# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Zhan Shi' _publ_contact_author_email zshi@mail.jlu.edu.cn loop_ _publ_author_name 'Qi Zhou' 'Fen Yang' 'Dan Liu' 'Yu Peng' 'Guanghua Li' 'Zhan Shi' ; Shouhua Feng ; data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 857518' # 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 1.000 0.000 0.500 483 70 ' ' 2 1.000 0.500 0.000 483 71 ' ' _platon_squeeze_details ; The Platon SQUEEZE procedure was applied to recover 141 electrons per unit cell in one void (total volume 966 ^A^3); that is 35.25 electrons per formula unit. Lattice solvent water molecules (10 electrons/H2O) were present, and the electrons recovered by SQUEEZE have been assigned as 3 water molecules per formula unit. These water molecules have been included in the formula for the calculation of intensive properties. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C103 H130 Dy2 Fe6 N18 Na2 O44' _chemical_formula_sum 'C103 H130 Dy2 Fe6 N18 Na2 O44' _chemical_formula_weight 3030.33 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' Na Na 0.0362 0.0249 '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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.567(5) _cell_length_b 23.458(5) _cell_length_c 29.624(6) _cell_angle_alpha 90.00 _cell_angle_beta 121.65(3) _cell_angle_gamma 90.00 _cell_volume 13941(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24395 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6144 _exptl_absorpt_coefficient_mu 1.751 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6041 _exptl_absorpt_correction_T_max 0.6594 _exptl_absorpt_process_details Process-auto _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 107110 _diffrn_reflns_av_R_equivalents 0.1066 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 24395 _reflns_number_gt 16612 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+51.7576P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24395 _refine_ls_number_parameters 1705 _refine_ls_number_restraints 488 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2120 _refine_ls_wR_factor_gt 0.1941 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.51529(2) 0.769664(17) 0.371557(15) 0.03747(13) Uani 1 1 d . A . Dy2 Dy 0.67603(2) 0.721915(18) 0.503267(17) 0.04157(14) Uani 1 1 d . A . Fe1 Fe 0.22478(7) 0.79093(5) 0.25592(5) 0.0437(3) Uani 1 1 d . A . Fe2 Fe 0.28462(6) 0.91961(5) 0.28317(5) 0.0426(3) Uani 1 1 d . A . Fe3 Fe 0.36754(6) 0.81838(5) 0.27543(5) 0.0385(3) Uani 1 1 d . A . Fe4 Fe 0.80754(6) 0.60130(6) 0.70176(5) 0.0427(3) Uani 1 1 d . B . Fe5 Fe 0.82759(7) 0.73451(6) 0.73289(5) 0.0500(4) Uani 1 1 d . . . Fe6 Fe 0.80403(6) 0.69362(6) 0.62233(6) 0.0455(3) Uani 1 1 d . . . Na1 Na 0.1800(2) 0.87998(16) 0.3283(2) 0.0664(12) Uani 1 1 d . A . Na2 Na 0.7573(2) 0.64605(16) 0.78515(15) 0.0570(10) Uani 1 1 d D B . N1 N 0.2660(4) 0.7077(3) 0.2811(3) 0.0433(18) Uani 1 1 d . . . N2 N 0.3805(4) 0.9579(3) 0.3317(3) 0.0398(17) Uani 1 1 d . A . N3 N 0.7548(4) 0.5520(3) 0.6322(3) 0.0430(19) Uani 1 1 d . . . N4 N 0.7858(4) 0.8114(3) 0.6909(3) 0.0475(19) Uani 1 1 d . B . N5 N 0.1427(5) 0.7621(4) 0.1918(4) 0.079(3) Uani 1 1 d U . . N6 N 0.1171(7) 0.7185(7) 0.1901(6) 0.112(3) Uani 1 1 d U . . N7 N 0.0875(7) 0.6721(7) 0.1876(6) 0.125(3) Uani 1 1 d U . . N8 N 0.2468(5) 0.9905(4) 0.2415(4) 0.071(3) Uani 1 1 d D . . N9 N 0.2068(7) 1.0173(6) 0.2362(6) 0.069(4) Uani 0.70 1 d P A 1 N10 N 0.1646(8) 1.0497(7) 0.2327(6) 0.087(4) Uani 0.70 1 d PU A 1 N9' N 0.2280(14) 1.0058(12) 0.2000(7) 0.057(7) Uani 0.30 1 d PDU A 2 N10' N 0.216(2) 1.016(2) 0.1584(9) 0.131(14) Uani 0.30 1 d PDU A 2 N11 N 0.8668(4) 0.5346(4) 0.7397(4) 0.063(3) Uani 1 1 d . . . N12 N 0.8446(4) 0.4879(4) 0.7361(4) 0.066(3) Uani 1 1 d . . . N13 N 0.8231(6) 0.4434(5) 0.7335(5) 0.089(3) Uani 1 1 d U . . N14 N 0.9097(8) 0.7707(6) 0.7869(5) 0.062(4) Uani 0.60 1 d PDU B 1 N16 N 0.9669(11) 0.7973(10) 0.8754(5) 0.106(5) Uani 0.60 1 d PDU B 1 N14' N 0.8818(8) 0.7792(12) 0.7978(10) 0.079(6) Uani 0.40 1 d PDU B 2 N16' N 0.9934(8) 0.8036(14) 0.8513(13) 0.106(8) Uani 0.40 1 d PDU B 2 N15 N 0.9367(6) 0.7888(5) 0.8290(5) 0.095(4) Uani 1 1 d DU . . N17 N 0.2695(8) 0.6559(7) 0.9497(7) 0.141(4) Uani 1 1 d U . . N18 N 0.2954(14) 0.8509(12) 0.5996(14) 0.125(7) Uani 0.40 1 d PDU . . N19 N 0.2631(12) 0.6131(11) 0.5337(9) 0.129(5) Uani 0.60 1 d PU . . O1 O 0.1972(3) 0.7867(2) 0.3069(3) 0.0452(15) Uani 1 1 d . . . O2 O 0.2805(3) 0.7829(2) 0.2231(2) 0.0428(15) Uani 1 1 d . . . O3 O 0.4040(3) 0.7471(2) 0.3138(2) 0.0417(14) Uani 1 1 d . . . O4 O 0.3114(5) 0.6104(4) 0.2030(4) 0.054(2) Uani 0.70 1 d P C 1 H4 H 0.3519 0.6149 0.2186 0.100 Uiso 0.70 1 calc P D 1 O4' O 0.2140(12) 0.6119(11) 0.2073(10) 0.072(7) Uani 0.30 1 d P C 2 H4' H 0.1978 0.6198 0.2252 0.100 Uiso 0.30 1 calc P E 2 O5 O 0.1350(4) 0.8064(3) 0.3561(3) 0.064(2) Uani 1 1 d . . . O6 O 0.2697(3) 0.9368(2) 0.3400(2) 0.0454(15) Uani 1 1 d . . . O7 O 0.3311(3) 0.8962(2) 0.2461(2) 0.0450(15) Uani 1 1 d . . . O8 O 0.4490(3) 0.8494(2) 0.3348(2) 0.0416(14) Uani 1 1 d . . . O9 O 0.4945(3) 0.9997(3) 0.2857(3) 0.0610(19) Uani 1 1 d . . . H9 H 0.5159 1.0284 0.2883 0.100 Uiso 1 1 calc . . . O10 O 0.2084(3) 0.9557(3) 0.3901(3) 0.0608(19) Uani 1 1 d . . . O11 O 0.7375(3) 0.5850(3) 0.7155(2) 0.0449(15) Uani 1 1 d . . . O12 O 0.8538(3) 0.6238(3) 0.6629(3) 0.0502(17) Uani 1 1 d . B . O13 O 0.7339(3) 0.6499(3) 0.5636(2) 0.0456(15) Uani 1 1 d . A . O14 O 0.7281(5) 0.4733(3) 0.5355(4) 0.079(2) Uani 1 1 d . B . H14 H 0.7346 0.4422 0.5264 0.100 Uiso 1 1 calc . . . O15 O 0.6615(3) 0.5809(3) 0.7553(3) 0.0530(17) Uani 1 1 d . . . O16 O 0.7645(4) 0.7366(3) 0.7560(3) 0.0540(17) Uani 1 1 d . B . O17 O 0.8651(3) 0.7392(3) 0.6856(3) 0.0572(19) Uani 1 1 d . B . O18 O 0.7471(3) 0.7584(2) 0.5860(2) 0.0423(14) Uani 1 1 d . A . O19 O 0.8636(7) 0.9059(6) 0.6373(6) 0.110(5) Uani 0.70 1 d PU B 1 H19 H 0.8985 0.8877 0.6530 0.100 Uiso 0.70 1 calc P F 1 O19' O 0.8821(11) 0.9071(9) 0.7080(8) 0.053(5) Uani 0.30 1 d PU B 2 H19' H 0.8725 0.9133 0.7304 0.100 Uiso 0.30 1 calc P G 2 O20 O 0.7197(4) 0.7219(3) 0.8185(3) 0.0571(18) Uani 1 1 d . . . O21 O 0.4054(3) 0.8110(3) 0.2292(2) 0.0457(15) Uani 1 1 d . . . O22 O 0.5092(3) 0.7818(3) 0.2900(2) 0.0464(15) Uani 1 1 d . . . O23 O 0.5274(4) 0.6766(3) 0.3431(3) 0.0530(17) Uani 1 1 d . . . O24 O 0.6212(3) 0.7078(3) 0.4111(2) 0.0460(15) Uani 1 1 d . . . O25 O 0.5015(3) 0.7030(2) 0.4244(2) 0.0466(15) Uani 1 1 d . . . O26 O 0.5938(4) 0.6575(3) 0.4850(2) 0.0532(17) Uani 1 1 d . . . O27 O 0.5308(3) 0.8185(2) 0.4458(2) 0.0416(14) Uani 1 1 d . . . O28 O 0.6048(3) 0.7727(3) 0.5195(2) 0.0459(15) Uani 1 1 d . . . O29 O 0.6008(3) 0.8340(2) 0.3930(2) 0.0448(15) Uani 1 1 d . . . O30 O 0.6840(3) 0.8094(3) 0.4735(2) 0.0457(15) Uani 1 1 d . . . O31 O 0.7774(4) 0.7115(3) 0.5046(3) 0.067(2) Uani 1 1 d D . . O32 O 0.8576(3) 0.7010(3) 0.5880(3) 0.070(2) Uani 1 1 d D A . O33 O 0.3133(3) 0.8350(2) 0.3119(2) 0.0398(14) Uani 1 1 d . . . O34 O 0.7617(3) 0.6801(2) 0.6682(2) 0.0375(13) Uani 1 1 d . B . O35 O 0.2013(3) 0.8734(3) 0.2415(2) 0.0465(15) Uani 1 1 d . . . O36 O 0.8571(3) 0.6557(3) 0.7608(2) 0.0485(16) Uani 1 1 d . B . O37 O 0.0732(4) 0.9135(3) 0.2857(4) 0.080(3) Uani 1 1 d . . . O38 O 0.8347(10) 0.6222(10) 0.8724(7) 0.105(7) Uani 0.50 1 d PDU B 1 O38' O 0.8111(12) 0.5862(10) 0.8564(8) 0.125(8) Uani 0.50 1 d PDU B 2 O39 O -0.0094(4) 0.6604(5) 0.7153(4) 0.111(3) Uani 1 1 d U . . O40 O 0.0109(10) 0.8905(8) 0.7178(9) 0.144(7) Uani 0.65 1 d PU . . O41 O 0.4284(4) 0.9056(3) 0.7014(4) 0.086(3) Uani 1 1 d . . . O42 O 0.1301(19) 0.5739(16) 0.4904(15) 0.139(11) Uani 0.35 1 d PU . . C1 C 0.1957(5) 0.7442(4) 0.3362(4) 0.051(2) Uani 1 1 d . . . C2 C 0.2247(5) 0.6906(4) 0.3405(4) 0.053(3) Uani 1 1 d . . . C3 C 0.2211(6) 0.6490(4) 0.3712(5) 0.063(3) Uani 1 1 d . . . H3 H 0.2399 0.6135 0.3731 0.100 Uiso 1 1 calc . . . C4 C 0.1911(7) 0.6578(5) 0.3988(6) 0.083(4) Uani 1 1 d . . . H4A H 0.1903 0.6288 0.4199 0.100 Uiso 1 1 calc . . . C5 C 0.1607(7) 0.7110(5) 0.3961(5) 0.075(4) Uani 1 1 d . . . H5 H 0.1396 0.7178 0.4147 0.100 Uiso 1 1 calc . . . C6 C 0.1640(6) 0.7526(4) 0.3640(5) 0.059(3) Uani 1 1 d . . . C7 C 0.2602(5) 0.6757(4) 0.3138(4) 0.051(2) Uani 1 1 d . . . H7 H 0.2803 0.6400 0.3211 0.100 Uiso 1 1 calc . . . C8 C 0.3054(5) 0.6870(4) 0.2585(4) 0.053(3) Uani 1 1 d . C . C9 C 0.2849(5) 0.7251(4) 0.2101(4) 0.052(3) Uani 1 1 d . . . H9A H 0.3175 0.7220 0.1997 0.100 Uiso 1 1 calc . . . H9B H 0.2421 0.7128 0.1805 0.100 Uiso 1 1 calc . . . C10 C 0.3808(5) 0.6906(4) 0.2989(4) 0.045(2) Uani 1 1 d . . . H10A H 0.3912 0.6693 0.3304 0.100 Uiso 1 1 calc . . . H10B H 0.4043 0.6728 0.2839 0.100 Uiso 1 1 calc . . . C11 C 0.2880(5) 0.6240(4) 0.2389(4) 0.054(3) Uani 1 1 d . . . H11A H 0.3088 0.5984 0.2692 0.100 Uiso 1 1 calc . H 1 H11B H 0.2401 0.6185 0.2206 0.100 Uiso 1 1 calc . I 1 C12 C 0.0986(6) 0.8173(5) 0.3811(6) 0.077(4) Uani 1 1 d . . . H12A H 0.0818 0.8556 0.3735 0.100 Uiso 1 1 calc . . . H12B H 0.1273 0.8125 0.4187 0.100 Uiso 1 1 calc . . . H12C H 0.0620 0.7910 0.3679 0.100 Uiso 1 1 calc . . . C13 C 0.3004(4) 0.9699(4) 0.3825(4) 0.043(2) Uani 1 1 d . A . C14 C 0.3630(5) 0.9949(4) 0.3995(4) 0.050(2) Uani 1 1 d . . . C15 C 0.3924(5) 1.0287(4) 0.4457(5) 0.058(3) Uani 1 1 d . A . H15 H 0.4344 1.0442 0.4581 0.100 Uiso 1 1 calc . . . C16 C 0.3620(5) 1.0394(5) 0.4727(4) 0.059(3) Uani 1 1 d . . . H16 H 0.3827 1.0622 0.5029 0.100 Uiso 1 1 calc . . . C17 C 0.2979(5) 1.0155(4) 0.4546(4) 0.055(3) Uani 1 1 d . A . H17 H 0.2759 1.0229 0.4724 0.100 Uiso 1 1 calc . . . C18 C 0.2694(5) 0.9814(4) 0.4103(4) 0.047(2) Uani 1 1 d . A . C19 C 0.4009(5) 0.9857(4) 0.3745(4) 0.049(2) Uani 1 1 d . A . H19A H 0.4435 1.0013 0.3909 0.100 Uiso 1 1 calc . . . C20 C 0.4256(4) 0.9518(4) 0.3115(4) 0.041(2) Uani 1 1 d . . . C21 C 0.3790(5) 0.9379(4) 0.2521(4) 0.046(2) Uani 1 1 d . A . H21A H 0.3564 0.9722 0.2328 0.100 Uiso 1 1 calc . . . H21B H 0.4049 0.9232 0.2378 0.100 Uiso 1 1 calc . . . C22 C 0.4764(4) 0.9042(3) 0.3409(4) 0.042(2) Uani 1 1 d . A . H22A H 0.5073 0.9033 0.3286 0.100 Uiso 1 1 calc . . . H22B H 0.5018 0.9134 0.3784 0.100 Uiso 1 1 calc . . . C23 C 0.4654(5) 1.0064(4) 0.3170(4) 0.050(2) Uani 1 1 d . A . H23A H 0.4360 1.0393 0.3049 0.100 Uiso 1 1 calc . . . H23B H 0.4999 1.0124 0.3539 0.100 Uiso 1 1 calc . . . C24 C 0.1736(6) 0.9651(5) 0.4165(5) 0.076(4) Uani 1 1 d . A . H24A H 0.1320 0.9449 0.3984 0.100 Uiso 1 1 calc . . . H24B H 0.1653 1.0051 0.4166 0.100 Uiso 1 1 calc . . . H24C H 0.2001 0.9516 0.4523 0.100 Uiso 1 1 calc . . . C25 C 0.6871(4) 0.5481(4) 0.6931(4) 0.039(2) Uani 1 1 d . B . C26 C 0.6708(4) 0.5143(4) 0.6488(4) 0.041(2) Uani 1 1 d . . . C27 C 0.6195(5) 0.4745(4) 0.6300(4) 0.053(2) Uani 1 1 d . B . H27 H 0.6104 0.4515 0.6014 0.100 Uiso 1 1 calc . . . C28 C 0.5820(5) 0.4687(4) 0.6530(4) 0.054(3) Uani 1 1 d . . . H28 H 0.5487 0.4411 0.6406 0.100 Uiso 1 1 calc . . . C29 C 0.5942(5) 0.5044(4) 0.6954(4) 0.048(2) Uani 1 1 d . B . H29 H 0.5679 0.5021 0.7103 0.100 Uiso 1 1 calc . . . C30 C 0.6461(5) 0.5431(4) 0.7145(3) 0.040(2) Uani 1 1 d . B . C31 C 0.7052(5) 0.5194(4) 0.6196(4) 0.045(2) Uani 1 1 d . B . H31 H 0.6897 0.4970 0.5895 0.100 Uiso 1 1 calc . . . C32 C 0.7819(5) 0.5535(4) 0.5970(4) 0.055(3) Uani 1 1 d . B . C33 C 0.8541(5) 0.5768(4) 0.6317(4) 0.056(3) Uani 1 1 d . . . H33A H 0.8835 0.5469 0.6549 0.100 Uiso 1 1 calc . . . H33B H 0.8703 0.5894 0.6093 0.100 Uiso 1 1 calc . . . C34 C 0.7385(5) 0.5930(4) 0.5489(4) 0.052(3) Uani 1 1 d . . . H34A H 0.7573 0.5940 0.5266 0.100 Uiso 1 1 calc . . . H34B H 0.6940 0.5771 0.5282 0.100 Uiso 1 1 calc . . . C35 C 0.7891(7) 0.4953(4) 0.5773(5) 0.065(3) Uani 1 1 d . . . H35A H 0.8202 0.4985 0.5654 0.100 Uiso 1 1 calc . . . H35B H 0.8077 0.4685 0.6067 0.100 Uiso 1 1 calc . . . C36 C 0.6184(7) 0.5807(5) 0.7760(5) 0.080(4) Uani 1 1 d . B . H36A H 0.6342 0.6079 0.8043 0.100 Uiso 1 1 calc . . . H36B H 0.6182 0.5434 0.7892 0.100 Uiso 1 1 calc . . . H36C H 0.5739 0.5906 0.7483 0.100 Uiso 1 1 calc . . . C37 C 0.7326(5) 0.7801(4) 0.7602(4) 0.050(2) Uani 1 1 d . . . C38 C 0.7206(5) 0.8320(4) 0.7318(4) 0.052(3) Uani 1 1 d . B . C39 C 0.6840(6) 0.8748(5) 0.7389(5) 0.071(3) Uani 1 1 d . . . H39 H 0.6747 0.9084 0.7196 0.100 Uiso 1 1 calc . . . C40 C 0.6620(6) 0.8695(5) 0.7720(5) 0.067(3) Uani 1 1 d . B . H40 H 0.6392 0.8993 0.7763 0.100 Uiso 1 1 calc . . . C41 C 0.6737(6) 0.8180(5) 0.8006(4) 0.063(3) Uani 1 1 d . . . H41 H 0.6589 0.8137 0.8239 0.100 Uiso 1 1 calc . . . C42 C 0.7068(5) 0.7750(4) 0.7935(4) 0.052(2) Uani 1 1 d . B . C43 C 0.7451(5) 0.8426(4) 0.6970(4) 0.057(3) Uani 1 1 d . . . H43 H 0.7299 0.8757 0.6766 0.100 Uiso 1 1 calc . . . C44 C 0.8088(5) 0.8305(4) 0.6561(4) 0.051(3) Uani 1 1 d . . . C45 C 0.8732(5) 0.7963(4) 0.6736(4) 0.059(3) Uani 1 1 d . B . H45A H 0.8826 0.7964 0.6454 0.100 Uiso 1 1 calc . . . H45B H 0.9104 0.8139 0.7046 0.100 Uiso 1 1 calc . . . C46 C 0.7555(5) 0.8165(4) 0.5979(4) 0.049(2) Uani 1 1 d . A . H46A H 0.7132 0.8323 0.5901 0.100 Uiso 1 1 calc . . . H46B H 0.7676 0.8353 0.5750 0.100 Uiso 1 1 calc . . . C47 C 0.8248(6) 0.8941(5) 0.6601(5) 0.071(3) Uani 1 1 d U B . H47A H 0.7837 0.9158 0.6418 0.100 Uiso 1 1 calc . J 1 H47B H 0.8491 0.9057 0.6971 0.100 Uiso 1 1 calc . K 1 C48 C 0.7014(7) 0.7146(4) 0.8572(5) 0.069(3) Uani 1 1 d . B . H48A H 0.7124 0.6767 0.8713 0.100 Uiso 1 1 calc . . . H48B H 0.6544 0.7208 0.8409 0.100 Uiso 1 1 calc . . . H48C H 0.7253 0.7417 0.8853 0.100 Uiso 1 1 calc . . . C49 C 0.4846(5) 0.8054(4) 0.2040(3) 0.046(2) Uani 1 1 d . . . C50 C 0.4445(7) 0.8371(6) 0.1590(5) 0.087(4) Uani 1 1 d . A . H50 H 0.4050 0.8534 0.1528 0.100 Uiso 1 1 calc . . . C51 C 0.4655(8) 0.8438(7) 0.1229(7) 0.108(5) Uani 1 1 d U . . H51 H 0.4399 0.8654 0.0924 0.100 Uiso 1 1 calc . . . C52 C 0.5230(8) 0.8189(7) 0.1318(6) 0.099(4) Uani 1 1 d U A . H52 H 0.5354 0.8230 0.1069 0.100 Uiso 1 1 calc . . . C53 C 0.5612(6) 0.7888(5) 0.1755(5) 0.070(3) Uani 1 1 d . . . H53 H 0.6004 0.7724 0.1815 0.100 Uiso 1 1 calc . . . C54 C 0.5424(5) 0.7822(4) 0.2122(4) 0.052(2) Uani 1 1 d . A . H54 H 0.5696 0.7615 0.2430 0.100 Uiso 1 1 calc . . . C55 C 0.4668(5) 0.7982(4) 0.2448(4) 0.043(2) Uani 1 1 d . A . C56 C 0.6177(6) 0.6117(4) 0.3804(4) 0.053(3) Uani 1 1 d . . . C57 C 0.5770(7) 0.5689(4) 0.3473(4) 0.066(3) Uani 1 1 d . A . H57 H 0.5317 0.5755 0.3242 0.100 Uiso 1 1 calc . . . C58 C 0.6038(7) 0.5158(6) 0.3485(6) 0.085(4) Uani 1 1 d U . . H58 H 0.5769 0.4863 0.3268 0.100 Uiso 1 1 calc . . . C59 C 0.6693(8) 0.5082(6) 0.3817(6) 0.089(4) Uani 1 1 d U A . H59 H 0.6872 0.4726 0.3824 0.100 Uiso 1 1 calc . . . C60 C 0.7115(8) 0.5498(6) 0.4146(5) 0.091(4) Uani 1 1 d . . . H60 H 0.7567 0.5424 0.4372 0.100 Uiso 1 1 calc . . . C61 C 0.6855(6) 0.6035(5) 0.4136(4) 0.066(3) Uani 1 1 d . A . H61 H 0.7131 0.6329 0.4348 0.100 Uiso 1 1 calc . . . C62 C 0.5870(6) 0.6687(4) 0.3779(4) 0.050(3) Uani 1 1 d . A . C63 C 0.4920(5) 0.6347(4) 0.4780(3) 0.043(2) Uani 1 1 d . . . C64 C 0.4270(6) 0.6488(4) 0.4607(4) 0.055(3) Uani 1 1 d . A . H64 H 0.4072 0.6794 0.4376 0.100 Uiso 1 1 calc . . . C65 C 0.3900(5) 0.6180(4) 0.4770(4) 0.053(3) Uani 1 1 d . . . H65 H 0.3462 0.6283 0.4650 0.100 Uiso 1 1 calc . . . C66 C 0.4189(7) 0.5723(5) 0.5111(4) 0.061(3) Uani 1 1 d . A . H66 H 0.3946 0.5510 0.5218 0.100 Uiso 1 1 calc . . . C67 C 0.4831(7) 0.5591(4) 0.5286(4) 0.066(3) Uani 1 1 d . . . H67 H 0.5025 0.5283 0.5515 0.100 Uiso 1 1 calc . . . C68 C 0.5209(6) 0.5892(4) 0.5140(4) 0.061(3) Uani 1 1 d . A . H68 H 0.5653 0.5796 0.5278 0.100 Uiso 1 1 calc . . . C69 C 0.5314(5) 0.6678(4) 0.4603(3) 0.046(2) Uani 1 1 d . A . C70 C 0.5259(4) 0.8339(3) 0.5225(3) 0.038(2) Uani 1 1 d . . . C71 C 0.4728(4) 0.8702(4) 0.4971(3) 0.038(2) Uani 1 1 d . A . H71 H 0.4558 0.8789 0.4616 0.100 Uiso 1 1 calc . . . C72 C 0.4438(5) 0.8941(4) 0.5222(4) 0.052(3) Uani 1 1 d . . . H72 H 0.4079 0.9188 0.5040 0.100 Uiso 1 1 calc . . . C73 C 0.4684(5) 0.8812(5) 0.5754(5) 0.058(3) Uani 1 1 d . A . H73 H 0.4486 0.8965 0.5928 0.100 Uiso 1 1 calc . . . C74 C 0.5226(6) 0.8454(5) 0.6017(4) 0.069(3) Uani 1 1 d . . . H74 H 0.5398 0.8371 0.6373 0.100 Uiso 1 1 calc . . . C75 C 0.5525(5) 0.8211(4) 0.5757(4) 0.049(2) Uani 1 1 d . A . H75 H 0.5892 0.7971 0.5937 0.100 Uiso 1 1 calc . . . C76 C 0.5553(4) 0.8065(4) 0.4931(3) 0.040(2) Uani 1 1 d . A . C77 C 0.6948(5) 0.8955(4) 0.4382(3) 0.042(2) Uani 1 1 d . . . C78 C 0.6611(5) 0.9426(4) 0.4066(4) 0.053(3) Uani 1 1 d . A . H78 H 0.6151 0.9419 0.3833 0.100 Uiso 1 1 calc . . . C79 C 0.6983(7) 0.9907(5) 0.4112(5) 0.080(4) Uani 1 1 d . . . H79 H 0.6762 1.0225 0.3906 0.100 Uiso 1 1 calc . . . C80 C 0.7647(7) 0.9932(5) 0.4439(5) 0.075(3) Uani 1 1 d . A . H80 H 0.7881 1.0260 0.4458 0.100 Uiso 1 1 calc . . . C81 C 0.7979(6) 0.9458(6) 0.4748(5) 0.076(3) Uani 1 1 d . . . H81 H 0.8439 0.9470 0.4975 0.100 Uiso 1 1 calc . . . C82 C 0.7635(5) 0.8973(4) 0.4724(4) 0.056(3) Uani 1 1 d . A . H82 H 0.7862 0.8660 0.4935 0.100 Uiso 1 1 calc . . . C83 C 0.6570(5) 0.8432(4) 0.4348(4) 0.042(2) Uani 1 1 d . A . C84 C 0.8954(6) 0.7191(8) 0.5314(6) 0.102(4) Uani 0.65 1 d PGU A 1 C85 C 0.8772(5) 0.7228(8) 0.4786(5) 0.106(4) Uani 0.65 1 d PGU A 1 H85 H 0.8323 0.7231 0.4519 0.100 Uiso 0.65 1 calc P L 1 C86 C 0.9259(7) 0.7263(8) 0.4657(5) 0.110(4) Uani 0.65 1 d PGU A 1 H86 H 0.9137 0.7288 0.4304 0.100 Uiso 0.65 1 calc P M 1 C87 C 0.9929(6) 0.7260(8) 0.5056(6) 0.111(4) Uani 0.65 1 d PGU A 1 H87 H 1.0255 0.7283 0.4970 0.100 Uiso 0.65 1 calc P N 1 C88 C 1.0112(5) 0.7222(8) 0.5584(5) 0.109(4) Uani 0.65 1 d PGU A 1 H88 H 1.0560 0.7220 0.5851 0.100 Uiso 0.65 1 calc P O 1 C89 C 0.9624(7) 0.7188(8) 0.5713(5) 0.101(4) Uani 0.65 1 d PGU A 1 H89 H 0.9746 0.7162 0.6066 0.100 Uiso 0.65 1 calc P P 1 C84' C 0.8670(12) 0.6698(14) 0.5115(10) 0.101(6) Uani 0.35 1 d PGDU A 2 C85' C 0.8407(10) 0.6632(14) 0.4574(9) 0.103(6) Uani 0.35 1 d PGU A 2 H85' H 0.7968 0.6737 0.4332 0.100 Uiso 0.35 1 calc P Q 2 C86' C 0.8800(12) 0.6410(14) 0.4394(8) 0.103(6) Uani 0.35 1 d PGU A 2 H86' H 0.8624 0.6366 0.4032 0.100 Uiso 0.35 1 calc P R 2 C87' C 0.9456(12) 0.6254(14) 0.4755(10) 0.104(6) Uani 0.35 1 d PGU A 2 H87' H 0.9719 0.6105 0.4634 0.100 Uiso 0.35 1 calc P S 2 C88' C 0.9719(10) 0.6320(14) 0.5295(9) 0.105(7) Uani 0.35 1 d PGU A 2 H88' H 1.0158 0.6215 0.5537 0.100 Uiso 0.35 1 calc P T 2 C89' C 0.9326(12) 0.6542(14) 0.5475(8) 0.102(6) Uani 0.35 1 d PGU A 2 H89' H 0.9502 0.6586 0.5837 0.100 Uiso 0.35 1 calc P U 2 C90 C 0.8441(10) 0.7122(8) 0.5465(9) 0.057(5) Uani 0.65 1 d PU A 1 C90' C 0.8269(9) 0.6937(8) 0.5310(5) 0.032(7) Uani 0.35 1 d PDU A 2 C91 C 0.3459(5) 0.8212(4) 0.3675(3) 0.042(2) Uani 1 1 d . A . H91A H 0.3168 0.8302 0.3801 0.100 Uiso 1 1 calc . . . H91B H 0.3862 0.8430 0.3869 0.100 Uiso 1 1 calc . . . H91C H 0.3563 0.7813 0.3724 0.100 Uiso 1 1 calc . . . C92 C 0.6897(4) 0.6857(4) 0.6412(3) 0.040(2) Uani 1 1 d . . . H92A H 0.6757 0.6781 0.6657 0.100 Uiso 1 1 calc . . . H92B H 0.6690 0.6590 0.6124 0.100 Uiso 1 1 calc . . . H92C H 0.6770 0.7238 0.6277 0.100 Uiso 1 1 calc . . . C93 C 0.1401(6) 0.8945(5) 0.1982(5) 0.076(4) Uani 1 1 d . A . H93A H 0.1398 0.9353 0.1996 0.100 Uiso 1 1 calc . . . H93B H 0.1036 0.8796 0.2003 0.100 Uiso 1 1 calc . . . H93C H 0.1356 0.8826 0.1654 0.100 Uiso 1 1 calc . . . C94 C 0.9234(6) 0.6434(5) 0.8055(5) 0.074(3) Uani 1 1 d . . . H94A H 0.9390 0.6750 0.8297 0.100 Uiso 1 1 calc . . . H94B H 0.9532 0.6374 0.7930 0.100 Uiso 1 1 calc . . . H94C H 0.9221 0.6097 0.8233 0.100 Uiso 1 1 calc . . . C95 C 0.0487(9) 0.9684(8) 0.2707(7) 0.119(5) Uani 1 1 d U A . H95A H 0.0009 0.9677 0.2525 0.100 Uiso 1 1 calc . . . H95B H 0.0620 0.9835 0.2476 0.100 Uiso 1 1 calc . . . H95C H 0.0661 0.9920 0.3017 0.100 Uiso 1 1 calc . . . C96 C 0.8839(17) 0.6453(17) 0.9211(13) 0.141(13) Uani 0.50 1 d PDU B 1 H96A H 0.9035 0.6154 0.9471 0.100 Uiso 0.50 1 calc P V 1 H96B H 0.8642 0.6732 0.9325 0.100 Uiso 0.50 1 calc P W 1 H96C H 0.9178 0.6630 0.9172 0.100 Uiso 0.50 1 calc P X 1 C96' C 0.8102(17) 0.5260(12) 0.8464(14) 0.117(11) Uani 0.50 1 d PDU B 2 H96D H 0.8398 0.5065 0.8790 0.100 Uiso 0.50 1 calc P Y 2 H96E H 0.8243 0.5197 0.8217 0.100 Uiso 0.50 1 calc P Z 2 H96F H 0.7657 0.5116 0.8317 0.100 Uiso 0.50 1 calc P A 2 C97 C 0.0140(7) 0.7177(7) 0.7252(7) 0.099(5) Uani 1 1 d U . . C98 C 0.0410(12) 0.8868(10) 0.7780(10) 0.105(7) Uani 0.65 1 d PU . . C99 C 0.4596(6) 0.8520(4) 0.7082(5) 0.067(3) Uani 1 1 d . . . C100 C 0.3029(11) 0.6938(10) 0.9733(9) 0.141(4) Uani 1 1 d U . . C101 C 0.3470(11) 0.7393(9) 0.9984(9) 0.141(4) Uani 1 1 d U . . C102 C 0.2385(16) 0.8630(14) 0.5984(17) 0.125(7) Uani 0.40 1 d PDU . . C103 C 0.1807(16) 0.8857(15) 0.6007(17) 0.125(7) Uani 0.40 1 d PDU . . C104 C 0.2627(16) 0.6328(14) 0.5753(11) 0.130(5) Uani 0.60 1 d PDU . . C105 C 0.2465(15) 0.6493(14) 0.6149(11) 0.130(5) Uani 0.60 1 d PDU . . C106 C 0.070(2) 0.597(2) 0.476(2) 0.113(15) Uani 0.35 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0484(3) 0.0317(2) 0.0276(2) 0.00331(17) 0.01666(19) 0.00568(19) Dy2 0.0504(3) 0.0420(2) 0.0352(2) 0.01127(19) 0.0243(2) 0.0156(2) Fe1 0.0423(7) 0.0360(7) 0.0405(7) 0.0007(6) 0.0134(6) -0.0042(6) Fe2 0.0381(7) 0.0327(7) 0.0426(7) 0.0045(6) 0.0112(6) -0.0009(6) Fe3 0.0431(7) 0.0350(7) 0.0298(6) 0.0016(5) 0.0138(6) -0.0012(6) Fe4 0.0347(7) 0.0451(7) 0.0459(8) 0.0179(6) 0.0195(6) 0.0059(6) Fe5 0.0461(8) 0.0460(8) 0.0366(7) 0.0124(6) 0.0070(6) -0.0100(7) Fe6 0.0356(7) 0.0504(8) 0.0524(8) 0.0244(7) 0.0244(6) 0.0123(6) Na1 0.047(2) 0.046(2) 0.104(3) -0.015(2) 0.038(2) -0.0069(19) Na2 0.073(3) 0.048(2) 0.050(2) 0.0068(18) 0.033(2) -0.001(2) N1 0.040(4) 0.033(4) 0.050(5) -0.005(4) 0.018(4) -0.002(3) N2 0.043(4) 0.030(4) 0.047(5) 0.004(3) 0.023(4) 0.003(3) N3 0.049(5) 0.048(4) 0.046(4) 0.023(4) 0.034(4) 0.024(4) N4 0.046(5) 0.046(5) 0.039(4) -0.002(4) 0.013(4) -0.018(4) N5 0.080(5) 0.067(5) 0.096(5) 0.000(4) 0.051(4) -0.016(4) N6 0.112(3) 0.112(3) 0.112(3) 0.0003(10) 0.0583(19) -0.0004(10) N7 0.125(4) 0.124(4) 0.125(4) 0.0003(10) 0.065(2) -0.0008(10) N8 0.041(5) 0.049(5) 0.089(8) 0.025(5) 0.011(5) 0.002(5) N9 0.054(8) 0.052(8) 0.075(10) -0.004(7) 0.016(8) 0.000(7) N10 0.087(5) 0.087(5) 0.087(5) -0.0001(10) 0.046(3) 0.0001(10) N9' 0.057(7) 0.057(7) 0.057(7) 0.0001(10) 0.030(4) -0.0001(10) N10' 0.131(14) 0.131(14) 0.131(14) 0.0001(10) 0.069(8) 0.0000(10) N11 0.041(5) 0.061(6) 0.077(6) 0.038(5) 0.024(5) 0.018(4) N12 0.054(5) 0.050(5) 0.101(8) 0.037(5) 0.045(5) 0.016(5) N13 0.089(3) 0.088(3) 0.089(3) 0.0011(10) 0.0462(19) -0.0001(10) N14 0.061(6) 0.070(7) 0.054(6) 0.005(5) 0.029(5) -0.008(6) N16 0.108(8) 0.123(8) 0.080(7) -0.007(7) 0.044(6) -0.010(7) N14' 0.079(7) 0.079(7) 0.079(7) 0.0004(10) 0.042(3) -0.0002(10) N16' 0.083(10) 0.099(11) 0.111(11) 0.002(9) 0.033(10) -0.002(9) N15 0.094(7) 0.112(7) 0.086(7) -0.024(6) 0.051(6) -0.028(6) N17 0.134(6) 0.128(6) 0.152(6) -0.007(5) 0.068(4) -0.003(4) N18 0.094(11) 0.106(12) 0.165(13) 0.109(11) 0.061(11) 0.031(10) N19 0.134(8) 0.139(8) 0.105(8) -0.025(7) 0.056(6) 0.026(7) O1 0.046(4) 0.039(3) 0.053(4) 0.007(3) 0.027(3) 0.004(3) O2 0.042(3) 0.041(3) 0.035(3) -0.006(3) 0.013(3) -0.009(3) O3 0.056(4) 0.031(3) 0.031(3) -0.004(2) 0.019(3) -0.004(3) O4 0.055(6) 0.041(5) 0.076(7) -0.026(5) 0.041(5) -0.017(5) O4' 0.067(16) 0.070(16) 0.060(16) -0.029(13) 0.020(13) -0.021(14) O5 0.067(5) 0.050(4) 0.081(5) 0.012(4) 0.043(4) 0.011(4) O6 0.039(3) 0.033(3) 0.053(4) -0.003(3) 0.017(3) -0.001(3) O7 0.044(4) 0.043(3) 0.034(3) 0.006(3) 0.011(3) -0.006(3) O8 0.047(4) 0.042(3) 0.028(3) -0.002(3) 0.015(3) -0.002(3) O9 0.059(4) 0.044(4) 0.082(5) 0.005(4) 0.038(4) -0.008(3) O10 0.044(4) 0.062(4) 0.071(5) -0.011(4) 0.026(4) -0.003(4) O11 0.049(4) 0.048(4) 0.041(4) 0.001(3) 0.026(3) -0.008(3) O12 0.037(3) 0.054(4) 0.061(4) 0.026(3) 0.026(3) 0.014(3) O13 0.048(4) 0.046(4) 0.052(4) 0.011(3) 0.032(3) 0.020(3) O14 0.109(7) 0.056(5) 0.091(6) 0.003(4) 0.065(6) 0.025(5) O15 0.066(4) 0.059(4) 0.054(4) -0.005(3) 0.046(4) -0.011(4) O16 0.083(5) 0.036(3) 0.045(4) 0.006(3) 0.035(4) 0.005(3) O17 0.039(4) 0.063(4) 0.056(4) 0.027(3) 0.016(3) -0.001(3) O18 0.048(4) 0.038(3) 0.042(3) 0.017(3) 0.025(3) 0.018(3) O19 0.110(5) 0.110(5) 0.110(5) 0.0003(10) 0.058(3) -0.0002(10) O19' 0.052(9) 0.045(9) 0.050(9) -0.002(7) 0.019(7) -0.017(7) O20 0.088(5) 0.044(4) 0.049(4) -0.002(3) 0.042(4) -0.006(4) O21 0.059(4) 0.046(4) 0.028(3) 0.002(3) 0.020(3) 0.002(3) O22 0.052(4) 0.045(4) 0.035(4) 0.001(3) 0.018(3) 0.004(3) O23 0.071(5) 0.037(4) 0.042(4) -0.004(3) 0.024(4) 0.008(4) O24 0.061(4) 0.046(4) 0.042(4) 0.004(3) 0.034(3) 0.007(3) O25 0.060(4) 0.036(3) 0.035(3) 0.010(3) 0.019(3) 0.006(3) O26 0.066(5) 0.047(4) 0.038(4) 0.007(3) 0.022(4) 0.014(4) O27 0.047(4) 0.042(3) 0.028(3) -0.002(3) 0.015(3) 0.006(3) O28 0.049(4) 0.046(4) 0.040(4) -0.003(3) 0.022(3) 0.002(3) O29 0.060(4) 0.038(3) 0.034(3) 0.004(3) 0.023(3) 0.011(3) O30 0.053(4) 0.043(3) 0.037(3) 0.012(3) 0.021(3) 0.018(3) O31 0.077(5) 0.083(5) 0.067(5) 0.042(4) 0.055(5) 0.037(4) O32 0.054(4) 0.090(6) 0.088(6) 0.056(5) 0.053(4) 0.039(4) O33 0.041(3) 0.031(3) 0.039(3) 0.003(3) 0.016(3) -0.001(3) O34 0.030(3) 0.039(3) 0.041(3) 0.008(3) 0.017(3) 0.006(3) O35 0.037(3) 0.043(3) 0.041(4) 0.009(3) 0.008(3) -0.001(3) O36 0.036(3) 0.053(4) 0.040(4) 0.014(3) 0.008(3) 0.003(3) O37 0.052(4) 0.046(4) 0.119(7) 0.009(4) 0.030(5) 0.002(4) O38 0.116(10) 0.110(10) 0.091(10) 0.014(8) 0.056(8) 0.010(8) O38' 0.131(11) 0.116(11) 0.117(11) 0.006(8) 0.058(8) -0.001(9) O39 0.062(5) 0.120(7) 0.125(7) 0.026(6) 0.031(5) 0.020(5) O40 0.140(10) 0.131(10) 0.160(11) 0.001(8) 0.079(8) -0.012(8) O41 0.068(5) 0.055(5) 0.143(8) 0.015(5) 0.061(6) 0.002(4) O42 0.139(11) 0.139(11) 0.139(11) -0.0001(10) 0.073(6) 0.0000(10) C1 0.046(6) 0.042(5) 0.057(6) 0.009(5) 0.022(5) 0.003(5) C2 0.060(6) 0.040(5) 0.055(6) 0.008(5) 0.027(5) 0.004(5) C3 0.073(7) 0.042(6) 0.091(9) 0.012(6) 0.054(7) 0.012(5) C4 0.101(10) 0.052(7) 0.116(11) 0.032(7) 0.071(9) 0.022(7) C5 0.102(10) 0.054(7) 0.095(9) 0.022(6) 0.069(9) 0.013(7) C6 0.068(7) 0.043(5) 0.071(7) 0.016(5) 0.040(6) 0.020(5) C7 0.053(6) 0.031(5) 0.066(7) 0.000(5) 0.028(5) -0.001(5) C8 0.054(6) 0.038(5) 0.056(6) -0.006(5) 0.021(5) 0.003(5) C9 0.065(7) 0.040(5) 0.048(6) -0.017(4) 0.027(5) -0.013(5) C10 0.050(5) 0.028(4) 0.043(5) -0.007(4) 0.015(4) -0.010(4) C11 0.052(6) 0.043(5) 0.073(7) -0.010(5) 0.037(6) -0.003(5) C12 0.073(8) 0.066(7) 0.115(11) 0.001(7) 0.064(8) 0.010(6) C13 0.042(5) 0.030(4) 0.042(5) 0.002(4) 0.011(4) 0.011(4) C14 0.045(5) 0.033(5) 0.063(6) -0.010(5) 0.021(5) -0.009(4) C15 0.044(6) 0.045(6) 0.080(8) -0.013(5) 0.029(6) -0.010(5) C16 0.053(6) 0.062(7) 0.062(7) -0.015(6) 0.030(6) -0.008(5) C17 0.058(6) 0.046(6) 0.059(7) -0.004(5) 0.031(5) 0.003(5) C18 0.044(6) 0.034(5) 0.057(6) 0.005(4) 0.023(5) 0.005(4) C19 0.041(5) 0.039(5) 0.059(6) 0.002(5) 0.019(5) 0.000(4) C20 0.037(5) 0.034(5) 0.049(6) 0.004(4) 0.020(4) 0.001(4) C21 0.049(5) 0.035(5) 0.047(6) 0.012(4) 0.020(5) 0.000(4) C22 0.046(5) 0.020(4) 0.053(6) 0.005(4) 0.022(5) -0.003(4) C23 0.054(6) 0.031(5) 0.068(7) 0.008(5) 0.034(5) 0.003(4) C24 0.069(8) 0.073(8) 0.109(10) -0.030(7) 0.063(8) -0.013(6) C25 0.041(5) 0.035(5) 0.045(5) 0.010(4) 0.025(4) 0.001(4) C26 0.045(5) 0.037(5) 0.048(5) 0.011(4) 0.028(5) 0.003(4) C27 0.071(7) 0.042(5) 0.053(6) -0.001(5) 0.038(6) -0.005(5) C28 0.059(6) 0.053(6) 0.057(6) -0.001(5) 0.034(5) -0.013(5) C29 0.055(6) 0.040(5) 0.053(6) 0.006(4) 0.032(5) -0.002(5) C30 0.052(5) 0.038(5) 0.035(5) 0.009(4) 0.026(4) 0.004(4) C31 0.056(6) 0.031(5) 0.057(6) 0.015(4) 0.036(5) 0.012(5) C32 0.055(6) 0.061(6) 0.062(7) 0.020(5) 0.039(6) 0.018(5) C33 0.055(6) 0.051(6) 0.077(7) 0.023(5) 0.046(6) 0.017(5) C34 0.069(7) 0.043(5) 0.049(6) 0.018(5) 0.035(5) 0.024(5) C35 0.089(9) 0.049(6) 0.087(9) 0.023(6) 0.068(8) 0.026(6) C36 0.106(10) 0.081(8) 0.093(9) -0.021(7) 0.081(9) -0.018(8) C37 0.055(6) 0.051(6) 0.033(5) -0.003(4) 0.015(5) -0.008(5) C38 0.051(6) 0.031(5) 0.048(6) -0.004(4) 0.008(5) -0.001(5) C39 0.074(8) 0.044(6) 0.069(8) 0.016(6) 0.019(7) 0.006(6) C40 0.086(9) 0.050(6) 0.083(9) -0.001(6) 0.056(8) 0.008(6) C41 0.071(7) 0.056(7) 0.047(6) -0.019(5) 0.021(6) -0.008(6) C42 0.060(6) 0.050(6) 0.039(5) -0.011(5) 0.021(5) -0.005(5) C43 0.058(7) 0.045(6) 0.037(5) 0.003(5) 0.005(5) -0.027(5) C44 0.046(6) 0.040(5) 0.055(6) 0.017(5) 0.017(5) -0.014(5) C45 0.049(6) 0.052(6) 0.060(7) 0.019(5) 0.018(5) -0.009(5) C46 0.048(6) 0.044(5) 0.043(5) 0.011(4) 0.016(5) -0.007(5) C47 0.071(3) 0.071(3) 0.071(3) 0.0013(10) 0.0371(19) -0.0016(10) C48 0.113(10) 0.049(6) 0.058(7) -0.004(5) 0.055(7) -0.006(6) C49 0.050(6) 0.049(5) 0.028(5) 0.007(4) 0.012(4) -0.002(5) C50 0.099(10) 0.109(10) 0.063(8) 0.038(7) 0.049(8) 0.036(8) C51 0.108(5) 0.108(5) 0.108(5) 0.0011(10) 0.057(3) -0.0001(10) C52 0.099(5) 0.100(5) 0.099(5) 0.0005(10) 0.052(2) -0.0001(10) C53 0.058(7) 0.090(9) 0.059(7) 0.013(6) 0.028(6) -0.005(6) C54 0.050(6) 0.063(6) 0.041(5) 0.007(5) 0.022(5) 0.002(5) C55 0.046(6) 0.031(5) 0.039(5) -0.001(4) 0.013(5) 0.005(4) C56 0.093(8) 0.037(5) 0.045(6) 0.003(4) 0.047(6) 0.016(5) C57 0.115(10) 0.046(6) 0.061(7) 0.008(5) 0.062(7) 0.017(6) C58 0.086(4) 0.085(4) 0.085(4) -0.0001(10) 0.045(2) 0.0003(10) C59 0.123(8) 0.065(6) 0.086(7) -0.005(6) 0.060(6) 0.016(6) C60 0.113(11) 0.092(10) 0.068(8) 0.004(7) 0.046(8) 0.048(9) C61 0.093(9) 0.058(7) 0.059(7) 0.019(5) 0.048(7) 0.043(7) C62 0.094(9) 0.033(5) 0.044(6) -0.001(5) 0.050(6) -0.003(6) C63 0.060(6) 0.033(5) 0.034(5) 0.000(4) 0.023(5) 0.000(4) C64 0.076(7) 0.036(5) 0.051(6) 0.003(4) 0.033(6) 0.007(5) C65 0.063(7) 0.052(6) 0.049(6) -0.002(5) 0.033(5) 0.002(5) C66 0.094(9) 0.056(6) 0.048(6) -0.002(5) 0.048(7) -0.007(6) C67 0.096(9) 0.044(6) 0.055(7) 0.010(5) 0.036(7) -0.004(6) C68 0.082(8) 0.046(6) 0.059(7) 0.013(5) 0.039(6) 0.013(6) C69 0.068(7) 0.036(5) 0.029(5) -0.007(4) 0.023(5) -0.002(5) C70 0.042(5) 0.034(4) 0.029(4) -0.002(4) 0.014(4) -0.001(4) C71 0.030(4) 0.037(5) 0.038(5) -0.009(4) 0.011(4) 0.000(4) C72 0.042(5) 0.039(5) 0.068(7) -0.014(5) 0.024(5) -0.001(4) C73 0.062(7) 0.062(7) 0.067(7) -0.014(6) 0.045(6) 0.003(6) C74 0.086(8) 0.080(8) 0.043(6) 0.002(6) 0.036(6) 0.005(7) C75 0.051(6) 0.056(6) 0.038(5) 0.002(4) 0.022(5) 0.020(5) C76 0.042(5) 0.039(5) 0.034(5) -0.003(4) 0.017(4) -0.004(4) C77 0.054(6) 0.042(5) 0.037(5) -0.005(4) 0.029(5) -0.007(5) C78 0.074(7) 0.031(5) 0.038(5) 0.001(4) 0.019(5) -0.004(5) C79 0.087(9) 0.044(6) 0.078(9) 0.018(6) 0.023(7) -0.004(6) C80 0.080(9) 0.067(8) 0.068(8) -0.008(7) 0.032(7) -0.029(7) C81 0.069(8) 0.093(9) 0.068(8) -0.021(7) 0.038(7) -0.012(7) C82 0.053(6) 0.055(6) 0.052(6) -0.008(5) 0.022(5) 0.004(5) C83 0.055(6) 0.033(5) 0.045(6) 0.005(4) 0.030(5) 0.014(5) C84 0.071(6) 0.158(10) 0.110(9) 0.017(8) 0.071(7) 0.010(7) C85 0.074(6) 0.161(10) 0.113(9) 0.014(8) 0.070(7) 0.010(7) C86 0.078(6) 0.164(10) 0.115(9) 0.015(8) 0.069(7) 0.010(7) C87 0.077(6) 0.163(10) 0.116(9) 0.016(8) 0.067(7) 0.009(7) C88 0.074(6) 0.161(10) 0.116(9) 0.013(8) 0.067(7) 0.011(7) C89 0.070(6) 0.157(10) 0.111(9) 0.015(8) 0.072(7) 0.008(7) C84' 0.090(12) 0.139(15) 0.106(14) -0.022(13) 0.073(12) 0.023(12) C85' 0.092(12) 0.141(15) 0.106(14) -0.021(13) 0.073(12) 0.022(12) C86' 0.092(12) 0.142(15) 0.106(14) -0.022(13) 0.074(12) 0.023(12) C87' 0.092(12) 0.143(15) 0.107(14) -0.021(13) 0.073(12) 0.023(12) C88' 0.091(12) 0.143(15) 0.109(14) -0.022(13) 0.072(12) 0.026(12) C89' 0.090(12) 0.142(15) 0.106(14) -0.021(13) 0.074(12) 0.024(12) C90 0.056(8) 0.059(8) 0.062(9) 0.002(7) 0.036(7) -0.003(7) C90' 0.040(11) 0.037(11) 0.022(10) 0.004(7) 0.019(8) 0.007(8) C91 0.052(6) 0.048(5) 0.027(4) 0.005(4) 0.021(4) 0.002(4) C92 0.025(4) 0.045(5) 0.043(5) 0.010(4) 0.013(4) 0.005(4) C93 0.059(7) 0.067(7) 0.070(8) -0.004(6) 0.012(6) -0.026(6) C94 0.056(7) 0.076(8) 0.058(7) 0.024(6) 0.007(6) 0.009(6) C95 0.107(9) 0.111(9) 0.135(10) 0.004(7) 0.060(7) -0.002(7) C96 0.135(16) 0.151(17) 0.152(16) -0.002(10) 0.085(11) -0.001(9) C96' 0.119(14) 0.125(14) 0.110(13) 0.011(9) 0.062(10) 0.002(9) C97 0.078(7) 0.097(8) 0.113(9) 0.025(7) 0.043(6) 0.000(6) C98 0.096(10) 0.097(10) 0.107(11) 0.003(8) 0.042(8) -0.009(8) C99 0.087(8) 0.041(6) 0.084(8) 0.012(6) 0.052(7) 0.013(6) C100 0.134(6) 0.128(6) 0.152(6) -0.007(5) 0.068(4) -0.003(4) C101 0.134(6) 0.128(6) 0.152(6) -0.007(5) 0.068(4) -0.003(4) C102 0.094(11) 0.106(12) 0.165(13) 0.110(11) 0.061(11) 0.031(10) C103 0.094(11) 0.106(12) 0.165(13) 0.110(11) 0.061(11) 0.031(10) C104 0.134(8) 0.139(8) 0.105(8) -0.025(7) 0.055(6) 0.026(7) C105 0.134(8) 0.139(8) 0.105(8) -0.025(7) 0.055(6) 0.026(7) C106 0.108(17) 0.112(17) 0.115(17) -0.002(10) 0.056(11) 0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O8 2.311(6) . ? Dy1 O3 2.318(6) . ? Dy1 O29 2.323(7) . ? Dy1 O27 2.332(6) . ? Dy1 O25 2.352(6) . ? Dy1 O22 2.362(6) . ? Dy1 O23 2.411(6) . ? Dy1 O24 2.576(6) . ? Dy1 C62 2.857(10) . ? Dy1 Fe3 3.3366(19) . ? Dy1 Dy2 3.9134(18) . ? Dy2 O30 2.280(6) . ? Dy2 O26 2.287(7) . ? Dy2 O18 2.288(6) . ? Dy2 O28 2.304(6) . ? Dy2 O13 2.313(6) . ? Dy2 O24 2.351(6) . ? Dy2 O31 2.381(7) . ? Dy2 Fe6 3.288(2) . ? Fe1 O1 1.936(6) . ? Fe1 N5 1.988(11) . ? Fe1 O35 1.996(6) . ? Fe1 O2 2.011(6) . ? Fe1 O33 2.131(6) . ? Fe1 N1 2.134(7) . ? Fe1 Na1 3.527(4) . ? Fe2 O6 1.933(7) . ? Fe2 N8 1.983(9) . ? Fe2 O7 1.992(7) . ? Fe2 O35 2.003(6) . ? Fe2 O33 2.125(6) . ? Fe2 N2 2.138(7) . ? Fe2 Na1 3.490(5) . ? Fe3 O8 1.940(6) . ? Fe3 O3 1.949(6) . ? Fe3 O2 1.991(6) . ? Fe3 O21 1.995(6) . ? Fe3 O7 2.010(6) . ? Fe3 O33 2.098(6) . ? Fe4 O11 1.934(6) . ? Fe4 O36 1.977(7) . ? Fe4 N11 2.004(8) . ? Fe4 O12 2.028(6) . ? Fe4 N3 2.106(8) . ? Fe4 O34 2.108(5) . ? Fe4 Na2 3.417(4) . ? Fe5 O16 1.936(7) . ? Fe5 N14 1.942(14) . ? Fe5 N14' 1.96(2) . ? Fe5 O36 1.995(6) . ? Fe5 O17 2.016(7) . ? Fe5 N4 2.118(8) . ? Fe5 O34 2.143(6) . ? Fe5 Na2 3.484(4) . ? Fe6 O18 1.937(5) . ? Fe6 O13 1.947(7) . ? Fe6 O17 1.974(7) . ? Fe6 O32 2.000(7) . ? Fe6 O12 2.006(6) . ? Fe6 O34 2.090(6) . ? Na1 O37 2.285(8) . ? Na1 O6 2.365(7) . ? Na1 O1 2.369(7) . ? Na1 O10 2.382(8) . ? Na1 O5 2.388(8) . ? Na1 O35 2.868(8) . ? Na2 O38' 2.287(16) . ? Na2 O38 2.318(15) . ? Na2 O16 2.333(7) . ? Na2 O11 2.350(7) . ? Na2 O20 2.417(8) . ? Na2 O15 2.474(8) . ? Na2 O36 2.807(8) . ? N1 C7 1.289(12) . ? N1 C8 1.480(12) . ? N2 C19 1.274(12) . ? N2 C20 1.475(11) . ? N3 C31 1.278(11) . ? N3 C32 1.482(12) . ? N4 C43 1.292(14) . ? N4 C44 1.464(12) . ? N5 N6 1.174(15) . ? N6 N7 1.274(18) . ? N8 N9 1.073(15) . ? N8 N9' 1.124(9) . ? N9 N10 1.212(19) . ? N9' N10' 1.139(9) . ? N11 N12 1.195(12) . ? N12 N13 1.144(13) . ? N14 N15 1.145(8) . ? N16 N15 1.186(8) . ? N14' N15 1.151(9) . ? N16' N15 1.191(9) . ? N17 C100 1.15(2) . ? N18 C102 1.354(9) . ? N19 C104 1.32(3) . ? O1 C1 1.334(11) . ? O2 C9 1.428(10) . ? O3 C10 1.414(10) . ? O4 C11 1.468(13) . ? O4 H4 0.8200 . ? O4' C11 1.51(3) . ? O4' H4' 0.8200 . ? O5 C6 1.395(12) . ? O5 C12 1.419(13) . ? O6 C13 1.326(10) . ? O7 C21 1.433(10) . ? O8 C22 1.406(9) . ? O9 C23 1.422(12) . ? O9 H9 0.8200 . ? O10 C18 1.373(11) . ? O10 C24 1.416(13) . ? O11 C25 1.331(10) . ? O12 C33 1.441(12) . ? O13 C34 1.425(11) . ? O14 C35 1.413(15) . ? O14 H14 0.8200 . ? O15 C30 1.384(10) . ? O15 C36 1.438(12) . ? O16 C37 1.312(12) . ? O17 C45 1.422(11) . ? O18 C46 1.397(11) . ? O19 C47 1.421(18) . ? O19 H19 0.8200 . ? O19' C47 1.38(2) . ? O19' H19' 0.8200 . ? O20 C42 1.399(11) . ? O20 C48 1.430(12) . ? O21 C55 1.303(11) . ? O22 C55 1.238(10) . ? O23 C62 1.245(12) . ? O24 C62 1.275(11) . ? O25 C69 1.236(10) . ? O26 C69 1.276(11) . ? O27 C76 1.236(10) . ? O28 C76 1.283(10) . ? O29 C83 1.269(11) . ? O30 C83 1.258(10) . ? O31 C90' 1.091(19) . ? O31 C90 1.40(2) . ? O32 C90 1.13(2) . ? O32 C90' 1.458(10) . ? O33 C91 1.441(10) . ? O34 C92 1.451(9) . ? O35 C93 1.425(13) . ? O36 C94 1.452(12) . ? O37 C95 1.384(18) . ? O38 C96 1.401(19) . ? O38' C96' 1.441(19) . ? O39 C97 1.424(17) . ? O40 C98 1.54(3) . ? O41 C99 1.416(12) . ? O42 C106 1.35(5) . ? C1 C6 1.384(14) . ? C1 C2 1.406(13) . ? C2 C3 1.367(14) . ? C2 C7 1.463(14) . ? C3 C4 1.349(16) . ? C3 H3 0.9300 . ? C4 C5 1.421(16) . ? C4 H4A 0.9300 . ? C5 C6 1.394(15) . ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.537(14) . ? C8 C10 1.538(13) . ? C8 C11 1.561(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.385(13) . ? C13 C14 1.412(13) . ? C14 C15 1.409(14) . ? C14 C19 1.446(14) . ? C15 C16 1.347(14) . ? C15 H15 0.9300 . ? C16 C17 1.426(14) . ? C16 H16 0.9300 . ? C17 C18 1.373(13) . ? C17 H17 0.9300 . ? C19 H19A 0.9300 . ? C20 C22 1.532(12) . ? C20 C21 1.541(13) . ? C20 C23 1.545(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.403(12) . ? C25 C30 1.410(12) . ? C26 C27 1.390(13) . ? C26 C31 1.469(12) . ? C27 C28 1.378(14) . ? C27 H27 0.9300 . ? C28 C29 1.410(14) . ? C28 H28 0.9300 . ? C29 C30 1.384(13) . ? C29 H29 0.9300 . ? C31 H31 0.9300 . ? C32 C35 1.528(15) . ? C32 C34 1.553(13) . ? C32 C33 1.554(15) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C42 1.409(14) . ? C37 C38 1.422(13) . ? C38 C39 1.413(15) . ? C38 C43 1.442(15) . ? C39 C40 1.331(16) . ? C39 H39 0.9300 . ? C40 C41 1.418(15) . ? C40 H40 0.9300 . ? C41 C42 1.355(14) . ? C41 H41 0.9300 . ? C43 H43 0.9300 . ? C44 C47 1.529(14) . ? C44 C46 1.544(13) . ? C44 C45 1.544(14) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C54 1.368(14) . ? C49 C50 1.378(14) . ? C49 C55 1.481(13) . ? C50 C51 1.404(19) . ? C50 H50 0.9300 . ? C51 C52 1.37(2) . ? C51 H51 0.9300 . ? C52 C53 1.327(18) . ? C52 H52 0.9300 . ? C53 C54 1.378(15) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C56 C57 1.379(15) . ? C56 C61 1.383(15) . ? C56 C62 1.504(13) . ? C57 C58 1.388(16) . ? C57 H57 0.9300 . ? C58 C59 1.338(19) . ? C58 H58 0.9300 . ? C59 C60 1.370(19) . ? C59 H59 0.9300 . ? C60 C61 1.393(15) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C63 C64 1.377(14) . ? C63 C68 1.407(13) . ? C63 C69 1.497(13) . ? C64 C65 1.398(14) . ? C64 H64 0.9300 . ? C65 C66 1.382(14) . ? C65 H65 0.9300 . ? C66 C67 1.354(16) . ? C66 H66 0.9300 . ? C67 C68 1.372(15) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C70 C71 1.367(11) . ? C70 C75 1.390(12) . ? C70 C76 1.510(12) . ? C71 C72 1.368(13) . ? C71 H71 0.9300 . ? C72 C73 1.398(15) . ? C72 H72 0.9300 . ? C73 C74 1.378(15) . ? C73 H73 0.9300 . ? C74 C75 1.410(14) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C77 C82 1.390(13) . ? C77 C78 1.395(13) . ? C77 C83 1.489(12) . ? C78 C79 1.392(15) . ? C78 H78 0.9300 . ? C79 C80 1.342(17) . ? C79 H79 0.9300 . ? C80 C81 1.391(17) . ? C80 H80 0.9300 . ? C81 C82 1.377(16) . ? C81 H81 0.9300 . ? C82 H82 0.9300 . ? C84 C85 1.3900 . ? C84 C89 1.3900 . ? C84 C90 1.50(2) . ? C85 C86 1.3900 . ? C85 H85 0.9300 . ? C86 C87 1.3900 . ? C86 H86 0.9300 . ? C87 C88 1.3900 . ? C87 H87 0.9300 . ? C88 C89 1.3900 . ? C88 H88 0.9300 . ? C89 H89 0.9300 . ? C84' C85' 1.3900 . ? C84' C89' 1.3900 . ? C84' C90' 1.455(10) . ? C85' C86' 1.3900 . ? C85' H85' 0.9300 . ? C86' C87' 1.3900 . ? C86' H86' 0.9300 . ? C87' C88' 1.3900 . ? C87' H87' 0.9300 . ? C88' C89' 1.3900 . ? C88' H88' 0.9300 . ? C89' H89' 0.9300 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? C96' H96D 0.9600 . ? C96' H96E 0.9600 . ? C96' H96F 0.9600 . ? C100 C101 1.40(3) . ? C102 C103 1.499(9) . ? C104 C105 1.464(18) . ? 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 Dy1 O3 67.3(2) . . ? O8 Dy1 O29 83.0(2) . . ? O3 Dy1 O29 146.4(2) . . ? O8 Dy1 O27 77.3(2) . . ? O3 Dy1 O27 111.4(2) . . ? O29 Dy1 O27 74.8(2) . . ? O8 Dy1 O25 123.8(2) . . ? O3 Dy1 O25 80.9(2) . . ? O29 Dy1 O25 130.7(2) . . ? O27 Dy1 O25 73.0(2) . . ? O8 Dy1 O22 76.0(2) . . ? O3 Dy1 O22 80.4(2) . . ? O29 Dy1 O22 77.3(2) . . ? O27 Dy1 O22 143.3(2) . . ? O25 Dy1 O22 143.6(2) . . ? O8 Dy1 O23 138.0(2) . . ? O3 Dy1 O23 80.3(2) . . ? O29 Dy1 O23 116.1(2) . . ? O27 Dy1 O23 141.8(2) . . ? O25 Dy1 O23 73.4(2) . . ? O22 Dy1 O23 72.9(2) . . ? O8 Dy1 O24 157.6(2) . . ? O3 Dy1 O24 131.1(2) . . ? O29 Dy1 O24 75.4(2) . . ? O27 Dy1 O24 102.3(2) . . ? O25 Dy1 O24 76.2(2) . . ? O22 Dy1 O24 93.3(2) . . ? O23 Dy1 O24 52.0(2) . . ? O8 Dy1 C62 158.8(2) . . ? O3 Dy1 C62 105.1(3) . . ? O29 Dy1 C62 97.1(3) . . ? O27 Dy1 C62 123.4(2) . . ? O25 Dy1 C62 71.8(2) . . ? O22 Dy1 C62 83.3(2) . . ? O23 Dy1 C62 25.6(2) . . ? O24 Dy1 C62 26.5(3) . . ? O8 Dy1 Fe3 34.51(14) . . ? O3 Dy1 Fe3 34.76(15) . . ? O29 Dy1 Fe3 112.19(15) . . ? O27 Dy1 Fe3 102.35(15) . . ? O25 Dy1 Fe3 110.43(16) . . ? O22 Dy1 Fe3 67.03(16) . . ? O23 Dy1 Fe3 105.89(17) . . ? O24 Dy1 Fe3 155.38(14) . . ? C62 Dy1 Fe3 131.0(2) . . ? O8 Dy1 Dy2 139.70(14) . . ? O3 Dy1 Dy2 143.03(14) . . ? O29 Dy1 Dy2 70.51(14) . . ? O27 Dy1 Dy2 67.01(14) . . ? O25 Dy1 Dy2 62.98(16) . . ? O22 Dy1 Dy2 124.18(16) . . ? O23 Dy1 Dy2 81.91(17) . . ? O24 Dy1 Dy2 35.45(14) . . ? C62 Dy1 Dy2 57.8(2) . . ? Fe3 Dy1 Dy2 168.40(3) . . ? O30 Dy2 O26 137.3(2) . . ? O30 Dy2 O18 85.1(2) . . ? O26 Dy2 O18 123.6(2) . . ? O30 Dy2 O28 80.4(2) . . ? O26 Dy2 O28 76.8(2) . . ? O18 Dy2 O28 77.7(2) . . ? O30 Dy2 O13 145.2(2) . . ? O26 Dy2 O13 77.5(2) . . ? O18 Dy2 O13 69.0(2) . . ? O28 Dy2 O13 114.5(2) . . ? O30 Dy2 O24 77.6(2) . . ? O26 Dy2 O24 75.5(2) . . ? O18 Dy2 O24 160.7(2) . . ? O28 Dy2 O24 107.3(2) . . ? O13 Dy2 O24 122.5(2) . . ? O30 Dy2 O31 79.2(2) . . ? O26 Dy2 O31 130.9(3) . . ? O18 Dy2 O31 81.8(3) . . ? O28 Dy2 O31 152.1(3) . . ? O13 Dy2 O31 74.5(2) . . ? O24 Dy2 O31 86.6(2) . . ? O30 Dy2 Fe6 112.39(16) . . ? O26 Dy2 Fe6 107.89(16) . . ? O18 Dy2 Fe6 35.19(14) . . ? O28 Dy2 Fe6 103.83(16) . . ? O13 Dy2 Fe6 35.57(16) . . ? O24 Dy2 Fe6 148.53(15) . . ? O31 Dy2 Fe6 67.29(18) . . ? O30 Dy2 Dy1 65.80(15) . . ? O26 Dy2 Dy1 72.32(16) . . ? O18 Dy2 Dy1 137.93(14) . . ? O28 Dy2 Dy1 68.30(15) . . ? O13 Dy2 Dy1 148.13(16) . . ? O24 Dy2 Dy1 39.46(15) . . ? O31 Dy2 Dy1 118.92(17) . . ? Fe6 Dy2 Dy1 172.01(3) . . ? O1 Fe1 N5 99.9(4) . . ? O1 Fe1 O35 92.7(3) . . ? N5 Fe1 O35 96.0(4) . . ? O1 Fe1 O2 160.8(3) . . ? N5 Fe1 O2 93.5(3) . . ? O35 Fe1 O2 99.6(3) . . ? O1 Fe1 O33 90.6(2) . . ? N5 Fe1 O33 166.7(3) . . ? O35 Fe1 O33 75.2(2) . . ? O2 Fe1 O33 78.5(2) . . ? O1 Fe1 N1 87.7(3) . . ? N5 Fe1 N1 93.3(4) . . ? O35 Fe1 N1 170.5(3) . . ? O2 Fe1 N1 77.8(3) . . ? O33 Fe1 N1 95.3(2) . . ? O1 Fe1 Na1 39.26(19) . . ? N5 Fe1 Na1 109.3(3) . . ? O35 Fe1 Na1 54.4(2) . . ? O2 Fe1 Na1 145.95(18) . . ? O33 Fe1 Na1 73.88(17) . . ? N1 Fe1 Na1 123.8(2) . . ? O6 Fe2 N8 98.0(4) . . ? O6 Fe2 O7 160.2(2) . . ? N8 Fe2 O7 94.9(4) . . ? O6 Fe2 O35 94.7(3) . . ? N8 Fe2 O35 95.5(3) . . ? O7 Fe2 O35 99.0(3) . . ? O6 Fe2 O33 90.6(2) . . ? N8 Fe2 O33 167.8(4) . . ? O7 Fe2 O33 79.2(2) . . ? O35 Fe2 O33 75.2(2) . . ? O6 Fe2 N2 86.4(3) . . ? N8 Fe2 N2 92.2(3) . . ? O7 Fe2 N2 78.1(3) . . ? O35 Fe2 N2 172.1(3) . . ? O33 Fe2 N2 97.0(2) . . ? O6 Fe2 Na1 40.10(19) . . ? N8 Fe2 Na1 106.5(3) . . ? O7 Fe2 Na1 147.18(18) . . ? O35 Fe2 Na1 55.3(2) . . ? O33 Fe2 Na1 74.81(18) . . ? N2 Fe2 Na1 124.4(2) . . ? O8 Fe3 O3 82.5(2) . . ? O8 Fe3 O2 170.8(3) . . ? O3 Fe3 O2 93.1(2) . . ? O8 Fe3 O21 93.9(3) . . ? O3 Fe3 O21 96.1(2) . . ? O2 Fe3 O21 94.5(3) . . ? O8 Fe3 O7 92.6(2) . . ? O3 Fe3 O7 171.3(2) . . ? O2 Fe3 O7 90.7(2) . . ? O21 Fe3 O7 91.5(3) . . ? O8 Fe3 O33 92.5(2) . . ? O3 Fe3 O33 93.5(2) . . ? O2 Fe3 O33 79.7(2) . . ? O21 Fe3 O33 169.1(2) . . ? O7 Fe3 O33 79.4(2) . . ? O8 Fe3 Dy1 42.44(17) . . ? O3 Fe3 Dy1 42.69(17) . . ? O2 Fe3 Dy1 135.09(18) . . ? O21 Fe3 Dy1 85.05(18) . . ? O7 Fe3 Dy1 134.25(17) . . ? O33 Fe3 Dy1 105.62(16) . . ? O11 Fe4 O36 96.6(3) . . ? O11 Fe4 N11 98.5(3) . . ? O36 Fe4 N11 95.4(3) . . ? O11 Fe4 O12 160.6(3) . . ? O36 Fe4 O12 95.2(3) . . ? N11 Fe4 O12 95.6(3) . . ? O11 Fe4 N3 88.1(3) . . ? O36 Fe4 N3 172.3(3) . . ? N11 Fe4 N3 89.9(3) . . ? O12 Fe4 N3 78.7(3) . . ? O11 Fe4 O34 89.4(2) . . ? O36 Fe4 O34 76.7(2) . . ? N11 Fe4 O34 169.5(3) . . ? O12 Fe4 O34 78.5(2) . . ? N3 Fe4 O34 97.3(2) . . ? O11 Fe4 Na2 41.53(19) . . ? O36 Fe4 Na2 55.2(2) . . ? N11 Fe4 Na2 103.8(3) . . ? O12 Fe4 Na2 145.5(2) . . ? N3 Fe4 Na2 128.7(2) . . ? O34 Fe4 Na2 77.58(17) . . ? O16 Fe5 N14 108.4(5) . . ? O16 Fe5 N14' 82.3(8) . . ? N14 Fe5 N14' 26.5(7) . . ? O16 Fe5 O36 92.4(3) . . ? N14 Fe5 O36 94.8(5) . . ? N14' Fe5 O36 100.5(8) . . ? O16 Fe5 O17 160.6(3) . . ? N14 Fe5 O17 86.4(5) . . ? N14' Fe5 O17 110.8(8) . . ? O36 Fe5 O17 98.9(3) . . ? O16 Fe5 N4 88.8(3) . . ? N14 Fe5 N4 93.8(5) . . ? N14' Fe5 N4 89.0(8) . . ? O36 Fe5 N4 170.4(3) . . ? O17 Fe5 N4 77.5(3) . . ? O16 Fe5 O34 90.0(3) . . ? N14 Fe5 O34 159.7(5) . . ? N14' Fe5 O34 171.2(8) . . ? O36 Fe5 O34 75.5(2) . . ? O17 Fe5 O34 77.7(3) . . ? N4 Fe5 O34 95.0(2) . . ? O16 Fe5 Na2 39.28(19) . . ? N14 Fe5 Na2 113.2(4) . . ? N14' Fe5 Na2 95.7(8) . . ? O36 Fe5 Na2 53.7(2) . . ? O17 Fe5 Na2 145.7(2) . . ? N4 Fe5 Na2 125.8(2) . . ? O34 Fe5 Na2 75.63(17) . . ? O18 Fe6 O13 84.3(3) . . ? O18 Fe6 O17 92.9(3) . . ? O13 Fe6 O17 171.0(3) . . ? O18 Fe6 O32 95.1(3) . . ? O13 Fe6 O32 93.3(3) . . ? O17 Fe6 O32 95.4(3) . . ? O18 Fe6 O12 172.0(3) . . ? O13 Fe6 O12 93.4(3) . . ? O17 Fe6 O12 88.2(3) . . ? O32 Fe6 O12 92.7(3) . . ? O18 Fe6 O34 93.0(2) . . ? O13 Fe6 O34 91.7(2) . . ? O17 Fe6 O34 79.9(3) . . ? O32 Fe6 O34 170.9(3) . . ? O12 Fe6 O34 79.4(2) . . ? O18 Fe6 Dy2 42.91(19) . . ? O13 Fe6 Dy2 43.73(17) . . ? O17 Fe6 Dy2 135.25(19) . . ? O32 Fe6 Dy2 84.6(2) . . ? O12 Fe6 Dy2 136.6(2) . . ? O34 Fe6 Dy2 104.23(15) . . ? O37 Na1 O6 121.9(3) . . ? O37 Na1 O1 117.6(3) . . ? O6 Na1 O1 107.2(3) . . ? O37 Na1 O10 87.2(3) . . ? O6 Na1 O10 66.3(2) . . ? O1 Na1 O10 151.1(3) . . ? O37 Na1 O5 83.1(3) . . ? O6 Na1 O5 151.8(3) . . ? O1 Na1 O5 66.0(2) . . ? O10 Na1 O5 105.6(3) . . ? O37 Na1 O35 100.6(3) . . ? O6 Na1 O35 66.4(2) . . ? O1 Na1 O35 65.0(2) . . ? O10 Na1 O35 128.2(3) . . ? O5 Na1 O35 126.1(3) . . ? O37 Na1 Fe2 119.5(3) . . ? O6 Na1 Fe2 31.76(17) . . ? O1 Na1 Fe2 83.72(19) . . ? O10 Na1 Fe2 97.2(2) . . ? O5 Na1 Fe2 148.8(2) . . ? O35 Na1 Fe2 35.02(13) . . ? O37 Na1 Fe1 117.6(3) . . ? O6 Na1 Fe1 83.90(19) . . ? O1 Na1 Fe1 31.15(16) . . ? O10 Na1 Fe1 148.9(2) . . ? O5 Na1 Fe1 96.4(2) . . ? O35 Na1 Fe1 34.45(13) . . ? Fe2 Na1 Fe1 55.17(7) . . ? O38' Na2 O38 24.7(7) . . ? O38' Na2 O16 142.0(7) . . ? O38 Na2 O16 117.7(7) . . ? O38' Na2 O11 101.2(7) . . ? O38 Na2 O11 120.6(6) . . ? O16 Na2 O11 104.5(3) . . ? O38' Na2 O20 102.7(7) . . ? O38 Na2 O20 88.0(6) . . ? O16 Na2 O20 66.1(2) . . ? O11 Na2 O20 149.5(3) . . ? O38' Na2 O15 84.9(7) . . ? O38 Na2 O15 106.6(7) . . ? O16 Na2 O15 131.3(3) . . ? O11 Na2 O15 65.5(2) . . ? O20 Na2 O15 98.0(3) . . ? O38' Na2 O36 98.8(7) . . ? O38 Na2 O36 91.8(6) . . ? O16 Na2 O36 66.3(2) . . ? O11 Na2 O36 68.3(2) . . ? O20 Na2 O36 125.6(3) . . ? O15 Na2 O36 133.5(3) . . ? O38' Na2 Fe4 104.1(7) . . ? O38 Na2 Fe4 111.3(6) . . ? O16 Na2 Fe4 83.8(2) . . ? O11 Na2 Fe4 33.07(15) . . ? O20 Na2 Fe4 149.5(2) . . ? O15 Na2 Fe4 98.56(19) . . ? O36 Na2 Fe4 35.35(14) . . ? O38' Na2 Fe5 127.8(7) . . ? O38 Na2 Fe5 111.1(6) . . ? O16 Na2 Fe5 31.70(18) . . ? O11 Na2 Fe5 83.94(18) . . ? O20 Na2 Fe5 96.04(19) . . ? O15 Na2 Fe5 140.0(2) . . ? O36 Na2 Fe5 34.93(13) . . ? Fe4 Na2 Fe5 55.66(7) . . ? C7 N1 C8 119.2(8) . . ? C7 N1 Fe1 125.9(7) . . ? C8 N1 Fe1 114.9(6) . . ? C19 N2 C20 118.5(8) . . ? C19 N2 Fe2 126.7(6) . . ? C20 N2 Fe2 114.7(6) . . ? C31 N3 C32 118.3(9) . . ? C31 N3 Fe4 126.4(6) . . ? C32 N3 Fe4 115.2(6) . . ? C43 N4 C44 120.1(8) . . ? C43 N4 Fe5 123.5(7) . . ? C44 N4 Fe5 116.3(7) . . ? N6 N5 Fe1 124.0(11) . . ? N5 N6 N7 178.1(16) . . ? N9 N8 N9' 80.9(17) . . ? N9 N8 Fe2 131.0(12) . . ? N9' N8 Fe2 137.6(18) . . ? N8 N9 N10 176.1(17) . . ? N8 N9' N10' 170(4) . . ? N12 N11 Fe4 121.5(7) . . ? N13 N12 N11 178.9(13) . . ? N15 N14 Fe5 143.5(14) . . ? N15 N14' Fe5 140(2) . . ? N14 N15 N14' 45.9(15) . . ? N14 N15 N16 168(2) . . ? N14' N15 N16 135(2) . . ? N14 N15 N16' 122(2) . . ? N14' N15 N16' 165(3) . . ? N16 N15 N16' 59.5(19) . . ? C1 O1 Fe1 132.8(6) . . ? C1 O1 Na1 116.8(6) . . ? Fe1 O1 Na1 109.6(3) . . ? C9 O2 Fe3 114.6(6) . . ? C9 O2 Fe1 112.2(5) . . ? Fe3 O2 Fe1 104.6(3) . . ? C10 O3 Fe3 130.0(5) . . ? C10 O3 Dy1 123.2(5) . . ? Fe3 O3 Dy1 102.6(2) . . ? C11 O4 H4 109.5 . . ? C11 O4' H4' 109.5 . . ? C6 O5 C12 117.0(8) . . ? C6 O5 Na1 116.3(6) . . ? C12 O5 Na1 123.4(6) . . ? C13 O6 Fe2 133.8(6) . . ? C13 O6 Na1 118.0(6) . . ? Fe2 O6 Na1 108.1(3) . . ? C21 O7 Fe2 111.6(5) . . ? C21 O7 Fe3 115.8(5) . . ? Fe2 O7 Fe3 104.3(3) . . ? C22 O8 Fe3 128.9(5) . . ? C22 O8 Dy1 121.8(5) . . ? Fe3 O8 Dy1 103.0(2) . . ? C23 O9 H9 109.5 . . ? C18 O10 C24 117.8(8) . . ? C18 O10 Na1 118.1(6) . . ? C24 O10 Na1 122.0(6) . . ? C25 O11 Fe4 131.4(6) . . ? C25 O11 Na2 123.2(5) . . ? Fe4 O11 Na2 105.4(3) . . ? C33 O12 Fe6 116.1(6) . . ? C33 O12 Fe4 110.5(5) . . ? Fe6 O12 Fe4 103.5(3) . . ? C34 O13 Fe6 126.9(6) . . ? C34 O13 Dy2 123.7(5) . . ? Fe6 O13 Dy2 100.7(3) . . ? C35 O14 H14 109.5 . . ? C30 O15 C36 116.8(8) . . ? C30 O15 Na2 118.7(5) . . ? C36 O15 Na2 124.5(6) . . ? C37 O16 Fe5 129.7(6) . . ? C37 O16 Na2 121.0(6) . . ? Fe5 O16 Na2 109.0(3) . . ? C45 O17 Fe6 113.6(6) . . ? C45 O17 Fe5 112.9(7) . . ? Fe6 O17 Fe5 105.2(3) . . ? C46 O18 Fe6 131.3(6) . . ? C46 O18 Dy2 124.3(5) . . ? Fe6 O18 Dy2 101.9(3) . . ? C47 O19 H19 109.5 . . ? C47 O19' H19' 109.5 . . ? C42 O20 C48 117.1(8) . . ? C42 O20 Na2 117.6(6) . . ? C48 O20 Na2 124.7(6) . . ? C55 O21 Fe3 126.2(6) . . ? C55 O22 Dy1 136.4(6) . . ? C62 O23 Dy1 97.7(5) . . ? C62 O24 Dy2 137.5(6) . . ? C62 O24 Dy1 89.2(6) . . ? Dy2 O24 Dy1 105.1(2) . . ? C69 O25 Dy1 143.5(7) . . ? C69 O26 Dy2 126.2(6) . . ? C76 O27 Dy1 135.0(6) . . ? C76 O28 Dy2 136.3(6) . . ? C83 O29 Dy1 133.5(6) . . ? C83 O30 Dy2 144.5(6) . . ? C90' O31 C90 24.3(12) . . ? C90' O31 Dy2 137.5(9) . . ? C90 O31 Dy2 131.6(9) . . ? C90 O32 C90' 22.9(12) . . ? C90 O32 Fe6 133.0(11) . . ? C90' O32 Fe6 121.1(8) . . ? C91 O33 Fe3 116.3(5) . . ? C91 O33 Fe2 122.3(5) . . ? Fe3 O33 Fe2 96.8(2) . . ? C91 O33 Fe1 119.8(5) . . ? Fe3 O33 Fe1 97.0(2) . . ? Fe2 O33 Fe1 99.6(2) . . ? C92 O34 Fe6 116.5(5) . . ? C92 O34 Fe4 120.1(5) . . ? Fe6 O34 Fe4 97.9(2) . . ? C92 O34 Fe5 121.8(5) . . ? Fe6 O34 Fe5 97.0(2) . . ? Fe4 O34 Fe5 98.6(2) . . ? C93 O35 Fe1 124.4(6) . . ? C93 O35 Fe2 124.7(6) . . ? Fe1 O35 Fe2 108.7(3) . . ? C93 O35 Na1 102.6(7) . . ? Fe1 O35 Na1 91.2(2) . . ? Fe2 O35 Na1 89.7(2) . . ? C94 O36 Fe4 122.1(7) . . ? C94 O36 Fe5 122.4(6) . . ? Fe4 O36 Fe5 108.4(3) . . ? C94 O36 Na2 113.4(6) . . ? Fe4 O36 Na2 89.4(2) . . ? Fe5 O36 Na2 91.4(2) . . ? C95 O37 Na1 130.6(9) . . ? C96 O38 Na2 143(2) . . ? C96' O38' Na2 118.0(19) . . ? O1 C1 C6 119.0(9) . . ? O1 C1 C2 123.4(9) . . ? C6 C1 C2 117.6(9) . . ? C3 C2 C1 120.0(10) . . ? C3 C2 C7 116.3(9) . . ? C1 C2 C7 123.7(9) . . ? C4 C3 C2 122.1(10) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 120.6(11) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 116.6(11) . . ? C6 C5 H5 121.7 . . ? C4 C5 H5 121.7 . . ? C1 C6 C5 123.2(10) . . ? C1 C6 O5 113.6(9) . . ? C5 C6 O5 123.2(10) . . ? N1 C7 C2 125.7(9) . . ? N1 C7 H7 117.1 . . ? C2 C7 H7 117.1 . . ? N1 C8 C9 105.4(8) . . ? N1 C8 C10 111.9(8) . . ? C9 C8 C10 111.3(8) . . ? N1 C8 C11 111.9(8) . . ? C9 C8 C11 108.1(8) . . ? C10 C8 C11 108.2(8) . . ? O2 C9 C8 109.4(7) . . ? O2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? O2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? O3 C10 C8 113.3(7) . . ? O3 C10 H10A 108.9 . . ? C8 C10 H10A 108.9 . . ? O3 C10 H10B 108.9 . . ? C8 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? O4 C11 O4' 105.1(12) . . ? O4 C11 C8 110.5(8) . . ? O4' C11 C8 113.6(12) . . ? O4 C11 H11A 109.6 . . ? O4' C11 H11A 108.4 . . ? C8 C11 H11A 109.6 . . ? O4 C11 H11B 109.6 . . ? O4' C11 H11B 4.9 . . ? C8 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 C13 C18 119.0(8) . . ? O6 C13 C14 121.9(9) . . ? C18 C13 C14 119.1(9) . . ? C15 C14 C13 117.9(9) . . ? C15 C14 C19 117.5(9) . . ? C13 C14 C19 124.5(9) . . ? C16 C15 C14 122.6(9) . . ? C16 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 C16 C17 119.4(9) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 118.6(9) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? O10 C18 C17 123.3(9) . . ? O10 C18 C13 114.4(8) . . ? C17 C18 C13 122.3(9) . . ? N2 C19 C14 125.1(9) . . ? N2 C19 H19A 117.5 . . ? C14 C19 H19A 117.5 . . ? N2 C20 C22 110.7(7) . . ? N2 C20 C21 104.5(7) . . ? C22 C20 C21 111.7(7) . . ? N2 C20 C23 113.8(7) . . ? C22 C20 C23 107.1(7) . . ? C21 C20 C23 109.0(7) . . ? O7 C21 C20 109.2(7) . . ? O7 C21 H21A 109.8 . . ? C20 C21 H21A 109.8 . . ? O7 C21 H21B 109.8 . . ? C20 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? O8 C22 C20 115.1(7) . . ? O8 C22 H22A 108.5 . . ? C20 C22 H22A 108.5 . . ? O8 C22 H22B 108.5 . . ? C20 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? O9 C23 C20 108.2(7) . . ? O9 C23 H23A 110.1 . . ? C20 C23 H23A 110.1 . . ? O9 C23 H23B 110.1 . . ? C20 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? O10 C24 H24A 109.5 . . ? O10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O11 C25 C26 124.6(8) . . ? O11 C25 C30 118.2(8) . . ? C26 C25 C30 117.2(8) . . ? C27 C26 C25 120.6(8) . . ? C27 C26 C31 116.8(9) . . ? C25 C26 C31 122.6(8) . . ? C28 C27 C26 121.0(9) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.9(9) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 118.5(9) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C29 C30 O15 123.1(8) . . ? C29 C30 C25 122.6(8) . . ? O15 C30 C25 114.3(8) . . ? N3 C31 C26 125.5(9) . . ? N3 C31 H31 117.3 . . ? C26 C31 H31 117.3 . . ? N3 C32 C35 115.0(8) . . ? N3 C32 C34 109.9(7) . . ? C35 C32 C34 109.6(9) . . ? N3 C32 C33 105.6(8) . . ? C35 C32 C33 105.4(9) . . ? C34 C32 C33 111.2(8) . . ? O12 C33 C32 108.7(7) . . ? O12 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O12 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O13 C34 C32 113.5(8) . . ? O13 C34 H34A 108.9 . . ? C32 C34 H34A 108.9 . . ? O13 C34 H34B 108.9 . . ? C32 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? O14 C35 C32 113.3(9) . . ? O14 C35 H35A 108.9 . . ? C32 C35 H35A 108.9 . . ? O14 C35 H35B 108.9 . . ? C32 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? O15 C36 H36A 109.5 . . ? O15 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O15 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O16 C37 C42 118.7(9) . . ? O16 C37 C38 123.5(9) . . ? C42 C37 C38 117.7(10) . . ? C39 C38 C37 117.7(10) . . ? C39 C38 C43 119.3(10) . . ? C37 C38 C43 123.0(9) . . ? C40 C39 C38 123.3(10) . . ? C40 C39 H39 118.4 . . ? C38 C39 H39 118.4 . . ? C39 C40 C41 119.4(10) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C42 C41 C40 119.3(11) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C41 C42 O20 124.3(10) . . ? C41 C42 C37 122.6(10) . . ? O20 C42 C37 113.1(8) . . ? N4 C43 C38 127.2(9) . . ? N4 C43 H43 116.4 . . ? C38 C43 H43 116.4 . . ? N4 C44 C47 114.2(9) . . ? N4 C44 C46 109.6(7) . . ? C47 C44 C46 108.4(8) . . ? N4 C44 C45 105.5(7) . . ? C47 C44 C45 108.8(8) . . ? C46 C44 C45 110.2(9) . . ? O17 C45 C44 109.6(8) . . ? O17 C45 H45A 109.7 . . ? C44 C45 H45A 109.7 . . ? O17 C45 H45B 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? O18 C46 C44 114.4(7) . . ? O18 C46 H46A 108.7 . . ? C44 C46 H46A 108.7 . . ? O18 C46 H46B 108.7 . . ? C44 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? O19' C47 O19 85.4(13) . . ? O19' C47 C44 111.2(12) . . ? O19 C47 C44 110.2(11) . . ? O19' C47 H47A 127.5 . . ? O19 C47 H47A 109.6 . . ? C44 C47 H47A 109.6 . . ? O19' C47 H47B 26.1 . . ? O19 C47 H47B 109.6 . . ? C44 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? O20 C48 H48A 109.5 . . ? O20 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O20 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C54 C49 C50 119.9(10) . . ? C54 C49 C55 119.5(8) . . ? C50 C49 C55 120.5(10) . . ? C49 C50 C51 117.5(12) . . ? C49 C50 H50 121.3 . . ? C51 C50 H50 121.3 . . ? C52 C51 C50 121.0(15) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C53 C52 C51 120.7(15) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 119.7(12) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C49 C54 C53 121.2(9) . . ? C49 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? O22 C55 O21 124.8(9) . . ? O22 C55 C49 120.3(9) . . ? O21 C55 C49 114.9(8) . . ? C57 C56 C61 121.1(9) . . ? C57 C56 C62 118.4(10) . . ? C61 C56 C62 120.4(10) . . ? C56 C57 C58 119.9(12) . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C59 C58 C57 118.2(13) . . ? C59 C58 H58 120.9 . . ? C57 C58 H58 120.9 . . ? C58 C59 C60 123.7(13) . . ? C58 C59 H59 118.1 . . ? C60 C59 H59 118.1 . . ? C59 C60 C61 118.8(13) . . ? C59 C60 H60 120.6 . . ? C61 C60 H60 120.6 . . ? C56 C61 C60 118.2(12) . . ? C56 C61 H61 120.9 . . ? C60 C61 H61 120.9 . . ? O23 C62 O24 120.9(9) . . ? O23 C62 C56 118.5(9) . . ? O24 C62 C56 120.6(10) . . ? O23 C62 Dy1 56.7(5) . . ? O24 C62 Dy1 64.3(5) . . ? C56 C62 Dy1 173.2(8) . . ? C64 C63 C68 117.7(9) . . ? C64 C63 C69 121.3(8) . . ? C68 C63 C69 121.0(9) . . ? C63 C64 C65 121.5(9) . . ? C63 C64 H64 119.3 . . ? C65 C64 H64 119.3 . . ? C66 C65 C64 119.8(10) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C67 C66 C65 118.6(10) . . ? C67 C66 H66 120.7 . . ? C65 C66 H66 120.7 . . ? C66 C67 C68 122.9(10) . . ? C66 C67 H67 118.6 . . ? C68 C67 H67 118.6 . . ? C67 C68 C63 119.6(10) . . ? C67 C68 H68 120.2 . . ? C63 C68 H68 120.2 . . ? O25 C69 O26 125.6(9) . . ? O25 C69 C63 118.1(9) . . ? O26 C69 C63 116.3(8) . . ? C71 C70 C75 119.8(8) . . ? C71 C70 C76 120.8(8) . . ? C75 C70 C76 119.4(8) . . ? C70 C71 C72 122.0(9) . . ? C70 C71 H71 119.0 . . ? C72 C71 H71 119.0 . . ? C71 C72 C73 119.7(9) . . ? C71 C72 H72 120.1 . . ? C73 C72 H72 120.1 . . ? C74 C73 C72 118.8(9) . . ? C74 C73 H73 120.6 . . ? C72 C73 H73 120.6 . . ? C73 C74 C75 121.2(10) . . ? C73 C74 H74 119.4 . . ? C75 C74 H74 119.4 . . ? C70 C75 C74 118.5(9) . . ? C70 C75 H75 120.8 . . ? C74 C75 H75 120.8 . . ? O27 C76 O28 124.4(8) . . ? O27 C76 C70 118.3(8) . . ? O28 C76 C70 117.3(8) . . ? C82 C77 C78 120.0(9) . . ? C82 C77 C83 120.1(9) . . ? C78 C77 C83 119.8(9) . . ? C79 C78 C77 117.9(10) . . ? C79 C78 H78 121.0 . . ? C77 C78 H78 121.0 . . ? C80 C79 C78 122.9(11) . . ? C80 C79 H79 118.5 . . ? C78 C79 H79 118.5 . . ? C79 C80 C81 118.7(11) . . ? C79 C80 H80 120.7 . . ? C81 C80 H80 120.7 . . ? C82 C81 C80 121.0(11) . . ? C82 C81 H81 119.5 . . ? C80 C81 H81 119.5 . . ? C81 C82 C77 119.5(10) . . ? C81 C82 H82 120.3 . . ? C77 C82 H82 120.3 . . ? O30 C83 O29 123.5(8) . . ? O30 C83 C77 117.3(9) . . ? O29 C83 C77 119.1(8) . . ? C85 C84 C89 120.0 . . ? C85 C84 C90 121.3(12) . . ? C89 C84 C90 118.6(12) . . ? C84 C85 C86 120.0 . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C85 C86 C87 120.0 . . ? C85 C86 H86 120.0 . . ? C87 C86 H86 120.0 . . ? C86 C87 C88 120.0 . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C89 C88 C87 120.0 . . ? C89 C88 H88 120.0 . . ? C87 C88 H88 120.0 . . ? C88 C89 C84 120.0 . . ? C88 C89 H89 120.0 . . ? C84 C89 H89 120.0 . . ? C85' C84' C89' 120.0 . . ? C85' C84' C90' 120.8(17) . . ? C89' C84' C90' 119.2(17) . . ? C86' C85' C84' 120.0 . . ? C86' C85' H85' 120.0 . . ? C84' C85' H85' 120.0 . . ? C85' C86' C87' 120.0 . . ? C85' C86' H86' 120.0 . . ? C87' C86' H86' 120.0 . . ? C88' C87' C86' 120.0 . . ? C88' C87' H87' 120.0 . . ? C86' C87' H87' 120.0 . . ? C87' C88' C89' 120.0 . . ? C87' C88' H88' 120.0 . . ? C89' C88' H88' 120.0 . . ? C88' C89' C84' 120.0 . . ? C88' C89' H89' 120.0 . . ? C84' C89' H89' 120.0 . . ? O32 C90 O31 120.4(16) . . ? O32 C90 C84 122.7(17) . . ? O31 C90 C84 116.2(16) . . ? O31 C90' C84' 122.4(15) . . ? O31 C90' O32 118.7(12) . . ? C84' C90' O32 118.4(16) . . ? O33 C91 H91A 109.5 . . ? O33 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? O33 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? O34 C92 H92A 109.5 . . ? O34 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? O34 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? O35 C93 H93A 109.5 . . ? O35 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? O35 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O36 C94 H94A 109.5 . . ? O36 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? O36 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? O37 C95 H95A 109.5 . . ? O37 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? O37 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? O38 C96 H96A 109.5 . . ? O38 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? O38 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? O38' C96' H96D 109.5 . . ? O38' C96' H96E 109.5 . . ? H96D C96' H96E 109.5 . . ? O38' C96' H96F 109.5 . . ? H96D C96' H96F 109.5 . . ? H96E C96' H96F 109.5 . . ? N17 C100 C101 173(3) . . ? N18 C102 C103 171(4) . . ? N19 C104 C105 167(3) . . ? 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 O4 H4 O41 0.82 2.17 2.809(12) 134.8 4_575 O4' H4' N13 0.82 2.14 2.67(3) 122.6 3_666 O4' H4' N7 0.82 2.54 3.06(3) 122.7 . O14 H14 N19 0.82 2.22 2.97(2) 150.4 3_666 O19 H19 O40 0.82 2.32 3.03(3) 145.7 1_655 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.406 _refine_diff_density_min -2.217 _refine_diff_density_rms 0.145 _iucr_refine_instructions_details ; TITL sad in P2(1)/c CELL 0.71073 23.5669 23.4579 29.6243 90.000 121.654 90.000 ZERR 4.00 0.0047 0.0047 0.0059 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Na Fe Dy UNIT 412 520 72 176 8 24 8 omit -1 2 4 omit 1 4 1 omit 0 0 6 omit -6 3 8 omit -4 2 1 omit -4 2 5 omit -6 2 4 omit -1 6 2 omit 5 5 1 omit -3 0 8 omit 3 8 3 omit -3 8 8 omit -5 1 5 omit -5 4 10 omit -2 4 6 omit 2 1 5 omit -5 2 2 omit -10 4 4 omit 1 2 5 omit -8 0 10 omit 3 1 0 omit -5 3 7 omit -8 2 1 omit -10 2 10 omit -1 3 3 omit -4 2 6 omit -2 4 2 omit 4 4 0 omit -7 3 4 omit 7 0 0 omit -4 3 10 omit -1 8 6 omit -7 4 4 omit -4 1 2 omit -3 1 9 omit 2 8 1 omit -5 0 2 omit 0 4 5 omit 0 1 4 omit -6 0 2 omit 0 4 1 omit -4 0 2 omit 1 4 5 omit -5 0 4 omit -7 2 4 omit -6 0 4 omit 2 0 6 omit 0 6 5 omit 1 3 7 omit -1 2 6 omit -7 0 4 omit -4 3 5 omit 1 0 4 omit -4 5 2 omit -6 2 1 omit -3 8 4 omit 4 6 3 omit -6 2 2 omit -6 4 4 omit -3 1 4 omit -4 1 1 omit 1 3 5 omit -9 2 6 omit -2 6 2 omit -1 7 1 omit -3 4 3 omit -4 4 3 omit -5 3 3 omit -3 5 2 omit -5 4 7 omit -8 2 6 omit 1 1 5 omit -4 3 9 omit 0 2 4 omit 1 3 1 omit -7 1 5 omit -3 4 5 omit -3 0 6 omit 3 1 1 omit 2 4 5 omit -4 4 9 omit -5 2 5 omit -4 4 8 L.S. 20 BOND $h eqiv $1 x, -y+3/2, z-1/2 eqiv $2 -x+1, -y+1, -z+1 eqiv $3 x+1, y, z Htab O4 O41_$1 htab O4' N13_$2 htab O4' N7 htab O14 N19_$2 htab O19 O40_$3 acta htab dfix 1.45 0.01 c90' c84' c90' o32 flat c84' c90' o32 o31 dfix 1.40 0.02 o38 c96 o38' c96' dfix 2.30 0.02 na2 o38 na2 o38' dfix 1.10 0.01 n8 n9' dfix 1.10 0.01 n9' n10' dfix 2.30 0.01 n8 n10' dfix 1.10 0.01 n14 n15 dfix 1.10 0.01 n15 n16 dfix 2.40 0.01 n14 n16 dfix 1.10 0.01 n14' n15 dfix 1.10 0.01 n15 n16' dfix 2.40 0.01 n14' n16' dfix 1.40 0.02 c104 c105 dfix 1.45 0.01 c103 c102 dfix 1.30 0.01 c102 n18 dfix 2.90 0.01 c103 n18 isor 0.01 0.01 n17 n19 o39 o40 c97 c98 c90 c90' isor 0.01 0.01 c100 c101 c106 o19' isor 0.01 0.01 o38 o38' n15 n14 n16 c59 c95 c96 c96' omit 0 50 isor 0.001 0.001 n6 n7 n10 n10' n9' n13 o19 c47 c51 c52 c58 n14' o42 simu 0.001 0.001 3.3 c104 c105 n19 simu 0.001 0.001 3.3 c102 c103 n18 simu 0.001 0.001 3.3 n17 c100 c101 simu 0.01 0.01 3.3 c84 c85 c86 c87 c88 c89 simu 0.01 0.01 3.3 c84' c85' c86' c87' c88' c89' simu 0.01 0.01 3.3 n5 n6 n7 simu 0.01 0.01 4.0 n14 n16 simu 0.01 0.01 4.0 n14' n16' FMAP 2 PLAN -20 WGHT 0.107000 51.757599 FVAR 0.05816 DY1 7 0.515292 0.769664 0.371557 11.00000 0.04840 0.03167 = 0.02760 0.00331 0.01666 0.00568 DY2 7 0.676029 0.721915 0.503267 11.00000 0.05036 0.04196 = 0.03515 0.01127 0.02434 0.01561 FE1 6 0.224778 0.790926 0.255918 11.00000 0.04233 0.03602 = 0.04051 0.00072 0.01336 -0.00415 FE2 6 0.284623 0.919608 0.283170 11.00000 0.03815 0.03272 = 0.04259 0.00455 0.01119 -0.00095 FE3 6 0.367541 0.818380 0.275428 11.00000 0.04306 0.03495 = 0.02975 0.00157 0.01377 -0.00119 FE4 6 0.807536 0.601297 0.701758 11.00000 0.03469 0.04505 = 0.04593 0.01787 0.01950 0.00586 FE5 6 0.827586 0.734507 0.732892 11.00000 0.04610 0.04604 = 0.03655 0.01237 0.00703 -0.01000 FE6 6 0.804026 0.693625 0.622329 11.00000 0.03558 0.05037 = 0.05236 0.02440 0.02437 0.01233 NA1 5 0.180044 0.879978 0.328266 11.00000 0.04724 0.04586 = 0.10399 -0.01494 0.03827 -0.00689 NA2 5 0.757311 0.646048 0.785151 11.00000 0.07341 0.04816 = 0.04993 0.00685 0.03266 -0.00101 N1 3 0.266003 0.707662 0.281052 11.00000 0.03960 0.03264 = 0.04999 -0.00455 0.01815 -0.00196 N2 3 0.380530 0.957900 0.331692 11.00000 0.04277 0.02970 = 0.04687 0.00428 0.02347 0.00322 N3 3 0.754839 0.552022 0.632227 11.00000 0.04913 0.04766 = 0.04570 0.02347 0.03423 0.02396 N4 3 0.785811 0.811427 0.690932 11.00000 0.04573 0.04558 = 0.03860 -0.00196 0.01349 -0.01774 N5 3 0.142695 0.762053 0.191806 11.00000 0.07991 0.06741 = 0.09570 -0.00033 0.05109 -0.01585 N6 3 0.117088 0.718474 0.190051 11.00000 0.11194 0.11155 = 0.11225 0.00030 0.05829 -0.00043 N7 3 0.087532 0.672062 0.187552 11.00000 0.12469 0.12429 = 0.12519 0.00034 0.06465 -0.00078 N8 3 0.246774 0.990517 0.241506 11.00000 0.04113 0.04892 = 0.08866 0.02516 0.01056 0.00195 PART 1 N9 3 0.206848 1.017329 0.236227 10.70000 0.05374 0.05198 = 0.07488 -0.00437 0.01568 0.00030 N10 3 0.164567 1.049654 0.232691 10.70000 0.08712 0.08695 = 0.08722 -0.00006 0.04565 0.00012 PART 2 N9' 3 0.228002 1.005767 0.200023 10.30000 0.05710 0.05713 = 0.05714 0.00013 0.02999 -0.00011 N10' 3 0.216196 1.016421 0.158430 10.30000 0.13079 0.13083 = 0.13081 0.00011 0.06864 -0.00002 PART 0 N11 3 0.866804 0.534566 0.739651 11.00000 0.04148 0.06108 = 0.07711 0.03830 0.02414 0.01800 N12 3 0.844571 0.487868 0.736150 11.00000 0.05428 0.04960 = 0.10090 0.03670 0.04493 0.01588 N13 3 0.823141 0.443377 0.733486 11.00000 0.08858 0.08814 = 0.08936 0.00112 0.04623 -0.00012 PART 1 N14 3 0.909680 0.770650 0.786900 10.60000 0.06060 0.07028 = 0.05412 0.00496 0.02856 -0.00787 N16 3 0.966909 0.797280 0.875423 10.60000 0.10850 0.12257 = 0.08047 -0.00699 0.04446 -0.01027 PART 2 N14' 3 0.881794 0.779218 0.797834 10.40000 0.07911 0.07918 = 0.07899 0.00036 0.04153 -0.00017 N16' 3 0.993443 0.803607 0.851343 10.40000 0.08344 0.09905 = 0.11052 0.00165 0.03279 -0.00196 PART 0 N15 3 0.936707 0.788781 0.829048 11.00000 0.09376 0.11212 = 0.08566 -0.02435 0.05060 -0.02766 N17 3 0.269527 0.655860 0.949663 11.00000 0.13437 0.12785 = 0.15169 -0.00707 0.06832 -0.00306 N18 3 0.295450 0.850889 0.599650 10.40000 0.09385 0.10616 = 0.16538 0.10948 0.06077 0.03078 N19 3 0.263067 0.613090 0.533673 10.60000 0.13356 0.13946 = 0.10511 -0.02505 0.05555 0.02588 O1 4 0.197154 0.786733 0.306928 11.00000 0.04584 0.03865 = 0.05280 0.00724 0.02709 0.00435 O2 4 0.280510 0.782867 0.223123 11.00000 0.04167 0.04146 = 0.03496 -0.00594 0.01298 -0.00924 O3 4 0.404048 0.747143 0.313774 11.00000 0.05643 0.03146 = 0.03127 -0.00434 0.01890 -0.00437 PART 1 O4 4 0.311384 0.610382 0.203005 10.70000 0.05494 0.04124 = 0.07584 -0.02579 0.04124 -0.01689 AFIX 81 H4 2 0.351875 0.614860 0.218577 10.70000 10.10000 AFIX 0 PART 2 O4' 4 0.213986 0.611914 0.207309 10.30000 0.06690 0.06964 = 0.06043 -0.02950 0.02023 -0.02115 AFIX 81 H4' 2 0.197808 0.619811 0.225193 10.30000 10.10000 AFIX 0 PART 0 O5 4 0.135047 0.806413 0.356141 11.00000 0.06750 0.05033 = 0.08101 0.01153 0.04316 0.01062 O6 4 0.269728 0.936792 0.339960 11.00000 0.03940 0.03346 = 0.05324 -0.00310 0.01744 -0.00069 O7 4 0.331079 0.896181 0.246108 11.00000 0.04416 0.04272 = 0.03399 0.00576 0.01085 -0.00616 O8 4 0.448992 0.849427 0.334805 11.00000 0.04746 0.04170 = 0.02799 -0.00160 0.01454 -0.00206 O9 4 0.494512 0.999714 0.285725 11.00000 0.05852 0.04443 = 0.08206 0.00503 0.03827 -0.00830 AFIX 81 H9 2 0.515930 1.028374 0.288278 11.00000 10.10000 AFIX 0 O10 4 0.208371 0.955744 0.390053 11.00000 0.04398 0.06158 = 0.07130 -0.01110 0.02638 -0.00346 O11 4 0.737497 0.584953 0.715462 11.00000 0.04865 0.04821 = 0.04095 0.00097 0.02565 -0.00842 O12 4 0.853807 0.623785 0.662875 11.00000 0.03667 0.05398 = 0.06056 0.02588 0.02585 0.01357 O13 4 0.733908 0.649910 0.563639 11.00000 0.04774 0.04561 = 0.05153 0.01136 0.03168 0.02045 O14 4 0.728090 0.473305 0.535489 11.00000 0.10892 0.05628 = 0.09116 0.00342 0.06535 0.02483 AFIX 81 H14 2 0.734602 0.442212 0.526352 11.00000 10.10000 AFIX 0 O15 4 0.661510 0.580905 0.755271 11.00000 0.06625 0.05936 = 0.05449 -0.00508 0.04619 -0.01140 O16 4 0.764476 0.736618 0.755980 11.00000 0.08345 0.03645 = 0.04460 0.00626 0.03540 0.00512 O17 4 0.865132 0.739245 0.685569 11.00000 0.03910 0.06268 = 0.05613 0.02732 0.01556 -0.00116 O18 4 0.747084 0.758389 0.585989 11.00000 0.04839 0.03765 = 0.04229 0.01669 0.02482 0.01815 PART 1 O19 4 0.863623 0.905864 0.637301 10.70000 0.11006 0.11018 = 0.11038 0.00032 0.05796 -0.00017 AFIX 81 H19 2 0.898532 0.887737 0.653036 10.70000 10.10000 AFIX 0 PART 2 O19' 4 0.882106 0.907112 0.707997 10.30000 0.05189 0.04452 = 0.04960 -0.00230 0.01864 -0.01681 AFIX 81 H19' 2 0.872495 0.913346 0.730431 10.30000 10.10000 AFIX 0 PART 0 O20 4 0.719679 0.721858 0.818492 11.00000 0.08790 0.04369 = 0.04900 -0.00247 0.04225 -0.00600 O21 4 0.405390 0.810973 0.229221 11.00000 0.05870 0.04586 = 0.02823 0.00221 0.01988 0.00187 O22 4 0.509207 0.781781 0.289968 11.00000 0.05234 0.04510 = 0.03505 0.00082 0.01829 0.00386 O23 4 0.527438 0.676615 0.343059 11.00000 0.07142 0.03716 = 0.04172 -0.00391 0.02362 0.00776 O24 4 0.621166 0.707800 0.411131 11.00000 0.06086 0.04574 = 0.04179 0.00358 0.03407 0.00725 O25 4 0.501526 0.703011 0.424363 11.00000 0.05953 0.03574 = 0.03547 0.01045 0.01877 0.00606 O26 4 0.593807 0.657502 0.484955 11.00000 0.06620 0.04733 = 0.03833 0.00712 0.02199 0.01356 O27 4 0.530826 0.818473 0.445824 11.00000 0.04731 0.04186 = 0.02820 -0.00233 0.01464 0.00593 O28 4 0.604826 0.772656 0.519489 11.00000 0.04897 0.04599 = 0.04018 -0.00257 0.02173 0.00162 O29 4 0.600763 0.834041 0.393047 11.00000 0.06024 0.03769 = 0.03399 0.00353 0.02310 0.01126 O30 4 0.684037 0.809411 0.473511 11.00000 0.05322 0.04339 = 0.03720 0.01222 0.02147 0.01792 O31 4 0.777384 0.711517 0.504590 11.00000 0.07685 0.08253 = 0.06667 0.04224 0.05500 0.03716 O32 4 0.857603 0.700973 0.588046 11.00000 0.05383 0.09029 = 0.08846 0.05643 0.05250 0.03886 O33 4 0.313287 0.835015 0.311893 11.00000 0.04142 0.03128 = 0.03876 0.00256 0.01556 -0.00100 O34 4 0.761657 0.680075 0.668207 11.00000 0.02984 0.03944 = 0.04094 0.00804 0.01696 0.00562 O35 4 0.201283 0.873402 0.241547 11.00000 0.03730 0.04349 = 0.04080 0.00872 0.00816 -0.00124 O36 4 0.857082 0.655709 0.760806 11.00000 0.03567 0.05311 = 0.03964 0.01404 0.00798 0.00266 O37 4 0.073172 0.913527 0.285674 11.00000 0.05203 0.04639 = 0.11923 0.00910 0.03031 0.00244 PART 1 O38 4 0.834733 0.622190 0.872416 10.50000 0.11584 0.10964 = 0.09114 0.01365 0.05635 0.01020 PART 2 O38' 4 0.811130 0.586172 0.856438 10.50000 0.13134 0.11645 = 0.11741 0.00610 0.05813 -0.00066 PART 0 O39 4 -0.009410 0.660407 0.715264 11.00000 0.06150 0.11989 = 0.12535 0.02605 0.03052 0.01961 O40 4 0.010920 0.890480 0.717830 10.65000 0.14017 0.13120 = 0.16025 0.00069 0.07930 -0.01171 O41 4 0.428423 0.905608 0.701403 11.00000 0.06803 0.05468 = 0.14341 0.01544 0.06055 0.00192 O42 4 0.130119 0.573914 0.490400 10.35000 0.13920 0.13897 = 0.13898 -0.00007 0.07292 0.00002 C1 1 0.195694 0.744207 0.336215 11.00000 0.04587 0.04225 = 0.05661 0.00890 0.02177 0.00283 C2 1 0.224745 0.690580 0.340492 11.00000 0.05990 0.04025 = 0.05509 0.00848 0.02665 0.00351 C3 1 0.221083 0.649005 0.371190 11.00000 0.07284 0.04196 = 0.09103 0.01215 0.05448 0.01172 AFIX 41 H3 2 0.239856 0.613540 0.373086 11.00000 10.10000 AFIX 0 C4 1 0.191087 0.657802 0.398828 11.00000 0.10121 0.05179 = 0.11630 0.03240 0.07116 0.02246 AFIX 41 H4A 2 0.190320 0.628767 0.419877 11.00000 10.10000 AFIX 0 C5 1 0.160661 0.711037 0.396056 11.00000 0.10175 0.05375 = 0.09478 0.02247 0.06927 0.01290 AFIX 41 H5 2 0.139575 0.717774 0.414697 11.00000 10.10000 AFIX 0 C6 1 0.164044 0.752636 0.363964 11.00000 0.06795 0.04296 = 0.07108 0.01611 0.03961 0.02000 C7 1 0.260213 0.675667 0.313805 11.00000 0.05258 0.03111 = 0.06591 -0.00030 0.02774 -0.00070 AFIX 41 H7 2 0.280348 0.639983 0.321101 11.00000 10.10000 AFIX 0 C8 1 0.305375 0.686971 0.258541 11.00000 0.05351 0.03794 = 0.05617 -0.00618 0.02144 0.00277 C9 1 0.284859 0.725083 0.210116 11.00000 0.06545 0.04005 = 0.04763 -0.01744 0.02693 -0.01326 AFIX 21 H9A 2 0.317522 0.721960 0.199736 11.00000 10.10000 H9B 2 0.242061 0.712773 0.180536 11.00000 10.10000 AFIX 0 C10 1 0.380799 0.690620 0.298940 11.00000 0.04999 0.02815 = 0.04274 -0.00717 0.01550 -0.01007 AFIX 21 H10A 2 0.391155 0.669279 0.330418 11.00000 10.10000 H10B 2 0.404330 0.672849 0.283860 11.00000 10.10000 AFIX 0 C11 1 0.287971 0.624004 0.238941 11.00000 0.05234 0.04344 = 0.07251 -0.00982 0.03716 -0.00278 AFIX 21 H11A 2 0.308770 0.598444 0.269168 11.00000 10.10000 H11B 2 0.240105 0.618535 0.220619 11.00000 10.10000 AFIX 0 C12 1 0.098610 0.817261 0.381067 11.00000 0.07349 0.06565 = 0.11471 0.00099 0.06437 0.00972 AFIX 31 H12A 2 0.081835 0.855581 0.373475 11.00000 10.10000 H12B 2 0.127329 0.812515 0.418705 11.00000 10.10000 H12C 2 0.062013 0.791027 0.367888 11.00000 10.10000 AFIX 0 C13 1 0.300394 0.969943 0.382486 11.00000 0.04233 0.02984 = 0.04235 0.00158 0.01128 0.01145 C14 1 0.363013 0.994889 0.399517 11.00000 0.04457 0.03343 = 0.06256 -0.01009 0.02127 -0.00943 C15 1 0.392368 1.028673 0.445710 11.00000 0.04376 0.04487 = 0.08047 -0.01260 0.02911 -0.00952 AFIX 41 H15 2 0.434354 1.044154 0.458055 11.00000 10.10000 AFIX 0 C16 1 0.362012 1.039430 0.472695 11.00000 0.05340 0.06165 = 0.06195 -0.01507 0.02954 -0.00843 AFIX 41 H16 2 0.382668 1.062238 0.502852 11.00000 10.10000 AFIX 0 C17 1 0.297911 1.015522 0.454596 11.00000 0.05793 0.04604 = 0.05944 -0.00353 0.03056 0.00265 AFIX 41 H17 2 0.275886 1.022863 0.472406 11.00000 10.10000 AFIX 0 C18 1 0.269381 0.981436 0.410321 11.00000 0.04447 0.03425 = 0.05733 0.00548 0.02305 0.00494 C19 1 0.400944 0.985689 0.374488 11.00000 0.04056 0.03892 = 0.05898 0.00169 0.01948 0.00005 AFIX 41 H19A 2 0.443531 1.001258 0.390896 11.00000 10.10000 AFIX 0 C20 1 0.425576 0.951819 0.311452 11.00000 0.03699 0.03371 = 0.04932 0.00444 0.02033 0.00115 C21 1 0.379041 0.937870 0.252124 11.00000 0.04857 0.03542 = 0.04663 0.01242 0.02005 0.00026 AFIX 21 H21A 2 0.356380 0.972196 0.232773 11.00000 10.10000 H21B 2 0.404912 0.923209 0.237817 11.00000 10.10000 AFIX 0 C22 1 0.476411 0.904185 0.340898 11.00000 0.04583 0.02021 = 0.05272 0.00526 0.02172 -0.00349 AFIX 21 H22A 2 0.507258 0.903325 0.328569 11.00000 10.10000 H22B 2 0.501838 0.913432 0.378384 11.00000 10.10000 AFIX 0 C23 1 0.465397 1.006425 0.317001 11.00000 0.05380 0.03071 = 0.06811 0.00767 0.03380 0.00283 AFIX 21 H23A 2 0.436008 1.039261 0.304922 11.00000 10.10000 H23B 2 0.499914 1.012376 0.353852 11.00000 10.10000 AFIX 0 C24 1 0.173638 0.965105 0.416482 11.00000 0.06927 0.07278 = 0.10945 -0.03005 0.06346 -0.01290 AFIX 31 H24A 2 0.132036 0.944899 0.398434 11.00000 10.10000 H24B 2 0.165270 1.005140 0.416602 11.00000 10.10000 H24C 2 0.200054 0.951626 0.452334 11.00000 10.10000 AFIX 0 C25 1 0.687051 0.548104 0.693092 11.00000 0.04146 0.03509 = 0.04487 0.01041 0.02498 0.00080 C26 1 0.670759 0.514268 0.648815 11.00000 0.04518 0.03665 = 0.04774 0.01147 0.02807 0.00340 C27 1 0.619516 0.474491 0.629969 11.00000 0.07073 0.04167 = 0.05313 -0.00107 0.03797 -0.00472 AFIX 41 H27 2 0.610405 0.451463 0.601367 11.00000 10.10000 AFIX 0 C28 1 0.582027 0.468660 0.653010 11.00000 0.05915 0.05289 = 0.05662 -0.00081 0.03419 -0.01280 AFIX 41 H28 2 0.548721 0.441146 0.640588 11.00000 10.10000 AFIX 0 C29 1 0.594194 0.504437 0.695437 11.00000 0.05519 0.04044 = 0.05334 0.00641 0.03175 -0.00187 AFIX 41 H29 2 0.567914 0.502098 0.710261 11.00000 10.10000 AFIX 0 C30 1 0.646132 0.543107 0.714508 11.00000 0.05157 0.03828 = 0.03468 0.00906 0.02568 0.00351 C31 1 0.705237 0.519377 0.619642 11.00000 0.05641 0.03115 = 0.05688 0.01512 0.03601 0.01202 AFIX 41 H31 2 0.689669 0.496979 0.589482 11.00000 10.10000 AFIX 0 C32 1 0.781927 0.553450 0.597023 11.00000 0.05500 0.06082 = 0.06249 0.02032 0.03937 0.01808 C33 1 0.854129 0.576766 0.631721 11.00000 0.05516 0.05148 = 0.07705 0.02275 0.04645 0.01736 AFIX 21 H33A 2 0.883499 0.546934 0.654871 11.00000 10.10000 H33B 2 0.870257 0.589412 0.609255 11.00000 10.10000 AFIX 0 C34 1 0.738537 0.593047 0.548909 11.00000 0.06899 0.04273 = 0.04906 0.01805 0.03515 0.02393 AFIX 21 H34A 2 0.757282 0.593969 0.526561 11.00000 10.10000 H34B 2 0.694032 0.577117 0.528158 11.00000 10.10000 AFIX 0 C35 1 0.789051 0.495254 0.577318 11.00000 0.08934 0.04910 = 0.08730 0.02255 0.06801 0.02599 AFIX 21 H35A 2 0.820154 0.498532 0.565367 11.00000 10.10000 H35B 2 0.807690 0.468520 0.606656 11.00000 10.10000 AFIX 0 C36 1 0.618355 0.580680 0.775998 11.00000 0.10641 0.08132 = 0.09323 -0.02092 0.08146 -0.01809 AFIX 31 H36A 2 0.634161 0.607899 0.804300 11.00000 10.10000 H36B 2 0.618151 0.543356 0.789203 11.00000 10.10000 H36C 2 0.573935 0.590635 0.748332 11.00000 10.10000 AFIX 0 C37 1 0.732553 0.780103 0.760238 11.00000 0.05522 0.05097 = 0.03274 -0.00313 0.01505 -0.00806 C38 1 0.720650 0.831975 0.731761 11.00000 0.05094 0.03129 = 0.04789 -0.00368 0.00790 -0.00114 C39 1 0.683963 0.874822 0.738948 11.00000 0.07378 0.04384 = 0.06944 0.01598 0.01945 0.00593 AFIX 41 H39 2 0.674687 0.908423 0.719643 11.00000 10.10000 AFIX 0 C40 1 0.662023 0.869484 0.771975 11.00000 0.08597 0.05018 = 0.08293 -0.00145 0.05585 0.00814 AFIX 41 H40 2 0.639220 0.899283 0.776250 11.00000 10.10000 AFIX 0 C41 1 0.673731 0.817954 0.800581 11.00000 0.07139 0.05592 = 0.04723 -0.01914 0.02130 -0.00786 AFIX 41 H41 2 0.658873 0.813671 0.823921 11.00000 10.10000 AFIX 0 C42 1 0.706814 0.774996 0.793547 11.00000 0.06003 0.04968 = 0.03883 -0.01090 0.02147 -0.00528 C43 1 0.745089 0.842641 0.696985 11.00000 0.05836 0.04509 = 0.03735 0.00300 0.00505 -0.02687 AFIX 41 H43 2 0.729851 0.875660 0.676643 11.00000 10.10000 AFIX 0 C44 1 0.808833 0.830463 0.656130 11.00000 0.04552 0.04032 = 0.05472 0.01699 0.01676 -0.01378 C45 1 0.873164 0.796296 0.673593 11.00000 0.04923 0.05229 = 0.06030 0.01881 0.01803 -0.00928 AFIX 21 H45A 2 0.882564 0.796409 0.645399 11.00000 10.10000 H45B 2 0.910449 0.813935 0.704635 11.00000 10.10000 AFIX 0 C46 1 0.755466 0.816542 0.597942 11.00000 0.04811 0.04413 = 0.04255 0.01121 0.01589 -0.00682 AFIX 21 H46A 2 0.713160 0.832275 0.590085 11.00000 10.10000 H46B 2 0.767559 0.835306 0.574985 11.00000 10.10000 AFIX 0 C47 1 0.824800 0.894126 0.660136 11.00000 0.07150 0.07112 = 0.07100 0.00132 0.03714 -0.00156 AFIX 21 H47A 2 0.783662 0.915806 0.641794 11.00000 10.10000 H47B 2 0.849142 0.905658 0.697076 11.00000 10.10000 AFIX 0 C48 1 0.701443 0.714646 0.857186 11.00000 0.11347 0.04896 = 0.05834 -0.00352 0.05539 -0.00567 AFIX 31 H48A 2 0.712402 0.676670 0.871290 11.00000 10.10000 H48B 2 0.654387 0.720759 0.840898 11.00000 10.10000 H48C 2 0.725298 0.741666 0.885350 11.00000 10.10000 AFIX 0 C49 1 0.484572 0.805445 0.204022 11.00000 0.04988 0.04877 = 0.02820 0.00749 0.01227 -0.00223 C50 1 0.444497 0.837062 0.159024 11.00000 0.09861 0.10868 = 0.06282 0.03803 0.04899 0.03632 AFIX 41 H50 2 0.405044 0.853351 0.152819 11.00000 10.10000 AFIX 0 C51 1 0.465479 0.843756 0.122897 11.00000 0.10796 0.10830 = 0.10762 0.00114 0.05667 -0.00011 AFIX 41 H51 2 0.439913 0.865436 0.092448 11.00000 10.10000 AFIX 0 C52 1 0.522993 0.818856 0.131815 11.00000 0.09918 0.09972 = 0.09889 0.00051 0.05247 -0.00007 AFIX 41 H52 2 0.535434 0.823012 0.106947 11.00000 10.10000 AFIX 0 C53 1 0.561206 0.788850 0.175542 11.00000 0.05776 0.09008 = 0.05902 0.01350 0.02828 -0.00470 AFIX 41 H53 2 0.600447 0.772392 0.181458 11.00000 10.10000 AFIX 0 C54 1 0.542446 0.782195 0.212157 11.00000 0.04969 0.06255 = 0.04095 0.00728 0.02153 0.00207 AFIX 41 H54 2 0.569638 0.761516 0.242960 11.00000 10.10000 AFIX 0 C55 1 0.466849 0.798235 0.244807 11.00000 0.04628 0.03074 = 0.03860 -0.00114 0.01296 0.00524 C56 1 0.617664 0.611693 0.380370 11.00000 0.09267 0.03667 = 0.04478 0.00255 0.04729 0.01632 C57 1 0.577005 0.568863 0.347298 11.00000 0.11457 0.04622 = 0.06120 0.00815 0.06194 0.01693 AFIX 41 H57 2 0.531723 0.575543 0.324237 11.00000 10.10000 AFIX 0 C58 1 0.603760 0.515784 0.348478 11.00000 0.08552 0.08467 = 0.08500 -0.00007 0.04471 0.00026 AFIX 41 H58 2 0.576867 0.486306 0.326809 11.00000 10.10000 AFIX 0 C59 1 0.669313 0.508177 0.381650 11.00000 0.12329 0.06472 = 0.08553 -0.00476 0.06007 0.01615 AFIX 41 H59 2 0.687221 0.472614 0.382386 11.00000 10.10000 AFIX 0 C60 1 0.711541 0.549807 0.414587 11.00000 0.11301 0.09156 = 0.06776 0.00354 0.04610 0.04815 AFIX 41 H60 2 0.756750 0.542397 0.437181 11.00000 10.10000 AFIX 0 C61 1 0.685534 0.603453 0.413625 11.00000 0.09261 0.05845 = 0.05862 0.01876 0.04786 0.04254 AFIX 41 H61 2 0.713077 0.632920 0.434777 11.00000 10.10000 AFIX 0 C62 1 0.586988 0.668708 0.377908 11.00000 0.09421 0.03333 = 0.04430 -0.00110 0.05049 -0.00349 C63 1 0.492014 0.634729 0.477972 11.00000 0.05981 0.03280 = 0.03420 -0.00021 0.02304 -0.00005 C64 1 0.426991 0.648758 0.460684 11.00000 0.07556 0.03634 = 0.05105 0.00260 0.03282 0.00692 AFIX 41 H64 2 0.407204 0.679357 0.437627 11.00000 10.10000 AFIX 0 C65 1 0.390042 0.618021 0.477023 11.00000 0.06340 0.05212 = 0.04865 -0.00152 0.03257 0.00204 AFIX 41 H65 2 0.346240 0.628301 0.465016 11.00000 10.10000 AFIX 0 C66 1 0.418857 0.572290 0.511093 11.00000 0.09386 0.05558 = 0.04834 -0.00176 0.04823 -0.00653 AFIX 41 H66 2 0.394622 0.551023 0.521774 11.00000 10.10000 AFIX 0 C67 1 0.483101 0.559120 0.528582 11.00000 0.09580 0.04424 = 0.05490 0.01014 0.03649 -0.00446 AFIX 41 H67 2 0.502454 0.528336 0.551479 11.00000 10.10000 AFIX 0 C68 1 0.520910 0.589212 0.513996 11.00000 0.08167 0.04636 = 0.05901 0.01291 0.03869 0.01327 AFIX 41 H68 2 0.565339 0.579585 0.527828 11.00000 10.10000 AFIX 0 C69 1 0.531376 0.667767 0.460344 11.00000 0.06812 0.03594 = 0.02916 -0.00723 0.02308 -0.00199 C70 1 0.525917 0.833941 0.522453 11.00000 0.04239 0.03430 = 0.02891 -0.00201 0.01389 -0.00109 C71 1 0.472788 0.870181 0.497058 11.00000 0.03040 0.03672 = 0.03769 -0.00892 0.01130 -0.00023 AFIX 41 H71 2 0.455817 0.878863 0.461580 11.00000 10.10000 AFIX 0 C72 1 0.443810 0.894073 0.522229 11.00000 0.04240 0.03929 = 0.06784 -0.01418 0.02393 -0.00067 AFIX 41 H72 2 0.407870 0.918783 0.504002 11.00000 10.10000 AFIX 0 C73 1 0.468424 0.881205 0.575445 11.00000 0.06196 0.06152 = 0.06662 -0.01429 0.04469 0.00342 AFIX 41 H73 2 0.448580 0.896531 0.592806 11.00000 10.10000 AFIX 0 C74 1 0.522626 0.845401 0.601744 11.00000 0.08623 0.08032 = 0.04315 0.00167 0.03603 0.00490 AFIX 41 H74 2 0.539788 0.837096 0.637321 11.00000 10.10000 AFIX 0 C75 1 0.552517 0.821140 0.575666 11.00000 0.05105 0.05596 = 0.03832 0.00165 0.02190 0.02039 AFIX 41 H75 2 0.589189 0.797126 0.593664 11.00000 10.10000 AFIX 0 C76 1 0.555261 0.806480 0.493126 11.00000 0.04241 0.03873 = 0.03400 -0.00313 0.01686 -0.00422 C77 1 0.694766 0.895503 0.438163 11.00000 0.05359 0.04219 = 0.03738 -0.00516 0.02867 -0.00741 C78 1 0.661055 0.942597 0.406619 11.00000 0.07439 0.03132 = 0.03819 0.00082 0.01893 -0.00403 AFIX 41 H78 2 0.615115 0.941882 0.383267 11.00000 10.10000 AFIX 0 C79 1 0.698296 0.990685 0.411175 11.00000 0.08744 0.04396 = 0.07829 0.01805 0.02314 -0.00424 AFIX 41 H79 2 0.676173 1.022464 0.390632 11.00000 10.10000 AFIX 0 C80 1 0.764713 0.993232 0.443895 11.00000 0.08010 0.06702 = 0.06847 -0.00832 0.03202 -0.02892 AFIX 41 H80 2 0.788091 1.026015 0.445842 11.00000 10.10000 AFIX 0 C81 1 0.797889 0.945848 0.474845 11.00000 0.06896 0.09256 = 0.06792 -0.02062 0.03790 -0.01237 AFIX 41 H81 2 0.843949 0.946973 0.497520 11.00000 10.10000 AFIX 0 C82 1 0.763540 0.897316 0.472399 11.00000 0.05303 0.05494 = 0.05226 -0.00801 0.02214 0.00421 AFIX 41 H82 2 0.786169 0.865991 0.493485 11.00000 10.10000 AFIX 0 C83 1 0.656968 0.843187 0.434785 11.00000 0.05483 0.03321 = 0.04453 0.00502 0.02960 0.01404 AFIX 66 PART 1 C84 1 0.895393 0.719067 0.531369 10.65000 0.07070 0.15788 = 0.11038 0.01655 0.07070 0.00993 C85 1 0.877151 0.722845 0.478587 10.65000 0.07354 0.16064 = 0.11338 0.01427 0.07030 0.01019 AFIX 41 H85 2 0.832321 0.723054 0.451879 10.65000 10.10000 AFIX 65 C86 1 0.925914 0.726313 0.465724 10.65000 0.07831 0.16360 = 0.11506 0.01508 0.06906 0.01035 AFIX 41 H86 2 0.913708 0.728841 0.430409 10.65000 10.10000 AFIX 65 C87 1 0.992919 0.726001 0.505642 10.65000 0.07699 0.16281 = 0.11642 0.01559 0.06679 0.00887 AFIX 41 H87 2 1.025544 0.728321 0.497036 10.65000 10.10000 AFIX 65 C88 1 1.011161 0.722223 0.558425 10.65000 0.07412 0.16143 = 0.11572 0.01315 0.06694 0.01102 AFIX 41 H88 2 1.055992 0.722014 0.585133 10.65000 10.10000 AFIX 65 C89 1 0.962399 0.718756 0.571289 10.65000 0.06965 0.15747 = 0.11138 0.01546 0.07192 0.00844 AFIX 41 H89 2 0.974605 0.716228 0.606604 10.65000 10.10000 AFIX 66 PART 2 C84' 1 0.867015 0.669823 0.511451 10.35000 0.08966 0.13940 = 0.10600 -0.02152 0.07317 0.02316 C85' 1 0.840722 0.663221 0.457378 10.35000 0.09189 0.14118 = 0.10640 -0.02060 0.07321 0.02207 AFIX 41 H85' 2 0.796838 0.673681 0.433241 10.35000 10.10000 AFIX 65 C86' 1 0.880017 0.640985 0.439382 10.35000 0.09184 0.14246 = 0.10647 -0.02178 0.07414 0.02331 AFIX 41 H86' 2 0.862424 0.636568 0.403204 10.35000 10.10000 AFIX 65 C87' 1 0.945606 0.625351 0.475458 10.35000 0.09169 0.14268 = 0.10670 -0.02122 0.07260 0.02306 AFIX 41 H87' 2 0.971897 0.610474 0.463416 10.35000 10.10000 AFIX 65 C88' 1 0.971900 0.631953 0.529530 10.35000 0.09089 0.14272 = 0.10947 -0.02175 0.07161 0.02555 AFIX 41 H88' 2 1.015784 0.621493 0.553667 10.35000 10.10000 AFIX 65 C89' 1 0.932606 0.654190 0.547527 10.35000 0.09002 0.14168 = 0.10625 -0.02132 0.07405 0.02411 AFIX 41 H89' 2 0.950199 0.658607 0.583705 10.35000 10.10000 AFIX 0 PART 0 part 1 C90 1 0.844115 0.712151 0.546474 10.65000 0.05565 0.05886 = 0.06247 0.00234 0.03576 -0.00266 part 2 C90' 1 0.826901 0.693691 0.530998 10.35000 0.04043 0.03705 = 0.02169 0.00414 0.01885 0.00676 PART 0 C91 1 0.345890 0.821213 0.367456 11.00000 0.05179 0.04785 = 0.02717 0.00473 0.02079 0.00239 AFIX 31 H91A 2 0.316813 0.830180 0.380055 11.00000 10.10000 H91B 2 0.386225 0.842981 0.386938 11.00000 10.10000 H91C 2 0.356349 0.781284 0.372384 11.00000 10.10000 AFIX 0 C92 1 0.689748 0.685712 0.641227 11.00000 0.02522 0.04521 = 0.04292 0.00970 0.01258 0.00489 AFIX 31 H92A 2 0.675681 0.678065 0.665731 11.00000 10.10000 H92B 2 0.668980 0.659026 0.612411 11.00000 10.10000 H92C 2 0.677021 0.723772 0.627695 11.00000 10.10000 AFIX 0 C93 1 0.140063 0.894451 0.198176 11.00000 0.05912 0.06715 = 0.06994 -0.00385 0.01178 -0.02588 AFIX 31 H93A 2 0.139789 0.935328 0.199610 11.00000 10.10000 H93B 2 0.103562 0.879568 0.200268 11.00000 10.10000 H93C 2 0.135592 0.882637 0.165432 11.00000 10.10000 AFIX 0 C94 1 0.923449 0.643398 0.805467 11.00000 0.05624 0.07557 = 0.05836 0.02416 0.00737 0.00931 AFIX 31 H94A 2 0.938958 0.674958 0.829699 11.00000 10.10000 H94B 2 0.953207 0.637383 0.792963 11.00000 10.10000 H94C 2 0.922063 0.609714 0.823268 11.00000 10.10000 AFIX 0 C95 1 0.048669 0.968363 0.270731 11.00000 0.10693 0.11122 = 0.13471 0.00405 0.06024 -0.00156 AFIX 31 H95A 2 0.000893 0.967669 0.252546 11.00000 10.10000 H95B 2 0.062038 0.983472 0.247589 11.00000 10.10000 H95C 2 0.066083 0.991980 0.301694 11.00000 10.10000 AFIX 0 part 1 C96 1 0.883938 0.645252 0.921117 10.50000 0.13520 0.15097 = 0.15155 -0.00238 0.08499 -0.00136 AFIX 31 H96A 2 0.903501 0.615414 0.947072 10.50000 10.10000 H96B 2 0.864239 0.673151 0.932492 10.50000 10.10000 H96C 2 0.917789 0.662992 0.917156 10.50000 10.10000 AFIX 0 part 2 C96' 1 0.810178 0.525962 0.846365 10.50000 0.11895 0.12483 = 0.10954 0.01065 0.06245 0.00236 AFIX 31 H96D 2 0.839808 0.506508 0.878990 10.50000 10.10000 H96E 2 0.824348 0.519708 0.821727 10.50000 10.10000 H96F 2 0.765745 0.511567 0.831670 10.50000 10.10000 AFIX 0 part 0 C97 1 0.013997 0.717736 0.725164 11.00000 0.07832 0.09656 = 0.11271 0.02465 0.04339 -0.00011 C98 1 0.040962 0.886758 0.778021 10.65000 0.09557 0.09689 = 0.10747 0.00256 0.04243 -0.00882 C99 1 0.459603 0.852028 0.708166 11.00000 0.08699 0.04065 = 0.08433 0.01241 0.05250 0.01280 C100 1 0.302942 0.693815 0.973304 11.00000 0.13416 0.12770 = 0.15158 -0.00698 0.06849 -0.00322 C101 1 0.346967 0.739316 0.998375 11.00000 0.13431 0.12770 = 0.15163 -0.00701 0.06841 -0.00325 C102 1 0.238466 0.863032 0.598358 10.40000 0.09374 0.10602 = 0.16516 0.10956 0.06092 0.03080 C103 1 0.180651 0.885732 0.600734 10.40000 0.09378 0.10609 = 0.16518 0.10956 0.06086 0.03083 C104 1 0.262707 0.632751 0.575283 10.60000 0.13361 0.13947 = 0.10515 -0.02515 0.05537 0.02587 C105 1 0.246476 0.649270 0.614870 10.60000 0.13368 0.13947 = 0.10500 -0.02524 0.05540 0.02585 C106 1 0.070296 0.596683 0.475912 10.35000 0.10803 0.11239 = 0.11508 -0.00230 0.05588 0.00828 HKLF 4 REM sad in P2(1)/c REM R1 = 0.0790 for 16612 Fo > 4sig(Fo) and 0.1185 for all 24395 data REM 1705 parameters refined using 488 restraints END ; #======================END data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 857519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C98 H110 Dy2 Fe6 N16 Na2 O34' _chemical_formula_sum 'C98 H110 Dy2 Fe6 N16 Na2 O34' _chemical_formula_weight 2762.10 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' Na Na 0.0362 0.0249 '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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7815(5) _cell_length_b 35.7632(15) _cell_length_c 17.0680(6) _cell_angle_alpha 90.00 _cell_angle_beta 126.198(2) _cell_angle_gamma 90.00 _cell_volume 6296.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 8.17 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour 'black brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 1.925 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5557 _exptl_absorpt_correction_T_max 0.6118 _exptl_absorpt_process_details SADA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 33715 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 8.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10664 _reflns_number_gt 8386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+46.3618P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10664 _refine_ls_number_parameters 772 _refine_ls_number_restraints 162 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_restrained_S_all 1.316 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 1.51232(4) 0.974147(12) 1.40031(3) 0.03392(14) Uani 1 1 d . . . Fe1 Fe 1.53597(12) 0.92430(3) 1.24311(9) 0.0329(3) Uani 1 1 d . A . Fe2 Fe 1.43889(17) 0.84141(4) 1.17155(11) 0.0551(4) Uani 1 1 d . A . Fe3 Fe 1.74547(15) 0.86161(4) 1.29927(11) 0.0505(4) Uani 1 1 d . A . Na1 Na 1.6650(8) 0.77154(15) 1.3151(5) 0.108(2) Uani 1 1 d . . . O1 O 1.4524(10) 0.7975(2) 1.2432(7) 0.080(3) Uani 1 1 d . A . O2 O 1.4118(6) 0.89423(17) 1.1230(4) 0.0413(15) Uani 1 1 d . . . O3 O 1.4105(6) 0.93166(17) 1.2718(4) 0.0366(13) Uani 1 1 d . . . O4 O 1.5183(15) 0.7333(3) 1.3286(9) 0.124(5) Uani 1 1 d . A . O5 O 1.8067(9) 0.8228(2) 1.3971(7) 0.073(2) Uani 1 1 d . A . O6 O 1.6540(5) 0.94862(17) 1.3710(4) 0.0339(13) Uani 1 1 d . . . O7 O 1.6775(6) 0.91117(17) 1.2306(4) 0.0398(14) Uani 1 1 d . . . O8 O 1.8474(14) 0.7598(4) 1.4850(11) 0.144(5) Uani 1 1 d . A . O9 O 1.789(3) 0.7300(9) 1.300(3) 0.112(10) Uani 0.35 1 d PU A 1 O9' O 1.623(8) 0.718(2) 1.217(6) 0.11(2) Uani 0.15 1 d PU A 2 O10 O 1.5836(6) 0.87012(16) 1.3026(4) 0.0415(15) Uani 1 1 d . . . O11 O 1.6062(9) 0.8290(2) 1.1896(6) 0.065(2) Uani 1 1 d . A . O12 O 1.5469(6) 1.03470(18) 1.4529(4) 0.0480(16) Uani 1 1 d . . . O13 O 1.5397(7) 1.07671(19) 1.5428(5) 0.0531(17) Uani 1 1 d . . . O14 O 1.7057(6) 0.9707(2) 1.5577(4) 0.0466(15) Uani 1 1 d . . . O15 O 1.6950(6) 1.00820(19) 1.6575(4) 0.0434(15) Uani 1 1 d . . . O16 O 1.4957(6) 0.97270(18) 1.1704(4) 0.0418(14) Uani 1 1 d . . . O17 O 1.4632(7) 1.00828(17) 1.2627(4) 0.0450(16) Uani 1 1 d . . . N1 N 1.3204(14) 0.8194(4) 1.0367(10) 0.100(4) Uani 1 1 d DU . . N2 N 1.307(3) 0.8404(9) 0.962(2) 0.108(6) Uani 0.50 1 d PU A 1 N3 N 1.309(3) 0.8600(8) 0.897(2) 0.105(6) Uani 0.50 1 d PU A 1 N2' N 1.245(3) 0.7956(6) 1.024(2) 0.113(6) Uani 0.50 1 d PDU A 2 N3' N 1.185(3) 0.7627(7) 1.025(2) 0.138(8) Uani 0.50 1 d PDU A 2 N4 N 1.8764(12) 0.8519(4) 1.2731(10) 0.092(3) Uani 1 1 d DU . . N5 N 1.902(3) 0.8540(7) 1.224(2) 0.094(5) Uani 0.65 1 d PU A 1 N6 N 1.923(3) 0.8566(8) 1.167(2) 0.118(6) Uani 0.65 1 d PU A 1 N5' N 1.925(6) 0.8656(14) 1.240(4) 0.094(7) Uani 0.35 1 d PDU A 2 N6' N 1.981(4) 0.8802(11) 1.214(3) 0.099(7) Uani 0.35 1 d PDU A 2 N7 N 1.2838(9) 0.8596(3) 1.1763(6) 0.056(2) Uani 1 1 d . . . N8 N 1.8648(7) 0.9000(2) 1.4133(6) 0.046(2) Uani 1 1 d . . . C1 C 1.3827(10) 0.7860(2) 1.2750(7) 0.081(4) Uani 1 1 d G . . C2 C 1.2848(10) 0.8068(2) 1.2669(6) 0.081(4) Uani 1 1 d GU A . C3 C 1.2230(9) 0.7932(3) 1.3062(7) 0.091(4) Uani 1 1 d GU A . H3 H 1.1575 0.8071 1.3008 0.100 Uiso 1 1 calc . . . C4 C 1.2592(11) 0.7589(3) 1.3535(7) 0.104(4) Uani 1 1 d GU A . H4 H 1.2178 0.7498 1.3797 0.100 Uiso 1 1 calc . . . C5 C 1.3570(11) 0.7382(2) 1.3615(7) 0.107(5) Uani 1 1 d GU A . H5 H 1.3812 0.7152 1.3932 0.100 Uiso 1 1 calc . . . C6 C 1.4188(10) 0.7517(2) 1.3223(8) 0.103(5) Uani 1 1 d GU A . C7 C 1.2408(12) 0.8422(3) 1.2167(9) 0.065(3) Uani 1 1 d . A . H7 H 1.1731 0.8537 1.2136 0.100 Uiso 1 1 calc . . . C8 C 1.2278(10) 0.8970(3) 1.1298(8) 0.054(3) Uani 1 1 d . A . C9 C 1.2805(9) 0.9053(3) 1.0707(7) 0.050(2) Uani 1 1 d . A . H9A H 1.2294 0.8919 1.0095 0.100 Uiso 1 1 calc . . . H9B H 1.2732 0.9318 1.0567 0.100 Uiso 1 1 calc . . . C10 C 1.2748(10) 0.9261(3) 1.2098(8) 0.052(3) Uani 1 1 d . A . H10A H 1.2336 0.9498 1.1797 0.100 Uiso 1 1 calc . . . H10B H 1.2463 0.9186 1.2490 0.100 Uiso 1 1 calc . . . C11 C 1.0778(12) 0.8978(4) 1.0632(9) 0.077(4) Uani 1 1 d . . . H11A H 1.0469 0.8754 1.0234 0.100 Uiso 1 1 calc . . . H11B H 1.0479 0.8967 1.1038 0.100 Uiso 1 1 calc . . . C12 C 1.0180(16) 0.9307(7) 0.9985(14) 0.122(6) Uani 1 1 d . A . H12A H 0.9253 0.9288 0.9607 0.100 Uiso 1 1 calc . . . H12B H 1.0438 0.9315 0.9559 0.100 Uiso 1 1 calc . . . H12C H 1.0461 0.9531 1.0369 0.100 Uiso 1 1 calc . . . C13 C 1.541(2) 0.6948(7) 1.3585(18) 0.147(7) Uani 1 1 d U . . H13A H 1.4618 0.6810 1.3184 0.100 Uiso 1 1 calc . . . H13B H 1.5715 0.6932 1.4251 0.100 Uiso 1 1 calc . . . H13C H 1.6051 0.6846 1.3522 0.100 Uiso 1 1 calc . . . C14 C 1.8948(14) 0.8246(4) 1.4945(11) 0.081(3) Uani 1 1 d U . . C15 C 1.9604(13) 0.8564(4) 1.5471(10) 0.079(3) Uani 1 1 d U A . C16 C 2.0475(15) 0.8535(5) 1.6486(12) 0.102(4) Uani 1 1 d U . . H16 H 2.0901 0.8748 1.6852 0.100 Uiso 1 1 calc . . . C17 C 2.0709(19) 0.8199(6) 1.6947(14) 0.129(5) Uani 1 1 d U A . H17 H 2.1299 0.8186 1.7619 0.100 Uiso 1 1 calc . . . C18 C 2.007(2) 0.7881(6) 1.6420(15) 0.134(5) Uani 1 1 d U . . H18 H 2.0275 0.7651 1.6735 0.100 Uiso 1 1 calc . . . C19 C 1.9170(18) 0.7900(6) 1.5458(14) 0.112(5) Uani 1 1 d U A . C20 C 1.9424(10) 0.8924(3) 1.5042(8) 0.056(3) Uani 1 1 d . A . H20 H 1.9913 0.9120 1.5460 0.100 Uiso 1 1 calc . . . C21 C 1.8546(9) 0.9398(3) 1.3811(7) 0.039(2) Uani 1 1 d . A . C22 C 1.7790(9) 0.9382(3) 1.2691(7) 0.043(2) Uani 1 1 d . A . H22A H 1.7427 0.9625 1.2413 0.100 Uiso 1 1 calc . . . H22B H 1.8373 0.9313 1.2527 0.100 Uiso 1 1 calc . . . C23 C 1.7801(9) 0.9624(3) 1.4091(7) 0.042(2) Uani 1 1 d . A . H23A H 1.8304 0.9630 1.4794 0.100 Uiso 1 1 calc . . . H23B H 1.7722 0.9879 1.3870 0.100 Uiso 1 1 calc . . . C24 C 1.9874(10) 0.9586(3) 1.4262(8) 0.059(3) Uani 1 1 d . . . H24A H 1.9724 0.9828 1.3956 0.100 Uiso 1 1 calc . . . H24B H 2.0273 0.9630 1.4944 0.100 Uiso 1 1 calc . . . C25 C 2.0830(11) 0.9374(4) 1.4180(10) 0.077(4) Uani 1 1 d . A . H25A H 2.1624 0.9513 1.4493 0.100 Uiso 1 1 calc . . . H25B H 2.0472 0.9340 1.3507 0.100 Uiso 1 1 calc . . . H25C H 2.1002 0.9135 1.4487 0.100 Uiso 1 1 calc . . . C26 C 1.872(6) 0.7260(17) 1.552(4) 0.131(19) Uani 0.50 1 d PU A 1 C26' C 1.900(6) 0.7198(14) 1.516(4) 0.139(19) Uani 0.50 1 d PU A 2 C27 C 1.5945(11) 0.8637(3) 1.3907(7) 0.052(3) Uani 1 1 d . A . H27A H 1.6147 0.8379 1.4090 0.100 Uiso 1 1 calc . . . H27B H 1.5138 0.8698 1.3799 0.100 Uiso 1 1 calc . . . H27C H 1.6621 0.8792 1.4417 0.100 Uiso 1 1 calc . . . C28 C 1.6103(18) 0.8136(4) 1.1158(12) 0.094(5) Uani 1 1 d . . . H28A H 1.5327 0.7995 1.0721 0.100 Uiso 1 1 calc . . . H28B H 1.6843 0.7975 1.1440 0.100 Uiso 1 1 calc . . . H28C H 1.6169 0.8334 1.0808 0.100 Uiso 1 1 calc . . . C30 C 1.6092(10) 1.0970(3) 1.4486(7) 0.045(2) Uani 1 1 d . . . C31 C 1.6566(15) 1.1308(3) 1.4981(10) 0.076(4) Uani 1 1 d . A . H31 H 1.6574 1.1353 1.5521 0.100 Uiso 1 1 calc . . . C32 C 1.7025(16) 1.1577(5) 1.4671(12) 0.093(4) Uani 1 1 d U . . H32 H 1.7331 1.1803 1.5000 0.100 Uiso 1 1 calc . . . C33 C 1.7029(19) 1.1511(5) 1.3889(13) 0.103(5) Uani 1 1 d . A . H33 H 1.7354 1.1691 1.3691 0.100 Uiso 1 1 calc . . . C34 C 1.6559(16) 1.1182(5) 1.3394(11) 0.086(4) Uani 1 1 d . . . H34 H 1.6562 1.1138 1.2858 0.100 Uiso 1 1 calc . . . C35 C 1.6084(11) 1.0916(3) 1.3683(8) 0.055(3) Uani 1 1 d . A . H35 H 1.5751 1.0695 1.3332 0.100 Uiso 1 1 calc . . . C36 C 1.5633(8) 1.0674(3) 1.4830(6) 0.039(2) Uani 1 1 d . A . C37 C 1.8990(9) 0.9827(3) 1.7140(6) 0.044(2) Uani 1 1 d . . . C38 C 1.9650(11) 1.0077(4) 1.7897(8) 0.067(3) Uani 1 1 d . A . H38 H 1.9201 1.0271 1.7937 0.100 Uiso 1 1 calc . . . C39 C 2.0993(12) 1.0042(5) 1.8611(10) 0.089(4) Uani 1 1 d . . . H39 H 2.1436 1.0218 1.9107 0.100 Uiso 1 1 calc . . . C40 C 2.1628(11) 0.9753(6) 1.8569(10) 0.086(4) Uani 1 1 d . A . H40 H 2.2510 0.9723 1.9053 0.100 Uiso 1 1 calc . . . C41 C 2.0997(13) 0.9507(5) 1.7831(12) 0.093(5) Uani 1 1 d . . . H41 H 2.1452 0.9310 1.7809 0.100 Uiso 1 1 calc . . . C42 C 1.9665(11) 0.9542(4) 1.7096(8) 0.066(3) Uani 1 1 d . A . H42 H 1.9246 0.9373 1.6583 0.100 Uiso 1 1 calc . . . C43 C 1.7546(8) 0.9874(3) 1.6373(6) 0.038(2) Uani 1 1 d . A . C44 C 1.4326(9) 1.0351(2) 1.1242(6) 0.038(2) Uani 1 1 d . . . C45 C 1.3557(11) 1.0641(3) 1.1164(8) 0.058(3) Uani 1 1 d . A . H45 H 1.3272 1.0646 1.1554 0.100 Uiso 1 1 calc . . . C46 C 1.3207(13) 1.0930(3) 1.0491(9) 0.074(4) Uani 1 1 d . . . H46 H 1.2690 1.1127 1.0433 0.100 Uiso 1 1 calc . . . C47 C 1.3638(16) 1.0918(4) 0.9924(9) 0.081(4) Uani 1 1 d . A . H47 H 1.3384 1.1105 0.9466 0.100 Uiso 1 1 calc . . . C48 C 1.4409(16) 1.0647(4) 1.0007(10) 0.083(4) Uani 1 1 d . . . H48 H 1.4726 1.0652 0.9637 0.100 Uiso 1 1 calc . . . C49 C 1.4737(11) 1.0354(3) 1.0652(7) 0.057(3) Uani 1 1 d . A . H49 H 1.5240 1.0158 1.0687 0.100 Uiso 1 1 calc . . . C50 C 1.4680(8) 1.0036(2) 1.1914(6) 0.035(2) Uani 1 1 d . A . O1W O 0.729(3) 0.6729(8) 0.194(2) 0.078(8) Uani 0.30 1 d PU . . O2W O 0.977(4) 0.7710(11) 0.339(3) 0.070(11) Uani 0.20 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0340(2) 0.0429(2) 0.0304(2) 0.0025(2) 0.02202(17) 0.0059(2) Fe1 0.0372(7) 0.0331(6) 0.0345(6) 0.0034(5) 0.0246(6) 0.0046(5) Fe2 0.0825(11) 0.0428(8) 0.0577(9) -0.0085(7) 0.0512(9) -0.0075(8) Fe3 0.0689(10) 0.0429(8) 0.0622(9) 0.0118(7) 0.0510(8) 0.0194(7) Na1 0.175(6) 0.051(3) 0.134(5) 0.010(3) 0.110(5) 0.012(3) O1 0.129(8) 0.045(4) 0.095(6) -0.006(4) 0.082(6) -0.008(5) O2 0.052(4) 0.046(4) 0.035(3) -0.001(3) 0.031(3) -0.001(3) O3 0.041(3) 0.046(4) 0.030(3) -0.002(3) 0.025(3) -0.005(3) O4 0.190(13) 0.042(5) 0.112(8) 0.013(5) 0.073(9) -0.028(6) O5 0.099(6) 0.050(4) 0.089(6) 0.030(4) 0.065(6) 0.029(4) O6 0.031(3) 0.050(4) 0.030(3) 0.004(3) 0.024(3) 0.009(3) O7 0.049(4) 0.044(4) 0.045(4) 0.005(3) 0.039(3) 0.007(3) O8 0.143(11) 0.088(8) 0.149(11) 0.079(9) 0.059(9) 0.031(8) O9 0.114(13) 0.101(13) 0.125(13) -0.020(9) 0.073(9) 0.017(9) O9' 0.11(2) 0.11(2) 0.11(2) 0.000(10) 0.067(15) 0.001(10) O10 0.062(4) 0.037(3) 0.042(3) 0.006(3) 0.040(3) 0.006(3) O11 0.102(6) 0.048(4) 0.072(5) -0.002(4) 0.067(5) 0.008(4) O12 0.055(4) 0.044(4) 0.037(3) 0.001(3) 0.023(3) 0.003(3) O13 0.074(5) 0.056(4) 0.053(4) -0.002(3) 0.050(4) -0.004(4) O14 0.040(3) 0.063(4) 0.035(3) 0.000(3) 0.022(3) 0.013(3) O15 0.030(3) 0.067(4) 0.036(3) -0.004(3) 0.021(3) 0.008(3) O16 0.056(4) 0.043(3) 0.036(3) 0.001(3) 0.033(3) 0.009(3) O17 0.067(4) 0.045(4) 0.036(3) 0.008(3) 0.038(3) 0.017(3) N1 0.127(9) 0.107(9) 0.099(8) -0.050(7) 0.084(7) -0.036(7) N2 0.130(10) 0.108(11) 0.101(10) -0.042(9) 0.077(9) -0.012(9) N3 0.131(12) 0.114(13) 0.090(11) -0.033(10) 0.076(10) 0.001(11) N2' 0.139(11) 0.125(12) 0.110(9) -0.065(9) 0.092(9) -0.048(9) N3' 0.155(14) 0.142(14) 0.123(12) -0.069(12) 0.085(11) -0.056(11) N4 0.104(8) 0.100(8) 0.127(9) 0.013(7) 0.098(7) 0.030(6) N5 0.103(9) 0.111(11) 0.126(11) 0.017(9) 0.100(8) 0.031(8) N6 0.118(11) 0.130(12) 0.139(13) 0.020(11) 0.094(10) 0.024(10) N5' 0.105(11) 0.107(12) 0.128(12) 0.016(10) 0.100(10) 0.030(10) N6' 0.109(13) 0.115(15) 0.131(14) 0.015(13) 0.103(11) 0.022(12) N7 0.061(5) 0.065(6) 0.052(5) -0.016(4) 0.039(5) -0.024(5) N8 0.042(4) 0.057(5) 0.050(5) 0.017(4) 0.034(4) 0.023(4) C1 0.125(12) 0.044(7) 0.070(8) -0.017(6) 0.056(9) -0.046(8) C2 0.108(8) 0.083(8) 0.062(6) -0.026(6) 0.055(6) -0.053(7) C3 0.113(8) 0.097(7) 0.071(6) -0.017(5) 0.059(6) -0.057(6) C4 0.122(8) 0.102(8) 0.080(6) -0.002(6) 0.056(6) -0.061(7) C5 0.129(9) 0.086(8) 0.082(7) 0.002(6) 0.050(7) -0.052(7) C6 0.130(10) 0.072(8) 0.077(8) -0.005(7) 0.045(8) -0.043(8) C7 0.078(8) 0.064(7) 0.067(7) -0.025(6) 0.051(7) -0.037(6) C8 0.047(6) 0.068(7) 0.050(6) -0.014(5) 0.030(5) -0.009(5) C9 0.040(5) 0.073(7) 0.041(5) -0.002(5) 0.027(5) 0.002(5) C10 0.042(5) 0.065(7) 0.054(6) -0.006(5) 0.031(5) -0.004(5) C11 0.056(7) 0.108(11) 0.061(8) -0.023(8) 0.032(6) -0.023(7) C12 0.074(10) 0.173(19) 0.099(12) 0.012(13) 0.039(9) 0.015(11) C13 0.147(7) 0.146(7) 0.147(7) 0.0003(10) 0.087(4) -0.0003(10) C14 0.079(6) 0.085(7) 0.088(7) 0.056(6) 0.053(6) 0.036(5) C15 0.074(6) 0.097(7) 0.080(6) 0.047(6) 0.052(5) 0.034(5) C16 0.089(7) 0.113(8) 0.084(7) 0.052(6) 0.041(6) 0.029(6) C17 0.111(8) 0.126(8) 0.092(8) 0.062(7) 0.028(7) 0.018(7) C18 0.116(8) 0.115(8) 0.103(8) 0.070(7) 0.027(7) 0.016(7) C19 0.098(7) 0.096(7) 0.102(7) 0.060(7) 0.037(6) 0.025(7) C20 0.051(6) 0.070(7) 0.053(6) 0.016(6) 0.035(5) 0.021(5) C21 0.039(5) 0.042(5) 0.044(5) 0.005(4) 0.030(4) 0.006(4) C22 0.046(5) 0.051(6) 0.046(5) 0.010(4) 0.035(5) 0.007(4) C23 0.036(5) 0.046(5) 0.048(5) 0.000(4) 0.027(4) 0.003(4) C24 0.039(5) 0.076(8) 0.066(7) 0.010(6) 0.033(5) 0.009(5) C25 0.050(7) 0.096(10) 0.097(10) 0.025(8) 0.051(7) 0.025(6) C26 0.14(3) 0.11(3) 0.13(3) 0.06(3) 0.07(3) 0.02(2) C26' 0.20(4) 0.07(2) 0.15(3) 0.07(2) 0.11(3) 0.05(2) C27 0.080(7) 0.047(6) 0.049(6) 0.009(5) 0.050(6) 0.002(5) C28 0.142(14) 0.066(9) 0.098(11) -0.017(8) 0.085(11) 0.003(9) C30 0.056(6) 0.046(6) 0.044(5) 0.008(4) 0.037(5) 0.006(5) C31 0.118(11) 0.060(7) 0.088(9) -0.016(7) 0.082(9) -0.033(7) C32 0.094(4) 0.093(4) 0.093(4) 0.0004(10) 0.055(3) -0.0010(10) C33 0.153(15) 0.086(10) 0.111(12) -0.007(9) 0.101(12) -0.049(10) C34 0.112(11) 0.106(11) 0.086(9) 0.009(9) 0.083(9) -0.015(9) C35 0.063(7) 0.068(7) 0.053(6) 0.007(5) 0.044(6) -0.009(5) C36 0.026(4) 0.049(6) 0.023(4) 0.008(4) 0.005(4) 0.006(4) C37 0.038(5) 0.059(6) 0.035(5) 0.007(4) 0.022(4) 0.008(4) C38 0.044(6) 0.090(9) 0.054(7) -0.015(6) 0.022(5) 0.003(6) C39 0.044(7) 0.123(12) 0.064(8) -0.018(8) 0.013(6) -0.003(8) C40 0.035(6) 0.134(13) 0.066(8) 0.013(9) 0.017(6) 0.017(8) C41 0.055(8) 0.115(12) 0.082(10) 0.014(9) 0.025(8) 0.042(8) C42 0.047(6) 0.092(9) 0.048(6) 0.004(6) 0.022(5) 0.028(6) C43 0.034(5) 0.049(5) 0.033(5) 0.008(4) 0.022(4) 0.005(4) C44 0.051(5) 0.030(5) 0.032(5) 0.005(4) 0.024(4) 0.008(4) C45 0.068(7) 0.053(6) 0.052(6) 0.009(5) 0.034(6) 0.020(5) C46 0.080(9) 0.061(7) 0.066(8) 0.026(6) 0.034(7) 0.034(6) C47 0.116(11) 0.068(8) 0.059(8) 0.031(6) 0.051(8) 0.015(8) C48 0.125(12) 0.079(9) 0.068(8) 0.031(7) 0.070(9) 0.021(9) C49 0.077(7) 0.065(7) 0.044(5) 0.011(5) 0.044(6) 0.008(6) C50 0.044(5) 0.039(5) 0.031(4) 0.008(4) 0.026(4) 0.013(4) O1W 0.091(11) 0.067(11) 0.074(11) -0.001(8) 0.048(8) 0.015(8) O2W 0.069(13) 0.066(14) 0.076(14) 0.000(9) 0.043(10) 0.013(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O12 2.285(7) . ? Dy1 O15 2.304(6) 3_878 ? Dy1 O6 2.331(5) . ? Dy1 O3 2.332(6) . ? Dy1 O13 2.336(7) 3_878 ? Dy1 O14 2.345(6) . ? Dy1 O17 2.378(6) . ? Dy1 Fe1 3.3803(12) . ? Fe1 O3 1.952(6) . ? Fe1 O6 1.977(6) . ? Fe1 O7 2.000(6) . ? Fe1 O2 2.008(6) . ? Fe1 O16 2.011(6) . ? Fe1 O10 2.104(6) . ? Fe2 O1 1.933(8) . ? Fe2 O2 2.009(6) . ? Fe2 O11 2.021(8) . ? Fe2 N1 2.022(13) . ? Fe2 N7 2.132(9) . ? Fe2 O10 2.143(7) . ? Fe2 Na1 3.498(7) . ? Fe3 O5 1.946(8) . ? Fe3 N4 2.000(11) . ? Fe3 O7 2.017(6) . ? Fe3 O11 2.024(9) . ? Fe3 N8 2.120(9) . ? Fe3 O10 2.125(6) . ? Fe3 Na1 3.440(6) . ? Na1 O9 2.29(3) . ? Na1 O5 2.367(12) . ? Na1 O9' 2.39(8) . ? Na1 O1 2.411(13) . ? Na1 O4 2.440(15) . ? Na1 O8 2.457(16) . ? Na1 O11 2.733(10) . ? O1 C1 1.352(11) . ? O2 C9 1.414(11) . ? O3 C10 1.413(11) . ? O4 C6 1.379(17) . ? O4 C13 1.44(3) . ? O5 C14 1.350(17) . ? O6 C23 1.422(11) . ? O7 C22 1.428(11) . ? O8 C19 1.39(2) . ? O8 C26' 1.54(5) . ? O8 C26 1.56(5) . ? O10 C27 1.444(11) . ? O11 C28 1.404(15) . ? O12 C36 1.244(11) . ? O13 C36 1.268(11) . ? O13 Dy1 2.336(7) 3_878 ? O14 C43 1.262(11) . ? O15 C43 1.249(10) . ? O15 Dy1 2.304(6) 3_878 ? O16 C50 1.276(10) . ? O17 C50 1.265(10) . ? N1 N2' 1.207(9) . ? N1 N2 1.40(4) . ? N2 N3 1.32(4) . ? N2' N3' 1.407(9) . ? N4 N5 1.07(2) . ? N4 N5' 1.164(9) . ? N5 N6 1.14(3) . ? N5' N6' 1.164(9) . ? N7 C7 1.270(13) . ? N7 C8 1.502(15) . ? N8 C20 1.284(13) . ? N8 C21 1.502(12) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 C7 1.445(15) . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.531(15) . ? C8 C9 1.536(14) . ? C8 C11 1.547(17) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.48(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.38(2) . ? C14 C19 1.44(2) . ? C15 C16 1.41(2) . ? C15 C20 1.429(17) . ? C16 C17 1.37(2) . ? C16 H16 0.9300 . ? C17 C18 1.38(3) . ? C17 H17 0.9300 . ? C18 C19 1.34(3) . ? C18 H18 0.9300 . ? C20 H20 0.9300 . ? C21 C23 1.526(12) . ? C21 C24 1.544(14) . ? C21 C22 1.552(13) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.513(16) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C30 C35 1.378(13) . ? C30 C31 1.391(15) . ? C30 C36 1.491(13) . ? C31 C32 1.383(19) . ? C31 H31 0.9300 . ? C32 C33 1.36(2) . ? C32 H32 0.9300 . ? C33 C34 1.36(2) . ? C33 H33 0.9300 . ? C34 C35 1.368(16) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C37 C42 1.366(14) . ? C37 C38 1.374(15) . ? C37 C43 1.514(13) . ? C38 C39 1.406(17) . ? C38 H38 0.9300 . ? C39 C40 1.34(2) . ? C39 H39 0.9300 . ? C40 C41 1.35(2) . ? C40 H40 0.9300 . ? C41 C42 1.401(17) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C44 C45 1.382(13) . ? C44 C49 1.383(13) . ? C44 C50 1.473(12) . ? C45 C46 1.407(16) . ? C45 H45 0.9300 . ? C46 C47 1.369(19) . ? C46 H46 0.9300 . ? C47 C48 1.329(19) . ? C47 H47 0.9300 . ? C48 C49 1.391(16) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Dy1 O15 79.3(2) . 3_878 ? O12 Dy1 O6 117.4(2) . . ? O15 Dy1 O6 149.2(2) 3_878 . ? O12 Dy1 O3 149.1(2) . . ? O15 Dy1 O3 85.1(2) 3_878 . ? O6 Dy1 O3 67.4(2) . . ? O12 Dy1 O13 127.7(2) . 3_878 ? O15 Dy1 O13 81.6(2) 3_878 3_878 ? O6 Dy1 O13 103.4(2) . 3_878 ? O3 Dy1 O13 75.3(2) . 3_878 ? O12 Dy1 O14 76.8(2) . . ? O15 Dy1 O14 132.3(2) 3_878 . ? O6 Dy1 O14 78.4(2) . . ? O3 Dy1 O14 131.9(2) . . ? O13 Dy1 O14 81.3(3) 3_878 . ? O12 Dy1 O17 77.2(2) . . ? O15 Dy1 O17 82.6(2) 3_878 . ? O6 Dy1 O17 77.0(2) . . ? O3 Dy1 O17 74.4(2) . . ? O13 Dy1 O17 146.7(2) 3_878 . ? O14 Dy1 O17 130.0(2) . . ? O12 Dy1 Fe1 136.42(17) . . ? O15 Dy1 Fe1 115.11(15) 3_878 . ? O6 Dy1 Fe1 34.73(14) . . ? O3 Dy1 Fe1 34.11(14) . . ? O13 Dy1 Fe1 95.75(16) 3_878 . ? O14 Dy1 Fe1 110.71(15) . . ? O17 Dy1 Fe1 65.31(14) . . ? O3 Fe1 O6 82.4(2) . . ? O3 Fe1 O7 171.2(2) . . ? O6 Fe1 O7 94.2(2) . . ? O3 Fe1 O2 93.3(2) . . ? O6 Fe1 O2 172.0(2) . . ? O7 Fe1 O2 89.1(3) . . ? O3 Fe1 O16 95.1(2) . . ? O6 Fe1 O16 93.0(2) . . ? O7 Fe1 O16 93.1(2) . . ? O2 Fe1 O16 94.1(2) . . ? O3 Fe1 O10 92.8(2) . . ? O6 Fe1 O10 93.3(2) . . ? O7 Fe1 O10 79.2(2) . . ? O2 Fe1 O10 80.1(3) . . ? O16 Fe1 O10 170.4(2) . . ? O3 Fe1 Dy1 42.07(17) . . ? O6 Fe1 Dy1 42.21(15) . . ? O7 Fe1 Dy1 136.03(19) . . ? O2 Fe1 Dy1 134.84(18) . . ? O16 Fe1 Dy1 85.71(16) . . ? O10 Fe1 Dy1 103.80(16) . . ? O1 Fe2 O2 162.4(3) . . ? O1 Fe2 O11 91.9(4) . . ? O2 Fe2 O11 100.3(3) . . ? O1 Fe2 N1 97.5(5) . . ? O2 Fe2 N1 93.7(5) . . ? O11 Fe2 N1 95.9(4) . . ? O1 Fe2 N7 87.8(4) . . ? O2 Fe2 N7 77.9(3) . . ? O11 Fe2 N7 169.9(3) . . ? N1 Fe2 N7 94.2(5) . . ? O1 Fe2 O10 91.7(3) . . ? O2 Fe2 O10 79.2(2) . . ? O11 Fe2 O10 76.3(3) . . ? N1 Fe2 O10 168.1(4) . . ? N7 Fe2 O10 93.6(3) . . ? O1 Fe2 Na1 41.3(3) . . ? O2 Fe2 Na1 146.2(2) . . ? O11 Fe2 Na1 51.2(2) . . ? N1 Fe2 Na1 105.9(5) . . ? N7 Fe2 Na1 126.4(3) . . ? O10 Fe2 Na1 76.4(2) . . ? O5 Fe3 N4 95.8(4) . . ? O5 Fe3 O7 160.6(3) . . ? N4 Fe3 O7 98.8(4) . . ? O5 Fe3 O11 94.0(4) . . ? N4 Fe3 O11 95.1(5) . . ? O7 Fe3 O11 97.3(3) . . ? O5 Fe3 N8 88.1(4) . . ? N4 Fe3 N8 94.3(5) . . ? O7 Fe3 N8 78.1(3) . . ? O11 Fe3 N8 170.1(3) . . ? O5 Fe3 O10 89.0(3) . . ? N4 Fe3 O10 170.7(5) . . ? O7 Fe3 O10 78.4(2) . . ? O11 Fe3 O10 76.6(3) . . ? N8 Fe3 O10 93.8(3) . . ? O5 Fe3 Na1 41.6(3) . . ? N4 Fe3 Na1 100.5(4) . . ? O7 Fe3 Na1 145.3(2) . . ? O11 Fe3 Na1 52.6(3) . . ? N8 Fe3 Na1 128.4(2) . . ? O10 Fe3 Na1 77.9(2) . . ? O9 Na1 O5 103.2(10) . . ? O9 Na1 O9' 44(2) . . ? O5 Na1 O9' 144(2) . . ? O9 Na1 O1 147.0(10) . . ? O5 Na1 O1 104.0(3) . . ? O9' Na1 O1 103.6(19) . . ? O9 Na1 O4 105.5(10) . . ? O5 Na1 O4 137.8(5) . . ? O9' Na1 O4 76(2) . . ? O1 Na1 O4 64.3(4) . . ? O9 Na1 O8 77.5(10) . . ? O5 Na1 O8 64.7(4) . . ? O9' Na1 O8 110.7(19) . . ? O1 Na1 O8 131.7(5) . . ? O4 Na1 O8 92.2(5) . . ? O9 Na1 O11 106.8(10) . . ? O5 Na1 O11 69.0(3) . . ? O9' Na1 O11 102.1(19) . . ? O1 Na1 O11 66.8(3) . . ? O4 Na1 O11 128.7(5) . . ? O8 Na1 O11 133.1(5) . . ? O9 Na1 Fe3 109.8(10) . . ? O5 Na1 Fe3 33.1(2) . . ? O9' Na1 Fe3 130.5(19) . . ? O1 Na1 Fe3 84.2(2) . . ? O4 Na1 Fe3 144.6(4) . . ? O8 Na1 Fe3 97.6(4) . . ? O11 Na1 Fe3 36.04(19) . . ? O9 Na1 Fe2 136.5(10) . . ? O5 Na1 Fe2 83.6(2) . . ? O9' Na1 Fe2 109.4(19) . . ? O1 Na1 Fe2 32.0(2) . . ? O4 Na1 Fe2 96.0(4) . . ? O8 Na1 Fe2 139.8(4) . . ? O11 Na1 Fe2 35.22(19) . . ? Fe3 Na1 Fe2 55.79(9) . . ? C1 O1 Fe2 131.8(8) . . ? C1 O1 Na1 119.4(7) . . ? Fe2 O1 Na1 106.7(4) . . ? C9 O2 Fe1 115.0(5) . . ? C9 O2 Fe2 112.0(6) . . ? Fe1 O2 Fe2 104.1(3) . . ? C10 O3 Fe1 128.3(5) . . ? C10 O3 Dy1 123.5(5) . . ? Fe1 O3 Dy1 103.8(2) . . ? C6 O4 C13 118.0(14) . . ? C6 O4 Na1 116.6(6) . . ? C13 O4 Na1 124.4(14) . . ? C14 O5 Fe3 130.0(9) . . ? C14 O5 Na1 123.7(8) . . ? Fe3 O5 Na1 105.4(4) . . ? C23 O6 Fe1 125.2(5) . . ? C23 O6 Dy1 125.5(5) . . ? Fe1 O6 Dy1 103.1(2) . . ? C22 O7 Fe1 115.2(5) . . ? C22 O7 Fe3 111.4(5) . . ? Fe1 O7 Fe3 104.5(3) . . ? C19 O8 C26' 121(3) . . ? C19 O8 C26 107(3) . . ? C26' O8 C26 34(2) . . ? C19 O8 Na1 119.3(8) . . ? C26' O8 Na1 119(3) . . ? C26 O8 Na1 130(2) . . ? C27 O10 Fe1 118.1(5) . . ? C27 O10 Fe3 120.6(6) . . ? Fe1 O10 Fe3 97.3(2) . . ? C27 O10 Fe2 120.2(6) . . ? Fe1 O10 Fe2 96.4(2) . . ? Fe3 O10 Fe2 99.0(2) . . ? C28 O11 Fe2 123.1(9) . . ? C28 O11 Fe3 125.2(9) . . ? Fe2 O11 Fe3 106.7(3) . . ? C28 O11 Na1 105.7(7) . . ? Fe2 O11 Na1 93.5(3) . . ? Fe3 O11 Na1 91.4(3) . . ? C36 O12 Dy1 177.6(6) . . ? C36 O13 Dy1 113.0(6) . 3_878 ? C43 O14 Dy1 136.5(6) . . ? C43 O15 Dy1 141.2(6) . 3_878 ? C50 O16 Fe1 125.9(5) . . ? C50 O17 Dy1 138.4(5) . . ? N2' N1 N2 124(2) . . ? N2' N1 Fe2 117.6(15) . . ? N2 N1 Fe2 115.9(13) . . ? N3 N2 N1 173(3) . . ? N1 N2' N3' 166(3) . . ? N5 N4 N5' 25(4) . . ? N5 N4 Fe3 148(2) . . ? N5' N4 Fe3 142(3) . . ? N4 N5 N6 176(4) . . ? N4 N5' N6' 175(7) . . ? C7 N7 C8 119.8(10) . . ? C7 N7 Fe2 125.6(9) . . ? C8 N7 Fe2 114.6(6) . . ? C20 N8 C21 118.8(9) . . ? C20 N8 Fe3 126.5(8) . . ? C21 N8 Fe3 114.7(6) . . ? O1 C1 C2 124.5(8) . . ? O1 C1 C6 115.4(8) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 C7 117.4(8) . . ? C1 C2 C7 122.6(8) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? O4 C6 C5 123.7(8) . . ? O4 C6 C1 116.3(8) . . ? C5 C6 C1 120.0 . . ? N7 C7 C2 127.6(12) . . ? N7 C7 H7 116.2 . . ? C2 C7 H7 116.2 . . ? N7 C8 C10 108.7(8) . . ? N7 C8 C9 105.2(8) . . ? C10 C8 C9 111.1(9) . . ? N7 C8 C11 113.7(10) . . ? C10 C8 C11 107.8(9) . . ? C9 C8 C11 110.3(9) . . ? O2 C9 C8 110.4(8) . . ? O2 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? O2 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O3 C10 C8 115.2(8) . . ? O3 C10 H10A 108.5 . . ? C8 C10 H10A 108.5 . . ? O3 C10 H10B 108.5 . . ? C8 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C8 115.7(12) . . ? C12 C11 H11A 108.4 . . ? C8 C11 H11A 108.4 . . ? C12 C11 H11B 108.4 . . ? C8 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 125.6(11) . . ? O5 C14 C19 115.4(16) . . ? C15 C14 C19 119.0(15) . . ? C14 C15 C16 118.2(13) . . ? C14 C15 C20 123.7(12) . . ? C16 C15 C20 118.0(15) . . ? C17 C16 C15 121.3(18) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 120.3(16) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.4(17) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 O8 125.5(17) . . ? C18 C19 C14 120(2) . . ? O8 C19 C14 113.7(15) . . ? N8 C20 C15 125.9(12) . . ? N8 C20 H20 117.1 . . ? C15 C20 H20 117.1 . . ? N8 C21 C23 108.8(7) . . ? N8 C21 C24 113.5(8) . . ? C23 C21 C24 108.6(8) . . ? N8 C21 C22 105.8(7) . . ? C23 C21 C22 110.8(7) . . ? C24 C21 C22 109.4(8) . . ? O7 C22 C21 109.2(7) . . ? O7 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? O7 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? O6 C23 C21 114.9(7) . . ? O6 C23 H23A 108.5 . . ? C21 C23 H23A 108.5 . . ? O6 C23 H23B 108.5 . . ? C21 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C21 116.4(10) . . ? C25 C24 H24A 108.2 . . ? C21 C24 H24A 108.2 . . ? C25 C24 H24B 108.2 . . ? C21 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O10 C27 H27A 109.5 . . ? O10 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O10 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O11 C28 H28A 109.5 . . ? O11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C35 C30 C31 118.1(9) . . ? C35 C30 C36 121.2(9) . . ? C31 C30 C36 120.6(9) . . ? C32 C31 C30 120.1(12) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C31 120.3(14) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 120.1(12) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 120.2(12) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C30 121.1(11) . . ? C34 C35 H35 119.5 . . ? C30 C35 H35 119.5 . . ? O12 C36 O13 121.2(9) . . ? O12 C36 C30 121.0(9) . . ? O13 C36 C30 117.8(9) . . ? C42 C37 C38 118.6(9) . . ? C42 C37 C43 121.5(9) . . ? C38 C37 C43 119.9(9) . . ? C37 C38 C39 121.1(11) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C40 C39 C38 119.2(13) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 120.4(11) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C42 121.3(13) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C37 C42 C41 119.4(12) . . ? C37 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? O15 C43 O14 125.7(8) . . ? O15 C43 C37 117.3(8) . . ? O14 C43 C37 117.0(8) . . ? C45 C44 C49 118.5(9) . . ? C45 C44 C50 121.5(8) . . ? C49 C44 C50 120.1(8) . . ? C44 C45 C46 119.8(10) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 119.1(11) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C48 C47 C46 122.0(11) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C47 C48 C49 119.5(12) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? C44 C49 C48 121.1(11) . . ? C44 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? O17 C50 O16 124.2(7) . . ? O17 C50 C44 118.9(7) . . ? O16 C50 C44 116.8(7) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.496 _refine_diff_density_min -1.104 _refine_diff_density_rms 0.115 _iucr_refine_instructions_details ; TITL aaa in P2(1)/c CELL 0.71073 12.7815 35.7632 17.0680 90.000 126.198 90.000 ZERR 2.00 0.0005 0.0015 0.0006 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Na Fe Dy UNIT 196 220 32 68 4 12 4 omit 0 50 omit 1 1 0 omit -1 1 1 omit -2 1 2 omit 0 4 1 omit 1 4 1 omit -2 2 1 omit -2 0 2 omit -1 3 1 omit 0 4 2 omit -2 2 3 omit 3 3 0 omit -3 3 2 omit -3 0 4 omit -2 5 1 omit -3 2 3 omit 2 4 2 omit 0 8 0 omit 1 3 2 omit -2 3 3 omit -2 7 1 omit -5 1 6 omit 1 8 1 omit 1 5 0 omit 2 4 0 omit -1 7 4 omit -2 1 3 omit 1 8 0 omit -1 5 1 omit -2 2 2 omit 0 0 2 omit 1 6 1 omit -1 2 1 omit 3 5 0 omit -1 9 4 omit -4 1 6 omit -1 2 3 omit 0 6 3 omit -3 2 5 L.S. 10 BOND $h acta simu 0.01 0.01 1.7 n1 n2 n3 n2' n3' simu 0.01 0.01 1.7 n4 n5 n6 simu 0.01 0.01 1.7 n4 n5' n6' simu 0.01 0.01 1.7 c2 c3 c4 c5 c6 simu 0.01 0.01 1.7 c14 c15 c16 c17 c18 c19 isor 0.01 0.05 c26 c26' isor 0.01 0.01 o9 o9' o2w o1w isor 0.001 0.001 c32 c13 dfix 1.15 0.01 n4 n5' dfix 1.15 0.01 n5' n6' dfix 2.34 0.01 n4 n6' dfix 1.20 0.01 n1 n2' dfix 1.40 0.01 n2' n3' dfix 2.60 0.01 n1 n3' shel 0.5 2.5 htab FMAP 2 PLAN -20 TEMP 20 WGHT 0.000000 46.361801 FVAR 0.12398 DY1 7 1.512318 0.974147 1.400305 11.00000 0.03398 0.04289 = 0.03037 0.00250 0.02202 0.00587 FE1 6 1.535973 0.924298 1.243110 11.00000 0.03725 0.03310 = 0.03447 0.00335 0.02460 0.00458 FE2 6 1.438888 0.841411 1.171549 11.00000 0.08247 0.04282 = 0.05775 -0.00848 0.05120 -0.00746 FE3 6 1.745471 0.861605 1.299266 11.00000 0.06887 0.04291 = 0.06216 0.01184 0.05103 0.01943 NA1 5 1.664974 0.771544 1.315082 11.00000 0.17475 0.05108 = 0.13406 0.01017 0.11042 0.01235 O1 4 1.452385 0.797521 1.243153 11.00000 0.12925 0.04456 = 0.09468 -0.00552 0.08206 -0.00813 O2 4 1.411790 0.894230 1.123035 11.00000 0.05206 0.04553 = 0.03540 -0.00113 0.03079 -0.00059 O3 4 1.410477 0.931658 1.271831 11.00000 0.04105 0.04650 = 0.03001 -0.00176 0.02531 -0.00498 O4 4 1.518279 0.733261 1.328619 11.00000 0.18995 0.04222 = 0.11159 0.01331 0.07266 -0.02778 O5 4 1.806689 0.822776 1.397149 11.00000 0.09861 0.04953 = 0.08935 0.02969 0.06535 0.02939 O6 4 1.654039 0.948625 1.371001 11.00000 0.03127 0.04996 = 0.03021 0.00425 0.02354 0.00891 O7 4 1.677550 0.911173 1.230550 11.00000 0.04913 0.04445 = 0.04534 0.00510 0.03864 0.00700 O8 4 1.847383 0.759848 1.485049 11.00000 0.14310 0.08842 = 0.14897 0.07905 0.05853 0.03100 PART 1 O9 4 1.789217 0.730026 1.300468 10.35000 0.11439 0.10115 = 0.12515 -0.01991 0.07319 0.01705 PART 2 O9' 4 1.623496 0.717932 1.216945 10.15000 0.11404 0.10771 = 0.10683 0.00021 0.06688 0.00143 PART 0 O10 4 1.583647 0.870124 1.302636 11.00000 0.06203 0.03674 = 0.04219 0.00563 0.03988 0.00646 O11 4 1.606151 0.828985 1.189630 11.00000 0.10172 0.04828 = 0.07220 -0.00222 0.06675 0.00752 O12 4 1.546863 1.034697 1.452882 11.00000 0.05546 0.04373 = 0.03746 0.00100 0.02337 0.00266 O13 4 1.539736 1.076714 1.542819 11.00000 0.07378 0.05564 = 0.05336 -0.00230 0.05050 -0.00354 O14 4 1.705726 0.970679 1.557727 11.00000 0.04035 0.06344 = 0.03480 -0.00037 0.02156 0.01299 O15 4 1.694993 1.008201 1.657452 11.00000 0.02981 0.06742 = 0.03630 -0.00366 0.02143 0.00785 O16 4 1.495651 0.972699 1.170425 11.00000 0.05610 0.04278 = 0.03624 0.00136 0.03259 0.00917 O17 4 1.463241 1.008283 1.262740 11.00000 0.06663 0.04550 = 0.03606 0.00751 0.03764 0.01662 N1 3 1.320374 0.819449 1.036739 11.00000 0.12707 0.10663 = 0.09901 -0.05021 0.08429 -0.03590 PART 1 N2 3 1.306795 0.840378 0.961803 10.50000 0.13015 0.10833 = 0.10064 -0.04246 0.07665 -0.01215 N3 3 1.308596 0.859961 0.897253 10.50000 0.13069 0.11393 = 0.08961 -0.03347 0.07577 0.00093 PART 2 N2' 3 1.244789 0.795626 1.023781 10.50000 0.13882 0.12463 = 0.10970 -0.06540 0.09176 -0.04810 N3' 3 1.185279 0.762689 1.024652 10.50000 0.15465 0.14242 = 0.12293 -0.06865 0.08453 -0.05562 PART 0 N4 3 1.876390 0.851859 1.273137 11.00000 0.10421 0.10050 = 0.12726 0.01286 0.09847 0.03007 PART 1 N5 3 1.902207 0.853992 1.223862 10.65000 0.10262 0.11134 = 0.12639 0.01675 0.10036 0.03096 N6 3 1.922647 0.856563 1.167218 10.65000 0.11769 0.13049 = 0.13942 0.02045 0.09371 0.02402 PART 2 N5' 3 1.924929 0.865622 1.240220 10.35000 0.10515 0.10709 = 0.12805 0.01567 0.10026 0.02956 N6' 3 1.980791 0.880204 1.214164 10.35000 0.10938 0.11505 = 0.13145 0.01483 0.10336 0.02213 PART 0 N7 3 1.283837 0.859607 1.176255 11.00000 0.06080 0.06467 = 0.05242 -0.01596 0.03926 -0.02426 N8 3 1.864758 0.900020 1.413309 11.00000 0.04224 0.05734 = 0.04996 0.01733 0.03386 0.02267 AFIX 66 C1 1 1.382650 0.786050 1.274960 11.00000 0.12533 0.04429 = 0.07002 -0.01737 0.05632 -0.04625 C2 1 1.284775 0.806809 1.266913 11.00000 0.10830 0.08346 = 0.06157 -0.02629 0.05545 -0.05286 C3 1 1.223027 0.793240 1.306173 11.00000 0.11306 0.09681 = 0.07082 -0.01698 0.05851 -0.05736 AFIX 41 H3 2 1.157542 0.807129 1.300789 11.00000 10.10000 AFIX 65 C4 1 1.259153 0.758911 1.353480 11.00000 0.12209 0.10210 = 0.08027 -0.00193 0.05627 -0.06091 AFIX 41 H4 2 1.217839 0.749832 1.379748 11.00000 10.10000 AFIX 65 C5 1 1.357028 0.738151 1.361528 11.00000 0.12934 0.08643 = 0.08210 0.00239 0.05031 -0.05228 AFIX 41 H5 2 1.381198 0.715183 1.393180 11.00000 10.10000 AFIX 65 C6 1 1.418777 0.751720 1.322268 11.00000 0.12997 0.07220 = 0.07679 -0.00492 0.04512 -0.04318 AFIX 0 C7 1 1.240804 0.842247 1.216673 11.00000 0.07841 0.06369 = 0.06710 -0.02504 0.05091 -0.03672 AFIX 41 H7 2 1.173088 0.853671 1.213584 11.00000 10.10000 AFIX 0 C8 1 1.227800 0.896969 1.129787 11.00000 0.04692 0.06788 = 0.04998 -0.01387 0.03040 -0.00950 C9 1 1.280487 0.905286 1.070720 11.00000 0.03986 0.07336 = 0.04118 -0.00220 0.02704 0.00203 AFIX 21 H9A 2 1.229421 0.891933 1.009475 11.00000 10.10000 H9B 2 1.273166 0.931836 1.056731 11.00000 10.10000 AFIX 0 C10 1 1.274849 0.926115 1.209848 11.00000 0.04200 0.06490 = 0.05350 -0.00601 0.03052 -0.00352 AFIX 21 H10A 2 1.233567 0.949811 1.179667 11.00000 10.10000 H10B 2 1.246336 0.918585 1.249046 11.00000 10.10000 AFIX 0 C11 1 1.077843 0.897772 1.063225 11.00000 0.05649 0.10848 = 0.06065 -0.02347 0.03239 -0.02313 AFIX 21 H11A 2 1.046880 0.875404 1.023395 11.00000 10.10000 H11B 2 1.047901 0.896749 1.103814 11.00000 10.10000 AFIX 0 C12 1 1.017994 0.930662 0.998492 11.00000 0.07363 0.17338 = 0.09880 0.01165 0.03897 0.01496 AFIX 31 H12A 2 0.925311 0.928754 0.960745 11.00000 10.10000 H12B 2 1.043764 0.931509 0.955871 11.00000 10.10000 H12C 2 1.046094 0.953054 1.036878 11.00000 10.10000 AFIX 0 C13 1 1.541051 0.694817 1.358549 11.00000 0.14680 0.14637 = 0.14656 0.00028 0.08652 -0.00034 AFIX 31 H13A 2 1.461769 0.680968 1.318380 11.00000 10.10000 H13B 2 1.571477 0.693216 1.425055 11.00000 10.10000 H13C 2 1.605136 0.684555 1.352231 11.00000 10.10000 AFIX 0 C14 1 1.894782 0.824564 1.494502 11.00000 0.07858 0.08474 = 0.08758 0.05615 0.05318 0.03623 C15 1 1.960387 0.856422 1.547109 11.00000 0.07373 0.09718 = 0.07972 0.04667 0.05223 0.03384 C16 1 2.047490 0.853479 1.648622 11.00000 0.08950 0.11323 = 0.08393 0.05157 0.04095 0.02850 AFIX 41 H16 2 2.090094 0.874774 1.685216 11.00000 10.10000 AFIX 0 C17 1 2.070869 0.819914 1.694692 11.00000 0.11092 0.12608 = 0.09215 0.06215 0.02850 0.01768 AFIX 41 H17 2 2.129878 0.818555 1.761889 11.00000 10.10000 AFIX 0 C18 1 2.007406 0.788099 1.642017 11.00000 0.11618 0.11515 = 0.10324 0.07008 0.02710 0.01616 AFIX 41 H18 2 2.027453 0.765147 1.673452 11.00000 10.10000 AFIX 0 C19 1 1.916968 0.790027 1.545760 11.00000 0.09775 0.09626 = 0.10242 0.06043 0.03706 0.02463 C20 1 1.942410 0.892381 1.504249 11.00000 0.05082 0.07017 = 0.05320 0.01599 0.03471 0.02076 AFIX 41 H20 2 1.991344 0.912009 1.545968 11.00000 10.10000 AFIX 0 C21 1 1.854645 0.939768 1.381086 11.00000 0.03943 0.04246 = 0.04427 0.00497 0.03005 0.00637 C22 1 1.779025 0.938152 1.269099 11.00000 0.04612 0.05073 = 0.04570 0.00974 0.03484 0.00725 AFIX 21 H22A 2 1.742657 0.962528 1.241260 11.00000 10.10000 H22B 2 1.837315 0.931286 1.252664 11.00000 10.10000 AFIX 0 C23 1 1.780088 0.962386 1.409103 11.00000 0.03590 0.04550 = 0.04817 0.00049 0.02691 0.00277 AFIX 21 H23A 2 1.830415 0.962977 1.479353 11.00000 10.10000 H23B 2 1.772158 0.987911 1.386984 11.00000 10.10000 AFIX 0 C24 1 1.987443 0.958628 1.426156 11.00000 0.03863 0.07568 = 0.06619 0.01041 0.03274 0.00920 AFIX 21 H24A 2 1.972447 0.982849 1.395606 11.00000 10.10000 H24B 2 2.027309 0.963018 1.494431 11.00000 10.10000 AFIX 0 C25 1 2.083042 0.937415 1.417976 11.00000 0.04962 0.09633 = 0.09744 0.02498 0.05071 0.02521 AFIX 31 H25A 2 2.162393 0.951332 1.449347 11.00000 10.10000 H25B 2 2.047234 0.934006 1.350717 11.00000 10.10000 H25C 2 2.100153 0.913450 1.448676 11.00000 10.10000 AFIX 0 PART 1 C26 1 1.872483 0.726002 1.551841 10.50000 0.14172 0.10656 = 0.13344 0.05731 0.07450 0.01603 PART 2 C26' 1 1.900376 0.719771 1.515617 10.50000 0.19839 0.07312 = 0.15047 0.07122 0.10597 0.05112 PART 0 C27 1 1.594472 0.863720 1.390682 11.00000 0.07972 0.04733 = 0.04922 0.00872 0.04964 0.00208 AFIX 31 H27A 2 1.614696 0.837902 1.408995 11.00000 10.10000 H27B 2 1.513782 0.869827 1.379938 11.00000 10.10000 H27C 2 1.662137 0.879172 1.441660 11.00000 10.10000 AFIX 0 C28 1 1.610346 0.813641 1.115786 11.00000 0.14242 0.06620 = 0.09808 -0.01658 0.08512 0.00334 AFIX 31 H28A 2 1.532719 0.799525 1.072067 11.00000 10.10000 H28B 2 1.684330 0.797497 1.143992 11.00000 10.10000 H28C 2 1.616856 0.833411 1.080824 11.00000 10.10000 AFIX 0 C30 1 1.609198 1.097047 1.448554 11.00000 0.05639 0.04587 = 0.04427 0.00802 0.03656 0.00604 C31 1 1.656579 1.130803 1.498062 11.00000 0.11782 0.05973 = 0.08799 -0.01647 0.08159 -0.03308 AFIX 41 H31 2 1.657407 1.135316 1.552087 11.00000 10.10000 AFIX 0 C32 1 1.702471 1.157673 1.467115 11.00000 0.09386 0.09304 = 0.09345 0.00039 0.05535 -0.00096 AFIX 41 H32 2 1.733135 1.180330 1.499956 11.00000 10.10000 AFIX 0 C33 1 1.702934 1.151096 1.388883 11.00000 0.15300 0.08568 = 0.11149 -0.00656 0.10129 -0.04941 AFIX 41 H33 2 1.735386 1.169070 1.369087 11.00000 10.10000 AFIX 0 C34 1 1.655931 1.118210 1.339373 11.00000 0.11249 0.10635 = 0.08569 0.00929 0.08349 -0.01520 AFIX 41 H34 2 1.656151 1.113847 1.285755 11.00000 10.10000 AFIX 0 C35 1 1.608439 1.091605 1.368306 11.00000 0.06311 0.06775 = 0.05296 0.00748 0.04401 -0.00863 AFIX 41 H35 2 1.575089 1.069479 1.333224 11.00000 10.10000 AFIX 0 C36 1 1.563264 1.067389 1.482992 11.00000 0.02629 0.04897 = 0.02256 0.00770 0.00453 0.00575 C37 1 1.898973 0.982735 1.713997 11.00000 0.03812 0.05942 = 0.03543 0.00746 0.02234 0.00798 C38 1 1.965001 1.007652 1.789672 11.00000 0.04365 0.09043 = 0.05435 -0.01513 0.02226 0.00292 AFIX 41 H38 2 1.920113 1.027115 1.793693 11.00000 10.10000 AFIX 0 C39 1 2.099274 1.004218 1.861124 11.00000 0.04425 0.12336 = 0.06430 -0.01783 0.01284 -0.00345 AFIX 41 H39 2 2.143566 1.021762 1.910733 11.00000 10.10000 AFIX 0 C40 1 2.162816 0.975330 1.856923 11.00000 0.03486 0.13437 = 0.06581 0.01254 0.01729 0.01659 AFIX 41 H40 2 2.251024 0.972304 1.905275 11.00000 10.10000 AFIX 0 C41 1 2.099656 0.950704 1.783147 11.00000 0.05488 0.11482 = 0.08153 0.01355 0.02536 0.04220 AFIX 41 H41 2 2.145242 0.930969 1.780943 11.00000 10.10000 AFIX 0 C42 1 1.966540 0.954234 1.709604 11.00000 0.04698 0.09240 = 0.04750 0.00357 0.02238 0.02791 AFIX 41 H42 2 1.924587 0.937337 1.658297 11.00000 10.10000 AFIX 0 C43 1 1.754605 0.987423 1.637317 11.00000 0.03432 0.04946 = 0.03324 0.00775 0.02185 0.00513 C44 1 1.432645 1.035053 1.124160 11.00000 0.05059 0.03020 = 0.03217 0.00518 0.02416 0.00830 C45 1 1.355725 1.064134 1.116352 11.00000 0.06780 0.05304 = 0.05162 0.00873 0.03436 0.01992 AFIX 41 H45 2 1.327203 1.064591 1.155419 11.00000 10.10000 AFIX 0 C46 1 1.320737 1.093040 1.049103 11.00000 0.07970 0.06111 = 0.06605 0.02602 0.03436 0.03369 AFIX 41 H46 2 1.269032 1.112728 1.043288 11.00000 10.10000 AFIX 0 C47 1 1.363827 1.091789 0.992361 11.00000 0.11558 0.06759 = 0.05893 0.03103 0.05130 0.01486 AFIX 41 H47 2 1.338406 1.110506 0.946552 11.00000 10.10000 AFIX 0 C48 1 1.440864 1.064656 1.000703 11.00000 0.12480 0.07919 = 0.06812 0.03063 0.07006 0.02081 AFIX 41 H48 2 1.472586 1.065210 0.963741 11.00000 10.10000 AFIX 0 C49 1 1.473669 1.035423 1.065163 11.00000 0.07708 0.06477 = 0.04350 0.01109 0.04361 0.00766 AFIX 41 H49 2 1.524020 1.015801 1.068651 11.00000 10.10000 AFIX 0 C50 1 1.467953 1.003643 1.191387 11.00000 0.04371 0.03934 = 0.03053 0.00845 0.02616 0.01277 O1W 4 0.729199 0.672928 0.194125 10.30000 0.09114 0.06743 = 0.07420 -0.00078 0.04803 0.01465 O2W 4 0.976789 0.771022 0.339319 10.20000 0.06873 0.06557 = 0.07640 0.00019 0.04326 0.01316 HKLF 4 REM aaa in P2(1)/c REM R1 = 0.0796 for 8386 Fo > 4sig(Fo) and 0.1060 for all 10664 data REM 772 parameters refined using 162 restraints END ; #======================END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 857520' # 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 0.072 0.250 0.955 449 54 ' ' 2 -0.072 0.750 0.556 449 54 ' ' _platon_squeeze_details ; The Platon SQUEEZE procedure was applied to recover 108 electrons per unit cell in one void (total volume 898 ^A^3); that is 54 electrons per formula unit. Lattice solvent water molecules (10 electrons/H2O) were present, and the electrons recovered by SQUEEZE have been assigned as 5 water molecules per formula unit. These water molecules have been included in the formula for the calculation of intensive properties. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C88 H143 Dy2 Fe6 N17 Na2 O37' _chemical_formula_sum 'C88 H143 Dy2 Fe6 N17 Na2 O37' _chemical_formula_weight 2737.27 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' Na Na 0.0362 0.0249 '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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.408(3) _cell_length_b 41.897(8) _cell_length_c 13.420(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.04(3) _cell_angle_gamma 90.00 _cell_volume 6371(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11112 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour 'black brown' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 1.903 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3175 _exptl_absorpt_correction_T_max 0.4281 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 47736 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11112 _reflns_number_gt 8688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+10.8699P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11112 _refine_ls_number_parameters 817 _refine_ls_number_restraints 248 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.39588(2) 0.962157(6) 0.47757(2) 0.03533(12) Uani 1 1 d . . . Fe1 Fe 0.33540(8) 0.825505(19) 0.50063(10) 0.0510(3) Uani 1 1 d . . . Fe2 Fe 0.26792(8) 0.85630(2) 0.70051(10) 0.0522(3) Uani 1 1 d . . . Fe3 Fe 0.25286(7) 0.896620(18) 0.47662(8) 0.0384(2) Uani 1 1 d . . . Na1 Na 0.448(2) 0.7905(5) 0.7640(15) 0.060(4) Uani 0.50 1 d P . 1 Na1' Na 0.4523(19) 0.7968(4) 0.7987(14) 0.055(4) Uani 0.50 1 d P . 2 C1 C 0.5641(3) 0.80623(10) 0.6004(4) 0.063(2) Uani 1 1 d G . . C2 C 0.5911(3) 0.81931(7) 0.5181(4) 0.078(3) Uani 1 1 d GD . . C3 C 0.7050(3) 0.81680(11) 0.5232(4) 0.081(3) Uani 1 1 d G . . H3 H 0.7230 0.8256 0.4682 0.100 Uiso 1 1 calc . . . C4 C 0.7918(3) 0.80120(14) 0.6105(5) 0.096(3) Uani 1 1 d GU . . H4 H 0.8679 0.7995 0.6139 0.100 Uiso 1 1 calc . . . C5 C 0.7648(4) 0.78812(11) 0.6928(4) 0.088(3) Uani 1 1 d GU . . H5 H 0.8229 0.7777 0.7512 0.100 Uiso 1 1 calc . . . C6 C 0.6509(4) 0.79063(10) 0.6877(4) 0.074(3) Uani 1 1 d G . . C7 C 0.5179(4) 0.83758(11) 0.4188(4) 0.059(2) Uani 1 1 d GD . . H7 H 0.5525 0.8455 0.3740 0.100 Uiso 1 1 calc . . . C8 C 0.3455(6) 0.86143(15) 0.2878(6) 0.0518(18) Uani 1 1 d D . . C9 C 0.2277(6) 0.85560(15) 0.2776(7) 0.0537(19) Uani 1 1 d . . . H9A H 0.2002 0.8353 0.2411 0.100 Uiso 1 1 calc . . . H9B H 0.1757 0.8722 0.2333 0.100 Uiso 1 1 calc . . . C10 C 0.3729(5) 0.89704(14) 0.3139(6) 0.0474(17) Uani 1 1 d . . . H10A H 0.4540 0.9008 0.3243 0.100 Uiso 1 1 calc . . . H10B H 0.3228 0.9093 0.2508 0.100 Uiso 1 1 calc . . . C11 C 0.3570(7) 0.85240(17) 0.1770(7) 0.066(2) Uani 1 1 d DU . . H11A H 0.2932 0.8631 0.1181 0.100 Uiso 1 1 calc . A 1 H11B H 0.4301 0.8616 0.1805 0.100 Uiso 1 1 calc . B 1 C12 C 0.3556(9) 0.8176(2) 0.1443(10) 0.066(3) Uani 0.75 1 d PD . 1 H12A H 0.3628 0.8164 0.0759 0.100 Uiso 0.75 1 calc P C 1 H12B H 0.2827 0.8079 0.1372 0.100 Uiso 0.75 1 calc P D 1 H12C H 0.4204 0.8065 0.1993 0.100 Uiso 0.75 1 calc P E 1 C12' C 0.265(3) 0.8665(8) 0.077(3) 0.062(8) Uani 0.25 1 d PU . 2 H12D H 0.2781 0.8597 0.0143 0.100 Uiso 0.25 1 calc P F 2 H12E H 0.2697 0.8894 0.0819 0.100 Uiso 0.25 1 calc P G 2 H12F H 0.1886 0.8597 0.0697 0.100 Uiso 0.25 1 calc P H 2 C13 C 0.6881(16) 0.7576(5) 0.8835(14) 0.060(6) Uani 0.50 1 d PDU . 1 H13A H 0.6351 0.7540 0.9183 0.100 Uiso 0.50 1 calc P I 1 H13B H 0.7558 0.7692 0.9319 0.100 Uiso 0.50 1 calc P J 1 H13C H 0.7129 0.7374 0.8660 0.100 Uiso 0.50 1 calc P K 1 C13' C 0.7162(17) 0.7567(5) 0.8556(17) 0.066(6) Uani 0.50 1 d PDU . 2 H13D H 0.6904 0.7493 0.9100 0.100 Uiso 0.50 1 calc P L 2 H13E H 0.7877 0.7688 0.8900 0.100 Uiso 0.50 1 calc P M 2 H13F H 0.7306 0.7387 0.8184 0.100 Uiso 0.50 1 calc P N 2 C14 C 0.4647(4) 0.85814(9) 0.9370(4) 0.063(2) Uani 1 1 d G . . C15 C 0.4544(3) 0.89031(9) 0.9570(3) 0.059(2) Uani 1 1 d G . . C16 C 0.5258(4) 0.90348(11) 1.0574(3) 0.072(2) Uani 1 1 d G . . H16 H 0.5189 0.9250 1.0708 0.100 Uiso 1 1 calc . . . C17 C 0.6073(4) 0.88449(16) 1.1378(3) 0.090(3) Uani 1 1 d G . . H17 H 0.6551 0.8933 1.2050 0.100 Uiso 1 1 calc . . . C18 C 0.6176(4) 0.85233(15) 1.1178(4) 0.083(3) Uani 1 1 d G . . H18 H 0.6721 0.8396 1.1716 0.100 Uiso 1 1 calc . . . C19 C 0.5462(5) 0.83915(10) 1.0174(5) 0.074(3) Uani 1 1 d G . . C20 C 0.3688(4) 0.91064(11) 0.8764(4) 0.0542(18) Uani 1 1 d G . . H20 H 0.3676 0.9319 0.8960 0.100 Uiso 1 1 calc . . . C21 C 0.2113(6) 0.92699(14) 0.7069(6) 0.0457(16) Uani 1 1 d . . . C22 C 0.1206(6) 0.90854(16) 0.6086(6) 0.0512(18) Uani 1 1 d . . . C23 C 0.2672(6) 0.94974(15) 0.6517(6) 0.0432(15) Uani 1 1 d . . . H23A H 0.2108 0.9665 0.6156 0.100 Uiso 1 1 calc . . . H23B H 0.3354 0.9597 0.7080 0.100 Uiso 1 1 calc . . . C24 C 0.1625(7) 0.94667(18) 0.7780(7) 0.0584(19) Uani 1 1 d . . . H24A H 0.0957 0.9590 0.7292 0.100 Uiso 1 1 calc . . . H24B H 0.2231 0.9617 0.8208 0.100 Uiso 1 1 calc . . . C25 C 0.1224(8) 0.9280(2) 0.8578(8) 0.075(2) Uani 1 1 d U . . H25A H 0.0957 0.9428 0.8974 0.100 Uiso 1 1 calc . . . H25B H 0.1876 0.9159 0.9081 0.100 Uiso 1 1 calc . . . H25C H 0.0592 0.9137 0.8168 0.100 Uiso 1 1 calc . . . C26 C 0.6109(18) 0.7914(5) 1.0990(17) 0.058(5) Uani 0.50 1 d PU . 1 H26A H 0.6139 0.7689 1.0873 0.100 Uiso 0.50 1 calc P O 1 H26B H 0.5698 0.7952 1.1450 0.100 Uiso 0.50 1 calc P P 1 H26C H 0.6898 0.7996 1.1336 0.100 Uiso 0.50 1 calc P Q 1 C26' C 0.613(2) 0.7810(5) 1.0643(19) 0.075(7) Uani 0.50 1 d PU . 2 H26D H 0.5958 0.7614 1.0241 0.100 Uiso 0.50 1 calc P R 2 H26E H 0.5895 0.7794 1.1239 0.100 Uiso 0.50 1 calc P S 2 H26F H 0.6963 0.7852 1.0921 0.100 Uiso 0.50 1 calc P T 2 C27 C 0.4786(5) 0.87933(15) 0.6675(6) 0.0488(17) Uani 1 1 d . . . C28 C 0.1870(19) 0.7919(5) 0.6108(18) 0.064(5) Uani 0.50 1 d PU . 1 C28' C 0.169(2) 0.7931(5) 0.5599(17) 0.061(5) Uani 0.50 1 d PU . 2 C29 C 0.1263(5) 0.94518(14) 0.3061(5) 0.0360(14) Uani 1 1 d . . . C30 C 0.0151(5) 0.95488(15) 0.2054(6) 0.0462(15) Uani 1 1 d DU . . C31 C -0.0128(10) 0.9302(2) 0.1123(8) 0.098(3) Uani 1 1 d DU . . H31A H 0.0462 0.9315 0.0832 0.100 Uiso 1 1 calc . . . H31B H -0.0889 0.9347 0.0556 0.100 Uiso 1 1 calc . . . H31C H -0.0128 0.9091 0.1403 0.100 Uiso 1 1 calc . . . C32 C 0.0230(7) 0.98688(19) 0.1581(7) 0.070(2) Uani 1 1 d DU . . H32A H 0.0789 0.9858 0.1256 0.100 Uiso 1 1 calc . . . H32B H 0.0481 1.0026 0.2150 0.100 Uiso 1 1 calc . . . H32C H -0.0531 0.9926 0.1036 0.100 Uiso 1 1 calc . . . C33 C -0.0693(8) 0.9554(2) 0.2559(9) 0.086(3) Uani 1 1 d DU . . H33A H -0.0734 0.9346 0.2842 0.100 Uiso 1 1 calc . . . H33B H -0.1457 0.9613 0.2024 0.100 Uiso 1 1 calc . . . H33C H -0.0442 0.9707 0.3143 0.100 Uiso 1 1 calc . . . C34 C 0.5660(5) 0.99226(16) 0.7270(6) 0.0427(15) Uani 1 1 d . . . C35 C 0.6462(16) 0.9856(5) 0.8456(16) 0.062(4) Uani 0.50 1 d PU U 1 C35' C 0.615(2) 0.9934(7) 0.863(2) 0.088(5) Uani 0.50 1 d PU U 2 C36 C 0.7150(19) 1.0078(5) 0.9246(17) 0.071(5) Uani 0.50 1 d PU U 1 H36A H 0.6644 1.0213 0.9443 0.100 Uiso 0.50 1 calc P V 1 H36B H 0.7596 1.0205 0.8954 0.100 Uiso 0.50 1 calc P W 1 H36C H 0.7681 0.9966 0.9882 0.100 Uiso 0.50 1 calc P X 1 C37 C 0.6064(15) 0.9587(4) 0.9046(13) 0.067(4) Uani 0.50 1 d PU U 1 H37A H 0.5681 0.9419 0.8537 0.100 Uiso 0.50 1 calc P Y 1 H37B H 0.5525 0.9674 0.9322 0.100 Uiso 0.50 1 calc P Z 1 H37C H 0.6743 0.9503 0.9640 0.100 Uiso 0.50 1 calc P A 1 C36' C 0.696(2) 1.0221(6) 0.902(2) 0.092(6) Uani 0.50 1 d PU U 2 H36D H 0.6532 1.0411 0.8695 0.100 Uiso 0.50 1 calc P B 2 H36E H 0.7608 1.0196 0.8804 0.100 Uiso 0.50 1 calc P C 2 H36F H 0.7262 1.0236 0.9798 0.100 Uiso 0.50 1 calc P D 2 C37' C 0.697(2) 0.9675(7) 0.904(2) 0.113(6) Uani 0.50 1 d PU U 2 H37D H 0.7504 0.9677 0.8679 0.100 Uiso 0.50 1 calc P E 2 H37E H 0.6552 0.9476 0.8893 0.100 Uiso 0.50 1 calc P F 2 H37F H 0.7414 0.9699 0.9808 0.100 Uiso 0.50 1 calc P G 2 C38 C 0.7417(14) 0.9649(4) 0.8192(15) 0.070(4) Uani 0.50 1 d PU U 1 H38A H 0.7018 0.9484 0.7678 0.100 Uiso 0.50 1 calc P H 1 H38B H 0.7973 0.9554 0.8854 0.100 Uiso 0.50 1 calc P I 1 H38C H 0.7827 0.9786 0.7889 0.100 Uiso 0.50 1 calc P J 1 C38' C 0.5354(16) 0.9972(5) 0.9168(16) 0.083(5) Uani 0.50 1 d PU U 2 H38D H 0.4829 1.0147 0.8844 0.100 Uiso 0.50 1 calc P K 2 H38E H 0.5803 1.0015 0.9930 0.100 Uiso 0.50 1 calc P L 2 H38F H 0.4904 0.9780 0.9088 0.100 Uiso 0.50 1 calc P M 2 C39 C 0.6442(6) 0.95698(14) 0.5058(7) 0.0506(18) Uani 1 1 d . . . C40 C 0.7305(12) 0.9443(3) 0.4698(13) 0.051(4) Uani 0.50 1 d PD . 1 C40' C 0.7505(10) 0.9376(3) 0.5495(13) 0.040(3) Uani 0.50 1 d PD . 2 C41 C 0.7020(16) 0.9519(4) 0.3509(14) 0.076(5) Uani 0.50 1 d PDU . 1 H41A H 0.6305 0.9413 0.3050 0.100 Uiso 0.50 1 calc P N 1 H41B H 0.7655 0.9448 0.3329 0.100 Uiso 0.50 1 calc P O 1 H41C H 0.6921 0.9746 0.3396 0.100 Uiso 0.50 1 calc P P 1 C41' C 0.8014(19) 0.9374(5) 0.6734(16) 0.102(7) Uani 0.50 1 d PDU . 2 H41D H 0.7544 0.9238 0.6975 0.100 Uiso 0.50 1 calc P Q 2 H41E H 0.8010 0.9587 0.6996 0.100 Uiso 0.50 1 calc P R 2 H41F H 0.8809 0.9295 0.7014 0.100 Uiso 0.50 1 calc P S 2 C42 C 0.7269(19) 0.9038(5) 0.5085(18) 0.054(5) Uani 0.50 1 d PU . 1 H42A H 0.7787 0.8913 0.4870 0.100 Uiso 0.50 1 calc P T 1 H42B H 0.6479 0.8957 0.4731 0.100 Uiso 0.50 1 calc P U 1 H42C H 0.7522 0.9025 0.5862 0.100 Uiso 0.50 1 calc P V 1 C43 C 0.8383(11) 0.9602(3) 0.5450(12) 0.062(3) Uani 0.70 1 d PU . 1 H43A H 0.9038 0.9536 0.5293 0.100 Uiso 0.70 1 calc P W 1 H43B H 0.8530 0.9546 0.6187 0.100 Uiso 0.70 1 calc P X 1 H43C H 0.8286 0.9829 0.5362 0.100 Uiso 0.70 1 calc P Y 1 C42' C 0.734(3) 0.9089(7) 0.473(2) 0.079(9) Uani 0.50 1 d PU . 2 H42D H 0.8029 0.8956 0.5014 0.100 Uiso 0.50 1 calc P Z 2 H42E H 0.7226 0.9165 0.4018 0.100 Uiso 0.50 1 calc P A 2 H42F H 0.6663 0.8968 0.4679 0.100 Uiso 0.50 1 calc P B 2 C43' C 0.827(3) 0.9514(9) 0.493(3) 0.074(10) Uani 0.30 1 d PU . 2 H43D H 0.9044 0.9422 0.5249 0.100 Uiso 0.30 1 calc P C 2 H43E H 0.8325 0.9742 0.5027 0.100 Uiso 0.30 1 calc P D 2 H43F H 0.7910 0.9465 0.4166 0.100 Uiso 0.30 1 calc P E 2 C44 C 0.8897(13) 0.8267(4) 0.3407(12) 0.056(4) Uani 0.50 1 d P . . C45 C 0.9497(15) 0.8553(4) 0.3439(16) 0.076(5) Uani 0.50 1 d PU . . N1 N 0.4145(4) 0.84244(11) 0.3948(5) 0.0511(15) Uani 1 1 d D . . N2 N 0.2917(5) 0.90240(13) 0.7776(5) 0.0492(14) Uani 1 1 d . . . N3 N 0.2759(6) 0.78722(14) 0.3965(7) 0.072(2) Uani 1 1 d DU . . N4 N 0.333(2) 0.7653(5) 0.390(2) 0.068(8) Uani 0.50 1 d PDU . 1 N4' N 0.332(2) 0.7706(4) 0.362(2) 0.056(6) Uani 0.50 1 d PU . 2 N5 N 0.3910(18) 0.7451(4) 0.3735(18) 0.086(7) Uani 0.50 1 d PDU . 1 N5' N 0.3862(17) 0.7531(4) 0.3333(15) 0.068(5) Uani 0.50 1 d PU . 2 N6 N 0.1557(7) 0.84379(18) 0.7570(8) 0.085(2) Uani 1 1 d DU . . N7 N 0.0666(14) 0.8468(3) 0.7117(15) 0.097(3) Uani 0.60 1 d PU . 1 N8 N -0.0295(14) 0.8491(4) 0.6538(15) 0.109(3) Uani 0.60 1 d PU . 1 N7' N 0.1359(19) 0.8437(5) 0.8374(13) 0.099(3) Uani 0.40 1 d PDU . 2 N8' N 0.123(2) 0.8472(6) 0.9217(14) 0.110(4) Uani 0.40 1 d PDU . 2 N9 N 0.8577(14) 0.8045(4) 0.3474(13) 0.084(4) Uani 0.50 1 d PU . . O1 O 0.4718(4) 0.80748(10) 0.6063(5) 0.0679(17) Uani 1 1 d . . . O2 O 0.2229(3) 0.85494(9) 0.3894(4) 0.0446(11) Uani 1 1 d . . . O3 O 0.3573(3) 0.90983(9) 0.4125(4) 0.0433(11) Uani 1 1 d . . . O4 O 0.6230(5) 0.77737(12) 0.7756(6) 0.090(2) Uani 1 1 d D . . O5 O 0.3964(4) 0.84291(12) 0.8371(5) 0.0663(15) Uani 1 1 d . . . O6 O 0.1655(4) 0.88288(9) 0.5656(4) 0.0467(11) Uani 1 1 d . . . O7 O 0.3042(3) 0.93536(9) 0.5726(4) 0.0397(10) Uani 1 1 d . . . O8 O 0.5462(5) 0.80809(15) 0.9896(6) 0.088(2) Uani 1 1 d . . . O9 O 0.3667(3) 0.86729(9) 0.6065(4) 0.0454(11) Uani 1 1 d . . . O10 O 0.2625(4) 0.81672(10) 0.6093(5) 0.0612(15) Uani 1 1 d U . . O11 O 0.1256(3) 0.91817(9) 0.3515(4) 0.0411(10) Uani 1 1 d . . . O12 O 0.2062(3) 0.96359(9) 0.3349(4) 0.0388(10) Uani 1 1 d . . . O13 O 0.4978(4) 0.97156(13) 0.6751(4) 0.0627(14) Uani 1 1 d . U . O14 O 0.5807(6) 1.02124(19) 0.6908(7) 0.0381(18) Uani 0.65 1 d P . 1 O14' O 0.5840(11) 1.0069(4) 0.6529(14) 0.042(4) Uani 0.35 1 d P . 2 O15 O 0.5636(4) 0.94104(12) 0.5012(5) 0.0627(14) Uani 1 1 d . . . O16 O 0.6389(9) 0.9855(2) 0.5243(8) 0.043(2) Uani 0.65 1 d P . 1 O16' O 0.6604(14) 0.9883(4) 0.4789(15) 0.041(4) Uani 0.35 1 d P . 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 Dy1 0.02222(17) 0.02628(17) 0.0505(2) 0.00443(11) 0.00763(13) -0.00131(9) Fe1 0.0282(5) 0.0245(4) 0.0896(8) 0.0000(4) 0.0131(5) -0.0031(3) Fe2 0.0360(5) 0.0382(5) 0.0763(8) 0.0153(5) 0.0168(5) -0.0072(4) Fe3 0.0222(4) 0.0276(4) 0.0600(6) 0.0026(4) 0.0111(4) -0.0023(3) Na1 0.057(5) 0.053(9) 0.063(9) 0.013(5) 0.016(7) 0.008(5) Na1' 0.045(4) 0.034(6) 0.080(11) 0.017(6) 0.020(8) -0.002(4) C1 0.051(5) 0.021(3) 0.106(7) -0.006(4) 0.022(5) -0.003(3) C2 0.023(3) 0.037(4) 0.145(9) -0.039(5) 0.006(5) 0.003(3) C3 0.043(5) 0.060(5) 0.142(9) -0.042(5) 0.038(5) -0.003(4) C4 0.064(5) 0.085(6) 0.125(7) -0.027(5) 0.025(5) 0.016(5) C5 0.045(4) 0.062(4) 0.116(7) -0.039(5) -0.008(4) 0.020(4) C6 0.043(4) 0.036(4) 0.118(8) -0.016(4) 0.008(5) -0.002(3) C7 0.037(4) 0.027(3) 0.114(7) -0.023(4) 0.031(4) -0.008(3) C8 0.032(3) 0.043(4) 0.079(5) -0.005(3) 0.022(4) -0.005(3) C9 0.037(4) 0.037(3) 0.085(6) -0.013(3) 0.023(4) -0.007(3) C10 0.032(3) 0.029(3) 0.081(5) -0.001(3) 0.023(3) -0.001(2) C11 0.053(4) 0.056(4) 0.094(6) -0.012(4) 0.035(4) -0.006(3) C12 0.050(6) 0.067(6) 0.092(9) -0.035(6) 0.040(6) -0.013(5) C12' 0.065(11) 0.068(11) 0.056(11) 0.002(9) 0.029(9) 0.005(9) C13 0.044(8) 0.058(8) 0.070(9) -0.013(7) 0.016(7) 0.029(6) C13' 0.056(9) 0.065(9) 0.067(9) 0.008(7) 0.015(7) 0.016(7) C14 0.046(4) 0.071(5) 0.070(6) 0.031(4) 0.020(4) -0.010(4) C15 0.050(4) 0.074(5) 0.053(5) 0.016(4) 0.021(4) -0.018(4) C16 0.065(6) 0.099(6) 0.055(5) 0.012(5) 0.026(5) -0.006(5) C17 0.044(5) 0.171(11) 0.049(5) 0.012(6) 0.013(4) -0.021(6) C18 0.052(5) 0.111(8) 0.085(7) 0.045(6) 0.028(5) 0.011(5) C19 0.053(5) 0.096(7) 0.068(6) 0.039(5) 0.020(5) -0.008(5) C20 0.049(4) 0.061(4) 0.054(5) 0.012(4) 0.023(4) -0.011(3) C21 0.043(4) 0.036(3) 0.063(5) 0.003(3) 0.027(4) -0.003(3) C22 0.032(3) 0.048(4) 0.076(5) -0.003(3) 0.023(4) -0.001(3) C23 0.039(4) 0.041(3) 0.051(4) -0.001(3) 0.019(3) -0.007(3) C24 0.056(5) 0.057(4) 0.071(5) -0.005(4) 0.035(4) -0.009(3) C25 0.070(5) 0.077(5) 0.093(6) -0.009(4) 0.050(5) -0.010(4) C26 0.056(8) 0.054(8) 0.059(9) 0.011(7) 0.016(7) 0.021(6) C26' 0.080(10) 0.066(10) 0.066(10) 0.015(8) 0.018(8) 0.017(8) C27 0.018(3) 0.040(3) 0.071(5) 0.006(3) 0.001(3) -0.006(2) C28 0.053(8) 0.054(8) 0.078(10) 0.000(8) 0.020(8) -0.026(6) C28' 0.061(9) 0.052(8) 0.069(9) 0.001(8) 0.026(8) -0.031(6) C29 0.025(3) 0.036(3) 0.046(4) -0.005(3) 0.013(3) 0.000(2) C30 0.023(3) 0.052(4) 0.055(4) 0.006(3) 0.007(3) -0.003(3) C31 0.085(6) 0.092(6) 0.080(6) -0.025(4) -0.003(5) 0.006(5) C32 0.045(4) 0.070(5) 0.076(5) 0.025(4) 0.005(4) 0.000(3) C33 0.050(5) 0.099(6) 0.114(7) 0.036(5) 0.038(5) 0.018(4) C34 0.022(3) 0.057(4) 0.044(4) 0.002(3) 0.008(3) 0.000(3) C35 0.037(6) 0.079(8) 0.050(7) 0.025(6) -0.003(5) -0.013(6) C35' 0.060(8) 0.115(11) 0.083(10) -0.029(8) 0.021(7) -0.006(7) C36 0.044(8) 0.083(10) 0.053(8) 0.021(8) -0.012(7) -0.016(8) C37 0.052(7) 0.086(9) 0.050(7) 0.034(7) 0.008(6) -0.017(7) C36' 0.066(10) 0.114(13) 0.087(12) -0.043(10) 0.021(9) -0.009(10) C37' 0.082(11) 0.128(13) 0.103(12) -0.014(11) 0.011(10) 0.004(10) C38 0.041(7) 0.081(9) 0.064(8) 0.011(7) -0.003(7) 0.014(6) C38' 0.057(9) 0.119(11) 0.079(10) -0.020(9) 0.035(8) -0.010(8) C39 0.039(4) 0.031(3) 0.075(5) -0.017(3) 0.016(4) 0.001(3) C40 0.031(8) 0.051(8) 0.067(11) -0.029(8) 0.017(8) -0.004(6) C40' 0.009(5) 0.047(7) 0.058(9) -0.004(7) 0.006(6) 0.008(5) C41 0.070(8) 0.080(8) 0.091(9) -0.014(7) 0.046(7) 0.002(7) C41' 0.078(9) 0.102(10) 0.114(11) -0.006(8) 0.027(8) 0.006(8) C42 0.058(8) 0.038(7) 0.064(9) -0.003(7) 0.022(7) 0.029(6) C43 0.037(5) 0.068(6) 0.073(7) -0.015(6) 0.014(5) -0.002(4) C42' 0.074(11) 0.077(11) 0.087(12) 0.013(8) 0.035(8) 0.018(7) C43' 0.067(13) 0.080(13) 0.079(13) -0.001(9) 0.033(10) -0.004(9) C44 0.050(9) 0.065(9) 0.054(9) 0.012(7) 0.024(7) -0.021(7) C45 0.054(7) 0.052(7) 0.094(9) -0.007(7) 0.002(6) -0.025(6) N1 0.026(3) 0.029(2) 0.091(5) -0.012(3) 0.016(3) -0.005(2) N2 0.039(3) 0.051(3) 0.058(4) 0.012(3) 0.019(3) -0.008(2) N3 0.044(3) 0.034(3) 0.118(6) -0.006(3) 0.013(4) -0.003(3) N4 0.064(10) 0.051(11) 0.072(11) 0.009(7) 0.010(7) -0.011(7) N4' 0.054(8) 0.020(6) 0.068(10) -0.007(7) -0.002(6) 0.001(6) N5 0.094(10) 0.059(9) 0.091(11) -0.013(8) 0.023(8) 0.019(7) N5' 0.077(8) 0.035(7) 0.073(9) -0.001(7) 0.010(6) 0.023(6) N6 0.060(4) 0.080(4) 0.126(6) 0.026(4) 0.048(4) -0.014(4) N7 0.066(4) 0.087(4) 0.137(7) 0.027(5) 0.042(5) -0.017(5) N8 0.071(6) 0.095(6) 0.149(8) 0.026(6) 0.035(6) -0.017(6) N7' 0.070(5) 0.095(5) 0.134(7) 0.026(5) 0.044(5) -0.014(5) N8' 0.079(6) 0.107(6) 0.141(9) 0.024(7) 0.040(7) -0.012(6) N9 0.071(8) 0.096(8) 0.088(8) 0.004(7) 0.034(7) -0.033(7) O1 0.025(2) 0.030(2) 0.132(5) 0.005(3) 0.015(3) 0.0021(18) O2 0.025(2) 0.032(2) 0.072(3) -0.002(2) 0.016(2) -0.0060(16) O3 0.018(2) 0.034(2) 0.077(3) 0.000(2) 0.019(2) 0.0001(16) O4 0.042(3) 0.041(3) 0.132(6) -0.003(3) -0.021(3) 0.012(2) O5 0.044(3) 0.054(3) 0.087(4) 0.032(3) 0.013(3) -0.007(2) O6 0.026(2) 0.035(2) 0.075(3) 0.004(2) 0.017(2) -0.0028(17) O7 0.027(2) 0.031(2) 0.054(3) 0.0023(19) 0.009(2) -0.0063(16) O8 0.059(4) 0.084(4) 0.106(5) 0.052(4) 0.017(4) 0.001(3) O9 0.020(2) 0.028(2) 0.077(3) 0.008(2) 0.008(2) -0.0036(15) O10 0.031(2) 0.034(2) 0.110(4) 0.012(2) 0.020(3) -0.0092(18) O11 0.021(2) 0.034(2) 0.066(3) -0.001(2) 0.015(2) -0.0009(16) O12 0.025(2) 0.035(2) 0.051(3) -0.0005(18) 0.009(2) 0.0005(16) O13 0.031(3) 0.076(3) 0.066(4) -0.019(3) 0.005(2) -0.008(2) O14 0.025(4) 0.042(5) 0.044(5) -0.002(3) 0.012(3) -0.001(3) O14' 0.016(6) 0.047(9) 0.063(11) 0.003(7) 0.015(7) 0.003(6) O15 0.022(2) 0.068(3) 0.092(4) -0.012(3) 0.017(2) -0.003(2) O16 0.040(5) 0.029(4) 0.053(6) 0.004(4) 0.010(4) 0.002(3) O16' 0.021(7) 0.026(7) 0.057(12) 0.010(8) -0.003(7) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O15 2.162(5) . ? Dy1 O16 2.233(10) 3_676 ? Dy1 O14' 2.272(16) 3_676 ? Dy1 O7 2.316(4) . ? Dy1 O3 2.336(4) . ? Dy1 O16' 2.338(18) 3_676 ? Dy1 O12 2.353(4) . ? Dy1 O13 2.460(5) . ? Dy1 O14 2.492(8) 3_676 ? Dy1 C39 2.955(7) . ? Dy1 Fe3 3.2665(10) . ? Dy1 Dy1 3.9783(8) 3_676 ? Fe1 O1 1.868(5) . ? Fe1 O2 2.000(5) . ? Fe1 O10 2.038(6) . ? Fe1 N3 2.057(7) . ? Fe1 N1 2.149(6) . ? Fe1 O9 2.187(4) . ? Fe1 Na1 3.55(2) . ? Fe2 N6 1.910(7) . ? Fe2 O5 1.958(5) . ? Fe2 O10 2.046(5) . ? Fe2 O6 2.064(5) . ? Fe2 O9 2.137(5) . ? Fe2 N2 2.154(6) . ? Fe2 Na1' 3.28(2) . ? Fe2 Na1 3.43(2) . ? Fe3 O3 1.906(4) . ? Fe3 O11 1.992(4) . ? Fe3 O6 1.996(5) . ? Fe3 O7 2.008(4) . ? Fe3 O2 2.050(4) . ? Fe3 O9 2.130(4) . ? Na1 O4 2.18(3) . ? Na1 O1 2.36(2) . ? Na1 N5 2.39(3) 4_576 ? Na1 O5 2.589(19) . ? Na1 O10 2.63(3) . ? Na1 O8 2.861(18) . ? Na1' O5 2.184(19) . ? Na1' N5' 2.36(2) 4_576 ? Na1' O8 2.390(18) . ? Na1' O4 2.40(2) . ? Na1' O1 2.727(19) . ? Na1' O10 2.80(2) . ? C1 O1 1.182(6) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 C7 1.4837 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 O4 1.467(9) . ? C7 N1 1.206(7) . ? C7 H7 0.9300 . ? C8 C9 1.433(9) . ? C8 C10 1.539(8) . ? C8 N1 1.558(10) . ? C8 C11 1.595(10) . ? C9 O2 1.526(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O3 1.511(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12' 1.49(3) . ? C11 C12 1.520(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13 O4 1.576(15) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C13' O4 1.493(15) . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C14 O5 1.413(7) . ? C15 C16 1.3900 . ? C15 C20 1.4450 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 O8 1.354(8) . ? C20 N2 1.326(8) . ? C20 H20 0.9300 . ? C21 N2 1.478(8) . ? C21 C23 1.535(9) . ? C21 C22 1.547(10) . ? C21 C24 1.558(10) . ? C22 O6 1.436(8) . ? C23 O7 1.448(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.562(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O8 1.53(2) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C26' O8 1.52(2) . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? C27 O9 1.388(7) . ? C28 O10 1.41(2) . ? C28' O10 1.46(2) . ? C29 O12 1.190(7) . ? C29 O11 1.287(7) . ? C29 C30 1.541(9) . ? C30 C33 1.460(10) . ? C30 C32 1.504(9) . ? C30 C31 1.548(10) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O13 1.214(8) . ? C34 O14' 1.263(17) . ? C34 O14 1.347(10) . ? C34 C35 1.52(2) . ? C34 C35' 1.67(3) . ? C35 C36 1.41(3) . ? C35 C37 1.57(2) . ? C35 C38 1.62(3) . ? C35' C37' 1.44(4) . ? C35' C38' 1.45(3) . ? C35' C36' 1.52(4) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C36' H36D 0.9600 . ? C36' H36E 0.9600 . ? C36' H36F 0.9600 . ? C37' H37D 0.9600 . ? C37' H37E 0.9600 . ? C37' H37F 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C38' H38D 0.9600 . ? C38' H38E 0.9600 . ? C38' H38F 0.9600 . ? C39 O15 1.184(8) . ? C39 O16 1.228(11) . ? C39 O16' 1.398(17) . ? C39 C40 1.445(15) . ? C39 C40' 1.455(13) . ? C40 C43 1.468(18) . ? C40 C41 1.521(17) . ? C40 C42 1.78(3) . ? C40' C41' 1.519(17) . ? C40' C42' 1.54(3) . ? C40' C43' 1.55(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C41' H41D 0.9600 . ? C41' H41E 0.9600 . ? C41' H41F 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C42' H42D 0.9600 . ? C42' H42E 0.9600 . ? C42' H42F 0.9600 . ? C43' H43D 0.9600 . ? C43' H43E 0.9600 . ? C43' H43F 0.9600 . ? C44 N9 1.032(18) . ? C44 C45 1.40(2) . ? N3 N4 1.181(8) . ? N3 N4' 1.206(19) . ? N4 N5 1.193(8) . ? N4' N5' 1.16(2) . ? N5 Na1 2.39(3) 4_575 ? N5' Na1' 2.36(2) 4_575 ? N6 N7 1.029(16) . ? N6 N7' 1.200(8) . ? N7 N8 1.132(19) . ? N7' N8' 1.215(9) . ? O14 Dy1 2.492(8) 3_676 ? O14' Dy1 2.272(16) 3_676 ? O16 Dy1 2.233(10) 3_676 ? O16' Dy1 2.338(18) 3_676 ? 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 O15 Dy1 O16 125.0(3) . 3_676 ? O15 Dy1 O14' 86.9(4) . 3_676 ? O16 Dy1 O14' 60.8(5) 3_676 3_676 ? O15 Dy1 O7 112.33(18) . . ? O16 Dy1 O7 110.3(3) 3_676 . ? O14' Dy1 O7 159.0(3) 3_676 . ? O15 Dy1 O3 73.09(16) . . ? O16 Dy1 O3 155.2(3) 3_676 . ? O14' Dy1 O3 108.5(4) 3_676 . ? O7 Dy1 O3 71.29(15) . . ? O15 Dy1 O16' 134.0(4) . 3_676 ? O16 Dy1 O16' 19.2(4) 3_676 3_676 ? O14' Dy1 O16' 79.9(6) 3_676 3_676 ? O7 Dy1 O16' 91.6(4) . 3_676 ? O3 Dy1 O16' 152.8(4) . 3_676 ? O15 Dy1 O12 135.51(18) . . ? O16 Dy1 O12 80.9(3) 3_676 . ? O14' Dy1 O12 75.3(4) 3_676 . ? O7 Dy1 O12 84.71(15) . . ? O3 Dy1 O12 74.63(14) . . ? O16' Dy1 O12 83.1(4) 3_676 . ? O15 Dy1 O13 82.3(2) . . ? O16 Dy1 O13 82.4(3) 3_676 . ? O14' Dy1 O13 124.7(4) 3_676 . ? O7 Dy1 O13 68.68(16) . . ? O3 Dy1 O13 119.36(18) . . ? O16' Dy1 O13 70.3(4) 3_676 . ? O12 Dy1 O13 141.05(16) . . ? O15 Dy1 O14 77.7(2) . 3_676 ? O16 Dy1 O14 79.0(3) 3_676 3_676 ? O14' Dy1 O14 18.6(3) 3_676 3_676 ? O7 Dy1 O14 154.1(2) . 3_676 ? O3 Dy1 O14 90.3(2) . 3_676 ? O16' Dy1 O14 97.8(5) 3_676 3_676 ? O12 Dy1 O14 72.7(2) . 3_676 ? O13 Dy1 O14 137.2(2) . 3_676 ? O15 Dy1 C39 20.02(18) . . ? O16 Dy1 C39 105.1(3) 3_676 . ? O14' Dy1 C39 72.8(4) 3_676 . ? O7 Dy1 C39 127.90(18) . . ? O3 Dy1 C39 91.33(15) . . ? O16' Dy1 C39 115.8(4) 3_676 . ? O12 Dy1 C39 138.7(2) . . ? O13 Dy1 C39 79.7(2) . . ? O14 Dy1 C39 68.7(2) 3_676 . ? O15 Dy1 Fe3 98.35(14) . . ? O16 Dy1 Fe3 136.3(3) 3_676 . ? O14' Dy1 Fe3 135.0(4) 3_676 . ? O7 Dy1 Fe3 37.51(10) . . ? O3 Dy1 Fe3 35.06(11) . . ? O16' Dy1 Fe3 122.0(4) 3_676 . ? O12 Dy1 Fe3 69.92(9) . . ? O13 Dy1 Fe3 100.30(13) . . ? O14 Dy1 Fe3 119.66(18) 3_676 . ? C39 Dy1 Fe3 118.37(12) . . ? O15 Dy1 Dy1 77.13(14) . 3_676 ? O16 Dy1 Dy1 47.9(3) 3_676 3_676 ? O14' Dy1 Dy1 52.7(4) 3_676 3_676 ? O7 Dy1 Dy1 137.52(10) . 3_676 ? O3 Dy1 Dy1 145.70(10) . 3_676 ? O16' Dy1 Dy1 59.8(4) 3_676 3_676 ? O12 Dy1 Dy1 118.39(9) . 3_676 ? O13 Dy1 Dy1 72.07(13) . 3_676 ? O14 Dy1 Dy1 66.82(18) 3_676 3_676 ? C39 Dy1 Dy1 57.32(12) . 3_676 ? Fe3 Dy1 Dy1 171.46(2) . 3_676 ? O1 Fe1 O2 163.12(18) . . ? O1 Fe1 O10 85.0(2) . . ? O2 Fe1 O10 105.47(19) . . ? O1 Fe1 N3 99.4(2) . . ? O2 Fe1 N3 91.5(2) . . ? O10 Fe1 N3 101.8(3) . . ? O1 Fe1 N1 96.8(2) . . ? O2 Fe1 N1 70.79(19) . . ? O10 Fe1 N1 170.93(19) . . ? N3 Fe1 N1 86.7(3) . . ? O1 Fe1 O9 88.0(2) . . ? O2 Fe1 O9 82.90(17) . . ? O10 Fe1 O9 72.12(18) . . ? N3 Fe1 O9 170.1(2) . . ? N1 Fe1 O9 99.02(18) . . ? O1 Fe1 Na1 37.7(4) . . ? O2 Fe1 Na1 150.5(4) . . ? O10 Fe1 Na1 47.3(4) . . ? N3 Fe1 Na1 103.9(3) . . ? N1 Fe1 Na1 134.0(4) . . ? O9 Fe1 Na1 77.9(3) . . ? N6 Fe2 O5 89.9(3) . . ? N6 Fe2 O10 99.4(3) . . ? O5 Fe2 O10 98.3(2) . . ? N6 Fe2 O6 102.0(3) . . ? O5 Fe2 O6 162.04(18) . . ? O10 Fe2 O6 93.1(2) . . ? N6 Fe2 O9 168.4(3) . . ? O5 Fe2 O9 99.8(2) . . ? O10 Fe2 O9 73.03(18) . . ? O6 Fe2 O9 70.23(16) . . ? N6 Fe2 N2 92.0(3) . . ? O5 Fe2 N2 84.7(2) . . ? O10 Fe2 N2 168.2(2) . . ? O6 Fe2 N2 81.5(2) . . ? O9 Fe2 N2 95.23(18) . . ? N6 Fe2 Na1' 97.7(4) . . ? O5 Fe2 Na1' 40.2(3) . . ? O10 Fe2 Na1' 58.1(3) . . ? O6 Fe2 Na1' 147.5(3) . . ? O9 Fe2 Na1' 85.8(3) . . ? N2 Fe2 Na1' 123.6(3) . . ? N6 Fe2 Na1 100.8(5) . . ? O5 Fe2 Na1 48.5(3) . . ? O10 Fe2 Na1 50.0(3) . . ? O6 Fe2 Na1 139.3(3) . . ? O9 Fe2 Na1 81.3(4) . . ? N2 Fe2 Na1 130.8(3) . . ? Na1' Fe2 Na1 8.5(5) . . ? O3 Fe3 O11 86.49(18) . . ? O3 Fe3 O6 171.1(2) . . ? O11 Fe3 O6 101.41(18) . . ? O3 Fe3 O7 87.63(18) . . ? O11 Fe3 O7 96.31(17) . . ? O6 Fe3 O7 87.53(18) . . ? O3 Fe3 O2 89.33(18) . . ? O11 Fe3 O2 90.43(18) . . ? O6 Fe3 O2 94.55(18) . . ? O7 Fe3 O2 172.43(17) . . ? O3 Fe3 O9 101.00(17) . . ? O11 Fe3 O9 170.05(15) . . ? O6 Fe3 O9 71.64(17) . . ? O7 Fe3 O9 90.58(17) . . ? O2 Fe3 O9 83.19(18) . . ? O3 Fe3 Dy1 44.74(12) . . ? O11 Fe3 Dy1 82.24(11) . . ? O6 Fe3 Dy1 131.79(13) . . ? O7 Fe3 Dy1 44.62(12) . . ? O2 Fe3 Dy1 133.65(13) . . ? O9 Fe3 Dy1 107.68(11) . . ? O4 Na1 O1 69.8(7) . . ? O4 Na1 N5 109.5(12) . 4_576 ? O1 Na1 N5 156.0(9) . 4_576 ? O4 Na1 O5 125.3(9) . . ? O1 Na1 O5 102.9(9) . . ? N5 Na1 O5 96.7(9) 4_576 . ? O4 Na1 O10 133.3(9) . . ? O1 Na1 O10 63.6(6) . . ? N5 Na1 O10 111.3(11) 4_576 . ? O5 Na1 O10 70.9(6) . . ? O4 Na1 O8 90.4(8) . . ? O1 Na1 O8 135.6(9) . . ? N5 Na1 O8 67.4(7) 4_576 . ? O5 Na1 O8 56.3(3) . . ? O10 Na1 O8 125.9(7) . . ? O4 Na1 Fe2 138.4(9) . . ? O1 Na1 Fe2 80.9(7) . . ? N5 Na1 Fe2 109.2(10) 4_576 . ? O5 Na1 Fe2 34.5(3) . . ? O10 Na1 Fe2 36.5(3) . . ? O8 Na1 Fe2 90.5(5) . . ? O4 Na1 Fe1 98.7(7) . . ? O1 Na1 Fe1 28.9(3) . . ? N5 Na1 Fe1 140.8(10) 4_576 . ? O5 Na1 Fe1 88.2(7) . . ? O10 Na1 Fe1 34.7(3) . . ? O8 Na1 Fe1 140.6(7) . . ? Fe2 Na1 Fe1 57.8(4) . . ? O5 Na1' N5' 124.6(10) . 4_576 ? O5 Na1' O8 68.6(4) . . ? N5' Na1' O8 91.2(8) 4_576 . ? O5 Na1' O4 135.3(8) . . ? N5' Na1' O4 97.0(9) 4_576 . ? O8 Na1' O4 97.7(8) . . ? O5 Na1' O1 103.7(8) . . ? N5' Na1' O1 120.3(7) 4_576 . ? O8 Na1' O1 142.2(8) . . ? O4 Na1' O1 60.7(4) . . ? O5 Na1' O10 73.7(7) . . ? N5' Na1' O10 102.2(8) 4_576 . ? O8 Na1' O10 141.0(8) . . ? O4 Na1' O10 116.3(7) . . ? O1 Na1' O10 57.1(4) . . ? O5 Na1' Fe2 35.4(4) . . ? N5' Na1' Fe2 120.8(9) 4_576 . ? O8 Na1' Fe2 103.7(6) . . ? O4 Na1' Fe2 135.5(8) . . ? O1 Na1' Fe2 79.1(5) . . ? O10 Na1' Fe2 38.4(3) . . ? O1 C1 C2 126.2(4) . . ? O1 C1 C6 113.8(4) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 C7 108.8 . . ? C1 C2 C7 131.2 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 O4 120.0(3) . . ? C1 C6 O4 120.0(3) . . ? N1 C7 C2 121.5(4) . . ? N1 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? C9 C8 C10 108.0(5) . . ? C9 C8 N1 99.0(6) . . ? C10 C8 N1 107.3(6) . . ? C9 C8 C11 110.2(6) . . ? C10 C8 C11 110.3(6) . . ? N1 C8 C11 120.9(6) . . ? C8 C9 O2 110.8(6) . . ? C8 C9 H9A 109.5 . . ? O2 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O3 C10 C8 116.6(5) . . ? O3 C10 H10A 108.1 . . ? C8 C10 H10A 108.1 . . ? O3 C10 H10B 108.1 . . ? C8 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? C12' C11 C12 101.9(14) . . ? C12' C11 C8 115.0(13) . . ? C12 C11 C8 120.1(7) . . ? C12' C11 H11A 7.7 . . ? C12 C11 H11A 107.3 . . ? C8 C11 H11A 107.3 . . ? C12' C11 H11B 103.9 . . ? C12 C11 H11B 107.3 . . ? C8 C11 H11B 107.3 . . ? H11A C11 H11B 106.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12' H12D 109.5 . . ? C11 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C13' H13D 109.5 . . ? O4 C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? O4 C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C15 C14 C19 120.0 . . ? C15 C14 O5 123.7(3) . . ? C19 C14 O5 116.3(3) . . ? C16 C15 C14 120.0 . . ? C16 C15 C20 118.4 . . ? C14 C15 C20 121.6 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? O8 C19 C18 125.3(4) . . ? O8 C19 C14 114.7(4) . . ? C18 C19 C14 120.0 . . ? N2 C20 C15 127.3(4) . . ? N2 C20 H20 116.4 . . ? C15 C20 H20 116.4 . . ? N2 C21 C23 115.0(5) . . ? N2 C21 C22 105.4(5) . . ? C23 C21 C22 102.4(6) . . ? N2 C21 C24 107.7(6) . . ? C23 C21 C24 109.3(5) . . ? C22 C21 C24 117.2(6) . . ? O6 C22 C21 116.8(5) . . ? O7 C23 C21 115.8(5) . . ? O7 C23 H23A 108.3 . . ? C21 C23 H23A 108.3 . . ? O7 C23 H23B 108.3 . . ? C21 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C21 C24 C25 117.8(6) . . ? C21 C24 H24A 107.9 . . ? C25 C24 H24A 107.9 . . ? C21 C24 H24B 107.9 . . ? C25 C24 H24B 107.9 . . ? H24A C24 H24B 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O8 C26 H26A 109.5 . . ? O8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C26' H26D 109.5 . . ? O8 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? O8 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? O12 C29 O11 125.6(6) . . ? O12 C29 C30 116.4(5) . . ? O11 C29 C30 118.1(5) . . ? C33 C30 C32 111.4(7) . . ? C33 C30 C29 98.8(6) . . ? C32 C30 C29 114.6(5) . . ? C33 C30 C31 114.7(8) . . ? C32 C30 C31 106.6(7) . . ? C29 C30 C31 110.9(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O13 C34 O14' 101.6(9) . . ? O13 C34 O14 127.1(7) . . ? O14' C34 O14 35.5(6) . . ? O13 C34 C35 118.4(9) . . ? O14' C34 C35 131.6(11) . . ? O14 C34 C35 114.6(9) . . ? O13 C34 C35' 120.2(11) . . ? O14' C34 C35' 138.0(13) . . ? O14 C34 C35' 109.0(11) . . ? C35 C34 C35' 21.8(10) . . ? C36 C35 C34 127.3(16) . . ? C36 C35 C37 108.3(17) . . ? C34 C35 C37 117.0(13) . . ? C36 C35 C38 104.2(16) . . ? C34 C35 C38 95.4(14) . . ? C37 C35 C38 97.7(15) . . ? C37' C35' C38' 115(3) . . ? C37' C35' C36' 101(2) . . ? C38' C35' C36' 103.6(19) . . ? C37' C35' C34 106.1(19) . . ? C38' C35' C34 122.0(18) . . ? C36' C35' C34 107(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35' C36' H36D 109.5 . . ? C35' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C35' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C35' C37' H37D 109.5 . . ? C35' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C35' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35' C38' H38D 109.5 . . ? C35' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C35' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? O15 C39 O16 116.5(8) . . ? O15 C39 O16' 136.4(9) . . ? O16 C39 O16' 33.2(7) . . ? O15 C39 C40 120.1(8) . . ? O16 C39 C40 122.3(9) . . ? O16' C39 C40 93.1(11) . . ? O15 C39 C40' 108.3(8) . . ? O16 C39 C40' 125.3(9) . . ? O16' C39 C40' 115.3(10) . . ? C40 C39 C40' 41.8(8) . . ? O15 C39 Dy1 38.7(3) . . ? O16 C39 Dy1 79.4(6) . . ? O16' C39 Dy1 98.7(7) . . ? C40 C39 Dy1 149.4(7) . . ? C40' C39 Dy1 145.1(7) . . ? C39 C40 C43 101.2(10) . . ? C39 C40 C41 112.7(12) . . ? C43 C40 C41 112.5(14) . . ? C39 C40 C42 98.2(12) . . ? C43 C40 C42 111.0(13) . . ? C41 C40 C42 119.0(13) . . ? C39 C40' C41' 110.4(12) . . ? C39 C40' C42' 108.3(14) . . ? C41' C40' C42' 127.5(16) . . ? C39 C40' C43' 103.2(17) . . ? C41' C40' C43' 118(2) . . ? C42' C40' C43' 84.7(19) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40' C41' H41D 109.5 . . ? C40' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C40' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40' C42' H42D 109.5 . . ? C40' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C40' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? C40' C43' H43D 109.5 . . ? C40' C43' H43E 109.5 . . ? H43D C43' H43E 109.5 . . ? C40' C43' H43F 109.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? N9 C44 C45 171.2(19) . . ? C7 N1 C8 117.2(6) . . ? C7 N1 Fe1 119.4(5) . . ? C8 N1 Fe1 123.4(4) . . ? C20 N2 C21 118.9(5) . . ? C20 N2 Fe2 128.0(4) . . ? C21 N2 Fe2 113.1(4) . . ? N4 N3 N4' 21(2) . . ? N4 N3 Fe1 126.4(15) . . ? N4' N3 Fe1 127.4(12) . . ? N3 N4 N5 172(3) . . ? N5' N4' N3 175(3) . . ? N4 N5 Na1 156(2) . 4_575 ? N4' N5' Na1' 157(2) . 4_575 ? N7 N6 N7' 88.2(15) . . ? N7 N6 Fe2 120.8(11) . . ? N7' N6 Fe2 143.8(12) . . ? N6 N7 N8 174(2) . . ? N6 N7' N8' 172(2) . . ? C1 O1 Fe1 124.7(5) . . ? C1 O1 Na1 121.7(8) . . ? Fe1 O1 Na1 113.4(7) . . ? C1 O1 Na1' 121.3(6) . . ? Fe1 O1 Na1' 112.5(5) . . ? Na1 O1 Na1' 8.4(7) . . ? C9 O2 Fe1 116.7(4) . . ? C9 O2 Fe3 118.4(3) . . ? Fe1 O2 Fe3 100.9(2) . . ? C10 O3 Fe3 130.2(3) . . ? C10 O3 Dy1 125.5(3) . . ? Fe3 O3 Dy1 100.20(19) . . ? C6 O4 C13' 115.5(10) . . ? C6 O4 C13 137.5(8) . . ? C13' O4 C13 22.6(9) . . ? C6 O4 Na1 113.7(7) . . ? C13' O4 Na1 130.8(12) . . ? C13 O4 Na1 108.6(10) . . ? C6 O4 Na1' 119.0(6) . . ? C13' O4 Na1' 124.6(11) . . ? C13 O4 Na1' 102.0(9) . . ? Na1 O4 Na1' 11.8(7) . . ? C14 O5 Fe2 134.7(4) . . ? C14 O5 Na1' 119.9(6) . . ? Fe2 O5 Na1' 104.4(6) . . ? C14 O5 Na1 126.7(6) . . ? Fe2 O5 Na1 97.0(6) . . ? Na1' O5 Na1 7.8(10) . . ? C22 O6 Fe3 114.8(4) . . ? C22 O6 Fe2 104.6(4) . . ? Fe3 O6 Fe2 112.96(19) . . ? C23 O7 Fe3 134.0(3) . . ? C23 O7 Dy1 125.1(3) . . ? Fe3 O7 Dy1 97.87(18) . . ? C19 O8 C26' 126.7(11) . . ? C19 O8 C26 103.6(9) . . ? C26' O8 C26 24.5(9) . . ? C19 O8 Na1' 115.5(6) . . ? C26' O8 Na1' 117.2(11) . . ? C26 O8 Na1' 140.9(10) . . ? C19 O8 Na1 119.5(6) . . ? C26' O8 Na1 112.9(11) . . ? C26 O8 Na1 136.9(10) . . ? Na1' O8 Na1 4.7(10) . . ? C27 O9 Fe3 116.3(4) . . ? C27 O9 Fe2 114.0(4) . . ? Fe3 O9 Fe2 105.01(17) . . ? C27 O9 Fe1 123.0(4) . . ? Fe3 O9 Fe1 92.71(18) . . ? Fe2 O9 Fe1 102.61(16) . . ? C28 O10 C28' 25.3(10) . . ? C28 O10 Fe1 129.5(10) . . ? C28' O10 Fe1 107.3(9) . . ? C28 O10 Fe2 116.8(11) . . ? C28' O10 Fe2 130.5(10) . . ? Fe1 O10 Fe2 111.46(19) . . ? C28 O10 Na1 93.0(11) . . ? C28' O10 Na1 110.5(10) . . ? Fe1 O10 Na1 98.0(5) . . ? Fe2 O10 Na1 93.5(4) . . ? C28 O10 Na1' 94.9(10) . . ? C28' O10 Na1' 115.3(10) . . ? Fe1 O10 Na1' 104.4(4) . . ? Fe2 O10 Na1' 83.5(4) . . ? Na1 O10 Na1' 10.4(6) . . ? C29 O11 Fe3 130.0(4) . . ? C29 O12 Dy1 132.3(4) . . ? C34 O13 Dy1 131.7(5) . . ? C34 O14 Dy1 131.3(6) . 3_676 ? C34 O14' Dy1 173.5(11) . 3_676 ? C39 O15 Dy1 121.3(5) . . ? C39 O16 Dy1 168.4(8) . 3_676 ? C39 O16' Dy1 132.8(12) . 3_676 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.068 _refine_diff_density_min -1.489 _refine_diff_density_rms 0.116 _iucr_refine_instructions_details ; TITL p21c in P2(1)/c CELL 0.71073 12.4076 41.8973 13.4195 90.000 114.038 90.000 ZERR 2.00 0.0025 0.0084 0.0027 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Na Fe Dy UNIT 176 286 34 74 4 12 4 omit 0 50 omit -1 6 2 omit 2 5 1 omit -3 4 3 omit 5 8 0 omit 0 5 1 omit 1 8 0 omit -2 6 2 omit 0 7 2 omit 0 4 3 omit 3 3 1 omit -1 8 1 omit -2 15 4 omit -2 4 2 omit 3 1 2 omit -6 1 4 omit -2 4 3 omit -2 14 1 omit 3 4 0 omit 1 11 0 omit 5 1 0 omit 1 4 1 omit 2 5 0 omit 2 7 1 omit 3 10 1 omit 1 3 2 omit 1 14 3 omit -2 13 1 omit 1 9 2 omit -3 7 1 omit -1 8 3 omit 2 4 2 omit -3 13 2 omit -4 4 3 omit -2 1 2 omit -1 13 2 omit 4 8 1 omit -1 6 3 omit -2 7 3 omit -3 2 1 omit 3 12 1 omit 2 0 0 omit 2 1 0 omit -3 11 1 omit 2 14 0 omit -1 12 5 omit 1 4 2 omit 3 8 0 omit -5 2 3 omit 0 5 2 omit -2 1 1 omit 0 9 2 omit -5 12 3 omit -3 0 4 omit 4 5 2 omit 3 7 0 omit -4 1 1 omit -5 7 2 omit 5 6 0 omit -1 8 5 omit -3 0 2 omit 2 1 3 omit -2 2 3 omit 3 5 1 omit -4 4 1 omit -2 8 2 omit -4 9 1 omit 0 11 2 omit 2 5 2 omit 2 11 0 omit -3 7 2 omit 3 12 0 L.S. 10 BOND $h acta htab free na1 c13 free c6 na1 free c28 na1 free c14 na1' delu 0.02 o10 c28 delu 0.002 c30 c31 delu 0.02 c30 c33 dfix 1.40 0.02 c40 c41 c40' c41' dfix 1.35 0.02 c7 c2 c7 n1 dfix 1.55 0.02 o4 c13 o4 c13' dfix 1.40 0.02 c11 c8 c11 c12 dfix 1.40 0.02 c30 c31 c30 c32 c30 c33 dfix 1.10 0.01 n4 n5 dfix 1.10 0.01 n3 n4 dfix 2.40 0.005 n3 n5 dfix 1.20 0.01 n7' n8' dfix 1.20 0.01 n7' n6 dfix 2.40 0.01 n6 n8' isor 0.01 0.01 c42 c43 c42' c43' isor 0.01 0.01 c4 c5 c12' c13 c13' c11 C41 c41' isor 0.01 0.01 c25 c26 c26' c28 c28' c31 c32 c33 C45 isor 0.01 0.01 n9 N3 N4 N4' N5' N5 SIMU 0.01 0.01 1.7 c35 c36 c37 c38 SIMU 0.01 0.01 1.7 C35' C36' C37' C38' SIMU 0.005 0.005 1.7 N6 N7 N7' N8 N8' FMAP 2 PLAN -20 WGHT 0.0788 10.8699 FVAR 1.52231 DY1 7 0.395878 0.962157 0.477569 11.00000 0.02222 0.02628 = 0.05047 0.00443 0.00763 -0.00131 FE1 6 0.335401 0.825505 0.500629 11.00000 0.02817 0.02447 = 0.08962 -0.00002 0.01313 -0.00315 FE2 6 0.267916 0.856297 0.700514 11.00000 0.03603 0.03815 = 0.07633 0.01529 0.01678 -0.00720 FE3 6 0.252865 0.896620 0.476620 11.00000 0.02225 0.02755 = 0.05999 0.00263 0.01111 -0.00226 PART 1 NA1 5 0.447878 0.790463 0.764050 10.50000 0.05705 0.05306 = 0.06303 0.01323 0.01607 0.00752 PART 2 NA1' 5 0.452255 0.796790 0.798718 10.50000 0.04544 0.03411 = 0.08010 0.01686 0.02032 -0.00162 PART 0 AFIX 66 C1 1 0.564119 0.806226 0.600377 11.00000 0.05121 0.02081 = 0.10646 -0.00607 0.02190 -0.00267 C2 1 0.591128 0.819310 0.518137 11.00000 0.02281 0.03694 = 0.14528 -0.03928 0.00571 0.00256 C3 1 0.704958 0.816798 0.523214 11.00000 0.04323 0.05959 = 0.14217 -0.04207 0.03839 -0.00281 AFIX 41 H3 2 0.723028 0.825552 0.468190 11.00000 10.10000 AFIX 65 C4 1 0.791780 0.801201 0.610530 11.00000 0.06446 0.08485 = 0.12537 -0.02720 0.02455 0.01575 AFIX 41 H4 2 0.867939 0.799521 0.613927 11.00000 10.10000 AFIX 65 C5 1 0.764772 0.788117 0.692771 11.00000 0.04518 0.06170 = 0.11626 -0.03872 -0.00771 0.02025 AFIX 41 H5 2 0.822861 0.777682 0.751191 11.00000 10.10000 AFIX 65 C6 1 0.650942 0.790629 0.687696 11.00000 0.04330 0.03605 = 0.11845 -0.01560 0.00776 -0.00174 C7 1 0.517881 0.837578 0.418820 11.00000 0.03672 0.02660 = 0.11443 -0.02260 0.03116 -0.00752 AFIX 41 H7 2 0.552492 0.845457 0.374033 11.00000 10.10000 AFIX 0 C8 1 0.345490 0.861433 0.287772 11.00000 0.03235 0.04335 = 0.07928 -0.00519 0.02240 -0.00523 C9 1 0.227655 0.855596 0.277555 11.00000 0.03656 0.03739 = 0.08535 -0.01282 0.02306 -0.00698 AFIX 21 H9A 2 0.200158 0.835325 0.241119 11.00000 10.10000 H9B 2 0.175728 0.872209 0.233258 11.00000 10.10000 AFIX 0 C10 1 0.372937 0.897041 0.313925 11.00000 0.03191 0.02932 = 0.08110 -0.00104 0.02323 -0.00134 AFIX 21 H10A 2 0.453957 0.900823 0.324316 11.00000 10.10000 H10B 2 0.322759 0.909321 0.250758 11.00000 10.10000 AFIX 0 C11 1 0.356956 0.852395 0.177048 11.00000 0.05312 0.05564 = 0.09409 -0.01205 0.03512 -0.00555 AFIX 21 H11A 2 0.293228 0.863071 0.118146 11.00000 10.10000 H11B 2 0.430053 0.861649 0.180490 11.00000 10.10000 AFIX 0 part 1 C12 1 0.355582 0.817603 0.144336 10.75000 0.04985 0.06734 = 0.09216 -0.03465 0.03977 -0.01278 AFIX 31 H12A 2 0.362846 0.816372 0.075901 10.75000 10.10000 H12B 2 0.282657 0.807921 0.137165 10.75000 10.10000 H12C 2 0.420375 0.806550 0.199287 10.75000 10.10000 AFIX 0 part 2 C12' 1 0.265239 0.866547 0.076876 10.25000 0.06517 0.06763 = 0.05625 0.00161 0.02904 0.00480 AFIX 31 H12D 2 0.278106 0.859714 0.014310 10.25000 10.10000 H12E 2 0.269736 0.889403 0.081903 10.25000 10.10000 H12F 2 0.188611 0.859669 0.069688 10.25000 10.10000 AFIX 0 part 0 PART 1 C13 1 0.688060 0.757556 0.883513 10.50000 0.04355 0.05797 = 0.07013 -0.01293 0.01597 0.02932 AFIX 31 H13A 2 0.635137 0.753984 0.918318 10.50000 10.10000 H13B 2 0.755769 0.769208 0.931939 10.50000 10.10000 H13C 2 0.712880 0.737410 0.865990 10.50000 10.10000 AFIX 0 PART 2 C13' 1 0.716235 0.756723 0.855644 10.50000 0.05580 0.06462 = 0.06699 0.00810 0.01463 0.01555 AFIX 31 H13D 2 0.690426 0.749335 0.910038 10.50000 10.10000 H13E 2 0.787678 0.768803 0.890020 10.50000 10.10000 H13F 2 0.730555 0.738748 0.818352 10.50000 10.10000 AFIX 66 PART 0 C14 1 0.464652 0.858142 0.936977 11.00000 0.04631 0.07073 = 0.06955 0.03072 0.02007 -0.01024 C15 1 0.454418 0.890308 0.956972 11.00000 0.04973 0.07383 = 0.05303 0.01597 0.02108 -0.01812 C16 1 0.525758 0.903484 1.057377 11.00000 0.06514 0.09920 = 0.05478 0.01184 0.02613 -0.00599 AFIX 41 H16 2 0.518911 0.925005 1.070755 11.00000 10.10000 AFIX 65 C17 1 0.607332 0.884494 1.137789 11.00000 0.04381 0.17090 = 0.04939 0.01160 0.01338 -0.02118 AFIX 41 H17 2 0.655063 0.893310 1.204968 11.00000 10.10000 AFIX 65 C18 1 0.617567 0.852328 1.117796 11.00000 0.05236 0.11085 = 0.08485 0.04512 0.02824 0.01065 AFIX 41 H18 2 0.672145 0.839623 1.171597 11.00000 10.10000 AFIX 65 C19 1 0.546228 0.839152 1.017390 11.00000 0.05335 0.09609 = 0.06796 0.03878 0.02044 -0.00824 C20 1 0.368768 0.910644 0.876406 11.00000 0.04947 0.06127 = 0.05389 0.01240 0.02310 -0.01070 AFIX 41 H20 2 0.367582 0.931888 0.896030 11.00000 10.10000 AFIX 0 C21 1 0.211307 0.926989 0.706879 11.00000 0.04272 0.03606 = 0.06313 0.00330 0.02656 -0.00273 C22 1 0.120626 0.908535 0.608636 11.00000 0.03163 0.04759 = 0.07579 -0.00338 0.02329 -0.00109 C23 1 0.267200 0.949735 0.651736 11.00000 0.03918 0.04078 = 0.05051 -0.00130 0.01914 -0.00658 AFIX 21 H23A 2 0.210802 0.966489 0.615640 11.00000 10.10000 H23B 2 0.335365 0.959729 0.708036 11.00000 10.10000 AFIX 0 C24 1 0.162533 0.946673 0.778011 11.00000 0.05568 0.05698 = 0.07129 -0.00484 0.03493 -0.00915 AFIX 21 H24A 2 0.095749 0.959016 0.729204 11.00000 10.10000 H24B 2 0.223069 0.961739 0.820792 11.00000 10.10000 AFIX 0 C25 1 0.122387 0.927989 0.857780 11.00000 0.07028 0.07729 = 0.09321 -0.00943 0.04963 -0.01013 AFIX 31 H25A 2 0.095669 0.942816 0.897373 11.00000 10.10000 H25B 2 0.187621 0.915926 0.908133 11.00000 10.10000 H25C 2 0.059205 0.913746 0.816845 11.00000 10.10000 AFIX 0 PART 1 C26 1 0.610925 0.791389 1.099039 10.50000 0.05576 0.05369 = 0.05899 0.01122 0.01650 0.02073 AFIX 31 H26A 2 0.613861 0.768860 1.087334 10.50000 10.10000 H26B 2 0.569826 0.795182 1.144984 10.50000 10.10000 H26C 2 0.689773 0.799623 1.133623 10.50000 10.10000 AFIX 0 PART 2 C26' 1 0.613121 0.781021 1.064309 10.50000 0.08030 0.06634 = 0.06626 0.01500 0.01826 0.01687 AFIX 31 H26D 2 0.595822 0.761354 1.024121 10.50000 10.10000 H26E 2 0.589536 0.779401 1.123949 10.50000 10.10000 H26F 2 0.696327 0.785183 1.092130 10.50000 10.10000 AFIX 0 PART 0 C27 1 0.478561 0.879328 0.667478 11.00000 0.01844 0.03996 = 0.07096 0.00640 0.00068 -0.00585 PART 1 C28 1 0.186966 0.791866 0.610772 10.50000 0.05312 0.05367 = 0.07810 0.00014 0.02022 -0.02637 PART 2 C28' 1 0.169458 0.793076 0.559850 10.50000 0.06126 0.05207 = 0.06874 0.00061 0.02639 -0.03121 PART 0 C29 1 0.126270 0.945180 0.306091 11.00000 0.02489 0.03556 = 0.04598 -0.00519 0.01291 0.00041 C30 1 0.015066 0.954880 0.205438 11.00000 0.02294 0.05186 = 0.05500 0.00624 0.00671 -0.00252 C31 1 -0.012770 0.930223 0.112275 11.00000 0.08512 0.09230 = 0.07969 -0.02538 -0.00272 0.00584 AFIX 31 H31A 2 0.046160 0.931532 0.083238 11.00000 10.10000 H31B 2 -0.088922 0.934710 0.055551 11.00000 10.10000 H31C 2 -0.012807 0.909140 0.140278 11.00000 10.10000 AFIX 0 C32 1 0.022967 0.986883 0.158114 11.00000 0.04454 0.06993 = 0.07614 0.02522 0.00487 0.00025 AFIX 31 H32A 2 0.078907 0.985793 0.125565 11.00000 10.10000 H32B 2 0.048115 1.002638 0.214988 11.00000 10.10000 H32C 2 -0.053076 0.992647 0.103578 11.00000 10.10000 AFIX 0 C33 1 -0.069276 0.955409 0.255924 11.00000 0.04951 0.09851 = 0.11405 0.03643 0.03839 0.01793 AFIX 31 H33A 2 -0.073365 0.934616 0.284244 11.00000 10.10000 H33B 2 -0.145747 0.961282 0.202389 11.00000 10.10000 H33C 2 -0.044166 0.970676 0.314330 11.00000 10.10000 AFIX 0 C34 1 0.566045 0.992255 0.726958 11.00000 0.02220 0.05692 = 0.04372 0.00241 0.00800 0.00030 PART 1 C35 1 0.646210 0.985600 0.845617 10.50000 0.03718 0.07916 = 0.05027 0.02462 -0.00253 -0.01327 PART 2 C35' 1 0.614794 0.993400 0.863060 10.50000 0.05956 0.11480 = 0.08252 -0.02928 0.02123 -0.00556 PART 1 C36 1 0.715041 1.007776 0.924636 10.50000 0.04449 0.08318 = 0.05308 0.02069 -0.01213 -0.01634 AFIX 31 H36A 2 0.664400 1.021335 0.944255 10.50000 10.10000 H36B 2 0.759627 1.020520 0.895415 10.50000 10.10000 H36C 2 0.768065 0.996606 0.988157 10.50000 10.10000 AFIX 0 C37 1 0.606411 0.958708 0.904601 10.50000 0.05174 0.08595 = 0.05030 0.03419 0.00845 -0.01743 AFIX 31 H37A 2 0.568132 0.941933 0.853718 10.50000 10.10000 H37B 2 0.552482 0.967449 0.932239 10.50000 10.10000 H37C 2 0.674252 0.950277 0.963962 10.50000 10.10000 AFIX 0 PART 2 C36' 1 0.696251 1.022096 0.901729 10.50000 0.06551 0.11395 = 0.08709 -0.04263 0.02110 -0.00908 AFIX 31 H36D 2 0.653183 1.041149 0.869494 10.50000 10.10000 H36E 2 0.760816 1.019647 0.880365 10.50000 10.10000 H36F 2 0.726215 1.023620 0.979758 10.50000 10.10000 AFIX 0 C37' 1 0.697284 0.967505 0.903633 10.50000 0.08223 0.12802 = 0.10332 -0.01428 0.01079 0.00429 AFIX 31 H37D 2 0.750374 0.967655 0.867881 10.50000 10.10000 H37E 2 0.655177 0.947627 0.889259 10.50000 10.10000 H37F 2 0.741379 0.969941 0.980849 10.50000 10.10000 AFIX 0 PART 1 C38 1 0.741734 0.964885 0.819242 10.50000 0.04122 0.08146 = 0.06395 0.01139 -0.00269 0.01400 AFIX 31 H38A 2 0.701768 0.948384 0.767795 10.50000 10.10000 H38B 2 0.797310 0.955420 0.885362 10.50000 10.10000 H38C 2 0.782725 0.978578 0.788941 10.50000 10.10000 AFIX 0 PART 2 C38' 1 0.535407 0.997233 0.916836 10.50000 0.05718 0.11882 = 0.07936 -0.02011 0.03507 -0.00957 AFIX 31 H38D 2 0.482853 1.014744 0.884416 10.50000 10.10000 H38E 2 0.580288 1.001472 0.992953 10.50000 10.10000 H38F 2 0.490436 0.978025 0.908799 10.50000 10.10000 AFIX 0 PART 0 C39 1 0.644191 0.956984 0.505811 11.00000 0.03867 0.03051 = 0.07514 -0.01723 0.01555 0.00098 PART 1 C40 1 0.730544 0.944279 0.469759 10.50000 0.03121 0.05109 = 0.06716 -0.02858 0.01650 -0.00449 PART 2 C40' 1 0.750526 0.937572 0.549526 10.50000 0.00866 0.04655 = 0.05777 -0.00449 0.00587 0.00769 PART 1 C41 1 0.702027 0.951947 0.350875 10.50000 0.06978 0.08030 = 0.09102 -0.01382 0.04636 0.00206 AFIX 31 H41A 2 0.630499 0.941269 0.305010 10.50000 10.10000 H41B 2 0.765513 0.944836 0.332940 10.50000 10.10000 H41C 2 0.692073 0.974575 0.339643 10.50000 10.10000 AFIX 0 PART 2 C41' 1 0.801388 0.937351 0.673392 10.50000 0.07849 0.10219 = 0.11396 -0.00599 0.02719 0.00594 AFIX 31 H41D 2 0.754408 0.923764 0.697464 10.50000 10.10000 H41E 2 0.800963 0.958652 0.699592 10.50000 10.10000 H41F 2 0.880943 0.929498 0.701413 10.50000 10.10000 AFIX 0 PART 0 part 1 C42 1 0.726938 0.903770 0.508488 10.50000 0.05779 0.03788 = 0.06357 -0.00271 0.02231 0.02896 AFIX 31 H42A 2 0.778748 0.891259 0.487037 10.50000 10.10000 H42B 2 0.647922 0.895702 0.473132 10.50000 10.10000 H42C 2 0.752201 0.902512 0.586173 10.50000 10.10000 AFIX 0 C43 1 0.838317 0.960238 0.544971 10.70000 0.03735 0.06806 = 0.07281 -0.01455 0.01380 -0.00172 AFIX 31 H43A 2 0.903832 0.953630 0.529254 10.70000 10.10000 H43B 2 0.852978 0.954581 0.618702 10.70000 10.10000 H43C 2 0.828630 0.982940 0.536151 10.70000 10.10000 AFIX 0 part 2 C42' 1 0.734026 0.908943 0.472975 10.50000 0.07433 0.07700 = 0.08690 0.01256 0.03519 0.01805 AFIX 31 H42D 2 0.802906 0.895626 0.501384 10.50000 10.10000 H42E 2 0.722583 0.916484 0.401808 10.50000 10.10000 H42F 2 0.666289 0.896845 0.467944 10.50000 10.10000 AFIX 0 C43' 1 0.826848 0.951446 0.493067 10.30000 0.06663 0.08012 = 0.07924 -0.00138 0.03300 -0.00400 AFIX 31 H43D 2 0.904370 0.942243 0.524907 10.30000 10.10000 H43E 2 0.832529 0.974183 0.502659 10.30000 10.10000 H43F 2 0.791007 0.946522 0.416597 10.30000 10.10000 AFIX 0 part 0 C44 1 0.889735 0.826714 0.340701 10.50000 0.04974 0.06529 = 0.05394 0.01238 0.02361 -0.02079 C45 1 0.949675 0.855250 0.343931 10.50000 0.05384 0.05175 = 0.09401 -0.00698 0.00162 -0.02521 N1 3 0.414479 0.842444 0.394833 11.00000 0.02592 0.02852 = 0.09130 -0.01244 0.01626 -0.00475 N2 3 0.291657 0.902402 0.777604 11.00000 0.03862 0.05051 = 0.05804 0.01167 0.01912 -0.00774 N3 3 0.275884 0.787219 0.396475 11.00000 0.04415 0.03379 = 0.11795 -0.00636 0.01298 -0.00308 PART 1 N4 3 0.332880 0.765347 0.390244 10.50000 0.06381 0.05096 = 0.07185 0.00908 0.00964 -0.01056 PART 2 N4' 3 0.332256 0.770615 0.361881 10.50000 0.05430 0.01951 = 0.06770 -0.00734 -0.00241 0.00072 PART 1 N5 3 0.391012 0.745082 0.373466 10.50000 0.09353 0.05897 = 0.09145 -0.01296 0.02309 0.01926 PART 2 N5' 3 0.386155 0.753076 0.333320 10.50000 0.07656 0.03452 = 0.07280 -0.00106 0.00997 0.02298 PART 0 N6 3 0.155668 0.843785 0.756988 11.00000 0.05957 0.07980 = 0.12579 0.02561 0.04839 -0.01414 PART 1 N7 3 0.066634 0.846841 0.711672 10.60000 0.06630 0.08733 = 0.13698 0.02670 0.04186 -0.01663 N8 3 -0.029547 0.849149 0.653824 10.60000 0.07129 0.09509 = 0.14934 0.02570 0.03477 -0.01733 PART 2 N7' 3 0.135943 0.843678 0.837447 10.40000 0.06970 0.09468 = 0.13427 0.02630 0.04399 -0.01382 N8' 3 0.122823 0.847197 0.921715 10.40000 0.07931 0.10664 = 0.14116 0.02386 0.04040 -0.01187 PART 0 N9 3 0.857685 0.804450 0.347413 10.50000 0.07092 0.09556 = 0.08820 0.00403 0.03439 -0.03254 O1 4 0.471765 0.807476 0.606315 11.00000 0.02464 0.03044 = 0.13203 0.00515 0.01503 0.00207 O2 4 0.222870 0.854941 0.389391 11.00000 0.02537 0.03191 = 0.07215 -0.00197 0.01552 -0.00599 O3 4 0.357301 0.909832 0.412492 11.00000 0.01827 0.03430 = 0.07717 -0.00016 0.01918 0.00007 O4 4 0.623024 0.777372 0.775612 11.00000 0.04167 0.04127 = 0.13215 -0.00342 -0.02069 0.01155 O5 4 0.396416 0.842908 0.837054 11.00000 0.04411 0.05419 = 0.08717 0.03214 0.01294 -0.00687 O6 4 0.165506 0.882883 0.565566 11.00000 0.02610 0.03538 = 0.07535 0.00359 0.01741 -0.00280 O7 4 0.304180 0.935362 0.572625 11.00000 0.02720 0.03141 = 0.05368 0.00234 0.00944 -0.00629 O8 4 0.546225 0.808089 0.989584 11.00000 0.05910 0.08416 = 0.10589 0.05185 0.01709 0.00075 O9 4 0.366681 0.867289 0.606481 11.00000 0.01965 0.02849 = 0.07674 0.00830 0.00811 -0.00364 O10 4 0.262472 0.816724 0.609251 11.00000 0.03087 0.03357 = 0.11018 0.01175 0.01951 -0.00922 O11 4 0.125639 0.918166 0.351489 11.00000 0.02146 0.03353 = 0.06563 -0.00068 0.01496 -0.00090 O12 4 0.206212 0.963586 0.334866 11.00000 0.02468 0.03456 = 0.05122 -0.00047 0.00924 0.00047 O13 4 0.497809 0.971557 0.675101 11.00000 0.03104 0.07596 = 0.06633 -0.01859 0.00470 -0.00819 part 1 O14 4 0.580705 1.021245 0.690836 10.65000 0.02547 0.04225 = 0.04436 -0.00173 0.01185 -0.00064 part 2 O14' 4 0.583989 1.006897 0.652867 10.35000 0.01626 0.04663 = 0.06266 0.00346 0.01515 0.00284 part 0 O15 4 0.563552 0.941035 0.501208 11.00000 0.02172 0.06770 = 0.09224 -0.01178 0.01666 -0.00268 part 1 O16 4 0.638871 0.985501 0.524332 10.65000 0.03950 0.02888 = 0.05314 0.00446 0.01004 0.00233 part 2 O16' 4 0.660450 0.988330 0.478908 10.35000 0.02126 0.02625 = 0.05744 0.00965 -0.00286 -0.00271 part 0 HKLF 4 REM p21c in P2(1)/c REM R1 = 0.0579 for 8688 Fo > 4sig(Fo) and 0.0730 for all 11112 data REM 817 parameters refined using 248 restraints END ; #======================END data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 874771' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C100 H126 Fe6 Gd2 N16 Na2 O40' _chemical_formula_sum 'C100 H126 Fe6 Gd2 N16 Na2 O40' _chemical_formula_weight 2887.75 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' Na Na 0.0362 0.0249 '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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.659(3) _cell_length_b 35.205(7) _cell_length_c 17.180(3) _cell_angle_alpha 90.00 _cell_angle_beta 124.37(3) _cell_angle_gamma 90.00 _cell_volume 6320(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10709 _cell_measurement_theta_min 8.18 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 1.792 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9241 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details Process-auto _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45745 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 8.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10709 _reflns_number_gt 7495 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+17.4650P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10709 _refine_ls_number_parameters 877 _refine_ls_number_restraints 370 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.51657(4) 0.974632(10) 0.40349(2) 0.04084(16) Uani 1 1 d . . . Fe1 Fe 0.54418(12) 0.92587(3) 0.24487(8) 0.0470(3) Uani 1 1 d . A . Fe2 Fe 0.75170(15) 0.86257(3) 0.29250(9) 0.0598(4) Uani 1 1 d . A . Fe3 Fe 0.44891(17) 0.84245(4) 0.17062(11) 0.0764(5) Uani 1 1 d . . . Na1 Na 0.6958(10) 0.77090(18) 0.3143(6) 0.0563(19) Uani 0.50 1 d P A 1 Na1' Na 0.6320(11) 0.7714(3) 0.2847(8) 0.082(4) Uani 0.50 1 d PU A 2 O1 O 0.4940(15) 0.7939(4) 0.2555(10) 0.060(3) Uani 0.50 1 d PU A 1 O1' O 0.4322(13) 0.7993(3) 0.2217(9) 0.049(3) Uani 0.50 1 d PU A 2 O2 O 0.4226(6) 0.89645(17) 0.1261(4) 0.0638(16) Uani 1 1 d . A . O3 O 0.4175(6) 0.93224(16) 0.2735(4) 0.0532(14) Uani 1 1 d . . . O4 O 0.5670(19) 0.7258(6) 0.3256(14) 0.088(6) Uani 0.50 1 d PU A 1 O4' O 0.495(2) 0.7326(3) 0.3066(11) 0.077(5) Uani 0.50 1 d P A 2 O5 O 0.8103(8) 0.82235(16) 0.3857(5) 0.078(2) Uani 1 1 d . . . O6 O 0.6853(6) 0.91365(14) 0.2297(4) 0.0507(13) Uani 1 1 d . . . O7 O 0.6576(5) 0.94903(13) 0.3700(3) 0.0433(12) Uani 1 1 d . . . O8 O 0.873(2) 0.7547(5) 0.4672(13) 0.086(6) Uani 0.50 1 d PDU A 1 O8' O 0.8233(17) 0.7578(4) 0.4638(11) 0.085(5) Uani 0.50 1 d PDU A 2 O9 O 0.6152(8) 0.83052(16) 0.1862(5) 0.0726(19) Uani 1 1 d . A . O10 O 0.5897(6) 0.87018(15) 0.2981(4) 0.0582(15) Uani 1 1 d . A . O11 O 0.7978(13) 0.7333(4) 0.2785(9) 0.110(4) Uani 0.75 1 d PU A 1 O11' O 0.658(4) 0.7235(11) 0.210(3) 0.113(10) Uani 0.25 1 d PU A 2 O12 O 0.5048(6) 0.97525(15) 0.1760(4) 0.0500(13) Uani 1 1 d . . . O13 O 0.4717(5) 1.01113(14) 0.2696(3) 0.0469(13) Uani 1 1 d . . . O14 O 0.4659(6) 0.91940(15) 0.4556(4) 0.0526(14) Uani 1 1 d . . . O15 O 0.5428(6) 1.03628(14) 0.4579(3) 0.0472(13) Uani 1 1 d . . . O16 O 0.3044(5) 0.99111(14) 0.3450(4) 0.0480(13) Uani 1 1 d . . . O17 O 0.7098(5) 0.97087(15) 0.5559(3) 0.0471(12) Uani 1 1 d . . . N1 N 0.2901(10) 0.8620(3) 0.1740(6) 0.092(3) Uani 1 1 d D A . N2 N 0.8670(7) 0.90044(18) 0.4058(5) 0.0510(16) Uani 1 1 d . . . N3 N 0.3359(9) 0.8218(3) 0.0384(6) 0.0809(17) Uani 1 1 d DU A . N4 N 0.2835(17) 0.7893(4) 0.0427(13) 0.0805(17) Uani 0.50 1 d PDU A 1 N5 N 0.2212(17) 0.7596(5) 0.0370(13) 0.0809(17) Uani 0.50 1 d PDU A 1 N4' N 0.3035(17) 0.8426(5) -0.0419(11) 0.0809(17) Uani 0.50 1 d PDU A 2 N5' N 0.2776(19) 0.8585(5) -0.1188(12) 0.0802(17) Uani 0.50 1 d PDU A 2 N6 N 0.8795(14) 0.8556(4) 0.2631(10) 0.122(2) Uani 1 1 d U . . N7 N 0.9163(14) 0.8519(4) 0.2229(10) 0.125(2) Uani 1 1 d U A . N8 N 0.9285(14) 0.8472(4) 0.1558(10) 0.129(2) Uani 1 1 d U . . C1 C 0.4218(14) 0.7795(4) 0.2841(11) 0.091(3) Uani 0.50 1 d PGU A 1 C2 C 0.3223(12) 0.7962(3) 0.2842(7) 0.091(3) Uani 0.50 1 d PGDU A 1 C3 C 0.2653(13) 0.7768(3) 0.3218(10) 0.091(3) Uani 0.50 1 d PGU A 1 H3 H 0.1988 0.7879 0.3218 0.100 Uiso 0.50 1 calc P B 1 C4 C 0.3077(16) 0.7406(3) 0.3593(11) 0.091(3) Uani 0.50 1 d PGU A 1 H4 H 0.2696 0.7276 0.3844 0.100 Uiso 0.50 1 calc P C 1 C5 C 0.4071(15) 0.7239(3) 0.3592(11) 0.091(3) Uani 0.50 1 d PGU A 1 H5 H 0.4355 0.6997 0.3842 0.100 Uiso 0.50 1 calc P D 1 C6 C 0.4642(15) 0.7433(4) 0.3216(13) 0.091(3) Uani 0.50 1 d PGU A 1 C7 C 0.2734(17) 0.8356(4) 0.2368(10) 0.102(10) Uani 0.50 1 d PGD A 1 H7 H 0.2184 0.8462 0.2506 0.100 Uiso 0.50 1 calc P E 1 C1' C 0.3697(11) 0.7868(3) 0.2593(9) 0.060(2) Uani 0.50 1 d PGU A 2 C2' C 0.2753(9) 0.8092(3) 0.2536(8) 0.060(2) Uani 0.50 1 d PGDU A 2 C3' C 0.2116(10) 0.7968(3) 0.2934(8) 0.060(2) Uani 0.50 1 d PGU A 2 H3' H 0.1484 0.8118 0.2896 0.100 Uiso 0.50 1 calc P F 2 C4' C 0.2424(12) 0.7618(3) 0.3389(9) 0.060(2) Uani 0.50 1 d PGU A 2 H4' H 0.1998 0.7535 0.3656 0.100 Uiso 0.50 1 calc P G 2 C5' C 0.3368(12) 0.7393(3) 0.3446(9) 0.061(2) Uani 0.50 1 d PGU A 2 H5' H 0.3573 0.7160 0.3750 0.100 Uiso 0.50 1 calc P H 2 C6' C 0.4004(11) 0.7518(3) 0.3048(10) 0.060(2) Uani 0.50 1 d PGU A 2 C7' C 0.2298(14) 0.8450(3) 0.2091(12) 0.059(2) Uani 0.50 1 d PGDU A 2 H7' H 0.1600 0.8564 0.2041 0.100 Uiso 0.50 1 calc P I 2 C8 C 0.2388(11) 0.8995(4) 0.1351(8) 0.076(3) Uani 1 1 d . . . C9 C 0.2835(10) 0.9267(3) 0.2151(7) 0.071(3) Uani 1 1 d . A . H9A H 0.2427 0.9510 0.1894 0.100 Uiso 1 1 calc . . . H9B H 0.2554 0.9174 0.2537 0.100 Uiso 1 1 calc . . . C10 C 0.2929(11) 0.9079(3) 0.0784(7) 0.076(3) Uani 1 1 d . A . H10A H 0.2427 0.8947 0.0184 0.100 Uiso 1 1 calc . . . H10B H 0.2867 0.9349 0.0657 0.100 Uiso 1 1 calc . . . C11 C 0.0907(13) 0.9003(4) 0.0702(9) 0.098(4) Uani 1 1 d U A . H11A H 0.0623 0.8778 0.0308 0.100 Uiso 1 1 calc . . . H11B H 0.0587 0.8985 0.1097 0.100 Uiso 1 1 calc . . . C12 C 0.0299(15) 0.9339(4) 0.0076(11) 0.111(4) Uani 1 1 d U . . H12A H -0.0615 0.9315 -0.0278 0.100 Uiso 1 1 calc . . . H12B H 0.0561 0.9354 -0.0349 0.100 Uiso 1 1 calc . . . H12C H 0.0558 0.9566 0.0452 0.100 Uiso 1 1 calc . . . C13 C 0.589(3) 0.6872(7) 0.3508(17) 0.083(6) Uani 0.50 1 d PU A 1 H13A H 0.6594 0.6783 0.3499 0.100 Uiso 0.50 1 calc P J 1 H13B H 0.5134 0.6728 0.3068 0.100 Uiso 0.50 1 calc P K 1 H13C H 0.6077 0.6842 0.4131 0.100 Uiso 0.50 1 calc P L 1 C13' C 0.507(3) 0.6932(7) 0.3347(16) 0.079(6) Uani 0.50 1 d PU A 2 H13D H 0.5742 0.6814 0.3334 0.100 Uiso 0.50 1 calc P M 2 H13E H 0.4277 0.6802 0.2920 0.100 Uiso 0.50 1 calc P N 2 H13F H 0.5266 0.6918 0.3974 0.100 Uiso 0.50 1 calc P O 2 C14 C 0.8923(12) 0.8217(3) 0.4803(8) 0.074(3) Uani 1 1 d . A . C15 C 0.9536(10) 0.8540(3) 0.5332(7) 0.063(2) Uani 1 1 d . . . C16 C 1.0334(12) 0.8499(3) 0.6297(8) 0.079(3) Uani 1 1 d . A . H16 H 1.0751 0.8714 0.6657 0.100 Uiso 1 1 calc . . . C17 C 1.0549(13) 0.8163(4) 0.6752(9) 0.095(4) Uani 1 1 d U . . H17 H 1.1086 0.8147 0.7406 0.100 Uiso 1 1 calc . . . C18 C 0.9954(13) 0.7857(4) 0.6219(10) 0.099(4) Uani 1 1 d U A . H18 H 1.0109 0.7623 0.6516 0.100 Uiso 1 1 calc . . . C19 C 0.9139(12) 0.7870(3) 0.5270(8) 0.093(3) Uani 1 1 d DU . . C20 C 0.9382(9) 0.8914(2) 0.4931(6) 0.052(2) Uani 1 1 d . A . H20 H 0.9851 0.9109 0.5353 0.100 Uiso 1 1 calc . . . C21 C 0.8593(8) 0.9411(2) 0.3776(5) 0.0437(18) Uani 1 1 d . A . C22 C 0.7895(8) 0.9409(2) 0.2709(6) 0.0499(19) Uani 1 1 d . A . H22A H 0.7559 0.9660 0.2462 0.100 Uiso 1 1 calc . . . H22B H 0.8487 0.9342 0.2542 0.100 Uiso 1 1 calc . . . C23 C 0.7836(8) 0.9632(2) 0.4076(5) 0.0436(17) Uani 1 1 d . A . H23A H 0.8314 0.9629 0.4759 0.100 Uiso 1 1 calc . . . H23B H 0.7768 0.9895 0.3881 0.100 Uiso 1 1 calc . . . C24 C 0.9928(9) 0.9598(2) 0.4230(6) 0.053(2) Uani 1 1 d . . . H24A H 0.9810 0.9844 0.3939 0.100 Uiso 1 1 calc . . . H24B H 1.0289 0.9641 0.4892 0.100 Uiso 1 1 calc . . . C25 C 1.0898(10) 0.9374(3) 0.4152(7) 0.066(2) Uani 1 1 d . A . H25A H 1.1683 0.9515 0.4445 0.100 Uiso 1 1 calc . . . H25B H 1.0564 0.9333 0.3500 0.100 Uiso 1 1 calc . . . H25C H 1.1059 0.9134 0.4464 0.100 Uiso 1 1 calc . . . C26 C 0.931(3) 0.7208(9) 0.515(2) 0.098(8) Uani 0.50 1 d PU A 1 H26G H 0.8921 0.6998 0.4718 0.100 Uiso 0.50 1 calc P P 1 H26H H 0.9213 0.7176 0.5657 0.100 Uiso 0.50 1 calc P Q 1 H26I H 1.0208 0.7217 0.5393 0.100 Uiso 0.50 1 calc P R 1 C26' C 0.854(3) 0.7179(6) 0.4986(17) 0.081(6) Uani 0.50 1 d PU A 2 H26D H 0.7929 0.7011 0.4500 0.100 Uiso 0.50 1 calc P S 2 H26E H 0.8519 0.7154 0.5532 0.100 Uiso 0.50 1 calc P T 2 H26F H 0.9384 0.7116 0.5150 0.100 Uiso 0.50 1 calc P U 2 C27 C 0.6241(13) 0.8161(3) 0.1118(8) 0.086(3) Uani 1 1 d . . . H27A H 0.7125 0.8128 0.1348 0.100 Uiso 1 1 calc . . . H27B H 0.5847 0.8337 0.0601 0.100 Uiso 1 1 calc . . . H27C H 0.5810 0.7920 0.0908 0.100 Uiso 1 1 calc . . . C28 C 0.5975(11) 0.8627(2) 0.3829(7) 0.063(2) Uani 1 1 d . . . H28A H 0.6175 0.8364 0.3993 0.100 Uiso 1 1 calc . . . H28B H 0.5169 0.8685 0.3735 0.100 Uiso 1 1 calc . . . H28C H 0.6633 0.8782 0.4329 0.100 Uiso 1 1 calc . . . C29 C 0.928(2) 0.7461(6) 0.3086(15) 0.114(6) Uani 0.75 1 d PU A 1 C29' C 0.554(5) 0.7145(15) 0.088(4) 0.091(12) Uani 0.25 1 d PU A 2 C30 C 0.4215(8) 1.03612(18) 0.1241(4) 0.0809(15) Uani 1 1 d GU . . C31 C 0.3474(8) 1.0657(2) 0.1222(4) 0.0826(15) Uani 1 1 d GU A . H31 H 0.3305 1.0672 0.1683 0.100 Uiso 1 1 calc . . . C32 C 0.2985(8) 1.09301(19) 0.0516(5) 0.0849(15) Uani 1 1 d GU A . H32 H 0.2489 1.1128 0.0504 0.100 Uiso 1 1 calc . . . C33 C 0.3237(8) 1.09073(18) -0.0172(4) 0.0859(15) Uani 1 1 d GU A . H33 H 0.2910 1.1090 -0.0645 0.100 Uiso 1 1 calc . . . C34 C 0.3978(8) 1.0612(2) -0.0154(4) 0.0848(15) Uani 1 1 d GU A . H34 H 0.4146 1.0596 -0.0615 0.100 Uiso 1 1 calc . . . C35 C 0.4467(8) 1.03384(19) 0.0552(5) 0.0824(15) Uani 1 1 d GU A . H35 H 0.4962 1.0141 0.0564 0.100 Uiso 1 1 calc . . . C36 C 0.4687(8) 1.0057(2) 0.1954(5) 0.0486(19) Uani 1 1 d . A . C37 C 0.3911(8) 0.9004(2) 0.5472(5) 0.0455(18) Uani 1 1 d . . . C38 C 0.3452(10) 0.8663(2) 0.4999(7) 0.061(2) Uani 1 1 d . A . H38 H 0.3506 0.8614 0.4490 0.100 Uiso 1 1 calc . . . C39 C 0.2920(13) 0.8395(3) 0.5257(9) 0.086(3) Uani 1 1 d . . . H39 H 0.2586 0.8172 0.4913 0.100 Uiso 1 1 calc . . . C40 C 0.2884(13) 0.8462(3) 0.6043(9) 0.085(3) Uani 1 1 d . A . H40 H 0.2563 0.8277 0.6244 0.100 Uiso 1 1 calc . . . C41 C 0.3322(12) 0.8800(3) 0.6521(8) 0.080(3) Uani 1 1 d . . . H41 H 0.3266 0.8847 0.7029 0.100 Uiso 1 1 calc . . . C42 C 0.3853(10) 0.9075(3) 0.6248(6) 0.060(2) Uani 1 1 d . A . H42 H 0.4163 0.9302 0.6579 0.100 Uiso 1 1 calc . . . C43 C 0.4419(8) 0.9294(2) 0.5141(5) 0.0447(18) Uani 1 1 d . . . C44 C 0.1047(9) 1.0184(2) 0.2911(6) 0.0491(19) Uani 1 1 d . . . C45 C 0.0389(10) 0.9945(3) 0.2149(6) 0.062(2) Uani 1 1 d . A . H45 H 0.0830 0.9747 0.2092 0.100 Uiso 1 1 calc . . . C46 C -0.0921(10) 0.9987(3) 0.1455(7) 0.071(3) Uani 1 1 d . . . H46 H -0.1352 0.9816 0.0956 0.100 Uiso 1 1 calc . . . C47 C -0.1555(11) 1.0288(3) 0.1532(7) 0.075(3) Uani 1 1 d . A . H47 H -0.2418 1.0328 0.1067 0.100 Uiso 1 1 calc . . . C48 C -0.0923(10) 1.0527(3) 0.2286(7) 0.071(3) Uani 1 1 d . . . H48 H -0.1361 1.0727 0.2337 0.100 Uiso 1 1 calc . . . C49 C 0.0362(9) 1.0476(3) 0.2974(6) 0.058(2) Uani 1 1 d . A . H49 H 0.0776 1.0640 0.3487 0.100 Uiso 1 1 calc . . . C50 C 0.2437(8) 1.0125(2) 0.3661(5) 0.0432(18) Uani 1 1 d . . . O1W O 0.7264(9) 0.6678(3) 0.1796(7) 0.110(3) Uani 1 1 d U V 1 O4W O 0.601(2) 0.7073(6) 0.0538(16) 0.127(6) Uani 0.50 1 d PU W 1 O5W O 0.364(3) 0.8811(8) -0.0938(18) 0.149(8) Uani 0.50 1 d PU X 1 O2W O 0.7892(19) 0.6299(6) 0.2069(13) 0.112(5) Uani 0.50 1 d PU Y 2 O3W O 0.6673(15) 0.6700(5) 0.0818(11) 0.090(4) Uani 0.50 1 d PU Z 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 Gd1 0.0616(3) 0.0400(2) 0.0400(2) 0.00054(16) 0.0402(2) 0.00262(18) Fe1 0.0694(8) 0.0451(6) 0.0482(6) -0.0069(5) 0.0462(6) -0.0041(5) Fe2 0.0990(10) 0.0418(6) 0.0725(8) -0.0030(6) 0.0690(8) 0.0063(6) Fe3 0.1241(13) 0.0568(8) 0.0902(10) -0.0323(7) 0.0858(10) -0.0304(8) Na1 0.066(5) 0.028(3) 0.063(4) -0.016(3) 0.030(4) -0.008(4) Na1' 0.083(4) 0.082(4) 0.083(4) -0.0002(10) 0.047(2) 0.0003(10) O1 0.060(3) 0.059(3) 0.060(3) -0.0005(10) 0.033(2) -0.0001(10) O1' 0.049(3) 0.048(3) 0.049(3) -0.0004(10) 0.0276(18) 0.0004(10) O2 0.076(4) 0.066(4) 0.064(4) -0.025(3) 0.049(3) -0.015(3) O3 0.075(4) 0.059(3) 0.052(3) -0.009(3) 0.051(3) -0.007(3) O4 0.088(6) 0.087(7) 0.088(6) 0.0000(10) 0.049(4) -0.0003(10) O4' 0.121(15) 0.010(5) 0.089(10) 0.002(6) 0.053(11) -0.013(7) O5 0.126(6) 0.041(3) 0.094(5) 0.006(3) 0.079(5) 0.016(3) O6 0.080(4) 0.041(3) 0.053(3) 0.000(2) 0.051(3) 0.004(3) O7 0.070(4) 0.038(3) 0.042(3) -0.003(2) 0.044(3) 0.001(2) O8 0.086(6) 0.085(6) 0.086(6) 0.0000(10) 0.048(4) 0.0003(10) O8' 0.100(9) 0.066(8) 0.107(9) 0.032(6) 0.069(8) 0.025(7) O9 0.131(6) 0.046(3) 0.084(4) -0.009(3) 0.087(5) 0.001(4) O10 0.098(5) 0.046(3) 0.071(4) -0.012(3) 0.072(4) -0.010(3) O11 0.111(4) 0.110(4) 0.110(4) -0.0015(10) 0.062(2) 0.0010(10) O11' 0.113(10) 0.113(10) 0.113(10) -0.0001(10) 0.064(6) 0.0001(10) O12 0.075(4) 0.050(3) 0.044(3) -0.003(2) 0.045(3) 0.004(3) O13 0.071(4) 0.044(3) 0.041(3) 0.001(2) 0.041(3) 0.008(3) O14 0.080(4) 0.045(3) 0.060(3) 0.003(3) 0.056(3) 0.002(3) O15 0.074(4) 0.040(3) 0.043(3) -0.001(2) 0.043(3) 0.002(3) O16 0.062(3) 0.045(3) 0.050(3) -0.002(2) 0.040(3) 0.002(3) O17 0.063(3) 0.054(3) 0.040(3) 0.001(2) 0.039(3) 0.002(3) N1 0.123(8) 0.113(8) 0.092(6) -0.062(6) 0.091(6) -0.072(7) N2 0.072(5) 0.045(4) 0.062(4) 0.007(3) 0.053(4) 0.014(3) N3 0.0818(18) 0.0807(18) 0.0805(18) -0.0025(9) 0.0460(13) 0.0003(9) N4 0.0815(18) 0.0806(19) 0.0803(18) -0.0023(9) 0.0461(13) 0.0004(9) N5 0.0817(19) 0.0808(19) 0.0805(19) -0.0023(10) 0.0459(13) 0.0004(10) N4' 0.0815(18) 0.0807(18) 0.0806(18) -0.0020(8) 0.0458(11) 0.0004(8) N5' 0.0811(18) 0.0803(18) 0.0802(18) -0.0018(8) 0.0460(11) 0.0004(8) N6 0.150(6) 0.141(6) 0.141(6) -0.010(5) 0.122(5) 0.003(5) N7 0.151(6) 0.142(6) 0.143(6) -0.009(5) 0.120(5) 0.002(5) N8 0.153(6) 0.144(6) 0.144(6) -0.009(5) 0.117(5) 0.002(5) C1 0.094(7) 0.097(7) 0.090(6) -0.034(5) 0.056(6) -0.048(6) C2 0.094(7) 0.097(7) 0.090(6) -0.034(5) 0.056(6) -0.048(6) C3 0.094(7) 0.097(7) 0.090(6) -0.034(5) 0.056(6) -0.048(6) C4 0.094(7) 0.097(7) 0.090(6) -0.034(5) 0.056(6) -0.048(6) C5 0.094(7) 0.097(7) 0.090(6) -0.034(5) 0.056(6) -0.048(6) C6 0.094(7) 0.097(7) 0.090(6) -0.034(5) 0.056(6) -0.048(6) C7 0.078(16) 0.15(2) 0.074(14) -0.086(16) 0.041(13) -0.022(15) C1' 0.062(2) 0.059(2) 0.060(2) 0.0009(13) 0.0345(17) -0.0034(13) C2' 0.062(2) 0.059(2) 0.059(2) 0.0009(13) 0.0346(17) -0.0034(13) C3' 0.061(2) 0.059(2) 0.060(2) 0.0009(12) 0.0344(16) -0.0028(12) C4' 0.061(2) 0.060(2) 0.060(2) 0.0006(8) 0.0342(13) -0.0018(8) C5' 0.061(2) 0.060(2) 0.060(2) 0.0006(8) 0.0342(13) -0.0017(8) C6' 0.062(2) 0.060(2) 0.060(2) 0.0008(12) 0.0343(16) -0.0028(12) C7' 0.062(2) 0.059(2) 0.059(2) 0.0008(16) 0.035(2) -0.0038(16) C8 0.086(7) 0.091(8) 0.086(7) -0.036(6) 0.070(6) -0.033(6) C9 0.069(6) 0.093(7) 0.073(6) -0.040(5) 0.053(5) -0.032(5) C10 0.079(7) 0.087(7) 0.073(6) -0.040(6) 0.050(6) -0.031(6) C11 0.098(4) 0.098(4) 0.098(4) -0.0009(10) 0.056(2) -0.0006(10) C12 0.111(4) 0.111(4) 0.111(4) -0.0005(10) 0.063(3) 0.0000(10) C13 0.083(6) 0.083(6) 0.083(6) 0.0002(10) 0.047(4) -0.0003(10) C13' 0.079(6) 0.079(6) 0.079(6) 0.0001(10) 0.045(3) 0.0000(10) C14 0.121(9) 0.046(5) 0.088(7) 0.024(5) 0.079(7) 0.029(5) C15 0.092(7) 0.056(5) 0.067(6) 0.011(4) 0.060(5) 0.015(5) C16 0.119(9) 0.074(6) 0.078(6) 0.028(5) 0.077(7) 0.025(6) C17 0.096(4) 0.095(4) 0.095(4) 0.0007(10) 0.054(2) 0.0002(10) C18 0.100(4) 0.099(4) 0.099(4) 0.0010(10) 0.056(2) -0.0002(10) C19 0.093(4) 0.093(4) 0.093(4) 0.0001(10) 0.053(2) 0.0001(10) C20 0.069(6) 0.050(4) 0.065(5) 0.010(4) 0.055(5) 0.013(4) C21 0.063(5) 0.043(4) 0.044(4) 0.007(3) 0.042(4) 0.010(4) C22 0.068(5) 0.049(4) 0.052(4) 0.006(4) 0.046(4) 0.006(4) C23 0.050(5) 0.044(4) 0.051(4) -0.001(3) 0.037(4) 0.002(3) C24 0.061(5) 0.056(5) 0.060(5) 0.002(4) 0.044(4) 0.002(4) C25 0.073(6) 0.069(6) 0.078(6) 0.014(5) 0.056(5) 0.016(5) C26 0.097(8) 0.097(8) 0.098(8) 0.0001(10) 0.055(5) 0.0000(10) C26' 0.086(10) 0.050(8) 0.092(10) 0.021(7) 0.042(7) 0.004(7) C27 0.120(10) 0.074(7) 0.089(7) -0.019(6) 0.073(7) 0.003(6) C28 0.114(8) 0.037(4) 0.071(5) -0.004(4) 0.072(6) -0.003(5) C29 0.114(6) 0.114(6) 0.114(6) -0.0003(10) 0.064(3) 0.0002(10) C29' 0.091(12) 0.091(12) 0.091(12) 0.0001(10) 0.052(7) -0.0001(10) C30 0.115(4) 0.075(3) 0.055(2) 0.012(2) 0.050(3) 0.008(3) C31 0.116(4) 0.075(3) 0.057(2) 0.012(2) 0.049(3) 0.008(3) C32 0.117(4) 0.075(3) 0.059(2) 0.012(2) 0.047(3) 0.008(3) C33 0.118(4) 0.076(3) 0.059(2) 0.012(2) 0.047(3) 0.008(3) C34 0.118(4) 0.076(3) 0.058(2) 0.012(2) 0.048(3) 0.008(3) C35 0.116(4) 0.076(3) 0.056(2) 0.012(2) 0.049(3) 0.008(3) C36 0.053(5) 0.054(5) 0.042(4) -0.004(4) 0.030(4) -0.003(4) C37 0.051(5) 0.048(4) 0.050(4) 0.009(4) 0.036(4) 0.009(4) C38 0.081(6) 0.049(5) 0.069(5) -0.002(4) 0.053(5) -0.005(4) C39 0.130(10) 0.055(6) 0.109(8) -0.005(6) 0.088(8) -0.021(6) C40 0.117(9) 0.074(7) 0.099(8) 0.011(6) 0.083(8) -0.015(6) C41 0.122(9) 0.075(7) 0.080(7) 0.013(6) 0.080(7) -0.008(6) C42 0.084(6) 0.056(5) 0.055(5) 0.012(4) 0.047(5) 0.009(5) C43 0.056(5) 0.043(4) 0.045(4) 0.004(3) 0.035(4) 0.005(4) C44 0.068(5) 0.049(4) 0.048(4) 0.011(4) 0.044(4) 0.010(4) C45 0.072(6) 0.063(5) 0.059(5) 0.003(4) 0.042(5) 0.015(5) C46 0.073(7) 0.081(7) 0.057(5) -0.004(5) 0.035(5) 0.002(5) C47 0.076(7) 0.084(7) 0.066(6) 0.013(6) 0.041(5) 0.012(6) C48 0.073(7) 0.077(6) 0.072(6) 0.001(5) 0.047(6) 0.017(5) C49 0.068(6) 0.056(5) 0.058(5) 0.004(4) 0.040(5) 0.008(4) C50 0.064(5) 0.043(4) 0.041(4) 0.013(3) 0.041(4) 0.013(4) O1W 0.111(3) 0.110(3) 0.110(3) 0.0000(10) 0.0623(17) 0.0009(10) O4W 0.127(6) 0.126(6) 0.126(6) -0.0001(10) 0.071(4) 0.0003(10) O5W 0.149(8) 0.149(8) 0.149(8) -0.0002(10) 0.084(4) 0.0007(10) O2W 0.113(5) 0.112(5) 0.112(5) -0.0002(10) 0.063(3) 0.0007(10) O3W 0.090(4) 0.089(4) 0.089(4) 0.0000(10) 0.050(3) 0.0002(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O15 2.312(5) . ? Gd1 O7 2.343(5) . ? Gd1 O16 2.348(6) . ? Gd1 O17 2.372(5) . ? Gd1 O3 2.372(5) . ? Gd1 O14 2.375(5) . ? Gd1 O13 2.407(5) . ? Gd1 O15 2.899(5) 3_676 ? Gd1 Gd1 3.9917(9) 3_676 ? Fe1 O3 1.938(6) . ? Fe1 O7 1.965(5) . ? Fe1 O6 1.993(6) . ? Fe1 O12 2.001(5) . ? Fe1 O2 2.015(6) . ? Fe1 O10 2.101(6) . ? Fe2 O5 1.944(7) . ? Fe2 N6 1.964(12) . ? Fe2 O9 2.008(7) . ? Fe2 O6 2.020(5) . ? Fe2 N2 2.119(7) . ? Fe2 O10 2.123(6) . ? Fe3 O1' 1.826(12) . ? Fe3 O2 2.006(7) . ? Fe3 O9 2.011(8) . ? Fe3 N3 2.017(9) . ? Fe3 O1 2.106(14) . ? Fe3 O10 2.125(6) . ? Fe3 N1 2.156(11) . ? Na1 O11 2.166(16) . ? Na1 O5 2.209(10) . ? Na1 O1 2.299(19) . ? Na1 O4 2.36(2) . ? Na1 O8 2.37(2) . ? Na1 O9 2.785(10) . ? Na1' O11' 2.26(4) . ? Na1' O1' 2.333(19) . ? Na1' O4' 2.40(2) . ? Na1' O9 2.615(13) . ? Na1' O5 2.628(15) . ? Na1' O8' 2.67(2) . ? O1 C1 1.358(16) . ? O1' C1' 1.348(14) . ? O2 C10 1.417(13) . ? O3 C9 1.414(11) . ? O4 C13 1.40(3) . ? O4 C6 1.41(2) . ? O4' C6' 1.36(2) . ? O4' C13' 1.45(3) . ? O5 C14 1.347(13) . ? O6 C22 1.450(10) . ? O7 C23 1.431(9) . ? O8 C26 1.40(3) . ? O8 C19 1.421(10) . ? O8' C19 1.467(10) . ? O8' C26' 1.49(2) . ? O9 C27 1.438(12) . ? O10 C28 1.429(10) . ? O11 C29 1.50(2) . ? O11' C29' 1.75(7) . ? O12 C36 1.283(9) . ? O13 C36 1.267(9) . ? O14 C43 1.254(9) . ? O15 C43 1.275(9) 3_676 ? O15 Gd1 2.899(5) 3_676 ? O16 C50 1.267(9) . ? O17 C50 1.262(9) 3_676 ? N1 C7' 1.352(9) . ? N1 C8 1.456(16) . ? N1 C7 1.528(5) . ? N2 C20 1.280(11) . ? N2 C21 1.495(10) . ? N3 N4 1.343(14) . ? N3 N4' 1.404(14) . ? N4 N5 1.280(15) . ? N4' N5' 1.294(15) . ? N6 N7 1.036(14) . ? N7 N8 1.257(15) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 C7 1.5501 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? C1' C2' 1.3900 . ? C1' C6' 1.3900 . ? C2' C3' 1.3900 . ? C2' C7' 1.4152 . ? C3' C4' 1.3900 . ? C3' H3' 0.9300 . ? C4' C5' 1.3900 . ? C4' H4' 0.9300 . ? C5' C6' 1.3900 . ? C5' H5' 0.9300 . ? C7' H7' 0.9300 . ? C8 C9 1.498(13) . ? C8 C10 1.502(14) . ? C8 C11 1.549(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.488(19) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C14 C15 1.387(15) . ? C14 C19 1.401(15) . ? C15 C16 1.378(14) . ? C15 C20 1.445(12) . ? C16 C17 1.358(16) . ? C16 H16 0.9300 . ? C17 C18 1.337(18) . ? C17 H17 0.9300 . ? C18 C19 1.351(17) . ? C18 H18 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.521(11) . ? C21 C23 1.534(10) . ? C21 C24 1.552(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.527(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26G 0.9600 . ? C26 H26H 0.9600 . ? C26 H26I 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C30 C36 1.475(9) . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C37 C38 1.378(12) . ? C37 C42 1.399(11) . ? C37 C43 1.480(11) . ? C38 C39 1.371(13) . ? C38 H38 0.9300 . ? C39 C40 1.397(15) . ? C39 H39 0.9300 . ? C40 C41 1.372(15) . ? C40 H40 0.9300 . ? C41 C42 1.400(13) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 O15 1.275(9) 3_676 ? C44 C45 1.374(12) . ? C44 C49 1.388(12) . ? C44 C50 1.496(12) . ? C45 C46 1.401(14) . ? C45 H45 0.9300 . ? C46 C47 1.381(15) . ? C46 H46 0.9300 . ? C47 C48 1.363(15) . ? C47 H47 0.9300 . ? C48 C49 1.380(14) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 O17 1.262(9) 3_676 ? 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 O15 Gd1 O7 120.33(19) . . ? O15 Gd1 O16 79.03(19) . . ? O7 Gd1 O16 146.72(17) . . ? O15 Gd1 O17 77.45(18) . . ? O7 Gd1 O17 78.22(17) . . ? O16 Gd1 O17 134.73(17) . . ? O15 Gd1 O3 148.26(19) . . ? O7 Gd1 O3 66.29(19) . . ? O16 Gd1 O3 83.30(19) . . ? O17 Gd1 O3 132.22(19) . . ? O15 Gd1 O14 128.60(18) . . ? O7 Gd1 O14 100.54(18) . . ? O16 Gd1 O14 82.90(19) . . ? O17 Gd1 O14 82.40(19) . . ? O3 Gd1 O14 74.22(19) . . ? O15 Gd1 O13 77.75(16) . . ? O7 Gd1 O13 76.81(17) . . ? O16 Gd1 O13 82.16(18) . . ? O17 Gd1 O13 128.68(19) . . ? O3 Gd1 O13 73.85(18) . . ? O14 Gd1 O13 146.02(19) . . ? O15 Gd1 O15 80.61(17) . 3_676 ? O7 Gd1 O15 137.53(16) . 3_676 ? O16 Gd1 O15 67.65(17) . 3_676 ? O17 Gd1 O15 70.72(17) . 3_676 ? O3 Gd1 O15 116.46(17) . 3_676 ? O14 Gd1 O15 48.06(16) . 3_676 ? O13 Gd1 O15 145.62(16) . 3_676 ? O15 Gd1 Gd1 45.77(12) . 3_676 ? O7 Gd1 Gd1 145.91(13) . 3_676 ? O16 Gd1 Gd1 67.27(12) . 3_676 ? O17 Gd1 Gd1 68.56(12) . 3_676 ? O3 Gd1 Gd1 144.69(14) . 3_676 ? O14 Gd1 Gd1 82.87(13) . 3_676 ? O13 Gd1 Gd1 118.46(12) . 3_676 ? O15 Gd1 Gd1 34.84(10) 3_676 3_676 ? O3 Fe1 O7 82.7(2) . . ? O3 Fe1 O6 171.8(2) . . ? O7 Fe1 O6 94.4(2) . . ? O3 Fe1 O12 94.8(2) . . ? O7 Fe1 O12 94.1(2) . . ? O6 Fe1 O12 93.0(2) . . ? O3 Fe1 O2 92.7(3) . . ? O7 Fe1 O2 171.8(2) . . ? O6 Fe1 O2 89.1(2) . . ? O12 Fe1 O2 93.1(2) . . ? O3 Fe1 O10 93.5(2) . . ? O7 Fe1 O10 93.4(2) . . ? O6 Fe1 O10 79.0(2) . . ? O12 Fe1 O10 169.5(2) . . ? O2 Fe1 O10 80.0(3) . . ? O5 Fe2 N6 97.7(5) . . ? O5 Fe2 O9 94.1(3) . . ? N6 Fe2 O9 96.1(5) . . ? O5 Fe2 O6 159.9(2) . . ? N6 Fe2 O6 97.4(4) . . ? O9 Fe2 O6 97.4(3) . . ? O5 Fe2 N2 87.5(3) . . ? N6 Fe2 N2 94.3(5) . . ? O9 Fe2 N2 169.2(3) . . ? O6 Fe2 N2 78.1(2) . . ? O5 Fe2 O10 89.1(3) . . ? N6 Fe2 O10 169.9(5) . . ? O9 Fe2 O10 75.8(2) . . ? O6 Fe2 O10 77.9(2) . . ? N2 Fe2 O10 93.5(2) . . ? O1' Fe3 O2 158.9(4) . . ? O1' Fe3 O9 99.1(5) . . ? O2 Fe3 O9 100.6(3) . . ? O1' Fe3 N3 92.3(5) . . ? O2 Fe3 N3 93.1(3) . . ? O9 Fe3 N3 95.6(3) . . ? O1' Fe3 O1 18.4(4) . . ? O2 Fe3 O1 162.8(4) . . ? O9 Fe3 O1 83.3(4) . . ? N3 Fe3 O1 103.2(4) . . ? O1' Fe3 O10 98.3(4) . . ? O2 Fe3 O10 79.6(2) . . ? O9 Fe3 O10 75.7(2) . . ? N3 Fe3 O10 167.2(3) . . ? O1 Fe3 O10 85.3(4) . . ? O1' Fe3 N1 83.8(5) . . ? O2 Fe3 N1 75.5(3) . . ? O9 Fe3 N1 170.0(3) . . ? N3 Fe3 N1 93.8(4) . . ? O1 Fe3 N1 97.7(5) . . ? O10 Fe3 N1 94.5(3) . . ? O11 Na1 O5 110.4(6) . . ? O11 Na1 O1 141.5(6) . . ? O5 Na1 O1 100.0(5) . . ? O11 Na1 O4 99.4(7) . . ? O5 Na1 O4 140.6(6) . . ? O1 Na1 O4 68.0(7) . . ? O11 Na1 O8 80.0(6) . . ? O5 Na1 O8 70.6(5) . . ? O1 Na1 O8 133.9(7) . . ? O4 Na1 O8 90.7(7) . . ? O11 Na1 O9 104.3(5) . . ? O5 Na1 O9 69.7(3) . . ? O1 Na1 O9 64.3(4) . . ? O4 Na1 O9 127.6(7) . . ? O8 Na1 O9 138.9(6) . . ? O11' Na1' O1' 121.2(12) . . ? O11' Na1' O4' 91.0(12) . . ? O1' Na1' O4' 67.7(6) . . ? O11' Na1' O9 102.1(11) . . ? O1' Na1' O9 72.2(5) . . ? O4' Na1' O9 138.8(7) . . ? O11' Na1' O5 122.7(12) . . ? O1' Na1' O5 108.7(5) . . ? O4' Na1' O5 135.5(6) . . ? O9 Na1' O5 67.0(4) . . ? O11' Na1' O8' 101.2(11) . . ? O1' Na1' O8' 130.5(7) . . ? O4' Na1' O8' 89.0(7) . . ? O9 Na1' O8' 125.3(6) . . ? O5 Na1' O8' 58.7(4) . . ? C1 O1 Fe3 125.4(12) . . ? C1 O1 Na1 121.2(11) . . ? Fe3 O1 Na1 113.0(6) . . ? C1' O1' Fe3 139.5(10) . . ? C1' O1' Na1' 114.6(9) . . ? Fe3 O1' Na1' 100.6(6) . . ? C10 O2 Fe3 112.2(6) . . ? C10 O2 Fe1 114.4(5) . . ? Fe3 O2 Fe1 103.5(3) . . ? C9 O3 Fe1 129.5(5) . . ? C9 O3 Gd1 122.7(5) . . ? Fe1 O3 Gd1 103.8(3) . . ? C13 O4 C6 116.9(19) . . ? C13 O4 Na1 130.7(16) . . ? C6 O4 Na1 111.3(13) . . ? C6' O4' C13' 114.3(17) . . ? C6' O4' Na1' 114.7(8) . . ? C13' O4' Na1' 130.4(17) . . ? C14 O5 Fe2 133.0(6) . . ? C14 O5 Na1 118.3(6) . . ? Fe2 O5 Na1 108.3(4) . . ? C14 O5 Na1' 125.1(6) . . ? Fe2 O5 Na1' 99.6(4) . . ? Na1 O5 Na1' 12.4(3) . . ? C22 O6 Fe1 115.4(4) . . ? C22 O6 Fe2 109.7(5) . . ? Fe1 O6 Fe2 104.8(2) . . ? C23 O7 Fe1 125.4(4) . . ? C23 O7 Gd1 124.3(4) . . ? Fe1 O7 Gd1 103.9(2) . . ? C26 O8 C19 113.9(18) . . ? C26 O8 Na1 135.3(14) . . ? C19 O8 Na1 109.9(12) . . ? C19 O8' C26' 116.5(15) . . ? C19 O8' Na1' 123.2(10) . . ? C26' O8' Na1' 119.6(12) . . ? C27 O9 Fe2 123.3(7) . . ? C27 O9 Fe3 123.8(7) . . ? Fe2 O9 Fe3 107.6(3) . . ? C27 O9 Na1' 105.9(6) . . ? Fe2 O9 Na1' 98.3(4) . . ? Fe3 O9 Na1' 87.1(3) . . ? C27 O9 Na1 105.0(6) . . ? Fe2 O9 Na1 87.8(3) . . ? Fe3 O9 Na1 98.7(3) . . ? Na1' O9 Na1 13.8(2) . . ? C28 O10 Fe1 117.4(4) . . ? C28 O10 Fe2 120.7(6) . . ? Fe1 O10 Fe2 97.6(2) . . ? C28 O10 Fe3 120.1(5) . . ? Fe1 O10 Fe3 96.7(3) . . ? Fe2 O10 Fe3 99.5(2) . . ? C29 O11 Na1 115.9(11) . . ? C29' O11' Na1' 124(3) . . ? C36 O12 Fe1 125.4(5) . . ? C36 O13 Gd1 137.6(5) . . ? C43 O14 Gd1 108.2(5) . . ? C43 O15 Gd1 178.0(5) 3_676 . ? C43 O15 Gd1 82.6(4) 3_676 3_676 ? Gd1 O15 Gd1 99.39(17) . 3_676 ? C50 O16 Gd1 139.2(5) . . ? C50 O17 Gd1 135.9(5) 3_676 . ? C7' N1 C8 112.9(9) . . ? C7' N1 C7 22.4(8) . . ? C8 N1 C7 132.2(10) . . ? C7' N1 Fe3 129.8(9) . . ? C8 N1 Fe3 117.3(5) . . ? C7 N1 Fe3 109.1(10) . . ? C20 N2 C21 119.5(7) . . ? C20 N2 Fe2 125.7(6) . . ? C21 N2 Fe2 114.8(5) . . ? N4 N3 N4' 128.2(12) . . ? N4 N3 Fe3 107.7(9) . . ? N4' N3 Fe3 123.1(9) . . ? N5 N4 N3 173.0(19) . . ? N5' N4' N3 173.6(18) . . ? N7 N6 Fe2 158.9(15) . . ? N6 N7 N8 164.0(18) . . ? O1 C1 C2 129.7(11) . . ? O1 C1 C6 110.3(11) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 C7 121.8 . . ? C1 C2 C7 118.2 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 O4 118.0(13) . . ? C1 C6 O4 122.0(13) . . ? N1 C7 C2 138.0(10) . . ? N1 C7 H7 111.0 . . ? C2 C7 H7 111.0 . . ? O1' C1' C2' 119.7(8) . . ? O1' C1' C6' 120.3(8) . . ? C2' C1' C6' 120.0 . . ? C3' C2' C1' 120.0 . . ? C3' C2' C7' 112.0 . . ? C1' C2' C7' 128.0 . . ? C4' C3' C2' 120.0 . . ? C4' C3' H3' 120.0 . . ? C2' C3' H3' 120.0 . . ? C3' C4' C5' 120.0 . . ? C3' C4' H4' 120.0 . . ? C5' C4' H4' 120.0 . . ? C6' C5' C4' 120.0 . . ? C6' C5' H5' 120.0 . . ? C4' C5' H5' 120.0 . . ? O4' C6' C5' 125.3(9) . . ? O4' C6' C1' 114.7(9) . . ? C5' C6' C1' 120.0 . . ? N1 C7' C2' 118.5(8) . . ? N1 C7' H7' 120.8 . . ? C2' C7' H7' 120.8 . . ? N1 C8 C9 108.5(9) . . ? N1 C8 C10 103.1(9) . . ? C9 C8 C10 113.3(8) . . ? N1 C8 C11 113.1(9) . . ? C9 C8 C11 109.1(9) . . ? C10 C8 C11 109.9(10) . . ? O3 C9 C8 114.9(8) . . ? O3 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? O3 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? O2 C10 C8 111.9(9) . . ? O2 C10 H10A 109.2 . . ? C8 C10 H10A 109.2 . . ? O2 C10 H10B 109.2 . . ? C8 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C8 117.2(11) . . ? C12 C11 H11A 108.0 . . ? C8 C11 H11A 108.0 . . ? C12 C11 H11B 108.0 . . ? C8 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4' C13' H13D 109.5 . . ? O4' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? O4' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? O5 C14 C15 122.8(8) . . ? O5 C14 C19 118.2(10) . . ? C15 C14 C19 118.9(10) . . ? C16 C15 C14 117.5(9) . . ? C16 C15 C20 118.6(9) . . ? C14 C15 C20 123.9(8) . . ? C17 C16 C15 123.9(11) . . ? C17 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? C18 C17 C16 117.0(12) . . ? C18 C17 H17 121.5 . . ? C16 C17 H17 121.5 . . ? C17 C18 C19 123.4(13) . . ? C17 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C18 C19 C14 119.3(11) . . ? C18 C19 O8 124.3(14) . . ? C14 C19 O8 114.3(13) . . ? C18 C19 O8' 127.9(13) . . ? C14 C19 O8' 111.7(11) . . ? O8 C19 O8' 24.1(10) . . ? N2 C20 C15 127.0(8) . . ? N2 C20 H20 116.5 . . ? C15 C20 H20 116.5 . . ? N2 C21 C22 105.9(6) . . ? N2 C21 C23 108.5(6) . . ? C22 C21 C23 111.1(6) . . ? N2 C21 C24 112.9(6) . . ? C22 C21 C24 109.5(6) . . ? C23 C21 C24 109.0(6) . . ? O6 C22 C21 110.0(6) . . ? O6 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? O6 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? O7 C23 C21 114.7(6) . . ? O7 C23 H23A 108.6 . . ? C21 C23 H23A 108.6 . . ? O7 C23 H23B 108.6 . . ? C21 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C21 116.1(7) . . ? C25 C24 H24A 108.3 . . ? C21 C24 H24A 108.3 . . ? C25 C24 H24B 108.3 . . ? C21 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O8 C26 H26G 109.5 . . ? O8 C26 H26H 109.5 . . ? H26G C26 H26H 109.5 . . ? O8 C26 H26I 109.5 . . ? H26G C26 H26I 109.5 . . ? H26H C26 H26I 109.5 . . ? O8' C26' H26D 109.5 . . ? O8' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? O8' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? O9 C27 H27A 109.5 . . ? O9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O10 C28 H28A 109.5 . . ? O10 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O10 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C30 C35 120.0 . . ? C31 C30 C36 120.9(5) . . ? C35 C30 C36 119.1(5) . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? O13 C36 O12 125.1(7) . . ? O13 C36 C30 119.7(7) . . ? O12 C36 C30 115.2(6) . . ? C38 C37 C42 119.0(8) . . ? C38 C37 C43 120.3(7) . . ? C42 C37 C43 120.7(7) . . ? C39 C38 C37 121.9(9) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 119.1(10) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C41 C40 C39 120.1(9) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.4(9) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C37 C42 C41 119.3(9) . . ? C37 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? O14 C43 O15 120.9(7) . 3_676 ? O14 C43 C37 118.0(7) . . ? O15 C43 C37 121.1(7) 3_676 . ? C45 C44 C49 117.3(8) . . ? C45 C44 C50 121.4(7) . . ? C49 C44 C50 121.2(7) . . ? C44 C45 C46 122.4(8) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C47 C46 C45 118.2(9) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C48 C47 C46 120.3(10) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C49 120.6(9) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C48 C49 C44 121.1(8) . . ? C48 C49 H49 119.5 . . ? C44 C49 H49 119.5 . . ? O17 C50 O16 125.8(7) 3_676 . ? O17 C50 C44 117.9(7) 3_676 . ? O16 C50 C44 116.4(7) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.432 _refine_diff_density_min -1.194 _refine_diff_density_rms 0.113 _iucr_refine_instructions_details ; TITL sad in P2(1)/c CELL 0.71073 12.6587 35.2046 17.1800 90.000 124.368 90.000 ZERR 2.00 0.0025 0.0070 0.0034 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Na Fe Gd UNIT 200 252 32 80 4 12 4 omit 0 50 omit 0 8 0 omit -4 2 6 omit -2 4 2 omit 0 10 1 omit -2 8 2 omit 1 11 0 omit -2 7 1 omit 2 1 2 omit 0 3 2 omit 1 4 3 omit -2 6 1 omit -4 1 2 omit -1 1 3 omit -3 9 1 omit -1 2 5 omit -6 2 6 omit 2 3 0 omit -1 1 4 omit -1 5 4 omit -2 2 1 omit 0 4 2 omit 0 6 1 omit 0 1 3 omit -3 0 4 omit -5 5 5 omit -1 6 6 omit -4 8 3 omit -3 8 2 omit -2 1 2 omit -2 3 2 omit 3 11 0 omit 2 0 2 omit -3 3 2 omit -3 1 3 omit -4 10 4 omit -2 0 2 omit 1 10 0 omit -1 6 3 omit 0 9 1 omit -4 1 4 omit 1 4 4 omit 2 10 0 omit -2 7 3 omit 4 5 0 omit 1 7 2 omit 0 12 0 L.S. 20 BOND $h acta SHEL 0.5 2.5 htab free o5w n5' free c29 na1 free na1' c1' free na1' fe3 free fe1 gd1 free c43 gd1 free fe2 na1 free fe2 na1' free c14 na1 free c19 na1 isor 0.01 0.01 o8 o8' c26 c26' isor 0.001 0.001 na1' o1 o1' o4 o8 o11 o11' c5' c11 c12 c13 c13' isor 0.001 0.001 c17 c18 c19 c26 c29 c29' c4' isor 0.001 0.001 o1w o2w o3w o4w o5w n4' n5' simu 0.001 0.001 1.5 c1 c2 c3 c4 c5 c6 c7 simu 0.001 0.001 1.5 c1' c2' c3' c4' c5' c6' c7' simu 0.001 0.001 1.5 c30 c31 c32 c33 c34 c35 dfix 1.35 0.02 n3 n4 n4 n5 n3 n4' n4' n5' dfix 1.33 0.01 c2' c7' c7' n1 dfix 1.45 0.01 o8' c19 dfix 1.45 0.01 o8 c19 dfix 1.50 0.005 c2 c7 dfix 1.55 0.005 c7 n1 SIMU 0.001 0.001 4.0 N3 N4 N5 N4' N5' SIMU 0.001 0.001 1.7 N6 N7 N8 FMAP 2 PLAN 20 WGHT 0.0839 17.4650 FVAR 0.14547 GD1 7 0.516566 0.974632 0.403488 11.00000 0.06164 0.03997 = 0.04000 0.00054 0.04021 0.00262 FE1 6 0.544178 0.925873 0.244870 11.00000 0.06935 0.04506 = 0.04824 -0.00693 0.04622 -0.00414 FE2 6 0.751703 0.862572 0.292504 11.00000 0.09898 0.04184 = 0.07254 -0.00297 0.06897 0.00626 FE3 6 0.448907 0.842448 0.170624 11.00000 0.12411 0.05677 = 0.09016 -0.03235 0.08579 -0.03036 PART 1 NA1 5 0.695815 0.770898 0.314332 10.50000 0.06607 0.02838 = 0.06304 -0.01594 0.02950 -0.00801 PART 2 NA1' 5 0.632035 0.771361 0.284705 10.50000 0.08267 0.08158 = 0.08270 -0.00021 0.04672 0.00028 PART 1 O1 4 0.494026 0.793877 0.255460 10.50000 0.05963 0.05919 = 0.05983 -0.00054 0.03346 -0.00014 PART 2 O1' 4 0.432227 0.799254 0.221675 10.50000 0.04910 0.04849 = 0.04901 -0.00035 0.02759 0.00045 PART 0 O2 4 0.422611 0.896455 0.126103 11.00000 0.07646 0.06643 = 0.06448 -0.02451 0.04948 -0.01485 O3 4 0.417456 0.932239 0.273470 11.00000 0.07468 0.05908 = 0.05179 -0.00923 0.05129 -0.00715 PART 1 O4 4 0.566999 0.725803 0.325645 10.50000 0.08771 0.08733 = 0.08793 0.00003 0.04940 -0.00028 PART 2 O4' 4 0.494800 0.732584 0.306623 10.50000 0.12051 0.01048 = 0.08916 0.00155 0.05312 -0.01288 PART 0 O5 4 0.810322 0.822354 0.385728 11.00000 0.12565 0.04081 = 0.09412 0.00588 0.07888 0.01584 O6 4 0.685338 0.913651 0.229676 11.00000 0.07975 0.04140 = 0.05264 -0.00025 0.05055 0.00410 O7 4 0.657572 0.949028 0.369961 11.00000 0.07025 0.03845 = 0.04194 -0.00287 0.04422 0.00061 PART 1 O8 4 0.872789 0.754707 0.467213 10.50000 0.08590 0.08512 = 0.08574 -0.00004 0.04844 0.00030 PART 2 O8' 4 0.823309 0.757771 0.463783 10.50000 0.09979 0.06610 = 0.10717 0.03244 0.06885 0.02489 PART 0 O9 4 0.615203 0.830519 0.186194 11.00000 0.13128 0.04616 = 0.08350 -0.00902 0.08670 0.00088 O10 4 0.589699 0.870184 0.298058 11.00000 0.09822 0.04590 = 0.07061 -0.01217 0.07181 -0.01009 PART 1 O11 4 0.797782 0.733324 0.278467 10.75000 0.11058 0.11019 = 0.11024 -0.00151 0.06231 0.00098 PART 2 O11' 4 0.658059 0.723458 0.209506 10.25000 0.11339 0.11326 = 0.11338 -0.00010 0.06398 0.00006 PART 0 O12 4 0.504802 0.975245 0.175980 11.00000 0.07464 0.04988 = 0.04430 -0.00254 0.04489 0.00351 O13 4 0.471709 1.011134 0.269566 11.00000 0.07118 0.04374 = 0.04063 0.00054 0.04052 0.00822 O14 4 0.465915 0.919403 0.455583 11.00000 0.08006 0.04466 = 0.06018 0.00304 0.05591 0.00187 O15 4 0.542818 1.036276 0.457913 11.00000 0.07421 0.03985 = 0.04318 -0.00121 0.04261 0.00247 O16 4 0.304365 0.991105 0.345016 11.00000 0.06226 0.04450 = 0.05021 -0.00242 0.03963 0.00226 O17 4 0.709794 0.970867 0.555895 11.00000 0.06342 0.05350 = 0.04032 0.00060 0.03883 0.00184 N1 3 0.290125 0.862039 0.173965 11.00000 0.12262 0.11274 = 0.09224 -0.06158 0.09107 -0.07249 N2 3 0.867036 0.900442 0.405791 11.00000 0.07164 0.04502 = 0.06216 0.00660 0.05329 0.01448 N3 3 0.335919 0.821755 0.038417 11.00000 0.08180 0.08072 = 0.08053 -0.00252 0.04605 0.00034 PART 1 N4 3 0.283472 0.789349 0.042684 10.50000 0.08145 0.08059 = 0.08030 -0.00227 0.04615 0.00045 N5 3 0.221204 0.759618 0.036990 10.50000 0.08171 0.08077 = 0.08047 -0.00231 0.04592 0.00043 PART 2 N4' 3 0.303493 0.842586 -0.041942 10.50000 0.08149 0.08070 = 0.08063 -0.00196 0.04581 0.00044 N5' 3 0.277551 0.858521 -0.118775 10.50000 0.08107 0.08030 = 0.08019 -0.00180 0.04601 0.00040 PART 0 N6 3 0.879488 0.855567 0.263095 11.00000 0.15005 0.14119 = 0.14122 -0.00996 0.12154 0.00318 N7 3 0.916290 0.851852 0.222932 11.00000 0.15130 0.14227 = 0.14271 -0.00881 0.11966 0.00242 N8 3 0.928503 0.847225 0.155847 11.00000 0.15319 0.14352 = 0.14448 -0.00855 0.11721 0.00201 AFIX 66 PART 1 C1 1 0.421775 0.779490 0.284123 10.50000 0.09432 0.09652 = 0.08964 -0.03408 0.05606 -0.04796 C2 1 0.322348 0.796198 0.284205 10.50000 0.09439 0.09672 = 0.08976 -0.03420 0.05593 -0.04790 C3 1 0.265319 0.776757 0.321769 10.50000 0.09444 0.09698 = 0.08979 -0.03404 0.05606 -0.04794 AFIX 41 H3 2 0.198796 0.787935 0.321824 10.50000 10.10000 AFIX 65 C4 1 0.307715 0.740607 0.359251 10.50000 0.09429 0.09696 = 0.08984 -0.03379 0.05619 -0.04801 AFIX 41 H4 2 0.269558 0.727600 0.384384 10.50000 10.10000 AFIX 65 C5 1 0.407142 0.723899 0.359169 10.50000 0.09430 0.09684 = 0.08982 -0.03374 0.05616 -0.04794 AFIX 41 H5 2 0.435507 0.699713 0.384247 10.50000 10.10000 AFIX 65 C6 1 0.464172 0.743340 0.321606 10.50000 0.09437 0.09661 = 0.08983 -0.03385 0.05596 -0.04797 C7 1 0.273448 0.835621 0.236835 10.50000 0.07760 0.15068 = 0.07428 -0.08609 0.04101 -0.02246 AFIX 41 H7 2 0.218400 0.846171 0.250572 10.50000 10.10000 AFIX 66 PART 2 C1' 1 0.369679 0.786758 0.259315 10.50000 0.06179 0.05926 = 0.05952 0.00089 0.03454 -0.00336 C2' 1 0.275266 0.809229 0.253638 10.50000 0.06178 0.05908 = 0.05924 0.00086 0.03455 -0.00339 C3' 1 0.211603 0.796755 0.293441 10.50000 0.06138 0.05940 = 0.05958 0.00091 0.03445 -0.00283 AFIX 41 H3' 2 0.148435 0.811790 0.289642 10.50000 10.10000 AFIX 65 C4' 1 0.242352 0.761810 0.338921 10.50000 0.06106 0.05993 = 0.06014 0.00065 0.03423 -0.00180 AFIX 41 H4' 2 0.199756 0.753465 0.365552 10.50000 10.10000 AFIX 65 C5' 1 0.336764 0.739339 0.344599 10.50000 0.06118 0.06008 = 0.06029 0.00056 0.03420 -0.00171 AFIX 41 H5' 2 0.357336 0.715959 0.375028 10.50000 10.10000 AFIX 65 C6' 1 0.400428 0.751812 0.304796 10.50000 0.06155 0.05961 = 0.06007 0.00076 0.03432 -0.00275 C7' 1 0.229790 0.844966 0.209079 10.50000 0.06186 0.05896 = 0.05879 0.00079 0.03482 -0.00381 AFIX 41 H7' 2 0.160016 0.856446 0.204060 10.50000 10.10000 AFIX 0 PART 0 C8 1 0.238766 0.899534 0.135052 11.00000 0.08631 0.09076 = 0.08557 -0.03636 0.06969 -0.03326 C9 1 0.283549 0.926659 0.215086 11.00000 0.06909 0.09319 = 0.07256 -0.03997 0.05258 -0.03182 AFIX 21 H9A 2 0.242657 0.951030 0.189404 11.00000 10.10000 H9B 2 0.255378 0.917374 0.253691 11.00000 10.10000 AFIX 0 C10 1 0.292942 0.907887 0.078410 11.00000 0.07874 0.08689 = 0.07312 -0.03989 0.04972 -0.03114 AFIX 21 H10A 2 0.242699 0.894734 0.018426 11.00000 10.10000 H10B 2 0.286691 0.934928 0.065665 11.00000 10.10000 AFIX 0 C11 1 0.090678 0.900322 0.070165 11.00000 0.09792 0.09842 = 0.09782 -0.00091 0.05573 -0.00057 AFIX 21 H11A 2 0.062254 0.877803 0.030781 11.00000 10.10000 H11B 2 0.058673 0.898469 0.109716 11.00000 10.10000 AFIX 0 C12 1 0.029867 0.933923 0.007613 11.00000 0.11085 0.11147 = 0.11070 -0.00047 0.06276 -0.00002 AFIX 31 H12A 2 -0.061536 0.931465 -0.027817 11.00000 10.10000 H12B 2 0.056101 0.935418 -0.034940 11.00000 10.10000 H12C 2 0.055790 0.956572 0.045227 11.00000 10.10000 AFIX 0 PART 1 C13 1 0.588586 0.687226 0.350846 10.50000 0.08313 0.08290 = 0.08341 0.00016 0.04687 -0.00032 AFIX 31 H13A 2 0.659446 0.678267 0.349856 10.50000 10.10000 H13B 2 0.513404 0.672841 0.306816 10.50000 10.10000 H13C 2 0.607660 0.684204 0.413089 10.50000 10.10000 AFIX 0 PART 2 C13' 1 0.506844 0.693191 0.334725 10.50000 0.07938 0.07901 = 0.07930 0.00012 0.04476 0.00005 AFIX 31 H13D 2 0.574201 0.681416 0.333382 10.50000 10.10000 H13E 2 0.427702 0.680197 0.291978 10.50000 10.10000 H13F 2 0.526614 0.691842 0.397449 10.50000 10.10000 AFIX 0 PART 0 C14 1 0.892278 0.821748 0.480291 11.00000 0.12068 0.04635 = 0.08769 0.02390 0.07860 0.02933 C15 1 0.953558 0.854036 0.533166 11.00000 0.09212 0.05581 = 0.06671 0.01090 0.05990 0.01463 C16 1 1.033447 0.849921 0.629666 11.00000 0.11903 0.07430 = 0.07849 0.02831 0.07712 0.02491 AFIX 41 H16 2 1.075094 0.871407 0.665705 11.00000 10.10000 AFIX 0 C17 1 1.054932 0.816333 0.675229 11.00000 0.09582 0.09528 = 0.09476 0.00067 0.05390 0.00023 AFIX 41 H17 2 1.108619 0.814682 0.740603 11.00000 10.10000 AFIX 0 C18 1 0.995416 0.785744 0.621858 11.00000 0.09962 0.09876 = 0.09871 0.00099 0.05600 -0.00021 AFIX 41 H18 2 1.010936 0.762350 0.651617 11.00000 10.10000 AFIX 0 C19 1 0.913940 0.787046 0.526993 11.00000 0.09341 0.09273 = 0.09299 0.00012 0.05265 0.00014 C20 1 0.938198 0.891361 0.493100 11.00000 0.06947 0.04951 = 0.06516 0.00986 0.05505 0.01344 AFIX 41 H20 2 0.985071 0.910896 0.535298 11.00000 10.10000 AFIX 0 C21 1 0.859299 0.941064 0.377597 11.00000 0.06321 0.04299 = 0.04371 0.00690 0.04151 0.00992 C22 1 0.789466 0.940859 0.270892 11.00000 0.06843 0.04889 = 0.05208 0.00631 0.04596 0.00601 AFIX 21 H22A 2 0.755933 0.966007 0.246157 11.00000 10.10000 H22B 2 0.848670 0.934182 0.254237 11.00000 10.10000 AFIX 0 C23 1 0.783555 0.963249 0.407636 11.00000 0.05000 0.04375 = 0.05080 -0.00071 0.03682 0.00154 AFIX 21 H23A 2 0.831408 0.962931 0.475918 11.00000 10.10000 H23B 2 0.776811 0.989495 0.388146 11.00000 10.10000 AFIX 0 C24 1 0.992791 0.959758 0.422966 11.00000 0.06056 0.05563 = 0.05978 0.00226 0.04385 0.00170 AFIX 21 H24A 2 0.981020 0.984407 0.393875 11.00000 10.10000 H24B 2 1.028892 0.964056 0.489248 11.00000 10.10000 AFIX 0 C25 1 1.089848 0.937398 0.415239 11.00000 0.07335 0.06937 = 0.07842 0.01406 0.05636 0.01582 AFIX 31 H25A 2 1.168297 0.951496 0.444491 11.00000 10.10000 H25B 2 1.056394 0.933284 0.349969 11.00000 10.10000 H25C 2 1.105883 0.913354 0.446400 11.00000 10.10000 AFIX 0 PART 1 C26 1 0.931334 0.720789 0.514733 10.50000 0.09749 0.09727 = 0.09754 0.00014 0.05491 0.00005 AFIX 31 H26G 2 0.892095 0.699836 0.471776 10.50000 10.10000 H26H 2 0.921286 0.717580 0.565706 10.50000 10.10000 H26I 2 1.020784 0.721684 0.539314 10.50000 10.10000 AFIX 0 PART 2 C26' 1 0.854370 0.717928 0.498591 10.50000 0.08606 0.04989 = 0.09236 0.02110 0.04204 0.00394 AFIX 31 H26D 2 0.792868 0.701055 0.450033 10.50000 10.10000 H26E 2 0.851857 0.715388 0.553162 10.50000 10.10000 H26F 2 0.938421 0.711634 0.515035 10.50000 10.10000 AFIX 0 PART 0 C27 1 0.624085 0.816063 0.111797 11.00000 0.11993 0.07441 = 0.08862 -0.01880 0.07307 0.00262 AFIX 31 H27A 2 0.712477 0.812841 0.134823 11.00000 10.10000 H27B 2 0.584701 0.833672 0.060107 11.00000 10.10000 H27C 2 0.581008 0.792024 0.090790 11.00000 10.10000 AFIX 0 C28 1 0.597515 0.862680 0.382899 11.00000 0.11426 0.03656 = 0.07113 -0.00411 0.07199 -0.00331 AFIX 31 H28A 2 0.617548 0.836363 0.399343 11.00000 10.10000 H28B 2 0.516924 0.868462 0.373451 11.00000 10.10000 H28C 2 0.663326 0.878174 0.432909 11.00000 10.10000 AFIX 0 part 1 C29 1 0.928375 0.746141 0.308647 10.75000 0.11393 0.11369 = 0.11384 -0.00026 0.06434 0.00017 part 2 C29' 1 0.554215 0.714459 0.088216 10.25000 0.09144 0.09137 = 0.09143 0.00008 0.05160 -0.00007 part 0 AFIX 66 C30 1 0.421469 1.036115 0.124052 11.00000 0.11544 0.07455 = 0.05550 0.01179 0.04994 0.00783 C31 1 0.347391 1.065698 0.122249 11.00000 0.11580 0.07476 = 0.05694 0.01199 0.04860 0.00788 AFIX 41 H31 2 0.330543 1.067219 0.168304 11.00000 10.10000 AFIX 65 C32 1 0.298494 1.093007 0.051611 11.00000 0.11677 0.07540 = 0.05852 0.01208 0.04699 0.00800 AFIX 41 H32 2 0.248931 1.112800 0.050405 11.00000 10.10000 AFIX 65 C33 1 0.323675 1.090734 -0.017224 11.00000 0.11763 0.07609 = 0.05862 0.01247 0.04659 0.00784 AFIX 41 H33 2 0.290959 1.109006 -0.064485 11.00000 10.10000 AFIX 65 C34 1 0.397753 1.061152 -0.015421 11.00000 0.11764 0.07626 = 0.05778 0.01203 0.04790 0.00771 AFIX 41 H34 2 0.414600 1.059631 -0.061476 11.00000 10.10000 AFIX 65 C35 1 0.446650 1.033842 0.055216 11.00000 0.11650 0.07553 = 0.05632 0.01184 0.04945 0.00760 AFIX 41 H35 2 0.496214 1.014050 0.056422 11.00000 10.10000 AFIX 0 C36 1 0.468664 1.005742 0.195436 11.00000 0.05345 0.05427 = 0.04231 -0.00433 0.02961 -0.00343 C37 1 0.391106 0.900353 0.547160 11.00000 0.05098 0.04790 = 0.04986 0.00875 0.03581 0.00872 C38 1 0.345240 0.866323 0.499903 11.00000 0.08124 0.04901 = 0.06871 -0.00244 0.05268 -0.00473 AFIX 41 H38 2 0.350589 0.861404 0.449042 11.00000 10.10000 AFIX 0 C39 1 0.291964 0.839515 0.525688 11.00000 0.12954 0.05519 = 0.10948 -0.00529 0.08847 -0.02110 AFIX 41 H39 2 0.258618 0.817166 0.491284 11.00000 10.10000 AFIX 0 C40 1 0.288431 0.846216 0.604340 11.00000 0.11749 0.07360 = 0.09852 0.01114 0.08257 -0.01504 AFIX 41 H40 2 0.256349 0.827730 0.624385 11.00000 10.10000 AFIX 0 C41 1 0.332199 0.880014 0.652060 11.00000 0.12242 0.07458 = 0.07973 0.01300 0.08005 -0.00798 AFIX 41 H41 2 0.326568 0.884729 0.702872 11.00000 10.10000 AFIX 0 C42 1 0.385273 0.907452 0.624791 11.00000 0.08377 0.05560 = 0.05501 0.01220 0.04742 0.00899 AFIX 41 H42 2 0.416332 0.930158 0.657920 11.00000 10.10000 AFIX 0 C43 1 0.441896 0.929362 0.514149 11.00000 0.05650 0.04308 = 0.04531 0.00422 0.03521 0.00466 C44 1 0.104706 1.018402 0.291135 11.00000 0.06796 0.04868 = 0.04835 0.01085 0.04360 0.01045 C45 1 0.038921 0.994455 0.214894 11.00000 0.07223 0.06269 = 0.05868 0.00303 0.04234 0.01477 AFIX 41 H45 2 0.082992 0.974735 0.209162 11.00000 10.10000 AFIX 0 C46 1 -0.092101 0.998671 0.145508 11.00000 0.07272 0.08100 = 0.05697 -0.00396 0.03513 0.00243 AFIX 41 H46 2 -0.135248 0.981625 0.095599 11.00000 10.10000 AFIX 0 C47 1 -0.155534 1.028820 0.153177 11.00000 0.07597 0.08419 = 0.06563 0.01285 0.04069 0.01242 AFIX 41 H47 2 -0.241765 1.032815 0.106689 11.00000 10.10000 AFIX 0 C48 1 -0.092276 1.052730 0.228576 11.00000 0.07273 0.07685 = 0.07215 0.00115 0.04693 0.01709 AFIX 41 H48 2 -0.136113 1.072685 0.233740 11.00000 10.10000 AFIX 0 C49 1 0.036222 1.047618 0.297351 11.00000 0.06809 0.05596 = 0.05819 0.00441 0.04024 0.00786 AFIX 41 H49 2 0.077602 1.064026 0.348716 11.00000 10.10000 AFIX 0 C50 1 0.243678 1.012544 0.366092 11.00000 0.06434 0.04274 = 0.04141 0.01310 0.04131 0.01276 part 1 O1W 4 0.726402 0.667839 0.179562 11.00000 0.11090 0.10977 = 0.10958 -0.00003 0.06227 0.00090 O4W 4 0.601370 0.707325 0.053839 10.50000 0.12661 0.12634 = 0.12649 -0.00014 0.07131 0.00031 O5W 4 0.363787 0.881096 -0.093836 10.50000 0.14882 0.14888 = 0.14855 -0.00021 0.08395 0.00071 part 2 O2W 4 0.789200 0.629890 0.206900 10.50000 0.11253 0.11171 = 0.11226 -0.00019 0.06325 0.00073 O3W 4 0.667279 0.669990 0.081847 10.50000 0.09003 0.08945 = 0.08947 -0.00003 0.05043 0.00016 part 0 HKLF 4 REM sad in P2(1)/c REM R1 = 0.0700 for 7495 Fo > 4sig(Fo) and 0.1021 for all 10709 data REM 877 parameters refined using 370 restraints END ; #======================END #=========================END data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 874772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C98 H110 Fe6 N16 Na2 O34 Y2' _chemical_formula_sum 'C98 H110 Fe6 N16 Na2 O34 Y2' _chemical_formula_weight 2614.92 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' Na Na 0.0362 0.0249 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6479(5) _cell_length_b 35.2806(13) _cell_length_c 16.9188(9) _cell_angle_alpha 90.00 _cell_angle_beta 126.420(3) _cell_angle_gamma 90.00 _cell_volume 6075.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10288 _cell_measurement_theta_min 8.19 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 1.725 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7357 _exptl_absorpt_correction_T_max 0.7518 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 32484 _diffrn_reflns_av_R_equivalents 0.1018 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 8.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10288 _reflns_number_gt 7740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+24.4044P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10288 _refine_ls_number_parameters 775 _refine_ls_number_restraints 111 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.202 _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 Y1 Y 0.51200(6) 0.973704(17) 0.39966(4) 0.02725(17) Uani 1 1 d . . . Fe1 Fe 0.53726(8) 0.92299(2) 0.24363(6) 0.0260(2) Uani 1 1 d . . . Fe2 Fe 0.43693(11) 0.83923(3) 0.17050(7) 0.0390(3) Uani 1 1 d . A . Fe3 Fe 0.74825(10) 0.85923(3) 0.30205(7) 0.0369(3) Uani 1 1 d . . . Na1 Na 0.6635(4) 0.76829(10) 0.3160(3) 0.0798(11) Uani 1 1 d U . . O1 O 0.4489(6) 0.79562(14) 0.2437(4) 0.0572(14) Uani 1 1 d . . . O2 O 0.4137(4) 0.89265(12) 0.1219(3) 0.0303(10) Uani 1 1 d . A . O3 O 0.4079(4) 0.93091(12) 0.2696(3) 0.0282(9) Uani 1 1 d . A . O4 O 0.5167(8) 0.73114(17) 0.3358(5) 0.0802(19) Uani 1 1 d U A . O5 O 0.8102(5) 0.82010(14) 0.4004(4) 0.0518(13) Uani 1 1 d . . . O6 O 0.6562(4) 0.94798(12) 0.3726(3) 0.0275(9) Uani 1 1 d . . . O7 O 0.6816(4) 0.90942(11) 0.2325(3) 0.0284(9) Uani 1 1 d . . . O8 O 0.8463(8) 0.7556(2) 0.4880(6) 0.101(2) Uani 1 1 d U . . O9 O 0.706(2) 0.7165(6) 0.2475(16) 0.139(6) Uani 0.50 1 d PU . . O10 O 0.5838(4) 0.86839(11) 0.3038(3) 0.0285(9) Uani 1 1 d . . . O11 O 0.6073(5) 0.82607(13) 0.1923(4) 0.0461(12) Uani 1 1 d . . . O12 O 0.5444(5) 1.03501(13) 0.4504(3) 0.0400(11) Uani 1 1 d . . . O13 O 0.4675(5) 0.92268(13) 0.4610(3) 0.0452(12) Uani 1 1 d . . . O14 O 0.7071(4) 0.97095(14) 0.5582(3) 0.0397(11) Uani 1 1 d . . . O15 O 0.3030(4) 0.99039(14) 0.3415(3) 0.0394(11) Uani 1 1 d . . . O16 O 0.4967(4) 0.97209(12) 0.1696(3) 0.0349(10) Uani 1 1 d . . . O17 O 0.4630(5) 1.00790(12) 0.2620(3) 0.0386(11) Uani 1 1 d . . . N1 N 0.3174(8) 0.8166(2) 0.0354(6) 0.071(2) Uani 1 1 d D . . N2 N 0.2071(9) 0.8084(5) -0.0101(16) 0.050(6) Uani 0.30 1 d PDU A 1 N3 N 0.1017(13) 0.7977(9) -0.052(2) 0.103(10) Uani 0.30 1 d PDU A 1 N2' N 0.243(2) 0.7916(7) 0.0287(15) 0.080(5) Uani 0.50 1 d PU A 2 N3' N 0.158(3) 0.7705(9) 0.013(2) 0.138(8) Uani 0.50 1 d PU A 2 N2" N 0.310(3) 0.8395(9) -0.041(2) 0.050(8) Uani 0.20 1 d PU A 3 N3" N 0.301(4) 0.8578(10) -0.106(3) 0.062(9) Uani 0.20 1 d PU A 3 N4 N 0.8803(7) 0.8489(2) 0.2768(6) 0.0662(19) Uani 1 1 d U . . N5 N 0.9115(8) 0.8577(3) 0.2290(7) 0.081(2) Uani 1 1 d U . . N6 C 0.9433(12) 0.8657(4) 0.1808(10) 0.106(3) Uani 1 1 d U . . N7 N 0.2802(5) 0.85834(16) 0.1732(4) 0.0365(13) Uani 1 1 d . . . N8 N 0.8694(5) 0.89795(15) 0.4177(4) 0.0342(13) Uani 1 1 d . . . C1 C 0.3827(9) 0.7854(2) 0.2797(6) 0.055(2) Uani 1 1 d . A . C2 C 0.2821(9) 0.8069(2) 0.2685(6) 0.052(2) Uani 1 1 d . . . C3 C 0.2227(9) 0.7941(3) 0.3128(6) 0.065(2) Uani 1 1 d . A . H3 H 0.1564 0.8083 0.3070 0.100 Uiso 1 1 calc . . . C4 C 0.2629(12) 0.7611(3) 0.3640(7) 0.076(3) Uani 1 1 d . . . H4 H 0.2234 0.7531 0.3931 0.100 Uiso 1 1 calc . . . C5 C 0.3600(12) 0.7389(3) 0.3742(7) 0.074(3) Uani 1 1 d . A . H5 H 0.3851 0.7163 0.4093 0.100 Uiso 1 1 calc . . . C6 C 0.4194(10) 0.7508(3) 0.3315(6) 0.065(2) Uani 1 1 d . . . C7 C 0.2370(8) 0.8420(2) 0.2161(5) 0.0448(18) Uani 1 1 d . A . H7 H 0.1693 0.8541 0.2129 0.100 Uiso 1 1 calc . . . C8 C 0.2246(6) 0.89641(19) 0.1241(4) 0.0331(15) Uani 1 1 d . A . C9 C 0.2799(7) 0.9038(2) 0.0663(5) 0.0388(16) Uani 1 1 d . . . H9A H 0.2295 0.8897 0.0052 0.100 Uiso 1 1 calc . . . H9B H 0.2724 0.9305 0.0506 0.100 Uiso 1 1 calc . . . C10 C 0.2721(7) 0.9259(2) 0.2045(5) 0.0385(16) Uani 1 1 d . . . H10A H 0.2325 0.9500 0.1735 0.100 Uiso 1 1 calc . . . H10B H 0.2399 0.9188 0.2421 0.100 Uiso 1 1 calc . . . C11 C 0.0726(7) 0.8958(3) 0.0542(5) 0.053(2) Uani 1 1 d . . . C12 C 0.011(2) 0.8680(6) -0.0194(15) 0.061(6) Uani 0.40 1 d P A 1 H12A H -0.0822 0.8706 -0.0568 0.100 Uiso 0.40 1 calc P B 1 H12B H 0.0371 0.8433 0.0102 0.100 Uiso 0.40 1 calc P C 1 H12C H 0.0376 0.8711 -0.0619 0.100 Uiso 0.40 1 calc P D 1 C12' C 0.0135(13) 0.9278(6) -0.0129(12) 0.077(5) Uani 0.60 1 d P A 2 H12D H -0.0805 0.9258 -0.0518 0.100 Uiso 0.60 1 calc P E 2 H12E H 0.0407 0.9277 -0.0551 0.100 Uiso 0.60 1 calc P F 2 H12F H 0.0412 0.9510 0.0241 0.100 Uiso 0.60 1 calc P G 2 C13 C 0.5411(14) 0.6931(3) 0.3680(9) 0.098(4) Uani 1 1 d U . . H13A H 0.6109 0.6831 0.3669 0.100 Uiso 1 1 calc . . . H13B H 0.4630 0.6783 0.3252 0.100 Uiso 1 1 calc . . . H13C H 0.5661 0.6919 0.4337 0.100 Uiso 1 1 calc . . . C14 C 0.8955(8) 0.8215(3) 0.4985(7) 0.054(2) Uani 1 1 d . . . C15 C 0.9611(8) 0.8531(3) 0.5525(6) 0.054(2) Uani 1 1 d . . . C16 C 1.0473(10) 0.8513(3) 0.6558(7) 0.080(3) Uani 1 1 d . . . H16 H 1.0909 0.8729 0.6923 0.100 Uiso 1 1 calc . . . C17 C 1.0666(14) 0.8177(4) 0.7018(9) 0.106(4) Uani 1 1 d U . . H17 H 1.1246 0.8164 0.7699 0.100 Uiso 1 1 calc . . . C18 C 1.0020(14) 0.7859(4) 0.6492(10) 0.109(4) Uani 1 1 d U . . H18 H 1.0169 0.7633 0.6825 0.100 Uiso 1 1 calc . . . C19 C 0.9146(11) 0.7863(3) 0.5478(8) 0.083(3) Uani 1 1 d . . . C20 C 0.9450(7) 0.8900(2) 0.5088(5) 0.0446(18) Uani 1 1 d . . . H20 H 0.9948 0.9098 0.5515 0.100 Uiso 1 1 calc . . . C21 C 0.8599(6) 0.93835(18) 0.3847(5) 0.0312(14) Uani 1 1 d . . . C22 C 0.7850(7) 0.9364(2) 0.2727(5) 0.0362(16) Uani 1 1 d . . . H22A H 0.7489 0.9611 0.2442 0.100 Uiso 1 1 calc . . . H22B H 0.8447 0.9292 0.2572 0.100 Uiso 1 1 calc . . . C23 C 0.7830(6) 0.96161(19) 0.4118(5) 0.0355(15) Uani 1 1 d . . . H23A H 0.8333 0.9623 0.4828 0.100 Uiso 1 1 calc . . . H23B H 0.7755 0.9874 0.3893 0.100 Uiso 1 1 calc . . . C24 C 0.9945(7) 0.9571(2) 0.4315(6) 0.0494(19) Uani 1 1 d . . . H24A H 0.9803 0.9819 0.4017 0.100 Uiso 1 1 calc . . . H24B H 1.0350 0.9611 0.5007 0.100 Uiso 1 1 calc . . . C25 C 1.0904(9) 0.9355(3) 0.4225(7) 0.068(3) Uani 1 1 d . . . H25A H 1.1712 0.9494 0.4544 0.100 Uiso 1 1 calc . . . H25B H 1.0536 0.9322 0.3543 0.100 Uiso 1 1 calc . . . H25C H 1.1074 0.9111 0.4530 0.100 Uiso 1 1 calc . . . C26 C 0.8867(17) 0.7193(4) 0.5333(13) 0.143(5) Uani 1 1 d U . . H26A H 0.8345 0.7001 0.4851 0.100 Uiso 1 1 calc . . . H26B H 0.8752 0.7179 0.5844 0.100 Uiso 1 1 calc . . . H26C H 0.9776 0.7155 0.5608 0.100 Uiso 1 1 calc . . . C27 C 0.5934(7) 0.8620(2) 0.3917(5) 0.0405(17) Uani 1 1 d . . . H27A H 0.6162 0.8360 0.4114 0.100 Uiso 1 1 calc . . . H27B H 0.5104 0.8675 0.3794 0.100 Uiso 1 1 calc . . . H27C H 0.6599 0.8782 0.4431 0.100 Uiso 1 1 calc . . . C28 C 0.6126(10) 0.8096(3) 0.1198(7) 0.072(3) Uani 1 1 d . . . H28A H 0.7026 0.8057 0.1449 0.100 Uiso 1 1 calc . . . H28B H 0.5709 0.8260 0.0636 0.100 Uiso 1 1 calc . . . H28C H 0.5678 0.7856 0.1009 0.100 Uiso 1 1 calc . . . C30 C 0.5966(7) 1.0987(2) 0.4406(5) 0.0372(16) Uani 1 1 d . . . C31 C 0.6372(10) 1.1336(3) 0.4869(7) 0.066(2) Uani 1 1 d . . . H31 H 0.6345 1.1388 0.5396 0.100 Uiso 1 1 calc . . . C32 C 0.6815(14) 1.1606(3) 0.4542(9) 0.091(4) Uani 1 1 d . . . H32 H 0.7088 1.1840 0.4854 0.100 Uiso 1 1 calc . . . C33 C 0.6863(13) 1.1538(3) 0.3776(9) 0.089(3) Uani 1 1 d . . . H33 H 0.7164 1.1724 0.3566 0.100 Uiso 1 1 calc . . . C34 C 0.6472(11) 1.1198(3) 0.3319(7) 0.079(3) Uani 1 1 d . . . H34 H 0.6506 1.1152 0.2794 0.100 Uiso 1 1 calc . . . C35 C 0.6023(8) 1.0918(2) 0.3623(5) 0.0498(19) Uani 1 1 d . . . H35 H 0.5760 1.0685 0.3304 0.100 Uiso 1 1 calc . . . C36 C 0.5545(6) 1.0682(2) 0.4788(4) 0.0338(15) Uani 1 1 d . . . C37 C 0.9020(6) 0.9834(2) 0.7170(4) 0.0344(15) Uani 1 1 d . . . C38 C 0.9693(8) 1.0093(3) 0.7909(6) 0.056(2) Uani 1 1 d . . . H38 H 0.9248 1.0298 0.7926 0.100 Uiso 1 1 calc . . . C39 C 1.1032(9) 1.0054(3) 0.8636(6) 0.071(3) Uani 1 1 d . . . H39 H 1.1477 1.0235 0.9130 0.100 Uiso 1 1 calc . . . C40 C 1.1681(8) 0.9757(4) 0.8627(7) 0.073(3) Uani 1 1 d . . . H40 H 1.2575 0.9730 0.9123 0.100 Uiso 1 1 calc . . . C41 C 1.1043(10) 0.9495(3) 0.7898(8) 0.083(3) Uani 1 1 d . . . H41 H 1.1501 0.9290 0.7894 0.100 Uiso 1 1 calc . . . C42 C 0.9690(8) 0.9534(3) 0.7149(6) 0.064(2) Uani 1 1 d . . . H42 H 0.9253 0.9356 0.6644 0.100 Uiso 1 1 calc . . . C43 C 0.7568(7) 0.98820(19) 0.6377(5) 0.0343(15) Uani 1 1 d . . . C44 C 0.4328(7) 1.03537(18) 0.1229(4) 0.0332(15) Uani 1 1 d . . . C45 C 0.3541(8) 1.0647(2) 0.1138(5) 0.0454(18) Uani 1 1 d . . . H45 H 0.3237 1.0649 0.1522 0.100 Uiso 1 1 calc . . . C46 C 0.3202(9) 1.0938(2) 0.0480(6) 0.063(2) Uani 1 1 d . . . H46 H 0.2653 1.1132 0.0409 0.100 Uiso 1 1 calc . . . C47 C 0.3674(11) 1.0941(3) -0.0067(7) 0.069(3) Uani 1 1 d . . . H47 H 0.3447 1.1137 -0.0507 0.100 Uiso 1 1 calc . . . C48 C 0.4468(11) 1.0659(3) 0.0026(7) 0.071(3) Uani 1 1 d . . . H48 H 0.4802 1.0666 -0.0337 0.100 Uiso 1 1 calc . . . C49 C 0.4781(8) 1.0361(2) 0.0663(5) 0.0469(19) Uani 1 1 d . . . H49 H 0.5303 1.0164 0.0709 0.100 Uiso 1 1 calc . . . C50 C 0.4677(6) 1.00287(18) 0.1910(4) 0.0296(14) Uani 1 1 d . . . O1W O 0.943(3) 0.7647(8) 0.323(2) 0.141(8) Uani 0.40 1 d PU . . O2W O 0.745(6) 0.6491(18) 0.170(5) 0.073(14) Uani 0.10 1 d PU . . 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 Y1 0.0272(3) 0.0354(3) 0.0216(3) 0.0001(3) 0.0159(2) 0.0035(3) Fe1 0.0300(5) 0.0290(5) 0.0240(4) 0.0007(4) 0.0187(4) 0.0019(4) Fe2 0.0539(6) 0.0335(5) 0.0403(5) -0.0061(5) 0.0337(5) -0.0044(5) Fe3 0.0465(6) 0.0347(5) 0.0413(5) 0.0054(5) 0.0324(5) 0.0105(5) Na1 0.103(3) 0.0505(19) 0.094(3) 0.0095(19) 0.063(2) 0.008(2) O1 0.085(4) 0.033(3) 0.074(4) 0.003(3) 0.058(4) 0.000(3) O2 0.036(2) 0.035(2) 0.026(2) -0.0013(19) 0.021(2) -0.002(2) O3 0.026(2) 0.039(2) 0.023(2) -0.0034(19) 0.0163(18) -0.005(2) O4 0.106(5) 0.044(3) 0.093(4) 0.016(3) 0.060(4) 0.000(4) O5 0.062(3) 0.040(3) 0.059(3) 0.017(3) 0.039(3) 0.018(3) O6 0.025(2) 0.038(2) 0.023(2) -0.0010(19) 0.0160(18) 0.000(2) O7 0.033(2) 0.031(2) 0.031(2) 0.0036(19) 0.025(2) 0.003(2) O8 0.102(5) 0.069(4) 0.105(5) 0.049(4) 0.046(4) 0.022(4) O9 0.139(6) 0.140(7) 0.139(6) 0.0002(10) 0.083(4) 0.0002(10) O10 0.041(2) 0.027(2) 0.026(2) 0.0040(18) 0.024(2) 0.006(2) O11 0.067(3) 0.037(3) 0.052(3) -0.007(2) 0.045(3) 0.006(3) O12 0.050(3) 0.034(3) 0.033(2) 0.000(2) 0.023(2) -0.001(2) O13 0.067(3) 0.046(3) 0.042(3) -0.004(2) 0.043(3) -0.003(3) O14 0.035(2) 0.055(3) 0.024(2) -0.002(2) 0.015(2) 0.012(2) O15 0.027(2) 0.061(3) 0.031(2) -0.005(2) 0.017(2) 0.008(2) O16 0.048(3) 0.034(2) 0.031(2) 0.002(2) 0.028(2) 0.007(2) O17 0.058(3) 0.040(3) 0.027(2) 0.003(2) 0.031(2) 0.009(2) N1 0.071(5) 0.072(5) 0.071(5) -0.039(4) 0.043(4) -0.023(5) N2 0.050(10) 0.045(10) 0.046(9) -0.016(7) 0.023(7) 0.011(8) N3 0.097(13) 0.107(14) 0.105(13) -0.017(9) 0.061(10) 0.003(9) N2' 0.084(9) 0.092(10) 0.081(9) -0.016(7) 0.058(7) -0.004(8) N3' 0.142(12) 0.146(13) 0.143(12) -0.020(9) 0.093(9) -0.016(9) N2" 0.054(11) 0.037(11) 0.054(11) -0.005(8) 0.029(9) 0.003(8) N3" 0.066(12) 0.060(13) 0.056(12) 0.000(9) 0.034(9) 0.009(9) N4 0.074(4) 0.075(4) 0.087(5) 0.014(4) 0.068(4) 0.024(4) N5 0.080(4) 0.097(5) 0.099(5) 0.032(4) 0.072(4) 0.042(4) N6 0.108(6) 0.145(8) 0.122(7) 0.058(6) 0.100(6) 0.048(6) N7 0.039(3) 0.042(3) 0.033(3) -0.011(3) 0.023(3) -0.014(3) N8 0.035(3) 0.041(3) 0.034(3) 0.011(3) 0.025(3) 0.012(3) C1 0.075(6) 0.039(4) 0.051(5) -0.004(4) 0.037(5) -0.022(5) C2 0.064(5) 0.049(5) 0.049(4) -0.009(4) 0.036(4) -0.023(5) C3 0.076(6) 0.070(6) 0.056(5) -0.008(5) 0.043(5) -0.036(5) C4 0.089(8) 0.077(7) 0.067(6) 0.003(5) 0.050(6) -0.039(7) C5 0.086(7) 0.061(6) 0.061(6) 0.019(5) 0.036(6) -0.019(6) C6 0.079(7) 0.044(5) 0.055(5) -0.004(4) 0.031(5) -0.020(5) C7 0.051(4) 0.047(4) 0.045(4) -0.014(4) 0.033(4) -0.018(4) C8 0.027(3) 0.041(4) 0.028(3) -0.007(3) 0.015(3) -0.004(3) C9 0.036(4) 0.057(4) 0.027(3) 0.001(3) 0.020(3) 0.000(4) C10 0.037(4) 0.044(4) 0.039(4) -0.001(3) 0.025(3) 0.003(4) C11 0.035(4) 0.076(6) 0.035(4) -0.009(4) 0.014(3) -0.009(4) C12 0.050(12) 0.062(14) 0.058(12) -0.025(11) 0.025(10) -0.013(12) C12' 0.029(7) 0.115(14) 0.071(10) 0.023(10) 0.022(7) 0.008(9) C13 0.126(8) 0.073(6) 0.092(6) 0.014(5) 0.061(6) -0.004(6) C14 0.052(5) 0.053(5) 0.062(5) 0.032(5) 0.037(5) 0.026(5) C15 0.049(5) 0.062(6) 0.046(4) 0.020(4) 0.027(4) 0.019(5) C16 0.082(7) 0.090(7) 0.053(5) 0.021(5) 0.033(5) 0.012(6) C17 0.111(8) 0.113(8) 0.069(6) 0.032(6) 0.041(5) 0.004(6) C18 0.112(8) 0.091(7) 0.094(7) 0.048(6) 0.045(6) 0.011(6) C19 0.077(7) 0.066(7) 0.082(7) 0.045(6) 0.035(6) 0.029(6) C20 0.042(4) 0.050(5) 0.047(4) 0.008(4) 0.029(4) 0.015(4) C21 0.027(3) 0.035(4) 0.040(4) -0.001(3) 0.024(3) 0.002(3) C22 0.041(4) 0.043(4) 0.038(4) 0.009(3) 0.031(3) 0.005(4) C23 0.032(4) 0.035(4) 0.038(4) -0.002(3) 0.020(3) -0.003(3) C24 0.031(4) 0.057(5) 0.059(5) 0.002(4) 0.026(4) 0.001(4) C25 0.050(5) 0.074(6) 0.094(7) 0.014(5) 0.050(5) 0.015(5) C26 0.140(9) 0.096(8) 0.142(9) 0.038(7) 0.057(7) 0.005(7) C27 0.060(5) 0.040(4) 0.037(4) 0.009(3) 0.038(4) 0.007(4) C28 0.090(7) 0.074(6) 0.076(6) -0.022(5) 0.062(6) -0.007(6) C30 0.040(4) 0.038(4) 0.035(3) 0.002(3) 0.023(3) 0.003(3) C31 0.097(7) 0.058(5) 0.069(6) -0.016(5) 0.064(6) -0.023(5) C32 0.158(11) 0.049(5) 0.104(8) -0.017(5) 0.098(9) -0.040(7) C33 0.141(10) 0.074(7) 0.097(8) -0.004(6) 0.094(8) -0.040(7) C34 0.112(8) 0.092(7) 0.070(6) -0.001(6) 0.075(6) -0.019(7) C35 0.067(5) 0.056(5) 0.042(4) 0.002(4) 0.042(4) -0.005(4) C36 0.025(3) 0.041(4) 0.020(3) 0.008(3) 0.005(3) 0.002(3) C37 0.030(3) 0.049(4) 0.025(3) 0.002(3) 0.016(3) 0.004(3) C38 0.039(4) 0.071(6) 0.046(4) -0.009(4) 0.018(4) 0.007(4) C39 0.040(5) 0.093(7) 0.057(5) -0.021(5) 0.016(4) -0.005(5) C40 0.032(4) 0.119(9) 0.050(5) 0.010(6) 0.014(4) 0.009(6) C41 0.053(6) 0.097(8) 0.076(7) 0.003(6) 0.025(5) 0.039(6) C42 0.044(5) 0.087(6) 0.043(4) -0.003(5) 0.016(4) 0.027(5) C43 0.037(4) 0.040(4) 0.032(3) 0.006(3) 0.023(3) 0.007(3) C44 0.042(4) 0.028(3) 0.025(3) 0.000(3) 0.017(3) 0.002(3) C45 0.054(5) 0.040(4) 0.043(4) 0.006(4) 0.030(4) 0.010(4) C46 0.069(6) 0.045(5) 0.061(5) 0.023(4) 0.032(5) 0.025(5) C47 0.096(7) 0.050(5) 0.060(5) 0.019(5) 0.046(6) 0.002(6) C48 0.098(7) 0.072(6) 0.060(5) 0.024(5) 0.056(6) 0.011(6) C49 0.063(5) 0.052(5) 0.033(4) 0.006(3) 0.033(4) 0.002(4) C50 0.028(3) 0.031(3) 0.028(3) 0.005(3) 0.016(3) 0.004(3) O1W 0.141(8) 0.141(8) 0.141(8) -0.0002(10) 0.084(5) 0.0003(10) O2W 0.073(14) 0.073(14) 0.073(14) -0.0001(10) 0.044(8) 0.0001(10) _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 Y1 O12 2.273(5) . ? Y1 O15 2.283(4) . ? Y1 O13 2.308(5) . ? Y1 O6 2.313(4) . ? Y1 O3 2.326(4) . ? Y1 O14 2.331(4) . ? Y1 O17 2.356(4) . ? Y1 C36 3.029(6) 3_676 ? Y1 Fe1 3.3575(9) . ? Y1 Y1 4.0356(11) 3_676 ? Fe1 O3 1.950(4) . ? Fe1 O6 1.976(4) . ? Fe1 O7 2.002(4) . ? Fe1 O2 2.002(4) . ? Fe1 O16 2.017(4) . ? Fe1 O10 2.093(4) . ? Fe2 O1 1.924(5) . ? Fe2 O2 2.007(4) . ? Fe2 N1 2.011(7) . ? Fe2 O11 2.013(5) . ? Fe2 N7 2.120(5) . ? Fe2 O10 2.150(4) . ? Fe2 Na1 3.487(4) . ? Fe3 O5 1.934(5) . ? Fe3 N4 1.988(6) . ? Fe3 O7 2.013(4) . ? Fe3 O11 2.016(5) . ? Fe3 N8 2.117(6) . ? Fe3 O10 2.122(4) . ? Fe3 Na1 3.435(4) . ? Na1 O5 2.382(7) . ? Na1 O9 2.39(2) . ? Na1 O1 2.419(7) . ? Na1 O4 2.454(8) . ? Na1 O8 2.455(9) . ? Na1 O11 2.696(6) . ? O1 C1 1.344(9) . ? O2 C9 1.419(8) . ? O3 C10 1.396(8) . ? O4 C6 1.376(12) . ? O4 C13 1.413(12) . ? O5 C14 1.340(10) . ? O6 C23 1.408(7) . ? O7 C22 1.422(8) . ? O8 C19 1.380(14) . ? O8 C26 1.421(15) . ? O10 C27 1.437(7) . ? O11 C28 1.396(9) . ? O12 C36 1.244(8) . ? O13 C36 1.246(8) 3_676 ? O14 C43 1.254(7) . ? O15 C43 1.258(7) 3_676 ? O16 C50 1.265(7) . ? O17 C50 1.251(7) . ? N1 N2 1.1608(10) . ? N1 N2' 1.24(2) . ? N1 N2" 1.48(4) . ? N2 N3 1.1408(10) . ? N2' N3' 1.19(3) . ? N2" N3" 1.22(4) . ? N4 N5 1.134(9) . ? N5 N6 1.138(11) . ? N7 C7 1.277(8) . ? N7 C8 1.515(9) . ? N8 C20 1.272(8) . ? N8 C21 1.509(8) . ? C1 C2 1.395(12) . ? C1 C6 1.411(12) . ? C2 C3 1.414(11) . ? C2 C7 1.427(11) . ? C3 C4 1.359(14) . ? C3 H3 0.9300 . ? C4 C5 1.377(15) . ? C4 H4 0.9300 . ? C5 C6 1.381(14) . ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.524(9) . ? C8 C9 1.524(8) . ? C8 C11 1.548(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.40(2) . ? C11 C12' 1.454(18) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.365(12) . ? C14 C19 1.435(12) . ? C15 C16 1.409(12) . ? C15 C20 1.450(11) . ? C16 C17 1.358(16) . ? C16 H16 0.9300 . ? C17 C18 1.360(18) . ? C17 H17 0.9300 . ? C18 C19 1.384(17) . ? C18 H18 0.9300 . ? C20 H20 0.9300 . ? C21 C23 1.535(9) . ? C21 C22 1.537(9) . ? C21 C24 1.538(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.515(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C30 C31 1.384(11) . ? C30 C35 1.391(9) . ? C30 C36 1.505(9) . ? C31 C32 1.377(12) . ? C31 H31 0.9300 . ? C32 C33 1.354(13) . ? C32 H32 0.9300 . ? C33 C34 1.349(14) . ? C33 H33 0.9300 . ? C34 C35 1.381(11) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 O13 1.246(8) 3_676 ? C36 Y1 3.029(6) 3_676 ? C37 C38 1.363(10) . ? C37 C42 1.369(10) . ? C37 C43 1.509(9) . ? C38 C39 1.387(12) . ? C38 H38 0.9300 . ? C39 C40 1.336(14) . ? C39 H39 0.9300 . ? C40 C41 1.359(14) . ? C40 H40 0.9300 . ? C41 C42 1.406(12) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 O15 1.258(7) 3_676 ? C44 C49 1.377(9) . ? C44 C45 1.381(9) . ? C44 C50 1.494(9) . ? C45 C46 1.382(10) . ? C45 H45 0.9300 . ? C46 C47 1.367(13) . ? C46 H46 0.9300 . ? C47 C48 1.354(13) . ? C47 H47 0.9300 . ? C48 C49 1.383(11) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Y1 O15 79.64(17) . . ? O12 Y1 O13 127.55(15) . . ? O15 Y1 O13 82.29(18) . . ? O12 Y1 O6 117.51(16) . . ? O15 Y1 O6 149.65(14) . . ? O13 Y1 O6 102.38(15) . . ? O12 Y1 O3 148.07(15) . . ? O15 Y1 O3 84.23(15) . . ? O13 Y1 O3 76.52(15) . . ? O6 Y1 O3 68.18(14) . . ? O12 Y1 O14 76.98(16) . . ? O15 Y1 O14 132.11(15) . . ? O13 Y1 O14 79.88(18) . . ? O6 Y1 O14 77.92(14) . . ? O3 Y1 O14 132.77(16) . . ? O12 Y1 O17 76.65(15) . . ? O15 Y1 O17 83.35(16) . . ? O13 Y1 O17 148.49(17) . . ? O6 Y1 O17 77.33(14) . . ? O3 Y1 O17 74.24(15) . . ? O14 Y1 O17 129.52(17) . . ? O12 Y1 C36 105.58(17) . 3_676 ? O15 Y1 C36 72.63(17) . 3_676 ? O13 Y1 C36 22.16(17) . 3_676 ? O6 Y1 C36 120.80(17) . 3_676 ? O3 Y1 C36 95.48(16) . 3_676 ? O14 Y1 C36 74.32(16) . 3_676 ? O17 Y1 C36 154.82(17) . 3_676 ? O12 Y1 Fe1 136.42(11) . . ? O15 Y1 Fe1 115.14(11) . . ? O13 Y1 Fe1 95.76(11) . . ? O6 Y1 Fe1 35.02(10) . . ? O3 Y1 Fe1 34.45(9) . . ? O14 Y1 Fe1 110.63(11) . . ? O17 Y1 Fe1 65.64(10) . . ? C36 Y1 Fe1 117.88(14) 3_676 . ? O12 Y1 Y1 48.02(11) . 3_676 ? O15 Y1 Y1 66.28(10) . 3_676 ? O13 Y1 Y1 79.64(11) . 3_676 ? O6 Y1 Y1 143.99(10) . 3_676 ? O3 Y1 Y1 144.18(10) . 3_676 ? O14 Y1 Y1 66.94(10) . 3_676 ? O17 Y1 Y1 119.30(10) . 3_676 ? C36 Y1 Y1 57.57(14) 3_676 3_676 ? Fe1 Y1 Y1 175.05(3) . 3_676 ? O3 Fe1 O6 82.97(16) . . ? O3 Fe1 O7 171.81(17) . . ? O6 Fe1 O7 94.11(17) . . ? O3 Fe1 O2 93.54(16) . . ? O6 Fe1 O2 172.84(16) . . ? O7 Fe1 O2 88.49(17) . . ? O3 Fe1 O16 94.51(17) . . ? O6 Fe1 O16 92.79(17) . . ? O7 Fe1 O16 93.28(17) . . ? O2 Fe1 O16 93.72(17) . . ? O3 Fe1 O10 93.09(16) . . ? O6 Fe1 O10 93.65(16) . . ? O7 Fe1 O10 79.42(16) . . ? O2 Fe1 O10 80.25(16) . . ? O16 Fe1 O10 170.59(15) . . ? O3 Fe1 Y1 42.44(12) . . ? O6 Fe1 Y1 42.23(11) . . ? O7 Fe1 Y1 136.01(12) . . ? O2 Fe1 Y1 135.50(12) . . ? O16 Fe1 Y1 85.56(11) . . ? O10 Fe1 Y1 103.82(10) . . ? O1 Fe2 O2 162.01(19) . . ? O1 Fe2 N1 97.7(3) . . ? O2 Fe2 N1 94.5(3) . . ? O1 Fe2 O11 91.8(2) . . ? O2 Fe2 O11 99.91(18) . . ? N1 Fe2 O11 96.8(3) . . ? O1 Fe2 N7 87.6(2) . . ? O2 Fe2 N7 78.39(19) . . ? N1 Fe2 N7 94.0(3) . . ? O11 Fe2 N7 169.3(2) . . ? O1 Fe2 O10 91.1(2) . . ? O2 Fe2 O10 78.77(16) . . ? N1 Fe2 O10 168.7(3) . . ? O11 Fe2 O10 75.72(17) . . ? N7 Fe2 O10 93.56(17) . . ? O1 Fe2 Na1 41.77(19) . . ? O2 Fe2 Na1 145.31(14) . . ? N1 Fe2 Na1 105.4(3) . . ? O11 Fe2 Na1 50.44(15) . . ? N7 Fe2 Na1 126.90(17) . . ? O10 Fe2 Na1 76.52(13) . . ? O5 Fe3 N4 95.2(3) . . ? O5 Fe3 O7 161.06(19) . . ? N4 Fe3 O7 98.6(2) . . ? O5 Fe3 O11 93.6(2) . . ? N4 Fe3 O11 95.3(3) . . ? O7 Fe3 O11 97.91(19) . . ? O5 Fe3 N8 88.0(2) . . ? N4 Fe3 N8 94.5(3) . . ? O7 Fe3 N8 78.17(19) . . ? O11 Fe3 N8 169.97(19) . . ? O5 Fe3 O10 89.78(19) . . ? N4 Fe3 O10 170.5(3) . . ? O7 Fe3 O10 78.49(15) . . ? O11 Fe3 O10 76.30(17) . . ? N8 Fe3 O10 93.81(17) . . ? O5 Fe3 Na1 42.07(19) . . ? N4 Fe3 Na1 100.3(2) . . ? O7 Fe3 Na1 145.31(15) . . ? O11 Fe3 Na1 51.66(16) . . ? N8 Fe3 Na1 128.57(16) . . ? O10 Fe3 Na1 78.06(13) . . ? O5 Na1 O9 123.9(6) . . ? O5 Na1 O1 103.7(2) . . ? O9 Na1 O1 124.6(6) . . ? O5 Na1 O4 135.3(3) . . ? O9 Na1 O4 93.7(6) . . ? O1 Na1 O4 64.4(2) . . ? O5 Na1 O8 65.1(3) . . ? O9 Na1 O8 96.4(6) . . ? O1 Na1 O8 131.0(3) . . ? O4 Na1 O8 89.8(3) . . ? O5 Na1 O11 68.78(19) . . ? O9 Na1 O11 103.5(5) . . ? O1 Na1 O11 66.85(18) . . ? O4 Na1 O11 129.6(3) . . ? O8 Na1 O11 133.4(3) . . ? O5 Na1 Fe3 32.96(13) . . ? O9 Na1 Fe3 120.8(5) . . ? O1 Na1 Fe3 83.98(15) . . ? O4 Na1 Fe3 143.2(2) . . ? O8 Na1 Fe3 98.0(2) . . ? O11 Na1 Fe3 35.89(12) . . ? O5 Na1 Fe2 83.89(15) . . ? O9 Na1 Fe2 122.3(5) . . ? O1 Na1 Fe2 31.99(13) . . ? O4 Na1 Fe2 96.2(2) . . ? O8 Na1 Fe2 140.2(3) . . ? O11 Na1 Fe2 35.13(11) . . ? Fe3 Na1 Fe2 55.97(6) . . ? C1 O1 Fe2 132.4(5) . . ? C1 O1 Na1 118.6(5) . . ? Fe2 O1 Na1 106.2(3) . . ? C9 O2 Fe1 115.4(4) . . ? C9 O2 Fe2 111.0(4) . . ? Fe1 O2 Fe2 104.23(18) . . ? C10 O3 Fe1 127.4(3) . . ? C10 O3 Y1 124.7(4) . . ? Fe1 O3 Y1 103.11(17) . . ? C6 O4 C13 119.0(8) . . ? C6 O4 Na1 116.7(5) . . ? C13 O4 Na1 123.4(7) . . ? C14 O5 Fe3 131.0(5) . . ? C14 O5 Na1 122.7(5) . . ? Fe3 O5 Na1 105.0(3) . . ? C23 O6 Fe1 125.5(3) . . ? C23 O6 Y1 125.8(3) . . ? Fe1 O6 Y1 102.75(16) . . ? C22 O7 Fe1 115.2(3) . . ? C22 O7 Fe3 111.2(4) . . ? Fe1 O7 Fe3 104.13(17) . . ? C19 O8 C26 116.3(10) . . ? C19 O8 Na1 117.7(5) . . ? C26 O8 Na1 125.9(9) . . ? C27 O10 Fe1 118.3(4) . . ? C27 O10 Fe3 120.6(4) . . ? Fe1 O10 Fe3 97.39(16) . . ? C27 O10 Fe2 120.0(4) . . ? Fe1 O10 Fe2 96.43(16) . . ? Fe3 O10 Fe2 99.00(15) . . ? C28 O11 Fe2 122.7(5) . . ? C28 O11 Fe3 125.1(5) . . ? Fe2 O11 Fe3 107.47(19) . . ? C28 O11 Na1 103.8(5) . . ? Fe2 O11 Na1 94.42(19) . . ? Fe3 O11 Na1 92.5(2) . . ? C36 O12 Y1 175.3(5) . . ? C36 O13 Y1 113.5(4) 3_676 . ? C43 O14 Y1 136.7(4) . . ? C43 O15 Y1 140.3(4) 3_676 . ? C50 O16 Fe1 124.8(4) . . ? C50 O17 Y1 138.0(4) . . ? N2 N1 N2' 38.5(11) . . ? N2 N1 N2" 97.3(19) . . ? N2' N1 N2" 130.8(17) . . ? N2 N1 Fe2 130.4(13) . . ? N2' N1 Fe2 113.8(10) . . ? N2" N1 Fe2 113.1(13) . . ? N3 N2 N1 174.8(18) . . ? N3' N2' N1 171(3) . . ? N3" N2" N1 178(3) . . ? N5 N4 Fe3 142.7(7) . . ? N4 N5 N6 178.5(11) . . ? C7 N7 C8 119.8(6) . . ? C7 N7 Fe2 126.1(5) . . ? C8 N7 Fe2 113.9(4) . . ? C20 N8 C21 119.6(6) . . ? C20 N8 Fe3 126.0(5) . . ? C21 N8 Fe3 114.4(4) . . ? O1 C1 C2 123.8(7) . . ? O1 C1 C6 116.8(9) . . ? C2 C1 C6 119.5(8) . . ? C1 C2 C3 118.9(8) . . ? C1 C2 C7 123.5(7) . . ? C3 C2 C7 117.6(8) . . ? C4 C3 C2 119.7(10) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 122.4(8) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C4 C5 C6 118.9(9) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? O4 C6 C5 124.5(9) . . ? O4 C6 C1 115.0(8) . . ? C5 C6 C1 120.5(10) . . ? N7 C7 C2 126.6(7) . . ? N7 C7 H7 116.7 . . ? C2 C7 H7 116.7 . . ? N7 C8 C10 107.9(5) . . ? N7 C8 C9 105.2(5) . . ? C10 C8 C9 111.6(5) . . ? N7 C8 C11 111.6(6) . . ? C10 C8 C11 110.1(5) . . ? C9 C8 C11 110.3(5) . . ? O2 C9 C8 110.4(5) . . ? O2 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? O2 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O3 C10 C8 116.1(5) . . ? O3 C10 H10A 108.3 . . ? C8 C10 H10A 108.3 . . ? O3 C10 H10B 108.3 . . ? C8 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C12' 95.3(13) . . ? C12 C11 C8 117.9(11) . . ? C12' C11 C8 114.5(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12' H12D 109.5 . . ? C11 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 125.6(7) . . ? O5 C14 C19 114.8(9) . . ? C15 C14 C19 119.5(9) . . ? C14 C15 C16 120.5(8) . . ? C14 C15 C20 123.1(7) . . ? C16 C15 C20 116.4(9) . . ? C17 C16 C15 119.7(11) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.6(10) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 122.1(10) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? O8 C19 C18 126.4(10) . . ? O8 C19 C14 116.0(9) . . ? C18 C19 C14 117.6(12) . . ? N8 C20 C15 126.4(7) . . ? N8 C20 H20 116.8 . . ? C15 C20 H20 116.8 . . ? N8 C21 C23 108.7(5) . . ? N8 C21 C22 105.6(5) . . ? C23 C21 C22 110.8(5) . . ? N8 C21 C24 113.3(5) . . ? C23 C21 C24 108.7(5) . . ? C22 C21 C24 109.7(5) . . ? O7 C22 C21 109.8(5) . . ? O7 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? O7 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? O6 C23 C21 115.1(5) . . ? O6 C23 H23A 108.5 . . ? C21 C23 H23A 108.5 . . ? O6 C23 H23B 108.5 . . ? C21 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C21 116.1(7) . . ? C25 C24 H24A 108.3 . . ? C21 C24 H24A 108.3 . . ? C25 C24 H24B 108.3 . . ? C21 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O8 C26 H26A 109.5 . . ? O8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O10 C27 H27A 109.5 . . ? O10 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O10 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O11 C28 H28A 109.5 . . ? O11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C30 C35 118.8(7) . . ? C31 C30 C36 119.9(6) . . ? C35 C30 C36 121.1(6) . . ? C32 C31 C30 119.4(7) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C33 C32 C31 121.4(9) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C34 C33 C32 119.8(8) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.9(8) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C30 119.7(8) . . ? C34 C35 H35 120.2 . . ? C30 C35 H35 120.2 . . ? O12 C36 O13 122.4(6) . 3_676 ? O12 C36 C30 119.2(6) . . ? O13 C36 C30 118.3(6) 3_676 . ? O12 C36 Y1 78.2(4) . 3_676 ? O13 C36 Y1 44.3(3) 3_676 3_676 ? C30 C36 Y1 162.2(5) . 3_676 ? C38 C37 C42 118.8(7) . . ? C38 C37 C43 120.5(6) . . ? C42 C37 C43 120.6(6) . . ? C37 C38 C39 121.1(8) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 120.1(8) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.4(8) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C42 120.1(8) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C37 C42 C41 119.5(8) . . ? C37 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? O14 C43 O15 126.2(6) . 3_676 ? O14 C43 C37 117.9(5) . . ? O15 C43 C37 115.9(6) 3_676 . ? C49 C44 C45 118.5(6) . . ? C49 C44 C50 119.7(6) . . ? C45 C44 C50 121.7(6) . . ? C44 C45 C46 120.4(7) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 119.9(8) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 120.6(7) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 119.8(8) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? C44 C49 C48 120.8(7) . . ? C44 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? O17 C50 O16 125.6(5) . . ? O17 C50 C44 118.1(6) . . ? O16 C50 C44 116.3(5) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.841 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.084 _iucr_refine_instructions_details ; TITL sad in P2(1)/c CELL 0.71073 12.6479 35.2806 16.9188 90.000 126.420 90.000 ZERR 2.00 0.0005 0.0013 0.0009 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Na Fe Y UNIT 196 220 32 68 4 12 4 L.S. 20 omit 0 50 shel 0.5 2.5 BOND $h acta htab dfix 1.16 0.001 n1 n2 dfix 1.14 0.001 n2 n3 dfix 2.30 0.001 n1 n3 isor 0.01 0.01 n2 n2' n3 n3' n2" N3" isor 0.01 0.01 na1 o4 o8 c13 c17 c18 c26 ISOR 0.001 0.001 O9 o1w o2w simu 0.01 0.01 n4 n5 n6 FMAP 2 PLAN 20 TEMP 20 WGHT 0.0000 24.4044 FVAR 0.09318 Y1 7 0.511997 0.973704 0.399661 11.00000 0.02724 0.03543 = 0.02163 0.00007 0.01589 0.00355 FE1 6 0.537257 0.922992 0.243635 11.00000 0.03002 0.02903 = 0.02397 0.00068 0.01873 0.00188 FE2 6 0.436927 0.839225 0.170503 11.00000 0.05389 0.03351 = 0.04027 -0.00610 0.03373 -0.00445 FE3 6 0.748251 0.859234 0.302053 11.00000 0.04649 0.03467 = 0.04129 0.00537 0.03244 0.01053 NA1 5 0.663530 0.768286 0.315962 11.00000 0.10273 0.05055 = 0.09447 0.00952 0.06300 0.00834 O1 4 0.448901 0.795621 0.243730 11.00000 0.08496 0.03335 = 0.07397 0.00261 0.05845 -0.00040 O2 4 0.413709 0.892654 0.121911 11.00000 0.03598 0.03467 = 0.02561 -0.00131 0.02113 -0.00246 O3 4 0.407905 0.930914 0.269645 11.00000 0.02603 0.03902 = 0.02278 -0.00340 0.01632 -0.00472 O4 4 0.516670 0.731141 0.335814 11.00000 0.10560 0.04380 = 0.09260 0.01638 0.05967 -0.00043 O5 4 0.810162 0.820096 0.400419 11.00000 0.06154 0.04044 = 0.05867 0.01749 0.03859 0.01803 O6 4 0.656195 0.947979 0.372579 11.00000 0.02478 0.03806 = 0.02305 -0.00104 0.01604 -0.00047 O7 4 0.681590 0.909419 0.232488 11.00000 0.03337 0.03072 = 0.03138 0.00361 0.02475 0.00252 O8 4 0.846303 0.755600 0.488032 11.00000 0.10216 0.06889 = 0.10452 0.04871 0.04647 0.02223 O9 4 0.706119 0.716518 0.247464 10.50000 0.13940 0.13953 = 0.13940 0.00023 0.08298 0.00016 O10 4 0.583848 0.868392 0.303796 11.00000 0.04074 0.02652 = 0.02590 0.00398 0.02403 0.00604 O11 4 0.607327 0.826072 0.192339 11.00000 0.06707 0.03651 = 0.05215 -0.00685 0.04492 0.00611 O12 4 0.544371 1.035011 0.450442 11.00000 0.04997 0.03369 = 0.03325 -0.00049 0.02298 -0.00104 O13 4 0.467502 0.922676 0.461011 11.00000 0.06746 0.04634 = 0.04172 -0.00362 0.04332 -0.00348 O14 4 0.707112 0.970945 0.558159 11.00000 0.03515 0.05476 = 0.02412 -0.00196 0.01483 0.01184 O15 4 0.303030 0.990391 0.341532 11.00000 0.02689 0.06054 = 0.03052 -0.00459 0.01696 0.00832 O16 4 0.496661 0.972085 0.169626 11.00000 0.04841 0.03384 = 0.03076 0.00186 0.02805 0.00725 O17 4 0.462963 1.007898 0.261959 11.00000 0.05832 0.04018 = 0.02692 0.00293 0.03053 0.00914 N1 3 0.317406 0.816608 0.035395 11.00000 0.07077 0.07190 = 0.07079 -0.03880 0.04308 -0.02264 PART 1 N2 3 0.207094 0.808421 -0.010074 10.30000 0.04991 0.04510 = 0.04636 -0.01624 0.02318 0.01092 N3 3 0.101681 0.797656 -0.052248 10.30000 0.09701 0.10712 = 0.10465 -0.01673 0.06050 0.00296 PART 2 N2' 3 0.243109 0.791595 0.028649 10.50000 0.08422 0.09204 = 0.08137 -0.01613 0.05799 -0.00402 N3' 3 0.158475 0.770537 0.012605 10.50000 0.14221 0.14629 = 0.14267 -0.01988 0.09330 -0.01639 PART 3 N2" 3 0.309814 0.839473 -0.041161 10.20000 0.05353 0.03726 = 0.05398 -0.00472 0.02925 0.00258 N3" 3 0.300915 0.857826 -0.106007 10.20000 0.06600 0.06044 = 0.05564 -0.00028 0.03426 0.00899 PART 0 N4 3 0.880305 0.848888 0.276789 11.00000 0.07401 0.07527 = 0.08693 0.01440 0.06821 0.02385 N5 3 0.911484 0.857665 0.228965 11.00000 0.08048 0.09657 = 0.09927 0.03190 0.07179 0.04212 N6 1 0.943300 0.865682 0.180810 11.00000 0.10849 0.14540 = 0.12197 0.05848 0.09957 0.04806 N7 3 0.280207 0.858342 0.173192 11.00000 0.03850 0.04223 = 0.03256 -0.01136 0.02310 -0.01395 N8 3 0.869422 0.897954 0.417710 11.00000 0.03528 0.04130 = 0.03436 0.01122 0.02515 0.01248 C1 1 0.382713 0.785404 0.279675 11.00000 0.07480 0.03931 = 0.05088 -0.00397 0.03743 -0.02186 C2 1 0.282126 0.806929 0.268512 11.00000 0.06402 0.04945 = 0.04873 -0.00943 0.03605 -0.02257 C3 1 0.222698 0.794137 0.312820 11.00000 0.07597 0.07045 = 0.05641 -0.00822 0.04287 -0.03641 AFIX 41 H3 2 0.156358 0.808299 0.306974 11.00000 10.10000 AFIX 0 C4 1 0.262932 0.761067 0.363973 11.00000 0.08870 0.07678 = 0.06710 0.00328 0.04956 -0.03947 AFIX 41 H4 2 0.223433 0.753103 0.393145 11.00000 10.10000 AFIX 0 C5 1 0.360006 0.738908 0.374226 11.00000 0.08632 0.06147 = 0.06057 0.01921 0.03595 -0.01909 AFIX 41 H5 2 0.385130 0.716307 0.409292 11.00000 10.10000 AFIX 0 C6 1 0.419427 0.750821 0.331542 11.00000 0.07917 0.04420 = 0.05521 -0.00381 0.03096 -0.01984 C7 1 0.237015 0.841953 0.216125 11.00000 0.05065 0.04750 = 0.04488 -0.01368 0.03308 -0.01765 AFIX 41 H7 2 0.169271 0.854075 0.212926 11.00000 10.10000 AFIX 0 C8 1 0.224617 0.896412 0.124090 11.00000 0.02715 0.04130 = 0.02809 -0.00701 0.01490 -0.00412 C9 1 0.279871 0.903791 0.066304 11.00000 0.03570 0.05705 = 0.02663 0.00123 0.02011 -0.00019 AFIX 21 H9A 2 0.229463 0.889692 0.005161 11.00000 10.10000 H9B 2 0.272378 0.930545 0.050560 11.00000 10.10000 AFIX 0 C10 1 0.272079 0.925873 0.204503 11.00000 0.03664 0.04375 = 0.03914 -0.00131 0.02470 0.00279 AFIX 21 H10A 2 0.232458 0.950036 0.173497 11.00000 10.10000 H10B 2 0.239945 0.918770 0.242144 11.00000 10.10000 AFIX 0 C11 1 0.072592 0.895783 0.054175 11.00000 0.03517 0.07590 = 0.03463 -0.00891 0.01390 -0.00857 PART 1 C12 1 0.011503 0.868031 -0.019387 10.40000 0.04998 0.06228 = 0.05836 -0.02466 0.02500 -0.01267 AFIX 31 H12A 2 -0.082143 0.870627 -0.056844 10.40000 10.10000 H12B 2 0.037156 0.843345 0.010207 10.40000 10.10000 H12C 2 0.037637 0.871105 -0.061930 10.40000 10.10000 AFIX 0 PART 2 C12' 1 0.013456 0.927802 -0.012870 10.60000 0.02934 0.11517 = 0.07126 0.02258 0.02217 0.00851 AFIX 31 H12D 2 -0.080513 0.925838 -0.051837 10.60000 10.10000 H12E 2 0.040657 0.927738 -0.055128 10.60000 10.10000 H12F 2 0.041185 0.950966 0.024097 10.60000 10.10000 AFIX 0 PART 0 C13 1 0.541122 0.693077 0.367974 11.00000 0.12553 0.07273 = 0.09162 0.01439 0.06148 -0.00396 AFIX 31 H13A 2 0.610876 0.683136 0.366853 11.00000 10.10000 H13B 2 0.463030 0.678318 0.325210 11.00000 10.10000 H13C 2 0.566077 0.691907 0.433715 11.00000 10.10000 AFIX 0 C14 1 0.895496 0.821544 0.498535 11.00000 0.05189 0.05314 = 0.06187 0.03205 0.03704 0.02628 C15 1 0.961073 0.853118 0.552506 11.00000 0.04945 0.06198 = 0.04636 0.01969 0.02659 0.01950 C16 1 1.047341 0.851260 0.655779 11.00000 0.08213 0.09033 = 0.05314 0.02112 0.03277 0.01229 AFIX 41 H16 2 1.090869 0.872925 0.692268 11.00000 10.10000 AFIX 0 C17 1 1.066639 0.817669 0.701806 11.00000 0.11128 0.11272 = 0.06936 0.03241 0.04083 0.00423 AFIX 41 H17 2 1.124632 0.816355 0.769936 11.00000 10.10000 AFIX 0 C18 1 1.001986 0.785941 0.649236 11.00000 0.11213 0.09097 = 0.09422 0.04816 0.04499 0.01116 AFIX 41 H18 2 1.016925 0.763292 0.682514 11.00000 10.10000 AFIX 0 C19 1 0.914645 0.786289 0.547764 11.00000 0.07669 0.06591 = 0.08206 0.04462 0.03464 0.02905 C20 1 0.944986 0.889992 0.508807 11.00000 0.04218 0.05044 = 0.04663 0.00803 0.02934 0.01473 AFIX 41 H20 2 0.994765 0.909758 0.551540 11.00000 10.10000 AFIX 0 C21 1 0.859909 0.938353 0.384746 11.00000 0.02725 0.03453 = 0.03982 -0.00066 0.02426 0.00236 C22 1 0.784960 0.936395 0.272746 11.00000 0.04130 0.04283 = 0.03801 0.00879 0.03098 0.00532 AFIX 21 H22A 2 0.748933 0.961126 0.244201 11.00000 10.10000 H22B 2 0.844671 0.929181 0.257169 11.00000 10.10000 AFIX 0 C23 1 0.783043 0.961610 0.411768 11.00000 0.03193 0.03520 = 0.03822 -0.00216 0.02015 -0.00331 AFIX 21 H23A 2 0.833280 0.962311 0.482764 11.00000 10.10000 H23B 2 0.775549 0.987438 0.389310 11.00000 10.10000 AFIX 0 C24 1 0.994529 0.957118 0.431474 11.00000 0.03146 0.05717 = 0.05879 0.00194 0.02636 0.00086 AFIX 21 H24A 2 0.980324 0.981861 0.401677 11.00000 10.10000 H24B 2 1.035052 0.961110 0.500680 11.00000 10.10000 AFIX 0 C25 1 1.090449 0.935487 0.422495 11.00000 0.05050 0.07384 = 0.09390 0.01393 0.04986 0.01513 AFIX 31 H25A 2 1.171213 0.949419 0.454440 11.00000 10.10000 H25B 2 1.053550 0.932239 0.354340 11.00000 10.10000 H25C 2 1.107353 0.911100 0.453018 11.00000 10.10000 AFIX 0 C26 1 0.886676 0.719345 0.533266 11.00000 0.13970 0.09635 = 0.14238 0.03818 0.05661 0.00456 AFIX 31 H26A 2 0.834533 0.700104 0.485106 11.00000 10.10000 H26B 2 0.875176 0.717949 0.584404 11.00000 10.10000 H26C 2 0.977602 0.715484 0.560851 11.00000 10.10000 AFIX 0 C27 1 0.593383 0.861974 0.391720 11.00000 0.06049 0.04015 = 0.03692 0.00912 0.03771 0.00705 AFIX 31 H27A 2 0.616226 0.835976 0.411445 11.00000 10.10000 H27B 2 0.510431 0.867475 0.379356 11.00000 10.10000 H27C 2 0.659863 0.878182 0.443088 11.00000 10.10000 AFIX 0 C28 1 0.612555 0.809558 0.119772 11.00000 0.08966 0.07361 = 0.07626 -0.02218 0.06247 -0.00710 AFIX 31 H28A 2 0.702602 0.805715 0.144865 11.00000 10.10000 H28B 2 0.570867 0.825989 0.063629 11.00000 10.10000 H28C 2 0.567793 0.785612 0.100904 11.00000 10.10000 AFIX 0 C30 1 0.596588 1.098685 0.440605 11.00000 0.03971 0.03839 = 0.03456 0.00165 0.02265 0.00295 C31 1 0.637191 1.133584 0.486907 11.00000 0.09709 0.05808 = 0.06884 -0.01577 0.06371 -0.02254 AFIX 41 H31 2 0.634539 1.138754 0.539607 11.00000 10.10000 AFIX 0 C32 1 0.681550 1.160577 0.454218 11.00000 0.15811 0.04853 = 0.10353 -0.01670 0.09790 -0.04023 AFIX 41 H32 2 0.708850 1.184007 0.485433 11.00000 10.10000 AFIX 0 C33 1 0.686288 1.153752 0.377615 11.00000 0.14074 0.07428 = 0.09660 -0.00426 0.09423 -0.04031 AFIX 41 H33 2 0.716360 1.172388 0.356551 11.00000 10.10000 AFIX 0 C34 1 0.647238 1.119826 0.331942 11.00000 0.11228 0.09198 = 0.06976 -0.00145 0.07496 -0.01937 AFIX 41 H34 2 0.650630 1.115228 0.279360 11.00000 10.10000 AFIX 0 C35 1 0.602285 1.091830 0.362264 11.00000 0.06721 0.05615 = 0.04248 0.00186 0.04157 -0.00489 AFIX 41 H35 2 0.575956 1.068509 0.330436 11.00000 10.10000 AFIX 0 C36 1 0.554506 1.068231 0.478836 11.00000 0.02500 0.04085 = 0.02008 0.00796 0.00488 0.00238 C37 1 0.902028 0.983384 0.716952 11.00000 0.02958 0.04869 = 0.02525 0.00213 0.01644 0.00415 C38 1 0.969321 1.009254 0.790852 11.00000 0.03862 0.07055 = 0.04592 -0.00921 0.01804 0.00732 AFIX 41 H38 2 0.924754 1.029829 0.792564 11.00000 10.10000 AFIX 0 C39 1 1.103154 1.005426 0.863568 11.00000 0.04001 0.09282 = 0.05654 -0.02061 0.01638 -0.00536 AFIX 41 H39 2 1.147729 1.023533 0.912964 11.00000 10.10000 AFIX 0 C40 1 1.168083 0.975740 0.862697 11.00000 0.03203 0.11940 = 0.04993 0.00964 0.01417 0.00883 AFIX 41 H40 2 1.257467 0.973016 0.912273 11.00000 10.10000 AFIX 0 C41 1 1.104280 0.949504 0.789796 11.00000 0.05254 0.09709 = 0.07553 0.00325 0.02528 0.03851 AFIX 41 H41 2 1.150146 0.928987 0.789422 11.00000 10.10000 AFIX 0 C42 1 0.968958 0.953356 0.714925 11.00000 0.04355 0.08684 = 0.04338 -0.00343 0.01601 0.02682 AFIX 41 H42 2 0.925283 0.935646 0.664438 11.00000 10.10000 AFIX 0 C43 1 0.756791 0.988203 0.637723 11.00000 0.03661 0.03990 = 0.03206 0.00582 0.02339 0.00675 C44 1 0.432791 1.035372 0.122899 11.00000 0.04155 0.02776 = 0.02484 0.00049 0.01671 0.00160 C45 1 0.354077 1.064733 0.113795 11.00000 0.05369 0.04042 = 0.04340 0.00593 0.02957 0.01038 AFIX 41 H45 2 0.323708 1.064937 0.152159 11.00000 10.10000 AFIX 0 C46 1 0.320166 1.093817 0.048001 11.00000 0.06947 0.04546 = 0.06127 0.02277 0.03236 0.02541 AFIX 41 H46 2 0.265303 1.113199 0.040935 11.00000 10.10000 AFIX 0 C47 1 0.367354 1.094065 -0.006683 11.00000 0.09633 0.05048 = 0.06012 0.01937 0.04588 0.00157 AFIX 41 H47 2 0.344712 1.113747 -0.050667 11.00000 10.10000 AFIX 0 C48 1 0.446789 1.065902 0.002626 11.00000 0.09788 0.07191 = 0.06005 0.02358 0.05578 0.01105 AFIX 41 H48 2 0.480210 1.066566 -0.033682 11.00000 10.10000 AFIX 0 C49 1 0.478074 1.036142 0.066299 11.00000 0.06319 0.05195 = 0.03294 0.00561 0.03260 0.00169 AFIX 41 H49 2 0.530299 1.016422 0.070946 11.00000 10.10000 AFIX 0 C50 1 0.467737 1.002874 0.190960 11.00000 0.02821 0.03069 = 0.02807 0.00458 0.01563 0.00447 O1W 4 0.943208 0.764744 0.323199 10.40000 0.14110 0.14076 = 0.14089 -0.00016 0.08370 0.00028 O2W 4 0.744552 0.649153 0.170462 10.10000 0.07333 0.07333 = 0.07335 -0.00013 0.04357 0.00008 HKLF 4 REM sad in P2(1)/c REM R1 = 0.0789 for 7740 Fo > 4sig(Fo) and 0.1082 for all 10288 data REM 775 parameters refined using 111 restraints END ;