# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_amfun3s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C99 H132 F3 Fe5 N7 O41 S Yb3, 10(C2 H3 N)' _chemical_formula_sum 'C119 H162 F3 Fe5 N17 O41 S Yb3' _chemical_formula_weight 3374.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.4830(8) _cell_length_b 19.8976(9) _cell_length_c 20.2276(9) _cell_angle_alpha 76.119(1) _cell_angle_beta 74.622(1) _cell_angle_gamma 81.570(1) _cell_volume 6185.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13149 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.96 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3412 _exptl_absorpt_coefficient_mu 2.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_T_max 0.588 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49751 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 26.73 _reflns_number_total 25848 _reflns_number_gt 21874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. N-H and O-H distances were restrained: DFIX 0.88 0.04 N1 H11 O1 H1 O7 H7 O10 H10 O13 H13 O16 H16 O19 H19 The non-coordinated oxygen O(22) was disordered and modelled with two 50% occupancy isotropic O atoms. Two carbons bonded to N(1) were also disordered and modelled with partial occupancy atoms. A triflate anion and an MeCN were disordered over an inversion centre (i.e. half an anion and half a MeCN per cluster, which is on a general position). The geometry of this disordered half-MeCN was restrained to be similar to that of the ordered lattice MeCN: SAME N111 C111 C112 The other half anion was disordered against lattice MeCN over three sites, and this and a total of 8.5 MeCN per cluster were handled using SQUEEZE (see below). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.006 0.007 0.049 10 3 ' ' 2 -0.027 0.344 0.721 420 229 ; 0.5 triflate (37 e) + 8.5 MeCN (187 e) = 224 e ; 3 0.027 0.657 0.278 420 224 ; 0.5 triflate (37 e) + 8.5 MeCN (187 e) = 224 e ; 4 -0.007 0.992 0.948 8 2 ' ' 5 0.190 0.260 0.115 7 0 ' ' 6 0.809 0.740 0.885 7 0 ' ' _platon_squeeze_details ; ; _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^)+(0.0463P)^2^+0.9104P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25848 _refine_ls_number_parameters 1526 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Yb1 Yb 0.195707(8) -0.016715(7) 0.291196(7) 0.01649(4) Uani 1 1 d . A . Yb2 Yb 0.650253(9) 0.177742(7) 0.091868(7) 0.01699(4) Uani 1 1 d . . . Yb3 Yb 0.401221(8) 0.382398(7) 0.267328(7) 0.01600(4) Uani 1 1 d . . . Fe1 Fe 0.40414(3) -0.05578(2) 0.22576(2) 0.01566(9) Uani 1 1 d . . . Fe2 Fe 0.56414(3) 0.02047(2) 0.15937(2) 0.01626(9) Uani 1 1 d . . . Fe3 Fe 0.14128(3) 0.15020(2) 0.31400(2) 0.01963(10) Uani 1 1 d . . . Fe4 Fe 0.22307(3) 0.28328(2) 0.31116(2) 0.01839(10) Uani 1 1 d . . . Fe5 Fe 0.57164(3) 0.32955(2) 0.14827(2) 0.01680(10) Uani 1 1 d . . . O1 O 0.48640(14) -0.03088(11) 0.13533(11) 0.0181(5) Uani 1 1 d D . . H1 H 0.511(2) -0.0493(18) 0.1060(17) 0.022 Uiso 1 1 d D . . N1 N 0.41982(17) 0.16353(13) 0.29187(13) 0.0162(5) Uani 1 1 d D . . H11 H 0.385(2) 0.1965(16) 0.3187(17) 0.019 Uiso 1 1 d D . . C1 C 0.3962(2) 0.09141(16) 0.33004(17) 0.0193(7) Uani 1 1 d . . . H1A H 0.3399 0.0857 0.3246 0.023 Uiso 1 1 calc R . . H1B H 0.3918 0.0869 0.3807 0.023 Uiso 1 1 calc R . . C2 C 0.4589(2) 0.03279(16) 0.30452(16) 0.0177(6) Uani 1 1 d . . . H2A H 0.5166 0.0414 0.3044 0.021 Uiso 1 1 calc R . . H2B H 0.4452 -0.0118 0.3377 0.021 Uiso 1 1 calc R . . O2 O 0.45758(13) 0.02699(11) 0.23618(11) 0.0167(4) Uani 1 1 d . . . C3 C 0.40322(19) 0.18647(16) 0.21954(16) 0.0166(6) Uani 1 1 d . . . H3A H 0.4456 0.1610 0.1874 0.020 Uiso 1 1 calc R . . H3B H 0.4113 0.2366 0.2025 0.020 Uiso 1 1 calc R . . C4 C 0.31486(19) 0.17481(17) 0.21586(17) 0.0193(7) Uani 1 1 d . . . H4A H 0.3069 0.1971 0.1684 0.023 Uiso 1 1 calc R . . H4B H 0.3112 0.1243 0.2226 0.023 Uiso 1 1 calc R . . O3 O 0.24875(13) 0.20115(11) 0.26594(11) 0.0183(5) Uani 1 1 d . . . C5 C 0.5100(2) 0.17129(16) 0.29044(17) 0.0181(6) Uani 1 1 d . . . H5A H 0.5470 0.1617 0.2458 0.022 Uiso 1 1 calc R . . H5B H 0.5271 0.1360 0.3291 0.022 Uiso 1 1 calc R . . C6 C 0.5238(2) 0.24238(16) 0.29743(16) 0.0181(6) Uani 1 1 d . . . H6A H 0.4912 0.2503 0.3440 0.022 Uiso 1 1 calc R . . H6B H 0.5844 0.2440 0.2947 0.022 Uiso 1 1 calc R . . O4 O 0.49919(13) 0.29580(11) 0.24511(11) 0.0171(5) Uani 1 1 d . . . N2 N 0.17348(19) -0.07796(16) 0.41834(15) 0.0316(7) Uani 1 1 d . . . C7 C 0.2399(2) -0.13561(18) 0.42335(18) 0.0250(7) Uani 1 1 d . A . H7A H 0.2270 -0.1737 0.4050 0.030 Uiso 1 1 calc R . . H7B H 0.2411 -0.1538 0.4732 0.030 Uiso 1 1 calc R . . C8 C 0.3259(2) -0.1119(2) 0.38187(19) 0.0347(9) Uani 1 1 d . . . H8A H 0.3477 -0.0864 0.4090 0.042 Uiso 1 1 calc R A . H8B H 0.3662 -0.1529 0.3738 0.042 Uiso 1 1 calc R . . O5 O 0.31929(13) -0.06803(11) 0.31646(11) 0.0182(5) Uani 1 1 d . A . C9A C 0.1585(5) -0.0308(3) 0.4613(3) 0.0336(15) Uani 0.62 1 d P A 1 H9A1 H 0.1817 -0.0525 0.5026 0.040 Uiso 0.62 1 calc PR A 1 H9A2 H 0.0966 -0.0222 0.4785 0.040 Uiso 0.62 1 calc PR A 1 C9B C 0.2116(6) -0.0231(4) 0.4551(4) 0.0171(18) Uiso 0.38 1 d P A 2 H9B1 H 0.1865 -0.0320 0.5063 0.021 Uiso 0.38 1 calc PR A 2 H9B2 H 0.2736 -0.0330 0.4478 0.021 Uiso 0.38 1 calc PR A 2 C10 C 0.1947(4) 0.0393(3) 0.4289(2) 0.0559(15) Uani 1 1 d . . . H10A H 0.1605 0.0747 0.4544 0.067 Uiso 0.62 1 calc PR A 1 H10B H 0.2531 0.0359 0.4346 0.067 Uiso 0.62 1 calc PR A 1 H10C H 0.2348 0.0664 0.4382 0.067 Uiso 0.38 1 calc PR A 2 H10D H 0.1377 0.0536 0.4556 0.067 Uiso 0.38 1 calc PR A 2 O6 O 0.19543(14) 0.06136(12) 0.35656(11) 0.0205(5) Uani 1 1 d . A . C11A C 0.0907(4) -0.1183(3) 0.4328(3) 0.0314(14) Uani 0.62 1 d P A 1 H11A H 0.1063 -0.1597 0.4116 0.038 Uiso 0.62 1 calc PR A 1 H11B H 0.0697 -0.1346 0.4841 0.038 Uiso 0.62 1 calc PR A 1 C11B C 0.0907(6) -0.0833(5) 0.4566(5) 0.024(2) Uiso 0.38 1 d P A 2 H11C H 0.0731 -0.0454 0.4827 0.029 Uiso 0.38 1 calc PR A 2 H11D H 0.0868 -0.1281 0.4912 0.029 Uiso 0.38 1 calc PR A 2 C12 C 0.0292(3) -0.0791(3) 0.4072(2) 0.0568(14) Uani 1 1 d . . . H12A H -0.0045 -0.0531 0.4429 0.068 Uiso 0.62 1 calc PR A 1 H12B H -0.0084 -0.1103 0.4008 0.068 Uiso 0.62 1 calc PR A 1 H12C H 0.0297 -0.1256 0.3974 0.068 Uiso 0.38 1 calc PR A 2 H12D H -0.0291 -0.0652 0.4316 0.068 Uiso 0.38 1 calc PR A 2 O7 O 0.05343(15) -0.03045(12) 0.34260(13) 0.0244(5) Uani 1 1 d D A . H7 H 0.022(2) -0.0002(18) 0.337(2) 0.029 Uiso 1 1 d D . . N3 N 0.14703(17) -0.01434(14) 0.18190(14) 0.0203(6) Uani 1 1 d . . . C13 C 0.2222(2) -0.01182(19) 0.12175(18) 0.0256(7) Uani 1 1 d . A . H13A H 0.2047 0.0125 0.0783 0.031 Uiso 1 1 calc R . . H13B H 0.2439 -0.0599 0.1169 0.031 Uiso 1 1 calc R . . C14 C 0.2929(2) 0.02465(18) 0.12918(17) 0.0230(7) Uani 1 1 d . . . H14A H 0.3455 0.0149 0.0943 0.028 Uiso 1 1 calc R A . H14B H 0.2780 0.0755 0.1205 0.028 Uiso 1 1 calc R . . O8 O 0.30564(13) 0.00045(11) 0.19796(11) 0.0179(5) Uani 1 1 d . A . C15 C 0.0846(2) 0.04655(19) 0.17251(19) 0.0281(8) Uani 1 1 d . A . H15A H 0.0298 0.0359 0.2057 0.034 Uiso 1 1 calc R . . H15B H 0.0763 0.0561 0.1243 0.034 Uiso 1 1 calc R . . C16 C 0.1134(2) 0.11115(18) 0.18490(19) 0.0259(8) Uani 1 1 d . . . H16A H 0.1583 0.1302 0.1441 0.031 Uiso 1 1 calc R A . H16B H 0.0654 0.1472 0.1902 0.031 Uiso 1 1 calc R . . O9 O 0.14488(14) 0.09329(11) 0.24690(11) 0.0191(5) Uani 1 1 d . A . C17 C 0.1053(2) -0.07894(19) 0.19337(19) 0.0270(8) Uani 1 1 d . A . H17A H 0.0961 -0.0837 0.1484 0.032 Uiso 1 1 calc R . . H17B H 0.0495 -0.0756 0.2267 0.032 Uiso 1 1 calc R . . C18 C 0.1576(3) -0.14204(19) 0.2219(2) 0.0308(8) Uani 1 1 d . . . H18A H 0.1233 -0.1824 0.2389 0.037 Uiso 1 1 calc R A . H18B H 0.2066 -0.1529 0.1843 0.037 Uiso 1 1 calc R . . O10 O 0.18664(15) -0.12952(12) 0.27855(13) 0.0235(5) Uani 1 1 d D A . H10 H 0.230(2) -0.1554(18) 0.279(2) 0.028 Uiso 1 1 d D . . N4 N 0.78163(17) 0.14514(14) 0.14120(15) 0.0230(6) Uani 1 1 d . . . C19 C 0.7516(2) 0.10909(18) 0.21562(18) 0.0246(7) Uani 1 1 d . . . H19A H 0.7198 0.1434 0.2435 0.030 Uiso 1 1 calc R . . H19B H 0.8008 0.0879 0.2351 0.030 Uiso 1 1 calc R . . C20 C 0.6960(2) 0.05373(17) 0.22153(18) 0.0232(7) Uani 1 1 d . . . H20A H 0.7307 0.0139 0.2037 0.028 Uiso 1 1 calc R . . H20B H 0.6676 0.0370 0.2714 0.028 Uiso 1 1 calc R . . O11 O 0.63443(13) 0.08097(11) 0.18192(11) 0.0174(5) Uani 1 1 d . . . C21 C 0.8142(2) 0.21135(17) 0.13821(19) 0.0248(7) Uani 1 1 d . . . H21A H 0.8387 0.2331 0.0888 0.030 Uiso 1 1 calc R . . H21B H 0.8595 0.2022 0.1639 0.030 Uiso 1 1 calc R . . C22 C 0.7431(2) 0.26100(18) 0.17079(19) 0.0232(7) Uani 1 1 d . . . H22C H 0.7346 0.2496 0.2224 0.028 Uiso 1 1 calc R . . H22D H 0.7589 0.3094 0.1534 0.028 Uiso 1 1 calc R . . O12 O 0.66673(14) 0.25505(11) 0.15280(12) 0.0200(5) Uani 1 1 d . . . C23 C 0.8461(2) 0.09865(18) 0.1017(2) 0.0283(8) Uani 1 1 d . . . H23A H 0.8412 0.0498 0.1275 0.034 Uiso 1 1 calc R . . H23B H 0.9033 0.1107 0.0985 0.034 Uiso 1 1 calc R . . C24 C 0.8345(2) 0.10543(19) 0.0285(2) 0.0296(8) Uani 1 1 d . . . H24A H 0.8525 0.1507 -0.0009 0.035 Uiso 1 1 calc R . . H24B H 0.8706 0.0682 0.0070 0.035 Uiso 1 1 calc R . . O13 O 0.74772(15) 0.10069(12) 0.02984(13) 0.0241(5) Uani 1 1 d D . . H13 H 0.734(2) 0.0619(16) 0.044(2) 0.029 Uiso 1 1 d D . . N5 N 0.60178(19) 0.21010(14) -0.02186(14) 0.0241(6) Uani 1 1 d . . . C25 C 0.5714(2) 0.14664(17) -0.03095(17) 0.0256(8) Uani 1 1 d . . . H25A H 0.6204 0.1131 -0.0440 0.031 Uiso 1 1 calc R . . H25B H 0.5418 0.1593 -0.0694 0.031 Uiso 1 1 calc R . . C26 C 0.5126(2) 0.11342(18) 0.03553(17) 0.0231(7) Uani 1 1 d . . . H26A H 0.4575 0.1416 0.0425 0.028 Uiso 1 1 calc R . . H26B H 0.5028 0.0664 0.0325 0.028 Uiso 1 1 calc R . . O14 O 0.54952(14) 0.10874(11) 0.09296(11) 0.0187(5) Uani 1 1 d . . . C27 C 0.5334(2) 0.26843(18) -0.01779(18) 0.0288(8) Uani 1 1 d . . . H27A H 0.4925 0.2629 -0.0438 0.035 Uiso 1 1 calc R . . H27B H 0.5584 0.3130 -0.0407 0.035 Uiso 1 1 calc R . . C28 C 0.4868(2) 0.27106(18) 0.05757(17) 0.0229(7) Uani 1 1 d . . . H28A H 0.4294 0.2540 0.0779 0.027 Uiso 1 1 calc R . . O15 O 0.54598(14) 0.26213(11) 0.09969(11) 0.0187(5) Uani 1 1 d . . . C29 C 0.6753(3) 0.2309(2) -0.08021(19) 0.0338(9) Uani 1 1 d . . . H29A H 0.6557 0.2522 -0.1234 0.041 Uiso 1 1 calc R . . H29B H 0.7138 0.1891 -0.0888 0.041 Uiso 1 1 calc R . . C30 C 0.7229(3) 0.28195(19) -0.06431(19) 0.0346(9) Uani 1 1 d . . . H30A H 0.7771 0.2885 -0.0998 0.042 Uiso 1 1 calc R . . H30B H 0.6893 0.3275 -0.0654 0.042 Uiso 1 1 calc R . . O16 O 0.73819(16) 0.25457(12) 0.00401(13) 0.0257(5) Uani 1 1 d D . . H16 H 0.758(2) 0.2791(19) 0.020(2) 0.031 Uiso 1 1 d D . . N6 N 0.34663(17) 0.49181(14) 0.18733(14) 0.0202(6) Uani 1 1 d . . . C31 C 0.2668(2) 0.47532(18) 0.17577(18) 0.0244(7) Uani 1 1 d . . . H31A H 0.2594 0.5025 0.1295 0.029 Uiso 1 1 calc R . . H31B H 0.2186 0.4898 0.2121 0.029 Uiso 1 1 calc R . . C32 C 0.2655(2) 0.39818(18) 0.17824(18) 0.0252(7) Uani 1 1 d . . . H32A H 0.2091 0.3890 0.1757 0.030 Uiso 1 1 calc R . . H32B H 0.3078 0.3846 0.1377 0.030 Uiso 1 1 calc R . . O17 O 0.28435(14) 0.35842(11) 0.24224(11) 0.0202(5) Uani 1 1 d . . . C33 C 0.4125(2) 0.50745(16) 0.12137(17) 0.0212(7) Uani 1 1 d . . . H33A H 0.4589 0.5280 0.1300 0.025 Uiso 1 1 calc R . . H33B H 0.3881 0.5420 0.0861 0.025 Uiso 1 1 calc R . . C34 C 0.4476(2) 0.44249(16) 0.09288(17) 0.0209(7) Uani 1 1 d . . . H34A H 0.4063 0.4292 0.0717 0.025 Uiso 1 1 calc R . . H34B H 0.5003 0.4516 0.0560 0.025 Uiso 1 1 calc R . . O18 O 0.46451(14) 0.38772(11) 0.14810(11) 0.0184(5) Uani 1 1 d . . . C35 C 0.3313(2) 0.55207(17) 0.22169(18) 0.0246(7) Uani 1 1 d . . . H35A H 0.2967 0.5899 0.1974 0.030 Uiso 1 1 calc R . . H35B H 0.3860 0.5696 0.2178 0.030 Uiso 1 1 calc R . . C36 C 0.2864(2) 0.53210(17) 0.29805(18) 0.0253(8) Uani 1 1 d . . . H36A H 0.2919 0.5675 0.3233 0.030 Uiso 1 1 calc R . . H36B H 0.2256 0.5296 0.3025 0.030 Uiso 1 1 calc R . . O19 O 0.32347(15) 0.46595(12) 0.32770(12) 0.0220(5) Uani 1 1 d D . . H19 H 0.345(2) 0.466(2) 0.3590(17) 0.026 Uiso 1 1 d D . . N7 N 0.16449(18) 0.32938(15) 0.40661(15) 0.0252(6) Uani 1 1 d . . . C37 C 0.2312(2) 0.31608(19) 0.44712(19) 0.0282(8) Uani 1 1 d . . . H37A H 0.2051 0.3004 0.4976 0.034 Uiso 1 1 calc R . . H37B H 0.2568 0.3599 0.4410 0.034 Uiso 1 1 calc R . . C38 C 0.2998(2) 0.26121(17) 0.42282(17) 0.0236(7) Uani 1 1 d . . . H38A H 0.3492 0.2611 0.4420 0.028 Uiso 1 1 calc R . . H38B H 0.2783 0.2147 0.4401 0.028 Uiso 1 1 calc R . . O20 O 0.32463(14) 0.27621(11) 0.34756(11) 0.0198(5) Uani 1 1 d . . . C39 C 0.0882(2) 0.29172(19) 0.4445(2) 0.0315(9) Uani 1 1 d . . . H39A H 0.0418 0.3101 0.4206 0.038 Uiso 1 1 calc R . . H39B H 0.0693 0.2995 0.4930 0.038 Uiso 1 1 calc R . . C40 C 0.1076(2) 0.21475(19) 0.44632(19) 0.0308(8) Uani 1 1 d . . . H40A H 0.1392 0.1931 0.4826 0.037 Uiso 1 1 calc R . . H40B H 0.0544 0.1922 0.4581 0.037 Uiso 1 1 calc R . . O21 O 0.15688(14) 0.20559(12) 0.37930(12) 0.0229(5) Uani 1 1 d . . . C41 C 0.1392(2) 0.40507(18) 0.3860(2) 0.0308(8) Uani 1 1 d . C . H41A H 0.0986 0.4113 0.3562 0.037 Uiso 1 1 calc R . . H41B H 0.1898 0.4286 0.3573 0.037 Uiso 1 1 calc R . . C42 C 0.0989(3) 0.4408(2) 0.4479(2) 0.0440(11) Uani 1 1 d . . . H42A H 0.1242 0.4186 0.4880 0.053 Uiso 0.50 1 calc PR B 1 H42B H 0.1102 0.4904 0.4341 0.053 Uiso 0.50 1 calc PR B 1 H42C H 0.0440 0.4228 0.4742 0.053 Uiso 0.50 1 d PR B 2 H42D H 0.1367 0.4326 0.4803 0.053 Uiso 0.50 1 d PR B 2 O22A O 0.0070(4) 0.4353(4) 0.4690(4) 0.070(2) Uani 0.50 1 d P C 1 H22A H -0.0158 0.4620 0.4387 0.105 Uiso 0.50 1 calc PR C 1 O22B O 0.0882(4) 0.5145(3) 0.4171(3) 0.0525(17) Uani 0.50 1 d P C 2 H22B H 0.0662 0.5366 0.4489 0.079 Uiso 0.50 1 calc PR C 2 O23 O 0.49155(14) -0.12038(11) 0.27600(11) 0.0190(5) Uani 1 1 d . . . O24 O 0.60838(14) -0.06365(11) 0.22593(12) 0.0215(5) Uani 1 1 d . . . C43 C 0.5695(2) -0.11466(16) 0.26511(17) 0.0193(7) Uani 1 1 d . . . C44 C 0.6214(2) -0.17270(17) 0.30201(18) 0.0247(7) Uani 1 1 d . . . C45 C 0.5905(2) -0.23665(17) 0.33445(17) 0.0246(7) Uani 1 1 d . . . H45A H 0.5346 -0.2438 0.3349 0.030 Uiso 1 1 calc R . . C46 C 0.6404(3) -0.2901(2) 0.3662(2) 0.0342(9) Uani 1 1 d . . . H46A H 0.6195 -0.3343 0.3869 0.041 Uiso 1 1 calc R . . C47 C 0.7204(3) -0.2793(2) 0.3677(2) 0.0462(11) Uani 1 1 d . . . H47A H 0.7543 -0.3158 0.3900 0.055 Uiso 1 1 calc R . . C48 C 0.7513(3) -0.2160(2) 0.3373(3) 0.0674(17) Uani 1 1 d . . . H48A H 0.8060 -0.2084 0.3394 0.081 Uiso 1 1 calc R . . C49 C 0.7022(3) -0.1627(2) 0.3032(3) 0.0521(13) Uani 1 1 d . . . H49A H 0.7244 -0.1193 0.2807 0.063 Uiso 1 1 calc R . . O25 O 0.08140(15) 0.23060(12) 0.25127(13) 0.0257(5) Uani 1 1 d . . . O26 O 0.11930(14) 0.32473(12) 0.27433(13) 0.0249(5) Uani 1 1 d . . . C50 C 0.0803(2) 0.29573(18) 0.24389(19) 0.0245(7) Uani 1 1 d . . . C51 C 0.0319(2) 0.34189(18) 0.19520(19) 0.0268(8) Uani 1 1 d . . . C52 C 0.0285(2) 0.4141(2) 0.1860(2) 0.0351(9) Uani 1 1 d . . . H52A H 0.0551 0.4334 0.2125 0.042 Uiso 1 1 calc R . . C53 C -0.0130(3) 0.4575(2) 0.1390(2) 0.0435(11) Uani 1 1 d . . . H53A H -0.0152 0.5065 0.1333 0.052 Uiso 1 1 calc R . . C54 C -0.0516(3) 0.4291(2) 0.0999(2) 0.0490(12) Uani 1 1 d . . . H54A H -0.0796 0.4588 0.0669 0.059 Uiso 1 1 calc R . . C55 C -0.0495(3) 0.3583(3) 0.1089(3) 0.0530(13) Uani 1 1 d . . . H55A H -0.0766 0.3393 0.0825 0.064 Uiso 1 1 calc R . . C56 C -0.0079(2) 0.3145(2) 0.1563(2) 0.0386(10) Uani 1 1 d . . . H56A H -0.0067 0.2656 0.1623 0.046 Uiso 1 1 calc R . . O27 O 0.62644(14) 0.38702(11) 0.19389(12) 0.0210(5) Uani 1 1 d . . . O28 O 0.51350(14) 0.44602(11) 0.25179(12) 0.0208(5) Uani 1 1 d . . . C57 C 0.5920(2) 0.42819(17) 0.23456(17) 0.0213(7) Uani 1 1 d . . . C58 C 0.6501(2) 0.45765(17) 0.26388(18) 0.0229(7) Uani 1 1 d . . . C59 C 0.7357(2) 0.4605(2) 0.2307(2) 0.0375(10) Uani 1 1 d . . . H59A H 0.7580 0.4427 0.1893 0.045 Uiso 1 1 calc R . . C60 C 0.7880(3) 0.4888(3) 0.2576(3) 0.0574(14) Uani 1 1 d . . . H60A H 0.8455 0.4929 0.2333 0.069 Uiso 1 1 calc R . . C61 C 0.7566(3) 0.5118(3) 0.3209(3) 0.0550(14) Uani 1 1 d . . . H61A H 0.7929 0.5299 0.3404 0.066 Uiso 1 1 calc R . . C62 C 0.6731(2) 0.5076(2) 0.3542(2) 0.0366(9) Uani 1 1 d . . . H62A H 0.6517 0.5230 0.3971 0.044 Uiso 1 1 calc R . . C63 C 0.6191(2) 0.48137(17) 0.32666(18) 0.0244(7) Uani 1 1 d . . . H63A H 0.5611 0.4794 0.3502 0.029 Uiso 1 1 calc R . . O29 O 0.38439(15) -0.14280(11) 0.20021(12) 0.0216(5) Uani 1 1 d . . . O30 O 0.31341(16) -0.22363(12) 0.28267(14) 0.0316(6) Uani 1 1 d . . . C64 C 0.3779(2) -0.20420(17) 0.23787(17) 0.0213(7) Uani 1 1 d . . . C65 C 0.4528(2) -0.25644(17) 0.22501(17) 0.0222(7) Uani 1 1 d . . . C66 C 0.5301(2) -0.23645(18) 0.18152(17) 0.0266(8) Uani 1 1 d . . . H66A H 0.5354 -0.1893 0.1579 0.032 Uiso 1 1 calc R . . C67 C 0.5996(3) -0.28519(19) 0.1725(2) 0.0322(9) Uani 1 1 d . . . H67A H 0.6522 -0.2714 0.1428 0.039 Uiso 1 1 calc R . . C68 C 0.5918(3) -0.3541(2) 0.2069(2) 0.0372(9) Uani 1 1 d . . . H68A H 0.6396 -0.3872 0.2017 0.045 Uiso 1 1 calc R . . C69 C 0.5148(3) -0.37487(19) 0.2486(2) 0.0343(9) Uani 1 1 d . . . H69A H 0.5092 -0.4224 0.2705 0.041 Uiso 1 1 calc R . . C70 C 0.4455(2) -0.32579(18) 0.25852(19) 0.0266(8) Uani 1 1 d . . . H70A H 0.3930 -0.3398 0.2883 0.032 Uiso 1 1 calc R . . O31 O 0.66792(14) -0.01513(11) 0.08566(12) 0.0220(5) Uani 1 1 d . . . O32 O 0.61766(15) -0.10418(12) 0.06277(13) 0.0262(5) Uani 1 1 d . . . C71 C 0.6761(2) -0.07459(17) 0.06756(16) 0.0212(7) Uani 1 1 d . . . C72 C 0.7649(2) -0.10886(17) 0.05081(18) 0.0240(7) Uani 1 1 d . . . C73 C 0.8284(2) -0.0904(2) 0.0734(2) 0.0403(10) Uani 1 1 d . . . H73A H 0.8168 -0.0553 0.1000 0.048 Uiso 1 1 calc R . . C74 C 0.9106(3) -0.1234(3) 0.0573(3) 0.0639(16) Uani 1 1 d . . . H74A H 0.9548 -0.1101 0.0722 0.077 Uiso 1 1 calc R . . C75 C 0.9265(3) -0.1759(2) 0.0193(3) 0.0508(12) Uani 1 1 d . . . H75A H 0.9819 -0.1984 0.0082 0.061 Uiso 1 1 calc R . . C76 C 0.8630(3) -0.1950(2) -0.0022(2) 0.0399(10) Uani 1 1 d . . . H76A H 0.8745 -0.2307 -0.0282 0.048 Uiso 1 1 calc R . . C77 C 0.7815(2) -0.16250(18) 0.01393(18) 0.0286(8) Uani 1 1 d . . . H77A H 0.7373 -0.1768 -0.0001 0.034 Uiso 1 1 calc R . . O33 O 0.02513(14) 0.13248(12) 0.37341(13) 0.0252(5) Uani 1 1 d . . . O34 O -0.06168(16) 0.07341(15) 0.34714(18) 0.0452(8) Uani 1 1 d . . . C78 C -0.0450(2) 0.12607(18) 0.36087(18) 0.0237(7) Uani 1 1 d . . . C79 C -0.1115(2) 0.18692(19) 0.36387(18) 0.0280(8) Uani 1 1 d . . . C80 C -0.1928(2) 0.1801(2) 0.36221(19) 0.0346(9) Uani 1 1 d . . . H80A H -0.2079 0.1368 0.3594 0.042 Uiso 1 1 calc R . . C81 C -0.2533(3) 0.2377(3) 0.3646(2) 0.0456(11) Uani 1 1 d . . . H81A H -0.3100 0.2330 0.3652 0.055 Uiso 1 1 calc R . . C82 C -0.2300(3) 0.3013(3) 0.3661(3) 0.0600(14) Uani 1 1 d . . . H82A H -0.2706 0.3405 0.3656 0.072 Uiso 1 1 calc R . . C83 C -0.1497(3) 0.3087(3) 0.3684(3) 0.0691(17) Uani 1 1 d . . . H83A H -0.1347 0.3523 0.3707 0.083 Uiso 1 1 calc R . . C84 C -0.0899(3) 0.2509(2) 0.3674(2) 0.0451(11) Uani 1 1 d . . . H84A H -0.0340 0.2554 0.3692 0.054 Uiso 1 1 calc R . . O35 O 0.63344(14) 0.39149(12) 0.05770(12) 0.0227(5) Uani 1 1 d . . . O36 O 0.77369(15) 0.37012(12) 0.02400(13) 0.0297(6) Uani 1 1 d . . . C85 C 0.7088(2) 0.41041(18) 0.03762(17) 0.0222(7) Uani 1 1 d . . . C86 C 0.7188(2) 0.48652(17) 0.02813(17) 0.0214(7) Uani 1 1 d . . . C87 C 0.6523(2) 0.53032(18) 0.05617(18) 0.0254(7) Uani 1 1 d . . . H87A H 0.6002 0.5122 0.0819 0.030 Uiso 1 1 calc R . . C88 C 0.6608(2) 0.60036(19) 0.04713(19) 0.0299(8) Uani 1 1 d . . . H88A H 0.6147 0.6301 0.0666 0.036 Uiso 1 1 calc R . . C89 C 0.7374(3) 0.62719(19) 0.0092(2) 0.0343(9) Uani 1 1 d . . . H89A H 0.7432 0.6753 0.0026 0.041 Uiso 1 1 calc R . . C90 C 0.8041(2) 0.58416(19) -0.0185(2) 0.0314(8) Uani 1 1 d . . . H90A H 0.8562 0.6024 -0.0440 0.038 Uiso 1 1 calc R . . C91 C 0.7952(2) 0.51321(18) -0.00922(18) 0.0258(8) Uani 1 1 d . . . H91A H 0.8413 0.4834 -0.0284 0.031 Uiso 1 1 calc R . . O37 O 0.43513(14) 0.35982(11) 0.37526(11) 0.0212(5) Uani 1 1 d . . . O38 O 0.39516(17) 0.45193(12) 0.42535(13) 0.0301(6) Uani 1 1 d . . . C92 C 0.4379(2) 0.39440(17) 0.41923(17) 0.0217(7) Uani 1 1 d . . . C93 C 0.4958(2) 0.36588(17) 0.46745(17) 0.0214(7) Uani 1 1 d . . . C94 C 0.5400(2) 0.30061(18) 0.46751(18) 0.0272(8) Uani 1 1 d . . . H94A H 0.5333 0.2733 0.4370 0.033 Uiso 1 1 calc R . . C95 C 0.5937(3) 0.2754(2) 0.5122(2) 0.0340(9) Uani 1 1 d . . . H95A H 0.6235 0.2307 0.5121 0.041 Uiso 1 1 calc R . . C96 C 0.6044(3) 0.3146(2) 0.5566(2) 0.0348(9) Uani 1 1 d . . . H96A H 0.6413 0.2971 0.5870 0.042 Uiso 1 1 calc R . . C97 C 0.5606(3) 0.3798(2) 0.5566(2) 0.0356(9) Uani 1 1 d . . . H97A H 0.5679 0.4071 0.5869 0.043 Uiso 1 1 calc R . . C98 C 0.5063(2) 0.40534(18) 0.51261(18) 0.0266(8) Uani 1 1 d . . . H98A H 0.4761 0.4498 0.5132 0.032 Uiso 1 1 calc R . . N111 N 0.8815(3) -0.0536(2) 0.2481(3) 0.0674(14) Uani 1 1 d D . . C111 C 0.8475(3) -0.0498(3) 0.3056(4) 0.0600(16) Uani 1 1 d D . . C112 C 0.8010(4) -0.0444(3) 0.3774(3) 0.085(2) Uani 1 1 d D . . H11E H 0.7406 -0.0338 0.3790 0.127 Uiso 1 1 calc R . . H11F H 0.8216 -0.0072 0.3910 0.127 Uiso 1 1 calc R . . H11G H 0.8097 -0.0886 0.4098 0.127 Uiso 1 1 calc R . . O44 O 0.5652(5) 0.0346(3) 0.4091(3) 0.061(2) Uani 0.50 1 d P D -1 O45 O 0.6330(7) 0.1124(8) 0.4482(7) 0.072(4) Uani 0.50 1 d P D -1 O46 O 0.6092(4) -0.0017(3) 0.5168(3) 0.0467(15) Uani 0.50 1 d P D -1 S2 S 0.58311(14) 0.05467(10) 0.46637(10) 0.0339(4) Uani 0.50 1 d P D -1 C100 C 0.4815(6) 0.0881(5) 0.5135(5) 0.040(2) Uani 0.50 1 d P D -1 F4 F 0.4467(4) 0.1423(3) 0.4733(3) 0.0617(16) Uani 0.50 1 d P D -1 F5 F 0.4864(5) 0.1124(4) 0.5672(3) 0.075(2) Uani 0.50 1 d P D -1 F6 F 0.4273(4) 0.0420(4) 0.5363(5) 0.109(3) Uani 0.50 1 d P D -1 N211 N 0.6061(10) 0.1145(10) 0.4322(8) 0.062(5) Uani 0.50 1 d PD E 2 C211 C 0.5467(8) 0.1201(5) 0.4757(5) 0.054(3) Uani 0.50 1 d PD E 2 C212 C 0.4702(9) 0.1294(7) 0.5304(6) 0.068(4) Uani 0.50 1 d PD E 2 H21C H 0.4779 0.1010 0.5756 0.103 Uiso 0.50 1 calc PR E 2 H21D H 0.4222 0.1149 0.5190 0.103 Uiso 0.50 1 calc PR E 2 H21E H 0.4593 0.1784 0.5334 0.103 Uiso 0.50 1 calc PR E 2 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 Yb1 0.01605(7) 0.01515(7) 0.01740(7) -0.00408(5) -0.00251(5) -0.00028(5) Yb2 0.01799(7) 0.01293(7) 0.01806(7) -0.00374(5) -0.00133(5) 0.00013(5) Yb3 0.01661(7) 0.01279(7) 0.01861(7) -0.00475(5) -0.00399(5) 0.00065(5) Fe1 0.0162(2) 0.0133(2) 0.0172(2) -0.00386(17) -0.00356(18) 0.00020(17) Fe2 0.0171(2) 0.0130(2) 0.0184(2) -0.00375(18) -0.00386(18) -0.00029(17) Fe3 0.0164(2) 0.0178(2) 0.0250(2) -0.00921(19) -0.00093(19) -0.00213(18) Fe4 0.0162(2) 0.0165(2) 0.0224(2) -0.00757(19) -0.00136(19) -0.00153(18) Fe5 0.0176(2) 0.0133(2) 0.0184(2) -0.00408(18) -0.00247(18) 0.00010(17) O1 0.0199(12) 0.0172(11) 0.0174(11) -0.0072(9) -0.0020(9) -0.0011(9) N1 0.0196(14) 0.0143(13) 0.0145(13) -0.0039(10) -0.0038(11) 0.0005(11) C1 0.0203(17) 0.0160(16) 0.0209(16) -0.0044(13) -0.0032(13) -0.0021(13) C2 0.0241(17) 0.0126(15) 0.0158(15) -0.0005(12) -0.0058(13) -0.0023(13) O2 0.0205(11) 0.0152(11) 0.0159(11) -0.0052(9) -0.0056(9) -0.0005(9) C3 0.0181(16) 0.0151(15) 0.0148(15) -0.0025(12) -0.0026(12) 0.0001(12) C4 0.0183(16) 0.0198(16) 0.0201(16) -0.0081(13) -0.0040(13) 0.0025(13) O3 0.0149(11) 0.0196(11) 0.0206(11) -0.0081(9) -0.0010(9) -0.0015(9) C5 0.0187(16) 0.0140(15) 0.0215(16) -0.0031(13) -0.0069(13) 0.0012(12) C6 0.0208(16) 0.0166(16) 0.0169(15) -0.0038(12) -0.0062(13) 0.0016(13) O4 0.0201(11) 0.0138(11) 0.0161(11) -0.0021(9) -0.0037(9) -0.0006(9) N2 0.0278(17) 0.0298(17) 0.0235(16) 0.0025(13) 0.0042(13) 0.0081(13) C7 0.0313(19) 0.0202(17) 0.0203(17) -0.0017(14) -0.0043(15) 0.0001(14) C8 0.026(2) 0.043(2) 0.0247(19) 0.0099(17) -0.0042(16) 0.0008(17) O5 0.0184(11) 0.0173(11) 0.0159(11) -0.0005(9) -0.0021(9) -0.0014(9) C9A 0.051(4) 0.029(3) 0.018(3) -0.007(2) -0.002(3) -0.003(3) C10 0.093(4) 0.065(3) 0.0168(19) 0.000(2) -0.009(2) -0.055(3) O6 0.0214(12) 0.0219(12) 0.0174(11) -0.0039(9) -0.0033(9) -0.0026(9) C11A 0.021(3) 0.041(4) 0.025(3) 0.002(3) 0.004(2) -0.013(3) C12 0.070(3) 0.070(3) 0.034(2) 0.006(2) -0.010(2) -0.050(3) O7 0.0203(13) 0.0216(13) 0.0289(13) -0.0057(11) -0.0015(10) -0.0021(10) N3 0.0178(14) 0.0202(14) 0.0260(15) -0.0094(12) -0.0063(12) -0.0022(11) C13 0.0259(18) 0.0309(19) 0.0212(17) -0.0096(15) -0.0046(14) -0.0011(15) C14 0.0220(17) 0.0266(18) 0.0198(17) -0.0024(14) -0.0070(14) -0.0012(14) O8 0.0196(11) 0.0162(11) 0.0185(11) -0.0044(9) -0.0061(9) 0.0009(9) C15 0.0258(19) 0.031(2) 0.0309(19) -0.0105(16) -0.0135(16) 0.0049(15) C16 0.0286(19) 0.0222(18) 0.0310(19) -0.0092(15) -0.0150(16) 0.0053(15) O9 0.0185(11) 0.0194(11) 0.0208(11) -0.0075(9) -0.0065(9) 0.0027(9) C17 0.0256(19) 0.031(2) 0.0277(19) -0.0108(15) -0.0066(15) -0.0068(15) C18 0.041(2) 0.0228(18) 0.034(2) -0.0139(16) -0.0119(17) -0.0042(16) O10 0.0219(13) 0.0198(12) 0.0305(13) -0.0102(10) -0.0053(11) -0.0013(10) N4 0.0173(14) 0.0191(14) 0.0320(16) -0.0081(12) -0.0029(12) -0.0008(11) C19 0.0223(18) 0.0213(17) 0.0321(19) -0.0048(15) -0.0110(15) -0.0010(14) C20 0.0218(17) 0.0202(17) 0.0277(18) -0.0017(14) -0.0101(14) 0.0000(14) O11 0.0188(11) 0.0148(11) 0.0190(11) -0.0027(9) -0.0074(9) 0.0012(9) C21 0.0209(17) 0.0171(17) 0.035(2) -0.0053(15) -0.0044(15) -0.0025(13) C22 0.0164(16) 0.0210(17) 0.0318(19) -0.0077(15) -0.0031(14) -0.0016(13) O12 0.0169(11) 0.0184(11) 0.0241(12) -0.0057(9) -0.0046(9) 0.0014(9) C23 0.0181(17) 0.0209(18) 0.045(2) -0.0115(16) -0.0044(16) 0.0036(14) C24 0.0229(18) 0.0215(18) 0.039(2) -0.0090(16) 0.0037(16) -0.0001(14) O13 0.0238(13) 0.0159(12) 0.0277(13) -0.0053(10) 0.0024(10) -0.0013(10) N5 0.0358(17) 0.0154(14) 0.0180(14) -0.0043(11) -0.0026(13) 0.0012(12) C25 0.039(2) 0.0177(17) 0.0203(17) -0.0043(14) -0.0078(15) -0.0021(15) C26 0.0295(19) 0.0205(17) 0.0214(17) -0.0042(14) -0.0107(15) -0.0008(14) O14 0.0213(12) 0.0179(11) 0.0183(11) -0.0042(9) -0.0069(9) -0.0016(9) C27 0.043(2) 0.0212(18) 0.0207(18) -0.0050(14) -0.0084(16) 0.0062(16) C28 0.0240(18) 0.0280(18) 0.0182(16) -0.0072(14) -0.0087(14) 0.0032(14) O15 0.0217(12) 0.0162(11) 0.0179(11) -0.0050(9) -0.0043(9) 0.0002(9) C29 0.048(2) 0.0258(19) 0.0215(18) -0.0038(15) 0.0005(17) -0.0016(17) C30 0.049(2) 0.0250(19) 0.0214(18) -0.0007(15) 0.0050(17) -0.0069(17) O16 0.0291(14) 0.0187(12) 0.0255(13) -0.0056(10) 0.0013(11) -0.0028(10) N6 0.0203(14) 0.0163(14) 0.0228(14) -0.0048(11) -0.0044(12) 0.0017(11) C31 0.0233(18) 0.0242(18) 0.0247(18) -0.0031(14) -0.0085(14) 0.0029(14) C32 0.0212(18) 0.0305(19) 0.0250(18) -0.0035(15) -0.0081(14) -0.0049(15) O17 0.0224(12) 0.0178(11) 0.0195(11) -0.0025(9) -0.0046(9) -0.0022(9) C33 0.0256(18) 0.0135(15) 0.0225(17) -0.0019(13) -0.0051(14) 0.0008(13) C34 0.0203(17) 0.0185(16) 0.0204(17) -0.0022(13) -0.0028(13) 0.0022(13) O18 0.0210(12) 0.0137(11) 0.0184(11) -0.0013(9) -0.0049(9) 0.0022(9) C35 0.0295(19) 0.0148(16) 0.0270(18) -0.0052(14) -0.0043(15) 0.0029(14) C36 0.0271(19) 0.0155(16) 0.0323(19) -0.0081(14) -0.0048(15) 0.0020(14) O19 0.0240(13) 0.0187(12) 0.0255(13) -0.0074(10) -0.0096(10) 0.0022(10) N7 0.0207(15) 0.0214(15) 0.0320(16) -0.0122(13) 0.0038(12) -0.0051(12) C37 0.031(2) 0.0293(19) 0.0252(18) -0.0140(15) 0.0017(15) -0.0069(16) C38 0.0308(19) 0.0216(17) 0.0182(16) -0.0031(13) -0.0041(14) -0.0066(14) O20 0.0230(12) 0.0186(11) 0.0178(11) -0.0074(9) -0.0017(9) -0.0012(9) C39 0.0266(19) 0.031(2) 0.036(2) -0.0183(17) 0.0087(16) -0.0103(16) C40 0.031(2) 0.0282(19) 0.030(2) -0.0142(16) 0.0085(16) -0.0103(16) O21 0.0230(12) 0.0229(12) 0.0216(12) -0.0112(10) 0.0046(10) -0.0062(10) C41 0.029(2) 0.0204(18) 0.042(2) -0.0161(16) 0.0013(17) -0.0030(15) C42 0.043(3) 0.028(2) 0.059(3) -0.025(2) 0.002(2) 0.0021(18) O22A 0.044(4) 0.053(4) 0.104(6) -0.049(4) 0.030(4) -0.006(3) O22B 0.060(4) 0.033(3) 0.053(4) -0.019(3) 0.012(3) 0.000(3) O23 0.0193(12) 0.0164(11) 0.0218(12) -0.0045(9) -0.0069(9) 0.0008(9) O24 0.0198(12) 0.0156(11) 0.0280(12) -0.0007(10) -0.0079(10) -0.0005(9) C43 0.0244(18) 0.0136(15) 0.0207(16) -0.0066(13) -0.0058(14) 0.0018(13) C44 0.0290(19) 0.0157(16) 0.0310(19) -0.0028(14) -0.0133(15) 0.0008(14) C45 0.0277(19) 0.0208(17) 0.0222(17) 0.0003(14) -0.0057(14) -0.0011(14) C46 0.045(2) 0.0225(19) 0.031(2) 0.0013(16) -0.0094(18) 0.0006(17) C47 0.051(3) 0.027(2) 0.064(3) 0.003(2) -0.039(2) 0.0081(19) C48 0.054(3) 0.036(3) 0.121(5) 0.008(3) -0.057(3) -0.004(2) C49 0.045(3) 0.024(2) 0.091(4) 0.012(2) -0.040(3) -0.0103(19) O25 0.0223(13) 0.0187(12) 0.0366(14) -0.0064(10) -0.0076(11) -0.0016(10) O26 0.0173(12) 0.0206(12) 0.0374(14) -0.0108(11) -0.0050(10) 0.0011(9) C50 0.0119(16) 0.0284(19) 0.0318(19) -0.0101(15) 0.0005(14) -0.0014(14) C51 0.0149(16) 0.0242(18) 0.037(2) -0.0038(16) -0.0022(15) 0.0007(14) C52 0.027(2) 0.030(2) 0.044(2) -0.0097(18) -0.0021(17) 0.0029(16) C53 0.034(2) 0.036(2) 0.050(3) 0.000(2) -0.006(2) 0.0090(18) C54 0.028(2) 0.052(3) 0.052(3) 0.011(2) -0.010(2) 0.006(2) C55 0.039(3) 0.059(3) 0.063(3) 0.008(2) -0.029(2) -0.014(2) C56 0.028(2) 0.032(2) 0.055(3) 0.0012(19) -0.0160(19) -0.0072(17) O27 0.0196(12) 0.0182(12) 0.0255(12) -0.0079(10) -0.0034(10) -0.0012(9) O28 0.0184(12) 0.0174(11) 0.0260(12) -0.0052(9) -0.0047(10) 0.0001(9) C57 0.0235(18) 0.0159(16) 0.0224(17) -0.0013(13) -0.0034(14) -0.0032(13) C58 0.0206(17) 0.0155(16) 0.0327(19) -0.0058(14) -0.0074(14) 0.0008(13) C59 0.028(2) 0.045(2) 0.044(2) -0.028(2) 0.0002(18) -0.0038(18) C60 0.024(2) 0.082(4) 0.077(4) -0.050(3) 0.001(2) -0.009(2) C61 0.034(2) 0.075(4) 0.076(3) -0.051(3) -0.014(2) -0.010(2) C62 0.033(2) 0.040(2) 0.042(2) -0.0197(19) -0.0112(18) 0.0012(18) C63 0.0214(17) 0.0207(17) 0.0313(19) -0.0069(15) -0.0061(15) -0.0009(14) O29 0.0281(13) 0.0157(11) 0.0238(12) -0.0073(9) -0.0092(10) 0.0001(10) O30 0.0298(14) 0.0178(12) 0.0399(15) -0.0034(11) 0.0006(12) -0.0002(10) C64 0.0280(18) 0.0177(16) 0.0221(17) -0.0074(13) -0.0099(14) -0.0016(14) C65 0.0309(19) 0.0185(16) 0.0219(17) -0.0078(13) -0.0133(15) 0.0013(14) C66 0.038(2) 0.0209(17) 0.0214(18) -0.0090(14) -0.0051(16) 0.0009(15) C67 0.036(2) 0.028(2) 0.029(2) -0.0100(16) -0.0011(17) 0.0041(16) C68 0.043(2) 0.030(2) 0.039(2) -0.0149(18) -0.0132(19) 0.0139(18) C69 0.044(2) 0.0189(18) 0.041(2) -0.0059(16) -0.0165(19) 0.0026(16) C70 0.033(2) 0.0194(17) 0.0314(19) -0.0075(15) -0.0125(16) -0.0019(15) O31 0.0208(12) 0.0171(11) 0.0266(12) -0.0089(10) -0.0003(10) 0.0002(9) O32 0.0243(13) 0.0249(13) 0.0316(14) -0.0145(11) -0.0034(11) -0.0014(10) C71 0.0254(18) 0.0172(16) 0.0163(16) -0.0013(13) -0.0007(13) 0.0007(14) C72 0.0244(18) 0.0173(16) 0.0241(18) -0.0019(14) -0.0001(14) 0.0034(14) C73 0.027(2) 0.029(2) 0.068(3) -0.019(2) -0.013(2) 0.0066(16) C74 0.032(3) 0.046(3) 0.123(5) -0.031(3) -0.028(3) 0.007(2) C75 0.028(2) 0.036(2) 0.081(4) -0.017(2) -0.002(2) 0.0100(19) C76 0.042(2) 0.025(2) 0.038(2) -0.0056(17) 0.0040(19) 0.0129(18) C77 0.034(2) 0.0207(18) 0.0246(18) -0.0016(14) -0.0006(16) 0.0011(15) O33 0.0168(12) 0.0247(13) 0.0326(14) -0.0088(11) -0.0007(10) -0.0021(10) O34 0.0233(14) 0.0368(16) 0.087(2) -0.0370(16) -0.0159(15) 0.0052(12) C78 0.0221(18) 0.0227(18) 0.0223(17) -0.0021(14) -0.0014(14) -0.0011(14) C79 0.0253(19) 0.0286(19) 0.0233(18) -0.0036(15) 0.0003(15) 0.0053(15) C80 0.029(2) 0.050(3) 0.0258(19) -0.0151(18) -0.0089(16) 0.0082(18) C81 0.031(2) 0.071(3) 0.032(2) -0.017(2) -0.0101(18) 0.017(2) C82 0.048(3) 0.044(3) 0.067(3) 0.001(2) -0.002(3) 0.021(2) C83 0.045(3) 0.033(3) 0.105(5) -0.010(3) 0.014(3) 0.005(2) C84 0.028(2) 0.027(2) 0.069(3) -0.011(2) 0.006(2) 0.0009(17) O35 0.0253(13) 0.0188(12) 0.0207(12) -0.0016(9) -0.0015(10) -0.0030(10) O36 0.0245(13) 0.0208(13) 0.0371(15) -0.0062(11) 0.0041(11) -0.0019(10) C85 0.0247(18) 0.0228(17) 0.0160(16) -0.0025(13) -0.0007(14) -0.0032(14) C86 0.0273(18) 0.0187(16) 0.0172(16) -0.0009(13) -0.0057(14) -0.0030(14) C87 0.0238(18) 0.0266(18) 0.0237(18) -0.0047(15) -0.0039(14) -0.0002(14) C88 0.035(2) 0.0245(19) 0.031(2) -0.0095(16) -0.0092(16) 0.0044(16) C89 0.049(2) 0.0190(18) 0.038(2) -0.0054(16) -0.0154(19) -0.0032(17) C90 0.032(2) 0.030(2) 0.033(2) -0.0047(16) -0.0064(17) -0.0107(16) C91 0.0275(19) 0.0255(18) 0.0258(18) -0.0065(15) -0.0073(15) -0.0029(15) O37 0.0265(13) 0.0168(11) 0.0210(12) -0.0042(9) -0.0071(10) -0.0011(9) O38 0.0405(15) 0.0225(13) 0.0325(14) -0.0135(11) -0.0158(12) 0.0065(11) C92 0.0239(18) 0.0184(17) 0.0223(17) -0.0047(13) -0.0033(14) -0.0038(13) C93 0.0239(17) 0.0201(17) 0.0190(16) -0.0026(13) -0.0026(14) -0.0052(14) C94 0.036(2) 0.0240(18) 0.0251(18) -0.0098(15) -0.0120(16) 0.0016(15) C95 0.039(2) 0.032(2) 0.033(2) -0.0092(17) -0.0161(18) 0.0067(17) C96 0.043(2) 0.036(2) 0.030(2) -0.0028(17) -0.0187(18) -0.0041(18) C97 0.053(3) 0.034(2) 0.0264(19) -0.0099(17) -0.0154(18) -0.0102(19) C98 0.035(2) 0.0218(18) 0.0252(18) -0.0067(14) -0.0073(16) -0.0073(15) N111 0.033(2) 0.052(3) 0.114(4) -0.007(3) -0.020(3) -0.005(2) C111 0.038(3) 0.040(3) 0.105(5) 0.009(3) -0.040(3) -0.013(2) C112 0.102(5) 0.093(5) 0.071(4) 0.007(4) -0.043(4) -0.049(4) O44 0.110(6) 0.040(4) 0.049(4) -0.021(3) -0.051(4) 0.023(4) O45 0.060(7) 0.057(6) 0.095(10) -0.031(7) 0.014(6) -0.033(6) O46 0.057(4) 0.047(4) 0.040(3) -0.008(3) -0.030(3) 0.014(3) S2 0.0471(12) 0.0291(10) 0.0278(10) -0.0047(8) -0.0143(9) -0.0034(9) C100 0.039(5) 0.036(5) 0.050(6) -0.010(5) -0.018(4) -0.002(4) F4 0.082(4) 0.050(3) 0.066(4) -0.024(3) -0.048(3) 0.030(3) F5 0.083(5) 0.093(6) 0.041(4) -0.027(4) -0.018(3) 0.040(4) F6 0.052(4) 0.059(4) 0.186(9) -0.014(5) 0.019(5) -0.015(3) N211 0.099(13) 0.046(6) 0.056(7) -0.003(5) -0.043(8) -0.027(8) C211 0.095(9) 0.037(5) 0.039(6) -0.005(4) -0.030(6) -0.011(6) C212 0.115(12) 0.047(7) 0.048(7) -0.003(6) -0.030(8) -0.016(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 Yb1 O8 2.240(2) . ? Yb1 O6 2.267(2) . ? Yb1 O5 2.268(2) . ? Yb1 O9 2.284(2) . ? Yb1 O7 2.327(2) . ? Yb1 O10 2.349(2) . ? Yb1 N2 2.522(3) . ? Yb1 N3 2.532(3) . ? Yb1 Fe1 3.3851(5) . ? Yb1 Fe3 3.4191(5) . ? Yb2 O15 2.222(2) . ? Yb2 O12 2.274(2) . ? Yb2 O14 2.297(2) . ? Yb2 O11 2.304(2) . ? Yb2 O16 2.361(2) . ? Yb2 O13 2.374(2) . ? Yb2 N5 2.541(3) . ? Yb2 N4 2.555(3) . ? Yb2 Fe5 3.4390(5) . ? Yb2 Fe2 3.4490(5) . ? Yb3 O4 2.225(2) . ? Yb3 O17 2.258(2) . ? Yb3 O28 2.305(2) . ? Yb3 O37 2.320(2) . ? Yb3 O19 2.328(2) . ? Yb3 O18 2.343(2) . ? Yb3 N6 2.584(3) . ? Yb3 O20 2.596(2) . ? Yb3 Fe5 3.3996(5) . ? Yb3 Fe4 3.5744(5) . ? Fe1 O8 1.963(2) . ? Fe1 O1 1.969(2) . ? Fe1 O5 1.976(2) . ? Fe1 O29 2.014(2) . ? Fe1 O2 2.055(2) . ? Fe1 O23 2.090(2) . ? Fe2 O14 1.965(2) . ? Fe2 O1 1.969(2) . ? Fe2 O11 1.988(2) . ? Fe2 O2 2.024(2) . ? Fe2 O24 2.056(2) . ? Fe2 O31 2.109(2) . ? Fe3 O9 1.950(2) . ? Fe3 O6 1.969(2) . ? Fe3 O21 1.997(2) . ? Fe3 O33 2.002(2) . ? Fe3 O3 2.062(2) . ? Fe3 O25 2.091(2) . ? Fe4 O17 1.974(2) . ? Fe4 O20 1.975(2) . ? Fe4 O3 1.999(2) . ? Fe4 O26 2.032(2) . ? Fe4 O21 2.038(2) . ? Fe4 N7 2.259(3) . ? Fe5 O18 1.965(2) . ? Fe5 O15 1.991(2) . ? Fe5 O12 1.998(2) . ? Fe5 O4 2.019(2) . ? Fe5 O35 2.051(2) . ? Fe5 O27 2.056(2) . ? O1 H1 0.76(3) . ? N1 C5 1.509(4) . ? N1 C3 1.510(4) . ? N1 C1 1.510(4) . ? N1 H11 0.98(3) . ? C1 C2 1.532(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.421(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.532(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.411(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.406(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N2 C9A 1.381(6) . ? N2 C11B 1.383(10) . ? N2 C7 1.469(4) . ? N2 C11A 1.609(7) . ? N2 C9B 1.726(9) . ? C7 C8 1.521(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O5 1.421(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9A C10 1.526(7) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C9B C10 1.250(9) . ? C9B H9B1 0.9900 . ? C9B H9B2 0.9900 . ? C10 O6 1.421(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 H10C 0.9900 . ? C10 H10D 0.9900 . ? C11A C12 1.325(8) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C11B C12 1.583(10) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12 O7 1.426(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? O7 H7 0.74(3) . ? N3 C15 1.480(4) . ? N3 C13 1.486(4) . ? N3 C17 1.487(4) . ? C13 C14 1.517(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O8 1.420(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.529(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O9 1.430(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.500(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O10 1.438(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O10 H10 0.82(3) . ? N4 C21 1.476(4) . ? N4 C19 1.489(4) . ? N4 C23 1.497(4) . ? C19 C20 1.497(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O11 1.424(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.532(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O12 1.428(4) . ? C22 H22C 0.9900 . ? C22 H22D 0.9900 . ? C23 C24 1.515(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O13 1.439(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O13 H13 0.80(3) . ? N5 C29 1.479(5) . ? N5 C25 1.491(4) . ? N5 C27 1.496(4) . ? C25 C26 1.502(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O14 1.427(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.524(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O15 1.423(4) . ? C28 H28A 1.0000 . ? C29 C30 1.509(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O16 1.433(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O16 H16 0.80(3) . ? N6 C33 1.479(4) . ? N6 C35 1.484(4) . ? N6 C31 1.490(4) . ? C31 C32 1.527(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O17 1.431(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.516(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O18 1.416(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.509(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O19 1.430(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O19 H19 0.81(3) . ? N7 C39 1.490(4) . ? N7 C41 1.491(4) . ? N7 C37 1.496(5) . ? C37 C38 1.521(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O20 1.436(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.512(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O21 1.422(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.537(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O22B 1.454(7) . ? C42 O22A 1.473(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 H42C 0.9897 . ? C42 H42D 0.9901 . ? O22A H22A 0.8400 . ? O22B H22B 0.8400 . ? O23 C43 1.263(4) . ? O24 C43 1.266(4) . ? C43 C44 1.503(4) . ? C44 C49 1.381(5) . ? C44 C45 1.387(5) . ? C45 C46 1.385(5) . ? C45 H45A 0.9500 . ? C46 C47 1.376(6) . ? C46 H46A 0.9500 . ? C47 C48 1.369(6) . ? C47 H47A 0.9500 . ? C48 C49 1.397(6) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? O25 C50 1.266(4) . ? O26 C50 1.270(4) . ? C50 C51 1.489(5) . ? C51 C56 1.389(5) . ? C51 C52 1.398(5) . ? C52 C53 1.377(6) . ? C52 H52A 0.9500 . ? C53 C54 1.392(7) . ? C53 H53A 0.9500 . ? C54 C55 1.371(7) . ? C54 H54A 0.9500 . ? C55 C56 1.387(6) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? O27 C57 1.269(4) . ? O28 C57 1.268(4) . ? C57 C58 1.499(5) . ? C58 C59 1.395(5) . ? C58 C63 1.403(5) . ? C59 C60 1.377(6) . ? C59 H59A 0.9500 . ? C60 C61 1.406(6) . ? C60 H60A 0.9500 . ? C61 C62 1.367(6) . ? C61 H61A 0.9500 . ? C62 C63 1.383(5) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? O29 C64 1.278(4) . ? O30 C64 1.242(4) . ? C64 C65 1.501(5) . ? C65 C70 1.391(5) . ? C65 C66 1.394(5) . ? C66 C67 1.390(5) . ? C66 H66A 0.9500 . ? C67 C68 1.388(5) . ? C67 H67A 0.9500 . ? C68 C69 1.382(6) . ? C68 H68A 0.9500 . ? C69 C70 1.395(5) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? O31 C71 1.299(4) . ? O32 C71 1.236(4) . ? C71 C72 1.509(5) . ? C72 C73 1.373(5) . ? C72 C77 1.400(5) . ? C73 C74 1.407(6) . ? C73 H73A 0.9500 . ? C74 C75 1.395(7) . ? C74 H74A 0.9500 . ? C75 C76 1.367(7) . ? C75 H75A 0.9500 . ? C76 C77 1.395(5) . ? C76 H76A 0.9500 . ? C77 H77A 0.9500 . ? O33 C78 1.277(4) . ? O34 C78 1.231(4) . ? C78 C79 1.510(5) . ? C79 C80 1.377(5) . ? C79 C84 1.394(6) . ? C80 C81 1.406(6) . ? C80 H80A 0.9500 . ? C81 C82 1.384(7) . ? C81 H81A 0.9500 . ? C82 C83 1.368(7) . ? C82 H82A 0.9500 . ? C83 C84 1.400(6) . ? C83 H83A 0.9500 . ? C84 H84A 0.9500 . ? O35 C85 1.283(4) . ? O36 C85 1.250(4) . ? C85 C86 1.508(5) . ? C86 C87 1.382(5) . ? C86 C91 1.392(5) . ? C87 C88 1.384(5) . ? C87 H87A 0.9500 . ? C88 C89 1.398(5) . ? C88 H88A 0.9500 . ? C89 C90 1.373(5) . ? C89 H89A 0.9500 . ? C90 C91 1.403(5) . ? C90 H90A 0.9500 . ? C91 H91A 0.9500 . ? O37 C92 1.261(4) . ? O38 C92 1.268(4) . ? C92 C93 1.501(5) . ? C93 C94 1.392(5) . ? C93 C98 1.396(5) . ? C94 C95 1.389(5) . ? C94 H94A 0.9500 . ? C95 C96 1.381(5) . ? C95 H95A 0.9500 . ? C96 C97 1.389(6) . ? C96 H96A 0.9500 . ? C97 C98 1.388(5) . ? C97 H97A 0.9500 . ? C98 H98A 0.9500 . ? N111 C111 1.165(7) . ? C111 C112 1.473(9) . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? O44 S2 1.424(6) . ? O45 S2 1.430(13) . ? O46 S2 1.424(6) . ? S2 C100 1.813(10) . ? C100 F6 1.291(11) . ? C100 F5 1.315(12) . ? C100 F4 1.341(10) . ? N211 C211 1.141(15) . ? C211 C212 1.462(14) . ? C212 H21C 0.9800 . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? 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 O8 Yb1 O6 107.36(8) . . ? O8 Yb1 O5 67.55(7) . . ? O6 Yb1 O5 88.61(8) . . ? O8 Yb1 O9 85.70(8) . . ? O6 Yb1 O9 66.14(8) . . ? O5 Yb1 O9 136.06(8) . . ? O8 Yb1 O7 152.26(8) . . ? O6 Yb1 O7 91.04(8) . . ? O5 Yb1 O7 135.15(8) . . ? O9 Yb1 O7 83.01(8) . . ? O8 Yb1 O10 92.31(8) . . ? O6 Yb1 O10 152.29(8) . . ? O5 Yb1 O10 80.96(8) . . ? O9 Yb1 O10 136.47(8) . . ? O7 Yb1 O10 78.92(8) . . ? O8 Yb1 N2 136.40(9) . . ? O6 Yb1 N2 70.95(9) . . ? O5 Yb1 N2 68.86(9) . . ? O9 Yb1 N2 127.48(9) . . ? O7 Yb1 N2 68.75(9) . . ? O10 Yb1 N2 81.34(10) . . ? O8 Yb1 N3 71.07(8) . . ? O6 Yb1 N3 135.79(8) . . ? O5 Yb1 N3 126.71(8) . . ? O9 Yb1 N3 69.72(8) . . ? O7 Yb1 N3 81.25(9) . . ? O10 Yb1 N3 68.59(9) . . ? N2 Yb1 N3 141.03(10) . . ? O15 Yb2 O12 66.73(8) . . ? O15 Yb2 O14 85.89(8) . . ? O12 Yb2 O14 138.37(8) . . ? O15 Yb2 O11 116.16(8) . . ? O12 Yb2 O11 98.50(8) . . ? O14 Yb2 O11 65.14(7) . . ? O15 Yb2 O16 90.23(8) . . ? O12 Yb2 O16 78.35(8) . . ? O14 Yb2 O16 134.83(8) . . ? O11 Yb2 O16 150.07(8) . . ? O15 Yb2 O13 152.45(8) . . ? O12 Yb2 O13 132.53(8) . . ? O14 Yb2 O13 85.51(8) . . ? O11 Yb2 O13 83.44(8) . . ? O16 Yb2 O13 77.61(8) . . ? O15 Yb2 N5 70.94(8) . . ? O12 Yb2 N5 124.85(8) . . ? O14 Yb2 N5 68.23(8) . . ? O11 Yb2 N5 131.82(8) . . ? O16 Yb2 N5 68.02(9) . . ? O13 Yb2 N5 81.56(9) . . ? O15 Yb2 N4 134.00(8) . . ? O12 Yb2 N4 67.34(8) . . ? O14 Yb2 N4 129.32(8) . . ? O11 Yb2 N4 68.59(8) . . ? O16 Yb2 N4 83.08(9) . . ? O13 Yb2 N4 69.60(9) . . ? N5 Yb2 N4 142.96(9) . . ? O4 Yb3 O17 106.34(8) . . ? O4 Yb3 O28 85.32(8) . . ? O17 Yb3 O28 154.61(8) . . ? O4 Yb3 O37 84.87(8) . . ? O17 Yb3 O37 128.59(8) . . ? O28 Yb3 O37 73.90(8) . . ? O4 Yb3 O19 157.22(8) . . ? O17 Yb3 O19 91.28(8) . . ? O28 Yb3 O19 84.50(8) . . ? O37 Yb3 O19 72.74(8) . . ? O4 Yb3 O18 65.33(7) . . ? O17 Yb3 O18 85.49(8) . . ? O28 Yb3 O18 78.96(8) . . ? O37 Yb3 O18 141.04(8) . . ? O19 Yb3 O18 131.94(8) . . ? O4 Yb3 N6 132.54(8) . . ? O17 Yb3 N6 71.70(8) . . ? O28 Yb3 N6 83.75(8) . . ? O37 Yb3 N6 134.77(8) . . ? O19 Yb3 N6 66.28(8) . . ? O18 Yb3 N6 67.26(8) . . ? O4 Yb3 O20 79.08(7) . . ? O17 Yb3 O20 62.44(7) . . ? O28 Yb3 O20 142.91(7) . . ? O37 Yb3 O20 71.37(7) . . ? O19 Yb3 O20 97.18(7) . . ? O18 Yb3 O20 122.59(7) . . ? N6 Yb3 O20 130.89(8) . . ? O8 Fe1 O1 97.23(9) . . ? O8 Fe1 O5 79.02(9) . . ? O1 Fe1 O5 172.73(9) . . ? O8 Fe1 O29 95.71(9) . . ? O1 Fe1 O29 90.74(9) . . ? O5 Fe1 O29 95.80(9) . . ? O8 Fe1 O2 94.86(9) . . ? O1 Fe1 O2 76.18(9) . . ? O5 Fe1 O2 97.83(9) . . ? O29 Fe1 O2 164.12(9) . . ? O8 Fe1 O23 167.98(9) . . ? O1 Fe1 O23 94.77(9) . . ? O5 Fe1 O23 88.98(9) . . ? O29 Fe1 O23 84.83(9) . . ? O2 Fe1 O23 87.29(8) . . ? O14 Fe2 O1 97.64(9) . . ? O14 Fe2 O11 77.58(9) . . ? O1 Fe2 O11 174.10(9) . . ? O14 Fe2 O2 100.92(9) . . ? O1 Fe2 O2 76.89(9) . . ? O11 Fe2 O2 100.46(9) . . ? O14 Fe2 O24 165.73(9) . . ? O1 Fe2 O24 95.10(9) . . ? O11 Fe2 O24 90.06(9) . . ? O2 Fe2 O24 88.21(9) . . ? O14 Fe2 O31 91.41(9) . . ? O1 Fe2 O31 91.82(9) . . ? O11 Fe2 O31 91.76(9) . . ? O2 Fe2 O31 164.20(9) . . ? O24 Fe2 O31 81.75(9) . . ? O9 Fe3 O6 78.63(9) . . ? O9 Fe3 O21 171.20(9) . . ? O6 Fe3 O21 96.79(10) . . ? O9 Fe3 O33 97.86(10) . . ? O6 Fe3 O33 94.89(9) . . ? O21 Fe3 O33 89.98(9) . . ? O9 Fe3 O3 100.43(9) . . ? O6 Fe3 O3 98.19(9) . . ? O21 Fe3 O3 72.60(9) . . ? O33 Fe3 O3 159.28(9) . . ? O9 Fe3 O25 87.35(9) . . ? O6 Fe3 O25 165.94(9) . . ? O21 Fe3 O25 97.25(10) . . ? O33 Fe3 O25 85.88(10) . . ? O3 Fe3 O25 85.31(9) . . ? O17 Fe4 O20 79.81(9) . . ? O17 Fe4 O3 105.78(9) . . ? O20 Fe4 O3 100.61(9) . . ? O17 Fe4 O26 87.41(9) . . ? O20 Fe4 O26 160.59(9) . . ? O3 Fe4 O26 96.88(9) . . ? O17 Fe4 O21 177.52(10) . . ? O20 Fe4 O21 102.52(9) . . ? O3 Fe4 O21 73.06(9) . . ? O26 Fe4 O21 90.56(10) . . ? O17 Fe4 N7 104.44(10) . . ? O20 Fe4 N7 81.15(10) . . ? O3 Fe4 N7 149.56(10) . . ? O26 Fe4 N7 88.05(10) . . ? O21 Fe4 N7 76.89(9) . . ? O18 Fe5 O15 94.96(9) . . ? O18 Fe5 O12 168.88(9) . . ? O15 Fe5 O12 76.62(9) . . ? O18 Fe5 O4 76.53(9) . . ? O15 Fe5 O4 98.91(9) . . ? O12 Fe5 O4 97.38(9) . . ? O18 Fe5 O35 92.34(9) . . ? O15 Fe5 O35 94.51(9) . . ? O12 Fe5 O35 95.52(9) . . ? O4 Fe5 O35 163.19(9) . . ? O18 Fe5 O27 98.47(9) . . ? O15 Fe5 O27 166.33(9) . . ? O12 Fe5 O27 90.36(9) . . ? O4 Fe5 O27 86.72(9) . . ? O35 Fe5 O27 82.46(9) . . ? Fe2 O1 Fe1 102.11(10) . . ? Fe2 O1 H1 109(3) . . ? Fe1 O1 H1 137(3) . . ? C5 N1 C3 111.4(2) . . ? C5 N1 C1 110.5(2) . . ? C3 N1 C1 115.0(2) . . ? C5 N1 H11 106(2) . . ? C3 N1 H11 105(2) . . ? C1 N1 H11 108(2) . . ? N1 C1 C2 114.2(3) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? O2 C2 C1 112.6(3) . . ? O2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? O2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C2 O2 Fe2 122.52(18) . . ? C2 O2 Fe1 118.59(18) . . ? Fe2 O2 Fe1 97.30(9) . . ? N1 C3 C4 114.5(2) . . ? N1 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? O3 C4 C3 114.0(3) . . ? O3 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? O3 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 O3 Fe4 137.68(19) . . ? C4 O3 Fe3 121.71(18) . . ? Fe4 O3 Fe3 100.62(9) . . ? N1 C5 C6 113.7(3) . . ? N1 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N1 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? O4 C6 C5 112.4(3) . . ? O4 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? O4 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 O4 Fe5 125.63(19) . . ? C6 O4 Yb3 123.78(18) . . ? Fe5 O4 Yb3 106.36(9) . . ? C9A N2 C7 120.8(4) . . ? C11B N2 C7 123.0(5) . . ? C9A N2 C11A 109.9(4) . . ? C7 N2 C11A 102.1(3) . . ? C11B N2 C9B 104.1(6) . . ? C7 N2 C9B 98.3(4) . . ? C9A N2 Yb1 111.0(3) . . ? C11B N2 Yb1 116.8(4) . . ? C7 N2 Yb1 107.6(2) . . ? C11A N2 Yb1 104.0(3) . . ? C9B N2 Yb1 103.2(3) . . ? N2 C7 C8 111.0(3) . . ? N2 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? O5 C8 C7 110.1(3) . . ? O5 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O5 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? C8 O5 Fe1 128.9(2) . . ? C8 O5 Yb1 124.18(19) . . ? Fe1 O5 Yb1 105.58(9) . . ? N2 C9A C10 116.8(5) . . ? N2 C9A H9A1 108.1 . . ? C10 C9A H9A1 108.1 . . ? N2 C9A H9A2 108.1 . . ? C10 C9A H9A2 108.1 . . ? H9A1 C9A H9A2 107.3 . . ? C10 C9B N2 111.7(6) . . ? C10 C9B H9B1 109.3 . . ? N2 C9B H9B1 109.3 . . ? C10 C9B H9B2 109.3 . . ? N2 C9B H9B2 109.3 . . ? H9B1 C9B H9B2 107.9 . . ? C9B C10 O6 121.0(5) . . ? O6 C10 C9A 112.4(4) . . ? O6 C10 H10A 109.1 . . ? C9A C10 H10A 109.1 . . ? O6 C10 H10B 109.1 . . ? C9A C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C9B C10 H10C 107.1 . . ? O6 C10 H10C 107.1 . . ? C9B C10 H10D 107.1 . . ? O6 C10 H10D 107.1 . . ? H10C C10 H10D 106.8 . . ? C10 O6 Fe3 124.9(3) . . ? C10 O6 Yb1 120.9(2) . . ? Fe3 O6 Yb1 107.41(10) . . ? C12 C11A N2 113.0(5) . . ? C12 C11A H11A 109.0 . . ? N2 C11A H11A 109.0 . . ? C12 C11A H11B 109.0 . . ? N2 C11A H11B 109.0 . . ? H11A C11A H11B 107.8 . . ? N2 C11B C12 111.3(6) . . ? N2 C11B H11C 109.4 . . ? C12 C11B H11C 109.4 . . ? N2 C11B H11D 109.4 . . ? C12 C11B H11D 109.4 . . ? H11C C11B H11D 108.0 . . ? C11A C12 O7 117.1(4) . . ? O7 C12 C11B 111.6(4) . . ? C11A C12 H12A 108.0 . . ? O7 C12 H12A 108.0 . . ? C11A C12 H12B 108.0 . . ? O7 C12 H12B 108.0 . . ? H12A C12 H12B 107.3 . . ? O7 C12 H12C 109.3 . . ? C11B C12 H12C 109.3 . . ? O7 C12 H12D 109.3 . . ? C11B C12 H12D 109.3 . . ? H12C C12 H12D 108.0 . . ? C12 O7 Yb1 120.0(3) . . ? C12 O7 H7 115(3) . . ? Yb1 O7 H7 118(3) . . ? C15 N3 C13 112.9(3) . . ? C15 N3 C17 109.3(3) . . ? C13 N3 C17 110.2(3) . . ? C15 N3 Yb1 107.89(19) . . ? C13 N3 Yb1 108.48(19) . . ? C17 N3 Yb1 108.0(2) . . ? N3 C13 C14 113.6(3) . . ? N3 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N3 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? O8 C14 C13 109.2(3) . . ? O8 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? O8 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C14 O8 Fe1 127.71(19) . . ? C14 O8 Yb1 120.84(18) . . ? Fe1 O8 Yb1 107.12(9) . . ? N3 C15 C16 111.6(3) . . ? N3 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N3 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? O9 C16 C15 109.6(3) . . ? O9 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? O9 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C16 O9 Fe3 128.86(19) . . ? C16 O9 Yb1 123.30(18) . . ? Fe3 O9 Yb1 107.46(9) . . ? N3 C17 C18 111.6(3) . . ? N3 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N3 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? O10 C18 C17 109.7(3) . . ? O10 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O10 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C18 O10 Yb1 122.1(2) . . ? C18 O10 H10 104(3) . . ? Yb1 O10 H10 115(3) . . ? C21 N4 C19 109.8(3) . . ? C21 N4 C23 112.3(3) . . ? C19 N4 C23 110.4(3) . . ? C21 N4 Yb2 106.1(2) . . ? C19 N4 Yb2 105.91(19) . . ? C23 N4 Yb2 112.0(2) . . ? N4 C19 C20 111.0(3) . . ? N4 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N4 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? O11 C20 C19 109.7(3) . . ? O11 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? O11 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 O11 Fe2 122.41(19) . . ? C20 O11 Yb2 123.29(18) . . ? Fe2 O11 Yb2 106.73(9) . . ? N4 C21 C22 110.5(3) . . ? N4 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N4 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? O12 C22 C21 109.9(3) . . ? O12 C22 H22C 109.7 . . ? C21 C22 H22C 109.7 . . ? O12 C22 H22D 109.7 . . ? C21 C22 H22D 109.7 . . ? H22C C22 H22D 108.2 . . ? C22 O12 Fe5 125.09(19) . . ? C22 O12 Yb2 125.12(18) . . ? Fe5 O12 Yb2 107.06(10) . . ? N4 C23 C24 111.5(3) . . ? N4 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? N4 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? O13 C24 C23 111.2(3) . . ? O13 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? O13 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 O13 Yb2 113.87(19) . . ? C24 O13 H13 113(3) . . ? Yb2 O13 H13 110(3) . . ? C29 N5 C25 109.3(3) . . ? C29 N5 C27 110.8(3) . . ? C25 N5 C27 111.7(3) . . ? C29 N5 Yb2 108.3(2) . . ? C25 N5 Yb2 107.23(19) . . ? C27 N5 Yb2 109.34(19) . . ? N5 C25 C26 110.7(3) . . ? N5 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? O14 C26 C25 108.8(3) . . ? O14 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O14 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C26 O14 Fe2 121.91(19) . . ? C26 O14 Yb2 124.34(19) . . ? Fe2 O14 Yb2 107.77(9) . . ? N5 C27 C28 112.3(3) . . ? N5 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? N5 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? O15 C28 C27 109.8(3) . . ? O15 C28 Yb2 37.41(13) . . ? C27 C28 Yb2 82.88(19) . . ? O15 C28 H28A 120.8 . . ? C27 C28 H28A 120.8 . . ? Yb2 C28 H28A 120.8 . . ? C28 O15 Fe5 128.77(19) . . ? C28 O15 Yb2 119.68(18) . . ? Fe5 O15 Yb2 109.33(10) . . ? N5 C29 C30 111.6(3) . . ? N5 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N5 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? O16 C30 C29 108.0(3) . . ? O16 C30 H30A 110.1 . . ? C29 C30 H30A 110.1 . . ? O16 C30 H30B 110.1 . . ? C29 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C30 O16 Yb2 122.8(2) . . ? C30 O16 H16 118(3) . . ? Yb2 O16 H16 112(3) . . ? C33 N6 C35 108.4(2) . . ? C33 N6 C31 112.5(3) . . ? C35 N6 C31 111.0(3) . . ? C33 N6 Yb3 108.31(18) . . ? C35 N6 Yb3 110.04(19) . . ? C31 N6 Yb3 106.56(19) . . ? N6 C31 C32 112.9(3) . . ? N6 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? N6 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? O17 C32 C31 109.1(3) . . ? O17 C32 H32A 109.9 . . ? C31 C32 H32A 109.9 . . ? O17 C32 H32B 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C32 O17 Fe4 128.6(2) . . ? C32 O17 Yb3 116.31(18) . . ? Fe4 O17 Yb3 115.10(10) . . ? N6 C33 C34 111.4(3) . . ? N6 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? N6 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? O18 C34 C33 109.4(3) . . ? O18 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O18 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C34 O18 Fe5 126.12(19) . . ? C34 O18 Yb3 124.75(18) . . ? Fe5 O18 Yb3 103.86(9) . . ? N6 C35 C36 111.1(3) . . ? N6 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? N6 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? O19 C36 C35 108.7(3) . . ? O19 C36 H36A 109.9 . . ? C35 C36 H36A 109.9 . . ? O19 C36 H36B 109.9 . . ? C35 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? C36 O19 Yb3 126.8(2) . . ? C36 O19 H19 115(3) . . ? Yb3 O19 H19 107(3) . . ? C39 N7 C41 109.7(3) . . ? C39 N7 C37 113.1(3) . . ? C41 N7 C37 111.8(3) . . ? C39 N7 Fe4 106.0(2) . . ? C41 N7 Fe4 111.0(2) . . ? C37 N7 Fe4 104.98(19) . . ? N7 C37 C38 111.3(3) . . ? N7 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? N7 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? O20 C38 C37 109.3(3) . . ? O20 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? O20 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.3 . . ? C38 O20 Fe4 108.60(19) . . ? C38 O20 Yb3 126.68(18) . . ? Fe4 O20 Yb3 102.02(9) . . ? N7 C39 C40 110.4(3) . . ? N7 C39 H39A 109.6 . . ? C40 C39 H39A 109.6 . . ? N7 C39 H39B 109.6 . . ? C40 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? O21 C40 C39 108.7(3) . . ? O21 C40 H40A 110.0 . . ? C39 C40 H40A 110.0 . . ? O21 C40 H40B 110.0 . . ? C39 C40 H40B 110.0 . . ? H40A C40 H40B 108.3 . . ? C40 O21 Fe3 131.6(2) . . ? C40 O21 Fe4 121.07(19) . . ? Fe3 O21 Fe4 101.50(10) . . ? N7 C41 C42 114.5(3) . . ? N7 C41 H41A 108.6 . . ? C42 C41 H41A 108.6 . . ? N7 C41 H41B 108.6 . . ? C42 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? O22B C42 C41 105.6(4) . . ? O22A C42 C41 110.1(4) . . ? O22A C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? O22A C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.2 . . ? O22B C42 H42C 111.1 . . ? C41 C42 H42C 110.8 . . ? O22B C42 H42D 110.2 . . ? C41 C42 H42D 110.2 . . ? H42C C42 H42D 108.8 . . ? C42 O22A H22A 109.5 . . ? C42 O22B H22B 109.5 . . ? C43 O23 Fe1 127.9(2) . . ? C43 O24 Fe2 128.7(2) . . ? O23 C43 O24 125.7(3) . . ? O23 C43 C44 117.8(3) . . ? O24 C43 C44 116.5(3) . . ? C49 C44 C45 119.0(3) . . ? C49 C44 C43 119.5(3) . . ? C45 C44 C43 121.5(3) . . ? C46 C45 C44 120.5(3) . . ? C46 C45 H45A 119.8 . . ? C44 C45 H45A 119.8 . . ? C47 C46 C45 120.0(4) . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C48 C47 C46 120.3(4) . . ? C48 C47 H47A 119.8 . . ? C46 C47 H47A 119.8 . . ? C47 C48 C49 119.8(4) . . ? C47 C48 H48A 120.1 . . ? C49 C48 H48A 120.1 . . ? C44 C49 C48 120.3(4) . . ? C44 C49 H49A 119.8 . . ? C48 C49 H49A 119.8 . . ? C50 O25 Fe3 129.4(2) . . ? C50 O26 Fe4 126.5(2) . . ? O25 C50 O26 124.3(3) . . ? O25 C50 C51 118.3(3) . . ? O26 C50 C51 117.3(3) . . ? C56 C51 C52 118.8(4) . . ? C56 C51 C50 121.0(3) . . ? C52 C51 C50 120.1(3) . . ? C53 C52 C51 120.9(4) . . ? C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C52 C53 C54 119.5(4) . . ? C52 C53 H53A 120.3 . . ? C54 C53 H53A 120.3 . . ? C55 C54 C53 120.3(4) . . ? C55 C54 H54A 119.9 . . ? C53 C54 H54A 119.9 . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55A 119.9 . . ? C56 C55 H55A 119.9 . . ? C55 C56 C51 120.3(4) . . ? C55 C56 H56A 119.8 . . ? C51 C56 H56A 119.8 . . ? C57 O27 Fe5 129.6(2) . . ? C57 O28 Yb3 129.0(2) . . ? O28 C57 O27 125.4(3) . . ? O28 C57 C58 118.3(3) . . ? O27 C57 C58 116.3(3) . . ? C59 C58 C63 118.9(3) . . ? C59 C58 C57 121.1(3) . . ? C63 C58 C57 119.9(3) . . ? C60 C59 C58 120.4(4) . . ? C60 C59 H59A 119.8 . . ? C58 C59 H59A 119.8 . . ? C59 C60 C61 120.2(4) . . ? C59 C60 H60A 119.9 . . ? C61 C60 H60A 119.9 . . ? C62 C61 C60 119.3(4) . . ? C62 C61 H61A 120.3 . . ? C60 C61 H61A 120.3 . . ? C61 C62 C63 121.2(4) . . ? C61 C62 H62A 119.4 . . ? C63 C62 H62A 119.4 . . ? C62 C63 C58 119.9(3) . . ? C62 C63 H63A 120.0 . . ? C58 C63 H63A 120.0 . . ? C64 O29 Fe1 129.2(2) . . ? O30 C64 O29 124.3(3) . . ? O30 C64 C65 118.4(3) . . ? O29 C64 C65 117.3(3) . . ? C70 C65 C66 119.3(3) . . ? C70 C65 C64 119.4(3) . . ? C66 C65 C64 121.2(3) . . ? C67 C66 C65 120.3(3) . . ? C67 C66 H66A 119.8 . . ? C65 C66 H66A 119.8 . . ? C68 C67 C66 119.8(4) . . ? C68 C67 H67A 120.1 . . ? C66 C67 H67A 120.1 . . ? C69 C68 C67 120.4(4) . . ? C69 C68 H68A 119.8 . . ? C67 C68 H68A 119.8 . . ? C68 C69 C70 119.8(4) . . ? C68 C69 H69A 120.1 . . ? C70 C69 H69A 120.1 . . ? C65 C70 C69 120.3(4) . . ? C65 C70 H70A 119.8 . . ? C69 C70 H70A 119.8 . . ? C71 O31 Fe2 125.0(2) . . ? O32 C71 O31 125.3(3) . . ? O32 C71 C72 118.6(3) . . ? O31 C71 C72 116.1(3) . . ? C73 C72 C77 119.7(3) . . ? C73 C72 C71 121.4(3) . . ? C77 C72 C71 118.9(3) . . ? C72 C73 C74 120.3(4) . . ? C72 C73 H73A 119.9 . . ? C74 C73 H73A 119.9 . . ? C75 C74 C73 119.4(4) . . ? C75 C74 H74A 120.3 . . ? C73 C74 H74A 120.3 . . ? C76 C75 C74 120.4(4) . . ? C76 C75 H75A 119.8 . . ? C74 C75 H75A 119.8 . . ? C75 C76 C77 120.3(4) . . ? C75 C76 H76A 119.9 . . ? C77 C76 H76A 119.9 . . ? C76 C77 C72 120.0(4) . . ? C76 C77 H77A 120.0 . . ? C72 C77 H77A 120.0 . . ? C78 O33 Fe3 134.6(2) . . ? O34 C78 O33 124.1(3) . . ? O34 C78 C79 118.4(3) . . ? O33 C78 C79 117.5(3) . . ? C80 C79 C84 119.7(4) . . ? C80 C79 C78 120.7(4) . . ? C84 C79 C78 119.6(3) . . ? C79 C80 C81 119.6(4) . . ? C79 C80 H80A 120.2 . . ? C81 C80 H80A 120.2 . . ? C82 C81 C80 119.8(4) . . ? C82 C81 H81A 120.1 . . ? C80 C81 H81A 120.1 . . ? C83 C82 C81 121.2(4) . . ? C83 C82 H82A 119.4 . . ? C81 C82 H82A 119.4 . . ? C82 C83 C84 118.8(5) . . ? C82 C83 H83A 120.6 . . ? C84 C83 H83A 120.6 . . ? C79 C84 C83 120.9(4) . . ? C79 C84 H84A 119.6 . . ? C83 C84 H84A 119.6 . . ? C85 O35 Fe5 131.8(2) . . ? O36 C85 O35 124.1(3) . . ? O36 C85 C86 118.4(3) . . ? O35 C85 C86 117.5(3) . . ? C87 C86 C91 119.5(3) . . ? C87 C86 C85 120.4(3) . . ? C91 C86 C85 120.1(3) . . ? C86 C87 C88 120.7(3) . . ? C86 C87 H87A 119.7 . . ? C88 C87 H87A 119.7 . . ? C87 C88 C89 119.7(3) . . ? C87 C88 H88A 120.1 . . ? C89 C88 H88A 120.1 . . ? C90 C89 C88 120.1(3) . . ? C90 C89 H89A 119.9 . . ? C88 C89 H89A 119.9 . . ? C89 C90 C91 119.9(4) . . ? C89 C90 H90A 120.0 . . ? C91 C90 H90A 120.0 . . ? C86 C91 C90 120.0(3) . . ? C86 C91 H91A 120.0 . . ? C90 C91 H91A 120.0 . . ? C92 O37 Yb3 136.8(2) . . ? O37 C92 O38 124.3(3) . . ? O37 C92 C93 118.0(3) . . ? O38 C92 C93 117.6(3) . . ? C94 C93 C98 119.3(3) . . ? C94 C93 C92 121.0(3) . . ? C98 C93 C92 119.8(3) . . ? C95 C94 C93 120.1(3) . . ? C95 C94 H94A 120.0 . . ? C93 C94 H94A 120.0 . . ? C96 C95 C94 120.7(4) . . ? C96 C95 H95A 119.7 . . ? C94 C95 H95A 119.7 . . ? C95 C96 C97 119.5(4) . . ? C95 C96 H96A 120.3 . . ? C97 C96 H96A 120.3 . . ? C98 C97 C96 120.4(3) . . ? C98 C97 H97A 119.8 . . ? C96 C97 H97A 119.8 . . ? C97 C98 C93 120.2(3) . . ? C97 C98 H98A 119.9 . . ? C93 C98 H98A 119.9 . . ? N111 C111 C112 177.4(6) . . ? C111 C112 H11E 109.5 . . ? C111 C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C111 C112 H11G 109.5 . . ? H11E C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? O46 S2 O44 114.4(4) . . ? O46 S2 O45 113.5(6) . . ? O44 S2 O45 115.6(6) . . ? O46 S2 C100 103.8(4) . . ? O44 S2 C100 104.4(4) . . ? O45 S2 C100 103.2(6) . . ? F6 C100 F5 107.9(9) . . ? F6 C100 F4 106.6(8) . . ? F5 C100 F4 104.1(8) . . ? F6 C100 S2 112.5(7) . . ? F5 C100 S2 112.9(7) . . ? F4 C100 S2 112.1(7) . . ? N211 C211 C212 178.3(15) . . ? C211 C212 H21C 109.5 . . ? C211 C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? C211 C212 H21E 109.5 . . ? H21C C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H11 O20 0.98(3) 1.87(3) 2.829(3) 165(3) . O1 H1 O32 0.76(3) 2.03(3) 2.717(3) 149(4) . O7 H7 O34 0.74(3) 1.87(3) 2.594(4) 165(4) . O10 H10 O30 0.82(3) 1.78(3) 2.598(3) 170(4) . O13 H13 O31 0.80(3) 1.91(3) 2.677(3) 162(4) . O16 H16 O36 0.80(3) 1.89(3) 2.600(3) 148(4) . O19 H19 O38 0.81(3) 1.70(3) 2.501(3) 171(4) . O22B H22B O22A 0.84 1.93 2.739(8) 162.4 2_566 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.216 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 912845' ####################################################################### # # 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_amb1ybs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C79 H102 Fe4 N4 O29 Yb2), 3(C2 H3 N)' _chemical_formula_sum 'C85 H111 Fe4 N7 O29 Yb2' _chemical_formula_weight 2264.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2113(9) _cell_length_b 18.5580(13) _cell_length_c 19.2000(12) _cell_angle_alpha 84.231(5) _cell_angle_beta 70.788(5) _cell_angle_gamma 83.144(5) _cell_volume 4737.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 56190 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 27.89 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 2.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.467 _exptl_absorpt_correction_T_max 0.629 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76472 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_unetI/netI 0.0501 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.59 _reflns_number_total 21770 _reflns_number_gt 15906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. O-H distances were resrrained: DFIX 0.92 0.04 O3 H3 O6 H6 O9 H9 O12 H12 O15 H15 Three methylene carbons of Me-tea ligands and two benzoate ligands were two fold disordered, and modelled using isotropic partial occupancy atoms. Geometrical similarity restraints were applied to these methylene and carboxylate groups, and the disordered phenyl rings were modelled as rigid hexagons (AFIX 66): SADI C8 C9A C8 C9B SADI C45 C46A C45 C46B SADI C66 C67A C66 C67B SAME O22 O23B C52B C53B Two lattice MeCN per cluster were multiply disordered and treated using SQUEEZE (see below). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.057 0.500 0.500 376 84 '4 MeCN (= 88 e)' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _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^)+(0.1079P)^2^+9.2199P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21770 _refine_ls_number_parameters 1014 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1851 _refine_ls_wR_factor_gt 0.1752 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.032 _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 Yb1 Yb 0.56885(2) 0.312215(17) 0.244193(17) 0.04474(9) Uani 1 1 d . B . Yb2 Yb 0.23920(2) 0.186719(17) 0.077943(17) 0.04478(9) Uani 1 1 d . . . Fe1 Fe 0.59800(8) 0.30737(6) 0.06325(6) 0.0491(2) Uani 1 1 d . B . Fe2 Fe 0.45836(8) 0.25521(6) -0.00928(5) 0.0470(2) Uani 1 1 d . D . Fe3 Fe 0.38035(8) 0.21106(5) 0.34132(6) 0.0450(2) Uani 1 1 d . B . Fe4 Fe 0.23315(8) 0.13880(6) 0.25299(6) 0.0469(2) Uani 1 1 d . D . O1 O 0.5086(4) 0.2270(3) 0.0769(3) 0.0473(11) Uani 1 1 d . . . C1 C 0.5419(6) 0.1539(4) 0.0927(5) 0.0530(18) Uani 1 1 d . D . H1A H 0.4923 0.1335 0.1367 0.080 Uiso 1 1 calc R . . H1B H 0.6060 0.1524 0.1018 0.080 Uiso 1 1 calc R . . H1C H 0.5503 0.1252 0.0505 0.080 Uiso 1 1 calc R . . O2 O 0.5159(4) 0.3457(3) 0.0002(3) 0.0545(13) Uani 1 1 d . . . C2 C 0.5258(11) 0.4093(5) -0.0487(5) 0.088(4) Uani 1 1 d . D . H2A H 0.5473 0.4478 -0.0275 0.132 Uiso 1 1 calc R . . H2B H 0.4612 0.4256 -0.0558 0.132 Uiso 1 1 calc R . . H2C H 0.5757 0.3983 -0.0964 0.132 Uiso 1 1 calc R . . O3 O 0.3374(4) 0.1999(3) 0.2553(3) 0.0463(11) Uani 1 1 d D . . H3 H 0.360(6) 0.228(4) 0.212(3) 0.056 Uiso 1 1 d D . . N1 N 0.4831(5) 0.4407(3) 0.2662(3) 0.0529(15) Uani 1 1 d . . . C3 C 0.4422(8) 0.4664(5) 0.2059(5) 0.065(2) Uani 1 1 d . . . H3A H 0.4878 0.4996 0.1707 0.078 Uiso 1 1 calc R . . H3B H 0.3767 0.4945 0.2268 0.078 Uiso 1 1 calc R . . C4 C 0.4285(7) 0.4062(5) 0.1646(5) 0.064(2) Uani 1 1 d . B . H4A H 0.3674 0.3826 0.1938 0.076 Uiso 1 1 calc R . . H4B H 0.4203 0.4262 0.1169 0.076 Uiso 1 1 calc R . . O4 O 0.5126(4) 0.3542(3) 0.1514(3) 0.0452(11) Uani 1 1 d . . . C5 C 0.4036(7) 0.4366(4) 0.3388(4) 0.0558(19) Uani 1 1 d . . . H5A H 0.3600 0.4829 0.3457 0.067 Uiso 1 1 calc R . . H5B H 0.4342 0.4292 0.3788 0.067 Uiso 1 1 calc R . . C6 C 0.3418(6) 0.3742(4) 0.3430(5) 0.0550(18) Uani 1 1 d . D . H6A H 0.2999 0.3636 0.3947 0.066 Uiso 1 1 calc R . . H6B H 0.2971 0.3874 0.3127 0.066 Uiso 1 1 calc R . . O5 O 0.4065(4) 0.3127(3) 0.3165(3) 0.0439(10) Uani 1 1 d . . . C7 C 0.5567(8) 0.4879(6) 0.2688(7) 0.079(3) Uani 1 1 d . B . H7A H 0.5691 0.4782 0.3169 0.095 Uiso 1 1 calc R . . H7B H 0.5292 0.5392 0.2657 0.095 Uiso 1 1 calc R . . C8 C 0.6536(9) 0.4771(7) 0.2079(9) 0.099(4) Uani 1 1 d D . . H8A H 0.6343 0.4903 0.1623 0.119 Uiso 0.54 1 calc PR A 1 H8B H 0.6507 0.5015 0.1599 0.119 Uiso 0.46 1 d PR A 2 C9A C 0.7344(17) 0.5284(13) 0.2001(15) 0.099(7) Uiso 0.54 1 d PD B 1 H9A1 H 0.7930 0.5163 0.1574 0.148 Uiso 0.54 1 calc PR B 1 H9A2 H 0.7539 0.5228 0.2449 0.148 Uiso 0.54 1 calc PR B 1 H9A3 H 0.7077 0.5788 0.1930 0.148 Uiso 0.54 1 calc PR B 1 C9B C 0.7325(17) 0.5046(13) 0.2377(14) 0.077(6) Uiso 0.46 1 d PD B 2 H9B1 H 0.7987 0.5001 0.2001 0.115 Uiso 0.46 1 calc PR B 2 H9B2 H 0.7345 0.4753 0.2827 0.115 Uiso 0.46 1 calc PR B 2 H9B3 H 0.7135 0.5557 0.2490 0.115 Uiso 0.46 1 calc PR B 2 O6 O 0.6844(5) 0.4000(4) 0.2035(4) 0.0674(16) Uani 1 1 d D B . H6 H 0.728(6) 0.385(6) 0.158(3) 0.081 Uiso 1 1 d D . . N2 N 0.7180(5) 0.2301(5) 0.2565(5) 0.070(2) Uani 1 1 d . . . C10 C 0.7975(7) 0.2328(6) 0.1840(6) 0.077(3) Uani 1 1 d . D . H10A H 0.8519 0.1942 0.1843 0.093 Uiso 1 1 calc R . . H10B H 0.8260 0.2804 0.1752 0.093 Uiso 1 1 calc R . . C11 C 0.7566(7) 0.2224(6) 0.1218(6) 0.076(3) Uani 1 1 d . . . H11A H 0.8043 0.2375 0.0734 0.092 Uiso 1 1 calc R D . H11B H 0.7464 0.1706 0.1214 0.092 Uiso 1 1 calc R . . O7 O 0.6641(4) 0.2661(3) 0.1348(3) 0.0523(12) Uani 1 1 d . B . C12 C 0.6886(9) 0.1575(8) 0.2809(11) 0.137(7) Uani 1 1 d . D . H12A H 0.7397 0.1231 0.2492 0.165 Uiso 1 1 calc R . . H12B H 0.6914 0.1471 0.3318 0.165 Uiso 1 1 calc R . . C13 C 0.5943(7) 0.1415(5) 0.2811(8) 0.084(3) Uani 1 1 d . . . H13A H 0.6042 0.1155 0.2363 0.101 Uiso 1 1 calc R D . H13B H 0.5673 0.1074 0.3243 0.101 Uiso 1 1 calc R . . O8 O 0.5227(4) 0.1989(3) 0.2831(3) 0.0484(11) Uani 1 1 d . B . C14 C 0.7561(10) 0.2611(11) 0.3102(8) 0.125(6) Uani 1 1 d . D . H14A H 0.8004 0.2232 0.3272 0.150 Uiso 1 1 calc R . . H14B H 0.7963 0.3018 0.2849 0.150 Uiso 1 1 calc R . . C15 C 0.6775(13) 0.2865(11) 0.3723(10) 0.133(6) Uani 1 1 d . . . H15A H 0.6524 0.2424 0.4043 0.160 Uiso 1 1 calc R D . C16 C 0.7141(11) 0.3316(13) 0.4189(8) 0.170(9) Uani 1 1 d . D . H16A H 0.6572 0.3491 0.4605 0.255 Uiso 1 1 calc R . . H16B H 0.7455 0.3733 0.3883 0.255 Uiso 1 1 calc R . . H16C H 0.7631 0.3015 0.4377 0.255 Uiso 1 1 calc R . . O9 O 0.5939(5) 0.3245(4) 0.3553(3) 0.0640(16) Uani 1 1 d D B . H9 H 0.551(6) 0.310(5) 0.402(3) 0.077 Uiso 1 1 d D . . N3 N 0.1163(5) 0.2998(4) 0.0914(4) 0.0555(16) Uani 1 1 d . D . C17 C 0.1730(8) 0.3643(5) 0.0750(6) 0.072(3) Uani 1 1 d . . . H17A H 0.1818 0.3831 0.0233 0.086 Uiso 0.53 1 calc PR C 1 H17B H 0.1338 0.4028 0.1078 0.086 Uiso 0.53 1 calc PR C 1 H17C H 0.1675 0.3833 0.1227 0.086 Uiso 0.47 1 calc PR C 2 H17D H 0.1393 0.4021 0.0488 0.086 Uiso 0.47 1 calc PR C 2 C18A C 0.2694(12) 0.3494(9) 0.0847(9) 0.057(3) Uiso 0.53 1 d P D 1 H18A H 0.3094 0.3909 0.0622 0.068 Uiso 0.53 1 calc PR D 1 H18B H 0.2605 0.3454 0.1383 0.068 Uiso 0.53 1 calc PR D 1 C18B C 0.2807(13) 0.3559(9) 0.0307(10) 0.055(4) Uiso 0.47 1 d P D 2 H18C H 0.2886 0.3579 -0.0227 0.066 Uiso 0.47 1 calc PR D 2 H18D H 0.3156 0.3955 0.0393 0.066 Uiso 0.47 1 calc PR D 2 O10 O 0.3229(4) 0.2856(3) 0.0536(3) 0.0475(11) Uani 1 1 d . D . C19 C 0.0483(6) 0.2963(5) 0.1684(5) 0.060(2) Uani 1 1 d . . . H19A H -0.0010 0.2609 0.1737 0.072 Uiso 1 1 calc R D . H19B H 0.0110 0.3446 0.1797 0.072 Uiso 1 1 calc R . . C20 C 0.1039(7) 0.2741(4) 0.2230(4) 0.058(2) Uani 1 1 d . D . H20A H 0.1389 0.3151 0.2283 0.070 Uiso 1 1 calc R . . H20B H 0.0563 0.2605 0.2719 0.070 Uiso 1 1 calc R . . O11 O 0.1737(4) 0.2143(3) 0.1969(3) 0.0491(11) Uani 1 1 d . D . C21 C 0.0585(7) 0.2947(6) 0.0394(5) 0.071(3) Uani 1 1 d . . . H21A H 0.0129 0.2557 0.0589 0.085 Uiso 1 1 calc R D . H21B H 0.0170 0.3411 0.0371 0.085 Uiso 1 1 calc R . . C22 C 0.1253(8) 0.2789(6) -0.0367(5) 0.074(3) Uani 1 1 d . D . H22 H 0.1579 0.3239 -0.0604 0.088 Uiso 1 1 calc R . . C23 C 0.0689(8) 0.2574(7) -0.0842(6) 0.089(3) Uani 1 1 d . . . H23A H 0.1156 0.2482 -0.1335 0.133 Uiso 1 1 calc R D . H23B H 0.0182 0.2969 -0.0881 0.133 Uiso 1 1 calc R . . H23C H 0.0362 0.2133 -0.0618 0.133 Uiso 1 1 calc R . . O12 O 0.2032(4) 0.2222(3) -0.0315(3) 0.0566(13) Uani 1 1 d D D . H12 H 0.251(5) 0.223(5) -0.077(3) 0.068 Uiso 1 1 d D . . N4 N 0.2630(5) 0.0617(4) 0.0301(4) 0.0556(16) Uani 1 1 d . D . C24 C 0.3407(7) 0.0653(5) -0.0443(4) 0.0566(19) Uani 1 1 d . . . H24A H 0.3105 0.0915 -0.0804 0.068 Uiso 1 1 calc R D . H24B H 0.3642 0.0153 -0.0600 0.068 Uiso 1 1 calc R . . C25 C 0.4289(6) 0.1031(5) -0.0448(5) 0.0573(19) Uani 1 1 d . D . H25A H 0.4719 0.0702 -0.0216 0.069 Uiso 1 1 calc R . . H25B H 0.4693 0.1162 -0.0964 0.069 Uiso 1 1 calc R . . O13 O 0.3943(4) 0.1660(3) -0.0056(3) 0.0463(11) Uani 1 1 d . D . C26 C 0.2904(8) 0.0091(5) 0.0826(5) 0.069(2) Uani 1 1 d . . . H26A H 0.3346 -0.0312 0.0551 0.083 Uiso 1 1 calc R D . H26B H 0.2289 -0.0116 0.1157 0.083 Uiso 1 1 calc R . . C27 C 0.3421(7) 0.0371(4) 0.1293(5) 0.061(2) Uani 1 1 d . D . H27A H 0.3374 0.0029 0.1731 0.073 Uiso 1 1 calc R . . H27B H 0.4138 0.0392 0.1007 0.073 Uiso 1 1 calc R . . O14 O 0.3003(4) 0.1066(3) 0.1529(3) 0.0464(11) Uani 1 1 d . D . C28 C 0.1634(8) 0.0489(6) 0.0215(6) 0.073(3) Uani 1 1 d . . . H28A H 0.1542 0.0793 -0.0216 0.087 Uiso 1 1 calc R D . H28B H 0.1647 -0.0027 0.0120 0.087 Uiso 1 1 calc R . . C29 C 0.0793(7) 0.0665(6) 0.0877(6) 0.073(3) Uani 1 1 d . D . H29 H 0.0855 0.0290 0.1275 0.088 Uiso 1 1 calc R . . C30 C -0.0221(8) 0.0608(8) 0.0786(8) 0.098(4) Uani 1 1 d . . . H30A H -0.0754 0.0732 0.1244 0.147 Uiso 1 1 calc R D . H30B H -0.0262 0.0110 0.0678 0.147 Uiso 1 1 calc R . . H30C H -0.0299 0.0946 0.0378 0.147 Uiso 1 1 calc R . . O15 O 0.0880(4) 0.1342(3) 0.1117(3) 0.0545(13) Uani 1 1 d D D . H15 H 0.076(7) 0.118(5) 0.161(3) 0.065 Uiso 1 1 d D . . O16 O 0.6996(4) 0.2489(4) -0.0211(3) 0.0618(14) Uani 1 1 d . . . O17 O 0.5972(4) 0.2125(3) -0.0765(3) 0.0578(13) Uani 1 1 d . . . C31 C 0.6829(7) 0.2173(5) -0.0703(4) 0.059(2) Uani 1 1 d . D . C32 C 0.7715(7) 0.1828(5) -0.1265(5) 0.062(2) Uani 1 1 d . . . C33 C 0.7613(8) 0.1607(5) -0.1912(5) 0.068(2) Uani 1 1 d . D . H33 H 0.6985 0.1682 -0.1995 0.081 Uiso 1 1 calc R . . C34 C 0.8445(8) 0.1276(6) -0.2432(6) 0.079(3) Uani 1 1 d . . . H34 H 0.8396 0.1143 -0.2883 0.095 Uiso 1 1 calc R D . C35 C 0.9350(9) 0.1140(7) -0.2286(7) 0.093(4) Uani 1 1 d . D . H35 H 0.9906 0.0894 -0.2631 0.111 Uiso 1 1 calc R . . C36 C 0.9455(7) 0.1355(7) -0.1653(7) 0.088(3) Uani 1 1 d . . . H36 H 1.0079 0.1274 -0.1564 0.105 Uiso 1 1 calc R D . C37 C 0.8604(8) 0.1701(6) -0.1140(6) 0.080(3) Uani 1 1 d . D . H37 H 0.8659 0.1848 -0.0696 0.095 Uiso 1 1 calc R . . O18 O 0.3704(4) 0.1043(3) 0.3723(3) 0.0537(13) Uani 1 1 d . . . O19 O 0.3018(4) 0.0534(3) 0.3007(3) 0.0566(14) Uani 1 1 d . . . C38 C 0.3475(6) 0.0505(4) 0.3467(4) 0.0469(16) Uani 1 1 d . D . C39 C 0.3791(6) -0.0233(4) 0.3754(4) 0.0484(16) Uani 1 1 d . . . C40 C 0.4322(7) -0.0312(4) 0.4254(4) 0.0558(19) Uani 1 1 d . D . H40 H 0.4491 0.0107 0.4415 0.067 Uiso 1 1 calc R . . C41 C 0.4609(7) -0.1001(5) 0.4521(5) 0.062(2) Uani 1 1 d . . . H41 H 0.4979 -0.1054 0.4858 0.075 Uiso 1 1 calc R D . C42 C 0.4339(7) -0.1615(4) 0.4281(5) 0.066(2) Uani 1 1 d . D . H42 H 0.4525 -0.2090 0.4457 0.079 Uiso 1 1 calc R . . C43 C 0.3810(7) -0.1527(4) 0.3798(5) 0.060(2) Uani 1 1 d . . . H43 H 0.3622 -0.1945 0.3648 0.072 Uiso 1 1 calc R D . C44 C 0.3539(6) -0.0849(4) 0.3519(5) 0.0563(19) Uani 1 1 d . D . H44 H 0.3186 -0.0802 0.3171 0.068 Uiso 1 1 calc R . . O20 O 0.2331(4) 0.2373(3) 0.4017(3) 0.0558(13) Uani 1 1 d . . . O21 O 0.1467(4) 0.1752(3) 0.3522(3) 0.0569(13) Uani 1 1 d . . . C45 C 0.1540(6) 0.2153(5) 0.3992(4) 0.0555(19) Uani 1 1 d D D . C46A C 0.0564(5) 0.2323(5) 0.4585(4) 0.050(2) Uiso 0.73 1 d PGD D 1 C47A C -0.0317(6) 0.2089(5) 0.4560(4) 0.062(3) Uiso 0.73 1 d PG D 1 H47A H -0.0317 0.1854 0.4143 0.075 Uiso 0.73 1 calc PR D 1 C48A C -0.1198(5) 0.2199(6) 0.5146(5) 0.084(4) Uiso 0.73 1 d PG D 1 H48A H -0.1800 0.2040 0.5129 0.101 Uiso 0.73 1 calc PR D 1 C49A C -0.1197(6) 0.2544(6) 0.5756(5) 0.098(5) Uiso 0.73 1 d PG D 1 H49A H -0.1799 0.2619 0.6157 0.118 Uiso 0.73 1 calc PR D 1 C50A C -0.0316(8) 0.2778(6) 0.5781(4) 0.111(6) Uiso 0.73 1 d PG D 1 H50A H -0.0316 0.3013 0.6198 0.133 Uiso 0.73 1 calc PR D 1 C51A C 0.0565(6) 0.2667(5) 0.5195(5) 0.077(4) Uiso 0.73 1 d PG D 1 H51A H 0.1167 0.2827 0.5212 0.092 Uiso 0.73 1 calc PR D 1 C46B C 0.0722(14) 0.2566(13) 0.4591(11) 0.055(7) Uiso 0.27 1 d PGD D 2 C47B C -0.0224(18) 0.2361(13) 0.4687(13) 0.069(9) Uiso 0.27 1 d PG D 2 H47B H -0.0317 0.2061 0.4346 0.083 Uiso 0.27 1 calc PR D 2 C48B C -0.1035(14) 0.2595(16) 0.5281(15) 0.108(15) Uiso 0.27 1 d PG D 2 H48B H -0.1682 0.2455 0.5347 0.130 Uiso 0.27 1 calc PR D 2 C49B C -0.0899(16) 0.3034(16) 0.5780(12) 0.078(10) Uiso 0.27 1 d PG D 2 H49B H -0.1453 0.3194 0.6186 0.094 Uiso 0.27 1 calc PR D 2 C50B C 0.005(2) 0.3239(15) 0.5684(12) 0.101(14) Uiso 0.27 1 d PG D 2 H50B H 0.0140 0.3538 0.6025 0.121 Uiso 0.27 1 calc PR D 2 C51B C 0.0858(14) 0.3005(15) 0.5090(14) 0.086(11) Uiso 0.27 1 d PG D 2 H51B H 0.1505 0.3145 0.5024 0.104 Uiso 0.27 1 calc PR D 2 O22 O 0.6867(5) 0.3894(4) 0.0219(4) 0.0709(17) Uani 1 1 d D . . O23A O 0.8028(10) 0.4058(8) 0.0777(8) 0.071(4) Uiso 0.58 1 d PD D 1 C52A C 0.7749(10) 0.4011(13) 0.0234(12) 0.060(6) Uiso 0.58 1 d PD D 1 C53A C 0.8515(8) 0.4199(7) -0.0490(6) 0.063(4) Uiso 0.58 1 d PGD D 1 C54A C 0.9350(9) 0.4541(7) -0.0525(6) 0.066(4) Uiso 0.58 1 d PG D 1 H54A H 0.9434 0.4670 -0.0084 0.080 Uiso 0.58 1 calc PR D 1 C55A C 1.0060(8) 0.4695(8) -0.1205(8) 0.093(6) Uiso 0.58 1 d PG D 1 H55A H 1.0630 0.4929 -0.1229 0.112 Uiso 0.58 1 calc PR D 1 C56A C 0.9936(12) 0.4507(11) -0.1850(6) 0.118(10) Uiso 0.58 1 d PG D 1 H56A H 1.0421 0.4612 -0.2315 0.141 Uiso 0.58 1 calc PR D 1 C57A C 0.9102(13) 0.4164(11) -0.1815(6) 0.141(11) Uiso 0.58 1 d PG D 1 H57A H 0.9017 0.4036 -0.2256 0.169 Uiso 0.58 1 calc PR D 1 C58A C 0.8391(10) 0.4010(8) -0.1135(8) 0.104(7) Uiso 0.58 1 d PG D 1 H58A H 0.7821 0.3776 -0.1111 0.125 Uiso 0.58 1 calc PR D 1 O23B O 0.8162(15) 0.3917(13) 0.0563(12) 0.087(7) Uiso 0.42 1 d PD D 2 C52B C 0.7766(15) 0.402(2) 0.0070(14) 0.079(13) Uiso 0.42 1 d PD D 2 C53B C 0.8312(12) 0.4175(10) -0.0726(8) 0.067(5) Uiso 0.42 1 d PGD D 2 C54B C 0.9271(12) 0.4392(10) -0.0907(9) 0.069(6) Uiso 0.42 1 d PG D 2 H54B H 0.9545 0.4447 -0.0528 0.083 Uiso 0.42 1 calc PR D 2 C55B C 0.9830(12) 0.4529(13) -0.1644(11) 0.089(9) Uiso 0.42 1 d PG D 2 H55B H 1.0486 0.4677 -0.1768 0.106 Uiso 0.42 1 calc PR D 2 C56B C 0.9430(18) 0.4448(16) -0.2199(8) 0.150(16) Uiso 0.42 1 d PG D 2 H56B H 0.9812 0.4542 -0.2702 0.180 Uiso 0.42 1 calc PR D 2 C57B C 0.8471(19) 0.4231(15) -0.2017(10) 0.151(16) Uiso 0.42 1 d PG D 2 H57B H 0.8198 0.4176 -0.2397 0.181 Uiso 0.42 1 calc PR D 2 C58B C 0.7912(12) 0.4094(12) -0.1281(12) 0.104(9) Uiso 0.42 1 d PG D 2 H58B H 0.7257 0.3946 -0.1157 0.125 Uiso 0.42 1 calc PR D 2 O24 O 0.4389(5) 0.2986(3) -0.1044(3) 0.0644(16) Uani 1 1 d . . . O25 O 0.3447(5) 0.2474(4) -0.1550(3) 0.0680(16) Uani 1 1 d . . . C59 C 0.4178(7) 0.2811(5) -0.1588(4) 0.0553(19) Uani 1 1 d . D . C60 C 0.4857(7) 0.3057(4) -0.2331(4) 0.0531(18) Uani 1 1 d . . . C61 C 0.5804(7) 0.3249(4) -0.2412(4) 0.058(2) Uani 1 1 d . D . H61 H 0.6028 0.3206 -0.1993 0.069 Uiso 1 1 calc R . . C62 C 0.6425(7) 0.3502(5) -0.3085(5) 0.061(2) Uani 1 1 d . . . H62 H 0.7070 0.3632 -0.3131 0.073 Uiso 1 1 calc R D . C63 C 0.6099(8) 0.3563(5) -0.3694(5) 0.070(3) Uani 1 1 d . D . H63 H 0.6518 0.3746 -0.4158 0.084 Uiso 1 1 calc R . . C64 C 0.5165(8) 0.3360(4) -0.3635(4) 0.063(2) Uani 1 1 d . . . H64 H 0.4956 0.3395 -0.4060 0.075 Uiso 1 1 calc R D . C65 C 0.4528(7) 0.3103(4) -0.2950(4) 0.0570(19) Uani 1 1 d . D . H65 H 0.3888 0.2964 -0.2906 0.068 Uiso 1 1 calc R . . O26 O 0.4089(5) 0.2137(3) 0.4406(3) 0.0574(14) Uani 1 1 d . . . O27 O 0.4458(5) 0.3132(3) 0.4762(3) 0.0666(16) Uani 1 1 d . . . C66 C 0.3935(7) 0.2612(5) 0.4849(4) 0.0553(19) Uani 1 1 d D D . C67A C 0.3095(7) 0.2473(6) 0.5555(4) 0.052(3) Uiso 0.62 1 d PGD D 1 C68A C 0.2779(8) 0.3019(5) 0.6049(6) 0.061(3) Uiso 0.62 1 d PG D 1 H68A H 0.3104 0.3455 0.5942 0.073 Uiso 0.62 1 calc PR D 1 C69A C 0.1989(8) 0.2927(6) 0.6700(5) 0.086(5) Uiso 0.62 1 d PG D 1 H69A H 0.1773 0.3300 0.7038 0.104 Uiso 0.62 1 calc PR D 1 C70A C 0.1514(7) 0.2289(7) 0.6857(5) 0.078(4) Uiso 0.62 1 d PG D 1 H70A H 0.0974 0.2227 0.7302 0.093 Uiso 0.62 1 calc PR D 1 C71A C 0.1830(8) 0.1743(6) 0.6363(6) 0.078(4) Uiso 0.62 1 d PG D 1 H71A H 0.1505 0.1307 0.6471 0.094 Uiso 0.62 1 calc PR D 1 C72A C 0.2620(8) 0.1835(5) 0.5712(5) 0.067(4) Uiso 0.62 1 d PG D 1 H72A H 0.2836 0.1462 0.5375 0.080 Uiso 0.62 1 calc PR D 1 C67B C 0.3075(11) 0.2687(11) 0.5577(8) 0.051(5) Uiso 0.38 1 d PGD D 2 C68B C 0.2742(14) 0.3313(9) 0.5963(10) 0.079(8) Uiso 0.38 1 d PG D 2 H68B H 0.3071 0.3743 0.5785 0.095 Uiso 0.38 1 calc PR D 2 C69B C 0.1928(15) 0.3308(11) 0.6609(10) 0.098(10) Uiso 0.38 1 d PG D 2 H69B H 0.1700 0.3736 0.6873 0.118 Uiso 0.38 1 calc PR D 2 C70B C 0.1447(13) 0.2678(13) 0.6869(9) 0.088(8) Uiso 0.38 1 d PG D 2 H70B H 0.0891 0.2675 0.7310 0.105 Uiso 0.38 1 calc PR D 2 C71B C 0.1780(15) 0.2053(10) 0.6483(11) 0.096(9) Uiso 0.38 1 d PG D 2 H71B H 0.1452 0.1622 0.6660 0.115 Uiso 0.38 1 calc PR D 2 C72B C 0.2594(15) 0.2057(9) 0.5837(10) 0.083(8) Uiso 0.38 1 d PG D 2 H72B H 0.2822 0.1629 0.5573 0.099 Uiso 0.38 1 calc PR D 2 O28 O 0.1245(4) 0.0704(3) 0.2713(4) 0.0610(14) Uani 1 1 d . . . O29 O -0.0128(4) 0.1225(4) 0.2499(3) 0.0674(16) Uani 1 1 d . . . C73 C 0.0307(6) 0.0801(4) 0.2867(5) 0.0536(18) Uani 1 1 d . D . C74 C -0.0311(6) 0.0370(5) 0.3515(4) 0.0561(18) Uani 1 1 d . . . C75 C 0.0146(8) -0.0108(5) 0.3940(5) 0.065(2) Uani 1 1 d . D . H75 H 0.0854 -0.0160 0.3822 0.078 Uiso 1 1 calc R . . C76 C -0.0445(11) -0.0507(6) 0.4538(5) 0.087(3) Uani 1 1 d . . . H76 H -0.0140 -0.0828 0.4835 0.105 Uiso 1 1 calc R D . C77 C -0.1447(11) -0.0445(7) 0.4706(7) 0.105(4) Uani 1 1 d . D . H77 H -0.1841 -0.0742 0.5101 0.126 Uiso 1 1 calc R . . C78 C -0.1884(10) 0.0030(11) 0.4319(9) 0.149(8) Uani 1 1 d . . . H78 H -0.2593 0.0113 0.4480 0.179 Uiso 1 1 calc R D . C79 C -0.1334(8) 0.0407(8) 0.3688(8) 0.125(6) Uani 1 1 d . D . H79 H -0.1658 0.0689 0.3378 0.150 Uiso 1 1 calc R . . N81 N 0.2097(15) 0.0456(13) 0.8087(10) 0.201(10) Uani 1 1 d . . . C81 C 0.2793(11) 0.0724(9) 0.7780(7) 0.106(4) Uani 1 1 d . . . C82 C 0.3616(11) 0.1114(8) 0.7405(7) 0.104(4) Uani 1 1 d . . . H82A H 0.3637 0.1227 0.6891 0.156 Uiso 1 1 calc R . . H82B H 0.4232 0.0821 0.7418 0.156 Uiso 1 1 calc R . . H82C H 0.3554 0.1567 0.7644 0.156 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 Yb1 0.04411(17) 0.05108(18) 0.04189(16) 0.00742(12) -0.01946(13) -0.00794(13) Yb2 0.04530(17) 0.04880(17) 0.04146(16) 0.00597(12) -0.01787(13) -0.00515(13) Fe1 0.0498(6) 0.0577(6) 0.0388(5) 0.0023(4) -0.0110(4) -0.0150(5) Fe2 0.0541(6) 0.0510(6) 0.0370(5) 0.0057(4) -0.0164(5) -0.0115(5) Fe3 0.0508(6) 0.0430(5) 0.0422(5) 0.0079(4) -0.0184(5) -0.0073(4) Fe4 0.0446(5) 0.0523(6) 0.0461(5) 0.0126(4) -0.0201(5) -0.0105(4) O1 0.051(3) 0.055(3) 0.038(2) 0.005(2) -0.017(2) -0.009(2) C1 0.054(4) 0.051(4) 0.056(4) 0.009(3) -0.023(4) -0.009(3) O2 0.073(4) 0.052(3) 0.041(3) 0.010(2) -0.022(3) -0.015(3) C2 0.160(12) 0.058(5) 0.054(5) 0.023(4) -0.042(6) -0.043(6) O3 0.047(3) 0.051(3) 0.042(3) 0.009(2) -0.018(2) -0.008(2) N1 0.062(4) 0.049(3) 0.043(3) 0.006(3) -0.011(3) -0.014(3) C3 0.078(6) 0.057(5) 0.053(5) 0.008(4) -0.020(4) 0.004(4) C4 0.065(5) 0.074(5) 0.053(5) 0.005(4) -0.029(4) 0.008(4) O4 0.049(3) 0.051(3) 0.038(2) 0.008(2) -0.022(2) -0.003(2) C5 0.068(5) 0.047(4) 0.049(4) 0.000(3) -0.014(4) -0.012(4) C6 0.057(5) 0.047(4) 0.053(4) 0.006(3) -0.009(4) -0.007(3) O5 0.046(3) 0.044(2) 0.040(2) 0.004(2) -0.014(2) -0.004(2) C7 0.083(7) 0.065(6) 0.093(7) -0.008(5) -0.023(6) -0.033(5) C8 0.083(8) 0.079(7) 0.136(11) -0.013(7) -0.025(8) -0.029(6) O6 0.059(4) 0.067(4) 0.077(4) 0.004(3) -0.020(3) -0.026(3) N2 0.048(4) 0.088(5) 0.074(5) 0.016(4) -0.026(4) -0.003(4) C10 0.047(5) 0.089(7) 0.092(7) 0.002(6) -0.021(5) 0.001(5) C11 0.057(5) 0.090(7) 0.082(7) -0.015(5) -0.027(5) 0.016(5) O7 0.039(3) 0.065(3) 0.054(3) 0.000(2) -0.017(2) -0.004(2) C12 0.053(6) 0.113(10) 0.214(18) 0.073(11) -0.028(9) 0.006(6) C13 0.057(5) 0.050(5) 0.146(11) 0.011(6) -0.042(6) 0.005(4) O8 0.047(3) 0.046(3) 0.052(3) 0.008(2) -0.020(2) -0.003(2) C14 0.078(8) 0.223(18) 0.085(8) -0.019(10) -0.054(7) 0.032(10) C15 0.120(12) 0.187(17) 0.133(13) -0.018(12) -0.100(12) 0.006(11) C16 0.092(10) 0.36(3) 0.095(10) -0.049(14) -0.070(9) -0.014(14) O9 0.072(4) 0.087(4) 0.047(3) 0.010(3) -0.038(3) -0.017(3) N3 0.053(4) 0.061(4) 0.051(4) 0.010(3) -0.022(3) 0.002(3) C17 0.075(6) 0.058(5) 0.072(6) 0.018(4) -0.017(5) -0.001(4) O10 0.053(3) 0.043(3) 0.049(3) 0.005(2) -0.020(2) -0.010(2) C19 0.050(4) 0.066(5) 0.056(5) 0.010(4) -0.014(4) 0.002(4) C20 0.068(5) 0.055(4) 0.047(4) 0.009(3) -0.018(4) 0.002(4) O11 0.050(3) 0.051(3) 0.045(3) 0.005(2) -0.017(2) -0.001(2) C21 0.059(5) 0.097(7) 0.057(5) 0.017(5) -0.030(4) 0.000(5) C22 0.073(6) 0.089(7) 0.062(5) 0.004(5) -0.034(5) 0.007(5) C23 0.075(7) 0.124(9) 0.079(7) -0.002(6) -0.053(6) 0.023(6) O12 0.054(3) 0.075(4) 0.045(3) 0.009(3) -0.025(3) -0.006(3) N4 0.059(4) 0.057(4) 0.051(4) 0.002(3) -0.016(3) -0.016(3) C24 0.065(5) 0.055(4) 0.049(4) -0.004(3) -0.015(4) -0.012(4) C25 0.057(5) 0.058(4) 0.052(4) -0.009(4) -0.005(4) -0.017(4) O13 0.044(3) 0.050(3) 0.043(3) -0.001(2) -0.011(2) -0.010(2) C26 0.091(7) 0.058(5) 0.062(5) 0.004(4) -0.031(5) -0.009(5) C27 0.059(5) 0.053(4) 0.074(6) -0.004(4) -0.031(4) 0.005(4) O14 0.053(3) 0.041(2) 0.047(3) 0.008(2) -0.021(2) -0.004(2) C28 0.073(6) 0.080(6) 0.074(6) 0.001(5) -0.032(5) -0.023(5) C29 0.059(5) 0.081(6) 0.087(7) -0.004(5) -0.030(5) -0.019(5) C30 0.059(6) 0.134(11) 0.110(9) -0.034(8) -0.030(6) -0.022(6) O15 0.048(3) 0.065(3) 0.055(3) 0.008(3) -0.022(3) -0.018(2) O16 0.051(3) 0.080(4) 0.052(3) -0.012(3) -0.007(3) -0.017(3) O17 0.059(3) 0.068(3) 0.044(3) -0.005(2) -0.009(3) -0.015(3) C31 0.061(5) 0.058(5) 0.044(4) -0.001(3) 0.001(4) -0.008(4) C32 0.058(5) 0.055(5) 0.062(5) -0.004(4) 0.001(4) -0.021(4) C33 0.072(6) 0.069(5) 0.055(5) -0.005(4) -0.009(4) -0.011(5) C34 0.078(7) 0.085(7) 0.066(6) -0.023(5) -0.008(5) -0.007(5) C35 0.071(7) 0.093(8) 0.101(9) -0.044(7) 0.002(6) -0.012(6) C36 0.042(5) 0.114(9) 0.103(8) -0.046(7) -0.006(5) -0.011(5) C37 0.061(6) 0.090(7) 0.081(7) -0.027(6) -0.011(5) -0.001(5) O18 0.065(3) 0.049(3) 0.050(3) 0.012(2) -0.025(3) -0.009(2) O19 0.067(3) 0.052(3) 0.061(3) 0.018(2) -0.038(3) -0.014(3) C38 0.049(4) 0.048(4) 0.042(4) 0.015(3) -0.016(3) -0.008(3) C39 0.049(4) 0.044(4) 0.050(4) 0.012(3) -0.017(3) -0.008(3) C40 0.073(5) 0.050(4) 0.050(4) 0.010(3) -0.030(4) -0.009(4) C41 0.075(6) 0.058(5) 0.061(5) 0.007(4) -0.037(5) 0.001(4) C42 0.083(6) 0.045(4) 0.069(5) 0.015(4) -0.034(5) 0.006(4) C43 0.068(5) 0.039(4) 0.079(6) 0.013(4) -0.037(5) 0.000(3) C44 0.057(5) 0.050(4) 0.065(5) 0.013(4) -0.028(4) -0.006(3) O20 0.058(3) 0.056(3) 0.049(3) 0.002(2) -0.013(3) -0.008(3) O21 0.051(3) 0.078(4) 0.043(3) 0.009(3) -0.018(2) -0.013(3) C45 0.046(4) 0.066(5) 0.044(4) 0.015(4) -0.007(3) -0.001(4) O22 0.073(4) 0.078(4) 0.064(4) 0.003(3) -0.018(3) -0.033(3) O24 0.094(5) 0.067(4) 0.040(3) 0.010(2) -0.030(3) -0.025(3) O25 0.077(4) 0.089(4) 0.042(3) 0.010(3) -0.025(3) -0.022(3) C59 0.069(5) 0.060(5) 0.040(4) 0.008(3) -0.022(4) -0.016(4) C60 0.072(5) 0.050(4) 0.038(4) 0.003(3) -0.019(4) -0.008(4) C61 0.075(6) 0.056(4) 0.044(4) 0.004(3) -0.025(4) -0.003(4) C62 0.071(6) 0.058(5) 0.053(4) 0.002(4) -0.021(4) -0.006(4) C63 0.097(7) 0.055(5) 0.046(4) 0.004(4) -0.006(5) -0.010(5) C64 0.092(7) 0.052(4) 0.042(4) 0.005(3) -0.019(4) -0.011(4) C65 0.080(6) 0.055(4) 0.038(4) 0.005(3) -0.023(4) -0.008(4) O26 0.077(4) 0.057(3) 0.045(3) 0.008(2) -0.033(3) -0.004(3) O27 0.092(5) 0.068(4) 0.046(3) 0.007(3) -0.029(3) -0.019(3) C66 0.064(5) 0.065(5) 0.040(4) 0.010(3) -0.026(4) -0.002(4) O28 0.047(3) 0.061(3) 0.075(4) 0.017(3) -0.023(3) -0.013(2) O29 0.052(3) 0.084(4) 0.065(4) 0.025(3) -0.022(3) -0.017(3) C73 0.046(4) 0.057(4) 0.058(4) 0.007(4) -0.020(4) -0.008(3) C74 0.052(4) 0.066(5) 0.048(4) 0.003(4) -0.017(4) -0.002(4) C75 0.073(6) 0.070(5) 0.054(5) 0.010(4) -0.024(4) -0.013(4) C76 0.123(10) 0.081(7) 0.050(5) 0.016(5) -0.021(6) -0.014(7) C77 0.106(10) 0.102(9) 0.075(7) 0.027(7) 0.007(7) -0.018(8) C78 0.066(8) 0.202(18) 0.130(12) 0.092(13) 0.001(8) -0.005(9) C79 0.050(6) 0.153(12) 0.132(11) 0.084(10) -0.005(7) -0.009(7) N81 0.170(16) 0.30(3) 0.145(14) 0.071(15) -0.059(13) -0.133(18) C81 0.095(9) 0.150(13) 0.077(8) 0.010(8) -0.027(7) -0.038(9) C82 0.108(10) 0.117(10) 0.079(8) -0.010(7) -0.005(7) -0.045(8) _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 Yb1 O4 2.220(4) . ? Yb1 O8 2.258(5) . ? Yb1 O5 2.268(5) . ? Yb1 O7 2.278(6) . ? Yb1 O9 2.312(5) . ? Yb1 O6 2.344(6) . ? Yb1 N2 2.521(7) . ? Yb1 N1 2.554(7) . ? Yb2 O10 2.232(5) . ? Yb2 O11 2.252(5) . ? Yb2 O14 2.262(4) . ? Yb2 O13 2.274(5) . ? Yb2 O15 2.333(5) . ? Yb2 O12 2.337(5) . ? Yb2 N4 2.525(7) . ? Yb2 N3 2.542(7) . ? Fe1 O4 1.946(5) . ? Fe1 O7 1.956(5) . ? Fe1 O2 1.972(5) . ? Fe1 O1 2.015(5) . ? Fe1 O22 2.022(6) . ? Fe1 O16 2.080(6) . ? Fe2 O10 1.957(6) . ? Fe2 O13 1.967(5) . ? Fe2 O2 2.003(5) . ? Fe2 O1 2.010(5) . ? Fe2 O24 2.011(5) . ? Fe2 O17 2.084(6) . ? Fe3 O5 1.947(5) . ? Fe3 O8 1.961(5) . ? Fe3 O3 1.977(5) . ? Fe3 O18 2.018(5) . ? Fe3 O20 2.057(6) . ? Fe3 O26 2.083(5) . ? Fe4 O11 1.962(5) . ? Fe4 O14 1.962(5) . ? Fe4 O3 1.984(5) . ? Fe4 O21 2.029(6) . ? Fe4 O28 2.034(5) . ? Fe4 O19 2.057(5) . ? O1 C1 1.420(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C2 1.422(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 H3 0.92(4) . ? N1 C7 1.458(11) . ? N1 C3 1.474(10) . ? N1 C5 1.479(10) . ? C3 C4 1.499(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.413(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.516(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O5 1.401(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.492(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O6 1.447(14) . ? C8 C9A 1.539(19) . ? C8 C9B 1.570(19) . ? C8 H8A 1.0000 . ? C8 H8B 0.9974 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? O6 H6 0.93(4) . ? N2 C12 1.446(15) . ? N2 C10 1.476(13) . ? N2 C14 1.501(15) . ? C10 C11 1.527(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O7 1.420(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.405(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O8 1.377(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.41(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O9 1.422(14) . ? C15 C16 1.53(2) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O9 H9 0.93(4) . ? N3 C19 1.476(11) . ? N3 C17 1.473(12) . ? N3 C21 1.502(10) . ? C17 C18A 1.434(18) . ? C17 C18B 1.49(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 H17C 0.9900 . ? C17 H17D 0.9900 . ? C18A O10 1.402(17) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C18B O10 1.458(18) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19 C20 1.508(11) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O11 1.409(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.493(14) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O12 1.454(11) . ? C22 C23 1.503(13) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O12 H12 0.91(4) . ? N4 C26 1.447(11) . ? N4 C24 1.491(10) . ? N4 C28 1.525(11) . ? C24 C25 1.504(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O13 1.403(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.494(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O14 1.408(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.463(15) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O15 1.413(11) . ? C29 C30 1.524(13) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? O15 H15 0.93(4) . ? O16 C31 1.259(10) . ? O17 C31 1.277(11) . ? C31 C32 1.487(12) . ? C32 C37 1.351(14) . ? C32 C33 1.403(13) . ? C33 C34 1.395(14) . ? C33 H33 0.9500 . ? C34 C35 1.392(16) . ? C34 H34 0.9500 . ? C35 C36 1.374(16) . ? C35 H35 0.9500 . ? C36 C37 1.415(14) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? O18 C38 1.276(9) . ? O19 C38 1.251(8) . ? C38 C39 1.499(9) . ? C39 C40 1.390(10) . ? C39 C44 1.394(11) . ? C40 C41 1.394(11) . ? C40 H40 0.9500 . ? C41 C42 1.409(13) . ? C41 H41 0.9500 . ? C42 C43 1.361(12) . ? C42 H42 0.9500 . ? C43 C44 1.380(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? O20 C45 1.257(10) . ? O21 C45 1.262(10) . ? C45 C46A 1.499(10) . ? C45 C46B 1.532(16) . ? C46A C47A 1.3900 . ? C46A C51A 1.3900 . ? C47A C48A 1.3900 . ? C47A H47A 0.9500 . ? C48A C49A 1.3900 . ? C48A H48A 0.9500 . ? C49A C50A 1.3900 . ? C49A H49A 0.9500 . ? C50A C51A 1.3900 . ? C50A H50A 0.9500 . ? C51A H51A 0.9500 . ? C46B C47B 1.3900 . ? C46B C51B 1.3900 . ? C47B C48B 1.3900 . ? C47B H47B 0.9500 . ? C48B C49B 1.3900 . ? C48B H48B 0.9500 . ? C49B C50B 1.3900 . ? C49B H49B 0.9500 . ? C50B C51B 1.3900 . ? C50B H50B 0.9500 . ? C51B H51B 0.9500 . ? O22 C52B 1.260(17) . ? O22 C52A 1.308(14) . ? O23A C52A 1.25(2) . ? C52A C53A 1.495(19) . ? C53A C54A 1.3900 . ? C53A C58A 1.3900 . ? C54A C55A 1.3900 . ? C54A H54A 0.9500 . ? C55A C56A 1.3900 . ? C55A H55A 0.9500 . ? C56A C57A 1.3900 . ? C56A H56A 0.9500 . ? C57A C58A 1.3900 . ? C57A H57A 0.9500 . ? C58A H58A 0.9500 . ? O23B C52B 1.24(2) . ? C52B C53B 1.48(2) . ? C53B C54B 1.3900 . ? C53B C58B 1.3900 . ? C54B C55B 1.3900 . ? C54B H54B 0.9500 . ? C55B C56B 1.3900 . ? C55B H55B 0.9500 . ? C56B C57B 1.3900 . ? C56B H56B 0.9500 . ? C57B C58B 1.3900 . ? C57B H57B 0.9500 . ? C58B H58B 0.9500 . ? O24 C59 1.259(9) . ? O25 C59 1.253(10) . ? C59 C60 1.498(11) . ? C60 C61 1.389(12) . ? C60 C65 1.405(10) . ? C61 C62 1.377(12) . ? C61 H61 0.9500 . ? C62 C63 1.383(13) . ? C62 H62 0.9500 . ? C63 C64 1.389(14) . ? C63 H63 0.9500 . ? C64 C65 1.402(12) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? O26 C66 1.236(10) . ? O27 C66 1.254(10) . ? C66 C67A 1.506(11) . ? C66 C67B 1.529(14) . ? C67A C68A 1.3900 . ? C67A C72A 1.3900 . ? C68A C69A 1.3900 . ? C68A H68A 0.9500 . ? C69A C70A 1.3900 . ? C69A H69A 0.9500 . ? C70A C71A 1.3900 . ? C70A H70A 0.9500 . ? C71A C72A 1.3900 . ? C71A H71A 0.9500 . ? C72A H72A 0.9500 . ? C67B C68B 1.3900 . ? C67B C72B 1.3900 . ? C68B C69B 1.3900 . ? C68B H68B 0.9500 . ? C69B C70B 1.3900 . ? C69B H69B 0.9500 . ? C70B C71B 1.3900 . ? C70B H70B 0.9500 . ? C71B C72B 1.3900 . ? C71B H71B 0.9500 . ? C72B H72B 0.9500 . ? O28 C73 1.262(9) . ? O29 C73 1.249(9) . ? C73 C74 1.486(11) . ? C74 C79 1.375(13) . ? C74 C75 1.394(11) . ? C75 C76 1.383(13) . ? C75 H75 0.9500 . ? C76 C77 1.345(18) . ? C76 H76 0.9500 . ? C77 C78 1.324(18) . ? C77 H77 0.9500 . ? C78 C79 1.380(16) . ? C78 H78 0.9500 . ? C79 H79 0.9500 . ? N81 C81 1.117(18) . ? C81 C82 1.398(18) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? 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 Yb1 O8 109.61(18) . . ? O4 Yb1 O5 87.08(17) . . ? O8 Yb1 O5 67.60(18) . . ? O4 Yb1 O7 67.37(18) . . ? O8 Yb1 O7 87.4(2) . . ? O5 Yb1 O7 136.05(18) . . ? O4 Yb1 O9 152.2(2) . . ? O8 Yb1 O9 90.3(2) . . ? O5 Yb1 O9 82.8(2) . . ? O7 Yb1 O9 134.9(2) . . ? O4 Yb1 O6 87.4(2) . . ? O8 Yb1 O6 154.1(2) . . ? O5 Yb1 O6 134.6(2) . . ? O7 Yb1 O6 81.3(2) . . ? O9 Yb1 O6 81.6(2) . . ? O4 Yb1 N2 135.2(2) . . ? O8 Yb1 N2 70.7(2) . . ? O5 Yb1 N2 128.7(2) . . ? O7 Yb1 N2 67.9(2) . . ? O9 Yb1 N2 68.9(3) . . ? O6 Yb1 N2 83.5(3) . . ? O4 Yb1 N1 69.91(19) . . ? O8 Yb1 N1 135.0(2) . . ? O5 Yb1 N1 67.48(19) . . ? O7 Yb1 N1 127.99(19) . . ? O9 Yb1 N1 82.3(2) . . ? O6 Yb1 N1 68.4(2) . . ? N2 Yb1 N1 142.4(3) . . ? O10 Yb2 O11 89.21(19) . . ? O10 Yb2 O14 108.75(17) . . ? O11 Yb2 O14 68.33(18) . . ? O10 Yb2 O13 68.64(19) . . ? O11 Yb2 O13 137.21(18) . . ? O14 Yb2 O13 84.26(18) . . ? O10 Yb2 O15 149.9(2) . . ? O11 Yb2 O15 79.6(2) . . ? O14 Yb2 O15 92.99(18) . . ? O13 Yb2 O15 136.06(19) . . ? O10 Yb2 O12 85.61(19) . . ? O11 Yb2 O12 136.1(2) . . ? O14 Yb2 O12 153.3(2) . . ? O13 Yb2 O12 80.16(19) . . ? O15 Yb2 O12 83.52(19) . . ? O10 Yb2 N4 137.4(2) . . ? O11 Yb2 N4 126.3(2) . . ? O14 Yb2 N4 71.4(2) . . ? O13 Yb2 N4 69.1(2) . . ? O15 Yb2 N4 68.5(2) . . ? O12 Yb2 N4 82.7(2) . . ? O10 Yb2 N3 70.6(2) . . ? O11 Yb2 N3 68.97(19) . . ? O14 Yb2 N3 137.3(2) . . ? O13 Yb2 N3 129.5(2) . . ? O15 Yb2 N3 79.3(2) . . ? O12 Yb2 N3 68.2(2) . . ? N4 Yb2 N3 138.7(2) . . ? O4 Fe1 O7 79.5(2) . . ? O4 Fe1 O2 95.8(2) . . ? O7 Fe1 O2 173.0(2) . . ? O4 Fe1 O1 93.9(2) . . ? O7 Fe1 O1 96.7(2) . . ? O2 Fe1 O1 78.3(2) . . ? O4 Fe1 O22 96.3(3) . . ? O7 Fe1 O22 96.1(3) . . ? O2 Fe1 O22 89.6(2) . . ? O1 Fe1 O22 164.8(2) . . ? O4 Fe1 O16 171.8(2) . . ? O7 Fe1 O16 92.3(2) . . ? O2 Fe1 O16 92.2(2) . . ? O1 Fe1 O16 86.1(2) . . ? O22 Fe1 O16 85.3(3) . . ? O10 Fe2 O13 80.7(2) . . ? O10 Fe2 O2 94.6(2) . . ? O13 Fe2 O2 173.1(2) . . ? O10 Fe2 O1 93.5(2) . . ? O13 Fe2 O1 97.4(2) . . ? O2 Fe2 O1 77.7(2) . . ? O10 Fe2 O24 95.6(3) . . ? O13 Fe2 O24 95.7(2) . . ? O2 Fe2 O24 89.8(2) . . ? O1 Fe2 O24 165.1(2) . . ? O10 Fe2 O17 174.0(2) . . ? O13 Fe2 O17 93.3(2) . . ? O2 Fe2 O17 91.3(2) . . ? O1 Fe2 O17 87.2(2) . . ? O24 Fe2 O17 85.0(3) . . ? O5 Fe3 O8 80.2(2) . . ? O5 Fe3 O3 95.8(2) . . ? O8 Fe3 O3 92.8(2) . . ? O5 Fe3 O18 171.7(2) . . ? O8 Fe3 O18 94.7(2) . . ? O3 Fe3 O18 90.9(2) . . ? O5 Fe3 O20 92.8(2) . . ? O8 Fe3 O20 172.9(2) . . ? O3 Fe3 O20 88.9(2) . . ? O18 Fe3 O20 92.2(2) . . ? O5 Fe3 O26 90.6(2) . . ? O8 Fe3 O26 93.5(2) . . ? O3 Fe3 O26 171.7(2) . . ? O18 Fe3 O26 83.2(2) . . ? O20 Fe3 O26 85.5(2) . . ? O11 Fe4 O14 80.5(2) . . ? O11 Fe4 O3 93.4(2) . . ? O14 Fe4 O3 96.9(2) . . ? O11 Fe4 O21 93.4(2) . . ? O14 Fe4 O21 172.1(2) . . ? O3 Fe4 O21 88.4(2) . . ? O11 Fe4 O28 95.0(2) . . ? O14 Fe4 O28 91.7(2) . . ? O3 Fe4 O28 168.9(2) . . ? O21 Fe4 O28 83.8(3) . . ? O11 Fe4 O19 173.4(2) . . ? O14 Fe4 O19 93.0(2) . . ? O3 Fe4 O19 88.6(2) . . ? O21 Fe4 O19 92.9(2) . . ? O28 Fe4 O19 83.9(2) . . ? C1 O1 Fe2 121.5(4) . . ? C1 O1 Fe1 120.6(4) . . ? Fe2 O1 Fe1 99.0(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 O2 Fe1 128.7(6) . . ? C2 O2 Fe2 126.4(5) . . ? Fe1 O2 Fe2 100.7(2) . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Fe3 O3 Fe4 126.5(3) . . ? Fe3 O3 H3 122(5) . . ? Fe4 O3 H3 111(5) . . ? C7 N1 C3 110.7(7) . . ? C7 N1 C5 109.6(7) . . ? C3 N1 C5 112.0(7) . . ? C7 N1 Yb1 108.4(6) . . ? C3 N1 Yb1 109.3(5) . . ? C5 N1 Yb1 106.8(4) . . ? N1 C3 C4 113.6(7) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? O4 C4 C3 109.8(7) . . ? O4 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? Yb1 C4 H4A 95.0 . . ? O4 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? Yb1 C4 H4B 146.4 . . ? H4A C4 H4B 108.2 . . ? C4 O4 Fe1 132.9(4) . . ? C4 O4 Yb1 119.3(4) . . ? Fe1 O4 Yb1 107.8(2) . . ? N1 C5 C6 109.8(6) . . ? N1 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? N1 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O5 C6 C5 108.9(7) . . ? O5 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? O5 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C6 O5 Fe3 127.5(4) . . ? C6 O5 Yb1 126.1(4) . . ? Fe3 O5 Yb1 106.1(2) . . ? N1 C7 C8 112.8(9) . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O6 C8 C7 109.1(9) . . ? O6 C8 C9A 117.7(13) . . ? C7 C8 C9A 117.9(14) . . ? O6 C8 C9B 102.5(13) . . ? C7 C8 C9B 104.5(14) . . ? O6 C8 H8A 103.2 . . ? C7 C8 H8A 103.2 . . ? C9A C8 H8A 103.2 . . ? O6 C8 H8B 112.9 . . ? C7 C8 H8B 112.5 . . ? C9B C8 H8B 114.6 . . ? C8 C9A H9A1 109.5 . . ? C8 C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8 C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C8 C9B H9B1 109.5 . . ? C8 C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C8 C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C8 O6 Yb1 122.1(6) . . ? C8 O6 H6 117(7) . . ? Yb1 O6 H6 105(7) . . ? C12 N2 C10 112.6(11) . . ? C12 N2 C14 111.8(12) . . ? C10 N2 C14 107.1(9) . . ? C12 N2 Yb1 109.3(6) . . ? C10 N2 Yb1 107.7(5) . . ? C14 N2 Yb1 108.2(7) . . ? N2 C10 C11 111.0(8) . . ? N2 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N2 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? O7 C11 C10 107.4(8) . . ? O7 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? O7 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 O7 Fe1 128.4(6) . . ? C11 O7 Yb1 126.1(5) . . ? Fe1 O7 Yb1 105.2(2) . . ? C13 C12 N2 118.5(9) . . ? C13 C12 H12A 107.7 . . ? N2 C12 H12A 107.7 . . ? C13 C12 H12B 107.7 . . ? N2 C12 H12B 107.7 . . ? H12A C12 H12B 107.1 . . ? O8 C13 C12 117.6(9) . . ? O8 C13 H13A 107.9 . . ? C12 C13 H13A 107.9 . . ? O8 C13 H13B 107.9 . . ? C12 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? C13 O8 Fe3 131.2(6) . . ? C13 O8 Yb1 120.1(5) . . ? Fe3 O8 Yb1 106.0(2) . . ? C15 C14 N2 112.2(11) . . ? C15 C14 H14A 109.2 . . ? N2 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? N2 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? O9 C15 C14 114.4(11) . . ? O9 C15 C16 110.6(14) . . ? C14 C15 C16 112.2(14) . . ? O9 C15 H15A 106.3 . . ? C14 C15 H15A 106.3 . . ? C16 C15 H15A 106.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 O9 Yb1 120.9(8) . . ? C15 O9 H9 91(6) . . ? Yb1 O9 H9 125(6) . . ? C19 N3 C17 111.4(7) . . ? C19 N3 C21 109.7(7) . . ? C17 N3 C21 113.6(7) . . ? C19 N3 Yb2 106.8(4) . . ? C17 N3 Yb2 108.5(5) . . ? C21 N3 Yb2 106.4(6) . . ? C18A C17 N3 112.9(9) . . ? N3 C17 C18B 118.2(10) . . ? C18A C17 H17A 109.0 . . ? N3 C17 H17A 109.0 . . ? C18A C17 H17B 109.0 . . ? N3 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N3 C17 H17C 107.8 . . ? C18B C17 H17C 107.8 . . ? N3 C17 H17D 107.8 . . ? C18B C17 H17D 107.8 . . ? H17C C17 H17D 107.1 . . ? O10 C18A C17 113.8(12) . . ? O10 C18A H18A 108.8 . . ? C17 C18A H18A 108.8 . . ? O10 C18A H18B 108.8 . . ? C17 C18A H18B 108.8 . . ? H18A C18A H18B 107.7 . . ? O10 C18B C17 107.7(12) . . ? O10 C18B H18C 110.2 . . ? C17 C18B H18C 110.2 . . ? O10 C18B H18D 110.2 . . ? C17 C18B H18D 110.2 . . ? H18C C18B H18D 108.5 . . ? C18A O10 Fe2 137.6(7) . . ? C18B O10 Fe2 114.7(8) . . ? C18A O10 Yb2 116.5(7) . . ? C18B O10 Yb2 121.8(7) . . ? Fe2 O10 Yb2 105.9(2) . . ? N3 C19 C20 112.1(7) . . ? N3 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N3 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? O11 C20 C19 108.7(7) . . ? O11 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? O11 C20 H20B 110.0 . . ? C19 C20 H20B 110.0 . . ? H20A C20 H20B 108.3 . . ? C20 O11 Fe4 129.0(4) . . ? C20 O11 Yb2 125.2(4) . . ? Fe4 O11 Yb2 105.8(2) . . ? C22 C21 N3 112.3(7) . . ? C22 C21 H21A 109.1 . . ? N3 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? N3 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? O12 C22 C21 109.0(7) . . ? O12 C22 C23 110.8(9) . . ? C21 C22 C23 112.5(9) . . ? O12 C22 H22 108.1 . . ? C21 C22 H22 108.1 . . ? C23 C22 H22 108.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 O12 Yb2 123.4(5) . . ? C22 O12 H12 106(6) . . ? Yb2 O12 H12 123(6) . . ? C26 N4 C24 113.7(7) . . ? C26 N4 C28 112.1(7) . . ? C24 N4 C28 109.2(7) . . ? C26 N4 Yb2 108.7(5) . . ? C24 N4 Yb2 106.4(5) . . ? C28 N4 Yb2 106.2(6) . . ? N4 C24 C25 112.4(6) . . ? N4 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? N4 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? O13 C25 C24 109.1(7) . . ? O13 C25 H25A 109.9 . . ? C24 C25 H25A 109.9 . . ? O13 C25 H25B 109.9 . . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C25 O13 Fe2 131.1(5) . . ? C25 O13 Yb2 124.9(4) . . ? Fe2 O13 Yb2 104.0(2) . . ? N4 C26 C27 115.9(7) . . ? N4 C26 H26A 108.3 . . ? C27 C26 H26A 108.3 . . ? N4 C26 H26B 108.3 . . ? C27 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? O14 C27 C26 112.0(7) . . ? O14 C27 H27A 109.2 . . ? C26 C27 H27A 109.2 . . ? O14 C27 H27B 109.2 . . ? C26 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 O14 Fe4 130.0(5) . . ? C27 O14 Yb2 119.7(5) . . ? Fe4 O14 Yb2 105.4(2) . . ? C29 C28 N4 111.6(8) . . ? C29 C28 H28A 109.3 . . ? N4 C28 H28A 109.3 . . ? C29 C28 H28B 109.3 . . ? N4 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? O15 C29 C28 110.4(8) . . ? O15 C29 C30 113.6(9) . . ? C28 C29 C30 113.0(9) . . ? O15 C29 H29 106.4 . . ? C28 C29 H29 106.4 . . ? C30 C29 H29 106.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 O15 Yb2 122.9(5) . . ? C29 O15 H15 96(6) . . ? Yb2 O15 H15 104(6) . . ? C31 O16 Fe1 128.5(6) . . ? C31 O17 Fe2 127.6(5) . . ? O16 C31 O17 126.0(8) . . ? O16 C31 C32 116.8(8) . . ? O17 C31 C32 117.2(8) . . ? C37 C32 C33 120.1(9) . . ? C37 C32 C31 120.2(9) . . ? C33 C32 C31 119.6(9) . . ? C34 C33 C32 119.2(10) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C33 119.6(10) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C36 C35 C34 121.4(10) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 117.8(10) . . ? C35 C36 H36 121.1 . . ? C37 C36 H36 121.1 . . ? C32 C37 C36 121.8(10) . . ? C32 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C38 O18 Fe3 135.1(4) . . ? C38 O19 Fe4 132.3(5) . . ? O19 C38 O18 126.7(6) . . ? O19 C38 C39 117.5(7) . . ? O18 C38 C39 115.8(6) . . ? C40 C39 C44 119.7(7) . . ? C40 C39 C38 121.1(7) . . ? C44 C39 C38 119.2(7) . . ? C39 C40 C41 120.7(8) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C40 C41 C42 118.6(7) . . ? C40 C41 H41 120.7 . . ? C42 C41 H41 120.7 . . ? C43 C42 C41 119.8(7) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 122.0(8) . . ? C42 C43 H43 119.0 . . ? C44 C43 H43 119.0 . . ? C43 C44 C39 119.1(7) . . ? C43 C44 H44 120.5 . . ? C39 C44 H44 120.5 . . ? C45 O20 Fe3 130.8(6) . . ? C45 O21 Fe4 137.7(5) . . ? O20 C45 O21 126.5(8) . . ? O20 C45 C46A 120.4(8) . . ? O21 C45 C46A 113.0(7) . . ? O20 C45 C46B 103.0(11) . . ? O21 C45 C46B 130.0(11) . . ? C47A C46A C51A 120.0 . . ? C47A C46A C45 120.9(6) . . ? C51A C46A C45 118.9(6) . . ? C46A C47A C48A 120.0 . . ? C46A C47A H47A 120.0 . . ? C48A C47A H47A 120.0 . . ? C49A C48A C47A 120.0 . . ? C49A C48A H48A 120.0 . . ? C47A C48A H48A 120.0 . . ? C48A C49A C50A 120.0 . . ? C48A C49A H49A 120.0 . . ? C50A C49A H49A 120.0 . . ? C51A C50A C49A 120.0 . . ? C51A C50A H50A 120.0 . . ? C49A C50A H50A 120.0 . . ? C50A C51A C46A 120.0 . . ? C50A C51A H51A 120.0 . . ? C46A C51A H51A 120.0 . . ? C47B C46B C51B 120.0 . . ? C47B C46B C45 112.2(16) . . ? C51B C46B C45 127.0(16) . . ? C46B C47B C48B 120.0 . . ? C46B C47B H47B 120.0 . . ? C48B C47B H47B 120.0 . . ? C49B C48B C47B 120.0 . . ? C49B C48B H48B 120.0 . . ? C47B C48B H48B 120.0 . . ? C48B C49B C50B 120.0 . . ? C48B C49B H49B 120.0 . . ? C50B C49B H49B 120.0 . . ? C51B C50B C49B 120.0 . . ? C51B C50B H50B 120.0 . . ? C49B C50B H50B 120.0 . . ? C50B C51B C46B 120.0 . . ? C50B C51B H51B 120.0 . . ? C46B C51B H51B 120.0 . . ? C52B O22 Fe1 139.9(19) . . ? C52A O22 Fe1 133.5(11) . . ? O23A C52A O22 129.1(17) . . ? O23A C52A C53A 113.5(12) . . ? O22 C52A C53A 117.1(16) . . ? C54A C53A C58A 120.0 . . ? C54A C53A C52A 121.3(11) . . ? C58A C53A C52A 118.6(11) . . ? C55A C54A C53A 120.0 . . ? C55A C54A H54A 120.0 . . ? C53A C54A H54A 120.0 . . ? C54A C55A C56A 120.0 . . ? C54A C55A H55A 120.0 . . ? C56A C55A H55A 120.0 . . ? C57A C56A C55A 120.0 . . ? C57A C56A H56A 120.0 . . ? C55A C56A H56A 120.0 . . ? C58A C57A C56A 120.0 . . ? C58A C57A H57A 120.0 . . ? C56A C57A H57A 120.0 . . ? C57A C58A C53A 120.0 . . ? C57A C58A H58A 120.0 . . ? C53A C58A H58A 120.0 . . ? O23B C52B O22 119(2) . . ? O23B C52B C53B 124.7(18) . . ? O22 C52B C53B 115.4(19) . . ? C54B C53B C58B 120.0 . . ? C54B C53B C52B 117.2(14) . . ? C58B C53B C52B 122.8(14) . . ? C53B C54B C55B 120.0 . . ? C53B C54B H54B 120.0 . . ? C55B C54B H54B 120.0 . . ? C54B C55B C56B 120.0 . . ? C54B C55B H55B 120.0 . . ? C56B C55B H55B 120.0 . . ? C55B C56B C57B 120.0 . . ? C55B C56B H56B 120.0 . . ? C57B C56B H56B 120.0 . . ? C58B C57B C56B 120.0 . . ? C58B C57B H57B 120.0 . . ? C56B C57B H57B 120.0 . . ? C57B C58B C53B 120.0 . . ? C57B C58B H58B 120.0 . . ? C53B C58B H58B 120.0 . . ? C59 O24 Fe2 140.8(6) . . ? O25 C59 O24 125.4(8) . . ? O25 C59 C60 119.3(7) . . ? O24 C59 C60 115.3(7) . . ? C61 C60 C65 119.7(7) . . ? C61 C60 C59 120.6(7) . . ? C65 C60 C59 119.7(8) . . ? C62 C61 C60 121.4(8) . . ? C62 C61 H61 119.3 . . ? C60 C61 H61 119.3 . . ? C61 C62 C63 119.3(9) . . ? C61 C62 H62 120.4 . . ? C63 C62 H62 120.4 . . ? C62 C63 C64 120.7(8) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C65 120.3(8) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C64 C65 C60 118.6(9) . . ? C64 C65 H65 120.7 . . ? C60 C65 H65 120.7 . . ? C66 O26 Fe3 133.3(5) . . ? O26 C66 O27 124.9(8) . . ? O26 C66 C67A 113.3(8) . . ? O27 C66 C67A 121.7(8) . . ? O26 C66 C67B 127.1(10) . . ? O27 C66 C67B 108.0(10) . . ? C68A C67A C72A 120.0 . . ? C68A C67A C66 117.6(7) . . ? C72A C67A C66 122.4(7) . . ? C69A C68A C67A 120.0 . . ? C69A C68A H68A 120.0 . . ? C67A C68A H68A 120.0 . . ? C70A C69A C68A 120.0 . . ? C70A C69A H69A 120.0 . . ? C68A C69A H69A 120.0 . . ? C69A C70A C71A 120.0 . . ? C69A C70A H70A 120.0 . . ? C71A C70A H70A 120.0 . . ? C72A C71A C70A 120.0 . . ? C72A C71A H71A 120.0 . . ? C70A C71A H71A 120.0 . . ? C71A C72A C67A 120.0 . . ? C71A C72A H72A 120.0 . . ? C67A C72A H72A 120.0 . . ? C68B C67B C72B 120.0 . . ? C68B C67B C66 126.3(12) . . ? C72B C67B C66 113.7(12) . . ? C67B C68B C69B 120.0 . . ? C67B C68B H68B 120.0 . . ? C69B C68B H68B 120.0 . . ? C68B C69B C70B 120.0 . . ? C68B C69B H69B 120.0 . . ? C70B C69B H69B 120.0 . . ? C71B C70B C69B 120.0 . . ? C71B C70B H70B 120.0 . . ? C69B C70B H70B 120.0 . . ? C70B C71B C72B 120.0 . . ? C70B C71B H71B 120.0 . . ? C72B C71B H71B 120.0 . . ? C71B C72B C67B 120.0 . . ? C71B C72B H72B 120.0 . . ? C67B C72B H72B 120.0 . . ? C73 O28 Fe4 133.5(6) . . ? O29 C73 O28 124.0(8) . . ? O29 C73 C74 118.4(7) . . ? O28 C73 C74 117.6(7) . . ? C79 C74 C75 118.6(9) . . ? C79 C74 C73 121.2(8) . . ? C75 C74 C73 120.2(8) . . ? C76 C75 C74 119.0(10) . . ? C76 C75 H75 120.5 . . ? C74 C75 H75 120.5 . . ? C77 C76 C75 121.0(11) . . ? C77 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? C78 C77 C76 119.9(11) . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C79 121.6(13) . . ? C77 C78 H78 119.2 . . ? C79 C78 H78 119.2 . . ? C74 C79 C78 119.2(11) . . ? C74 C79 H79 120.4 . . ? C78 C79 H79 120.4 . . ? N81 C81 C82 175(2) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 O23A 0.93(4) 1.60(7) 2.448(17) 149(10) . O6 H6 O23B 0.93(4) 1.95(6) 2.84(2) 159(10) . O9 H9 O27 0.93(4) 1.70(5) 2.579(9) 157(10) . O12 H12 O25 0.91(4) 1.71(5) 2.597(8) 164(9) . O15 H15 O29 0.93(4) 1.76(6) 2.569(8) 144(8) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.142 _refine_diff_density_min -4.213 _refine_diff_density_rms 0.177 _database_code_depnum_ccdc_archive 'CCDC 912846' ####################################################################### # # 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_ambf3yb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H91 Fe3 N4 O25 Yb2, C2 H3 N' _chemical_formula_sum 'C72 H94 Fe3 N5 O25 Yb2' _chemical_formula_weight 1943.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 19.9227(15) _cell_length_b 19.6790(12) _cell_length_c 22.0382(15) _cell_angle_alpha 90.00 _cell_angle_beta 108.184(8) _cell_angle_gamma 90.00 _cell_volume 8208.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.87 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3916 _exptl_absorpt_coefficient_mu 2.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 0.598 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Stoe IPDS' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47608 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_unetI/netI 0.0840 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.96 _reflns_number_total 15902 _reflns_number_gt 9349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_cell_refinement 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_data_reduction 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. Three of the ligands were partly disordered. They were modelled with isotropic partial occupancy carbon atoms as appropriate, using geometrical similarity restraints: SAME C5A C6A C7A O4 SADI N2 C12A N2 C12B SAME C12A C13A C14A O7 SADI N3 C19A N3 C19B SAME C19A C20A C21A O10 The isotropic U of closely separated disordered patial atoms were restrained to be similar: SIMU 0.03 C7A C7B SIMU 0.03 C14A C14B O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4 O7 H7 O10 H10 O13 H13 DFIX 1.54 0.04 H7 O21 H4 O19 H10 O23 The H atoms on O(4), O(7) and O(10) could not be resolved into disorder components. ; _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^)+(0.0796P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15902 _refine_ls_number_parameters 971 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.982 _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 Yb1 Yb 0.15810(2) 0.07888(2) 0.211532(17) 0.05026(12) Uani 1 1 d . A . Yb2 Yb 0.36312(2) 0.15036(2) 0.085187(16) 0.04691(11) Uani 1 1 d . C . Fe1 Fe 0.30786(6) -0.01122(6) 0.27278(5) 0.0455(3) Uani 1 1 d . . . Fe2 Fe 0.41501(7) 0.00719(6) 0.17209(5) 0.0466(3) Uani 1 1 d . . . Fe3 Fe 0.20033(7) 0.18376(7) 0.10367(6) 0.0523(3) Uani 1 1 d . . . O1 O 0.3317(3) 0.0293(3) 0.1996(3) 0.0506(14) Uani 1 1 d D . . H1 H 0.311(5) 0.069(3) 0.190(4) 0.061 Uiso 1 1 d D . . N1 N 0.1620(5) 0.1608(4) 0.3020(4) 0.067(2) Uani 1 1 d D . . C1 C 0.1304(9) 0.2264(6) 0.2707(6) 0.099(5) Uani 1 1 d . A . H1A H 0.0784 0.2215 0.2535 0.118 Uiso 1 1 calc R . . H1B H 0.1410 0.2630 0.3030 0.118 Uiso 1 1 calc R . . C2 C 0.1589(7) 0.2457(6) 0.2173(5) 0.078(3) Uani 1 1 d . . . H2A H 0.1245 0.2758 0.1870 0.094 Uiso 1 1 calc R A . H2B H 0.2034 0.2716 0.2352 0.094 Uiso 1 1 calc R . . O2 O 0.1722(3) 0.1883(3) 0.1841(3) 0.0525(14) Uani 1 1 d . A . C3 C 0.2368(7) 0.1731(7) 0.3403(6) 0.092(4) Uani 1 1 d . A . H3A H 0.2387 0.1891 0.3833 0.111 Uiso 1 1 calc R . . H3B H 0.2565 0.2093 0.3197 0.111 Uiso 1 1 calc R . . C4 C 0.2813(6) 0.1103(6) 0.3466(4) 0.071(3) Uani 1 1 d . . . H4A H 0.3319 0.1228 0.3627 0.085 Uiso 1 1 calc R A . H4B H 0.2713 0.0790 0.3778 0.085 Uiso 1 1 calc R . . O3 O 0.2670(3) 0.0773(3) 0.2869(2) 0.0492(14) Uani 1 1 d . A . C5A C 0.1253(10) 0.1322(8) 0.3468(8) 0.066(5) Uiso 0.62 1 d PD A 1 H5A1 H 0.1037 0.1695 0.3644 0.079 Uiso 0.62 1 calc PR A 1 H5A2 H 0.1601 0.1088 0.3828 0.079 Uiso 0.62 1 calc PR A 1 C6A C 0.0682(9) 0.0821(8) 0.3108(8) 0.068(4) Uiso 0.62 1 d PD A 1 H6A H 0.0358 0.1073 0.2737 0.082 Uiso 0.62 1 calc PR A 1 C7A C 0.025(2) 0.054(2) 0.345(2) 0.19(2) Uiso 0.62 1 d PDU A 1 H7A1 H -0.0093 0.0227 0.3176 0.286 Uiso 0.62 1 calc PR A 1 H7A2 H 0.0008 0.0901 0.3601 0.286 Uiso 0.62 1 calc PR A 1 H7A3 H 0.0554 0.0285 0.3824 0.286 Uiso 0.62 1 calc PR A 1 C5B C 0.0982(16) 0.1433(12) 0.3226(19) 0.091(11) Uiso 0.38 1 d PD A 2 H5B1 H 0.0544 0.1528 0.2872 0.109 Uiso 0.38 1 calc PR A 2 H5B2 H 0.0980 0.1718 0.3595 0.109 Uiso 0.38 1 calc PR A 2 C6B C 0.1001(17) 0.0686(13) 0.3409(13) 0.089(10) Uiso 0.38 1 d PD A 2 H6B H 0.1443 0.0608 0.3773 0.106 Uiso 0.38 1 calc PR A 2 C7B C 0.0417(16) 0.0473(14) 0.3611(15) 0.063(8) Uiso 0.38 1 d PDU A 2 H7B1 H 0.0468 -0.0011 0.3722 0.095 Uiso 0.38 1 calc PR A 2 H7B2 H -0.0024 0.0545 0.3263 0.095 Uiso 0.38 1 calc PR A 2 H7B3 H 0.0409 0.0737 0.3985 0.095 Uiso 0.38 1 calc PR A 2 O4 O 0.1068(4) 0.0298(4) 0.2837(3) 0.073(2) Uani 1 1 d D . . H4 H 0.130(5) -0.008(4) 0.315(4) 0.088 Uiso 1 1 d D B 1 N2 N 0.3270(5) 0.1079(5) -0.0292(3) 0.064(2) Uani 1 1 d D . . C8 C 0.2660(6) 0.1511(6) -0.0663(4) 0.071(3) Uani 1 1 d . C . H8A H 0.2443 0.1311 -0.1092 0.085 Uiso 1 1 calc R . . H8B H 0.2832 0.1972 -0.0719 0.085 Uiso 1 1 calc R . . C9 C 0.2108(5) 0.1563(6) -0.0319(4) 0.064(3) Uani 1 1 d . . . H9A H 0.1809 0.1968 -0.0474 0.077 Uiso 1 1 calc R C . H9B H 0.1800 0.1157 -0.0416 0.077 Uiso 1 1 calc R . . O5 O 0.2435(3) 0.1613(3) 0.0348(2) 0.0505(14) Uani 1 1 d . C . C10 C 0.3053(8) 0.0365(6) -0.0295(4) 0.092(4) Uani 1 1 d . C . H10A H 0.3086 0.0146 -0.0689 0.110 Uiso 1 1 calc R . . H10B H 0.2552 0.0351 -0.0309 0.110 Uiso 1 1 calc R . . C11 C 0.3483(7) -0.0038(5) 0.0270(4) 0.074(3) Uani 1 1 d . . . H11A H 0.3237 -0.0468 0.0297 0.088 Uiso 1 1 calc R C . H11B H 0.3947 -0.0152 0.0218 0.088 Uiso 1 1 calc R . . O6 O 0.3586(3) 0.0344(3) 0.0836(2) 0.0490(13) Uani 1 1 d . C . C12A C 0.3900(8) 0.1032(10) -0.0532(8) 0.048(4) Uiso 0.50 1 d PD C 1 H12A H 0.4141 0.0590 -0.0406 0.058 Uiso 0.50 1 calc PR C 1 H12B H 0.3744 0.1063 -0.1004 0.058 Uiso 0.50 1 calc PR C 1 C13A C 0.4398(9) 0.1605(9) -0.0247(6) 0.047(4) Uiso 0.50 1 d PD C 1 H13A H 0.4130 0.2041 -0.0348 0.056 Uiso 0.50 1 calc PR C 1 C14A C 0.5016(16) 0.165(2) -0.0477(16) 0.117(16) Uiso 0.50 1 d PDU C 1 H14A H 0.5304 0.2046 -0.0278 0.175 Uiso 0.50 1 calc PR C 1 H14B H 0.4856 0.1710 -0.0942 0.175 Uiso 0.50 1 calc PR C 1 H14C H 0.5299 0.1238 -0.0364 0.175 Uiso 0.50 1 calc PR C 1 C12B C 0.3825(9) 0.1348(14) -0.0590(9) 0.073(6) Uiso 0.50 1 d PD C 2 H12C H 0.3756 0.1115 -0.1004 0.088 Uiso 0.50 1 calc PR C 2 H12D H 0.3743 0.1839 -0.0678 0.088 Uiso 0.50 1 calc PR C 2 C13B C 0.4569(11) 0.1246(13) -0.0180(8) 0.077(6) Uiso 0.50 1 d PD C 2 H13B H 0.4644 0.0743 -0.0141 0.093 Uiso 0.50 1 calc PR C 2 C14B C 0.5138(14) 0.1518(17) -0.0400(12) 0.076(9) Uiso 0.50 1 d PDU C 2 H14D H 0.5594 0.1436 -0.0075 0.115 Uiso 0.50 1 calc PR C 2 H14E H 0.5070 0.2008 -0.0474 0.115 Uiso 0.50 1 calc PR C 2 H14F H 0.5130 0.1293 -0.0799 0.115 Uiso 0.50 1 calc PR C 2 O7 O 0.4618(4) 0.1495(4) 0.0471(3) 0.0627(17) Uani 1 1 d D . . H7 H 0.495(4) 0.111(4) 0.061(4) 0.075 Uiso 1 1 d D D 1 N3 N 0.0811(4) -0.0075(5) 0.1310(4) 0.073(2) Uani 1 1 d D . . C15 C 0.0964(8) 0.0006(8) 0.0716(5) 0.109(5) Uani 1 1 d . A . H15A H 0.0601 0.0307 0.0434 0.131 Uiso 1 1 calc R . . H15B H 0.0920 -0.0444 0.0505 0.131 Uiso 1 1 calc R . . C16 C 0.1685(7) 0.0294(6) 0.0771(5) 0.078(3) Uani 1 1 d . . . H16A H 0.2048 -0.0063 0.0926 0.093 Uiso 1 1 calc R A . H16B H 0.1694 0.0443 0.0344 0.093 Uiso 1 1 calc R . . O8 O 0.1846(3) 0.0854(3) 0.1198(2) 0.0557(15) Uani 1 1 d . A . C17 C 0.0971(6) -0.0760(5) 0.1613(5) 0.067(3) Uani 1 1 d . A . H17A H 0.0758 -0.1115 0.1293 0.080 Uiso 1 1 calc R . . H17B H 0.0762 -0.0799 0.1964 0.080 Uiso 1 1 calc R . . C18 C 0.1765(5) -0.0867(5) 0.1873(5) 0.066(3) Uani 1 1 d . . . H18A H 0.1872 -0.1266 0.2161 0.079 Uiso 1 1 calc R A . H18B H 0.1960 -0.0951 0.1518 0.079 Uiso 1 1 calc R . . O9 O 0.2075(3) -0.0270(3) 0.2215(3) 0.0501(14) Uani 1 1 d . A . C19A C 0.0040(9) 0.0053(9) 0.1284(12) 0.077(6) Uiso 0.62 1 d PD A 1 H19A H -0.0279 -0.0232 0.0946 0.092 Uiso 0.62 1 calc PR A 1 H19B H -0.0023 -0.0078 0.1697 0.092 Uiso 0.62 1 calc PR A 1 C20A C -0.0151(10) 0.0792(9) 0.1150(9) 0.080(5) Uiso 0.62 1 d PD A 1 H20A H -0.0124 0.0909 0.0717 0.096 Uiso 0.62 1 calc PR A 1 C21A C -0.0895(11) 0.0939(13) 0.1168(14) 0.111(9) Uiso 0.62 1 d PD A 1 H21A H -0.0966 0.1432 0.1171 0.167 Uiso 0.62 1 calc PR A 1 H21B H -0.0957 0.0739 0.1554 0.167 Uiso 0.62 1 calc PR A 1 H21C H -0.1240 0.0742 0.0790 0.167 Uiso 0.62 1 calc PR A 1 C19B C 0.0032(12) 0.0126(18) 0.106(2) 0.118(19) Uiso 0.38 1 d PD A 2 H19C H -0.0072 0.0341 0.0632 0.142 Uiso 0.38 1 calc PR A 2 H19D H -0.0271 -0.0281 0.1016 0.142 Uiso 0.38 1 calc PR A 2 C20B C -0.0111(17) 0.0613(16) 0.152(2) 0.128(15) Uiso 0.38 1 d PD A 2 H20B H 0.0029 0.0358 0.1931 0.153 Uiso 0.38 1 calc PR A 2 C21B C -0.0865(17) 0.083(2) 0.143(3) 0.132(19) Uiso 0.38 1 d PD A 2 H21D H -0.0879 0.1322 0.1497 0.198 Uiso 0.38 1 calc PR A 2 H21E H -0.1039 0.0593 0.1745 0.198 Uiso 0.38 1 calc PR A 2 H21F H -0.1164 0.0715 0.1000 0.198 Uiso 0.38 1 calc PR A 2 O10 O 0.0393(3) 0.1183(5) 0.1636(4) 0.081(2) Uani 1 1 d D . . H10 H 0.028(7) 0.159(4) 0.134(5) 0.097 Uiso 1 1 d D E 1 N4 N 0.4364(5) 0.2404(4) 0.1620(4) 0.068(2) Uani 1 1 d . . . C22 C 0.3927(6) 0.2640(6) 0.2017(5) 0.073(3) Uani 1 1 d . C . H22A H 0.3645 0.3037 0.1805 0.088 Uiso 1 1 calc R . . H22B H 0.4246 0.2794 0.2435 0.088 Uiso 1 1 calc R . . C23 C 0.3434(6) 0.2110(6) 0.2129(4) 0.071(3) Uani 1 1 d . . . H23A H 0.3710 0.1763 0.2430 0.085 Uiso 1 1 calc R C . H23B H 0.3102 0.2325 0.2325 0.085 Uiso 1 1 calc R . . O11 O 0.3040(3) 0.1788(3) 0.1533(2) 0.0541(15) Uani 1 1 d . C . C24 C 0.5035(6) 0.2078(6) 0.2003(5) 0.069(3) Uani 1 1 d . C . H24A H 0.5274 0.2376 0.2368 0.083 Uiso 1 1 calc R . . H24B H 0.5350 0.2034 0.1735 0.083 Uiso 1 1 calc R . . C25 C 0.4931(5) 0.1394(5) 0.2249(4) 0.065(3) Uani 1 1 d . . . H25A H 0.5385 0.1144 0.2390 0.078 Uiso 1 1 calc R C . H25B H 0.4751 0.1439 0.2618 0.078 Uiso 1 1 calc R . . O12 O 0.4430(3) 0.1035(3) 0.1739(2) 0.0493(14) Uani 1 1 d . C . C26 C 0.4536(8) 0.2958(6) 0.1230(6) 0.086(4) Uani 1 1 d . C . H26A H 0.4706 0.3357 0.1510 0.103 Uiso 1 1 calc R . . H26B H 0.4929 0.2803 0.1079 0.103 Uiso 1 1 calc R . . C27 C 0.3954(9) 0.3176(6) 0.0677(7) 0.097(4) Uani 1 1 d . . . H27A H 0.3647 0.3478 0.0843 0.116 Uiso 1 1 calc R C . C28 C 0.4178(9) 0.3590(6) 0.0194(6) 0.098(4) Uani 1 1 d . C . H28A H 0.3759 0.3720 -0.0159 0.147 Uiso 1 1 calc R . . H28B H 0.4493 0.3318 0.0027 0.147 Uiso 1 1 calc R . . H28C H 0.4426 0.4000 0.0400 0.147 Uiso 1 1 calc R . . O13 O 0.3526(4) 0.2595(3) 0.0388(3) 0.0689(19) Uani 1 1 d D C . H13 H 0.309(4) 0.282(5) 0.023(5) 0.083 Uiso 1 1 d D . . O14 O 0.3399(4) -0.1040(3) 0.2468(3) 0.0565(15) Uani 1 1 d . . . O15 O 0.3848(3) -0.0933(3) 0.1642(3) 0.0545(15) Uani 1 1 d . . . C29 C 0.3566(5) -0.1259(5) 0.1984(4) 0.054(2) Uani 1 1 d . . . C30 C 0.3405(5) -0.2009(5) 0.1837(4) 0.054(2) Uani 1 1 d . . . C31 C 0.3575(6) -0.2312(6) 0.1334(5) 0.074(3) Uani 1 1 d . . . H31A H 0.3776 -0.2047 0.1074 0.089 Uiso 1 1 calc R . . C32 C 0.3450(8) -0.3007(7) 0.1209(8) 0.100(4) Uani 1 1 d . . . H32A H 0.3555 -0.3215 0.0861 0.120 Uiso 1 1 calc R . . C33 C 0.3165(8) -0.3395(6) 0.1611(8) 0.096(4) Uani 1 1 d . . . H33A H 0.3089 -0.3868 0.1537 0.115 Uiso 1 1 calc R . . C34 C 0.2995(7) -0.3095(6) 0.2109(7) 0.087(4) Uani 1 1 d . . . H34A H 0.2796 -0.3356 0.2373 0.104 Uiso 1 1 calc R . . C35 C 0.3118(5) -0.2400(5) 0.2220(5) 0.064(3) Uani 1 1 d . . . H35A H 0.3004 -0.2191 0.2563 0.076 Uiso 1 1 calc R . . O16 O 0.4072(3) 0.0096(3) 0.3329(3) 0.0529(15) Uani 1 1 d . . . O17 O 0.4736(3) -0.0074(3) 0.2673(3) 0.0531(14) Uani 1 1 d . . . C36 C 0.4662(5) 0.0053(4) 0.3211(4) 0.048(2) Uani 1 1 d . . . C37 C 0.5324(5) 0.0161(4) 0.3760(4) 0.0473(19) Uani 1 1 d . . . C38 C 0.5975(5) 0.0020(5) 0.3685(4) 0.058(2) Uani 1 1 d . . . H38A H 0.5998 -0.0131 0.3283 0.069 Uiso 1 1 calc R . . C39 C 0.6599(5) 0.0098(6) 0.4192(4) 0.067(3) Uani 1 1 d . . . H39A H 0.7040 0.0000 0.4131 0.080 Uiso 1 1 calc R . . C40 C 0.6578(6) 0.0316(6) 0.4783(5) 0.070(3) Uani 1 1 d . . . H40A H 0.7003 0.0361 0.5129 0.084 Uiso 1 1 calc R . . C41 C 0.5919(6) 0.0473(6) 0.4867(4) 0.068(3) Uani 1 1 d . . . H41A H 0.5897 0.0631 0.5268 0.082 Uiso 1 1 calc R . . C42 C 0.5299(5) 0.0392(5) 0.4352(4) 0.058(2) Uani 1 1 d . . . H42A H 0.4855 0.0495 0.4406 0.069 Uiso 1 1 calc R . . O18 O 0.2936(4) -0.0590(3) 0.3497(3) 0.0605(16) Uani 1 1 d . . . O19 O 0.1842(4) -0.0646(5) 0.3597(4) 0.085(2) Uani 1 1 d D . . C43 C 0.2450(6) -0.0900(6) 0.3654(5) 0.065(3) Uani 1 1 d . . . C44 C 0.2633(6) -0.1602(6) 0.3923(5) 0.070(3) Uani 1 1 d . . . C45 C 0.3237(8) -0.1924(7) 0.3886(5) 0.084(4) Uani 1 1 d . . . H45A H 0.3542 -0.1694 0.3698 0.101 Uiso 1 1 calc R . . C46 C 0.3406(10) -0.2589(8) 0.4123(7) 0.110(5) Uani 1 1 d . . . H46A H 0.3816 -0.2809 0.4086 0.132 Uiso 1 1 calc R . . C47 C 0.2967(12) -0.2923(8) 0.4415(9) 0.134(7) Uani 1 1 d . . . H47A H 0.3068 -0.3377 0.4561 0.160 Uiso 1 1 calc R . . C48 C 0.2375(10) -0.2582(9) 0.4491(8) 0.118(5) Uani 1 1 d . . . H48A H 0.2090 -0.2796 0.4709 0.142 Uiso 1 1 calc R . . C49 C 0.2208(7) -0.1921(8) 0.4240(6) 0.093(4) Uani 1 1 d . . . H49A H 0.1807 -0.1691 0.4287 0.112 Uiso 1 1 calc R . . O20 O 0.5036(4) -0.0218(4) 0.1513(3) 0.0668(18) Uani 1 1 d . . . O21 O 0.5526(5) 0.0576(5) 0.1042(5) 0.109(3) Uani 1 1 d D . . C50 C 0.5565(6) 0.0128(6) 0.1445(5) 0.071(3) Uani 1 1 d . . . C51 C 0.6294(5) -0.0065(5) 0.1883(5) 0.060(2) Uani 1 1 d . . . C52 C 0.6885(8) 0.0343(6) 0.1873(7) 0.086(4) Uani 1 1 d . . . H52A H 0.6825 0.0738 0.1614 0.103 Uiso 1 1 calc R . . C53 C 0.7572(8) 0.0134(10) 0.2268(9) 0.115(5) Uani 1 1 d . . . H53A H 0.7979 0.0387 0.2270 0.138 Uiso 1 1 calc R . . C54 C 0.7637(9) -0.0432(10) 0.2641(9) 0.124(6) Uani 1 1 d . . . H54A H 0.8096 -0.0565 0.2896 0.149 Uiso 1 1 calc R . . C55 C 0.7085(8) -0.0810(8) 0.2665(7) 0.096(4) Uani 1 1 d . . . H55A H 0.7154 -0.1194 0.2938 0.115 Uiso 1 1 calc R . . C56 C 0.6400(7) -0.0625(6) 0.2279(5) 0.071(3) Uani 1 1 d . . . H56A H 0.6006 -0.0891 0.2291 0.085 Uiso 1 1 calc R . . O22 O 0.1015(4) 0.1902(4) 0.0356(3) 0.076(2) Uani 1 1 d . . . O23 O 0.0237(5) 0.2209(5) 0.0852(4) 0.101(3) Uani 1 1 d D . . C57 C 0.0413(6) 0.2145(6) 0.0359(5) 0.072(3) Uani 1 1 d . . . C58 C -0.0086(6) 0.2375(6) -0.0274(5) 0.069(3) Uani 1 1 d . . . C59 C -0.0785(7) 0.2534(10) -0.0314(7) 0.122(6) Uani 1 1 d . . . H59A H -0.0942 0.2500 0.0050 0.146 Uiso 1 1 calc R . . C60 C -0.1242(9) 0.2744(12) -0.0900(8) 0.146(8) Uani 1 1 d . . . H60A H -0.1711 0.2868 -0.0926 0.175 Uiso 1 1 calc R . . C61 C -0.1046(8) 0.2777(9) -0.1432(7) 0.110(5) Uani 1 1 d . . . H61A H -0.1369 0.2932 -0.1822 0.132 Uiso 1 1 calc R . . C62 C -0.0374(7) 0.2583(8) -0.1404(6) 0.101(5) Uani 1 1 d . . . H62A H -0.0236 0.2592 -0.1779 0.121 Uiso 1 1 calc R . . C63 C 0.0116(6) 0.2368(6) -0.0811(5) 0.075(3) Uani 1 1 d . . . H63A H 0.0577 0.2223 -0.0791 0.090 Uiso 1 1 calc R . . O24 O 0.2004(4) 0.2877(4) 0.0973(3) 0.072(2) Uani 1 1 d . . . O25 O 0.2307(5) 0.3191(4) 0.0104(4) 0.095(3) Uani 1 1 d . . . C64 C 0.1996(6) 0.3290(5) 0.0514(5) 0.068(3) Uani 1 1 d . . . C65 C 0.1587(6) 0.3935(5) 0.0487(4) 0.063(3) Uani 1 1 d . . . C66 C 0.1708(6) 0.4487(6) 0.0141(6) 0.078(3) Uani 1 1 d . . . H66A H 0.2035 0.4438 -0.0091 0.094 Uiso 1 1 calc R . . C67 C 0.1370(8) 0.5102(7) 0.0121(7) 0.098(4) Uani 1 1 d . . . H67A H 0.1460 0.5471 -0.0121 0.117 Uiso 1 1 calc R . . C68 C 0.0913(13) 0.5164(9) 0.0452(9) 0.155(9) Uani 1 1 d . . . H68A H 0.0695 0.5592 0.0462 0.186 Uiso 1 1 calc R . . C69 C 0.0744(14) 0.4604(12) 0.0794(11) 0.194(13) Uani 1 1 d . . . H69A H 0.0390 0.4642 0.0997 0.233 Uiso 1 1 calc R . . C70 C 0.1118(10) 0.4000(8) 0.0817(8) 0.127(7) Uani 1 1 d . . . H70A H 0.1044 0.3630 0.1066 0.153 Uiso 1 1 calc R . . N81 N 0.0647(10) 0.1010(11) -0.2354(11) 0.160(7) Uani 1 1 d . . . C81 C 0.0204(13) 0.1271(11) -0.2736(14) 0.133(7) Uani 1 1 d . . . C82 C -0.0336(12) 0.1609(12) -0.3216(13) 0.174(9) Uani 1 1 d . . . H82A H -0.0549 0.1294 -0.3568 0.261 Uiso 1 1 calc R . . H82B H -0.0135 0.1998 -0.3377 0.261 Uiso 1 1 calc R . . H82C H -0.0700 0.1769 -0.3036 0.261 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 Yb1 0.0406(2) 0.0646(3) 0.04342(19) 0.00138(17) 0.00990(15) 0.00263(18) Yb2 0.0501(2) 0.0505(2) 0.04044(18) 0.00203(16) 0.01450(15) 0.00467(17) Fe1 0.0387(7) 0.0529(7) 0.0406(6) 0.0003(5) 0.0060(5) -0.0025(5) Fe2 0.0444(7) 0.0528(7) 0.0393(5) 0.0019(5) 0.0082(5) 0.0033(5) Fe3 0.0491(8) 0.0634(8) 0.0437(6) 0.0067(6) 0.0136(5) 0.0133(6) O1 0.050(4) 0.052(4) 0.045(3) 0.004(3) 0.008(3) 0.001(3) N1 0.076(6) 0.074(6) 0.060(5) 0.003(4) 0.034(5) 0.012(5) C1 0.154(14) 0.066(7) 0.093(8) 0.004(6) 0.063(9) 0.034(8) C2 0.111(10) 0.064(7) 0.068(6) -0.004(5) 0.039(7) 0.028(6) O2 0.058(4) 0.051(3) 0.053(3) 0.001(3) 0.023(3) 0.005(3) C3 0.075(8) 0.115(10) 0.079(7) -0.051(7) 0.012(6) -0.006(7) C4 0.072(7) 0.071(7) 0.047(5) -0.017(5) -0.014(5) 0.004(5) O3 0.033(3) 0.061(4) 0.041(3) -0.010(3) -0.007(2) -0.003(3) O4 0.082(5) 0.087(5) 0.068(4) 0.007(4) 0.048(4) -0.001(4) N2 0.065(5) 0.088(6) 0.039(4) 0.008(4) 0.015(4) 0.020(5) C8 0.076(7) 0.098(8) 0.033(4) 0.005(5) 0.009(4) 0.023(6) C9 0.052(6) 0.099(8) 0.034(4) 0.000(4) 0.003(4) 0.021(5) O5 0.043(3) 0.071(4) 0.036(3) 0.003(3) 0.010(2) 0.010(3) C10 0.137(12) 0.066(7) 0.041(5) -0.016(5) -0.017(6) 0.016(7) C11 0.101(9) 0.059(6) 0.043(5) -0.014(4) -0.002(5) 0.016(6) O6 0.058(4) 0.043(3) 0.042(3) -0.009(2) 0.010(3) 0.000(3) O7 0.061(4) 0.079(5) 0.058(4) 0.005(3) 0.033(3) 0.005(3) N3 0.039(4) 0.109(7) 0.058(5) -0.001(5) -0.003(4) -0.013(5) C15 0.121(12) 0.140(13) 0.049(6) -0.025(7) 0.001(7) -0.063(10) C16 0.097(9) 0.084(8) 0.062(6) -0.035(6) 0.039(6) -0.024(7) O8 0.063(4) 0.071(4) 0.037(3) -0.002(3) 0.023(3) -0.002(3) C17 0.056(6) 0.071(7) 0.063(6) -0.011(5) 0.003(5) -0.027(5) C18 0.053(6) 0.059(6) 0.072(6) -0.016(5) 0.000(5) -0.013(5) O9 0.046(3) 0.046(3) 0.051(3) -0.010(3) 0.005(3) -0.001(3) O10 0.028(3) 0.113(6) 0.090(5) 0.011(5) 0.003(3) 0.020(4) N4 0.074(6) 0.067(5) 0.062(5) 0.000(4) 0.021(4) -0.014(4) C22 0.086(8) 0.075(7) 0.060(5) -0.039(5) 0.025(6) -0.015(6) C23 0.067(7) 0.107(9) 0.042(4) -0.025(5) 0.024(5) -0.010(6) O11 0.047(4) 0.080(4) 0.039(3) -0.009(3) 0.019(3) 0.006(3) C24 0.051(6) 0.077(7) 0.067(6) -0.010(5) 0.001(5) -0.022(5) C25 0.049(6) 0.076(7) 0.053(5) -0.003(5) -0.008(4) -0.008(5) O12 0.039(3) 0.061(4) 0.040(3) 0.006(3) 0.001(2) 0.005(3) C26 0.112(11) 0.054(6) 0.098(8) -0.003(6) 0.042(8) -0.035(6) C27 0.131(13) 0.061(7) 0.095(9) 0.015(7) 0.030(9) -0.014(8) C28 0.151(14) 0.063(7) 0.096(9) 0.012(6) 0.059(9) -0.014(8) O13 0.095(6) 0.044(4) 0.071(4) 0.016(3) 0.030(4) 0.009(4) O14 0.059(4) 0.053(4) 0.055(3) 0.005(3) 0.014(3) 0.002(3) O15 0.059(4) 0.053(4) 0.051(3) 0.003(3) 0.015(3) 0.000(3) C29 0.050(5) 0.058(5) 0.047(5) 0.000(4) 0.006(4) 0.006(4) C30 0.044(5) 0.052(5) 0.056(5) -0.001(4) 0.001(4) 0.005(4) C31 0.079(8) 0.063(7) 0.080(7) -0.002(5) 0.025(6) 0.006(6) C32 0.094(11) 0.070(8) 0.136(12) -0.032(8) 0.038(9) -0.002(7) C33 0.084(10) 0.058(7) 0.134(12) -0.018(8) 0.017(9) 0.008(6) C34 0.070(8) 0.058(7) 0.116(10) 0.017(7) 0.006(7) -0.001(6) C35 0.054(6) 0.056(6) 0.070(6) 0.006(5) 0.004(5) 0.006(5) O16 0.038(3) 0.076(4) 0.041(3) -0.002(3) 0.006(2) -0.003(3) O17 0.040(3) 0.069(4) 0.045(3) 0.004(3) 0.006(3) 0.005(3) C36 0.049(5) 0.048(5) 0.043(4) 0.005(4) 0.006(4) -0.002(4) C37 0.043(5) 0.049(5) 0.042(4) 0.002(4) 0.003(4) -0.005(4) C38 0.050(6) 0.077(7) 0.043(4) 0.003(4) 0.011(4) -0.004(5) C39 0.036(5) 0.102(8) 0.052(5) 0.004(5) -0.002(4) -0.004(5) C40 0.049(6) 0.088(8) 0.056(5) -0.008(5) -0.007(4) -0.009(5) C41 0.056(6) 0.087(7) 0.048(5) -0.015(5) -0.002(4) -0.009(5) C42 0.043(5) 0.073(6) 0.049(5) -0.005(4) 0.005(4) -0.007(5) O18 0.058(4) 0.072(4) 0.048(3) 0.008(3) 0.012(3) -0.011(3) O19 0.061(5) 0.111(7) 0.087(5) 0.027(5) 0.026(4) 0.002(4) C43 0.068(7) 0.071(7) 0.058(5) 0.010(5) 0.021(5) -0.009(5) C44 0.064(7) 0.087(8) 0.058(5) 0.007(5) 0.017(5) -0.017(6) C45 0.097(10) 0.094(9) 0.063(6) 0.018(6) 0.027(6) 0.008(7) C46 0.138(14) 0.096(10) 0.101(10) 0.039(8) 0.045(10) 0.032(9) C47 0.18(2) 0.083(11) 0.150(15) 0.047(10) 0.063(15) 0.012(11) C48 0.112(13) 0.107(12) 0.136(13) 0.044(10) 0.041(11) -0.011(10) C49 0.068(8) 0.120(11) 0.090(8) 0.034(8) 0.022(7) -0.009(7) O20 0.064(5) 0.070(4) 0.072(4) 0.000(3) 0.028(4) 0.010(4) O21 0.098(7) 0.115(7) 0.143(8) 0.071(6) 0.081(6) 0.048(6) C50 0.076(8) 0.068(7) 0.085(7) 0.012(6) 0.050(6) 0.016(6) C51 0.051(6) 0.060(6) 0.077(6) -0.012(5) 0.032(5) 0.004(5) C52 0.095(10) 0.070(7) 0.110(9) -0.025(7) 0.057(8) -0.016(7) C53 0.057(9) 0.136(14) 0.157(15) -0.034(12) 0.039(9) -0.028(9) C54 0.070(10) 0.140(15) 0.154(15) 0.033(13) 0.023(10) 0.012(10) C55 0.074(9) 0.122(11) 0.092(8) 0.016(8) 0.024(7) 0.020(8) C56 0.074(8) 0.076(7) 0.065(6) 0.009(5) 0.025(6) 0.010(6) O22 0.049(4) 0.115(6) 0.056(4) 0.003(4) 0.003(3) 0.022(4) O23 0.076(6) 0.155(9) 0.071(5) 0.019(5) 0.024(4) 0.052(6) C57 0.052(6) 0.098(8) 0.056(5) 0.010(5) 0.001(5) 0.018(6) C58 0.051(6) 0.072(7) 0.072(6) 0.013(5) 0.003(5) 0.009(5) C59 0.051(7) 0.215(19) 0.088(8) 0.030(10) 0.004(6) 0.058(10) C60 0.072(10) 0.24(2) 0.104(11) 0.025(13) 0.001(9) 0.067(13) C61 0.070(9) 0.142(13) 0.094(9) 0.040(9) -0.009(7) 0.024(9) C62 0.061(8) 0.141(13) 0.086(8) 0.043(8) 0.001(6) -0.010(8) C63 0.048(6) 0.091(8) 0.075(7) 0.018(6) 0.003(5) -0.003(6) O24 0.093(6) 0.063(4) 0.060(4) 0.009(3) 0.025(4) 0.014(4) O25 0.130(8) 0.087(6) 0.090(5) 0.027(5) 0.064(6) 0.042(5) C64 0.077(8) 0.056(6) 0.071(6) 0.007(5) 0.021(6) 0.012(5) C65 0.065(7) 0.071(7) 0.048(5) 0.006(5) 0.012(5) 0.014(5) C66 0.064(7) 0.069(7) 0.095(8) 0.000(6) 0.013(6) 0.004(6) C67 0.099(11) 0.071(8) 0.114(10) 0.023(7) 0.019(9) 0.030(7) C68 0.23(2) 0.112(13) 0.132(14) 0.034(11) 0.066(15) 0.115(15) C69 0.26(3) 0.18(2) 0.20(2) 0.103(18) 0.16(2) 0.17(2) C70 0.173(17) 0.106(11) 0.132(12) 0.058(10) 0.089(13) 0.078(11) N81 0.101(13) 0.156(17) 0.23(2) 0.014(14) 0.057(14) -0.037(12) C81 0.093(15) 0.113(14) 0.20(2) 0.022(14) 0.057(15) -0.017(12) C82 0.118(18) 0.16(2) 0.24(3) 0.021(19) 0.044(19) -0.046(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O8 2.247(5) . ? Yb1 O2 2.278(6) . ? Yb1 O3 2.284(5) . ? Yb1 O9 2.286(6) . ? Yb1 O4 2.350(6) . ? Yb1 O10 2.400(6) . ? Yb1 N1 2.546(8) . ? Yb1 N3 2.588(9) . ? Yb2 O11 2.249(5) . ? Yb2 O6 2.284(5) . ? Yb2 O12 2.295(5) . ? Yb2 O5 2.303(6) . ? Yb2 O13 2.359(6) . ? Yb2 O7 2.366(6) . ? Yb2 N2 2.538(7) . ? Yb2 N4 2.568(9) . ? Fe1 O1 1.986(6) . ? Fe1 O3 1.987(6) . ? Fe1 O9 1.990(6) . ? Fe1 O18 2.034(6) . ? Fe1 O16 2.050(6) . ? Fe1 O14 2.073(6) . ? Fe2 O12 1.972(6) . ? Fe2 O1 1.984(6) . ? Fe2 O6 1.995(6) . ? Fe2 O20 2.039(7) . ? Fe2 O15 2.059(6) . ? Fe2 O17 2.078(6) . ? Fe3 O8 2.010(7) . ? Fe3 O5 2.014(5) . ? Fe3 O11 2.016(6) . ? Fe3 O2 2.020(5) . ? Fe3 O24 2.050(7) . ? Fe3 O22 2.075(7) . ? O1 H1 0.88(4) . ? N1 C3 1.485(15) . ? N1 C1 1.506(14) . ? N1 C5A 1.508(15) . ? N1 C5B 1.52(2) . ? C1 C2 1.505(16) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.416(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.502(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.415(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5A C6A 1.526(19) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A C7A 1.42(2) . ? C6A O4 1.516(16) . ? C6A H6A 1.0000 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C5B C6B 1.52(2) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B C7B 1.43(3) . ? C6B O4 1.52(2) . ? C6B H6B 1.0000 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? O4 H4 1.02(3) . ? N2 C10 1.470(15) . ? N2 C8 1.500(12) . ? N2 C12A 1.508(15) . ? N2 C12B 1.544(17) . ? C8 C9 1.521(14) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O5 1.414(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.499(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O6 1.417(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12A C13A 1.504(18) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A C14A 1.47(2) . ? C13A O7 1.520(14) . ? C13A H13A 1.0000 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C12B C13B 1.49(2) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.47(2) . ? C13B O7 1.490(17) . ? C13B H13B 1.0000 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? O7 H7 1.00(3) . ? N3 C15 1.444(14) . ? N3 C17 1.492(14) . ? N3 C19B 1.53(2) . ? N3 C19A 1.539(18) . ? C15 C16 1.514(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O8 1.419(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O9 1.428(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19A C20A 1.51(2) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C20A O10 1.479(19) . ? C20A C21A 1.52(2) . ? C20A H20A 1.0000 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C19B C20B 1.49(3) . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C20B O10 1.47(2) . ? C20B C21B 1.52(3) . ? C20B H20B 1.0000 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? O10 H10 1.01(3) . ? N4 C24 1.486(14) . ? N4 C22 1.488(13) . ? N4 C26 1.493(13) . ? C22 C23 1.505(15) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O11 1.449(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.491(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O12 1.435(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.460(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O13 1.451(15) . ? C27 C28 1.513(16) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O13 H13 0.94(4) . ? O14 C29 1.286(10) . ? O15 C29 1.249(11) . ? C29 C30 1.523(13) . ? C30 C31 1.390(14) . ? C30 C35 1.391(14) . ? C31 C32 1.403(16) . ? C31 H31A 0.9500 . ? C32 C33 1.42(2) . ? C32 H32A 0.9500 . ? C33 C34 1.378(19) . ? C33 H33A 0.9500 . ? C34 C35 1.397(15) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? O16 C36 1.282(11) . ? O17 C36 1.267(10) . ? C36 C37 1.500(11) . ? C37 C38 1.386(13) . ? C37 C42 1.398(12) . ? C38 C39 1.395(12) . ? C38 H38A 0.9500 . ? C39 C40 1.383(14) . ? C39 H39A 0.9500 . ? C40 C41 1.418(15) . ? C40 H40A 0.9500 . ? C41 C42 1.402(13) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? O18 C43 1.280(12) . ? O19 C43 1.279(13) . ? C43 C44 1.503(15) . ? C44 C45 1.386(17) . ? C44 C49 1.403(15) . ? C45 C46 1.411(18) . ? C45 H45A 0.9500 . ? C46 C47 1.40(2) . ? C46 H46A 0.9500 . ? C47 C48 1.41(2) . ? C47 H47A 0.9500 . ? C48 C49 1.41(2) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? O20 C50 1.301(13) . ? O21 C50 1.237(12) . ? C50 C51 1.519(15) . ? C51 C56 1.381(14) . ? C51 C52 1.431(15) . ? C52 C53 1.43(2) . ? C52 H52A 0.9500 . ? C53 C54 1.37(2) . ? C53 H53A 0.9500 . ? C54 C55 1.34(2) . ? C54 H54A 0.9500 . ? C55 C56 1.412(17) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? O22 C57 1.292(12) . ? O23 C57 1.248(12) . ? C57 C58 1.509(14) . ? C58 C63 1.365(15) . ? C58 C59 1.402(16) . ? C59 C60 1.389(19) . ? C59 H59A 0.9500 . ? C60 C61 1.35(2) . ? C60 H60A 0.9500 . ? C61 C62 1.374(19) . ? C61 H61A 0.9500 . ? C62 C63 1.430(15) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? O24 C64 1.296(12) . ? O25 C64 1.260(13) . ? C64 C65 1.500(14) . ? C65 C70 1.357(17) . ? C65 C66 1.391(15) . ? C66 C67 1.379(17) . ? C66 H66A 0.9500 . ? C67 C68 1.34(2) . ? C67 H67A 0.9500 . ? C68 C69 1.43(3) . ? C68 H68A 0.9500 . ? C69 C70 1.40(2) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? N81 C81 1.13(3) . ? C81 C82 1.42(3) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? 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 O8 Yb1 O2 67.9(2) . . ? O8 Yb1 O3 102.6(2) . . ? O2 Yb1 O3 92.2(2) . . ? O8 Yb1 O9 85.6(2) . . ? O2 Yb1 O9 143.4(2) . . ? O3 Yb1 O9 68.6(2) . . ? O8 Yb1 O4 155.0(3) . . ? O2 Yb1 O4 133.2(2) . . ? O3 Yb1 O4 91.0(3) . . ? O9 Yb1 O4 79.9(2) . . ? O8 Yb1 O10 93.5(3) . . ? O2 Yb1 O10 76.3(3) . . ? O3 Yb1 O10 155.1(3) . . ? O9 Yb1 O10 132.3(3) . . ? O4 Yb1 O10 81.6(3) . . ? O8 Yb1 N1 135.3(3) . . ? O2 Yb1 N1 68.5(2) . . ? O3 Yb1 N1 69.5(3) . . ? O9 Yb1 N1 126.5(2) . . ? O4 Yb1 N1 69.1(3) . . ? O10 Yb1 N1 85.7(3) . . ? O8 Yb1 N3 71.1(3) . . ? O2 Yb1 N3 122.3(3) . . ? O3 Yb1 N3 135.6(3) . . ? O9 Yb1 N3 67.2(3) . . ? O4 Yb1 N3 84.5(3) . . ? O10 Yb1 N3 67.5(3) . . ? N1 Yb1 N3 145.0(3) . . ? O11 Yb2 O6 103.4(2) . . ? O11 Yb2 O12 84.2(2) . . ? O6 Yb2 O12 67.9(2) . . ? O11 Yb2 O5 67.7(2) . . ? O6 Yb2 O5 93.2(2) . . ? O12 Yb2 O5 141.9(2) . . ? O11 Yb2 O13 93.9(2) . . ? O6 Yb2 O13 154.8(2) . . ? O12 Yb2 O13 132.8(3) . . ? O5 Yb2 O13 76.5(3) . . ? O11 Yb2 O7 154.8(2) . . ? O6 Yb2 O7 91.2(2) . . ? O12 Yb2 O7 82.4(2) . . ? O5 Yb2 O7 132.7(2) . . ? O13 Yb2 O7 79.9(3) . . ? O11 Yb2 N2 134.4(2) . . ? O6 Yb2 N2 70.1(2) . . ? O12 Yb2 N2 128.4(2) . . ? O5 Yb2 N2 67.8(2) . . ? O13 Yb2 N2 84.8(3) . . ? O7 Yb2 N2 69.8(3) . . ? O11 Yb2 N4 72.3(3) . . ? O6 Yb2 N4 135.3(2) . . ? O12 Yb2 N4 67.4(3) . . ? O5 Yb2 N4 122.9(3) . . ? O13 Yb2 N4 67.3(3) . . ? O7 Yb2 N4 82.8(3) . . ? N2 Yb2 N4 144.0(3) . . ? O1 Fe1 O3 89.3(2) . . ? O1 Fe1 O9 93.1(2) . . ? O3 Fe1 O9 80.7(2) . . ? O1 Fe1 O18 173.6(3) . . ? O3 Fe1 O18 96.0(3) . . ? O9 Fe1 O18 91.3(3) . . ? O1 Fe1 O16 91.0(2) . . ? O3 Fe1 O16 94.8(2) . . ? O9 Fe1 O16 173.8(2) . . ? O18 Fe1 O16 84.9(2) . . ? O1 Fe1 O14 87.5(2) . . ? O3 Fe1 O14 172.5(2) . . ? O9 Fe1 O14 92.7(2) . . ? O18 Fe1 O14 87.7(3) . . ? O16 Fe1 O14 92.1(3) . . ? O12 Fe2 O1 92.4(2) . . ? O12 Fe2 O6 80.3(2) . . ? O1 Fe2 O6 88.3(2) . . ? O12 Fe2 O20 90.8(3) . . ? O1 Fe2 O20 174.4(3) . . ? O6 Fe2 O20 96.8(3) . . ? O12 Fe2 O15 176.5(2) . . ? O1 Fe2 O15 89.2(3) . . ? O6 Fe2 O15 96.6(2) . . ? O20 Fe2 O15 87.9(3) . . ? O12 Fe2 O17 92.6(2) . . ? O1 Fe2 O17 89.0(2) . . ? O6 Fe2 O17 172.3(2) . . ? O20 Fe2 O17 86.3(3) . . ? O15 Fe2 O17 90.6(2) . . ? O8 Fe3 O5 92.8(2) . . ? O8 Fe3 O11 92.7(3) . . ? O5 Fe3 O11 78.0(2) . . ? O8 Fe3 O2 77.7(2) . . ? O5 Fe3 O2 166.3(2) . . ? O11 Fe3 O2 92.5(2) . . ? O8 Fe3 O24 167.5(3) . . ? O5 Fe3 O24 99.1(3) . . ? O11 Fe3 O24 93.6(3) . . ? O2 Fe3 O24 91.2(3) . . ? O8 Fe3 O22 91.2(3) . . ? O5 Fe3 O22 90.0(3) . . ? O11 Fe3 O22 167.6(3) . . ? O2 Fe3 O22 99.8(3) . . ? O24 Fe3 O22 84.8(3) . . ? Fe2 O1 Fe1 126.5(3) . . ? Fe2 O1 H1 120(6) . . ? Fe1 O1 H1 110(6) . . ? C3 N1 C1 108.8(11) . . ? C3 N1 C5A 107.1(11) . . ? C1 N1 C5A 113.7(11) . . ? C3 N1 C5B 130.8(18) . . ? C1 N1 C5B 93.6(15) . . ? C3 N1 Yb1 109.1(6) . . ? C1 N1 Yb1 106.1(6) . . ? C5A N1 Yb1 111.9(7) . . ? C5B N1 Yb1 105.5(13) . . ? C2 C1 N1 111.7(9) . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1B 109.3 . . ? N1 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? O2 C2 C1 112.3(9) . . ? O2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? O2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C2 O2 Fe3 129.6(6) . . ? C2 O2 Yb1 123.9(5) . . ? Fe3 O2 Yb1 106.4(2) . . ? N1 C3 C4 112.2(9) . . ? N1 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 110.5(8) . . ? O3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? O3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 O3 Fe1 125.1(5) . . ? C4 O3 Yb1 122.7(6) . . ? Fe1 O3 Yb1 104.0(2) . . ? N1 C5A C6A 109.7(12) . . ? N1 C5A H5A1 109.7 . . ? C6A C5A H5A1 109.7 . . ? N1 C5A H5A2 109.7 . . ? C6A C5A H5A2 109.7 . . ? H5A1 C5A H5A2 108.2 . . ? C7A C6A O4 113.9(19) . . ? C7A C6A C5A 117(2) . . ? O4 C6A C5A 104.8(12) . . ? C7A C6A H6A 107.0 . . ? O4 C6A H6A 107.0 . . ? C5A C6A H6A 107.0 . . ? C6A C7A H7A1 109.5 . . ? C6A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C6A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? N1 C5B C6B 110.2(19) . . ? N1 C5B H5B1 109.6 . . ? C6B C5B H5B1 109.6 . . ? N1 C5B H5B2 109.6 . . ? C6B C5B H5B2 109.6 . . ? H5B1 C5B H5B2 108.1 . . ? C7B C6B O4 114(2) . . ? C7B C6B C5B 114(2) . . ? O4 C6B C5B 105.5(18) . . ? C7B C6B H6B 107.7 . . ? O4 C6B H6B 107.7 . . ? C5B C6B H6B 107.7 . . ? C6B C7B H7B1 109.5 . . ? C6B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C6B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C6A O4 Yb1 111.6(7) . . ? C6B O4 Yb1 121.7(11) . . ? C6A O4 H4 114(6) . . ? Yb1 O4 H4 124(6) . . ? C10 N2 C8 110.6(9) . . ? C10 N2 C12A 102.4(11) . . ? C8 N2 C12A 117.8(10) . . ? C10 N2 C12B 125.0(13) . . ? C8 N2 C12B 98.1(11) . . ? C10 N2 Yb2 108.1(5) . . ? C8 N2 Yb2 106.6(5) . . ? C12A N2 Yb2 111.1(7) . . ? C12B N2 Yb2 107.0(9) . . ? N2 C8 C9 110.8(7) . . ? N2 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O5 C9 C8 110.6(8) . . ? O5 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 O5 Fe3 129.2(5) . . ? C9 O5 Yb2 124.5(5) . . ? Fe3 O5 Yb2 106.2(2) . . ? N2 C10 C11 114.3(9) . . ? N2 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? N2 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? O6 C11 C10 109.8(8) . . ? O6 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? O6 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 O6 Fe2 127.0(5) . . ? C11 O6 Yb2 122.5(5) . . ? Fe2 O6 Yb2 104.2(2) . . ? C13A C12A N2 108.7(12) . . ? C13A C12A H12A 110.0 . . ? N2 C12A H12A 110.0 . . ? C13A C12A H12B 110.0 . . ? N2 C12A H12B 110.0 . . ? H12A C12A H12B 108.3 . . ? C14A C13A C12A 114.8(18) . . ? C14A C13A O7 111.6(18) . . ? C12A C13A O7 105.4(11) . . ? C14A C13A H13A 108.3 . . ? C12A C13A H13A 108.3 . . ? O7 C13A H13A 108.3 . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C13B C12B N2 113.8(14) . . ? C13B C12B H12C 108.8 . . ? N2 C12B H12C 108.8 . . ? C13B C12B H12D 108.8 . . ? N2 C12B H12D 108.8 . . ? H12C C12B H12D 107.7 . . ? C14B C13B C12B 118.4(19) . . ? C14B C13B O7 111.9(16) . . ? C12B C13B O7 107.1(15) . . ? C14B C13B H13B 106.2 . . ? C12B C13B H13B 106.2 . . ? O7 C13B H13B 106.2 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13B O7 Yb2 122.1(9) . . ? C13A O7 Yb2 111.6(7) . . ? C13A O7 H7 113(5) . . ? Yb2 O7 H7 116(6) . . ? C15 N3 C17 115.4(11) . . ? C15 N3 C19B 97(2) . . ? C17 N3 C19B 116.6(19) . . ? C15 N3 C19A 116.1(13) . . ? C17 N3 C19A 103.7(10) . . ? C15 N3 Yb1 107.5(7) . . ? C17 N3 Yb1 106.8(5) . . ? C19B N3 Yb1 113.4(12) . . ? C19A N3 Yb1 106.8(9) . . ? N3 C15 C16 115.7(9) . . ? N3 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? N3 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.4 . . ? O8 C16 C15 110.9(9) . . ? O8 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? O8 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 O8 Fe3 130.2(6) . . ? C16 O8 Yb1 119.0(6) . . ? Fe3 O8 Yb1 107.9(3) . . ? N3 C17 C18 110.3(8) . . ? N3 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N3 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? O9 C18 C17 108.3(8) . . ? O9 C18 H18A 110.0 . . ? C17 C18 H18A 110.0 . . ? O9 C18 H18B 110.0 . . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? C18 O9 Fe1 128.4(6) . . ? C18 O9 Yb1 126.6(6) . . ? Fe1 O9 Yb1 103.8(2) . . ? C20A C19A N3 110.7(15) . . ? C20A C19A H19A 109.5 . . ? N3 C19A H19A 109.5 . . ? C20A C19A H19B 109.5 . . ? N3 C19A H19B 109.5 . . ? H19A C19A H19B 108.1 . . ? O10 C20A C19A 106.0(14) . . ? O10 C20A C21A 112.4(15) . . ? C19A C20A C21A 111.5(17) . . ? O10 C20A H20A 108.9 . . ? C19A C20A H20A 108.9 . . ? C21A C20A H20A 108.9 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20B C19B N3 108(2) . . ? C20B C19B H19C 110.1 . . ? N3 C19B H19C 110.1 . . ? C20B C19B H19D 110.1 . . ? N3 C19B H19D 110.1 . . ? H19C C19B H19D 108.4 . . ? O10 C20B C19B 110(2) . . ? O10 C20B C21B 114(2) . . ? C19B C20B C21B 119(3) . . ? O10 C20B H20B 103.8 . . ? C19B C20B H20B 103.8 . . ? C21B C20B H20B 103.8 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20B O10 Yb1 110.9(16) . . ? C20A O10 Yb1 123.3(9) . . ? C20B O10 H10 119(8) . . ? Yb1 O10 H10 122(7) . . ? C24 N4 C22 112.9(8) . . ? C24 N4 C26 108.3(9) . . ? C22 N4 C26 113.0(9) . . ? C24 N4 Yb2 107.6(6) . . ? C22 N4 Yb2 106.6(6) . . ? C26 N4 Yb2 108.1(6) . . ? N4 C22 C23 114.3(8) . . ? N4 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N4 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? O11 C23 C22 110.5(7) . . ? O11 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? O11 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 O11 Fe3 130.1(6) . . ? C23 O11 Yb2 117.8(5) . . ? Fe3 O11 Yb2 108.1(2) . . ? N4 C24 C25 113.2(8) . . ? N4 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N4 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.8 . . ? O12 C25 C24 107.5(7) . . ? O12 C25 H25A 110.2 . . ? C24 C25 H25A 110.2 . . ? O12 C25 H25B 110.2 . . ? C24 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C25 O12 Fe2 127.8(5) . . ? C25 O12 Yb2 126.7(5) . . ? Fe2 O12 Yb2 104.6(2) . . ? C27 C26 N4 115.5(11) . . ? C27 C26 H26A 108.4 . . ? N4 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? N4 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? O13 C27 C26 109.8(10) . . ? O13 C27 C28 112.2(11) . . ? C26 C27 C28 114.5(13) . . ? O13 C27 H27A 106.6 . . ? C26 C27 H27A 106.6 . . ? C28 C27 H27A 106.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 O13 Yb2 124.5(7) . . ? C27 O13 H13 98(7) . . ? Yb2 O13 H13 123(7) . . ? C29 O14 Fe1 134.9(6) . . ? C29 O15 Fe2 128.1(6) . . ? O15 C29 O14 127.6(9) . . ? O15 C29 C30 118.2(8) . . ? O14 C29 C30 114.2(8) . . ? C31 C30 C35 119.7(9) . . ? C31 C30 C29 119.9(9) . . ? C35 C30 C29 120.4(8) . . ? C30 C31 C32 120.1(12) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C31 C32 C33 119.0(13) . . ? C31 C32 H32A 120.5 . . ? C33 C32 H32A 120.5 . . ? C34 C33 C32 121.0(12) . . ? C34 C33 H33A 119.5 . . ? C32 C33 H33A 119.5 . . ? C33 C34 C35 118.9(13) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C30 C35 C34 121.3(11) . . ? C30 C35 H35A 119.3 . . ? C34 C35 H35A 119.3 . . ? C36 O16 Fe1 128.1(5) . . ? C36 O17 Fe2 136.5(6) . . ? O17 C36 O16 125.8(8) . . ? O17 C36 C37 116.8(8) . . ? O16 C36 C37 117.3(7) . . ? C38 C37 C42 118.9(8) . . ? C38 C37 C36 119.8(8) . . ? C42 C37 C36 121.3(8) . . ? C37 C38 C39 121.0(9) . . ? C37 C38 H38A 119.5 . . ? C39 C38 H38A 119.5 . . ? C40 C39 C38 120.5(9) . . ? C40 C39 H39A 119.7 . . ? C38 C39 H39A 119.7 . . ? C39 C40 C41 119.4(9) . . ? C39 C40 H40A 120.3 . . ? C41 C40 H40A 120.3 . . ? C42 C41 C40 119.2(9) . . ? C42 C41 H41A 120.4 . . ? C40 C41 H41A 120.4 . . ? C37 C42 C41 121.0(9) . . ? C37 C42 H42A 119.5 . . ? C41 C42 H42A 119.5 . . ? C43 O18 Fe1 139.4(6) . . ? O19 C43 O18 124.1(10) . . ? O19 C43 C44 120.2(9) . . ? O18 C43 C44 115.8(10) . . ? C45 C44 C49 119.7(12) . . ? C45 C44 C43 120.3(10) . . ? C49 C44 C43 119.9(11) . . ? C44 C45 C46 120.9(13) . . ? C44 C45 H45A 119.6 . . ? C46 C45 H45A 119.6 . . ? C47 C46 C45 119.6(15) . . ? C47 C46 H46A 120.2 . . ? C45 C46 H46A 120.2 . . ? C46 C47 C48 119.8(14) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? C49 C48 C47 119.6(14) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C44 C49 C48 120.1(14) . . ? C44 C49 H49A 119.9 . . ? C48 C49 H49A 119.9 . . ? C50 O20 Fe2 131.8(6) . . ? O21 C50 O20 125.7(12) . . ? O21 C50 C51 117.8(10) . . ? O20 C50 C51 116.4(9) . . ? C56 C51 C52 119.5(11) . . ? C56 C51 C50 121.8(9) . . ? C52 C51 C50 118.6(10) . . ? C51 C52 C53 117.7(13) . . ? C51 C52 H52A 121.2 . . ? C53 C52 H52A 121.2 . . ? C54 C53 C52 119.5(14) . . ? C54 C53 H53A 120.2 . . ? C52 C53 H53A 120.2 . . ? C55 C54 C53 123.4(16) . . ? C55 C54 H54A 118.3 . . ? C53 C54 H54A 118.3 . . ? C54 C55 C56 118.9(15) . . ? C54 C55 H55A 120.6 . . ? C56 C55 H55A 120.6 . . ? C51 C56 C55 121.0(12) . . ? C51 C56 H56A 119.5 . . ? C55 C56 H56A 119.5 . . ? C57 O22 Fe3 133.7(7) . . ? O23 C57 O22 123.8(9) . . ? O23 C57 C58 119.4(10) . . ? O22 C57 C58 116.8(9) . . ? C63 C58 C59 120.2(10) . . ? C63 C58 C57 120.7(10) . . ? C59 C58 C57 118.8(11) . . ? C60 C59 C58 118.4(14) . . ? C60 C59 H59A 120.8 . . ? C58 C59 H59A 120.8 . . ? C61 C60 C59 122.6(14) . . ? C61 C60 H60A 118.7 . . ? C59 C60 H60A 118.7 . . ? C60 C61 C62 119.3(12) . . ? C60 C61 H61A 120.3 . . ? C62 C61 H61A 120.3 . . ? C61 C62 C63 120.1(13) . . ? C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C58 C63 C62 119.1(11) . . ? C58 C63 H63A 120.4 . . ? C62 C63 H63A 120.4 . . ? C64 O24 Fe3 132.8(6) . . ? O25 C64 O24 125.1(10) . . ? O25 C64 C65 119.1(9) . . ? O24 C64 C65 115.8(9) . . ? C70 C65 C66 119.2(11) . . ? C70 C65 C64 121.0(10) . . ? C66 C65 C64 119.8(10) . . ? C67 C66 C65 122.4(12) . . ? C67 C66 H66A 118.8 . . ? C65 C66 H66A 118.8 . . ? C68 C67 C66 118.1(14) . . ? C68 C67 H67A 121.0 . . ? C66 C67 H67A 121.0 . . ? C67 C68 C69 121.8(14) . . ? C67 C68 H68A 119.1 . . ? C69 C68 H68A 119.1 . . ? C70 C69 C68 117.7(16) . . ? C70 C69 H69A 121.1 . . ? C68 C69 H69A 121.1 . . ? C65 C70 C69 120.6(14) . . ? C65 C70 H70A 119.7 . . ? C69 C70 H70A 119.7 . . ? N81 C81 C82 179(2) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O11 0.88(4) 2.29(6) 3.106(9) 153(9) . O4 H4 O19 1.02(3) 1.65(3) 2.650(11) 165(10) . O7 H7 O21 1.00(3) 1.62(3) 2.590(11) 164(9) . O10 H10 O23 1.01(3) 1.61(3) 2.611(12) 170(11) . O13 H13 O25 0.94(4) 1.67(5) 2.592(12) 167(10) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.716 _refine_diff_density_min -2.449 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 912847' ####################################################################### # # 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_ambf11ybs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H100 Fe4 N6 O24 S2 Yb2, (C2 H3 N), 3(C H4 O)' _chemical_formula_sum 'C61 H115 Fe4 N7 O27 S2 Yb2' _chemical_formula_weight 2012.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0043 0.0021 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0082 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0142 0.0079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1500 0.1576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3536 1.0498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.5923 6.7648 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.449(2) _cell_length_b 24.951(4) _cell_length_c 23.760(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.820(2) _cell_angle_gamma 90.00 _cell_volume 8384(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9821 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 32.19 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4088 _exptl_absorpt_coefficient_mu 4.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.437 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; The measurement was carried out on the SCD beamline at the ANKA synchrotron source, Karslruhe Institute of Technology. Crystal decomposition in the beam during the latter part of the measurement resulted in data completeness of only 77.7%. However the data were sufficient to establish the structure of the complex. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.80000 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30732 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_unetI/netI 0.0747 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.81 _reflns_number_total 11932 _reflns_number_gt 9576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'Apex2 (Bruker AXS Inc., 2005)' _computing_data_reduction 'Apex2 (Bruker AXS Inc., 2005)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. Parts of the ligands centred on N(4) and N(5) was disordered, and were modelled using isotropic partial-occupancy (66:34 and 54:46, respectively) carbon atoms, using geometrical similarity restraints: SADI C24 C25A C24 C25B SADI C25A O11 C25B O11 SADI C26 C27A C26 C27B SADI C27A O12 C27B O12 SADI C27A C28A C27B C28B SADI N5 C29A N5 C29B N5 C31A N5 C31B SADI C29A C30A C29B C30B C31A C32 C31B C32 SADI C30A O13 C30B O13 O-H distances were restrained: DFIX 0.92 0.04 O3 H3 O6 H6 DFIX 1.53 0.04 H3 O9 H6 O18 The lattice solvent could be identified as a total of 1 MeCN and 3 MeOH per cluster molecule, but could not be satisfactorily refined and was dealt with using SQUEEZE - see below. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 897 153 '2MeCN + 6MeOH (= 152 e)' 2 0.000 0.500 0.500 897 153 '2MeCN + 6MeOH (= 152 e)' 3 0.439 0.862 0.423 10 1 ' ' 4 0.439 0.638 0.923 10 1 ' ' 5 0.561 0.362 0.077 10 1 ' ' 6 0.561 0.138 0.577 10 1 ' ' _platon_squeeze_details ; ; _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^)+(0.1374P)^2^+55.8240P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11932 _refine_ls_number_parameters 847 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.2858 _refine_ls_wR_factor_gt 0.2615 _refine_ls_goodness_of_fit_ref 1.293 _refine_ls_restrained_S_all 1.292 _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 Yb1 Yb 0.59176(5) 0.18829(2) 0.32773(2) 0.0475(3) Uani 1 1 d . . . Yb2 Yb 0.54474(5) 0.32678(2) 0.36427(2) 0.0481(3) Uani 1 1 d . B . Fe1 Fe 0.40811(15) 0.11779(8) 0.35619(8) 0.0493(5) Uani 1 1 d . . . Fe2 Fe 0.25304(18) 0.12882(9) 0.43524(9) 0.0605(6) Uani 1 1 d . B . Fe3 Fe 0.26506(18) 0.23993(9) 0.50277(10) 0.0645(6) Uani 1 1 d . B . Fe4 Fe 0.41665(18) 0.32061(9) 0.46806(9) 0.0555(6) Uani 1 1 d . B . N1 N 0.7051(9) 0.1575(4) 0.4191(5) 0.051(3) Uani 1 1 d . . . C1 C 0.7707(12) 0.2039(6) 0.4359(6) 0.066(5) Uani 1 1 d . . . H1A H 0.8134 0.2071 0.4084 0.079 Uiso 1 1 calc R . . H1B H 0.8101 0.1974 0.4746 0.079 Uiso 1 1 calc R . . C2 C 0.7167(11) 0.2550(5) 0.4365(6) 0.056(4) Uani 1 1 d . . . H2A H 0.6871 0.2559 0.4705 0.067 Uiso 1 1 calc R . . H2B H 0.7602 0.2860 0.4388 0.067 Uiso 1 1 calc R . . O1 O 0.6443(7) 0.2582(4) 0.3842(4) 0.052(2) Uani 1 1 d . . . C3 C 0.6536(12) 0.1442(6) 0.4615(6) 0.064(5) Uani 1 1 d . . . H3A H 0.6911 0.1547 0.4996 0.077 Uiso 1 1 calc R . . H3B H 0.6453 0.1048 0.4617 0.077 Uiso 1 1 calc R . . C4 C 0.5534(11) 0.1714(7) 0.4530(6) 0.059(4) Uani 1 1 d . . . H4A H 0.5147 0.1537 0.4775 0.071 Uiso 1 1 calc R . . H4B H 0.5598 0.2098 0.4634 0.071 Uiso 1 1 calc R . . O2 O 0.5110(8) 0.1653(4) 0.3944(4) 0.058(3) Uani 1 1 d . . . C5 C 0.7595(12) 0.1128(6) 0.4025(6) 0.059(4) Uani 1 1 d . . . H5A H 0.7987 0.0970 0.4377 0.071 Uiso 1 1 calc R . . H5B H 0.8028 0.1268 0.3787 0.071 Uiso 1 1 calc R . . C6 C 0.7003(11) 0.0698(6) 0.3700(7) 0.059(4) Uani 1 1 d . . . H6A H 0.6712 0.0487 0.3976 0.071 Uiso 1 1 calc R . . C7 C 0.7539(14) 0.0312(7) 0.3384(8) 0.072(5) Uani 1 1 d . . . H7A H 0.7106 0.0034 0.3194 0.108 Uiso 1 1 calc R . . H7B H 0.8055 0.0144 0.3660 0.108 Uiso 1 1 calc R . . H7C H 0.7800 0.0509 0.3095 0.108 Uiso 1 1 calc R . . O3 O 0.6249(7) 0.0938(4) 0.3277(4) 0.054(2) Uani 1 1 d D . . H3 H 0.570(6) 0.074(5) 0.333(6) 0.065 Uiso 1 1 d D . . N2 N 0.4039(9) 0.3518(4) 0.2850(5) 0.050(3) Uani 1 1 d . . . C8 C 0.4239(12) 0.3267(5) 0.2312(6) 0.054(4) Uani 1 1 d . . . H8A H 0.3670 0.3293 0.2001 0.064 Uiso 1 1 calc R . . H8B H 0.4758 0.3465 0.2189 0.064 Uiso 1 1 calc R . . C9 C 0.4511(10) 0.2696(6) 0.2414(5) 0.050(4) Uani 1 1 d . . . H9A H 0.3948 0.2483 0.2449 0.060 Uiso 1 1 calc R . . H9B H 0.4754 0.2556 0.2082 0.060 Uiso 1 1 calc R . . O4 O 0.5234(7) 0.2637(4) 0.2935(4) 0.052(2) Uani 1 1 d . . . C10 C 0.3151(10) 0.3291(6) 0.3005(6) 0.052(4) Uani 1 1 d . . . H10A H 0.2809 0.3581 0.3160 0.062 Uiso 1 1 calc R . . H10B H 0.2732 0.3150 0.2654 0.062 Uiso 1 1 calc R . . C11 C 0.3367(11) 0.2854(6) 0.3439(6) 0.060(4) Uani 1 1 d . . . H11A H 0.2804 0.2783 0.3605 0.071 Uiso 1 1 calc R . . H11B H 0.3520 0.2521 0.3249 0.071 Uiso 1 1 calc R . . O5 O 0.4122(7) 0.2991(4) 0.3873(4) 0.057(3) Uani 1 1 d . . . C12 C 0.4014(12) 0.4097(5) 0.2780(6) 0.057(4) Uani 1 1 d . . . H12A H 0.3425 0.4203 0.2510 0.068 Uiso 1 1 calc R . . H12B H 0.4557 0.4215 0.2615 0.068 Uiso 1 1 calc R . . C13 C 0.4058(14) 0.4375(6) 0.3374(6) 0.065(5) Uani 1 1 d . . . H13A H 0.3442 0.4330 0.3498 0.079 Uiso 1 1 calc R . . C14 C 0.4270(14) 0.4964(7) 0.3317(8) 0.074(5) Uani 1 1 d . . . H14A H 0.4296 0.5142 0.3688 0.111 Uiso 1 1 calc R . . H14B H 0.3771 0.5127 0.3026 0.111 Uiso 1 1 calc R . . H14C H 0.4880 0.5004 0.3202 0.111 Uiso 1 1 calc R . . O6 O 0.4803(8) 0.4140(4) 0.3785(4) 0.058(3) Uani 1 1 d D . . H6 H 0.453(10) 0.412(6) 0.413(4) 0.069 Uiso 1 1 d D . . N3 N 0.3077(10) 0.0784(6) 0.2827(6) 0.069(4) Uani 1 1 d . . . C15 C 0.3321(15) 0.0984(8) 0.2278(7) 0.082(6) Uani 1 1 d . . . H15A H 0.3283 0.0683 0.2003 0.098 Uiso 1 1 calc R . . H15B H 0.2854 0.1258 0.2105 0.098 Uiso 1 1 calc R . . C16 C 0.4261(11) 0.1214(6) 0.2378(6) 0.057(4) Uani 1 1 d . . . H16A H 0.4728 0.0921 0.2394 0.068 Uiso 1 1 calc R . . H16B H 0.4313 0.1446 0.2048 0.068 Uiso 1 1 calc R . . O7 O 0.4493(7) 0.1517(4) 0.2888(4) 0.050(2) Uani 1 1 d . . . C17 C 0.2113(12) 0.0951(9) 0.2869(8) 0.079(5) Uani 1 1 d . . . H17A H 0.1867 0.0712 0.3137 0.095 Uiso 1 1 calc R . . H17B H 0.1685 0.0927 0.2487 0.095 Uiso 1 1 calc R . . C18 C 0.2148(15) 0.1511(8) 0.3081(8) 0.083(6) Uani 1 1 d . . . H18A H 0.2296 0.1757 0.2785 0.100 Uiso 1 1 calc R . . H18B H 0.1527 0.1614 0.3162 0.100 Uiso 1 1 calc R . . O8 O 0.2881(8) 0.1553(4) 0.3609(4) 0.064(3) Uani 1 1 d . . . C19 C 0.3273(14) 0.0213(7) 0.2950(8) 0.080(5) Uani 1 1 d . . . H19A H 0.2974 -0.0002 0.2611 0.096 Uiso 1 1 calc R . . H19B H 0.2990 0.0104 0.3278 0.096 Uiso 1 1 calc R . . C20 C 0.4324(14) 0.0100(8) 0.3091(9) 0.082(6) Uani 1 1 d . . . H20A H 0.4570 0.0126 0.2728 0.099 Uiso 1 1 calc R . . C21 C 0.4559(17) -0.0437(8) 0.3345(9) 0.092(7) Uani 1 1 d . . . H21A H 0.5247 -0.0486 0.3428 0.139 Uiso 1 1 calc R . . H21B H 0.4263 -0.0712 0.3072 0.139 Uiso 1 1 calc R . . H21C H 0.4323 -0.0469 0.3702 0.139 Uiso 1 1 calc R . . O9 O 0.4765(8) 0.0510(4) 0.3476(5) 0.066(3) Uani 1 1 d D . . N4 N 0.2657(11) 0.0554(6) 0.5012(6) 0.069(4) Uani 1 1 d . B . C22 C 0.3385(16) 0.0205(8) 0.4871(9) 0.087(6) Uani 1 1 d . . . H22A H 0.3092 -0.0045 0.4562 0.104 Uiso 1 1 calc R . . H22B H 0.3665 -0.0011 0.5213 0.104 Uiso 1 1 calc R . . C23 C 0.4153(15) 0.0514(7) 0.4678(8) 0.078(5) Uani 1 1 d . . . H23A H 0.4568 0.0689 0.5010 0.093 Uiso 1 1 calc R . . H23B H 0.4543 0.0271 0.4492 0.093 Uiso 1 1 calc R . . O10 O 0.3716(7) 0.0900(4) 0.4286(4) 0.056(3) Uani 1 1 d . . . C24 C 0.2911(19) 0.0782(9) 0.5577(10) 0.104(7) Uani 1 1 d D . . H24A H 0.3295 0.0519 0.5836 0.124 Uiso 0.64 1 calc PR A 1 H24B H 0.2327 0.0849 0.5723 0.124 Uiso 0.64 1 calc PR A 1 H24C H 0.3597 0.0729 0.5723 0.124 Uiso 0.36 1 calc PR A 2 H24D H 0.2573 0.0586 0.5836 0.124 Uiso 0.36 1 calc PR A 2 C25A C 0.3435(19) 0.1277(9) 0.5598(10) 0.064(6) Uiso 0.64 1 d PD B 1 H25A H 0.4098 0.1201 0.5574 0.077 Uiso 0.64 1 calc PR B 1 H25B H 0.3436 0.1465 0.5965 0.077 Uiso 0.64 1 calc PR B 1 C25B C 0.270(4) 0.1347(13) 0.5603(19) 0.090(16) Uiso 0.36 1 d PD B 2 H25C H 0.3049 0.1501 0.5969 0.108 Uiso 0.36 1 calc PR B 2 H25D H 0.2015 0.1399 0.5582 0.108 Uiso 0.36 1 calc PR B 2 O11 O 0.2988(13) 0.1610(5) 0.5117(5) 0.100(5) Uani 1 1 d D . . C26 C 0.1767(17) 0.0335(10) 0.4909(10) 0.099(7) Uani 1 1 d D . . H26A H 0.1386 0.0518 0.5154 0.119 Uiso 0.64 1 calc PR B 1 H26B H 0.1814 -0.0048 0.5020 0.119 Uiso 0.64 1 calc PR B 1 H26C H 0.1563 0.0300 0.5280 0.119 Uiso 0.36 1 calc PR B 2 H26D H 0.1801 -0.0030 0.4752 0.119 Uiso 0.36 1 calc PR B 2 C27A C 0.127(2) 0.0380(10) 0.4293(11) 0.070(7) Uiso 0.64 1 d PD B 1 H27A H 0.1669 0.0149 0.4096 0.085 Uiso 0.64 1 calc PR B 1 C28A C 0.029(3) 0.011(2) 0.411(2) 0.152(19) Uiso 0.64 1 d PD B 1 H28A H 0.0053 0.0168 0.3700 0.227 Uiso 0.64 1 calc PR B 1 H28B H -0.0146 0.0270 0.4329 0.227 Uiso 0.64 1 calc PR B 1 H28C H 0.0354 -0.0273 0.4192 0.227 Uiso 0.64 1 calc PR B 1 C27B C 0.103(3) 0.064(4) 0.450(3) 0.20(5) Uiso 0.36 1 d PD B 2 H27B H 0.0828 0.0939 0.4736 0.246 Uiso 0.36 1 calc PR B 2 C28B C 0.011(4) 0.037(3) 0.419(3) 0.090(16) Uiso 0.36 1 d PD B 2 H28D H -0.0225 0.0616 0.3890 0.134 Uiso 0.36 1 calc PR B 2 H28E H -0.0292 0.0293 0.4462 0.134 Uiso 0.36 1 calc PR B 2 H28F H 0.0265 0.0040 0.4009 0.134 Uiso 0.36 1 calc PR B 2 O12 O 0.1406(10) 0.0892(5) 0.4069(6) 0.087(4) Uani 1 1 d D . . N5 N 0.1163(11) 0.2790(6) 0.4935(7) 0.078(4) Uani 1 1 d D . . C29A C 0.051(2) 0.2583(13) 0.4439(14) 0.083(11) Uiso 0.54 1 d PD B 1 H29A H 0.0536 0.2794 0.4090 0.100 Uiso 0.54 1 calc PR B 1 H29B H -0.0148 0.2587 0.4502 0.100 Uiso 0.54 1 calc PR B 1 C30A C 0.085(2) 0.2005(11) 0.4384(15) 0.070(8) Uiso 0.54 1 d PD B 1 H30A H 0.0762 0.1792 0.4721 0.084 Uiso 0.54 1 calc PR B 1 H30B H 0.0477 0.1837 0.4034 0.084 Uiso 0.54 1 calc PR B 1 C29B C 0.058(3) 0.2389(15) 0.4571(14) 0.067(10) Uiso 0.46 1 d PD B 2 H29C H -0.0062 0.2537 0.4440 0.080 Uiso 0.46 1 calc PR B 2 H29D H 0.0528 0.2068 0.4807 0.080 Uiso 0.46 1 calc PR B 2 C30B C 0.097(3) 0.222(2) 0.4039(15) 0.101(14) Uiso 0.46 1 d PD B 2 H30C H 0.0566 0.1938 0.3808 0.122 Uiso 0.46 1 calc PR B 2 H30D H 0.1058 0.2521 0.3791 0.122 Uiso 0.46 1 calc PR B 2 O13 O 0.1844(10) 0.2002(5) 0.4355(6) 0.088(4) Uani 1 1 d D . . C31A C 0.134(2) 0.3364(9) 0.4866(13) 0.063(8) Uiso 0.54 1 d PD B 1 H31A H 0.1624 0.3525 0.5242 0.075 Uiso 0.54 1 calc PR B 1 H31B H 0.0739 0.3552 0.4709 0.075 Uiso 0.54 1 calc PR B 1 C31B C 0.107(3) 0.3287(18) 0.461(3) 0.13(2) Uiso 0.46 1 d PD B 2 H31C H 0.0880 0.3581 0.4839 0.158 Uiso 0.46 1 calc PR B 2 H31D H 0.0573 0.3247 0.4254 0.158 Uiso 0.46 1 calc PR B 2 C32 C 0.2027(14) 0.3420(9) 0.4446(8) 0.081(5) Uani 1 1 d D . . H32A H 0.1721 0.3296 0.4057 0.097 Uiso 0.54 1 calc PR B 1 H32B H 0.2223 0.3798 0.4422 0.097 Uiso 0.54 1 calc PR B 1 H32C H 0.1935 0.3407 0.4022 0.097 Uiso 0.46 1 calc PR B 2 H32D H 0.2190 0.3794 0.4565 0.097 Uiso 0.46 1 calc PR B 2 O14 O 0.2774(9) 0.3111(4) 0.4665(5) 0.066(3) Uani 1 1 d . B . C33 C 0.0954(17) 0.2722(10) 0.5525(10) 0.102(7) Uani 1 1 d . B . H33A H 0.0651 0.2369 0.5553 0.122 Uiso 1 1 calc R . . H33B H 0.0514 0.3005 0.5598 0.122 Uiso 1 1 calc R . . C34 C 0.191(2) 0.2758(10) 0.5988(9) 0.119(10) Uani 1 1 d . . . H34A H 0.2135 0.3138 0.5997 0.143 Uiso 1 1 calc R B . C35 C 0.169(3) 0.2630(13) 0.6577(10) 0.139(11) Uani 1 1 d . B . H35A H 0.2277 0.2650 0.6871 0.208 Uiso 1 1 calc R . . H35B H 0.1428 0.2268 0.6572 0.208 Uiso 1 1 calc R . . H35C H 0.1235 0.2890 0.6666 0.208 Uiso 1 1 calc R . . O15 O 0.2563(13) 0.2453(6) 0.5826(6) 0.103(5) Uani 1 1 d . B . N6 N 0.4832(11) 0.3436(6) 0.5582(5) 0.067(4) Uani 1 1 d . . . C36 C 0.4653(15) 0.2987(7) 0.5958(6) 0.073(5) Uani 1 1 d . . . H36A H 0.4033 0.3038 0.6067 0.088 Uiso 1 1 calc R . . H36B H 0.5148 0.2983 0.6315 0.088 Uiso 1 1 calc R . . C37 C 0.4658(15) 0.2463(8) 0.5649(7) 0.080(5) Uani 1 1 d . B . H37A H 0.5313 0.2367 0.5624 0.096 Uiso 1 1 calc R . . H37B H 0.4406 0.2176 0.5864 0.096 Uiso 1 1 calc R . . O16 O 0.4092(8) 0.2510(4) 0.5092(4) 0.065(3) Uani 1 1 d . . . C38 C 0.5860(13) 0.3497(8) 0.5618(7) 0.077(5) Uani 1 1 d . . . H38A H 0.6185 0.3163 0.5772 0.093 Uiso 1 1 calc R . . H38B H 0.6102 0.3791 0.5887 0.093 Uiso 1 1 calc R . . C39 C 0.6082(13) 0.3617(7) 0.5032(6) 0.066(5) Uani 1 1 d . B . H39A H 0.5938 0.3997 0.4931 0.079 Uiso 1 1 calc R . . H39B H 0.6762 0.3556 0.5044 0.079 Uiso 1 1 calc R . . O17 O 0.5526(8) 0.3277(4) 0.4610(4) 0.054(3) Uani 1 1 d . . . C40 C 0.4305(16) 0.3931(8) 0.5665(7) 0.080(5) Uani 1 1 d . . . H40A H 0.4642 0.4118 0.6015 0.096 Uiso 1 1 calc R . . H40B H 0.3670 0.3831 0.5726 0.096 Uiso 1 1 calc R . . C41 C 0.4200(16) 0.4302(6) 0.5169(7) 0.080(6) Uani 1 1 d . B . H41A H 0.4836 0.4469 0.5192 0.096 Uiso 1 1 calc R . . C42 C 0.3547(17) 0.4743(8) 0.5161(9) 0.091(6) Uani 1 1 d . . . H42A H 0.3555 0.4970 0.4825 0.136 Uiso 1 1 calc R . . H42B H 0.3736 0.4956 0.5512 0.136 Uiso 1 1 calc R . . H42C H 0.2907 0.4602 0.5140 0.136 Uiso 1 1 calc R . . O18 O 0.4009(10) 0.4005(4) 0.4640(5) 0.078(4) Uani 1 1 d D . . O19 O 0.6049(7) 0.1753(4) 0.2273(4) 0.050(2) Uani 1 1 d . . . O20 O 0.7428(8) 0.1898(4) 0.2973(5) 0.058(3) Uani 1 1 d . . . O21 O 0.7501(9) 0.1337(5) 0.2140(5) 0.074(3) Uani 1 1 d . . . S1 S 0.7078(3) 0.17859(16) 0.23465(17) 0.0574(10) Uani 1 1 d . . . C43 C 0.7353(13) 0.2355(6) 0.1977(6) 0.060(4) Uani 1 1 d . . . C44 C 0.7965(15) 0.2340(8) 0.1607(8) 0.077(5) Uani 1 1 d . . . H44A H 0.8232 0.2009 0.1522 0.092 Uiso 1 1 calc R . . C45 C 0.8192(18) 0.2815(11) 0.1356(8) 0.098(7) Uani 1 1 d . . . H45A H 0.8642 0.2803 0.1115 0.117 Uiso 1 1 calc R . . C46 C 0.778(2) 0.3309(10) 0.1446(8) 0.099(8) Uani 1 1 d . . . C47 C 0.715(2) 0.3294(8) 0.1778(9) 0.101(9) Uani 1 1 d . . . H47A H 0.6854 0.3624 0.1839 0.121 Uiso 1 1 calc R . . C48 C 0.6866(14) 0.2843(7) 0.2047(8) 0.080(6) Uani 1 1 d . . . H48A H 0.6181 0.2786 0.1898 0.095 Uiso 1 1 calc R . . H48B H 0.6953 0.2920 0.2464 0.095 Uiso 1 1 calc R . . C49 C 0.801(3) 0.3801(10) 0.1182(10) 0.151(14) Uani 1 1 d . . . H49A H 0.8508 0.3732 0.0968 0.227 Uiso 1 1 calc R . . H49B H 0.8228 0.4069 0.1482 0.227 Uiso 1 1 calc R . . H49C H 0.7445 0.3936 0.0919 0.227 Uiso 1 1 calc R . . O22 O 0.6933(8) 0.3785(4) 0.3965(4) 0.060(3) Uani 1 1 d . . . O23 O 0.6167(8) 0.3778(4) 0.2977(4) 0.059(3) Uani 1 1 d . . . O24 O 0.7064(10) 0.4578(5) 0.3383(5) 0.081(4) Uani 1 1 d . . . S2 S 0.6996(3) 0.40089(15) 0.34082(16) 0.0601(11) Uani 1 1 d . B . C50 C 0.8017(13) 0.3725(7) 0.3236(6) 0.064(5) Uani 1 1 d . . . C51 C 0.8154(14) 0.3180(7) 0.3262(7) 0.065(5) Uani 1 1 d . B . H51A H 0.7710 0.2955 0.3392 0.078 Uiso 1 1 calc R . . C52 C 0.8930(14) 0.2962(9) 0.3102(8) 0.080(6) Uani 1 1 d . . . H52A H 0.9019 0.2585 0.3135 0.096 Uiso 1 1 calc R B . C53 C 0.9581(18) 0.3259(9) 0.2898(10) 0.087(6) Uani 1 1 d U B . C54 C 0.9461(17) 0.3823(10) 0.2891(9) 0.096(7) Uani 1 1 d . . . H54A H 0.9929 0.4047 0.2784 0.115 Uiso 1 1 calc R B . C55 C 0.8650(17) 0.4056(8) 0.3041(8) 0.081(6) Uani 1 1 d . B . H55A H 0.8544 0.4431 0.3007 0.097 Uiso 1 1 calc R . . C56 C 1.0434(19) 0.3026(12) 0.2707(14) 0.127(10) Uani 1 1 d . . . H56A H 1.0422 0.2634 0.2738 0.191 Uiso 1 1 calc R B . H56B H 1.1013 0.3164 0.2953 0.191 Uiso 1 1 calc R . . H56C H 1.0419 0.3128 0.2307 0.191 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 Yb1 0.0436(5) 0.0603(4) 0.0385(3) 0.0037(2) 0.0086(3) -0.0028(3) Yb2 0.0487(5) 0.0603(4) 0.0354(3) 0.0005(2) 0.0094(3) -0.0066(3) Fe1 0.0467(13) 0.0609(11) 0.0424(10) -0.0006(8) 0.0141(9) -0.0067(9) Fe2 0.0604(16) 0.0670(12) 0.0566(12) 0.0017(9) 0.0181(11) -0.0003(10) Fe3 0.0668(16) 0.0681(13) 0.0602(13) -0.0037(10) 0.0166(12) -0.0097(11) Fe4 0.0573(15) 0.0721(12) 0.0379(10) -0.0033(8) 0.0120(10) -0.0103(10) N1 0.049(8) 0.048(6) 0.056(7) 0.009(5) 0.009(6) -0.006(5) C1 0.065(11) 0.078(10) 0.046(7) 0.006(7) -0.008(8) -0.012(8) C2 0.048(9) 0.055(7) 0.062(8) -0.001(6) 0.008(7) -0.002(6) O1 0.044(6) 0.070(6) 0.041(5) 0.012(4) 0.005(4) 0.004(4) C3 0.069(12) 0.076(9) 0.043(7) 0.009(7) 0.002(8) -0.019(8) C4 0.040(10) 0.093(11) 0.043(7) -0.010(7) 0.007(7) -0.004(7) O2 0.061(7) 0.080(6) 0.028(4) -0.003(4) -0.005(5) -0.013(5) C5 0.058(10) 0.063(8) 0.053(8) 0.015(6) 0.005(8) 0.004(7) C6 0.041(9) 0.076(9) 0.057(8) -0.012(7) 0.003(7) 0.013(7) C7 0.068(12) 0.073(10) 0.087(12) 0.005(8) 0.043(10) 0.000(8) O3 0.043(6) 0.068(6) 0.052(5) 0.003(4) 0.011(5) 0.004(4) N2 0.059(8) 0.046(5) 0.048(6) 0.002(5) 0.017(6) 0.001(5) C8 0.069(11) 0.058(7) 0.032(6) -0.004(5) 0.008(7) 0.000(7) C9 0.041(8) 0.070(8) 0.037(6) -0.006(6) -0.001(6) 0.000(6) O4 0.045(6) 0.072(6) 0.036(4) 0.001(4) 0.005(4) 0.000(4) C10 0.035(9) 0.063(8) 0.054(8) -0.004(6) 0.003(7) 0.001(6) C11 0.053(10) 0.068(8) 0.056(8) 0.014(7) 0.005(7) -0.010(7) O5 0.049(6) 0.077(6) 0.041(5) -0.004(4) 0.001(5) -0.014(5) C12 0.071(11) 0.057(7) 0.040(7) 0.000(6) 0.006(7) -0.012(7) C13 0.088(13) 0.053(7) 0.054(8) -0.010(6) 0.011(8) 0.003(8) C14 0.076(13) 0.072(10) 0.075(11) -0.005(8) 0.019(10) 0.006(9) O6 0.078(8) 0.053(5) 0.043(5) -0.007(4) 0.016(5) 0.005(5) N3 0.059(10) 0.084(9) 0.065(8) -0.005(7) 0.013(7) -0.023(7) C15 0.096(16) 0.110(14) 0.045(8) -0.012(8) 0.030(10) -0.039(12) C16 0.048(10) 0.076(9) 0.053(8) -0.005(7) 0.022(7) -0.006(7) O7 0.044(6) 0.071(6) 0.041(5) -0.004(4) 0.021(5) 0.004(4) C17 0.041(11) 0.130(16) 0.063(10) -0.016(10) 0.005(9) -0.006(10) C18 0.080(14) 0.103(13) 0.062(10) 0.007(9) 0.003(10) -0.003(11) O8 0.066(8) 0.068(6) 0.056(6) 0.007(5) 0.008(5) -0.001(5) C19 0.082(14) 0.081(11) 0.070(10) -0.017(9) 0.001(10) -0.010(9) C20 0.067(13) 0.094(13) 0.086(12) -0.031(10) 0.017(10) -0.029(10) C21 0.102(17) 0.092(13) 0.098(14) -0.047(11) 0.054(13) -0.012(11) O9 0.073(8) 0.064(6) 0.067(6) -0.007(5) 0.027(6) -0.012(5) N4 0.062(10) 0.088(9) 0.063(8) 0.011(7) 0.027(8) -0.008(7) C22 0.103(17) 0.083(12) 0.088(13) 0.016(10) 0.056(13) 0.017(11) C23 0.080(14) 0.078(11) 0.081(11) 0.028(9) 0.031(11) 0.011(9) O10 0.050(7) 0.076(6) 0.048(5) 0.013(4) 0.028(5) 0.009(5) C24 0.12(2) 0.104(15) 0.099(16) 0.034(13) 0.042(15) -0.003(13) O11 0.171(16) 0.069(7) 0.063(7) 0.005(6) 0.029(9) 0.015(8) C26 0.085(16) 0.124(17) 0.096(15) -0.008(13) 0.035(13) -0.019(13) O12 0.076(9) 0.101(9) 0.083(8) -0.006(7) 0.018(7) -0.016(7) N5 0.073(11) 0.095(10) 0.078(9) -0.001(8) 0.041(9) -0.007(8) O13 0.088(10) 0.092(8) 0.078(8) -0.010(7) 0.006(7) -0.005(7) C32 0.068(14) 0.105(13) 0.077(12) 0.001(10) 0.030(11) -0.001(11) O14 0.056(8) 0.075(6) 0.074(7) 0.006(5) 0.033(6) -0.004(5) C33 0.091(17) 0.119(17) 0.107(17) -0.013(13) 0.047(15) -0.014(13) C34 0.17(3) 0.098(15) 0.069(12) -0.028(11) -0.020(15) 0.018(16) C35 0.19(3) 0.17(3) 0.075(14) 0.006(15) 0.060(18) 0.01(2) O15 0.144(14) 0.086(9) 0.074(8) -0.021(7) 0.012(9) 0.008(9) N6 0.079(11) 0.088(9) 0.035(6) -0.012(6) 0.016(7) -0.027(8) C36 0.097(15) 0.082(10) 0.040(7) -0.002(7) 0.012(9) -0.012(10) C37 0.090(14) 0.090(12) 0.056(9) 0.000(8) 0.006(10) -0.013(10) O16 0.074(8) 0.071(6) 0.050(5) 0.003(5) 0.010(5) -0.009(5) C38 0.066(13) 0.108(13) 0.060(9) -0.023(9) 0.016(9) -0.038(10) C39 0.066(11) 0.080(10) 0.051(8) -0.014(7) 0.007(8) -0.033(8) O17 0.057(7) 0.063(5) 0.040(5) 0.002(4) 0.003(5) -0.010(4) C40 0.100(16) 0.090(12) 0.058(9) -0.010(9) 0.033(10) -0.005(11) C41 0.115(17) 0.058(9) 0.066(10) -0.013(8) 0.017(10) 0.013(9) C42 0.110(18) 0.084(12) 0.079(12) -0.006(10) 0.018(12) -0.008(11) O18 0.117(11) 0.068(6) 0.055(6) 0.001(5) 0.028(7) -0.005(6) O19 0.046(7) 0.068(6) 0.037(5) 0.001(4) 0.015(5) -0.001(4) O20 0.046(6) 0.067(6) 0.063(6) -0.002(5) 0.019(5) 0.005(5) O21 0.068(8) 0.097(8) 0.065(7) 0.010(6) 0.036(6) 0.022(6) S1 0.049(3) 0.074(2) 0.053(2) 0.0029(16) 0.018(2) 0.0064(17) C43 0.060(11) 0.074(9) 0.049(8) -0.005(7) 0.017(9) -0.002(8) C44 0.070(13) 0.092(12) 0.081(12) 0.017(9) 0.048(12) -0.006(9) C45 0.107(19) 0.14(2) 0.061(11) 0.003(12) 0.056(12) -0.023(15) C46 0.13(2) 0.115(17) 0.048(10) 0.012(10) 0.008(12) -0.056(15) C47 0.16(2) 0.078(12) 0.057(10) 0.013(9) -0.004(14) -0.029(13) C48 0.081(14) 0.075(10) 0.078(11) 0.021(9) 0.004(10) -0.013(9) C49 0.25(4) 0.115(18) 0.078(14) 0.021(13) 0.017(19) -0.09(2) O22 0.061(7) 0.072(6) 0.049(5) 0.004(4) 0.015(5) -0.007(5) O23 0.073(8) 0.065(6) 0.040(5) 0.007(4) 0.012(5) -0.012(5) O24 0.085(9) 0.082(7) 0.080(8) -0.001(6) 0.024(7) -0.027(6) S2 0.062(3) 0.066(2) 0.0496(19) 0.0033(15) 0.0059(19) -0.0170(18) C50 0.058(12) 0.095(12) 0.046(8) 0.004(7) 0.026(8) -0.023(9) C51 0.049(12) 0.084(11) 0.064(10) 0.005(8) 0.018(9) -0.009(8) C52 0.058(13) 0.108(14) 0.066(10) 0.010(10) -0.003(10) -0.013(11) C53 0.081(10) 0.102(9) 0.085(9) 0.003(7) 0.036(8) -0.001(8) C54 0.067(15) 0.15(2) 0.079(13) -0.002(12) 0.038(12) -0.050(14) C55 0.094(17) 0.091(12) 0.066(10) -0.006(9) 0.036(12) -0.027(11) C56 0.086(19) 0.16(2) 0.15(3) -0.02(2) 0.071(19) -0.008(17) _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 Yb1 O4 2.202(9) . ? Yb1 O2 2.226(11) . ? Yb1 O1 2.237(9) . ? Yb1 O7 2.269(10) . ? Yb1 O3 2.406(10) . ? Yb1 O20 2.435(11) . ? Yb1 O19 2.453(9) . ? Yb1 N1 2.555(11) . ? Yb2 O5 2.208(11) . ? Yb2 O1 2.223(9) . ? Yb2 O4 2.276(9) . ? Yb2 O17 2.278(10) . ? Yb2 O6 2.417(9) . ? Yb2 O23 2.426(10) . ? Yb2 O22 2.487(10) . ? Yb2 N2 2.550(11) . ? Fe1 O9 1.969(11) . ? Fe1 O2 1.971(9) . ? Fe1 O8 1.993(12) . ? Fe1 O7 2.006(10) . ? Fe1 O10 2.023(10) . ? Fe1 N3 2.255(13) . ? Fe2 O12 1.903(13) . ? Fe2 O11 1.973(13) . ? Fe2 O10 2.002(11) . ? Fe2 O13 2.040(14) . ? Fe2 O8 2.044(11) . ? Fe2 N4 2.393(14) . ? Fe3 O15 1.931(14) . ? Fe3 O14 1.997(11) . ? Fe3 O11 2.030(13) . ? Fe3 O13 2.033(12) . ? Fe3 O16 2.075(12) . ? Fe3 N5 2.330(17) . ? Fe4 O5 1.981(10) . ? Fe4 O18 2.005(11) . ? Fe4 O16 2.006(10) . ? Fe4 O17 2.012(12) . ? Fe4 O14 2.019(12) . ? Fe4 N6 2.236(11) . ? N1 C3 1.41(2) . ? N1 C5 1.47(2) . ? N1 C1 1.497(19) . ? C1 C2 1.50(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.453(16) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.57(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.411(16) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.49(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O3 1.451(16) . ? C6 C7 1.53(2) . ? C6 H6A 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O3 H3 0.96(3) . ? N2 C12 1.456(17) . ? N2 C8 1.503(18) . ? N2 C10 1.52(2) . ? C8 C9 1.486(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O4 1.456(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.488(19) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O5 1.382(16) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.56(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O6 1.424(18) . ? C13 C14 1.51(2) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O6 H6 0.98(3) . ? N3 C19 1.47(2) . ? N3 C17 1.48(2) . ? N3 C15 1.50(2) . ? C15 C16 1.45(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O7 1.410(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.48(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O8 1.470(19) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.51(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O9 1.432(19) . ? C20 C21 1.48(3) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N4 C26 1.37(3) . ? N4 C24 1.44(3) . ? N4 C22 1.46(2) . ? C22 C23 1.50(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O10 1.396(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25A 1.44(3) . ? C24 C25B 1.44(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 0.9900 . ? C24 H24D 0.9900 . ? C25A O11 1.45(2) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C25B O11 1.46(3) . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C26 C27B 1.49(4) . ? C26 C27A 1.50(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 H26C 0.9900 . ? C26 H26D 0.9900 . ? C27A O12 1.41(3) . ? C27A C28A 1.54(5) . ? C27A H27A 1.0000 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C27B O12 1.41(3) . ? C27B C28B 1.54(5) . ? C27B H27B 1.0000 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? N5 C29A 1.45(2) . ? N5 C31B 1.45(2) . ? N5 C29B 1.47(2) . ? N5 C31A 1.47(2) . ? N5 C33 1.50(3) . ? C29A C30A 1.54(3) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C30A O13 1.45(3) . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? C29B C30B 1.54(3) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30B O13 1.44(3) . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31A C32 1.55(3) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C31B C32 1.55(3) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32 O14 1.34(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 H32C 0.9900 . ? C32 H32D 0.9900 . ? C33 C34 1.58(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O15 1.33(3) . ? C34 C35 1.53(3) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N6 C38 1.48(2) . ? N6 C40 1.48(2) . ? N6 C36 1.49(2) . ? C36 C37 1.50(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O16 1.412(19) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.52(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O17 1.430(15) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.48(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O18 1.435(19) . ? C41 C42 1.45(3) . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O19 S1 1.463(11) . ? O20 S1 1.497(11) . ? O21 S1 1.412(12) . ? C43 C44 1.37(3) . ? C43 C48 1.43(3) . ? C44 C45 1.40(3) . ? C44 H44A 0.9500 . ? C45 C46 1.41(4) . ? C45 H45A 0.9500 . ? C46 C47 1.32(4) . ? C46 C49 1.45(3) . ? C47 C48 1.39(3) . ? C47 H47A 0.9500 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? O22 S2 1.457(11) . ? O23 S2 1.521(10) . ? O24 S2 1.426(12) . ? C50 C51 1.37(2) . ? C50 C55 1.38(2) . ? C51 C52 1.37(3) . ? C51 H51A 0.9500 . ? C52 C53 1.36(3) . ? C52 H52A 0.9500 . ? C53 C54 1.42(3) . ? C53 C56 1.51(3) . ? C54 C55 1.42(3) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? 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 Yb1 O2 102.8(4) . . ? O4 Yb1 O1 68.0(3) . . ? O2 Yb1 O1 86.4(3) . . ? O4 Yb1 O7 83.8(3) . . ? O2 Yb1 O7 67.8(3) . . ? O1 Yb1 O7 136.6(3) . . ? O4 Yb1 O3 155.8(3) . . ? O2 Yb1 O3 83.2(4) . . ? O1 Yb1 O3 136.2(3) . . ? O7 Yb1 O3 76.7(3) . . ? O4 Yb1 O20 103.8(4) . . ? O2 Yb1 O20 147.9(3) . . ? O1 Yb1 O20 87.2(4) . . ? O7 Yb1 O20 132.7(3) . . ? O3 Yb1 O20 79.9(3) . . ? O4 Yb1 O19 82.6(3) . . ? O2 Yb1 O19 144.5(3) . . ? O1 Yb1 O19 127.0(3) . . ? O7 Yb1 O19 78.2(3) . . ? O3 Yb1 O19 79.4(3) . . ? O20 Yb1 O19 57.4(3) . . ? O4 Yb1 N1 137.0(3) . . ? O2 Yb1 N1 69.9(4) . . ? O1 Yb1 N1 69.2(3) . . ? O7 Yb1 N1 126.6(4) . . ? O3 Yb1 N1 67.2(3) . . ? O20 Yb1 N1 78.4(4) . . ? O19 Yb1 N1 128.5(4) . . ? O5 Yb2 O1 105.2(4) . . ? O5 Yb2 O4 88.5(4) . . ? O1 Yb2 O4 67.0(3) . . ? O5 Yb2 O17 67.6(3) . . ? O1 Yb2 O17 84.1(4) . . ? O4 Yb2 O17 136.3(3) . . ? O5 Yb2 O6 82.4(4) . . ? O1 Yb2 O6 156.0(3) . . ? O4 Yb2 O6 136.7(3) . . ? O17 Yb2 O6 77.9(3) . . ? O5 Yb2 O23 146.7(4) . . ? O1 Yb2 O23 101.4(4) . . ? O4 Yb2 O23 83.8(3) . . ? O17 Yb2 O23 135.6(3) . . ? O6 Yb2 O23 81.2(4) . . ? O5 Yb2 O22 145.5(3) . . ? O1 Yb2 O22 81.6(3) . . ? O4 Yb2 O22 124.3(4) . . ? O17 Yb2 O22 79.8(3) . . ? O6 Yb2 O22 79.8(4) . . ? O23 Yb2 O22 58.0(3) . . ? O5 Yb2 N2 70.0(4) . . ? O1 Yb2 N2 136.8(3) . . ? O4 Yb2 N2 69.9(3) . . ? O17 Yb2 N2 127.6(4) . . ? O6 Yb2 N2 67.1(3) . . ? O23 Yb2 N2 76.9(4) . . ? O22 Yb2 N2 127.5(3) . . ? O9 Fe1 O2 102.1(5) . . ? O9 Fe1 O8 149.7(5) . . ? O2 Fe1 O8 105.9(5) . . ? O9 Fe1 O7 92.2(4) . . ? O2 Fe1 O7 78.1(4) . . ? O8 Fe1 O7 104.5(4) . . ? O9 Fe1 O10 91.2(4) . . ? O2 Fe1 O10 96.8(4) . . ? O8 Fe1 O10 74.4(4) . . ? O7 Fe1 O10 174.4(4) . . ? O9 Fe1 N3 78.9(5) . . ? O2 Fe1 N3 157.5(5) . . ? O8 Fe1 N3 79.6(5) . . ? O7 Fe1 N3 79.3(5) . . ? O10 Fe1 N3 105.7(5) . . ? O12 Fe2 O11 129.6(7) . . ? O12 Fe2 O10 113.8(5) . . ? O11 Fe2 O10 98.0(6) . . ? O12 Fe2 O13 94.3(6) . . ? O11 Fe2 O13 73.4(5) . . ? O10 Fe2 O13 147.9(5) . . ? O12 Fe2 O8 102.0(5) . . ? O11 Fe2 O8 124.7(6) . . ? O10 Fe2 O8 73.8(4) . . ? O13 Fe2 O8 85.8(5) . . ? O12 Fe2 N4 77.2(6) . . ? O11 Fe2 N4 75.1(5) . . ? O10 Fe2 N4 74.3(5) . . ? O13 Fe2 N4 129.7(6) . . ? O8 Fe2 N4 144.5(5) . . ? O15 Fe3 O14 113.1(6) . . ? O15 Fe3 O11 91.6(6) . . ? O14 Fe3 O11 150.1(6) . . ? O15 Fe3 O13 131.6(7) . . ? O14 Fe3 O13 100.4(5) . . ? O11 Fe3 O13 72.3(6) . . ? O15 Fe3 O16 100.7(6) . . ? O14 Fe3 O16 74.7(5) . . ? O11 Fe3 O16 84.6(6) . . ? O13 Fe3 O16 121.9(5) . . ? O15 Fe3 N5 79.6(6) . . ? O14 Fe3 N5 75.5(5) . . ? O11 Fe3 N5 127.9(6) . . ? O13 Fe3 N5 76.1(5) . . ? O16 Fe3 N5 147.5(5) . . ? O5 Fe4 O18 104.0(4) . . ? O5 Fe4 O16 104.0(4) . . ? O18 Fe4 O16 150.0(5) . . ? O5 Fe4 O17 77.4(4) . . ? O18 Fe4 O17 90.7(5) . . ? O16 Fe4 O17 105.5(4) . . ? O5 Fe4 O14 96.6(5) . . ? O18 Fe4 O14 90.8(5) . . ? O16 Fe4 O14 75.8(5) . . ? O17 Fe4 O14 174.0(4) . . ? O5 Fe4 N6 156.9(5) . . ? O18 Fe4 N6 79.2(5) . . ? O16 Fe4 N6 79.1(5) . . ? O17 Fe4 N6 79.7(5) . . ? O14 Fe4 N6 106.2(5) . . ? C3 N1 C5 113.8(12) . . ? C3 N1 C1 113.0(12) . . ? C5 N1 C1 108.4(13) . . ? C3 N1 Yb1 109.7(9) . . ? C5 N1 Yb1 106.6(8) . . ? C1 N1 Yb1 104.8(7) . . ? N1 C1 C2 111.0(13) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? O1 C2 C1 108.9(11) . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 O1 Yb2 123.1(8) . . ? C2 O1 Yb1 124.5(8) . . ? Yb2 O1 Yb1 110.3(4) . . ? N1 C3 C4 114.5(12) . . ? N1 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? O2 C4 C3 106.4(13) . . ? O2 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? O2 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.6 . . ? C4 O2 Fe1 130.8(10) . . ? C4 O2 Yb1 119.3(10) . . ? Fe1 O2 Yb1 106.5(4) . . ? N1 C5 C6 114.0(13) . . ? N1 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N1 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? O3 C6 C5 109.5(12) . . ? O3 C6 C7 107.8(12) . . ? C5 C6 C7 114.6(14) . . ? O3 C6 H6A 108.3 . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6A 108.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 O3 Yb1 121.6(8) . . ? C6 O3 H3 103(9) . . ? Yb1 O3 H3 109(9) . . ? C12 N2 C8 108.6(11) . . ? C12 N2 C10 113.4(12) . . ? C8 N2 C10 111.8(11) . . ? C12 N2 Yb2 109.0(8) . . ? C8 N2 Yb2 105.3(8) . . ? C10 N2 Yb2 108.4(7) . . ? C9 C8 N2 110.6(11) . . ? C9 C8 H8A 109.5 . . ? N2 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O4 C9 C8 110.7(10) . . ? O4 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? O4 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 O4 Yb1 126.1(8) . . ? C9 O4 Yb2 121.6(8) . . ? Yb1 O4 Yb2 109.6(3) . . ? C11 C10 N2 112.0(12) . . ? C11 C10 H10A 109.2 . . ? N2 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? N2 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O5 C11 C10 110.9(12) . . ? O5 C11 Yb2 38.3(7) . . ? C10 C11 Yb2 85.6(9) . . ? O5 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? Yb2 C11 H11A 147.2 . . ? O5 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? Yb2 C11 H11B 93.0 . . ? H11A C11 H11B 108.1 . . ? C11 O5 Fe4 130.9(10) . . ? C11 O5 Yb2 118.9(9) . . ? Fe4 O5 Yb2 107.3(4) . . ? N2 C12 C13 109.9(11) . . ? N2 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? N2 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O6 C13 C14 108.9(13) . . ? O6 C13 C12 108.8(12) . . ? C14 C13 C12 108.8(14) . . ? O6 C13 H13A 110.1 . . ? C14 C13 H13A 110.1 . . ? C12 C13 H13A 110.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 O6 Yb2 122.2(7) . . ? C13 O6 H6 103(10) . . ? Yb2 O6 H6 108(9) . . ? C19 N3 C17 114.0(15) . . ? C19 N3 C15 115.1(16) . . ? C17 N3 C15 110.9(15) . . ? C19 N3 Fe1 101.6(9) . . ? C17 N3 Fe1 106.9(10) . . ? C15 N3 Fe1 107.4(9) . . ? C16 C15 N3 111.6(14) . . ? C16 C15 H15A 109.3 . . ? N3 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? N3 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? O7 C16 C15 113.7(14) . . ? O7 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? O7 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C16 O7 Fe1 113.7(9) . . ? C16 O7 Yb1 127.0(9) . . ? Fe1 O7 Yb1 103.7(4) . . ? N3 C17 C18 108.8(15) . . ? N3 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N3 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? O8 C18 C17 109.0(15) . . ? O8 C18 H18A 109.9 . . ? C17 C18 H18A 109.9 . . ? O8 C18 H18B 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C18 O8 Fe1 113.7(11) . . ? C18 O8 Fe2 116.8(11) . . ? Fe1 O8 Fe2 105.6(5) . . ? N3 C19 C20 111.6(16) . . ? N3 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? N3 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? O9 C20 C21 110.6(16) . . ? O9 C20 C19 107.7(15) . . ? C21 C20 C19 113.3(17) . . ? O9 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? C19 C20 H20A 108.4 . . ? 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 . . ? C20 O9 Fe1 120.2(11) . . ? C26 N4 C24 112.0(18) . . ? C26 N4 C22 114.6(18) . . ? C24 N4 C22 113.2(17) . . ? C26 N4 Fe2 104.1(13) . . ? C24 N4 Fe2 106.2(11) . . ? C22 N4 Fe2 105.6(10) . . ? N4 C22 C23 112.2(16) . . ? N4 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? N4 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O10 C23 C22 107.2(15) . . ? O10 C23 H23A 110.3 . . ? C22 C23 H23A 110.3 . . ? O10 C23 H23B 110.3 . . ? C22 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? C23 O10 Fe2 124.0(11) . . ? C23 O10 Fe1 129.9(11) . . ? Fe2 O10 Fe1 106.1(4) . . ? N4 C24 C25A 113.8(19) . . ? N4 C24 C25B 114(3) . . ? N4 C24 H24A 108.8 . . ? C25A C24 H24A 108.8 . . ? N4 C24 H24B 108.8 . . ? C25A C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? N4 C24 H24C 108.7 . . ? C25B C24 H24C 108.7 . . ? N4 C24 H24D 108.7 . . ? C25B C24 H24D 108.7 . . ? H24C C24 H24D 107.6 . . ? C24 C25A O11 108.5(18) . . ? C24 C25A H25A 110.0 . . ? O11 C25A H25A 110.0 . . ? C24 C25A H25B 110.0 . . ? O11 C25A H25B 110.0 . . ? H25A C25A H25B 108.4 . . ? C24 C25B O11 108(2) . . ? C24 C25B H25C 110.1 . . ? O11 C25B H25C 110.1 . . ? C24 C25B H25D 110.1 . . ? O11 C25B H25D 110.1 . . ? H25C C25B H25D 108.4 . . ? C25A O11 Fe2 120.2(12) . . ? C25B O11 Fe2 117(2) . . ? C25A O11 Fe3 134.1(13) . . ? C25B O11 Fe3 114.7(15) . . ? Fe2 O11 Fe3 105.7(6) . . ? N4 C26 C27B 116(3) . . ? N4 C26 C27A 113(2) . . ? N4 C26 H26A 109.0 . . ? C27A C26 H26A 109.0 . . ? N4 C26 H26B 109.0 . . ? C27A C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? N4 C26 H26C 108.4 . . ? C27B C26 H26C 108.4 . . ? N4 C26 H26D 108.4 . . ? C27B C26 H26D 108.4 . . ? H26C C26 H26D 107.5 . . ? O12 C27A C26 111(2) . . ? O12 C27A C28A 119(3) . . ? C26 C27A C28A 118(3) . . ? O12 C27A H27A 101.8 . . ? C26 C27A H27A 101.8 . . ? C28A C27A H27A 101.8 . . ? C27A C28A H28A 109.5 . . ? C27A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C27A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? O12 C27B C26 111(3) . . ? O12 C27B C28B 105(5) . . ? C26 C27B C28B 121(6) . . ? O12 C27B H27B 106.0 . . ? C26 C27B H27B 106.0 . . ? C28B C27B H27B 106.0 . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B O12 Fe2 114(3) . . ? C27A O12 Fe2 120.9(14) . . ? C31B N5 C29B 107(3) . . ? C29A N5 C31A 111(2) . . ? C29A N5 C33 120(2) . . ? C31B N5 C33 126(3) . . ? C29B N5 C33 105.8(19) . . ? C31A N5 C33 106.8(16) . . ? C29A N5 Fe3 111.3(16) . . ? C31B N5 Fe3 113.0(15) . . ? C29B N5 Fe3 100.1(18) . . ? C31A N5 Fe3 103.9(14) . . ? C33 N5 Fe3 102.8(13) . . ? N5 C29A C30A 104(2) . . ? N5 C29A H29A 111.1 . . ? C30A C29A H29A 111.1 . . ? N5 C29A H29B 111.1 . . ? C30A C29A H29B 111.1 . . ? H29A C29A H29B 109.0 . . ? O13 C30A C29A 110(2) . . ? O13 C30A H30A 109.6 . . ? C29A C30A H30A 109.6 . . ? O13 C30A H30B 109.6 . . ? C29A C30A H30B 109.6 . . ? H30A C30A H30B 108.1 . . ? N5 C29B C30B 115(3) . . ? N5 C29B H29C 108.6 . . ? C30B C29B H29C 108.6 . . ? N5 C29B H29D 108.6 . . ? C30B C29B H29D 108.6 . . ? H29C C29B H29D 107.6 . . ? O13 C30B C29B 96(3) . . ? O13 C30B H30C 112.6 . . ? C29B C30B H30C 112.6 . . ? O13 C30B H30D 112.6 . . ? C29B C30B H30D 112.6 . . ? H30C C30B H30D 110.1 . . ? C30B O13 Fe3 122(2) . . ? C30A O13 Fe3 111.9(15) . . ? C30B O13 Fe2 134(2) . . ? C30A O13 Fe2 119.3(14) . . ? Fe3 O13 Fe2 103.1(6) . . ? N5 C31A C32 108.0(18) . . ? N5 C31A H31A 110.1 . . ? C32 C31A H31A 110.1 . . ? N5 C31A H31B 110.1 . . ? C32 C31A H31B 110.1 . . ? H31A C31A H31B 108.4 . . ? N5 C31B C32 109(2) . . ? N5 C31B H31C 109.9 . . ? C32 C31B H31C 109.9 . . ? N5 C31B H31D 109.9 . . ? C32 C31B H31D 109.9 . . ? H31C C31B H31D 108.3 . . ? O14 C32 C31B 118.1(18) . . ? O14 C32 C31A 105.7(18) . . ? O14 C32 H32A 110.6 . . ? C31A C32 H32A 110.6 . . ? O14 C32 H32B 110.6 . . ? C31A C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? O14 C32 H32C 107.8 . . ? C31B C32 H32C 107.8 . . ? O14 C32 H32D 107.8 . . ? C31B C32 H32D 107.8 . . ? H32C C32 H32D 107.1 . . ? C32 O14 Fe3 122.8(12) . . ? C32 O14 Fe4 131.2(11) . . ? Fe3 O14 Fe4 105.9(5) . . ? N5 C33 C34 109.1(19) . . ? N5 C33 H33A 109.9 . . ? C34 C33 H33A 109.9 . . ? N5 C33 H33B 109.9 . . ? C34 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O15 C34 C35 116(2) . . ? O15 C34 C33 109.7(17) . . ? C35 C34 C33 108(3) . . ? O15 C34 H34A 107.7 . . ? C35 C34 H34A 107.7 . . ? C33 C34 H34A 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 O15 Fe3 121.1(13) . . ? C38 N6 C40 116.4(15) . . ? C38 N6 C36 109.8(15) . . ? C40 N6 C36 113.0(15) . . ? C38 N6 Fe4 108.1(9) . . ? C40 N6 Fe4 102.1(10) . . ? C36 N6 Fe4 106.7(9) . . ? N6 C36 C37 110.2(13) . . ? N6 C36 H36A 109.6 . . ? C37 C36 H36A 109.6 . . ? N6 C36 H36B 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? O16 C37 C36 109.0(15) . . ? O16 C37 H37A 109.9 . . ? C36 C37 H37A 109.9 . . ? O16 C37 H37B 109.9 . . ? C36 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? C37 O16 Fe4 116.8(10) . . ? C37 O16 Fe3 115.9(11) . . ? Fe4 O16 Fe3 103.5(5) . . ? N6 C38 C39 111.5(14) . . ? N6 C38 H38A 109.3 . . ? C39 C38 H38A 109.3 . . ? N6 C38 H38B 109.3 . . ? C39 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? O17 C39 C38 109.3(12) . . ? O17 C39 H39A 109.8 . . ? C38 C39 H39A 109.8 . . ? O17 C39 H39B 109.8 . . ? C38 C39 H39B 109.8 . . ? H39A C39 H39B 108.3 . . ? C39 O17 Fe4 114.3(10) . . ? C39 O17 Yb2 128.2(9) . . ? Fe4 O17 Yb2 103.6(4) . . ? N6 C40 C41 112.7(15) . . ? N6 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? N6 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? O18 C41 C42 111.9(16) . . ? O18 C41 C40 110.0(13) . . ? C42 C41 C40 116.5(18) . . ? O18 C41 H41A 105.9 . . ? C42 C41 H41A 105.9 . . ? C40 C41 H41A 105.9 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 O18 Fe4 118.2(9) . . ? S1 O19 Yb1 99.0(5) . . ? S1 O20 Yb1 98.7(5) . . ? O21 S1 O19 114.6(7) . . ? O21 S1 O20 114.3(7) . . ? O19 S1 O20 104.9(6) . . ? C44 C43 C48 119.7(17) . . ? C44 C43 S1 122.7(14) . . ? C48 C43 S1 117.5(14) . . ? C43 C44 C45 119(2) . . ? C43 C44 H44A 120.3 . . ? C45 C44 H44A 120.3 . . ? C44 C45 C46 122(2) . . ? C44 C45 H45A 118.8 . . ? C46 C45 H45A 118.8 . . ? C47 C46 C45 116(2) . . ? C47 C46 C49 122(3) . . ? C45 C46 C49 122(3) . . ? C46 C47 C48 127(2) . . ? C46 C47 H47A 116.7 . . ? C48 C47 H47A 116.7 . . ? C47 C48 C43 116(2) . . ? C47 C48 H48A 108.3 . . ? C43 C48 H48A 108.3 . . ? C47 C48 H48B 108.3 . . ? C43 C48 H48B 108.3 . . ? H48A C48 H48B 107.4 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? S2 O22 Yb2 97.5(5) . . ? S2 O23 Yb2 98.2(4) . . ? O24 S2 O22 116.0(7) . . ? O24 S2 O23 113.5(7) . . ? O22 S2 O23 106.3(6) . . ? C51 C50 C55 120.5(19) . . ? C51 C50 S2 120.5(14) . . ? C55 C50 S2 118.9(16) . . ? C52 C51 C50 120.0(17) . . ? C52 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C53 C52 C51 123(2) . . ? C53 C52 H52A 118.4 . . ? C51 C52 H52A 118.4 . . ? C52 C53 C54 117(2) . . ? C52 C53 C56 124(2) . . ? C54 C53 C56 119(2) . . ? C53 C54 C55 120.6(19) . . ? C53 C54 H54A 119.7 . . ? C55 C54 H54A 119.7 . . ? C50 C55 C54 119(2) . . ? C50 C55 H55A 120.7 . . ? C54 C55 H55A 120.7 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O9 0.96(3) 1.58(3) 2.525(16) 170(15) . O6 H6 O18 0.98(3) 1.58(3) 2.552(16) 171(14) . _diffrn_measured_fraction_theta_max 0.777 _diffrn_reflns_theta_full 28.81 _diffrn_measured_fraction_theta_full 0.777 _refine_diff_density_max 3.393 _refine_diff_density_min -2.947 _refine_diff_density_rms 0.217 _database_code_depnum_ccdc_archive 'CCDC 912848' ####################################################################### # # 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_ambf10ybs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C140 H290 Fe10 N30 O90 Yb10, 21(C2 H3 N)' _chemical_formula_sum 'C182 H353 Fe10 N51 O90 Yb10' _chemical_formula_weight 6985.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.5530(12) _cell_length_b 20.5964(13) _cell_length_c 21.1312(16) _cell_angle_alpha 108.791(5) _cell_angle_beta 101.118(6) _cell_angle_gamma 95.993(5) _cell_volume 6583.9(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38566 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 26.31 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3482 _exptl_absorpt_coefficient_mu 4.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.353 _exptl_absorpt_correction_T_max 0.502 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62927 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.02 _reflns_number_total 25727 _reflns_number_gt 15716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. O-H distances were restrained: DFIX 0.92 0.04 O3 H3 O9 H9 O15 H15 O21 H21 O27 H27 The lattice MeCN was badly disordered and treated using SQUEEZE: ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 99 44 '1 MeCN ' 2 -0.008 0.500 0.489 1767 421 '20 MeCN ' _platon_squeeze_details ; Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13 ; _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^)+(0.0518P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25727 _refine_ls_number_parameters 1276 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 Yb1 Yb 0.15473(2) 0.823284(16) 0.405657(15) 0.05423(9) Uani 1 1 d . . . Yb2 Yb -0.00235(2) 0.511641(17) 0.238352(18) 0.06092(9) Uani 1 1 d . . . Yb3 Yb 0.23322(2) 0.339230(18) 0.091731(19) 0.06549(10) Uani 1 1 d . . . Yb4 Yb 0.33703(2) 0.090863(18) 0.172421(17) 0.06011(9) Uani 1 1 d . . . Yb5 Yb 0.71196(2) 0.091236(18) 0.281050(16) 0.06132(10) Uani 1 1 d . . . Fe1 Fe 0.11817(7) 0.67060(5) 0.27422(5) 0.0583(3) Uani 1 1 d . . . Fe2 Fe 0.07594(7) 0.36622(5) 0.17572(5) 0.0577(3) Uani 1 1 d . . . Fe3 Fe 0.36324(7) 0.23253(6) 0.12361(7) 0.0684(3) Uani 1 1 d . . . Fe4 Fe 0.50191(7) 0.05522(7) 0.26790(6) 0.0729(3) Uani 1 1 d . . . Fe5 Fe 0.85697(7) 0.16201(6) 0.43141(5) 0.0598(3) Uani 1 1 d . . . N1 N 0.0205(4) 0.8612(3) 0.3610(3) 0.0637(17) Uani 1 1 d . . . C1 C -0.0201(7) 0.8892(6) 0.4170(4) 0.093(3) Uani 1 1 d . . . H1A H -0.0637 0.8519 0.4160 0.112 Uiso 1 1 calc R . . H1B H -0.0482 0.9269 0.4091 0.112 Uiso 1 1 calc R . . C2 C 0.0390(5) 0.9172(4) 0.4868(4) 0.071(2) Uani 1 1 d . . . H2A H 0.0723 0.9628 0.4937 0.086 Uiso 1 1 calc R . . H2B H 0.0072 0.9239 0.5229 0.086 Uiso 1 1 calc R . . O1 O 0.0931(3) 0.8683(2) 0.4914(2) 0.0600(13) Uani 1 1 d . . . C3 C -0.0354(6) 0.7983(5) 0.3056(6) 0.097(3) Uani 1 1 d . . . H3A H -0.0941 0.8055 0.3000 0.116 Uiso 1 1 calc R . . H3B H -0.0199 0.7923 0.2614 0.116 Uiso 1 1 calc R . . C4 C -0.0283(5) 0.7339(4) 0.3225(5) 0.076(2) Uani 1 1 d . . . H4A H -0.0513 0.7365 0.3631 0.091 Uiso 1 1 calc R . . H4B H -0.0606 0.6925 0.2832 0.091 Uiso 1 1 calc R . . O2 O 0.0579(3) 0.7281(2) 0.3371(2) 0.0568(12) Uani 1 1 d . . . C5 C 0.0433(6) 0.9131(5) 0.3313(5) 0.090(3) Uani 1 1 d . . . H5A H 0.0684 0.9578 0.3693 0.108 Uiso 1 1 calc R . . H5B H -0.0084 0.9203 0.3039 0.108 Uiso 1 1 calc R . . C6 C 0.1037(6) 0.8951(5) 0.2859(5) 0.076(2) Uani 1 1 d . . . H6A H 0.0684 0.8684 0.2385 0.092 Uiso 1 1 calc R . . O3 O 0.1546(4) 0.8482(3) 0.3040(3) 0.0667(14) Uani 1 1 d D . . H3 H 0.144(5) 0.806(3) 0.271(3) 0.080 Uiso 1 1 d D . . C7 C 0.1536(8) 0.9572(5) 0.2804(6) 0.108(4) Uani 1 1 d . . . H7A H 0.1907 0.9416 0.2497 0.162 Uiso 1 1 calc R . . H7B H 0.1871 0.9870 0.3262 0.162 Uiso 1 1 calc R . . H7C H 0.1156 0.9835 0.2617 0.162 Uiso 1 1 calc R . . N2 N 0.2270(5) 0.6356(4) 0.2357(4) 0.081(2) Uani 1 1 d . . . C8 C 0.3051(6) 0.6862(5) 0.2815(5) 0.098(3) Uani 1 1 d . . . H8A H 0.3444 0.6598 0.2999 0.117 Uiso 1 1 calc R . . H8B H 0.3324 0.7069 0.2529 0.117 Uiso 1 1 calc R . . C9 C 0.2925(7) 0.7392(7) 0.3358(9) 0.199(10) Uani 1 1 d . . . H9A H 0.3067 0.7834 0.3280 0.239 Uiso 1 1 calc R . . H9B H 0.3330 0.7415 0.3779 0.239 Uiso 1 1 calc R . . O4 O 0.2141(3) 0.7366(2) 0.3492(2) 0.0591(12) Uani 1 1 d . . . C10 C 0.2261(6) 0.5632(5) 0.2365(6) 0.091(3) Uani 1 1 d . . . H10A H 0.1864 0.5295 0.1947 0.109 Uiso 1 1 calc R . . H10B H 0.2825 0.5512 0.2373 0.109 Uiso 1 1 calc R . . C11 C 0.1997(5) 0.5604(5) 0.2994(5) 0.078(2) Uani 1 1 d . . . H11A H 0.1940 0.5122 0.2997 0.093 Uiso 1 1 calc R . . H11B H 0.2420 0.5910 0.3414 0.093 Uiso 1 1 calc R . . O5 O 0.1211(3) 0.5835(2) 0.2981(3) 0.0628(13) Uani 1 1 d . . . C12 C 0.2062(7) 0.6376(5) 0.1653(5) 0.095(3) Uani 1 1 d . . . H12A H 0.1601 0.5987 0.1359 0.114 Uiso 1 1 calc R . . H12B H 0.2555 0.6321 0.1453 0.114 Uiso 1 1 calc R . . C13 C 0.1799(7) 0.7067(5) 0.1672(4) 0.088(3) Uani 1 1 d . . . H13A H 0.2309 0.7438 0.1843 0.106 Uiso 1 1 calc R . . O6 O 0.1263(4) 0.7243(3) 0.2128(3) 0.0699(14) Uani 1 1 d . . . C14 C 0.1358(8) 0.7010(6) 0.0942(5) 0.120(4) Uani 1 1 d . . . H14A H 0.1190 0.7456 0.0953 0.180 Uiso 1 1 calc R . . H14B H 0.0860 0.6642 0.0768 0.180 Uiso 1 1 calc R . . H14C H 0.1741 0.6896 0.0638 0.180 Uiso 1 1 calc R . . N3 N -0.1028(4) 0.4974(3) 0.1278(4) 0.080(2) Uani 1 1 d . . . C15 C -0.1158(6) 0.5674(4) 0.1315(5) 0.088(3) Uani 1 1 d . . . H15A H -0.1449 0.5657 0.0852 0.105 Uiso 1 1 calc R . . H15B H -0.1525 0.5833 0.1631 0.105 Uiso 1 1 calc R . . C16 C -0.0392(8) 0.6168(5) 0.1548(5) 0.112(4) Uani 1 1 d . . . H16A H -0.0118 0.6118 0.1162 0.135 Uiso 1 1 calc R . . H16B H -0.0516 0.6647 0.1704 0.135 Uiso 1 1 calc R . . O7 O 0.0155(3) 0.6068(3) 0.2094(2) 0.0666(14) Uani 1 1 d . . . C17 C -0.0700(8) 0.4576(8) 0.0720(5) 0.143(6) Uani 1 1 d . . . H17A H -0.0794 0.4789 0.0359 0.171 Uiso 1 1 calc R . . H17B H -0.1042 0.4102 0.0521 0.171 Uiso 1 1 calc R . . C18 C 0.0173(6) 0.4499(5) 0.0849(4) 0.078(2) Uani 1 1 d . . . H18A H 0.0562 0.4800 0.0707 0.094 Uiso 1 1 calc R . . O8 O 0.0455(3) 0.4459(2) 0.1507(2) 0.0580(12) Uani 1 1 d . . . C19 C -0.1873(8) 0.4624(7) 0.1286(10) 0.174(8) Uani 1 1 d . . . H19A H -0.2125 0.4971 0.1597 0.209 Uiso 1 1 calc R . . H19B H -0.2241 0.4472 0.0817 0.209 Uiso 1 1 calc R . . C20 C -0.1852(7) 0.4049(7) 0.1498(7) 0.121(4) Uani 1 1 d . . . H20A H -0.1765 0.3674 0.1091 0.146 Uiso 1 1 calc R . . O9 O -0.1109(4) 0.4143(3) 0.2035(4) 0.0851(18) Uani 1 1 d D . . H9 H -0.091(6) 0.374(3) 0.185(5) 0.102 Uiso 1 1 d D . . C21 C -0.2595(9) 0.3723(12) 0.1659(16) 0.294(16) Uani 1 1 d . . . H21A H -0.3095 0.3663 0.1297 0.441 Uiso 1 1 calc R . . H21B H -0.2668 0.4024 0.2102 0.441 Uiso 1 1 calc R . . H21C H -0.2512 0.3267 0.1685 0.441 Uiso 1 1 calc R . . N4 N 0.0974(5) 0.2994(4) 0.2384(4) 0.078(2) Uani 1 1 d . . . C22 C 0.0878(7) 0.3377(5) 0.3082(5) 0.095(3) Uani 1 1 d . . . H22A H 0.1441 0.3552 0.3400 0.114 Uiso 1 1 calc R . . H22B H 0.0567 0.3048 0.3242 0.114 Uiso 1 1 calc R . . C23 C 0.0427(8) 0.3986(5) 0.3125(5) 0.097(3) Uani 1 1 d . . . H23A H -0.0185 0.3819 0.3006 0.117 Uiso 1 1 calc R . . H23B H 0.0589 0.4326 0.3602 0.117 Uiso 1 1 calc R . . O10 O 0.0628(3) 0.4315(3) 0.2668(3) 0.0644(13) Uani 1 1 d . . . C24 C 0.1863(7) 0.2900(5) 0.2425(5) 0.092(3) Uani 1 1 d . . . H24A H 0.1905 0.2530 0.2002 0.110 Uiso 1 1 calc R . . H24B H 0.2073 0.2759 0.2824 0.110 Uiso 1 1 calc R . . C25 C 0.2385(6) 0.3592(5) 0.2505(4) 0.085(3) Uani 1 1 d . . . H25A H 0.2390 0.3949 0.2952 0.103 Uiso 1 1 calc R . . H25B H 0.2969 0.3534 0.2495 0.103 Uiso 1 1 calc R . . O11 O 0.2025(3) 0.3806(3) 0.1955(2) 0.0633(13) Uani 1 1 d . . . C26 C 0.0342(8) 0.2354(5) 0.1977(6) 0.099(3) Uani 1 1 d . . . H26A H 0.0306 0.2048 0.2251 0.118 Uiso 1 1 calc R . . H26B H 0.0512 0.2096 0.1555 0.118 Uiso 1 1 calc R . . C27 C -0.0495(8) 0.2549(5) 0.1784(7) 0.108(4) Uani 1 1 d . . . H27A H -0.0723 0.2698 0.2204 0.130 Uiso 1 1 calc R . . O12 O -0.0374(4) 0.3127(3) 0.1559(3) 0.0791(16) Uani 1 1 d . . . C28 C -0.1114(9) 0.1934(7) 0.1232(8) 0.154(6) Uani 1 1 d . . . H28A H -0.1656 0.2076 0.1122 0.232 Uiso 1 1 calc R . . H28B H -0.1184 0.1547 0.1403 0.232 Uiso 1 1 calc R . . H28C H -0.0900 0.1784 0.0816 0.232 Uiso 1 1 calc R . . N5 N 0.1560(5) 0.2574(4) -0.0279(4) 0.084(2) Uani 1 1 d . . . C29 C 0.0675(7) 0.2681(5) -0.0376(4) 0.089(3) Uani 1 1 d . . . H29A H 0.0325 0.2298 -0.0787 0.106 Uiso 1 1 calc R . . H29B H 0.0639 0.3125 -0.0459 0.106 Uiso 1 1 calc R . . C30 C 0.0336(6) 0.2701(4) 0.0245(4) 0.078(3) Uani 1 1 d . . . H30A H -0.0184 0.2900 0.0225 0.094 Uiso 1 1 calc R . . H30B H 0.0204 0.2224 0.0251 0.094 Uiso 1 1 calc R . . O13 O 0.0955(3) 0.3122(3) 0.0850(3) 0.0657(14) Uani 1 1 d . . . C31 C 0.1627(8) 0.1841(5) -0.0309(5) 0.094(3) Uani 1 1 d . . . H31A H 0.2084 0.1692 -0.0532 0.113 Uiso 1 1 calc R . . H31B H 0.1099 0.1526 -0.0600 0.113 Uiso 1 1 calc R . . C32 C 0.1795(6) 0.1767(4) 0.0393(4) 0.070(2) Uani 1 1 d . . . H32A H 0.1280 0.1786 0.0565 0.084 Uiso 1 1 calc R . . H32B H 0.1961 0.1310 0.0356 0.084 Uiso 1 1 calc R . . O14 O 0.2437(3) 0.2307(2) 0.0857(3) 0.0640(13) Uani 1 1 d . . . C33 C 0.1960(8) 0.2765(5) -0.0786(5) 0.102(4) Uani 1 1 d . . . H33A H 0.1732 0.2401 -0.1247 0.123 Uiso 1 1 calc R . . H33B H 0.1806 0.3209 -0.0813 0.123 Uiso 1 1 calc R . . C34 C 0.2885(9) 0.2843(7) -0.0615(6) 0.111(4) Uani 1 1 d . . . H34A H 0.3029 0.2365 -0.0730 0.134 Uiso 1 1 calc R . . O15 O 0.3184(5) 0.3194(3) 0.0109(4) 0.097(2) Uani 1 1 d D . . H15 H 0.359(5) 0.298(5) 0.028(5) 0.116 Uiso 1 1 d D . . C35 C 0.3258(11) 0.3192(9) -0.1036(9) 0.182(8) Uani 1 1 d . . . H35A H 0.3867 0.3231 -0.0918 0.273 Uiso 1 1 calc R . . H35B H 0.3115 0.3658 -0.0941 0.273 Uiso 1 1 calc R . . H35C H 0.3036 0.2916 -0.1526 0.273 Uiso 1 1 calc R . . N6 N 0.4941(5) 0.2774(4) 0.1826(5) 0.097(3) Uani 1 1 d . . . C36 C 0.5046(7) 0.3540(5) 0.2080(8) 0.121(4) Uani 1 1 d . . . H36A H 0.5587 0.3737 0.2023 0.146 Uiso 1 1 calc R . . H36B H 0.5062 0.3710 0.2578 0.146 Uiso 1 1 calc R . . C37 C 0.4331(6) 0.3802(5) 0.1696(7) 0.101(3) Uani 1 1 d . . . H37A H 0.4293 0.4279 0.1984 0.121 Uiso 1 1 calc R . . H37B H 0.4452 0.3821 0.1261 0.121 Uiso 1 1 calc R . . O16 O 0.3566(3) 0.3353(3) 0.1551(3) 0.0780(16) Uani 1 1 d . . . C38 C 0.5096(7) 0.2493(6) 0.2396(7) 0.112(4) Uani 1 1 d . . . H38A H 0.5582 0.2789 0.2767 0.134 Uiso 1 1 calc R . . H38B H 0.5210 0.2013 0.2225 0.134 Uiso 1 1 calc R . . C39 C 0.4300(6) 0.2499(5) 0.2661(5) 0.095(3) Uani 1 1 d . . . H39A H 0.4348 0.2295 0.3029 0.115 Uiso 1 1 calc R . . H39B H 0.4198 0.2981 0.2849 0.115 Uiso 1 1 calc R . . O17 O 0.3642(3) 0.2093(3) 0.2089(3) 0.0691(15) Uani 1 1 d . . . C40 C 0.5407(8) 0.2489(6) 0.1317(9) 0.135(5) Uani 1 1 d . . . H40A H 0.5392 0.1987 0.1238 0.162 Uiso 1 1 calc R . . H40B H 0.5999 0.2727 0.1491 0.162 Uiso 1 1 calc R . . C41 C 0.5032(9) 0.2584(6) 0.0639(8) 0.125(5) Uani 1 1 d . . . H41A H 0.5203 0.3085 0.0701 0.150 Uiso 1 1 calc R . . O18 O 0.4135(5) 0.2437(3) 0.0491(4) 0.098(2) Uani 1 1 d . . . C42 C 0.5304(10) 0.2143(7) 0.0009(10) 0.177(8) Uani 1 1 d . . . H42A H 0.5033 0.2242 -0.0397 0.265 Uiso 1 1 calc R . . H42B H 0.5140 0.1648 -0.0067 0.265 Uiso 1 1 calc R . . H42C H 0.5913 0.2258 0.0087 0.265 Uiso 1 1 calc R . . N7 N 0.3332(4) -0.0068(3) 0.0620(3) 0.0647(17) Uani 1 1 d . . . C43 C 0.3007(5) 0.0171(4) 0.0048(4) 0.068(2) Uani 1 1 d . . . H43A H 0.2405 0.0190 0.0010 0.081 Uiso 1 1 calc R . . H43B H 0.3069 -0.0160 -0.0391 0.081 Uiso 1 1 calc R . . C44 C 0.3485(6) 0.0882(4) 0.0181(4) 0.074(2) Uani 1 1 d . . . H44A H 0.4052 0.0845 0.0103 0.089 Uiso 1 1 calc R . . H44B H 0.3193 0.1092 -0.0138 0.089 Uiso 1 1 calc R . . O19 O 0.3544(3) 0.1310(3) 0.0879(3) 0.0630(13) Uani 1 1 d . . . C45 C 0.4181(5) -0.0222(5) 0.0635(4) 0.077(3) Uani 1 1 d . . . H45A H 0.4279 -0.0324 0.0168 0.093 Uiso 1 1 calc R . . H45B H 0.4217 -0.0647 0.0754 0.093 Uiso 1 1 calc R . . C46 C 0.4861(5) 0.0359(5) 0.1139(4) 0.072(2) Uani 1 1 d . . . H46A H 0.5390 0.0179 0.1215 0.087 Uiso 1 1 calc R . . H46B H 0.4953 0.0732 0.0946 0.087 Uiso 1 1 calc R . . O20 O 0.4645(3) 0.0636(3) 0.1768(2) 0.0633(13) Uani 1 1 d . . . C47 C 0.2719(7) -0.0678(4) 0.0551(5) 0.088(3) Uani 1 1 d . . . H47A H 0.2146 -0.0582 0.0436 0.105 Uiso 1 1 calc R . . H47B H 0.2775 -0.1087 0.0168 0.105 Uiso 1 1 calc R . . C48 C 0.2840(11) -0.0844(6) 0.1186(6) 0.132(5) Uani 1 1 d . . . H48A H 0.3343 -0.1073 0.1216 0.159 Uiso 1 1 calc R . . O21 O 0.3007(4) -0.0220(3) 0.1782(3) 0.0778(16) Uani 1 1 d D . . H21 H 0.346(4) -0.022(5) 0.211(4) 0.093 Uiso 1 1 d D . . C49 C 0.2118(16) -0.1341(8) 0.1185(9) 0.272(15) Uani 1 1 d . . . H49A H 0.2231 -0.1443 0.1612 0.408 Uiso 1 1 calc R . . H49B H 0.2035 -0.1775 0.0790 0.408 Uiso 1 1 calc R . . H49C H 0.1612 -0.1134 0.1150 0.408 Uiso 1 1 calc R . . N8 N 0.5018(5) 0.0700(6) 0.3778(4) 0.109(3) Uani 1 1 d . . . C50 C 0.4325(7) 0.1087(9) 0.3967(6) 0.140(6) Uani 1 1 d . . . H50A H 0.4561 0.1586 0.4222 0.168 Uiso 1 1 calc R . . H50B H 0.4065 0.0901 0.4273 0.168 Uiso 1 1 calc R . . C51 C 0.3665(6) 0.1014(7) 0.3335(5) 0.098(3) Uani 1 1 d . . . H51A H 0.3288 0.0558 0.3177 0.117 Uiso 1 1 calc R . . H51B H 0.3325 0.1385 0.3451 0.117 Uiso 1 1 calc R . . O22 O 0.4041(3) 0.1066(3) 0.2799(3) 0.0716(15) Uani 1 1 d . . . C52 C 0.5811(7) 0.1120(8) 0.4188(5) 0.118(4) Uani 1 1 d . . . H52A H 0.6246 0.0825 0.4186 0.142 Uiso 1 1 calc R . . H52B H 0.5776 0.1346 0.4670 0.142 Uiso 1 1 calc R . . C53 C 0.6043(6) 0.1687(7) 0.3875(5) 0.108(4) Uani 1 1 d . . . H53A H 0.5641 0.2013 0.3919 0.129 Uiso 1 1 calc R . . H53B H 0.6612 0.1956 0.4120 0.129 Uiso 1 1 calc R . . O23 O 0.6011(3) 0.1333(3) 0.3169(2) 0.0736(16) Uani 1 1 d . . . C54 C 0.4942(8) -0.0036(8) 0.3768(7) 0.129(5) Uani 1 1 d . . . H54A H 0.4804 -0.0056 0.4198 0.154 Uiso 1 1 calc R . . H54B H 0.5483 -0.0195 0.3744 0.154 Uiso 1 1 calc R . . C55 C 0.4266(9) -0.0510(8) 0.3154(7) 0.129(5) Uani 1 1 d . . . H55A H 0.3708 -0.0435 0.3250 0.155 Uiso 1 1 calc R . . O24 O 0.4335(4) -0.0331(4) 0.2560(4) 0.101(2) Uani 1 1 d . . . C56 C 0.4329(13) -0.1279(9) 0.3018(11) 0.213(9) Uani 1 1 d . . . H56A H 0.3880 -0.1574 0.2622 0.319 Uiso 1 1 calc R . . H56B H 0.4276 -0.1394 0.3425 0.319 Uiso 1 1 calc R . . H56C H 0.4873 -0.1360 0.2920 0.319 Uiso 1 1 calc R . . N9 N 0.7470(4) -0.0313(3) 0.2581(3) 0.0650(17) Uani 1 1 d . . . C57 C 0.6705(6) -0.0834(5) 0.2321(8) 0.134(5) Uani 1 1 d . . . H57A H 0.6579 -0.0968 0.2707 0.161 Uiso 1 1 calc R . . H57B H 0.6802 -0.1254 0.1974 0.161 Uiso 1 1 calc R . . C58 C 0.5976(6) -0.0601(5) 0.2010(5) 0.084(3) Uani 1 1 d . . . H58A H 0.6002 -0.0622 0.1540 0.101 Uiso 1 1 calc R . . H58B H 0.5457 -0.0911 0.1975 0.101 Uiso 1 1 calc R . . O25 O 0.5965(3) 0.0097(3) 0.2425(3) 0.0704(15) Uani 1 1 d . . . C59 C 0.7946(10) -0.0341(5) 0.3238(5) 0.126(5) Uani 1 1 d . . . H59A H 0.7846 -0.0828 0.3226 0.151 Uiso 1 1 calc R . . H59B H 0.8551 -0.0209 0.3276 0.151 Uiso 1 1 calc R . . C60 C 0.7740(6) 0.0099(4) 0.3834(4) 0.079(3) Uani 1 1 d . . . H60A H 0.8171 0.0138 0.4247 0.095 Uiso 1 1 calc R . . H60B H 0.7197 -0.0115 0.3874 0.095 Uiso 1 1 calc R . . O26 O 0.7684(3) 0.0783(3) 0.3817(2) 0.0609(13) Uani 1 1 d . . . C61 C 0.7996(7) -0.0408(5) 0.2103(6) 0.097(3) Uani 1 1 d . . . H61A H 0.7631 -0.0534 0.1635 0.116 Uiso 1 1 calc R . . H61B H 0.8266 -0.0813 0.2111 0.116 Uiso 1 1 calc R . . C62 C 0.8652(6) 0.0172(5) 0.2202(5) 0.079(2) Uani 1 1 d . . . H62A H 0.9141 0.0110 0.2525 0.095 Uiso 1 1 calc R . . O27 O 0.8458(3) 0.0826(3) 0.2582(3) 0.0651(14) Uani 1 1 d D . . H27 H 0.882(4) 0.104(4) 0.297(3) 0.078 Uiso 1 1 d D . . C63 C 0.8976(9) 0.0197(6) 0.1617(7) 0.130(5) Uani 1 1 d . . . H63A H 0.9412 0.0612 0.1762 0.195 Uiso 1 1 calc R . . H63B H 0.8520 0.0219 0.1255 0.195 Uiso 1 1 calc R . . H63C H 0.9213 -0.0222 0.1438 0.195 Uiso 1 1 calc R . . N10 N 0.9341(5) 0.2633(3) 0.4496(3) 0.0726(19) Uani 1 1 d . . . C64 C 0.8976(7) 0.2863(6) 0.3910(5) 0.100(3) Uani 1 1 d . . . H64A H 0.8985 0.3371 0.4099 0.120 Uiso 1 1 calc R . . H64B H 0.9348 0.2786 0.3588 0.120 Uiso 1 1 calc R . . C65 C 0.8149(9) 0.2531(6) 0.3527(6) 0.149(7) Uani 1 1 d . . . H65A H 0.7805 0.2734 0.3257 0.178 Uiso 1 1 calc R . . O28 O 0.7882(3) 0.1906(3) 0.3573(2) 0.0680(14) Uani 1 1 d . . . C66 C 0.9242(6) 0.3107(4) 0.5173(5) 0.081(3) Uani 1 1 d . . . H66A H 0.9369 0.3598 0.5203 0.097 Uiso 1 1 calc R . . H66B H 0.9642 0.3046 0.5554 0.097 Uiso 1 1 calc R . . C67 C 0.8349(6) 0.2942(4) 0.5242(4) 0.073(2) Uani 1 1 d . . . H67A H 0.8306 0.3202 0.5714 0.087 Uiso 1 1 calc R . . H67B H 0.7954 0.3080 0.4913 0.087 Uiso 1 1 calc R . . O29 O 0.8150(3) 0.2213(2) 0.5097(2) 0.0590(12) Uani 1 1 d . . . C68 C 1.0199(6) 0.2469(5) 0.4510(5) 0.087(3) Uani 1 1 d . . . H68A H 1.0426 0.2382 0.4939 0.105 Uiso 1 1 calc R . . H68B H 1.0577 0.2864 0.4492 0.105 Uiso 1 1 calc R . . C69 C 1.0128(6) 0.1801(5) 0.3867(5) 0.093(3) Uani 1 1 d . . . H69A H 1.0059 0.1934 0.3447 0.112 Uiso 1 1 calc R . . O30 O 0.9413(3) 0.1307(3) 0.3792(3) 0.0740(15) Uani 1 1 d . . . C70 C 1.0916(7) 0.1470(8) 0.3941(8) 0.146(5) Uani 1 1 d . . . H70A H 1.0861 0.1061 0.3528 0.219 Uiso 1 1 calc R . . H70B H 1.0981 0.1329 0.4346 0.219 Uiso 1 1 calc R . . H70C H 1.1408 0.1810 0.3995 0.219 Uiso 1 1 calc R . . N11 N 0.2847(5) 0.9412(4) 0.4534(3) 0.0688(18) Uani 1 1 d . . . O31 O 0.2092(4) 0.9496(3) 0.4463(3) 0.0681(14) Uani 1 1 d . . . O32 O 0.2985(3) 0.8793(3) 0.4393(3) 0.0692(14) Uani 1 1 d . . . O33 O 0.3420(4) 0.9919(3) 0.4748(3) 0.0938(19) Uani 1 1 d . . . N12 N -0.0914(6) 0.5626(5) 0.3402(5) 0.096(2) Uani 1 1 d . . . O34 O -0.0291(4) 0.5320(3) 0.3523(3) 0.0837(17) Uani 1 1 d . . . O35 O -0.1132(4) 0.5670(4) 0.2815(4) 0.0919(19) Uani 1 1 d . . . O36 O -0.1297(5) 0.5852(5) 0.3861(4) 0.139(3) Uani 1 1 d . . . N13 N 0.2557(7) 0.4647(5) 0.0643(5) 0.095(3) Uani 1 1 d . . . O37 O 0.3067(5) 0.4570(3) 0.1144(4) 0.0884(18) Uani 1 1 d . . . O38 O 0.1909(5) 0.4182(3) 0.0350(3) 0.0867(19) Uani 1 1 d . . . O39 O 0.2686(6) 0.5144(4) 0.0467(4) 0.123(3) Uani 1 1 d . . . N14 N 0.1673(5) 0.0845(4) 0.1734(5) 0.078(2) Uani 1 1 d . . . O40 O 0.2220(4) 0.1098(3) 0.2293(3) 0.0803(17) Uani 1 1 d . . . O41 O 0.1914(3) 0.0646(3) 0.1170(3) 0.0739(15) Uani 1 1 d . . . O42 O 0.0922(4) 0.0797(4) 0.1741(4) 0.109(2) Uani 1 1 d . . . N15 N 0.6875(4) 0.1230(4) 0.1594(3) 0.0715(19) Uani 1 1 d . . . O43 O 0.6925(4) 0.0623(3) 0.1578(2) 0.0691(15) Uani 1 1 d . . . O44 O 0.6949(4) 0.1702(3) 0.2174(3) 0.0831(18) Uani 1 1 d . . . O45 O 0.6758(4) 0.1375(3) 0.1059(3) 0.0834(17) 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 Yb1 0.05926(19) 0.04914(17) 0.04608(16) 0.00899(13) 0.00417(14) 0.01521(15) Yb2 0.0625(2) 0.05010(18) 0.0652(2) 0.01104(15) 0.01722(16) 0.01481(15) Yb3 0.0814(2) 0.05074(19) 0.0686(2) 0.01724(16) 0.02745(18) 0.02454(17) Yb4 0.05475(19) 0.0597(2) 0.05781(19) 0.01279(15) 0.00590(15) 0.01513(15) Yb5 0.0647(2) 0.0676(2) 0.04658(17) 0.01176(15) 0.00831(14) 0.02627(17) Fe1 0.0646(6) 0.0491(6) 0.0495(6) 0.0047(4) 0.0078(5) 0.0111(5) Fe2 0.0690(7) 0.0463(5) 0.0561(6) 0.0141(5) 0.0143(5) 0.0177(5) Fe3 0.0605(7) 0.0514(6) 0.0877(8) 0.0154(6) 0.0176(6) 0.0155(5) Fe4 0.0641(7) 0.0995(9) 0.0599(7) 0.0297(6) 0.0137(5) 0.0314(7) Fe5 0.0661(7) 0.0613(6) 0.0471(5) 0.0136(5) 0.0081(5) 0.0182(5) N1 0.068(4) 0.055(4) 0.057(4) 0.009(3) 0.004(3) 0.022(3) C1 0.108(7) 0.106(7) 0.067(5) 0.024(5) 0.009(5) 0.066(6) C2 0.072(5) 0.067(5) 0.066(5) 0.010(4) 0.007(4) 0.034(4) O1 0.071(3) 0.056(3) 0.048(3) 0.011(2) 0.007(2) 0.024(3) C3 0.061(5) 0.080(6) 0.126(8) 0.025(6) -0.014(5) 0.017(5) C4 0.063(5) 0.064(5) 0.081(6) 0.008(4) -0.002(4) 0.019(4) O2 0.047(3) 0.056(3) 0.054(3) 0.007(2) 0.002(2) 0.012(2) C5 0.095(7) 0.098(7) 0.092(7) 0.056(6) 0.009(6) 0.035(6) C6 0.079(6) 0.083(6) 0.078(6) 0.043(5) 0.015(5) 0.025(5) O3 0.078(4) 0.058(3) 0.057(3) 0.013(2) 0.009(3) 0.021(3) C7 0.137(10) 0.089(7) 0.115(9) 0.048(7) 0.038(7) 0.035(7) N2 0.076(5) 0.065(4) 0.086(5) 0.003(4) 0.026(4) 0.007(4) C8 0.075(6) 0.092(7) 0.101(7) 0.009(6) 0.019(5) -0.005(5) C9 0.065(7) 0.138(11) 0.253(18) -0.119(12) 0.048(9) -0.002(7) O4 0.058(3) 0.053(3) 0.058(3) 0.008(2) 0.010(2) 0.017(2) C10 0.082(6) 0.065(6) 0.115(8) 0.015(5) 0.026(6) 0.023(5) C11 0.062(5) 0.066(5) 0.098(7) 0.022(5) 0.012(5) 0.020(4) O5 0.062(3) 0.051(3) 0.070(3) 0.013(2) 0.014(3) 0.020(2) C12 0.110(8) 0.081(7) 0.081(7) 0.004(5) 0.045(6) 0.000(6) C13 0.108(7) 0.081(6) 0.061(5) 0.005(5) 0.032(5) 0.000(6) O6 0.088(4) 0.064(3) 0.048(3) 0.013(2) 0.011(3) 0.001(3) C14 0.149(11) 0.123(9) 0.058(6) 0.020(6) 0.001(6) -0.028(8) N3 0.068(4) 0.052(4) 0.093(5) 0.007(4) -0.011(4) 0.014(3) C15 0.099(7) 0.063(5) 0.086(6) 0.021(5) -0.009(5) 0.027(5) C16 0.153(10) 0.077(6) 0.070(6) 0.028(5) -0.043(6) -0.015(7) O7 0.081(4) 0.053(3) 0.052(3) 0.013(2) -0.001(3) 0.000(3) C17 0.136(11) 0.183(13) 0.068(7) -0.004(7) -0.018(7) 0.087(10) C18 0.073(5) 0.102(7) 0.071(5) 0.049(5) 0.009(4) 0.021(5) O8 0.069(3) 0.052(3) 0.051(3) 0.013(2) 0.016(2) 0.019(2) C19 0.082(8) 0.110(10) 0.30(2) 0.090(13) -0.046(11) -0.010(7) C20 0.071(7) 0.125(10) 0.117(9) -0.008(8) 0.013(6) -0.018(7) O9 0.071(4) 0.067(4) 0.103(5) 0.010(3) 0.025(3) 0.004(3) C21 0.068(9) 0.26(2) 0.60(5) 0.24(3) 0.050(17) -0.014(12) N4 0.097(5) 0.074(5) 0.082(5) 0.039(4) 0.040(4) 0.030(4) C22 0.132(9) 0.094(7) 0.090(7) 0.049(6) 0.058(6) 0.043(7) C23 0.143(10) 0.083(6) 0.080(6) 0.032(5) 0.039(6) 0.043(7) O10 0.082(4) 0.056(3) 0.060(3) 0.020(2) 0.025(3) 0.018(3) C24 0.127(9) 0.097(7) 0.073(6) 0.044(5) 0.030(6) 0.055(7) C25 0.092(7) 0.097(7) 0.064(5) 0.026(5) 0.005(5) 0.037(6) O11 0.072(3) 0.065(3) 0.054(3) 0.021(2) 0.010(2) 0.025(3) C26 0.144(10) 0.060(6) 0.098(7) 0.030(5) 0.043(7) 0.012(6) C27 0.118(9) 0.057(6) 0.143(10) 0.030(6) 0.037(8) -0.008(6) O12 0.077(4) 0.056(3) 0.096(4) 0.016(3) 0.024(3) 0.007(3) C28 0.143(12) 0.093(9) 0.203(16) 0.043(10) 0.020(11) -0.016(9) N5 0.129(7) 0.073(5) 0.064(4) 0.025(4) 0.035(4) 0.057(5) C29 0.141(9) 0.068(5) 0.050(5) 0.012(4) 0.008(5) 0.043(6) C30 0.095(6) 0.067(5) 0.058(5) 0.011(4) -0.001(4) 0.021(5) O13 0.078(3) 0.054(3) 0.059(3) 0.013(2) 0.009(3) 0.019(3) C31 0.148(9) 0.063(5) 0.066(5) 0.012(4) 0.017(6) 0.043(6) C32 0.083(6) 0.059(5) 0.061(5) 0.015(4) 0.007(4) 0.019(4) O14 0.069(3) 0.047(3) 0.070(3) 0.011(2) 0.014(3) 0.018(3) C33 0.171(12) 0.086(7) 0.069(6) 0.030(5) 0.043(7) 0.068(7) C34 0.152(11) 0.117(9) 0.111(9) 0.058(8) 0.076(8) 0.077(9) O15 0.135(6) 0.070(4) 0.108(5) 0.033(4) 0.066(5) 0.043(4) C35 0.222(18) 0.228(19) 0.203(17) 0.147(16) 0.146(15) 0.093(15) N6 0.071(5) 0.062(5) 0.140(8) 0.013(5) 0.025(5) 0.009(4) C36 0.078(7) 0.066(6) 0.190(13) 0.025(7) 0.005(8) 0.000(5) C37 0.072(6) 0.065(6) 0.160(10) 0.030(6) 0.031(6) 0.012(5) O16 0.060(3) 0.053(3) 0.111(5) 0.013(3) 0.022(3) 0.013(3) C38 0.079(7) 0.082(7) 0.136(10) 0.014(7) -0.015(7) 0.011(6) C39 0.089(7) 0.069(6) 0.087(7) -0.003(5) -0.019(5) 0.008(5) O17 0.059(3) 0.056(3) 0.068(3) 0.005(2) -0.011(3) 0.011(2) C40 0.088(8) 0.084(8) 0.234(18) 0.045(10) 0.053(10) 0.021(7) C41 0.123(10) 0.087(8) 0.190(14) 0.043(9) 0.098(10) 0.036(8) O18 0.109(5) 0.068(4) 0.148(6) 0.049(4) 0.070(5) 0.039(4) C42 0.176(14) 0.102(10) 0.30(2) 0.062(12) 0.172(15) 0.045(10) N7 0.070(4) 0.049(3) 0.064(4) 0.009(3) 0.008(3) 0.017(3) C43 0.079(5) 0.061(5) 0.051(4) 0.009(4) 0.006(4) 0.012(4) C44 0.091(6) 0.070(5) 0.058(5) 0.013(4) 0.016(4) 0.028(5) O19 0.067(3) 0.053(3) 0.068(3) 0.015(2) 0.019(3) 0.023(3) C45 0.081(6) 0.075(5) 0.062(5) 0.003(4) 0.008(4) 0.038(5) C46 0.066(5) 0.093(6) 0.055(4) 0.019(4) 0.013(4) 0.026(5) O20 0.062(3) 0.076(3) 0.054(3) 0.021(3) 0.016(2) 0.024(3) C47 0.105(7) 0.055(5) 0.091(7) 0.016(5) 0.019(6) -0.003(5) C48 0.217(16) 0.067(7) 0.110(9) 0.017(6) 0.067(10) 0.005(8) O21 0.084(4) 0.072(4) 0.079(4) 0.027(3) 0.021(3) 0.018(3) C49 0.49(4) 0.126(13) 0.159(15) 0.015(11) 0.14(2) -0.127(19) N8 0.079(6) 0.194(10) 0.084(6) 0.072(7) 0.035(5) 0.055(6) C50 0.091(8) 0.271(18) 0.091(8) 0.084(10) 0.037(6) 0.082(10) C51 0.089(7) 0.153(10) 0.067(6) 0.046(6) 0.028(5) 0.054(7) O22 0.072(3) 0.088(4) 0.053(3) 0.021(3) 0.011(3) 0.028(3) C52 0.100(8) 0.200(14) 0.059(6) 0.041(8) 0.019(6) 0.062(9) C53 0.080(7) 0.143(10) 0.067(6) -0.011(6) 0.007(5) 0.053(7) O23 0.073(3) 0.088(4) 0.047(3) 0.004(3) 0.008(2) 0.032(3) C54 0.127(10) 0.199(14) 0.122(10) 0.119(11) 0.041(8) 0.072(10) C55 0.139(11) 0.176(14) 0.122(10) 0.092(10) 0.060(9) 0.062(10) O24 0.095(5) 0.123(6) 0.126(6) 0.084(5) 0.041(4) 0.043(4) C56 0.25(2) 0.173(16) 0.30(3) 0.181(18) 0.093(19) 0.075(15) N9 0.067(4) 0.059(4) 0.059(4) 0.007(3) 0.011(3) 0.022(3) C57 0.075(7) 0.063(6) 0.217(15) -0.003(7) 0.012(8) 0.015(5) C58 0.085(6) 0.080(6) 0.071(6) 0.013(5) -0.001(5) 0.019(5) O25 0.071(3) 0.079(4) 0.055(3) 0.017(3) 0.009(3) 0.024(3) C59 0.244(15) 0.079(7) 0.061(6) 0.020(5) 0.032(7) 0.077(9) C60 0.090(6) 0.065(5) 0.064(5) 0.013(4) -0.008(4) 0.013(5) O26 0.068(3) 0.061(3) 0.049(3) 0.013(2) 0.007(2) 0.022(3) C61 0.099(7) 0.074(6) 0.111(8) 0.010(6) 0.041(6) 0.033(6) C62 0.082(6) 0.066(5) 0.079(6) 0.003(4) 0.031(5) 0.022(5) O27 0.064(3) 0.069(3) 0.051(3) 0.007(3) 0.011(2) 0.017(3) C63 0.165(12) 0.089(8) 0.132(10) 0.007(7) 0.089(9) 0.013(8) N10 0.091(5) 0.064(4) 0.053(4) 0.011(3) 0.013(3) 0.011(4) C64 0.125(9) 0.104(8) 0.092(7) 0.059(6) 0.034(7) 0.026(7) C65 0.189(13) 0.080(7) 0.119(9) 0.047(7) -0.077(9) -0.054(8) O28 0.083(4) 0.061(3) 0.052(3) 0.014(2) 0.005(3) 0.017(3) C66 0.098(7) 0.057(5) 0.074(6) 0.016(4) 0.010(5) 0.002(5) C67 0.090(6) 0.057(5) 0.064(5) 0.015(4) 0.011(4) 0.016(4) O29 0.071(3) 0.050(3) 0.050(3) 0.012(2) 0.008(2) 0.015(2) C68 0.076(6) 0.087(7) 0.087(6) 0.018(5) 0.019(5) 0.006(5) C69 0.083(7) 0.095(7) 0.088(7) 0.011(6) 0.025(5) 0.018(6) O30 0.064(3) 0.084(4) 0.064(3) 0.017(3) 0.011(3) 0.013(3) C70 0.081(8) 0.152(12) 0.177(14) 0.017(10) 0.032(8) 0.031(8) N11 0.078(5) 0.065(5) 0.050(4) 0.014(3) 0.006(3) -0.006(4) O31 0.076(4) 0.052(3) 0.063(3) 0.008(2) 0.007(3) 0.014(3) O32 0.070(3) 0.057(3) 0.068(3) 0.014(3) 0.003(3) 0.007(3) O33 0.098(5) 0.070(4) 0.096(5) 0.022(3) 0.011(4) -0.012(4) N12 0.092(6) 0.090(6) 0.092(6) 0.005(5) 0.038(5) 0.011(5) O34 0.086(4) 0.088(4) 0.071(4) 0.015(3) 0.027(3) 0.015(4) O35 0.096(5) 0.093(5) 0.095(5) 0.024(4) 0.044(4) 0.039(4) O36 0.121(6) 0.170(8) 0.121(7) 0.018(6) 0.068(6) 0.048(6) N13 0.133(8) 0.065(5) 0.116(7) 0.040(5) 0.074(7) 0.038(6) O37 0.116(5) 0.055(3) 0.103(5) 0.023(3) 0.046(4) 0.027(4) O38 0.123(6) 0.065(4) 0.098(5) 0.043(4) 0.049(4) 0.039(4) O39 0.195(9) 0.070(4) 0.135(7) 0.048(5) 0.082(6) 0.038(5) N14 0.060(5) 0.069(5) 0.106(6) 0.038(4) 0.009(4) 0.015(4) O40 0.060(3) 0.092(4) 0.081(4) 0.019(3) 0.013(3) 0.025(3) O41 0.060(3) 0.087(4) 0.072(4) 0.031(3) 0.005(3) 0.011(3) O42 0.062(4) 0.142(7) 0.131(6) 0.057(5) 0.024(4) 0.024(4) N15 0.069(4) 0.093(5) 0.049(4) 0.018(4) 0.010(3) 0.032(4) O43 0.087(4) 0.070(4) 0.046(3) 0.016(3) 0.010(3) 0.027(3) O44 0.114(5) 0.083(4) 0.050(3) 0.017(3) 0.014(3) 0.041(4) O45 0.101(5) 0.090(4) 0.061(3) 0.026(3) 0.019(3) 0.032(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.239(5) . ? Yb1 O4 2.242(5) . ? Yb1 O29 2.258(5) 2_666 ? Yb1 O2 2.265(5) . ? Yb1 O3 2.364(5) . ? Yb1 O32 2.397(5) . ? Yb1 O31 2.468(5) . ? Yb1 N1 2.542(6) . ? Yb2 O10 2.239(5) . ? Yb2 O7 2.241(5) . ? Yb2 O8 2.251(5) . ? Yb2 O5 2.265(5) . ? Yb2 O9 2.362(6) . ? Yb2 O35 2.431(6) . ? Yb2 O34 2.443(6) . ? Yb2 N3 2.503(7) . ? Yb3 O14 2.226(5) . ? Yb3 O16 2.240(5) . ? Yb3 O13 2.256(6) . ? Yb3 O11 2.260(5) . ? Yb3 O15 2.382(7) . ? Yb3 O38 2.396(5) . ? Yb3 O37 2.449(6) . ? Yb3 N5 2.534(7) . ? Yb4 O22 2.230(5) . ? Yb4 O20 2.233(5) . ? Yb4 O19 2.249(5) . ? Yb4 O17 2.275(5) . ? Yb4 O21 2.388(6) . ? Yb4 O41 2.389(5) . ? Yb4 O40 2.441(6) . ? Yb4 N7 2.527(6) . ? Yb5 O28 2.220(5) . ? Yb5 O25 2.233(6) . ? Yb5 O26 2.262(4) . ? Yb5 O23 2.267(5) . ? Yb5 O27 2.369(5) . ? Yb5 O43 2.424(5) . ? Yb5 O44 2.428(6) . ? Yb5 N9 2.563(6) . ? Fe1 O6 1.970(5) . ? Fe1 O2 1.977(5) . ? Fe1 O7 1.992(5) . ? Fe1 O5 2.016(5) . ? Fe1 O4 2.018(5) . ? Fe1 N2 2.210(7) . ? Fe2 O8 1.963(5) . ? Fe2 O12 1.969(6) . ? Fe2 O13 1.988(5) . ? Fe2 O11 2.025(5) . ? Fe2 O10 2.029(5) . ? Fe2 N4 2.206(7) . ? Fe3 O19 1.960(5) . ? Fe3 O14 1.978(5) . ? Fe3 O18 1.980(7) . ? Fe3 O17 2.006(6) . ? Fe3 O16 2.027(5) . ? Fe3 N6 2.213(8) . ? Fe4 O24 1.956(7) . ? Fe4 O20 1.974(5) . ? Fe4 O25 1.981(5) . ? Fe4 O23 2.018(6) . ? Fe4 O22 2.037(5) . ? Fe4 N8 2.244(8) . ? Fe5 O30 1.976(6) . ? Fe5 O26 1.984(5) . ? Fe5 O1 1.993(4) 2_666 ? Fe5 O29 2.007(5) . ? Fe5 O28 2.035(5) . ? Fe5 N10 2.206(7) . ? N1 C5 1.457(11) . ? N1 C1 1.460(11) . ? N1 C3 1.503(11) . ? C1 C2 1.498(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.430(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 Fe5 1.994(4) 2_666 ? C3 C4 1.490(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.427(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.509(13) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O3 1.440(9) . ? C6 C7 1.496(14) . ? C6 H6A 1.0000 . ? O3 H3 0.89(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? N2 C12 1.477(12) . ? N2 C10 1.495(11) . ? N2 C8 1.509(11) . ? C8 C9 1.374(14) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O4 1.379(12) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.494(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O5 1.429(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.521(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O6 1.421(11) . ? C13 C14 1.536(12) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N3 C17 1.442(13) . ? N3 C15 1.458(10) . ? N3 C19 1.510(16) . ? C15 C16 1.433(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O7 1.409(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.453(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O8 1.410(9) . ? C18 H18A 1.0000 . ? C19 C20 1.396(17) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O9 1.451(13) . ? C20 C21 1.49(2) . ? C20 H20A 1.0000 . ? O9 H9 0.93(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N4 C22 1.481(12) . ? N4 C26 1.485(12) . ? N4 C24 1.495(12) . ? C22 C23 1.512(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O10 1.413(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.529(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O11 1.422(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.501(15) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O12 1.426(11) . ? C27 C28 1.527(15) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? N5 C29 1.490(12) . ? N5 C33 1.494(13) . ? N5 C31 1.505(11) . ? C29 C30 1.514(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O13 1.425(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.517(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O14 1.405(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.483(16) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O15 1.424(13) . ? C34 C35 1.490(16) . ? C34 H34A 1.0000 . ? O15 H15 0.92(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N6 C40 1.451(16) . ? N6 C36 1.472(12) . ? N6 C38 1.487(14) . ? C36 C37 1.549(14) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O16 1.405(11) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.529(16) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O17 1.413(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.530(19) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O18 1.435(14) . ? C41 C42 1.529(18) . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N7 C45 1.469(10) . ? N7 C43 1.476(9) . ? N7 C47 1.480(11) . ? C43 C44 1.501(12) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O19 1.432(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.507(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 O20 1.398(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.472(15) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O21 1.436(12) . ? C48 C49 1.49(2) . ? C48 H48A 1.0000 . ? O21 H21 0.91(4) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? N8 C52 1.436(14) . ? N8 C54 1.501(16) . ? N8 C50 1.507(13) . ? C50 C51 1.507(12) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O22 1.420(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.565(17) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 O23 1.420(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.512(18) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O24 1.438(13) . ? C55 C56 1.535(19) . ? C55 H55A 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? N9 C61 1.438(12) . ? N9 C57 1.458(12) . ? N9 C59 1.480(11) . ? C57 C58 1.461(13) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 O25 1.427(10) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.422(13) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 O26 1.433(9) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.460(13) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O27 1.434(9) . ? C62 C63 1.453(14) . ? C62 H62A 1.0000 . ? O27 H27 0.86(4) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? N10 C68 1.490(11) . ? N10 C66 1.499(11) . ? N10 C64 1.507(11) . ? C64 C65 1.421(15) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O28 1.358(11) . ? C65 H65A 0.9500 . ? C66 C67 1.528(13) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 O29 1.422(9) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? O29 Yb1 2.258(5) 2_666 ? C68 C69 1.566(13) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 O30 1.427(12) . ? C69 C70 1.538(14) . ? C69 H69A 1.0000 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? N11 O33 1.232(8) . ? N11 O32 1.267(8) . ? N11 O31 1.268(9) . ? N12 O36 1.252(11) . ? N12 O35 1.259(10) . ? N12 O34 1.290(10) . ? N13 O39 1.211(10) . ? N13 O38 1.264(11) . ? N13 O37 1.285(11) . ? N14 O42 1.240(9) . ? N14 O40 1.257(9) . ? N14 O41 1.285(10) . ? N15 O45 1.246(8) . ? N15 O43 1.252(8) . ? N15 O44 1.271(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O4 148.64(18) . . ? O1 Yb1 O29 67.77(17) . 2_666 ? O4 Yb1 O29 82.78(17) . 2_666 ? O1 Yb1 O2 101.49(18) . . ? O4 Yb1 O2 68.32(17) . . ? O29 Yb1 O2 92.81(17) 2_666 . ? O1 Yb1 O3 130.55(17) . . ? O4 Yb1 O3 79.56(18) . . ? O29 Yb1 O3 161.57(18) 2_666 . ? O2 Yb1 O3 85.58(18) . . ? O1 Yb1 O32 109.08(19) . . ? O4 Yb1 O32 79.04(19) . . ? O29 Yb1 O32 87.59(18) 2_666 . ? O2 Yb1 O32 147.02(18) . . ? O3 Yb1 O32 83.92(19) . . ? O1 Yb1 O31 76.20(19) . . ? O4 Yb1 O31 127.2(2) . . ? O29 Yb1 O31 112.02(17) 2_666 . ? O2 Yb1 O31 151.14(17) . . ? O3 Yb1 O31 75.37(18) . . ? O32 Yb1 O31 52.89(18) . . ? O1 Yb1 N1 69.50(19) . . ? O4 Yb1 N1 128.15(18) . . ? O29 Yb1 N1 129.4(2) 2_666 . ? O2 Yb1 N1 70.42(18) . . ? O3 Yb1 N1 67.2(2) . . ? O32 Yb1 N1 131.9(2) . . ? O31 Yb1 N1 82.16(19) . . ? O10 Yb2 O7 144.2(2) . . ? O10 Yb2 O8 68.64(17) . . ? O7 Yb2 O8 93.49(19) . . ? O10 Yb2 O5 83.34(18) . . ? O7 Yb2 O5 67.61(17) . . ? O8 Yb2 O5 96.62(18) . . ? O10 Yb2 O9 76.8(2) . . ? O7 Yb2 O9 134.0(2) . . ? O8 Yb2 O9 84.4(2) . . ? O5 Yb2 O9 158.3(2) . . ? O10 Yb2 O35 129.6(2) . . ? O7 Yb2 O35 80.9(2) . . ? O8 Yb2 O35 150.4(2) . . ? O5 Yb2 O35 107.8(2) . . ? O9 Yb2 O35 79.1(2) . . ? O10 Yb2 O34 80.5(2) . . ? O7 Yb2 O34 115.2(2) . . ? O8 Yb2 O34 148.7(2) . . ? O5 Yb2 O34 84.1(2) . . ? O9 Yb2 O34 84.1(2) . . ? O35 Yb2 O34 53.4(2) . . ? O10 Yb2 N3 128.3(2) . . ? O7 Yb2 N3 68.4(2) . . ? O8 Yb2 N3 71.8(2) . . ? O5 Yb2 N3 133.5(2) . . ? O9 Yb2 N3 67.4(2) . . ? O35 Yb2 N3 79.2(3) . . ? O34 Yb2 N3 128.8(3) . . ? O14 Yb3 O16 68.75(19) . . ? O14 Yb3 O13 88.09(18) . . ? O16 Yb3 O13 139.1(2) . . ? O14 Yb3 O11 100.08(19) . . ? O16 Yb3 O11 83.2(2) . . ? O13 Yb3 O11 67.73(18) . . ? O14 Yb3 O15 83.9(2) . . ? O16 Yb3 O15 77.4(3) . . ? O13 Yb3 O15 135.0(2) . . ? O11 Yb3 O15 157.3(2) . . ? O14 Yb3 O38 149.0(2) . . ? O16 Yb3 O38 132.1(2) . . ? O13 Yb3 O38 84.5(2) . . ? O11 Yb3 O38 104.74(19) . . ? O15 Yb3 O38 80.3(2) . . ? O14 Yb3 O37 147.1(2) . . ? O16 Yb3 O37 80.7(2) . . ? O13 Yb3 O37 124.1(2) . . ? O11 Yb3 O37 87.8(2) . . ? O15 Yb3 O37 77.5(2) . . ? O38 Yb3 O37 53.2(2) . . ? O14 Yb3 N5 71.7(2) . . ? O16 Yb3 N5 128.4(2) . . ? O13 Yb3 N5 68.9(2) . . ? O11 Yb3 N5 136.1(2) . . ? O15 Yb3 N5 66.5(3) . . ? O38 Yb3 N5 77.5(2) . . ? O37 Yb3 N5 122.9(2) . . ? O22 Yb4 O20 68.55(19) . . ? O22 Yb4 O19 138.2(2) . . ? O20 Yb4 O19 87.87(18) . . ? O22 Yb4 O17 84.17(19) . . ? O20 Yb4 O17 102.69(19) . . ? O19 Yb4 O17 67.38(19) . . ? O22 Yb4 O21 78.4(2) . . ? O20 Yb4 O21 83.8(2) . . ? O19 Yb4 O21 134.68(19) . . ? O17 Yb4 O21 157.7(2) . . ? O22 Yb4 O41 131.7(2) . . ? O20 Yb4 O41 149.4(2) . . ? O19 Yb4 O41 85.6(2) . . ? O17 Yb4 O41 102.27(19) . . ? O21 Yb4 O41 79.8(2) . . ? O22 Yb4 O40 80.2(2) . . ? O20 Yb4 O40 147.08(19) . . ? O19 Yb4 O40 123.59(18) . . ? O17 Yb4 O40 83.5(2) . . ? O21 Yb4 O40 80.0(2) . . ? O41 Yb4 O40 53.8(2) . . ? O22 Yb4 N7 128.97(19) . . ? O20 Yb4 N7 71.30(19) . . ? O19 Yb4 N7 68.03(19) . . ? O17 Yb4 N7 135.2(2) . . ? O21 Yb4 N7 67.1(2) . . ? O41 Yb4 N7 78.5(2) . . ? O40 Yb4 N7 126.1(2) . . ? O28 Yb5 O25 150.9(2) . . ? O28 Yb5 O26 68.69(18) . . ? O25 Yb5 O26 100.82(19) . . ? O28 Yb5 O23 85.5(2) . . ? O25 Yb5 O23 67.8(2) . . ? O26 Yb5 O23 94.28(18) . . ? O28 Yb5 O27 78.5(2) . . ? O25 Yb5 O27 128.98(19) . . ? O26 Yb5 O27 85.39(18) . . ? O23 Yb5 O27 163.0(2) . . ? O28 Yb5 O43 122.8(2) . . ? O25 Yb5 O43 79.5(2) . . ? O26 Yb5 O43 152.05(18) . . ? O23 Yb5 O43 111.20(18) . . ? O27 Yb5 O43 73.60(18) . . ? O28 Yb5 O44 78.12(19) . . ? O25 Yb5 O44 107.9(2) . . ? O26 Yb5 O44 146.79(19) . . ? O23 Yb5 O44 81.7(2) . . ? O27 Yb5 O44 89.2(2) . . ? O43 Yb5 O44 53.01(18) . . ? O28 Yb5 N9 127.18(19) . . ? O25 Yb5 N9 68.3(2) . . ? O26 Yb5 N9 70.01(18) . . ? O23 Yb5 N9 129.0(2) . . ? O27 Yb5 N9 66.7(2) . . ? O43 Yb5 N9 84.61(19) . . ? O44 Yb5 N9 136.4(2) . . ? O6 Fe1 O2 100.6(2) . . ? O6 Fe1 O7 92.1(2) . . ? O2 Fe1 O7 95.1(2) . . ? O6 Fe1 O5 153.0(2) . . ? O2 Fe1 O5 105.0(2) . . ? O7 Fe1 O5 77.4(2) . . ? O6 Fe1 O4 92.6(2) . . ? O2 Fe1 O4 78.65(19) . . ? O7 Fe1 O4 172.8(2) . . ? O5 Fe1 O4 100.6(2) . . ? O6 Fe1 N2 79.9(3) . . ? O2 Fe1 N2 157.2(2) . . ? O7 Fe1 N2 107.7(3) . . ? O5 Fe1 N2 79.8(3) . . ? O4 Fe1 N2 78.6(2) . . ? O8 Fe2 O12 98.6(2) . . ? O8 Fe2 O13 96.1(2) . . ? O12 Fe2 O13 93.8(2) . . ? O8 Fe2 O11 105.3(2) . . ? O12 Fe2 O11 155.3(2) . . ? O13 Fe2 O11 77.6(2) . . ? O8 Fe2 O10 78.7(2) . . ? O12 Fe2 O10 91.4(2) . . ? O13 Fe2 O10 173.2(2) . . ? O11 Fe2 O10 99.3(2) . . ? O8 Fe2 N4 158.8(2) . . ? O12 Fe2 N4 78.6(3) . . ? O13 Fe2 N4 104.9(2) . . ? O11 Fe2 N4 81.3(3) . . ? O10 Fe2 N4 80.4(2) . . ? O19 Fe3 O14 94.7(2) . . ? O19 Fe3 O18 92.3(2) . . ? O14 Fe3 O18 101.4(3) . . ? O19 Fe3 O17 78.5(2) . . ? O14 Fe3 O17 104.1(2) . . ? O18 Fe3 O17 153.4(3) . . ? O19 Fe3 O16 172.7(2) . . ? O14 Fe3 O16 78.0(2) . . ? O18 Fe3 O16 89.3(3) . . ? O17 Fe3 O16 103.0(2) . . ? O19 Fe3 N6 107.3(3) . . ? O14 Fe3 N6 157.9(3) . . ? O18 Fe3 N6 80.1(4) . . ? O17 Fe3 N6 79.0(3) . . ? O16 Fe3 N6 80.0(3) . . ? O24 Fe4 O20 101.8(3) . . ? O24 Fe4 O25 92.6(3) . . ? O20 Fe4 O25 93.2(2) . . ? O24 Fe4 O23 152.5(2) . . ? O20 Fe4 O23 104.3(2) . . ? O25 Fe4 O23 77.7(2) . . ? O24 Fe4 O22 91.8(3) . . ? O20 Fe4 O22 77.6(2) . . ? O25 Fe4 O22 170.5(2) . . ? O23 Fe4 O22 101.9(2) . . ? O24 Fe4 N8 79.6(4) . . ? O20 Fe4 N8 156.5(3) . . ? O25 Fe4 N8 110.1(3) . . ? O23 Fe4 N8 79.8(3) . . ? O22 Fe4 N8 79.0(3) . . ? O30 Fe5 O26 97.1(2) . . ? O30 Fe5 O1 93.5(2) . 2_666 ? O26 Fe5 O1 96.9(2) . 2_666 ? O30 Fe5 O29 156.0(2) . . ? O26 Fe5 O29 106.1(2) . . ? O1 Fe5 O29 77.61(19) 2_666 . ? O30 Fe5 O28 94.9(2) . . ? O26 Fe5 O28 78.0(2) . . ? O1 Fe5 O28 170.6(2) 2_666 . ? O29 Fe5 O28 96.2(2) . . ? O30 Fe5 N10 79.6(3) . . ? O26 Fe5 N10 157.2(2) . . ? O1 Fe5 N10 105.8(2) 2_666 . ? O29 Fe5 N10 81.4(2) . . ? O28 Fe5 N10 79.9(2) . . ? C5 N1 C1 111.7(7) . . ? C5 N1 C3 109.5(7) . . ? C1 N1 C3 110.7(8) . . ? C5 N1 Yb1 107.1(5) . . ? C1 N1 Yb1 110.1(4) . . ? C3 N1 Yb1 107.6(4) . . ? N1 C1 C2 113.7(8) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O1 C2 C1 108.3(6) . . ? O1 C2 Yb1 37.3(3) . . ? C1 C2 Yb1 81.9(5) . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? Yb1 C2 H2A 96.3 . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? Yb1 C2 H2B 145.8 . . ? H2A C2 H2B 108.4 . . ? C2 O1 Fe5 132.5(5) . 2_666 ? C2 O1 Yb1 120.0(4) . . ? Fe5 O1 Yb1 106.9(2) 2_666 . ? C4 C3 N1 111.4(7) . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? N1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O2 C4 C3 108.5(7) . . ? O2 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O2 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C4 O2 Fe1 127.5(5) . . ? C4 O2 Yb1 119.5(4) . . ? Fe1 O2 Yb1 104.6(2) . . ? N1 C5 C6 115.1(8) . . ? N1 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? O3 C6 C7 113.2(8) . . ? O3 C6 C5 111.4(7) . . ? C7 C6 C5 114.0(9) . . ? O3 C6 H6A 105.8 . . ? C7 C6 H6A 105.8 . . ? C5 C6 H6A 105.8 . . ? C6 O3 Yb1 120.9(5) . . ? C6 O3 H3 113(5) . . ? Yb1 O3 H3 104(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 N2 C10 112.7(7) . . ? C12 N2 C8 113.5(8) . . ? C10 N2 C8 113.4(8) . . ? C12 N2 Fe1 101.6(6) . . ? C10 N2 Fe1 106.1(6) . . ? C8 N2 Fe1 108.5(6) . . ? C9 C8 N2 115.0(9) . . ? C9 C8 H8A 108.5 . . ? N2 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? N2 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C8 C9 O4 118.5(9) . . ? C8 C9 H9A 107.7 . . ? O4 C9 H9A 107.7 . . ? C8 C9 H9B 107.7 . . ? O4 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? C9 O4 Fe1 117.4(6) . . ? C9 O4 Yb1 129.4(6) . . ? Fe1 O4 Yb1 104.1(2) . . ? C11 C10 N2 108.0(8) . . ? C11 C10 H10A 110.1 . . ? N2 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? N2 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? O5 C11 C10 107.5(7) . . ? O5 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? O5 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 O5 Fe1 113.4(5) . . ? C11 O5 Yb2 122.6(5) . . ? Fe1 O5 Yb2 106.1(2) . . ? N2 C12 C13 109.7(7) . . ? N2 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? N2 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O6 C13 C12 109.8(8) . . ? O6 C13 C14 110.9(9) . . ? C12 C13 C14 109.4(8) . . ? O6 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C13 O6 Fe1 117.9(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 N3 C15 117.7(10) . . ? C17 N3 C19 113.2(10) . . ? C15 N3 C19 103.5(8) . . ? C17 N3 Yb2 107.8(5) . . ? C15 N3 Yb2 106.2(5) . . ? C19 N3 Yb2 107.9(8) . . ? C16 C15 N3 112.9(8) . . ? C16 C15 H15A 109.0 . . ? N3 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? N3 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? O7 C16 C15 111.0(8) . . ? O7 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? O7 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 O7 Fe1 128.4(5) . . ? C16 O7 Yb2 123.7(5) . . ? Fe1 O7 Yb2 107.9(2) . . ? N3 C17 C18 119.7(8) . . ? N3 C17 H17A 107.4 . . ? C18 C17 H17A 107.4 . . ? N3 C17 H17B 107.4 . . ? C18 C17 H17B 107.4 . . ? H17A C17 H17B 106.9 . . ? O8 C18 C17 111.6(9) . . ? O8 C18 Yb2 38.6(3) . . ? C17 C18 Yb2 79.9(6) . . ? O8 C18 H18A 116.4 . . ? C17 C18 H18A 116.4 . . ? Yb2 C18 H18A 116.4 . . ? C18 O8 Fe2 129.4(5) . . ? C18 O8 Yb2 118.4(5) . . ? Fe2 O8 Yb2 105.8(2) . . ? C20 C19 N3 114.5(10) . . ? C20 C19 H19A 108.6 . . ? N3 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? N3 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C19 C20 O9 112.1(10) . . ? C19 C20 C21 121.5(14) . . ? O9 C20 C21 109.8(14) . . ? C19 C20 H20A 103.8 . . ? O9 C20 H20A 103.8 . . ? C21 C20 H20A 103.8 . . ? C20 O9 Yb2 121.6(7) . . ? C20 O9 H9 100(6) . . ? Yb2 O9 H9 110(6) . . ? 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 . . ? C22 N4 C26 116.0(8) . . ? C22 N4 C24 109.2(8) . . ? C26 N4 C24 114.8(8) . . ? C22 N4 Fe2 108.2(5) . . ? C26 N4 Fe2 102.5(5) . . ? C24 N4 Fe2 105.2(5) . . ? N4 C22 C23 114.2(8) . . ? N4 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N4 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? O10 C23 C22 110.5(8) . . ? O10 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? O10 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 O10 Fe2 115.2(5) . . ? C23 O10 Yb2 125.6(5) . . ? Fe2 O10 Yb2 103.9(2) . . ? N4 C24 C25 108.2(7) . . ? N4 C24 H24A 110.1 . . ? C25 C24 H24A 110.1 . . ? N4 C24 H24B 110.1 . . ? C25 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? O11 C25 C24 108.4(7) . . ? O11 C25 H25A 110.0 . . ? C24 C25 H25A 110.0 . . ? O11 C25 H25B 110.0 . . ? C24 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? C25 O11 Fe2 112.7(5) . . ? C25 O11 Yb3 120.9(5) . . ? Fe2 O11 Yb3 105.7(2) . . ? N4 C26 C27 109.7(8) . . ? N4 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N4 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? O12 C27 C26 108.0(9) . . ? O12 C27 C28 111.6(10) . . ? C26 C27 C28 111.4(10) . . ? O12 C27 H27A 108.6 . . ? C26 C27 H27A 108.6 . . ? C28 C27 H27A 108.6 . . ? C27 O12 Fe2 119.9(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 N5 C33 110.8(7) . . ? C29 N5 C31 111.5(8) . . ? C33 N5 C31 111.7(7) . . ? C29 N5 Yb3 106.9(5) . . ? C33 N5 Yb3 108.0(6) . . ? C31 N5 Yb3 107.7(5) . . ? N5 C29 C30 111.8(7) . . ? N5 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N5 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? O13 C30 C29 108.5(8) . . ? O13 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? O13 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? C30 O13 Fe2 126.9(5) . . ? C30 O13 Yb3 125.6(5) . . ? Fe2 O13 Yb3 107.1(2) . . ? N5 C31 C32 113.3(7) . . ? N5 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? N5 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? O14 C32 C31 109.9(7) . . ? O14 C32 Yb3 38.9(3) . . ? C31 C32 Yb3 83.2(5) . . ? O14 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? Yb3 C32 H32A 94.0 . . ? O14 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? Yb3 C32 H32B 147.7 . . ? H32A C32 H32B 108.2 . . ? C32 O14 Fe3 132.0(4) . . ? C32 O14 Yb3 117.7(4) . . ? Fe3 O14 Yb3 106.0(2) . . ? C34 C33 N5 113.8(8) . . ? C34 C33 H33A 108.8 . . ? N5 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? N5 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? O15 C34 C33 108.0(9) . . ? O15 C34 C35 114.0(13) . . ? C33 C34 C35 111.1(11) . . ? O15 C34 H34A 107.8 . . ? C33 C34 H34A 107.8 . . ? C35 C34 H34A 107.8 . . ? C34 O15 Yb3 125.1(7) . . ? C34 O15 H15 110(7) . . ? Yb3 O15 H15 104(7) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C40 N6 C36 114.5(10) . . ? C40 N6 C38 111.5(10) . . ? C36 N6 C38 112.3(10) . . ? C40 N6 Fe3 102.0(7) . . ? C36 N6 Fe3 109.2(6) . . ? C38 N6 Fe3 106.5(6) . . ? N6 C36 C37 112.3(9) . . ? N6 C36 H36A 109.1 . . ? C37 C36 H36A 109.1 . . ? N6 C36 H36B 109.1 . . ? C37 C36 H36B 109.1 . . ? H36A C36 H36B 107.9 . . ? O16 C37 C36 110.1(8) . . ? O16 C37 H37A 109.6 . . ? C36 C37 H37A 109.6 . . ? O16 C37 H37B 109.6 . . ? C36 C37 H37B 109.6 . . ? H37A C37 H37B 108.2 . . ? C37 O16 Fe3 114.7(5) . . ? C37 O16 Yb3 127.0(6) . . ? Fe3 O16 Yb3 103.8(2) . . ? N6 C38 C39 106.1(8) . . ? N6 C38 H38A 110.5 . . ? C39 C38 H38A 110.5 . . ? N6 C38 H38B 110.5 . . ? C39 C38 H38B 110.5 . . ? H38A C38 H38B 108.7 . . ? O17 C39 C38 106.1(8) . . ? O17 C39 H39A 110.5 . . ? C38 C39 H39A 110.5 . . ? O17 C39 H39B 110.5 . . ? C38 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? C39 O17 Fe3 114.4(6) . . ? C39 O17 Yb4 122.3(5) . . ? Fe3 O17 Yb4 105.4(2) . . ? N6 C40 C41 110.4(10) . . ? N6 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? N6 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? O18 C41 C42 108.1(12) . . ? O18 C41 C40 110.0(10) . . ? C42 C41 C40 115.6(13) . . ? O18 C41 H41A 107.6 . . ? C42 C41 H41A 107.6 . . ? C40 C41 H41A 107.6 . . ? C41 O18 Fe3 116.8(8) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C45 N7 C43 112.8(7) . . ? C45 N7 C47 112.6(7) . . ? C43 N7 C47 106.9(6) . . ? C45 N7 Yb4 108.6(4) . . ? C43 N7 Yb4 106.9(4) . . ? C47 N7 Yb4 108.9(5) . . ? N7 C43 C44 109.4(6) . . ? N7 C43 H43A 109.8 . . ? C44 C43 H43A 109.8 . . ? N7 C43 H43B 109.8 . . ? C44 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? O19 C44 C43 108.7(7) . . ? O19 C44 H44A 109.9 . . ? C43 C44 H44A 109.9 . . ? O19 C44 H44B 109.9 . . ? C43 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C44 O19 Fe3 126.6(5) . . ? C44 O19 Yb4 125.0(5) . . ? Fe3 O19 Yb4 107.9(2) . . ? N7 C45 C46 113.9(6) . . ? N7 C45 H45A 108.8 . . ? C46 C45 H45A 108.8 . . ? N7 C45 H45B 108.8 . . ? C46 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? O20 C46 C45 110.8(7) . . ? O20 C46 Yb4 39.6(3) . . ? C45 C46 Yb4 83.2(5) . . ? O20 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? Yb4 C46 H46A 148.0 . . ? O20 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? Yb4 C46 H46B 94.1 . . ? H46A C46 H46B 108.1 . . ? C46 O20 Fe4 133.2(5) . . ? C46 O20 Yb4 116.8(4) . . ? Fe4 O20 Yb4 106.0(2) . . ? C48 C47 N7 112.1(8) . . ? C48 C47 H47A 109.2 . . ? N7 C47 H47A 109.2 . . ? C48 C47 H47B 109.2 . . ? N7 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? O21 C48 C47 110.8(9) . . ? O21 C48 C49 110.7(12) . . ? C47 C48 C49 112.5(14) . . ? O21 C48 H48A 107.6 . . ? C47 C48 H48A 107.6 . . ? C49 C48 H48A 107.6 . . ? C48 O21 Yb4 122.1(6) . . ? C48 O21 H21 111(6) . . ? Yb4 O21 H21 101(6) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 N8 C54 112.3(9) . . ? C52 N8 C50 109.5(11) . . ? C54 N8 C50 117.3(10) . . ? C52 N8 Fe4 106.4(7) . . ? C54 N8 Fe4 101.7(7) . . ? C50 N8 Fe4 108.7(6) . . ? N8 C50 C51 111.3(9) . . ? N8 C50 H50A 109.4 . . ? C51 C50 H50A 109.4 . . ? N8 C50 H50B 109.4 . . ? C51 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? O22 C51 C50 110.5(8) . . ? O22 C51 H51A 109.5 . . ? C50 C51 H51A 109.5 . . ? O22 C51 H51B 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C51 O22 Fe4 115.4(5) . . ? C51 O22 Yb4 126.2(5) . . ? Fe4 O22 Yb4 103.9(2) . . ? N8 C52 C53 108.4(8) . . ? N8 C52 H52A 110.0 . . ? C53 C52 H52A 110.0 . . ? N8 C52 H52B 110.0 . . ? C53 C52 H52B 110.0 . . ? H52A C52 H52B 108.4 . . ? O23 C53 C52 107.3(9) . . ? O23 C53 H53A 110.3 . . ? C52 C53 H53A 110.3 . . ? O23 C53 H53B 110.3 . . ? C52 C53 H53B 110.3 . . ? H53A C53 H53B 108.5 . . ? C53 O23 Fe4 114.1(7) . . ? C53 O23 Yb5 122.4(5) . . ? Fe4 O23 Yb5 105.6(2) . . ? N8 C54 C55 110.2(9) . . ? N8 C54 H54A 109.6 . . ? C55 C54 H54A 109.6 . . ? N8 C54 H54B 109.6 . . ? C55 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? O24 C55 C54 109.2(11) . . ? O24 C55 C56 110.4(12) . . ? C54 C55 C56 111.2(12) . . ? O24 C55 H55A 108.7 . . ? C54 C55 H55A 108.7 . . ? C56 C55 H55A 108.7 . . ? C55 O24 Fe4 119.7(8) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C61 N9 C57 112.6(8) . . ? C61 N9 C59 109.0(8) . . ? C57 N9 C59 109.7(10) . . ? C61 N9 Yb5 106.9(6) . . ? C57 N9 Yb5 110.3(5) . . ? C59 N9 Yb5 108.1(5) . . ? N9 C57 C58 114.2(9) . . ? N9 C57 H57A 108.7 . . ? C58 C57 H57A 108.7 . . ? N9 C57 H57B 108.7 . . ? C58 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? O25 C58 C57 109.1(7) . . ? O25 C58 Yb5 36.6(4) . . ? C57 C58 Yb5 83.0(6) . . ? O25 C58 H58A 109.9 . . ? C57 C58 H58A 109.9 . . ? Yb5 C58 H58A 96.6 . . ? O25 C58 H58B 109.9 . . ? C57 C58 H58B 109.9 . . ? Yb5 C58 H58B 145.1 . . ? H58A C58 H58B 108.3 . . ? C58 O25 Fe4 130.5(5) . . ? C58 O25 Yb5 121.0(5) . . ? Fe4 O25 Yb5 108.2(2) . . ? C60 C59 N9 114.3(9) . . ? C60 C59 H59A 108.7 . . ? N9 C59 H59A 108.7 . . ? C60 C59 H59B 108.7 . . ? N9 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? C59 C60 O26 112.6(8) . . ? C59 C60 H60A 109.1 . . ? O26 C60 H60A 109.1 . . ? C59 C60 H60B 109.1 . . ? O26 C60 H60B 109.1 . . ? H60A C60 H60B 107.8 . . ? C60 O26 Fe5 125.0(4) . . ? C60 O26 Yb5 119.6(4) . . ? Fe5 O26 Yb5 104.7(2) . . ? N9 C61 C62 118.2(8) . . ? N9 C61 H61A 107.8 . . ? C62 C61 H61A 107.8 . . ? N9 C61 H61B 107.8 . . ? C62 C61 H61B 107.8 . . ? H61A C61 H61B 107.1 . . ? O27 C62 C63 112.7(8) . . ? O27 C62 C61 111.3(7) . . ? C63 C62 C61 118.8(9) . . ? O27 C62 H62A 104.1 . . ? C63 C62 H62A 104.1 . . ? C61 C62 H62A 104.1 . . ? C62 O27 Yb5 121.5(5) . . ? C62 O27 H27 112(6) . . ? Yb5 O27 H27 107(6) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C68 N10 C66 114.2(7) . . ? C68 N10 C64 114.8(8) . . ? C66 N10 C64 111.8(7) . . ? C68 N10 Fe5 103.5(5) . . ? C66 N10 Fe5 105.1(5) . . ? C64 N10 Fe5 106.3(6) . . ? C65 C64 N10 116.7(9) . . ? C65 C64 H64A 108.1 . . ? N10 C64 H64A 108.1 . . ? C65 C64 H64B 108.1 . . ? N10 C64 H64B 108.1 . . ? H64A C64 H64B 107.3 . . ? O28 C65 C64 115.5(9) . . ? O28 C65 H65A 122.2 . . ? C64 C65 H65A 122.2 . . ? C65 O28 Fe5 118.4(6) . . ? C65 O28 Yb5 133.0(5) . . ? Fe5 O28 Yb5 104.5(2) . . ? N10 C66 C67 110.1(7) . . ? N10 C66 H66A 109.6 . . ? C67 C66 H66A 109.6 . . ? N10 C66 H66B 109.6 . . ? C67 C66 H66B 109.6 . . ? H66A C66 H66B 108.2 . . ? O29 C67 C66 107.9(7) . . ? O29 C67 H67A 110.1 . . ? C66 C67 H67A 110.1 . . ? O29 C67 H67B 110.1 . . ? C66 C67 H67B 110.1 . . ? H67A C67 H67B 108.4 . . ? C67 O29 Fe5 114.7(5) . . ? C67 O29 Yb1 120.6(4) . 2_666 ? Fe5 O29 Yb1 105.7(2) . 2_666 ? N10 C68 C69 107.3(7) . . ? N10 C68 H68A 110.2 . . ? C69 C68 H68A 110.2 . . ? N10 C68 H68B 110.2 . . ? C69 C68 H68B 110.2 . . ? H68A C68 H68B 108.5 . . ? O30 C69 C70 109.4(9) . . ? O30 C69 C68 109.4(8) . . ? C70 C69 C68 111.1(9) . . ? O30 C69 H69A 109.0 . . ? C70 C69 H69A 109.0 . . ? C68 C69 H69A 109.0 . . ? C69 O30 Fe5 118.7(5) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O33 N11 O32 122.1(8) . . ? O33 N11 O31 120.4(7) . . ? O32 N11 O31 117.5(6) . . ? N11 O31 Yb1 93.1(4) . . ? N11 O32 Yb1 96.5(5) . . ? O36 N12 O35 122.0(10) . . ? O36 N12 O34 119.4(10) . . ? O35 N12 O34 118.5(8) . . ? N12 O34 Yb2 93.3(5) . . ? N12 O35 Yb2 94.7(5) . . ? O39 N13 O38 121.8(11) . . ? O39 N13 O37 121.6(11) . . ? O38 N13 O37 116.6(8) . . ? N13 O37 Yb3 93.2(6) . . ? N13 O38 Yb3 96.3(6) . . ? O42 N14 O40 119.4(9) . . ? O42 N14 O41 122.1(8) . . ? O40 N14 O41 118.5(7) . . ? N14 O40 Yb4 93.0(5) . . ? N14 O41 Yb4 94.7(4) . . ? O45 N15 O43 121.6(7) . . ? O45 N15 O44 120.1(7) . . ? O43 N15 O44 118.3(6) . . ? N15 O43 Yb5 94.7(4) . . ? N15 O44 Yb5 94.0(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O6 0.89(4) 1.70(4) 2.584(7) 176(8) . O9 H9 O12 0.93(4) 1.63(4) 2.554(8) 168(9) . O15 H15 O18 0.92(4) 1.62(5) 2.528(9) 166(11) . O21 H21 O24 0.91(4) 1.66(4) 2.557(8) 168(9) . O27 H27 O30 0.86(4) 1.70(4) 2.550(7) 166(8) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.951 _refine_diff_density_min -1.530 _refine_diff_density_rms 0.126 _database_code_depnum_ccdc_archive 'CCDC 912849' ####################################################################### # # 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_amdf3ybx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H60 N2 O14 Yb2' _chemical_formula_sum 'C46 H60 N2 O14 Yb2' _chemical_formula_weight 1211.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8980(15) _cell_length_b 14.2365(15) _cell_length_c 17.039(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.369(13) _cell_angle_gamma 90.00 _cell_volume 2394.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6891 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 26.28 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 3.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.767 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15933 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4544 _reflns_number_gt 2870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The positions of O-H H atoms were restrained: DFIX 0.92 0.04 O2 H2 O3 H3 DFIX 1.78 0.04 H3 O7_$1 The phenyl ring of one benzoate ligand was disordered, and refined as two partial-occupancy rigid hexagons (AFIX 66; SADI C17 C18A C17 C18B) ; _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^)+(0.0482P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4544 _refine_ls_number_parameters 289 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.982 _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 Yb1 Yb 0.54099(4) 0.53921(3) 0.09937(2) 0.03594(13) Uani 1 1 d . . . N1 N 0.7135(7) 0.4208(5) 0.1493(4) 0.0365(17) Uani 1 1 d . . . C1 C 0.8137(8) 0.4180(7) 0.0888(5) 0.040(2) Uani 1 1 d . . . H1A H 0.8757 0.3642 0.0993 0.048 Uiso 1 1 calc R . . H1B H 0.8685 0.4763 0.0920 0.048 Uiso 1 1 calc R . . C2 C 0.7437(8) 0.4088(7) 0.0056(5) 0.041(2) Uani 1 1 d . . . H2A H 0.7177 0.3417 -0.0042 0.049 Uiso 1 1 calc R . . C3 C 0.8440(9) 0.4390(8) -0.0536(6) 0.052(3) Uani 1 1 d . . . H3A H 0.8012 0.4329 -0.1072 0.079 Uiso 1 1 calc R . . H3B H 0.9246 0.3989 -0.0478 0.079 Uiso 1 1 calc R . . H3C H 0.8704 0.5046 -0.0439 0.079 Uiso 1 1 calc R . . O1 O 0.6261(5) 0.4651(5) -0.0011(3) 0.0352(12) Uani 1 1 d . . . C4 C 0.7803(9) 0.4540(8) 0.2258(5) 0.048(2) Uani 1 1 d . . . H4A H 0.8394 0.5082 0.2160 0.058 Uiso 1 1 calc R . . H4B H 0.8382 0.4032 0.2494 0.058 Uiso 1 1 calc R . . C5 C 0.6794(9) 0.4827(7) 0.2830(5) 0.043(2) Uani 1 1 d . . . H5A H 0.6461 0.4253 0.3093 0.051 Uiso 1 1 calc R . . C6 C 0.7423(10) 0.5497(8) 0.3460(6) 0.058(3) Uani 1 1 d . . . H6A H 0.6750 0.5649 0.3834 0.088 Uiso 1 1 calc R . . H6B H 0.7712 0.6075 0.3209 0.088 Uiso 1 1 calc R . . H6C H 0.8209 0.5196 0.3740 0.088 Uiso 1 1 calc R . . O2 O 0.5669(6) 0.5267(5) 0.2376(3) 0.0421(15) Uani 1 1 d D . . H2 H 0.546(9) 0.573(5) 0.273(5) 0.050 Uiso 1 1 d D . . C7 C 0.6521(9) 0.3266(7) 0.1560(6) 0.045(2) Uani 1 1 d . . . H7A H 0.7062 0.2900 0.1966 0.054 Uiso 1 1 calc R . . H7B H 0.6554 0.2932 0.1052 0.054 Uiso 1 1 calc R . . C8 C 0.5055(9) 0.3311(7) 0.1777(6) 0.045(2) Uani 1 1 d . . . H8A H 0.5041 0.3547 0.2329 0.054 Uiso 1 1 calc R . . C9 C 0.4432(10) 0.2335(7) 0.1729(6) 0.047(2) Uani 1 1 d . . . H9A H 0.3485 0.2369 0.1858 0.071 Uiso 1 1 calc R . . H9B H 0.4938 0.1918 0.2104 0.071 Uiso 1 1 calc R . . H9C H 0.4472 0.2088 0.1195 0.071 Uiso 1 1 calc R . . O3 O 0.4317(6) 0.3951(4) 0.1260(3) 0.0370(14) Uani 1 1 d D . . H3 H 0.415(9) 0.372(6) 0.077(3) 0.044 Uiso 1 1 d D . . O4 O 0.4230(6) 0.6561(5) 0.1464(4) 0.0461(16) Uani 1 1 d . . . O5 O 0.4469(9) 0.6824(6) 0.2752(5) 0.077(2) Uani 1 1 d . . . C10 C 0.4255(10) 0.7089(8) 0.2059(6) 0.048(2) Uani 1 1 d . . . C11 C 0.3954(9) 0.8117(8) 0.1901(6) 0.046(2) Uani 1 1 d . . . C12 C 0.3513(10) 0.8693(9) 0.2492(7) 0.059(3) Uani 1 1 d . . . H12A H 0.3487 0.8461 0.3013 0.070 Uiso 1 1 calc R . . C13 C 0.3120(11) 0.9594(10) 0.2316(8) 0.067(3) Uani 1 1 d . . . H13A H 0.2740 0.9967 0.2706 0.081 Uiso 1 1 calc R . . C14 C 0.3267(12) 0.9969(9) 0.1582(10) 0.079(4) Uani 1 1 d . . . H14A H 0.3028 1.0606 0.1476 0.094 Uiso 1 1 calc R . . C15 C 0.3769(11) 0.9412(8) 0.0992(8) 0.065(3) Uani 1 1 d . . . H15A H 0.3877 0.9667 0.0485 0.077 Uiso 1 1 calc R . . C16 C 0.4103(9) 0.8494(8) 0.1153(7) 0.054(3) Uani 1 1 d . . . H16A H 0.4439 0.8111 0.0755 0.065 Uiso 1 1 calc R . . O6 O 0.7329(6) 0.6328(5) 0.1292(4) 0.0447(15) Uani 1 1 d . A . O7 O 0.6190(6) 0.6752(5) 0.0183(3) 0.0420(15) Uani 1 1 d . A . C17 C 0.7232(9) 0.6822(7) 0.0684(5) 0.042(2) Uani 1 1 d D . . C18A C 0.8428(18) 0.7400(15) 0.0514(13) 0.040(7) Uiso 0.56 1 d PD A 1 C19A C 0.948(2) 0.7510(18) 0.1095(15) 0.040(7) Uiso 0.56 1 d P A 1 H19A H 0.9458 0.7166 0.1572 0.048 Uiso 0.56 1 calc PR A 1 C20A C 1.053(2) 0.8087(16) 0.1003(14) 0.047(6) Uiso 0.56 1 d P A 1 H20A H 1.1157 0.8251 0.1434 0.056 Uiso 0.56 1 calc PR A 1 C21A C 1.067(2) 0.8442(17) 0.0234(13) 0.067(6) Uiso 0.56 1 d P A 1 H21A H 1.1458 0.8801 0.0146 0.080 Uiso 0.56 1 calc PR A 1 C22A C 0.969(2) 0.8286(19) -0.0415(15) 0.079(7) Uiso 0.56 1 d P A 1 H22A H 0.9793 0.8534 -0.0925 0.095 Uiso 0.56 1 calc PR A 1 C23A C 0.8530(19) 0.7721(15) -0.0237(11) 0.054(5) Uiso 0.56 1 d P A 1 H23A H 0.7845 0.7575 -0.0640 0.065 Uiso 0.56 1 calc PR A 1 C18B C 0.822(2) 0.7599(18) 0.0562(16) 0.040(8) Uiso 0.44 1 d PD A 2 C19B C 0.933(3) 0.771(2) 0.1086(18) 0.036(9) Uiso 0.44 1 d P A 2 H19B H 0.9404 0.7361 0.1564 0.043 Uiso 0.44 1 calc PR A 2 C20B C 1.038(3) 0.8359(18) 0.0901(15) 0.035(6) Uiso 0.44 1 d P A 2 H20B H 1.1229 0.8341 0.1202 0.043 Uiso 0.44 1 calc PR A 2 C21B C 1.020(2) 0.8958(18) 0.0344(12) 0.046(5) Uiso 0.44 1 d P A 2 H21B H 1.0856 0.9434 0.0289 0.055 Uiso 0.44 1 calc PR A 2 C22B C 0.909(3) 0.893(2) -0.0169(16) 0.070(7) Uiso 0.44 1 d P A 2 H22B H 0.8987 0.9346 -0.0602 0.084 Uiso 0.44 1 calc PR A 2 C23B C 0.806(3) 0.824(2) -0.0041(15) 0.059(6) Uiso 0.44 1 d P A 2 H23B H 0.7258 0.8230 -0.0382 0.070 Uiso 0.44 1 calc PR A 2 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 Yb1 0.03424(18) 0.0346(2) 0.03869(19) 0.0000(2) 0.00078(12) -0.0010(2) N1 0.033(4) 0.033(4) 0.043(4) 0.001(3) -0.002(3) 0.000(3) C1 0.031(4) 0.047(6) 0.041(5) 0.001(4) 0.001(4) 0.002(4) C2 0.029(4) 0.039(6) 0.056(6) -0.007(4) 0.005(4) 0.008(4) C3 0.037(5) 0.071(8) 0.051(5) 0.001(5) 0.009(4) -0.009(5) O1 0.029(2) 0.040(3) 0.036(3) -0.002(3) -0.001(2) 0.002(3) C4 0.041(4) 0.057(6) 0.045(5) 0.002(5) -0.009(4) -0.002(5) C5 0.039(4) 0.046(7) 0.043(5) 0.003(4) 0.000(4) 0.003(4) C6 0.056(6) 0.059(7) 0.059(6) -0.018(6) -0.006(5) -0.001(6) O2 0.048(3) 0.047(4) 0.030(3) 0.002(3) -0.005(2) 0.008(3) C7 0.043(5) 0.045(6) 0.047(5) -0.001(4) 0.005(4) 0.000(4) C8 0.048(5) 0.040(6) 0.046(5) 0.003(4) 0.000(4) -0.002(4) C9 0.049(5) 0.039(6) 0.052(6) 0.005(5) -0.002(5) -0.003(5) O3 0.039(3) 0.030(3) 0.041(3) 0.008(3) -0.001(3) -0.009(3) O4 0.048(4) 0.039(4) 0.049(4) -0.007(3) -0.008(3) 0.008(3) O5 0.104(6) 0.075(6) 0.051(5) -0.009(4) -0.001(4) 0.032(5) C10 0.049(6) 0.045(6) 0.049(6) -0.005(5) 0.004(5) 0.008(5) C11 0.031(5) 0.056(7) 0.049(6) -0.011(5) -0.007(4) 0.002(4) C12 0.050(6) 0.065(8) 0.061(6) -0.021(6) 0.007(5) -0.004(5) C13 0.066(7) 0.050(7) 0.087(8) -0.018(8) 0.002(6) -0.003(7) C14 0.056(7) 0.046(7) 0.133(13) -0.027(8) 0.000(8) -0.013(6) C15 0.050(6) 0.055(8) 0.089(8) 0.009(6) 0.006(5) -0.010(5) C16 0.039(5) 0.057(7) 0.068(7) -0.005(6) 0.005(5) -0.003(5) O6 0.040(3) 0.039(4) 0.053(4) 0.003(3) -0.005(3) -0.011(3) O7 0.041(3) 0.042(4) 0.042(4) 0.004(3) -0.005(3) -0.009(3) C17 0.044(5) 0.043(6) 0.038(5) -0.008(4) 0.004(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O4 2.217(6) . ? Yb1 O1 2.230(5) . ? Yb1 O1 2.263(5) 3_665 ? Yb1 O6 2.345(6) . ? Yb1 O2 2.357(5) . ? Yb1 O3 2.380(6) . ? Yb1 N1 2.502(7) . ? Yb1 O7 2.533(6) . ? N1 C7 1.480(12) . ? N1 C1 1.485(11) . ? N1 C4 1.493(11) . ? C1 C2 1.534(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.411(10) . ? C2 C3 1.531(12) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O1 Yb1 2.263(5) 3_665 ? C4 C5 1.504(13) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O2 1.448(10) . ? C5 C6 1.532(13) . ? C5 H5A 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O2 H2 0.93(4) . ? C7 C8 1.526(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O3 1.429(11) . ? C8 C9 1.519(13) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O3 H3 0.90(3) . ? O4 C10 1.262(11) . ? O5 C10 1.243(12) . ? C10 C11 1.514(15) . ? C11 C12 1.395(14) . ? C11 C16 1.400(14) . ? C12 C13 1.367(17) . ? C12 H12A 0.9500 . ? C13 C14 1.378(19) . ? C13 H13A 0.9500 . ? C14 C15 1.401(17) . ? C14 H14A 0.9500 . ? C15 C16 1.370(15) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? O6 C17 1.249(11) . ? O7 C17 1.291(10) . ? C17 C18A 1.489(16) . ? C17 C18B 1.500(17) . ? C18A C23A 1.37(3) . ? C18A C19A 1.39(3) . ? C19A C20A 1.34(3) . ? C19A H19A 0.9500 . ? C20A C21A 1.42(3) . ? C20A H20A 0.9500 . ? C21A C22A 1.43(3) . ? C21A H21A 0.9500 . ? C22A C23A 1.46(3) . ? C22A H22A 0.9500 . ? C23A H23A 0.9500 . ? C18B C19B 1.37(4) . ? C18B C23B 1.37(4) . ? C19B C20B 1.45(4) . ? C19B H19B 0.9500 . ? C20B C21B 1.28(3) . ? C20B H20B 0.9500 . ? C21B C22B 1.35(3) . ? C21B H21B 0.9500 . ? C22B C23B 1.44(4) . ? C22B H22B 0.9500 . ? C23B H23B 0.9500 . ? 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 Yb1 O1 150.8(2) . . ? O4 Yb1 O1 85.0(2) . 3_665 ? O1 Yb1 O1 73.6(2) . 3_665 ? O4 Yb1 O6 86.3(2) . . ? O1 Yb1 O6 95.1(2) . . ? O1 Yb1 O6 135.3(2) 3_665 . ? O4 Yb1 O2 73.5(2) . . ? O1 Yb1 O2 135.4(2) . . ? O1 Yb1 O2 139.06(19) 3_665 . ? O6 Yb1 O2 78.5(2) . . ? O4 Yb1 O3 108.6(2) . . ? O1 Yb1 O3 86.7(2) . . ? O1 Yb1 O3 78.5(2) 3_665 . ? O6 Yb1 O3 145.3(2) . . ? O2 Yb1 O3 76.2(2) . . ? O4 Yb1 N1 138.4(2) . . ? O1 Yb1 N1 69.8(2) . . ? O1 Yb1 N1 132.4(2) 3_665 . ? O6 Yb1 N1 77.8(2) . . ? O2 Yb1 N1 65.8(2) . . ? O3 Yb1 N1 70.3(2) . . ? O4 Yb1 O7 79.3(2) . . ? O1 Yb1 O7 78.1(2) . . ? O1 Yb1 O7 81.6(2) 3_665 . ? O6 Yb1 O7 53.7(2) . . ? O2 Yb1 O7 126.0(2) . . ? O3 Yb1 O7 157.67(19) . . ? N1 Yb1 O7 118.2(2) . . ? C7 N1 C1 109.2(7) . . ? C7 N1 C4 112.1(7) . . ? C1 N1 C4 109.9(6) . . ? C7 N1 Yb1 111.3(5) . . ? C1 N1 Yb1 104.8(5) . . ? C4 N1 Yb1 109.2(6) . . ? N1 C1 C2 111.4(7) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? O1 C2 C3 111.0(8) . . ? O1 C2 C1 109.7(7) . . ? C3 C2 C1 108.4(7) . . ? O1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 O1 Yb1 124.3(5) . . ? C2 O1 Yb1 126.6(5) . 3_665 ? Yb1 O1 Yb1 106.4(2) . 3_665 ? N1 C4 C5 112.3(7) . . ? N1 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? O2 C5 C4 107.0(7) . . ? O2 C5 C6 111.1(8) . . ? C4 C5 C6 111.7(8) . . ? O2 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 O2 Yb1 126.0(5) . . ? C5 O2 H2 99(6) . . ? Yb1 O2 H2 126(6) . . ? N1 C7 C8 112.6(8) . . ? N1 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? O3 C8 C9 111.3(7) . . ? O3 C8 C7 109.1(7) . . ? C9 C8 C7 109.7(8) . . ? O3 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 O3 Yb1 116.7(5) . . ? C8 O3 H3 113(6) . . ? Yb1 O3 H3 101(6) . . ? C10 O4 Yb1 139.4(6) . . ? O5 C10 O4 125.1(10) . . ? O5 C10 C11 118.7(9) . . ? O4 C10 C11 116.2(9) . . ? C12 C11 C16 119.4(10) . . ? C12 C11 C10 120.5(10) . . ? C16 C11 C10 120.0(9) . . ? C13 C12 C11 119.5(11) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 121.0(12) . . ? C12 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C13 C14 C15 120.0(13) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 119.3(12) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C15 C16 C11 120.5(11) . . ? C15 C16 H16A 119.7 . . ? C11 C16 H16A 119.7 . . ? C17 O6 Yb1 97.4(5) . . ? C17 O7 Yb1 87.7(5) . . ? O6 C17 O7 120.8(8) . . ? O6 C17 C18A 117.4(11) . . ? O7 C17 C18A 121.3(11) . . ? O6 C17 C18B 121.3(13) . . ? O7 C17 C18B 117.3(13) . . ? C23A C18A C19A 121.6(16) . . ? C23A C18A C17 118.9(16) . . ? C19A C18A C17 119.2(18) . . ? C20A C19A C18A 122(2) . . ? C20A C19A H19A 119.0 . . ? C18A C19A H19A 119.0 . . ? C19A C20A C21A 117(2) . . ? C19A C20A H20A 121.5 . . ? C21A C20A H20A 121.5 . . ? C20A C21A C22A 123(2) . . ? C20A C21A H21A 118.4 . . ? C22A C21A H21A 118.4 . . ? C21A C22A C23A 115(2) . . ? C21A C22A H22A 122.4 . . ? C23A C22A H22A 122.4 . . ? C18A C23A C22A 119.7(18) . . ? C18A C23A H23A 120.2 . . ? C22A C23A H23A 120.2 . . ? C19B C18B C23B 117(2) . . ? C19B C18B C17 119(2) . . ? C23B C18B C17 124(2) . . ? C18B C19B C20B 119(3) . . ? C18B C19B H19B 120.5 . . ? C20B C19B H19B 120.5 . . ? C21B C20B C19B 122(2) . . ? C21B C20B H20B 119.2 . . ? C19B C20B H20B 119.2 . . ? C20B C21B C22B 121(3) . . ? C20B C21B H21B 119.3 . . ? C22B C21B H21B 119.3 . . ? C21B C22B C23B 118(3) . . ? C21B C22B H22B 120.9 . . ? C23B C22B H22B 120.9 . . ? C18B C23B C22B 122(2) . . ? C18B C23B H23B 119.1 . . ? C22B C23B H23B 119.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O5 0.93(4) 1.84(7) 2.618(10) 139(8) . O3 H3 O7 0.90(3) 1.77(3) 2.666(8) 179(9) 3_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.721 _refine_diff_density_min -2.116 _refine_diff_density_rms 0.180 _database_code_depnum_ccdc_archive 'CCDC 912850'