1 1 d . . . O16 O 0.4288(3) 0.33311(19) 0.69509(10) 0.0305(8) Uani 1 1 d . . . F16 F 0.6517(3) 0.43213(19) 0.93291(12) 0.0599(11) Uani 1 1 d . . . N1 N 0.2316(3) 0.2965(2) 1.09349(10) 0.0244(9) Uani 1 1 d . . . F22 F 0.2530(3) 0.40722(18) 0.81603(9) 0.0423(8) Uani 1 1 d . . . C8 C 0.3062(4) 0.3021(3) 1.06733(13) 0.0221(11) Uani 1 1 d . . . F29 F 0.6046(3) 0.1253(2) 0.63860(10) 0.0555(10) Uani 1 1 d . . . C3 C 0.6197(4) 0.2925(3) 1.05837(14) 0.0253(11) Uani 1 1 d . . . F28 F 0.5962(3) 0.02687(18) 0.66493(11) 0.0498(9) Uani 1 1 d . . . C38 C 0.5313(4) 0.2820(3) 0.84395(13) 0.0204(10) Uani 1 1 d . . . F15 F 0.1707(3) 0.5336(2) 0.87920(11) 0.0548(10) Uani 1 1 d . . . C35 C 0.1451(4) 0.2554(3) 0.83109(14) 0.0224(11) Uani 1 1 d . . . H35 H 0.1679 0.2956 0.8447 0.027 Uiso 1 1 calc R . . C41 C 0.5432(4) 0.2293(3) 0.81087(13) 0.0212(10) Uani 1 1 d . . . C11 C 0.0457(4) 0.3482(3) 1.10546(15) 0.0389(15) Uani 1 1 d . . . H11A H 0.0363 0.3167 1.1263 0.058 Uiso 1 1 calc R . . H11B H -0.0287 0.3632 1.0928 0.058 Uiso 1 1 calc R . . H11C H 0.0898 0.3872 1.1162 0.058 Uiso 1 1 calc R . . C26 C 0.2465(4) 0.1167(3) 0.90448(15) 0.0312(12) Uani 1 1 d . . . F1 F 0.2605(3) 0.1286(2) 1.06566(10) 0.0532(10) Uani 1 1 d . . . F18 F 0.5640(3) 0.5274(2) 0.92336(12) 0.0648(11) Uani 1 1 d . . . C20 C 0.5687(4) 0.4690(3) 0.94395(15) 0.0299(12) Uani 1 1 d . . . F5 F 0.6617(3) 0.1166(2) 0.94126(11) 0.0671(12) Uani 1 1 d . . . F3 F 0.3677(4) 0.0435(2) 1.05663(13) 0.0726(13) Uani 1 1 d . . . C12 C 0.1327(4) 0.3582(3) 1.04028(14) 0.0240(11) Uani 1 1 d . . . F33 F 0.1633(4) 0.5150(2) 0.62900(16) 0.1010(18) Uani 1 1 d . . . O14 O 0.0843(3) 0.2473(2) 0.70477(11) 0.0327(9) Uani 1 1 d . . . C43 C 0.6112(4) 0.2530(3) 0.77900(14) 0.0282(12) Uani 1 1 d . . . H43A H 0.6135 0.2167 0.7601 0.042 Uiso 1 1 calc R . . H43B H 0.6884 0.2645 0.7907 0.042 Uiso 1 1 calc R . . H43C H 0.5747 0.2928 0.7660 0.042 Uiso 1 1 calc R . . F36 F 0.5322(3) 0.50234(19) 0.70118(12) 0.0589(10) Uani 1 1 d . . . F31 F 0.0781(3) 0.4252(2) 0.60356(10) 0.0573(10) Uani 1 1 d . . . F4 F 0.6971(3) 0.0833(2) 1.00087(11) 0.0671(12) Uani 1 1 d . . . C21 C 0.4531(4) 0.4297(3) 0.93864(13) 0.0232(11) Uani 1 1 d . . . C6 C 0.4650(4) 0.2259(3) 1.09789(14) 0.0282(12) Uani 1 1 d . . . H6 H 0.4138 0.2039 1.1121 0.034 Uiso 1 1 calc R . . F8 F 0.2107(3) 0.0090(2) 0.87081(12) 0.0611(10) Uani 1 1 d . . . F24 F 0.2775(4) 0.46409(19) 0.76410(11) 0.0611(11) Uani 1 1 d . . . C40 C 0.5294(4) 0.3567(3) 0.83038(16) 0.0311(12) Uani 1 1 d . . . H40A H 0.4790 0.3612 0.8058 0.047 Uiso 1 1 calc R . . H40B H 0.6060 0.3706 0.8270 0.047 Uiso 1 1 calc R . . H40C H 0.5022 0.3855 0.8498 0.047 Uiso 1 1 calc R . . C9 C 0.1089(4) 0.3121(3) 1.07528(13) 0.0257(11) Uani 1 1 d . . . C50 C 0.2739(4) 0.0715(3) 0.69272(15) 0.0278(11) Uani 1 1 d . . . F30 F 0.6608(3) 0.1117(2) 0.70053(10) 0.0554(10) Uani 1 1 d . . . F9 F 0.3620(3) 0.06428(19) 0.86229(12) 0.0645(11) Uani 1 1 d . . . F23 F 0.1119(3) 0.4645(2) 0.78392(11) 0.0664(12) Uani 1 1 d . . . C33 C 0.1910(4) 0.1536(3) 0.79648(14) 0.0264(11) Uani 1 1 d . . . H33 H 0.2450 0.1264 0.7863 0.032 Uiso 1 1 calc R . . F20 F -0.1324(3) 0.2496(3) 0.67137(13) 0.0831(15) Uani 1 1 d . . . C22 C 0.3559(4) 0.4645(3) 0.92072(14) 0.0286(12) Uani 1 1 d . . . H22 H 0.3626 0.5100 0.9130 0.034 Uiso 1 1 calc R . . F25 F 0.1858(4) 0.0039(2) 0.73667(13) 0.0731(12) Uani 1 1 d . . . C7 C 0.4273(4) 0.2805(3) 1.07358(13) 0.0212(10) Uani 1 1 d . . . C52 C 0.4606(4) 0.1125(3) 0.67950(14) 0.0259(11) Uani 1 1 d . . . C53 C 0.5817(4) 0.0938(3) 0.67076(16) 0.0341(13) Uani 1 1 d . . . F26 F 0.0925(3) 0.0193(2) 0.68032(14) 0.0737(13) Uani 1 1 d . . . C2 C 0.6563(4) 0.2360(3) 1.08090(15) 0.0310(12) Uani 1 1 d . . . F34 F 0.6183(3) 0.4188(2) 0.67900(14) 0.0774(14) Uani 1 1 d . . . C17 C 0.4740(4) 0.1193(3) 1.00540(15) 0.0315(12) Uani 1 1 d . . . H17 H 0.5048 0.0779 1.0157 0.038 Uiso 1 1 calc R . . C23 C 0.2479(4) 0.4324(3) 0.91407(14) 0.0267(11) Uani 1 1 d . . . C51 C 0.3842(4) 0.0586(3) 0.68359(16) 0.0337(13) Uani 1 1 d . . . H51 H 0.4071 0.0135 0.6802 0.040 Uiso 1 1 calc R . . C4 C 0.5066(4) 0.3153(3) 1.05373(13) 0.0221(10) Uani 1 1 d . . . H4 H 0.4836 0.3531 1.0378 0.027 Uiso 1 1 calc R . . F27 F 0.2358(3) -0.0492(2) 0.68865(16) 0.0835(15) Uani 1 1 d . . . F2 F 0.2131(4) 0.0620(2) 1.01656(12) 0.0750(13) Uani 1 1 d . . . C32 C 0.0767(4) 0.1331(3) 0.79185(15) 0.0278(12) Uani 1 1 d . . . H32 H 0.0544 0.0919 0.7792 0.033 Uiso 1 1 calc R . . C16 C 0.3650(4) 0.1392(3) 1.01191(15) 0.0310(12) Uani 1 1 d . . . F32 F 0.0476(4) 0.4602(3) 0.65962(12) 0.0789(14) Uani 1 1 d . . . C45 C 0.0216(4) 0.2918(3) 0.71731(16) 0.0357(13) Uani 1 1 d . . . C36 C 0.2260(4) 0.2141(3) 0.81603(13) 0.0195(10) Uani 1 1 d . . . C39 C 0.6133(4) 0.2716(3) 0.88214(14) 0.0298(12) Uani 1 1 d . . . H39A H 0.5972 0.3051 0.9012 0.045 Uiso 1 1 calc R . . H39B H 0.6914 0.2769 0.8773 0.045 Uiso 1 1 calc R . . H39C H 0.6031 0.2262 0.8921 0.045 Uiso 1 1 calc R . . C57 C 0.4266(4) 0.3975(3) 0.68821(15) 0.0307(12) Uani 1 1 d . . . C46 C 0.0561(4) 0.3486(3) 0.74000(16) 0.0363(14) Uani 1 1 d . . . H46 H 0.0003 0.3795 0.7457 0.044 Uiso 1 1 calc R . . C24 C 0.1448(5) 0.4781(3) 0.89826(19) 0.0420(15) Uani 1 1 d . . . F21 F -0.1462(3) 0.2377(3) 0.73158(14) 0.106(2) Uani 1 1 d . . . C44 C -0.1078(5) 0.2777(4) 0.70581(18) 0.0500(18) Uani 1 1 d . . . C5 C 0.5780(4) 0.2035(3) 1.10142(15) 0.0322(12) Uani 1 1 d . . . H5 H 0.6019 0.1663 1.1177 0.039 Uiso 1 1 calc R . . C28 C 0.0848(4) 0.1765(3) 0.92557(16) 0.0355(13) Uani 1 1 d . . . F35 F 0.5802(4) 0.4177(2) 0.73806(12) 0.0867(16) Uani 1 1 d . . . F7 F 0.3526(3) 0.0148(2) 0.91751(12) 0.0634(11) Uani 1 1 d . . . C18 C 0.5381(4) 0.1608(3) 0.98356(15) 0.0305(12) Uani 1 1 d . . . C27 C 0.1310(5) 0.1186(3) 0.90979(16) 0.0391(14) Uani 1 1 d . . . H27 H 0.0842 0.0807 0.9027 0.047 Uiso 1 1 calc R . . C49 C 0.1974(5) 0.0094(3) 0.6985(2) 0.0432(15) Uani 1 1 d . . . F19 F -0.1700(3) 0.3343(3) 0.70413(17) 0.1005(18) Uani 1 1 d . . . C13 C 0.1516(4) 0.4333(3) 1.05035(19) 0.0428(15) Uani 1 1 d . . . H13A H 0.1994 0.4374 1.0755 0.064 Uiso 1 1 calc R . . H13B H 0.0786 0.4550 1.0514 0.064 Uiso 1 1 calc R . . H13C H 0.1889 0.4551 1.0305 0.064 Uiso 1 1 calc R . . C47 C 0.1697(4) 0.3613(3) 0.75447(14) 0.0301(12) Uani 1 1 d . . . C54 C 0.1304(5) 0.4528(3) 0.63701(19) 0.0473(16) Uani 1 1 d . . . C19 C 0.6596(5) 0.1362(4) 0.97838(19) 0.0471(16) Uani 1 1 d . . . C31 C -0.0053(4) 0.1744(3) 0.80628(14) 0.0250(11) Uani 1 1 d . . . C48 C 0.2008(5) 0.4247(3) 0.77976(17) 0.0418(14) Uani 1 1 d . . . C58 C 0.5404(5) 0.4331(3) 0.70211(18) 0.0403(14) Uani 1 1 d . . . C1 C 0.7968(5) 0.1478(3) 1.0956(2) 0.0489(17) Uani 1 1 d . . . H1A H 0.7398 0.1159 1.0835 0.073 Uiso 1 1 calc R . . H1B H 0.7995 0.1465 1.1237 0.073 Uiso 1 1 calc R . . H1C H 0.8710 0.1355 1.0890 0.073 Uiso 1 1 calc R . . C56 C 0.3350(5) 0.4363(3) 0.66952(16) 0.0375(13) Uani 1 1 d . . . H56 H 0.3460 0.4829 0.6652 0.045 Uiso 1 1 calc R . . C15 C 0.3019(5) 0.0925(3) 1.03809(18) 0.0450(15) Uani 1 1 d . . . C14 C 0.0478(4) 0.3488(3) 1.00289(15) 0.0376(14) Uani 1 1 d . . . H14A H 0.0726 0.3752 0.9820 0.056 Uiso 1 1 calc R . . H14B H -0.0272 0.3642 1.0072 0.056 Uiso 1 1 calc R . . H14C H 0.0442 0.3010 0.9957 0.056 Uiso 1 1 calc R . . C25 C 0.2918(5) 0.0501(3) 0.88877(18) 0.0430(15) Uani 1 1 d . . . C55 C 0.2258(5) 0.4070(3) 0.65691(16) 0.0345(13) Uani 1 1 d . . . F13 F 0.0663(3) 0.4445(2) 0.87543(16) 0.0923(17) Uani 1 1 d . . . C30 C -0.1564(4) 0.0994(3) 0.77959(17) 0.0416(15) Uani 1 1 d . . . H30A H -0.1324 0.1034 0.7541 0.062 Uiso 1 1 calc R . . H30B H -0.2389 0.0959 0.7766 0.062 Uiso 1 1 calc R . . H30C H -0.1224 0.0590 0.7926 0.062 Uiso 1 1 calc R . . F6 F 0.7354(3) 0.1863(2) 0.98602(16) 0.0849(15) Uani 1 1 d . . . F14 F 0.0977(3) 0.5008(2) 0.92916(13) 0.0832(16) Uani 1 1 d . . . C42 C 0.5859(4) 0.1588(3) 0.82655(15) 0.0293(12) Uani 1 1 d . . . H42A H 0.5399 0.1434 0.8458 0.044 Uiso 1 1 calc R . . H42B H 0.6651 0.1623 0.8385 0.044 Uiso 1 1 calc R . . H42C H 0.5795 0.1265 0.8052 0.044 Uiso 1 1 calc R . . C10 C 0.0537(4) 0.2428(3) 1.06313(17) 0.0381(14) Uani 1 1 d . . . H10A H 0.0927 0.2223 1.0433 0.057 Uiso 1 1 calc R . . H10B H -0.0262 0.2495 1.0527 0.057 Uiso 1 1 calc R . . H10C H 0.0597 0.2131 1.0857 0.057 Uiso 1 1 calc R . . F12 F -0.0881(3) 0.2304(2) 0.93899(13) 0.0655(12) Uani 1 1 d . . . F10 F -0.1090(3) 0.1440(3) 0.90379(18) 0.111(2) Uani 1 1 d . . . F11 F -0.0449(4) 0.1341(3) 0.96465(19) 0.133(3) Uani 1 1 d . . . C29 C -0.0420(5) 0.1701(4) 0.9337(2) 0.0543(18) Uani 1 1 d . . . O2 O 0.2554(3) 0.2732(2) 1.12855(10) 0.0394(10) 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 Nd1 0.01916(13) 0.01984(15) 0.01796(14) -0.00160(11) 0.00539(9) -0.00042(10) Nd2 0.02286(14) 0.02350(16) 0.01818(14) -0.00241(11) 0.00346(10) -0.00109(10) Br3 0.0207(2) 0.0392(4) 0.0574(4) 0.0120(3) 0.0112(2) -0.0015(2) Br4 0.0188(2) 0.0512(4) 0.0601(4) -0.0250(3) 0.0067(2) 0.0023(2) O12 0.0237(16) 0.028(2) 0.0196(17) -0.0041(16) 0.0035(13) -0.0002(14) O4 0.0312(18) 0.024(2) 0.0285(18) 0.0025(17) 0.0081(15) 0.0005(15) O3 0.0246(16) 0.031(2) 0.0152(16) 0.0005(15) 0.0068(13) 0.0028(14) O8 0.0249(17) 0.034(2) 0.035(2) -0.0055(18) 0.0043(15) -0.0058(15) O13 0.0279(17) 0.030(2) 0.0264(18) 0.0000(17) 0.0048(14) 0.0051(15) O7 0.0243(16) 0.022(2) 0.0194(17) -0.0019(15) 0.0053(13) -0.0020(13) N2 0.0173(18) 0.026(2) 0.019(2) -0.0060(18) 0.0064(15) -0.0017(16) O17 0.0250(16) 0.023(2) 0.0270(18) -0.0055(16) 0.0048(14) -0.0003(14) O11 0.0219(16) 0.028(2) 0.0162(16) -0.0023(15) 0.0088(13) 0.0010(14) O9 0.0346(18) 0.023(2) 0.0287(19) -0.0083(17) 0.0111(15) -0.0058(15) N3 0.0162(18) 0.026(2) 0.0146(19) -0.0011(17) 0.0033(15) -0.0026(15) C34 0.021(2) 0.036(3) 0.021(2) 0.000(2) 0.0051(19) 0.002(2) N4 0.0193(18) 0.022(2) 0.0115(18) -0.0022(17) 0.0022(14) 0.0005(16) F17 0.049(2) 0.082(3) 0.042(2) -0.020(2) 0.0028(16) -0.0298(19) O6 0.0192(15) 0.026(2) 0.0247(18) -0.0002(16) 0.0034(13) 0.0015(14) O5 0.0226(16) 0.025(2) 0.0320(19) 0.0011(17) 0.0051(14) 0.0023(14) O15 0.0348(19) 0.035(2) 0.0271(19) 0.0067(18) -0.0021(15) 0.0027(16) O18 0.0245(17) 0.029(2) 0.0286(19) -0.0028(17) 0.0060(14) 0.0025(14) C37 0.020(2) 0.019(3) 0.016(2) 0.001(2) 0.0037(18) -0.0015(18) O1 0.0213(18) 0.043(3) 0.058(3) 0.018(2) 0.0100(17) 0.0080(16) O10 0.0179(16) 0.047(3) 0.039(2) -0.0182(19) 0.0055(15) -0.0083(15) O16 0.0289(18) 0.031(2) 0.0322(19) -0.0007(18) 0.0049(15) -0.0001(15) F16 0.0340(17) 0.043(2) 0.110(3) -0.028(2) 0.0366(19) -0.0158(16) N1 0.0216(19) 0.040(3) 0.0126(19) -0.0037(19) 0.0049(15) -0.0022(18) F22 0.057(2) 0.035(2) 0.0337(17) -0.0068(16) 0.0042(15) -0.0009(15) C8 0.020(2) 0.030(3) 0.018(2) -0.003(2) 0.0059(18) -0.0057(19) F29 0.049(2) 0.064(3) 0.061(2) 0.025(2) 0.0334(18) 0.0270(18) C3 0.024(2) 0.027(3) 0.026(3) -0.001(2) 0.0041(19) -0.001(2) F28 0.0429(18) 0.037(2) 0.073(2) -0.0041(19) 0.0192(17) 0.0161(15) C38 0.016(2) 0.027(3) 0.019(2) -0.003(2) 0.0060(17) -0.0087(19) F15 0.0449(19) 0.047(2) 0.072(2) 0.025(2) 0.0066(17) 0.0136(17) C35 0.019(2) 0.025(3) 0.022(2) -0.003(2) -0.0014(18) -0.0004(19) C41 0.016(2) 0.026(3) 0.020(2) 0.001(2) -0.0004(18) -0.0005(18) C11 0.024(3) 0.063(4) 0.032(3) -0.003(3) 0.012(2) 0.008(3) C26 0.044(3) 0.027(3) 0.023(3) 0.001(2) 0.007(2) -0.004(2) F1 0.062(2) 0.049(2) 0.055(2) 0.008(2) 0.0301(18) -0.0042(18) F18 0.046(2) 0.043(2) 0.099(3) 0.034(2) -0.0091(19) -0.0218(17) C20 0.034(3) 0.019(3) 0.036(3) -0.001(3) 0.003(2) -0.004(2) F5 0.072(3) 0.078(3) 0.057(2) 0.003(2) 0.031(2) 0.040(2) F3 0.081(3) 0.053(3) 0.089(3) 0.045(2) 0.030(2) 0.019(2) C12 0.018(2) 0.030(3) 0.025(3) 0.002(2) 0.0068(19) 0.004(2) F33 0.085(3) 0.049(3) 0.152(5) 0.053(3) -0.039(3) -0.004(2) O14 0.0241(17) 0.037(2) 0.037(2) -0.0007(18) 0.0042(15) 0.0021(16) C43 0.022(2) 0.040(3) 0.025(3) -0.006(2) 0.009(2) -0.005(2) F36 0.056(2) 0.030(2) 0.090(3) 0.000(2) 0.0082(19) -0.0100(16) F31 0.058(2) 0.062(3) 0.046(2) -0.001(2) -0.0117(17) 0.0196(19) F4 0.064(2) 0.070(3) 0.070(3) 0.023(2) 0.017(2) 0.040(2) C21 0.028(2) 0.024(3) 0.019(2) -0.004(2) 0.0079(19) -0.004(2) C6 0.025(2) 0.035(3) 0.025(3) -0.002(2) 0.006(2) -0.002(2) F8 0.064(2) 0.038(2) 0.079(3) -0.028(2) 0.003(2) -0.0111(18) F24 0.106(3) 0.028(2) 0.055(2) -0.0041(19) 0.030(2) -0.016(2) C40 0.033(3) 0.027(3) 0.036(3) -0.001(3) 0.011(2) -0.006(2) C9 0.017(2) 0.040(3) 0.021(2) 0.000(2) 0.0060(18) -0.001(2) C50 0.029(3) 0.023(3) 0.029(3) -0.005(2) 0.001(2) 0.002(2) F30 0.0274(16) 0.074(3) 0.060(2) -0.016(2) -0.0090(15) 0.0140(16) F9 0.084(3) 0.040(2) 0.079(3) -0.025(2) 0.045(2) -0.006(2) F23 0.076(3) 0.055(3) 0.067(2) -0.022(2) 0.005(2) 0.034(2) C33 0.021(2) 0.031(3) 0.028(3) -0.006(2) 0.0081(19) -0.002(2) F20 0.036(2) 0.139(5) 0.070(3) -0.024(3) -0.0071(19) 0.008(2) C22 0.034(3) 0.025(3) 0.027(3) 0.001(2) 0.006(2) 0.002(2) F25 0.091(3) 0.057(3) 0.078(3) 0.009(2) 0.035(2) -0.019(2) C7 0.019(2) 0.029(3) 0.015(2) -0.002(2) 0.0005(17) 0.0011(19) C52 0.026(2) 0.031(3) 0.020(2) -0.006(2) 0.0014(19) 0.006(2) C53 0.034(3) 0.033(3) 0.035(3) 0.000(3) 0.003(2) 0.011(2) F26 0.040(2) 0.054(3) 0.118(4) 0.011(3) -0.017(2) -0.0206(18) C2 0.020(2) 0.038(3) 0.035(3) -0.003(3) 0.004(2) 0.001(2) F34 0.044(2) 0.067(3) 0.128(4) -0.038(3) 0.035(2) -0.0131(19) C17 0.038(3) 0.023(3) 0.034(3) 0.003(3) 0.006(2) 0.004(2) C23 0.033(3) 0.025(3) 0.024(3) -0.002(2) 0.009(2) 0.007(2) C51 0.033(3) 0.025(3) 0.044(3) -0.009(3) 0.006(2) 0.002(2) C4 0.022(2) 0.023(3) 0.021(2) -0.005(2) 0.0028(18) 0.0019(19) F27 0.067(3) 0.029(2) 0.166(5) -0.027(3) 0.054(3) -0.0092(19) F2 0.089(3) 0.062(3) 0.072(3) 0.010(2) 0.002(2) -0.045(2) C32 0.024(2) 0.027(3) 0.032(3) -0.011(2) 0.005(2) -0.005(2) C16 0.044(3) 0.025(3) 0.024(3) 0.002(2) 0.005(2) 0.001(2) F32 0.076(3) 0.095(4) 0.066(3) 0.002(3) 0.015(2) 0.051(3) C45 0.030(3) 0.046(4) 0.031(3) 0.006(3) 0.004(2) 0.002(3) C36 0.015(2) 0.027(3) 0.017(2) -0.001(2) 0.0029(17) -0.0027(18) C39 0.018(2) 0.046(4) 0.024(3) -0.007(3) -0.0013(19) 0.002(2) C57 0.037(3) 0.027(3) 0.030(3) 0.000(3) 0.013(2) -0.002(2) C46 0.033(3) 0.043(4) 0.035(3) 0.006(3) 0.012(2) 0.023(3) C24 0.032(3) 0.032(4) 0.061(4) 0.012(3) 0.004(3) 0.005(2) F21 0.040(2) 0.178(6) 0.096(3) 0.068(4) 0.000(2) -0.031(3) C44 0.033(3) 0.079(5) 0.037(3) 0.005(4) 0.003(3) 0.014(3) C5 0.027(3) 0.035(3) 0.034(3) 0.008(3) 0.004(2) 0.003(2) C28 0.026(3) 0.047(4) 0.033(3) -0.001(3) 0.004(2) -0.007(2) F35 0.106(3) 0.074(3) 0.066(3) 0.032(3) -0.035(2) -0.058(3) F7 0.080(3) 0.035(2) 0.070(3) -0.004(2) -0.006(2) 0.0133(19) C18 0.034(3) 0.030(3) 0.026(3) -0.008(3) -0.001(2) 0.004(2) C27 0.043(3) 0.032(4) 0.043(3) -0.011(3) 0.009(3) -0.015(3) C49 0.033(3) 0.031(4) 0.065(4) -0.006(3) 0.008(3) -0.002(2) F19 0.041(2) 0.103(4) 0.151(5) -0.024(4) -0.006(3) 0.033(2) C13 0.028(3) 0.035(4) 0.070(4) -0.003(3) 0.026(3) 0.002(2) C47 0.040(3) 0.029(3) 0.023(3) 0.002(2) 0.013(2) 0.009(2) C54 0.052(4) 0.039(4) 0.050(4) 0.011(3) 0.004(3) 0.008(3) C19 0.044(3) 0.044(4) 0.056(4) 0.003(3) 0.016(3) 0.014(3) C31 0.017(2) 0.033(3) 0.025(3) -0.004(2) 0.0009(19) -0.004(2) C48 0.057(4) 0.035(4) 0.034(3) -0.003(3) 0.009(3) 0.009(3) C58 0.045(3) 0.028(3) 0.048(4) 0.003(3) 0.008(3) -0.004(3) C1 0.033(3) 0.042(4) 0.073(4) 0.019(4) 0.012(3) 0.013(3) C56 0.047(3) 0.028(3) 0.038(3) 0.007(3) 0.008(3) 0.000(3) C15 0.054(4) 0.036(4) 0.044(4) 0.010(3) 0.004(3) -0.004(3) C14 0.023(3) 0.062(4) 0.027(3) 0.006(3) 0.003(2) 0.004(2) C25 0.049(3) 0.035(4) 0.046(4) -0.008(3) 0.009(3) -0.003(3) C55 0.042(3) 0.029(3) 0.033(3) 0.005(3) 0.005(2) 0.008(2) F13 0.052(2) 0.050(3) 0.154(4) 0.023(3) -0.056(3) 0.0016(19) C30 0.022(3) 0.054(4) 0.047(3) -0.015(3) 0.002(2) -0.013(2) F6 0.0307(19) 0.065(3) 0.160(5) -0.019(3) 0.018(2) 0.0105(19) F14 0.074(3) 0.090(4) 0.098(3) 0.032(3) 0.055(3) 0.058(3) C42 0.021(2) 0.033(3) 0.035(3) -0.002(3) 0.005(2) 0.002(2) C10 0.023(3) 0.041(4) 0.048(3) 0.011(3) 0.000(2) -0.003(2) F12 0.0321(18) 0.068(3) 0.099(3) -0.015(3) 0.0156(19) -0.0053(18) F10 0.035(2) 0.111(4) 0.184(5) -0.080(4) 0.012(3) -0.025(2) F11 0.059(3) 0.161(6) 0.196(6) 0.126(5) 0.076(4) 0.039(3) C29 0.036(3) 0.052(5) 0.077(5) -0.019(4) 0.014(3) -0.017(3) O2 0.0280(18) 0.073(3) 0.0182(18) 0.0073(19) 0.0063(14) 0.0053(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O5 2.389(3) . ? Nd1 O8 2.405(3) . ? Nd1 O11 2.413(3) . ? Nd1 O6 2.417(3) . ? Nd1 O9 2.426(3) . ? Nd1 O4 2.433(3) . ? Nd1 O7 2.435(3) . ? Nd1 O3 2.439(3) . ? Nd2 O2 2.374(3) 4_565 ? Nd2 O17 2.391(3) . ? Nd2 O16 2.391(4) . ? Nd2 O13 2.411(3) . ? Nd2 O14 2.417(3) . ? Nd2 O18 2.431(3) . ? Nd2 O15 2.467(4) . ? Nd2 O12 2.468(3) . ? Br3 C3 1.893(5) . ? Br4 C34 1.888(5) . ? O12 N4 1.292(5) . ? O4 C16 1.251(6) . ? O3 N2 1.295(4) . ? O8 C28 1.241(7) . ? O13 C47 1.274(6) . ? O7 C21 1.255(6) . ? N2 C8 1.329(6) . ? N2 C12 1.508(5) . ? O17 C50 1.236(6) . ? O11 N3 1.283(4) . ? O9 C26 1.249(6) . ? N3 C37 1.335(6) . ? N3 C38 1.514(5) . ? C34 C35 1.382(6) . ? C34 C31 1.388(7) . ? N4 C37 1.354(5) . ? N4 C41 1.496(5) . ? F17 C20 1.309(6) . ? O6 C23 1.236(6) . ? O5 C18 1.241(6) . ? O15 C55 1.247(7) . ? O18 C52 1.234(6) . ? C37 C36 1.455(6) . ? O1 C2 1.356(6) . ? O1 C1 1.428(7) . ? O10 C31 1.363(5) . ? O10 C30 1.426(7) . ? O16 C57 1.273(6) . ? F16 C20 1.309(6) . ? N1 O2 1.277(5) . ? N1 C8 1.347(5) . ? N1 C9 1.511(6) . ? F22 C48 1.346(7) . ? C8 C7 1.465(6) . ? F29 C53 1.324(6) . ? C3 C2 1.374(7) . ? C3 C4 1.384(6) . ? F28 C53 1.330(7) . ? C38 C39 1.519(6) . ? C38 C40 1.524(7) . ? C38 C41 1.550(7) . ? F15 C24 1.320(7) . ? C35 C36 1.398(6) . ? C41 C43 1.517(6) . ? C41 C42 1.528(7) . ? C11 C9 1.529(6) . ? C26 C27 1.392(7) . ? C26 C25 1.528(8) . ? F1 C15 1.326(7) . ? F18 C20 1.334(6) . ? C20 C21 1.542(6) . ? F5 C19 1.333(7) . ? F3 C15 1.326(7) . ? C12 C13 1.507(8) . ? C12 C14 1.513(7) . ? C12 C9 1.556(7) . ? F33 C54 1.310(8) . ? O14 C45 1.252(7) . ? F36 C58 1.348(7) . ? F31 C54 1.331(7) . ? F4 C19 1.322(7) . ? C21 C22 1.387(7) . ? C6 C7 1.381(7) . ? C6 C5 1.382(7) . ? F8 C25 1.321(7) . ? F24 C48 1.351(7) . ? C9 C10 1.525(8) . ? C50 C51 1.396(7) . ? C50 C49 1.535(8) . ? F30 C53 1.320(6) . ? F9 C25 1.342(6) . ? F23 C48 1.322(6) . ? C33 C32 1.384(6) . ? C33 C36 1.386(7) . ? F20 C44 1.294(7) . ? C22 C23 1.399(7) . ? F25 C49 1.341(7) . ? C7 C4 1.406(6) . ? C52 C51 1.399(7) . ? C52 C53 1.537(6) . ? F26 C49 1.307(7) . ? C2 C5 1.388(7) . ? F34 C58 1.325(6) . ? C17 C16 1.384(7) . ? C17 C18 1.393(7) . ? C23 C24 1.532(7) . ? F27 C49 1.287(7) . ? F2 C15 1.324(7) . ? C32 C31 1.398(7) . ? C16 C15 1.540(8) . ? F32 C54 1.337(7) . ? C45 C46 1.376(8) . ? C45 C44 1.535(8) . ? C57 C56 1.388(8) . ? C57 C58 1.515(8) . ? C46 C47 1.373(8) . ? C24 F13 1.293(7) . ? C24 F14 1.341(7) . ? F21 C44 1.306(8) . ? C44 F19 1.316(8) . ? C28 C27 1.393(8) . ? C28 C29 1.558(7) . ? F35 C58 1.287(7) . ? F7 C25 1.319(7) . ? C18 C19 1.536(7) . ? C47 C48 1.520(8) . ? C54 C55 1.511(8) . ? C19 F6 1.318(8) . ? C56 C55 1.409(8) . ? F12 C29 1.313(8) . ? F10 C29 1.299(8) . ? F11 C29 1.277(8) . ? O2 Nd2 2.374(3) 4_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Nd1 O8 133.36(13) . . ? O5 Nd1 O11 93.40(11) . . ? O8 Nd1 O11 102.33(11) . . ? O5 Nd1 O6 149.59(11) . . ? O8 Nd1 O6 76.55(12) . . ? O11 Nd1 O6 71.01(11) . . ? O5 Nd1 O9 73.15(12) . . ? O8 Nd1 O9 70.92(12) . . ? O11 Nd1 O9 71.59(11) . . ? O6 Nd1 O9 122.65(12) . . ? O5 Nd1 O4 71.02(11) . . ? O8 Nd1 O4 73.07(12) . . ? O11 Nd1 O4 148.56(11) . . ? O6 Nd1 O4 134.30(10) . . ? O9 Nd1 O4 77.70(11) . . ? O5 Nd1 O7 78.65(11) . . ? O8 Nd1 O7 147.83(12) . . ? O11 Nd1 O7 74.29(11) . . ? O6 Nd1 O7 72.12(11) . . ? O9 Nd1 O7 133.68(10) . . ? O4 Nd1 O7 126.04(11) . . ? O5 Nd1 O3 106.53(11) . . ? O8 Nd1 O3 90.94(11) . . ? O11 Nd1 O3 137.32(11) . . ? O6 Nd1 O3 73.12(11) . . ? O9 Nd1 O3 149.95(11) . . ? O4 Nd1 O3 74.09(11) . . ? O7 Nd1 O3 73.30(10) . . ? O2 Nd2 O17 81.60(13) 4_565 . ? O2 Nd2 O16 94.43(13) 4_565 . ? O17 Nd2 O16 151.59(11) . . ? O2 Nd2 O13 144.24(13) 4_565 . ? O17 Nd2 O13 123.10(11) . . ? O16 Nd2 O13 75.17(11) . . ? O2 Nd2 O14 95.44(12) 4_565 . ? O17 Nd2 O14 74.40(12) . . ? O16 Nd2 O14 134.00(12) . . ? O13 Nd2 O14 70.83(12) . . ? O2 Nd2 O18 73.29(12) 4_565 . ? O17 Nd2 O18 71.55(11) . . ? O16 Nd2 O18 80.33(12) . . ? O13 Nd2 O18 135.54(11) . . ? O14 Nd2 O18 145.30(12) . . ? O2 Nd2 O15 68.66(14) 4_565 . ? O17 Nd2 O15 131.49(12) . . ? O16 Nd2 O15 70.78(12) . . ? O13 Nd2 O15 75.63(12) . . ? O14 Nd2 O15 71.44(12) . . ? O18 Nd2 O15 129.35(11) . . ? O2 Nd2 O12 140.76(13) 4_565 . ? O17 Nd2 O12 73.44(11) . . ? O16 Nd2 O12 93.59(12) . . ? O13 Nd2 O12 74.77(11) . . ? O14 Nd2 O12 106.07(11) . . ? O18 Nd2 O12 70.35(11) . . ? O15 Nd2 O12 149.24(12) . . ? N4 O12 Nd2 132.6(3) . . ? C16 O4 Nd1 132.5(3) . . ? N2 O3 Nd1 136.0(3) . . ? C28 O8 Nd1 135.1(3) . . ? C47 O13 Nd2 131.4(3) . . ? C21 O7 Nd1 133.3(3) . . ? O3 N2 C8 125.9(3) . . ? O3 N2 C12 120.3(4) . . ? C8 N2 C12 113.3(3) . . ? C50 O17 Nd2 136.1(3) . . ? N3 O11 Nd1 146.0(3) . . ? C26 O9 Nd1 134.6(3) . . ? O11 N3 C37 125.1(3) . . ? O11 N3 C38 120.8(3) . . ? C37 N3 C38 113.3(3) . . ? C35 C34 C31 121.8(4) . . ? C35 C34 Br4 118.0(4) . . ? C31 C34 Br4 120.3(3) . . ? O12 N4 C37 125.5(4) . . ? O12 N4 C41 121.5(3) . . ? C37 N4 C41 112.7(3) . . ? C23 O6 Nd1 134.4(3) . . ? C18 O5 Nd1 133.8(3) . . ? C55 O15 Nd2 134.9(3) . . ? C52 O18 Nd2 134.3(3) . . ? N3 C37 N4 106.9(4) . . ? N3 C37 C36 128.2(4) . . ? N4 C37 C36 124.8(4) . . ? C2 O1 C1 117.3(4) . . ? C31 O10 C30 116.4(4) . . ? C57 O16 Nd2 135.2(3) . . ? O2 N1 C8 125.7(4) . . ? O2 N1 C9 121.5(3) . . ? C8 N1 C9 112.4(4) . . ? N2 C8 N1 107.2(4) . . ? N2 C8 C7 126.6(4) . . ? N1 C8 C7 126.1(4) . . ? C2 C3 C4 122.3(4) . . ? C2 C3 Br3 119.9(3) . . ? C4 C3 Br3 117.8(4) . . ? N3 C38 C39 109.4(3) . . ? N3 C38 C40 105.5(4) . . ? C39 C38 C40 111.6(4) . . ? N3 C38 C41 99.7(3) . . ? C39 C38 C41 115.4(4) . . ? C40 C38 C41 113.9(4) . . ? C34 C35 C36 119.0(5) . . ? N4 C41 C43 110.2(4) . . ? N4 C41 C42 106.0(4) . . ? C43 C41 C42 110.3(4) . . ? N4 C41 C38 100.1(3) . . ? C43 C41 C38 116.2(4) . . ? C42 C41 C38 113.3(4) . . ? O9 C26 C27 128.2(5) . . ? O9 C26 C25 114.1(5) . . ? C27 C26 C25 117.7(5) . . ? F17 C20 F16 107.1(5) . . ? F17 C20 F18 106.1(5) . . ? F16 C20 F18 106.7(4) . . ? F17 C20 C21 111.5(4) . . ? F16 C20 C21 111.9(4) . . ? F18 C20 C21 113.1(4) . . ? N2 C12 C13 106.1(4) . . ? N2 C12 C14 110.0(4) . . ? C13 C12 C14 111.6(5) . . ? N2 C12 C9 98.9(4) . . ? C13 C12 C9 114.7(4) . . ? C14 C12 C9 114.5(4) . . ? C45 O14 Nd2 132.6(4) . . ? O7 C21 C22 129.0(5) . . ? O7 C21 C20 113.5(4) . . ? C22 C21 C20 117.5(5) . . ? C7 C6 C5 120.8(5) . . ? N1 C9 C10 106.0(4) . . ? N1 C9 C11 109.8(4) . . ? C10 C9 C11 111.1(4) . . ? N1 C9 C12 99.6(3) . . ? C10 C9 C12 114.5(4) . . ? C11 C9 C12 114.8(5) . . ? O17 C50 C51 128.2(5) . . ? O17 C50 C49 114.0(4) . . ? C51 C50 C49 117.8(5) . . ? C32 C33 C36 120.8(4) . . ? C21 C22 C23 121.3(5) . . ? C6 C7 C4 119.1(4) . . ? C6 C7 C8 121.7(4) . . ? C4 C7 C8 119.1(4) . . ? O18 C52 C51 128.7(4) . . ? O18 C52 C53 113.5(4) . . ? C51 C52 C53 117.7(5) . . ? F30 C53 F29 108.5(5) . . ? F30 C53 F28 106.4(4) . . ? F29 C53 F28 106.3(4) . . ? F30 C53 C52 110.5(4) . . ? F29 C53 C52 111.1(4) . . ? F28 C53 C52 113.8(5) . . ? O1 C2 C3 117.5(4) . . ? O1 C2 C5 124.2(5) . . ? C3 C2 C5 118.3(4) . . ? C16 C17 C18 120.7(5) . . ? O6 C23 C22 129.2(5) . . ? O6 C23 C24 114.2(4) . . ? C22 C23 C24 116.6(5) . . ? C50 C51 C52 121.1(5) . . ? C3 C4 C7 118.7(5) . . ? C33 C32 C31 119.9(5) . . ? O4 C16 C17 128.6(5) . . ? O4 C16 C15 113.7(5) . . ? C17 C16 C15 117.7(5) . . ? O14 C45 C46 127.6(5) . . ? O14 C45 C44 113.4(6) . . ? C46 C45 C44 119.0(5) . . ? C33 C36 C35 119.8(4) . . ? C33 C36 C37 119.3(4) . . ? C35 C36 C37 120.9(4) . . ? O16 C57 C56 127.7(5) . . ? O16 C57 C58 113.5(5) . . ? C56 C57 C58 118.8(5) . . ? C47 C46 C45 122.4(5) . . ? F13 C24 F15 107.9(5) . . ? F13 C24 F14 107.8(5) . . ? F15 C24 F14 105.9(5) . . ? F13 C24 C23 112.0(5) . . ? F15 C24 C23 114.9(4) . . ? F14 C24 C23 107.8(5) . . ? F20 C44 F21 108.3(7) . . ? F20 C44 F19 105.4(5) . . ? F21 C44 F19 106.4(6) . . ? F20 C44 C45 112.9(5) . . ? F21 C44 C45 111.1(5) . . ? F19 C44 C45 112.4(6) . . ? C6 C5 C2 120.6(5) . . ? O8 C28 C27 128.3(5) . . ? O8 C28 C29 115.4(5) . . ? C27 C28 C29 116.2(5) . . ? O5 C18 C17 128.5(5) . . ? O5 C18 C19 113.8(5) . . ? C17 C18 C19 117.7(5) . . ? C28 C27 C26 120.9(5) . . ? F27 C49 F26 110.3(6) . . ? F27 C49 F25 106.1(6) . . ? F26 C49 F25 104.7(5) . . ? F27 C49 C50 115.3(5) . . ? F26 C49 C50 110.4(5) . . ? F25 C49 C50 109.5(5) . . ? O13 C47 C46 127.6(5) . . ? O13 C47 C48 113.1(5) . . ? C46 C47 C48 119.3(5) . . ? F33 C54 F31 107.7(5) . . ? F33 C54 F32 106.5(6) . . ? F31 C54 F32 105.2(5) . . ? F33 C54 C55 114.7(5) . . ? F31 C54 C55 111.6(5) . . ? F32 C54 C55 110.7(5) . . ? F6 C19 F4 107.6(6) . . ? F6 C19 F5 107.1(5) . . ? F4 C19 F5 106.4(5) . . ? F6 C19 C18 110.9(5) . . ? F4 C19 C18 114.1(5) . . ? F5 C19 C18 110.4(5) . . ? O10 C31 C34 117.4(4) . . ? O10 C31 C32 123.8(5) . . ? C34 C31 C32 118.8(4) . . ? F23 C48 F22 107.8(4) . . ? F23 C48 F24 107.1(5) . . ? F22 C48 F24 105.8(5) . . ? F23 C48 C47 114.1(5) . . ? F22 C48 C47 111.1(5) . . ? F24 C48 C47 110.5(4) . . ? F35 C58 F34 109.9(5) . . ? F35 C58 F36 105.6(5) . . ? F34 C58 F36 104.4(5) . . ? F35 C58 C57 111.9(5) . . ? F34 C58 C57 111.6(5) . . ? F36 C58 C57 113.1(5) . . ? C57 C56 C55 121.9(5) . . ? F2 C15 F3 107.5(5) . . ? F2 C15 F1 107.1(5) . . ? F3 C15 F1 106.6(5) . . ? F2 C15 C16 110.1(5) . . ? F3 C15 C16 114.0(5) . . ? F1 C15 C16 111.2(5) . . ? F7 C25 F8 107.8(5) . . ? F7 C25 F9 107.2(5) . . ? F8 C25 F9 106.2(5) . . ? F7 C25 C26 110.8(5) . . ? F8 C25 C26 114.3(5) . . ? F9 C25 C26 110.2(5) . . ? O15 C55 C56 127.1(5) . . ? O15 C55 C54 114.2(5) . . ? C56 C55 C54 118.6(5) . . ? F11 C29 F10 110.8(7) . . ? F11 C29 F12 108.2(6) . . ? F10 C29 F12 104.2(6) . . ? F11 C29 C28 109.6(6) . . ? F10 C29 C28 111.8(5) . . ? F12 C29 C28 112.1(5) . . ? N1 O2 Nd2 167.3(4) . 4_566 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.318 _refine_diff_density_min -1.345 _refine_diff_density_rms 0.122 _database_code_depnum_ccdc_archive 'CCDC 958922' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Gd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H42 Br2 F36 Gd2 N4 O18' _chemical_formula_weight 2241.28 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.822(7) _cell_length_b 19.451(10) _cell_length_c 34.170(19) _cell_angle_alpha 90.00 _cell_angle_beta 98.083(7) _cell_angle_gamma 90.00 _cell_volume 7780(7) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 18285 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Darkgreen _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 _exptl_absorpt_coefficient_mu 2.870 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51532 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13335 _reflns_number_gt 11529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+230.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13335 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.2340 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.17647(5) 0.72451(3) 0.555543(18) 0.01658(18) Uani 1 1 d . . . Gd2 Gd 0.21451(5) 0.74885(3) 0.804008(18) 0.01782(18) Uani 1 1 d . . . Br1 Br 0.58435(12) 0.69664(8) 0.65885(5) 0.0370(4) Uani 1 1 d . . . O4 O -0.0013(8) 0.7778(5) 0.5376(3) 0.024(2) Uani 1 1 d . . . F1 F 0.3287(8) 0.4624(4) 0.6211(3) 0.044(2) Uani 1 1 d . . . O8 O 0.0435(8) 0.6313(4) 0.5495(3) 0.0211(19) Uani 1 1 d . . . F25 F 0.2488(8) 0.5890(5) 0.6860(2) 0.038(2) Uani 1 1 d . . . O5 O 0.1995(8) 0.8063(5) 0.5054(3) 0.028(2) Uani 1 1 d . . . F4 F -0.1475(8) 0.5668(5) 0.5685(3) 0.052(3) Uani 1 1 d . . . N2 N 0.0894(9) 0.7748(6) 0.7083(3) 0.018(2) Uani 1 1 d . . . O13 O 0.3034(8) 0.6500(5) 0.8397(3) 0.026(2) Uani 1 1 d . . . O15 O 0.2426(8) 0.6690(5) 0.7535(3) 0.026(2) Uani 1 1 d . . . O6 O 0.1858(8) 0.8308(5) 0.5898(3) 0.025(2) Uani 1 1 d . . . O14 O 0.0724(8) 0.6636(4) 0.8067(3) 0.022(2) Uani 1 1 d . . . O16 O 0.4137(7) 0.7499(4) 0.7985(3) 0.0185(18) Uani 1 1 d . . . O17 O 0.2706(8) 0.8652(4) 0.8034(3) 0.0216(19) Uani 1 1 d . . . F5 F -0.1009(8) 0.5170(6) 0.5182(3) 0.051(3) Uani 1 1 d . . . O1 O 0.1375(8) 0.7024(5) 0.6210(3) 0.023(2) Uani 1 1 d . . . O9 O 0.2807(8) 0.6257(5) 0.5809(3) 0.025(2) Uani 1 1 d . . . N1 N 0.0985(9) 0.7271(6) 0.6507(3) 0.020(2) Uani 1 1 d . . . O18 O 0.0561(8) 0.8165(4) 0.8190(3) 0.0210(19) Uani 1 1 d U . . F19 F 0.4226(9) 0.5722(5) 0.8980(3) 0.047(2) Uani 1 1 d . . . O10 O 0.2433(8) 0.7692(5) 0.8720(3) 0.030(2) Uani 1 1 d . . . N3 N 0.2685(10) 0.7941(6) 0.9074(3) 0.026(3) Uani 1 1 d . . . O12 O -0.2627(10) 0.7103(5) 0.9220(3) 0.038(3) Uani 1 1 d . . . F6 F -0.0613(8) 0.4710(5) 0.5757(4) 0.057(3) Uani 1 1 d . . . F10 F 0.2483(9) 0.8714(5) 0.4391(3) 0.046(2) Uani 1 1 d . . . F22 F -0.0336(8) 0.4957(5) 0.7996(3) 0.048(2) Uani 1 1 d . . . C4 C 0.2525(12) 0.5638(7) 0.5859(4) 0.022(3) Uani 1 1 d . . . F26 F 0.2238(10) 0.5306(4) 0.7379(3) 0.048(3) Uani 1 1 d . . . C56 C 0.3899(11) 0.8111(7) 0.9244(4) 0.022(3) Uani 1 1 d . . . C53 C 0.3641(11) 0.8585(7) 0.9594(4) 0.021(3) Uani 1 1 d . . . C52 C 0.1953(10) 0.7992(6) 0.9343(4) 0.014(2) Uani 1 1 d . . . C1 C -0.0647(11) 0.5308(7) 0.5559(5) 0.028(3) Uani 1 1 d . . . C58 C 0.4519(13) 0.8480(8) 0.8937(4) 0.031(3) Uani 1 1 d . . . H58A H 0.4622 0.8161 0.8723 0.046 Uiso 1 1 calc R . . H58B H 0.5268 0.8640 0.9064 0.046 Uiso 1 1 calc R . . H58C H 0.4063 0.8875 0.8829 0.046 Uiso 1 1 calc R . . O3 O 0.6235(8) 0.8337(5) 0.6980(3) 0.025(2) Uani 1 1 d . . . C16 C 0.3591(11) 0.7367(7) 0.6704(4) 0.025(3) Uani 1 1 d . . . H16 H 0.3350 0.6951 0.6573 0.030 Uiso 1 1 calc R . . C12 C 0.2635(13) 0.8770(8) 0.5973(4) 0.030(3) Uani 1 1 d . . . O2 O 0.1193(8) 0.7970(5) 0.7434(3) 0.0211(19) Uani 1 1 d . . . F13 F 0.2991(9) 0.9857(5) 0.6305(3) 0.051(3) Uani 1 1 d . . . C18 C 0.1585(11) 0.7595(6) 0.6814(4) 0.019(3) Uani 1 1 d . . . C28 C 0.4760(11) 0.7566(6) 0.6757(4) 0.019(3) Uani 1 1 d . . . F24 F -0.0825(12) 0.5805(6) 0.7634(3) 0.081(5) Uani 1 1 d . . . F23 F -0.1189(9) 0.5794(6) 0.8230(4) 0.066(3) Uani 1 1 d . . . F2 F 0.4015(10) 0.4938(6) 0.5703(4) 0.072(4) Uani 1 1 d . . . F27 F 0.3872(10) 0.5308(5) 0.7176(3) 0.059(3) Uani 1 1 d . . . C25 C 0.3140(11) 0.8394(6) 0.7047(4) 0.021(3) Uani 1 1 d . . . H25 H 0.2592 0.8678 0.7146 0.025 Uiso 1 1 calc R . . C2 C 0.0504(11) 0.5701(6) 0.5621(4) 0.016(3) Uani 1 1 d U . . C22 C -0.0341(9) 0.7664(6) 0.6910(3) 0.013(2) Uani 1 1 d . . . C47 C -0.1550(12) 0.7304(8) 0.9230(4) 0.030(3) Uani 1 1 d . . . C35 C 0.3661(15) 0.5431(8) 0.8655(5) 0.041(4) Uani 1 1 d . . . C27 C 0.5159(12) 0.8186(7) 0.6952(4) 0.027(3) Uani 1 1 d . . . C7 C 0.1454(14) 0.8579(7) 0.4928(4) 0.030(3) Uani 1 1 d . . . F14 F 0.1479(10) 0.9312(5) 0.6410(3) 0.055(3) Uani 1 1 d . . . C36 C 0.2738(13) 0.5896(7) 0.8451(4) 0.025(3) Uani 1 1 d . . . C37 C 0.1621(15) 0.5604(8) 0.8328(4) 0.036(4) Uani 1 1 d . . . H37 H 0.1495 0.5132 0.8377 0.043 Uiso 1 1 calc R . . C54 C 0.3421(13) 0.9335(7) 0.9481(5) 0.035(4) Uani 1 1 d . . . H54A H 0.4122 0.9541 0.9411 0.052 Uiso 1 1 calc R . . H54B H 0.3184 0.9584 0.9705 0.052 Uiso 1 1 calc R . . H54C H 0.2815 0.9363 0.9254 0.052 Uiso 1 1 calc R . . C11 C 0.2159(14) 0.9439(7) 0.6144(4) 0.032(3) Uani 1 1 d . . . C23 C -0.0779(13) 0.8378(8) 0.6754(4) 0.030(3) Uani 1 1 d . . . H23A H -0.0839 0.8684 0.6978 0.046 Uiso 1 1 calc R . . H23B H -0.1532 0.8327 0.6596 0.046 Uiso 1 1 calc R . . H23C H -0.0242 0.8574 0.6591 0.046 Uiso 1 1 calc R . . C30 C -0.0812(12) 0.8985(7) 0.8307(4) 0.027(3) Uani 1 1 d . . . C50 C -0.0050(11) 0.8133(7) 0.9489(4) 0.024(3) Uani 1 1 d . . . H50 H 0.0177 0.8517 0.9654 0.029 Uiso 1 1 calc R . . F11 F 0.1383(11) 0.9556(5) 0.4489(3) 0.061(3) Uani 1 1 d . . . C9 C -0.0312(11) 0.8338(7) 0.5214(4) 0.024(3) Uani 1 1 d . . . C41 C 0.4749(12) 0.7051(8) 0.7855(4) 0.033(4) Uani 1 1 d . . . C21 C -0.0240(13) 0.6382(8) 0.6716(5) 0.035(4) Uani 1 1 d . . . H21A H -0.0028 0.6085 0.6506 0.052 Uiso 1 1 calc R . . H21B H -0.1000 0.6253 0.6774 0.052 Uiso 1 1 calc R . . H21C H 0.0318 0.6328 0.6955 0.052 Uiso 1 1 calc R . . C45 C 0.0407(12) 0.7196(7) 0.9050(4) 0.029(3) Uani 1 1 d . . . H45 H 0.0944 0.6959 0.8916 0.034 Uiso 1 1 calc R . . C5 C 0.3553(14) 0.5169(8) 0.6023(5) 0.037(4) Uani 1 1 d . . . C20 C -0.1080(11) 0.7240(8) 0.6192(4) 0.027(3) Uani 1 1 d . . . H20A H -0.1061 0.7722 0.6110 0.041 Uiso 1 1 calc R . . H20B H -0.1857 0.7119 0.6236 0.041 Uiso 1 1 calc R . . H20C H -0.0845 0.6945 0.5986 0.041 Uiso 1 1 calc R . . C48 C -0.2936(13) 0.6408(8) 0.9063(5) 0.035(4) Uani 1 1 d U . . H48A H -0.2935 0.6404 0.8776 0.053 Uiso 1 1 calc R . . H48B H -0.3699 0.6286 0.9121 0.053 Uiso 1 1 calc R . . H48C H -0.2378 0.6073 0.9187 0.053 Uiso 1 1 calc R . . C43 C 0.3296(13) 0.6342(7) 0.7478(4) 0.027(3) Uani 1 1 d . . . C31 C 0.0398(11) 0.8790(7) 0.8209(4) 0.024(3) Uani 1 1 d . . . F28 F 0.6663(9) 0.6619(7) 0.7983(4) 0.075(4) Uani 1 1 d . . . C19 C -0.0256(11) 0.7138(7) 0.6579(4) 0.022(3) Uani 1 1 d . . . C51 C 0.0747(11) 0.7779(6) 0.9284(4) 0.018(3) Uani 1 1 d . . . C32 C 0.1149(13) 0.9340(7) 0.8160(4) 0.028(3) Uani 1 1 d . . . H32 H 0.0902 0.9800 0.8187 0.034 Uiso 1 1 calc R . . C39 C -0.0395(13) 0.5645(8) 0.7996(4) 0.029(3) Uani 1 1 d . . . C3 C 0.1466(13) 0.5339(7) 0.5796(4) 0.030(3) Uani 1 1 d . . . H3 H 0.1383 0.4875 0.5874 0.036 Uiso 1 1 calc R . . C46 C -0.0741(12) 0.6968(7) 0.9015(4) 0.025(3) Uani 1 1 d . . . H46 H -0.0981 0.6589 0.8848 0.030 Uiso 1 1 calc R . . C6 C 0.2047(14) 0.9063(7) 0.4677(5) 0.034(4) Uani 1 1 d . . . C38 C 0.0725(12) 0.5998(6) 0.8138(4) 0.020(3) Uani 1 1 d . . . F15 F 0.1541(9) 0.9789(5) 0.5849(3) 0.055(3) Uani 1 1 d . . . C8 C 0.0333(12) 0.8772(7) 0.4995(4) 0.027(3) Uani 1 1 d . . . H8 H 0.0016 0.9195 0.4893 0.032 Uiso 1 1 calc R . . C42 C 0.4427(13) 0.6462(7) 0.7618(4) 0.029(3) Uani 1 1 d . . . H42 H 0.4996 0.6151 0.7556 0.035 Uiso 1 1 calc R . . C24 C -0.1062(12) 0.7408(8) 0.7227(4) 0.027(3) Uani 1 1 d . . . H24A H -0.0916 0.6918 0.7277 0.041 Uiso 1 1 calc R . . H24B H -0.1875 0.7478 0.7131 0.041 Uiso 1 1 calc R . . H24C H -0.0851 0.7668 0.7472 0.041 Uiso 1 1 calc R . . C26 C 0.4331(12) 0.8586(7) 0.7103(4) 0.028(3) Uani 1 1 d . . . H26 H 0.4561 0.8993 0.7247 0.034 Uiso 1 1 calc R . . C44 C 0.2976(14) 0.5713(8) 0.7212(5) 0.035(4) Uani 1 1 d . . . C40 C 0.6039(13) 0.7203(9) 0.7976(4) 0.037(4) Uani 1 1 d . . . C13 C 0.3787(13) 0.8736(7) 0.5923(5) 0.032(3) Uani 1 1 d . . . H13 H 0.4283 0.9107 0.6009 0.038 Uiso 1 1 calc R . . O7 O 0.3710(8) 0.7583(5) 0.5667(3) 0.024(2) Uani 1 1 d . . . C29 C 0.6663(14) 0.8936(8) 0.7208(5) 0.037(4) Uani 1 1 d U . . H29A H 0.6337 0.9354 0.7077 0.056 Uiso 1 1 calc R . . H29B H 0.7498 0.8952 0.7227 0.056 Uiso 1 1 calc R . . H29C H 0.6444 0.8907 0.7474 0.056 Uiso 1 1 calc R . . C55 C 0.4507(13) 0.8531(8) 0.9975(4) 0.031(3) Uani 1 1 d . . . H55A H 0.4511 0.8060 1.0077 0.047 Uiso 1 1 calc R . . H55B H 0.4288 0.8849 1.0174 0.047 Uiso 1 1 calc R . . H55C H 0.5272 0.8649 0.9917 0.047 Uiso 1 1 calc R . . F3 F 0.4347(9) 0.5507(5) 0.6246(4) 0.080(5) Uani 1 1 d . . . C57 C 0.4478(13) 0.7448(7) 0.9367(5) 0.033(3) Uani 1 1 d . . . H57A H 0.4018 0.7192 0.9535 0.049 Uiso 1 1 calc R . . H57B H 0.5234 0.7542 0.9515 0.049 Uiso 1 1 calc R . . H57C H 0.4563 0.7174 0.9132 0.049 Uiso 1 1 calc R . . C17 C 0.2808(10) 0.7801(6) 0.6850(4) 0.017(3) Uani 1 1 d . . . C15 C 0.5478(14) 0.8213(8) 0.5676(6) 0.041(4) Uani 1 1 d . . . F29 F 0.6414(10) 0.7611(9) 0.7726(4) 0.095(6) Uani 1 1 d . . . O11 O 0.2104(8) 0.8404(5) 0.9987(2) 0.0215(19) Uani 1 1 d U . . F31 F -0.0978(8) 0.9651(5) 0.8348(3) 0.048(3) Uani 1 1 d . . . F32 F -0.1606(8) 0.8791(6) 0.7996(3) 0.052(3) Uani 1 1 d . . . F7 F -0.1475(10) 0.8849(6) 0.5646(3) 0.055(3) Uani 1 1 d . . . F30 F 0.6292(9) 0.7447(7) 0.8325(4) 0.070(4) Uani 1 1 d . . . F33 F -0.1052(9) 0.8675(6) 0.8628(3) 0.054(3) Uani 1 1 d . . . F8 F -0.1914(9) 0.9087(6) 0.5029(3) 0.057(3) Uani 1 1 d . . . F34 F 0.4048(9) 0.9753(5) 0.8183(4) 0.060(3) Uani 1 1 d . . . F9 F -0.2253(9) 0.8095(6) 0.5245(5) 0.075(4) Uani 1 1 d . . . N4 N 0.2507(9) 0.8294(5) 0.9663(3) 0.018(2) Uani 1 1 d . . . F12 F 0.2909(12) 0.9375(7) 0.4891(4) 0.077(4) Uani 1 1 d . . . F35 F 0.3109(10) 0.9892(6) 0.7617(3) 0.057(3) Uani 1 1 d . . . F36 F 0.2593(10) 1.0436(5) 0.8107(4) 0.066(4) Uani 1 1 d . . . C10 C -0.1512(13) 0.8592(8) 0.5281(5) 0.037(4) Uani 1 1 d U . . C34 C 0.3001(13) 0.9840(7) 0.8012(5) 0.037(4) Uani 1 1 d . . . Br2 Br -0.22548(12) 0.83947(8) 0.96909(5) 0.0353(4) Uani 1 1 d . . . F17 F 0.5887(8) 0.7600(5) 0.5621(3) 0.048(3) Uani 1 1 d . . . C49 C -0.1170(11) 0.7896(7) 0.9439(4) 0.027(3) Uani 1 1 d . . . C33 C 0.2224(12) 0.9217(6) 0.8075(4) 0.022(3) Uani 1 1 d . . . C14 C 0.4211(12) 0.8167(7) 0.5750(4) 0.027(3) Uani 1 1 d . . . F18 F 0.5491(10) 0.8553(8) 0.5346(5) 0.093(5) Uani 1 1 d . . . F16 F 0.6142(9) 0.8501(6) 0.5973(4) 0.076(4) Uani 1 1 d . . . F20 F 0.4461(11) 0.5317(7) 0.8420(3) 0.074(4) Uani 1 1 d . . . F21 F 0.3313(12) 0.4830(6) 0.8761(5) 0.099(6) 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 Gd1 0.0183(3) 0.0161(3) 0.0161(3) -0.0003(2) 0.0051(2) -0.0005(2) Gd2 0.0193(3) 0.0183(3) 0.0163(3) -0.0019(2) 0.0042(2) 0.0001(2) Br1 0.0179(7) 0.0404(8) 0.0535(10) -0.0181(7) 0.0077(6) 0.0006(6) O4 0.033(5) 0.019(5) 0.023(5) 0.003(4) 0.011(4) 0.002(4) F1 0.043(5) 0.025(5) 0.063(6) 0.022(4) 0.004(5) 0.003(4) O8 0.025(5) 0.018(5) 0.021(5) 0.000(4) 0.005(4) 0.002(4) F25 0.051(6) 0.039(5) 0.025(5) -0.001(4) 0.014(4) -0.004(4) O5 0.028(5) 0.018(5) 0.039(6) 0.006(4) 0.006(4) 0.007(4) F4 0.037(5) 0.037(5) 0.086(8) -0.022(5) 0.026(5) -0.010(4) N2 0.015(5) 0.026(6) 0.013(5) 0.001(4) -0.001(4) -0.001(4) O13 0.033(5) 0.018(5) 0.027(5) 0.005(4) 0.002(4) -0.004(4) O15 0.027(5) 0.026(5) 0.027(5) -0.002(4) 0.007(4) 0.004(4) O6 0.020(5) 0.021(5) 0.034(6) 0.001(4) 0.008(4) -0.001(4) O14 0.032(5) 0.015(5) 0.023(5) -0.006(4) 0.009(4) -0.003(4) O16 0.017(4) 0.014(4) 0.026(5) -0.004(4) 0.009(4) -0.001(3) O17 0.022(5) 0.017(5) 0.026(5) -0.002(4) 0.004(4) 0.000(4) F5 0.038(5) 0.075(7) 0.039(6) -0.014(5) 0.002(4) -0.021(5) O1 0.029(5) 0.023(5) 0.016(5) 0.000(4) 0.005(4) 0.001(4) O9 0.025(5) 0.025(5) 0.027(5) 0.002(4) 0.007(4) 0.002(4) N1 0.024(6) 0.023(6) 0.014(6) -0.001(4) 0.004(4) -0.004(5) O18 0.031(5) 0.014(4) 0.020(4) -0.004(3) 0.013(4) 0.006(3) F19 0.046(6) 0.053(6) 0.041(6) 0.005(5) -0.002(5) 0.016(5) O10 0.032(5) 0.048(6) 0.011(5) -0.013(4) 0.007(4) -0.009(5) N3 0.024(6) 0.034(7) 0.022(6) -0.001(5) 0.006(5) -0.009(5) O12 0.044(7) 0.022(5) 0.049(7) -0.012(5) 0.015(5) -0.006(5) F6 0.039(6) 0.037(5) 0.094(8) 0.037(5) -0.002(5) -0.017(4) F10 0.055(6) 0.039(5) 0.052(6) 0.003(4) 0.029(5) -0.004(5) F22 0.044(6) 0.027(5) 0.072(7) -0.002(5) 0.009(5) -0.015(4) C4 0.027(7) 0.019(7) 0.023(7) -0.008(5) 0.010(6) 0.001(5) F26 0.077(7) 0.014(4) 0.059(6) -0.009(4) 0.028(6) -0.011(4) C56 0.024(7) 0.024(7) 0.019(7) -0.008(5) 0.009(5) -0.008(5) C53 0.017(6) 0.026(7) 0.020(7) -0.006(5) 0.006(5) 0.000(5) C52 0.013(6) 0.009(5) 0.019(6) -0.001(5) 0.000(5) 0.002(4) C1 0.016(7) 0.030(8) 0.039(9) -0.012(6) 0.004(6) -0.007(6) C58 0.032(8) 0.039(8) 0.025(8) -0.001(6) 0.015(6) 0.000(6) O3 0.017(5) 0.031(5) 0.028(5) -0.008(4) 0.002(4) -0.002(4) C16 0.020(7) 0.032(8) 0.025(7) 0.001(6) 0.004(6) 0.005(6) C12 0.029(8) 0.040(9) 0.021(7) 0.002(6) 0.001(6) -0.003(6) O2 0.024(5) 0.024(5) 0.015(5) -0.003(4) -0.001(4) -0.005(4) F13 0.044(6) 0.036(5) 0.070(7) -0.027(5) 0.003(5) -0.011(4) C18 0.017(6) 0.019(6) 0.019(7) -0.003(5) -0.006(5) 0.003(5) C28 0.022(7) 0.015(6) 0.020(7) 0.002(5) 0.001(5) -0.004(5) F24 0.104(10) 0.068(8) 0.059(8) 0.034(6) -0.034(7) -0.055(7) F23 0.034(6) 0.066(7) 0.106(10) -0.032(7) 0.036(6) -0.003(5) F2 0.061(7) 0.085(8) 0.083(8) 0.044(7) 0.053(7) 0.051(6) F27 0.077(8) 0.040(6) 0.061(7) -0.017(5) 0.008(6) 0.031(5) C25 0.023(7) 0.015(6) 0.027(7) -0.008(5) 0.008(5) -0.003(5) C2 0.022(6) 0.009(5) 0.016(5) -0.009(4) 0.001(4) -0.004(4) C22 0.009(5) 0.016(6) 0.013(6) -0.003(5) 0.003(4) 0.004(4) C47 0.020(7) 0.036(8) 0.034(8) 0.019(7) 0.009(6) 0.000(6) C35 0.044(10) 0.025(8) 0.051(11) 0.003(7) -0.006(8) 0.000(7) C27 0.024(7) 0.028(7) 0.028(8) -0.006(6) 0.000(6) -0.002(6) C7 0.049(9) 0.024(7) 0.019(7) 0.002(6) 0.012(6) 0.001(7) F14 0.071(7) 0.040(6) 0.063(7) -0.013(5) 0.039(6) 0.003(5) C36 0.037(8) 0.023(7) 0.016(7) 0.004(5) 0.004(6) 0.005(6) C37 0.059(11) 0.023(8) 0.028(8) 0.004(6) 0.016(7) -0.004(7) C54 0.032(8) 0.021(7) 0.052(10) 0.003(7) 0.009(7) -0.001(6) C11 0.045(9) 0.023(7) 0.030(8) 0.002(6) 0.010(7) -0.014(7) C23 0.028(8) 0.041(9) 0.023(8) 0.002(6) 0.005(6) 0.015(6) C30 0.023(7) 0.028(7) 0.032(8) 0.006(6) 0.006(6) 0.007(6) C50 0.012(6) 0.023(7) 0.040(8) 0.005(6) 0.013(6) 0.007(5) F11 0.082(8) 0.038(6) 0.070(7) 0.027(5) 0.037(6) 0.022(5) C9 0.014(6) 0.029(8) 0.027(8) -0.010(6) -0.001(5) 0.000(5) C41 0.023(7) 0.045(9) 0.033(8) 0.016(7) 0.014(6) 0.008(7) C21 0.028(8) 0.035(8) 0.044(10) 0.004(7) 0.012(7) 0.001(6) C45 0.027(7) 0.029(8) 0.030(8) 0.001(6) 0.006(6) -0.003(6) C5 0.040(9) 0.028(8) 0.046(10) 0.009(7) 0.010(8) 0.021(7) C20 0.018(7) 0.035(8) 0.028(8) 0.005(6) -0.001(6) 0.006(6) C48 0.029(6) 0.028(6) 0.052(8) -0.005(6) 0.010(6) -0.011(5) C43 0.046(9) 0.019(7) 0.017(7) 0.008(5) 0.014(6) 0.013(6) C31 0.018(7) 0.037(8) 0.016(7) 0.000(6) -0.003(5) 0.002(6) F28 0.034(6) 0.077(8) 0.109(10) -0.026(7) -0.009(6) 0.023(6) C19 0.017(6) 0.029(7) 0.021(7) -0.002(6) 0.007(5) -0.003(5) C51 0.018(6) 0.011(6) 0.023(7) 0.003(5) -0.004(5) 0.004(5) C32 0.037(8) 0.011(6) 0.038(9) -0.001(6) 0.011(7) 0.006(6) C39 0.030(8) 0.032(8) 0.027(8) -0.002(6) 0.013(6) -0.002(6) C3 0.045(9) 0.020(7) 0.020(7) 0.010(6) -0.010(6) 0.003(6) C46 0.037(8) 0.020(7) 0.019(7) -0.005(5) 0.009(6) -0.004(6) C6 0.043(9) 0.020(7) 0.040(9) 0.007(6) 0.012(7) -0.005(6) C38 0.030(7) 0.019(7) 0.014(6) -0.006(5) 0.013(5) -0.004(5) F15 0.059(7) 0.040(6) 0.062(7) -0.004(5) -0.004(5) 0.019(5) C8 0.031(8) 0.020(7) 0.027(8) 0.006(6) -0.003(6) 0.011(6) C42 0.032(8) 0.032(8) 0.025(8) -0.007(6) 0.007(6) 0.011(6) C24 0.024(7) 0.043(9) 0.017(7) 0.001(6) 0.007(6) -0.002(6) C26 0.030(8) 0.028(7) 0.026(8) -0.013(6) 0.001(6) -0.009(6) C44 0.042(9) 0.029(8) 0.036(9) -0.010(7) 0.006(7) 0.007(7) C40 0.028(8) 0.065(11) 0.015(7) 0.012(7) -0.001(6) 0.015(8) C13 0.030(8) 0.026(7) 0.040(9) 0.001(6) 0.006(7) -0.016(6) O7 0.020(5) 0.027(5) 0.025(5) 0.005(4) 0.003(4) -0.002(4) C29 0.036(7) 0.031(6) 0.044(7) -0.008(6) 0.002(6) -0.019(6) C55 0.034(8) 0.033(8) 0.029(8) -0.009(6) 0.011(6) 0.003(6) F3 0.041(6) 0.037(6) 0.142(12) 0.004(7) -0.051(7) 0.001(5) C57 0.027(8) 0.029(8) 0.041(9) -0.011(7) 0.004(7) 0.004(6) C17 0.012(6) 0.020(6) 0.019(7) 0.002(5) 0.005(5) -0.002(5) C15 0.037(9) 0.019(7) 0.062(12) -0.004(7) -0.015(8) 0.000(6) F29 0.045(7) 0.148(13) 0.088(10) 0.073(10) -0.007(6) -0.039(8) O11 0.028(5) 0.029(5) 0.009(4) 0.000(3) 0.009(3) 0.002(4) F31 0.043(6) 0.035(5) 0.073(7) 0.002(5) 0.030(5) 0.023(4) F32 0.026(5) 0.065(7) 0.059(7) -0.023(5) -0.013(4) 0.009(4) F7 0.065(7) 0.065(7) 0.042(6) 0.006(5) 0.025(5) 0.033(6) F30 0.035(6) 0.093(9) 0.082(9) -0.023(7) 0.002(6) -0.003(6) F33 0.050(6) 0.069(7) 0.050(6) 0.031(5) 0.031(5) 0.028(5) F8 0.056(7) 0.070(7) 0.046(6) 0.011(5) 0.006(5) 0.038(6) F34 0.034(6) 0.038(6) 0.105(9) 0.009(6) 0.006(6) -0.013(4) F9 0.025(5) 0.046(6) 0.161(13) 0.002(7) 0.032(7) 0.005(5) N4 0.026(6) 0.015(5) 0.017(6) 0.001(4) 0.015(5) 0.009(4) F12 0.087(9) 0.079(8) 0.061(8) 0.010(6) 0.000(7) -0.055(7) F35 0.072(8) 0.057(7) 0.045(6) 0.009(5) 0.021(5) -0.015(6) F36 0.073(8) 0.021(5) 0.115(10) -0.016(6) 0.047(7) -0.008(5) C10 0.029(6) 0.039(7) 0.044(7) 0.008(6) 0.009(6) 0.011(6) C34 0.032(8) 0.010(7) 0.068(12) -0.006(7) 0.004(8) 0.003(6) Br2 0.0215(7) 0.0323(8) 0.0542(10) -0.0110(7) 0.0126(7) 0.0014(6) F17 0.029(5) 0.043(6) 0.073(7) -0.015(5) 0.011(5) 0.001(4) C49 0.012(6) 0.031(8) 0.037(8) 0.000(6) 0.002(6) 0.007(5) C33 0.029(7) 0.007(6) 0.027(7) 0.005(5) 0.000(6) 0.003(5) C14 0.026(7) 0.031(8) 0.024(8) 0.012(6) 0.003(6) 0.005(6) F18 0.048(7) 0.112(11) 0.133(13) 0.074(10) 0.056(8) 0.020(7) F16 0.030(6) 0.063(7) 0.130(12) -0.041(7) -0.008(6) -0.017(5) F20 0.072(8) 0.096(10) 0.053(7) -0.009(6) 0.009(6) 0.045(7) F21 0.073(9) 0.051(7) 0.157(14) 0.061(8) -0.041(9) -0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4 2.346(10) . ? Gd1 O7 2.371(9) . ? Gd1 O6 2.371(9) . ? Gd1 O9 2.380(9) . ? Gd1 O5 2.383(10) . ? Gd1 O1 2.387(9) . ? Gd1 O8 2.389(9) . ? Gd1 O11 2.398(8) 4_575 ? Gd2 O10 2.335(9) . ? Gd2 O17 2.359(9) . ? Gd2 O14 2.372(9) . ? Gd2 O15 2.379(9) . ? Gd2 O16 2.388(9) . ? Gd2 O18 2.402(8) . ? Gd2 O2 2.403(9) . ? Gd2 O13 2.435(9) . ? Br1 C28 1.881(13) . ? O4 C9 1.249(17) . ? F1 C5 1.299(18) . ? O8 C2 1.265(15) . ? F25 C44 1.306(18) . ? O5 C7 1.233(17) . ? F4 C1 1.325(17) . ? N2 O2 1.277(13) . ? N2 C18 1.346(17) . ? N2 C22 1.505(15) . ? O13 C36 1.248(16) . ? O15 C43 1.269(17) . ? O6 C12 1.284(18) . ? O14 C38 1.265(16) . ? O16 C41 1.254(17) . ? O17 C33 1.254(15) . ? F5 C1 1.326(17) . ? O1 N1 1.266(14) . ? O9 C4 1.268(16) . ? N1 C18 1.339(16) . ? N1 C19 1.543(16) . ? O18 C31 1.234(17) . ? F19 C35 1.336(19) . ? O10 N3 1.298(14) . ? N3 C52 1.351(16) . ? N3 C56 1.507(17) . ? O12 C47 1.328(18) . ? O12 C48 1.483(17) . ? F6 C1 1.345(18) . ? F10 C6 1.350(18) . ? F22 C39 1.340(17) . ? C4 C3 1.37(2) . ? C4 C5 1.560(19) . ? F26 C44 1.361(19) . ? C56 C57 1.49(2) . ? C56 C58 1.540(18) . ? C56 C53 1.572(17) . ? C53 N4 1.505(16) . ? C53 C54 1.523(19) . ? C53 C55 1.54(2) . ? C52 N4 1.332(16) . ? C52 C51 1.470(17) . ? C1 C2 1.549(17) . ? O3 C27 1.296(17) . ? O3 C29 1.453(17) . ? C16 C17 1.396(18) . ? C16 C28 1.422(19) . ? C12 C13 1.40(2) . ? C12 C11 1.56(2) . ? F13 C11 1.333(17) . ? C18 C17 1.489(17) . ? C28 C27 1.426(19) . ? F24 C39 1.306(18) . ? F23 C39 1.347(17) . ? F2 C5 1.365(19) . ? F27 C44 1.340(18) . ? C25 C17 1.365(18) . ? C25 C26 1.443(19) . ? C2 C3 1.399(19) . ? C22 C19 1.539(17) . ? C22 C23 1.550(18) . ? C22 C24 1.550(17) . ? C47 C49 1.39(2) . ? C47 C46 1.44(2) . ? C35 F21 1.31(2) . ? C35 F20 1.34(2) . ? C35 C36 1.51(2) . ? C27 C26 1.40(2) . ? C7 C8 1.43(2) . ? C7 C6 1.51(2) . ? F14 C11 1.317(18) . ? C36 C37 1.45(2) . ? C37 C38 1.39(2) . ? C11 F15 1.344(18) . ? C30 F33 1.316(17) . ? C30 F31 1.320(17) . ? C30 F32 1.370(17) . ? C30 C31 1.561(19) . ? C50 C49 1.389(19) . ? C50 C51 1.428(18) . ? F11 C6 1.343(18) . ? C9 C8 1.42(2) . ? C9 C10 1.549(19) . ? C41 C42 1.42(2) . ? C41 C40 1.55(2) . ? C21 C19 1.54(2) . ? C45 C51 1.414(19) . ? C45 C46 1.42(2) . ? C5 F3 1.30(2) . ? C20 C19 1.540(19) . ? C43 C42 1.38(2) . ? C43 C44 1.54(2) . ? C31 C32 1.42(2) . ? F28 C40 1.353(19) . ? C32 C33 1.36(2) . ? C39 C38 1.51(2) . ? C6 F12 1.316(19) . ? C40 F30 1.281(19) . ? C40 F29 1.287(19) . ? C13 C14 1.38(2) . ? O7 C14 1.294(17) . ? C15 F18 1.31(2) . ? C15 F17 1.309(18) . ? C15 F16 1.318(19) . ? C15 C14 1.56(2) . ? O11 N4 1.282(13) . ? O11 Gd1 2.398(8) 4_576 ? F7 C10 1.339(19) . ? F8 C10 1.334(18) . ? F34 C34 1.303(19) . ? F9 C10 1.30(2) . ? F35 C34 1.38(2) . ? F36 C34 1.314(17) . ? C34 C33 1.553(19) . ? Br2 C49 1.908(14) . ? 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 O4 Gd1 O7 137.1(3) . . ? O4 Gd1 O6 73.8(3) . . ? O7 Gd1 O6 72.6(3) . . ? O4 Gd1 O9 148.3(3) . . ? O7 Gd1 O9 74.0(3) . . ? O6 Gd1 O9 122.6(3) . . ? O4 Gd1 O5 72.9(3) . . ? O7 Gd1 O5 74.0(3) . . ? O6 Gd1 O5 76.8(3) . . ? O9 Gd1 O5 134.1(3) . . ? O4 Gd1 O1 92.3(3) . . ? O7 Gd1 O1 102.1(3) . . ? O6 Gd1 O1 72.3(3) . . ? O9 Gd1 O1 70.8(3) . . ? O5 Gd1 O1 148.4(3) . . ? O4 Gd1 O8 76.0(3) . . ? O7 Gd1 O8 146.7(3) . . ? O6 Gd1 O8 133.5(3) . . ? O9 Gd1 O8 73.7(3) . . ? O5 Gd1 O8 125.8(3) . . ? O1 Gd1 O8 74.5(3) . . ? O4 Gd1 O11 105.5(3) . 4_575 ? O7 Gd1 O11 90.5(3) . 4_575 ? O6 Gd1 O11 149.1(3) . 4_575 ? O9 Gd1 O11 74.5(3) . 4_575 ? O5 Gd1 O11 73.7(3) . 4_575 ? O1 Gd1 O11 137.8(3) . 4_575 ? O8 Gd1 O11 73.3(3) . 4_575 ? O10 Gd2 O17 81.1(3) . . ? O10 Gd2 O14 94.8(3) . . ? O17 Gd2 O14 150.8(3) . . ? O10 Gd2 O15 144.8(4) . . ? O17 Gd2 O15 123.5(3) . . ? O14 Gd2 O15 75.2(3) . . ? O10 Gd2 O16 94.0(3) . . ? O17 Gd2 O16 73.1(3) . . ? O14 Gd2 O16 136.1(3) . . ? O15 Gd2 O16 73.1(3) . . ? O10 Gd2 O18 72.8(3) . . ? O17 Gd2 O18 72.8(3) . . ? O14 Gd2 O18 78.3(3) . . ? O15 Gd2 O18 134.8(3) . . ? O16 Gd2 O18 145.0(3) . . ? O10 Gd2 O2 141.0(3) . . ? O17 Gd2 O2 73.5(3) . . ? O14 Gd2 O2 93.3(3) . . ? O15 Gd2 O2 74.1(3) . . ? O16 Gd2 O2 106.1(3) . . ? O18 Gd2 O2 71.6(3) . . ? O10 Gd2 O13 69.1(4) . . ? O17 Gd2 O13 131.3(3) . . ? O14 Gd2 O13 71.7(3) . . ? O15 Gd2 O13 75.8(3) . . ? O16 Gd2 O13 71.6(3) . . ? O18 Gd2 O13 128.3(3) . . ? O2 Gd2 O13 148.9(3) . . ? C9 O4 Gd1 133.5(9) . . ? C2 O8 Gd1 132.4(8) . . ? C7 O5 Gd1 133.4(9) . . ? O2 N2 C18 127.0(10) . . ? O2 N2 C22 122.1(10) . . ? C18 N2 C22 110.9(10) . . ? C36 O13 Gd2 135.1(9) . . ? C43 O15 Gd2 131.2(9) . . ? C12 O6 Gd1 133.7(9) . . ? C38 O14 Gd2 135.4(9) . . ? C41 O16 Gd2 130.3(9) . . ? C33 O17 Gd2 135.0(9) . . ? N1 O1 Gd1 145.3(8) . . ? C4 O9 Gd1 133.1(9) . . ? O1 N1 C18 126.4(11) . . ? O1 N1 C19 121.7(10) . . ? C18 N1 C19 111.5(10) . . ? C31 O18 Gd2 133.1(9) . . ? N3 O10 Gd2 166.7(9) . . ? O10 N3 C52 125.1(11) . . ? O10 N3 C56 121.5(10) . . ? C52 N3 C56 112.9(10) . . ? C47 O12 C48 117.7(12) . . ? O9 C4 C3 129.4(13) . . ? O9 C4 C5 113.4(12) . . ? C3 C4 C5 117.2(12) . . ? C57 C56 N3 107.0(11) . . ? C57 C56 C58 110.6(12) . . ? N3 C56 C58 111.0(11) . . ? C57 C56 C53 115.0(12) . . ? N3 C56 C53 98.4(10) . . ? C58 C56 C53 113.9(11) . . ? N4 C53 C54 106.0(10) . . ? N4 C53 C55 109.9(11) . . ? C54 C53 C55 110.4(12) . . ? N4 C53 C56 99.9(10) . . ? C54 C53 C56 114.5(12) . . ? C55 C53 C56 115.2(11) . . ? N4 C52 N3 107.6(11) . . ? N4 C52 C51 126.3(11) . . ? N3 C52 C51 126.0(11) . . ? F4 C1 F5 105.6(12) . . ? F4 C1 F6 105.4(12) . . ? F5 C1 F6 107.3(12) . . ? F4 C1 C2 111.7(11) . . ? F5 C1 C2 112.9(12) . . ? F6 C1 C2 113.3(12) . . ? C27 O3 C29 119.1(11) . . ? C17 C16 C28 118.2(13) . . ? O6 C12 C13 128.6(14) . . ? O6 C12 C11 111.8(12) . . ? C13 C12 C11 119.6(13) . . ? N2 O2 Gd2 135.4(8) . . ? N1 C18 N2 109.4(11) . . ? N1 C18 C17 126.4(12) . . ? N2 C18 C17 124.1(11) . . ? C16 C28 C27 122.7(12) . . ? C16 C28 Br1 119.0(10) . . ? C27 C28 Br1 118.2(10) . . ? C17 C25 C26 119.5(12) . . ? O8 C2 C3 129.0(12) . . ? O8 C2 C1 113.9(11) . . ? C3 C2 C1 117.1(11) . . ? N2 C22 C19 101.6(9) . . ? N2 C22 C23 107.2(10) . . ? C19 C22 C23 113.4(11) . . ? N2 C22 C24 111.0(10) . . ? C19 C22 C24 113.5(10) . . ? C23 C22 C24 109.7(10) . . ? O12 C47 C49 119.7(13) . . ? O12 C47 C46 123.7(14) . . ? C49 C47 C46 116.5(12) . . ? F21 C35 F19 106.9(15) . . ? F21 C35 F20 107.1(16) . . ? F19 C35 F20 104.8(14) . . ? F21 C35 C36 115.4(14) . . ? F19 C35 C36 111.9(13) . . ? F20 C35 C36 110.2(14) . . ? O3 C27 C26 125.1(13) . . ? O3 C27 C28 118.9(12) . . ? C26 C27 C28 116.0(12) . . ? O5 C7 C8 127.4(13) . . ? O5 C7 C6 116.4(14) . . ? C8 C7 C6 116.2(13) . . ? O13 C36 C37 126.2(13) . . ? O13 C36 C35 115.7(13) . . ? C37 C36 C35 118.1(13) . . ? C38 C37 C36 121.7(13) . . ? F14 C11 F13 108.5(13) . . ? F14 C11 F15 107.0(14) . . ? F13 C11 F15 106.9(12) . . ? F14 C11 C12 112.9(12) . . ? F13 C11 C12 112.2(13) . . ? F15 C11 C12 109.0(12) . . ? F33 C30 F31 108.1(12) . . ? F33 C30 F32 108.3(13) . . ? F31 C30 F32 104.9(11) . . ? F33 C30 C31 112.3(11) . . ? F31 C30 C31 114.6(12) . . ? F32 C30 C31 108.3(11) . . ? C49 C50 C51 117.5(13) . . ? O4 C9 C8 127.7(12) . . ? O4 C9 C10 114.9(12) . . ? C8 C9 C10 117.3(12) . . ? O16 C41 C42 129.8(14) . . ? O16 C41 C40 111.6(14) . . ? C42 C41 C40 118.6(13) . . ? C51 C45 C46 119.4(13) . . ? F1 C5 F3 109.1(14) . . ? F1 C5 F2 106.1(12) . . ? F3 C5 F2 107.4(15) . . ? F1 C5 C4 115.1(13) . . ? F3 C5 C4 112.2(12) . . ? F2 C5 C4 106.4(12) . . ? O15 C43 C42 128.7(13) . . ? O15 C43 C44 112.2(13) . . ? C42 C43 C44 119.1(12) . . ? O18 C31 C32 129.3(13) . . ? O18 C31 C30 113.9(12) . . ? C32 C31 C30 116.8(12) . . ? C22 C19 C20 116.5(11) . . ? C22 C19 C21 114.2(11) . . ? C20 C19 C21 111.3(12) . . ? C22 C19 N1 99.6(9) . . ? C20 C19 N1 110.0(10) . . ? C21 C19 N1 103.7(11) . . ? C45 C51 C50 120.7(12) . . ? C45 C51 C52 119.7(12) . . ? C50 C51 C52 119.4(11) . . ? C33 C32 C31 120.8(12) . . ? F24 C39 F22 104.6(12) . . ? F24 C39 F23 107.4(14) . . ? F22 C39 F23 104.9(12) . . ? F24 C39 C38 113.8(12) . . ? F22 C39 C38 114.2(12) . . ? F23 C39 C38 111.3(12) . . ? C4 C3 C2 121.6(12) . . ? C45 C46 C47 120.7(13) . . ? F12 C6 F11 107.0(13) . . ? F12 C6 F10 106.8(14) . . ? F11 C6 F10 105.6(13) . . ? F12 C6 C7 110.8(13) . . ? F11 C6 C7 115.5(14) . . ? F10 C6 C7 110.6(12) . . ? O14 C38 C37 127.6(13) . . ? O14 C38 C39 114.0(12) . . ? C37 C38 C39 118.4(12) . . ? C9 C8 C7 120.4(12) . . ? C43 C42 C41 120.3(13) . . ? C27 C26 C25 121.7(12) . . ? F25 C44 F27 108.8(13) . . ? F25 C44 F26 108.3(13) . . ? F27 C44 F26 105.0(13) . . ? F25 C44 C43 111.9(12) . . ? F27 C44 C43 113.0(13) . . ? F26 C44 C43 109.6(12) . . ? F30 C40 F29 109.4(17) . . ? F30 C40 F28 103.7(12) . . ? F29 C40 F28 107.1(15) . . ? F30 C40 C41 114.2(13) . . ? F29 C40 C41 111.0(12) . . ? F28 C40 C41 111.0(15) . . ? C14 C13 C12 120.6(13) . . ? C14 O7 Gd1 133.0(9) . . ? C25 C17 C16 121.8(12) . . ? C25 C17 C18 118.5(11) . . ? C16 C17 C18 119.5(12) . . ? F18 C15 F17 106.8(16) . . ? F18 C15 F16 111.7(16) . . ? F17 C15 F16 107.8(13) . . ? F18 C15 C14 107.2(12) . . ? F17 C15 C14 110.7(13) . . ? F16 C15 C14 112.4(15) . . ? N4 O11 Gd1 137.3(7) . 4_576 ? O11 N4 C52 125.7(11) . . ? O11 N4 C53 121.4(10) . . ? C52 N4 C53 112.5(10) . . ? F9 C10 F8 107.6(14) . . ? F9 C10 F7 107.4(14) . . ? F8 C10 F7 107.1(13) . . ? F9 C10 C9 111.5(13) . . ? F8 C10 C9 112.7(13) . . ? F7 C10 C9 110.3(13) . . ? F34 C34 F36 111.3(14) . . ? F34 C34 F35 103.5(14) . . ? F36 C34 F35 105.4(13) . . ? F34 C34 C33 112.4(12) . . ? F36 C34 C33 114.2(13) . . ? F35 C34 C33 109.2(12) . . ? C50 C49 C47 124.8(13) . . ? C50 C49 Br2 117.7(11) . . ? C47 C49 Br2 117.5(10) . . ? O17 C33 C32 128.9(12) . . ? O17 C33 C34 112.4(12) . . ? C32 C33 C34 118.6(11) . . ? O7 C14 C13 127.8(13) . . ? O7 C14 C15 115.9(12) . . ? C13 C14 C15 116.1(13) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.473 _refine_diff_density_min -1.803 _refine_diff_density_rms 0.192 _database_code_depnum_ccdc_archive 'CCDC 958923' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Tb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H42 Br2 F36 N4 O18 Tb2' _chemical_formula_weight 2244.62 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' 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8487(14) _cell_length_b 19.418(2) _cell_length_c 34.089(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.844(6) _cell_angle_gamma 90.00 _cell_volume 7769.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 17229 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.1 _exptl_crystal_description Prism _exptl_crystal_colour Darkgreen _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4344 _exptl_absorpt_coefficient_mu 2.987 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48668 _diffrn_reflns_av_R_equivalents 0.1869 _diffrn_reflns_av_sigmaI/netI 0.1770 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13017 _reflns_number_gt 9573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13017 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1387 _refine_ls_R_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.2657 _refine_ls_wR_factor_gt 0.2476 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.82037(5) 0.72261(3) 0.443202(17) 0.0260(2) Uani 1 1 d . . . Tb2 Tb 0.78549(5) 0.75392(3) 0.694840(17) 0.0272(2) Uani 1 1 d . . . Br2 Br 0.41281(13) 0.80758(8) 0.84036(5) 0.0469(4) Uani 1 1 d . . . O10 O 0.7286(8) 0.6402(5) 0.6955(3) 0.037(2) Uani 1 1 d . . . O6 O 0.9965(8) 0.7747(4) 0.4598(2) 0.031(2) Uani 1 1 d . . . O2 O 0.7958(8) 0.8043(5) 0.4925(3) 0.037(2) Uani 1 1 d . . . F35 F 0.7493(8) 0.9147(4) 0.8129(2) 0.044(2) Uani 1 1 d . . . O3 O 0.7905(8) 0.6592(5) 0.5008(2) 0.034(2) Uani 1 1 d . . . O14 O 0.6979(9) 0.8518(5) 0.6593(3) 0.041(2) Uani 1 1 d . . . O15 O 0.9265(8) 0.8372(4) 0.6926(2) 0.030(2) Uani 1 1 d . . . O1 O 0.9535(8) 0.6303(4) 0.4500(2) 0.029(2) Uani 1 1 d . . . N2 N 0.9082(9) 0.7282(5) 0.7910(3) 0.024(2) Uani 1 1 d . . . O11 O 0.5896(9) 0.7533(4) 0.7007(3) 0.033(2) Uani 1 1 d . . . O13 O 0.7587(8) 0.8331(5) 0.7446(2) 0.036(2) Uani 1 1 d . . . N1 N 0.9007(9) 0.7753(5) 0.8484(3) 0.027(2) Uani 1 1 d . . . O17 O 0.8591(8) 0.8012(4) 0.8788(2) 0.030(2) Uani 1 1 d . . . F34 F 0.7766(9) 0.9717(4) 0.7608(2) 0.056(2) Uani 1 1 d . . . F9 F 0.8443(9) 0.9760(5) 0.4130(3) 0.067(3) Uani 1 1 d . . . C19 C 1.1167(12) 0.7134(7) 0.5549(4) 0.034(3) Uani 1 1 d . . . C18 C 1.1535(12) 0.7724(8) 0.5762(4) 0.035(3) Uani 1 1 d . . . F6 F 1.0987(9) 0.5204(6) 0.4819(3) 0.070(3) Uani 1 1 d . . . F8 F 0.8447(10) 0.9263(5) 0.3561(3) 0.068(3) Uani 1 1 d . . . C23 C 0.8078(12) 0.7024(6) 0.5650(4) 0.030(3) Uani 1 1 d . . . F7 F 0.6967(9) 0.9821(4) 0.3686(3) 0.062(3) Uani 1 1 d . . . O4 O 0.7155(7) 0.6237(4) 0.4190(2) 0.0295(19) Uani 1 1 d . . . O5 O 0.6271(9) 0.7556(5) 0.4326(3) 0.036(2) Uani 1 1 d . . . C11 C 1.0659(14) 0.5308(8) 0.4442(4) 0.044(4) Uani 1 1 d . . . C33 C 0.7299(14) 0.9128(8) 0.6531(4) 0.044(4) Uani 1 1 d . . . C42 C 1.0194(12) 0.7907(6) 0.8413(4) 0.032(3) Uani 1 1 d . . . O16 O 0.3701(9) 0.6701(5) 0.8009(3) 0.044(2) Uani 1 1 d . . . F4 F 1.0575(9) 0.4685(5) 0.4266(3) 0.075(3) Uani 1 1 d . . . C25 C 0.6109(11) 0.6899(7) 0.5750(3) 0.028(3) Uani 1 1 d . . . F3 F 0.6712(8) 0.4610(4) 0.3790(3) 0.056(2) Uani 1 1 d . . . N3 N 0.7321(10) 0.7056(6) 0.5924(3) 0.035(3) Uani 1 1 d . . . F30 F 0.7428(10) 0.4601(5) 0.6898(4) 0.087(4) Uani 1 1 d . . . C50 C 0.4840(11) 0.6837(7) 0.8037(3) 0.030(3) Uani 1 1 d . . . C48 C 0.6344(12) 0.7664(7) 0.8286(4) 0.030(3) Uani 1 1 d . . . H48 H 0.6569 0.8075 0.8427 0.035 Uiso 1 1 calc R . . C51 C 0.5219(12) 0.7473(7) 0.8230(4) 0.034(3) Uani 1 1 d . . . C7 C 0.8546(13) 0.8585(7) 0.5045(4) 0.036(3) Uani 1 1 d U . . F28 F 0.6952(11) 0.5132(6) 0.7382(3) 0.075(3) Uani 1 1 d . . . F1 F 0.5971(10) 0.4937(6) 0.4298(3) 0.079(4) Uani 1 1 d . . . O7 O 1.2597(8) 0.7950(5) 0.5763(3) 0.039(2) Uani 1 1 d . . . F36 F 0.6117(9) 0.9726(5) 0.7804(3) 0.063(3) Uani 1 1 d . . . C12 C 0.9460(12) 0.5694(6) 0.4384(4) 0.030(3) Uani 1 1 d U . . C5FA C 0.7775(12) 0.5827(7) 0.6921(4) 0.033(3) Uani 1 1 d . . . C38 C 0.6696(12) 0.8678(7) 0.7503(4) 0.034(3) Uani 1 1 d . . . C14 C 0.7454(13) 0.5627(7) 0.4139(3) 0.034(3) Uani 1 1 d . . . F17 F 0.7482(10) 0.8740(5) 0.5578(3) 0.063(3) Uani 1 1 d . . . C20 C 1.0066(10) 0.6910(7) 0.5505(4) 0.027(3) Uani 1 1 d . . . H20 H 0.9843 0.6520 0.5345 0.033 Uiso 1 1 calc R . . C45 C 0.8355(13) 0.7425(7) 0.8170(4) 0.033(3) Uani 1 1 d . . . C3GA C 0.8865(12) 0.5696(7) 0.6827(4) 0.036(3) Uani 1 1 d . . . H3GA H 0.9089 0.5233 0.6792 0.044 Uiso 1 1 calc R . . F29 F 0.5975(9) 0.5273(6) 0.6822(3) 0.079(3) Uani 1 1 d . . . C21 C 0.9253(12) 0.7266(7) 0.5701(4) 0.034(3) Uani 1 1 d . . . C13 C 0.8509(13) 0.5327(7) 0.4210(4) 0.035(3) Uani 1 1 d . . . H13 H 0.8595 0.4859 0.4138 0.042 Uiso 1 1 calc R . . F18 F 0.8582(11) 0.9572(6) 0.5473(3) 0.079(3) Uani 1 1 d . . . O8 O 0.7572(9) 0.7347(6) 0.6270(3) 0.041(2) Uani 1 1 d . . . C46 C 0.7177(12) 0.7248(7) 0.8134(4) 0.030(3) Uani 1 1 d . . . C5 C 0.4516(13) 0.8168(7) 0.4307(5) 0.042(4) Uani 1 1 d . . . C15 C 0.6388(15) 0.5163(9) 0.3988(4) 0.048(4) Uani 1 1 d . . . N4 N 0.7514(9) 0.6714(5) 0.5328(3) 0.029(2) Uani 1 1 d . . . C0IA C 1.1018(11) 0.7596(7) 0.7754(4) 0.033(3) Uani 1 1 d . . . H0IA H 1.0908 0.7266 0.7534 0.049 Uiso 1 1 calc R . . H0IB H 1.1830 0.7622 0.7858 0.049 Uiso 1 1 calc R . . H0IC H 1.0747 0.8051 0.7659 0.049 Uiso 1 1 calc R . . C6 C 0.7928(17) 0.9063(8) 0.5285(5) 0.053(4) Uani 1 1 d . . . C39 C 0.7011(15) 0.9315(8) 0.7767(4) 0.045(4) Uani 1 1 d . . . C29 C 0.5475(12) 0.6473(8) 0.5041(4) 0.040(3) Uani 1 1 d . . . H29A H 0.4721 0.6363 0.5112 0.060 Uiso 1 1 calc R . . H29B H 0.5663 0.6146 0.4841 0.060 Uiso 1 1 calc R . . H29C H 0.5468 0.6942 0.4934 0.060 Uiso 1 1 calc R . . F13 F 0.3851(10) 0.8447(6) 0.4023(4) 0.085(4) Uani 1 1 d . . . C47 C 0.6819(12) 0.6639(7) 0.7934(4) 0.033(3) Uani 1 1 d . . . H47 H 0.7357 0.6352 0.7831 0.040 Uiso 1 1 calc R . . C0JA C 0.7026(13) 0.5199(6) 0.6990(5) 0.040(3) Uani 1 1 d . . . C32 C 0.8413(13) 0.9405(7) 0.6656(4) 0.038(3) Uani 1 1 d . . . H32 H 0.8571 0.9872 0.6602 0.046 Uiso 1 1 calc R . . C1 C 0.7796(12) 0.9395(7) 0.3841(4) 0.037(3) Uani 1 1 d . . . F16 F 0.7098(11) 0.9401(6) 0.5073(3) 0.087(4) Uani 1 1 d . . . C36 C 0.5244(14) 0.7957(7) 0.7129(4) 0.037(3) Uani 1 1 d . . . C24 C 0.6363(12) 0.6423(7) 0.5408(4) 0.033(3) Uani 1 1 d . . . C9 C 1.0273(14) 0.8334(7) 0.4751(4) 0.040(4) Uani 1 1 d . . . C28 C 0.6575(12) 0.5643(8) 0.5519(5) 0.044(4) Uani 1 1 d . . . H28A H 0.7205 0.5605 0.5736 0.066 Uiso 1 1 calc R . . H28B H 0.6769 0.5392 0.5288 0.066 Uiso 1 1 calc R . . H28C H 0.5884 0.5445 0.5602 0.066 Uiso 1 1 calc R . . C8 C 0.9609(12) 0.8756(8) 0.4978(4) 0.039(3) Uani 1 1 d . . . H8 H 0.9931 0.9174 0.5087 0.047 Uiso 1 1 calc R . . F33 F 0.3740(11) 0.7602(8) 0.6656(3) 0.092(4) Uani 1 1 d . . . C44 C 1.0338(11) 0.7355(6) 0.8086(4) 0.029(3) Uani 1 1 d . . . O9 O 0.8112(9) 0.8276(5) 0.4081(3) 0.043(2) Uani 1 1 d . . . O12 O 0.8795(8) 0.7053(4) 0.7554(2) 0.031(2) Uani 1 1 d . . . C35 C 0.3964(17) 0.7820(10) 0.7019(5) 0.056(5) Uani 1 1 d . . . Br1 Br 1.22570(13) 0.66264(8) 0.53008(5) 0.0473(4) Uani 1 1 d . . . C43 C 1.0694(13) 0.6623(7) 0.8232(4) 0.038(3) Uani 1 1 d . . . H43A H 1.0237 0.6481 0.8436 0.056 Uiso 1 1 calc R . . H43B H 1.1502 0.6622 0.8342 0.056 Uiso 1 1 calc R . . H43C H 1.0568 0.6300 0.8009 0.056 Uiso 1 1 calc R . . C40 C 1.0208(14) 0.8650(7) 0.8267(4) 0.044(4) Uani 1 1 d . . . H40A H 0.9676 0.8698 0.8022 0.066 Uiso 1 1 calc R . . H40B H 1.0979 0.8770 0.8216 0.066 Uiso 1 1 calc R . . H40C H 0.9979 0.8960 0.8469 0.066 Uiso 1 1 calc R . . F5 F 1.1414(8) 0.5663(5) 0.4295(3) 0.065(3) Uani 1 1 d . . . F14 F 0.4068(10) 0.7519(5) 0.4369(3) 0.065(3) Uani 1 1 d . . . C22 C 0.9625(12) 0.7831(7) 0.5929(4) 0.035(3) Uani 1 1 d . . . H22 H 0.9100 0.8061 0.6071 0.042 Uiso 1 1 calc R . . C4 C 0.5759(12) 0.8125(7) 0.4238(4) 0.039(3) Uani 1 1 d . . . C3 C 0.6221(15) 0.8700(8) 0.4073(4) 0.051(4) Uani 1 1 d . . . H3 H 0.5743 0.9087 0.4004 0.061 Uiso 1 1 calc R . . C41 C 1.1012(13) 0.7794(8) 0.8783(4) 0.041(4) Uani 1 1 d . . . H41A H 1.0707 0.8002 0.9009 0.062 Uiso 1 1 calc R . . H41B H 1.1746 0.8008 0.8754 0.062 Uiso 1 1 calc R . . H41C H 1.1121 0.7299 0.8829 0.062 Uiso 1 1 calc R . . F23 F 1.1164(9) 0.9225(6) 0.6759(4) 0.085(4) Uani 1 1 d . . . F22 F 1.0325(9) 1.0047(4) 0.6997(3) 0.064(3) Uani 1 1 d . . . C26 C 0.5516(13) 0.6526(9) 0.6066(4) 0.045(4) Uani 1 1 d . . . H26A H 0.6001 0.6149 0.6182 0.067 Uiso 1 1 calc R . . H26B H 0.4784 0.6340 0.5942 0.067 Uiso 1 1 calc R . . H26C H 0.5385 0.6853 0.6274 0.067 Uiso 1 1 calc R . . C17 C 1.0748(12) 0.8081(7) 0.5959(4) 0.036(3) Uani 1 1 d . . . H17 H 1.0969 0.8482 0.6109 0.043 Uiso 1 1 calc R . . C31 C 0.9251(13) 0.8997(8) 0.6854(4) 0.037(3) Uani 1 1 d . . . C49 C 0.5680(13) 0.6457(7) 0.7889(4) 0.039(3) Uani 1 1 d . . . H49 H 0.5459 0.6046 0.7748 0.046 Uiso 1 1 calc R . . C30 C 1.0423(13) 0.9366(8) 0.6990(5) 0.044(4) Uani 1 1 d . . . C37 C 0.5601(13) 0.8558(7) 0.7363(4) 0.041(4) Uani 1 1 d . . . H37 H 0.5041 0.8879 0.7420 0.049 Uiso 1 1 calc R . . O18 O 0.9429(8) 0.6872(5) 0.6808(2) 0.034(2) Uani 1 1 d . . . C9DA C 0.9639(12) 0.6226(7) 0.6782(3) 0.034(3) Uani 1 1 d . . . C52 C 0.3319(15) 0.6093(7) 0.7790(5) 0.052(4) Uani 1 1 d . . . H52A H 0.3543 0.6118 0.7524 0.077 Uiso 1 1 calc R . . H52B H 0.2487 0.6060 0.7769 0.077 Uiso 1 1 calc R . . H52C H 0.3665 0.5685 0.7927 0.077 Uiso 1 1 calc R . . C27 C 0.5511(14) 0.7561(7) 0.5619(5) 0.047(4) Uani 1 1 d . . . H27A H 0.5733 0.7921 0.5815 0.070 Uiso 1 1 calc R . . H27B H 0.4684 0.7492 0.5592 0.070 Uiso 1 1 calc R . . H27C H 0.5725 0.7701 0.5363 0.070 Uiso 1 1 calc R . . C16 C 1.2958(15) 0.8635(8) 0.5912(5) 0.052(4) Uani 1 1 d U . . H16A H 1.2426 0.8982 0.5787 0.079 Uiso 1 1 calc R . . H16B H 1.3725 0.8731 0.5850 0.079 Uiso 1 1 calc R . . H16C H 1.2964 0.8648 0.6200 0.079 Uiso 1 1 calc R . . C2 C 0.7356(12) 0.8732(9) 0.4003(4) 0.042(4) Uani 1 1 d . . . F10 F 1.1891(8) 0.9051(5) 0.4947(3) 0.058(2) Uani 1 1 d . . . F11 F 1.1419(10) 0.8859(6) 0.4329(3) 0.070(3) Uani 1 1 d . . . F12 F 1.2180(9) 0.8047(5) 0.4688(4) 0.074(3) Uani 1 1 d . . . C10 C 1.1462(13) 0.8553(9) 0.4689(4) 0.044(4) Uani 1 1 d . . . F26 F 1.0999(8) 0.5390(5) 0.6654(3) 0.060(2) Uani 1 1 d . . . F20 F 0.5747(9) 0.9281(5) 0.6019(3) 0.065(3) Uani 1 1 d . . . F25 F 1.1595(7) 0.6267(6) 0.6993(3) 0.065(3) Uani 1 1 d . . . F27 F 1.1041(9) 0.6358(6) 0.6366(3) 0.070(3) Uani 1 1 d . . . F21 F 0.5590(11) 0.9718(7) 0.6574(3) 0.092(4) Uani 1 1 d . . . C4AA C 1.0873(14) 0.6071(7) 0.6704(4) 0.040(4) Uani 1 1 d . . . C34 C 0.6365(16) 0.9598(9) 0.6327(5) 0.053(4) Uani 1 1 d . . . F31 F 0.3565(11) 0.7431(10) 0.7260(4) 0.128(7) Uani 1 1 d . . . F2 F 0.5652(10) 0.5489(6) 0.3750(4) 0.092(4) Uani 1 1 d . . . F19 F 0.6739(12) 1.0181(5) 0.6205(4) 0.113(5) Uani 1 1 d . . . F24 F 1.0808(12) 0.9197(7) 0.7354(3) 0.106(5) Uani 1 1 d . . . F32 F 0.3347(11) 0.8406(7) 0.7008(4) 0.105(5) Uani 1 1 d . . . F15 F 0.4487(10) 0.8501(7) 0.4644(4) 0.099(4) 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 Tb1 0.0275(4) 0.0190(3) 0.0314(4) 0.0008(2) 0.0039(3) 0.0010(2) Tb2 0.0295(4) 0.0221(3) 0.0297(4) -0.0020(2) 0.0024(3) -0.0005(2) Br2 0.0271(8) 0.0408(8) 0.0725(10) -0.0165(7) 0.0061(7) 0.0006(6) O10 0.038(6) 0.033(5) 0.039(5) -0.005(4) -0.001(4) 0.004(4) O6 0.034(6) 0.018(5) 0.039(5) 0.000(4) 0.001(4) 0.008(4) O2 0.040(6) 0.024(5) 0.048(6) -0.007(4) 0.011(4) 0.000(4) F35 0.055(6) 0.029(4) 0.050(5) -0.006(4) 0.006(4) -0.002(4) O3 0.042(6) 0.028(5) 0.032(5) 0.000(4) 0.007(4) 0.003(4) O14 0.053(7) 0.027(5) 0.043(6) 0.003(4) 0.003(5) -0.006(5) O15 0.036(6) 0.012(4) 0.043(5) 0.003(4) 0.006(4) -0.003(4) O1 0.038(6) 0.013(4) 0.036(5) 0.004(3) 0.002(4) 0.006(4) N2 0.027(6) 0.020(5) 0.025(6) -0.004(4) 0.001(4) -0.004(4) O11 0.044(6) 0.010(4) 0.045(6) 0.000(4) 0.006(4) -0.007(4) O13 0.038(6) 0.027(5) 0.043(5) -0.004(4) 0.009(4) -0.002(4) N1 0.026(6) 0.014(5) 0.039(6) 0.001(4) 0.002(5) 0.003(4) O17 0.031(5) 0.027(5) 0.034(5) -0.002(4) 0.009(4) -0.005(4) F34 0.080(7) 0.024(4) 0.067(5) 0.002(4) 0.017(5) -0.006(4) F9 0.070(8) 0.036(5) 0.088(7) 0.006(5) -0.010(5) -0.015(5) C19 0.033(8) 0.036(8) 0.034(7) -0.002(6) 0.008(6) 0.001(6) C18 0.026(8) 0.041(8) 0.038(8) 0.011(6) 0.005(6) 0.005(6) F6 0.051(7) 0.096(9) 0.062(6) 0.016(6) 0.002(5) 0.029(6) F8 0.091(9) 0.037(5) 0.086(7) 0.018(5) 0.046(6) 0.008(5) C23 0.034(8) 0.020(6) 0.036(7) 0.003(5) 0.006(6) 0.009(5) F7 0.067(7) 0.028(5) 0.092(7) 0.020(5) 0.011(5) 0.005(4) O4 0.025(5) 0.023(5) 0.040(5) 0.002(4) 0.000(4) -0.005(4) O5 0.045(6) 0.025(5) 0.039(5) -0.011(4) 0.012(4) -0.004(4) C11 0.054(11) 0.030(8) 0.048(9) 0.001(7) 0.010(7) -0.002(7) C33 0.057(11) 0.044(9) 0.030(8) 0.007(6) -0.001(7) 0.007(8) C42 0.043(9) 0.008(5) 0.048(8) -0.005(5) 0.015(6) 0.000(5) O16 0.034(6) 0.026(5) 0.069(7) -0.011(5) 0.002(5) -0.020(4) F4 0.055(7) 0.034(5) 0.127(8) -0.020(5) -0.019(6) 0.010(5) C25 0.019(7) 0.041(8) 0.024(6) -0.003(5) -0.003(5) -0.003(5) F3 0.050(6) 0.032(5) 0.088(6) -0.030(5) 0.012(5) -0.014(4) N3 0.029(7) 0.046(7) 0.030(6) -0.007(5) 0.003(5) -0.018(5) F30 0.071(8) 0.027(5) 0.173(11) -0.015(6) 0.050(7) -0.010(5) C50 0.030(8) 0.034(7) 0.026(7) 0.001(5) 0.001(5) 0.000(6) C48 0.036(8) 0.029(7) 0.025(7) 0.014(5) 0.011(6) 0.012(6) C51 0.034(9) 0.024(7) 0.048(9) -0.010(6) 0.019(6) 0.012(6) C7 0.050(7) 0.021(6) 0.034(6) -0.002(5) -0.007(5) -0.003(5) F28 0.090(9) 0.055(7) 0.081(7) 0.000(5) 0.018(6) -0.039(6) F1 0.080(8) 0.081(8) 0.085(7) -0.026(6) 0.038(6) -0.052(7) O7 0.022(5) 0.034(5) 0.059(6) -0.004(4) -0.004(4) -0.008(4) F36 0.069(7) 0.043(5) 0.075(6) -0.024(5) 0.005(5) 0.020(5) C12 0.038(7) 0.011(5) 0.041(6) 0.003(5) 0.000(5) 0.001(5) C5FA 0.030(8) 0.028(7) 0.041(8) -0.001(6) -0.002(6) 0.002(6) C38 0.031(8) 0.042(8) 0.028(7) 0.007(6) 0.007(6) 0.008(6) C14 0.050(9) 0.028(7) 0.024(7) -0.002(5) 0.003(6) -0.005(6) F17 0.084(8) 0.043(5) 0.069(6) -0.011(5) 0.035(5) -0.002(5) C20 0.018(7) 0.025(7) 0.041(7) 0.006(5) 0.010(5) 0.002(5) C45 0.043(9) 0.024(7) 0.032(8) -0.003(5) 0.006(6) 0.007(6) C3GA 0.035(9) 0.016(6) 0.060(9) 0.001(6) 0.011(6) 0.003(5) F29 0.052(7) 0.062(7) 0.115(8) 0.034(6) -0.014(6) -0.023(5) C21 0.028(8) 0.036(8) 0.037(8) 0.007(6) 0.001(6) -0.002(6) C13 0.055(10) 0.013(6) 0.040(8) -0.002(5) 0.010(6) -0.004(6) F18 0.088(9) 0.051(6) 0.102(8) -0.035(6) 0.032(6) -0.016(6) O8 0.038(6) 0.053(6) 0.033(5) -0.011(5) 0.007(4) -0.011(5) C46 0.028(8) 0.025(7) 0.035(7) 0.002(5) -0.001(6) 0.016(5) C5 0.040(9) 0.027(7) 0.058(9) 0.004(7) 0.006(7) -0.005(6) C15 0.051(11) 0.046(10) 0.044(9) 0.002(7) -0.004(7) -0.001(8) N4 0.032(7) 0.017(5) 0.038(6) 0.009(4) 0.006(5) -0.014(4) C0IA 0.008(6) 0.045(8) 0.046(8) -0.003(6) 0.007(5) -0.004(5) C6 0.079(13) 0.032(9) 0.048(9) -0.013(7) 0.008(9) 0.009(8) C39 0.056(11) 0.041(9) 0.041(9) -0.007(7) 0.017(7) -0.008(8) C29 0.030(8) 0.043(9) 0.047(8) -0.005(7) 0.008(6) 0.005(6) F13 0.053(7) 0.064(7) 0.135(9) 0.045(7) -0.003(6) 0.015(6) C47 0.037(9) 0.027(7) 0.036(7) 0.001(6) 0.009(6) -0.003(6) C0JA 0.042(9) 0.012(6) 0.062(10) -0.008(6) -0.002(7) 0.003(6) C32 0.041(9) 0.017(6) 0.057(9) -0.002(6) 0.011(7) -0.007(6) C1 0.022(8) 0.018(6) 0.070(10) 0.006(6) -0.004(7) -0.003(5) F16 0.109(10) 0.071(8) 0.076(7) -0.011(6) -0.002(6) 0.055(8) C36 0.053(10) 0.026(7) 0.031(7) 0.010(6) 0.005(6) -0.016(7) C24 0.032(8) 0.037(8) 0.030(7) -0.004(6) 0.004(6) -0.011(6) C9 0.061(11) 0.026(7) 0.033(7) -0.003(6) 0.008(7) 0.009(7) C28 0.024(8) 0.033(8) 0.081(11) -0.006(7) 0.026(7) 0.004(6) C8 0.031(8) 0.040(8) 0.043(8) -0.004(6) -0.005(6) -0.002(6) F33 0.054(8) 0.138(13) 0.078(8) -0.014(7) -0.008(6) 0.003(7) C44 0.020(7) 0.014(6) 0.054(8) -0.013(5) 0.011(6) -0.005(5) O9 0.056(7) 0.021(5) 0.054(6) -0.002(4) 0.015(5) -0.001(5) O12 0.037(6) 0.023(5) 0.030(5) -0.002(4) 0.002(4) 0.000(4) C35 0.071(13) 0.059(11) 0.038(9) -0.001(8) 0.008(8) 0.047(10) Br1 0.0306(9) 0.0376(8) 0.0747(11) -0.0104(7) 0.0104(7) 0.0020(6) C43 0.047(9) 0.025(7) 0.041(8) -0.005(6) 0.006(6) 0.011(6) C40 0.057(11) 0.018(7) 0.058(9) 0.000(6) 0.011(7) -0.004(6) F5 0.040(6) 0.043(5) 0.120(8) 0.027(5) 0.034(5) 0.011(4) F14 0.057(7) 0.046(6) 0.091(7) 0.008(5) 0.009(5) -0.011(5) C22 0.025(8) 0.040(8) 0.040(8) -0.001(6) 0.001(6) 0.000(6) C4 0.031(8) 0.020(7) 0.065(9) -0.009(6) 0.005(6) 0.003(6) C3 0.060(12) 0.035(9) 0.055(9) 0.005(7) 0.000(8) 0.010(8) C41 0.037(9) 0.052(9) 0.034(8) -0.001(7) 0.003(6) -0.011(7) F23 0.044(7) 0.071(8) 0.146(10) -0.045(7) 0.032(6) -0.012(5) F22 0.060(7) 0.019(4) 0.114(8) 0.007(5) 0.016(5) 0.001(4) C26 0.032(9) 0.067(11) 0.034(8) -0.013(7) 0.004(6) -0.031(8) C17 0.040(9) 0.021(7) 0.046(8) -0.006(6) 0.008(6) -0.008(6) C31 0.041(9) 0.037(8) 0.034(7) -0.005(6) 0.001(6) -0.007(6) C49 0.055(10) 0.027(7) 0.033(7) 0.002(6) 0.002(6) -0.002(6) C30 0.033(9) 0.037(9) 0.065(10) 0.015(7) 0.013(7) 0.001(6) C37 0.048(10) 0.028(7) 0.050(8) -0.004(6) 0.015(7) 0.025(7) O18 0.043(6) 0.024(5) 0.036(5) -0.005(4) 0.008(4) -0.004(4) C9DA 0.036(8) 0.038(8) 0.026(7) -0.002(6) -0.006(5) 0.010(6) C52 0.051(11) 0.020(7) 0.080(11) -0.002(7) -0.004(8) -0.017(7) C27 0.035(9) 0.027(8) 0.079(11) -0.012(7) 0.010(8) 0.014(6) C16 0.044(7) 0.043(7) 0.068(8) -0.003(6) 0.001(6) -0.023(6) C2 0.026(8) 0.058(10) 0.038(8) -0.005(7) -0.003(6) -0.001(7) F10 0.055(6) 0.038(5) 0.081(6) -0.009(4) 0.003(5) -0.021(4) F11 0.071(8) 0.069(7) 0.072(6) 0.003(5) 0.019(5) -0.027(6) F12 0.041(6) 0.034(5) 0.150(10) 0.002(6) 0.027(6) 0.000(4) C10 0.027(8) 0.057(10) 0.045(9) -0.007(7) -0.007(6) -0.015(7) F26 0.047(6) 0.047(6) 0.087(6) -0.008(5) 0.016(4) 0.006(5) F20 0.077(8) 0.057(6) 0.054(5) 0.004(5) -0.015(5) 0.018(5) F25 0.019(5) 0.089(8) 0.083(6) -0.032(6) -0.003(4) 0.010(5) F27 0.062(7) 0.083(8) 0.072(6) 0.030(6) 0.034(5) 0.021(6) F21 0.091(10) 0.111(10) 0.074(7) -0.013(6) 0.006(6) 0.065(8) C4AA 0.055(11) 0.026(7) 0.040(8) 0.006(6) 0.017(7) 0.016(7) C34 0.062(12) 0.039(9) 0.052(10) 0.004(7) -0.011(8) 0.010(8) F31 0.050(9) 0.192(18) 0.137(11) 0.085(11) -0.011(7) -0.057(10) F2 0.055(7) 0.052(7) 0.150(10) -0.002(7) -0.056(7) -0.007(5) F19 0.099(11) 0.034(6) 0.187(12) 0.058(7) -0.044(9) -0.016(6) F24 0.115(12) 0.108(11) 0.078(7) 0.043(7) -0.047(7) -0.067(9) F32 0.052(8) 0.060(8) 0.194(13) -0.032(8) -0.012(8) 0.019(6) F15 0.064(8) 0.110(10) 0.134(9) -0.061(9) 0.056(7) -0.034(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6 2.319(10) . ? Tb1 O17 2.351(8) 4_575 ? Tb1 O5 2.358(11) . ? Tb1 O2 2.358(8) . ? Tb1 O9 2.359(9) . ? Tb1 O4 2.373(8) . ? Tb1 O1 2.378(8) . ? Tb1 O3 2.384(9) . ? Tb2 O10 2.309(10) . ? Tb2 O8 2.322(9) . ? Tb2 O15 2.334(9) . ? Tb2 O13 2.343(9) . ? Tb2 O11 2.357(10) . ? Tb2 O18 2.372(10) . ? Tb2 O12 2.402(8) . ? Tb2 O14 2.412(10) . ? Br2 C51 1.897(12) . ? O10 C5FA 1.271(16) . ? O6 C9 1.286(17) . ? O2 C7 1.299(16) . ? F35 C39 1.328(17) . ? O3 N4 1.265(13) . ? O14 C33 1.269(18) . ? O15 C31 1.237(17) . ? O1 C12 1.246(14) . ? N2 O12 1.291(12) . ? N2 C45 1.347(17) . ? N2 C44 1.534(17) . ? O11 C36 1.239(18) . ? O13 C38 1.289(16) . ? N1 O17 1.306(13) . ? N1 C45 1.388(18) . ? N1 C42 1.488(18) . ? O17 Tb1 2.351(8) 4_576 ? F34 C39 1.353(18) . ? F9 C1 1.361(16) . ? C19 C20 1.364(19) . ? C19 C18 1.39(2) . ? C19 Br1 1.912(14) . ? C18 O7 1.332(17) . ? C18 C17 1.40(2) . ? F6 C11 1.305(17) . ? F8 C1 1.333(17) . ? C23 N4 1.346(17) . ? C23 N3 1.381(17) . ? C23 C21 1.46(2) . ? F7 C1 1.338(16) . ? O4 C14 1.255(16) . ? O5 C4 1.277(16) . ? C11 F5 1.284(18) . ? C11 F4 1.349(17) . ? C11 C12 1.59(2) . ? C33 C32 1.43(2) . ? C33 C34 1.53(2) . ? C42 C41 1.50(2) . ? C42 C40 1.528(17) . ? C42 C44 1.573(17) . ? O16 C50 1.365(17) . ? O16 C52 1.437(16) . ? C25 C27 1.51(2) . ? C25 N3 1.507(16) . ? C25 C24 1.550(18) . ? C25 C26 1.543(18) . ? F3 C15 1.352(18) . ? N3 O8 1.306(13) . ? F30 C0JA 1.311(16) . ? C50 C49 1.39(2) . ? C50 C51 1.443(19) . ? C48 C51 1.37(2) . ? C48 C46 1.426(18) . ? C7 C8 1.35(2) . ? C7 C6 1.49(2) . ? F28 C0JA 1.355(17) . ? F1 C15 1.302(18) . ? O7 C16 1.466(17) . ? F36 C39 1.346(19) . ? C12 C13 1.396(19) . ? C5FA C3GA 1.396(19) . ? C5FA C0JA 1.54(2) . ? C38 C37 1.34(2) . ? C38 C39 1.55(2) . ? C14 C13 1.37(2) . ? C14 C15 1.58(2) . ? F17 C6 1.35(2) . ? C20 C21 1.423(19) . ? C45 C46 1.43(2) . ? C3GA C9DA 1.40(2) . ? F29 C0JA 1.306(18) . ? C21 C22 1.38(2) . ? F18 C6 1.36(2) . ? C46 C47 1.402(19) . ? C5 F13 1.282(18) . ? C5 F15 1.324(18) . ? C5 F14 1.395(17) . ? C5 C4 1.53(2) . ? C15 F2 1.274(18) . ? N4 C24 1.533(16) . ? C0IA C44 1.549(18) . ? C6 F16 1.31(2) . ? C29 C24 1.525(19) . ? C47 C49 1.38(2) . ? C32 C31 1.37(2) . ? C1 C2 1.52(2) . ? C36 C37 1.44(2) . ? C36 C35 1.54(3) . ? C24 C28 1.57(2) . ? C9 C8 1.43(2) . ? C9 C10 1.51(2) . ? F33 C35 1.298(19) . ? C44 C43 1.545(18) . ? O9 C2 1.262(18) . ? C35 F31 1.26(2) . ? C35 F32 1.350(18) . ? C22 C17 1.41(2) . ? C4 C3 1.40(2) . ? C3 C2 1.40(2) . ? F23 C30 1.286(18) . ? F22 C30 1.327(18) . ? C31 C30 1.58(2) . ? C30 F24 1.302(17) . ? O18 C9DA 1.284(16) . ? C9DA C4AA 1.55(2) . ? F10 C10 1.357(17) . ? F11 C10 1.357(17) . ? F12 C10 1.300(19) . ? F26 C4AA 1.344(17) . ? F20 C34 1.343(19) . ? F25 C4AA 1.272(18) . ? F27 C4AA 1.321(15) . ? F21 C34 1.35(2) . ? C34 F19 1.30(2) . ? 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 O6 Tb1 O17 91.7(3) . 4_575 ? O6 Tb1 O5 137.9(3) . . ? O17 Tb1 O5 102.7(3) 4_575 . ? O6 Tb1 O2 74.2(3) . . ? O17 Tb1 O2 149.0(3) 4_575 . ? O5 Tb1 O2 73.4(3) . . ? O6 Tb1 O9 74.0(3) . . ? O17 Tb1 O9 72.4(3) 4_575 . ? O5 Tb1 O9 73.2(3) . . ? O2 Tb1 O9 77.2(3) . . ? O6 Tb1 O4 148.1(3) . . ? O17 Tb1 O4 71.1(3) 4_575 . ? O5 Tb1 O4 73.5(3) . . ? O2 Tb1 O4 133.0(3) . . ? O9 Tb1 O4 122.5(3) . . ? O6 Tb1 O1 75.0(3) . . ? O17 Tb1 O1 74.4(3) 4_575 . ? O5 Tb1 O1 146.9(3) . . ? O2 Tb1 O1 125.6(3) . . ? O9 Tb1 O1 133.2(3) . . ? O4 Tb1 O1 74.5(3) . . ? O6 Tb1 O3 104.7(3) . . ? O17 Tb1 O3 137.6(3) 4_575 . ? O5 Tb1 O3 90.9(3) . . ? O2 Tb1 O3 73.3(3) . . ? O9 Tb1 O3 149.5(3) . . ? O4 Tb1 O3 74.9(3) . . ? O1 Tb1 O3 72.7(3) . . ? O10 Tb2 O8 81.6(3) . . ? O10 Tb2 O15 150.9(3) . . ? O8 Tb2 O15 94.9(3) . . ? O10 Tb2 O13 123.5(3) . . ? O8 Tb2 O13 144.3(4) . . ? O15 Tb2 O13 74.8(3) . . ? O10 Tb2 O11 72.7(3) . . ? O8 Tb2 O11 94.2(3) . . ? O15 Tb2 O11 136.4(3) . . ? O13 Tb2 O11 73.1(3) . . ? O10 Tb2 O18 73.7(3) . . ? O8 Tb2 O18 73.9(3) . . ? O15 Tb2 O18 77.6(3) . . ? O13 Tb2 O18 133.8(3) . . ? O11 Tb2 O18 145.6(3) . . ? O10 Tb2 O12 73.6(3) . . ? O8 Tb2 O12 141.3(3) . . ? O15 Tb2 O12 92.9(3) . . ? O13 Tb2 O12 74.2(3) . . ? O11 Tb2 O12 105.7(3) . . ? O18 Tb2 O12 71.0(3) . . ? O10 Tb2 O14 130.7(3) . . ? O8 Tb2 O14 68.4(4) . . ? O15 Tb2 O14 72.4(3) . . ? O13 Tb2 O14 75.8(3) . . ? O11 Tb2 O14 71.7(3) . . ? O18 Tb2 O14 128.7(3) . . ? O12 Tb2 O14 149.2(3) . . ? C5FA O10 Tb2 134.7(9) . . ? C9 O6 Tb1 133.0(9) . . ? C7 O2 Tb1 131.1(9) . . ? N4 O3 Tb1 136.6(7) . . ? C33 O14 Tb2 134.5(10) . . ? C31 O15 Tb2 134.1(9) . . ? C12 O1 Tb1 131.8(9) . . ? O12 N2 C45 125.3(11) . . ? O12 N2 C44 121.1(10) . . ? C45 N2 C44 113.4(10) . . ? C36 O11 Tb2 133.7(9) . . ? C38 O13 Tb2 130.2(8) . . ? O17 N1 C45 123.9(11) . . ? O17 N1 C42 121.2(10) . . ? C45 N1 C42 114.0(11) . . ? N1 O17 Tb1 143.8(7) . 4_576 ? C20 C19 C18 123.1(13) . . ? C20 C19 Br1 118.7(10) . . ? C18 C19 Br1 118.2(11) . . ? O7 C18 C17 121.7(13) . . ? O7 C18 C19 120.0(13) . . ? C17 C18 C19 118.3(13) . . ? N4 C23 N3 105.9(12) . . ? N4 C23 C21 126.9(12) . . ? N3 C23 C21 127.2(12) . . ? C14 O4 Tb1 131.9(9) . . ? C4 O5 Tb1 133.8(9) . . ? F5 C11 F6 109.7(14) . . ? F5 C11 F4 108.6(13) . . ? F6 C11 F4 107.1(13) . . ? F5 C11 C12 110.8(12) . . ? F6 C11 C12 109.7(11) . . ? F4 C11 C12 110.8(12) . . ? O14 C33 C32 125.7(14) . . ? O14 C33 C34 114.7(15) . . ? C32 C33 C34 119.5(14) . . ? C41 C42 N1 110.6(11) . . ? C41 C42 C40 112.2(12) . . ? N1 C42 C40 107.2(11) . . ? C41 C42 C44 112.1(12) . . ? N1 C42 C44 100.1(10) . . ? C40 C42 C44 113.9(11) . . ? C50 O16 C52 115.7(12) . . ? C27 C25 N3 109.2(12) . . ? C27 C25 C24 114.6(11) . . ? N3 C25 C24 98.2(10) . . ? C27 C25 C26 111.6(13) . . ? N3 C25 C26 108.8(10) . . ? C24 C25 C26 113.5(12) . . ? O8 N3 C23 122.8(11) . . ? O8 N3 C25 121.9(10) . . ? C23 N3 C25 113.5(10) . . ? O16 C50 C49 128.5(13) . . ? O16 C50 C51 116.2(11) . . ? C49 C50 C51 115.3(13) . . ? C51 C48 C46 120.3(13) . . ? C48 C51 C50 122.1(12) . . ? C48 C51 Br2 118.7(10) . . ? C50 C51 Br2 119.2(11) . . ? O2 C7 C8 128.2(14) . . ? O2 C7 C6 113.2(14) . . ? C8 C7 C6 118.6(14) . . ? C18 O7 C16 122.0(12) . . ? O1 C12 C13 129.7(13) . . ? O1 C12 C11 112.5(11) . . ? C13 C12 C11 117.8(11) . . ? O10 C5FA C3GA 128.8(13) . . ? O10 C5FA C0JA 113.7(12) . . ? C3GA C5FA C0JA 117.5(12) . . ? O13 C38 C37 129.0(13) . . ? O13 C38 C39 111.6(12) . . ? C37 C38 C39 119.4(12) . . ? O4 C14 C13 130.2(13) . . ? O4 C14 C15 110.8(13) . . ? C13 C14 C15 119.0(12) . . ? C19 C20 C21 119.4(12) . . ? N2 C45 N1 105.3(12) . . ? N2 C45 C46 127.0(12) . . ? N1 C45 C46 127.7(12) . . ? C5FA C3GA C9DA 122.2(12) . . ? C22 C21 C20 117.8(13) . . ? C22 C21 C23 123.2(13) . . ? C20 C21 C23 119.0(12) . . ? C14 C13 C12 121.4(12) . . ? N3 O8 Tb2 162.7(9) . . ? C47 C46 C45 118.1(12) . . ? C47 C46 C48 118.4(13) . . ? C45 C46 C48 123.5(13) . . ? F13 C5 F15 111.3(15) . . ? F13 C5 F14 106.8(13) . . ? F15 C5 F14 104.7(12) . . ? F13 C5 C4 114.5(13) . . ? F15 C5 C4 107.5(12) . . ? F14 C5 C4 111.7(12) . . ? F2 C15 F1 112.4(17) . . ? F2 C15 F3 107.0(12) . . ? F1 C15 F3 107.6(13) . . ? F2 C15 C14 111.8(13) . . ? F1 C15 C14 107.7(11) . . ? F3 C15 C14 110.3(13) . . ? O3 N4 C23 125.9(11) . . ? O3 N4 C24 121.6(10) . . ? C23 N4 C24 112.0(10) . . ? F16 C6 F17 107.5(17) . . ? F16 C6 F18 103.3(14) . . ? F17 C6 F18 104.2(12) . . ? F16 C6 C7 113.3(12) . . ? F17 C6 C7 112.9(13) . . ? F18 C6 C7 114.7(16) . . ? F35 C39 F36 107.6(11) . . ? F35 C39 F34 106.9(13) . . ? F36 C39 F34 105.6(13) . . ? F35 C39 C38 112.5(12) . . ? F36 C39 C38 113.4(13) . . ? F34 C39 C38 110.4(11) . . ? C49 C47 C46 119.7(13) . . ? F29 C0JA F30 110.3(13) . . ? F29 C0JA F28 104.9(13) . . ? F30 C0JA F28 103.1(12) . . ? F29 C0JA C5FA 112.3(11) . . ? F30 C0JA C5FA 115.3(13) . . ? F28 C0JA C5FA 110.0(11) . . ? C31 C32 C33 120.3(13) . . ? F8 C1 F7 107.4(11) . . ? F8 C1 F9 107.1(12) . . ? F7 C1 F9 105.9(11) . . ? F8 C1 C2 111.0(12) . . ? F7 C1 C2 113.5(12) . . ? F9 C1 C2 111.5(11) . . ? O11 C36 C37 125.0(14) . . ? O11 C36 C35 116.4(12) . . ? C37 C36 C35 118.7(14) . . ? C29 C24 N4 111.2(10) . . ? C29 C24 C25 113.4(12) . . ? N4 C24 C25 100.6(10) . . ? C29 C24 C28 109.1(12) . . ? N4 C24 C28 106.3(11) . . ? C25 C24 C28 115.7(11) . . ? O6 C9 C8 125.4(15) . . ? O6 C9 C10 114.2(12) . . ? C8 C9 C10 120.3(13) . . ? C7 C8 C9 122.9(14) . . ? N2 C44 C43 104.4(10) . . ? N2 C44 C0IA 108.3(10) . . ? C43 C44 C0IA 111.5(11) . . ? N2 C44 C42 98.5(10) . . ? C43 C44 C42 116.8(11) . . ? C0IA C44 C42 115.5(10) . . ? C2 O9 Tb1 134.0(10) . . ? N2 O12 Tb2 134.7(7) . . ? F31 C35 F33 112(2) . . ? F31 C35 F32 105.9(17) . . ? F33 C35 F32 102.2(13) . . ? F31 C35 C36 113.0(13) . . ? F33 C35 C36 110.8(14) . . ? F32 C35 C36 111.9(17) . . ? C21 C22 C17 122.7(13) . . ? O5 C4 C3 126.0(14) . . ? O5 C4 C5 116.7(13) . . ? C3 C4 C5 117.3(13) . . ? C4 C3 C2 122.9(15) . . ? C18 C17 C22 118.6(13) . . ? O15 C31 C32 130.7(14) . . ? O15 C31 C30 113.6(13) . . ? C32 C31 C30 115.6(13) . . ? C47 C49 C50 124.1(13) . . ? F23 C30 F24 110.5(15) . . ? F23 C30 F22 107.0(13) . . ? F24 C30 F22 104.7(14) . . ? F23 C30 C31 111.7(13) . . ? F24 C30 C31 110.2(12) . . ? F22 C30 C31 112.5(13) . . ? C38 C37 C36 122.2(13) . . ? C9DA O18 Tb2 135.4(9) . . ? O18 C9DA C3GA 125.0(13) . . ? O18 C9DA C4AA 113.5(13) . . ? C3GA C9DA C4AA 121.5(12) . . ? O9 C2 C3 127.2(15) . . ? O9 C2 C1 113.6(13) . . ? C3 C2 C1 119.0(14) . . ? F12 C10 F11 105.8(13) . . ? F12 C10 F10 110.7(12) . . ? F11 C10 F10 103.9(13) . . ? F12 C10 C9 114.1(13) . . ? F11 C10 C9 109.2(11) . . ? F10 C10 C9 112.4(12) . . ? F25 C4AA F27 112.6(15) . . ? F25 C4AA F26 108.5(12) . . ? F27 C4AA F26 105.8(11) . . ? F25 C4AA C9DA 111.1(11) . . ? F27 C4AA C9DA 109.0(12) . . ? F26 C4AA C9DA 109.7(13) . . ? F19 C34 F20 108.9(13) . . ? F19 C34 F21 109.7(16) . . ? F20 C34 F21 102.8(15) . . ? F19 C34 C33 114.1(16) . . ? F20 C34 C33 111.5(13) . . ? F21 C34 C33 109.3(13) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 2.622 _refine_diff_density_min -2.175 _refine_diff_density_rms 0.258 _database_code_depnum_ccdc_archive 'CCDC 958924' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Dy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H42 Br2 Dy2 F36 N4 O18' _chemical_formula_weight 2251.76 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' Dy Dy -0.1892 4.4098 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.778(4) _cell_length_b 19.370(7) _cell_length_c 34.026(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.894(9) _cell_angle_gamma 90.00 _cell_volume 7689(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 24887 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 28.0 _exptl_crystal_description Prism _exptl_crystal_colour Darkgreen _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4351 _exptl_absorpt_coefficient_mu 3.122 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57037 _diffrn_reflns_av_R_equivalents 0.1384 _diffrn_reflns_av_sigmaI/netI 0.1542 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13126 _reflns_number_gt 9183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13126 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.2243 _refine_ls_wR_factor_gt 0.2136 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.82014(4) 0.27755(3) -0.056872(16) 0.02017(17) Uani 1 1 d . . . Dy2 Dy 0.78544(5) 0.24581(3) 0.194734(16) 0.02188(18) Uani 1 1 d . . . Br1 Br 1.22572(11) 0.33715(7) 0.03006(4) 0.0402(4) Uani 1 1 d . . . Br2 Br 0.41257(11) 0.30810(7) -0.15981(4) 0.0398(4) Uani 1 1 d . . . O2 O 0.5906(7) 0.2466(4) 0.2006(2) 0.0254(19) Uani 1 1 d U . . O6 O 0.9420(7) 0.3112(4) 0.1805(2) 0.0261(19) Uani 1 1 d . . . F22 F 1.1894(8) 0.0959(5) -0.0053(3) 0.057(2) Uani 1 1 d . . . O11 O 0.6288(7) 0.2444(4) -0.0673(3) 0.031(2) Uani 1 1 d . . . F23 F 1.2156(8) 0.1961(5) -0.0309(3) 0.067(3) Uani 1 1 d . . . C34 C 1.1449(13) 0.1441(8) -0.0316(4) 0.043(4) Uani 1 1 d . . . C21 C 0.5544(12) 0.2433(7) 0.0615(5) 0.044(4) Uani 1 1 d . . . H21A H 0.5969 0.2213 0.0429 0.066 Uiso 1 1 calc R . . H21B H 0.4775 0.2520 0.0491 0.066 Uiso 1 1 calc R . . H21C H 0.5526 0.2136 0.0840 0.066 Uiso 1 1 calc R . . C8 C 0.8410(11) 0.0594(7) 0.1653(4) 0.035(3) Uani 1 1 d . . . H8 H 0.8562 0.0136 0.1595 0.042 Uiso 1 1 calc R . . C33 C 1.0270(12) 0.1670(7) -0.0247(4) 0.034(3) Uani 1 1 d . . . C37 C 0.6205(12) 0.1310(7) -0.0932(4) 0.039(3) Uani 1 1 d . . . H37 H 0.5723 0.0936 -0.1001 0.047 Uiso 1 1 calc R . . C58 C 0.3333(12) 0.1097(7) -0.2214(4) 0.040(3) Uani 1 1 d . . . H58A H 0.3473 0.1153 -0.2484 0.060 Uiso 1 1 calc R . . H58B H 0.2527 0.1034 -0.2209 0.060 Uiso 1 1 calc R . . H58C H 0.3742 0.0700 -0.2100 0.060 Uiso 1 1 calc R . . O9 O 0.7904(7) 0.3400(4) 0.0005(2) 0.0239(18) Uani 1 1 d . . . F24 F 1.1402(9) 0.1137(5) -0.0675(3) 0.061(3) Uani 1 1 d . . . O4 O 0.9272(7) 0.1628(4) 0.1927(2) 0.0251(18) Uani 1 1 d . . . O14 O 0.7976(7) 0.1946(4) -0.0075(2) 0.028(2) Uani 1 1 d . . . F26 F 1.1439(7) 0.4338(4) -0.0704(3) 0.059(3) Uani 1 1 d . . . C36 C 0.5752(10) 0.1905(6) -0.0768(4) 0.028(3) Uani 1 1 d U . . N1 N 0.9074(8) 0.2291(5) -0.2095(3) 0.020(2) Uani 1 1 d . . . O18 O 0.9982(7) 0.2245(4) -0.0404(2) 0.0252(19) Uani 1 1 d . . . O8 O 1.2606(7) 0.2055(5) 0.0762(3) 0.036(2) Uani 1 1 d . . . F28 F 0.6707(7) 0.5395(4) -0.1207(3) 0.052(2) Uani 1 1 d . . . F36 F 0.8446(8) 0.0733(4) -0.1440(3) 0.054(2) Uani 1 1 d . . . O1 O 0.7582(7) 0.1663(4) 0.2446(2) 0.0256(18) Uani 1 1 d . . . F6 F 0.7509(7) 0.0856(4) 0.3127(2) 0.0378(19) Uani 1 1 d . . . O3 O 0.6999(8) 0.1476(4) 0.1594(3) 0.036(2) Uani 1 1 d . . . O12 O 0.9535(7) 0.3701(4) -0.0499(2) 0.0250(18) Uani 1 1 d . . . O15 O 0.8606(7) 0.3009(4) -0.1215(2) 0.0225(18) Uani 1 1 d . . . O16 O 0.8774(7) 0.2051(4) -0.2448(2) 0.0229(18) Uani 1 1 d . . . O5 O 0.7299(7) 0.3599(4) 0.1955(2) 0.0248(18) Uani 1 1 d . . . F17 F 1.0985(7) 0.4610(4) 0.1653(3) 0.056(2) Uani 1 1 d . . . F18 F 1.1052(8) 0.3651(5) 0.1362(3) 0.062(3) Uani 1 1 d . . . O17 O 0.3719(7) 0.1702(4) -0.1989(3) 0.032(2) Uani 1 1 d . . . F4 F 0.6131(8) 0.0273(5) 0.2807(3) 0.058(3) Uani 1 1 d . . . N2 N 0.8990(8) 0.2760(5) -0.1516(3) 0.021(2) Uani 1 1 d . . . F34 F 0.6974(8) 0.0174(4) -0.1316(3) 0.054(2) Uani 1 1 d . . . O10 O 0.8092(7) 0.1718(4) -0.0924(2) 0.030(2) Uani 1 1 d . . . F11 F 0.5767(8) 0.0721(5) 0.1019(2) 0.057(3) Uani 1 1 d . . . F35 F 0.8414(8) 0.0241(4) -0.0873(3) 0.054(2) Uani 1 1 d . . . N4 N 0.7322(8) 0.2934(5) 0.0921(3) 0.025(2) Uani 1 1 d . . . F31 F 0.4085(7) 0.2470(5) -0.0631(3) 0.058(3) Uani 1 1 d . . . F5 F 0.7760(8) 0.0283(4) 0.2608(2) 0.052(2) Uani 1 1 d . . . C26 C 1.1530(11) 0.2261(6) 0.0763(4) 0.028(3) Uani 1 1 d . . . F20 F 0.8607(9) 0.0439(5) 0.0473(3) 0.071(3) Uani 1 1 d . . . F15 F 1.0845(11) 0.0817(6) 0.2352(3) 0.098(5) Uani 1 1 d . . . F29 F 0.5639(9) 0.4526(5) -0.1251(4) 0.090(4) Uani 1 1 d . . . F27 F 1.0570(8) 0.5316(5) -0.0733(3) 0.072(3) Uani 1 1 d . . . O13 O 0.7167(7) 0.3755(4) -0.0810(2) 0.0260(19) Uani 1 1 d . . . F25 F 1.0993(7) 0.4804(5) -0.0178(2) 0.054(2) Uani 1 1 d . . . C22 C 0.8077(10) 0.2972(6) 0.0651(3) 0.023(3) Uani 1 1 d . . . F19 F 0.7479(8) 0.1273(5) 0.0574(3) 0.056(2) Uani 1 1 d . . . C43 C 0.9469(10) 0.4304(6) -0.0617(3) 0.022(3) Uani 1 1 d . . . C44 C 1.0620(10) 0.4694(6) -0.0555(4) 0.024(3) Uani 1 1 d . . . C53 C 0.7187(10) 0.2259(6) -0.1867(3) 0.023(3) Uani 1 1 d . . . F2 F 0.3741(8) 0.2396(7) 0.1652(3) 0.081(4) Uani 1 1 d . . . C35 C 0.4556(13) 0.1821(7) -0.0688(5) 0.047(4) Uani 1 1 d . . . C48 C 1.0705(10) 0.1644(7) -0.1768(4) 0.029(3) Uani 1 1 d . . . H48A H 1.0233 0.1507 -0.1573 0.044 Uiso 1 1 calc R . . H48B H 1.1493 0.1654 -0.1650 0.044 Uiso 1 1 calc R . . H48C H 1.0614 0.1320 -0.1984 0.044 Uiso 1 1 calc R . . F10 F 0.5587(10) 0.0274(6) 0.1570(3) 0.084(4) Uani 1 1 d . . . F9 F 0.7444(9) 0.5400(5) 0.1899(4) 0.085(4) Uani 1 1 d . . . C45 C 1.1010(11) 0.2780(7) -0.1207(4) 0.035(3) Uani 1 1 d . . . H45A H 1.0658 0.2933 -0.0984 0.052 Uiso 1 1 calc R . . H45B H 1.1709 0.3031 -0.1215 0.052 Uiso 1 1 calc R . . H45C H 1.1176 0.2296 -0.1181 0.052 Uiso 1 1 calc R . . F33 F 0.3841(8) 0.1558(5) -0.0979(3) 0.072(3) Uani 1 1 d . . . C24 C 1.0051(10) 0.3096(6) 0.0505(3) 0.022(3) Uani 1 1 d . . . H24 H 0.9828 0.3480 0.0349 0.026 Uiso 1 1 calc R . . C56 C 0.4827(10) 0.1857(6) -0.1962(4) 0.025(3) Uani 1 1 d . . . C20 C 0.6107(9) 0.3100(6) 0.0749(3) 0.021(2) Uani 1 1 d . . . C17 C 0.6349(10) 0.3577(6) 0.0405(3) 0.025(3) Uani 1 1 d . . . F30 F 0.5948(8) 0.5062(6) -0.0704(3) 0.075(3) Uani 1 1 d . . . O7 O 0.7563(7) 0.2659(5) 0.1268(2) 0.035(2) Uani 1 1 d . . . C2 C 0.6689(11) 0.1320(6) 0.2501(4) 0.029(3) Uani 1 1 d . . . F14 F 1.1186(8) 0.0784(6) 0.1760(4) 0.085(4) Uani 1 1 d . . . F21 F 0.7130(10) 0.0600(6) 0.0069(3) 0.083(4) Uani 1 1 d . . . C25 C 1.1173(11) 0.2867(7) 0.0550(4) 0.029(3) Uani 1 1 d . . . C42 C 0.8520(11) 0.4680(7) -0.0793(4) 0.031(3) Uani 1 1 d . . . H42 H 0.8609 0.5138 -0.0864 0.038 Uiso 1 1 calc R . . F16 F 1.1576(7) 0.3721(5) 0.1992(3) 0.059(3) Uani 1 1 d . . . C13 C 0.8877(10) 0.4298(6) 0.1832(4) 0.028(3) Uani 1 1 d U . . H13 H 0.9122 0.4752 0.1815 0.034 Uiso 1 1 calc R . . F8 F 0.5969(8) 0.4716(5) 0.1822(3) 0.073(3) Uani 1 1 d . . . F13 F 1.0338(8) -0.0050(4) 0.2000(3) 0.058(2) Uani 1 1 d . . . N3 N 0.7512(9) 0.3287(5) 0.0331(3) 0.024(2) Uani 1 1 d . . . C1 C 0.7022(12) 0.0663(7) 0.2760(4) 0.037(3) Uani 1 1 d . . . C46 C 1.0193(9) 0.2909(6) -0.1589(3) 0.021(2) Uani 1 1 d . . . F7 F 0.6927(9) 0.4860(5) 0.2378(3) 0.070(3) Uani 1 1 d . . . C52 C 0.6346(10) 0.2662(6) -0.1713(4) 0.023(3) Uani 1 1 d . . . H52 H 0.6567 0.3061 -0.1572 0.027 Uiso 1 1 calc R . . C28 C 0.9618(11) 0.2150(7) 0.0937(4) 0.029(3) Uani 1 1 d . . . H28 H 0.9106 0.1920 0.1076 0.035 Uiso 1 1 calc R . . C9 C 0.7284(12) 0.0870(7) 0.1534(4) 0.036(3) Uani 1 1 d . . . C57 C 0.5229(10) 0.2478(6) -0.1768(4) 0.025(3) Uani 1 1 d . . . C6 C 1.0403(12) 0.0635(7) 0.1983(4) 0.039(3) Uani 1 1 d . . . C51 C 0.8348(10) 0.2423(6) -0.1830(3) 0.020(2) Uani 1 1 d . . . F32 F 0.4486(8) 0.1505(6) -0.0355(4) 0.089(4) Uani 1 1 d . . . C47 C 1.0210(13) 0.3653(7) -0.1729(4) 0.039(3) Uani 1 1 d . . . H47A H 0.9606 0.3723 -0.1945 0.058 Uiso 1 1 calc R . . H47B H 1.0935 0.3750 -0.1815 0.058 Uiso 1 1 calc R . . H47C H 1.0100 0.3956 -0.1514 0.058 Uiso 1 1 calc R . . C40 C 0.6403(13) 0.4844(7) -0.1022(4) 0.040(4) Uani 1 1 d . . . C23 C 0.9264(11) 0.2743(6) 0.0698(3) 0.027(3) Uani 1 1 d . . . C15 C 1.0834(13) 0.3925(7) 0.1700(4) 0.038(3) Uani 1 1 d . . . C38 C 0.7346(11) 0.1266(6) -0.0994(4) 0.028(3) Uani 1 1 d . . . C4 C 0.5241(10) 0.2020(6) 0.2132(4) 0.025(3) Uani 1 1 d . . . C3 C 0.5576(11) 0.1441(7) 0.2363(4) 0.036(3) Uani 1 1 d . . . H3 H 0.5022 0.1131 0.2423 0.043 Uiso 1 1 calc R . . C31 C 0.8541(13) 0.1414(7) 0.0042(4) 0.036(3) Uani 1 1 d . . . C30 C 0.7921(14) 0.0932(7) 0.0283(4) 0.043(4) Uani 1 1 d . . . C12 C 0.7784(10) 0.4174(6) 0.1912(4) 0.028(3) Uani 1 1 d . . . C54 C 0.6793(10) 0.1640(6) -0.2063(3) 0.024(3) Uani 1 1 d . . . H54 H 0.7322 0.1358 -0.2164 0.029 Uiso 1 1 calc R . . C5 C 0.3970(13) 0.2180(9) 0.2016(5) 0.046(4) Uani 1 1 d . . . C49 C 1.0343(9) 0.2367(6) -0.1926(4) 0.020(3) Uani 1 1 d . . . C55 C 0.5668(11) 0.1443(7) -0.2109(4) 0.032(3) Uani 1 1 d . . . H55 H 0.5451 0.1032 -0.2239 0.038 Uiso 1 1 calc R . . C32 C 0.9623(12) 0.1246(7) -0.0033(4) 0.035(3) Uani 1 1 d . . . H32 H 0.9938 0.0830 0.0064 0.042 Uiso 1 1 calc R . . C16 C 0.6602(10) 0.4334(7) 0.0531(4) 0.035(3) Uani 1 1 d . . . H16A H 0.5895 0.4569 0.0552 0.053 Uiso 1 1 calc R . . H16B H 0.6990 0.4561 0.0337 0.053 Uiso 1 1 calc R . . H16C H 0.7079 0.4343 0.0784 0.053 Uiso 1 1 calc R . . C50 C 1.1043(10) 0.2603(6) -0.2248(4) 0.029(3) Uani 1 1 d U . . H50A H 1.0943 0.2281 -0.2464 0.044 Uiso 1 1 calc R . . H50B H 1.1839 0.2626 -0.2140 0.044 Uiso 1 1 calc R . . H50C H 1.0785 0.3052 -0.2342 0.044 Uiso 1 1 calc R . . F12 F 0.6739(10) -0.0175(5) 0.1210(4) 0.105(5) Uani 1 1 d . . . C19 C 0.5499(11) 0.3460(8) 0.1064(4) 0.037(3) Uani 1 1 d . . . H19A H 0.4757 0.3616 0.0945 0.055 Uiso 1 1 calc R . . H19B H 0.5947 0.3848 0.1170 0.055 Uiso 1 1 calc R . . H19C H 0.5413 0.3141 0.1274 0.055 Uiso 1 1 calc R . . C29 C 1.2895(12) 0.1375(7) 0.0910(5) 0.044(4) Uani 1 1 d . . . H29A H 1.2307 0.1057 0.0804 0.066 Uiso 1 1 calc R . . H29B H 1.2958 0.1377 0.1194 0.066 Uiso 1 1 calc R . . H29C H 1.3613 0.1237 0.0831 0.066 Uiso 1 1 calc R . . F3 F 0.3360(10) 0.1590(7) 0.2003(4) 0.109(5) Uani 1 1 d . . . C14 C 0.9637(11) 0.3759(7) 0.1775(4) 0.030(3) Uani 1 1 d . . . C39 C 0.7803(12) 0.0602(7) -0.1164(4) 0.038(3) Uani 1 1 d . . . C41 C 0.7452(11) 0.4375(6) -0.0861(4) 0.029(3) Uani 1 1 d . . . C18 C 0.5481(11) 0.3536(7) 0.0038(4) 0.035(3) Uani 1 1 d . . . H18A H 0.5573 0.3108 -0.0097 0.053 Uiso 1 1 calc R . . H18B H 0.5594 0.3914 -0.0135 0.053 Uiso 1 1 calc R . . H18C H 0.4723 0.3559 0.0110 0.053 Uiso 1 1 calc R . . C11 C 0.6970(12) 0.4797(6) 0.1990(5) 0.036(3) Uani 1 1 d . . . C27 C 1.0714(11) 0.1934(7) 0.0954(4) 0.035(3) Uani 1 1 d . . . H27 H 1.0935 0.1542 0.1103 0.042 Uiso 1 1 calc R . . C10 C 0.6366(14) 0.0420(8) 0.1333(5) 0.047(4) Uani 1 1 d . . . C7 C 0.9257(10) 0.0991(6) 0.1849(4) 0.026(3) Uani 1 1 d . . . F1 F 0.3592(10) 0.2582(7) 0.2253(4) 0.094(4) Uani 1 1 d U . . 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 Dy1 0.0197(3) 0.0138(3) 0.0276(4) -0.0004(2) 0.0054(2) -0.0013(2) Dy2 0.0216(3) 0.0170(3) 0.0273(4) 0.0021(2) 0.0041(2) 0.0007(2) Br1 0.0228(7) 0.0321(8) 0.0671(10) 0.0099(6) 0.0110(6) -0.0019(6) Br2 0.0193(6) 0.0361(8) 0.0644(10) -0.0167(7) 0.0071(6) 0.0005(6) O2 0.026(3) 0.016(3) 0.034(4) -0.002(3) 0.002(3) 0.010(3) O6 0.026(5) 0.012(4) 0.043(5) 0.006(3) 0.014(4) 0.003(3) F22 0.049(5) 0.051(6) 0.068(6) 0.018(4) 0.000(4) 0.026(5) O11 0.028(5) 0.030(5) 0.040(6) -0.005(4) 0.017(4) -0.003(4) F23 0.036(5) 0.037(5) 0.131(9) -0.002(5) 0.021(5) 0.001(4) C34 0.034(8) 0.041(9) 0.051(10) -0.004(7) 0.003(6) 0.005(7) C21 0.025(7) 0.043(9) 0.062(11) 0.025(7) -0.003(7) -0.006(7) C8 0.029(7) 0.036(8) 0.040(8) -0.006(6) 0.004(6) 0.011(6) C33 0.039(8) 0.032(7) 0.029(8) -0.001(6) 0.001(6) 0.002(6) C37 0.035(8) 0.022(7) 0.057(10) -0.005(6) -0.004(6) -0.009(6) C58 0.033(8) 0.030(8) 0.056(9) -0.013(6) 0.001(6) -0.017(6) O9 0.030(5) 0.021(4) 0.022(5) 0.002(3) 0.008(3) 0.009(4) F24 0.069(7) 0.061(6) 0.057(6) 0.004(5) 0.021(5) 0.027(5) O4 0.026(4) 0.016(4) 0.036(5) -0.005(3) 0.012(3) 0.005(4) O14 0.035(5) 0.013(4) 0.037(5) 0.006(3) 0.006(4) -0.001(4) F26 0.026(4) 0.038(5) 0.118(8) -0.032(5) 0.034(4) -0.009(4) C36 0.025(6) 0.026(6) 0.033(6) 0.007(5) 0.003(5) -0.013(5) N1 0.010(5) 0.019(5) 0.029(6) 0.001(4) -0.001(4) -0.002(4) O18 0.026(4) 0.013(4) 0.036(5) 0.002(3) 0.002(4) -0.003(4) O8 0.022(5) 0.028(5) 0.056(6) 0.008(4) 0.003(4) 0.013(4) F28 0.047(5) 0.031(5) 0.079(6) 0.025(4) 0.009(4) 0.014(4) F36 0.076(7) 0.028(4) 0.066(6) -0.015(4) 0.036(5) -0.007(4) O1 0.023(4) 0.021(4) 0.033(5) 0.003(3) 0.005(3) -0.001(4) F6 0.054(5) 0.024(4) 0.036(5) 0.008(3) 0.009(4) -0.002(4) O3 0.048(6) 0.022(5) 0.038(6) -0.002(4) 0.003(4) 0.006(4) O12 0.029(5) 0.018(4) 0.028(5) -0.004(3) 0.006(3) -0.008(4) O15 0.023(4) 0.018(4) 0.027(5) 0.000(3) 0.009(3) -0.008(3) O16 0.024(4) 0.024(4) 0.022(5) -0.004(3) 0.008(3) 0.001(4) O5 0.020(4) 0.019(4) 0.035(5) 0.006(3) 0.003(3) -0.006(4) F17 0.047(5) 0.034(5) 0.093(7) -0.002(4) 0.027(4) -0.023(4) F18 0.060(6) 0.062(6) 0.071(6) -0.036(5) 0.033(5) -0.032(5) O17 0.021(5) 0.025(5) 0.049(6) -0.009(4) 0.000(4) -0.012(4) F4 0.064(6) 0.041(5) 0.068(6) 0.016(4) 0.008(5) -0.019(5) N2 0.021(5) 0.013(5) 0.030(6) -0.001(4) 0.001(4) 0.001(4) F34 0.050(5) 0.024(4) 0.088(7) -0.023(4) 0.005(4) -0.012(4) O10 0.030(5) 0.026(5) 0.035(5) -0.009(4) 0.009(4) 0.000(4) F11 0.056(6) 0.051(6) 0.057(6) -0.005(4) -0.014(4) -0.010(5) F35 0.055(6) 0.029(5) 0.076(6) -0.007(4) -0.001(5) 0.016(4) N4 0.024(5) 0.029(6) 0.020(6) 0.006(4) 0.000(4) 0.009(5) F31 0.032(5) 0.047(6) 0.095(7) -0.010(5) 0.009(4) 0.004(4) F5 0.081(7) 0.018(4) 0.058(6) 0.004(4) 0.021(5) 0.014(4) C26 0.031(7) 0.021(6) 0.032(8) -0.003(5) 0.006(5) 0.001(5) F20 0.073(7) 0.046(6) 0.102(8) 0.038(5) 0.039(6) 0.029(5) F15 0.119(10) 0.080(8) 0.077(8) -0.035(6) -0.046(7) 0.057(8) F29 0.052(6) 0.040(6) 0.157(10) 0.006(6) -0.065(7) 0.005(5) F27 0.052(6) 0.038(5) 0.117(8) 0.034(5) -0.019(6) -0.017(5) O13 0.023(4) 0.024(5) 0.031(5) 0.001(3) 0.006(3) -0.006(4) F25 0.036(5) 0.069(7) 0.057(6) -0.015(5) 0.003(4) -0.025(5) C22 0.021(6) 0.023(6) 0.025(7) -0.008(5) 0.001(5) 0.003(5) F19 0.063(6) 0.038(5) 0.073(6) 0.012(4) 0.035(5) 0.003(5) C43 0.026(6) 0.012(6) 0.028(7) -0.003(5) 0.007(5) 0.003(5) C44 0.020(6) 0.013(6) 0.040(8) 0.002(5) 0.005(5) -0.002(5) C53 0.031(7) 0.019(6) 0.020(7) 0.001(5) 0.003(5) 0.010(5) F2 0.041(6) 0.122(11) 0.076(8) 0.027(7) -0.010(5) 0.012(6) C35 0.037(8) 0.026(8) 0.076(12) -0.011(7) 0.005(7) -0.024(7) C48 0.020(6) 0.033(7) 0.035(8) 0.000(5) 0.002(5) 0.012(6) F10 0.078(8) 0.090(9) 0.080(8) 0.006(6) -0.003(6) -0.052(7) F9 0.061(7) 0.016(4) 0.185(11) 0.014(6) 0.045(7) 0.000(5) C45 0.023(7) 0.051(9) 0.029(8) -0.011(6) -0.005(5) -0.006(6) F33 0.031(5) 0.050(6) 0.132(9) -0.031(6) -0.002(5) -0.011(5) C24 0.021(6) 0.011(6) 0.035(7) -0.005(5) 0.006(5) 0.009(5) C56 0.016(6) 0.022(6) 0.035(7) -0.003(5) 0.002(5) -0.003(5) C20 0.010(5) 0.026(6) 0.028(7) 0.004(5) 0.004(4) -0.001(5) C17 0.024(6) 0.022(6) 0.028(7) 0.004(5) 0.006(5) 0.007(5) F30 0.063(7) 0.080(8) 0.090(8) 0.035(6) 0.044(5) 0.057(6) O7 0.028(5) 0.054(6) 0.024(5) 0.015(4) 0.002(4) 0.003(5) C2 0.038(8) 0.018(6) 0.033(8) -0.002(5) 0.011(5) -0.005(6) F14 0.033(5) 0.081(8) 0.147(10) 0.054(7) 0.032(6) 0.012(5) F21 0.089(8) 0.073(8) 0.081(7) 0.014(6) -0.008(6) -0.055(7) C25 0.026(7) 0.030(7) 0.032(8) -0.002(5) 0.004(5) 0.007(6) C42 0.035(7) 0.025(7) 0.034(8) -0.001(5) 0.003(5) -0.002(6) F16 0.021(4) 0.079(7) 0.072(6) 0.026(5) -0.009(4) -0.018(4) C13 0.025(6) 0.012(5) 0.049(7) -0.002(5) 0.009(5) -0.002(5) F8 0.037(6) 0.052(6) 0.121(8) -0.031(6) -0.021(5) 0.016(5) F13 0.052(6) 0.019(4) 0.105(7) 0.006(4) 0.017(5) 0.019(4) N3 0.031(6) 0.017(5) 0.024(6) 0.002(4) 0.008(4) 0.000(4) C1 0.046(8) 0.031(8) 0.036(9) 0.005(6) 0.015(6) -0.005(7) C46 0.017(6) 0.015(6) 0.031(7) -0.006(5) 0.007(5) 0.002(5) F7 0.085(8) 0.040(6) 0.088(8) -0.003(5) 0.027(6) 0.029(5) C52 0.025(6) 0.007(5) 0.037(8) 0.000(5) 0.006(5) 0.006(5) C28 0.026(7) 0.030(7) 0.032(8) 0.000(5) 0.006(5) -0.005(6) C9 0.045(8) 0.028(7) 0.034(8) -0.009(6) 0.003(6) -0.015(6) C57 0.014(6) 0.023(7) 0.040(8) -0.002(5) 0.010(5) 0.000(5) C6 0.034(8) 0.021(7) 0.062(10) -0.004(6) 0.010(7) 0.003(6) C51 0.018(6) 0.018(6) 0.025(7) -0.002(5) 0.006(5) -0.002(5) F32 0.048(6) 0.097(9) 0.131(10) 0.060(8) 0.047(6) 0.014(6) C47 0.047(9) 0.029(7) 0.042(9) 0.001(6) 0.012(6) -0.011(7) C40 0.048(9) 0.014(6) 0.057(10) 0.003(6) 0.006(7) 0.005(6) C23 0.037(7) 0.021(6) 0.021(7) 0.000(5) 0.001(5) 0.001(6) C15 0.048(9) 0.034(8) 0.033(8) -0.001(6) 0.010(6) -0.014(7) C38 0.037(7) 0.011(6) 0.034(8) 0.003(5) -0.004(6) -0.004(5) C4 0.029(7) 0.008(5) 0.040(8) -0.003(5) 0.010(5) 0.005(5) C3 0.032(8) 0.038(8) 0.040(8) -0.009(6) 0.011(6) -0.016(6) C31 0.054(9) 0.024(7) 0.029(8) 0.003(5) -0.002(6) 0.014(7) C30 0.049(9) 0.029(8) 0.050(10) 0.011(7) 0.003(7) -0.003(7) C12 0.022(6) 0.021(6) 0.038(8) 0.004(5) -0.003(5) -0.007(5) C54 0.020(6) 0.023(6) 0.031(7) -0.010(5) 0.006(5) -0.013(5) C5 0.044(9) 0.055(10) 0.040(10) -0.007(7) 0.012(7) -0.024(8) C49 0.006(5) 0.016(6) 0.040(8) -0.004(5) 0.008(5) -0.003(4) C55 0.031(7) 0.038(8) 0.027(7) -0.006(5) 0.004(5) -0.002(6) C32 0.046(8) 0.028(7) 0.032(8) 0.001(5) 0.013(6) 0.009(6) C16 0.016(6) 0.033(8) 0.060(9) 0.000(6) 0.015(5) 0.005(6) C50 0.024(6) 0.027(6) 0.037(6) -0.006(5) 0.007(5) -0.011(5) F12 0.069(8) 0.041(6) 0.189(12) -0.062(7) -0.042(8) 0.008(6) C19 0.033(7) 0.042(8) 0.036(8) 0.000(6) 0.006(6) 0.012(7) C29 0.026(7) 0.023(7) 0.082(11) 0.005(7) 0.001(7) 0.016(6) F3 0.055(7) 0.083(9) 0.182(13) 0.029(9) -0.008(8) -0.037(7) C14 0.027(7) 0.029(7) 0.032(8) 0.004(5) -0.001(5) 0.001(6) C39 0.040(8) 0.023(7) 0.051(10) -0.006(6) 0.006(7) -0.009(6) C41 0.030(7) 0.019(6) 0.036(8) -0.001(5) 0.001(5) 0.010(5) C18 0.025(7) 0.040(8) 0.043(8) 0.001(6) 0.010(5) -0.009(6) C11 0.036(8) 0.009(6) 0.063(10) -0.005(6) 0.008(7) 0.002(6) C27 0.028(7) 0.043(8) 0.032(8) 0.009(6) -0.001(5) 0.014(6) C10 0.044(9) 0.033(8) 0.061(11) 0.006(7) -0.004(8) -0.005(7) C7 0.026(6) 0.016(6) 0.035(8) 0.003(5) 0.009(5) 0.005(5) F1 0.058(6) 0.113(8) 0.107(7) -0.045(6) -0.002(5) 0.031(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O11 2.323(9) . ? Dy1 O18 2.334(8) . ? Dy1 O13 2.342(8) . ? Dy1 O15 2.358(8) . ? Dy1 O9 2.364(8) . ? Dy1 O14 2.365(8) . ? Dy1 O10 2.373(8) . ? Dy1 O12 2.374(8) . ? Dy2 O5 2.306(8) . ? Dy2 O7 2.322(8) . ? Dy2 O4 2.326(8) . ? Dy2 O2 2.330(9) . ? Dy2 O6 2.343(8) . ? Dy2 O1 2.347(8) . ? Dy2 O16 2.387(8) 4_566 ? Dy2 O3 2.397(9) . ? Br1 C25 1.898(14) . ? Br2 C57 1.896(12) . ? O2 C4 1.279(15) . ? O6 C14 1.286(15) . ? F22 C34 1.350(17) . ? O11 C36 1.240(14) . ? F23 C34 1.305(17) . ? C34 F24 1.348(16) . ? C34 C33 1.51(2) . ? C21 C20 1.496(18) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C8 C7 1.360(17) . ? C8 C9 1.436(18) . ? C8 H8 0.9300 . ? C33 O18 1.261(15) . ? C33 C32 1.392(19) . ? C37 C38 1.392(19) . ? C37 C36 1.415(19) . ? C37 H37 0.9300 . ? C58 O17 1.439(14) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? O9 N3 1.276(12) . ? O4 C7 1.261(14) . ? O14 C31 1.261(14) . ? F26 C44 1.340(14) . ? C36 C35 1.481(19) . ? N1 O16 1.290(11) . ? N1 C51 1.350(15) . ? N1 C49 1.534(13) . ? O8 C26 1.330(15) . ? O8 C29 1.434(15) . ? F28 C40 1.315(16) . ? F36 C39 1.311(17) . ? O1 C2 1.279(15) . ? F6 C1 1.354(15) . ? O3 C9 1.246(16) . ? O12 C43 1.233(13) . ? O15 N2 1.270(12) . ? O16 Dy2 2.387(8) 4_565 ? O5 C12 1.269(14) . ? F17 C15 1.350(16) . ? F18 C15 1.322(16) . ? O17 C56 1.330(14) . ? F4 C1 1.322(16) . ? N2 C51 1.386(14) . ? N2 C46 1.500(14) . ? F34 C39 1.330(15) . ? O10 C38 1.239(14) . ? F11 C10 1.331(16) . ? F35 C39 1.339(16) . ? N4 O7 1.290(12) . ? N4 C22 1.366(15) . ? N4 C20 1.505(14) . ? F31 C35 1.399(17) . ? F5 C1 1.300(16) . ? C26 C27 1.385(19) . ? C26 C25 1.413(17) . ? F20 C30 1.356(16) . ? F15 C6 1.340(16) . ? F29 C40 1.266(16) . ? F27 C44 1.346(14) . ? O13 C41 1.265(15) . ? F25 C44 1.315(14) . ? C22 N3 1.343(15) . ? C22 C23 1.455(17) . ? F19 C30 1.352(18) . ? C43 C42 1.399(16) . ? C43 C44 1.541(16) . ? C53 C51 1.393(16) . ? C53 C52 1.415(16) . ? C53 C54 1.418(16) . ? F2 C5 1.301(17) . ? C35 F32 1.299(18) . ? C35 F33 1.311(16) . ? C48 C49 1.538(16) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? F10 C10 1.332(19) . ? F9 C11 1.350(16) . ? C45 C46 1.529(16) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C24 C25 1.383(16) . ? C24 C23 1.389(17) . ? C24 H24 0.9300 . ? C56 C55 1.419(17) . ? C56 C57 1.421(16) . ? C20 C19 1.537(17) . ? C20 C17 1.547(16) . ? C17 C18 1.504(16) . ? C17 N3 1.533(15) . ? C17 C16 1.547(17) . ? F30 C40 1.338(17) . ? C2 C3 1.350(18) . ? C2 C1 1.566(17) . ? F14 C6 1.303(17) . ? F21 C30 1.276(16) . ? C42 C41 1.380(18) . ? C42 H42 0.9300 . ? F16 C15 1.294(15) . ? C13 C12 1.373(17) . ? C13 C14 1.405(17) . ? C13 H13 0.9300 . ? F8 C11 1.247(15) . ? F13 C6 1.332(15) . ? C46 C47 1.518(16) . ? C46 C49 1.581(15) . ? F7 C11 1.333(16) . ? C52 C57 1.350(16) . ? C52 H52 0.9300 . ? C28 C27 1.351(18) . ? C28 C23 1.435(17) . ? C28 H28 0.9300 . ? C9 C10 1.482(19) . ? C6 C7 1.527(17) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C40 C41 1.569(17) . ? C15 C14 1.503(19) . ? C38 C39 1.538(18) . ? C4 C3 1.396(18) . ? C4 C5 1.526(19) . ? C3 H3 0.9300 . ? C31 C32 1.37(2) . ? C31 C30 1.50(2) . ? C12 C11 1.585(18) . ? C54 C55 1.368(17) . ? C54 H54 0.9300 . ? C5 F1 1.246(18) . ? C5 F3 1.347(18) . ? C49 C50 1.531(16) . ? C55 H55 0.9300 . ? C32 H32 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? F12 C10 1.323(18) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C27 H27 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Dy1 O18 137.4(3) . . ? O11 Dy1 O13 73.9(3) . . ? O18 Dy1 O13 148.0(3) . . ? O11 Dy1 O15 103.1(3) . . ? O18 Dy1 O15 91.1(3) . . ? O13 Dy1 O15 71.3(3) . . ? O11 Dy1 O9 91.0(3) . . ? O18 Dy1 O9 104.9(3) . . ? O13 Dy1 O9 75.3(3) . . ? O15 Dy1 O9 138.1(3) . . ? O11 Dy1 O14 73.8(3) . . ? O18 Dy1 O14 73.5(3) . . ? O13 Dy1 O14 134.0(3) . . ? O15 Dy1 O14 148.2(3) . . ? O9 Dy1 O14 73.5(3) . . ? O11 Dy1 O10 72.5(3) . . ? O18 Dy1 O10 74.1(3) . . ? O13 Dy1 O10 122.1(3) . . ? O15 Dy1 O10 72.2(3) . . ? O9 Dy1 O10 149.2(3) . . ? O14 Dy1 O10 76.8(3) . . ? O11 Dy1 O12 147.0(3) . . ? O18 Dy1 O12 75.4(3) . . ? O13 Dy1 O12 74.2(3) . . ? O15 Dy1 O12 74.5(3) . . ? O9 Dy1 O12 72.7(3) . . ? O14 Dy1 O12 125.4(3) . . ? O10 Dy1 O12 133.8(3) . . ? O5 Dy2 O7 81.2(3) . . ? O5 Dy2 O4 150.3(3) . . ? O7 Dy2 O4 95.5(3) . . ? O5 Dy2 O2 73.1(3) . . ? O7 Dy2 O2 94.1(3) . . ? O4 Dy2 O2 136.6(3) . . ? O5 Dy2 O6 73.5(3) . . ? O7 Dy2 O6 73.5(3) . . ? O4 Dy2 O6 77.2(3) . . ? O2 Dy2 O6 145.8(3) . . ? O5 Dy2 O1 123.6(3) . . ? O7 Dy2 O1 144.5(3) . . ? O4 Dy2 O1 74.8(3) . . ? O2 Dy2 O1 73.0(3) . . ? O6 Dy2 O1 134.0(3) . . ? O5 Dy2 O16 72.8(3) . 4_566 ? O7 Dy2 O16 141.1(3) . 4_566 ? O4 Dy2 O16 93.3(3) . 4_566 ? O2 Dy2 O16 105.0(3) . 4_566 ? O6 Dy2 O16 71.7(3) . 4_566 ? O1 Dy2 O16 74.2(3) . 4_566 ? O5 Dy2 O3 131.7(3) . . ? O7 Dy2 O3 68.9(3) . . ? O4 Dy2 O3 72.0(3) . . ? O2 Dy2 O3 72.4(3) . . ? O6 Dy2 O3 127.9(3) . . ? O1 Dy2 O3 75.7(3) . . ? O16 Dy2 O3 149.1(3) 4_566 . ? C4 O2 Dy2 132.9(7) . . ? C14 O6 Dy2 135.5(8) . . ? C36 O11 Dy1 136.1(9) . . ? F23 C34 F24 107.5(13) . . ? F23 C34 F22 109.5(12) . . ? F24 C34 F22 105.2(12) . . ? F23 C34 C33 111.7(12) . . ? F24 C34 C33 110.3(11) . . ? F22 C34 C33 112.4(13) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C7 C8 C9 121.0(12) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? O18 C33 C32 127.4(13) . . ? O18 C33 C34 113.1(13) . . ? C32 C33 C34 119.4(12) . . ? C38 C37 C36 122.2(12) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? O17 C58 H58A 109.5 . . ? O17 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O17 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N3 O9 Dy1 137.9(7) . . ? C7 O4 Dy2 133.9(8) . . ? C31 O14 Dy1 132.3(9) . . ? O11 C36 C37 125.6(12) . . ? O11 C36 C35 120.5(13) . . ? C37 C36 C35 113.8(11) . . ? O16 N1 C51 124.9(9) . . ? O16 N1 C49 120.9(9) . . ? C51 N1 C49 113.8(9) . . ? C33 O18 Dy1 132.1(9) . . ? C26 O8 C29 117.0(11) . . ? C2 O1 Dy2 130.0(7) . . ? C9 O3 Dy2 136.5(9) . . ? C43 O12 Dy1 132.1(7) . . ? N2 O15 Dy1 145.0(7) . . ? N1 O16 Dy2 133.8(7) . 4_565 ? C12 O5 Dy2 135.0(8) . . ? C56 O17 C58 117.2(10) . . ? O15 N2 C51 125.7(10) . . ? O15 N2 C46 120.7(9) . . ? C51 N2 C46 113.0(10) . . ? C38 O10 Dy1 134.0(9) . . ? O7 N4 C22 123.8(10) . . ? O7 N4 C20 121.5(9) . . ? C22 N4 C20 113.4(9) . . ? O8 C26 C27 126.0(11) . . ? O8 C26 C25 117.6(12) . . ? C27 C26 C25 116.4(12) . . ? C41 O13 Dy1 133.0(8) . . ? N3 C22 N4 106.0(10) . . ? N3 C22 C23 126.1(11) . . ? N4 C22 C23 127.9(11) . . ? O12 C43 C42 130.1(12) . . ? O12 C43 C44 113.9(10) . . ? C42 C43 C44 116.0(10) . . ? F25 C44 F26 106.8(10) . . ? F25 C44 F27 106.3(10) . . ? F26 C44 F27 106.3(11) . . ? F25 C44 C43 112.4(10) . . ? F26 C44 C43 111.3(9) . . ? F27 C44 C43 113.3(10) . . ? C51 C53 C52 124.7(11) . . ? C51 C53 C54 119.2(11) . . ? C52 C53 C54 116.1(11) . . ? F32 C35 F33 111.4(13) . . ? F32 C35 F31 103.4(13) . . ? F33 C35 F31 103.1(12) . . ? F32 C35 C36 112.8(13) . . ? F33 C35 C36 115.6(14) . . ? F31 C35 C36 109.4(11) . . ? C49 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C25 C24 C23 118.6(11) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? O17 C56 C55 125.0(11) . . ? O17 C56 C57 119.1(11) . . ? C55 C56 C57 115.9(11) . . ? C21 C20 N4 107.0(10) . . ? C21 C20 C19 112.0(11) . . ? N4 C20 C19 109.5(9) . . ? C21 C20 C17 114.0(10) . . ? N4 C20 C17 99.2(9) . . ? C19 C20 C17 114.2(10) . . ? C18 C17 N3 111.4(10) . . ? C18 C17 C20 115.0(10) . . ? N3 C17 C20 99.7(8) . . ? C18 C17 C16 111.4(10) . . ? N3 C17 C16 104.5(9) . . ? C20 C17 C16 113.8(10) . . ? N4 O7 Dy2 164.5(8) . . ? O1 C2 C3 129.6(12) . . ? O1 C2 C1 110.9(11) . . ? C3 C2 C1 119.5(12) . . ? C24 C25 C26 122.4(12) . . ? C24 C25 Br1 118.5(9) . . ? C26 C25 Br1 119.1(9) . . ? C41 C42 C43 120.3(12) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C12 C13 C14 122.0(12) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? O9 N3 C22 125.8(10) . . ? O9 N3 C17 121.2(9) . . ? C22 N3 C17 112.7(10) . . ? F5 C1 F4 108.1(12) . . ? F5 C1 F6 107.5(12) . . ? F4 C1 F6 106.7(11) . . ? F5 C1 C2 111.5(11) . . ? F4 C1 C2 113.1(11) . . ? F6 C1 C2 109.7(11) . . ? N2 C46 C47 106.7(10) . . ? N2 C46 C45 109.0(10) . . ? C47 C46 C45 112.8(10) . . ? N2 C46 C49 101.2(8) . . ? C47 C46 C49 113.4(10) . . ? C45 C46 C49 112.8(9) . . ? C57 C52 C53 121.4(11) . . ? C57 C52 H52 119.3 . . ? C53 C52 H52 119.3 . . ? C27 C28 C23 118.4(13) . . ? C27 C28 H28 120.8 . . ? C23 C28 H28 120.8 . . ? O3 C9 C8 124.4(12) . . ? O3 C9 C10 115.7(13) . . ? C8 C9 C10 119.9(13) . . ? C52 C57 C56 122.9(11) . . ? C52 C57 Br2 119.4(9) . . ? C56 C57 Br2 117.6(8) . . ? F14 C6 F13 107.2(12) . . ? F14 C6 F15 105.8(13) . . ? F13 C6 F15 103.8(12) . . ? F14 C6 C7 113.2(12) . . ? F13 C6 C7 114.1(11) . . ? F15 C6 C7 112.0(12) . . ? N1 C51 N2 106.0(10) . . ? N1 C51 C53 127.0(10) . . ? N2 C51 C53 127.0(11) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? F29 C40 F28 108.4(12) . . ? F29 C40 F30 108.7(15) . . ? F28 C40 F30 107.3(11) . . ? F29 C40 C41 113.1(11) . . ? F28 C40 C41 112.6(12) . . ? F30 C40 C41 106.6(11) . . ? C24 C23 C28 120.1(11) . . ? C24 C23 C22 119.4(11) . . ? C28 C23 C22 120.5(12) . . ? F16 C15 F18 110.7(14) . . ? F16 C15 F17 107.8(11) . . ? F18 C15 F17 104.4(11) . . ? F16 C15 C14 110.6(11) . . ? F18 C15 C14 111.2(11) . . ? F17 C15 C14 111.8(13) . . ? O10 C38 C37 127.0(12) . . ? O10 C38 C39 112.9(12) . . ? C37 C38 C39 120.2(11) . . ? O2 C4 C3 126.3(11) . . ? O2 C4 C5 113.7(10) . . ? C3 C4 C5 120.0(12) . . ? C2 C3 C4 121.4(12) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? O14 C31 C32 126.9(14) . . ? O14 C31 C30 114.0(13) . . ? C32 C31 C30 119.2(12) . . ? F21 C30 F19 109.9(14) . . ? F21 C30 F20 104.9(13) . . ? F19 C30 F20 105.1(12) . . ? F21 C30 C31 111.9(12) . . ? F19 C30 C31 111.2(12) . . ? F20 C30 C31 113.4(13) . . ? O5 C12 C13 128.7(12) . . ? O5 C12 C11 110.9(11) . . ? C13 C12 C11 120.3(11) . . ? C55 C54 C53 122.6(12) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? F1 C5 F2 111.6(16) . . ? F1 C5 F3 108.5(15) . . ? F2 C5 F3 101.6(12) . . ? F1 C5 C4 112.6(12) . . ? F2 C5 C4 112.3(12) . . ? F3 C5 C4 109.6(14) . . ? C50 C49 N1 110.6(9) . . ? C50 C49 C48 111.8(10) . . ? N1 C49 C48 104.7(9) . . ? C50 C49 C46 116.4(9) . . ? N1 C49 C46 97.8(8) . . ? C48 C49 C46 114.0(10) . . ? C54 C55 C56 121.0(12) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C31 C32 C33 123.1(13) . . ? C31 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O8 C29 H29A 109.5 . . ? O8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O6 C14 C13 125.2(12) . . ? O6 C14 C15 115.0(12) . . ? C13 C14 C15 119.7(12) . . ? F36 C39 F34 107.8(11) . . ? F36 C39 F35 109.1(13) . . ? F34 C39 F35 104.7(11) . . ? F36 C39 C38 111.9(11) . . ? F34 C39 C38 113.1(12) . . ? F35 C39 C38 109.8(11) . . ? O13 C41 C42 129.5(11) . . ? O13 C41 C40 112.7(11) . . ? C42 C41 C40 117.8(11) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? F8 C11 F7 107.7(13) . . ? F8 C11 F9 113.5(12) . . ? F7 C11 F9 102.7(11) . . ? F8 C11 C12 112.5(11) . . ? F7 C11 C12 110.0(11) . . ? F9 C11 C12 109.9(12) . . ? C28 C27 C26 123.9(12) . . ? C28 C27 H27 118.0 . . ? C26 C27 H27 118.0 . . ? F12 C10 F11 106.8(13) . . ? F12 C10 F10 107.0(14) . . ? F11 C10 F10 104.3(13) . . ? F12 C10 C9 114.0(14) . . ? F11 C10 C9 112.7(12) . . ? F10 C10 C9 111.4(14) . . ? O4 C7 C8 130.1(12) . . ? O4 C7 C6 113.1(11) . . ? C8 C7 C6 116.7(11) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.646 _refine_diff_density_min -2.404 _refine_diff_density_rms 0.231 _database_code_depnum_ccdc_archive 'CCDC 958925'